# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Konstantin V. Domasevitch' _publ_contact_author_email DK@MAIL.UNIV.KIEV.UA _publ_section_title ; 1,2,4,5-Tetrazine: An unprecedented mu4-coordination that enhances ability for anion/pi interactions ; loop_ _publ_author_name 'Konstantin V. Domasevitch' 'Alexander N Chernega' 'Daniel Escudero' 'Antonio Frontera' ; I.Gural'skiy ; 'Harald Krautscheid' 'Eduard B Rusanov' 'Pavlo V Solntsev' # Attachment 'Cif_data.cif' data_(1) _database_code_depnum_ccdc_archive 'CCDC 679092' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Nitrate complex with 1,2,4,5-tetrazine ; _chemical_name_common 'Silver(i) Nitrate complex with 1,2,4,5-tetrazine' _chemical_melting_point ? _chemical_formula_moiety '(C2 H2 N4), Ag, (N O3)' _chemical_formula_sum 'C2 H2 Ag N5 O3' _chemical_formula_weight 251.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.7351(7) _cell_length_b 10.8172(8) _cell_length_c 7.1540(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 598.59(9) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4180 _cell_measurement_theta_min 3.88 _cell_measurement_theta_max 28.19 _exptl_crystal_description prism _exptl_crystal_colour red-violet _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.796 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 480 _exptl_absorpt_coefficient_mu 3.328 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5857 _exptl_absorpt_correction_T_max 0.7320 _exptl_absorpt_process_details 'X-RED and X-SHAPE, Stoe&Cie GmbH' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4180 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.88 _diffrn_reflns_theta_max 28.19 _reflns_number_total 762 _reflns_number_gt 678 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0293P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 762 _refine_ls_number_parameters 71 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.77445(3) 0.7500 0.20789(4) 0.02955(10) Uani 1 2 d S . . O1 O 0.9962(6) 0.6732(5) -0.0031(8) 0.0545(13) Uani 0.50 1 d P . . O2 O 0.9823(6) 0.8584(4) -0.1109(10) 0.0538(12) Uani 0.50 1 d P . . O3 O 1.1096(8) 0.7150(4) -0.2675(7) 0.0688(15) Uani 0.50 1 d P . . N1 N 0.5911(2) 0.58155(16) 0.1046(3) 0.0320(4) Uani 1 1 d . . . N2 N 0.4214(2) 0.59212(16) 0.0959(3) 0.0318(4) Uani 1 1 d . . . N3 N 1.0290(3) 0.7500 -0.1305(4) 0.0299(5) Uani 1 2 d S . . C1 C 0.6635(3) 0.48930(18) 0.0092(4) 0.0322(5) Uani 1 1 d . . . H1 H 0.784(3) 0.481(2) 0.017(5) 0.036(8) 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 Ag1 0.02906(14) 0.02561(13) 0.03399(16) 0.000 -0.00507(9) 0.000 O1 0.049(2) 0.066(3) 0.049(3) 0.029(2) 0.014(2) 0.019(2) O2 0.049(2) 0.0346(19) 0.078(4) -0.014(2) -0.011(3) 0.0101(16) O3 0.094(4) 0.073(4) 0.040(2) 0.0025(18) 0.030(2) 0.023(3) N1 0.0264(9) 0.0330(8) 0.0366(11) -0.0086(8) 0.0003(8) -0.0005(7) N2 0.0260(9) 0.0306(7) 0.0388(11) -0.0073(8) 0.0029(7) 0.0003(7) N3 0.0307(13) 0.0345(12) 0.0245(12) 0.000 -0.0020(11) 0.000 C1 0.0237(9) 0.0325(10) 0.0406(13) -0.0066(8) 0.0010(9) 0.0000(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 Ag1 N1 2.4242(18) . ? Ag1 N1 2.4242(18) 7_575 ? Ag1 O1 2.431(5) 7_575 ? Ag1 O1 2.431(5) . ? Ag1 N2 2.4857(19) 4_565 ? Ag1 N2 2.4857(19) 6_656 ? O1 N3 1.259(5) . ? O2 N3 1.235(4) . ? O3 N3 1.222(5) . ? N1 N2 1.320(3) . ? N1 C1 1.332(3) . ? N2 C1 1.331(3) 5_665 ? C1 N2 1.331(3) 5_665 ? C1 H1 0.94(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N1 97.47(9) . 7_575 ? N1 Ag1 O1 118.69(11) . 7_575 ? N1 Ag1 O1 88.08(16) . . ? N1 Ag1 O1 118.69(11) 7_575 . ? N1 Ag1 N2 162.93(8) . 4_565 ? O1 Ag1 N2 78.09(11) 7_575 4_565 ? O1 Ag1 N2 105.25(16) . 4_565 ? N1 Ag1 N2 85.59(6) . 6_656 ? N1 Ag1 N2 162.93(8) 7_575 6_656 ? O1 Ag1 N2 105.25(16) 7_575 6_656 ? O1 Ag1 N2 78.09(11) . 6_656 ? N2 Ag1 N2 86.79(9) 4_565 6_656 ? N3 O1 Ag1 111.5(3) . . ? N2 N1 C1 117.30(19) . . ? N2 N1 Ag1 122.09(13) . . ? C1 N1 Ag1 118.26(14) . . ? N1 N2 C1 117.39(18) . 5_665 ? N1 N2 Ag1 119.19(14) . 6_556 ? C1 N2 Ag1 123.25(14) 5_665 6_556 ? O3 N3 O2 122.3(4) 7_575 7_575 ? O3 N3 O2 122.3(4) . . ? O3 N3 O1 118.6(3) 7_575 7_575 ? O2 N3 O1 119.0(5) 7_575 7_575 ? O3 N3 O1 118.6(3) . . ? O2 N3 O1 119.0(5) . . ? N2 C1 N1 125.3(2) 5_665 . ? N2 C1 H1 117.6(19) 5_665 . ? N1 C1 H1 117.1(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ag1 O1 N3 115.8(4) . . . . ? N1 Ag1 O1 N3 18.4(5) 7_575 . . . ? N2 Ag1 O1 N3 -75.0(4) 4_565 . . . ? N2 Ag1 O1 N3 -158.3(4) 6_656 . . . ? N1 Ag1 O1 O1 142.00(7) . . . 7_575 ? N1 Ag1 N1 N2 -29.6(2) 7_575 . . . ? O1 Ag1 N1 N2 -121.5(3) 7_575 . . . ? O1 Ag1 N1 N2 -148.2(2) . . . . ? N2 Ag1 N1 N2 69.8(3) 4_565 . . . ? N2 Ag1 N1 N2 133.56(18) 6_656 . . . ? N1 Ag1 N1 C1 132.58(16) 7_575 . . . ? O1 Ag1 N1 C1 40.7(3) 7_575 . . . ? O1 Ag1 N1 C1 13.9(2) . . . . ? N2 Ag1 N1 C1 -128.1(2) 4_565 . . . ? N2 Ag1 N1 C1 -64.3(2) 6_656 . . . ? C1 N1 N2 C1 -0.7(4) . . . 5_665 ? Ag1 N1 N2 C1 161.56(16) . . . 5_665 ? C1 N1 N2 Ag1 174.60(17) . . . 6_556 ? Ag1 N1 N2 Ag1 -23.1(3) . . . 6_556 ? Ag1 O1 N3 O3 -164.9(4) . . . . ? N2 N1 C1 N2 0.8(4) . . . 5_665 ? Ag1 N1 C1 N2 -162.19(19) . . . 5_665 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.19 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.541 _refine_diff_density_min -0.868 _refine_diff_density_rms 0.089 #============================================================================== data_(2) _database_code_depnum_ccdc_archive 'CCDC 679093' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Perchlorate complex with 1,2,4,5-tetrazine ; _chemical_name_common 'Silver(i) Perchlorate complex with 1,2,4,5-tetrazine' _chemical_melting_point ? _chemical_formula_moiety '(C2 H2 N4), Ag, (Cl O4)' _chemical_formula_sum 'C2 H2 Ag Cl N4 O4' _chemical_formula_weight 289.40 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 Orthorhombic _symmetry_space_group_name_H-M 'I m m a' _space_group_name_Hall '-I 2b 2' _symmetry_Int_Tables_number 74 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-x, y+1/2, -z' 'x, -y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x, y-1/2, -z' 'x, -y-1/2, z' '-x, y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 8.4650(7) _cell_length_b 10.4250(11) _cell_length_c 7.7750(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 686.13(11) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 1878 _cell_measurement_theta_min 4.29 _cell_measurement_theta_max 28.13 _exptl_crystal_description prism _exptl_crystal_colour red-violet _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 3.306 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6924 _exptl_absorpt_correction_T_max 0.7779 _exptl_absorpt_process_details 'X-RED and X-SHAPE, Stoe&Cie GmbH' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 1878 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0240 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 4.29 _diffrn_reflns_theta_max 28.13 _reflns_number_total 473 _reflns_number_gt 368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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. Chlorine atom of the perchlorate anion is situated on intersection of two mirror planes (site letter 4e). Oxygen atoms of the anion reside in general positions and are equally disordered over two crystallographically independent orientations. In total this affords disordering of the oxygen atoms over 8 positions. The disorder was readily resolved and refined with a set of soft restraints for the geometry of ClO4, the ordered Cl atom was refined anisotropically and the oxygen atoms were left isotropic. Subsequent refinement led to a perfect convergence and very reasonable isotropic U values for all oxygen atoms (Uiso = 0.051-0.101 A^2). Attempted refinement in space groups of lower symmetry (cf. C2/m) gave no any improvements and led to unresoluble disorder of oxygen atoms of ClO4 group. ; _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^)+(0.0612P)^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_number_reflns 473 _refine_ls_number_parameters 55 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0449 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0845 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.2500 0.7500 0.2500 0.0472(3) Uani 1 4 d S . . N1 N 0.0787(5) 0.5851(3) 0.1021(6) 0.0501(9) Uani 1 1 d . . . C2 C 0.1506(8) 0.5000 0.0000 0.0537(17) Uani 1 2 d S . . H2 H 0.2617 0.5000 0.0000 0.064 Uiso 1 2 calc SR B . Cl1 Cl 0.0000 0.7500 0.6145(3) 0.0429(5) Uani 1 4 d SD . . O1 O -0.1602(14) 0.713(2) 0.636(5) 0.092(13) Uiso 0.13 1 d PD A -1 O2 O 0.100(3) 0.6458(17) 0.641(4) 0.100(13) Uiso 0.13 1 d PD B -1 O3 O 0.020(5) 0.801(2) 0.4472(15) 0.090(11) Uiso 0.13 1 d PD C -1 O4 O 0.033(3) 0.8494(15) 0.734(2) 0.051(7) Uiso 0.13 1 d PD D -1 O1A O 0.014(4) 0.7121(16) 0.7871(14) 0.057(7) Uiso 0.13 1 d PD B -2 O2A O -0.1563(13) 0.7235(19) 0.554(3) 0.045(7) Uiso 0.13 1 d PD . -2 O3A O 0.024(3) 0.8845(9) 0.602(3) 0.067(7) Uiso 0.13 1 d PD E -2 O4A O 0.109(2) 0.685(2) 0.511(3) 0.102(13) Uiso 0.13 1 d PD B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0467(5) 0.0446(4) 0.0503(4) 0.000 -0.0085(3) 0.000 N1 0.044(2) 0.0407(17) 0.066(3) -0.0092(14) -0.0029(19) 0.0008(14) C2 0.047(5) 0.042(3) 0.072(5) -0.015(3) 0.000 0.000 Cl1 0.0483(13) 0.0464(9) 0.0341(10) 0.000 0.000 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 O4A 2.45(2) 11_575 ? Ag1 O4A 2.45(2) . ? Ag1 O4A 2.45(2) 7_545 ? Ag1 O4A 2.45(2) 13_565 ? Ag1 O2A 2.51(2) 2_565 ? Ag1 O2A 2.51(2) 12 ? Ag1 O2A 2.51(2) 14 ? Ag1 O2A 2.51(2) 8_565 ? Ag1 N1 2.526(4) 13_565 ? Ag1 N1 2.526(4) . ? Ag1 N1 2.526(4) 7_545 ? Ag1 N1 2.526(4) 11_575 ? Ag1 O3 2.54(3) 11_575 ? Ag1 O3 2.54(3) 7_545 ? Ag1 O3 2.54(3) 13_565 ? Ag1 O3 2.54(3) . ? N1 N1 1.333(8) 12 ? N1 C2 1.337(5) . ? C2 N1 1.337(5) 4_565 ? C2 H2 0.9400 . ? O1 Cl1 1.420(9) . ? O2 Cl1 1.392(9) . ? O3 Cl1 1.416(9) . ? O4 Cl1 1.421(9) . ? O1A Cl1 1.404(8) . ? O2A Cl1 1.430(9) . ? O2A Ag1 2.51(2) 2_565 ? O3A Cl1 1.420(8) . ? O4A Cl1 1.398(9) . ? 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 O4A Ag1 N1 84.8(5) . . ? O2A Ag1 N1 108.8(4) 2_565 . ? O2A Ag1 N1 80.1(4) 14 11_575 ? O2A Ag1 N1 71.2(4) 8_565 11_575 ? N1 Ag1 O3 88.7(7) 13_565 13_565 ? N1 Ag1 O3 91.3(6) . 13_565 ? N1 Ag1 O3 72.0(5) 7_545 13_565 ? N1 Ag1 O3 108.0(5) 11_575 13_565 ? N1 Ag1 N1 94.22(17) 13_565 11_575 ? N1 Ag1 N1 85.78(17) . 11_575 ? N1 Ag1 N1 180.0 7_545 11_575 ? N1 N1 C2 117.1(3) 12 . ? N1 N1 Ag1 125.03(9) 12 . ? C2 N1 Ag1 117.4(4) . . ? N1 C2 N1 125.8(7) 4_565 . ? N1 C2 H2 117.1 4_565 . ? N1 C2 H2 117.1 . . ? Cl1 O3 Ag1 125(2) . . ? Cl1 O2A Ag1 125.4(13) . 2_565 ? Cl1 O4A Ag1 131.8(17) . . ? O1 Cl1 O2 110.5(9) . . ? O1 Cl1 O3 108.8(9) . . ? O1 Cl1 O4 108.2(8) . . ? O2 Cl1 O3 111.0(9) . . ? O2 Cl1 O4 110.7(8) . . ? O3 Cl1 O4 107.7(8) . . ? O1A Cl1 O2A 109.5(8) . . ? O1A Cl1 O3A 109.5(8) . . ? O1A Cl1 O4A 111.2(8) . . ? O2A Cl1 O3A 107.4(8) . . ? O2A Cl1 O4A 109.2(8) . . ? O3A Cl1 O4A 110.1(8) . . ? 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 O4A Ag1 N1 N1 34.0(6) 11_575 . . 12 ? O4A Ag1 N1 N1 57.7(5) . . . 12 ? O4A Ag1 N1 N1 -146.0(6) 7_545 . . 12 ? O4A Ag1 N1 N1 -122.3(5) 13_565 . . 12 ? O2A Ag1 N1 N1 49.7(5) 2_565 . . 12 ? O2A Ag1 N1 N1 59.0(4) 12 . . 12 ? O2A Ag1 N1 N1 -130.3(5) 14 . . 12 ? O2A Ag1 N1 N1 -121.0(4) 8_565 . . 12 ? N1 Ag1 N1 N1 130.64(16) 7_545 . . 12 ? N1 Ag1 N1 N1 -49.36(16) 11_575 . . 12 ? O4A Ag1 N1 C2 -154.1(6) 11_575 . . . ? O4A Ag1 N1 C2 -130.4(6) . . . . ? O4A Ag1 N1 C2 25.9(6) 7_545 . . . ? O4A Ag1 N1 C2 49.6(6) 13_565 . . . ? O2A Ag1 N1 C2 -138.4(5) 2_565 . . . ? O2A Ag1 N1 C2 -129.0(5) 12 . . . ? O2A Ag1 N1 C2 41.6(5) 14 . . . ? O2A Ag1 N1 C2 51.0(5) 8_565 . . . ? O3 Ag1 N1 N1 40.6(7) 11_575 . . 12 ? O3 Ag1 N1 N1 -139.4(7) 7_545 . . 12 ? O3 Ag1 N1 N1 -157.3(5) 13_565 . . 12 ? O3 Ag1 N1 N1 22.7(5) . . . 12 ? N1 Ag1 N1 C2 -57.4(2) 7_545 . . . ? N1 Ag1 N1 C2 122.6(2) 11_575 . . . ? N1 N1 C2 N1 0.0 12 . . 4_565 ? Ag1 N1 C2 N1 -172.6(3) . . . 4_565 ? N1 Ag1 O3 Cl1 -82.6(18) 13_565 . . . ? N1 Ag1 O3 Cl1 97.4(18) . . . . ? N1 Ag1 O3 Cl1 3(2) 7_545 . . . ? N1 Ag1 O3 Cl1 -177(2) 11_575 . . . ? N1 Ag1 O4A Cl1 68.5(19) 13_565 . . . ? N1 Ag1 O4A Cl1 -111.5(19) . . . . ? N1 Ag1 O4A Cl1 153(2) 7_545 . . . ? N1 Ag1 O4A Cl1 -27(2) 11_575 . . . ? Ag1 O4A Cl1 O1A -148(2) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 28.13 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.691 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.125 #============================================================================== data_(3) _database_code_depnum_ccdc_archive 'CCDC 679094' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Nitrate 2:1 complex with 3,6-dimethyl-1,2,4,5-tetrazine ; _chemical_name_common ;Silver(i) Nitrate 2:1 complex with 3,6-dimethyl-1,2,4,5- tetrazine ; _chemical_melting_point ? _chemical_formula_moiety '(C4 H6 N4), 2Ag, 2(N O3)' _chemical_formula_sum 'C4 H6 Ag2 N6 O6' _chemical_formula_weight 449.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _space_group_name_Hall '-P 2ac 2n' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 9.0359(8) _cell_length_b 13.2071(13) _cell_length_c 8.7513(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1044.36(16) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7298 _cell_measurement_theta_min 4.48 _cell_measurement_theta_max 27.87 _exptl_crystal_description prism _exptl_crystal_colour red-violet _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 2.861 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 3.785 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5490 _exptl_absorpt_correction_T_max 0.7034 _exptl_absorpt_process_details 'X-RED and X-SHAPE, Stoe&Cie GmbH' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 7298 _diffrn_reflns_av_R_equivalents 0.0714 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 4.48 _diffrn_reflns_theta_max 27.87 _reflns_number_total 1291 _reflns_number_gt 934 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0262P)^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_number_reflns 1291 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0213 _refine_ls_wR_factor_ref 0.0520 _refine_ls_wR_factor_gt 0.0504 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _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 0.59722(3) 0.496842(10) 0.16703(2) 0.03552(9) Uani 1 1 d . . . O1 O 0.7384(2) 0.52280(14) 0.4111(2) 0.0423(5) Uani 1 1 d . . . O2 O 0.5258(2) 0.59775(13) 0.4026(2) 0.0412(4) Uani 1 1 d . . . O3 O 0.6569(2) 0.60301(15) 0.6111(2) 0.0494(5) Uani 1 1 d . . . N1 N 0.5814(2) 0.66090(12) 0.0373(2) 0.0244(4) Uani 1 1 d . . . N2 N 0.4962(2) 0.66093(11) -0.0859(2) 0.0239(4) Uani 1 1 d . . . N3 N 0.6398(3) 0.57494(14) 0.4756(2) 0.0332(5) Uani 1 1 d . . . C1 C 0.6325(4) 0.7500 0.0899(4) 0.0236(6) Uani 1 2 d S . . C2 C 0.7451(4) 0.7500 0.2136(4) 0.0323(8) Uani 1 2 d S . . H2A H 0.7708 0.8192 0.2394 0.048 Uiso 0.50 1 calc PR . . H2B H 0.8328 0.7144 0.1792 0.048 Uiso 0.50 1 calc PR . . H2C H 0.7051 0.7164 0.3031 0.048 Uiso 0.50 1 calc PR . . C3 C 0.4620(4) 0.7500 -0.1526(3) 0.0239(7) Uani 1 2 d S . . C4 C 0.3770(4) 0.7500 -0.2981(4) 0.0297(7) Uani 1 2 d S . . H4A H 0.3611 0.6808 -0.3313 0.045 Uiso 0.50 1 calc PR . . H4B H 0.4322 0.7864 -0.3756 0.045 Uiso 0.50 1 calc PR . . H4C H 0.2822 0.7828 -0.2822 0.045 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.04761(17) 0.02646(11) 0.03248(12) -0.00351(7) -0.00816(8) 0.00113(7) O1 0.0434(12) 0.0440(8) 0.0396(10) -0.0067(8) -0.0013(9) 0.0118(9) O2 0.0329(12) 0.0490(8) 0.0416(10) 0.0043(8) -0.0110(9) 0.0013(8) O3 0.0455(13) 0.0687(11) 0.0340(10) -0.0183(9) -0.0049(10) 0.0010(10) N1 0.0243(11) 0.0256(8) 0.0234(9) -0.0008(7) 0.0007(8) 0.0000(7) N2 0.0220(10) 0.0264(7) 0.0233(9) -0.0019(6) -0.0004(8) 0.0001(8) N3 0.0347(12) 0.0351(9) 0.0299(10) -0.0015(8) 0.0003(10) -0.0030(9) C1 0.0215(17) 0.0241(12) 0.0252(16) 0.000 0.0010(13) 0.000 C2 0.032(2) 0.0297(12) 0.0354(19) 0.000 -0.0126(16) 0.000 C3 0.0192(17) 0.0270(11) 0.0255(16) 0.000 0.0016(12) 0.000 C4 0.030(2) 0.0305(13) 0.0282(16) 0.000 -0.0061(15) 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 N2 2.3577(16) 5_665 ? Ag1 N1 2.4504(17) . ? Ag1 O1 2.5113(18) . ? Ag1 O2 2.5378(18) . ? O1 N3 1.260(3) . ? O2 N3 1.249(3) . ? O3 N3 1.252(2) . ? N1 N2 1.324(2) . ? N1 C1 1.345(2) . ? N2 C3 1.349(2) . ? C1 N1 1.345(2) 7_575 ? C1 C2 1.486(5) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 N2 1.349(2) 7_575 ? C3 C4 1.487(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 128.39(6) 5_665 . ? N2 Ag1 O1 123.96(6) 5_665 . ? N1 Ag1 O1 107.64(6) . . ? N2 Ag1 O2 128.15(6) 5_665 . ? N1 Ag1 O2 84.10(6) . . ? O1 Ag1 O2 50.71(6) . . ? N3 O1 Ag1 95.55(14) . . ? N3 O2 Ag1 94.56(13) . . ? N2 N1 C1 118.53(18) . . ? N2 N1 Ag1 114.29(11) . . ? C1 N1 Ag1 126.49(16) . . ? N1 N2 C3 119.05(18) . . ? N1 N2 Ag1 116.93(11) . 5_665 ? C3 N2 Ag1 123.94(16) . 5_665 ? O2 N3 O3 121.0(2) . . ? O2 N3 O1 119.03(19) . . ? O3 N3 O1 120.0(2) . . ? N1 C1 N1 122.0(3) 7_575 . ? N1 C1 C2 118.98(14) 7_575 . ? N1 C1 C2 118.98(14) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 N2 121.4(3) 7_575 . ? N2 C3 C4 119.26(14) 7_575 . ? N2 C3 C4 119.26(14) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? 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 Ag1 O1 N3 -112.12(14) 5_665 . . . ? N1 Ag1 O1 N3 68.60(15) . . . . ? O2 Ag1 O1 N3 2.16(12) . . . . ? N2 Ag1 O2 N3 103.80(13) 5_665 . . . ? N1 Ag1 O2 N3 -120.75(13) . . . . ? O1 Ag1 O2 N3 -2.17(12) . . . . ? N2 Ag1 N1 N2 7.5(2) 5_665 . . . ? O1 Ag1 N1 N2 -173.28(13) . . . . ? O2 Ag1 N1 N2 -127.78(15) . . . . ? N2 Ag1 N1 C1 177.8(2) 5_665 . . . ? O1 Ag1 N1 C1 -2.9(2) . . . . ? O2 Ag1 N1 C1 42.6(2) . . . . ? C1 N1 N2 C3 -1.0(3) . . . . ? Ag1 N1 N2 C3 170.17(19) . . . . ? C1 N1 N2 Ag1 -177.74(19) . . . 5_665 ? Ag1 N1 N2 Ag1 -6.57(18) . . . 5_665 ? Ag1 O2 N3 O3 -176.13(19) . . . . ? Ag1 O2 N3 O1 3.8(2) . . . . ? Ag1 O1 N3 O2 -3.9(2) . . . . ? Ag1 O1 N3 O3 176.08(18) . . . . ? N2 N1 C1 N1 10.9(4) . . . 7_575 ? Ag1 N1 C1 N1 -159.10(16) . . . 7_575 ? N2 N1 C1 C2 -171.2(3) . . . . ? Ag1 N1 C1 C2 18.8(4) . . . . ? N1 N2 C3 N2 -8.7(4) . . . 7_575 ? Ag1 N2 C3 N2 167.80(16) 5_665 . . 7_575 ? N1 N2 C3 C4 174.9(3) . . . . ? Ag1 N2 C3 C4 -8.6(4) 5_665 . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.482 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.095 #============================================================================== data_(4) _database_code_depnum_ccdc_archive 'CCDC 679095' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Perchlorate 2:1 complex with 3,6-dimethyl-1,2,4,5-tetrazine, Dihydrate ; _chemical_name_common ; Silver(i) Perchlorate 2:1 complex with 3,6-dimethyl-1,2,4,5- tetrazine, Dihydrate ; _chemical_melting_point ? _chemical_formula_moiety '(C4 H6 N4), 2Ag, 2(Cl O4), 2(H2 O)' _chemical_formula_sum 'C4 H10 Ag2 Cl2 N4 O10' _chemical_formula_weight 560.80 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.7481(8) _cell_length_b 7.9981(9) _cell_length_c 8.1382(10) _cell_angle_alpha 65.302(11) _cell_angle_beta 65.663(10) _cell_angle_gamma 66.151(11) _cell_volume 349.00(8) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3180 _cell_measurement_theta_min 4.68 _cell_measurement_theta_max 28.01 _exptl_crystal_description prism _exptl_crystal_colour red-violet _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 270 _exptl_absorpt_coefficient_mu 3.247 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6592 _exptl_absorpt_correction_T_max 0.7165 _exptl_absorpt_process_details 'X-RED and X-SHAPE, Stoe&Cie GmbH' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 3380 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.68 _diffrn_reflns_theta_max 28.01 _reflns_number_total 1662 _reflns_number_gt 1414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0478P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 1662 _refine_ls_number_parameters 100 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0712 _refine_ls_wR_factor_gt 0.0705 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.46609(3) 0.21585(3) 0.35201(3) 0.02200(11) Uani 1 1 d . . . Cl1 Cl 0.32773(11) 0.72807(9) 0.12648(11) 0.01699(16) Uani 1 1 d . . . O1 O 0.3225(5) 0.5709(3) 0.2998(4) 0.0353(6) Uani 1 1 d . . . O2 O 0.5460(4) 0.7623(4) 0.0462(4) 0.0319(6) Uani 1 1 d . . . O3 O 0.2826(5) 0.6827(4) -0.0067(4) 0.0302(6) Uani 1 1 d . . . O4 O 0.1565(4) 0.8969(3) 0.1671(4) 0.0304(6) Uani 1 1 d . . . O5 O 0.3093(4) 0.1315(4) 0.7237(4) 0.0289(5) Uani 1 1 d . . . H1W H 0.3348 0.1631 0.7992 0.043 Uiso 1 1 d . . . H2W H 0.1727 0.1272 0.7667 0.043 Uiso 1 1 d . . . N1 N 0.8053(4) 0.0939(3) 0.4514(4) 0.0153(5) Uani 1 1 d . . . N2 N 1.1647(4) 0.0860(3) 0.4371(4) 0.0148(5) Uani 1 1 d . . . C1 C 0.9694(4) 0.1782(4) 0.3912(5) 0.0140(5) Uani 1 1 d . . . C2 C 0.9365(5) 0.3792(4) 0.2680(5) 0.0230(7) Uani 1 1 d . . . H2A H 0.8203 0.4146 0.2106 0.035 Uiso 1 1 d R . . H2B H 1.0762 0.3930 0.1712 0.035 Uiso 1 1 d R . . H2C H 0.8925 0.4628 0.3410 0.035 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 0.01618(14) 0.02017(15) 0.02687(19) 0.00089(11) -0.00976(11) -0.00723(9) Cl1 0.0167(3) 0.0149(3) 0.0179(4) -0.0063(3) -0.0042(3) -0.0025(2) O1 0.0506(15) 0.0218(11) 0.0213(17) -0.0002(10) -0.0091(13) -0.0066(11) O2 0.0176(10) 0.0380(13) 0.0399(18) -0.0148(12) -0.0040(11) -0.0087(9) O3 0.0371(13) 0.0327(12) 0.0302(16) -0.0126(11) -0.0136(12) -0.0114(10) O4 0.0243(11) 0.0243(11) 0.0331(17) -0.0143(11) -0.0042(11) 0.0038(9) O5 0.0220(11) 0.0421(14) 0.0268(16) -0.0135(12) -0.0049(11) -0.0120(10) N1 0.0126(10) 0.0141(10) 0.0171(15) -0.0034(9) -0.0055(10) -0.0020(8) N2 0.0116(9) 0.0142(10) 0.0180(15) -0.0049(9) -0.0051(10) -0.0022(8) C1 0.0126(11) 0.0147(11) 0.0141(15) -0.0042(10) -0.0050(11) -0.0024(9) C2 0.0195(13) 0.0168(13) 0.030(2) 0.0007(12) -0.0119(14) -0.0055(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N2 2.375(2) 1_455 ? Ag1 N1 2.431(2) . ? Ag1 O1 2.507(2) . ? Ag1 O3 2.590(3) 2_665 ? Ag1 Ag1 3.2579(7) 2_656 ? Cl1 O2 1.433(2) . ? Cl1 O4 1.437(2) . ? Cl1 O1 1.444(3) . ? Cl1 O3 1.446(2) . ? O5 H1W 0.8507 . ? O5 H2W 0.8508 . ? N1 N2 1.326(3) 2_756 ? N1 C1 1.342(3) . ? N2 N1 1.326(3) 2_756 ? N2 C1 1.345(3) . ? C1 C2 1.479(4) . ? C2 H2A 0.9621 . ? C2 H2B 0.9594 . ? C2 H2C 0.9560 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ag1 N1 132.50(8) 1_455 . ? N2 Ag1 O1 110.79(9) 1_455 . ? N1 Ag1 O1 108.29(9) . . ? N2 Ag1 O3 122.70(8) 1_455 2_665 ? N1 Ag1 O3 87.87(8) . 2_665 ? O1 Ag1 O3 82.65(9) . 2_665 ? N2 Ag1 Ag1 66.89(6) 1_455 2_656 ? N1 Ag1 Ag1 65.66(6) . 2_656 ? O1 Ag1 Ag1 148.48(7) . 2_656 ? O3 Ag1 Ag1 126.22(6) 2_665 2_656 ? O2 Cl1 O4 109.59(15) . . ? O2 Cl1 O1 109.80(18) . . ? O4 Cl1 O1 109.05(17) . . ? O2 Cl1 O3 109.47(17) . . ? O4 Cl1 O3 109.12(15) . . ? O1 Cl1 O3 109.80(16) . . ? Cl1 O1 Ag1 130.36(17) . . ? Cl1 O3 Ag1 114.28(14) . 2_665 ? H1W O5 H2W 108.5 . . ? N2 N1 C1 118.7(2) 2_756 . ? N2 N1 Ag1 112.93(16) 2_756 . ? C1 N1 Ag1 127.88(19) . . ? N1 N2 C1 118.8(2) 2_756 . ? N1 N2 Ag1 114.31(15) 2_756 1_655 ? C1 N2 Ag1 126.83(19) . 1_655 ? N1 C1 N2 122.5(3) . . ? N1 C1 C2 119.1(2) . . ? N2 C1 C2 118.5(2) . . ? C1 C2 H2A 110.4 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.8 . . ? H2A C2 H2C 108.8 . . ? H2B C2 H2C 109.0 . . ? 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 O2 Cl1 O1 Ag1 -81.1(2) . . . . ? O4 Cl1 O1 Ag1 158.79(19) . . . . ? O3 Cl1 O1 Ag1 39.3(3) . . . . ? N2 Ag1 O1 Cl1 -100.6(2) 1_455 . . . ? N1 Ag1 O1 Cl1 107.0(2) . . . . ? O3 Ag1 O1 Cl1 21.7(2) 2_665 . . . ? Ag1 Ag1 O1 Cl1 -179.96(11) 2_656 . . . ? O2 Cl1 O3 Ag1 -18.24(18) . . . 2_665 ? O4 Cl1 O3 Ag1 101.68(16) . . . 2_665 ? O1 Cl1 O3 Ag1 -138.85(16) . . . 2_665 ? N2 Ag1 N1 N2 6.3(3) 1_455 . . 2_756 ? O1 Ag1 N1 N2 150.45(18) . . . 2_756 ? O3 Ag1 N1 N2 -128.01(19) 2_665 . . 2_756 ? Ag1 Ag1 N1 N2 3.74(16) 2_656 . . 2_756 ? N2 Ag1 N1 C1 178.6(2) 1_455 . . . ? O1 Ag1 N1 C1 -37.3(3) . . . . ? O3 Ag1 N1 C1 44.2(2) 2_665 . . . ? Ag1 Ag1 N1 C1 176.0(3) 2_656 . . . ? N2 N1 C1 N2 1.2(5) 2_756 . . . ? Ag1 N1 C1 N2 -170.6(2) . . . . ? N2 N1 C1 C2 -179.6(3) 2_756 . . . ? Ag1 N1 C1 C2 8.6(4) . . . . ? N1 N2 C1 N1 -1.2(5) 2_756 . . . ? Ag1 N2 C1 N1 -177.8(2) 1_655 . . . ? N1 N2 C1 C2 179.6(3) 2_756 . . . ? Ag1 N2 C1 C2 3.0(4) 1_655 . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.01 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.209 _refine_diff_density_min -1.190 _refine_diff_density_rms 0.166 #============================================================================== data_(5) _database_code_depnum_ccdc_archive 'CCDC 679096' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Silver(I) Triflate 3:1 complex with 2,6-dimethyl-1,2,4,5-tetrazine, dihydrate ; _chemical_name_common ;Silver(i) Triflate 3:1 complex with 2,6-dimethyl-1,2,4,5- tetrazine, dihydrate ; _chemical_melting_point ? _chemical_formula_moiety '2(C4 H6 N4), 6Ag, 6(C F3 O3 S), 4(H2 O)' _chemical_formula_sum 'C14 H20 Ag6 F18 N8 O22 S6' _chemical_formula_weight 1833.96 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'P 21/c' _space_group_name_Hall '-P 2ybc ' _symmetry_Int_Tables_number 14 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 10.5847(9) _cell_length_b 19.0579(13) _cell_length_c 23.1327(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.038(10) _cell_angle_gamma 90.00 _cell_volume 4563.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 3.05 _cell_measurement_theta_max 25.68 _exptl_crystal_description prism _exptl_crystal_colour red-violet _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_diffrn 2.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 2.956 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6182 _exptl_absorpt_correction_T_max 0.6492 _exptl_absorpt_process_details 'X-RED and X-SHAPE, Stoe&Cie GmbH' _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 19171 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0707 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 25.68 _reflns_number_total 8501 _reflns_number_gt 5122 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.700.00 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.1284P)^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_number_reflns 8501 _refine_ls_number_parameters 671 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1213 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.2061 _refine_ls_wR_factor_gt 0.1867 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.006 _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 0.38349(8) 0.92526(4) 0.12783(4) 0.0269(2) Uani 1 1 d . . . Ag2 Ag 0.07130(9) 0.86340(5) 0.14239(4) 0.0370(3) Uani 1 1 d . . . Ag3 Ag -0.13077(8) 0.58301(4) 0.12314(4) 0.0295(2) Uani 1 1 d . . . Ag4 Ag -0.29755(9) 0.87089(5) 0.10983(4) 0.0388(3) Uani 1 1 d . . . Ag5 Ag 0.18571(10) 0.65204(5) 0.09535(4) 0.0381(3) Uani 1 1 d . . . Ag6 Ag 0.40602(13) 1.16018(6) 0.33581(6) 0.0584(4) Uani 1 1 d . . . C1 C 0.3372(11) 1.0434(6) 0.2275(5) 0.026(2) Uani 1 1 d . . . C2 C 0.4408(12) 1.0827(7) 0.2067(5) 0.035(3) Uani 1 1 d . . . H2A H 0.4986 1.0498 0.1934 0.053 Uiso 1 1 calc R . . H2B H 0.4891 1.1107 0.2389 0.053 Uiso 1 1 calc R . . H2C H 0.4024 1.1132 0.1742 0.053 Uiso 1 1 calc R . . C3 C 0.1529(11) 0.9774(6) 0.2639(5) 0.031(2) Uani 1 1 d . . . C4 C 0.0468(14) 0.9398(7) 0.2842(6) 0.042(3) Uani 1 1 d . . . H4A H -0.0174 0.9247 0.2502 0.063 Uiso 1 1 calc R . . H4B H 0.0070 0.9710 0.3083 0.063 Uiso 1 1 calc R . . H4C H 0.0817 0.8991 0.3073 0.063 Uiso 1 1 calc R . . C5 C -0.0919(11) 0.4670(5) 0.0180(5) 0.024(2) Uani 1 1 d . . . C6 C -0.1940(15) 0.4279(7) 0.0386(6) 0.043(3) Uani 1 1 d . . . H6A H -0.1946 0.3796 0.0253 0.064 Uiso 1 1 calc R . . H6B H -0.2771 0.4493 0.0227 0.064 Uiso 1 1 calc R . . H6C H -0.1777 0.4291 0.0815 0.064 Uiso 1 1 calc R . . C7 C -0.4059(9) 0.9670(5) -0.0178(4) 0.0155(19) Uani 1 1 d . . . C8 C -0.3033(13) 0.9292(6) -0.0400(5) 0.034(3) Uani 1 1 d . . . H8A H -0.2293 0.9224 -0.0078 0.051 Uiso 1 1 calc R . . H8B H -0.2776 0.9566 -0.0710 0.051 Uiso 1 1 calc R . . H8C H -0.3357 0.8840 -0.0556 0.051 Uiso 1 1 calc R . . C9 C 0.3350(17) 0.7602(9) 0.2830(6) 0.055(4) Uani 1 1 d . . . C10 C -0.0811(13) 0.7518(7) -0.0302(6) 0.039(3) Uani 1 1 d . . . C11 C -0.160(2) 1.0784(9) 0.1443(9) 0.071(5) Uani 1 1 d . . . C12 C -0.5624(16) 0.7594(9) -0.0276(7) 0.053(4) Uani 1 1 d . . . C13 C 0.326(2) 0.4116(10) 0.1021(10) 0.081(6) Uani 1 1 d . . . C14 C 0.1397(15) 1.2556(8) 0.2126(6) 0.047(3) Uani 1 1 d . . . N1 N 0.2912(9) 0.9835(5) 0.2005(4) 0.0229(18) Uani 1 1 d . . . N2 N 0.1953(9) 0.9506(5) 0.2178(4) 0.027(2) Uani 1 1 d . . . N3 N 0.2953(9) 1.0695(5) 0.2748(4) 0.028(2) Uani 1 1 d . . . N4 N 0.2022(9) 1.0351(5) 0.2934(4) 0.027(2) Uani 1 1 d . . . N5 N -0.0409(9) 0.5247(5) 0.0479(4) 0.0249(19) Uani 1 1 d . . . N6 N 0.0516(9) 0.5584(4) 0.0298(4) 0.0237(19) Uani 1 1 d . . . N7 N -0.4346(9) 0.9472(4) 0.0335(4) 0.0254(19) Uani 1 1 d . . . N8 N -0.5295(9) 0.9805(5) 0.0517(4) 0.0242(19) Uani 1 1 d . . . O1 O 0.3036(9) 0.8145(5) 0.1780(4) 0.049(2) Uani 1 1 d . . . O2 O 0.358(2) 0.6903(6) 0.1922(5) 0.118(7) Uani 1 1 d . . . O3 O 0.5154(11) 0.7702(9) 0.2274(7) 0.096(5) Uani 1 1 d . . . O4 O 0.0261(8) 0.7458(5) 0.0817(4) 0.040(2) Uani 1 1 d . . . O5 O -0.1794(11) 0.8054(5) 0.0520(4) 0.052(3) Uani 1 1 d . . . O6 O -0.1688(9) 0.6779(4) 0.0464(4) 0.038(2) Uani 1 1 d . . . O7 O -0.1061(10) 0.9527(4) 0.1235(4) 0.048(2) Uani 1 1 d . . . O8 O 0.0532(10) 1.0439(6) 0.1179(7) 0.074(4) Uani 1 1 d . . . O9 O -0.1394(14) 1.0363(7) 0.0427(5) 0.076(4) Uani 1 1 d . . . O10 O -0.5211(10) 0.8119(5) 0.0783(4) 0.048(2) Uani 1 1 d . . . O11 O -0.5160(15) 0.6855(6) 0.0660(5) 0.074(4) Uani 1 1 d . . . O12 O -0.7180(11) 0.7463(6) 0.0416(5) 0.063(3) Uani 1 1 d . . . O13 O 0.3472(16) 0.5478(6) 0.1128(6) 0.080(4) Uani 1 1 d . . . O14 O 0.5125(13) 0.4793(9) 0.1690(7) 0.096(5) Uani 1 1 d . . . O15 O 0.3140(14) 0.4880(8) 0.1982(5) 0.080(4) Uani 1 1 d . . . O16 O 0.2497(12) 1.2562(7) 0.3234(5) 0.070(3) Uani 1 1 d . . . O17 O 0.0652(12) 1.1818(5) 0.2933(5) 0.062(3) Uani 1 1 d . . . O18 O 0.0415(16) 1.3063(7) 0.2951(5) 0.083(4) Uani 1 1 d . . . O19 O 0.6012(10) 0.9037(6) 0.1927(4) 0.050(2) Uani 1 1 d . . . H19A H 0.6027 0.8697 0.2168 0.075 Uiso 1 1 d . . . H19B H 0.6351 0.9399 0.2111 0.075 Uiso 1 1 d . . . O20 O 0.1805(10) 0.8872(5) 0.0632(4) 0.047(2) Uani 1 1 d . . . H20A H 0.1893 0.8498 0.0432 0.070 Uiso 1 1 d . . . H20B H 0.1456 0.9191 0.0386 0.070 Uiso 1 1 d . . . O21 O 0.1049(10) 0.5932(6) 0.1739(4) 0.059(3) Uani 1 1 d . . . H21A H 0.1409 0.5532 0.1829 0.088 Uiso 1 1 d . . . H21B H 0.1161 0.6181 0.2058 0.088 Uiso 1 1 d . . . O22 O -0.3647(13) 0.5662(8) 0.0778(6) 0.084(4) Uani 1 1 d . . . H22A H -0.3907 0.5246 0.0763 0.126 Uiso 1 1 d . . . H22B H -0.3851 0.5834 0.0409 0.126 Uiso 1 1 d . . . F1 F 0.2191(15) 0.7421(14) 0.2784(9) 0.161(9) Uani 1 1 d . . . F2 F 0.4083(14) 0.7216(7) 0.3216(4) 0.106(5) Uani 1 1 d . . . F3 F 0.335(2) 0.8224(8) 0.3043(4) 0.152(9) Uani 1 1 d . . . F4 F -0.0220(11) 0.8121(5) -0.0371(4) 0.072(3) Uani 1 1 d . . . F5 F -0.1924(8) 0.7534(4) -0.0687(3) 0.052(2) Uani 1 1 d . . . F6 F -0.0115(9) 0.6994(5) -0.0437(3) 0.059(2) Uani 1 1 d . . . F7 F -0.109(2) 1.0738(7) 0.2001(5) 0.130(6) Uani 1 1 d . . . F8 F -0.2888(13) 1.0599(7) 0.1354(7) 0.107(4) Uani 1 1 d . . . F9 F -0.1506(11) 1.1455(4) 0.1271(5) 0.081(3) Uani 1 1 d . . . F10 F -0.4402(11) 0.7573(8) -0.0303(5) 0.097(4) Uani 1 1 d . . . F11 F -0.6274(14) 0.7107(7) -0.0627(4) 0.105(5) Uani 1 1 d . . . F12 F -0.5973(15) 0.8200(6) -0.0500(4) 0.098(4) Uani 1 1 d . . . F13 F 0.368(2) 0.4147(9) 0.0555(7) 0.145(7) Uani 1 1 d . . . F14 F 0.3583(13) 0.3549(5) 0.1302(6) 0.093(4) Uani 1 1 d . . . F15 F 0.1936(14) 0.4137(7) 0.0873(8) 0.130(7) Uani 1 1 d . . . F16 F 0.1906(13) 1.3193(7) 0.2039(5) 0.088(3) Uani 1 1 d . . . F17 F 0.2155(12) 1.2095(6) 0.1983(4) 0.079(3) Uani 1 1 d . . . F18 F 0.0313(11) 1.2601(6) 0.1754(4) 0.078(3) Uani 1 1 d . . . S1 S 0.3763(3) 0.75897(15) 0.21156(11) 0.0298(6) Uani 1 1 d . . . S2 S -0.1042(3) 0.74399(14) 0.04523(12) 0.0270(6) Uani 1 1 d . . . S3 S -0.0778(4) 1.02143(17) 0.10120(15) 0.0432(8) Uani 1 1 d . . . S4 S -0.5857(3) 0.75178(15) 0.04670(12) 0.0335(7) Uani 1 1 d . . . S5 S 0.3735(5) 0.49005(19) 0.15068(18) 0.0566(10) Uani 1 1 d . . . S6 S 0.1227(3) 1.24996(15) 0.28936(12) 0.0323(7) 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 0.0344(5) 0.0256(4) 0.0244(4) 0.0025(3) 0.0146(3) 0.0018(4) Ag2 0.0308(5) 0.0375(5) 0.0413(5) -0.0142(4) 0.0039(4) -0.0013(4) Ag3 0.0353(5) 0.0325(4) 0.0245(4) -0.0004(3) 0.0152(3) -0.0010(4) Ag4 0.0347(5) 0.0439(6) 0.0400(5) 0.0119(4) 0.0124(4) 0.0137(4) Ag5 0.0428(6) 0.0313(5) 0.0403(5) -0.0022(4) 0.0092(4) -0.0016(4) Ag6 0.0654(8) 0.0492(7) 0.0660(7) -0.0282(6) 0.0262(6) -0.0327(6) C1 0.025(6) 0.026(6) 0.027(5) 0.000(4) 0.003(4) -0.002(4) C2 0.034(6) 0.040(7) 0.035(6) -0.011(5) 0.016(5) -0.014(5) C3 0.033(6) 0.034(6) 0.027(6) -0.002(5) 0.010(5) -0.001(5) C4 0.048(8) 0.041(7) 0.040(7) -0.015(6) 0.017(6) -0.015(6) C5 0.028(6) 0.020(5) 0.028(5) 0.004(4) 0.013(4) 0.003(4) C6 0.061(9) 0.034(7) 0.041(7) -0.015(6) 0.028(6) -0.015(6) C7 0.018(5) 0.014(4) 0.015(4) 0.000(3) 0.004(4) 0.000(4) C8 0.046(7) 0.027(6) 0.034(6) 0.011(5) 0.020(5) 0.015(5) C9 0.066(11) 0.071(11) 0.031(7) 0.010(7) 0.015(7) 0.024(9) C10 0.037(7) 0.046(7) 0.037(7) 0.004(6) 0.016(5) -0.002(6) C11 0.088(14) 0.043(9) 0.074(12) 0.006(8) 0.000(10) -0.001(9) C12 0.054(9) 0.062(10) 0.046(8) -0.011(7) 0.016(7) -0.015(8) C13 0.094(15) 0.066(12) 0.071(12) 0.036(10) -0.007(11) 0.022(11) C14 0.055(9) 0.056(9) 0.036(7) 0.003(6) 0.022(6) -0.002(7) N1 0.025(5) 0.027(5) 0.019(4) -0.008(4) 0.011(3) -0.005(4) N2 0.027(5) 0.029(5) 0.024(4) -0.005(4) 0.008(4) 0.006(4) N3 0.033(5) 0.027(5) 0.026(5) -0.005(4) 0.012(4) -0.008(4) N4 0.031(5) 0.024(5) 0.027(5) -0.014(4) 0.007(4) -0.004(4) N5 0.034(5) 0.023(4) 0.021(4) -0.004(3) 0.014(4) -0.007(4) N6 0.035(5) 0.016(4) 0.022(4) -0.003(3) 0.010(4) 0.004(4) N7 0.030(5) 0.018(4) 0.031(5) 0.009(4) 0.012(4) 0.004(4) N8 0.025(5) 0.024(5) 0.027(4) 0.004(4) 0.011(4) 0.010(4) O1 0.046(6) 0.051(6) 0.051(5) 0.016(4) 0.008(4) 0.012(4) O2 0.27(2) 0.025(5) 0.041(6) -0.009(5) -0.007(9) 0.047(9) O3 0.031(6) 0.133(13) 0.127(11) 0.079(10) 0.024(6) 0.023(7) O4 0.038(5) 0.036(5) 0.040(5) 0.000(4) -0.005(4) 0.003(4) O5 0.087(8) 0.030(5) 0.045(5) 0.011(4) 0.030(5) 0.029(5) O6 0.044(5) 0.029(4) 0.038(4) 0.007(3) 0.003(4) -0.005(4) O7 0.054(6) 0.024(4) 0.061(6) 0.007(4) 0.000(5) 0.003(4) O8 0.032(5) 0.068(7) 0.124(10) 0.020(7) 0.023(6) -0.008(5) O9 0.113(11) 0.079(8) 0.034(5) 0.008(5) 0.009(6) -0.013(7) O10 0.049(6) 0.044(5) 0.050(5) -0.004(4) 0.010(4) -0.005(4) O11 0.124(11) 0.041(6) 0.057(6) 0.002(5) 0.019(7) 0.030(6) O12 0.059(7) 0.065(7) 0.066(7) -0.007(6) 0.013(5) -0.012(6) O13 0.126(11) 0.034(5) 0.094(9) 0.017(6) 0.055(8) 0.010(6) O14 0.049(7) 0.119(12) 0.119(11) -0.042(10) 0.013(7) -0.032(8) O15 0.098(10) 0.084(9) 0.063(7) -0.003(7) 0.028(7) -0.009(8) O16 0.062(7) 0.077(8) 0.066(7) -0.013(6) 0.003(6) -0.007(6) O17 0.079(8) 0.034(5) 0.074(7) 0.018(5) 0.019(6) -0.007(5) O18 0.137(12) 0.068(8) 0.059(7) 0.006(6) 0.050(7) 0.039(8) O19 0.049(6) 0.059(6) 0.042(5) -0.001(5) 0.009(4) 0.009(5) O20 0.057(6) 0.047(5) 0.031(4) 0.000(4) -0.003(4) -0.017(5) O21 0.056(6) 0.082(8) 0.038(5) 0.000(5) 0.009(4) -0.020(6) O22 0.064(8) 0.122(12) 0.065(7) -0.023(8) 0.013(6) 0.019(8) F1 0.073(9) 0.25(2) 0.168(15) 0.117(17) 0.055(9) 0.022(12) F2 0.159(12) 0.121(9) 0.040(5) 0.037(5) 0.024(6) 0.108(9) F3 0.29(2) 0.122(11) 0.038(5) 0.003(6) 0.024(8) 0.146(15) F4 0.106(8) 0.061(6) 0.055(5) 0.007(4) 0.027(5) -0.042(6) F5 0.062(5) 0.057(5) 0.034(4) 0.000(4) -0.001(4) 0.006(4) F6 0.072(6) 0.072(6) 0.040(4) -0.005(4) 0.025(4) 0.024(5) F7 0.242(19) 0.101(9) 0.039(6) -0.024(6) 0.010(8) 0.029(10) F8 0.078(8) 0.094(9) 0.167(13) -0.003(9) 0.069(8) 0.007(7) F9 0.088(8) 0.029(4) 0.117(9) -0.005(5) -0.002(6) 0.007(4) F10 0.064(7) 0.149(11) 0.092(8) -0.053(8) 0.046(6) -0.032(7) F11 0.148(11) 0.131(10) 0.047(5) -0.041(6) 0.047(6) -0.089(9) F12 0.158(12) 0.073(7) 0.051(6) 0.026(5) -0.007(6) -0.036(7) F13 0.25(2) 0.112(12) 0.078(9) -0.041(8) 0.043(11) -0.034(12) F14 0.112(10) 0.036(5) 0.121(10) 0.006(5) -0.001(8) -0.010(5) F15 0.093(10) 0.082(8) 0.173(14) 0.008(9) -0.070(10) -0.021(7) F16 0.098(9) 0.094(8) 0.080(7) 0.014(6) 0.035(6) -0.021(7) F17 0.100(8) 0.095(8) 0.048(5) 0.011(5) 0.029(5) 0.049(7) F18 0.094(8) 0.085(7) 0.043(5) 0.006(5) -0.014(5) 0.024(6) S1 0.0432(17) 0.0250(14) 0.0217(13) 0.0025(10) 0.0080(11) 0.0116(12) S2 0.0357(16) 0.0186(13) 0.0269(13) -0.0019(10) 0.0068(11) 0.0034(11) S3 0.053(2) 0.0327(16) 0.0436(18) 0.0081(14) 0.0096(15) 0.0038(15) S4 0.0499(19) 0.0248(14) 0.0279(14) 0.0011(11) 0.0131(13) -0.0077(13) S5 0.076(3) 0.0354(18) 0.057(2) -0.0049(16) 0.0108(19) -0.0078(18) S6 0.0490(18) 0.0253(14) 0.0245(13) -0.0048(11) 0.0121(12) -0.0018(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.386(8) . ? Ag1 N8 2.395(9) 1_655 ? Ag1 O20 2.457(9) . ? Ag1 O19 2.508(9) . ? Ag2 O18 2.330(12) 2_545 ? Ag2 O20 2.405(10) . ? Ag2 O7 2.504(9) . ? Ag2 N2 2.565(9) . ? Ag2 O1 2.597(9) . ? Ag3 N4 2.396(9) 2_545 ? Ag3 N5 2.421(9) . ? Ag3 O22 2.500(13) . ? Ag3 O6 2.507(8) . ? Ag3 O21 2.533(10) . ? Ag4 O5 2.368(9) . ? Ag4 O19 2.464(10) 1_455 ? Ag4 N7 2.504(8) . ? Ag4 O7 2.524(10) . ? Ag4 O10 2.584(10) . ? Ag5 O4 2.434(9) . ? Ag5 O21 2.436(10) . ? Ag5 O12 2.518(12) 1_655 ? Ag5 N6 2.570(9) . ? Ag5 O13 2.597(13) . ? Ag6 O11 2.376(12) 2 ? Ag6 N3 2.379(9) . ? Ag6 O16 2.443(13) . ? C1 N1 1.344(14) . ? C1 N3 1.357(15) . ? C1 C2 1.488(16) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 H2C 0.9700 . ? C3 N2 1.340(15) . ? C3 N4 1.342(14) . ? C3 C4 1.488(18) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 N5 1.350(14) . ? C5 N6 1.355(14) 3_565 ? C5 C6 1.472(17) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C7 N7 1.340(13) . ? C7 N8 1.363(12) 3_475 ? C7 C8 1.481(15) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 H8C 0.9700 . ? C9 F1 1.26(2) . ? C9 F3 1.28(2) . ? C9 F2 1.286(16) . ? C9 S1 1.795(15) . ? C10 F6 1.317(16) . ? C10 F5 1.322(15) . ? C10 F4 1.334(16) . ? C10 S2 1.817(13) . ? C11 F7 1.29(2) . ? C11 F9 1.349(19) . ? C11 F8 1.38(2) . ? C11 S3 1.81(2) . ? C12 F12 1.29(2) . ? C12 F10 1.307(19) . ? C12 F11 1.327(17) . ? C12 S4 1.794(16) . ? C13 F13 1.25(3) . ? C13 F14 1.270(19) . ? C13 F15 1.37(3) . ? C13 S5 1.87(2) . ? C14 F17 1.279(18) . ? C14 F18 1.286(18) . ? C14 F16 1.360(18) . ? C14 S6 1.825(14) . ? N1 N2 1.325(13) . ? N3 N4 1.328(13) . ? N4 Ag3 2.396(9) 2 ? N5 N6 1.310(13) . ? N6 C5 1.355(14) 3_565 ? N7 N8 1.329(12) . ? N8 C7 1.363(12) 3_475 ? N8 Ag1 2.395(9) 1_455 ? O1 S1 1.437(9) . ? O2 S1 1.384(11) . ? O3 S1 1.456(12) . ? O4 S2 1.460(9) . ? O5 S2 1.442(9) . ? O6 S2 1.436(8) . ? O7 S3 1.462(9) . ? O8 S3 1.426(11) . ? O9 S3 1.402(11) . ? O10 S4 1.451(10) . ? O11 S4 1.484(11) . ? O11 Ag6 2.376(12) 2_545 ? O12 S4 1.384(12) . ? O12 Ag5 2.518(12) 1_455 ? O13 S5 1.399(12) . ? O14 S5 1.458(14) . ? O15 S5 1.377(14) . ? O16 S6 1.414(12) . ? O17 S6 1.445(10) . ? O18 S6 1.398(13) . ? O18 Ag2 2.330(12) 2 ? O19 Ag4 2.464(10) 1_655 ? O19 H19A 0.8532 . ? O19 H19B 0.8504 . ? O20 H20A 0.8650 . ? O20 H20B 0.8605 . ? O21 H21A 0.8583 . ? O21 H21B 0.8640 . ? O22 H22A 0.8372 . ? O22 H22B 0.8971 . ? 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 N8 126.2(3) . 1_655 ? N1 Ag1 O20 97.6(3) . . ? N8 Ag1 O20 95.9(3) 1_655 . ? N1 Ag1 O19 96.6(3) . . ? N8 Ag1 O19 93.8(3) 1_655 . ? O20 Ag1 O19 153.3(3) . . ? O18 Ag2 O20 162.1(4) 2_545 . ? O18 Ag2 O7 87.9(5) 2_545 . ? O20 Ag2 O7 101.6(3) . . ? O18 Ag2 N2 97.8(4) 2_545 . ? O20 Ag2 N2 97.9(3) . . ? O7 Ag2 N2 86.4(3) . . ? O18 Ag2 O1 102.1(5) 2_545 . ? O20 Ag2 O1 74.7(3) . . ? O7 Ag2 O1 157.7(3) . . ? N2 Ag2 O1 72.6(3) . . ? N4 Ag3 N5 129.9(3) 2_545 . ? N4 Ag3 O22 80.7(4) 2_545 . ? N5 Ag3 O22 98.2(4) . . ? N4 Ag3 O6 144.5(3) 2_545 . ? N5 Ag3 O6 81.4(3) . . ? O22 Ag3 O6 78.2(4) . . ? N4 Ag3 O21 95.8(3) 2_545 . ? N5 Ag3 O21 82.6(3) . . ? O22 Ag3 O21 176.1(5) . . ? O6 Ag3 O21 105.6(3) . . ? O5 Ag4 O19 160.0(3) . 1_455 ? O5 Ag4 N7 101.8(3) . . ? O19 Ag4 N7 96.9(3) 1_455 . ? O5 Ag4 O7 83.8(4) . . ? O19 Ag4 O7 102.4(3) 1_455 . ? N7 Ag4 O7 93.5(3) . . ? O5 Ag4 O10 99.9(4) . . ? O19 Ag4 O10 79.0(3) 1_455 . ? N7 Ag4 O10 72.1(3) . . ? O7 Ag4 O10 165.6(3) . . ? O4 Ag5 O21 95.3(4) . . ? O4 Ag5 O12 75.8(4) . 1_655 ? O21 Ag5 O12 159.7(4) . 1_655 ? O4 Ag5 N6 98.6(3) . . ? O21 Ag5 N6 83.3(3) . . ? O12 Ag5 N6 115.8(3) 1_655 . ? O4 Ag5 O13 176.7(4) . . ? O21 Ag5 O13 81.6(4) . . ? O12 Ag5 O13 107.5(4) 1_655 . ? N6 Ag5 O13 79.9(4) . . ? O11 Ag6 N3 142.8(3) 2 . ? O11 Ag6 O16 98.4(4) 2 . ? N3 Ag6 O16 103.7(4) . . ? N1 C1 N3 122.6(10) . . ? N1 C1 C2 119.8(10) . . ? N3 C1 C2 117.6(10) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 N4 123.8(11) . . ? N2 C3 C4 117.9(10) . . ? N4 C3 C4 118.3(10) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N5 C5 N6 123.2(10) . 3_565 ? N5 C5 C6 119.3(10) . . ? N6 C5 C6 117.4(10) 3_565 . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N7 C7 N8 122.5(9) . 3_475 ? N7 C7 C8 119.1(9) . . ? N8 C7 C8 118.4(9) 3_475 . ? 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 . . ? F1 C9 F3 102.0(19) . . ? F1 C9 F2 109.8(16) . . ? F3 C9 F2 108.0(14) . . ? F1 C9 S1 109.9(14) . . ? F3 C9 S1 112.6(13) . . ? F2 C9 S1 113.9(12) . . ? F6 C10 F5 108.7(11) . . ? F6 C10 F4 109.0(11) . . ? F5 C10 F4 105.9(11) . . ? F6 C10 S2 111.1(9) . . ? F5 C10 S2 111.7(9) . . ? F4 C10 S2 110.3(9) . . ? F7 C11 F9 108.5(15) . . ? F7 C11 F8 109(2) . . ? F9 C11 F8 109.1(15) . . ? F7 C11 S3 111.4(14) . . ? F9 C11 S3 109.6(15) . . ? F8 C11 S3 109.7(12) . . ? F12 C12 F10 102.2(15) . . ? F12 C12 F11 108.2(14) . . ? F10 C12 F11 110.0(14) . . ? F12 C12 S4 111.9(12) . . ? F10 C12 S4 112.2(11) . . ? F11 C12 S4 111.9(11) . . ? F13 C13 F14 112(2) . . ? F13 C13 F15 108.2(18) . . ? F14 C13 F15 107.7(18) . . ? F13 C13 S5 112.3(16) . . ? F14 C13 S5 111.2(14) . . ? F15 C13 S5 105.1(16) . . ? F17 C14 F18 113.1(13) . . ? F17 C14 F16 106.5(13) . . ? F18 C14 F16 99.6(12) . . ? F17 C14 S6 114.0(10) . . ? F18 C14 S6 113.5(11) . . ? F16 C14 S6 108.6(10) . . ? N2 N1 C1 119.1(9) . . ? N2 N1 Ag1 116.5(6) . . ? C1 N1 Ag1 124.1(7) . . ? N1 N2 C3 117.8(9) . . ? N1 N2 Ag2 114.6(6) . . ? C3 N2 Ag2 125.4(8) . . ? N4 N3 C1 118.0(9) . . ? N4 N3 Ag6 118.2(6) . . ? C1 N3 Ag6 122.7(7) . . ? N3 N4 C3 118.4(9) . . ? N3 N4 Ag3 117.0(6) . 2 ? C3 N4 Ag3 124.6(8) . 2 ? N6 N5 C5 118.8(9) . . ? N6 N5 Ag3 115.9(6) . . ? C5 N5 Ag3 124.5(7) . . ? N5 N6 C5 118.0(8) . 3_565 ? N5 N6 Ag5 120.6(6) . . ? C5 N6 Ag5 120.1(7) 3_565 . ? N8 N7 C7 118.1(8) . . ? N8 N7 Ag4 114.8(6) . . ? C7 N7 Ag4 125.8(7) . . ? N7 N8 C7 119.4(8) . 3_475 ? N7 N8 Ag1 117.1(6) . 1_455 ? C7 N8 Ag1 121.4(7) 3_475 1_455 ? S1 O1 Ag2 143.2(6) . . ? S2 O4 Ag5 127.2(5) . . ? S2 O5 Ag4 149.0(6) . . ? S2 O6 Ag3 129.8(5) . . ? S3 O7 Ag2 118.0(6) . . ? S3 O7 Ag4 136.7(5) . . ? Ag2 O7 Ag4 98.9(3) . . ? S4 O10 Ag4 142.5(6) . . ? S4 O11 Ag6 125.0(6) . 2_545 ? S4 O12 Ag5 121.2(7) . 1_455 ? S5 O13 Ag5 137.5(8) . . ? S6 O16 Ag6 123.0(7) . . ? S6 O18 Ag2 145.3(8) . 2 ? Ag4 O19 Ag1 94.1(3) 1_655 . ? Ag4 O19 H19A 111.3 1_655 . ? Ag1 O19 H19A 113.9 . . ? Ag4 O19 H19B 113.0 1_655 . ? Ag1 O19 H19B 114.0 . . ? H19A O19 H19B 109.9 . . ? Ag2 O20 Ag1 95.2(3) . . ? Ag2 O20 H20A 111.9 . . ? Ag1 O20 H20A 113.0 . . ? Ag2 O20 H20B 115.4 . . ? Ag1 O20 H20B 113.2 . . ? H20A O20 H20B 107.9 . . ? Ag5 O21 Ag3 98.9(3) . . ? Ag5 O21 H21A 112.6 . . ? Ag3 O21 H21A 112.9 . . ? Ag5 O21 H21B 112.2 . . ? Ag3 O21 H21B 112.6 . . ? H21A O21 H21B 107.7 . . ? Ag3 O22 H22A 115.2 . . ? Ag3 O22 H22B 111.9 . . ? H22A O22 H22B 107.1 . . ? O2 S1 O1 119.8(7) . . ? O2 S1 O3 106.7(12) . . ? O1 S1 O3 115.3(7) . . ? O2 S1 C9 105.3(9) . . ? O1 S1 C9 106.3(7) . . ? O3 S1 C9 101.2(9) . . ? O6 S2 O5 115.7(6) . . ? O6 S2 O4 113.9(5) . . ? O5 S2 O4 113.2(6) . . ? O6 S2 C10 104.5(6) . . ? O5 S2 C10 103.0(6) . . ? O4 S2 C10 104.7(6) . . ? O9 S3 O8 115.5(8) . . ? O9 S3 O7 115.7(7) . . ? O8 S3 O7 115.6(6) . . ? O9 S3 C11 103.3(9) . . ? O8 S3 C11 102.8(9) . . ? O7 S3 C11 100.7(8) . . ? O12 S4 O10 117.7(7) . . ? O12 S4 O11 113.1(8) . . ? O10 S4 O11 111.6(7) . . ? O12 S4 C12 105.3(7) . . ? O10 S4 C12 105.9(7) . . ? O11 S4 C12 101.4(8) . . ? O15 S5 O13 117.3(9) . . ? O15 S5 O14 111.4(9) . . ? O13 S5 O14 110.5(10) . . ? O15 S5 C13 110.2(10) . . ? O13 S5 C13 105.0(8) . . ? O14 S5 C13 101.0(9) . . ? O18 S6 O16 114.5(9) . . ? O18 S6 O17 114.1(9) . . ? O16 S6 O17 113.9(7) . . ? O18 S6 C14 103.5(7) . . ? O16 S6 C14 105.2(8) . . ? O17 S6 C14 104.1(7) . . ? 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 N3 C1 N1 N2 4.6(15) . . . . ? C2 C1 N1 N2 -177.2(10) . . . . ? N3 C1 N1 Ag1 -169.6(8) . . . . ? C2 C1 N1 Ag1 8.6(14) . . . . ? N8 Ag1 N1 N2 146.8(7) 1_655 . . . ? O20 Ag1 N1 N2 43.7(7) . . . . ? O19 Ag1 N1 N2 -113.6(7) . . . . ? N8 Ag1 N1 C1 -38.9(9) 1_655 . . . ? O20 Ag1 N1 C1 -142.0(8) . . . . ? O19 Ag1 N1 C1 60.7(8) . . . . ? C1 N1 N2 C3 -3.2(14) . . . . ? Ag1 N1 N2 C3 171.4(8) . . . . ? C1 N1 N2 Ag2 160.7(7) . . . . ? Ag1 N1 N2 Ag2 -24.7(8) . . . . ? N4 C3 N2 N1 -0.3(16) . . . . ? C4 C3 N2 N1 -178.9(10) . . . . ? N4 C3 N2 Ag2 -162.3(8) . . . . ? C4 C3 N2 Ag2 19.2(15) . . . . ? O18 Ag2 N2 N1 166.9(8) 2_545 . . . ? O20 Ag2 N2 N1 -4.5(7) . . . . ? O7 Ag2 N2 N1 -105.7(7) . . . . ? O1 Ag2 N2 N1 66.6(7) . . . . ? O18 Ag2 N2 C3 -30.6(10) 2_545 . . . ? O20 Ag2 N2 C3 158.0(9) . . . . ? O7 Ag2 N2 C3 56.7(9) . . . . ? O1 Ag2 N2 C3 -130.9(9) . . . . ? N1 C1 N3 N4 -2.2(16) . . . . ? C2 C1 N3 N4 179.6(10) . . . . ? N1 C1 N3 Ag6 166.1(7) . . . . ? C2 C1 N3 Ag6 -12.2(14) . . . . ? O11 Ag6 N3 N4 50.5(12) 2 . . . ? O16 Ag6 N3 N4 -74.2(8) . . . . ? O11 Ag6 N3 C1 -117.8(10) 2 . . . ? O16 Ag6 N3 C1 117.6(9) . . . . ? C1 N3 N4 C3 -1.3(15) . . . . ? Ag6 N3 N4 C3 -170.2(8) . . . . ? C1 N3 N4 Ag3 -179.9(7) . . . 2 ? Ag6 N3 N4 Ag3 11.3(10) . . . 2 ? N2 C3 N4 N3 2.7(16) . . . . ? C4 C3 N4 N3 -178.8(11) . . . . ? N2 C3 N4 Ag3 -179.0(8) . . . 2 ? C4 C3 N4 Ag3 -0.4(15) . . . 2 ? N6 C5 N5 N6 0.5(17) 3_565 . . . ? C6 C5 N5 N6 178.8(10) . . . . ? N6 C5 N5 Ag3 169.7(7) 3_565 . . . ? C6 C5 N5 Ag3 -12.0(14) . . . . ? N4 Ag3 N5 N6 -142.4(7) 2_545 . . . ? O22 Ag3 N5 N6 132.9(8) . . . . ? O6 Ag3 N5 N6 56.2(7) . . . . ? O21 Ag3 N5 N6 -50.9(7) . . . . ? N4 Ag3 N5 C5 48.1(10) 2_545 . . . ? O22 Ag3 N5 C5 -36.6(9) . . . . ? O6 Ag3 N5 C5 -113.3(8) . . . . ? O21 Ag3 N5 C5 139.6(9) . . . . ? C5 N5 N6 C5 -0.4(16) . . . 3_565 ? Ag3 N5 N6 C5 -170.6(7) . . . 3_565 ? C5 N5 N6 Ag5 -167.1(7) . . . . ? Ag3 N5 N6 Ag5 22.7(9) . . . . ? O4 Ag5 N6 N5 -75.0(8) . . . . ? O21 Ag5 N6 N5 19.3(8) . . . . ? O12 Ag5 N6 N5 -153.3(7) 1_655 . . . ? O13 Ag5 N6 N5 102.0(8) . . . . ? O4 Ag5 N6 C5 118.6(8) . . . 3_565 ? O21 Ag5 N6 C5 -147.1(8) . . . 3_565 ? O12 Ag5 N6 C5 40.3(9) 1_655 . . 3_565 ? O13 Ag5 N6 C5 -64.4(8) . . . 3_565 ? N8 C7 N7 N8 -0.1(16) 3_475 . . . ? C8 C7 N7 N8 -178.1(10) . . . . ? N8 C7 N7 Ag4 -166.2(7) 3_475 . . . ? C8 C7 N7 Ag4 15.8(13) . . . . ? O5 Ag4 N7 N8 167.6(7) . . . . ? O19 Ag4 N7 N8 -5.1(7) 1_455 . . . ? O7 Ag4 N7 N8 -108.0(7) . . . . ? O10 Ag4 N7 N8 70.9(7) . . . . ? O5 Ag4 N7 C7 -25.9(9) . . . . ? O19 Ag4 N7 C7 161.4(8) 1_455 . . . ? O7 Ag4 N7 C7 58.5(8) . . . . ? O10 Ag4 N7 C7 -122.6(9) . . . . ? C7 N7 N8 C7 0.1(15) . . . 3_475 ? Ag4 N7 N8 C7 167.7(7) . . . 3_475 ? C7 N7 N8 Ag1 163.8(7) . . . 1_455 ? Ag4 N7 N8 Ag1 -28.6(9) . . . 1_455 ? O18 Ag2 O1 S1 16.9(11) 2_545 . . . ? O20 Ag2 O1 S1 -145.0(11) . . . . ? O7 Ag2 O1 S1 131.8(10) . . . . ? N2 Ag2 O1 S1 111.4(11) . . . . ? O21 Ag5 O4 S2 -84.9(7) . . . . ? O12 Ag5 O4 S2 113.7(7) 1_655 . . . ? N6 Ag5 O4 S2 -0.8(7) . . . . ? O19 Ag4 O5 S2 -1(2) 1_455 . . . ? N7 Ag4 O5 S2 -159.3(14) . . . . ? O7 Ag4 O5 S2 108.3(14) . . . . ? O10 Ag4 O5 S2 -85.8(14) . . . . ? N4 Ag3 O6 S2 97.8(8) 2_545 . . . ? N5 Ag3 O6 S2 -107.1(7) . . . . ? O22 Ag3 O6 S2 152.6(8) . . . . ? O21 Ag3 O6 S2 -27.3(8) . . . . ? O18 Ag2 O7 S3 159.2(7) 2_545 . . . ? O20 Ag2 O7 S3 -36.1(6) . . . . ? N2 Ag2 O7 S3 61.2(6) . . . . ? O1 Ag2 O7 S3 41.7(12) . . . . ? O18 Ag2 O7 Ag4 -44.2(4) 2_545 . . . ? O20 Ag2 O7 Ag4 120.5(3) . . . . ? N2 Ag2 O7 Ag4 -142.2(4) . . . . ? O1 Ag2 O7 Ag4 -161.7(7) . . . . ? O5 Ag4 O7 S3 105.4(9) . . . . ? O19 Ag4 O7 S3 -93.9(9) 1_455 . . . ? N7 Ag4 O7 S3 3.9(9) . . . . ? O10 Ag4 O7 S3 0(2) . . . . ? O5 Ag4 O7 Ag2 -43.9(3) . . . . ? O19 Ag4 O7 Ag2 116.8(4) 1_455 . . . ? N7 Ag4 O7 Ag2 -145.3(3) . . . . ? O10 Ag4 O7 Ag2 -149.5(12) . . . . ? O5 Ag4 O10 S4 11.4(10) . . . . ? O19 Ag4 O10 S4 -148.3(10) 1_455 . . . ? N7 Ag4 O10 S4 110.7(10) . . . . ? O7 Ag4 O10 S4 115.0(14) . . . . ? O4 Ag5 O13 S5 -23(8) . . . . ? O12 Ag5 O13 S5 158.9(12) 1_655 . . . ? N6 Ag5 O13 S5 -87.1(13) . . . . ? O11 Ag6 O16 S6 -146.2(9) 2 . . . ? N3 Ag6 O16 S6 3.7(10) . . . . ? N1 Ag1 O19 Ag4 -167.2(3) . . . 1_655 ? N8 Ag1 O19 Ag4 -40.1(4) 1_655 . . 1_655 ? O20 Ag1 O19 Ag4 71.1(8) . . . 1_655 ? O18 Ag2 O20 Ag1 -123.9(15) 2_545 . . . ? O7 Ag2 O20 Ag1 115.2(3) . . . . ? N2 Ag2 O20 Ag1 27.4(4) . . . . ? O1 Ag2 O20 Ag1 -42.1(3) . . . . ? N1 Ag1 O20 Ag2 -36.6(4) . . . . ? N8 Ag1 O20 Ag2 -164.3(3) 1_655 . . . ? O19 Ag1 O20 Ag2 85.0(8) . . . . ? O4 Ag5 O21 Ag3 51.8(4) . . . . ? O12 Ag5 O21 Ag3 114.4(10) 1_655 . . . ? N6 Ag5 O21 Ag3 -46.3(4) . . . . ? O13 Ag5 O21 Ag3 -127.0(5) . . . . ? N4 Ag3 O21 Ag5 -175.0(4) 2_545 . . . ? N5 Ag3 O21 Ag5 55.4(4) . . . . ? O6 Ag3 O21 Ag5 -23.6(5) . . . . ? Ag2 O1 S1 O2 64.6(15) . . . . ? Ag2 O1 S1 O3 -165.7(11) . . . . ? Ag2 O1 S1 C9 -54.4(12) . . . . ? F1 C9 S1 O2 -60.5(17) . . . . ? F3 C9 S1 O2 -173.5(16) . . . . ? F2 C9 S1 O2 63.1(18) . . . . ? F1 C9 S1 O1 67.7(16) . . . . ? F3 C9 S1 O1 -45.3(16) . . . . ? F2 C9 S1 O1 -168.7(14) . . . . ? F1 C9 S1 O3 -171.5(16) . . . . ? F3 C9 S1 O3 75.5(16) . . . . ? F2 C9 S1 O3 -47.9(16) . . . . ? Ag3 O6 S2 O5 -110.5(7) . . . . ? Ag3 O6 S2 O4 23.4(9) . . . . ? Ag3 O6 S2 C10 137.0(7) . . . . ? Ag4 O5 S2 O6 60.2(15) . . . . ? Ag4 O5 S2 O4 -73.9(15) . . . . ? Ag4 O5 S2 C10 173.6(13) . . . . ? Ag5 O4 S2 O6 38.4(9) . . . . ? Ag5 O4 S2 O5 173.4(6) . . . . ? Ag5 O4 S2 C10 -75.1(8) . . . . ? F6 C10 S2 O6 -59.5(10) . . . . ? F5 C10 S2 O6 62.1(10) . . . . ? F4 C10 S2 O6 179.6(10) . . . . ? F6 C10 S2 O5 179.2(10) . . . . ? F5 C10 S2 O5 -59.2(11) . . . . ? F4 C10 S2 O5 58.2(11) . . . . ? F6 C10 S2 O4 60.5(10) . . . . ? F5 C10 S2 O4 -177.9(9) . . . . ? F4 C10 S2 O4 -60.4(11) . . . . ? Ag2 O7 S3 O9 110.8(8) . . . . ? Ag4 O7 S3 O9 -34.3(12) . . . . ? Ag2 O7 S3 O8 -28.7(10) . . . . ? Ag4 O7 S3 O8 -173.8(9) . . . . ? Ag2 O7 S3 C11 -138.6(7) . . . . ? Ag4 O7 S3 C11 76.2(10) . . . . ? F7 C11 S3 O9 -176.7(15) . . . . ? F9 C11 S3 O9 -56.7(14) . . . . ? F8 C11 S3 O9 63.0(14) . . . . ? F7 C11 S3 O8 -56.2(16) . . . . ? F9 C11 S3 O8 63.8(13) . . . . ? F8 C11 S3 O8 -176.5(12) . . . . ? F7 C11 S3 O7 63.5(16) . . . . ? F9 C11 S3 O7 -176.5(11) . . . . ? F8 C11 S3 O7 -56.8(13) . . . . ? Ag5 O12 S4 O10 -110.9(7) 1_455 . . . ? Ag5 O12 S4 O11 21.6(10) 1_455 . . . ? Ag5 O12 S4 C12 131.4(8) 1_455 . . . ? Ag4 O10 S4 O12 -178.4(9) . . . . ? Ag4 O10 S4 O11 48.5(12) . . . . ? Ag4 O10 S4 C12 -61.0(11) . . . . ? Ag6 O11 S4 O12 -99.6(10) 2_545 . . . ? Ag6 O11 S4 O10 35.7(12) 2_545 . . . ? Ag6 O11 S4 C12 148.1(9) 2_545 . . . ? F12 C12 S4 O12 72.8(13) . . . . ? F10 C12 S4 O12 -173.0(12) . . . . ? F11 C12 S4 O12 -48.8(15) . . . . ? F12 C12 S4 O10 -52.6(13) . . . . ? F10 C12 S4 O10 61.6(14) . . . . ? F11 C12 S4 O10 -174.2(13) . . . . ? F12 C12 S4 O11 -169.2(12) . . . . ? F10 C12 S4 O11 -55.0(14) . . . . ? F11 C12 S4 O11 69.2(15) . . . . ? Ag5 O13 S5 O15 -11.1(17) . . . . ? Ag5 O13 S5 O14 -140.2(12) . . . . ? Ag5 O13 S5 C13 111.7(14) . . . . ? F13 C13 S5 O15 173.8(17) . . . . ? F14 C13 S5 O15 -59.9(19) . . . . ? F15 C13 S5 O15 56.3(15) . . . . ? F13 C13 S5 O13 46.6(19) . . . . ? F14 C13 S5 O13 172.9(17) . . . . ? F15 C13 S5 O13 -70.9(16) . . . . ? F13 C13 S5 O14 -68.3(18) . . . . ? F14 C13 S5 O14 58.0(19) . . . . ? F15 C13 S5 O14 174.2(14) . . . . ? Ag2 O18 S6 O16 -70(2) 2 . . . ? Ag2 O18 S6 O17 63(2) 2 . . . ? Ag2 O18 S6 C14 175.8(17) 2 . . . ? Ag6 O16 S6 O18 170.3(8) . . . . ? Ag6 O16 S6 O17 36.5(11) . . . . ? Ag6 O16 S6 C14 -76.7(9) . . . . ? F17 C14 S6 O18 177.5(13) . . . . ? F18 C14 S6 O18 -50.9(14) . . . . ? F16 C14 S6 O18 58.9(13) . . . . ? F17 C14 S6 O16 57.1(14) . . . . ? F18 C14 S6 O16 -171.4(11) . . . . ? F16 C14 S6 O16 -61.5(12) . . . . ? F17 C14 S6 O17 -62.9(14) . . . . ? F18 C14 S6 O17 68.6(13) . . . . ? F16 C14 S6 O17 178.5(11) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 3.255 _refine_diff_density_min -2.692 _refine_diff_density_rms 0.225 #============================================================================== data_(6) _database_code_depnum_ccdc_archive 'CCDC 705413' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Copper(I) chloride 4:1 complex with 3,6-dimethyl-1,2,4,5-tetrazine ; _chemical_name_common ;Copper(i) chloride 4:1 complex with 3,6-dimethyl-1,2,4,5- tetrazine ; _chemical_melting_point ? _chemical_formula_moiety 'C4H6N4, 4(Cu Cl)' _chemical_formula_sum 'C4 H6 Cl4 Cu4 N4' _chemical_formula_weight 506.09 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _space_group_name_Hall '-P 2ybc ' _symmetry_Int_Tables_number 14 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 6.8143(9) _cell_length_b 6.2582(8) _cell_length_c 13.6220(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.907(4) _cell_angle_gamma 90.00 _cell_volume 573.91(13) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1968 _cell_measurement_theta_min 3.03 _cell_measurement_theta_max 26.53 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.929 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 8.210 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.0543 _exptl_absorpt_correction_T_max 0.2905 _exptl_absorpt_process_details 'X-RED (Stoe & Cie, 2001) and X-SHAPE (Stoe & Cie, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'Stoe Imaging plate diffraction system' _diffrn_measurement_method '\f oscillation scans' _diffrn_standards_decay_% 0 _diffrn_reflns_number 1968 _diffrn_reflns_av_R_equivalents 0.0179 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 26.53 _reflns_number_total 1155 _reflns_number_gt 1058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS Software (Stoe & Cie, 2000)' _computing_cell_refinement 'IPDS Software (Stoe & Cie, 2000)' _computing_data_reduction 'IPDS Software (Stoe & Cie, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e (Brandenburg, 1999)' _computing_publication_material 'WinGX 1.70.01 (Farrugia, 1999)' #------------------------------- Refinement data-----------------------# _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^)+(0.0338P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0259(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1155 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0561 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 Cu1 Cu 0.08768(5) 0.10379(6) 0.84074(3) 0.01454(15) Uani 1 1 d . . . Cu2 Cu 0.16369(5) 0.34635(6) 1.05213(3) 0.01597(15) Uani 1 1 d . . . Cl1 Cl -0.13849(10) 0.28959(11) 0.93276(5) 0.01205(18) Uani 1 1 d . . . Cl2 Cl -0.12310(10) -0.18842(11) 0.79401(5) 0.01239(18) Uani 1 1 d . . . C1 C 0.4550(4) -0.1251(4) 0.9229(2) 0.0101(6) Uani 1 1 d . . . C2 C 0.3966(4) -0.2742(5) 0.8387(2) 0.0194(7) Uani 1 1 d . . . H2A H 0.4905 -0.3893 0.8424 0.029 Uiso 1 1 calc R . . H2B H 0.3946 -0.1991 0.7771 0.029 Uiso 1 1 calc R . . H2C H 0.2667 -0.3305 0.8420 0.029 Uiso 1 1 calc R . . N1 N 0.3787(3) 0.1680(3) 1.01287(16) 0.0087(5) Uani 1 1 d . . . N2 N 0.3336(3) 0.0401(4) 0.93311(17) 0.0093(5) 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 Cu1 0.0133(2) 0.0169(2) 0.0129(2) 0.00115(14) 0.00044(15) 0.00163(14) Cu2 0.0167(2) 0.0144(2) 0.0175(2) -0.00174(15) 0.00468(16) 0.00637(14) Cl1 0.0125(3) 0.0101(3) 0.0144(4) -0.0012(3) 0.0049(3) 0.0009(2) Cl2 0.0152(4) 0.0116(3) 0.0114(4) -0.0020(2) 0.0050(3) -0.0014(2) C1 0.0082(13) 0.0120(14) 0.0116(14) -0.0009(11) 0.0059(11) -0.0006(10) C2 0.0135(15) 0.0236(17) 0.0207(16) -0.0119(14) 0.0015(12) 0.0031(12) N1 0.0096(11) 0.0089(11) 0.0089(12) -0.0015(9) 0.0051(9) -0.0003(9) N2 0.0095(11) 0.0117(12) 0.0077(12) -0.0001(9) 0.0046(9) -0.0005(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 1.974(2) . ? Cu1 Cl2 2.2925(8) 2_556 ? Cu1 Cl2 2.3514(8) . ? Cu1 Cl1 2.4283(8) . ? Cu2 N1 1.981(2) . ? Cu2 Cl1 2.2965(8) 3_567 ? Cu2 Cl2 2.3718(8) 3_557 ? Cu2 Cl1 2.4442(8) . ? C1 N2 1.345(4) . ? C1 N1 1.347(4) 3_657 ? C1 C2 1.484(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? N1 N2 1.346(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Cu1 Cl2 116.15(7) . 2_556 ? N2 Cu1 Cl2 115.99(7) . . ? Cl2 Cu1 Cl2 111.10(2) 2_556 . ? N2 Cu1 Cl1 108.15(7) . . ? Cl2 Cu1 Cl1 107.19(3) 2_556 . ? Cl2 Cu1 Cl1 95.87(3) . . ? N1 Cu2 Cl1 130.71(7) . 3_567 ? N1 Cu2 Cl2 101.31(7) . 3_557 ? Cl1 Cu2 Cl2 108.28(3) 3_567 3_557 ? N1 Cu2 Cl1 108.71(7) . . ? Cl1 Cu2 Cl1 97.87(3) 3_567 . ? Cl2 Cu2 Cl1 109.02(3) 3_557 . ? Cu2 Cl1 Cu1 125.70(3) 3_567 . ? Cu2 Cl1 Cu2 82.13(3) 3_567 . ? Cu1 Cl1 Cu2 82.90(3) . . ? Cu1 Cl2 Cu1 121.48(3) 2_546 . ? Cu1 Cl2 Cu2 120.82(3) 2_546 3_557 ? Cu1 Cl2 Cu2 103.58(3) . 3_557 ? N2 C1 N1 123.7(2) . 3_657 ? N2 C1 C2 117.9(2) . . ? N1 C1 C2 118.4(2) 3_657 . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 N1 C1 118.1(2) . 3_657 ? N2 N1 Cu2 117.83(17) . . ? C1 N1 Cu2 121.30(19) 3_657 . ? C1 N2 N1 118.3(2) . . ? C1 N2 Cu1 124.34(19) . . ? N1 N2 Cu1 117.38(17) . . ? 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 Cu1 Cl1 Cu2 92.17(8) . . . 3_567 ? Cl2 Cu1 Cl1 Cu2 -33.77(5) 2_556 . . 3_567 ? Cl2 Cu1 Cl1 Cu2 -148.01(4) . . . 3_567 ? N2 Cu1 Cl1 Cu2 17.20(7) . . . . ? Cl2 Cu1 Cl1 Cu2 -108.74(3) 2_556 . . . ? Cl2 Cu1 Cl1 Cu2 137.02(3) . . . . ? N1 Cu2 Cl1 Cu2 -137.90(7) . . . 3_567 ? Cl1 Cu2 Cl1 Cu2 0.0 3_567 . . 3_567 ? Cl2 Cu2 Cl1 Cu2 112.49(3) 3_557 . . 3_567 ? N1 Cu2 Cl1 Cu1 -10.24(7) . . . . ? Cl1 Cu2 Cl1 Cu1 127.65(3) 3_567 . . . ? Cl2 Cu2 Cl1 Cu1 -119.86(3) 3_557 . . . ? N2 Cu1 Cl2 Cu1 -88.71(8) . . . 2_546 ? Cl2 Cu1 Cl2 Cu1 46.81(4) 2_556 . . 2_546 ? Cl1 Cu1 Cl2 Cu1 157.80(4) . . . 2_546 ? N2 Cu1 Cl2 Cu2 51.27(8) . . . 3_557 ? Cl2 Cu1 Cl2 Cu2 -173.20(3) 2_556 . . 3_557 ? Cl1 Cu1 Cl2 Cu2 -62.21(3) . . . 3_557 ? Cl1 Cu2 N1 N2 -121.14(17) 3_567 . . . ? Cl2 Cu2 N1 N2 112.41(18) 3_557 . . . ? Cl1 Cu2 N1 N2 -2.3(2) . . . . ? Cl1 Cu2 N1 C1 78.2(2) 3_567 . . 3_657 ? Cl2 Cu2 N1 C1 -48.3(2) 3_557 . . 3_657 ? Cl1 Cu2 N1 C1 -163.02(19) . . . 3_657 ? N1 C1 N2 N1 -1.1(4) 3_657 . . . ? C2 C1 N2 N1 175.7(2) . . . . ? N1 C1 N2 Cu1 -179.2(2) 3_657 . . . ? C2 C1 N2 Cu1 -2.4(4) . . . . ? C1 N1 N2 C1 1.1(4) 3_657 . . . ? Cu2 N1 N2 C1 -160.3(2) . . . . ? C1 N1 N2 Cu1 179.31(19) 3_657 . . . ? Cu2 N1 N2 Cu1 18.0(2) . . . . ? Cl2 Cu1 N2 C1 -87.0(2) 2_556 . . . ? Cl2 Cu1 N2 C1 46.2(2) . . . . ? Cl1 Cu1 N2 C1 152.5(2) . . . . ? Cl2 Cu1 N2 N1 94.84(18) 2_556 . . . ? Cl2 Cu1 N2 N1 -131.89(16) . . . . ? Cl1 Cu1 N2 N1 -25.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 26.53 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.632 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.115 # ------------- END of CIF -----------------#