Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Andrew M. Brodie' _publ_contact_author_address ; Chemistry Massey University Inst Fundamental Sciences Private Bag 11 222 Palmerston North NEW ZEALAND ; _publ_contact_author_email A.BRODIE@MASSEY.AC.NZ _publ_section_title ; A new diphosphine ligand based on the cyclotriphosphazene platform ; loop_ _publ_author_name 'Andrew M. Brodie' 'Eric W. Ainscough' 'Adrian B. Chaplin' J.M.O'Connor 'Carl A. Otter' data_cao159 _database_code_depnum_ccdc_archive 'CCDC 287631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H56 Cl2 N7 O6 P5 Pt' _chemical_formula_weight 1488.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5768(2) _cell_length_b 11.1807(2) _cell_length_c 42.2143(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.8110(10) _cell_angle_gamma 90.00 _cell_volume 6348.60(15) _cell_formula_units_Z 4 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 2.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712611 _exptl_absorpt_correction_T_max 0.928673 _exptl_absorpt_process_details 'Blessing, Acta Cryst., A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Brucker P4' _diffrn_measurement_method 'Area detector / w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28324 _diffrn_reflns_av_R_equivalents 0.1263 _diffrn_reflns_av_sigmaI/netI 0.1445 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 23.26 _reflns_number_total 9094 _reflns_number_gt 5816 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.1403P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9094 _refine_ls_number_parameters 806 _refine_ls_number_restraints 486 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.09326(3) 0.10924(4) 0.916674(10) 0.01345(14) Uani 1 1 d . . . P4 P 0.2188(2) 0.1338(2) 0.95718(6) 0.0113(7) Uani 1 1 d . . . P5 P 0.0287(2) 0.2964(2) 0.91361(7) 0.0138(7) Uani 1 1 d . . . Cl1 Cl 0.1365(2) -0.0924(2) 0.91442(6) 0.0191(7) Uani 1 1 d . . . Cl2 Cl -0.0341(2) 0.0724(2) 0.87397(6) 0.0184(7) Uani 1 1 d . . . P1 P 0.2763(2) 0.2314(2) 0.86735(7) 0.0134(7) Uani 1 1 d . . . P2 P 0.2890(2) 0.0526(2) 0.82415(7) 0.0125(7) Uani 1 1 d . . . P3 P 0.3775(2) 0.2677(2) 0.81584(7) 0.0136(7) Uani 1 1 d . . . N3 N 0.3479(6) 0.3077(7) 0.84884(19) 0.012(2) Uani 1 1 d U . . N1 N 0.2328(6) 0.1099(8) 0.85104(19) 0.015(2) Uani 1 1 d U . . N2 N 0.3444(7) 0.1376(7) 0.80255(19) 0.017(2) Uani 1 1 d U . . O1 O 0.3246(5) 0.2004(6) 0.90258(15) 0.0129(17) Uani 1 1 d U . . O2 O 0.1895(5) 0.3146(6) 0.87663(16) 0.0161(18) Uani 1 1 d U . . O3 O 0.3687(5) -0.0422(6) 0.83874(15) 0.0131(17) Uani 1 1 d U . . O4 O 0.2087(5) -0.0276(6) 0.80288(15) 0.0126(17) Uani 1 1 d U . . O5 O 0.4938(5) 0.2746(6) 0.81487(16) 0.0133(17) Uani 1 1 d U . . O6 O 0.3353(5) 0.3712(6) 0.79107(15) 0.0136(17) Uani 1 1 d U . . C1 C 0.3426(8) 0.2846(9) 0.9278(2) 0.014(3) Uani 1 1 d U . . C2 C 0.4085(7) 0.3796(9) 0.9251(2) 0.014(2) Uani 1 1 d U . . H2 H 0.4391 0.3895 0.9069 0.017 Uiso 1 1 calc R . . C3 C 0.4261(9) 0.4575(10) 0.9504(3) 0.022(3) Uani 1 1 d U . . H3 H 0.4693 0.5213 0.9492 0.027 Uiso 1 1 calc R . . C4 C 0.3815(8) 0.4434(9) 0.9775(3) 0.017(3) Uani 1 1 d U . . H4 H 0.3950 0.4973 0.9944 0.020 Uiso 1 1 calc R . . C5 C 0.3163(8) 0.3487(9) 0.9799(3) 0.017(3) Uani 1 1 d U . . H5 H 0.2850 0.3401 0.9981 0.020 Uiso 1 1 calc R . . C6 C 0.2982(8) 0.2664(9) 0.9548(2) 0.011(2) Uani 1 1 d U . . C7 C 0.3136(8) 0.0155(9) 0.9640(2) 0.014(3) Uani 1 1 d U . . C8 C 0.4084(8) 0.0251(10) 0.9547(2) 0.018(3) Uani 1 1 d U . . H8 H 0.4251 0.0935 0.9440 0.022 Uiso 1 1 calc R . . C9 C 0.4765(9) -0.0645(10) 0.9610(3) 0.025(3) Uani 1 1 d U . . H9 H 0.5392 -0.0551 0.9548 0.030 Uiso 1 1 calc R . . C10 C 0.4554(8) -0.1687(9) 0.9762(2) 0.014(3) Uani 1 1 d U . . H10 H 0.5020 -0.2298 0.9800 0.017 Uiso 1 1 calc R . . C11 C 0.3628(8) -0.1787(10) 0.9857(3) 0.020(3) Uani 1 1 d U . . H11 H 0.3474 -0.2477 0.9963 0.024 Uiso 1 1 calc R . . C12 C 0.2925(9) -0.0915(10) 0.9800(2) 0.022(3) Uani 1 1 d U . . H12 H 0.2306 -0.1019 0.9867 0.026 Uiso 1 1 calc R . . C13 C 0.1738(8) 0.1379(8) 0.9961(2) 0.011(3) Uani 1 1 d U . . C14 C 0.2394(9) 0.1407(9) 1.0249(2) 0.019(3) Uani 1 1 d U . . H14 H 0.3076 0.1424 1.0244 0.022 Uiso 1 1 calc R . . C15 C 0.2036(9) 0.1410(9) 1.0536(3) 0.023(3) Uani 1 1 d U . . H15 H 0.2479 0.1440 1.0724 0.028 Uiso 1 1 calc R . . C16 C 0.1021(8) 0.1368(9) 1.0550(3) 0.021(3) Uani 1 1 d U . . H16 H 0.0788 0.1374 1.0748 0.025 Uiso 1 1 calc R . . C17 C 0.0357(9) 0.1319(9) 1.0271(2) 0.020(3) Uani 1 1 d U . . H17 H -0.0325 0.1292 1.0277 0.024 Uiso 1 1 calc R . . C18 C 0.0733(8) 0.1310(9) 0.9983(2) 0.016(3) Uani 1 1 d U . . H18 H 0.0289 0.1255 0.9795 0.019 Uiso 1 1 calc R . . C19 C 0.1046(8) 0.3548(8) 0.8577(2) 0.013(3) Uani 1 1 d U . . C20 C 0.1069(8) 0.3981(10) 0.8270(2) 0.020(3) Uani 1 1 d U . . H20 H 0.1649 0.3950 0.8176 0.024 Uiso 1 1 calc R . . C21 C 0.0198(9) 0.4464(10) 0.8109(3) 0.024(3) Uani 1 1 d U . . H21 H 0.0187 0.4761 0.7902 0.029 Uiso 1 1 calc R . . C22 C -0.0648(8) 0.4498(9) 0.8256(3) 0.018(3) Uani 1 1 d U . . H22 H -0.1226 0.4829 0.8147 0.021 Uiso 1 1 calc R . . C23 C -0.0659(8) 0.4060(9) 0.8555(2) 0.021(3) Uani 1 1 d U . . H23 H -0.1244 0.4095 0.8646 0.025 Uiso 1 1 calc R . . C24 C 0.0190(8) 0.3558(8) 0.8729(2) 0.011(2) Uani 1 1 d U . . C25 C 0.0832(8) 0.4190(8) 0.9383(2) 0.013(3) Uani 1 1 d U . . C26 C 0.1264(8) 0.5207(9) 0.9261(3) 0.017(3) Uani 1 1 d U . . H26 H 0.1316 0.5255 0.9044 0.020 Uiso 1 1 calc R . . C27 C 0.1608(8) 0.6126(10) 0.9460(2) 0.018(3) Uani 1 1 d U . . H27 H 0.1889 0.6795 0.9377 0.022 Uiso 1 1 calc R . . C28 C 0.1543(8) 0.6070(10) 0.9781(2) 0.021(3) Uani 1 1 d U . . H28 H 0.1781 0.6701 0.9914 0.025 Uiso 1 1 calc R . . C29 C 0.1130(8) 0.5090(9) 0.9910(3) 0.019(3) Uani 1 1 d U . . H29 H 0.1087 0.5050 1.0128 0.023 Uiso 1 1 calc R . . C30 C 0.0783(8) 0.4168(9) 0.9708(2) 0.016(3) Uani 1 1 d U . . H30 H 0.0503 0.3504 0.9794 0.020 Uiso 1 1 calc R . . C31 C -0.0973(8) 0.3020(9) 0.9236(2) 0.015(3) Uani 1 1 d U . . C32 C -0.1486(8) 0.4101(10) 0.9246(2) 0.018(3) Uani 1 1 d U . . H32 H -0.1166 0.4809 0.9206 0.022 Uiso 1 1 calc R . . C33 C -0.2447(8) 0.4149(10) 0.9313(2) 0.022(3) Uani 1 1 d U . . H33 H -0.2780 0.4878 0.9308 0.027 Uiso 1 1 calc R . . C34 C -0.2927(9) 0.3098(10) 0.9389(3) 0.023(3) Uani 1 1 d U . . H34 H -0.3579 0.3126 0.9433 0.028 Uiso 1 1 calc R . . C35 C -0.2425(9) 0.2022(10) 0.9398(2) 0.022(3) Uani 1 1 d U . . H35 H -0.2729 0.1327 0.9457 0.026 Uiso 1 1 calc R . . C36 C -0.1470(8) 0.1978(10) 0.9318(2) 0.018(3) Uani 1 1 d U . . H36 H -0.1147 0.1244 0.9319 0.021 Uiso 1 1 calc R . . C37 C 0.3411(8) -0.1536(9) 0.8514(2) 0.014(3) Uani 1 1 d U . . C38 C 0.3572(8) -0.1703(10) 0.8837(2) 0.018(3) Uani 1 1 d U . . H38 H 0.3780 -0.1070 0.8973 0.022 Uiso 1 1 calc R . . C39 C 0.3420(8) -0.2834(9) 0.8962(3) 0.022(3) Uani 1 1 d U . . H39 H 0.3530 -0.2974 0.9181 0.026 Uiso 1 1 calc R . . C40 C 0.3099(8) -0.3746(10) 0.8747(3) 0.023(3) Uani 1 1 d U . . H40 H 0.3008 -0.4510 0.8825 0.027 Uiso 1 1 calc R . . C41 C 0.2915(8) -0.3550(9) 0.8428(3) 0.020(3) Uani 1 1 d U . . H41 H 0.2687 -0.4179 0.8294 0.024 Uiso 1 1 calc R . . C42 C 0.3062(8) -0.2408(9) 0.8292(2) 0.013(3) Uani 1 1 d U . . C43 C 0.2871(8) -0.2198(9) 0.7953(2) 0.014(3) Uani 1 1 d U . . C44 C 0.3139(8) -0.3020(10) 0.7727(2) 0.020(3) Uani 1 1 d U . . H44 H 0.3425 -0.3743 0.7799 0.024 Uiso 1 1 calc R . . C45 C 0.2997(8) -0.2799(10) 0.7409(3) 0.021(3) Uani 1 1 d U . . H45 H 0.3213 -0.3356 0.7270 0.025 Uiso 1 1 calc R . . C46 C 0.2540(8) -0.1764(9) 0.7287(3) 0.017(3) Uani 1 1 d U . . H46 H 0.2431 -0.1636 0.7067 0.020 Uiso 1 1 calc R . . C47 C 0.2243(8) -0.0909(10) 0.7496(2) 0.018(3) Uani 1 1 d U . . H47 H 0.1934 -0.0203 0.7420 0.022 Uiso 1 1 calc R . . C48 C 0.2423(8) -0.1150(10) 0.7816(2) 0.021(3) Uani 1 1 d U . . C49 C 0.5452(8) 0.3852(10) 0.8164(2) 0.016(2) Uani 1 1 d U . . C50 C 0.6085(8) 0.4124(9) 0.8434(3) 0.022(3) Uani 1 1 d U . . H50 H 0.6110 0.3645 0.8615 0.027 Uiso 1 1 calc R . . C51 C 0.6691(9) 0.5127(9) 0.8434(3) 0.022(3) Uani 1 1 d U . . H51 H 0.7141 0.5307 0.8614 0.026 Uiso 1 1 calc R . . C52 C 0.6629(9) 0.5846(10) 0.8172(3) 0.027(3) Uani 1 1 d U . . H52 H 0.7043 0.6509 0.8171 0.033 Uiso 1 1 calc R . . C53 C 0.5940(8) 0.5583(10) 0.7903(3) 0.021(3) Uani 1 1 d U . . H53 H 0.5885 0.6095 0.7728 0.025 Uiso 1 1 calc R . . C54 C 0.5334(8) 0.4572(9) 0.7891(2) 0.015(3) Uani 1 1 d U . . C55 C 0.4648(8) 0.4285(9) 0.7601(3) 0.018(3) Uani 1 1 d U . . C56 C 0.4903(9) 0.4508(9) 0.7298(2) 0.019(3) Uani 1 1 d U . . H56 H 0.5532 0.4808 0.7280 0.023 Uiso 1 1 calc R . . C57 C 0.4248(9) 0.4295(10) 0.7024(3) 0.026(3) Uani 1 1 d U . . H57 H 0.4444 0.4438 0.6825 0.031 Uiso 1 1 calc R . . C58 C 0.3284(8) 0.3861(10) 0.7045(2) 0.020(3) Uani 1 1 d U . . H58 H 0.2834 0.3732 0.6862 0.024 Uiso 1 1 calc R . . C59 C 0.3023(9) 0.3634(9) 0.7343(3) 0.021(3) Uani 1 1 d U . . H59 H 0.2395 0.3336 0.7363 0.025 Uiso 1 1 calc R . . C60 C 0.3683(8) 0.3843(10) 0.7610(2) 0.016(2) Uani 1 1 d U . . C90 C 0.4088(10) 0.2271(11) 0.1238(3) 0.040(4) Uani 1 1 d U . . H90A H 0.4244 0.1449 0.1202 0.060 Uiso 1 1 calc R . . H90B H 0.3453 0.2318 0.1314 0.060 Uiso 1 1 calc R . . H90C H 0.4589 0.2606 0.1396 0.060 Uiso 1 1 calc R . . C91 C 0.4055(9) 0.2928(11) 0.0945(3) 0.030(3) Uani 1 1 d U . . N90 N 0.4025(8) 0.3409(9) 0.0705(2) 0.032(3) Uani 1 1 d U . . C93 C 1.0205(9) 0.7745(11) 0.8420(3) 0.037(3) Uani 1 1 d U . . H93A H 1.0132 0.7605 0.8193 0.055 Uiso 1 1 calc R . . H93B H 1.0676 0.7188 0.8526 0.055 Uiso 1 1 calc R . . H93C H 1.0437 0.8546 0.8464 0.055 Uiso 1 1 calc R . . C94 C 0.9254(10) 0.7586(11) 0.8533(3) 0.033(3) Uani 1 1 d U . . N91 N 0.8487(9) 0.7492(10) 0.8609(3) 0.049(3) Uani 1 1 d U . . C95 C -0.0145(10) 0.1174(12) 0.7914(3) 0.045(4) Uani 1 1 d U . . H95A H 0.0355 0.1112 0.8097 0.067 Uiso 1 1 calc R . . H95B H -0.0399 0.0392 0.7855 0.067 Uiso 1 1 calc R . . H95C H -0.0677 0.1674 0.7965 0.067 Uiso 1 1 calc R . . C96 C 0.0291(10) 0.1696(12) 0.7647(3) 0.039(4) Uani 1 1 d U . . N93 N 0.0654(9) 0.2094(10) 0.7441(3) 0.054(3) Uani 1 1 d U . . C97 C 0.7054(10) 0.1214(12) 0.8579(3) 0.048(4) Uani 1 1 d U . . H97A H 0.7396 0.1931 0.8655 0.072 Uiso 1 1 calc R . . H97B H 0.6811 0.1297 0.8356 0.072 Uiso 1 1 calc R . . H97C H 0.7503 0.0548 0.8610 0.072 Uiso 1 1 calc R . . C98 C 0.6218(11) 0.1010(13) 0.8757(3) 0.044(4) Uani 1 1 d U . . N94 N 0.5565(9) 0.0866(10) 0.8906(3) 0.054(3) Uani 1 1 d U . . 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 Pt1 0.0168(2) 0.0063(2) 0.0177(2) 0.0005(2) 0.00412(18) 0.0008(2) P4 0.0133(16) 0.0059(16) 0.0151(15) 0.0004(12) 0.0033(13) -0.0008(12) P5 0.0132(17) 0.0106(16) 0.0179(16) -0.0003(13) 0.0032(14) 0.0031(13) Cl1 0.0238(16) 0.0079(15) 0.0261(15) -0.0004(12) 0.0054(13) 0.0014(12) Cl2 0.0205(17) 0.0134(15) 0.0204(15) -0.0028(12) -0.0001(13) 0.0003(12) P1 0.0154(17) 0.0087(16) 0.0174(16) -0.0002(12) 0.0068(14) -0.0007(13) P2 0.0149(18) 0.0064(15) 0.0166(16) -0.0017(12) 0.0039(14) -0.0019(13) P3 0.0178(18) 0.0050(15) 0.0185(16) 0.0022(12) 0.0044(14) 0.0008(13) N3 0.014(4) 0.009(4) 0.013(4) 0.002(3) 0.005(3) -0.002(3) N1 0.015(4) 0.010(4) 0.019(4) -0.002(3) 0.002(3) -0.005(3) N2 0.021(4) 0.015(4) 0.017(4) -0.003(3) 0.005(3) 0.002(3) O1 0.016(3) 0.009(3) 0.014(3) -0.002(3) 0.001(3) -0.005(3) O2 0.019(4) 0.011(3) 0.017(3) -0.001(3) 0.000(3) 0.004(3) O3 0.013(3) 0.013(3) 0.014(3) 0.001(3) 0.002(3) -0.002(3) O4 0.013(3) 0.012(3) 0.013(3) 0.000(3) 0.005(3) 0.002(3) O5 0.018(3) 0.003(3) 0.019(3) 0.005(3) 0.004(3) 0.003(3) O6 0.017(3) 0.013(3) 0.010(3) 0.006(3) 0.002(3) 0.004(3) C1 0.014(4) 0.012(4) 0.014(4) -0.004(4) -0.003(4) -0.001(4) C2 0.015(4) 0.014(4) 0.013(4) 0.001(4) 0.003(4) 0.001(4) C3 0.025(5) 0.018(4) 0.023(5) 0.003(4) 0.001(4) -0.003(4) C4 0.019(5) 0.011(4) 0.020(4) 0.001(4) 0.001(4) 0.000(4) C5 0.016(4) 0.018(4) 0.016(4) 0.000(4) 0.002(4) 0.007(4) C6 0.011(4) 0.009(4) 0.014(4) 0.003(3) 0.002(4) 0.006(4) C7 0.018(5) 0.010(4) 0.017(4) 0.002(4) 0.004(4) 0.001(4) C8 0.018(5) 0.018(4) 0.019(4) 0.001(4) 0.001(4) 0.003(4) C9 0.023(5) 0.025(5) 0.028(5) -0.002(4) 0.006(4) 0.005(4) C10 0.013(4) 0.015(4) 0.014(4) 0.003(4) -0.002(4) 0.005(4) C11 0.022(5) 0.016(4) 0.022(4) 0.001(4) 0.001(4) 0.001(4) C12 0.021(5) 0.023(5) 0.022(4) 0.000(4) 0.002(4) -0.001(4) C13 0.014(4) 0.005(4) 0.015(4) -0.001(3) 0.004(4) -0.003(3) C14 0.019(5) 0.017(5) 0.019(4) 0.003(4) 0.001(4) -0.001(4) C15 0.026(5) 0.025(5) 0.018(4) 0.001(4) 0.003(4) -0.003(4) C16 0.025(5) 0.019(5) 0.020(4) 0.002(4) 0.007(4) -0.002(4) C17 0.022(5) 0.018(5) 0.023(4) -0.001(4) 0.009(4) -0.001(4) C18 0.019(4) 0.012(4) 0.017(4) 0.002(4) 0.003(4) -0.003(4) C19 0.017(4) 0.008(4) 0.014(4) 0.000(3) -0.002(4) -0.003(3) C20 0.017(4) 0.020(4) 0.023(4) -0.003(4) 0.003(4) 0.003(4) C21 0.028(5) 0.021(4) 0.024(5) 0.004(4) 0.004(4) 0.000(4) C22 0.017(5) 0.014(4) 0.022(4) -0.004(4) 0.002(4) -0.001(4) C23 0.020(4) 0.018(4) 0.024(4) -0.004(4) 0.003(4) -0.003(4) C24 0.014(4) 0.006(4) 0.012(4) -0.004(3) 0.001(4) 0.001(3) C25 0.016(4) 0.005(4) 0.019(4) 0.000(3) 0.001(4) 0.000(3) C26 0.017(5) 0.021(4) 0.014(4) -0.002(4) 0.004(4) 0.003(4) C27 0.017(4) 0.015(4) 0.022(4) 0.001(4) 0.005(4) -0.004(4) C28 0.020(4) 0.018(4) 0.025(4) -0.006(4) 0.000(4) -0.004(4) C29 0.017(5) 0.020(4) 0.021(4) 0.000(4) 0.006(4) 0.005(4) C30 0.013(4) 0.016(5) 0.020(4) 0.003(4) 0.000(4) 0.002(4) C31 0.015(4) 0.017(4) 0.012(4) 0.001(4) -0.001(4) 0.004(4) C32 0.017(4) 0.017(5) 0.021(4) 0.001(4) 0.003(4) 0.003(4) C33 0.022(5) 0.023(5) 0.021(4) 0.000(4) -0.001(4) 0.008(4) C34 0.016(5) 0.031(5) 0.023(4) -0.003(4) 0.002(4) 0.002(4) C35 0.021(5) 0.023(5) 0.020(4) 0.004(4) 0.001(4) -0.004(4) C36 0.017(5) 0.021(4) 0.015(4) 0.000(4) 0.000(4) -0.003(4) C37 0.013(4) 0.013(4) 0.016(4) 0.002(3) 0.006(4) 0.004(4) C38 0.019(5) 0.019(4) 0.017(4) 0.003(4) 0.002(4) 0.001(4) C39 0.021(5) 0.022(5) 0.023(4) 0.001(4) 0.005(4) 0.006(4) C40 0.026(5) 0.017(4) 0.027(4) 0.000(4) 0.007(4) -0.001(4) C41 0.018(5) 0.020(5) 0.021(4) -0.004(4) 0.003(4) 0.000(4) C42 0.010(4) 0.016(4) 0.015(4) -0.005(4) 0.004(4) 0.004(4) C43 0.016(4) 0.007(4) 0.018(4) 0.002(3) 0.000(4) 0.002(4) C44 0.022(5) 0.019(4) 0.019(4) -0.003(4) 0.003(4) 0.002(4) C45 0.020(5) 0.019(4) 0.023(4) -0.004(4) 0.003(4) 0.000(4) C46 0.021(5) 0.014(4) 0.016(4) 0.001(4) 0.004(4) -0.001(4) C47 0.020(4) 0.017(4) 0.018(4) 0.003(4) 0.003(4) 0.001(4) C48 0.022(4) 0.020(4) 0.021(4) -0.007(4) 0.005(4) -0.001(4) C49 0.016(4) 0.012(4) 0.022(4) -0.004(4) 0.006(4) 0.001(4) C50 0.025(5) 0.020(5) 0.022(4) 0.003(4) 0.005(4) 0.001(4) C51 0.020(5) 0.020(4) 0.025(5) -0.002(4) 0.004(4) -0.006(4) C52 0.025(5) 0.026(5) 0.031(5) -0.002(4) 0.004(4) -0.003(4) C53 0.022(5) 0.018(4) 0.022(4) 0.004(4) 0.005(4) 0.000(4) C54 0.014(4) 0.013(4) 0.017(4) -0.001(4) 0.005(4) 0.004(4) C55 0.020(5) 0.015(4) 0.020(4) -0.001(4) 0.006(4) -0.002(4) C56 0.021(5) 0.017(4) 0.021(4) 0.001(4) 0.010(4) 0.001(4) C57 0.033(5) 0.024(5) 0.022(5) 0.003(4) 0.007(4) 0.003(4) C58 0.026(4) 0.018(4) 0.015(4) -0.001(4) 0.002(4) 0.000(4) C59 0.023(5) 0.015(5) 0.026(4) -0.004(4) 0.007(4) 0.001(4) C60 0.020(4) 0.014(4) 0.016(4) -0.003(4) 0.007(4) 0.001(4) C90 0.041(5) 0.040(5) 0.040(5) 0.000(4) 0.008(4) 0.005(4) C91 0.028(5) 0.030(5) 0.033(5) -0.004(4) 0.004(4) -0.001(4) N90 0.031(5) 0.028(4) 0.038(4) 0.000(4) 0.010(4) 0.002(4) C93 0.035(5) 0.034(5) 0.040(5) -0.008(4) 0.001(4) 0.005(4) C94 0.032(5) 0.033(5) 0.032(5) -0.007(4) 0.000(4) 0.000(4) N91 0.047(5) 0.048(5) 0.053(5) -0.009(4) 0.005(4) -0.004(4) C95 0.045(5) 0.043(5) 0.047(5) 0.002(4) 0.008(4) 0.000(4) C96 0.041(5) 0.039(5) 0.037(5) -0.001(4) 0.004(4) -0.002(4) N93 0.053(5) 0.057(5) 0.051(5) -0.001(4) 0.008(4) -0.010(4) C97 0.047(5) 0.047(5) 0.050(5) -0.004(4) 0.005(4) 0.000(4) C98 0.045(5) 0.043(5) 0.044(5) -0.003(4) 0.007(4) 0.001(4) N94 0.054(5) 0.055(5) 0.055(5) -0.004(4) 0.007(4) -0.007(4) _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 Pt1 P4 2.261(3) . ? Pt1 P5 2.266(3) . ? Pt1 Cl1 2.334(3) . ? Pt1 Cl2 2.358(3) . ? P4 C13 1.830(10) . ? P4 C7 1.840(11) . ? P4 C6 1.844(11) . ? P5 C25 1.818(10) . ? P5 C31 1.818(11) . ? P5 C24 1.832(10) . ? P1 N3 1.578(8) . ? P1 O1 1.580(7) . ? P1 O2 1.592(7) . ? P1 N1 1.600(9) . ? P2 N2 1.577(9) . ? P2 O3 1.579(7) . ? P2 N1 1.586(8) . ? P2 O4 1.591(7) . ? P3 N3 1.567(8) . ? P3 O5 1.586(7) . ? P3 N2 1.602(9) . ? P3 O6 1.612(7) . ? O1 C1 1.417(11) . ? O2 C19 1.385(12) . ? O3 C37 1.425(11) . ? O4 C48 1.443(12) . ? O5 C49 1.418(12) . ? O6 C60 1.408(11) . ? C1 C6 1.375(13) . ? C1 C2 1.403(14) . ? C2 C3 1.374(14) . ? C2 H2 0.9300 . ? C3 C4 1.375(14) . ? C3 H3 0.9300 . ? C4 C5 1.393(14) . ? C4 H4 0.9300 . ? C5 C6 1.400(14) . ? C5 H5 0.9300 . ? C7 C8 1.400(14) . ? C7 C12 1.423(14) . ? C8 C9 1.366(14) . ? C8 H8 0.9300 . ? C9 C10 1.380(14) . ? C9 H9 0.9300 . ? C10 C11 1.374(14) . ? C10 H10 0.9300 . ? C11 C12 1.362(15) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.382(14) . ? C13 C14 1.407(14) . ? C14 C15 1.362(14) . ? C14 H14 0.9300 . ? C15 C16 1.388(15) . ? C15 H15 0.9300 . ? C16 C17 1.385(15) . ? C16 H16 0.9300 . ? C17 C18 1.383(13) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.386(14) . ? C19 C24 1.402(14) . ? C20 C21 1.392(15) . ? C20 H20 0.9300 . ? C21 C22 1.380(14) . ? C21 H21 0.9300 . ? C22 C23 1.356(14) . ? C22 H22 0.9300 . ? C23 C24 1.396(14) . ? C23 H23 0.9300 . ? C25 C30 1.384(13) . ? C25 C26 1.409(14) . ? C26 C27 1.369(14) . ? C26 H26 0.9300 . ? C27 C28 1.372(13) . ? C27 H27 0.9300 . ? C28 C29 1.375(14) . ? C28 H28 0.9300 . ? C29 C30 1.379(14) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.398(14) . ? C31 C36 1.413(14) . ? C32 C33 1.374(14) . ? C32 H32 0.9300 . ? C33 C34 1.402(15) . ? C33 H33 0.9300 . ? C34 C35 1.381(15) . ? C34 H34 0.9300 . ? C35 C36 1.383(14) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.364(14) . ? C37 C42 1.390(14) . ? C38 C39 1.396(14) . ? C38 H38 0.9300 . ? C39 C40 1.395(15) . ? C39 H39 0.9300 . ? C40 C41 1.353(14) . ? C40 H40 0.9300 . ? C41 C42 1.424(14) . ? C41 H41 0.9300 . ? C42 C43 1.441(14) . ? C43 C48 1.407(14) . ? C43 C44 1.407(13) . ? C44 C45 1.351(14) . ? C44 H44 0.9300 . ? C45 C46 1.380(14) . ? C45 H45 0.9300 . ? C46 C47 1.397(14) . ? C46 H46 0.9300 . ? C47 C48 1.367(14) . ? C47 H47 0.9300 . ? C49 C50 1.365(14) . ? C49 C54 1.396(14) . ? C50 C51 1.392(14) . ? C50 H50 0.9300 . ? C51 C52 1.362(14) . ? C51 H51 0.9300 . ? C52 C53 1.401(15) . ? C52 H52 0.9300 . ? C53 C54 1.395(14) . ? C53 H53 0.9300 . ? C54 C55 1.471(15) . ? C55 C56 1.392(14) . ? C55 C60 1.405(15) . ? C56 C57 1.380(15) . ? C56 H56 0.9300 . ? C57 C58 1.411(15) . ? C57 H57 0.9300 . ? C58 C59 1.377(14) . ? C58 H58 0.9300 . ? C59 C60 1.362(14) . ? C59 H59 0.9300 . ? C90 C91 1.435(16) . ? C90 H90A 0.9600 . ? C90 H90B 0.9600 . ? C90 H90C 0.9600 . ? C91 N90 1.142(13) . ? C93 C94 1.447(17) . ? C93 H93A 0.9600 . ? C93 H93B 0.9600 . ? C93 H93C 0.9600 . ? C94 N91 1.136(15) . ? C95 C96 1.462(17) . ? C95 H95A 0.9600 . ? C95 H95B 0.9600 . ? C95 H95C 0.9600 . ? C96 N93 1.149(14) . ? C97 C98 1.461(17) . ? C97 H97A 0.9600 . ? C97 H97B 0.9600 . ? C97 H97C 0.9600 . ? C98 N94 1.166(15) . ? 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 P4 Pt1 P5 100.21(10) . . ? P4 Pt1 Cl1 88.87(10) . . ? P5 Pt1 Cl1 170.72(11) . . ? P4 Pt1 Cl2 176.67(10) . . ? P5 Pt1 Cl2 83.09(10) . . ? Cl1 Pt1 Cl2 87.85(9) . . ? C13 P4 C7 100.9(5) . . ? C13 P4 C6 107.3(4) . . ? C7 P4 C6 100.7(5) . . ? C13 P4 Pt1 111.9(4) . . ? C7 P4 Pt1 118.0(4) . . ? C6 P4 Pt1 116.2(3) . . ? C25 P5 C31 99.4(5) . . ? C25 P5 C24 103.6(4) . . ? C31 P5 C24 104.8(5) . . ? C25 P5 Pt1 122.7(4) . . ? C31 P5 Pt1 112.8(4) . . ? C24 P5 Pt1 111.5(3) . . ? N3 P1 O1 112.3(4) . . ? N3 P1 O2 109.4(4) . . ? O1 P1 O2 97.1(4) . . ? N3 P1 N1 117.5(4) . . ? O1 P1 N1 107.5(4) . . ? O2 P1 N1 111.1(4) . . ? N2 P2 O3 105.9(4) . . ? N2 P2 N1 119.0(5) . . ? O3 P2 N1 111.3(4) . . ? N2 P2 O4 110.9(4) . . ? O3 P2 O4 102.9(4) . . ? N1 P2 O4 105.8(4) . . ? N3 P3 O5 112.7(5) . . ? N3 P3 N2 118.5(4) . . ? O5 P3 N2 105.5(4) . . ? N3 P3 O6 105.1(4) . . ? O5 P3 O6 102.5(4) . . ? N2 P3 O6 111.5(4) . . ? P3 N3 P1 122.4(5) . . ? P2 N1 P1 117.8(5) . . ? P2 N2 P3 118.6(5) . . ? C1 O1 P1 124.6(6) . . ? C19 O2 P1 129.3(6) . . ? C37 O3 P2 122.1(6) . . ? C48 O4 P2 118.8(6) . . ? C49 O5 P3 121.7(6) . . ? C60 O6 P3 122.0(6) . . ? C6 C1 C2 122.3(10) . . ? C6 C1 O1 118.3(9) . . ? C2 C1 O1 119.3(9) . . ? C3 C2 C1 117.5(10) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 121.7(11) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C3 C4 C5 120.2(10) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 119.5(10) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 118.6(10) . . ? C1 C6 P4 119.3(8) . . ? C5 C6 P4 122.0(8) . . ? C8 C7 C12 116.8(10) . . ? C8 C7 P4 123.4(8) . . ? C12 C7 P4 119.8(8) . . ? C9 C8 C7 120.9(11) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 122.1(11) . . ? C8 C9 H9 118.9 . . ? C10 C9 H9 118.9 . . ? C11 C10 C9 117.4(11) . . ? C11 C10 H10 121.3 . . ? C9 C10 H10 121.3 . . ? C12 C11 C10 122.6(11) . . ? C12 C11 H11 118.7 . . ? C10 C11 H11 118.7 . . ? C11 C12 C7 120.2(11) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C18 C13 C14 117.3(9) . . ? C18 C13 P4 120.7(8) . . ? C14 C13 P4 121.9(8) . . ? C15 C14 C13 120.5(11) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 121.0(11) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 119.9(10) . . ? C17 C16 H16 120.0 . . ? C15 C16 H16 120.0 . . ? C18 C17 C16 118.3(11) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C17 C18 C13 122.9(11) . . ? C17 C18 H18 118.5 . . ? C13 C18 H18 118.5 . . ? O2 C19 C20 122.0(9) . . ? O2 C19 C24 114.6(8) . . ? C20 C19 C24 123.3(10) . . ? C19 C20 C21 117.9(10) . . ? C19 C20 H20 121.0 . . ? C21 C20 H20 121.0 . . ? C22 C21 C20 119.6(10) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 121.6(11) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C24 121.5(11) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C19 116.1(9) . . ? C23 C24 P5 126.0(8) . . ? C19 C24 P5 117.9(8) . . ? C30 C25 C26 117.1(10) . . ? C30 C25 P5 119.0(8) . . ? C26 C25 P5 123.9(8) . . ? C27 C26 C25 120.3(10) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C26 C27 C28 120.7(11) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C27 C28 C29 120.7(11) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C28 C29 C30 118.4(10) . . ? C28 C29 H29 120.8 . . ? C30 C29 H29 120.8 . . ? C29 C30 C25 122.8(10) . . ? C29 C30 H30 118.6 . . ? C25 C30 H30 118.6 . . ? C32 C31 C36 116.7(10) . . ? C32 C31 P5 121.6(8) . . ? C36 C31 P5 121.6(8) . . ? C33 C32 C31 122.1(11) . . ? C33 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? C32 C33 C34 119.9(11) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C35 C34 C33 119.6(11) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.0(11) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 121.6(11) . . ? C35 C36 H36 119.2 . . ? C31 C36 H36 119.2 . . ? C38 C37 C42 124.8(10) . . ? C38 C37 O3 118.7(9) . . ? C42 C37 O3 116.4(9) . . ? C37 C38 C39 119.4(11) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C40 C39 C38 117.7(11) . . ? C40 C39 H39 121.1 . . ? C38 C39 H39 121.1 . . ? C41 C40 C39 121.8(11) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C42 122.0(10) . . ? C40 C41 H41 119.0 . . ? C42 C41 H41 119.0 . . ? C37 C42 C41 114.3(9) . . ? C37 C42 C43 123.6(10) . . ? C41 C42 C43 122.1(10) . . ? C48 C43 C44 113.8(9) . . ? C48 C43 C42 123.6(9) . . ? C44 C43 C42 122.6(9) . . ? C45 C44 C43 122.5(11) . . ? C45 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? C44 C45 C46 121.3(10) . . ? C44 C45 H45 119.3 . . ? C46 C45 H45 119.3 . . ? C45 C46 C47 119.5(10) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C48 C47 C46 117.4(10) . . ? C48 C47 H47 121.3 . . ? C46 C47 H47 121.3 . . ? C47 C48 C43 125.4(10) . . ? C47 C48 O4 116.9(10) . . ? C43 C48 O4 117.7(9) . . ? C50 C49 C54 123.3(11) . . ? C50 C49 O5 118.9(9) . . ? C54 C49 O5 117.7(9) . . ? C49 C50 C51 119.0(10) . . ? C49 C50 H50 120.5 . . ? C51 C50 H50 120.5 . . ? C52 C51 C50 120.3(11) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 119.7(11) . . ? C51 C52 H52 120.1 . . ? C53 C52 H52 120.1 . . ? C54 C53 C52 121.6(10) . . ? C54 C53 H53 119.2 . . ? C52 C53 H53 119.2 . . ? C53 C54 C49 115.9(10) . . ? C53 C54 C55 120.6(10) . . ? C49 C54 C55 123.4(10) . . ? C56 C55 C60 116.0(10) . . ? C56 C55 C54 121.2(10) . . ? C60 C55 C54 122.7(9) . . ? C57 C56 C55 121.7(11) . . ? C57 C56 H56 119.1 . . ? C55 C56 H56 119.1 . . ? C56 C57 C58 120.4(10) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C59 C58 C57 118.4(11) . . ? C59 C58 H58 120.8 . . ? C57 C58 H58 120.8 . . ? C60 C59 C58 120.3(11) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C55 123.3(10) . . ? C59 C60 O6 118.2(9) . . ? C55 C60 O6 118.3(9) . . ? C91 C90 H90A 109.5 . . ? C91 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C91 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? N90 C91 C90 177.4(13) . . ? C94 C93 H93A 109.5 . . ? C94 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C94 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? N91 C94 C93 176.7(15) . . ? C96 C95 H95A 109.5 . . ? C96 C95 H95B 109.5 . . ? H95A C95 H95B 109.5 . . ? C96 C95 H95C 109.5 . . ? H95A C95 H95C 109.5 . . ? H95B C95 H95C 109.5 . . ? N93 C96 C95 178.4(16) . . ? C98 C97 H97A 109.5 . . ? C98 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C98 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? N94 C98 C97 178.1(15) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.963 _refine_diff_density_min -1.869 _refine_diff_density_rms 0.177 #===END data_cao376 _database_code_depnum_ccdc_archive 'CCDC 287632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62.7 H46.7 Au2 Cl10.1 N3 O6 P5' _chemical_formula_weight 1845.06 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' Cl Cl 0.1484 0.1585 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8387(2) _cell_length_b 14.0919(1) _cell_length_c 18.3886(1) _cell_angle_alpha 93.237(1) _cell_angle_beta 104.527(1) _cell_angle_gamma 100.185(1) _cell_volume 3397.49(6) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1485 _exptl_absorpt_coefficient_mu 4.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2358 _exptl_absorpt_correction_T_max 0.4088 _exptl_absorpt_process_details 'Blessing, Acta Cryst., 1995, A51, 33-38' _exptl_special_details ; PLATON / SQUEEZE used to remove disordered electron density corresponding to ca 2.7 molecules of CHCl3 / formula unit. removed 314 e- per cell and 869 A3 was left by the void ; _diffrn_ambient_temperature 356(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 'Brucker P4' _diffrn_measurement_method 'Area detector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30919 _diffrn_reflns_av_R_equivalents 0.0627 _diffrn_reflns_av_sigmaI/netI 0.0831 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 25.86 _reflns_number_total 12898 _reflns_number_gt 9596 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0715P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12898 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1295 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 0.62966(2) 0.70085(2) 0.849120(14) 0.02719(9) Uani 1 1 d . . . Au2 Au 0.33405(2) 0.834691(19) 0.464693(13) 0.02522(9) Uani 1 1 d . . . Cl1 Cl 0.72930(15) 0.85189(14) 0.88402(12) 0.0436(5) Uani 1 1 d . . . Cl2 Cl 0.35992(15) 0.70518(13) 0.39627(10) 0.0345(4) Uani 1 1 d . . . P1 P 0.33349(13) 0.75493(12) 0.70863(9) 0.0204(4) Uani 1 1 d . . . P2 P 0.26637(13) 0.78859(13) 0.83338(9) 0.0208(4) Uani 1 1 d . . . P3 P 0.14271(13) 0.66569(13) 0.71041(9) 0.0222(4) Uani 1 1 d . . . P4 P 0.52594(14) 0.55765(13) 0.80896(9) 0.0244(4) Uani 1 1 d . . . P5 P 0.31292(14) 0.95703(13) 0.53716(10) 0.0252(4) Uani 1 1 d . . . N1 N 0.3481(4) 0.8140(4) 0.7870(3) 0.0216(12) Uani 1 1 d . . . N2 N 0.1683(4) 0.7087(4) 0.7959(3) 0.0228(12) Uani 1 1 d . . . N3 N 0.2268(4) 0.6907(4) 0.6668(3) 0.0232(12) Uani 1 1 d . . . O1 O 0.4203(3) 0.6910(3) 0.7228(2) 0.0232(10) Uani 1 1 d . . . O2 O 0.3646(3) 0.8252(3) 0.6507(2) 0.0236(10) Uani 1 1 d . . . O3 O 0.3150(4) 0.7550(3) 0.9125(2) 0.0229(10) Uani 1 1 d . . . O4 O 0.2385(3) 0.8889(3) 0.8558(2) 0.0228(10) Uani 1 1 d . . . O5 O 0.1089(3) 0.5525(3) 0.7106(2) 0.0243(10) Uani 1 1 d . . . O6 O 0.0438(3) 0.6954(3) 0.6604(2) 0.0227(10) Uani 1 1 d . . . C1 C 0.4269(5) 0.6148(5) 0.6739(3) 0.0216(14) Uani 1 1 d . . . C2 C 0.3895(5) 0.6109(5) 0.5950(4) 0.0274(16) Uani 1 1 d . . . H2 H 0.3572 0.6589 0.5732 0.033 Uiso 1 1 calc R . . C3 C 0.4019(6) 0.5343(6) 0.5509(4) 0.0316(17) Uani 1 1 d . . . H3 H 0.3775 0.5301 0.4986 0.038 Uiso 1 1 calc R . . C4 C 0.4503(5) 0.4635(5) 0.5835(4) 0.0286(16) Uani 1 1 d . . . H4 H 0.4589 0.4127 0.5528 0.034 Uiso 1 1 calc R . . C5 C 0.4860(5) 0.4669(5) 0.6610(4) 0.0268(15) Uani 1 1 d . . . H5 H 0.5172 0.4181 0.6824 0.032 Uiso 1 1 calc R . . C6 C 0.4749(5) 0.5439(5) 0.7068(3) 0.0218(14) Uani 1 1 d . . . C7 C 0.5856(5) 0.4528(5) 0.8289(3) 0.0248(15) Uani 1 1 d . . . C8 C 0.5268(7) 0.3626(6) 0.8262(5) 0.047(2) Uani 1 1 d . . . H8 H 0.4563 0.3544 0.8154 0.057 Uiso 1 1 calc R . . C9 C 0.5736(8) 0.2854(7) 0.8398(5) 0.056(3) Uani 1 1 d . . . H9 H 0.5339 0.2239 0.8364 0.067 Uiso 1 1 calc R . . C10 C 0.6768(8) 0.2961(7) 0.8580(5) 0.054(3) Uani 1 1 d . . . H10 H 0.7077 0.2431 0.8685 0.065 Uiso 1 1 calc R . . C11 C 0.7340(7) 0.3863(8) 0.8604(5) 0.057(3) Uani 1 1 d . . . H11 H 0.8044 0.3938 0.8711 0.068 Uiso 1 1 calc R . . C12 C 0.6904(6) 0.4670(6) 0.8474(4) 0.0386(19) Uani 1 1 d . . . H12 H 0.7302 0.5285 0.8510 0.046 Uiso 1 1 calc R . . C13 C 0.4206(6) 0.5364(6) 0.8508(4) 0.0330(18) Uani 1 1 d . . . C14 C 0.3236(6) 0.4883(7) 0.8108(5) 0.051(2) Uani 1 1 d . . . H14 H 0.3097 0.4703 0.7592 0.061 Uiso 1 1 calc R . . C15 C 0.2476(7) 0.4670(9) 0.8475(6) 0.075(4) Uani 1 1 d . . . H15 H 0.1824 0.4350 0.8211 0.090 Uiso 1 1 calc R . . C16 C 0.2714(8) 0.4948(9) 0.9255(6) 0.071(4) Uani 1 1 d . . . H16 H 0.2210 0.4803 0.9507 0.085 Uiso 1 1 calc R . . C17 C 0.3631(8) 0.5410(7) 0.9642(5) 0.048(2) Uani 1 1 d . . . H17 H 0.3768 0.5586 1.0158 0.057 Uiso 1 1 calc R . . C18 C 0.4379(7) 0.5626(6) 0.9277(4) 0.0371(19) Uani 1 1 d . . . H18 H 0.5021 0.5958 0.9551 0.045 Uiso 1 1 calc R . . C19 C 0.4357(5) 0.9120(5) 0.6700(4) 0.0265(15) Uani 1 1 d . . . C20 C 0.5228(5) 0.9237(6) 0.7299(4) 0.0286(16) Uani 1 1 d . . . H20 H 0.5351 0.8737 0.7597 0.034 Uiso 1 1 calc R . . C21 C 0.5898(5) 1.0109(6) 0.7439(4) 0.0329(18) Uani 1 1 d . . . H21 H 0.6488 1.0195 0.7834 0.039 Uiso 1 1 calc R . . C22 C 0.5721(7) 1.0857(6) 0.7010(4) 0.041(2) Uani 1 1 d . . . H22 H 0.6177 1.1449 0.7124 0.049 Uiso 1 1 calc R . . C23 C 0.4850(6) 1.0727(5) 0.6401(4) 0.0327(17) Uani 1 1 d . . . H23 H 0.4729 1.1233 0.6109 0.039 Uiso 1 1 calc R . . C24 C 0.4170(5) 0.9849(5) 0.6232(4) 0.0241(15) Uani 1 1 d . . . C25 C 0.3155(6) 1.0717(5) 0.4974(4) 0.0324(17) Uani 1 1 d . . . C26 C 0.3657(8) 1.0902(6) 0.4407(4) 0.048(2) Uani 1 1 d . . . H26 H 0.3914 1.0417 0.4198 0.057 Uiso 1 1 calc R . . C27 C 0.3768(9) 1.1831(7) 0.4158(5) 0.065(3) Uani 1 1 d . . . H27 H 0.4121 1.1969 0.3796 0.078 Uiso 1 1 calc R . . C28 C 0.3366(7) 1.2518(6) 0.4440(5) 0.055(3) Uani 1 1 d . . . H28 H 0.3430 1.3124 0.4260 0.066 Uiso 1 1 calc R . . C29 C 0.2849(6) 1.2344(6) 0.5002(6) 0.048(2) Uani 1 1 d . . . H29 H 0.2585 1.2829 0.5203 0.058 Uiso 1 1 calc R . . C30 C 0.2742(6) 1.1423(6) 0.5250(5) 0.047(2) Uani 1 1 d . . . H30 H 0.2383 1.1288 0.5609 0.056 Uiso 1 1 calc R . . C31 C 0.1937(6) 0.9345(5) 0.5639(4) 0.0318(17) Uani 1 1 d . . . C32 C 0.1068(6) 0.8979(5) 0.5076(5) 0.0396(19) Uani 1 1 d . . . H32 H 0.1116 0.8806 0.4593 0.048 Uiso 1 1 calc R . . C33 C 0.0123(7) 0.8863(6) 0.5218(6) 0.049(2) Uani 1 1 d . . . H33 H -0.0466 0.8641 0.4829 0.058 Uiso 1 1 calc R . . C34 C 0.0066(8) 0.9083(6) 0.5951(7) 0.059(3) Uani 1 1 d . . . H34 H -0.0566 0.9001 0.6055 0.070 Uiso 1 1 calc R . . C35 C 0.0946(8) 0.9427(7) 0.6530(6) 0.056(3) Uani 1 1 d . . . H35 H 0.0903 0.9569 0.7019 0.067 Uiso 1 1 calc R . . C36 C 0.1881(6) 0.9555(6) 0.6378(5) 0.042(2) Uani 1 1 d . . . H36 H 0.2472 0.9779 0.6764 0.050 Uiso 1 1 calc R . . C37 C 0.1862(5) 0.8928(5) 0.9121(4) 0.0266(15) Uani 1 1 d . . . C38 C 0.0844(6) 0.8959(6) 0.8909(4) 0.039(2) Uani 1 1 d . . . H38 H 0.0506 0.8924 0.8400 0.047 Uiso 1 1 calc R . . C39 C 0.0322(6) 0.9041(7) 0.9449(5) 0.046(2) Uani 1 1 d . . . H39 H -0.0369 0.9052 0.9307 0.055 Uiso 1 1 calc R . . C40 C 0.0843(6) 0.9108(6) 1.0207(4) 0.0394(19) Uani 1 1 d . . . H40 H 0.0500 0.9184 1.0575 0.047 Uiso 1 1 calc R . . C41 C 0.1867(6) 0.9063(5) 1.0423(4) 0.0311(17) Uani 1 1 d . . . H41 H 0.2203 0.9101 1.0933 0.037 Uiso 1 1 calc R . . C42 C 0.2400(5) 0.8960(5) 0.9874(4) 0.0223(14) Uani 1 1 d . . . C43 C 0.3488(5) 0.8892(5) 1.0096(3) 0.0238(15) Uani 1 1 d . . . C44 C 0.4202(5) 0.9508(5) 1.0687(3) 0.0252(15) Uani 1 1 d . . . H44 H 0.3990 0.9968 1.0961 0.030 Uiso 1 1 calc R . . C45 C 0.5216(5) 0.9439(5) 1.0867(4) 0.0283(16) Uani 1 1 d . . . H45 H 0.5678 0.9838 1.1271 0.034 Uiso 1 1 calc R . . C46 C 0.5544(6) 0.8783(6) 1.0453(4) 0.0323(17) Uani 1 1 d . . . H46 H 0.6232 0.8754 1.0574 0.039 Uiso 1 1 calc R . . C47 C 0.4869(5) 0.8163(5) 0.9858(4) 0.0238(15) Uani 1 1 d . . . H47 H 0.5093 0.7723 0.9575 0.029 Uiso 1 1 calc R . . C48 C 0.3857(5) 0.8221(5) 0.9700(3) 0.0219(14) Uani 1 1 d . . . C49 C 0.0502(5) 0.4926(5) 0.6430(4) 0.0268(16) Uani 1 1 d . . . C50 C 0.0973(6) 0.4315(5) 0.6113(4) 0.0332(18) Uani 1 1 d . . . H50 H 0.1663 0.4320 0.6305 0.040 Uiso 1 1 calc R . . C51 C 0.0384(7) 0.3676(6) 0.5487(4) 0.0386(19) Uani 1 1 d . . . H51 H 0.0685 0.3242 0.5263 0.046 Uiso 1 1 calc R . . C52 C -0.0623(7) 0.3676(6) 0.5201(4) 0.041(2) Uani 1 1 d . . . H52 H -0.1009 0.3242 0.4787 0.050 Uiso 1 1 calc R . . C53 C -0.1068(6) 0.4325(5) 0.5530(4) 0.0335(18) Uani 1 1 d . . . H53 H -0.1753 0.4331 0.5326 0.040 Uiso 1 1 calc R . . C54 C -0.0518(5) 0.4972(5) 0.6160(4) 0.0283(16) Uani 1 1 d . . . C55 C -0.0992(5) 0.5674(5) 0.6522(4) 0.0292(16) Uani 1 1 d . . . C56 C -0.1972(6) 0.5383(6) 0.6640(4) 0.0355(19) Uani 1 1 d . . . H56 H -0.2338 0.4756 0.6470 0.043 Uiso 1 1 calc R . . C57 C -0.2377(6) 0.6019(7) 0.7001(4) 0.047(2) Uani 1 1 d . . . H57 H -0.3011 0.5816 0.7087 0.056 Uiso 1 1 calc R . . C58 C -0.1857(6) 0.6964(6) 0.7241(4) 0.0369(19) Uani 1 1 d . . . H58 H -0.2141 0.7391 0.7489 0.044 Uiso 1 1 calc R . . C59 C -0.0916(6) 0.7269(6) 0.7110(4) 0.0325(17) Uani 1 1 d . . . H59 H -0.0567 0.7906 0.7258 0.039 Uiso 1 1 calc R . . C60 C -0.0509(5) 0.6623(5) 0.6762(4) 0.0268(16) 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 0.02762(16) 0.02776(17) 0.02179(15) -0.00179(11) 0.00290(11) 0.00058(12) Au2 0.03142(17) 0.02286(15) 0.01770(14) 0.00355(11) 0.00544(11) -0.00315(12) Cl1 0.0354(11) 0.0323(11) 0.0521(12) -0.0082(9) -0.0005(9) -0.0006(9) Cl2 0.0467(11) 0.0273(9) 0.0298(9) 0.0019(7) 0.0187(8) -0.0038(8) P1 0.0260(9) 0.0211(9) 0.0125(8) 0.0013(7) 0.0073(7) -0.0023(7) P2 0.0244(9) 0.0213(9) 0.0139(8) -0.0003(7) 0.0054(7) -0.0026(7) P3 0.0260(9) 0.0224(9) 0.0147(8) -0.0006(7) 0.0062(7) -0.0048(8) P4 0.0292(10) 0.0284(10) 0.0158(8) 0.0030(7) 0.0090(7) 0.0019(8) P5 0.0276(10) 0.0246(10) 0.0214(9) 0.0038(7) 0.0066(8) -0.0008(8) N1 0.024(3) 0.024(3) 0.015(3) 0.000(2) 0.008(2) -0.004(2) N2 0.024(3) 0.026(3) 0.014(3) 0.001(2) 0.005(2) -0.004(3) N3 0.026(3) 0.029(3) 0.014(3) 0.000(2) 0.008(2) -0.001(3) O1 0.029(3) 0.024(3) 0.014(2) 0.0035(19) 0.0046(19) -0.001(2) O2 0.032(3) 0.023(2) 0.013(2) 0.0054(18) 0.0053(19) -0.002(2) O3 0.034(3) 0.020(2) 0.011(2) 0.0004(18) 0.0042(19) -0.003(2) O4 0.026(3) 0.027(3) 0.014(2) 0.0026(19) 0.0057(19) -0.002(2) O5 0.029(3) 0.021(2) 0.017(2) 0.0024(19) 0.005(2) -0.009(2) O6 0.021(2) 0.024(3) 0.020(2) 0.0015(19) 0.0071(19) -0.004(2) C1 0.023(4) 0.024(4) 0.016(3) -0.001(3) 0.011(3) -0.007(3) C2 0.027(4) 0.034(4) 0.017(3) 0.003(3) 0.004(3) -0.002(3) C3 0.032(4) 0.039(4) 0.019(4) 0.000(3) 0.009(3) -0.007(4) C4 0.028(4) 0.034(4) 0.022(4) -0.005(3) 0.012(3) -0.003(3) C5 0.032(4) 0.022(4) 0.023(4) 0.004(3) 0.008(3) -0.005(3) C6 0.023(4) 0.022(3) 0.018(3) 0.004(3) 0.010(3) -0.009(3) C7 0.033(4) 0.028(4) 0.015(3) 0.006(3) 0.011(3) 0.004(3) C8 0.049(5) 0.040(5) 0.057(6) 0.008(4) 0.027(5) -0.001(4) C9 0.087(8) 0.040(5) 0.054(6) 0.023(4) 0.040(6) 0.007(5) C10 0.077(7) 0.040(5) 0.060(6) 0.030(5) 0.034(5) 0.025(5) C11 0.045(6) 0.071(7) 0.059(6) 0.024(5) 0.012(5) 0.020(5) C12 0.041(5) 0.041(5) 0.039(4) 0.020(4) 0.013(4) 0.012(4) C13 0.051(5) 0.036(4) 0.022(4) 0.009(3) 0.021(4) 0.015(4) C14 0.033(5) 0.084(7) 0.030(4) 0.019(4) 0.008(4) -0.008(5) C15 0.040(5) 0.133(11) 0.062(7) 0.059(7) 0.020(5) 0.018(6) C16 0.061(7) 0.131(11) 0.055(6) 0.059(7) 0.046(6) 0.052(7) C17 0.070(7) 0.061(6) 0.038(5) 0.029(4) 0.039(5) 0.037(5) C18 0.053(5) 0.049(5) 0.019(4) 0.015(3) 0.019(4) 0.021(4) C19 0.025(4) 0.034(4) 0.018(3) 0.002(3) 0.009(3) -0.006(3) C20 0.025(4) 0.038(4) 0.022(3) 0.008(3) 0.011(3) -0.005(3) C21 0.024(4) 0.045(5) 0.022(4) -0.001(3) 0.006(3) -0.012(3) C22 0.057(5) 0.039(5) 0.023(4) 0.006(3) 0.016(4) -0.012(4) C23 0.039(4) 0.025(4) 0.030(4) -0.003(3) 0.010(3) -0.008(3) C24 0.026(4) 0.027(4) 0.018(3) 0.000(3) 0.009(3) -0.002(3) C25 0.031(4) 0.027(4) 0.029(4) 0.007(3) -0.002(3) -0.005(3) C26 0.091(7) 0.023(4) 0.031(4) 0.014(3) 0.024(5) 0.000(4) C27 0.129(10) 0.037(5) 0.021(4) 0.002(4) 0.019(5) -0.007(6) C28 0.074(7) 0.020(4) 0.043(5) 0.012(4) -0.021(5) -0.012(4) C29 0.034(5) 0.026(4) 0.085(7) 0.016(4) 0.013(5) 0.006(4) C30 0.028(4) 0.043(5) 0.070(6) 0.014(5) 0.016(4) 0.001(4) C31 0.029(4) 0.026(4) 0.039(4) 0.009(3) 0.013(3) -0.004(3) C32 0.039(5) 0.027(4) 0.054(5) 0.007(4) 0.016(4) 0.003(4) C33 0.037(5) 0.031(5) 0.073(6) 0.004(4) 0.011(5) 0.000(4) C34 0.050(6) 0.034(5) 0.113(9) 0.035(6) 0.047(6) 0.019(5) C35 0.055(6) 0.046(6) 0.078(7) 0.024(5) 0.038(6) 0.008(5) C36 0.039(5) 0.034(5) 0.052(5) 0.008(4) 0.014(4) 0.004(4) C37 0.029(4) 0.033(4) 0.018(3) -0.001(3) 0.010(3) 0.001(3) C38 0.034(4) 0.052(5) 0.022(4) -0.013(4) -0.007(3) 0.008(4) C39 0.024(4) 0.068(6) 0.041(5) -0.005(4) 0.007(4) 0.005(4) C40 0.035(5) 0.052(5) 0.028(4) -0.006(4) 0.013(3) -0.004(4) C41 0.043(5) 0.032(4) 0.021(4) 0.000(3) 0.016(3) 0.002(4) C42 0.025(4) 0.020(3) 0.022(3) 0.002(3) 0.010(3) -0.002(3) C43 0.035(4) 0.023(4) 0.012(3) 0.003(3) 0.011(3) -0.002(3) C44 0.035(4) 0.026(4) 0.011(3) 0.005(3) 0.006(3) -0.005(3) C45 0.031(4) 0.031(4) 0.016(3) 0.007(3) 0.003(3) -0.009(3) C46 0.025(4) 0.040(5) 0.031(4) 0.019(4) 0.008(3) -0.001(3) C47 0.026(4) 0.027(4) 0.018(3) 0.006(3) 0.009(3) -0.001(3) C48 0.031(4) 0.020(3) 0.009(3) 0.001(3) 0.003(3) -0.006(3) C49 0.033(4) 0.023(4) 0.018(3) 0.007(3) 0.004(3) -0.009(3) C50 0.050(5) 0.025(4) 0.019(4) 0.003(3) 0.006(3) -0.002(4) C51 0.057(6) 0.027(4) 0.029(4) -0.005(3) 0.018(4) -0.003(4) C52 0.059(6) 0.037(5) 0.013(3) -0.004(3) 0.001(4) -0.017(4) C53 0.039(4) 0.028(4) 0.022(4) 0.002(3) 0.000(3) -0.011(3) C54 0.032(4) 0.025(4) 0.017(3) 0.004(3) 0.000(3) -0.010(3) C55 0.027(4) 0.034(4) 0.021(3) 0.008(3) 0.006(3) -0.009(3) C56 0.029(4) 0.048(5) 0.017(3) 0.009(3) -0.002(3) -0.015(4) C57 0.035(5) 0.080(7) 0.026(4) 0.021(4) 0.010(4) 0.004(5) C58 0.036(4) 0.049(5) 0.025(4) 0.009(4) 0.011(3) 0.003(4) C59 0.037(4) 0.036(4) 0.023(4) 0.003(3) 0.011(3) -0.001(4) C60 0.022(4) 0.032(4) 0.021(3) 0.006(3) 0.002(3) -0.005(3) _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 P4 2.2256(19) . ? Au1 Cl1 2.282(2) . ? Au2 P5 2.2244(19) . ? Au2 Cl2 2.2890(18) . ? P1 N1 1.571(5) . ? P1 N3 1.572(6) . ? P1 O2 1.580(4) . ? P1 O1 1.604(5) . ? P2 N2 1.577(6) . ? P2 O3 1.580(4) . ? P2 N1 1.584(5) . ? P2 O4 1.589(5) . ? P3 N3 1.573(5) . ? P3 O5 1.581(5) . ? P3 N2 1.582(5) . ? P3 O6 1.585(5) . ? P4 C13 1.800(7) . ? P4 C6 1.819(6) . ? P4 C7 1.828(7) . ? P5 C25 1.809(7) . ? P5 C31 1.817(7) . ? P5 C24 1.822(7) . ? O1 C1 1.392(8) . ? O2 C19 1.394(8) . ? O3 C48 1.418(8) . ? O4 C37 1.409(7) . ? O5 C49 1.432(8) . ? O6 C60 1.416(8) . ? C1 C6 1.380(9) . ? C1 C2 1.408(9) . ? C2 C3 1.375(10) . ? C3 C4 1.380(10) . ? C4 C5 1.383(9) . ? C5 C6 1.390(9) . ? C7 C8 1.373(11) . ? C7 C12 1.378(10) . ? C8 C9 1.366(12) . ? C9 C10 1.362(13) . ? C10 C11 1.366(13) . ? C11 C12 1.384(12) . ? C13 C14 1.389(11) . ? C13 C18 1.390(9) . ? C14 C15 1.386(12) . ? C15 C16 1.405(14) . ? C16 C17 1.320(14) . ? C17 C18 1.369(11) . ? C19 C20 1.391(9) . ? C19 C24 1.394(10) . ? C20 C21 1.370(10) . ? C21 C22 1.371(11) . ? C22 C23 1.401(11) . ? C23 C24 1.383(10) . ? C25 C30 1.365(11) . ? C25 C26 1.404(11) . ? C26 C27 1.407(11) . ? C27 C28 1.339(13) . ? C28 C29 1.407(13) . ? C29 C30 1.395(11) . ? C31 C32 1.371(11) . ? C31 C36 1.399(11) . ? C32 C33 1.379(11) . ? C33 C34 1.392(14) . ? C34 C35 1.391(14) . ? C35 C36 1.373(12) . ? C37 C38 1.373(10) . ? C37 C42 1.392(9) . ? C38 C39 1.376(11) . ? C39 C40 1.389(10) . ? C40 C41 1.386(11) . ? C41 C42 1.407(9) . ? C42 C43 1.479(10) . ? C43 C44 1.401(9) . ? C43 C48 1.401(9) . ? C44 C45 1.381(10) . ? C45 C46 1.372(10) . ? C46 C47 1.387(10) . ? C47 C48 1.376(9) . ? C49 C50 1.356(10) . ? C49 C54 1.388(10) . ? C50 C51 1.397(10) . ? C51 C52 1.360(12) . ? C52 C53 1.380(11) . ? C53 C54 1.395(9) . ? C54 C55 1.493(10) . ? C55 C60 1.378(10) . ? C55 C56 1.420(10) . ? C56 C57 1.362(12) . ? C57 C58 1.386(12) . ? C58 C59 1.382(10) . ? C59 C60 1.362(10) . ? 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 P4 Au1 Cl1 176.21(7) . . ? P5 Au2 Cl2 176.73(6) . . ? N1 P1 N3 119.8(3) . . ? N1 P1 O2 110.1(3) . . ? N3 P1 O2 106.6(3) . . ? N1 P1 O1 105.3(3) . . ? N3 P1 O1 110.9(3) . . ? O2 P1 O1 103.0(2) . . ? N2 P2 O3 105.7(3) . . ? N2 P2 N1 118.0(3) . . ? O3 P2 N1 111.6(3) . . ? N2 P2 O4 111.9(3) . . ? O3 P2 O4 102.9(2) . . ? N1 P2 O4 105.7(3) . . ? N3 P3 O5 111.7(3) . . ? N3 P3 N2 118.2(3) . . ? O5 P3 N2 105.1(3) . . ? N3 P3 O6 105.8(3) . . ? O5 P3 O6 103.2(3) . . ? N2 P3 O6 112.1(3) . . ? C13 P4 C6 108.1(3) . . ? C13 P4 C7 103.6(3) . . ? C6 P4 C7 104.6(3) . . ? C13 P4 Au1 113.7(3) . . ? C6 P4 Au1 111.1(2) . . ? C7 P4 Au1 114.9(2) . . ? C25 P5 C31 104.5(4) . . ? C25 P5 C24 103.4(3) . . ? C31 P5 C24 108.2(3) . . ? C25 P5 Au2 115.9(3) . . ? C31 P5 Au2 113.9(3) . . ? C24 P5 Au2 110.1(2) . . ? P1 N1 P2 119.8(3) . . ? P2 N2 P3 121.7(3) . . ? P1 N3 P3 120.1(3) . . ? C1 O1 P1 126.3(4) . . ? C19 O2 P1 125.3(4) . . ? C48 O3 P2 120.4(4) . . ? C37 O4 P2 118.3(4) . . ? C49 O5 P3 121.0(4) . . ? C60 O6 P3 118.8(4) . . ? C6 C1 O1 116.4(5) . . ? C6 C1 C2 121.4(6) . . ? O1 C1 C2 122.1(6) . . ? C3 C2 C1 118.2(7) . . ? C2 C3 C4 120.6(7) . . ? C3 C4 C5 121.1(7) . . ? C4 C5 C6 119.5(7) . . ? C1 C6 C5 119.2(6) . . ? C1 C6 P4 118.4(5) . . ? C5 C6 P4 122.3(5) . . ? C8 C7 C12 121.3(7) . . ? C8 C7 P4 120.3(6) . . ? C12 C7 P4 118.3(6) . . ? C9 C8 C7 118.9(8) . . ? C10 C9 C8 121.7(9) . . ? C9 C10 C11 118.5(8) . . ? C10 C11 C12 122.1(9) . . ? C7 C12 C11 117.4(8) . . ? C14 C13 C18 118.0(7) . . ? C14 C13 P4 122.8(6) . . ? C18 C13 P4 119.1(6) . . ? C15 C14 C13 120.2(9) . . ? C14 C15 C16 118.4(10) . . ? C17 C16 C15 122.0(8) . . ? C16 C17 C18 119.4(8) . . ? C17 C18 C13 121.9(9) . . ? C20 C19 C24 122.0(7) . . ? C20 C19 O2 122.1(6) . . ? C24 C19 O2 115.9(6) . . ? C21 C20 C19 118.2(7) . . ? C20 C21 C22 121.6(7) . . ? C21 C22 C23 119.8(7) . . ? C24 C23 C22 120.2(7) . . ? C23 C24 C19 118.2(6) . . ? C23 C24 P5 122.4(5) . . ? C19 C24 P5 119.1(5) . . ? C30 C25 C26 119.7(7) . . ? C30 C25 P5 120.7(6) . . ? C26 C25 P5 119.6(6) . . ? C25 C26 C27 119.2(8) . . ? C28 C27 C26 120.3(9) . . ? C27 C28 C29 121.5(8) . . ? C30 C29 C28 118.2(8) . . ? C25 C30 C29 121.1(8) . . ? C32 C31 C36 120.1(7) . . ? C32 C31 P5 117.2(6) . . ? C36 C31 P5 122.7(6) . . ? C31 C32 C33 120.9(8) . . ? C32 C33 C34 118.9(9) . . ? C35 C34 C33 120.4(9) . . ? C36 C35 C34 120.0(9) . . ? C35 C36 C31 119.6(9) . . ? C38 C37 C42 122.4(6) . . ? C38 C37 O4 118.8(6) . . ? C42 C37 O4 118.8(6) . . ? C37 C38 C39 120.2(7) . . ? C38 C39 C40 119.1(7) . . ? C41 C40 C39 120.9(7) . . ? C40 C41 C42 120.3(7) . . ? C37 C42 C41 117.1(6) . . ? C37 C42 C43 122.0(6) . . ? C41 C42 C43 120.9(6) . . ? C44 C43 C48 116.8(6) . . ? C44 C43 C42 122.3(6) . . ? C48 C43 C42 120.9(6) . . ? C45 C44 C43 120.8(7) . . ? C46 C45 C44 120.3(7) . . ? C45 C46 C47 121.1(7) . . ? C48 C47 C46 117.8(7) . . ? C47 C48 C43 123.1(6) . . ? C47 C48 O3 118.3(6) . . ? C43 C48 O3 118.5(6) . . ? C50 C49 C54 124.1(7) . . ? C50 C49 O5 117.4(6) . . ? C54 C49 O5 118.4(6) . . ? C49 C50 C51 117.6(8) . . ? C52 C51 C50 121.2(8) . . ? C51 C52 C53 119.4(7) . . ? C52 C53 C54 121.9(7) . . ? C49 C54 C53 115.9(7) . . ? C49 C54 C55 121.9(6) . . ? C53 C54 C55 122.3(7) . . ? C60 C55 C56 116.9(7) . . ? C60 C55 C54 122.4(6) . . ? C56 C55 C54 120.7(7) . . ? C57 C56 C55 120.1(8) . . ? C56 C57 C58 121.0(8) . . ? C59 C58 C57 119.6(8) . . ? C60 C59 C58 118.9(7) . . ? C59 C60 C55 123.3(7) . . ? C59 C60 O6 118.4(6) . . ? C55 C60 O6 118.1(6) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.86 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 3.690 _refine_diff_density_min -3.577 _refine_diff_density_rms 0.195 #===END data_gf333 _database_code_depnum_ccdc_archive 'CCDC 287633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H47 Au B F4 N4 O6 P3' _chemical_formula_weight 1320.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.20100(10) _cell_length_b 14.29780(10) _cell_length_c 17.67400(10) _cell_angle_alpha 69.2870(10) _cell_angle_beta 83.0740(10) _cell_angle_gamma 67.9420(10) _cell_volume 2672.54(3) _cell_formula_units_Z 2 _cell_measurement_temperature 83(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 2.915 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789285 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'Blessing, Acta Cryst., 1995, A51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 83(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 'Brucker P4' _diffrn_measurement_method 'Area detector /w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27712 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0341 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 27.04 _reflns_number_total 11570 _reflns_number_gt 10643 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0216P)^2^+3.8760P] 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 11570 _refine_ls_number_parameters 749 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0304 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0638 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.049138(9) 0.822011(9) 0.382580(7) 0.01357(4) Uani 1 1 d . . . P1 P 0.23798(6) 0.68324(5) 0.27339(4) 0.01006(13) Uani 1 1 d . . . P2 P 0.41128(6) 0.64844(6) 0.16448(4) 0.01087(14) Uani 1 1 d . . . P3 P 0.29448(6) 0.84863(6) 0.16758(4) 0.01075(14) Uani 1 1 d . . . P4 P 0.20919(6) 0.81281(6) 0.44176(4) 0.01242(14) Uani 1 1 d . . . P5 P -0.10117(6) 0.80608(6) 0.33168(4) 0.01235(14) Uani 1 1 d . . . N1 N 0.2252(2) 0.80296(18) 0.24162(14) 0.0111(5) Uani 1 1 d . . . N2 N 0.3285(2) 0.60855(18) 0.23128(14) 0.0122(5) Uani 1 1 d . . . N3 N 0.3834(2) 0.77068(19) 0.12760(14) 0.0134(5) Uani 1 1 d . . . O1 O 0.26179(16) 0.63668(15) 0.36711(11) 0.0111(4) Uani 1 1 d . . . O2 O 0.11476(16) 0.67208(15) 0.27857(11) 0.0113(4) Uani 1 1 d . . . O3 O 0.53825(17) 0.58531(16) 0.20246(11) 0.0127(4) Uani 1 1 d . . . O4 O 0.41625(17) 0.61122(15) 0.09151(11) 0.0129(4) Uani 1 1 d . . . O5 O 0.35411(17) 0.91043(15) 0.19553(11) 0.0124(4) Uani 1 1 d . . . O6 O 0.20798(17) 0.93884(15) 0.09853(11) 0.0112(4) Uani 1 1 d . . . C1 C 0.3607(2) 0.6452(2) 0.39064(16) 0.0126(5) Uani 1 1 d . . . C2 C 0.4678(3) 0.5714(2) 0.38482(17) 0.0159(6) Uani 1 1 d . . . H2 H 0.4731 0.5152 0.3678 0.019 Uiso 1 1 calc R . . C3 C 0.5675(3) 0.5803(3) 0.40410(18) 0.0192(6) Uani 1 1 d . . . H3 H 0.6413 0.5298 0.4009 0.023 Uiso 1 1 calc R . . C4 C 0.5582(3) 0.6633(3) 0.42810(19) 0.0198(6) Uani 1 1 d . . . H4 H 0.6262 0.6702 0.4404 0.024 Uiso 1 1 calc R . . C5 C 0.4505(3) 0.7364(2) 0.43426(18) 0.0170(6) Uani 1 1 d . . . H5 H 0.4456 0.7934 0.4500 0.020 Uiso 1 1 calc R . . C6 C 0.3486(2) 0.7272(2) 0.41750(17) 0.0141(6) Uani 1 1 d . . . C7 C 0.2244(3) 0.9380(2) 0.42065(18) 0.0151(6) Uani 1 1 d . . . C8 C 0.2034(3) 1.0087(2) 0.34293(18) 0.0175(6) Uani 1 1 d . . . H8 H 0.1815 0.9904 0.3030 0.021 Uiso 1 1 calc R . . C9 C 0.2145(3) 1.1050(3) 0.32429(19) 0.0214(6) Uani 1 1 d . . . H9 H 0.2014 1.1524 0.2714 0.026 Uiso 1 1 calc R . . C10 C 0.2447(3) 1.1326(3) 0.3826(2) 0.0230(7) Uani 1 1 d . . . H10 H 0.2505 1.1995 0.3696 0.028 Uiso 1 1 calc R . . C11 C 0.2666(3) 1.0631(3) 0.4598(2) 0.0250(7) Uani 1 1 d . . . H11 H 0.2885 1.0820 0.4993 0.030 Uiso 1 1 calc R . . C12 C 0.2563(3) 0.9656(3) 0.47925(19) 0.0219(7) Uani 1 1 d . . . H12 H 0.2708 0.9180 0.5320 0.026 Uiso 1 1 calc R . . C13 C 0.2011(3) 0.7561(2) 0.54854(17) 0.0143(6) Uani 1 1 d . . . C14 C 0.2991(3) 0.6939(3) 0.59764(19) 0.0208(6) Uani 1 1 d . . . H14 H 0.3741 0.6824 0.5755 0.025 Uiso 1 1 calc R . . C15 C 0.2871(3) 0.6489(3) 0.67867(19) 0.0229(7) Uani 1 1 d . . . H15 H 0.3541 0.6072 0.7116 0.028 Uiso 1 1 calc R . . C16 C 0.1787(3) 0.6646(3) 0.71138(19) 0.0226(7) Uani 1 1 d . . . H16 H 0.1709 0.6323 0.7665 0.027 Uiso 1 1 calc R . . C17 C 0.0809(3) 0.7275(3) 0.6637(2) 0.0309(8) Uani 1 1 d . . . H17 H 0.0062 0.7396 0.6865 0.037 Uiso 1 1 calc R . . C18 C 0.0918(3) 0.7731(3) 0.58263(19) 0.0249(7) Uani 1 1 d . . . H18 H 0.0245 0.8160 0.5503 0.030 Uiso 1 1 calc R . . C19 C 0.0356(2) 0.7346(2) 0.21462(17) 0.0130(5) Uani 1 1 d . . . C20 C 0.0627(3) 0.7269(2) 0.14008(18) 0.0158(6) Uani 1 1 d . . . H20 H 0.1351 0.6794 0.1306 0.019 Uiso 1 1 calc R . . C21 C -0.0192(3) 0.7906(2) 0.07894(18) 0.0180(6) Uani 1 1 d . . . H21 H -0.0016 0.7874 0.0270 0.022 Uiso 1 1 calc R . . C22 C -0.1256(3) 0.8584(2) 0.09337(18) 0.0179(6) Uani 1 1 d . . . H22 H -0.1801 0.9020 0.0512 0.021 Uiso 1 1 calc R . . C23 C -0.1528(3) 0.8628(2) 0.16937(17) 0.0141(6) Uani 1 1 d . . . H23 H -0.2269 0.9077 0.1792 0.017 Uiso 1 1 calc R . . C24 C -0.0716(2) 0.8013(2) 0.23157(16) 0.0115(5) Uani 1 1 d . . . C25 C -0.1210(2) 0.6835(2) 0.38999(18) 0.0162(6) Uani 1 1 d . . . C26 C -0.1117(3) 0.6080(2) 0.35652(19) 0.0183(6) Uani 1 1 d . . . H26 H -0.0983 0.6212 0.3015 0.022 Uiso 1 1 calc R . . C27 C -0.1224(3) 0.5129(3) 0.4047(2) 0.0243(7) Uani 1 1 d . . . H27 H -0.1161 0.4612 0.3823 0.029 Uiso 1 1 calc R . . C28 C -0.1423(3) 0.4943(3) 0.4850(2) 0.0261(7) Uani 1 1 d . . . H28 H -0.1493 0.4296 0.5175 0.031 Uiso 1 1 calc R . . C29 C -0.1519(3) 0.5694(3) 0.5182(2) 0.0269(8) Uani 1 1 d . . . H29 H -0.1662 0.5562 0.5732 0.032 Uiso 1 1 calc R . . C30 C -0.1406(3) 0.6638(3) 0.47135(18) 0.0204(6) Uani 1 1 d . . . H30 H -0.1462 0.7148 0.4943 0.024 Uiso 1 1 calc R . . C31 C -0.2403(2) 0.9111(2) 0.32392(16) 0.0147(6) Uani 1 1 d . . . C32 C -0.3435(3) 0.8936(3) 0.32679(18) 0.0197(6) Uani 1 1 d . . . H32 H -0.3417 0.8248 0.3363 0.024 Uiso 1 1 calc R . . C33 C -0.4489(3) 0.9764(3) 0.3159(2) 0.0261(7) Uani 1 1 d . . . H33 H -0.5192 0.9643 0.3186 0.031 Uiso 1 1 calc R . . C34 C -0.4508(3) 1.0774(3) 0.3008(2) 0.0290(8) Uani 1 1 d . . . H34 H -0.5226 1.1345 0.2921 0.035 Uiso 1 1 calc R . . C35 C -0.3484(3) 1.0949(3) 0.2986(2) 0.0282(7) Uani 1 1 d . . . H35 H -0.3503 1.1638 0.2889 0.034 Uiso 1 1 calc R . . C36 C -0.2429(3) 1.0119(3) 0.31058(19) 0.0203(6) Uani 1 1 d . . . H36 H -0.1728 1.0238 0.3097 0.024 Uiso 1 1 calc R . . C37 C 0.6375(2) 0.5809(2) 0.15527(17) 0.0140(6) Uani 1 1 d . . . C38 C 0.7095(3) 0.6269(2) 0.16793(19) 0.0189(6) Uani 1 1 d . . . H38 H 0.6878 0.6661 0.2030 0.023 Uiso 1 1 calc R . . C39 C 0.8139(3) 0.6147(3) 0.1285(2) 0.0229(7) Uani 1 1 d . . . H39 H 0.8655 0.6437 0.1377 0.027 Uiso 1 1 calc R . . C40 C 0.8428(3) 0.5599(3) 0.0754(2) 0.0222(7) Uani 1 1 d . . . H40 H 0.9132 0.5537 0.0471 0.027 Uiso 1 1 calc R . . C41 C 0.7701(3) 0.5145(2) 0.06337(18) 0.0188(6) Uani 1 1 d . . . H41 H 0.7908 0.4777 0.0266 0.023 Uiso 1 1 calc R . . C42 C 0.6656(2) 0.5220(2) 0.10486(17) 0.0131(5) Uani 1 1 d . . . C43 C 0.5937(3) 0.4626(2) 0.10051(17) 0.0151(6) Uani 1 1 d . . . C44 C 0.6457(3) 0.3588(2) 0.10118(18) 0.0182(6) Uani 1 1 d . . . H44 H 0.7277 0.3279 0.1014 0.022 Uiso 1 1 calc R . . C45 C 0.5799(3) 0.3007(3) 0.10154(19) 0.0223(7) Uani 1 1 d . . . H45 H 0.6169 0.2310 0.1010 0.027 Uiso 1 1 calc R . . C46 C 0.4601(3) 0.3440(3) 0.10267(19) 0.0217(7) Uani 1 1 d . . . H46 H 0.4152 0.3032 0.1044 0.026 Uiso 1 1 calc R . . C47 C 0.4054(3) 0.4468(2) 0.10127(17) 0.0168(6) Uani 1 1 d . . . H47 H 0.3233 0.4772 0.1016 0.020 Uiso 1 1 calc R . . C48 C 0.4733(3) 0.5041(2) 0.09931(16) 0.0131(5) Uani 1 1 d . . . C49 C 0.3900(3) 0.9877(2) 0.13771(17) 0.0127(5) Uani 1 1 d . . . C50 C 0.5074(3) 0.9655(2) 0.12524(18) 0.0158(6) Uani 1 1 d . . . H50 H 0.5622 0.8985 0.1523 0.019 Uiso 1 1 calc R . . C51 C 0.5432(3) 1.0440(2) 0.07188(19) 0.0186(6) Uani 1 1 d . . . H51 H 0.6233 1.0306 0.0619 0.022 Uiso 1 1 calc R . . C52 C 0.4624(3) 1.1417(2) 0.03329(18) 0.0187(6) Uani 1 1 d . . . H52 H 0.4879 1.1949 -0.0026 0.022 Uiso 1 1 calc R . . C53 C 0.3450(3) 1.1628(2) 0.04635(17) 0.0167(6) Uani 1 1 d . . . H53 H 0.2907 1.2302 0.0196 0.020 Uiso 1 1 calc R . . C54 C 0.3060(2) 1.0852(2) 0.09887(16) 0.0123(5) Uani 1 1 d . . . C55 C 0.1812(3) 1.1045(2) 0.11259(16) 0.0133(5) Uani 1 1 d . . . C56 C 0.1041(3) 1.1983(2) 0.12243(17) 0.0163(6) Uani 1 1 d . . . H56 H 0.1320 1.2517 0.1195 0.020 Uiso 1 1 calc R . . C57 C -0.0122(3) 1.2137(3) 0.13636(18) 0.0199(6) Uani 1 1 d . . . H57 H -0.0633 1.2774 0.1431 0.024 Uiso 1 1 calc R . . C58 C -0.0544(3) 1.1363(3) 0.14059(19) 0.0214(6) Uani 1 1 d . . . H58 H -0.1337 1.1466 0.1517 0.026 Uiso 1 1 calc R . . C59 C 0.0192(3) 1.0438(2) 0.12866(17) 0.0165(6) Uani 1 1 d . . . H59 H -0.0094 0.9915 0.1298 0.020 Uiso 1 1 calc R . . C60 C 0.1351(2) 1.0300(2) 0.11516(16) 0.0126(5) Uani 1 1 d . . . B1 B 0.1228(4) 0.4177(3) 0.1938(3) 0.0273(8) Uani 1 1 d . . . F1 F 0.1102(3) 0.4496(3) 0.25788(19) 0.0781(10) Uani 1 1 d . . . F2 F 0.12363(19) 0.50000(18) 0.12518(16) 0.0426(6) Uani 1 1 d . . . F3 F 0.03438(18) 0.38471(16) 0.18959(14) 0.0339(5) Uani 1 1 d . . . F4 F 0.2277(2) 0.33352(18) 0.19918(17) 0.0502(7) Uani 1 1 d . . . C90 C 0.4146(4) 0.2752(4) 0.3875(3) 0.0405(10) Uani 1 1 d . . . C91 C 0.4005(4) 0.3525(3) 0.3077(3) 0.0410(10) Uani 1 1 d . . . H91A H 0.3720 0.4233 0.3112 0.061 Uiso 1 1 calc R . . H91B H 0.3447 0.3464 0.2775 0.061 Uiso 1 1 calc R . . H91C H 0.4753 0.3397 0.2810 0.061 Uiso 1 1 calc R . . N90 N 0.4249(4) 0.2152(3) 0.4508(2) 0.0502(10) 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 0.01079(6) 0.01679(6) 0.01313(6) -0.00571(4) 0.00007(4) -0.00427(4) P1 0.0100(3) 0.0092(3) 0.0093(3) -0.0014(3) 0.0009(3) -0.0035(3) P2 0.0102(3) 0.0104(3) 0.0098(3) -0.0022(3) 0.0013(3) -0.0029(3) P3 0.0110(3) 0.0086(3) 0.0103(3) -0.0008(3) 0.0006(3) -0.0033(3) P4 0.0110(3) 0.0134(3) 0.0124(3) -0.0041(3) -0.0008(3) -0.0038(3) P5 0.0099(3) 0.0165(4) 0.0098(3) -0.0033(3) 0.0008(3) -0.0051(3) N1 0.0117(11) 0.0087(11) 0.0113(11) -0.0032(9) 0.0022(9) -0.0026(9) N2 0.0117(11) 0.0097(11) 0.0135(11) -0.0029(9) 0.0026(9) -0.0036(9) N3 0.0141(12) 0.0122(11) 0.0124(11) -0.0025(9) 0.0029(9) -0.0054(10) O1 0.0100(9) 0.0126(9) 0.0091(9) -0.0006(7) 0.0002(7) -0.0053(8) O2 0.0102(9) 0.0122(9) 0.0098(9) -0.0008(7) 0.0000(7) -0.0047(8) O3 0.0093(9) 0.0153(10) 0.0112(9) -0.0032(8) 0.0011(7) -0.0032(8) O4 0.0128(9) 0.0116(9) 0.0113(9) -0.0035(8) -0.0001(7) -0.0015(8) O5 0.0138(10) 0.0116(9) 0.0098(9) 0.0009(8) -0.0013(7) -0.0062(8) O6 0.0128(9) 0.0083(9) 0.0102(9) -0.0010(7) -0.0010(7) -0.0030(8) C1 0.0120(13) 0.0149(13) 0.0096(12) -0.0004(11) -0.0005(10) -0.0068(11) C2 0.0170(14) 0.0163(14) 0.0115(13) -0.0020(11) -0.0001(11) -0.0053(12) C3 0.0132(14) 0.0233(16) 0.0171(15) -0.0054(12) -0.0004(11) -0.0034(12) C4 0.0145(14) 0.0245(16) 0.0189(15) -0.0034(13) -0.0009(12) -0.0088(13) C5 0.0152(14) 0.0186(15) 0.0174(14) -0.0057(12) -0.0001(11) -0.0067(12) C6 0.0116(13) 0.0151(14) 0.0118(13) -0.0007(11) 0.0006(10) -0.0043(11) C7 0.0145(14) 0.0130(13) 0.0174(14) -0.0051(11) 0.0000(11) -0.0045(11) C8 0.0164(14) 0.0206(15) 0.0155(14) -0.0069(12) 0.0015(11) -0.0062(12) C9 0.0195(15) 0.0185(15) 0.0200(15) -0.0003(12) -0.0008(12) -0.0055(13) C10 0.0222(16) 0.0167(15) 0.0299(17) -0.0076(13) 0.0025(13) -0.0078(13) C11 0.0341(19) 0.0197(16) 0.0246(17) -0.0072(13) -0.0035(14) -0.0124(14) C12 0.0273(17) 0.0203(16) 0.0175(15) -0.0026(12) -0.0056(13) -0.0097(13) C13 0.0181(14) 0.0116(13) 0.0130(13) -0.0046(11) 0.0009(11) -0.0048(11) C14 0.0141(14) 0.0226(16) 0.0203(15) -0.0033(13) 0.0018(12) -0.0049(12) C15 0.0198(15) 0.0189(16) 0.0192(15) 0.0009(13) -0.0063(12) -0.0001(13) C16 0.0260(17) 0.0191(16) 0.0152(15) -0.0043(12) 0.0015(13) -0.0018(13) C17 0.0204(17) 0.042(2) 0.0175(16) -0.0066(15) 0.0047(13) -0.0014(15) C18 0.0158(15) 0.0310(18) 0.0181(15) -0.0052(14) 0.0011(12) -0.0008(13) C19 0.0151(13) 0.0128(13) 0.0112(13) -0.0008(11) -0.0012(11) -0.0078(11) C20 0.0147(14) 0.0180(14) 0.0161(14) -0.0063(12) 0.0023(11) -0.0073(12) C21 0.0205(15) 0.0229(16) 0.0120(13) -0.0060(12) 0.0016(11) -0.0097(13) C22 0.0185(15) 0.0209(15) 0.0139(14) -0.0042(12) -0.0024(11) -0.0076(12) C23 0.0133(13) 0.0141(14) 0.0133(13) -0.0024(11) 0.0006(11) -0.0053(11) C24 0.0127(13) 0.0116(13) 0.0116(13) -0.0036(10) 0.0018(10) -0.0065(11) C25 0.0087(13) 0.0184(15) 0.0154(14) 0.0008(12) -0.0025(11) -0.0034(11) C26 0.0145(14) 0.0188(15) 0.0176(14) 0.0007(12) -0.0006(11) -0.0079(12) C27 0.0154(15) 0.0185(16) 0.0331(18) 0.0008(14) 0.0000(13) -0.0087(13) C28 0.0112(14) 0.0222(16) 0.0303(18) 0.0089(14) 0.0002(13) -0.0068(13) C29 0.0113(14) 0.0356(19) 0.0170(15) 0.0053(14) 0.0016(12) -0.0039(13) C30 0.0117(14) 0.0261(16) 0.0164(14) -0.0005(13) -0.0006(11) -0.0051(12) C31 0.0123(13) 0.0198(15) 0.0088(12) -0.0030(11) 0.0014(10) -0.0042(11) C32 0.0145(14) 0.0231(16) 0.0189(15) -0.0037(13) 0.0012(12) -0.0073(12) C33 0.0159(15) 0.0304(18) 0.0260(17) -0.0061(14) 0.0010(13) -0.0055(14) C34 0.0197(16) 0.0284(18) 0.0300(18) -0.0105(15) 0.0007(14) 0.0016(14) C35 0.0277(18) 0.0224(17) 0.0315(18) -0.0106(15) 0.0004(15) -0.0044(14) C36 0.0195(15) 0.0215(16) 0.0188(15) -0.0068(13) 0.0020(12) -0.0066(13) C37 0.0092(13) 0.0119(13) 0.0147(13) 0.0005(11) 0.0001(10) -0.0018(11) C38 0.0166(14) 0.0176(15) 0.0223(15) -0.0039(12) -0.0028(12) -0.0074(12) C39 0.0180(15) 0.0183(15) 0.0286(17) 0.0003(13) -0.0024(13) -0.0094(13) C40 0.0123(14) 0.0229(16) 0.0237(16) -0.0006(13) 0.0021(12) -0.0052(12) C41 0.0134(14) 0.0178(15) 0.0175(14) -0.0024(12) 0.0011(11) -0.0007(12) C42 0.0109(13) 0.0107(13) 0.0126(13) 0.0004(10) -0.0027(10) -0.0014(11) C43 0.0154(14) 0.0164(14) 0.0115(13) -0.0043(11) 0.0012(11) -0.0043(12) C44 0.0193(15) 0.0159(14) 0.0163(14) -0.0067(12) 0.0003(12) -0.0017(12) C45 0.0302(17) 0.0143(15) 0.0210(15) -0.0067(12) -0.0011(13) -0.0053(13) C46 0.0309(18) 0.0237(16) 0.0175(15) -0.0092(13) 0.0019(13) -0.0158(14) C47 0.0169(14) 0.0213(15) 0.0140(14) -0.0064(12) 0.0009(11) -0.0084(12) C48 0.0159(14) 0.0123(13) 0.0091(12) -0.0030(10) 0.0001(10) -0.0033(11) C49 0.0158(14) 0.0129(13) 0.0116(13) -0.0042(11) 0.0020(11) -0.0078(11) C50 0.0145(14) 0.0150(14) 0.0181(14) -0.0058(12) 0.0004(11) -0.0052(11) C51 0.0170(15) 0.0229(16) 0.0209(15) -0.0103(13) 0.0056(12) -0.0113(13) C52 0.0260(16) 0.0171(15) 0.0170(14) -0.0049(12) 0.0041(12) -0.0139(13) C53 0.0231(15) 0.0130(14) 0.0141(14) -0.0032(11) 0.0017(12) -0.0082(12) C54 0.0152(14) 0.0114(13) 0.0118(13) -0.0055(11) 0.0013(11) -0.0051(11) C55 0.0154(14) 0.0118(13) 0.0095(12) -0.0014(10) -0.0008(10) -0.0032(11) C56 0.0196(15) 0.0127(14) 0.0133(13) -0.0029(11) -0.0013(11) -0.0033(12) C57 0.0170(15) 0.0175(15) 0.0173(14) -0.0050(12) 0.0006(12) 0.0016(12) C58 0.0134(14) 0.0237(16) 0.0194(15) -0.0020(13) 0.0038(12) -0.0043(12) C59 0.0149(14) 0.0150(14) 0.0145(14) 0.0006(11) -0.0007(11) -0.0049(11) C60 0.0133(13) 0.0118(13) 0.0073(12) 0.0004(10) 0.0000(10) -0.0019(11) B1 0.0255(19) 0.0248(19) 0.034(2) -0.0090(17) 0.0073(16) -0.0145(16) F1 0.095(3) 0.115(3) 0.067(2) -0.063(2) 0.0161(18) -0.058(2) F2 0.0271(11) 0.0288(12) 0.0623(16) -0.0050(11) 0.0108(11) -0.0123(9) F3 0.0274(11) 0.0271(11) 0.0491(13) -0.0104(10) 0.0053(9) -0.0155(9) F4 0.0247(11) 0.0285(12) 0.0778(19) 0.0022(12) 0.0017(12) -0.0074(10) C90 0.041(2) 0.042(2) 0.051(3) -0.027(2) -0.0013(19) -0.0171(19) C91 0.043(2) 0.030(2) 0.042(2) 0.0070(17) -0.0133(19) -0.0174(18) N90 0.067(3) 0.065(3) 0.033(2) -0.0142(19) -0.0058(18) -0.039(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 P5 2.2542(7) . ? Au1 P4 2.2643(7) . ? P1 N2 1.547(2) . ? P1 N1 1.553(2) . ? P1 O2 1.5591(19) . ? P1 O1 1.5691(19) . ? P2 O4 1.547(2) . ? P2 N3 1.548(2) . ? P2 N2 1.552(2) . ? P2 O3 1.561(2) . ? P3 N3 1.544(2) . ? P3 N1 1.548(2) . ? P3 O5 1.560(2) . ? P3 O6 1.5625(19) . ? P4 C7 1.772(3) . ? P4 C13 1.778(3) . ? P4 C6 1.791(3) . ? P5 C31 1.775(3) . ? P5 C25 1.781(3) . ? P5 C24 1.783(3) . ? O1 C1 1.383(3) . ? O2 C19 1.382(3) . ? O3 C37 1.380(3) . ? O4 C48 1.387(3) . ? O5 C49 1.383(3) . ? O6 C60 1.383(3) . ? C1 C2 1.357(4) . ? C1 C6 1.366(4) . ? C2 C3 1.363(4) . ? C3 C4 1.359(4) . ? C4 C5 1.358(4) . ? C5 C6 1.375(4) . ? C7 C12 1.371(4) . ? C7 C8 1.372(4) . ? C8 C9 1.354(4) . ? C9 C10 1.356(5) . ? C10 C11 1.361(5) . ? C11 C12 1.364(4) . ? C13 C18 1.366(4) . ? C13 C14 1.371(4) . ? C14 C15 1.362(4) . ? C15 C16 1.349(5) . ? C16 C17 1.358(5) . ? C17 C18 1.362(4) . ? C19 C20 1.352(4) . ? C19 C24 1.371(4) . ? C20 C21 1.369(4) . ? C21 C22 1.357(4) . ? C22 C23 1.362(4) . ? C23 C24 1.374(4) . ? C25 C26 1.368(4) . ? C25 C30 1.373(4) . ? C26 C27 1.371(4) . ? C27 C28 1.357(5) . ? C28 C29 1.360(5) . ? C29 C30 1.359(5) . ? C31 C36 1.364(4) . ? C31 C32 1.365(4) . ? C32 C33 1.359(4) . ? C33 C34 1.364(5) . ? C34 C35 1.357(5) . ? C35 C36 1.360(5) . ? C37 C38 1.357(4) . ? C37 C42 1.364(4) . ? C38 C39 1.357(4) . ? C39 C40 1.361(5) . ? C40 C41 1.353(4) . ? C41 C42 1.379(4) . ? C42 C43 1.455(4) . ? C43 C48 1.362(4) . ? C43 C44 1.374(4) . ? C44 C45 1.352(4) . ? C45 C46 1.358(5) . ? C46 C47 1.360(4) . ? C47 C48 1.356(4) . ? C49 C50 1.354(4) . ? C49 C54 1.373(4) . ? C50 C51 1.364(4) . ? C51 C52 1.357(4) . ? C52 C53 1.357(4) . ? C53 C54 1.371(4) . ? C54 C55 1.448(4) . ? C55 C60 1.364(4) . ? C55 C56 1.375(4) . ? C56 C57 1.357(4) . ? C57 C58 1.363(5) . ? C58 C59 1.363(4) . ? C59 C60 1.356(4) . ? B1 F1 1.336(5) . ? B1 F3 1.349(4) . ? B1 F2 1.361(5) . ? B1 F4 1.374(5) . ? C90 N90 1.130(6) . ? C90 C91 1.433(6) . ? 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 P5 Au1 P4 171.99(3) . . ? N2 P1 N1 117.50(13) . . ? N2 P1 O2 111.07(12) . . ? N1 P1 O2 110.82(12) . . ? N2 P1 O1 110.49(12) . . ? N1 P1 O1 109.29(12) . . ? O2 P1 O1 95.45(10) . . ? O4 P2 N3 105.22(12) . . ? O4 P2 N2 111.71(12) . . ? N3 P2 N2 117.81(13) . . ? O4 P2 O3 103.71(11) . . ? N3 P2 O3 112.80(12) . . ? N2 P2 O3 104.84(12) . . ? N3 P3 N1 118.37(13) . . ? N3 P3 O5 112.01(12) . . ? N1 P3 O5 105.48(12) . . ? N3 P3 O6 105.98(12) . . ? N1 P3 O6 110.86(12) . . ? O5 P3 O6 103.16(10) . . ? C7 P4 C13 107.53(14) . . ? C7 P4 C6 105.62(14) . . ? C13 P4 C6 103.79(13) . . ? C7 P4 Au1 114.37(10) . . ? C13 P4 Au1 109.46(10) . . ? C6 P4 Au1 115.30(10) . . ? C31 P5 C25 107.60(14) . . ? C31 P5 C24 104.74(13) . . ? C25 P5 C24 105.60(14) . . ? C31 P5 Au1 115.99(10) . . ? C25 P5 Au1 110.64(10) . . ? C24 P5 Au1 111.59(9) . . ? P3 N1 P1 121.94(15) . . ? P1 N2 P2 121.79(15) . . ? P3 N3 P2 121.21(15) . . ? C1 O1 P1 114.48(17) . . ? C19 O2 P1 119.04(17) . . ? C37 O3 P2 121.34(18) . . ? C48 O4 P2 119.96(17) . . ? C49 O5 P3 119.01(17) . . ? C60 O6 P3 116.91(17) . . ? C2 C1 C6 122.2(3) . . ? C2 C1 O1 117.9(3) . . ? C6 C1 O1 119.9(2) . . ? C1 C2 C3 119.4(3) . . ? C4 C3 C2 119.6(3) . . ? C5 C4 C3 120.5(3) . . ? C4 C5 C6 120.9(3) . . ? C1 C6 C5 117.3(3) . . ? C1 C6 P4 123.5(2) . . ? C5 C6 P4 118.8(2) . . ? C12 C7 C8 119.7(3) . . ? C12 C7 P4 122.1(2) . . ? C8 C7 P4 118.2(2) . . ? C9 C8 C7 120.0(3) . . ? C8 C9 C10 120.1(3) . . ? C9 C10 C11 120.5(3) . . ? C10 C11 C12 119.9(3) . . ? C11 C12 C7 119.7(3) . . ? C18 C13 C14 118.7(3) . . ? C18 C13 P4 118.2(2) . . ? C14 C13 P4 123.0(2) . . ? C15 C14 C13 120.4(3) . . ? C16 C15 C14 120.3(3) . . ? C15 C16 C17 120.0(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C13 120.4(3) . . ? C20 C19 C24 122.5(3) . . ? C20 C19 O2 120.9(3) . . ? C24 C19 O2 116.6(2) . . ? C19 C20 C21 118.4(3) . . ? C22 C21 C20 120.6(3) . . ? C21 C22 C23 120.2(3) . . ? C22 C23 C24 120.5(3) . . ? C19 C24 C23 117.8(3) . . ? C19 C24 P5 119.8(2) . . ? C23 C24 P5 122.4(2) . . ? C26 C25 C30 120.1(3) . . ? C26 C25 P5 121.8(2) . . ? C30 C25 P5 118.1(2) . . ? C25 C26 C27 119.6(3) . . ? C28 C27 C26 119.9(3) . . ? C27 C28 C29 120.5(3) . . ? C30 C29 C28 120.2(3) . . ? C29 C30 C25 119.6(3) . . ? C36 C31 C32 119.9(3) . . ? C36 C31 P5 118.8(2) . . ? C32 C31 P5 121.2(2) . . ? C33 C32 C31 120.2(3) . . ? C32 C33 C34 119.6(3) . . ? C35 C34 C33 120.3(3) . . ? C34 C35 C36 120.2(3) . . ? C35 C36 C31 119.8(3) . . ? C38 C37 C42 122.9(3) . . ? C38 C37 O3 117.3(3) . . ? C42 C37 O3 119.4(3) . . ? C37 C38 C39 118.9(3) . . ? C38 C39 C40 119.9(3) . . ? C41 C40 C39 120.5(3) . . ? C40 C41 C42 120.9(3) . . ? C37 C42 C41 116.8(3) . . ? C37 C42 C43 121.3(3) . . ? C41 C42 C43 121.6(3) . . ? C48 C43 C44 116.7(3) . . ? C48 C43 C42 122.5(3) . . ? C44 C43 C42 120.7(3) . . ? C45 C44 C43 121.3(3) . . ? C44 C45 C46 120.1(3) . . ? C45 C46 C47 120.2(3) . . ? C48 C47 C46 118.5(3) . . ? C47 C48 C43 123.1(3) . . ? C47 C48 O4 117.7(3) . . ? C43 C48 O4 119.1(3) . . ? C50 C49 C54 122.9(3) . . ? C50 C49 O5 118.2(3) . . ? C54 C49 O5 118.8(3) . . ? C49 C50 C51 118.2(3) . . ? C52 C51 C50 120.3(3) . . ? C53 C52 C51 120.8(3) . . ? C52 C53 C54 120.3(3) . . ? C53 C54 C49 117.5(3) . . ? C53 C54 C55 121.6(3) . . ? C49 C54 C55 120.9(3) . . ? C60 C55 C56 117.3(3) . . ? C60 C55 C54 120.9(3) . . ? C56 C55 C54 121.9(3) . . ? C57 C56 C55 120.7(3) . . ? C56 C57 C58 120.3(3) . . ? C57 C58 C59 120.3(3) . . ? C60 C59 C58 118.3(3) . . ? C59 C60 C55 123.1(3) . . ? C59 C60 O6 118.0(3) . . ? C55 C60 O6 118.8(2) . . ? F1 B1 F3 110.8(3) . . ? F1 B1 F2 109.4(3) . . ? F3 B1 F2 109.9(3) . . ? F1 B1 F4 110.5(4) . . ? F3 B1 F4 107.8(3) . . ? F2 B1 F4 108.4(3) . . ? N90 C90 C91 179.2(5) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.866 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.101 #===END