# CIF Copied by cif2cif, version 0.0.8 - beta ( 2 Apr 98) data_global _publ_requested_journal Chem.Commun. _publ_contact_author_name 'Gilmour, R.' _publ_contact_author_address ; ; _publ_contact_author_email gilmour@org.chem.ethz.ch _publ_contact_author_phone ' ' _publ_contact_author_fax ' ' loop_ _publ_author_name _publ_author_address 'Paul, S' ;ETH Zurich Wolfgang-Pauli-Str. 10 8093 Zurich, Switzerland ; 'Ebert, M-O.' ;ETH Zurich Wolfgang-Pauli-Str. 10 8093 Zurich, Switzerland ; 'Schweizer, W.B.' ;ETH Zurich Wolfgang-Pauli-Str. 10 8093 Zurich, Switzerland ; 'Gilmour, R.' ;ETH Zurich Wolfgang-Pauli-Str. 10 8093 Zurich, Switzerland ; _audit_creation_method maXus _publ_section_title ; A Novel Fluorinated Au(I) N-Heterocyclic Carbene Complex: Exploiting Fluorine Stereoelectronic Effects to Control Molecular Topology ; data_8 _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description 'Cube' _exptl_crystal_size_max .45 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .15 _exptl_crystal_F_000 568.0 _exptl_crystal_colour 'pale yellow' _diffrn_ambient_temperature 173 _cell_measurement_temperature 173 _refine_ls_hydrogen_treatment 'mixed' # Submission details _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 0.08275 _diffrn_orient_matrix_UB_12 -0.10361 _diffrn_orient_matrix_UB_13 -0.00540 _diffrn_orient_matrix_UB_21 -0.00514 _diffrn_orient_matrix_UB_22 -0.01075 _diffrn_orient_matrix_UB_23 0.12743 _diffrn_orient_matrix_UB_31 -0.03331 _diffrn_orient_matrix_UB_32 -0.02642 _diffrn_orient_matrix_UB_33 -0.00357 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 269.319 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X+ 1/2,-Y,+Z+ 1/2' '+X+ 1/2,-Y+ 1/2,-Z' '-X,+Y+ 1/2,-Z+ 1/2' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_cell_setting 'Orthorhombic' _chemical_formula_moiety 'C17 H16 F N O ' _chemical_formula_sum 'C17 H16 F N O ' _chemical_name_systematic ; ? ; _cell_length_a 7.5353(2) _cell_length_b 7.8131(2) _cell_length_c 23.4370(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1379.83(8) _diffrn_reflns_av_R_equivalents 0.044 _diffrn_reflns_number 2908 _diffrn_reflns_theta_max 27.45 _diffrn_reflns_theta_min 2.84 _diffrn_reflns_theta_full 27.45 _cell_measurement_reflns_used 9575 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _diffrn_measurement_method 'CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97(Altomare et al., J. Appl. Cryst.,1999)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _exptl_absorpt_coefficient_mu 0.090 _reflns_number_total 2889 _reflns_number_gt 2566 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.7(8) _refine_ls_number_reflns 2889 _refine_ls_number_parameters 245 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1131 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 F8 F -0.82796(14) 0.06624(12) -0.64806(4) 0.0334(3) Uani 1 1 d . . . O6 O -0.43270(18) 0.00515(17) -0.76368(6) 0.0389(3) Uani 1 1 d . . . N1 N -0.55479(19) -0.1431(2) -0.68861(7) 0.0292(3) Uani 1 1 d . . . C2 C -0.4717(2) -0.0090(2) -0.71291(8) 0.0314(4) Uani 1 1 d . . . C3 C -0.4334(3) 0.1220(3) -0.66673(9) 0.0386(4) Uani 1 1 d D . . C4 C -0.4721(3) 0.0272(3) -0.61081(9) 0.0372(4) Uani 1 1 d D . . C5 C -0.5932(2) -0.1229(2) -0.62832(8) 0.0280(4) Uani 1 1 d D . . C7 C -0.7920(2) -0.0877(2) -0.61829(7) 0.0274(4) Uani 1 1 d . . . C9 C -0.9070(2) -0.2271(2) -0.64455(8) 0.0267(4) Uani 1 1 d . . . C10 C -1.0358(2) -0.1883(3) -0.68508(8) 0.0325(4) Uani 1 1 d D . . C11 C -1.1373(3) -0.3182(3) -0.70945(9) 0.0384(5) Uani 1 1 d D . . C12 C -1.1113(3) -0.4853(3) -0.69367(9) 0.0395(5) Uani 1 1 d D . . C13 C -0.9839(3) -0.5256(3) -0.65314(10) 0.0405(5) Uani 1 1 d D . . C14 C -0.8827(2) -0.3968(2) -0.62829(9) 0.0341(4) Uani 1 1 d D . . C15 C -0.8387(2) -0.0541(2) -0.55606(8) 0.0297(4) Uani 1 1 d . . . C16 C -0.9796(3) 0.0551(3) -0.54364(9) 0.0369(4) Uani 1 1 d D . . C17 C -1.0250(3) 0.0910(3) -0.48743(10) 0.0441(5) Uani 1 1 d D . . C18 C -0.9303(3) 0.0176(3) -0.44297(9) 0.0445(5) Uani 1 1 d D . . C19 C -0.7927(3) -0.0939(3) -0.45487(9) 0.0417(5) Uani 1 1 d D . . C20 C -0.7468(3) -0.1306(3) -0.51100(8) 0.0358(4) Uani 1 1 d D . . H1 H -0.576(3) -0.236(3) -0.7070(12) 0.049(7) Uiso 1 1 d . . . H3A H -0.301(2) 0.160(3) -0.6698(9) 0.039(5) Uiso 1 1 d D . . H3B H -0.507(3) 0.229(2) -0.6711(9) 0.036(5) Uiso 1 1 d D . . H4A H -0.354(3) -0.017(3) -0.5932(10) 0.056(7) Uiso 1 1 d D . . H4B H -0.535(3) 0.111(3) -0.5819(10) 0.048(6) Uiso 1 1 d D . . H5 H -0.555(3) -0.233(2) -0.6061(8) 0.023(5) Uiso 1 1 d D . . H10 H -1.052(3) -0.068(2) -0.6983(10) 0.046(6) Uiso 1 1 d D . . H11 H -1.237(3) -0.295(3) -0.7355(10) 0.061(8) Uiso 1 1 d D . . H12 H -1.185(3) -0.571(2) -0.7124(9) 0.040(6) Uiso 1 1 d D . . H13 H -0.959(3) -0.644(2) -0.6410(12) 0.058(7) Uiso 1 1 d D . . H14 H -0.797(3) -0.418(3) -0.5999(8) 0.038(5) Uiso 1 1 d D . . H16 H -1.050(3) 0.108(3) -0.5754(9) 0.043(6) Uiso 1 1 d D . . H17 H -1.131(3) 0.164(3) -0.4817(11) 0.052(7) Uiso 1 1 d D . . H18 H -0.967(3) 0.048(3) -0.4034(8) 0.055(7) Uiso 1 1 d D . . H19 H -0.722(3) -0.148(3) -0.4240(8) 0.047(7) Uiso 1 1 d D . . H20 H -0.646(2) -0.201(3) -0.5191(10) 0.039(6) Uiso 1 1 d 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 F8 0.0442(6) 0.0214(5) 0.0345(6) 0.0038(4) -0.0004(5) 0.0032(4) O6 0.0465(7) 0.0335(7) 0.0367(7) 0.0056(6) 0.0105(6) 0.0011(6) N1 0.0355(7) 0.0234(7) 0.0288(8) -0.0009(6) 0.0034(6) -0.0010(6) C2 0.0314(8) 0.0271(9) 0.0357(10) 0.0029(7) 0.0032(7) 0.0009(7) C3 0.0445(10) 0.0292(10) 0.0421(11) -0.0004(8) 0.0020(8) -0.0071(8) C4 0.0403(10) 0.0383(11) 0.0332(10) -0.0030(8) -0.0027(8) -0.0112(8) C5 0.0321(8) 0.0254(8) 0.0265(8) 0.0007(7) -0.0012(7) -0.0024(7) C7 0.0353(8) 0.0214(8) 0.0255(8) 0.0030(6) -0.0011(7) 0.0007(6) C9 0.0277(7) 0.0267(8) 0.0256(8) -0.0015(6) 0.0027(6) -0.0007(6) C10 0.0331(9) 0.0357(10) 0.0286(9) 0.0007(8) 0.0001(7) 0.0012(7) C11 0.0354(9) 0.0463(12) 0.0336(10) -0.0058(9) -0.0005(7) -0.0042(8) C12 0.0407(9) 0.0407(11) 0.0371(11) -0.0117(9) 0.0056(8) -0.0095(8) C13 0.0451(10) 0.0274(10) 0.0491(12) -0.0019(8) 0.0042(9) -0.0037(8) C14 0.0353(9) 0.0264(10) 0.0407(11) 0.0025(8) -0.0023(8) 0.0001(7) C15 0.0356(9) 0.0262(9) 0.0273(9) -0.0026(7) 0.0007(7) -0.0045(7) C16 0.0407(9) 0.0323(10) 0.0376(10) -0.0040(8) 0.0018(8) 0.0015(8) C17 0.0480(11) 0.0403(12) 0.0439(12) -0.0120(9) 0.0117(9) -0.0014(9) C18 0.0563(12) 0.0432(12) 0.0338(11) -0.0127(9) 0.0086(9) -0.0145(10) C19 0.0498(11) 0.0467(12) 0.0287(9) -0.0003(8) 0.0004(8) -0.0105(9) C20 0.0420(10) 0.0360(10) 0.0294(10) -0.0008(7) 0.0000(8) -0.0008(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F8 C7 1.416(2) . ? O6 C2 1.230(2) . ? N1 C2 1.347(2) . ? N1 C5 1.451(2) . ? C2 C3 1.518(3) . ? C3 C4 1.533(3) . ? C4 C5 1.542(2) . ? C5 C7 1.541(2) . ? C7 C15 1.523(2) . ? C7 C9 1.522(2) . ? C9 C10 1.391(3) . ? C9 C14 1.392(3) . ? C10 C11 1.394(3) . ? C11 C12 1.371(3) . ? C12 C13 1.387(3) . ? C13 C14 1.391(3) . ? C15 C16 1.393(3) . ? C15 C20 1.397(3) . ? C16 C17 1.390(3) . ? C17 C18 1.387(3) . ? C18 C19 1.383(3) . ? C19 C20 1.390(3) . ? N1 H1 0.86(3) . ? C3 H3A 1.046(15) . ? C3 H3B 1.009(15) . ? C4 H4A 1.041(16) . ? C4 H4B 1.054(17) . ? C5 H5 1.044(14) . ? C10 H10 0.999(16) . ? C11 H11 0.986(17) . ? C12 H12 0.971(16) . ? C13 H13 0.986(17) . ? C14 H14 0.941(16) . ? C16 H16 1.003(16) . ? C17 H17 0.989(16) . ? C18 H18 0.996(16) . ? C19 H19 0.991(16) . ? C20 H20 0.956(16) . ? 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 C2 N1 C5 114.83(15) . . ? O6 C2 N1 126.16(18) . . ? O6 C2 C3 125.69(17) . . ? N1 C2 C3 108.15(16) . . ? C2 C3 C4 104.33(16) . . ? C3 C4 C5 104.63(15) . . ? N1 C5 C7 111.22(14) . . ? N1 C5 C4 102.95(14) . . ? C7 C5 C4 113.50(15) . . ? F8 C7 C15 106.32(13) . . ? F8 C7 C9 107.42(14) . . ? C15 C7 C9 112.29(14) . . ? F8 C7 C5 105.22(14) . . ? C15 C7 C5 113.66(15) . . ? C9 C7 C5 111.35(14) . . ? C10 C9 C14 119.06(17) . . ? C10 C9 C7 121.18(16) . . ? C14 C9 C7 119.76(16) . . ? C9 C10 C11 120.30(18) . . ? C12 C11 C10 120.30(19) . . ? C11 C12 C13 119.99(18) . . ? C12 C13 C14 120.16(18) . . ? C13 C14 C9 120.18(19) . . ? C16 C15 C20 118.81(18) . . ? C16 C15 C7 118.81(17) . . ? C20 C15 C7 122.37(17) . . ? C17 C16 C15 120.6(2) . . ? C18 C17 C16 120.1(2) . . ? C19 C18 C17 119.65(19) . . ? C18 C19 C20 120.5(2) . . ? C19 C20 C15 120.25(19) . . ? C2 N1 H1 122.2(18) . . ? C5 N1 H1 122.9(18) . . ? C2 C3 H3A 109.0(12) . . ? C4 C3 H3A 112.3(12) . . ? C2 C3 H3B 112.5(12) . . ? C4 C3 H3B 112.5(12) . . ? H3A C3 H3B 106.3(16) . . ? C3 C4 H4A 109.6(14) . . ? C5 C4 H4A 111.1(15) . . ? C3 C4 H4B 109.6(15) . . ? C5 C4 H4B 112.2(14) . . ? H4A C4 H4B 109(2) . . ? N1 C5 H5 110.0(11) . . ? C7 C5 H5 109.9(11) . . ? C4 C5 H5 109.1(11) . . ? C9 C10 H10 120.1(15) . . ? C11 C10 H10 119.5(15) . . ? C12 C11 H11 116.7(16) . . ? C10 C11 H11 122.8(15) . . ? C11 C12 H12 116.8(13) . . ? C13 C12 H12 123.2(13) . . ? C12 C13 H13 122.8(16) . . ? C14 C13 H13 117.0(16) . . ? C13 C14 H14 123.2(14) . . ? C9 C14 H14 116.6(14) . . ? C17 C16 H16 119.4(14) . . ? C15 C16 H16 120.0(14) . . ? C18 C17 H17 123.5(16) . . ? C16 C17 H17 116.3(16) . . ? C19 C18 H18 123.1(15) . . ? C17 C18 H18 117.3(15) . . ? C18 C19 H19 121.5(14) . . ? C20 C19 H19 118.0(14) . . ? C19 C20 H20 120.2(14) . . ? C15 C20 H20 119.3(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C2 O6 -176.85(18) . . . . ? C5 N1 C2 C3 3.4(2) . . . . ? O6 C2 C3 C4 -168.43(18) . . . . ? N1 C2 C3 C4 11.3(2) . . . . ? C2 C3 C4 C5 -20.5(2) . . . . ? C2 N1 C5 C7 105.46(17) . . . . ? C2 N1 C5 C4 -16.43(19) . . . . ? C3 C4 C5 N1 22.01(19) . . . . ? C3 C4 C5 C7 -98.31(19) . . . . ? N1 C5 C7 F8 -60.43(17) . . . . ? C4 C5 C7 F8 55.10(19) . . . . ? N1 C5 C7 C15 -176.35(14) . . . . ? C4 C5 C7 C15 -60.8(2) . . . . ? N1 C5 C7 C9 55.64(19) . . . . ? C4 C5 C7 C9 171.17(14) . . . . ? F8 C7 C9 C10 -7.5(2) . . . . ? C15 C7 C9 C10 109.08(19) . . . . ? C5 C7 C9 C10 -122.17(18) . . . . ? F8 C7 C9 C14 172.02(16) . . . . ? C15 C7 C9 C14 -71.4(2) . . . . ? C5 C7 C9 C14 57.3(2) . . . . ? C14 C9 C10 C11 -0.8(3) . . . . ? C7 C9 C10 C11 178.73(17) . . . . ? C9 C10 C11 C12 0.0(3) . . . . ? C10 C11 C12 C13 0.2(3) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? C12 C13 C14 C9 -0.9(3) . . . . ? C10 C9 C14 C13 1.2(3) . . . . ? C7 C9 C14 C13 -178.31(17) . . . . ? F8 C7 C15 C16 33.9(2) . . . . ? C9 C7 C15 C16 -83.3(2) . . . . ? C5 C7 C15 C16 149.13(17) . . . . ? F8 C7 C15 C20 -147.02(16) . . . . ? C9 C7 C15 C20 95.8(2) . . . . ? C5 C7 C15 C20 -31.8(2) . . . . ? C20 C15 C16 C17 1.7(3) . . . . ? C7 C15 C16 C17 -179.14(18) . . . . ? C15 C16 C17 C18 -0.2(3) . . . . ? C16 C17 C18 C19 -1.2(3) . . . . ? C17 C18 C19 C20 1.1(3) . . . . ? C18 C19 C20 C15 0.4(3) . . . . ? C16 C15 C20 C19 -1.8(3) . . . . ? C7 C15 C20 C19 179.06(17) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.180 _refine_diff_density_min -0.161 _refine_diff_density_rms 0.034 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Moliterni, A.G.G & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; data_11 _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description 'Cube' _exptl_crystal_size_max .27 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .105 _exptl_crystal_F_000 944.0 _exptl_crystal_colour 'pale yellow' _diffrn_ambient_temperature 173 _cell_measurement_temperature 173 _refine_ls_hydrogen_treatment 'constr' # Submission details _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 -0.00178 _diffrn_orient_matrix_UB_12 0.00465 _diffrn_orient_matrix_UB_13 -0.06147 _diffrn_orient_matrix_UB_21 -0.05366 _diffrn_orient_matrix_UB_22 0.13266 _diffrn_orient_matrix_UB_23 0.01159 _diffrn_orient_matrix_UB_31 0.04897 _diffrn_orient_matrix_UB_32 0.02107 _diffrn_orient_matrix_UB_33 -0.01439 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 457.254 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '+X+ 1/2,+Y+ 1/2,+Z' '-X,+Y,-Z' '-X+ 1/2,+Y+ 1/2,-Z' _symmetry_space_group_name_H-M 'C 2 ' _symmetry_cell_setting 'Monoclinic' _chemical_formula_moiety 'C24 H21 F N3 +1, B F4 -1 ' _chemical_formula_sum 'C24 H21 B F5 N3 ' _chemical_name_systematic ; ? ; _cell_length_a 16.8056(8) _cell_length_b 6.9654(4) _cell_length_c 18.7706(9) _cell_angle_alpha 90.00 _cell_angle_beta 105.241(2) _cell_angle_gamma 90.00 _cell_volume 2120.0(2) _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_number 4441 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_full 27.48 _cell_measurement_reflns_used 65150 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _diffrn_measurement_method 'CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _exptl_absorpt_coefficient_mu 0.115 _reflns_number_total 4441 _reflns_number_gt 3649 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.4(7) _refine_ls_number_reflns 4441 _refine_ls_number_parameters 298 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1240 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 F16 F 0.73788(9) 0.3942(2) 0.78021(8) 0.0487(4) Uani 1 1 d . . . F30 F 0.93165(9) 0.6923(3) 0.68824(8) 0.0515(4) Uani 1 1 d . . . F31 F 1.05274(10) 0.5567(3) 0.75352(9) 0.0606(4) Uani 1 1 d . . . F32 F 1.00099(10) 0.4820(3) 0.63338(9) 0.0614(5) Uani 1 1 d . . . F33 F 0.93616(12) 0.3754(3) 0.71681(12) 0.0720(5) Uani 1 1 d . . . N1 N 0.70717(10) 0.6278(3) 0.55706(9) 0.0347(4) Uani 1 1 d . . . N2 N 0.62505(12) 0.5742(3) 0.53908(10) 0.0386(4) Uani 1 1 d . . . N4 N 0.67341(10) 0.6330(3) 0.65892(9) 0.0334(4) Uani 1 1 d . . . C3 C 0.60726(13) 0.5775(4) 0.60289(11) 0.0361(5) Uani 1 1 d . . . C5 C 0.65156(12) 0.6517(3) 0.73053(11) 0.0348(5) Uani 1 1 d . . . C6 C 0.57132(14) 0.5329(4) 0.71450(12) 0.0427(6) Uani 1 1 d . . . C7 C 0.53384(14) 0.5368(4) 0.63000(12) 0.0445(6) Uani 1 1 d . . . C8 C 0.73682(13) 0.6639(3) 0.62908(11) 0.0337(5) Uani 1 1 d . . . C9 C 0.74878(14) 0.6318(3) 0.49885(12) 0.0351(5) Uani 1 1 d . . . C10 C 0.70226(14) 0.6664(4) 0.42771(12) 0.0390(5) Uani 1 1 d . . . C11 C 0.74167(15) 0.6690(4) 0.37096(12) 0.0410(5) Uani 1 1 d . . . C12 C 0.82539(15) 0.6315(4) 0.38579(13) 0.0443(6) Uani 1 1 d . . . C13 C 0.87061(16) 0.5947(4) 0.45783(14) 0.0455(6) Uani 1 1 d . . . C14 C 0.83241(14) 0.5968(4) 0.51534(13) 0.0416(5) Uani 1 1 d . . . C15 C 0.71930(13) 0.5826(4) 0.79721(12) 0.0375(5) Uani 1 1 d . . . C17 C 0.68568(14) 0.5780(4) 0.86521(12) 0.0451(6) Uani 1 1 d . . . C18 C 0.65220(17) 0.7430(5) 0.88713(14) 0.0550(7) Uani 1 1 d . . . C19 C 0.6237(2) 0.7399(7) 0.95059(16) 0.0791(12) Uani 1 1 d . . . C20 C 0.6295(2) 0.5757(10) 0.99184(17) 0.0975(18) Uani 1 1 d . . . C21 C 0.6632(2) 0.4149(9) 0.9709(2) 0.0930(17) Uani 1 1 d . . . C22 C 0.69141(19) 0.4110(6) 0.90685(17) 0.0698(10) Uani 1 1 d . . . C23 C 0.79916(13) 0.6983(4) 0.81341(11) 0.0361(5) Uani 1 1 d . . . C24 C 0.80061(15) 0.8915(4) 0.79687(12) 0.0412(5) Uani 1 1 d . . . C25 C 0.87467(16) 0.9934(4) 0.81483(13) 0.0484(6) Uani 1 1 d . . . C26 C 0.94686(16) 0.9018(5) 0.84995(14) 0.0511(7) Uani 1 1 d . . . C27 C 0.94592(15) 0.7099(5) 0.86801(15) 0.0552(7) Uani 1 1 d . . . C28 C 0.87254(15) 0.6073(5) 0.85018(14) 0.0479(6) Uani 1 1 d . . . B29 B 0.97968(16) 0.5257(5) 0.69887(15) 0.0430(6) Uani 1 1 d . . . H5 H 0.6375 0.8001 0.7387 0.042 Uiso 1 1 calc R . . H6A H 0.5288 0.5946 0.7424 0.051 Uiso 1 1 calc R . . H6B H 0.5845 0.3870 0.7335 0.051 Uiso 1 1 calc R . . H7A H 0.5065 0.4004 0.6099 0.053 Uiso 1 1 calc R . . H7B H 0.4880 0.6485 0.6141 0.053 Uiso 1 1 calc R . . H8 H 0.7929 0.7044 0.6547 0.040 Uiso 1 1 calc R . . H10 H 0.6427 0.6887 0.4173 0.047 Uiso 1 1 calc R . . H11 H 0.7100 0.6975 0.3203 0.049 Uiso 1 1 calc R . . H12 H 0.8526 0.6308 0.3456 0.053 Uiso 1 1 calc R . . H13 H 0.9297 0.5672 0.4683 0.055 Uiso 1 1 calc R . . H14 H 0.8643 0.5740 0.5664 0.050 Uiso 1 1 calc R . . H18 H 0.6486 0.8612 0.8581 0.066 Uiso 1 1 calc R . . H19 H 0.5994 0.8559 0.9657 0.095 Uiso 1 1 calc R . . H20 H 0.6094 0.5742 1.0363 0.117 Uiso 1 1 calc R . . H21 H 0.6680 0.2989 1.0013 0.112 Uiso 1 1 calc R . . H22 H 0.7146 0.2934 0.8918 0.084 Uiso 1 1 calc R . . H24 H 0.7492 0.9573 0.7723 0.049 Uiso 1 1 calc R . . H25 H 0.8753 1.1300 0.8025 0.058 Uiso 1 1 calc R . . H26 H 0.9990 0.9730 0.8622 0.061 Uiso 1 1 calc R . . H27 H 0.9974 0.6457 0.8936 0.066 Uiso 1 1 calc R . . H28 H 0.8722 0.4712 0.8634 0.057 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 F16 0.0493(8) 0.0417(8) 0.0507(8) -0.0002(6) 0.0052(6) 0.0006(6) F30 0.0398(7) 0.0633(10) 0.0502(8) -0.0048(7) 0.0096(6) 0.0019(7) F31 0.0487(8) 0.0630(10) 0.0590(9) -0.0057(8) -0.0053(7) 0.0028(8) F32 0.0503(9) 0.0883(13) 0.0505(8) -0.0043(8) 0.0217(7) 0.0090(8) F33 0.0714(11) 0.0609(11) 0.0980(14) -0.0131(10) 0.0476(10) -0.0209(9) N1 0.0307(8) 0.0434(11) 0.0308(9) -0.0010(8) 0.0097(7) -0.0038(8) N2 0.0325(9) 0.0499(12) 0.0329(9) 0.0012(8) 0.0075(7) -0.0041(8) N4 0.0279(8) 0.0418(10) 0.0304(8) 0.0009(7) 0.0074(7) -0.0024(7) C3 0.0309(10) 0.0461(13) 0.0298(10) -0.0010(9) 0.0057(8) -0.0056(9) C5 0.0341(10) 0.0453(13) 0.0272(9) 0.0012(9) 0.0122(8) -0.0015(9) C6 0.0360(11) 0.0615(16) 0.0313(11) -0.0013(10) 0.0101(9) -0.0096(11) C7 0.0306(10) 0.0682(17) 0.0350(11) -0.0019(11) 0.0091(9) -0.0092(11) C8 0.0312(10) 0.0397(13) 0.0299(10) 0.0024(8) 0.0077(8) -0.0021(9) C9 0.0369(10) 0.0397(12) 0.0306(9) -0.0005(8) 0.0119(8) -0.0033(9) C10 0.0379(11) 0.0447(14) 0.0348(11) -0.0010(9) 0.0102(9) -0.0021(10) C11 0.0464(12) 0.0469(14) 0.0319(10) -0.0016(9) 0.0141(9) -0.0042(11) C12 0.0447(12) 0.0533(15) 0.0387(12) -0.0027(10) 0.0178(10) -0.0069(11) C13 0.0367(11) 0.0579(16) 0.0454(12) -0.0014(11) 0.0169(10) -0.0021(11) C14 0.0369(11) 0.0527(15) 0.0364(11) 0.0016(10) 0.0118(9) -0.0011(11) C15 0.0365(11) 0.0415(13) 0.0353(11) 0.0022(9) 0.0110(9) -0.0006(9) C17 0.0354(11) 0.0683(17) 0.0299(10) 0.0062(11) 0.0059(9) -0.0129(11) C18 0.0531(15) 0.078(2) 0.0380(12) -0.0112(13) 0.0203(11) -0.0165(14) C19 0.0649(19) 0.138(4) 0.0421(15) -0.0199(19) 0.0275(14) -0.033(2) C20 0.0546(18) 0.203(6) 0.0340(15) 0.010(2) 0.0100(13) -0.042(3) C21 0.054(2) 0.165(5) 0.0520(19) 0.056(3) -0.0003(16) -0.030(2) C22 0.0496(16) 0.097(3) 0.0569(17) 0.0375(17) 0.0033(13) -0.0105(16) C23 0.0323(10) 0.0482(13) 0.0288(9) -0.0022(9) 0.0099(8) -0.0001(10) C24 0.0372(12) 0.0519(15) 0.0327(10) 0.0004(10) 0.0057(9) -0.0038(10) C25 0.0472(14) 0.0612(17) 0.0355(12) -0.0028(11) 0.0085(10) -0.0155(12) C26 0.0400(13) 0.075(2) 0.0400(12) -0.0104(13) 0.0135(10) -0.0151(13) C27 0.0321(12) 0.081(2) 0.0510(14) -0.0074(14) 0.0085(10) 0.0035(13) C28 0.0378(12) 0.0588(17) 0.0456(13) -0.0008(11) 0.0084(10) 0.0060(11) B29 0.0348(13) 0.0546(17) 0.0403(13) -0.0028(12) 0.0112(11) -0.0034(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 F16 C15 1.405(3) . ? F30 B29 1.397(4) . ? F31 B29 1.394(3) . ? F32 B29 1.401(3) . ? F33 B29 1.369(4) . ? N1 C8 1.336(3) . ? N1 N2 1.383(3) . ? N1 C9 1.444(3) . ? N2 C3 1.309(3) . ? N4 C8 1.345(3) . ? N4 C3 1.370(3) . ? N4 C5 1.489(2) . ? C3 C7 1.481(3) . ? C5 C15 1.531(3) . ? C5 C6 1.543(3) . ? C6 C7 1.545(3) . ? C9 C14 1.379(3) . ? C9 C10 1.380(3) . ? C10 C11 1.394(3) . ? C11 C12 1.385(4) . ? C12 C13 1.390(4) . ? C13 C14 1.394(3) . ? C15 C23 1.526(3) . ? C15 C17 1.526(3) . ? C17 C18 1.388(5) . ? C17 C22 1.391(4) . ? C18 C19 1.396(4) . ? C19 C20 1.370(8) . ? C20 C21 1.359(8) . ? C21 C22 1.404(5) . ? C23 C24 1.382(4) . ? C23 C28 1.397(3) . ? C24 C25 1.395(4) . ? C25 C26 1.376(4) . ? C26 C27 1.380(5) . ? C27 C28 1.388(4) . ? C5 H5 1.0800 . ? C6 H6A 1.0800 . ? C6 H6B 1.0800 . ? C7 H7A 1.0800 . ? C7 H7B 1.0800 . ? C8 H8 0.9800 . ? C10 H10 0.9800 . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C13 H13 0.9800 . ? C14 H14 0.9800 . ? C18 H18 0.9800 . ? C19 H19 0.9800 . ? C20 H20 0.9800 . ? C21 H21 0.9800 . ? C22 H22 0.9800 . ? C24 H24 0.9800 . ? C25 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C28 H28 0.9800 . ? 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 C8 N1 N2 112.37(16) . . ? C8 N1 C9 129.50(18) . . ? N2 N1 C9 118.10(17) . . ? C3 N2 N1 103.01(17) . . ? C8 N4 C3 107.29(17) . . ? C8 N4 C5 140.54(18) . . ? C3 N4 C5 112.01(16) . . ? N2 C3 N4 111.91(18) . . ? N2 C3 C7 136.3(2) . . ? N4 C3 C7 111.81(18) . . ? N4 C5 C15 113.79(16) . . ? N4 C5 C6 100.79(16) . . ? C15 C5 C6 114.50(19) . . ? C5 C6 C7 106.88(18) . . ? C3 C7 C6 101.80(18) . . ? N1 C8 N4 105.40(18) . . ? C14 C9 C10 122.2(2) . . ? C14 C9 N1 119.6(2) . . ? C10 C9 N1 118.1(2) . . ? C9 C10 C11 118.7(2) . . ? C12 C11 C10 120.3(2) . . ? C11 C12 C13 119.8(2) . . ? C12 C13 C14 120.4(2) . . ? C9 C14 C13 118.5(2) . . ? F16 C15 C23 107.59(18) . . ? F16 C15 C17 108.9(2) . . ? C23 C15 C17 110.11(18) . . ? F16 C15 C5 105.65(18) . . ? C23 C15 C5 115.01(19) . . ? C17 C15 C5 109.33(17) . . ? C18 C17 C22 120.0(3) . . ? C18 C17 C15 119.9(2) . . ? C22 C17 C15 120.1(3) . . ? C17 C18 C19 119.8(3) . . ? C20 C19 C18 120.4(4) . . ? C21 C20 C19 119.8(3) . . ? C20 C21 C22 121.6(4) . . ? C17 C22 C21 118.4(4) . . ? C24 C23 C28 119.1(2) . . ? C24 C23 C15 122.4(2) . . ? C28 C23 C15 118.4(2) . . ? C23 C24 C25 120.6(2) . . ? C26 C25 C24 119.9(3) . . ? C25 C26 C27 120.1(2) . . ? C26 C27 C28 120.4(3) . . ? C27 C28 C23 119.9(3) . . ? F33 B29 F31 111.2(2) . . ? F33 B29 F30 110.1(2) . . ? F31 B29 F30 109.9(2) . . ? F33 B29 F32 109.0(2) . . ? F31 B29 F32 107.49(19) . . ? F30 B29 F32 109.0(2) . . ? N4 C5 H5 109.1 . . ? C15 C5 H5 109.1 . . ? C6 C5 H5 109.1 . . ? C5 C6 H6A 110.3 . . ? C7 C6 H6A 110.3 . . ? C5 C6 H6B 110.3 . . ? C7 C6 H6B 110.3 . . ? H6A C6 H6B 108.6 . . ? C3 C7 H7A 111.4 . . ? C6 C7 H7A 111.4 . . ? C3 C7 H7B 111.4 . . ? C6 C7 H7B 111.4 . . ? H7A C7 H7B 109.3 . . ? N1 C8 H8 127.3 . . ? N4 C8 H8 127.3 . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C9 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C17 C18 H18 120.1 . . ? C19 C18 H18 120.1 . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C17 C22 H22 120.8 . . ? C21 C22 H22 120.8 . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 H28 120.0 . . ? C23 C28 H28 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C8 N1 N2 C3 -0.7(3) . . . . ? C9 N1 N2 C3 177.5(2) . . . . ? N1 N2 C3 N4 0.9(3) . . . . ? N1 N2 C3 C7 -179.2(3) . . . . ? C8 N4 C3 N2 -0.9(3) . . . . ? C5 N4 C3 N2 175.5(2) . . . . ? C8 N4 C3 C7 179.2(2) . . . . ? C5 N4 C3 C7 -4.4(3) . . . . ? C8 N4 C5 C15 -43.6(4) . . . . ? C3 N4 C5 C15 141.8(2) . . . . ? C8 N4 C5 C6 -166.7(3) . . . . ? C3 N4 C5 C6 18.7(3) . . . . ? N4 C5 C6 C7 -25.5(3) . . . . ? C15 C5 C6 C7 -148.1(2) . . . . ? N2 C3 C7 C6 168.0(3) . . . . ? N4 C3 C7 C6 -12.1(3) . . . . ? C5 C6 C7 C3 23.4(3) . . . . ? N2 N1 C8 N4 0.2(3) . . . . ? C9 N1 C8 N4 -177.7(2) . . . . ? C3 N4 C8 N1 0.4(2) . . . . ? C5 N4 C8 N1 -174.4(3) . . . . ? C8 N1 C9 C14 27.4(4) . . . . ? N2 N1 C9 C14 -150.4(2) . . . . ? C8 N1 C9 C10 -154.1(2) . . . . ? N2 N1 C9 C10 28.1(3) . . . . ? C14 C9 C10 C11 -1.1(4) . . . . ? N1 C9 C10 C11 -179.5(2) . . . . ? C9 C10 C11 C12 2.0(4) . . . . ? C10 C11 C12 C13 -1.3(4) . . . . ? C11 C12 C13 C14 -0.5(4) . . . . ? C10 C9 C14 C13 -0.7(4) . . . . ? N1 C9 C14 C13 177.8(2) . . . . ? C12 C13 C14 C9 1.4(4) . . . . ? N4 C5 C15 F16 -54.0(2) . . . . ? C6 C5 C15 F16 61.2(2) . . . . ? N4 C5 C15 C23 64.5(3) . . . . ? C6 C5 C15 C23 179.69(19) . . . . ? N4 C5 C15 C17 -171.0(2) . . . . ? C6 C5 C15 C17 -55.8(3) . . . . ? F16 C15 C17 C18 -171.2(2) . . . . ? C23 C15 C17 C18 71.1(3) . . . . ? C5 C15 C17 C18 -56.2(3) . . . . ? F16 C15 C17 C22 11.3(3) . . . . ? C23 C15 C17 C22 -106.4(3) . . . . ? C5 C15 C17 C22 126.3(3) . . . . ? C22 C17 C18 C19 -0.6(4) . . . . ? C15 C17 C18 C19 -178.1(2) . . . . ? C17 C18 C19 C20 0.8(4) . . . . ? C18 C19 C20 C21 0.1(5) . . . . ? C19 C20 C21 C22 -1.1(5) . . . . ? C18 C17 C22 C21 -0.4(4) . . . . ? C15 C17 C22 C21 177.1(2) . . . . ? C20 C21 C22 C17 1.3(5) . . . . ? F16 C15 C23 C24 147.4(2) . . . . ? C17 C15 C23 C24 -94.1(3) . . . . ? C5 C15 C23 C24 30.0(3) . . . . ? F16 C15 C23 C28 -36.4(3) . . . . ? C17 C15 C23 C28 82.1(3) . . . . ? C5 C15 C23 C28 -153.8(2) . . . . ? C28 C23 C24 C25 1.7(3) . . . . ? C15 C23 C24 C25 177.9(2) . . . . ? C23 C24 C25 C26 -0.6(4) . . . . ? C24 C25 C26 C27 -0.6(4) . . . . ? C25 C26 C27 C28 0.8(4) . . . . ? C26 C27 C28 C23 0.3(4) . . . . ? C24 C23 C28 C27 -1.5(3) . . . . ? C15 C23 C28 C27 -177.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.174 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.050 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; data_16 _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description 'needle' _exptl_crystal_size_max .21 _exptl_crystal_size_mid .045 _exptl_crystal_size_min .006 _exptl_crystal_F_000 2232 _exptl_crystal_colour 'pale yellow' _diffrn_ambient_temperature 100 _cell_measurement_temperature 100 _refine_ls_hydrogen_treatment 'constr' # Submission details _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 -0.08780 _diffrn_orient_matrix_UB_12 -0.05469 _diffrn_orient_matrix_UB_13 0.00091 _diffrn_orient_matrix_UB_21 0.02343 _diffrn_orient_matrix_UB_22 -0.03798 _diffrn_orient_matrix_UB_23 -0.02156 _diffrn_orient_matrix_UB_31 0.00873 _diffrn_orient_matrix_UB_32 -0.01346 _diffrn_orient_matrix_UB_33 0.03318 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 1097.66 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X+ 1/2,-Y,+Z+ 1/2' '+X+ 1/2,-Y+ 1/2,-Z' '-X,+Y+ 1/2,-Z+ 1/2' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_cell_setting 'Orthorhombic' _chemical_formula_moiety '2(C24 H20 Ag Cl F N3) , C5 H12 ' _chemical_formula_sum 'C53 H52 Ag2 Cl2 F2 N6 ' _chemical_name_systematic ; ? ; _cell_length_a 9.6676(3) _cell_length_b 20.1778(5) _cell_length_c 27.1375(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5293.7(3) _diffrn_reflns_av_R_equivalents 0.092 _diffrn_reflns_number 26194 _diffrn_reflns_theta_max 25.01 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_full 25.01 _cell_measurement_reflns_used 241052 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.028 _diffrn_measurement_method 'CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? 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' 'Ag' 'Ag' -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _exptl_absorpt_coefficient_mu 0.887 _reflns_number_total 9018 _reflns_number_gt 7645 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 9018 _refine_ls_number_parameters 578 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0868 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.1823 _refine_ls_wR_factor_gt 0.1728 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.201 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 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 0.91162(7) 0.09137(3) 0.24925(3) 0.02625(19) Uani 1 1 d . . . Ag2 Ag 0.90091(7) -0.00817(3) 0.16152(2) 0.02647(19) Uani 1 1 d . . . Cl4 Cl 0.8096(3) 0.18110(12) 0.20895(9) 0.0308(6) Uani 1 1 d . . . Cl5 Cl 0.6870(3) -0.04108(16) 0.19212(10) 0.0435(7) Uani 1 1 d . . . F27 F 1.1370(5) 0.1259(3) 0.03346(18) 0.0252(12) Uani 1 1 d . . . F55 F 0.9124(6) -0.1029(3) 0.37805(19) 0.0354(13) Uani 1 1 d . . . N6 N 1.2159(8) -0.0217(4) 0.1366(3) 0.0271(19) Uani 1 1 d . . . N8 N 1.1452(7) 0.0761(4) 0.1255(3) 0.0220(17) Uani 1 1 d . . . N13 N 1.3360(8) 0.0144(4) 0.1241(3) 0.0280(18) Uani 1 1 d . . . N35 N 1.1778(8) 0.0145(4) 0.2763(3) 0.0271(19) Uani 1 1 d . . . N36 N 1.2365(8) -0.0482(4) 0.2843(3) 0.0278(19) Uani 1 1 d . . . N41 N 1.0043(8) -0.0481(4) 0.2879(3) 0.0247(18) Uani 1 1 d . . . C7 C 1.1001(11) 0.0164(5) 0.1383(3) 0.029(2) Uani 1 1 d . . . C9 C 1.0887(11) 0.1424(5) 0.1171(3) 0.027(2) Uani 1 1 d . . . C10 C 1.2219(9) 0.1851(5) 0.1257(4) 0.029(2) Uani 1 1 d . . . C11 C 1.3474(11) 0.1409(5) 0.1095(4) 0.030(2) Uani 1 1 d . . . C12 C 1.2905(9) 0.0755(5) 0.1188(3) 0.025(2) Uani 1 1 d . . . C14 C 1.0296(10) 0.1475(5) 0.0651(3) 0.025(2) Uani 1 1 d . . . C15 C 0.9056(11) 0.1013(4) 0.0566(3) 0.029(2) Uani 1 1 d . . . C16 C 0.9012(13) 0.0638(5) 0.0120(4) 0.038(2) Uani 1 1 d . . . C17 C 0.7867(12) 0.0220(5) 0.0041(5) 0.041(3) Uani 1 1 d . . . C18 C 0.6841(11) 0.0150(5) 0.0366(4) 0.041(3) Uani 1 1 d . . . C19 C 0.6893(12) 0.0532(5) 0.0801(4) 0.039(3) Uani 1 1 d . . . C20 C 0.7996(9) 0.0945(5) 0.0900(4) 0.027(2) Uani 1 1 d . . . C21 C 0.9968(9) 0.2205(5) 0.0510(4) 0.026(2) Uani 1 1 d . . . C22 C 1.0844(11) 0.2552(4) 0.0200(3) 0.027(2) Uani 1 1 d . . . C23 C 1.0613(9) 0.3198(5) 0.0077(3) 0.025(2) Uani 1 1 d . . . C24 C 0.9455(10) 0.3517(5) 0.0276(4) 0.032(2) Uani 1 1 d . . . C25 C 0.8558(10) 0.3175(5) 0.0579(4) 0.026(2) Uani 1 1 d . . . C26 C 0.8824(9) 0.2523(4) 0.0709(3) 0.024(2) Uani 1 1 d . . . C28 C 1.2341(11) -0.0889(5) 0.1511(4) 0.031(2) Uani 1 1 d . . . C29 C 1.3637(11) -0.1114(5) 0.1664(4) 0.033(2) Uani 1 1 d . . . C30 C 1.3779(12) -0.1758(5) 0.1805(4) 0.038(3) Uani 1 1 d . . . C31 C 1.2732(14) -0.2200(6) 0.1812(4) 0.050(3) Uani 1 1 d . . . C32 C 1.1427(12) -0.1984(6) 0.1635(5) 0.048(3) Uani 1 1 d . . . C33 C 1.1244(10) -0.1329(5) 0.1480(4) 0.038(3) Uani 1 1 d . . . C34 C 1.0396(10) 0.0174(5) 0.2776(3) 0.024(2) Uani 1 1 d . . . C37 C 1.1253(10) -0.0842(5) 0.2912(4) 0.028(2) Uani 1 1 d . . . C38 C 1.0929(11) -0.1564(5) 0.2986(4) 0.034(2) Uani 1 1 d . . . C39 C 0.9367(10) -0.1585(5) 0.2852(4) 0.034(3) Uani 1 1 d . . . C40 C 0.8811(10) -0.0868(5) 0.2936(3) 0.028(2) Uani 1 1 d . . . C42 C 0.8152(10) -0.0776(5) 0.3441(3) 0.028(2) Uani 1 1 d . . . C43 C 0.6826(10) -0.1190(4) 0.3495(3) 0.022(2) Uani 1 1 d . . . C44 C 0.6537(10) -0.1472(5) 0.3959(4) 0.026(2) Uani 1 1 d . . . C45 C 0.5400(11) -0.1864(5) 0.4022(4) 0.034(3) Uani 1 1 d . . . C46 C 0.4544(11) -0.1960(5) 0.3627(4) 0.037(3) Uani 1 1 d . . . C47 C 0.4746(12) -0.1677(5) 0.3167(5) 0.039(3) Uani 1 1 d . . . C48 C 0.5927(11) -0.1280(5) 0.3122(4) 0.033(2) Uani 1 1 d . . . C49 C 0.7963(9) -0.0054(5) 0.3570(3) 0.027(2) Uani 1 1 d . . . C50 C 0.6809(12) 0.0304(5) 0.3376(5) 0.044(3) Uani 1 1 d . . . C51 C 0.6642(15) 0.0970(6) 0.3505(5) 0.054(3) Uani 1 1 d . . . C52 C 0.7504(18) 0.1283(6) 0.3817(5) 0.065(4) Uani 1 1 d . . . C53 C 0.8656(13) 0.0923(6) 0.4012(4) 0.046(3) Uani 1 1 d . . . C54 C 0.8855(13) 0.0269(5) 0.3898(4) 0.038(3) Uani 1 1 d . . . C56 C 1.2691(11) 0.0686(5) 0.2664(4) 0.028(2) Uani 1 1 d . . . C57 C 1.2319(10) 0.1327(5) 0.2806(4) 0.026(2) Uani 1 1 d . . . C58 C 1.3231(12) 0.1838(6) 0.2693(4) 0.043(3) Uani 1 1 d . . . C59 C 1.4463(10) 0.1715(5) 0.2434(4) 0.035(3) Uani 1 1 d . . . C60 C 1.4780(11) 0.1089(6) 0.2309(4) 0.037(3) Uani 1 1 d . . . C61 C 1.3894(11) 0.0555(5) 0.2413(3) 0.031(2) Uani 1 1 d . . . C65 C 0.692(2) 0.4917(10) 0.0944(7) 0.038(5) Uiso 0.484(11) 1 d PD A 1 C66 C 0.722(2) 0.5268(11) 0.0452(7) 0.046(6) Uiso 0.484(11) 1 d PD A 1 C67 C 0.611(3) 0.5799(14) 0.0397(10) 0.085(10) Uiso 0.484(11) 1 d PD A 1 C68 C 0.631(4) 0.611(2) -0.0120(12) 0.130(18) Uiso 0.484(11) 1 d PD A 1 C69 C 0.509(3) 0.6606(14) -0.0189(11) 0.069(9) Uiso 0.484(11) 1 d PD A 1 C70 C 0.262(4) 0.7178(17) -0.1192(11) 0.098(6) Uiso 0.516(11) 1 d PD A 2 C71 C 0.212(4) 0.6570(14) -0.0922(10) 0.098(6) Uiso 0.516(11) 1 d PD A 2 C72 C 0.199(2) 0.6684(17) -0.0365(9) 0.098(6) Uiso 0.516(11) 1 d PD A 2 C73 C 0.049(3) 0.6925(14) -0.0308(13) 0.098(6) Uiso 0.516(11) 1 d PD A 2 C74 C -0.055(3) 0.6381(17) -0.0333(14) 0.098(6) Uiso 0.516(11) 1 d PD A 2 H9 H 1.0105 0.1540 0.1442 0.033 Uiso 1 1 calc R . . H10A H 1.2311 0.1985 0.1641 0.034 Uiso 1 1 calc R . . H10B H 1.2179 0.2299 0.1040 0.034 Uiso 1 1 calc R . . H11A H 1.3723 0.1479 0.0710 0.036 Uiso 1 1 calc R . . H11B H 1.4380 0.1504 0.1316 0.036 Uiso 1 1 calc R . . H16 H 0.9757 0.0670 -0.0124 0.045 Uiso 1 1 calc R . . H17 H 0.7821 -0.0031 -0.0267 0.049 Uiso 1 1 calc R . . H18 H 0.6075 -0.0157 0.0304 0.049 Uiso 1 1 calc R . . H19 H 0.6131 0.0503 0.1038 0.047 Uiso 1 1 calc R . . H20 H 0.8024 0.1192 0.1210 0.033 Uiso 1 1 calc R . . H22 H 1.1658 0.2327 0.0065 0.032 Uiso 1 1 calc R . . H23 H 1.1242 0.3433 -0.0146 0.029 Uiso 1 1 calc R . . H24 H 0.9280 0.3984 0.0199 0.038 Uiso 1 1 calc R . . H25 H 0.7725 0.3395 0.0704 0.031 Uiso 1 1 calc R . . H26 H 0.8213 0.2290 0.0939 0.029 Uiso 1 1 calc R . . H29 H 1.4433 -0.0814 0.1669 0.040 Uiso 1 1 calc R . . H30 H 1.4698 -0.1909 0.1908 0.045 Uiso 1 1 calc R . . H31 H 1.2868 -0.2652 0.1936 0.060 Uiso 1 1 calc R . . H32 H 1.0651 -0.2296 0.1620 0.057 Uiso 1 1 calc R . . H33 H 1.0349 -0.1182 0.1351 0.046 Uiso 1 1 calc R . . H38A H 1.1104 -0.1715 0.3362 0.041 Uiso 1 1 calc R . . H38B H 1.1532 -0.1873 0.2742 0.041 Uiso 1 1 calc R . . H39A H 0.8826 -0.1933 0.3084 0.040 Uiso 1 1 calc R . . H39B H 0.9229 -0.1731 0.2472 0.040 Uiso 1 1 calc R . . H40 H 0.8077 -0.0742 0.2651 0.034 Uiso 1 1 calc R . . H44 H 0.7156 -0.1386 0.4238 0.031 Uiso 1 1 calc R . . H45 H 0.5202 -0.2070 0.4341 0.041 Uiso 1 1 calc R . . H46 H 0.3738 -0.2249 0.3672 0.044 Uiso 1 1 calc R . . H47 H 0.4105 -0.1749 0.2893 0.046 Uiso 1 1 calc R . . H48 H 0.6106 -0.1060 0.2807 0.039 Uiso 1 1 calc R . . H50 H 0.6147 0.0087 0.3156 0.053 Uiso 1 1 calc R . . H51 H 0.5867 0.1218 0.3364 0.065 Uiso 1 1 calc R . . H52 H 0.7345 0.1746 0.3909 0.078 Uiso 1 1 calc R . . H53 H 0.9313 0.1149 0.4230 0.055 Uiso 1 1 calc R . . H54 H 0.9626 0.0025 0.4047 0.046 Uiso 1 1 calc R . . H57 H 1.1447 0.1414 0.2979 0.032 Uiso 1 1 calc R . . H58 H 1.3011 0.2291 0.2795 0.051 Uiso 1 1 calc R . . H59 H 1.5082 0.2080 0.2346 0.042 Uiso 1 1 calc R . . H60 H 1.5658 0.1001 0.2141 0.044 Uiso 1 1 calc R . . H61 H 1.4126 0.0104 0.2309 0.037 Uiso 1 1 calc R . . H65A H 0.7678 0.4535 0.1006 0.046 Uiso 0.484(11) 1 calc PR A 1 H65B H 0.5899 0.4697 0.0930 0.046 Uiso 0.484(11) 1 calc PR A 1 H65C H 0.6959 0.5273 0.1241 0.046 Uiso 0.484(11) 1 calc PR A 1 H66A H 0.8237 0.5490 0.0459 0.055 Uiso 0.484(11) 1 calc PR A 1 H66B H 0.7173 0.4921 0.0150 0.055 Uiso 0.484(11) 1 calc PR A 1 H67A H 0.6219 0.6171 0.0681 0.102 Uiso 0.484(11) 1 calc PR A 1 H67B H 0.5091 0.5582 0.0427 0.102 Uiso 0.484(11) 1 calc PR A 1 H68A H 0.6289 0.5735 -0.0402 0.157 Uiso 0.484(11) 1 calc PR A 1 H68B H 0.7289 0.6369 -0.0140 0.157 Uiso 0.484(11) 1 calc PR A 1 H69A H 0.5202 0.6861 -0.0536 0.082 Uiso 0.484(11) 1 calc PR A 1 H69B H 0.5095 0.6963 0.0108 0.082 Uiso 0.484(11) 1 calc PR A 1 H69C H 0.4124 0.6337 -0.0186 0.082 Uiso 0.484(11) 1 calc PR A 1 H70A H 0.2830 0.7053 -0.1571 0.117 Uiso 0.516(11) 1 calc PR A 2 H70B H 0.3554 0.7360 -0.1020 0.117 Uiso 0.516(11) 1 calc PR A 2 H70C H 0.1832 0.7557 -0.1177 0.117 Uiso 0.516(11) 1 calc PR A 2 H71A H 0.2841 0.6169 -0.0987 0.117 Uiso 0.516(11) 1 calc PR A 2 H71B H 0.1130 0.6424 -0.1067 0.117 Uiso 0.516(11) 1 calc PR A 2 H72A H 0.2717 0.7055 -0.0240 0.117 Uiso 0.516(11) 1 calc PR A 2 H72B H 0.2165 0.6231 -0.0163 0.117 Uiso 0.516(11) 1 calc PR A 2 H73A H 0.0381 0.7177 0.0041 0.117 Uiso 0.516(11) 1 calc PR A 2 H73B H 0.0265 0.7280 -0.0596 0.117 Uiso 0.516(11) 1 calc PR A 2 H74A H -0.1578 0.6590 -0.0344 0.117 Uiso 0.516(11) 1 calc PR A 2 H74B H -0.0447 0.6068 -0.0012 0.117 Uiso 0.516(11) 1 calc PR A 2 H74C H -0.0376 0.6091 -0.0662 0.117 Uiso 0.516(11) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0284(4) 0.0228(4) 0.0276(4) 0.0020(3) 0.0008(4) 0.0002(3) Ag2 0.0223(3) 0.0290(4) 0.0281(4) 0.0044(3) 0.0019(3) -0.0010(3) Cl4 0.0373(14) 0.0224(13) 0.0325(13) 0.0056(10) 0.0077(11) 0.0055(10) Cl5 0.0221(14) 0.074(2) 0.0340(14) 0.0189(14) 0.0009(11) -0.0062(12) F27 0.023(3) 0.031(3) 0.023(3) 0.000(2) 0.005(2) 0.002(2) F55 0.029(3) 0.047(3) 0.030(3) 0.008(2) -0.013(3) -0.008(3) N6 0.025(4) 0.026(5) 0.030(4) 0.006(4) 0.000(3) -0.001(3) N8 0.013(4) 0.029(5) 0.024(4) 0.001(3) 0.004(3) 0.004(3) N13 0.020(4) 0.034(5) 0.030(4) 0.007(4) 0.000(3) -0.006(4) N35 0.026(5) 0.027(5) 0.029(4) 0.005(4) 0.008(3) 0.002(4) N36 0.028(5) 0.019(4) 0.037(5) 0.007(4) -0.003(4) 0.001(4) N41 0.019(4) 0.023(5) 0.032(5) 0.002(4) 0.001(3) -0.008(3) C7 0.033(5) 0.036(6) 0.019(4) -0.004(4) 0.005(4) 0.018(5) C9 0.025(5) 0.032(5) 0.024(5) 0.002(4) 0.009(5) 0.001(5) C10 0.018(5) 0.036(6) 0.032(6) 0.001(5) 0.001(4) 0.002(4) C11 0.034(6) 0.031(6) 0.024(5) 0.003(4) -0.008(4) -0.003(4) C12 0.022(5) 0.037(6) 0.016(5) 0.004(4) -0.007(4) 0.008(4) C14 0.025(5) 0.031(6) 0.019(5) 0.004(4) 0.008(4) 0.004(4) C15 0.037(5) 0.023(5) 0.026(5) 0.005(4) -0.003(5) -0.015(5) C16 0.041(6) 0.034(6) 0.038(6) -0.003(4) 0.002(6) -0.004(5) C17 0.046(7) 0.022(6) 0.056(7) -0.002(5) -0.013(6) -0.007(5) C18 0.028(6) 0.032(6) 0.062(8) 0.011(6) -0.023(5) -0.013(5) C19 0.041(6) 0.033(6) 0.044(7) 0.021(5) 0.005(5) -0.008(5) C20 0.022(5) 0.030(5) 0.030(5) 0.009(4) -0.014(4) -0.001(4) C21 0.018(5) 0.034(6) 0.027(5) -0.011(4) -0.009(4) -0.008(4) C22 0.029(5) 0.029(5) 0.022(4) 0.000(4) 0.001(5) -0.003(5) C23 0.022(5) 0.036(6) 0.016(4) -0.004(4) 0.003(4) -0.003(4) C24 0.033(6) 0.034(6) 0.029(6) 0.008(5) -0.007(4) -0.006(4) C25 0.029(5) 0.017(5) 0.031(5) 0.005(4) -0.006(4) -0.003(4) C26 0.022(5) 0.024(5) 0.027(5) -0.005(4) 0.006(4) 0.000(4) C28 0.041(6) 0.027(5) 0.025(5) -0.003(4) 0.004(4) 0.007(5) C29 0.040(6) 0.024(5) 0.036(6) 0.006(5) -0.007(5) 0.002(4) C30 0.040(7) 0.032(6) 0.041(6) 0.000(5) -0.003(5) 0.009(5) C31 0.078(10) 0.028(6) 0.044(7) -0.004(5) 0.001(6) 0.023(6) C32 0.044(7) 0.031(6) 0.068(8) 0.008(6) 0.009(6) -0.006(5) C33 0.022(6) 0.025(6) 0.067(8) 0.017(5) 0.011(5) 0.011(4) C34 0.029(5) 0.025(6) 0.018(5) -0.001(4) 0.000(4) -0.004(4) C37 0.030(6) 0.023(5) 0.032(5) 0.005(4) -0.001(4) -0.009(4) C38 0.033(6) 0.025(5) 0.043(6) 0.004(4) -0.007(5) 0.003(5) C39 0.037(6) 0.021(5) 0.043(6) 0.004(4) -0.010(5) -0.012(4) C40 0.032(6) 0.026(5) 0.028(5) 0.000(4) 0.001(4) 0.000(4) C42 0.024(5) 0.040(6) 0.019(5) 0.012(4) -0.004(4) -0.004(4) C43 0.027(5) 0.016(5) 0.025(5) 0.005(4) 0.004(4) 0.000(4) C44 0.025(5) 0.029(5) 0.024(5) -0.006(4) 0.005(4) 0.004(4) C45 0.044(6) 0.023(5) 0.036(6) 0.000(5) 0.019(5) 0.004(5) C46 0.032(6) 0.026(6) 0.053(7) -0.001(5) 0.016(5) -0.008(4) C47 0.042(6) 0.018(5) 0.055(7) 0.001(5) 0.014(5) -0.009(5) C48 0.025(5) 0.036(5) 0.037(6) 0.007(4) 0.006(5) -0.010(5) C49 0.024(5) 0.026(5) 0.031(5) 0.005(4) -0.001(4) -0.012(4) C50 0.046(7) 0.035(6) 0.050(7) -0.006(6) -0.003(6) 0.001(5) C51 0.081(9) 0.027(6) 0.055(8) 0.001(6) -0.021(7) 0.010(6) C52 0.125(14) 0.028(7) 0.043(8) -0.001(6) -0.002(8) -0.015(8) C53 0.065(9) 0.046(7) 0.026(6) -0.003(5) 0.009(5) -0.013(6) C54 0.062(8) 0.032(6) 0.022(5) 0.002(4) -0.008(5) -0.003(5) C56 0.036(6) 0.021(5) 0.027(5) 0.006(4) 0.000(4) -0.009(4) C57 0.023(5) 0.030(6) 0.026(5) 0.004(4) -0.004(4) -0.010(4) C58 0.037(7) 0.034(7) 0.056(7) 0.001(5) -0.006(5) 0.009(5) C59 0.034(6) 0.031(6) 0.039(6) 0.009(5) -0.010(5) -0.012(4) C60 0.027(6) 0.048(8) 0.036(6) 0.005(5) -0.008(4) -0.008(5) C61 0.036(6) 0.027(5) 0.030(6) 0.005(4) -0.002(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 C34 2.085(10) . ? Ag1 Cl4 2.334(2) . ? Ag1 Ag2 3.1166(10) . ? Ag2 C7 2.086(11) . ? Ag2 Cl5 2.326(3) . ? F27 C14 1.415(10) . ? F55 C42 1.412(11) . ? N6 C7 1.358(12) . ? N6 N13 1.411(11) . ? N6 C28 1.423(13) . ? N8 C7 1.328(13) . ? N8 C12 1.416(12) . ? N8 C9 1.463(12) . ? N13 C12 1.318(13) . ? N35 C34 1.337(12) . ? N35 N36 1.404(11) . ? N35 C56 1.429(12) . ? N36 C37 1.312(12) . ? N41 C37 1.381(12) . ? N41 C34 1.394(12) . ? N41 C40 1.433(12) . ? C9 C14 1.526(13) . ? C9 C10 1.567(14) . ? C10 C11 1.569(14) . ? C11 C12 1.452(14) . ? C14 C15 1.536(13) . ? C14 C21 1.554(14) . ? C15 C20 1.375(14) . ? C15 C16 1.428(14) . ? C16 C17 1.407(16) . ? C17 C18 1.335(17) . ? C18 C19 1.410(17) . ? C19 C20 1.379(15) . ? C21 C22 1.384(13) . ? C21 C26 1.389(13) . ? C22 C23 1.364(13) . ? C23 C24 1.400(14) . ? C24 C25 1.381(14) . ? C25 C26 1.386(13) . ? C28 C33 1.386(15) . ? C28 C29 1.396(14) . ? C29 C30 1.361(14) . ? C30 C31 1.349(17) . ? C31 C32 1.418(17) . ? C32 C33 1.399(15) . ? C37 C38 1.503(13) . ? C38 C39 1.554(15) . ? C39 C40 1.560(14) . ? C40 C42 1.522(13) . ? C42 C49 1.509(14) . ? C42 C43 1.537(13) . ? C43 C48 1.346(14) . ? C43 C44 1.410(13) . ? C44 C45 1.365(14) . ? C45 C46 1.368(16) . ? C46 C47 1.386(16) . ? C47 C48 1.399(14) . ? C49 C54 1.400(14) . ? C49 C50 1.430(15) . ? C50 C51 1.397(16) . ? C51 C52 1.345(19) . ? C52 C53 1.43(2) . ? C53 C54 1.370(16) . ? C56 C61 1.373(15) . ? C56 C57 1.397(14) . ? C57 C58 1.390(15) . ? C58 C59 1.405(15) . ? C59 C60 1.343(16) . ? C60 C61 1.404(15) . ? C65 C66 1.539(17) . ? C66 C67 1.526(18) . ? C67 C68 1.551(19) . ? C68 C69 1.556(19) . ? C70 C71 1.507(19) . ? C71 C72 1.533(19) . ? C72 C73 1.544(18) . ? C73 C74 1.487(19) . ? C9 H9 1.0800 . ? C10 H10A 1.0800 . ? C10 H10B 1.0800 . ? C11 H11A 1.0800 . ? C11 H11B 1.0800 . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C18 H18 0.9800 . ? C19 H19 0.9800 . ? C20 H20 0.9800 . ? C22 H22 0.9800 . ? C23 H23 0.9800 . ? C24 H24 0.9800 . ? C25 H25 0.9800 . ? C26 H26 0.9800 . ? C29 H29 0.9800 . ? C30 H30 0.9800 . ? C31 H31 0.9800 . ? C32 H32 0.9800 . ? C33 H33 0.9800 . ? C38 H38A 1.0800 . ? C38 H38B 1.0800 . ? C39 H39A 1.0800 . ? C39 H39B 1.0800 . ? C40 H40 1.0800 . ? C44 H44 0.9800 . ? C45 H45 0.9800 . ? C46 H46 0.9800 . ? C47 H47 0.9800 . ? C48 H48 0.9800 . ? C50 H50 0.9800 . ? C51 H51 0.9800 . ? C52 H52 0.9800 . ? C53 H53 0.9800 . ? C54 H54 0.9800 . ? C57 H57 0.9800 . ? C58 H58 0.9800 . ? C59 H59 0.9800 . ? C60 H60 0.9800 . ? C61 H61 0.9800 . ? C65 H65A 1.0800 . ? C65 H65B 1.0800 . ? C65 H65C 1.0800 . ? C66 H66A 1.0800 . ? C66 H66B 1.0800 . ? C67 H67A 1.0800 . ? C67 H67B 1.0800 . ? C68 H68A 1.0800 . ? C68 H68B 1.0800 . ? C69 H69A 1.0800 . ? C69 H69B 1.0800 . ? C69 H69C 1.0800 . ? C70 H70A 1.0800 . ? C70 H70B 1.0800 . ? C70 H70C 1.0800 . ? C71 H71A 1.0800 . ? C71 H71B 1.0800 . ? C72 H72A 1.0800 . ? C72 H72B 1.0800 . ? C73 H73A 1.0800 . ? C73 H73B 1.0800 . ? C74 H74A 1.0800 . ? C74 H74B 1.0800 . ? C74 H74C 1.0800 . ? 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 C34 Ag1 Cl4 168.1(3) . . ? C34 Ag1 Ag2 80.8(3) . . ? Cl4 Ag1 Ag2 97.35(7) . . ? C7 Ag2 Cl5 175.4(3) . . ? C7 Ag2 Ag1 92.7(2) . . ? Cl5 Ag2 Ag1 86.61(8) . . ? C7 N6 N13 113.3(8) . . ? C7 N6 C28 129.2(8) . . ? N13 N6 C28 117.1(8) . . ? C7 N8 C12 110.6(8) . . ? C7 N8 C9 138.4(8) . . ? C12 N8 C9 111.0(8) . . ? C12 N13 N6 103.5(7) . . ? C34 N35 N36 116.1(8) . . ? C34 N35 C56 126.1(9) . . ? N36 N35 C56 117.8(8) . . ? C37 N36 N35 101.0(7) . . ? C37 N41 C34 107.8(7) . . ? C37 N41 C40 114.2(7) . . ? C34 N41 C40 137.9(8) . . ? N8 C7 N6 103.5(8) . . ? N8 C7 Ag2 126.7(7) . . ? N6 C7 Ag2 129.5(7) . . ? N8 C9 C14 110.3(8) . . ? N8 C9 C10 99.9(8) . . ? C14 C9 C10 114.1(8) . . ? C9 C10 C11 106.3(8) . . ? C12 C11 C10 100.0(8) . . ? N13 C12 N8 108.9(8) . . ? N13 C12 C11 138.0(9) . . ? N8 C12 C11 113.0(8) . . ? F27 C14 C9 105.4(7) . . ? F27 C14 C15 107.1(8) . . ? C9 C14 C15 113.0(8) . . ? F27 C14 C21 107.0(7) . . ? C9 C14 C21 111.6(8) . . ? C15 C14 C21 112.2(8) . . ? C20 C15 C16 118.8(9) . . ? C20 C15 C14 122.9(8) . . ? C16 C15 C14 118.2(9) . . ? C17 C16 C15 118.1(11) . . ? C18 C17 C16 123.2(11) . . ? C17 C18 C19 118.0(10) . . ? C20 C19 C18 121.3(10) . . ? C15 C20 C19 120.6(10) . . ? C22 C21 C26 119.3(9) . . ? C22 C21 C14 120.3(9) . . ? C26 C21 C14 120.3(9) . . ? C23 C22 C21 122.2(9) . . ? C22 C23 C24 118.5(9) . . ? C25 C24 C23 120.1(10) . . ? C24 C25 C26 120.6(9) . . ? C25 C26 C21 119.2(9) . . ? C33 C28 C29 119.7(9) . . ? C33 C28 N6 119.9(9) . . ? C29 C28 N6 120.3(9) . . ? C30 C29 C28 119.1(10) . . ? C31 C30 C29 124.0(10) . . ? C30 C31 C32 117.4(10) . . ? C33 C32 C31 120.3(11) . . ? C28 C33 C32 119.4(10) . . ? N35 C34 N41 102.0(9) . . ? N35 C34 Ag1 127.9(7) . . ? N41 C34 Ag1 127.4(7) . . ? N36 C37 N41 113.1(8) . . ? N36 C37 C38 136.6(9) . . ? N41 C37 C38 110.1(8) . . ? C37 C38 C39 101.4(8) . . ? C38 C39 C40 106.0(8) . . ? N41 C40 C42 112.3(8) . . ? N41 C40 C39 101.7(8) . . ? C42 C40 C39 113.0(8) . . ? F55 C42 C49 106.1(7) . . ? F55 C42 C40 105.3(7) . . ? C49 C42 C40 112.2(8) . . ? F55 C42 C43 107.2(7) . . ? C49 C42 C43 113.7(8) . . ? C40 C42 C43 111.6(8) . . ? C48 C43 C44 119.2(9) . . ? C48 C43 C42 122.7(8) . . ? C44 C43 C42 118.0(8) . . ? C45 C44 C43 120.4(10) . . ? C44 C45 C46 118.1(10) . . ? C45 C46 C47 124.1(10) . . ? C46 C47 C48 115.5(11) . . ? C43 C48 C47 122.6(9) . . ? C54 C49 C50 118.6(10) . . ? C54 C49 C42 121.5(9) . . ? C50 C49 C42 119.8(8) . . ? C51 C50 C49 118.9(11) . . ? C52 C51 C50 122.5(13) . . ? C51 C52 C53 118.5(12) . . ? C54 C53 C52 121.0(11) . . ? C53 C54 C49 120.4(11) . . ? C61 C56 C57 122.2(9) . . ? C61 C56 N35 118.1(9) . . ? C57 C56 N35 119.7(9) . . ? C58 C57 C56 117.5(9) . . ? C57 C58 C59 121.2(10) . . ? C60 C59 C58 119.0(10) . . ? C59 C60 C61 122.1(10) . . ? C56 C61 C60 118.0(9) . . ? C67 C66 C65 105.9(14) . . ? C66 C67 C68 106.6(15) . . ? C67 C68 C69 105.9(17) . . ? C70 C71 C72 112.5(18) . . ? C71 C72 C73 102.9(15) . . ? C74 C73 C72 113.5(18) . . ? N8 C9 H9 110.7 . . ? C14 C9 H9 110.7 . . ? C10 C9 H9 110.7 . . ? C9 C10 H10A 110.5 . . ? C11 C10 H10A 110.5 . . ? C9 C10 H10B 110.5 . . ? C11 C10 H10B 110.5 . . ? H10A C10 H10B 108.6 . . ? C12 C11 H11A 111.8 . . ? C10 C11 H11A 111.8 . . ? C12 C11 H11B 111.8 . . ? C10 C11 H11B 111.8 . . ? H11A C11 H11B 109.5 . . ? C17 C16 H16 121.0 . . ? C15 C16 H16 121.0 . . ? C18 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C15 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C23 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? C22 C23 H23 120.8 . . ? C24 C23 H23 120.8 . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C25 C26 H26 120.4 . . ? C21 C26 H26 120.4 . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C31 C30 H30 118.0 . . ? C29 C30 H30 118.0 . . ? C30 C31 H31 121.3 . . ? C32 C31 H31 121.3 . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C28 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C37 C38 H38A 111.5 . . ? C39 C38 H38A 111.5 . . ? C37 C38 H38B 111.5 . . ? C39 C38 H38B 111.5 . . ? H38A C38 H38B 109.3 . . ? C38 C39 H39A 110.5 . . ? C40 C39 H39A 110.5 . . ? C38 C39 H39B 110.5 . . ? C40 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? N41 C40 H40 109.9 . . ? C42 C40 H40 109.9 . . ? C39 C40 H40 109.9 . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C44 C45 H45 121.0 . . ? C46 C45 H45 121.0 . . ? C45 C46 H46 117.9 . . ? C47 C46 H46 117.9 . . ? C46 C47 H47 122.3 . . ? C48 C47 H47 122.3 . . ? C43 C48 H48 118.7 . . ? C47 C48 H48 118.7 . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C52 C51 H51 118.7 . . ? C50 C51 H51 118.7 . . ? C51 C52 H52 120.8 . . ? C53 C52 H52 120.8 . . ? C54 C53 H53 119.5 . . ? C52 C53 H53 119.5 . . ? C53 C54 H54 119.8 . . ? C49 C54 H54 119.8 . . ? C58 C57 H57 121.3 . . ? C56 C57 H57 121.3 . . ? C57 C58 H58 119.4 . . ? C59 C58 H58 119.4 . . ? C60 C59 H59 120.5 . . ? C58 C59 H59 120.5 . . ? C59 C60 H60 119.0 . . ? C61 C60 H60 119.0 . . ? C56 C61 H61 121.0 . . ? C60 C61 H61 121.0 . . ? C66 C65 H65A 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C66 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C67 C66 H66A 110.6 . . ? C65 C66 H66A 110.6 . . ? C67 C66 H66B 110.6 . . ? C65 C66 H66B 110.6 . . ? H66A C66 H66B 108.7 . . ? C66 C67 H67A 110.4 . . ? C68 C67 H67A 110.4 . . ? C66 C67 H67B 110.4 . . ? C68 C67 H67B 110.4 . . ? H67A C67 H67B 108.6 . . ? C67 C68 H68A 110.6 . . ? C69 C68 H68A 110.6 . . ? C67 C68 H68B 110.6 . . ? C69 C68 H68B 110.6 . . ? H68A C68 H68B 108.7 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.4 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C70 C71 H71A 109.1 . . ? C72 C71 H71A 109.1 . . ? C70 C71 H71B 109.1 . . ? C72 C71 H71B 109.1 . . ? H71A C71 H71B 107.8 . . ? C71 C72 H72A 111.2 . . ? C73 C72 H72A 111.1 . . ? C71 C72 H72B 111.2 . . ? C73 C72 H72B 111.2 . . ? H72A C72 H72B 109.1 . . ? C74 C73 H73A 108.9 . . ? C72 C73 H73A 108.9 . . ? C74 C73 H73B 108.8 . . ? C72 C73 H73B 108.9 . . ? H73A C73 H73B 107.7 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.4 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.266 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.130 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; # CIF Copied by cif2cif, version 0.0.8 - beta ( 2 Apr 98) data_13 _chemical_compound_source 'LOC ETH Zurich' _exptl_crystal_description 'Cube' _exptl_crystal_size_max .225 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .105 _exptl_crystal_F_000 2320.0 _exptl_crystal_colour 'Colourless' _diffrn_ambient_temperature 173 _cell_measurement_temperature 173 _refine_ls_hydrogen_treatment 'constr' # Submission details _diffrn_measurement_device 'KappaCCD' _computing_data_collection 'KappaCCD' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 35 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type 'X=UH' _diffrn_orient_matrix_UB_11 0.09216 _diffrn_orient_matrix_UB_12 -0.03598 _diffrn_orient_matrix_UB_13 0.02345 _diffrn_orient_matrix_UB_21 -0.01127 _diffrn_orient_matrix_UB_22 -0.04304 _diffrn_orient_matrix_UB_23 -0.02177 _diffrn_orient_matrix_UB_31 0.01316 _diffrn_orient_matrix_UB_32 0.01279 _diffrn_orient_matrix_UB_33 -0.03211 _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.489 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 601.866 _diffrn_radiation_type ' MoK\a' loop_ _symmetry_equiv_pos_as_xyz '+X,+Y,+Z' '-X+ 1/2,-Y,+Z+ 1/2' '+X+ 1/2,-Y+ 1/2,-Z' '-X,+Y+ 1/2,-Z+ 1/2' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_cell_setting 'Orthorhombic' _chemical_formula_moiety 'C24 H20 Au Cl F N3 ' _chemical_formula_sum 'C24 H20 Au Cl F N3 ' _chemical_name_systematic ; ? ; _cell_length_a 9.8352(2) _cell_length_b 20.1882(4) _cell_length_c 27.0406(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5369.0(2) _diffrn_reflns_av_R_equivalents 0.09 _diffrn_reflns_number 30180 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_full 27.48 _cell_measurement_reflns_used 163030 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _diffrn_measurement_method 'CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap # Absorption correction loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.024 0 0 -1 0.076 1 0 -4 0.127 -1 0 0 0.113 0 1 0 0.138 1 -8 0 0.052 1 -2 0 0.050 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.354 _exptl_absorpt_correction_T_max 0.590 _exptl_absorpt_process_details ; Gaussian integration (Coppens, 1970) ; 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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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' _exptl_absorpt_coefficient_mu 5.599 _reflns_number_total 11306 _reflns_number_gt 9598 _reflns_threshold_expression >2sigma(I) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+ (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.086(17) _refine_ls_number_reflns 11306 _refine_ls_number_parameters 541 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.2250 _refine_ls_wR_factor_gt 0.2182 _refine_ls_goodness_of_fit_ref 1.518 _refine_ls_restrained_S_all 1.518 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.005 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 0.55934(6) 0.59356(3) 0.24857(2) 0.03702(18) Uani 1 1 d . . . Au31 Au 0.59281(6) 0.48499(3) 0.33953(2) 0.03678(18) Uani 1 1 d . . . Cl29 Cl 0.6756(5) 0.6810(2) 0.28163(18) 0.0467(10) Uani 1 1 d . . . Cl60 Cl 0.8015(5) 0.4494(3) 0.31440(19) 0.0570(13) Uani 1 1 d . . . F28 F 0.5638(11) 0.3999(5) 0.1233(3) 0.050(3) Uani 1 1 d . . . F59 F 0.3909(10) 0.6228(4) 0.4656(3) 0.042(2) Uani 1 1 d . . . N1 N 0.4771(15) 0.4562(7) 0.2127(5) 0.042(3) Uani 1 1 d . . . N3 N 0.3027(16) 0.5177(8) 0.2230(6) 0.049(4) Uani 1 1 d . . . N4 N 0.2575(16) 0.4534(7) 0.2152(6) 0.049(4) Uani 1 1 d . . . N32 N 0.3719(13) 0.5762(7) 0.3711(4) 0.033(3) Uani 1 1 d . . . N34 N 0.2893(14) 0.4796(8) 0.3617(5) 0.043(3) Uani 1 1 d . . . N35 N 0.1827(15) 0.5184(8) 0.3751(5) 0.044(3) Uani 1 1 d . . . C2 C 0.4494(15) 0.5195(8) 0.2240(6) 0.034(3) Uani 1 1 d . . . C5 C 0.354(2) 0.4219(9) 0.2106(8) 0.053(5) Uani 1 1 d . . . C6 C 0.397(3) 0.3477(9) 0.2027(9) 0.075(8) Uani 1 1 d . . . C7 C 0.554(2) 0.3486(9) 0.2163(9) 0.063(6) Uani 1 1 d . . . C8 C 0.6035(18) 0.4185(7) 0.2067(7) 0.042(4) Uani 1 1 d . . . C9 C 0.2108(18) 0.5702(8) 0.2351(7) 0.041(4) Uani 1 1 d . . . C10 C 0.241(3) 0.6366(10) 0.2247(9) 0.072(7) Uani 1 1 d . . . C11 C 0.158(2) 0.6838(9) 0.2336(8) 0.051(5) Uani 1 1 d . . . C12 C 0.034(2) 0.6687(11) 0.2574(8) 0.060(6) Uani 1 1 d . . . C13 C 0.004(2) 0.6034(9) 0.2685(7) 0.049(5) Uani 1 1 d . . . C14 C 0.0943(19) 0.5556(8) 0.2579(6) 0.043(4) Uani 1 1 d . . . C15 C 0.6738(16) 0.4270(10) 0.1571(6) 0.045(5) Uani 1 1 d . . . C16 C 0.806(2) 0.3818(8) 0.1517(6) 0.047(5) Uani 1 1 d . . . C17 C 0.8823(19) 0.3729(11) 0.1893(9) 0.063(6) Uani 1 1 d . . . C18 C 1.006(2) 0.3357(11) 0.1838(8) 0.056(5) Uani 1 1 d . . . C19 C 1.020(3) 0.3075(9) 0.1385(9) 0.062(6) Uani 1 1 d . . . C20 C 0.945(2) 0.3164(9) 0.1007(9) 0.058(6) Uani 1 1 d . . . C21 C 0.818(2) 0.3544(9) 0.1048(8) 0.054(5) Uani 1 1 d . . . C22 C 0.6893(19) 0.4969(8) 0.1440(7) 0.047(5) Uani 1 1 d . . . C23 C 0.804(2) 0.5332(9) 0.1606(9) 0.060(6) Uani 1 1 d . . . C24 C 0.830(3) 0.5930(11) 0.1460(9) 0.068(6) Uani 1 1 d . . . C25 C 0.729(3) 0.6307(12) 0.1171(7) 0.066(6) Uani 1 1 d . . . C26 C 0.624(4) 0.5990(10) 0.0994(11) 0.098(11) Uani 1 1 d . . . C27 C 0.596(2) 0.5308(10) 0.1133(8) 0.060(5) Uani 1 1 d . . . C33 C 0.4009(17) 0.5127(8) 0.3603(5) 0.034(3) Uani 1 1 d . . . C36 C 0.2304(15) 0.5796(9) 0.3804(5) 0.036(4) Uani 1 1 d . . . C37 C 0.1821(19) 0.6438(10) 0.3864(7) 0.049(5) Uani 1 1 d . . . C38 C 0.3147(18) 0.6876(9) 0.3729(6) 0.041(4) Uani 1 1 d . . . C39 C 0.4375(16) 0.6432(8) 0.3817(6) 0.036(4) Uani 1 1 d . . . C40 C 0.2636(19) 0.4117(8) 0.3506(6) 0.043(4) Uani 1 1 d . . . C41 C 0.364(2) 0.3634(10) 0.3520(8) 0.060(6) Uani 1 1 d . . . C42 C 0.332(2) 0.2991(9) 0.3382(11) 0.070(7) Uani 1 1 d . . . C43 C 0.214(3) 0.2861(11) 0.3223(8) 0.067(7) Uani 1 1 d . . . C44 C 0.106(2) 0.3308(9) 0.3238(8) 0.061(6) Uani 1 1 d . . . C45 C 0.1353(18) 0.3942(8) 0.3348(7) 0.043(4) Uani 1 1 d . . . C46 C 0.4951(16) 0.6468(8) 0.4320(6) 0.039(4) Uani 1 1 d . . . C47 C 0.5224(17) 0.7174(9) 0.4494(6) 0.040(4) Uani 1 1 d . . . C48 C 0.435(2) 0.7524(7) 0.4797(6) 0.044(4) Uani 1 1 d . . . C49 C 0.454(3) 0.8153(11) 0.4929(7) 0.062(6) Uani 1 1 d . . . C50 C 0.570(2) 0.8510(7) 0.4736(6) 0.046(5) Uani 1 1 d . . . C51 C 0.6621(18) 0.8184(9) 0.4404(7) 0.047(5) Uani 1 1 d . . . C52 C 0.6288(16) 0.7526(7) 0.4283(6) 0.034(3) Uani 1 1 d . . . C53 C 0.6178(19) 0.6013(8) 0.4409(6) 0.042(4) Uani 1 1 d . . . C54 C 0.623(3) 0.5656(12) 0.4865(9) 0.074(7) Uani 1 1 d . . . C55 C 0.747(3) 0.5203(9) 0.4896(11) 0.079(9) Uani 1 1 d . . . C56 C 0.842(3) 0.5169(16) 0.4558(9) 0.095(11) Uani 1 1 d . . . C57 C 0.832(2) 0.5578(9) 0.4166(9) 0.059(6) Uani 1 1 d . . . C58 C 0.7272(19) 0.5991(11) 0.4054(7) 0.052(5) Uani 1 1 d . . . H6A H 0.3818 0.3325 0.1649 0.090 Uiso 1 1 calc R . . H6B H 0.3417 0.3150 0.2269 0.090 Uiso 1 1 calc R . . H7A H 0.5692 0.3355 0.2546 0.075 Uiso 1 1 calc R . . H7B H 0.6096 0.3138 0.1935 0.075 Uiso 1 1 calc R . . H8 H 0.6732 0.4326 0.2357 0.050 Uiso 1 1 calc R . . H10 H 0.3287 0.6472 0.2098 0.087 Uiso 1 1 calc R . . H11 H 0.1801 0.7294 0.2242 0.061 Uiso 1 1 calc R . . H12 H -0.0294 0.7041 0.2661 0.072 Uiso 1 1 calc R . . H13 H -0.0832 0.5921 0.2839 0.059 Uiso 1 1 calc R . . H14 H 0.0745 0.5096 0.2670 0.052 Uiso 1 1 calc R . . H17 H 0.8570 0.3913 0.2216 0.075 Uiso 1 1 calc R . . H18 H 1.0734 0.3311 0.2102 0.067 Uiso 1 1 calc R . . H19 H 1.0968 0.2769 0.1345 0.074 Uiso 1 1 calc R . . H20 H 0.9719 0.2978 0.0687 0.069 Uiso 1 1 calc R . . H21 H 0.7510 0.3596 0.0782 0.065 Uiso 1 1 calc R . . H23 H 0.8659 0.5122 0.1841 0.072 Uiso 1 1 calc R . . H24 H 0.9170 0.6134 0.1544 0.082 Uiso 1 1 calc R . . H25 H 0.7405 0.6783 0.1113 0.080 Uiso 1 1 calc R . . H26 H 0.5636 0.6215 0.0761 0.118 Uiso 1 1 calc R . . H27 H 0.5132 0.5087 0.1017 0.072 Uiso 1 1 calc R . . H37A H 0.1492 0.6526 0.4239 0.059 Uiso 1 1 calc R . . H37B H 0.0991 0.6540 0.3614 0.059 Uiso 1 1 calc R . . H38A H 0.3110 0.7034 0.3347 0.049 Uiso 1 1 calc R . . H38B H 0.3198 0.7310 0.3962 0.049 Uiso 1 1 calc R . . H39 H 0.5154 0.6535 0.3547 0.043 Uiso 1 1 calc R . . H41 H 0.4564 0.3746 0.3627 0.072 Uiso 1 1 calc R . . H42 H 0.4002 0.2639 0.3406 0.084 Uiso 1 1 calc R . . H43 H 0.1971 0.2422 0.3082 0.080 Uiso 1 1 calc R . . H44 H 0.0121 0.3167 0.3172 0.074 Uiso 1 1 calc R . . H45 H 0.0650 0.4283 0.3314 0.052 Uiso 1 1 calc R . . H48 H 0.3535 0.7296 0.4921 0.053 Uiso 1 1 calc R . . H49 H 0.3906 0.8372 0.5155 0.075 Uiso 1 1 calc R . . H50 H 0.5857 0.8973 0.4831 0.055 Uiso 1 1 calc R . . H51 H 0.7428 0.8405 0.4270 0.056 Uiso 1 1 calc R . . H52 H 0.6845 0.7302 0.4034 0.041 Uiso 1 1 calc R . . H54 H 0.5542 0.5697 0.5126 0.089 Uiso 1 1 calc R . . H55 H 0.7554 0.4919 0.5188 0.095 Uiso 1 1 calc R . . H56 H 0.9181 0.4857 0.4589 0.114 Uiso 1 1 calc R . . H57 H 0.9091 0.5579 0.3935 0.071 Uiso 1 1 calc R . . H58 H 0.7260 0.6256 0.3751 0.063 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 0.0404(4) 0.0346(3) 0.0361(3) -0.0018(3) 0.0059(3) 0.0008(2) Au31 0.0279(3) 0.0453(3) 0.0371(3) -0.0106(3) -0.0006(3) 0.0025(3) Cl29 0.049(3) 0.034(2) 0.057(3) -0.0055(18) 0.010(2) -0.0097(19) Cl60 0.033(2) 0.088(4) 0.051(3) -0.025(2) -0.003(2) 0.008(2) F28 0.051(6) 0.063(6) 0.035(5) -0.016(4) -0.013(4) -0.017(5) F59 0.043(6) 0.044(5) 0.039(5) 0.001(4) 0.014(4) -0.002(4) N1 0.036(8) 0.039(8) 0.049(9) -0.013(6) 0.008(6) -0.015(6) N3 0.048(9) 0.047(9) 0.053(9) -0.001(8) -0.001(7) -0.004(8) N4 0.041(9) 0.034(8) 0.072(11) 0.005(7) 0.003(8) -0.006(7) N32 0.029(7) 0.049(8) 0.021(6) 0.001(5) -0.003(5) -0.003(6) N34 0.036(7) 0.062(10) 0.033(7) 0.012(7) -0.012(6) -0.015(8) N35 0.044(8) 0.051(9) 0.037(7) -0.007(7) -0.007(6) 0.023(8) C2 0.024(7) 0.037(8) 0.040(8) 0.006(7) 0.001(6) -0.016(7) C5 0.050(11) 0.036(10) 0.072(14) -0.001(9) -0.014(10) 0.009(9) C6 0.11(2) 0.021(9) 0.092(16) -0.021(9) -0.052(16) 0.018(11) C7 0.060(13) 0.041(10) 0.086(15) 0.002(10) 0.039(12) -0.001(9) C8 0.034(8) 0.020(8) 0.072(12) -0.020(7) 0.013(8) -0.006(7) C9 0.034(9) 0.040(9) 0.048(10) 0.013(7) -0.007(7) -0.009(7) C10 0.083(17) 0.037(12) 0.096(18) 0.021(11) -0.029(14) -0.020(11) C11 0.048(11) 0.028(9) 0.077(14) 0.007(8) 0.006(9) -0.001(8) C12 0.051(11) 0.072(14) 0.057(13) -0.011(10) -0.008(10) 0.029(10) C13 0.041(10) 0.054(12) 0.053(11) -0.017(9) -0.002(8) 0.008(9) C14 0.050(10) 0.043(9) 0.036(9) 0.006(7) 0.028(8) 0.012(8) C15 0.032(8) 0.082(13) 0.022(7) -0.026(8) -0.004(7) -0.017(8) C16 0.078(14) 0.027(8) 0.035(10) 0.001(7) 0.008(9) -0.003(8) C17 0.031(10) 0.092(16) 0.065(13) 0.025(11) 0.022(9) 0.020(10) C18 0.045(11) 0.075(14) 0.049(11) -0.010(10) 0.022(9) -0.008(10) C19 0.080(16) 0.031(10) 0.075(15) -0.004(9) 0.032(13) 0.016(10) C20 0.067(14) 0.039(10) 0.067(14) -0.009(9) 0.045(12) 0.010(10) C21 0.059(13) 0.034(10) 0.071(13) -0.016(9) 0.013(10) -0.008(9) C22 0.047(10) 0.027(9) 0.066(12) -0.025(7) -0.008(9) 0.004(7) C23 0.057(12) 0.035(10) 0.087(15) -0.007(10) -0.036(12) -0.006(8) C24 0.083(16) 0.041(11) 0.080(16) -0.012(10) 0.001(12) 0.006(11) C25 0.091(19) 0.070(15) 0.038(11) 0.016(10) 0.012(11) 0.002(14) C26 0.16(3) 0.021(10) 0.11(2) -0.013(11) -0.05(2) 0.036(14) C27 0.056(12) 0.064(13) 0.060(12) 0.010(9) 0.009(10) 0.000(11) C33 0.052(9) 0.039(8) 0.012(6) -0.006(6) 0.009(6) -0.011(8) C36 0.025(7) 0.060(11) 0.022(7) -0.014(7) 0.016(6) -0.010(7) C37 0.032(9) 0.069(13) 0.047(11) 0.007(9) 0.021(8) 0.009(9) C38 0.048(10) 0.045(10) 0.029(8) -0.004(7) -0.024(8) 0.010(8) C39 0.029(8) 0.037(8) 0.042(9) -0.004(7) 0.010(7) -0.007(7) C40 0.055(11) 0.030(8) 0.044(10) -0.004(7) 0.008(8) -0.017(8) C41 0.046(11) 0.052(12) 0.080(15) -0.020(10) -0.014(10) -0.003(9) C42 0.042(11) 0.021(9) 0.15(2) -0.015(12) -0.011(14) 0.002(7) C43 0.098(19) 0.051(13) 0.052(12) -0.007(9) -0.011(12) -0.030(13) C44 0.056(12) 0.029(9) 0.099(17) 0.000(9) -0.039(12) -0.008(9) C45 0.044(9) 0.039(9) 0.045(10) -0.004(7) -0.007(8) -0.002(7) C46 0.029(8) 0.047(10) 0.041(9) 0.005(7) 0.021(7) 0.004(7) C47 0.039(10) 0.049(10) 0.032(8) -0.013(7) -0.002(7) 0.012(8) C48 0.059(12) 0.029(8) 0.043(9) 0.012(7) -0.009(9) -0.015(8) C49 0.078(15) 0.067(14) 0.042(11) -0.022(9) 0.001(10) 0.002(12) C50 0.072(14) 0.019(7) 0.048(10) -0.001(6) -0.026(10) 0.002(8) C51 0.034(9) 0.061(12) 0.045(10) -0.010(8) -0.026(8) 0.005(8) C52 0.038(9) 0.031(8) 0.032(8) -0.006(6) -0.003(7) -0.009(7) C53 0.056(11) 0.024(8) 0.045(9) -0.004(7) 0.000(8) 0.021(7) C54 0.088(18) 0.079(16) 0.056(13) 0.022(11) -0.037(13) -0.017(13) C55 0.093(18) 0.021(9) 0.12(2) 0.005(11) -0.067(17) 0.022(11) C56 0.068(15) 0.15(3) 0.066(15) -0.054(17) -0.034(12) 0.082(18) C57 0.050(12) 0.033(10) 0.094(17) -0.024(10) -0.021(12) 0.010(9) C58 0.047(11) 0.072(13) 0.037(9) -0.021(9) -0.017(8) -0.017(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C2 1.961(15) . ? Au1 Cl29 2.285(4) . ? Au1 Au31 3.3108(9) . ? Au31 C33 2.047(17) . ? Au31 Cl60 2.279(5) . ? F28 C15 1.519(16) . ? F59 C46 1.454(17) . ? N1 C2 1.34(2) . ? N1 C5 1.40(2) . ? N1 C8 1.47(2) . ? N3 N4 1.39(2) . ? N3 C9 1.43(2) . ? N3 C2 1.44(2) . ? N4 C5 1.15(2) . ? N32 C33 1.34(2) . ? N32 C36 1.417(19) . ? N32 C39 1.53(2) . ? N34 C33 1.29(2) . ? N34 N35 1.36(2) . ? N34 C40 1.43(2) . ? N35 C36 1.33(2) . ? C5 C6 1.57(2) . ? C6 C7 1.59(3) . ? C7 C8 1.51(2) . ? C8 C15 1.52(2) . ? C9 C14 1.33(2) . ? C9 C10 1.40(3) . ? C10 C11 1.27(3) . ? C11 C12 1.41(3) . ? C12 C13 1.39(3) . ? C13 C14 1.34(2) . ? C15 C22 1.46(3) . ? C15 C16 1.59(3) . ? C16 C17 1.28(3) . ? C16 C21 1.39(3) . ? C17 C18 1.44(3) . ? C18 C19 1.36(3) . ? C19 C20 1.28(3) . ? C20 C21 1.47(3) . ? C22 C27 1.41(3) . ? C22 C23 1.42(2) . ? C23 C24 1.29(3) . ? C24 C25 1.47(3) . ? C25 C26 1.30(4) . ? C26 C27 1.45(3) . ? C36 C37 1.39(3) . ? C37 C38 1.62(3) . ? C38 C39 1.52(2) . ? C39 C46 1.47(2) . ? C40 C45 1.38(2) . ? C40 C41 1.39(3) . ? C41 C42 1.39(3) . ? C42 C43 1.27(3) . ? C43 C44 1.39(3) . ? C44 C45 1.35(2) . ? C46 C47 1.53(2) . ? C46 C53 1.54(2) . ? C47 C48 1.38(2) . ? C47 C52 1.39(2) . ? C48 C49 1.33(2) . ? C49 C50 1.45(3) . ? C50 C51 1.43(3) . ? C51 C52 1.41(2) . ? C53 C54 1.43(3) . ? C53 C58 1.44(3) . ? C54 C55 1.53(3) . ? C55 C56 1.31(4) . ? C56 C57 1.35(4) . ? C57 C58 1.36(3) . ? C6 H6A 1.0800 . ? C6 H6B 1.0800 . ? C7 H7A 1.0800 . ? C7 H7B 1.0800 . ? C8 H8 1.0800 . ? C10 H10 0.9800 . ? C11 H11 0.9800 . ? C12 H12 0.9800 . ? C13 H13 0.9800 . ? C14 H14 0.9800 . ? C17 H17 0.9800 . ? C18 H18 0.9800 . ? C19 H19 0.9800 . ? C20 H20 0.9800 . ? C21 H21 0.9800 . ? C23 H23 0.9800 . ? C24 H24 0.9800 . ? C25 H25 0.9800 . ? C26 H26 0.9800 . ? C27 H27 0.9800 . ? C37 H37A 1.0800 . ? C37 H37B 1.0800 . ? C38 H38A 1.0800 . ? C38 H38B 1.0800 . ? C39 H39 1.0800 . ? C41 H41 0.9800 . ? C42 H42 0.9800 . ? C43 H43 0.9800 . ? C44 H44 0.9800 . ? C45 H45 0.9800 . ? C48 H48 0.9800 . ? C49 H49 0.9800 . ? C50 H50 0.9800 . ? C51 H51 0.9800 . ? C52 H52 0.9800 . ? C54 H54 0.9800 . ? C55 H55 0.9800 . ? C56 H56 0.9800 . ? C57 H57 0.9800 . ? C58 H58 0.9800 . ? 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 C2 Au1 Cl29 175.8(5) . . ? C2 Au1 Au31 78.6(4) . . ? Cl29 Au1 Au31 99.84(12) . . ? C33 Au31 Cl60 177.0(4) . . ? C33 Au31 Au1 86.0(4) . . ? Cl60 Au31 Au1 94.41(15) . . ? C2 N1 C5 107.7(14) . . ? C2 N1 C8 133.7(13) . . ? C5 N1 C8 118.4(13) . . ? N4 N3 C9 121.7(15) . . ? N4 N3 C2 110.3(15) . . ? C9 N3 C2 127.4(16) . . ? C5 N4 N3 105.7(17) . . ? C33 N32 C36 107.0(13) . . ? C33 N32 C39 142.8(14) . . ? C36 N32 C39 109.8(13) . . ? C33 N34 N35 111.4(15) . . ? C33 N34 C40 130.3(16) . . ? N35 N34 C40 118.3(14) . . ? C36 N35 N34 107.0(14) . . ? N1 C2 N3 100.0(13) . . ? N1 C2 Au1 133.7(12) . . ? N3 C2 Au1 125.2(13) . . ? N4 C5 N1 116.0(17) . . ? N4 C5 C6 140(2) . . ? N1 C5 C6 103.8(17) . . ? C5 C6 C7 103.0(16) . . ? C8 C7 C6 106.3(17) . . ? N1 C8 C7 101.2(14) . . ? N1 C8 C15 115.2(16) . . ? C7 C8 C15 113.6(14) . . ? C14 C9 C10 118.9(19) . . ? C14 C9 N3 118.9(15) . . ? C10 C9 N3 122.1(19) . . ? C11 C10 C9 123(2) . . ? C10 C11 C12 118.3(19) . . ? C13 C12 C11 119.5(17) . . ? C14 C13 C12 119.6(19) . . ? C9 C14 C13 120.5(17) . . ? C22 C15 C8 111.8(14) . . ? C22 C15 F28 106.0(14) . . ? C8 C15 F28 99.6(12) . . ? C22 C15 C16 116.4(14) . . ? C8 C15 C16 112.9(15) . . ? F28 C15 C16 108.5(13) . . ? C17 C16 C21 128(2) . . ? C17 C16 C15 119.1(16) . . ? C21 C16 C15 112.6(17) . . ? C16 C17 C18 119(2) . . ? C19 C18 C17 114(2) . . ? C20 C19 C18 127(2) . . ? C19 C20 C21 120.3(19) . . ? C16 C21 C20 111(2) . . ? C27 C22 C23 116.8(17) . . ? C27 C22 C15 122.8(16) . . ? C23 C22 C15 120.4(17) . . ? C24 C23 C22 123(2) . . ? C23 C24 C25 121(2) . . ? C26 C25 C24 118(2) . . ? C25 C26 C27 121(2) . . ? C22 C27 C26 119(2) . . ? N34 C33 N32 108.0(15) . . ? N34 C33 Au31 130.7(13) . . ? N32 C33 Au31 121.0(11) . . ? N35 C36 C37 139.4(16) . . ? N35 C36 N32 106.4(14) . . ? C37 C36 N32 113.6(14) . . ? C36 C37 C38 102.1(13) . . ? C39 C38 C37 106.3(13) . . ? C46 C39 C38 114.9(13) . . ? C46 C39 N32 112.3(13) . . ? C38 C39 N32 99.1(13) . . ? C45 C40 C41 118.7(16) . . ? C45 C40 N34 118.3(16) . . ? C41 C40 N34 122.9(16) . . ? C40 C41 C42 119.2(18) . . ? C43 C42 C41 119.6(19) . . ? C42 C43 C44 123.8(19) . . ? C45 C44 C43 117.2(18) . . ? C44 C45 C40 120.7(17) . . ? F59 C46 C39 106.8(13) . . ? F59 C46 C47 104.0(12) . . ? C39 C46 C47 113.5(14) . . ? F59 C46 C53 104.9(13) . . ? C39 C46 C53 114.7(14) . . ? C47 C46 C53 111.8(14) . . ? C48 C47 C52 116.8(16) . . ? C48 C47 C46 123.4(15) . . ? C52 C47 C46 119.0(14) . . ? C49 C48 C47 123.6(19) . . ? C48 C49 C50 119.5(19) . . ? C51 C50 C49 119.6(16) . . ? C52 C51 C50 115.6(17) . . ? C47 C52 C51 124.4(16) . . ? C54 C53 C58 122.3(19) . . ? C54 C53 C46 117.5(18) . . ? C58 C53 C46 120.1(15) . . ? C53 C54 C55 112(2) . . ? C56 C55 C54 124(2) . . ? C55 C56 C57 118(2) . . ? C56 C57 C58 127(2) . . ? C57 C58 C53 116(2) . . ? C5 C6 H6A 111.2 . . ? C7 C6 H6A 111.2 . . ? C5 C6 H6B 111.2 . . ? C7 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? C8 C7 H7A 110.5 . . ? C6 C7 H7A 110.5 . . ? C8 C7 H7B 110.5 . . ? C6 C7 H7B 110.5 . . ? H7A C7 H7B 108.7 . . ? N1 C8 H8 108.8 . . ? C7 C8 H8 108.8 . . ? C15 C8 H8 108.8 . . ? C11 C10 H10 118.5 . . ? C9 C10 H10 118.5 . . ? C10 C11 H11 120.9 . . ? C12 C11 H11 120.9 . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C9 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 H18 123.2 . . ? C17 C18 H18 123.2 . . ? C20 C19 H19 116.4 . . ? C18 C19 H19 116.4 . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C16 C21 H21 124.7 . . ? C20 C21 H21 124.7 . . ? C24 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.3 . . ? C22 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C36 C37 H37A 111.4 . . ? C38 C37 H37A 111.4 . . ? C36 C37 H37B 111.4 . . ? C38 C37 H37B 111.4 . . ? H37A C37 H37B 109.2 . . ? C39 C38 H38A 110.5 . . ? C37 C38 H38A 110.5 . . ? C39 C38 H38B 110.5 . . ? C37 C38 H38B 110.5 . . ? H38A C38 H38B 108.7 . . ? C46 C39 H39 110.0 . . ? C38 C39 H39 110.0 . . ? N32 C39 H39 110.0 . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C42 C43 H43 118.1 . . ? C44 C43 H43 118.1 . . ? C45 C44 H44 121.4 . . ? C43 C44 H44 121.4 . . ? C44 C45 H45 119.7 . . ? C40 C45 H45 119.7 . . ? C49 C48 H48 118.2 . . ? C47 C48 H48 118.2 . . ? C48 C49 H49 120.2 . . ? C50 C49 H49 120.2 . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C52 C51 H51 122.2 . . ? C50 C51 H51 122.2 . . ? C47 C52 H52 117.8 . . ? C51 C52 H52 117.8 . . ? C53 C54 H54 123.9 . . ? C55 C54 H54 123.9 . . ? C56 C55 H55 117.9 . . ? C54 C55 H55 117.8 . . ? C55 C56 H56 121.2 . . ? C57 C56 H56 121.2 . . ? C56 C57 H57 116.4 . . ? C58 C57 H57 116.4 . . ? C57 C58 H58 122.0 . . ? C53 C58 H58 122.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Au1 Au31 C33 -77.0(6) . . . . ? Cl29 Au1 Au31 C33 99.1(4) . . . . ? C2 Au1 Au31 Cl60 100.0(5) . . . . ? Cl29 Au1 Au31 Cl60 -83.95(17) . . . . ? C9 N3 N4 C5 -173.8(18) . . . . ? C2 N3 N4 C5 -2(2) . . . . ? C33 N34 N35 C36 2.5(17) . . . . ? C40 N34 N35 C36 -176.3(13) . . . . ? C5 N1 C2 N3 -5.3(18) . . . . ? C8 N1 C2 N3 -179.6(18) . . . . ? C5 N1 C2 Au1 163.2(14) . . . . ? C8 N1 C2 Au1 -11(3) . . . . ? N4 N3 C2 N1 4.5(18) . . . . ? C9 N3 C2 N1 176.0(16) . . . . ? N4 N3 C2 Au1 -165.3(12) . . . . ? C9 N3 C2 Au1 6(2) . . . . ? Cl29 Au1 C2 N1 -129(6) . . . . ? Au31 Au1 C2 N1 -60.9(15) . . . . ? Cl29 Au1 C2 N3 37(8) . . . . ? Au31 Au1 C2 N3 105.2(13) . . . . ? N3 N4 C5 N1 -2(3) . . . . ? N3 N4 C5 C6 177(3) . . . . ? C2 N1 C5 N4 5(3) . . . . ? C8 N1 C5 N4 -179(2) . . . . ? C2 N1 C5 C6 -174.4(15) . . . . ? C8 N1 C5 C6 1(2) . . . . ? N4 C5 C6 C7 -164(3) . . . . ? N1 C5 C6 C7 15(2) . . . . ? C5 C6 C7 C8 -26(2) . . . . ? C2 N1 C8 C7 156.5(19) . . . . ? C5 N1 C8 C7 -17(2) . . . . ? C2 N1 C8 C15 -81(2) . . . . ? C5 N1 C8 C15 105.6(18) . . . . ? C6 C7 C8 N1 26(2) . . . . ? C6 C7 C8 C15 -98.4(19) . . . . ? N4 N3 C9 C14 27(3) . . . . ? C2 N3 C9 C14 -144.0(18) . . . . ? N4 N3 C9 C10 -154.6(18) . . . . ? C2 N3 C9 C10 35(3) . . . . ? C14 C9 C10 C11 -4(3) . . . . ? N3 C9 C10 C11 177(2) . . . . ? C9 C10 C11 C12 3(3) . . . . ? C10 C11 C12 C13 -3(3) . . . . ? C11 C12 C13 C14 2(3) . . . . ? C10 C9 C14 C13 3(3) . . . . ? N3 C9 C14 C13 -177.9(17) . . . . ? C12 C13 C14 C9 -3(3) . . . . ? N1 C8 C15 C22 49.8(18) . . . . ? C7 C8 C15 C22 165.9(17) . . . . ? N1 C8 C15 F28 -61.8(16) . . . . ? C7 C8 C15 F28 54(2) . . . . ? N1 C8 C15 C16 -176.7(13) . . . . ? C7 C8 C15 C16 -61(2) . . . . ? C22 C15 C16 C17 94(2) . . . . ? C8 C15 C16 C17 -37(2) . . . . ? F28 C15 C16 C17 -146.9(17) . . . . ? C22 C15 C16 C21 -88.8(18) . . . . ? C8 C15 C16 C21 140.0(15) . . . . ? F28 C15 C16 C21 31(2) . . . . ? C21 C16 C17 C18 7(3) . . . . ? C15 C16 C17 C18 -176.1(17) . . . . ? C16 C17 C18 C19 -7(3) . . . . ? C17 C18 C19 C20 8(3) . . . . ? C18 C19 C20 C21 -8(4) . . . . ? C17 C16 C21 C20 -6(3) . . . . ? C15 C16 C21 C20 176.7(15) . . . . ? C19 C20 C21 C16 6(3) . . . . ? C8 C15 C22 C27 -95(2) . . . . ? F28 C15 C22 C27 12(2) . . . . ? C16 C15 C22 C27 132.8(18) . . . . ? C8 C15 C22 C23 87(2) . . . . ? F28 C15 C22 C23 -165.9(17) . . . . ? C16 C15 C22 C23 -45(2) . . . . ? C27 C22 C23 C24 -5(3) . . . . ? C15 C22 C23 C24 173(2) . . . . ? C22 C23 C24 C25 10(4) . . . . ? C23 C24 C25 C26 -12(4) . . . . ? C24 C25 C26 C27 9(4) . . . . ? C23 C22 C27 C26 2(3) . . . . ? C15 C22 C27 C26 -176(2) . . . . ? C25 C26 C27 C22 -5(4) . . . . ? N35 N34 C33 N32 -2.1(16) . . . . ? C40 N34 C33 N32 176.5(15) . . . . ? N35 N34 C33 Au31 -176.4(11) . . . . ? C40 N34 C33 Au31 2(2) . . . . ? C36 N32 C33 N34 1.0(16) . . . . ? C39 N32 C33 N34 172.6(17) . . . . ? C36 N32 C33 Au31 175.9(10) . . . . ? C39 N32 C33 Au31 -12(3) . . . . ? Cl60 Au31 C33 N34 17(9) . . . . ? Au1 Au31 C33 N34 115.6(14) . . . . ? Cl60 Au31 C33 N32 -156(8) . . . . ? Au1 Au31 C33 N32 -58.0(11) . . . . ? N34 N35 C36 C37 169(2) . . . . ? N34 N35 C36 N32 -1.7(16) . . . . ? C33 N32 C36 N35 0.5(16) . . . . ? C39 N32 C36 N35 -174.1(12) . . . . ? C33 N32 C36 C37 -172.6(14) . . . . ? C39 N32 C36 C37 12.8(18) . . . . ? N35 C36 C37 C38 -163.2(19) . . . . ? N32 C36 C37 C38 6.6(18) . . . . ? C36 C37 C38 C39 -23.5(17) . . . . ? C37 C38 C39 C46 -90.7(16) . . . . ? C37 C38 C39 N32 29.1(15) . . . . ? C33 N32 C39 C46 -76(2) . . . . ? C36 N32 C39 C46 95.5(15) . . . . ? C33 N32 C39 C38 162.3(18) . . . . ? C36 N32 C39 C38 -26.3(15) . . . . ? C33 N34 C40 C45 -153.0(17) . . . . ? N35 N34 C40 C45 26(2) . . . . ? C33 N34 C40 C41 23(3) . . . . ? N35 N34 C40 C41 -158.9(17) . . . . ? C45 C40 C41 C42 -1(3) . . . . ? N34 C40 C41 C42 -176(2) . . . . ? C40 C41 C42 C43 3(4) . . . . ? C41 C42 C43 C44 -9(4) . . . . ? C42 C43 C44 C45 12(4) . . . . ? C43 C44 C45 C40 -9(3) . . . . ? C41 C40 C45 C44 4(3) . . . . ? N34 C40 C45 C44 179.9(18) . . . . ? C38 C39 C46 F59 63.6(17) . . . . ? N32 C39 C46 F59 -48.6(16) . . . . ? C38 C39 C46 C47 -50.4(19) . . . . ? N32 C39 C46 C47 -162.6(13) . . . . ? C38 C39 C46 C53 179.3(14) . . . . ? N32 C39 C46 C53 67.1(18) . . . . ? F59 C46 C47 C48 -17(2) . . . . ? C39 C46 C47 C48 98.3(19) . . . . ? C53 C46 C47 C48 -130.0(17) . . . . ? F59 C46 C47 C52 172.9(14) . . . . ? C39 C46 C47 C52 -71.4(19) . . . . ? C53 C46 C47 C52 60(2) . . . . ? C52 C47 C48 C49 -6(3) . . . . ? C46 C47 C48 C49 -176.2(18) . . . . ? C47 C48 C49 C50 2(3) . . . . ? C48 C49 C50 C51 0(3) . . . . ? C49 C50 C51 C52 1(2) . . . . ? C48 C47 C52 C51 8(3) . . . . ? C46 C47 C52 C51 178.4(15) . . . . ? C50 C51 C52 C47 -6(2) . . . . ? F59 C46 C53 C54 -20(2) . . . . ? C39 C46 C53 C54 -137.1(17) . . . . ? C47 C46 C53 C54 91.9(19) . . . . ? F59 C46 C53 C58 163.8(14) . . . . ? C39 C46 C53 C58 47(2) . . . . ? C47 C46 C53 C58 -84.1(19) . . . . ? C58 C53 C54 C55 -6(3) . . . . ? C46 C53 C54 C55 177.7(16) . . . . ? C53 C54 C55 C56 4(3) . . . . ? C54 C55 C56 C57 2(4) . . . . ? C55 C56 C57 C58 -6(4) . . . . ? C56 C57 C58 C53 3(3) . . . . ? C54 C53 C58 C57 4(3) . . . . ? C46 C53 C58 C57 179.4(16) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.942 _refine_diff_density_min -2.320 _refine_diff_density_rms 0.250 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Coppens, P. (1970). In Crystallographic Computing, edited by F.R. Ahmed, S.R.Hall & C.P.Huber, pp 255-270. Copenhagen: Munksgaard. ;