# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_npm028 _database_code_depnum_ccdc_archive 'CCDC 901602' #TrackingRef 'web_deposit_cif_file_4_MilesW.Johnson_1352328108.IPrAuNiPr2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common IPrAuNiPr2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H50 Au N3' _chemical_formula_weight 685.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.5384(10) _cell_length_b 13.4689(11) _cell_length_c 19.1735(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.3730(10) _cell_angle_gamma 90.00 _cell_volume 3232.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 4.575 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2619 _exptl_absorpt_correction_T_max 0.6576 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94771 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0127 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.10 _reflns_number_total 7128 _reflns_number_gt 6578 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+10.1754P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7128 _refine_ls_number_parameters 346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0329 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0937 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.756508(11) 0.587748(10) 0.244413(8) 0.02022(7) Uani 1 1 d . . . N1 N 0.6780(3) 0.5425(2) 0.09691(18) 0.0219(7) Uani 1 1 d . . . N2 N 0.7940(3) 0.6587(2) 0.09843(18) 0.0225(7) Uani 1 1 d . . . N3 N 0.7622(3) 0.5791(3) 0.3470(2) 0.0270(8) Uani 1 1 d . . . C1 C 0.7452(3) 0.5954(3) 0.1424(2) 0.0229(8) Uani 1 1 d . . . C2 C 0.7588(4) 0.6455(3) 0.0291(2) 0.0274(9) Uani 1 1 d . . . H2 H 0.7818 0.6810 -0.0100 0.033 Uiso 1 1 calc R . . C3 C 0.6857(4) 0.5727(3) 0.0283(2) 0.0261(9) Uani 1 1 d . . . H3 H 0.6467 0.5468 -0.0116 0.031 Uiso 1 1 calc R . . C4 C 0.6060(3) 0.4652(3) 0.1173(2) 0.0230(8) Uani 1 1 d . . . C5 C 0.6377(4) 0.3659(3) 0.1113(2) 0.0277(9) Uani 1 1 d . . . C6 C 0.5636(4) 0.2933(3) 0.1268(3) 0.0339(10) Uani 1 1 d . . . H6 H 0.5824 0.2253 0.1232 0.041 Uiso 1 1 calc R . . C7 C 0.4633(4) 0.3185(3) 0.1473(3) 0.0331(10) Uani 1 1 d . . . H7 H 0.4134 0.2679 0.1567 0.040 Uiso 1 1 calc R . . C8 C 0.4352(4) 0.4176(3) 0.1542(3) 0.0293(10) Uani 1 1 d . . . H8 H 0.3663 0.4339 0.1689 0.035 Uiso 1 1 calc R . . C9 C 0.5061(3) 0.4936(3) 0.1401(2) 0.0255(8) Uani 1 1 d . . . C10 C 0.7509(4) 0.3386(3) 0.0934(3) 0.0359(11) Uani 1 1 d . . . H10 H 0.7782 0.3931 0.0638 0.043 Uiso 1 1 calc R . . C11 C 0.7571(5) 0.2415(4) 0.0521(3) 0.0432(12) Uani 1 1 d . . . H11A H 0.7372 0.1858 0.0816 0.065 Uiso 1 1 calc R . . H11B H 0.8301 0.2319 0.0379 0.065 Uiso 1 1 calc R . . H11C H 0.7078 0.2448 0.0106 0.065 Uiso 1 1 calc R . . C12 C 0.8235(4) 0.3327(5) 0.1598(4) 0.0537(15) Uani 1 1 d . . . H12A H 0.8206 0.3957 0.1852 0.080 Uiso 1 1 calc R . . H12B H 0.8970 0.3199 0.1476 0.080 Uiso 1 1 calc R . . H12C H 0.7995 0.2788 0.1894 0.080 Uiso 1 1 calc R . . C13 C 0.4771(4) 0.6021(3) 0.1495(2) 0.0283(9) Uani 1 1 d . . . H13 H 0.5457 0.6395 0.1576 0.034 Uiso 1 1 calc R . . C14 C 0.4210(6) 0.6443(4) 0.0842(3) 0.0597(18) Uani 1 1 d . . . H14A H 0.3504 0.6135 0.0768 0.090 Uiso 1 1 calc R . . H14B H 0.4634 0.6306 0.0440 0.090 Uiso 1 1 calc R . . H14C H 0.4127 0.7162 0.0895 0.090 Uiso 1 1 calc R . . C15 C 0.4120(6) 0.6205(5) 0.2123(3) 0.0544(15) Uani 1 1 d . . . H15A H 0.3412 0.5902 0.2043 0.082 Uiso 1 1 calc R . . H15B H 0.4041 0.6921 0.2193 0.082 Uiso 1 1 calc R . . H15C H 0.4484 0.5909 0.2539 0.082 Uiso 1 1 calc R . . C16 C 0.8760(3) 0.7287(3) 0.1217(2) 0.0261(8) Uani 1 1 d . . . C17 C 0.9809(4) 0.6943(3) 0.1327(3) 0.0306(9) Uani 1 1 d . . . C18 C 1.0585(4) 0.7641(4) 0.1533(3) 0.0398(11) Uani 1 1 d . . . H18 H 1.1307 0.7434 0.1613 0.048 Uiso 1 1 calc R . . C19 C 1.0324(4) 0.8631(4) 0.1620(3) 0.0424(12) Uani 1 1 d . . . H19 H 1.0865 0.9097 0.1759 0.051 Uiso 1 1 calc R . . C20 C 0.9277(4) 0.8940(4) 0.1507(3) 0.0366(11) Uani 1 1 d . . . H20 H 0.9108 0.9620 0.1571 0.044 Uiso 1 1 calc R . . C21 C 0.8469(3) 0.8284(3) 0.1301(2) 0.0273(9) Uani 1 1 d . . . C22 C 1.0116(4) 0.5862(3) 0.1228(3) 0.0356(11) Uani 1 1 d . . . H22 H 0.9450 0.5489 0.1084 0.043 Uiso 1 1 calc R . . C23 C 1.0877(5) 0.5771(4) 0.0633(4) 0.0606(19) Uani 1 1 d . . . H23A H 1.1535 0.6141 0.0755 0.091 Uiso 1 1 calc R . . H23B H 1.0533 0.6043 0.0203 0.091 Uiso 1 1 calc R . . H23C H 1.1050 0.5070 0.0562 0.091 Uiso 1 1 calc R . . C24 C 1.0575(5) 0.5409(4) 0.1906(3) 0.0507(14) Uani 1 1 d . . . H24A H 1.1240 0.5752 0.2055 0.076 Uiso 1 1 calc R . . H24B H 1.0723 0.4704 0.1833 0.076 Uiso 1 1 calc R . . H24C H 1.0059 0.5480 0.2267 0.076 Uiso 1 1 calc R . . C25 C 0.7312(4) 0.8631(3) 0.1192(2) 0.0283(9) Uani 1 1 d . . . H25 H 0.6940 0.8190 0.0836 0.034 Uiso 1 1 calc R . . C26 C 0.7224(4) 0.9698(3) 0.0931(3) 0.0379(11) Uani 1 1 d . . . H26A H 0.7494 1.0151 0.1301 0.057 Uiso 1 1 calc R . . H26B H 0.6474 0.9854 0.0803 0.057 Uiso 1 1 calc R . . H26C H 0.7647 0.9777 0.0521 0.057 Uiso 1 1 calc R . . C27 C 0.6749(4) 0.8534(4) 0.1875(3) 0.0394(11) Uani 1 1 d . . . H27A H 0.6745 0.7835 0.2019 0.059 Uiso 1 1 calc R . . H27B H 0.6012 0.8772 0.1805 0.059 Uiso 1 1 calc R . . H27C H 0.7128 0.8931 0.2239 0.059 Uiso 1 1 calc R . . C28 C 0.6994(3) 0.5062(3) 0.3836(2) 0.0226(8) Uani 1 1 d . . . H28 H 0.7458 0.4790 0.4234 0.027 Uiso 1 1 calc R . . C29 C 0.6638(4) 0.4204(3) 0.3372(3) 0.0346(10) Uani 1 1 d . . . H29A H 0.6203 0.4455 0.2969 0.052 Uiso 1 1 calc R . . H29B H 0.6215 0.3740 0.3636 0.052 Uiso 1 1 calc R . . H29C H 0.7267 0.3861 0.3210 0.052 Uiso 1 1 calc R . . C30 C 0.5993(4) 0.5533(4) 0.4144(3) 0.0365(10) Uani 1 1 d . . . H30A H 0.6209 0.6112 0.4429 0.055 Uiso 1 1 calc R . . H30B H 0.5649 0.5044 0.4435 0.055 Uiso 1 1 calc R . . H30C H 0.5489 0.5742 0.3762 0.055 Uiso 1 1 calc R . . C31 C 0.8242(4) 0.6465(3) 0.3949(2) 0.0291(9) Uani 1 1 d . . . H31 H 0.7773 0.6646 0.4333 0.035 Uiso 1 1 calc R . . C32 C 0.8520(4) 0.7423(4) 0.3580(3) 0.0380(11) Uani 1 1 d . . . H32A H 0.8972 0.7272 0.3194 0.057 Uiso 1 1 calc R . . H32B H 0.8905 0.7868 0.3912 0.057 Uiso 1 1 calc R . . H32C H 0.7862 0.7747 0.3396 0.057 Uiso 1 1 calc R . . C33 C 0.9256(4) 0.6003(4) 0.4288(4) 0.0487(14) Uani 1 1 d . . . H33A H 0.9085 0.5357 0.4489 0.073 Uiso 1 1 calc R . . H33B H 0.9552 0.6442 0.4659 0.073 Uiso 1 1 calc R . . H33C H 0.9782 0.5913 0.3935 0.073 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01792(9) 0.01755(10) 0.02546(10) 0.00092(5) 0.00372(6) -0.00148(5) N1 0.0240(16) 0.0146(15) 0.0279(17) 0.0010(13) 0.0080(13) -0.0025(13) N2 0.0236(16) 0.0150(15) 0.0297(17) -0.0001(13) 0.0082(14) -0.0022(13) N3 0.0299(19) 0.0241(18) 0.0272(18) -0.0018(14) 0.0048(15) -0.0097(14) C1 0.0188(19) 0.0163(18) 0.035(2) -0.0005(15) 0.0125(17) -0.0013(14) C2 0.036(2) 0.0192(19) 0.028(2) 0.0037(16) 0.0140(17) -0.0012(17) C3 0.035(2) 0.0200(19) 0.024(2) -0.0008(15) 0.0064(17) -0.0011(16) C4 0.0237(19) 0.0151(18) 0.031(2) 0.0029(15) 0.0063(16) -0.0031(15) C5 0.031(2) 0.019(2) 0.035(2) 0.0033(16) 0.0090(18) -0.0008(17) C6 0.040(3) 0.019(2) 0.044(3) 0.0047(18) 0.011(2) -0.0054(18) C7 0.031(2) 0.026(2) 0.042(3) 0.0048(19) 0.0066(19) -0.0116(18) C8 0.022(2) 0.032(2) 0.035(2) 0.0000(17) 0.0043(18) -0.0065(16) C9 0.025(2) 0.023(2) 0.029(2) 0.0012(16) 0.0054(16) -0.0019(16) C10 0.033(2) 0.020(2) 0.056(3) 0.004(2) 0.015(2) 0.0025(18) C11 0.052(3) 0.025(2) 0.054(3) 0.001(2) 0.012(3) 0.010(2) C12 0.033(3) 0.050(3) 0.077(4) -0.016(3) -0.003(3) 0.007(2) C13 0.025(2) 0.024(2) 0.037(2) -0.0056(17) 0.0043(18) 0.0004(16) C14 0.097(5) 0.032(3) 0.048(3) -0.007(2) -0.009(3) 0.027(3) C15 0.073(4) 0.045(3) 0.048(3) -0.007(3) 0.023(3) 0.013(3) C16 0.0255(19) 0.0191(19) 0.035(2) -0.0009(16) 0.0121(17) -0.0049(16) C17 0.026(2) 0.022(2) 0.045(3) 0.0004(18) 0.0124(19) -0.0024(17) C18 0.024(2) 0.032(2) 0.063(3) -0.002(2) 0.007(2) -0.0023(19) C19 0.032(2) 0.030(2) 0.065(3) -0.008(2) 0.004(2) -0.011(2) C20 0.036(3) 0.020(2) 0.054(3) -0.006(2) 0.009(2) -0.0038(19) C21 0.029(2) 0.0188(19) 0.035(2) -0.0007(16) 0.0111(17) -0.0020(16) C22 0.025(2) 0.025(2) 0.058(3) -0.0014(19) 0.015(2) 0.0020(17) C23 0.054(4) 0.041(3) 0.091(5) -0.015(3) 0.045(4) 0.000(3) C24 0.042(3) 0.040(3) 0.069(4) 0.004(3) -0.005(3) 0.005(2) C25 0.030(2) 0.020(2) 0.035(2) -0.0027(17) 0.0048(18) 0.0008(16) C26 0.042(3) 0.026(2) 0.045(3) 0.006(2) 0.005(2) 0.003(2) C27 0.037(3) 0.035(3) 0.048(3) 0.007(2) 0.016(2) 0.009(2) C28 0.0211(18) 0.0232(19) 0.0232(19) 0.0096(15) -0.0003(15) -0.0052(15) C29 0.036(2) 0.026(2) 0.043(3) 0.0046(19) 0.009(2) -0.0069(18) C30 0.031(2) 0.038(3) 0.042(3) 0.002(2) 0.012(2) -0.003(2) C31 0.032(2) 0.025(2) 0.030(2) -0.0078(17) 0.0000(17) -0.0001(17) C32 0.037(2) 0.040(3) 0.038(2) -0.002(2) 0.003(2) -0.013(2) C33 0.034(3) 0.041(3) 0.070(4) -0.003(3) -0.009(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 1.955(5) . ? Au1 N3 1.968(4) . ? N1 C1 1.375(6) . ? N1 C3 1.385(5) . ? N1 C4 1.448(5) . ? N2 C1 1.369(5) . ? N2 C2 1.387(6) . ? N2 C16 1.446(5) . ? N3 C28 1.463(5) . ? N3 C31 1.479(5) . ? C2 C3 1.342(6) . ? C4 C5 1.401(6) . ? C4 C9 1.404(6) . ? C5 C6 1.393(6) . ? C5 C10 1.525(6) . ? C6 C7 1.381(7) . ? C7 C8 1.389(6) . ? C8 C9 1.392(6) . ? C9 C13 1.520(6) . ? C10 C12 1.523(8) . ? C10 C11 1.532(7) . ? C13 C14 1.510(7) . ? C13 C15 1.515(7) . ? C16 C17 1.398(6) . ? C16 C21 1.403(6) . ? C17 C18 1.394(7) . ? C17 C22 1.520(6) . ? C18 C19 1.385(7) . ? C19 C20 1.382(7) . ? C20 C21 1.384(6) . ? C21 C25 1.527(6) . ? C22 C24 1.518(8) . ? C22 C23 1.534(7) . ? C25 C26 1.524(6) . ? C25 C27 1.529(6) . ? C28 C29 1.510(6) . ? C28 C30 1.554(6) . ? C31 C32 1.523(6) . ? C31 C33 1.526(7) . ? 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 N3 177.88(14) . . ? C1 N1 C3 112.1(3) . . ? C1 N1 C4 124.7(3) . . ? C3 N1 C4 123.1(4) . . ? C1 N2 C2 112.4(3) . . ? C1 N2 C16 123.5(4) . . ? C2 N2 C16 124.0(3) . . ? C28 N3 C31 113.1(4) . . ? C28 N3 Au1 122.0(3) . . ? C31 N3 Au1 124.8(3) . . ? N2 C1 N1 102.2(4) . . ? N2 C1 Au1 129.8(3) . . ? N1 C1 Au1 127.8(3) . . ? C3 C2 N2 106.5(4) . . ? C2 C3 N1 106.8(4) . . ? C5 C4 C9 123.2(4) . . ? C5 C4 N1 118.7(4) . . ? C9 C4 N1 118.1(3) . . ? C6 C5 C4 117.1(4) . . ? C6 C5 C10 121.3(4) . . ? C4 C5 C10 121.4(4) . . ? C7 C6 C5 121.2(4) . . ? C6 C7 C8 120.2(4) . . ? C7 C8 C9 121.3(4) . . ? C8 C9 C4 116.9(4) . . ? C8 C9 C13 121.6(4) . . ? C4 C9 C13 121.5(4) . . ? C12 C10 C5 110.0(4) . . ? C12 C10 C11 110.0(4) . . ? C5 C10 C11 113.4(4) . . ? C14 C13 C15 110.5(5) . . ? C14 C13 C9 111.5(4) . . ? C15 C13 C9 113.3(4) . . ? C17 C16 C21 123.3(4) . . ? C17 C16 N2 118.4(4) . . ? C21 C16 N2 118.3(4) . . ? C18 C17 C16 117.0(4) . . ? C18 C17 C22 120.2(4) . . ? C16 C17 C22 122.8(4) . . ? C19 C18 C17 121.1(5) . . ? C20 C19 C18 120.0(5) . . ? C19 C20 C21 121.7(4) . . ? C20 C21 C16 116.9(4) . . ? C20 C21 C25 121.2(4) . . ? C16 C21 C25 121.9(4) . . ? C24 C22 C17 111.3(5) . . ? C24 C22 C23 112.5(5) . . ? C17 C22 C23 110.1(4) . . ? C26 C25 C21 112.6(4) . . ? C26 C25 C27 109.5(4) . . ? C21 C25 C27 109.8(4) . . ? N3 C28 C29 112.3(3) . . ? N3 C28 C30 112.2(4) . . ? C29 C28 C30 108.6(4) . . ? N3 C31 C32 111.0(4) . . ? N3 C31 C33 114.1(4) . . ? C32 C31 C33 109.7(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.194 _refine_diff_density_min -1.824 _refine_diff_density_rms 0.150 data_npm029 _database_code_depnum_ccdc_archive 'CCDC 901603' #TrackingRef 'web_deposit_cif_file_6_MilesW.Johnson_1352328108.[IPrAuN(H)iPr2][BF4].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ((IPr)AuNHiPr2)(BF4) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H51 Au B F4 N3' _chemical_formula_weight 773.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 12.0547(6) _cell_length_b 14.2387(7) _cell_length_c 20.0505(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3441.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 4.322 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2212 _exptl_absorpt_correction_T_max 0.4786 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100442 _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.46 _reflns_number_total 7850 _reflns_number_gt 7754 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0121P)^2^+0.5117P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(3) _refine_ls_number_reflns 7850 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0122 _refine_ls_R_factor_gt 0.0118 _refine_ls_wR_factor_ref 0.0286 _refine_ls_wR_factor_gt 0.0285 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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 Au1 Au 0.283901(5) 0.488972(4) 0.854249(3) 0.01393(2) Uani 1 1 d . . . N1 N 0.43234(12) 0.34820(10) 0.78895(7) 0.0150(3) Uani 1 1 d . . . N2 N 0.49553(12) 0.38605(10) 0.88537(7) 0.0143(3) Uani 1 1 d . . . N3 N 0.15369(13) 0.58528(10) 0.86275(8) 0.0161(3) Uani 1 1 d . . . H1 H 0.1752(17) 0.6268(14) 0.8376(10) 0.015(5) Uiso 1 1 d . . . C1 C 0.40986(14) 0.40114(12) 0.84329(9) 0.0144(4) Uani 1 1 d . . . C2 C 0.57143(14) 0.32436(11) 0.85717(10) 0.0181(3) Uani 1 1 d . . . H2 H 0.6384 0.3027 0.8769 0.022 Uiso 1 1 calc R . . C3 C 0.53213(15) 0.30103(13) 0.79651(10) 0.0180(4) Uani 1 1 d . . . H3 H 0.5661 0.2602 0.7651 0.022 Uiso 1 1 calc R . . C4 C 0.35603(15) 0.34019(12) 0.73370(9) 0.0160(3) Uani 1 1 d . . . C5 C 0.37069(16) 0.39841(12) 0.67810(9) 0.0188(4) Uani 1 1 d . . . C6 C 0.28803(18) 0.39579(12) 0.62944(9) 0.0228(4) Uani 1 1 d . . . H6 H 0.2950 0.4342 0.5909 0.027 Uiso 1 1 calc R . . C7 C 0.19596(16) 0.33824(12) 0.63618(10) 0.0226(4) Uani 1 1 d . . . H7 H 0.1394 0.3391 0.6032 0.027 Uiso 1 1 calc R . . C8 C 0.18607(15) 0.27926(13) 0.69106(10) 0.0203(4) Uani 1 1 d . . . H8 H 0.1234 0.2392 0.6946 0.024 Uiso 1 1 calc R . . C9 C 0.26605(15) 0.27787(12) 0.74079(9) 0.0171(4) Uani 1 1 d . . . C10 C 0.47174(16) 0.46117(13) 0.67057(10) 0.0227(4) Uani 1 1 d . . . H10 H 0.5139 0.4588 0.7135 0.027 Uiso 1 1 calc R . . C11 C 0.5471(2) 0.4234(2) 0.61618(15) 0.0638(10) Uani 1 1 d . . . H11A H 0.5093 0.4279 0.5730 0.096 Uiso 1 1 calc R . . H11B H 0.5651 0.3576 0.6255 0.096 Uiso 1 1 calc R . . H11C H 0.6156 0.4604 0.6149 0.096 Uiso 1 1 calc R . . C12 C 0.4398(2) 0.56179(17) 0.6584(2) 0.0750(12) Uani 1 1 d . . . H12A H 0.3950 0.5847 0.6958 0.113 Uiso 1 1 calc R . . H12B H 0.3965 0.5661 0.6171 0.113 Uiso 1 1 calc R . . H12C H 0.5069 0.6002 0.6543 0.113 Uiso 1 1 calc R . . C13 C 0.25616(15) 0.20975(13) 0.79923(10) 0.0209(4) Uani 1 1 d . . . H13 H 0.3240 0.2168 0.8275 0.025 Uiso 1 1 calc R . . C14 C 0.25180(18) 0.10727(13) 0.77423(11) 0.0298(5) Uani 1 1 d . . . H14A H 0.1871 0.0990 0.7453 0.045 Uiso 1 1 calc R . . H14B H 0.2461 0.0647 0.8125 0.045 Uiso 1 1 calc R . . H14C H 0.3195 0.0931 0.7491 0.045 Uiso 1 1 calc R . . C15 C 0.15638(19) 0.23194(15) 0.84225(11) 0.0332(5) Uani 1 1 d . . . H15A H 0.0887 0.2267 0.8154 0.050 Uiso 1 1 calc R . . H15B H 0.1629 0.2960 0.8597 0.050 Uiso 1 1 calc R . . H15C H 0.1529 0.1875 0.8795 0.050 Uiso 1 1 calc R . . C16 C 0.50112(15) 0.42295(13) 0.95228(9) 0.0155(4) Uani 1 1 d . . . C17 C 0.57001(14) 0.50033(13) 0.96439(8) 0.0190(3) Uani 1 1 d . . . C18 C 0.57575(17) 0.53255(14) 1.03009(10) 0.0255(4) Uani 1 1 d . . . H18 H 0.6223 0.5843 1.0405 0.031 Uiso 1 1 calc R . . C19 C 0.51478(16) 0.49036(16) 1.08033(9) 0.0295(4) Uani 1 1 d . . . H19 H 0.5200 0.5136 1.1246 0.035 Uiso 1 1 calc R . . C20 C 0.44658(17) 0.41500(15) 1.06681(10) 0.0268(4) Uani 1 1 d . . . H20 H 0.4052 0.3870 1.1019 0.032 Uiso 1 1 calc R . . C21 C 0.43759(16) 0.37923(14) 1.00194(10) 0.0207(4) Uani 1 1 d . . . C22 C 0.63149(15) 0.55022(13) 0.90895(10) 0.0211(4) Uani 1 1 d . . . H22 H 0.6404 0.5050 0.8712 0.025 Uiso 1 1 calc R . . C23 C 0.74676(16) 0.58300(15) 0.92976(12) 0.0299(5) Uani 1 1 d . . . H23A H 0.7868 0.5307 0.9505 0.045 Uiso 1 1 calc R . . H23B H 0.7400 0.6347 0.9618 0.045 Uiso 1 1 calc R . . H23C H 0.7876 0.6047 0.8904 0.045 Uiso 1 1 calc R . . C24 C 0.56184(18) 0.63396(14) 0.88360(11) 0.0268(4) Uani 1 1 d . . . H24A H 0.5480 0.6776 0.9205 0.040 Uiso 1 1 calc R . . H24B H 0.4910 0.6109 0.8661 0.040 Uiso 1 1 calc R . . H24C H 0.6024 0.6665 0.8481 0.040 Uiso 1 1 calc R . . C25 C 0.36236(17) 0.29628(15) 0.98805(10) 0.0254(4) Uani 1 1 d . . . H25 H 0.3614 0.2857 0.9387 0.031 Uiso 1 1 calc R . . C26 C 0.4059(2) 0.20661(16) 1.02101(13) 0.0373(6) Uani 1 1 d . . . H26A H 0.4091 0.2155 1.0694 0.056 Uiso 1 1 calc R . . H26B H 0.4804 0.1927 1.0041 0.056 Uiso 1 1 calc R . . H26C H 0.3561 0.1542 1.0106 0.056 Uiso 1 1 calc R . . C27 C 0.24320(17) 0.31642(18) 1.01035(13) 0.0364(6) Uani 1 1 d . . . H27A H 0.2155 0.3724 0.9872 0.055 Uiso 1 1 calc R . . H27B H 0.2418 0.3273 1.0586 0.055 Uiso 1 1 calc R . . H27C H 0.1960 0.2625 0.9995 0.055 Uiso 1 1 calc R . . C28 C 0.04668(15) 0.54887(14) 0.83425(9) 0.0206(4) Uani 1 1 d . . . H28 H -0.0086 0.6012 0.8342 0.025 Uiso 1 1 calc R . . C29 C 0.06605(17) 0.51832(17) 0.76247(10) 0.0314(5) Uani 1 1 d . . . H29A H 0.1181 0.4655 0.7617 0.047 Uiso 1 1 calc R . . H29B H 0.0970 0.5709 0.7370 0.047 Uiso 1 1 calc R . . H29C H -0.0045 0.4989 0.7425 0.047 Uiso 1 1 calc R . . C30 C 0.00162(16) 0.46985(14) 0.87666(11) 0.0276(5) Uani 1 1 d . . . H30A H -0.0128 0.4930 0.9219 0.041 Uiso 1 1 calc R . . H30B H 0.0560 0.4188 0.8785 0.041 Uiso 1 1 calc R . . H30C H -0.0676 0.4465 0.8571 0.041 Uiso 1 1 calc R . . C31 C 0.14494(16) 0.62683(13) 0.93170(9) 0.0190(4) Uani 1 1 d . . . H31 H 0.1296 0.5748 0.9639 0.023 Uiso 1 1 calc R . . C32 C 0.25597(16) 0.67073(15) 0.94974(11) 0.0279(5) Uani 1 1 d . . . H32A H 0.2730 0.7213 0.9182 0.042 Uiso 1 1 calc R . . H32B H 0.3142 0.6228 0.9476 0.042 Uiso 1 1 calc R . . H32C H 0.2523 0.6964 0.9950 0.042 Uiso 1 1 calc R . . C33 C 0.05161(17) 0.69829(15) 0.93703(11) 0.0275(4) Uani 1 1 d . . . H33A H -0.0200 0.6662 0.9327 0.041 Uiso 1 1 calc R . . H33B H 0.0592 0.7449 0.9014 0.041 Uiso 1 1 calc R . . H33C H 0.0555 0.7298 0.9804 0.041 Uiso 1 1 calc R . . B1 B 0.1821(2) 0.78502(19) 0.74738(14) 0.0315(6) Uani 1 1 d . . . F1 F 0.18988(14) 0.75077(14) 0.68268(8) 0.0655(5) Uani 1 1 d . . . F2 F 0.07849(11) 0.76197(12) 0.77231(8) 0.0518(4) Uani 1 1 d . . . F3 F 0.20199(15) 0.87813(10) 0.74609(11) 0.0728(6) Uani 1 1 d . . . F4 F 0.26149(10) 0.73908(10) 0.78584(7) 0.0401(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01338(3) 0.01460(3) 0.01382(3) -0.00031(2) 0.00040(2) 0.00267(2) N1 0.0137(7) 0.0146(7) 0.0167(8) -0.0003(6) 0.0017(6) 0.0005(6) N2 0.0116(7) 0.0150(7) 0.0164(7) 0.0015(6) 0.0018(6) 0.0022(6) N3 0.0181(7) 0.0168(7) 0.0134(8) 0.0002(7) 0.0001(6) 0.0018(6) C1 0.0146(8) 0.0137(8) 0.0149(9) 0.0021(7) 0.0001(7) -0.0023(6) C2 0.0143(8) 0.0170(8) 0.0230(9) 0.0017(9) 0.0022(8) 0.0044(6) C3 0.0156(9) 0.0171(9) 0.0214(10) 0.0000(8) 0.0030(7) 0.0029(7) C4 0.0150(8) 0.0157(8) 0.0174(9) -0.0042(7) 0.0003(7) 0.0022(7) C5 0.0213(10) 0.0157(8) 0.0195(9) -0.0026(7) -0.0005(8) 0.0003(7) C6 0.0285(10) 0.0200(8) 0.0198(9) 0.0001(7) -0.0026(8) -0.0001(9) C7 0.0218(10) 0.0223(8) 0.0235(10) -0.0054(8) -0.0053(8) 0.0025(7) C8 0.0172(10) 0.0190(9) 0.0247(10) -0.0063(8) 0.0011(7) -0.0012(7) C9 0.0164(9) 0.0154(8) 0.0193(9) -0.0040(7) 0.0030(7) -0.0001(7) C10 0.0243(10) 0.0214(9) 0.0224(9) 0.0025(8) -0.0036(8) -0.0065(8) C11 0.0451(16) 0.086(2) 0.0601(19) -0.0329(17) 0.0236(14) -0.0384(16) C12 0.0447(16) 0.0216(11) 0.159(4) 0.0165(19) -0.017(2) -0.0110(11) C13 0.0205(10) 0.0176(9) 0.0248(10) 0.0012(8) 0.0002(8) -0.0036(7) C14 0.0371(13) 0.0186(9) 0.0337(12) 0.0016(9) -0.0028(9) -0.0007(8) C15 0.0321(11) 0.0333(11) 0.0343(13) 0.0074(10) 0.0129(10) 0.0026(9) C16 0.0143(8) 0.0183(9) 0.0141(9) 0.0008(7) -0.0003(7) 0.0051(7) C17 0.0194(8) 0.0189(9) 0.0188(8) 0.0001(8) -0.0001(6) 0.0039(8) C18 0.0320(11) 0.0223(10) 0.0221(9) -0.0038(8) -0.0022(8) 0.0029(8) C19 0.0373(11) 0.0365(12) 0.0149(8) -0.0022(9) -0.0006(7) 0.0118(10) C20 0.0291(11) 0.0349(11) 0.0166(9) 0.0054(9) 0.0051(8) 0.0076(9) C21 0.0177(9) 0.0246(10) 0.0200(10) 0.0055(8) 0.0016(8) 0.0053(8) C22 0.0231(10) 0.0176(8) 0.0226(9) -0.0015(8) 0.0017(8) -0.0015(8) C23 0.0232(10) 0.0306(10) 0.0360(12) 0.0028(10) -0.0003(8) -0.0017(8) C24 0.0265(11) 0.0265(10) 0.0272(11) 0.0060(9) 0.0010(9) 0.0002(8) C25 0.0218(10) 0.0317(11) 0.0228(10) 0.0085(9) 0.0026(8) -0.0034(9) C26 0.0336(13) 0.0297(12) 0.0484(15) 0.0119(11) -0.0001(11) -0.0016(10) C27 0.0230(11) 0.0486(14) 0.0376(13) 0.0138(11) 0.0058(9) -0.0018(9) C28 0.0172(9) 0.0229(9) 0.0217(9) -0.0044(8) -0.0029(7) 0.0055(7) C29 0.0288(10) 0.0418(12) 0.0237(10) -0.0127(10) -0.0076(8) 0.0094(10) C30 0.0165(9) 0.0241(10) 0.0422(12) -0.0032(9) 0.0002(8) 0.0003(7) C31 0.0226(9) 0.0198(9) 0.0147(9) -0.0033(8) 0.0014(8) 0.0025(8) C32 0.0281(11) 0.0320(11) 0.0236(11) -0.0103(9) -0.0024(8) 0.0001(8) C33 0.0291(11) 0.0270(10) 0.0265(11) -0.0084(9) 0.0028(9) 0.0061(9) B1 0.0238(12) 0.0351(13) 0.0356(14) 0.0119(11) -0.0003(10) -0.0028(10) F1 0.0540(11) 0.1079(15) 0.0345(9) -0.0021(9) 0.0046(7) -0.0268(10) F2 0.0211(7) 0.0784(12) 0.0559(9) 0.0236(9) 0.0090(7) 0.0016(7) F3 0.0592(11) 0.0331(8) 0.1262(17) 0.0105(9) -0.0094(12) 0.0023(8) F4 0.0227(7) 0.0505(8) 0.0469(9) 0.0266(7) 0.0014(6) -0.0025(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 1.9793(17) . ? Au1 N3 2.0912(15) . ? N1 C1 1.352(2) . ? N1 C3 1.386(2) . ? N1 C4 1.444(2) . ? N2 C1 1.351(2) . ? N2 C2 1.389(2) . ? N2 C16 1.442(2) . ? N3 C28 1.503(2) . ? N3 C31 1.507(2) . ? C2 C3 1.347(3) . ? C4 C5 1.400(3) . ? C4 C9 1.409(2) . ? C5 C6 1.395(3) . ? C5 C10 1.518(3) . ? C6 C7 1.386(3) . ? C7 C8 1.389(3) . ? C8 C9 1.387(3) . ? C9 C13 1.526(3) . ? C10 C12 1.504(3) . ? C10 C11 1.518(3) . ? C13 C15 1.514(3) . ? C13 C14 1.544(3) . ? C16 C17 1.401(3) . ? C16 C21 1.402(3) . ? C17 C18 1.397(2) . ? C17 C22 1.513(2) . ? C18 C19 1.384(3) . ? C19 C20 1.379(3) . ? C20 C21 1.401(3) . ? C21 C25 1.515(3) . ? C22 C23 1.524(3) . ? C22 C24 1.544(3) . ? C25 C26 1.531(3) . ? C25 C27 1.532(3) . ? C28 C30 1.511(3) . ? C28 C29 1.522(3) . ? C31 C32 1.521(3) . ? C31 C33 1.521(3) . ? B1 F3 1.348(3) . ? B1 F2 1.385(3) . ? B1 F1 1.389(3) . ? B1 F4 1.392(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 N3 177.63(7) . . ? C1 N1 C3 110.85(15) . . ? C1 N1 C4 122.29(15) . . ? C3 N1 C4 126.75(15) . . ? C1 N2 C2 110.50(15) . . ? C1 N2 C16 123.97(15) . . ? C2 N2 C16 125.33(15) . . ? C28 N3 C31 115.08(15) . . ? C28 N3 Au1 112.77(11) . . ? C31 N3 Au1 112.62(11) . . ? N2 C1 N1 105.15(15) . . ? N2 C1 Au1 128.15(13) . . ? N1 C1 Au1 126.54(13) . . ? C3 C2 N2 106.97(16) . . ? C2 C3 N1 106.53(16) . . ? C5 C4 C9 123.40(17) . . ? C5 C4 N1 118.91(16) . . ? C9 C4 N1 117.56(16) . . ? C6 C5 C4 116.79(17) . . ? C6 C5 C10 121.28(17) . . ? C4 C5 C10 121.93(17) . . ? C7 C6 C5 121.30(17) . . ? C6 C7 C8 120.21(18) . . ? C9 C8 C7 121.22(18) . . ? C8 C9 C4 116.97(17) . . ? C8 C9 C13 120.45(17) . . ? C4 C9 C13 122.56(16) . . ? C12 C10 C11 112.0(3) . . ? C12 C10 C5 111.80(18) . . ? C11 C10 C5 110.08(17) . . ? C15 C13 C9 111.54(16) . . ? C15 C13 C14 110.81(16) . . ? C9 C13 C14 110.74(17) . . ? C17 C16 C21 123.37(17) . . ? C17 C16 N2 118.38(15) . . ? C21 C16 N2 118.25(16) . . ? C18 C17 C16 116.82(16) . . ? C18 C17 C22 120.96(17) . . ? C16 C17 C22 122.16(16) . . ? C19 C18 C17 121.17(19) . . ? C20 C19 C18 120.76(18) . . ? C19 C20 C21 120.77(19) . . ? C20 C21 C16 117.10(19) . . ? C20 C21 C25 120.03(18) . . ? C16 C21 C25 122.87(17) . . ? C17 C22 C23 112.90(17) . . ? C17 C22 C24 109.76(16) . . ? C23 C22 C24 110.45(16) . . ? C21 C25 C26 111.45(17) . . ? C21 C25 C27 111.21(18) . . ? C26 C25 C27 110.60(18) . . ? N3 C28 C30 110.57(16) . . ? N3 C28 C29 109.05(15) . . ? C30 C28 C29 111.99(17) . . ? N3 C31 C32 108.53(16) . . ? N3 C31 C33 112.26(16) . . ? C32 C31 C33 111.06(16) . . ? F3 B1 F2 113.6(2) . . ? F3 B1 F1 108.4(2) . . ? F2 B1 F1 108.3(2) . . ? F3 B1 F4 110.5(2) . . ? F2 B1 F4 107.98(19) . . ? F1 B1 F4 107.8(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.415 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.051 data_npm031 _database_code_depnum_ccdc_archive 'CCDC 901604' #TrackingRef 'web_deposit_cif_file_5_MilesW.Johnson_1352328108.IPrAuN(H)Ph.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (IPr)AuNHPh*THF _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 Au N3 O' _chemical_formula_weight 749.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5675(7) _cell_length_b 19.0611(10) _cell_length_c 14.9662(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.9710(10) _cell_angle_gamma 90.00 _cell_volume 3390.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9415 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 28.20 _exptl_crystal_description blade _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.465 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 4.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2186 _exptl_absorpt_correction_T_max 0.3539 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 130079 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0124 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7777 _reflns_number_gt 7273 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0154P)^2^+3.4136P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7777 _refine_ls_number_parameters 391 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0184 _refine_ls_R_factor_gt 0.0161 _refine_ls_wR_factor_ref 0.0390 _refine_ls_wR_factor_gt 0.0373 _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au -0.017965(5) 0.162125(3) 0.876794(4) 0.01243(3) Uani 1 1 d . . . C1 C 0.07288(15) 0.21505(9) 0.98962(12) 0.0133(3) Uani 1 1 d . . . C2 C 0.11546(15) 0.27351(9) 1.12909(13) 0.0164(3) Uani 1 1 d . . . H2 H 0.1078 0.2934 1.1849 0.020 Uiso 1 1 calc R . . C3 C 0.20637(15) 0.27707(10) 1.10031(13) 0.0169(4) Uani 1 1 d . . . H3 H 0.2757 0.2997 1.1322 0.020 Uiso 1 1 calc R . . C4 C 0.25395(15) 0.23440(10) 0.95954(12) 0.0152(3) Uani 1 1 d . . . C5 C 0.30836(16) 0.17006(10) 0.96023(13) 0.0170(4) Uani 1 1 d . . . C6 C 0.38285(17) 0.16655(10) 0.90868(15) 0.0217(4) Uani 1 1 d . . . H6 H 0.4217 0.1240 0.9077 0.026 Uiso 1 1 calc R . . C7 C 0.40129(17) 0.22412(12) 0.85883(15) 0.0249(4) Uani 1 1 d . . . H7 H 0.4530 0.2207 0.8247 0.030 Uiso 1 1 calc R . . C8 C 0.34470(17) 0.28641(11) 0.85865(14) 0.0221(4) Uani 1 1 d . . . H8 H 0.3575 0.3252 0.8236 0.027 Uiso 1 1 calc R . . C9 C 0.26908(15) 0.29334(10) 0.90904(13) 0.0175(4) Uani 1 1 d . . . C10 C 0.28944(17) 0.10762(10) 1.01633(14) 0.0208(4) Uani 1 1 d . . . H10 H 0.2103 0.1104 1.0172 0.025 Uiso 1 1 calc R . . C11 C 0.3670(3) 0.11123(13) 1.11826(16) 0.0420(6) Uani 1 1 d . . . H11A H 0.4453 0.1063 1.1201 0.063 Uiso 1 1 calc R . . H11B H 0.3483 0.0732 1.1547 0.063 Uiso 1 1 calc R . . H11C H 0.3574 0.1565 1.1457 0.063 Uiso 1 1 calc R . . C12 C 0.3032(2) 0.03704(11) 0.97343(17) 0.0359(5) Uani 1 1 d . . . H12A H 0.3822 0.0303 0.9785 0.054 Uiso 1 1 calc R . . H12B H 0.2564 0.0361 0.9067 0.054 Uiso 1 1 calc R . . H12C H 0.2797 -0.0006 1.0075 0.054 Uiso 1 1 calc R . . C13 C 0.20053(17) 0.35982(10) 0.90312(14) 0.0212(4) Uani 1 1 d . . . H13 H 0.1835 0.3645 0.9636 0.025 Uiso 1 1 calc R . . C14 C 0.2615(2) 0.42641(11) 0.89011(17) 0.0309(5) Uani 1 1 d . . . H14A H 0.3360 0.4282 0.9385 0.046 Uiso 1 1 calc R . . H14B H 0.2177 0.4676 0.8962 0.046 Uiso 1 1 calc R . . H14C H 0.2701 0.4261 0.8273 0.046 Uiso 1 1 calc R . . C15 C 0.08842(19) 0.35286(12) 0.82270(17) 0.0302(5) Uani 1 1 d . . . H15A H 0.0425 0.3947 0.8210 0.045 Uiso 1 1 calc R . . H15B H 0.0483 0.3112 0.8332 0.045 Uiso 1 1 calc R . . H15C H 0.1028 0.3482 0.7624 0.045 Uiso 1 1 calc R . . C16 C -0.07510(15) 0.21651(9) 1.06419(12) 0.0147(3) Uani 1 1 d . . . C17 C -0.08428(16) 0.15642(9) 1.11552(13) 0.0155(4) Uani 1 1 d . . . C18 C -0.19255(16) 0.13805(10) 1.11393(14) 0.0197(4) Uani 1 1 d . . . H18 H -0.2026 0.0979 1.1480 0.024 Uiso 1 1 calc R . . C19 C -0.28542(17) 0.17722(11) 1.06360(14) 0.0220(4) Uani 1 1 d . . . H19 H -0.3583 0.1634 1.0630 0.026 Uiso 1 1 calc R . . C20 C -0.27303(16) 0.23631(11) 1.01419(14) 0.0209(4) Uani 1 1 d . . . H20 H -0.3376 0.2627 0.9801 0.025 Uiso 1 1 calc R . . C21 C -0.16703(16) 0.25777(10) 1.01358(13) 0.0172(4) Uani 1 1 d . . . C22 C 0.01696(16) 0.11041(10) 1.16370(13) 0.0183(4) Uani 1 1 d . . . H22 H 0.0863 0.1392 1.1732 0.022 Uiso 1 1 calc R . . C23 C 0.01909(18) 0.08280(11) 1.26012(14) 0.0240(4) Uani 1 1 d . . . H23A H 0.0187 0.1224 1.3018 0.036 Uiso 1 1 calc R . . H23B H 0.0873 0.0548 1.2879 0.036 Uiso 1 1 calc R . . H23C H -0.0474 0.0535 1.2525 0.036 Uiso 1 1 calc R . . C24 C 0.0202(2) 0.04888(11) 1.09827(15) 0.0266(4) Uani 1 1 d . . . H24A H 0.0891 0.0216 1.1265 0.040 Uiso 1 1 calc R . . H24B H 0.0191 0.0671 1.0367 0.040 Uiso 1 1 calc R . . H24C H -0.0455 0.0187 1.0899 0.040 Uiso 1 1 calc R . . C25 C -0.15468(17) 0.32330(11) 0.96009(14) 0.0210(4) Uani 1 1 d . . . H25 H -0.0727 0.3304 0.9704 0.025 Uiso 1 1 calc R . . C26 C -0.1978(2) 0.38797(11) 0.99831(16) 0.0295(5) Uani 1 1 d . . . H26A H -0.2788 0.3833 0.9866 0.044 Uiso 1 1 calc R . . H26B H -0.1835 0.4300 0.9664 0.044 Uiso 1 1 calc R . . H26C H -0.1587 0.3920 1.0664 0.044 Uiso 1 1 calc R . . C27 C -0.2143(2) 0.31455(13) 0.85362(15) 0.0303(5) Uani 1 1 d . . . H27A H -0.1818 0.2746 0.8304 0.045 Uiso 1 1 calc R . . H27B H -0.2046 0.3573 0.8207 0.045 Uiso 1 1 calc R . . H27C H -0.2947 0.3062 0.8417 0.045 Uiso 1 1 calc R . . C28 C -0.22741(15) 0.08946(9) 0.75533(13) 0.0157(3) Uani 1 1 d . . . C29 C -0.27759(16) 0.10400(10) 0.82498(13) 0.0190(4) Uani 1 1 d . . . H29 H -0.2345 0.1262 0.8821 0.023 Uiso 1 1 calc R . . C30 C -0.38876(17) 0.08651(11) 0.81146(15) 0.0231(4) Uani 1 1 d . . . H30 H -0.4206 0.0975 0.8593 0.028 Uiso 1 1 calc R . . C31 C -0.45460(17) 0.05336(11) 0.72960(16) 0.0270(4) Uani 1 1 d . . . H31 H -0.5311 0.0424 0.7205 0.032 Uiso 1 1 calc R . . C32 C -0.40592(17) 0.03666(11) 0.66124(15) 0.0254(4) Uani 1 1 d . . . H32 H -0.4494 0.0131 0.6053 0.030 Uiso 1 1 calc R . . C33 C -0.29479(17) 0.05380(10) 0.67338(14) 0.0206(4) Uani 1 1 d . . . H33 H -0.2633 0.0414 0.6258 0.025 Uiso 1 1 calc R . . C34 C 0.01874(17) 0.19085(12) 0.62680(15) 0.0255(4) Uani 1 1 d . . . H34A H -0.0223 0.2190 0.6606 0.031 Uiso 1 1 calc R . . H34B H 0.0242 0.2185 0.5725 0.031 Uiso 1 1 calc R . . C35 C 0.13640(18) 0.17215(11) 0.69327(15) 0.0243(4) Uani 1 1 d . . . H35A H 0.1953 0.1921 0.6702 0.029 Uiso 1 1 calc R . . H35B H 0.1477 0.1898 0.7579 0.029 Uiso 1 1 calc R . . C36 C 0.1389(2) 0.09215(12) 0.69167(17) 0.0329(5) Uani 1 1 d . . . H36A H 0.2124 0.0747 0.6899 0.039 Uiso 1 1 calc R . . H36B H 0.1239 0.0721 0.7474 0.039 Uiso 1 1 calc R . . C37 C 0.0452(2) 0.07429(12) 0.60111(16) 0.0305(5) Uani 1 1 d . . . H37A H 0.0721 0.0770 0.5460 0.037 Uiso 1 1 calc R . . H37B H 0.0158 0.0265 0.6044 0.037 Uiso 1 1 calc R . . N1 N 0.17898(12) 0.24109(8) 1.01469(10) 0.0140(3) Uani 1 1 d . . . N2 N 0.03506(12) 0.23494(8) 1.06084(10) 0.0134(3) Uani 1 1 d . . . N3 N -0.11987(13) 0.10998(8) 0.76597(11) 0.0167(3) Uani 1 1 d . . . H1 H -0.1000(19) 0.0999(12) 0.7194(16) 0.018(6) Uiso 1 1 d . . . O1 O -0.03905(12) 0.12582(8) 0.59477(10) 0.0262(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01208(4) 0.01220(4) 0.01331(4) -0.00099(2) 0.00454(3) -0.00041(2) C1 0.0141(8) 0.0113(7) 0.0148(8) 0.0027(6) 0.0052(6) 0.0014(7) C2 0.0181(9) 0.0148(8) 0.0152(8) -0.0015(7) 0.0039(7) -0.0001(7) C3 0.0163(8) 0.0155(8) 0.0174(9) -0.0019(7) 0.0033(7) -0.0011(7) C4 0.0123(8) 0.0177(8) 0.0158(8) -0.0006(7) 0.0047(6) -0.0015(7) C5 0.0132(8) 0.0179(9) 0.0188(9) -0.0005(7) 0.0038(7) -0.0004(7) C6 0.0157(9) 0.0230(10) 0.0273(10) -0.0030(8) 0.0082(8) 0.0021(7) C7 0.0178(9) 0.0336(11) 0.0270(10) -0.0014(9) 0.0124(8) -0.0021(8) C8 0.0207(9) 0.0248(10) 0.0222(10) 0.0027(8) 0.0089(8) -0.0061(8) C9 0.0153(8) 0.0163(8) 0.0193(9) 0.0002(7) 0.0033(7) -0.0027(7) C10 0.0199(9) 0.0171(9) 0.0257(10) 0.0042(7) 0.0076(8) 0.0032(8) C11 0.0694(19) 0.0243(11) 0.0243(12) 0.0031(9) 0.0043(11) -0.0035(12) C12 0.0567(16) 0.0191(10) 0.0286(12) -0.0005(9) 0.0094(11) -0.0020(10) C13 0.0244(10) 0.0152(9) 0.0235(10) 0.0029(7) 0.0071(8) 0.0002(8) C14 0.0332(12) 0.0167(9) 0.0374(12) 0.0057(9) 0.0041(9) -0.0045(9) C15 0.0233(11) 0.0227(10) 0.0390(13) 0.0043(9) 0.0025(9) 0.0025(9) C16 0.0139(8) 0.0157(8) 0.0158(8) -0.0038(7) 0.0065(7) -0.0011(7) C17 0.0169(9) 0.0146(8) 0.0160(9) -0.0045(6) 0.0069(7) -0.0022(7) C18 0.0215(9) 0.0180(9) 0.0225(9) -0.0033(7) 0.0112(8) -0.0046(8) C19 0.0155(9) 0.0286(10) 0.0248(10) -0.0067(8) 0.0107(8) -0.0033(8) C20 0.0160(9) 0.0257(10) 0.0207(9) -0.0028(8) 0.0052(7) 0.0021(8) C21 0.0180(9) 0.0184(9) 0.0161(8) -0.0031(7) 0.0070(7) 0.0009(7) C22 0.0205(9) 0.0144(8) 0.0221(9) 0.0022(7) 0.0099(7) 0.0001(7) C23 0.0247(10) 0.0261(10) 0.0224(10) 0.0047(8) 0.0091(8) 0.0019(8) C24 0.0383(12) 0.0175(9) 0.0268(10) 0.0014(8) 0.0145(9) 0.0076(9) C25 0.0180(9) 0.0230(9) 0.0222(10) 0.0056(8) 0.0070(8) 0.0051(8) C26 0.0366(12) 0.0213(10) 0.0307(11) 0.0018(8) 0.0109(9) 0.0047(9) C27 0.0343(12) 0.0342(12) 0.0224(10) 0.0057(9) 0.0092(9) 0.0114(10) C28 0.0179(8) 0.0105(8) 0.0175(9) 0.0020(6) 0.0041(7) 0.0012(7) C29 0.0201(9) 0.0180(9) 0.0184(9) 0.0007(7) 0.0055(7) 0.0004(7) C30 0.0205(9) 0.0231(10) 0.0275(10) 0.0056(8) 0.0102(8) 0.0015(8) C31 0.0153(9) 0.0256(10) 0.0377(12) 0.0064(9) 0.0052(8) -0.0039(8) C32 0.0213(10) 0.0214(9) 0.0260(10) -0.0022(8) -0.0026(8) -0.0065(8) C33 0.0220(9) 0.0161(9) 0.0220(9) -0.0019(7) 0.0049(7) 0.0003(8) C34 0.0217(10) 0.0235(10) 0.0310(11) 0.0017(8) 0.0084(9) -0.0021(8) C35 0.0232(10) 0.0255(10) 0.0236(10) 0.0006(8) 0.0067(8) -0.0026(8) C36 0.0308(12) 0.0264(11) 0.0364(12) -0.0013(9) 0.0041(10) 0.0051(9) C37 0.0348(12) 0.0276(11) 0.0315(11) -0.0061(9) 0.0142(10) -0.0028(10) N1 0.0138(7) 0.0132(7) 0.0152(7) -0.0001(6) 0.0049(6) -0.0010(6) N2 0.0132(7) 0.0125(7) 0.0148(7) -0.0008(5) 0.0048(6) -0.0004(6) N3 0.0169(7) 0.0181(7) 0.0159(8) -0.0032(6) 0.0067(6) -0.0009(6) O1 0.0244(7) 0.0291(8) 0.0250(7) -0.0015(6) 0.0077(6) -0.0052(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 1.9797(18) . ? Au1 N3 1.9996(16) . ? C1 N2 1.355(2) . ? C1 N1 1.356(2) . ? C2 C3 1.347(3) . ? C2 N2 1.391(2) . ? C2 H2 0.9500 . ? C3 N1 1.394(2) . ? C3 H3 0.9500 . ? C4 C9 1.401(3) . ? C4 C5 1.403(3) . ? C4 N1 1.446(2) . ? C5 C6 1.395(3) . ? C5 C10 1.519(3) . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C8 1.384(3) . ? C7 H7 0.9500 . ? C8 C9 1.398(3) . ? C8 H8 0.9500 . ? C9 C13 1.519(3) . ? C10 C11 1.522(3) . ? C10 C12 1.524(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.528(3) . ? C13 C15 1.533(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.399(3) . ? C16 C17 1.405(3) . ? C16 N2 1.445(2) . ? C17 C18 1.398(3) . ? C17 C22 1.520(3) . ? C18 C19 1.384(3) . ? C18 H18 0.9500 . ? C19 C20 1.384(3) . ? C19 H19 0.9500 . ? C20 C21 1.396(3) . ? C20 H20 0.9500 . ? C21 C25 1.519(3) . ? C22 C23 1.528(3) . ? C22 C24 1.537(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.530(3) . ? C25 C27 1.534(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 N3 1.366(2) . ? C28 C29 1.410(3) . ? C28 C33 1.417(3) . ? C29 C30 1.386(3) . ? C29 H29 0.9500 . ? C30 C31 1.388(3) . ? C30 H30 0.9500 . ? C31 C32 1.389(3) . ? C31 H31 0.9500 . ? C32 C33 1.388(3) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 O1 1.438(3) . ? C34 C35 1.532(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.526(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.518(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 O1 1.424(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? N3 H1 0.84(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 N3 175.65(7) . . ? N2 C1 N1 104.17(15) . . ? N2 C1 Au1 124.13(13) . . ? N1 C1 Au1 131.67(13) . . ? C3 C2 N2 106.32(16) . . ? C3 C2 H2 126.8 . . ? N2 C2 H2 126.8 . . ? C2 C3 N1 106.69(16) . . ? C2 C3 H3 126.7 . . ? N1 C3 H3 126.7 . . ? C9 C4 C5 123.62(17) . . ? C9 C4 N1 117.72(16) . . ? C5 C4 N1 118.65(16) . . ? C6 C5 C4 116.82(17) . . ? C6 C5 C10 121.45(17) . . ? C4 C5 C10 121.71(17) . . ? C7 C6 C5 121.24(18) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C8 C7 C6 120.26(18) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.26(18) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C8 C9 C4 116.78(17) . . ? C8 C9 C13 121.30(17) . . ? C4 C9 C13 121.78(17) . . ? C5 C10 C11 110.75(17) . . ? C5 C10 C12 113.52(17) . . ? C11 C10 C12 109.81(18) . . ? C5 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? C12 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 113.70(17) . . ? C9 C13 C15 109.44(17) . . ? C14 C13 C15 110.06(17) . . ? C9 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 123.66(17) . . ? C21 C16 N2 118.44(16) . . ? C17 C16 N2 117.85(16) . . ? C18 C17 C16 116.58(17) . . ? C18 C17 C22 121.57(17) . . ? C16 C17 C22 121.66(16) . . ? C19 C18 C17 121.21(18) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C20 C19 C18 120.57(18) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 121.01(18) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 116.96(17) . . ? C20 C21 C25 120.37(17) . . ? C16 C21 C25 122.67(17) . . ? C17 C22 C23 113.68(16) . . ? C17 C22 C24 109.24(16) . . ? C23 C22 C24 110.07(16) . . ? C17 C22 H22 107.9 . . ? C23 C22 H22 107.9 . . ? C24 C22 H22 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 110.87(16) . . ? C21 C25 C27 111.04(18) . . ? C26 C25 C27 111.29(17) . . ? C21 C25 H25 107.8 . . ? C26 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N3 C28 C29 121.40(17) . . ? N3 C28 C33 121.90(17) . . ? C29 C28 C33 116.68(17) . . ? C30 C29 C28 121.12(18) . . ? C30 C29 H29 119.4 . . ? C28 C29 H29 119.4 . . ? C29 C30 C31 121.46(19) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C32 118.40(19) . . ? C30 C31 H31 120.8 . . ? C32 C31 H31 120.8 . . ? C33 C32 C31 121.02(19) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C28 121.27(19) . . ? C32 C33 H33 119.4 . . ? C28 C33 H33 119.4 . . ? O1 C34 C35 106.99(17) . . ? O1 C34 H34A 110.3 . . ? C35 C34 H34A 110.3 . . ? O1 C34 H34B 110.3 . . ? C35 C34 H34B 110.3 . . ? H34A C34 H34B 108.6 . . ? C36 C35 C34 104.06(17) . . ? C36 C35 H35A 110.9 . . ? C34 C35 H35A 110.9 . . ? C36 C35 H35B 110.9 . . ? C34 C35 H35B 110.9 . . ? H35A C35 H35B 109.0 . . ? C37 C36 C35 102.95(18) . . ? C37 C36 H36A 111.2 . . ? C35 C36 H36A 111.2 . . ? C37 C36 H36B 111.2 . . ? C35 C36 H36B 111.2 . . ? H36A C36 H36B 109.1 . . ? O1 C37 C36 104.43(17) . . ? O1 C37 H37A 110.9 . . ? C36 C37 H37A 110.9 . . ? O1 C37 H37B 110.9 . . ? C36 C37 H37B 110.9 . . ? H37A C37 H37B 108.9 . . ? C1 N1 C3 111.17(15) . . ? C1 N1 C4 125.05(15) . . ? C3 N1 C4 123.77(15) . . ? C1 N2 C2 111.65(15) . . ? C1 N2 C16 122.99(15) . . ? C2 N2 C16 125.35(15) . . ? C28 N3 Au1 125.57(13) . . ? C28 N3 H1 112.9(16) . . ? Au1 N3 H1 121.5(16) . . ? C37 O1 C34 106.76(16) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.088 _refine_diff_density_min -1.012 _refine_diff_density_rms 0.071 data_npm038 _database_code_depnum_ccdc_archive 'CCDC 901605' #TrackingRef 'web_deposit_cif_file_1_MilesW.Johnson_1352328108.npm038.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; npm038 ; _chemical_name_common npm038 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H53 Au N4' _chemical_formula_weight 738.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8111(8) _cell_length_b 20.7615(16) _cell_length_c 16.2556(12) _cell_angle_alpha 90.00 _cell_angle_beta 103.247(3) _cell_angle_gamma 90.00 _cell_volume 3551.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9851 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.382 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 4.170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6805 _exptl_absorpt_correction_T_max 0.8851 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 8842 _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.42 _reflns_number_total 8842 _reflns_number_gt 7050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0573P)^2^+83.2080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8842 _refine_ls_number_parameters 383 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0875 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1588 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0506(9) 0.2612(5) -0.0007(6) 0.017(2) Uani 1 1 d . . . C2 C -0.0267(10) 0.2802(5) -0.1389(6) 0.019(2) Uani 1 1 d . . . H2 H -0.0585 0.2733 -0.1977 0.023 Uiso 1 1 calc R . . C3 C -0.0101(10) 0.3381(5) -0.0985(7) 0.017(2) Uani 1 1 d . . . H3 H -0.0273 0.3795 -0.1234 0.020 Uiso 1 1 calc R . . C4 C 0.0737(10) 0.3761(5) 0.0468(6) 0.017(2) Uani 1 1 d . . . C5 C -0.0132(10) 0.3986(5) 0.0905(6) 0.022(2) Uani 1 1 d . . . C6 C 0.0259(11) 0.4510(5) 0.1435(7) 0.022(3) Uani 1 1 d . . . H6 H -0.0312 0.4683 0.1743 0.027 Uiso 1 1 calc R . . C7 C 0.1414(12) 0.4783(5) 0.1528(8) 0.030(3) Uani 1 1 d . . . H7 H 0.1632 0.5151 0.1877 0.036 Uiso 1 1 calc R . . C8 C 0.2305(11) 0.4519(6) 0.1102(7) 0.028(3) Uani 1 1 d . . . H8 H 0.3126 0.4705 0.1180 0.033 Uiso 1 1 calc R . . C9 C 0.1986(11) 0.3990(6) 0.0574(7) 0.024(3) Uani 1 1 d . . . C10 C -0.1427(11) 0.3669(6) 0.0844(7) 0.026(3) Uani 1 1 d . . . H10 H -0.1612 0.3388 0.0330 0.031 Uiso 1 1 calc R . . C11 C -0.2478(12) 0.4151(7) 0.0759(9) 0.042(3) Uani 1 1 d . . . H11A H -0.3299 0.3931 0.0594 0.063 Uiso 1 1 calc R . . H11B H -0.2406 0.4468 0.0326 0.063 Uiso 1 1 calc R . . H11C H -0.2416 0.4370 0.1301 0.063 Uiso 1 1 calc R . . C12 C -0.1364(14) 0.3246(7) 0.1604(8) 0.043(4) Uani 1 1 d . . . H12A H -0.0701 0.2920 0.1629 0.065 Uiso 1 1 calc R . . H12B H -0.2185 0.3033 0.1559 0.065 Uiso 1 1 calc R . . H12C H -0.1164 0.3509 0.2117 0.065 Uiso 1 1 calc R . . C13 C 0.2942(12) 0.3702(6) 0.0140(8) 0.032(3) Uani 1 1 d . . . H13 H 0.2494 0.3375 -0.0274 0.039 Uiso 1 1 calc R . . C14 C 0.3532(14) 0.4196(7) -0.0344(9) 0.047(4) Uani 1 1 d . . . H14A H 0.2858 0.4447 -0.0712 0.070 Uiso 1 1 calc R . . H14B H 0.4036 0.3975 -0.0688 0.070 Uiso 1 1 calc R . . H14C H 0.4082 0.4486 0.0056 0.070 Uiso 1 1 calc R . . C15 C 0.3987(12) 0.3348(6) 0.0801(9) 0.036(3) Uani 1 1 d . . . H15A H 0.4345 0.3642 0.1266 0.054 Uiso 1 1 calc R . . H15B H 0.4662 0.3204 0.0532 0.054 Uiso 1 1 calc R . . H15C H 0.3615 0.2974 0.1023 0.054 Uiso 1 1 calc R . . C16 C 0.0115(10) 0.1645(5) -0.0915(6) 0.022(2) Uani 1 1 d . . . C17 C -0.0886(11) 0.1290(6) -0.0780(7) 0.028(3) Uani 1 1 d . . . C18 C -0.0836(12) 0.0617(6) -0.0904(8) 0.035(3) Uani 1 1 d . . . H18 H -0.1510 0.0354 -0.0810 0.042 Uiso 1 1 calc R . . C19 C 0.0171(12) 0.0333(6) -0.1160(7) 0.032(3) Uani 1 1 d . . . H19 H 0.0190 -0.0120 -0.1243 0.039 Uiso 1 1 calc R . . C20 C 0.1142(11) 0.0716(6) -0.1291(7) 0.027(3) Uani 1 1 d . . . H20 H 0.1834 0.0520 -0.1466 0.032 Uiso 1 1 calc R . . C21 C 0.1148(10) 0.1379(5) -0.1176(6) 0.020(2) Uani 1 1 d . . . C22 C -0.2017(13) 0.1583(7) -0.0508(9) 0.041(3) Uani 1 1 d . . . H22 H -0.1871 0.2058 -0.0471 0.049 Uiso 1 1 calc R . . C23 C -0.3277(14) 0.1473(8) -0.1194(11) 0.060(4) Uani 1 1 d . . . H23A H -0.3155 0.1608 -0.1748 0.090 Uiso 1 1 calc R . . H23B H -0.3962 0.1727 -0.1050 0.090 Uiso 1 1 calc R . . H23C H -0.3503 0.1015 -0.1213 0.090 Uiso 1 1 calc R . . C24 C -0.2108(16) 0.1362(8) 0.0357(10) 0.060(5) Uani 1 1 d . . . H24A H -0.2058 0.0891 0.0386 0.090 Uiso 1 1 calc R . . H24B H -0.2919 0.1505 0.0468 0.090 Uiso 1 1 calc R . . H24C H -0.1406 0.1548 0.0782 0.090 Uiso 1 1 calc R . . C25 C 0.2255(10) 0.1791(6) -0.1313(7) 0.023(3) Uani 1 1 d . . . H25 H 0.1955 0.2248 -0.1389 0.027 Uiso 1 1 calc R . . C26 C 0.2738(12) 0.1599(6) -0.2093(7) 0.027(3) Uani 1 1 d . . . H26A H 0.3095 0.1164 -0.2016 0.041 Uiso 1 1 calc R . . H26B H 0.3396 0.1903 -0.2170 0.041 Uiso 1 1 calc R . . H26C H 0.2031 0.1608 -0.2593 0.041 Uiso 1 1 calc R . . C27 C 0.3372(12) 0.1766(8) -0.0531(8) 0.047(4) Uani 1 1 d . . . H27A H 0.3078 0.1902 -0.0030 0.070 Uiso 1 1 calc R . . H27B H 0.4048 0.2055 -0.0614 0.070 Uiso 1 1 calc R . . H27C H 0.3699 0.1325 -0.0450 0.070 Uiso 1 1 calc R . . C28 C 0.2424(11) 0.1644(6) 0.2125(7) 0.029(3) Uani 1 1 d . . . H28 H 0.2762 0.1963 0.2583 0.035 Uiso 1 1 calc R . . C29 C 0.1650(13) 0.1195(6) 0.2429(8) 0.032(3) Uani 1 1 d . . . C30 C 0.3556(12) 0.1322(6) 0.1856(7) 0.035(3) Uani 1 1 d . . . H30A H 0.3243 0.0931 0.1525 0.042 Uiso 1 1 calc R . . H30B H 0.3872 0.1621 0.1476 0.042 Uiso 1 1 calc R . . C31 C 0.5166(14) 0.0524(7) 0.2417(8) 0.044(4) Uani 1 1 d . . . H31 H 0.6022 0.0521 0.2815 0.053 Uiso 1 1 calc R . . C32 C 0.5379(16) 0.0379(8) 0.1537(10) 0.058(4) Uani 1 1 d . . . H32A H 0.4559 0.0366 0.1128 0.086 Uiso 1 1 calc R . . H32B H 0.5804 -0.0039 0.1545 0.086 Uiso 1 1 calc R . . H32C H 0.5911 0.0716 0.1375 0.086 Uiso 1 1 calc R . . C33 C 0.4398(14) -0.0009(7) 0.2704(8) 0.041(3) Uani 1 1 d . . . H33A H 0.4356 0.0067 0.3292 0.062 Uiso 1 1 calc R . . H33B H 0.4806 -0.0425 0.2661 0.062 Uiso 1 1 calc R . . H33C H 0.3536 -0.0012 0.2344 0.062 Uiso 1 1 calc R . . C34 C 0.5469(14) 0.1695(7) 0.2806(9) 0.043(3) Uani 1 1 d . . . H34 H 0.4923 0.2084 0.2808 0.052 Uiso 1 1 calc R . . C35 C 0.6331(14) 0.1847(8) 0.2219(9) 0.051(4) Uani 1 1 d . . . H35A H 0.6959 0.1502 0.2250 0.077 Uiso 1 1 calc R . . H35B H 0.6769 0.2256 0.2387 0.077 Uiso 1 1 calc R . . H35C H 0.5823 0.1882 0.1638 0.077 Uiso 1 1 calc R . . C36 C 0.6216(15) 0.1604(9) 0.3705(9) 0.057(4) Uani 1 1 d . . . H36A H 0.5648 0.1653 0.4092 0.086 Uiso 1 1 calc R . . H36B H 0.6893 0.1927 0.3837 0.086 Uiso 1 1 calc R . . H36C H 0.6590 0.1171 0.3768 0.086 Uiso 1 1 calc R . . N1 N 0.0116(8) 0.2331(4) -0.0777(5) 0.021(2) Uani 1 1 d . . . N2 N 0.0366(8) 0.3245(4) -0.0145(5) 0.0145(18) Uani 1 1 d . . . N3 N 0.0973(13) 0.0819(6) 0.2651(7) 0.050(3) Uani 1 1 d . . . N4 N 0.4589(9) 0.1146(5) 0.2524(6) 0.033(3) Uani 1 1 d . . . Au1 Au 0.13346(6) 0.21408(2) 0.10755(3) 0.02107(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.006(5) 0.026(6) 0.020(5) 0.004(4) 0.002(4) 0.002(4) C2 0.017(6) 0.024(6) 0.016(5) 0.003(4) 0.004(4) 0.010(5) C3 0.014(6) 0.012(6) 0.028(6) -0.001(4) 0.011(5) 0.006(4) C4 0.021(6) 0.017(6) 0.011(5) 0.008(4) -0.003(4) 0.001(4) C5 0.029(7) 0.022(6) 0.015(5) 0.005(4) 0.004(5) 0.001(5) C6 0.022(6) 0.021(6) 0.022(6) 0.000(5) 0.002(5) 0.009(5) C7 0.044(8) 0.008(6) 0.040(7) -0.011(5) 0.012(6) 0.002(5) C8 0.020(6) 0.023(7) 0.035(7) -0.001(5) -0.004(5) -0.008(5) C9 0.027(7) 0.025(7) 0.019(6) 0.001(5) 0.006(5) -0.004(5) C10 0.028(7) 0.027(7) 0.024(6) -0.005(5) 0.007(5) 0.001(5) C11 0.030(8) 0.055(10) 0.043(8) -0.005(7) 0.010(6) 0.002(6) C12 0.042(9) 0.051(10) 0.038(8) 0.004(7) 0.013(7) -0.004(7) C13 0.034(7) 0.031(8) 0.038(7) -0.011(6) 0.021(6) -0.004(6) C14 0.058(10) 0.047(10) 0.041(8) -0.001(7) 0.025(7) -0.003(7) C15 0.030(8) 0.029(8) 0.053(8) -0.003(6) 0.020(7) -0.005(6) C16 0.024(6) 0.021(6) 0.019(6) 0.002(4) 0.003(5) -0.001(5) C17 0.035(7) 0.029(7) 0.021(6) 0.001(5) 0.009(5) -0.002(5) C18 0.037(8) 0.031(8) 0.037(7) -0.003(6) 0.007(6) -0.005(6) C19 0.043(8) 0.022(7) 0.031(7) -0.001(5) 0.007(6) 0.005(6) C20 0.029(7) 0.026(7) 0.026(6) -0.005(5) 0.006(5) 0.003(5) C21 0.025(6) 0.023(6) 0.012(5) -0.002(4) 0.005(4) 0.004(5) C22 0.034(8) 0.038(9) 0.056(9) -0.004(7) 0.022(7) -0.009(6) C23 0.036(9) 0.058(11) 0.087(12) -0.018(9) 0.018(9) -0.004(8) C24 0.072(11) 0.063(11) 0.061(10) -0.006(8) 0.051(9) 0.005(9) C25 0.018(6) 0.019(6) 0.027(6) -0.006(5) -0.003(5) -0.001(5) C26 0.036(8) 0.026(7) 0.025(6) 0.001(5) 0.017(6) -0.004(5) C27 0.027(8) 0.080(12) 0.034(7) -0.020(7) 0.007(6) -0.007(7) C28 0.030(7) 0.032(7) 0.022(6) 0.005(5) -0.001(5) 0.015(5) C29 0.049(8) 0.018(7) 0.030(7) -0.001(5) 0.009(6) 0.000(6) C30 0.046(8) 0.033(8) 0.027(6) 0.002(5) 0.009(6) -0.004(6) C31 0.053(9) 0.049(10) 0.031(7) 0.009(6) 0.010(6) 0.018(7) C32 0.064(11) 0.056(11) 0.058(10) 0.006(8) 0.025(8) 0.010(8) C33 0.057(9) 0.032(8) 0.034(7) 0.002(6) 0.008(6) 0.009(7) C34 0.040(9) 0.046(9) 0.043(8) 0.002(7) 0.010(7) -0.001(7) C35 0.049(9) 0.064(11) 0.040(8) 0.010(7) 0.008(7) -0.019(8) C36 0.053(10) 0.076(13) 0.041(8) 0.008(8) 0.009(7) -0.007(9) N1 0.025(5) 0.021(5) 0.017(4) -0.008(4) 0.006(4) 0.006(4) N2 0.018(5) 0.015(5) 0.011(4) -0.002(3) 0.005(3) -0.002(4) N3 0.077(9) 0.035(7) 0.040(7) 0.000(5) 0.019(6) -0.007(6) N4 0.022(6) 0.044(7) 0.031(6) 0.010(5) 0.004(4) 0.005(5) Au1 0.0221(2) 0.0241(2) 0.0162(2) 0.00577(19) 0.00266(13) 0.0044(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.335(13) . ? C1 N1 1.357(13) . ? C1 Au1 2.033(10) . ? C2 C3 1.363(15) . ? C2 N1 1.388(13) . ? C2 H2 0.9500 . ? C3 N2 1.372(13) . ? C3 H3 0.9500 . ? C4 C5 1.383(15) . ? C4 C9 1.404(15) . ? C4 N2 1.457(13) . ? C5 C6 1.392(15) . ? C5 C10 1.531(16) . ? C6 C7 1.348(16) . ? C6 H6 0.9500 . ? C7 C8 1.418(16) . ? C7 H7 0.9500 . ? C8 C9 1.387(16) . ? C8 H8 0.9500 . ? C9 C13 1.502(16) . ? C10 C11 1.497(17) . ? C10 C12 1.504(17) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.519(17) . ? C13 C15 1.555(18) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.368(16) . ? C16 C21 1.397(15) . ? C16 N1 1.443(14) . ? C17 C18 1.414(17) . ? C17 C22 1.519(18) . ? C18 C19 1.383(17) . ? C18 H18 0.9500 . ? C19 C20 1.372(17) . ? C19 H19 0.9500 . ? C20 C21 1.389(15) . ? C20 H20 0.9500 . ? C21 C25 1.529(15) . ? C22 C24 1.50(2) . ? C22 C23 1.57(2) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.531(15) . ? C25 C27 1.540(16) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.416(18) . ? C28 C30 1.543(17) . ? C28 Au1 2.107(11) . ? C28 H28 1.0000 . ? C29 N3 1.181(16) . ? C30 N4 1.416(15) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 N4 1.461(17) . ? C31 C33 1.52(2) . ? C31 C32 1.531(19) . ? C31 H31 1.0000 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 N4 1.489(17) . ? C34 C35 1.512(19) . ? C34 C36 1.511(19) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 105.5(9) . . ? N2 C1 Au1 129.0(8) . . ? N1 C1 Au1 125.0(8) . . ? C3 C2 N1 106.9(9) . . ? C3 C2 H2 126.5 . . ? N1 C2 H2 126.5 . . ? C2 C3 N2 105.9(9) . . ? C2 C3 H3 127.0 . . ? N2 C3 H3 127.0 . . ? C5 C4 C9 124.7(10) . . ? C5 C4 N2 119.2(9) . . ? C9 C4 N2 116.1(9) . . ? C4 C5 C6 115.9(10) . . ? C4 C5 C10 122.7(10) . . ? C6 C5 C10 121.4(10) . . ? C7 C6 C5 122.7(10) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 C8 119.9(10) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C9 C8 C7 120.5(10) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C4 116.1(10) . . ? C8 C9 C13 120.3(10) . . ? C4 C9 C13 123.6(10) . . ? C11 C10 C12 111.0(10) . . ? C11 C10 C5 112.4(10) . . ? C12 C10 C5 109.3(10) . . ? C11 C10 H10 108.0 . . ? C12 C10 H10 108.0 . . ? C5 C10 H10 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 113.0(11) . . ? C9 C13 C15 109.5(10) . . ? C14 C13 C15 110.6(11) . . ? C9 C13 H13 107.9 . . ? C14 C13 H13 107.9 . . ? C15 C13 H13 107.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.6(11) . . ? C17 C16 N1 118.7(10) . . ? C21 C16 N1 117.8(9) . . ? C16 C17 C18 116.9(11) . . ? C16 C17 C22 123.4(11) . . ? C18 C17 C22 119.8(11) . . ? C19 C18 C17 121.5(12) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 118.8(12) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C19 C20 C21 122.3(11) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C20 C21 C16 117.0(10) . . ? C20 C21 C25 121.0(9) . . ? C16 C21 C25 122.0(10) . . ? C24 C22 C17 112.3(12) . . ? C24 C22 C23 112.9(12) . . ? C17 C22 C23 111.2(11) . . ? C24 C22 H22 106.6 . . ? C17 C22 H22 106.6 . . ? C23 C22 H22 106.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 113.7(9) . . ? C21 C25 C27 110.6(10) . . ? C26 C25 C27 108.9(10) . . ? C21 C25 H25 107.8 . . ? C26 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C30 112.6(11) . . ? C29 C28 Au1 109.8(8) . . ? C30 C28 Au1 108.3(7) . . ? C29 C28 H28 108.7 . . ? C30 C28 H28 108.7 . . ? Au1 C28 H28 108.7 . . ? N3 C29 C28 177.4(14) . . ? N4 C30 C28 115.6(10) . . ? N4 C30 H30A 108.4 . . ? C28 C30 H30A 108.4 . . ? N4 C30 H30B 108.4 . . ? C28 C30 H30B 108.4 . . ? H30A C30 H30B 107.4 . . ? N4 C31 C33 109.2(11) . . ? N4 C31 C32 116.4(11) . . ? C33 C31 C32 110.7(13) . . ? N4 C31 H31 106.7 . . ? C33 C31 H31 106.7 . . ? C32 C31 H31 106.7 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 C35 114.1(12) . . ? N4 C34 C36 111.3(12) . . ? C35 C34 C36 111.5(13) . . ? N4 C34 H34 106.4 . . ? C35 C34 H34 106.4 . . ? C36 C34 H34 106.4 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 N1 C2 109.7(9) . . ? C1 N1 C16 123.8(9) . . ? C2 N1 C16 126.5(9) . . ? C1 N2 C3 111.9(8) . . ? C1 N2 C4 127.3(8) . . ? C3 N2 C4 120.6(8) . . ? C30 N4 C31 114.9(11) . . ? C30 N4 C34 112.0(11) . . ? C31 N4 C34 116.9(11) . . ? C1 Au1 C28 171.8(4) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 3.953 _refine_diff_density_min -2.205 _refine_diff_density_rms 0.207 _iucr_refine_instructions_details ; TITL npm038 in P2(1)/c CELL 0.71073 10.8111 20.7615 16.2556 90.000 103.247 90.000 ZERR 4.00 0.0008 0.0016 0.0012 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N AU UNIT 144 212 16 4 MERG 0 FMAP 2 PLAN 25 SIZE 0.03 0.10 0.10 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.057300 83.208000 BASF 0.28492 FVAR 0.22765 C1 1 0.050617 0.261192 -0.000705 11.00000 0.00575 0.02572 = 0.01957 0.00418 0.00169 0.00249 C2 1 -0.026740 0.280169 -0.138875 11.00000 0.01657 0.02371 = 0.01627 0.00269 0.00412 0.00973 AFIX 43 H2 2 -0.058538 0.273279 -0.197704 11.00000 -1.20000 AFIX 0 C3 1 -0.010117 0.338135 -0.098487 11.00000 0.01415 0.01222 = 0.02794 -0.00127 0.01118 0.00562 AFIX 43 H3 2 -0.027330 0.379531 -0.123377 11.00000 -1.20000 AFIX 0 C4 1 0.073722 0.376119 0.046792 11.00000 0.02098 0.01712 = 0.01108 0.00835 -0.00257 0.00140 C5 1 -0.013200 0.398645 0.090486 11.00000 0.02888 0.02193 = 0.01548 0.00523 0.00382 0.00115 C6 1 0.025896 0.451042 0.143460 11.00000 0.02212 0.02110 = 0.02174 0.00014 0.00178 0.00896 AFIX 43 H6 2 -0.031164 0.468303 0.174322 11.00000 -1.20000 AFIX 0 C7 1 0.141431 0.478291 0.152752 11.00000 0.04415 0.00752 = 0.03989 -0.01056 0.01185 0.00182 AFIX 43 H7 2 0.163171 0.515138 0.187729 11.00000 -1.20000 AFIX 0 C8 1 0.230503 0.451851 0.110215 11.00000 0.01976 0.02310 = 0.03514 -0.00050 -0.00418 -0.00802 AFIX 43 H8 2 0.312636 0.470470 0.117962 11.00000 -1.20000 AFIX 0 C9 1 0.198585 0.399011 0.057390 11.00000 0.02725 0.02532 = 0.01938 0.00123 0.00582 -0.00449 C10 1 -0.142716 0.366853 0.084397 11.00000 0.02762 0.02654 = 0.02358 -0.00450 0.00749 0.00063 AFIX 13 H10 2 -0.161211 0.338846 0.032983 11.00000 -1.20000 AFIX 0 C11 1 -0.247770 0.415103 0.075867 11.00000 0.03002 0.05471 = 0.04261 -0.00527 0.01044 0.00151 AFIX 137 H11A 2 -0.329886 0.393054 0.059404 11.00000 -1.50000 H11B 2 -0.240628 0.446828 0.032555 11.00000 -1.50000 H11C 2 -0.241578 0.437017 0.130056 11.00000 -1.50000 AFIX 0 C12 1 -0.136366 0.324569 0.160354 11.00000 0.04188 0.05088 = 0.03849 0.00376 0.01338 -0.00436 AFIX 137 H12A 2 -0.070060 0.291957 0.162898 11.00000 -1.50000 H12B 2 -0.218524 0.303273 0.155950 11.00000 -1.50000 H12C 2 -0.116374 0.350919 0.211717 11.00000 -1.50000 AFIX 0 C13 1 0.294179 0.370229 0.014024 11.00000 0.03374 0.03108 = 0.03831 -0.01054 0.02112 -0.00419 AFIX 13 H13 2 0.249362 0.337486 -0.027357 11.00000 -1.20000 AFIX 0 C14 1 0.353166 0.419644 -0.034394 11.00000 0.05767 0.04708 = 0.04131 -0.00080 0.02451 -0.00284 AFIX 137 H14A 2 0.285752 0.444693 -0.071245 11.00000 -1.50000 H14B 2 0.403615 0.397518 -0.068768 11.00000 -1.50000 H14C 2 0.408175 0.448591 0.005604 11.00000 -1.50000 AFIX 0 C15 1 0.398750 0.334787 0.080141 11.00000 0.03043 0.02895 = 0.05291 -0.00312 0.02014 -0.00470 AFIX 137 H15A 2 0.434470 0.364241 0.126629 11.00000 -1.50000 H15B 2 0.466226 0.320363 0.053182 11.00000 -1.50000 H15C 2 0.361460 0.297420 0.102281 11.00000 -1.50000 AFIX 0 C16 1 0.011469 0.164493 -0.091522 11.00000 0.02385 0.02077 = 0.01940 0.00220 0.00312 -0.00052 C17 1 -0.088635 0.128980 -0.078022 11.00000 0.03490 0.02932 = 0.02065 0.00099 0.00858 -0.00237 C18 1 -0.083608 0.061721 -0.090412 11.00000 0.03687 0.03095 = 0.03703 -0.00293 0.00699 -0.00540 AFIX 43 H18 2 -0.150951 0.035442 -0.080972 11.00000 -1.20000 AFIX 0 C19 1 0.017106 0.033280 -0.115966 11.00000 0.04251 0.02214 = 0.03113 -0.00119 0.00710 0.00508 AFIX 43 H19 2 0.018986 -0.011970 -0.124277 11.00000 -1.20000 AFIX 0 C20 1 0.114186 0.071552 -0.129089 11.00000 0.02897 0.02600 = 0.02558 -0.00524 0.00574 0.00261 AFIX 43 H20 2 0.183368 0.052045 -0.146633 11.00000 -1.20000 AFIX 0 C21 1 0.114816 0.137876 -0.117604 11.00000 0.02453 0.02293 = 0.01237 -0.00160 0.00545 0.00386 C22 1 -0.201707 0.158255 -0.050837 11.00000 0.03392 0.03834 = 0.05608 -0.00359 0.02192 -0.00925 AFIX 13 H22 2 -0.187085 0.205832 -0.047096 11.00000 -1.20000 AFIX 0 C23 1 -0.327708 0.147287 -0.119394 11.00000 0.03639 0.05780 = 0.08668 -0.01810 0.01796 -0.00364 AFIX 137 H23A 2 -0.315455 0.160763 -0.174758 11.00000 -1.50000 H23B 2 -0.396171 0.172723 -0.105033 11.00000 -1.50000 H23C 2 -0.350329 0.101515 -0.121283 11.00000 -1.50000 AFIX 0 C24 1 -0.210787 0.136247 0.035746 11.00000 0.07246 0.06322 = 0.06065 -0.00573 0.05102 0.00452 AFIX 137 H24A 2 -0.205818 0.089141 0.038634 11.00000 -1.50000 H24B 2 -0.291873 0.150466 0.046823 11.00000 -1.50000 H24C 2 -0.140584 0.154797 0.078191 11.00000 -1.50000 AFIX 0 C25 1 0.225515 0.179142 -0.131270 11.00000 0.01784 0.01932 = 0.02723 -0.00614 -0.00319 -0.00122 AFIX 13 H25 2 0.195458 0.224771 -0.138931 11.00000 -1.20000 AFIX 0 C26 1 0.273759 0.159941 -0.209330 11.00000 0.03636 0.02565 = 0.02455 0.00100 0.01666 -0.00373 AFIX 137 H26A 2 0.309542 0.116399 -0.201601 11.00000 -1.50000 H26B 2 0.339561 0.190323 -0.217028 11.00000 -1.50000 H26C 2 0.203052 0.160813 -0.259324 11.00000 -1.50000 AFIX 0 C27 1 0.337155 0.176597 -0.053077 11.00000 0.02737 0.08000 = 0.03353 -0.01954 0.00740 -0.00676 AFIX 137 H27A 2 0.307770 0.190174 -0.003040 11.00000 -1.50000 H27B 2 0.404847 0.205525 -0.061445 11.00000 -1.50000 H27C 2 0.369885 0.132472 -0.044993 11.00000 -1.50000 AFIX 0 C28 1 0.242419 0.164425 0.212500 11.00000 0.03013 0.03174 = 0.02193 0.00528 -0.00070 0.01509 AFIX 13 H28 2 0.276170 0.196274 0.258293 11.00000 -1.20000 AFIX 0 C29 1 0.164965 0.119510 0.242869 11.00000 0.04912 0.01763 = 0.02985 -0.00097 0.00869 -0.00045 C30 1 0.355557 0.132211 0.185567 11.00000 0.04594 0.03302 = 0.02659 0.00204 0.00861 -0.00355 AFIX 23 H30A 2 0.324274 0.093075 0.152507 11.00000 -1.20000 H30B 2 0.387246 0.162092 0.147598 11.00000 -1.20000 AFIX 0 C31 1 0.516577 0.052417 0.241736 11.00000 0.05309 0.04911 = 0.03119 0.00886 0.01047 0.01818 AFIX 13 H31 2 0.602193 0.052079 0.281471 11.00000 -1.20000 AFIX 0 C32 1 0.537927 0.037871 0.153697 11.00000 0.06395 0.05566 = 0.05815 0.00595 0.02485 0.00985 AFIX 137 H32A 2 0.455853 0.036570 0.112751 11.00000 -1.50000 H32B 2 0.580448 -0.003885 0.154466 11.00000 -1.50000 H32C 2 0.591146 0.071618 0.137522 11.00000 -1.50000 AFIX 0 C33 1 0.439774 -0.000890 0.270381 11.00000 0.05716 0.03188 = 0.03405 0.00197 0.00820 0.00851 AFIX 137 H33A 2 0.435554 0.006658 0.329186 11.00000 -1.50000 H33B 2 0.480612 -0.042501 0.266058 11.00000 -1.50000 H33C 2 0.353615 -0.001213 0.234375 11.00000 -1.50000 AFIX 0 C34 1 0.546901 0.169520 0.280589 11.00000 0.04015 0.04563 = 0.04320 0.00222 0.00961 -0.00069 AFIX 13 H34 2 0.492313 0.208375 0.280808 11.00000 -1.20000 AFIX 0 C35 1 0.633064 0.184746 0.221865 11.00000 0.04894 0.06378 = 0.03972 0.01023 0.00833 -0.01905 AFIX 137 H35A 2 0.695855 0.150247 0.225050 11.00000 -1.50000 H35B 2 0.676908 0.225625 0.238696 11.00000 -1.50000 H35C 2 0.582272 0.188234 0.163791 11.00000 -1.50000 AFIX 0 C36 1 0.621580 0.160360 0.370498 11.00000 0.05261 0.07642 = 0.04112 0.00770 0.00897 -0.00737 AFIX 137 H36A 2 0.564808 0.165343 0.409209 11.00000 -1.50000 H36B 2 0.689350 0.192655 0.383749 11.00000 -1.50000 H36C 2 0.659017 0.117143 0.376848 11.00000 -1.50000 AFIX 0 N1 3 0.011626 0.233136 -0.077704 11.00000 0.02474 0.02125 = 0.01663 -0.00763 0.00618 0.00554 N2 3 0.036564 0.324464 -0.014526 11.00000 0.01817 0.01486 = 0.01145 -0.00243 0.00514 -0.00196 N3 3 0.097303 0.081908 0.265054 11.00000 0.07742 0.03464 = 0.04019 -0.00049 0.01889 -0.00670 N4 3 0.458871 0.114573 0.252378 11.00000 0.02185 0.04439 = 0.03091 0.00954 0.00383 0.00487 AU1 4 0.133462 0.214082 0.107549 11.00000 0.02209 0.02407 = 0.01620 0.00577 0.00266 0.00438 HKLF 5 REM npm038 in P2(1)/c REM R1 = 0.0618 for 7050 Fo > 4sig(Fo) and 0.0875 for all 8842 data REM 383 parameters refined using 0 restraints END WGHT 0.0585 83.3970 REM Highest difference peak 3.953, deepest hole -2.205, 1-sigma level 0.207 Q1 1 0.1039 0.1807 0.0839 11.00000 0.05 3.95 Q2 1 0.1294 0.3548 0.1029 11.00000 0.05 3.05 Q3 1 0.0868 0.2135 0.1327 11.00000 0.05 2.36 Q4 1 0.1889 0.2150 0.0779 11.00000 0.05 2.16 Q5 1 0.0980 0.2423 0.0958 11.00000 0.05 1.48 Q6 1 -0.0363 0.2083 0.1412 11.00000 0.05 1.22 Q7 1 0.1337 0.1156 0.1079 11.00000 0.05 1.21 Q8 1 0.1077 0.3015 0.1224 11.00000 0.05 1.11 Q9 1 -0.3678 0.2825 0.1626 11.00000 0.05 1.09 Q10 1 0.2952 0.2113 0.0654 11.00000 0.05 0.86 Q11 1 0.5816 0.3067 0.2007 11.00000 0.05 0.79 Q12 1 0.1519 0.3898 0.0594 11.00000 0.05 0.77 Q13 1 0.5583 0.2849 0.1849 11.00000 0.05 0.77 Q14 1 0.1234 0.2446 0.0218 11.00000 0.05 0.77 Q15 1 -0.1048 -0.0720 -0.1422 11.00000 0.05 0.75 Q16 1 0.0610 0.1136 0.2045 11.00000 0.05 0.73 Q17 1 0.1442 0.3134 0.0550 11.00000 0.05 0.71 Q18 1 0.2008 0.1298 0.1817 11.00000 0.05 0.71 Q19 1 0.1197 0.2624 0.1621 11.00000 0.05 0.71 Q20 1 0.2184 0.1586 0.0619 11.00000 0.05 0.70 Q21 1 0.1369 0.1742 0.0115 11.00000 0.05 0.70 Q22 1 0.1228 0.4981 0.1011 11.00000 0.05 0.68 Q23 1 0.0809 0.2636 0.1389 11.00000 0.05 0.68 Q24 1 -0.0591 0.2647 0.1367 11.00000 0.05 0.67 Q25 1 0.5877 0.2168 0.1734 11.00000 0.05 0.67 ; data_npm032 _database_code_depnum_ccdc_archive 'CCDC 901606' #TrackingRef 'web_deposit_cif_file_3_MilesW.Johnson_1352328108.IPrAuPMes2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common IPrAuPMes2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H58 Au N2 P' _chemical_formula_weight 854.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.8187(6) _cell_length_b 19.5498(8) _cell_length_c 28.0267(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8119.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9521 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 34.14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3456 _exptl_absorpt_coefficient_mu 3.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7089 _exptl_absorpt_correction_T_max 0.7089 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 280900 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 33.14 _reflns_number_total 15119 _reflns_number_gt 10640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0167P)^2^+42.7992P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15119 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0922 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.304010(8) 0.238182(7) 0.078820(4) 0.01650(4) Uani 1 1 d . . . P1 P 0.16779(6) 0.26100(5) 0.11635(3) 0.02081(17) Uani 1 1 d . . . C1 C 0.4247(2) 0.22992(16) 0.04411(11) 0.0165(6) Uani 1 1 d . . . C2 C 0.5353(2) 0.21418(19) -0.01107(12) 0.0204(6) Uani 1 1 d . . . H2 H 0.5644 0.2036 -0.0404 0.024 Uiso 1 1 calc R . . C3 C 0.5755(2) 0.23397(18) 0.02960(12) 0.0203(6) Uani 1 1 d . . . H3 H 0.6383 0.2409 0.0345 0.024 Uiso 1 1 calc R . . C4 C 0.5211(2) 0.27294(19) 0.10967(12) 0.0220(7) Uani 1 1 d . . . C5 C 0.5115(3) 0.3440(2) 0.11280(14) 0.0269(8) Uani 1 1 d . . . C6 C 0.5242(3) 0.3734(2) 0.15766(15) 0.0345(9) Uani 1 1 d . . . H6 H 0.5151 0.4212 0.1616 0.041 Uiso 1 1 calc R . . C7 C 0.5498(3) 0.3343(2) 0.19651(14) 0.0327(9) Uani 1 1 d . . . H7 H 0.5593 0.3555 0.2266 0.039 Uiso 1 1 calc R . . C8 C 0.5616(3) 0.2641(2) 0.19169(12) 0.0260(7) Uani 1 1 d . . . H8 H 0.5788 0.2377 0.2186 0.031 Uiso 1 1 calc R . . C9 C 0.5486(2) 0.23208(19) 0.14788(11) 0.0196(6) Uani 1 1 d . . . C10 C 0.4894(3) 0.3885(2) 0.07033(15) 0.0321(9) Uani 1 1 d . . . H10 H 0.4829 0.3577 0.0421 0.039 Uiso 1 1 calc R . . C11 C 0.5670(5) 0.4379(3) 0.0596(2) 0.070(2) Uani 1 1 d . . . H11A H 0.5544 0.4626 0.0299 0.106 Uiso 1 1 calc R . . H11B H 0.6233 0.4121 0.0561 0.106 Uiso 1 1 calc R . . H11C H 0.5731 0.4707 0.0859 0.106 Uiso 1 1 calc R . . C12 C 0.4011(4) 0.4263(3) 0.0763(2) 0.0573(16) Uani 1 1 d . . . H12A H 0.3521 0.3932 0.0808 0.086 Uiso 1 1 calc R . . H12B H 0.3892 0.4537 0.0477 0.086 Uiso 1 1 calc R . . H12C H 0.4047 0.4564 0.1041 0.086 Uiso 1 1 calc R . . C13 C 0.5614(2) 0.15536(18) 0.14162(13) 0.0213(7) Uani 1 1 d . . . H13 H 0.5842 0.1474 0.1085 0.026 Uiso 1 1 calc R . . C14 C 0.6302(3) 0.1244(2) 0.17623(14) 0.0283(8) Uani 1 1 d . . . H14A H 0.6867 0.1503 0.1745 0.042 Uiso 1 1 calc R . . H14B H 0.6415 0.0766 0.1676 0.042 Uiso 1 1 calc R . . H14C H 0.6063 0.1266 0.2088 0.042 Uiso 1 1 calc R . . C15 C 0.4706(3) 0.1188(2) 0.14627(14) 0.0260(7) Uani 1 1 d . . . H15A H 0.4446 0.1283 0.1777 0.039 Uiso 1 1 calc R . . H15B H 0.4795 0.0694 0.1427 0.039 Uiso 1 1 calc R . . H15C H 0.4294 0.1352 0.1214 0.039 Uiso 1 1 calc R . . C16 C 0.3771(2) 0.20184(18) -0.03976(11) 0.0173(6) Uani 1 1 d . . . C17 C 0.3372(2) 0.25968(19) -0.06028(12) 0.0196(6) Uani 1 1 d . . . C18 C 0.2789(2) 0.2482(2) -0.09855(13) 0.0249(8) Uani 1 1 d . . . H18 H 0.2508 0.2861 -0.1136 0.030 Uiso 1 1 calc R . . C19 C 0.2612(3) 0.1833(2) -0.11512(13) 0.0264(8) Uani 1 1 d . . . H19 H 0.2209 0.1770 -0.1411 0.032 Uiso 1 1 calc R . . C20 C 0.3019(3) 0.1274(2) -0.09402(13) 0.0238(7) Uani 1 1 d . . . H20 H 0.2894 0.0829 -0.1059 0.029 Uiso 1 1 calc R . . C21 C 0.3611(2) 0.13487(18) -0.05559(12) 0.0190(6) Uani 1 1 d . . . C22 C 0.3599(2) 0.33194(19) -0.04337(13) 0.0224(7) Uani 1 1 d . . . H22 H 0.3732 0.3285 -0.0085 0.027 Uiso 1 1 calc R . . C23 C 0.4453(4) 0.3593(3) -0.0671(2) 0.0444(12) Uani 1 1 d . . . H23A H 0.4937 0.3254 -0.0642 0.067 Uiso 1 1 calc R . . H23B H 0.4637 0.4019 -0.0515 0.067 Uiso 1 1 calc R . . H23C H 0.4333 0.3682 -0.1010 0.067 Uiso 1 1 calc R . . C24 C 0.2828(3) 0.3824(2) -0.0485(2) 0.0485(13) Uani 1 1 d . . . H24A H 0.3009 0.4268 -0.0354 0.073 Uiso 1 1 calc R . . H24B H 0.2299 0.3654 -0.0312 0.073 Uiso 1 1 calc R . . H24C H 0.2677 0.3877 -0.0824 0.073 Uiso 1 1 calc R . . C25 C 0.4040(3) 0.07312(18) -0.03154(13) 0.0218(7) Uani 1 1 d . . . H25 H 0.4659 0.0865 -0.0208 0.026 Uiso 1 1 calc R . . C26 C 0.4132(3) 0.0113(2) -0.06455(15) 0.0292(8) Uani 1 1 d . . . H26A H 0.3531 -0.0067 -0.0721 0.044 Uiso 1 1 calc R . . H26B H 0.4489 -0.0242 -0.0487 0.044 Uiso 1 1 calc R . . H26C H 0.4434 0.0252 -0.0941 0.044 Uiso 1 1 calc R . . C27 C 0.3490(3) 0.0534(2) 0.01276(14) 0.0315(9) Uani 1 1 d . . . H27A H 0.3472 0.0922 0.0349 0.047 Uiso 1 1 calc R . . H27B H 0.3772 0.0141 0.0285 0.047 Uiso 1 1 calc R . . H27C H 0.2874 0.0415 0.0032 0.047 Uiso 1 1 calc R . . C28 C 0.2042(2) 0.32032(19) 0.16410(12) 0.0210(7) Uani 1 1 d . . . C29 C 0.1863(3) 0.3904(2) 0.15837(13) 0.0261(8) Uani 1 1 d . . . C30 C 0.2110(3) 0.4371(2) 0.19378(15) 0.0309(8) Uani 1 1 d . . . H30 H 0.1976 0.4842 0.1894 0.037 Uiso 1 1 calc R . . C31 C 0.2547(3) 0.4164(2) 0.23516(14) 0.0308(8) Uani 1 1 d . . . C32 C 0.2737(3) 0.3472(2) 0.24041(13) 0.0283(8) Uani 1 1 d . . . H32 H 0.3036 0.3323 0.2685 0.034 Uiso 1 1 calc R . . C33 C 0.2504(2) 0.2988(2) 0.20604(12) 0.0235(7) Uani 1 1 d . . . C34 C 0.1394(3) 0.4171(2) 0.11408(15) 0.0368(10) Uani 1 1 d . . . H34A H 0.0807 0.3945 0.1106 0.055 Uiso 1 1 calc R . . H34B H 0.1766 0.4074 0.0860 0.055 Uiso 1 1 calc R . . H34C H 0.1305 0.4666 0.1170 0.055 Uiso 1 1 calc R . . C35 C 0.2813(4) 0.4669(3) 0.27337(18) 0.0475(12) Uani 1 1 d . . . H35A H 0.2811 0.5132 0.2600 0.071 Uiso 1 1 calc R . . H35B H 0.3418 0.4559 0.2851 0.071 Uiso 1 1 calc R . . H35C H 0.2380 0.4644 0.2998 0.071 Uiso 1 1 calc R . . C36 C 0.2774(3) 0.2257(2) 0.21406(15) 0.0324(9) Uani 1 1 d . . . H36A H 0.3186 0.2230 0.2413 0.049 Uiso 1 1 calc R . . H36B H 0.3076 0.2081 0.1855 0.049 Uiso 1 1 calc R . . H36C H 0.2235 0.1982 0.2206 0.049 Uiso 1 1 calc R . . C37 C 0.1128(2) 0.1907(2) 0.14964(13) 0.0246(7) Uani 1 1 d . . . C38 C 0.1364(3) 0.1209(2) 0.14686(13) 0.0265(8) Uani 1 1 d . . . C39 C 0.0885(3) 0.0727(3) 0.17347(15) 0.0363(10) Uani 1 1 d . . . H39 H 0.1069 0.0262 0.1720 0.044 Uiso 1 1 calc R . . C40 C 0.0156(3) 0.0896(3) 0.20184(16) 0.0440(13) Uani 1 1 d . . . C41 C -0.0104(3) 0.1574(3) 0.20232(16) 0.0433(12) Uani 1 1 d . . . H41 H -0.0614 0.1700 0.2209 0.052 Uiso 1 1 calc R . . C42 C 0.0348(3) 0.2085(3) 0.17671(14) 0.0335(10) Uani 1 1 d . . . C43 C 0.2106(3) 0.0953(2) 0.11536(17) 0.0354(10) Uani 1 1 d . . . H43A H 0.2678 0.1162 0.1251 0.053 Uiso 1 1 calc R . . H43B H 0.1975 0.1075 0.0822 0.053 Uiso 1 1 calc R . . H43C H 0.2150 0.0455 0.1182 0.053 Uiso 1 1 calc R . . C44 C -0.0347(5) 0.0360(3) 0.2300(2) 0.069(2) Uani 1 1 d . . . H44A H -0.0796 0.0140 0.2094 0.103 Uiso 1 1 calc R . . H44B H -0.0651 0.0576 0.2571 0.103 Uiso 1 1 calc R . . H44C H 0.0080 0.0016 0.2417 0.103 Uiso 1 1 calc R . . C45 C -0.0030(3) 0.2798(3) 0.17709(18) 0.0427(12) Uani 1 1 d . . . H45A H -0.0592 0.2805 0.1955 0.064 Uiso 1 1 calc R . . H45B H -0.0152 0.2945 0.1443 0.064 Uiso 1 1 calc R . . H45C H 0.0407 0.3110 0.1917 0.064 Uiso 1 1 calc R . . N1 N 0.50748(19) 0.24229(15) 0.06292(9) 0.0164(5) Uani 1 1 d . . . N2 N 0.44300(19) 0.21201(15) -0.00221(10) 0.0165(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01604(6) 0.02007(6) 0.01340(5) -0.00137(4) 0.00094(4) 0.00286(4) P1 0.0152(4) 0.0316(5) 0.0156(4) -0.0045(3) -0.0015(3) 0.0055(4) C1 0.0210(15) 0.0158(16) 0.0128(13) 0.0023(11) -0.0007(11) 0.0001(12) C2 0.0186(16) 0.0243(17) 0.0184(15) 0.0000(13) 0.0032(12) 0.0016(13) C3 0.0180(15) 0.0243(17) 0.0187(14) 0.0034(13) 0.0039(12) 0.0001(13) C4 0.0202(16) 0.028(2) 0.0183(15) -0.0001(13) -0.0023(12) 0.0023(13) C5 0.036(2) 0.0221(18) 0.0230(17) -0.0022(14) -0.0061(15) 0.0009(15) C6 0.047(3) 0.024(2) 0.033(2) -0.0096(16) -0.0083(19) 0.0053(18) C7 0.040(2) 0.037(2) 0.0213(17) -0.0093(16) -0.0032(16) 0.0029(18) C8 0.032(2) 0.0314(19) 0.0142(14) 0.0015(14) -0.0021(13) 0.0013(16) C9 0.0184(15) 0.0261(18) 0.0144(13) -0.0013(12) 0.0011(11) 0.0028(13) C10 0.042(2) 0.0200(18) 0.034(2) -0.0005(15) -0.0123(18) 0.0003(16) C11 0.081(4) 0.048(3) 0.082(4) 0.042(3) -0.048(4) -0.030(3) C12 0.075(4) 0.052(3) 0.045(3) -0.008(2) -0.019(3) 0.035(3) C13 0.0223(17) 0.0216(17) 0.0201(15) 0.0029(13) -0.0010(13) 0.0044(13) C14 0.029(2) 0.030(2) 0.0261(18) 0.0080(15) 0.0000(15) 0.0058(16) C15 0.0283(19) 0.0232(18) 0.0264(18) 0.0002(14) -0.0004(15) 0.0014(14) C16 0.0153(14) 0.0229(17) 0.0137(13) -0.0027(11) 0.0028(11) 0.0007(12) C17 0.0182(15) 0.0219(16) 0.0188(14) 0.0005(13) -0.0022(12) 0.0004(13) C18 0.0183(16) 0.035(2) 0.0212(16) 0.0056(14) 0.0027(13) -0.0003(14) C19 0.0214(18) 0.037(2) 0.0207(16) -0.0053(15) -0.0044(13) 0.0030(15) C20 0.0232(17) 0.0264(18) 0.0219(15) -0.0064(13) 0.0003(14) -0.0012(14) C21 0.0168(15) 0.0225(17) 0.0176(14) -0.0009(12) 0.0028(12) -0.0002(12) C22 0.0225(17) 0.0211(17) 0.0236(16) 0.0000(13) 0.0026(13) 0.0030(13) C23 0.044(3) 0.031(2) 0.058(3) -0.001(2) 0.012(2) -0.005(2) C24 0.038(3) 0.030(2) 0.078(4) -0.016(2) -0.015(2) 0.0101(19) C25 0.0231(17) 0.0193(17) 0.0229(16) -0.0013(13) 0.0010(13) -0.0007(13) C26 0.032(2) 0.0208(18) 0.034(2) -0.0053(15) 0.0029(16) 0.0007(15) C27 0.042(2) 0.028(2) 0.0246(18) 0.0041(15) 0.0065(17) -0.0027(17) C28 0.0148(15) 0.0315(19) 0.0167(14) -0.0039(13) -0.0003(12) 0.0049(13) C29 0.0260(19) 0.032(2) 0.0201(15) -0.0044(14) -0.0010(14) 0.0071(15) C30 0.034(2) 0.029(2) 0.0292(19) -0.0060(16) 0.0011(16) 0.0037(16) C31 0.030(2) 0.037(2) 0.0254(18) -0.0099(16) -0.0010(16) -0.0014(17) C32 0.0233(18) 0.042(2) 0.0191(16) -0.0027(15) -0.0045(13) 0.0008(16) C33 0.0185(16) 0.033(2) 0.0187(15) -0.0025(14) 0.0009(13) 0.0034(14) C34 0.047(3) 0.035(2) 0.028(2) 0.0000(17) -0.0079(18) 0.019(2) C35 0.054(3) 0.049(3) 0.040(3) -0.020(2) -0.008(2) -0.005(2) C36 0.034(2) 0.038(2) 0.0253(18) -0.0023(16) -0.0117(16) 0.0092(17) C37 0.0151(15) 0.040(2) 0.0187(15) -0.0081(14) 0.0011(12) -0.0021(14) C38 0.0186(17) 0.038(2) 0.0228(17) -0.0046(15) 0.0030(13) -0.0068(15) C39 0.038(2) 0.044(3) 0.0271(19) -0.0076(17) 0.0050(17) -0.018(2) C40 0.044(3) 0.060(3) 0.028(2) -0.017(2) 0.0117(19) -0.029(2) C41 0.028(2) 0.071(4) 0.031(2) -0.022(2) 0.0135(17) -0.017(2) C42 0.0212(19) 0.058(3) 0.0213(17) -0.0197(18) 0.0023(14) -0.0017(18) C43 0.032(2) 0.030(2) 0.044(2) -0.0051(18) 0.0122(18) -0.0052(17) C44 0.082(4) 0.073(4) 0.051(3) -0.035(3) 0.042(3) -0.050(4) C45 0.020(2) 0.065(3) 0.043(2) -0.018(2) 0.0041(17) 0.008(2) N1 0.0186(13) 0.0208(13) 0.0097(10) 0.0038(10) -0.0030(9) 0.0014(11) N2 0.0175(13) 0.0169(13) 0.0152(12) -0.0007(10) 0.0005(10) -0.0010(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.043(3) . ? Au1 P1 2.3195(9) . ? P1 C28 1.851(4) . ? P1 C37 1.851(4) . ? C1 N1 1.356(4) . ? C1 N2 1.372(4) . ? C2 C3 1.343(5) . ? C2 N2 1.390(4) . ? C2 H2 0.9500 . ? C3 N1 1.384(4) . ? C3 H3 0.9500 . ? C4 C9 1.397(5) . ? C4 C5 1.400(5) . ? C4 N1 1.455(4) . ? C5 C6 1.395(5) . ? C5 C10 1.510(5) . ? C6 C7 1.384(6) . ? C6 H6 0.9500 . ? C7 C8 1.389(6) . ? C7 H7 0.9500 . ? C8 C9 1.392(5) . ? C8 H8 0.9500 . ? C9 C13 1.522(5) . ? C10 C12 1.512(7) . ? C10 C11 1.532(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.531(5) . ? C13 C15 1.530(5) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.400(5) . ? C16 C21 1.403(5) . ? C16 N2 1.449(4) . ? C17 C18 1.395(5) . ? C17 C22 1.528(5) . ? C18 C19 1.375(6) . ? C18 H18 0.9500 . ? C19 C20 1.382(6) . ? C19 H19 0.9500 . ? C20 C21 1.397(5) . ? C20 H20 0.9500 . ? C21 C25 1.522(5) . ? C22 C24 1.516(6) . ? C22 C23 1.527(6) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.528(5) . ? C25 C27 1.535(5) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.404(5) . ? C28 C33 1.424(5) . ? C29 C30 1.398(5) . ? C29 C34 1.515(5) . ? C30 C31 1.389(6) . ? C30 H30 0.9500 . ? C31 C32 1.389(6) . ? C31 C35 1.509(6) . ? C32 C33 1.394(5) . ? C32 H32 0.9500 . ? C33 C36 1.501(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.411(6) . ? C37 C42 1.426(5) . ? C38 C39 1.395(6) . ? C38 C43 1.496(6) . ? C39 C40 1.382(6) . ? C39 H39 0.9500 . ? C40 C41 1.381(8) . ? C40 C44 1.508(7) . ? C41 C42 1.400(7) . ? C41 H41 0.9500 . ? C42 C45 1.504(7) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Au1 P1 173.37(9) . . ? C28 P1 C37 103.26(16) . . ? C28 P1 Au1 101.22(11) . . ? C37 P1 Au1 117.98(13) . . ? N1 C1 N2 103.6(3) . . ? N1 C1 Au1 126.3(2) . . ? N2 C1 Au1 130.1(2) . . ? C3 C2 N2 107.1(3) . . ? C3 C2 H2 126.5 . . ? N2 C2 H2 126.5 . . ? C2 C3 N1 106.4(3) . . ? C2 C3 H3 126.8 . . ? N1 C3 H3 126.8 . . ? C9 C4 C5 123.3(3) . . ? C9 C4 N1 119.7(3) . . ? C5 C4 N1 116.8(3) . . ? C6 C5 C4 116.9(4) . . ? C6 C5 C10 120.1(4) . . ? C4 C5 C10 123.0(3) . . ? C7 C6 C5 121.2(4) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 120.3(4) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C7 C8 C9 120.8(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C4 117.3(3) . . ? C8 C9 C13 121.9(3) . . ? C4 C9 C13 120.8(3) . . ? C12 C10 C5 112.5(4) . . ? C12 C10 C11 111.4(5) . . ? C5 C10 C11 110.8(4) . . ? C12 C10 H10 107.3 . . ? C5 C10 H10 107.3 . . ? C11 C10 H10 107.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 113.5(3) . . ? C9 C13 C15 109.9(3) . . ? C14 C13 C15 110.3(3) . . ? C9 C13 H13 107.6 . . ? C14 C13 H13 107.6 . . ? C15 C13 H13 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.5(3) . . ? C17 C16 N2 118.2(3) . . ? C21 C16 N2 118.1(3) . . ? C18 C17 C16 116.6(3) . . ? C18 C17 C22 121.6(3) . . ? C16 C17 C22 121.8(3) . . ? C19 C18 C17 121.8(4) . . ? C19 C18 H18 119.1 . . ? C17 C18 H18 119.1 . . ? C18 C19 C20 120.1(3) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 121.4(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 116.6(3) . . ? C20 C21 C25 121.4(3) . . ? C16 C21 C25 122.0(3) . . ? C24 C22 C17 114.0(3) . . ? C24 C22 C23 110.8(4) . . ? C17 C22 C23 111.8(3) . . ? C24 C22 H22 106.6 . . ? C17 C22 H22 106.6 . . ? C23 C22 H22 106.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 113.3(3) . . ? C21 C25 C27 109.6(3) . . ? C26 C25 C27 109.8(3) . . ? C21 C25 H25 108.0 . . ? C26 C25 H25 108.0 . . ? C27 C25 H25 108.0 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 118.3(3) . . ? C29 C28 P1 118.2(3) . . ? C33 C28 P1 123.5(3) . . ? C30 C29 C28 120.4(4) . . ? C30 C29 C34 118.5(4) . . ? C28 C29 C34 121.1(3) . . ? C31 C30 C29 121.6(4) . . ? C31 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C32 C31 C30 117.8(4) . . ? C32 C31 C35 120.6(4) . . ? C30 C31 C35 121.5(4) . . ? C31 C32 C33 122.6(4) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C32 C33 C28 119.2(4) . . ? C32 C33 C36 118.5(3) . . ? C28 C33 C36 122.2(3) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C42 117.8(4) . . ? C38 C37 P1 125.5(3) . . ? C42 C37 P1 116.4(3) . . ? C39 C38 C37 119.8(4) . . ? C39 C38 C43 117.6(4) . . ? C37 C38 C43 122.6(4) . . ? C40 C39 C38 122.9(5) . . ? C40 C39 H39 118.5 . . ? C38 C39 H39 118.5 . . ? C39 C40 C41 117.0(4) . . ? C39 C40 C44 121.4(5) . . ? C41 C40 C44 121.6(5) . . ? C40 C41 C42 123.1(4) . . ? C40 C41 H41 118.5 . . ? C42 C41 H41 118.5 . . ? C41 C42 C37 119.1(4) . . ? C41 C42 C45 118.7(4) . . ? C37 C42 C45 122.2(4) . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C1 N1 C3 112.0(3) . . ? C1 N1 C4 123.3(3) . . ? C3 N1 C4 123.7(3) . . ? C1 N2 C2 110.8(3) . . ? C1 N2 C16 126.1(3) . . ? C2 N2 C16 122.5(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 33.14 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 5.832 _refine_diff_density_min -2.610 _refine_diff_density_rms 0.161 data_npm041 _database_code_depnum_ccdc_archive 'CCDC 901607' #TrackingRef 'web_deposit_cif_file_2_MilesW.Johnson_1352328108.npm041.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; npm041 ; _chemical_name_common npm041 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H59 Au B F4 N2 P' _chemical_formula_weight 942.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 11.8034(6) _cell_length_b 8.9229(4) _cell_length_c 50.327(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.9920(10) _cell_angle_gamma 90.00 _cell_volume 5293.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9719 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 2.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3299 _exptl_absorpt_correction_T_max 0.4353 _exptl_absorpt_process_details SADABS loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.750 -0.039 0.250 432 177 DCM 2 0.250 -0.001 0.750 433 176 DCM 3 1.000 0.500 0.500 152 73 DCM 4 0.500 0.500 1.000 152 73 DCM _platon_squeeze_details ; ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 87063 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -60 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.36 _reflns_number_total 9669 _reflns_number_gt 9319 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+59.6314P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9669 _refine_ls_number_parameters 490 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1190 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.237 _refine_ls_restrained_S_all 1.237 _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 C1 C 0.3777(5) 0.3069(6) 0.35508(12) 0.0122(12) Uani 1 1 d U . . C2 C 0.2497(6) 0.1487(8) 0.33775(15) 0.0272(16) Uani 1 1 d . . . H2 H 0.1855 0.0846 0.3359 0.033 Uiso 1 1 calc R . . C3 C 0.3214(6) 0.1823(9) 0.31865(15) 0.0292(16) Uani 1 1 d . . . H3 H 0.3185 0.1459 0.3009 0.035 Uiso 1 1 calc R . . C4 C 0.4954(6) 0.3471(8) 0.31721(13) 0.0252(15) Uani 1 1 d . . . C5 C 0.4824(7) 0.4886(9) 0.30684(14) 0.0303(17) Uani 1 1 d . . . C6 C 0.5777(8) 0.5495(10) 0.29488(16) 0.042(2) Uani 1 1 d . . . H6 H 0.5725 0.6463 0.2871 0.050 Uiso 1 1 calc R . . C7 C 0.6766(8) 0.4721(10) 0.29435(18) 0.047(2) Uani 1 1 d . . . H7 H 0.7399 0.5164 0.2865 0.057 Uiso 1 1 calc R . . C8 C 0.6867(8) 0.3295(10) 0.30514(19) 0.046(2) Uani 1 1 d . . . H8 H 0.7566 0.2772 0.3046 0.056 Uiso 1 1 calc R . . C9 C 0.5950(7) 0.2623(9) 0.31680(17) 0.0366(19) Uani 1 1 d . . . C10 C 0.3726(7) 0.5793(10) 0.30754(16) 0.040(2) Uani 1 1 d . . . H10 H 0.3197 0.5213 0.3185 0.048 Uiso 1 1 calc R . . C11 C 0.3160(11) 0.5942(15) 0.2800(2) 0.077(4) Uani 1 1 d . . . H11A H 0.2439 0.6476 0.2811 0.115 Uiso 1 1 calc R . . H11B H 0.3018 0.4942 0.2725 0.115 Uiso 1 1 calc R . . H11C H 0.3657 0.6503 0.2686 0.115 Uiso 1 1 calc R . . C12 C 0.3881(9) 0.7348(12) 0.3206(2) 0.059(3) Uani 1 1 d . . . H12A H 0.4265 0.7237 0.3382 0.088 Uiso 1 1 calc R . . H12B H 0.3136 0.7813 0.3224 0.088 Uiso 1 1 calc R . . H12C H 0.4339 0.7984 0.3095 0.088 Uiso 1 1 calc R . . C13 C 0.6068(7) 0.1075(9) 0.32940(18) 0.040(2) Uani 1 1 d . . . H13 H 0.5286 0.0715 0.3328 0.048 Uiso 1 1 calc R . . C14 C 0.6588(10) -0.0054(12) 0.3110(3) 0.073(4) Uani 1 1 d . . . H14A H 0.6158 -0.0057 0.2938 0.110 Uiso 1 1 calc R . . H14B H 0.6565 -0.1055 0.3189 0.110 Uiso 1 1 calc R . . H14C H 0.7378 0.0224 0.3083 0.110 Uiso 1 1 calc R . . C15 C 0.6732(9) 0.1168(12) 0.3566(2) 0.064(3) Uani 1 1 d . . . H15A H 0.7515 0.1475 0.3540 0.096 Uiso 1 1 calc R . . H15B H 0.6731 0.0184 0.3653 0.096 Uiso 1 1 calc R . . H15C H 0.6371 0.1905 0.3679 0.096 Uiso 1 1 calc R . . C16 C 0.2387(5) 0.2208(7) 0.38624(14) 0.0214(14) Uani 1 1 d . . . C17 C 0.1479(5) 0.3162(8) 0.39107(15) 0.0253(15) Uani 1 1 d . . . C18 C 0.1093(6) 0.3142(9) 0.41664(16) 0.0295(17) Uani 1 1 d . . . H18 H 0.0479 0.3776 0.4207 0.035 Uiso 1 1 calc R . . C19 C 0.1561(6) 0.2252(9) 0.43612(16) 0.0343(18) Uani 1 1 d . . . H19 H 0.1278 0.2270 0.4534 0.041 Uiso 1 1 calc R . . C20 C 0.2459(6) 0.1311(9) 0.43052(15) 0.0318(17) Uani 1 1 d . . . H20 H 0.2781 0.0686 0.4442 0.038 Uiso 1 1 calc R . . C21 C 0.2887(6) 0.1265(8) 0.40585(14) 0.0247(15) Uani 1 1 d . . . C22 C 0.0976(6) 0.4187(8) 0.36948(16) 0.0306(16) Uani 1 1 d . . . H22 H 0.1312 0.3889 0.3524 0.037 Uiso 1 1 calc R . . C23 C -0.0312(7) 0.4022(12) 0.3654(2) 0.053(3) Uani 1 1 d . . . H23A H -0.0499 0.2982 0.3607 0.079 Uiso 1 1 calc R . . H23B H -0.0592 0.4689 0.3511 0.079 Uiso 1 1 calc R . . H23C H -0.0670 0.4288 0.3819 0.079 Uiso 1 1 calc R . . C24 C 0.1321(8) 0.5831(11) 0.3751(3) 0.067(3) Uani 1 1 d . . . H24A H 0.1021 0.6155 0.3919 0.100 Uiso 1 1 calc R . . H24B H 0.1012 0.6470 0.3606 0.100 Uiso 1 1 calc R . . H24C H 0.2151 0.5911 0.3762 0.100 Uiso 1 1 calc R . . C25 C 0.3859(6) 0.0209(7) 0.39924(14) 0.0242(15) Uani 1 1 d . . . H25 H 0.4159 0.0537 0.3820 0.029 Uiso 1 1 calc R . . C26 C 0.3405(8) -0.1377(10) 0.3957(2) 0.049(2) Uani 1 1 d . . . H26A H 0.4016 -0.2040 0.3905 0.074 Uiso 1 1 calc R . . H26B H 0.2790 -0.1385 0.3819 0.074 Uiso 1 1 calc R . . H26C H 0.3116 -0.1727 0.4126 0.074 Uiso 1 1 calc R . . C27 C 0.4823(7) 0.0241(9) 0.42004(17) 0.0367(19) Uani 1 1 d . . . H27A H 0.5057 0.1281 0.4234 0.055 Uiso 1 1 calc R . . H27B H 0.5465 -0.0331 0.4137 0.055 Uiso 1 1 calc R . . H27C H 0.4575 -0.0206 0.4365 0.055 Uiso 1 1 calc R . . C28 C 0.5914(5) 0.4191(8) 0.44390(13) 0.0204(13) Uani 1 1 d . . . C29 C 0.6917(5) 0.3325(8) 0.44581(15) 0.0246(15) Uani 1 1 d . . . C30 C 0.7065(6) 0.2303(8) 0.46701(15) 0.0285(16) Uani 1 1 d . . . H30 H 0.7742 0.1726 0.4687 0.034 Uiso 1 1 calc R . . C31 C 0.6253(6) 0.2125(8) 0.48525(14) 0.0280(16) Uani 1 1 d . . . C32 C 0.5252(6) 0.2930(8) 0.48230(14) 0.0264(15) Uani 1 1 d . . . H32 H 0.4679 0.2775 0.4946 0.032 Uiso 1 1 calc R . . C33 C 0.5062(6) 0.3958(7) 0.46186(13) 0.0199(14) Uani 1 1 d . . . C34 C 0.7814(7) 0.3417(10) 0.42548(19) 0.044(2) Uani 1 1 d . . . H34A H 0.8405 0.2670 0.4297 0.066 Uiso 1 1 calc R . . H34B H 0.8151 0.4421 0.4259 0.066 Uiso 1 1 calc R . . H34C H 0.7466 0.3220 0.4077 0.066 Uiso 1 1 calc R . . C35 C 0.6445(7) 0.1052(9) 0.50824(16) 0.0354(18) Uani 1 1 d . . . H35A H 0.6874 0.0182 0.5024 0.053 Uiso 1 1 calc R . . H35B H 0.5712 0.0720 0.5144 0.053 Uiso 1 1 calc R . . H35C H 0.6874 0.1558 0.5228 0.053 Uiso 1 1 calc R . . C36 C 0.3941(5) 0.4780(9) 0.45953(15) 0.0273(16) Uani 1 1 d . . . H36A H 0.3425 0.4358 0.4722 0.041 Uiso 1 1 calc R . . H36B H 0.3606 0.4672 0.4414 0.041 Uiso 1 1 calc R . . H36C H 0.4066 0.5845 0.4635 0.041 Uiso 1 1 calc R . . C37 C 0.6898(5) 0.6691(7) 0.41189(14) 0.0217(14) Uani 1 1 d . . . C38 C 0.7376(5) 0.6805(7) 0.38679(14) 0.0210(14) Uani 1 1 d . . . C39 C 0.8309(6) 0.7756(8) 0.38414(15) 0.0262(16) Uani 1 1 d . . . H39 H 0.8619 0.7857 0.3672 0.031 Uiso 1 1 calc R . . C40 C 0.8783(6) 0.8539(9) 0.40508(18) 0.0370(19) Uani 1 1 d . . . C41 C 0.8295(6) 0.8452(8) 0.42965(17) 0.0341(18) Uani 1 1 d . . . H41 H 0.8603 0.9036 0.4441 0.041 Uiso 1 1 calc R . . C42 C 0.7364(6) 0.7530(8) 0.43362(16) 0.0269(16) Uani 1 1 d . . . C43 C 0.6936(6) 0.5967(8) 0.36240(14) 0.0267(16) Uani 1 1 d . . . H43A H 0.7375 0.6251 0.3472 0.040 Uiso 1 1 calc R . . H43B H 0.6135 0.6218 0.3586 0.040 Uiso 1 1 calc R . . H43C H 0.7009 0.4887 0.3655 0.040 Uiso 1 1 calc R . . C44 C 0.9783(8) 0.9560(11) 0.4013(2) 0.058(3) Uani 1 1 d . . . H44A H 1.0241 0.9158 0.3873 0.088 Uiso 1 1 calc R . . H44B H 1.0247 0.9624 0.4180 0.088 Uiso 1 1 calc R . . H44C H 0.9509 1.0562 0.3962 0.088 Uiso 1 1 calc R . . C45 C 0.6891(7) 0.7501(9) 0.46088(16) 0.0380(19) Uani 1 1 d . . . H45A H 0.7315 0.8205 0.4726 0.057 Uiso 1 1 calc R . . H45B H 0.6961 0.6487 0.4683 0.057 Uiso 1 1 calc R . . H45C H 0.6089 0.7791 0.4595 0.057 Uiso 1 1 calc R . . B1 B 0.2715(16) 0.0293(18) 0.2518(5) 0.035(5) Uiso 0.50 1 d P . . B2 B 0.0126(12) 0.962(2) 0.4941(2) 0.069(7) Uiso 0.50 1 d PD . . N1 N 0.4003(5) 0.2809(6) 0.33021(11) 0.0225(12) Uani 1 1 d . . . N2 N 0.2865(4) 0.2244(6) 0.36040(11) 0.0212(12) Uani 1 1 d . . . F1 F 0.2178(8) -0.0302(10) 0.27190(18) 0.075(2) Uiso 0.75 1 d P . . F2 F 0.2500 0.1813(10) 0.2500 0.059(2) Uiso 1 2 d S . . F3 F 0.3780(9) 0.0074(12) 0.2619(2) 0.094(3) Uiso 0.75 1 d P . . F4 F 0.0412(9) 0.9264(13) 0.5196(2) 0.082(3) Uiso 0.67 1 d PD . . F5 F -0.0957(12) 0.9252(19) 0.4992(3) 0.134(5) Uiso 0.67 1 d PD . . F6 F 0.0708(11) 0.8780(15) 0.4770(3) 0.106(4) Uiso 0.67 1 d PD . . P1 P 0.56655(13) 0.55219(19) 0.41708(3) 0.0192(3) Uani 1 1 d . . . H1 H 0.5097 0.6234 0.4240 0.023 Uiso 1 1 calc R . . Au1 Au 0.46983(2) 0.43243(3) 0.382977(5) 0.01908(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.010(2) 0.006(2) 0.021(3) 0.004(2) 0.000(2) 0.004(2) C2 0.019(3) 0.025(4) 0.036(4) -0.005(3) -0.008(3) -0.001(3) C3 0.030(4) 0.029(4) 0.029(4) -0.008(3) -0.005(3) -0.001(3) C4 0.030(4) 0.027(4) 0.019(3) -0.001(3) 0.007(3) -0.004(3) C5 0.043(4) 0.031(4) 0.018(3) -0.001(3) 0.006(3) -0.001(3) C6 0.061(6) 0.030(4) 0.036(4) 0.006(4) 0.019(4) -0.008(4) C7 0.053(6) 0.040(5) 0.052(5) -0.009(4) 0.031(4) -0.013(4) C8 0.042(5) 0.033(5) 0.067(6) -0.005(4) 0.027(4) 0.003(4) C9 0.036(4) 0.033(4) 0.042(5) -0.002(4) 0.015(4) 0.004(4) C10 0.047(5) 0.038(5) 0.035(4) 0.015(4) -0.003(4) 0.008(4) C11 0.091(9) 0.079(9) 0.056(7) -0.006(6) -0.032(6) 0.034(7) C12 0.054(6) 0.053(6) 0.067(7) -0.014(5) -0.011(5) 0.026(5) C13 0.034(4) 0.024(4) 0.062(6) -0.003(4) 0.012(4) 0.002(3) C14 0.061(7) 0.037(5) 0.125(11) -0.007(6) 0.029(7) 0.009(5) C15 0.057(6) 0.041(6) 0.092(8) 0.016(6) -0.006(6) 0.010(5) C16 0.015(3) 0.017(3) 0.033(4) -0.001(3) 0.005(3) -0.009(3) C17 0.009(3) 0.020(3) 0.046(4) -0.004(3) 0.000(3) -0.005(3) C18 0.016(3) 0.026(4) 0.047(5) -0.005(3) 0.006(3) -0.007(3) C19 0.032(4) 0.039(5) 0.033(4) -0.010(4) 0.009(3) -0.018(4) C20 0.031(4) 0.032(4) 0.032(4) 0.003(3) -0.006(3) -0.005(3) C21 0.022(3) 0.021(3) 0.030(4) 0.002(3) 0.000(3) -0.007(3) C22 0.022(3) 0.022(4) 0.048(5) 0.010(4) -0.001(3) 0.001(3) C23 0.023(4) 0.068(7) 0.067(6) 0.015(5) -0.002(4) -0.003(4) C24 0.045(5) 0.032(5) 0.120(10) 0.005(6) -0.020(6) 0.002(4) C25 0.030(4) 0.014(3) 0.028(4) 0.003(3) -0.005(3) 0.003(3) C26 0.041(5) 0.028(4) 0.075(7) -0.006(4) -0.027(5) 0.004(4) C27 0.030(4) 0.026(4) 0.053(5) -0.003(4) -0.005(4) 0.002(3) C28 0.017(3) 0.022(3) 0.022(3) 0.001(3) -0.004(2) 0.000(3) C29 0.013(3) 0.021(3) 0.040(4) 0.004(3) 0.000(3) 0.000(3) C30 0.019(3) 0.026(4) 0.040(4) 0.005(3) -0.008(3) 0.006(3) C31 0.030(4) 0.023(4) 0.030(4) -0.001(3) -0.007(3) -0.007(3) C32 0.023(4) 0.028(4) 0.027(4) 0.001(3) 0.000(3) -0.003(3) C33 0.024(3) 0.013(3) 0.022(3) -0.007(3) -0.005(3) -0.002(3) C34 0.025(4) 0.037(5) 0.073(6) 0.023(4) 0.018(4) 0.020(4) C35 0.042(5) 0.027(4) 0.037(4) 0.007(3) -0.006(3) -0.003(3) C36 0.014(3) 0.034(4) 0.034(4) 0.002(3) 0.006(3) 0.006(3) C37 0.014(3) 0.013(3) 0.038(4) 0.001(3) -0.002(3) 0.002(3) C38 0.013(3) 0.013(3) 0.037(4) 0.005(3) -0.004(3) 0.005(2) C39 0.019(3) 0.020(3) 0.040(4) 0.003(3) 0.004(3) -0.003(3) C40 0.024(4) 0.022(4) 0.066(6) -0.005(4) 0.005(4) -0.005(3) C41 0.025(4) 0.023(4) 0.054(5) -0.013(4) -0.006(3) -0.008(3) C42 0.018(3) 0.015(3) 0.048(5) -0.003(3) -0.005(3) 0.004(3) C43 0.022(3) 0.028(4) 0.030(4) 0.005(3) 0.003(3) -0.006(3) C44 0.035(5) 0.040(5) 0.101(8) -0.012(5) 0.012(5) -0.025(4) C45 0.037(4) 0.034(4) 0.042(5) -0.014(4) -0.007(4) -0.007(4) N1 0.022(3) 0.019(3) 0.027(3) 0.002(2) 0.002(2) -0.002(2) N2 0.016(3) 0.018(3) 0.029(3) -0.001(2) -0.002(2) 0.001(2) P1 0.0150(8) 0.0165(8) 0.0260(9) 0.0018(7) -0.0002(6) 0.0025(7) Au1 0.01404(12) 0.01981(13) 0.02324(13) 0.00242(11) -0.00040(9) -0.00097(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.314(8) . ? C1 N2 1.343(8) . ? C1 Au1 2.061(6) . ? C2 C3 1.347(11) . ? C2 N2 1.376(9) . ? C2 H2 0.9500 . ? C3 N1 1.387(9) . ? C3 H3 0.9500 . ? C4 C5 1.372(10) . ? C4 C9 1.400(11) . ? C4 N1 1.454(9) . ? C5 C6 1.411(11) . ? C5 C10 1.530(11) . ? C6 C7 1.358(13) . ? C6 H6 0.9500 . ? C7 C8 1.386(13) . ? C7 H7 0.9500 . ? C8 C9 1.393(11) . ? C8 H8 0.9500 . ? C9 C13 1.523(11) . ? C10 C11 1.512(12) . ? C10 C12 1.542(13) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.520(13) . ? C13 C15 1.544(14) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.399(9) . ? C16 C21 1.404(10) . ? C16 N2 1.445(9) . ? C17 C18 1.388(10) . ? C17 C22 1.518(10) . ? C18 C19 1.357(11) . ? C18 H18 0.9500 . ? C19 C20 1.392(11) . ? C19 H19 0.9500 . ? C20 C21 1.365(10) . ? C20 H20 0.9500 . ? C21 C25 1.535(10) . ? C22 C23 1.530(10) . ? C22 C24 1.544(12) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.505(10) . ? C25 C26 1.520(10) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.402(9) . ? C28 C29 1.413(9) . ? C28 P1 1.811(7) . ? C29 C30 1.408(10) . ? C29 C34 1.512(10) . ? C30 C31 1.371(11) . ? C30 H30 0.9500 . ? C31 C32 1.384(10) . ? C31 C35 1.510(10) . ? C32 C33 1.387(10) . ? C32 H32 0.9500 . ? C33 C36 1.512(9) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C42 1.412(10) . ? C37 C38 1.414(10) . ? C37 P1 1.820(7) . ? C38 C39 1.401(9) . ? C38 C43 1.507(10) . ? C39 C40 1.360(11) . ? C39 H39 0.9500 . ? C40 C41 1.393(12) . ? C40 C44 1.511(10) . ? C41 C42 1.396(10) . ? C41 H41 0.9500 . ? C42 C45 1.508(11) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? B1 B1 0.53(4) 2 ? B1 F1 1.32(2) 2 ? B1 F1 1.33(2) . ? B1 F3 1.35(2) . ? B1 F2 1.382(18) . ? B1 F3 1.87(2) 2 ? B2 B2 0.96(3) 3_576 ? B2 F4 1.35(2) 3_576 ? B2 F4 1.350(5) . ? B2 F6 1.355(5) . ? B2 F5 1.358(5) . ? B2 F5 1.43(3) 3_576 ? F1 B1 1.32(2) 2 ? F2 B1 1.382(18) 2 ? F3 B1 1.87(2) 2 ? F4 B2 1.35(2) 3_576 ? F4 F5 1.769(18) 3_576 ? F5 B2 1.43(3) 3_576 ? F5 F4 1.769(18) 3_576 ? P1 Au1 2.2771(17) . ? P1 H1 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 107.3(5) . . ? N1 C1 Au1 128.2(4) . . ? N2 C1 Au1 124.2(4) . . ? C3 C2 N2 107.4(6) . . ? C3 C2 H2 126.3 . . ? N2 C2 H2 126.3 . . ? C2 C3 N1 106.0(6) . . ? C2 C3 H3 127.0 . . ? N1 C3 H3 127.0 . . ? C5 C4 C9 124.7(7) . . ? C5 C4 N1 118.1(7) . . ? C9 C4 N1 117.1(7) . . ? C4 C5 C6 116.1(7) . . ? C4 C5 C10 123.8(7) . . ? C6 C5 C10 120.1(7) . . ? C7 C6 C5 121.2(8) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 121.0(8) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C7 C8 C9 120.5(8) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C4 116.4(8) . . ? C8 C9 C13 120.7(7) . . ? C4 C9 C13 122.9(7) . . ? C11 C10 C5 111.1(8) . . ? C11 C10 C12 110.4(8) . . ? C5 C10 C12 113.8(7) . . ? C11 C10 H10 107.1 . . ? C5 C10 H10 107.1 . . ? C12 C10 H10 107.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C9 112.2(8) . . ? C14 C13 C15 112.0(9) . . ? C9 C13 C15 110.6(7) . . ? C14 C13 H13 107.3 . . ? C9 C13 H13 107.3 . . ? C15 C13 H13 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 122.7(7) . . ? C17 C16 N2 118.8(6) . . ? C21 C16 N2 118.4(6) . . ? C18 C17 C16 116.4(7) . . ? C18 C17 C22 122.4(6) . . ? C16 C17 C22 121.1(7) . . ? C19 C18 C17 122.4(7) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C19 C20 119.5(7) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C21 C20 C19 121.6(7) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C16 117.3(7) . . ? C20 C21 C25 122.1(7) . . ? C16 C21 C25 120.5(6) . . ? C17 C22 C23 112.7(6) . . ? C17 C22 C24 110.7(7) . . ? C23 C22 C24 111.5(7) . . ? C17 C22 H22 107.2 . . ? C23 C22 H22 107.2 . . ? C24 C22 H22 107.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 110.3(6) . . ? C27 C25 C21 112.6(6) . . ? C26 C25 C21 109.5(6) . . ? C27 C25 H25 108.1 . . ? C26 C25 H25 108.1 . . ? C21 C25 H25 108.1 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 120.1(6) . . ? C33 C28 P1 118.9(5) . . ? C29 C28 P1 120.8(5) . . ? C30 C29 C28 118.4(6) . . ? C30 C29 C34 119.0(6) . . ? C28 C29 C34 122.5(6) . . ? C31 C30 C29 121.3(6) . . ? C31 C30 H30 119.4 . . ? C29 C30 H30 119.4 . . ? C30 C31 C32 119.4(7) . . ? C30 C31 C35 120.3(7) . . ? C32 C31 C35 120.3(7) . . ? C31 C32 C33 121.8(7) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C32 C33 C28 118.8(6) . . ? C32 C33 C36 119.0(6) . . ? C28 C33 C36 122.2(6) . . ? C29 C34 H34A 109.5 . . ? C29 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C29 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 H35A 109.5 . . ? C31 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C31 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C42 C37 C38 119.7(6) . . ? C42 C37 P1 118.3(5) . . ? C38 C37 P1 121.9(5) . . ? C39 C38 C37 118.7(6) . . ? C39 C38 C43 117.5(6) . . ? C37 C38 C43 123.7(6) . . ? C40 C39 C38 122.0(7) . . ? C40 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? C39 C40 C41 119.1(7) . . ? C39 C40 C44 120.4(8) . . ? C41 C40 C44 120.4(8) . . ? C40 C41 C42 121.6(7) . . ? C40 C41 H41 119.2 . . ? C42 C41 H41 119.2 . . ? C41 C42 C37 118.6(7) . . ? C41 C42 C45 118.2(7) . . ? C37 C42 C45 123.2(6) . . ? C38 C43 H43A 109.5 . . ? C38 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C38 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C40 C44 H44A 109.5 . . ? C40 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C40 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? B1 B1 F1 80(5) 2 2 ? B1 B1 F1 77(5) 2 . ? F1 B1 F1 126.8(15) 2 . ? B1 B1 F3 171(2) 2 . ? F1 B1 F3 98.7(15) 2 . ? F1 B1 F3 97.3(15) . . ? B1 B1 F2 78.9(7) 2 . ? F1 B1 F2 111.2(16) 2 . ? F1 B1 F2 110.4(15) . . ? F3 B1 F2 109.4(13) . . ? B1 B1 F3 6.2(16) 2 2 ? F1 B1 F3 75.9(10) 2 2 ? F1 B1 F3 76.2(10) . 2 ? F3 B1 F3 165.6(14) . 2 ? F2 B1 F3 85.0(9) . 2 ? B2 B2 F4 69.2(15) 3_576 3_576 ? B2 B2 F4 69.2(13) 3_576 . ? F4 B2 F4 138.4(12) 3_576 . ? B2 B2 F6 166(3) 3_576 . ? F4 B2 F6 108.9(12) 3_576 . ? F4 B2 F6 111.3(12) . . ? B2 B2 F5 74.1(18) 3_576 . ? F4 B2 F5 81.6(11) 3_576 . ? F4 B2 F5 87.3(10) . . ? F6 B2 F5 120.0(16) . . ? B2 B2 F5 65.8(17) 3_576 3_576 ? F4 B2 F5 84.3(12) 3_576 3_576 ? F4 B2 F5 78.9(10) . 3_576 ? F6 B2 F5 100.1(14) . 3_576 ? F5 B2 F5 139.9(12) . 3_576 ? C1 N1 C3 110.3(6) . . ? C1 N1 C4 123.8(6) . . ? C3 N1 C4 125.9(6) . . ? C1 N2 C2 109.0(6) . . ? C1 N2 C16 123.1(5) . . ? C2 N2 C16 127.8(6) . . ? B1 F1 B1 23.1(15) 2 . ? B1 F2 B1 22.1(15) 2 . ? B1 F3 B1 2.4(6) . 2 ? B2 F4 B2 41.6(12) 3_576 . ? B2 F4 F5 49.4(6) 3_576 3_576 ? B2 F4 F5 52.6(11) . 3_576 ? B2 F5 B2 40.1(12) . 3_576 ? B2 F5 F4 49.0(9) . 3_576 ? B2 F5 F4 48.5(6) 3_576 3_576 ? C28 P1 C37 112.5(3) . . ? C28 P1 Au1 108.0(2) . . ? C37 P1 Au1 122.3(2) . . ? C28 P1 H1 104.0 . . ? C37 P1 H1 104.0 . . ? Au1 P1 H1 104.0 . . ? C1 Au1 P1 173.82(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.813 _refine_diff_density_min -3.059 _refine_diff_density_rms 0.146 _iucr_refine_instructions_details ; TITL npm041 in P2/n CELL 0.71073 11.8034 8.9229 50.3272 90.000 92.992 90.000 ZERR 4.00 0.0006 0.0004 0.0025 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, Y, 1/2 - Z SFAC C H B N F P AU UNIT 180 236 4 8 16 4 4 MERG 2 TWIN 0.00 1.00 0.00 1.00 0.00 0.00 0.00 0.00 -1.00 2 ISOR 0.005 C1 DFIX 1.350 0.005 B2 F4 DFIX 1.350 0.005 B2 F5 DFIX 1.350 0.005 B2 F6 FMAP 2 PLAN 10 SIZE 0.35 0.50 0.50 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.017000 59.631400 BASF 0.01115 FVAR 0.53260 0.92107 0.92463 0.47407 C1 1 0.377735 0.306929 0.355084 11.00000 0.00950 0.00557 = 0.02138 0.00427 0.00001 0.00439 C2 1 0.249658 0.148701 0.337746 11.00000 0.01935 0.02497 = 0.03644 -0.00517 -0.00794 -0.00079 AFIX 43 H2 2 0.185481 0.084568 0.335911 11.00000 -1.20000 AFIX 0 C3 1 0.321358 0.182309 0.318648 11.00000 0.02974 0.02857 = 0.02854 -0.00846 -0.00454 -0.00078 AFIX 43 H3 2 0.318468 0.145903 0.300887 11.00000 -1.20000 AFIX 0 C4 1 0.495413 0.347114 0.317207 11.00000 0.03000 0.02713 = 0.01918 -0.00091 0.00695 -0.00431 C5 1 0.482419 0.488648 0.306838 11.00000 0.04250 0.03120 = 0.01763 -0.00069 0.00561 -0.00060 C6 1 0.577671 0.549510 0.294876 11.00000 0.06093 0.02960 = 0.03594 0.00643 0.01934 -0.00841 AFIX 43 H6 2 0.572488 0.646331 0.287055 11.00000 -1.20000 AFIX 0 C7 1 0.676613 0.472109 0.294347 11.00000 0.05300 0.03989 = 0.05207 -0.00915 0.03066 -0.01310 AFIX 43 H7 2 0.739892 0.516393 0.286460 11.00000 -1.20000 AFIX 0 C8 1 0.686690 0.329480 0.305138 11.00000 0.04188 0.03325 = 0.06682 -0.00505 0.02677 0.00274 AFIX 43 H8 2 0.756627 0.277177 0.304573 11.00000 -1.20000 AFIX 0 C9 1 0.595043 0.262268 0.316804 11.00000 0.03613 0.03278 = 0.04221 -0.00184 0.01476 0.00364 C10 1 0.372591 0.579327 0.307543 11.00000 0.04748 0.03755 = 0.03542 0.01509 -0.00326 0.00817 AFIX 13 H10 2 0.319684 0.521318 0.318535 11.00000 -1.20000 AFIX 0 C11 1 0.316005 0.594157 0.280019 11.00000 0.09141 0.07905 = 0.05574 -0.00601 -0.03175 0.03435 AFIX 137 H11A 2 0.243878 0.647603 0.281141 11.00000 -1.50000 H11B 2 0.301786 0.494222 0.272486 11.00000 -1.50000 H11C 2 0.365671 0.650260 0.268588 11.00000 -1.50000 AFIX 0 C12 1 0.388070 0.734848 0.320607 11.00000 0.05397 0.05317 = 0.06745 -0.01366 -0.01145 0.02589 AFIX 137 H12A 2 0.426528 0.723692 0.338228 11.00000 -1.50000 H12B 2 0.313629 0.781261 0.322432 11.00000 -1.50000 H12C 2 0.433888 0.798407 0.309462 11.00000 -1.50000 AFIX 0 C13 1 0.606805 0.107456 0.329403 11.00000 0.03412 0.02421 = 0.06213 -0.00306 0.01249 0.00199 AFIX 13 H13 2 0.528615 0.071491 0.332780 11.00000 -1.20000 AFIX 0 C14 1 0.658809 -0.005356 0.310980 11.00000 0.06137 0.03685 = 0.12457 -0.00733 0.02937 0.00879 AFIX 137 H14A 2 0.615752 -0.005729 0.293795 11.00000 -1.50000 H14B 2 0.656459 -0.105463 0.318942 11.00000 -1.50000 H14C 2 0.737753 0.022370 0.308321 11.00000 -1.50000 AFIX 0 C15 1 0.673183 0.116818 0.356601 11.00000 0.05748 0.04144 = 0.09198 0.01602 -0.00565 0.01038 AFIX 137 H15A 2 0.751514 0.147496 0.353953 11.00000 -1.50000 H15B 2 0.673113 0.018425 0.365252 11.00000 -1.50000 H15C 2 0.637065 0.190478 0.367866 11.00000 -1.50000 AFIX 0 C16 1 0.238672 0.220838 0.386237 11.00000 0.01494 0.01718 = 0.03252 -0.00113 0.00456 -0.00917 C17 1 0.147921 0.316152 0.391067 11.00000 0.00905 0.02028 = 0.04638 -0.00354 0.00031 -0.00504 C18 1 0.109335 0.314236 0.416644 11.00000 0.01599 0.02636 = 0.04671 -0.00470 0.00596 -0.00749 AFIX 43 H18 2 0.047881 0.377644 0.420663 11.00000 -1.20000 AFIX 0 C19 1 0.156107 0.225182 0.436122 11.00000 0.03173 0.03918 = 0.03277 -0.01021 0.00922 -0.01771 AFIX 43 H19 2 0.127822 0.227020 0.453448 11.00000 -1.20000 AFIX 0 C20 1 0.245857 0.131099 0.430523 11.00000 0.03080 0.03196 = 0.03179 0.00316 -0.00586 -0.00467 AFIX 43 H20 2 0.278107 0.068590 0.444201 11.00000 -1.20000 AFIX 0 C21 1 0.288675 0.126462 0.405850 11.00000 0.02228 0.02143 = 0.03008 0.00180 -0.00015 -0.00709 C22 1 0.097577 0.418709 0.369480 11.00000 0.02189 0.02196 = 0.04766 0.00992 -0.00147 0.00063 AFIX 13 H22 2 0.131152 0.388877 0.352427 11.00000 -1.20000 AFIX 0 C23 1 -0.031204 0.402152 0.365448 11.00000 0.02290 0.06782 = 0.06735 0.01532 -0.00158 -0.00250 AFIX 137 H23A 2 -0.049918 0.298185 0.360726 11.00000 -1.50000 H23B 2 -0.059186 0.468877 0.351096 11.00000 -1.50000 H23C 2 -0.066987 0.428790 0.381941 11.00000 -1.50000 AFIX 0 C24 1 0.132137 0.583112 0.375053 11.00000 0.04453 0.03244 = 0.12034 0.00507 -0.02008 0.00248 AFIX 137 H24A 2 0.102135 0.615494 0.391915 11.00000 -1.50000 H24B 2 0.101153 0.647042 0.360601 11.00000 -1.50000 H24C 2 0.215054 0.591125 0.376179 11.00000 -1.50000 AFIX 0 C25 1 0.385919 0.020866 0.399244 11.00000 0.02953 0.01415 = 0.02818 0.00256 -0.00512 0.00262 AFIX 13 H25 2 0.415856 0.053728 0.381955 11.00000 -1.20000 AFIX 0 C26 1 0.340490 -0.137663 0.395745 11.00000 0.04130 0.02769 = 0.07502 -0.00598 -0.02712 0.00401 AFIX 137 H26A 2 0.401625 -0.204042 0.390523 11.00000 -1.50000 H26B 2 0.278965 -0.138496 0.381896 11.00000 -1.50000 H26C 2 0.311586 -0.172678 0.412561 11.00000 -1.50000 AFIX 0 C27 1 0.482297 0.024093 0.420035 11.00000 0.03028 0.02649 = 0.05267 -0.00332 -0.00538 0.00193 AFIX 137 H27A 2 0.505683 0.128069 0.423378 11.00000 -1.50000 H27B 2 0.546460 -0.033121 0.413718 11.00000 -1.50000 H27C 2 0.457498 -0.020569 0.436547 11.00000 -1.50000 AFIX 0 C28 1 0.591413 0.419079 0.443905 11.00000 0.01704 0.02194 = 0.02179 0.00140 -0.00416 0.00029 C29 1 0.691740 0.332510 0.445810 11.00000 0.01264 0.02100 = 0.03989 0.00370 0.00031 -0.00008 C30 1 0.706543 0.230309 0.467013 11.00000 0.01885 0.02569 = 0.04007 0.00479 -0.00795 0.00619 AFIX 43 H30 2 0.774157 0.172577 0.468719 11.00000 -1.20000 AFIX 0 C31 1 0.625290 0.212464 0.485247 11.00000 0.03028 0.02303 = 0.02978 -0.00093 -0.00750 -0.00656 C32 1 0.525179 0.293017 0.482297 11.00000 0.02348 0.02819 = 0.02735 0.00050 -0.00039 -0.00342 AFIX 43 H32 2 0.467942 0.277501 0.494598 11.00000 -1.20000 AFIX 0 C33 1 0.506183 0.395786 0.461863 11.00000 0.02409 0.01286 = 0.02224 -0.00711 -0.00500 -0.00211 C34 1 0.781361 0.341740 0.425481 11.00000 0.02506 0.03662 = 0.07266 0.02274 0.01801 0.02021 AFIX 137 H34A 2 0.840490 0.267031 0.429660 11.00000 -1.50000 H34B 2 0.815082 0.442131 0.425890 11.00000 -1.50000 H34C 2 0.746605 0.322043 0.407714 11.00000 -1.50000 AFIX 0 C35 1 0.644513 0.105185 0.508236 11.00000 0.04154 0.02674 = 0.03700 0.00693 -0.00554 -0.00293 AFIX 137 H35A 2 0.687429 0.018158 0.502431 11.00000 -1.50000 H35B 2 0.571176 0.071993 0.514375 11.00000 -1.50000 H35C 2 0.687414 0.155761 0.522826 11.00000 -1.50000 AFIX 0 C36 1 0.394099 0.478047 0.459532 11.00000 0.01418 0.03417 = 0.03394 0.00183 0.00580 0.00589 AFIX 137 H36A 2 0.342521 0.435761 0.472207 11.00000 -1.50000 H36B 2 0.360571 0.467181 0.441408 11.00000 -1.50000 H36C 2 0.406566 0.584513 0.463473 11.00000 -1.50000 AFIX 0 C37 1 0.689833 0.669085 0.411893 11.00000 0.01411 0.01316 = 0.03763 0.00140 -0.00186 0.00243 C38 1 0.737649 0.680535 0.386792 11.00000 0.01278 0.01299 = 0.03661 0.00525 -0.00351 0.00479 C39 1 0.830882 0.775585 0.384138 11.00000 0.01887 0.01984 = 0.04027 0.00264 0.00412 -0.00257 AFIX 43 H39 2 0.861942 0.785662 0.367192 11.00000 -1.20000 AFIX 0 C40 1 0.878271 0.853855 0.405078 11.00000 0.02354 0.02167 = 0.06623 -0.00490 0.00545 -0.00477 C41 1 0.829473 0.845233 0.429646 11.00000 0.02515 0.02294 = 0.05354 -0.01326 -0.00553 -0.00760 AFIX 43 H41 2 0.860343 0.903600 0.444058 11.00000 -1.20000 AFIX 0 C42 1 0.736370 0.752994 0.433615 11.00000 0.01779 0.01456 = 0.04758 -0.00305 -0.00540 0.00356 C43 1 0.693551 0.596703 0.362399 11.00000 0.02194 0.02847 = 0.02975 0.00468 0.00291 -0.00641 AFIX 137 H43A 2 0.737519 0.625082 0.347195 11.00000 -1.50000 H43B 2 0.613513 0.621849 0.358610 11.00000 -1.50000 H43C 2 0.700943 0.488659 0.365529 11.00000 -1.50000 AFIX 0 C44 1 0.978297 0.956049 0.401325 11.00000 0.03511 0.04025 = 0.10065 -0.01201 0.01229 -0.02485 AFIX 137 H44A 2 1.024147 0.915805 0.387294 11.00000 -1.50000 H44B 2 1.024726 0.962392 0.418008 11.00000 -1.50000 H44C 2 0.950873 1.056213 0.396241 11.00000 -1.50000 AFIX 0 C45 1 0.689084 0.750060 0.460877 11.00000 0.03707 0.03397 = 0.04206 -0.01431 -0.00681 -0.00710 AFIX 137 H45A 2 0.731474 0.820475 0.472565 11.00000 -1.50000 H45B 2 0.696129 0.648683 0.468271 11.00000 -1.50000 H45C 2 0.608923 0.779117 0.459510 11.00000 -1.50000 AFIX 0 B1 3 0.271465 0.029313 0.251817 10.50000 0.03464 B2 3 0.012610 0.962160 0.494080 10.50000 0.06851 N1 4 0.400269 0.280934 0.330215 11.00000 0.02159 0.01859 = 0.02742 0.00226 0.00211 -0.00173 N2 4 0.286513 0.224394 0.360403 11.00000 0.01646 0.01792 = 0.02883 -0.00090 -0.00195 0.00094 F1 5 0.217838 -0.030156 0.271901 10.75000 0.07509 F2 5 0.250000 0.181273 0.250000 10.50000 0.05862 F3 5 0.377964 0.007368 0.261912 10.75000 0.09416 F4 5 0.041168 0.926409 0.519620 10.66667 0.08166 F5 5 -0.095668 0.925231 0.499218 10.66667 0.13367 F6 5 0.070767 0.877980 0.476995 10.66667 0.10625 P1 6 0.566550 0.552186 0.417075 11.00000 0.01501 0.01651 = 0.02599 0.00184 -0.00019 0.00246 AFIX 13 H1 2 0.509704 0.623377 0.424010 11.00000 -1.20000 AFIX 0 AU1 7 0.469833 0.432434 0.382977 11.00000 0.01404 0.01981 = 0.02324 0.00242 -0.00040 -0.00097 HKLF 4 REM npm041 in P2/n REM R1 = 0.0536 for 9319 Fo > 4sig(Fo) and 0.0556 for all 9669 data REM 490 parameters refined using 9 restraints END WGHT 0.0169 59.6309 REM Highest difference peak 2.813, deepest hole -3.059, 1-sigma level 0.146 Q1 1 0.0807 0.9856 0.5112 11.00000 0.05 2.81 Q2 1 0.2694 -0.0662 0.2688 11.00000 0.05 2.38 Q3 1 0.1844 0.0132 0.2740 11.00000 0.05 1.84 Q4 1 0.4667 0.1594 0.3830 11.00000 0.05 1.72 Q5 1 0.0873 0.2973 0.3512 11.00000 0.05 1.67 Q6 1 -0.1193 0.9008 0.5049 11.00000 0.05 1.45 Q7 1 0.0176 0.8982 0.5249 11.00000 0.05 1.26 Q8 1 0.5017 -0.2583 0.3936 11.00000 0.05 1.05 Q9 1 0.8556 0.5733 0.4144 11.00000 0.05 1.04 Q10 1 0.4787 0.6369 0.3924 11.00000 0.05 0.87 ; data_npm023 _database_code_depnum_ccdc_archive 'CCDC 906061' #TrackingRef 'web_deposit_cif_file_0_MilesW.Johnson_1352328108.npm023.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; npm023 ; _chemical_name_common npm023 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H59 Au B Cl4 F4 N2 P' _chemical_formula_weight 988.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9915(6) _cell_length_b 12.2396(6) _cell_length_c 16.7165(9) _cell_angle_alpha 96.5550(10) _cell_angle_beta 108.3860(10) _cell_angle_gamma 105.0960(10) _cell_volume 2195.71(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9274 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 3.674 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2609 _exptl_absorpt_correction_T_max 0.4053 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'microfocus sealed tube' _diffrn_radiation_monochromator 'QUAZAR multilayer mirrors' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 72223 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0124 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 25.37 _reflns_number_total 8051 _reflns_number_gt 7702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+49.6006P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8051 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0683 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_ref 0.1471 _refine_ls_wR_factor_gt 0.1449 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1227(7) 0.8178(7) 0.7454(5) 0.0143(15) Uani 1 1 d . . . C2 C 0.2912(7) 0.9729(7) 0.7848(5) 0.0175(16) Uani 1 1 d . . . H2 H 0.3733 1.0235 0.8143 0.021 Uiso 1 1 calc R . . C3 C 0.2004(7) 0.9938(7) 0.7220(5) 0.0190(16) Uani 1 1 d . . . H3 H 0.2064 1.0615 0.6988 0.023 Uiso 1 1 calc R . . C4 C -0.0241(7) 0.8787(7) 0.6354(5) 0.0170(16) Uani 1 1 d . . . C5 C -0.0482(7) 0.8292(7) 0.5495(5) 0.0197(17) Uani 1 1 d . . . C6 C -0.1685(8) 0.8065(8) 0.4911(6) 0.0243(18) Uani 1 1 d . . . H6 H -0.1884 0.7743 0.4320 0.029 Uiso 1 1 calc R . . C7 C -0.2581(8) 0.8300(8) 0.5180(6) 0.0270(19) Uani 1 1 d . . . H7 H -0.3400 0.8115 0.4776 0.032 Uiso 1 1 calc R . . C8 C -0.2314(8) 0.8806(8) 0.6035(6) 0.0269(19) Uani 1 1 d . . . H8 H -0.2944 0.8978 0.6206 0.032 Uiso 1 1 calc R . . C9 C -0.1118(8) 0.9064(7) 0.6646(5) 0.0225(18) Uani 1 1 d . . . C10 C 0.0495(8) 0.7982(7) 0.5200(5) 0.0220(17) Uani 1 1 d . . . H10 H 0.1320 0.8391 0.5664 0.026 Uiso 1 1 calc R . . C11 C 0.0531(9) 0.8372(9) 0.4371(6) 0.033(2) Uani 1 1 d . . . H11A H -0.0264 0.7974 0.3902 0.049 Uiso 1 1 calc R . . H11B H 0.1196 0.8181 0.4223 0.049 Uiso 1 1 calc R . . H11C H 0.0683 0.9210 0.4456 0.049 Uiso 1 1 calc R . . C12 C 0.0302(11) 0.6683(9) 0.5090(7) 0.038(2) Uani 1 1 d . . . H12A H 0.0319 0.6450 0.5634 0.057 Uiso 1 1 calc R . . H12B H 0.0964 0.6506 0.4928 0.057 Uiso 1 1 calc R . . H12C H -0.0501 0.6259 0.4636 0.057 Uiso 1 1 calc R . . C13 C -0.0827(8) 0.9636(9) 0.7572(6) 0.027(2) Uani 1 1 d . . . H13 H 0.0061 0.9736 0.7901 0.033 Uiso 1 1 calc R . . C14 C -0.0981(10) 1.0835(9) 0.7621(7) 0.039(2) Uani 1 1 d . . . H14A H -0.0395 1.1325 0.7411 0.059 Uiso 1 1 calc R . . H14B H -0.0819 1.1183 0.8220 0.059 Uiso 1 1 calc R . . H14C H -0.1828 1.0769 0.7262 0.059 Uiso 1 1 calc R . . C15 C -0.1609(9) 0.8861(10) 0.7982(6) 0.036(2) Uani 1 1 d . . . H15A H -0.2486 0.8766 0.7684 0.054 Uiso 1 1 calc R . . H15B H -0.1362 0.9219 0.8593 0.054 Uiso 1 1 calc R . . H15C H -0.1481 0.8101 0.7934 0.054 Uiso 1 1 calc R . . C16 C 0.3044(7) 0.8067(7) 0.8600(5) 0.0175(16) Uani 1 1 d . . . C17 C 0.3503(7) 0.7222(7) 0.8328(5) 0.0212(17) Uani 1 1 d . . . C18 C 0.4048(8) 0.6656(7) 0.8944(6) 0.0248(18) Uani 1 1 d . . . H18 H 0.4358 0.6061 0.8780 0.030 Uiso 1 1 calc R . . C19 C 0.4142(8) 0.6946(8) 0.9789(6) 0.028(2) Uani 1 1 d . . . H19 H 0.4515 0.6549 1.0199 0.033 Uiso 1 1 calc R . . C20 C 0.3699(8) 0.7811(8) 1.0048(6) 0.0247(18) Uani 1 1 d . . . H20 H 0.3789 0.8011 1.0636 0.030 Uiso 1 1 calc R . . C21 C 0.3127(7) 0.8389(7) 0.9458(5) 0.0208(17) Uani 1 1 d . . . C22 C 0.3421(8) 0.6901(8) 0.7401(6) 0.0251(19) Uani 1 1 d . . . H22 H 0.3075 0.7445 0.7073 0.030 Uiso 1 1 calc R . . C23 C 0.4708(9) 0.7031(9) 0.7367(7) 0.037(2) Uani 1 1 d . . . H23A H 0.5034 0.6459 0.7644 0.055 Uiso 1 1 calc R . . H23B H 0.5263 0.7813 0.7671 0.055 Uiso 1 1 calc R . . H23C H 0.4651 0.6905 0.6764 0.055 Uiso 1 1 calc R . . C24 C 0.2561(9) 0.5664(9) 0.6966(7) 0.035(2) Uani 1 1 d . . . H24A H 0.2532 0.5481 0.6372 0.052 Uiso 1 1 calc R . . H24B H 0.1727 0.5600 0.6961 0.052 Uiso 1 1 calc R . . H24C H 0.2874 0.5119 0.7288 0.052 Uiso 1 1 calc R . . C25 C 0.2587(7) 0.9294(7) 0.9737(5) 0.0216(17) Uani 1 1 d . . . H25 H 0.2360 0.9700 0.9252 0.026 Uiso 1 1 calc R . . C26 C 0.3516(9) 1.0207(9) 1.0532(6) 0.033(2) Uani 1 1 d . . . H26A H 0.3737 0.9838 1.1023 0.050 Uiso 1 1 calc R . . H26B H 0.3146 1.0796 1.0666 0.050 Uiso 1 1 calc R . . H26C H 0.4262 1.0574 1.0415 0.050 Uiso 1 1 calc R . . C27 C 0.1400(9) 0.8715(9) 0.9895(7) 0.035(2) Uani 1 1 d . . . H27A H 0.0825 0.8121 0.9383 0.052 Uiso 1 1 calc R . . H27B H 0.1013 0.9299 1.0009 0.052 Uiso 1 1 calc R . . H27C H 0.1604 0.8354 1.0393 0.052 Uiso 1 1 calc R . . C28 C -0.2943(8) 0.4698(8) 0.6292(6) 0.028(2) Uani 1 1 d . . . C29 C -0.2602(10) 0.5194(11) 0.5569(7) 0.045(3) Uani 1 1 d . . . H29A H -0.3360 0.5102 0.5082 0.067 Uiso 1 1 calc R . . H29B H -0.2102 0.4778 0.5379 0.067 Uiso 1 1 calc R . . H29C H -0.2127 0.6018 0.5783 0.067 Uiso 1 1 calc R . . C30 C -0.3667(10) 0.5345(11) 0.6613(8) 0.047(3) Uani 1 1 d . . . H30A H -0.3155 0.6155 0.6865 0.071 Uiso 1 1 calc R . . H30B H -0.3915 0.4992 0.7053 0.071 Uiso 1 1 calc R . . H30C H -0.4407 0.5313 0.6132 0.071 Uiso 1 1 calc R . . C31 C -0.3706(12) 0.3407(11) 0.5922(9) 0.059(3) Uani 1 1 d . . . H31A H -0.3957 0.3072 0.6368 0.089 Uiso 1 1 calc R . . H31B H -0.3202 0.2992 0.5738 0.089 Uiso 1 1 calc R . . H31C H -0.4445 0.3338 0.5426 0.089 Uiso 1 1 calc R . . C32 C -0.1477(9) 0.4444(9) 0.8162(7) 0.035(2) Uani 1 1 d . . . C33 C -0.0203(11) 0.4379(12) 0.8620(10) 0.062(4) Uani 1 1 d . . . H33A H -0.0176 0.4107 0.9152 0.093 Uiso 1 1 calc R . . H33B H 0.0407 0.5150 0.8761 0.093 Uiso 1 1 calc R . . H33C H -0.0010 0.3839 0.8244 0.093 Uiso 1 1 calc R . . C34 C -0.1715(13) 0.5410(12) 0.8710(8) 0.057(3) Uani 1 1 d . . . H34A H -0.2537 0.5465 0.8408 0.085 Uiso 1 1 calc R . . H34B H -0.1085 0.6153 0.8797 0.085 Uiso 1 1 calc R . . H34C H -0.1672 0.5222 0.9271 0.085 Uiso 1 1 calc R . . C35 C -0.2469(10) 0.3293(10) 0.8027(9) 0.049(3) Uani 1 1 d . . . H35A H -0.2399 0.3087 0.8586 0.073 Uiso 1 1 calc R . . H35B H -0.2353 0.2687 0.7655 0.073 Uiso 1 1 calc R . . H35C H -0.3290 0.3369 0.7754 0.073 Uiso 1 1 calc R . . C36 C 0.2492(10) 0.2528(9) 0.9254(8) 0.041(3) Uani 1 1 d . . . H36A H 0.3201 0.2224 0.9427 0.049 Uiso 1 1 calc R . . H36B H 0.2078 0.2278 0.8619 0.049 Uiso 1 1 calc R . . C37 C 0.4569(12) 1.0295(11) 0.6226(8) 0.054(3) Uani 1 1 d . . . H37A H 0.4989 1.0896 0.5975 0.065 Uiso 1 1 calc R . . H37B H 0.3872 1.0509 0.6319 0.065 Uiso 1 1 calc R . . B1 B 0.3923(10) 0.2935(9) 0.7575(7) 0.026(2) Uani 1 1 d . . . N1 N 0.0974(6) 0.8967(5) 0.6985(4) 0.0140(13) Uani 1 1 d . . . N2 N 0.2414(6) 0.8640(5) 0.7975(4) 0.0153(13) Uani 1 1 d . . . F1 F 0.2657(5) 0.2773(5) 0.7345(4) 0.0360(13) Uani 1 1 d . . . F2 F 0.4600(6) 0.4078(5) 0.7904(5) 0.0465(16) Uani 1 1 d . . . F3 F 0.4139(7) 0.2524(7) 0.6844(4) 0.062(2) Uani 1 1 d . . . F4 F 0.4269(6) 0.2297(5) 0.8188(4) 0.0481(17) Uani 1 1 d . . . P1 P -0.1438(2) 0.4850(2) 0.71371(17) 0.0297(5) Uani 1 1 d . . . Au1 Au -0.00121(3) 0.66197(3) 0.73511(2) 0.02554(12) Uani 1 1 d . . . Cl1 Cl 0.1440(2) 0.1936(2) 0.97477(19) 0.0435(6) Uani 1 1 d . . . Cl2 Cl 0.3034(3) 0.4028(2) 0.9535(3) 0.0582(9) Uani 1 1 d . . . Cl3 Cl 0.5613(3) 1.0246(3) 0.7214(2) 0.0553(8) Uani 1 1 d . . . Cl4 Cl 0.3999(3) 0.8954(4) 0.5504(3) 0.0733(10) Uani 1 1 d . . . H1 H -0.104(10) 0.391(10) 0.681(7) 0.05(3) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.016(4) 0.017(4) 0.015(4) 0.001(3) 0.012(3) 0.007(3) C2 0.014(4) 0.015(4) 0.024(4) 0.003(3) 0.010(3) 0.004(3) C3 0.019(4) 0.015(4) 0.023(4) 0.002(3) 0.010(3) 0.003(3) C4 0.015(4) 0.019(4) 0.017(4) 0.006(3) 0.006(3) 0.005(3) C5 0.019(4) 0.018(4) 0.022(4) 0.008(3) 0.007(3) 0.004(3) C6 0.022(4) 0.028(5) 0.019(4) 0.008(4) 0.004(3) 0.005(4) C7 0.018(4) 0.032(5) 0.028(5) 0.011(4) 0.003(4) 0.007(4) C8 0.017(4) 0.037(5) 0.032(5) 0.012(4) 0.011(4) 0.013(4) C9 0.019(4) 0.026(4) 0.022(4) 0.007(4) 0.008(3) 0.005(3) C10 0.026(4) 0.023(4) 0.018(4) 0.002(3) 0.010(3) 0.009(4) C11 0.032(5) 0.042(6) 0.033(5) 0.015(4) 0.018(4) 0.015(4) C12 0.058(7) 0.032(5) 0.043(6) 0.012(5) 0.031(5) 0.024(5) C13 0.018(4) 0.045(6) 0.024(5) 0.009(4) 0.012(4) 0.013(4) C14 0.042(6) 0.046(6) 0.031(5) 0.002(5) 0.016(5) 0.014(5) C15 0.034(5) 0.055(7) 0.025(5) 0.013(5) 0.018(4) 0.013(5) C16 0.011(4) 0.019(4) 0.020(4) 0.007(3) 0.004(3) 0.001(3) C17 0.015(4) 0.020(4) 0.025(4) 0.004(3) 0.007(3) 0.001(3) C18 0.020(4) 0.022(4) 0.032(5) 0.005(4) 0.009(4) 0.007(3) C19 0.019(4) 0.027(5) 0.033(5) 0.014(4) 0.004(4) 0.005(4) C20 0.020(4) 0.028(5) 0.022(4) 0.006(4) 0.006(3) 0.003(4) C21 0.013(4) 0.022(4) 0.024(4) 0.005(3) 0.006(3) 0.000(3) C22 0.030(5) 0.023(4) 0.025(4) 0.002(4) 0.012(4) 0.012(4) C23 0.035(5) 0.043(6) 0.041(6) 0.006(5) 0.024(5) 0.015(5) C24 0.033(5) 0.036(5) 0.034(5) -0.004(4) 0.013(4) 0.013(4) C25 0.017(4) 0.027(4) 0.019(4) 0.004(3) 0.007(3) 0.005(3) C26 0.028(5) 0.037(5) 0.034(5) -0.008(4) 0.011(4) 0.014(4) C27 0.028(5) 0.034(5) 0.046(6) 0.002(4) 0.023(5) 0.008(4) C28 0.020(4) 0.028(5) 0.030(5) 0.001(4) 0.008(4) 0.001(4) C29 0.033(6) 0.064(8) 0.034(6) 0.005(5) 0.013(5) 0.012(5) C30 0.029(5) 0.059(7) 0.048(7) 0.002(6) 0.006(5) 0.020(5) C31 0.044(7) 0.042(7) 0.068(9) -0.003(6) 0.007(6) -0.003(6) C32 0.032(5) 0.034(5) 0.039(6) 0.016(4) 0.014(4) 0.005(4) C33 0.043(7) 0.063(8) 0.078(10) 0.045(8) 0.013(7) 0.011(6) C34 0.066(8) 0.068(9) 0.043(7) 0.018(6) 0.026(6) 0.020(7) C35 0.039(6) 0.039(6) 0.073(8) 0.037(6) 0.022(6) 0.007(5) C36 0.035(6) 0.036(6) 0.058(7) 0.014(5) 0.026(5) 0.009(5) C37 0.060(8) 0.060(8) 0.061(8) 0.029(7) 0.030(7) 0.031(7) B1 0.028(5) 0.021(5) 0.027(5) 0.004(4) 0.007(4) 0.009(4) N1 0.015(3) 0.016(3) 0.016(3) 0.002(3) 0.010(3) 0.006(3) N2 0.013(3) 0.015(3) 0.016(3) 0.002(3) 0.006(3) 0.003(3) F1 0.028(3) 0.033(3) 0.040(3) 0.009(3) 0.005(2) 0.007(2) F2 0.039(3) 0.023(3) 0.071(4) 0.005(3) 0.019(3) 0.003(3) F3 0.057(4) 0.100(6) 0.028(3) -0.008(4) 0.005(3) 0.044(4) F4 0.036(3) 0.040(3) 0.051(4) 0.026(3) -0.004(3) 0.002(3) P1 0.0262(12) 0.0245(12) 0.0396(14) 0.0072(10) 0.0142(11) 0.0069(10) Au1 0.01663(17) 0.02490(19) 0.02785(19) 0.01232(14) 0.00260(13) -0.00144(13) Cl1 0.0356(13) 0.0414(14) 0.0588(17) 0.0184(13) 0.0252(13) 0.0075(11) Cl2 0.0546(18) 0.0317(14) 0.105(3) 0.0178(15) 0.0495(19) 0.0134(13) Cl3 0.0416(16) 0.068(2) 0.0611(19) 0.0144(16) 0.0204(14) 0.0228(15) Cl4 0.059(2) 0.076(2) 0.069(2) 0.0026(19) 0.0196(18) 0.0038(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 C1 N2 1.338(10) . ? C1 N1 1.348(10) . ? C1 Au1 2.040(8) . ? C2 C3 1.355(12) . ? C2 N2 1.382(10) . ? C2 H2 0.9500 . ? C3 N1 1.384(10) . ? C3 H3 0.9500 . ? C4 C9 1.390(12) . ? C4 C5 1.399(11) . ? C4 N1 1.447(10) . ? C5 C6 1.398(12) . ? C5 C10 1.521(11) . ? C6 C7 1.370(13) . ? C6 H6 0.9500 . ? C7 C8 1.390(13) . ? C7 H7 0.9500 . ? C8 C9 1.402(12) . ? C8 H8 0.9500 . ? C9 C13 1.515(12) . ? C10 C11 1.526(12) . ? C10 C12 1.526(12) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.523(14) . ? C13 C15 1.530(13) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.388(12) . ? C16 C21 1.407(12) . ? C16 N2 1.449(10) . ? C17 C18 1.395(12) . ? C17 C22 1.520(12) . ? C18 C19 1.377(13) . ? C18 H18 0.9500 . ? C19 C20 1.387(13) . ? C19 H19 0.9500 . ? C20 C21 1.389(12) . ? C20 H20 0.9500 . ? C21 C25 1.520(12) . ? C22 C23 1.530(13) . ? C22 C24 1.532(13) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.527(12) . ? C25 C27 1.534(12) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.492(14) . ? C28 C29 1.531(14) . ? C28 C31 1.544(14) . ? C28 P1 1.856(9) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.505(15) . ? C32 C35 1.528(13) . ? C32 C34 1.553(17) . ? C32 P1 1.848(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 Cl2 1.734(11) . ? C36 Cl1 1.764(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 Cl3 1.748(13) . ? C37 Cl4 1.748(14) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? B1 F2 1.367(12) . ? B1 F4 1.385(12) . ? B1 F3 1.392(12) . ? B1 F1 1.397(12) . ? P1 Au1 2.292(2) . ? P1 H1 1.46(11) . ? 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 N2 C1 N1 105.9(7) . . ? N2 C1 Au1 129.4(6) . . ? N1 C1 Au1 124.8(6) . . ? C3 C2 N2 106.9(7) . . ? C3 C2 H2 126.6 . . ? N2 C2 H2 126.6 . . ? C2 C3 N1 106.2(7) . . ? C2 C3 H3 126.9 . . ? N1 C3 H3 126.9 . . ? C9 C4 C5 123.9(7) . . ? C9 C4 N1 117.8(7) . . ? C5 C4 N1 118.2(7) . . ? C6 C5 C4 116.8(8) . . ? C6 C5 C10 120.6(8) . . ? C4 C5 C10 122.5(7) . . ? C7 C6 C5 120.8(8) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C8 121.2(8) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? C7 C8 C9 120.3(8) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C4 C9 C8 116.9(8) . . ? C4 C9 C13 123.1(7) . . ? C8 C9 C13 120.0(8) . . ? C5 C10 C11 112.7(7) . . ? C5 C10 C12 110.7(7) . . ? C11 C10 C12 110.2(7) . . ? C5 C10 H10 107.7 . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 110.4(8) . . ? C9 C13 C15 110.8(8) . . ? C14 C13 C15 112.5(8) . . ? C9 C13 H13 107.6 . . ? C14 C13 H13 107.6 . . ? C15 C13 H13 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.6(8) . . ? C17 C16 N2 119.3(7) . . ? C21 C16 N2 117.1(7) . . ? C16 C17 C18 117.1(8) . . ? C16 C17 C22 122.7(8) . . ? C18 C17 C22 120.2(8) . . ? C19 C18 C17 120.8(8) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 120.9(8) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 120.7(8) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 116.8(8) . . ? C20 C21 C25 120.5(8) . . ? C16 C21 C25 122.7(7) . . ? C17 C22 C23 110.5(8) . . ? C17 C22 C24 111.4(8) . . ? C23 C22 C24 110.0(8) . . ? C17 C22 H22 108.3 . . ? C23 C22 H22 108.3 . . ? C24 C22 H22 108.3 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C26 112.4(7) . . ? C21 C25 C27 110.5(7) . . ? C26 C25 C27 110.8(7) . . ? C21 C25 H25 107.7 . . ? C26 C25 H25 107.7 . . ? C27 C25 H25 107.7 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 110.5(9) . . ? C30 C28 C31 110.8(9) . . ? C29 C28 C31 107.7(9) . . ? C30 C28 P1 112.3(7) . . ? C29 C28 P1 104.9(6) . . ? C31 C28 P1 110.5(8) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C35 111.0(9) . . ? C33 C32 C34 109.3(10) . . ? C35 C32 C34 108.9(10) . . ? C33 C32 P1 105.1(8) . . ? C35 C32 P1 112.9(8) . . ? C34 C32 P1 109.6(7) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Cl2 C36 Cl1 112.1(6) . . ? Cl2 C36 H36A 109.2 . . ? Cl1 C36 H36A 109.2 . . ? Cl2 C36 H36B 109.2 . . ? Cl1 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? Cl3 C37 Cl4 110.9(7) . . ? Cl3 C37 H37A 109.4 . . ? Cl4 C37 H37A 109.4 . . ? Cl3 C37 H37B 109.4 . . ? Cl4 C37 H37B 109.4 . . ? H37A C37 H37B 108.0 . . ? F2 B1 F4 109.3(8) . . ? F2 B1 F3 110.3(9) . . ? F4 B1 F3 108.7(8) . . ? F2 B1 F1 111.2(8) . . ? F4 B1 F1 108.9(8) . . ? F3 B1 F1 108.4(8) . . ? C1 N1 C3 110.5(7) . . ? C1 N1 C4 122.3(6) . . ? C3 N1 C4 127.2(7) . . ? C1 N2 C2 110.5(7) . . ? C1 N2 C16 123.2(6) . . ? C2 N2 C16 126.2(6) . . ? C32 P1 C28 117.3(4) . . ? C32 P1 Au1 112.4(3) . . ? C28 P1 Au1 111.7(3) . . ? C32 P1 H1 99(4) . . ? C28 P1 H1 105(4) . . ? Au1 P1 H1 111(4) . . ? C1 Au1 P1 176.2(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 12.228 _refine_diff_density_min -5.646 _refine_diff_density_rms 0.222 _iucr_refine_instructions_details ; TITL npm023 in P-1 CELL 0.71073 11.9915 12.2396 16.7165 96.555 108.386 105.096 ZERR 2.00 0.0006 0.0006 0.0009 0.001 0.001 0.001 LATT 1 SFAC C H B N F P AU CL UNIT 74 118 2 4 8 2 2 8 MERG 2 FMAP 2 PLAN 20 SIZE 0.30 0.40 0.50 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.000000 49.600600 FVAR 0.10272 C1 1 0.122712 0.817809 0.745423 11.00000 0.01556 0.01733 = 0.01550 0.00082 0.01231 0.00703 C2 1 0.291208 0.972934 0.784778 11.00000 0.01428 0.01533 = 0.02441 0.00285 0.01017 0.00374 AFIX 43 H2 2 0.373331 1.023469 0.814337 11.00000 -1.20000 AFIX 0 C3 1 0.200446 0.993836 0.722014 11.00000 0.01872 0.01521 = 0.02300 0.00244 0.00964 0.00312 AFIX 43 H3 2 0.206378 1.061546 0.698806 11.00000 -1.20000 AFIX 0 C4 1 -0.024111 0.878663 0.635369 11.00000 0.01491 0.01884 = 0.01741 0.00589 0.00552 0.00508 C5 1 -0.048177 0.829219 0.549539 11.00000 0.01862 0.01797 = 0.02238 0.00848 0.00687 0.00439 C6 1 -0.168525 0.806480 0.491119 11.00000 0.02232 0.02811 = 0.01861 0.00850 0.00393 0.00454 AFIX 43 H6 2 -0.188449 0.774273 0.431989 11.00000 -1.20000 AFIX 0 C7 1 -0.258117 0.830044 0.518037 11.00000 0.01805 0.03198 = 0.02793 0.01071 0.00343 0.00695 AFIX 43 H7 2 -0.339976 0.811480 0.477582 11.00000 -1.20000 AFIX 0 C8 1 -0.231395 0.880638 0.603497 11.00000 0.01711 0.03737 = 0.03176 0.01236 0.01128 0.01258 AFIX 43 H8 2 -0.294430 0.897838 0.620578 11.00000 -1.20000 AFIX 0 C9 1 -0.111806 0.906383 0.664580 11.00000 0.01867 0.02630 = 0.02221 0.00690 0.00769 0.00528 C10 1 0.049505 0.798196 0.520038 11.00000 0.02575 0.02316 = 0.01838 0.00166 0.00962 0.00908 AFIX 13 H10 2 0.132018 0.839092 0.566407 11.00000 -1.20000 AFIX 0 C11 1 0.053078 0.837152 0.437119 11.00000 0.03179 0.04168 = 0.03312 0.01526 0.01793 0.01494 AFIX 137 H11A 2 -0.026386 0.797373 0.390165 11.00000 -1.50000 H11B 2 0.119571 0.818058 0.422288 11.00000 -1.50000 H11C 2 0.068342 0.921045 0.445648 11.00000 -1.50000 AFIX 0 C12 1 0.030208 0.668301 0.508959 11.00000 0.05768 0.03166 = 0.04262 0.01235 0.03124 0.02397 AFIX 137 H12A 2 0.031937 0.644981 0.563394 11.00000 -1.50000 H12B 2 0.096353 0.650638 0.492776 11.00000 -1.50000 H12C 2 -0.050057 0.625883 0.463594 11.00000 -1.50000 AFIX 0 C13 1 -0.082746 0.963555 0.757205 11.00000 0.01805 0.04530 = 0.02416 0.00906 0.01214 0.01346 AFIX 13 H13 2 0.006127 0.973637 0.790149 11.00000 -1.20000 AFIX 0 C14 1 -0.098108 1.083489 0.762070 11.00000 0.04205 0.04570 = 0.03110 0.00175 0.01648 0.01398 AFIX 137 H14A 2 -0.039518 1.132488 0.741085 11.00000 -1.50000 H14B 2 -0.081854 1.118251 0.822048 11.00000 -1.50000 H14C 2 -0.182839 1.076919 0.726209 11.00000 -1.50000 AFIX 0 C15 1 -0.160927 0.886067 0.798237 11.00000 0.03397 0.05464 = 0.02519 0.01284 0.01818 0.01292 AFIX 137 H15A 2 -0.248605 0.876599 0.768354 11.00000 -1.50000 H15B 2 -0.136157 0.921882 0.859277 11.00000 -1.50000 H15C 2 -0.148105 0.810078 0.793369 11.00000 -1.50000 AFIX 0 C16 1 0.304398 0.806699 0.860048 11.00000 0.01085 0.01914 = 0.01972 0.00691 0.00365 0.00112 C17 1 0.350305 0.722248 0.832790 11.00000 0.01514 0.02031 = 0.02493 0.00399 0.00675 0.00143 C18 1 0.404773 0.665556 0.894446 11.00000 0.02032 0.02184 = 0.03220 0.00532 0.00925 0.00719 AFIX 43 H18 2 0.435777 0.606144 0.877975 11.00000 -1.20000 AFIX 0 C19 1 0.414181 0.694619 0.978911 11.00000 0.01903 0.02732 = 0.03320 0.01441 0.00355 0.00461 AFIX 43 H19 2 0.451461 0.654898 1.019939 11.00000 -1.20000 AFIX 0 C20 1 0.369934 0.781117 1.004844 11.00000 0.02002 0.02820 = 0.02193 0.00598 0.00608 0.00286 AFIX 43 H20 2 0.378851 0.801078 1.063643 11.00000 -1.20000 AFIX 0 C21 1 0.312712 0.838912 0.945807 11.00000 0.01324 0.02169 = 0.02356 0.00527 0.00625 -0.00045 C22 1 0.342058 0.690106 0.740065 11.00000 0.03041 0.02303 = 0.02452 0.00205 0.01168 0.01182 AFIX 13 H22 2 0.307458 0.744513 0.707265 11.00000 -1.20000 AFIX 0 C23 1 0.470779 0.703117 0.736661 11.00000 0.03459 0.04334 = 0.04134 0.00603 0.02386 0.01475 AFIX 137 H23A 2 0.503389 0.645886 0.764352 11.00000 -1.50000 H23B 2 0.526277 0.781269 0.767089 11.00000 -1.50000 H23C 2 0.465124 0.690532 0.676360 11.00000 -1.50000 AFIX 0 C24 1 0.256101 0.566386 0.696643 11.00000 0.03257 0.03598 = 0.03410 -0.00418 0.01260 0.01318 AFIX 137 H24A 2 0.253194 0.548124 0.637249 11.00000 -1.50000 H24B 2 0.172678 0.560009 0.696104 11.00000 -1.50000 H24C 2 0.287440 0.511871 0.728797 11.00000 -1.50000 AFIX 0 C25 1 0.258731 0.929447 0.973706 11.00000 0.01730 0.02705 = 0.01917 0.00447 0.00697 0.00468 AFIX 13 H25 2 0.235974 0.969964 0.925222 11.00000 -1.20000 AFIX 0 C26 1 0.351620 1.020734 1.053161 11.00000 0.02755 0.03715 = 0.03367 -0.00785 0.01147 0.01369 AFIX 137 H26A 2 0.373652 0.983751 1.102326 11.00000 -1.50000 H26B 2 0.314588 1.079633 1.066634 11.00000 -1.50000 H26C 2 0.426221 1.057388 1.041503 11.00000 -1.50000 AFIX 0 C27 1 0.140046 0.871486 0.989481 11.00000 0.02757 0.03380 = 0.04645 0.00156 0.02252 0.00793 AFIX 137 H27A 2 0.082530 0.812090 0.938320 11.00000 -1.50000 H27B 2 0.101334 0.929895 1.000876 11.00000 -1.50000 H27C 2 0.160430 0.835436 1.039328 11.00000 -1.50000 AFIX 0 C28 1 -0.294262 0.469850 0.629164 11.00000 0.01988 0.02799 = 0.02971 0.00074 0.00789 0.00145 C29 1 -0.260208 0.519371 0.556892 11.00000 0.03306 0.06405 = 0.03441 0.00519 0.01269 0.01229 AFIX 137 H29A 2 -0.335956 0.510184 0.508161 11.00000 -1.50000 H29B 2 -0.210204 0.477828 0.537935 11.00000 -1.50000 H29C 2 -0.212661 0.601807 0.578311 11.00000 -1.50000 AFIX 0 C30 1 -0.366708 0.534509 0.661291 11.00000 0.02912 0.05935 = 0.04793 0.00169 0.00631 0.01979 AFIX 137 H30A 2 -0.315538 0.615454 0.686460 11.00000 -1.50000 H30B 2 -0.391467 0.499238 0.705338 11.00000 -1.50000 H30C 2 -0.440716 0.531316 0.613183 11.00000 -1.50000 AFIX 0 C31 1 -0.370619 0.340696 0.592218 11.00000 0.04376 0.04212 = 0.06849 -0.00338 0.00736 -0.00260 AFIX 137 H31A 2 -0.395697 0.307161 0.636772 11.00000 -1.50000 H31B 2 -0.320159 0.299200 0.573825 11.00000 -1.50000 H31C 2 -0.444453 0.333771 0.542613 11.00000 -1.50000 AFIX 0 C32 1 -0.147663 0.444429 0.816164 11.00000 0.03194 0.03370 = 0.03929 0.01634 0.01360 0.00504 C33 1 -0.020287 0.437947 0.861966 11.00000 0.04322 0.06282 = 0.07790 0.04493 0.01308 0.01138 AFIX 137 H33A 2 -0.017576 0.410694 0.915232 11.00000 -1.50000 H33B 2 0.040660 0.514981 0.876051 11.00000 -1.50000 H33C 2 -0.000998 0.383945 0.824439 11.00000 -1.50000 AFIX 0 C34 1 -0.171451 0.541039 0.870980 11.00000 0.06556 0.06827 = 0.04307 0.01787 0.02642 0.01983 AFIX 137 H34A 2 -0.253690 0.546542 0.840754 11.00000 -1.50000 H34B 2 -0.108462 0.615282 0.879686 11.00000 -1.50000 H34C 2 -0.167211 0.522249 0.927087 11.00000 -1.50000 AFIX 0 C35 1 -0.246851 0.329348 0.802697 11.00000 0.03920 0.03911 = 0.07272 0.03748 0.02236 0.00683 AFIX 137 H35A 2 -0.239902 0.308692 0.858614 11.00000 -1.50000 H35B 2 -0.235273 0.268674 0.765487 11.00000 -1.50000 H35C 2 -0.328985 0.336880 0.775352 11.00000 -1.50000 AFIX 0 C36 1 0.249171 0.252753 0.925415 11.00000 0.03530 0.03561 = 0.05824 0.01405 0.02611 0.00898 AFIX 23 H36A 2 0.320119 0.222358 0.942736 11.00000 -1.20000 H36B 2 0.207782 0.227781 0.861949 11.00000 -1.20000 AFIX 0 C37 1 0.456931 1.029455 0.622559 11.00000 0.06024 0.05996 = 0.06074 0.02885 0.03026 0.03106 AFIX 23 H37A 2 0.498906 1.089576 0.597532 11.00000 -1.20000 H37B 2 0.387184 1.050867 0.631924 11.00000 -1.20000 AFIX 0 B1 3 0.392328 0.293499 0.757454 11.00000 0.02798 0.02144 = 0.02719 0.00372 0.00655 0.00905 N1 4 0.097357 0.896744 0.698501 11.00000 0.01477 0.01551 = 0.01550 0.00203 0.00960 0.00644 N2 4 0.241403 0.864027 0.797539 11.00000 0.01326 0.01535 = 0.01597 0.00245 0.00554 0.00261 F1 5 0.265692 0.277331 0.734523 11.00000 0.02826 0.03348 = 0.03953 0.00888 0.00493 0.00746 F2 5 0.460037 0.407779 0.790404 11.00000 0.03897 0.02336 = 0.07094 0.00512 0.01935 0.00251 F3 5 0.413927 0.252369 0.684406 11.00000 0.05680 0.10020 = 0.02792 -0.00788 0.00474 0.04449 F4 5 0.426884 0.229692 0.818831 11.00000 0.03554 0.04031 = 0.05131 0.02556 -0.00431 0.00160 P1 6 -0.143838 0.485004 0.713706 11.00000 0.02620 0.02453 = 0.03956 0.00720 0.01421 0.00693 AU1 7 -0.001210 0.661966 0.735114 11.00000 0.01663 0.02490 = 0.02785 0.01232 0.00260 -0.00144 CL1 8 0.143986 0.193601 0.974772 11.00000 0.03555 0.04138 = 0.05884 0.01836 0.02521 0.00751 CL2 8 0.303434 0.402819 0.953548 11.00000 0.05457 0.03168 = 0.10483 0.01782 0.04950 0.01345 CL3 8 0.561262 1.024558 0.721383 11.00000 0.04160 0.06819 = 0.06112 0.01435 0.02041 0.02280 CL4 8 0.399893 0.895430 0.550400 11.00000 0.05897 0.07588 = 0.06860 0.00262 0.01960 0.00375 H1 2 -0.104024 0.391324 0.681114 11.00000 0.04586 HKLF 4 REM npm023 in P-1 REM R1 = 0.0650 for 7702 Fo > 4sig(Fo) and 0.0683 for all 8051 data REM 469 parameters refined using 0 restraints END WGHT 0.0000 49.6006 REM Highest difference peak 12.228, deepest hole -5.646, 1-sigma level 0.222 Q1 1 -0.0292 0.7076 0.7659 11.00000 0.05 12.23 Q2 1 -0.1783 0.5396 0.7509 11.00000 0.05 4.52 Q3 1 0.0442 0.5965 0.6910 11.00000 0.05 1.71 Q4 1 0.3329 0.4217 1.0329 11.00000 0.05 1.48 Q5 1 0.0015 1.0198 0.8022 11.00000 0.05 1.39 Q6 1 0.5000 1.0000 0.5000 10.50000 0.05 1.30 Q7 1 0.0813 0.6350 0.7096 11.00000 0.05 1.21 Q8 1 -0.0549 0.7536 0.8007 11.00000 0.05 1.15 Q9 1 -0.0843 0.7448 0.7956 11.00000 0.05 1.13 Q10 1 0.0145 0.9692 0.7687 11.00000 0.05 1.12 Q11 1 0.4548 0.8987 0.6359 11.00000 0.05 1.03 Q12 1 -0.2399 0.4347 0.5866 11.00000 0.05 1.01 Q13 1 -0.1196 0.7161 0.7626 11.00000 0.05 0.97 Q14 1 -0.0243 0.7261 0.3506 11.00000 0.05 0.88 Q15 1 -0.0415 0.3846 0.7798 11.00000 0.05 0.79 Q16 1 -0.0942 0.7560 0.7377 11.00000 0.05 0.77 Q17 1 -0.1006 0.6007 0.7376 11.00000 0.05 0.73 Q18 1 -0.4183 0.3944 0.6296 11.00000 0.05 0.73 Q19 1 -0.3321 0.5935 0.6167 11.00000 0.05 0.72 Q20 1 0.1240 0.2514 0.9975 11.00000 0.05 0.71 ;