# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- Crystallographic_CIF.txt' _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chi Zhang' _publ_contact_author_email chizhang@ujs.edu.cn _publ_section_title ; Solvent-induced syntheses of 2D/3D [AgSCN]n-based supramolecular isomers with unusual topologies: structural, theoretical and nonlinear optical studies ; loop_ _publ_author_name 'Jianghua Li.' 'Suci Meng.' 'Yinglin Song.' 'Jinfang Zhang.' ; Zhipeng Huang ; 'Huajian Zhao.' 'Hongyang Wei.' 'Wenjiang Huang.' 'Marie P. Cifuentes' ; M.G.Humphrey ; 'Chi Zhang.' #---------------------------------------------------------- data_1 _database_code_depnum_ccdc_archive 'CCDC 788744' #TrackingRef '- Crystallographic_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H12 Ag N5 S' _chemical_formula_weight 306.16 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' Ag Ag -0.8971 1.1015 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pmc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, z' 'x, -y, z+1/2' _cell_length_a 6.2611(13) _cell_length_b 6.4887(13) _cell_length_c 12.483(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 507.14(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2276 _cell_measurement_theta_min 3.1395 _cell_measurement_theta_max 31.1250 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.005 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 304 _exptl_absorpt_coefficient_mu 2.160 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.3349 _exptl_absorpt_correction_T_max 0.5649 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type CCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3780 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0173 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1236 _reflns_number_gt 1229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear(Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear(Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.0655P] 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 0.074(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1236 _refine_ls_number_parameters 89 _refine_ls_number_restraints 67 _refine_ls_R_factor_all 0.0190 _refine_ls_R_factor_gt 0.0190 _refine_ls_wR_factor_ref 0.0534 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.119 _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 Ag1A Ag 0.0000 -0.9231(16) -0.4537(12) 0.0310(6) Uani 0.50 2 d SPU . . Ag1B Ag 0.0000 -0.9466(16) -0.4480(13) 0.0368(14) Uani 0.50 2 d SPU . . S1A S 0.0000 -0.6608(16) -0.6152(9) 0.0298(9) Uani 0.50 2 d SPU . . S1B S 0.0000 -0.6710(19) -0.5959(9) 0.044(2) Uani 0.50 2 d SPU . . N1 N 0.0000 -0.2687(6) -0.5052(3) 0.0489(9) Uani 1 2 d SU . . N2 N -0.3112(3) -0.8531(3) -0.35500(15) 0.0280(4) Uani 1 1 d U . . N3 N -0.5000 -0.5522(4) -0.2776(3) 0.0358(7) Uani 1 2 d SU . . N4 N -0.5000 -0.8957(7) -0.1874(3) 0.0442(8) Uani 1 2 d SU . . C2 C -0.5000 -0.6641(8) -0.1748(3) 0.0470(10) Uani 1 2 d SU . . H2A H -0.6251 -0.6237 -0.1340 0.056 Uiso 0.50 1 calc PR . . H2B H -0.3749 -0.6237 -0.1340 0.056 Uiso 0.50 1 calc PR . . C1 C 0.0000 -0.4340(4) -0.5452(3) 0.0294(7) Uani 1 2 d SU . . C3 C -0.3185(4) -0.6197(4) -0.3371(2) 0.0341(5) Uani 1 1 d U . . H3A H -0.1900 -0.5779 -0.2995 0.041 Uiso 1 1 calc R . . H3B H -0.3186 -0.5514 -0.4063 0.041 Uiso 1 1 calc R . . C4 C -0.5000 -0.9159(5) -0.4137(3) 0.0295(7) Uani 1 2 d SU . . H4A H -0.5000 -1.0643 -0.4230 0.035 Uiso 1 2 calc SR . . H4B H -0.5000 -0.8525 -0.4841 0.035 Uiso 1 2 calc SR . . C5 C -0.3179(5) -0.9574(5) -0.2486(2) 0.0389(6) Uani 1 1 d U . . H5A H -0.3218 -1.1055 -0.2591 0.047 Uiso 1 1 calc R . . H5B H -0.1890 -0.9245 -0.2090 0.047 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 Ag1A 0.0270(6) 0.0260(17) 0.0400(11) -0.0007(15) 0.000 0.000 Ag1B 0.0322(7) 0.0275(19) 0.051(4) -0.0101(18) 0.000 0.000 S1A 0.0491(19) 0.0238(15) 0.016(3) 0.0024(17) 0.000 0.000 S1B 0.080(3) 0.034(2) 0.018(4) 0.0015(19) 0.000 0.000 N1 0.056(2) 0.0314(15) 0.060(2) -0.0022(14) 0.000 0.000 N2 0.0189(9) 0.0353(10) 0.0299(8) -0.0014(7) 0.0004(7) 0.0022(8) N3 0.0213(15) 0.0370(17) 0.0492(18) -0.0151(12) 0.000 0.000 N4 0.0266(16) 0.077(2) 0.0289(13) 0.0105(15) 0.000 0.000 C2 0.0265(17) 0.081(3) 0.0336(16) -0.0195(18) 0.000 0.000 C1 0.0261(17) 0.0257(16) 0.0365(17) 0.0040(11) 0.000 0.000 C3 0.0219(11) 0.0338(10) 0.0466(12) -0.0048(10) 0.0030(9) -0.0038(10) C4 0.0215(16) 0.0363(17) 0.0307(13) -0.0068(11) 0.000 0.000 C5 0.0253(13) 0.0560(17) 0.0353(12) 0.0126(9) -0.0027(10) 0.0067(10) _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 Ag1A N1 2.333(12) 1_545 ? Ag1A N2 2.350(9) 3 ? Ag1A N2 2.350(9) . ? Ag1A S1B 2.414(16) . ? Ag1A S1A 2.638(16) . ? Ag1B N1 2.209(13) 1_545 ? Ag1B N2 2.348(9) 3 ? Ag1B N2 2.348(9) . ? Ag1B S1B 2.570(17) . ? Ag1B S1A 2.791(17) . ? S1A C1 1.711(11) . ? S1B C1 1.663(13) . ? N1 C1 1.183(5) . ? N1 Ag1B 2.209(13) 1_565 ? N1 Ag1A 2.333(12) 1_565 ? N2 C4 1.449(3) . ? N2 C5 1.492(3) . ? N2 C3 1.531(3) . ? N3 C3 1.427(3) 3_455 ? N3 C3 1.427(3) . ? N3 C2 1.475(6) . ? N4 C5 1.429(4) 3_455 ? N4 C5 1.429(4) . ? N4 C2 1.511(7) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.449(3) 3_455 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1A N2 109.3(3) 1_545 3 ? N1 Ag1A N2 109.3(3) 1_545 . ? N2 Ag1A N2 112.0(6) 3 . ? N1 Ag1A S1B 116.7(7) 1_545 . ? N2 Ag1A S1B 104.8(3) 3 . ? N2 Ag1A S1B 104.8(3) . . ? N1 Ag1A S1A 114.2(6) 1_545 . ? N2 Ag1A S1A 106.0(3) 3 . ? N2 Ag1A S1A 106.0(3) . . ? S1B Ag1A S1A 2.5(5) . . ? N1 Ag1B N2 113.8(3) 1_545 3 ? N1 Ag1B N2 113.8(3) 1_545 . ? N2 Ag1B N2 112.2(6) 3 . ? N1 Ag1B S1B 115.2(7) 1_545 . ? N2 Ag1B S1B 100.1(3) 3 . ? N2 Ag1B S1B 100.1(3) . . ? N1 Ag1B S1A 112.8(7) 1_545 . ? N2 Ag1B S1A 101.4(3) 3 . ? N2 Ag1B S1A 101.4(3) . . ? S1B Ag1B S1A 2.5(5) . . ? C1 S1A Ag1A 99.5(6) . . ? C1 S1A Ag1B 101.0(6) . . ? Ag1A S1A Ag1B 1.5(6) . . ? C1 S1B Ag1A 110.3(7) . . ? C1 S1B Ag1B 111.7(6) . . ? Ag1A S1B Ag1B 1.4(7) . . ? C1 N1 Ag1B 173.8(5) . 1_565 ? C1 N1 Ag1A 171.0(5) . 1_565 ? Ag1B N1 Ag1A 2.9(7) 1_565 1_565 ? C4 N2 C5 107.4(2) . . ? C4 N2 C3 109.1(2) . . ? C5 N2 C3 108.55(18) . . ? C4 N2 Ag1B 110.7(4) . . ? C5 N2 Ag1B 110.3(3) . . ? C3 N2 Ag1B 110.6(3) . . ? C4 N2 Ag1A 110.9(3) . . ? C5 N2 Ag1A 113.8(3) . . ? C3 N2 Ag1A 107.0(3) . . ? Ag1B N2 Ag1A 4.1(5) . . ? C3 N3 C3 105.6(3) 3_455 . ? C3 N3 C2 107.6(2) 3_455 . ? C3 N3 C2 107.6(2) . . ? C5 N4 C5 105.8(3) 3_455 . ? C5 N4 C2 109.5(3) 3_455 . ? C5 N4 C2 109.5(3) . . ? N3 C2 N4 113.5(3) . . ? N3 C2 H2A 108.9 . . ? N4 C2 H2A 108.9 . . ? N3 C2 H2B 108.9 . . ? N4 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N1 C1 S1B 177.4(5) . . ? N1 C1 S1A 174.3(5) . . ? S1B C1 S1A 8.3(7) . . ? N3 C3 N2 113.8(2) . . ? N3 C3 H3A 108.8 . . ? N2 C3 H3A 108.8 . . ? N3 C3 H3B 108.8 . . ? N2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? N2 C4 N2 109.3(3) . 3_455 ? N2 C4 H4A 109.8 . . ? N2 C4 H4A 109.8 3_455 . ? N2 C4 H4B 109.8 . . ? N2 C4 H4B 109.8 3_455 . ? H4A C4 H4B 108.3 . . ? N4 C5 N2 111.8(2) . . ? N4 C5 H5A 109.3 . . ? N2 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? N2 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.448 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.108 #---------------------------------------------------------- #---------------------------------------------------------- data_2 _database_code_depnum_ccdc_archive 'CCDC 788745' #TrackingRef '- Crystallographic_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H12 Ag2 N6 S2' _chemical_formula_weight 472.12 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' Ag Ag -0.8971 1.1015 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.505(2) _cell_length_b 7.7023(15) _cell_length_c 16.840(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.00(3) _cell_angle_gamma 90.00 _cell_volume 1357.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6039 _cell_measurement_theta_min 2.4285 _cell_measurement_theta_max 29.0528 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 3.183 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.6917 _exptl_absorpt_correction_T_max 0.8583 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6148 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 26.03 _reflns_number_total 2606 _reflns_number_gt 2501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+0.8152P] 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 0.0031(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2606 _refine_ls_number_parameters 182 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0690 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.148 _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 Ag1A Ag 0.3521(7) 0.2733(8) 0.5544(3) 0.0471(11) Uani 0.50 1 d PU . . Ag1B Ag 0.3381(7) 0.2887(8) 0.5512(3) 0.0404(5) Uani 0.50 1 d PU . . Ag2A Ag 0.6184(7) 0.0633(8) 0.7901(3) 0.0454(8) Uani 0.50 1 d PU . . Ag2B Ag 0.6319(7) 0.0470(8) 0.7935(2) 0.0439(7) Uani 0.50 1 d PU . . S1 S 0.41908(8) -0.12725(10) 0.77114(5) 0.0437(2) Uani 1 1 d . . . S2 S 0.25889(7) 0.58683(10) 0.57042(5) 0.04035(19) Uani 1 1 d . . . N1 N 0.2380(2) 0.0430(3) 0.30291(13) 0.0322(5) Uani 1 1 d . . . N2 N 0.2277(2) 0.1867(3) 0.43141(13) 0.0316(5) Uani 1 1 d . . . N3 N 0.5494(3) 0.2698(4) 0.5152(2) 0.0570(8) Uani 1 1 d . . . N4 N 0.3278(3) 0.0605(4) 0.63580(17) 0.0510(7) Uani 1 1 d . . . N5 N 0.0653(2) 0.2468(3) 0.32242(15) 0.0403(6) Uani 1 1 d . . . N6 N 0.0702(2) -0.0351(3) 0.38815(15) 0.0386(5) Uani 1 1 d . . . C1 C 0.3666(3) -0.0173(4) 0.69082(18) 0.0357(6) Uani 1 1 d . . . C2 C 0.1468(3) 0.0418(4) 0.45586(17) 0.0367(6) Uani 1 1 d . . . H2A H 0.2010 -0.0470 0.4819 0.044 Uiso 1 1 calc R . . H2B H 0.0904 0.0843 0.4941 0.044 Uiso 1 1 calc R . . C3 C 0.1572(3) -0.0981(4) 0.33136(18) 0.0379(6) Uani 1 1 d . . . H3C H 0.1077 -0.1498 0.2861 0.046 Uiso 1 1 calc R . . H3D H 0.2117 -0.1876 0.3565 0.046 Uiso 1 1 calc R . . C4 C 0.3118(3) 0.1202(4) 0.37314(16) 0.0323(6) Uani 1 1 d . . . H4B H 0.3684 0.0330 0.3984 0.039 Uiso 1 1 calc R . . H4C H 0.3641 0.2143 0.3558 0.039 Uiso 1 1 calc R . . C5 C 0.3742(3) 0.6708(4) 0.52076(18) 0.0408(7) Uani 1 1 d . . . C6 C -0.0105(3) 0.1005(4) 0.3495(2) 0.0447(7) Uani 1 1 d . . . H6A H -0.0687 0.1431 0.3867 0.054 Uiso 1 1 calc R . . H6B H -0.0611 0.0512 0.3041 0.054 Uiso 1 1 calc R . . C7 C 0.1425(3) 0.3188(4) 0.39157(17) 0.0383(6) Uani 1 1 d . . . H7A H 0.0863 0.3642 0.4293 0.046 Uiso 1 1 calc R . . H7B H 0.1936 0.4143 0.3743 0.046 Uiso 1 1 calc R . . C8 C 0.1520(3) 0.1792(4) 0.26644(17) 0.0401(6) Uani 1 1 d . . . H8A H 0.2030 0.2738 0.2482 0.048 Uiso 1 1 calc R . . H8B H 0.1022 0.1312 0.2204 0.048 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 Ag1A 0.0501(14) 0.0474(17) 0.0426(7) 0.0112(7) -0.0022(7) -0.0002(10) Ag1B 0.0493(13) 0.0327(5) 0.0383(8) -0.0005(9) -0.0023(6) 0.0007(9) Ag2A 0.0406(12) 0.0464(7) 0.0491(12) -0.0156(7) 0.0036(5) 0.0013(12) Ag2B 0.0418(12) 0.0572(15) 0.0333(7) -0.0106(5) 0.0073(7) 0.0069(7) S1 0.0485(4) 0.0394(4) 0.0423(4) 0.0084(3) -0.0013(3) -0.0098(3) S2 0.0390(4) 0.0430(4) 0.0392(4) -0.0037(3) 0.0046(3) 0.0030(3) N1 0.0301(11) 0.0378(12) 0.0289(11) -0.0033(9) 0.0034(9) 0.0004(9) N2 0.0326(11) 0.0342(11) 0.0279(11) -0.0004(9) 0.0025(9) 0.0003(9) N3 0.0537(17) 0.0583(18) 0.0610(19) 0.0139(15) 0.0159(15) 0.0084(14) N4 0.0602(18) 0.0427(15) 0.0496(17) 0.0102(13) 0.0018(13) -0.0034(13) N5 0.0388(13) 0.0448(13) 0.0366(13) 0.0036(11) -0.0001(10) 0.0111(11) N6 0.0326(12) 0.0404(13) 0.0437(14) 0.0022(11) 0.0087(10) -0.0037(10) C1 0.0354(14) 0.0317(13) 0.0413(15) 0.0001(13) 0.0098(11) -0.0045(11) C2 0.0387(15) 0.0386(15) 0.0338(14) 0.0051(11) 0.0093(11) -0.0002(11) C3 0.0368(15) 0.0351(14) 0.0419(16) -0.0054(12) 0.0035(12) -0.0032(12) C4 0.0288(13) 0.0373(14) 0.0312(13) -0.0024(11) 0.0042(10) -0.0004(11) C5 0.0449(16) 0.0386(15) 0.0385(15) 0.0002(13) 0.0010(13) 0.0113(13) C6 0.0288(14) 0.0562(18) 0.0492(18) -0.0004(15) 0.0032(12) 0.0049(13) C7 0.0434(15) 0.0334(13) 0.0382(15) -0.0010(12) 0.0050(12) 0.0076(12) C8 0.0428(16) 0.0462(16) 0.0309(14) 0.0038(13) 0.0006(12) 0.0066(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 Ag1A N4 2.166(7) . ? Ag1A N3 2.229(8) . ? Ag1A N2 2.443(6) . ? Ag1A S2 2.628(7) . ? Ag1A Ag2B 3.311(8) 2_656 ? Ag1A Ag2A 3.435(8) 2_656 ? Ag1B N4 2.271(7) . ? Ag1B N3 2.355(8) . ? Ag1B N2 2.371(5) . ? Ag1B S2 2.473(7) . ? Ag1B Ag2B 3.280(7) 2_656 ? Ag1B Ag2A 3.408(8) 2_656 ? Ag2A N1 2.411(6) 3_656 ? Ag2A S1 2.554(4) . ? Ag2A S2 2.585(6) 2_646 ? Ag2A S1 2.613(7) 2_656 ? Ag2A Ag1B 3.408(8) 2_646 ? Ag2A Ag1A 3.435(8) 2_646 ? Ag2B N1 2.317(5) 3_656 ? Ag2B S2 2.491(5) 2_646 ? Ag2B S1 2.606(5) . ? Ag2B S1 2.768(7) 2_656 ? Ag2B Ag1B 3.280(7) 2_646 ? Ag2B Ag1A 3.311(8) 2_646 ? S1 C1 1.649(3) . ? S1 Ag2A 2.613(7) 2_646 ? S1 Ag2B 2.768(7) 2_646 ? S2 C5 1.662(3) . ? S2 Ag2B 2.491(5) 2_656 ? S2 Ag2A 2.585(6) 2_656 ? N1 C4 1.481(3) . ? N1 C8 1.482(4) . ? N1 C3 1.484(4) . ? N1 Ag2B 2.317(5) 3_656 ? N1 Ag2A 2.411(6) 3_656 ? N2 C4 1.469(3) . ? N2 C7 1.477(4) . ? N2 C2 1.483(4) . ? N3 C5 1.143(4) 3_666 ? N4 C1 1.148(4) . ? N5 C8 1.463(4) . ? N5 C7 1.469(4) . ? N5 C6 1.475(4) . ? N6 C3 1.461(4) . ? N6 C6 1.462(4) . ? N6 C2 1.462(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 N3 1.143(4) 3_666 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? 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 Ag1A N3 110.0(4) . . ? N4 Ag1A N2 104.3(2) . . ? N3 Ag1A N2 100.9(2) . . ? N4 Ag1A S2 124.4(3) . . ? N3 Ag1A S2 113.9(2) . . ? N2 Ag1A S2 99.3(3) . . ? N4 Ag1A Ag2B 89.6(2) . 2_656 ? N3 Ag1A Ag2B 104.5(2) . 2_656 ? N2 Ag1A Ag2B 144.8(4) . 2_656 ? S2 Ag1A Ag2B 47.92(11) . 2_656 ? N4 Ag1A Ag2A 91.0(2) . 2_656 ? N3 Ag1A Ag2A 102.1(2) . 2_656 ? N2 Ag1A Ag2A 146.1(3) . 2_656 ? S2 Ag1A Ag2A 48.24(10) . 2_656 ? Ag2B Ag1A Ag2A 2.5(2) 2_656 2_656 ? N4 Ag1B N3 102.2(4) . . ? N4 Ag1B N2 103.35(19) . . ? N3 Ag1B N2 99.4(2) . . ? N4 Ag1B S2 126.9(2) . . ? N3 Ag1B S2 115.2(2) . . ? N2 Ag1B S2 105.9(3) . . ? N4 Ag1B Ag2B 88.58(19) . 2_656 ? N3 Ag1B Ag2B 102.4(2) . 2_656 ? N2 Ag1B Ag2B 152.3(4) . 2_656 ? S2 Ag1B Ag2B 48.88(10) . 2_656 ? N4 Ag1B Ag2A 89.91(18) . 2_656 ? N3 Ag1B Ag2A 100.1(2) . 2_656 ? N2 Ag1B Ag2A 153.5(4) . 2_656 ? S2 Ag1B Ag2A 49.05(10) . 2_656 ? Ag2B Ag1B Ag2A 2.5(2) 2_656 2_656 ? N1 Ag2A S1 106.04(16) 3_656 . ? N1 Ag2A S2 108.9(3) 3_656 2_646 ? S1 Ag2A S2 119.49(17) . 2_646 ? N1 Ag2A S1 97.74(16) 3_656 2_656 ? S1 Ag2A S1 112.4(3) . 2_656 ? S2 Ag2A S1 109.92(15) 2_646 2_656 ? N1 Ag2A Ag1B 104.5(3) 3_656 2_646 ? S1 Ag2A Ag1B 78.10(19) . 2_646 ? S2 Ag2A Ag1B 46.27(18) 2_646 2_646 ? S1 Ag2A Ag1B 151.75(18) 2_656 2_646 ? N1 Ag2A Ag1A 104.7(3) 3_656 2_646 ? S1 Ag2A Ag1A 74.9(2) . 2_646 ? S2 Ag2A Ag1A 49.32(17) 2_646 2_646 ? S1 Ag2A Ag1A 153.42(19) 2_656 2_646 ? Ag1B Ag2A Ag1A 3.2(3) 2_646 2_646 ? N1 Ag2B S2 115.4(3) 3_656 2_646 ? N1 Ag2B S1 107.21(16) 3_656 . ? S2 Ag2B S1 121.11(15) 2_646 . ? N1 Ag2B S1 95.82(16) 3_656 2_656 ? S2 Ag2B S1 107.93(17) 2_646 2_656 ? S1 Ag2B S1 106.0(3) . 2_656 ? N1 Ag2B Ag1B 110.8(3) 3_656 2_646 ? S2 Ag2B Ag1B 48.41(17) 2_646 2_646 ? S1 Ag2B Ag1B 79.9(2) . 2_646 ? S1 Ag2B Ag1B 149.89(19) 2_656 2_646 ? N1 Ag2B Ag1A 111.0(3) 3_656 2_646 ? S2 Ag2B Ag1A 51.54(19) 2_646 2_646 ? S1 Ag2B Ag1A 76.65(18) . 2_646 ? S1 Ag2B Ag1A 151.19(19) 2_656 2_646 ? Ag1B Ag2B Ag1A 3.3(3) 2_646 2_646 ? C1 S1 Ag2A 91.11(19) . . ? C1 S1 Ag2B 94.32(19) . . ? Ag2A S1 Ag2B 4.1(4) . . ? C1 S1 Ag2A 96.69(14) . 2_646 ? Ag2A S1 Ag2A 131.84(9) . 2_646 ? Ag2B S1 Ag2A 128.6(3) . 2_646 ? C1 S1 Ag2B 95.94(14) . 2_646 ? Ag2A S1 Ag2B 134.3(3) . 2_646 ? Ag2B S1 Ag2B 131.10(10) . 2_646 ? Ag2A S1 Ag2B 2.5(3) 2_646 2_646 ? C5 S2 Ag1B 91.53(17) . . ? C5 S2 Ag2B 102.31(19) . 2_656 ? Ag1B S2 Ag2B 82.71(18) . 2_656 ? C5 S2 Ag2A 99.02(19) . 2_656 ? Ag1B S2 Ag2A 84.68(19) . 2_656 ? Ag2B S2 Ag2A 3.8(3) 2_656 2_656 ? C5 S2 Ag1A 90.65(17) . . ? Ag1B S2 Ag1A 2.6(3) . . ? Ag2B S2 Ag1A 80.54(19) 2_656 . ? Ag2A S2 Ag1A 82.44(17) 2_656 . ? C4 N1 C8 107.7(2) . . ? C4 N1 C3 108.1(2) . . ? C8 N1 C3 107.9(2) . . ? C4 N1 Ag2B 112.3(2) . 3_656 ? C8 N1 Ag2B 107.3(3) . 3_656 ? C3 N1 Ag2B 113.3(2) . 3_656 ? C4 N1 Ag2A 110.0(2) . 3_656 ? C8 N1 Ag2A 111.4(2) . 3_656 ? C3 N1 Ag2A 111.7(2) . 3_656 ? Ag2B N1 Ag2A 4.1(4) 3_656 3_656 ? C4 N2 C7 108.2(2) . . ? C4 N2 C2 108.4(2) . . ? C7 N2 C2 107.8(2) . . ? C4 N2 Ag1B 113.9(2) . . ? C7 N2 Ag1B 113.0(3) . . ? C2 N2 Ag1B 105.2(2) . . ? C4 N2 Ag1A 110.7(2) . . ? C7 N2 Ag1A 117.1(3) . . ? C2 N2 Ag1A 104.3(2) . . ? Ag1B N2 Ag1A 4.2(4) . . ? C5 N3 Ag1A 150.0(3) 3_666 . ? C5 N3 Ag1B 146.4(3) 3_666 . ? Ag1A N3 Ag1B 3.6(4) . . ? C1 N4 Ag1A 148.5(3) . . ? C1 N4 Ag1B 151.4(3) . . ? Ag1A N4 Ag1B 4.2(4) . . ? C8 N5 C7 108.3(2) . . ? C8 N5 C6 108.1(3) . . ? C7 N5 C6 108.6(2) . . ? C3 N6 C6 108.5(2) . . ? C3 N6 C2 108.2(2) . . ? C6 N6 C2 108.4(2) . . ? N4 C1 S1 178.5(3) . . ? N6 C2 N2 112.2(2) . . ? N6 C2 H2A 109.2 . . ? N2 C2 H2A 109.2 . . ? N6 C2 H2B 109.2 . . ? N2 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N6 C3 N1 112.1(2) . . ? N6 C3 H3C 109.2 . . ? N1 C3 H3C 109.2 . . ? N6 C3 H3D 109.2 . . ? N1 C3 H3D 109.2 . . ? H3C C3 H3D 107.9 . . ? N2 C4 N1 111.7(2) . . ? N2 C4 H4B 109.3 . . ? N1 C4 H4B 109.3 . . ? N2 C4 H4C 109.3 . . ? N1 C4 H4C 109.3 . . ? H4B C4 H4C 107.9 . . ? N3 C5 S2 177.8(3) 3_666 . ? N6 C6 N5 112.1(2) . . ? N6 C6 H6A 109.2 . . ? N5 C6 H6A 109.2 . . ? N6 C6 H6B 109.2 . . ? N5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N5 C7 N2 111.8(2) . . ? N5 C7 H7A 109.3 . . ? N2 C7 H7A 109.3 . . ? N5 C7 H7B 109.3 . . ? N2 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? N5 C8 N1 112.1(2) . . ? N5 C8 H8A 109.2 . . ? N1 C8 H8A 109.2 . . ? N5 C8 H8B 109.2 . . ? N1 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag2A S1 C1 -79.2(3) 3_656 . . . ? S2 Ag2A S1 C1 157.5(3) 2_646 . . . ? S1 Ag2A S1 C1 26.48(17) 2_656 . . . ? Ag1B Ag2A S1 C1 178.96(16) 2_646 . . . ? Ag1A Ag2A S1 C1 179.46(16) 2_646 . . . ? N1 Ag2A S1 Ag2B 61(2) 3_656 . . . ? S2 Ag2A S1 Ag2B -62(2) 2_646 . . . ? S1 Ag2A S1 Ag2B 167(2) 2_656 . . . ? Ag1B Ag2A S1 Ag2B -40(2) 2_646 . . . ? Ag1A Ag2A S1 Ag2B -40(2) 2_646 . . . ? N1 Ag2A S1 Ag2A 20.8(3) 3_656 . . 2_646 ? S2 Ag2A S1 Ag2A -102.5(2) 2_646 . . 2_646 ? S1 Ag2A S1 Ag2A 126.5(2) 2_656 . . 2_646 ? Ag1B Ag2A S1 Ag2A -81.03(12) 2_646 . . 2_646 ? Ag1A Ag2A S1 Ag2A -80.53(12) 2_646 . . 2_646 ? N1 Ag2A S1 Ag2B 20.2(4) 3_656 . . 2_646 ? S2 Ag2A S1 Ag2B -103.1(3) 2_646 . . 2_646 ? S1 Ag2A S1 Ag2B 125.9(2) 2_656 . . 2_646 ? Ag1B Ag2A S1 Ag2B -81.6(2) 2_646 . . 2_646 ? Ag1A Ag2A S1 Ag2B -81.1(2) 2_646 . . 2_646 ? N1 Ag2B S1 C1 -73.7(3) 3_656 . . . ? S2 Ag2B S1 C1 151.0(3) 2_646 . . . ? S1 Ag2B S1 C1 27.81(15) 2_656 . . . ? Ag1B Ag2B S1 C1 177.47(17) 2_646 . . . ? Ag1A Ag2B S1 C1 178.14(16) 2_646 . . . ? N1 Ag2B S1 Ag2A -113(2) 3_656 . . . ? S2 Ag2B S1 Ag2A 111(2) 2_646 . . . ? S1 Ag2B S1 Ag2A -12(2) 2_656 . . . ? Ag1B Ag2B S1 Ag2A 138(2) 2_646 . . . ? Ag1A Ag2B S1 Ag2A 139(2) 2_646 . . . ? N1 Ag2B S1 Ag2A 28.4(4) 3_656 . . 2_646 ? S2 Ag2B S1 Ag2A -106.9(3) 2_646 . . 2_646 ? S1 Ag2B S1 Ag2A 129.93(17) 2_656 . . 2_646 ? Ag1B Ag2B S1 Ag2A -80.4(2) 2_646 . . 2_646 ? Ag1A Ag2B S1 Ag2A -79.7(2) 2_646 . . 2_646 ? N1 Ag2B S1 Ag2B 28.1(3) 3_656 . . 2_646 ? S2 Ag2B S1 Ag2B -107.3(2) 2_646 . . 2_646 ? S1 Ag2B S1 Ag2B 129.6(2) 2_656 . . 2_646 ? Ag1B Ag2B S1 Ag2B -80.78(12) 2_646 . . 2_646 ? Ag1A Ag2B S1 Ag2B -80.11(12) 2_646 . . 2_646 ? N4 Ag1B S2 C5 148.0(3) . . . . ? N3 Ag1B S2 C5 17.7(3) . . . . ? N2 Ag1B S2 C5 -91.1(2) . . . . ? Ag2B Ag1B S2 C5 102.22(19) 2_656 . . . ? Ag2A Ag1B S2 C5 98.92(19) 2_656 . . . ? N4 Ag1B S2 Ag2B 45.8(4) . . . 2_656 ? N3 Ag1B S2 Ag2B -84.5(3) . . . 2_656 ? N2 Ag1B S2 Ag2B 166.7(3) . . . 2_656 ? Ag2A Ag1B S2 Ag2B -3.3(3) 2_656 . . 2_656 ? N4 Ag1B S2 Ag2A 49.1(3) . . . 2_656 ? N3 Ag1B S2 Ag2A -81.2(3) . . . 2_656 ? N2 Ag1B S2 Ag2A 170.0(3) . . . 2_656 ? Ag2B Ag1B S2 Ag2A 3.3(3) 2_656 . . 2_656 ? N4 Ag1B S2 Ag1A 78(6) . . . . ? N3 Ag1B S2 Ag1A -52(6) . . . . ? N2 Ag1B S2 Ag1A -161(6) . . . . ? Ag2B Ag1B S2 Ag1A 32(6) 2_656 . . . ? Ag2A Ag1B S2 Ag1A 29(6) 2_656 . . . ? N4 Ag1A S2 C5 153.4(3) . . . . ? N3 Ag1A S2 C5 14.2(3) . . . . ? N2 Ag1A S2 C5 -92.2(2) . . . . ? Ag2B Ag1A S2 C5 102.4(2) 2_656 . . . ? Ag2A Ag1A S2 C5 99.01(19) 2_656 . . . ? N4 Ag1A S2 Ag1B -96(6) . . . . ? N3 Ag1A S2 Ag1B 124(6) . . . . ? N2 Ag1A S2 Ag1B 18(5) . . . . ? Ag2B Ag1A S2 Ag1B -147(6) 2_656 . . . ? Ag2A Ag1A S2 Ag1B -151(6) 2_656 . . . ? N4 Ag1A S2 Ag2B 51.0(3) . . . 2_656 ? N3 Ag1A S2 Ag2B -88.2(3) . . . 2_656 ? N2 Ag1A S2 Ag2B 165.4(3) . . . 2_656 ? Ag2A Ag1A S2 Ag2B -3.4(3) 2_656 . . 2_656 ? N4 Ag1A S2 Ag2A 54.3(4) . . . 2_656 ? N3 Ag1A S2 Ag2A -84.8(3) . . . 2_656 ? N2 Ag1A S2 Ag2A 168.8(2) . . . 2_656 ? Ag2B Ag1A S2 Ag2A 3.4(3) 2_656 . . 2_656 ? N4 Ag1B N2 C4 -97.8(3) . . . . ? N3 Ag1B N2 C4 7.3(3) . . . . ? S2 Ag1B N2 C4 127.0(2) . . . . ? Ag2B Ag1B N2 C4 148.9(5) 2_656 . . . ? Ag2A Ag1B N2 C4 144.1(5) 2_656 . . . ? N4 Ag1B N2 C7 138.2(3) . . . . ? N3 Ag1B N2 C7 -116.8(3) . . . . ? S2 Ag1B N2 C7 3.0(3) . . . . ? Ag2B Ag1B N2 C7 24.8(6) 2_656 . . . ? Ag2A Ag1B N2 C7 20.1(6) 2_656 . . . ? N4 Ag1B N2 C2 20.8(3) . . . . ? N3 Ag1B N2 C2 125.8(2) . . . . ? S2 Ag1B N2 C2 -114.4(2) . . . . ? Ag2B Ag1B N2 C2 -92.5(6) 2_656 . . . ? Ag2A Ag1B N2 C2 -97.3(5) 2_656 . . . ? N4 Ag1B N2 Ag1A -57(3) . . . . ? N3 Ag1B N2 Ag1A 48(3) . . . . ? S2 Ag1B N2 Ag1A 168(4) . . . . ? Ag2B Ag1B N2 Ag1A -170(4) 2_656 . . . ? Ag2A Ag1B N2 Ag1A -175(4) 2_656 . . . ? N4 Ag1A N2 C4 -101.6(3) . . . . ? N3 Ag1A N2 C4 12.4(3) . . . . ? S2 Ag1A N2 C4 129.2(2) . . . . ? Ag2B Ag1A N2 C4 148.1(4) 2_656 . . . ? Ag2A Ag1A N2 C4 144.2(4) 2_656 . . . ? N4 Ag1A N2 C7 133.8(3) . . . . ? N3 Ag1A N2 C7 -112.2(3) . . . . ? S2 Ag1A N2 C7 4.6(3) . . . . ? Ag2B Ag1A N2 C7 23.5(5) 2_656 . . . ? Ag2A Ag1A N2 C7 19.6(5) 2_656 . . . ? N4 Ag1A N2 C2 14.7(4) . . . . ? N3 Ag1A N2 C2 128.8(2) . . . . ? S2 Ag1A N2 C2 -114.4(2) . . . . ? Ag2B Ag1A N2 C2 -95.6(4) 2_656 . . . ? Ag2A Ag1A N2 C2 -99.4(4) 2_656 . . . ? N4 Ag1A N2 Ag1B 118(4) . . . . ? N3 Ag1A N2 Ag1B -128(4) . . . . ? S2 Ag1A N2 Ag1B -11(3) . . . . ? Ag2B Ag1A N2 Ag1B 8(3) 2_656 . . . ? Ag2A Ag1A N2 Ag1B 4(3) 2_656 . . . ? N4 Ag1A N3 C5 -178.7(6) . . . 3_666 ? N2 Ag1A N3 C5 71.6(7) . . . 3_666 ? S2 Ag1A N3 C5 -33.8(7) . . . 3_666 ? Ag2B Ag1A N3 C5 -83.8(7) 2_656 . . 3_666 ? Ag2A Ag1A N3 C5 -83.2(7) 2_656 . . 3_666 ? N4 Ag1A N3 Ag1B 177(3) . . . . ? N2 Ag1A N3 Ag1B 68(3) . . . . ? S2 Ag1A N3 Ag1B -38(3) . . . . ? Ag2B Ag1A N3 Ag1B -88(3) 2_656 . . . ? Ag2A Ag1A N3 Ag1B -87(3) 2_656 . . . ? N4 Ag1B N3 C5 -178.9(5) . . . 3_666 ? N2 Ag1B N3 C5 75.1(6) . . . 3_666 ? S2 Ag1B N3 C5 -37.5(6) . . . 3_666 ? Ag2B Ag1B N3 C5 -87.7(6) 2_656 . . 3_666 ? Ag2A Ag1B N3 C5 -86.8(6) 2_656 . . 3_666 ? N4 Ag1B N3 Ag1A -2(3) . . . . ? N2 Ag1B N3 Ag1A -108(3) . . . . ? S2 Ag1B N3 Ag1A 139(3) . . . . ? Ag2B Ag1B N3 Ag1A 89(3) 2_656 . . . ? Ag2A Ag1B N3 Ag1A 90(3) 2_656 . . . ? N3 Ag1A N4 C1 47.3(7) . . . . ? N2 Ag1A N4 C1 154.7(5) . . . . ? S2 Ag1A N4 C1 -93.2(7) . . . . ? Ag2B Ag1A N4 C1 -58.0(7) 2_656 . . . ? Ag2A Ag1A N4 C1 -55.9(7) 2_656 . . . ? N3 Ag1A N4 Ag1B -178(3) . . . . ? N2 Ag1A N4 Ag1B -70(3) . . . . ? S2 Ag1A N4 Ag1B 42(3) . . . . ? Ag2B Ag1A N4 Ag1B 77(3) 2_656 . . . ? Ag2A Ag1A N4 Ag1B 79(3) 2_656 . . . ? N3 Ag1B N4 C1 52.4(7) . . . . ? N2 Ag1B N4 C1 155.3(6) . . . . ? S2 Ag1B N4 C1 -82.7(8) . . . . ? Ag2B Ag1B N4 C1 -50.0(7) 2_656 . . . ? Ag2A Ag1B N4 C1 -47.9(7) 2_656 . . . ? N3 Ag1B N4 Ag1A 2(3) . . . . ? N2 Ag1B N4 Ag1A 105(3) . . . . ? S2 Ag1B N4 Ag1A -133(3) . . . . ? Ag2B Ag1B N4 Ag1A -100(3) 2_656 . . . ? Ag2A Ag1B N4 Ag1A -98(3) 2_656 . . . ? Ag1A N4 C1 S1 113(11) . . . . ? Ag1B N4 C1 S1 107(11) . . . . ? Ag2A S1 C1 N4 -113(11) . . . . ? Ag2B S1 C1 N4 -116(11) . . . . ? Ag2A S1 C1 N4 114(11) 2_646 . . . ? Ag2B S1 C1 N4 112(11) 2_646 . . . ? C3 N6 C2 N2 58.8(3) . . . . ? C6 N6 C2 N2 -58.6(3) . . . . ? C4 N2 C2 N6 -58.5(3) . . . . ? C7 N2 C2 N6 58.4(3) . . . . ? Ag1B N2 C2 N6 179.3(3) . . . . ? Ag1A N2 C2 N6 -176.4(3) . . . . ? C6 N6 C3 N1 58.4(3) . . . . ? C2 N6 C3 N1 -59.0(3) . . . . ? C4 N1 C3 N6 58.6(3) . . . . ? C8 N1 C3 N6 -57.6(3) . . . . ? Ag2B N1 C3 N6 -176.2(3) 3_656 . . . ? Ag2A N1 C3 N6 179.7(3) 3_656 . . . ? C7 N2 C4 N1 -58.9(3) . . . . ? C2 N2 C4 N1 57.8(3) . . . . ? Ag1B N2 C4 N1 174.6(2) . . . . ? Ag1A N2 C4 N1 171.6(2) . . . . ? C8 N1 C4 N2 58.4(3) . . . . ? C3 N1 C4 N2 -57.9(3) . . . . ? Ag2B N1 C4 N2 176.3(2) 3_656 . . . ? Ag2A N1 C4 N2 180.0(2) 3_656 . . . ? Ag1B S2 C5 N3 114(8) . . . 3_666 ? Ag2B S2 C5 N3 -163(8) 2_656 . . 3_666 ? Ag2A S2 C5 N3 -161(8) 2_656 . . 3_666 ? Ag1A S2 C5 N3 116(8) . . . 3_666 ? C3 N6 C6 N5 -59.0(3) . . . . ? C2 N6 C6 N5 58.3(3) . . . . ? C8 N5 C6 N6 59.0(3) . . . . ? C7 N5 C6 N6 -58.2(3) . . . . ? C8 N5 C7 N2 -58.9(3) . . . . ? C6 N5 C7 N2 58.2(3) . . . . ? C4 N2 C7 N5 59.0(3) . . . . ? C2 N2 C7 N5 -58.0(3) . . . . ? Ag1B N2 C7 N5 -173.9(2) . . . . ? Ag1A N2 C7 N5 -175.2(2) . . . . ? C7 N5 C8 N1 58.9(3) . . . . ? C6 N5 C8 N1 -58.5(3) . . . . ? C4 N1 C8 N5 -58.6(3) . . . . ? C3 N1 C8 N5 57.9(3) . . . . ? Ag2B N1 C8 N5 -179.7(2) 3_656 . . . ? Ag2A N1 C8 N5 -179.2(2) 3_656 . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.436 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.084 #---------------------------------------------------------- #---------------------------------------------------------- data_3 _database_code_depnum_ccdc_archive 'CCDC 788746' #TrackingRef '- Crystallographic_CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H6 Ag N3 S' _chemical_formula_weight 236.06 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' Ag Ag -0.8971 1.1015 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 6.3439(13) _cell_length_b 14.097(3) _cell_length_c 7.3832(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.69(3) _cell_angle_gamma 90.00 _cell_volume 654.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2778 _cell_measurement_theta_min 2.7840 _cell_measurement_theta_max 31.1250 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 3.301 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_min 0.4799 _exptl_absorpt_correction_T_max 0.6819 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5124 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.47 _reflns_number_total 1529 _reflns_number_gt 1481 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0269P)^2^+0.4720P] 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 0.0269(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1529 _refine_ls_number_parameters 101 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0222 _refine_ls_R_factor_gt 0.0212 _refine_ls_wR_factor_ref 0.0550 _refine_ls_wR_factor_gt 0.0544 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.119 _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 -0.61312(4) 0.2500 -0.60181(3) 0.03016(11) Uani 1 2 d S . . Ag2 Ag -1.0000 0.0000 -1.0000 0.04317(11) Uani 1 2 d S . . S3A S -0.6751(16) 0.0931(7) -0.7586(14) 0.0481(15) Uani 0.50 1 d PU . . S3B S -0.6714(14) 0.0862(6) -0.7345(13) 0.0351(10) Uani 0.50 1 d PU . . N1 N -0.8906(4) 0.2500 -0.4078(3) 0.0253(5) Uani 1 2 d S . . N2 N -0.0509(3) 0.33695(13) -0.1753(2) 0.0277(4) Uani 1 1 d . . . N3 N -0.2657(4) 0.05182(18) -0.8323(4) 0.0513(6) Uani 1 1 d . . . N5 N -0.2780(4) 0.2500 -0.4127(3) 0.0267(5) Uani 1 2 d S . . C1 C -0.4327(4) 0.06745(15) -0.7977(3) 0.0336(5) Uani 1 1 d . . . C3 C -0.2551(3) 0.33566(15) -0.2956(3) 0.0291(4) Uani 1 1 d . . . H3A H -0.2655 0.3917 -0.3725 0.035 Uiso 1 1 calc R . . H3B H -0.3704 0.3376 -0.2217 0.035 Uiso 1 1 calc R . . C4 C -0.8796(3) 0.33537(15) -0.2903(3) 0.0285(4) Uani 1 1 d . . . H4A H -0.7434 0.3368 -0.2130 0.034 Uiso 1 1 calc R . . H4B H -0.8893 0.3916 -0.3667 0.034 Uiso 1 1 calc R . . C8 C -0.0361(5) 0.2500 -0.0629(4) 0.0312(6) Uani 1 2 d S . . H8A H 0.0981 0.2500 0.0173 0.037 Uiso 1 2 calc SR . . H8B H -0.1498 0.2500 0.0129 0.037 Uiso 1 2 calc SR . . C10 C -1.0995(5) 0.2500 -0.5237(4) 0.0272(6) Uani 1 2 d S . . H10A H -1.1102 0.1944 -0.6017 0.033 Uiso 0.50 1 calc PR . . H10B H -1.1102 0.3056 -0.6017 0.033 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 Ag1 0.02708(15) 0.02889(14) 0.03453(15) 0.000 0.00416(10) 0.000 Ag2 0.04254(18) 0.04193(17) 0.04870(19) 0.00984(11) 0.01952(13) 0.00983(11) S3A 0.033(2) 0.042(3) 0.065(3) -0.025(2) -0.0063(17) 0.0059(17) S3B 0.032(2) 0.0252(11) 0.0512(18) -0.0095(11) 0.0160(18) -0.0048(13) N1 0.0242(12) 0.0255(12) 0.0272(12) 0.000 0.0070(10) 0.000 N2 0.0226(8) 0.0324(9) 0.0279(8) -0.0053(7) 0.0028(7) -0.0006(7) N3 0.0448(14) 0.0494(13) 0.0630(15) -0.0116(11) 0.0194(11) 0.0020(11) N5 0.0251(12) 0.0242(11) 0.0296(12) 0.000 -0.0013(10) 0.000 C1 0.0403(13) 0.0257(10) 0.0348(11) -0.0044(8) 0.0045(9) 0.0001(9) C3 0.0228(10) 0.0296(10) 0.0345(11) -0.0052(8) 0.0025(8) 0.0045(8) C4 0.0242(10) 0.0295(10) 0.0320(10) -0.0045(8) 0.0048(8) -0.0040(8) C8 0.0295(15) 0.0416(17) 0.0225(13) 0.000 0.0033(11) 0.000 C10 0.0311(15) 0.0269(13) 0.0234(13) 0.000 0.0027(11) 0.000 _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 N5 2.382(2) . ? Ag1 N1 2.413(3) . ? Ag1 S3A 2.503(11) . ? Ag1 S3A 2.503(11) 4_565 ? Ag1 S3B 2.516(10) . ? Ag1 S3B 2.516(10) 4_565 ? Ag2 N3 2.338(2) 1_455 ? Ag2 N3 2.338(2) 3_453 ? Ag2 N2 2.6364(18) 4_464 ? Ag2 N2 2.6364(18) 2_444 ? Ag2 S3A 2.857(10) 3_353 ? Ag2 S3A 2.857(10) . ? Ag2 S3B 2.928(10) 3_353 ? Ag2 S3B 2.928(10) . ? S3A C1 1.642(10) . ? S3B C1 1.664(9) . ? N1 C10 1.478(4) . ? N1 C4 1.480(2) . ? N1 C4 1.480(2) 4_565 ? N2 C4 1.467(3) 1_655 ? N2 C3 1.469(3) . ? N2 C8 1.476(2) . ? N2 Ag2 2.6364(18) 2_454 ? N3 C1 1.144(3) . ? N3 Ag2 2.338(2) 1_655 ? N5 C3 1.481(2) . ? N5 C3 1.481(2) 4_565 ? N5 C10 1.483(4) 1_655 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 N2 1.467(3) 1_455 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C8 N2 1.476(2) 4_565 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 N5 1.483(4) 1_455 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? 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 N5 Ag1 N1 108.47(9) . . ? N5 Ag1 S3A 110.1(3) . . ? N1 Ag1 S3A 101.1(2) . . ? N5 Ag1 S3A 110.1(3) . 4_565 ? N1 Ag1 S3A 101.10(19) . 4_565 ? S3A Ag1 S3A 124.2(5) . 4_565 ? N5 Ag1 S3B 107.5(2) . . ? N1 Ag1 S3B 98.65(17) . . ? S3A Ag1 S3B 4.6(4) . . ? S3A Ag1 S3B 128.69(8) 4_565 . ? N5 Ag1 S3B 107.5(2) . 4_565 ? N1 Ag1 S3B 98.65(17) . 4_565 ? S3A Ag1 S3B 128.69(8) . 4_565 ? S3A Ag1 S3B 4.6(4) 4_565 4_565 ? S3B Ag1 S3B 133.2(4) . 4_565 ? N3 Ag2 N3 180.000(1) 1_455 3_453 ? N3 Ag2 N2 86.44(8) 1_455 4_464 ? N3 Ag2 N2 93.56(8) 3_453 4_464 ? N3 Ag2 N2 93.56(8) 1_455 2_444 ? N3 Ag2 N2 86.44(8) 3_453 2_444 ? N2 Ag2 N2 180.0 4_464 2_444 ? N3 Ag2 S3A 87.9(2) 1_455 3_353 ? N3 Ag2 S3A 92.1(2) 3_453 3_353 ? N2 Ag2 S3A 93.6(2) 4_464 3_353 ? N2 Ag2 S3A 86.4(2) 2_444 3_353 ? N3 Ag2 S3A 92.1(2) 1_455 . ? N3 Ag2 S3A 87.9(2) 3_453 . ? N2 Ag2 S3A 86.4(2) 4_464 . ? N2 Ag2 S3A 93.6(2) 2_444 . ? S3A Ag2 S3A 180.0 3_353 . ? N3 Ag2 S3B 89.15(19) 1_455 3_353 ? N3 Ag2 S3B 90.85(19) 3_453 3_353 ? N2 Ag2 S3B 90.22(18) 4_464 3_353 ? N2 Ag2 S3B 89.78(18) 2_444 3_353 ? S3A Ag2 S3B 3.7(3) 3_353 3_353 ? S3A Ag2 S3B 176.3(3) . 3_353 ? N3 Ag2 S3B 90.85(19) 1_455 . ? N3 Ag2 S3B 89.15(19) 3_453 . ? N2 Ag2 S3B 89.78(18) 4_464 . ? N2 Ag2 S3B 90.22(18) 2_444 . ? S3A Ag2 S3B 176.3(3) 3_353 . ? S3A Ag2 S3B 3.7(3) . . ? S3B Ag2 S3B 180.0 3_353 . ? C1 S3A Ag1 100.5(4) . . ? C1 S3A Ag2 113.8(5) . . ? Ag1 S3A Ag2 138.6(4) . . ? C1 S3B Ag1 99.4(4) . . ? C1 S3B Ag2 109.8(5) . . ? Ag1 S3B Ag2 134.1(4) . . ? C10 N1 C4 107.91(15) . . ? C10 N1 C4 107.91(15) . 4_565 ? C4 N1 C4 108.8(2) . 4_565 ? C10 N1 Ag1 108.98(17) . . ? C4 N1 Ag1 111.53(13) . . ? C4 N1 Ag1 111.53(13) 4_565 . ? C4 N2 C3 108.12(16) 1_655 . ? C4 N2 C8 108.45(19) 1_655 . ? C3 N2 C8 108.32(18) . . ? C4 N2 Ag2 104.23(12) 1_655 2_454 ? C3 N2 Ag2 110.35(12) . 2_454 ? C8 N2 Ag2 116.99(13) . 2_454 ? C1 N3 Ag2 158.9(2) . 1_655 ? C3 N5 C3 109.3(2) . 4_565 ? C3 N5 C10 107.45(16) . 1_655 ? C3 N5 C10 107.45(16) 4_565 1_655 ? C3 N5 Ag1 110.62(13) . . ? C3 N5 Ag1 110.62(13) 4_565 . ? C10 N5 Ag1 111.32(17) 1_655 . ? N3 C1 S3A 176.9(4) . . ? N3 C1 S3B 176.2(4) . . ? S3A C1 S3B 6.9(6) . . ? N2 C3 N5 111.89(18) . . ? N2 C3 H3A 109.2 . . ? N5 C3 H3A 109.2 . . ? N2 C3 H3B 109.2 . . ? N5 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? N2 C4 N1 111.80(17) 1_455 . ? N2 C4 H4A 109.3 1_455 . ? N1 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 1_455 . ? N1 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? N2 C8 N2 112.3(2) 4_565 . ? N2 C8 H8A 109.1 4_565 . ? N2 C8 H8A 109.1 . . ? N2 C8 H8B 109.1 4_565 . ? N2 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N1 C10 N5 111.8(2) . 1_455 ? N1 C10 H10A 109.3 . . ? N5 C10 H10A 109.3 1_455 . ? N1 C10 H10B 109.3 . . ? N5 C10 H10B 109.3 1_455 . ? H10A C10 H10B 107.9 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.912 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.086 #----------------------------------------------------------