# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 #1. submission details _publ_contact_author # Name and address of author for correspondence ; Dr C. Train Laboratoire de chimie Inorganique et Materiaux Moleculaires CIM2 Unit CNRS 7071 Universite Pierre et Marie Curie 4 place Jussieu, case 42 75252 Paris Cedex 05 France ; _publ_contact_author_phone '(33) 01 44 27 30 59' _publ_contact_author_fax '(33) 01 44 27 38 41' _publ_contact_author_email train@ccr.jussieu.fr _publ_section_title ; First Verdazyl-based Extended Structures: Synthesis, Structures and Magnetic Properties of Silver(I) 1D Compounds. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address F.Pointillart ; Laboratoire de chimie Inorganique et Materiaux Moleculaires CIM2 Unit CNRS 7071 Universite Pierre et Marie Curie 4 place Jussieu, case 42 75252 Paris Cedex 05 France ; C.Train ; Laboratoire de chimie Inorganique et Materiaux Moleculaires CIM2 Unit CNRS 7071 Universite Pierre et Marie Curie 4 place Jussieu, case 42 75252 Paris Cedex 05 France ; P.Herson ; Laboratoire de chimie Inorganique et Materiaux Moleculaires CIM2 Unit CNRS 7071 Universite Pierre et Marie Curie 4 place Jussieu, case 42 75252 Paris Cedex 05 France ; J.Marrot ; Institut Lavoisier de Versailles, UMR CNRS 8180 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles Cedex France ; M.Verdaguer ; Laboratoire de chimie Inorganique et Materiaux Moleculaires CIM2 Unit CNRS 7071 Universite Pierre et Marie Curie 4 place Jussieu, case 42 75252 Paris Cedex 05 France ; _publ_section_references ; Sheldrick, G.M. (1993). SHELXL-93. Program for crystal structure determination. Univ. of G\"ottingen, Federal Republic of Germany. Sheldrick, G.M. (1997). SHELXS-86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. ; _publ_contact_author_name 'Dr C. Train' #============================================================================== data_fp303sa _database_code_depnum_ccdc_archive 'CCDC 634853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H15 Ag Cl N6 O6' _chemical_formula_weight 458.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3656(4) _cell_length_b 14.7041(6) _cell_length_c 11.0971(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.493(2) _cell_angle_gamma 90.00 _cell_volume 1573.77(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5202 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 33.04 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.936 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 1.493 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7158 _exptl_absorpt_correction_T_max 0.9707 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38252 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 35.48 _reflns_number_total 7122 _reflns_number_gt 4716 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0605P)^2^+4.7303P] 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 7122 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1310 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Ag Ag 0.65043(3) 0.227738(19) 0.48877(2) 0.02974(9) Uani 1 1 d . . . N1 N 0.5532(2) 0.18323(17) 0.2789(2) 0.0176(4) Uani 1 1 d . . . C2 C 0.6155(3) 0.1279(2) 0.2195(3) 0.0207(5) Uani 1 1 d . . . C3 C 0.5544(3) 0.1111(2) 0.0880(3) 0.0220(6) Uani 1 1 d . . . H3 H 0.5996 0.0743 0.0451 0.026 Uiso 1 1 calc R . . C4 C 0.4253(3) 0.1492(2) 0.0201(3) 0.0196(5) Uani 1 1 d . . . N5 N 0.3644(3) 0.20418(17) 0.0805(2) 0.0176(4) Uani 1 1 d . . . C6 C 0.4327(3) 0.22007(18) 0.2061(3) 0.0155(5) Uani 1 1 d . . . C7 C 0.3713(3) 0.28891(19) 0.2688(2) 0.0156(5) Uani 1 1 d . . . N8 N 0.2532(2) 0.32756(18) 0.1942(2) 0.0188(4) Uani 1 1 d . . . N9 N 0.2072(3) 0.39560(18) 0.2502(3) 0.0218(5) Uani 1 1 d . . . C10 C 0.2739(3) 0.4232(2) 0.3770(3) 0.0217(5) Uani 1 1 d . . . O10 O 0.2285(3) 0.48413(18) 0.4240(3) 0.0336(6) Uani 1 1 d . . . N11 N 0.3937(3) 0.37589(18) 0.4447(2) 0.0207(5) Uani 1 1 d . . . N12 N 0.4444(2) 0.30846(17) 0.3912(2) 0.0172(4) Uani 1 1 d . . . C13 C 0.7517(4) 0.0882(3) 0.3027(4) 0.0326(7) Uani 1 1 d . . . H13A H 0.8155 0.1373 0.3467 0.049 Uiso 1 1 calc R . . H13B H 0.7907 0.0535 0.2487 0.049 Uiso 1 1 calc R . . H13C H 0.7382 0.0479 0.3674 0.049 Uiso 1 1 calc R . . C14 C 0.3507(4) 0.1344(2) -0.1209(3) 0.0301(7) Uani 1 1 d . . . H14A H 0.2561 0.1137 -0.1365 0.045 Uiso 1 1 calc R . . H14B H 0.3994 0.0882 -0.1517 0.045 Uiso 1 1 calc R . . H14C H 0.3473 0.1915 -0.1674 0.045 Uiso 1 1 calc R . . C15 C 0.0800(3) 0.4407(3) 0.1674(4) 0.0311(7) Uani 1 1 d . . . H15A H 0.0929 0.4650 0.0904 0.047 Uiso 1 1 calc R . . H15B H 0.0582 0.4906 0.2154 0.047 Uiso 1 1 calc R . . H15C H 0.0036 0.3968 0.1411 0.047 Uiso 1 1 calc R . . C16 C 0.4736(4) 0.3951(2) 0.5815(3) 0.0289(7) Uani 1 1 d . . . H16A H 0.4606 0.3455 0.6350 0.043 Uiso 1 1 calc R . . H16B H 0.4416 0.4523 0.6061 0.043 Uiso 1 1 calc R . . H16C H 0.5722 0.4002 0.5948 0.043 Uiso 1 1 calc R . . O1W O 0.9839(4) 0.0470(2) 0.6907(3) 0.0475(8) Uani 1 1 d . . . Cl Cl 0.18443(9) 0.17178(6) 0.47789(10) 0.03418(19) Uani 1 1 d . . . O2 O 0.2289(5) 0.0920(3) 0.4357(6) 0.102(2) Uani 1 1 d . . . O3 O 0.1293(4) 0.2362(2) 0.3770(3) 0.0488(8) Uani 1 1 d . . . O4 O 0.2985(4) 0.2111(3) 0.5811(3) 0.0497(8) Uani 1 1 d . . . O5 O 0.0774(4) 0.1520(3) 0.5290(5) 0.0831(16) 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 Ag 0.02163(12) 0.03951(16) 0.01443(11) -0.00394(9) -0.00952(8) 0.00373(10) N1 0.0129(9) 0.0217(11) 0.0137(10) -0.0021(8) -0.0006(8) 0.0001(8) C2 0.0170(12) 0.0228(13) 0.0200(13) -0.0035(10) 0.0041(10) 0.0005(10) C3 0.0248(14) 0.0233(13) 0.0196(13) -0.0034(10) 0.0102(11) 0.0001(11) C4 0.0255(13) 0.0211(12) 0.0103(11) -0.0016(9) 0.0045(10) -0.0027(10) N5 0.0174(10) 0.0235(11) 0.0082(9) -0.0006(8) 0.0003(8) -0.0019(9) C6 0.0134(10) 0.0194(12) 0.0103(10) -0.0001(9) 0.0002(8) -0.0019(9) C7 0.0126(10) 0.0230(12) 0.0078(10) -0.0006(8) -0.0002(8) 0.0014(9) N8 0.0138(10) 0.0250(12) 0.0134(10) 0.0006(9) 0.0001(8) 0.0017(9) N9 0.0173(11) 0.0260(12) 0.0203(11) 0.0025(9) 0.0047(9) 0.0049(9) C10 0.0203(13) 0.0230(13) 0.0232(14) 0.0008(11) 0.0097(11) 0.0015(10) O10 0.0363(14) 0.0323(13) 0.0344(14) -0.0044(11) 0.0155(11) 0.0047(11) N11 0.0194(11) 0.0259(12) 0.0151(10) -0.0028(9) 0.0042(9) 0.0003(9) N12 0.0162(10) 0.0218(11) 0.0103(9) -0.0026(8) 0.0009(8) 0.0006(8) C13 0.0209(14) 0.0353(18) 0.0352(18) -0.0076(15) 0.0029(13) 0.0068(13) C14 0.0426(19) 0.0315(16) 0.0106(12) -0.0034(11) 0.0031(12) 0.0017(14) C15 0.0191(14) 0.0389(18) 0.0300(17) 0.0064(14) 0.0027(12) 0.0100(13) C16 0.0342(17) 0.0321(16) 0.0155(13) -0.0089(12) 0.0033(12) -0.0019(13) O1W 0.0495(19) 0.0467(17) 0.0392(16) -0.0052(13) 0.0080(14) 0.0171(15) Cl 0.0241(4) 0.0304(4) 0.0401(5) 0.0071(3) 0.0024(3) -0.0017(3) O2 0.068(3) 0.074(3) 0.134(5) -0.050(3) 0.001(3) 0.026(2) O3 0.0460(18) 0.063(2) 0.0279(14) 0.0161(14) 0.0024(13) 0.0025(15) O4 0.0398(17) 0.069(2) 0.0289(14) 0.0051(14) -0.0003(12) -0.0082(15) O5 0.049(2) 0.085(3) 0.123(4) 0.052(3) 0.041(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag N1 2.269(2) . ? Ag N8 2.284(2) 4_666 ? Ag N5 2.303(2) 4_666 ? Ag N12 2.334(2) . ? N1 C6 1.329(3) . ? N1 C2 1.351(4) . ? C2 C3 1.384(4) . ? C2 C13 1.493(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 N5 1.345(4) . ? C4 C14 1.486(4) . ? N5 C6 1.332(3) . ? N5 Ag 2.303(2) 4_565 ? C6 C7 1.495(4) . ? C7 N12 1.323(3) . ? C7 N8 1.328(3) . ? N8 N9 1.353(4) . ? N8 Ag 2.284(2) 4_565 ? N9 C10 1.383(4) . ? N9 C15 1.461(4) . ? C10 O10 1.215(4) . ? C10 N11 1.380(4) . ? N11 N12 1.357(3) . ? N11 C16 1.466(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Cl O2 1.402(4) . ? Cl O3 1.417(3) . ? Cl O4 1.433(3) . ? Cl O5 1.449(4) . ? 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 Ag N8 142.32(9) . 4_666 ? N1 Ag N5 124.94(9) . 4_666 ? N8 Ag N5 72.06(9) 4_666 4_666 ? N1 Ag N12 71.57(8) . . ? N8 Ag N12 131.06(9) 4_666 . ? N5 Ag N12 123.59(9) 4_666 . ? C6 N1 C2 117.4(2) . . ? C6 N1 Ag 118.09(19) . . ? C2 N1 Ag 124.20(19) . . ? N1 C2 C3 120.4(3) . . ? N1 C2 C13 116.5(3) . . ? C3 C2 C13 123.1(3) . . ? C2 C3 C4 118.5(3) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? N5 C4 C3 120.4(3) . . ? N5 C4 C14 117.1(3) . . ? C3 C4 C14 122.5(3) . . ? C6 N5 C4 117.4(2) . . ? C6 N5 Ag 116.26(19) . 4_565 ? C4 N5 Ag 126.32(18) . 4_565 ? N1 C6 N5 125.8(3) . . ? N1 C6 C7 117.3(2) . . ? N5 C6 C7 116.9(2) . . ? N12 C7 N8 126.7(3) . . ? N12 C7 C6 116.3(2) . . ? N8 C7 C6 116.9(2) . . ? C7 N8 N9 115.5(2) . . ? C7 N8 Ag 117.11(19) . 4_565 ? N9 N8 Ag 127.42(18) . 4_565 ? N8 N9 C10 123.7(2) . . ? N8 N9 C15 115.8(3) . . ? C10 N9 C15 120.4(3) . . ? O10 C10 N11 123.5(3) . . ? O10 C10 N9 121.7(3) . . ? N11 C10 N9 114.9(3) . . ? N12 N11 C10 123.1(2) . . ? N12 N11 C16 115.5(2) . . ? C10 N11 C16 121.4(3) . . ? C7 N12 N11 116.1(2) . . ? C7 N12 Ag 116.65(18) . . ? N11 N12 Ag 127.19(17) . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C4 C14 H14A 109.5 . . ? C4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N9 C15 H15A 109.5 . . ? N9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N11 C16 H16A 109.5 . . ? N11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 Cl O3 112.4(3) . . ? O2 Cl O4 109.2(3) . . ? O3 Cl O4 109.8(2) . . ? O2 Cl O5 110.8(4) . . ? O3 Cl O5 107.4(2) . . ? O4 Cl O5 107.1(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 35.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.893 _refine_diff_density_min -1.396 _refine_diff_density_rms 0.149 #===END # Attachment 'B701686G_CCDC635223.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 635223' _audit_creation_date 07-01-25 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title '12021155 Compound X' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 12.2251(7) _cell_length_b 15.406(9) _cell_length_c 19.7291(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3716(2) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ag -0.8971 1.1015 19.2808 0.6446 16.6885 7.4726 4.8045 24.6605 1.0463 99.8156 5.1790 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 8 # Given Formula = C12 H19 Ag1 Cl1 N7 O5 # Dc = 1.73 Fooo = 1936.00 Mu = 12.68 M = 484.65 # Found Formula = C12 H17 Ag1 Cl1 N7 O5 # Dc = 1.73 FOOO = 1936.00 Mu = 12.67 M = 482.63 _chemical_formula_sum 'C12 H19 Ag Cl N7 O5' _chemical_formula_moiety 'C10 H16 Ag N6 O, C2 H3 N, Cl O4' _chemical_compound_source ? _chemical_formula_weight 484.65 _cell_measurement_reflns_used 115 _cell_measurement_theta_min 4 _cell_measurement_theta_max 19 _cell_measurement_temperature 250 _exptl_crystal_description parallelepiped _exptl_crystal_colour yellow _exptl_crystal_size_min 0.08 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.18 _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1952 _exptl_absorpt_coefficient_mu 1.268 # Sheldrick geometric approximatio 0.86 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.90 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_data_reduction 'EvalCCD (Duisenberg & Schreurs 1990-2000)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 250 _diffrn_reflns_number 14966 _reflns_number_total 4268 _diffrn_reflns_av_R_equivalents 0.050 # Number of reflections with Friedels Law is 1904 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 4271 _diffrn_reflns_theta_min 2.064 _diffrn_reflns_theta_max 27.508 _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.032 _diffrn_measured_fraction_theta_full 0.955 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min 0 _reflns_limit_h_max 15 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.52 _refine_diff_density_max 1.52 _refine_ls_number_reflns 1940 _refine_ls_number_restraints 3 _refine_ls_number_parameters 174 #_refine_ls_R_factor_ref 0.1142 _refine_ls_wR_factor_ref 0.1095 _refine_ls_goodness_of_fit_ref 1.0707 #_reflns_number_all 4158 _refine_ls_R_factor_all 0.1999 _refine_ls_wR_factor_all 0.1415 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.0\s(I) _reflns_number_gt 1940 _refine_ls_R_factor_gt 0.1142 _refine_ls_wR_factor_gt 0.1095 _refine_ls_shift/su_max 0.000128 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment refu # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.84 0.228 2.99 ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ag1 Ag -0.29475(8) 0.22397(7) 0.27030(5) 0.0464 1.0000 Uani . . . . . . N1 N 0.0477(8) 0.3098(7) 0.2017(5) 0.0355 1.0000 Uani . . . . . . N2 N 0.0613(7) 0.1918(6) 0.3010(5) 0.0300 1.0000 Uani . . . . . . N3 N -0.1269(9) 0.1936(6) 0.3147(5) 0.0333 1.0000 Uani . . . . . . N4 N -0.1494(9) 0.3112(6) 0.2132(4) 0.0333 1.0000 Uani . . . . . . N5 N -0.1561(9) 0.3534(8) 0.1492(5) 0.0448 1.0000 Uani . . . . . . N6 N 0.0319(8) 0.3518(7) 0.1380(5) 0.0426 1.0000 Uani D . . . . . O1 O -0.0743(9) 0.4233(6) 0.0614(5) 0.0508 1.0000 Uani . . . . . . C1 C -0.0648(10) 0.3806(7) 0.1134(5) 0.0300 1.0000 Uani . . . . . . C2 C 0.1365(11) 0.3835(10) 0.1063(8) 0.0616 1.0000 Uani D . . . . . C3 C -0.2659(12) 0.3807(11) 0.1324(7) 0.0589 1.0000 Uani . . . . . . C4 C -0.0507(9) 0.2581(7) 0.2160(5) 0.0222 1.0000 Uani . . . . . . C5 C -0.0375(9) 0.2109(7) 0.2822(5) 0.0276 1.0000 Uani . . . . . . C6 C -0.0166(11) 0.1228(8) 0.3966(6) 0.0390 1.0000 Uani . . . . . . C7 C 0.0727(10) 0.1427(8) 0.3591(6) 0.0355 1.0000 Uani . . . . . . C8 C -0.1178(11) 0.1463(7) 0.3736(6) 0.0363 1.0000 Uani . . . . . . C9 C 0.1870(11) 0.1214(11) 0.3796(9) 0.0599 1.0000 Uani . . . . . . C10 C -0.2204(13) 0.1262(12) 0.4115(8) 0.0650 1.0000 Uani . . . . . . Cl1 Cl 0.0364(3) 0.0010(2) 0.19529(19) 0.0526(9) 1.0000 Uiso . . . . . . N7 N 0.111(3) 0.232(3) -0.005(3) 0.27(2) 1.0000 Uiso D . . . . . O2 O -0.0454(15) 0.0050(12) 0.2451(9) 0.108(5) 1.0000 Uiso . . . . . . O3 O 0.1390(16) 0.0100(13) 0.2233(9) 0.118(6) 1.0000 Uiso . . . . . . O4 O 0.0187(12) 0.0694(10) 0.1504(7) 0.087(4) 1.0000 Uiso . . . . . . O5 O 0.0324(10) -0.0839(8) 0.1653(6) 0.069(3) 1.0000 Uiso . . . . . . C11 C 0.025(3) 0.202(2) -0.0028(19) 0.139(11) 1.0000 Uiso D . . . . . C12 C -0.091(3) 0.168(3) 0.004(2) 0.169(13) 1.0000 Uiso D . . . . . H11 H 0.0462 0.3578 0.2360 0.17(3) 1.0000 Uiso . . . . . . H42 H -0.1362 0.3534 0.2417 0.17(3) 1.0000 Uiso . . . . . . H21 H 0.1197 0.4117 0.0618 0.17(3) 1.0000 Uiso . . . . . . H22 H 0.1727 0.4260 0.1369 0.17(3) 1.0000 Uiso . . . . . . H23 H 0.1865 0.3328 0.0984 0.17(3) 1.0000 Uiso . . . . . . H31 H -0.2658 0.4097 0.0870 0.17(3) 1.0000 Uiso . . . . . . H32 H -0.2928 0.4225 0.1674 0.17(3) 1.0000 Uiso . . . . . . H33 H -0.3152 0.3290 0.1310 0.17(3) 1.0000 Uiso . . . . . . H41 H -0.0568 0.2135 0.1794 0.17(3) 1.0000 Uiso . . . . . . H61 H -0.0085 0.0911 0.4406 0.17(3) 1.0000 Uiso . . . . . . H91 H 0.1859 0.0856 0.4219 0.17(3) 1.0000 Uiso . . . . . . H92 H 0.2287 0.1760 0.3877 0.17(3) 1.0000 Uiso . . . . . . H93 H 0.2231 0.0874 0.3424 0.17(3) 1.0000 Uiso . . . . . . H101 H -0.2020 0.0916 0.4529 0.17(3) 1.0000 Uiso . . . . . . H102 H -0.2568 0.1815 0.4251 0.17(3) 1.0000 Uiso . . . . . . H103 H -0.2706 0.0918 0.3819 0.17(3) 1.0000 Uiso . . . . . . H121 H -0.1036 0.1214 -0.0299 0.17(3) 1.0000 Uiso . . . . . . H122 H -0.1438 0.2160 -0.0020 0.17(3) 1.0000 Uiso . . . . . . H123 H -0.1001 0.1426 0.0512 0.17(3) 1.0000 Uiso . . . . . . 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 0.0385(5) 0.0502(6) 0.0505(6) 0.0074(5) -0.0051(5) 0.0012(5) N1 0.0355(12) 0.0355(12) 0.0355(12) 0.0016(12) 0.0016(12) 0.0016(12) N2 0.0300(11) 0.0300(11) 0.0300(11) 0.0000(11) 0.0000(11) 0.0000(11) N3 0.057(6) 0.019(5) 0.024(5) -0.002(4) 0.003(4) -0.001(4) N4 0.056(6) 0.028(5) 0.015(5) 0.002(3) -0.011(4) 0.003(5) N5 0.057(6) 0.059(7) 0.018(5) 0.020(5) -0.003(4) -0.008(6) N6 0.056(7) 0.047(6) 0.025(5) 0.013(5) 0.013(5) -0.004(5) O1 0.077(7) 0.040(5) 0.035(5) 0.011(4) 0.000(4) -0.005(5) C1 0.051(7) 0.021(6) 0.019(5) 0.010(4) -0.003(5) -0.005(5) C2 0.067(10) 0.063(10) 0.055(9) 0.025(8) 0.028(8) -0.001(8) C3 0.055(9) 0.069(10) 0.053(9) 0.041(8) -0.017(7) 0.022(7) C4 0.0222(12) 0.0222(12) 0.0222(12) 0.0016(12) 0.0016(12) 0.0016(12) C5 0.0276(11) 0.0276(11) 0.0276(11) 0.0000(11) 0.0000(11) 0.0000(11) C6 0.066(9) 0.027(6) 0.024(6) 0.008(5) -0.018(6) -0.001(6) C7 0.054(7) 0.029(6) 0.023(6) 0.005(5) -0.010(5) -0.001(5) C8 0.053(7) 0.027(6) 0.029(6) 0.012(5) 0.004(6) -0.001(5) C9 0.044(9) 0.058(9) 0.077(11) 0.021(8) -0.024(7) -0.001(7) C10 0.065(10) 0.083(12) 0.047(8) 0.040(8) 0.006(7) 0.000(8) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2473(14) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ag1 . N1 8_455 2.400(10) yes Ag1 . N2 8_455 2.307(9) yes Ag1 . N3 . 2.279(11) yes Ag1 . N4 . 2.496(10) yes N1 . N6 . 1.427(14) yes N1 . C4 . 1.470(15) yes N1 . H11 . 1.002 no N2 . C5 . 1.297(14) yes N2 . C7 . 1.380(15) yes N3 . C5 . 1.294(14) yes N3 . C8 . 1.376(14) yes N4 . N5 . 1.422(13) yes N4 . C4 . 1.458(14) yes N4 . H42 . 0.875 no N5 . C1 . 1.386(15) yes N5 . C3 . 1.445(18) yes N6 . C1 . 1.353(15) yes N6 . C2 . 1.505(9) yes O1 . C1 . 1.223(14) yes C2 . H21 . 1.002 no C2 . H22 . 0.995 no C2 . H23 . 1.003 no C3 . H31 . 1.001 no C3 . H32 . 1.001 no C3 . H33 . 0.999 no C4 . C5 . 1.505(14) yes C4 . H41 . 0.999 no C6 . C7 . 1.354(18) yes C6 . C8 . 1.367(18) yes C6 . H61 . 1.000 no C7 . C9 . 1.492(18) yes C8 . C10 . 1.494(19) yes C9 . H91 . 0.999 no C9 . H92 . 0.996 no C9 . H93 . 1.005 no C10 . H101 . 1.000 no C10 . H102 . 0.998 no C10 . H103 . 0.999 no Cl1 . O2 . 1.404(18) yes Cl1 . O3 . 1.38(2) yes Cl1 . O4 . 1.393(15) yes Cl1 . O5 . 1.437(12) yes N7 . C11 . 1.150(10) yes C11 . C12 . 1.517(10) yes C12 . H121 . 0.992 no C12 . H122 . 0.989 no C12 . H123 . 1.014 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 8_455 Ag1 . N2 8_455 69.3(3) yes N1 8_455 Ag1 . N3 . 138.3(3) yes N2 8_455 Ag1 . N3 . 151.3(3) yes N1 8_455 Ag1 . N4 . 112.2(3) yes N2 8_455 Ag1 . N4 . 112.5(3) yes N3 . Ag1 . N4 . 69.1(3) yes Ag1 8_555 N1 . N6 . 124.1(7) yes Ag1 8_555 N1 . C4 . 108.3(7) yes N6 . N1 . C4 . 107.6(9) yes Ag1 8_555 N1 . H11 . 105.5 no N6 . N1 . H11 . 104.9 no C4 . N1 . H11 . 104.8 no Ag1 8_555 N2 . C5 . 119.1(7) yes Ag1 8_555 N2 . C7 . 123.2(8) yes C5 . N2 . C7 . 117.1(10) yes Ag1 . N3 . C5 . 121.9(7) yes Ag1 . N3 . C8 . 120.4(8) yes C5 . N3 . C8 . 117.3(10) yes Ag1 . N4 . N5 . 127.3(7) yes Ag1 . N4 . C4 . 105.7(6) yes N5 . N4 . C4 . 109.7(9) yes Ag1 . N4 . H42 . 103.9 no N5 . N4 . H42 . 103.9 no C4 . N4 . H42 . 103.9 no N4 . N5 . C1 . 123.0(10) yes N4 . N5 . C3 . 113.0(10) yes C1 . N5 . C3 . 122.9(10) yes N1 . N6 . C1 . 125.7(9) yes N1 . N6 . C2 . 113.4(10) yes C1 . N6 . C2 . 119.1(10) yes N5 . C1 . N6 . 114.9(9) yes N5 . C1 . O1 . 120.9(11) yes N6 . C1 . O1 . 124.1(11) yes N6 . C2 . H21 . 109.3 no N6 . C2 . H22 . 109.8 no H21 . C2 . H22 . 109.7 no N6 . C2 . H23 . 109.3 no H21 . C2 . H23 . 109.1 no H22 . C2 . H23 . 109.6 no N5 . C3 . H31 . 109.5 no N5 . C3 . H32 . 109.5 no H31 . C3 . H32 . 109.3 no N5 . C3 . H33 . 109.6 no H31 . C3 . H33 . 109.5 no H32 . C3 . H33 . 109.5 no N1 . C4 . N4 . 111.5(8) yes N1 . C4 . C5 . 109.9(9) yes N4 . C4 . C5 . 113.1(8) yes N1 . C4 . H41 . 107.2 no N4 . C4 . H41 . 107.3 no C5 . C4 . H41 . 107.6 no C4 . C5 . N2 . 117.3(9) yes C4 . C5 . N3 . 116.0(9) yes N2 . C5 . N3 . 126.7(10) yes C7 . C6 . C8 . 119.2(10) yes C7 . C6 . H61 . 120.3 no C8 . C6 . H61 . 120.5 no N2 . C7 . C6 . 119.7(11) yes N2 . C7 . C9 . 116.2(11) yes C6 . C7 . C9 . 123.8(11) yes N3 . C8 . C6 . 119.6(11) yes N3 . C8 . C10 . 117.7(11) yes C6 . C8 . C10 . 122.6(11) yes C7 . C9 . H91 . 109.6 no C7 . C9 . H92 . 109.7 no H91 . C9 . H92 . 109.9 no C7 . C9 . H93 . 109.1 no H91 . C9 . H93 . 109.2 no H92 . C9 . H93 . 109.4 no C8 . C10 . H101 . 109.3 no C8 . C10 . H102 . 109.4 no H101 . C10 . H102 . 109.6 no C8 . C10 . H103 . 109.4 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.7 no O2 . Cl1 . O3 . 111.3(11) yes O2 . Cl1 . O4 . 107.6(10) yes O3 . Cl1 . O4 . 108.7(10) yes O2 . Cl1 . O5 . 107.7(9) yes O3 . Cl1 . O5 . 106.7(10) yes O4 . Cl1 . O5 . 114.9(8) yes N7 . C11 . C12 . 176(5) yes C11 . C12 . H121 . 109.5 no C11 . C12 . H122 . 109.5 no H121 . C12 . H122 . 111.1 no C11 . C12 . H123 . 108.4 no H121 . C12 . H123 . 109.0 no H122 . C12 . H123 . 109.2 no