# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_publication_text _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Christopher Sumby' _publ_contact_author_address ;School of Chemistry & Physics The University of Adelaide Adelaide SA 5005 Australia ; _publ_contact_author_email christopher.sumby@adelaide.edu.au _publ_contact_author_phone '+61 8 83037406' _publ_contact_author_fax '+61 8 83034358' loop_ _publ_author_name 'Witold Bloch' 'Christopher Sumby' data_1(as) _database_code_depnum_ccdc_archive 'CCDC 855398' #TrackingRef 'CC_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H14 Ag Cl N4 O5 S' _chemical_formula_weight 457.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 27.978(2) _cell_length_b 27.978(2) _cell_length_c 14.9798(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10155.0(13) _cell_formula_units_Z 18 _cell_measurement_temperature 150(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 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4104 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_T_min 0.68015 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -47.00 47.00 1.0000 82.3200 omega____ theta____ kappa____ phi______ frames - 19.0026 -77.0000 -120.0000 94 #__ type_ start__ end____ width___ exp.time_ 2 omega -62.00 -35.00 1.0000 82.3200 omega____ theta____ kappa____ phi______ frames - -19.7838 179.0000 -150.0000 27 #__ type_ start__ end____ width___ exp.time_ 3 omega -13.00 90.00 1.0000 82.3200 omega____ theta____ kappa____ phi______ frames - 19.0026 77.0000 0.0000 103 #__ type_ start__ end____ width___ exp.time_ 4 omega 17.00 76.00 1.0000 82.3200 omega____ theta____ kappa____ phi______ frames - 19.0026 -155.0000 92.0000 59 #__ type_ start__ end____ width___ exp.time_ 5 omega -92.00 8.00 1.0000 82.3200 omega____ theta____ kappa____ phi______ frames - -19.7838 -37.0000 -180.0000 100 ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24591 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 29.24 _reflns_number_total 5459 _reflns_number_gt 2625 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2003)' _computing_publication_material 'CIFTAB (Sheldrick)' _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^)+(0.1530P)^2^+63.9051P] 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 5459 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1831 _refine_ls_R_factor_gt 0.1058 _refine_ls_wR_factor_ref 0.3373 _refine_ls_wR_factor_gt 0.3047 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _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 0.74308(4) 0.12940(3) 0.42770(5) 0.0647(4) Uani 1 1 d . . . Cl30 Cl 0.45921(12) 0.07063(13) 0.61106(19) 0.0663(8) Uani 1 1 d . . . S40 S 0.8702(2) 0.1353(3) 0.5483(3) 0.1301(18) Uani 1 1 d . . . N24 N 0.5471(3) 0.0775(3) 0.2921(5) 0.056(2) Uani 1 1 d . . . C13 C 0.5973(4) 0.0490(4) 0.6173(6) 0.050(2) Uani 1 1 d . . . H13 H 0.5640 0.0499 0.6236 0.061 Uiso 1 1 calc R . . C12 C 0.6365(4) 0.0849(4) 0.5578(6) 0.054(2) Uani 1 1 d . . . C23 C 0.5615(4) 0.0925(4) 0.3764(6) 0.048(2) Uani 1 1 d . . . H23 H 0.5349 0.0920 0.4162 0.057 Uiso 1 1 calc R . . N21 N 0.6527(3) 0.1092(4) 0.3565(6) 0.064(2) Uani 1 1 d . . . C26 C 0.6386(5) 0.0926(7) 0.2744(8) 0.089(4) Uani 1 1 d . . . H26 H 0.6652 0.0914 0.2366 0.107 Uiso 1 1 calc R . . N11 N 0.6830(3) 0.0834(4) 0.5430(6) 0.059(2) Uani 1 1 d . . . C22 C 0.6139(4) 0.1087(4) 0.4086(6) 0.053(2) Uani 1 1 d . . . N14 N 0.6042(4) 0.0137(4) 0.6656(6) 0.067(3) Uani 1 1 d . . . C16 C 0.6910(4) 0.0481(5) 0.5919(8) 0.070(3) Uani 1 1 d . . . H16 H 0.7244 0.0474 0.5849 0.084 Uiso 1 1 calc R . . C25 C 0.5874(5) 0.0768(5) 0.2396(7) 0.069(3) Uani 1 1 d . . . H25 H 0.5797 0.0653 0.1791 0.082 Uiso 1 1 calc R . . C15 C 0.6523(5) 0.0126(5) 0.6523(8) 0.073(3) Uani 1 1 d . . . H15 H 0.6588 -0.0127 0.6849 0.088 Uiso 1 1 calc R . . C42 C 0.9243(10) 0.2043(14) 0.5542(19) 0.26(2) Uani 1 1 d . . . H42A H 0.9283 0.2223 0.4963 0.392 Uiso 1 1 calc R . . H42B H 0.9588 0.2051 0.5692 0.392 Uiso 1 1 calc R . . H42C H 0.9159 0.2239 0.6002 0.392 Uiso 1 1 calc R . . O43 O 0.8172(4) 0.1340(6) 0.5422(7) 0.134(5) Uani 1 1 d . . . C41 C 0.8798(10) 0.1234(11) 0.6664(14) 0.170(9) Uani 1 1 d . . . H41A H 0.8533 0.0851 0.6825 0.255 Uiso 1 1 calc R . . H41B H 0.8740 0.1485 0.7043 0.255 Uiso 1 1 calc R . . H41C H 0.9174 0.1301 0.6751 0.255 Uiso 1 1 calc R . . C1 C 0.6283(5) 0.1262(4) 0.5037(6) 0.063(3) Uani 1 1 d . . . H1A H 0.5985 0.1305 0.5311 0.075 Uiso 1 1 calc R . . H1B H 0.6626 0.1626 0.5057 0.075 Uiso 1 1 calc R . . O33 O 0.5043(5) 0.1102(6) 0.5669(9) 0.132(4) Uani 1 1 d . . . O31 O 0.4310(8) 0.0324(6) 0.5470(9) 0.179(7) Uani 1 1 d . . . O32 O 0.4299(5) 0.0928(6) 0.6408(12) 0.178(7) Uani 1 1 d . . . O34 O 0.4695(8) 0.0440(7) 0.6748(10) 0.199(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0655(6) 0.0588(6) 0.0516(6) 0.0018(4) 0.0031(4) 0.0174(4) Cl30 0.0678(17) 0.0739(18) 0.0568(17) 0.0131(14) 0.0082(13) 0.0350(15) S40 0.114(4) 0.179(5) 0.094(3) 0.022(3) 0.004(3) 0.071(4) N24 0.058(5) 0.065(5) 0.045(5) 0.006(4) 0.003(4) 0.031(4) C13 0.044(5) 0.067(6) 0.049(6) -0.001(5) -0.005(4) 0.035(5) C12 0.068(6) 0.072(6) 0.033(5) -0.011(5) -0.014(5) 0.044(6) C23 0.055(6) 0.058(6) 0.042(5) 0.018(4) 0.016(4) 0.037(5) N21 0.054(5) 0.096(7) 0.044(5) 0.010(5) 0.010(4) 0.040(5) C26 0.055(7) 0.158(13) 0.051(7) 0.026(8) 0.019(6) 0.051(8) N11 0.053(5) 0.064(5) 0.056(5) 0.014(4) 0.006(4) 0.027(4) C22 0.065(6) 0.054(6) 0.044(5) 0.005(4) -0.009(5) 0.032(5) N14 0.065(6) 0.109(7) 0.048(5) 0.021(5) 0.003(4) 0.058(6) C16 0.049(6) 0.101(9) 0.075(8) 0.021(7) 0.007(6) 0.049(6) C25 0.077(8) 0.089(8) 0.039(6) 0.002(5) -0.006(5) 0.041(7) C15 0.060(7) 0.092(8) 0.078(8) 0.047(7) 0.012(6) 0.045(6) C42 0.15(2) 0.44(6) 0.16(2) -0.02(3) -0.097(19) 0.12(3) O43 0.081(7) 0.213(14) 0.097(8) 0.040(8) -0.012(6) 0.065(8) C41 0.16(2) 0.21(2) 0.131(16) 0.033(16) -0.051(15) 0.087(19) C1 0.069(7) 0.065(7) 0.043(6) -0.003(5) -0.007(5) 0.025(6) O33 0.099(8) 0.135(10) 0.162(11) 0.022(8) 0.022(8) 0.060(8) O31 0.27(2) 0.128(11) 0.107(10) -0.014(8) -0.033(11) 0.074(12) O32 0.109(9) 0.120(10) 0.30(2) 0.017(11) 0.095(11) 0.054(8) O34 0.29(2) 0.174(15) 0.126(12) 0.052(10) -0.018(12) 0.116(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 N24 2.249(8) 18_545 ? Ag1 N11 2.302(8) . ? Ag1 N14 2.353(9) 9_654 ? Ag1 N21 2.535(9) . ? Cl30 O32 1.328(12) . ? Cl30 O34 1.327(14) . ? Cl30 O31 1.357(14) . ? Cl30 O33 1.363(12) . ? S40 O43 1.467(12) . ? S40 C42 1.76(3) . ? S40 C41 1.845(19) . ? N24 C23 1.329(12) . ? N24 C25 1.383(14) . ? N24 Ag1 2.249(8) 17 ? C13 N14 1.316(12) . ? C13 C12 1.380(14) . ? C13 H13 0.9500 . ? C12 N11 1.340(13) . ? C12 C1 1.521(14) . ? C23 C22 1.386(13) . ? C23 H23 0.9500 . ? N21 C26 1.304(15) . ? N21 C22 1.331(13) . ? C26 C25 1.372(16) . ? C26 H26 0.9500 . ? N11 C16 1.335(13) . ? C22 C1 1.496(13) . ? N14 C15 1.375(13) . ? N14 Ag1 2.353(9) 5_545 ? C16 C15 1.379(15) . ? C16 H16 0.9500 . ? C25 H25 0.9500 . ? C15 H15 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N24 Ag1 N11 143.6(3) 18_545 . ? N24 Ag1 N14 109.0(3) 18_545 9_654 ? N11 Ag1 N14 107.4(3) . 9_654 ? N24 Ag1 N21 102.8(3) 18_545 . ? N11 Ag1 N21 79.8(3) . . ? N14 Ag1 N21 87.8(3) 9_654 . ? O32 Cl30 O34 112.2(12) . . ? O32 Cl30 O31 110.7(12) . . ? O34 Cl30 O31 105.7(11) . . ? O32 Cl30 O33 108.7(8) . . ? O34 Cl30 O33 115.6(10) . . ? O31 Cl30 O33 103.5(9) . . ? O43 S40 C42 109.6(12) . . ? O43 S40 C41 107.1(9) . . ? C42 S40 C41 91.5(12) . . ? C23 N24 C25 115.1(8) . . ? C23 N24 Ag1 122.6(6) . 17 ? C25 N24 Ag1 122.3(7) . 17 ? N14 C13 C12 122.6(9) . . ? N14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? N11 C12 C13 121.1(9) . . ? N11 C12 C1 117.0(9) . . ? C13 C12 C1 121.9(9) . . ? N24 C23 C22 122.5(8) . . ? N24 C23 H23 118.7 . . ? C22 C23 H23 118.7 . . ? C26 N21 C22 116.7(9) . . ? C26 N21 Ag1 124.5(7) . . ? C22 N21 Ag1 118.2(6) . . ? N21 C26 C25 123.6(11) . . ? N21 C26 H26 118.2 . . ? C25 C26 H26 118.2 . . ? C16 N11 C12 117.1(9) . . ? C16 N11 Ag1 118.7(7) . . ? C12 N11 Ag1 123.7(7) . . ? N21 C22 C23 121.5(9) . . ? N21 C22 C1 118.0(9) . . ? C23 C22 C1 120.4(9) . . ? C13 N14 C15 116.8(9) . . ? C13 N14 Ag1 124.9(7) . 5_545 ? C15 N14 Ag1 118.0(7) . 5_545 ? N11 C16 C15 122.1(9) . . ? N11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C26 C25 N24 120.4(10) . . ? C26 C25 H25 119.8 . . ? N24 C25 H25 119.8 . . ? N14 C15 C16 120.3(9) . . ? N14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? S40 C42 H42A 109.5 . . ? S40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? S40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? S40 C41 H41A 109.5 . . ? S40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? S40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C22 C1 C12 112.1(9) . . ? C22 C1 H1A 109.2 . . ? C12 C1 H1A 109.2 . . ? C22 C1 H1B 109.2 . . ? C12 C1 H1B 109.2 . . ? H1A C1 H1B 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 N14 C13 C12 N11 3.4(15) . . . . ? N14 C13 C12 C1 -178.8(9) . . . . ? C25 N24 C23 C22 2.9(14) . . . . ? Ag1 N24 C23 C22 -178.6(7) 17 . . . ? N24 Ag1 N21 C26 79.1(11) 18_545 . . . ? N11 Ag1 N21 C26 -138.0(11) . . . . ? N14 Ag1 N21 C26 -29.8(11) 9_654 . . . ? N24 Ag1 N21 C22 -109.7(8) 18_545 . . . ? N11 Ag1 N21 C22 33.2(8) . . . . ? N14 Ag1 N21 C22 141.4(8) 9_654 . . . ? C22 N21 C26 C25 2(2) . . . . ? Ag1 N21 C26 C25 173.5(10) . . . . ? C13 C12 N11 C16 -3.7(15) . . . . ? C1 C12 N11 C16 178.4(10) . . . . ? C13 C12 N11 Ag1 168.2(7) . . . . ? C1 C12 N11 Ag1 -9.7(12) . . . . ? N24 Ag1 N11 C16 -121.5(9) 18_545 . . . ? N14 Ag1 N11 C16 56.3(9) 9_654 . . . ? N21 Ag1 N11 C16 140.7(9) . . . . ? N24 Ag1 N11 C12 66.8(10) 18_545 . . . ? N14 Ag1 N11 C12 -115.5(8) 9_654 . . . ? N21 Ag1 N11 C12 -31.1(8) . . . . ? C26 N21 C22 C23 -1.4(16) . . . . ? Ag1 N21 C22 C23 -173.3(7) . . . . ? C26 N21 C22 C1 178.6(11) . . . . ? Ag1 N21 C22 C1 6.7(12) . . . . ? N24 C23 C22 N21 -1.2(15) . . . . ? N24 C23 C22 C1 178.8(9) . . . . ? C12 C13 N14 C15 -2.0(16) . . . . ? C12 C13 N14 Ag1 -175.5(7) . . . 5_545 ? C12 N11 C16 C15 2.9(18) . . . . ? Ag1 N11 C16 C15 -169.4(10) . . . . ? N21 C26 C25 N24 0(2) . . . . ? C23 N24 C25 C26 -2.1(16) . . . . ? Ag1 N24 C25 C26 179.3(10) 17 . . . ? C13 N14 C15 C16 1.1(18) . . . . ? Ag1 N14 C15 C16 175.1(10) 5_545 . . . ? N11 C16 C15 N14 -2(2) . . . . ? N21 C22 C1 C12 -69.3(12) . . . . ? C23 C22 C1 C12 110.7(11) . . . . ? N11 C12 C1 C22 73.8(12) . . . . ? C13 C12 C1 C22 -104.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.888 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.375 _refine_diff_density_min -0.770 _refine_diff_density_rms 0.159 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.007 1094.8 17.1 2 0.333 0.667 0.259 1097.6 17.1 3 0.667 0.333 0.926 1097.5 17.0 _platon_squeeze_details ; ; ####END data_1(dcm) _database_code_depnum_ccdc_archive 'CCDC 855399' #TrackingRef 'CC_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9.50 H9 Ag Cl2 N4 O4' _chemical_formula_weight 421.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'R -3' _symmetry_cell_setting TRIGONAL loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 28.3911(13) _cell_length_b 28.3911(13) _cell_length_c 11.7766(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 8220.8(13) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2483 _cell_measurement_theta_min 2.4801 _cell_measurement_theta_max 29.0700 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.534 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3726 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_T_min 0.60354 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -20.00 90.00 1.0000 28.0000 omega____ theta____ kappa____ phi______ frames - 18.8463 0.0000 -150.0000 110 #__ type_ start__ end____ width___ exp.time_ 2 omega -91.00 -10.00 1.0000 28.0000 omega____ theta____ kappa____ phi______ frames - -19.6276 -77.0000 0.0000 81 #__ type_ start__ end____ width___ exp.time_ 3 omega -47.00 53.00 1.0000 28.0000 omega____ theta____ kappa____ phi______ frames - -19.6276 37.0000 120.0000 100 ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15970 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0722 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 29.13 _reflns_number_total 4358 _reflns_number_gt 2280 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2003)' _computing_publication_material 'CIFTAB (Sheldrick)' _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^)+(0.1591P)^2^+5.7134P] 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 4358 _refine_ls_number_parameters 191 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1381 _refine_ls_R_factor_gt 0.0796 _refine_ls_wR_factor_ref 0.2950 _refine_ls_wR_factor_gt 0.2647 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.089 _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 0.58933(2) 0.06732(3) 0.19318(7) 0.0723(4) Uani 1 1 d . . . N21 N 0.6493(2) 0.0792(2) 0.0486(6) 0.0532(17) Uani 1 1 d . . . C26 C 0.6448(3) 0.0361(3) -0.0087(7) 0.0471(18) Uani 1 1 d . . . H26 H 0.6105 0.0036 -0.0107 0.057 Uiso 1 1 calc R . . N31 N 0.6757(3) 0.1274(3) 0.2921(10) 0.078(3) Uani 1 1 d . . . C23 C 0.7413(3) 0.1258(3) -0.0116(9) 0.070(3) Uani 1 1 d . . . H23 H 0.7754 0.1586 -0.0135 0.084 Uiso 1 1 calc R . . C32 C 0.7168(4) 0.1676(3) 0.2398(10) 0.070(3) Uani 1 1 d . . . C33 C 0.7656(4) 0.2010(4) 0.2857(12) 0.079(3) Uani 1 1 d . . . H33 H 0.7940 0.2274 0.2396 0.095 Uiso 1 1 calc R . . N24 N 0.7365(2) 0.0821(2) -0.0663(6) 0.0505(16) Uani 1 1 d . . . C36 C 0.6847(3) 0.1214(4) 0.3988(12) 0.079(3) Uani 1 1 d . . . H36 H 0.6567 0.0924 0.4409 0.095 Uiso 1 1 calc R . . C22 C 0.6991(3) 0.1252(3) 0.0474(9) 0.067(3) Uani 1 1 d . . . C1 C 0.7056(4) 0.1730(3) 0.1126(12) 0.089(4) Uani 1 1 d . . . H1A H 0.6722 0.1755 0.1058 0.107 Uiso 1 1 calc R . . H1B H 0.7363 0.2067 0.0809 0.107 Uiso 1 1 calc R . . C35 C 0.7350(3) 0.1568(4) 0.4545(11) 0.080(3) Uani 1 1 d . . . H35 H 0.7404 0.1517 0.5321 0.096 Uiso 1 1 calc R . . C25 C 0.6872(3) 0.0374(3) -0.0636(7) 0.0502(19) Uani 1 1 d . . . H25 H 0.6819 0.0055 -0.1014 0.060 Uiso 1 1 calc R . . N34 N 0.7744(3) 0.1974(3) 0.3938(11) 0.085(3) Uani 1 1 d . . . Cl40 Cl 0.78804(9) 0.06068(9) 0.3383(2) 0.0669(7) Uani 1 1 d . . . O43 O 0.8389(3) 0.0734(3) 0.3032(7) 0.093(2) Uani 1 1 d . . . O44 O 0.7561(3) 0.0055(3) 0.3596(10) 0.144(4) Uani 1 1 d . . . O42 O 0.7621(4) 0.0761(4) 0.2531(9) 0.125(3) Uani 1 1 d . . . O41 O 0.7964(4) 0.0935(4) 0.4396(7) 0.115(3) Uani 1 1 d . . . Cl51 Cl 0.9024(2) 0.0957(2) 0.6034(8) 0.122(3) Uani 0.50 1 d PD . . Cl52 Cl 0.8482(3) 0.1608(3) 0.6602(8) 0.118(3) Uani 0.50 1 d PD . . C50 C 0.8912(3) 0.1446(3) 0.5926(8) 0.159(13) Uiso 0.50 1 d PRD . . H50A H 0.8824 0.1447 0.5113 0.191 Uiso 0.50 1 calc PR . . H50B H 0.9274 0.1773 0.6033 0.191 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 0.0306(4) 0.0394(4) 0.1502(9) 0.0089(4) 0.0086(3) 0.0199(3) N21 0.028(3) 0.027(3) 0.102(5) 0.008(3) 0.004(3) 0.012(3) C26 0.024(3) 0.029(3) 0.080(5) 0.005(3) -0.006(3) 0.007(3) N31 0.033(4) 0.035(4) 0.153(8) -0.017(5) 0.017(5) 0.007(3) C23 0.032(4) 0.038(4) 0.138(8) -0.010(5) 0.002(5) 0.015(4) C32 0.044(5) 0.026(4) 0.134(9) -0.007(5) 0.022(5) 0.012(4) C33 0.044(5) 0.041(5) 0.147(10) -0.007(6) 0.032(6) 0.017(4) N24 0.031(3) 0.028(3) 0.088(5) -0.003(3) -0.004(3) 0.011(3) C36 0.029(4) 0.044(5) 0.145(10) -0.015(6) 0.028(6) 0.004(4) C22 0.036(4) 0.029(4) 0.138(8) -0.001(4) 0.004(5) 0.017(3) C1 0.038(5) 0.025(4) 0.194(12) 0.002(6) 0.031(6) 0.008(4) C35 0.032(4) 0.042(5) 0.160(10) -0.023(5) 0.006(5) 0.014(4) C25 0.034(4) 0.028(4) 0.083(5) 0.004(3) 0.002(4) 0.011(3) N34 0.025(4) 0.029(4) 0.188(10) -0.014(5) 0.023(5) 0.003(3) Cl40 0.0363(11) 0.0466(12) 0.1068(18) 0.0084(11) 0.0094(11) 0.0124(9) O43 0.038(3) 0.064(4) 0.161(7) 0.010(4) 0.019(4) 0.012(3) O44 0.065(5) 0.063(5) 0.251(11) 0.067(6) -0.004(6) -0.006(4) O42 0.132(8) 0.085(6) 0.167(8) -0.008(5) -0.049(6) 0.061(6) O41 0.146(8) 0.119(7) 0.117(6) 0.005(5) 0.028(5) 0.094(7) Cl51 0.057(3) 0.051(3) 0.247(8) -0.055(4) -0.050(4) 0.020(2) Cl52 0.093(6) 0.079(4) 0.149(5) 0.010(4) -0.035(5) 0.019(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N34 2.259(9) 17 ? Ag1 N21 2.311(7) . ? Ag1 N24 2.361(6) 5_545 ? Ag1 N31 2.469(9) . ? N21 C26 1.345(10) . ? N21 C22 1.362(9) . ? C26 C25 1.351(11) . ? C26 H26 0.9500 . ? N31 C32 1.307(12) . ? N31 C36 1.311(14) . ? C23 N24 1.342(10) . ? C23 C22 1.378(12) . ? C23 H23 0.9500 . ? C32 C33 1.341(14) . ? C32 C1 1.554(16) . ? C33 N34 1.311(14) . ? C33 H33 0.9500 . ? N24 C25 1.340(9) . ? N24 Ag1 2.362(6) 9_654 ? C36 C35 1.430(14) . ? C36 H36 0.9500 . ? C22 C1 1.489(12) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C35 N34 1.341(13) . ? C35 H35 0.9500 . ? C25 H25 0.9500 . ? N34 Ag1 2.260(9) 18_545 ? Cl40 O43 1.366(7) . ? Cl40 O44 1.385(8) . ? Cl40 O42 1.435(9) . ? Cl40 O41 1.458(9) . ? Cl51 C50 1.578(8) . ? Cl52 Cl52 1.066(14) 13_656 ? Cl52 C50 1.6985 . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N34 Ag1 N21 149.0(3) 17 . ? N34 Ag1 N24 114.7(3) 17 5_545 ? N21 Ag1 N24 95.5(2) . 5_545 ? N34 Ag1 N31 103.1(3) 17 . ? N21 Ag1 N31 80.9(3) . . ? N24 Ag1 N31 92.9(3) 5_545 . ? C26 N21 C22 116.6(6) . . ? C26 N21 Ag1 120.5(5) . . ? C22 N21 Ag1 118.9(6) . . ? N21 C26 C25 122.5(6) . . ? N21 C26 H26 118.8 . . ? C25 C26 H26 118.8 . . ? C32 N31 C36 114.7(9) . . ? C32 N31 Ag1 121.7(9) . . ? C36 N31 Ag1 123.6(6) . . ? N24 C23 C22 123.0(7) . . ? N24 C23 H23 118.5 . . ? C22 C23 H23 118.5 . . ? N31 C32 C33 125.6(12) . . ? N31 C32 C1 113.8(9) . . ? C33 C32 C1 120.6(9) . . ? N34 C33 C32 120.5(10) . . ? N34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C25 N24 C23 116.1(7) . . ? C25 N24 Ag1 119.9(5) . 9_654 ? C23 N24 Ag1 123.4(5) . 9_654 ? N31 C36 C35 122.7(10) . . ? N31 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? N21 C22 C23 119.7(7) . . ? N21 C22 C1 117.7(7) . . ? C23 C22 C1 122.5(7) . . ? C22 C1 C32 110.2(8) . . ? C22 C1 H1A 109.6 . . ? C32 C1 H1A 109.6 . . ? C22 C1 H1B 109.6 . . ? C32 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N34 C35 C36 118.0(12) . . ? N34 C35 H35 121.0 . . ? C36 C35 H35 121.0 . . ? N24 C25 C26 122.1(7) . . ? N24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C33 N34 C35 118.3(9) . . ? C33 N34 Ag1 120.6(7) . 18_545 ? C35 N34 Ag1 121.0(9) . 18_545 ? O43 Cl40 O44 111.1(6) . . ? O43 Cl40 O42 110.1(6) . . ? O44 Cl40 O42 109.0(6) . . ? O43 Cl40 O41 105.5(6) . . ? O44 Cl40 O41 112.3(7) . . ? O42 Cl40 O41 108.8(6) . . ? Cl52 Cl52 C50 160.3(10) 13_656 . ? Cl51 C50 Cl52 133.5(5) . . ? Cl51 C50 H50A 103.8 . . ? Cl52 C50 H50A 103.8 . . ? Cl51 C50 H50B 103.8 . . ? Cl52 C50 H50B 103.8 . . ? H50A C50 H50B 105.4 . . ? 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 N34 Ag1 N21 C26 -128.9(7) 17 . . . ? N24 Ag1 N21 C26 38.8(6) 5_545 . . . ? N31 Ag1 N21 C26 130.8(6) . . . . ? N34 Ag1 N21 C22 74.2(9) 17 . . . ? N24 Ag1 N21 C22 -118.0(6) 5_545 . . . ? N31 Ag1 N21 C22 -26.0(6) . . . . ? C22 N21 C26 C25 1.0(12) . . . . ? Ag1 N21 C26 C25 -156.3(6) . . . . ? N34 Ag1 N31 C32 -110.7(7) 17 . . . ? N21 Ag1 N31 C32 37.9(6) . . . . ? N24 Ag1 N31 C32 133.1(7) 5_545 . . . ? N34 Ag1 N31 C36 70.8(8) 17 . . . ? N21 Ag1 N31 C36 -140.6(8) . . . . ? N24 Ag1 N31 C36 -45.4(8) 5_545 . . . ? C36 N31 C32 C33 1.0(14) . . . . ? Ag1 N31 C32 C33 -177.7(7) . . . . ? C36 N31 C32 C1 178.6(8) . . . . ? Ag1 N31 C32 C1 -0.1(10) . . . . ? N31 C32 C33 N34 -4.8(15) . . . . ? C1 C32 C33 N34 177.8(8) . . . . ? C22 C23 N24 C25 1.8(13) . . . . ? C22 C23 N24 Ag1 -168.9(7) . . . 9_654 ? C32 N31 C36 C35 1.5(14) . . . . ? Ag1 N31 C36 C35 -179.8(6) . . . . ? C26 N21 C22 C23 0.6(13) . . . . ? Ag1 N21 C22 C23 158.3(7) . . . . ? C26 N21 C22 C1 -178.4(9) . . . . ? Ag1 N21 C22 C1 -20.7(11) . . . . ? N24 C23 C22 N21 -2.1(15) . . . . ? N24 C23 C22 C1 176.9(10) . . . . ? N21 C22 C1 C32 83.0(10) . . . . ? C23 C22 C1 C32 -95.9(11) . . . . ? N31 C32 C1 C22 -66.6(10) . . . . ? C33 C32 C1 C22 111.1(9) . . . . ? N31 C36 C35 N34 -0.5(14) . . . . ? C23 N24 C25 C26 -0.2(12) . . . . ? Ag1 N24 C25 C26 170.9(6) 9_654 . . . ? N21 C26 C25 N24 -1.3(12) . . . . ? C32 C33 N34 C35 5.6(14) . . . . ? C32 C33 N34 Ag1 -177.3(6) . . . 18_545 ? C36 C35 N34 C33 -3.2(13) . . . . ? C36 C35 N34 Ag1 179.7(6) . . . 18_545 ? Cl52 Cl52 C50 Cl51 -131(3) 13_656 . . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.510 _refine_diff_density_min -0.867 _refine_diff_density_rms 0.150 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.004 637.7 21.1 2 0.333 0.667 0.525 640.1 20.7 3 0.667 0.333 0.191 640.1 20.6 _platon_squeeze_details ; ; ####END data_1ace _database_code_depnum_ccdc_archive 'CCDC 855400' #TrackingRef 'CC_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H14 Ag Cl N4 O5' _chemical_formula_weight 437.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 28.3534(15) _cell_length_b 28.3534(15) _cell_length_c 13.9544(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9715.2(15) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4358 _cell_measurement_theta_min 2.4834 _cell_measurement_theta_max 29.1540 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3924 _exptl_absorpt_coefficient_mu 1.079 _exptl_absorpt_correction_T_min 0.20336 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -90.00 29.00 1.0000 17.5500 omega____ theta____ kappa____ phi______ frames - -19.7838 0.0000 30.0000 119 #__ type_ start__ end____ width___ exp.time_ 2 omega -13.00 90.00 1.0000 17.5500 omega____ theta____ kappa____ phi______ frames - 18.9244 77.0000 -120.0000 103 #__ type_ start__ end____ width___ exp.time_ 3 omega 34.00 85.00 1.0000 17.5500 omega____ theta____ kappa____ phi______ frames - 18.9244 179.0000 150.0000 51 #__ type_ start__ end____ width___ exp.time_ 4 omega -54.00 46.00 1.0000 17.5500 omega____ theta____ kappa____ phi______ frames - 18.9244 -37.0000 120.0000 100 ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21843 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.1099 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 29.22 _reflns_number_total 5230 _reflns_number_gt 2435 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2003)' _computing_publication_material 'CIFTAB (Sheldrick)' _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^)+(0.2000P)^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 5230 _refine_ls_number_parameters 208 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.2050 _refine_ls_R_factor_gt 0.1306 _refine_ls_wR_factor_ref 0.4174 _refine_ls_wR_factor_gt 0.3826 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.203 _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 0.26961(4) 0.19888(3) 0.39475(8) 0.0785(6) Uani 1 1 d . . . N24 N 0.1374(3) 0.2560(3) 0.5515(8) 0.065(2) Uani 1 1 d . . . C22 C 0.1684(4) 0.2259(4) 0.4201(9) 0.064(3) Uani 1 1 d . . . C32 C 0.2165(4) 0.2510(4) 0.2636(8) 0.063(3) Uani 1 1 d . . . C31 C 0.2169(4) 0.2903(4) 0.2064(8) 0.064(3) Uani 1 1 d . . . H31 H 0.1850 0.2932 0.2035 0.077 Uiso 1 1 calc R . . N33 N 0.2635(4) 0.2498(3) 0.2738(7) 0.068(2) Uani 1 1 d . . . N21 N 0.2069(3) 0.2240(4) 0.4774(8) 0.071(3) Uani 1 1 d . . . C23 C 0.1345(4) 0.2425(4) 0.4600(11) 0.068(3) Uani 1 1 d . . . H23 H 0.1082 0.2442 0.4204 0.081 Uiso 1 1 calc R . . C2 C 0.1667(4) 0.2103(4) 0.3188(9) 0.069(3) Uani 1 1 d . . . H2A H 0.1338 0.2071 0.2882 0.082 Uiso 1 1 calc R . . H2B H 0.1640 0.1741 0.3157 0.082 Uiso 1 1 calc R . . C34 C 0.3068(4) 0.2847(5) 0.2286(9) 0.076(3) Uani 1 1 d . . . H34 H 0.3398 0.2839 0.2347 0.092 Uiso 1 1 calc R . . C25 C 0.1733(5) 0.2537(5) 0.6052(10) 0.076(3) Uani 1 1 d . . . H25 H 0.1747 0.2620 0.6715 0.091 Uiso 1 1 calc R . . C26 C 0.2099(5) 0.2397(6) 0.5682(11) 0.079(3) Uani 1 1 d . . . H26 H 0.2377 0.2412 0.6083 0.095 Uiso 1 1 calc R . . N36 N 0.2595(3) 0.3246(4) 0.1549(8) 0.078(3) Uani 1 1 d . . . C35 C 0.3042(4) 0.3240(5) 0.1697(9) 0.079(4) Uani 1 1 d . . . H35 H 0.3367 0.3510 0.1399 0.095 Uiso 1 1 calc R . . Cl40 Cl 0.46000(12) 0.38874(12) 0.1349(3) 0.0838(11) Uani 1 1 d . . . O44 O 0.4300(4) 0.3310(4) 0.1309(9) 0.118(4) Uani 1 1 d . . . O42 O 0.4453(8) 0.4071(6) 0.0545(12) 0.186(7) Uani 1 1 d . . . O41 O 0.4405(9) 0.3983(9) 0.2204(13) 0.213(9) Uani 1 1 d . . . O43 O 0.5148(5) 0.4069(6) 0.1514(16) 0.204(9) Uani 1 1 d . . . O53 O 0.3514(7) 0.2033(9) 0.2856(13) 0.197(8) Uani 1 1 d D . . C50 C 0.3979(9) 0.2109(9) 0.2822(15) 0.158(9) Uani 1 1 d D . . C52 C 0.4076(13) 0.1723(17) 0.226(2) 0.260(18) Uani 1 1 d U . . H52A H 0.3739 0.1460 0.1941 0.390 Uiso 1 1 calc R . . H52B H 0.4194 0.1529 0.2696 0.390 Uiso 1 1 calc R . . H52C H 0.4360 0.1923 0.1785 0.390 Uiso 1 1 calc R . . C51 C 0.4475(11) 0.249(2) 0.340(2) 0.40(3) Uani 1 1 d DU . . H51A H 0.4403 0.2744 0.3755 0.602 Uiso 1 1 calc R . . H51B H 0.4785 0.2692 0.2967 0.602 Uiso 1 1 calc R . . H51C H 0.4560 0.2276 0.3850 0.602 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 0.0655(6) 0.0506(6) 0.1322(12) -0.0007(4) -0.0111(5) 0.0385(4) N24 0.045(4) 0.043(4) 0.107(8) 0.011(5) 0.001(5) 0.023(4) C22 0.036(5) 0.054(6) 0.101(9) 0.013(6) 0.014(5) 0.023(4) C32 0.053(6) 0.056(6) 0.082(8) -0.010(5) -0.009(5) 0.028(5) C31 0.047(5) 0.058(6) 0.093(8) 0.000(6) -0.003(5) 0.031(5) N33 0.061(5) 0.052(5) 0.108(7) 0.015(5) 0.012(5) 0.040(4) N21 0.036(4) 0.060(5) 0.118(9) 0.013(5) -0.002(5) 0.024(4) C23 0.043(5) 0.041(5) 0.120(11) 0.009(6) -0.008(6) 0.021(4) C2 0.040(5) 0.037(5) 0.118(10) 0.007(5) -0.007(5) 0.011(4) C34 0.049(6) 0.081(8) 0.113(10) 0.012(7) 0.019(6) 0.042(6) C25 0.064(7) 0.073(7) 0.103(9) 0.024(7) 0.009(6) 0.044(6) C26 0.059(7) 0.096(9) 0.094(10) 0.014(7) 0.003(6) 0.047(7) N36 0.045(5) 0.058(5) 0.136(9) 0.025(5) 0.016(5) 0.030(4) C35 0.044(6) 0.085(8) 0.112(10) 0.010(7) -0.009(6) 0.035(6) Cl40 0.0621(17) 0.0564(16) 0.123(3) -0.0144(17) 0.0061(17) 0.0218(14) O44 0.082(7) 0.072(6) 0.167(10) 0.032(6) 0.025(6) 0.013(5) O42 0.28(2) 0.111(11) 0.195(14) 0.020(9) 0.003(14) 0.121(13) O41 0.205(17) 0.29(2) 0.195(18) -0.107(15) -0.053(13) 0.164(17) O43 0.068(7) 0.123(11) 0.42(3) 0.066(13) 0.057(11) 0.044(8) O53 0.190(16) 0.28(2) 0.227(17) 0.029(14) 0.009(12) 0.195(17) C50 0.22(3) 0.21(2) 0.140(17) 0.015(15) -0.003(16) 0.18(2) C52 0.26(3) 0.46(5) 0.22(3) -0.15(3) -0.07(2) 0.30(3) C51 0.17(3) 0.78(8) 0.26(4) -0.10(5) 0.03(3) 0.24(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N24 2.240(9) 11_556 ? Ag1 N33 2.284(9) . ? Ag1 N36 2.399(9) 5 ? Ag1 N21 2.505(10) . ? N24 C25 1.291(14) . ? N24 C23 1.324(14) . ? N24 Ag1 2.241(9) 12_556 ? C22 N21 1.374(14) . ? C22 C23 1.380(15) . ? C22 C2 1.475(16) . ? C32 N33 1.357(13) . ? C32 C31 1.368(15) . ? C32 C2 1.513(15) . ? C31 N36 1.321(13) . ? C31 H31 0.9500 . ? N33 C34 1.292(13) . ? N21 C26 1.330(15) . ? C23 H23 0.9500 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C34 C35 1.414(17) . ? C34 H34 0.9500 . ? C25 C26 1.384(16) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? N36 C35 1.293(12) . ? N36 Ag1 2.399(9) 9_554 ? C35 H35 0.9500 . ? Cl40 O42 1.387(16) . ? Cl40 O43 1.390(13) . ? Cl40 O41 1.398(17) . ? Cl40 O44 1.419(10) . ? O53 C50 1.226(16) . ? C50 C52 1.48(3) . ? C50 C51 1.507(19) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N24 Ag1 N33 149.5(4) 11_556 . ? N24 Ag1 N36 107.1(3) 11_556 5 ? N33 Ag1 N36 100.8(3) . 5 ? N24 Ag1 N21 110.4(3) 11_556 . ? N33 Ag1 N21 82.6(3) . . ? N36 Ag1 N21 87.4(3) 5 . ? C25 N24 C23 118.8(10) . . ? C25 N24 Ag1 124.6(9) . 12_556 ? C23 N24 Ag1 115.9(7) . 12_556 ? N21 C22 C23 118.6(11) . . ? N21 C22 C2 117.0(9) . . ? C23 C22 C2 124.4(10) . . ? N33 C32 C31 118.3(10) . . ? N33 C32 C2 118.7(9) . . ? C31 C32 C2 123.0(10) . . ? N36 C31 C32 123.2(10) . . ? N36 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C34 N33 C32 120.0(9) . . ? C34 N33 Ag1 120.1(8) . . ? C32 N33 Ag1 118.7(7) . . ? C26 N21 C22 117.6(10) . . ? C26 N21 Ag1 126.6(7) . . ? C22 N21 Ag1 115.6(8) . . ? N24 C23 C22 122.3(10) . . ? N24 C23 H23 118.8 . . ? C22 C23 H23 118.8 . . ? C22 C2 C32 112.4(8) . . ? C22 C2 H2A 109.1 . . ? C32 C2 H2A 109.1 . . ? C22 C2 H2B 109.1 . . ? C32 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? N33 C34 C35 118.9(10) . . ? N33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? N24 C25 C26 121.4(13) . . ? N24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? N21 C26 C25 121.2(11) . . ? N21 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C35 N36 C31 116.5(10) . . ? C35 N36 Ag1 118.8(8) . 9_554 ? C31 N36 Ag1 123.5(7) . 9_554 ? N36 C35 C34 122.7(11) . . ? N36 C35 H35 118.7 . . ? C34 C35 H35 118.7 . . ? O42 Cl40 O43 119.0(11) . . ? O42 Cl40 O41 113.2(12) . . ? O43 Cl40 O41 105.4(12) . . ? O42 Cl40 O44 106.4(9) . . ? O43 Cl40 O44 110.3(8) . . ? O41 Cl40 O44 101.0(11) . . ? O53 C50 C52 118(2) . . ? O53 C50 C51 130(2) . . ? C52 C50 C51 111(2) . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N33 C32 C31 N36 5.4(18) . . . . ? C2 C32 C31 N36 -177.1(11) . . . . ? C31 C32 N33 C34 -1.4(17) . . . . ? C2 C32 N33 C34 -179.0(11) . . . . ? C31 C32 N33 Ag1 165.5(8) . . . . ? C2 C32 N33 Ag1 -12.1(13) . . . . ? N24 Ag1 N33 C34 -106.5(10) 11_556 . . . ? N36 Ag1 N33 C34 49.5(9) 5 . . . ? N21 Ag1 N33 C34 135.4(9) . . . . ? N24 Ag1 N33 C32 86.7(10) 11_556 . . . ? N36 Ag1 N33 C32 -117.4(8) 5 . . . ? N21 Ag1 N33 C32 -31.5(8) . . . . ? C23 C22 N21 C26 -1.6(15) . . . . ? C2 C22 N21 C26 178.0(9) . . . . ? C23 C22 N21 Ag1 -176.4(7) . . . . ? C2 C22 N21 Ag1 3.1(11) . . . . ? N24 Ag1 N21 C26 71.5(10) 11_556 . . . ? N33 Ag1 N21 C26 -137.1(10) . . . . ? N36 Ag1 N21 C26 -35.8(9) 5 . . . ? N24 Ag1 N21 C22 -114.2(7) 11_556 . . . ? N33 Ag1 N21 C22 37.3(7) . . . . ? N36 Ag1 N21 C22 138.5(7) 5 . . . ? C25 N24 C23 C22 0.2(15) . . . . ? Ag1 N24 C23 C22 -171.3(7) 12_556 . . . ? N21 C22 C23 N24 -0.7(15) . . . . ? C2 C22 C23 N24 179.7(9) . . . . ? N21 C22 C2 C32 -68.6(12) . . . . ? C23 C22 C2 C32 111.0(11) . . . . ? N33 C32 C2 C22 78.5(12) . . . . ? C31 C32 C2 C22 -99.0(12) . . . . ? C32 N33 C34 C35 0.7(18) . . . . ? Ag1 N33 C34 C35 -165.9(10) . . . . ? C23 N24 C25 C26 2.5(16) . . . . ? Ag1 N24 C25 C26 173.3(9) 12_556 . . . ? C22 N21 C26 C25 4.3(17) . . . . ? Ag1 N21 C26 C25 178.5(8) . . . . ? N24 C25 C26 N21 -5.0(19) . . . . ? C32 C31 N36 C35 -8.4(18) . . . . ? C32 C31 N36 Ag1 -176.3(8) . . . 9_554 ? C31 N36 C35 C34 7.7(19) . . . . ? Ag1 N36 C35 C34 176.2(10) 9_554 . . . ? N33 C34 C35 N36 -4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 3.332 _refine_diff_density_min -1.114 _refine_diff_density_rms 0.186 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 -0.005 916.7 11.3 2 0.333 0.667 0.378 918.0 11.1 3 0.667 0.333 0.045 917.9 11.1 _platon_squeeze_details ; ; ####END data_2a_syn _database_code_depnum_ccdc_archive 'CCDC 855401' #TrackingRef 'CC_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H10 Ag Cl N4 O5' _chemical_formula_weight 397.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 7.1340(6) _cell_length_b 18.3483(17) _cell_length_c 10.5892(12) _cell_angle_alpha 90.00 _cell_angle_beta 108.596(10) _cell_angle_gamma 90.00 _cell_volume 1313.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4624 _cell_measurement_theta_min 3.0022 _cell_measurement_theta_max 29.2455 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.763 _exptl_absorpt_correction_T_min 0.69524 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 43.00 69.00 1.0000 3.1200 omega____ theta____ kappa____ phi______ frames - 18.4797 179.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 2 omega -28.00 45.00 1.0000 3.1200 omega____ theta____ kappa____ phi______ frames - -19.1829 37.0000 -120.0000 73 #__ type_ start__ end____ width___ exp.time_ 3 omega -91.00 16.00 1.0000 3.1200 omega____ theta____ kappa____ phi______ frames - -19.1829 0.0000 30.0000 107 #__ type_ start__ end____ width___ exp.time_ 4 omega -12.00 89.00 1.0000 3.1200 omega____ theta____ kappa____ phi______ frames - 18.4797 77.0000 -120.0000 101 #__ type_ start__ end____ width___ exp.time_ 5 omega -12.00 89.00 1.0000 3.1200 omega____ theta____ kappa____ phi______ frames - 18.4797 77.0000 0.0000 101 #__ type_ start__ end____ width___ exp.time_ 6 omega -49.00 33.00 1.0000 3.1200 omega____ theta____ kappa____ phi______ frames - -19.1829 77.0000 -30.0000 82 #__ type_ start__ end____ width___ exp.time_ 7 omega -96.00 -32.00 1.0000 3.1200 omega____ theta____ kappa____ phi______ frames - -19.1829 179.0000 0.0000 64 ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14822 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0556 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 29.31 _reflns_number_total 3234 _reflns_number_gt 2440 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2003)' _computing_publication_material 'CIFTAB (Sheldrick)' _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^)+(0.0267P)^2^+2.3508P] 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 3234 _refine_ls_number_parameters 187 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0754 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.01236(4) 0.099880(17) 0.64259(3) 0.02388(11) Uani 1 1 d . . . O40 O 0.1106(5) 0.0098(2) 0.8756(4) 0.0425(9) Uani 1 1 d D . . N24 N 0.0347(5) 0.30943(19) 0.3142(4) 0.0279(8) Uani 1 1 d . . . C1 C 0.1843(6) 0.1129(2) 0.3832(4) 0.0217(9) Uani 1 1 d . . . H1A H 0.0783 0.0758 0.3670 0.026 Uiso 1 1 calc R . . H1B H 0.2346 0.1121 0.3062 0.026 Uiso 1 1 calc R . . Cl31 Cl 0.51316(16) 0.35581(7) 0.60493(11) 0.0329(3) Uani 1 1 d . . . N21 N -0.0082(5) 0.19440(18) 0.4746(3) 0.0234(8) Uani 1 1 d . . . O33 O 0.5630(8) 0.3773(3) 0.4939(5) 0.116(2) Uani 1 1 d . . . C26 C -0.0921(6) 0.2590(2) 0.4773(4) 0.0308(10) Uani 1 1 d . . . H26 H -0.1680 0.2660 0.5355 0.037 Uiso 1 1 calc R . . C23 C 0.1201(6) 0.2446(2) 0.3128(4) 0.0244(9) Uani 1 1 d . . . H23 H 0.1986 0.2379 0.2562 0.029 Uiso 1 1 calc R . . O35 O 0.3400(5) 0.3953(2) 0.6052(4) 0.0526(10) Uani 1 1 d . . . N11 N 0.3022(4) 0.06845(17) 0.6133(3) 0.0185(7) Uani 1 1 d . . . C22 C 0.0974(5) 0.1870(2) 0.3915(4) 0.0188(8) Uani 1 1 d . . . C12 C 0.3493(5) 0.0925(2) 0.5067(4) 0.0171(8) Uani 1 1 d . . . N14 N 0.6934(4) 0.07081(17) 0.6156(3) 0.0178(7) Uani 1 1 d . . . C25 C -0.0715(7) 0.3161(3) 0.3978(5) 0.0343(11) Uani 1 1 d . . . H25 H -0.1341 0.3612 0.4023 0.041 Uiso 1 1 calc R . . C13 C 0.5459(5) 0.0946(2) 0.5105(4) 0.0184(8) Uani 1 1 d . . . H13 H 0.5765 0.1135 0.4359 0.022 Uiso 1 1 calc R . . O34 O 0.6703(6) 0.3736(3) 0.7202(5) 0.0887(17) Uani 1 1 d . . . O32 O 0.4796(7) 0.2810(2) 0.6014(6) 0.0975(18) Uani 1 1 d . . . C15 C 0.6445(5) 0.0447(2) 0.7187(4) 0.0196(8) Uani 1 1 d . . . H15 H 0.7449 0.0255 0.7936 0.024 Uiso 1 1 calc R . . C16 C 0.4510(5) 0.0450(2) 0.7187(4) 0.0205(8) Uani 1 1 d . . . H16 H 0.4223 0.0282 0.7954 0.025 Uiso 1 1 calc R . . H40A H 0.168(6) -0.0312(15) 0.891(5) 0.031 Uiso 1 1 d D . . H40B H 0.184(6) 0.037(2) 0.934(4) 0.031 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01704(16) 0.02634(18) 0.0332(2) -0.00023(15) 0.01503(13) -0.00092(13) O40 0.0300(19) 0.051(2) 0.043(2) 0.0011(19) 0.0082(16) 0.0045(16) N24 0.0299(19) 0.024(2) 0.030(2) 0.0048(16) 0.0100(16) 0.0071(15) C1 0.024(2) 0.022(2) 0.017(2) -0.0013(17) 0.0033(16) 0.0020(16) Cl31 0.0328(6) 0.0377(7) 0.0311(6) -0.0008(5) 0.0143(5) 0.0041(5) N21 0.0258(17) 0.0226(19) 0.0250(19) 0.0042(15) 0.0128(14) 0.0068(14) O33 0.131(5) 0.166(6) 0.094(4) 0.080(4) 0.094(4) 0.097(4) C26 0.036(2) 0.031(3) 0.032(3) 0.008(2) 0.021(2) 0.016(2) C23 0.0206(19) 0.028(2) 0.024(2) 0.0010(19) 0.0068(16) 0.0039(17) O35 0.042(2) 0.078(3) 0.039(2) -0.007(2) 0.0139(17) 0.0147(19) N11 0.0183(16) 0.0170(17) 0.0231(19) -0.0023(14) 0.0106(14) -0.0007(13) C22 0.0169(18) 0.024(2) 0.014(2) -0.0005(17) 0.0026(15) 0.0027(15) C12 0.0197(18) 0.0142(19) 0.020(2) -0.0015(16) 0.0103(15) 0.0004(15) N14 0.0173(15) 0.0147(16) 0.0232(19) -0.0006(14) 0.0091(13) -0.0012(13) C25 0.041(3) 0.031(3) 0.033(3) 0.005(2) 0.015(2) 0.017(2) C13 0.0210(19) 0.0165(19) 0.021(2) 0.0026(17) 0.0118(16) -0.0002(15) O34 0.054(3) 0.086(3) 0.090(4) -0.030(3) -0.028(2) 0.018(2) O32 0.086(3) 0.041(3) 0.151(5) -0.003(3) 0.018(3) -0.011(2) C15 0.0198(19) 0.018(2) 0.020(2) -0.0017(17) 0.0047(16) -0.0020(15) C16 0.0212(19) 0.021(2) 0.021(2) -0.0025(17) 0.0091(16) -0.0024(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N11 2.262(3) . ? Ag1 N14 2.265(3) 1_455 ? Ag1 N24 2.432(4) 4_566 ? Ag1 N21 2.455(3) . ? O40 H40A 0.847(19) . ? O40 H40B 0.837(19) . ? N24 C23 1.338(5) . ? N24 C25 1.341(6) . ? N24 Ag1 2.432(4) 4_565 ? C1 C12 1.501(5) . ? C1 C22 1.509(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? Cl31 O33 1.389(4) . ? Cl31 O32 1.393(5) . ? Cl31 O34 1.407(4) . ? Cl31 O35 1.432(3) . ? N21 C26 1.332(5) . ? N21 C22 1.335(5) . ? C26 C25 1.382(6) . ? C26 H26 0.9500 . ? C23 C22 1.387(5) . ? C23 H23 0.9500 . ? N11 C16 1.342(5) . ? N11 C12 1.351(5) . ? C12 C13 1.390(5) . ? N14 C15 1.337(5) . ? N14 C13 1.338(5) . ? N14 Ag1 2.265(3) 1_655 ? C25 H25 0.9500 . ? C13 H13 0.9500 . ? C15 C16 1.380(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 Ag1 N14 148.05(11) . 1_455 ? N11 Ag1 N24 115.61(11) . 4_566 ? N14 Ag1 N24 94.54(11) 1_455 4_566 ? N11 Ag1 N21 85.80(11) . . ? N14 Ag1 N21 104.45(11) 1_455 . ? N24 Ag1 N21 91.87(12) 4_566 . ? H40A O40 H40B 104(4) . . ? C23 N24 C25 116.3(4) . . ? C23 N24 Ag1 121.4(3) . 4_565 ? C25 N24 Ag1 121.0(3) . 4_565 ? C12 C1 C22 113.3(3) . . ? C12 C1 H1A 108.9 . . ? C22 C1 H1A 108.9 . . ? C12 C1 H1B 108.9 . . ? C22 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O33 Cl31 O32 110.2(4) . . ? O33 Cl31 O34 108.7(4) . . ? O32 Cl31 O34 109.5(3) . . ? O33 Cl31 O35 108.2(3) . . ? O32 Cl31 O35 110.9(3) . . ? O34 Cl31 O35 109.3(3) . . ? C26 N21 C22 117.1(4) . . ? C26 N21 Ag1 122.4(3) . . ? C22 N21 Ag1 119.4(3) . . ? N21 C26 C25 121.7(4) . . ? N21 C26 H26 119.2 . . ? C25 C26 H26 119.2 . . ? N24 C23 C22 122.0(4) . . ? N24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C16 N11 C12 117.3(3) . . ? C16 N11 Ag1 118.9(2) . . ? C12 N11 Ag1 120.9(2) . . ? N21 C22 C23 121.2(4) . . ? N21 C22 C1 117.2(3) . . ? C23 C22 C1 121.6(3) . . ? N11 C12 C13 120.1(3) . . ? N11 C12 C1 118.3(3) . . ? C13 C12 C1 121.5(3) . . ? C15 N14 C13 117.1(3) . . ? C15 N14 Ag1 119.7(2) . 1_655 ? C13 N14 Ag1 121.4(2) . 1_655 ? N24 C25 C26 121.7(4) . . ? N24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? N14 C13 C12 122.3(3) . . ? N14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? N14 C15 C16 121.3(4) . . ? N14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? N11 C16 C15 121.8(4) . . ? N11 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? 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 N11 Ag1 N21 C26 -147.0(3) . . . . ? N14 Ag1 N21 C26 63.7(3) 1_455 . . . ? N24 Ag1 N21 C26 -31.4(3) 4_566 . . . ? N11 Ag1 N21 C22 20.7(3) . . . . ? N14 Ag1 N21 C22 -128.6(3) 1_455 . . . ? N24 Ag1 N21 C22 136.3(3) 4_566 . . . ? C22 N21 C26 C25 0.1(6) . . . . ? Ag1 N21 C26 C25 168.0(3) . . . . ? C25 N24 C23 C22 1.1(6) . . . . ? Ag1 N24 C23 C22 -165.9(3) 4_565 . . . ? N14 Ag1 N11 C16 -104.5(3) 1_455 . . . ? N24 Ag1 N11 C16 54.7(3) 4_566 . . . ? N21 Ag1 N11 C16 144.7(3) . . . . ? N14 Ag1 N11 C12 95.6(3) 1_455 . . . ? N24 Ag1 N11 C12 -105.3(3) 4_566 . . . ? N21 Ag1 N11 C12 -15.2(3) . . . . ? C26 N21 C22 C23 0.7(6) . . . . ? Ag1 N21 C22 C23 -167.6(3) . . . . ? C26 N21 C22 C1 -177.1(4) . . . . ? Ag1 N21 C22 C1 14.6(4) . . . . ? N24 C23 C22 N21 -1.4(6) . . . . ? N24 C23 C22 C1 176.3(4) . . . . ? C12 C1 C22 N21 -70.0(4) . . . . ? C12 C1 C22 C23 112.2(4) . . . . ? C16 N11 C12 C13 -2.0(5) . . . . ? Ag1 N11 C12 C13 158.2(3) . . . . ? C16 N11 C12 C1 174.7(3) . . . . ? Ag1 N11 C12 C1 -25.0(4) . . . . ? C22 C1 C12 N11 78.8(4) . . . . ? C22 C1 C12 C13 -104.5(4) . . . . ? C23 N24 C25 C26 -0.3(7) . . . . ? Ag1 N24 C25 C26 166.8(3) 4_565 . . . ? N21 C26 C25 N24 -0.3(7) . . . . ? C15 N14 C13 C12 -0.1(5) . . . . ? Ag1 N14 C13 C12 -164.4(3) 1_655 . . . ? N11 C12 C13 N14 2.5(6) . . . . ? C1 C12 C13 N14 -174.2(3) . . . . ? C13 N14 C15 C16 -2.5(6) . . . . ? Ag1 N14 C15 C16 162.1(3) 1_655 . . . ? C12 N11 C16 C15 -0.6(6) . . . . ? Ag1 N11 C16 C15 -161.2(3) . . . . ? N14 C15 C16 N11 3.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.131 _refine_diff_density_min -0.773 _refine_diff_density_rms 0.135 #####END data_2_(from_1as) _database_code_depnum_ccdc_archive 'CCDC 855402' #TrackingRef 'CC_final.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H10 Ag Cl N4 O5' _chemical_formula_weight 397.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1312(2) _cell_length_b 18.2962(4) _cell_length_c 10.5785(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.561(3) _cell_angle_gamma 90.00 _cell_volume 1308.43(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4846 _cell_measurement_theta_min 3.0071 _cell_measurement_theta_max 29.1410 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.018 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.770 _exptl_absorpt_correction_T_min 0.98841 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -46.00 43.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.8463 -77.0000 30.0000 89 #__ type_ start__ end____ width___ exp.time_ 2 omega -89.00 -51.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.6276 -37.0000 -90.0000 38 #__ type_ start__ end____ width___ exp.time_ 3 omega -88.00 10.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.6276 -77.0000 -120.0000 98 #__ type_ start__ end____ width___ exp.time_ 4 omega -54.00 46.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.8463 -37.0000 -120.0000 100 #__ type_ start__ end____ width___ exp.time_ 5 omega 34.00 97.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.8463 179.0000 -120.0000 63 #__ type_ start__ end____ width___ exp.time_ 6 omega -13.00 64.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - 18.8463 77.0000 150.0000 77 #__ type_ start__ end____ width___ exp.time_ 7 omega -92.00 8.00 1.0000 15.0000 omega____ theta____ kappa____ phi______ frames - -19.6276 -37.0000 -30.0000 100 ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14744 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 29.21 _reflns_number_total 3219 _reflns_number_gt 2668 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2003)' _computing_publication_material 'CIFTAB (Sheldrick)' _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^)+(0.0233P)^2^+1.8353P] 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 3219 _refine_ls_number_parameters 187 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Ag1 Ag 0.98765(3) 0.400459(13) 0.35731(3) 0.02146(9) Uani 1 1 d . . . Cl30 Cl 0.51222(13) 0.64466(5) 0.10460(9) 0.0287(2) Uani 1 1 d . . . N11 N 1.0083(4) 0.30568(15) 0.5247(3) 0.0225(6) Uani 1 1 d . . . C22 C 0.6497(4) 0.40831(15) 0.4930(3) 0.0160(6) Uani 1 1 d . . . C23 C 0.4539(5) 0.40526(15) 0.4897(3) 0.0175(6) Uani 1 1 d . . . H23 H 0.4234 0.3859 0.5641 0.021 Uiso 1 1 calc R . . C15 C 1.0712(5) 0.18357(19) 0.6018(4) 0.0298(8) Uani 1 1 d . . . H15 H 1.1341 0.1383 0.5971 0.036 Uiso 1 1 calc R . . N21 N 0.6974(4) 0.43162(13) 0.3865(3) 0.0166(5) Uani 1 1 d . . . C16 C 1.0913(5) 0.24049(19) 0.5223(3) 0.0286(8) Uani 1 1 d . . . H16 H 1.1667 0.2332 0.4637 0.034 Uiso 1 1 calc R . . O34 O 0.3394(4) 0.60439(17) 0.1049(3) 0.0497(8) Uani 1 1 d . . . C12 C 0.9025(4) 0.31294(16) 0.6082(3) 0.0174(6) Uani 1 1 d . . . C13 C 0.8803(5) 0.25500(17) 0.6875(3) 0.0221(7) Uani 1 1 d . . . H13 H 0.8024 0.2618 0.7446 0.026 Uiso 1 1 calc R . . N24 N 0.3066(4) 0.42900(13) 0.3840(3) 0.0170(5) Uani 1 1 d . . . C1 C 0.8157(5) 0.38709(16) 0.6168(3) 0.0192(7) Uani 1 1 d . . . H1A H 0.9220 0.4242 0.6335 0.023 Uiso 1 1 calc R . . H1B H 0.7655 0.3876 0.6939 0.023 Uiso 1 1 calc R . . C26 C 0.5496(4) 0.45507(17) 0.2812(3) 0.0188(7) Uani 1 1 d . . . H26 H 0.5787 0.4718 0.2045 0.023 Uiso 1 1 calc R . . C25 C 0.3560(4) 0.45561(16) 0.2809(3) 0.0176(6) Uani 1 1 d . . . H25 H 0.2559 0.4752 0.2062 0.021 Uiso 1 1 calc R . . N14 N 0.9656(4) 0.19002(15) 0.6856(3) 0.0248(6) Uani 1 1 d . . . O31 O 0.5605(7) 0.6236(3) -0.0077(5) 0.114(2) Uani 1 1 d . . . O33 O 0.4783(6) 0.71939(18) 0.1022(5) 0.0902(15) Uani 1 1 d . . . O32 O 0.6713(5) 0.6267(2) 0.2179(4) 0.0892(15) Uani 1 1 d . . . O40 O 0.8884(4) 0.49071(16) 0.1230(3) 0.0407(7) Uani 1 1 d D . . H40A H 0.835(6) 0.5331(15) 0.119(5) 0.061 Uiso 1 1 d D . . H40B H 0.827(6) 0.461(2) 0.060(4) 0.061 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01562(13) 0.02393(13) 0.02909(15) 0.00016(11) 0.01314(10) -0.00068(10) Cl30 0.0280(4) 0.0329(4) 0.0279(4) 0.0003(4) 0.0125(4) -0.0033(4) N11 0.0209(14) 0.0244(14) 0.0247(15) 0.0046(12) 0.0108(12) 0.0062(11) C22 0.0174(15) 0.0127(14) 0.0194(16) -0.0018(12) 0.0080(13) 0.0016(11) C23 0.0218(16) 0.0146(14) 0.0196(16) 0.0016(12) 0.0114(13) 0.0003(12) C15 0.036(2) 0.0267(18) 0.0297(19) 0.0080(15) 0.0153(16) 0.0148(16) N21 0.0147(13) 0.0164(12) 0.0200(14) -0.0025(10) 0.0075(11) -0.0015(10) C16 0.0321(19) 0.0328(19) 0.0255(18) 0.0078(15) 0.0158(16) 0.0165(16) O34 0.0368(17) 0.071(2) 0.0424(18) 0.0081(15) 0.0147(14) -0.0162(15) C12 0.0131(15) 0.0212(15) 0.0158(15) 0.0006(12) 0.0014(12) 0.0013(12) C13 0.0202(16) 0.0274(17) 0.0196(16) 0.0012(14) 0.0078(13) 0.0036(13) N24 0.0137(13) 0.0161(12) 0.0227(14) 0.0002(11) 0.0081(11) -0.0014(10) C1 0.0188(16) 0.0219(16) 0.0162(15) -0.0011(12) 0.0048(13) 0.0034(12) C26 0.0211(16) 0.0200(15) 0.0153(15) -0.0024(12) 0.0058(13) -0.0005(13) C25 0.0175(15) 0.0140(14) 0.0197(16) 0.0000(12) 0.0036(13) 0.0003(12) N14 0.0266(15) 0.0210(14) 0.0280(16) 0.0031(12) 0.0102(13) 0.0047(12) O31 0.123(4) 0.165(4) 0.095(3) -0.086(3) 0.092(3) -0.097(3) O33 0.078(3) 0.0355(18) 0.145(4) 0.001(2) 0.018(3) 0.0101(18) O32 0.050(2) 0.079(2) 0.097(3) 0.031(2) -0.035(2) -0.0196(19) O40 0.0318(16) 0.0474(18) 0.0410(17) 0.0011(14) 0.0087(13) 0.0054(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 N21 2.261(2) . ? Ag1 N24 2.262(2) 1_655 ? Ag1 N14 2.426(3) 4_565 ? Ag1 N11 2.449(3) . ? Cl30 O33 1.387(3) . ? Cl30 O31 1.392(4) . ? Cl30 O32 1.402(3) . ? Cl30 O34 1.437(3) . ? N11 C16 1.335(4) . ? N11 C12 1.339(4) . ? C22 N21 1.346(4) . ? C22 C23 1.387(4) . ? C22 C1 1.510(4) . ? C23 N24 1.339(4) . ? C23 H23 0.9500 . ? C15 N14 1.339(5) . ? C15 C16 1.374(5) . ? C15 H15 0.9500 . ? N21 C26 1.337(4) . ? C16 H16 0.9500 . ? C12 C13 1.392(4) . ? C12 C1 1.506(4) . ? C13 N14 1.338(4) . ? C13 H13 0.9500 . ? N24 C25 1.340(4) . ? N24 Ag1 2.262(2) 1_455 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C26 C25 1.380(4) . ? C26 H26 0.9500 . ? C25 H25 0.9500 . ? N14 Ag1 2.426(3) 4_566 ? O40 H40A 0.860(19) . ? O40 H40B 0.861(19) . ? 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 N21 Ag1 N24 148.50(9) . 1_655 ? N21 Ag1 N14 115.49(9) . 4_565 ? N24 Ag1 N14 94.24(9) 1_655 4_565 ? N21 Ag1 N11 85.80(9) . . ? N24 Ag1 N11 104.27(9) 1_655 . ? N14 Ag1 N11 91.88(10) 4_565 . ? O33 Cl30 O31 110.2(3) . . ? O33 Cl30 O32 109.6(3) . . ? O31 Cl30 O32 108.2(3) . . ? O33 Cl30 O34 111.1(2) . . ? O31 Cl30 O34 107.8(2) . . ? O32 Cl30 O34 109.8(2) . . ? C16 N11 C12 116.6(3) . . ? C16 N11 Ag1 123.0(2) . . ? C12 N11 Ag1 119.3(2) . . ? N21 C22 C23 120.8(3) . . ? N21 C22 C1 118.1(3) . . ? C23 C22 C1 121.1(3) . . ? N24 C23 C22 121.6(3) . . ? N24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? N14 C15 C16 121.9(3) . . ? N14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C26 N21 C22 117.2(3) . . ? C26 N21 Ag1 118.7(2) . . ? C22 N21 Ag1 121.4(2) . . ? N11 C16 C15 122.2(3) . . ? N11 C16 H16 118.9 . . ? C15 C16 H16 118.9 . . ? N11 C12 C13 121.2(3) . . ? N11 C12 C1 117.3(3) . . ? C13 C12 C1 121.5(3) . . ? N14 C13 C12 121.9(3) . . ? N14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C23 N24 C25 117.2(3) . . ? C23 N24 Ag1 121.3(2) . 1_455 ? C25 N24 Ag1 119.8(2) . 1_455 ? C12 C1 C22 113.7(2) . . ? C12 C1 H1A 108.8 . . ? C22 C1 H1A 108.8 . . ? C12 C1 H1B 108.8 . . ? C22 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N21 C26 C25 121.8(3) . . ? N21 C26 H26 119.1 . . ? C25 C26 H26 119.1 . . ? N24 C25 C26 121.2(3) . . ? N24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C13 N14 C15 116.2(3) . . ? C13 N14 Ag1 121.1(2) . 4_566 ? C15 N14 Ag1 121.3(2) . 4_566 ? H40A O40 H40B 115(4) . . ? 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 N21 Ag1 N11 C16 146.5(3) . . . . ? N24 Ag1 N11 C16 -63.8(3) 1_655 . . . ? N14 Ag1 N11 C16 31.1(3) 4_565 . . . ? N21 Ag1 N11 C12 -20.9(2) . . . . ? N24 Ag1 N11 C12 128.8(2) 1_655 . . . ? N14 Ag1 N11 C12 -136.3(2) 4_565 . . . ? N21 C22 C23 N24 -3.7(4) . . . . ? C1 C22 C23 N24 175.0(3) . . . . ? C23 C22 N21 C26 3.4(4) . . . . ? C1 C22 N21 C26 -175.4(3) . . . . ? C23 C22 N21 Ag1 -157.6(2) . . . . ? C1 C22 N21 Ag1 23.6(3) . . . . ? N24 Ag1 N21 C26 104.5(3) 1_655 . . . ? N14 Ag1 N21 C26 -54.7(2) 4_565 . . . ? N11 Ag1 N21 C26 -144.8(2) . . . . ? N24 Ag1 N21 C22 -94.7(3) 1_655 . . . ? N14 Ag1 N21 C22 106.1(2) 4_565 . . . ? N11 Ag1 N21 C22 16.0(2) . . . . ? C12 N11 C16 C15 -0.5(5) . . . . ? Ag1 N11 C16 C15 -168.2(3) . . . . ? N14 C15 C16 N11 0.6(6) . . . . ? C16 N11 C12 C13 -0.3(4) . . . . ? Ag1 N11 C12 C13 167.9(2) . . . . ? C16 N11 C12 C1 177.2(3) . . . . ? Ag1 N11 C12 C1 -14.5(4) . . . . ? N11 C12 C13 N14 1.0(5) . . . . ? C1 C12 C13 N14 -176.4(3) . . . . ? C22 C23 N24 C25 0.3(4) . . . . ? C22 C23 N24 Ag1 165.5(2) . . . 1_455 ? N11 C12 C1 C22 69.8(4) . . . . ? C13 C12 C1 C22 -112.6(3) . . . . ? N21 C22 C1 C12 -77.6(3) . . . . ? C23 C22 C1 C12 103.6(3) . . . . ? C22 N21 C26 C25 0.1(4) . . . . ? Ag1 N21 C26 C25 161.6(2) . . . . ? C23 N24 C25 C26 3.2(4) . . . . ? Ag1 N24 C25 C26 -162.2(2) 1_455 . . . ? N21 C26 C25 N24 -3.5(5) . . . . ? C12 C13 N14 C15 -0.9(5) . . . . ? C12 C13 N14 Ag1 166.1(2) . . . 4_566 ? C16 C15 N14 C13 0.1(5) . . . . ? C16 C15 N14 Ag1 -166.8(3) . . . 4_566 ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.755 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.116 ####END