# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Neil Champness' 'Alexander J. Blake' 'Neil Champness' 'Olege V. Dolomanov' 'Martin Schroder' 'Claire Wilson' _publ_contact_author_name 'Dr Neil Champness' _publ_contact_author_address ; School of Chemistry University of Nottingham University Park Nottingham NG7 2RD UNITED KINGDOM ; _publ_contact_author_email NEIL.CHAMPNESS@NOTTINGHAM.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; A Novel Synthetic Strategy for Hexanuclear Supramolecular Architectures ; data_Compund_1(PYYNCU) _database_code_CSD 201515 _refine_special_details ; Distance and similarity restraints were applied to B-F bonds. The PLATON SQUEEZE procedure was used to treat regions of diffuse solvent which could not be sensibly modelled in terms of atomic sites. Their contribution to the diffraction pattern was removed and modified F(obs)**2 written to a new HKL file. The number of electrons thus located, 1791 per unit cell, are included in the formula, formula weight, calculated density, mu and F(000). This residual electron density was assigned to two molecules of the DMF solvent and 0.3367 counteranions [1791/18 = 100 e per ligand; 100 - 41*0.3367 (BF4) = 87 e. Two molecules of DMF would give 80 e.] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl cupper(I) tetrafluoroborate hexamer ; _chemical_name_common ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl cupper(I) tetrafluoroborate hexamer ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 B Cu F4 N6 O2' _chemical_formula_weight 654.93 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M 'R -3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.467(2) _cell_length_b 20.467(2) _cell_length_c 40.139(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 14561(3) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4997 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 20.75 _exptl_crystal_description block _exptl_crystal_colour 'deep red' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method ? _exptl_crystal_F_000 6048 _exptl_absorpt_coefficient_mu 0.734 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details . _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 30887 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.086 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -53 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 28.86 _reflns_number_total 7646 _reflns_number_gt 3221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OLEX (Dolomanov, 2001)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2003)' _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^)+(0.158P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7646 _refine_ls_number_parameters 300 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.1270 _refine_ls_R_factor_gt 0.0761 _refine_ls_wR_factor_ref 0.2416 _refine_ls_wR_factor_gt 0.2204 _refine_ls_goodness_of_fit_ref 0.828 _refine_ls_restrained_S_all 0.834 _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 0.74946(3) 0.63369(3) 0.251095(14) 0.0630(2) Uani 1 1 d . . . N1 N 0.8326(2) 0.68996(18) 0.21603(8) 0.0544(9) Uani 1 1 d . . . C2 C 0.8385(3) 0.7550(2) 0.20454(10) 0.0546(11) Uani 1 1 d . . . C3 C 0.8982(3) 0.8050(2) 0.18445(11) 0.0613(12) Uani 1 1 d . . . H3A H 0.9010 0.8501 0.1767 0.074 Uiso 1 1 calc R . . C4 C 0.9544(3) 0.7877(2) 0.17579(12) 0.0673(13) Uani 1 1 d . . . H4A H 0.9958 0.8211 0.1622 0.081 Uiso 1 1 calc R . . C5 C 0.9488(3) 0.7225(2) 0.18707(12) 0.0641(12) Uani 1 1 d . . . H5 H 0.9860 0.7094 0.1816 0.077 Uiso 1 1 calc R . . C6 C 0.8869(3) 0.6749(2) 0.20704(11) 0.0551(11) Uani 1 1 d . . . C7 C 0.8783(3) 0.6032(3) 0.21945(12) 0.0664(13) Uani 1 1 d . . . C8 C 0.8758(3) 0.5466(3) 0.22644(13) 0.0657(13) Uani 1 1 d . . . C9 C 0.8786(3) 0.4792(2) 0.23369(11) 0.0597(12) Uani 1 1 d . . . C10 C 0.8230(3) 0.4209(3) 0.25345(13) 0.0664(13) Uani 1 1 d . . . H10A H 0.7843 0.4264 0.2638 0.080 Uiso 1 1 calc R . . C11 C 0.8262(3) 0.3563(3) 0.25743(12) 0.0632(12) Uani 1 1 d . . . H11A H 0.7878 0.3168 0.2703 0.076 Uiso 1 1 calc R . . N12 N 0.8797(2) 0.3449(2) 0.24445(9) 0.0553(9) Uani 1 1 d . . . C13 C 0.9328(3) 0.4010(3) 0.22615(12) 0.0648(12) Uani 1 1 d . . . H13A H 0.9711 0.3937 0.2166 0.078 Uiso 1 1 calc R . . C14 C 0.9358(3) 0.4684(3) 0.22016(12) 0.0633(12) Uani 1 1 d . . . H14A H 0.9753 0.5067 0.2073 0.076 Uiso 1 1 calc R . . N1' N 0.7293(2) 0.7225(2) 0.23891(9) 0.0621(10) Uani 1 1 d . . . C2' C 0.7765(3) 0.7688(3) 0.21445(11) 0.0599(11) Uani 1 1 d . . . C3' C 0.7639(3) 0.8237(3) 0.19897(14) 0.0781(15) Uani 1 1 d . . . H3'A H 0.7964 0.8544 0.1816 0.094 Uiso 1 1 calc R . . C4' C 0.7054(4) 0.8321(3) 0.20903(15) 0.0930(18) Uani 1 1 d . . . H4'A H 0.6960 0.8683 0.1987 0.112 Uiso 1 1 calc R . . C5' C 0.6592(4) 0.7868(3) 0.23478(15) 0.0953(19) Uani 1 1 d . . . H5'A H 0.6191 0.7932 0.2428 0.114 Uiso 1 1 calc R . . C6' C 0.6725(3) 0.7326(3) 0.24840(13) 0.0718(13) Uani 1 1 d . . . C7' C 0.6247(4) 0.6818(3) 0.27497(14) 0.0882(17) Uani 1 1 d . . . C8' C 0.6006(5) 0.6381(4) 0.29606(15) 0.115(2) Uani 1 1 d . . . C9' C 0.5589(4) 0.5808(3) 0.32164(14) 0.0887(18) Uani 1 1 d . . . C10' C 0.5898(3) 0.5406(3) 0.33361(14) 0.0902(18) Uani 1 1 d . . . H10B H 0.6361 0.5484 0.3247 0.108 Uiso 1 1 calc R . . C11' C 0.5544(3) 0.4880(3) 0.35881(13) 0.0843(17) Uani 1 1 d . . . H11B H 0.5780 0.4613 0.3669 0.101 Uiso 1 1 calc R . . N12' N 0.4895(2) 0.4738(2) 0.37194(10) 0.0708(11) Uani 1 1 d . . . C13' C 0.4578(4) 0.5096(5) 0.35908(18) 0.133(3) Uani 1 1 d . . . H13B H 0.4091 0.4974 0.3669 0.159 Uiso 1 1 calc R . . C14' C 0.4907(5) 0.5641(5) 0.3349(2) 0.154(4) Uani 1 1 d . . . H14B H 0.4660 0.5901 0.3273 0.185 Uiso 1 1 calc R . . B1 B 0.6667 0.3333 0.3333 0.040(5) Uiso 0.48 6 d SPD . . F1 F 0.6667 0.3333 0.3002(3) 0.047(4) Uiso 0.24 3 d SPD . . F2 F 0.6327(12) 0.3756(12) 0.3434(4) 0.143(6) Uiso 0.24 1 d PD . . B10 B 0.6667 0.3333 0.1882(2) 0.065(2) Uiso 1 3 d SD . . F11 F 0.6667 0.3333 0.22368(15) 0.1103(19) Uiso 1 3 d SD . . F12 F 0.63239(15) 0.37367(15) 0.17761(6) 0.0668(7) Uiso 1 1 d D . . B20 B 0.3302(9) 0.4497(8) 0.1858(4) 0.059(5) Uiso 0.25 1 d PD . . F21 F 0.2942(6) 0.3947(6) 0.1632(2) 0.070(3) Uiso 0.25 1 d PD . . F22 F 0.2929(15) 0.4904(15) 0.1921(7) 0.290(16) Uiso 0.25 1 d PD . . F23 F 0.4037(11) 0.5018(13) 0.1769(7) 0.311(18) Uiso 0.25 1 d PD . . F24 F 0.3334(17) 0.4186(15) 0.2167(5) 0.296(16) Uiso 0.25 1 d PD . . 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 0.0616(4) 0.0453(3) 0.0656(4) 0.0143(3) -0.0128(3) 0.0144(3) N1 0.057(2) 0.0407(19) 0.056(2) 0.0025(16) -0.0145(17) 0.0177(17) C2 0.059(3) 0.043(2) 0.055(2) 0.0045(19) -0.009(2) 0.021(2) C3 0.060(3) 0.041(2) 0.071(3) 0.011(2) 0.000(2) 0.016(2) C4 0.068(3) 0.039(2) 0.076(3) 0.004(2) -0.003(3) 0.013(2) C5 0.066(3) 0.046(3) 0.072(3) -0.002(2) -0.012(2) 0.021(2) C6 0.062(3) 0.031(2) 0.063(3) -0.0012(19) -0.016(2) 0.016(2) C7 0.070(3) 0.055(3) 0.067(3) 0.001(2) -0.014(2) 0.026(3) C8 0.072(3) 0.049(3) 0.077(3) 0.003(2) -0.008(2) 0.031(2) C9 0.068(3) 0.047(3) 0.064(3) -0.004(2) -0.014(2) 0.029(2) C10 0.061(3) 0.058(3) 0.087(3) 0.010(3) 0.007(3) 0.035(2) C11 0.065(3) 0.049(3) 0.083(3) 0.012(2) 0.013(2) 0.034(2) N12 0.060(2) 0.055(2) 0.059(2) 0.0056(17) 0.0104(18) 0.0343(19) C13 0.072(3) 0.066(3) 0.066(3) 0.009(2) 0.019(2) 0.041(3) C14 0.061(3) 0.052(3) 0.073(3) 0.010(2) 0.005(2) 0.025(2) N1' 0.073(3) 0.052(2) 0.057(2) 0.0108(18) -0.0029(19) 0.029(2) C2' 0.064(3) 0.053(3) 0.059(3) 0.012(2) 0.002(2) 0.026(2) C3' 0.087(4) 0.073(3) 0.086(4) 0.032(3) 0.023(3) 0.049(3) C4' 0.100(4) 0.087(4) 0.107(4) 0.044(3) 0.031(4) 0.057(4) C5' 0.109(5) 0.096(4) 0.103(4) 0.042(4) 0.036(4) 0.068(4) C6' 0.082(4) 0.059(3) 0.072(3) 0.014(2) 0.014(3) 0.033(3) C7' 0.115(5) 0.073(4) 0.077(3) 0.027(3) 0.026(3) 0.048(4) C8' 0.188(7) 0.093(5) 0.074(4) 0.027(4) 0.033(5) 0.078(5) C9' 0.134(5) 0.080(4) 0.068(3) 0.022(3) 0.034(3) 0.065(4) C10' 0.103(5) 0.086(4) 0.089(4) 0.033(3) 0.048(3) 0.053(4) C11' 0.105(4) 0.093(4) 0.078(3) 0.029(3) 0.035(3) 0.067(4) N12' 0.089(3) 0.076(3) 0.065(2) 0.018(2) 0.025(2) 0.054(3) C13' 0.142(6) 0.181(8) 0.137(6) 0.092(6) 0.064(5) 0.127(6) C14' 0.195(9) 0.184(9) 0.157(7) 0.109(7) 0.080(7) 0.149(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 Cu1 N1 2.060(4) . Y Cu1 N1' 2.113(4) . Y Cu1 N12 1.996(3) 2_655 Y Cu1 N12' 2.041(4) 17 Y N1 C6 1.342(6) . ? N1 C2 1.356(5) . ? C2 C3 1.393(6) . ? C2 C2' 1.486(6) . ? C3 C4 1.405(7) . ? C4 C5 1.359(6) . ? C5 C6 1.401(7) . ? C6 C7 1.476(6) . ? C7 C8 1.166(6) . ? C8 C9 1.439(6) . ? C9 C14 1.405(6) . ? C9 C10 1.411(6) . ? C10 C11 1.365(6) . ? C11 N12 1.334(5) . ? N12 C13 1.339(6) . ? C13 C14 1.371(6) . ? N1' C6' 1.333(6) . ? N1' C2' 1.371(5) . ? C2' C3' 1.415(6) . ? C3' C4' 1.354(7) . ? C4' C5' 1.395(7) . ? C5' C6' 1.382(7) . ? C6' C7' 1.469(7) . ? C7' C8' 1.148(7) . ? C8' C9' 1.468(8) . ? C9' C10' 1.351(8) . ? C9' C14' 1.367(9) . ? C10' C11' 1.388(7) . ? C11' N12' 1.320(6) . ? N12' C13' 1.304(7) . ? C13' C14' 1.375(9) . ? B1 F1 1.329(11) . ? B1 F2 1.411(12) . ? B10 F12 1.390(3) 3_665 ? B10 F12 1.390(3) 2_655 ? B10 F12 1.390(3) . ? B10 F11 1.426(9) . ? B20 F21 1.345(12) . ? B20 F23 1.387(13) . ? B20 F22 1.407(13) . ? B20 F24 1.410(13) . ? 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 N12 Cu1 N12' 118.19(15) 2_655 17 Y N12 Cu1 N1 125.82(14) 2_655 . Y N12' Cu1 N1 104.18(15) 17 . Y N12 Cu1 N1' 109.58(15) 2_655 . Y N12' Cu1 N1' 113.23(16) 17 . Y N1 Cu1 N1' 79.80(15) . . Y C6 N1 C2 117.2(4) . . ? C6 N1 Cu1 127.1(3) . . Y C2 N1 Cu1 115.1(3) . . Y N1 C2 C3 122.1(4) . . ? N1 C2 C2' 115.5(4) . . ? C3 C2 C2' 122.4(4) . . ? C2 C3 C4 119.1(4) . . ? C5 C4 C3 119.1(5) . . ? C4 C5 C6 118.4(5) . . ? N1 C6 C5 124.0(4) . . ? N1 C6 C7 116.0(4) . . ? C5 C6 C7 120.0(4) . . ? C8 C7 C6 173.1(6) . . ? C7 C8 C9 175.2(6) . . ? C14 C9 C10 117.8(4) . . ? C14 C9 C8 120.6(4) . . ? C10 C9 C8 121.6(4) . . ? C11 C10 C9 118.5(4) . . ? N12 C11 C10 124.4(4) . . ? C11 N12 C13 116.6(4) . . ? C11 N12 Cu1 123.8(3) . 3_665 Y C13 N12 Cu1 119.6(3) . 3_665 Y N12 C13 C14 124.6(4) . . ? C13 C14 C9 118.0(4) . . ? C6' N1' C2' 117.7(4) . . ? C6' N1' Cu1 128.8(3) . . Y C2' N1' Cu1 112.8(3) . . Y N1' C2' C3' 121.3(4) . . ? N1' C2' C2 115.7(4) . . ? C3' C2' C2 123.0(4) . . ? C4' C3' C2' 119.5(5) . . ? C3' C4' C5' 119.1(5) . . ? C6' C5' C4' 119.1(5) . . ? N1' C6' C5' 123.3(5) . . ? N1' C6' C7' 114.9(5) . . ? C5' C6' C7' 121.7(5) . . ? C8' C7' C6' 163.9(7) . . ? C7' C8' C9' 171.6(9) . . ? C10' C9' C14' 116.0(5) . . ? C10' C9' C8' 118.2(6) . . ? C14' C9' C8' 125.8(6) . . ? C9' C10' C11' 120.7(5) . . ? N12' C11' C10' 122.6(5) . . ? C13' N12' C11' 116.6(5) . . ? C13' N12' Cu1 119.5(4) . 18_545 y C11' N12' Cu1 122.8(3) . 18_545 y N12' C13' C14' 123.7(7) . . ? C9' C14' C13' 120.2(6) . . ? F1 B1 F2 106.6(8) . 2_655 ? F12 B10 F11 107.7(3) . . ? F21 B20 F22 112.5(11) . . ? F21 B20 F23 113.5(11) . . ? F21 B20 F24 110.2(11) . . ? F22 B20 F23 107.0(11) . . ? F22 B20 F24 105.8(10) . . ? F23 B20 F24 107.4(11) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.01 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.11 #===END data_Compound_2_(AG4PYY) _database_code_CSD 201516 _refine_special_details ; Distance and similarity restraints were applied to B-F bonds. After failing to model regions of diffuse electron density, we resorted to the PLATON SQUEEZE procedure. This removed the contribution of the diffuse regions to the diffraction pattern and gave a new HKL file. The number of electrons thus estimated were included in the final formula, formula weight, calculated density, mu and F(000) is 2690 per unit cell. The residual electron density was assigned to three molecules of the DMF solvent and half a counteranion [2690/18 = 150 e per ligand molecule. 150 - 41*0.5(BF4) = 130 e. Three molecules of DMF would give 120 e.] ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl silver tetrafluoroborate hexamer ; _chemical_name_common ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl silver tetrafluoroborate hexamer ; _chemical_formula_sum 'C33 H35 Ag B F4 N7 O3' _chemical_formula_weight 772.36 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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 Rhombohedral _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 20.803(3) _cell_length_b 20.803(3) _cell_length_c 40.125(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 15038(5) _cell_formula_units_Z 18 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1488 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 19.2 _exptl_crystal_description sphenoid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method ? _exptl_crystal_F_000 7092 _exptl_absorpt_coefficient_mu 0.671 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min . _exptl_absorpt_correction_T_max . _exptl_absorpt_process_details . _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_standards_number . _diffrn_standards_decay_% none _diffrn_reflns_number 14447 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_av_sigmaI/netI 0.216 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 54 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 19.2 _reflns_number_total 7605 _reflns_number_gt 2430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OLEX (Dolomanov, 2001)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0416P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_number_reflns 7605 _refine_ls_number_parameters 284 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.122 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.103 _refine_ls_wR_factor_gt 0.092 _refine_ls_goodness_of_fit_ref 0.610 _refine_ls_restrained_S_all 0.648 _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 0.21069(2) 0.29381(2) -0.081432(10) 0.06340(16) Uani 1 1 d . . . N1 N 0.3255(3) 0.3990(2) -0.09759(10) 0.0600(12) Uani 1 1 d . . . C2 C 0.3226(3) 0.4407(3) -0.12238(13) 0.0590(14) Uani 1 1 d . . . C3 C 0.3880(3) 0.4944(3) -0.13836(13) 0.0723(16) Uani 1 1 d . . . H3A H 0.3858 0.5239 -0.1559 0.087 Uiso 1 1 calc R . . C4 C 0.4551(3) 0.5032(3) -0.12800(15) 0.096(2) Uani 1 1 d . . . H4A H 0.4998 0.5392 -0.1383 0.115 Uiso 1 1 calc R . . C5 C 0.4570(3) 0.4591(3) -0.10240(14) 0.090(2) Uani 1 1 d . . . H5A H 0.5027 0.4635 -0.0955 0.108 Uiso 1 1 calc R . . C6 C 0.3921(4) 0.4096(3) -0.08745(14) 0.0761(18) Uani 1 1 d . . . C7 C 0.3875(3) 0.3606(3) -0.06111(14) 0.0790(19) Uani 1 1 d . . . C8 C 0.3765(3) 0.3168(3) -0.04012(14) 0.0826(19) Uani 1 1 d . . . C9 C 0.3559(4) 0.2600(3) -0.01491(14) 0.086(2) Uani 1 1 d . . . C10 C 0.2834(3) 0.2180(3) -0.00442(12) 0.0715(16) Uani 1 1 d . . . H10A H 0.2460 0.2265 -0.0133 0.086 Uiso 1 1 calc R . . C11 C 0.2659(3) 0.1640(3) 0.01891(12) 0.0723(17) Uani 1 1 d . . . H11A H 0.2152 0.1340 0.0249 0.087 Uiso 1 1 calc R . . N12 N 0.3146(3) 0.1506(3) 0.03363(11) 0.0858(16) Uani 1 1 d . . . C13 C 0.3846(4) 0.1893(5) 0.02377(19) 0.153(4) Uani 1 1 d . . . H13A H 0.4206 0.1792 0.0331 0.183 Uiso 1 1 calc R . . C14 C 0.4060(4) 0.2457(4) -0.00075(19) 0.165(4) Uani 1 1 d . . . H14A H 0.4566 0.2739 -0.0072 0.198 Uiso 1 1 calc R . . N1' N 0.1904(2) 0.3653(2) -0.12086(9) 0.0511(11) Uani 1 1 d . . . C2' C 0.2493(3) 0.4277(3) -0.13225(11) 0.0492(13) Uani 1 1 d . . . C3' C 0.2392(3) 0.4770(3) -0.15245(11) 0.0538(13) Uani 1 1 d . . . H3'A H 0.2810 0.5216 -0.1600 0.065 Uiso 1 1 calc R . . C4' C 0.1675(3) 0.4603(3) -0.16149(12) 0.0596(15) Uani 1 1 d . . . H4'A H 0.1604 0.4934 -0.1753 0.071 Uiso 1 1 calc R . . C5' C 0.1079(3) 0.3962(3) -0.15037(13) 0.0603(14) Uani 1 1 d . . . H5'A H 0.0588 0.3830 -0.1566 0.072 Uiso 1 1 calc R . . C6' C 0.1216(3) 0.3501(3) -0.12931(12) 0.0538(14) Uani 1 1 d . . . C7' C 0.0594(3) 0.2811(3) -0.11673(13) 0.0586(15) Uani 1 1 d . . . C8' C 0.0073(3) 0.2261(3) -0.10800(13) 0.0605(15) Uani 1 1 d . . . C9' C -0.0594(3) 0.1585(3) -0.09944(12) 0.0534(14) Uani 1 1 d . . . C10' C -0.0568(3) 0.1040(3) -0.08038(12) 0.0534(13) Uani 1 1 d . . . H10B H -0.0112 0.1112 -0.0716 0.064 Uiso 1 1 calc R . . C11' C -0.1237(3) 0.0380(3) -0.07448(12) 0.0521(13) Uani 1 1 d . . . H11B H -0.1222 0.0009 -0.0612 0.063 Uiso 1 1 calc R . . N12' N -0.1885(2) 0.0244(2) -0.08617(9) 0.0512(10) Uani 1 1 d . . . C13' C -0.1898(3) 0.0782(3) -0.10379(12) 0.0601(14) Uani 1 1 d . . . H13B H -0.2363 0.0695 -0.1120 0.072 Uiso 1 1 calc R . . C14' C -0.1270(3) 0.1466(3) -0.11090(12) 0.0608(14) Uani 1 1 d . . . H14B H -0.1308 0.1836 -0.1232 0.073 Uiso 1 1 calc R . . B10 B 0.0000 0.0000 -0.1400(2) 0.065(3) Uani 1 3 d SD . . F11 F -0.03481(13) -0.07332(12) -0.14982(6) 0.0556(7) Uani 1 1 d D . . F12 F 0.0000 0.0000 -0.10466(13) 0.0819(16) Uani 1 3 d SD . . B1 B 0.0000 0.0000 0.0000 0.148(9) Uiso 1 6 d SD . . F1 F 0.0000 0.0000 -0.03513(18) 0.133(5) Uiso 0.50 3 d SPD A 1 F2 F 0.0266(6) 0.0745(3) -0.0120(2) 0.163(4) Uiso 0.50 1 d PD . 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 0.0833(3) 0.0438(3) 0.0647(3) 0.0181(2) 0.0348(2) 0.0329(3) N1 0.075(3) 0.044(3) 0.051(3) 0.015(2) 0.011(2) 0.022(3) C2 0.062(4) 0.051(4) 0.059(4) 0.014(3) 0.017(3) 0.025(3) C3 0.066(4) 0.067(4) 0.075(4) 0.031(3) 0.011(3) 0.027(3) C4 0.064(5) 0.091(5) 0.111(5) 0.046(4) 0.010(4) 0.022(4) C5 0.069(4) 0.082(5) 0.098(5) 0.054(4) 0.003(4) 0.021(4) C6 0.065(4) 0.060(4) 0.074(4) 0.029(3) 0.002(3) 0.009(3) C7 0.071(4) 0.068(4) 0.065(4) 0.028(3) -0.004(3) 0.010(3) C8 0.078(5) 0.087(5) 0.068(4) 0.013(4) -0.004(3) 0.029(4) C9 0.080(5) 0.082(5) 0.070(4) 0.041(4) -0.016(4) 0.021(4) C10 0.074(4) 0.091(5) 0.057(4) 0.023(3) 0.000(3) 0.047(4) C11 0.065(4) 0.097(5) 0.057(4) 0.024(3) -0.006(3) 0.043(4) N12 0.060(3) 0.094(4) 0.081(3) 0.042(3) -0.002(3) 0.022(3) C13 0.087(6) 0.197(9) 0.161(8) 0.117(7) 0.006(5) 0.061(6) C14 0.083(6) 0.190(8) 0.160(8) 0.128(7) 0.001(5) 0.022(6) N1' 0.052(3) 0.031(2) 0.064(3) 0.007(2) 0.022(2) 0.016(2) C2' 0.061(4) 0.033(3) 0.045(3) 0.004(2) 0.015(3) 0.017(3) C3' 0.067(4) 0.030(3) 0.057(3) 0.012(2) 0.015(3) 0.019(3) C4' 0.062(4) 0.040(3) 0.077(4) 0.009(3) 0.005(3) 0.025(3) C5' 0.059(4) 0.045(3) 0.078(4) 0.000(3) 0.012(3) 0.026(3) C6' 0.059(4) 0.036(3) 0.062(3) 0.001(3) 0.026(3) 0.021(3) C7' 0.063(4) 0.032(3) 0.078(4) 0.004(3) 0.023(3) 0.022(3) C8' 0.068(4) 0.041(3) 0.073(4) -0.002(3) 0.023(3) 0.027(3) C9' 0.049(4) 0.041(3) 0.067(4) 0.006(3) 0.021(3) 0.021(3) C10' 0.038(3) 0.048(3) 0.073(3) -0.003(3) 0.007(3) 0.020(3) C11' 0.044(3) 0.049(3) 0.059(3) 0.002(3) -0.002(3) 0.020(3) N12' 0.043(3) 0.050(3) 0.055(3) 0.006(2) -0.003(2) 0.019(2) C13' 0.050(4) 0.064(4) 0.065(4) 0.006(3) -0.007(3) 0.028(3) C14' 0.060(4) 0.047(4) 0.072(4) 0.013(3) 0.013(3) 0.024(3) B10 0.060(5) 0.060(5) 0.075(9) 0.000 0.000 0.030(3) F11 0.0435(16) 0.0333(15) 0.088(2) -0.0057(14) -0.0058(14) 0.0173(13) F12 0.082(3) 0.082(3) 0.081(4) 0.000 0.000 0.0412(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 N12' 2.222(4) 3 y Ag1 N12 2.287(4) 12 y Ag1 N1' 2.349(4) . y Ag1 N1 2.385(4) . y N1 C2 1.340(6) . ? N1 C6 1.353(6) . ? C2 C3 1.411(6) . ? C2 C2' 1.466(6) . ? C3 C4 1.377(7) . ? C4 C5 1.390(7) . ? C5 C6 1.361(7) . ? C6 C7 1.438(7) . ? C7 C8 1.177(7) . y C8 C9 1.448(7) . ? C9 C14 1.343(8) . ? C9 C10 1.378(7) . ? C10 C11 1.364(6) . ? C11 N12 1.316(6) . ? N12 C13 1.323(7) . ? N12 Ag1 2.287(4) 11 ? C13 C14 1.423(8) . ? N1' C2' 1.343(5) . ? N1' C6' 1.347(6) . ? C2' C3' 1.402(6) . ? C3' C4' 1.399(6) . ? C4' C5' 1.365(6) . ? C5' C6' 1.409(6) . ? C6' C7' 1.461(7) . ? C7' C8' 1.168(6) . y C8' C9' 1.438(7) . ? C9' C14' 1.380(6) . ? C9' C10' 1.391(6) . ? C10' C11' 1.403(6) . ? C11' N12' 1.317(5) . ? N12' C13' 1.336(5) . ? N12' Ag1 2.222(4) 2 y C13' C14' 1.397(6) . ? B10 F11 1.379(3) . ? B10 F12 1.416(7) . ? B1 F1 1.410(7) . ? B1 F2 1.442(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12' Ag1 N12 118.58(16) 3 12 y N12' Ag1 N1' 131.68(13) 3 . y N12 Ag1 N1' 102.56(15) 12 . y N12' Ag1 N1 112.15(15) 3 . y N12 Ag1 N1 112.29(16) 12 . y N1' Ag1 N1 69.52(15) . . y C2 N1 C6 119.4(5) . . ? C2 N1 Ag1 116.6(4) . . y C6 N1 Ag1 122.8(3) . . y N1 C2 C3 120.8(5) . . ? N1 C2 C2' 117.4(5) . . ? C3 C2 C2' 121.7(5) . . ? C4 C3 C2 118.7(5) . . ? C3 C4 C5 119.7(6) . . ? C6 C5 C4 118.7(6) . . ? N1 C6 C5 122.5(5) . . ? N1 C6 C7 113.9(5) . . ? C5 C6 C7 123.4(6) . . ? C8 C7 C6 173.6(7) . . y C7 C8 C9 174.9(7) . . y C14 C9 C10 117.0(5) . . ? C14 C9 C8 122.0(6) . . ? C10 C9 C8 120.9(6) . . ? C11 C10 C9 119.3(5) . . ? N12 C11 C10 124.4(5) . . ? C11 N12 C13 117.8(5) . . ? C11 N12 Ag1 125.2(4) . 11 ? C13 N12 Ag1 115.9(4) . 11 ? N12 C13 C14 120.3(6) . . ? C9 C14 C13 121.1(7) . . ? C2' N1' C6' 119.2(4) . . ? C2' N1' Ag1 118.5(3) . . y C6' N1' Ag1 121.8(3) . . y N1' C2' C3' 120.5(5) . . ? N1' C2' C2 116.5(4) . . ? C3' C2' C2 123.0(5) . . ? C4' C3' C2' 119.9(5) . . ? C5' C4' C3' 119.5(5) . . ? C4' C5' C6' 117.9(5) . . ? N1' C6' C5' 123.0(5) . . ? N1' C6' C7' 117.3(5) . . ? C5' C6' C7' 119.7(5) . . ? C8' C7' C6' 176.4(6) . . y C7' C8' C9' 175.9(6) . . y C14' C9' C10' 119.2(5) . . ? C14' C9' C8' 119.6(5) . . ? C10' C9' C8' 121.2(5) . . ? C9' C10' C11' 117.8(5) . . ? N12' C11' C10' 124.0(5) . . ? C11' N12' C13' 117.1(4) . . ? C11' N12' Ag1 125.0(3) . 2 ? C13' N12' Ag1 117.8(3) . 2 ? N12' C13' C14' 124.2(5) . . ? C9' C14' C13' 117.7(5) . . ? F11 B10 F11 112.1(3) 2 . ? F11 B10 F12 106.7(3) . . ? F1 B1 F2 109.5(3) . 10 ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.54 _refine_diff_density_min -0.40 _refine_diff_density_rms 0.06 #===END data_Compound_3(AGSBL6) _database_code_CSD 201517 _refine_special_details ; 1. Similarity restraints were applied to Sb-F distances in the SbF6- anion. 2. All non-H atoms were refined anisotropically. 3. Acetonitrile hydrogens could not be located from the Fourier synthesis and# are not included in the refinement model. HOWEVER, THEY ARE INCLUDED IN THE CALCULATION OF THE FORMULA WEIGHT, ETC. 4. As expected, the largest electron density extrema lie near the Sb atoms. 5. Rigid-bond restraints were applied to anisotropic displacement parameters. 6. The original dataset was truncated to 2theta of 50 degrees as higher-angle reflections had no significant intensity. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl silver hexafluoroantimonate ; _chemical_name_common ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl silver hexafluoroantimonate ; _chemical_formula_sum 'C168 H120 Ag6 F36 N36 Sb6' _chemical_formula_weight 4704.72 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' F F 0.0171 0.0103 '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' Sb Sb -0.5866 1.5461 '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 15.971(5) _cell_length_b 18.961(6) _cell_length_c 19.029(6) _cell_angle_alpha 113.311(4) _cell_angle_beta 96.282(5) _cell_angle_gamma 113.352(4) _cell_volume 4610(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3736 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 23.85 _exptl_crystal_description column _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.695 _exptl_crystal_density_method ? _exptl_crystal_F_000 2292 _exptl_absorpt_coefficient_mu 1.580 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.646 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_standards_number . _diffrn_standards_decay_% none _diffrn_reflns_number 41278 _diffrn_reflns_av_R_equivalents 0.109 _diffrn_reflns_av_sigmaI/netI 0.169 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16122 _reflns_number_gt 7531 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OLEX (Oleg V. Dolomanov, 2002)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0873P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00120(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 16122 _refine_ls_number_parameters 1141 _refine_ls_number_restraints 321 _refine_ls_R_factor_all 0.1856 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2485 _refine_ls_wR_factor_gt 0.1806 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.002 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 Sb15 Sb 0.0000 0.0000 0.0000 0.0396(4) Uani 1 2 d SU . . F16 F 0.0751(9) -0.0221(11) 0.0596(10) 0.140(6) Uani 1 1 d U . . F17 F 0.0546(12) 0.1136(8) 0.0794(8) 0.146(6) Uani 1 1 d U . . F18 F -0.0997(8) -0.0355(8) 0.0434(8) 0.103(4) Uani 1 1 d U . . Sb19 Sb 0.57030(8) 0.37091(7) 0.04528(7) 0.0498(3) Uani 1 1 d U . . F20 F 0.5823(6) 0.4509(7) 0.1470(6) 0.076(3) Uani 1 1 d U . . F21 F 0.6829(7) 0.4568(7) 0.0452(7) 0.084(3) Uani 1 1 d U . . F22 F 0.6418(8) 0.3350(8) 0.0911(7) 0.095(3) Uani 1 1 d U . . F23 F 0.5560(9) 0.2914(8) -0.0571(7) 0.108(4) Uani 1 1 d U . . F24 F 0.4569(7) 0.2868(6) 0.0451(6) 0.073(3) Uani 1 1 d U . . F25 F 0.4980(8) 0.4077(8) 0.0003(7) 0.090(3) Uani 1 1 d U . . Ag1 Ag -0.03225(7) -0.30228(7) 0.08868(7) 0.0378(3) Uani 1 1 d U . . Ag2 Ag 0.34015(7) 0.26388(8) 0.32990(7) 0.0419(3) Uani 1 1 d U . . Ag3 Ag 0.28847(8) -0.05641(7) -0.20501(7) 0.0388(3) Uani 1 1 d U . . N1 N -0.0779(7) -0.3706(7) 0.1702(6) 0.029(2) Uani 1 1 d U . . N1' N 0.0462(7) -0.3858(7) 0.0890(6) 0.030(2) Uani 1 1 d U . . N1A N 0.4464(7) 0.2985(7) 0.4525(6) 0.031(2) Uani 1 1 d U . . N1B N 0.4829(7) 0.4045(7) 0.3821(6) 0.032(2) Uani 1 1 d U . . N1C N 0.3118(8) -0.1421(8) -0.3245(7) 0.038(3) Uani 1 1 d U . . N1D N 0.4536(7) -0.0245(7) -0.1830(7) 0.035(3) Uani 1 1 d U . . N12 N -0.2465(8) -0.0467(8) 0.1922(7) 0.042(3) Uani 1 1 d U . . N12' N 0.2158(8) -0.1482(8) -0.1531(7) 0.037(3) Uani 1 1 d U . . N12A N 0.0775(9) -0.1594(8) 0.1908(8) 0.051(3) Uani 1 1 d U . . N12B N 0.1456(8) 0.3241(8) 0.0091(7) 0.039(3) Uani 1 1 d U . . N12C N -0.1919(7) -0.2306(7) -0.3412(7) 0.037(3) Uani 1 1 d U . . N12D N 0.3761(8) 0.1974(8) 0.2184(7) 0.045(3) Uani 1 1 d U . . C2 C -0.0526(9) -0.4296(9) 0.1674(9) 0.035(3) Uani 1 1 d U . . C2' C 0.0277(9) -0.4294(9) 0.1311(8) 0.033(3) Uani 1 1 d U . . C2A C 0.5225(9) 0.3834(9) 0.4961(8) 0.031(3) Uani 1 1 d U . . C2B C 0.5492(9) 0.4300(8) 0.4493(8) 0.029(3) Uani 1 1 d U . . C2C C 0.4005(9) -0.1319(9) -0.3244(8) 0.031(3) Uani 1 1 d U . . C2D C 0.4803(10) -0.0597(9) -0.2473(8) 0.038(3) Uani 1 1 d U . . C3 C -0.0941(10) -0.4861(9) 0.2001(9) 0.040(3) Uani 1 1 d U . . H3A H -0.0745 -0.5279 0.1982 0.048 Uiso 1 1 calc R . . C3' C 0.0804(10) -0.4704(9) 0.1418(9) 0.037(3) Uani 1 1 d U . . H3'A H 0.0661 -0.5009 0.1720 0.045 Uiso 1 1 calc R . . C3A C 0.5722(9) 0.4168(9) 0.5770(8) 0.037(3) Uani 1 1 d U . . H3AA H 0.6246 0.4748 0.6062 0.045 Uiso 1 1 calc R . . C3B C 0.6438(9) 0.4989(9) 0.4723(9) 0.038(3) Uani 1 1 d U . . H3BA H 0.6906 0.5190 0.5208 0.046 Uiso 1 1 calc R . . C3C C 0.4175(10) -0.1834(9) -0.3904(9) 0.047(4) Uani 1 1 d U . . H3CA H 0.4812 -0.1722 -0.3894 0.057 Uiso 1 1 calc R . . C3D C 0.5772(10) -0.0283(11) -0.2444(10) 0.058(5) Uani 1 1 d U . . H3DA H 0.5946 -0.0515 -0.2911 0.070 Uiso 1 1 calc R . . C4 C -0.1619(12) -0.4785(11) 0.2336(10) 0.054(4) Uani 1 1 d U . . H4A H -0.1912 -0.5168 0.2544 0.065 Uiso 1 1 calc R . . C4' C 0.1527(10) -0.4664(9) 0.1083(9) 0.041(3) Uani 1 1 d U . . H4'A H 0.1895 -0.4935 0.1155 0.049 Uiso 1 1 calc R . . C4A C 0.5456(10) 0.3661(9) 0.6148(9) 0.039(3) Uani 1 1 d U . . H4AA H 0.5788 0.3900 0.6701 0.047 Uiso 1 1 calc R . . C4B C 0.6671(10) 0.5369(10) 0.4227(9) 0.048(4) Uani 1 1 d U . . H4BA H 0.7307 0.5820 0.4372 0.058 Uiso 1 1 calc R . . C4C C 0.3387(11) -0.2529(10) -0.4591(10) 0.056(4) Uani 1 1 d U . . H4CA H 0.3478 -0.2923 -0.5033 0.067 Uiso 1 1 calc R . . C4D C 0.6460(12) 0.0372(13) -0.1713(11) 0.087(7) Uani 1 1 d U . . H4DA H 0.7123 0.0594 -0.1668 0.105 Uiso 1 1 calc R . . C5 C -0.1905(10) -0.4177(10) 0.2390(9) 0.044(4) Uani 1 1 d U . . H5A H -0.2369 -0.4117 0.2647 0.053 Uiso 1 1 calc R . . C5' C 0.1712(10) -0.4227(9) 0.0644(9) 0.040(3) Uani 1 1 d U . . H5'A H 0.2204 -0.4203 0.0400 0.048 Uiso 1 1 calc R . . C5A C 0.4708(10) 0.2807(10) 0.5725(9) 0.040(3) Uani 1 1 d U . . H5AA H 0.4531 0.2443 0.5971 0.048 Uiso 1 1 calc R . . C5B C 0.5985(9) 0.5095(9) 0.3523(9) 0.043(4) Uani 1 1 d U . . H5BA H 0.6133 0.5346 0.3179 0.051 Uiso 1 1 calc R . . C5C C 0.2469(11) -0.2627(11) -0.4608(9) 0.056(4) Uani 1 1 d U . . H5CA H 0.1931 -0.3065 -0.5077 0.067 Uiso 1 1 calc R . . C5D C 0.6186(12) 0.0707(13) -0.1047(11) 0.085(7) Uani 1 1 d U . . H5DA H 0.6663 0.1149 -0.0542 0.102 Uiso 1 1 calc R . . C6 C -0.1481(10) -0.3653(9) 0.2051(8) 0.036(3) Uani 1 1 d U . . C6' C 0.1183(9) -0.3817(9) 0.0552(8) 0.034(3) Uani 1 1 d U . . C6A C 0.4219(10) 0.2498(10) 0.4913(9) 0.040(3) Uani 1 1 d U . . C6B C 0.5044(9) 0.4415(9) 0.3349(8) 0.034(3) Uani 1 1 d U . . C6C C 0.2354(10) -0.2068(10) -0.3923(9) 0.040(3) Uani 1 1 d U . . C6D C 0.5229(11) 0.0405(11) -0.1108(9) 0.054(4) Uani 1 1 d U . . C7 C -0.1712(10) -0.2977(10) 0.2062(9) 0.042(4) Uani 1 1 d U . . C7' C 0.1347(9) -0.3346(9) 0.0118(8) 0.034(3) Uani 1 1 d U . . C7A C 0.3442(10) 0.1621(10) 0.4391(9) 0.042(4) Uani 1 1 d U . . C7B C 0.4297(10) 0.4125(9) 0.2643(9) 0.040(4) Uani 1 1 d U . . C7C C 0.1430(10) -0.2163(10) -0.3883(9) 0.044(4) Uani 1 1 d U . . C7D C 0.4892(11) 0.0738(10) -0.0438(9) 0.049(4) Uani 1 1 d U . . C8 C -0.1891(9) -0.2452(10) 0.1996(9) 0.040(4) Uani 1 1 d U . . C8' C 0.1463(9) -0.2945(9) -0.0254(9) 0.036(3) Uani 1 1 d U . . C8A C 0.2820(11) 0.0905(10) 0.3869(9) 0.046(4) Uani 1 1 d U . . C8B C 0.3702(10) 0.3915(11) 0.2058(9) 0.045(4) Uani 1 1 d U . . C8C C 0.0695(11) -0.2165(10) -0.3788(9) 0.048(4) Uani 1 1 d U . . C8D C 0.4629(11) 0.0998(10) 0.0121(9) 0.043(4) Uani 1 1 d U . . C9 C -0.2072(10) -0.1786(9) 0.1944(8) 0.038(3) Uani 1 1 d U . . C9' C 0.1671(9) -0.2460(8) -0.0707(8) 0.031(3) Uani 1 1 d U . . C9A C 0.2118(10) 0.0059(10) 0.3218(9) 0.044(3) Uani 1 1 d U . . C9B C 0.2932(10) 0.3661(9) 0.1379(8) 0.037(3) Uani 1 1 d U . . C9C C -0.0188(10) -0.2216(9) -0.3657(10) 0.043(3) Uani 1 1 d U . . C9D C 0.4359(11) 0.1345(10) 0.0832(9) 0.041(3) Uani 1 1 d U . . C10 C -0.2848(11) -0.1993(10) 0.1350(10) 0.049(4) Uani 1 1 d U . . H10A H -0.3261 -0.2581 0.0941 0.059 Uiso 1 1 calc R . . C10' C 0.2137(10) -0.2642(9) -0.1289(9) 0.038(3) Uani 1 1 d U . . H10B H 0.2300 -0.3099 -0.1415 0.046 Uiso 1 1 calc R . . C10A C 0.1491(11) -0.0024(10) 0.2578(9) 0.047(4) Uani 1 1 d U . . H10C H 0.1509 0.0482 0.2576 0.056 Uiso 1 1 calc R . . C10B C 0.3138(10) 0.3923(10) 0.0803(9) 0.044(4) Uani 1 1 d U . . H10D H 0.3786 0.4249 0.0838 0.053 Uiso 1 1 calc R . . C10C C -0.0299(9) -0.1985(10) -0.2896(9) 0.047(4) Uani 1 1 d U . . H10E H 0.0216 -0.1791 -0.2446 0.056 Uiso 1 1 calc R . . C10D C 0.4993(10) 0.1923(10) 0.1573(9) 0.046(4) Uani 1 1 d U . . H10F H 0.5660 0.2130 0.1644 0.055 Uiso 1 1 calc R . . C11 C -0.3003(11) -0.1312(10) 0.1372(9) 0.050(4) Uani 1 1 d U . . H11A H -0.3535 -0.1460 0.0961 0.060 Uiso 1 1 calc R . . C11' C 0.2351(10) -0.2133(10) -0.1674(9) 0.042(3) Uani 1 1 d U . . H11B H 0.2659 -0.2264 -0.2070 0.050 Uiso 1 1 calc R . . C11A C 0.0854(11) -0.0841(10) 0.1956(9) 0.048(4) Uani 1 1 d U . . H11C H 0.0438 -0.0879 0.1529 0.057 Uiso 1 1 calc R . . C11B C 0.2380(10) 0.3703(10) 0.0170(9) 0.040(3) Uani 1 1 d U . . H11D H 0.2530 0.3890 -0.0218 0.048 Uiso 1 1 calc R . . C11C C -0.1168(10) -0.2040(10) -0.2800(9) 0.048(4) Uani 1 1 d U . . H11E H -0.1233 -0.1882 -0.2277 0.058 Uiso 1 1 calc R . . C11D C 0.4700(10) 0.2223(10) 0.2234(9) 0.047(4) Uani 1 1 d U . . H11F H 0.5176 0.2622 0.2748 0.057 Uiso 1 1 calc R . . C13 C -0.1691(10) -0.0257(10) 0.2487(10) 0.050(4) Uani 1 1 d U . . H13A H -0.1281 0.0340 0.2876 0.060 Uiso 1 1 calc R . . C13' C 0.1700(9) -0.1306(9) -0.0979(8) 0.035(3) Uani 1 1 d U . . H13B H 0.1556 -0.0840 -0.0863 0.042 Uiso 1 1 calc R . . C13A C 0.1316(13) -0.1522(11) 0.2526(11) 0.078(6) Uani 1 1 d U . . H13C H 0.1244 -0.2046 0.2521 0.094 Uiso 1 1 calc R . . C13B C 0.1258(11) 0.3004(12) 0.0642(10) 0.061(5) Uani 1 1 d U . . H13D H 0.0605 0.2706 0.0611 0.073 Uiso 1 1 calc R . . C13C C -0.1801(10) -0.2492(10) -0.4135(9) 0.045(4) Uani 1 1 d U . . H13E H -0.2318 -0.2650 -0.4565 0.054 Uiso 1 1 calc R . . C13D C 0.3101(11) 0.1413(11) 0.1446(9) 0.060(5) Uani 1 1 d U . . H13F H 0.2443 0.1240 0.1397 0.071 Uiso 1 1 calc R . . C14 C -0.1472(11) -0.0898(10) 0.2514(10) 0.058(5) Uani 1 1 d U . . H14A H -0.0921 -0.0731 0.2917 0.069 Uiso 1 1 calc R . . C14' C 0.1436(9) -0.1797(8) -0.0575(9) 0.034(3) Uani 1 1 d U . . H14B H 0.1092 -0.1676 -0.0206 0.041 Uiso 1 1 calc R . . C14A C 0.2004(13) -0.0713(11) 0.3204(11) 0.073(6) Uani 1 1 d U . . H14C H 0.2378 -0.0699 0.3639 0.087 Uiso 1 1 calc R . . C14B C 0.1979(11) 0.3180(12) 0.1271(10) 0.065(5) Uani 1 1 d U . . H14D H 0.1805 0.2960 0.1633 0.078 Uiso 1 1 calc R . . C14C C -0.0964(10) -0.2468(10) -0.4292(9) 0.046(4) Uani 1 1 d U . . H14E H -0.0917 -0.2618 -0.4820 0.055 Uiso 1 1 calc R . . C14D C 0.3348(11) 0.1073(11) 0.0745(10) 0.061(5) Uani 1 1 d U . . H14F H 0.2869 0.0678 0.0232 0.073 Uiso 1 1 calc R . . Sb33 Sb 0.5000 0.0000 0.5000 0.0583(5) Uani 1 2 d SU . . F34 F 0.3812(13) -0.0671(12) 0.4258(13) 0.246(11) Uani 1 1 d U . . F35 F 0.5142(10) -0.1002(8) 0.4650(8) 0.112(4) Uani 1 1 d U . . F36 F 0.548(2) 0.0203(13) 0.4255(12) 0.232(10) Uani 1 1 d U . . Sb26 Sb 0.12259(8) 0.44881(9) 0.32320(8) 0.0691(4) Uani 1 1 d U . . F27 F 0.1954(9) 0.5005(11) 0.2710(9) 0.130(5) Uani 1 1 d U . . F28 F 0.1993(7) 0.3990(6) 0.3306(6) 0.069(3) Uani 1 1 d U . . F29 F 0.0425(8) 0.3519(11) 0.2249(7) 0.154(5) Uani 1 1 d U . . F30 F 0.0498(8) 0.3982(6) 0.3772(6) 0.077(3) Uani 1 1 d U . . F31 F 0.0485(9) 0.5029(12) 0.3200(11) 0.151(5) Uani 1 1 d U . . F32 F 0.2060(7) 0.5459(6) 0.4231(7) 0.089(3) Uani 1 1 d U . . N40 N 0.2872(11) -0.3505(11) -0.3188(9) 0.077(5) Uani 1 1 d U . . C41 C 0.2136(13) -0.3985(13) -0.3639(11) 0.064(5) Uani 1 1 d U . . C42 C 0.1187(13) -0.4637(15) -0.4206(12) 0.102(8) Uani 1 1 d U . . H42C H 0.0902 -0.5095 -0.4054 0.152 Uiso 1 1 calc R . . H42B H 0.1235 -0.4897 -0.4749 0.152 Uiso 1 1 calc R . . H42A H 0.0782 -0.4360 -0.4199 0.152 Uiso 1 1 calc R . . N52 N 0.4002(13) 0.6291(13) 0.1992(12) 0.102(6) Uani 1 1 d U . . C53 C 0.4701(15) 0.6256(13) 0.1921(12) 0.071(5) Uani 1 1 d U . . C54 C 0.5599(15) 0.6251(15) 0.1894(13) 0.089(7) Uani 1 1 d U . . H54A H 0.5663 0.5868 0.2097 0.133 Uiso 1 1 calc R . . H54B H 0.6134 0.6848 0.2229 0.133 Uiso 1 1 calc R . . H54C H 0.5610 0.6034 0.1336 0.133 Uiso 1 1 calc R . . N49 N 0.7503(13) 0.7105(11) 0.3899(10) 0.086(5) Uani 1 1 d U . . C50 C 0.7878(14) 0.7814(14) 0.4081(12) 0.072(6) Uani 1 1 d U . . C51 C 0.8410(19) 0.8797(16) 0.4388(18) 0.135(11) Uani 1 1 d U . . N43 N 0.135(2) -0.2674(18) 0.3550(18) 0.140(11) Uani 1 1 d U . . C44 C 0.195(3) -0.2807(17) 0.3401(13) 0.105(9) Uani 1 1 d U . . C45 C 0.292(2) -0.2826(17) 0.3220(18) 0.156(12) Uani 1 1 d U . . H45C H 0.3473 -0.2418 0.3716 0.235 Uiso 1 1 calc R . . H45B H 0.3046 -0.2652 0.2805 0.235 Uiso 1 1 calc R . . H45A H 0.2837 -0.3420 0.3032 0.235 Uiso 1 1 calc R . . N46 N 0.6414(17) -0.1511(17) 0.3239(15) 0.129(8) Uani 1 1 d U . . C47 C 0.578(2) -0.1489(16) 0.2888(15) 0.095(7) Uani 1 1 d U . . C48 C 0.493(2) -0.1489(16) 0.2447(14) 0.116(9) Uani 1 1 d U . . N37 N 0.0470(18) -0.0841(18) -0.463(2) 0.159(11) Uani 1 1 d U . . C38 C 0.122(2) -0.0772(18) -0.465(2) 0.127(11) Uani 1 1 d U . . C39 C 0.2148(18) -0.0654(17) -0.4662(16) 0.123(9) Uani 1 1 d U . . H39C H 0.2153 -0.0899 -0.5221 0.185 Uiso 1 1 calc R . . H39B H 0.2321 -0.0955 -0.4403 0.185 Uiso 1 1 calc R . . H39A H 0.2613 -0.0027 -0.4367 0.185 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb15 0.0260(8) 0.0358(8) 0.0452(9) 0.0120(7) 0.0059(6) 0.0132(7) F16 0.071(8) 0.195(13) 0.214(16) 0.166(13) 0.028(9) 0.052(10) F17 0.161(14) 0.056(6) 0.113(11) -0.008(6) 0.047(10) 0.004(7) F18 0.081(7) 0.104(9) 0.157(12) 0.073(9) 0.082(8) 0.051(7) Sb19 0.0336(6) 0.0534(7) 0.0566(8) 0.0214(6) 0.0144(5) 0.0209(6) F20 0.038(5) 0.073(6) 0.082(6) 0.017(5) 0.034(5) 0.012(5) F21 0.057(6) 0.088(7) 0.099(8) 0.047(6) 0.043(6) 0.022(5) F22 0.064(7) 0.104(9) 0.139(9) 0.071(8) 0.024(7) 0.049(7) F23 0.111(10) 0.105(8) 0.079(6) 0.020(6) 0.043(6) 0.048(7) F24 0.049(5) 0.054(6) 0.093(7) 0.037(5) 0.010(5) 0.006(4) F25 0.069(7) 0.094(8) 0.128(9) 0.077(7) 0.024(6) 0.036(6) Ag1 0.0240(6) 0.0340(7) 0.0504(8) 0.0225(6) 0.0029(5) 0.0095(5) Ag2 0.0154(6) 0.0466(7) 0.0406(7) 0.0109(6) 0.0050(5) 0.0056(5) Ag3 0.0293(6) 0.0373(7) 0.0543(8) 0.0216(6) 0.0222(5) 0.0181(5) N1 0.027(6) 0.032(6) 0.030(6) 0.016(5) 0.007(4) 0.014(5) N1' 0.014(5) 0.030(6) 0.037(7) 0.014(5) 0.001(4) 0.006(5) N1A 0.020(5) 0.030(5) 0.037(5) 0.008(4) 0.013(4) 0.013(4) N1B 0.018(5) 0.034(6) 0.030(6) 0.009(4) 0.005(4) 0.007(4) N1C 0.025(5) 0.043(7) 0.038(6) 0.012(5) 0.011(4) 0.016(5) N1D 0.021(5) 0.038(7) 0.040(5) 0.011(5) 0.012(4) 0.015(5) N12 0.030(7) 0.033(6) 0.057(8) 0.018(6) 0.017(5) 0.013(6) N12' 0.024(6) 0.042(7) 0.053(7) 0.023(6) 0.020(5) 0.020(6) N12A 0.037(7) 0.035(5) 0.063(8) 0.022(5) -0.005(6) 0.008(5) N12B 0.028(5) 0.041(7) 0.044(7) 0.025(6) 0.005(5) 0.011(6) N12C 0.017(5) 0.034(7) 0.038(6) 0.008(6) 0.004(5) 0.002(5) N12D 0.026(6) 0.039(7) 0.041(5) 0.005(5) 0.008(5) 0.005(6) C2 0.023(7) 0.031(8) 0.048(9) 0.021(7) 0.009(6) 0.008(6) C2' 0.024(7) 0.033(8) 0.036(8) 0.014(6) 0.009(5) 0.013(6) C2A 0.017(6) 0.034(7) 0.036(6) 0.011(5) 0.008(5) 0.012(5) C2B 0.013(5) 0.029(7) 0.031(7) 0.006(6) 0.005(5) 0.008(4) C2C 0.024(5) 0.039(8) 0.031(6) 0.019(5) 0.015(4) 0.012(6) C2D 0.024(5) 0.041(9) 0.040(7) 0.009(6) 0.010(5) 0.018(6) C3 0.032(8) 0.035(8) 0.058(10) 0.030(8) 0.015(6) 0.012(7) C3' 0.029(8) 0.029(8) 0.052(10) 0.022(7) 0.010(6) 0.011(6) C3A 0.021(7) 0.038(8) 0.038(7) 0.011(6) 0.003(5) 0.010(6) C3B 0.015(6) 0.035(8) 0.044(9) 0.012(7) -0.004(6) 0.005(5) C3C 0.027(7) 0.041(9) 0.046(8) 0.005(6) 0.023(6) 0.005(6) C3D 0.026(6) 0.066(12) 0.051(9) 0.001(8) 0.014(6) 0.020(7) C4 0.054(10) 0.074(12) 0.070(12) 0.059(10) 0.034(8) 0.033(9) C4' 0.037(8) 0.036(9) 0.056(10) 0.020(7) 0.012(7) 0.026(7) C4A 0.036(8) 0.036(7) 0.036(8) 0.011(6) 0.005(6) 0.018(6) C4B 0.025(7) 0.041(9) 0.062(10) 0.026(8) 0.002(6) 0.003(6) C4C 0.041(8) 0.046(10) 0.052(9) 0.000(7) 0.020(7) 0.016(8) C4D 0.023(7) 0.097(16) 0.074(11) -0.011(10) 0.004(6) 0.023(9) C5 0.026(8) 0.060(10) 0.056(10) 0.038(8) 0.016(7) 0.020(7) C5' 0.020(7) 0.034(9) 0.062(10) 0.022(7) 0.013(6) 0.008(6) C5A 0.033(8) 0.041(7) 0.043(7) 0.020(6) 0.016(6) 0.014(6) C5B 0.023(6) 0.044(9) 0.065(10) 0.034(8) 0.010(6) 0.013(6) C5C 0.036(7) 0.062(11) 0.035(8) 0.007(7) 0.009(6) 0.011(8) C5D 0.025(6) 0.081(14) 0.063(10) -0.022(10) -0.005(7) 0.012(9) C6 0.035(8) 0.033(8) 0.036(8) 0.016(7) 0.013(6) 0.014(7) C6' 0.021(7) 0.029(8) 0.041(9) 0.016(6) 0.003(5) 0.006(6) C6A 0.028(8) 0.041(7) 0.044(7) 0.015(5) 0.012(5) 0.016(5) C6B 0.022(6) 0.043(8) 0.033(7) 0.015(6) 0.012(5) 0.013(5) C6C 0.021(5) 0.045(9) 0.043(7) 0.018(6) 0.012(5) 0.009(6) C6D 0.039(6) 0.072(12) 0.036(7) 0.011(7) 0.008(5) 0.032(8) C7 0.022(8) 0.048(9) 0.056(10) 0.028(8) 0.009(7) 0.017(7) C7' 0.019(7) 0.029(8) 0.040(9) 0.013(6) 0.002(6) 0.005(6) C7A 0.024(8) 0.045(7) 0.051(9) 0.023(6) 0.014(6) 0.011(5) C7B 0.027(7) 0.041(9) 0.044(8) 0.019(7) 0.006(5) 0.013(7) C7C 0.025(6) 0.042(9) 0.059(10) 0.021(8) 0.005(6) 0.017(7) C7D 0.041(9) 0.049(10) 0.035(7) 0.002(7) 0.004(6) 0.024(8) C8 0.014(7) 0.046(8) 0.058(10) 0.027(8) 0.009(7) 0.012(7) C8' 0.020(7) 0.029(8) 0.044(9) 0.013(6) 0.006(6) 0.004(7) C8A 0.032(8) 0.042(7) 0.054(9) 0.017(6) 0.014(6) 0.015(6) C8B 0.031(7) 0.067(11) 0.044(9) 0.033(9) 0.015(6) 0.023(8) C8C 0.033(7) 0.044(10) 0.056(10) 0.014(8) 0.007(7) 0.019(8) C8D 0.040(9) 0.047(10) 0.039(7) 0.017(7) 0.012(6) 0.023(8) C9 0.034(8) 0.042(7) 0.039(9) 0.012(6) 0.017(6) 0.025(6) C9' 0.017(7) 0.023(7) 0.035(8) 0.007(6) 0.001(5) 0.001(6) C9A 0.029(8) 0.043(6) 0.048(8) 0.019(6) 0.013(5) 0.007(6) C9B 0.029(6) 0.039(9) 0.036(8) 0.013(7) 0.003(5) 0.017(6) C9C 0.023(6) 0.033(8) 0.056(8) 0.014(8) 0.011(6) 0.006(7) C9D 0.039(7) 0.040(9) 0.040(6) 0.013(6) 0.011(5) 0.023(7) C10 0.038(9) 0.035(7) 0.060(10) 0.017(7) 0.001(6) 0.014(7) C10' 0.031(8) 0.030(8) 0.046(9) 0.014(7) 0.012(6) 0.013(7) C10A 0.043(9) 0.036(6) 0.052(9) 0.019(6) 0.012(6) 0.014(7) C10B 0.023(7) 0.055(10) 0.044(9) 0.025(8) 0.006(6) 0.010(7) C10C 0.012(6) 0.044(9) 0.051(7) 0.015(8) -0.002(6) -0.005(7) C10D 0.026(7) 0.058(11) 0.042(7) 0.018(7) 0.014(5) 0.014(7) C11 0.037(9) 0.042(7) 0.054(10) 0.013(7) -0.003(7) 0.018(7) C11' 0.023(8) 0.057(9) 0.063(10) 0.037(8) 0.025(7) 0.025(7) C11A 0.036(9) 0.039(6) 0.056(9) 0.025(6) 0.001(6) 0.008(7) C11B 0.027(6) 0.049(10) 0.050(9) 0.030(8) 0.016(6) 0.017(7) C11C 0.024(7) 0.055(10) 0.047(8) 0.019(8) 0.008(6) 0.008(8) C11D 0.026(6) 0.050(10) 0.039(7) 0.000(7) 0.001(5) 0.019(7) C13 0.026(8) 0.027(7) 0.072(11) 0.015(7) 0.005(6) 0.001(6) C13' 0.022(7) 0.034(8) 0.043(9) 0.014(6) 0.012(6) 0.014(7) C13A 0.065(13) 0.040(7) 0.085(13) 0.031(8) -0.031(9) -0.002(9) C13B 0.026(7) 0.088(13) 0.063(11) 0.057(11) 0.001(7) 0.004(9) C13C 0.029(7) 0.054(10) 0.046(7) 0.017(8) 0.013(6) 0.021(8) C13D 0.025(7) 0.061(11) 0.042(7) -0.003(7) 0.000(5) 0.006(8) C14 0.028(9) 0.040(7) 0.078(12) 0.023(7) -0.008(7) 0.003(7) C14' 0.013(7) 0.029(8) 0.053(9) 0.016(6) 0.014(6) 0.006(6) C14A 0.060(12) 0.043(7) 0.073(12) 0.028(8) -0.022(8) -0.002(8) C14B 0.030(6) 0.090(14) 0.062(11) 0.052(11) -0.001(7) 0.005(9) C14C 0.031(7) 0.058(10) 0.041(8) 0.019(8) 0.017(6) 0.017(8) C14D 0.025(6) 0.055(11) 0.047(8) -0.011(8) -0.002(6) 0.010(8) Sb33 0.0464(10) 0.0495(10) 0.0627(11) 0.0178(9) 0.0073(8) 0.0204(9) F34 0.118(11) 0.154(16) 0.27(2) -0.037(13) -0.100(11) 0.073(10) F35 0.116(10) 0.084(8) 0.142(11) 0.041(8) 0.043(9) 0.066(8) F36 0.44(3) 0.161(16) 0.195(19) 0.126(15) 0.22(2) 0.159(18) Sb26 0.0302(6) 0.0883(10) 0.0772(9) 0.0567(8) -0.0015(6) 0.0060(6) F27 0.087(8) 0.217(13) 0.189(11) 0.178(11) 0.067(8) 0.079(8) F28 0.053(6) 0.040(5) 0.075(7) 0.019(5) 0.000(5) 0.003(4) F29 0.034(6) 0.241(12) 0.056(6) 0.035(7) -0.017(5) -0.004(7) F30 0.080(7) 0.054(6) 0.077(7) 0.032(5) 0.027(5) 0.013(5) F31 0.073(8) 0.235(14) 0.266(16) 0.207(12) 0.071(9) 0.089(10) F32 0.059(6) 0.036(5) 0.127(7) 0.021(5) 0.010(5) 0.006(4) N40 0.053(9) 0.082(12) 0.069(11) 0.012(9) 0.006(7) 0.035(9) C41 0.053(10) 0.087(15) 0.053(12) 0.026(10) 0.018(7) 0.042(9) C42 0.048(11) 0.13(2) 0.083(16) 0.050(14) 0.011(9) 0.005(11) N52 0.053(11) 0.110(15) 0.133(17) 0.065(14) 0.032(11) 0.024(11) C53 0.059(12) 0.076(14) 0.074(13) 0.042(11) 0.020(11) 0.023(12) C54 0.092(15) 0.100(17) 0.116(18) 0.069(15) 0.056(15) 0.062(15) N49 0.086(14) 0.060(9) 0.092(13) 0.031(11) 0.033(11) 0.021(10) C50 0.055(13) 0.064(9) 0.079(14) 0.035(12) 0.008(10) 0.014(10) C51 0.10(2) 0.071(11) 0.17(3) 0.063(17) -0.003(18) -0.009(14) N43 0.15(2) 0.103(19) 0.16(3) 0.075(18) 0.006(18) 0.057(18) C44 0.16(3) 0.069(15) 0.033(12) 0.003(11) -0.017(15) 0.05(2) C45 0.12(2) 0.080(19) 0.17(3) 0.018(19) -0.024(19) 0.025(19) N46 0.100(18) 0.15(2) 0.14(2) 0.075(17) 0.045(15) 0.052(17) C47 0.12(2) 0.086(16) 0.085(19) 0.038(15) 0.049(15) 0.049(18) C48 0.20(3) 0.109(19) 0.090(18) 0.043(15) 0.053(16) 0.12(2) N37 0.085(16) 0.14(2) 0.25(3) 0.13(2) 0.03(2) 0.021(17) C38 0.091(17) 0.087(19) 0.18(3) 0.08(2) 0.02(2) 0.02(2) C39 0.092(15) 0.11(2) 0.13(2) 0.065(18) 0.042(18) 0.002(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb15 F17 1.825(11) . ? Sb15 F16 1.838(11) . ? Sb15 F18 1.884(11) . ? Sb19 F22 1.843(10) . ? Sb19 F23 1.851(11) . ? Sb19 F25 1.856(10) . ? Sb19 F20 1.856(10) . ? Sb19 F24 1.878(9) . ? Sb19 F21 1.889(10) . ? Ag1 N12B 2.230(11) 2 y Ag1 N12A 2.347(12) . y Ag1 N1' 2.378(10) . y Ag1 N1 2.388(11) . y Ag2 N12C 2.255(11) 2 y Ag2 N12D 2.267(12) . y Ag2 N1A 2.407(11) . y Ag2 N1B 2.425(11) . y Ag3 N12 2.244(11) 2 y Ag3 N12' 2.315(12) . y Ag3 N1C 2.386(11) . y Ag3 N1D 2.407(10) . y N1 C2 1.317(16) . ? N1 C6 1.382(17) . ? N1' C2' 1.341(16) . ? N1' C6' 1.369(17) . ? N1A C6A 1.365(17) . ? N1A C2A 1.388(16) . ? N1B C6B 1.339(17) . ? N1B C2B 1.341(15) . ? N1C C2C 1.351(16) . ? N1C C6C 1.368(17) . ? N1D C2D 1.349(17) . ? N1D C6D 1.370(18) . ? N12 C11 1.335(18) . ? N12 C13 1.349(18) . ? N12 Ag3 2.244(11) 2 ? N12' C11' 1.321(17) . ? N12' C13' 1.354(17) . ? N12A C13A 1.305(19) . ? N12A C11A 1.348(18) . ? N12B C13B 1.318(18) . ? N12B C11B 1.338(17) . ? N12B Ag1 2.230(11) 2 ? N12C C13C 1.333(17) . ? N12C C11C 1.341(17) . ? N12C Ag2 2.255(11) 2 ? N12D C13D 1.349(17) . ? N12D C11D 1.363(17) . ? C2 C3 1.425(19) . ? C2 C2' 1.520(19) . ? C2' C3' 1.402(18) . ? C2A C3A 1.402(18) . ? C2A C2B 1.471(19) . ? C2B C3B 1.420(18) . ? C2C C3C 1.385(18) . ? C2C C2D 1.507(18) . ? C2D C3D 1.405(19) . ? C3 C4 1.34(2) . ? C3' C4' 1.369(19) . ? C3A C4A 1.383(19) . ? C3B C4B 1.39(2) . ? C3C C4C 1.41(2) . ? C3D C4D 1.38(2) . ? C4 C5 1.37(2) . ? C4' C5' 1.37(2) . ? C4A C5A 1.387(19) . ? C4B C5B 1.395(19) . ? C4C C5C 1.40(2) . ? C4D C5D 1.38(2) . ? C5 C6 1.390(19) . ? C5' C6' 1.394(18) . ? C5A C6A 1.414(19) . ? C5B C6B 1.431(19) . ? C5C C6C 1.40(2) . ? C5D C6D 1.38(2) . ? C6 C7 1.460(19) . ? C6' C7' 1.412(19) . ? C6A C7A 1.44(2) . ? C6B C7B 1.442(18) . ? C6C C7C 1.429(19) . ? C6D C7D 1.45(2) . ? C7 C8 1.186(18) . ? C7' C8' 1.207(18) . ? C7A C8A 1.210(19) . ? C7B C8B 1.190(18) . ? C7C C8C 1.205(19) . ? C7D C8D 1.183(19) . ? C8 C9 1.439(19) . ? C8' C9' 1.465(19) . ? C8A C9A 1.44(2) . ? C8B C9B 1.451(19) . ? C8C C9C 1.43(2) . ? C8D C9D 1.45(2) . ? C9 C10 1.386(19) . ? C9 C14 1.41(2) . ? C9' C14' 1.388(17) . ? C9' C10' 1.407(19) . ? C9A C14A 1.39(2) . ? C9A C10A 1.40(2) . ? C9B C14B 1.37(2) . ? C9B C10B 1.39(2) . ? C9C C10C 1.39(2) . ? C9C C14C 1.40(2) . ? C9D C10D 1.342(19) . ? C9D C14D 1.45(2) . ? C10 C11 1.395(19) . ? C10' C11' 1.393(19) . ? C10A C11A 1.37(2) . ? C10B C11B 1.405(18) . ? C10C C11C 1.388(19) . ? C10D C11D 1.376(19) . ? C13 C14 1.41(2) . ? C13' C14' 1.402(19) . ? C13A C14A 1.42(2) . ? C13B C14B 1.397(19) . ? C13C C14C 1.390(19) . ? C13D C14D 1.41(2) . ? Sb33 F36 1.782(16) 2_656 ? Sb33 F36 1.782(16) . ? Sb33 F34 1.814(14) 2_656 ? Sb33 F34 1.814(14) . ? Sb33 F35 1.865(11) 2_656 ? Sb33 F35 1.865(11) . ? Sb26 F28 1.843(10) . ? Sb26 F29 1.844(12) . ? Sb26 F27 1.849(11) . ? Sb26 F31 1.858(12) . ? Sb26 F30 1.866(10) . ? Sb26 F32 1.873(10) . ? N40 C41 1.12(2) . ? C41 C42 1.45(3) . ? N52 C53 1.16(2) . ? C53 C54 1.44(3) . ? N49 C50 1.11(2) . ? C50 C51 1.52(3) . ? N43 C44 1.13(4) . ? C44 C45 1.64(4) . ? N46 C47 1.18(3) . ? C47 C48 1.52(3) . ? N37 C38 1.16(3) . ? C38 C39 1.41(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F17 Sb15 F16 90.8(8) . . ? F17 Sb15 F18 91.9(6) . . ? F16 Sb15 F18 91.8(6) . . ? F22 Sb19 F23 90.9(6) . . ? F22 Sb19 F25 179.3(6) . . ? F23 Sb19 F25 89.8(6) . . ? F22 Sb19 F20 90.4(5) . . ? F23 Sb19 F20 178.7(5) . . ? F25 Sb19 F20 89.0(5) . . ? F22 Sb19 F24 90.5(5) . . ? F23 Sb19 F24 90.3(5) . . ? F25 Sb19 F24 89.3(4) . . ? F20 Sb19 F24 89.3(4) . . ? F22 Sb19 F21 90.7(5) . . ? F23 Sb19 F21 90.0(5) . . ? F25 Sb19 F21 89.5(5) . . ? F20 Sb19 F21 90.3(4) . . ? F24 Sb19 F21 178.8(5) . . ? N12B Ag1 N12A 120.1(4) 2 . y N12B Ag1 N1' 130.8(4) 2 . y N12A Ag1 N1' 104.3(4) . . y N12B Ag1 N1 119.5(4) 2 . y N12A Ag1 N1 99.2(4) . . y N1' Ag1 N1 68.4(4) . . y N12C Ag2 N12D 126.5(4) 2 . y N12C Ag2 N1A 109.4(4) 2 . y N12D Ag2 N1A 113.1(4) . . y N12C Ag2 N1B 130.8(4) 2 . y N12D Ag2 N1B 94.5(4) . . y N1A Ag2 N1B 69.3(4) . . y N12 Ag3 N12' 118.0(4) 2 . y N12 Ag3 N1C 123.6(4) 2 . y N12' Ag3 N1C 106.9(4) . . y N12 Ag3 N1D 121.1(4) 2 . y N12' Ag3 N1D 108.6(4) . . y N1C Ag3 N1D 68.5(4) . . y C2 N1 C6 118.0(12) . . ? C2 N1 Ag1 119.4(9) . . y C6 N1 Ag1 120.9(8) . . y C2' N1' C6' 119.0(11) . . ? C2' N1' Ag1 119.3(9) . . y C6' N1' Ag1 121.2(9) . . y C6A N1A C2A 117.8(12) . . ? C6A N1A Ag2 123.2(9) . . y C2A N1A Ag2 116.4(9) . . y C6B N1B C2B 121.2(11) . . ? C6B N1B Ag2 120.0(8) . . y C2B N1B Ag2 116.4(9) . . y C2C N1C C6C 118.6(11) . . ? C2C N1C Ag3 120.1(9) . . y C6C N1C Ag3 121.0(9) . . y C2D N1D C6D 119.3(12) . . ? C2D N1D Ag3 118.3(8) . . y C6D N1D Ag3 121.2(9) . . y C11 N12 C13 117.0(12) . . ? C11 N12 Ag3 123.6(10) . 2 y C13 N12 Ag3 118.9(10) . 2 y C11' N12' C13' 117.5(13) . . ? C11' N12' Ag3 117.1(9) . . y C13' N12' Ag3 124.2(9) . . y C13A N12A C11A 116.2(14) . . ? C13A N12A Ag1 116.7(10) . . y C11A N12A Ag1 126.9(10) . . y C13B N12B C11B 118.2(12) . . ? C13B N12B Ag1 122.6(10) . 2 y C11B N12B Ag1 118.9(9) . 2 y C13C N12C C11C 117.7(12) . . ? C13C N12C Ag2 119.4(9) . 2 y C11C N12C Ag2 122.2(10) . 2 y C13D N12D C11D 117.2(13) . . ? C13D N12D Ag2 123.4(10) . . y C11D N12D Ag2 118.9(9) . . y N1 C2 C3 122.2(13) . . ? N1 C2 C2' 115.1(12) . . ? C3 C2 C2' 122.6(13) . . ? N1' C2' C3' 121.7(12) . . ? N1' C2' C2 115.6(11) . . ? C3' C2' C2 122.8(13) . . ? N1A C2A C3A 120.4(13) . . ? N1A C2A C2B 115.0(11) . . ? C3A C2A C2B 124.5(12) . . ? N1B C2B C3B 119.8(13) . . ? N1B C2B C2A 118.6(11) . . ? C3B C2B C2A 121.6(12) . . ? N1C C2C C3C 122.7(12) . . ? N1C C2C C2D 115.2(11) . . ? C3C C2C C2D 122.1(12) . . ? N1D C2D C3D 122.2(13) . . ? N1D C2D C2C 116.5(11) . . ? C3D C2D C2C 121.2(13) . . ? C4 C3 C2 117.8(14) . . ? C4' C3' C2' 119.5(13) . . ? C4A C3A C2A 120.5(13) . . ? C4B C3B C2B 119.2(13) . . ? C2C C3C C4C 119.0(13) . . ? C4D C3D C2D 117.7(15) . . ? C3 C4 C5 122.8(15) . . ? C3' C4' C5' 119.0(13) . . ? C3A C4A C5A 120.4(14) . . ? C5B C4B C3B 121.0(14) . . ? C5C C4C C3C 118.7(14) . . ? C3D C4D C5D 119.9(16) . . ? C4 C5 C6 116.6(14) . . ? C4' C5' C6' 120.4(14) . . ? C4A C5A C6A 117.2(14) . . ? C4B C5B C6B 116.1(14) . . ? C4C C5C C6C 118.9(14) . . ? C6D C5D C4D 120.6(15) . . ? N1 C6 C5 122.7(13) . . ? N1 C6 C7 114.4(12) . . ? C5 C6 C7 122.9(13) . . ? N1' C6' C5' 120.3(13) . . ? N1' C6' C7' 116.4(12) . . ? C5' C6' C7' 123.2(13) . . ? N1A C6A C5A 123.6(13) . . ? N1A C6A C7A 112.6(13) . . ? C5A C6A C7A 123.7(14) . . ? N1B C6B C5B 122.6(12) . . ? N1B C6B C7B 118.8(12) . . ? C5B C6B C7B 118.6(13) . . ? N1C C6C C5C 121.8(13) . . ? N1C C6C C7C 116.3(13) . . ? C5C C6C C7C 121.8(13) . . ? N1D C6D C5D 120.2(14) . . ? N1D C6D C7D 116.3(13) . . ? C5D C6D C7D 123.5(14) . . ? C8 C7 C6 173.4(17) . . ? C8' C7' C6' 178.2(15) . . ? C8A C7A C6A 171.1(17) . . ? C8B C7B C6B 177.4(17) . . ? C8C C7C C6C 173.8(17) . . ? C8D C7D C6D 177.8(18) . . ? C7 C8 C9 177.7(16) . . ? C7' C8' C9' 175.7(14) . . ? C7A C8A C9A 176.5(17) . . ? C7B C8B C9B 176.0(16) . . ? C7C C8C C9C 175.7(18) . . ? C7D C8D C9D 177.0(16) . . ? C10 C9 C14 117.9(13) . . ? C10 C9 C8 121.8(13) . . ? C14 C9 C8 120.3(13) . . ? C14' C9' C10' 117.3(13) . . ? C14' C9' C8' 122.0(13) . . ? C10' C9' C8' 120.7(12) . . ? C14A C9A C10A 116.9(14) . . ? C14A C9A C8A 121.9(14) . . ? C10A C9A C8A 121.1(14) . . ? C14B C9B C10B 116.3(13) . . ? C14B C9B C8B 123.3(14) . . ? C10B C9B C8B 120.4(13) . . ? C10C C9C C14C 117.5(13) . . ? C10C C9C C8C 121.7(14) . . ? C14C C9C C8C 120.7(15) . . ? C10D C9D C8D 123.8(14) . . ? C10D C9D C14D 117.4(14) . . ? C8D C9D C14D 118.8(13) . . ? C9 C10 C11 118.0(14) . . ? C11' C10' C9' 117.9(13) . . ? C11A C10A C9A 119.3(14) . . ? C9B C10B C11B 119.5(13) . . ? C11C C10C C9C 119.5(14) . . ? C9D C10D C11D 121.7(14) . . ? N12 C11 C10 125.4(14) . . ? N12' C11' C10' 125.1(14) . . ? N12A C11A C10A 124.5(14) . . ? N12B C11B C10B 122.5(14) . . ? N12C C11C C10C 122.9(15) . . ? N12D C11D C10D 123.1(13) . . ? N12 C13 C14 121.9(14) . . ? N12' C13' C14' 121.4(13) . . ? N12A C13A C14A 124.4(16) . . ? N12B C13B C14B 121.9(15) . . ? N12C C13C C14C 123.5(14) . . ? N12D C13D C14D 122.8(14) . . ? C9 C14 C13 119.8(14) . . ? C9' C14' C13' 120.7(13) . . ? C9A C14A C13A 118.3(15) . . ? C9B C14B C13B 121.5(15) . . ? C13C C14C C9C 118.8(14) . . ? C13D C14D C9D 117.9(13) . . ? F36 Sb33 F36 180.000(3) 2_656 . ? F36 Sb33 F34 88.8(13) 2_656 2_656 ? F36 Sb33 F34 91.2(13) . 2_656 ? F36 Sb33 F34 91.2(13) 2_656 . ? F36 Sb33 F34 88.8(13) . . ? F34 Sb33 F34 180.000(2) 2_656 . ? F36 Sb33 F35 89.2(7) 2_656 2_656 ? F36 Sb33 F35 90.8(7) . 2_656 ? F34 Sb33 F35 88.1(7) 2_656 2_656 ? F34 Sb33 F35 91.9(7) . 2_656 ? F36 Sb33 F35 90.8(7) 2_656 . ? F36 Sb33 F35 89.2(7) . . ? F34 Sb33 F35 91.9(7) 2_656 . ? F34 Sb33 F35 88.1(7) . . ? F35 Sb33 F35 180.0(10) 2_656 . ? F28 Sb26 F29 90.1(6) . . ? F28 Sb26 F27 89.9(5) . . ? F29 Sb26 F27 89.8(7) . . ? F28 Sb26 F31 177.6(7) . . ? F29 Sb26 F31 92.2(8) . . ? F27 Sb26 F31 90.3(6) . . ? F28 Sb26 F30 90.4(5) . . ? F29 Sb26 F30 91.0(5) . . ? F27 Sb26 F30 179.2(6) . . ? F31 Sb26 F30 89.4(5) . . ? F28 Sb26 F32 88.4(4) . . ? F29 Sb26 F32 178.5(6) . . ? F27 Sb26 F32 90.1(6) . . ? F31 Sb26 F32 89.3(7) . . ? F30 Sb26 F32 89.1(5) . . ? N40 C41 C42 177(2) . . ? N52 C53 C54 176(2) . . ? N49 C50 C51 176(2) . . ? N43 C44 C45 170(3) . . ? N46 C47 C48 177(3) . . ? N37 C38 C39 178(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.17 _refine_diff_density_min -1.56 _refine_diff_density_rms 0.23 #===END data_Compound_4_(AGCOBQ) _database_code_CSD 201518 _refine_special_details ; 1. The cobaltocarborate anions were refined using extensive distance and similarity restraints. 2. The BF4- anion is partially disordered and two F atoms were modelled across three 2/3-occupied sites. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexa[bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl silver penta-cobaltocarborate tetrafluoroborate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C178 H220 Ag6 B91 Co5 F4 N28 O1.50' _chemical_formula_weight 4777.40 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' B B 0.0013 0.0007 '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' Co Co 0.3494 0.9721 '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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.7177(10) _cell_length_b 20.1484(12) _cell_length_c 20.3876(12) _cell_angle_alpha 74.800(2) _cell_angle_beta 70.7470(2) _cell_angle_gamma 86.5800(2) _cell_volume 5879.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16829 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.3 _exptl_crystal_description column _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method ? _exptl_crystal_F_000 2404 _exptl_absorpt_coefficient_mu 0.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker SADABS, 1996' _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 53172 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 26.00 _reflns_number_total 22869 _reflns_number_gt 16377 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OLEX (Oleg V. Dolomanov, 2001)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.1496P)^2^+42.5013P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22869 _refine_ls_number_parameters 1126 _refine_ls_number_restraints 394 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.2974 _refine_ls_wR_factor_gt 0.2559 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.40672(4) 0.40367(3) -0.10368(3) 0.04499(16) Uani 1 1 d U . . Ag2 Ag 0.03939(4) 0.57393(4) 0.27404(4) 0.0581(2) Uani 1 1 d U . . Ag3 Ag 0.07548(5) 0.81825(3) -0.17065(4) 0.05609(19) Uani 1 1 d U . . N1 N 0.5289(3) 0.3593(3) -0.1845(3) 0.0344(12) Uani 1 1 d U . . N1' N 0.5328(4) 0.3826(3) -0.0630(3) 0.0375(12) Uani 1 1 d U . . N1A N 0.0739(4) 0.5219(4) 0.3816(4) 0.0510(15) Uani 1 1 d U . . N1B N 0.0832(4) 0.6585(4) 0.3213(4) 0.0476(14) Uani 1 1 d U . . N1C N 0.2129(5) 0.8830(3) -0.2198(3) 0.0438(13) Uani 1 1 d U . . N1D N 0.0506(5) 0.9394(3) -0.1870(4) 0.0476(14) Uani 1 1 d U . . N12 N 0.1004(4) 0.4102(4) -0.2695(4) 0.0510(17) Uani 1 1 d U . . H12A H 0.0463 0.4165 -0.2705 0.061 Uiso 1 1 calc R . . N12' N 0.1563(4) 0.5336(4) 0.1951(3) 0.0494(16) Uani 1 1 d U . . N12A N -0.0315(5) 0.2512(4) 0.2232(4) 0.0549(17) Uani 1 1 d U . . H12B H -0.0438 0.2255 0.1996 0.066 Uiso 1 1 calc R . . N12B N 0.0655(6) 0.7858(4) -0.0507(4) 0.065(2) Uani 1 1 d U . . N12C N 0.3570(4) 0.5074(3) -0.1425(3) 0.0405(13) Uani 1 1 d U . . N12D N -0.3181(5) 0.6892(4) 0.0271(4) 0.061(2) Uani 1 1 d U . . H12C H -0.3475 0.6529 0.0569 0.074 Uiso 1 1 calc R . . C2 C 0.6055(4) 0.3451(4) -0.1692(4) 0.0367(14) Uani 1 1 d U . . C2' C 0.6053(5) 0.3525(4) -0.0993(4) 0.0390(15) Uani 1 1 d U . . C2A C 0.0964(5) 0.5627(5) 0.4166(4) 0.0506(17) Uani 1 1 d U . . C2B C 0.0904(5) 0.6379(5) 0.3871(4) 0.0477(16) Uani 1 1 d U . . C2C C 0.2117(5) 0.9524(4) -0.2356(4) 0.0449(16) Uani 1 1 d U . . C2D C 0.1217(5) 0.9825(4) -0.2151(4) 0.0417(15) Uani 1 1 d U . . C3 C 0.6819(5) 0.3249(5) -0.2182(5) 0.056(2) Uani 1 1 d U . . H3A H 0.7352 0.3157 -0.2074 0.067 Uiso 1 1 calc R . . C3' C 0.6743(6) 0.3302(6) -0.0714(5) 0.063(3) Uani 1 1 d U . . H3'A H 0.7250 0.3110 -0.0978 0.075 Uiso 1 1 calc R . . C3A C 0.1261(6) 0.5355(6) 0.4747(5) 0.061(2) Uani 1 1 d U . . H3AA H 0.1417 0.5641 0.4983 0.073 Uiso 1 1 calc R . . C3B C 0.0945(5) 0.6857(5) 0.4255(5) 0.0546(19) Uani 1 1 d U . . H3BA H 0.0970 0.6709 0.4720 0.065 Uiso 1 1 calc R . . C3C C 0.2900(6) 0.9919(5) -0.2692(6) 0.066(3) Uani 1 1 d U . . H3CA H 0.2880 1.0396 -0.2794 0.079 Uiso 1 1 calc R . . C3D C 0.1107(6) 1.0531(4) -0.2220(5) 0.057(2) Uani 1 1 d U . . H3DA H 0.1607 1.0830 -0.2408 0.068 Uiso 1 1 calc R . . C4 C 0.6765(6) 0.3191(7) -0.2817(6) 0.078(3) Uani 1 1 d U . . H4A H 0.7268 0.3067 -0.3153 0.093 Uiso 1 1 calc R . . C4' C 0.6672(8) 0.3368(8) -0.0041(6) 0.088(4) Uani 1 1 d U . . H4'A H 0.7133 0.3219 0.0149 0.106 Uiso 1 1 calc R . . C4A C 0.1321(8) 0.4659(6) 0.4966(6) 0.074(3) Uani 1 1 d U . . H4AA H 0.1517 0.4474 0.5358 0.089 Uiso 1 1 calc R . . C4B C 0.0947(6) 0.7537(6) 0.3933(6) 0.065(2) Uani 1 1 d U . . H4BA H 0.0985 0.7857 0.4180 0.078 Uiso 1 1 calc R . . C4C C 0.3705(7) 0.9606(6) -0.2873(9) 0.105(5) Uani 1 1 d U . . H4CA H 0.4237 0.9868 -0.3110 0.126 Uiso 1 1 calc R . . C4D C 0.0251(7) 1.0776(5) -0.2007(6) 0.073(3) Uani 1 1 d U . . H4DA H 0.0174 1.1247 -0.2065 0.087 Uiso 1 1 calc R . . C5 C 0.5963(6) 0.3315(6) -0.2965(5) 0.066(3) Uani 1 1 d U . . H5A H 0.5912 0.3261 -0.3389 0.079 Uiso 1 1 calc R . . C5' C 0.5927(8) 0.3651(7) 0.0348(6) 0.083(4) Uani 1 1 d U . . H5'A H 0.5865 0.3688 0.0807 0.100 Uiso 1 1 calc R . . C5A C 0.1104(8) 0.4227(6) 0.4629(6) 0.073(3) Uani 1 1 d U . . H5AA H 0.1152 0.3753 0.4776 0.088 Uiso 1 1 calc R . . C5B C 0.0895(6) 0.7764(5) 0.3251(5) 0.060(2) Uani 1 1 d U . . H5BA H 0.0899 0.8231 0.3027 0.072 Uiso 1 1 calc R . . C5C C 0.3724(7) 0.8893(6) -0.2703(8) 0.094(4) Uani 1 1 d U . . H5CA H 0.4266 0.8668 -0.2819 0.113 Uiso 1 1 calc R . . C5D C -0.0477(6) 1.0346(5) -0.1714(6) 0.068(3) Uani 1 1 d U . . H5DA H -0.1057 1.0506 -0.1558 0.082 Uiso 1 1 calc R . . C6 C 0.5240(5) 0.3523(5) -0.2462(4) 0.0446(17) Uani 1 1 d U . . C6' C 0.5263(6) 0.3885(5) 0.0029(4) 0.0490(18) Uani 1 1 d U . . C6A C 0.0803(6) 0.4539(5) 0.4047(5) 0.0584(19) Uani 1 1 d U . . C6B C 0.0835(5) 0.7263(5) 0.2913(5) 0.0538(18) Uani 1 1 d U . . C6C C 0.2925(6) 0.8530(5) -0.2362(5) 0.057(2) Uani 1 1 d U . . C6D C -0.0318(6) 0.9636(4) -0.1653(5) 0.058(2) Uani 1 1 d U . . C7 C 0.4383(5) 0.3679(5) -0.2577(4) 0.0507(19) Uani 1 1 d U . . C7' C 0.4478(6) 0.4192(5) 0.0404(4) 0.053(2) Uani 1 1 d U . . C7A C 0.0550(7) 0.4113(6) 0.3663(6) 0.068(3) Uani 1 1 d U . . C7B C 0.0780(6) 0.7438(5) 0.2186(5) 0.059(2) Uani 1 1 d U . . C7C C 0.2920(6) 0.7785(4) -0.2156(5) 0.0527(19) Uani 1 1 d U . . C7D C -0.1043(7) 0.9127(5) -0.1308(6) 0.069(3) Uani 1 1 d U . . C8 C 0.3658(6) 0.3781(5) -0.2633(5) 0.058(2) Uani 1 1 d U . . C8' C 0.3812(6) 0.4452(5) 0.0712(4) 0.054(2) Uani 1 1 d U . . C8A C 0.0338(6) 0.3763(6) 0.3369(6) 0.068(3) Uani 1 1 d U . . C8B C 0.0744(6) 0.7521(5) 0.1608(5) 0.061(2) Uani 1 1 d U . . C8C C 0.2984(6) 0.7179(4) -0.1998(4) 0.0490(18) Uani 1 1 d U . . C8D C -0.1573(7) 0.8655(5) -0.1009(7) 0.076(3) Uani 1 1 d U . . C9 C 0.2763(6) 0.3899(5) -0.2666(5) 0.0523(19) Uani 1 1 d U . . C9' C 0.3034(6) 0.4745(5) 0.1126(4) 0.0509(19) Uani 1 1 d U . . C9A C 0.0112(6) 0.3339(5) 0.2979(6) 0.059(2) Uani 1 1 d U . . C9B C 0.0711(7) 0.7636(6) 0.0892(5) 0.063(2) Uani 1 1 d U . . C9C C 0.3161(5) 0.6462(4) -0.1814(4) 0.0413(15) Uani 1 1 d U . . C9D C -0.2128(7) 0.8062(5) -0.0588(6) 0.070(3) Uani 1 1 d U . . C10 C 0.2432(7) 0.3615(8) -0.3080(6) 0.085(4) Uani 1 1 d U . . H10A H 0.2798 0.3349 -0.3366 0.102 Uiso 1 1 calc R . . C10' C 0.2300(7) 0.4938(5) 0.0892(5) 0.062(2) Uani 1 1 d U . . H10B H 0.2295 0.4879 0.0456 0.074 Uiso 1 1 calc R . . C10A C 0.0000(6) 0.2634(5) 0.3257(5) 0.062(2) Uani 1 1 d U . . H10C H 0.0061 0.2428 0.3704 0.074 Uiso 1 1 calc R . . C10B C 0.0463(10) 0.7120(6) 0.0651(6) 0.084(3) Uani 1 1 d U . . H10D H 0.0306 0.6682 0.0959 0.101 Uiso 1 1 calc R . . C10C C 0.4015(5) 0.6230(4) -0.2114(4) 0.0413(15) Uani 1 1 d U . . H10E H 0.4464 0.6536 -0.2456 0.050 Uiso 1 1 calc R . . C10D C -0.1894(9) 0.7435(7) -0.0668(8) 0.111(6) Uani 1 1 d U . . H10F H -0.1362 0.7384 -0.1024 0.134 Uiso 1 1 calc R . . C11 C 0.1552(7) 0.3727(7) -0.3068(6) 0.075(3) Uani 1 1 d U . . H11A H 0.1339 0.3520 -0.3344 0.090 Uiso 1 1 calc R . . C11' C 0.1580(7) 0.5220(6) 0.1319(5) 0.062(2) Uani 1 1 d U . . H11B H 0.1081 0.5337 0.1169 0.074 Uiso 1 1 calc R . . C11A C -0.0203(6) 0.2243(5) 0.2867(5) 0.058(2) Uani 1 1 d U . . H11C H -0.0265 0.1768 0.3055 0.070 Uiso 1 1 calc R . . C11B C 0.0448(10) 0.7256(6) -0.0049(6) 0.087(4) Uani 1 1 d U . . H11D H 0.0283 0.6900 -0.0198 0.104 Uiso 1 1 calc R . . C11C C 0.4191(5) 0.5548(4) -0.1904(4) 0.0433(16) Uani 1 1 d U . . H11E H 0.4771 0.5405 -0.2102 0.052 Uiso 1 1 calc R . . C11D C -0.2416(9) 0.6861(6) -0.0238(8) 0.110(6) Uani 1 1 d U . . H11F H -0.2221 0.6433 -0.0310 0.132 Uiso 1 1 calc R . . C12D C -0.2950(10) 0.8083(7) -0.0102(11) 0.145(9) Uani 1 1 d U . . H12D H -0.3176 0.8506 -0.0036 0.174 Uiso 1 1 calc R . . C13 C 0.1315(8) 0.4385(6) -0.2297(7) 0.082(4) Uani 1 1 d U . . H13A H 0.0935 0.4658 -0.2027 0.099 Uiso 1 1 calc R . . C13' C 0.2268(6) 0.5144(5) 0.2157(4) 0.055(2) Uani 1 1 d U . . H13B H 0.2266 0.5216 0.2590 0.066 Uiso 1 1 calc R . . C13A C -0.0230(7) 0.3194(5) 0.1974(6) 0.060(2) Uani 1 1 d U . . H13C H -0.0324 0.3387 0.1538 0.072 Uiso 1 1 calc R . . C13B C 0.0897(15) 0.8336(7) -0.0288(7) 0.138(8) Uani 1 1 d U . . H13D H 0.1062 0.8766 -0.0610 0.165 Uiso 1 1 calc R . . C13C C 0.2746(5) 0.5301(4) -0.1151(4) 0.0387(15) Uani 1 1 d U . . H13E H 0.2306 0.4981 -0.0822 0.046 Uiso 1 1 calc R . . C13D C -0.3460(9) 0.7500(6) 0.0295(10) 0.130(7) Uani 1 1 d U . . H13F H -0.4038 0.7545 0.0598 0.156 Uiso 1 1 calc R . . C14 C 0.2187(7) 0.4290(6) -0.2266(7) 0.077(3) Uani 1 1 d U . . H14A H 0.2377 0.4492 -0.1975 0.092 Uiso 1 1 calc R . . C14' C 0.3013(6) 0.4844(5) 0.1775(4) 0.053(2) Uani 1 1 d U . . H14B H 0.3490 0.4713 0.1951 0.063 Uiso 1 1 calc R . . C14A C -0.0018(7) 0.3614(5) 0.2309(6) 0.063(2) Uani 1 1 d U . . H14C H 0.0044 0.4086 0.2101 0.075 Uiso 1 1 calc R . . C14B C 0.0927(14) 0.8244(7) 0.0416(7) 0.126(7) Uani 1 1 d U . . H14D H 0.1098 0.8611 0.0547 0.151 Uiso 1 1 calc R . . C14C C 0.2508(5) 0.5964(4) -0.1320(4) 0.0428(16) Uani 1 1 d U . . H14E H 0.1921 0.6090 -0.1113 0.051 Uiso 1 1 calc R . . Co1 Co 0.33245(10) 0.76232(10) 0.52911(7) 0.0802(5) Uani 1 1 d . . . C100 C 0.3175(11) 0.8234(9) 0.4365(11) 0.142(7) Uiso 1 1 d DU . . H100 H 0.3351 0.7803 0.4112 0.170 Uiso 1 1 calc R . . C101 C 0.2114(18) 0.8019(10) 0.5144(12) 0.189(10) Uiso 1 1 d DU . . H101 H 0.1774 0.7520 0.5257 0.227 Uiso 1 1 calc R . . C111 C 0.2925(12) 0.6571(8) 0.5034(8) 0.130(6) Uiso 1 1 d DU . . H111 H 0.2495 0.6836 0.4722 0.156 Uiso 1 1 calc R . . C112 C 0.3994(13) 0.6894(8) 0.4702(9) 0.136(6) Uiso 1 1 d DU . . H112 H 0.4085 0.7363 0.4259 0.163 Uiso 1 1 calc R . . B102 B 0.2462(13) 0.8174(10) 0.5853(12) 0.147(8) Uiso 1 1 d DU . . H102 H 0.2308 0.7726 0.6323 0.177 Uiso 1 1 calc R . . B103 B 0.3622(11) 0.8427(9) 0.5507(8) 0.110(5) Uiso 1 1 d DU . . H103 H 0.4001 0.8079 0.5817 0.132 Uiso 1 1 calc R . . B104 B 0.4110(9) 0.8447(7) 0.4593(7) 0.077(3) Uiso 1 1 d DU . . H104 H 0.4711 0.8137 0.4453 0.092 Uiso 1 1 calc R . . B105 B 0.3510(12) 0.9100(9) 0.4156(11) 0.162(10) Uiso 1 1 d DU . . H105 H 0.3845 0.9409 0.3605 0.195 Uiso 1 1 calc R . . B106 B 0.2322(12) 0.8829(10) 0.4480(10) 0.146(8) Uiso 1 1 d DU . . H106 H 0.1904 0.8961 0.4126 0.176 Uiso 1 1 calc R . . B107 B 0.1878(13) 0.8798(10) 0.5409(10) 0.157(9) Uiso 1 1 d DU . . H107 H 0.1174 0.8914 0.5671 0.188 Uiso 1 1 calc R . . B108 B 0.2794(13) 0.9052(10) 0.5650(11) 0.162(10) Uiso 1 1 d DU . . H108 H 0.2679 0.9328 0.6070 0.194 Uiso 1 1 calc R . . B109 B 0.3810(19) 0.9235(10) 0.4875(11) 0.238(18) Uiso 1 1 d DU . . H109 H 0.4325 0.9619 0.4801 0.285 Uiso 1 1 calc R . . B110 B 0.2693(13) 0.9441(9) 0.4802(9) 0.129(7) Uiso 1 1 d DU . . H110 H 0.2493 0.9979 0.4667 0.155 Uiso 1 1 calc R . . B113 B 0.4300(6) 0.6964(5) 0.5392(5) 0.050(2) Uiso 1 1 d DU . . H113 H 0.4577 0.7492 0.5243 0.061 Uiso 1 1 calc R . . B114 B 0.3472(6) 0.6876(5) 0.6146(5) 0.049(2) Uiso 1 1 d DU . . H114 H 0.3371 0.7335 0.6357 0.059 Uiso 1 1 calc R . . B115 B 0.2524(12) 0.6607(9) 0.5965(10) 0.134(7) Uiso 1 1 d DU . . H115 H 0.1919 0.6915 0.6098 0.161 Uiso 1 1 calc R . . B116 B 0.2879(9) 0.5821(7) 0.5725(7) 0.092(4) Uiso 1 1 d DU . . H116 H 0.2383 0.5405 0.5850 0.110 Uiso 1 1 calc R . . B117 B 0.3802(11) 0.5990(9) 0.4920(9) 0.150(9) Uiso 1 1 d DU . . H117 H 0.3946 0.5714 0.4498 0.181 Uiso 1 1 calc R . . B118 B 0.4663(12) 0.6231(8) 0.5121(9) 0.140(8) Uiso 1 1 d DU . . H118 H 0.5367 0.6131 0.4837 0.168 Uiso 1 1 calc R . . B119 B 0.4255(9) 0.6193(6) 0.6065(7) 0.091(4) Uiso 1 1 d DU . . H119 H 0.4689 0.6044 0.6403 0.110 Uiso 1 1 calc R . . B120 B 0.3117(9) 0.6001(7) 0.6431(8) 0.102(5) Uiso 1 1 d DU . . H120 H 0.2784 0.5750 0.7003 0.122 Uiso 1 1 calc R . . B121 B 0.3908(10) 0.5563(8) 0.5776(8) 0.126(7) Uiso 1 1 d DU . . H121 H 0.4092 0.5022 0.5917 0.151 Uiso 1 1 calc R . . Co2 Co 0.28392(8) 0.20484(6) 0.40723(6) 0.0509(3) Uani 1 1 d . . . C200 C 0.2920(6) 0.1419(5) 0.3429(5) 0.062(2) Uiso 1 1 d DU . . H200 H 0.2646 0.1035 0.3947 0.074 Uiso 1 1 calc R . . C201 C 0.2245(8) 0.2058(5) 0.3338(6) 0.073(3) Uiso 1 1 d DU . . H201 H 0.1642 0.1976 0.3820 0.088 Uiso 1 1 calc R . . C211 C 0.1982(5) 0.1462(4) 0.5001(4) 0.0472(18) Uiso 1 1 d DU . . H211 H 0.1882 0.1237 0.4594 0.057 Uiso 1 1 calc R . . C212 C 0.2994(8) 0.1378(6) 0.4967(6) 0.079(3) Uiso 1 1 d DU . . H212 H 0.3381 0.1096 0.4574 0.095 Uiso 1 1 calc R . . B202 B 0.2768(9) 0.2852(7) 0.3211(7) 0.091(4) Uiso 1 1 d DU . . H202 H 0.2426 0.3155 0.3596 0.109 Uiso 1 1 calc R . . B203 B 0.3880(10) 0.2639(7) 0.3188(7) 0.095(4) Uiso 1 1 d DU . . H203 H 0.4100 0.2844 0.3558 0.114 Uiso 1 1 calc R . . B204 B 0.3952(8) 0.1734(6) 0.3351(6) 0.076(3) Uiso 1 1 d DU . . H204 H 0.4192 0.1506 0.3808 0.091 Uiso 1 1 calc R . . B205 B 0.3793(8) 0.1476(6) 0.2620(6) 0.076(3) Uiso 1 1 d DU . . H205 H 0.4137 0.1031 0.2443 0.091 Uiso 1 1 calc R . . B206 B 0.2666(9) 0.1681(7) 0.2620(7) 0.101(5) Uiso 1 1 d DU . . H206 H 0.2266 0.1376 0.2445 0.122 Uiso 1 1 calc R . . B207 B 0.2601(9) 0.2610(7) 0.2470(7) 0.098(5) Uiso 1 1 d DU . . H207 H 0.2155 0.2908 0.2190 0.117 Uiso 1 1 calc R . . B208 B 0.3647(9) 0.2950(7) 0.2368(7) 0.093(4) Uiso 1 1 d DU . . H208 H 0.3894 0.3462 0.2014 0.112 Uiso 1 1 calc R . . B209 B 0.4354(8) 0.2260(6) 0.2450(6) 0.079(3) Uiso 1 1 d DU . . H209 H 0.5077 0.2327 0.2138 0.094 Uiso 1 1 calc R . . B210 B 0.3575(8) 0.2225(6) 0.2015(7) 0.085(4) Uiso 1 1 d DU . . H210 H 0.3768 0.2263 0.1436 0.102 Uiso 1 1 calc R . . B213 B 0.3450(11) 0.2221(7) 0.4765(8) 0.113(6) Uiso 1 1 d DU . . H213 H 0.4062 0.2343 0.4291 0.136 Uiso 1 1 calc R . . B214 B 0.2575(10) 0.2810(9) 0.4688(8) 0.109(5) Uiso 1 1 d DU . . H214 H 0.2764 0.3223 0.4186 0.131 Uiso 1 1 calc R . . B215 B 0.1638(9) 0.2308(6) 0.4824(6) 0.077(3) Uiso 1 1 d DU . . H215 H 0.1355 0.2466 0.4381 0.093 Uiso 1 1 calc R . . B216 B 0.1340(7) 0.1754(5) 0.5725(5) 0.063(3) Uiso 1 1 d DU . . H216 H 0.0636 0.1589 0.6039 0.076 Uiso 1 1 calc R . . B217 B 0.2181(7) 0.1153(6) 0.5815(6) 0.069(3) Uiso 1 1 d DU . . H217 H 0.2047 0.0627 0.6166 0.083 Uiso 1 1 calc R . . B218 B 0.3128(10) 0.1674(8) 0.5669(8) 0.127(7) Uiso 1 1 d DU . . H218 H 0.3631 0.1476 0.5935 0.152 Uiso 1 1 calc R . . B219 B 0.2828(10) 0.2562(8) 0.5500(8) 0.131(7) Uiso 1 1 d DU . . H219 H 0.3132 0.2942 0.5664 0.157 Uiso 1 1 calc R . . B220 B 0.1684(9) 0.2612(7) 0.5552(7) 0.098(5) Uiso 1 1 d DU . . H220 H 0.1225 0.3002 0.5750 0.117 Uiso 1 1 calc R . . B221 B 0.2072(9) 0.1922(7) 0.6146(8) 0.105(5) Uiso 1 1 d DU . . H221 H 0.1880 0.1887 0.6724 0.126 Uiso 1 1 calc R . . Co3 Co 0.49322(16) 0.00889(13) 0.07777(12) 0.0519(5) Uani 0.50 1 d P A -1 C300 C 0.455(2) -0.0636(15) 0.1719(16) 0.117(10) Uiso 0.50 1 d PDU B -1 H300 H 0.5132 -0.0377 0.1741 0.141 Uiso 0.50 1 calc PR B -1 C301 C 0.3813(17) -0.0100(13) 0.1738(12) 0.099(8) Uiso 0.50 1 d PDU B -1 H301 H 0.4028 0.0386 0.1794 0.119 Uiso 0.50 1 calc PR B -1 C311 C 0.5691(18) 0.0608(13) 0.1150(16) 0.122(11) Uiso 0.50 1 d PDU C -1 C312 C 0.6286(18) 0.0140(13) 0.0627(11) 0.103(8) Uiso 0.50 1 d PDU C -1 H312 H 0.6168 -0.0405 0.0927 0.124 Uiso 0.50 1 calc PR C -1 B302 B 0.3560(15) 0.0012(10) 0.0941(10) 0.074(6) Uiso 0.50 1 d PDU B -1 H302 H 0.3643 0.0549 0.0617 0.088 Uiso 0.50 1 calc PR B -1 B303 B 0.4223(15) -0.0543(11) 0.0435(12) 0.087(8) Uiso 0.50 1 d PDU B -1 H303 H 0.4600 -0.0290 -0.0128 0.105 Uiso 0.50 1 calc PR B -1 B304 B 0.4909(17) -0.0972(17) 0.0951(13) 0.127(13) Uiso 0.50 1 d PDU B -1 H304 H 0.5636 -0.0927 0.0651 0.153 Uiso 0.50 1 calc PR B -1 B305 B 0.4201(19) -0.1481(15) 0.1788(14) 0.139(15) Uiso 0.50 1 d PDU B -1 H305 H 0.4448 -0.1962 0.2058 0.167 Uiso 0.50 1 calc PR B -1 B306 B 0.345(2) -0.0931(15) 0.2326(16) 0.18(2) Uiso 0.50 1 d PDU B -1 H306 H 0.3208 -0.1063 0.2917 0.216 Uiso 0.50 1 calc PR B -1 B307 B 0.2826(14) -0.0488(11) 0.1782(11) 0.094(9) Uiso 0.50 1 d PDU B -1 H307 H 0.2150 -0.0318 0.2044 0.113 Uiso 0.50 1 calc PR B -1 B308 B 0.3071(14) -0.0773(11) 0.0981(11) 0.100(9) Uiso 0.50 1 d PDU B -1 H308 H 0.2549 -0.0794 0.0736 0.120 Uiso 0.50 1 calc PR B -1 B309 B 0.3926(15) -0.1398(11) 0.0992(12) 0.112(11) Uiso 0.50 1 d PDU B -1 H309 H 0.3964 -0.1835 0.0755 0.134 Uiso 0.50 1 calc PR B -1 B310 B 0.3065(16) -0.1361(11) 0.1802(11) 0.089(8) Uiso 0.50 1 d PDU B -1 H310 H 0.2549 -0.1778 0.2078 0.107 Uiso 0.50 1 calc PR B -1 B313 B 0.6051(14) 0.0242(10) -0.0190(12) 0.072(6) Uiso 0.50 1 d PDU C -1 H313 H 0.5884 -0.0237 -0.0289 0.086 Uiso 0.50 1 calc PR C -1 B314 B 0.5196(14) 0.0867(12) -0.0172(14) 0.103(10) Uiso 0.50 1 d PDU C -1 H314 H 0.4592 0.0697 -0.0249 0.123 Uiso 0.50 1 calc PR C -1 B315 B 0.5053(17) 0.1100(14) 0.0646(12) 0.085(8) Uiso 0.50 1 d PDU C -1 H315 H 0.4334 0.1029 0.0968 0.103 Uiso 0.50 1 calc PR C -1 B316 B 0.5988(17) 0.1488(12) 0.0742(16) 0.125(13) Uiso 0.50 1 d PDU C -1 H316 H 0.5964 0.1862 0.1056 0.150 Uiso 0.50 1 calc PR C -1 B317 B 0.6834(18) 0.0872(13) 0.0653(13) 0.18(2) Uiso 0.50 1 d PDU C -1 H317 H 0.7376 0.0863 0.0885 0.213 Uiso 0.50 1 calc PR C -1 B318 B 0.7020(13) 0.0661(10) -0.0178(11) 0.081(7) Uiso 0.50 1 d PDU C -1 H318 H 0.7702 0.0516 -0.0462 0.097 Uiso 0.50 1 calc PR C -1 B319 B 0.6343(13) 0.1121(9) -0.0665(10) 0.074(6) Uiso 0.50 1 d PDU C -1 H319 H 0.6589 0.1277 -0.1256 0.089 Uiso 0.50 1 calc PR C -1 B320 B 0.5651(15) 0.1665(11) -0.0178(15) 0.121(12) Uiso 0.50 1 d PDU C -1 H320 H 0.5420 0.2156 -0.0442 0.145 Uiso 0.50 1 calc PR C -1 B321 B 0.6762(16) 0.1514(10) -0.0134(12) 0.083(7) Uiso 0.50 1 d PDU C -1 H321 H 0.7251 0.1950 -0.0389 0.100 Uiso 0.50 1 calc PR C -1 H311 H 0.5032 0.0554 0.1541 0.100 Uiso 0.50 1 d PR C -1 N403 N 0.0653(12) 0.0797(10) 0.4232(10) 0.100 Uiso 0.676(14) 1 d PU D -1 C404 C 0.0500(15) 0.0412(12) 0.4021(12) 0.100 Uiso 0.676(14) 1 d PU D -1 C405 C 0.0116(15) -0.0089(11) 0.3854(12) 0.100 Uiso 0.676(14) 1 d PU D -1 H40C H 0.0197 -0.0532 0.4143 0.150 Uiso 0.676(14) 1 calc PR D -1 H40B H 0.0399 -0.0074 0.3355 0.150 Uiso 0.676(14) 1 calc PR D -1 H40A H -0.0517 -0.0011 0.3947 0.150 Uiso 0.676(14) 1 calc PR D -1 O3S O 0.6732(12) 0.8163(10) 0.2004(10) 0.100 Uiso 0.494(11) 1 d PDU E -1 C1S C 0.5556(19) 0.8773(13) 0.2901(16) 0.100 Uiso 0.494(11) 1 d PDU E -1 C2S C 0.6170(18) 0.8197(14) 0.2702(11) 0.100 Uiso 0.494(11) 1 d PDU E -1 C4S C 0.7513(15) 0.8601(14) 0.1664(14) 0.100 Uiso 0.494(11) 1 d PDU E -1 C5S C 0.8281(18) 0.8540(16) 0.0993(14) 0.100 Uiso 0.494(11) 1 d PDU E -1 F2 F 0.9303(16) 0.5494(12) -0.0095(13) 0.195(8) Uiso 0.67 1 d PU F -1 F3 F 0.9613(18) 0.4934(13) 0.0771(14) 0.218(10) Uiso 0.67 1 d PU F -1 F4 F 0.9443(12) 0.4567(9) 0.0054(10) 0.156(6) Uiso 0.67 1 d PU F -1 B1 B 1.0000 0.5000 0.0000 0.075(5) Uiso 1 2 d SU F -1 N400 N 0.3698(9) 0.4921(7) 0.3097(7) 0.109(4) Uiso 1 1 d U G -1 C401 C 0.3702(8) 0.4788(6) 0.3645(7) 0.074(3) Uiso 1 1 d U G -1 C402 C 0.3691(13) 0.4605(10) 0.4393(10) 0.128(6) Uiso 1 1 d U G -1 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 0.0307(3) 0.0480(3) 0.0533(4) -0.0149(3) -0.0099(2) 0.0109(2) Ag2 0.0404(3) 0.0987(5) 0.0566(4) -0.0485(4) -0.0248(3) 0.0203(3) Ag3 0.0711(4) 0.0425(3) 0.0621(4) -0.0124(3) -0.0310(3) -0.0061(3) N1 0.022(2) 0.047(3) 0.032(3) -0.010(2) -0.007(2) 0.004(2) N1' 0.035(3) 0.046(3) 0.028(3) -0.010(2) -0.007(2) 0.008(2) N1A 0.038(3) 0.078(4) 0.046(3) -0.033(3) -0.010(3) -0.003(3) N1B 0.031(3) 0.078(4) 0.046(3) -0.035(3) -0.016(3) 0.016(3) N1C 0.053(3) 0.041(3) 0.035(3) -0.005(3) -0.016(3) 0.003(2) N1D 0.049(3) 0.043(3) 0.047(4) -0.005(3) -0.015(3) -0.001(3) N12 0.037(3) 0.078(5) 0.054(4) -0.031(4) -0.027(3) 0.011(3) N12' 0.042(3) 0.074(5) 0.038(3) -0.027(3) -0.012(3) 0.013(3) N12A 0.053(4) 0.055(4) 0.069(4) -0.021(3) -0.030(4) 0.002(3) N12B 0.089(6) 0.055(4) 0.049(4) -0.004(3) -0.025(4) -0.015(4) N12C 0.034(3) 0.046(3) 0.045(3) -0.016(3) -0.015(3) 0.008(2) N12D 0.049(4) 0.051(4) 0.070(5) -0.018(4) 0.001(3) -0.009(3) C2 0.028(3) 0.051(4) 0.032(3) -0.016(3) -0.008(3) 0.006(3) C2' 0.035(3) 0.051(4) 0.034(3) -0.015(3) -0.014(3) 0.010(3) C2A 0.039(4) 0.082(4) 0.041(4) -0.032(4) -0.013(3) 0.003(4) C2B 0.027(3) 0.084(4) 0.046(4) -0.039(3) -0.014(3) 0.008(3) C2C 0.048(4) 0.044(4) 0.036(4) -0.002(3) -0.011(3) 0.003(3) C2D 0.052(4) 0.036(3) 0.034(4) -0.003(3) -0.015(3) 0.000(3) C3 0.028(4) 0.098(7) 0.053(5) -0.043(5) -0.012(3) 0.014(4) C3' 0.048(5) 0.101(7) 0.049(5) -0.032(5) -0.025(4) 0.033(5) C3A 0.057(5) 0.086(5) 0.057(5) -0.034(4) -0.029(4) 0.007(5) C3B 0.040(4) 0.084(5) 0.057(5) -0.038(4) -0.023(4) 0.007(4) C3C 0.057(4) 0.041(4) 0.073(6) 0.011(4) -0.007(5) -0.002(3) C3D 0.049(4) 0.041(4) 0.065(5) -0.001(4) -0.009(4) 0.000(3) C4 0.035(4) 0.152(11) 0.063(6) -0.070(7) -0.004(4) 0.007(5) C4' 0.077(7) 0.148(11) 0.070(6) -0.054(7) -0.053(6) 0.054(7) C4A 0.075(7) 0.091(6) 0.064(6) -0.023(5) -0.031(5) 0.013(6) C4B 0.054(5) 0.085(5) 0.073(6) -0.046(5) -0.026(5) 0.010(5) C4C 0.049(5) 0.062(5) 0.149(12) 0.019(7) 0.002(7) 0.003(4) C4D 0.065(5) 0.041(4) 0.094(8) -0.004(5) -0.013(5) 0.003(4) C5 0.042(4) 0.128(9) 0.035(4) -0.039(5) -0.008(3) 0.000(5) C5' 0.085(7) 0.137(10) 0.049(5) -0.051(6) -0.036(5) 0.045(7) C5A 0.076(7) 0.082(6) 0.058(6) -0.014(5) -0.017(5) -0.011(5) C5B 0.047(5) 0.073(5) 0.069(5) -0.035(4) -0.023(4) 0.013(4) C5C 0.054(5) 0.059(5) 0.121(10) 0.015(6) 0.004(6) 0.015(4) C5D 0.049(4) 0.051(4) 0.088(7) -0.006(5) -0.010(5) 0.010(3) C6 0.033(3) 0.068(5) 0.034(4) -0.013(3) -0.010(3) -0.003(3) C6' 0.054(4) 0.062(5) 0.032(4) -0.020(3) -0.014(3) 0.016(4) C6A 0.045(4) 0.079(5) 0.052(5) -0.025(4) -0.008(4) -0.013(4) C6B 0.036(4) 0.080(5) 0.055(4) -0.033(4) -0.018(4) 0.018(4) C6C 0.060(4) 0.050(4) 0.050(5) -0.001(4) -0.014(4) 0.013(3) C6D 0.055(4) 0.044(4) 0.064(6) -0.002(4) -0.013(4) -0.001(3) C7 0.040(4) 0.079(6) 0.035(4) -0.013(4) -0.014(3) -0.002(4) C7' 0.060(5) 0.062(5) 0.029(4) -0.014(3) -0.002(3) 0.010(4) C7A 0.061(6) 0.079(6) 0.065(6) -0.028(5) -0.013(5) -0.018(5) C7B 0.048(5) 0.076(6) 0.055(4) -0.024(4) -0.018(4) 0.017(4) C7C 0.061(5) 0.049(4) 0.044(4) -0.009(4) -0.016(4) 0.013(4) C7D 0.054(5) 0.052(5) 0.083(7) 0.002(5) -0.015(5) -0.001(4) C8 0.048(4) 0.080(6) 0.049(5) -0.012(4) -0.025(4) 0.002(4) C8' 0.064(5) 0.062(5) 0.032(4) -0.019(4) -0.005(4) 0.014(4) C8A 0.048(5) 0.086(7) 0.078(6) -0.037(5) -0.016(5) -0.012(5) C8B 0.054(5) 0.072(6) 0.057(4) -0.019(4) -0.021(4) 0.020(4) C8C 0.055(5) 0.051(4) 0.042(4) -0.012(3) -0.019(4) 0.011(3) C8D 0.058(6) 0.056(5) 0.098(8) -0.002(5) -0.017(5) -0.004(4) C9 0.041(4) 0.071(6) 0.047(4) -0.009(4) -0.022(3) 0.000(4) C9' 0.051(4) 0.062(5) 0.032(4) -0.017(3) -0.001(3) 0.010(4) C9A 0.039(4) 0.072(5) 0.074(5) -0.036(4) -0.014(4) -0.003(4) C9B 0.062(5) 0.074(6) 0.052(4) -0.014(4) -0.021(4) 0.010(5) C9C 0.052(4) 0.043(3) 0.036(4) -0.013(3) -0.023(3) 0.009(3) C9D 0.049(5) 0.060(5) 0.088(7) -0.010(5) -0.012(4) -0.007(4) C10 0.054(5) 0.157(12) 0.077(7) -0.073(8) -0.038(5) 0.036(6) C10' 0.070(5) 0.084(7) 0.037(4) -0.030(4) -0.016(4) 0.018(5) C10A 0.053(5) 0.078(5) 0.060(5) -0.020(4) -0.024(4) -0.003(4) C10B 0.125(10) 0.062(6) 0.063(6) 0.002(5) -0.039(7) -0.003(6) C10C 0.043(4) 0.048(4) 0.036(4) -0.015(3) -0.014(3) 0.001(3) C10D 0.090(9) 0.074(6) 0.119(11) -0.041(7) 0.050(8) -0.031(6) C11 0.063(5) 0.129(10) 0.072(6) -0.067(7) -0.047(5) 0.034(6) C11' 0.062(5) 0.092(7) 0.041(4) -0.031(4) -0.020(4) 0.021(5) C11A 0.056(5) 0.058(5) 0.067(5) -0.015(4) -0.030(5) -0.002(4) C11B 0.144(11) 0.055(5) 0.070(6) -0.007(4) -0.050(7) -0.020(6) C11C 0.032(3) 0.051(4) 0.048(4) -0.020(3) -0.010(3) 0.007(3) C11D 0.085(8) 0.067(6) 0.134(12) -0.048(7) 0.046(7) -0.026(6) C12D 0.084(9) 0.054(6) 0.22(2) -0.035(9) 0.054(9) -0.007(6) C13 0.073(6) 0.097(8) 0.128(10) -0.081(8) -0.066(7) 0.037(6) C13' 0.048(4) 0.088(6) 0.036(4) -0.033(4) -0.010(3) 0.014(4) C13A 0.066(6) 0.051(4) 0.068(6) -0.013(4) -0.030(5) -0.004(4) C13B 0.28(2) 0.076(8) 0.062(7) 0.011(6) -0.070(11) -0.081(11) C13C 0.035(3) 0.047(4) 0.038(4) -0.018(3) -0.012(3) 0.008(3) C13D 0.080(8) 0.056(6) 0.186(16) -0.032(8) 0.048(9) -0.005(5) C14 0.062(5) 0.091(8) 0.115(9) -0.061(7) -0.054(6) 0.013(5) C14' 0.043(4) 0.073(6) 0.040(4) -0.021(4) -0.008(3) 0.015(4) C14A 0.063(5) 0.051(5) 0.079(6) -0.025(4) -0.020(5) -0.006(4) C14B 0.24(2) 0.078(7) 0.072(7) -0.008(5) -0.074(11) -0.049(10) C14C 0.036(3) 0.060(4) 0.034(4) -0.017(3) -0.012(3) 0.016(3) Co1 0.0609(8) 0.1392(15) 0.0402(7) -0.0181(8) -0.0219(6) 0.0149(9) Co2 0.0625(7) 0.0480(6) 0.0401(6) -0.0031(5) -0.0177(5) -0.0151(5) Co3 0.0526(13) 0.0600(14) 0.0443(12) -0.0217(10) -0.0116(10) 0.0067(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 N12C 2.225(6) . y Ag1 N12D 2.286(7) 2_565 y Ag1 N1' 2.365(6) . y Ag1 N1 2.383(5) . y Ag2 N12 2.231(6) 2_565 y Ag2 N12' 2.277(6) . y Ag2 N1A 2.390(7) . y Ag2 N1B 2.397(7) . y Ag3 N12A 2.230(7) 2_565 y Ag3 N12B 2.313(8) . y Ag3 N1C 2.364(7) . y Ag3 N1D 2.402(7) . y N1 C6 1.329(9) . ? N1 C2 1.338(9) . ? N1' C2' 1.345(9) . ? N1' C6' 1.350(9) . ? N1A C6A 1.337(13) . ? N1A C2A 1.348(10) . ? N1B C2B 1.338(10) . ? N1B C6B 1.341(12) . ? N1C C6C 1.335(11) . ? N1C C2C 1.351(10) . ? N1D C2D 1.329(10) . ? N1D C6D 1.330(11) . ? N12 C11 1.298(11) . ? N12 C13 1.327(11) . ? N12 Ag2 2.231(6) 2_565 ? N12' C13' 1.312(11) . ? N12' C11' 1.360(10) . ? N12A C11A 1.332(12) . ? N12A C13A 1.333(12) . ? N12A Ag3 2.230(7) 2_565 ? N12B C13B 1.287(14) . ? N12B C11B 1.306(13) . ? N12C C13C 1.335(9) . ? N12C C11C 1.347(10) . ? N12D C13D 1.283(14) . ? N12D C11D 1.315(13) . ? N12D Ag1 2.286(7) 2_565 ? C2 C3 1.403(10) . ? C2 C2' 1.469(10) . ? C2' C3' 1.385(11) . ? C2A C3A 1.384(12) . ? C2A C2B 1.487(13) . ? C2B C3B 1.406(11) . ? C2C C3C 1.376(12) . ? C2C C2D 1.478(11) . ? C2D C3D 1.396(11) . ? C3 C4 1.361(12) . ? C3' C4' 1.379(13) . ? C3A C4A 1.363(15) . ? C3B C4B 1.354(15) . ? C3C C4C 1.360(14) . ? C3D C4D 1.376(13) . ? C4 C5 1.383(13) . ? C4' C5' 1.367(14) . ? C4A C5A 1.359(16) . ? C4B C5B 1.374(14) . ? C4C C5C 1.389(16) . ? C4D C5D 1.348(14) . ? C5 C6 1.385(11) . ? C5' C6' 1.401(13) . ? C5A C6A 1.404(15) . ? C5B C6B 1.386(13) . ? C5C C6C 1.364(15) . ? C5D C6D 1.416(13) . ? C6 C7 1.445(11) . ? C6' C7' 1.423(11) . ? C6A C7A 1.452(13) . ? C6B C7B 1.462(13) . ? C6C C7C 1.449(12) . ? C6D C7D 1.441(13) . ? C7 C8 1.182(12) . y C7' C8' 1.200(12) . y C7A C8A 1.161(13) . y C7B C8B 1.167(13) . y C7C C8C 1.187(12) . y C7D C8D 1.195(14) . y C8 C9 1.433(12) . ? C8' C9' 1.431(11) . ? C8A C9A 1.438(13) . ? C8B C9B 1.436(13) . ? C8C C9C 1.428(11) . ? C8D C9D 1.420(14) . ? C9 C14 1.367(14) . ? C9 C10 1.375(13) . ? C9' C14' 1.379(12) . ? C9' C10' 1.385(13) . ? C9A C10A 1.383(14) . ? C9A C14A 1.410(15) . ? C9B C14B 1.329(16) . ? C9B C10B 1.383(16) . ? C9C C10C 1.389(11) . ? C9C C14C 1.409(11) . ? C9D C10D 1.330(16) . ? C9D C12D 1.351(16) . ? C10 C11 1.381(13) . ? C10' C11' 1.377(12) . ? C10A C11A 1.372(13) . ? C10B C11B 1.389(15) . ? C10C C11C 1.368(11) . ? C10D C11D 1.374(16) . ? C12D C13D 1.365(17) . ? C13 C14 1.391(13) . ? C13' C14' 1.379(11) . ? C13A C14A 1.335(13) . ? C13B C14B 1.415(17) . ? C13C C14C 1.352(11) . ? C100 B106 1.742(17) . ? C100 B105 1.753(17) . ? C100 B104 1.786(16) . ? C100 C101 1.86(3) . ? C101 B107 1.771(18) . ? C101 B106 1.795(18) . ? C101 B102 1.807(18) . ? C111 C112 1.69(3) . ? C111 B117 1.750(17) . ? C111 B116 1.761(16) . ? C111 B115 1.811(16) . ? C112 B113 1.670(15) . ? C112 B117 1.778(17) . ? C112 B118 1.858(16) . ? B102 B107 1.749(18) . ? B102 B103 1.777(17) . ? B102 B108 1.777(18) . ? B103 B104 1.757(16) . ? B103 B109 1.761(18) . ? B103 B108 1.763(17) . ? B104 B105 1.791(17) . ? B104 B109 1.813(18) . ? B105 B110 1.764(18) . ? B105 B109 1.769(18) . ? B105 B106 1.828(17) . ? B106 B110 1.749(17) . ? B106 B107 1.775(18) . ? B107 B110 1.778(17) . ? B107 B108 1.806(18) . ? B108 B110 1.756(18) . ? B108 B109 1.812(19) . ? B109 B110 1.82(4) . ? B113 B114 1.628(11) . ? B113 B118 1.712(15) . ? B113 B119 1.770(13) . ? B114 B120 1.768(14) . ? B114 B115 1.793(16) . ? B114 B119 1.793(13) . ? B115 B120 1.761(16) . ? B115 B116 1.784(16) . ? B116 B121 1.696(16) . ? B116 B120 1.728(15) . ? B116 B117 1.762(17) . ? B117 B118 1.670(17) . ? B117 B121 1.789(17) . ? B118 B121 1.790(17) . ? B118 B119 1.797(16) . ? B119 B121 1.714(16) . ? B119 B120 1.720(15) . ? B120 B121 1.870(16) . ? C200 C201 1.632(14) . ? C200 B204 1.719(13) . ? C200 B205 1.744(13) . ? C200 B206 1.764(14) . ? C201 B206 1.744(14) . ? C201 B207 1.753(14) . ? C201 B202 1.760(14) . ? C211 C212 1.571(14) . ? C211 B216 1.716(11) . ? C211 B217 1.738(12) . ? C211 B215 1.739(12) . ? C212 B217 1.740(13) . ? C212 B218 1.764(15) . ? C212 B213 1.775(15) . ? B202 B203 1.763(15) . ? B202 B208 1.785(15) . ? B202 B207 1.804(15) . ? B203 B204 1.769(14) . ? B203 B208 1.775(15) . ? B203 B209 1.788(15) . ? B204 B209 1.786(14) . ? B204 B205 1.794(14) . ? B205 B209 1.752(14) . ? B205 B210 1.776(14) . ? B205 B206 1.795(14) . ? B206 B210 1.754(15) . ? B206 B207 1.818(15) . ? B207 B208 1.746(15) . ? B207 B210 1.762(15) . ? B208 B209 1.736(14) . ? B208 B210 1.815(15) . ? B209 B210 1.747(14) . ? B213 B214 1.781(16) . ? B213 B219 1.781(17) . ? B213 B218 1.804(16) . ? B214 B215 1.741(15) . ? B214 B219 1.767(16) . ? B214 B220 1.814(16) . ? B215 B220 1.770(15) . ? B215 B216 1.807(13) . ? B216 B221 1.739(14) . ? B216 B220 1.753(14) . ? B216 B217 1.760(13) . ? B217 B218 1.772(15) . ? B217 B221 1.824(15) . ? B218 B221 1.744(16) . ? B218 B219 1.795(17) . ? B219 B221 1.751(16) . ? B219 B220 1.764(16) . ? B220 B221 1.809(15) . ? C300 C301 1.53(4) . ? C300 B305 1.777(19) . ? C300 B304 1.777(19) . ? C300 B306 1.783(19) . ? C301 B307 1.744(18) . ? C301 B302 1.753(18) . ? C301 B306 1.781(19) . ? C311 C312 1.63(4) . ? C311 B315 1.753(19) . ? C311 B316 1.767(19) . ? C311 B317 1.780(19) . ? C312 B318 1.767(18) . ? C312 B317 1.773(19) . ? C312 B313 1.781(18) . ? B302 B308 1.771(18) . ? B302 B303 1.777(18) . ? B302 B307 1.792(18) . ? B303 B304 1.783(19) . ? B303 B309 1.787(19) . ? B303 B308 1.799(18) . ? B304 B305 1.780(19) . ? B304 B309 1.780(19) . ? B305 B309 1.777(19) . ? B305 B310 1.780(19) . ? B305 B306 1.86(6) . ? B306 B307 1.759(19) . ? B306 B310 1.801(19) . ? B307 B310 1.770(19) . ? B307 B308 1.788(18) . ? B308 B310 1.776(18) . ? B308 B309 1.787(19) . ? B309 B310 1.772(19) . ? B313 B314 1.785(18) . ? B313 B319 1.786(18) . ? B313 B318 1.795(18) . ? B314 B319 1.780(18) . ? B314 B315 1.788(19) . ? B314 B320 1.793(19) . ? B315 B320 1.756(19) . ? B315 B316 1.794(19) . ? B316 B317 1.762(19) . ? B316 B321 1.788(19) . ? B316 B320 2.05(5) . ? B317 B318 1.781(19) . ? B317 B321 1.808(19) . ? B318 B319 1.754(18) . ? B318 B321 1.761(18) . ? B319 B320 1.756(19) . ? B319 B321 1.794(18) . ? B320 B321 1.782(19) . ? N403 C404 1.05(2) . ? C404 C405 1.37(3) . ? O3S C4S 1.419(10) . ? O3S C2S 1.422(10) . ? C1S C2S 1.516(10) . ? C4S C5S 1.524(10) . ? F2 B1 1.46(2) . ? F3 B1 1.46(3) . ? F4 B1 1.231(18) . ? N400 C401 1.080(15) . ? C401 C402 1.47(2) . ? 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 N12C Ag1 N12D 125.3(3) . 2_565 y N12C Ag1 N1' 124.9(2) . . y N12D Ag1 N1' 98.5(3) 2_565 . y N12C Ag1 N1 119.1(2) . . y N12D Ag1 N1 106.3(2) 2_565 . y N1' Ag1 N1 68.10(19) . . y N12 Ag2 N12' 126.4(2) 2_565 . y N12 Ag2 N1A 124.0(2) 2_565 . y N12' Ag2 N1A 98.5(2) . . y N12 Ag2 N1B 111.4(2) 2_565 . y N12' Ag2 N1B 114.0(2) . . y N1A Ag2 N1B 68.5(2) . . y N12A Ag3 N12B 122.5(3) 2_565 . y N12A Ag3 N1C 124.8(3) 2_565 . ? N12B Ag3 N1C 99.9(3) . . y N12A Ag3 N1D 126.8(3) 2_565 . y N12B Ag3 N1D 100.7(3) . . y N1C Ag3 N1D 68.4(2) . . y C6 N1 C2 119.6(6) . . ? C6 N1 Ag1 121.2(5) . . y C2 N1 Ag1 119.1(4) . . y C2' N1' C6' 118.9(6) . . ? C2' N1' Ag1 119.8(5) . . y C6' N1' Ag1 120.2(5) . . y C6A N1A C2A 118.3(8) . . ? C6A N1A Ag2 122.4(5) . . y C2A N1A Ag2 118.9(6) . . y C2B N1B C6B 118.2(7) . . ? C2B N1B Ag2 117.8(6) . . y C6B N1B Ag2 122.7(5) . . y C6C N1C C2C 118.3(7) . . ? C6C N1C Ag3 121.8(6) . . y C2C N1C Ag3 119.7(5) . . y C2D N1D C6D 119.7(7) . . ? C2D N1D Ag3 118.6(5) . . y C6D N1D Ag3 121.6(5) . . y C11 N12 C13 117.2(8) . . ? C11 N12 Ag2 120.5(5) . 2_565 ? C13 N12 Ag2 122.3(6) . 2_565 ? C13' N12' C11' 116.6(7) . . ? C13' N12' Ag2 116.2(5) . . ? C11' N12' Ag2 127.0(6) . . ? C11A N12A C13A 117.6(8) . . ? C11A N12A Ag3 118.6(6) . 2_565 ? C13A N12A Ag3 123.5(6) . 2_565 ? C13B N12B C11B 116.8(9) . . ? C13B N12B Ag3 113.9(7) . . ? C11B N12B Ag3 129.2(7) . . ? C13C N12C C11C 116.4(6) . . ? C13C N12C Ag1 126.1(5) . . ? C11C N12C Ag1 116.7(5) . . ? C13D N12D C11D 115.6(10) . . ? C13D N12D Ag1 119.1(7) . 2_565 ? C11D N12D Ag1 125.1(7) . 2_565 ? N1 C2 C3 121.1(7) . . ? N1 C2 C2' 116.5(6) . . ? C3 C2 C2' 122.3(6) . . ? N1' C2' C3' 121.1(7) . . ? N1' C2' C2 115.7(6) . . ? C3' C2' C2 123.1(7) . . ? N1A C2A C3A 121.4(9) . . ? N1A C2A C2B 115.8(7) . . ? C3A C2A C2B 122.8(8) . . ? N1B C2B C3B 121.2(9) . . ? N1B C2B C2A 116.9(7) . . ? C3B C2B C2A 121.9(8) . . ? N1C C2C C3C 121.4(8) . . ? N1C C2C C2D 115.9(7) . . ? C3C C2C C2D 122.8(7) . . ? N1D C2D C3D 120.6(8) . . ? N1D C2D C2C 117.3(7) . . ? C3D C2D C2C 122.1(7) . . ? C4 C3 C2 118.6(8) . . ? C4' C3' C2' 119.4(8) . . ? C4A C3A C2A 118.7(9) . . ? C4B C3B C2B 118.7(9) . . ? C4C C3C C2C 119.6(9) . . ? C4D C3D C2D 119.2(8) . . ? C3 C4 C5 120.2(8) . . ? C5' C4' C3' 120.5(9) . . ? C5A C4A C3A 122.1(10) . . ? C3B C4B C5B 121.4(9) . . ? C3C C4C C5C 119.4(10) . . ? C5D C4D C3D 121.0(9) . . ? C4 C5 C6 118.0(7) . . ? C4' C5' C6' 117.5(8) . . ? C4A C5A C6A 116.1(11) . . ? C4B C5B C6B 116.6(10) . . ? C6C C5C C4C 118.2(10) . . ? C4D C5D C6D 116.9(9) . . ? N1 C6 C5 122.4(7) . . ? N1 C6 C7 115.7(7) . . ? C5 C6 C7 121.9(7) . . ? N1' C6' C5' 122.5(7) . . ? N1' C6' C7' 117.4(7) . . ? C5' C6' C7' 120.1(8) . . ? N1A C6A C5A 123.4(9) . . ? N1A C6A C7A 117.1(9) . . ? C5A C6A C7A 119.5(10) . . ? N1B C6B C5B 123.8(8) . . ? N1B C6B C7B 114.3(8) . . ? C5B C6B C7B 121.9(9) . . ? N1C C6C C5C 123.1(9) . . ? N1C C6C C7C 117.1(8) . . ? C5C C6C C7C 119.8(9) . . ? N1D C6D C5D 122.6(8) . . ? N1D C6D C7D 115.9(8) . . ? C5D C6D C7D 121.4(9) . . ? C8 C7 C6 176.3(10) . . y C8' C7' C6' 179.0(10) . . y C8A C7A C6A 178.6(12) . . y C8B C7B C6B 174.5(11) . . y C8C C7C C6C 175.0(10) . . y C8D C7D C6D 172.7(11) . . y C7 C8 C9 177.3(10) . . y C7' C8' C9' 175.9(9) . . y C7A C8A C9A 177.4(11) . . y C7B C8B C9B 179.0(13) . . y C7C C8C C9C 173.8(10) . . y C7D C8D C9D 171.9(13) . . y C14 C9 C10 116.7(8) . . ? C14 C9 C8 121.0(8) . . ? C10 C9 C8 122.3(9) . . ? C14' C9' C10' 118.7(7) . . ? C14' C9' C8' 119.3(8) . . ? C10' C9' C8' 122.1(8) . . ? C10A C9A C14A 116.9(8) . . ? C10A C9A C8A 120.6(10) . . ? C14A C9A C8A 122.5(10) . . ? C14B C9B C10B 116.0(10) . . ? C14B C9B C8B 121.8(10) . . ? C10B C9B C8B 122.2(10) . . ? C10C C9C C14C 116.9(7) . . ? C10C C9C C8C 120.0(7) . . ? C14C C9C C8C 123.1(7) . . ? C10D C9D C12D 114.0(10) . . ? C10D C9D C8D 122.1(10) . . ? C12D C9D C8D 123.8(11) . . ? C9 C10 C11 119.5(9) . . ? C11' C10' C9' 118.5(8) . . ? C11A C10A C9A 119.2(9) . . ? C9B C10B C11B 120.0(10) . . ? C11C C10C C9C 119.5(7) . . ? C9D C10D C11D 121.8(11) . . ? N12 C11 C10 124.0(9) . . ? N12' C11' C10' 123.2(9) . . ? N12A C11A C10A 122.9(9) . . ? N12B C11B C10B 123.4(10) . . ? N12C C11C C10C 123.5(7) . . ? N12D C11D C10D 122.7(11) . . ? C9D C12D C13D 121.9(11) . . ? N12 C13 C14 122.7(9) . . ? N12' C13' C14' 124.6(7) . . ? N12A C13A C14A 123.7(10) . . ? N12B C13B C14B 123.6(11) . . ? N12C C13C C14C 124.5(7) . . ? N12D C13D C12D 123.2(11) . . ? C9 C14 C13 119.8(9) . . ? C13' C14' C9' 118.5(8) . . ? C13A C14A C9A 119.6(9) . . ? C9B C14B C13B 120.3(11) . . ? C13C C14C C9C 119.1(7) . . ? B106 C100 B105 63.1(8) . . ? B106 C100 B104 112.7(11) . . ? B105 C100 B104 60.8(7) . . ? B106 C100 C101 59.6(9) . . ? B105 C100 C101 111.9(12) . . ? B104 C100 C101 113.7(13) . . ? B107 C101 B106 59.7(8) . . ? B107 C101 B102 58.5(8) . . ? B106 C101 B102 104.1(12) . . ? B107 C101 C100 103.1(12) . . ? B106 C101 C100 56.9(9) . . ? B102 C101 C100 101.3(15) . . ? C112 C111 B117 62.2(8) . . ? C112 C111 B116 107.8(11) . . ? B117 C111 B116 60.3(7) . . ? C112 C111 B115 105.4(13) . . ? B117 C111 B115 108.8(11) . . ? B116 C111 B115 59.9(7) . . ? B113 C112 C111 107.9(12) . . ? B113 C112 B117 100.8(10) . . ? C111 C112 B117 60.6(8) . . ? B113 C112 B118 57.8(7) . . ? C111 C112 B118 105.7(11) . . ? B117 C112 B118 54.6(7) . . ? B107 B102 B103 108.2(12) . . ? B107 B102 B108 61.6(8) . . ? B103 B102 B108 59.5(8) . . ? B107 B102 C101 59.7(8) . . ? B103 B102 C101 109.4(16) . . ? B108 B102 C101 110.4(12) . . ? B104 B103 B109 62.0(8) . . ? B104 B103 B108 112.3(11) . . ? B109 B103 B108 61.9(8) . . ? B104 B103 B102 112.7(13) . . ? B109 B103 B102 111.5(13) . . ? B108 B103 B102 60.3(8) . . ? B103 B104 C100 102.7(11) . . ? B103 B104 B105 103.8(10) . . ? C100 B104 B105 58.7(7) . . ? B103 B104 B109 59.1(7) . . ? C100 B104 B109 105.1(12) . . ? B105 B104 B109 58.8(7) . . ? C100 B105 B110 104.6(12) . . ? C100 B105 B109 108.5(13) . . ? B110 B105 B109 62.2(15) . . ? C100 B105 B104 60.5(7) . . ? B110 B105 B104 109.6(14) . . ? B109 B105 B104 61.2(8) . . ? C100 B105 B106 58.2(8) . . ? B110 B105 B106 58.2(8) . . ? B109 B105 B106 109.3(15) . . ? B104 B105 B106 108.5(11) . . ? C100 B106 B110 105.7(12) . . ? C100 B106 B107 108.0(13) . . ? B110 B106 B107 60.6(8) . . ? C100 B106 C101 63.5(12) . . ? B110 B106 C101 109.5(12) . . ? B107 B106 C101 59.5(8) . . ? C100 B106 B105 58.7(7) . . ? B110 B106 B105 59.0(8) . . ? B107 B106 B105 108.2(12) . . ? C101 B106 B105 111.6(14) . . ? B102 B107 C101 61.7(8) . . ? B102 B107 B106 107.4(13) . . ? C101 B107 B106 60.8(8) . . ? B102 B107 B110 106.3(12) . . ? C101 B107 B110 109.2(13) . . ? B106 B107 B110 59.0(8) . . ? B102 B107 B108 60.0(8) . . ? C101 B107 B108 110.7(13) . . ? B106 B107 B108 106.4(12) . . ? B110 B107 B108 58.7(8) . . ? B110 B108 B103 105.6(14) . . ? B110 B108 B102 106.1(12) . . ? B103 B108 B102 60.2(8) . . ? B110 B108 B107 59.9(8) . . ? B103 B108 B107 106.2(12) . . ? B102 B108 B107 58.4(8) . . ? B110 B108 B109 61.5(14) . . ? B103 B108 B109 59.0(8) . . ? B102 B108 B109 109.2(13) . . ? B107 B108 B109 110.3(15) . . ? B103 B109 B105 104.6(13) . . ? B103 B109 B108 59.1(8) . . ? B105 B109 B108 105.8(18) . . ? B103 B109 B104 58.9(7) . . ? B105 B109 B104 60.0(8) . . ? B108 B109 B104 107.5(12) . . ? B103 B109 B110 102.8(13) . . ? B105 B109 B110 58.8(11) . . ? B108 B109 B110 57.7(10) . . ? B104 B109 B110 106.1(13) . . ? B106 B110 B108 109.8(12) . . ? B106 B110 B105 62.7(8) . . ? B108 B110 B105 108.5(15) . . ? B106 B110 B107 60.4(8) . . ? B108 B110 B107 61.5(8) . . ? B105 B110 B107 111.0(12) . . ? B106 B110 B109 110.4(12) . . ? B108 B110 B109 60.8(9) . . ? B105 B110 B109 59.0(9) . . ? B107 B110 B109 111.0(12) . . ? B114 B113 C112 114.5(9) . . ? B114 B113 B118 116.9(8) . . ? C112 B113 B118 66.6(7) . . ? B114 B113 B119 63.6(6) . . ? C112 B113 B119 115.9(9) . . ? B118 B113 B119 62.1(6) . . ? B113 B114 B120 106.3(7) . . ? B113 B114 B115 104.5(9) . . ? B120 B114 B115 59.3(6) . . ? B113 B114 B119 62.1(6) . . ? B120 B114 B119 57.7(6) . . ? B115 B114 B119 105.4(8) . . ? B120 B115 B116 58.3(7) . . ? B120 B115 B114 59.7(7) . . ? B116 B115 B114 103.1(9) . . ? B120 B115 C111 107.8(10) . . ? B116 B115 C111 58.7(7) . . ? B114 B115 C111 106.4(12) . . ? B121 B116 B120 66.2(7) . . ? B121 B116 C111 113.4(10) . . ? B120 B116 C111 111.6(10) . . ? B121 B116 B117 62.3(7) . . ? B120 B116 B117 113.2(10) . . ? C111 B116 B117 59.5(7) . . ? B121 B116 B115 115.1(10) . . ? B120 B116 B115 60.2(7) . . ? C111 B116 B115 61.4(7) . . ? B117 B116 B115 109.5(11) . . ? B118 B117 C111 111.6(13) . . ? B118 B117 B116 106.1(11) . . ? C111 B117 B116 60.2(7) . . ? B118 B117 C112 65.1(8) . . ? C111 B117 C112 57.2(10) . . ? B116 B117 C112 103.9(12) . . ? B118 B117 B121 62.2(8) . . ? C111 B117 B121 109.5(11) . . ? B116 B117 B121 57.0(7) . . ? C112 B117 B121 112.3(11) . . ? B117 B118 B113 103.6(11) . . ? B117 B118 B121 62.1(8) . . ? B113 B118 B121 104.7(10) . . ? B117 B118 B119 106.8(11) . . ? B113 B118 B119 60.5(7) . . ? B121 B118 B119 57.1(7) . . ? B117 B118 C112 60.2(8) . . ? B113 B118 C112 55.6(7) . . ? B121 B118 C112 108.6(11) . . ? B119 B118 C112 105.9(10) . . ? B121 B119 B120 66.0(7) . . ? B121 B119 B113 105.5(9) . . ? B120 B119 B113 102.3(9) . . ? B121 B119 B114 112.6(9) . . ? B120 B119 B114 60.4(6) . . ? B113 B119 B114 54.4(5) . . ? B121 B119 B118 61.2(7) . . ? B120 B119 B118 111.5(10) . . ? B113 B119 B118 57.4(6) . . ? B114 B119 B118 104.9(9) . . ? B119 B120 B116 101.9(9) . . ? B119 B120 B115 110.1(10) . . ? B116 B120 B115 61.5(7) . . ? B119 B120 B114 61.9(6) . . ? B116 B120 B114 106.5(9) . . ? B115 B120 B114 61.1(7) . . ? B119 B120 B121 56.9(7) . . ? B116 B120 B121 56.1(7) . . ? B115 B120 B121 107.9(10) . . ? B114 B120 B121 106.7(9) . . ? B116 B121 B119 103.5(10) . . ? B116 B121 B117 60.7(7) . . ? B119 B121 B117 105.2(10) . . ? B116 B121 B118 103.8(10) . . ? B119 B121 B118 61.7(7) . . ? B117 B121 B118 55.6(7) . . ? B116 B121 B120 57.7(7) . . ? B119 B121 B120 57.1(7) . . ? B117 B121 B120 105.6(10) . . ? B118 B121 B120 105.2(10) . . ? C201 C200 B204 109.0(8) . . ? C201 C200 B205 110.0(7) . . ? B204 C200 B205 62.4(6) . . ? C201 C200 B206 61.6(6) . . ? B204 C200 B206 112.7(8) . . ? B205 C200 B206 61.5(6) . . ? C200 C201 B206 62.9(6) . . ? C200 C201 B207 112.0(8) . . ? B206 C201 B207 62.6(6) . . ? C200 C201 B202 111.9(8) . . ? B206 C201 B202 114.7(8) . . ? B207 C201 B202 61.8(6) . . ? C212 C211 B216 112.2(7) . . ? C212 C211 B217 63.2(6) . . ? B216 C211 B217 61.3(5) . . ? C212 C211 B215 114.9(7) . . ? B216 C211 B215 63.0(5) . . ? B217 C211 B215 115.7(7) . . ? C211 C212 B217 63.1(6) . . ? C211 C212 B218 108.1(8) . . ? B217 C212 B218 60.7(6) . . ? C211 C212 B213 106.4(9) . . ? B217 C212 B213 111.8(8) . . ? B218 C212 B213 61.3(7) . . ? C201 B202 B203 104.1(10) . . ? C201 B202 B208 103.2(8) . . ? B203 B202 B208 60.0(6) . . ? C201 B202 B207 58.9(6) . . ? B203 B202 B207 106.7(9) . . ? B208 B202 B207 58.2(6) . . ? B202 B203 B204 107.6(10) . . ? B202 B203 B208 60.6(7) . . ? B204 B203 B208 107.4(9) . . ? B202 B203 B209 106.6(9) . . ? B204 B203 B209 60.3(6) . . ? B208 B203 B209 58.3(6) . . ? C200 B204 B203 107.2(9) . . ? C200 B204 B209 104.2(8) . . ? B203 B204 B209 60.4(6) . . ? C200 B204 B205 59.5(6) . . ? B203 B204 B205 109.0(8) . . ? B209 B204 B205 58.6(6) . . ? C200 B205 B209 104.6(8) . . ? C200 B205 B210 104.9(8) . . ? B209 B205 B210 59.4(6) . . ? C200 B205 B204 58.1(5) . . ? B209 B205 B204 60.5(6) . . ? B210 B205 B204 107.9(8) . . ? C200 B205 B206 59.8(6) . . ? B209 B205 B206 106.4(8) . . ? B210 B205 B206 58.8(6) . . ? B204 B205 B206 107.8(8) . . ? C201 B206 B210 104.5(9) . . ? C201 B206 C200 55.5(6) . . ? B210 B206 C200 105.0(9) . . ? C201 B206 B205 102.8(9) . . ? B210 B206 B205 60.0(6) . . ? C200 B206 B205 58.7(6) . . ? C201 B206 B207 58.9(6) . . ? B210 B206 B207 59.1(6) . . ? C200 B206 B207 103.2(9) . . ? B205 B206 B207 106.0(9) . . ? B208 B207 C201 105.2(9) . . ? B208 B207 B210 62.3(7) . . ? C201 B207 B210 103.8(9) . . ? B208 B207 B202 60.4(6) . . ? C201 B207 B202 59.3(6) . . ? B210 B207 B202 110.0(9) . . ? B208 B207 B206 109.1(9) . . ? C201 B207 B206 58.4(6) . . ? B210 B207 B206 58.7(6) . . ? B202 B207 B206 109.1(9) . . ? B209 B208 B207 106.7(9) . . ? B209 B208 B203 61.2(6) . . ? B207 B208 B203 108.8(9) . . ? B209 B208 B202 107.9(9) . . ? B207 B208 B202 61.4(6) . . ? B203 B208 B202 59.4(6) . . ? B209 B208 B210 58.9(6) . . ? B207 B208 B210 59.3(6) . . ? B203 B208 B210 108.6(9) . . ? B202 B208 B210 108.5(9) . . ? B208 B209 B210 62.8(6) . . ? B208 B209 B205 111.7(9) . . ? B210 B209 B205 61.0(6) . . ? B208 B209 B204 108.5(9) . . ? B210 B209 B204 109.5(8) . . ? B205 B209 B204 60.9(6) . . ? B208 B209 B203 60.5(6) . . ? B210 B209 B203 111.1(9) . . ? B205 B209 B203 110.1(9) . . ? B204 B209 B203 59.3(6) . . ? B209 B210 B206 108.5(9) . . ? B209 B210 B207 105.5(9) . . ? B206 B210 B207 62.3(6) . . ? B209 B210 B205 59.6(6) . . ? B206 B210 B205 61.1(6) . . ? B207 B210 B205 109.3(9) . . ? B209 B210 B208 58.3(6) . . ? B206 B210 B208 108.9(9) . . ? B207 B210 B208 58.4(6) . . ? B205 B210 B208 107.0(8) . . ? C212 B213 B214 107.7(11) . . ? C212 B213 B219 105.8(10) . . ? B214 B213 B219 59.5(7) . . ? C212 B213 B218 59.0(7) . . ? B214 B213 B218 108.8(10) . . ? B219 B213 B218 60.1(7) . . ? B215 B214 B219 105.9(10) . . ? B215 B214 B213 105.7(11) . . ? B219 B214 B213 60.3(7) . . ? B215 B214 B220 59.7(7) . . ? B219 B214 B220 59.0(7) . . ? B213 B214 B220 107.1(10) . . ? C211 B215 B214 105.3(9) . . ? C211 B215 B220 104.8(8) . . ? B214 B215 B220 62.2(7) . . ? C211 B215 B216 57.9(5) . . ? B214 B215 B216 107.6(8) . . ? B220 B215 B216 58.7(6) . . ? C211 B216 B221 106.9(8) . . ? C211 B216 B220 106.6(7) . . ? B221 B216 B220 62.4(6) . . ? C211 B216 B217 60.0(5) . . ? B221 B216 B217 62.8(6) . . ? B220 B216 B217 114.3(8) . . ? C211 B216 B215 59.1(5) . . ? B221 B216 B215 109.5(8) . . ? B220 B216 B215 59.6(6) . . ? B217 B216 B215 111.2(8) . . ? C211 B217 C212 53.7(6) . . ? C211 B217 B216 58.8(5) . . ? C212 B217 B216 102.5(8) . . ? C211 B217 B218 100.7(8) . . ? C212 B217 B218 60.3(6) . . ? B216 B217 B218 103.4(8) . . ? C211 B217 B221 102.3(7) . . ? C212 B217 B221 104.8(8) . . ? B216 B217 B221 58.0(6) . . ? B218 B217 B221 58.0(6) . . ? B221 B218 C212 107.2(10) . . ? B221 B218 B217 62.5(7) . . ? C212 B218 B217 59.0(6) . . ? B221 B218 B219 59.3(7) . . ? C212 B218 B219 105.6(10) . . ? B217 B218 B219 109.3(10) . . ? B221 B218 B213 107.8(10) . . ? C212 B218 B213 59.6(7) . . ? B217 B218 B213 108.9(10) . . ? B219 B218 B213 59.3(7) . . ? B221 B219 B220 61.9(7) . . ? B221 B219 B214 111.8(11) . . ? B220 B219 B214 61.8(7) . . ? B221 B219 B213 108.6(11) . . ? B220 B219 B213 109.3(11) . . ? B214 B219 B213 60.3(7) . . ? B221 B219 B218 58.9(7) . . ? B220 B219 B218 108.9(10) . . ? B214 B219 B218 109.8(11) . . ? B213 B219 B218 60.6(7) . . ? B216 B220 B219 104.0(9) . . ? B216 B220 B215 61.7(6) . . ? B219 B220 B215 104.8(9) . . ? B216 B220 B221 58.4(6) . . ? B219 B220 B221 58.7(7) . . ? B215 B220 B221 108.0(9) . . ? B216 B220 B214 106.7(9) . . ? B219 B220 B214 59.2(7) . . ? B215 B220 B214 58.1(6) . . ? B221 B220 B214 107.0(9) . . ? B216 B221 B218 105.5(9) . . ? B216 B221 B219 105.2(10) . . ? B218 B221 B219 61.8(7) . . ? B216 B221 B220 59.2(6) . . ? B218 B221 B220 109.2(10) . . ? B219 B221 B220 59.4(7) . . ? B216 B221 B217 59.2(6) . . ? B218 B221 B217 59.5(7) . . ? B219 B221 B217 108.9(10) . . ? B220 B221 B217 108.7(9) . . ? C301 C300 B305 115(2) . . ? C301 C300 B304 116(2) . . ? B305 C300 B304 60.1(9) . . ? C301 C300 B306 64.5(12) . . ? B305 C300 B306 63(2) . . ? B304 C300 B306 115(2) . . ? C300 C301 B307 109.0(16) . . ? C300 C301 B302 106(2) . . ? B307 C301 B302 61.7(8) . . ? C300 C301 B306 64.6(12) . . ? B307 C301 B306 59.9(8) . . ? B302 C301 B306 111.4(14) . . ? C312 C311 B315 103(2) . . ? C312 C311 B316 110.0(16) . . ? B315 C311 B316 61.3(9) . . ? C312 C311 B317 62.4(12) . . ? B315 C311 B317 105.6(15) . . ? B316 C311 B317 59.6(8) . . ? C311 C312 B318 111.0(15) . . ? C311 C312 B317 62.8(11) . . ? B318 C312 B317 60.4(8) . . ? C311 C312 B313 115(2) . . ? B318 C312 B313 60.8(8) . . ? B317 C312 B313 113.2(13) . . ? C301 B302 B308 107.3(13) . . ? C301 B302 B303 109.6(18) . . ? B308 B302 B303 60.9(8) . . ? C301 B302 B307 58.9(8) . . ? B308 B302 B307 60.2(8) . . ? B303 B302 B307 109.8(12) . . ? B302 B303 B304 104.6(19) . . ? B302 B303 B309 105.9(12) . . ? B304 B303 B309 59.8(8) . . ? B302 B303 B308 59.4(8) . . ? B304 B303 B308 106.8(13) . . ? B309 B303 B308 59.8(8) . . ? C300 B304 B305 59.9(9) . . ? C300 B304 B309 103.9(15) . . ? B305 B304 B309 59.9(9) . . ? C300 B304 B303 103(2) . . ? B305 B304 B303 108.8(14) . . ? B309 B304 B303 60.2(9) . . ? C300 B305 B309 104.0(16) . . ? C300 B305 B310 102(2) . . ? B309 B305 B310 59.8(9) . . ? C300 B305 B304 60.0(9) . . ? B309 B305 B304 60.1(9) . . ? B310 B305 B304 107.8(14) . . ? C300 B305 B306 58.7(12) . . ? B309 B305 B306 109.0(15) . . ? B310 B305 B306 59.3(12) . . ? B304 B305 B306 110.9(17) . . ? B307 B306 C301 59.0(8) . . ? B307 B306 C300 97.8(17) . . ? C301 B306 C300 50.9(15) . . ? B307 B306 B310 59.6(9) . . ? C301 B306 B310 103.7(14) . . ? C300 B306 B310 101(2) . . ? B307 B306 B305 104.4(15) . . ? C301 B306 B305 100.4(18) . . ? C300 B306 B305 58.4(13) . . ? B310 B306 B305 58.2(13) . . ? C301 B307 B306 61.1(9) . . ? C301 B307 B310 106.6(15) . . ? B306 B307 B310 61.4(9) . . ? C301 B307 B308 107.0(13) . . ? B306 B307 B308 111.4(14) . . ? B310 B307 B308 59.9(8) . . ? C301 B307 B302 59.4(8) . . ? B306 B307 B302 110.5(14) . . ? B310 B307 B302 106.5(12) . . ? B308 B307 B302 59.3(8) . . ? B302 B308 B310 107.2(13) . . ? B302 B308 B309 106.2(13) . . ? B310 B308 B309 59.7(8) . . ? B302 B308 B307 60.5(8) . . ? B310 B308 B307 59.6(8) . . ? B309 B308 B307 107.2(13) . . ? B302 B308 B303 59.7(8) . . ? B310 B308 B303 108.3(13) . . ? B309 B308 B303 59.8(8) . . ? B307 B308 B303 109.1(13) . . ? B310 B309 B305 60.2(9) . . ? B310 B309 B304 108.1(14) . . ? B305 B309 B304 60.0(9) . . ? B310 B309 B308 59.9(8) . . ? B305 B309 B308 107.8(14) . . ? B304 B309 B308 107.5(14) . . ? B310 B309 B303 109.0(13) . . ? B305 B309 B303 108.7(14) . . ? B304 B309 B303 60.0(9) . . ? B308 B309 B303 60.4(8) . . ? B307 B310 B309 108.6(13) . . ? B307 B310 B308 60.5(8) . . ? B309 B310 B308 60.5(8) . . ? B307 B310 B305 107.2(18) . . ? B309 B310 B305 60.0(8) . . ? B308 B310 B305 108.1(13) . . ? B307 B310 B306 59.0(8) . . ? B309 B310 B306 111.8(19) . . ? B308 B310 B306 110.0(13) . . ? B305 B310 B306 62(2) . . ? C312 B313 B314 105.2(18) . . ? C312 B313 B319 104.9(12) . . ? B314 B313 B319 59.8(8) . . ? C312 B313 B318 59.2(8) . . ? B314 B313 B318 106.6(12) . . ? B319 B313 B318 58.7(8) . . ? B319 B314 B313 60.1(8) . . ? B319 B314 B315 101.5(13) . . ? B313 B314 B315 102.9(18) . . ? B319 B314 B320 58.9(8) . . ? B313 B314 B320 108.4(13) . . ? B315 B314 B320 58.7(8) . . ? C311 B315 B320 116.9(18) . . ? C311 B315 B314 113(2) . . ? B320 B315 B314 60.8(8) . . ? C311 B315 B316 59.8(8) . . ? B320 B315 B316 70.6(18) . . ? B314 B315 B316 118.9(18) . . ? B317 B316 C311 60.6(9) . . ? B317 B316 B321 61.2(9) . . ? C311 B316 B321 105.1(15) . . ? B317 B316 B315 104.6(15) . . ? C311 B316 B315 59.0(8) . . ? B321 B316 B315 97.0(18) . . ? B317 B316 B320 104.9(13) . . ? C311 B316 B320 102.9(14) . . ? B321 B316 B320 54.8(11) . . ? B315 B316 B320 53.9(11) . . ? B316 B317 C312 104.1(17) . . ? B316 B317 C311 59.9(9) . . ? C312 B317 C311 54.8(16) . . ? B316 B317 B318 108.3(14) . . ? C312 B317 B318 59.6(8) . . ? C311 B317 B318 103.9(17) . . ? B316 B317 B321 60.1(9) . . ? C312 B317 B321 103.1(14) . . ? C311 B317 B321 103.8(15) . . ? B318 B317 B321 58.8(8) . . ? B319 B318 B321 61.4(8) . . ? B319 B318 C312 106.8(13) . . ? B321 B318 C312 105.3(14) . . ? B319 B318 B317 112.9(13) . . ? B321 B318 B317 61.4(8) . . ? C312 B318 B317 60.0(8) . . ? B319 B318 B313 60.4(8) . . ? B321 B318 B313 109.3(12) . . ? C312 B318 B313 60.0(8) . . ? B317 B318 B313 112.1(13) . . ? B318 B319 B320 109.4(13) . . ? B318 B319 B314 108.6(13) . . ? B320 B319 B314 60.9(8) . . ? B318 B319 B313 60.9(8) . . ? B320 B319 B313 110.1(13) . . ? B314 B319 B313 60.1(8) . . ? B318 B319 B321 59.5(8) . . ? B320 B319 B321 60.3(8) . . ? B314 B319 B321 107.7(13) . . ? B313 B319 B321 108.2(12) . . ? B319 B320 B315 103.7(14) . . ? B319 B320 B321 60.9(8) . . ? B315 B320 B321 98.6(19) . . ? B319 B320 B314 60.2(8) . . ? B315 B320 B314 60.5(9) . . ? B321 B320 B314 107.6(13) . . ? B319 B320 B316 104.5(13) . . ? B315 B320 B316 55.6(11) . . ? B321 B320 B316 55.1(11) . . ? B314 B320 B316 106.6(14) . . ? B318 B321 B320 107.9(12) . . ? B318 B321 B316 108.0(13) . . ? B320 B321 B316 70.1(18) . . ? B318 B321 B319 59.1(8) . . ? B320 B321 B319 58.8(8) . . ? B316 B321 B319 114.7(16) . . ? B318 B321 B317 59.9(8) . . ? B320 B321 B317 115.1(17) . . ? B316 B321 B317 58.7(8) . . ? B319 B321 B317 109.8(12) . . ? N403 C404 C405 167(3) . . ? C4S O3S C2S 118(2) . . ? O3S C2S C1S 127(2) . . ? O3S C4S C5S 125(2) . . ? F4 B1 F3 89.3(12) . . ? F4 B1 F2 84.8(12) . . ? F3 B1 F2 87.6(13) . . ? N400 C401 C402 179.0(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 2.356 _refine_diff_density_min -1.255 _refine_diff_density_rms 0.160 #===END data_Compound_5(SSB0347) _database_code_CSD 201519 _refine_special_details ; There is some sort of minor disorder affecting C7 and C8 which affects the length of the triple bond. The disorder has not been modelled as there is no obvious solution. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl silver cobaltocarborate ; _chemical_name_common ; bis(6,6'-ethynyl-4-pyridine)2,2'-bipyridyl silver cobaltocarborate ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H42 Ag B18 Co N6' _chemical_formula_weight 872.10 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' B B 0.0013 0.0007 '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' Co Co 0.3494 0.9721 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1082(5) _cell_length_b 38.364(3) _cell_length_c 14.9966(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.861(2) _cell_angle_gamma 90.00 _cell_volume 4016.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16314 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 29.51 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.005 _exptl_crystal_size_min 0.002 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6900 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% 15 _diffrn_reflns_number 16880 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0541 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 46 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 29.51 _reflns_number_total 10585 _reflns_number_gt 9236 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'OLEX (Oleg V. Dolomanov, 2001)' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2001)' _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^)+(0.0511P)^2^+5.5212P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10585 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 0.51794(3) 0.089626(5) 0.800059(14) 0.02358(7) Uani 1 1 d . . . N1 N 0.4404(3) 0.13837(5) 0.71610(14) 0.0189(4) Uani 1 1 d . . . N1' N 0.1807(3) 0.08940(6) 0.73869(14) 0.0194(4) Uani 1 1 d . . . N12 N 1.4528(4) 0.13430(7) 0.97792(18) 0.0316(5) Uani 1 1 d . . . N12' N 0.3352(3) -0.05434(6) 1.09397(15) 0.0219(4) Uani 1 1 d . . . C2 C 0.2612(4) 0.14173(6) 0.66707(16) 0.0188(5) Uani 1 1 d . . . C2' C 0.1267(4) 0.11217(6) 0.67078(16) 0.0176(5) Uani 1 1 d . . . C3 C 0.2031(4) 0.17186(7) 0.61689(18) 0.0231(5) Uani 1 1 d . . . H3A H 0.0768 0.1737 0.5826 0.028 Uiso 1 1 calc R . . C3' C -0.0460(4) 0.10888(7) 0.60861(17) 0.0230(5) Uani 1 1 d . . . H3'A H -0.0818 0.1256 0.5617 0.028 Uiso 1 1 calc R . . C4 C 0.3323(5) 0.19889(7) 0.61796(19) 0.0272(6) Uani 1 1 d . . . H4A H 0.2957 0.2194 0.5835 0.033 Uiso 1 1 calc R . . C4' C -0.1639(4) 0.08071(8) 0.61707(18) 0.0260(6) Uani 1 1 d . . . H4'A H -0.2813 0.0778 0.5755 0.031 Uiso 1 1 calc R . . C5 C 0.5151(4) 0.19604(7) 0.66936(19) 0.0262(6) Uani 1 1 d . . . H5A H 0.6044 0.2146 0.6715 0.031 Uiso 1 1 calc R . . C5' C -0.1090(4) 0.05693(7) 0.68666(18) 0.0244(5) Uani 1 1 d . . . H5'A H -0.1872 0.0374 0.6935 0.029 Uiso 1 1 calc R . . C6 C 0.5652(4) 0.16522(7) 0.71808(17) 0.0210(5) Uani 1 1 d . . . C6' C 0.0646(4) 0.06241(7) 0.74666(17) 0.0209(5) Uani 1 1 d . . . C7 C 0.7641(4) 0.16019(6) 0.78007(18) 0.0163(5) Uani 1 1 d . . . C7' C 0.1261(4) 0.03865(7) 0.82099(19) 0.0235(5) Uani 1 1 d . . . C8 C 0.8937(7) 0.15736(7) 0.8195(2) 0.0385(9) Uani 1 1 d . . . C8' C 0.1678(4) 0.01858(7) 0.88222(18) 0.0228(5) Uani 1 1 d . . . C9 C 1.0889(4) 0.15075(7) 0.87733(19) 0.0255(5) Uani 1 1 d . . . C9' C 0.2215(4) -0.00622(7) 0.95420(17) 0.0205(5) Uani 1 1 d . . . C10 C 1.1224(4) 0.11942(8) 0.9257(2) 0.0281(6) Uani 1 1 d . . . H10A H 1.0215 0.1032 0.9258 0.034 Uiso 1 1 calc R . . C10' C 0.2721(4) 0.00456(7) 1.04467(19) 0.0233(5) Uani 1 1 d . . . H10B H 0.2680 0.0285 1.0599 0.028 Uiso 1 1 calc R . . C11 C 1.3048(5) 0.11249(8) 0.9734(2) 0.0301(6) Uani 1 1 d . . . H11A H 1.3261 0.0909 1.0049 0.036 Uiso 1 1 calc R . . C11' C 0.3281(4) -0.02016(7) 1.11168(18) 0.0221(5) Uani 1 1 d . . . H11B H 0.3632 -0.0126 1.1729 0.026 Uiso 1 1 calc R . . C13 C 1.4172(5) 0.16442(8) 0.9340(2) 0.0317(6) Uani 1 1 d . . . H13A H 1.5199 0.1805 0.9380 0.038 Uiso 1 1 calc R . . C13' C 0.2815(4) -0.06485(7) 1.00716(18) 0.0231(5) Uani 1 1 d . . . H13B H 0.2831 -0.0891 0.9942 0.028 Uiso 1 1 calc R . . C14 C 1.2429(5) 0.17403(8) 0.8831(2) 0.0290(6) Uani 1 1 d . . . H14A H 1.2273 0.1959 0.8528 0.035 Uiso 1 1 calc R . . C14' C 0.2238(4) -0.04182(7) 0.93595(18) 0.0246(5) Uani 1 1 d . . . H14B H 0.1865 -0.0502 0.8756 0.029 Uiso 1 1 calc R . . N38 N 0.4635(4) 0.03909(7) 0.67398(19) 0.0319(5) Uani 1 1 d . . . C39 C 0.3529(4) 0.01997(7) 0.63688(19) 0.0242(5) Uani 1 1 d . . . C40 C 0.2093(5) -0.00439(9) 0.5919(3) 0.0392(8) Uani 1 1 d . . . H40A H 0.2459 -0.0282 0.6120 0.112(10) Uiso 1 1 calc R . . H40B H 0.2004 -0.0028 0.5260 0.112(10) Uiso 1 1 calc R . . H40C H 0.0849 0.0013 0.6073 0.112(10) Uiso 1 1 calc R . . Co15 Co 0.15784(5) 0.142124(8) 0.26641(2) 0.01517(8) Uani 1 1 d . . . C16 C 0.3971(4) 0.11114(6) 0.27802(16) 0.0181(4) Uani 1 1 d . . . C17 C 0.3645(4) 0.12767(6) 0.37306(16) 0.0171(4) Uani 1 1 d . . . C27 C 0.2714(4) 0.18803(6) 0.23278(17) 0.0194(5) Uani 1 1 d . . . C28 C 0.1590(4) 0.16648(7) 0.14573(16) 0.0192(5) Uani 1 1 d . . . B18 B 0.1372(4) 0.12061(7) 0.39076(18) 0.0184(5) Uani 1 1 d . . . B19 B 0.0210(4) 0.09530(8) 0.2937(2) 0.0204(5) Uani 1 1 d . . . B20 B 0.1950(4) 0.09127(7) 0.22112(19) 0.0197(5) Uani 1 1 d . . . B21 B 0.3966(5) 0.06692(8) 0.2807(2) 0.0220(6) Uani 1 1 d . . . B22 B 0.5077(5) 0.09090(8) 0.3771(2) 0.0212(5) Uani 1 1 d . . . B23 B 0.3392(4) 0.09618(8) 0.44873(19) 0.0203(5) Uani 1 1 d . . . B24 B 0.1252(5) 0.07452(8) 0.3989(2) 0.0220(6) Uani 1 1 d . . . B25 B 0.1609(5) 0.05596(8) 0.2936(2) 0.0221(6) Uani 1 1 d . . . B26 B 0.3503(5) 0.05629(8) 0.3901(2) 0.0224(6) Uani 1 1 d . . . B29 B -0.0654(5) 0.15441(8) 0.1589(2) 0.0230(6) Uani 1 1 d . . . B30 B -0.0917(4) 0.17224(8) 0.2669(2) 0.0226(6) Uani 1 1 d . . . B31 B 0.1338(5) 0.19295(7) 0.31362(19) 0.0215(6) Uani 1 1 d . . . B32 B 0.1723(5) 0.22791(8) 0.2400(2) 0.0242(6) Uani 1 1 d . . . B33 B 0.1930(5) 0.21059(8) 0.1330(2) 0.0229(6) Uani 1 1 d . . . B34 B -0.0258(5) 0.19016(9) 0.0865(2) 0.0247(6) Uani 1 1 d . . . B35 B -0.1845(5) 0.19509(9) 0.1637(2) 0.0264(6) Uani 1 1 d . . . B36 B -0.0612(5) 0.21880(9) 0.2591(2) 0.0278(7) Uani 1 1 d . . . B37 B -0.0257(5) 0.22957(9) 0.1484(2) 0.0266(6) Uani 1 1 d . . . H16 H 0.493(6) 0.1223(10) 0.251(3) 0.036(10) Uiso 1 1 d . . . H17 H 0.446(4) 0.1473(8) 0.394(2) 0.012(7) Uiso 1 1 d . . . H18 H 0.079(5) 0.1373(9) 0.437(2) 0.026(9) Uiso 1 1 d . . . H19 H -0.137(6) 0.0930(9) 0.271(3) 0.035(10) Uiso 1 1 d . . . H20 H 0.166(5) 0.0887(8) 0.149(2) 0.023(8) Uiso 1 1 d . . . H21 H 0.489(5) 0.0538(9) 0.246(3) 0.031(9) Uiso 1 1 d . . . H22 H 0.657(5) 0.0932(8) 0.397(2) 0.023(8) Uiso 1 1 d . . . H23 H 0.377(6) 0.1004(11) 0.521(3) 0.046(11) Uiso 1 1 d . . . H24 H 0.050(5) 0.0633(9) 0.442(3) 0.031(9) Uiso 1 1 d . . . H25 H 0.088(5) 0.0318(9) 0.269(2) 0.030(9) Uiso 1 1 d . . . H26 H 0.390(6) 0.0303(10) 0.427(3) 0.039(10) Uiso 1 1 d . . . H27 H 0.405(5) 0.1861(8) 0.244(2) 0.021(8) Uiso 1 1 d . . . H28 H 0.233(5) 0.1544(8) 0.114(2) 0.021(8) Uiso 1 1 d . . . H29 H -0.132(5) 0.1327(8) 0.120(2) 0.019(8) Uiso 1 1 d . . . H30 H -0.207(5) 0.1627(10) 0.307(3) 0.036(10) Uiso 1 1 d . . . H31 H 0.203(5) 0.1955(9) 0.379(2) 0.024(8) Uiso 1 1 d . . . H32 H 0.268(5) 0.2488(8) 0.265(2) 0.019(8) Uiso 1 1 d . . . H33 H 0.293(5) 0.2180(8) 0.094(2) 0.023(8) Uiso 1 1 d . . . H34 H -0.059(5) 0.1879(9) 0.017(2) 0.026(9) Uiso 1 1 d . . . H35 H -0.326(6) 0.1976(10) 0.144(3) 0.038(10) Uiso 1 1 d . . . H36 H -0.134(5) 0.2361(8) 0.298(2) 0.023(8) Uiso 1 1 d . . . H37 H -0.075(5) 0.2538(9) 0.114(2) 0.031(9) Uiso 1 1 d . . . N41 N 0.7281(4) 0.18185(8) 0.4912(2) 0.0379(6) Uani 1 1 d . . . C42 C 0.6777(5) 0.20921(8) 0.4698(2) 0.0301(6) Uani 1 1 d . . . C43 C 0.6125(5) 0.24455(9) 0.4442(3) 0.0405(8) Uani 1 1 d . . . H43A H 0.5761 0.2563 0.4965 0.112(10) Uiso 1 1 calc R . . H43B H 0.5015 0.2435 0.3943 0.112(10) Uiso 1 1 calc R . . H43C H 0.7161 0.2576 0.4245 0.112(10) Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02240(12) 0.02373(11) 0.02194(10) 0.00645(7) -0.00269(8) 0.00179(7) N1 0.0229(12) 0.0197(10) 0.0143(9) -0.0003(7) 0.0040(8) 0.0014(8) N1' 0.0191(11) 0.0221(10) 0.0164(9) 0.0030(7) 0.0018(8) 0.0018(8) N12 0.0301(14) 0.0346(13) 0.0291(12) -0.0072(10) 0.0030(10) 0.0019(10) N12' 0.0178(11) 0.0256(11) 0.0209(10) 0.0043(8) -0.0001(8) -0.0001(8) C2 0.0232(13) 0.0208(11) 0.0131(10) 0.0001(8) 0.0049(9) 0.0034(9) C2' 0.0200(13) 0.0207(11) 0.0127(10) 0.0010(8) 0.0046(9) 0.0035(9) C3 0.0283(15) 0.0201(11) 0.0199(11) 0.0018(9) 0.0023(10) 0.0048(10) C3' 0.0214(14) 0.0310(13) 0.0158(11) 0.0058(9) 0.0017(9) 0.0043(10) C4 0.0346(17) 0.0204(12) 0.0268(13) 0.0044(10) 0.0062(12) 0.0033(10) C4' 0.0183(14) 0.0381(15) 0.0198(12) 0.0065(10) -0.0014(10) -0.0012(10) C5 0.0331(16) 0.0200(12) 0.0261(13) -0.0014(10) 0.0072(11) -0.0023(10) C5' 0.0178(13) 0.0315(14) 0.0231(12) 0.0085(10) 0.0018(10) -0.0006(10) C6 0.0243(14) 0.0220(12) 0.0174(11) -0.0020(9) 0.0057(10) -0.0002(9) C6' 0.0187(13) 0.0255(12) 0.0181(11) 0.0069(9) 0.0025(9) 0.0033(9) C7 0.0169(13) 0.0107(9) 0.0256(12) -0.0088(8) 0.0150(10) -0.0082(8) C7' 0.0170(13) 0.0273(13) 0.0252(12) 0.0040(10) 0.0017(10) -0.0019(9) C8 0.076(3) 0.0176(13) 0.0308(16) -0.0039(11) 0.0332(19) -0.0035(14) C8' 0.0151(13) 0.0267(13) 0.0256(12) 0.0059(10) 0.0017(10) -0.0006(9) C9 0.0289(15) 0.0268(13) 0.0221(12) -0.0053(10) 0.0083(11) -0.0016(10) C9' 0.0107(12) 0.0280(13) 0.0218(11) 0.0073(9) 0.0006(9) -0.0009(9) C10 0.0283(16) 0.0286(13) 0.0283(13) -0.0028(11) 0.0082(11) -0.0028(11) C10' 0.0202(13) 0.0232(12) 0.0266(13) 0.0049(10) 0.0046(10) 0.0013(9) C11 0.0359(17) 0.0319(14) 0.0238(13) -0.0018(11) 0.0084(12) 0.0038(12) C11' 0.0210(13) 0.0247(12) 0.0195(11) 0.0045(9) 0.0012(9) 0.0000(9) C13 0.0323(17) 0.0283(14) 0.0339(15) -0.0077(11) 0.0046(12) -0.0029(11) C13' 0.0203(13) 0.0230(12) 0.0232(12) 0.0029(9) -0.0032(10) -0.0022(9) C14 0.0307(16) 0.0267(13) 0.0303(14) -0.0028(11) 0.0072(12) -0.0009(11) C14' 0.0226(14) 0.0278(13) 0.0204(12) 0.0046(10) -0.0032(10) -0.0029(10) N38 0.0249(14) 0.0352(13) 0.0361(13) -0.0069(11) 0.0066(11) 0.0001(10) C39 0.0197(14) 0.0273(13) 0.0257(13) 0.0022(10) 0.0047(10) 0.0031(10) C40 0.0223(16) 0.0408(18) 0.051(2) -0.0110(15) -0.0032(14) -0.0041(12) Co15 0.01417(17) 0.01804(16) 0.01307(14) -0.00140(11) 0.00196(12) -0.00007(11) C16 0.0161(12) 0.0217(11) 0.0171(10) -0.0003(8) 0.0048(9) -0.0003(9) C17 0.0168(12) 0.0184(11) 0.0154(10) -0.0006(8) 0.0013(9) -0.0006(8) C27 0.0188(13) 0.0192(11) 0.0189(11) -0.0001(8) 0.0003(9) -0.0007(9) C28 0.0207(13) 0.0219(11) 0.0150(10) -0.0008(8) 0.0036(9) 0.0029(9) B18 0.0196(14) 0.0204(12) 0.0155(11) -0.0009(9) 0.0043(10) -0.0009(10) B19 0.0166(14) 0.0232(13) 0.0220(13) -0.0028(10) 0.0054(11) -0.0033(10) B20 0.0198(14) 0.0211(13) 0.0188(12) -0.0033(10) 0.0054(10) -0.0030(10) B21 0.0245(16) 0.0210(13) 0.0219(13) 0.0001(10) 0.0082(11) 0.0023(11) B22 0.0184(15) 0.0234(13) 0.0213(13) 0.0025(10) 0.0024(11) 0.0023(10) B23 0.0217(15) 0.0224(13) 0.0169(12) 0.0020(10) 0.0041(10) 0.0019(10) B24 0.0229(15) 0.0236(13) 0.0210(13) 0.0006(10) 0.0076(11) -0.0021(11) B25 0.0256(16) 0.0192(12) 0.0226(13) -0.0029(10) 0.0074(11) -0.0034(10) B26 0.0262(16) 0.0207(13) 0.0218(13) 0.0009(10) 0.0083(11) 0.0018(11) B29 0.0196(15) 0.0288(15) 0.0190(13) -0.0013(11) -0.0007(11) 0.0021(11) B30 0.0174(15) 0.0310(15) 0.0189(12) -0.0001(11) 0.0024(10) 0.0055(11) B31 0.0268(16) 0.0204(13) 0.0162(12) -0.0035(10) 0.0018(11) 0.0028(11) B32 0.0306(17) 0.0206(13) 0.0199(13) 0.0006(10) 0.0010(11) 0.0027(11) B33 0.0275(16) 0.0229(13) 0.0183(12) 0.0028(10) 0.0044(11) 0.0030(11) B34 0.0237(16) 0.0314(15) 0.0175(12) -0.0011(11) -0.0001(11) 0.0061(12) B35 0.0195(16) 0.0355(16) 0.0232(14) 0.0013(12) 0.0018(11) 0.0079(12) B36 0.0334(18) 0.0286(15) 0.0213(14) 0.0007(11) 0.0045(12) 0.0111(13) B37 0.0293(17) 0.0283(15) 0.0219(13) 0.0022(11) 0.0042(12) 0.0101(12) N41 0.0385(17) 0.0375(15) 0.0365(14) -0.0058(11) 0.0039(12) 0.0020(12) C42 0.0296(16) 0.0363(16) 0.0228(13) -0.0070(11) 0.0012(11) -0.0019(12) C43 0.041(2) 0.0385(17) 0.0390(18) -0.0001(14) -0.0005(15) 0.0010(14) _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 N12' 2.196(2) 3_657 y Ag1 N1 2.264(2) . y Ag1 N1' 2.401(2) . y N1 C2 1.352(3) . ? N1 C6 1.356(3) . ? N1' C2' 1.342(3) . ? N1' C6' 1.343(3) . ? N12 C13 1.331(4) . ? N12 C11 1.336(4) . ? N12' C11' 1.341(3) . ? N12' C13' 1.348(3) . ? N12' Ag1 2.196(2) 3_657 ? C2 C3 1.399(3) . ? C2 C2' 1.491(4) . ? C2' C3' 1.401(4) . ? C3 C4 1.383(4) . ? C3' C4' 1.388(4) . ? C4 C5 1.384(4) . ? C4' C5' 1.386(4) . ? C5 C6 1.400(4) . ? C5' C6' 1.399(4) . ? C6 C7 1.550(4) . ? C6' C7' 1.442(4) . ? C7 C8 1.003(5) . ? C7' C8' 1.192(4) . ? C8 C9 1.512(6) . ? C8' C9' 1.436(3) . ? C9 C10 1.401(4) . ? C9 C14 1.403(4) . ? C9' C14' 1.393(4) . ? C9' C10' 1.399(4) . ? C10 C11 1.384(5) . ? C10' C11' 1.385(4) . ? C13 C14 1.377(5) . ? C13' C14' 1.387(4) . ? N38 C39 1.140(4) . ? C39 C40 1.453(4) . ? Co15 C17 2.034(2) . ? Co15 C28 2.038(2) . ? Co15 C27 2.040(3) . ? Co15 C16 2.055(3) . ? Co15 B18 2.070(3) . ? Co15 B29 2.092(3) . ? Co15 B31 2.092(3) . ? Co15 B20 2.099(3) . ? Co15 B30 2.118(3) . ? Co15 B19 2.119(3) . ? C16 C17 1.616(3) . ? C16 B21 1.697(4) . ? C16 B20 1.706(4) . ? C16 B22 1.728(4) . ? C17 B23 1.690(4) . ? C17 B18 1.707(4) . ? C17 B22 1.734(4) . ? C27 C28 1.622(4) . ? C27 B32 1.696(4) . ? C27 B31 1.706(4) . ? C27 B33 1.727(4) . ? C28 B34 1.703(4) . ? C28 B29 1.708(4) . ? C28 B33 1.725(4) . ? B18 B24 1.776(4) . ? B18 B23 1.796(4) . ? B18 B19 1.814(4) . ? B19 B24 1.798(4) . ? B19 B20 1.802(4) . ? B19 B25 1.808(4) . ? B20 B25 1.782(4) . ? B20 B21 1.801(4) . ? B21 B22 1.768(4) . ? B21 B25 1.773(4) . ? B21 B26 1.780(4) . ? B22 B23 1.765(4) . ? B22 B26 1.770(4) . ? B23 B24 1.771(4) . ? B23 B26 1.774(4) . ? B24 B26 1.774(4) . ? B24 B25 1.793(4) . ? B25 B26 1.781(5) . ? B29 B35 1.783(5) . ? B29 B30 1.800(4) . ? B29 B34 1.804(5) . ? B30 B35 1.793(4) . ? B30 B36 1.806(5) . ? B30 B31 1.808(5) . ? B31 B36 1.774(5) . ? B31 B32 1.791(4) . ? B32 B33 1.767(4) . ? B32 B36 1.772(5) . ? B32 B37 1.773(5) . ? B33 B34 1.764(5) . ? B33 B37 1.770(5) . ? B34 B35 1.772(5) . ? B34 B37 1.774(5) . ? B35 B36 1.781(5) . ? B35 B37 1.782(5) . ? B36 B37 1.775(5) . ? N41 C42 1.136(4) . ? C42 C43 1.461(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 N12' Ag1 N1 160.81(8) 3_657 . y N12' Ag1 N1' 125.41(8) 3_657 . y N1 Ag1 N1' 70.66(8) . . y C2 N1 C6 119.0(2) . . ? C2 N1 Ag1 119.15(17) . . y C6 N1 Ag1 121.69(17) . . y C2' N1' C6' 118.5(2) . . ? C2' N1' Ag1 114.23(17) . . y C6' N1' Ag1 123.68(16) . . y C13 N12 C11 116.4(3) . . ? C11' N12' C13' 118.0(2) . . ? C11' N12' Ag1 119.34(17) . 3_657 y C13' N12' Ag1 121.62(18) . 3_657 y N1 C2 C3 121.6(2) . . ? N1 C2 C2' 116.9(2) . . ? C3 C2 C2' 121.5(2) . . ? N1' C2' C3' 122.4(2) . . ? N1' C2' C2 115.5(2) . . ? C3' C2' C2 122.1(2) . . ? C4 C3 C2 119.0(3) . . ? C4' C3' C2' 118.5(2) . . ? C3 C4 C5 119.9(2) . . ? C5' C4' C3' 119.5(3) . . ? C4 C5 C6 118.5(3) . . ? C4' C5' C6' 118.3(3) . . ? N1 C6 C5 121.9(3) . . ? N1 C6 C7 115.9(2) . . ? C5 C6 C7 122.1(2) . . ? N1' C6' C5' 122.7(2) . . ? N1' C6' C7' 117.0(2) . . ? C5' C6' C7' 120.3(2) . . ? C8 C7 C6 178.8(3) . . ? C8' C7' C6' 176.8(3) . . ? C7 C8 C9 176.5(3) . . ? C7' C8' C9' 178.2(3) . . ? C10 C9 C14 117.3(3) . . ? C10 C9 C8 119.3(3) . . ? C14 C9 C8 123.4(3) . . ? C14' C9' C10' 118.0(2) . . ? C14' C9' C8' 120.9(2) . . ? C10' C9' C8' 121.1(2) . . ? C11 C10 C9 118.9(3) . . ? C11' C10' C9' 119.2(3) . . ? N12 C11 C10 123.9(3) . . ? N12' C11' C10' 122.9(2) . . ? N12 C13 C14 125.0(3) . . ? N12' C13' C14' 122.8(3) . . ? C13 C14 C9 118.3(3) . . ? C13' C14' C9' 119.1(3) . . ? N38 C39 C40 178.3(3) . . ? C17 Co15 C28 134.42(11) . . ? C17 Co15 C27 99.72(10) . . ? C28 Co15 C27 46.89(10) . . ? C17 Co15 C16 46.56(10) . . ? C28 Co15 C16 101.45(10) . . ? C27 Co15 C16 99.25(11) . . ? C17 Co15 B18 49.16(11) . . ? C28 Co15 B18 174.72(11) . . ? C27 Co15 B18 131.73(11) . . ? C16 Co15 B18 83.73(11) . . ? C17 Co15 B29 176.36(11) . . ? C28 Co15 B29 48.85(12) . . ? C27 Co15 B29 83.87(12) . . ? C16 Co15 B29 133.73(11) . . ? B18 Co15 B29 127.73(12) . . ? C17 Co15 B31 94.64(11) . . ? C28 Co15 B31 83.54(11) . . ? C27 Co15 B31 48.74(11) . . ? C16 Co15 B31 129.01(11) . . ? B18 Co15 B31 92.44(11) . . ? B29 Co15 B31 87.26(12) . . ? C17 Co15 B20 83.39(11) . . ? C28 Co15 B20 96.72(11) . . ? C27 Co15 B20 130.00(11) . . ? C16 Co15 B20 48.48(11) . . ? B18 Co15 B20 87.44(11) . . ? B29 Co15 B20 94.79(12) . . ? B31 Co15 B20 177.49(12) . . ? C17 Co15 B30 128.83(11) . . ? C28 Co15 B30 84.07(11) . . ? C27 Co15 B30 84.30(12) . . ? C16 Co15 B30 174.47(11) . . ? B18 Co15 B30 90.74(12) . . ? B29 Co15 B30 50.62(12) . . ? B31 Co15 B30 50.84(13) . . ? B20 Co15 B30 131.66(12) . . ? C17 Co15 B19 84.65(11) . . ? C28 Co15 B19 129.72(11) . . ? C27 Co15 B19 175.61(11) . . ? C16 Co15 B19 84.03(11) . . ? B18 Co15 B19 51.30(11) . . ? B29 Co15 B19 91.75(12) . . ? B31 Co15 B19 130.90(12) . . ? B20 Co15 B19 50.57(11) . . ? B30 Co15 B19 92.66(12) . . ? C17 C16 B21 111.72(19) . . ? C17 C16 B20 111.7(2) . . ? B21 C16 B20 63.90(17) . . ? C17 C16 B22 62.35(16) . . ? B21 C16 B22 62.16(17) . . ? B20 C16 B22 115.7(2) . . ? C17 C16 Co15 66.04(13) . . ? B21 C16 Co15 125.10(18) . . ? B20 C16 Co15 67.10(13) . . ? B22 C16 Co15 124.60(17) . . ? C16 C17 B23 111.25(19) . . ? C16 C17 B18 111.82(19) . . ? B23 C17 B18 63.82(17) . . ? C16 C17 B22 62.00(16) . . ? B23 C17 B22 62.03(16) . . ? B18 C17 B22 115.58(19) . . ? C16 C17 Co15 67.40(13) . . ? B23 C17 Co15 124.78(18) . . ? B18 C17 Co15 66.50(13) . . ? B22 C17 Co15 125.53(16) . . ? C28 C27 B32 111.3(2) . . ? C28 C27 B31 111.5(2) . . ? B32 C27 B31 63.54(17) . . ? C28 C27 B33 61.89(16) . . ? B32 C27 B33 62.15(17) . . ? B31 C27 B33 115.2(2) . . ? C28 C27 Co15 66.51(13) . . ? B32 C27 Co15 125.08(19) . . ? B31 C27 Co15 67.24(13) . . ? B33 C27 Co15 124.65(18) . . ? C27 C28 B34 111.2(2) . . ? C27 C28 B29 112.0(2) . . ? B34 C28 B29 63.86(18) . . ? C27 C28 B33 62.05(16) . . ? B34 C28 B33 61.92(18) . . ? B29 C28 B33 115.6(2) . . ? C27 C28 Co15 66.60(12) . . ? B34 C28 Co15 125.15(18) . . ? B29 C28 Co15 67.20(13) . . ? B33 C28 Co15 124.89(17) . . ? C17 B18 B24 103.2(2) . . ? C17 B18 B23 57.63(16) . . ? B24 B18 B23 59.44(17) . . ? C17 B18 B19 105.17(19) . . ? B24 B18 B19 60.11(16) . . ? B23 B18 B19 108.1(2) . . ? C17 B18 Co15 64.34(12) . . ? B24 B18 Co15 118.16(17) . . ? B23 B18 Co15 117.29(17) . . ? B19 B18 Co15 65.76(13) . . ? B24 B19 B20 106.0(2) . . ? B24 B19 B25 59.65(17) . . ? B20 B19 B25 59.16(16) . . ? B24 B19 B18 58.89(16) . . ? B20 B19 B18 105.7(2) . . ? B25 B19 B18 106.3(2) . . ? B24 B19 Co15 114.66(18) . . ? B20 B19 Co15 64.13(13) . . ? B25 B19 Co15 115.78(17) . . ? B18 B19 Co15 62.94(12) . . ? C16 B20 B25 103.5(2) . . ? C16 B20 B21 57.81(16) . . ? B25 B20 B21 59.32(17) . . ? C16 B20 B19 105.57(19) . . ? B25 B20 B19 60.58(17) . . ? B21 B20 B19 108.5(2) . . ? C16 B20 Co15 64.42(12) . . ? B25 B20 Co15 117.99(17) . . ? B21 B20 Co15 117.29(18) . . ? B19 B20 Co15 65.29(13) . . ? C16 B21 B22 59.80(16) . . ? C16 B21 B25 104.2(2) . . ? B22 B21 B25 108.7(2) . . ? C16 B21 B26 104.6(2) . . ? B22 B21 B26 59.85(17) . . ? B25 B21 B26 60.18(18) . . ? C16 B21 B20 58.30(16) . . ? B22 B21 B20 109.1(2) . . ? B25 B21 B20 59.81(17) . . ? B26 B21 B20 108.0(2) . . ? C16 B22 C17 55.65(14) . . ? C16 B22 B23 102.8(2) . . ? C17 B22 B23 57.76(16) . . ? C16 B22 B21 58.05(16) . . ? C17 B22 B21 103.1(2) . . ? B23 B22 B21 107.9(2) . . ? C16 B22 B26 103.7(2) . . ? C17 B22 B26 103.6(2) . . ? B23 B22 B26 60.23(17) . . ? B21 B22 B26 60.41(17) . . ? C17 B23 B22 60.21(16) . . ? C17 B23 B24 104.1(2) . . ? B22 B23 B24 108.5(2) . . ? C17 B23 B26 105.30(19) . . ? B22 B23 B26 60.05(17) . . ? B24 B23 B26 60.07(18) . . ? C17 B23 B18 58.56(15) . . ? B22 B23 B18 109.7(2) . . ? B24 B23 B18 59.71(17) . . ? B26 B23 B18 108.5(2) . . ? B23 B24 B26 60.05(17) . . ? B23 B24 B18 60.85(17) . . ? B26 B24 B18 109.4(2) . . ? B23 B24 B25 107.7(2) . . ? B26 B24 B25 59.91(17) . . ? B18 B24 B25 108.5(2) . . ? B23 B24 B19 109.9(2) . . ? B26 B24 B19 109.7(2) . . ? B18 B24 B19 61.00(16) . . ? B25 B24 B19 60.44(17) . . ? B21 B25 B26 60.12(17) . . ? B21 B25 B20 60.87(17) . . ? B26 B25 B20 108.7(2) . . ? B21 B25 B24 107.2(2) . . ? B26 B25 B24 59.50(17) . . ? B20 B25 B24 107.1(2) . . ? B21 B25 B19 109.5(2) . . ? B26 B25 B19 109.0(2) . . ? B20 B25 B19 60.25(16) . . ? B24 B25 B19 59.91(17) . . ? B22 B26 B23 59.72(17) . . ? B22 B26 B24 108.1(2) . . ? B23 B26 B24 59.88(17) . . ? B22 B26 B21 59.74(17) . . ? B23 B26 B21 107.0(2) . . ? B24 B26 B21 107.7(2) . . ? B22 B26 B25 108.2(2) . . ? B23 B26 B25 108.1(2) . . ? B24 B26 B25 60.58(18) . . ? B21 B26 B25 59.70(17) . . ? C28 B29 B35 103.2(2) . . ? C28 B29 B30 105.0(2) . . ? B35 B29 B30 60.05(17) . . ? C28 B29 B34 57.93(17) . . ? B35 B29 B34 59.19(18) . . ? B30 B29 B34 107.9(2) . . ? C28 B29 Co15 63.94(13) . . ? B35 B29 Co15 117.60(19) . . ? B30 B29 Co15 65.46(13) . . ? B34 B29 Co15 116.96(19) . . ? B35 B30 B29 59.52(17) . . ? B35 B30 B36 59.31(18) . . ? B29 B30 B36 106.5(2) . . ? B35 B30 B31 105.9(2) . . ? B29 B30 B31 106.3(2) . . ? B36 B30 B31 58.78(18) . . ? B35 B30 Co15 115.82(18) . . ? B29 B30 Co15 63.92(14) . . ? B36 B30 Co15 115.4(2) . . ? B31 B30 Co15 63.83(13) . . ? C27 B31 B36 103.7(2) . . ? C27 B31 B32 57.98(16) . . ? B36 B31 B32 59.59(19) . . ? C27 B31 B30 105.15(19) . . ? B36 B31 B30 60.56(19) . . ? B32 B31 B30 108.5(2) . . ? C27 B31 Co15 64.02(12) . . ? B36 B31 Co15 118.16(19) . . ? B32 B31 Co15 117.22(18) . . ? B30 B31 Co15 65.32(13) . . ? C27 B32 B33 59.79(16) . . ? C27 B32 B36 104.2(2) . . ? B33 B32 B36 108.3(2) . . ? C27 B32 B37 105.2(2) . . ? B33 B32 B37 60.01(18) . . ? B36 B32 B37 60.10(19) . . ? C27 B32 B31 58.48(16) . . ? B33 B32 B31 109.1(2) . . ? B36 B32 B31 59.70(18) . . ? B37 B32 B31 108.3(2) . . ? C28 B33 C27 56.06(15) . . ? C28 B33 B34 58.43(17) . . ? C27 B33 B34 103.7(2) . . ? C28 B33 B32 103.4(2) . . ? C27 B33 B32 58.06(16) . . ? B34 B33 B32 107.9(2) . . ? C28 B33 B37 104.2(2) . . ? C27 B33 B37 104.0(2) . . ? B34 B33 B37 60.26(19) . . ? B32 B33 B37 60.15(18) . . ? C28 B34 B33 59.64(17) . . ? C28 B34 B35 103.9(2) . . ? B33 B34 B35 108.5(2) . . ? C28 B34 B37 104.9(2) . . ? B33 B34 B37 60.06(19) . . ? B35 B34 B37 60.33(19) . . ? C28 B34 B29 58.21(17) . . ? B33 B34 B29 109.0(2) . . ? B35 B34 B29 59.82(18) . . ? B37 B34 B29 108.5(2) . . ? B34 B35 B36 107.6(2) . . ? B34 B35 B37 59.89(19) . . ? B36 B35 B37 59.77(19) . . ? B34 B35 B29 60.99(18) . . ? B36 B35 B29 108.3(2) . . ? B37 B35 B29 109.1(2) . . ? B34 B35 B30 109.6(2) . . ? B36 B35 B30 60.71(18) . . ? B37 B35 B30 109.6(2) . . ? B29 B35 B30 60.43(17) . . ? B32 B36 B31 60.70(18) . . ? B32 B36 B37 59.99(19) . . ? B31 B36 B37 109.0(2) . . ? B32 B36 B35 107.7(2) . . ? B31 B36 B35 107.9(2) . . ? B37 B36 B35 60.14(19) . . ? B32 B36 B30 109.5(2) . . ? B31 B36 B30 60.66(17) . . ? B37 B36 B30 109.3(2) . . ? B35 B36 B30 59.98(18) . . ? B33 B37 B32 59.84(18) . . ? B33 B37 B34 59.68(18) . . ? B32 B37 B34 107.2(2) . . ? B33 B37 B36 108.0(2) . . ? B32 B37 B36 59.91(19) . . ? B34 B37 B36 107.7(2) . . ? B33 B37 B35 107.7(2) . . ? B32 B37 B35 107.6(2) . . ? B34 B37 B35 59.78(19) . . ? B36 B37 B35 60.09(19) . . ? N41 C42 C43 178.9(3) . . ? _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.944 _refine_diff_density_max 1.43 _refine_diff_density_min -0.74 _refine_diff_density_rms 0.12 #===END