Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Richard Hartshorn' _publ_contact_author_address ; Department of Chemistry University of Canterbury Private Bag 4800 Christchurch NEW ZEALAND ; _publ_contact_author_email ICHARD.HARTSHORN@CANTERBURY.AC.NZ _publ_section_title ; Coordination chemistry of a terpyridine-tris(pyrazolyl) ditopic ligand ; loop_ _publ_author_name 'Richard Hartshorn' 'Ramin Zibaseresht' data_PzT _database_code_depnum_ccdc_archive 'CCDC 277287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H27 N9 O' _chemical_formula_sum 'C33 H27 N9 O' _chemical_formula_weight 565.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 11.429(11) _cell_length_b 8.715(7) _cell_length_c 55.97(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5575(9) _cell_formula_units_Z 8 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used 3781 _cell_measurement_theta_min 4.992 _cell_measurement_theta_max 51.319 _exptl_crystal_description Rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9377 _exptl_absorpt_correction_T_max 0.9948 _exptl_absorpt_process_details 'SADABS V2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 191(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 SMART/CCD _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14399 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -66 _diffrn_reflns_limit_l_max 65 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.05 _reflns_number_total 4801 _reflns_number_gt 3327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker XPREP' _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^)+(0.0390P)^2^+7.1027P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4801 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1336 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.6956(2) 0.1730(3) 0.20828(4) 0.0315(6) Uani 1 1 d . . . N1' N 0.3973(2) 0.3023(3) 0.19740(4) 0.0276(6) Uani 1 1 d . . . N1" N 0.1431(2) 0.4395(4) 0.16532(5) 0.0391(7) Uani 1 1 d . . . N01 N 0.9843(2) 0.5799(3) 0.05317(4) 0.0319(7) Uani 1 1 d . . . N02 N 0.8888(2) 0.5674(4) 0.03851(5) 0.0443(8) Uani 1 1 d . . . N01' N 1.0934(2) 0.8042(3) 0.04141(4) 0.0339(7) Uani 1 1 d . . . N02' N 1.0518(3) 0.9227(4) 0.02827(5) 0.0497(8) Uani 1 1 d . . . N01" N 1.0947(2) 0.7227(3) 0.08116(4) 0.0312(6) Uani 1 1 d . . . N02" N 1.1848(2) 0.8249(4) 0.08504(5) 0.0402(7) Uani 1 1 d . . . O O 0.8506(2) 0.7670(3) 0.08333(4) 0.0475(7) Uani 1 1 d . . . C2 C 0.5812(3) 0.2031(4) 0.21285(5) 0.0266(7) Uani 1 1 d . . . C3 C 0.5243(3) 0.1433(4) 0.23272(5) 0.0335(8) Uani 1 1 d . . . H3 H 0.4444 0.1666 0.2357 0.040 Uiso 1 1 calc R . . C4 C 0.5866(3) 0.0490(4) 0.24802(6) 0.0396(9) Uani 1 1 d . . . H4 H 0.5497 0.0072 0.2618 0.048 Uiso 1 1 calc R . . C5 C 0.7040(3) 0.0153(4) 0.24320(6) 0.0393(9) Uani 1 1 d . . . H5 H 0.7478 -0.0508 0.2533 0.047 Uiso 1 1 calc R . . C6 C 0.7538(3) 0.0812(4) 0.22335(5) 0.0355(8) Uani 1 1 d . . . H6 H 0.8339 0.0605 0.2201 0.043 Uiso 1 1 calc R . . C2' C 0.5159(2) 0.3003(4) 0.19525(5) 0.0257(7) Uani 1 1 d . . . C3' C 0.5758(3) 0.3816(4) 0.17771(5) 0.0269(7) Uani 1 1 d . . . H3' H 0.6586 0.3755 0.1767 0.032 Uiso 1 1 calc R . . C4' C 0.5132(3) 0.4725(4) 0.16153(5) 0.0250(7) Uani 1 1 d . . . C5' C 0.3904(2) 0.4704(4) 0.16357(5) 0.0270(7) Uani 1 1 d . . . H4' H 0.3442 0.5285 0.1527 0.032 Uiso 1 1 calc R . . C6' C 0.3361(2) 0.3842(4) 0.18126(5) 0.0251(7) Uani 1 1 d . . . C2" C 0.2043(2) 0.3762(4) 0.18315(5) 0.0280(7) Uani 1 1 d . . . C3" C 0.1494(3) 0.3046(4) 0.20204(5) 0.0339(8) Uani 1 1 d . . . H3" H 0.1942 0.2593 0.2145 0.041 Uiso 1 1 calc R . . C4" C 0.0274(3) 0.2994(4) 0.20276(6) 0.0385(9) Uani 1 1 d . . . H4" H -0.0112 0.2520 0.2159 0.046 Uiso 1 1 calc R . . C5" C -0.0364(3) 0.3625(4) 0.18458(6) 0.0387(9) Uani 1 1 d . . . H5" H -0.1195 0.3591 0.1846 0.046 Uiso 1 1 calc R . . C6" C 0.0246(3) 0.4307(5) 0.16634(6) 0.0428(9) Uani 1 1 d . . . H6" H -0.0189 0.4747 0.1536 0.051 Uiso 1 1 calc R . . C1"' C 0.5733(2) 0.5656(4) 0.14302(5) 0.0264(7) Uani 1 1 d . . . C2"' C 0.5144(3) 0.6081(4) 0.12240(5) 0.0292(7) Uani 1 1 d . . . H2"' H 0.4361 0.5752 0.1199 0.035 Uiso 1 1 calc R . . C3"' C 0.5693(3) 0.6985(4) 0.10536(5) 0.0318(8) Uani 1 1 d . . . H3"' H 0.5277 0.7262 0.0913 0.038 Uiso 1 1 calc R . . C4"' C 0.6850(3) 0.7500(4) 0.10839(5) 0.0285(7) Uani 1 1 d . . . C5"' C 0.7446(3) 0.7094(4) 0.12897(5) 0.0316(8) Uani 1 1 d . . . H5"' H 0.8228 0.7431 0.1314 0.038 Uiso 1 1 calc R . . C6"' C 0.6895(3) 0.6191(4) 0.14597(5) 0.0289(7) Uani 1 1 d . . . H6"' H 0.7310 0.5923 0.1601 0.035 Uiso 1 1 calc R . . C7 C 0.7458(3) 0.8439(4) 0.08946(6) 0.0378(8) Uani 1 1 d . . . H7A H 0.6950 0.8543 0.0752 0.045 Uiso 1 1 calc R . . H7B H 0.7635 0.9478 0.0956 0.045 Uiso 1 1 calc R . . C01 C 0.9134(3) 0.8409(4) 0.06485(5) 0.0359(8) Uani 1 1 d . . . H01A H 0.9382 0.9448 0.0699 0.043 Uiso 1 1 calc R . . H01B H 0.8646 0.8503 0.0503 0.043 Uiso 1 1 calc R . . C02 C 1.0214(3) 0.7378(4) 0.05998(5) 0.0298(7) Uani 1 1 d . . . C03 C 0.8933(3) 0.4204(5) 0.03105(6) 0.0517(10) Uani 1 1 d . . . H03 H 0.8373 0.3768 0.0205 0.062 Uiso 1 1 calc R . . C04 C 0.9888(3) 0.3375(5) 0.04033(6) 0.0454(9) Uani 1 1 d . . . H04 H 1.0080 0.2327 0.0378 0.054 Uiso 1 1 calc R . . C05 C 1.0474(3) 0.4434(4) 0.05386(6) 0.0364(8) Uani 1 1 d . . . H05 H 1.1186 0.4267 0.0622 0.044 Uiso 1 1 calc R . . C03' C 1.1338(3) 0.9388(5) 0.01154(6) 0.0492(10) Uani 1 1 d . . . H03' H 1.1300 1.0142 -0.0007 0.059 Uiso 1 1 calc R . . C04' C 1.2248(3) 0.8356(5) 0.01366(6) 0.0454(10) Uani 1 1 d . . . H04' H 1.2922 0.8277 0.0038 0.054 Uiso 1 1 calc R . . C05' C 1.1972(3) 0.7474(5) 0.03295(6) 0.0472(10) Uani 1 1 d . . . H05' H 1.2409 0.6639 0.0392 0.057 Uiso 1 1 calc R . . C03" C 1.2161(3) 0.7966(4) 0.10731(6) 0.0396(9) Uani 1 1 d . . . H03" H 1.2785 0.8474 0.1153 0.047 Uiso 1 1 calc R . . C04" C 1.1466(3) 0.6830(4) 0.11781(6) 0.0392(9) Uani 1 1 d . . . H04" H 1.1531 0.6449 0.1337 0.047 Uiso 1 1 calc R . . C05" C 1.0676(3) 0.6375(4) 0.10095(5) 0.0377(9) Uani 1 1 d . . . H05" H 1.0073 0.5633 0.1026 0.045 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 N1 0.0284(14) 0.0370(17) 0.0291(14) 0.0012(13) -0.0031(11) 0.0007(13) N1' 0.0263(13) 0.0317(16) 0.0247(13) 0.0004(12) 0.0006(10) -0.0010(13) N1" 0.0252(14) 0.060(2) 0.0318(15) 0.0045(14) -0.0031(12) 0.0013(14) N01 0.0304(14) 0.0371(18) 0.0283(14) 0.0002(13) -0.0022(11) -0.0007(14) N02 0.0400(17) 0.057(2) 0.0355(16) -0.0002(16) -0.0098(13) -0.0018(16) N01' 0.0376(15) 0.0415(18) 0.0226(13) 0.0070(13) 0.0036(11) 0.0005(14) N02' 0.0463(18) 0.057(2) 0.0455(18) 0.0217(17) 0.0058(14) 0.0050(17) N01" 0.0334(14) 0.0363(17) 0.0238(13) 0.0005(12) 0.0003(11) -0.0034(14) N02" 0.0348(15) 0.0447(19) 0.0412(17) 0.0024(14) -0.0013(13) -0.0066(15) O 0.0489(14) 0.0519(17) 0.0417(14) 0.0210(13) 0.0220(11) 0.0185(13) C2 0.0308(17) 0.0268(18) 0.0221(15) -0.0018(13) -0.0010(12) -0.0022(15) C3 0.0350(18) 0.038(2) 0.0277(16) 0.0014(15) 0.0022(14) 0.0041(16) C4 0.050(2) 0.041(2) 0.0278(17) 0.0047(16) 0.0026(15) 0.0009(19) C5 0.046(2) 0.040(2) 0.0321(18) 0.0057(16) -0.0103(15) 0.0043(18) C6 0.0304(16) 0.039(2) 0.0366(18) -0.0005(17) -0.0063(15) 0.0026(17) C2' 0.0255(15) 0.0302(19) 0.0214(15) -0.0023(14) 0.0010(12) 0.0001(15) C3' 0.0235(15) 0.0321(19) 0.0252(16) -0.0025(14) -0.0001(12) -0.0012(14) C4' 0.0264(16) 0.0298(19) 0.0190(14) -0.0025(13) 0.0001(12) -0.0016(14) C5' 0.0254(16) 0.034(2) 0.0213(15) -0.0008(14) -0.0027(12) 0.0014(15) C6' 0.0240(15) 0.0293(19) 0.0220(15) -0.0040(14) 0.0018(12) -0.0002(14) C2" 0.0240(16) 0.033(2) 0.0266(16) -0.0050(14) -0.0005(12) -0.0006(15) C3" 0.0269(16) 0.045(2) 0.0302(17) 0.0001(16) 0.0025(13) -0.0030(17) C4" 0.0328(18) 0.046(2) 0.0363(18) -0.0051(17) 0.0075(14) -0.0047(18) C5" 0.0222(16) 0.050(2) 0.044(2) -0.0138(18) 0.0017(15) -0.0009(16) C6" 0.0280(18) 0.065(3) 0.0351(19) 0.0017(18) -0.0058(14) 0.0032(18) C1"' 0.0271(16) 0.0274(19) 0.0248(15) 0.0003(14) 0.0013(12) 0.0029(15) C2"' 0.0231(15) 0.037(2) 0.0275(16) 0.0014(15) 0.0004(12) 0.0013(15) C3"' 0.0337(17) 0.037(2) 0.0250(16) 0.0061(15) 0.0023(13) 0.0033(16) C4"' 0.0309(16) 0.0246(19) 0.0300(16) 0.0034(14) 0.0071(13) 0.0010(15) C5"' 0.0267(16) 0.033(2) 0.0356(17) 0.0017(15) 0.0026(14) -0.0056(16) C6"' 0.0301(16) 0.035(2) 0.0216(15) 0.0006(14) -0.0014(12) -0.0008(15) C7 0.0337(18) 0.036(2) 0.0437(19) 0.0123(16) 0.0077(15) 0.0023(16) C01 0.046(2) 0.036(2) 0.0254(16) 0.0100(15) 0.0091(14) 0.0031(17) C02 0.0307(17) 0.036(2) 0.0230(15) 0.0040(14) 0.0028(13) -0.0008(16) C03 0.060(3) 0.055(3) 0.040(2) -0.008(2) -0.0101(18) -0.011(2) C04 0.050(2) 0.040(2) 0.045(2) -0.0074(19) 0.0035(17) -0.0029(19) C05 0.0312(18) 0.042(2) 0.0362(19) 0.0015(17) 0.0016(14) 0.0019(17) C03' 0.045(2) 0.065(3) 0.038(2) 0.022(2) 0.0040(16) -0.012(2) C04' 0.048(2) 0.056(3) 0.0317(18) -0.0077(18) 0.0107(16) -0.014(2) C05' 0.049(2) 0.049(2) 0.044(2) 0.0063(19) 0.0155(17) 0.005(2) C03" 0.039(2) 0.042(2) 0.0369(19) -0.0036(17) -0.0110(15) 0.0010(18) C04" 0.045(2) 0.044(2) 0.0283(17) 0.0036(17) -0.0040(15) 0.0070(19) C05" 0.0407(19) 0.044(2) 0.0282(17) 0.0067(16) 0.0019(14) -0.0016(17) _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 N1 C6 1.340(4) . ? N1 C2 1.358(4) . ? N1' C6' 1.348(4) . ? N1' C2' 1.361(4) . ? N1" C2" 1.338(4) . ? N1" C6" 1.358(4) . ? N01 N02 1.369(4) . ? N01 C05 1.392(4) . ? N01 C02 1.490(4) . ? N02 C03 1.349(5) . ? N01' N02' 1.354(4) . ? N01' C05' 1.370(4) . ? N01' C02 1.447(4) . ? N02' C03' 1.333(4) . ? N01" C05" 1.369(4) . ? N01" N02" 1.379(4) . ? N01" C02 1.457(4) . ? N02" C03" 1.320(4) . ? O C01 1.414(4) . ? O C7 1.415(4) . ? C2 C3 1.390(4) . ? C2 C2' 1.499(4) . ? C3 C4 1.384(5) . ? C3 H3 0.9500 . ? C4 C5 1.400(5) . ? C4 H4 0.9500 . ? C5 C6 1.374(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C2' C3' 1.390(4) . ? C3' C4' 1.399(4) . ? C3' H3' 0.9500 . ? C4' C5' 1.409(4) . ? C4' C1"' 1.484(4) . ? C5' C6' 1.389(4) . ? C5' H4' 0.9500 . ? C6' C2" 1.511(4) . ? C2" C3" 1.379(4) . ? C3" C4" 1.395(4) . ? C3" H3" 0.9500 . ? C4" C5" 1.367(5) . ? C4" H4" 0.9500 . ? C5" C6" 1.372(5) . ? C5" H5" 0.9500 . ? C6" H6" 0.9500 . ? C1"' C2"' 1.387(4) . ? C1"' C6"' 1.417(4) . ? C2"' C3"' 1.387(4) . ? C2"' H2"' 0.9500 . ? C3"' C4"' 1.407(4) . ? C3"' H3"' 0.9500 . ? C4"' C5"' 1.384(4) . ? C4"' C7 1.508(4) . ? C5"' C6"' 1.386(4) . ? C5"' H5"' 0.9500 . ? C6"' H6"' 0.9500 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C01 C02 1.551(5) . ? C01 H01A 0.9900 . ? C01 H01B 0.9900 . ? C03 C04 1.407(5) . ? C03 H03 0.9500 . ? C04 C05 1.369(5) . ? C04 H04 0.9500 . ? C05 H05 0.9500 . ? C03' C04' 1.381(5) . ? C03' H03' 0.9500 . ? C04' C05' 1.363(5) . ? C04' H04' 0.9500 . ? C05' H05' 0.9500 . ? C03" C04" 1.399(5) . ? C03" H03" 0.9500 . ? C04" C05" 1.364(5) . ? C04" H04" 0.9500 . ? C05" H05" 0.9500 . ? 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 C6 N1 C2 118.3(3) . . ? C6' N1' C2' 117.7(3) . . ? C2" N1" C6" 117.9(3) . . ? N02 N01 C05 111.2(3) . . ? N02 N01 C02 117.0(3) . . ? C05 N01 C02 129.4(3) . . ? C03 N02 N01 103.3(3) . . ? N02' N01' C05' 113.1(3) . . ? N02' N01' C02 119.7(3) . . ? C05' N01' C02 126.6(3) . . ? C03' N02' N01' 102.4(3) . . ? C05" N01" N02" 113.0(3) . . ? C05" N01" C02 125.2(3) . . ? N02" N01" C02 120.0(3) . . ? C03" N02" N01" 103.3(3) . . ? C01 O C7 113.0(2) . . ? N1 C2 C3 121.9(3) . . ? N1 C2 C2' 117.7(3) . . ? C3 C2 C2' 120.3(3) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 119.9(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 117.7(3) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? N1 C6 C5 123.6(3) . . ? N1 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? N1' C2' C3' 123.1(3) . . ? N1' C2' C2 116.4(3) . . ? C3' C2' C2 120.5(3) . . ? C2' C3' C4' 119.6(3) . . ? C2' C3' H3' 120.2 . . ? C4' C3' H3' 120.2 . . ? C3' C4' C5' 116.7(3) . . ? C3' C4' C1"' 121.6(3) . . ? C5' C4' C1"' 121.6(3) . . ? C6' C5' C4' 120.7(3) . . ? C6' C5' H4' 119.7 . . ? C4' C5' H4' 119.7 . . ? N1' C6' C5' 122.2(3) . . ? N1' C6' C2" 116.5(3) . . ? C5' C6' C2" 121.4(3) . . ? N1" C2" C3" 121.3(3) . . ? N1" C2" C6' 116.7(3) . . ? C3" C2" C6' 121.9(3) . . ? C2" C3" C4" 119.5(3) . . ? C2" C3" H3" 120.3 . . ? C4" C3" H3" 120.3 . . ? C5" C4" C3" 119.9(3) . . ? C5" C4" H4" 120.1 . . ? C3" C4" H4" 120.1 . . ? C4" C5" C6" 117.2(3) . . ? C4" C5" H5" 121.4 . . ? C6" C5" H5" 121.4 . . ? N1" C6" C5" 124.2(3) . . ? N1" C6" H6" 117.9 . . ? C5" C6" H6" 117.9 . . ? C2"' C1"' C6"' 117.6(3) . . ? C2"' C1"' C4' 120.2(3) . . ? C6"' C1"' C4' 122.2(3) . . ? C1"' C2"' C3"' 120.3(3) . . ? C1"' C2"' H2"' 119.8 . . ? C3"' C2"' H2"' 119.8 . . ? C2"' C3"' C4"' 121.6(3) . . ? C2"' C3"' H3"' 119.2 . . ? C4"' C3"' H3"' 119.2 . . ? C5"' C4"' C3"' 118.8(3) . . ? C5"' C4"' C7 119.8(3) . . ? C3"' C4"' C7 121.4(3) . . ? C4"' C5"' C6"' 119.5(3) . . ? C4"' C5"' H5"' 120.2 . . ? C6"' C5"' H5"' 120.2 . . ? C5"' C6"' C1"' 122.2(3) . . ? C5"' C6"' H6"' 118.9 . . ? C1"' C6"' H6"' 118.9 . . ? O C7 C4"' 107.6(3) . . ? O C7 H7A 110.2 . . ? C4"' C7 H7A 110.2 . . ? O C7 H7B 110.2 . . ? C4"' C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? O C01 C02 105.5(3) . . ? O C01 H01A 110.6 . . ? C02 C01 H01A 110.6 . . ? O C01 H01B 110.6 . . ? C02 C01 H01B 110.6 . . ? H01A C01 H01B 108.8 . . ? N01' C02 N01" 107.0(2) . . ? N01' C02 N01 110.3(2) . . ? N01" C02 N01 106.8(2) . . ? N01' C02 C01 110.3(3) . . ? N01" C02 C01 111.5(2) . . ? N01 C02 C01 110.7(3) . . ? N02 C03 C04 113.8(3) . . ? N02 C03 H03 123.1 . . ? C04 C03 H03 123.1 . . ? C05 C04 C03 103.8(3) . . ? C05 C04 H04 128.1 . . ? C03 C04 H04 128.1 . . ? C04 C05 N01 107.8(3) . . ? C04 C05 H05 126.1 . . ? N01 C05 H05 126.1 . . ? N02' C03' C04' 113.7(3) . . ? N02' C03' H03' 123.2 . . ? C04' C03' H03' 123.2 . . ? C05' C04' C03' 105.1(3) . . ? C05' C04' H04' 127.4 . . ? C03' C04' H04' 127.4 . . ? C04' C05' N01' 105.7(3) . . ? C04' C05' H05' 127.2 . . ? N01' C05' H05' 127.2 . . ? N02" C03" C04" 112.0(3) . . ? N02" C03" H03" 124.0 . . ? C04" C03" H03" 124.0 . . ? C05" C04" C03" 106.9(3) . . ? C05" C04" H04" 126.6 . . ? C03" C04" H04" 126.6 . . ? C04" C05" N01" 104.6(3) . . ? C04" C05" H05" 127.7 . . ? N01" C05" H05" 127.7 . . ? 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 C05 N01 N02 C03 1.9(4) . . . . ? C02 N01 N02 C03 166.0(3) . . . . ? C05' N01' N02' C03' -0.7(4) . . . . ? C02 N01' N02' C03' -172.4(3) . . . . ? C05" N01" N02" C03" 2.5(4) . . . . ? C02 N01" N02" C03" 168.2(3) . . . . ? C6 N1 C2 C3 0.9(5) . . . . ? C6 N1 C2 C2' -177.4(3) . . . . ? N1 C2 C3 C4 -0.8(5) . . . . ? C2' C2 C3 C4 177.4(3) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 1.3(5) . . . . ? C2 N1 C6 C5 0.2(5) . . . . ? C4 C5 C6 N1 -1.2(5) . . . . ? C6' N1' C2' C3' 1.7(5) . . . . ? C6' N1' C2' C2 -177.6(3) . . . . ? N1 C2 C2' N1' 166.6(3) . . . . ? C3 C2 C2' N1' -11.7(4) . . . . ? N1 C2 C2' C3' -12.7(4) . . . . ? C3 C2 C2' C3' 169.0(3) . . . . ? N1' C2' C3' C4' 1.1(5) . . . . ? C2 C2' C3' C4' -179.6(3) . . . . ? C2' C3' C4' C5' -2.6(4) . . . . ? C2' C3' C4' C1"' 177.8(3) . . . . ? C3' C4' C5' C6' 1.4(4) . . . . ? C1"' C4' C5' C6' -179.0(3) . . . . ? C2' N1' C6' C5' -3.0(4) . . . . ? C2' N1' C6' C2" 176.3(3) . . . . ? C4' C5' C6' N1' 1.4(5) . . . . ? C4' C5' C6' C2" -177.8(3) . . . . ? C6" N1" C2" C3" -0.2(5) . . . . ? C6" N1" C2" C6' 178.5(3) . . . . ? N1' C6' C2" N1" -171.0(3) . . . . ? C5' C6' C2" N1" 8.2(5) . . . . ? N1' C6' C2" C3" 7.7(5) . . . . ? C5' C6' C2" C3" -173.0(3) . . . . ? N1" C2" C3" C4" -0.7(5) . . . . ? C6' C2" C3" C4" -179.4(3) . . . . ? C2" C3" C4" C5" 1.2(5) . . . . ? C3" C4" C5" C6" -0.8(5) . . . . ? C2" N1" C6" C5" 0.7(6) . . . . ? C4" C5" C6" N1" -0.2(6) . . . . ? C3' C4' C1"' C2"' 156.4(3) . . . . ? C5' C4' C1"' C2"' -23.2(5) . . . . ? C3' C4' C1"' C6"' -26.1(5) . . . . ? C5' C4' C1"' C6"' 154.3(3) . . . . ? C6"' C1"' C2"' C3"' 0.7(5) . . . . ? C4' C1"' C2"' C3"' 178.3(3) . . . . ? C1"' C2"' C3"' C4"' -0.2(5) . . . . ? C2"' C3"' C4"' C5"' -0.2(5) . . . . ? C2"' C3"' C4"' C7 178.0(3) . . . . ? C3"' C4"' C5"' C6"' 0.2(5) . . . . ? C7 C4"' C5"' C6"' -178.0(3) . . . . ? C4"' C5"' C6"' C1"' 0.3(5) . . . . ? C2"' C1"' C6"' C5"' -0.8(5) . . . . ? C4' C1"' C6"' C5"' -178.3(3) . . . . ? C01 O C7 C4"' 177.4(3) . . . . ? C5"' C4"' C7 O 53.9(4) . . . . ? C3"' C4"' C7 O -124.2(3) . . . . ? C7 O C01 C02 -177.8(3) . . . . ? N02' N01' C02 N01" -133.1(3) . . . . ? C05' N01' C02 N01" 56.4(4) . . . . ? N02' N01' C02 N01 111.1(3) . . . . ? C05' N01' C02 N01 -59.4(4) . . . . ? N02' N01' C02 C01 -11.6(4) . . . . ? C05' N01' C02 C01 177.9(3) . . . . ? C05" N01" C02 N01' -166.1(3) . . . . ? N02" N01" C02 N01' 30.1(4) . . . . ? C05" N01" C02 N01 -47.9(4) . . . . ? N02" N01" C02 N01 148.3(3) . . . . ? C05" N01" C02 C01 73.2(4) . . . . ? N02" N01" C02 C01 -90.6(3) . . . . ? N02 N01 C02 N01' -82.9(3) . . . . ? C05 N01 C02 N01' 77.8(4) . . . . ? N02 N01 C02 N01" 161.1(2) . . . . ? C05 N01 C02 N01" -38.2(4) . . . . ? N02 N01 C02 C01 39.5(3) . . . . ? C05 N01 C02 C01 -159.8(3) . . . . ? O C01 C02 N01' -179.2(3) . . . . ? O C01 C02 N01" -60.4(3) . . . . ? O C01 C02 N01 58.3(3) . . . . ? N01 N02 C03 C04 -0.2(4) . . . . ? N02 C03 C04 C05 -1.6(4) . . . . ? C03 C04 C05 N01 2.6(4) . . . . ? N02 N01 C05 C04 -3.0(4) . . . . ? C02 N01 C05 C04 -164.6(3) . . . . ? N01' N02' C03' C04' 0.0(4) . . . . ? N02' C03' C04' C05' 0.7(5) . . . . ? C03' C04' C05' N01' -1.0(4) . . . . ? N02' N01' C05' C04' 1.1(4) . . . . ? C02 N01' C05' C04' 172.1(3) . . . . ? N01" N02" C03" C04" -1.7(4) . . . . ? N02" C03" C04" C05" 0.3(4) . . . . ? C03" C04" C05" N01" 1.2(4) . . . . ? N02" N01" C05" C04" -2.4(4) . . . . ? C02 N01" C05" C04" -167.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.282 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.048 #====END data_[Ag2(PzT)2](BF4)2 _database_code_depnum_ccdc_archive 'CCDC 277288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C66 H54 Ag2 N18 O2, 2(B F4) ; _chemical_formula_sum 'C66 H54 Ag2 B2 F8 N18 O2' _chemical_formula_weight 1520.63 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' 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 'p 21/c' _symmetry_space_group_name_hall '-p 2ybc' 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 8.5329(16) _cell_length_b 22.108(5) _cell_length_c 17.393(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.534(3) _cell_angle_gamma 90.00 _cell_volume 3259.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3782 _cell_measurement_theta_min 4.376 _cell_measurement_theta_max 41.325 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.549 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7482 _exptl_absorpt_correction_T_max 0.9537 _exptl_absorpt_process_details 'sadabs v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type SMART/CCD _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28177 _diffrn_reflns_av_R_equivalents 0.1203 _diffrn_reflns_av_sigmaI/netI 0.1290 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 26.41 _reflns_number_total 6637 _reflns_number_gt 2895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker XPREP' _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^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6637 _refine_ls_number_parameters 480 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1633 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.953 _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 Ag Ag 0.62909(5) -0.063530(18) 1.23285(2) 0.06719(17) Uani 1 1 d . . . N1 N 0.4809(6) 0.0255(2) 1.2883(3) 0.0923(16) Uani 1 1 d . . . N1' N 0.4332(4) -0.02136(17) 1.14480(19) 0.0446(9) Uani 1 1 d . . . N1" N 0.5636(4) -0.13154(17) 1.1287(2) 0.0512(10) Uani 1 1 d . . . N01 N 0.0719(4) 0.07711(16) 0.62938(19) 0.0479(10) Uani 1 1 d . . . N02 N 0.1612(4) 0.04320(18) 0.6819(2) 0.0533(10) Uani 1 1 d . . . N01' N 0.0049(4) 0.16688(16) 0.5594(2) 0.0492(10) Uani 1 1 d . . . N02' N 0.0558(5) 0.14914(19) 0.4915(2) 0.0756(13) Uani 1 1 d . . . N01" N 0.2565(4) 0.15659(18) 0.6333(2) 0.0528(10) Uani 1 1 d . . . N02" N 0.3211(5) 0.2019(2) 0.6787(2) 0.0703(12) Uani 1 1 d . . . O O -0.1259(3) 0.14409(13) 0.70666(15) 0.0497(8) Uani 1 1 d . . . C2 C 0.3957(5) 0.0577(2) 1.2366(3) 0.0592(13) Uani 1 1 d . . . C3 C 0.3361(9) 0.1124(3) 1.2542(4) 0.135(3) Uani 1 1 d . . . H3 H 0.2741 0.1344 1.2166 0.163 Uiso 1 1 calc R . . C4 C 0.3683(11) 0.1349(4) 1.3280(4) 0.157(4) Uani 1 1 d . . . H4 H 0.3251 0.1716 1.3413 0.188 Uiso 1 1 calc R . . C5 C 0.4623(8) 0.1036(4) 1.3805(4) 0.106(2) Uani 1 1 d . . . H5 H 0.4924 0.1190 1.4297 0.127 Uiso 1 1 calc R . . C6 C 0.5111(7) 0.0493(4) 1.3594(4) 0.117(3) Uani 1 1 d . . . H6 H 0.5705 0.0263 1.3968 0.140 Uiso 1 1 calc R . . C2' C 0.3610(5) 0.0311(2) 1.1573(3) 0.0475(11) Uani 1 1 d . . . C3' C 0.2594(5) 0.0586(2) 1.1007(2) 0.0503(11) Uani 1 1 d . . . H3' H 0.2118 0.0950 1.1114 0.060 Uiso 1 1 calc R . . C4' C 0.2270(5) 0.0328(2) 1.0277(2) 0.0421(11) Uani 1 1 d . . . C5' C 0.2995(5) -0.0222(2) 1.0160(2) 0.0453(11) Uani 1 1 d . . . H5' H 0.2812 -0.0415 0.9683 0.054 Uiso 1 1 calc R . . C6' C 0.3991(5) -0.04849(19) 1.0754(2) 0.0410(11) Uani 1 1 d . . . C2" C 0.4747(5) -0.1088(2) 1.0663(3) 0.0436(11) Uani 1 1 d . . . C3" C 0.4548(6) -0.1404(2) 0.9979(3) 0.0641(14) Uani 1 1 d . . . H3" H 0.3918 -0.1245 0.9556 0.077 Uiso 1 1 calc R . . C4" C 0.5279(7) -0.1954(3) 0.9918(3) 0.0781(16) Uani 1 1 d . . . H4" H 0.5165 -0.2165 0.9452 0.094 Uiso 1 1 calc R . . C5" C 0.6170(6) -0.2186(2) 1.0549(3) 0.0697(15) Uani 1 1 d . . . H5" H 0.6671 -0.2558 1.0525 0.084 Uiso 1 1 calc R . . C6" C 0.6306(6) -0.1858(2) 1.1213(3) 0.0642(14) Uani 1 1 d . . . H6" H 0.6901 -0.2021 1.1645 0.077 Uiso 1 1 calc R . . C1"' C 0.1201(5) 0.0622(2) 0.9646(2) 0.0440(10) Uani 1 1 d . . . C6"' C 0.0667(6) 0.1206(2) 0.9731(3) 0.0641(14) Uani 1 1 d . . . H6"' H 0.0954 0.1412 1.0191 0.077 Uiso 1 1 calc R . . C5"' C -0.0287(6) 0.1488(2) 0.9141(3) 0.0702(15) Uani 1 1 d . . . H5"' H -0.0614 0.1883 0.9212 0.084 Uiso 1 1 calc R . . C4"' C -0.0760(5) 0.1203(2) 0.8458(3) 0.0492(12) Uani 1 1 d . . . C3"' C -0.0262(5) 0.0618(2) 0.8375(2) 0.0539(12) Uani 1 1 d . . . H3"' H -0.0583 0.0410 0.7920 0.065 Uiso 1 1 calc R . . C2"' C 0.0708(5) 0.0333(2) 0.8955(3) 0.0484(12) Uani 1 1 d . . . H2"' H 0.1036 -0.0061 0.8880 0.058 Uiso 1 1 calc R . . C7 C -0.1791(5) 0.1524(2) 0.7815(2) 0.0626(14) Uani 1 1 d . . . H7A H -0.2862 0.1373 0.7800 0.075 Uiso 1 1 calc R . . H7B H -0.1807 0.1953 0.7931 0.075 Uiso 1 1 calc R . . C01 C 0.0249(5) 0.16921(19) 0.7022(2) 0.0449(11) Uani 1 1 d . . . H01A H 0.0948 0.1590 0.7483 0.054 Uiso 1 1 calc R . . H01B H 0.0174 0.2129 0.6985 0.054 Uiso 1 1 calc R . . C02 C 0.0899(5) 0.1436(2) 0.6306(2) 0.0431(11) Uani 1 1 d . . . C03 C 0.0976(7) -0.0121(3) 0.6739(3) 0.0682(15) Uani 1 1 d . . . H03 H 0.1357 -0.0457 0.7023 0.082 Uiso 1 1 calc R . . C04 C -0.0307(7) -0.0132(3) 0.6186(3) 0.0760(16) Uani 1 1 d . . . H04 H -0.0940 -0.0462 0.6031 0.091 Uiso 1 1 calc R . . C05 C -0.0453(6) 0.0447(3) 0.5912(3) 0.0702(15) Uani 1 1 d . . . H05 H -0.1221 0.0589 0.5533 0.084 Uiso 1 1 calc R . . C03' C -0.0541(7) 0.1715(2) 0.4387(3) 0.0735(16) Uani 1 1 d . . . H03' H -0.0530 0.1665 0.3857 0.088 Uiso 1 1 calc R . . C04' C -0.1692(6) 0.2027(2) 0.4709(3) 0.0666(14) Uani 1 1 d . . . H04' H -0.2564 0.2222 0.4450 0.080 Uiso 1 1 calc R . . C05' C -0.1287(5) 0.1992(2) 0.5486(3) 0.0532(12) Uani 1 1 d . . . H05' H -0.1830 0.2160 0.5868 0.064 Uiso 1 1 calc R . . C03" C 0.4742(8) 0.1993(3) 0.6683(4) 0.089(2) Uani 1 1 d . . . H03" H 0.5505 0.2254 0.6917 0.107 Uiso 1 1 calc R . . C04" C 0.5048(7) 0.1539(4) 0.6195(4) 0.098(2) Uani 1 1 d . . . H04" H 0.6023 0.1435 0.6043 0.117 Uiso 1 1 calc R . . C05" C 0.3650(7) 0.1271(3) 0.5976(3) 0.0858(18) Uani 1 1 d . . . H05" H 0.3472 0.0944 0.5641 0.103 Uiso 1 1 calc R . . B B 0.8518(4) 0.15770(14) 0.18808(19) 0.079(2) Uani 1 1 d D . . F1A F 0.7567(13) 0.2046(4) 0.1868(7) 0.136(7) Uani 0.478(15) 1 d PD A 1 F2A F 0.9418(12) 0.1627(6) 0.1318(5) 0.174(8) Uani 0.478(15) 1 d PD A 1 F3A F 0.9410(12) 0.1558(6) 0.2549(4) 0.151(6) Uani 0.478(15) 1 d PD A 1 F4A F 0.7680(15) 0.1078(4) 0.1788(7) 0.187(9) Uani 0.478(15) 1 d PD A 1 F1B F 0.846(2) 0.1583(5) 0.2634(2) 0.288(11) Uani 0.522(15) 1 d PD A 2 F2B F 0.7551(12) 0.1990(3) 0.1553(7) 0.111(5) Uani 0.522(15) 1 d PD A 2 F3B F 0.8093(14) 0.1040(3) 0.1604(6) 0.162(8) Uani 0.522(15) 1 d PD A 2 F4B F 0.9964(8) 0.1696(5) 0.1732(11) 0.273(13) Uani 0.522(15) 1 d PD A 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 Ag 0.0756(3) 0.0738(3) 0.0472(2) 0.0032(2) -0.01456(16) 0.0121(2) N1 0.113(4) 0.115(4) 0.044(3) -0.020(3) -0.017(3) 0.055(3) N1' 0.047(2) 0.046(3) 0.039(2) 0.000(2) -0.0009(17) -0.0001(19) N1" 0.055(2) 0.047(3) 0.050(3) 0.000(2) -0.0019(19) 0.007(2) N01 0.053(2) 0.045(3) 0.044(2) 0.002(2) -0.0036(18) 0.0049(19) N02 0.063(3) 0.044(3) 0.051(3) 0.007(2) -0.0029(19) 0.012(2) N01' 0.063(3) 0.047(3) 0.036(2) 0.0014(19) -0.0016(19) 0.006(2) N02' 0.106(4) 0.079(3) 0.040(3) 0.004(2) 0.000(2) 0.026(3) N01" 0.043(2) 0.066(3) 0.049(2) 0.009(2) 0.0029(19) -0.005(2) N02" 0.067(3) 0.075(3) 0.063(3) 0.017(2) -0.018(2) -0.022(2) O 0.0454(19) 0.065(2) 0.0381(18) 0.0104(15) 0.0034(13) -0.0001(15) C2 0.063(3) 0.061(4) 0.052(3) -0.016(3) 0.000(2) 0.007(3) C3 0.216(8) 0.096(6) 0.080(5) -0.041(4) -0.050(5) 0.063(5) C4 0.236(9) 0.130(7) 0.087(6) -0.064(5) -0.058(6) 0.070(6) C5 0.112(5) 0.133(7) 0.070(5) -0.049(5) -0.005(4) 0.026(5) C6 0.127(6) 0.160(7) 0.056(4) -0.025(4) -0.024(4) 0.068(5) C2' 0.051(3) 0.049(3) 0.041(3) 0.002(2) 0.001(2) 0.004(2) C3' 0.057(3) 0.046(3) 0.047(3) -0.002(3) 0.005(2) 0.004(2) C4' 0.045(3) 0.039(3) 0.042(3) 0.006(2) 0.003(2) 0.002(2) C5' 0.052(3) 0.054(3) 0.029(3) 0.004(2) 0.001(2) -0.003(2) C6' 0.041(2) 0.045(3) 0.037(3) 0.003(2) 0.0058(19) -0.001(2) C2" 0.045(3) 0.043(3) 0.041(3) -0.001(2) -0.001(2) -0.005(2) C3" 0.078(4) 0.055(4) 0.054(3) -0.005(3) -0.015(3) 0.012(3) C4" 0.110(5) 0.058(4) 0.061(4) -0.017(3) -0.009(3) 0.012(3) C5" 0.091(4) 0.045(3) 0.068(4) -0.006(3) -0.012(3) 0.013(3) C6" 0.076(4) 0.048(4) 0.064(4) 0.002(3) -0.014(3) 0.007(3) C1"' 0.047(2) 0.047(3) 0.038(3) 0.009(3) 0.0064(19) 0.004(2) C6"' 0.085(4) 0.059(4) 0.047(3) -0.004(3) -0.002(3) 0.017(3) C5"' 0.091(4) 0.059(4) 0.059(4) 0.008(3) 0.004(3) 0.029(3) C4"' 0.052(3) 0.057(4) 0.040(3) 0.014(3) 0.010(2) 0.015(2) C3"' 0.059(3) 0.065(4) 0.038(3) 0.007(3) 0.003(2) 0.001(3) C2"' 0.060(3) 0.044(3) 0.041(3) 0.008(2) 0.004(2) 0.005(2) C7 0.056(3) 0.088(4) 0.045(3) 0.018(3) 0.012(2) 0.017(3) C01 0.049(3) 0.046(3) 0.039(3) 0.001(2) 0.003(2) 0.000(2) C02 0.045(3) 0.048(3) 0.035(3) 0.007(2) 0.000(2) 0.000(2) C03 0.097(4) 0.046(4) 0.060(4) 0.004(3) 0.005(3) 0.009(3) C04 0.097(4) 0.042(4) 0.086(4) -0.006(3) -0.002(3) -0.014(3) C05 0.061(3) 0.071(4) 0.073(4) -0.010(3) -0.014(3) -0.002(3) C03' 0.106(5) 0.075(4) 0.036(3) 0.009(3) -0.009(3) 0.000(3) C04' 0.069(4) 0.064(4) 0.062(4) 0.024(3) -0.011(3) 0.003(3) C05' 0.053(3) 0.050(3) 0.056(3) 0.013(3) 0.000(2) 0.000(2) C03" 0.059(4) 0.112(6) 0.089(5) 0.053(4) -0.020(3) -0.035(4) C04" 0.056(4) 0.124(6) 0.117(6) 0.047(5) 0.023(4) -0.005(4) C05" 0.059(4) 0.104(5) 0.098(5) 0.006(4) 0.027(3) -0.003(4) B 0.090(6) 0.082(7) 0.058(6) 0.009(5) -0.015(5) 0.016(5) F1A 0.133(11) 0.086(8) 0.201(16) -0.015(9) 0.075(9) 0.046(7) F2A 0.239(15) 0.220(17) 0.080(7) 0.057(7) 0.092(9) 0.102(12) F3A 0.135(10) 0.257(15) 0.053(8) -0.004(7) -0.026(5) -0.014(7) F4A 0.168(12) 0.153(17) 0.219(19) 0.075(13) -0.074(10) -0.051(10) F1B 0.63(3) 0.169(13) 0.042(7) -0.007(7) -0.046(11) -0.003(16) F2B 0.150(10) 0.075(7) 0.100(7) 0.031(5) -0.030(6) 0.029(6) F3B 0.337(19) 0.037(8) 0.092(9) -0.042(6) -0.067(10) 0.058(9) F4B 0.117(9) 0.226(16) 0.45(3) -0.120(19) -0.069(15) 0.069(9) _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 Ag N02 2.236(4) 3_657 ? Ag N1' 2.329(3) . ? Ag N1" 2.372(4) . ? Ag N1 2.586(4) . ? N1 C2 1.302(6) . ? N1 C6 1.340(7) . ? N1' C2' 1.342(5) . ? N1' C6' 1.350(5) . ? N1" C6" 1.342(5) . ? N1" C2" 1.348(5) . ? N01 C05 1.343(5) . ? N01 N02 1.349(4) . ? N01 C02 1.478(5) . ? N02 C03 1.339(6) . ? N02 Ag 2.236(4) 3_657 ? N01' C05' 1.340(5) . ? N01' N02' 1.361(5) . ? N01' C02 1.456(5) . ? N02' C03' 1.331(6) . ? N01" C05" 1.342(6) . ? N01" N02" 1.354(5) . ? N01" C02 1.446(5) . ? N02" C03" 1.340(7) . ? O C01 1.411(4) . ? O C7 1.438(5) . ? C2 C3 1.361(7) . ? C2 C2' 1.497(6) . ? C3 C4 1.376(8) . ? C3 H3 0.9300 . ? C4 C5 1.338(8) . ? C4 H4 0.9300 . ? C5 C6 1.336(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C2' C3' 1.378(5) . ? C3' C4' 1.391(5) . ? C3' H3' 0.9300 . ? C4' C5' 1.390(6) . ? C4' C1"' 1.493(5) . ? C5' C6' 1.389(5) . ? C5' H5' 0.9300 . ? C6' C2" 1.497(6) . ? C2" C3" 1.373(6) . ? C3" C4" 1.377(6) . ? C3" H3" 0.9300 . ? C4" C5" 1.362(6) . ? C4" H4" 0.9300 . ? C5" C6" 1.358(6) . ? C5" H5" 0.9300 . ? C6" H6" 0.9300 . ? C1"' C6"' 1.382(6) . ? C1"' C2"' 1.383(6) . ? C6"' C5"' 1.383(6) . ? C6"' H6"' 0.9300 . ? C5"' C4"' 1.365(6) . ? C5"' H5"' 0.9300 . ? C4"' C3"' 1.374(6) . ? C4"' C7 1.518(6) . ? C3"' C2"' 1.382(5) . ? C3"' H3"' 0.9300 . ? C2"' H2"' 0.9300 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C01 C02 1.529(5) . ? C01 H01A 0.9700 . ? C01 H01B 0.9700 . ? C03 C04 1.373(6) . ? C03 H03 0.9300 . ? C04 C05 1.365(6) . ? C04 H04 0.9300 . ? C05 H05 0.9300 . ? C03' C04' 1.371(7) . ? C03' H03' 0.9300 . ? C04' C05' 1.359(6) . ? C04' H04' 0.9300 . ? C05' H05' 0.9300 . ? C03" C04" 1.358(8) . ? C03" H03" 0.9300 . ? C04" C05" 1.347(7) . ? C04" H04" 0.9300 . ? C05" H05" 0.9300 . ? B F4A 1.315(2) . ? B F4B 1.315(2) . ? B F1B 1.316(2) . ? B F3A 1.316(2) . ? B F1A 1.316(2) . ? B F2B 1.316(2) . ? B F3B 1.316(2) . ? B F2A 1.316(2) . ? 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 N02 Ag N1' 144.67(14) 3_657 . ? N02 Ag N1" 137.33(13) 3_657 . ? N1' Ag N1" 70.27(13) . . ? N02 Ag N1 89.31(14) 3_657 . ? N1' Ag N1 66.16(14) . . ? N1" Ag N1 133.25(14) . . ? C2 N1 C6 117.2(5) . . ? C2 N1 Ag 114.6(3) . . ? C6 N1 Ag 126.3(4) . . ? C2' N1' C6' 118.2(3) . . ? C2' N1' Ag 123.2(3) . . ? C6' N1' Ag 118.4(3) . . ? C6" N1" C2" 117.6(4) . . ? C6" N1" Ag 125.0(3) . . ? C2" N1" Ag 116.1(3) . . ? C05 N01 N02 111.7(4) . . ? C05 N01 C02 127.5(4) . . ? N02 N01 C02 119.6(3) . . ? C03 N02 N01 104.2(4) . . ? C03 N02 Ag 122.5(3) . 3_657 ? N01 N02 Ag 133.3(3) . 3_657 ? C05' N01' N02' 112.5(4) . . ? C05' N01' C02 129.8(4) . . ? N02' N01' C02 117.3(4) . . ? C03' N02' N01' 102.8(4) . . ? C05" N01" N02" 111.9(4) . . ? C05" N01" C02 128.0(5) . . ? N02" N01" C02 120.0(4) . . ? C03" N02" N01" 103.2(5) . . ? C01 O C7 112.5(3) . . ? N1 C2 C3 121.5(5) . . ? N1 C2 C2' 117.3(5) . . ? C3 C2 C2' 121.1(5) . . ? C2 C3 C4 119.5(6) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C5 C4 C3 119.3(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 117.3(6) . . ? C4 C5 H5 121.3 . . ? C6 C5 H5 121.3 . . ? C5 C6 N1 124.9(6) . . ? C5 C6 H6 117.5 . . ? N1 C6 H6 117.5 . . ? N1' C2' C3' 122.0(4) . . ? N1' C2' C2 116.2(4) . . ? C3' C2' C2 121.8(4) . . ? C2' C3' C4' 120.9(4) . . ? C2' C3' H3' 119.5 . . ? C4' C3' H3' 119.5 . . ? C5' C4' C3' 116.6(4) . . ? C5' C4' C1"' 121.2(4) . . ? C3' C4' C1"' 122.2(4) . . ? C4' C5' C6' 120.2(4) . . ? C4' C5' H5' 119.9 . . ? C6' C5' H5' 119.9 . . ? N1' C6' C5' 122.1(4) . . ? N1' C6' C2" 116.0(4) . . ? C5' C6' C2" 121.9(4) . . ? N1" C2" C3" 120.6(4) . . ? N1" C2" C6' 117.2(4) . . ? C3" C2" C6' 122.1(4) . . ? C2" C3" C4" 120.3(4) . . ? C2" C3" H3" 119.9 . . ? C4" C3" H3" 119.9 . . ? C5" C4" C3" 119.1(5) . . ? C5" C4" H4" 120.4 . . ? C3" C4" H4" 120.4 . . ? C6" C5" C4" 118.1(5) . . ? C6" C5" H5" 121.0 . . ? C4" C5" H5" 121.0 . . ? N1" C6" C5" 124.2(4) . . ? N1" C6" H6" 117.9 . . ? C5" C6" H6" 117.9 . . ? C6"' C1"' C2"' 116.9(4) . . ? C6"' C1"' C4' 120.7(4) . . ? C2"' C1"' C4' 122.5(4) . . ? C1"' C6"' C5"' 121.1(4) . . ? C1"' C6"' H6"' 119.5 . . ? C5"' C6"' H6"' 119.5 . . ? C4"' C5"' C6"' 121.8(5) . . ? C4"' C5"' H5"' 119.1 . . ? C6"' C5"' H5"' 119.1 . . ? C5"' C4"' C3"' 117.5(4) . . ? C5"' C4"' C7 121.0(5) . . ? C3"' C4"' C7 121.5(4) . . ? C4"' C3"' C2"' 121.3(4) . . ? C4"' C3"' H3"' 119.4 . . ? C2"' C3"' H3"' 119.4 . . ? C3"' C2"' C1"' 121.5(4) . . ? C3"' C2"' H2"' 119.3 . . ? C1"' C2"' H2"' 119.3 . . ? O C7 C4"' 113.0(4) . . ? O C7 H7A 109.0 . . ? C4"' C7 H7A 109.0 . . ? O C7 H7B 109.0 . . ? C4"' C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? O C01 C02 108.5(3) . . ? O C01 H01A 110.0 . . ? C02 C01 H01A 110.0 . . ? O C01 H01B 110.0 . . ? C02 C01 H01B 110.0 . . ? H01A C01 H01B 108.4 . . ? N01" C02 N01' 110.5(3) . . ? N01" C02 N01 107.4(3) . . ? N01' C02 N01 107.4(3) . . ? N01" C02 C01 110.3(4) . . ? N01' C02 C01 111.7(3) . . ? N01 C02 C01 109.4(3) . . ? N02 C03 C04 111.7(5) . . ? N02 C03 H03 124.1 . . ? C04 C03 H03 124.1 . . ? C05 C04 C03 105.2(5) . . ? C05 C04 H04 127.4 . . ? C03 C04 H04 127.4 . . ? N01 C05 C04 107.1(5) . . ? N01 C05 H05 126.4 . . ? C04 C05 H05 126.4 . . ? N02' C03' C04' 112.8(5) . . ? N02' C03' H03' 123.6 . . ? C04' C03' H03' 123.6 . . ? C05' C04' C03' 105.3(4) . . ? C05' C04' H04' 127.3 . . ? C03' C04' H04' 127.3 . . ? N01' C05' C04' 106.6(4) . . ? N01' C05' H05' 126.7 . . ? C04' C05' H05' 126.7 . . ? N02" C03" C04" 112.1(6) . . ? N02" C03" H03" 123.9 . . ? C04" C03" H03" 123.9 . . ? C05" C04" C03" 105.9(6) . . ? C05" C04" H04" 127.0 . . ? C03" C04" H04" 127.0 . . ? N01" C05" C04" 106.9(6) . . ? N01" C05" H05" 126.5 . . ? C04" C05" H05" 126.5 . . ? F4A B F4B 130.7(9) . . ? F4A B F1B 92.9(8) . . ? F4B B F1B 109.49(10) . . ? F4A B F3A 109.50(10) . . ? F4B B F3A 73.6(7) . . ? F1B B F3A 37.2(7) . . ? F4A B F1A 109.51(10) . . ? F4B B F1A 115.5(10) . . ? F1B B F1A 85.3(8) . . ? F3A B F1A 109.47(10) . . ? F4A B F2B 102.9(10) . . ? F4B B F2B 109.45(10) . . ? F1B B F2B 109.45(10) . . ? F3A B F2B 132.5(8) . . ? F1A B F2B 24.6(8) . . ? F4A B F3B 22.3(8) . . ? F4B B F3B 109.49(10) . . ? F1B B F3B 109.46(10) . . ? F3A B F3B 113.7(9) . . ? F1A B F3B 124.1(9) . . ? F2B B F3B 109.49(10) . . ? F4A B F2A 109.50(10) . . ? F4B B F2A 36.6(7) . . ? F1B B F2A 146.1(7) . . ? F3A B F2A 109.42(10) . . ? F1A B F2A 109.43(10) . . ? F2B B F2A 90.6(8) . . ? F3B B F2A 87.9(8) . . ? 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 N02 Ag N1 C2 139.9(4) 3_657 . . . ? N1' Ag N1 C2 -13.9(4) . . . . ? N1" Ag N1 C2 -36.6(5) . . . . ? N02 Ag N1 C6 -23.6(6) 3_657 . . . ? N1' Ag N1 C6 -177.5(6) . . . . ? N1" Ag N1 C6 159.8(5) . . . . ? N02 Ag N1' C2' -38.2(4) 3_657 . . . ? N1" Ag N1' C2' 174.1(4) . . . . ? N1 Ag N1' C2' 11.5(3) . . . . ? N02 Ag N1' C6' 136.5(3) 3_657 . . . ? N1" Ag N1' C6' -11.1(3) . . . . ? N1 Ag N1' C6' -173.7(3) . . . . ? N02 Ag N1" C6" 26.6(5) 3_657 . . . ? N1' Ag N1" C6" 179.4(4) . . . . ? N1 Ag N1" C6" -158.5(4) . . . . ? N02 Ag N1" C2" -140.5(3) 3_657 . . . ? N1' Ag N1" C2" 12.3(3) . . . . ? N1 Ag N1" C2" 34.4(4) . . . . ? C05 N01 N02 C03 1.4(5) . . . . ? C02 N01 N02 C03 169.5(4) . . . . ? C05 N01 N02 Ag -179.1(3) . . . 3_657 ? C02 N01 N02 Ag -11.0(5) . . . 3_657 ? C05' N01' N02' C03' -0.8(5) . . . . ? C02 N01' N02' C03' 173.0(4) . . . . ? C05" N01" N02" C03" 0.7(5) . . . . ? C02 N01" N02" C03" 178.2(4) . . . . ? C6 N1 C2 C3 -1.7(9) . . . . ? Ag N1 C2 C3 -166.8(5) . . . . ? C6 N1 C2 C2' -179.7(5) . . . . ? Ag N1 C2 C2' 15.2(6) . . . . ? N1 C2 C3 C4 1.0(11) . . . . ? C2' C2 C3 C4 178.9(7) . . . . ? C2 C3 C4 C5 2.4(13) . . . . ? C3 C4 C5 C6 -4.8(13) . . . . ? C4 C5 C6 N1 4.3(12) . . . . ? C2 N1 C6 C5 -1.0(11) . . . . ? Ag N1 C6 C5 162.2(6) . . . . ? C6' N1' C2' C3' -2.7(6) . . . . ? Ag N1' C2' C3' 172.1(3) . . . . ? C6' N1' C2' C2 176.7(4) . . . . ? Ag N1' C2' C2 -8.5(5) . . . . ? N1 C2 C2' N1' -5.9(6) . . . . ? C3 C2 C2' N1' 176.1(5) . . . . ? N1 C2 C2' C3' 173.5(5) . . . . ? C3 C2 C2' C3' -4.5(8) . . . . ? N1' C2' C3' C4' 0.2(7) . . . . ? C2 C2' C3' C4' -179.1(4) . . . . ? C2' C3' C4' C5' 1.3(6) . . . . ? C2' C3' C4' C1"' -178.7(4) . . . . ? C3' C4' C5' C6' -0.4(6) . . . . ? C1"' C4' C5' C6' 179.7(4) . . . . ? C2' N1' C6' C5' 3.7(6) . . . . ? Ag N1' C6' C5' -171.4(3) . . . . ? C2' N1' C6' C2" -176.1(4) . . . . ? Ag N1' C6' C2" 8.9(4) . . . . ? C4' C5' C6' N1' -2.1(6) . . . . ? C4' C5' C6' C2" 177.6(4) . . . . ? C6" N1" C2" C3" -0.3(6) . . . . ? Ag N1" C2" C3" 167.8(3) . . . . ? C6" N1" C2" C6' 179.4(4) . . . . ? Ag N1" C2" C6' -12.6(5) . . . . ? N1' C6' C2" N1" 2.7(5) . . . . ? C5' C6' C2" N1" -177.0(4) . . . . ? N1' C6' C2" C3" -177.6(4) . . . . ? C5' C6' C2" C3" 2.6(6) . . . . ? N1" C2" C3" C4" -1.1(7) . . . . ? C6' C2" C3" C4" 179.3(4) . . . . ? C2" C3" C4" C5" 1.4(8) . . . . ? C3" C4" C5" C6" -0.4(8) . . . . ? C2" N1" C6" C5" 1.4(7) . . . . ? Ag N1" C6" C5" -165.5(4) . . . . ? C4" C5" C6" N1" -1.0(8) . . . . ? C5' C4' C1"' C6"' -170.7(4) . . . . ? C3' C4' C1"' C6"' 9.4(6) . . . . ? C5' C4' C1"' C2"' 8.7(6) . . . . ? C3' C4' C1"' C2"' -171.2(4) . . . . ? C2"' C1"' C6"' C5"' -1.4(7) . . . . ? C4' C1"' C6"' C5"' 178.1(4) . . . . ? C1"' C6"' C5"' C4"' 0.9(8) . . . . ? C6"' C5"' C4"' C3"' 0.4(7) . . . . ? C6"' C5"' C4"' C7 -179.3(4) . . . . ? C5"' C4"' C3"' C2"' -1.2(6) . . . . ? C7 C4"' C3"' C2"' 178.4(4) . . . . ? C4"' C3"' C2"' C1"' 0.8(6) . . . . ? C6"' C1"' C2"' C3"' 0.5(6) . . . . ? C4' C1"' C2"' C3"' -178.9(4) . . . . ? C01 O C7 C4"' -63.4(5) . . . . ? C5"' C4"' C7 O 134.4(4) . . . . ? C3"' C4"' C7 O -45.2(6) . . . . ? C7 O C01 C02 164.5(3) . . . . ? C05" N01" C02 N01' -79.5(6) . . . . ? N02" N01" C02 N01' 103.5(4) . . . . ? C05" N01" C02 N01 37.4(6) . . . . ? N02" N01" C02 N01 -139.7(4) . . . . ? C05" N01" C02 C01 156.5(4) . . . . ? N02" N01" C02 C01 -20.5(5) . . . . ? C05' N01' C02 N01" -133.1(5) . . . . ? N02' N01' C02 N01" 54.4(5) . . . . ? C05' N01' C02 N01 110.1(5) . . . . ? N02' N01' C02 N01 -62.4(5) . . . . ? C05' N01' C02 C01 -9.9(6) . . . . ? N02' N01' C02 C01 177.6(4) . . . . ? C05 N01 C02 N01" -144.3(4) . . . . ? N02 N01 C02 N01" 49.7(5) . . . . ? C05 N01 C02 N01' -25.4(6) . . . . ? N02 N01 C02 N01' 168.5(3) . . . . ? C05 N01 C02 C01 96.1(5) . . . . ? N02 N01 C02 C01 -70.0(4) . . . . ? O C01 C02 N01" -166.6(3) . . . . ? O C01 C02 N01' 70.1(4) . . . . ? O C01 C02 N01 -48.7(4) . . . . ? N01 N02 C03 C04 -1.0(5) . . . . ? Ag N02 C03 C04 179.4(3) 3_657 . . . ? N02 C03 C04 C05 0.3(6) . . . . ? N02 N01 C05 C04 -1.3(5) . . . . ? C02 N01 C05 C04 -168.2(4) . . . . ? C03 C04 C05 N01 0.6(6) . . . . ? N01' N02' C03' C04' 0.7(6) . . . . ? N02' C03' C04' C05' -0.4(6) . . . . ? N02' N01' C05' C04' 0.6(5) . . . . ? C02 N01' C05' C04' -172.2(4) . . . . ? C03' C04' C05' N01' -0.1(5) . . . . ? N01" N02" C03" C04" -0.8(6) . . . . ? N02" C03" C04" C05" 0.6(7) . . . . ? N02" N01" C05" C04" -0.4(6) . . . . ? C02 N01" C05" C04" -177.7(4) . . . . ? C03" C04" C05" N01" -0.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.311 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.063 #====END data_[Cu(PzT)(NO3)2].CH3CN _database_code_depnum_ccdc_archive 'CCDC 277289' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C33 H27 Cu N11 O7, C2 H3 N ; _chemical_formula_sum 'C35 H30 Cu N12 O7' _chemical_formula_weight 794.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8307(7) _cell_length_b 11.8013(9) _cell_length_c 17.3963(13) _cell_angle_alpha 88.3580(10) _cell_angle_beta 79.6760(10) _cell_angle_gamma 83.2590(10) _cell_volume 1771.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 168(2) _cell_measurement_reflns_used 7466 _cell_measurement_theta_min 4.719 _cell_measurement_theta_max 54.921 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 818 _exptl_absorpt_coefficient_mu 0.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5937 _exptl_absorpt_correction_T_max 0.9347 _exptl_absorpt_process_details 'SADABS V2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 168(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 SMART/CCD _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20709 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_sigmaI/netI 0.0160 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6267 _reflns_number_gt 5586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker XPREP' _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^)+(0.0590P)^2^+1.1377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6267 _refine_ls_number_parameters 516 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0353 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0995 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.003 _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 Cu Cu 0.62838(3) 0.70164(2) 1.124601(15) 0.02737(10) Uani 1 1 d . . . N1' N 0.53048(19) 0.73464(14) 1.03448(10) 0.0246(4) Uani 1 1 d . . . N1" N 0.7204(2) 0.56299(15) 1.05733(11) 0.0273(4) Uani 1 1 d . . . N1 N 0.4973(2) 0.85000(16) 1.15901(11) 0.0294(4) Uani 1 1 d . . . N4 N 0.5701(2) 0.56182(17) 1.25191(11) 0.0364(5) Uani 1 1 d . . . O41 O 0.6617(2) 0.63883(14) 1.22809(9) 0.0365(4) Uani 1 1 d . . . O42 O 0.5894(3) 0.50673(18) 1.31049(12) 0.0576(5) Uani 1 1 d . . . O43 O 0.4695(2) 0.54715(18) 1.21298(11) 0.0502(5) Uani 1 1 d . . . N5 N 0.8926(2) 0.83848(15) 1.07363(11) 0.0291(4) Uani 1 1 d . . . O51 O 0.85186(18) 0.76544(14) 1.12644(9) 0.0337(4) Uani 1 1 d . . . O53 O 1.01959(18) 0.87568(14) 1.07026(11) 0.0390(4) Uani 1 1 d . . . O52 O 0.8050(2) 0.87018(18) 1.02763(12) 0.0559(5) Uani 1 1 d . . . N01 N 0.0791(3) 0.77911(19) 0.38493(12) 0.0430(5) Uani 1 1 d . . . C05 C 0.1605(4) 0.7865(3) 0.31140(16) 0.0523(7) Uani 1 1 d . . . H05 H 0.2676 0.7825 0.2971 0.063 Uiso 1 1 calc R . . C04 C 0.0556(4) 0.8009(3) 0.26259(17) 0.0539(7) Uani 1 1 d . . . H04 H 0.0749 0.8099 0.2086 0.065 Uiso 1 1 calc R . . C03 C -0.0863(4) 0.7993(3) 0.31109(18) 0.0574(8) Uani 1 1 d . . . H03 H -0.1803 0.8065 0.2934 0.069 Uiso 1 1 calc R . . N02 N -0.0734(3) 0.7863(2) 0.38564(13) 0.0487(6) Uani 1 1 d . . . N01' N 0.2885(3) 0.8012(2) 0.44769(14) 0.0489(6) Uani 1 1 d . . . C05' C 0.4318(4) 0.7477(3) 0.4476(2) 0.0608(8) Uani 1 1 d . . . H05' H 0.4592 0.6696 0.4518 0.073 Uiso 1 1 calc R . . C04' C 0.5286(4) 0.8303(4) 0.4403(2) 0.0728(10) Uani 1 1 d . . . H04' H 0.6352 0.8207 0.4385 0.087 Uiso 1 1 calc R . . C03' C 0.4341(4) 0.9322(4) 0.43588(19) 0.0699(10) Uani 1 1 d . . . H03' H 0.4706 1.0033 0.4302 0.084 Uiso 1 1 calc R . . N02' N 0.2854(3) 0.9170(2) 0.44064(16) 0.0623(7) Uani 1 1 d . . . N01" N 0.1703(3) 0.6311(2) 0.46678(13) 0.0460(5) Uani 1 1 d . . . C05" C 0.1654(4) 0.5688(3) 0.53298(19) 0.0618(8) Uani 1 1 d . . . H05" H 0.1295 0.5953 0.5836 0.074 Uiso 1 1 calc R . . C04" C 0.2229(4) 0.4597(3) 0.5122(2) 0.0673(9) Uani 1 1 d . . . H04" H 0.2338 0.3969 0.5451 0.081 Uiso 1 1 calc R . . C03" C 0.2615(4) 0.4624(3) 0.4320(2) 0.0700(9) Uani 1 1 d . . . H03" H 0.3046 0.3990 0.4018 0.084 Uiso 1 1 calc R . . N02" N 0.2302(4) 0.5660(3) 0.40265(17) 0.0692(8) Uani 1 1 d . . . C2' C 0.4303(2) 0.82983(17) 1.03384(12) 0.0246(4) Uani 1 1 d . . . C3' C 0.3582(2) 0.85653(18) 0.97054(12) 0.0252(4) Uani 1 1 d . . . H3' H 0.2892 0.9225 0.9707 0.030 Uiso 1 1 calc R . . C4' C 0.3895(2) 0.78336(18) 0.90581(12) 0.0254(4) Uani 1 1 d . . . C5' C 0.4962(2) 0.68540(18) 0.90818(12) 0.0255(4) Uani 1 1 d . . . H5' H 0.5207 0.6356 0.8661 0.031 Uiso 1 1 calc R . . C6' C 0.5640(2) 0.66390(17) 0.97329(12) 0.0247(4) Uani 1 1 d . . . C2" C 0.6762(2) 0.56396(17) 0.98677(12) 0.0249(4) Uani 1 1 d . . . C3" C 0.7306(2) 0.47735(19) 0.93310(13) 0.0289(5) Uani 1 1 d . . . H3" H 0.6985 0.4793 0.8849 0.035 Uiso 1 1 calc R . . C4" C 0.8338(2) 0.38769(19) 0.95269(14) 0.0309(5) Uani 1 1 d . . . H4" H 0.8720 0.3288 0.9176 0.037 Uiso 1 1 calc R . . C5" C 0.8791(3) 0.38683(19) 1.02486(14) 0.0318(5) Uani 1 1 d . . . H5" H 0.9482 0.3276 1.0389 0.038 Uiso 1 1 calc R . . C6" C 0.8200(2) 0.47529(19) 1.07566(14) 0.0308(5) Uani 1 1 d . . . H6" H 0.8501 0.4744 1.1243 0.037 Uiso 1 1 calc R . . C2 C 0.4125(2) 0.89738(18) 1.10634(12) 0.0254(4) Uani 1 1 d . . . C3 C 0.3219(3) 1.00149(19) 1.11902(13) 0.0313(5) Uani 1 1 d . . . H3 H 0.2629 1.0317 1.0825 0.038 Uiso 1 1 calc R . . C4 C 0.3210(3) 1.0599(2) 1.18737(14) 0.0364(5) Uani 1 1 d . . . H4 H 0.2620 1.1303 1.1971 0.044 Uiso 1 1 calc R . . C5 C 0.4090(3) 1.0120(2) 1.24069(14) 0.0380(5) Uani 1 1 d . . . H5 H 0.4109 1.0503 1.2864 0.046 Uiso 1 1 calc R . . C6 C 0.4942(3) 0.9067(2) 1.22541(14) 0.0350(5) Uani 1 1 d . . . H6 H 0.5511 0.8740 1.2621 0.042 Uiso 1 1 calc R . . C1"' C 0.3098(2) 0.80869(18) 0.83811(13) 0.0274(4) Uani 1 1 d . . . C2"' C 0.3685(3) 0.7594(2) 0.76488(14) 0.0370(5) Uani 1 1 d . . . H2"' H 0.4588 0.7088 0.7585 0.044 Uiso 1 1 calc R . . C3"' C 0.2942(3) 0.7847(2) 0.70227(15) 0.0435(6) Uani 1 1 d . . . H3"' H 0.3352 0.7511 0.6542 0.052 Uiso 1 1 calc R . . C4"' C 0.1584(3) 0.8600(2) 0.70999(15) 0.0412(6) Uani 1 1 d . . . C5"' C 0.1002(3) 0.9090(2) 0.78225(15) 0.0390(6) Uani 1 1 d . . . H5"' H 0.0104 0.9601 0.7881 0.047 Uiso 1 1 calc R . . C6"' C 0.1724(3) 0.88372(19) 0.84563(14) 0.0319(5) Uani 1 1 d . . . H6"' H 0.1298 0.9166 0.8938 0.038 Uiso 1 1 calc R . . C7 C 0.0745(4) 0.8882(3) 0.64208(18) 0.0590(8) Uani 1 1 d . . . H7A H -0.0356 0.9058 0.6614 0.071 Uiso 1 1 calc R . . H7B H 0.1120 0.9546 0.6142 0.071 Uiso 1 1 calc R . . O O 0.0992(3) 0.79703(19) 0.59247(12) 0.0670(6) Uani 1 1 d . . . C01 C 0.0274(3) 0.8094(3) 0.52611(16) 0.0507(7) Uani 1 1 d . . . H01A H 0.0010 0.8896 0.5152 0.061 Uiso 1 1 calc R . . H01B H -0.0670 0.7728 0.5353 0.061 Uiso 1 1 calc R . . C02 C 0.1404(3) 0.7539(2) 0.45678(15) 0.0424(6) Uani 1 1 d . . . C8 C 0.9979(5) 0.4882(4) 0.7309(2) 0.0809(11) Uani 0.50 1 d PD A 1 H8A H 1.0004 0.4301 0.7706 0.121 Uiso 0.50 1 calc PR A 1 H8B H 1.1016 0.4956 0.7046 0.121 Uiso 0.50 1 calc PR A 1 H8C H 0.9375 0.4676 0.6939 0.121 Uiso 0.50 1 calc PR A 1 C9 C 0.928(2) 0.5982(16) 0.7674(10) 0.074(5) Uani 0.50 1 d PD A 1 N6 N 0.8768(14) 0.6731(7) 0.8012(8) 0.124(5) Uani 0.50 1 d PD A 1 C8' C 0.9979(5) 0.4882(4) 0.7309(2) 0.0809(11) Uani 0.50 1 d P B 2 H8'A H 1.0683 0.4833 0.7673 0.121 Uiso 0.50 1 calc PR B 2 H8'B H 1.0556 0.4853 0.6786 0.121 Uiso 0.50 1 calc PR B 2 H8'C H 0.9367 0.4255 0.7395 0.121 Uiso 0.50 1 calc PR B 2 C9' C 0.8952(18) 0.5967(14) 0.7422(9) 0.063(4) Uani 0.50 1 d PD B 2 N6' N 0.8136(10) 0.6756(7) 0.7529(7) 0.098(3) Uani 0.50 1 d PD B 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 Cu 0.02839(16) 0.02787(16) 0.02640(16) -0.00218(11) -0.00964(11) 0.00243(11) N1' 0.0235(9) 0.0226(9) 0.0272(9) -0.0021(7) -0.0045(7) 0.0006(7) N1" 0.0253(9) 0.0261(9) 0.0306(10) 0.0006(7) -0.0080(7) 0.0007(7) N1 0.0283(9) 0.0330(10) 0.0274(9) -0.0033(8) -0.0069(7) -0.0017(8) N4 0.0427(11) 0.0339(11) 0.0300(10) -0.0027(8) -0.0020(9) 0.0002(9) O41 0.0438(9) 0.0376(9) 0.0311(8) 0.0055(7) -0.0126(7) -0.0086(7) O42 0.0743(14) 0.0530(12) 0.0436(11) 0.0185(9) -0.0081(10) -0.0077(10) O43 0.0470(11) 0.0624(13) 0.0446(11) -0.0064(9) -0.0085(9) -0.0185(9) N5 0.0296(10) 0.0222(9) 0.0344(10) -0.0011(8) -0.0059(8) 0.0022(7) O51 0.0304(8) 0.0378(9) 0.0338(9) 0.0074(7) -0.0086(7) -0.0051(7) O53 0.0297(9) 0.0312(9) 0.0551(11) 0.0029(8) -0.0051(8) -0.0043(7) O52 0.0530(12) 0.0615(13) 0.0617(13) 0.0317(10) -0.0322(10) -0.0154(10) N01 0.0462(12) 0.0514(13) 0.0359(12) 0.0060(10) -0.0172(10) -0.0108(10) C05 0.0556(17) 0.0665(19) 0.0382(15) 0.0076(13) -0.0105(13) -0.0200(15) C04 0.075(2) 0.0581(18) 0.0342(14) 0.0054(12) -0.0217(14) -0.0153(15) C03 0.0625(19) 0.0653(19) 0.0536(18) 0.0039(15) -0.0365(16) -0.0057(15) N02 0.0411(12) 0.0652(15) 0.0421(13) 0.0015(11) -0.0183(10) 0.0005(11) N01' 0.0493(13) 0.0567(15) 0.0469(13) 0.0047(11) -0.0212(11) -0.0135(11) C05' 0.0439(16) 0.078(2) 0.063(2) 0.0029(17) -0.0177(14) -0.0059(15) C04' 0.0511(19) 0.105(3) 0.070(2) 0.001(2) -0.0195(17) -0.024(2) C03' 0.082(2) 0.088(3) 0.0534(19) 0.0095(18) -0.0284(17) -0.044(2) N02' 0.0745(18) 0.0616(17) 0.0618(16) 0.0081(13) -0.0324(14) -0.0242(14) N01" 0.0456(12) 0.0515(13) 0.0425(12) 0.0050(10) -0.0137(10) -0.0038(10) C05" 0.072(2) 0.061(2) 0.0503(18) 0.0151(15) -0.0094(15) -0.0052(16) C04" 0.075(2) 0.0524(19) 0.074(2) 0.0191(17) -0.0182(18) -0.0049(16) C03" 0.075(2) 0.055(2) 0.079(2) -0.0013(17) -0.0150(19) 0.0016(17) N02" 0.087(2) 0.0614(17) 0.0565(17) -0.0046(13) -0.0123(15) 0.0027(15) C2' 0.0215(10) 0.0232(10) 0.0282(11) 0.0000(8) -0.0025(8) -0.0015(8) C3' 0.0230(10) 0.0227(10) 0.0285(11) 0.0007(8) -0.0035(8) 0.0009(8) C4' 0.0224(10) 0.0256(10) 0.0278(11) 0.0015(8) -0.0039(8) -0.0027(8) C5' 0.0250(10) 0.0252(10) 0.0255(10) -0.0031(8) -0.0035(8) -0.0002(8) C6' 0.0220(10) 0.0239(10) 0.0275(11) -0.0011(8) -0.0032(8) -0.0013(8) C2" 0.0214(10) 0.0242(10) 0.0288(11) 0.0008(8) -0.0043(8) -0.0012(8) C3" 0.0265(11) 0.0294(11) 0.0299(11) -0.0019(9) -0.0051(9) 0.0007(9) C4" 0.0271(11) 0.0251(11) 0.0379(13) -0.0034(9) -0.0021(9) 0.0027(9) C5" 0.0249(11) 0.0270(11) 0.0418(13) 0.0039(9) -0.0053(9) 0.0023(9) C6" 0.0270(11) 0.0326(12) 0.0334(12) 0.0043(9) -0.0100(9) 0.0000(9) C2 0.0239(10) 0.0259(11) 0.0262(11) -0.0015(8) -0.0029(8) -0.0037(8) C3 0.0333(12) 0.0281(11) 0.0312(12) 0.0000(9) -0.0044(9) -0.0005(9) C4 0.0429(13) 0.0262(11) 0.0370(13) -0.0049(10) -0.0009(10) -0.0003(10) C5 0.0448(14) 0.0381(13) 0.0314(12) -0.0104(10) -0.0051(10) -0.0057(11) C6 0.0378(13) 0.0392(13) 0.0296(12) -0.0055(10) -0.0099(10) -0.0027(10) C1"' 0.0282(11) 0.0258(11) 0.0285(11) 0.0009(9) -0.0069(9) -0.0017(8) C2"' 0.0369(13) 0.0397(13) 0.0324(12) -0.0037(10) -0.0099(10) 0.0098(10) C3"' 0.0499(15) 0.0492(15) 0.0296(13) -0.0084(11) -0.0120(11) 0.0108(12) C4"' 0.0464(14) 0.0423(14) 0.0362(13) -0.0008(11) -0.0183(11) 0.0064(11) C5"' 0.0375(13) 0.0374(13) 0.0414(14) -0.0016(11) -0.0140(11) 0.0098(10) C6"' 0.0318(12) 0.0314(12) 0.0319(12) -0.0027(9) -0.0083(9) 0.0034(9) C7 0.070(2) 0.0621(19) 0.0457(16) -0.0119(14) -0.0314(15) 0.0230(16) O 0.0951(17) 0.0657(14) 0.0440(12) -0.0059(10) -0.0396(12) 0.0184(12) C01 0.0545(17) 0.0614(18) 0.0376(14) 0.0030(13) -0.0189(12) 0.0034(14) C02 0.0435(14) 0.0496(15) 0.0381(14) 0.0049(11) -0.0178(11) -0.0073(12) C8 0.097(3) 0.079(3) 0.064(2) -0.0188(19) -0.018(2) 0.012(2) C9 0.060(7) 0.056(10) 0.098(13) 0.027(9) -0.003(7) 0.005(6) N6 0.098(7) 0.040(4) 0.204(13) 0.015(6) 0.045(8) 0.003(5) C8' 0.097(3) 0.079(3) 0.064(2) -0.0188(19) -0.018(2) 0.012(2) C9' 0.064(9) 0.048(8) 0.072(8) -0.022(6) 0.009(5) -0.014(7) N6' 0.074(5) 0.064(5) 0.145(9) -0.043(5) 0.006(5) 0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu N1' 1.9310(18) . ? Cu O41 1.9849(16) . ? Cu N1 2.0249(19) . ? Cu N1" 2.0407(18) . ? Cu O51 2.1990(16) . ? N1' C6' 1.341(3) . ? N1' C2' 1.347(3) . ? N1" C6" 1.347(3) . ? N1" C2" 1.352(3) . ? N1 C6 1.346(3) . ? N1 C2 1.353(3) . ? N4 O42 1.220(3) . ? N4 O43 1.239(3) . ? N4 O41 1.298(3) . ? N5 O52 1.231(3) . ? N5 O53 1.243(2) . ? N5 O51 1.275(2) . ? N01 N02 1.337(3) . ? N01 C05 1.356(4) . ? N01 C02 1.458(3) . ? C05 C04 1.358(4) . ? C05 H05 0.9300 . ? C04 C03 1.381(5) . ? C04 H04 0.9300 . ? C03 N02 1.325(4) . ? C03 H03 0.9300 . ? N01' C05' 1.346(4) . ? N01' N02' 1.366(4) . ? N01' C02 1.462(3) . ? C05' C04' 1.359(5) . ? C05' H05' 0.9300 . ? C04' C03' 1.389(6) . ? C04' H04' 0.9300 . ? C03' N02' 1.334(4) . ? C03' H03' 0.9300 . ? N01" C05" 1.346(4) . ? N01" N02" 1.363(4) . ? N01" C02 1.453(4) . ? C05" C04" 1.361(5) . ? C05" H05" 0.9300 . ? C04" C03" 1.375(5) . ? C04" H04" 0.9300 . ? C03" N02" 1.330(4) . ? C03" H03" 0.9300 . ? C2' C3' 1.379(3) . ? C2' C2 1.486(3) . ? C3' C4' 1.407(3) . ? C3' H3' 0.9300 . ? C4' C5' 1.407(3) . ? C4' C1"' 1.483(3) . ? C5' C6' 1.377(3) . ? C5' H5' 0.9300 . ? C6' C2" 1.491(3) . ? C2" C3" 1.388(3) . ? C3" C4" 1.389(3) . ? C3" H3" 0.9300 . ? C4" C5" 1.384(3) . ? C4" H4" 0.9300 . ? C5" C6" 1.379(3) . ? C5" H5" 0.9300 . ? C6" H6" 0.9300 . ? C2 C3 1.386(3) . ? C3 C4 1.390(3) . ? C3 H3 0.9300 . ? C4 C5 1.382(4) . ? C4 H4 0.9300 . ? C5 C6 1.381(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C1"' C2"' 1.402(3) . ? C1"' C6"' 1.404(3) . ? C2"' C3"' 1.377(3) . ? C2"' H2"' 0.9300 . ? C3"' C4"' 1.394(4) . ? C3"' H3"' 0.9300 . ? C4"' C5"' 1.386(4) . ? C4"' C7 1.513(3) . ? C5"' C6"' 1.379(3) . ? C5"' H5"' 0.9300 . ? C6"' H6"' 0.9300 . ? C7 O 1.371(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? O C01 1.410(3) . ? C01 C02 1.529(4) . ? C01 H01A 0.9700 . ? C01 H01B 0.9700 . ? C8 C9 1.48(2) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N6 1.08(2) . ? C9' N6' 1.106(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 N1' Cu O41 159.30(7) . . ? N1' Cu N1 80.07(7) . . ? O41 Cu N1 99.52(7) . . ? N1' Cu N1" 79.60(7) . . ? O41 Cu N1" 99.10(7) . . ? N1 Cu N1" 159.64(7) . . ? N1' Cu O51 118.75(7) . . ? O41 Cu O51 81.94(6) . . ? N1 Cu O51 95.48(7) . . ? N1" Cu O51 95.22(7) . . ? C6' N1' C2' 120.91(18) . . ? C6' N1' Cu 119.99(14) . . ? C2' N1' Cu 119.10(14) . . ? C6" N1" C2" 118.79(19) . . ? C6" N1" Cu 126.87(15) . . ? C2" N1" Cu 114.32(13) . . ? C6 N1 C2 118.68(19) . . ? C6 N1 Cu 126.60(16) . . ? C2 N1 Cu 114.60(14) . . ? O42 N4 O43 123.7(2) . . ? O42 N4 O41 118.3(2) . . ? O43 N4 O41 117.98(19) . . ? N4 O41 Cu 111.06(13) . . ? O52 N5 O53 121.99(19) . . ? O52 N5 O51 119.08(19) . . ? O53 N5 O51 118.93(18) . . ? N5 O51 Cu 115.78(13) . . ? N02 N01 C05 111.9(2) . . ? N02 N01 C02 120.3(2) . . ? C05 N01 C02 127.5(2) . . ? N01 C05 C04 106.9(3) . . ? N01 C05 H05 126.6 . . ? C04 C05 H05 126.6 . . ? C05 C04 C03 104.6(3) . . ? C05 C04 H04 127.7 . . ? C03 C04 H04 127.7 . . ? N02 C03 C04 112.4(3) . . ? N02 C03 H03 123.8 . . ? C04 C03 H03 123.8 . . ? C03 N02 N01 104.2(2) . . ? C05' N01' N02' 112.9(3) . . ? C05' N01' C02 129.7(3) . . ? N02' N01' C02 117.3(2) . . ? N01' C05' C04' 106.6(3) . . ? N01' C05' H05' 126.7 . . ? C04' C05' H05' 126.7 . . ? C05' C04' C03' 105.2(3) . . ? C05' C04' H04' 127.4 . . ? C03' C04' H04' 127.4 . . ? N02' C03' C04' 112.7(3) . . ? N02' C03' H03' 123.6 . . ? C04' C03' H03' 123.6 . . ? C03' N02' N01' 102.6(3) . . ? C05" N01" N02" 111.3(3) . . ? C05" N01" C02 129.4(3) . . ? N02" N01" C02 118.7(2) . . ? N01" C05" C04" 107.3(3) . . ? N01" C05" H05" 126.4 . . ? C04" C05" H05" 126.4 . . ? C05" C04" C03" 105.2(3) . . ? C05" C04" H04" 127.4 . . ? C03" C04" H04" 127.4 . . ? N02" C03" C04" 112.3(3) . . ? N02" C03" H03" 123.9 . . ? C04" C03" H03" 123.9 . . ? C03" N02" N01" 103.9(3) . . ? N1' C2' C3' 120.88(19) . . ? N1' C2' C2 112.23(18) . . ? C3' C2' C2 126.88(19) . . ? C2' C3' C4' 119.57(19) . . ? C2' C3' H3' 120.2 . . ? C4' C3' H3' 120.2 . . ? C3' C4' C5' 117.96(19) . . ? C3' C4' C1"' 120.45(19) . . ? C5' C4' C1"' 121.59(19) . . ? C6' C5' C4' 119.42(19) . . ? C6' C5' H5' 120.3 . . ? C4' C5' H5' 120.3 . . ? N1' C6' C5' 121.26(18) . . ? N1' C6' C2" 111.84(18) . . ? C5' C6' C2" 126.90(19) . . ? N1" C2" C3" 121.83(19) . . ? N1" C2" C6' 114.19(18) . . ? C3" C2" C6' 123.97(19) . . ? C2" C3" C4" 118.7(2) . . ? C2" C3" H3" 120.6 . . ? C4" C3" H3" 120.6 . . ? C5" C4" C3" 119.4(2) . . ? C5" C4" H4" 120.3 . . ? C3" C4" H4" 120.3 . . ? C6" C5" C4" 118.9(2) . . ? C6" C5" H5" 120.5 . . ? C4" C5" H5" 120.5 . . ? N1" C6" C5" 122.3(2) . . ? N1" C6" H6" 118.8 . . ? C5" C6" H6" 118.8 . . ? N1 C2 C3 122.1(2) . . ? N1 C2 C2' 113.98(18) . . ? C3 C2 C2' 123.9(2) . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.1(2) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C6 C5 C4 119.4(2) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? N1 C6 C5 122.0(2) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? C2"' C1"' C6"' 117.9(2) . . ? C2"' C1"' C4' 121.54(19) . . ? C6"' C1"' C4' 120.6(2) . . ? C3"' C2"' C1"' 120.9(2) . . ? C3"' C2"' H2"' 119.5 . . ? C1"' C2"' H2"' 119.5 . . ? C2"' C3"' C4"' 120.9(2) . . ? C2"' C3"' H3"' 119.5 . . ? C4"' C3"' H3"' 119.5 . . ? C5"' C4"' C3"' 118.3(2) . . ? C5"' C4"' C7 120.0(2) . . ? C3"' C4"' C7 121.7(2) . . ? C6"' C5"' C4"' 121.4(2) . . ? C6"' C5"' H5"' 119.3 . . ? C4"' C5"' H5"' 119.3 . . ? C5"' C6"' C1"' 120.5(2) . . ? C5"' C6"' H6"' 119.7 . . ? C1"' C6"' H6"' 119.7 . . ? O C7 C4"' 109.7(2) . . ? O C7 H7A 109.7 . . ? C4"' C7 H7A 109.7 . . ? O C7 H7B 109.7 . . ? C4"' C7 H7B 109.7 . . ? H7A C7 H7B 108.2 . . ? C7 O C01 116.7(2) . . ? O C01 C02 108.3(2) . . ? O C01 H01A 110.0 . . ? C02 C01 H01A 110.0 . . ? O C01 H01B 110.0 . . ? C02 C01 H01B 110.0 . . ? H01A C01 H01B 108.4 . . ? N01" C02 N01 109.6(2) . . ? N01" C02 N01' 107.9(2) . . ? N01 C02 N01' 107.3(2) . . ? N01" C02 C01 112.0(2) . . ? N01 C02 C01 109.8(2) . . ? N01' C02 C01 110.1(2) . . ? N6 C9 C8 172.6(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 O41 Cu N1' C6' -90.1(2) . . . . ? N1 Cu N1' C6' 179.19(17) . . . . ? N1" Cu N1' C6' -1.91(15) . . . . ? O51 Cu N1' C6' 88.37(16) . . . . ? O41 Cu N1' C2' 90.6(2) . . . . ? N1 Cu N1' C2' -0.02(15) . . . . ? N1" Cu N1' C2' 178.87(16) . . . . ? O51 Cu N1' C2' -90.85(16) . . . . ? N1' Cu N1" C6" -179.22(19) . . . . ? O41 Cu N1" C6" -20.18(19) . . . . ? N1 Cu N1" C6" -176.1(2) . . . . ? O51 Cu N1" C6" 62.47(19) . . . . ? N1' Cu N1" C2" 2.28(14) . . . . ? O41 Cu N1" C2" 161.32(15) . . . . ? N1 Cu N1" C2" 5.4(3) . . . . ? O51 Cu N1" C2" -116.03(15) . . . . ? N1' Cu N1 C6 -176.6(2) . . . . ? O41 Cu N1 C6 24.4(2) . . . . ? N1" Cu N1 C6 -179.7(2) . . . . ? O51 Cu N1 C6 -58.3(2) . . . . ? N1' Cu N1 C2 -0.60(15) . . . . ? O41 Cu N1 C2 -159.60(15) . . . . ? N1" Cu N1 C2 -3.7(3) . . . . ? O51 Cu N1 C2 117.68(15) . . . . ? O42 N4 O41 Cu 171.98(17) . . . . ? O43 N4 O41 Cu -6.8(2) . . . . ? N1' Cu O41 N4 13.9(3) . . . . ? N1 Cu O41 N4 100.97(15) . . . . ? N1" Cu O41 N4 -70.75(15) . . . . ? O51 Cu O41 N4 -164.78(15) . . . . ? O52 N5 O51 Cu 2.0(3) . . . . ? O53 N5 O51 Cu -178.17(14) . . . . ? N1' Cu O51 N5 12.00(17) . . . . ? O41 Cu O51 N5 -168.53(15) . . . . ? N1 Cu O51 N5 -69.66(15) . . . . ? N1" Cu O51 N5 92.99(15) . . . . ? N02 N01 C05 C04 1.0(3) . . . . ? C02 N01 C05 C04 174.5(3) . . . . ? N01 C05 C04 C03 -1.0(3) . . . . ? C05 C04 C03 N02 0.8(4) . . . . ? C04 C03 N02 N01 -0.2(4) . . . . ? C05 N01 N02 C03 -0.5(3) . . . . ? C02 N01 N02 C03 -174.5(2) . . . . ? N02' N01' C05' C04' 0.0(4) . . . . ? C02 N01' C05' C04' -177.6(3) . . . . ? N01' C05' C04' C03' -0.2(4) . . . . ? C05' C04' C03' N02' 0.4(4) . . . . ? C04' C03' N02' N01' -0.4(4) . . . . ? C05' N01' N02' C03' 0.3(3) . . . . ? C02 N01' N02' C03' 178.2(2) . . . . ? N02" N01" C05" C04" -0.2(4) . . . . ? C02 N01" C05" C04" -171.8(3) . . . . ? N01" C05" C04" C03" 0.4(4) . . . . ? C05" C04" C03" N02" -0.4(5) . . . . ? C04" C03" N02" N01" 0.3(4) . . . . ? C05" N01" N02" C03" 0.0(4) . . . . ? C02 N01" N02" C03" 172.5(3) . . . . ? C6' N1' C2' C3' 0.7(3) . . . . ? Cu N1' C2' C3' 179.90(15) . . . . ? C6' N1' C2' C2 -178.64(18) . . . . ? Cu N1' C2' C2 0.6(2) . . . . ? N1' C2' C3' C4' 0.0(3) . . . . ? C2 C2' C3' C4' 179.25(19) . . . . ? C2' C3' C4' C5' -0.8(3) . . . . ? C2' C3' C4' C1"' 178.21(19) . . . . ? C3' C4' C5' C6' 0.8(3) . . . . ? C1"' C4' C5' C6' -178.16(19) . . . . ? C2' N1' C6' C5' -0.7(3) . . . . ? Cu N1' C6' C5' -179.86(15) . . . . ? C2' N1' C6' C2" -179.61(18) . . . . ? Cu N1' C6' C2" 1.2(2) . . . . ? C4' C5' C6' N1' -0.1(3) . . . . ? C4' C5' C6' C2" 178.68(19) . . . . ? C6" N1" C2" C3" 0.0(3) . . . . ? Cu N1" C2" C3" 178.65(16) . . . . ? C6" N1" C2" C6' 179.06(18) . . . . ? Cu N1" C2" C6' -2.3(2) . . . . ? N1' C6' C2" N1" 0.8(3) . . . . ? C5' C6' C2" N1" -178.0(2) . . . . ? N1' C6' C2" C3" 179.85(19) . . . . ? C5' C6' C2" C3" 1.0(3) . . . . ? N1" C2" C3" C4" -0.3(3) . . . . ? C6' C2" C3" C4" -179.2(2) . . . . ? C2" C3" C4" C5" 0.2(3) . . . . ? C3" C4" C5" C6" 0.1(3) . . . . ? C2" N1" C6" C5" 0.3(3) . . . . ? Cu N1" C6" C5" -178.11(16) . . . . ? C4" C5" C6" N1" -0.4(3) . . . . ? C6 N1 C2 C3 -0.7(3) . . . . ? Cu N1 C2 C3 -177.01(17) . . . . ? C6 N1 C2 C2' 177.38(19) . . . . ? Cu N1 C2 C2' 1.0(2) . . . . ? N1' C2' C2 N1 -1.1(3) . . . . ? C3' C2' C2 N1 179.7(2) . . . . ? N1' C2' C2 C3 177.0(2) . . . . ? C3' C2' C2 C3 -2.3(3) . . . . ? N1 C2 C3 C4 1.4(3) . . . . ? C2' C2 C3 C4 -176.5(2) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C2 N1 C6 C5 -0.8(3) . . . . ? Cu N1 C6 C5 175.00(18) . . . . ? C4 C5 C6 N1 1.6(4) . . . . ? C3' C4' C1"' C2"' 160.9(2) . . . . ? C5' C4' C1"' C2"' -20.2(3) . . . . ? C3' C4' C1"' C6"' -18.9(3) . . . . ? C5' C4' C1"' C6"' 160.1(2) . . . . ? C6"' C1"' C2"' C3"' 0.6(4) . . . . ? C4' C1"' C2"' C3"' -179.2(2) . . . . ? C1"' C2"' C3"' C4"' -0.1(4) . . . . ? C2"' C3"' C4"' C5"' 0.2(4) . . . . ? C2"' C3"' C4"' C7 -179.5(3) . . . . ? C3"' C4"' C5"' C6"' -0.8(4) . . . . ? C7 C4"' C5"' C6"' 178.9(3) . . . . ? C4"' C5"' C6"' C1"' 1.3(4) . . . . ? C2"' C1"' C6"' C5"' -1.2(3) . . . . ? C4' C1"' C6"' C5"' 178.6(2) . . . . ? C5"' C4"' C7 O -150.2(3) . . . . ? C3"' C4"' C7 O 29.5(4) . . . . ? C4"' C7 O C01 179.5(3) . . . . ? C7 O C01 C02 140.7(3) . . . . ? C05" N01" C02 N01 -150.0(3) . . . . ? N02" N01" C02 N01 39.0(3) . . . . ? C05" N01" C02 N01' 93.5(3) . . . . ? N02" N01" C02 N01' -77.5(3) . . . . ? C05" N01" C02 C01 -27.8(4) . . . . ? N02" N01" C02 C01 161.2(3) . . . . ? N02 N01 C02 N01" 88.4(3) . . . . ? C05 N01 C02 N01" -84.6(3) . . . . ? N02 N01 C02 N01' -154.7(2) . . . . ? C05 N01 C02 N01' 32.3(4) . . . . ? N02 N01 C02 C01 -35.0(3) . . . . ? C05 N01 C02 C01 152.0(3) . . . . ? C05' N01' C02 N01" 0.1(4) . . . . ? N02' N01' C02 N01" -177.4(2) . . . . ? C05' N01' C02 N01 -117.9(3) . . . . ? N02' N01' C02 N01 64.5(3) . . . . ? C05' N01' C02 C01 122.6(3) . . . . ? N02' N01' C02 C01 -54.9(3) . . . . ? O C01 C02 N01" 66.0(3) . . . . ? O C01 C02 N01 -172.0(2) . . . . ? O C01 C02 N01' -54.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.850 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.058 #====END data_[Zn(PzT)(Cl)2].CH3CN _database_code_depnum_ccdc_archive 'CCDC 277290' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C33 H27 Cl2 N9 O Zn, C2 H3 N ; _chemical_formula_sum 'C35 H30 Cl2 N10 O Zn' _chemical_formula_weight 742.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3507(15) _cell_length_b 11.1461(15) _cell_length_c 18.124(3) _cell_angle_alpha 86.826(3) _cell_angle_beta 82.396(2) _cell_angle_gamma 85.480(2) _cell_volume 1665.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used 7386 _cell_measurement_theta_min 4.395 _cell_measurement_theta_max 52.736 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.88 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4902 _exptl_absorpt_correction_T_max 0.9114 _exptl_absorpt_process_details 'sadabs v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(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 SMART/CCD _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14016 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 26.47 _reflns_number_total 6541 _reflns_number_gt 5379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker XPREP' _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^)+(0.0443P)^2^+1.7457P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6541 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0957 _refine_ls_wR_factor_gt 0.0869 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Zn Zn 0.63396(3) 0.72730(2) 0.610059(15) 0.01842(9) Uani 1 1 d . . . N1 N 0.7197(2) 0.56935(17) 0.54617(11) 0.0182(4) Uani 1 1 d . . . N1' N 0.5182(2) 0.74715(16) 0.51526(11) 0.0168(4) Uani 1 1 d . . . N1" N 0.4574(2) 0.88060(17) 0.62958(11) 0.0186(4) Uani 1 1 d . . . C2 C 0.6748(3) 0.5700(2) 0.47818(13) 0.0182(5) Uani 1 1 d . . . C3 C 0.7279(3) 0.4793(2) 0.42969(14) 0.0218(5) Uani 1 1 d . . . H3 H 0.6943 0.4811 0.3815 0.026 Uiso 1 1 calc R . . C4 C 0.8315(3) 0.3857(2) 0.45324(15) 0.0237(5) Uani 1 1 d . . . H4 H 0.8709 0.3225 0.4210 0.028 Uiso 1 1 calc R . . C5 C 0.8765(3) 0.3849(2) 0.52339(15) 0.0226(5) Uani 1 1 d . . . H5 H 0.9465 0.3211 0.5405 0.027 Uiso 1 1 calc R . . C6 C 0.8183(3) 0.4784(2) 0.56861(14) 0.0210(5) Uani 1 1 d . . . H6 H 0.8495 0.4782 0.6172 0.025 Uiso 1 1 calc R . . C2' C 0.5597(3) 0.6723(2) 0.45988(13) 0.0173(5) Uani 1 1 d . . . C3' C 0.4970(3) 0.6897(2) 0.39361(13) 0.0193(5) Uani 1 1 d . . . H3' H 0.5283 0.6347 0.3552 0.023 Uiso 1 1 calc R . . C4' C 0.3875(3) 0.7880(2) 0.38239(13) 0.0185(5) Uani 1 1 d . . . C5' C 0.3463(3) 0.8649(2) 0.44114(13) 0.0193(5) Uani 1 1 d . . . H5' H 0.2728 0.9335 0.4359 0.023 Uiso 1 1 calc R . . C6' C 0.4118(3) 0.8416(2) 0.50656(13) 0.0178(5) Uani 1 1 d . . . C2" C 0.3742(3) 0.9160(2) 0.57295(13) 0.0181(5) Uani 1 1 d . . . C3" C 0.2620(3) 1.0143(2) 0.57682(14) 0.0211(5) Uani 1 1 d . . . H3" H 0.2025 1.0372 0.5364 0.025 Uiso 1 1 calc R . . C4" C 0.2387(3) 1.0784(2) 0.64086(14) 0.0245(5) Uani 1 1 d . . . H4" H 0.1637 1.1471 0.6447 0.029 Uiso 1 1 calc R . . C5" C 0.3240(3) 1.0425(2) 0.69889(14) 0.0245(5) Uani 1 1 d . . . H5" H 0.3087 1.0856 0.7434 0.029 Uiso 1 1 calc R . . C6" C 0.4320(3) 0.9432(2) 0.69142(14) 0.0222(5) Uani 1 1 d . . . H6" H 0.4908 0.9180 0.7317 0.027 Uiso 1 1 calc R . . C1"' C 0.3159(3) 0.8083(2) 0.31222(13) 0.0196(5) Uani 1 1 d . . . C2"' C 0.1953(3) 0.8986(2) 0.30434(15) 0.0304(6) Uani 1 1 d . . . H2"' H 0.1598 0.9493 0.3446 0.036 Uiso 1 1 calc R . . C3"' C 0.1258(3) 0.9168(2) 0.24006(15) 0.0306(6) Uani 1 1 d . . . H3"' H 0.0438 0.9803 0.2365 0.037 Uiso 1 1 calc R . . C4"' C 0.1720(3) 0.8456(2) 0.18094(14) 0.0243(5) Uani 1 1 d . . . C5"' C 0.2918(4) 0.7550(3) 0.18764(16) 0.0408(8) Uani 1 1 d . . . H5"' H 0.3265 0.7048 0.1470 0.049 Uiso 1 1 calc R . . C6"' C 0.3623(4) 0.7360(3) 0.25212(16) 0.0401(8) Uani 1 1 d . . . H6"' H 0.4440 0.6723 0.2555 0.048 Uiso 1 1 calc R . . C7 C 0.0845(3) 0.8636(3) 0.11395(15) 0.0312(6) Uani 1 1 d . . . H7A H -0.0221 0.8289 0.1247 0.037 Uiso 1 1 calc R . . H7B H 0.0657 0.9509 0.1019 0.037 Uiso 1 1 calc R . . O O 0.1744(2) 0.8088(2) 0.05358(10) 0.0357(5) Uani 1 1 d . . . C01 C 0.0810(3) 0.8025(3) -0.00483(14) 0.0307(6) Uani 1 1 d . . . H01A H 0.0334 0.8837 -0.0183 0.037 Uiso 1 1 calc R . . H01B H -0.0082 0.7493 0.0104 0.037 Uiso 1 1 calc R . . C02 C 0.1930(3) 0.7522(2) -0.07096(14) 0.0286(6) Uani 1 1 d . . . N01 N 0.2459(3) 0.6269(2) -0.05671(12) 0.0343(6) Uani 1 1 d . . . N02 N 0.1782(3) 0.5651(2) 0.00441(13) 0.0362(6) Uani 1 1 d . . . N01' N 0.1075(3) 0.7635(2) -0.13614(12) 0.0256(5) Uani 1 1 d . . . N02' N -0.0563(3) 0.7712(2) -0.12752(13) 0.0313(5) Uani 1 1 d . . . N01" N 0.3346(3) 0.8207(2) -0.08702(12) 0.0322(5) Uani 1 1 d . . . N02" N 0.3123(3) 0.9379(2) -0.11074(15) 0.0400(6) Uani 1 1 d . . . C03 C 0.2387(4) 0.4536(3) -0.00443(18) 0.0405(7) Uani 1 1 d . . . H03 H 0.2143 0.3888 0.0305 0.049 Uiso 1 1 calc R . . C04 C 0.3413(4) 0.4410(3) -0.07013(18) 0.0501(9) Uani 1 1 d . . . H04 H 0.3977 0.3693 -0.0887 0.060 Uiso 1 1 calc R . . C05 C 0.3441(5) 0.5538(3) -0.10240(18) 0.0515(9) Uani 1 1 d . . . H05 H 0.4041 0.5769 -0.1486 0.062 Uiso 1 1 calc R . . C03' C -0.0924(4) 0.7738(3) -0.19666(16) 0.0351(7) Uani 1 1 d . . . H03' H -0.1998 0.7798 -0.2092 0.042 Uiso 1 1 calc R . . C04' C 0.0464(4) 0.7666(3) -0.24886(16) 0.0358(7) Uani 1 1 d . . . H04' H 0.0515 0.7663 -0.3015 0.043 Uiso 1 1 calc R . . C05' C 0.1721(4) 0.7602(2) -0.20827(15) 0.0304(6) Uani 1 1 d . . . H05' H 0.2840 0.7545 -0.2270 0.037 Uiso 1 1 calc R . . C03" C 0.4521(4) 0.9834(4) -0.10717(19) 0.0493(9) Uani 1 1 d . . . H03" H 0.4739 1.0644 -0.1215 0.059 Uiso 1 1 calc R . . C04" C 0.5629(4) 0.8991(4) -0.0801(2) 0.0578(10) Uani 1 1 d . . . H04" H 0.6710 0.9108 -0.0726 0.069 Uiso 1 1 calc R . . C05" C 0.4851(4) 0.7964(4) -0.06661(18) 0.0500(9) Uani 1 1 d . . . H05" H 0.5276 0.7217 -0.0467 0.060 Uiso 1 1 calc R . . Cl1 Cl 0.86000(7) 0.83105(5) 0.58766(3) 0.02135(13) Uani 1 1 d . . . Cl2 Cl 0.57887(8) 0.62474(6) 0.71978(4) 0.03203(16) Uani 1 1 d . . . N N 0.8295(5) 0.6613(3) 0.2692(3) 0.0997(17) Uani 1 1 d . . . C C 0.9161(5) 0.6069(3) 0.2312(2) 0.0510(9) Uani 1 1 d . . . C' C 1.0268(5) 0.5347(3) 0.1807(2) 0.0532(9) Uani 1 1 d . . . H'1 H 0.9719 0.4666 0.1665 0.080 Uiso 1 1 calc R . . H'2 H 1.1207 0.5045 0.2052 0.080 Uiso 1 1 calc R . . H'3 H 1.0629 0.5841 0.1360 0.080 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 Zn 0.02044(15) 0.01539(15) 0.01934(15) -0.00158(10) -0.00343(11) 0.00125(10) N1 0.0161(10) 0.0148(10) 0.0234(11) -0.0009(7) -0.0013(8) -0.0016(7) N1' 0.0151(10) 0.0130(10) 0.0226(10) -0.0026(7) -0.0022(8) -0.0016(7) N1" 0.0199(10) 0.0165(10) 0.0193(10) -0.0017(7) -0.0022(8) 0.0003(7) C2 0.0140(11) 0.0147(11) 0.0258(13) -0.0012(9) -0.0005(9) -0.0033(8) C3 0.0197(12) 0.0188(12) 0.0267(13) -0.0046(9) -0.0002(10) -0.0032(9) C4 0.0185(12) 0.0162(12) 0.0350(15) -0.0053(10) 0.0037(10) -0.0005(9) C5 0.0165(12) 0.0143(12) 0.0355(15) 0.0027(9) -0.0002(10) 0.0002(8) C6 0.0174(12) 0.0183(12) 0.0269(13) 0.0029(9) -0.0020(10) -0.0030(9) C2' 0.0157(11) 0.0134(11) 0.0226(12) -0.0026(8) -0.0003(9) -0.0015(8) C3' 0.0197(12) 0.0155(11) 0.0227(13) -0.0057(9) -0.0007(10) -0.0022(9) C4' 0.0174(12) 0.0162(12) 0.0223(13) -0.0029(9) -0.0022(9) -0.0038(8) C5' 0.0188(12) 0.0157(12) 0.0235(13) -0.0032(9) -0.0032(10) -0.0001(8) C6' 0.0174(11) 0.0134(11) 0.0227(12) -0.0029(8) -0.0028(9) -0.0006(8) C2" 0.0189(12) 0.0156(11) 0.0197(12) -0.0020(8) -0.0012(9) -0.0018(8) C3" 0.0226(12) 0.0189(12) 0.0227(13) -0.0026(9) -0.0067(10) -0.0001(9) C4" 0.0272(13) 0.0194(13) 0.0257(13) -0.0049(9) -0.0008(11) 0.0043(9) C5" 0.0295(14) 0.0217(13) 0.0221(13) -0.0072(9) -0.0009(10) 0.0003(10) C6" 0.0258(13) 0.0215(13) 0.0197(13) -0.0020(9) -0.0039(10) -0.0013(9) C1"' 0.0195(12) 0.0168(12) 0.0234(13) -0.0050(9) -0.0042(10) -0.0016(9) C2"' 0.0382(16) 0.0248(14) 0.0294(15) -0.0116(10) -0.0123(12) 0.0106(11) C3"' 0.0329(15) 0.0271(14) 0.0334(15) -0.0078(11) -0.0146(12) 0.0099(11) C4"' 0.0246(13) 0.0239(13) 0.0252(14) -0.0015(10) -0.0075(10) 0.0004(10) C5"' 0.0428(18) 0.052(2) 0.0280(16) -0.0192(13) -0.0128(13) 0.0200(14) C6"' 0.0448(18) 0.0439(18) 0.0316(16) -0.0164(13) -0.0168(13) 0.0266(14) C7 0.0318(15) 0.0356(16) 0.0271(15) -0.0078(11) -0.0102(12) 0.0078(11) O 0.0303(11) 0.0569(14) 0.0194(10) -0.0084(8) -0.0077(8) 0.0113(9) C01 0.0305(15) 0.0426(17) 0.0187(13) -0.0042(11) -0.0079(11) 0.0099(11) C02 0.0302(14) 0.0350(15) 0.0199(13) -0.0017(10) -0.0065(11) 0.0087(11) N01 0.0388(14) 0.0406(14) 0.0196(12) 0.0031(9) -0.0005(10) 0.0130(10) N02 0.0339(13) 0.0425(15) 0.0289(13) 0.0064(10) 0.0005(10) 0.0059(10) N01' 0.0267(12) 0.0305(12) 0.0200(11) -0.0008(8) -0.0076(9) 0.0026(9) N02' 0.0289(12) 0.0353(13) 0.0299(13) -0.0026(9) -0.0094(10) 0.0072(9) N01" 0.0261(12) 0.0484(15) 0.0225(12) -0.0046(10) -0.0073(9) 0.0038(10) N02" 0.0405(15) 0.0400(15) 0.0415(15) -0.0088(11) -0.0089(12) -0.0039(11) C03 0.0389(17) 0.0402(18) 0.0394(18) 0.0073(13) -0.0040(14) 0.0078(13) C04 0.062(2) 0.044(2) 0.0367(18) 0.0036(14) 0.0030(16) 0.0238(16) C05 0.067(2) 0.051(2) 0.0263(16) 0.0067(14) 0.0106(15) 0.0249(17) C03' 0.0372(16) 0.0363(16) 0.0346(16) -0.0041(12) -0.0187(13) 0.0055(12) C04' 0.0493(18) 0.0385(17) 0.0216(14) -0.0029(11) -0.0135(13) 0.0000(13) C05' 0.0370(15) 0.0313(15) 0.0227(14) -0.0015(10) -0.0045(12) 0.0006(11) C03" 0.0427(19) 0.065(2) 0.043(2) -0.0165(16) -0.0028(15) -0.0177(16) C04" 0.0307(18) 0.098(3) 0.048(2) -0.014(2) -0.0075(16) -0.0137(19) C05" 0.0277(16) 0.083(3) 0.0363(18) 0.0034(16) -0.0069(14) 0.0126(16) Cl1 0.0199(3) 0.0167(3) 0.0290(3) -0.0040(2) -0.0093(2) 0.0012(2) Cl2 0.0396(4) 0.0276(3) 0.0244(3) 0.0050(2) 0.0040(3) 0.0078(3) N 0.116(3) 0.052(2) 0.114(3) -0.036(2) 0.078(3) -0.030(2) C 0.063(2) 0.0304(18) 0.054(2) -0.0076(14) 0.0236(18) -0.0120(15) C' 0.067(2) 0.041(2) 0.044(2) -0.0055(15) 0.0152(17) 0.0060(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 Zn N1' 2.074(2) . ? Zn N1" 2.180(2) . ? Zn N1 2.1818(19) . ? Zn Cl2 2.2499(7) . ? Zn Cl1 2.2704(7) . ? N1 C2 1.334(3) . ? N1 C6 1.335(3) . ? N1' C2' 1.334(3) . ? N1' C6' 1.339(3) . ? N1" C6" 1.337(3) . ? N1" C2" 1.339(3) . ? C2 C3 1.384(3) . ? C2 C2' 1.485(3) . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.372(4) . ? C4 H4 0.9500 . ? C5 C6 1.380(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C2' C3' 1.371(3) . ? C3' C4' 1.394(3) . ? C3' H3' 0.9500 . ? C4' C5' 1.395(3) . ? C4' C1"' 1.474(3) . ? C5' C6' 1.374(3) . ? C5' H5' 0.9500 . ? C6' C2" 1.484(3) . ? C2" C3" 1.384(3) . ? C3" C4" 1.380(3) . ? C3" H3" 0.9500 . ? C4" C5" 1.371(4) . ? C4" H4" 0.9500 . ? C5" C6" 1.373(3) . ? C5" H5" 0.9500 . ? C6" H6" 0.9500 . ? C1"' C2"' 1.382(3) . ? C1"' C6"' 1.386(4) . ? C2"' C3"' 1.368(4) . ? C2"' H2"' 0.9500 . ? C3"' C4"' 1.366(4) . ? C3"' H3"' 0.9500 . ? C4"' C5"' 1.376(4) . ? C4"' C7 1.494(4) . ? C5"' C6"' 1.375(4) . ? C5"' H5"' 0.9500 . ? C6"' H6"' 0.9500 . ? C7 O 1.385(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? O C01 1.403(3) . ? C01 C02 1.523(4) . ? C01 H01A 0.9900 . ? C01 H01B 0.9900 . ? C02 N01" 1.447(4) . ? C02 N01 1.452(4) . ? C02 N01' 1.453(3) . ? N01 C05 1.346(4) . ? N01 N02 1.353(3) . ? N02 C03 1.315(4) . ? N01' C05' 1.348(3) . ? N01' N02' 1.353(3) . ? N02' C03' 1.325(4) . ? N01" C05" 1.359(4) . ? N01" N02" 1.359(4) . ? N02" C03" 1.319(4) . ? C03 C04 1.379(4) . ? C03 H03 0.9500 . ? C04 C05 1.358(5) . ? C04 H04 0.9500 . ? C05 H05 0.9500 . ? C03' C04' 1.395(4) . ? C03' H03' 0.9500 . ? C04' C05' 1.355(4) . ? C04' H04' 0.9500 . ? C05' H05' 0.9500 . ? C03" C04" 1.383(5) . ? C03" H03" 0.9500 . ? C04" C05" 1.356(6) . ? C04" H04" 0.9500 . ? C05" H05" 0.9500 . ? N C 1.101(4) . ? C C' 1.442(4) . ? C' H'1 0.9800 . ? C' H'2 0.9800 . ? C' H'3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1' Zn N1" 74.97(7) . . ? N1' Zn N1 74.71(7) . . ? N1" Zn N1 148.54(8) . . ? N1' Zn Cl2 132.68(6) . . ? N1" Zn Cl2 98.73(5) . . ? N1 Zn Cl2 95.63(5) . . ? N1' Zn Cl1 107.55(5) . . ? N1" Zn Cl1 97.90(5) . . ? N1 Zn Cl1 98.99(5) . . ? Cl2 Zn Cl1 119.75(3) . . ? C2 N1 C6 119.3(2) . . ? C2 N1 Zn 115.65(15) . . ? C6 N1 Zn 124.95(17) . . ? C2' N1' C6' 119.6(2) . . ? C2' N1' Zn 120.18(15) . . ? C6' N1' Zn 119.97(15) . . ? C6" N1" C2" 118.8(2) . . ? C6" N1" Zn 125.26(16) . . ? C2" N1" Zn 115.88(15) . . ? N1 C2 C3 122.1(2) . . ? N1 C2 C2' 115.0(2) . . ? C3 C2 C2' 122.9(2) . . ? C2 C3 C4 118.2(2) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 118.9(2) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? N1 C6 C5 122.0(2) . . ? N1 C6 H6 119.0 . . ? C5 C6 H6 119.0 . . ? N1' C2' C3' 121.7(2) . . ? N1' C2' C2 113.6(2) . . ? C3' C2' C2 124.7(2) . . ? C2' C3' C4' 120.2(2) . . ? C2' C3' H3' 119.9 . . ? C4' C3' H3' 119.9 . . ? C5' C4' C3' 117.0(2) . . ? C5' C4' C1"' 121.5(2) . . ? C3' C4' C1"' 121.5(2) . . ? C6' C5' C4' 120.0(2) . . ? C6' C5' H5' 120.0 . . ? C4' C5' H5' 120.0 . . ? N1' C6' C5' 121.6(2) . . ? N1' C6' C2" 113.9(2) . . ? C5' C6' C2" 124.5(2) . . ? N1" C2" C3" 122.0(2) . . ? N1" C2" C6' 114.8(2) . . ? C3" C2" C6' 123.2(2) . . ? C4" C3" C2" 118.3(2) . . ? C4" C3" H3" 120.9 . . ? C2" C3" H3" 120.9 . . ? C5" C4" C3" 119.8(2) . . ? C5" C4" H4" 120.1 . . ? C3" C4" H4" 120.1 . . ? C6" C5" C4" 118.7(2) . . ? C6" C5" H5" 120.7 . . ? C4" C5" H5" 120.7 . . ? N1" C6" C5" 122.4(2) . . ? N1" C6" H6" 118.8 . . ? C5" C6" H6" 118.8 . . ? C2"' C1"' C6"' 116.9(2) . . ? C2"' C1"' C4' 121.1(2) . . ? C6"' C1"' C4' 121.9(2) . . ? C3"' C2"' C1"' 121.7(2) . . ? C3"' C2"' H2"' 119.1 . . ? C1"' C2"' H2"' 119.1 . . ? C4"' C3"' C2"' 121.2(2) . . ? C4"' C3"' H3"' 119.4 . . ? C2"' C3"' H3"' 119.4 . . ? C3"' C4"' C5"' 118.0(2) . . ? C3"' C4"' C7 119.2(2) . . ? C5"' C4"' C7 122.7(2) . . ? C6"' C5"' C4"' 121.1(3) . . ? C6"' C5"' H5"' 119.4 . . ? C4"' C5"' H5"' 119.4 . . ? C5"' C6"' C1"' 121.0(2) . . ? C5"' C6"' H6"' 119.5 . . ? C1"' C6"' H6"' 119.5 . . ? O C7 C4"' 110.3(2) . . ? O C7 H7A 109.6 . . ? C4"' C7 H7A 109.6 . . ? O C7 H7B 109.6 . . ? C4"' C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 O C01 111.0(2) . . ? O C01 C02 107.4(2) . . ? O C01 H01A 110.2 . . ? C02 C01 H01A 110.2 . . ? O C01 H01B 110.2 . . ? C02 C01 H01B 110.2 . . ? H01A C01 H01B 108.5 . . ? N01" C02 N01 108.5(2) . . ? N01" C02 N01' 107.8(2) . . ? N01 C02 N01' 109.8(2) . . ? N01" C02 C01 110.3(2) . . ? N01 C02 C01 111.5(2) . . ? N01' C02 C01 108.8(2) . . ? C05 N01 N02 111.4(2) . . ? C05 N01 C02 127.9(2) . . ? N02 N01 C02 120.1(2) . . ? C03 N02 N01 104.2(2) . . ? C05' N01' N02' 112.4(2) . . ? C05' N01' C02 127.6(2) . . ? N02' N01' C02 119.8(2) . . ? C03' N02' N01' 103.8(2) . . ? C05" N01" N02" 111.0(3) . . ? C05" N01" C02 129.5(3) . . ? N02" N01" C02 117.7(2) . . ? C03" N02" N01" 104.7(3) . . ? N02 C03 C04 112.5(3) . . ? N02 C03 H03 123.8 . . ? C04 C03 H03 123.8 . . ? C05 C04 C03 104.8(3) . . ? C05 C04 H04 127.6 . . ? C03 C04 H04 127.6 . . ? N01 C05 C04 107.1(3) . . ? N01 C05 H05 126.4 . . ? C04 C05 H05 126.4 . . ? N02' C03' C04' 111.9(3) . . ? N02' C03' H03' 124.1 . . ? C04' C03' H03' 124.1 . . ? C05' C04' C03' 105.2(2) . . ? C05' C04' H04' 127.4 . . ? C03' C04' H04' 127.4 . . ? N01' C05' C04' 106.7(3) . . ? N01' C05' H05' 126.6 . . ? C04' C05' H05' 126.6 . . ? N02" C03" C04" 111.9(3) . . ? N02" C03" H03" 124.0 . . ? C04" C03" H03" 124.0 . . ? C05" C04" C03" 105.6(3) . . ? C05" C04" H04" 127.2 . . ? C03" C04" H04" 127.2 . . ? C04" C05" N01" 106.8(3) . . ? C04" C05" H05" 126.6 . . ? N01" C05" H05" 126.6 . . ? N C C' 178.8(5) . . ? C C' H'1 109.5 . . ? C C' H'2 109.5 . . ? H'1 C' H'2 109.5 . . ? C C' H'3 109.5 . . ? H'1 C' H'3 109.5 . . ? H'2 C' H'3 109.5 . . ? 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' Zn N1 C2 7.46(15) . . . . ? N1" Zn N1 C2 23.3(2) . . . . ? Cl2 Zn N1 C2 140.23(15) . . . . ? Cl1 Zn N1 C2 -98.40(15) . . . . ? N1' Zn N1 C6 -176.39(19) . . . . ? N1" Zn N1 C6 -160.57(17) . . . . ? Cl2 Zn N1 C6 -43.61(18) . . . . ? Cl1 Zn N1 C6 77.75(18) . . . . ? N1" Zn N1' C2' -179.74(18) . . . . ? N1 Zn N1' C2' -8.21(16) . . . . ? Cl2 Zn N1' C2' -91.68(17) . . . . ? Cl1 Zn N1' C2' 86.58(16) . . . . ? N1" Zn N1' C6' 6.26(16) . . . . ? N1 Zn N1' C6' 177.80(18) . . . . ? Cl2 Zn N1' C6' 94.32(17) . . . . ? Cl1 Zn N1' C6' -87.42(17) . . . . ? N1' Zn N1" C6" 178.6(2) . . . . ? N1 Zn N1" C6" 162.79(17) . . . . ? Cl2 Zn N1" C6" 46.61(19) . . . . ? Cl1 Zn N1" C6" -75.28(19) . . . . ? N1' Zn N1" C2" -4.33(16) . . . . ? N1 Zn N1" C2" -20.1(2) . . . . ? Cl2 Zn N1" C2" -136.31(15) . . . . ? Cl1 Zn N1" C2" 101.80(16) . . . . ? C6 N1 C2 C3 -0.3(3) . . . . ? Zn N1 C2 C3 176.11(17) . . . . ? C6 N1 C2 C2' 177.59(19) . . . . ? Zn N1 C2 C2' -6.0(2) . . . . ? N1 C2 C3 C4 -0.2(3) . . . . ? C2' C2 C3 C4 -177.9(2) . . . . ? C2 C3 C4 C5 0.6(3) . . . . ? C3 C4 C5 C6 -0.6(3) . . . . ? C2 N1 C6 C5 0.4(3) . . . . ? Zn N1 C6 C5 -175.66(16) . . . . ? C4 C5 C6 N1 0.1(3) . . . . ? C6' N1' C2' C3' 0.4(3) . . . . ? Zn N1' C2' C3' -173.61(16) . . . . ? C6' N1' C2' C2 -178.35(19) . . . . ? Zn N1' C2' C2 7.6(3) . . . . ? N1 C2 C2' N1' -0.6(3) . . . . ? C3 C2 C2' N1' 177.2(2) . . . . ? N1 C2 C2' C3' -179.3(2) . . . . ? C3 C2 C2' C3' -1.5(4) . . . . ? N1' C2' C3' C4' 0.4(3) . . . . ? C2 C2' C3' C4' 179.0(2) . . . . ? C2' C3' C4' C5' -0.3(3) . . . . ? C2' C3' C4' C1"' -179.0(2) . . . . ? C3' C4' C5' C6' -0.5(3) . . . . ? C1"' C4' C5' C6' 178.2(2) . . . . ? C2' N1' C6' C5' -1.3(3) . . . . ? Zn N1' C6' C5' 172.75(17) . . . . ? C2' N1' C6' C2" 178.91(19) . . . . ? Zn N1' C6' C2" -7.1(3) . . . . ? C4' C5' C6' N1' 1.4(3) . . . . ? C4' C5' C6' C2" -178.9(2) . . . . ? C6" N1" C2" C3" -0.7(3) . . . . ? Zn N1" C2" C3" -177.95(18) . . . . ? C6" N1" C2" C6' 179.5(2) . . . . ? Zn N1" C2" C6' 2.2(2) . . . . ? N1' C6' C2" N1" 2.9(3) . . . . ? C5' C6' C2" N1" -176.9(2) . . . . ? N1' C6' C2" C3" -177.0(2) . . . . ? C5' C6' C2" C3" 3.2(4) . . . . ? N1" C2" C3" C4" 1.3(4) . . . . ? C6' C2" C3" C4" -178.9(2) . . . . ? C2" C3" C4" C5" -1.0(4) . . . . ? C3" C4" C5" C6" 0.3(4) . . . . ? C2" N1" C6" C5" -0.1(4) . . . . ? Zn N1" C6" C5" 176.86(18) . . . . ? C4" C5" C6" N1" 0.3(4) . . . . ? C5' C4' C1"' C2"' -5.4(3) . . . . ? C3' C4' C1"' C2"' 173.3(2) . . . . ? C5' C4' C1"' C6"' 176.6(3) . . . . ? C3' C4' C1"' C6"' -4.7(4) . . . . ? C6"' C1"' C2"' C3"' -0.6(4) . . . . ? C4' C1"' C2"' C3"' -178.7(2) . . . . ? C1"' C2"' C3"' C4"' 0.6(5) . . . . ? C2"' C3"' C4"' C5"' -0.5(4) . . . . ? C2"' C3"' C4"' C7 175.8(3) . . . . ? C3"' C4"' C5"' C6"' 0.5(5) . . . . ? C7 C4"' C5"' C6"' -175.6(3) . . . . ? C4"' C5"' C6"' C1"' -0.6(5) . . . . ? C2"' C1"' C6"' C5"' 0.7(5) . . . . ? C4' C1"' C6"' C5"' 178.8(3) . . . . ? C3"' C4"' C7 O 163.4(3) . . . . ? C5"' C4"' C7 O -20.5(4) . . . . ? C4"' C7 O C01 167.5(2) . . . . ? C7 O C01 C02 174.7(2) . . . . ? O C01 C02 N01" -52.3(3) . . . . ? O C01 C02 N01 68.3(3) . . . . ? O C01 C02 N01' -170.4(2) . . . . ? N01" C02 N01 C05 -58.6(4) . . . . ? N01' C02 N01 C05 59.0(4) . . . . ? C01 C02 N01 C05 179.7(3) . . . . ? N01" C02 N01 N02 130.8(3) . . . . ? N01' C02 N01 N02 -111.6(3) . . . . ? C01 C02 N01 N02 9.1(4) . . . . ? C05 N01 N02 C03 0.8(4) . . . . ? C02 N01 N02 C03 172.8(3) . . . . ? N01" C02 N01' C05' 41.4(3) . . . . ? N01 C02 N01' C05' -76.6(3) . . . . ? C01 C02 N01' C05' 161.1(3) . . . . ? N01" C02 N01' N02' -143.1(2) . . . . ? N01 C02 N01' N02' 98.9(3) . . . . ? C01 C02 N01' N02' -23.4(3) . . . . ? C05' N01' N02' C03' -0.6(3) . . . . ? C02 N01' N02' C03' -176.7(2) . . . . ? N01 C02 N01" C05" -24.6(4) . . . . ? N01' C02 N01" C05" -143.5(3) . . . . ? C01 C02 N01" C05" 97.8(3) . . . . ? N01 C02 N01" N02" 172.3(2) . . . . ? N01' C02 N01" N02" 53.4(3) . . . . ? C01 C02 N01" N02" -65.3(3) . . . . ? C05" N01" N02" C03" 2.2(3) . . . . ? C02 N01" N02" C03" 168.3(2) . . . . ? N01 N02 C03 C04 -1.0(4) . . . . ? N02 C03 C04 C05 0.9(4) . . . . ? N02 N01 C05 C04 -0.3(4) . . . . ? C02 N01 C05 C04 -171.5(3) . . . . ? C03 C04 C05 N01 -0.3(4) . . . . ? N01' N02' C03' C04' 0.6(3) . . . . ? N02' C03' C04' C05' -0.4(3) . . . . ? N02' N01' C05' C04' 0.4(3) . . . . ? C02 N01' C05' C04' 176.1(3) . . . . ? C03' C04' C05' N01' 0.0(3) . . . . ? N01" N02" C03" C04" -1.3(4) . . . . ? N02" C03" C04" C05" 0.0(4) . . . . ? C03" C04" C05" N01" 1.3(4) . . . . ? N02" N01" C05" C04" -2.3(4) . . . . ? C02 N01" C05" C04" -166.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.703 _refine_diff_density_min -0.346 _refine_diff_density_rms 0.066 #====END