Supplementary Material (ESI) 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 'S. Berners-Price' _publ_contact_author_address ; Department of Chemistry The University of Western Australia 35 Stirling Highway Crawley Perth WA 6009 AUSTRALIA ; _publ_contact_author_email SBP@CHEM.UWA.EDU.AU _publ_section_title ; Gold(I) chloride adducts of 1,3-bis(di-2-pyridylphosphino)propane: synthesis, structural studies and antitumour activity ; loop_ _publ_author_name 'S. Berners-Price' 'Aleksandra Filipovska' 'Anthony S. Humphreys' 'George A. Koutantonis' ; B.A.Skelton ; 'A. H. White' #===END # Attachment 'Compound2new.cif' data_gk127 _database_code_depnum_ccdc_archive 'CCDC 640094' _audit_creation_date 2007-03-13T07:39:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C46 H51.50 Au Cl N8 O3.75 P4' _chemical_formula_moiety 'C46 H44 Au Cl N8 P4, 3.75(H2 O)' _chemical_formula_weight 1132.75 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P_21_21_21 _symmetry_space_group_name_Hall p_2ac_2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.276(2) _cell_length_b 18.3940(10) _cell_length_c 34.794(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9776.7(16) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7945 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 32.1 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4556 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.245 _exptl_crystal_description block _exptl_crystal_size_max .14 _exptl_crystal_size_mid .14 _exptl_crystal_size_min .08 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .62 _exptl_absorpt_correction_T_max .86 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents .081 _diffrn_reflns_av_unetI/netI 0.0808 _diffrn_reflns_number 155499 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.11 _diffrn_reflns_theta_max 32.66 _diffrn_reflns_theta_full 32.5 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 35424 _reflns_number_gt 23553 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0653P)^2^+17.5936P] 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_number_reflns 35424 _refine_ls_number_parameters 1107 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.134 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(13) _refine_diff_density_max 2.836 _refine_diff_density_min -5.238 _refine_diff_density_rms 0.189 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 0.351280(16) 0.304359(15) 0.387677(6) 0.01964(6) Uani 1 1 d . . . Au2 Au 0.355175(17) 0.694057(15) 0.607228(6) 0.02088(6) Uani 1 1 d . . . Cl1 Cl 0.84234(16) 0.49770(11) 0.48951(7) 0.0406(5) Uani 1 1 d . . . Cl2 Cl 0.7399(3) 0.5914(2) 0.71638(10) 0.0813(10) Uani 1 1 d . . . P1 P 0.20489(12) 0.27069(10) 0.36988(5) 0.0198(3) Uani 1 1 d . . . C111 C 0.1133(5) 0.3093(4) 0.3992(2) 0.0284(15) Uani 1 1 d . . . N112 N 0.0328(4) 0.3010(4) 0.3841(2) 0.0440(18) Uani 1 1 d . . . C113 C -0.0332(6) 0.3310(5) 0.4038(2) 0.0366(19) Uiso 1 1 d . . . H113 H -0.0913 0.3249 0.3946 0.044 Uiso 1 1 calc R . . C114 C -0.0199(6) 0.3707(5) 0.4373(3) 0.042(2) Uani 1 1 d . . . H114 H -0.068 0.3923 0.4503 0.051 Uiso 1 1 calc R . . C115 C 0.0620(7) 0.3782(6) 0.4510(3) 0.047(2) Uani 1 1 d . . . H115 H 0.0724 0.4046 0.474 0.056 Uiso 1 1 calc R . . C116 C 0.1315(6) 0.3467(5) 0.4310(2) 0.038(2) Uani 1 1 d . . . H116 H 0.19 0.3519 0.4397 0.046 Uiso 1 1 calc R . . C121 C 0.1814(5) 0.1725(4) 0.3693(2) 0.0228(14) Uani 1 1 d . . . N122 N 0.2022(5) 0.1396(3) 0.40211(18) 0.0295(14) Uani 1 1 d . . . C123 C 0.1925(6) 0.0680(4) 0.4030(3) 0.0365(19) Uani 1 1 d . . . H123 H 0.2051 0.044 0.4265 0.044 Uiso 1 1 calc R . . C124 C 0.1653(5) 0.0250(4) 0.3721(2) 0.0306(17) Uani 1 1 d . . . H124 H 0.1595 -0.0263 0.3745 0.037 Uiso 1 1 calc R . . C125 C 0.1472(8) 0.0602(5) 0.3383(2) 0.047(2) Uani 1 1 d . . . H125 H 0.1318 0.0335 0.3159 0.056 Uiso 1 1 calc R . . C126 C 0.1519(7) 0.1358(4) 0.3373(2) 0.042(2) Uani 1 1 d . . . H126 H 0.135 0.1617 0.3149 0.05 Uiso 1 1 calc R . . C10 C 0.1777(5) 0.3033(4) 0.32158(18) 0.0254(13) Uani 1 1 d . . . H10A H 0.215 0.2776 0.3027 0.03 Uiso 1 1 calc R . . H10B H 0.116 0.2906 0.3159 0.03 Uiso 1 1 calc R . . C12 C 0.1898(5) 0.3858(4) 0.3163(2) 0.0251(15) Uani 1 1 d . . . H12A H 0.1681 0.4108 0.3397 0.03 Uiso 1 1 calc R . . H12B H 0.1533 0.402 0.2944 0.03 Uiso 1 1 calc R . . C20 C 0.2851(5) 0.4094(4) 0.3091(2) 0.0248(15) Uani 1 1 d . . . H20A H 0.2844 0.4583 0.2972 0.03 Uiso 1 1 calc R . . H20B H 0.3113 0.3756 0.2902 0.03 Uiso 1 1 calc R . . P2 P 0.35648(13) 0.41255(9) 0.35155(4) 0.0189(3) Uani 1 1 d . . . C211 C 0.3220(5) 0.4962(4) 0.3753(2) 0.0240(14) Uiso 1 1 d . . . N212 N 0.3216(5) 0.5568(4) 0.3527(2) 0.044(2) Uani 1 1 d . . . C213 C 0.2923(8) 0.6179(5) 0.3693(4) 0.058(3) Uani 1 1 d . . . H213 H 0.2925 0.6611 0.3543 0.07 Uiso 1 1 calc R . . C214 C 0.2621(6) 0.6225(5) 0.4065(3) 0.043(2) Uani 1 1 d . . . H214 H 0.2417 0.6673 0.4167 0.051 Uiso 1 1 calc R . . C215 C 0.2622(7) 0.5597(5) 0.4287(3) 0.044(2) Uani 1 1 d . . . H215 H 0.2413 0.5608 0.4544 0.052 Uiso 1 1 calc R . . C216 C 0.2928(6) 0.4960(4) 0.4131(2) 0.037(2) Uani 1 1 d . . . H216 H 0.2939 0.4526 0.4278 0.044 Uiso 1 1 calc R . . C221 C 0.4641(5) 0.4351(4) 0.32987(19) 0.0198(13) Uani 1 1 d . . . N222 N 0.4843(4) 0.3966(4) 0.29869(18) 0.0337(16) Uani 1 1 d . . . C223 C 0.5652(5) 0.4043(4) 0.2836(2) 0.0296(16) Uani 1 1 d . . . H223 H 0.5791 0.3779 0.261 0.036 Uiso 1 1 calc R . . C224 C 0.6292(5) 0.4489(4) 0.2994(2) 0.0308(17) Uani 1 1 d . . . H224 H 0.6856 0.4523 0.2881 0.037 Uiso 1 1 calc R . . C225 C 0.6082(5) 0.4885(4) 0.3324(2) 0.0315(17) Uani 1 1 d . . . H225 H 0.6497 0.5202 0.344 0.038 Uiso 1 1 calc R . . C226 C 0.5230(5) 0.4801(4) 0.3482(2) 0.0249(14) Uani 1 1 d . . . H226 H 0.5069 0.5051 0.371 0.03 Uiso 1 1 calc R . . P3 P 0.44382(12) 0.20701(9) 0.36627(5) 0.0215(3) Uani 1 1 d . . . C311 C 0.5633(5) 0.2215(4) 0.3621(2) 0.0210(13) Uani 1 1 d . . . N312 N 0.6113(5) 0.1616(4) 0.3567(2) 0.0392(18) Uani 1 1 d . . . C313 C 0.6966(6) 0.1692(6) 0.3531(3) 0.050(3) Uani 1 1 d . . . H313 H 0.7309 0.1266 0.3496 0.06 Uiso 1 1 calc R . . C314 C 0.7401(6) 0.2368(7) 0.3541(3) 0.056(3) Uani 1 1 d . . . H314 H 0.8018 0.2401 0.351 0.068 Uiso 1 1 calc R . . C315 C 0.6888(6) 0.2988(5) 0.3600(3) 0.041(2) Uani 1 1 d . . . H315 H 0.7138 0.346 0.3611 0.049 Uiso 1 1 calc R . . C316 C 0.6000(5) 0.2878(4) 0.3639(2) 0.0332(18) Uani 1 1 d . . . H316 H 0.5633 0.3287 0.3681 0.04 Uiso 1 1 calc R . . C321 C 0.4150(5) 0.1710(4) 0.3186(2) 0.0262(15) Uani 1 1 d . . . N322 N 0.3882(4) 0.1028(4) 0.31521(19) 0.0310(14) Uani 1 1 d . . . C323 C 0.3630(7) 0.0795(5) 0.2797(3) 0.050(3) Uani 1 1 d . . . H323 H 0.3441 0.0306 0.2768 0.06 Uiso 1 1 calc R . . C324 C 0.3638(7) 0.1239(5) 0.2479(2) 0.045(2) Uani 1 1 d . . . H324 H 0.3467 0.1054 0.2235 0.054 Uiso 1 1 calc R . . C325 C 0.3892(6) 0.1943(6) 0.2515(2) 0.043(2) Uani 1 1 d . . . H325 H 0.3892 0.2259 0.2299 0.051 Uiso 1 1 calc R . . C326 C 0.4158(6) 0.2197(4) 0.2882(2) 0.0349(19) Uani 1 1 d . . . H326 H 0.4336 0.2687 0.2918 0.042 Uiso 1 1 calc R . . C30 C 0.4367(6) 0.1295(4) 0.3991(2) 0.0294(16) Uani 1 1 d . . . H30A H 0.3755 0.1117 0.3998 0.035 Uiso 1 1 calc R . . H30B H 0.474 0.0896 0.3893 0.035 Uiso 1 1 calc R . . C34 C 0.4660(5) 0.1491(4) 0.4406(2) 0.0282(16) Uani 1 1 d . . . H34A H 0.4802 0.1035 0.4544 0.034 Uiso 1 1 calc R . . H34B H 0.5204 0.1782 0.4391 0.034 Uiso 1 1 calc R . . C40 C 0.3998(5) 0.1910(4) 0.46422(18) 0.0231(13) Uani 1 1 d . . . H40A H 0.4159 0.1863 0.4917 0.028 Uiso 1 1 calc R . . H40B H 0.3419 0.1676 0.4609 0.028 Uiso 1 1 calc R . . P4 P 0.38820(12) 0.28714(10) 0.45331(5) 0.0202(4) Uani 1 1 d . . . C411 C 0.4926(5) 0.3270(4) 0.46812(19) 0.0214(13) Uani 1 1 d . . . N412 N 0.5267(4) 0.3027(4) 0.50170(17) 0.0335(14) Uani 1 1 d . . . C413 C 0.6033(6) 0.3328(5) 0.5134(3) 0.039(2) Uani 1 1 d . . . H413 H 0.6286 0.3171 0.5369 0.047 Uiso 1 1 calc R . . C414 C 0.6461(6) 0.3860(5) 0.4919(3) 0.044(2) Uani 1 1 d . . . H414 H 0.6994 0.4066 0.5009 0.053 Uiso 1 1 calc R . . C415 C 0.6098(7) 0.4085(5) 0.4574(3) 0.044(2) Uani 1 1 d . . . H415 H 0.6383 0.4446 0.4424 0.053 Uiso 1 1 calc R . . C416 C 0.5326(6) 0.3785(5) 0.4451(2) 0.0328(18) Uani 1 1 d . . . H416 H 0.5071 0.3928 0.4214 0.039 Uiso 1 1 calc R . . C421 C 0.3180(5) 0.3230(4) 0.49260(19) 0.0210(14) Uani 1 1 d . . . N422 N 0.3122(4) 0.3946(4) 0.49251(19) 0.0292(14) Uani 1 1 d . . . C423 C 0.2606(6) 0.4250(5) 0.5188(2) 0.0359(19) Uani 1 1 d . . . H423 H 0.2558 0.4765 0.5189 0.043 Uiso 1 1 calc R . . C424 C 0.2140(7) 0.3865(6) 0.5456(2) 0.045(2) Uani 1 1 d . . . H424 H 0.1777 0.4107 0.5637 0.054 Uiso 1 1 calc R . . C425 C 0.2212(6) 0.3114(6) 0.5456(2) 0.045(2) Uani 1 1 d . . . H425 H 0.1907 0.283 0.5641 0.053 Uiso 1 1 calc R . . C426 C 0.2728(5) 0.2791(5) 0.5186(2) 0.0325(17) Uani 1 1 d . . . H426 H 0.2779 0.2276 0.5175 0.039 Uiso 1 1 calc R . . P5 P 0.34604(13) 0.58841(10) 0.64654(5) 0.0225(4) Uani 1 1 d . . . C511 C 0.3862(5) 0.5028(4) 0.6263(3) 0.0318(17) Uani 1 1 d . . . N512 N 0.3986(5) 0.4463(4) 0.6512(2) 0.0392(17) Uani 1 1 d . . . C513 C 0.4304(6) 0.3854(5) 0.6346(3) 0.049(3) Uani 1 1 d . . . H513 H 0.4373 0.3438 0.6505 0.059 Uiso 1 1 calc R . . C514 C 0.4535(6) 0.3784(5) 0.5969(3) 0.045(2) Uani 1 1 d . . . H514 H 0.48 0.3348 0.588 0.054 Uiso 1 1 calc R . . C515 C 0.4388(7) 0.4332(5) 0.5725(3) 0.046(2) Uani 1 1 d . . . H515 H 0.4508 0.4284 0.5458 0.056 Uiso 1 1 calc R . . C516 C 0.4051(6) 0.4973(5) 0.5875(3) 0.041(2) Uani 1 1 d . . . H516 H 0.3951 0.5377 0.5711 0.049 Uiso 1 1 calc R . . C521 C 0.2388(5) 0.5663(4) 0.6660(2) 0.0281(16) Uiso 1 1 d . . . N522 N 0.1863(7) 0.5274(6) 0.6413(3) 0.068(3) Uiso 1 1 d . . . C523 C 0.0975(9) 0.5149(7) 0.6617(4) 0.074(4) Uiso 1 1 d . . . H523 H 0.0573 0.4829 0.6496 0.089 Uiso 1 1 calc R . . C524 C 0.0736(10) 0.5430(8) 0.6928(4) 0.080(4) Uiso 1 1 d . . . H524 H 0.0179 0.5328 0.7036 0.096 Uiso 1 1 calc R . . C525 C 0.1329(10) 0.5904(9) 0.7110(4) 0.087(4) Uiso 1 1 d . . . H525 H 0.1148 0.6143 0.7339 0.105 Uiso 1 1 calc R . . C526 C 0.2120(8) 0.6030(6) 0.6979(3) 0.056(3) Uiso 1 1 d . . . H526 H 0.2496 0.6369 0.7102 0.068 Uiso 1 1 calc R . . C50 C 0.4126(5) 0.5968(5) 0.6892(2) 0.0303(17) Uani 1 1 d . . . H50A H 0.3882 0.6359 0.7055 0.036 Uiso 1 1 calc R . . H50B H 0.4088 0.5508 0.7039 0.036 Uiso 1 1 calc R . . C56 C 0.5111(5) 0.6138(4) 0.6812(3) 0.0331(18) Uani 1 1 d . . . H56A H 0.5465 0.5964 0.7032 0.04 Uiso 1 1 calc R . . H56B H 0.53 0.5866 0.6581 0.04 Uiso 1 1 calc R . . C60 C 0.5294(5) 0.6953(4) 0.67496(19) 0.0269(14) Uani 1 1 d . . . H60A H 0.5924 0.7047 0.6796 0.032 Uiso 1 1 calc R . . H60B H 0.4957 0.7237 0.6941 0.032 Uiso 1 1 calc R . . P6 P 0.50094(12) 0.72726(10) 0.62681(5) 0.0218(4) Uani 1 1 d . . . C611 C 0.5899(4) 0.6876(4) 0.5984(2) 0.0229(13) Uani 1 1 d . . . N612 N 0.6744(4) 0.7011(4) 0.60960(18) 0.0307(13) Uani 1 1 d . . . C613 C 0.7359(6) 0.6678(5) 0.5897(3) 0.040(2) Uiso 1 1 d . . . H613 H 0.7948 0.6759 0.5974 0.048 Uiso 1 1 calc R . . C614 C 0.7224(6) 0.6224(4) 0.5587(2) 0.035(2) Uani 1 1 d . . . H614 H 0.77 0.6005 0.5455 0.042 Uiso 1 1 calc R . . C615 C 0.6392(8) 0.6105(4) 0.5480(2) 0.045(3) Uani 1 1 d . . . H615 H 0.6269 0.5791 0.527 0.054 Uiso 1 1 calc R . . C616 C 0.5706(6) 0.6445(5) 0.5678(2) 0.0330(18) Uani 1 1 d . . . H616 H 0.5117 0.6376 0.5599 0.04 Uiso 1 1 calc R . . C621 C 0.5233(5) 0.8259(4) 0.6282(2) 0.0219(14) Uani 1 1 d . . . N622 N 0.4919(5) 0.8612(4) 0.59846(19) 0.0309(15) Uani 1 1 d . . . C623 C 0.5011(5) 0.9330(4) 0.5975(2) 0.0310(17) Uani 1 1 d . . . H623 H 0.4793 0.959 0.5759 0.037 Uiso 1 1 calc R . . C624 C 0.5425(5) 0.9724(4) 0.6277(2) 0.0318(17) Uani 1 1 d . . . H624 H 0.5481 1.0238 0.6265 0.038 Uiso 1 1 calc R . . C625 C 0.5734(6) 0.9348(5) 0.6579(3) 0.042(2) Uani 1 1 d . . . H625 H 0.6013 0.9598 0.6784 0.051 Uiso 1 1 calc R . . C626 C 0.5648(7) 0.8591(5) 0.6593(3) 0.039(2) Uani 1 1 d . . . H626 H 0.5861 0.8316 0.6804 0.047 Uiso 1 1 calc R . . P7 P 0.32223(11) 0.70222(11) 0.53994(5) 0.0209(3) Uani 1 1 d . . . C711 C 0.2180(5) 0.6610(4) 0.5255(2) 0.0231(14) Uani 1 1 d . . . N712 N 0.1781(4) 0.6903(4) 0.49472(17) 0.0334(14) Uani 1 1 d . . . C713 C 0.1001(7) 0.6619(5) 0.4842(3) 0.043(2) Uani 1 1 d . . . H713 H 0.0716 0.6819 0.4623 0.051 Uiso 1 1 calc R . . C714 C 0.0600(6) 0.6062(5) 0.5030(3) 0.0371(19) Uani 1 1 d . . . H714 H 0.0047 0.5884 0.4947 0.044 Uiso 1 1 calc R . . C715 C 0.1016(6) 0.5767(5) 0.5342(3) 0.038(2) Uani 1 1 d . . . H715 H 0.0754 0.5375 0.5478 0.046 Uiso 1 1 calc R . . C716 C 0.1826(5) 0.6041(4) 0.5460(2) 0.0240(14) Uani 1 1 d . . . H716 H 0.2123 0.5841 0.5675 0.029 Uiso 1 1 calc R . . C721 C 0.3945(5) 0.6660(4) 0.5027(2) 0.0259(15) Uani 1 1 d . . . N722 N 0.4029(5) 0.5924(4) 0.5044(2) 0.0341(15) Uani 1 1 d . . . C723 C 0.4530(6) 0.5609(5) 0.4777(2) 0.040(2) Uani 1 1 d . . . H723 H 0.456 0.5094 0.4777 0.047 Uiso 1 1 calc R . . C724 C 0.5001(6) 0.5969(6) 0.4506(2) 0.043(2) Uani 1 1 d . . . H724 H 0.5366 0.5711 0.4332 0.051 Uiso 1 1 calc R . . C725 C 0.4936(5) 0.6711(5) 0.4489(2) 0.038(2) Uani 1 1 d . . . H725 H 0.5254 0.6981 0.4303 0.046 Uiso 1 1 calc R . . C726 C 0.4382(5) 0.7067(6) 0.4757(2) 0.037(2) Uani 1 1 d . . . H726 H 0.4314 0.758 0.475 0.045 Uiso 1 1 calc R . . C70 C 0.3078(5) 0.7974(4) 0.52496(19) 0.0276(15) Uani 1 1 d . . . H70A H 0.3631 0.8241 0.5294 0.033 Uiso 1 1 calc R . . H70B H 0.2952 0.7988 0.4971 0.033 Uiso 1 1 calc R . . C78 C 0.2350(5) 0.8352(4) 0.5462(2) 0.0294(16) Uani 1 1 d . . . H78A H 0.1856 0.8006 0.5485 0.035 Uiso 1 1 calc R . . H78B H 0.2146 0.8762 0.5301 0.035 Uiso 1 1 calc R . . C80 C 0.2551(5) 0.8648(4) 0.5864(2) 0.0284(16) Uiso 1 1 d . . . H80A H 0.2087 0.8998 0.5937 0.034 Uiso 1 1 calc R . . H80B H 0.3112 0.8918 0.5854 0.034 Uiso 1 1 calc R . . P8 P 0.26271(12) 0.79484(10) 0.62342(5) 0.0228(4) Uani 1 1 d . . . C811 C 0.1474(5) 0.7770(4) 0.63452(19) 0.0243(13) Uani 1 1 d . . . N812 N 0.1012(4) 0.8349(3) 0.64799(19) 0.0275(14) Uani 1 1 d . . . C813 C 0.0172(5) 0.8208(4) 0.6560(2) 0.0314(17) Uani 1 1 d . . . H813 H -0.016 0.8597 0.6665 0.038 Uiso 1 1 calc R . . C814 C -0.0258(5) 0.7568(5) 0.6508(2) 0.0353(19) Uani 1 1 d . . . H814 H -0.0862 0.7521 0.6567 0.042 Uiso 1 1 calc R . . C815 C 0.0228(5) 0.6977(5) 0.6363(3) 0.041(2) Uani 1 1 d . . . H815 H -0.004 0.6518 0.6319 0.049 Uiso 1 1 calc R . . C816 C 0.1102(5) 0.7085(4) 0.6286(2) 0.0334(18) Uani 1 1 d . . . H816 H 0.1451 0.6696 0.6193 0.04 Uiso 1 1 calc R . . C821 C 0.3007(5) 0.8459(5) 0.6653(2) 0.0309(17) Uani 1 1 d . . . N822 N 0.3115(5) 0.9188(4) 0.6610(2) 0.045(2) Uani 1 1 d . . . C823 C 0.3476(8) 0.9536(7) 0.6924(4) 0.067(4) Uani 1 1 d . . . H823 H 0.3571 1.0045 0.6906 0.08 Uiso 1 1 calc R . . C824 C 0.3705(8) 0.9199(9) 0.7260(3) 0.077(4) Uani 1 1 d . . . H824 H 0.3928 0.9465 0.7472 0.092 Uiso 1 1 calc R . . C825 C 0.3601(9) 0.8468(10) 0.7276(3) 0.079(4) Uani 1 1 d . . . H825 H 0.3779 0.8219 0.7502 0.095 Uiso 1 1 calc R . . C826 C 0.3246(6) 0.8068(7) 0.6977(2) 0.050(2) Uani 1 1 d . . . H826 H 0.317 0.7556 0.6992 0.06 Uiso 1 1 calc R . . O01 O -0.1327(5) 0.5389(4) 0.6454(2) 0.057(2) Uani 1 1 d . . . O02 O 0.7910(4) 0.4549(3) 0.3990(2) 0.0451(16) Uani 1 1 d . . . O03 O -0.0760(5) 0.5503(5) 0.5713(2) 0.074(2) Uani 1 1 d . . . O04 O 0.4073(9) 0.4072(8) 0.7342(3) 0.137(5) Uani 1 1 d . . . O05 O 0.2572(8) 0.7576(7) 0.3157(4) 0.149(6) Uani 1 1 d . . . O06 O 0.2335(11) 0.6366(12) 0.2701(4) 0.087(6) Uani 0.5 1 d P . . O07 O 0.4787(9) 0.2685(10) 0.7219(5) 0.069(5) Uani 0.5 1 d P . . O08 O 0.4296(15) 0.1556(12) 0.7109(6) 0.103(7) Uiso 0.5 1 d P . . O09 O 0.3558(15) 0.6910(14) 0.2495(6) 0.108(7) Uiso 0.5 1 d P . . O09' O 0.3685(14) 0.6211(13) 0.2506(6) 0.094(6) Uiso 0.5 1 d P . . 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 0.01852(12) 0.01749(12) 0.02289(10) -0.00177(10) -0.00010(9) 0.00172(11) Au2 0.01819(12) 0.01814(12) 0.02631(11) -0.00229(10) -0.00143(10) 0.00035(11) Cl1 0.0395(12) 0.0276(9) 0.0549(12) -0.0046(9) 0.0086(10) 0.0009(9) Cl2 0.085(2) 0.077(2) 0.082(2) -0.0182(18) -0.0228(18) 0.0316(19) P1 0.0182(9) 0.0173(8) 0.0240(8) -0.0009(7) -0.0001(6) -0.0005(7) C111 0.025(3) 0.024(4) 0.036(4) 0.007(3) 0.008(3) 0.005(3) N112 0.024(3) 0.039(4) 0.069(5) -0.021(4) 0.001(3) 0.004(3) C114 0.043(5) 0.042(5) 0.043(5) 0.023(4) 0.026(4) 0.021(4) C115 0.047(6) 0.057(6) 0.036(5) -0.008(4) 0.012(4) 0.016(5) C116 0.029(5) 0.058(6) 0.029(4) -0.011(4) -0.003(3) 0.013(4) C121 0.017(3) 0.020(3) 0.031(3) -0.005(3) 0.002(3) -0.002(3) N122 0.040(4) 0.021(3) 0.027(3) 0.002(2) 0.002(3) -0.006(3) C123 0.046(5) 0.021(4) 0.043(5) 0.010(3) 0.004(4) -0.003(3) C124 0.029(4) 0.018(3) 0.045(4) -0.004(3) 0.005(3) -0.004(3) C125 0.073(7) 0.031(4) 0.036(4) -0.004(3) -0.005(5) -0.016(5) C126 0.067(7) 0.027(4) 0.031(4) -0.001(3) -0.005(4) -0.010(5) C10 0.027(3) 0.022(3) 0.027(3) 0.001(3) -0.007(2) -0.008(3) C12 0.024(4) 0.022(4) 0.029(4) 0.005(3) -0.003(3) -0.004(3) C20 0.022(4) 0.027(4) 0.025(3) 0.008(3) -0.002(3) -0.001(3) P2 0.0208(9) 0.0148(8) 0.0210(7) -0.0013(6) -0.0002(7) 0.0002(7) N212 0.047(5) 0.020(3) 0.064(5) 0.011(3) 0.024(4) 0.004(3) C213 0.066(7) 0.018(4) 0.091(8) 0.010(5) 0.032(6) 0.005(4) C214 0.034(5) 0.024(4) 0.070(6) -0.021(4) -0.005(4) 0.007(4) C215 0.058(6) 0.031(5) 0.042(5) -0.014(4) -0.011(4) 0.022(4) C216 0.058(6) 0.023(4) 0.030(4) -0.005(3) -0.007(4) 0.010(4) C221 0.023(3) 0.017(3) 0.020(3) -0.002(2) 0.000(2) -0.002(2) N222 0.023(3) 0.050(4) 0.028(3) -0.009(3) 0.002(3) -0.014(3) C223 0.030(4) 0.033(4) 0.026(3) -0.008(3) 0.005(3) 0.001(3) C224 0.021(4) 0.022(4) 0.050(5) 0.014(3) 0.007(3) -0.002(3) C225 0.018(4) 0.028(4) 0.049(5) 0.003(3) -0.006(3) -0.012(3) C226 0.025(4) 0.018(3) 0.031(4) -0.003(3) 0.000(3) -0.004(3) P3 0.0206(8) 0.0153(9) 0.0285(8) -0.0048(6) 0.0019(7) 0.0028(6) C311 0.016(3) 0.019(3) 0.028(3) -0.003(3) -0.001(3) -0.004(3) N312 0.028(4) 0.037(4) 0.052(5) -0.010(3) 0.003(3) 0.007(3) C313 0.032(5) 0.050(6) 0.067(7) -0.007(5) -0.001(5) 0.016(4) C314 0.020(5) 0.076(8) 0.073(7) 0.018(6) 0.001(4) -0.007(5) C315 0.040(5) 0.025(4) 0.059(5) 0.018(4) -0.009(4) -0.012(4) C316 0.025(4) 0.024(4) 0.050(5) 0.000(3) -0.003(3) -0.001(3) C321 0.025(4) 0.029(4) 0.024(3) -0.006(3) -0.001(3) 0.008(3) N322 0.032(4) 0.028(3) 0.032(3) -0.008(3) 0.001(3) -0.004(3) C323 0.060(7) 0.030(4) 0.059(6) -0.027(4) -0.006(5) -0.004(5) C324 0.052(6) 0.049(6) 0.033(4) -0.015(4) -0.011(4) 0.009(5) C325 0.053(5) 0.046(5) 0.030(4) 0.006(4) -0.002(3) 0.000(5) C326 0.048(5) 0.017(3) 0.039(4) -0.002(3) -0.004(4) 0.007(3) C30 0.037(4) 0.016(3) 0.035(4) -0.003(3) 0.006(3) 0.006(3) C34 0.027(4) 0.025(4) 0.032(4) 0.001(3) 0.003(3) 0.006(3) C40 0.028(3) 0.018(3) 0.024(3) 0.005(3) 0.000(2) 0.004(3) P4 0.0202(8) 0.0188(9) 0.0216(8) -0.0022(6) -0.0001(6) 0.0002(6) C411 0.019(3) 0.022(3) 0.023(3) -0.008(2) -0.001(2) -0.001(3) N412 0.033(3) 0.037(4) 0.031(3) 0.002(3) -0.008(3) -0.005(4) C413 0.033(5) 0.039(5) 0.046(5) -0.006(4) -0.014(4) -0.001(4) C414 0.020(4) 0.037(5) 0.076(6) -0.020(4) -0.010(5) -0.002(4) C415 0.048(6) 0.029(5) 0.056(6) -0.005(4) 0.012(5) -0.011(4) C416 0.031(4) 0.035(5) 0.032(4) 0.003(3) -0.003(3) -0.006(4) C421 0.017(3) 0.023(3) 0.023(3) -0.005(2) -0.001(2) 0.003(2) N422 0.021(3) 0.031(4) 0.035(3) -0.006(3) 0.002(3) 0.002(3) C423 0.047(5) 0.033(4) 0.028(4) -0.008(3) 0.003(3) 0.009(4) C424 0.048(6) 0.057(6) 0.029(4) -0.009(4) 0.012(4) 0.006(5) C425 0.030(4) 0.063(6) 0.041(4) 0.012(5) 0.013(3) -0.009(5) C426 0.026(4) 0.028(4) 0.043(4) 0.001(3) 0.004(3) -0.010(3) P5 0.0211(9) 0.0159(8) 0.0306(8) 0.0008(6) -0.0037(8) -0.0021(7) C511 0.022(4) 0.024(4) 0.050(5) -0.001(3) -0.002(3) -0.002(3) N512 0.031(4) 0.027(4) 0.060(5) 0.004(3) 0.004(3) -0.001(3) C513 0.028(5) 0.022(4) 0.097(8) 0.005(5) -0.004(5) -0.005(3) C514 0.038(5) 0.025(4) 0.072(7) -0.012(4) -0.009(5) 0.006(4) C515 0.040(5) 0.039(5) 0.060(6) -0.019(4) -0.010(5) 0.007(4) C516 0.037(5) 0.027(4) 0.058(6) -0.012(4) -0.016(4) 0.008(4) C50 0.025(4) 0.037(4) 0.029(4) 0.006(3) -0.001(3) -0.008(3) C56 0.027(4) 0.023(4) 0.050(5) 0.002(3) -0.013(4) 0.004(3) C60 0.024(3) 0.021(3) 0.035(3) -0.006(3) -0.011(3) 0.000(3) P6 0.0184(9) 0.0184(8) 0.0284(9) -0.0030(7) 0.0013(7) -0.0012(7) C611 0.018(3) 0.016(3) 0.034(3) -0.001(3) 0.001(3) 0.005(3) N612 0.018(3) 0.033(3) 0.042(3) -0.002(3) 0.003(2) 0.001(3) C614 0.038(5) 0.025(4) 0.041(4) 0.011(3) 0.018(4) 0.021(4) C615 0.080(8) 0.022(4) 0.034(4) -0.002(3) 0.000(5) 0.026(5) C616 0.033(5) 0.036(5) 0.030(4) -0.004(3) -0.003(3) 0.003(4) C621 0.016(3) 0.013(3) 0.037(4) -0.001(3) 0.003(3) -0.002(2) N622 0.035(4) 0.025(3) 0.032(3) -0.002(3) 0.011(3) 0.004(3) C623 0.035(4) 0.023(4) 0.035(4) 0.002(3) 0.000(3) 0.005(3) C624 0.030(4) 0.015(3) 0.050(5) 0.004(3) 0.005(4) 0.004(3) C625 0.042(5) 0.027(4) 0.058(6) -0.008(4) -0.014(4) -0.003(4) C626 0.046(5) 0.026(4) 0.045(5) -0.005(4) -0.013(4) -0.001(4) P7 0.0190(8) 0.0212(9) 0.0225(7) -0.0032(7) 0.0011(6) -0.0006(7) C711 0.021(3) 0.021(3) 0.027(3) -0.011(3) -0.001(3) 0.002(3) N712 0.034(3) 0.039(4) 0.027(3) -0.009(3) -0.007(2) -0.006(3) C713 0.048(6) 0.040(5) 0.040(5) -0.011(4) -0.020(4) 0.008(4) C714 0.025(4) 0.039(5) 0.048(5) -0.013(4) -0.011(4) 0.000(4) C715 0.035(5) 0.034(5) 0.046(5) -0.007(4) 0.002(4) -0.013(4) C716 0.022(3) 0.024(4) 0.026(3) -0.008(3) -0.002(3) 0.002(3) C721 0.019(3) 0.031(4) 0.028(3) -0.005(3) -0.002(3) 0.000(3) N722 0.035(4) 0.029(4) 0.038(4) -0.009(3) 0.007(3) 0.005(3) C723 0.034(5) 0.044(5) 0.041(5) -0.024(4) 0.001(4) 0.006(4) C724 0.024(4) 0.074(7) 0.030(4) -0.023(4) 0.006(3) 0.002(4) C725 0.023(4) 0.058(6) 0.033(4) 0.002(4) 0.008(3) -0.009(4) C726 0.024(4) 0.056(6) 0.032(4) -0.004(4) 0.001(3) -0.007(4) C70 0.028(4) 0.031(4) 0.024(3) -0.004(3) -0.001(3) -0.004(3) C78 0.029(4) 0.026(4) 0.032(4) 0.006(3) 0.000(3) 0.007(3) P8 0.0200(8) 0.0214(9) 0.0272(8) -0.0060(7) 0.0024(6) 0.0032(7) C811 0.019(3) 0.027(3) 0.027(3) -0.003(2) 0.002(3) 0.009(3) N812 0.025(3) 0.023(3) 0.034(3) -0.008(3) 0.004(3) 0.007(3) C813 0.024(4) 0.030(4) 0.041(4) -0.007(3) 0.006(3) 0.008(3) C814 0.017(4) 0.051(5) 0.038(4) 0.006(4) 0.004(3) 0.003(4) C815 0.023(4) 0.027(4) 0.073(6) 0.012(5) -0.006(4) 0.000(4) C816 0.027(4) 0.022(4) 0.051(5) -0.001(3) -0.004(3) 0.011(3) C821 0.018(4) 0.041(5) 0.033(4) -0.017(3) 0.007(3) 0.005(3) N822 0.040(4) 0.042(5) 0.053(5) -0.027(4) 0.006(4) -0.004(4) C823 0.053(7) 0.066(7) 0.082(8) -0.045(6) 0.018(7) -0.015(6) C824 0.060(8) 0.117(12) 0.053(7) -0.054(8) -0.005(6) -0.001(8) C825 0.075(9) 0.134(13) 0.028(5) -0.014(6) -0.004(6) 0.015(9) C826 0.054(6) 0.073(7) 0.023(4) -0.010(5) 0.001(3) 0.011(6) O01 0.054(5) 0.040(4) 0.078(5) 0.008(3) -0.021(4) -0.014(3) O02 0.039(4) 0.030(3) 0.066(4) -0.013(3) -0.006(3) -0.001(3) O03 0.042(5) 0.103(7) 0.078(6) 0.004(5) 0.009(4) -0.005(5) O04 0.163(13) 0.170(13) 0.079(7) 0.024(8) -0.030(8) 0.039(10) O05 0.104(10) 0.113(10) 0.231(15) 0.099(10) -0.051(10) -0.017(8) O06 0.064(11) 0.148(18) 0.049(9) -0.060(11) 0.002(8) -0.007(11) O07 0.031(8) 0.097(13) 0.077(11) 0.021(9) 0.021(7) 0.019(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 P2 2.3552(17) . ? Au1 P4 2.3734(18) . ? Au1 P3 2.3999(17) . ? Au1 P1 2.4016(19) . ? Au2 P5 2.3804(18) . ? Au2 P8 2.3978(18) . ? Au2 P7 2.3993(17) . ? Au2 P6 2.4073(19) . ? P1 C10 1.832(7) . ? P1 C121 1.842(7) . ? P1 C111 1.872(7) . ? C111 C116 1.330(11) . ? C111 N112 1.347(10) . ? N112 C113 1.338(11) . ? C113 C114 1.390(13) . ? C113 H113 0.95 . ? C114 C115 1.345(14) . ? C114 H114 0.95 . ? C115 C116 1.396(12) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 N122 1.331(9) . ? C121 C126 1.376(10) . ? N122 C123 1.325(10) . ? C123 C124 1.398(12) . ? C123 H123 0.95 . ? C124 C125 1.371(12) . ? C124 H124 0.95 . ? C125 C126 1.393(12) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 C12 1.540(10) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C12 C20 1.541(10) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? C20 P2 1.838(7) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P2 C211 1.825(7) . ? P2 C221 1.856(7) . ? C211 N212 1.363(10) . ? C211 C216 1.388(11) . ? N212 C213 1.340(11) . ? C213 C214 1.378(14) . ? C213 H213 0.95 . ? C214 C215 1.390(13) . ? C214 H214 0.95 . ? C215 C216 1.373(11) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 N222 1.332(9) . ? C221 C226 1.379(9) . ? N222 C223 1.350(10) . ? C223 C224 1.390(11) . ? C223 H223 0.95 . ? C224 C225 1.398(12) . ? C224 H224 0.95 . ? C225 C226 1.421(10) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? P3 C30 1.831(7) . ? P3 C321 1.840(7) . ? P3 C311 1.851(7) . ? C311 N312 1.338(10) . ? C311 C316 1.343(10) . ? N312 C313 1.316(12) . ? C313 C314 1.410(15) . ? C313 H313 0.95 . ? C314 C315 1.399(14) . ? C314 H314 0.95 . ? C315 C316 1.378(12) . ? C315 H315 0.95 . ? C316 H316 0.95 . ? C321 N322 1.326(10) . ? C321 C326 1.385(11) . ? N322 C323 1.364(10) . ? C323 C324 1.375(14) . ? C323 H323 0.95 . ? C324 C325 1.358(14) . ? C324 H324 0.95 . ? C325 C326 1.419(11) . ? C325 H325 0.95 . ? C326 H326 0.95 . ? C30 C34 1.555(11) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C34 C40 1.513(10) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C40 P4 1.817(7) . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? P4 C411 1.830(7) . ? P4 C421 1.858(7) . ? C411 N412 1.355(9) . ? C411 C416 1.381(11) . ? N412 C413 1.357(10) . ? C413 C414 1.393(13) . ? C413 H413 0.95 . ? C414 C415 1.386(14) . ? C414 H414 0.95 . ? C415 C416 1.372(12) . ? C415 H415 0.95 . ? C416 H416 0.95 . ? C421 N422 1.321(9) . ? C421 C426 1.396(10) . ? N422 C423 1.329(10) . ? C423 C424 1.371(12) . ? C423 H423 0.95 . ? C424 C425 1.386(14) . ? C424 H424 0.95 . ? C425 C426 1.363(12) . ? C425 H425 0.95 . ? C426 H426 0.95 . ? P5 C50 1.805(8) . ? P5 C521 1.820(8) . ? P5 C511 1.831(8) . ? C511 N512 1.365(11) . ? C511 C516 1.385(13) . ? N512 C513 1.352(12) . ? C513 C514 1.366(14) . ? C513 H513 0.95 . ? C514 C515 1.336(14) . ? C514 H514 0.95 . ? C515 C516 1.390(12) . ? C515 H515 0.95 . ? C516 H516 0.95 . ? C521 C526 1.360(13) . ? C521 N522 1.376(12) . ? N522 C523 1.548(17) . ? C523 C524 1.252(17) . ? C523 H523 0.95 . ? C524 C525 1.407(19) . ? C524 H524 0.95 . ? C525 C526 1.314(18) . ? C525 H525 0.95 . ? C526 H526 0.95 . ? C50 C56 1.561(11) . ? C50 H50A 0.99 . ? C50 H50B 0.99 . ? C56 C60 1.541(11) . ? C56 H56A 0.99 . ? C56 H56B 0.99 . ? C60 P6 1.828(7) . ? C60 H60A 0.99 . ? C60 H60B 0.99 . ? P6 C611 1.831(7) . ? P6 C621 1.847(7) . ? C611 C616 1.361(10) . ? C611 N612 1.371(9) . ? N612 C613 1.317(11) . ? C613 C614 1.380(12) . ? C613 H613 0.95 . ? C614 C615 1.342(14) . ? C614 H614 0.95 . ? C615 C616 1.400(12) . ? C615 H615 0.95 . ? C616 H616 0.95 . ? C621 N622 1.311(10) . ? C621 C626 1.395(11) . ? N622 C623 1.330(10) . ? C623 C624 1.424(11) . ? C623 H623 0.95 . ? C624 C625 1.344(12) . ? C624 H624 0.95 . ? C625 C626 1.400(12) . ? C625 H625 0.95 . ? C626 H626 0.95 . ? P7 C721 1.828(8) . ? P7 C711 1.834(7) . ? P7 C70 1.840(8) . ? C711 N712 1.345(9) . ? C711 C716 1.376(10) . ? N712 C713 1.353(11) . ? C713 C714 1.360(13) . ? C713 H713 0.95 . ? C714 C715 1.371(12) . ? C714 H714 0.95 . ? C715 C716 1.398(11) . ? C715 H715 0.95 . ? C716 H716 0.95 . ? C721 N722 1.361(10) . ? C721 C726 1.374(11) . ? N722 C723 1.335(10) . ? C723 C724 1.358(13) . ? C723 H723 0.95 . ? C724 C725 1.371(13) . ? C724 H724 0.95 . ? C725 C726 1.420(11) . ? C725 H725 0.95 . ? C726 H726 0.95 . ? C70 C78 1.504(10) . ? C70 H70A 0.99 . ? C70 H70B 0.99 . ? C78 C80 1.533(10) . ? C78 H78A 0.99 . ? C78 H78B 0.99 . ? C80 P8 1.825(8) . ? C80 H80A 0.99 . ? C80 H80B 0.99 . ? P8 C821 1.828(8) . ? P8 C811 1.832(8) . ? C811 N812 1.361(9) . ? C811 C816 1.397(11) . ? N812 C813 1.338(10) . ? C813 C814 1.360(12) . ? C813 H813 0.95 . ? C814 C815 1.410(12) . ? C814 H814 0.95 . ? C815 C816 1.376(11) . ? C815 H815 0.95 . ? C816 H816 0.95 . ? C821 N822 1.359(11) . ? C821 C826 1.386(12) . ? N822 C823 1.382(13) . ? C823 C824 1.367(19) . ? C823 H823 0.95 . ? C824 C825 1.36(2) . ? C824 H824 0.95 . ? C825 C826 1.386(15) . ? C825 H825 0.95 . ? C826 H826 0.95 . ? O09 O09' 1.30(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 P2 Au1 P4 128.19(6) . . ? P2 Au1 P3 116.42(6) . . ? P4 Au1 P3 93.39(6) . . ? P2 Au1 P1 96.41(6) . . ? P4 Au1 P1 115.78(6) . . ? P3 Au1 P1 106.03(6) . . ? P5 Au2 P8 117.49(7) . . ? P5 Au2 P7 126.83(6) . . ? P8 Au2 P7 93.29(6) . . ? P5 Au2 P6 95.66(7) . . ? P8 Au2 P6 106.39(6) . . ? P7 Au2 P6 117.02(6) . . ? C10 P1 C121 105.4(3) . . ? C10 P1 C111 101.9(3) . . ? C121 P1 C111 103.5(3) . . ? C10 P1 Au1 111.3(2) . . ? C121 P1 Au1 115.9(2) . . ? C111 P1 Au1 117.2(3) . . ? C116 C111 N112 125.0(7) . . ? C116 C111 P1 119.6(6) . . ? N112 C111 P1 115.2(6) . . ? C113 N112 C111 116.1(7) . . ? N112 C113 C114 122.5(9) . . ? N112 C113 H113 118.8 . . ? C114 C113 H113 118.8 . . ? C115 C114 C113 119.1(8) . . ? C115 C114 H114 120.5 . . ? C113 C114 H114 120.5 . . ? C114 C115 C116 119.2(9) . . ? C114 C115 H115 120.4 . . ? C116 C115 H115 120.4 . . ? C111 C116 C115 118.1(8) . . ? C111 C116 H116 121 . . ? C115 C116 H116 121 . . ? N122 C121 C126 123.3(7) . . ? N122 C121 P1 112.9(5) . . ? C126 C121 P1 123.6(6) . . ? C123 N122 C121 116.4(7) . . ? N122 C123 C124 125.4(8) . . ? N122 C123 H123 117.3 . . ? C124 C123 H123 117.3 . . ? C125 C124 C123 116.8(7) . . ? C125 C124 H124 121.6 . . ? C123 C124 H124 121.6 . . ? C124 C125 C126 118.9(8) . . ? C124 C125 H125 120.6 . . ? C126 C125 H125 120.6 . . ? C121 C126 C125 119.1(8) . . ? C121 C126 H126 120.5 . . ? C125 C126 H126 120.5 . . ? C12 C10 P1 113.8(5) . . ? C12 C10 H10A 108.8 . . ? P1 C10 H10A 108.8 . . ? C12 C10 H10B 108.8 . . ? P1 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C10 C12 C20 114.3(6) . . ? C10 C12 H12A 108.7 . . ? C20 C12 H12A 108.7 . . ? C10 C12 H12B 108.7 . . ? C20 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C12 C20 P2 115.9(5) . . ? C12 C20 H20A 108.3 . . ? P2 C20 H20A 108.3 . . ? C12 C20 H20B 108.3 . . ? P2 C20 H20B 108.3 . . ? H20A C20 H20B 107.4 . . ? C211 P2 C20 102.7(3) . . ? C211 P2 C221 104.6(3) . . ? C20 P2 C221 101.9(3) . . ? C211 P2 Au1 117.5(2) . . ? C20 P2 Au1 112.5(2) . . ? C221 P2 Au1 115.8(2) . . ? N212 C211 C216 123.1(7) . . ? N212 C211 P2 115.4(5) . . ? C216 C211 P2 121.3(6) . . ? C213 N212 C211 116.1(8) . . ? N212 C213 C214 124.6(9) . . ? N212 C213 H213 117.7 . . ? C214 C213 H213 117.7 . . ? C213 C214 C215 118.0(8) . . ? C213 C214 H214 121 . . ? C215 C214 H214 121 . . ? C216 C215 C214 119.4(9) . . ? C216 C215 H215 120.3 . . ? C214 C215 H215 120.3 . . ? C215 C216 C211 118.8(8) . . ? C215 C216 H216 120.6 . . ? C211 C216 H216 120.6 . . ? N222 C221 C226 123.0(7) . . ? N222 C221 P2 114.7(5) . . ? C226 C221 P2 121.6(5) . . ? C221 N222 C223 118.2(6) . . ? N222 C223 C224 123.6(7) . . ? N222 C223 H223 118.2 . . ? C224 C223 H223 118.2 . . ? C223 C224 C225 118.1(7) . . ? C223 C224 H224 120.9 . . ? C225 C224 H224 120.9 . . ? C224 C225 C226 118.0(7) . . ? C224 C225 H225 121 . . ? C226 C225 H225 121 . . ? C221 C226 C225 119.1(7) . . ? C221 C226 H226 120.5 . . ? C225 C226 H226 120.5 . . ? C30 P3 C321 105.6(4) . . ? C30 P3 C311 102.7(4) . . ? C321 P3 C311 102.6(3) . . ? C30 P3 Au1 110.6(2) . . ? C321 P3 Au1 114.0(2) . . ? C311 P3 Au1 119.8(2) . . ? N312 C311 C316 121.8(7) . . ? N312 C311 P3 115.6(5) . . ? C316 C311 P3 122.6(6) . . ? C313 N312 C311 117.9(8) . . ? N312 C313 C314 123.9(9) . . ? N312 C313 H313 118 . . ? C314 C313 H313 118 . . ? C315 C314 C313 117.3(8) . . ? C315 C314 H314 121.4 . . ? C313 C314 H314 121.4 . . ? C316 C315 C314 116.5(8) . . ? C316 C315 H315 121.7 . . ? C314 C315 H315 121.7 . . ? C311 C316 C315 122.6(8) . . ? C311 C316 H316 118.7 . . ? C315 C316 H316 118.7 . . ? N322 C321 C326 123.2(7) . . ? N322 C321 P3 119.6(6) . . ? C326 C321 P3 117.0(6) . . ? C321 N322 C323 117.7(7) . . ? N322 C323 C324 122.7(8) . . ? N322 C323 H323 118.7 . . ? C324 C323 H323 118.7 . . ? C325 C324 C323 119.6(8) . . ? C325 C324 H324 120.2 . . ? C323 C324 H324 120.2 . . ? C324 C325 C326 118.7(8) . . ? C324 C325 H325 120.7 . . ? C326 C325 H325 120.7 . . ? C321 C326 C325 118.1(8) . . ? C321 C326 H326 120.9 . . ? C325 C326 H326 121 . . ? C34 C30 P3 112.5(5) . . ? C34 C30 H30A 109.1 . . ? P3 C30 H30A 109.1 . . ? C34 C30 H30B 109.1 . . ? P3 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C40 C34 C30 115.4(6) . . ? C40 C34 H34A 108.4 . . ? C30 C34 H34A 108.4 . . ? C40 C34 H34B 108.4 . . ? C30 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? C34 C40 P4 116.6(5) . . ? C34 C40 H40A 108.2 . . ? P4 C40 H40A 108.2 . . ? C34 C40 H40B 108.2 . . ? P4 C40 H40B 108.2 . . ? H40A C40 H40B 107.3 . . ? C40 P4 C411 104.3(3) . . ? C40 P4 C421 104.4(3) . . ? C411 P4 C421 98.8(3) . . ? C40 P4 Au1 110.7(2) . . ? C411 P4 Au1 115.1(2) . . ? C421 P4 Au1 121.6(2) . . ? N412 C411 C416 123.8(7) . . ? N412 C411 P4 116.4(5) . . ? C416 C411 P4 119.8(6) . . ? C411 N412 C413 117.0(7) . . ? N412 C413 C414 122.1(8) . . ? N412 C413 H413 118.9 . . ? C414 C413 H413 118.9 . . ? C415 C414 C413 119.1(8) . . ? C415 C414 H414 120.5 . . ? C413 C414 H414 120.5 . . ? C416 C415 C414 119.6(9) . . ? C416 C415 H415 120.2 . . ? C414 C415 H415 120.2 . . ? C415 C416 C411 118.4(8) . . ? C415 C416 H416 120.8 . . ? C411 C416 H416 120.8 . . ? N422 C421 C426 123.1(7) . . ? N422 C421 P4 113.0(5) . . ? C426 C421 P4 123.8(6) . . ? C421 N422 C423 117.3(7) . . ? N422 C423 C424 123.9(8) . . ? N422 C423 H423 118.1 . . ? C424 C423 H423 118.1 . . ? C423 C424 C425 118.4(8) . . ? C423 C424 H424 120.8 . . ? C425 C424 H424 120.8 . . ? C426 C425 C424 118.7(8) . . ? C426 C425 H425 120.7 . . ? C424 C425 H425 120.7 . . ? C425 C426 C421 118.7(8) . . ? C425 C426 H426 120.6 . . ? C421 C426 H426 120.6 . . ? C50 P5 C521 102.7(4) . . ? C50 P5 C511 101.6(4) . . ? C521 P5 C511 104.6(4) . . ? C50 P5 Au2 111.7(3) . . ? C521 P5 Au2 116.7(3) . . ? C511 P5 Au2 117.5(3) . . ? N512 C511 C516 122.3(8) . . ? N512 C511 P5 117.2(7) . . ? C516 C511 P5 120.4(6) . . ? C513 N512 C511 114.2(8) . . ? N512 C513 C514 125.6(9) . . ? N512 C513 H513 117.2 . . ? C514 C513 H513 117.2 . . ? C515 C514 C513 119.8(9) . . ? C515 C514 H514 120.1 . . ? C513 C514 H514 120.1 . . ? C514 C515 C516 117.6(10) . . ? C514 C515 H515 121.2 . . ? C516 C515 H515 121.2 . . ? C511 C516 C515 120.4(9) . . ? C511 C516 H516 119.8 . . ? C515 C516 H516 119.8 . . ? C526 C521 N522 126.3(9) . . ? C526 C521 P5 117.6(7) . . ? N522 C521 P5 114.1(7) . . ? C521 N522 C523 107.5(9) . . ? C524 C523 N522 126.1(14) . . ? C524 C523 H523 116.9 . . ? N522 C523 H523 116.9 . . ? C523 C524 C525 117.3(16) . . ? C523 C524 H524 121.4 . . ? C525 C524 H524 121.4 . . ? C526 C525 C524 122.9(15) . . ? C526 C525 H525 118.5 . . ? C524 C525 H525 118.5 . . ? C525 C526 C521 118.2(12) . . ? C525 C526 H526 120.9 . . ? C521 C526 H526 120.9 . . ? C56 C50 P5 114.5(6) . . ? C56 C50 H50A 108.6 . . ? P5 C50 H50A 108.6 . . ? C56 C50 H50B 108.6 . . ? P5 C50 H50B 108.6 . . ? H50A C50 H50B 107.6 . . ? C60 C56 C50 113.3(7) . . ? C60 C56 H56A 108.9 . . ? C50 C56 H56A 108.9 . . ? C60 C56 H56B 108.9 . . ? C50 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? C56 C60 P6 113.5(5) . . ? C56 C60 H60A 108.9 . . ? P6 C60 H60A 108.9 . . ? C56 C60 H60B 108.9 . . ? P6 C60 H60B 108.9 . . ? H60A C60 H60B 107.7 . . ? C60 P6 C611 101.0(3) . . ? C60 P6 C621 104.4(3) . . ? C611 P6 C621 105.5(3) . . ? C60 P6 Au2 113.5(2) . . ? C611 P6 Au2 115.6(2) . . ? C621 P6 Au2 115.3(2) . . ? C616 C611 N612 122.1(7) . . ? C616 C611 P6 119.6(6) . . ? N612 C611 P6 118.3(5) . . ? C613 N612 C611 116.0(7) . . ? N612 C613 C614 125.8(9) . . ? N612 C613 H613 117.1 . . ? C614 C613 H613 117.1 . . ? C615 C614 C613 117.2(8) . . ? C615 C614 H614 121.4 . . ? C613 C614 H614 121.4 . . ? C614 C615 C616 120.0(8) . . ? C614 C615 H615 120 . . ? C616 C615 H615 120 . . ? C611 C616 C615 118.9(8) . . ? C611 C616 H616 120.5 . . ? C615 C616 H616 120.5 . . ? N622 C621 C626 124.1(7) . . ? N622 C621 P6 113.5(5) . . ? C626 C621 P6 122.2(6) . . ? C621 N622 C623 118.3(7) . . ? N622 C623 C624 122.2(7) . . ? N622 C623 H623 118.9 . . ? C624 C623 H623 118.9 . . ? C625 C624 C623 118.2(7) . . ? C625 C624 H624 120.9 . . ? C623 C624 H624 120.9 . . ? C624 C625 C626 120.4(8) . . ? C624 C625 H625 119.8 . . ? C626 C625 H625 119.8 . . ? C621 C626 C625 116.8(8) . . ? C621 C626 H626 121.6 . . ? C625 C626 H626 121.6 . . ? C721 P7 C711 100.3(3) . . ? C721 P7 C70 102.6(3) . . ? C711 P7 C70 102.2(3) . . ? C721 P7 Au2 122.8(2) . . ? C711 P7 Au2 115.1(2) . . ? C70 P7 Au2 111.2(2) . . ? N712 C711 C716 122.6(7) . . ? N712 C711 P7 116.5(6) . . ? C716 C711 P7 120.9(6) . . ? C711 N712 C713 117.4(8) . . ? N712 C713 C714 123.9(8) . . ? N712 C713 H713 118.1 . . ? C714 C713 H713 118.1 . . ? C713 C714 C715 118.1(8) . . ? C713 C714 H714 121 . . ? C715 C714 H714 121 . . ? C714 C715 C716 119.9(8) . . ? C714 C715 H715 120 . . ? C716 C715 H715 120 . . ? C711 C716 C715 118.1(7) . . ? C711 C716 H716 120.9 . . ? C715 C716 H716 120.9 . . ? N722 C721 C726 121.7(8) . . ? N722 C721 P7 112.9(6) . . ? C726 C721 P7 125.4(7) . . ? C723 N722 C721 117.1(8) . . ? N722 C723 C724 125.2(9) . . ? N722 C723 H723 117.4 . . ? C724 C723 H723 117.4 . . ? C723 C724 C725 118.5(8) . . ? C723 C724 H724 120.8 . . ? C725 C724 H724 120.8 . . ? C724 C725 C726 118.3(8) . . ? C724 C725 H725 120.9 . . ? C726 C725 H725 120.9 . . ? C721 C726 C725 119.2(9) . . ? C721 C726 H726 120.4 . . ? C725 C726 H726 120.4 . . ? C78 C70 P7 112.9(5) . . ? C78 C70 H70A 109 . . ? P7 C70 H70A 109 . . ? C78 C70 H70B 109 . . ? P7 C70 H70B 109 . . ? H70A C70 H70B 107.8 . . ? C70 C78 C80 117.6(7) . . ? C70 C78 H78A 107.9 . . ? C80 C78 H78A 107.9 . . ? C70 C78 H78B 107.9 . . ? C80 C78 H78B 107.9 . . ? H78A C78 H78B 107.2 . . ? C78 C80 P8 114.0(5) . . ? C78 C80 H80A 108.8 . . ? P8 C80 H80A 108.8 . . ? C78 C80 H80B 108.8 . . ? P8 C80 H80B 108.8 . . ? H80A C80 H80B 107.7 . . ? C80 P8 C821 102.7(4) . . ? C80 P8 C811 102.4(3) . . ? C821 P8 C811 103.2(3) . . ? C80 P8 Au2 114.6(3) . . ? C821 P8 Au2 113.4(3) . . ? C811 P8 Au2 118.5(2) . . ? N812 C811 C816 123.0(7) . . ? N812 C811 P8 115.6(6) . . ? C816 C811 P8 121.4(5) . . ? C813 N812 C811 114.7(7) . . ? N812 C813 C814 127.1(7) . . ? N812 C813 H813 116.5 . . ? C814 C813 H813 116.5 . . ? C813 C814 C815 117.5(8) . . ? C813 C814 H814 121.3 . . ? C815 C814 H814 121.3 . . ? C816 C815 C814 117.9(9) . . ? C816 C815 H815 121 . . ? C814 C815 H815 121 . . ? C815 C816 C811 119.8(8) . . ? C815 C816 H816 120.1 . . ? C811 C816 H816 120.1 . . ? N822 C821 C826 124.8(8) . . ? N822 C821 P8 117.2(6) . . ? C826 C821 P8 117.7(7) . . ? C821 N822 C823 114.7(9) . . ? C824 C823 N822 124.6(12) . . ? C824 C823 H823 117.7 . . ? N822 C823 H823 117.7 . . ? C825 C824 C823 117.1(10) . . ? C825 C824 H824 121.4 . . ? C823 C824 H824 121.4 . . ? C824 C825 C826 122.7(12) . . ? C824 C825 H825 118.6 . . ? C826 C825 H825 118.6 . . ? C821 C826 C825 116.0(12) . . ? C821 C826 H826 122 . . ? C825 C826 H826 122 . . ? #===END # Attachment 'Compound3new.cif' #======================================================================= # Data block for single structure (one for each study in the paper) #======================================================================= data_gk128 _database_code_depnum_ccdc_archive 'CCDC 640095' _audit_creation_date 2007-03-12T11:35:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C44 H50 Au Cl N8 O5 P4' _chemical_formula_moiety 'C44 H40 Au N8 P4, Cl, 5(H2 O)' _chemical_formula_weight 1127.22 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I_41/a _symmetry_space_group_name_Hall -i_4ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 13.4748(9) _cell_length_b 13.4748(9) _cell_length_c 53.133(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 9647.4(11) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 24.6 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4528 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.29 _exptl_crystal_description bar _exptl_crystal_size_max .18 _exptl_crystal_size_mid .13 _exptl_crystal_size_min .11 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .52 _exptl_absorpt_correction_T_max .79 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_av_unetI/netI 0.0187 _diffrn_reflns_number 12696 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -90 _diffrn_reflns_limit_l_max 90 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 37.51 _diffrn_reflns_theta_full 37.5 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 12696 _reflns_number_gt 9829 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0470P)^2^+15.4346P] 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_number_reflns 12696 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.951 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.147 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Au Au 0.5 0.25 0.086920(2) 0.01713(3) Uani 1 2 d S . . Cl1 Cl 1 0.25 0.125 0.0549(5) Uani 1 4 d S . . Cl2 Cl -0.1462(4) 0.2810(4) -0.02602(8) 0.0659(11) Uani 0.25 1 d P . . P1 P 0.65254(4) 0.19824(4) 0.106208(10) 0.01949(9) Uani 1 1 d . . . C111 C 0.70757(15) 0.08122(15) 0.09601(4) 0.0214(3) Uani 1 1 d . . . C112 C 0.7297(2) 0.0036(2) 0.11233(5) 0.0325(5) Uani 1 1 d . . . H112 H 0.7138 0.012 0.1296 0.039 Uiso 1 1 calc R . . N113 N 0.7720(2) -0.08239(19) 0.10544(5) 0.0428(6) Uani 1 1 d . . . C114 C 0.7936(2) -0.0928(2) 0.08112(5) 0.0356(5) Uani 1 1 d . . . H114 H 0.8236 -0.1532 0.0759 0.043 Uiso 1 1 calc R . . C115 C 0.7752(2) -0.0222(2) 0.06324(5) 0.0366(6) Uani 1 1 d . . . H115 H 0.7927 -0.0331 0.0461 0.044 Uiso 1 1 calc R . . C116 C 0.7306(2) 0.06575(19) 0.07062(5) 0.0337(5) Uani 1 1 d . . . H116 H 0.7157 0.1154 0.0585 0.04 Uiso 1 1 calc R . . C121 C 0.66741(17) 0.19460(17) 0.14006(4) 0.0245(4) Uani 1 1 d . . . C122 C 0.5864(2) 0.1689(2) 0.15508(4) 0.0306(5) Uani 1 1 d . . . H122 H 0.5258 0.1523 0.147 0.037 Uiso 1 1 calc R . . N123 N 0.5894(3) 0.1662(2) 0.18054(5) 0.0467(7) Uani 1 1 d . . . C124 C 0.6777(4) 0.1888(3) 0.19135(6) 0.0561(10) Uani 1 1 d . . . H124 H 0.6818 0.1878 0.2092 0.067 Uiso 1 1 calc R . . C125 C 0.7628(3) 0.2135(3) 0.17784(6) 0.0515(9) Uani 1 1 d . . . H125 H 0.8233 0.2279 0.1862 0.062 Uiso 1 1 calc R . . C126 C 0.7568(2) 0.2162(2) 0.15215(5) 0.0373(6) Uani 1 1 d . . . H126 H 0.8137 0.2329 0.1425 0.045 Uiso 1 1 calc R . . C10 C 0.74324(16) 0.29267(17) 0.09594(4) 0.0248(4) Uani 1 1 d . . . H10A H 0.7378 0.3515 0.107 0.03 Uiso 1 1 calc R . . H10B H 0.8111 0.2655 0.0978 0.03 Uiso 1 1 calc R . . C20 C 0.72755(16) 0.32514(17) 0.06846(4) 0.0248(4) Uani 1 1 d . . . H20A H 0.7427 0.269 0.0571 0.03 Uiso 1 1 calc R . . H20B H 0.7735 0.3802 0.0644 0.03 Uiso 1 1 calc R . . P2 P 0.59917(4) 0.36588(4) 0.063390(10) 0.01881(9) Uani 1 1 d . . . C211 C 0.58329(17) 0.36969(15) 0.02945(4) 0.0223(3) Uani 1 1 d . . . C212 C 0.48575(19) 0.37739(17) 0.02027(4) 0.0264(4) Uani 1 1 d . . . H212 H 0.4331 0.3821 0.0321 0.032 Uiso 1 1 calc R . . N213 N 0.4629(2) 0.37847(17) -0.00435(4) 0.0367(5) Uani 1 1 d . . . C214 C 0.5401(3) 0.3703(2) -0.02059(5) 0.0433(7) Uani 1 1 d . . . H214 H 0.5259 0.37 -0.0381 0.052 Uiso 1 1 calc R . . C215 C 0.6372(3) 0.3625(2) -0.01334(5) 0.0408(6) Uani 1 1 d . . . H215 H 0.6885 0.3571 -0.0255 0.049 Uiso 1 1 calc R . . C216 C 0.6593(2) 0.3625(2) 0.01195(5) 0.0314(5) Uani 1 1 d . . . H216 H 0.7263 0.3577 0.0174 0.038 Uiso 1 1 calc R . . C221 C 0.60450(16) 0.49622(15) 0.07248(4) 0.0209(3) Uani 1 1 d . . . C222 C 0.54986(19) 0.53217(18) 0.09279(5) 0.0281(4) Uani 1 1 d . . . H222 H 0.5079 0.4883 0.1019 0.034 Uiso 1 1 calc R . . N223 N 0.5556(2) 0.62928(19) 0.09986(5) 0.0413(5) Uani 1 1 d . . . C224 C 0.6167(2) 0.6902(2) 0.08659(6) 0.0375(6) Uani 1 1 d . . . H224 H 0.6212 0.7577 0.0916 0.045 Uiso 1 1 calc R . . C225 C 0.67175(19) 0.66011(17) 0.06659(5) 0.0316(5) Uani 1 1 d . . . H225 H 0.7131 0.7054 0.0578 0.038 Uiso 1 1 calc R . . C226 C 0.66585(19) 0.56335(17) 0.05955(5) 0.0291(4) Uani 1 1 d . . . H226 H 0.7039 0.5407 0.0456 0.035 Uiso 1 1 calc R . . O01 O -0.2353(2) 0.1232(2) 0.00497(6) 0.0624(7) Uani 1 1 d . . . O02 O 0.8997(2) 0.4642(3) -0.00098(6) 0.0710(9) Uani 1 1 d . . . O03 O -0.0300(12) 0.242(2) 0.0654(2) 0.165(9) Uani 0.5 1 d P . . 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 Au 0.01656(4) 0.01852(5) 0.01630(4) 0 0 -0.00061(3) Cl1 0.0341(4) 0.0341(4) 0.0965(15) 0 0 0 Cl2 0.078(3) 0.070(3) 0.050(2) -0.0145(18) 0.0165(19) 0.010(2) P1 0.0188(2) 0.0211(2) 0.0186(2) 0.00124(17) -0.00255(16) -0.00025(16) C111 0.0211(8) 0.0213(8) 0.0220(8) 0.0016(6) -0.0039(6) 0.0007(6) C112 0.0421(13) 0.0305(11) 0.0248(10) 0.0061(8) 0.0035(9) 0.0095(9) N113 0.0641(17) 0.0329(11) 0.0313(11) 0.0074(9) 0.0054(11) 0.0179(11) C114 0.0475(15) 0.0262(11) 0.0330(12) -0.0012(9) -0.0014(11) 0.0104(10) C115 0.0548(17) 0.0297(11) 0.0254(11) -0.0033(9) -0.0004(11) 0.0072(11) C116 0.0522(15) 0.0259(10) 0.0231(10) 0.0010(8) -0.0044(10) 0.0068(10) C121 0.0273(9) 0.0250(9) 0.0214(9) -0.0008(7) -0.0052(7) 0.0023(7) C122 0.0367(12) 0.0344(12) 0.0207(9) 0.0035(8) -0.0011(8) 0.0015(9) N123 0.072(2) 0.0452(14) 0.0233(10) 0.0041(9) 0.0034(11) 0.0107(13) C124 0.104(3) 0.0410(16) 0.0233(12) -0.0010(11) -0.0180(16) 0.0141(18) C125 0.070(2) 0.0472(17) 0.0374(15) -0.0010(13) -0.0326(16) 0.0012(16) C126 0.0355(13) 0.0449(15) 0.0316(12) -0.0011(11) -0.0139(10) -0.0002(11) C10 0.0195(8) 0.0242(9) 0.0308(10) 0.0021(8) -0.0036(7) -0.0029(7) C20 0.0214(8) 0.0245(9) 0.0284(10) 0.0032(7) 0.0037(7) 0.0005(7) P2 0.0208(2) 0.0177(2) 0.0179(2) 0.00122(16) 0.00109(16) -0.00122(16) C211 0.0301(10) 0.0176(8) 0.0192(8) 0.0012(6) 0.0017(7) -0.0030(7) C212 0.0338(11) 0.0237(9) 0.0218(9) 0.0004(7) -0.0014(8) -0.0013(8) N213 0.0554(15) 0.0273(10) 0.0273(10) 0.0029(8) -0.0106(9) -0.0033(9) C214 0.080(2) 0.0299(12) 0.0195(10) 0.0025(9) -0.0059(12) -0.0036(13) C215 0.0624(19) 0.0401(14) 0.0200(10) 0.0015(9) 0.0130(11) -0.0029(13) C216 0.0356(12) 0.0362(12) 0.0223(9) 0.0014(8) 0.0068(9) -0.0030(9) C221 0.0228(8) 0.0196(8) 0.0202(8) 0.0003(6) -0.0025(6) -0.0018(6) C222 0.0334(11) 0.0252(10) 0.0256(10) -0.0028(8) 0.0027(8) -0.0010(8) N223 0.0523(15) 0.0316(11) 0.0400(13) -0.0104(10) 0.0060(11) 0.0008(10) C224 0.0443(15) 0.0221(10) 0.0461(15) -0.0083(10) -0.0010(12) -0.0032(10) C225 0.0313(11) 0.0193(9) 0.0441(14) -0.0004(9) 0.0026(10) -0.0073(8) C226 0.0308(11) 0.0228(9) 0.0336(11) 0.0013(8) 0.0030(9) -0.0052(8) O01 0.0734(19) 0.0581(17) 0.0556(16) 0.0120(13) 0.0184(14) 0.0017(14) O02 0.0698(19) 0.089(2) 0.0544(16) -0.0293(16) -0.0003(15) -0.0085(17) O03 0.16(2) 0.153(11) 0.179(10) 0.037(11) 0.046(10) 0.114(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Au P1 2.4003(5) . ? Au P1 2.4003(5) 6_554 ? Au P2 2.4056(5) 6_554 ? Au P2 2.4056(5) . ? P1 C121 1.810(2) . ? P1 C111 1.825(2) . ? P1 C10 1.847(2) . ? C111 C112 1.391(3) . ? C111 C116 1.400(3) . ? C112 N113 1.342(4) . ? C112 H112 0.95 . ? N113 C114 1.332(4) . ? C114 C115 1.368(4) . ? C114 H114 0.95 . ? C115 C116 1.385(4) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 C126 1.396(3) . ? C121 C122 1.396(4) . ? C122 N123 1.354(3) . ? C122 H122 0.95 . ? N123 C124 1.357(5) . ? C124 C125 1.392(6) . ? C124 H124 0.95 . ? C125 C126 1.368(4) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C10 C20 1.539(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C20 P2 1.835(2) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? P2 C211 1.817(2) . ? P2 C221 1.823(2) . ? C211 C216 1.387(3) . ? C211 C212 1.406(3) . ? C212 N213 1.344(3) . ? C212 H212 0.95 . ? N213 C214 1.357(4) . ? C214 C215 1.368(5) . ? C214 H214 0.95 . ? C215 C216 1.376(4) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 C222 1.393(3) . ? C221 C226 1.405(3) . ? C222 N223 1.364(3) . ? C222 H222 0.95 . ? N223 C224 1.359(4) . ? C224 C225 1.358(4) . ? C224 H224 0.95 . ? C225 C226 1.359(3) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au P1 129.45(3) . 6_554 ? P1 Au P2 120.593(19) . 6_554 ? P1 Au P2 86.264(19) 6_554 6_554 ? P1 Au P2 86.264(19) . . ? P1 Au P2 120.593(19) 6_554 . ? P2 Au P2 117.37(3) 6_554 . ? C121 P1 C111 103.11(10) . . ? C121 P1 C10 103.81(11) . . ? C111 P1 C10 103.81(10) . . ? C121 P1 Au 121.79(8) . . ? C111 P1 Au 118.18(7) . . ? C10 P1 Au 103.91(7) . . ? C112 C111 C116 116.2(2) . . ? C112 C111 P1 123.49(18) . . ? C116 C111 P1 120.34(17) . . ? N113 C112 C111 124.8(2) . . ? N113 C112 H112 117.6 . . ? C111 C112 H112 117.6 . . ? C114 N113 C112 116.7(2) . . ? N113 C114 C115 124.1(2) . . ? N113 C114 H114 117.9 . . ? C115 C114 H114 117.9 . . ? C114 C115 C116 118.5(2) . . ? C114 C115 H115 120.7 . . ? C116 C115 H115 120.7 . . ? C115 C116 C111 119.8(2) . . ? C115 C116 H116 120.1 . . ? C111 C116 H116 120.1 . . ? C126 C121 C122 117.6(2) . . ? C126 C121 P1 123.2(2) . . ? C122 C121 P1 119.21(17) . . ? N123 C122 C121 123.7(3) . . ? N123 C122 H122 118.2 . . ? C121 C122 H122 118.2 . . ? C122 N123 C124 116.3(3) . . ? N123 C124 C125 123.9(3) . . ? N123 C124 H124 118 . . ? C125 C124 H124 118 . . ? C126 C125 C124 118.2(3) . . ? C126 C125 H125 120.9 . . ? C124 C125 H125 120.9 . . ? C125 C126 C121 120.3(3) . . ? C125 C126 H126 119.8 . . ? C121 C126 H126 119.8 . . ? C20 C10 P1 112.66(15) . . ? C20 C10 H10A 109.1 . . ? P1 C10 H10A 109.1 . . ? C20 C10 H10B 109.1 . . ? P1 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C10 C20 P2 110.72(15) . . ? C10 C20 H20A 109.5 . . ? P2 C20 H20A 109.5 . . ? C10 C20 H20B 109.5 . . ? P2 C20 H20B 109.5 . . ? H20A C20 H20B 108.1 . . ? C211 P2 C221 103.91(10) . . ? C211 P2 C20 105.37(11) . . ? C221 P2 C20 102.25(10) . . ? C211 P2 Au 117.96(7) . . ? C221 P2 Au 120.64(7) . . ? C20 P2 Au 104.67(7) . . ? C216 C211 C212 117.6(2) . . ? C216 C211 P2 125.22(19) . . ? C212 C211 P2 117.19(17) . . ? N213 C212 C211 123.6(2) . . ? N213 C212 H212 118.2 . . ? C211 C212 H212 118.2 . . ? C212 N213 C214 116.3(3) . . ? N213 C214 C215 124.1(2) . . ? N213 C214 H214 117.9 . . ? C215 C214 H214 117.9 . . ? C214 C215 C216 118.8(3) . . ? C214 C215 H215 120.6 . . ? C216 C215 H215 120.6 . . ? C215 C216 C211 119.7(3) . . ? C215 C216 H216 120.2 . . ? C211 C216 H216 120.2 . . ? C222 C221 C226 117.8(2) . . ? C222 C221 P2 121.29(16) . . ? C226 C221 P2 120.93(17) . . ? N223 C222 C221 121.1(2) . . ? N223 C222 H222 119.4 . . ? C221 C222 H222 119.4 . . ? C224 N223 C222 118.1(2) . . ? C225 C224 N223 123.8(2) . . ? C225 C224 H224 118.1 . . ? N223 C224 H224 118.1 . . ? C224 C225 C226 118.0(2) . . ? C224 C225 H225 121 . . ? C226 C225 H225 121 . . ? C225 C226 C221 121.2(2) . . ? C225 C226 H226 119.4 . . ? C221 C226 H226 119.4 . . ? #===END data_gk140 _database_code_depnum_ccdc_archive 'CCDC 640096' _audit_creation_date 2007-03-11T17:13:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C23 H22 Au2 Cl2 N4 P2' _chemical_formula_moiety 'C23 H22 Au2 Cl2 N4 P2' _chemical_formula_weight 881.22 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P_-1 _symmetry_space_group_name_Hall -p_1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.189(6) _cell_length_b 11.499(7) _cell_length_c 12.259(8) _cell_angle_alpha 95.62(4) _cell_angle_beta 103.85(3) _cell_angle_gamma 92.06(3) _cell_volume 1249.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5563 _cell_measurement_theta_min 1.8 _cell_measurement_theta_max 21.2 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 2.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.584 _exptl_crystal_description fragment _exptl_crystal_size_max .07 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .04 _exptl_crystal_size_rad ? _exptl_crystal_colour colourless _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .85 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.5594 _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents .033 _diffrn_reflns_av_unetI/netI 0.0264 _diffrn_reflns_number 38163 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 27.36 _diffrn_reflns_theta_full 24.5 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.838 _diffrn_radiation_type synchrotron _reflns_number_total 9718 _reflns_number_gt 9123 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction 'xtal ADDREF SORTRF' _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0336P)^2^+29.4588P] 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_number_reflns 9718 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1354 _refine_ls_wR_factor_gt 0.134 _refine_ls_goodness_of_fit_ref 1.198 _refine_ls_restrained_S_all 1.198 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 13.572 _refine_diff_density_min -4.78 _refine_diff_density_rms 0.403 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -0.7638 5.9978 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0998 0.0984 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.003 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.0667 0.058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1.01211(3) 0.32128(2) 0.48570(2) 0.01908(7) Uani 1 1 d . . . Au2 Au 0.47365(3) 0.34290(2) -0.00201(2) 0.01977(7) Uani 1 1 d . . . Cl1 Cl 1.2096(2) 0.41937(17) 0.61563(16) 0.0260(3) Uani 1 1 d . . . Cl2 Cl 0.2435(2) 0.35315(17) 0.0328(2) 0.0313(4) Uani 1 1 d . . . P1 P 0.8189(2) 0.22691(16) 0.36072(16) 0.0201(3) Uani 1 1 d . . . C111 C 0.6537(10) 0.2130(7) 0.4146(7) 0.0263(14) Uani 1 1 d . . . N112 N 0.6790(10) 0.1593(7) 0.5093(7) 0.0329(15) Uani 1 1 d . . . C113 C 0.5638(13) 0.1447(9) 0.5553(10) 0.040(2) Uani 1 1 d . . . H113 H 0.5793 0.1079 0.6228 0.048 Uiso 1 1 calc R . . C114 C 0.4217(13) 0.1807(10) 0.5094(11) 0.044(2) Uani 1 1 d . . . H114 H 0.3412 0.1671 0.5437 0.052 Uiso 1 1 calc R . . C115 C 0.4006(13) 0.2355(11) 0.4146(11) 0.046(3) Uani 1 1 d . . . H115 H 0.3043 0.2616 0.3826 0.056 Uiso 1 1 calc R . . C116 C 0.5176(10) 0.2541(9) 0.3632(8) 0.0335(18) Uani 1 1 d . . . H116 H 0.5047 0.2928 0.2969 0.04 Uiso 1 1 calc R . . C121 C 0.8469(9) 0.0752(7) 0.3175(6) 0.0222(12) Uani 1 1 d . . . N122 N 0.7311(9) 0.0222(7) 0.2375(8) 0.039(2) Uani 1 1 d . . . C123 C 0.7412(11) -0.0906(9) 0.2040(10) 0.039(2) Uani 1 1 d . . . H123 H 0.6608 -0.1295 0.147 0.046 Uiso 1 1 calc R . . C124 C 0.8623(11) -0.1532(7) 0.2480(8) 0.0311(17) Uani 1 1 d . . . H124 H 0.8631 -0.2341 0.2237 0.037 Uiso 1 1 calc R . . C125 C 0.9812(11) -0.0976(8) 0.3269(8) 0.0322(17) Uani 1 1 d . . . H125 H 1.0673 -0.1384 0.3568 0.039 Uiso 1 1 calc R . . C126 C 0.9734(10) 0.0206(7) 0.3626(6) 0.0255(14) Uani 1 1 d . . . H126 H 1.0544 0.0621 0.4172 0.031 Uiso 1 1 calc R . . C1 C 0.7635(9) 0.2911(7) 0.2295(6) 0.0230(13) Uani 1 1 d . . . H1A H 0.68 0.2417 0.1776 0.028 Uiso 1 1 calc R . . H1B H 0.7263 0.3694 0.2445 0.028 Uiso 1 1 calc R . . C2 C 0.8923(9) 0.3032(7) 0.1727(6) 0.0242(13) Uani 1 1 d . . . H2A H 0.9175 0.224 0.1463 0.029 Uiso 1 1 calc R . . H2B H 0.9816 0.34 0.2294 0.029 Uiso 1 1 calc R . . C3 C 0.8589(8) 0.3761(7) 0.0716(6) 0.0229(13) Uani 1 1 d . . . H3A H 0.9473 0.3784 0.0388 0.028 Uiso 1 1 calc R . . H3B H 0.8431 0.4574 0.099 0.028 Uiso 1 1 calc R . . P2 P 0.6952(2) 0.31873(16) -0.03803(15) 0.0176(3) Uani 1 1 d . . . C211 C 0.7154(9) 0.3777(6) -0.1657(6) 0.0223(13) Uani 1 1 d . . . N212 N 0.8531(8) 0.3851(6) -0.1803(6) 0.0250(12) Uani 1 1 d . . . C213 C 0.8696(10) 0.4238(8) -0.2754(8) 0.0300(16) Uani 1 1 d . . . H213 H 0.9678 0.4297 -0.2875 0.036 Uiso 1 1 calc R . . C214 C 0.7511(12) 0.4562(8) -0.3580(8) 0.0327(18) Uani 1 1 d . . . H214 H 0.7679 0.484 -0.4247 0.039 Uiso 1 1 calc R . . C215 C 0.6112(11) 0.4473(8) -0.3414(7) 0.0306(17) Uani 1 1 d . . . H215 H 0.5282 0.4684 -0.397 0.037 Uiso 1 1 calc R . . C216 C 0.5884(9) 0.4073(7) -0.2433(7) 0.0253(14) Uani 1 1 d . . . H216 H 0.4911 0.4004 -0.2296 0.03 Uiso 1 1 calc R . . C221 C 0.7271(9) 0.1650(7) -0.0678(7) 0.0240(13) Uani 1 1 d . . . N222 N 0.6181(9) 0.0900(7) -0.0638(10) 0.043(2) Uani 1 1 d . . . C223 C 0.6377(12) -0.0248(9) -0.0887(13) 0.050(3) Uani 1 1 d . . . H223 H 0.5594 -0.08 -0.0864 0.06 Uiso 1 1 calc R . . C224 C 0.7592(16) -0.0654(8) -0.1164(10) 0.045(3) Uani 1 1 d . . . H224 H 0.7654 -0.1468 -0.1359 0.054 Uiso 1 1 calc R . . C225 C 0.8769(16) 0.0142(9) -0.1160(11) 0.046(3) Uani 1 1 d . . . H225 H 0.9672 -0.0116 -0.1324 0.056 Uiso 1 1 calc R . . C226 C 0.8587(13) 0.1325(8) -0.0910(10) 0.039(2) Uani 1 1 d . . . H226 H 0.9365 0.1895 -0.0901 0.047 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 0.01989(12) 0.02016(11) 0.01502(10) 0.00221(8) 0.00008(8) 0.00042(8) Au2 0.01824(11) 0.01960(11) 0.02086(12) 0.00254(8) 0.00309(9) 0.00377(8) Cl1 0.0226(7) 0.0278(8) 0.0238(8) 0.0029(6) -0.0008(6) -0.0044(6) Cl2 0.0249(8) 0.0227(8) 0.0500(12) 0.0035(8) 0.0161(8) 0.0072(6) P1 0.0210(8) 0.0191(7) 0.0171(7) 0.0006(6) -0.0013(6) 0.0034(6) C111 0.028(4) 0.023(3) 0.024(3) -0.004(3) -0.001(3) 0.002(3) N112 0.033(4) 0.033(4) 0.032(4) 0.004(3) 0.007(3) -0.001(3) C113 0.043(5) 0.037(5) 0.043(5) 0.005(4) 0.019(4) 0.001(4) C114 0.037(5) 0.042(5) 0.055(6) -0.007(5) 0.023(5) -0.005(4) C115 0.031(5) 0.053(6) 0.051(6) -0.008(5) 0.006(4) 0.008(4) C116 0.026(4) 0.039(4) 0.033(4) -0.001(3) 0.004(3) 0.008(3) C121 0.023(3) 0.022(3) 0.020(3) 0.000(2) 0.002(2) 0.003(2) N122 0.031(4) 0.025(3) 0.047(5) -0.009(3) -0.012(3) 0.005(3) C123 0.029(4) 0.028(4) 0.050(6) -0.011(4) 0.000(4) 0.000(3) C124 0.039(4) 0.020(3) 0.036(4) 0.005(3) 0.010(4) 0.004(3) C125 0.040(5) 0.027(4) 0.029(4) 0.009(3) 0.003(3) 0.013(3) C126 0.028(3) 0.027(3) 0.018(3) 0.005(3) -0.001(3) 0.005(3) C1 0.027(3) 0.023(3) 0.016(3) 0.002(2) -0.001(2) 0.006(3) C2 0.025(3) 0.025(3) 0.020(3) 0.006(2) -0.001(2) 0.004(3) C3 0.017(3) 0.026(3) 0.022(3) 0.006(3) -0.002(2) -0.001(2) P2 0.0163(7) 0.0175(7) 0.0179(7) 0.0030(6) 0.0015(6) 0.0025(6) C211 0.027(3) 0.018(3) 0.019(3) 0.004(2) 0.002(2) -0.001(2) N212 0.025(3) 0.026(3) 0.024(3) 0.003(2) 0.006(2) 0.002(2) C213 0.031(4) 0.029(4) 0.032(4) 0.001(3) 0.012(3) -0.004(3) C214 0.044(5) 0.030(4) 0.027(4) 0.007(3) 0.013(3) -0.005(3) C215 0.034(4) 0.034(4) 0.021(3) 0.009(3) 0.000(3) -0.002(3) C216 0.024(3) 0.029(3) 0.022(3) 0.008(3) 0.002(3) -0.002(3) C221 0.028(3) 0.021(3) 0.022(3) 0.004(2) 0.004(3) 0.002(3) N222 0.025(3) 0.024(3) 0.079(7) 0.005(4) 0.010(4) -0.001(3) C223 0.030(4) 0.022(4) 0.090(10) -0.001(5) 0.004(5) -0.006(3) C224 0.070(8) 0.020(4) 0.041(5) 0.003(3) 0.005(5) 0.010(4) C225 0.067(8) 0.029(4) 0.057(7) 0.010(4) 0.037(6) 0.014(5) C226 0.044(5) 0.024(4) 0.055(6) 0.008(4) 0.025(5) 0.005(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 P1 2.216(2) . ? Au1 Cl1 2.285(2) . ? Au2 P2 2.205(2) . ? Au2 Cl2 2.260(2) . ? P1 C111 1.802(10) . ? P1 C1 1.806(7) . ? P1 C121 1.819(8) . ? C111 N112 1.344(12) . ? C111 C116 1.381(12) . ? N112 C113 1.326(13) . ? C113 C114 1.387(17) . ? C113 H113 0.95 . ? C114 C115 1.353(19) . ? C114 H114 0.95 . ? C115 C116 1.389(16) . ? C115 H115 0.95 . ? C116 H116 0.95 . ? C121 N122 1.343(10) . ? C121 C126 1.365(11) . ? N122 C123 1.334(12) . ? C123 C124 1.376(14) . ? C123 H123 0.95 . ? C124 C125 1.363(14) . ? C124 H124 0.95 . ? C125 C126 1.397(12) . ? C125 H125 0.95 . ? C126 H126 0.95 . ? C1 C2 1.519(12) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 C3 1.540(10) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 P2 1.814(7) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? P2 C211 1.811(8) . ? P2 C221 1.819(8) . ? C211 N212 1.321(11) . ? C211 C216 1.394(11) . ? N212 C213 1.327(11) . ? C213 C214 1.388(14) . ? C213 H213 0.95 . ? C214 C215 1.350(14) . ? C214 H214 0.95 . ? C215 C216 1.387(11) . ? C215 H215 0.95 . ? C216 H216 0.95 . ? C221 N222 1.311(11) . ? C221 C226 1.364(13) . ? N222 C223 1.354(13) . ? C223 C224 1.329(18) . ? C223 H223 0.95 . ? C224 C225 1.390(18) . ? C224 H224 0.95 . ? C225 C226 1.390(14) . ? C225 H225 0.95 . ? C226 H226 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 179.38(8) . . ? P2 Au2 Cl2 175.77(7) . . ? C111 P1 C1 106.9(4) . . ? C111 P1 C121 102.0(4) . . ? C1 P1 C121 104.3(4) . . ? C111 P1 Au1 113.0(3) . . ? C1 P1 Au1 114.6(3) . . ? C121 P1 Au1 114.9(3) . . ? N112 C111 C116 124.6(9) . . ? N112 C111 P1 112.4(6) . . ? C116 C111 P1 123.0(7) . . ? C113 N112 C111 116.9(9) . . ? N112 C113 C114 123.2(11) . . ? N112 C113 H113 118.4 . . ? C114 C113 H113 118.4 . . ? C115 C114 C113 118.4(10) . . ? C115 C114 H114 120.8 . . ? C113 C114 H114 120.8 . . ? C114 C115 C116 121.0(10) . . ? C114 C115 H115 119.5 . . ? C116 C115 H115 119.5 . . ? C111 C116 C115 116.0(10) . . ? C111 C116 H116 122 . . ? C115 C116 H116 122 . . ? N122 C121 C126 123.4(7) . . ? N122 C121 P1 113.5(6) . . ? C126 C121 P1 123.1(6) . . ? C123 N122 C121 117.0(8) . . ? N122 C123 C124 123.3(9) . . ? N122 C123 H123 118.4 . . ? C124 C123 H123 118.4 . . ? C125 C124 C123 119.2(8) . . ? C125 C124 H124 120.4 . . ? C123 C124 H124 120.4 . . ? C124 C125 C126 118.5(8) . . ? C124 C125 H125 120.8 . . ? C126 C125 H125 120.8 . . ? C121 C126 C125 118.5(8) . . ? C121 C126 H126 120.7 . . ? C125 C126 H126 120.7 . . ? C2 C1 P1 112.1(5) . . ? C2 C1 H1A 109.2 . . ? P1 C1 H1A 109.2 . . ? C2 C1 H1B 109.2 . . ? P1 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 C3 114.1(6) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C2 C3 P2 113.2(5) . . ? C2 C3 H3A 108.9 . . ? P2 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? P2 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? C211 P2 C3 105.9(4) . . ? C211 P2 C221 102.1(4) . . ? C3 P2 C221 104.6(4) . . ? C211 P2 Au2 113.7(3) . . ? C3 P2 Au2 117.1(3) . . ? C221 P2 Au2 112.0(3) . . ? N212 C211 C216 124.3(7) . . ? N212 C211 P2 116.0(6) . . ? C216 C211 P2 119.6(6) . . ? C211 N212 C213 117.0(7) . . ? N212 C213 C214 123.5(8) . . ? N212 C213 H213 118.2 . . ? C214 C213 H213 118.2 . . ? C215 C214 C213 118.4(8) . . ? C215 C214 H214 120.8 . . ? C213 C214 H214 120.8 . . ? C214 C215 C216 120.2(8) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C215 C216 C211 116.6(8) . . ? C215 C216 H216 121.7 . . ? C211 C216 H216 121.7 . . ? N222 C221 C226 123.4(8) . . ? N222 C221 P2 116.0(7) . . ? C226 C221 P2 120.6(7) . . ? C221 N222 C223 117.0(9) . . ? C224 C223 N222 124.4(10) . . ? C224 C223 H223 117.8 . . ? N222 C223 H223 117.8 . . ? C223 C224 C225 118.3(9) . . ? C223 C224 H224 120.8 . . ? C225 C224 H224 120.8 . . ? C226 C225 C224 118.1(11) . . ? C226 C225 H225 120.9 . . ? C224 C225 H225 120.9 . . ? C221 C226 C225 118.7(10) . . ? C221 C226 H226 120.7 . . ? C225 C226 H226 120.7 . . ?