# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_sad _database_code_depnum_ccdc_archive 'CCDC 913591' #TrackingRef '(H4-1)(Br)4-new-913591.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56 Br4 N8 O6' _chemical_formula_weight 1016.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.0020(4) _cell_length_b 19.5502(6) _cell_length_c 9.0187(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.397(2) _cell_angle_gamma 90.00 _cell_volume 2187.61(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 4.908 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6143 _exptl_absorpt_correction_T_max 0.8279 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.702899 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10315 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 72.40 _reflns_number_total 3889 _reflns_number_gt 3433 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ; Brucker SHELXTL ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The diffrn_measured_fraction_theta_max value has been evaluated as low. This is caused by the instrumental set-up when using Cu-Ka radiation. The number of reflections:refined parameters is larger than 15.5. ; _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^)+(0.0543P)^2^+3.5266P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3889 _refine_ls_number_parameters 250 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0512 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1247 _refine_ls_wR_factor_gt 0.1204 _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 Br1 Br 0.89807(4) 0.44064(2) 0.65301(5) 0.03807(16) Uani 1 1 d . . . Br2 Br 0.19949(3) 0.32733(2) 0.94207(5) 0.03106(15) Uani 1 1 d . . . C1 C 0.0482(3) 0.58831(19) 0.7043(4) 0.0250(7) Uani 1 1 d . . . H1 H 0.0407 0.5924 0.5966 0.030 Uiso 1 1 calc R . . C2 C 0.1029(3) 0.5556(2) 0.9494(5) 0.0304(8) Uani 1 1 d . . . H2 H 0.1418 0.5326 1.0420 0.036 Uiso 1 1 calc R . . C3 C 0.0232(3) 0.6012(2) 0.9345(4) 0.0298(8) Uani 1 1 d . . . H3 H -0.0051 0.6164 1.0144 0.036 Uiso 1 1 calc R . . C4 C -0.0953(3) 0.67070(18) 0.7102(5) 0.0289(8) Uani 1 1 d . . . H4A H -0.1132 0.6974 0.7924 0.035 Uiso 1 1 calc R . . H4B H -0.0699 0.7030 0.6441 0.035 Uiso 1 1 calc R . . C5 C -0.2231(3) 0.63287(19) 0.4610(4) 0.0258(8) Uani 1 1 d . . . H5 H -0.1886 0.6545 0.3943 0.031 Uiso 1 1 calc R . . C6 C -0.2611(3) 0.5967(2) 0.6708(4) 0.0316(8) Uani 1 1 d . . . H6 H -0.2568 0.5893 0.7766 0.038 Uiso 1 1 calc R . . C7 C 0.3366(3) 0.4282(2) 0.4540(5) 0.0326(9) Uani 1 1 d . . . H7 H 0.3960 0.4564 0.4530 0.039 Uiso 1 1 calc R . . C8 C 0.3764(3) 0.4182(2) 0.7455(4) 0.0286(8) Uani 1 1 d . . . H8A H 0.4481 0.3968 0.7641 0.034 Uiso 1 1 calc R . . H8B H 0.3408 0.3963 0.8160 0.034 Uiso 1 1 calc R . . C9 C 0.3910(3) 0.4931(2) 0.7839(4) 0.0267(8) Uani 1 1 d . . . C10 C 0.4932(3) 0.5220(2) 0.8124(4) 0.0327(9) Uani 1 1 d . . . H10 H 0.5514 0.4945 0.8041 0.039 Uiso 1 1 calc R . . C11 C 0.5109(3) 0.5900(2) 0.8525(5) 0.0387(10) Uani 1 1 d . . . H11 H 0.5809 0.6090 0.8719 0.046 Uiso 1 1 calc R . . C12 C 0.4269(4) 0.6302(2) 0.8644(5) 0.0397(10) Uani 1 1 d . . . H12 H 0.4389 0.6771 0.8915 0.048 Uiso 1 1 calc R . . C13 C 0.3252(3) 0.6024(2) 0.8371(5) 0.0337(9) Uani 1 1 d . . . H13 H 0.2677 0.6306 0.8455 0.040 Uiso 1 1 calc R . . C14 C 0.3057(3) 0.5341(2) 0.7977(4) 0.0257(7) Uani 1 1 d . . . C15 C 0.1942(3) 0.50306(18) 0.7633(5) 0.0273(8) Uani 1 1 d . . . H15A H 0.1668 0.4920 0.6512 0.033 Uiso 1 1 calc R . . H15B H 0.1993 0.4598 0.8219 0.033 Uiso 1 1 calc R . . C21 C 0.1270(5) 0.7335(3) 0.5304(8) 0.0658(15) Uani 1 1 d . . . H21A H 0.1564 0.7656 0.4700 0.099 Uiso 1 1 calc R . . H21B H 0.1756 0.6943 0.5614 0.099 Uiso 1 1 calc R . . H21C H 0.1199 0.7565 0.6233 0.099 Uiso 1 1 calc R . . C22 C 0.5654(6) 0.7332(4) 0.6343(9) 0.085(2) Uani 1 1 d . . . H22A H 0.6334 0.7269 0.7171 0.128 Uiso 1 1 calc R . . H22B H 0.5152 0.6965 0.6391 0.128 Uiso 1 1 calc R . . H22C H 0.5338 0.7775 0.6477 0.128 Uiso 1 1 calc R . . C23 C 0.6512(7) 0.3489(4) 0.6865(15) 0.123(4) Uani 1 1 d . . . H23A H 0.6908 0.3265 0.6229 0.185 Uiso 1 1 calc R . . H23B H 0.5777 0.3306 0.6592 0.185 Uiso 1 1 calc R . . H23C H 0.6879 0.3401 0.7966 0.185 Uiso 1 1 calc R . . N1 N 0.1177(2) 0.54841(15) 0.8041(4) 0.0250(6) Uani 1 1 d . . . N2 N -0.0099(2) 0.62203(15) 0.7813(4) 0.0242(6) Uani 1 1 d . . . N3 N -0.1910(2) 0.63531(15) 0.6164(4) 0.0247(6) Uani 1 1 d . . . N4 N 0.3118(2) 0.40531(16) 0.5836(3) 0.0255(6) Uani 1 1 d . . . O1 O 0.0246(3) 0.71055(19) 0.4386(4) 0.0550(9) Uani 1 1 d . . . H25 H 0.0322 0.6768 0.3853 0.083 Uiso 1 1 calc R . . O2 O 0.6475(4) 0.4157(2) 0.6604(8) 0.0929(17) Uani 1 1 d . . . H26 H 0.7071 0.4290 0.6527 0.139 Uiso 1 1 calc R . . O3 O 0.5862(3) 0.7316(2) 0.4801(5) 0.0721(11) Uani 1 1 d . . . H27 H 0.6464 0.7495 0.4882 0.108 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 Br1 0.0464(3) 0.0411(3) 0.0301(2) -0.00475(18) 0.0166(2) -0.00390(18) Br2 0.0333(2) 0.0328(2) 0.0305(2) -0.00427(17) 0.01462(18) -0.00562(15) C1 0.0256(18) 0.0274(18) 0.0234(17) 0.0001(16) 0.0097(15) 0.0016(14) C2 0.033(2) 0.036(2) 0.0222(18) 0.0050(17) 0.0083(16) 0.0011(16) C3 0.0313(19) 0.036(2) 0.0233(18) -0.0016(17) 0.0098(16) -0.0006(16) C4 0.0297(19) 0.0257(18) 0.032(2) -0.0062(16) 0.0096(17) -0.0009(14) C5 0.0265(18) 0.0256(18) 0.0273(18) 0.0000(16) 0.0113(16) 0.0007(14) C6 0.035(2) 0.039(2) 0.0251(18) 0.0014(18) 0.0151(17) -0.0015(17) C7 0.034(2) 0.039(2) 0.030(2) -0.0032(18) 0.0161(18) -0.0063(16) C8 0.0263(18) 0.035(2) 0.0238(17) 0.0021(17) 0.0061(16) 0.0047(15) C9 0.0263(18) 0.036(2) 0.0169(16) 0.0024(16) 0.0057(15) 0.0002(15) C10 0.0238(18) 0.050(2) 0.0245(18) -0.0024(18) 0.0079(16) -0.0042(16) C11 0.031(2) 0.052(3) 0.035(2) -0.002(2) 0.0125(18) -0.0145(19) C12 0.043(2) 0.036(2) 0.041(2) -0.007(2) 0.013(2) -0.0136(18) C13 0.032(2) 0.034(2) 0.036(2) -0.0039(19) 0.0115(18) -0.0021(16) C14 0.0252(18) 0.0320(19) 0.0198(16) 0.0001(16) 0.0067(15) -0.0012(15) C15 0.0227(17) 0.0262(18) 0.034(2) -0.0023(17) 0.0096(16) 0.0011(14) C21 0.077(4) 0.049(3) 0.073(4) 0.013(3) 0.024(3) 0.010(3) C22 0.097(5) 0.077(4) 0.101(5) 0.036(4) 0.058(5) 0.029(4) C23 0.092(5) 0.066(4) 0.247(13) 0.017(6) 0.106(7) 0.007(4) N1 0.0224(15) 0.0275(15) 0.0260(15) -0.0007(13) 0.0087(13) 0.0010(12) N2 0.0245(15) 0.0240(15) 0.0246(15) 0.0000(13) 0.0080(13) 0.0009(11) N3 0.0246(15) 0.0251(15) 0.0253(15) -0.0024(14) 0.0091(13) 0.0010(12) N4 0.0261(15) 0.0280(15) 0.0244(15) -0.0014(14) 0.0106(13) 0.0022(12) O1 0.065(2) 0.053(2) 0.0454(19) 0.0002(17) 0.0132(17) 0.0191(17) O2 0.085(3) 0.065(3) 0.157(5) 0.019(3) 0.080(4) 0.017(2) O3 0.065(3) 0.071(3) 0.081(3) 0.006(2) 0.022(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.323(5) . ? C1 N2 1.342(5) . ? C2 C3 1.343(6) . ? C2 N1 1.387(5) . ? C3 N2 1.380(5) . ? C4 N3 1.454(5) . ? C4 N2 1.457(5) . ? C5 N4 1.331(5) 3_566 ? C5 N3 1.338(5) . ? C6 C7 1.345(6) 3_566 ? C6 N3 1.381(5) . ? C7 C6 1.345(6) 3_566 ? C7 N4 1.377(5) . ? C8 N4 1.472(5) . ? C8 C9 1.502(5) . ? C9 C10 1.395(5) . ? C9 C14 1.405(5) . ? C10 C11 1.378(6) . ? C11 C12 1.375(6) . ? C12 C13 1.383(6) . ? C13 C14 1.384(6) . ? C14 C15 1.517(5) . ? C15 N1 1.460(4) . ? C21 O1 1.414(7) . ? C22 O3 1.494(8) . ? C23 O2 1.326(8) . ? N4 C5 1.331(5) 3_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 108.2(3) . . ? C3 C2 N1 107.0(3) . . ? C2 C3 N2 107.2(3) . . ? N3 C4 N2 110.6(3) . . ? N4 C5 N3 107.9(3) 3_566 . ? C7 C6 N3 107.1(3) 3_566 . ? C6 C7 N4 107.1(3) 3_566 . ? N4 C8 C9 113.0(3) . . ? C10 C9 C14 119.0(4) . . ? C10 C9 C8 119.0(3) . . ? C14 C9 C8 121.9(3) . . ? C11 C10 C9 121.0(4) . . ? C12 C11 C10 119.8(4) . . ? C11 C12 C13 120.1(4) . . ? C12 C13 C14 121.1(4) . . ? C13 C14 C9 119.0(3) . . ? C13 C14 C15 121.9(3) . . ? C9 C14 C15 119.0(3) . . ? N1 C15 C14 112.8(3) . . ? C1 N1 C2 108.9(3) . . ? C1 N1 C15 124.4(3) . . ? C2 N1 C15 126.7(3) . . ? C1 N2 C3 108.6(3) . . ? C1 N2 C4 124.5(3) . . ? C3 N2 C4 127.0(3) . . ? C5 N3 C6 108.7(3) . . ? C5 N3 C4 124.8(3) . . ? C6 N3 C4 126.4(3) . . ? C5 N4 C7 109.2(3) 3_566 . ? C5 N4 C8 125.6(3) 3_566 . ? C7 N4 C8 125.2(3) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 72.40 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 1.164 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.108 data_sad_(H4-1)(PF6)4 _database_code_depnum_ccdc_archive 'CCDC 913592' #TrackingRef '(H4-1)(PF6)4-new-913592.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H38 F24 N10 P4' _chemical_formula_weight 1166.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.1901(5) _cell_length_b 8.9195(3) _cell_length_c 19.5264(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.171(2) _cell_angle_gamma 90.00 _cell_volume 2283.95(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.696 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 2.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5882 _exptl_absorpt_correction_T_max 0.7652 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.661652 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12957 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 71.90 _reflns_number_total 4185 _reflns_number_gt 3593 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ; Bruker SHELXTL ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The diffrn_measured_fraction_theta_max value has been evaluated as low. This is caused by the instrumental set-up when using Cu-Ka radiation. The number of reflections:refined parameters is larger than 12.8. ; _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^)+(0.0630P)^2^+2.1620P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4185 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0488 _refine_ls_wR_factor_ref 0.1351 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 C1 C 0.37736(18) 0.3445(3) 0.06773(12) 0.0259(5) Uani 1 1 d . . . H1 H 0.4011 0.3044 0.0273 0.031 Uiso 1 1 calc R . . C2 C 0.29970(19) 0.4861(3) 0.13762(12) 0.0274(5) Uani 1 1 d . . . H2 H 0.2595 0.5639 0.1540 0.033 Uiso 1 1 calc R . . C3 C 0.34820(18) 0.3765(3) 0.17556(12) 0.0275(5) Uani 1 1 d . . . H3 H 0.3487 0.3621 0.2238 0.033 Uiso 1 1 calc R . . C4 C 0.46388(18) 0.1614(3) 0.14886(13) 0.0283(5) Uani 1 1 d . . . H4A H 0.4493 0.0809 0.1143 0.034 Uiso 1 1 calc R . . H4B H 0.4504 0.1214 0.1943 0.034 Uiso 1 1 calc R . . C5 C 0.63221(19) 0.1745(3) 0.10290(12) 0.0255(5) Uani 1 1 d . . . H5 H 0.6138 0.1196 0.0618 0.031 Uiso 1 1 calc R . . C6 C 0.62572(19) 0.2859(3) 0.20305(12) 0.0269(5) Uani 1 1 d . . . H6 H 0.6012 0.3224 0.2439 0.032 Uiso 1 1 calc R . . C7 C 0.72057(19) 0.3028(3) 0.18475(12) 0.0272(5) Uani 1 1 d . . . H7 H 0.7756 0.3534 0.2104 0.033 Uiso 1 1 calc R . . C8 C 0.81440(19) 0.2188(3) 0.08389(13) 0.0289(5) Uani 1 1 d . . . H8A H 0.7944 0.1704 0.0388 0.035 Uiso 1 1 calc R . . H8B H 0.8654 0.1537 0.1103 0.035 Uiso 1 1 calc R . . C9 C 0.86162(18) 0.3690(3) 0.07242(12) 0.0275(5) Uani 1 1 d . . . C10 C 0.9552(2) 0.4045(4) 0.10848(13) 0.0363(6) Uani 1 1 d . . . H10 H 0.9882 0.3337 0.1397 0.044 Uiso 1 1 calc R . . C11 C 1.0009(2) 0.5415(4) 0.09942(14) 0.0407(7) Uani 1 1 d . . . H11 H 1.0647 0.5644 0.1246 0.049 Uiso 1 1 calc R . . C12 C 0.0457(2) 0.3550(3) -0.05409(14) 0.0381(6) Uani 1 1 d . . . H12 H 0.0139 0.2613 -0.0476 0.046 Uiso 1 1 calc R . . C13 C 0.1391(2) 0.3882(3) -0.01801(13) 0.0315(6) Uani 1 1 d . . . H13 H 0.1716 0.3162 0.0128 0.038 Uiso 1 1 calc R . . C14 C 0.18594(18) 0.5255(3) -0.02627(12) 0.0254(5) Uani 1 1 d . . . C15 C 0.28911(18) 0.5632(3) 0.01148(12) 0.0275(5) Uani 1 1 d . . . H15A H 0.3412 0.5569 -0.0213 0.033 Uiso 1 1 calc R . . H15B H 0.2878 0.6679 0.0281 0.033 Uiso 1 1 calc R . . C21 C 0.8692(3) 0.9049(4) 0.22685(14) 0.0461(8) Uani 1 1 d . . . C22 C 0.8867(4) 0.7476(4) 0.2191(2) 0.0684(11) Uani 1 1 d . . . H22A H 0.9600 0.7293 0.2189 0.103 Uiso 1 1 calc R . . H22B H 0.8505 0.7128 0.1755 0.103 Uiso 1 1 calc R . . H22C H 0.8616 0.6931 0.2574 0.103 Uiso 1 1 calc R . . N4 N 0.72300(15) 0.2333(2) 0.12216(10) 0.0234(4) Uani 1 1 d . . . N3 N 0.57088(15) 0.2058(2) 0.15130(10) 0.0233(4) Uani 1 1 d . . . N2 N 0.39713(15) 0.2890(2) 0.13093(10) 0.0234(4) Uani 1 1 d . . . N1 N 0.31950(15) 0.4640(2) 0.07052(10) 0.0236(4) Uani 1 1 d . . . N11 N 0.8563(3) 1.0289(4) 0.23420(16) 0.0656(9) Uani 1 1 d . . . P1 P 0.18609(5) 0.98325(7) 0.11403(4) 0.03075(19) Uani 1 1 d . . . P2 P 0.55561(5) 0.73848(7) 0.12020(3) 0.02918(19) Uani 1 1 d . . . F1 F 0.10283(15) 0.9593(2) 0.16593(11) 0.0577(5) Uani 1 1 d . . . F2 F 0.27269(14) 1.0059(2) 0.06251(9) 0.0499(5) Uani 1 1 d . . . F3 F 0.27363(14) 0.9897(2) 0.17753(9) 0.0502(5) Uani 1 1 d . . . F4 F 0.10216(15) 0.9778(3) 0.04968(11) 0.0632(6) Uani 1 1 d . . . F5 F 0.17426(15) 1.16003(19) 0.11889(10) 0.0519(5) Uani 1 1 d . . . F6 F 0.19952(16) 0.8062(2) 0.10820(12) 0.0658(6) Uani 1 1 d . . . F7 F 0.52350(15) 0.5957(2) 0.07358(9) 0.0526(5) Uani 1 1 d . . . F8 F 0.58504(16) 0.88469(19) 0.16491(9) 0.0533(5) Uani 1 1 d . . . F9 F 0.53016(17) 0.8448(2) 0.05308(9) 0.0583(5) Uani 1 1 d . . . F10 F 0.5787(2) 0.6377(2) 0.18557(10) 0.0814(8) Uani 1 1 d . . . F11 F 0.66713(15) 0.7220(3) 0.09990(12) 0.0654(6) Uani 1 1 d . . . F12 F 0.44092(16) 0.7608(3) 0.13604(12) 0.0722(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0290(13) 0.0271(13) 0.0222(11) 0.0011(9) 0.0061(9) -0.0015(9) C2 0.0286(13) 0.0297(13) 0.0244(12) -0.0026(9) 0.0057(10) 0.0006(9) C3 0.0286(13) 0.0328(14) 0.0217(11) -0.0004(9) 0.0055(9) -0.0010(10) C4 0.0268(13) 0.0242(12) 0.0342(13) 0.0059(10) 0.0048(10) -0.0019(9) C5 0.0327(13) 0.0215(12) 0.0222(11) 0.0017(9) 0.0037(9) 0.0003(9) C6 0.0317(13) 0.0268(13) 0.0223(11) -0.0013(9) 0.0039(9) 0.0020(9) C7 0.0289(13) 0.0277(13) 0.0248(12) -0.0026(9) 0.0011(9) 0.0006(9) C8 0.0301(13) 0.0321(14) 0.0260(12) 0.0061(10) 0.0097(10) 0.0082(10) C9 0.0250(12) 0.0351(14) 0.0236(11) 0.0007(10) 0.0082(9) 0.0020(10) C10 0.0263(13) 0.0560(18) 0.0268(13) 0.0047(12) 0.0039(10) 0.0063(12) C11 0.0271(14) 0.062(2) 0.0327(14) -0.0058(13) 0.0029(11) -0.0088(12) C12 0.0341(15) 0.0472(17) 0.0342(14) -0.0062(12) 0.0094(11) -0.0154(12) C13 0.0327(14) 0.0349(14) 0.0277(12) 0.0033(10) 0.0074(10) -0.0048(10) C14 0.0236(12) 0.0322(13) 0.0211(11) 0.0019(9) 0.0055(9) -0.0013(9) C15 0.0290(13) 0.0264(13) 0.0266(12) 0.0094(10) 0.0005(10) -0.0025(9) C21 0.0538(19) 0.057(2) 0.0281(14) 0.0087(13) 0.0082(13) 0.0163(15) C22 0.100(3) 0.060(2) 0.045(2) -0.0030(16) 0.007(2) 0.023(2) N4 0.0270(10) 0.0231(10) 0.0205(9) 0.0036(7) 0.0049(8) 0.0028(7) N3 0.0242(10) 0.0201(10) 0.0259(10) 0.0027(8) 0.0039(8) 0.0005(7) N2 0.0244(10) 0.0229(10) 0.0233(9) 0.0026(8) 0.0049(8) -0.0030(7) N1 0.0243(10) 0.0255(10) 0.0206(9) 0.0026(8) 0.0012(8) -0.0023(8) N11 0.084(2) 0.061(2) 0.0522(18) 0.0133(15) 0.0074(16) 0.0229(17) P1 0.0302(4) 0.0244(4) 0.0377(4) 0.0004(3) 0.0040(3) -0.0036(2) P2 0.0375(4) 0.0271(4) 0.0236(3) -0.0046(2) 0.0060(3) -0.0022(2) F1 0.0529(11) 0.0509(11) 0.0747(13) -0.0068(10) 0.0323(10) -0.0128(9) F2 0.0481(11) 0.0621(12) 0.0411(9) -0.0046(8) 0.0121(8) -0.0140(8) F3 0.0465(10) 0.0640(12) 0.0381(9) 0.0155(8) -0.0048(8) -0.0051(8) F4 0.0470(11) 0.0759(14) 0.0623(13) -0.0083(10) -0.0145(10) -0.0115(9) F5 0.0651(12) 0.0267(9) 0.0633(12) 0.0042(8) 0.0040(9) 0.0007(8) F6 0.0715(14) 0.0278(10) 0.1021(17) -0.0056(10) 0.0278(12) 0.0007(8) F7 0.0651(12) 0.0433(10) 0.0520(10) -0.0209(8) 0.0192(9) -0.0202(8) F8 0.0929(14) 0.0284(9) 0.0343(9) -0.0064(7) -0.0125(9) 0.0017(8) F9 0.0917(15) 0.0527(12) 0.0291(9) 0.0003(8) 0.0005(9) 0.0103(10) F10 0.172(3) 0.0354(11) 0.0368(10) 0.0062(8) 0.0119(13) 0.0259(13) F11 0.0373(11) 0.0782(15) 0.0812(15) -0.0241(12) 0.0089(9) -0.0077(9) F12 0.0580(14) 0.0781(16) 0.0867(16) -0.0200(12) 0.0362(12) -0.0010(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.315(3) . ? C1 N2 1.329(3) . ? C2 C3 1.346(4) . ? C2 N1 1.377(3) . ? C3 N2 1.380(3) . ? C4 N2 1.459(3) . ? C4 N3 1.462(3) . ? C5 N4 1.324(3) . ? C5 N3 1.338(3) . ? C6 C7 1.346(3) . ? C6 N3 1.378(3) . ? C7 N4 1.374(3) . ? C8 N4 1.491(3) . ? C8 C9 1.504(4) . ? C9 C10 1.390(4) . ? C9 C14 1.403(3) 3_665 ? C10 C11 1.382(4) . ? C11 C12 1.377(4) 3_665 ? C12 C11 1.377(4) 3_665 ? C12 C13 1.384(4) . ? C13 C14 1.388(4) . ? C14 C9 1.403(3) 3_665 ? C14 C15 1.514(3) . ? C15 N1 1.474(3) . ? C21 N11 1.131(4) . ? C21 C22 1.433(5) . ? P1 F4 1.584(2) . ? P1 F1 1.5868(18) . ? P1 F5 1.5884(18) . ? P1 F6 1.5942(19) . ? P1 F3 1.6020(18) . ? P1 F2 1.6141(18) . ? P2 F10 1.564(2) . ? P2 F11 1.571(2) . ? P2 F12 1.589(2) . ? P2 F8 1.5940(17) . ? P2 F7 1.5962(17) . ? P2 F9 1.6231(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 108.7(2) . . ? C3 C2 N1 107.0(2) . . ? C2 C3 N2 106.8(2) . . ? N2 C4 N3 110.59(19) . . ? N4 C5 N3 108.3(2) . . ? C7 C6 N3 107.0(2) . . ? C6 C7 N4 107.3(2) . . ? N4 C8 C9 111.54(19) . . ? C10 C9 C14 118.9(2) . 3_665 ? C10 C9 C8 119.1(2) . . ? C14 C9 C8 121.9(2) 3_665 . ? C11 C10 C9 120.8(3) . . ? C12 C11 C10 120.3(3) 3_665 . ? C11 C12 C13 119.6(3) 3_665 . ? C12 C13 C14 120.8(3) . . ? C13 C14 C9 119.5(2) . 3_665 ? C13 C14 C15 121.8(2) . . ? C9 C14 C15 118.7(2) 3_665 . ? N1 C15 C14 113.71(19) . . ? N11 C21 C22 178.7(4) . . ? C5 N4 C7 108.9(2) . . ? C5 N4 C8 125.3(2) . . ? C7 N4 C8 125.6(2) . . ? C5 N3 C6 108.46(19) . . ? C5 N3 C4 125.1(2) . . ? C6 N3 C4 126.4(2) . . ? C1 N2 C3 108.5(2) . . ? C1 N2 C4 124.5(2) . . ? C3 N2 C4 126.9(2) . . ? C1 N1 C2 109.0(2) . . ? C1 N1 C15 124.3(2) . . ? C2 N1 C15 126.5(2) . . ? F4 P1 F1 91.72(12) . . ? F4 P1 F5 90.74(11) . . ? F1 P1 F5 90.95(11) . . ? F4 P1 F6 89.23(12) . . ? F1 P1 F6 90.11(11) . . ? F5 P1 F6 178.94(12) . . ? F4 P1 F3 178.21(11) . . ? F1 P1 F3 90.07(11) . . ? F5 P1 F3 89.17(10) . . ? F6 P1 F3 90.83(12) . . ? F4 P1 F2 89.45(11) . . ? F1 P1 F2 178.69(12) . . ? F5 P1 F2 89.62(10) . . ? F6 P1 F2 89.32(11) . . ? F3 P1 F2 88.76(10) . . ? F10 P2 F11 92.66(15) . . ? F10 P2 F12 91.10(15) . . ? F11 P2 F12 176.21(14) . . ? F10 P2 F8 90.50(11) . . ? F11 P2 F8 92.02(11) . . ? F12 P2 F8 88.39(12) . . ? F10 P2 F7 91.33(11) . . ? F11 P2 F7 88.84(10) . . ? F12 P2 F7 90.63(11) . . ? F8 P2 F7 177.95(11) . . ? F10 P2 F9 178.97(12) . . ? F11 P2 F9 88.22(12) . . ? F12 P2 F9 88.02(13) . . ? F8 P2 F9 88.93(10) . . ? F7 P2 F9 89.23(10) . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 71.90 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.611 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.107 data_platon _database_code_depnum_ccdc_archive 'CCDC 913593' #TrackingRef '[Ag2(1)](PF6)2-new913593.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 Ag2 F12 N8 O P2 S' _chemical_formula_weight 1084.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.1472(6) _cell_length_b 14.5134(7) _cell_length_c 31.8567(12) _cell_angle_alpha 90.00 _cell_angle_beta 99.567(3) _cell_angle_gamma 90.00 _cell_volume 5082.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent stick' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2152 _exptl_absorpt_coefficient_mu 7.846 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2771 _exptl_absorpt_correction_T_max 0.6503 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.279065 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27706 _diffrn_reflns_av_R_equivalents 0.0894 _diffrn_reflns_av_sigmaI/netI 0.1244 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 72.63 _reflns_number_total 9380 _reflns_number_gt 7314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ; Bruker SHELXTL ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The diffrn_measured_fraction_theta_max value has been evaluated as low. This is caused by the instrumental set-up when using Cu-Ka radiation. The number of reflections:refined parameters is larger than 17.7. A final Difference Fourier map feature some large peaks. The were assigned to solvent molecules (DMSO). Refinement of the positional parameters of these solvent molecules did not proceed satisfactorily due to disorder. The program SQUEEZE was therefore used to remove mathematically the effect of the disordered solvent molecules. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.007 0.514 0.009 1663 212 ' ' _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^)+(0.1174P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9380 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2119 _refine_ls_wR_factor_gt 0.1988 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.62340(4) 0.04657(3) 0.974675(12) 0.03659(17) Uani 1 1 d . . . Ag2 Ag 0.69558(4) 0.13607(3) 0.896517(13) 0.04029(17) Uani 1 1 d . . . S31 S 0.3970(2) 0.1602(3) 0.84613(9) 0.1170(13) Uani 1 1 d . . . P1 P 0.25275(19) 0.42790(12) 0.92630(8) 0.0617(5) Uani 1 1 d . . . P2 P 0.17914(16) 0.88176(13) 0.79137(5) 0.0458(4) Uani 1 1 d . . . F1 F 0.1814(6) 0.4015(5) 0.8818(2) 0.1044(19) Uani 1 1 d . . . F2 F 0.3472(6) 0.3486(4) 0.9226(2) 0.102(2) Uani 1 1 d . . . F3 F 0.1602(6) 0.5043(4) 0.9342(2) 0.119(2) Uani 1 1 d . . . F4 F 0.3278(6) 0.4519(5) 0.9721(2) 0.112(2) Uani 1 1 d . . . F5 F 0.1723(6) 0.3541(4) 0.9479(2) 0.110(2) Uani 1 1 d . . . F6 F 0.3093(5) 0.8707(5) 0.81792(17) 0.113(2) Uani 1 1 d . . . F7 F 0.1522(9) 0.9596(8) 0.8206(3) 0.193(6) Uani 1 1 d . . . F8 F 0.1263(9) 0.8354(11) 0.8272(3) 0.217(7) Uani 1 1 d . . . F9 F 0.2291(8) 0.9406(10) 0.7590(4) 0.215(6) Uani 1 1 d . . . F10 F 0.2120(10) 0.8077(9) 0.7613(3) 0.211(6) Uani 1 1 d . . . F11 F 0.0494(5) 0.8919(8) 0.76521(18) 0.156(4) Uani 1 1 d . . . F12 F 0.3314(8) 0.4991(5) 0.9075(2) 0.132(3) Uani 1 1 d . . . O31 O 0.4502(4) 0.1292(3) 0.88914(15) 0.0357(11) Uani 0.80 1 d P . . O31A O 0.426(2) 0.1301(14) 0.8052(7) 0.044(5) Uiso 0.20 1 d P . . N1 N 0.6730(5) -0.1548(3) 0.98585(17) 0.0429(12) Uani 1 1 d . . . N2 N 0.6131(5) -0.1373(3) 0.91918(16) 0.0418(12) Uani 1 1 d . . . N3 N 0.6758(5) -0.0684(4) 0.85854(16) 0.0431(12) Uani 1 1 d . . . N4 N 0.8229(5) 0.0102(4) 0.84141(15) 0.0441(12) Uani 1 1 d . . . N5 N 0.8447(6) 0.3100(4) 0.91483(18) 0.0544(15) Uani 1 1 d . . . N6 N 0.7005(6) 0.3214(4) 0.95203(18) 0.0542(15) Uani 1 1 d . . . N7 N 0.6308(5) 0.2530(3) 1.01188(17) 0.0448(12) Uani 1 1 d . . . N8 N 0.6804(5) 0.1450(3) 1.05767(16) 0.0408(12) Uani 1 1 d . . . C1 C 0.6333(6) -0.0904(4) 0.95615(19) 0.0374(13) Uani 1 1 d . . . C2 C 0.6784(8) -0.2387(5) 0.9671(3) 0.060(2) Uani 1 1 d . . . H2 H 0.7047 -0.2945 0.9813 0.073 Uiso 1 1 calc R . . C3 C 0.6403(7) -0.2291(4) 0.9253(3) 0.0564(18) Uani 1 1 d . . . H3 H 0.6334 -0.2760 0.9042 0.068 Uiso 1 1 calc R . . C4 C 0.5754(5) -0.0939(5) 0.87766(19) 0.0429(14) Uani 1 1 d . . . H4A H 0.5235 -0.1373 0.8587 0.051 Uiso 1 1 calc R . . H4B H 0.5262 -0.0385 0.8812 0.051 Uiso 1 1 calc R . . C5 C 0.7292(5) 0.0167(4) 0.86255(18) 0.0383(13) Uani 1 1 d . . . C6 C 0.7402(7) -0.1258(6) 0.8345(2) 0.0560(19) Uani 1 1 d . . . H6 H 0.7233 -0.1884 0.8272 0.067 Uiso 1 1 calc R . . C7 C 0.8329(7) -0.0725(6) 0.8239(2) 0.0579(19) Uani 1 1 d . . . H7 H 0.8922 -0.0909 0.8073 0.070 Uiso 1 1 calc R . . C8 C 0.9079(6) 0.0886(6) 0.8379(2) 0.0530(18) Uani 1 1 d . . . H8A H 0.9665 0.0702 0.8192 0.064 Uiso 1 1 calc R . . H8B H 0.9546 0.1024 0.8664 0.064 Uiso 1 1 calc R . . C9 C 0.8418(6) 0.1736(6) 0.8202(2) 0.0532(18) Uani 1 1 d . . . C10 C 0.7718(7) 0.1671(7) 0.7800(2) 0.067(2) Uani 1 1 d . . . H10 H 0.7683 0.1104 0.7649 0.081 Uiso 1 1 calc R . . C11 C 0.7066(8) 0.2426(8) 0.7613(2) 0.081(3) Uani 1 1 d . . . H11 H 0.6572 0.2368 0.7341 0.097 Uiso 1 1 calc R . . C12 C 0.7138(8) 0.3264(8) 0.7825(3) 0.076(3) Uani 1 1 d . . . H12 H 0.6702 0.3782 0.7697 0.091 Uiso 1 1 calc R . . C13 C 0.7821(8) 0.3343(7) 0.8212(3) 0.069(2) Uani 1 1 d . . . H13 H 0.7855 0.3921 0.8353 0.083 Uiso 1 1 calc R . . C14 C 0.8491(6) 0.2598(6) 0.8416(2) 0.0529(18) Uani 1 1 d . . . C15 C 0.9205(7) 0.2754(6) 0.8855(2) 0.0583(19) Uani 1 1 d . . . H15A H 0.9584 0.2166 0.8965 0.070 Uiso 1 1 calc R . . H15B H 0.9867 0.3201 0.8837 0.070 Uiso 1 1 calc R . . C16 C 0.7461(6) 0.2649(5) 0.9243(2) 0.0464(15) Uani 1 1 d . . . C17 C 0.8631(11) 0.3918(6) 0.9361(3) 0.087(3) Uani 1 1 d . . . H17 H 0.9267 0.4345 0.9344 0.104 Uiso 1 1 calc R . . C18 C 0.7734(10) 0.4009(6) 0.9600(3) 0.084(3) Uani 1 1 d . . . H18 H 0.7622 0.4506 0.9784 0.100 Uiso 1 1 calc R . . C19 C 0.5983(7) 0.2967(5) 0.9715(2) 0.0510(16) Uani 1 1 d . . . H19A H 0.5510 0.3531 0.9752 0.061 Uiso 1 1 calc R . . H19B H 0.5450 0.2548 0.9522 0.061 Uiso 1 1 calc R . . C20 C 0.6409(6) 0.1585(4) 1.01572(17) 0.0359(12) Uani 1 1 d . . . C21 C 0.6633(7) 0.2952(5) 1.0509(2) 0.0560(18) Uani 1 1 d . . . H21 H 0.6643 0.3596 1.0562 0.067 Uiso 1 1 calc R . . C22 C 0.6929(7) 0.2293(5) 1.0797(2) 0.0550(18) Uani 1 1 d . . . H22 H 0.7177 0.2375 1.1095 0.066 Uiso 1 1 calc R . . C23 C 0.7029(6) 0.0543(4) 1.07681(19) 0.0438(15) Uani 1 1 d . . . H23A H 0.6307 0.0148 1.0680 0.053 Uiso 1 1 calc R . . H23B H 0.7157 0.0602 1.1082 0.053 Uiso 1 1 calc R . . C24 C 0.8151(6) 0.0081(5) 1.06346(16) 0.0405(14) Uani 1 1 d . . . C25 C 0.9262(6) 0.0566(5) 1.0729(2) 0.0500(17) Uani 1 1 d . . . H25 H 0.9283 0.1142 1.0871 0.060 Uiso 1 1 calc R . . C26 C 1.0321(7) 0.0219(7) 1.0617(2) 0.063(2) Uani 1 1 d . . . H26 H 1.1060 0.0557 1.0676 0.075 Uiso 1 1 calc R . . C27 C 1.0282(6) -0.0610(6) 1.0424(2) 0.0531(18) Uani 1 1 d . . . H27 H 1.1007 -0.0853 1.0347 0.064 Uiso 1 1 calc R . . C28 C 0.9242(7) -0.1106(5) 1.0335(2) 0.0509(17) Uani 1 1 d . . . H28 H 0.9253 -0.1690 1.0202 0.061 Uiso 1 1 calc R . . C29 C 0.8145(6) -0.0766(5) 1.04387(18) 0.0407(14) Uani 1 1 d . . . C30 C 0.7026(7) -0.1358(4) 1.0324(2) 0.0465(16) Uani 1 1 d . . . H30A H 0.7155 -0.1950 1.0479 0.056 Uiso 1 1 calc R . . H30B H 0.6326 -0.1044 1.0416 0.056 Uiso 1 1 calc R . . C31 C 0.4502(11) 0.2712(10) 0.8376(4) 0.122(5) Uani 1 1 d . . . H31A H 0.5362 0.2680 0.8347 0.183 Uiso 1 1 calc R . . H31B H 0.4410 0.3107 0.8618 0.183 Uiso 1 1 calc R . . H31C H 0.4030 0.2968 0.8115 0.183 Uiso 1 1 calc R . . C32 C 0.2432(9) 0.1832(9) 0.8409(4) 0.107(4) Uani 1 1 d . . . H32A H 0.2135 0.2067 0.8122 0.161 Uiso 1 1 calc R . . H32B H 0.2293 0.2295 0.8620 0.161 Uiso 1 1 calc R . . H32C H 0.1995 0.1265 0.8455 0.161 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 0.0525(3) 0.0338(3) 0.0259(2) -0.00108(15) 0.01368(19) 0.00307(16) Ag2 0.0450(3) 0.0487(3) 0.0292(2) 0.00385(17) 0.0121(2) 0.00181(17) S31 0.0681(15) 0.201(3) 0.0778(16) 0.080(2) -0.0004(13) -0.0064(17) P1 0.0714(13) 0.0341(9) 0.0809(14) -0.0074(9) 0.0161(11) 0.0046(8) P2 0.0504(10) 0.0593(10) 0.0294(7) -0.0061(7) 0.0117(7) -0.0050(7) F1 0.129(5) 0.098(4) 0.081(4) -0.005(3) 0.001(3) -0.022(4) F2 0.096(4) 0.076(3) 0.135(5) -0.032(3) 0.016(4) 0.025(3) F3 0.136(5) 0.085(4) 0.143(6) -0.008(4) 0.048(5) 0.039(4) F4 0.134(5) 0.103(5) 0.098(5) -0.040(4) 0.018(4) -0.012(4) F5 0.116(5) 0.091(4) 0.115(5) 0.033(4) -0.001(4) -0.026(3) F6 0.072(3) 0.207(8) 0.055(3) -0.012(4) -0.001(3) 0.031(4) F7 0.186(9) 0.243(12) 0.131(7) -0.105(8) -0.029(6) 0.122(8) F8 0.140(7) 0.365(18) 0.151(8) 0.134(10) 0.038(6) -0.054(9) F9 0.118(6) 0.313(15) 0.221(11) 0.194(11) 0.046(6) 0.007(7) F10 0.205(9) 0.258(13) 0.145(7) -0.142(9) -0.045(7) 0.098(9) F11 0.055(3) 0.354(13) 0.054(3) -0.030(5) -0.001(3) 0.010(5) F12 0.189(7) 0.090(4) 0.132(6) -0.010(4) 0.074(5) -0.067(5) O31 0.037(3) 0.044(3) 0.031(2) 0.012(2) 0.019(2) 0.006(2) N1 0.055(3) 0.038(3) 0.040(3) 0.006(2) 0.019(2) 0.002(2) N2 0.051(3) 0.045(3) 0.034(3) -0.008(2) 0.019(2) -0.007(2) N3 0.045(3) 0.058(3) 0.028(2) -0.008(2) 0.011(2) 0.006(2) N4 0.039(3) 0.072(4) 0.026(2) -0.002(2) 0.021(2) 0.006(2) N5 0.069(4) 0.058(4) 0.039(3) 0.008(3) 0.018(3) -0.013(3) N6 0.087(4) 0.038(3) 0.044(3) 0.010(2) 0.030(3) 0.001(3) N7 0.065(3) 0.033(3) 0.042(3) -0.003(2) 0.022(3) 0.008(2) N8 0.056(3) 0.041(3) 0.029(2) 0.000(2) 0.017(2) 0.000(2) C1 0.049(3) 0.034(3) 0.033(3) 0.000(2) 0.016(3) 0.000(2) C2 0.093(6) 0.033(3) 0.062(4) -0.003(3) 0.029(4) 0.009(3) C3 0.080(5) 0.028(3) 0.066(5) -0.017(3) 0.027(4) 0.002(3) C4 0.037(3) 0.059(4) 0.036(3) -0.010(3) 0.013(3) -0.001(3) C5 0.041(3) 0.049(3) 0.028(3) -0.007(3) 0.014(2) -0.003(2) C6 0.065(5) 0.068(5) 0.039(3) -0.021(3) 0.019(3) 0.005(3) C7 0.045(4) 0.094(6) 0.037(3) -0.014(4) 0.013(3) 0.006(4) C8 0.036(3) 0.094(6) 0.032(3) 0.007(3) 0.017(3) -0.006(3) C9 0.048(4) 0.084(5) 0.031(3) 0.021(3) 0.017(3) -0.008(3) C10 0.068(5) 0.112(7) 0.026(3) 0.014(4) 0.018(3) -0.008(4) C11 0.065(5) 0.143(9) 0.032(3) 0.041(5) 0.002(4) -0.012(5) C12 0.081(6) 0.099(7) 0.049(4) 0.035(5) 0.016(4) 0.000(5) C13 0.071(5) 0.089(6) 0.051(4) 0.028(4) 0.019(4) 0.002(4) C14 0.047(4) 0.078(5) 0.037(3) 0.022(3) 0.017(3) -0.007(3) C15 0.058(4) 0.066(5) 0.052(4) 0.018(4) 0.013(3) -0.008(3) C16 0.060(4) 0.044(4) 0.035(3) 0.007(3) 0.008(3) -0.004(3) C17 0.128(9) 0.064(5) 0.076(6) 0.009(5) 0.039(6) -0.039(5) C18 0.134(8) 0.042(4) 0.084(6) -0.006(4) 0.041(6) -0.022(5) C19 0.069(4) 0.035(3) 0.053(4) 0.008(3) 0.021(3) 0.011(3) C20 0.053(3) 0.033(3) 0.026(3) -0.003(2) 0.018(3) -0.001(2) C21 0.082(5) 0.041(4) 0.050(4) -0.017(3) 0.026(4) -0.005(3) C22 0.077(5) 0.054(4) 0.034(3) -0.017(3) 0.013(3) -0.004(3) C23 0.063(4) 0.046(4) 0.025(3) 0.010(2) 0.018(3) 0.002(3) C24 0.052(4) 0.058(4) 0.014(2) 0.006(2) 0.013(2) -0.003(3) C25 0.055(4) 0.059(4) 0.033(3) 0.008(3) -0.001(3) -0.002(3) C26 0.046(4) 0.097(6) 0.044(4) 0.022(4) 0.002(3) 0.003(4) C27 0.040(4) 0.076(5) 0.044(4) 0.021(4) 0.010(3) 0.018(3) C28 0.063(4) 0.062(4) 0.031(3) 0.016(3) 0.017(3) 0.028(3) C29 0.049(3) 0.052(4) 0.024(2) 0.010(3) 0.015(3) 0.008(3) C30 0.071(4) 0.040(3) 0.033(3) 0.016(3) 0.021(3) 0.007(3) C31 0.107(8) 0.149(11) 0.104(8) 0.090(9) 0.003(7) -0.016(7) C32 0.059(6) 0.118(9) 0.140(11) 0.012(8) 0.002(6) -0.001(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C20 2.073(6) . ? Ag1 C1 2.082(6) . ? Ag1 Ag2 3.0331(6) . ? Ag2 C16 2.105(7) . ? Ag2 C5 2.109(6) . ? S31 O31A 1.46(2) . ? S31 O31 1.471(5) . ? S31 C32 1.727(10) . ? S31 C31 1.753(12) . ? P1 F12 1.539(6) . ? P1 F1 1.554(6) . ? P1 F3 1.563(6) . ? P1 F2 1.578(5) . ? P1 F4 1.595(7) . ? P1 F5 1.622(6) . ? P2 F9 1.515(8) . ? P2 F10 1.523(8) . ? P2 F8 1.524(8) . ? P2 F7 1.524(7) . ? P2 F11 1.552(6) . ? P2 F6 1.561(6) . ? N1 C1 1.351(8) . ? N1 C2 1.363(8) . ? N1 C30 1.489(8) . ? N2 C1 1.346(7) . ? N2 C3 1.373(8) . ? N2 C4 1.462(8) . ? N3 C5 1.367(8) . ? N3 C6 1.406(8) . ? N3 C4 1.410(8) . ? N4 C7 1.336(10) . ? N4 C5 1.337(8) . ? N4 C8 1.496(9) . ? N5 C16 1.356(9) . ? N5 C17 1.364(11) . ? N5 C15 1.450(10) . ? N6 C16 1.364(9) . ? N6 C18 1.409(10) . ? N6 C19 1.431(9) . ? N7 C21 1.378(8) . ? N7 C20 1.381(7) . ? N7 C19 1.425(8) . ? N8 C20 1.350(7) . ? N8 C22 1.406(8) . ? N8 C23 1.456(8) . ? C2 C3 1.334(11) . ? C6 C7 1.377(11) . ? C8 C9 1.498(11) . ? C9 C10 1.389(9) . ? C9 C14 1.420(11) . ? C10 C11 1.392(13) . ? C11 C12 1.386(14) . ? C12 C13 1.342(12) . ? C13 C14 1.409(11) . ? C14 C15 1.507(10) . ? C17 C18 1.362(14) . ? C21 C22 1.330(10) . ? C23 C24 1.539(9) . ? C24 C29 1.379(9) . ? C24 C25 1.412(9) . ? C25 C26 1.383(11) . ? C26 C27 1.349(12) . ? C27 C28 1.354(11) . ? C28 C29 1.408(9) . ? C29 C30 1.508(10) . ? 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 C20 Ag1 C1 157.3(2) . . ? C20 Ag1 Ag2 99.92(16) . . ? C1 Ag1 Ag2 98.18(17) . . ? C16 Ag2 C5 152.6(3) . . ? C16 Ag2 Ag1 97.13(18) . . ? C5 Ag2 Ag1 99.41(17) . . ? O31A S31 O31 128.7(9) . . ? O31A S31 C32 109.5(10) . . ? O31 S31 C32 112.9(5) . . ? O31A S31 C31 90.4(10) . . ? O31 S31 C31 109.4(5) . . ? C32 S31 C31 99.4(6) . . ? F12 P1 F1 92.8(4) . . ? F12 P1 F3 91.1(4) . . ? F1 P1 F3 94.0(4) . . ? F12 P1 F2 91.8(4) . . ? F1 P1 F2 89.9(4) . . ? F3 P1 F2 175.0(4) . . ? F12 P1 F4 87.9(4) . . ? F1 P1 F4 178.2(4) . . ? F3 P1 F4 87.6(4) . . ? F2 P1 F4 88.4(4) . . ? F12 P1 F5 177.8(4) . . ? F1 P1 F5 89.4(4) . . ? F3 P1 F5 88.5(4) . . ? F2 P1 F5 88.4(4) . . ? F4 P1 F5 89.9(4) . . ? F9 P2 F10 79.4(8) . . ? F9 P2 F8 171.9(10) . . ? F10 P2 F8 108.7(9) . . ? F9 P2 F7 97.5(9) . . ? F10 P2 F7 176.5(9) . . ? F8 P2 F7 74.4(7) . . ? F9 P2 F11 89.8(5) . . ? F10 P2 F11 91.7(5) . . ? F8 P2 F11 90.1(5) . . ? F7 P2 F11 89.8(5) . . ? F9 P2 F6 90.7(5) . . ? F10 P2 F6 88.2(4) . . ? F8 P2 F6 89.4(5) . . ? F7 P2 F6 90.3(4) . . ? F11 P2 F6 179.4(5) . . ? C1 N1 C2 110.1(6) . . ? C1 N1 C30 124.2(5) . . ? C2 N1 C30 125.7(6) . . ? C1 N2 C3 111.4(6) . . ? C1 N2 C4 123.7(5) . . ? C3 N2 C4 124.8(6) . . ? C5 N3 C6 109.4(6) . . ? C5 N3 C4 124.2(5) . . ? C6 N3 C4 126.3(6) . . ? C7 N4 C5 113.6(6) . . ? C7 N4 C8 123.7(6) . . ? C5 N4 C8 122.7(6) . . ? C16 N5 C17 111.7(7) . . ? C16 N5 C15 123.8(6) . . ? C17 N5 C15 124.4(7) . . ? C16 N6 C18 110.1(7) . . ? C16 N6 C19 122.7(6) . . ? C18 N6 C19 127.0(7) . . ? C21 N7 C20 110.9(5) . . ? C21 N7 C19 127.2(6) . . ? C20 N7 C19 121.8(5) . . ? C20 N8 C22 111.0(5) . . ? C20 N8 C23 123.4(5) . . ? C22 N8 C23 125.6(5) . . ? N2 C1 N1 104.5(5) . . ? N2 C1 Ag1 136.2(5) . . ? N1 C1 Ag1 119.2(4) . . ? C3 C2 N1 108.3(6) . . ? C2 C3 N2 105.6(6) . . ? N3 C4 N2 112.0(5) . . ? N4 C5 N3 104.7(5) . . ? N4 C5 Ag2 122.5(5) . . ? N3 C5 Ag2 132.7(4) . . ? C7 C6 N3 105.8(7) . . ? N4 C7 C6 106.5(6) . . ? N4 C8 C9 112.2(5) . . ? C10 C9 C14 118.7(7) . . ? C10 C9 C8 117.2(8) . . ? C14 C9 C8 124.1(6) . . ? C9 C10 C11 120.9(9) . . ? C12 C11 C10 119.9(7) . . ? C13 C12 C11 120.0(9) . . ? C12 C13 C14 122.3(10) . . ? C13 C14 C9 118.1(7) . . ? C13 C14 C15 118.1(8) . . ? C9 C14 C15 123.8(6) . . ? N5 C15 C14 112.1(6) . . ? N5 C16 N6 104.9(6) . . ? N5 C16 Ag2 120.4(5) . . ? N6 C16 Ag2 134.7(5) . . ? C18 C17 N5 107.4(8) . . ? C17 C18 N6 105.9(8) . . ? N7 C19 N6 113.6(6) . . ? N8 C20 N7 103.9(5) . . ? N8 C20 Ag1 119.5(4) . . ? N7 C20 Ag1 136.5(4) . . ? C22 C21 N7 107.6(6) . . ? C21 C22 N8 106.7(6) . . ? N8 C23 C24 111.7(5) . . ? C29 C24 C25 118.6(6) . . ? C29 C24 C23 124.7(6) . . ? C25 C24 C23 116.7(6) . . ? C26 C25 C24 121.4(7) . . ? C27 C26 C25 118.6(8) . . ? C26 C27 C28 122.1(7) . . ? C27 C28 C29 120.8(7) . . ? C24 C29 C28 118.6(6) . . ? C24 C29 C30 124.0(6) . . ? C28 C29 C30 117.4(6) . . ? N1 C30 C29 112.6(5) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 72.63 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 1.910 _refine_diff_density_min -1.594 _refine_diff_density_rms 0.155 data_sad4 _database_code_depnum_ccdc_archive 'CCDC 913594' #TrackingRef '[Au2(1)](PF6)2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H34 Au2 F12 N10 P2' _chemical_formula_weight 1266.58 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.2635(5) _cell_length_b 21.8591(8) _cell_length_c 26.3883(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7650.7(5) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4832 _exptl_absorpt_coefficient_mu 7.847 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5725 _exptl_absorpt_correction_T_max 0.7987 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.765594 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61109 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0478 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 30.00 _reflns_number_total 11076 _reflns_number_gt 7598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+6.4426P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11076 _refine_ls_number_parameters 543 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 Au1 Au 0.126842(15) 0.988773(8) 0.489632(8) 0.02100(5) Uani 1 1 d . . . Au2 Au 0.147583(15) 0.990380(8) 0.373628(8) 0.02235(6) Uani 1 1 d . . . C1 C 0.1162(4) 0.8972(2) 0.49823(19) 0.0203(11) Uani 1 1 d . . . C2 C 0.1512(4) 0.8075(2) 0.5346(2) 0.0263(12) Uani 1 1 d . . . H2 H 0.1792 0.7780 0.5571 0.032 Uiso 1 1 calc R . . C3 C 0.0908(4) 0.7956(2) 0.49551(19) 0.0241(11) Uani 1 1 d . . . H3 H 0.0668 0.7566 0.4852 0.029 Uiso 1 1 calc R . . C4 C 0.0145(4) 0.8604(2) 0.42591(19) 0.0230(11) Uani 1 1 d . . . H4A H -0.0157 0.9018 0.4257 0.028 Uiso 1 1 calc R . . H4B H -0.0410 0.8302 0.4241 0.028 Uiso 1 1 calc R . . C5 C 0.1314(4) 0.9005(2) 0.3609(2) 0.0244(11) Uani 1 1 d . . . C6 C 0.0947(4) 0.7996(2) 0.3558(2) 0.0271(12) Uani 1 1 d . . . H6 H 0.0668 0.7607 0.3634 0.033 Uiso 1 1 calc R . . C7 C 0.1571(4) 0.8131(2) 0.3176(2) 0.0284(12) Uani 1 1 d . . . H7 H 0.1816 0.7855 0.2927 0.034 Uiso 1 1 calc R . . C8 C 0.2460(4) 0.9088(2) 0.2859(2) 0.0275(12) Uani 1 1 d . . . H8A H 0.2788 0.8794 0.2626 0.033 Uiso 1 1 calc R . . H8B H 0.2997 0.9293 0.3056 0.033 Uiso 1 1 calc R . . C9 C 0.1902(4) 0.9561(2) 0.2551(2) 0.0271(12) Uani 1 1 d . . . C10 C 0.1141(5) 0.9346(3) 0.2221(2) 0.0352(14) Uani 1 1 d . . . H10 H 0.1008 0.8920 0.2205 0.042 Uiso 1 1 calc R . . C11 C 0.0584(5) 0.9737(3) 0.1920(2) 0.0379(14) Uani 1 1 d . . . H11 H 0.0068 0.9582 0.1706 0.045 Uiso 1 1 calc R . . C12 C 0.0785(5) 1.0353(3) 0.1932(2) 0.0402(15) Uani 1 1 d . . . H12 H 0.0401 1.0624 0.1728 0.048 Uiso 1 1 calc R . . C13 C 0.1540(5) 1.0583(3) 0.2239(2) 0.0352(14) Uani 1 1 d . . . H13 H 0.1687 1.1008 0.2235 0.042 Uiso 1 1 calc R . . C14 C 0.2085(4) 1.0197(2) 0.2554(2) 0.0290(12) Uani 1 1 d . . . C15 C 0.2890(4) 1.0497(2) 0.2886(2) 0.0282(12) Uani 1 1 d . . . H15A H 0.3250 1.0177 0.3080 0.034 Uiso 1 1 calc R . . H15B H 0.3387 1.0707 0.2667 0.034 Uiso 1 1 calc R . . C16 C 0.1850(4) 1.0792(2) 0.3633(2) 0.0243(11) Uani 1 1 d . . . C17 C 0.2552(5) 1.1573(2) 0.3214(2) 0.0319(14) Uani 1 1 d . . . H17 H 0.2928 1.1792 0.2967 0.038 Uiso 1 1 calc R . . C18 C 0.2028(4) 1.1816(2) 0.3597(2) 0.0287(12) Uani 1 1 d . . . H18 H 0.1973 1.2237 0.3681 0.034 Uiso 1 1 calc R . . C19 C 0.0967(4) 1.1368(2) 0.43015(18) 0.0218(11) Uani 1 1 d . . . H19A H 0.0443 1.1046 0.4294 0.026 Uiso 1 1 calc R . . H19B H 0.0624 1.1770 0.4308 0.026 Uiso 1 1 calc R . . C20 C 0.1741(4) 1.0760(2) 0.4992(2) 0.0248(12) Uani 1 1 d . . . C21 C 0.2145(4) 1.1755(2) 0.4976(2) 0.0266(12) Uani 1 1 d . . . H21 H 0.2158 1.2175 0.4883 0.032 Uiso 1 1 calc R . . C22 C 0.2680(4) 1.1492(2) 0.5348(2) 0.0265(12) Uani 1 1 d . . . H22 H 0.3147 1.1689 0.5567 0.032 Uiso 1 1 calc R . . C23 C 0.2873(4) 1.0410(2) 0.5693(2) 0.0305(13) Uani 1 1 d . . . H23A H 0.3408 1.0604 0.5900 0.037 Uiso 1 1 calc R . . H23B H 0.3192 1.0089 0.5483 0.037 Uiso 1 1 calc R . . C24 C 0.2122(4) 1.0120(2) 0.6038(2) 0.0257(11) Uani 1 1 d . . . C25 C 0.1642(4) 1.0503(2) 0.6391(2) 0.0288(12) Uani 1 1 d . . . H25 H 0.1808 1.0925 0.6396 0.035 Uiso 1 1 calc R . . C26 C 0.0942(4) 1.0285(3) 0.6730(2) 0.0333(13) Uani 1 1 d . . . H26 H 0.0619 1.0558 0.6958 0.040 Uiso 1 1 calc R . . C27 C 0.0709(4) 0.9670(3) 0.6737(2) 0.0319(13) Uani 1 1 d . . . H27 H 0.0228 0.9516 0.6972 0.038 Uiso 1 1 calc R . . C28 C 0.1184(4) 0.9275(3) 0.6396(2) 0.0308(13) Uani 1 1 d . . . H28 H 0.1028 0.8851 0.6405 0.037 Uiso 1 1 calc R . . C29 C 0.1886(4) 0.9490(2) 0.6043(2) 0.0239(11) Uani 1 1 d . . . C30 C 0.2385(4) 0.9020(2) 0.5705(2) 0.0272(12) Uani 1 1 d . . . H30A H 0.2900 0.9226 0.5494 0.033 Uiso 1 1 calc R . . H30B H 0.2734 0.8715 0.5919 0.033 Uiso 1 1 calc R . . N1 N 0.1662(3) 0.86982(18) 0.53683(16) 0.0229(9) Uani 1 1 d . . . N2 N 0.0696(3) 0.85164(17) 0.47260(16) 0.0207(9) Uani 1 1 d . . . N3 N 0.0789(3) 0.85352(18) 0.38197(16) 0.0223(9) Uani 1 1 d . . . N4 N 0.1796(3) 0.87493(18) 0.32098(17) 0.0240(9) Uani 1 1 d . . . N5 N 0.2448(3) 1.09433(18) 0.32422(17) 0.0254(10) Uani 1 1 d . . . N6 N 0.1577(3) 1.13247(18) 0.38515(16) 0.0227(9) Uani 1 1 d . . . N7 N 0.1572(3) 1.13002(18) 0.47552(16) 0.0215(9) Uani 1 1 d . . . N8 N 0.2424(3) 1.08814(18) 0.53524(17) 0.0244(10) Uani 1 1 d . . . P1 P 0.70202(12) 0.24170(7) 0.83075(6) 0.0312(3) Uani 1 1 d . . . F1 F 0.6227(3) 0.1901(2) 0.81615(18) 0.0660(13) Uani 1 1 d . . . F2 F 0.7830(3) 0.29071(19) 0.84612(16) 0.0667(13) Uani 1 1 d . . . F3 F 0.6195(3) 0.2918(2) 0.82470(19) 0.0742(14) Uani 1 1 d . . . F4 F 0.7334(4) 0.2481(2) 0.77381(16) 0.0851(17) Uani 1 1 d . . . F5 F 0.6701(3) 0.2346(2) 0.88849(16) 0.0724(14) Uani 1 1 d . . . F6 F 0.7849(3) 0.19015(19) 0.8383(2) 0.0856(17) Uani 1 1 d . . . P2 P 0.09482(12) 0.14911(7) 0.93565(6) 0.0328(4) Uani 1 1 d . . . F7 F 0.0952(4) 0.1755(2) 0.99132(17) 0.0782(15) Uani 1 1 d . . . F8 F 0.1575(4) 0.0925(2) 0.9535(2) 0.0858(16) Uani 1 1 d . . . F9 F 0.1969(4) 0.1838(2) 0.92555(19) 0.0819(16) Uani 1 1 d . . . F10 F 0.0337(4) 0.2075(2) 0.91826(19) 0.0904(18) Uani 1 1 d . . . F11 F 0.0952(4) 0.1242(2) 0.88026(18) 0.0857(16) Uani 1 1 d . . . F12 F -0.0058(3) 0.1141(2) 0.9455(2) 0.0951(19) Uani 1 1 d . . . N41 N 0.4587(5) 0.3385(3) 0.7402(3) 0.0655(19) Uani 1 1 d . . . C41 C 0.4837(5) 0.2924(3) 0.7261(3) 0.0435(16) Uani 1 1 d . . . C42 C 0.5126(6) 0.2321(3) 0.7078(3) 0.0533(19) Uani 1 1 d . . . H42A H 0.4980 0.2014 0.7340 0.080 Uiso 1 1 calc R . . H42B H 0.5849 0.2317 0.7001 0.080 Uiso 1 1 calc R . . H42C H 0.4743 0.2224 0.6771 0.080 Uiso 1 1 calc R . . N51 N 0.9296(6) 0.1594(3) 0.0862(3) 0.080(2) Uani 1 1 d . . . C51 C 0.9311(6) 0.1096(3) 0.0751(3) 0.0503(18) Uani 1 1 d . . . C52 C 0.9344(7) 0.0453(4) 0.0610(3) 0.066(2) Uani 1 1 d . . . H52A H 0.9441 0.0418 0.0243 0.099 Uiso 1 1 calc R . . H52B H 0.8708 0.0256 0.0705 0.099 Uiso 1 1 calc R . . H52C H 0.9904 0.0252 0.0785 0.099 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 Au1 0.02500(10) 0.01508(9) 0.02293(11) 0.00187(8) -0.00377(8) -0.00077(7) Au2 0.02807(11) 0.01568(9) 0.02330(11) -0.00110(8) 0.00389(8) -0.00171(7) C1 0.022(3) 0.018(2) 0.020(3) 0.0024(18) -0.002(2) -0.0006(19) C2 0.037(3) 0.018(2) 0.024(3) 0.002(2) 0.001(3) 0.005(2) C3 0.033(3) 0.018(2) 0.021(3) 0.0021(19) 0.001(2) 0.001(2) C4 0.023(3) 0.020(2) 0.027(3) 0.002(2) -0.005(2) -0.0036(19) C5 0.029(3) 0.019(2) 0.025(3) 0.001(2) 0.000(2) 0.0014(19) C6 0.036(3) 0.017(2) 0.028(3) 0.000(2) -0.005(3) -0.001(2) C7 0.036(3) 0.019(3) 0.030(3) -0.004(2) -0.003(3) 0.003(2) C8 0.032(3) 0.024(3) 0.027(3) -0.002(2) 0.009(2) 0.000(2) C9 0.029(3) 0.027(3) 0.026(3) -0.004(2) 0.010(2) 0.000(2) C10 0.049(4) 0.029(3) 0.027(3) -0.005(2) 0.007(3) -0.009(3) C11 0.041(4) 0.047(4) 0.026(3) -0.005(3) 0.000(3) 0.001(3) C12 0.043(4) 0.046(4) 0.031(4) 0.007(3) -0.001(3) 0.012(3) C13 0.047(4) 0.026(3) 0.032(3) 0.006(2) 0.006(3) 0.002(2) C14 0.035(3) 0.023(3) 0.029(3) -0.001(2) 0.006(3) -0.001(2) C15 0.034(3) 0.023(3) 0.028(3) -0.002(2) 0.012(3) -0.004(2) C16 0.023(3) 0.025(3) 0.024(3) -0.001(2) -0.002(2) -0.001(2) C17 0.045(4) 0.019(3) 0.032(3) 0.003(2) 0.007(3) -0.011(2) C18 0.044(3) 0.016(2) 0.026(3) 0.004(2) -0.002(3) -0.003(2) C19 0.025(3) 0.019(2) 0.021(3) 0.003(2) 0.002(2) -0.0025(19) C20 0.029(3) 0.022(3) 0.024(3) -0.002(2) -0.001(2) 0.001(2) C21 0.034(3) 0.016(2) 0.030(3) -0.001(2) -0.001(2) -0.005(2) C22 0.034(3) 0.019(2) 0.027(3) 0.000(2) -0.004(3) -0.007(2) C23 0.029(3) 0.025(3) 0.037(3) 0.008(2) -0.009(3) -0.001(2) C24 0.029(3) 0.024(2) 0.024(3) 0.001(2) -0.005(2) -0.003(2) C25 0.040(3) 0.020(2) 0.026(3) 0.001(2) -0.013(3) 0.002(2) C26 0.037(3) 0.042(3) 0.021(3) -0.003(2) -0.003(3) 0.012(3) C27 0.027(3) 0.044(3) 0.025(3) 0.007(3) -0.006(3) 0.002(2) C28 0.041(3) 0.029(3) 0.023(3) 0.003(2) -0.010(3) -0.005(2) C29 0.024(3) 0.026(3) 0.021(3) 0.002(2) -0.007(2) 0.001(2) C30 0.030(3) 0.026(3) 0.025(3) 0.006(2) -0.006(2) 0.005(2) N1 0.027(2) 0.018(2) 0.024(2) 0.0017(17) -0.002(2) 0.0043(17) N2 0.025(2) 0.0135(18) 0.024(2) 0.0020(16) -0.0007(19) -0.0006(16) N3 0.025(2) 0.019(2) 0.023(2) 0.0029(17) -0.0039(19) -0.0006(16) N4 0.029(2) 0.018(2) 0.024(2) 0.0005(17) 0.004(2) 0.0025(17) N5 0.030(2) 0.019(2) 0.028(3) -0.0002(18) 0.005(2) -0.0048(17) N6 0.030(2) 0.0158(19) 0.023(2) 0.0011(16) 0.002(2) -0.0001(16) N7 0.030(2) 0.0159(19) 0.018(2) 0.0011(16) -0.0001(19) 0.0008(16) N8 0.029(2) 0.020(2) 0.024(3) 0.0027(17) -0.005(2) -0.0033(17) P1 0.0394(9) 0.0259(7) 0.0282(9) -0.0001(6) 0.0024(7) -0.0042(6) F1 0.052(3) 0.055(3) 0.091(4) -0.011(2) -0.009(2) -0.019(2) F2 0.082(3) 0.062(3) 0.057(3) -0.020(2) 0.017(2) -0.041(2) F3 0.080(3) 0.049(3) 0.094(4) 0.016(2) 0.002(3) 0.027(2) F4 0.110(4) 0.119(4) 0.027(2) -0.014(2) 0.022(3) -0.037(3) F5 0.065(3) 0.114(4) 0.038(3) 0.029(2) 0.003(2) -0.018(3) F6 0.047(3) 0.045(3) 0.165(5) 0.004(3) 0.011(3) 0.006(2) P2 0.0293(8) 0.0285(7) 0.0406(10) 0.0008(7) 0.0007(7) 0.0012(6) F7 0.085(4) 0.100(4) 0.049(3) -0.018(3) 0.010(3) 0.005(3) F8 0.079(3) 0.062(3) 0.116(4) 0.006(3) -0.034(3) 0.022(3) F9 0.065(3) 0.087(4) 0.093(4) -0.009(3) 0.021(3) -0.034(3) F10 0.126(5) 0.061(3) 0.084(4) 0.000(3) -0.016(3) 0.049(3) F11 0.096(4) 0.104(4) 0.057(3) -0.035(3) -0.015(3) 0.012(3) F12 0.043(3) 0.096(4) 0.146(5) -0.009(4) 0.012(3) -0.026(3) N41 0.072(5) 0.050(4) 0.075(5) -0.004(4) -0.008(4) 0.010(3) C41 0.039(4) 0.048(4) 0.043(4) 0.005(3) -0.005(3) -0.007(3) C42 0.054(5) 0.058(4) 0.048(5) -0.007(4) 0.002(4) -0.007(3) N51 0.108(7) 0.054(5) 0.078(5) -0.007(4) 0.018(5) 0.008(4) C51 0.059(5) 0.047(4) 0.045(5) -0.003(3) -0.001(4) 0.010(3) C52 0.082(6) 0.055(5) 0.062(6) -0.009(4) -0.009(5) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.019(5) . ? Au1 C20 2.023(5) . ? Au1 Au2 3.0737(3) . ? Au2 C5 2.005(5) . ? Au2 C16 2.023(5) . ? C1 N2 1.354(6) . ? C1 N1 1.355(6) . ? C2 C3 1.332(7) . ? C2 N1 1.379(6) . ? C3 N2 1.394(6) . ? C4 N2 1.445(6) . ? C4 N3 1.448(7) . ? C5 N4 1.354(6) . ? C5 N3 1.359(6) . ? C6 C7 1.337(8) . ? C6 N3 1.382(6) . ? C7 N4 1.386(6) . ? C8 N4 1.478(6) . ? C8 C9 1.508(7) . ? C9 C14 1.412(7) . ? C9 C10 1.414(8) . ? C10 C11 1.381(8) . ? C11 C12 1.371(9) . ? C12 C13 1.383(9) . ? C13 C14 1.387(8) . ? C14 C15 1.530(8) . ? C15 N5 1.475(6) . ? C16 N5 1.342(7) . ? C16 N6 1.349(6) . ? C17 C18 1.337(8) . ? C17 N5 1.385(6) . ? C18 N6 1.400(6) . ? C19 N6 1.440(6) . ? C19 N7 1.448(6) . ? C20 N8 1.339(7) . ? C20 N7 1.355(6) . ? C21 C22 1.341(7) . ? C21 N7 1.382(6) . ? C22 N8 1.377(6) . ? C23 N8 1.490(6) . ? C23 C24 1.491(8) . ? C24 C25 1.405(8) . ? C24 C29 1.413(7) . ? C25 C26 1.374(8) . ? C26 C27 1.381(8) . ? C27 C28 1.397(8) . ? C28 C29 1.397(8) . ? C29 C30 1.513(7) . ? C30 N1 1.485(7) . ? P1 F3 1.557(4) . ? P1 F4 1.565(4) . ? P1 F2 1.570(4) . ? P1 F6 1.586(4) . ? P1 F5 1.589(4) . ? P1 F1 1.590(4) . ? P2 F11 1.560(5) . ? P2 F12 1.561(5) . ? P2 F8 1.563(5) . ? P2 F9 1.575(5) . ? P2 F7 1.578(5) . ? P2 F10 1.580(4) . ? N41 C41 1.123(8) . ? C41 C42 1.456(9) . ? N51 C51 1.128(9) . ? C51 C52 1.454(10) . ? 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 C1 Au1 C20 160.4(2) . . ? C1 Au1 Au2 97.44(14) . . ? C20 Au1 Au2 94.93(15) . . ? C5 Au2 C16 160.8(2) . . ? C5 Au2 Au1 98.37(15) . . ? C16 Au2 Au1 99.64(15) . . ? N2 C1 N1 105.9(4) . . ? N2 C1 Au1 134.9(4) . . ? N1 C1 Au1 119.2(4) . . ? C3 C2 N1 108.1(4) . . ? C2 C3 N2 106.7(4) . . ? N2 C4 N3 111.8(4) . . ? N4 C5 N3 104.4(4) . . ? N4 C5 Au2 118.9(4) . . ? N3 C5 Au2 136.6(4) . . ? C7 C6 N3 106.4(4) . . ? C6 C7 N4 107.4(5) . . ? N4 C8 C9 112.8(4) . . ? C14 C9 C10 116.9(5) . . ? C14 C9 C8 126.0(5) . . ? C10 C9 C8 117.1(5) . . ? C11 C10 C9 122.1(5) . . ? C12 C11 C10 119.3(6) . . ? C11 C12 C13 120.8(6) . . ? C12 C13 C14 120.5(5) . . ? C13 C14 C9 120.4(5) . . ? C13 C14 C15 116.5(5) . . ? C9 C14 C15 123.1(5) . . ? N5 C15 C14 111.8(4) . . ? N5 C16 N6 106.0(4) . . ? N5 C16 Au2 119.0(4) . . ? N6 C16 Au2 134.8(4) . . ? C18 C17 N5 107.6(5) . . ? C17 C18 N6 106.2(4) . . ? N6 C19 N7 111.4(4) . . ? N8 C20 N7 105.5(4) . . ? N8 C20 Au1 119.0(4) . . ? N7 C20 Au1 135.4(4) . . ? C22 C21 N7 106.9(4) . . ? C21 C22 N8 106.9(5) . . ? N8 C23 C24 113.3(5) . . ? C25 C24 C29 118.2(5) . . ? C25 C24 C23 117.0(5) . . ? C29 C24 C23 124.8(5) . . ? C26 C25 C24 122.2(5) . . ? C25 C26 C27 119.8(5) . . ? C26 C27 C28 119.5(6) . . ? C27 C28 C29 121.4(5) . . ? C28 C29 C24 118.9(5) . . ? C28 C29 C30 117.2(5) . . ? C24 C29 C30 123.9(5) . . ? N1 C30 C29 113.1(4) . . ? C1 N1 C2 109.6(4) . . ? C1 N1 C30 123.8(4) . . ? C2 N1 C30 125.9(4) . . ? C1 N2 C3 109.7(4) . . ? C1 N2 C4 124.0(4) . . ? C3 N2 C4 126.0(4) . . ? C5 N3 C6 111.2(4) . . ? C5 N3 C4 123.4(4) . . ? C6 N3 C4 125.3(4) . . ? C5 N4 C7 110.5(4) . . ? C5 N4 C8 124.3(4) . . ? C7 N4 C8 125.2(4) . . ? C16 N5 C17 110.2(4) . . ? C16 N5 C15 124.1(4) . . ? C17 N5 C15 125.7(4) . . ? C16 N6 C18 110.0(4) . . ? C16 N6 C19 124.1(4) . . ? C18 N6 C19 125.7(4) . . ? C20 N7 C21 109.9(4) . . ? C20 N7 C19 124.3(4) . . ? C21 N7 C19 125.4(4) . . ? C20 N8 C22 110.7(4) . . ? C20 N8 C23 124.1(4) . . ? C22 N8 C23 125.1(4) . . ? F3 P1 F4 91.5(3) . . ? F3 P1 F2 91.5(3) . . ? F4 P1 F2 90.3(2) . . ? F3 P1 F6 178.5(3) . . ? F4 P1 F6 90.0(3) . . ? F2 P1 F6 88.8(3) . . ? F3 P1 F5 88.8(3) . . ? F4 P1 F5 179.5(3) . . ? F2 P1 F5 90.1(2) . . ? F6 P1 F5 89.7(3) . . ? F3 P1 F1 90.5(3) . . ? F4 P1 F1 90.4(3) . . ? F2 P1 F1 177.8(3) . . ? F6 P1 F1 89.1(2) . . ? F5 P1 F1 89.2(3) . . ? F11 P2 F12 89.3(3) . . ? F11 P2 F8 90.3(3) . . ? F12 P2 F8 90.9(3) . . ? F11 P2 F9 90.4(3) . . ? F12 P2 F9 179.4(3) . . ? F8 P2 F9 88.6(3) . . ? F11 P2 F7 178.9(3) . . ? F12 P2 F7 91.6(3) . . ? F8 P2 F7 90.4(3) . . ? F9 P2 F7 88.8(3) . . ? F11 P2 F10 90.6(3) . . ? F12 P2 F10 90.3(3) . . ? F8 P2 F10 178.5(3) . . ? F9 P2 F10 90.2(3) . . ? F7 P2 F10 88.7(3) . . ? N41 C41 C42 178.1(8) . . ? N51 C51 C52 179.4(10) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.155 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.183 data_sad3 _database_code_depnum_ccdc_archive 'CCDC 913595' #TrackingRef '[Au(H2-1)](PF6)3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 Au F18 N8 P3' _chemical_formula_weight 1134.50 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 '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 10.0766(4) _cell_length_b 13.1939(5) _cell_length_c 15.1674(6) _cell_angle_alpha 108.1110(10) _cell_angle_beta 90.9680(10) _cell_angle_gamma 101.2730(10) _cell_volume 1873.08(13) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 22.5 _exptl_crystal_description 'transparent plate' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.012 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 4.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7874 _exptl_absorpt_correction_T_max 0.9210 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.794862 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22256 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10852 _reflns_number_gt 9172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2(Bruker AXS, 2007)' _computing_cell_refinement 'APEX2(Bruker AXS, 2007)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2007 )' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10852 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Au1 Au 0.370143(13) 0.335318(11) 0.262165(9) 0.01592(4) Uani 1 1 d . . . C1 C 0.1836(3) 0.2567(3) 0.1984(2) 0.0177(7) Uani 1 1 d . . . C2 C -0.0145(4) 0.1341(3) 0.1609(3) 0.0250(8) Uani 1 1 d . . . H2 H -0.0847 0.0743 0.1607 0.030 Uiso 1 1 calc R . . C3 C -0.0152(4) 0.1996(3) 0.1088(3) 0.0251(8) Uani 1 1 d . . . H3 H -0.0853 0.1949 0.0642 0.030 Uiso 1 1 calc R . . C4 C 0.1481(4) 0.3527(3) 0.0812(2) 0.0195(7) Uani 1 1 d . . . H4A H 0.2049 0.3218 0.0313 0.023 Uiso 1 1 calc R . . H4B H 0.0664 0.3642 0.0516 0.023 Uiso 1 1 calc R . . C5 C 0.3588(4) 0.4890(3) 0.1467(2) 0.0187(7) Uani 1 1 d . . . H5 H 0.4184 0.4495 0.1094 0.022 Uiso 1 1 calc R . . C6 C 0.1732(4) 0.5355(3) 0.2087(3) 0.0250(8) Uani 1 1 d . . . H6 H 0.0809 0.5331 0.2215 0.030 Uiso 1 1 calc R . . C7 C 0.2807(4) 0.6164(3) 0.2510(3) 0.0234(8) Uani 1 1 d . . . H7 H 0.2779 0.6823 0.2989 0.028 Uiso 1 1 calc R . . C8 C 0.5371(4) 0.6488(3) 0.2326(2) 0.0224(7) Uani 1 1 d . . . H8A H 0.5572 0.6880 0.1867 0.027 Uiso 1 1 calc R . . H8B H 0.5986 0.5971 0.2244 0.027 Uiso 1 1 calc R . . C9 C 0.5682(4) 0.7310(3) 0.3297(2) 0.0196(7) Uani 1 1 d . . . C10 C 0.6266(4) 0.8381(3) 0.3353(3) 0.0231(8) Uani 1 1 d . . . H10 H 0.6341 0.8575 0.2800 0.028 Uiso 1 1 calc R . . C11 C 0.6738(4) 0.9167(3) 0.4207(3) 0.0270(8) Uani 1 1 d . . . H11 H 0.7134 0.9893 0.4236 0.032 Uiso 1 1 calc R . . C12 C 0.6631(4) 0.8891(3) 0.5007(3) 0.0302(9) Uani 1 1 d . . . H12 H 0.6973 0.9421 0.5591 0.036 Uiso 1 1 calc R . . C13 C 0.6023(4) 0.7839(3) 0.4963(3) 0.0257(8) Uani 1 1 d . . . H13 H 0.5930 0.7662 0.5523 0.031 Uiso 1 1 calc R . . C14 C 0.5548(4) 0.7036(3) 0.4121(3) 0.0193(7) Uani 1 1 d . . . C15 C 0.4953(4) 0.5901(3) 0.4132(3) 0.0206(7) Uani 1 1 d . . . H15A H 0.4708 0.5935 0.4768 0.025 Uiso 1 1 calc R . . H15B H 0.4111 0.5603 0.3709 0.025 Uiso 1 1 calc R . . C16 C 0.5573(4) 0.4123(3) 0.3276(2) 0.0180(7) Uani 1 1 d . . . C17 C 0.7277(4) 0.5446(3) 0.4153(3) 0.0303(9) Uani 1 1 d . . . H17 H 0.7754 0.6137 0.4551 0.036 Uiso 1 1 calc R . . C18 C 0.7790(4) 0.4561(3) 0.3784(3) 0.0302(9) Uani 1 1 d . . . H18 H 0.8704 0.4500 0.3870 0.036 Uiso 1 1 calc R . . C19 C 0.6998(4) 0.2731(3) 0.2616(3) 0.0238(8) Uani 1 1 d . . . H19A H 0.7125 0.2812 0.1994 0.029 Uiso 1 1 calc R . . H19B H 0.7854 0.2600 0.2845 0.029 Uiso 1 1 calc R . . C20 C 0.4949(4) 0.1368(3) 0.1818(3) 0.0208(7) Uani 1 1 d . . . H20 H 0.4878 0.1622 0.1301 0.025 Uiso 1 1 calc R . . C21 C 0.5681(4) 0.1201(3) 0.3136(3) 0.0223(7) Uani 1 1 d . . . H21 H 0.6207 0.1327 0.3700 0.027 Uiso 1 1 calc R . . C22 C 0.4561(4) 0.0407(3) 0.2776(3) 0.0227(7) Uani 1 1 d . . . H22 H 0.4161 -0.0137 0.3037 0.027 Uiso 1 1 calc R . . C23 C 0.2892(4) -0.0137(3) 0.1337(2) 0.0218(7) Uani 1 1 d . . . H23A H 0.3163 -0.0734 0.0842 0.026 Uiso 1 1 calc R . . H23B H 0.2516 0.0323 0.1034 0.026 Uiso 1 1 calc R . . C24 C 0.1802(4) -0.0624(3) 0.1854(3) 0.0213(7) Uani 1 1 d . . . C25 C 0.1438(4) -0.1759(3) 0.1595(3) 0.0275(8) Uani 1 1 d . . . H25 H 0.1902 -0.2192 0.1133 0.033 Uiso 1 1 calc R . . C26 C 0.0400(4) -0.2262(3) 0.2011(3) 0.0325(9) Uani 1 1 d . . . H26 H 0.0140 -0.3035 0.1816 0.039 Uiso 1 1 calc R . . C27 C -0.0241(4) -0.1651(3) 0.2692(3) 0.0334(9) Uani 1 1 d . . . H27 H -0.0937 -0.1999 0.2979 0.040 Uiso 1 1 calc R . . C28 C 0.0117(4) -0.0511(3) 0.2972(3) 0.0267(8) Uani 1 1 d . . . H28 H -0.0328 -0.0089 0.3455 0.032 Uiso 1 1 calc R . . C29 C 0.1127(3) 0.0009(3) 0.2545(2) 0.0181(7) Uani 1 1 d . . . C30 C 0.1443(4) 0.1244(3) 0.2874(2) 0.0210(7) Uani 1 1 d . . . H30A H 0.0946 0.1510 0.3428 0.025 Uiso 1 1 calc R . . H30B H 0.2427 0.1513 0.3063 0.025 Uiso 1 1 calc R . . N1 N 0.1065(3) 0.1699(2) 0.2146(2) 0.0192(6) Uani 1 1 d . . . N2 N 0.1066(3) 0.2752(2) 0.1328(2) 0.0187(6) Uani 1 1 d . . . N3 N 0.2240(3) 0.4565(2) 0.1426(2) 0.0177(6) Uani 1 1 d . . . N4 N 0.3953(3) 0.5859(2) 0.2119(2) 0.0184(6) Uani 1 1 d . . . N5 N 0.5903(3) 0.5160(2) 0.3841(2) 0.0197(6) Uani 1 1 d . . . N6 N 0.6730(3) 0.3744(2) 0.3249(2) 0.0209(6) Uani 1 1 d . . . N7 N 0.5910(3) 0.1790(2) 0.2527(2) 0.0192(6) Uani 1 1 d . . . N8 N 0.4108(3) 0.0532(2) 0.19624(19) 0.0185(6) Uani 1 1 d . . . P1 P 0.65707(10) 0.86919(8) 0.07256(6) 0.02027(19) Uani 1 1 d . . . P2 P 0.24967(10) 0.57867(8) 0.93269(7) 0.0238(2) Uani 1 1 d . . . P3 P 0.09674(10) 0.73820(8) 0.49180(7) 0.0246(2) Uani 1 1 d . . . F1 F 0.7197(2) 0.78444(19) 0.10646(16) 0.0312(5) Uani 1 1 d . . . F2 F 0.5937(3) 0.9533(2) 0.03741(18) 0.0409(6) Uani 1 1 d . . . F3 F 0.5187(2) 0.83735(19) 0.11703(15) 0.0279(5) Uani 1 1 d . . . F4 F 0.7954(2) 0.9013(2) 0.02746(17) 0.0345(6) Uani 1 1 d . . . F5 F 0.6013(2) 0.7757(2) -0.02477(15) 0.0332(5) Uani 1 1 d . . . F6 F 0.7137(2) 0.96338(19) 0.16862(16) 0.0334(6) Uani 1 1 d . . . F7 F 0.2727(3) 0.7093(2) 0.95550(18) 0.0404(6) Uani 1 1 d . . . F8 F 0.2279(3) 0.4519(2) 0.9096(2) 0.0543(8) Uani 1 1 d . . . F9 F 0.3620(3) 0.5791(2) 0.85964(19) 0.0390(6) Uani 1 1 d . . . F10 F 0.1374(3) 0.5827(3) 1.0053(2) 0.0559(8) Uani 1 1 d . . . F11 F 0.3631(3) 0.5976(3) 1.0120(2) 0.0595(9) Uani 1 1 d . . . F12 F 0.1352(3) 0.5661(3) 0.8531(2) 0.0547(8) Uani 1 1 d . . . F13 F 0.1815(3) 0.8196(2) 0.4446(2) 0.0473(7) Uani 1 1 d . . . F14 F 0.0133(3) 0.6582(2) 0.5412(2) 0.0496(7) Uani 1 1 d . . . F15 F 0.0547(3) 0.6491(2) 0.39300(19) 0.0541(8) Uani 1 1 d . . . F16 F 0.1395(3) 0.8297(2) 0.59274(18) 0.0464(7) Uani 1 1 d . . . F17 F 0.2313(2) 0.6934(2) 0.5035(2) 0.0438(7) Uani 1 1 d . . . F18 F -0.0357(3) 0.7848(2) 0.48319(18) 0.0398(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01346(6) 0.01572(6) 0.01812(7) 0.00529(5) -0.00105(4) 0.00243(4) C1 0.0157(16) 0.0138(16) 0.0207(17) 0.0005(13) -0.0002(13) 0.0050(13) C2 0.0138(16) 0.0230(19) 0.036(2) 0.0078(16) 0.0006(15) 0.0012(14) C3 0.0142(17) 0.0245(19) 0.033(2) 0.0061(16) -0.0073(15) 0.0028(14) C4 0.0198(17) 0.0197(17) 0.0187(17) 0.0053(14) -0.0005(13) 0.0050(14) C5 0.0198(17) 0.0215(17) 0.0154(16) 0.0053(13) 0.0016(13) 0.0062(14) C6 0.0236(19) 0.0246(19) 0.027(2) 0.0043(16) 0.0041(15) 0.0118(15) C7 0.0233(18) 0.0210(18) 0.0248(19) 0.0035(15) 0.0024(15) 0.0083(15) C8 0.0230(18) 0.0180(17) 0.0214(18) 0.0042(14) 0.0038(14) -0.0033(14) C9 0.0196(17) 0.0197(17) 0.0180(17) 0.0042(14) 0.0039(13) 0.0036(14) C10 0.0275(19) 0.0188(17) 0.0241(19) 0.0092(15) 0.0057(15) 0.0031(15) C11 0.031(2) 0.0185(18) 0.028(2) 0.0040(15) 0.0037(16) 0.0024(15) C12 0.041(2) 0.0229(19) 0.0184(18) -0.0015(15) -0.0021(16) 0.0017(17) C13 0.033(2) 0.0247(19) 0.0170(17) 0.0049(15) 0.0025(15) 0.0037(16) C14 0.0173(16) 0.0161(16) 0.0244(18) 0.0072(14) 0.0032(14) 0.0024(13) C15 0.0227(18) 0.0184(17) 0.0207(17) 0.0072(14) 0.0023(14) 0.0028(14) C16 0.0191(17) 0.0192(17) 0.0193(17) 0.0113(14) 0.0027(13) 0.0038(13) C17 0.024(2) 0.026(2) 0.039(2) 0.0133(18) -0.0104(17) -0.0013(16) C18 0.0179(18) 0.028(2) 0.044(2) 0.0147(18) -0.0108(17) -0.0018(15) C19 0.0184(17) 0.0219(18) 0.033(2) 0.0115(16) 0.0046(15) 0.0036(14) C20 0.0242(18) 0.0201(17) 0.0211(17) 0.0070(14) 0.0064(14) 0.0108(14) C21 0.0246(19) 0.0219(18) 0.0227(18) 0.0083(15) 0.0021(14) 0.0086(15) C22 0.0255(19) 0.0234(18) 0.0211(18) 0.0079(15) 0.0043(14) 0.0080(15) C23 0.0205(18) 0.0258(19) 0.0169(17) 0.0033(14) 0.0008(13) 0.0055(14) C24 0.0202(17) 0.0227(18) 0.0208(18) 0.0068(14) -0.0013(14) 0.0050(14) C25 0.027(2) 0.0235(19) 0.031(2) 0.0037(16) 0.0010(16) 0.0104(16) C26 0.034(2) 0.0184(19) 0.044(3) 0.0117(18) -0.0071(19) 0.0023(16) C27 0.025(2) 0.031(2) 0.048(3) 0.020(2) 0.0045(18) 0.0030(17) C28 0.0246(19) 0.029(2) 0.032(2) 0.0151(17) 0.0061(16) 0.0099(16) C29 0.0170(16) 0.0175(16) 0.0216(17) 0.0087(14) 0.0012(13) 0.0040(13) C30 0.0211(18) 0.0212(18) 0.0215(18) 0.0070(14) 0.0034(14) 0.0059(14) N1 0.0169(14) 0.0172(14) 0.0226(15) 0.0050(12) 0.0004(11) 0.0039(11) N2 0.0174(14) 0.0160(14) 0.0209(15) 0.0032(12) -0.0025(11) 0.0041(11) N3 0.0200(14) 0.0155(14) 0.0188(14) 0.0064(11) 0.0004(11) 0.0049(11) N4 0.0208(15) 0.0165(14) 0.0168(14) 0.0050(11) 0.0013(11) 0.0020(11) N5 0.0188(15) 0.0187(15) 0.0225(15) 0.0095(12) -0.0029(12) 0.0015(12) N6 0.0152(14) 0.0216(15) 0.0275(16) 0.0114(13) -0.0011(12) 0.0023(12) N7 0.0184(14) 0.0192(15) 0.0226(15) 0.0086(12) 0.0034(12) 0.0066(12) N8 0.0213(15) 0.0184(14) 0.0146(14) 0.0023(11) 0.0023(11) 0.0062(12) P1 0.0219(5) 0.0216(5) 0.0184(4) 0.0068(4) 0.0039(4) 0.0062(4) P2 0.0205(5) 0.0257(5) 0.0258(5) 0.0087(4) 0.0031(4) 0.0055(4) P3 0.0190(5) 0.0256(5) 0.0264(5) 0.0051(4) 0.0000(4) 0.0039(4) F1 0.0358(13) 0.0371(14) 0.0285(12) 0.0153(10) 0.0048(10) 0.0178(11) F2 0.0564(17) 0.0424(15) 0.0423(15) 0.0270(13) 0.0195(13) 0.0300(13) F3 0.0205(11) 0.0341(13) 0.0285(12) 0.0099(10) 0.0052(9) 0.0047(10) F4 0.0323(13) 0.0381(14) 0.0330(13) 0.0118(11) 0.0159(10) 0.0051(11) F5 0.0352(13) 0.0384(14) 0.0205(11) -0.0002(10) -0.0011(10) 0.0111(11) F6 0.0328(13) 0.0305(13) 0.0258(12) -0.0005(10) 0.0061(10) -0.0037(10) F7 0.0547(17) 0.0297(13) 0.0405(15) 0.0129(11) 0.0099(12) 0.0142(12) F8 0.070(2) 0.0219(13) 0.069(2) 0.0127(13) 0.0242(16) 0.0065(13) F9 0.0337(14) 0.0422(15) 0.0520(16) 0.0230(13) 0.0225(12) 0.0187(12) F10 0.0568(19) 0.059(2) 0.0593(19) 0.0265(16) 0.0344(16) 0.0157(16) F11 0.061(2) 0.065(2) 0.0568(19) 0.0419(17) -0.0255(15) -0.0093(16) F12 0.0324(15) 0.071(2) 0.0542(18) 0.0189(16) -0.0147(13) -0.0016(14) F13 0.0425(16) 0.0495(17) 0.0544(18) 0.0295(15) 0.0077(13) -0.0011(13) F14 0.0306(14) 0.0581(19) 0.075(2) 0.0444(17) 0.0093(14) 0.0055(13) F15 0.0420(16) 0.0521(18) 0.0414(16) -0.0176(13) -0.0004(13) 0.0021(14) F16 0.0344(14) 0.0558(18) 0.0347(15) -0.0048(13) -0.0043(11) 0.0086(13) F17 0.0245(13) 0.0465(16) 0.0654(19) 0.0193(14) 0.0053(12) 0.0168(12) F18 0.0304(13) 0.0493(16) 0.0412(15) 0.0118(12) -0.0037(11) 0.0165(12) _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 Au1 C1 2.024(3) . ? Au1 C16 2.033(3) . ? C1 N1 1.346(4) . ? C1 N2 1.361(4) . ? C2 C3 1.341(5) . ? C2 N1 1.370(5) . ? C3 N2 1.383(4) . ? C4 N3 1.450(4) . ? C4 N2 1.475(4) . ? C5 N4 1.329(4) . ? C5 N3 1.336(4) . ? C6 C7 1.350(5) . ? C6 N3 1.389(4) . ? C7 N4 1.379(5) . ? C8 N4 1.480(4) . ? C8 C9 1.517(5) . ? C9 C10 1.395(5) . ? C9 C14 1.406(5) . ? C10 C11 1.389(5) . ? C11 C12 1.373(6) . ? C12 C13 1.384(5) . ? C13 C14 1.387(5) . ? C14 C15 1.506(5) . ? C15 N5 1.476(5) . ? C16 N5 1.341(4) . ? C16 N6 1.353(4) . ? C17 C18 1.336(6) . ? C17 N5 1.395(5) . ? C18 N6 1.392(5) . ? C19 N7 1.456(4) . ? C19 N6 1.460(5) . ? C20 N8 1.332(5) . ? C20 N7 1.336(5) . ? C21 C22 1.353(5) . ? C21 N7 1.376(4) . ? C22 N8 1.376(5) . ? C23 N8 1.483(4) . ? C23 C24 1.517(5) . ? C24 C25 1.396(5) . ? C24 C29 1.400(5) . ? C25 C26 1.393(6) . ? C26 C27 1.357(6) . ? C27 C28 1.400(6) . ? C28 C29 1.397(5) . ? C29 C30 1.514(5) . ? C30 N1 1.486(5) . ? P1 F1 1.592(2) . ? P1 F3 1.598(2) . ? P1 F2 1.599(3) . ? P1 F6 1.601(2) . ? P1 F4 1.604(2) . ? P1 F5 1.608(2) . ? P2 F8 1.568(3) . ? P2 F11 1.572(3) . ? P2 F10 1.590(3) . ? P2 F9 1.598(3) . ? P2 F12 1.603(3) . ? P2 F7 1.617(3) . ? P3 F15 1.580(3) . ? P3 F13 1.592(3) . ? P3 F18 1.594(3) . ? P3 F14 1.597(3) . ? P3 F17 1.609(3) . ? P3 F16 1.616(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 C16 178.92(14) . . ? N1 C1 N2 103.9(3) . . ? N1 C1 Au1 125.0(3) . . ? N2 C1 Au1 131.1(3) . . ? C3 C2 N1 107.0(3) . . ? C2 C3 N2 106.4(3) . . ? N3 C4 N2 111.1(3) . . ? N4 C5 N3 108.3(3) . . ? C7 C6 N3 106.5(3) . . ? C6 C7 N4 107.5(3) . . ? N4 C8 C9 114.6(3) . . ? C10 C9 C14 119.2(3) . . ? C10 C9 C8 116.4(3) . . ? C14 C9 C8 124.1(3) . . ? C11 C10 C9 120.9(3) . . ? C12 C11 C10 119.7(4) . . ? C11 C12 C13 119.9(4) . . ? C12 C13 C14 121.6(3) . . ? C13 C14 C9 118.7(3) . . ? C13 C14 C15 118.2(3) . . ? C9 C14 C15 123.1(3) . . ? N5 C15 C14 112.4(3) . . ? N5 C16 N6 105.2(3) . . ? N5 C16 Au1 125.2(3) . . ? N6 C16 Au1 129.6(3) . . ? C18 C17 N5 106.7(3) . . ? C17 C18 N6 106.9(3) . . ? N7 C19 N6 113.0(3) . . ? N8 C20 N7 108.2(3) . . ? C22 C21 N7 106.7(3) . . ? C21 C22 N8 107.4(3) . . ? N8 C23 C24 112.2(3) . . ? C25 C24 C29 119.5(3) . . ? C25 C24 C23 117.4(3) . . ? C29 C24 C23 123.1(3) . . ? C26 C25 C24 120.4(4) . . ? C27 C26 C25 120.3(4) . . ? C26 C27 C28 120.4(4) . . ? C29 C28 C27 120.2(4) . . ? C28 C29 C24 119.2(3) . . ? C28 C29 C30 117.2(3) . . ? C24 C29 C30 123.6(3) . . ? N1 C30 C29 112.6(3) . . ? C1 N1 C2 111.8(3) . . ? C1 N1 C30 123.7(3) . . ? C2 N1 C30 124.4(3) . . ? C1 N2 C3 110.9(3) . . ? C1 N2 C4 127.1(3) . . ? C3 N2 C4 121.4(3) . . ? C5 N3 C6 108.8(3) . . ? C5 N3 C4 124.0(3) . . ? C6 N3 C4 127.2(3) . . ? C5 N4 C7 108.9(3) . . ? C5 N4 C8 123.1(3) . . ? C7 N4 C8 128.0(3) . . ? C16 N5 C17 110.8(3) . . ? C16 N5 C15 125.6(3) . . ? C17 N5 C15 123.6(3) . . ? C16 N6 C18 110.4(3) . . ? C16 N6 C19 127.7(3) . . ? C18 N6 C19 120.7(3) . . ? C20 N7 C21 109.0(3) . . ? C20 N7 C19 123.8(3) . . ? C21 N7 C19 127.2(3) . . ? C20 N8 C22 108.6(3) . . ? C20 N8 C23 124.6(3) . . ? C22 N8 C23 126.8(3) . . ? F1 P1 F3 90.21(13) . . ? F1 P1 F2 179.37(15) . . ? F3 P1 F2 89.85(13) . . ? F1 P1 F6 90.49(14) . . ? F3 P1 F6 89.81(12) . . ? F2 P1 F6 90.14(15) . . ? F1 P1 F4 90.10(13) . . ? F3 P1 F4 179.65(15) . . ? F2 P1 F4 89.84(14) . . ? F6 P1 F4 90.35(13) . . ? F1 P1 F5 90.01(13) . . ? F3 P1 F5 90.88(13) . . ? F2 P1 F5 89.36(14) . . ? F6 P1 F5 179.14(15) . . ? F4 P1 F5 88.95(13) . . ? F8 P2 F11 90.96(18) . . ? F8 P2 F10 90.43(16) . . ? F11 P2 F10 90.38(18) . . ? F8 P2 F9 91.63(15) . . ? F11 P2 F9 90.24(17) . . ? F10 P2 F9 177.84(16) . . ? F8 P2 F12 91.98(18) . . ? F11 P2 F12 177.06(18) . . ? F10 P2 F12 89.64(18) . . ? F9 P2 F12 89.64(16) . . ? F8 P2 F7 179.40(16) . . ? F11 P2 F7 89.27(16) . . ? F10 P2 F7 90.13(15) . . ? F9 P2 F7 87.82(14) . . ? F12 P2 F7 87.79(16) . . ? F15 P3 F13 90.26(17) . . ? F15 P3 F18 90.33(16) . . ? F13 P3 F18 90.97(16) . . ? F15 P3 F14 90.92(18) . . ? F13 P3 F14 178.79(18) . . ? F18 P3 F14 89.29(15) . . ? F15 P3 F17 91.29(16) . . ? F13 P3 F17 89.27(15) . . ? F18 P3 F17 178.37(16) . . ? F14 P3 F17 90.44(15) . . ? F15 P3 F16 179.80(19) . . ? F13 P3 F16 89.64(16) . . ? F18 P3 F16 89.50(15) . . ? F14 P3 F16 89.18(17) . . ? F17 P3 F16 88.88(15) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.537 _refine_diff_density_min -0.754 _refine_diff_density_rms 0.147 data_sad5 _database_code_depnum_ccdc_archive 'CCDC 913596' #TrackingRef '[{Ag(H2-1)}2Ag2](PF6)4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H68 Ag4 F24 N20 P4' _chemical_formula_weight 2176.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 14.4717(4) _cell_length_b 25.3501(6) _cell_length_c 21.5532(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.799(2) _cell_angle_gamma 90.00 _cell_volume 7879.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 1 _cell_measurement_theta_max 75 _exptl_crystal_description 'transparent prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4320 _exptl_absorpt_coefficient_mu 9.640 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.4774 _exptl_absorpt_correction_T_max 0.5127 _exptl_absorpt_process_details ; Corrections were done with the SADABS program, utilizing the none merged raw data obtained from the integration process. Integration and final cell refinement were done with SAINT. SADABS reports ratio of Tmin/Tmax = 0.565312 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator goebel-mirror _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean 80 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22777 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0872 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 72.00 _reflns_number_total 7328 _reflns_number_gt 6260 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker AXS, 2000)' _computing_cell_refinement 'SAINT (Bruker AXS, 2000)' _computing_data_reduction 'SAINT,SADABS (Bruker AXS, 2000)' _computing_structure_solution ; SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_structure_refinement ; SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122 ; _computing_molecular_graphics ; ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565 ; _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+36.4273P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7328 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1263 _refine_ls_wR_factor_gt 0.1197 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _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 0.56979(2) 0.719631(11) 0.326203(15) 0.02032(11) Uani 1 1 d . . . Ag2 Ag 0.5000 0.597336(16) 0.2500 0.01996(13) Uani 1 2 d S . . Ag3 Ag 0.5000 0.845998(16) 0.2500 0.01901(13) Uani 1 2 d S . . C1 C 0.4591(3) 0.73872(16) 0.3810(2) 0.0192(8) Uani 1 1 d . . . C2 C 0.3794(4) 0.77099(19) 0.4586(2) 0.0319(11) Uani 1 1 d . . . H2 H 0.3615 0.7939 0.4904 0.038 Uiso 1 1 calc R . . C3 C 0.3393(4) 0.72438(18) 0.4409(2) 0.0305(11) Uani 1 1 d . . . H3 H 0.2881 0.7080 0.4578 0.037 Uiso 1 1 calc R . . C4 C 0.3697(3) 0.65530(16) 0.3624(2) 0.0234(9) Uani 1 1 d . . . H4A H 0.3068 0.6432 0.3704 0.028 Uiso 1 1 calc R . . H4B H 0.3716 0.6598 0.3169 0.028 Uiso 1 1 calc R . . C5 C 0.4975(3) 0.59265(16) 0.3475(2) 0.0201(9) Uani 1 1 d . . . C6 C 0.4493(4) 0.59855(19) 0.4449(2) 0.0303(11) Uani 1 1 d . . . H6 H 0.4149 0.6090 0.4785 0.036 Uiso 1 1 calc R . . C7 C 0.5196(4) 0.5637(2) 0.4472(2) 0.0328(11) Uani 1 1 d . . . H7 H 0.5454 0.5451 0.4828 0.039 Uiso 1 1 calc R . . C8 C 0.6216(3) 0.52372(19) 0.3727(2) 0.0304(11) Uani 1 1 d . . . H8A H 0.6009 0.4872 0.3802 0.036 Uiso 1 1 calc R . . H8B H 0.6769 0.5306 0.4018 0.036 Uiso 1 1 calc R . . C9 C 0.6497(3) 0.52713(16) 0.3074(2) 0.0234(9) Uani 1 1 d . . . C10 C 0.6222(3) 0.48759(17) 0.2653(2) 0.0295(10) Uani 1 1 d . . . H10 H 0.5841 0.4597 0.2779 0.035 Uiso 1 1 calc R . . C11 C 0.6495(3) 0.48808(18) 0.2053(3) 0.0322(11) Uani 1 1 d . . . H11 H 0.6279 0.4617 0.1763 0.039 Uiso 1 1 calc R . . C12 C 0.7083(3) 0.52729(19) 0.1879(2) 0.0307(11) Uani 1 1 d . . . H12 H 0.7294 0.5271 0.1473 0.037 Uiso 1 1 calc R . . C13 C 0.7366(3) 0.56708(17) 0.2297(2) 0.0235(9) Uani 1 1 d . . . H13 H 0.7772 0.5938 0.2172 0.028 Uiso 1 1 calc R . . C14 C 0.7067(3) 0.56851(17) 0.2890(2) 0.0242(9) Uani 1 1 d . . . C15 C 0.7356(3) 0.61263(17) 0.3341(2) 0.0244(9) Uani 1 1 d . . . H15A H 0.6848 0.6193 0.3610 0.029 Uiso 1 1 calc R . . H15B H 0.7905 0.6011 0.3611 0.029 Uiso 1 1 calc R . . C16 C 0.6973(3) 0.70165(16) 0.2893(2) 0.0185(8) Uani 1 1 d . . . C17 C 0.8423(3) 0.67060(18) 0.2788(2) 0.0265(10) Uani 1 1 d . . . H17 H 0.8951 0.6483 0.2831 0.032 Uiso 1 1 calc R . . C18 C 0.8349(3) 0.71661(17) 0.2480(2) 0.0259(10) Uani 1 1 d . . . H18 H 0.8813 0.7333 0.2263 0.031 Uiso 1 1 calc R . . C19 C 0.7117(3) 0.78525(16) 0.2294(2) 0.0204(9) Uani 1 1 d . . . H19A H 0.7509 0.7973 0.1967 0.024 Uiso 1 1 calc R . . H19B H 0.6476 0.7808 0.2102 0.024 Uiso 1 1 calc R . . C20 C 0.6351(3) 0.84893(16) 0.2956(2) 0.0196(9) Uani 1 1 d . . . C21 C 0.7908(3) 0.84005(17) 0.3144(2) 0.0236(9) Uani 1 1 d . . . H21 H 0.8526 0.8288 0.3104 0.028 Uiso 1 1 calc R . . C22 C 0.7627(3) 0.87385(17) 0.3562(2) 0.0226(9) Uani 1 1 d . . . H22 H 0.8006 0.8911 0.3881 0.027 Uiso 1 1 calc R . . C23 C 0.6149(3) 0.91586(17) 0.3808(2) 0.0248(10) Uani 1 1 d . . . H23A H 0.6367 0.9522 0.3737 0.030 Uiso 1 1 calc R . . H23B H 0.6288 0.9078 0.4256 0.030 Uiso 1 1 calc R . . C24 C 0.5110(3) 0.91388(17) 0.3656(2) 0.0216(9) Uani 1 1 d . . . C25 C 0.4685(3) 0.95540(18) 0.3314(2) 0.0264(10) Uani 1 1 d . . . H25 H 0.5052 0.9833 0.3173 0.032 Uiso 1 1 calc R . . C26 C 0.3730(3) 0.95598(19) 0.3180(2) 0.0314(11) Uani 1 1 d . . . H26 H 0.3444 0.9836 0.2936 0.038 Uiso 1 1 calc R . . C27 C 0.3199(3) 0.91621(19) 0.3404(2) 0.0289(10) Uani 1 1 d . . . H27 H 0.2543 0.9171 0.3325 0.035 Uiso 1 1 calc R . . C28 C 0.3614(3) 0.87522(17) 0.3742(2) 0.0246(9) Uani 1 1 d . . . H28 H 0.3239 0.8481 0.3893 0.029 Uiso 1 1 calc R . . C29 C 0.4575(3) 0.87276(16) 0.3865(2) 0.0218(9) Uani 1 1 d . . . C30 C 0.5060(3) 0.82744(16) 0.4230(2) 0.0221(9) Uani 1 1 d . . . H30A H 0.5659 0.8201 0.4055 0.027 Uiso 1 1 calc R . . H30B H 0.5196 0.8385 0.4668 0.027 Uiso 1 1 calc R . . C41 C 0.2726(5) 0.9914(2) 1.0091(3) 0.0435(14) Uani 1 1 d . . . C42 C 0.3597(6) 0.9951(3) 0.9788(3) 0.0637(19) Uani 1 1 d . . . H42A H 0.4102 1.0052 1.0096 0.096 Uiso 1 1 calc R . . H42B H 0.3532 1.0216 0.9457 0.096 Uiso 1 1 calc R . . H42C H 0.3736 0.9607 0.9608 0.096 Uiso 1 1 calc R . . C51 C 0.6878(4) 0.1977(3) 0.0384(3) 0.0458(14) Uani 1 1 d . . . C52 C 0.6446(5) 0.2437(3) 0.0639(4) 0.0599(18) Uani 1 1 d . . . H52A H 0.5974 0.2578 0.0330 0.090 Uiso 1 1 calc R . . H52B H 0.6918 0.2707 0.0743 0.090 Uiso 1 1 calc R . . H52C H 0.6155 0.2336 0.1015 0.090 Uiso 1 1 calc R . . N1 N 0.4510(3) 0.77867(13) 0.42142(18) 0.0219(8) Uani 1 1 d . . . N2 N 0.3884(2) 0.70569(14) 0.39317(17) 0.0210(7) Uani 1 1 d . . . N3 N 0.4366(3) 0.61620(14) 0.38431(17) 0.0230(8) Uani 1 1 d . . . N4 N 0.5470(3) 0.56049(14) 0.38742(18) 0.0250(8) Uani 1 1 d . . . N5 N 0.7578(2) 0.66187(14) 0.30324(17) 0.0217(8) Uani 1 1 d . . . N6 N 0.7462(2) 0.73470(14) 0.25431(17) 0.0204(7) Uani 1 1 d . . . N7 N 0.7125(2) 0.82453(13) 0.27806(17) 0.0199(7) Uani 1 1 d . . . N8 N 0.6675(2) 0.87904(13) 0.34413(17) 0.0203(7) Uani 1 1 d . . . N41 N 0.2066(4) 0.9871(2) 1.0329(3) 0.0578(15) Uani 1 1 d . . . N51 N 0.7201(4) 0.1610(2) 0.0183(3) 0.0649(16) Uani 1 1 d . . . P1 P 0.93127(8) 0.84036(5) 0.12463(6) 0.0284(3) Uani 1 1 d . . . P2 P 0.43805(9) 0.11218(5) 0.10229(6) 0.0321(3) Uani 1 1 d . . . F1 F 0.8818(2) 0.85564(13) 0.18558(15) 0.0436(7) Uani 1 1 d . . . F2 F 0.8517(2) 0.79752(15) 0.10920(17) 0.0543(9) Uani 1 1 d . . . F3 F 0.9920(2) 0.79732(12) 0.16334(15) 0.0420(7) Uani 1 1 d . . . F4 F 0.8699(2) 0.88371(15) 0.08596(16) 0.0540(9) Uani 1 1 d . . . F5 F 0.9783(3) 0.82446(15) 0.06367(17) 0.0576(10) Uani 1 1 d . . . F6 F 1.0089(2) 0.88345(13) 0.1415(2) 0.0590(10) Uani 1 1 d . . . F7 F 0.3958(3) 0.05605(16) 0.11002(18) 0.0766(13) Uani 1 1 d . . . F8 F 0.4446(4) 0.1196(2) 0.1743(2) 0.108(2) Uani 1 1 d . . . F9 F 0.5380(3) 0.0894(3) 0.1126(3) 0.117(2) Uani 1 1 d . . . F10 F 0.4332(5) 0.1049(3) 0.0310(2) 0.137(3) Uani 1 1 d . . . F11 F 0.3410(4) 0.1348(3) 0.0966(5) 0.183(4) Uani 1 1 d . . . F12 F 0.4838(4) 0.16755(18) 0.0931(3) 0.1051(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.01624(18) 0.01736(18) 0.02862(19) -0.00032(12) 0.00926(14) 0.00020(10) Ag2 0.0204(2) 0.0181(2) 0.0219(2) 0.000 0.00536(18) 0.000 Ag3 0.0119(2) 0.0179(2) 0.0272(2) 0.000 0.00132(18) 0.000 C1 0.015(2) 0.017(2) 0.027(2) 0.0022(18) 0.0074(17) 0.0020(15) C2 0.038(3) 0.025(2) 0.036(3) -0.006(2) 0.020(2) -0.0044(19) C3 0.029(3) 0.025(3) 0.041(3) -0.005(2) 0.021(2) -0.0032(18) C4 0.022(2) 0.016(2) 0.033(2) -0.0047(18) 0.007(2) -0.0038(16) C5 0.022(2) 0.014(2) 0.025(2) -0.0016(17) 0.0058(18) -0.0028(15) C6 0.041(3) 0.028(3) 0.023(2) 0.002(2) 0.015(2) -0.003(2) C7 0.044(3) 0.028(3) 0.026(2) 0.009(2) 0.002(2) -0.001(2) C8 0.031(3) 0.023(2) 0.037(3) 0.011(2) 0.007(2) 0.0055(18) C9 0.024(2) 0.014(2) 0.033(2) 0.0046(18) 0.0048(19) 0.0082(16) C10 0.026(2) 0.016(2) 0.047(3) 0.005(2) 0.004(2) 0.0031(17) C11 0.027(2) 0.019(2) 0.050(3) -0.013(2) -0.001(2) 0.0083(18) C12 0.029(3) 0.024(2) 0.039(3) 0.000(2) 0.008(2) 0.0140(18) C13 0.020(2) 0.017(2) 0.033(2) 0.0019(19) 0.0052(19) 0.0060(16) C14 0.023(2) 0.015(2) 0.034(2) 0.0026(19) 0.002(2) 0.0056(16) C15 0.026(2) 0.021(2) 0.027(2) 0.0014(19) 0.0035(19) 0.0007(17) C16 0.015(2) 0.014(2) 0.027(2) -0.0017(17) 0.0059(17) -0.0011(14) C17 0.018(2) 0.023(2) 0.040(3) -0.001(2) 0.006(2) 0.0018(16) C18 0.015(2) 0.021(2) 0.042(3) -0.0024(19) 0.008(2) -0.0017(15) C19 0.016(2) 0.018(2) 0.027(2) 0.0014(17) 0.0003(18) -0.0016(15) C20 0.015(2) 0.016(2) 0.028(2) 0.0039(17) 0.0011(18) -0.0029(15) C21 0.014(2) 0.020(2) 0.037(3) 0.0058(19) 0.0019(19) -0.0024(15) C22 0.014(2) 0.019(2) 0.035(2) 0.0040(19) -0.0015(19) -0.0019(15) C23 0.021(2) 0.018(2) 0.035(2) -0.0106(19) 0.003(2) -0.0005(16) C24 0.019(2) 0.017(2) 0.029(2) -0.0061(18) 0.0043(19) 0.0012(15) C25 0.025(2) 0.018(2) 0.036(2) -0.0019(19) 0.005(2) 0.0004(17) C26 0.030(3) 0.024(2) 0.040(3) -0.001(2) 0.005(2) 0.0104(19) C27 0.019(2) 0.027(2) 0.041(3) -0.009(2) 0.003(2) 0.0060(17) C28 0.020(2) 0.018(2) 0.036(2) -0.0090(19) 0.0065(19) -0.0024(16) C29 0.021(2) 0.015(2) 0.030(2) -0.0069(18) 0.0043(19) 0.0038(15) C30 0.021(2) 0.016(2) 0.030(2) -0.0021(18) 0.0053(19) -0.0022(16) C41 0.060(4) 0.036(3) 0.032(3) -0.003(2) -0.009(3) 0.008(3) C42 0.090(6) 0.054(4) 0.049(4) -0.006(3) 0.014(4) -0.008(4) C51 0.044(3) 0.052(4) 0.041(3) -0.002(3) 0.004(3) -0.004(3) C52 0.067(5) 0.044(4) 0.071(5) -0.009(3) 0.020(4) 0.001(3) N1 0.0214(19) 0.0154(19) 0.030(2) -0.0023(15) 0.0081(17) -0.0023(13) N2 0.0202(19) 0.0159(17) 0.0281(19) -0.0028(15) 0.0096(16) -0.0015(13) N3 0.027(2) 0.0157(18) 0.0274(19) -0.0023(15) 0.0067(16) -0.0020(14) N4 0.028(2) 0.0200(19) 0.0277(19) 0.0030(16) 0.0070(17) -0.0013(15) N5 0.0195(18) 0.0177(18) 0.0283(19) 0.0014(15) 0.0043(16) 0.0000(13) N6 0.0154(17) 0.0179(18) 0.0286(19) 0.0020(15) 0.0069(15) -0.0001(13) N7 0.0141(17) 0.0144(17) 0.0314(19) 0.0020(15) 0.0030(15) -0.0003(12) N8 0.0152(17) 0.0148(17) 0.0311(19) 0.0006(15) 0.0025(15) -0.0022(13) N41 0.044(3) 0.078(4) 0.049(3) -0.019(3) -0.012(3) 0.015(3) N51 0.065(4) 0.064(4) 0.066(4) -0.003(3) 0.008(3) 0.020(3) P1 0.0205(6) 0.0289(6) 0.0367(7) 0.0044(5) 0.0073(5) 0.0006(4) P2 0.0293(7) 0.0263(7) 0.0420(7) 0.0017(5) 0.0106(6) -0.0022(5) F1 0.0443(18) 0.0442(19) 0.0444(17) 0.0011(14) 0.0153(15) 0.0046(14) F2 0.0401(19) 0.057(2) 0.065(2) -0.0092(18) -0.0003(17) -0.0166(16) F3 0.0343(16) 0.0355(17) 0.0561(19) 0.0081(15) 0.0035(15) 0.0067(13) F4 0.0447(19) 0.062(2) 0.056(2) 0.0212(18) 0.0126(17) 0.0243(16) F5 0.056(2) 0.067(2) 0.053(2) 0.0120(18) 0.0275(18) 0.0207(18) F6 0.0374(18) 0.0392(19) 0.100(3) 0.0082(19) 0.0022(19) -0.0130(14) F7 0.115(4) 0.049(2) 0.061(2) 0.0152(19) -0.018(2) -0.041(2) F8 0.127(5) 0.138(5) 0.065(3) -0.039(3) 0.046(3) -0.066(4) F9 0.051(3) 0.130(5) 0.170(6) -0.015(4) 0.012(3) 0.024(3) F10 0.226(7) 0.146(5) 0.042(2) 0.001(3) 0.021(3) -0.130(5) F11 0.054(3) 0.168(7) 0.325(12) 0.030(7) 0.014(5) 0.061(4) F12 0.148(5) 0.052(3) 0.114(4) 0.006(3) 0.004(4) -0.053(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C16 2.120(4) . ? Ag1 C1 2.124(4) . ? Ag2 C5 2.109(4) . ? Ag2 C5 2.109(4) 2_655 ? Ag3 C20 2.115(4) . ? Ag3 C20 2.115(4) 2_655 ? C1 N1 1.347(6) . ? C1 N2 1.365(5) . ? C2 C3 1.357(7) . ? C2 N1 1.375(6) . ? C3 N2 1.381(6) . ? C4 N3 1.437(6) . ? C4 N2 1.454(5) . ? C5 N4 1.347(6) . ? C5 N3 1.370(6) . ? C6 C7 1.346(7) . ? C6 N3 1.378(6) . ? C7 N4 1.382(6) . ? C8 N4 1.481(6) . ? C8 C9 1.500(6) . ? C9 C10 1.387(7) . ? C9 C14 1.411(6) . ? C10 C11 1.383(7) . ? C11 C12 1.381(7) . ? C12 C13 1.391(7) . ? C13 C14 1.385(6) . ? C14 C15 1.517(6) . ? C15 N5 1.462(6) . ? C16 N5 1.353(5) . ? C16 N6 1.364(5) . ? C17 C18 1.341(7) . ? C17 N5 1.388(6) . ? C18 N6 1.381(6) . ? C19 N7 1.445(6) . ? C19 N6 1.461(5) . ? C20 N8 1.347(5) . ? C20 N7 1.361(5) . ? C21 C22 1.330(7) . ? C21 N7 1.379(5) . ? C22 N8 1.388(5) . ? C23 N8 1.475(6) . ? C23 C24 1.513(6) . ? C24 C29 1.395(6) . ? C24 C25 1.398(6) . ? C25 C26 1.389(7) . ? C26 C27 1.379(7) . ? C27 C28 1.377(7) . ? C28 C29 1.396(6) . ? C29 C30 1.529(6) . ? C30 N1 1.469(5) . ? C41 N41 1.127(8) . ? C41 C42 1.470(10) . ? C51 N51 1.142(8) . ? C51 C52 1.451(9) . ? P1 F5 1.581(4) . ? P1 F6 1.587(3) . ? P1 F3 1.592(3) . ? P1 F1 1.596(3) . ? P1 F2 1.597(3) . ? P1 F4 1.602(3) . ? P2 F11 1.513(5) . ? P2 F10 1.542(5) . ? P2 F9 1.556(5) . ? P2 F8 1.559(4) . ? P2 F7 1.563(4) . ? P2 F12 1.571(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 C16 Ag1 C1 168.11(16) . . ? C5 Ag2 C5 173.5(2) . 2_655 ? C20 Ag3 C20 176.0(2) . 2_655 ? N1 C1 N2 103.3(4) . . ? N1 C1 Ag1 129.9(3) . . ? N2 C1 Ag1 125.4(3) . . ? C3 C2 N1 106.6(4) . . ? C2 C3 N2 105.9(4) . . ? N3 C4 N2 111.2(4) . . ? N4 C5 N3 103.2(4) . . ? N4 C5 Ag2 128.1(3) . . ? N3 C5 Ag2 128.2(3) . . ? C7 C6 N3 106.7(4) . . ? C6 C7 N4 106.2(4) . . ? N4 C8 C9 115.1(4) . . ? C10 C9 C14 119.8(4) . . ? C10 C9 C8 119.1(4) . . ? C14 C9 C8 121.1(4) . . ? C11 C10 C9 121.1(4) . . ? C12 C11 C10 119.4(5) . . ? C11 C12 C13 120.1(5) . . ? C14 C13 C12 121.3(4) . . ? C13 C14 C9 118.3(4) . . ? C13 C14 C15 121.3(4) . . ? C9 C14 C15 120.3(4) . . ? N5 C15 C14 113.5(4) . . ? N5 C16 N6 103.0(3) . . ? N5 C16 Ag1 130.1(3) . . ? N6 C16 Ag1 125.7(3) . . ? C18 C17 N5 106.9(4) . . ? C17 C18 N6 106.0(4) . . ? N7 C19 N6 110.9(4) . . ? N8 C20 N7 103.5(3) . . ? N8 C20 Ag3 128.9(3) . . ? N7 C20 Ag3 127.3(3) . . ? C22 C21 N7 106.6(4) . . ? C21 C22 N8 106.8(4) . . ? N8 C23 C24 114.2(3) . . ? C29 C24 C25 120.1(4) . . ? C29 C24 C23 121.5(4) . . ? C25 C24 C23 118.3(4) . . ? C26 C25 C24 120.2(4) . . ? C27 C26 C25 119.6(4) . . ? C28 C27 C26 120.4(4) . . ? C27 C28 C29 121.2(4) . . ? C24 C29 C28 118.4(4) . . ? C24 C29 C30 119.0(4) . . ? C28 C29 C30 122.6(4) . . ? N1 C30 C29 113.3(4) . . ? N41 C41 C42 177.8(7) . . ? N51 C51 C52 178.6(7) . . ? C1 N1 C2 112.4(4) . . ? C1 N1 C30 124.8(4) . . ? C2 N1 C30 122.6(4) . . ? C1 N2 C3 111.9(4) . . ? C1 N2 C4 124.4(4) . . ? C3 N2 C4 123.6(4) . . ? C5 N3 C6 111.5(4) . . ? C5 N3 C4 123.9(4) . . ? C6 N3 C4 124.6(4) . . ? C5 N4 C7 112.4(4) . . ? C5 N4 C8 127.1(4) . . ? C7 N4 C8 120.5(4) . . ? C16 N5 C17 111.8(4) . . ? C16 N5 C15 125.1(4) . . ? C17 N5 C15 122.8(4) . . ? C16 N6 C18 112.3(4) . . ? C16 N6 C19 124.4(4) . . ? C18 N6 C19 123.2(4) . . ? C20 N7 C21 111.6(4) . . ? C20 N7 C19 123.9(4) . . ? C21 N7 C19 124.4(4) . . ? C20 N8 C22 111.5(4) . . ? C20 N8 C23 127.9(3) . . ? C22 N8 C23 120.6(4) . . ? F5 P1 F6 91.1(2) . . ? F5 P1 F3 90.21(19) . . ? F6 P1 F3 90.15(18) . . ? F5 P1 F1 178.7(2) . . ? F6 P1 F1 90.1(2) . . ? F3 P1 F1 90.05(18) . . ? F5 P1 F2 90.4(2) . . ? F6 P1 F2 178.5(2) . . ? F3 P1 F2 89.98(19) . . ? F1 P1 F2 88.36(19) . . ? F5 P1 F4 90.07(19) . . ? F6 P1 F4 89.9(2) . . ? F3 P1 F4 179.7(2) . . ? F1 P1 F4 89.67(18) . . ? F2 P1 F4 90.0(2) . . ? F11 P2 F10 90.0(5) . . ? F11 P2 F9 176.4(5) . . ? F10 P2 F9 93.6(4) . . ? F11 P2 F8 90.8(5) . . ? F10 P2 F8 179.1(3) . . ? F9 P2 F8 85.6(4) . . ? F11 P2 F7 89.2(4) . . ? F10 P2 F7 90.7(2) . . ? F9 P2 F7 90.8(3) . . ? F8 P2 F7 89.8(3) . . ? F11 P2 F12 92.8(4) . . ? F10 P2 F12 88.1(3) . . ? F9 P2 F12 87.3(4) . . ? F8 P2 F12 91.5(3) . . ? F7 P2 F12 177.6(3) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 72.00 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.533 _refine_diff_density_min -0.907 _refine_diff_density_rms 0.137