# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Malcolm A Halcrow' _publ_contact_author_email M.A.Halcrow@leeds.ac.uk _publ_section_title ; New Insights into the Aggregation of Silver Pyrazolides Using Sterically Hindered Bidentate Pyrazole Ligands ; loop_ _publ_author_name J.Henkelis C.Kilner M.A.Halcrow # Attachment '- Ag Chem Comm.CIF' data_jjh23_(alpha-2) _database_code_depnum_ccdc_archive 'CCDC 806534' #TrackingRef '- Ag Chem Comm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[3{5}-(pyrid-2-yl)-5{3}-tertbutylpyrazolido]bromotrisilver(I) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 Ag3 Br N6' _chemical_formula_sum 'C24 H28 Ag3 Br N6' _chemical_formula_weight 804.04 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6895(12) _cell_length_b 11.8611(14) _cell_length_c 11.9531(13) _cell_angle_alpha 100.553(6) _cell_angle_beta 92.229(6) _cell_angle_gamma 91.219(6) _cell_volume 1348.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35404 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 30.74 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.980 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 3.661 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.618 _exptl_absorpt_correction_T_max 0.846 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35404 _diffrn_reflns_av_R_equivalents 0.0587 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 30.74 _reflns_number_total 8185 _reflns_number_gt 6502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The asymmetric unit contains a trinuclear [Ag3(m\-Br)(\m-L)2] molecule, which dimerises across the crystallographic inversion centre at 0, 0, 0 through argentophilic interactions between Ag2 and Ag3^i^ (symmetry code (i) -x, 2-y, 1-z) and their symmetry equivalents. The methyl groups of the tertbutyl group C31-C34 are disordered over two sites, labelled 'A' and 'B', with a refined occupancy ratio of 0.68:0.32. The fixed restraints C---C = 1.52(2) and 1,3-C...C = 2.48(2)\%A were applied to this group. All non-H atoms except for the minor tert-butyl disorder site were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. The highest residual Fourier peak (+1.4 e.\%A^-3^) is 0.4 \%A from Ag3, while the largest Fourier trough of -4.8 e.\%A^-3^ is associated with Br4. ; _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^)+(0.1083P)^2^+6.2662P] 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 8185 _refine_ls_number_parameters 326 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1909 _refine_ls_wR_factor_gt 0.1776 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.062 _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 0.06318(4) 0.81322(4) 0.33578(4) 0.02859(12) Uani 1 1 d . . . Ag2 Ag 0.22533(5) 1.03887(4) 0.55820(4) 0.03031(13) Uani 1 1 d . . . Ag3 Ag 0.00220(5) 0.90045(4) 0.64696(4) 0.03232(13) Uani 1 1 d . . . Br4 Br 0.17365(8) 1.04312(7) 0.76605(7) 0.0481(2) Uani 1 1 d . . . N5 N 0.4333(5) 1.1583(4) 0.5336(4) 0.0292(10) Uani 1 1 d . . . C6 C 0.5048(7) 1.2375(5) 0.6110(5) 0.0325(12) Uani 1 1 d . . . H6 H 0.4720 1.2554 0.6859 0.039 Uiso 1 1 calc R . . C7 C 0.6252(7) 1.2947(5) 0.5868(6) 0.0358(13) Uani 1 1 d . . . H7 H 0.6729 1.3498 0.6437 0.043 Uiso 1 1 calc R . . C8 C 0.6723(7) 1.2685(6) 0.4777(6) 0.0387(14) Uani 1 1 d . . . H8 H 0.7534 1.3064 0.4593 0.046 Uiso 1 1 calc R . . C9 C 0.6013(6) 1.1855(5) 0.3925(5) 0.0307(11) Uani 1 1 d . . . H9 H 0.6338 1.1664 0.3176 0.037 Uiso 1 1 calc R . . C10 C 0.4799(6) 1.1325(5) 0.4244(5) 0.0254(10) Uani 1 1 d . . . C11 C 0.3963(5) 1.0435(4) 0.3440(5) 0.0236(9) Uani 1 1 d . . . N12 N 0.2814(5) 0.9949(4) 0.3783(4) 0.0254(9) Uani 1 1 d . . . N13 N 0.2259(5) 0.9138(4) 0.2873(4) 0.0253(9) Uani 1 1 d . . . C14 C 0.3089(6) 0.9132(5) 0.1947(5) 0.0268(10) Uani 1 1 d . . . C15 C 0.4195(6) 0.9955(5) 0.2285(5) 0.0263(10) Uani 1 1 d . . . H15 H 0.4925 1.0141 0.1837 0.032 Uiso 1 1 calc R . . C16 C 0.2798(6) 0.8316(5) 0.0819(5) 0.0303(11) Uani 1 1 d . . . C17 C 0.1244(7) 0.8282(7) 0.0463(6) 0.0431(16) Uani 1 1 d . . . H17A H 0.0710 0.7973 0.1024 0.065 Uiso 1 1 calc R . . H17B H 0.1089 0.7792 -0.0287 0.065 Uiso 1 1 calc R . . H17C H 0.0949 0.9061 0.0429 0.065 Uiso 1 1 calc R . . C18 C 0.3289(10) 0.7102(6) 0.0920(6) 0.0500(19) Uani 1 1 d . . . H18A H 0.4260 0.7150 0.1190 0.075 Uiso 1 1 calc R . . H18B H 0.3192 0.6598 0.0172 0.075 Uiso 1 1 calc R . . H18C H 0.2725 0.6791 0.1461 0.075 Uiso 1 1 calc R . . C19 C 0.3613(8) 0.8734(7) -0.0129(5) 0.0421(16) Uani 1 1 d . . . H19A H 0.3388 0.9531 -0.0154 0.063 Uiso 1 1 calc R . . H19B H 0.3358 0.8249 -0.0866 0.063 Uiso 1 1 calc R . . H19C H 0.4606 0.8686 0.0035 0.063 Uiso 1 1 calc R . . N20 N -0.1498(5) 0.7895(5) 0.7581(4) 0.0312(10) Uani 1 1 d . . . C21 C -0.1811(7) 0.8124(6) 0.8693(6) 0.0380(14) Uani 1 1 d . . . H21 H -0.1326 0.8734 0.9189 0.046 Uiso 1 1 calc R . . C22 C -0.2837(8) 0.7486(7) 0.9145(6) 0.0458(17) Uani 1 1 d . . . H22 H -0.3010 0.7648 0.9934 0.055 Uiso 1 1 calc R . . C23 C -0.3585(9) 0.6619(7) 0.8416(7) 0.0486(18) Uani 1 1 d . . . H23 H -0.4280 0.6187 0.8704 0.058 Uiso 1 1 calc R . . C24 C -0.3310(7) 0.6381(6) 0.7250(6) 0.0394(14) Uani 1 1 d . . . H24 H -0.3826 0.5802 0.6739 0.047 Uiso 1 1 calc R . . C25 C -0.2240(6) 0.7029(5) 0.6856(5) 0.0277(10) Uani 1 1 d . . . C26 C -0.1831(6) 0.6795(5) 0.5655(5) 0.0279(10) Uani 1 1 d . . . N27 N -0.0906(5) 0.7523(4) 0.5278(4) 0.0276(9) Uani 1 1 d . . . N28 N -0.0706(5) 0.7096(4) 0.4137(4) 0.0290(10) Uani 1 1 d . A . C29 C -0.1494(7) 0.6092(5) 0.3787(5) 0.0330(12) Uani 1 1 d D . . C30 C -0.2228(7) 0.5881(5) 0.4743(5) 0.0333(12) Uani 1 1 d . A . H30 H -0.2852 0.5259 0.4767 0.040 Uiso 1 1 calc R . . C31A C -0.1401(14) 0.5395(8) 0.2592(7) 0.031(2) Uani 0.68 1 d PD A 1 C32A C -0.2259(17) 0.5978(12) 0.1761(7) 0.057(4) Uani 0.68 1 d PD A 1 H32A H -0.2208 0.5539 0.0986 0.085 Uiso 0.68 1 calc PR A 1 H32B H -0.1893 0.6760 0.1790 0.085 Uiso 0.68 1 calc PR A 1 H32C H -0.3224 0.6007 0.1979 0.085 Uiso 0.68 1 calc PR A 1 C33A C 0.0075(10) 0.5260(9) 0.2185(9) 0.047(3) Uani 0.68 1 d PD A 1 H33A H 0.0055 0.4799 0.1414 0.070 Uiso 0.68 1 calc PR A 1 H33B H 0.0622 0.4875 0.2702 0.070 Uiso 0.68 1 calc PR A 1 H33C H 0.0492 0.6018 0.2177 0.070 Uiso 0.68 1 calc PR A 1 C34A C -0.2013(13) 0.4168(8) 0.2548(8) 0.049(3) Uani 0.68 1 d PD A 1 H34A H -0.1944 0.3719 0.1779 0.073 Uiso 0.68 1 calc PR A 1 H34B H -0.2986 0.4213 0.2744 0.073 Uiso 0.68 1 calc PR A 1 H34C H -0.1496 0.3796 0.3094 0.073 Uiso 0.68 1 calc PR A 1 C31B C -0.173(2) 0.5465(19) 0.2576(16) 0.046(10) Uiso 0.32 1 d PD A 2 C32B C -0.179(4) 0.632(3) 0.178(2) 0.084(17) Uiso 0.32 1 d PD A 2 H32D H -0.1951 0.5906 0.0995 0.126 Uiso 0.32 1 calc PR A 2 H32E H -0.0918 0.6759 0.1846 0.126 Uiso 0.32 1 calc PR A 2 H32F H -0.2551 0.6839 0.1983 0.126 Uiso 0.32 1 calc PR A 2 C33B C -0.050(3) 0.469(2) 0.233(2) 0.078(9) Uiso 0.32 1 d PD A 2 H33D H -0.0442 0.4171 0.2882 0.116 Uiso 0.32 1 calc PR A 2 H33E H 0.0354 0.5156 0.2388 0.116 Uiso 0.32 1 calc PR A 2 H33F H -0.0619 0.4232 0.1557 0.116 Uiso 0.32 1 calc PR A 2 C34B C -0.305(2) 0.471(2) 0.241(2) 0.057(6) Uiso 0.32 1 d PD A 2 H34D H -0.3009 0.4166 0.2929 0.086 Uiso 0.32 1 calc PR A 2 H34E H -0.3124 0.4293 0.1619 0.086 Uiso 0.32 1 calc PR A 2 H34F H -0.3848 0.5197 0.2561 0.086 Uiso 0.32 1 calc PR A 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 0.0269(2) 0.0289(2) 0.0293(2) 0.00367(16) 0.00390(15) -0.00362(16) Ag2 0.0288(2) 0.0362(2) 0.0252(2) 0.00256(16) 0.00685(15) 0.00082(17) Ag3 0.0280(2) 0.0311(2) 0.0356(2) 0.00092(17) 0.00055(17) -0.00503(17) Br4 0.0436(4) 0.0557(5) 0.0424(4) 0.0022(3) 0.0041(3) -0.0007(3) N5 0.026(2) 0.031(2) 0.029(2) 0.0011(18) -0.0018(18) 0.0062(19) C6 0.034(3) 0.033(3) 0.027(3) -0.002(2) -0.002(2) 0.003(2) C7 0.037(3) 0.027(3) 0.040(3) 0.000(2) -0.010(2) 0.001(2) C8 0.036(3) 0.031(3) 0.049(4) 0.010(3) -0.006(3) -0.003(2) C9 0.032(3) 0.030(3) 0.032(3) 0.008(2) 0.003(2) 0.000(2) C10 0.026(3) 0.021(2) 0.028(2) 0.0024(19) -0.0009(19) 0.0047(19) C11 0.021(2) 0.023(2) 0.026(2) 0.0049(19) 0.0011(18) 0.0005(18) N12 0.025(2) 0.027(2) 0.024(2) 0.0027(17) 0.0029(16) 0.0017(17) N13 0.022(2) 0.029(2) 0.025(2) 0.0021(17) 0.0043(16) -0.0017(17) C14 0.024(2) 0.033(3) 0.022(2) 0.000(2) 0.0034(18) 0.001(2) C15 0.022(2) 0.033(3) 0.023(2) 0.003(2) 0.0038(18) 0.000(2) C16 0.031(3) 0.036(3) 0.022(2) -0.001(2) 0.004(2) -0.001(2) C17 0.030(3) 0.053(4) 0.038(3) -0.012(3) 0.001(2) -0.002(3) C18 0.077(6) 0.035(3) 0.034(3) -0.005(3) -0.008(3) 0.010(3) C19 0.040(4) 0.056(4) 0.026(3) -0.004(3) 0.007(2) -0.010(3) N20 0.028(2) 0.035(3) 0.030(2) 0.005(2) 0.0012(18) 0.005(2) C21 0.035(3) 0.045(4) 0.034(3) 0.006(3) -0.003(2) 0.008(3) C22 0.050(4) 0.057(4) 0.032(3) 0.010(3) 0.011(3) 0.016(3) C23 0.053(5) 0.047(4) 0.049(4) 0.013(3) 0.021(3) 0.001(3) C24 0.036(3) 0.042(3) 0.042(3) 0.010(3) 0.008(3) -0.003(3) C25 0.028(3) 0.026(2) 0.030(3) 0.006(2) 0.004(2) 0.003(2) C26 0.028(3) 0.025(2) 0.032(3) 0.006(2) 0.001(2) 0.001(2) N27 0.025(2) 0.027(2) 0.030(2) 0.0037(18) 0.0005(17) -0.0004(18) N28 0.026(2) 0.027(2) 0.033(2) 0.0047(18) 0.0010(18) -0.0090(18) C29 0.043(3) 0.023(3) 0.032(3) 0.003(2) 0.001(2) -0.008(2) C30 0.042(3) 0.026(3) 0.030(3) 0.004(2) -0.002(2) -0.007(2) C31A 0.038(6) 0.026(5) 0.027(5) 0.002(3) 0.000(3) -0.005(4) C32A 0.093(11) 0.056(7) 0.018(4) -0.004(4) -0.012(5) 0.036(9) C33A 0.049(6) 0.036(5) 0.048(6) -0.017(4) 0.018(5) 0.003(4) C34A 0.080(8) 0.036(5) 0.026(4) -0.004(4) 0.014(5) -0.023(5) _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 N13 2.119(5) . ? Ag1 N28 2.122(5) . ? Ag1 Br4 3.2187(10) 2_576 ? Ag2 N12 2.210(5) . ? Ag2 N5 2.496(5) . ? Ag2 Br4 2.5452(9) . ? Ag3 N27 2.201(5) . ? Ag3 N20 2.524(5) . ? Ag3 Br4 2.5424(10) . ? Ag1 Ag3 3.4385(8) 2_576 ? Ag1 Ag2 3.4884(7) 2_576 ? Ag1 Ag2 3.6864(7) . ? Ag1 Ag3 3.7473(8) . ? Ag2 Ag3 3.0267(7) . ? Ag2 Ag3 3.4184(7) 2_576 ? N5 C6 1.350(8) . ? N5 C10 1.381(7) . ? C6 C7 1.404(10) . ? C7 C8 1.381(10) . ? C8 C9 1.425(9) . ? C9 C10 1.420(8) . ? C10 C11 1.492(8) . ? C11 N12 1.355(7) . ? C11 C15 1.422(7) . ? N12 N13 1.395(7) . ? N13 C14 1.392(7) . ? C14 C15 1.429(8) . ? C14 C16 1.521(8) . ? C16 C17 1.546(9) . ? C16 C18 1.550(9) . ? C16 C19 1.552(9) . ? N20 C21 1.355(8) . ? N20 C25 1.385(8) . ? C21 C22 1.419(11) . ? C22 C23 1.390(12) . ? C23 C24 1.407(10) . ? C24 C25 1.423(9) . ? C25 C26 1.482(8) . ? C26 N27 1.376(8) . ? C26 C30 1.424(8) . ? N27 N28 1.388(7) . ? N28 C29 1.389(7) . ? C29 C30 1.427(9) . ? C29 C31B 1.507(17) . ? C29 C31A 1.520(10) . ? C31A C33A 1.531(14) . ? C31A C32A 1.538(12) . ? C31A C34A 1.551(11) . ? C31B C32B 1.510(17) . ? C31B C34B 1.526(17) . ? C31B C33B 1.529(17) . ? 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 N13 Ag1 N28 167.88(19) . . ? N13 Ag1 Br4 93.42(13) . 2_576 ? N28 Ag1 Br4 96.80(14) . 2_576 ? N12 Ag2 N5 72.07(17) . . ? N12 Ag2 Br4 167.19(13) . . ? N5 Ag2 Br4 113.14(12) . . ? N27 Ag3 N20 72.03(18) . . ? N27 Ag3 Br4 163.34(13) . . ? N20 Ag3 Br4 115.43(12) . . ? C6 N5 C10 118.5(5) . . ? C6 N5 Ag2 129.5(4) . . ? C10 N5 Ag2 112.0(4) . . ? N5 C6 C7 123.5(6) . . ? C8 C7 C6 118.0(6) . . ? C7 C8 C9 121.1(6) . . ? C10 C9 C8 117.0(6) . . ? N5 C10 C9 121.9(5) . . ? N5 C10 C11 115.5(5) . . ? C9 C10 C11 122.6(5) . . ? N12 C11 C15 110.2(5) . . ? N12 C11 C10 120.7(5) . . ? C15 C11 C10 129.2(5) . . ? C11 N12 N13 108.4(4) . . ? C11 N12 Ag2 119.6(4) . . ? N13 N12 Ag2 131.6(4) . . ? C14 N13 N12 108.3(4) . . ? C14 N13 Ag1 138.4(4) . . ? N12 N13 Ag1 112.5(3) . . ? N13 C14 C15 108.2(5) . . ? N13 C14 C16 122.0(5) . . ? C15 C14 C16 129.8(5) . . ? C11 C15 C14 104.9(5) . . ? C14 C16 C17 110.8(5) . . ? C14 C16 C18 109.6(5) . . ? C17 C16 C18 110.8(6) . . ? C14 C16 C19 109.7(5) . . ? C17 C16 C19 107.8(5) . . ? C18 C16 C19 108.1(6) . . ? C21 N20 C25 118.5(6) . . ? C21 N20 Ag3 130.1(5) . . ? C25 N20 Ag3 110.7(4) . . ? N20 C21 C22 122.4(7) . . ? C23 C22 C21 119.0(6) . . ? C22 C23 C24 119.9(7) . . ? C23 C24 C25 118.4(7) . . ? N20 C25 C24 121.8(6) . . ? N20 C25 C26 116.2(5) . . ? C24 C25 C26 122.0(6) . . ? N27 C26 C30 109.3(5) . . ? N27 C26 C25 120.1(5) . . ? C30 C26 C25 130.6(5) . . ? C26 N27 N28 107.8(4) . . ? C26 N27 Ag3 120.1(4) . . ? N28 N27 Ag3 132.1(4) . . ? N27 N28 C29 109.7(5) . . ? N27 N28 Ag1 114.2(3) . . ? C29 N28 Ag1 136.1(4) . . ? N28 C29 C30 107.4(5) . . ? N28 C29 C31B 125.9(10) . . ? C30 C29 C31B 125.9(10) . . ? N28 C29 C31A 120.9(6) . . ? C30 C29 C31A 131.5(6) . . ? C26 C30 C29 105.9(5) . . ? C29 C31A C33A 114.0(8) . . ? C29 C31A C32A 108.5(8) . . ? C33A C31A C32A 109.1(9) . . ? C29 C31A C34A 109.7(7) . . ? C33A C31A C34A 106.8(9) . . ? C32A C31A C34A 108.6(10) . . ? C29 C31B C32B 109.8(15) . . ? C29 C31B C34B 112.6(14) . . ? C32B C31B C34B 109.5(15) . . ? C29 C31B C33B 106.1(14) . . ? C32B C31B C33B 110.7(15) . . ? C34B C31B C33B 108.1(14) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 30.74 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.477 _refine_diff_density_min -4.775 _refine_diff_density_rms 0.278 #=END data_mh391_(beta-2) _database_code_depnum_ccdc_archive 'CCDC 806535' #TrackingRef '- Ag Chem Comm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[3{5}-(pyrid-2-yl)-5{3}-tertbutylpyrazolido]bromotrisilver(I) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H28 Ag3 Br N6' _chemical_formula_sum 'C24 H28 Ag3 Br N6' _chemical_formula_weight 804.04 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' 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 12.9535(13) _cell_length_b 9.6805(9) _cell_length_c 21.741(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.199(5) _cell_angle_gamma 90.00 _cell_volume 2691.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 74513 _cell_measurement_theta_min 1.59 _cell_measurement_theta_max 28.47 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.984 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 3.670 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.571 _exptl_absorpt_correction_T_max 0.730 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74513 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.47 _reflns_number_total 6763 _reflns_number_gt 5726 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2003)' _computing_publication_material 'local program' _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. The asymmetric unit contains a trinuclear [Ag3(m\-Br)(\m-L)2] molecule, which dimerises across the crystallographic inversion centre at 0, 0, 0 through argentophilic interactions between Ag2 and Ag3^i^ (symmetry code (i) -x, -y, -z) and their symmetry equivalents. The methyl groups of the tertbutyl group C31-C34 are disordered over two sites, labelled 'A' and 'B', with a refined occupancy ratio of 0.69:0.31. The fixed restraints C---C = 1.52(2) and 1,3-C...C = 2.48(2)\%A were applied to this group. All non-H atoms except for the minor tert-butyl disorder site were refined anisotropically, and all H atoms were placed in calculated positions and refined using a riding model. ; _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^)+(0.0000P)^2^+1.9005P] 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 6763 _refine_ls_number_parameters 323 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0307 _refine_ls_R_factor_gt 0.0201 _refine_ls_wR_factor_ref 0.0505 _refine_ls_wR_factor_gt 0.0448 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.002 _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 0.229058(13) 0.307875(18) 0.535910(8) 0.02491(5) Uani 1 1 d . . . Ag2 Ag 0.015017(14) 0.495138(19) 0.585226(8) 0.02825(5) Uani 1 1 d . . . Ag3 Ag -0.062010(14) 0.267094(19) 0.500092(8) 0.02732(5) Uani 1 1 d . . . Br4 Br -0.177475(18) 0.42949(2) 0.552575(11) 0.02799(6) Uani 1 1 d . . . N5 N 0.02859(16) 0.6604(2) 0.67638(9) 0.0268(4) Uani 1 1 d . . . C6 C -0.0464(2) 0.7352(3) 0.69771(12) 0.0331(6) Uani 1 1 d . . . H6 H -0.1172 0.7202 0.6795 0.040 Uiso 1 1 calc R . . C7 C -0.0252(2) 0.8336(3) 0.74533(12) 0.0353(6) Uani 1 1 d . . . H7 H -0.0802 0.8841 0.7591 0.042 Uiso 1 1 calc R . . C8 C 0.0791(2) 0.8555(3) 0.77204(11) 0.0356(6) Uani 1 1 d . . . H8 H 0.0963 0.9216 0.8043 0.043 Uiso 1 1 calc R . . C9 C 0.1584(2) 0.7785(3) 0.75056(11) 0.0306(5) Uani 1 1 d . . . H9 H 0.2296 0.7911 0.7684 0.037 Uiso 1 1 calc R . . C10 C 0.13005(19) 0.6819(2) 0.70194(10) 0.0241(5) Uani 1 1 d . . . C11 C 0.20979(18) 0.5995(2) 0.67591(10) 0.0220(4) Uani 1 1 d . . . N12 N 0.17961(15) 0.50935(19) 0.62836(9) 0.0242(4) Uani 1 1 d . . . N13 N 0.26886(15) 0.4497(2) 0.61209(8) 0.0248(4) Uani 1 1 d . . . C14 C 0.35458(18) 0.5038(2) 0.64952(10) 0.0226(5) Uani 1 1 d . . . C15 C 0.32005(19) 0.5988(2) 0.69101(10) 0.0250(5) Uani 1 1 d . . . H15 H 0.3620 0.6513 0.7225 0.030 Uiso 1 1 calc R . . C16 C 0.46685(18) 0.4600(3) 0.64402(11) 0.0266(5) Uani 1 1 d . . . C17 C 0.4858(2) 0.4721(4) 0.57575(12) 0.0453(7) Uani 1 1 d . . . H17A H 0.4724 0.5673 0.5612 0.068 Uiso 1 1 calc R . . H17B H 0.4385 0.4093 0.5494 0.068 Uiso 1 1 calc R . . H17C H 0.5584 0.4475 0.5734 0.068 Uiso 1 1 calc R . . C18 C 0.4851(3) 0.3093(3) 0.66657(17) 0.0545(9) Uani 1 1 d . . . H18A H 0.4372 0.2479 0.6398 0.082 Uiso 1 1 calc R . . H18B H 0.4720 0.3016 0.7096 0.082 Uiso 1 1 calc R . . H18C H 0.5575 0.2826 0.6646 0.082 Uiso 1 1 calc R . . C19 C 0.5458(2) 0.5546(4) 0.68565(15) 0.0499(8) Uani 1 1 d . . . H19A H 0.5359 0.5452 0.7292 0.075 Uiso 1 1 calc R . . H19B H 0.5341 0.6509 0.6724 0.075 Uiso 1 1 calc R . . H19C H 0.6173 0.5274 0.6816 0.075 Uiso 1 1 calc R . . N20 N -0.15624(15) 0.1095(2) 0.42122(9) 0.0259(4) Uani 1 1 d . . . C21 C -0.25969(19) 0.0968(3) 0.40004(11) 0.0316(5) Uani 1 1 d . . . H21 H -0.3062 0.1605 0.4145 0.038 Uiso 1 1 calc R . . C22 C -0.3019(2) -0.0053(3) 0.35782(13) 0.0382(6) Uani 1 1 d . . . H22 H -0.3751 -0.0099 0.3434 0.046 Uiso 1 1 calc R . . C23 C -0.2333(2) -0.1007(3) 0.33745(12) 0.0376(6) Uani 1 1 d . . . H23 H -0.2596 -0.1728 0.3096 0.045 Uiso 1 1 calc R . . C24 C -0.1255(2) -0.0888(3) 0.35846(11) 0.0297(5) Uani 1 1 d . . . H24 H -0.0780 -0.1527 0.3451 0.036 Uiso 1 1 calc R . . C25 C -0.08850(18) 0.0197(2) 0.39982(10) 0.0240(5) Uani 1 1 d . . . C26 C 0.02484(18) 0.0453(2) 0.42020(10) 0.0223(4) Uani 1 1 d . . . N27 N 0.05716(15) 0.14844(19) 0.46132(8) 0.0224(4) Uani 1 1 d . . . N28 N 0.16514(15) 0.15896(19) 0.46707(8) 0.0233(4) Uani 1 1 d . . . C29 C 0.19960(18) 0.0616(2) 0.42904(10) 0.0233(5) Uani 1 1 d D A . C30 C 0.11232(19) -0.0141(2) 0.39930(10) 0.0253(5) Uani 1 1 d . . . H30 H 0.1126 -0.0892 0.3712 0.030 Uiso 1 1 calc R . . C31 C 0.31362(19) 0.0469(3) 0.41907(11) 0.0285(5) Uani 1 1 d D . . C32A C 0.3466(3) -0.1084(4) 0.4305(2) 0.0409(10) Uani 0.69 1 d PD A 1 H32A H 0.2987 -0.1676 0.4026 0.061 Uiso 0.69 1 calc PR A 1 H32B H 0.3435 -0.1331 0.4739 0.061 Uiso 0.69 1 calc PR A 1 H32C H 0.4181 -0.1213 0.4221 0.061 Uiso 0.69 1 calc PR A 1 C33A C 0.3886(3) 0.1380(5) 0.4634(2) 0.0397(11) Uani 0.69 1 d PD A 1 H33A H 0.4602 0.1245 0.4553 0.060 Uiso 0.69 1 calc PR A 1 H33B H 0.3848 0.1124 0.5066 0.060 Uiso 0.69 1 calc PR A 1 H33C H 0.3688 0.2351 0.4567 0.060 Uiso 0.69 1 calc PR A 1 C34A C 0.3209(4) 0.0831(8) 0.3506(2) 0.0438(13) Uani 0.69 1 d PD A 1 H34A H 0.2734 0.0235 0.3227 0.066 Uiso 0.69 1 calc PR A 1 H34B H 0.3928 0.0687 0.3431 0.066 Uiso 0.69 1 calc PR A 1 H34C H 0.3012 0.1799 0.3425 0.066 Uiso 0.69 1 calc PR A 1 C32B C 0.3661(9) -0.0771(10) 0.4525(5) 0.047(3) Uiso 0.31 1 d PD A 2 H32D H 0.4385 -0.0829 0.4448 0.071 Uiso 0.31 1 calc PR A 2 H32E H 0.3283 -0.1611 0.4371 0.071 Uiso 0.31 1 calc PR A 2 H32F H 0.3656 -0.0678 0.4974 0.071 Uiso 0.31 1 calc PR A 2 C33B C 0.3783(9) 0.1789(10) 0.4410(5) 0.048(4) Uiso 0.31 1 d PD A 2 H33D H 0.3455 0.2597 0.4188 0.072 Uiso 0.31 1 calc PR A 2 H33E H 0.4497 0.1685 0.4322 0.072 Uiso 0.31 1 calc PR A 2 H33F H 0.3803 0.1914 0.4859 0.072 Uiso 0.31 1 calc PR A 2 C34B C 0.3170(12) 0.0334(14) 0.3491(5) 0.050(5) Uiso 0.31 1 d PD A 2 H34D H 0.2840 0.1145 0.3272 0.075 Uiso 0.31 1 calc PR A 2 H34E H 0.2793 -0.0501 0.3330 0.075 Uiso 0.31 1 calc PR A 2 H34F H 0.3899 0.0272 0.3424 0.075 Uiso 0.31 1 calc PR A 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 0.02685(9) 0.02468(10) 0.02262(9) -0.00924(6) 0.00218(7) -0.00272(7) Ag2 0.02754(9) 0.02798(11) 0.02830(10) -0.00576(7) 0.00162(7) -0.00451(7) Ag3 0.03012(10) 0.02515(10) 0.02703(9) -0.00652(7) 0.00562(7) -0.00092(7) Br4 0.02573(12) 0.02489(13) 0.03217(13) -0.00313(9) 0.00105(9) 0.00273(9) N5 0.0332(11) 0.0184(10) 0.0294(10) -0.0009(8) 0.0068(8) 0.0001(8) C6 0.0378(14) 0.0238(13) 0.0385(14) 0.0023(10) 0.0090(11) 0.0019(10) C7 0.0494(16) 0.0268(14) 0.0330(13) 0.0030(10) 0.0171(12) 0.0095(11) C8 0.0559(17) 0.0259(13) 0.0253(12) -0.0045(10) 0.0072(11) 0.0056(12) C9 0.0441(15) 0.0254(13) 0.0219(11) -0.0047(9) 0.0038(10) 0.0010(10) C10 0.0363(13) 0.0179(11) 0.0186(10) 0.0018(8) 0.0063(9) -0.0014(9) C11 0.0300(12) 0.0186(11) 0.0171(10) -0.0003(8) 0.0030(8) -0.0020(9) N12 0.0293(10) 0.0212(10) 0.0222(9) -0.0052(7) 0.0045(8) -0.0024(8) N13 0.0290(10) 0.0236(10) 0.0212(9) -0.0068(7) 0.0027(8) -0.0022(8) C14 0.0294(12) 0.0197(11) 0.0175(10) 0.0001(8) 0.0003(8) -0.0041(9) C15 0.0321(12) 0.0223(12) 0.0191(11) -0.0044(8) -0.0001(9) -0.0047(9) C16 0.0262(12) 0.0290(13) 0.0238(11) -0.0008(9) 0.0014(9) -0.0021(9) C17 0.0335(14) 0.071(2) 0.0322(14) -0.0037(14) 0.0090(11) -0.0073(14) C18 0.0429(17) 0.0444(19) 0.078(2) 0.0190(16) 0.0160(16) 0.0126(14) C19 0.0303(14) 0.066(2) 0.0512(18) -0.0242(16) -0.0011(13) -0.0065(14) N20 0.0276(10) 0.0252(11) 0.0243(10) 0.0028(8) 0.0020(8) -0.0042(8) C21 0.0282(12) 0.0328(14) 0.0324(13) 0.0042(10) 0.0010(10) -0.0007(10) C22 0.0333(14) 0.0411(16) 0.0365(14) 0.0046(12) -0.0054(11) -0.0110(12) C23 0.0413(15) 0.0382(16) 0.0303(13) -0.0049(11) -0.0032(11) -0.0168(12) C24 0.0350(13) 0.0279(13) 0.0252(12) -0.0033(9) 0.0019(10) -0.0068(10) C25 0.0315(12) 0.0216(12) 0.0183(10) 0.0028(8) 0.0026(9) -0.0053(9) C26 0.0301(12) 0.0188(11) 0.0175(10) -0.0002(8) 0.0023(8) -0.0051(9) N27 0.0263(10) 0.0221(10) 0.0191(9) -0.0024(7) 0.0046(7) -0.0018(8) N28 0.0280(10) 0.0195(10) 0.0221(9) -0.0038(7) 0.0033(7) -0.0025(8) C29 0.0294(12) 0.0194(11) 0.0210(11) -0.0025(8) 0.0043(9) 0.0010(9) C30 0.0336(12) 0.0204(12) 0.0214(11) -0.0059(9) 0.0032(9) -0.0027(9) C31 0.0276(12) 0.0286(13) 0.0294(12) -0.0071(10) 0.0047(9) 0.0005(10) C32A 0.034(2) 0.032(2) 0.056(3) -0.010(2) 0.003(2) 0.0059(17) C33A 0.0225(19) 0.044(3) 0.052(3) -0.022(2) 0.0039(18) -0.0011(18) C34A 0.033(2) 0.064(5) 0.038(3) 0.009(2) 0.0136(17) 0.000(3) _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 N28 2.1465(18) . ? Ag1 N13 2.1496(18) . ? Ag1 Br4 3.1938(4) 3_566 ? Ag2 N12 2.1919(19) . ? Ag2 N5 2.5312(19) . ? Ag2 Br4 2.5611(4) . ? Ag3 N27 2.1975(19) . ? Ag3 N20 2.4674(19) . ? Ag3 Br4 2.5605(3) . ? Ag1 Ag2 3.6157(4) . ? Ag1 Ag3 3.7469(4) . ? Ag1 Ag2 4.2316(4) 3_566 ? Ag1 Ag3 4.6565(4) 3_566 ? Ag2 Ag3 2.9503(3) . ? Ag2 Ag3 3.0774(3) 3_566 ? N5 C6 1.352(3) . ? N5 C10 1.359(3) . ? C6 C7 1.402(4) . ? C7 C8 1.399(4) . ? C8 C9 1.407(4) . ? C9 C10 1.415(3) . ? C10 C11 1.487(3) . ? C11 N12 1.362(3) . ? C11 C15 1.414(3) . ? N12 N13 1.388(3) . ? N13 C14 1.372(3) . ? C14 C15 1.410(3) . ? C14 C16 1.538(3) . ? C16 C18 1.546(4) . ? C16 C17 1.547(3) . ? C16 C19 1.552(3) . ? N20 C21 1.351(3) . ? N20 C25 1.368(3) . ? C21 C22 1.400(4) . ? C22 C23 1.401(4) . ? C23 C24 1.403(4) . ? C24 C25 1.416(3) . ? C25 C26 1.485(3) . ? C26 N27 1.361(3) . ? C26 C30 1.409(3) . ? N27 N28 1.388(3) . ? N28 C29 1.375(3) . ? C29 C30 1.414(3) . ? C29 C31 1.533(3) . ? C31 C32B 1.508(9) . ? C31 C33A 1.533(4) . ? C31 C34B 1.535(10) . ? C31 C34A 1.548(5) . ? C31 C33B 1.560(9) . ? C31 C32A 1.571(5) . ? 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 N28 Ag1 N13 169.87(7) . . ? N28 Ag1 Br4 95.42(5) . 3_566 ? N13 Ag1 Br4 87.54(5) . 3_566 ? N12 Ag2 N5 71.60(7) . . ? N12 Ag2 Br4 166.28(5) . . ? N5 Ag2 Br4 108.45(5) . . ? N27 Ag3 N20 73.15(7) . . ? N27 Ag3 Br4 171.14(5) . . ? N20 Ag3 Br4 115.47(5) . . ? C6 N5 C10 118.6(2) . . ? C6 N5 Ag2 130.03(17) . . ? C10 N5 Ag2 111.01(14) . . ? N5 C6 C7 123.4(3) . . ? C8 C7 C6 118.1(2) . . ? C7 C8 C9 119.3(2) . . ? C8 C9 C10 118.8(2) . . ? N5 C10 C9 121.7(2) . . ? N5 C10 C11 116.59(19) . . ? C9 C10 C11 121.7(2) . . ? N12 C11 C15 109.28(19) . . ? N12 C11 C10 120.0(2) . . ? C15 C11 C10 130.7(2) . . ? C11 N12 N13 108.09(18) . . ? C11 N12 Ag2 120.44(15) . . ? N13 N12 Ag2 131.13(13) . . ? C14 N13 N12 108.55(17) . . ? C14 N13 Ag1 140.62(16) . . ? N12 N13 Ag1 110.80(13) . . ? N13 C14 C15 108.6(2) . . ? N13 C14 C16 122.3(2) . . ? C15 C14 C16 129.1(2) . . ? C14 C15 C11 105.45(19) . . ? C14 C16 C18 109.5(2) . . ? C14 C16 C17 110.5(2) . . ? C18 C16 C17 109.6(2) . . ? C14 C16 C19 109.6(2) . . ? C18 C16 C19 108.6(2) . . ? C17 C16 C19 108.9(2) . . ? C21 N20 C25 118.8(2) . . ? C21 N20 Ag3 130.29(17) . . ? C25 N20 Ag3 110.87(14) . . ? N20 C21 C22 123.4(2) . . ? C21 C22 C23 118.1(2) . . ? C22 C23 C24 119.5(2) . . ? C23 C24 C25 119.1(2) . . ? N20 C25 C24 121.1(2) . . ? N20 C25 C26 116.7(2) . . ? C24 C25 C26 122.1(2) . . ? N27 C26 C30 109.42(19) . . ? N27 C26 C25 120.3(2) . . ? C30 C26 C25 130.0(2) . . ? C26 N27 N28 108.22(17) . . ? C26 N27 Ag3 118.32(15) . . ? N28 N27 Ag3 133.37(14) . . ? C29 N28 N27 108.36(17) . . ? C29 N28 Ag1 138.92(16) . . ? N27 N28 Ag1 112.51(13) . . ? N28 C29 C30 108.5(2) . . ? N28 C29 C31 124.14(19) . . ? C30 C29 C31 127.2(2) . . ? C26 C30 C29 105.45(19) . . ? C29 C31 C33A 112.7(2) . . ? C29 C31 C34A 108.9(3) . . ? C33A C31 C34A 110.2(4) . . ? C29 C31 C32A 108.0(2) . . ? C33A C31 C32A 108.8(3) . . ? C34A C31 C32A 108.2(3) . . ? C32B C31 C29 112.1(5) . . ? C32B C31 C34B 109.2(7) . . ? C29 C31 C34B 109.2(6) . . ? C32B C31 C33B 109.0(6) . . ? C29 C31 C33B 111.3(5) . . ? C34B C31 C33B 105.9(6) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.552 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.127 #=END data_jjh4_(compound_3) _database_code_depnum_ccdc_archive 'CCDC 806536' #TrackingRef '- Ag Chem Comm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Octakis[3-{pyrid-2-yl}-5-tertbutylpyrazolyl]decasilver(I) dichloride ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C96 H112 Ag10 N24, 2 Cl' _chemical_formula_sum 'C96 H112 Ag10 Cl2 N24' _chemical_formula_weight 2751.70 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' 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 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.170(2) _cell_length_b 17.8880(14) _cell_length_c 24.0804(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.925(4) _cell_angle_gamma 90.00 _cell_volume 10645.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 116871 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 28.11 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5352 _exptl_absorpt_coefficient_mu 1.851 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 1.075 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 116871 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.11 _reflns_number_total 12807 _reflns_number_gt 9389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'local program' _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. The asymmetric unit contains half a cluster molecule spanning the crystallographic C~2~ axis at 0, y, 0.25, together with a disordered region of electron density occupying a void in the lattice spanning the crystallographic inversion centre at 0.25, 0.25, 0.5. Each void was presumed to contain two anions on charge balancing grounds, which were likely to be either BF~4~^-^ or Cl^-^ based on the contents of the reaction mixture. A SQUEEZE analysis of the isotropically refined model found four voids of 248 \%A^3^ per asymmetric unit, containing a total of 152 electrons. That equates to 38 electrons per void, or 19 electrons per asymmetric unit. Thus, there appears to be one disordered chloride ion (18 electrons) in the asymmetric unit. The original dataset, rather than the SQUEEZEd one, was used for the final refinement cycles. Seven Fourier peaks in the disordered region were located, which were each refined as 0.1 of a Cl atom. The remaining 0.3 of a Cl atom could not be located in the Fourier map, but was included in the density and F(000) calculations. Three of the four unique tertbutyl groups in the model are disordered over two sites, that were each modelled with a 0.6:0.4 occupancy ratio. Disorder sites were refined for the complete tertbutyl fragments C17-C20 and C62-C65, but the third disordered tertbutyl moiety was refined with partial methyl groups C33-C35 only, which shared a common wholly-occupied ipso-C atom C32. The fixed restraints C---C = 1.52(2) and 1,3-C...C = 2.48(2)\%A were applied to the disordered residues. All fully occupied non-H atoms were refined anisotropically, and H atoms were palced in calculated positions and refined using a riding model. There are several residual Fourier peaks between 2.0 and 3.9 e.\%A^-3^ in the final model, all of them between 1.0 and 1.3 \%A from an Ag atom. ; _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^)+(0.1286P)^2^+454.9295P] 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 12807 _refine_ls_number_parameters 607 _refine_ls_number_restraints 58 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2860 _refine_ls_wR_factor_gt 0.2603 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.115 _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 0.00924(3) 0.60872(4) 0.19480(3) 0.0290(2) Uani 1 1 d . . . Ag2 Ag 0.08572(4) 0.48038(5) 0.25158(4) 0.0385(2) Uani 1 1 d . . . Ag3 Ag 0.08314(3) 0.68571(4) 0.27600(3) 0.0305(2) Uani 1 1 d . . . Ag4 Ag 0.07992(4) 0.88889(5) 0.30258(4) 0.0444(3) Uani 1 1 d . . . Ag5 Ag -0.00407(3) 0.76168(4) 0.30706(3) 0.0300(2) Uani 1 1 d . . . N6 N 0.0457(4) 0.5866(5) 0.1105(4) 0.0335(19) Uani 1 1 d . . . C7 C 0.0778(5) 0.6323(7) 0.0864(5) 0.039(3) Uani 1 1 d . . . H7 H 0.0832 0.6819 0.1003 0.047 Uiso 1 1 calc R . . C8 C 0.1032(6) 0.6107(8) 0.0427(6) 0.052(3) Uani 1 1 d . . . H8 H 0.1250 0.6448 0.0265 0.062 Uiso 1 1 calc R . . C9 C 0.0958(7) 0.5361(9) 0.0230(6) 0.058(4) Uani 1 1 d . . . H9 H 0.1127 0.5192 -0.0068 0.069 Uiso 1 1 calc R . . C10 C 0.0640(6) 0.4885(8) 0.0470(6) 0.049(3) Uani 1 1 d . . . H10 H 0.0586 0.4385 0.0337 0.059 Uiso 1 1 calc R . . C11 C 0.0394(5) 0.5138(7) 0.0914(5) 0.036(2) Uani 1 1 d . . . C12 C 0.0050(5) 0.4663(6) 0.1197(5) 0.032(2) Uani 1 1 d . . . N13 N -0.0109(4) 0.4911(5) 0.1674(4) 0.0318(19) Uani 1 1 d . . . N14 N -0.0447(4) 0.4382(5) 0.1840(4) 0.038(2) Uani 1 1 d . . . C15 C -0.0486(5) 0.3790(6) 0.1469(6) 0.045(3) Uani 1 1 d D . . C16 C -0.0172(6) 0.3951(7) 0.1056(6) 0.045(3) Uani 1 1 d . A . H16 H -0.0121 0.3644 0.0748 0.054 Uiso 1 1 calc R . . C17B C -0.0871(8) 0.3136(10) 0.1488(9) 0.055(9) Uiso 0.60 1 d PD A 1 C18B C -0.1428(7) 0.3331(16) 0.1169(12) 0.089(10) Uiso 0.60 1 d PD A 1 H18D H -0.1559 0.3779 0.1335 0.134 Uiso 0.60 1 calc PR A 1 H18E H -0.1675 0.2914 0.1192 0.134 Uiso 0.60 1 calc PR A 1 H18F H -0.1412 0.3428 0.0771 0.134 Uiso 0.60 1 calc PR A 1 C19B C -0.0906(11) 0.2943(15) 0.2108(8) 0.058(6) Uiso 0.60 1 d PD A 1 H19D H -0.1053 0.3372 0.2282 0.087 Uiso 0.60 1 calc PR A 1 H19E H -0.0544 0.2826 0.2321 0.087 Uiso 0.60 1 calc PR A 1 H19F H -0.1143 0.2510 0.2113 0.087 Uiso 0.60 1 calc PR A 1 C20B C -0.0647(12) 0.2445(10) 0.1245(12) 0.080(10) Uiso 0.60 1 d PD A 1 H20D H -0.0894 0.2024 0.1253 0.121 Uiso 0.60 1 calc PR A 1 H20E H -0.0291 0.2322 0.1471 0.121 Uiso 0.60 1 calc PR A 1 H20F H -0.0611 0.2543 0.0853 0.121 Uiso 0.60 1 calc PR A 1 C17A C -0.0793(12) 0.3080(13) 0.1579(14) 0.052(13) Uiso 0.40 1 d PD A 2 C18A C -0.1383(12) 0.331(2) 0.158(3) 0.15(3) Uiso 0.40 1 d PD A 2 H18A H -0.1540 0.3539 0.1217 0.219 Uiso 0.40 1 calc PR A 2 H18B H -0.1391 0.3671 0.1885 0.219 Uiso 0.40 1 calc PR A 2 H18C H -0.1594 0.2868 0.1641 0.219 Uiso 0.40 1 calc PR A 2 C19A C -0.059(3) 0.264(4) 0.2120(16) 0.17(4) Uiso 0.40 1 d PD A 2 H19A H -0.0582 0.2965 0.2448 0.253 Uiso 0.40 1 calc PR A 2 H19B H -0.0222 0.2456 0.2117 0.253 Uiso 0.40 1 calc PR A 2 H19C H -0.0830 0.2215 0.2141 0.253 Uiso 0.40 1 calc PR A 2 C20A C -0.0813(16) 0.2552(15) 0.1072(15) 0.057(10) Uiso 0.40 1 d PD A 2 H20A H -0.0908 0.2838 0.0720 0.085 Uiso 0.40 1 calc PR A 2 H20B H -0.1085 0.2163 0.1082 0.085 Uiso 0.40 1 calc PR A 2 H20C H -0.0457 0.2319 0.1091 0.085 Uiso 0.40 1 calc PR A 2 N21 N 0.1361(5) 0.4128(7) 0.1798(5) 0.050(3) Uani 1 1 d . . . C22 C 0.1356(7) 0.3414(9) 0.1609(6) 0.054(3) Uani 1 1 d . . . H22 H 0.1072 0.3096 0.1674 0.065 Uiso 1 1 calc R . . C23 C 0.1747(7) 0.3115(8) 0.1325(6) 0.056(4) Uani 1 1 d . . . H23 H 0.1720 0.2616 0.1189 0.068 Uiso 1 1 calc R . . C24 C 0.2173(7) 0.3571(9) 0.1250(6) 0.058(4) Uani 1 1 d . . . H24 H 0.2455 0.3380 0.1078 0.069 Uiso 1 1 calc R . . C25 C 0.2182(6) 0.4320(9) 0.1430(6) 0.055(4) Uani 1 1 d . . . H25 H 0.2463 0.4647 0.1370 0.066 Uiso 1 1 calc R . . C26 C 0.1769(5) 0.4575(7) 0.1698(5) 0.041(3) Uani 1 1 d . . . C27 C 0.1759(5) 0.5359(7) 0.1878(5) 0.038(3) Uani 1 1 d . . . N28 N 0.1391(4) 0.5588(6) 0.2192(4) 0.034(2) Uani 1 1 d . . . N29 N 0.1434(4) 0.6352(6) 0.2274(4) 0.039(2) Uani 1 1 d . . . C30 C 0.1820(5) 0.6619(6) 0.2001(5) 0.041(3) Uani 1 1 d D B . C31 C 0.2039(5) 0.5996(7) 0.1750(6) 0.044(3) Uani 1 1 d . . . H31 H 0.2321 0.6010 0.1538 0.053 Uiso 1 1 calc R . . C32 C 0.1995(5) 0.7430(7) 0.2000(5) 0.049(3) Uani 1 1 d D . . C33A C 0.1778(13) 0.7793(15) 0.1435(9) 0.103(12) Uiso 0.60 1 d PD B 1 H33A H 0.1887 0.8320 0.1448 0.155 Uiso 0.60 1 calc PR B 1 H33B H 0.1382 0.7759 0.1354 0.155 Uiso 0.60 1 calc PR B 1 H33C H 0.1925 0.7536 0.1138 0.155 Uiso 0.60 1 calc PR B 1 C34A C 0.1792(10) 0.7882(12) 0.2461(9) 0.066(7) Uiso 0.60 1 d PD B 1 H34A H 0.1903 0.8405 0.2442 0.099 Uiso 0.60 1 calc PR B 1 H34B H 0.1948 0.7676 0.2833 0.099 Uiso 0.60 1 calc PR B 1 H34C H 0.1397 0.7853 0.2401 0.099 Uiso 0.60 1 calc PR B 1 C35A C 0.2613(6) 0.7474(14) 0.2128(12) 0.077(8) Uiso 0.60 1 d PD B 1 H35A H 0.2726 0.7999 0.2132 0.116 Uiso 0.60 1 calc PR B 1 H35B H 0.2758 0.7203 0.1836 0.116 Uiso 0.60 1 calc PR B 1 H35C H 0.2751 0.7249 0.2498 0.116 Uiso 0.60 1 calc PR B 1 C33B C 0.228(2) 0.756(2) 0.1504(17) 0.13(3) Uiso 0.40 1 d PD B 2 H33D H 0.2397 0.8082 0.1502 0.202 Uiso 0.40 1 calc PR B 2 H33E H 0.2031 0.7448 0.1149 0.202 Uiso 0.40 1 calc PR B 2 H33F H 0.2597 0.7231 0.1541 0.202 Uiso 0.40 1 calc PR B 2 C34B C 0.1511(12) 0.7940(14) 0.1948(19) 0.082(14) Uiso 0.40 1 d PD B 2 H34D H 0.1628 0.8461 0.1937 0.123 Uiso 0.40 1 calc PR B 2 H34E H 0.1335 0.7868 0.2274 0.123 Uiso 0.40 1 calc PR B 2 H34F H 0.1254 0.7823 0.1599 0.123 Uiso 0.40 1 calc PR B 2 C35B C 0.2391(17) 0.760(2) 0.2547(15) 0.14(3) Uiso 0.40 1 d PD B 2 H35D H 0.2515 0.8116 0.2543 0.205 Uiso 0.40 1 calc PR B 2 H35E H 0.2702 0.7259 0.2581 0.205 Uiso 0.40 1 calc PR B 2 H35F H 0.2211 0.7522 0.2870 0.205 Uiso 0.40 1 calc PR B 2 N36 N 0.1058(5) 0.9553(6) 0.4010(5) 0.046(3) Uani 1 1 d . . . C37 C 0.0964(7) 1.0239(8) 0.4182(7) 0.061(4) Uani 1 1 d . . . H37 H 0.0777 1.0580 0.3911 0.073 Uiso 1 1 calc R . . C38 C 0.1122(7) 1.0486(9) 0.4735(8) 0.066(4) Uani 1 1 d . . . H38 H 0.1040 1.0980 0.4839 0.079 Uiso 1 1 calc R . . C39 C 0.1403(7) 0.9996(10) 0.5134(7) 0.066(4) Uani 1 1 d . . . H39 H 0.1520 1.0148 0.5516 0.079 Uiso 1 1 calc R . . C40 C 0.1509(6) 0.9273(8) 0.4962(6) 0.051(3) Uani 1 1 d . . . H40 H 0.1700 0.8927 0.5226 0.061 Uiso 1 1 calc R . . C41 C 0.1331(5) 0.9063(7) 0.4395(5) 0.039(3) Uani 1 1 d . . . C42 C 0.1395(5) 0.8296(6) 0.4205(5) 0.035(2) Uani 1 1 d . . . N43 N 0.1185(4) 0.8089(5) 0.3664(4) 0.036(2) Uani 1 1 d . . . N44 N 0.1272(4) 0.7346(6) 0.3597(4) 0.040(2) Uani 1 1 d . . . C45 C 0.1574(5) 0.7076(7) 0.4091(5) 0.036(2) Uani 1 1 d . . . C46 C 0.1666(5) 0.7670(7) 0.4484(5) 0.036(2) Uani 1 1 d . . . H46 H 0.1869 0.7653 0.4859 0.043 Uiso 1 1 calc R . . C47 C 0.1771(5) 0.6275(7) 0.4143(5) 0.041(3) Uani 1 1 d . . . C48 C 0.1302(6) 0.5729(7) 0.3924(6) 0.055(4) Uani 1 1 d . . . H48A H 0.1018 0.5788 0.4147 0.082 Uiso 1 1 calc R . . H48B H 0.1438 0.5214 0.3959 0.082 Uiso 1 1 calc R . . H48C H 0.1154 0.5838 0.3526 0.082 Uiso 1 1 calc R . . C49 C 0.2230(6) 0.6165(8) 0.3796(6) 0.052(3) Uani 1 1 d . . . H49A H 0.2092 0.6288 0.3398 0.078 Uiso 1 1 calc R . . H49B H 0.2352 0.5644 0.3825 0.078 Uiso 1 1 calc R . . H49C H 0.2535 0.6495 0.3946 0.078 Uiso 1 1 calc R . . C50 C 0.1997(6) 0.6097(8) 0.4774(6) 0.047(3) Uani 1 1 d . . . H50A H 0.2301 0.6431 0.4915 0.071 Uiso 1 1 calc R . . H50B H 0.2122 0.5577 0.4810 0.071 Uiso 1 1 calc R . . H50C H 0.1712 0.6169 0.4995 0.071 Uiso 1 1 calc R . . N51 N 0.0075(4) 0.7843(5) 0.4092(4) 0.034(2) Uani 1 1 d . . . C52 C 0.0313(5) 0.7403(7) 0.4521(5) 0.038(3) Uani 1 1 d . . . H52 H 0.0414 0.6911 0.4435 0.046 Uiso 1 1 calc R . . C53 C 0.0420(6) 0.7628(8) 0.5081(5) 0.046(3) Uani 1 1 d . . . H53 H 0.0592 0.7299 0.5369 0.055 Uiso 1 1 calc R . . C54 C 0.0270(6) 0.8342(8) 0.5213(5) 0.050(3) Uani 1 1 d . . . H54 H 0.0325 0.8506 0.5595 0.060 Uiso 1 1 calc R . . C55 C 0.0037(6) 0.8815(8) 0.4774(5) 0.048(3) Uani 1 1 d . . . H55 H -0.0051 0.9316 0.4852 0.057 Uiso 1 1 calc R . . C56 C -0.0069(5) 0.8544(7) 0.4211(5) 0.036(2) Uani 1 1 d . . . C57 C -0.0323(5) 0.9022(6) 0.3737(5) 0.035(2) Uani 1 1 d . . . N58 N -0.0319(4) 0.8775(5) 0.3203(4) 0.036(2) Uani 1 1 d . . . N59 N -0.0606(5) 0.9285(5) 0.2835(5) 0.046(3) Uani 1 1 d . . . C60 C -0.0782(6) 0.9864(6) 0.3131(5) 0.051(4) Uani 1 1 d D . . C61 C -0.0593(6) 0.9715(7) 0.3718(6) 0.050(3) Uani 1 1 d . C . H61 H -0.0640 1.0017 0.4030 0.060 Uiso 1 1 calc R . . C62A C -0.1208(7) 1.0453(9) 0.2893(7) 0.039(4) Uiso 0.60 1 d PD C 1 C63A C -0.1139(10) 1.0666(13) 0.2301(7) 0.063(7) Uiso 0.60 1 d PD C 1 H63A H -0.1186 1.0222 0.2059 0.094 Uiso 0.60 1 calc PR C 1 H63B H -0.0775 1.0872 0.2316 0.094 Uiso 0.60 1 calc PR C 1 H63C H -0.1409 1.1043 0.2147 0.094 Uiso 0.60 1 calc PR C 1 C64A C -0.1779(7) 1.0127(16) 0.2850(12) 0.093(11) Uiso 0.60 1 d PD C 1 H64A H -0.1818 0.9686 0.2604 0.140 Uiso 0.60 1 calc PR C 1 H64B H -0.2048 1.0504 0.2690 0.140 Uiso 0.60 1 calc PR C 1 H64C H -0.1835 0.9984 0.3227 0.140 Uiso 0.60 1 calc PR C 1 C65A C -0.1158(10) 1.1124(10) 0.3276(9) 0.052(6) Uiso 0.60 1 d PD C 1 H65A H -0.1202 1.0969 0.3655 0.078 Uiso 0.60 1 calc PR C 1 H65B H -0.1439 1.1489 0.3125 0.078 Uiso 0.60 1 calc PR C 1 H65C H -0.0801 1.1352 0.3297 0.078 Uiso 0.60 1 calc PR C 1 C62B C -0.0991(10) 1.0563(11) 0.2796(9) 0.052(8) Uiso 0.40 1 d PD C 2 C63B C -0.0618(17) 1.078(2) 0.2395(15) 0.098(17) Uiso 0.40 1 d PD C 2 H63D H -0.0587 1.0357 0.2142 0.147 Uiso 0.40 1 calc PR C 2 H63E H -0.0259 1.0901 0.2613 0.147 Uiso 0.40 1 calc PR C 2 H63F H -0.0766 1.1213 0.2170 0.147 Uiso 0.40 1 calc PR C 2 C65B C -0.1009(15) 1.1205(11) 0.3202(13) 0.048(9) Uiso 0.40 1 d PD C 2 H65D H -0.1248 1.1076 0.3465 0.071 Uiso 0.40 1 calc PR C 2 H65E H -0.1146 1.1654 0.2989 0.071 Uiso 0.40 1 calc PR C 2 H65F H -0.0643 1.1302 0.3416 0.071 Uiso 0.40 1 calc PR C 2 C64B C -0.1553(12) 1.040(2) 0.2462(16) 0.105(18) Uiso 0.40 1 d PD C 2 H64D H -0.1534 0.9988 0.2198 0.157 Uiso 0.40 1 calc PR C 2 H64E H -0.1697 1.0846 0.2250 0.157 Uiso 0.40 1 calc PR C 2 H64F H -0.1792 1.0258 0.2722 0.157 Uiso 0.40 1 calc PR C 2 Cl1S Cl 0.245(4) 0.288(6) 0.518(4) 0.10(3) Uiso 0.10 1 d P . 1 Cl2S Cl 0.224(6) 0.284(8) 0.508(7) 0.15(5) Uiso 0.10 1 d P . 2 Cl5S Cl 0.252(4) 0.114(6) 0.499(5) 0.15(3) Uiso 0.10 1 d P D 5 Cl3S Cl 0.231(3) 0.161(5) 0.474(4) 0.11(2) Uiso 0.10 1 d P E 3 Cl4S Cl 0.228(3) 0.163(5) 0.504(4) 0.11(2) Uiso 0.10 1 d P F 4 Cl6S Cl 0.241(3) 0.090(5) 0.459(3) 0.12(2) Uiso 0.10 1 d P G 6 Cl7S Cl 0.257(5) 0.226(5) 0.505(5) 0.11(3) Uiso 0.10 1 d P . 7 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 0.0370(4) 0.0189(4) 0.0328(4) -0.0029(3) 0.0109(3) -0.0016(3) Ag2 0.0385(5) 0.0321(5) 0.0486(5) 0.0061(3) 0.0177(4) 0.0046(4) Ag3 0.0331(4) 0.0234(4) 0.0348(4) -0.0011(3) 0.0063(3) -0.0005(3) Ag4 0.0593(6) 0.0310(5) 0.0376(5) 0.0045(3) -0.0038(4) -0.0082(4) Ag5 0.0410(5) 0.0187(4) 0.0304(4) -0.0014(3) 0.0074(3) 0.0023(3) N6 0.031(5) 0.033(5) 0.037(5) 0.000(4) 0.008(4) 0.001(4) C7 0.040(6) 0.035(6) 0.043(6) 0.005(5) 0.009(5) -0.005(5) C8 0.056(8) 0.047(8) 0.058(8) 0.005(6) 0.026(7) -0.002(6) C9 0.065(9) 0.066(10) 0.049(8) -0.004(7) 0.029(7) -0.002(8) C10 0.057(8) 0.047(8) 0.049(7) -0.016(6) 0.022(6) -0.004(6) C11 0.038(6) 0.034(6) 0.040(6) -0.008(4) 0.012(5) -0.002(5) C12 0.036(6) 0.026(5) 0.036(5) 0.001(4) 0.012(4) 0.000(4) N13 0.041(5) 0.017(4) 0.039(5) -0.004(3) 0.012(4) 0.000(4) N14 0.052(6) 0.017(4) 0.046(5) -0.004(4) 0.012(4) -0.006(4) C15 0.052(7) 0.022(5) 0.064(8) -0.014(5) 0.016(6) -0.008(5) C16 0.051(7) 0.037(7) 0.051(7) -0.021(5) 0.019(6) -0.009(6) N21 0.058(7) 0.042(6) 0.049(6) 0.004(5) 0.011(5) 0.014(5) C22 0.067(9) 0.047(8) 0.049(8) 0.002(6) 0.013(7) 0.012(7) C23 0.079(11) 0.045(8) 0.046(8) -0.003(6) 0.016(7) 0.012(7) C24 0.068(10) 0.055(9) 0.053(8) 0.000(6) 0.017(7) 0.021(8) C25 0.051(8) 0.062(9) 0.057(8) 0.003(7) 0.026(7) 0.016(7) C26 0.039(6) 0.041(7) 0.046(7) 0.001(5) 0.013(5) 0.009(5) C27 0.030(5) 0.048(7) 0.041(6) 0.006(5) 0.016(5) 0.005(5) N28 0.023(4) 0.042(5) 0.040(5) 0.003(4) 0.012(4) 0.002(4) N29 0.047(6) 0.032(5) 0.039(5) 0.001(4) 0.013(4) -0.005(4) C30 0.033(6) 0.040(7) 0.052(7) 0.001(5) 0.008(5) -0.003(5) C31 0.032(6) 0.045(7) 0.059(8) 0.007(6) 0.018(5) 0.005(5) C32 0.044(7) 0.041(7) 0.063(8) 0.004(6) 0.013(6) -0.007(6) N36 0.056(7) 0.034(6) 0.046(6) -0.005(4) 0.005(5) 0.005(5) C37 0.082(11) 0.037(7) 0.059(9) -0.007(6) 0.003(8) 0.013(7) C38 0.066(10) 0.050(9) 0.081(11) -0.019(8) 0.015(8) 0.008(8) C39 0.078(11) 0.060(10) 0.055(9) -0.019(7) 0.005(8) 0.004(8) C40 0.052(8) 0.047(8) 0.050(7) -0.007(6) 0.001(6) 0.000(6) C41 0.033(6) 0.039(6) 0.044(6) -0.001(5) 0.006(5) -0.005(5) C42 0.032(6) 0.033(6) 0.037(6) 0.001(4) 0.004(4) -0.001(4) N43 0.040(5) 0.031(5) 0.038(5) 0.002(4) 0.007(4) 0.001(4) N44 0.050(6) 0.030(5) 0.039(5) 0.001(4) 0.005(4) 0.000(4) C45 0.032(6) 0.031(6) 0.042(6) 0.003(4) 0.000(5) -0.002(4) C46 0.030(5) 0.036(6) 0.041(6) 0.003(5) 0.006(4) -0.007(5) C47 0.044(7) 0.037(6) 0.039(6) 0.004(5) -0.001(5) -0.002(5) C48 0.067(9) 0.032(7) 0.058(8) 0.005(6) -0.008(7) -0.009(6) C49 0.051(8) 0.045(8) 0.061(9) 0.007(6) 0.018(6) 0.011(6) C50 0.052(8) 0.044(7) 0.043(7) 0.011(5) 0.002(6) -0.002(6) N51 0.036(5) 0.033(5) 0.034(5) 0.002(4) 0.006(4) 0.002(4) C52 0.042(6) 0.036(6) 0.036(6) 0.007(5) 0.004(5) 0.003(5) C53 0.049(7) 0.053(8) 0.034(6) 0.011(5) 0.001(5) -0.004(6) C54 0.065(9) 0.053(8) 0.031(6) -0.004(5) 0.006(6) -0.005(7) C55 0.070(9) 0.039(7) 0.033(6) -0.007(5) 0.008(6) -0.001(6) C56 0.042(6) 0.036(6) 0.030(5) -0.005(4) 0.006(4) 0.002(5) C57 0.046(6) 0.023(5) 0.036(6) -0.002(4) 0.002(5) -0.002(4) N58 0.043(5) 0.020(4) 0.045(5) -0.001(4) 0.007(4) 0.005(4) N59 0.065(7) 0.019(4) 0.047(6) 0.003(4) -0.003(5) 0.006(4) C60 0.078(10) 0.020(5) 0.048(7) -0.009(5) -0.007(6) 0.013(6) C61 0.072(9) 0.022(6) 0.051(7) -0.009(5) 0.003(6) 0.006(6) _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 N13 2.234(8) . ? Ag1 N6 2.414(9) . ? Ag2 N14 2.156(10) 2 ? Ag2 N28 2.186(9) . ? Ag2 N21 2.625(12) . ? Ag3 N29 2.272(10) . ? Ag3 N44 2.283(10) . ? Ag4 N59 2.157(11) 2 ? Ag4 N43 2.188(10) . ? Ag4 N36 2.621(11) . ? Ag5 N58 2.229(9) . ? Ag5 N51 2.454(9) . ? Ag1 Ag5 2.7393(11) 2 ? Ag1 Ag1 2.7844(15) 2 ? Ag1 Ag3 2.7931(11) . ? Ag1 Ag3 2.9012(11) 2 ? Ag1 Ag2 3.1380(12) . ? Ag2 Ag2 4.3012(18) 2 ? Ag2 Ag3 3.7223(12) . ? Ag3 Ag4 3.6939(12) . ? Ag3 Ag5 2.8011(11) . ? Ag3 Ag5 2.8807(11) 2 ? Ag4 Ag4 4.3285(20) 2 ? Ag4 Ag5 3.1218(13) . ? Ag5 Ag5 2.7940(15) 2 ? N6 C7 1.354(15) . ? N6 C11 1.381(15) . ? C7 C8 1.387(19) . ? C8 C9 1.42(2) . ? C9 C10 1.37(2) . ? C10 C11 1.409(16) . ? C11 C12 1.469(16) . ? C12 N13 1.360(14) . ? C12 C16 1.406(16) . ? N13 N14 1.381(13) . ? N14 C15 1.377(14) . ? C15 C16 1.413(18) . ? C15 C17B 1.525(16) . ? C15 C17A 1.535(18) . ? C17B C18B 1.508(17) . ? C17B C20B 1.521(16) . ? C17B C19B 1.551(17) . ? C17A C19A 1.525(19) . ? C17A C20A 1.537(18) . ? C17A C18A 1.542(19) . ? N21 C22 1.355(19) . ? N21 C26 1.358(18) . ? C22 C23 1.41(2) . ? C23 C24 1.39(2) . ? C24 C25 1.41(2) . ? C25 C26 1.400(17) . ? C26 C27 1.470(18) . ? C27 N28 1.365(14) . ? C27 C31 1.405(18) . ? N28 N29 1.382(14) . ? N29 C30 1.360(15) . ? C30 C31 1.426(18) . ? C30 C32 1.517(15) . ? C32 C34B 1.509(16) . ? C32 C33A 1.513(15) . ? C32 C35B 1.523(16) . ? C32 C33B 1.526(16) . ? C32 C35A 1.528(15) . ? C32 C34A 1.535(15) . ? N36 C37 1.332(17) . ? N36 C41 1.362(16) . ? C37 C38 1.39(2) . ? C38 C39 1.39(2) . ? C39 C40 1.40(2) . ? C40 C41 1.405(18) . ? C41 C42 1.465(17) . ? C42 N43 1.361(15) . ? C42 C46 1.412(16) . ? N43 N44 1.361(14) . ? N44 C45 1.372(15) . ? C45 C46 1.413(17) . ? C45 C47 1.514(17) . ? C47 C48 1.545(18) . ? C47 C50 1.550(17) . ? C47 C49 1.564(19) . ? N51 C52 1.346(14) . ? N51 C56 1.352(15) . ? C52 C53 1.384(18) . ? C53 C54 1.39(2) . ? C54 C55 1.393(19) . ? C55 C56 1.416(16) . ? C56 C57 1.472(16) . ? C57 N58 1.361(15) . ? C57 C61 1.412(16) . ? N58 N59 1.376(13) . ? N59 C60 1.378(15) . ? C60 C61 1.429(18) . ? C60 C62B 1.526(17) . ? C60 C62A 1.535(14) . ? C62A C65A 1.505(15) . ? C62A C63A 1.517(15) . ? C62A C64A 1.535(16) . ? C62B C65B 1.515(17) . ? C62B C64B 1.517(17) . ? C62B C63B 1.521(17) . ? 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 N13 Ag1 N6 72.5(3) . . ? N14 Ag2 N28 153.1(4) 2 . ? N14 Ag2 N21 132.1(4) 2 . ? N28 Ag2 N21 69.8(4) . . ? N29 Ag3 N44 110.3(4) . . ? N59 Ag4 N43 151.5(4) 2 . ? N59 Ag4 N36 133.9(4) 2 . ? N43 Ag4 N36 70.1(4) . . ? N58 Ag5 N51 71.6(3) . . ? C7 N6 C11 117.9(10) . . ? C7 N6 Ag1 127.9(8) . . ? C11 N6 Ag1 113.3(7) . . ? N6 C7 C8 123.8(12) . . ? C7 C8 C9 117.7(13) . . ? C10 C9 C8 119.7(13) . . ? C9 C10 C11 119.8(13) . . ? N6 C11 C10 121.1(11) . . ? N6 C11 C12 115.6(10) . . ? C10 C11 C12 123.4(11) . . ? N13 C12 C16 109.4(10) . . ? N13 C12 C11 119.8(10) . . ? C16 C12 C11 130.7(10) . . ? C12 N13 N14 108.4(8) . . ? C12 N13 Ag1 118.0(7) . . ? N14 N13 Ag1 132.7(7) . . ? C15 N14 N13 108.2(9) . . ? C15 N14 Ag2 138.6(8) . 2 ? N13 N14 Ag2 111.9(6) . 2 ? N14 C15 C16 108.6(9) . . ? N14 C15 C17B 122.6(13) . . ? C16 C15 C17B 128.4(12) . . ? N14 C15 C17A 120.0(14) . . ? C16 C15 C17A 131.2(13) . . ? C12 C16 C15 105.3(10) . . ? C18B C17B C20B 111.6(15) . . ? C18B C17B C15 109.9(13) . . ? C20B C17B C15 109.2(14) . . ? C18B C17B C19B 109.0(14) . . ? C20B C17B C19B 106.5(14) . . ? C15 C17B C19B 110.6(17) . . ? C19A C17A C15 118(4) . . ? C19A C17A C20A 108.4(17) . . ? C15 C17A C20A 108.2(16) . . ? C19A C17A C18A 107.8(17) . . ? C15 C17A C18A 107.2(15) . . ? C20A C17A C18A 106.3(17) . . ? C22 N21 C26 117.0(12) . . ? C22 N21 Ag2 132.8(10) . . ? C26 N21 Ag2 108.8(8) . . ? N21 C22 C23 124.0(15) . . ? C24 C23 C22 118.0(14) . . ? C23 C24 C25 119.2(14) . . ? C26 C25 C24 118.7(15) . . ? N21 C26 C25 122.9(13) . . ? N21 C26 C27 116.9(11) . . ? C25 C26 C27 120.1(12) . . ? N28 C27 C31 107.4(11) . . ? N28 C27 C26 120.1(11) . . ? C31 C27 C26 132.3(11) . . ? C27 N28 N29 109.4(9) . . ? C27 N28 Ag2 122.2(8) . . ? N29 N28 Ag2 128.4(7) . . ? C30 N29 N28 108.8(9) . . ? C30 N29 Ag3 135.9(8) . . ? N28 N29 Ag3 115.2(7) . . ? N29 C30 C31 107.4(10) . . ? N29 C30 C32 124.8(10) . . ? C31 C30 C32 127.7(10) . . ? C27 C31 C30 106.9(10) . . ? C33A C32 C30 110.9(12) . . ? C33A C32 C35A 109.8(13) . . ? C30 C32 C35A 109.5(11) . . ? C33A C32 C34A 108.1(13) . . ? C30 C32 C34A 111.5(11) . . ? C35A C32 C34A 107.0(12) . . ? C34B C32 C30 110.4(13) . . ? C34B C32 C35B 109.9(15) . . ? C30 C32 C35B 109.2(14) . . ? C34B C32 C33B 109.7(14) . . ? C30 C32 C33B 109.0(14) . . ? C35B C32 C33B 108.7(14) . . ? C37 N36 C41 118.6(12) . . ? C37 N36 Ag4 132.1(10) . . ? C41 N36 Ag4 109.3(8) . . ? N36 C37 C38 123.8(15) . . ? C37 C38 C39 118.5(15) . . ? C38 C39 C40 118.6(15) . . ? C39 C40 C41 119.5(14) . . ? N36 C41 C40 121.0(12) . . ? N36 C41 C42 117.4(11) . . ? C40 C41 C42 121.4(12) . . ? N43 C42 C46 107.7(10) . . ? N43 C42 C41 120.6(10) . . ? C46 C42 C41 131.7(11) . . ? C42 N43 N44 109.7(9) . . ? C42 N43 Ag4 122.3(8) . . ? N44 N43 Ag4 128.0(7) . . ? N43 N44 C45 108.5(10) . . ? N43 N44 Ag3 114.6(7) . . ? C45 N44 Ag3 136.6(8) . . ? N44 C45 C46 108.0(10) . . ? N44 C45 C47 121.7(10) . . ? C46 C45 C47 130.3(10) . . ? C42 C46 C45 106.0(10) . . ? C45 C47 C48 110.7(11) . . ? C45 C47 C50 109.3(10) . . ? C48 C47 C50 108.7(11) . . ? C45 C47 C49 109.7(10) . . ? C48 C47 C49 109.4(12) . . ? C50 C47 C49 109.0(11) . . ? C52 N51 C56 118.5(10) . . ? C52 N51 Ag5 128.6(8) . . ? C56 N51 Ag5 112.4(7) . . ? N51 C52 C53 123.7(12) . . ? C52 C53 C54 118.7(12) . . ? C53 C54 C55 118.6(12) . . ? C54 C55 C56 119.6(12) . . ? N51 C56 C55 120.8(11) . . ? N51 C56 C57 117.9(9) . . ? C55 C56 C57 121.3(11) . . ? N58 C57 C61 110.2(10) . . ? N58 C57 C56 117.8(10) . . ? C61 C57 C56 132.1(11) . . ? C57 N58 N59 107.3(9) . . ? C57 N58 Ag5 119.6(7) . . ? N59 N58 Ag5 131.6(8) . . ? N58 N59 C60 110.3(10) . . ? N58 N59 Ag4 113.4(7) . 2 ? C60 N59 Ag4 135.1(8) . 2 ? N59 C60 C61 107.0(9) . . ? N59 C60 C62B 117.1(13) . . ? C61 C60 C62B 133.9(12) . . ? N59 C60 C62A 126.4(11) . . ? C61 C60 C62A 125.1(11) . . ? C57 C61 C60 105.3(10) . . ? C65A C62A C63A 111.3(13) . . ? C65A C62A C64A 108.2(13) . . ? C63A C62A C64A 107.8(13) . . ? C65A C62A C60 110.3(12) . . ? C63A C62A C60 109.0(12) . . ? C64A C62A C60 110.2(13) . . ? C65B C62B C64B 110.6(15) . . ? C65B C62B C63B 108.4(15) . . ? C64B C62B C63B 109.8(15) . . ? C65B C62B C60 109.2(14) . . ? C64B C62B C60 108.4(15) . . ? C63B C62B C60 110.4(15) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 28.11 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 3.895 _refine_diff_density_min -2.249 _refine_diff_density_rms 0.334 #=END data_jjh38a_(compound_4) _database_code_depnum_ccdc_archive 'CCDC 806537' #TrackingRef '- Ag Chem Comm.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis[3-isoquinolinyl-5-tertbutylpyrazolido]tetrasilver(I) hydrate (3/2.7) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H64 Ag4 N12, 2.7[H2 O]' _chemical_formula_sum 'C64 H69.40 Ag4 N12 O2.70' _chemical_formula_weight 1481.40 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' Ag Ag -0.8971 1.1015 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'F d d 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+1/4, -y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+1/4, -y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+3/4, -y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' _cell_length_a 18.6771(12) _cell_length_b 44.784(3) _cell_length_c 17.1502(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14344.9(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 49319 _cell_measurement_theta_min 2.11 _cell_measurement_theta_max 28.87 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5976 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.671 _exptl_absorpt_correction_T_max 0.697 _exptl_absorpt_process_details ; Sheldrick, G. M. (2002). SADABS v. 2.03. University of G/ottingen, Germany. ; _exptl_special_details ; Rotating anode power 3 kW. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 Apex diffractometer' _diffrn_measurement_method 'Rotation images' _diffrn_detector_area_resol_mean '120 microns' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49319 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -60 _diffrn_reflns_limit_k_max 59 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 28.87 _reflns_number_total 9369 _reflns_number_gt 8111 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX 2 software, Bruker Nonius 2004' _computing_cell_refinement 'APEX 2 software, Bruker Nonius 2004' _computing_data_reduction 'SAINT, Bruker Nonius 2004' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSEED (Barbour, 2001)' _computing_publication_material 'local program' _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. The asymmetric unit contains half a complex molecule, with Ag2 and Ag3 lying on the crystallographic C~2~ axis 0.25, 0.25, z, and a series of weak Fourier peaks that are not bonded to any other atom that were modelled as partial water molecules. The occupancies of these partial water sites sum to 1.35, or 2.7 per formula unit. The presence of ca. 3 molar equiv of water in the bulk material is supported by elemental microanalysis. One of the two unique tertbutyl groups in the model, C38--C41, is disordered over two equally occupied sites labelled 'A' and 'B'. This was refined with the fixed restraints C---C = 1.52(2) and 1,3-C...C = 2.48(2) \%A. All non-H atoms were refined anistropically, and C-bound H atoms were placed in calculated positions and refined using a riding model. The partial water H atoms were not located or refined, but were included in the density and F(000) calculations. ; _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^)+(0.0789P)^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 -0.02(3) _refine_ls_number_reflns 9369 _refine_ls_number_parameters 423 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.245326(15) 0.178016(9) 0.61882(2) 0.04803(10) Uani 1 1 d . . . Ag2 Ag 0.2500 0.2500 0.67631(3) 0.04000(11) Uani 1 2 d S . . Ag3 Ag 0.2500 0.2500 0.49716(2) 0.03316(10) Uani 1 2 d S . . N4 N 0.33822(17) 0.14129(7) 0.6135(2) 0.0424(7) Uani 1 1 d . . . C5 C 0.3411(3) 0.11567(9) 0.6593(3) 0.0514(11) Uani 1 1 d . . . H5 H 0.3030 0.1116 0.6945 0.062 Uiso 1 1 calc R . . C6 C 0.3980(3) 0.09596(10) 0.6550(3) 0.0515(11) Uani 1 1 d . . . H6 H 0.4011 0.0797 0.6904 0.062 Uiso 1 1 calc R . . C7 C 0.4517(2) 0.10015(9) 0.5973(3) 0.0436(9) Uani 1 1 d . . . C8 C 0.5106(3) 0.07925(12) 0.5875(4) 0.0577(13) Uani 1 1 d . . . H8 H 0.5157 0.0629 0.6225 0.069 Uiso 1 1 calc R . . C9 C 0.5588(3) 0.08297(11) 0.5280(4) 0.0652(15) Uani 1 1 d . . . H9 H 0.5991 0.0701 0.5241 0.078 Uiso 1 1 calc R . . C10 C 0.5487(3) 0.10619(11) 0.4721(4) 0.0660(16) Uani 1 1 d . . . H10 H 0.5781 0.1070 0.4270 0.079 Uiso 1 1 calc R . . C11 C 0.4954(2) 0.12783(10) 0.4834(3) 0.0469(10) Uani 1 1 d . . . H11 H 0.4916 0.1442 0.4483 0.056 Uiso 1 1 calc R . . C12 C 0.4473(2) 0.12546(8) 0.5470(3) 0.0369(8) Uani 1 1 d . . . C13 C 0.39021(19) 0.14714(8) 0.5624(2) 0.0338(7) Uani 1 1 d . . . C14 C 0.3871(2) 0.17675(8) 0.5238(2) 0.0323(7) Uani 1 1 d . . . N15 N 0.32377(17) 0.19146(7) 0.52683(19) 0.0350(7) Uani 1 1 d . . . N16 N 0.33564(17) 0.21976(6) 0.4946(2) 0.0334(6) Uani 1 1 d . . . C17 C 0.4056(2) 0.22180(8) 0.4718(2) 0.0326(7) Uani 1 1 d . . . C18 C 0.4406(2) 0.19494(8) 0.4893(2) 0.0332(7) Uani 1 1 d . . . H18 H 0.4894 0.1900 0.4801 0.040 Uiso 1 1 calc R . . C19 C 0.4353(2) 0.25074(7) 0.4343(2) 0.0352(8) Uani 1 1 d . . . C20 C 0.5158(2) 0.24589(9) 0.4147(3) 0.0427(10) Uani 1 1 d . . . H20A H 0.5204 0.2301 0.3754 0.064 Uiso 1 1 calc R . . H20B H 0.5416 0.2400 0.4621 0.064 Uiso 1 1 calc R . . H20C H 0.5362 0.2645 0.3944 0.064 Uiso 1 1 calc R . . C21 C 0.4292(2) 0.27699(8) 0.4929(3) 0.0415(9) Uani 1 1 d . . . H21A H 0.4511 0.2949 0.4703 0.062 Uiso 1 1 calc R . . H21B H 0.4541 0.2718 0.5413 0.062 Uiso 1 1 calc R . . H21C H 0.3786 0.2809 0.5041 0.062 Uiso 1 1 calc R . . C22 C 0.3932(2) 0.25796(10) 0.3590(3) 0.0446(9) Uani 1 1 d . . . H22A H 0.3949 0.2407 0.3237 0.067 Uiso 1 1 calc R . . H22B H 0.4147 0.2753 0.3332 0.067 Uiso 1 1 calc R . . H22C H 0.3433 0.2624 0.3722 0.067 Uiso 1 1 calc R . . N23 N 0.1311(2) 0.28200(9) 0.7572(3) 0.0624(12) Uani 1 1 d . . . C24 C 0.1250(4) 0.31118(14) 0.7779(4) 0.0767(18) Uani 1 1 d . . . H24 H 0.1637 0.3202 0.8051 0.092 Uiso 1 1 calc R . . C25 C 0.0641(4) 0.32889(12) 0.7612(4) 0.0717(17) Uani 1 1 d . . . H25 H 0.0618 0.3491 0.7775 0.086 Uiso 1 1 calc R . . C26 C 0.0061(3) 0.31555(12) 0.7193(4) 0.0601(14) Uani 1 1 d . . . C27 C -0.0548(4) 0.33165(14) 0.6980(5) 0.080(2) Uani 1 1 d . . . H27 H -0.0598 0.3519 0.7138 0.096 Uiso 1 1 calc R . . C28 C -0.1077(4) 0.31836(15) 0.6544(5) 0.084(2) Uani 1 1 d . . . H28 H -0.1488 0.3296 0.6401 0.101 Uiso 1 1 calc R . . C29 C -0.1019(3) 0.28848(14) 0.6305(4) 0.0697(15) Uani 1 1 d . . . H29 H -0.1383 0.2798 0.5992 0.084 Uiso 1 1 calc R . . C30 C -0.0438(3) 0.27178(11) 0.6524(3) 0.0510(10) Uani 1 1 d . . . H30 H -0.0415 0.2514 0.6376 0.061 Uiso 1 1 calc R . . C31 C 0.0127(3) 0.28428(11) 0.6964(3) 0.0470(10) Uani 1 1 d . . . C32 C 0.0772(2) 0.26836(10) 0.7196(3) 0.0435(10) Uani 1 1 d . . . C33 C 0.0868(2) 0.23589(9) 0.7038(2) 0.0381(8) Uani 1 1 d . . . N34 N 0.15293(17) 0.22617(7) 0.6803(2) 0.0378(7) Uani 1 1 d . . . N35 N 0.15093(17) 0.19535(7) 0.6736(2) 0.0375(7) Uani 1 1 d . A . C36 C 0.0839(2) 0.18602(8) 0.6939(2) 0.0381(8) Uani 1 1 d D . . C37 C 0.0420(2) 0.21121(9) 0.7131(3) 0.0391(9) Uani 1 1 d . A . H37 H -0.0067 0.2113 0.7290 0.047 Uiso 1 1 calc R . . C38A C 0.0656(7) 0.1529(2) 0.6989(8) 0.041(4) Uani 0.50 1 d PD A 1 C39A C 0.0578(8) 0.1414(3) 0.6158(7) 0.083(4) Uani 0.50 1 d PD A 1 H39A H 0.0190 0.1522 0.5896 0.125 Uiso 0.50 1 calc PR A 1 H39B H 0.0466 0.1200 0.6168 0.125 Uiso 0.50 1 calc PR A 1 H39C H 0.1027 0.1446 0.5874 0.125 Uiso 0.50 1 calc PR A 1 C40A C -0.0066(6) 0.1491(3) 0.7423(10) 0.076(6) Uani 0.50 1 d PD A 1 H40A H -0.0438 0.1606 0.7153 0.114 Uiso 0.50 1 calc PR A 1 H40B H -0.0017 0.1565 0.7959 0.114 Uiso 0.50 1 calc PR A 1 H40C H -0.0199 0.1280 0.7432 0.114 Uiso 0.50 1 calc PR A 1 C41A C 0.1224(6) 0.1358(3) 0.7448(12) 0.135(10) Uani 0.50 1 d PD A 1 H41A H 0.1094 0.1146 0.7470 0.203 Uiso 0.50 1 calc PR A 1 H41B H 0.1253 0.1438 0.7979 0.203 Uiso 0.50 1 calc PR A 1 H41C H 0.1689 0.1380 0.7190 0.203 Uiso 0.50 1 calc PR A 1 C38B C 0.0575(9) 0.1547(3) 0.6910(10) 0.067(7) Uani 0.50 1 d PD A 2 C39B C -0.0017(8) 0.1522(4) 0.6296(10) 0.108(7) Uani 0.50 1 d PD A 2 H39D H -0.0190 0.1316 0.6273 0.162 Uiso 0.50 1 calc PR A 2 H39E H 0.0174 0.1580 0.5785 0.162 Uiso 0.50 1 calc PR A 2 H39F H -0.0414 0.1655 0.6436 0.162 Uiso 0.50 1 calc PR A 2 C40B C 0.0245(8) 0.1456(3) 0.7703(8) 0.076(5) Uani 0.50 1 d PD A 2 H40D H 0.0609 0.1474 0.8112 0.115 Uiso 0.50 1 calc PR A 2 H40E H 0.0077 0.1249 0.7675 0.115 Uiso 0.50 1 calc PR A 2 H40F H -0.0159 0.1588 0.7823 0.115 Uiso 0.50 1 calc PR A 2 C41B C 0.1179(9) 0.1329(3) 0.6703(14) 0.162(14) Uani 0.50 1 d PD A 2 H41D H 0.1567 0.1348 0.7085 0.244 Uiso 0.50 1 calc PR A 2 H41E H 0.1362 0.1375 0.6182 0.244 Uiso 0.50 1 calc PR A 2 H41F H 0.0995 0.1124 0.6712 0.244 Uiso 0.50 1 calc PR A 2 O42 O 0.0000 0.0000 0.8702(15) 0.065(5) Uiso 0.30 2 d SP B 1 O43 O 0.0533(6) 0.0613(2) 0.7990(7) 0.065(3) Uiso 0.35 1 d P C 2 O44 O 0.1076(10) 0.0501(4) 0.7992(12) 0.082(5) Uiso 0.25 1 d P D 3 O45 O 0.2317(10) 0.2574(4) 0.8708(12) 0.072(4) Uiso 0.25 1 d P . . O46 O 0.2697(14) 0.3081(6) 0.9052(17) 0.062(6) Uiso 0.15 1 d P E 5 O47 O 0.1643(11) 0.1856(4) 0.9025(13) 0.069(5) Uiso 0.20 1 d P F 6 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 0.03069(15) 0.0613(2) 0.0521(2) -0.00585(16) 0.01379(14) -0.00131(12) Ag2 0.0307(2) 0.0545(2) 0.0349(2) 0.000 0.000 -0.01128(17) Ag3 0.02859(19) 0.03776(19) 0.0331(2) 0.000 0.000 0.00962(14) N4 0.0396(16) 0.0379(16) 0.0498(19) 0.0087(15) 0.0098(17) 0.0011(13) C5 0.051(3) 0.046(2) 0.057(3) 0.015(2) 0.016(2) -0.0029(18) C6 0.059(3) 0.042(2) 0.053(3) 0.0182(19) 0.003(2) -0.0012(19) C7 0.044(2) 0.0347(18) 0.052(3) 0.0107(17) -0.0043(19) -0.0014(15) C8 0.061(3) 0.041(2) 0.071(4) 0.017(2) -0.006(3) 0.0093(19) C9 0.048(3) 0.048(2) 0.100(5) 0.020(3) 0.013(3) 0.015(2) C10 0.051(3) 0.047(2) 0.099(4) 0.016(3) 0.028(3) 0.019(2) C11 0.043(2) 0.039(2) 0.058(3) 0.010(2) 0.0127(18) 0.0100(15) C12 0.0338(18) 0.0304(16) 0.047(2) 0.0051(16) -0.0001(17) 0.0036(13) C13 0.0311(17) 0.0301(16) 0.040(2) 0.0024(14) -0.0003(15) 0.0009(13) C14 0.0316(19) 0.0342(17) 0.0312(18) 0.0036(13) 0.0019(14) 0.0040(13) N15 0.0345(17) 0.0356(16) 0.0348(16) 0.0066(12) 0.0060(13) 0.0053(12) N16 0.0309(15) 0.0328(14) 0.0364(16) 0.0065(13) 0.0053(13) 0.0052(11) C17 0.0316(18) 0.0374(17) 0.0288(17) 0.0005(13) 0.0064(14) 0.0047(14) C18 0.0292(17) 0.0377(18) 0.0328(18) 0.0009(15) 0.0064(15) 0.0072(13) C19 0.039(2) 0.0353(18) 0.0317(18) 0.0094(14) 0.0044(17) 0.0030(13) C20 0.038(2) 0.044(2) 0.046(2) 0.0112(17) 0.0089(18) 0.0004(15) C21 0.049(2) 0.0334(18) 0.042(2) 0.0071(16) 0.0033(18) 0.0064(15) C22 0.050(2) 0.049(2) 0.035(2) 0.0125(17) 0.0070(19) 0.0033(18) N23 0.051(2) 0.061(2) 0.075(3) -0.019(2) 0.013(2) -0.0176(19) C24 0.069(4) 0.074(4) 0.087(5) -0.021(3) 0.015(3) -0.030(3) C25 0.088(4) 0.047(3) 0.080(4) -0.018(3) 0.029(3) -0.016(3) C26 0.071(4) 0.046(2) 0.063(3) -0.006(2) 0.031(3) 0.003(2) C27 0.087(5) 0.057(3) 0.094(5) -0.004(3) 0.035(4) 0.019(3) C28 0.080(4) 0.072(4) 0.099(5) 0.004(4) 0.014(4) 0.035(3) C29 0.056(3) 0.081(4) 0.072(4) -0.009(3) -0.004(3) 0.019(3) C30 0.050(3) 0.054(2) 0.049(2) -0.008(2) 0.008(2) 0.007(2) C31 0.051(3) 0.051(2) 0.039(2) -0.0049(18) 0.0155(19) -0.0007(18) C32 0.041(2) 0.046(2) 0.043(2) -0.0048(17) 0.0153(18) -0.0040(17) C33 0.036(2) 0.043(2) 0.036(2) -0.0045(16) 0.0032(15) -0.0048(16) N34 0.0293(15) 0.0430(16) 0.0409(18) 0.0003(14) 0.0018(14) -0.0068(12) N35 0.0314(16) 0.0419(16) 0.0393(18) 0.0026(14) 0.0082(14) -0.0006(12) C36 0.035(2) 0.044(2) 0.0347(19) 0.0016(16) 0.0053(16) -0.0054(15) C37 0.0278(18) 0.048(2) 0.042(2) -0.0078(17) 0.0103(15) -0.0082(16) C38A 0.039(7) 0.024(6) 0.062(10) 0.005(5) 0.027(6) -0.003(5) C39A 0.087(9) 0.081(8) 0.081(9) -0.040(7) 0.037(8) -0.025(7) C40A 0.056(8) 0.061(8) 0.110(14) -0.039(9) 0.042(8) -0.029(7) C41A 0.042(7) 0.106(11) 0.26(3) 0.130(16) 0.012(11) 0.000(6) C38B 0.072(13) 0.074(14) 0.056(11) 0.007(10) 0.015(9) -0.014(10) C39B 0.100(13) 0.112(14) 0.112(15) -0.004(11) -0.007(9) -0.065(10) C40B 0.095(13) 0.060(7) 0.075(10) 0.010(7) 0.048(10) -0.003(9) C41B 0.153(19) 0.056(8) 0.28(3) -0.057(13) 0.17(2) -0.047(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N35 2.143(3) . ? Ag1 N15 2.236(3) . ? Ag1 N4 2.392(3) . ? Ag1 Ag2 3.3722(4) . ? Ag1 Ag3 3.8410(5) . ? Ag2 N34 2.105(3) . ? Ag2 Ag3 3.0724(6) . ? Ag3 N16 2.096(3) . ? N4 C13 1.334(5) . ? N4 C5 1.392(5) . ? C5 C6 1.383(7) . ? C6 C7 1.422(7) . ? C7 C12 1.427(5) . ? C7 C8 1.454(7) . ? C8 C9 1.371(8) . ? C9 C10 1.428(7) . ? C10 C11 1.402(6) . ? C11 C12 1.417(6) . ? C12 C13 1.466(5) . ? C13 C14 1.483(5) . ? C14 N15 1.355(5) . ? C14 C18 1.419(5) . ? N15 N16 1.400(4) . ? N16 C17 1.367(5) . ? C17 C18 1.402(5) . ? C17 C19 1.549(5) . ? C19 C22 1.547(6) . ? C19 C21 1.551(6) . ? C19 C20 1.556(6) . ? N23 C32 1.343(6) . ? N23 C24 1.359(7) . ? C24 C25 1.415(10) . ? C25 C26 1.431(9) . ? C26 C27 1.396(9) . ? C26 C31 1.459(7) . ? C27 C28 1.374(11) . ? C28 C29 1.403(9) . ? C29 C30 1.370(7) . ? C30 C31 1.414(7) . ? C31 C32 1.455(7) . ? C32 C33 1.490(6) . ? C33 N34 1.370(5) . ? C33 C37 1.396(6) . ? N34 N35 1.386(4) . ? N35 C36 1.364(5) . ? C36 C37 1.413(6) . ? C36 C38B 1.489(15) . ? C36 C38A 1.525(11) . ? C38A C39A 1.523(14) . ? C38A C41A 1.527(15) . ? C38A C40A 1.550(13) . ? C38B C39B 1.531(16) . ? C38B C41B 1.534(16) . ? C38B C40B 1.546(15) . ? 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 N35 Ag1 N15 138.66(12) . . ? N35 Ag1 N4 149.58(13) . . ? N15 Ag1 N4 71.52(11) . . ? N34 Ag2 N34 176.2(2) 14 . ? N16 Ag3 N16 177.6(2) 14 . ? C13 N4 C5 120.3(3) . . ? C13 N4 Ag1 114.7(2) . . ? C5 N4 Ag1 125.0(3) . . ? C6 C5 N4 121.7(4) . . ? C5 C6 C7 119.7(4) . . ? C6 C7 C12 119.0(4) . . ? C6 C7 C8 122.0(4) . . ? C12 C7 C8 119.0(4) . . ? C9 C8 C7 120.3(4) . . ? C8 C9 C10 120.1(4) . . ? C11 C10 C9 120.3(5) . . ? C10 C11 C12 120.3(4) . . ? C11 C12 C7 119.2(4) . . ? C11 C12 C13 123.4(4) . . ? C7 C12 C13 117.3(4) . . ? N4 C13 C12 121.2(3) . . ? N4 C13 C14 116.1(3) . . ? C12 C13 C14 122.7(3) . . ? N15 C14 C18 110.6(3) . . ? N15 C14 C13 116.9(3) . . ? C18 C14 C13 132.2(3) . . ? C14 N15 N16 106.7(3) . . ? C14 N15 Ag1 117.9(2) . . ? N16 N15 Ag1 128.7(2) . . ? C17 N16 N15 109.0(3) . . ? C17 N16 Ag3 133.8(2) . . ? N15 N16 Ag3 117.1(2) . . ? N16 C17 C18 109.1(3) . . ? N16 C17 C19 121.2(3) . . ? C18 C17 C19 129.7(3) . . ? C17 C18 C14 104.7(3) . . ? C22 C19 C17 109.8(3) . . ? C22 C19 C21 110.2(3) . . ? C17 C19 C21 109.8(3) . . ? C22 C19 C20 109.9(4) . . ? C17 C19 C20 108.6(3) . . ? C21 C19 C20 108.5(4) . . ? C32 N23 C24 120.0(5) . . ? N23 C24 C25 123.6(6) . . ? C24 C25 C26 118.4(5) . . ? C27 C26 C25 122.2(6) . . ? C27 C26 C31 119.6(6) . . ? C25 C26 C31 118.1(5) . . ? C28 C27 C26 120.3(6) . . ? C27 C28 C29 121.1(6) . . ? C30 C29 C28 120.1(6) . . ? C29 C30 C31 121.4(5) . . ? C30 C31 C32 124.8(4) . . ? C30 C31 C26 117.4(5) . . ? C32 C31 C26 117.8(5) . . ? N23 C32 C31 122.0(4) . . ? N23 C32 C33 116.2(4) . . ? C31 C32 C33 121.8(4) . . ? N34 C33 C37 108.8(4) . . ? N34 C33 C32 118.2(3) . . ? C37 C33 C32 132.8(4) . . ? C33 N34 N35 108.5(3) . . ? C33 N34 Ag2 128.7(3) . . ? N35 N34 Ag2 121.7(2) . . ? C36 N35 N34 107.9(3) . . ? C36 N35 Ag1 139.1(3) . . ? N34 N35 Ag1 112.0(2) . . ? N35 C36 C37 108.9(3) . . ? N35 C36 C38B 125.8(7) . . ? C37 C36 C38B 125.2(7) . . ? N35 C36 C38A 121.2(6) . . ? C37 C36 C38A 129.8(6) . . ? C33 C37 C36 105.8(3) . . ? C39A C38A C36 107.3(9) . . ? C39A C38A C41A 112.3(11) . . ? C36 C38A C41A 111.1(10) . . ? C39A C38A C40A 109.3(10) . . ? C36 C38A C40A 109.1(9) . . ? C41A C38A C40A 107.6(10) . . ? C36 C38B C39B 109.3(11) . . ? C36 C38B C41B 111.3(11) . . ? C39B C38B C41B 109.0(13) . . ? C36 C38B C40B 110.5(12) . . ? C39B C38B C40B 107.4(12) . . ? C41B C38B C40B 109.2(12) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.87 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.939 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.112