Supplementary data for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Helgard G. Raubenheimer' _publ_contact_author_address ; Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, Matieland,7602, South Africa ; _publ_contact_author_email hgr@sun.ac.za _publ_contact_author_fax '+27 21 808 3849' _publ_contact_author_phone '+27 21 808 3850' loop_ _publ_author_name _publ_author_address 'Elzet Stander' ; Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, Mateiland, 7602, South Africa ; 'Catharine Esterhysen' ; Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, Mateiland, 7602, South Africa ; 'Jean McKenzie' ; Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, Mateiland, 7602, South Africa ; 'Stephanie Cronje' ; Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, Mateiland, 7602, South Africa ; 'Helgard G. Raubenehimer' ; Department of Chemistry and Polymer Science, University of Stellenbosch, Private Bag X1, Mateiland, 7602, South Africa ; _publ_section_title ; Reaction and subsequent transformation of anionic acetylide carbene complexes using the Ph3PAu+ fragment ; data_Complex_2a _database_code_depnum_ccdc_archive 'CCDC 650396' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H21 Au Cr N O5 P, C H2 Cl2' _chemical_formula_sum 'C29 H23 Au Cl2 Cr N O5 P' _chemical_formula_weight 816.32 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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 monoclinic _symmetry_space_group_name_H-M 'P 21/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 16.108(3) _cell_length_b 12.840(2) _cell_length_c 16.159(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.924(2) _cell_angle_gamma 90.00 _cell_volume 3005.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 8870 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 28.3 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 5.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.406 _exptl_absorpt_correction_T_max 0.492 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(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 CCD area-detector' _diffrn_measurement_method '\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 30199 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_av_sigmaI/netI 0.022 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 27.0 _reflns_number_total 6570 _reflns_number_gt 6152 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood and Barbour, 2003) ; _computing_publication_material ; X-Seed ; _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^)+(0.0228P)^2^+1.5502P] 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 6570 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.020 _refine_ls_R_factor_gt 0.018 _refine_ls_wR_factor_ref 0.045 _refine_ls_wR_factor_gt 0.045 _refine_ls_goodness_of_fit_ref 1.06 _refine_ls_restrained_S_all 1.06 _refine_ls_shift/su_max 0.004 _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 0.860975(5) 0.946097(6) 0.233632(5) 0.01565(3) Uani 1 1 d . . . C11A C 0.65927(15) 0.89963(17) 0.24775(14) 0.0165(4) Uani 1 1 d . . . C11C C 0.79681(14) 0.73664(16) 0.32002(14) 0.0157(4) Uani 1 1 d . . . C11B C 0.69263(14) 0.76203(16) 0.12240(14) 0.0161(4) Uani 1 1 d . . . C12B C 0.70527(16) 0.79203(18) 0.04595(16) 0.0219(5) Uani 1 1 d . . . H12B H 0.7440 0.8495 0.0502 0.026 Uiso 1 1 calc R . . C16B C 0.63581(16) 0.67710(18) 0.11537(15) 0.0206(5) Uani 1 1 d . . . H16B H 0.6273 0.6555 0.1674 0.025 Uiso 1 1 calc R . . C13B C 0.66122(17) 0.7380(2) -0.03687(16) 0.0272(5) Uani 1 1 d . . . H13B H 0.6699 0.7585 -0.0890 0.033 Uiso 1 1 calc R . . C14B C 0.60461(16) 0.65407(19) -0.04283(16) 0.0254(5) Uani 1 1 d . . . H14B H 0.5746 0.6170 -0.0991 0.030 Uiso 1 1 calc R . . C12A C 0.56507(15) 0.88249(18) 0.19495(16) 0.0207(5) Uani 1 1 d . . . H12A H 0.5446 0.8330 0.1463 0.025 Uiso 1 1 calc R . . C16A C 0.68819(16) 0.97327(18) 0.31869(16) 0.0223(5) Uani 1 1 d . . . H16A H 0.7522 0.9854 0.3548 0.027 Uiso 1 1 calc R . . C13C C 0.78245(17) 0.61699(18) 0.42813(16) 0.0246(5) Uani 1 1 d . . . H13C H 0.7463 0.5860 0.4547 0.030 Uiso 1 1 calc R . . C12C C 0.74406(16) 0.69220(18) 0.35951(15) 0.0210(5) Uani 1 1 d . . . H12C H 0.6817 0.7131 0.3397 0.025 Uiso 1 1 calc R . . C14C C 0.87371(18) 0.58786(19) 0.45721(17) 0.0287(6) Uani 1 1 d . . . H14C H 0.9002 0.5370 0.5043 0.034 Uiso 1 1 calc R . . C15A C 0.62410(18) 1.02851(19) 0.33658(18) 0.0270(5) Uani 1 1 d . . . H15A H 0.6441 1.0786 0.3847 0.032 Uiso 1 1 calc R . . C15B C 0.59176(16) 0.62427(18) 0.03277(16) 0.0242(5) Uani 1 1 d . . . H15B H 0.5525 0.5672 0.0281 0.029 Uiso 1 1 calc R . . C16C C 0.88819(16) 0.70643(18) 0.34977(16) 0.0232(5) Uani 1 1 d . . . H16C H 0.9246 0.7367 0.3231 0.028 Uiso 1 1 calc R . . C15C C 0.92627(17) 0.6319(2) 0.41855(18) 0.0302(6) Uani 1 1 d . . . H15C H 0.9888 0.6114 0.4389 0.036 Uiso 1 1 calc R . . C13A C 0.50132(17) 0.93822(19) 0.21388(18) 0.0255(5) Uani 1 1 d . . . H13A H 0.4372 0.9263 0.1781 0.031 Uiso 1 1 calc R . . C14A C 0.53010(17) 1.0106(2) 0.28392(18) 0.0273(5) Uani 1 1 d . . . H14A H 0.4860 1.0483 0.2962 0.033 Uiso 1 1 calc R . . N1 N 1.06467(12) 1.23766(15) 0.17070(13) 0.0194(4) Uani 1 1 d . . . C4 C 0.96869(16) 1.25258(19) 0.10036(16) 0.0231(5) Uani 1 1 d . . . H4A H 0.9342 1.1875 0.0922 0.035 Uiso 1 1 calc R . . H4B H 0.9688 1.2725 0.0419 0.035 Uiso 1 1 calc R . . H4C H 0.9393 1.3076 0.1203 0.035 Uiso 1 1 calc R . . C5 C 1.12896(17) 1.31151(18) 0.16079(17) 0.0253(5) Uani 1 1 d . . . H5A H 1.1901 1.3036 0.2127 0.038 Uiso 1 1 calc R . . H5B H 1.1067 1.3827 0.1599 0.038 Uiso 1 1 calc R . . H5C H 1.1332 1.2977 0.1031 0.038 Uiso 1 1 calc R . . Cl1 Cl 1.10995(4) 1.07518(5) 0.01357(4) 0.03057(14) Uani 1 1 d . . . C17 C 1.01097(16) 1.11820(18) -0.08406(16) 0.0243(5) Uani 1 1 d . . . H17A H 1.0006 1.0724 -0.1370 0.029 Uiso 1 1 calc R . . H17B H 0.9563 1.1129 -0.0714 0.029 Uiso 1 1 calc R . . Cl2 Cl 1.02300(5) 1.24737(6) -0.11272(5) 0.04459(18) Uani 1 1 d . . . C9 C 1.26265(16) 1.25841(19) 0.37477(16) 0.0233(5) Uani 1 1 d . . . O4 O 1.28979(13) 1.34067(14) 0.39891(13) 0.0337(4) Uani 1 1 d . . . C6 C 1.18234(15) 0.98093(19) 0.30247(15) 0.0186(4) Uani 1 1 d . . . C8 C 1.33193(17) 1.06614(18) 0.42639(16) 0.0224(5) Uani 1 1 d . . . C7 C 1.16664(15) 1.11954(18) 0.42228(16) 0.0214(5) Uani 1 1 d . . . C10 C 1.27281(16) 1.1188(2) 0.25282(16) 0.0245(5) Uani 1 1 d . . . O3 O 1.40027(12) 1.03012(15) 0.47864(12) 0.0319(4) Uani 1 1 d . . . O5 O 1.30714(13) 1.11381(16) 0.20416(13) 0.0356(4) Uani 1 1 d . . . P1 P 0.74971(4) 0.83380(4) 0.22919(4) 0.01494(11) Uani 1 1 d . . . Cr1 Cr 1.22088(2) 1.12038(3) 0.33768(2) 0.01724(8) Uani 1 1 d . . . C3 C 0.95868(16) 1.04407(16) 0.23838(16) 0.0176(4) Uani 1 1 d . . . C2 C 1.01539(15) 1.10399(17) 0.23424(14) 0.0173(4) Uani 1 1 d . . . C1 C 1.08957(15) 1.16588(17) 0.23532(15) 0.0168(4) Uani 1 1 d . . . O1 O 1.16226(12) 0.89573(14) 0.28191(12) 0.0250(4) Uani 1 1 d . . . O2 O 1.13485(12) 1.11941(15) 0.47322(12) 0.0301(4) 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 0.01255(5) 0.01445(5) 0.02043(5) -0.00092(3) 0.00765(4) -0.00272(3) C11A 0.0151(10) 0.0152(11) 0.0188(10) 0.0037(8) 0.0069(8) 0.0013(8) C11C 0.0141(10) 0.0140(10) 0.0160(10) -0.0023(8) 0.0037(8) -0.0007(8) C11B 0.0128(10) 0.0151(10) 0.0191(10) 0.0001(8) 0.0058(8) 0.0014(8) C12B 0.0226(12) 0.0213(12) 0.0252(12) -0.0018(9) 0.0136(10) -0.0035(9) C16B 0.0210(11) 0.0199(11) 0.0208(11) 0.0005(8) 0.0091(9) -0.0016(9) C13B 0.0315(13) 0.0334(14) 0.0200(11) -0.0025(10) 0.0144(10) -0.0012(11) C14B 0.0225(12) 0.0269(13) 0.0227(12) -0.0074(10) 0.0062(9) 0.0005(10) C12A 0.0166(11) 0.0222(12) 0.0215(11) -0.0010(9) 0.0066(9) -0.0003(9) C16A 0.0183(11) 0.0211(11) 0.0259(12) -0.0018(9) 0.0082(9) -0.0011(9) C13C 0.0314(13) 0.0202(12) 0.0211(11) -0.0001(9) 0.0104(10) -0.0036(10) C12C 0.0186(11) 0.0216(12) 0.0222(11) -0.0017(9) 0.0083(9) -0.0013(9) C14C 0.0332(14) 0.0198(12) 0.0222(12) 0.0035(9) 0.0020(10) 0.0034(11) C15A 0.0275(13) 0.0225(12) 0.0315(13) -0.0048(10) 0.0133(11) 0.0004(10) C15B 0.0206(12) 0.0200(11) 0.0290(12) -0.0043(9) 0.0081(10) -0.0052(9) C16C 0.0176(11) 0.0221(12) 0.0289(12) 0.0002(9) 0.0092(10) 0.0002(9) C15C 0.0208(12) 0.0278(13) 0.0344(14) 0.0030(10) 0.0049(10) 0.0087(10) C13A 0.0158(12) 0.0317(14) 0.0279(13) 0.0036(10) 0.0084(10) 0.0037(9) C14A 0.0247(13) 0.0251(13) 0.0362(14) 0.0013(10) 0.0170(11) 0.0070(10) N1 0.0158(9) 0.0187(9) 0.0229(9) 0.0013(7) 0.0076(8) -0.0024(7) C4 0.0188(11) 0.0236(12) 0.0242(12) 0.0040(9) 0.0070(9) 0.0023(9) C5 0.0237(12) 0.0226(12) 0.0319(13) 0.0061(10) 0.0144(10) -0.0054(10) Cl1 0.0257(3) 0.0341(3) 0.0292(3) 0.0063(2) 0.0094(2) 0.0013(3) C17 0.0227(12) 0.0214(12) 0.0273(12) 0.0009(9) 0.0096(10) 0.0006(10) Cl2 0.0454(4) 0.0307(4) 0.0510(4) 0.0157(3) 0.0149(3) -0.0050(3) C9 0.0176(11) 0.0276(13) 0.0253(12) -0.0003(10) 0.0099(9) -0.0027(10) O4 0.0342(10) 0.0287(10) 0.0379(10) -0.0073(8) 0.0156(8) -0.0119(8) C6 0.0134(10) 0.0245(12) 0.0192(11) 0.0014(9) 0.0083(9) 0.0030(9) C8 0.0191(12) 0.0257(12) 0.0221(12) -0.0061(9) 0.0087(10) -0.0021(9) C7 0.0176(11) 0.0207(11) 0.0218(11) -0.0014(9) 0.0048(9) -0.0031(9) C10 0.0150(11) 0.0299(13) 0.0254(12) 0.0016(10) 0.0059(9) -0.0023(9) O3 0.0207(9) 0.0362(10) 0.0295(10) -0.0057(8) 0.0024(8) 0.0064(8) O5 0.0282(10) 0.0525(13) 0.0338(10) 0.0049(9) 0.0206(8) 0.0030(9) P1 0.0122(3) 0.0144(3) 0.0175(3) -0.0003(2) 0.0058(2) -0.0014(2) Cr1 0.01238(17) 0.02016(18) 0.01850(17) -0.00125(13) 0.00611(14) -0.00216(14) C3 0.0146(11) 0.0172(11) 0.0219(11) -0.0008(8) 0.0087(9) 0.0015(8) C2 0.0147(10) 0.0173(11) 0.0172(10) -0.0012(8) 0.0046(8) 0.0014(8) C1 0.0149(10) 0.0169(11) 0.0209(11) -0.0019(8) 0.0100(8) -0.0010(8) O1 0.0215(8) 0.0217(9) 0.0305(9) -0.0015(7) 0.0101(7) 0.0017(7) O2 0.0305(10) 0.0369(10) 0.0271(9) -0.0040(8) 0.0166(8) -0.0051(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C3 1.990(2) . ? Au1 P1 2.2768(6) . ? C11A C12A 1.395(3) . ? C11A C16A 1.399(3) . ? C11A P1 1.819(2) . ? C11C C12C 1.389(3) . ? C11C C16C 1.389(3) . ? C11C P1 1.820(2) . ? C11B C12B 1.391(3) . ? C11B C16B 1.396(3) . ? C11B P1 1.812(2) . ? C12B C13B 1.395(3) . ? C12B H12B 0.9500 . ? C16B C15B 1.385(3) . ? C16B H16B 0.9500 . ? C13B C14B 1.387(4) . ? C13B H13B 0.9500 . ? C14B C15B 1.379(3) . ? C14B H14B 0.9500 . ? C12A C13A 1.391(3) . ? C12A H12A 0.9500 . ? C16A C15A 1.383(3) . ? C16A H16A 0.9500 . ? C13C C14C 1.385(4) . ? C13C C12C 1.395(3) . ? C13C H13C 0.9500 . ? C12C H12C 0.9500 . ? C14C C15C 1.375(4) . ? C14C H14C 0.9500 . ? C15A C14A 1.394(4) . ? C15A H15A 0.9500 . ? C15B H15B 0.9500 . ? C16C C15C 1.389(3) . ? C16C H16C 0.9500 . ? C15C H15C 0.9500 . ? C13A C14A 1.379(4) . ? C13A H13A 0.9500 . ? C14A H14A 0.9500 . ? N1 C1 1.317(3) . ? N1 C5 1.464(3) . ? N1 C4 1.477(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? Cl1 C17 1.771(2) . ? C17 Cl2 1.755(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C9 O4 1.144(3) . ? C9 Cr1 1.897(2) . ? C6 O1 1.148(3) . ? C6 Cr1 1.899(2) . ? C8 O3 1.151(3) . ? C8 Cr1 1.870(2) . ? C7 O2 1.144(3) . ? C7 Cr1 1.918(2) . ? C10 O5 1.144(3) . ? C10 Cr1 1.893(3) . ? Cr1 C1 2.120(2) . ? C3 C2 1.218(3) . ? C2 C1 1.429(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 C3 Au1 P1 179.63(7) . . ? C12A C11A C16A 119.4(2) . . ? C12A C11A P1 124.13(17) . . ? C16A C11A P1 116.44(17) . . ? C12C C11C C16C 119.7(2) . . ? C12C C11C P1 121.95(16) . . ? C16C C11C P1 118.39(17) . . ? C12B C11B C16B 119.3(2) . . ? C12B C11B P1 119.63(17) . . ? C16B C11B P1 121.08(17) . . ? C11B C12B C13B 120.2(2) . . ? C11B C12B H12B 119.9 . . ? C13B C12B H12B 119.9 . . ? C15B C16B C11B 120.2(2) . . ? C15B C16B H16B 119.9 . . ? C11B C16B H16B 119.9 . . ? C14B C13B C12B 119.8(2) . . ? C14B C13B H13B 120.1 . . ? C12B C13B H13B 120.1 . . ? C15B C14B C13B 120.2(2) . . ? C15B C14B H14B 119.9 . . ? C13B C14B H14B 119.9 . . ? C13A C12A C11A 119.6(2) . . ? C13A C12A H12A 120.2 . . ? C11A C12A H12A 120.2 . . ? C15A C16A C11A 120.4(2) . . ? C15A C16A H16A 119.8 . . ? C11A C16A H16A 119.8 . . ? C14C C13C C12C 119.5(2) . . ? C14C C13C H13C 120.2 . . ? C12C C13C H13C 120.2 . . ? C11C C12C C13C 120.1(2) . . ? C11C C12C H12C 119.9 . . ? C13C C12C H12C 119.9 . . ? C15C C14C C13C 120.5(2) . . ? C15C C14C H14C 119.7 . . ? C13C C14C H14C 119.7 . . ? C16A C15A C14A 119.9(2) . . ? C16A C15A H15A 120.0 . . ? C14A C15A H15A 120.0 . . ? C14B C15B C16B 120.4(2) . . ? C14B C15B H15B 119.8 . . ? C16B C15B H15B 119.8 . . ? C15C C16C C11C 120.0(2) . . ? C15C C16C H16C 120.0 . . ? C11C C16C H16C 120.0 . . ? C14C C15C C16C 120.2(2) . . ? C14C C15C H15C 119.9 . . ? C16C C15C H15C 119.9 . . ? C14A C13A C12A 120.8(2) . . ? C14A C13A H13A 119.6 . . ? C12A C13A H13A 119.6 . . ? C13A C14A C15A 119.9(2) . . ? C13A C14A H14A 120.1 . . ? C15A C14A H14A 120.1 . . ? C1 N1 C5 123.73(19) . . ? C1 N1 C4 123.67(19) . . ? C5 N1 C4 112.60(18) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Cl2 C17 Cl1 111.68(13) . . ? Cl2 C17 H17A 109.3 . . ? Cl1 C17 H17A 109.3 . . ? Cl2 C17 H17B 109.3 . . ? Cl1 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? O4 C9 Cr1 178.3(2) . . ? O1 C6 Cr1 177.54(19) . . ? O3 C8 Cr1 177.5(2) . . ? O2 C7 Cr1 179.5(2) . . ? O5 C10 Cr1 176.4(2) . . ? C11B P1 C11A 106.49(10) . . ? C11B P1 C11C 106.16(10) . . ? C11A P1 C11C 105.49(10) . . ? C11B P1 Au1 114.62(7) . . ? C11A P1 Au1 112.13(7) . . ? C11C P1 Au1 111.34(7) . . ? C8 Cr1 C10 88.51(10) . . ? C8 Cr1 C9 91.00(10) . . ? C10 Cr1 C9 91.75(11) . . ? C8 Cr1 C6 87.50(10) . . ? C10 Cr1 C6 87.90(10) . . ? C9 Cr1 C6 178.47(10) . . ? C8 Cr1 C7 91.87(10) . . ? C10 Cr1 C7 178.80(10) . . ? C9 Cr1 C7 89.38(10) . . ? C6 Cr1 C7 90.98(10) . . ? C8 Cr1 C1 174.05(9) . . ? C10 Cr1 C1 92.51(9) . . ? C9 Cr1 C1 94.82(9) . . ? C6 Cr1 C1 86.68(9) . . ? C7 Cr1 C1 87.00(9) . . ? C2 C3 Au1 175.2(2) . . ? C3 C2 C1 173.6(2) . . ? N1 C1 C2 114.61(19) . . ? N1 C1 Cr1 131.75(16) . . ? C2 C1 Cr1 113.58(15) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cr1 C1 C2 C3 -17(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.0 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.21 _refine_diff_density_min -0.32 _refine_diff_density_rms 0.09 #====END data_Complex_2b _database_code_depnum_ccdc_archive 'CCDC 650397' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H21 Au N O5 P W, C H2 Cl2' _chemical_formula_sum 'C29 H23 Au Cl2 N O5 P W' _chemical_formula_weight 948.17 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/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 16.326(3) _cell_length_b 12.7472(19) _cell_length_c 16.336(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.163(2) _cell_angle_gamma 90.00 _cell_volume 3051.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6224 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.2 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 8.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.417 _exptl_absorpt_correction_T_max 0.538 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _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 CCD area-detector' _diffrn_measurement_method '\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 18062 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.050 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _reflns_number_total 6625 _reflns_number_gt 5846 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood and Barbour, 2003) ; _computing_publication_material ; X-Seed ; _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^)+(0.0341P)^2^+3.9960P] 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 6625 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.041 _refine_ls_R_factor_gt 0.035 _refine_ls_wR_factor_ref 0.080 _refine_ls_wR_factor_gt 0.077 _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_restrained_S_all 1.05 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.266090(14) 0.943003(16) 0.138996(14) 0.01554(7) Uani 1 1 d . . . W1 W 0.160019(14) 1.116114(17) -0.222719(14) 0.01617(7) Uani 1 1 d . . . P1 P 0.27027(9) 0.83135(11) 0.24957(9) 0.0147(3) Uani 1 1 d . . . O1 O 0.2201(3) 0.8811(3) -0.1585(3) 0.0253(9) Uani 1 1 d . . . O2 O 0.0225(3) 1.1201(3) -0.1313(3) 0.0291(10) Uani 1 1 d . . . O5 O 0.2969(3) 1.1093(4) -0.3133(3) 0.0347(11) Uani 1 1 d . . . N1 N 0.3308(3) 1.2379(4) -0.0594(3) 0.0199(10) Uani 1 1 d . . . O4 O 0.1006(3) 1.3490(3) -0.2950(3) 0.0341(11) Uani 1 1 d . . . C11A C 0.3774(4) 0.7600(4) 0.3071(4) 0.0152(11) Uani 1 1 d . . . C10 C 0.2489(4) 1.1138(4) -0.2788(4) 0.0215(12) Uani 1 1 d . . . C7 C 0.0711(4) 1.1185(4) -0.1643(4) 0.0223(13) Uani 1 1 d . . . C3 C 0.2628(4) 1.0416(4) 0.0423(4) 0.0185(12) Uani 1 1 d . . . C1 C 0.2666(4) 1.1648(4) -0.0849(4) 0.0173(11) Uani 1 1 d . . . C2 C 0.2678(4) 1.1009(4) -0.0126(4) 0.0164(11) Uani 1 1 d . . . C9 C 0.1219(4) 1.2649(5) -0.2678(4) 0.0232(13) Uani 1 1 d . . . C11B C 0.2529(4) 0.8990(4) 0.3384(4) 0.0164(11) Uani 1 1 d . . . C11C C 0.1797(4) 0.7342(4) 0.2041(4) 0.0170(11) Uani 1 1 d . . . O3 O 0.0106(3) 1.0188(4) -0.4055(3) 0.0305(10) Uani 1 1 d . . . C12B C 0.3052(4) 0.8823(4) 0.4318(4) 0.0223(12) Uani 1 1 d . . . H12B H 0.3530 0.8320 0.4522 0.027 Uiso 1 1 calc R . . C13C C 0.0720(4) 0.6144(4) 0.2201(5) 0.0245(13) Uani 1 1 d . . . H13C H 0.0468 0.5831 0.2566 0.029 Uiso 1 1 calc R . . C16C C 0.1480(4) 0.7036(4) 0.1138(4) 0.0224(12) Uani 1 1 d . . . H16C H 0.1741 0.7332 0.0773 0.027 Uiso 1 1 calc R . . C6 C 0.1982(4) 0.9654(5) -0.1805(4) 0.0172(11) Uani 1 1 d . . . C12C C 0.1417(4) 0.6909(4) 0.2572(4) 0.0195(12) Uani 1 1 d . . . H12C H 0.1625 0.7126 0.3188 0.023 Uiso 1 1 calc R . . C16A C 0.3841(4) 0.6749(4) 0.3637(4) 0.0209(12) Uani 1 1 d . . . H16A H 0.3324 0.6522 0.3712 0.025 Uiso 1 1 calc R . . C16B C 0.1837(4) 0.9740(5) 0.3099(4) 0.0218(12) Uani 1 1 d . . . H16B H 0.1478 0.9863 0.2467 0.026 Uiso 1 1 calc R . . C8 C 0.0637(4) 1.0560(4) -0.3387(4) 0.0202(12) Uani 1 1 d . . . C13B C 0.2875(4) 0.9390(5) 0.4948(4) 0.0265(14) Uani 1 1 d . . . H13B H 0.3230 0.9272 0.5583 0.032 Uiso 1 1 calc R . . C14A C 0.5421(4) 0.6556(5) 0.3965(4) 0.0264(14) Uani 1 1 d . . . H14A H 0.5986 0.6199 0.4274 0.032 Uiso 1 1 calc R . . C4 C 0.3997(4) 1.2538(5) 0.0352(4) 0.0257(13) Uani 1 1 d . . . H4A H 0.4049 1.1900 0.0706 0.039 Uiso 1 1 calc R . . H4B H 0.3812 1.3125 0.0621 0.039 Uiso 1 1 calc R . . H4C H 0.4588 1.2696 0.0360 0.039 Uiso 1 1 calc R . . C14C C 0.0416(4) 0.5861(5) 0.1300(4) 0.0272(14) Uani 1 1 d . . . H14C H -0.0057 0.5355 0.1042 0.033 Uiso 1 1 calc R . . C12A C 0.4517(4) 0.7908(4) 0.2948(4) 0.0227(12) Uani 1 1 d . . . H12A H 0.4466 0.8479 0.2555 0.027 Uiso 1 1 calc R . . C14B C 0.2184(4) 1.0125(5) 0.4654(4) 0.0269(14) Uani 1 1 d . . . H14B H 0.2063 1.0506 0.5088 0.032 Uiso 1 1 calc R . . C15A C 0.4671(4) 0.6242(5) 0.4087(4) 0.0242(13) Uani 1 1 d . . . H15A H 0.4726 0.5673 0.4483 0.029 Uiso 1 1 calc R . . C5 C 0.3394(4) 1.3130(5) -0.1238(4) 0.0260(13) Uani 1 1 d . . . H5A H 0.4011 1.3091 -0.1195 0.039 Uiso 1 1 calc R . . H5B H 0.3279 1.3842 -0.1088 0.039 Uiso 1 1 calc R . . H5C H 0.2948 1.2956 -0.1861 0.039 Uiso 1 1 calc R . . C13A C 0.5351(4) 0.7383(5) 0.3400(4) 0.0276(14) Uani 1 1 d . . . H13A H 0.5866 0.7599 0.3317 0.033 Uiso 1 1 calc R . . C15B C 0.1671(4) 1.0311(5) 0.3741(4) 0.0263(13) Uani 1 1 d . . . H15B H 0.1204 1.0828 0.3546 0.032 Uiso 1 1 calc R . . C15C C 0.0786(4) 0.6300(5) 0.0763(4) 0.0301(15) Uani 1 1 d . . . H15C H 0.0567 0.6099 0.0142 0.036 Uiso 1 1 calc R . . Cl1 Cl 0.48564(11) 1.07587(13) -0.11046(11) 0.0329(4) Uani 1 1 d . . . Cl2 Cl 0.60381(13) 1.25417(14) -0.02442(13) 0.0482(5) Uani 1 1 d . . . C17 C 0.5817(4) 1.1213(4) -0.0135(4) 0.0232(13) Uani 1 1 d . . . H17A H 0.5710 1.1122 0.0412 0.028 Uiso 1 1 calc R . . H17B H 0.6357 1.0789 -0.0049 0.028 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 0.02039(12) 0.01326(11) 0.01347(11) 0.00284(8) 0.00790(9) 0.00130(8) W1 0.01711(12) 0.01794(12) 0.01269(12) 0.00241(8) 0.00587(9) 0.00079(8) P1 0.0156(7) 0.0144(7) 0.0134(7) 0.0020(5) 0.0056(6) 0.0001(5) O1 0.028(2) 0.019(2) 0.027(2) -0.0004(18) 0.0115(19) 0.0026(17) O2 0.031(2) 0.030(2) 0.032(3) 0.0043(19) 0.020(2) 0.0037(19) O5 0.034(3) 0.047(3) 0.031(3) -0.002(2) 0.021(2) -0.005(2) N1 0.023(2) 0.017(2) 0.021(3) 0.0000(19) 0.012(2) -0.001(2) O4 0.038(3) 0.023(2) 0.041(3) 0.010(2) 0.017(2) 0.004(2) C11A 0.018(3) 0.014(3) 0.014(3) 0.000(2) 0.006(2) 0.003(2) C10 0.022(3) 0.022(3) 0.016(3) -0.001(2) 0.005(2) -0.004(2) C7 0.023(3) 0.021(3) 0.017(3) -0.001(2) 0.002(3) 0.003(2) C3 0.021(3) 0.014(3) 0.017(3) -0.001(2) 0.005(2) 0.002(2) C1 0.024(3) 0.011(3) 0.022(3) 0.001(2) 0.015(2) 0.005(2) C2 0.016(3) 0.013(3) 0.017(3) -0.001(2) 0.004(2) -0.001(2) C9 0.020(3) 0.025(3) 0.026(3) 0.002(3) 0.011(3) 0.000(2) C11B 0.017(3) 0.017(3) 0.018(3) -0.001(2) 0.010(2) -0.003(2) C11C 0.017(3) 0.011(3) 0.020(3) 0.002(2) 0.005(2) 0.002(2) O3 0.027(2) 0.034(3) 0.023(2) -0.0054(19) 0.004(2) 0.003(2) C12B 0.023(3) 0.021(3) 0.020(3) 0.003(2) 0.007(2) -0.001(2) C13C 0.019(3) 0.016(3) 0.038(4) -0.001(3) 0.012(3) -0.006(2) C16C 0.030(3) 0.020(3) 0.016(3) 0.001(2) 0.009(3) 0.001(2) C6 0.018(3) 0.026(3) 0.009(3) 0.000(2) 0.008(2) -0.003(2) C12C 0.017(3) 0.016(3) 0.020(3) -0.001(2) 0.004(2) -0.002(2) C16A 0.021(3) 0.017(3) 0.023(3) 0.003(2) 0.009(2) -0.001(2) C16B 0.025(3) 0.022(3) 0.017(3) 0.000(2) 0.007(2) 0.004(2) C8 0.019(3) 0.020(3) 0.020(3) -0.002(2) 0.008(3) 0.004(2) C13B 0.023(3) 0.034(4) 0.016(3) 0.001(3) 0.003(3) -0.002(3) C14A 0.020(3) 0.029(3) 0.024(3) -0.001(3) 0.004(3) 0.011(3) C4 0.032(3) 0.026(3) 0.018(3) 0.001(2) 0.009(3) -0.002(3) C14C 0.023(3) 0.020(3) 0.031(4) -0.004(3) 0.005(3) 0.000(2) C12A 0.027(3) 0.017(3) 0.026(3) 0.003(2) 0.014(3) 0.004(2) C14B 0.040(4) 0.024(3) 0.025(3) -0.003(3) 0.021(3) 0.004(3) C15A 0.027(3) 0.022(3) 0.020(3) 0.004(2) 0.008(3) 0.006(2) C5 0.030(3) 0.019(3) 0.030(3) 0.006(3) 0.015(3) -0.003(3) C13A 0.019(3) 0.030(3) 0.034(4) 0.000(3) 0.012(3) 0.003(3) C15B 0.030(3) 0.019(3) 0.029(3) -0.002(3) 0.013(3) 0.005(3) C15C 0.030(3) 0.034(4) 0.017(3) -0.009(3) 0.002(3) -0.007(3) Cl1 0.0314(8) 0.0336(9) 0.0293(8) -0.0045(7) 0.0094(7) -0.0079(7) Cl2 0.0523(11) 0.0318(10) 0.0482(11) 0.0062(8) 0.0111(9) -0.0185(8) C17 0.028(3) 0.014(3) 0.024(3) -0.001(2) 0.008(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 C3 2.000(6) . ? Au1 P1 2.2770(14) . ? W1 C8 2.006(6) . ? W1 C10 2.030(6) . ? W1 C9 2.030(6) . ? W1 C6 2.044(6) . ? W1 C7 2.060(6) . ? W1 C1 2.242(6) . ? P1 C11B 1.815(6) . ? P1 C11C 1.818(5) . ? P1 C11A 1.822(5) . ? O1 C6 1.140(7) . ? O2 C7 1.139(7) . ? O5 C10 1.150(7) . ? N1 C1 1.325(7) . ? N1 C4 1.470(7) . ? N1 C5 1.474(7) . ? O4 C9 1.154(7) . ? C11A C12A 1.372(8) . ? C11A C16A 1.399(8) . ? C3 C2 1.203(8) . ? C1 C2 1.429(8) . ? C11B C16B 1.393(8) . ? C11B C12B 1.398(8) . ? C11C C12C 1.384(8) . ? C11C C16C 1.387(8) . ? O3 C8 1.154(7) . ? C12B C13B 1.388(9) . ? C12B H12B 0.9500 . ? C13C C14C 1.378(9) . ? C13C C12C 1.416(7) . ? C13C H13C 0.9500 . ? C16C C15C 1.388(8) . ? C16C H16C 0.9500 . ? C12C H12C 0.9500 . ? C16A C15A 1.384(8) . ? C16A H16A 0.9500 . ? C16B C15B 1.398(8) . ? C16B H16B 0.9500 . ? C13B C14B 1.379(8) . ? C13B H13B 0.9500 . ? C14A C13A 1.372(9) . ? C14A C15A 1.383(9) . ? C14A H14A 0.9500 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C14C C15C 1.384(9) . ? C14C H14C 0.9500 . ? C12A C13A 1.400(8) . ? C12A H12A 0.9500 . ? C14B C15B 1.371(9) . ? C14B H14B 0.9500 . ? C15A H15A 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C13A H13A 0.9500 . ? C15B H15B 0.9500 . ? C15C H15C 0.9500 . ? Cl1 C17 1.764(6) . ? Cl2 C17 1.757(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? 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 C3 Au1 P1 179.71(18) . . ? C8 W1 C10 89.2(2) . . ? C8 W1 C9 91.6(2) . . ? C10 W1 C9 90.9(2) . . ? C8 W1 C6 87.4(2) . . ? C10 W1 C6 88.1(2) . . ? C9 W1 C6 178.6(2) . . ? C8 W1 C7 91.4(2) . . ? C10 W1 C7 179.3(2) . . ? C9 W1 C7 89.3(2) . . ? C6 W1 C7 91.7(2) . . ? C8 W1 C1 173.0(2) . . ? C10 W1 C1 93.7(2) . . ? C9 W1 C1 94.8(2) . . ? C6 W1 C1 86.3(2) . . ? C7 W1 C1 85.7(2) . . ? C11B P1 C11C 105.3(3) . . ? C11B P1 C11A 106.1(2) . . ? C11C P1 C11A 107.1(2) . . ? C11B P1 Au1 112.13(18) . . ? C11C P1 Au1 111.55(18) . . ? C11A P1 Au1 114.02(18) . . ? C1 N1 C4 124.0(5) . . ? C1 N1 C5 122.9(5) . . ? C4 N1 C5 113.1(5) . . ? C12A C11A C16A 120.1(5) . . ? C12A C11A P1 119.5(4) . . ? C16A C11A P1 120.4(4) . . ? O5 C10 W1 177.0(5) . . ? O2 C7 W1 179.5(5) . . ? C2 C3 Au1 175.1(5) . . ? N1 C1 C2 114.9(5) . . ? N1 C1 W1 131.8(4) . . ? C2 C1 W1 113.2(4) . . ? C3 C2 C1 174.0(6) . . ? O4 C9 W1 178.5(5) . . ? C16B C11B C12B 119.0(5) . . ? C16B C11B P1 116.6(4) . . ? C12B C11B P1 124.4(4) . . ? C12C C11C C16C 119.7(5) . . ? C12C C11C P1 121.6(4) . . ? C16C C11C P1 118.7(4) . . ? C13B C12B C11B 120.2(5) . . ? C13B C12B H12B 119.9 . . ? C11B C12B H12B 119.9 . . ? C14C C13C C12C 118.8(6) . . ? C14C C13C H13C 120.6 . . ? C12C C13C H13C 120.6 . . ? C11C C16C C15C 120.6(6) . . ? C11C C16C H16C 119.7 . . ? C15C C16C H16C 119.7 . . ? O1 C6 W1 178.5(5) . . ? C11C C12C C13C 120.2(6) . . ? C11C C12C H12C 119.9 . . ? C13C C12C H12C 119.9 . . ? C15A C16A C11A 119.1(5) . . ? C15A C16A H16A 120.5 . . ? C11A C16A H16A 120.5 . . ? C11B C16B C15B 120.2(5) . . ? C11B C16B H16B 119.9 . . ? C15B C16B H16B 119.9 . . ? O3 C8 W1 177.5(5) . . ? C14B C13B C12B 120.0(6) . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C13A C14A C15A 120.2(5) . . ? C13A C14A H14A 119.9 . . ? C15A C14A H14A 119.9 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C13C C14C C15C 121.3(6) . . ? C13C C14C H14C 119.4 . . ? C15C C14C H14C 119.4 . . ? C11A C12A C13A 120.3(5) . . ? C11A C12A H12A 119.9 . . ? C13A C12A H12A 119.9 . . ? C15B C14B C13B 120.7(6) . . ? C15B C14B H14B 119.6 . . ? C13B C14B H14B 119.6 . . ? C14A C15A C16A 120.7(6) . . ? C14A C15A H15A 119.7 . . ? C16A C15A H15A 119.7 . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C14A C13A C12A 119.7(6) . . ? C14A C13A H13A 120.2 . . ? C12A C13A H13A 120.2 . . ? C14B C15B C16B 119.8(6) . . ? C14B C15B H15B 120.1 . . ? C16B C15B H15B 120.1 . . ? C14C C15C C16C 119.5(6) . . ? C14C C15C H15C 120.2 . . ? C16C C15C H15C 120.2 . . ? Cl2 C17 Cl1 111.5(3) . . ? Cl2 C17 H17A 109.3 . . ? Cl1 C17 H17A 109.3 . . ? Cl2 C17 H17B 109.3 . . ? Cl1 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.0 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.63 _refine_diff_density_min -0.74 _refine_diff_density_rms 0.192 #====END data_Complex_3a _database_code_depnum_ccdc_archive 'CCDC 650398' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H21 Au Cr N O5 P' _chemical_formula_sum 'C28 H21 Au Cr N O5 P' _chemical_formula_weight 731.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cr Cr 0.3209 0.6236 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.364(3) _cell_length_b 11.566(3) _cell_length_c 12.463(4) _cell_angle_alpha 74.216(14) _cell_angle_beta 69.976(5) _cell_angle_gamma 82.605(8) _cell_volume 1349.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1374 _cell_measurement_theta_min 4.39 _cell_measurement_theta_max 36.31 _exptl_crystal_description Prisms _exptl_crystal_colour 'Red orange' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.800 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_absorpt_coefficient_mu 5.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5886 _exptl_absorpt_correction_T_max 0.6484 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _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 CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14294 _diffrn_reflns_av_R_equivalents 0.103 _diffrn_reflns_av_sigmaI/netI 0.153 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 26.8 _reflns_number_total 5629 _reflns_number_gt 3999 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood and Barbour, 2003) ; _computing_publication_material ; X-Seed ; _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^)+(0.0635P)^2^+6.9423P] 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 5629 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1156 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.1808 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.64447(6) 0.21674(5) 0.46093(5) 0.02318(19) Uani 1 1 d . . . Cr1 Cr 0.6898(2) 0.37070(18) 0.86529(19) 0.0223(5) Uani 1 1 d . . . P1 P 0.7742(4) 0.1047(3) 0.3321(3) 0.0217(8) Uani 1 1 d . . . O1 O 0.9854(11) 0.4187(10) 0.7123(10) 0.045(3) Uani 1 1 d . . . O2 O 0.6157(11) 0.6367(8) 0.7812(9) 0.035(2) Uani 1 1 d . . . O3 O 0.7119(10) 0.4151(9) 1.0873(9) 0.032(2) Uani 1 1 d . . . O4 O 0.3918(11) 0.3036(9) 0.9896(9) 0.035(2) Uani 1 1 d . . . O5 O 0.7783(10) 0.1055(8) 0.9258(8) 0.032(2) Uani 1 1 d . . . N1 N 0.4058(12) 0.3659(10) 0.5804(10) 0.028(3) Uani 1 1 d . . . C1 C 0.5334(16) 0.3130(13) 0.5733(14) 0.037(4) Uani 1 1 d . . . C2 C 0.5936(14) 0.3398(11) 0.6541(12) 0.025(3) Uani 1 1 d . . . C3 C 0.6421(14) 0.3482(11) 0.7274(12) 0.026(3) Uani 1 1 d . . . C4 C 0.3334(15) 0.3478(13) 0.5077(12) 0.032(3) Uani 1 1 d . . . H4A H 0.3795 0.2826 0.4703 0.048 Uiso 1 1 calc R . . H4B H 0.3321 0.4219 0.4468 0.048 Uiso 1 1 calc R . . H4C H 0.2389 0.3264 0.5561 0.048 Uiso 1 1 calc R . . C5 C 0.3261(15) 0.4357(13) 0.6669(12) 0.031(3) Uani 1 1 d . . . H5C H 0.3794 0.4393 0.7173 0.046 Uiso 1 1 calc R . . H5B H 0.2394 0.3967 0.7155 0.046 Uiso 1 1 calc R . . H5A H 0.3065 0.5174 0.6251 0.046 Uiso 1 1 calc R . . C6 C 0.8760(15) 0.4032(12) 0.7712(13) 0.026(3) Uani 1 1 d . . . C7 C 0.6453(14) 0.5363(14) 0.8156(12) 0.027(3) Uani 1 1 d . . . C8 C 0.7076(14) 0.3951(12) 1.0023(14) 0.028(3) Uani 1 1 d . . . C9 C 0.5040(16) 0.3316(12) 0.9442(12) 0.027(3) Uani 1 1 d . . . C10 C 0.7459(14) 0.2042(13) 0.9037(12) 0.027(3) Uani 1 1 d . . . C11A C 0.8688(13) -0.0216(11) 0.3958(11) 0.020(3) Uani 1 1 d . . . C11B C 0.6681(14) 0.0407(11) 0.2736(11) 0.023(3) Uani 1 1 d . . . C11C C 0.8943(13) 0.1921(12) 0.2011(11) 0.023(3) Uani 1 1 d . . . C12A C 0.8141(15) -0.0803(12) 0.5130(12) 0.029(3) Uani 1 1 d . . . H12A H 0.7294 -0.0513 0.5598 0.034 Uiso 1 1 calc R . . C12B C 0.7026(15) -0.0691(11) 0.2421(12) 0.025(3) Uani 1 1 d . . . H12B H 0.7794 -0.1161 0.2575 0.030 Uiso 1 1 calc R . . C12C C 0.9405(13) 0.1611(11) 0.0943(12) 0.022(3) Uani 1 1 d . . . H12C H 0.9092 0.0901 0.0885 0.027 Uiso 1 1 calc R . . C13A C 0.8802(17) -0.1795(13) 0.5626(13) 0.038(4) Uani 1 1 d . . . H13A H 0.8393 -0.2201 0.6426 0.045 Uiso 1 1 calc R . . C13B C 0.6273(14) -0.1103(12) 0.1893(13) 0.028(3) Uani 1 1 d . . . H13B H 0.6527 -0.1845 0.1672 0.034 Uiso 1 1 calc R . . C13C C 1.0311(14) 0.2310(13) -0.0041(13) 0.032(3) Uani 1 1 d . . . H13C H 1.0599 0.2103 -0.0778 0.039 Uiso 1 1 calc R . . C14A C 1.0060(17) -0.2216(13) 0.4978(13) 0.036(4) Uani 1 1 d . . . H14A H 1.0508 -0.2912 0.5326 0.043 Uiso 1 1 calc R . . C14B C 0.5151(16) -0.0431(14) 0.1687(13) 0.034(4) Uani 1 1 d . . . H14B H 0.4618 -0.0713 0.1330 0.041 Uiso 1 1 calc R . . C14C C 1.0798(14) 0.3339(13) 0.0073(13) 0.032(4) Uani 1 1 d . . . H14C H 1.1422 0.3827 -0.0598 0.039 Uiso 1 1 calc R . . C15A C 1.0661(17) -0.1604(13) 0.3809(13) 0.037(4) Uani 1 1 d . . . H15A H 1.1531 -0.1872 0.3357 0.044 Uiso 1 1 calc R . . C15B C 0.4799(16) 0.0642(13) 0.1996(12) 0.034(4) Uani 1 1 d . . . H15B H 0.4022 0.1102 0.1848 0.040 Uiso 1 1 calc R . . C15C C 1.0407(15) 0.3642(13) 0.1092(12) 0.029(3) Uani 1 1 d . . . H15C H 1.0762 0.4335 0.1146 0.035 Uiso 1 1 calc R . . C16A C 0.9985(16) -0.0605(14) 0.3310(13) 0.038(4) Uani 1 1 d . . . H16A H 1.0405 -0.0179 0.2519 0.046 Uiso 1 1 calc R . . C16B C 0.5574(14) 0.1077(12) 0.2532(12) 0.027(3) Uani 1 1 d . . . H16B H 0.5326 0.1824 0.2744 0.033 Uiso 1 1 calc R . . C16C C 0.9472(15) 0.2949(11) 0.2093(12) 0.027(3) Uani 1 1 d . . . H16C H 0.9196 0.3168 0.2823 0.032 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 0.0310(3) 0.0151(3) 0.0225(3) -0.00359(18) -0.0097(2) 0.0029(2) Cr1 0.0249(12) 0.0166(11) 0.0260(12) -0.0037(9) -0.0101(10) -0.0007(9) P1 0.029(2) 0.0132(16) 0.0200(18) -0.0013(13) -0.0062(15) 0.0000(14) O1 0.023(6) 0.046(7) 0.060(8) -0.024(6) 0.001(6) -0.001(5) O2 0.046(7) 0.018(5) 0.037(6) -0.004(4) -0.015(5) 0.011(5) O3 0.035(6) 0.034(6) 0.032(6) -0.011(5) -0.014(5) -0.004(5) O4 0.028(6) 0.033(6) 0.040(6) -0.002(5) -0.008(5) -0.009(5) O5 0.038(6) 0.021(5) 0.033(6) 0.001(4) -0.010(5) -0.003(5) N1 0.028(7) 0.022(6) 0.029(7) -0.001(5) -0.005(5) -0.002(5) C1 0.039(9) 0.027(8) 0.040(9) 0.013(7) -0.022(8) -0.004(7) C2 0.022(8) 0.016(7) 0.026(8) 0.006(6) -0.004(6) 0.002(6) C3 0.027(8) 0.010(6) 0.032(8) 0.005(5) -0.010(7) 0.004(5) C4 0.034(9) 0.031(8) 0.027(8) -0.002(6) -0.010(7) -0.001(7) C5 0.029(8) 0.029(8) 0.024(8) -0.002(6) -0.002(6) 0.005(6) C6 0.026(8) 0.021(7) 0.033(8) -0.003(6) -0.016(7) -0.001(6) C7 0.026(8) 0.040(9) 0.016(7) -0.008(6) -0.004(6) -0.010(7) C8 0.019(8) 0.018(7) 0.043(9) -0.010(6) -0.004(7) -0.004(6) C9 0.038(9) 0.024(7) 0.026(8) -0.010(6) -0.016(7) 0.002(7) C10 0.024(8) 0.028(8) 0.028(8) 0.000(6) -0.011(6) -0.004(6) C11A 0.022(7) 0.015(6) 0.019(7) 0.001(5) -0.004(6) -0.005(5) C11B 0.028(8) 0.016(6) 0.018(7) 0.002(5) -0.002(6) -0.006(6) C11C 0.016(7) 0.029(7) 0.017(7) 0.004(5) -0.005(6) 0.000(6) C12A 0.034(9) 0.022(7) 0.031(8) -0.002(6) -0.014(7) -0.005(6) C12B 0.036(8) 0.010(6) 0.030(8) -0.001(5) -0.014(7) -0.001(6) C12C 0.025(8) 0.011(6) 0.030(8) -0.002(5) -0.009(6) -0.006(5) C13A 0.050(11) 0.031(8) 0.026(8) 0.011(6) -0.019(8) 0.000(8) C13B 0.034(9) 0.016(7) 0.037(8) -0.008(6) -0.017(7) 0.010(6) C13C 0.026(8) 0.037(9) 0.026(8) 0.004(6) -0.005(6) -0.005(7) C14A 0.056(11) 0.020(7) 0.035(9) -0.001(6) -0.023(8) -0.005(7) C14B 0.041(9) 0.038(9) 0.037(9) -0.014(7) -0.018(7) -0.018(7) C14C 0.021(8) 0.030(8) 0.033(9) 0.012(6) -0.005(7) -0.011(6) C15A 0.049(10) 0.033(8) 0.029(8) -0.011(7) -0.015(7) 0.008(7) C15B 0.032(9) 0.035(9) 0.029(8) 0.008(7) -0.011(7) -0.014(7) C15C 0.033(9) 0.025(7) 0.024(8) 0.004(6) -0.009(7) -0.008(6) C16A 0.044(10) 0.040(9) 0.019(8) -0.003(7) -0.004(7) 0.011(8) C16B 0.036(9) 0.016(7) 0.033(8) -0.003(6) -0.016(7) -0.008(6) C16C 0.040(9) 0.017(7) 0.022(7) 0.007(5) -0.017(7) -0.003(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 1.985(17) . ? Au1 P1 2.295(4) . ? Cr1 C8 1.875(16) . ? Cr1 C9 1.888(16) . ? Cr1 C7 1.895(15) . ? Cr1 C6 1.907(15) . ? Cr1 C10 1.917(15) . ? Cr1 C3 2.030(15) . ? P1 C11A 1.805(13) . ? P1 C11C 1.809(13) . ? P1 C11B 1.828(14) . ? O1 C6 1.125(16) . ? O2 C7 1.163(16) . ? O3 C8 1.161(16) . ? O4 C9 1.151(16) . ? O5 C10 1.134(16) . ? N1 C1 1.368(18) . ? N1 C4 1.428(18) . ? N1 C5 1.479(17) . ? C1 C2 1.47(2) . ? C2 C3 1.215(19) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5C 0.9800 . ? C5 H5B 0.9800 . ? C5 H5A 0.9800 . ? C11A C12A 1.382(18) . ? C11A C16A 1.400(19) . ? C11B C16B 1.359(19) . ? C11B C12B 1.398(18) . ? C11C C12C 1.381(18) . ? C11C C16C 1.413(19) . ? C12A C13A 1.367(19) . ? C12A H12A 0.9500 . ? C12B C13B 1.373(19) . ? C12B H12B 0.9500 . ? C12C C13C 1.382(18) . ? C12C H12C 0.9500 . ? C13A C14A 1.39(2) . ? C13A H13A 0.9500 . ? C13B C14B 1.37(2) . ? C13B H13B 0.9500 . ? C13C C14C 1.41(2) . ? C13C H13C 0.9500 . ? C14A C15A 1.39(2) . ? C14A H14A 0.9500 . ? C14B C15B 1.37(2) . ? C14B H14B 0.9500 . ? C14C C15C 1.32(2) . ? C14C H14C 0.9500 . ? C15A C16A 1.38(2) . ? C15A H15A 0.9500 . ? C15B C16B 1.414(19) . ? C15B H15B 0.9500 . ? C15C C16C 1.402(19) . ? C15C H15C 0.9500 . ? C16A H16A 0.9500 . ? C16B H16B 0.9500 . ? C16C H16C 0.9500 . ? 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 179.5(4) . . ? C8 Cr1 C9 91.3(6) . . ? C8 Cr1 C7 90.7(6) . . ? C9 Cr1 C7 93.1(6) . . ? C8 Cr1 C6 95.2(6) . . ? C9 Cr1 C6 173.3(6) . . ? C7 Cr1 C6 88.3(6) . . ? C8 Cr1 C10 92.1(6) . . ? C9 Cr1 C10 90.4(6) . . ? C7 Cr1 C10 175.5(6) . . ? C6 Cr1 C10 87.9(6) . . ? C8 Cr1 C3 172.0(6) . . ? C9 Cr1 C3 81.3(6) . . ? C7 Cr1 C3 86.8(5) . . ? C6 Cr1 C3 92.3(6) . . ? C10 Cr1 C3 90.9(5) . . ? C11A P1 C11C 107.8(6) . . ? C11A P1 C11B 105.4(6) . . ? C11C P1 C11B 103.2(6) . . ? C11A P1 Au1 114.3(4) . . ? C11C P1 Au1 113.4(5) . . ? C11B P1 Au1 111.8(5) . . ? C1 N1 C4 120.5(13) . . ? C1 N1 C5 125.2(13) . . ? C4 N1 C5 114.1(11) . . ? N1 C1 C2 113.8(14) . . ? N1 C1 Au1 127.1(11) . . ? C2 C1 Au1 118.9(10) . . ? C3 C2 C1 172.6(14) . . ? C2 C3 Cr1 170.1(12) . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C5 H5C 109.5 . . ? N1 C5 H5B 109.5 . . ? H5C C5 H5B 109.5 . . ? N1 C5 H5A 109.5 . . ? H5C C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? O1 C6 Cr1 176.5(13) . . ? O2 C7 Cr1 176.7(12) . . ? O3 C8 Cr1 175.9(12) . . ? O4 C9 Cr1 176.9(12) . . ? O5 C10 Cr1 179.3(13) . . ? C12A C11A C16A 118.4(12) . . ? C12A C11A P1 119.4(10) . . ? C16A C11A P1 122.1(10) . . ? C16B C11B C12B 119.8(13) . . ? C16B C11B P1 117.6(10) . . ? C12B C11B P1 122.4(11) . . ? C12C C11C C16C 118.3(12) . . ? C12C C11C P1 123.3(10) . . ? C16C C11C P1 118.4(10) . . ? C13A C12A C11A 120.9(14) . . ? C13A C12A H12A 119.6 . . ? C11A C12A H12A 119.6 . . ? C13B C12B C11B 121.1(13) . . ? C13B C12B H12B 119.4 . . ? C11B C12B H12B 119.4 . . ? C11C C12C C13C 121.5(13) . . ? C11C C12C H12C 119.2 . . ? C13C C12C H12C 119.2 . . ? C12A C13A C14A 121.0(14) . . ? C12A C13A H13A 119.5 . . ? C14A C13A H13A 119.5 . . ? C14B C13B C12B 119.3(13) . . ? C14B C13B H13B 120.3 . . ? C12B C13B H13B 120.3 . . ? C12C C13C C14C 118.4(14) . . ? C12C C13C H13C 120.8 . . ? C14C C13C H13C 120.8 . . ? C13A C14A C15A 119.1(14) . . ? C13A C14A H14A 120.5 . . ? C15A C14A H14A 120.5 . . ? C15B C14B C13B 120.1(13) . . ? C15B C14B H14B 119.9 . . ? C13B C14B H14B 119.9 . . ? C15C C14C C13C 121.6(13) . . ? C15C C14C H14C 119.2 . . ? C13C C14C H14C 119.2 . . ? C16A C15A C14A 119.7(15) . . ? C16A C15A H15A 120.1 . . ? C14A C15A H15A 120.1 . . ? C14B C15B C16B 120.9(14) . . ? C14B C15B H15B 119.5 . . ? C16B C15B H15B 119.5 . . ? C14C C15C C16C 120.4(14) . . ? C14C C15C H15C 119.8 . . ? C16C C15C H15C 119.8 . . ? C15A C16A C11A 120.7(14) . . ? C15A C16A H16A 119.6 . . ? C11A C16A H16A 119.6 . . ? C11B C16B C15B 118.7(13) . . ? C11B C16B H16B 120.7 . . ? C15B C16B H16B 120.7 . . ? C15C C16C C11C 119.7(13) . . ? C15C C16C H16C 120.2 . . ? C11C C16C H16C 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 -5.1(19) . . . . ? C4 N1 C1 Au1 4.7(19) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 26.8 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 7.00 _refine_diff_density_min -2.87 _refine_diff_density_rms 0.29 #====END data_Complex_3b _database_code_depnum_ccdc_archive 'CCDC 650399' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H21 Au N O5 P W' _chemical_formula_sum 'C28 H21 Au N O5 P W' _chemical_formula_weight 863.24 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.2552(5) _cell_length_b 24.2452(14) _cell_length_c 12.4647(7) _cell_angle_alpha 90.00 _cell_angle_beta 103.429(1) _cell_angle_gamma 90.00 _cell_volume 2720.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9248 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.2 _exptl_crystal_description Prism _exptl_crystal_colour 'Red orange' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.108 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 9.708 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_T_max 0.415 _exptl_absorpt_process_details 'SADABS, Blessing, Acta Cryst. A51 (1995) 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 CCD area-detector' _diffrn_measurement_method '\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 16164 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.046 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.9 _diffrn_reflns_theta_max 27.0 _reflns_number_total 5914 _reflns_number_gt 5326 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; X-Seed (Barbour, 2001; Atwood and Barbour, 2003) ; _computing_publication_material ; X-Seed ; _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^)+(0.0433P)^2^+0.8777P] 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 5914 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.036 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.079 _refine_ls_wR_factor_gt 0.076 _refine_ls_goodness_of_fit_ref 1.03 _refine_ls_restrained_S_all 1.03 _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 0.574435(18) 1.019293(7) 0.765032(14) 0.01755(7) Uani 1 1 d . . . P1 P 0.65364(12) 1.08387(5) 0.90028(10) 0.0167(2) Uani 1 1 d . . . W1 W 0.84780(2) 0.831800(7) 0.545905(15) 0.01964(7) Uani 1 1 d . . . O1 O 1.1584(4) 0.87341(14) 0.6883(3) 0.0305(8) Uani 1 1 d . . . O2 O 0.7860(5) 0.75550(17) 0.7398(3) 0.0398(10) Uani 1 1 d . . . C8 C 0.9567(5) 0.76830(19) 0.4957(4) 0.0217(10) Uani 1 1 d . . . C3 C 0.7119(5) 0.89499(19) 0.5954(4) 0.0200(9) Uani 1 1 d . . . C6 C 1.0428(5) 0.85947(19) 0.6408(4) 0.0228(10) Uani 1 1 d . . . C7 C 0.8080(5) 0.7835(2) 0.6715(4) 0.0247(11) Uani 1 1 d . . . O3 O 1.0151(4) 0.73225(14) 0.4650(3) 0.0270(8) Uani 1 1 d . . . C11C C 0.7146(5) 1.14682(19) 0.8446(4) 0.0194(9) Uani 1 1 d . . . C11A C 0.8039(5) 1.06001(18) 1.0094(4) 0.0171(9) Uani 1 1 d . . . C11B C 0.5105(5) 1.10752(18) 0.9676(4) 0.0199(9) Uani 1 1 d . . . C12C C 0.6650(5) 1.19841(19) 0.8675(4) 0.0233(10) Uani 1 1 d . . . H12C H 0.6022 1.2021 0.9174 0.028 Uiso 1 1 calc R . . C13B C 0.4277(6) 1.1371(2) 1.1276(5) 0.0301(11) Uani 1 1 d . . . H13B H 0.4456 1.1415 1.2054 0.036 Uiso 1 1 calc R . . C15C C 0.8514(6) 1.1886(2) 0.7231(4) 0.0266(11) Uani 1 1 d . . . H15C H 0.9160 1.1851 0.6744 0.032 Uiso 1 1 calc R . . C14B C 0.2930(6) 1.1539(2) 1.0608(5) 0.0292(11) Uani 1 1 d . . . H14B H 0.2196 1.1702 1.0926 0.035 Uiso 1 1 calc R . . C16A C 0.9205(5) 1.09390(18) 1.0614(4) 0.0208(10) Uani 1 1 d . . . H16A H 0.9264 1.1306 1.0363 0.025 Uiso 1 1 calc R . . C16C C 0.8094(5) 1.14224(19) 0.7729(4) 0.0231(10) Uani 1 1 d . . . H16C H 0.8453 1.1070 0.7581 0.028 Uiso 1 1 calc R . . C14C C 0.7995(5) 1.2402(2) 0.7441(4) 0.0266(11) Uani 1 1 d . . . H14C H 0.8268 1.2719 0.7088 0.032 Uiso 1 1 calc R . . C12B C 0.5364(5) 1.1139(2) 1.0809(4) 0.0245(10) Uani 1 1 d . . . H12B H 0.6283 1.1025 1.1268 0.029 Uiso 1 1 calc R . . C16B C 0.3737(5) 1.12288(18) 0.9006(4) 0.0215(10) Uani 1 1 d . . . H16B H 0.3542 1.1171 0.8232 0.026 Uiso 1 1 calc R . . C15B C 0.2658(5) 1.1467(2) 0.9470(5) 0.0264(11) Uani 1 1 d . . . H15B H 0.1737 1.1580 0.9011 0.032 Uiso 1 1 calc R . . C13C C 0.7077(5) 1.24518(19) 0.8166(4) 0.0250(11) Uani 1 1 d . . . H13C H 0.6735 1.2806 0.8321 0.030 Uiso 1 1 calc R . . C14A C 1.0217(5) 1.02015(19) 1.1865(4) 0.0226(10) Uani 1 1 d . . . H14A H 1.0949 1.0066 1.2473 0.027 Uiso 1 1 calc R . . O5 O 0.9191(5) 0.90231(18) 0.3502(4) 0.0525(13) Uani 1 1 d . . . C12A C 0.7984(5) 1.00528(19) 1.0455(4) 0.0226(10) Uani 1 1 d . . . H12A H 0.7204 0.9815 1.0098 0.027 Uiso 1 1 calc R . . C15A C 1.0288(5) 1.0741(2) 1.1503(4) 0.0235(10) Uani 1 1 d . . . H15A H 1.1075 1.0975 1.1861 0.028 Uiso 1 1 calc R . . C13A C 0.9068(6) 0.98632(19) 1.1328(5) 0.0268(11) Uani 1 1 d . . . H13A H 0.9027 0.9493 1.1568 0.032 Uiso 1 1 calc R . . C2 C 0.6181(5) 0.92681(18) 0.6156(4) 0.0202(9) Uani 1 1 d . . . C10 C 0.8912(6) 0.8775(2) 0.4225(5) 0.0346(13) Uani 1 1 d . . . O4 O 0.5394(5) 0.7913(2) 0.3945(5) 0.080(2) Uani 1 1 d . . . C9 C 0.6513(6) 0.8057(3) 0.4478(5) 0.0415(15) Uani 1 1 d . . . N1 N 0.3729(4) 0.95839(15) 0.5815(3) 0.0187(8) Uani 1 1 d . . . C1 C 0.5096(5) 0.96223(18) 0.6402(4) 0.0175(9) Uani 1 1 d . . . C5 C 0.3289(5) 0.9185(2) 0.4905(4) 0.0260(11) Uani 1 1 d . . . H5A H 0.4180 0.9040 0.4705 0.039 Uiso 1 1 calc R . . H5B H 0.2660 0.9369 0.4264 0.039 Uiso 1 1 calc R . . H5C H 0.2737 0.8881 0.5140 0.039 Uiso 1 1 calc R . . C4 C 0.2532(5) 0.9944(2) 0.5978(5) 0.0260(11) Uani 1 1 d . . . H4A H 0.2920 1.0201 0.6582 0.039 Uiso 1 1 calc R . . H4B H 0.1741 0.9720 0.6162 0.039 Uiso 1 1 calc R . . H4C H 0.2132 1.0152 0.5300 0.039 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 0.01860(11) 0.01533(10) 0.01835(11) -0.00245(6) 0.00355(8) 0.00055(6) P1 0.0170(5) 0.0155(5) 0.0174(6) -0.0008(4) 0.0034(5) -0.0004(4) W1 0.02082(11) 0.01974(11) 0.01719(12) -0.00189(7) 0.00201(8) 0.00654(7) O1 0.028(2) 0.0268(19) 0.036(2) -0.0052(15) 0.0076(17) -0.0008(15) O2 0.052(3) 0.040(2) 0.032(2) 0.0017(18) 0.017(2) -0.0048(19) C8 0.021(2) 0.022(2) 0.022(3) 0.0006(18) 0.005(2) 0.0008(19) C3 0.019(2) 0.024(2) 0.018(2) -0.0019(18) 0.0053(19) -0.0031(18) C6 0.024(3) 0.021(2) 0.024(3) 0.0009(19) 0.007(2) 0.0015(19) C7 0.028(3) 0.022(2) 0.025(3) -0.010(2) 0.008(2) 0.0048(19) O3 0.0314(19) 0.0236(18) 0.0266(19) -0.0021(14) 0.0080(16) 0.0048(15) C11C 0.016(2) 0.020(2) 0.021(2) -0.0009(18) 0.0001(18) -0.0014(17) C11A 0.016(2) 0.017(2) 0.019(2) 0.0016(17) 0.0040(18) 0.0019(16) C11B 0.020(2) 0.016(2) 0.024(3) -0.0010(17) 0.0078(19) -0.0002(17) C12C 0.021(2) 0.020(2) 0.029(3) -0.0014(19) 0.006(2) -0.0018(18) C13B 0.032(3) 0.033(3) 0.028(3) -0.001(2) 0.012(2) 0.001(2) C15C 0.026(3) 0.031(3) 0.025(3) 0.001(2) 0.011(2) -0.004(2) C14B 0.031(3) 0.021(2) 0.041(3) 0.000(2) 0.019(2) 0.001(2) C16A 0.022(2) 0.017(2) 0.022(2) -0.0006(17) 0.0024(19) -0.0054(18) C16C 0.024(2) 0.019(2) 0.027(3) -0.0018(19) 0.008(2) 0.0001(18) C14C 0.027(3) 0.022(2) 0.027(3) 0.006(2) 0.001(2) -0.007(2) C12B 0.021(2) 0.029(3) 0.023(3) 0.0012(19) 0.006(2) 0.0014(19) C16B 0.022(2) 0.019(2) 0.024(3) -0.0024(18) 0.006(2) -0.0017(18) C15B 0.014(2) 0.023(2) 0.040(3) 0.000(2) 0.003(2) 0.0047(18) C13C 0.027(3) 0.014(2) 0.034(3) 0.0001(19) 0.006(2) -0.0005(18) C14A 0.020(2) 0.030(3) 0.018(2) -0.0007(18) 0.0038(19) 0.0076(18) O5 0.073(3) 0.050(3) 0.046(3) 0.029(2) 0.038(2) 0.040(2) C12A 0.019(2) 0.015(2) 0.032(3) 0.0004(19) 0.001(2) -0.0033(18) C15A 0.018(2) 0.030(3) 0.022(3) -0.0015(19) 0.005(2) -0.0023(19) C13A 0.030(3) 0.018(2) 0.033(3) 0.002(2) 0.010(2) 0.0035(19) C2 0.023(2) 0.018(2) 0.018(2) 0.0009(17) 0.0011(19) 0.0006(18) C10 0.041(3) 0.035(3) 0.030(3) 0.005(2) 0.012(3) 0.024(2) O4 0.038(3) 0.095(4) 0.085(4) -0.050(3) -0.027(3) 0.012(3) C9 0.036(3) 0.040(3) 0.043(4) -0.020(3) -0.002(3) 0.011(3) N1 0.0204(19) 0.0163(18) 0.019(2) 0.0001(15) 0.0034(16) 0.0027(15) C1 0.021(2) 0.014(2) 0.019(2) 0.0007(17) 0.0084(18) 0.0025(17) C5 0.022(2) 0.027(3) 0.027(3) -0.010(2) 0.002(2) -0.0022(19) C4 0.022(2) 0.024(2) 0.032(3) -0.002(2) 0.005(2) 0.0054(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 C1 2.065(4) . ? Au1 P1 2.2926(11) . ? P1 C11A 1.800(5) . ? P1 C11B 1.818(5) . ? P1 C11C 1.820(5) . ? W1 C10 2.010(6) . ? W1 C8 2.018(5) . ? W1 C6 2.028(5) . ? W1 C9 2.042(6) . ? W1 C7 2.055(5) . ? W1 C3 2.161(5) . ? O1 C6 1.147(6) . ? O2 C7 1.144(6) . ? C8 O3 1.139(6) . ? C3 C2 1.230(7) . ? C11C C12C 1.385(7) . ? C11C C16C 1.395(7) . ? C11A C16A 1.391(6) . ? C11A C12A 1.406(6) . ? C11B C12B 1.385(7) . ? C11B C16B 1.396(7) . ? C12C C13C 1.400(7) . ? C12C H12C 0.9500 . ? C13B C14B 1.390(8) . ? C13B C12B 1.393(7) . ? C13B H13B 0.9500 . ? C15C C16C 1.383(7) . ? C15C C14C 1.386(7) . ? C15C H15C 0.9500 . ? C14B C15B 1.393(8) . ? C14B H14B 0.9500 . ? C16A C15A 1.396(7) . ? C16A H16A 0.9500 . ? C16C H16C 0.9500 . ? C14C C13C 1.382(7) . ? C14C H14C 0.9500 . ? C12B H12B 0.9500 . ? C16B C15B 1.389(7) . ? C16B H16B 0.9500 . ? C15B H15B 0.9500 . ? C13C H13C 0.9500 . ? C14A C13A 1.386(7) . ? C14A C15A 1.390(7) . ? C14A H14A 0.9500 . ? O5 C10 1.162(7) . ? C12A C13A 1.377(7) . ? C12A H12A 0.9500 . ? C15A H15A 0.9500 . ? C13A H13A 0.9500 . ? C2 C1 1.408(6) . ? O4 C9 1.148(7) . ? N1 C1 1.309(6) . ? N1 C4 1.461(6) . ? N1 C5 1.474(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 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 177.70(13) . . ? C11A P1 C11B 105.7(2) . . ? C11A P1 C11C 107.7(2) . . ? C11B P1 C11C 103.6(2) . . ? C11A P1 Au1 113.27(15) . . ? C11B P1 Au1 114.33(15) . . ? C11C P1 Au1 111.54(16) . . ? C10 W1 C8 88.8(2) . . ? C10 W1 C6 87.4(2) . . ? C8 W1 C6 89.56(19) . . ? C10 W1 C9 91.2(3) . . ? C8 W1 C9 91.0(2) . . ? C6 W1 C9 178.5(2) . . ? C10 W1 C7 178.35(19) . . ? C8 W1 C7 89.58(19) . . ? C6 W1 C7 92.10(19) . . ? C9 W1 C7 89.3(2) . . ? C10 W1 C3 93.51(19) . . ? C8 W1 C3 174.44(18) . . ? C6 W1 C3 95.57(18) . . ? C9 W1 C3 83.9(2) . . ? C7 W1 C3 88.10(18) . . ? O3 C8 W1 178.2(4) . . ? C2 C3 W1 171.1(4) . . ? O1 C6 W1 174.6(4) . . ? O2 C7 W1 178.2(4) . . ? C12C C11C C16C 119.4(4) . . ? C12C C11C P1 122.2(4) . . ? C16C C11C P1 118.3(3) . . ? C16A C11A C12A 119.3(4) . . ? C16A C11A P1 122.8(3) . . ? C12A C11A P1 117.8(3) . . ? C12B C11B C16B 119.9(4) . . ? C12B C11B P1 122.3(4) . . ? C16B C11B P1 117.7(4) . . ? C11C C12C C13C 119.8(5) . . ? C11C C12C H12C 120.1 . . ? C13C C12C H12C 120.1 . . ? C14B C13B C12B 120.1(5) . . ? C14B C13B H13B 120.0 . . ? C12B C13B H13B 120.0 . . ? C16C C15C C14C 120.2(5) . . ? C16C C15C H15C 119.9 . . ? C14C C15C H15C 119.9 . . ? C13B C14B C15B 119.9(5) . . ? C13B C14B H14B 120.0 . . ? C15B C14B H14B 120.0 . . ? C11A C16A C15A 120.2(4) . . ? C11A C16A H16A 119.9 . . ? C15A C16A H16A 119.9 . . ? C15C C16C C11C 120.5(5) . . ? C15C C16C H16C 119.8 . . ? C11C C16C H16C 119.8 . . ? C13C C14C C15C 119.7(4) . . ? C13C C14C H14C 120.2 . . ? C15C C14C H14C 120.2 . . ? C11B C12B C13B 120.1(5) . . ? C11B C12B H12B 120.0 . . ? C13B C12B H12B 120.0 . . ? C15B C16B C11B 120.1(5) . . ? C15B C16B H16B 119.9 . . ? C11B C16B H16B 119.9 . . ? C16B C15B C14B 119.9(5) . . ? C16B C15B H15B 120.1 . . ? C14B C15B H15B 120.1 . . ? C14C C13C C12C 120.4(5) . . ? C14C C13C H13C 119.8 . . ? C12C C13C H13C 119.8 . . ? C13A C14A C15A 119.3(4) . . ? C13A C14A H14A 120.4 . . ? C15A C14A H14A 120.4 . . ? C13A C12A C11A 119.7(4) . . ? C13A C12A H12A 120.2 . . ? C11A C12A H12A 120.2 . . ? C14A C15A C16A 120.2(4) . . ? C14A C15A H15A 119.9 . . ? C16A C15A H15A 119.9 . . ? C12A C13A C14A 121.4(4) . . ? C12A C13A H13A 119.3 . . ? C14A C13A H13A 119.3 . . ? C3 C2 C1 178.6(5) . . ? O5 C10 W1 177.6(5) . . ? O4 C9 W1 178.5(6) . . ? C1 N1 C4 123.0(4) . . ? C1 N1 C5 122.3(4) . . ? C4 N1 C5 114.6(4) . . ? N1 C1 C2 118.7(4) . . ? N1 C1 Au1 122.9(3) . . ? C2 C1 Au1 118.4(3) . . ? N1 C5 H5A 109.5 . . ? N1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 -0.3(7) . . . . ? C4 N1 C1 Au1 0.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.0 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.08 _refine_diff_density_min -2.07 _refine_diff_density_rms 0.20 #====END