Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full CrystEngComm #========================================================================== # 1. Submission Details _journal_coden_Cambridge 1350 #============================================================================== _audit_creation_date ? _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _publ_contact_author_name 'Ulli Englert' _publ_contact_author_address ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; _publ_contact_author_email ullrich.englert@ac.rwth-aachen.de _publ_contact_author_fax 0049-241-8092288 _publ_contact_author_phone 0049-241-8094666 #========================================================================== # 3. Title and Author List # 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 #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' #<--'Last name, first name' I.Kalf ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; M.Braun ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; 'Y. Wang' ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; U.Englert ; Institut fuer Anorganische Chemie RWTH Aachen Landoltweg 1 52074 Aachen Germany ; #========================================================================== # 4. Text _publ_section_title ; Homo- and heterochiral coordination polymers of silver with diaminocyclohexane as bridging ligand: The effect of chirality on argentophilic interactions ; _publ_section_references ; Bruker (1999). SAINT+. Version 6.02. Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Bruker AXS Inc., Madison, Wisconson, USA. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXS-97. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G. M. (1998). SHELXTL. Version 5.1. Bruker AXS Inc., Madison, Wisconson, USA. Spek, A. L. (1990). Acta Cryst. A46, C-34. ; _publ_section_acknowledgements ; Support from the DFG is gratefully acknowledged. ; #========================================================================== data_1 _database_code_depnum_ccdc_archive 'CCDC 618006' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Ag(SS-chxn))COO\\times0.5 H2O' _chemical_melting_point ? _chemical_formula_moiety '2(C8 H17 Ag N2 O2), H2 O' _chemical_formula_sum 'C16 H36 Ag2 N4 O5' _chemical_formula_weight 580.23 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C2 ' 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' _cell_length_a 19.8677(14) _cell_length_b 5.2047(4) _cell_length_c 13.8276(10) _cell_angle_alpha 90.00 _cell_angle_beta 128.451(2) _cell_angle_gamma 90.00 _cell_volume 1119.77(14) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 5407 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 29.00 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.780 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.51 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7583 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0303 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 29.03 _reflns_number_total 2857 _reflns_number_gt 2783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _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^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _chemical_absolute_configuration rmad _refine_ls_number_reflns 2857 _refine_ls_number_parameters 124 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0262 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.332115(9) 0.82522(6) 0.419778(13) 0.02217(7) Uani 1 1 d . . . O1 O 0.37806(11) 1.0960(4) 0.59806(17) 0.0240(4) Uani 1 1 d . . . O2 O 0.50600(13) 0.9610(4) 0.6622(2) 0.0284(4) Uani 1 1 d . . . N1 N 0.26242(13) 0.4751(4) 0.39277(18) 0.0183(4) Uani 1 1 d . . . H1A H 0.2993 0.3653 0.4573 0.022 Uiso 1 1 calc R . . H1B H 0.2190 0.5160 0.3964 0.022 Uiso 1 1 calc R . . N2 N 0.36571(13) 0.1594(5) 0.3575(2) 0.0199(4) Uani 1 1 d . . . H2A H 0.4001 0.2692 0.4232 0.024 Uiso 1 1 calc R . . H2B H 0.3971 0.1023 0.3335 0.024 Uiso 1 1 calc R . . C1 C 0.22459(13) 0.3372(8) 0.27594(19) 0.0174(4) Uani 1 1 d . . . H1 H 0.2067 0.1626 0.2825 0.021 Uiso 1 1 calc R . . C2 C 0.29064(14) 0.3035(8) 0.25453(19) 0.0181(5) Uani 1 1 d . . . H2 H 0.3105 0.4777 0.2514 0.022 Uiso 1 1 calc R . . C3 C 0.25173(18) 0.1686(6) 0.1327(3) 0.0274(6) Uani 1 1 d . . . H3A H 0.2950 0.1595 0.1190 0.033 Uiso 1 1 calc R . . H3B H 0.2360 -0.0093 0.1367 0.033 Uiso 1 1 calc R . . C4 C 0.17264(16) 0.3082(12) 0.0255(2) 0.0330(6) Uani 1 1 d . . . H4A H 0.1469 0.2097 -0.0514 0.040 Uiso 1 1 calc R . . H4B H 0.1896 0.4790 0.0156 0.040 Uiso 1 1 calc R . . C5 C 0.10619(15) 0.3420(11) 0.0457(2) 0.0312(6) Uani 1 1 d . . . H5A H 0.0839 0.1716 0.0453 0.037 Uiso 1 1 calc R . . H5B H 0.0574 0.4446 -0.0228 0.037 Uiso 1 1 calc R . . C6 C 0.14502(16) 0.4766(6) 0.1683(2) 0.0246(5) Uani 1 1 d . . . H6A H 0.1605 0.6550 0.1645 0.030 Uiso 1 1 calc R . . H6B H 0.1017 0.4842 0.1819 0.030 Uiso 1 1 calc R . . C7 C 0.45890(16) 1.1098(5) 0.6677(2) 0.0200(5) Uani 1 1 d . . . C8 C 0.50002(18) 1.3312(17) 0.7594(3) 0.0311(6) Uani 1 1 d . . . H8A H 0.5599 1.2886 0.8278 0.047 Uiso 1 1 calc R . . H8B H 0.4685 1.3607 0.7915 0.047 Uiso 1 1 calc R . . H8C H 0.4981 1.4870 0.7179 0.047 Uiso 1 1 calc R . . O3 O 0.0000 0.1106(6) 0.5000 0.0321(6) Uani 1 2 d S . . H3O H 0.0026 0.1918 0.5486 0.039 Uiso 1 1 d 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 0.01972(10) 0.01720(10) 0.02958(10) -0.00150(14) 0.01533(8) -0.00007(13) O1 0.0191(8) 0.0319(11) 0.0228(9) -0.0022(8) 0.0139(7) -0.0047(8) O2 0.0267(10) 0.0275(11) 0.0387(11) -0.0009(9) 0.0242(9) -0.0014(9) N1 0.0166(9) 0.0219(11) 0.0204(9) -0.0010(8) 0.0134(8) 0.0024(8) N2 0.0154(9) 0.0215(11) 0.0249(10) -0.0034(8) 0.0136(9) 0.0005(8) C1 0.0153(8) 0.0189(11) 0.0195(8) -0.0010(14) 0.0116(7) -0.0024(15) C2 0.0183(9) 0.0186(13) 0.0219(9) -0.0026(12) 0.0147(8) -0.0012(12) C3 0.0258(13) 0.0365(16) 0.0256(13) -0.0086(11) 0.0188(12) -0.0044(12) C4 0.0301(12) 0.0505(19) 0.0210(10) -0.0061(19) 0.0173(9) -0.008(2) C5 0.0185(10) 0.0453(19) 0.0216(10) 0.0026(18) 0.0084(9) -0.0002(19) C6 0.0180(11) 0.0289(15) 0.0254(12) 0.0036(11) 0.0127(10) 0.0035(10) C7 0.0227(12) 0.0182(12) 0.0237(12) 0.0008(9) 0.0166(10) -0.0033(9) C8 0.0310(12) 0.0298(13) 0.0284(11) -0.014(2) 0.0164(10) -0.009(2) O3 0.0264(14) 0.0235(15) 0.0347(15) 0.000 0.0132(12) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.176(2) . ? Ag1 N2 2.220(2) 1_565 ? Ag1 O1 2.4694(19) . ? O1 C7 1.260(3) . ? O2 C7 1.252(3) . ? N1 C1 1.476(3) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.474(3) . ? N2 Ag1 2.220(2) 1_545 ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C1 C6 1.521(4) . ? C1 C2 1.524(3) . ? C1 H1 1.0000 . ? C2 C3 1.519(4) . ? C2 H2 1.0000 . ? C3 C4 1.516(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.520(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.527(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.522(7) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O3 H3O 0.7679 . ? 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 Ag1 N2 154.49(8) . 1_565 ? N1 Ag1 O1 116.75(7) . . ? N2 Ag1 O1 85.77(8) 1_565 . ? C7 O1 Ag1 107.41(16) . . ? C1 N1 Ag1 115.57(17) . . ? C1 N1 H1A 108.4 . . ? Ag1 N1 H1A 108.4 . . ? C1 N1 H1B 108.4 . . ? Ag1 N1 H1B 108.4 . . ? H1A N1 H1B 107.4 . . ? C2 N2 Ag1 113.93(17) . 1_545 ? C2 N2 H2A 108.8 . . ? Ag1 N2 H2A 108.8 1_545 . ? C2 N2 H2B 108.8 . . ? Ag1 N2 H2B 108.8 1_545 . ? H2A N2 H2B 107.7 . . ? N1 C1 C6 110.5(3) . . ? N1 C1 C2 110.76(19) . . ? C6 C1 C2 111.2(2) . . ? N1 C1 H1 108.1 . . ? C6 C1 H1 108.1 . . ? C2 C1 H1 108.1 . . ? N2 C2 C3 110.3(3) . . ? N2 C2 C1 110.3(2) . . ? C3 C2 C1 111.3(2) . . ? N2 C2 H2 108.3 . . ? C3 C2 H2 108.3 . . ? C1 C2 H2 108.3 . . ? C4 C3 C2 111.5(3) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 111.5(3) . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 111.1(2) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C1 C6 C5 111.6(3) . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6B 109.3 . . ? C5 C6 H6B 109.3 . . ? H6A C6 H6B 108.0 . . ? O2 C7 O1 124.3(2) . . ? O2 C7 C8 119.0(2) . . ? O1 C7 C8 116.6(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? _diffrn_measured_fraction_theta_max .975 _diffrn_reflns_theta_full 29.03 _diffrn_measured_fraction_theta_full .975 _refine_diff_density_max .947 _refine_diff_density_min -.295 _refine_diff_density_rms .094 # Attachment '2.cif' #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 618007' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Ag(rac-chxn))COO\\times2 H2O' _chemical_melting_point ? _chemical_formula_moiety 'C6 H16 Ag N2 O, C2 H3 O2, H2 O' _chemical_formula_sum 'C8 H21 Ag N2 O4' _chemical_formula_weight 317.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.394(4) _cell_length_b 10.851(4) _cell_length_c 11.268(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.477(6) _cell_angle_gamma 90.00 _cell_volume 1218.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 924 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 28.30 _exptl_crystal_description 'triangular plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 1.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.88 _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11290 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0253 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 30.95 _reflns_number_total 3030 _reflns_number_gt 2739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _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^)+(0.0420P)^2^+1.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3030 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0737 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Ag Ag 0.389886(17) 0.132148(16) 0.174320(17) 0.01904(8) Uani 1 1 d . . . N1 N 0.3731(2) 0.11257(18) 0.3780(2) 0.0185(4) Uani 1 1 d . . . H1A H 0.3691 0.0299 0.3947 0.022 Uiso 1 1 calc R . . H1B H 0.4510 0.1427 0.4312 0.022 Uiso 1 1 calc R . . N2 N 0.3653(2) 0.37431(17) 0.4596(2) 0.0175(4) Uani 1 1 d . . . H2A H 0.3569 0.4559 0.4366 0.021 Uiso 1 1 calc R . . H2B H 0.4449 0.3471 0.4484 0.021 Uiso 1 1 calc R . . C1 C 0.2645(2) 0.1710(2) 0.4058(2) 0.0163(4) Uani 1 1 d . . . H1 H 0.2694 0.1600 0.4951 0.020 Uiso 1 1 calc R . . C2 C 0.2581(2) 0.3079(2) 0.3715(2) 0.0149(4) Uani 1 1 d . . . H2 H 0.2638 0.3194 0.2851 0.018 Uiso 1 1 calc R . . C3 C 0.1395(2) 0.3651(2) 0.3875(3) 0.0209(5) Uani 1 1 d . . . H3A H 0.1364 0.4534 0.3646 0.025 Uiso 1 1 calc R . . H3B H 0.1377 0.3584 0.4746 0.025 Uiso 1 1 calc R . . C4 C 0.0244(2) 0.2976(3) 0.3041(3) 0.0254(5) Uani 1 1 d . . . H4A H 0.0283 0.3037 0.2175 0.030 Uiso 1 1 calc R . . H4B H -0.0611 0.3346 0.3088 0.030 Uiso 1 1 calc R . . C5 C 0.0306(3) 0.1623(3) 0.3432(3) 0.0263(6) Uani 1 1 d . . . H5A H 0.0328 0.1569 0.4315 0.032 Uiso 1 1 calc R . . H5B H -0.0508 0.1190 0.2937 0.032 Uiso 1 1 calc R . . C6 C 0.1482(3) 0.1031(2) 0.3255(3) 0.0229(5) Uani 1 1 d . . . H6A H 0.1480 0.1082 0.2377 0.028 Uiso 1 1 calc R . . H6B H 0.1513 0.0153 0.3498 0.028 Uiso 1 1 calc R . . O1 O 0.6609(2) 0.13701(16) 0.1138(2) 0.0260(4) Uani 1 1 d . . . O2 O 0.64126(17) 0.33274(16) 0.05117(17) 0.0209(4) Uani 1 1 d . . . C7 C 0.6888(2) 0.2267(2) 0.0532(2) 0.0173(4) Uani 1 1 d . . . C8 C 0.7831(3) 0.2072(3) -0.0227(3) 0.0261(5) Uani 1 1 d . . . H8A H 0.8573 0.1544 0.0226 0.039 Uiso 1 1 calc R . . H8B H 0.8187 0.2869 -0.0396 0.039 Uiso 1 1 calc R . . H8C H 0.7356 0.1676 -0.1010 0.039 Uiso 1 1 calc R . . O3 O 0.3402(2) 0.52086(18) 0.1578(2) 0.0285(4) Uani 1 1 d . . . O4 O 0.5142(2) 0.3408(2) 0.2508(2) 0.0238(4) Uani 1 1 d . . . H3C H 0.342(4) 0.556(3) 0.099(3) 0.032(10) Uiso 1 1 d . . . H4C H 0.548(4) 0.329(4) 0.194(4) 0.040(10) Uiso 1 1 d . . . H4D H 0.478(4) 0.394(3) 0.229(3) 0.031(11) Uiso 1 1 d . . . H3D H 0.334(4) 0.560(3) 0.223(3) 0.036(9) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag 0.01695(10) 0.01838(11) 0.02181(13) 0.00003(6) 0.00554(8) 0.00324(6) N1 0.0157(9) 0.0139(9) 0.0257(11) -0.0006(8) 0.0056(8) 0.0033(7) N2 0.0132(9) 0.0140(9) 0.0266(12) -0.0001(7) 0.0080(8) -0.0008(7) C1 0.0156(10) 0.0129(10) 0.0211(12) 0.0009(9) 0.0063(9) 0.0004(8) C2 0.0141(10) 0.0136(10) 0.0183(11) 0.0014(8) 0.0065(8) 0.0009(8) C3 0.0159(11) 0.0178(11) 0.0300(14) 0.0000(9) 0.0079(10) 0.0023(8) C4 0.0133(10) 0.0295(13) 0.0320(15) 0.0016(11) 0.0040(10) 0.0019(9) C5 0.0149(11) 0.0287(13) 0.0351(15) -0.0028(11) 0.0070(10) -0.0051(10) C6 0.0177(11) 0.0208(11) 0.0301(14) -0.0050(10) 0.0064(10) -0.0037(9) O1 0.0342(11) 0.0150(8) 0.0329(11) 0.0037(7) 0.0162(9) -0.0007(7) O2 0.0192(8) 0.0167(8) 0.0295(10) 0.0011(7) 0.0113(7) 0.0014(6) C7 0.0163(10) 0.0164(10) 0.0190(12) -0.0002(9) 0.0048(8) -0.0007(8) C8 0.0188(11) 0.0281(13) 0.0334(15) 0.0040(11) 0.0107(10) 0.0053(10) O3 0.0439(12) 0.0194(9) 0.0279(11) 0.0037(9) 0.0194(9) 0.0070(8) O4 0.0170(8) 0.0261(10) 0.0309(11) 0.0028(9) 0.0113(8) 0.0003(8) _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 2.360(2) . ? Ag N2 2.361(2) 4_565 ? N1 C1 1.406(3) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.456(3) . ? N2 Ag 2.361(2) 4_566 ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C1 C6 1.484(3) . ? C1 C2 1.532(3) . ? C1 H1 1.0000 . ? C2 C3 1.437(3) . ? C2 H2 1.0000 . ? C3 C4 1.488(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.529(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.443(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? O1 C7 1.269(3) . ? O2 C7 1.250(3) . ? C7 C8 1.488(3) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O3 H3C 0.77(4) . ? O3 H3D 0.86(4) . ? O4 H4C 0.82(4) . ? O4 H4D 0.69(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 N2 167.85(7) . 4_565 ? C1 N1 Ag 117.52(15) . . ? C1 N1 H1A 107.9 . . ? Ag N1 H1A 107.9 . . ? C1 N1 H1B 107.9 . . ? Ag N1 H1B 107.9 . . ? H1A N1 H1B 107.2 . . ? C2 N2 Ag 121.57(15) . 4_566 ? C2 N2 H2A 106.9 . . ? Ag N2 H2A 106.9 4_566 . ? C2 N2 H2B 106.9 . . ? Ag N2 H2B 106.9 4_566 . ? H2A N2 H2B 106.7 . . ? N1 C1 C6 101.9(2) . . ? N1 C1 C2 111.15(19) . . ? C6 C1 C2 111.0(2) . . ? N1 C1 H1 110.8 . . ? C6 C1 H1 110.8 . . ? C2 C1 H1 110.8 . . ? C3 C2 N2 102.62(19) . . ? C3 C2 C1 111.4(2) . . ? N2 C2 C1 109.77(19) . . ? C3 C2 H2 110.9 . . ? N2 C2 H2 110.9 . . ? C1 C2 H2 110.9 . . ? C2 C3 C4 105.8(2) . . ? C2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? C2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? C3 C4 C5 109.3(2) . . ? C3 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? C3 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C6 C5 C4 110.8(2) . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C1 105.6(2) . . ? C5 C6 H6A 110.6 . . ? C1 C6 H6A 110.6 . . ? C5 C6 H6B 110.6 . . ? C1 C6 H6B 110.6 . . ? H6A C6 H6B 108.7 . . ? O2 C7 O1 124.5(2) . . ? O2 C7 C8 116.2(2) . . ? O1 C7 C8 119.3(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? H3C O3 H3D 121(4) . . ? H4C O4 H4D 100(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 N2 Ag N1 C1 -68.1(4) 4_565 . . . ? Ag N1 C1 C6 64.6(2) . . . . ? Ag N1 C1 C2 -53.7(2) . . . . ? Ag N2 C2 C3 62.6(2) 4_566 . . . ? Ag N2 C2 C1 -55.9(2) 4_566 . . . ? N1 C1 C2 C3 173.9(2) . . . . ? C6 C1 C2 C3 61.2(3) . . . . ? N1 C1 C2 N2 -73.2(3) . . . . ? C6 C1 C2 N2 174.2(2) . . . . ? N2 C2 C3 C4 -177.3(2) . . . . ? C1 C2 C3 C4 -60.0(3) . . . . ? C2 C3 C4 C5 61.3(3) . . . . ? C3 C4 C5 C6 -65.1(3) . . . . ? C4 C5 C6 C1 61.0(3) . . . . ? N1 C1 C6 C5 -176.9(2) . . . . ? C2 C1 C6 C5 -58.4(3) . . . . ? _diffrn_measured_fraction_theta_max .782 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full .971 _refine_diff_density_max 1.930 _refine_diff_density_min -.566 _refine_diff_density_rms .113 # Attachment '3.cif' #============================================================================== data_3 _database_code_depnum_ccdc_archive 'CCDC 618008' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '(Ag(SS-chxn))BF4\\times0.33 H2O' _chemical_melting_point ? _chemical_formula_moiety 'C18 H42 Ag3 N6, 3(B F4), H2 O' _chemical_formula_sum 'C18 H44 Ag3 B3 F12 N6 O' _chemical_formula_weight 944.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 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' _cell_length_a 16.793(9) _cell_length_b 8.058(4) _cell_length_c 11.766(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1592.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2389 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 24.10 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 1.922 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.83 _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11789 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.0996 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 29.11 _reflns_number_total 4125 _reflns_number_gt 3371 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _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^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration rmad _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_number_reflns 4125 _refine_ls_number_parameters 196 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0684 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1409 _refine_ls_wR_factor_gt 0.1307 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.030 _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 Ag2 Ag 0.0000 0.5000 0.12507(7) 0.0379(2) Uani 1 2 d S . . Ag1 Ag 0.31206(3) 0.29978(6) 0.13683(5) 0.02959(15) Uani 1 1 d . . . N1 N 0.1897(3) 0.2399(6) 0.1632(4) 0.0252(11) Uani 1 1 d . . . H1A H 0.1619 0.2664 0.0983 0.030 Uiso 1 1 calc R . . H1B H 0.1855 0.1270 0.1735 0.030 Uiso 1 1 calc R . . N2 N 0.1226(4) 0.5755(7) 0.1488(5) 0.0369(13) Uani 1 1 d . . . H2A H 0.1517 0.5407 0.0870 0.044 Uiso 1 1 calc R . . H2B H 0.1246 0.6896 0.1503 0.044 Uiso 1 1 calc R . . N3 N 0.4347(4) 0.3780(8) 0.1325(5) 0.0394(14) Uani 1 1 d . . . H3A H 0.4670 0.2866 0.1237 0.047 Uiso 1 1 calc R . . H3B H 0.4426 0.4465 0.0709 0.047 Uiso 1 1 calc R . . C1 C 0.1511(4) 0.3240(8) 0.2611(5) 0.0245(13) Uani 1 1 d . . . H1 H 0.0929 0.2977 0.2595 0.029 Uiso 1 1 calc R . . C2 C 0.1609(5) 0.5117(9) 0.2526(5) 0.0320(16) Uani 1 1 d . . . H2 H 0.2191 0.5379 0.2490 0.038 Uiso 1 1 calc R . . C3 C 0.1259(5) 0.5966(9) 0.3561(7) 0.0431(18) Uani 1 1 d . . . H3C H 0.0676 0.5778 0.3578 0.052 Uiso 1 1 calc R . . H3D H 0.1352 0.7177 0.3506 0.052 Uiso 1 1 calc R . . C4 C 0.1627(5) 0.5315(11) 0.4655(6) 0.044(2) Uani 1 1 d . . . H4A H 0.1386 0.5881 0.5317 0.053 Uiso 1 1 calc R . . H4B H 0.2207 0.5539 0.4659 0.053 Uiso 1 1 calc R . . C5 C 0.1477(6) 0.3436(10) 0.4731(6) 0.044(2) Uani 1 1 d . . . H5A H 0.1709 0.2993 0.5443 0.053 Uiso 1 1 calc R . . H5B H 0.0897 0.3214 0.4741 0.053 Uiso 1 1 calc R . . C6 C 0.1855(4) 0.2588(8) 0.3713(6) 0.0316(14) Uani 1 1 d . . . H6A H 0.2437 0.2782 0.3723 0.038 Uiso 1 1 calc R . . H6B H 0.1763 0.1376 0.3762 0.038 Uiso 1 1 calc R . . C7 C 0.4570(4) 0.4655(9) 0.2357(5) 0.0276(15) Uani 1 1 d . . . H7 H 0.4204 0.5628 0.2430 0.033 Uiso 1 1 calc R . . C8 C 0.4454(5) 0.3607(9) 0.3388(6) 0.0355(16) Uani 1 1 d . . . H8A H 0.4836 0.2673 0.3372 0.043 Uiso 1 1 calc R . . H8B H 0.3909 0.3136 0.3379 0.043 Uiso 1 1 calc R . . C9 C 0.4570(5) 0.4587(11) 0.4469(6) 0.044(2) Uani 1 1 d . . . H9A H 0.4516 0.3843 0.5135 0.053 Uiso 1 1 calc R . . H9B H 0.4158 0.5460 0.4526 0.053 Uiso 1 1 calc R . . F1 F 0.3147(3) 0.6907(6) 0.1074(5) 0.0589(14) Uani 1 1 d U . . F2 F 0.3727(6) 0.8767(10) 0.2228(6) 0.109(3) Uani 1 1 d U . . F4 F 0.2430(5) 0.8689(8) 0.2189(6) 0.103(3) Uani 1 1 d U . . F3 F 0.3050(4) 0.9611(6) 0.0652(4) 0.0592(15) Uani 1 1 d U . . B1 B 0.3141(7) 0.8493(11) 0.1504(8) 0.049(2) Uani 1 1 d . . . F6 F -0.0249(3) 0.8700(6) 0.0870(4) 0.0507(13) Uani 1 1 d U . . F5 F 0.0607(5) 0.9487(9) 0.2177(8) 0.140(4) Uani 1 1 d U . . B2 B 0.0000 1.0000 0.1552(9) 0.028(2) Uani 1 2 d S . . O1 O 0.0000 0.5000 -0.1023(8) 0.096(4) Uani 1 2 d SU . . H1O H -0.0415 0.4721 -0.1362 0.116 Uiso 1 1 d 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 Ag2 0.0425(4) 0.0373(4) 0.0341(4) 0.000 0.000 0.0192(3) Ag1 0.0273(2) 0.0287(2) 0.0328(2) -0.0064(2) 0.0035(2) -0.00798(19) N1 0.025(3) 0.019(2) 0.032(3) -0.0026(18) 0.001(2) 0.004(2) N2 0.046(3) 0.021(3) 0.043(3) 0.009(3) 0.010(3) 0.013(2) N3 0.037(3) 0.047(4) 0.034(3) -0.010(3) 0.012(3) -0.017(3) C1 0.027(3) 0.015(3) 0.032(3) -0.004(2) -0.001(3) 0.003(2) C2 0.042(4) 0.025(3) 0.029(3) 0.001(3) 0.002(3) -0.006(3) C3 0.054(5) 0.026(3) 0.049(4) -0.012(4) 0.017(4) 0.000(3) C4 0.053(5) 0.043(5) 0.036(4) -0.020(3) -0.009(4) -0.013(4) C5 0.063(6) 0.046(5) 0.022(3) 0.004(3) -0.003(3) -0.005(4) C6 0.035(3) 0.030(3) 0.030(3) 0.006(3) 0.001(3) 0.003(3) C7 0.021(3) 0.033(4) 0.029(3) -0.003(3) 0.004(3) -0.002(3) C8 0.039(4) 0.026(3) 0.042(4) 0.001(3) 0.005(3) -0.006(3) C9 0.058(6) 0.043(5) 0.030(3) 0.004(3) 0.002(4) -0.008(4) F1 0.072(3) 0.030(2) 0.075(4) 0.001(2) -0.005(3) 0.011(3) F2 0.158(8) 0.096(6) 0.073(4) 0.002(4) -0.041(5) -0.030(6) F4 0.164(7) 0.046(4) 0.099(5) 0.001(4) 0.079(5) -0.009(4) F3 0.106(4) 0.028(2) 0.045(2) 0.0038(19) 0.015(3) 0.007(3) B1 0.073(7) 0.030(4) 0.043(5) -0.002(4) -0.002(6) 0.004(4) F6 0.073(3) 0.035(2) 0.044(2) -0.011(2) 0.021(2) -0.025(2) F5 0.161(8) 0.066(5) 0.192(8) 0.043(5) -0.128(7) -0.022(5) B2 0.037(6) 0.016(4) 0.030(5) 0.000 0.000 -0.013(4) O1 0.071(7) 0.155(13) 0.063(6) 0.000 0.000 -0.016(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag2 N2 2.165(7) 2_565 ? Ag2 N2 2.165(7) . ? Ag1 N1 2.133(5) . ? Ag1 N3 2.155(6) . ? N1 C1 1.485(8) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.473(9) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C7 1.453(8) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? C1 C6 1.514(9) . ? C1 C2 1.524(10) . ? C1 H1 1.0000 . ? C2 C3 1.515(10) . ? C2 H2 1.0000 . ? C3 C4 1.522(11) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 C5 1.538(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.519(10) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.492(9) . ? C7 C7 1.546(13) 2_665 ? C7 H7 1.0000 . ? C8 C9 1.510(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C9 1.590(16) 2_665 ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? F1 B1 1.375(10) . ? F2 B1 1.321(13) . ? F4 B1 1.448(13) . ? F3 B1 1.357(11) . ? F6 B2 1.384(7) . ? F5 B2 1.323(8) . ? B2 F5 1.323(8) 2_575 ? B2 F6 1.384(7) 2_575 ? O1 H1O 0.8339 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag2 N2 165.2(3) 2_565 . ? N1 Ag1 N3 172.1(2) . . ? C1 N1 Ag1 115.4(4) . . ? C1 N1 H1A 108.4 . . ? Ag1 N1 H1A 108.4 . . ? C1 N1 H1B 108.4 . . ? Ag1 N1 H1B 108.4 . . ? H1A N1 H1B 107.5 . . ? C2 N2 Ag2 115.1(5) . . ? C2 N2 H2A 108.5 . . ? Ag2 N2 H2A 108.5 . . ? C2 N2 H2B 108.5 . . ? Ag2 N2 H2B 108.5 . . ? H2A N2 H2B 107.5 . . ? C7 N3 Ag1 111.6(4) . . ? C7 N3 H3A 109.3 . . ? Ag1 N3 H3A 109.3 . . ? C7 N3 H3B 109.3 . . ? Ag1 N3 H3B 109.3 . . ? H3A N3 H3B 108.0 . . ? N1 C1 C6 109.8(5) . . ? N1 C1 C2 110.8(5) . . ? C6 C1 C2 111.1(5) . . ? N1 C1 H1 108.4 . . ? C6 C1 H1 108.4 . . ? C2 C1 H1 108.4 . . ? N2 C2 C3 109.8(6) . . ? N2 C2 C1 110.7(6) . . ? C3 C2 C1 110.7(6) . . ? N2 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? C1 C2 H2 108.5 . . ? C2 C3 C4 111.5(6) . . ? C2 C3 H3C 109.3 . . ? C4 C3 H3C 109.3 . . ? C2 C3 H3D 109.3 . . ? C4 C3 H3D 109.3 . . ? H3C C3 H3D 108.0 . . ? C3 C4 C5 108.8(6) . . ? C3 C4 H4A 109.9 . . ? C5 C4 H4A 109.9 . . ? C3 C4 H4B 109.9 . . ? C5 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C6 C5 C4 109.1(6) . . ? C6 C5 H5A 109.9 . . ? C4 C5 H5A 109.9 . . ? C6 C5 H5B 109.9 . . ? C4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C1 C6 C5 111.1(5) . . ? C1 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C1 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N3 C7 C8 111.8(6) . . ? N3 C7 C7 114.5(4) . 2_665 ? C8 C7 C7 109.0(5) . 2_665 ? N3 C7 H7 107.0 . . ? C8 C7 H7 107.0 . . ? C7 C7 H7 107.0 2_665 . ? C7 C8 C9 111.9(6) . . ? C7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? C7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? C8 C9 C9 109.7(6) . 2_665 ? C8 C9 H9A 109.7 . . ? C9 C9 H9A 109.7 2_665 . ? C8 C9 H9B 109.7 . . ? C9 C9 H9B 109.7 2_665 . ? H9A C9 H9B 108.2 . . ? F2 B1 F3 116.7(9) . . ? F2 B1 F1 112.8(9) . . ? F3 B1 F1 110.2(7) . . ? F2 B1 F4 103.7(8) . . ? F3 B1 F4 104.2(8) . . ? F1 B1 F4 108.2(8) . . ? F5 B2 F5 112.4(12) 2_575 . ? F5 B2 F6 108.6(4) 2_575 2_575 ? F5 B2 F6 109.0(4) . 2_575 ? F5 B2 F6 109.0(4) 2_575 . ? F5 B2 F6 108.6(4) . . ? F6 B2 F6 109.2(8) 2_575 . ? _diffrn_measured_fraction_theta_max .982 _diffrn_reflns_theta_full 29.11 _diffrn_measured_fraction_theta_full .982 _refine_diff_density_max 1.231 _refine_diff_density_min -.718 _refine_diff_density_rms .150 # Attachment '4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 618009' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ag(rac-chxn))BF4 _chemical_melting_point ? _chemical_formula_moiety 'C6 H14 Ag N2, B F4' _chemical_formula_sum 'C6 H14 Ag B F4 N2' _chemical_formula_weight 308.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B .0013 .0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -.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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.108(3) _cell_length_b 9.137(3) _cell_length_c 9.755(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.108(5) _cell_angle_gamma 90.00 _cell_volume 974.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2113 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 28.02 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 2.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.66 _exptl_absorpt_correction_T_max 0.88 _exptl_special_details ; non-merohedral twin: Total Number of Reflections in HKLF 5 file = 2431 Number of which with Twin Contribution = 504 ; _diffrn_ambient_temperature 130(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12883 _diffrn_reflns_av_R_equivalents 0.1378 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 28.37 _reflns_number_total 2431 _reflns_number_gt 2177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _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^)+(0.0409P)^2^+2.2420P] 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 2431 _refine_ls_number_parameters 128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0659 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1131 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.12093(4) 0.08829(4) 0.53813(4) 0.01899(13) Uani 1 1 d . . . N1 N 0.1459(5) 0.0867(5) 0.3231(5) 0.0250(10) Uani 1 1 d . . . H1A H 0.1570 -0.0085 0.2975 0.030 Uiso 1 1 calc R . . H1B H 0.0752 0.1203 0.2686 0.030 Uiso 1 1 calc R . . N2 N 0.1292(5) 0.4012(5) 0.2613(5) 0.0243(10) Uani 1 1 d . . . H2A H 0.1252 0.4950 0.2946 0.029 Uiso 1 1 calc R . . H2B H 0.0616 0.3515 0.2790 0.029 Uiso 1 1 calc R . . C1 C 0.2473(5) 0.1734(5) 0.2928(5) 0.0182(10) Uani 1 1 d . . . H1 H 0.2466 0.1711 0.1901 0.022 Uiso 1 1 calc R . . C2 C 0.2387(4) 0.3304(5) 0.3380(5) 0.0157(9) Uani 1 1 d . . . H2 H 0.2339 0.3317 0.4395 0.019 Uiso 1 1 calc R . . C3 C 0.3506(5) 0.4178(5) 0.3162(6) 0.0215(10) Uani 1 1 d . . . H3A H 0.3533 0.4232 0.2154 0.026 Uiso 1 1 calc R . . H3B H 0.3444 0.5188 0.3509 0.026 Uiso 1 1 calc R . . C4 C 0.4680(5) 0.3472(6) 0.3923(6) 0.0233(11) Uani 1 1 d . . . H4A H 0.5395 0.4030 0.3726 0.028 Uiso 1 1 calc R . . H4B H 0.4690 0.3503 0.4939 0.028 Uiso 1 1 calc R . . C5 C 0.4767(5) 0.1904(6) 0.3462(6) 0.0241(11) Uani 1 1 d . . . H5A H 0.5510 0.1448 0.4001 0.029 Uiso 1 1 calc R . . H5B H 0.4841 0.1883 0.2465 0.029 Uiso 1 1 calc R . . C6 C 0.3652(5) 0.1032(5) 0.3671(5) 0.0202(10) Uani 1 1 d . . . H6A H 0.3630 0.0964 0.4679 0.024 Uiso 1 1 calc R . . H6B H 0.3715 0.0027 0.3312 0.024 Uiso 1 1 calc R . . B1 B 0.1472(5) 0.8074(6) 0.0381(6) 0.0196(11) Uani 1 1 d . . . F1 F 0.2192(3) 0.9291(3) 0.0670(4) 0.0306(8) Uani 1 1 d . . . F2 F 0.2141(4) 0.6937(4) -0.0017(4) 0.0391(9) Uani 1 1 d . . . F3 F 0.0502(3) 0.8395(4) -0.0706(4) 0.0357(8) Uani 1 1 d . . . F4 F 0.0989(3) 0.7677(4) 0.1542(3) 0.0362(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 0.0169(2) 0.01946(19) 0.0196(2) -0.00107(14) 0.00048(15) -0.00356(14) N1 0.020(2) 0.029(2) 0.025(2) 0.0000(18) 0.000(2) -0.0008(17) N2 0.026(2) 0.021(2) 0.024(2) 0.0040(16) -0.002(2) 0.0034(17) C1 0.018(2) 0.021(2) 0.015(2) -0.0018(18) -0.0001(19) 0.0007(18) C2 0.017(2) 0.016(2) 0.014(2) -0.0013(17) 0.0018(19) -0.0002(17) C3 0.020(2) 0.022(2) 0.023(2) 0.0002(19) 0.005(2) -0.0046(18) C4 0.019(2) 0.029(3) 0.021(2) -0.002(2) 0.000(2) -0.006(2) C5 0.018(2) 0.032(3) 0.021(2) 0.001(2) 0.001(2) 0.005(2) C6 0.020(2) 0.020(2) 0.019(2) -0.0003(18) 0.000(2) 0.0066(18) B1 0.015(2) 0.014(2) 0.028(3) 0.002(2) -0.001(2) -0.0093(18) F1 0.0323(18) 0.0215(15) 0.0371(18) -0.0062(13) 0.0034(16) -0.0092(13) F2 0.041(2) 0.0249(17) 0.054(2) -0.0086(16) 0.0145(19) 0.0019(15) F3 0.034(2) 0.043(2) 0.0245(16) 0.0048(15) -0.0103(15) -0.0037(16) F4 0.0300(18) 0.052(2) 0.0286(17) 0.0135(16) 0.0118(15) -0.0019(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 N1 2.164(5) . ? Ag1 N2 2.164(5) 4_566 ? Ag1 Ag1 3.1102(10) 3_556 ? N1 C1 1.449(7) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.462(6) . ? N2 Ag1 2.164(5) 4_565 ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? C1 C2 1.509(6) . ? C1 C6 1.522(7) . ? C1 H1 1.0000 . ? C2 C3 1.524(7) . ? C2 H2 1.0000 . ? C3 C4 1.525(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.510(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.516(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? B1 F1 1.370(6) . ? B1 F2 1.373(7) . ? B1 F4 1.384(7) . ? B1 F3 1.403(6) . ? 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 Ag1 N2 170.10(19) . 4_566 ? N1 Ag1 Ag1 90.98(13) . 3_556 ? N2 Ag1 Ag1 98.40(13) 4_566 3_556 ? C1 N1 Ag1 115.5(3) . . ? C1 N1 H1A 108.4 . . ? Ag1 N1 H1A 108.4 . . ? C1 N1 H1B 108.4 . . ? Ag1 N1 H1B 108.4 . . ? H1A N1 H1B 107.5 . . ? C2 N2 Ag1 114.8(4) . 4_565 ? C2 N2 H2A 108.6 . . ? Ag1 N2 H2A 108.6 4_565 . ? C2 N2 H2B 108.6 . . ? Ag1 N2 H2B 108.6 4_565 . ? H2A N2 H2B 107.5 . . ? N1 C1 C2 111.6(4) . . ? N1 C1 C6 107.9(4) . . ? C2 C1 C6 110.8(4) . . ? N1 C1 H1 108.8 . . ? C2 C1 H1 108.8 . . ? C6 C1 H1 108.8 . . ? N2 C2 C1 111.1(4) . . ? N2 C2 C3 108.8(4) . . ? C1 C2 C3 111.2(4) . . ? N2 C2 H2 108.5 . . ? C1 C2 H2 108.5 . . ? C3 C2 H2 108.5 . . ? C4 C3 C2 111.0(4) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 110.5(4) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 111.2(4) . . ? C4 C5 H5A 109.4 . . ? C6 C5 H5A 109.4 . . ? C4 C5 H5B 109.4 . . ? C6 C5 H5B 109.4 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C1 111.7(4) . . ? C5 C6 H6A 109.3 . . ? C1 C6 H6A 109.3 . . ? C5 C6 H6B 109.3 . . ? C1 C6 H6B 109.3 . . ? H6A C6 H6B 107.9 . . ? F1 B1 F2 110.3(5) . . ? F1 B1 F4 109.9(5) . . ? F2 B1 F4 109.9(4) . . ? F1 B1 F3 109.2(4) . . ? F2 B1 F3 109.1(5) . . ? F4 B1 F3 108.5(4) . . ? _diffrn_measured_fraction_theta_max .995 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full .995 _refine_diff_density_max 2.244 _refine_diff_density_min -3.302 _refine_diff_density_rms .264 # Attachment '5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 618010' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Ag(SS-chxn))NO3 _chemical_melting_point ? _chemical_formula_moiety 'C6 H14 Ag N2, N O3' _chemical_formula_sum 'C6 H14 Ag N3 O3' _chemical_formula_weight 284.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2 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' _cell_length_a 24.132(6) _cell_length_b 6.8438(16) _cell_length_c 11.751(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.354(4) _cell_angle_gamma 90.00 _cell_volume 1937.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3826 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 24.95 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.948 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 2.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (1996)' _exptl_absorpt_correction_T_min 0.50 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; non-merohedral twin Total Number of Reflections in HKLF 5 file = 4407 Number of which with Twin Contribution = 3361 BASF 0.277 ; _diffrn_ambient_temperature 120(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12366 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0637 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.58 _reflns_number_total 4405 _reflns_number_gt 4189 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material ? _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^)+(0.0979P)^2^+1.9151P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(7) _chemical_absolute_configuration rmad _refine_ls_number_reflns 4405 _refine_ls_number_parameters 237 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0552 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1489 _refine_ls_wR_factor_gt 0.1471 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.108 _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 0.01541(2) 0.61610(10) 0.72861(5) 0.01761(16) Uani 1 1 d . . . Ag2 Ag 0.0000 0.38355(11) 0.5000 0.0150(2) Uani 1 2 d S . . Ag3 Ag 0.0000 0.69262(14) 1.0000 0.0240(2) Uani 1 2 d S . . N1 N -0.0763(3) 0.3538(10) 0.5859(6) 0.0138(14) Uani 1 1 d . . . H1A H -0.0917 0.2359 0.5638 0.017 Uiso 1 1 calc R . . H1B H -0.0667 0.3442 0.6627 0.017 Uiso 1 1 calc R . . N2 N -0.0568(3) 0.7624(11) 0.6506(6) 0.0169(14) Uani 1 1 d . . . H2A H -0.0585 0.8844 0.6830 0.020 Uiso 1 1 calc R . . H2B H -0.0505 0.7807 0.5749 0.020 Uiso 1 1 calc R . . N3 N 0.0787(3) 0.4491(11) 0.8173(6) 0.0177(14) Uani 1 1 d . . . H3A H 0.0633 0.3954 0.8799 0.021 Uiso 1 1 calc R . . H3B H 0.0872 0.3468 0.7706 0.021 Uiso 1 1 calc R . . N4 N 0.0881(3) 0.7071(12) 1.0194(6) 0.0204(15) Uani 1 1 d . . . H4A H 0.0968 0.8087 1.0686 0.024 Uiso 1 1 calc R . . H4B H 0.0999 0.5944 1.0560 0.024 Uiso 1 1 calc R . . C1 C -0.1205(3) 0.5017(13) 0.5725(7) 0.0161(17) Uani 1 1 d . . . H1 H -0.1206 0.5540 0.4930 0.019 Uiso 1 1 calc R . . C2 C -0.1117(3) 0.6747(12) 0.6554(7) 0.0151(16) Uani 1 1 d . . . H2 H -0.1148 0.6228 0.7343 0.018 Uiso 1 1 calc R . . C3 C -0.1584(4) 0.8213(13) 0.6332(8) 0.0192(17) Uani 1 1 d . . . H3C H -0.1577 0.8708 0.5541 0.023 Uiso 1 1 calc R . . H3D H -0.1529 0.9337 0.6857 0.023 Uiso 1 1 calc R . . C4 C -0.2147(4) 0.7269(15) 0.6506(8) 0.0233(19) Uani 1 1 d . . . H4C H -0.2160 0.6824 0.7306 0.028 Uiso 1 1 calc R . . H4D H -0.2446 0.8246 0.6361 0.028 Uiso 1 1 calc R . . C5 C -0.2246(4) 0.5551(13) 0.5715(8) 0.0229(19) Uani 1 1 d . . . H5A H -0.2275 0.6013 0.4915 0.027 Uiso 1 1 calc R . . H5B H -0.2600 0.4903 0.5878 0.027 Uiso 1 1 calc R . . C6 C -0.1762(4) 0.4074(13) 0.5876(8) 0.0197(17) Uani 1 1 d . . . H6A H -0.1764 0.3499 0.6649 0.024 Uiso 1 1 calc R . . H6B H -0.1819 0.3001 0.5316 0.024 Uiso 1 1 calc R . . C7 C 0.1325(3) 0.5408(13) 0.8585(7) 0.0162(16) Uani 1 1 d . . . H7 H 0.1520 0.4490 0.9134 0.019 Uiso 1 1 calc R . . C8 C 0.1229(4) 0.7318(13) 0.9200(7) 0.0183(17) Uani 1 1 d . . . H8 H 0.1035 0.8241 0.8651 0.022 Uiso 1 1 calc R . . C9 C 0.1796(4) 0.8229(16) 0.9603(8) 0.027(2) Uani 1 1 d . . . H9A H 0.1733 0.9511 0.9964 0.032 Uiso 1 1 calc R . . H9B H 0.1985 0.7368 1.0181 0.032 Uiso 1 1 calc R . . C10 C 0.2173(4) 0.8506(17) 0.8598(9) 0.031(2) Uani 1 1 d . . . H10A H 0.2006 0.9489 0.8063 0.037 Uiso 1 1 calc R . . H10B H 0.2540 0.8998 0.8888 0.037 Uiso 1 1 calc R . . C11 C 0.2244(4) 0.6599(16) 0.7977(9) 0.031(2) Uani 1 1 d . . . H11A H 0.2451 0.5668 0.8488 0.037 Uiso 1 1 calc R . . H11B H 0.2466 0.6827 0.7306 0.037 Uiso 1 1 calc R . . C12 C 0.1688(4) 0.5714(15) 0.7587(9) 0.027(2) Uani 1 1 d . . . H12A H 0.1750 0.4445 0.7211 0.032 Uiso 1 1 calc R . . H12B H 0.1496 0.6591 0.7022 0.032 Uiso 1 1 calc R . . O1 O 0.1144(3) 0.1373(12) 0.6374(6) 0.0343(17) Uani 1 1 d . . . O2 O 0.0329(4) 0.0813(13) 0.6940(11) 0.065(3) Uani 1 1 d . . . O3 O 0.0733(4) -0.1383(12) 0.5955(7) 0.0366(19) Uani 1 1 d . . . N5 N 0.0731(3) 0.0271(11) 0.6430(6) 0.0198(16) Uani 1 1 d . . . O4 O 0.0708(6) 0.1727(13) 0.0054(7) 0.070(4) Uani 1 1 d . . . O5 O 0.0645(4) 0.3518(10) 0.1562(6) 0.0348(18) Uani 1 1 d . . . O6 O 0.0827(4) 0.0454(11) 0.1738(6) 0.0359(19) Uani 1 1 d . . . N6 N 0.0731(4) 0.1919(13) 0.1112(7) 0.0255(17) 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 0.0155(3) 0.0176(3) 0.0193(3) -0.0016(3) -0.0035(2) -0.0012(2) Ag2 0.0122(4) 0.0153(4) 0.0176(4) 0.000 0.0028(3) 0.000 Ag3 0.0237(5) 0.0267(5) 0.0228(5) 0.000 0.0109(4) 0.000 N1 0.009(3) 0.011(3) 0.021(3) -0.001(3) 0.000(3) 0.001(2) N2 0.015(3) 0.018(3) 0.018(3) 0.000(3) 0.000(3) -0.002(3) N3 0.018(3) 0.016(3) 0.019(4) 0.000(3) 0.004(3) 0.000(3) N4 0.027(4) 0.017(3) 0.017(4) -0.002(3) 0.003(3) 0.001(3) C1 0.012(4) 0.018(4) 0.019(4) -0.002(3) -0.001(3) 0.001(3) C2 0.013(4) 0.014(4) 0.017(4) -0.003(3) -0.002(3) 0.000(3) C3 0.020(4) 0.014(4) 0.023(4) -0.001(3) 0.001(3) 0.005(3) C4 0.016(4) 0.031(5) 0.024(4) -0.003(4) 0.004(4) 0.005(4) C5 0.016(4) 0.023(4) 0.029(5) -0.008(4) 0.001(4) 0.000(3) C6 0.016(4) 0.019(4) 0.024(4) 0.004(4) 0.000(3) 0.000(3) C7 0.014(4) 0.019(4) 0.016(4) 0.003(3) -0.001(3) 0.001(3) C8 0.023(4) 0.018(4) 0.013(4) 0.001(3) -0.002(3) -0.001(3) C9 0.030(5) 0.030(5) 0.020(4) 0.000(4) -0.004(4) -0.008(4) C10 0.026(5) 0.044(6) 0.022(5) -0.003(4) -0.001(4) -0.018(4) C11 0.018(4) 0.047(7) 0.028(5) -0.009(5) 0.007(4) -0.005(4) C12 0.017(4) 0.036(6) 0.028(5) -0.002(4) 0.008(4) -0.001(4) O1 0.036(4) 0.026(4) 0.040(4) 0.002(3) 0.003(3) -0.015(3) O2 0.039(5) 0.037(6) 0.122(9) -0.049(6) 0.027(5) -0.014(4) O3 0.053(5) 0.026(4) 0.033(4) -0.013(3) 0.015(3) -0.005(4) N5 0.030(4) 0.011(3) 0.017(3) 0.004(3) -0.006(3) 0.008(3) O4 0.165(12) 0.033(5) 0.015(4) 0.005(3) 0.018(5) 0.020(6) O5 0.063(5) 0.012(3) 0.030(4) -0.004(3) 0.010(4) -0.004(3) O6 0.067(6) 0.023(4) 0.018(3) 0.008(3) 0.003(4) 0.007(4) N6 0.042(5) 0.017(3) 0.019(4) 0.002(3) 0.006(4) 0.000(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 N3 2.131(7) . ? Ag1 N2 2.167(7) . ? Ag1 Ag2 3.1258(9) . ? Ag1 Ag3 3.2744(10) . ? Ag2 N1 2.160(7) . ? Ag2 N1 2.160(7) 2_556 ? Ag2 Ag1 3.1259(9) 2_556 ? Ag3 N4 2.128(8) 2_557 ? Ag3 N4 2.128(8) . ? Ag3 Ag1 3.2744(10) 2_557 ? N1 C1 1.473(10) . ? N1 H1A 0.9200 . ? N1 H1B 0.9200 . ? N2 C2 1.458(11) . ? N2 H2A 0.9200 . ? N2 H2B 0.9200 . ? N3 C7 1.496(11) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? N4 C8 1.487(12) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? C1 C6 1.512(12) . ? C1 C2 1.540(11) . ? C1 H1 1.0000 . ? C2 C3 1.521(11) . ? C2 H2 1.0000 . ? C3 C4 1.530(13) . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 C5 1.509(13) . ? C4 H4C 0.9900 . ? C4 H4D 0.9900 . ? C5 C6 1.548(12) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.518(12) . ? C7 C12 1.519(13) . ? C7 H7 1.0000 . ? C8 C9 1.552(13) . ? C8 H8 1.0000 . ? C9 C10 1.542(14) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.510(15) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.518(13) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O1 N5 1.255(11) . ? O2 N5 1.227(12) . ? O3 N5 1.262(11) . ? O4 N6 1.247(11) . ? O5 N6 1.238(12) . ? O6 N6 1.257(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ag1 N2 172.2(3) . . ? N3 Ag1 Ag2 101.1(2) . . ? N2 Ag1 Ag2 79.6(2) . . ? N3 Ag1 Ag3 74.2(2) . . ? N2 Ag1 Ag3 101.8(2) . . ? Ag2 Ag1 Ag3 154.67(3) . . ? N1 Ag2 N1 169.2(4) . 2_556 ? N1 Ag2 Ag1 73.02(19) . . ? N1 Ag2 Ag1 112.83(19) 2_556 . ? N1 Ag2 Ag1 112.83(19) . 2_556 ? N1 Ag2 Ag1 73.02(19) 2_556 2_556 ? Ag1 Ag2 Ag1 118.79(4) . 2_556 ? N4 Ag3 N4 174.7(4) 2_557 . ? N4 Ag3 Ag1 86.7(2) 2_557 2_557 ? N4 Ag3 Ag1 94.2(2) . 2_557 ? N4 Ag3 Ag1 94.2(2) 2_557 . ? N4 Ag3 Ag1 86.7(2) . . ? Ag1 Ag3 Ag1 161.59(4) 2_557 . ? C1 N1 Ag2 121.1(5) . . ? C1 N1 H1A 107.0 . . ? Ag2 N1 H1A 107.0 . . ? C1 N1 H1B 107.0 . . ? Ag2 N1 H1B 107.0 . . ? H1A N1 H1B 106.8 . . ? C2 N2 Ag1 120.2(5) . . ? C2 N2 H2A 107.3 . . ? Ag1 N2 H2A 107.3 . . ? C2 N2 H2B 107.3 . . ? Ag1 N2 H2B 107.3 . . ? H2A N2 H2B 106.9 . . ? C7 N3 Ag1 121.1(5) . . ? C7 N3 H3A 107.1 . . ? Ag1 N3 H3A 107.1 . . ? C7 N3 H3B 107.1 . . ? Ag1 N3 H3B 107.1 . . ? H3A N3 H3B 106.8 . . ? C8 N4 Ag3 121.9(6) . . ? C8 N4 H4A 106.9 . . ? Ag3 N4 H4A 106.9 . . ? C8 N4 H4B 106.9 . . ? Ag3 N4 H4B 106.9 . . ? H4A N4 H4B 106.7 . . ? N1 C1 C6 109.8(7) . . ? N1 C1 C2 112.8(7) . . ? C6 C1 C2 110.2(7) . . ? N1 C1 H1 108.0 . . ? C6 C1 H1 108.0 . . ? C2 C1 H1 108.0 . . ? N2 C2 C3 112.8(7) . . ? N2 C2 C1 112.6(7) . . ? C3 C2 C1 109.0(7) . . ? N2 C2 H2 107.4 . . ? C3 C2 H2 107.4 . . ? C1 C2 H2 107.4 . . ? C2 C3 C4 110.7(7) . . ? C2 C3 H3C 109.5 . . ? C4 C3 H3C 109.5 . . ? C2 C3 H3D 109.5 . . ? C4 C3 H3D 109.5 . . ? H3C C3 H3D 108.1 . . ? C5 C4 C3 110.8(8) . . ? C5 C4 H4C 109.5 . . ? C3 C4 H4C 109.5 . . ? C5 C4 H4D 109.5 . . ? C3 C4 H4D 109.5 . . ? H4C C4 H4D 108.1 . . ? C4 C5 C6 110.1(7) . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.2 . . ? C1 C6 C5 112.1(7) . . ? C1 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C1 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N3 C7 C8 111.3(7) . . ? N3 C7 C12 109.8(7) . . ? C8 C7 C12 111.1(8) . . ? N3 C7 H7 108.2 . . ? C8 C7 H7 108.2 . . ? C12 C7 H7 108.2 . . ? N4 C8 C7 112.6(7) . . ? N4 C8 C9 109.5(7) . . ? C7 C8 C9 109.6(8) . . ? N4 C8 H8 108.3 . . ? C7 C8 H8 108.3 . . ? C9 C8 H8 108.3 . . ? C10 C9 C8 111.3(8) . . ? C10 C9 H9A 109.4 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.4 . . ? C8 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C9 110.7(9) . . ? C11 C10 H10A 109.5 . . ? C9 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C10 C11 C12 111.5(8) . . ? C10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C7 111.3(8) . . ? C11 C12 H12A 109.4 . . ? C7 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? C7 C12 H12B 109.4 . . ? H12A C12 H12B 108.0 . . ? O2 N5 O1 119.8(8) . . ? O2 N5 O3 120.7(9) . . ? O1 N5 O3 119.4(9) . . ? O5 N6 O4 121.3(9) . . ? O5 N6 O6 119.0(8) . . ? O4 N6 O6 119.7(8) . . ? _diffrn_measured_fraction_theta_max .983 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full .983 _refine_diff_density_max 2.156 _refine_diff_density_min -1.068 _refine_diff_density_rms .222