Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Xian-Ming Zhang' _publ_contact_author_address ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; _publ_contact_author_phone '+86 357 2051402' _publ_contact_author_fax '+86 357 2051402' _publ_contact_author_email zhangxm@dns.sxtu.edu.cn _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as a supplmentary data for a manuscript submitted to Dalton Trans. ; #================================================================= # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_coden_ASTM ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; loop_ _publ_author_name _publ_author_address 'Xian-Ming Zhang.' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; 'Yan-Fei Zhao.' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; 'Hai-Shun Wu.' ; School of Chemistry & Material Science Shanxi Normal University Linfen 041004 Shanxi Province P. R. China ; S.R.Batten ; School of Chemistry Monash University 3800 Australia ; _publ_contact_author_name 'Zhang, Xian-Ming' #====================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 293447' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H7 N5' _chemical_formula_weight 101.13 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.67(2) _cell_length_b 20.64(2) _cell_length_c 11.329(11) _cell_angle_alpha 90.00 _cell_angle_beta 118.008(15) _cell_angle_gamma 90.00 _cell_volume 4267(7) _cell_formula_units_Z 32 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.259 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 0.094 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9723 _exptl_absorpt_correction_T_max 0.9723 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15048 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 23.99 _reflns_number_total 3341 _reflns_number_gt 2442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0910P)^2^+1.8358P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3341 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1724 _refine_ls_wR_factor_gt 0.1569 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 N1 N 0.14901(12) 0.02083(11) 0.6340(2) 0.0454(6) Uani 1 1 d . . . N2 N 0.16610(13) 0.03355(12) 0.7607(2) 0.0497(6) Uani 1 1 d . . . N3 N 0.11762(14) 0.07282(11) 0.7628(2) 0.0498(6) Uani 1 1 d . . . N4 N 0.06761(12) 0.08730(11) 0.6373(2) 0.0457(6) Uani 1 1 d . . . N5 N 0.12239(12) 0.20655(11) 0.3619(2) 0.0467(6) Uani 1 1 d . . . N6 N 0.10523(13) 0.18892(12) 0.2369(2) 0.0496(6) Uani 1 1 d . . . N7 N 0.15372(13) 0.14847(12) 0.2402(2) 0.0504(6) Uani 1 1 d . . . N8 N 0.20398(12) 0.13807(11) 0.3669(2) 0.0471(6) Uani 1 1 d . . . N9 N 0.17881(13) 0.34131(11) 0.8633(2) 0.0468(6) Uani 1 1 d . . . N10 N 0.13439(14) 0.32253(12) 0.7378(2) 0.0511(6) Uani 1 1 d . . . N11 N 0.09554(14) 0.27333(12) 0.7379(2) 0.0520(6) Uani 1 1 d . . . N12 N 0.11304(13) 0.25884(11) 0.8641(2) 0.0470(6) Uani 1 1 d . . . N13 N 0.04583(12) 0.38835(11) 0.1316(2) 0.0457(6) Uani 1 1 d . . . N14 N 0.08745(13) 0.40683(12) 0.2587(2) 0.0490(6) Uani 1 1 d . . . N15 N 0.12855(12) 0.45459(11) 0.2623(2) 0.0486(6) Uani 1 1 d . . . N16 N 0.11584(13) 0.46882(11) 0.1378(2) 0.0454(6) Uani 1 1 d . . . C1 C 0.08819(14) 0.05439(12) 0.5605(3) 0.0374(6) Uani 1 1 d . . . C2 C 0.04893(18) 0.05534(16) 0.4125(3) 0.0541(8) Uani 1 1 d . . . H2A H 0.0135 0.0209 0.3804 0.147(19) Uiso 1 1 calc R . . H2B H 0.0834 0.0495 0.3789 0.115(15) Uiso 1 1 calc R . . H2C H 0.0244 0.0962 0.3821 0.16(2) Uiso 1 1 calc R . . C3 C 0.18306(14) 0.17431(13) 0.4392(3) 0.0396(6) Uani 1 1 d . . . C4 C 0.2227(2) 0.17892(18) 0.5877(3) 0.0619(9) Uani 1 1 d . . . H4A H 0.2441 0.1377 0.6247 0.139(18) Uiso 1 1 calc R . . H4B H 0.1889 0.1911 0.6198 0.17(2) Uiso 1 1 calc R . . H4C H 0.2606 0.2110 0.6143 0.20(3) Uiso 1 1 calc R . . C5 C 0.16428(14) 0.30107(13) 0.9390(3) 0.0406(7) Uani 1 1 d . . . C6 C 0.20031(19) 0.30359(18) 1.0870(3) 0.0616(9) Uani 1 1 d . . . H6A H 0.1637 0.3063 1.1162 0.119(15) Uiso 1 1 calc R . . H6B H 0.2315 0.3410 1.1177 0.17(2) Uiso 1 1 calc R . . H6C H 0.2291 0.2651 1.1230 0.144(19) Uiso 1 1 calc R . . C7 C 0.06489(13) 0.42719(12) 0.0600(2) 0.0364(6) Uani 1 1 d . . . C8 C 0.03339(17) 0.42495(17) -0.0870(3) 0.0556(8) Uani 1 1 d . . . H8A H 0.0105 0.3836 -0.1191 0.135(18) Uiso 1 1 calc R . . H8B H 0.0716 0.4311 -0.1113 0.099(13) Uiso 1 1 calc R . . H8C H -0.0025 0.4587 -0.1261 0.17(2) Uiso 1 1 calc R . . N17 N 0.02060(15) 0.26197(13) 0.4434(3) 0.0457(6) Uani 1 1 d . . . N18 N 0.15058(15) 0.40814(13) 0.5551(3) 0.0430(6) Uani 1 1 d . . . N19 N 0.25095(14) -0.03254(13) 0.5558(3) 0.0437(6) Uani 1 1 d . . . N20 N 0.07959(15) 0.13780(13) 0.9446(3) 0.0430(6) Uani 1 1 d . . . H19A H 0.2913(17) -0.0047(14) 0.599(3) 0.053(9) Uiso 1 1 d . . . H20A H 0.0961(14) 0.1140(13) 0.903(3) 0.043(8) Uiso 1 1 d . . . H17A H -0.0229(19) 0.2341(15) 0.397(3) 0.069(10) Uiso 1 1 d . . . H20B H 0.0276(19) 0.1272(15) 0.918(3) 0.073(10) Uiso 1 1 d . . . H17B H 0.0576(18) 0.2493(15) 0.419(3) 0.070(10) Uiso 1 1 d . . . H18A H 0.1401(17) 0.3759(15) 0.601(3) 0.065(9) Uiso 1 1 d . . . H18B H 0.1489(16) 0.4497(15) 0.589(3) 0.062(9) Uiso 1 1 d . . . H18C H 0.2002(19) 0.4025(15) 0.585(3) 0.063(9) Uiso 1 1 d . . . H19B H 0.2142(19) -0.0210(16) 0.589(3) 0.082(10) Uiso 1 1 d . . . H17C H 0.0432(17) 0.2578(14) 0.536(4) 0.068(10) Uiso 1 1 d . . . H18D H 0.1245(15) 0.4040(13) 0.464(3) 0.048(8) Uiso 1 1 d . . . H19C H 0.2673(17) -0.0797(16) 0.585(3) 0.070(10) Uiso 1 1 d . . . H17D H 0.0014(18) 0.3078(17) 0.411(3) 0.077(10) Uiso 1 1 d . . . H20C H 0.1085(16) 0.1361(13) 1.039(3) 0.057(9) Uiso 1 1 d . . . H19D H 0.229(2) -0.0283(15) 0.463(4) 0.081(11) Uiso 1 1 d . . . H20D H 0.0831(17) 0.1846(17) 0.911(3) 0.073(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0490(14) 0.0554(15) 0.0327(13) 0.0041(11) 0.0199(12) 0.0121(12) N2 0.0526(15) 0.0619(16) 0.0317(14) 0.0032(11) 0.0174(12) 0.0074(13) N3 0.0561(15) 0.0607(16) 0.0353(15) -0.0042(11) 0.0237(13) 0.0026(13) N4 0.0458(14) 0.0531(15) 0.0368(14) -0.0042(11) 0.0182(12) 0.0066(11) N5 0.0472(14) 0.0518(15) 0.0375(14) 0.0008(11) 0.0169(12) 0.0088(12) N6 0.0465(14) 0.0584(16) 0.0341(14) 0.0040(11) 0.0108(12) 0.0072(12) N7 0.0502(14) 0.0638(16) 0.0336(15) -0.0013(11) 0.0167(12) 0.0051(13) N8 0.0452(14) 0.0586(15) 0.0334(14) 0.0012(11) 0.0150(12) 0.0102(12) N9 0.0505(14) 0.0498(14) 0.0379(15) 0.0013(11) 0.0189(12) -0.0052(12) N10 0.0616(16) 0.0536(15) 0.0356(15) 0.0074(11) 0.0208(13) 0.0010(13) N11 0.0598(16) 0.0530(15) 0.0329(14) 0.0009(11) 0.0132(12) -0.0049(13) N12 0.0550(15) 0.0484(14) 0.0329(14) 0.0033(11) 0.0167(12) -0.0080(12) N13 0.0484(14) 0.0530(15) 0.0332(14) -0.0047(11) 0.0170(12) -0.0120(11) N14 0.0502(14) 0.0601(16) 0.0309(14) 0.0005(11) 0.0143(12) -0.0070(13) N15 0.0457(14) 0.0561(15) 0.0331(14) -0.0061(11) 0.0096(11) -0.0092(12) N16 0.0471(14) 0.0484(14) 0.0377(14) -0.0005(11) 0.0173(12) -0.0079(12) C1 0.0419(15) 0.0394(15) 0.0304(15) -0.0016(12) 0.0166(13) -0.0034(13) C2 0.064(2) 0.060(2) 0.0322(17) -0.0002(14) 0.0173(15) -0.0005(18) C3 0.0370(15) 0.0435(15) 0.0341(15) 0.0021(12) 0.0131(13) 0.0011(13) C4 0.070(2) 0.074(2) 0.0297(17) -0.0010(16) 0.0140(16) 0.000(2) C5 0.0456(16) 0.0429(16) 0.0326(16) 0.0033(12) 0.0178(14) 0.0015(13) C6 0.068(2) 0.074(2) 0.0350(18) 0.0024(16) 0.0184(17) 0.004(2) C7 0.0326(14) 0.0414(15) 0.0320(15) -0.0006(12) 0.0125(12) 0.0012(12) C8 0.0556(19) 0.076(2) 0.0334(17) -0.0019(15) 0.0197(15) 0.0005(18) N17 0.0420(15) 0.0510(17) 0.0317(15) -0.0065(12) 0.0071(12) 0.0063(13) N18 0.0489(16) 0.0515(17) 0.0316(15) 0.0082(12) 0.0213(13) 0.0116(13) N19 0.0362(14) 0.0529(17) 0.0320(15) -0.0109(12) 0.0078(12) -0.0004(13) N20 0.0545(16) 0.0496(16) 0.0315(15) -0.0094(11) 0.0259(13) -0.0096(13) _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 C1 1.330(3) . ? N1 N2 1.334(3) . ? N2 N3 1.297(3) . ? N3 N4 1.341(3) . ? N4 C1 1.321(3) . ? N5 C3 1.323(3) . ? N5 N6 1.339(3) . ? N6 N7 1.291(3) . ? N7 N8 1.336(3) . ? N8 C3 1.323(3) . ? N9 C5 1.326(3) . ? N9 N10 1.337(3) . ? N10 N11 1.295(3) . ? N11 N12 1.334(3) . ? N12 C5 1.325(3) . ? N13 C7 1.325(3) . ? N13 N14 1.340(3) . ? N14 N15 1.289(3) . ? N15 N16 1.341(3) . ? N16 C7 1.324(3) . ? C1 C2 1.481(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C4 1.489(4) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C6 1.482(4) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.477(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N17 H17A 0.99(3) . ? N17 H17B 0.97(3) . ? N17 H17C 0.93(4) . ? N17 H17D 1.02(3) . ? N18 H18A 0.93(3) . ? N18 H18B 0.95(3) . ? N18 H18C 0.93(3) . ? N18 H18D 0.91(3) . ? N19 H19A 0.94(3) . ? N19 H19B 1.02(4) . ? N19 H19C 1.03(3) . ? N19 H19D 0.93(4) . ? N20 H20A 0.86(3) . ? N20 H20B 1.00(3) . ? N20 H20C 0.95(3) . ? N20 H20D 1.05(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 N2 105.4(2) . . ? N3 N2 N1 109.0(2) . . ? N2 N3 N4 109.7(2) . . ? C1 N4 N3 104.9(2) . . ? C3 N5 N6 105.1(2) . . ? N7 N6 N5 109.2(2) . . ? N6 N7 N8 109.6(2) . . ? C3 N8 N7 105.0(2) . . ? C5 N9 N10 104.8(2) . . ? N11 N10 N9 110.1(2) . . ? N10 N11 N12 108.7(2) . . ? C5 N12 N11 105.7(2) . . ? C7 N13 N14 105.1(2) . . ? N15 N14 N13 109.4(2) . . ? N14 N15 N16 109.5(2) . . ? C7 N16 N15 105.1(2) . . ? N4 C1 N1 111.0(2) . . ? N4 C1 C2 124.3(3) . . ? N1 C1 C2 124.7(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N8 C3 N5 111.0(2) . . ? N8 C3 C4 124.7(3) . . ? N5 C3 C4 124.3(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N9 C5 N12 110.7(2) . . ? N9 C5 C6 124.3(3) . . ? N12 C5 C6 125.0(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N16 C7 N13 111.0(2) . . ? N16 C7 C8 124.2(2) . . ? N13 C7 C8 124.8(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H17A N17 H17B 110(2) . . ? H17A N17 H17C 113(3) . . ? H17B N17 H17C 105(3) . . ? H17A N17 H17D 104(3) . . ? H17B N17 H17D 112(3) . . ? H17C N17 H17D 113(3) . . ? H18A N18 H18B 110(3) . . ? H18A N18 H18C 103(3) . . ? H18B N18 H18C 102(3) . . ? H18A N18 H18D 113(3) . . ? H18B N18 H18D 115(2) . . ? H18C N18 H18D 111(2) . . ? H19A N19 H19B 108(2) . . ? H19A N19 H19C 109(2) . . ? H19B N19 H19C 107(3) . . ? H19A N19 H19D 112(3) . . ? H19B N19 H19D 109(3) . . ? H19C N19 H19D 111(3) . . ? H20A N20 H20B 111(2) . . ? H20A N20 H20C 114(3) . . ? H20B N20 H20C 111(2) . . ? H20A N20 H20D 102(2) . . ? H20B N20 H20D 110(3) . . ? H20C N20 H20D 109(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.270 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.075 #======================================================= data_2 _database_code_depnum_ccdc_archive 'CCDC 293448' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H7 N4 Na O2' _chemical_formula_weight 142.11 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Othorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 6.9599(19) _cell_length_b 7.0286(18) _cell_length_c 12.127(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 593.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 296 _exptl_absorpt_coefficient_mu 0.193 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9443 _exptl_absorpt_correction_T_max 0.9942 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _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 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1341 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -3 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 26.99 _reflns_number_total 652 _reflns_number_gt 493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0760P)^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 652 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1290 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.13958(16) 0.2500 0.72670(9) 0.0249(4) Uani 1 2 d S . . N1 N 0.0155(3) 0.2500 0.92460(19) 0.0253(7) Uani 1 2 d S . . N2 N -0.1712(4) 0.2500 0.95298(19) 0.0260(6) Uani 1 2 d S . . N3 N -0.1848(3) 0.2500 1.06098(18) 0.0253(6) Uani 1 2 d S . . N4 N -0.0080(3) 0.2500 1.10484(18) 0.0250(7) Uani 1 2 d S . . C1 C 0.1122(4) 0.2500 1.0191(2) 0.0198(7) Uani 1 2 d S . . C2 C 0.3244(5) 0.2500 1.0303(3) 0.0344(9) Uani 1 2 d S . . O1W O -0.1206(2) 0.0140(2) 0.71998(13) 0.0275(5) Uani 1 1 d . . . H1WA H -0.094(4) -0.057(4) 0.771(2) 0.041 Uiso 1 1 d . . . H1WB H -0.158(4) -0.057(4) 0.674(2) 0.041 Uiso 1 1 d . . . H2A H 0.365(7) 0.2500 1.100(5) 0.089(17) Uiso 1 2 d S . . H2B H 0.376(7) 0.149(7) 1.004(4) 0.15(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0201(7) 0.0289(8) 0.0257(7) 0.000 0.0019(4) 0.000 N1 0.0216(14) 0.0334(17) 0.0208(12) 0.000 0.0011(9) 0.000 N2 0.0204(14) 0.0339(16) 0.0237(12) 0.000 -0.0005(9) 0.000 N3 0.0214(14) 0.0334(16) 0.0213(12) 0.000 0.0001(10) 0.000 N4 0.0234(14) 0.0314(16) 0.0203(13) 0.000 -0.0012(9) 0.000 C1 0.0231(17) 0.0163(15) 0.0201(13) 0.000 -0.0017(10) 0.000 C2 0.0213(17) 0.049(3) 0.0325(19) 0.000 -0.0011(13) 0.000 O1W 0.0310(9) 0.0260(10) 0.0253(9) -0.0009(6) -0.0069(6) -0.0004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O1W 2.4403(19) 4_556 ? Na1 O1W 2.4403(19) 6_657 ? Na1 O1W 2.4568(19) . ? Na1 O1W 2.4568(19) 7_565 ? Na1 N2 2.546(3) 6_657 ? Na1 N1 2.551(3) . ? Na1 Na1 3.5255(10) 6_657 ? Na1 Na1 3.5255(10) 6_557 ? N1 C1 1.329(4) . ? N1 N2 1.345(3) . ? N2 N3 1.313(3) . ? N2 Na1 2.546(3) 6_557 ? N3 N4 1.340(3) . ? N4 C1 1.335(4) . ? C1 C2 1.483(5) . ? C2 H2A 0.89(6) . ? C2 H2B 0.86(5) . ? O1W Na1 2.4403(19) 6_557 ? O1W H1WA 0.81(3) . ? O1W H1WB 0.79(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Na1 O1W 85.63(9) 4_556 6_657 ? O1W Na1 O1W 166.34(5) 4_556 . ? O1W Na1 O1W 93.11(6) 6_657 . ? O1W Na1 O1W 93.11(6) 4_556 7_565 ? O1W Na1 O1W 166.34(5) 6_657 7_565 ? O1W Na1 O1W 84.92(9) . 7_565 ? O1W Na1 N2 82.71(6) 4_556 6_657 ? O1W Na1 N2 82.71(6) 6_657 6_657 ? O1W Na1 N2 110.65(6) . 6_657 ? O1W Na1 N2 110.65(6) 7_565 6_657 ? O1W Na1 N1 88.98(7) 4_556 . ? O1W Na1 N1 88.98(6) 6_657 . ? O1W Na1 N1 77.39(6) . . ? O1W Na1 N1 77.39(6) 7_565 . ? N2 Na1 N1 168.65(9) 6_657 . ? O1W Na1 Na1 44.14(4) 4_556 6_657 ? O1W Na1 Na1 44.14(4) 6_657 6_657 ? O1W Na1 Na1 137.12(4) . 6_657 ? O1W Na1 Na1 137.12(5) 7_565 6_657 ? N2 Na1 Na1 68.08(6) 6_657 6_657 ? N1 Na1 Na1 100.56(8) . 6_657 ? O1W Na1 Na1 129.25(5) 4_556 6_557 ? O1W Na1 Na1 129.25(5) 6_657 6_557 ? O1W Na1 Na1 43.77(4) . 6_557 ? O1W Na1 Na1 43.77(4) 7_565 6_557 ? N2 Na1 Na1 130.36(8) 6_657 6_557 ? N1 Na1 Na1 60.99(6) . 6_557 ? Na1 Na1 Na1 161.55(7) 6_657 6_557 ? C1 N1 N2 105.6(2) . . ? C1 N1 Na1 129.8(2) . . ? N2 N1 Na1 124.61(18) . . ? N3 N2 N1 108.9(2) . . ? N3 N2 Na1 144.75(18) . 6_557 ? N1 N2 Na1 106.31(16) . 6_557 ? N2 N3 N4 109.3(2) . . ? C1 N4 N3 105.4(2) . . ? N1 C1 N4 110.8(3) . . ? N1 C1 C2 125.7(3) . . ? N4 C1 C2 123.6(3) . . ? C1 C2 H2A 114(3) . . ? C1 C2 H2B 112(3) . . ? H2A C2 H2B 103(4) . . ? Na1 O1W Na1 92.10(6) 6_557 . ? Na1 O1W H1WA 112(2) 6_557 . ? Na1 O1W H1WA 103(2) . . ? Na1 O1W H1WB 113(2) 6_557 . ? Na1 O1W H1WB 134(2) . . ? H1WA O1W H1WB 103(3) . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.938 _refine_diff_density_max 0.247 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.081 #======================================================= data_3 _database_code_depnum_ccdc_archive 'CCDC 293449' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H27 Cu8 N39' _chemical_formula_weight 1298.11 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' _cell_length_a 13.959(3) _cell_length_b 13.959(3) _cell_length_c 16.292(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2749.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 3.086 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4681 _exptl_absorpt_correction_T_max 0.8865 _exptl_absorpt_process_details 'SADABS, Sheldrick 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15288 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.98 _reflns_number_total 1875 _reflns_number_gt 1518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1133P)^2^+16.4367P] 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 1875 _refine_ls_number_parameters 99 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.2355 _refine_ls_wR_factor_gt 0.2240 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.3333 0.6667 0.37020(10) 0.0153(4) Uani 1 3 d S . . Cu2 Cu 0.44469(9) 0.37383(9) 0.56017(9) 0.0397(5) Uani 1 1 d . . . N1 N 0.2127(5) 0.4471(6) 0.4718(5) 0.0331(18) Uani 1 1 d . . . N2 N 0.3105(6) 0.5311(6) 0.4441(5) 0.0344(19) Uani 1 1 d . . . N3 N 0.3895(6) 0.5162(6) 0.4697(6) 0.038(2) Uani 1 1 d . . . N4 N 0.3486(6) 0.4233(6) 0.5154(5) 0.0340(19) Uani 1 1 d . . . N5 N 0.1006(6) 0.4748(6) 0.3196(5) 0.0330(18) Uani 1 1 d . . . N6 N 0.1997(6) 0.5551(6) 0.2930(5) 0.0351(19) Uani 1 1 d . . . C1 C 0.1584(9) 0.2801(10) 0.5562(12) 0.087(6) Uani 1 1 d . . . H1A H 0.1170 0.2960 0.5954 0.131 Uiso 1 1 calc R . . H1B H 0.1976 0.2494 0.5840 0.131 Uiso 1 1 calc R . . H1C H 0.1088 0.2279 0.5166 0.131 Uiso 1 1 calc R . . C2 C 0.2380(8) 0.3828(8) 0.5141(9) 0.056(3) Uani 1 1 d . . . C3 C 0.0464(11) 0.4271(11) 0.2500 0.041(4) Uani 1 2 d S . . C4 C -0.0738(17) 0.3334(16) 0.2500 0.110(10) Uani 1 2 d S . . H4A H -0.1078 0.3329 0.1987 0.165 Uiso 0.50 1 calc PR . . H4B H -0.1130 0.3443 0.2941 0.165 Uiso 0.50 1 calc PR . . H4C H -0.0762 0.2640 0.2573 0.165 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0138(5) 0.0138(5) 0.0183(8) 0.000 0.000 0.0069(3) Cu2 0.0267(7) 0.0298(7) 0.0730(10) -0.0084(6) -0.0123(6) 0.0220(5) N1 0.012(3) 0.036(4) 0.057(5) -0.009(4) -0.005(3) 0.016(3) N2 0.022(4) 0.025(4) 0.057(6) -0.012(4) -0.009(3) 0.013(3) N3 0.018(3) 0.026(4) 0.073(6) -0.019(4) -0.015(4) 0.014(3) N4 0.026(4) 0.024(4) 0.058(6) -0.007(4) -0.007(4) 0.018(3) N5 0.014(3) 0.026(4) 0.040(5) 0.004(3) -0.011(3) -0.004(3) N6 0.024(4) 0.027(4) 0.059(5) 0.004(4) 0.003(3) 0.016(3) C1 0.023(6) 0.037(6) 0.20(2) 0.036(9) -0.006(8) 0.011(5) C2 0.016(4) 0.031(5) 0.119(11) -0.019(6) -0.017(6) 0.011(4) C3 0.024(7) 0.025(7) 0.070(11) 0.000 0.000 0.010(6) C4 0.044(12) 0.041(11) 0.20(3) 0.000 0.000 -0.011(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 Cu1 N2 2.128(8) 3_565 ? Cu1 N2 2.128(8) 2_665 ? Cu1 N2 2.128(8) . ? Cu1 N6 2.141(8) 3_565 ? Cu1 N6 2.141(8) . ? Cu1 N6 2.141(8) 2_665 ? Cu2 N4 1.933(7) . ? Cu2 N5 2.003(8) 8_556 ? Cu2 N1 2.032(7) 8_556 ? Cu2 N3 2.097(8) 7_666 ? N1 C2 1.312(14) . ? N1 N2 1.357(10) . ? N1 Cu2 2.032(7) 9_556 ? N2 N3 1.290(10) . ? N3 N4 1.350(11) . ? N3 Cu2 2.097(8) 7_666 ? N4 C2 1.352(12) . ? N5 C3 1.341(10) . ? N5 N6 1.344(10) . ? N5 Cu2 2.003(8) 9_556 ? N6 N6 1.400(17) 10_556 ? C1 C2 1.472(17) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C3 N5 1.341(10) 10_556 ? C3 C4 1.53(2) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N2 91.1(3) 3_565 2_665 ? N2 Cu1 N2 91.1(3) 3_565 . ? N2 Cu1 N2 91.1(3) 2_665 . ? N2 Cu1 N6 89.8(3) 3_565 3_565 ? N2 Cu1 N6 90.1(3) 2_665 3_565 ? N2 Cu1 N6 178.5(3) . 3_565 ? N2 Cu1 N6 90.1(3) 3_565 . ? N2 Cu1 N6 178.5(3) 2_665 . ? N2 Cu1 N6 89.8(3) . . ? N6 Cu1 N6 89.0(3) 3_565 . ? N2 Cu1 N6 178.5(3) 3_565 2_665 ? N2 Cu1 N6 89.8(3) 2_665 2_665 ? N2 Cu1 N6 90.1(3) . 2_665 ? N6 Cu1 N6 89.0(3) 3_565 2_665 ? N6 Cu1 N6 89.0(3) . 2_665 ? N4 Cu2 N5 123.4(3) . 8_556 ? N4 Cu2 N1 126.3(3) . 8_556 ? N5 Cu2 N1 98.6(3) 8_556 8_556 ? N4 Cu2 N3 111.1(3) . 7_666 ? N5 Cu2 N3 94.1(3) 8_556 7_666 ? N1 Cu2 N3 95.8(3) 8_556 7_666 ? C2 N1 N2 105.5(7) . . ? C2 N1 Cu2 135.8(7) . 9_556 ? N2 N1 Cu2 118.7(6) . 9_556 ? N3 N2 N1 109.0(7) . . ? N3 N2 Cu1 124.5(6) . . ? N1 N2 Cu1 126.6(5) . . ? N2 N3 N4 110.4(7) . . ? N2 N3 Cu2 121.8(7) . 7_666 ? N4 N3 Cu2 127.8(5) . 7_666 ? N3 N4 C2 103.8(8) . . ? N3 N4 Cu2 121.0(5) . . ? C2 N4 Cu2 135.0(7) . . ? C3 N5 N6 103.3(8) . . ? C3 N5 Cu2 135.8(7) . 9_556 ? N6 N5 Cu2 120.6(6) . 9_556 ? N5 N6 N6 108.8(5) . 10_556 ? N5 N6 Cu1 125.1(6) . . ? N6 N6 Cu1 126.0(2) 10_556 . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 N4 111.3(10) . . ? N1 C2 C1 125.5(9) . . ? N4 C2 C1 123.2(10) . . ? N5 C3 N5 115.5(12) . 10_556 ? N5 C3 C4 122.1(6) . . ? N5 C3 C4 122.1(6) 10_556 . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.459 _refine_diff_density_min -1.244 _refine_diff_density_rms 0.234 #======================================================= data_4 _database_code_depnum_ccdc_archive 'CCDC 293450' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H3 Cu2 N7' _chemical_formula_weight 252.19 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x-1/2, y-1/2, z' 'x-1/2, -y-1/2, z' _cell_length_a 15.428(4) _cell_length_b 6.1727(16) _cell_length_c 5.9765(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 569.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 7.395 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1706 _exptl_absorpt_correction_T_max 0.8662 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3235 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 28.31 _reflns_number_total 734 _reflns_number_gt 545 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0393P)^2^+0.3818P] 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 734 _refine_ls_number_parameters 61 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.38171(5) -0.01740(11) 0.0000 0.0294(3) Uani 1 2 d S . . Cu2 Cu 0.5000 -0.5000 -0.21663(11) 0.0229(2) Uani 1 2 d S . . N1 N 0.44166(18) -0.2641(4) -0.3901(4) 0.0152(6) Uani 1 1 d . . . N2 N 0.39667(19) -0.0911(5) -0.3162(5) 0.0150(7) Uani 1 1 d . . . N3 N 0.2319(3) 0.0400(7) 0.0000 0.0292(12) Uani 1 2 d S . . N4 N 0.1653(3) -0.0464(6) 0.0000 0.0173(10) Uani 1 2 d S . . N5 N 0.0962(3) -0.1387(7) 0.0000 0.0178(10) Uani 1 2 d S . . C1 C 0.3151(4) 0.2119(8) -0.5000 0.0226(12) Uani 1 2 d S . . H1A H 0.2906 0.2328 -0.6461 0.034 Uiso 0.50 1 calc PR . . H1B H 0.3501 0.3349 -0.4616 0.034 Uiso 0.50 1 calc PR . . H1C H 0.2693 0.1963 -0.3924 0.034 Uiso 0.50 1 calc PR . . C2 C 0.3698(3) 0.0126(7) -0.5000 0.0128(10) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0483(5) 0.0300(4) 0.0099(4) 0.000 0.000 0.0115(3) Cu2 0.0277(4) 0.0271(4) 0.0141(4) 0.000 0.000 0.0097(3) N1 0.0204(16) 0.0154(14) 0.0098(15) -0.0004(11) -0.0001(12) 0.0022(13) N2 0.0220(16) 0.0154(14) 0.0075(15) -0.0024(12) -0.0003(13) 0.0017(12) N3 0.020(3) 0.026(2) 0.041(3) 0.000 0.000 -0.004(2) N4 0.027(3) 0.012(2) 0.013(2) 0.000 0.000 0.004(2) N5 0.013(2) 0.023(2) 0.017(2) 0.000 0.000 0.0002(19) C1 0.028(3) 0.018(3) 0.021(3) 0.000 0.000 0.009(2) C2 0.014(2) 0.014(2) 0.011(2) 0.000 0.000 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.958(3) . ? Cu1 N2 1.958(3) 6 ? Cu1 N3 2.339(5) . ? Cu1 N5 2.363(4) 7_665 ? Cu2 N1 2.001(3) . ? Cu2 N1 2.001(3) 2_645 ? Cu2 N5 2.148(3) 3_545 ? Cu2 N5 2.148(3) 7_655 ? Cu2 Cu2 2.5894(15) 5_645 ? N1 N1 1.313(5) 6_554 ? N1 N2 1.348(4) . ? N2 C2 1.337(4) . ? N3 N4 1.157(6) . ? N4 N5 1.209(6) . ? N5 Cu2 2.148(3) 7_665 ? N5 Cu2 2.148(3) 3_445 ? N5 Cu1 2.363(4) 7_655 ? C1 C2 1.492(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N2 1.337(4) 6_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 N2 149.80(17) . 6 ? N2 Cu1 N3 98.73(9) . . ? N2 Cu1 N3 98.73(9) 6 . ? N2 Cu1 N5 102.29(9) . 7_665 ? N2 Cu1 N5 102.29(9) 6 7_665 ? N3 Cu1 N5 89.57(15) . 7_665 ? N1 Cu2 N1 117.59(15) . 2_645 ? N1 Cu2 N5 109.47(13) . 3_545 ? N1 Cu2 N5 106.94(14) 2_645 3_545 ? N1 Cu2 N5 106.94(14) . 7_655 ? N1 Cu2 N5 109.47(13) 2_645 7_655 ? N5 Cu2 N5 105.86(14) 3_545 7_655 ? N1 Cu2 Cu2 121.20(8) . 5_645 ? N1 Cu2 Cu2 121.20(8) 2_645 5_645 ? N5 Cu2 Cu2 52.93(7) 3_545 5_645 ? N5 Cu2 Cu2 52.93(7) 7_655 5_645 ? N1 N1 N2 109.11(16) 6_554 . ? N1 N1 Cu2 121.20(8) 6_554 . ? N2 N1 Cu2 129.7(2) . . ? C2 N2 N1 105.7(3) . . ? C2 N2 Cu1 130.2(2) . . ? N1 N2 Cu1 124.1(2) . . ? N4 N3 Cu1 143.8(4) . . ? N3 N4 N5 179.4(5) . . ? N4 N5 Cu2 115.0(3) . 7_665 ? N4 N5 Cu2 115.0(3) . 3_445 ? Cu2 N5 Cu2 74.14(14) 7_665 3_445 ? N4 N5 Cu1 109.8(3) . 7_655 ? Cu2 N5 Cu1 119.60(15) 7_665 7_655 ? Cu2 N5 Cu1 119.60(15) 3_445 7_655 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 N2 110.4(4) . 6_554 ? N2 C2 C1 124.8(2) . . ? N2 C2 C1 124.8(2) 6_554 . ? _diffrn_measured_fraction_theta_max 0.948 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.948 _refine_diff_density_max 0.591 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.130 #======================================================= data_5 _database_code_depnum_ccdc_archive 'CCDC 293451' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H3 Ag2 N7' _chemical_formula_weight 340.85 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbam loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z' 'x-1/2, -y-1/2, z' '-x-1/2, y-1/2, z' _cell_length_a 16.37(2) _cell_length_b 6.360(9) _cell_length_c 6.502(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 676.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 5.722 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4257 _exptl_absorpt_correction_T_max 0.8034 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _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 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 3238 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 28.07 _reflns_number_total 843 _reflns_number_gt 760 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0843P)^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 SHELXL _refine_ls_extinction_coef 0.076(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 843 _refine_ls_number_parameters 62 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1392 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.356 _refine_ls_restrained_S_all 1.356 _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 Ag1 Ag 0.37325(3) 0.00140(4) 0.0000 0.0308(3) Uani 1 2 d S . . Ag2 Ag 0.5000 -0.5000 -0.22963(10) 0.0352(3) Uani 1 2 d S . . N1 N 0.43634(13) -0.2361(3) -0.3993(3) 0.0266(6) Uani 1 1 d . . . N2 N 0.39296(14) -0.0715(4) -0.3311(3) 0.0236(6) Uani 1 1 d . . . N3 N 0.2244(2) 0.0954(6) 0.0000 0.0478(12) Uani 1 2 d S . . N4 N 0.1660(3) -0.0061(4) 0.0000 0.0267(10) Uani 1 2 d S . . N5 N 0.1059(2) -0.1110(5) 0.0000 0.0272(8) Uani 1 2 d S . . C1 C 0.3155(3) 0.2206(6) -0.5000 0.0334(10) Uani 1 2 d S . . H1A H 0.2998 0.2537 -0.6385 0.050 Uiso 0.50 1 calc PR . . H1B H 0.3458 0.3359 -0.4430 0.050 Uiso 0.50 1 calc PR . . H1C H 0.2675 0.1962 -0.4185 0.050 Uiso 0.50 1 calc PR . . C2 C 0.3672(3) 0.0286(8) -0.5000 0.0206(12) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0479(5) 0.0280(5) 0.0163(5) 0.000 0.000 0.00407(11) Ag2 0.0335(5) 0.0490(5) 0.0230(5) 0.000 0.000 0.01678(14) N1 0.0329(14) 0.0291(12) 0.0179(11) -0.0005(10) 0.0004(10) 0.0065(10) N2 0.0310(13) 0.0242(13) 0.0157(12) -0.0009(10) -0.0005(9) 0.0031(10) N3 0.026(2) 0.032(2) 0.085(4) 0.000 0.000 -0.0036(17) N4 0.025(2) 0.019(2) 0.036(3) 0.000 0.000 0.0056(11) N5 0.0236(17) 0.0238(17) 0.0341(19) 0.000 0.000 0.0015(13) C1 0.044(2) 0.029(2) 0.027(2) 0.000 0.000 0.0109(18) C2 0.024(2) 0.026(2) 0.012(3) 0.000 0.000 -0.0004(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.226(4) 6 ? Ag1 N2 2.226(4) . ? Ag1 N5 2.489(5) 3 ? Ag1 N3 2.509(5) . ? Ag2 N1 2.263(3) 2_645 ? Ag2 N1 2.263(3) . ? Ag2 N5 2.394(3) 7_655 ? Ag2 N5 2.394(3) 3_545 ? Ag2 Ag2 2.986(4) 5_645 ? N1 N1 1.310(4) 6_554 ? N1 N2 1.340(3) . ? N2 C2 1.337(4) . ? N3 N4 1.153(6) . ? N4 N5 1.189(6) . ? N5 Ag2 2.394(3) 7 ? N5 Ag2 2.394(3) 3 ? N5 Ag1 2.489(5) 3_545 ? C1 C2 1.486(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 N2 1.337(4) 6_554 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N2 150.59(14) 6 . ? N2 Ag1 N5 100.75(7) 6 3 ? N2 Ag1 N5 100.75(7) . 3 ? N2 Ag1 N3 100.98(7) 6 . ? N2 Ag1 N3 100.98(7) . . ? N5 Ag1 N3 84.10(12) 3 . ? N1 Ag2 N1 121.65(14) 2_645 . ? N1 Ag2 N5 100.92(12) 2_645 7_655 ? N1 Ag2 N5 114.75(12) . 7_655 ? N1 Ag2 N5 114.75(12) 2_645 3_545 ? N1 Ag2 N5 100.92(12) . 3_545 ? N5 Ag2 N5 102.84(14) 7_655 3_545 ? N1 Ag2 Ag2 119.18(7) 2_645 5_645 ? N1 Ag2 Ag2 119.18(7) . 5_645 ? N5 Ag2 Ag2 51.42(7) 7_655 5_645 ? N5 Ag2 Ag2 51.42(7) 3_545 5_645 ? N1 N1 N2 109.31(14) 6_554 . ? N1 N1 Ag2 119.18(7) 6_554 . ? N2 N1 Ag2 131.46(18) . . ? C2 N2 N1 105.5(3) . . ? C2 N2 Ag1 130.5(3) . . ? N1 N2 Ag1 124.02(18) . . ? N4 N3 Ag1 132.2(3) . . ? N3 N4 N5 179.9(4) . . ? N4 N5 Ag2 115.7(2) . 7 ? N4 N5 Ag2 115.7(2) . 3 ? Ag2 N5 Ag2 77.16(14) 7 3 ? N4 N5 Ag1 116.2(3) . 3_545 ? Ag2 N5 Ag1 113.04(11) 7 3_545 ? Ag2 N5 Ag1 113.04(11) 3 3_545 ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 N2 110.4(4) 6_554 . ? N2 C2 C1 124.8(2) 6_554 . ? N2 C2 C1 124.8(2) . . ? _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 28.07 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 3.396 _refine_diff_density_min -2.025 _refine_diff_density_rms 0.651 #======================================================= data_6 _database_code_depnum_ccdc_archive 'CCDC 293452' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H Cu N4' _chemical_formula_weight 132.60 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.050(6) _cell_length_b 14.647(7) _cell_length_c 14.025(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2681(2) _cell_formula_units_Z 32 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.628 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 6.291 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3023 _exptl_absorpt_correction_T_max 0.7040 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 5676 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_sigmaI/netI 0.1049 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2361 _reflns_number_gt 1560 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(9) _refine_ls_number_reflns 2361 _refine_ls_number_parameters 220 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0756 _refine_ls_wR_factor_ref 0.2006 _refine_ls_wR_factor_gt 0.1743 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.016 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 1.03747(17) 0.2500 0.0213(6) Uani 1 2 d S . . Cu2 Cu 0.40615(19) 1.0000 0.5000 0.0212(6) Uani 1 2 d S . . Cu3 Cu 0.18755(14) 0.72549(12) 0.25076(12) 0.0215(5) Uani 1 1 d . . . Cu4 Cu 0.21754(14) 0.81170(13) 0.50117(12) 0.0208(5) Uani 1 1 d . . . Cu5 Cu 0.53198(18) 0.5000 0.5000 0.0205(6) Uani 1 2 d S . . Cu6 Cu 0.5000 0.58592(17) 0.7500 0.0205(6) Uani 1 2 d S . . N1 N 0.2797(10) 0.8304(8) 0.3003(8) 0.019(3) Uani 1 1 d U . . N2 N 0.2865(9) 0.8680(8) 0.3854(8) 0.020(3) Uani 1 1 d U . . N3 N 0.3471(10) 0.9377(8) 0.3844(8) 0.018(3) Uani 1 1 d U . . N4 N 0.3889(10) 0.9468(8) 0.2962(10) 0.026(3) Uani 1 1 d U . . N5 N 0.4402(9) 0.6041(8) 0.5441(9) 0.021(3) Uani 1 1 d U . . N6 N 0.4327(9) 0.6405(8) 0.6355(8) 0.017(3) Uani 1 1 d U . . N7 N 0.3692(9) 0.7092(8) 0.6341(8) 0.016(3) Uani 1 1 d U . . N8 N 0.3294(9) 0.7219(8) 0.5465(9) 0.022(3) Uani 1 1 d U . . N9 N 0.6096(8) 0.4908(7) 0.6995(7) 0.018(3) Uani 1 1 d DU . . N10 N 0.6128(8) 0.4543(7) 0.6122(6) 0.018(3) Uani 1 1 d DU . . N11 N 0.6764(8) 0.3833(7) 0.6144(7) 0.017(3) Uani 1 1 d DU . . N12 N 0.7173(9) 0.3778(8) 0.7017(7) 0.027(3) Uani 1 1 d DU . . N13 N 0.6092(9) 0.7782(7) 0.5489(9) 0.018(3) Uani 1 1 d U . . N14 N 0.6088(9) 0.8169(8) 0.6368(8) 0.016(3) Uani 1 1 d U . . N15 N 0.5444(9) 0.8874(8) 0.6369(7) 0.018(3) Uani 1 1 d U . . N16 N 0.5024(10) 0.8974(7) 0.5496(8) 0.018(3) Uani 1 1 d U . . C1 C 0.3437(11) 0.8826(10) 0.2414(14) 0.024(4) Uani 1 1 d U . . H1A H 0.3533 0.8744 0.1762 0.029 Uiso 1 1 calc R . . C2 C 0.3772(12) 0.6536(10) 0.4997(17) 0.034(4) Uani 1 1 d U . . H2A H 0.3639 0.6433 0.4354 0.041 Uiso 1 1 calc R . . C3 C 0.6751(9) 0.4439(8) 0.7563(10) 0.022(3) Uani 1 1 d DU . . H3A H 0.6883 0.4550 0.8204 0.027 Uiso 1 1 calc R . . C4 C 0.5451(11) 0.8306(9) 0.5024(15) 0.025(3) Uani 1 1 d U . . H4A H 0.5306 0.8207 0.4383 0.030 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0322(15) 0.0205(13) 0.0111(13) 0.000 0.0017(17) 0.000 Cu2 0.0318(15) 0.0243(14) 0.0075(13) 0.0011(17) 0.000 0.000 Cu3 0.0324(12) 0.0206(10) 0.0114(10) 0.0018(16) 0.0028(8) -0.0004(7) Cu4 0.0306(12) 0.0214(10) 0.0105(10) -0.0024(8) 0.0000(16) -0.0002(7) Cu5 0.0317(16) 0.0201(13) 0.0098(13) -0.0037(17) 0.000 0.000 Cu6 0.0308(15) 0.0210(14) 0.0097(13) 0.000 -0.0016(17) 0.000 N1 0.036(6) 0.014(6) 0.008(5) 0.005(5) -0.003(5) -0.009(5) N2 0.026(6) 0.017(6) 0.016(6) 0.004(5) -0.002(5) 0.001(5) N3 0.029(6) 0.016(5) 0.009(6) 0.007(5) 0.003(5) 0.003(5) N4 0.038(6) 0.017(6) 0.022(6) 0.009(5) 0.004(6) -0.003(5) N5 0.025(6) 0.015(5) 0.023(6) -0.008(5) 0.003(5) 0.015(5) N6 0.021(6) 0.023(6) 0.007(6) -0.004(5) -0.001(4) -0.004(5) N7 0.020(6) 0.020(6) 0.007(5) 0.005(4) -0.002(4) 0.001(5) N8 0.028(6) 0.021(6) 0.015(6) 0.015(5) -0.001(5) 0.008(5) N9 0.027(5) 0.012(5) 0.015(5) -0.006(5) 0.003(5) 0.004(5) N10 0.029(6) 0.020(6) 0.005(5) -0.007(5) -0.005(5) -0.004(5) N11 0.021(6) 0.017(6) 0.013(6) 0.002(5) 0.000(5) 0.001(5) N12 0.037(6) 0.022(6) 0.022(6) -0.001(5) -0.007(6) 0.006(6) N13 0.019(6) 0.017(6) 0.019(6) -0.004(5) 0.000(5) 0.007(5) N14 0.023(6) 0.015(5) 0.011(6) 0.003(5) -0.001(5) -0.008(5) N15 0.033(6) 0.018(5) 0.003(5) 0.003(5) -0.005(5) -0.001(5) N16 0.027(5) 0.016(5) 0.010(5) 0.000(5) -0.002(5) 0.002(6) C1 0.035(7) 0.027(7) 0.011(7) -0.010(6) 0.004(6) -0.007(6) C2 0.047(8) 0.029(6) 0.027(7) -0.005(6) 0.000(7) 0.001(7) C3 0.037(7) 0.024(7) 0.005(6) 0.000(6) -0.010(6) 0.000(6) C4 0.028(7) 0.031(7) 0.016(6) -0.008(7) 0.000(6) -0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N15 2.016(11) 4_576 ? Cu1 N15 2.016(11) 2_674 ? Cu1 N4 2.070(12) . ? Cu1 N4 2.070(12) 3_655 ? Cu2 N3 2.013(12) . ? Cu2 N3 2.013(12) 4_576 ? Cu2 N16 2.079(12) 4_576 ? Cu2 N16 2.079(12) . ? Cu3 N14 1.983(12) 8_466 ? Cu3 N7 2.034(11) 6_564 ? Cu3 N12 2.075(9) 2_664 ? Cu3 N1 2.071(12) . ? Cu4 N11 1.977(9) 5_455 ? Cu4 N2 2.031(12) . ? Cu4 N13 2.057(11) 8_466 ? Cu4 N8 2.066(11) . ? Cu5 N10 2.010(8) . ? Cu5 N10 2.010(8) 4_566 ? Cu5 N5 2.035(11) 4_566 ? Cu5 N5 2.035(11) . ? Cu6 N6 1.998(12) 3_656 ? Cu6 N6 1.998(12) . ? Cu6 N9 2.118(9) 3_656 ? Cu6 N9 2.118(9) . ? N1 C1 1.401(19) . ? N1 N2 1.317(15) . ? N2 N3 1.293(15) . ? N3 N4 1.359(16) . ? N4 C1 1.351(19) . ? N5 C2 1.26(2) . ? N5 N6 1.391(16) . ? N6 N7 1.305(14) . ? N7 N8 1.347(15) . ? N7 Cu3 2.034(11) 6_565 ? N8 C2 1.35(2) . ? N9 N10 1.336(8) . ? N9 C3 1.356(9) . ? N10 N11 1.330(8) . ? N11 N12 1.338(8) . ? N11 Cu4 1.977(9) 5_545 ? N12 C3 1.352(9) . ? N12 Cu3 2.075(9) 2_665 ? N13 C4 1.309(19) . ? N13 N14 1.356(15) . ? N13 Cu4 2.057(11) 8_566 ? N14 N15 1.330(16) . ? N14 Cu3 1.983(12) 8_566 ? N15 N16 1.350(14) . ? N15 Cu1 2.016(11) 2_675 ? N16 C4 1.306(18) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? 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 N15 Cu1 N15 113.8(6) 4_576 2_674 ? N15 Cu1 N4 107.8(5) 4_576 . ? N15 Cu1 N4 113.3(5) 2_674 . ? N15 Cu1 N4 113.3(5) 4_576 3_655 ? N15 Cu1 N4 107.8(5) 2_674 3_655 ? N4 Cu1 N4 100.2(7) . 3_655 ? N3 Cu2 N3 135.0(7) . 4_576 ? N3 Cu2 N16 106.8(5) . 4_576 ? N3 Cu2 N16 100.0(5) 4_576 4_576 ? N3 Cu2 N16 100.0(5) . . ? N3 Cu2 N16 106.8(5) 4_576 . ? N16 Cu2 N16 105.7(7) 4_576 . ? N14 Cu3 N7 126.8(5) 8_466 6_564 ? N14 Cu3 N12 110.2(4) 8_466 2_664 ? N7 Cu3 N12 107.1(4) 6_564 2_664 ? N14 Cu3 N1 105.5(5) 8_466 . ? N7 Cu3 N1 97.6(5) 6_564 . ? N12 Cu3 N1 107.8(6) 2_664 . ? N11 Cu4 N2 123.2(5) 5_455 . ? N11 Cu4 N13 115.3(5) 5_455 8_466 ? N2 Cu4 N13 106.9(5) . 8_466 ? N11 Cu4 N8 106.4(5) 5_455 . ? N2 Cu4 N8 101.0(5) . . ? N13 Cu4 N8 100.6(5) 8_466 . ? N10 Cu5 N10 116.7(6) . 4_566 ? N10 Cu5 N5 107.3(5) . 4_566 ? N10 Cu5 N5 108.7(4) 4_566 4_566 ? N10 Cu5 N5 108.7(4) . . ? N10 Cu5 N5 107.3(5) 4_566 . ? N5 Cu5 N5 107.9(7) 4_566 . ? N6 Cu6 N6 132.8(7) 3_656 . ? N6 Cu6 N9 106.9(4) 3_656 3_656 ? N6 Cu6 N9 103.6(4) . 3_656 ? N6 Cu6 N9 103.6(4) 3_656 . ? N6 Cu6 N9 106.9(4) . . ? N9 Cu6 N9 97.8(6) 3_656 . ? C1 N1 N2 105.5(12) . . ? C1 N1 Cu3 123.5(10) . . ? N2 N1 Cu3 130.7(9) . . ? N3 N2 N1 111.2(11) . . ? N3 N2 Cu4 126.9(9) . . ? N1 N2 Cu4 121.7(9) . . ? N2 N3 N4 109.4(11) . . ? N2 N3 Cu2 125.7(9) . . ? N4 N3 Cu2 122.4(10) . . ? C1 N4 N3 106.0(13) . . ? C1 N4 Cu1 125.1(12) . . ? N3 N4 Cu1 129.0(10) . . ? C2 N5 N6 100.9(14) . . ? C2 N5 Cu5 131.6(14) . . ? N6 N5 Cu5 127.5(9) . . ? N7 N6 N5 109.1(10) . . ? N7 N6 Cu6 126.8(9) . . ? N5 N6 Cu6 123.8(9) . . ? N8 N7 N6 111.3(11) . . ? N8 N7 Cu3 121.9(9) . 6_565 ? N6 N7 Cu3 125.6(9) . 6_565 ? N7 N8 C2 99.5(14) . . ? N7 N8 Cu4 129.8(10) . . ? C2 N8 Cu4 130.5(13) . . ? N10 N9 C3 108.4(9) . . ? N10 N9 Cu6 126.3(7) . . ? C3 N9 Cu6 124.2(8) . . ? N9 N10 N11 108.2(7) . . ? N9 N10 Cu5 124.5(7) . . ? N11 N10 Cu5 127.2(7) . . ? N10 N11 N12 108.4(7) . . ? N10 N11 Cu4 124.5(7) . 5_545 ? N12 N11 Cu4 126.5(7) . 5_545 ? C3 N12 N11 108.2(9) . . ? C3 N12 Cu3 125.3(8) . 2_665 ? N11 N12 Cu3 125.9(8) . 2_665 ? C4 N13 N14 101.9(13) . . ? C4 N13 Cu4 130.1(11) . 8_566 ? N14 N13 Cu4 125.5(9) . 8_566 ? N15 N14 N13 109.1(11) . . ? N15 N14 Cu3 124.7(9) . 8_566 ? N13 N14 Cu3 126.2(9) . 8_566 ? N14 N15 N16 109.8(11) . . ? N14 N15 Cu1 127.3(8) . 2_675 ? N16 N15 Cu1 122.5(9) . 2_675 ? C4 N16 N15 101.8(13) . . ? C4 N16 Cu2 129.0(12) . . ? N15 N16 Cu2 128.9(9) . . ? N4 C1 N1 107.7(15) . . ? N4 C1 H1A 126.1 . . ? N1 C1 H1A 126.1 . . ? N5 C2 N8 119(2) . . ? N5 C2 H2A 120.4 . . ? N8 C2 H2A 120.4 . . ? N12 C3 N9 106.7(11) . . ? N12 C3 H3A 126.7 . . ? N9 C3 H3A 126.7 . . ? N16 C4 N13 117.3(17) . . ? N16 C4 H4A 121.4 . . ? N13 C4 H4A 121.4 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.778 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.527 #======================================================= data_7 _database_code_depnum_ccdc_archive 'CCDC 293453' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H3 Ag N4' _chemical_formula_weight 190.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.030(9) _cell_length_b 11.391(10) _cell_length_c 7.490(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.590(14) _cell_angle_gamma 90.00 _cell_volume 841.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 4.626 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3793 _exptl_absorpt_correction_T_max 0.9132 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2420 _diffrn_reflns_av_R_equivalents 0.0887 _diffrn_reflns_av_sigmaI/netI 0.1170 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 26.99 _reflns_number_total 910 _reflns_number_gt 576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0916P)^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 910 _refine_ls_number_parameters 65 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1447 _refine_ls_R_factor_gt 0.0918 _refine_ls_wR_factor_ref 0.2062 _refine_ls_wR_factor_gt 0.1814 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.12891(13) 0.11954(11) 0.1250(2) 0.0381(6) Uani 1 1 d . . . N1 N -0.0690(12) 0.1533(11) -0.0637(18) 0.024(3) Uani 1 1 d . . . N2 N -0.1451(13) 0.0740(12) -0.1699(19) 0.032(4) Uani 1 1 d . . . N3 N -0.2393(12) 0.1308(11) -0.2861(18) 0.028(3) Uani 1 1 d . . . N4 N -0.2290(12) 0.2462(10) -0.2509(18) 0.022(3) Uani 1 1 d . . . C1 C -0.1203(17) 0.2574(15) -0.120(2) 0.032(4) Uani 1 1 d . . . C2 C -0.0680(15) 0.3701(13) -0.046(2) 0.029(4) Uani 1 1 d . . . H2A H 0.0292 0.3700 -0.0295 0.043 Uiso 1 1 calc R . . H2B H -0.0950 0.3826 0.0693 0.043 Uiso 1 1 calc R . . H2C H -0.1038 0.4318 -0.1280 0.043 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 Ag1 0.0321(7) 0.0242(7) 0.0494(10) -0.0011(7) -0.0151(6) -0.0030(6) N1 0.014(6) 0.021(7) 0.032(8) 0.002(6) -0.010(6) 0.007(5) N2 0.029(8) 0.018(6) 0.042(10) 0.007(6) -0.012(7) -0.001(6) N3 0.020(6) 0.038(8) 0.024(7) -0.002(7) 0.001(6) 0.001(6) N4 0.017(6) 0.015(7) 0.028(8) -0.003(5) -0.012(6) -0.002(4) C1 0.032(9) 0.036(9) 0.029(9) -0.011(8) 0.008(8) -0.001(7) C2 0.027(8) 0.031(9) 0.024(8) -0.013(8) -0.009(7) -0.008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N4 2.178(12) 8_556 ? Ag1 N2 2.231(13) 5 ? Ag1 N1 2.248(11) . ? N1 C1 1.33(2) . ? N1 N2 1.345(19) . ? N2 N3 1.329(17) . ? N2 Ag1 2.231(13) 5 ? N3 N4 1.341(16) . ? N4 C1 1.331(18) . ? N4 Ag1 2.178(12) 8_455 ? C1 C2 1.46(2) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? 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 N4 Ag1 N2 127.3(4) 8_556 5 ? N4 Ag1 N1 125.5(4) 8_556 . ? N2 Ag1 N1 107.2(4) 5 . ? C1 N1 N2 105.4(12) . . ? C1 N1 Ag1 126.7(11) . . ? N2 N1 Ag1 126.6(10) . . ? N3 N2 N1 108.5(12) . . ? N3 N2 Ag1 127.1(10) . 5 ? N1 N2 Ag1 123.8(10) . 5 ? N2 N3 N4 109.2(12) . . ? C1 N4 N3 105.2(12) . . ? C1 N4 Ag1 129.0(10) . 8_455 ? N3 N4 Ag1 125.7(9) . 8_455 ? N1 C1 N4 111.4(14) . . ? N1 C1 C2 124.9(15) . . ? N4 C1 C2 123.7(15) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.685 _refine_diff_density_min -1.708 _refine_diff_density_rms 0.302 #======================================================= data_8 _database_code_depnum_ccdc_archive 'CCDC 293454' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H7 Ag N4' _chemical_formula_weight 219.01 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M C222(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.3192(5) _cell_length_b 24.9328(7) _cell_length_c 15.1064(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3886.7(4) _cell_formula_units_Z 24 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour grey _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 3.019 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4853 _exptl_absorpt_correction_T_max 0.7522 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14253 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4416 _reflns_number_gt 4139 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0575P)^2^+0.9421P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(5) _refine_ls_number_reflns 4416 _refine_ls_number_parameters 263 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.71297(4) 0.327687(15) 1.01099(3) 0.04521(11) Uani 1 1 d . . . Ag2 Ag 0.34575(4) 0.321582(16) 1.04485(3) 0.04548(12) Uani 1 1 d . . . Ag3 Ag 0.43857(6) 0.540681(19) 0.85164(4) 0.06234(16) Uani 1 1 d . . . N1 N 0.6352(4) 0.19767(17) 0.9939(4) 0.0482(11) Uani 1 1 d . . . N2 N 0.5902(4) 0.24704(17) 1.0033(3) 0.0422(9) Uani 1 1 d . . . N3 N 0.4638(4) 0.24564(17) 1.0139(3) 0.0423(10) Uani 1 1 d . . . N4 N 0.4238(4) 0.19449(16) 1.0097(3) 0.0435(10) Uani 1 1 d . . . N5 N 0.5808(4) 0.39341(17) 0.9566(3) 0.0459(10) Uani 1 1 d . B . N6 N 0.3968(5) 0.4345(2) 0.9467(5) 0.0640(15) Uani 1 1 d . . . N7 N 0.4523(5) 0.39157(18) 0.9755(4) 0.0512(12) Uani 1 1 d . . . N8 N 0.4857(5) 0.46574(19) 0.9071(4) 0.0560(13) Uani 1 1 d . B . N9 N 0.3054(5) 0.65084(18) 0.6642(3) 0.0519(12) Uani 1 1 d . . . N10 N 0.3395(6) 0.60137(19) 0.6922(3) 0.0554(13) Uani 1 1 d . . . N11 N 0.3511(5) 0.60383(17) 0.7779(3) 0.0486(11) Uani 1 1 d . . . N12 N 0.3323(5) 0.65377(17) 0.8074(3) 0.0500(12) Uani 1 1 d . . . C1 C 0.5321(5) 0.16607(19) 0.9985(5) 0.0525(14) Uani 1 1 d D . . C2 C 0.5441(8) 0.1055(2) 0.9951(6) 0.080(2) Uani 0.50 1 d PDU A -1 H2A H 0.4656 0.0893 1.0181 0.095 Uiso 0.50 1 calc PR A -1 H2B H 0.6159 0.0941 1.0321 0.095 Uiso 0.50 1 calc PR A -1 C3 C 0.567(3) 0.0863(5) 0.9006(9) 0.105(5) Uani 0.50 1 d PDU A -1 H3A H 0.6471 0.1013 0.8785 0.126 Uiso 0.50 1 calc PR A -1 H3B H 0.4968 0.0991 0.8631 0.126 Uiso 0.50 1 calc PR A -1 C4 C 0.573(3) 0.0253(5) 0.8962(13) 0.115(5) Uani 0.50 1 d PDU A -1 H4A H 0.5887 0.0143 0.8363 0.173 Uiso 0.50 1 calc PR A -1 H4B H 0.4919 0.0105 0.9160 0.173 Uiso 0.50 1 calc PR A -1 H4C H 0.6416 0.0126 0.9335 0.173 Uiso 0.50 1 calc PR A -1 C2' C 0.5441(8) 0.1055(2) 0.9951(6) 0.080(2) Uani 0.50 1 d P A -2 H2C H 0.6344 0.0960 0.9861 0.095 Uiso 0.50 1 calc PR A -2 H2D H 0.5172 0.0907 1.0516 0.095 Uiso 0.50 1 calc PR A -2 C3' C 0.4637(18) 0.0804(5) 0.9223(9) 0.105(5) Uani 0.50 1 d PD A -2 H3C H 0.3734 0.0901 0.9304 0.126 Uiso 0.50 1 calc PR A -2 H3D H 0.4704 0.0417 0.9257 0.126 Uiso 0.50 1 calc PR A -2 C4' C 0.510(2) 0.0993(8) 0.8315(8) 0.115(5) Uani 0.50 1 d PD A -2 H4D H 0.4587 0.0823 0.7863 0.173 Uiso 0.50 1 calc PR A -2 H4E H 0.5991 0.0901 0.8238 0.173 Uiso 0.50 1 calc PR A -2 H4F H 0.4995 0.1375 0.8272 0.173 Uiso 0.50 1 calc PR A -2 C5 C 0.5976(6) 0.4390(2) 0.9151(4) 0.0531(14) Uani 1 1 d D . . C6 C 0.7260(8) 0.4593(4) 0.8797(6) 0.094(3) Uani 0.50 1 d PDU B -1 H6A H 0.7795 0.4710 0.9289 0.112 Uiso 0.50 1 calc PR B -1 H6B H 0.7104 0.4902 0.8420 0.112 Uiso 0.50 1 calc PR B -1 C7 C 0.7984(18) 0.4168(9) 0.8273(15) 0.153(8) Uani 0.50 1 d PDU B -1 H7A H 0.7785 0.3816 0.8510 0.184 Uiso 0.50 1 calc PR B -1 H7B H 0.8910 0.4226 0.8330 0.184 Uiso 0.50 1 calc PR B -1 C8 C 0.760(6) 0.4191(19) 0.7294(13) 0.29(2) Uani 0.50 1 d PDU B -1 H8A H 0.8096 0.3931 0.6969 0.430 Uiso 0.50 1 calc PR B -1 H8B H 0.7776 0.4542 0.7065 0.430 Uiso 0.50 1 calc PR B -1 H8C H 0.6695 0.4113 0.7235 0.430 Uiso 0.50 1 calc PR B -1 C6' C 0.7260(8) 0.4593(4) 0.8797(6) 0.094(3) Uani 0.50 1 d P B -2 H6C H 0.7966 0.4427 0.9119 0.112 Uiso 0.50 1 calc PR B -2 H6D H 0.7317 0.4978 0.8882 0.112 Uiso 0.50 1 calc PR B -2 C7' C 0.738(2) 0.4460(14) 0.7803(9) 0.153(8) Uani 0.50 1 d PD B -2 H7C H 0.7196 0.4083 0.7708 0.184 Uiso 0.50 1 calc PR B -2 H7D H 0.6749 0.4668 0.7470 0.184 Uiso 0.50 1 calc PR B -2 C8' C 0.875(3) 0.459(2) 0.7477(18) 0.29(2) Uani 0.50 1 d PD B -2 H8D H 0.8803 0.4524 0.6853 0.430 Uiso 0.50 1 calc PR B -2 H8E H 0.9363 0.4369 0.7782 0.430 Uiso 0.50 1 calc PR B -2 H8F H 0.8937 0.4961 0.7594 0.430 Uiso 0.50 1 calc PR B -2 C9 C 0.2989(6) 0.6804(2) 0.7339(4) 0.0531(14) Uani 1 1 d D . . C10 C 0.2597(8) 0.7391(2) 0.7344(6) 0.080(2) Uani 0.50 1 d PDU C -1 H10A H 0.2945 0.7569 0.6825 0.096 Uiso 0.50 1 calc PR C -1 H10B H 0.2947 0.7566 0.7865 0.096 Uiso 0.50 1 calc PR C -1 C11 C 0.1096(11) 0.7437(6) 0.735(2) 0.152(7) Uani 0.50 1 d PDU C -1 H11A H 0.0743 0.7247 0.6839 0.182 Uiso 0.50 1 calc PR C -1 H11B H 0.0750 0.7275 0.7879 0.182 Uiso 0.50 1 calc PR C -1 C12 C 0.070(2) 0.8030(8) 0.730(3) 0.187(11) Uani 0.50 1 d PDU C -1 H12A H -0.0229 0.8056 0.7283 0.280 Uiso 0.50 1 calc PR C -1 H12B H 0.1061 0.8191 0.6782 0.280 Uiso 0.50 1 calc PR C -1 H12C H 0.1016 0.8213 0.7819 0.280 Uiso 0.50 1 calc PR C -1 C10' C 0.2597(8) 0.7391(2) 0.7344(6) 0.080(2) Uani 0.50 1 d P C -2 H10C H 0.2023 0.7463 0.7838 0.096 Uiso 0.50 1 calc PR C -2 H10D H 0.2146 0.7480 0.6800 0.096 Uiso 0.50 1 calc PR C -2 C11' C 0.3860(16) 0.7732(5) 0.743(2) 0.152(7) Uani 0.50 1 d PD C -2 H11C H 0.4334 0.7629 0.7957 0.182 Uiso 0.50 1 calc PR C -2 H11D H 0.4413 0.7674 0.6919 0.182 Uiso 0.50 1 calc PR C -2 C12' C 0.346(3) 0.8326(5) 0.749(3) 0.187(11) Uani 0.50 1 d PD C -2 H12D H 0.4223 0.8545 0.7545 0.280 Uiso 0.50 1 calc PR C -2 H12E H 0.2910 0.8379 0.7989 0.280 Uiso 0.50 1 calc PR C -2 H12F H 0.3006 0.8425 0.6957 0.280 Uiso 0.50 1 calc PR C -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 Ag1 0.03478(19) 0.03476(19) 0.0661(2) -0.00037(16) -0.00126(17) 0.00491(16) Ag2 0.0356(2) 0.0360(2) 0.0648(2) -0.00315(17) 0.00219(17) -0.00078(16) Ag3 0.0790(4) 0.0409(2) 0.0671(3) 0.0182(2) 0.0088(3) 0.0210(2) N1 0.031(2) 0.033(2) 0.081(3) -0.008(2) 0.008(2) 0.0011(17) N2 0.031(2) 0.0314(19) 0.064(2) -0.0050(19) -0.001(2) -0.0037(16) N3 0.030(2) 0.032(2) 0.065(3) -0.0094(19) 0.0017(19) -0.0005(16) N4 0.031(2) 0.031(2) 0.068(3) -0.0060(19) 0.006(2) -0.0006(17) N5 0.032(2) 0.036(2) 0.069(3) 0.015(2) 0.001(2) 0.0027(17) N6 0.043(3) 0.055(3) 0.095(4) 0.025(3) 0.009(3) 0.013(2) N7 0.041(3) 0.036(2) 0.076(3) 0.014(2) 0.005(2) 0.0029(19) N8 0.048(3) 0.037(2) 0.083(4) 0.020(2) 0.009(3) 0.008(2) N9 0.059(3) 0.039(2) 0.057(3) 0.004(2) -0.009(2) 0.011(2) N10 0.069(4) 0.035(2) 0.062(3) -0.003(2) -0.005(3) 0.013(2) N11 0.055(3) 0.034(2) 0.057(3) 0.0048(18) 0.005(2) 0.010(2) N12 0.064(3) 0.032(2) 0.054(2) -0.0032(18) -0.002(2) 0.010(2) C1 0.034(3) 0.032(3) 0.092(4) -0.008(3) 0.006(3) 0.001(2) C2 0.063(4) 0.045(3) 0.130(6) -0.002(4) 0.008(4) 0.000(3) C3 0.116(9) 0.079(7) 0.120(8) -0.013(6) 0.006(8) 0.005(7) C4 0.119(9) 0.085(7) 0.141(9) -0.026(7) 0.015(8) 0.001(7) C2' 0.063(4) 0.045(3) 0.130(6) -0.002(4) 0.008(4) 0.000(3) C3' 0.116(9) 0.079(7) 0.120(8) -0.013(6) 0.006(8) 0.005(7) C4' 0.119(9) 0.085(7) 0.141(9) -0.026(7) 0.015(8) 0.001(7) C5 0.043(3) 0.045(3) 0.071(4) 0.018(3) 0.003(3) -0.005(2) C6 0.071(5) 0.080(5) 0.130(6) 0.038(5) 0.017(5) 0.000(4) C7 0.135(11) 0.171(12) 0.155(11) 0.028(9) 0.024(9) -0.013(9) C8 0.29(2) 0.29(2) 0.28(2) -0.003(10) -0.005(10) 0.003(10) C6' 0.071(5) 0.080(5) 0.130(6) 0.038(5) 0.017(5) 0.000(4) C7' 0.135(11) 0.171(12) 0.155(11) 0.028(9) 0.024(9) -0.013(9) C8' 0.29(2) 0.29(2) 0.28(2) -0.003(10) -0.005(10) 0.003(10) C9 0.066(4) 0.037(3) 0.057(3) 0.004(2) -0.006(3) 0.008(3) C10 0.106(6) 0.051(3) 0.083(4) 0.001(3) -0.015(4) 0.014(4) C11 0.164(10) 0.144(11) 0.147(9) -0.003(9) -0.016(9) 0.018(9) C12 0.198(14) 0.174(13) 0.189(13) 0.009(9) 0.000(10) 0.007(9) C10' 0.106(6) 0.051(3) 0.083(4) 0.001(3) -0.015(4) 0.014(4) C11' 0.164(10) 0.144(11) 0.147(9) -0.003(9) -0.016(9) 0.018(9) C12' 0.198(14) 0.174(13) 0.189(13) 0.009(9) 0.000(10) 0.007(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 Ag1 N4 2.266(4) 8_557 ? Ag1 N5 2.285(4) . ? Ag1 N2 2.380(4) . ? Ag1 N9 2.383(5) 2_665 ? Ag2 N3 2.300(4) . ? Ag2 N1 2.301(4) 8_457 ? Ag2 N7 2.314(5) . ? Ag2 N12 2.319(5) 4_567 ? Ag3 N8 2.105(4) . ? Ag3 N11 2.129(4) . ? Ag3 Ag3 3.3222(11) 3_656 ? N1 N2 1.323(6) . ? N1 C1 1.325(7) . ? N1 Ag2 2.301(4) 8_557 ? N2 N3 1.314(6) . ? N3 N4 1.342(6) . ? N4 C1 1.334(7) . ? N4 Ag1 2.266(4) 8_457 ? N5 C5 1.311(7) . ? N5 N7 1.356(6) . ? N6 N7 1.290(7) . ? N6 N8 1.344(7) . ? N8 C5 1.338(8) . ? N9 C9 1.287(7) . ? N9 N10 1.351(6) . ? N9 Ag1 2.383(5) 2_664 ? N10 N11 1.302(7) . ? N11 N12 1.337(6) . ? N12 C9 1.339(7) . ? N12 Ag2 2.319(5) 4_567 ? C1 C2 1.517(6) . ? C2 C3 1.523(9) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.526(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C3' C4' 1.526(10) . ? C3' H3C 0.9700 . ? C3' H3D 0.9700 . ? C4' H4D 0.9600 . ? C4' H4E 0.9600 . ? C4' H4F 0.9600 . ? C5 C6 1.516(7) . ? C6 C7 1.520(10) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.531(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C7' C8' 1.532(10) . ? C7' H7C 0.9700 . ? C7' H7D 0.9700 . ? C8' H8D 0.9600 . ? C8' H8E 0.9600 . ? C8' H8F 0.9600 . ? C9 C10 1.519(6) . ? C10 C11 1.553(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.535(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C11' C12' 1.539(10) . ? C11' H11C 0.9700 . ? C11' H11D 0.9700 . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? 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 N4 Ag1 N5 134.31(17) 8_557 . ? N4 Ag1 N2 107.36(15) 8_557 . ? N5 Ag1 N2 105.70(17) . . ? N4 Ag1 N9 105.36(18) 8_557 2_665 ? N5 Ag1 N9 98.07(18) . 2_665 ? N2 Ag1 N9 101.24(17) . 2_665 ? N3 Ag2 N1 106.07(15) . 8_457 ? N3 Ag2 N7 106.09(16) . . ? N1 Ag2 N7 119.41(17) 8_457 . ? N3 Ag2 N12 116.47(18) . 4_567 ? N1 Ag2 N12 104.09(19) 8_457 4_567 ? N7 Ag2 N12 105.33(18) . 4_567 ? N8 Ag3 N11 164.3(2) . . ? N8 Ag3 Ag3 106.24(16) . 3_656 ? N11 Ag3 Ag3 71.24(13) . 3_656 ? N2 N1 C1 105.4(4) . . ? N2 N1 Ag2 123.6(3) . 8_557 ? C1 N1 Ag2 130.3(3) . 8_557 ? N3 N2 N1 109.7(4) . . ? N3 N2 Ag1 123.0(3) . . ? N1 N2 Ag1 127.2(3) . . ? N2 N3 N4 109.0(4) . . ? N2 N3 Ag2 121.9(3) . . ? N4 N3 Ag2 129.0(3) . . ? C1 N4 N3 104.6(4) . . ? C1 N4 Ag1 131.1(3) . 8_457 ? N3 N4 Ag1 122.3(3) . 8_457 ? C5 N5 N7 105.0(4) . . ? C5 N5 Ag1 135.7(4) . . ? N7 N5 Ag1 118.9(3) . . ? N7 N6 N8 109.2(5) . . ? N6 N7 N5 109.6(4) . . ? N6 N7 Ag2 124.6(4) . . ? N5 N7 Ag2 125.8(3) . . ? C5 N8 N6 105.1(4) . . ? C5 N8 Ag3 132.6(4) . . ? N6 N8 Ag3 122.3(4) . . ? C9 N9 N10 106.3(5) . . ? C9 N9 Ag1 131.5(4) . 2_664 ? N10 N9 Ag1 122.0(4) . 2_664 ? N11 N10 N9 107.0(5) . . ? N10 N11 N12 111.2(4) . . ? N10 N11 Ag3 121.6(4) . . ? N12 N11 Ag3 125.2(4) . . ? N11 N12 C9 102.8(4) . . ? N11 N12 Ag2 124.0(3) . 4_567 ? C9 N12 Ag2 133.0(4) . 4_567 ? N1 C1 N4 111.3(4) . . ? N1 C1 C2 121.7(5) . . ? N4 C1 C2 127.0(5) . . ? C1 C2 C3 110.8(7) . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 111.1(9) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C4' C3' H3C 109.5 . . ? C4' C3' H3D 109.5 . . ? H3C C3' H3D 108.1 . . ? C3' C4' H4D 109.5 . . ? C3' C4' H4E 109.5 . . ? H4D C4' H4E 109.5 . . ? C3' C4' H4F 109.5 . . ? H4D C4' H4F 109.5 . . ? H4E C4' H4F 109.5 . . ? N5 C5 N8 111.2(5) . . ? N5 C5 C6 125.0(6) . . ? N8 C5 C6 123.8(5) . . ? C5 C6 C7 112.4(9) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? C6 C7 C8 110.6(10) . . ? C6 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C8' C7' H7C 109.7 . . ? C8' C7' H7D 109.7 . . ? H7C C7' H7D 108.2 . . ? C7' C8' H8D 109.5 . . ? C7' C8' H8E 109.5 . . ? H8D C8' H8E 109.5 . . ? C7' C8' H8F 109.5 . . ? H8D C8' H8F 109.5 . . ? H8E C8' H8F 109.5 . . ? N9 C9 N12 112.5(4) . . ? N9 C9 C10 124.7(6) . . ? N12 C9 C10 122.8(6) . . ? C9 C10 C11 109.7(7) . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10B 109.7 . . ? C11 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C12 C11 C10 109.7(9) . . ? C12 C11 H11A 109.7 . . ? C10 C11 H11A 109.7 . . ? C12 C11 H11B 109.7 . . ? C10 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C12' C11' H11C 110.1 . . ? C12' C11' H11D 110.1 . . ? H11C C11' H11D 108.5 . . ? C11' C12' H12D 109.5 . . ? C11' C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C11' C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.989 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.134 #======================================================= data_9 _database_code_depnum_ccdc_archive 'CCDC 293455' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H4 Ag N5' _chemical_formula_weight 254.01 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.2687(8) _cell_length_b 7.8594(11) _cell_length_c 8.0612(11) _cell_angle_alpha 75.166(2) _cell_angle_beta 76.621(2) _cell_angle_gamma 68.327(2) _cell_volume 352.62(8) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellowish _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 244 _exptl_absorpt_coefficient_mu 2.796 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4589 _exptl_absorpt_correction_T_max 0.7674 _exptl_absorpt_process_details 'SADABS, Sheldrick, 1997' _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex CCD Diffractometer' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 2828 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 26.98 _reflns_number_total 1468 _reflns_number_gt 1332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0362P)^2^+0.4568P] 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 1468 _refine_ls_number_parameters 109 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0745 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Ag1 Ag 0.21956(5) 0.64660(4) 0.39556(4) 0.04724(15) Uani 1 1 d . . . N1 N 0.3512(5) 1.2719(4) -0.1152(4) 0.0333(7) Uani 1 1 d . . . N2 N 0.4034(5) 1.3687(4) -0.2732(4) 0.0356(7) Uani 1 1 d . . . N3 N 0.2142(5) 1.4531(4) -0.3470(4) 0.0318(6) Uani 1 1 d . . . N4 N 0.0346(5) 1.4124(4) -0.2398(4) 0.0302(6) Uani 1 1 d . . . N5 N 0.0153(5) 0.9633(4) 0.3009(4) 0.0333(7) Uani 1 1 d . . . C1 C 0.1252(6) 1.3014(4) -0.0996(4) 0.0258(6) Uani 1 1 d . . . C2 C -0.0039(6) 1.2131(4) 0.0534(4) 0.0256(6) Uani 1 1 d . . . C3 C -0.2426(6) 1.2739(5) 0.0891(5) 0.0324(7) Uani 1 1 d . . . H3A H -0.3297 1.3766 0.0176 0.039 Uiso 1 1 calc R . . C4 C -0.3517(7) 1.1803(6) 0.2328(5) 0.0387(8) Uani 1 1 d . . . H4A H -0.5128 1.2196 0.2600 0.046 Uiso 1 1 calc R . . C5 C -0.2170(7) 1.0283(5) 0.3343(5) 0.0373(8) Uani 1 1 d . . . H5A H -0.2910 0.9672 0.4316 0.045 Uiso 1 1 calc R . . C6 C 0.1187(6) 1.0559(5) 0.1627(4) 0.0290(7) Uani 1 1 d . . . H6A H 0.2801 1.0136 0.1384 0.035 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 Ag1 0.03461(19) 0.0550(2) 0.0436(2) 0.02691(15) -0.01664(14) -0.02285(15) N1 0.0275(15) 0.0368(16) 0.0303(15) 0.0109(12) -0.0088(12) -0.0134(12) N2 0.0272(15) 0.0387(17) 0.0343(15) 0.0126(13) -0.0098(12) -0.0131(13) N3 0.0291(15) 0.0351(16) 0.0274(14) 0.0114(12) -0.0090(12) -0.0150(12) N4 0.0261(14) 0.0345(15) 0.0274(14) 0.0096(12) -0.0080(11) -0.0150(12) N5 0.0358(16) 0.0327(15) 0.0265(14) 0.0075(12) -0.0063(13) -0.0133(13) C1 0.0258(16) 0.0242(15) 0.0250(15) 0.0036(12) -0.0072(13) -0.0090(12) C2 0.0269(16) 0.0262(15) 0.0232(15) 0.0023(12) -0.0054(12) -0.0118(13) C3 0.0275(17) 0.0319(18) 0.0325(18) 0.0028(14) -0.0054(14) -0.0091(14) C4 0.0266(18) 0.044(2) 0.040(2) -0.0036(17) 0.0012(16) -0.0121(15) C5 0.0345(19) 0.041(2) 0.0297(18) 0.0042(15) 0.0028(15) -0.0170(16) C6 0.0255(16) 0.0309(17) 0.0282(16) 0.0018(13) -0.0063(13) -0.0101(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N3 2.238(3) 1_546 ? Ag1 N2 2.312(3) 2_675 ? Ag1 N5 2.354(3) . ? Ag1 N4 2.469(3) 2_575 ? N1 C1 1.329(4) . ? N1 N2 1.342(4) . ? N2 N3 1.321(4) . ? N2 Ag1 2.312(3) 2_675 ? N3 N4 1.339(4) . ? N3 Ag1 2.238(3) 1_564 ? N4 C1 1.337(4) . ? N4 Ag1 2.469(3) 2_575 ? N5 C6 1.338(4) . ? N5 C5 1.339(5) . ? C1 C2 1.474(4) . ? C2 C3 1.376(5) . ? C2 C6 1.395(5) . ? C3 C4 1.386(5) . ? C3 H3A 0.9300 . ? C4 C5 1.372(6) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? 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 N3 Ag1 N2 110.44(11) 1_546 2_675 ? N3 Ag1 N5 133.49(11) 1_546 . ? N2 Ag1 N5 101.38(10) 2_675 . ? N3 Ag1 N4 105.30(10) 1_546 2_575 ? N2 Ag1 N4 121.36(11) 2_675 2_575 ? N5 Ag1 N4 84.65(10) . 2_575 ? C1 N1 N2 104.4(3) . . ? N3 N2 N1 109.6(3) . . ? N3 N2 Ag1 127.7(2) . 2_675 ? N1 N2 Ag1 122.4(2) . 2_675 ? N2 N3 N4 109.4(3) . . ? N2 N3 Ag1 121.1(2) . 1_564 ? N4 N3 Ag1 129.4(2) . 1_564 ? C1 N4 N3 104.4(3) . . ? C1 N4 Ag1 126.0(2) . 2_575 ? N3 N4 Ag1 112.2(2) . 2_575 ? C6 N5 C5 117.3(3) . . ? C6 N5 Ag1 117.3(2) . . ? C5 N5 Ag1 120.5(2) . . ? N1 C1 N4 112.3(3) . . ? N1 C1 C2 122.7(3) . . ? N4 C1 C2 125.0(3) . . ? C3 C2 C6 118.1(3) . . ? C3 C2 C1 122.6(3) . . ? C6 C2 C1 119.2(3) . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3A 120.4 . . ? C4 C3 H3A 120.4 . . ? C5 C4 C3 118.6(3) . . ? C5 C4 H4A 120.7 . . ? C3 C4 H4A 120.7 . . ? N5 C5 C4 123.6(3) . . ? N5 C5 H5A 118.2 . . ? C4 C5 H5A 118.2 . . ? N5 C6 C2 123.1(3) . . ? N5 C6 H6A 118.4 . . ? C2 C6 H6A 118.4 . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 26.98 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 1.082 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.103 #=======================================================