Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'T. Spalding' _publ_contact_author_address ; Chemistry Department University College Cork Cork REPUBLIC OF IRELAND ; _publ_contact_author_email T.SPALDING@UCC.IE _publ_section_title ; Metallaheteroborane Chemistry Part 18. Pentahapto-Bonded Gold Heteroborane Clusters [3-(R3P)-closo-2,1-AuTeB10H10]- and [3-(R3P)-closo-3,1,2-AuAs2B9H9]-. ; loop_ _publ_author_name 'T. Spalding' 'G. Ferguson' 'J. F. Gallagher' 'A. M. Kelleher' 'John D. Kennedy' data_2 # gf96-70:trs96-15 _database_code_depnum_ccdc_archive 'CCDC 270401' #_vrf_PLAT308_2 #; #PROBLEM: Single Bonded Metal Atom (Unusual !) ........... Au1 #RESPONSE: This is just an artefact of the checkcif routine. #Au1 is bonded to P1 and C1 with C1-Au1-P1 176.7(3) degrees #; # end Validation Reply Form #===================================================================== # 5. Chemical Data _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C24 H42 Au O P' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H42 Au O P' _chemical_formula_weight 574.52 _chemical_compound_source 'synthesized by the authors, see text' 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' O O 0.0106 0.0060 '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' #========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8012(11) _cell_length_b 11.2980(18) _cell_length_c 12.587(2) _cell_angle_alpha 110.808(16) _cell_angle_beta 106.498(15) _cell_angle_gamma 92.064(15) _cell_volume 1234.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 294(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.10 _cell_measurement_theta_max 13.13 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.18 _exptl_crystal_size_rad ? _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 6.033 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_process_details 'ABSO in NRCVAX (Gabe et al., 1989)' _exptl_absorpt_correction_T_min 0.0981 _exptl_absorpt_correction_T_max 0.2914 #========================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 0 0 0 2 1 0 0 2 _diffrn_reflns_number 4371 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 4371 _reflns_number_gt 2805 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1992)' _computing_cell_refinement 'SET4 & CELDIM (Enraf-Nonius, 1992)' _computing_data_reduction 'DATRD2 in NRCVAX96 (Gabe et al., 1989)' _computing_structure_solution 'NRCVAX96 via Patterson heavy-atom method' _computing_structure_refinement 'NRCVAX96 and SHELXL97 (Sheldrick, 1997b)' _computing_molecular_graphics 'NRCVAX96, ORTEP (Johnson, 1976), PLATON (Spek, 1998)' _computing_publication_material 'NRCVAX96, SHELXL97 and WordPerfect macro PREP8 (Ferguson, 1998)' #========================================================================= _refine_special_details ; Compound (2) crystallised in the triclinic system; space group P-1 assumed and confirmed by the analysis. It was obvious at an early stage in the analysis that several atoms were disordered. One of the cyclohexyl rings was clearly disordered over two unequal sites; five C atoms of the 3-hydroxy-3-methyl-1- pentyne moiety were also disordered over two sites. It was possible to model the disorders successfully using a combination of DFIX constraints with SHELXL97. H atoms were treated as riding atoms (C-H 0.96 to 0.98, O-H 0.82\%A). ; # 8. Refinement Data _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0605P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4371 _refine_ls_number_parameters 287 _refine_ls_number_restraints 151 _refine_ls_R_factor_all 0.0972 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1293 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 #========================================================================= # 9. Atomic Coordinates and Displacement Parameters 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.01713(5) 0.86852(4) 0.75498(4) 0.05702(19) Uani 1 d . . . P1 P -0.1039(3) 0.7304(3) 0.8035(3) 0.0530(7) Uani 1 d D . . C11A C -0.143(3) 0.5688(15) 0.684(2) 0.046(4) Uani 0.356(13) d PDU A 1 H11A H -0.0513 0.5510 0.6700 0.056 Uiso 0.356(13) calc PR A 1 C12A C -0.238(4) 0.576(2) 0.570(3) 0.082(6) Uani 0.356(13) d PDU A 1 H12A H -0.1950 0.6457 0.5559 0.099 Uiso 0.356(13) calc PR A 1 H12B H -0.3309 0.5960 0.5792 0.099 Uiso 0.356(13) calc PR A 1 C13A C -0.261(6) 0.453(3) 0.463(2) 0.110(7) Uani 0.356(13) d PDU A 1 H13A H -0.3312 0.4588 0.3941 0.132 Uiso 0.356(13) calc PR A 1 H13B H -0.1711 0.4413 0.4458 0.132 Uiso 0.356(13) calc PR A 1 C14A C -0.312(3) 0.339(3) 0.485(3) 0.080(6) Uani 0.356(13) d PDU A 1 H14A H -0.3147 0.2615 0.4177 0.096 Uiso 0.356(13) calc PR A 1 H14B H -0.4093 0.3436 0.4886 0.096 Uiso 0.356(13) calc PR A 1 C15A C -0.216(4) 0.332(2) 0.599(3) 0.080(7) Uani 0.356(13) d PDU A 1 H15A H -0.2578 0.2619 0.6125 0.096 Uiso 0.356(13) calc PR A 1 H15B H -0.1227 0.3158 0.5908 0.096 Uiso 0.356(13) calc PR A 1 C16A C -0.199(6) 0.455(3) 0.704(2) 0.080(6) Uani 0.356(13) d PDU A 1 H16A H -0.1321 0.4500 0.7756 0.096 Uiso 0.356(13) calc PR A 1 H16B H -0.2909 0.4669 0.7180 0.096 Uiso 0.356(13) calc PR A 1 C11B C -0.2046(15) 0.5826(11) 0.6741(11) 0.046(4) Uani 0.644(13) d PDU A 2 H11B H -0.3000 0.6044 0.6439 0.056 Uiso 0.644(13) calc PR A 2 C12B C -0.144(2) 0.5537(16) 0.5722(15) 0.082(6) Uani 0.644(13) d PDU A 2 H12C H -0.0449 0.5409 0.5996 0.099 Uiso 0.644(13) calc PR A 2 H12D H -0.1441 0.6275 0.5498 0.099 Uiso 0.644(13) calc PR A 2 C13B C -0.225(3) 0.4377(18) 0.4628(14) 0.110(7) Uani 0.644(13) d PDU A 2 H13C H -0.3196 0.4552 0.4268 0.132 Uiso 0.644(13) calc PR A 2 H13D H -0.1740 0.4200 0.4045 0.132 Uiso 0.644(13) calc PR A 2 C14B C -0.242(2) 0.3222(15) 0.4933(17) 0.080(6) Uani 0.644(13) d PDU A 2 H14C H -0.1477 0.2975 0.5187 0.096 Uiso 0.644(13) calc PR A 2 H14D H -0.3011 0.2514 0.4224 0.096 Uiso 0.644(13) calc PR A 2 C15B C -0.309(2) 0.3479(15) 0.5913(17) 0.080(7) Uani 0.644(13) d PDU A 2 H15C H -0.4087 0.3573 0.5605 0.096 Uiso 0.644(13) calc PR A 2 H15D H -0.3074 0.2746 0.6145 0.096 Uiso 0.644(13) calc PR A 2 C16B C -0.234(3) 0.4654(16) 0.6997(15) 0.080(6) Uani 0.644(13) d PDU A 2 H16C H -0.1429 0.4472 0.7419 0.096 Uiso 0.644(13) calc PR A 2 H16D H -0.2919 0.4845 0.7528 0.096 Uiso 0.644(13) calc PR A 2 C21 C 0.0093(12) 0.6929(10) 0.9286(10) 0.059(3) Uani 1 d . . . H21 H -0.0483 0.6276 0.9391 0.071 Uiso 1 calc R . . C22 C 0.1429(12) 0.6387(12) 0.9031(12) 0.070(3) Uani 1 d . . . H22A H 0.2000 0.7005 0.8896 0.084 Uiso 1 calc R . . H22B H 0.1133 0.5612 0.8311 0.084 Uiso 1 calc R . . C23 C 0.2343(13) 0.6085(13) 1.0085(13) 0.079(4) Uani 1 d . . . H23A H 0.1789 0.5427 1.0186 0.095 Uiso 1 calc R . . H23B H 0.3187 0.5754 0.9909 0.095 Uiso 1 calc R . . C24 C 0.2792(14) 0.7203(13) 1.1184(13) 0.081(4) Uani 1 d . . . H24A H 0.3432 0.7826 1.1112 0.097 Uiso 1 calc R . . H24B H 0.3325 0.6965 1.1835 0.097 Uiso 1 calc R . . C25 C 0.1531(14) 0.7804(13) 1.1476(12) 0.084(4) Uani 1 d . . . H25A H 0.1888 0.8588 1.2184 0.101 Uiso 1 calc R . . H25B H 0.0972 0.7226 1.1663 0.101 Uiso 1 calc R . . C26 C 0.0547(12) 0.8114(11) 1.0456(10) 0.067(3) Uani 1 d . . . H26A H 0.1050 0.8800 1.0353 0.081 Uiso 1 calc R . . H26B H -0.0301 0.8402 1.0656 0.081 Uiso 1 calc R . . C31 C -0.2507(11) 0.8020(10) 0.8554(11) 0.060(3) Uani 1 d . . . H31 H -0.2042 0.8799 0.9262 0.071 Uiso 1 calc R . . C32 C -0.3357(13) 0.7205(11) 0.8970(11) 0.070(3) Uani 1 d . . . H32A H -0.3855 0.6421 0.8298 0.084 Uiso 1 calc R . . H32B H -0.2697 0.6974 0.9576 0.084 Uiso 1 calc R . . C33 C -0.4420(14) 0.7916(12) 0.9473(12) 0.076(4) Uani 1 d . . . H33A H -0.4992 0.7357 0.9671 0.092 Uiso 1 calc R . . H33B H -0.3911 0.8637 1.0207 0.092 Uiso 1 calc R . . C34 C -0.5382(14) 0.8387(11) 0.8636(12) 0.078(4) Uani 1 d . . . H34A H -0.6012 0.8886 0.9026 0.094 Uiso 1 calc R . . H34B H -0.5981 0.7660 0.7947 0.094 Uiso 1 calc R . . C35 C -0.4596(13) 0.9200(13) 0.8208(13) 0.079(4) Uani 1 d . . . H35A H -0.4093 0.9987 0.8874 0.094 Uiso 1 calc R . . H35B H -0.5280 0.9423 0.7609 0.094 Uiso 1 calc R . . C36 C -0.3503(13) 0.8457(12) 0.7661(12) 0.078(4) Uani 1 d . . . H36A H -0.4016 0.7720 0.6942 0.094 Uiso 1 calc R . . H36B H -0.2948 0.9005 0.7441 0.094 Uiso 1 calc R . . O1 O 0.1022(10) 1.2015(9) 0.5630(10) 0.107(3) Uani 1 d D B 3 H1 H 0.0680 1.1370 0.5019 0.080 Uiso 1 calc R B 3 C1 C 0.1128(11) 0.9925(10) 0.7073(10) 0.060(3) Uani 1 d D B 3 C2 C 0.156(11) 1.0720(13) 0.677(5) 0.070(4) Uani 0.64(2) d PD B 3 C3 C 0.2159(16) 1.1722(15) 0.6471(15) 0.082(8) Uani 0.64(2) d PD B 3 C4 C 0.282(3) 1.2902(18) 0.764(2) 0.110(8) Uani 0.64(2) d PD B 3 H4A H 0.3198 1.3579 0.7460 0.166 Uiso 0.64(2) calc PR B 3 H4B H 0.3576 1.2684 0.8176 0.166 Uiso 0.64(2) calc PR B 3 H4C H 0.2087 1.3180 0.8001 0.166 Uiso 0.64(2) calc PR B 3 C5 C 0.332(2) 1.136(2) 0.589(2) 0.129(11) Uani 0.64(2) d PDU B 3 H5A H 0.3562 1.2036 0.5631 0.155 Uiso 0.64(2) calc PR B 3 H5B H 0.4173 1.1303 0.6470 0.155 Uiso 0.64(2) calc PR B 3 C6 C 0.286(4) 1.0136(18) 0.484(2) 0.136(10) Uani 0.64(2) d PD B 3 H6A H 0.3642 0.9937 0.4516 0.205 Uiso 0.64(2) calc PR B 3 H6B H 0.2047 1.0205 0.4240 0.205 Uiso 0.64(2) calc PR B 3 H6C H 0.2610 0.9468 0.5084 0.205 Uiso 0.64(2) calc PR B 3 C2A C 0.16(2) 1.0508(17) 0.657(8) 0.070(4) Uani 0.36(2) d PD B 4 C3A C 0.210(2) 1.126(3) 0.598(3) 0.082(8) Uani 0.36(2) d PD B 4 C4A C 0.264(6) 1.067(4) 0.490(3) 0.136(10) Uani 0.36(2) d PD B 4 H4A1 H 0.2952 1.1342 0.4682 0.205 Uiso 0.36(2) calc PR B 4 H4A2 H 0.1866 1.0083 0.4241 0.205 Uiso 0.36(2) calc PR B 4 H4A3 H 0.3424 1.0231 0.5109 0.205 Uiso 0.36(2) calc PR B 4 C5A C 0.332(3) 1.229(4) 0.697(3) 0.095(15) Uani 0.36(2) d PDU B 4 H5A1 H 0.3911 1.1918 0.7490 0.115 Uiso 0.36(2) calc PR B 4 H5A2 H 0.3925 1.2614 0.6610 0.115 Uiso 0.36(2) calc PR B 4 C6A C 0.269(7) 1.337(3) 0.769(5) 0.110(8) Uani 0.36(2) d PD B 4 H6A1 H 0.3459 1.4016 0.8301 0.166 Uiso 0.36(2) calc PR B 4 H6A2 H 0.2107 1.3050 0.8049 0.166 Uiso 0.36(2) calc PR B 4 H6A3 H 0.2113 1.3741 0.7168 0.166 Uiso 0.36(2) calc PR B 4 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 0.0654(3) 0.0580(3) 0.0585(3) 0.0306(2) 0.0257(2) 0.00405(19) P1 0.0626(18) 0.0512(17) 0.0523(19) 0.0247(15) 0.0228(15) 0.0061(13) C11A 0.041(12) 0.041(7) 0.055(9) 0.010(7) 0.020(9) 0.017(7) C12A 0.087(16) 0.084(12) 0.065(11) 0.013(10) 0.032(13) -0.021(13) C13A 0.14(2) 0.123(14) 0.062(11) 0.023(10) 0.038(11) 0.005(13) C14A 0.060(15) 0.061(10) 0.092(14) 0.007(10) 0.013(14) 0.012(10) C15A 0.12(2) 0.056(10) 0.046(10) 0.010(8) 0.016(15) -0.020(13) C16A 0.103(16) 0.071(9) 0.077(10) 0.041(8) 0.028(9) 0.015(9) C11B 0.041(12) 0.041(7) 0.055(9) 0.010(7) 0.020(9) 0.017(7) C12B 0.087(16) 0.084(12) 0.065(11) 0.013(10) 0.032(13) -0.021(13) C13B 0.14(2) 0.123(14) 0.062(11) 0.023(10) 0.038(11) 0.005(13) C14B 0.060(15) 0.061(10) 0.092(14) 0.007(10) 0.013(14) 0.012(10) C15B 0.12(2) 0.056(10) 0.046(10) 0.010(8) 0.016(15) -0.020(13) C16B 0.103(16) 0.071(9) 0.077(10) 0.041(8) 0.028(9) 0.015(9) C21 0.074(8) 0.057(7) 0.051(7) 0.022(6) 0.028(6) 0.004(6) C22 0.062(7) 0.076(8) 0.091(10) 0.037(8) 0.044(7) 0.028(6) C23 0.073(8) 0.077(9) 0.115(13) 0.056(10) 0.045(8) 0.031(7) C24 0.073(9) 0.080(9) 0.089(11) 0.047(9) 0.008(8) 0.002(7) C25 0.098(10) 0.087(10) 0.057(9) 0.029(8) 0.008(8) -0.005(8) C26 0.066(7) 0.065(8) 0.062(8) 0.023(7) 0.010(6) 0.002(6) C31 0.055(7) 0.055(7) 0.064(8) 0.022(6) 0.013(6) 0.000(5) C32 0.089(9) 0.067(8) 0.066(9) 0.027(7) 0.039(7) 0.008(6) C33 0.090(9) 0.078(9) 0.081(10) 0.037(8) 0.049(8) 0.011(7) C34 0.088(9) 0.058(8) 0.076(10) 0.005(7) 0.035(8) 0.006(7) C35 0.077(8) 0.080(9) 0.089(10) 0.038(8) 0.031(8) 0.019(7) C36 0.091(9) 0.074(8) 0.087(10) 0.045(8) 0.036(8) 0.007(7) O1 0.107(8) 0.091(7) 0.124(10) 0.066(7) 0.006(7) -0.004(6) C1 0.063(7) 0.062(7) 0.067(8) 0.036(7) 0.026(6) 0.001(5) C2 0.071(8) 0.067(9) 0.085(19) 0.043(11) 0.026(17) 0.009(16) C3 0.079(10) 0.082(17) 0.08(2) 0.059(18) -0.015(12) -0.030(11) C4 0.150(16) 0.056(18) 0.127(17) 0.059(16) 0.017(14) 0.002(18) C5 0.130(12) 0.130(12) 0.131(12) 0.052(6) 0.045(6) 0.018(5) C6 0.22(3) 0.07(2) 0.19(3) 0.09(2) 0.11(2) 0.065(19) C2A 0.071(8) 0.067(9) 0.085(19) 0.043(11) 0.026(17) 0.009(16) C3A 0.079(10) 0.082(17) 0.08(2) 0.059(18) -0.015(12) -0.030(11) C4A 0.22(3) 0.07(2) 0.19(3) 0.09(2) 0.11(2) 0.065(19) C5A 0.096(15) 0.094(15) 0.096(15) 0.038(7) 0.028(7) 0.013(5) C6A 0.150(16) 0.056(18) 0.127(17) 0.059(16) 0.017(14) 0.002(18) _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 2.005(8) . ? Au1 P1 2.274(3) . ? P1 C31 1.842(11) . ? P1 C21 1.845(11) . ? P1 C11A 1.848(10) . ? P1 C11B 1.858(8) . ? C11A C12A 1.505(11) . ? C11A C16A 1.509(11) . ? C11A H11A 0.98 . ? C12A C13A 1.508(11) . ? C12A H12A 0.97 . ? C12A H12B 0.97 . ? C13A C14A 1.502(11) . ? C13A H13A 0.97 . ? C13A H13B 0.97 . ? C14A C15A 1.506(11) . ? C14A H14A 0.97 . ? C14A H14B 0.97 . ? C15A C16A 1.506(11) . ? C15A H15A 0.97 . ? C15A H15B 0.97 . ? C16A H16A 0.97 . ? C16A H16B 0.97 . ? C11B C12B 1.500(10) . ? C11B C16B 1.506(10) . ? C11B H11B 0.98 . ? C12B C13B 1.506(11) . ? C12B H12C 0.97 . ? C12B H12D 0.97 . ? C13B C14B 1.500(11) . ? C13B H13C 0.97 . ? C13B H13D 0.97 . ? C14B C15B 1.504(11) . ? C14B H14C 0.97 . ? C14B H14D 0.97 . ? C15B C16B 1.497(11) . ? C15B H15C 0.97 . ? C15B H15D 0.97 . ? C16B H16C 0.97 . ? C16B H16D 0.97 . ? C21 C26 1.531(15) . ? C21 C22 1.533(14) . ? C21 H21 0.98 . ? C22 C23 1.533(17) . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 C24 1.440(17) . ? C23 H23A 0.97 . ? C23 H23B 0.97 . ? C24 C25 1.505(17) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C25 C26 1.530(16) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C31 C36 1.505(16) . ? C31 C32 1.534(14) . ? C31 H31 0.98 . ? C32 C33 1.485(15) . ? C32 H32A 0.97 . ? C32 H32B 0.97 . ? C33 C34 1.468(17) . ? C33 H33A 0.97 . ? C33 H33B 0.97 . ? C34 C35 1.504(16) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C35 C36 1.549(16) . ? C35 H35A 0.97 . ? C35 H35B 0.97 . ? C36 H36A 0.97 . ? C36 H36B 0.97 . ? O1 C3 1.441(12) . ? O1 H1 0.82 . ? C1 C2 1.199(5) . ? C2 C3 1.467(12) . ? C3 C5 1.514(13) . ? C3 C4 1.534(14) . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 C6 1.476(14) . ? C5 H5A 0.97 . ? C5 H5B 0.97 . ? C6 H6A 0.96 . ? C6 H6B 0.96 . ? C6 H6C 0.96 . ? C2A C3A 1.484(14) . ? C3A C4A 1.530(15) . ? C3A C5A 1.530(15) . ? C4A H4A1 0.96 . ? C4A H4A2 0.96 . ? C4A H4A3 0.96 . ? C5A C6A 1.510(15) . ? C5A H5A1 0.97 . ? C5A H5A2 0.97 . ? C6A H6A1 0.96 . ? C6A H6A2 0.96 . ? C6A H6A3 0.96 . ? 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 P1 176.7(3) . . ? C31 P1 C21 105.0(5) . . ? C31 P1 C11A 119.5(10) . . ? C21 P1 C11A 98.7(10) . . ? C31 P1 C11B 101.4(6) . . ? C21 P1 C11B 111.5(7) . . ? C31 P1 Au1 110.3(3) . . ? C21 P1 Au1 113.2(3) . . ? C11A P1 Au1 109.6(11) . . ? C11B P1 Au1 114.3(5) . . ? C12A C11A C16A 111.5(14) . . ? C12A C11A P1 108.0(17) . . ? C16A C11A P1 120(2) . . ? C12A C11A H11A 105.5 . . ? C16A C11A H11A 105.5 . . ? P1 C11A H11A 105.5 . . ? C11A C12A C13A 112.0(14) . . ? C11A C12A H12A 109.2 . . ? C13A C12A H12A 109.2 . . ? C11A C12A H12B 109.2 . . ? C13A C12A H12B 109.2 . . ? H12A C12A H12B 107.9 . . ? C14A C13A C12A 112.2(15) . . ? C14A C13A H13A 109.2 . . ? C12A C13A H13A 109.2 . . ? C14A C13A H13B 109.2 . . ? C12A C13A H13B 109.2 . . ? H13A C13A H13B 107.9 . . ? C13A C14A C15A 112.1(14) . . ? C13A C14A H14A 109.2 . . ? C15A C14A H14A 109.2 . . ? C13A C14A H14B 109.2 . . ? C15A C14A H14B 109.2 . . ? H14A C14A H14B 107.9 . . ? C16A C15A C14A 111.3(14) . . ? C16A C15A H15A 109.4 . . ? C14A C15A H15A 109.4 . . ? C16A C15A H15B 109.4 . . ? C14A C15A H15B 109.4 . . ? H15A C15A H15B 108.0 . . ? C15A C16A C11A 111.3(14) . . ? C15A C16A H16A 109.4 . . ? C11A C16A H16A 109.4 . . ? C15A C16A H16B 109.4 . . ? C11A C16A H16B 109.4 . . ? H16A C16A H16B 108.0 . . ? C12B C11B C16B 112.1(11) . . ? C12B C11B P1 111.9(10) . . ? C16B C11B P1 117.3(11) . . ? C12B C11B H11B 104.7 . . ? C16B C11B H11B 104.7 . . ? P1 C11B H11B 104.7 . . ? C11B C12B C13B 114.2(11) . . ? C11B C12B H12C 108.7 . . ? C13B C12B H12C 108.7 . . ? C11B C12B H12D 108.7 . . ? C13B C12B H12D 108.7 . . ? H12C C12B H12D 107.6 . . ? C14B C13B C12B 111.5(12) . . ? C14B C13B H13C 109.3 . . ? C12B C13B H13C 109.3 . . ? C14B C13B H13D 109.3 . . ? C12B C13B H13D 109.3 . . ? H13C C13B H13D 108.0 . . ? C13B C14B C15B 111.7(12) . . ? C13B C14B H14C 109.3 . . ? C15B C14B H14C 109.3 . . ? C13B C14B H14D 109.3 . . ? C15B C14B H14D 109.3 . . ? H14C C14B H14D 107.9 . . ? C16B C15B C14B 113.1(12) . . ? C16B C15B H15C 109.0 . . ? C14B C15B H15C 109.0 . . ? C16B C15B H15D 109.0 . . ? C14B C15B H15D 109.0 . . ? H15C C15B H15D 107.8 . . ? C15B C16B C11B 114.8(11) . . ? C15B C16B H16C 108.6 . . ? C11B C16B H16C 108.6 . . ? C15B C16B H16D 108.6 . . ? C11B C16B H16D 108.6 . . ? H16C C16B H16D 107.5 . . ? C26 C21 C22 109.8(10) . . ? C26 C21 P1 110.9(7) . . ? C22 C21 P1 112.0(8) . . ? C26 C21 H21 108.0 . . ? C22 C21 H21 108.0 . . ? P1 C21 H21 108.0 . . ? C21 C22 C23 110.7(10) . . ? C21 C22 H22A 109.5 . . ? C23 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C23 C22 H22B 109.5 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 111.7(10) . . ? C24 C23 H23A 109.3 . . ? C22 C23 H23A 109.3 . . ? C24 C23 H23B 109.3 . . ? C22 C23 H23B 109.3 . . ? H23A C23 H23B 107.9 . . ? C23 C24 C25 111.9(11) . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? C25 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C24 C25 C26 113.3(12) . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C25 C26 C21 110.4(10) . . ? C25 C26 H26A 109.6 . . ? C21 C26 H26A 109.6 . . ? C25 C26 H26B 109.6 . . ? C21 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? C36 C31 C32 111.0(9) . . ? C36 C31 P1 112.4(9) . . ? C32 C31 P1 115.3(8) . . ? C36 C31 H31 105.8 . . ? C32 C31 H31 105.8 . . ? P1 C31 H31 105.8 . . ? C33 C32 C31 110.9(10) . . ? C33 C32 H32A 109.5 . . ? C31 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 112.4(11) . . ? C34 C33 H33A 109.1 . . ? C32 C33 H33A 109.1 . . ? C34 C33 H33B 109.1 . . ? C32 C33 H33B 109.1 . . ? H33A C33 H33B 107.9 . . ? C33 C34 C35 113.5(11) . . ? C33 C34 H34A 108.9 . . ? C35 C34 H34A 108.9 . . ? C33 C34 H34B 108.9 . . ? C35 C34 H34B 108.9 . . ? H34A C34 H34B 107.7 . . ? C34 C35 C36 109.8(10) . . ? C34 C35 H35A 109.7 . . ? C36 C35 H35A 109.7 . . ? C34 C35 H35B 109.7 . . ? C36 C35 H35B 109.7 . . ? H35A C35 H35B 108.2 . . ? C31 C36 C35 110.1(11) . . ? C31 C36 H36A 109.6 . . ? C35 C36 H36A 109.6 . . ? C31 C36 H36B 109.6 . . ? C35 C36 H36B 109.6 . . ? H36A C36 H36B 108.2 . . ? C2 C1 Au1 173(5) . . ? C1 C2 C3 177(7) . . ? O1 C3 C2 109(4) . . ? O1 C3 C5 106.1(16) . . ? C2 C3 C5 115(3) . . ? O1 C3 C4 111.1(17) . . ? C2 C3 C4 108(2) . . ? C5 C3 C4 107.9(12) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C3 112.6(14) . . ? C6 C5 H5A 109.1 . . ? C3 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? C3 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2A C3A C4A 124(3) . . ? C2A C3A C5A 106(6) . . ? C4A C3A C5A 107.4(14) . . ? C3A C4A H4A1 109.5 . . ? C3A C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C3A C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? C6A C5A C3A 109.8(15) . . ? C6A C5A H5A1 109.7 . . ? C3A C5A H5A1 109.7 . . ? C6A C5A H5A2 109.7 . . ? C3A C5A H5A2 109.7 . . ? H5A1 C5A H5A2 108.2 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 P1 C11A C12A 67(2) . . . . ? C21 P1 C11A C12A 179(2) . . . . ? C11B P1 C11A C12A 46(3) . . . . ? Au1 P1 C11A C12A -62(2) . . . . ? C31 P1 C11A C16A -62(3) . . . . ? C21 P1 C11A C16A 50(2) . . . . ? C11B P1 C11A C16A -83(4) . . . . ? Au1 P1 C11A C16A 169(2) . . . . ? C16A C11A C12A C13A -54(3) . . . . ? P1 C11A C12A C13A 173(2) . . . . ? C11A C12A C13A C14A 52(3) . . . . ? C12A C13A C14A C15A -53(3) . . . . ? C13A C14A C15A C16A 54(3) . . . . ? C14A C15A C16A C11A -56(3) . . . . ? C12A C11A C16A C15A 56(3) . . . . ? P1 C11A C16A C15A -177(2) . . . . ? C31 P1 C11B C12B 141.8(13) . . . . ? C21 P1 C11B C12B -106.9(14) . . . . ? C11A P1 C11B C12B -57(4) . . . . ? Au1 P1 C11B C12B 23.1(15) . . . . ? C31 P1 C11B C16B -86.6(15) . . . . ? C21 P1 C11B C16B 24.8(16) . . . . ? C11A P1 C11B C16B 75(5) . . . . ? Au1 P1 C11B C16B 154.8(13) . . . . ? C16B C11B C12B C13B 48(2) . . . . ? P1 C11B C12B C13B -177.7(15) . . . . ? C11B C12B C13B C14B -53(3) . . . . ? C12B C13B C14B C15B 54(3) . . . . ? C13B C14B C15B C16B -52(2) . . . . ? C14B C15B C16B C11B 48(3) . . . . ? C12B C11B C16B C15B -46(3) . . . . ? P1 C11B C16B C15B -177.1(15) . . . . ? C31 P1 C21 C26 -53.7(8) . . . . ? C11A P1 C21 C26 -177.5(12) . . . . ? C11B P1 C21 C26 -162.8(8) . . . . ? Au1 P1 C21 C26 66.7(8) . . . . ? C31 P1 C21 C22 -176.8(8) . . . . ? C11A P1 C21 C22 59.3(13) . . . . ? C11B P1 C21 C22 74.1(9) . . . . ? Au1 P1 C21 C22 -56.4(9) . . . . ? C26 C21 C22 C23 56.3(12) . . . . ? P1 C21 C22 C23 -179.9(8) . . . . ? C21 C22 C23 C24 -58.3(14) . . . . ? C22 C23 C24 C25 56.0(14) . . . . ? C23 C24 C25 C26 -54.1(15) . . . . ? C24 C25 C26 C21 52.5(14) . . . . ? C22 C21 C26 C25 -53.4(12) . . . . ? P1 C21 C26 C25 -177.8(8) . . . . ? C21 P1 C31 C36 176.8(8) . . . . ? C11A P1 C31 C36 -73.8(14) . . . . ? C11B P1 C31 C36 -66.9(10) . . . . ? Au1 P1 C31 C36 54.5(8) . . . . ? C21 P1 C31 C32 -54.7(9) . . . . ? C11A P1 C31 C32 54.7(15) . . . . ? C11B P1 C31 C32 61.5(10) . . . . ? Au1 P1 C31 C32 -177.0(8) . . . . ? C36 C31 C32 C33 -56.1(14) . . . . ? P1 C31 C32 C33 174.8(9) . . . . ? C31 C32 C33 C34 54.4(14) . . . . ? C32 C33 C34 C35 -55.2(14) . . . . ? C33 C34 C35 C36 54.6(15) . . . . ? C32 C31 C36 C35 56.4(13) . . . . ? P1 C31 C36 C35 -172.9(8) . . . . ? C34 C35 C36 C31 -55.1(14) . . . . ? O1 C3 C5 C6 -69(3) . . . . ? C2 C3 C5 C6 52(5) . . . . ? C4 C3 C5 C6 172(2) . . . . ? C2A C3A C5A C6A -79(7) . . . . ? C4A C3A C5A C6A 147(4) . . . . ? _refine_diff_density_max 1.568 #(adjacent to Au) _refine_diff_density_min -0.829 _refine_diff_density_rms 0.178 # Attachment '270402.txt' ####################################################################### # # 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_5 #GF9416 _database_code_depnum_ccdc_archive 'CCDC 270402' #================================================================ # 5. Chemical Data _chemical_name_systematic ; ? #Insert the chemical name here. ; _chemical_name_common ? _chemical_formula_moiety 'C18 H24 As2 Au B9 P, C4 H12 N, C H2 Cl2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C23 H38 As2 Au B9 Cl2 N P' _chemical_formula_weight 874.58 _chemical_compound_source 'synthesized by the authors, see text' 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' As As 0.0499 2.0058 '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' B B 0.0013 0.0007 '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' N N 0.0061 0.0033 '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' #===================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.564(3) _cell_length_b 9.882(3) _cell_length_c 18.937(3) _cell_angle_alpha 102.84(2) _cell_angle_beta 93.69(2) _cell_angle_gamma 101.08(2) _cell_volume 1701.7(8) _cell_formula_units_Z 2 _cell_measurement_temperature 294(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.50 _cell_measurement_theta_max 15.21 _cell_special_details ; ? #Insert any comments here. ; _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.31 _exptl_crystal_size_rad ? _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844.1 _exptl_absorpt_coefficient_mu 6.474 _exptl_absorpt_correction_type psi-scan # 'empirical, \y-scans at 4\% steps (North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details '(North, Philips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.0701 _exptl_absorpt_correction_T_max 0.1335 #===================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? #Insert any special details here. ; _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 4.1 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 0 8 1 0 10 -3 -2 10 _diffrn_reflns_number 7389 _diffrn_reflns_av_R_equivalents 0.000 _diffrn_reflns_av_sigmaI/netI 0.0599 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 26.94 _diffrn_reflns_theta_full 26.94 _diffrn_measured_fraction_theta_max 1.0 _diffrn_measured_fraction_theta_full 1.0 _reflns_number_total 7389 _reflns_number_gt 4502 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1992)' _computing_cell_refinement 'SET4 & CELDIM (Enraf-Nonius, 1992)' _computing_data_reduction 'DATRD2 in NRCVAX96 (Gabe, Le Page, Charland, Lee & White, 1989)' _computing_structure_solution 'NRCVAX96 via Patterson heavy-atom method' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976), PLATON (Spek, 2003)' _computing_publication_material SHELXL97 #==================================================================== _refine_special_details ; The tetramethyl ammonium cation has normal geometry and the dichloromethane of solvation fills what would have been a void in the crystal lattice. Molecule (I) crystallised in the triclinic system; space group P-1 assumed and confirmed by the analysis. It soon became apparent from electron-density peak heights that the two As atoms of the AuAs~2~B~9~H~9~ cage were disordered unequally over the five possible sites bonded to Au3, with two major sites and three minor sites. The atom labels of the disordered atoms are As1/B1, As2/B2, As4/B4, As7/B7 and As8/B8. For the final refinement with SHELXL97, each site was allowed for as an As/B mixture with the occupancies restrained so that the sum of the As occupancies added to 2, the B atoms to 3; at each site the B occupancy was arranged to have a value (1 - (occupancy of As)). The final occpancies are:- As1 0.825(3), As2 0.706(3), As4 0.263(3), As7 0.135(3), As8 0.072(3). H atoms were positioned geometrically and treated as riding atoms (C-H 0.93 to 0.97, B-H 1.10\%A). ; # 8. Refinement Data _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7389 _refine_ls_number_parameters 358 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 Au3 Au 0.40305(3) 0.42963(3) 0.712915(14) 0.06594(14) Uani 1 1 d . . . As1 As 0.56617(9) 0.67514(8) 0.69703(4) 0.0556(3) Uani 0.825(3) 1 d P A . H1 H 0.5866 0.6769 0.6407 0.067 Uiso 0.175(3) 1 calc PR . . As2 As 0.37344(12) 0.69384(10) 0.77644(5) 0.0640(4) Uani 0.706(3) 1 d P A . H2 H 0.2766 0.7322 0.7633 0.077 Uiso 0.294(3) 1 calc PR . . As4 As 0.6749(2) 0.4938(2) 0.72614(11) 0.0615(9) Uani 0.263(3) 1 d P A . H4 H 0.7313 0.4297 0.6872 0.074 Uiso 0.737(3) 1 calc PR . . B1 B 0.56617(9) 0.67514(8) 0.69703(4) 0.0556(3) Uani 0.175(3) 1 d P A -1 B2 B 0.37344(12) 0.69384(10) 0.77644(5) 0.0640(4) Uani 0.294(3) 1 d P A -1 B4 B 0.6749(2) 0.4938(2) 0.72614(11) 0.0615(9) Uani 0.737(3) 1 d P A -1 B5 B 0.7339(9) 0.7122(8) 0.7827(4) 0.063(2) Uani 1 1 d . . . H5 H 0.8360 0.7683 0.7694 0.076 Uiso 1 1 calc R A . B6 B 0.5942(9) 0.8096(8) 0.8075(4) 0.062(2) Uani 1 1 d . A . H6 H 0.6079 0.9234 0.8093 0.075 Uiso 1 1 calc R . . As7 As 0.3934(5) 0.5332(4) 0.84549(18) 0.0752(16) Uani 0.135(3) 1 d P A . H7 H 0.3200 0.4555 0.8666 0.090 Uiso 0.865(3) 1 calc PR . . As8 As 0.5642(5) 0.4343(6) 0.8149(2) 0.077(2) Uani 0.072(3) 1 d P A . H8 H 0.5630 0.3273 0.8230 0.092 Uiso 0.928(3) 1 calc PR . . B7 B 0.3934(5) 0.5332(4) 0.84549(18) 0.0752(16) Uani 0.865(3) 1 d P A -1 B8 B 0.5642(5) 0.4343(6) 0.8149(2) 0.077(2) Uani 0.928(3) 1 d P A -1 B9 B 0.7288(8) 0.5839(8) 0.8343(4) 0.0554(19) Uani 1 1 d . A . H9 H 0.8297 0.5586 0.8534 0.066 Uiso 1 1 calc R . . B10 B 0.6929(10) 0.7535(8) 0.8716(4) 0.067(2) Uani 1 1 d . A . H10 H 0.7692 0.8342 0.9132 0.081 Uiso 1 1 calc R . . B11 B 0.5060(9) 0.7331(8) 0.8761(4) 0.058(2) Uani 1 1 d . . . H11 H 0.4664 0.8014 0.9211 0.069 Uiso 1 1 calc R A . B12 B 0.5893(9) 0.5967(8) 0.8914(4) 0.062(2) Uani 1 1 d . A . H12 H 0.6014 0.5787 0.9465 0.074 Uiso 1 1 calc R . . P1 P 0.24529(17) 0.27101(16) 0.62650(7) 0.0439(4) Uani 1 1 d . A . C11 C 0.1887(6) 0.3282(6) 0.5462(3) 0.0454(14) Uani 1 1 d . . . C12 C 0.2885(7) 0.4205(7) 0.5188(3) 0.0599(17) Uani 1 1 d . A . H12A H 0.3809 0.4551 0.5426 0.072 Uiso 1 1 calc R . . C13 C 0.2486(9) 0.4602(8) 0.4559(4) 0.070(2) Uani 1 1 d . . . H13 H 0.3156 0.5209 0.4375 0.084 Uiso 1 1 calc R A . C14 C 0.1140(9) 0.4124(8) 0.4208(3) 0.068(2) Uani 1 1 d . A . H14 H 0.0894 0.4400 0.3786 0.081 Uiso 1 1 calc R . . C15 C 0.0138(8) 0.3226(8) 0.4477(3) 0.0644(18) Uani 1 1 d . . . H15 H -0.0788 0.2894 0.4240 0.077 Uiso 1 1 calc R A . C16 C 0.0526(7) 0.2826(7) 0.5103(3) 0.0535(16) Uani 1 1 d . A . H16 H -0.0155 0.2230 0.5287 0.064 Uiso 1 1 calc R . . C21 C 0.3102(6) 0.1097(6) 0.5907(3) 0.0474(14) Uani 1 1 d . . . C22 C 0.2696(7) 0.0265(7) 0.5205(3) 0.0579(17) Uani 1 1 d . A . H22 H 0.2104 0.0545 0.4881 0.070 Uiso 1 1 calc R . . C23 C 0.3170(8) -0.0982(7) 0.4987(4) 0.070(2) Uani 1 1 d . . . H23 H 0.2906 -0.1547 0.4517 0.084 Uiso 1 1 calc R A . C24 C 0.4039(8) -0.1374(8) 0.5480(5) 0.079(2) Uani 1 1 d . A . H24 H 0.4336 -0.2228 0.5341 0.095 Uiso 1 1 calc R . . C25 C 0.4464(9) -0.0568(9) 0.6143(5) 0.082(2) Uani 1 1 d . . . H25 H 0.5064 -0.0859 0.6459 0.099 Uiso 1 1 calc R A . C26 C 0.4032(7) 0.0694(7) 0.6377(4) 0.0621(18) Uani 1 1 d . A . H26 H 0.4357 0.1267 0.6841 0.075 Uiso 1 1 calc R . . C31 C 0.0772(6) 0.2057(6) 0.6612(3) 0.0451(14) Uani 1 1 d . . . C32 C 0.0070(7) 0.0654(7) 0.6420(3) 0.0530(16) Uani 1 1 d . A . H32 H 0.0438 -0.0004 0.6094 0.064 Uiso 1 1 calc R . . C33 C -0.1177(8) 0.0222(8) 0.6709(4) 0.0663(19) Uani 1 1 d . . . H33 H -0.1662 -0.0722 0.6564 0.080 Uiso 1 1 calc R A . C34 C -0.1704(8) 0.1148(10) 0.7199(4) 0.078(2) Uani 1 1 d . A . H34 H -0.2528 0.0841 0.7405 0.094 Uiso 1 1 calc R . . C35 C -0.1021(10) 0.2534(10) 0.7391(4) 0.081(2) Uani 1 1 d . . . H35 H -0.1402 0.3179 0.7717 0.097 Uiso 1 1 calc R A . C36 C 0.0232(8) 0.3007(8) 0.7110(4) 0.0627(18) Uani 1 1 d . A . H36 H 0.0703 0.3956 0.7256 0.075 Uiso 1 1 calc R . . Cl1 Cl 0.9161(2) 0.3735(2) 1.04986(11) 0.0875(6) Uani 1 1 d . . . Cl2 Cl 0.7342(2) 0.1720(2) 0.92883(11) 0.0882(6) Uani 1 1 d . . . C1 C 0.7709(8) 0.3463(7) 0.9831(4) 0.070(2) Uani 1 1 d . . . H1A H 0.7927 0.4127 0.9526 0.084 Uiso 1 1 calc R . . H1B H 0.6868 0.3642 1.0066 0.084 Uiso 1 1 calc R . . N1 N 0.2091(6) 0.0885(6) 0.8802(3) 0.0566(14) Uani 1 1 d . . . C2 C 0.1534(14) 0.2125(12) 0.9101(6) 0.146(5) Uani 1 1 d . . . H2A H 0.2060 0.2932 0.8958 0.218 Uiso 1 1 calc R . . H2B H 0.1630 0.2303 0.9624 0.218 Uiso 1 1 calc R . . H2C H 0.0539 0.1964 0.8921 0.218 Uiso 1 1 calc R . . C3 C 0.2055(16) 0.0621(14) 0.8022(5) 0.178(6) Uani 1 1 d . . . H3A H 0.2588 0.1442 0.7894 0.267 Uiso 1 1 calc R . . H3B H 0.1079 0.0425 0.7806 0.267 Uiso 1 1 calc R . . H3C H 0.2474 -0.0180 0.7845 0.267 Uiso 1 1 calc R . . C4 C 0.3554(12) 0.1151(15) 0.9126(6) 0.174(6) Uani 1 1 d . . . H4A H 0.4107 0.1955 0.8992 0.261 Uiso 1 1 calc R . . H4B H 0.3950 0.0331 0.8955 0.261 Uiso 1 1 calc R . . H4C H 0.3577 0.1342 0.9647 0.261 Uiso 1 1 calc R . . C5 C 0.1310(17) -0.0311(13) 0.9014(7) 0.190(7) Uani 1 1 d . . . H5A H 0.1351 -0.0107 0.9536 0.286 Uiso 1 1 calc R . . H5B H 0.1722 -0.1120 0.8844 0.286 Uiso 1 1 calc R . . H5C H 0.0328 -0.0512 0.8806 0.286 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 Au3 0.0685(2) 0.05752(19) 0.05438(17) 0.00113(11) -0.01747(12) -0.00644(13) As1 0.0752(7) 0.0462(5) 0.0442(4) 0.0163(3) -0.0014(4) 0.0065(4) As2 0.0735(8) 0.0557(6) 0.0608(6) 0.0026(4) 0.0009(5) 0.0241(5) As4 0.0513(15) 0.0745(16) 0.0591(13) 0.0304(10) -0.0066(9) 0.0023(11) B1 0.0752(7) 0.0462(5) 0.0442(4) 0.0163(3) -0.0014(4) 0.0065(4) B2 0.0735(8) 0.0557(6) 0.0608(6) 0.0026(4) 0.0009(5) 0.0241(5) B4 0.0513(15) 0.0745(16) 0.0591(13) 0.0304(10) -0.0066(9) 0.0023(11) B5 0.067(6) 0.054(5) 0.053(4) 0.013(3) 0.001(4) -0.019(4) B6 0.085(6) 0.040(4) 0.056(4) 0.008(3) -0.002(4) 0.005(4) As7 0.100(3) 0.062(2) 0.055(2) -0.0030(15) -0.0056(18) 0.021(2) As8 0.064(4) 0.102(5) 0.050(3) 0.003(2) -0.007(2) 0.006(3) B7 0.100(3) 0.062(2) 0.055(2) -0.0030(15) -0.0056(18) 0.021(2) B8 0.064(4) 0.102(5) 0.050(3) 0.003(2) -0.007(2) 0.006(3) B9 0.048(5) 0.066(5) 0.052(4) 0.018(3) -0.004(3) 0.011(4) B10 0.086(6) 0.051(4) 0.049(4) 0.004(3) -0.010(4) -0.011(4) B11 0.075(6) 0.049(4) 0.043(4) 0.002(3) 0.004(3) 0.008(4) B12 0.085(6) 0.057(5) 0.035(3) 0.008(3) -0.006(3) 0.001(4) P1 0.0403(9) 0.0446(8) 0.0412(7) 0.0053(6) -0.0037(6) 0.0035(7) C11 0.050(4) 0.041(3) 0.043(3) 0.005(2) 0.002(3) 0.010(3) C12 0.050(4) 0.065(4) 0.057(4) 0.012(3) 0.002(3) 0.000(3) C13 0.081(6) 0.071(5) 0.058(4) 0.019(3) 0.019(4) 0.007(4) C14 0.087(6) 0.077(5) 0.049(4) 0.025(3) 0.010(4) 0.031(5) C15 0.061(5) 0.078(5) 0.057(4) 0.021(3) 0.000(3) 0.021(4) C16 0.050(4) 0.060(4) 0.053(3) 0.018(3) 0.008(3) 0.011(3) C21 0.044(4) 0.042(3) 0.049(3) 0.009(3) 0.003(3) -0.003(3) C22 0.047(4) 0.062(4) 0.058(4) 0.003(3) 0.001(3) 0.008(3) C23 0.052(5) 0.055(4) 0.085(5) -0.011(4) 0.017(4) 0.000(4) C24 0.058(5) 0.054(5) 0.130(7) 0.024(5) 0.014(5) 0.015(4) C25 0.078(6) 0.075(5) 0.104(6) 0.032(5) -0.004(5) 0.033(5) C26 0.059(5) 0.066(5) 0.065(4) 0.022(3) -0.001(3) 0.016(4) C31 0.043(4) 0.055(4) 0.039(3) 0.012(3) 0.000(2) 0.014(3) C32 0.048(4) 0.061(4) 0.046(3) 0.010(3) 0.001(3) 0.005(3) C33 0.060(5) 0.076(5) 0.057(4) 0.023(4) 0.008(3) -0.008(4) C34 0.057(5) 0.118(7) 0.067(5) 0.041(5) 0.018(4) 0.011(5) C35 0.086(6) 0.100(7) 0.074(5) 0.025(5) 0.026(5) 0.048(6) C36 0.063(5) 0.067(4) 0.068(4) 0.022(3) 0.020(4) 0.027(4) Cl1 0.0713(13) 0.0969(15) 0.0833(13) 0.0197(11) -0.0100(10) -0.0002(11) Cl2 0.0854(15) 0.0815(13) 0.0842(13) -0.0018(10) -0.0049(11) 0.0152(12) C1 0.066(5) 0.068(5) 0.072(4) 0.013(4) -0.007(4) 0.015(4) N1 0.055(4) 0.071(4) 0.045(3) 0.018(2) 0.003(2) 0.011(3) C2 0.173(12) 0.135(10) 0.151(10) 0.028(8) 0.017(9) 0.095(9) C3 0.254(16) 0.249(16) 0.055(6) 0.030(7) 0.007(7) 0.121(13) C4 0.095(9) 0.250(16) 0.141(10) -0.039(10) -0.038(7) 0.062(10) C5 0.255(18) 0.121(10) 0.176(12) 0.051(9) 0.070(12) -0.038(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 Au3 P1 2.2459(16) . ? Au3 As8 2.378(5) . ? Au3 As7 2.506(3) . ? Au3 As4 2.537(2) . ? Au3 As2 2.6975(12) . ? Au3 As1 2.7094(12) . ? As1 B5 2.125(8) . ? As1 B6 2.183(7) . ? As1 As2 2.4611(15) . ? As1 As4 2.383(2) . ? As1 H1 1.10 . ? As2 B11 2.121(7) . ? As2 B6 2.173(9) . ? As2 As7 2.296(4) . ? As2 H2 1.10 . ? As4 As8 2.173(5) . ? As4 B9 2.032(7) . ? As4 B5 2.134(8) . ? As4 H4 1.10 . ? B5 B10 1.731(10) . ? B5 B9 1.760(11) . ? B5 B6 1.818(12) . ? B5 H5 1.10 . ? B6 B10 1.740(11) . ? B6 B11 1.818(11) . ? B6 H6 1.10 . ? As7 As8 2.108(7) . ? As7 B12 1.937(9) . ? As7 B11 1.998(8) . ? As7 H7 1.10 . ? As8 B12 1.873(8) . ? As8 B9 1.895(9) . ? As8 H8 1.10 . ? B9 B10 1.776(11) . ? B9 B12 1.777(11) . ? B9 H9 1.10 . ? B10 B11 1.769(12) . ? B10 B12 1.800(11) . ? B10 H10 1.10 . ? B11 B12 1.758(12) . ? B11 H11 1.10 . ? B12 H12 1.10 . ? P1 C11 1.821(6) . ? P1 C21 1.828(6) . ? P1 C31 1.833(6) . ? C11 C16 1.373(8) . ? C11 C12 1.397(8) . ? C12 C13 1.387(9) . ? C12 H12A 0.93 . ? C13 C14 1.356(10) . ? C13 H13 0.93 . ? C14 C15 1.380(9) . ? C14 H14 0.93 . ? C15 C16 1.382(8) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C21 C22 1.385(8) . ? C21 C26 1.391(9) . ? C22 C23 1.381(9) . ? C22 H22 0.93 . ? C23 C24 1.377(11) . ? C23 H23 0.93 . ? C24 C25 1.320(11) . ? C24 H24 0.93 . ? C25 C26 1.378(10) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C31 C36 1.375(8) . ? C31 C32 1.376(8) . ? C32 C33 1.378(9) . ? C32 H32 0.93 . ? C33 C34 1.346(10) . ? C33 H33 0.93 . ? C34 C35 1.356(11) . ? C34 H34 0.93 . ? C35 C36 1.383(10) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? Cl1 C1 1.754(7) . ? Cl2 C1 1.756(7) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? N1 C5 1.424(11) . ? N1 C3 1.439(9) . ? N1 C4 1.442(11) . ? N1 C2 1.445(10) . ? C2 H2A 0.96 . ? C2 H2B 0.96 . ? C2 H2C 0.96 . ? C3 H3A 0.96 . ? C3 H3B 0.96 . ? C3 H3C 0.96 . ? C4 H4A 0.96 . ? C4 H4B 0.96 . ? C4 H4C 0.96 . ? C5 H5A 0.96 . ? C5 H5B 0.96 . ? C5 H5C 0.96 . ? 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 P1 Au3 As8 139.14(15) . . ? P1 Au3 As7 132.79(11) . . ? As8 Au3 As7 51.04(16) . . ? P1 Au3 As4 131.07(7) . . ? As8 Au3 As4 52.35(14) . . ? As7 Au3 As4 92.62(11) . . ? P1 Au3 As2 125.37(5) . . ? As8 Au3 As2 89.84(14) . . ? As7 Au3 As2 52.22(9) . . ? As4 Au3 As2 94.70(6) . . ? P1 Au3 As1 126.02(5) . . ? As8 Au3 As1 90.00(14) . . ? As7 Au3 As1 91.84(10) . . ? As4 Au3 As1 53.90(6) . . ? As2 Au3 As1 54.15(4) . . ? B5 As1 B6 49.9(3) . . ? B5 As1 As2 95.8(2) . . ? B6 As1 As2 55.4(2) . . ? B5 As1 Au3 100.6(2) . . ? B6 As1 Au3 102.2(2) . . ? As2 As1 Au3 62.68(4) . . ? B5 As1 H1 122.6 . . ? B6 As1 H1 142.6 . . ? As2 As1 H1 139.8 . . ? Au3 As1 H1 115.0 . . ? B11 As2 B6 50.1(3) . . ? B11 As2 As7 53.6(2) . . ? B6 As2 As7 94.0(2) . . ? B11 As2 As1 96.1(2) . . ? B6 As2 As1 55.8(2) . . ? As7 As2 As1 103.97(11) . . ? B11 As2 Au3 100.5(2) . . ? B6 As2 Au3 102.8(2) . . ? As7 As2 Au3 59.61(8) . . ? As1 As2 Au3 63.17(4) . . ? B11 As2 H2 130.8 . . ? B6 As2 H2 130.0 . . ? As7 As2 H2 126.9 . . ? As1 As2 H2 124.0 . . ? Au3 As2 H2 121.4 . . ? B9 As4 B5 49.9(3) . . ? B9 As4 Au3 103.7(2) . . ? B5 As4 Au3 106.1(3) . . ? B9 As4 H4 130.0 . . ? B5 As4 H4 130.2 . . ? Au3 As4 H4 118.2 . . ? B10 B5 B9 61.2(4) . . ? B10 B5 B6 58.7(5) . . ? B9 B5 B6 108.3(5) . . ? B10 B5 As1 118.2(6) . . ? B9 B5 As1 117.4(4) . . ? B6 B5 As1 66.7(4) . . ? B10 B5 As4 116.4(5) . . ? B9 B5 As4 62.1(3) . . ? B6 B5 As4 119.3(5) . . ? As1 B5 As4 68.0(2) . . ? B10 B5 H5 118.7 . . ? B9 B5 H5 121.3 . . ? B6 B5 H5 119.4 . . ? As1 B5 H5 111.7 . . ? As4 B5 H5 113.7 . . ? B10 B6 B11 59.6(5) . . ? B10 B6 B5 58.2(5) . . ? B11 B6 B5 105.9(5) . . ? B10 B6 As2 115.9(5) . . ? B11 B6 As2 63.5(4) . . ? B5 B6 As2 117.1(4) . . ? B10 B6 As1 114.9(5) . . ? B11 B6 As1 117.0(4) . . ? B5 B6 As1 63.4(3) . . ? As2 B6 As1 68.8(2) . . ? B10 B6 H6 120.1 . . ? B11 B6 H6 121.5 . . ? B5 B6 H6 122.1 . . ? As2 B6 H6 113.0 . . ? As1 B6 H6 113.5 . . ? B12 As7 B11 53.0(4) . . ? B12 As7 As2 103.0(3) . . ? B11 As7 As2 58.7(2) . . ? B12 As7 Au3 107.4(3) . . ? B11 As7 Au3 111.0(3) . . ? As2 As7 Au3 68.18(10) . . ? B12 As7 H7 118.1 . . ? B11 As7 H7 140.5 . . ? As2 As7 H7 136.8 . . ? Au3 As7 H7 108.2 . . ? B12 As8 B9 56.3(4) . . ? B12 As8 Au3 115.1(4) . . ? B9 As8 Au3 114.7(3) . . ? B12 As8 H8 123.6 . . ? B9 As8 H8 124.5 . . ? Au3 As8 H8 112.1 . . ? B5 B9 B10 58.6(4) . . ? B5 B9 B12 108.6(6) . . ? B10 B9 B12 60.9(4) . . ? B5 B9 As8 116.9(5) . . ? B10 B9 As8 113.7(5) . . ? B12 B9 As8 61.2(4) . . ? B5 B9 As4 68.0(3) . . ? B10 B9 As4 119.4(4) . . ? B12 B9 As4 118.5(5) . . ? As8 B9 As4 67.1(3) . . ? B5 B9 H9 119.4 . . ? B10 B9 H9 119.2 . . ? B12 B9 H9 120.8 . . ? As8 B9 H9 116.4 . . ? As4 B9 H9 110.4 . . ? B5 B10 B6 63.2(5) . . ? B5 B10 B11 112.1(5) . . ? B6 B10 B11 62.4(5) . . ? B5 B10 B9 60.2(4) . . ? B6 B10 B9 111.2(5) . . ? B11 B10 B9 108.2(5) . . ? B5 B10 B12 108.9(5) . . ? B6 B10 B12 110.0(6) . . ? B11 B10 B12 59.0(5) . . ? B9 B10 B12 59.6(4) . . ? B5 B10 H10 119.5 . . ? B6 B10 H10 118.5 . . ? B11 B10 H10 120.6 . . ? B9 B10 H10 121.6 . . ? B12 B10 H10 122.3 . . ? B12 B11 B10 61.4(5) . . ? B12 B11 B6 108.4(6) . . ? B10 B11 B6 58.0(4) . . ? B12 B11 As7 61.7(4) . . ? B10 B11 As7 115.2(5) . . ? B6 B11 As7 118.0(4) . . ? B12 B11 As2 117.5(4) . . ? B10 B11 As2 117.2(4) . . ? B6 B11 As2 66.5(3) . . ? As7 B11 As2 67.7(2) . . ? B12 B11 H11 120.8 . . ? B10 B11 H11 119.4 . . ? B6 B11 H11 119.9 . . ? As7 B11 H11 114.7 . . ? As2 B11 H11 112.0 . . ? B11 B12 B9 108.7(5) . . ? B11 B12 B10 59.6(5) . . ? B9 B12 B10 59.6(5) . . ? B11 B12 As8 116.8(5) . . ? B9 B12 As8 62.5(4) . . ? B10 B12 As8 113.7(5) . . ? B11 B12 As7 65.2(4) . . ? B9 B12 As7 117.6(4) . . ? B10 B12 As7 116.7(5) . . ? As8 B12 As7 67.1(3) . . ? B11 B12 H12 119.8 . . ? B9 B12 H12 120.7 . . ? B10 B12 H12 120.0 . . ? As8 B12 H12 115.4 . . ? As7 B12 H12 112.6 . . ? C11 P1 C21 104.9(3) . . ? C11 P1 C31 104.3(3) . . ? C21 P1 C31 103.7(3) . . ? C11 P1 Au3 117.53(19) . . ? C21 P1 Au3 112.64(19) . . ? C31 P1 Au3 112.54(18) . . ? C16 C11 C12 118.2(5) . . ? C16 C11 P1 122.9(5) . . ? C12 C11 P1 118.9(5) . . ? C13 C12 C11 119.5(6) . . ? C13 C12 H12A 120.2 . . ? C11 C12 H12A 120.2 . . ? C14 C13 C12 121.3(7) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.9(6) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 119.2(7) . . ? C14 C15 H15 120.4 . . ? C16 C15 H15 120.4 . . ? C11 C16 C15 121.9(6) . . ? C11 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C22 C21 C26 119.4(6) . . ? C22 C21 P1 123.4(5) . . ? C26 C21 P1 117.2(5) . . ? C23 C22 C21 120.0(7) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C24 C23 C22 118.7(7) . . ? C24 C23 H23 120.6 . . ? C22 C23 H23 120.6 . . ? C25 C24 C23 121.7(7) . . ? C25 C24 H24 119.1 . . ? C23 C24 H24 119.1 . . ? C24 C25 C26 121.2(7) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C21 118.8(7) . . ? C25 C26 H26 120.6 . . ? C21 C26 H26 120.6 . . ? C36 C31 C32 119.1(6) . . ? C36 C31 P1 118.1(5) . . ? C32 C31 P1 122.7(5) . . ? C31 C32 C33 120.1(6) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C34 C33 C32 120.9(7) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 119.3(7) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 121.3(7) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C31 C36 C35 119.2(7) . . ? C31 C36 H36 120.4 . . ? C35 C36 H36 120.4 . . ? Cl1 C1 Cl2 111.1(4) . . ? Cl1 C1 H1A 109.4 . . ? Cl2 C1 H1A 109.4 . . ? Cl1 C1 H1B 109.4 . . ? Cl2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C5 N1 C3 111.2(9) . . ? C5 N1 C4 107.6(10) . . ? C3 N1 C4 109.6(8) . . ? C5 N1 C2 109.4(8) . . ? C3 N1 C2 111.8(7) . . ? C4 N1 C2 107.0(8) . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Au3 As1 B5 -158.0(2) . . . . ? As8 Au3 As1 B5 1.3(3) . . . . ? As7 Au3 As1 B5 52.3(3) . . . . ? As4 Au3 As1 B5 -39.6(2) . . . . ? As2 Au3 As1 B5 91.1(2) . . . . ? P1 Au3 As1 B6 151.1(2) . . . . ? As8 Au3 As1 B6 -49.7(3) . . . . ? As7 Au3 As1 B6 1.3(3) . . . . ? As4 Au3 As1 B6 -90.6(2) . . . . ? As2 Au3 As1 B6 40.1(2) . . . . ? P1 Au3 As1 As2 110.95(6) . . . . ? As8 Au3 As1 As2 -89.80(13) . . . . ? As7 Au3 As1 As2 -38.78(10) . . . . ? As4 Au3 As1 As2 -130.68(7) . . . . ? B5 As1 As2 B11 -0.3(3) . . . . ? B6 As1 As2 B11 -31.4(3) . . . . ? Au3 As1 As2 B11 98.7(2) . . . . ? B5 As1 As2 B6 31.1(3) . . . . ? Au3 As1 As2 B6 130.1(3) . . . . ? B5 As1 As2 As7 -54.2(2) . . . . ? B6 As1 As2 As7 -85.3(3) . . . . ? Au3 As1 As2 As7 44.76(10) . . . . ? B5 As1 As2 Au3 -99.0(2) . . . . ? B6 As1 As2 Au3 -130.1(3) . . . . ? P1 Au3 As2 B11 156.3(2) . . . . ? As8 Au3 As2 B11 -1.5(3) . . . . ? As7 Au3 As2 B11 36.0(3) . . . . ? As4 Au3 As2 B11 -53.7(2) . . . . ? As1 Au3 As2 B11 -91.6(2) . . . . ? P1 Au3 As2 B6 -152.6(2) . . . . ? As8 Au3 As2 B6 49.7(2) . . . . ? As7 Au3 As2 B6 87.2(2) . . . . ? As4 Au3 As2 B6 -2.5(2) . . . . ? As1 Au3 As2 B6 -40.4(2) . . . . ? P1 Au3 As2 As7 120.25(14) . . . . ? As8 Au3 As2 As7 -37.50(18) . . . . ? As4 Au3 As2 As7 -89.68(14) . . . . ? As1 Au3 As2 As7 -127.61(13) . . . . ? P1 Au3 As2 As1 -112.14(6) . . . . ? As8 Au3 As2 As1 90.12(13) . . . . ? As7 Au3 As2 As1 127.61(13) . . . . ? As4 Au3 As2 As1 37.94(5) . . . . ? P1 Au3 As4 B9 -158.5(2) . . . . ? As8 Au3 As4 B9 -32.0(3) . . . . ? As7 Au3 As4 B9 1.9(3) . . . . ? As2 Au3 As4 B9 54.2(2) . . . . ? As1 Au3 As4 B9 92.2(2) . . . . ? P1 Au3 As4 B5 149.8(2) . . . . ? As8 Au3 As4 B5 -83.7(3) . . . . ? As7 Au3 As4 B5 -49.9(2) . . . . ? As2 Au3 As4 B5 2.4(2) . . . . ? As1 Au3 As4 B5 40.5(2) . . . . ? B6 As1 B5 B10 29.2(5) . . . . ? As2 As1 B5 B10 -4.6(5) . . . . ? Au3 As1 B5 B10 -67.8(5) . . . . ? B6 As1 B5 B9 99.4(6) . . . . ? As2 As1 B5 B9 65.6(5) . . . . ? Au3 As1 B5 B9 2.4(6) . . . . ? As2 As1 B5 B6 -33.8(3) . . . . ? Au3 As1 B5 B6 -97.0(3) . . . . ? B6 As1 B5 As4 138.3(4) . . . . ? As2 As1 B5 As4 104.58(16) . . . . ? Au3 As1 B5 As4 41.35(19) . . . . ? B9 As4 B5 B10 -29.2(5) . . . . ? Au3 As4 B5 B10 65.4(6) . . . . ? Au3 As4 B5 B9 94.6(4) . . . . ? B9 As4 B5 B6 -96.4(6) . . . . ? Au3 As4 B5 B6 -1.8(5) . . . . ? B9 As4 B5 As1 -140.8(4) . . . . ? Au3 As4 B5 As1 -46.19(19) . . . . ? B9 B5 B6 B10 37.2(5) . . . . ? As1 B5 B6 B10 149.8(5) . . . . ? As4 B5 B6 B10 104.8(5) . . . . ? B10 B5 B6 B11 -37.2(5) . . . . ? B9 B5 B6 B11 0.0(6) . . . . ? As1 B5 B6 B11 112.6(5) . . . . ? As4 B5 B6 B11 67.7(6) . . . . ? B10 B5 B6 As2 -105.1(5) . . . . ? B9 B5 B6 As2 -67.9(6) . . . . ? As1 B5 B6 As2 44.7(4) . . . . ? As4 B5 B6 As2 -0.3(7) . . . . ? B10 B5 B6 As1 -149.8(5) . . . . ? B9 B5 B6 As1 -112.6(5) . . . . ? As4 B5 B6 As1 -45.0(4) . . . . ? B11 As2 B6 B10 29.3(5) . . . . ? As7 As2 B6 B10 -4.1(5) . . . . ? As1 As2 B6 B10 -108.2(5) . . . . ? Au3 As2 B6 B10 -63.8(5) . . . . ? As7 As2 B6 B11 -33.4(3) . . . . ? As1 As2 B6 B11 -137.5(4) . . . . ? Au3 As2 B6 B11 -93.1(3) . . . . ? B11 As2 B6 B5 95.1(6) . . . . ? As7 As2 B6 B5 61.7(5) . . . . ? As1 As2 B6 B5 -42.4(4) . . . . ? Au3 As2 B6 B5 2.0(5) . . . . ? B11 As2 B6 As1 137.5(4) . . . . ? As7 As2 B6 As1 104.16(17) . . . . ? Au3 As2 B6 As1 44.43(18) . . . . ? B5 As1 B6 B10 -28.1(5) . . . . ? As2 As1 B6 B10 109.7(6) . . . . ? Au3 As1 B6 B10 65.7(5) . . . . ? B5 As1 B6 B11 -95.2(6) . . . . ? As2 As1 B6 B11 42.7(5) . . . . ? Au3 As1 B6 B11 -1.4(6) . . . . ? As2 As1 B6 B5 137.8(4) . . . . ? Au3 As1 B6 B5 93.8(3) . . . . ? B5 As1 B6 As2 -137.8(4) . . . . ? Au3 As1 B6 As2 -44.05(19) . . . . ? B11 As2 As7 B12 -30.4(4) . . . . ? B6 As2 As7 B12 1.3(3) . . . . ? As1 As2 As7 B12 57.0(3) . . . . ? Au3 As2 As7 B12 103.7(3) . . . . ? B6 As2 As7 B11 31.6(4) . . . . ? As1 As2 As7 B11 87.3(3) . . . . ? Au3 As2 As7 B11 134.1(3) . . . . ? B11 As2 As7 Au3 -134.1(3) . . . . ? B6 As2 As7 Au3 -102.5(2) . . . . ? As1 As2 As7 Au3 -46.76(9) . . . . ? P1 Au3 As7 B12 156.3(3) . . . . ? As8 Au3 As7 B12 31.1(3) . . . . ? As4 Au3 As7 B12 -3.5(3) . . . . ? As2 Au3 As7 B12 -97.4(3) . . . . ? As1 Au3 As7 B12 -57.4(3) . . . . ? P1 Au3 As7 B11 -147.4(3) . . . . ? As8 Au3 As7 B11 87.4(4) . . . . ? As4 Au3 As7 B11 52.8(3) . . . . ? As2 Au3 As7 B11 -41.1(3) . . . . ? As1 Au3 As7 B11 -1.1(3) . . . . ? P1 Au3 As7 As2 -106.28(11) . . . . ? As8 Au3 As7 As2 128.5(2) . . . . ? As4 Au3 As7 As2 93.91(10) . . . . ? As1 Au3 As7 As2 39.97(9) . . . . ? P1 Au3 As8 B12 -147.8(3) . . . . ? As7 Au3 As8 B12 -34.2(3) . . . . ? As4 Au3 As8 B12 100.1(4) . . . . ? As2 Au3 As8 B12 4.0(4) . . . . ? As1 Au3 As8 B12 58.2(4) . . . . ? P1 Au3 As8 B9 149.5(3) . . . . ? As7 Au3 As8 B9 -96.9(4) . . . . ? As4 Au3 As8 B9 37.4(3) . . . . ? As2 Au3 As8 B9 -58.6(4) . . . . ? As1 Au3 As8 B9 -4.5(4) . . . . ? B6 B5 B9 B10 -36.1(5) . . . . ? As1 B5 B9 B10 -108.8(6) . . . . ? As4 B5 B9 B10 -150.1(5) . . . . ? B10 B5 B9 B12 36.1(5) . . . . ? B6 B5 B9 B12 0.0(7) . . . . ? As1 B5 B9 B12 -72.7(6) . . . . ? As4 B5 B9 B12 -114.0(5) . . . . ? B10 B5 B9 As8 102.6(6) . . . . ? B6 B5 B9 As8 66.5(6) . . . . ? As1 B5 B9 As8 -6.2(8) . . . . ? As4 B5 B9 As8 -47.5(4) . . . . ? B10 B5 B9 As4 150.1(5) . . . . ? B6 B5 B9 As4 114.0(5) . . . . ? As1 B5 B9 As4 41.3(4) . . . . ? B12 As8 B9 B5 -97.5(6) . . . . ? Au3 As8 B9 B5 7.2(7) . . . . ? B12 As8 B9 B10 -32.0(5) . . . . ? Au3 As8 B9 B10 72.7(5) . . . . ? Au3 As8 B9 B12 104.7(4) . . . . ? B12 As8 B9 As4 -145.4(4) . . . . ? Au3 As8 B9 As4 -40.7(3) . . . . ? Au3 As4 B9 B5 -99.6(4) . . . . ? B5 As4 B9 B10 29.2(5) . . . . ? Au3 As4 B9 B10 -70.4(5) . . . . ? B5 As4 B9 B12 100.0(6) . . . . ? Au3 As4 B9 B12 0.4(6) . . . . ? B5 As4 B9 As8 134.5(5) . . . . ? Au3 As4 B9 As8 34.9(3) . . . . ? B9 B5 B10 B6 -139.1(6) . . . . ? As1 B5 B10 B6 -31.6(5) . . . . ? As4 B5 B10 B6 -109.7(6) . . . . ? B9 B5 B10 B11 -99.0(6) . . . . ? B6 B5 B10 B11 40.1(5) . . . . ? As1 B5 B10 B11 8.5(7) . . . . ? As4 B5 B10 B11 -69.6(7) . . . . ? B6 B5 B10 B9 139.1(6) . . . . ? As1 B5 B10 B9 107.5(5) . . . . ? As4 B5 B10 B9 29.4(5) . . . . ? B9 B5 B10 B12 -35.6(6) . . . . ? B6 B5 B10 B12 103.4(6) . . . . ? As1 B5 B10 B12 71.8(7) . . . . ? As4 B5 B10 B12 -6.2(8) . . . . ? B11 B6 B10 B5 137.7(5) . . . . ? As2 B6 B10 B5 107.1(5) . . . . ? As1 B6 B10 B5 29.7(5) . . . . ? B5 B6 B10 B11 -137.7(5) . . . . ? As2 B6 B10 B11 -30.5(4) . . . . ? As1 B6 B10 B11 -107.9(5) . . . . ? B11 B6 B10 B9 100.1(6) . . . . ? B5 B6 B10 B9 -37.6(5) . . . . ? As2 B6 B10 B9 69.6(7) . . . . ? As1 B6 B10 B9 -7.8(8) . . . . ? B11 B6 B10 B12 36.0(5) . . . . ? B5 B6 B10 B12 -101.7(6) . . . . ? As2 B6 B10 B12 5.5(7) . . . . ? As1 B6 B10 B12 -71.9(7) . . . . ? B12 B9 B10 B5 -140.3(6) . . . . ? As8 B9 B10 B5 -108.1(6) . . . . ? As4 B9 B10 B5 -32.0(5) . . . . ? B5 B9 B10 B6 38.8(6) . . . . ? B12 B9 B10 B6 -101.4(6) . . . . ? As8 B9 B10 B6 -69.3(7) . . . . ? As4 B9 B10 B6 6.8(8) . . . . ? B5 B9 B10 B11 105.5(6) . . . . ? B12 B9 B10 B11 -34.8(5) . . . . ? As8 B9 B10 B11 -2.6(6) . . . . ? As4 B9 B10 B11 73.5(6) . . . . ? B5 B9 B10 B12 140.3(6) . . . . ? As8 B9 B10 B12 32.1(5) . . . . ? As4 B9 B10 B12 108.2(6) . . . . ? B5 B10 B11 B12 99.5(6) . . . . ? B6 B10 B11 B12 139.9(5) . . . . ? B9 B10 B11 B12 35.0(5) . . . . ? B5 B10 B11 B6 -40.4(5) . . . . ? B9 B10 B11 B6 -104.9(5) . . . . ? B12 B10 B11 B6 -139.9(5) . . . . ? B5 B10 B11 As7 68.1(7) . . . . ? B6 B10 B11 As7 108.5(5) . . . . ? B9 B10 B11 As7 3.6(6) . . . . ? B12 B10 B11 As7 -31.4(4) . . . . ? B5 B10 B11 As2 -8.7(7) . . . . ? B6 B10 B11 As2 31.8(5) . . . . ? B9 B10 B11 As2 -73.2(6) . . . . ? B12 B10 B11 As2 -108.1(5) . . . . ? B10 B6 B11 B12 -36.6(5) . . . . ? B5 B6 B11 B12 0.0(6) . . . . ? As2 B6 B11 B12 112.7(5) . . . . ? As1 B6 B11 B12 67.8(6) . . . . ? B5 B6 B11 B10 36.5(5) . . . . ? As2 B6 B11 B10 149.3(4) . . . . ? As1 B6 B11 B10 104.4(6) . . . . ? B10 B6 B11 As7 -103.7(6) . . . . ? B5 B6 B11 As7 -67.2(7) . . . . ? As2 B6 B11 As7 45.6(4) . . . . ? As1 B6 B11 As7 0.7(8) . . . . ? B10 B6 B11 As2 -149.3(4) . . . . ? B5 B6 B11 As2 -112.8(4) . . . . ? As1 B6 B11 As2 -44.9(4) . . . . ? As2 As7 B11 B12 -142.0(4) . . . . ? Au3 As7 B11 B12 -96.4(4) . . . . ? B12 As7 B11 B10 31.3(5) . . . . ? As2 As7 B11 B10 -110.7(5) . . . . ? Au3 As7 B11 B10 -65.1(5) . . . . ? B12 As7 B11 B6 96.9(7) . . . . ? As2 As7 B11 B6 -45.1(5) . . . . ? Au3 As7 B11 B6 0.5(6) . . . . ? B12 As7 B11 As2 142.0(4) . . . . ? Au3 As7 B11 As2 45.6(3) . . . . ? B6 As2 B11 B12 -99.3(6) . . . . ? As7 As2 B11 B12 37.7(4) . . . . ? As1 As2 B11 B12 -65.1(5) . . . . ? Au3 As2 B11 B12 -1.3(6) . . . . ? B6 As2 B11 B10 -29.1(5) . . . . ? As7 As2 B11 B10 107.9(5) . . . . ? As1 As2 B11 B10 5.0(5) . . . . ? Au3 As2 B11 B10 68.8(5) . . . . ? As7 As2 B11 B6 137.0(4) . . . . ? As1 As2 B11 B6 34.2(3) . . . . ? Au3 As2 B11 B6 97.9(3) . . . . ? B6 As2 B11 As7 -137.0(4) . . . . ? As1 As2 B11 As7 -102.9(2) . . . . ? Au3 As2 B11 As7 -39.1(2) . . . . ? B10 B11 B12 B9 -35.1(5) . . . . ? B6 B11 B12 B9 0.1(7) . . . . ? As7 B11 B12 B9 112.5(5) . . . . ? As2 B11 B12 B9 72.5(6) . . . . ? B6 B11 B12 B10 35.1(5) . . . . ? As7 B11 B12 B10 147.6(4) . . . . ? As2 B11 B12 B10 107.6(5) . . . . ? B10 B11 B12 As8 -103.0(6) . . . . ? B6 B11 B12 As8 -67.9(7) . . . . ? As7 B11 B12 As8 44.6(5) . . . . ? As2 B11 B12 As8 4.6(8) . . . . ? B10 B11 B12 As7 -147.6(4) . . . . ? B6 B11 B12 As7 -112.5(5) . . . . ? As2 B11 B12 As7 -40.0(4) . . . . ? B5 B9 B12 B11 0.0(7) . . . . ? B10 B9 B12 B11 35.1(5) . . . . ? As8 B9 B12 B11 -111.1(5) . . . . ? As4 B9 B12 B11 -74.6(6) . . . . ? B5 B9 B12 B10 -35.2(5) . . . . ? As8 B9 B12 B10 -146.2(5) . . . . ? As4 B9 B12 B10 -109.7(5) . . . . ? B5 B9 B12 As8 111.1(5) . . . . ? B10 B9 B12 As8 146.2(5) . . . . ? As4 B9 B12 As8 36.5(5) . . . . ? B5 B9 B12 As7 71.2(6) . . . . ? B10 B9 B12 As7 106.3(6) . . . . ? As8 B9 B12 As7 -39.9(5) . . . . ? As4 B9 B12 As7 -3.4(8) . . . . ? B5 B10 B12 B11 -104.9(6) . . . . ? B6 B10 B12 B11 -37.4(5) . . . . ? B9 B10 B12 B11 -140.8(5) . . . . ? B5 B10 B12 B9 35.9(6) . . . . ? B6 B10 B12 B9 103.4(6) . . . . ? B11 B10 B12 B9 140.8(5) . . . . ? B5 B10 B12 As8 3.4(8) . . . . ? B6 B10 B12 As8 70.9(7) . . . . ? B11 B10 B12 As8 108.3(6) . . . . ? B9 B10 B12 As8 -32.6(5) . . . . ? B5 B10 B12 As7 -71.9(7) . . . . ? B6 B10 B12 As7 -4.4(7) . . . . ? B11 B10 B12 As7 33.0(5) . . . . ? B9 B10 B12 As7 -107.9(5) . . . . ? B9 As8 B12 B11 98.1(6) . . . . ? Au3 As8 B12 B11 -5.9(7) . . . . ? Au3 As8 B12 B9 -104.0(4) . . . . ? B9 As8 B12 B10 31.5(5) . . . . ? Au3 As8 B12 B10 -72.5(6) . . . . ? B9 As8 B12 As7 141.9(4) . . . . ? Au3 As8 B12 As7 37.9(3) . . . . ? As2 As7 B12 B11 32.7(3) . . . . ? Au3 As7 B12 B11 103.6(4) . . . . ? B11 As7 B12 B9 -99.0(6) . . . . ? As2 As7 B12 B9 -66.3(5) . . . . ? Au3 As7 B12 B9 4.6(6) . . . . ? B11 As7 B12 B10 -31.1(5) . . . . ? As2 As7 B12 B10 1.6(5) . . . . ? Au3 As7 B12 B10 72.5(5) . . . . ? B11 As7 B12 As8 -137.2(5) . . . . ? As2 As7 B12 As8 -104.4(3) . . . . ? Au3 As7 B12 As8 -33.6(3) . . . . ? As8 Au3 P1 C11 -162.9(3) . . . . ? As7 Au3 P1 C11 121.0(2) . . . . ? As4 Au3 P1 C11 -86.2(2) . . . . ? As2 Au3 P1 C11 52.5(2) . . . . ? As1 Au3 P1 C11 -15.7(2) . . . . ? As8 Au3 P1 C21 -40.8(3) . . . . ? As7 Au3 P1 C21 -116.9(2) . . . . ? As4 Au3 P1 C21 35.8(2) . . . . ? As2 Au3 P1 C21 174.6(2) . . . . ? As1 Au3 P1 C21 106.4(2) . . . . ? As8 Au3 P1 C31 76.0(3) . . . . ? As7 Au3 P1 C31 -0.2(3) . . . . ? As4 Au3 P1 C31 152.6(2) . . . . ? As2 Au3 P1 C31 -68.6(2) . . . . ? As1 Au3 P1 C31 -136.8(2) . . . . ? C21 P1 C11 C16 88.9(5) . . . . ? C31 P1 C11 C16 -19.7(6) . . . . ? Au3 P1 C11 C16 -145.1(4) . . . . ? C21 P1 C11 C12 -89.8(5) . . . . ? C31 P1 C11 C12 161.5(5) . . . . ? Au3 P1 C11 C12 36.2(5) . . . . ? C16 C11 C12 C13 -1.5(9) . . . . ? P1 C11 C12 C13 177.3(5) . . . . ? C11 C12 C13 C14 0.7(11) . . . . ? C12 C13 C14 C15 0.1(11) . . . . ? C13 C14 C15 C16 -0.1(11) . . . . ? C12 C11 C16 C15 1.6(9) . . . . ? P1 C11 C16 C15 -177.2(5) . . . . ? C14 C15 C16 C11 -0.8(10) . . . . ? C11 P1 C21 C22 -22.4(6) . . . . ? C31 P1 C21 C22 86.7(6) . . . . ? Au3 P1 C21 C22 -151.4(5) . . . . ? C11 P1 C21 C26 158.7(5) . . . . ? C31 P1 C21 C26 -92.2(5) . . . . ? Au3 P1 C21 C26 29.8(5) . . . . ? C26 C21 C22 C23 2.5(10) . . . . ? P1 C21 C22 C23 -176.4(5) . . . . ? C21 C22 C23 C24 0.3(10) . . . . ? C22 C23 C24 C25 -2.1(12) . . . . ? C23 C24 C25 C26 1.1(13) . . . . ? C24 C25 C26 C21 1.7(12) . . . . ? C22 C21 C26 C25 -3.5(10) . . . . ? P1 C21 C26 C25 175.4(6) . . . . ? C11 P1 C31 C36 -89.9(5) . . . . ? C21 P1 C31 C36 160.6(5) . . . . ? Au3 P1 C31 C36 38.6(5) . . . . ? C11 P1 C31 C32 92.9(5) . . . . ? C21 P1 C31 C32 -16.6(5) . . . . ? Au3 P1 C31 C32 -138.6(4) . . . . ? C36 C31 C32 C33 1.7(9) . . . . ? P1 C31 C32 C33 178.9(5) . . . . ? C31 C32 C33 C34 -2.1(10) . . . . ? C32 C33 C34 C35 2.3(11) . . . . ? C33 C34 C35 C36 -2.1(12) . . . . ? C32 C31 C36 C35 -1.5(9) . . . . ? P1 C31 C36 C35 -178.8(5) . . . . ? C34 C35 C36 C31 1.7(11) . . . . ? _refine_diff_density_max 0.953 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.105 # Attachment '270403.txt' ####################################################################### # # 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_7 # GF9468 _database_code_depnum_ccdc_archive 'CCDC 270403' #_vrf_PLAT201_compound7 #; #PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 20 #RESPONSE: These 20 atoms are the boron atoms in the two disordered #AuTeB~10~ cages; see experimental text. #; #_vrf_PLAT305_compound7 #; #PROBLEM: Isolated Hydrogen Atom (Outside Bond Range ??) #RESPONSE: This is an artefact of the Checkcif routine. #The isolated H atom is low occupancy "H21" bonded to low occupancy #B21 - on the same site as Te21. #; # end Validation Reply Form _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H25 Au B10 P Te, C8 H20 N' _chemical_formula_sum 'C26 H45 Au B10 N P Te' _chemical_formula_weight 835.27 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 20.705(3) _cell_length_b 8.6844(9) _cell_length_c 37.396(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6724.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 294(1) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3232 _exptl_absorpt_coefficient_mu 5.292 _exptl_absorpt_correction_type psi-scan # 'empirical, \y-scans at 4\% steps (North, Phillips & Mathews, 1968)' _exptl_absorpt_process_details '(North, Philips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.3703 _exptl_absorpt_correction_T_max 0.5603 _diffrn_ambient_temperature 294(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 1.5 _diffrn_reflns_number 7421 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.97 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _reflns_number_total 7421 _reflns_number_gt 3744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 (Enraf-Nonius, 1992)' _computing_cell_refinement 'SET4 & CELDIM (Enraf-Nonius, 1992)' _computing_data_reduction 'DATRD2 in NRCVAX96 (Gabe, Le Page, Charland, Lee & White, 1989)' _computing_structure_solution 'NRCVAX96 via Patterson heavy-atom method' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976), PLATON (Spek, 2003)' _computing_publication_material SHELXL97 _refine_special_details ; Compound 7 crystallised in the orthorhombic system; space groups Pna2~1~ or Pnam allowed from the systematic absences. Structure solution was only possible in Pna2~1~ with two independent anions and two independent (Et~4~N)^+^ cations in the asymmetric unit. It soon became apparent from electron-density peak heights and numerous subsequent refinement trials that in each case there was some B/Te interchange at the TeB4 face bonded to the gold atom. In one anion the Te atom was disordered unequally over three sites; in the other it was disordered unequally over two sites. For the final refinement with the SHELXL97 programme, each disordered site was allowed for as a Te/B mixture with the occupancies restrained so that the sum of the Te occupancies added to 1. At each disordered site the boron occupancy was set at {1 - (occupancy of Te)}. Because of the disorder, all the B atoms were only refined isotropically with an overall Uiso value. The disorder may very well affect the crystal packing and several phenyl C atoms have prolate ellipsoids; DELU and SIMU restraints were used for markedly anisotropic atoms in the cations. H atoms were treated as riding atoms (C-H 0.93 to 0.97, B-H 1.10\%A). ; _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^)+(0.0453P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.54(3) _refine_ls_number_reflns 7421 _refine_ls_number_parameters 608 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1269 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.902 _refine_ls_shift/su_max 0.007 _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 Au2 Au 0.23144(4) 0.23287(9) 0.057361(18) 0.0485(3) Uani 1 1 d . . . Te1 Te 0.19831(8) 0.43233(19) 0.00008(9) 0.0560(5) Uani 0.911(3) 1 d P A . Te3 Te 0.1188(9) 0.303(2) 0.0329(5) 0.0578(12) Uiso 0.028(3) 1 d P A . Te7 Te 0.2111(6) 0.0435(15) 0.0161(3) 0.0578(12) Uiso 0.061(3) 1 d P A . B1 B 0.19831(8) 0.43233(19) 0.00008(9) 0.0560(5) Uani 0.089(3) 1 d P A -1 H1 H 0.2136 0.5535 -0.0013 0.067 Uiso 0.089(3) 1 calc PR A -1 B3 B 0.1188(9) 0.303(2) 0.0329(5) 0.0578(12) Uiso 0.972(3) 1 d P A -1 H3 H 0.0914 0.3768 0.0513 0.069 Uiso 0.972(3) 1 calc PR A -1 B4 B 0.1049(13) 0.308(3) -0.0180(7) 0.0578(12) Uiso 1 1 d . . . H4 H 0.0686 0.3848 -0.0300 0.069 Uiso 1 1 calc R A . B5 B 0.1861(15) 0.243(3) -0.0416(8) 0.0578(12) Uiso 1 1 d . A . H5 H 0.2004 0.2831 -0.0684 0.069 Uiso 1 1 calc R . . B6 B 0.2497(14) 0.196(3) -0.0089(7) 0.0578(12) Uiso 1 1 d . A . H6 H 0.3014 0.2051 -0.0154 0.069 Uiso 1 1 calc R . . B7 B 0.2111(6) 0.0435(15) 0.0161(3) 0.0578(12) Uiso 0.939(3) 1 d P A -1 H7 H 0.2427 -0.0508 0.0250 0.069 Uiso 0.939(3) 1 calc PR A -1 B8 B 0.1378(12) 0.101(3) 0.0416(7) 0.0578(12) Uiso 1 1 d . A . H8 H 0.1201 0.0504 0.0668 0.069 Uiso 1 1 calc R . . B9 B 0.0832(13) 0.154(3) 0.0078(7) 0.0578(12) Uiso 1 1 d . A . H9 H 0.0310 0.1370 0.0119 0.069 Uiso 1 1 calc R . . B10 B 0.1197(12) 0.120(3) -0.0353(7) 0.0578(12) Uiso 1 1 d . A . H10 H 0.0918 0.0812 -0.0586 0.069 Uiso 1 1 calc R . . B11 B 0.1985(12) 0.062(3) -0.0296(8) 0.0578(12) Uiso 1 1 d . . . H11 H 0.2209 -0.0141 -0.0495 0.069 Uiso 1 1 calc R A . B12 B 0.1370(11) -0.003(3) 0.0018(7) 0.0578(12) Uiso 1 1 d . A . H12 H 0.1205 -0.1233 0.0032 0.069 Uiso 1 1 calc R . . P1 P 0.2811(3) 0.3270(6) 0.10581(16) 0.0393(12) Uani 1 1 d . A . C11 C 0.2924(9) 0.541(2) 0.1032(5) 0.042(5) Uani 1 1 d . . . C12 C 0.2373(12) 0.627(2) 0.0939(7) 0.056(7) Uani 1 1 d . A . H12A H 0.1977 0.5816 0.0889 0.067 Uiso 1 1 calc R . . C13 C 0.2468(16) 0.790(3) 0.0927(8) 0.080(9) Uani 1 1 d . . . H13 H 0.2126 0.8539 0.0862 0.095 Uiso 1 1 calc R A . C14 C 0.3046(12) 0.855(2) 0.1010(5) 0.047(5) Uani 1 1 d U A . H14 H 0.3087 0.9612 0.1004 0.056 Uiso 1 1 calc R . . C15 C 0.3574(13) 0.768(2) 0.1104(8) 0.059(7) Uani 1 1 d . . . H15 H 0.3969 0.8133 0.1158 0.071 Uiso 1 1 calc R A . C16 C 0.3493(13) 0.606(3) 0.1114(6) 0.062(7) Uani 1 1 d . A . H16 H 0.3839 0.5436 0.1178 0.075 Uiso 1 1 calc R . . C21 C 0.3606(11) 0.256(2) 0.1139(7) 0.047(6) Uani 1 1 d . . . C22 C 0.4044(11) 0.247(2) 0.0860(6) 0.060(6) Uani 1 1 d U A . H22 H 0.3893 0.2691 0.0632 0.071 Uiso 1 1 calc R . . C23 C 0.4642(12) 0.211(4) 0.0893(10) 0.115(13) Uani 1 1 d . . . H23 H 0.4926 0.2227 0.0703 0.138 Uiso 1 1 calc R A . C24 C 0.4858(12) 0.153(3) 0.1223(7) 0.077(8) Uani 1 1 d . A . H24 H 0.5277 0.1158 0.1246 0.092 Uiso 1 1 calc R . . C25 C 0.4457(12) 0.152(3) 0.1505(6) 0.073(7) Uani 1 1 d . . . H25 H 0.4583 0.1162 0.1728 0.088 Uiso 1 1 calc R A . C26 C 0.3830(12) 0.211(3) 0.1440(7) 0.067(8) Uani 1 1 d . A . H26 H 0.3553 0.2162 0.1635 0.081 Uiso 1 1 calc R . . C31 C 0.2353(13) 0.301(3) 0.1478(6) 0.056(7) Uani 1 1 d . . . C32 C 0.1950(10) 0.186(3) 0.1497(6) 0.060(7) Uani 1 1 d . A . H32 H 0.1906 0.1168 0.1309 0.072 Uiso 1 1 calc R . . C33 C 0.1585(12) 0.170(4) 0.1812(7) 0.098(10) Uani 1 1 d . . . H33 H 0.1261 0.0961 0.1820 0.117 Uiso 1 1 calc R A . C34 C 0.1687(11) 0.260(3) 0.2103(7) 0.069(9) Uani 1 1 d . A . H34 H 0.1468 0.2398 0.2315 0.083 Uiso 1 1 calc R . . C35 C 0.2112(11) 0.378(3) 0.2084(7) 0.070(7) Uani 1 1 d . . . H35 H 0.2159 0.4465 0.2274 0.083 Uiso 1 1 calc R A . C36 C 0.2475(11) 0.396(2) 0.1774(6) 0.062(6) Uani 1 1 d . A . H36 H 0.2798 0.4704 0.1763 0.074 Uiso 1 1 calc R . . Au22 Au 0.01256(4) 0.76541(9) 0.295680(18) 0.0494(3) Uani 1 1 d . . . Te21 Te 0.04630(8) 0.96863(18) 0.35263(8) 0.0599(5) Uani 0.956(3) 1 d P B . Te27 Te 0.0466(8) 0.5618(17) 0.3515(5) 0.0578(12) Uiso 0.044(2) 1 d P B . B21 B 0.04630(8) 0.96863(18) 0.35263(8) 0.0599(5) Uani 0.044(3) 1 d P B -2 H21 H 0.0297 1.0888 0.3538 0.072 Uiso 0.045(3) 1 calc PR B -2 B23 B 0.1261(13) 0.843(3) 0.3186(7) 0.0578(12) Uiso 1 1 d . B . H23A H 0.1523 0.9182 0.2998 0.069 Uiso 1 1 calc R . . B24 B 0.1402(13) 0.848(3) 0.3699(7) 0.0578(12) Uiso 1 1 d . . . H24A H 0.1758 0.9294 0.3809 0.069 Uiso 1 1 calc R B . B25 B 0.0642(15) 0.784(3) 0.3975(8) 0.0578(12) Uiso 1 1 d . B . H25A H 0.0535 0.8226 0.4249 0.069 Uiso 1 1 calc R . . B26 B -0.0036(14) 0.728(3) 0.3632(7) 0.0578(12) Uiso 1 1 d . B . H26A H -0.0560 0.7388 0.3673 0.069 Uiso 1 1 calc R . . B27 B 0.0466(8) 0.5618(17) 0.3515(5) 0.0578(12) Uiso 0.956(2) 1 d P B -2 H27 H 0.0109 0.4770 0.3421 0.069 Uiso 0.956(2) 1 calc PR B -2 B28 B 0.1089(12) 0.630(3) 0.3103(7) 0.0578(12) Uiso 1 1 d . B . H28 H 0.1228 0.5802 0.2843 0.069 Uiso 1 1 calc R . . B29 B 0.1637(13) 0.692(3) 0.3453(7) 0.0578(12) Uiso 1 1 d . B . H29 H 0.2158 0.6743 0.3415 0.069 Uiso 1 1 calc R . . B210 B 0.1298(13) 0.666(3) 0.3871(7) 0.0578(12) Uiso 1 1 d . B . H210 H 0.1610 0.6332 0.4097 0.069 Uiso 1 1 calc R . . B211 B 0.0484(12) 0.588(3) 0.3818(8) 0.0578(12) Uiso 1 1 d . . . H211 H 0.0235 0.5115 0.4008 0.069 Uiso 1 1 calc R B . B212 B 0.1068(12) 0.531(3) 0.3521(7) 0.0578(12) Uiso 1 1 d . B . H212 H 0.1227 0.4114 0.3481 0.069 Uiso 1 1 calc R . . P2 P -0.0371(3) 0.8595(6) 0.24638(16) 0.0384(12) Uani 1 1 d . B . C41 C -0.0471(12) 1.068(2) 0.2471(6) 0.053(6) Uani 1 1 d . . . C42 C 0.0023(12) 1.160(3) 0.2580(6) 0.059(7) Uani 1 1 d . B . H42 H 0.0405 1.1112 0.2645 0.070 Uiso 1 1 calc R . . C43 C 0.0015(16) 1.316(3) 0.2604(6) 0.072(8) Uani 1 1 d . . . H43 H 0.0385 1.3709 0.2662 0.087 Uiso 1 1 calc R B . C44 C -0.0540(15) 1.386(3) 0.2541(7) 0.083(9) Uani 1 1 d U B . H44 H -0.0569 1.4924 0.2570 0.100 Uiso 1 1 calc R . . C45 C -0.1094(13) 1.301(3) 0.2429(6) 0.064(7) Uani 1 1 d . . . H45 H -0.1482 1.3508 0.2381 0.077 Uiso 1 1 calc R B . C46 C -0.1041(10) 1.144(2) 0.2395(5) 0.037(5) Uani 1 1 d . B . H46 H -0.1397 1.0875 0.2320 0.044 Uiso 1 1 calc R . . C51 C -0.1186(9) 0.783(2) 0.2380(6) 0.031(5) Uani 1 1 d . . . C52 C -0.1649(11) 0.803(3) 0.2644(7) 0.061(5) Uani 1 1 d U B . H52 H -0.1544 0.8568 0.2851 0.074 Uiso 1 1 calc R . . C53 C -0.2280(12) 0.742(2) 0.2601(9) 0.063(5) Uani 1 1 d U . . H53 H -0.2579 0.7425 0.2786 0.076 Uiso 1 1 calc R B . C54 C -0.2417(11) 0.686(3) 0.2281(8) 0.080(9) Uani 1 1 d . B . H54 H -0.2838 0.6530 0.2242 0.096 Uiso 1 1 calc R . . C55 C -0.1995(11) 0.671(3) 0.2005(6) 0.068(7) Uani 1 1 d . . . H55 H -0.2135 0.6276 0.1791 0.081 Uiso 1 1 calc R B . C56 C -0.1358(11) 0.721(2) 0.2034(5) 0.051(6) Uani 1 1 d . B . H56 H -0.1065 0.7145 0.1846 0.061 Uiso 1 1 calc R . . C61 C 0.0083(9) 0.826(2) 0.2045(5) 0.036(4) Uani 1 1 d U . . C62 C 0.048(2) 0.709(3) 0.2019(9) 0.104(12) Uani 1 1 d . B . H62 H 0.0518 0.6434 0.2214 0.125 Uiso 1 1 calc R . . C63 C 0.0861(16) 0.677(4) 0.1701(9) 0.101(10) Uani 1 1 d . . . H63 H 0.1161 0.5980 0.1689 0.121 Uiso 1 1 calc R B . C64 C 0.0735(16) 0.776(4) 0.1421(10) 0.097(11) Uani 1 1 d . B . H64 H 0.0963 0.7613 0.1210 0.116 Uiso 1 1 calc R . . C65 C 0.0310(11) 0.892(3) 0.1432(6) 0.063(7) Uani 1 1 d . . . H65 H 0.0237 0.9519 0.1230 0.076 Uiso 1 1 calc R B . C66 C -0.0027(10) 0.922(2) 0.1752(5) 0.053(6) Uani 1 1 d . B . H66 H -0.0315 1.0040 0.1768 0.063 Uiso 1 1 calc R . . N1 N 0.4171(6) 0.7707(16) -0.0072(4) 0.035(4) Uani 1 1 d D . . C71 C 0.3917(10) 0.926(2) 0.0046(7) 0.071(7) Uani 1 1 d D . . H71A H 0.3881 0.9250 0.0304 0.086 Uiso 1 1 calc R . . H71B H 0.3484 0.9381 -0.0049 0.086 Uiso 1 1 calc R . . C72 C 0.4307(12) 1.067(3) -0.0060(7) 0.085(8) Uani 1 1 d D . . H72A H 0.4098 1.1580 0.0028 0.128 Uiso 1 1 calc R . . H72B H 0.4338 1.0722 -0.0316 0.128 Uiso 1 1 calc R . . H72C H 0.4733 1.0597 0.0040 0.128 Uiso 1 1 calc R . . C73 C 0.3705(10) 0.657(2) 0.0080(6) 0.057(6) Uani 1 1 d D . . H73A H 0.3277 0.6801 -0.0012 0.069 Uiso 1 1 calc R . . H73B H 0.3692 0.6700 0.0337 0.069 Uiso 1 1 calc R . . C74 C 0.3858(12) 0.487(3) -0.0003(8) 0.101(9) Uani 1 1 d D . . H74A H 0.3545 0.4219 0.0112 0.152 Uiso 1 1 calc R . . H74B H 0.4282 0.4621 0.0085 0.152 Uiso 1 1 calc R . . H74C H 0.3843 0.4704 -0.0257 0.152 Uiso 1 1 calc R . . C75 C 0.4158(14) 0.757(3) -0.0468(6) 0.088(11) Uani 1 1 d D . . H75A H 0.4359 0.6607 -0.0534 0.106 Uiso 1 1 calc R . . H75B H 0.4419 0.8397 -0.0567 0.106 Uiso 1 1 calc R . . C76 C 0.3500(15) 0.764(3) -0.0636(8) 0.110(13) Uani 1 1 d D . . H76A H 0.3539 0.7501 -0.0890 0.166 Uiso 1 1 calc R . . H76B H 0.3307 0.8626 -0.0588 0.166 Uiso 1 1 calc R . . H76C H 0.3233 0.6842 -0.0538 0.166 Uiso 1 1 calc R . . C77 C 0.4841(9) 0.748(3) 0.0039(9) 0.074(10) Uani 1 1 d D . . H77A H 0.5100 0.8246 -0.0085 0.089 Uiso 1 1 calc R . . H77B H 0.4976 0.6483 -0.0050 0.089 Uiso 1 1 calc R . . C78 C 0.5024(17) 0.756(3) 0.0434(8) 0.082(10) Uani 1 1 d D . . H78A H 0.5479 0.7373 0.0460 0.123 Uiso 1 1 calc R . . H78B H 0.4788 0.6789 0.0564 0.123 Uiso 1 1 calc R . . H78C H 0.4921 0.8559 0.0527 0.123 Uiso 1 1 calc R . . N2 N -0.1739(8) 0.2813(18) 0.3585(5) 0.052(5) Uani 1 1 d D . . C81 C -0.1724(12) 0.290(3) 0.3995(4) 0.067(8) Uani 1 1 d D . . H81A H -0.1988 0.3769 0.4069 0.080 Uiso 1 1 calc R . . H81B H -0.1923 0.1977 0.4090 0.080 Uiso 1 1 calc R . . C82 C -0.1062(11) 0.308(3) 0.4163(7) 0.087(10) Uani 1 1 d D . . H82A H -0.1105 0.3138 0.4419 0.130 Uiso 1 1 calc R . . H82B H -0.0861 0.3999 0.4076 0.130 Uiso 1 1 calc R . . H82C H -0.0800 0.2204 0.4102 0.130 Uiso 1 1 calc R . . C83 C -0.1359(10) 0.147(3) 0.3461(7) 0.081(9) Uani 1 1 d D . . H83A H -0.0908 0.1635 0.3521 0.097 Uiso 1 1 calc R . . H83B H -0.1391 0.1400 0.3203 0.097 Uiso 1 1 calc R . . C84 C -0.1578(14) -0.002(2) 0.3623(7) 0.109(12) Uani 1 1 d D . . H84A H -0.1319 -0.0844 0.3531 0.164 Uiso 1 1 calc R . . H84B H -0.2023 -0.0192 0.3563 0.164 Uiso 1 1 calc R . . H84C H -0.1532 0.0032 0.3878 0.164 Uiso 1 1 calc R . . C85 C -0.1424(10) 0.425(2) 0.3408(6) 0.057(6) Uani 1 1 d DU . . H85A H -0.0987 0.4375 0.3498 0.069 Uiso 1 1 calc R . . H85B H -0.1399 0.4101 0.3152 0.069 Uiso 1 1 calc R . . C86 C -0.1812(13) 0.570(2) 0.3488(8) 0.105(10) Uani 1 1 d D . . H86A H -0.1618 0.6563 0.3370 0.158 Uiso 1 1 calc R . . H86B H -0.1818 0.5877 0.3742 0.158 Uiso 1 1 calc R . . H86C H -0.2247 0.5568 0.3404 0.158 Uiso 1 1 calc R . . C87 C -0.2433(9) 0.262(2) 0.3469(7) 0.043(6) Uani 1 1 d D . . H87A H -0.2682 0.3497 0.3550 0.052 Uiso 1 1 calc R . . H87B H -0.2611 0.1706 0.3582 0.052 Uiso 1 1 calc R . . C88 C -0.2505(19) 0.247(3) 0.3062(8) 0.101(12) Uani 1 1 d D . . H88A H -0.2952 0.2324 0.3003 0.152 Uiso 1 1 calc R . . H88B H -0.2261 0.1595 0.2980 0.152 Uiso 1 1 calc R . . H88C H -0.2347 0.3383 0.2949 0.152 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 Au2 0.0550(6) 0.0470(5) 0.0434(6) -0.0010(5) -0.0117(5) -0.0069(4) Te1 0.0423(9) 0.0589(10) 0.0669(11) 0.0203(9) 0.0044(8) 0.0010(8) B1 0.0423(9) 0.0589(10) 0.0669(11) 0.0203(9) 0.0044(8) 0.0010(8) P1 0.044(3) 0.037(3) 0.037(3) 0.002(2) -0.002(2) 0.002(2) C11 0.033(11) 0.067(14) 0.025(9) -0.006(9) 0.012(8) 0.013(11) C12 0.063(16) 0.029(11) 0.076(16) 0.011(10) 0.003(13) 0.021(12) C13 0.10(2) 0.060(16) 0.08(2) 0.018(15) 0.052(18) 0.010(17) C14 0.071(10) 0.031(8) 0.039(8) -0.010(7) 0.005(7) 0.003(8) C15 0.068(16) 0.051(15) 0.058(16) -0.002(12) 0.016(12) -0.003(13) C16 0.10(2) 0.054(14) 0.038(12) -0.020(10) -0.005(12) -0.009(14) C21 0.058(14) 0.053(14) 0.030(12) -0.006(10) 0.005(10) -0.001(11) C22 0.064(9) 0.067(10) 0.048(8) 0.022(8) 0.011(7) 0.017(8) C23 0.037(13) 0.22(4) 0.08(2) 0.05(2) 0.020(15) 0.02(2) C24 0.070(18) 0.09(2) 0.069(17) 0.004(15) -0.008(14) 0.007(15) C25 0.073(18) 0.090(19) 0.055(14) -0.032(13) 0.023(13) -0.005(16) C26 0.048(15) 0.070(16) 0.08(2) -0.038(14) 0.008(13) 0.030(13) C31 0.10(2) 0.036(11) 0.035(11) 0.014(9) 0.015(12) -0.002(13) C32 0.040(12) 0.112(19) 0.029(12) -0.012(12) 0.010(9) -0.042(14) C33 0.062(17) 0.16(3) 0.07(2) 0.005(19) -0.005(15) -0.070(19) C34 0.043(12) 0.13(2) 0.034(14) 0.024(13) -0.011(10) -0.048(15) C35 0.051(15) 0.10(2) 0.053(16) -0.020(14) -0.014(12) 0.011(15) C36 0.069(15) 0.061(14) 0.056(14) -0.011(10) -0.008(12) -0.049(12) Au22 0.0559(6) 0.0538(5) 0.0385(5) 0.0028(5) -0.0136(5) 0.0072(4) Te21 0.0619(10) 0.0654(10) 0.0524(9) -0.0140(8) -0.0074(8) 0.0061(9) B21 0.0619(10) 0.0654(10) 0.0524(9) -0.0140(8) -0.0074(8) 0.0061(9) P2 0.039(3) 0.040(3) 0.036(3) 0.001(2) -0.005(2) 0.010(2) C41 0.083(17) 0.024(11) 0.051(13) -0.012(9) -0.011(12) -0.004(12) C42 0.036(13) 0.092(19) 0.048(14) -0.003(13) -0.012(10) 0.015(14) C43 0.11(2) 0.058(16) 0.054(16) -0.029(14) -0.010(16) -0.031(18) C44 0.097(12) 0.083(12) 0.070(11) -0.018(9) 0.009(9) 0.006(9) C45 0.078(18) 0.084(17) 0.029(13) -0.008(13) -0.005(12) 0.045(16) C46 0.054(13) 0.026(10) 0.031(10) 0.004(8) 0.011(9) 0.013(9) C51 0.025(9) 0.025(9) 0.043(13) -0.001(8) -0.011(8) 0.012(8) C52 0.059(8) 0.072(8) 0.053(8) -0.001(7) 0.015(7) -0.019(7) C53 0.057(8) 0.074(8) 0.058(8) -0.005(7) 0.010(7) -0.016(7) C54 0.036(13) 0.10(2) 0.11(2) 0.041(17) -0.010(14) -0.026(13) C55 0.043(13) 0.104(19) 0.055(14) -0.015(13) -0.012(12) -0.040(14) C56 0.051(13) 0.086(16) 0.015(8) -0.016(10) -0.017(8) 0.017(12) C61 0.028(8) 0.042(8) 0.039(8) -0.002(7) -0.016(6) -0.001(7) C62 0.18(4) 0.065(18) 0.07(2) -0.005(16) -0.02(2) 0.02(2) C63 0.12(3) 0.10(2) 0.08(2) 0.022(19) 0.03(2) 0.04(2) C64 0.10(2) 0.13(3) 0.07(2) 0.004(18) 0.042(18) 0.04(2) C65 0.053(14) 0.098(18) 0.039(13) -0.015(12) 0.019(11) 0.012(14) C66 0.071(14) 0.053(12) 0.035(10) 0.017(9) 0.006(10) -0.020(12) N1 0.017(7) 0.054(10) 0.034(10) -0.002(8) 0.008(7) -0.005(7) C71 0.042(12) 0.10(2) 0.071(17) -0.007(15) 0.020(12) 0.019(14) C72 0.091(19) 0.073(17) 0.092(19) 0.012(15) -0.002(16) -0.018(16) C73 0.049(13) 0.038(12) 0.085(18) 0.006(12) 0.008(12) -0.013(11) C74 0.10(2) 0.08(2) 0.13(2) 0.000(19) -0.04(2) -0.015(17) C75 0.09(2) 0.079(19) 0.09(2) 0.029(16) 0.040(18) -0.002(17) C76 0.11(3) 0.16(3) 0.061(19) -0.010(18) -0.052(19) -0.01(2) C77 0.042(16) 0.09(2) 0.09(2) 0.027(16) -0.007(13) 0.007(12) C78 0.10(2) 0.10(2) 0.046(18) -0.008(13) -0.021(17) 0.029(17) N2 0.055(12) 0.046(10) 0.055(14) -0.027(9) 0.006(10) -0.003(9) C81 0.082(18) 0.107(18) 0.013(10) -0.013(10) -0.005(10) 0.019(15) C82 0.057(16) 0.14(2) 0.07(2) -0.064(17) 0.018(15) -0.014(17) C83 0.042(14) 0.12(2) 0.076(19) -0.036(18) -0.025(13) 0.029(16) C84 0.18(3) 0.044(14) 0.10(2) -0.030(14) -0.08(2) 0.074(19) C85 0.047(9) 0.061(9) 0.064(9) 0.010(8) 0.017(7) -0.020(8) C86 0.14(3) 0.061(17) 0.11(2) 0.018(16) -0.03(2) -0.056(18) C87 0.019(9) 0.059(15) 0.052(14) -0.005(10) -0.003(8) 0.002(9) C88 0.11(2) 0.13(3) 0.06(3) 0.001(16) -0.02(2) 0.000(19) _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 Au2 P1 2.237(6) . ? Au2 Te7 2.294(13) . ? Au2 B8 2.33(3) . ? Au2 B6 2.53(3) . ? Au2 Te3 2.576(18) . ? Au2 Te1 2.839(3) . ? Te3 Te7 3.02(2) . ? B4 B9 1.71(4) . ? B4 B10 1.78(3) . ? B4 B5 1.98(4) . ? B4 H4 1.10 . ? B5 B11 1.65(3) . ? B5 B10 1.75(4) . ? B5 B6 1.84(4) . ? B5 H5 1.10 . ? B6 B11 1.75(4) . ? B6 H6 1.10 . ? B8 B12 1.74(3) . ? B8 B9 1.76(3) . ? B8 H8 1.10 . ? B9 B12 1.77(3) . ? B9 B10 1.81(3) . ? B9 H9 1.10 . ? B10 B11 1.72(3) . ? B10 B12 1.79(3) . ? B10 H10 1.10 . ? B11 B12 1.83(3) . ? B11 H11 1.10 . ? B12 H12 1.10 . ? P1 C21 1.78(2) . ? P1 C31 1.85(2) . ? P1 C11 1.87(2) . ? C11 C16 1.34(3) . ? C11 C12 1.41(3) . ? C12 C13 1.43(3) . ? C12 H12A 0.93 . ? C13 C14 1.36(4) . ? C13 H13 0.93 . ? C14 C15 1.37(3) . ? C14 H14 0.93 . ? C15 C16 1.42(3) . ? C15 H15 0.93 . ? C16 H16 0.93 . ? C21 C26 1.28(3) . ? C21 C22 1.39(3) . ? C22 C23 1.28(3) . ? C22 H22 0.93 . ? C23 C24 1.40(4) . ? C23 H23 0.93 . ? C24 C25 1.34(3) . ? C24 H24 0.93 . ? C25 C26 1.41(3) . ? C25 H25 0.93 . ? C26 H26 0.93 . ? C31 C32 1.30(3) . ? C31 C36 1.40(3) . ? C32 C33 1.40(3) . ? C32 H32 0.93 . ? C33 C34 1.36(4) . ? C33 H33 0.93 . ? C34 C35 1.36(3) . ? C34 H34 0.93 . ? C35 C36 1.39(3) . ? C35 H35 0.93 . ? C36 H36 0.93 . ? Au22 P2 2.263(6) . ? Au22 B28 2.38(3) . ? Au22 B26 2.57(3) . ? Au22 B23 2.59(3) . ? Au22 Te27 2.825(17) . ? Au22 Te21 2.853(3) . ? Te27 B210 2.36(3) . ? Te27 B29 2.68(3) . ? B23 B29 1.83(4) . ? B23 B28 1.91(4) . ? B23 B24 1.94(3) . ? B23 H23A 1.10 . ? B24 B29 1.71(3) . ? B24 B210 1.72(3) . ? B24 B25 1.96(4) . ? B24 H24A 1.10 . ? B25 B210 1.75(4) . ? B25 B211 1.83(3) . ? B25 B26 1.96(4) . ? B25 H25A 1.10 . ? B26 B211 1.76(4) . ? B26 H26A 1.10 . ? B28 B212 1.78(4) . ? B28 B29 1.81(4) . ? B28 H28 1.10 . ? B29 B210 1.73(3) . ? B29 B212 1.84(3) . ? B29 H29 1.10 . ? B210 B212 1.82(4) . ? B210 B211 1.83(4) . ? B210 H210 1.10 . ? B211 B212 1.72(4) . ? B211 H211 1.10 . ? B212 H212 1.10 . ? P2 C41 1.823(19) . ? P2 C51 1.84(2) . ? P2 C61 1.85(2) . ? C41 C42 1.36(3) . ? C41 C46 1.38(3) . ? C42 C43 1.35(4) . ? C42 H42 0.93 . ? C43 C44 1.32(4) . ? C43 H43 0.93 . ? C44 C45 1.43(4) . ? C44 H44 0.93 . ? C45 C46 1.38(3) . ? C45 H45 0.93 . ? C46 H46 0.93 . ? C51 C52 1.39(3) . ? C51 C56 1.45(3) . ? C52 C53 1.42(3) . ? C52 H52 0.93 . ? C53 C54 1.33(4) . ? C53 H53 0.93 . ? C54 C55 1.36(3) . ? C54 H54 0.93 . ? C55 C56 1.39(3) . ? C55 H55 0.93 . ? C56 H56 0.93 . ? C61 C62 1.31(4) . ? C61 C66 1.40(2) . ? C62 C63 1.45(4) . ? C62 H62 0.93 . ? C63 C64 1.38(4) . ? C63 H63 0.93 . ? C64 C65 1.34(3) . ? C64 H64 0.93 . ? C65 C66 1.41(2) . ? C65 H65 0.93 . ? C66 H66 0.93 . ? N1 C77 1.462(19) . ? N1 C75 1.48(2) . ? N1 C73 1.494(18) . ? N1 C71 1.514(19) . ? C71 C72 1.52(2) . ? C71 H71A 0.97 . ? C71 H71B 0.97 . ? C72 H72A 0.96 . ? C72 H72B 0.96 . ? C72 H72C 0.96 . ? C73 C74 1.54(2) . ? C73 H73A 0.97 . ? C73 H73B 0.97 . ? C74 H74A 0.96 . ? C74 H74B 0.96 . ? C74 H74C 0.96 . ? C75 C76 1.50(2) . ? C75 H75A 0.97 . ? C75 H75B 0.97 . ? C76 H76A 0.96 . ? C76 H76B 0.96 . ? C76 H76C 0.96 . ? C77 C78 1.53(2) . ? C77 H77A 0.97 . ? C77 H77B 0.97 . ? C78 H78A 0.96 . ? C78 H78B 0.96 . ? C78 H78C 0.96 . ? N2 C83 1.48(2) . ? N2 C87 1.51(2) . ? N2 C81 1.535(19) . ? N2 C85 1.557(19) . ? C81 C82 1.52(2) . ? C81 H81A 0.97 . ? C81 H81B 0.97 . ? C82 H82A 0.96 . ? C82 H82B 0.96 . ? C82 H82C 0.96 . ? C83 C84 1.50(2) . ? C83 H83A 0.97 . ? C83 H83B 0.97 . ? C84 H84A 0.96 . ? C84 H84B 0.96 . ? C84 H84C 0.96 . ? C85 C86 1.52(2) . ? C85 H85A 0.97 . ? C85 H85B 0.97 . ? C86 H86A 0.96 . ? C86 H86B 0.96 . ? C86 H86C 0.96 . ? C87 C88 1.53(2) . ? C87 H87A 0.97 . ? C87 H87B 0.97 . ? C88 H88A 0.96 . ? C88 H88B 0.96 . ? C88 H88C 0.96 . ? 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 P1 Au2 Te7 153.0(4) . . ? P1 Au2 B8 140.1(7) . . ? Te7 Au2 B8 47.4(7) . . ? P1 Au2 B6 140.5(7) . . ? Te7 Au2 B6 43.8(7) . . ? B8 Au2 B6 79.3(9) . . ? P1 Au2 Te3 128.1(4) . . ? Te7 Au2 Te3 76.3(5) . . ? B8 Au2 Te3 43.3(7) . . ? B6 Au2 Te3 79.5(8) . . ? P1 Au2 Te1 119.93(14) . . ? Te7 Au2 Te1 83.4(3) . . ? B8 Au2 Te1 84.8(7) . . ? B6 Au2 Te1 51.2(6) . . ? Te3 Au2 Te1 51.0(4) . . ? Au2 Te3 Te7 47.6(4) . . ? Au2 Te7 Te3 56.1(4) . . ? B9 B4 B10 62.3(15) . . ? B9 B4 B5 104.6(18) . . ? B10 B4 B5 55.3(13) . . ? B9 B4 H4 121.6 . . ? B10 B4 H4 121.6 . . ? B5 B4 H4 124.9 . . ? B11 B5 B10 60.6(15) . . ? B11 B5 B6 60.0(15) . . ? B10 B5 B6 109.7(18) . . ? B11 B5 B4 106(2) . . ? B10 B5 B4 56.5(14) . . ? B6 B5 B4 111.9(19) . . ? B11 B5 H5 120.5 . . ? B10 B5 H5 121.7 . . ? B6 B5 H5 118.8 . . ? B4 B5 H5 122.9 . . ? B11 B6 B5 54.6(14) . . ? B11 B6 Au2 115.3(16) . . ? B5 B6 Au2 121.1(17) . . ? B11 B6 H6 122.5 . . ? B5 B6 H6 122.3 . . ? Au2 B6 H6 110.6 . . ? B12 B8 B9 61.0(14) . . ? B12 B8 Au2 118.7(16) . . ? B9 B8 Au2 126.0(16) . . ? B12 B8 H8 121.6 . . ? B9 B8 H8 120.4 . . ? Au2 B8 H8 104.8 . . ? B4 B9 B8 116.3(19) . . ? B4 B9 B12 111.4(19) . . ? B8 B9 B12 59.0(14) . . ? B4 B9 B10 60.7(15) . . ? B8 B9 B10 109.3(18) . . ? B12 B9 B10 60.0(14) . . ? B4 B9 H9 116.1 . . ? B8 B9 H9 119.8 . . ? B12 B9 H9 122.0 . . ? B10 B9 H9 120.8 . . ? B11 B10 B5 56.7(14) . . ? B11 B10 B4 112.8(19) . . ? B5 B10 B4 68.2(15) . . ? B11 B10 B12 62.6(14) . . ? B5 B10 B12 108.1(19) . . ? B4 B10 B12 107.5(18) . . ? B11 B10 B9 109.5(19) . . ? B5 B10 B9 110.6(19) . . ? B4 B10 B9 57.0(14) . . ? B12 B10 B9 59.1(14) . . ? B11 B10 H10 120.3 . . ? B5 B10 H10 119.5 . . ? B4 B10 H10 118.8 . . ? B12 B10 H10 122.3 . . ? B9 B10 H10 122.5 . . ? B5 B11 B10 62.7(16) . . ? B5 B11 B6 65.5(16) . . ? B10 B11 B6 116(2) . . ? B5 B11 B12 111(2) . . ? B10 B11 B12 60.6(14) . . ? B6 B11 B12 110(2) . . ? B5 B11 H11 117.1 . . ? B10 B11 H11 119.6 . . ? B6 B11 H11 116.4 . . ? B12 B11 H11 122.8 . . ? B8 B12 B9 60.0(14) . . ? B8 B12 B10 110.8(18) . . ? B9 B12 B10 60.9(14) . . ? B8 B12 B11 112.5(19) . . ? B9 B12 B11 106.3(17) . . ? B10 B12 B11 56.8(13) . . ? B8 B12 H12 117.1 . . ? B9 B12 H12 121.9 . . ? B10 B12 H12 122.9 . . ? B11 B12 H12 122.8 . . ? C21 P1 C31 106.6(11) . . ? C21 P1 C11 103.6(9) . . ? C31 P1 C11 103.3(9) . . ? C21 P1 Au2 115.8(8) . . ? C31 P1 Au2 114.0(9) . . ? C11 P1 Au2 112.2(6) . . ? C16 C11 C12 123(2) . . ? C16 C11 P1 121.1(17) . . ? C12 C11 P1 116.0(16) . . ? C11 C12 C13 115(2) . . ? C11 C12 H12A 122.4 . . ? C13 C12 H12A 122.4 . . ? C14 C13 C12 121(3) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 122(2) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C14 C15 C16 117(2) . . ? C14 C15 H15 121.4 . . ? C16 C15 H15 121.4 . . ? C11 C16 C15 121(2) . . ? C11 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C26 C21 C22 114(2) . . ? C26 C21 P1 126.3(19) . . ? C22 C21 P1 119.7(19) . . ? C23 C22 C21 125(3) . . ? C23 C22 H22 117.5 . . ? C21 C22 H22 117.5 . . ? C22 C23 C24 119(3) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 120(3) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 116(2) . . ? C24 C25 H25 122.2 . . ? C26 C25 H25 122.2 . . ? C21 C26 C25 127(2) . . ? C21 C26 H26 116.7 . . ? C25 C26 H26 116.7 . . ? C32 C31 C36 121(2) . . ? C32 C31 P1 118.1(18) . . ? C36 C31 P1 120.3(18) . . ? C31 C32 C33 118(2) . . ? C31 C32 H32 121.1 . . ? C33 C32 H32 121.1 . . ? C34 C33 C32 122(2) . . ? C34 C33 H33 118.9 . . ? C32 C33 H33 118.9 . . ? C33 C34 C35 119(3) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 119(2) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C35 C36 C31 120(2) . . ? C35 C36 H36 120.2 . . ? C31 C36 H36 120.2 . . ? P2 Au22 B28 138.3(7) . . ? P2 Au22 B26 142.0(7) . . ? B28 Au22 B26 79.6(9) . . ? P2 Au22 B23 125.9(6) . . ? B28 Au22 B23 45.0(8) . . ? B26 Au22 B23 80.0(9) . . ? P2 Au22 Te27 160.2(4) . . ? B28 Au22 Te27 46.5(7) . . ? B26 Au22 Te27 39.3(7) . . ? B23 Au22 Te27 72.1(7) . . ? P2 Au22 Te21 119.74(14) . . ? B28 Au22 Te21 86.0(7) . . ? B26 Au22 Te21 51.4(6) . . ? B23 Au22 Te21 51.0(6) . . ? Te27 Au22 Te21 77.0(3) . . ? B210 Te27 Au22 111.1(8) . . ? B29 Te27 Au22 84.2(7) . . ? B29 B23 B28 57.9(13) . . ? B29 B23 B24 54.0(13) . . ? B28 B23 B24 102.0(16) . . ? B29 B23 Au22 112.2(15) . . ? B28 B23 Au22 61.7(10) . . ? B24 B23 Au22 117.9(15) . . ? B29 B23 H23A 124.5 . . ? B28 B23 H23A 124.2 . . ? B24 B23 H23A 123.0 . . ? Au22 B23 H23A 112.9 . . ? B29 B24 B210 60.4(14) . . ? B29 B24 B23 59.5(14) . . ? B210 B24 B23 109.3(18) . . ? B29 B24 B25 106.6(18) . . ? B210 B24 B25 56.2(13) . . ? B23 B24 B25 113.2(18) . . ? B29 B24 H24A 121.3 . . ? B210 B24 H24A 122.3 . . ? B23 B24 H24A 118.8 . . ? B25 B24 H24A 121.6 . . ? B210 B25 B211 61.4(14) . . ? B210 B25 B26 105.3(17) . . ? B211 B25 B26 55.4(13) . . ? B210 B25 B24 55.0(14) . . ? B211 B25 B24 103.8(18) . . ? B26 B25 B24 107.4(19) . . ? B210 B25 H25A 123.0 . . ? B211 B25 H25A 123.1 . . ? B26 B25 H25A 122.7 . . ? B24 B25 H25A 124.4 . . ? B211 B26 B25 58.5(14) . . ? B211 B26 Au22 113.3(16) . . ? B25 B26 Au22 121.2(16) . . ? B211 B26 H26A 127.4 . . ? B25 B26 H26A 126.4 . . ? Au22 B26 H26A 104.7 . . ? B212 B28 B29 61.8(14) . . ? B212 B28 B23 109.3(17) . . ? B29 B28 B23 58.6(13) . . ? B212 B28 Au22 114.8(15) . . ? B29 B28 Au22 122.9(16) . . ? B23 B28 Au22 73.3(11) . . ? B212 B28 H28 126.4 . . ? B29 B28 H28 126.1 . . ? B23 B28 H28 118.1 . . ? Au22 B28 H28 102.0 . . ? B24 B29 B210 60.1(15) . . ? B24 B29 B28 116.5(19) . . ? B210 B29 B28 111.1(18) . . ? B24 B29 B23 66.5(14) . . ? B210 B29 B23 114.6(19) . . ? B28 B29 B23 63.5(15) . . ? B24 B29 B212 110.2(19) . . ? B210 B29 B212 61.2(14) . . ? B28 B29 B212 58.3(14) . . ? B23 B29 B212 110.4(18) . . ? B24 B29 Te27 91.7(15) . . ? B210 B29 Te27 60.0(12) . . ? B28 B29 Te27 51.1(11) . . ? B23 B29 Te27 88.1(14) . . ? B24 B29 H29 117.2 . . ? B210 B29 H29 119.8 . . ? B28 B29 H29 118.7 . . ? B23 B29 H29 116.5 . . ? B212 B29 H29 122.8 . . ? Te27 B29 H29 147.3 . . ? B24 B210 B29 59.5(14) . . ? B24 B210 B25 68.9(15) . . ? B29 B210 B25 116(2) . . ? B24 B210 B212 110.8(18) . . ? B29 B210 B212 62.5(14) . . ? B25 B210 B212 109.5(19) . . ? B24 B210 B211 114.4(19) . . ? B29 B210 B211 109.0(19) . . ? B25 B210 B211 61.5(15) . . ? B212 B210 B211 56.2(14) . . ? B24 B210 Te27 103.4(15) . . ? B29 B210 Te27 80.5(14) . . ? B25 B210 Te27 77.4(14) . . ? B24 B210 H210 116.7 . . ? B29 B210 H210 119.4 . . ? B25 B210 H210 115.7 . . ? B212 B210 H210 122.9 . . ? B211 B210 H210 122.0 . . ? Te27 B210 H210 139.9 . . ? B212 B211 B26 112(2) . . ? B212 B211 B210 61.7(14) . . ? B26 B211 B210 110.6(19) . . ? B212 B211 B25 110.6(19) . . ? B26 B211 B25 66.2(15) . . ? B210 B211 B25 57.1(14) . . ? B212 B211 H211 124.9 . . ? B26 B211 H211 112.5 . . ? B210 B211 H211 126.0 . . ? B25 B211 H211 116.1 . . ? B211 B212 B28 116.6(19) . . ? B211 B212 B210 62.1(15) . . ? B28 B212 B210 108.4(18) . . ? B211 B212 B29 108.7(18) . . ? B28 B212 B29 59.9(14) . . ? B210 B212 B29 56.3(13) . . ? B211 B212 H212 124.8 . . ? B28 B212 H212 109.2 . . ? B210 B212 H212 128.7 . . ? B29 B212 H212 120.3 . . ? C41 P2 C51 105.0(10) . . ? C41 P2 C61 103.1(10) . . ? C51 P2 C61 105.4(9) . . ? C41 P2 Au22 113.5(7) . . ? C51 P2 Au22 115.0(7) . . ? C61 P2 Au22 113.7(6) . . ? C42 C41 C46 115.0(19) . . ? C42 C41 P2 120.2(19) . . ? C46 C41 P2 124.6(16) . . ? C43 C42 C41 127(2) . . ? C43 C42 H42 116.7 . . ? C41 C42 H42 116.7 . . ? C44 C43 C42 117(3) . . ? C44 C43 H43 121.3 . . ? C42 C43 H43 121.3 . . ? C43 C44 C45 121(3) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 118(2) . . ? C46 C45 H45 120.8 . . ? C44 C45 H45 120.8 . . ? C45 C46 C41 122(2) . . ? C45 C46 H46 119.2 . . ? C41 C46 H46 119.2 . . ? C52 C51 C56 120.9(19) . . ? C52 C51 P2 117.8(17) . . ? C56 C51 P2 120.8(17) . . ? C51 C52 C53 121(2) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 116(2) . . ? C54 C53 H53 122.0 . . ? C52 C53 H53 122.0 . . ? C53 C54 C55 126(2) . . ? C53 C54 H54 117.1 . . ? C55 C54 H54 117.1 . . ? C54 C55 C56 121(2) . . ? C54 C55 H55 119.3 . . ? C56 C55 H55 119.3 . . ? C55 C56 C51 115(2) . . ? C55 C56 H56 122.6 . . ? C51 C56 H56 122.6 . . ? C62 C61 C66 121(2) . . ? C62 C61 P2 120.2(19) . . ? C66 C61 P2 119.1(15) . . ? C61 C62 C63 123(3) . . ? C61 C62 H62 118.3 . . ? C63 C62 H62 118.3 . . ? C64 C63 C62 114(3) . . ? C64 C63 H63 123.2 . . ? C62 C63 H63 123.2 . . ? C65 C64 C63 125(3) . . ? C65 C64 H64 117.6 . . ? C63 C64 H64 117.6 . . ? C64 C65 C66 119(2) . . ? C64 C65 H65 120.3 . . ? C66 C65 H65 120.3 . . ? C61 C66 C65 118(2) . . ? C61 C66 H66 120.9 . . ? C65 C66 H66 120.9 . . ? C77 N1 C75 106.8(19) . . ? C77 N1 C73 114.6(16) . . ? C75 N1 C73 108.4(17) . . ? C77 N1 C71 111.5(16) . . ? C75 N1 C71 110.7(18) . . ? C73 N1 C71 104.8(14) . . ? N1 C71 C72 117.2(16) . . ? N1 C71 H71A 108.0 . . ? C72 C71 H71A 108.0 . . ? N1 C71 H71B 108.0 . . ? C72 C71 H71B 108.0 . . ? H71A C71 H71B 107.2 . . ? C71 C72 H72A 109.5 . . ? C71 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C71 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N1 C73 C74 115.2(18) . . ? N1 C73 H73A 108.5 . . ? C74 C73 H73A 108.5 . . ? N1 C73 H73B 108.5 . . ? C74 C73 H73B 108.5 . . ? H73A C73 H73B 107.5 . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N1 C75 C76 116(2) . . ? N1 C75 H75A 108.4 . . ? C76 C75 H75A 108.4 . . ? N1 C75 H75B 108.4 . . ? C76 C75 H75B 108.4 . . ? H75A C75 H75B 107.5 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N1 C77 C78 120(2) . . ? N1 C77 H77A 107.3 . . ? C78 C77 H77A 107.3 . . ? N1 C77 H77B 107.3 . . ? C78 C77 H77B 107.3 . . ? H77A C77 H77B 106.9 . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C83 N2 C87 109.2(15) . . ? C83 N2 C81 109.9(18) . . ? C87 N2 C81 108.2(17) . . ? C83 N2 C85 106.0(17) . . ? C87 N2 C85 111.6(16) . . ? C81 N2 C85 111.9(16) . . ? C82 C81 N2 116(2) . . ? C82 C81 H81A 108.3 . . ? N2 C81 H81A 108.3 . . ? C82 C81 H81B 108.3 . . ? N2 C81 H81B 108.3 . . ? H81A C81 H81B 107.4 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N2 C83 C84 113.1(19) . . ? N2 C83 H83A 109.0 . . ? C84 C83 H83A 109.0 . . ? N2 C83 H83B 109.0 . . ? C84 C83 H83B 109.0 . . ? H83A C83 H83B 107.8 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C86 C85 N2 110.9(16) . . ? C86 C85 H85A 109.5 . . ? N2 C85 H85A 109.5 . . ? C86 C85 H85B 109.5 . . ? N2 C85 H85B 109.5 . . ? H85A C85 H85B 108.0 . . ? C85 C86 H86A 109.5 . . ? C85 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C85 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N2 C87 C88 113(2) . . ? N2 C87 H87A 109.0 . . ? C88 C87 H87A 109.0 . . ? N2 C87 H87B 109.0 . . ? C88 C87 H87B 109.0 . . ? H87A C87 H87B 107.8 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? _refine_diff_density_max 1.573 _refine_diff_density_min -0.982 _refine_diff_density_rms 0.158 #### end of CIF for compound 7 #### #========================================================================= # END of CIF #=========================================================================