# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbpa130723 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H39 N2 P2, C F3 O3 S' _chemical_formula_sum 'C20 H39 F3 N2 O3 P2 S' _chemical_formula_weight 506.53 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 11.9434(18) _cell_length_b 11.9397(18) _cell_length_c 20.730(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.356(3) _cell_angle_gamma 90.00 _cell_volume 2951.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2691 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 25.60 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.257 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9385 _exptl_absorpt_correction_T_max 0.9747 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator triumph _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20827 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.14 _reflns_number_total 7188 _reflns_number_gt 4281 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0887P)^2^+2.3197P] 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 7188 _refine_ls_number_parameters 292 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2026 _refine_ls_wR_factor_gt 0.1835 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6853(3) 0.1823(3) 0.82283(17) 0.0258(7) Uani 1 1 d . A . H1 H 0.6643 0.1684 0.7786 0.031 Uiso 1 1 calc R . . C2 C 0.6933(3) 0.2549(3) 0.91994(17) 0.0337(9) Uani 1 1 d . A . H2 H 0.6780 0.3009 0.9558 0.040 Uiso 1 1 calc R . . C3 C 0.7712(3) 0.1754(3) 0.91892(18) 0.0341(9) Uani 1 1 d . A . H3 H 0.8216 0.1545 0.9540 0.041 Uiso 1 1 calc R . . C4 C 0.5808(3) 0.4841(3) 0.83757(19) 0.0351(9) Uani 1 1 d . . . C5 C 0.6965(4) 0.4850(4) 0.8096(2) 0.0540(12) Uani 1 1 d . . . H5A H 0.6917 0.4501 0.7668 0.081 Uiso 1 1 calc R . . H5B H 0.7496 0.4431 0.8383 0.081 Uiso 1 1 calc R . . H5C H 0.7225 0.5625 0.8059 0.081 Uiso 1 1 calc R . . C6 C 0.5013(4) 0.5601(4) 0.7963(2) 0.0529(12) Uani 1 1 d . . . H6A H 0.5344 0.6350 0.7936 0.079 Uiso 1 1 calc R . . H6B H 0.4291 0.5654 0.8163 0.079 Uiso 1 1 calc R . . H6C H 0.4897 0.5285 0.7528 0.079 Uiso 1 1 calc R . . C7 C 0.5912(4) 0.5323(4) 0.9070(2) 0.0538(12) Uani 1 1 d . . . H7A H 0.6307 0.6042 0.9068 0.081 Uiso 1 1 calc R . . H7B H 0.6333 0.4798 0.9355 0.081 Uiso 1 1 calc R . . H7C H 0.5162 0.5434 0.9227 0.081 Uiso 1 1 calc R . . C8 C 0.4099(3) 0.3050(3) 0.8791(2) 0.0353(9) Uani 1 1 d . . . C9 C 0.3728(8) 0.1860(9) 0.8550(4) 0.0499(11) Uani 0.55 1 d P A 1 H9A H 0.4385 0.1367 0.8551 0.075 Uiso 0.55 1 calc PR A 1 H9B H 0.3384 0.1914 0.8110 0.075 Uiso 0.55 1 calc PR A 1 H9C H 0.3183 0.1551 0.8837 0.075 Uiso 0.55 1 calc PR A 1 C10 C 0.3078(9) 0.3823(9) 0.8611(5) 0.0499(11) Uani 0.55 1 d P A 1 H10A H 0.2399 0.3497 0.8777 0.075 Uiso 0.55 1 calc PR A 1 H10B H 0.2983 0.3893 0.8140 0.075 Uiso 0.55 1 calc PR A 1 H10C H 0.3210 0.4565 0.8803 0.075 Uiso 0.55 1 calc PR A 1 C11 C 0.4331(8) 0.3031(8) 0.9499(5) 0.0499(11) Uani 0.55 1 d P A 1 H11A H 0.3629 0.2914 0.9712 0.075 Uiso 0.55 1 calc PR A 1 H11B H 0.4664 0.3747 0.9640 0.075 Uiso 0.55 1 calc PR A 1 H11C H 0.4854 0.2421 0.9614 0.075 Uiso 0.55 1 calc PR A 1 C9B C 0.4029(10) 0.1774(11) 0.8816(6) 0.0499(11) Uani 0.45 1 d P A 2 H9D H 0.4672 0.1480 0.9079 0.075 Uiso 0.45 1 calc PR A 2 H9E H 0.4036 0.1471 0.8377 0.075 Uiso 0.45 1 calc PR A 2 H9F H 0.3332 0.1552 0.9009 0.075 Uiso 0.45 1 calc PR A 2 C10B C 0.3062(12) 0.3562(11) 0.8430(6) 0.0499(11) Uani 0.45 1 d P A 2 H10D H 0.2391 0.3374 0.8658 0.075 Uiso 0.45 1 calc PR A 2 H10E H 0.2989 0.3261 0.7990 0.075 Uiso 0.45 1 calc PR A 2 H10F H 0.3145 0.4378 0.8413 0.075 Uiso 0.45 1 calc PR A 2 C11B C 0.4171(10) 0.3517(10) 0.9495(6) 0.0499(11) Uani 0.45 1 d P A 2 H11D H 0.3579 0.3179 0.9739 0.075 Uiso 0.45 1 calc PR A 2 H11E H 0.4075 0.4332 0.9485 0.075 Uiso 0.45 1 calc PR A 2 H11F H 0.4905 0.3333 0.9705 0.075 Uiso 0.45 1 calc PR A 2 C12 C 0.9850(3) 0.0716(4) 0.82632(19) 0.0412(10) Uani 1 1 d . . . C13 C 0.9783(4) 0.1899(5) 0.7982(3) 0.0794(19) Uani 1 1 d . . . H13A H 0.9368 0.2383 0.8266 0.119 Uiso 1 1 calc R . . H13B H 0.9396 0.1877 0.7552 0.119 Uiso 1 1 calc R . . H13C H 1.0542 0.2195 0.7948 0.119 Uiso 1 1 calc R . . C14 C 1.0521(4) -0.0037(7) 0.7832(3) 0.089(2) Uani 1 1 d . . . H14A H 1.1286 0.0254 0.7816 0.134 Uiso 1 1 calc R . . H14B H 1.0162 -0.0050 0.7395 0.134 Uiso 1 1 calc R . . H14C H 1.0547 -0.0799 0.8009 0.134 Uiso 1 1 calc R . . C15 C 1.0471(4) 0.0784(5) 0.8929(2) 0.0606(14) Uani 1 1 d . . . H15A H 1.0593 0.0026 0.9101 0.091 Uiso 1 1 calc R . . H15B H 1.0023 0.1215 0.9222 0.091 Uiso 1 1 calc R . . H15C H 1.1197 0.1153 0.8889 0.091 Uiso 1 1 calc R . . C16 C 0.8155(3) -0.1010(3) 0.8774(2) 0.0376(9) Uani 1 1 d . . . C17 C 0.8714(5) -0.2032(4) 0.8488(3) 0.0696(16) Uani 1 1 d . . . H17A H 0.8473 -0.2710 0.8707 0.104 Uiso 1 1 calc R . . H17B H 0.9531 -0.1958 0.8548 0.104 Uiso 1 1 calc R . . H17C H 0.8498 -0.2083 0.8025 0.104 Uiso 1 1 calc R . . C18 C 0.8557(5) -0.0920(5) 0.9484(2) 0.0684(16) Uani 1 1 d . . . H18A H 0.8169 -0.0299 0.9685 0.103 Uiso 1 1 calc R . . H18B H 0.9368 -0.0783 0.9518 0.103 Uiso 1 1 calc R . . H18C H 0.8393 -0.1621 0.9707 0.103 Uiso 1 1 calc R . . C19 C 0.6889(4) -0.1186(5) 0.8727(3) 0.0719(17) Uani 1 1 d . . . H19A H 0.6626 -0.1257 0.8272 0.108 Uiso 1 1 calc R . . H19B H 0.6521 -0.0544 0.8919 0.108 Uiso 1 1 calc R . . H19C H 0.6706 -0.1870 0.8960 0.108 Uiso 1 1 calc R . . C20 C 0.6500(4) 0.1525(4) 0.1056(2) 0.0443(10) Uani 1 1 d . . . N1 N 0.6383(2) 0.2584(3) 0.85874(14) 0.0287(7) Uani 1 1 d . . . N2 N 0.7659(2) 0.1276(3) 0.85684(14) 0.0275(7) Uani 1 1 d . . . O1 O 0.8402(2) 0.2174(3) 0.07166(16) 0.0555(9) Uani 1 1 d . . . O2 O 0.7677(3) 0.2957(3) 0.16919(15) 0.0651(10) Uani 1 1 d . . . O3 O 0.6867(3) 0.3486(2) 0.06455(14) 0.0487(8) Uani 1 1 d . . . F1 F 0.6946(3) 0.0665(3) 0.13944(17) 0.0838(10) Uani 1 1 d . . . F2 F 0.6192(3) 0.1114(3) 0.04795(15) 0.0861(11) Uani 1 1 d . . . F3 F 0.5594(3) 0.1802(3) 0.13431(19) 0.0955(12) Uani 1 1 d . . . P1 P 0.52432(8) 0.34117(8) 0.82449(4) 0.0273(2) Uani 1 1 d . A . P2 P 0.83935(8) 0.01648(9) 0.82023(5) 0.0299(2) Uani 1 1 d . A . S1 S 0.74798(8) 0.26655(9) 0.10294(5) 0.0361(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0296(18) 0.0237(18) 0.0239(17) -0.0009(14) -0.0011(14) 0.0022(14) C2 0.044(2) 0.037(2) 0.0191(17) -0.0058(16) -0.0018(15) 0.0053(17) C3 0.040(2) 0.040(2) 0.0225(18) -0.0037(17) -0.0034(15) 0.0023(17) C4 0.040(2) 0.029(2) 0.037(2) 0.0011(17) 0.0050(17) 0.0003(16) C5 0.049(3) 0.048(3) 0.067(3) 0.003(2) 0.018(2) -0.007(2) C6 0.062(3) 0.035(2) 0.061(3) 0.011(2) 0.003(2) 0.011(2) C7 0.077(3) 0.035(3) 0.049(3) -0.008(2) 0.006(2) -0.008(2) C8 0.031(2) 0.036(2) 0.040(2) -0.0056(18) 0.0075(17) -0.0022(16) C9 0.047(2) 0.053(3) 0.050(3) -0.008(3) 0.0138(19) -0.005(2) C10 0.047(2) 0.053(3) 0.050(3) -0.008(3) 0.0138(19) -0.005(2) C11 0.047(2) 0.053(3) 0.050(3) -0.008(3) 0.0138(19) -0.005(2) C9B 0.047(2) 0.053(3) 0.050(3) -0.008(3) 0.0138(19) -0.005(2) C10B 0.047(2) 0.053(3) 0.050(3) -0.008(3) 0.0138(19) -0.005(2) C11B 0.047(2) 0.053(3) 0.050(3) -0.008(3) 0.0138(19) -0.005(2) C12 0.029(2) 0.062(3) 0.034(2) 0.011(2) 0.0072(16) -0.0014(19) C13 0.046(3) 0.102(5) 0.090(4) 0.043(4) 0.001(3) -0.022(3) C14 0.043(3) 0.152(7) 0.074(4) -0.025(4) 0.020(3) 0.020(4) C15 0.029(2) 0.095(4) 0.058(3) 0.002(3) -0.004(2) -0.012(2) C16 0.035(2) 0.030(2) 0.047(2) 0.0017(18) -0.0012(18) -0.0003(16) C17 0.087(4) 0.039(3) 0.082(4) -0.002(3) 0.000(3) 0.018(3) C18 0.108(5) 0.056(3) 0.040(3) 0.018(2) -0.001(3) -0.011(3) C19 0.046(3) 0.067(4) 0.102(4) 0.035(3) -0.001(3) -0.010(3) C20 0.045(2) 0.046(3) 0.042(2) 0.001(2) 0.002(2) -0.007(2) N1 0.0343(16) 0.0292(17) 0.0224(15) -0.0044(13) 0.0005(12) 0.0033(13) N2 0.0300(16) 0.0270(16) 0.0255(15) -0.0036(13) 0.0005(12) 0.0008(12) O1 0.0347(16) 0.068(2) 0.064(2) -0.0042(18) 0.0095(15) 0.0020(15) O2 0.081(2) 0.077(3) 0.0355(17) -0.0121(17) -0.0155(17) -0.006(2) O3 0.066(2) 0.0372(17) 0.0423(17) -0.0003(14) -0.0022(15) 0.0075(15) F1 0.112(3) 0.0526(19) 0.086(2) 0.0298(17) -0.004(2) -0.0111(18) F2 0.120(3) 0.078(2) 0.0577(19) -0.0104(17) -0.0143(18) -0.047(2) F3 0.0578(19) 0.109(3) 0.124(3) -0.008(2) 0.041(2) -0.0168(19) P1 0.0307(5) 0.0293(5) 0.0215(4) -0.0026(4) -0.0012(4) 0.0047(4) P2 0.0269(5) 0.0361(5) 0.0265(5) -0.0034(4) 0.0000(4) 0.0072(4) S1 0.0372(5) 0.0393(6) 0.0311(5) -0.0030(4) -0.0029(4) -0.0001(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.320(4) . ? C1 N2 1.331(4) . ? C1 H1 0.9500 . ? C2 C3 1.330(5) . ? C2 N1 1.395(4) . ? C2 H2 0.9500 . ? C3 N2 1.406(4) . ? C3 H3 0.9500 . ? C4 C5 1.530(6) . ? C4 C6 1.537(6) . ? C4 C7 1.549(6) . ? C4 P1 1.849(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C11 1.478(11) . ? C8 C9B 1.527(13) . ? C8 C10B 1.536(15) . ? C8 C10 1.557(12) . ? C8 C11B 1.561(13) . ? C8 C9 1.562(11) . ? C8 P1 1.875(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C9B H9D 0.9800 . ? C9B H9E 0.9800 . ? C9B H9F 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? C12 C14 1.528(7) . ? C12 C13 1.528(7) . ? C12 C15 1.530(6) . ? C12 P2 1.857(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C19 1.524(6) . ? C16 C17 1.527(6) . ? C16 C18 1.527(6) . ? C16 P2 1.868(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 F3 1.307(5) . ? C20 F2 1.324(5) . ? C20 F1 1.336(5) . ? C20 S1 1.799(4) . ? N1 P1 1.795(3) . ? N2 P2 1.784(3) . ? O1 S1 1.436(3) . ? O2 S1 1.423(3) . ? O3 S1 1.435(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 N1 C1 N2 110.9(3) . . ? N1 C1 H1 124.6 . . ? N2 C1 H1 124.6 . . ? C3 C2 N1 107.4(3) . . ? C3 C2 H2 126.3 . . ? N1 C2 H2 126.3 . . ? C2 C3 N2 108.1(3) . . ? C2 C3 H3 126.0 . . ? N2 C3 H3 126.0 . . ? C5 C4 C6 109.1(4) . . ? C5 C4 C7 108.9(4) . . ? C6 C4 C7 108.1(4) . . ? C5 C4 P1 106.3(3) . . ? C6 C4 P1 104.8(3) . . ? C7 C4 P1 119.2(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C8 C9B 87.6(6) . . ? C11 C8 C10B 126.1(6) . . ? C9B C8 C10B 111.7(7) . . ? C11 C8 C10 110.2(5) . . ? C9B C8 C10 123.7(7) . . ? C9B C8 C11B 108.9(7) . . ? C10B C8 C11B 108.2(6) . . ? C10 C8 C11B 90.7(6) . . ? C11 C8 C9 109.7(6) . . ? C10B C8 C9 90.0(6) . . ? C10 C8 C9 105.0(6) . . ? C11B C8 C9 128.6(6) . . ? C11 C8 P1 120.1(4) . . ? C9B C8 P1 107.1(5) . . ? C10B C8 P1 102.1(5) . . ? C10 C8 P1 107.9(5) . . ? C11B C8 P1 118.7(5) . . ? C9 C8 P1 102.7(4) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? C8 C9B H9D 109.5 . . ? C8 C9B H9E 109.5 . . ? H9D C9B H9E 109.5 . . ? C8 C9B H9F 109.5 . . ? H9D C9B H9F 109.5 . . ? H9E C9B H9F 109.5 . . ? C8 C10B H10D 109.5 . . ? C8 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C8 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? C8 C11B H11D 109.5 . . ? C8 C11B H11E 109.5 . . ? H11D C11B H11E 109.5 . . ? C8 C11B H11F 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? C14 C12 C13 109.8(5) . . ? C14 C12 C15 108.4(4) . . ? C13 C12 C15 107.9(4) . . ? C14 C12 P2 105.9(4) . . ? C13 C12 P2 105.9(3) . . ? C15 C12 P2 118.9(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C19 C16 C17 108.7(4) . . ? C19 C16 C18 109.0(4) . . ? C17 C16 C18 108.1(4) . . ? C19 C16 P2 104.6(3) . . ? C17 C16 P2 105.5(3) . . ? C18 C16 P2 120.5(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F3 C20 F2 108.1(4) . . ? F3 C20 F1 105.8(4) . . ? F2 C20 F1 105.7(4) . . ? F3 C20 S1 112.3(3) . . ? F2 C20 S1 113.5(3) . . ? F1 C20 S1 110.9(3) . . ? C1 N1 C2 107.5(3) . . ? C1 N1 P1 119.6(2) . . ? C2 N1 P1 133.0(3) . . ? C1 N2 C3 106.2(3) . . ? C1 N2 P2 119.8(2) . . ? C3 N2 P2 134.0(3) . . ? N1 P1 C4 100.88(16) . . ? N1 P1 C8 101.35(16) . . ? C4 P1 C8 113.36(18) . . ? N2 P2 C12 100.90(18) . . ? N2 P2 C16 101.05(17) . . ? C12 P2 C16 113.59(18) . . ? O2 S1 O3 114.8(2) . . ? O2 S1 O1 116.6(2) . . ? O3 S1 O1 114.1(2) . . ? O2 S1 C20 103.1(2) . . ? O3 S1 C20 102.8(2) . . ? O1 S1 C20 102.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.1(4) . . . . ? N2 C1 N1 C2 1.2(4) . . . . ? N2 C1 N1 P1 -178.4(2) . . . . ? C3 C2 N1 C1 -0.7(4) . . . . ? C3 C2 N1 P1 178.9(3) . . . . ? N1 C1 N2 C3 -1.3(4) . . . . ? N1 C1 N2 P2 177.7(2) . . . . ? C2 C3 N2 C1 0.8(4) . . . . ? C2 C3 N2 P2 -178.0(3) . . . . ? C1 N1 P1 C4 -122.7(3) . . . . ? C2 N1 P1 C4 57.8(4) . . . . ? C1 N1 P1 C8 120.5(3) . . . . ? C2 N1 P1 C8 -59.0(4) . . . . ? C5 C4 P1 N1 52.0(3) . . . . ? C6 C4 P1 N1 167.5(3) . . . . ? C7 C4 P1 N1 -71.4(3) . . . . ? C5 C4 P1 C8 159.5(3) . . . . ? C6 C4 P1 C8 -85.0(3) . . . . ? C7 C4 P1 C8 36.1(4) . . . . ? C11 C8 P1 N1 45.5(5) . . . . ? C9B C8 P1 N1 -51.8(5) . . . . ? C10B C8 P1 N1 -169.3(5) . . . . ? C10 C8 P1 N1 172.9(4) . . . . ? C11B C8 P1 N1 71.9(6) . . . . ? C9 C8 P1 N1 -76.5(4) . . . . ? C11 C8 P1 C4 -61.7(5) . . . . ? C9B C8 P1 C4 -159.1(5) . . . . ? C10B C8 P1 C4 83.4(5) . . . . ? C10 C8 P1 C4 65.7(4) . . . . ? C11B C8 P1 C4 -35.3(6) . . . . ? C9 C8 P1 C4 176.2(4) . . . . ? C1 N2 P2 C12 119.1(3) . . . . ? C3 N2 P2 C12 -62.2(4) . . . . ? C1 N2 P2 C16 -124.0(3) . . . . ? C3 N2 P2 C16 54.7(4) . . . . ? C14 C12 P2 N2 -167.6(3) . . . . ? C13 C12 P2 N2 -51.1(4) . . . . ? C15 C12 P2 N2 70.3(4) . . . . ? C14 C12 P2 C16 85.1(4) . . . . ? C13 C12 P2 C16 -158.4(3) . . . . ? C15 C12 P2 C16 -37.0(5) . . . . ? C19 C16 P2 N2 63.1(4) . . . . ? C17 C16 P2 N2 177.7(3) . . . . ? C18 C16 P2 N2 -59.8(4) . . . . ? C19 C16 P2 C12 170.3(3) . . . . ? C17 C16 P2 C12 -75.1(4) . . . . ? C18 C16 P2 C12 47.4(4) . . . . ? F3 C20 S1 O2 56.9(4) . . . . ? F2 C20 S1 O2 179.9(4) . . . . ? F1 C20 S1 O2 -61.2(4) . . . . ? F3 C20 S1 O3 -62.7(4) . . . . ? F2 C20 S1 O3 60.3(4) . . . . ? F1 C20 S1 O3 179.2(3) . . . . ? F3 C20 S1 O1 178.5(3) . . . . ? F2 C20 S1 O1 -58.4(4) . . . . ? F1 C20 S1 O1 60.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.14 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.474 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.075 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.500 188.2 42.5 2 0.000 0.500 1.000 188.2 42.2 _platon_squeeze_details ; The residual electron density was assigned to half a molecule of the tetrahydrofuran [85/4= 21 e per asymmetric unit; half a molecule of C4H8O1 would give 20 e]. ; _database_code_depnum_ccdc_archive 'CCDC 963084' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbad130228 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H38 N2 P2' _chemical_formula_sum 'C19 H38 N2 P2' _chemical_formula_weight 356.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.8815(12) _cell_length_b 12.4951(6) _cell_length_c 15.9372(8) _cell_angle_alpha 90.00 _cell_angle_beta 108.7810(10) _cell_angle_gamma 90.00 _cell_volume 4502.5(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9831 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 30.05 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.052 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.196 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9085 _exptl_absorpt_correction_T_max 0.9436 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48197 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0181 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.07 _reflns_number_total 6585 _reflns_number_gt 5390 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0475P)^2^+3.9061P] 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 6585 _refine_ls_number_parameters 220 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1160 _refine_ls_wR_factor_gt 0.1054 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.85870(6) 0.37524(9) 0.89032(9) 0.0242(3) Uani 1 1 d . . . C2 C 0.76990(6) 0.41396(11) 0.78326(11) 0.0347(3) Uani 1 1 d . . . H2 H 0.7381 0.4540 0.7448 0.042 Uiso 1 1 calc R . . C3 C 0.77431(6) 0.30705(11) 0.78913(11) 0.0359(3) Uani 1 1 d . . . H3 H 0.7461 0.2567 0.7556 0.043 Uiso 1 1 calc R . . C4 C 0.89743(7) 0.61501(11) 0.82000(10) 0.0325(3) Uani 1 1 d . . . C5 C 0.90847(8) 0.73601(13) 0.82156(14) 0.0487(4) Uani 1 1 d . . . H5A H 0.9228 0.7610 0.8831 0.073 Uiso 1 1 calc R . . H5B H 0.8715 0.7729 0.7898 0.073 Uiso 1 1 calc R . . H5C H 0.9382 0.7515 0.7927 0.073 Uiso 1 1 calc R . . C6 C 0.87671(12) 0.5786(2) 0.72321(14) 0.0683(7) Uani 1 1 d . . . H6A H 0.8389 0.6130 0.6916 0.102 Uiso 1 1 calc R . . H6B H 0.8716 0.5007 0.7206 0.102 Uiso 1 1 calc R . . H6C H 0.9063 0.5987 0.6954 0.102 Uiso 1 1 calc R . . C7 C 0.95496(8) 0.55779(15) 0.87057(16) 0.0546(5) Uani 1 1 d . . . H7A H 0.9834 0.5655 0.8382 0.082 Uiso 1 1 calc R . . H7B H 0.9469 0.4817 0.8762 0.082 Uiso 1 1 calc R . . H7C H 0.9715 0.5895 0.9297 0.082 Uiso 1 1 calc R . . C8 C 0.84595(7) 0.61727(11) 0.97647(10) 0.0320(3) Uani 1 1 d . . . C9 C 0.90483(8) 0.57863(14) 1.04042(11) 0.0456(4) Uani 1 1 d . . . H9A H 0.9372 0.6189 1.0301 0.068 Uiso 1 1 calc R . . H9B H 0.9097 0.5022 1.0307 0.068 Uiso 1 1 calc R . . H9C H 0.9054 0.5899 1.1015 0.068 Uiso 1 1 calc R . . C10 C 0.79550(9) 0.56162(18) 0.99921(14) 0.0548(5) Uani 1 1 d . . . H10A H 0.8005 0.4839 0.9978 0.082 Uiso 1 1 calc R . . H10B H 0.7576 0.5820 0.9558 0.082 Uiso 1 1 calc R . . H10C H 0.7961 0.5834 1.0586 0.082 Uiso 1 1 calc R . . C11 C 0.84032(11) 0.73867(13) 0.98646(14) 0.0589(6) Uani 1 1 d . . . H11A H 0.8408 0.7550 1.0469 0.088 Uiso 1 1 calc R . . H11B H 0.8030 0.7636 0.9440 0.088 Uiso 1 1 calc R . . H11C H 0.8735 0.7749 0.9749 0.088 Uiso 1 1 calc R . . C12 C 0.91437(7) 0.14244(11) 0.83393(12) 0.0375(3) Uani 1 1 d . . . C13 C 0.96741(9) 0.21481(17) 0.87577(17) 0.0610(6) Uani 1 1 d . . . H13A H 0.9890 0.1890 0.9355 0.092 Uiso 1 1 calc R . . H13B H 0.9537 0.2881 0.8792 0.092 Uiso 1 1 calc R . . H13C H 0.9936 0.2138 0.8395 0.092 Uiso 1 1 calc R . . C14 C 0.88799(13) 0.1722(2) 0.73557(15) 0.0756(7) Uani 1 1 d . . . H14A H 0.9163 0.1542 0.7048 0.113 Uiso 1 1 calc R . . H14B H 0.8796 0.2491 0.7301 0.113 Uiso 1 1 calc R . . H14C H 0.8512 0.1321 0.7090 0.113 Uiso 1 1 calc R . . C15 C 0.93443(11) 0.02567(15) 0.8404(2) 0.0723(7) Uani 1 1 d . . . H15A H 0.9630 0.0164 0.8085 0.109 Uiso 1 1 calc R . . H15B H 0.9001 -0.0206 0.8140 0.109 Uiso 1 1 calc R . . H15C H 0.9530 0.0063 0.9028 0.109 Uiso 1 1 calc R . . C16 C 0.87337(7) 0.14322(11) 1.00076(11) 0.0343(3) Uani 1 1 d . . . C17 C 0.88053(11) 0.02368(14) 1.02443(15) 0.0603(6) Uani 1 1 d . . . H17A H 0.9149 -0.0047 1.0110 0.090 Uiso 1 1 calc R . . H17B H 0.8449 -0.0150 0.9897 0.090 Uiso 1 1 calc R . . H17C H 0.8863 0.0146 1.0877 0.090 Uiso 1 1 calc R . . C18 C 0.92857(9) 0.20357(15) 1.05525(12) 0.0515(5) Uani 1 1 d . . . H18A H 0.9256 0.2785 1.0363 0.077 Uiso 1 1 calc R . . H18B H 0.9636 0.1710 1.0464 0.077 Uiso 1 1 calc R . . H18C H 0.9321 0.2000 1.1182 0.077 Uiso 1 1 calc R . . C19 C 0.82036(10) 0.18594(19) 1.02496(16) 0.0607(5) Uani 1 1 d . . . H19A H 0.8251 0.1676 1.0866 0.091 Uiso 1 1 calc R . . H19B H 0.7839 0.1536 0.9858 0.091 Uiso 1 1 calc R . . H19C H 0.8182 0.2639 1.0179 0.091 Uiso 1 1 calc R . . N1 N 0.82144(4) 0.45504(8) 0.84497(7) 0.0237(2) Uani 1 1 d . . . N2 N 0.82832(5) 0.28370(8) 0.85404(8) 0.0249(2) Uani 1 1 d . . . P1 P 0.830677(15) 0.59369(2) 0.85532(2) 0.02433(9) Uani 1 1 d . . . P2 P 0.849838(15) 0.14980(3) 0.87659(3) 0.02728(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0232(6) 0.0123(5) 0.0313(7) -0.0009(4) 0.0006(5) -0.0007(4) C2 0.0247(6) 0.0239(6) 0.0409(8) -0.0010(6) -0.0097(6) -0.0007(5) C3 0.0255(6) 0.0236(6) 0.0445(8) -0.0040(6) -0.0084(6) -0.0038(5) C4 0.0390(7) 0.0222(6) 0.0370(8) 0.0033(5) 0.0132(6) -0.0036(5) C5 0.0491(10) 0.0273(7) 0.0672(12) 0.0108(7) 0.0151(9) -0.0087(7) C6 0.0999(18) 0.0702(14) 0.0480(11) -0.0151(10) 0.0423(13) -0.0275(13) C7 0.0381(9) 0.0416(9) 0.0913(16) 0.0187(10) 0.0308(10) 0.0064(7) C8 0.0428(8) 0.0214(6) 0.0300(7) -0.0028(5) 0.0092(6) 0.0014(5) C9 0.0534(10) 0.0418(9) 0.0295(8) -0.0013(6) -0.0036(7) -0.0006(7) C10 0.0581(11) 0.0599(12) 0.0567(12) -0.0031(9) 0.0328(10) -0.0022(9) C11 0.0996(17) 0.0266(8) 0.0480(11) -0.0100(7) 0.0202(11) 0.0113(9) C12 0.0432(8) 0.0238(6) 0.0503(9) -0.0059(6) 0.0219(7) 0.0030(6) C13 0.0467(10) 0.0516(11) 0.0991(17) -0.0201(11) 0.0436(11) -0.0112(8) C14 0.0951(18) 0.0921(18) 0.0505(12) -0.0013(12) 0.0383(13) 0.0144(15) C15 0.0750(15) 0.0307(9) 0.128(2) -0.0082(11) 0.0553(15) 0.0135(9) C16 0.0403(8) 0.0230(6) 0.0395(8) 0.0072(5) 0.0128(6) 0.0014(5) C17 0.0823(15) 0.0291(8) 0.0655(13) 0.0189(8) 0.0181(11) 0.0038(9) C18 0.0592(11) 0.0450(9) 0.0376(9) 0.0020(7) -0.0022(8) -0.0046(8) C19 0.0697(13) 0.0600(12) 0.0673(14) 0.0091(10) 0.0432(12) 0.0080(10) N1 0.0208(5) 0.0145(4) 0.0289(6) -0.0005(4) -0.0014(4) -0.0001(3) N2 0.0211(5) 0.0138(4) 0.0330(6) -0.0023(4) -0.0009(4) -0.0020(4) P1 0.02556(16) 0.01314(14) 0.02781(17) 0.00112(11) -0.00042(12) 0.00257(11) P2 0.02556(16) 0.01305(14) 0.0387(2) -0.00236(12) 0.00409(14) -0.00247(11) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.3763(15) . ? C1 N2 1.3779(14) . ? C2 C3 1.3409(19) . ? C2 N1 1.4023(16) . ? C2 H2 0.9500 . ? C3 N2 1.3999(17) . ? C3 H3 0.9500 . ? C4 C7 1.528(2) . ? C4 C6 1.530(3) . ? C4 C5 1.534(2) . ? C4 P1 1.8728(16) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.525(2) . ? C8 C10 1.532(2) . ? C8 C11 1.536(2) . ? C8 P1 1.8693(15) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.524(2) . ? C12 C15 1.529(2) . ? C12 C14 1.535(3) . ? C12 P2 1.8762(16) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.524(2) . ? C16 C19 1.533(3) . ? C16 C17 1.537(2) . ? C16 P2 1.8769(17) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? N1 P1 1.7475(10) . ? N2 P2 1.7531(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N2 102.54(10) . . ? C3 C2 N1 106.51(11) . . ? C3 C2 H2 126.7 . . ? N1 C2 H2 126.7 . . ? C2 C3 N2 106.99(11) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? C7 C4 C6 109.68(17) . . ? C7 C4 C5 109.39(14) . . ? C6 C4 C5 107.92(15) . . ? C7 C4 P1 118.86(11) . . ? C6 C4 P1 103.33(12) . . ? C5 C4 P1 107.09(11) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C10 108.92(15) . . ? C9 C8 C11 109.64(14) . . ? C10 C8 C11 108.78(16) . . ? C9 C8 P1 118.14(11) . . ? C10 C8 P1 105.43(12) . . ? C11 C8 P1 105.57(11) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C15 109.78(17) . . ? C13 C12 C14 108.26(18) . . ? C15 C12 C14 108.42(18) . . ? C13 C12 P2 118.45(12) . . ? C15 C12 P2 107.38(12) . . ? C14 C12 P2 104.08(14) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C19 108.49(16) . . ? C18 C16 C17 109.49(15) . . ? C19 C16 C17 108.20(15) . . ? C18 C16 P2 119.31(12) . . ? C19 C16 P2 105.00(12) . . ? C17 C16 P2 105.86(12) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C1 N1 C2 112.10(10) . . ? C1 N1 P1 128.91(8) . . ? C2 N1 P1 119.00(9) . . ? C1 N2 C3 111.86(10) . . ? C1 N2 P2 128.77(9) . . ? C3 N2 P2 119.33(9) . . ? N1 P1 C8 103.32(6) . . ? N1 P1 C4 101.91(6) . . ? C8 P1 C4 112.71(7) . . ? N2 P2 C12 101.14(6) . . ? N2 P2 C16 103.09(6) . . ? C12 P2 C16 112.20(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.07(18) . . . . ? N2 C1 N1 C2 0.23(16) . . . . ? N2 C1 N1 P1 -179.88(10) . . . . ? C3 C2 N1 C1 -0.10(18) . . . . ? C3 C2 N1 P1 179.99(11) . . . . ? N1 C1 N2 C3 -0.27(16) . . . . ? N1 C1 N2 P2 177.61(10) . . . . ? C2 C3 N2 C1 0.23(19) . . . . ? C2 C3 N2 P2 -177.88(12) . . . . ? C1 N1 P1 C8 -53.44(14) . . . . ? C2 N1 P1 C8 126.46(12) . . . . ? C1 N1 P1 C4 63.66(14) . . . . ? C2 N1 P1 C4 -116.45(12) . . . . ? C9 C8 P1 N1 69.66(13) . . . . ? C10 C8 P1 N1 -52.28(12) . . . . ? C11 C8 P1 N1 -167.34(13) . . . . ? C9 C8 P1 C4 -39.56(14) . . . . ? C10 C8 P1 C4 -161.49(11) . . . . ? C11 C8 P1 C4 83.44(14) . . . . ? C7 C4 P1 N1 -58.41(14) . . . . ? C6 C4 P1 N1 63.31(13) . . . . ? C5 C4 P1 N1 177.12(11) . . . . ? C7 C4 P1 C8 51.69(15) . . . . ? C6 C4 P1 C8 173.41(12) . . . . ? C5 C4 P1 C8 -72.78(13) . . . . ? C1 N2 P2 C12 -66.01(14) . . . . ? C3 N2 P2 C12 111.74(13) . . . . ? C1 N2 P2 C16 50.17(14) . . . . ? C3 N2 P2 C16 -132.08(12) . . . . ? C13 C12 P2 N2 60.79(16) . . . . ? C15 C12 P2 N2 -174.26(14) . . . . ? C14 C12 P2 N2 -59.43(14) . . . . ? C13 C12 P2 C16 -48.46(17) . . . . ? C15 C12 P2 C16 76.49(16) . . . . ? C14 C12 P2 C16 -168.68(14) . . . . ? C18 C16 P2 N2 -67.61(14) . . . . ? C19 C16 P2 N2 54.19(12) . . . . ? C17 C16 P2 N2 168.54(12) . . . . ? C18 C16 P2 C12 40.40(15) . . . . ? C19 C16 P2 C12 162.19(12) . . . . ? C17 C16 P2 C12 -83.46(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.596 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.052 _database_code_depnum_ccdc_archive 'CCDC 963085' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbad130416 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H76 Cu2 N4 P4, 2(C F3 O3 S)' _chemical_formula_sum 'C40 H76 Cu2 F6 N4 O6 P4 S2' _chemical_formula_weight 1138.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 8.8473(5) _cell_length_b 13.1451(7) _cell_length_c 23.5989(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.3950(10) _cell_angle_gamma 90.00 _cell_volume 2736.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4917 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 28.25 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.034 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6824 _exptl_absorpt_correction_T_max 0.9501 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator triumph _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22020 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.02 _reflns_number_total 7272 _reflns_number_gt 4812 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.1155P)^2^+7.9422P] 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 7272 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1190 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2284 _refine_ls_wR_factor_gt 0.2009 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3877(4) 0.6554(3) -0.01337(16) 0.0168(8) Uani 1 1 d . . . C2 C 0.3519(5) 0.7577(4) -0.08944(18) 0.0240(9) Uani 1 1 d . . . H2 H 0.3531 0.7829 -0.1271 0.029 Uiso 1 1 calc R . . C3 C 0.2986(5) 0.8063(4) -0.04571(18) 0.0247(9) Uani 1 1 d . . . H3 H 0.2538 0.8720 -0.0465 0.030 Uiso 1 1 calc R . . C4 C 0.3549(5) 0.5200(4) -0.15982(19) 0.0254(9) Uani 1 1 d . . . C5 C 0.4357(7) 0.4459(5) -0.1975(2) 0.0430(14) Uani 1 1 d . . . H5A H 0.3602 0.4053 -0.2200 0.064 Uiso 1 1 calc R . . H5B H 0.5014 0.4007 -0.1735 0.064 Uiso 1 1 calc R . . H5C H 0.4971 0.4843 -0.2229 0.064 Uiso 1 1 calc R . . C6 C 0.2691(6) 0.6004(4) -0.1953(2) 0.0326(11) Uani 1 1 d . . . H6A H 0.3409 0.6416 -0.2151 0.049 Uiso 1 1 calc R . . H6B H 0.2136 0.6443 -0.1705 0.049 Uiso 1 1 calc R . . H6C H 0.1974 0.5674 -0.2232 0.049 Uiso 1 1 calc R . . C7 C 0.2421(6) 0.4608(5) -0.1255(2) 0.0406(13) Uani 1 1 d . . . H7A H 0.1956 0.5074 -0.0995 0.061 Uiso 1 1 calc R . . H7B H 0.2960 0.4068 -0.1036 0.061 Uiso 1 1 calc R . . H7C H 0.1630 0.4306 -0.1516 0.061 Uiso 1 1 calc R . . C8 C 0.6646(5) 0.6355(4) -0.1331(2) 0.0315(11) Uani 1 1 d . . . C9 C 0.7285(7) 0.7060(6) -0.0848(3) 0.0510(16) Uani 1 1 d . . . H9A H 0.7436 0.6670 -0.0494 0.077 Uiso 1 1 calc R . . H9B H 0.6569 0.7616 -0.0797 0.077 Uiso 1 1 calc R . . H9C H 0.8257 0.7343 -0.0945 0.077 Uiso 1 1 calc R . . C10 C 0.7808(7) 0.5528(6) -0.1428(3) 0.0533(18) Uani 1 1 d . . . H10A H 0.7392 0.5060 -0.1724 0.080 Uiso 1 1 calc R . . H10B H 0.8042 0.5151 -0.1074 0.080 Uiso 1 1 calc R . . H10C H 0.8736 0.5841 -0.1549 0.080 Uiso 1 1 calc R . . C11 C 0.6299(6) 0.6972(5) -0.1877(2) 0.0362(12) Uani 1 1 d . . . H11A H 0.7211 0.7341 -0.1970 0.054 Uiso 1 1 calc R . . H11B H 0.5485 0.7459 -0.1821 0.054 Uiso 1 1 calc R . . H11C H 0.5979 0.6512 -0.2190 0.054 Uiso 1 1 calc R . . C12 C 0.0836(5) 0.7853(4) 0.0715(2) 0.0342(11) Uani 1 1 d . . . C13 C 0.0097(7) 0.6876(6) 0.0463(3) 0.0612(11) Uani 1 1 d . . . H13A H 0.0434 0.6292 0.0698 0.092 Uiso 1 1 calc R . . H13B H 0.0394 0.6779 0.0075 0.092 Uiso 1 1 calc R . . H13C H -0.1009 0.6937 0.0456 0.092 Uiso 1 1 calc R . . C14 C 0.0193(7) 0.8748(6) 0.0354(3) 0.0612(11) Uani 1 1 d . . . H14A H -0.0914 0.8690 0.0302 0.092 Uiso 1 1 calc R . . H14B H 0.0615 0.8735 -0.0018 0.092 Uiso 1 1 calc R . . H14C H 0.0466 0.9390 0.0547 0.092 Uiso 1 1 calc R . . C15 C 0.0436(7) 0.7962(6) 0.1326(3) 0.0612(11) Uani 1 1 d . . . H15A H 0.0900 0.8583 0.1490 0.092 Uiso 1 1 calc R . . H15B H 0.0818 0.7372 0.1546 0.092 Uiso 1 1 calc R . . H15C H -0.0667 0.8003 0.1336 0.092 Uiso 1 1 calc R . . C16 C 0.4135(6) 0.8698(4) 0.09349(19) 0.0293(10) Uani 1 1 d . . . C17 C 0.5702(7) 0.8408(6) 0.0762(3) 0.0572(19) Uani 1 1 d . . . H17A H 0.5691 0.8393 0.0347 0.086 Uiso 1 1 calc R . . H17B H 0.5977 0.7734 0.0915 0.086 Uiso 1 1 calc R . . H17C H 0.6445 0.8910 0.0914 0.086 Uiso 1 1 calc R . . C18 C 0.4186(8) 0.8783(6) 0.1585(2) 0.0539(17) Uani 1 1 d . . . H18A H 0.4487 0.8127 0.1756 0.081 Uiso 1 1 calc R . . H18B H 0.3181 0.8971 0.1698 0.081 Uiso 1 1 calc R . . H18C H 0.4923 0.9305 0.1715 0.081 Uiso 1 1 calc R . . C19 C 0.3686(9) 0.9743(5) 0.0694(3) 0.0584(19) Uani 1 1 d . . . H19A H 0.4455 1.0245 0.0825 0.088 Uiso 1 1 calc R . . H19B H 0.2703 0.9941 0.0826 0.088 Uiso 1 1 calc R . . H19C H 0.3611 0.9714 0.0278 0.088 Uiso 1 1 calc R . . C20 C 0.9886(7) 0.1190(5) 0.2003(3) 0.0496(16) Uani 1 1 d . . . O1 O 0.8447(7) -0.0440(4) 0.2215(2) 0.0749(17) Uani 1 1 d . . . O2 O 0.7018(5) 0.1127(4) 0.2064(2) 0.0586(13) Uani 1 1 d . . . O3 O 0.8112(6) 0.0297(3) 0.12762(18) 0.0520(11) Uani 1 1 d . . . F1 F 1.1098(4) 0.0683(3) 0.1854(2) 0.0700(13) Uani 1 1 d . . . F2 F 0.9789(4) 0.2055(3) 0.1706(2) 0.0717(13) Uani 1 1 d . . . F3 F 1.0157(7) 0.1423(5) 0.2545(2) 0.120(2) Uani 1 1 d . . . P1 P 0.50049(13) 0.56787(9) -0.10478(4) 0.0206(2) Uani 1 1 d . . . P2 P 0.29021(13) 0.75739(9) 0.07441(5) 0.0207(2) Uani 1 1 d . . . S1 S 0.81547(17) 0.04533(11) 0.18811(6) 0.0407(3) Uani 1 1 d . . . Cu1 Cu 0.56410(7) 0.45007(5) -0.04155(2) 0.02989(19) Uani 1 1 d . . . N1 N 0.4064(4) 0.6623(3) -0.06989(14) 0.0199(7) Uani 1 1 d . . . N2 N 0.3209(4) 0.7426(3) 0.00153(14) 0.0193(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0217(18) 0.0170(19) 0.0121(17) 0.0009(15) 0.0042(14) -0.0024(15) C2 0.034(2) 0.024(2) 0.0142(19) 0.0097(17) 0.0013(16) 0.0042(18) C3 0.032(2) 0.022(2) 0.020(2) 0.0053(17) 0.0013(17) 0.0029(18) C4 0.031(2) 0.027(2) 0.019(2) -0.0036(18) 0.0033(17) 0.0023(18) C5 0.055(3) 0.043(3) 0.030(3) -0.013(2) -0.001(2) 0.015(3) C6 0.033(2) 0.039(3) 0.024(2) 0.000(2) -0.0056(19) 0.002(2) C7 0.041(3) 0.042(3) 0.038(3) 0.005(2) 0.001(2) -0.013(2) C8 0.022(2) 0.051(3) 0.021(2) 0.012(2) 0.0033(17) -0.002(2) C9 0.037(3) 0.076(5) 0.039(3) 0.003(3) -0.001(2) -0.024(3) C10 0.038(3) 0.079(5) 0.045(3) 0.025(3) 0.017(3) 0.021(3) C11 0.034(3) 0.048(3) 0.028(3) 0.017(2) 0.008(2) -0.003(2) C12 0.028(2) 0.041(3) 0.036(3) 0.012(2) 0.012(2) 0.005(2) C13 0.0369(18) 0.075(3) 0.074(3) 0.019(2) 0.0167(18) 0.0084(18) C14 0.0369(18) 0.075(3) 0.074(3) 0.019(2) 0.0167(18) 0.0084(18) C15 0.0369(18) 0.075(3) 0.074(3) 0.019(2) 0.0167(18) 0.0084(18) C16 0.040(3) 0.029(3) 0.019(2) -0.0101(19) 0.0082(18) -0.008(2) C17 0.035(3) 0.068(5) 0.069(4) -0.033(4) 0.012(3) -0.018(3) C18 0.073(4) 0.064(4) 0.023(3) -0.012(3) 0.001(3) -0.020(4) C19 0.090(5) 0.032(3) 0.052(4) 0.000(3) -0.002(4) -0.018(3) C20 0.035(3) 0.048(4) 0.064(4) -0.008(3) -0.010(3) 0.011(3) O1 0.123(5) 0.052(3) 0.053(3) 0.035(2) 0.025(3) 0.009(3) O2 0.046(2) 0.073(3) 0.059(3) 0.029(3) 0.024(2) 0.008(2) O3 0.075(3) 0.041(2) 0.037(2) 0.0028(19) -0.018(2) -0.010(2) F1 0.0372(19) 0.072(3) 0.099(3) -0.010(2) -0.003(2) 0.0218(19) F2 0.0357(18) 0.035(2) 0.144(4) 0.007(2) 0.003(2) -0.0052(16) F3 0.115(4) 0.153(6) 0.081(3) -0.073(4) -0.060(3) 0.051(4) P1 0.0258(5) 0.0247(6) 0.0119(5) 0.0032(4) 0.0049(4) 0.0032(4) P2 0.0252(5) 0.0220(6) 0.0155(5) 0.0021(4) 0.0062(4) 0.0014(4) S1 0.0481(8) 0.0403(8) 0.0339(7) 0.0180(6) 0.0048(6) -0.0046(6) Cu1 0.0345(3) 0.0352(4) 0.0204(3) 0.0063(2) 0.0046(2) 0.0038(3) N1 0.0274(18) 0.0215(19) 0.0109(15) 0.0032(14) 0.0022(13) 0.0022(14) N2 0.0272(18) 0.0191(18) 0.0119(15) 0.0034(13) 0.0027(13) 0.0004(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.349(5) . ? C1 N1 1.360(5) . ? C1 Cu1 1.923(4) 3_665 ? C2 C3 1.330(6) . ? C2 N1 1.409(6) . ? C2 H2 0.9500 . ? C3 N2 1.396(5) . ? C3 H3 0.9500 . ? C4 C6 1.516(7) . ? C4 C5 1.531(7) . ? C4 C7 1.544(7) . ? C4 P1 1.867(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C10 1.525(8) . ? C8 C11 1.534(7) . ? C8 C9 1.544(8) . ? C8 P1 1.869(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15 1.516(9) . ? C12 C14 1.537(9) . ? C12 C13 1.540(10) . ? C12 P2 1.860(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.523(8) . ? C16 C19 1.528(8) . ? C16 C18 1.535(7) . ? C16 P2 1.871(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 F3 1.321(8) . ? C20 F1 1.332(7) . ? C20 F2 1.335(8) . ? C20 S1 1.816(7) . ? O1 S1 1.427(5) . ? O2 S1 1.431(5) . ? O3 S1 1.440(4) . ? P1 N1 1.736(4) . ? P1 Cu1 2.1936(13) . ? P2 N2 1.772(3) . ? Cu1 C1 1.923(4) 3_665 ? Cu1 Cu1 2.6827(12) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 106.7(3) . . ? N2 C1 Cu1 121.1(3) . 3_665 ? N1 C1 Cu1 132.2(3) . 3_665 ? C3 C2 N1 107.8(4) . . ? C3 C2 H2 126.1 . . ? N1 C2 H2 126.1 . . ? C2 C3 N2 107.2(4) . . ? C2 C3 H3 126.4 . . ? N2 C3 H3 126.4 . . ? C6 C4 C5 111.1(4) . . ? C6 C4 C7 109.0(4) . . ? C5 C4 C7 109.4(5) . . ? C6 C4 P1 116.0(4) . . ? C5 C4 P1 106.9(3) . . ? C7 C4 P1 104.1(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C10 C8 C11 110.2(4) . . ? C10 C8 C9 109.0(5) . . ? C11 C8 C9 109.9(5) . . ? C10 C8 P1 105.4(4) . . ? C11 C8 P1 116.2(3) . . ? C9 C8 P1 105.8(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C14 110.6(5) . . ? C15 C12 C13 108.9(5) . . ? C14 C12 C13 107.2(5) . . ? C15 C12 P2 106.5(4) . . ? C14 C12 P2 119.5(4) . . ? C13 C12 P2 103.7(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C19 110.0(5) . . ? C17 C16 C18 109.1(5) . . ? C19 C16 C18 107.0(5) . . ? C17 C16 P2 105.3(4) . . ? C19 C16 P2 119.4(4) . . ? C18 C16 P2 105.7(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? F3 C20 F1 106.4(5) . . ? F3 C20 F2 108.1(6) . . ? F1 C20 F2 107.9(6) . . ? F3 C20 S1 111.4(6) . . ? F1 C20 S1 112.2(5) . . ? F2 C20 S1 110.6(4) . . ? N1 P1 C4 103.92(19) . . ? N1 P1 C8 104.1(2) . . ? C4 P1 C8 115.1(2) . . ? N1 P1 Cu1 106.81(12) . . ? C4 P1 Cu1 111.27(16) . . ? C8 P1 Cu1 114.40(16) . . ? N2 P2 C12 102.1(2) . . ? N2 P2 C16 100.97(19) . . ? C12 P2 C16 114.0(2) . . ? O1 S1 O2 116.4(3) . . ? O1 S1 O3 114.8(3) . . ? O2 S1 O3 114.9(3) . . ? O1 S1 C20 103.7(4) . . ? O2 S1 C20 103.1(3) . . ? O3 S1 C20 101.0(3) . . ? C1 Cu1 P1 177.81(13) 3_665 . ? C1 Cu1 Cu1 86.81(12) 3_665 3_665 ? P1 Cu1 Cu1 92.93(4) . 3_665 ? C1 N1 C2 108.4(3) . . ? C1 N1 P1 121.1(3) . . ? C2 N1 P1 130.2(3) . . ? C1 N2 C3 109.9(3) . . ? C1 N2 P2 116.7(3) . . ? C3 N2 P2 133.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 0.8(5) . . . . ? C6 C4 P1 N1 48.3(4) . . . . ? C5 C4 P1 N1 172.8(3) . . . . ? C7 C4 P1 N1 -71.4(4) . . . . ? C6 C4 P1 C8 -64.9(4) . . . . ? C5 C4 P1 C8 59.6(4) . . . . ? C7 C4 P1 C8 175.4(3) . . . . ? C6 C4 P1 Cu1 162.9(3) . . . . ? C5 C4 P1 Cu1 -72.6(4) . . . . ? C7 C4 P1 Cu1 43.2(4) . . . . ? C10 C8 P1 N1 158.3(4) . . . . ? C11 C8 P1 N1 -79.4(4) . . . . ? C9 C8 P1 N1 42.9(4) . . . . ? C10 C8 P1 C4 -88.7(4) . . . . ? C11 C8 P1 C4 33.7(5) . . . . ? C9 C8 P1 C4 155.9(4) . . . . ? C10 C8 P1 Cu1 42.1(4) . . . . ? C11 C8 P1 Cu1 164.4(4) . . . . ? C9 C8 P1 Cu1 -73.4(4) . . . . ? C15 C12 P2 N2 178.3(4) . . . . ? C14 C12 P2 N2 -55.7(5) . . . . ? C13 C12 P2 N2 63.5(4) . . . . ? C15 C12 P2 C16 -73.8(5) . . . . ? C14 C12 P2 C16 52.3(6) . . . . ? C13 C12 P2 C16 171.4(4) . . . . ? C17 C16 P2 N2 -54.7(4) . . . . ? C19 C16 P2 N2 69.4(5) . . . . ? C18 C16 P2 N2 -170.1(4) . . . . ? C17 C16 P2 C12 -163.3(4) . . . . ? C19 C16 P2 C12 -39.2(5) . . . . ? C18 C16 P2 C12 81.2(5) . . . . ? F3 C20 S1 O1 -60.7(5) . . . . ? F1 C20 S1 O1 58.4(6) . . . . ? F2 C20 S1 O1 179.0(5) . . . . ? F3 C20 S1 O2 61.0(5) . . . . ? F1 C20 S1 O2 -179.8(5) . . . . ? F2 C20 S1 O2 -59.2(5) . . . . ? F3 C20 S1 O3 -179.9(5) . . . . ? F1 C20 S1 O3 -60.7(5) . . . . ? F2 C20 S1 O3 59.9(5) . . . . ? N1 P1 Cu1 Cu1 0.87(14) . . . 3_665 ? C4 P1 Cu1 Cu1 -111.91(16) . . . 3_665 ? C8 P1 Cu1 Cu1 115.50(19) . . . 3_665 ? N2 C1 N1 C2 1.3(5) . . . . ? Cu1 C1 N1 C2 -179.5(3) 3_665 . . . ? N2 C1 N1 P1 175.8(3) . . . . ? Cu1 C1 N1 P1 -5.0(6) 3_665 . . . ? C3 C2 N1 C1 -1.3(5) . . . . ? C3 C2 N1 P1 -175.1(3) . . . . ? C4 P1 N1 C1 119.3(3) . . . . ? C8 P1 N1 C1 -119.8(3) . . . . ? Cu1 P1 N1 C1 1.6(4) . . . . ? C4 P1 N1 C2 -67.6(4) . . . . ? C8 P1 N1 C2 53.3(4) . . . . ? Cu1 P1 N1 C2 174.7(4) . . . . ? N1 C1 N2 C3 -0.8(5) . . . . ? Cu1 C1 N2 C3 179.8(3) 3_665 . . . ? N1 C1 N2 P2 -177.2(3) . . . . ? Cu1 C1 N2 P2 3.4(4) 3_665 . . . ? C2 C3 N2 C1 0.0(5) . . . . ? C2 C3 N2 P2 175.6(3) . . . . ? C12 P2 N2 C1 -126.0(3) . . . . ? C16 P2 N2 C1 116.4(3) . . . . ? C12 P2 N2 C3 58.7(5) . . . . ? C16 P2 N2 C3 -59.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 29.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.454 _refine_diff_density_min -1.336 _refine_diff_density_rms 0.146 _database_code_depnum_ccdc_archive 'CCDC 963086' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbad130528 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C39 H76 Cu3 F3 N4 O3 P4 S, 2(C F3 O3 S), 2(C H2 Cl2)' _chemical_formula_sum 'C43 H80 Cl4 Cu3 F9 N4 O9 P4 S3' _chemical_formula_weight 1520.59 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 16.4659(12) _cell_length_b 15.6201(13) _cell_length_c 24.952(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6417.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2157 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.15 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.574 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3128 _exptl_absorpt_coefficient_mu 1.425 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5994 _exptl_absorpt_correction_T_max 0.9194 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator triumph _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25849 _diffrn_reflns_av_R_equivalents 0.1020 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.02 _reflns_number_total 8034 _reflns_number_gt 3806 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0838P)^2^+17.5811P] 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 8034 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1819 _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2160 _refine_ls_wR_factor_gt 0.1619 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2852(5) 0.2500 0.1620(3) 0.0192(17) Uani 1 2 d S . . C2 C 0.2978(4) 0.2927(4) 0.2477(2) 0.0359(17) Uani 1 1 d . . . H2 H 0.3018 0.3286 0.2783 0.043 Uiso 1 1 calc R . . C3 C 0.1707(4) 0.4481(5) 0.1979(3) 0.0386(17) Uani 1 1 d . . . C4 C 0.1403(5) 0.5291(6) 0.1706(4) 0.062(2) Uani 1 1 d . . . H4A H 0.0831 0.5384 0.1799 0.094 Uiso 1 1 calc R . . H4B H 0.1455 0.5230 0.1317 0.094 Uiso 1 1 calc R . . H4C H 0.1726 0.5781 0.1827 0.094 Uiso 1 1 calc R . . C5 C 0.1637(5) 0.4604(7) 0.2585(3) 0.068(3) Uani 1 1 d . . . H5A H 0.1902 0.5140 0.2688 0.102 Uiso 1 1 calc R . . H5B H 0.1900 0.4124 0.2769 0.102 Uiso 1 1 calc R . . H5C H 0.1062 0.4626 0.2686 0.102 Uiso 1 1 calc R . . C6 C 0.1173(5) 0.3725(6) 0.1821(4) 0.071(3) Uani 1 1 d . . . H6A H 0.1344 0.3214 0.2019 0.107 Uiso 1 1 calc R . . H6B H 0.1226 0.3621 0.1435 0.107 Uiso 1 1 calc R . . H6C H 0.0605 0.3855 0.1906 0.107 Uiso 1 1 calc R . . C7 C 0.3552(4) 0.4924(5) 0.2029(3) 0.0311(16) Uani 1 1 d . . . C8 C 0.3298(9) 0.5859(11) 0.1917(6) 0.0474(19) Uani 0.60 1 d P A 1 H8A H 0.3770 0.6235 0.1959 0.071 Uiso 0.60 1 calc PR A 1 H8B H 0.2874 0.6030 0.2171 0.071 Uiso 0.60 1 calc PR A 1 H8C H 0.3090 0.5906 0.1550 0.071 Uiso 0.60 1 calc PR A 1 C9 C 0.3783(8) 0.4812(10) 0.2607(5) 0.0474(19) Uani 0.60 1 d P A 1 H9A H 0.4057 0.4260 0.2654 0.071 Uiso 0.60 1 calc PR A 1 H9B H 0.3293 0.4826 0.2830 0.071 Uiso 0.60 1 calc PR A 1 H9C H 0.4149 0.5275 0.2715 0.071 Uiso 0.60 1 calc PR A 1 C10 C 0.4353(9) 0.4738(10) 0.1696(5) 0.0474(19) Uani 0.60 1 d P A 1 H10A H 0.4785 0.5125 0.1814 0.071 Uiso 0.60 1 calc PR A 1 H10B H 0.4246 0.4830 0.1314 0.071 Uiso 0.60 1 calc PR A 1 H10C H 0.4522 0.4143 0.1753 0.071 Uiso 0.60 1 calc PR A 1 C8B C 0.3484(13) 0.5799(17) 0.1748(9) 0.0474(19) Uani 0.40 1 d P A 2 H8B1 H 0.3882 0.6195 0.1903 0.071 Uiso 0.40 1 calc PR A 2 H8B2 H 0.2936 0.6030 0.1799 0.071 Uiso 0.40 1 calc PR A 2 H8B3 H 0.3592 0.5730 0.1365 0.071 Uiso 0.40 1 calc PR A 2 C9B C 0.3460(12) 0.5085(15) 0.2649(9) 0.0474(19) Uani 0.40 1 d P A 2 H9B1 H 0.3400 0.4536 0.2835 0.071 Uiso 0.40 1 calc PR A 2 H9B2 H 0.2979 0.5439 0.2715 0.071 Uiso 0.40 1 calc PR A 2 H9B3 H 0.3944 0.5381 0.2784 0.071 Uiso 0.40 1 calc PR A 2 C10B C 0.4343(14) 0.4524(15) 0.1931(8) 0.0474(19) Uani 0.40 1 d P A 2 H10D H 0.4776 0.4932 0.2017 0.071 Uiso 0.40 1 calc PR A 2 H10E H 0.4384 0.4358 0.1553 0.071 Uiso 0.40 1 calc PR A 2 H10F H 0.4399 0.4015 0.2158 0.071 Uiso 0.40 1 calc PR A 2 C11 C 0.2635(5) 0.2500 0.0068(3) 0.0209(18) Uani 1 2 d S . . C12 C 0.2494(4) 0.2930(5) -0.0795(2) 0.0356(16) Uani 1 1 d . . . H12 H 0.2443 0.3290 -0.1100 0.043 Uiso 1 1 calc R . . C13 C 0.3450(4) 0.4745(5) -0.0433(3) 0.045(2) Uani 1 1 d . . . C14 C 0.3664(5) 0.5570(6) -0.0141(3) 0.0681(17) Uani 1 1 d . . . H14A H 0.3773 0.5444 0.0237 0.102 Uiso 1 1 calc R . . H14B H 0.3208 0.5972 -0.0167 0.102 Uiso 1 1 calc R . . H14C H 0.4147 0.5825 -0.0305 0.102 Uiso 1 1 calc R . . C15 C 0.3280(5) 0.4966(7) -0.1017(3) 0.0681(17) Uani 1 1 d . . . H15A H 0.3778 0.5182 -0.1185 0.102 Uiso 1 1 calc R . . H15B H 0.2857 0.5406 -0.1036 0.102 Uiso 1 1 calc R . . H15C H 0.3097 0.4452 -0.1207 0.102 Uiso 1 1 calc R . . C16 C 0.4166(5) 0.4155(6) -0.0405(3) 0.0681(17) Uani 1 1 d . . . H16A H 0.4642 0.4437 -0.0561 0.102 Uiso 1 1 calc R . . H16B H 0.4047 0.3630 -0.0606 0.102 Uiso 1 1 calc R . . H16C H 0.4277 0.4010 -0.0030 0.102 Uiso 1 1 calc R . . C17 C 0.1593(4) 0.4655(5) -0.0163(3) 0.0348(16) Uani 1 1 d . . . C18 C 0.1570(6) 0.5580(5) 0.0066(3) 0.062(3) Uani 1 1 d . . . H18A H 0.1919 0.5952 -0.0151 0.093 Uiso 1 1 calc R . . H18B H 0.1765 0.5576 0.0437 0.093 Uiso 1 1 calc R . . H18C H 0.1011 0.5795 0.0056 0.093 Uiso 1 1 calc R . . C19 C 0.1298(5) 0.4673(6) -0.0745(3) 0.052(2) Uani 1 1 d . . . H19A H 0.1321 0.4094 -0.0895 0.077 Uiso 1 1 calc R . . H19B H 0.1647 0.5055 -0.0956 0.077 Uiso 1 1 calc R . . H19C H 0.0737 0.4882 -0.0757 0.077 Uiso 1 1 calc R . . C20 C 0.1028(4) 0.4081(6) 0.0163(3) 0.051(2) Uani 1 1 d . . . H20A H 0.0469 0.4291 0.0132 0.077 Uiso 1 1 calc R . . H20B H 0.1194 0.4090 0.0540 0.077 Uiso 1 1 calc R . . H20C H 0.1059 0.3494 0.0026 0.077 Uiso 1 1 calc R . . C21 C 0.5354(6) 0.2500 0.1383(4) 0.042(3) Uani 1 2 d S . . C22 C 0.9262(7) 0.2500 0.1049(4) 0.045(3) Uani 1 2 d S . . C23 C 0.0826(8) 0.7500 0.2976(5) 0.076(5) Uani 1 2 d S . . C24 C 0.4816(11) 0.2500 0.6419(7) 0.122(7) Uani 1 2 d S . . H24A H 0.4523 0.1990 0.6554 0.146 Uiso 0.50 1 calc PR . . H24B H 0.4523 0.3010 0.6554 0.146 Uiso 0.50 1 calc PR . . C25 C 0.1683(9) 0.2500 0.5561(7) 0.122(8) Uani 1 2 d S . . H25A H 0.1684 0.3011 0.5326 0.147 Uiso 0.50 1 calc PR . . H25B H 0.1684 0.1989 0.5326 0.147 Uiso 0.50 1 calc PR . . N1 N 0.2907(3) 0.3196(3) 0.19482(18) 0.0274(12) Uani 1 1 d . . . N2 N 0.2583(3) 0.3197(3) -0.02627(19) 0.0266(12) Uani 1 1 d . . . O1 O 0.4239(3) 0.3275(3) 0.08405(18) 0.0429(12) Uani 1 1 d . . . O2 O 0.5288(5) 0.2500 0.0352(3) 0.055(2) Uani 1 2 d S . . O3 O 0.7955(5) 0.2500 0.0473(3) 0.051(2) Uani 1 2 d S . . O4 O 0.7956(3) 0.1725(3) 0.13087(17) 0.0397(12) Uani 1 1 d . . . O5 O 0.2179(3) 0.6732(3) 0.29785(19) 0.0502(14) Uani 1 1 d . . . O6 O 0.1787(5) 0.7500 0.2177(3) 0.052(2) Uani 1 2 d S . . F1 F 0.5822(3) 0.1817(3) 0.13983(19) 0.0585(13) Uani 1 1 d . . . F2 F 0.4897(4) 0.2500 0.1824(2) 0.0479(16) Uani 1 2 d S . . F3 F 0.9524(4) 0.2500 0.1550(3) 0.0632(19) Uani 1 2 d S . . F4 F 0.9559(3) 0.1815(4) 0.0811(2) 0.0831(17) Uani 1 1 d . . . F5 F 0.0422(3) 0.8175(5) 0.2799(3) 0.112(2) Uani 1 1 d . . . F6 F 0.0769(5) 0.7500 0.3506(3) 0.133(5) Uani 1 2 d S . . P2 P 0.26342(11) 0.42383(12) -0.00348(6) 0.0293(4) Uani 1 1 d . . . P1 P 0.27492(10) 0.42383(11) 0.17240(6) 0.0267(4) Uani 1 1 d . A . S1 S 0.47144(14) 0.2500 0.07819(9) 0.0357(6) Uani 1 2 d S . . S2 S 0.81524(16) 0.2500 0.10302(9) 0.0312(6) Uani 1 2 d S . . S3 S 0.18613(16) 0.7500 0.27519(9) 0.0361(6) Uani 1 2 d S . . Cu1 Cu 0.27735(6) 0.2500 0.08413(4) 0.0234(3) Uani 1 2 d S . . Cu2 Cu 0.28852(6) 0.41450(6) 0.08400(3) 0.0444(3) Uani 1 1 d . A . Cl1 Cl 0.4744(3) 0.2500 0.5753(2) 0.136(2) Uani 1 2 d S . . Cl2 Cl 0.5755(3) 0.2500 0.6694(2) 0.140(2) Uani 1 2 d S . . Cl3 Cl 0.2570(3) 0.2500 0.59283(19) 0.1163(18) Uani 1 2 d S . . Cl4 Cl 0.0823(3) 0.2500 0.59122(18) 0.156(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.018(4) 0.026(5) 0.013(4) 0.000 -0.002(3) 0.000 C2 0.052(4) 0.044(4) 0.011(3) -0.007(3) -0.004(3) -0.002(3) C3 0.028(4) 0.043(5) 0.044(4) -0.008(3) 0.007(3) -0.002(3) C4 0.042(5) 0.052(6) 0.092(7) 0.005(5) 0.011(5) 0.014(4) C5 0.056(6) 0.095(8) 0.053(5) -0.011(5) 0.020(4) 0.013(5) C6 0.033(5) 0.062(6) 0.119(8) -0.031(6) 0.014(5) -0.009(4) C7 0.024(4) 0.043(4) 0.026(3) -0.013(3) -0.005(3) -0.003(3) C8 0.034(4) 0.056(5) 0.053(5) -0.023(4) 0.001(4) -0.004(3) C9 0.034(4) 0.056(5) 0.053(5) -0.023(4) 0.001(4) -0.004(3) C10 0.034(4) 0.056(5) 0.053(5) -0.023(4) 0.001(4) -0.004(3) C8B 0.034(4) 0.056(5) 0.053(5) -0.023(4) 0.001(4) -0.004(3) C9B 0.034(4) 0.056(5) 0.053(5) -0.023(4) 0.001(4) -0.004(3) C10B 0.034(4) 0.056(5) 0.053(5) -0.023(4) 0.001(4) -0.004(3) C11 0.020(4) 0.028(5) 0.015(4) 0.000 -0.003(3) 0.000 C12 0.043(4) 0.050(4) 0.015(3) 0.006(3) -0.006(3) -0.003(3) C13 0.029(4) 0.061(5) 0.044(4) 0.020(4) -0.015(3) -0.022(4) C14 0.056(3) 0.090(4) 0.058(3) 0.037(3) -0.011(3) -0.034(3) C15 0.056(3) 0.090(4) 0.058(3) 0.037(3) -0.011(3) -0.034(3) C16 0.056(3) 0.090(4) 0.058(3) 0.037(3) -0.011(3) -0.034(3) C17 0.041(4) 0.036(4) 0.028(3) 0.004(3) -0.007(3) -0.003(3) C18 0.081(6) 0.049(6) 0.056(5) -0.005(4) -0.023(5) 0.019(5) C19 0.047(5) 0.073(6) 0.035(4) 0.011(4) -0.012(4) 0.002(4) C20 0.035(4) 0.065(6) 0.054(5) 0.025(4) 0.004(4) -0.002(4) C21 0.031(6) 0.052(7) 0.043(6) 0.000 -0.014(5) 0.000 C22 0.038(6) 0.055(8) 0.044(6) 0.000 0.008(5) 0.000 C23 0.045(8) 0.140(16) 0.043(7) 0.000 -0.012(6) 0.000 C24 0.096(14) 0.17(2) 0.100(14) 0.000 0.050(11) 0.000 C25 0.060(11) 0.21(2) 0.095(13) 0.000 -0.004(10) 0.000 N1 0.031(3) 0.036(3) 0.015(2) -0.004(2) -0.003(2) -0.001(2) N2 0.028(3) 0.036(3) 0.016(2) 0.001(2) -0.001(2) -0.003(2) O1 0.032(3) 0.066(4) 0.031(2) 0.004(3) -0.003(2) 0.014(2) O2 0.054(5) 0.072(6) 0.039(4) 0.000 0.013(4) 0.000 O3 0.075(6) 0.050(5) 0.028(4) 0.000 -0.006(4) 0.000 O4 0.057(3) 0.037(3) 0.025(2) 0.006(2) -0.001(2) -0.008(2) O5 0.077(4) 0.041(3) 0.033(3) 0.000(2) -0.005(3) 0.010(3) O6 0.071(5) 0.063(6) 0.021(3) 0.000 -0.003(4) 0.000 F1 0.043(3) 0.058(3) 0.075(3) -0.002(3) -0.021(2) 0.014(2) F2 0.054(4) 0.063(4) 0.027(3) 0.000 -0.006(3) 0.000 F3 0.041(4) 0.075(5) 0.074(5) 0.000 -0.018(3) 0.000 F4 0.063(3) 0.089(4) 0.098(4) -0.031(3) 0.017(3) 0.022(3) F5 0.065(4) 0.176(7) 0.094(5) -0.028(5) -0.012(3) 0.053(4) F6 0.057(5) 0.307(16) 0.034(4) 0.000 0.014(4) 0.000 P2 0.0356(10) 0.0336(10) 0.0187(8) 0.0043(7) -0.0045(7) -0.0114(8) P1 0.0285(9) 0.0298(9) 0.0217(8) -0.0055(7) -0.0017(7) -0.0003(8) S1 0.0279(12) 0.0576(17) 0.0214(11) 0.000 0.0006(10) 0.000 S2 0.0413(14) 0.0337(14) 0.0186(10) 0.000 -0.0019(10) 0.000 S3 0.0474(15) 0.0423(16) 0.0186(11) 0.000 -0.0029(11) 0.000 Cu1 0.0284(6) 0.0315(6) 0.0105(4) 0.000 -0.0029(4) 0.000 Cu2 0.0777(7) 0.0370(5) 0.0186(4) 0.0029(4) -0.0111(4) -0.0238(5) Cl1 0.107(4) 0.192(6) 0.109(4) 0.000 0.022(3) 0.000 Cl2 0.086(3) 0.237(7) 0.098(3) 0.000 0.036(3) 0.000 Cl3 0.084(3) 0.164(5) 0.102(4) 0.000 -0.005(3) 0.000 Cl4 0.078(3) 0.317(10) 0.074(3) 0.000 -0.004(3) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.364(7) . ? C1 N1 1.364(7) 7_565 ? C1 Cu1 1.947(8) . ? C2 C2 1.333(13) 7_565 ? C2 N1 1.390(7) . ? C2 H2 0.9500 . ? C3 C4 1.523(11) . ? C3 C6 1.524(11) . ? C3 C5 1.527(10) . ? C3 P1 1.869(7) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C10B 1.47(2) . ? C7 C9 1.503(15) . ? C7 C8B 1.54(3) . ? C7 C8 1.544(19) . ? C7 C9B 1.58(2) . ? C7 C10 1.586(16) . ? C7 P1 1.864(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C8B H8B1 0.9800 . ? C8B H8B2 0.9800 . ? C8B H8B3 0.9800 . ? C9B H9B1 0.9800 . ? C9B H9B2 0.9800 . ? C9B H9B3 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11 N2 1.369(7) 7_565 ? C11 N2 1.369(7) . ? C11 Cu1 1.943(8) . ? C12 C12 1.343(14) 7_565 ? C12 N2 1.399(7) . ? C12 H12 0.9500 . ? C13 C16 1.499(12) . ? C13 C14 1.521(12) . ? C13 C15 1.523(10) . ? C13 P2 1.849(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.527(9) . ? C17 C19 1.531(9) . ? C17 C18 1.554(10) . ? C17 P2 1.861(7) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 F1 1.316(7) 7_565 ? C21 F1 1.316(7) . ? C21 F2 1.333(12) . ? C21 S1 1.833(10) . ? C22 F4 1.318(7) 7_565 ? C22 F4 1.318(7) . ? C22 F3 1.321(12) . ? C22 S2 1.828(11) . ? C23 F5 1.323(9) 7_575 ? C23 F5 1.323(9) . ? C23 F6 1.326(14) . ? C23 S3 1.795(14) . ? C24 Cl1 1.665(17) . ? C24 Cl2 1.693(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 Cl4 1.664(17) . ? C25 Cl3 1.724(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? N1 P1 1.741(6) . ? N2 P2 1.725(6) . ? O1 S1 1.450(5) . ? O2 S1 1.430(7) . ? O3 S2 1.429(7) . ? O4 S2 1.433(5) . ? O5 S3 1.426(5) . ? O6 S3 1.441(7) . ? P2 Cu2 2.2263(18) . ? P1 Cu2 2.2219(18) . ? S1 O1 1.450(5) 7_565 ? S2 O4 1.433(5) 7_565 ? S3 O5 1.426(5) 7_575 ? Cu1 Cu2 2.5761(9) . ? Cu1 Cu2 2.5761(9) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 N1 105.6(7) . 7_565 ? N1 C1 Cu1 127.1(3) . . ? N1 C1 Cu1 127.1(3) 7_565 . ? C2 C2 N1 107.6(4) 7_565 . ? C2 C2 H2 126.2 7_565 . ? N1 C2 H2 126.2 . . ? C4 C3 C6 109.7(7) . . ? C4 C3 C5 108.2(7) . . ? C6 C3 C5 108.1(7) . . ? C4 C3 P1 108.5(5) . . ? C6 C3 P1 106.5(5) . . ? C5 C3 P1 115.6(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C10B C7 C9 83.4(10) . . ? C10B C7 C8B 111.5(12) . . ? C9 C7 C8B 124.0(11) . . ? C10B C7 C8 127.8(12) . . ? C9 C7 C8 110.7(9) . . ? C10B C7 C9B 108.5(12) . . ? C8B C7 C9B 107.3(12) . . ? C8 C7 C9B 90.0(10) . . ? C9 C7 C10 105.8(8) . . ? C8B C7 C10 89.1(10) . . ? C8 C7 C10 107.7(9) . . ? C9B C7 C10 128.6(10) . . ? C10B C7 P1 108.5(9) . . ? C9 C7 P1 120.3(7) . . ? C8B C7 P1 105.9(9) . . ? C8 C7 P1 106.2(7) . . ? C9B C7 P1 115.1(9) . . ? C10 C7 P1 105.7(6) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? C7 C8B H8B1 109.5 . . ? C7 C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7 C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7 C9B H9B1 109.5 . . ? C7 C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7 C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7 C10B H10D 109.5 . . ? C7 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? N2 C11 N2 105.4(7) 7_565 . ? N2 C11 Cu1 127.3(3) 7_565 . ? N2 C11 Cu1 127.3(3) . . ? C12 C12 N2 107.4(4) 7_565 . ? C12 C12 H12 126.3 7_565 . ? N2 C12 H12 126.3 . . ? C16 C13 C14 108.4(6) . . ? C16 C13 C15 109.1(7) . . ? C14 C13 C15 108.0(7) . . ? C16 C13 P2 106.4(5) . . ? C14 C13 P2 105.9(6) . . ? C15 C13 P2 118.6(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 108.8(6) . . ? C20 C17 C18 109.5(7) . . ? C19 C17 C18 108.9(6) . . ? C20 C17 P2 105.3(5) . . ? C19 C17 P2 117.5(5) . . ? C18 C17 P2 106.6(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? F1 C21 F1 108.2(8) 7_565 . ? F1 C21 F2 107.9(6) 7_565 . ? F1 C21 F2 107.9(6) . . ? F1 C21 S1 111.1(5) 7_565 . ? F1 C21 S1 111.1(5) . . ? F2 C21 S1 110.6(7) . . ? F4 C22 F4 108.5(9) 7_565 . ? F4 C22 F3 107.8(7) 7_565 . ? F4 C22 F3 107.8(7) . . ? F4 C22 S2 111.1(6) 7_565 . ? F4 C22 S2 111.1(6) . . ? F3 C22 S2 110.5(7) . . ? F5 C23 F5 105.7(11) 7_575 . ? F5 C23 F6 107.3(8) 7_575 . ? F5 C23 F6 107.3(8) . . ? F5 C23 S3 111.9(7) 7_575 . ? F5 C23 S3 111.9(7) . . ? F6 C23 S3 112.2(9) . . ? Cl1 C24 Cl2 118.0(9) . . ? Cl1 C24 H24A 107.8 . . ? Cl2 C24 H24A 107.8 . . ? Cl1 C24 H24B 107.8 . . ? Cl2 C24 H24B 107.8 . . ? H24A C24 H24B 107.1 . . ? Cl4 C25 Cl3 116.2(11) . . ? Cl4 C25 H25A 108.2 . . ? Cl3 C25 H25A 108.2 . . ? Cl4 C25 H25B 108.2 . . ? Cl3 C25 H25B 108.2 . . ? H25A C25 H25B 107.4 . . ? C1 N1 C2 109.6(5) . . ? C1 N1 P1 122.8(4) . . ? C2 N1 P1 126.9(4) . . ? C11 N2 C12 110.0(5) . . ? C11 N2 P2 123.2(4) . . ? C12 N2 P2 126.8(4) . . ? N2 P2 C13 105.2(3) . . ? N2 P2 C17 103.2(3) . . ? C13 P2 C17 115.2(3) . . ? N2 P2 Cu2 105.71(18) . . ? C13 P2 Cu2 114.9(2) . . ? C17 P2 Cu2 111.3(2) . . ? N1 P1 C7 107.5(3) . . ? N1 P1 C3 102.5(3) . . ? C7 P1 C3 113.3(3) . . ? N1 P1 Cu2 104.04(17) . . ? C7 P1 Cu2 111.8(2) . . ? C3 P1 Cu2 116.4(2) . . ? O2 S1 O1 115.6(2) . . ? O2 S1 O1 115.6(2) . 7_565 ? O1 S1 O1 113.4(4) . 7_565 ? O2 S1 C21 103.6(5) . . ? O1 S1 C21 103.1(3) . . ? O1 S1 C21 103.1(3) 7_565 . ? O3 S2 O4 114.9(2) . . ? O3 S2 O4 114.9(2) . 7_565 ? O4 S2 O4 115.3(4) . 7_565 ? O3 S2 C22 104.7(5) . . ? O4 S2 C22 102.3(3) . . ? O4 S2 C22 102.3(3) 7_565 . ? O5 S3 O5 114.6(5) 7_575 . ? O5 S3 O6 115.2(2) 7_575 . ? O5 S3 O6 115.2(2) . . ? O5 S3 C23 103.0(3) 7_575 . ? O5 S3 C23 103.0(3) . . ? O6 S3 C23 103.3(5) . . ? C11 Cu1 C1 177.1(3) . . ? C11 Cu1 Cu2 90.40(3) . . ? C1 Cu1 Cu2 89.80(3) . . ? C11 Cu1 Cu2 90.40(3) . 7_565 ? C1 Cu1 Cu2 89.80(3) . 7_565 ? Cu2 Cu1 Cu2 171.81(7) . 7_565 ? P1 Cu2 P2 161.86(9) . . ? P1 Cu2 Cu1 93.26(6) . . ? P2 Cu2 Cu1 93.06(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 N1 C2 -1.3(9) 7_565 . . . ? Cu1 C1 N1 C2 -178.1(5) . . . . ? N1 C1 N1 P1 -172.3(2) 7_565 . . . ? Cu1 C1 N1 P1 10.9(9) . . . . ? C2 C2 N1 C1 0.8(6) 7_565 . . . ? C2 C2 N1 P1 171.3(3) 7_565 . . . ? N2 C11 N2 C12 0.3(9) 7_565 . . . ? Cu1 C11 N2 C12 179.4(5) . . . . ? N2 C11 N2 P2 -179.0(2) 7_565 . . . ? Cu1 C11 N2 P2 0.1(9) . . . . ? C12 C12 N2 C11 -0.2(6) 7_565 . . . ? C12 C12 N2 P2 179.1(3) 7_565 . . . ? C11 N2 P2 C13 126.0(6) . . . . ? C12 N2 P2 C13 -53.1(6) . . . . ? C11 N2 P2 C17 -112.8(6) . . . . ? C12 N2 P2 C17 68.1(6) . . . . ? C11 N2 P2 Cu2 4.1(6) . . . . ? C12 N2 P2 Cu2 -175.0(5) . . . . ? C16 C13 P2 N2 -49.6(6) . . . . ? C14 C13 P2 N2 -164.8(5) . . . . ? C15 C13 P2 N2 73.8(8) . . . . ? C16 C13 P2 C17 -162.5(5) . . . . ? C14 C13 P2 C17 82.3(6) . . . . ? C15 C13 P2 C17 -39.1(9) . . . . ? C16 C13 P2 Cu2 66.2(6) . . . . ? C14 C13 P2 Cu2 -49.0(6) . . . . ? C15 C13 P2 Cu2 -170.4(6) . . . . ? C20 C17 P2 N2 60.1(5) . . . . ? C19 C17 P2 N2 -61.2(6) . . . . ? C18 C17 P2 N2 176.4(5) . . . . ? C20 C17 P2 C13 174.2(5) . . . . ? C19 C17 P2 C13 52.9(7) . . . . ? C18 C17 P2 C13 -69.5(6) . . . . ? C20 C17 P2 Cu2 -52.8(5) . . . . ? C19 C17 P2 Cu2 -174.1(5) . . . . ? C18 C17 P2 Cu2 63.5(5) . . . . ? C1 N1 P1 C7 -137.1(6) . . . . ? C2 N1 P1 C7 53.5(6) . . . . ? C1 N1 P1 C3 103.2(6) . . . . ? C2 N1 P1 C3 -66.1(6) . . . . ? C1 N1 P1 Cu2 -18.4(6) . . . . ? C2 N1 P1 Cu2 172.2(5) . . . . ? C10B C7 P1 N1 50.7(10) . . . . ? C9 C7 P1 N1 -42.5(8) . . . . ? C8B C7 P1 N1 170.5(8) . . . . ? C8 C7 P1 N1 -169.0(6) . . . . ? C9B C7 P1 N1 -71.1(10) . . . . ? C10 C7 P1 N1 76.9(7) . . . . ? C10B C7 P1 C3 163.2(10) . . . . ? C9 C7 P1 C3 70.0(8) . . . . ? C8B C7 P1 C3 -77.0(9) . . . . ? C8 C7 P1 C3 -56.4(7) . . . . ? C9B C7 P1 C3 41.4(10) . . . . ? C10 C7 P1 C3 -170.6(7) . . . . ? C10B C7 P1 Cu2 -62.9(10) . . . . ? C9 C7 P1 Cu2 -156.1(7) . . . . ? C8B C7 P1 Cu2 56.9(8) . . . . ? C8 C7 P1 Cu2 77.5(6) . . . . ? C9B C7 P1 Cu2 175.3(9) . . . . ? C10 C7 P1 Cu2 -36.7(7) . . . . ? C4 C3 P1 N1 -166.9(5) . . . . ? C6 C3 P1 N1 -48.8(6) . . . . ? C5 C3 P1 N1 71.3(7) . . . . ? C4 C3 P1 C7 77.6(6) . . . . ? C6 C3 P1 C7 -164.4(6) . . . . ? C5 C3 P1 C7 -44.2(7) . . . . ? C4 C3 P1 Cu2 -54.1(6) . . . . ? C6 C3 P1 Cu2 64.0(6) . . . . ? C5 C3 P1 Cu2 -175.9(5) . . . . ? F1 C21 S1 O2 60.2(6) 7_565 . . . ? F1 C21 S1 O2 -60.2(6) . . . . ? F2 C21 S1 O2 180.0 . . . . ? F1 C21 S1 O1 -60.7(7) 7_565 . . . ? F1 C21 S1 O1 178.9(6) . . . . ? F2 C21 S1 O1 59.1(2) . . . . ? F1 C21 S1 O1 -178.9(6) 7_565 . . 7_565 ? F1 C21 S1 O1 60.7(7) . . . 7_565 ? F2 C21 S1 O1 -59.1(2) . . . 7_565 ? F4 C22 S2 O3 60.4(6) 7_565 . . . ? F4 C22 S2 O3 -60.4(6) . . . . ? F3 C22 S2 O3 180.0 . . . . ? F4 C22 S2 O4 -179.4(6) 7_565 . . . ? F4 C22 S2 O4 59.7(7) . . . . ? F3 C22 S2 O4 -59.9(2) . . . . ? F4 C22 S2 O4 -59.7(7) 7_565 . . 7_565 ? F4 C22 S2 O4 179.4(6) . . . 7_565 ? F3 C22 S2 O4 59.9(2) . . . 7_565 ? F5 C23 S3 O5 179.5(7) 7_575 . . 7_575 ? F5 C23 S3 O5 61.0(8) . . . 7_575 ? F6 C23 S3 O5 -59.7(2) . . . 7_575 ? F5 C23 S3 O5 -61.0(8) 7_575 . . . ? F5 C23 S3 O5 -179.5(7) . . . . ? F6 C23 S3 O5 59.7(2) . . . . ? F5 C23 S3 O6 59.3(7) 7_575 . . . ? F5 C23 S3 O6 -59.3(7) . . . . ? F6 C23 S3 O6 180.000(2) . . . . ? N2 C11 Cu1 Cu2 175.4(7) 7_565 . . . ? N2 C11 Cu1 Cu2 -3.5(7) . . . . ? N2 C11 Cu1 Cu2 3.5(7) 7_565 . . 7_565 ? N2 C11 Cu1 Cu2 -175.4(7) . . . 7_565 ? N1 C1 Cu1 Cu2 2.2(7) . . . . ? N1 C1 Cu1 Cu2 -174.0(7) 7_565 . . . ? N1 C1 Cu1 Cu2 174.0(7) . . . 7_565 ? N1 C1 Cu1 Cu2 -2.2(7) 7_565 . . 7_565 ? N1 P1 Cu2 P2 125.0(3) . . . . ? C7 P1 Cu2 P2 -119.2(3) . . . . ? C3 P1 Cu2 P2 13.1(4) . . . . ? N1 P1 Cu2 Cu1 14.82(19) . . . . ? C7 P1 Cu2 Cu1 130.5(2) . . . . ? C3 P1 Cu2 Cu1 -97.1(3) . . . . ? N2 P2 Cu2 P1 -115.1(3) . . . . ? C13 P2 Cu2 P1 129.4(4) . . . . ? C17 P2 Cu2 P1 -3.8(4) . . . . ? N2 P2 Cu2 Cu1 -4.81(19) . . . . ? C13 P2 Cu2 Cu1 -120.3(3) . . . . ? C17 P2 Cu2 Cu1 106.5(2) . . . . ? C11 Cu1 Cu2 P1 167.2(2) . . . . ? C1 Cu1 Cu2 P1 -9.8(2) . . . . ? C11 Cu1 Cu2 P2 4.2(2) . . . . ? C1 Cu1 Cu2 P2 -172.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.808 _refine_diff_density_min -1.201 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 963087' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbad130425 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H76 Ag3 N4 P4, 3(C F3 O3 S), 2(C H2 Cl2)' _chemical_formula_sum 'C43 H80 Ag3 Cl4 F9 N4 O9 P4 S3' _chemical_formula_weight 1653.58 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' 'x-1/2, y, -z-1/2' _cell_length_a 16.5334(6) _cell_length_b 15.6264(5) _cell_length_c 25.5667(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6605.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8880 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 30.95 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3344 _exptl_absorpt_coefficient_mu 1.308 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7272 _exptl_absorpt_correction_T_max 0.7798 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator triumph _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34171 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 31.02 _reflns_number_total 10868 _reflns_number_gt 6629 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0308P)^2^+20.4278P] 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 10868 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2371(3) 0.2500 0.49981(17) 0.0194(5) Uani 1 2 d S . . C2 C 0.2510(2) 0.2074(2) 0.41703(13) 0.0267(8) Uani 1 1 d . . . H2 H 0.2561 0.1713 0.3873 0.032 Uiso 1 1 calc R . . C3 C 0.1534(2) 0.0263(3) 0.45221(14) 0.0280(8) Uani 1 1 d . . . C4 C 0.1334(4) -0.0582(3) 0.47944(19) 0.0546(15) Uani 1 1 d . . . H4A H 0.0844 -0.0828 0.4639 0.082 Uiso 1 1 calc R . . H4B H 0.1243 -0.0478 0.5168 0.082 Uiso 1 1 calc R . . H4C H 0.1785 -0.0982 0.4750 0.082 Uiso 1 1 calc R . . C5 C 0.1685(3) 0.0076(3) 0.39435(15) 0.0372(10) Uani 1 1 d . . . H5A H 0.2109 -0.0360 0.3910 0.056 Uiso 1 1 calc R . . H5B H 0.1858 0.0601 0.3767 0.056 Uiso 1 1 calc R . . H5C H 0.1185 -0.0135 0.3782 0.056 Uiso 1 1 calc R . . C6 C 0.0814(3) 0.0880(4) 0.4575(2) 0.0529(15) Uani 1 1 d . . . H6A H 0.0935 0.1414 0.4391 0.079 Uiso 1 1 calc R . . H6B H 0.0716 0.1001 0.4946 0.079 Uiso 1 1 calc R . . H6C H 0.0331 0.0616 0.4422 0.079 Uiso 1 1 calc R . . C7 C 0.3406(2) 0.0338(3) 0.47806(15) 0.0295(8) Uani 1 1 d . . . C8 C 0.3435(3) -0.0568(3) 0.5013(2) 0.0544(14) Uani 1 1 d . . . H8A H 0.3098 -0.0952 0.4803 0.082 Uiso 1 1 calc R . . H8B H 0.3230 -0.0555 0.5373 0.082 Uiso 1 1 calc R . . H8C H 0.3994 -0.0775 0.5013 0.082 Uiso 1 1 calc R . . C9 C 0.3686(3) 0.0315(3) 0.42111(17) 0.0461(11) Uani 1 1 d . . . H9A H 0.3663 0.0893 0.4063 0.069 Uiso 1 1 calc R . . H9B H 0.3332 -0.0065 0.4010 0.069 Uiso 1 1 calc R . . H9C H 0.4243 0.0101 0.4195 0.069 Uiso 1 1 calc R . . C10 C 0.3967(3) 0.0927(4) 0.5094(2) 0.0499(13) Uani 1 1 d . . . H10A H 0.4520 0.0703 0.5080 0.075 Uiso 1 1 calc R . . H10B H 0.3785 0.0949 0.5459 0.075 Uiso 1 1 calc R . . H10C H 0.3954 0.1503 0.4944 0.075 Uiso 1 1 calc R . . C11 C 0.2142(3) 0.2500 0.66781(17) 0.0166(9) Uani 1 2 d S . . C12 C 0.2048(3) 0.2077(3) 0.75038(15) 0.0392(11) Uani 1 1 d . . . H12 H 0.2015 0.1717 0.7803 0.047 Uiso 1 1 calc R . . C13 C 0.3291(3) 0.0492(3) 0.69993(16) 0.0328(9) Uani 1 1 d . . . C14 C 0.3542(3) -0.0341(3) 0.6738(2) 0.0565(14) Uani 1 1 d . . . H14A H 0.3456 -0.0296 0.6359 0.085 Uiso 1 1 calc R . . H14B H 0.3217 -0.0812 0.6877 0.085 Uiso 1 1 calc R . . H14C H 0.4116 -0.0450 0.6808 0.085 Uiso 1 1 calc R . . C15 C 0.3375(4) 0.0388(5) 0.7592(2) 0.074(2) Uani 1 1 d . . . H15A H 0.3947 0.0317 0.7682 0.112 Uiso 1 1 calc R . . H15B H 0.3072 -0.0117 0.7706 0.112 Uiso 1 1 calc R . . H15C H 0.3160 0.0897 0.7767 0.112 Uiso 1 1 calc R . . C16 C 0.3827(3) 0.1209(4) 0.6801(3) 0.0683(19) Uani 1 1 d . . . H16A H 0.4395 0.1064 0.6866 0.102 Uiso 1 1 calc R . . H16B H 0.3692 0.1741 0.6984 0.102 Uiso 1 1 calc R . . H16C H 0.3741 0.1284 0.6424 0.102 Uiso 1 1 calc R . . C17 C 0.1429(3) 0.0097(3) 0.70819(17) 0.0340(10) Uani 1 1 d . . . C18 C 0.1635(9) -0.0850(11) 0.6966(5) 0.043(2) Uani 0.55 1 d P A 1 H18A H 0.2079 -0.1035 0.7194 0.064 Uiso 0.55 1 calc PR A 1 H18B H 0.1798 -0.0909 0.6600 0.064 Uiso 0.55 1 calc PR A 1 H18C H 0.1158 -0.1206 0.7033 0.064 Uiso 0.55 1 calc PR A 1 C19 C 0.1247(11) 0.0187(11) 0.7660(9) 0.057(4) Uani 0.55 1 d P A 1 H19A H 0.0991 0.0743 0.7724 0.086 Uiso 0.55 1 calc PR A 1 H19B H 0.1751 0.0149 0.7859 0.086 Uiso 0.55 1 calc PR A 1 H19C H 0.0880 -0.0271 0.7769 0.086 Uiso 0.55 1 calc PR A 1 C20 C 0.0634(10) 0.0323(12) 0.6760(4) 0.055(4) Uani 0.55 1 d P A 1 H20A H 0.0189 -0.0047 0.6875 0.083 Uiso 0.55 1 calc PR A 1 H20B H 0.0733 0.0232 0.6386 0.083 Uiso 0.55 1 calc PR A 1 H20C H 0.0489 0.0923 0.6821 0.083 Uiso 0.55 1 calc PR A 1 C18B C 0.1447(12) -0.0766(15) 0.6802(6) 0.043(2) Uani 0.45 1 d P A 2 H18D H 0.1990 -0.1013 0.6829 0.064 Uiso 0.45 1 calc PR A 2 H18E H 0.1307 -0.0685 0.6433 0.064 Uiso 0.45 1 calc PR A 2 H18F H 0.1054 -0.1153 0.6965 0.064 Uiso 0.45 1 calc PR A 2 C19B C 0.1540(14) -0.0066(16) 0.7686(11) 0.057(4) Uani 0.45 1 d P A 2 H19D H 0.1602 0.0483 0.7867 0.086 Uiso 0.45 1 calc PR A 2 H19E H 0.2023 -0.0416 0.7744 0.086 Uiso 0.45 1 calc PR A 2 H19F H 0.1064 -0.0365 0.7823 0.086 Uiso 0.45 1 calc PR A 2 C20B C 0.0665(13) 0.0556(15) 0.6995(5) 0.055(4) Uani 0.45 1 d P A 2 H20D H 0.0211 0.0190 0.7098 0.083 Uiso 0.45 1 calc PR A 2 H20E H 0.0616 0.0704 0.6624 0.083 Uiso 0.45 1 calc PR A 2 H20F H 0.0660 0.1080 0.7205 0.083 Uiso 0.45 1 calc PR A 2 C21 C 0.4156(5) 0.7500 0.7970(3) 0.058(2) Uani 1 2 d S . . C22 C -0.0459(4) 0.2500 0.6386(2) 0.0353(14) Uani 1 2 d S . . C23 C 0.4279(4) 0.7500 0.3948(3) 0.0428(16) Uani 1 2 d S . . C24 C 0.6690(6) 0.7500 0.9434(3) 0.071(3) Uani 1 2 d S . . H24A H 0.6695 0.6989 0.9663 0.085 Uiso 0.50 1 calc PR . . H24B H 0.6695 0.8011 0.9663 0.085 Uiso 0.50 1 calc PR . . C25 C 0.5228(9) 0.2500 0.3577(6) 0.155(7) Uani 1 2 d S . . H25A H 0.5523 0.1990 0.3449 0.186 Uiso 0.50 1 calc PR . . H25B H 0.5523 0.3010 0.3449 0.186 Uiso 0.50 1 calc PR . . N1 N 0.24206(19) 0.18097(18) 0.46910(10) 0.0194(5) Uani 1 1 d . . . N2 N 0.2105(2) 0.1809(2) 0.69819(11) 0.0269(7) Uani 1 1 d . . . O1 O 0.2799(2) 0.82731(19) 0.79712(11) 0.0432(8) Uani 1 1 d . . . O2 O 0.3196(3) 0.7500 0.71891(15) 0.0440(12) Uani 1 2 d S . . O3 O 0.06278(18) 0.17196(19) 0.58467(11) 0.0361(7) Uani 1 1 d . . . O4 O -0.0420(3) 0.2500 0.53780(18) 0.0471(12) Uani 1 2 d S . . O5 O 0.2988(2) 0.82779(18) 0.36895(11) 0.0372(7) Uani 1 1 d . . . O6 O 0.2982(3) 0.7500 0.45098(15) 0.0436(12) Uani 1 2 d S . . F1 F 0.4554(2) 0.8179(3) 0.77974(16) 0.0908(13) Uani 1 1 d . . . F2 F 0.4197(3) 0.7500 0.84892(18) 0.096(2) Uani 1 2 d S . . F3 F -0.09225(18) 0.18118(19) 0.64090(13) 0.0603(9) Uani 1 1 d . . . F4 F -0.0004(3) 0.2500 0.68134(14) 0.0528(11) Uani 1 2 d S . . F5 F 0.4588(2) 0.8186(2) 0.41805(14) 0.0718(10) Uani 1 1 d . . . F6 F 0.4557(3) 0.7500 0.34564(18) 0.0652(13) Uani 1 2 d S . . P1 P 0.23668(6) 0.07514(6) 0.49066(3) 0.01948(18) Uani 1 1 d . . . P2 P 0.22412(6) 0.07504(6) 0.67707(3) 0.02249(19) Uani 1 1 d . A . S1 S 0.31181(10) 0.7500 0.77475(5) 0.0297(3) Uani 1 2 d S . . S2 S 0.01597(8) 0.2500 0.57947(5) 0.0270(3) Uani 1 2 d S . . S3 S 0.31773(10) 0.7500 0.39620(5) 0.0272(3) Uani 1 2 d S . . Ag1 Ag 0.22386(2) 0.2500 0.583520(13) 0.01931(8) Uani 1 2 d S . . Ag2 Ag 0.211368(19) 0.073876(16) 0.583389(10) 0.02618(7) Uani 1 1 d . A . Cl1 Cl 0.75366(19) 0.7500 0.90767(13) 0.1475(19) Uani 1 2 d S . . Cl2 Cl 0.58248(18) 0.7500 0.90955(11) 0.1419(18) Uani 1 2 d S . . Cl3 Cl 0.4283(3) 0.2500 0.32940(16) 0.166(2) Uani 1 2 d S . . Cl4 Cl 0.5276(3) 0.2500 0.42188(19) 0.186(2) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0278(14) 0.0165(12) 0.0140(10) 0.000 0.0026(10) 0.000 C2 0.042(2) 0.0243(17) 0.0134(13) -0.0028(14) 0.0045(17) -0.0009(16) C3 0.030(2) 0.0285(19) 0.0256(17) -0.0087(15) 0.0011(16) -0.0091(17) C4 0.071(4) 0.048(3) 0.045(3) -0.002(2) 0.002(3) -0.041(3) C5 0.042(3) 0.042(3) 0.0272(19) -0.0121(18) 0.0007(19) -0.009(2) C6 0.024(2) 0.074(4) 0.061(3) -0.035(3) -0.004(2) 0.002(2) C7 0.029(2) 0.027(2) 0.0326(19) -0.0044(16) 0.0045(17) 0.0022(17) C8 0.058(3) 0.038(3) 0.067(3) 0.007(2) 0.011(3) 0.023(3) C9 0.038(2) 0.060(3) 0.040(2) -0.006(2) 0.014(2) 0.009(2) C10 0.027(2) 0.061(3) 0.062(3) -0.025(3) -0.002(2) 0.003(2) C11 0.025(2) 0.0073(18) 0.0172(19) 0.000 -0.0003(19) 0.000 C12 0.067(3) 0.035(2) 0.0155(14) 0.0040(15) 0.008(2) 0.002(2) C13 0.029(2) 0.034(2) 0.036(2) 0.0100(17) -0.0093(18) -0.0006(18) C14 0.041(3) 0.044(3) 0.085(4) 0.006(3) -0.010(3) 0.015(2) C15 0.065(4) 0.114(6) 0.044(3) 0.005(3) -0.029(3) 0.013(4) C16 0.031(3) 0.057(4) 0.117(5) 0.037(4) -0.018(3) -0.010(3) C17 0.027(2) 0.035(2) 0.039(2) 0.0159(18) 0.0079(18) 0.0024(18) C18 0.038(7) 0.043(5) 0.047(8) 0.008(6) -0.006(5) -0.015(5) C19 0.070(13) 0.058(11) 0.043(4) 0.010(7) 0.029(9) -0.017(7) C20 0.026(3) 0.080(10) 0.061(8) 0.040(8) 0.002(7) 0.000(5) C18B 0.038(7) 0.043(5) 0.047(8) 0.008(6) -0.006(5) -0.015(5) C19B 0.070(13) 0.058(11) 0.043(4) 0.010(7) 0.029(9) -0.017(7) C20B 0.026(3) 0.080(10) 0.061(8) 0.040(8) 0.002(7) 0.000(5) C21 0.046(4) 0.082(6) 0.045(4) 0.000 -0.003(4) 0.000 C22 0.033(3) 0.026(3) 0.047(3) 0.000 0.009(3) 0.000 C23 0.045(4) 0.037(4) 0.046(4) 0.000 -0.003(3) 0.000 C24 0.081(7) 0.086(7) 0.045(4) 0.000 0.004(5) 0.000 C25 0.110(12) 0.209(18) 0.147(14) 0.000 0.069(11) 0.000 N1 0.0278(14) 0.0165(12) 0.0140(10) 0.000 0.0026(10) 0.000 N2 0.0394(19) 0.0263(16) 0.0151(12) 0.0013(11) 0.0030(14) 0.0022(15) O1 0.066(2) 0.0320(16) 0.0315(14) -0.0021(12) 0.0026(16) 0.0087(16) O2 0.065(3) 0.047(3) 0.0200(18) 0.000 0.004(2) 0.000 O3 0.0319(15) 0.0372(16) 0.0392(15) -0.0003(14) 0.0042(14) 0.0105(13) O4 0.049(3) 0.045(3) 0.047(3) 0.000 -0.023(2) 0.000 O5 0.054(2) 0.0295(15) 0.0285(13) 0.0017(11) -0.0021(14) 0.0069(14) O6 0.063(3) 0.048(3) 0.0202(18) 0.000 0.004(2) 0.000 F1 0.060(2) 0.114(3) 0.098(3) -0.009(2) 0.004(2) -0.039(2) F2 0.062(3) 0.183(7) 0.042(2) 0.000 -0.022(2) 0.000 F3 0.0498(18) 0.0435(17) 0.087(2) -0.0022(15) 0.0278(17) -0.0189(15) F4 0.073(3) 0.054(3) 0.0317(18) 0.000 0.006(2) 0.000 F5 0.0500(18) 0.068(2) 0.097(3) -0.024(2) -0.0116(19) -0.0178(17) F6 0.054(3) 0.075(3) 0.067(3) 0.000 0.026(2) 0.000 P1 0.0248(5) 0.0153(4) 0.0184(4) -0.0020(3) 0.0029(4) -0.0019(4) P2 0.0270(5) 0.0219(4) 0.0186(4) 0.0047(3) 0.0009(4) 0.0011(4) S1 0.0429(9) 0.0278(7) 0.0185(6) 0.000 -0.0014(6) 0.000 S2 0.0243(6) 0.0292(7) 0.0274(6) 0.000 -0.0021(6) 0.000 S3 0.0369(8) 0.0256(7) 0.0191(5) 0.000 0.0010(6) 0.000 Ag1 0.0298(2) 0.01600(15) 0.01208(13) 0.000 0.00188(16) 0.000 Ag2 0.04261(17) 0.01856(12) 0.01738(11) 0.00088(10) 0.00239(13) -0.00472(12) Cl1 0.0597(16) 0.288(6) 0.095(2) 0.000 0.0136(17) 0.000 Cl2 0.0577(16) 0.302(6) 0.0661(16) 0.000 0.0017(14) 0.000 Cl3 0.106(3) 0.272(6) 0.120(3) 0.000 0.052(2) 0.000 Cl4 0.106(3) 0.300(7) 0.151(4) 0.000 0.042(3) 0.000 _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.337(4) . ? C1 N1 1.337(4) 7_565 ? C1 Ag1 2.152(4) . ? C2 C2 1.332(7) 7_565 ? C2 N1 1.402(4) . ? C2 H2 0.9500 . ? C3 C5 1.529(5) . ? C3 C4 1.530(6) . ? C3 C6 1.537(6) . ? C3 P1 1.856(4) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.529(6) . ? C7 C10 1.533(6) . ? C7 C8 1.537(6) . ? C7 P1 1.863(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N2 1.332(4) 7_565 ? C11 N2 1.332(4) . ? C11 Ag1 2.161(4) . ? C12 C12 1.321(8) 7_565 ? C12 N2 1.402(5) . ? C12 H12 0.9500 . ? C13 C16 1.516(6) . ? C13 C14 1.520(7) . ? C13 C15 1.529(6) . ? C13 P2 1.876(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20B 1.47(2) . ? C17 C19 1.51(2) . ? C17 C18B 1.53(2) . ? C17 C18 1.547(19) . ? C17 C19B 1.58(3) . ? C17 C20 1.590(16) . ? C17 P2 1.866(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20B H20D 0.9800 . ? C20B H20E 0.9800 . ? C20B H20F 0.9800 . ? C21 F1 1.325(6) . ? C21 F1 1.325(6) 7_575 ? C21 F2 1.329(8) . ? C21 S1 1.808(8) . ? C22 F3 1.321(4) 7_565 ? C22 F3 1.321(4) . ? C22 F4 1.328(7) . ? C22 S2 1.826(6) . ? C23 F5 1.328(5) 7_575 ? C23 F5 1.328(5) . ? C23 F6 1.338(8) . ? C23 S3 1.822(7) . ? C24 Cl2 1.672(10) . ? C24 Cl1 1.673(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 Cl4 1.642(15) . ? C25 Cl3 1.722(16) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? N1 P1 1.745(3) . ? N2 P2 1.754(3) . ? O1 S1 1.437(3) . ? O2 S1 1.433(4) . ? O3 S2 1.450(3) . ? O4 S2 1.433(4) . ? O5 S3 1.436(3) . ? O6 S3 1.437(4) . ? P1 Ag2 2.4076(9) . ? P2 Ag2 2.4046(9) . ? S1 O1 1.437(3) 7_575 ? S2 O3 1.450(3) 7_565 ? S3 O5 1.436(3) 7_575 ? Ag1 Ag2 2.7599(3) 7_565 ? Ag1 Ag2 2.7599(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 N1 C1 N1 107.6(4) . 7_565 ? N1 C1 Ag1 126.19(19) . . ? N1 C1 Ag1 126.19(19) 7_565 . ? C2 C2 N1 107.12(18) 7_565 . ? C2 C2 H2 126.4 7_565 . ? N1 C2 H2 126.4 . . ? C5 C3 C4 108.1(3) . . ? C5 C3 C6 109.4(4) . . ? C4 C3 C6 109.5(4) . . ? C5 C3 P1 118.0(3) . . ? C4 C3 P1 105.9(3) . . ? C6 C3 P1 105.7(3) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C10 109.2(4) . . ? C9 C7 C8 109.7(4) . . ? C10 C7 C8 109.3(4) . . ? C9 C7 P1 116.9(3) . . ? C10 C7 P1 105.1(3) . . ? C8 C7 P1 106.3(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 N2 108.4(4) 7_565 . ? N2 C11 Ag1 125.8(2) 7_565 . ? N2 C11 Ag1 125.8(2) . . ? C12 C12 N2 107.4(2) 7_565 . ? C12 C12 H12 126.3 7_565 . ? N2 C12 H12 126.3 . . ? C16 C13 C14 109.0(4) . . ? C16 C13 C15 110.9(5) . . ? C14 C13 C15 108.7(4) . . ? C16 C13 P2 106.1(3) . . ? C14 C13 P2 107.4(3) . . ? C15 C13 P2 114.5(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20B C17 C19 86.1(8) . . ? C20B C17 C18B 112.2(11) . . ? C19 C17 C18B 122.9(10) . . ? C20B C17 C18 128.9(11) . . ? C19 C17 C18 108.6(8) . . ? C20B C17 C19B 109.1(9) . . ? C18B C17 C19B 108.3(11) . . ? C18 C17 C19B 90.4(10) . . ? C19 C17 C20 108.6(8) . . ? C18B C17 C20 88.3(9) . . ? C18 C17 C20 107.2(8) . . ? C19B C17 C20 129.7(9) . . ? C20B C17 P2 106.7(9) . . ? C19 C17 P2 120.5(9) . . ? C18B C17 P2 105.7(8) . . ? C18 C17 P2 106.5(7) . . ? C19B C17 P2 115.0(10) . . ? C20 C17 P2 104.6(6) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? C17 C18B H18D 109.5 . . ? C17 C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17 C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17 C19B H19D 109.5 . . ? C17 C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17 C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C17 C20B H20D 109.5 . . ? C17 C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? C17 C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? F1 C21 F1 106.5(7) . 7_575 ? F1 C21 F2 107.9(5) . . ? F1 C21 F2 107.9(5) 7_575 . ? F1 C21 S1 111.5(4) . . ? F1 C21 S1 111.5(4) 7_575 . ? F2 C21 S1 111.2(6) . . ? F3 C22 F3 108.9(5) 7_565 . ? F3 C22 F4 107.0(4) 7_565 . ? F3 C22 F4 107.0(4) . . ? F3 C22 S2 111.2(3) 7_565 . ? F3 C22 S2 111.2(3) . . ? F4 C22 S2 111.3(4) . . ? F5 C23 F5 107.7(6) 7_575 . ? F5 C23 F6 106.8(4) 7_575 . ? F5 C23 F6 106.8(4) . . ? F5 C23 S3 112.0(4) 7_575 . ? F5 C23 S3 112.0(4) . . ? F6 C23 S3 111.2(5) . . ? Cl2 C24 Cl1 115.6(5) . . ? Cl2 C24 H24A 108.4 . . ? Cl1 C24 H24A 108.4 . . ? Cl2 C24 H24B 108.4 . . ? Cl1 C24 H24B 108.4 . . ? H24A C24 H24B 107.4 . . ? Cl4 C25 Cl3 117.6(8) . . ? Cl4 C25 H25A 107.9 . . ? Cl3 C25 H25A 107.9 . . ? Cl4 C25 H25B 107.9 . . ? Cl3 C25 H25B 107.9 . . ? H25A C25 H25B 107.2 . . ? C1 N1 C2 109.1(3) . . ? C1 N1 P1 125.2(2) . . ? C2 N1 P1 125.7(2) . . ? C11 N2 C12 108.4(3) . . ? C11 N2 P2 125.4(2) . . ? C12 N2 P2 125.7(3) . . ? N1 P1 C3 105.07(17) . . ? N1 P1 C7 103.11(17) . . ? C3 P1 C7 116.75(18) . . ? N1 P1 Ag2 109.12(9) . . ? C3 P1 Ag2 112.91(12) . . ? C7 P1 Ag2 109.13(13) . . ? N2 P2 C17 107.03(18) . . ? N2 P2 C13 103.04(18) . . ? C17 P2 C13 114.57(18) . . ? N2 P2 Ag2 107.61(10) . . ? C17 P2 Ag2 110.94(15) . . ? C13 P2 Ag2 112.94(14) . . ? O2 S1 O1 115.43(15) . 7_575 ? O2 S1 O1 115.43(15) . . ? O1 S1 O1 114.4(3) 7_575 . ? O2 S1 C21 103.2(3) . . ? O1 S1 C21 102.9(2) 7_575 . ? O1 S1 C21 102.9(2) . . ? O4 S2 O3 115.15(15) . 7_565 ? O4 S2 O3 115.15(15) . . ? O3 S2 O3 114.4(3) 7_565 . ? O4 S2 C22 103.9(3) . . ? O3 S2 C22 102.90(17) 7_565 . ? O3 S2 C22 102.90(17) . . ? O5 S3 O5 115.7(2) . 7_575 ? O5 S3 O6 115.09(15) . . ? O5 S3 O6 115.09(15) 7_575 . ? O5 S3 C23 102.04(19) . . ? O5 S3 C23 102.04(19) 7_575 . ? O6 S3 C23 104.1(3) . . ? C1 Ag1 C11 178.4(2) . . ? C1 Ag1 Ag2 90.368(14) . 7_565 ? C11 Ag1 Ag2 89.754(14) . 7_565 ? C1 Ag1 Ag2 90.368(14) . . ? C11 Ag1 Ag2 89.754(14) . . ? Ag2 Ag1 Ag2 171.41(2) 7_565 . ? P2 Ag2 P1 164.93(4) . . ? P2 Ag2 Ag1 89.12(3) . . ? P1 Ag2 Ag1 88.85(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 N1 C2 0.4(6) 7_565 . . . ? Ag1 C1 N1 C2 -179.5(3) . . . . ? N1 C1 N1 P1 -178.73(16) 7_565 . . . ? Ag1 C1 N1 P1 1.4(6) . . . . ? C2 C2 N1 C1 -0.3(4) 7_565 . . . ? C2 C2 N1 P1 178.9(2) 7_565 . . . ? N2 C11 N2 C12 -0.4(6) 7_565 . . . ? Ag1 C11 N2 C12 179.9(3) . . . . ? N2 C11 N2 P2 -172.71(16) 7_565 . . . ? Ag1 C11 N2 P2 7.6(6) . . . . ? C12 C12 N2 C11 0.3(4) 7_565 . . . ? C12 C12 N2 P2 172.5(2) 7_565 . . . ? C1 N1 P1 C3 124.6(4) . . . . ? C2 N1 P1 C3 -54.4(4) . . . . ? C1 N1 P1 C7 -112.7(4) . . . . ? C2 N1 P1 C7 68.3(3) . . . . ? C1 N1 P1 Ag2 3.2(4) . . . . ? C2 N1 P1 Ag2 -175.8(3) . . . . ? C5 C3 P1 N1 72.6(4) . . . . ? C4 C3 P1 N1 -166.2(3) . . . . ? C6 C3 P1 N1 -50.1(3) . . . . ? C5 C3 P1 C7 -40.9(4) . . . . ? C4 C3 P1 C7 80.3(3) . . . . ? C6 C3 P1 C7 -163.6(3) . . . . ? C5 C3 P1 Ag2 -168.6(3) . . . . ? C4 C3 P1 Ag2 -47.4(3) . . . . ? C6 C3 P1 Ag2 68.8(3) . . . . ? C9 C7 P1 N1 -62.9(4) . . . . ? C10 C7 P1 N1 58.4(3) . . . . ? C8 C7 P1 N1 174.3(3) . . . . ? C9 C7 P1 C3 51.7(4) . . . . ? C10 C7 P1 C3 173.0(3) . . . . ? C8 C7 P1 C3 -71.1(3) . . . . ? C9 C7 P1 Ag2 -178.8(3) . . . . ? C10 C7 P1 Ag2 -57.5(3) . . . . ? C8 C7 P1 Ag2 58.4(3) . . . . ? C11 N2 P2 C17 -135.5(4) . . . . ? C12 N2 P2 C17 53.5(4) . . . . ? C11 N2 P2 C13 103.3(4) . . . . ? C12 N2 P2 C13 -67.7(4) . . . . ? C11 N2 P2 Ag2 -16.2(4) . . . . ? C12 N2 P2 Ag2 172.8(3) . . . . ? C20B C17 P2 N2 48.4(8) . . . . ? C19 C17 P2 N2 -46.9(7) . . . . ? C18B C17 P2 N2 168.0(6) . . . . ? C18 C17 P2 N2 -171.1(4) . . . . ? C19B C17 P2 N2 -72.7(8) . . . . ? C20 C17 P2 N2 75.6(7) . . . . ? C20B C17 P2 C13 162.0(7) . . . . ? C19 C17 P2 C13 66.6(7) . . . . ? C18B C17 P2 C13 -78.5(6) . . . . ? C18 C17 P2 C13 -57.5(5) . . . . ? C19B C17 P2 C13 40.9(9) . . . . ? C20 C17 P2 C13 -170.9(7) . . . . ? C20B C17 P2 Ag2 -68.7(7) . . . . ? C19 C17 P2 Ag2 -164.0(6) . . . . ? C18B C17 P2 Ag2 50.8(6) . . . . ? C18 C17 P2 Ag2 71.8(5) . . . . ? C19B C17 P2 Ag2 170.2(8) . . . . ? C20 C17 P2 Ag2 -41.5(7) . . . . ? C16 C13 P2 N2 -51.6(4) . . . . ? C14 C13 P2 N2 -168.1(3) . . . . ? C15 C13 P2 N2 71.1(4) . . . . ? C16 C13 P2 C17 -167.5(4) . . . . ? C14 C13 P2 C17 76.1(4) . . . . ? C15 C13 P2 C17 -44.7(5) . . . . ? C16 C13 P2 Ag2 64.2(4) . . . . ? C14 C13 P2 Ag2 -52.3(3) . . . . ? C15 C13 P2 Ag2 -173.1(4) . . . . ? F1 C21 S1 O2 59.5(5) . . . . ? F1 C21 S1 O2 -59.5(5) 7_575 . . . ? F2 C21 S1 O2 180.000(2) . . . . ? F1 C21 S1 O1 179.9(4) . . . 7_575 ? F1 C21 S1 O1 60.9(5) 7_575 . . 7_575 ? F2 C21 S1 O1 -59.59(14) . . . 7_575 ? F1 C21 S1 O1 -60.9(5) . . . . ? F1 C21 S1 O1 -179.9(4) 7_575 . . . ? F2 C21 S1 O1 59.59(14) . . . . ? F3 C22 S2 O4 -60.8(4) 7_565 . . . ? F3 C22 S2 O4 60.8(4) . . . . ? F4 C22 S2 O4 180.000(1) . . . . ? F3 C22 S2 O3 59.6(4) 7_565 . . 7_565 ? F3 C22 S2 O3 -178.8(4) . . . 7_565 ? F4 C22 S2 O3 -59.60(14) . . . 7_565 ? F3 C22 S2 O3 178.8(4) 7_565 . . . ? F3 C22 S2 O3 -59.6(4) . . . . ? F4 C22 S2 O3 59.60(14) . . . . ? F5 C23 S3 O5 -179.4(4) 7_575 . . . ? F5 C23 S3 O5 59.4(5) . . . . ? F6 C23 S3 O5 -59.97(13) . . . . ? F5 C23 S3 O5 -59.4(5) 7_575 . . 7_575 ? F5 C23 S3 O5 179.4(4) . . . 7_575 ? F6 C23 S3 O5 59.97(13) . . . 7_575 ? F5 C23 S3 O6 60.6(4) 7_575 . . . ? F5 C23 S3 O6 -60.6(4) . . . . ? F6 C23 S3 O6 180.0 . . . . ? N1 C1 Ag1 Ag2 -175.8(4) . . . 7_565 ? N1 C1 Ag1 Ag2 4.3(4) 7_565 . . 7_565 ? N1 C1 Ag1 Ag2 -4.3(4) . . . . ? N1 C1 Ag1 Ag2 175.8(4) 7_565 . . . ? N2 C11 Ag1 Ag2 -4.1(4) 7_565 . . 7_565 ? N2 C11 Ag1 Ag2 175.5(4) . . . 7_565 ? N2 C11 Ag1 Ag2 -175.5(4) 7_565 . . . ? N2 C11 Ag1 Ag2 4.1(4) . . . . ? N2 P2 Ag2 P1 95.90(17) . . . . ? C17 P2 Ag2 P1 -147.33(17) . . . . ? C13 P2 Ag2 P1 -17.1(2) . . . . ? N2 P2 Ag2 Ag1 13.59(13) . . . . ? C17 P2 Ag2 Ag1 130.36(15) . . . . ? C13 P2 Ag2 Ag1 -99.44(15) . . . . ? N1 P1 Ag2 P2 -86.87(17) . . . . ? C3 P1 Ag2 P2 156.69(17) . . . . ? C7 P1 Ag2 P2 25.1(2) . . . . ? N1 P1 Ag2 Ag1 -4.53(12) . . . . ? C3 P1 Ag2 Ag1 -120.96(15) . . . . ? C7 P1 Ag2 Ag1 107.45(14) . . . . ? C1 Ag1 Ag2 P2 169.18(14) . . . . ? C11 Ag1 Ag2 P2 -9.19(14) . . . . ? C1 Ag1 Ag2 P1 4.11(14) . . . . ? C11 Ag1 Ag2 P1 -174.26(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.765 _refine_diff_density_min -1.403 _refine_diff_density_rms 0.126 _database_code_depnum_ccdc_archive 'CCDC 963088' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_pbad130719 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H76 Au3 N4 P4, 3(C F3 O3 S), 2(C2 H3 N)' _chemical_formula_sum 'C45 H82 Au3 F9 N6 O9 P4 S3' _chemical_formula_weight 1833.13 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' 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' S S 0.1246 0.1234 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0469(6) _cell_length_b 12.6938(6) _cell_length_c 24.4780(12) _cell_angle_alpha 90.0060(10) _cell_angle_beta 103.5620(10) _cell_angle_gamma 116.8880(10) _cell_volume 3221.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9319 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 31.04 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.890 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1784 _exptl_absorpt_coefficient_mu 7.090 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3313 _exptl_absorpt_correction_T_max 0.4833 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59662 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 31.24 _reflns_number_total 20683 _reflns_number_gt 15900 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0170P)^2^+16.8627P] 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 20683 _refine_ls_number_parameters 750 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6985(5) 0.0936(4) 0.03002(17) 0.0235(10) Uani 1 1 d . . . C2 C 0.8934(6) 0.1844(6) 0.0901(2) 0.0472(16) Uani 1 1 d . . . H2 H 0.9610 0.2152 0.1241 0.057 Uiso 1 1 calc R . . C3 C 0.9077(6) 0.1942(6) 0.0382(2) 0.0415(14) Uani 1 1 d . . . H3 H 0.9869 0.2340 0.0280 0.050 Uiso 1 1 calc R . . C4 C 0.7435(7) 0.2408(6) 0.1785(3) 0.0536(19) Uani 1 1 d . . . C5 C 0.8841(7) 0.3153(7) 0.2076(4) 0.066(2) Uani 1 1 d . . . H5A H 0.8999 0.3949 0.2208 0.099 Uiso 1 1 calc R . . H5B H 0.9356 0.3215 0.1810 0.099 Uiso 1 1 calc R . . H5C H 0.9087 0.2779 0.2401 0.099 Uiso 1 1 calc R . . C6 C 0.7036(15) 0.3057(10) 0.1305(4) 0.153(7) Uani 1 1 d . . . H6A H 0.7310 0.3878 0.1455 0.229 Uiso 1 1 calc R . . H6B H 0.6097 0.2644 0.1152 0.229 Uiso 1 1 calc R . . H6C H 0.7449 0.3063 0.1004 0.229 Uiso 1 1 calc R . . C7 C 0.6672(9) 0.2248(9) 0.2206(5) 0.107(4) Uani 1 1 d . . . H7A H 0.6926 0.1834 0.2510 0.161 Uiso 1 1 calc R . . H7B H 0.5751 0.1777 0.2019 0.161 Uiso 1 1 calc R . . H7C H 0.6838 0.3029 0.2367 0.161 Uiso 1 1 calc R . . C8 C 0.7606(6) -0.0034(6) 0.1835(2) 0.0411(14) Uani 1 1 d . . . C9 C 0.6992(12) -0.0391(12) 0.2321(4) 0.114(5) Uani 1 1 d . . . H9A H 0.6053 -0.0731 0.2177 0.170 Uiso 1 1 calc R . . H9B H 0.7316 0.0310 0.2596 0.170 Uiso 1 1 calc R . . H9C H 0.7207 -0.0985 0.2505 0.170 Uiso 1 1 calc R . . C10 C 0.7176(7) -0.1113(6) 0.1413(3) 0.0567(19) Uani 1 1 d . . . H10A H 0.7460 -0.1665 0.1600 0.085 Uiso 1 1 calc R . . H10B H 0.7558 -0.0855 0.1094 0.085 Uiso 1 1 calc R . . H10C H 0.6233 -0.1513 0.1274 0.085 Uiso 1 1 calc R . . C11 C 0.9078(8) 0.0546(8) 0.2061(4) 0.084(3) Uani 1 1 d . . . H11A H 0.9377 0.1262 0.2323 0.126 Uiso 1 1 calc R . . H11B H 0.9475 0.0764 0.1745 0.126 Uiso 1 1 calc R . . H11C H 0.9322 -0.0018 0.2261 0.126 Uiso 1 1 calc R . . C12 C 0.1784(6) -0.0271(5) 0.0898(2) 0.0348(12) Uani 1 1 d . . . C13 C 0.2401(7) 0.0865(5) 0.0614(3) 0.0468(15) Uani 1 1 d . . . H13A H 0.2095 0.0666 0.0202 0.070 Uiso 1 1 calc R . . H13B H 0.3342 0.1196 0.0731 0.070 Uiso 1 1 calc R . . H13C H 0.2157 0.1452 0.0730 0.070 Uiso 1 1 calc R . . C14 C 0.0318(6) -0.0810(6) 0.0703(3) 0.0478(16) Uani 1 1 d . . . H14A H -0.0069 -0.1498 0.0904 0.072 Uiso 1 1 calc R . . H14B H 0.0026 -0.1066 0.0295 0.072 Uiso 1 1 calc R . . H14C H 0.0056 -0.0214 0.0786 0.072 Uiso 1 1 calc R . . C15 C 0.2220(6) 0.0049(6) 0.1545(2) 0.0438(15) Uani 1 1 d . . . H15A H 0.1973 0.0643 0.1648 0.066 Uiso 1 1 calc R . . H15B H 0.3159 0.0375 0.1676 0.066 Uiso 1 1 calc R . . H15C H 0.1806 -0.0668 0.1724 0.066 Uiso 1 1 calc R . . C16 C 0.1852(7) -0.2763(5) 0.0901(2) 0.0421(14) Uani 1 1 d . . . C17 C 0.0390(8) -0.3468(7) 0.0790(3) 0.065(2) Uani 1 1 d . . . H17A H 0.0158 -0.4277 0.0888 0.098 Uiso 1 1 calc R . . H17B H -0.0016 -0.3506 0.0389 0.098 Uiso 1 1 calc R . . H17C H 0.0090 -0.3076 0.1022 0.098 Uiso 1 1 calc R . . C18 C 0.2438(8) -0.2696(6) 0.1538(3) 0.0575(19) Uani 1 1 d . . . H18A H 0.2149 -0.2265 0.1754 0.086 Uiso 1 1 calc R . . H18B H 0.3381 -0.2279 0.1621 0.086 Uiso 1 1 calc R . . H18C H 0.2157 -0.3504 0.1644 0.086 Uiso 1 1 calc R . . C19 C 0.2368(9) -0.3369(7) 0.0558(3) 0.067(2) Uani 1 1 d . . . H19A H 0.2157 -0.4166 0.0668 0.101 Uiso 1 1 calc R . . H19B H 0.3307 -0.2895 0.0635 0.101 Uiso 1 1 calc R . . H19C H 0.1971 -0.3432 0.0154 0.101 Uiso 1 1 calc R . . C20 C 0.5207(4) 0.3491(3) 0.49590(16) 0.0130(7) Uani 1 1 d . . . C21 C 0.5053(4) 0.1764(4) 0.46418(19) 0.0226(9) Uani 1 1 d . . . H21 H 0.4781 0.1048 0.4409 0.027 Uiso 1 1 calc R . . C22 C 0.5948(4) 0.2164(4) 0.5133(2) 0.0247(10) Uani 1 1 d . . . H22 H 0.6432 0.1783 0.5314 0.030 Uiso 1 1 calc R . . C23 C 0.3725(6) 0.2167(5) 0.3311(2) 0.0331(12) Uani 1 1 d . . . C24 C 0.5051(7) 0.3183(7) 0.3353(3) 0.0588(19) Uani 1 1 d . . . H24A H 0.5681 0.3117 0.3668 0.088 Uiso 1 1 calc R . . H24B H 0.5044 0.3942 0.3419 0.088 Uiso 1 1 calc R . . H24C H 0.5286 0.3150 0.2999 0.088 Uiso 1 1 calc R . . C25 C 0.2744(7) 0.2271(6) 0.2812(2) 0.0466(15) Uani 1 1 d . . . H25A H 0.2698 0.3008 0.2886 0.070 Uiso 1 1 calc R . . H25B H 0.1892 0.1588 0.2767 0.070 Uiso 1 1 calc R . . H25C H 0.3017 0.2285 0.2464 0.070 Uiso 1 1 calc R . . C26 C 0.3686(10) 0.0964(7) 0.3197(3) 0.078(3) Uani 1 1 d . . . H26A H 0.3927 0.0932 0.2845 0.117 Uiso 1 1 calc R . . H26B H 0.2812 0.0324 0.3163 0.117 Uiso 1 1 calc R . . H26C H 0.4294 0.0867 0.3511 0.117 Uiso 1 1 calc R . . C27 C 0.1874(5) 0.1153(4) 0.4118(2) 0.0276(10) Uani 1 1 d . . . C28 C 0.1751(6) 0.1593(6) 0.4670(3) 0.0503(17) Uani 1 1 d . . . H28A H 0.1678 0.2328 0.4626 0.075 Uiso 1 1 calc R . . H28B H 0.2516 0.1749 0.4975 0.075 Uiso 1 1 calc R . . H28C H 0.0980 0.0985 0.4762 0.075 Uiso 1 1 calc R . . C29 C 0.0681(5) 0.0926(5) 0.3643(3) 0.0419(14) Uani 1 1 d . . . H29A H -0.0098 0.0442 0.3766 0.063 Uiso 1 1 calc R . . H29B H 0.0671 0.0504 0.3305 0.063 Uiso 1 1 calc R . . H29C H 0.0706 0.1688 0.3554 0.063 Uiso 1 1 calc R . . C30 C 0.1977(6) -0.0005(5) 0.4182(4) 0.062(2) Uani 1 1 d . . . H30A H 0.2729 0.0138 0.4493 0.093 Uiso 1 1 calc R . . H30B H 0.2071 -0.0277 0.3829 0.093 Uiso 1 1 calc R . . H30C H 0.1194 -0.0616 0.4266 0.093 Uiso 1 1 calc R . . C31 C 0.6352(6) 0.3186(4) 0.6523(2) 0.0366(13) Uani 1 1 d . . . C32 C 0.6421(11) 0.2010(6) 0.6554(3) 0.083(3) Uani 1 1 d . . . H32A H 0.7325 0.2174 0.6652 0.125 Uiso 1 1 calc R . . H32B H 0.5967 0.1518 0.6187 0.125 Uiso 1 1 calc R . . H32C H 0.6014 0.1586 0.6845 0.125 Uiso 1 1 calc R . . C33 C 0.4952(6) 0.2953(6) 0.6381(3) 0.059(2) Uani 1 1 d . . . H33A H 0.4547 0.2528 0.6672 0.089 Uiso 1 1 calc R . . H33B H 0.4484 0.2469 0.6012 0.089 Uiso 1 1 calc R . . H33C H 0.4924 0.3713 0.6368 0.089 Uiso 1 1 calc R . . C34 C 0.7059(7) 0.3937(6) 0.7104(2) 0.0454(15) Uani 1 1 d . . . H34A H 0.6572 0.3559 0.7380 0.068 Uiso 1 1 calc R . . H34B H 0.7135 0.4736 0.7077 0.068 Uiso 1 1 calc R . . H34C H 0.7922 0.3995 0.7227 0.068 Uiso 1 1 calc R . . C35 C 0.8706(5) 0.4404(5) 0.5971(2) 0.0361(13) Uani 1 1 d . . . C36 C 0.9614(5) 0.5191(5) 0.6522(2) 0.0387(13) Uani 1 1 d . . . H36A H 1.0505 0.5548 0.6493 0.058 Uiso 1 1 calc R . . H36B H 0.9528 0.4708 0.6837 0.058 Uiso 1 1 calc R . . H36C H 0.9390 0.5823 0.6591 0.058 Uiso 1 1 calc R . . C37 C 0.8979(6) 0.5106(8) 0.5477(3) 0.068(2) Uani 1 1 d . . . H37A H 0.8808 0.5785 0.5510 0.102 Uiso 1 1 calc R . . H37B H 0.8422 0.4593 0.5122 0.102 Uiso 1 1 calc R . . H37C H 0.9885 0.5394 0.5479 0.102 Uiso 1 1 calc R . . C38 C 0.8933(7) 0.3317(7) 0.5924(6) 0.118(5) Uani 1 1 d . . . H38A H 0.8514 0.2898 0.5539 0.177 Uiso 1 1 calc R . . H38B H 0.8569 0.2781 0.6195 0.177 Uiso 1 1 calc R . . H38C H 0.9862 0.3578 0.6009 0.177 Uiso 1 1 calc R . . C39 C 0.3983(7) 0.4547(7) 0.1555(3) 0.0571(18) Uani 1 1 d . . . C40 C 0.1963(10) 0.3670(7) 0.7598(4) 0.087(3) Uani 1 1 d . . . C41 C 0.8213(10) 0.1953(9) 0.4219(5) 0.0326(16) Uani 0.50 1 d P A 1 C41B C 0.7557(10) 0.1661(9) 0.3824(5) 0.0326(16) Uani 0.50 1 d P A 2 C42 C 0.7810(6) 0.6485(6) 0.4113(3) 0.0435(14) Uani 1 1 d . . . C43 C 0.8440(11) 0.7624(7) 0.3939(6) 0.122(5) Uani 1 1 d . . . H43A H 0.7801 0.7797 0.3683 0.184 Uiso 1 1 calc R . . H43B H 0.9067 0.7638 0.3743 0.184 Uiso 1 1 calc R . . H43C H 0.8888 0.8227 0.4272 0.184 Uiso 1 1 calc R . . C44 C 0.5904(9) 0.6749(8) 0.0223(4) 0.068(2) Uani 1 1 d . . . C45 C 0.6742(9) 0.6222(9) 0.0453(4) 0.083(3) Uani 1 1 d . . . H45A H 0.6223 0.5421 0.0542 0.125 Uiso 1 1 calc R . . H45B H 0.7380 0.6717 0.0799 0.125 Uiso 1 1 calc R . . H45C H 0.7187 0.6175 0.0174 0.125 Uiso 1 1 calc R . . N1 N 0.7615(5) 0.1207(4) 0.08644(17) 0.0372(11) Uani 1 1 d . . . N2 N 0.7837(4) 0.1349(4) 0.00059(17) 0.0315(10) Uani 1 1 d . . . N3 N 0.4582(3) 0.2589(3) 0.45300(15) 0.0175(7) Uani 1 1 d . . . N4 N 0.6054(4) 0.3246(3) 0.53368(16) 0.0206(8) Uani 1 1 d . . . N5 N 0.7302(9) 0.5604(7) 0.4257(3) 0.088(2) Uani 1 1 d . . . N6 N 0.5236(9) 0.7138(8) 0.0044(4) 0.094(3) Uani 1 1 d . . . O1 O 0.1787(5) 0.4437(4) 0.1517(2) 0.0599(13) Uani 1 1 d . . . O2 O 0.2057(5) 0.3668(4) 0.06883(19) 0.0528(12) Uani 1 1 d . . . O3 O 0.1889(5) 0.2600(4) 0.1501(2) 0.0613(14) Uani 1 1 d . . . O4 O -0.0230(11) 0.3348(11) 0.7623(3) 0.170(5) Uani 1 1 d . . . O5 O 0.0557(7) 0.2114(6) 0.8134(3) 0.0867(19) Uani 1 1 d . . . O6 O -0.0059(6) 0.1806(6) 0.7126(3) 0.104(3) Uani 1 1 d . . . O7 O 0.7749(5) -0.0237(4) 0.4088(3) 0.0672(16) Uani 1 1 d . . . O8 O 0.6393(5) 0.0274(4) 0.4481(2) 0.0514(12) Uani 1 1 d . . . O9 O 0.6408(9) 0.0297(8) 0.3455(4) 0.0503(16) Uani 0.50 1 d P A 1 O9B O 0.8919(9) 0.1443(9) 0.4738(4) 0.0503(16) Uani 0.50 1 d P A 2 F1 F 0.4523(6) 0.3968(6) 0.1379(3) 0.117(2) Uani 1 1 d . . . F2 F 0.4343(5) 0.4697(5) 0.21190(19) 0.0830(15) Uani 1 1 d . . . F3 F 0.4450(4) 0.5602(5) 0.1393(2) 0.0927(18) Uani 1 1 d . . . F4 F 0.2661(5) 0.3152(6) 0.7551(4) 0.141(3) Uani 1 1 d . . . F5 F 0.1950(7) 0.4294(5) 0.7169(3) 0.121(2) Uani 1 1 d . . . F6 F 0.2579(11) 0.4417(6) 0.8052(3) 0.227(6) Uani 1 1 d . . . F7 F 0.7636(4) 0.2643(3) 0.4094(2) 0.0583(11) Uani 1 1 d . . . F8 F 0.9038(7) 0.2259(7) 0.3898(4) 0.0516(10) Uani 0.50 1 d P A 1 F9 F 0.8885(7) 0.2194(7) 0.4753(3) 0.0516(10) Uani 0.50 1 d P A 1 F8B F 0.8534(7) 0.2020(7) 0.3570(4) 0.0516(10) Uani 0.50 1 d P A 2 F9B F 0.6438(7) 0.1103(7) 0.3420(3) 0.0516(10) Uani 0.50 1 d P A 2 P1 P 0.69443(14) 0.09012(14) 0.14397(5) 0.0334(3) Uani 1 1 d . . . P2 P 0.25072(14) -0.12082(12) 0.07367(5) 0.0293(3) Uani 1 1 d . . . P3 P 0.32885(11) 0.24100(9) 0.39622(4) 0.0173(2) Uani 1 1 d . . . P4 P 0.70527(11) 0.40998(10) 0.59862(5) 0.0215(2) Uani 1 1 d . . . S1 S 0.22452(15) 0.37252(11) 0.12873(6) 0.0375(3) Uani 1 1 d . . . S2 S 0.0351(2) 0.2599(2) 0.76159(7) 0.0619(5) Uani 1 1 d . . . S3 S 0.7024(2) 0.0374(2) 0.40430(11) 0.0265(3) Uani 0.50 1 d P A 1 S3B S 0.7690(2) 0.0674(2) 0.43397(11) 0.0265(3) Uani 0.50 1 d P A 2 Au1 Au 0.5000 0.0000 0.0000 0.02885(6) Uani 1 2 d S . . Au2 Au 0.47283(2) -0.01731(2) 0.108925(8) 0.03558(6) Uani 1 1 d . . . Au3 Au 0.5000 0.5000 0.5000 0.01436(5) Uani 1 2 d S . . Au4 Au 0.311031(16) 0.415082(13) 0.398620(7) 0.01756(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(3) 0.032(2) 0.0093(18) -0.0079(16) -0.0062(17) 0.029(2) C2 0.040(3) 0.080(5) 0.018(2) -0.012(3) -0.010(2) 0.033(3) C3 0.038(3) 0.065(4) 0.023(3) -0.007(2) -0.006(2) 0.032(3) C4 0.065(4) 0.068(4) 0.032(3) -0.024(3) -0.016(3) 0.049(4) C5 0.067(5) 0.052(4) 0.072(5) -0.018(4) 0.016(4) 0.022(4) C6 0.276(17) 0.126(9) 0.075(7) -0.050(6) -0.067(9) 0.164(11) C7 0.077(6) 0.110(8) 0.121(8) -0.073(7) 0.036(6) 0.027(6) C8 0.046(3) 0.066(4) 0.021(2) -0.002(2) -0.006(2) 0.041(3) C9 0.170(11) 0.225(13) 0.054(5) 0.081(7) 0.062(6) 0.168(11) C10 0.070(5) 0.054(4) 0.047(4) -0.001(3) -0.010(3) 0.042(4) C11 0.067(5) 0.076(5) 0.088(6) -0.006(5) -0.043(5) 0.047(5) C12 0.044(3) 0.046(3) 0.026(3) -0.003(2) 0.001(2) 0.035(3) C13 0.071(4) 0.049(3) 0.042(3) 0.006(3) 0.014(3) 0.046(3) C14 0.046(4) 0.069(4) 0.040(3) -0.004(3) 0.000(3) 0.043(3) C15 0.059(4) 0.057(4) 0.026(3) -0.007(2) 0.001(3) 0.041(3) C16 0.062(4) 0.044(3) 0.026(3) -0.001(2) 0.000(3) 0.035(3) C17 0.069(5) 0.055(4) 0.063(5) 0.014(4) 0.005(4) 0.027(4) C18 0.096(6) 0.059(4) 0.027(3) 0.008(3) 0.007(3) 0.049(4) C19 0.124(7) 0.059(4) 0.048(4) 0.003(3) 0.021(4) 0.068(5) C20 0.0106(17) 0.0176(17) 0.0098(16) -0.0029(13) 0.0018(13) 0.0061(14) C21 0.027(2) 0.0184(19) 0.024(2) -0.0027(16) -0.0013(18) 0.0162(17) C22 0.027(2) 0.0183(19) 0.029(2) -0.0045(17) -0.0058(19) 0.0167(18) C23 0.057(3) 0.043(3) 0.016(2) 0.0021(19) 0.008(2) 0.038(3) C24 0.055(4) 0.097(6) 0.040(4) 0.014(4) 0.025(3) 0.042(4) C25 0.071(4) 0.061(4) 0.016(2) 0.002(2) 0.005(3) 0.041(4) C26 0.167(9) 0.087(6) 0.032(3) 0.007(3) 0.030(5) 0.101(6) C27 0.023(2) 0.021(2) 0.031(3) 0.0032(18) -0.0016(19) 0.0089(18) C28 0.044(4) 0.056(4) 0.034(3) 0.013(3) 0.017(3) 0.006(3) C29 0.024(3) 0.041(3) 0.050(4) -0.001(3) -0.005(2) 0.012(2) C30 0.036(3) 0.023(3) 0.109(6) 0.020(3) 0.002(4) 0.007(2) C31 0.055(3) 0.024(2) 0.027(3) 0.0061(19) -0.003(2) 0.021(2) C32 0.174(10) 0.047(4) 0.044(4) 0.018(3) 0.022(5) 0.067(5) C33 0.039(3) 0.059(4) 0.045(4) 0.024(3) 0.002(3) -0.002(3) C34 0.059(4) 0.054(4) 0.025(3) 0.002(2) 0.002(3) 0.031(3) C35 0.023(2) 0.036(3) 0.046(3) -0.018(2) -0.009(2) 0.020(2) C36 0.025(3) 0.033(3) 0.037(3) 0.002(2) -0.012(2) 0.005(2) C37 0.034(3) 0.141(8) 0.029(3) -0.009(4) 0.007(3) 0.043(4) C38 0.035(4) 0.060(5) 0.238(13) -0.072(7) -0.029(6) 0.035(4) C39 0.059(4) 0.071(5) 0.048(4) 0.010(3) 0.008(3) 0.038(4) C40 0.105(7) 0.035(4) 0.080(6) -0.002(4) -0.032(5) 0.024(4) C41 0.027(4) 0.029(3) 0.044(5) 0.007(3) 0.012(3) 0.013(3) C41B 0.027(4) 0.029(3) 0.044(5) 0.007(3) 0.012(3) 0.013(3) C42 0.032(3) 0.050(4) 0.046(4) -0.003(3) 0.007(3) 0.018(3) C43 0.124(9) 0.040(4) 0.257(15) 0.038(6) 0.148(10) 0.038(5) C44 0.060(5) 0.069(5) 0.050(5) -0.005(4) 0.021(4) 0.006(4) C45 0.073(6) 0.085(6) 0.069(6) -0.010(5) 0.020(5) 0.017(5) N1 0.042(3) 0.053(3) 0.0149(19) -0.0085(18) -0.0091(18) 0.028(2) N2 0.041(3) 0.040(2) 0.0164(19) -0.0039(16) -0.0018(18) 0.026(2) N3 0.0205(17) 0.0143(15) 0.0184(17) -0.0029(13) -0.0008(14) 0.0116(13) N4 0.0214(18) 0.0167(16) 0.0225(18) -0.0030(13) -0.0045(14) 0.0129(14) N5 0.129(7) 0.070(5) 0.075(5) 0.035(4) 0.041(5) 0.047(5) N6 0.096(7) 0.107(7) 0.073(6) 0.006(5) 0.020(5) 0.043(6) O1 0.055(3) 0.047(3) 0.083(4) 0.000(2) 0.026(3) 0.025(2) O2 0.058(3) 0.053(3) 0.036(2) 0.010(2) 0.008(2) 0.019(2) O3 0.087(4) 0.030(2) 0.051(3) 0.0124(19) 0.007(3) 0.019(2) O4 0.283(12) 0.324(13) 0.105(6) 0.114(7) 0.108(7) 0.285(12) O5 0.112(5) 0.116(5) 0.071(4) 0.029(4) 0.018(4) 0.089(5) O6 0.063(4) 0.117(5) 0.071(4) -0.041(4) 0.020(3) -0.010(4) O7 0.065(3) 0.034(2) 0.131(5) 0.021(3) 0.055(3) 0.033(2) O8 0.070(3) 0.041(2) 0.072(3) 0.029(2) 0.054(3) 0.033(2) O9 0.052(4) 0.052(4) 0.035(3) 0.002(3) -0.002(3) 0.021(3) O9B 0.052(4) 0.052(4) 0.035(3) 0.002(3) -0.002(3) 0.021(3) F1 0.081(4) 0.165(6) 0.131(5) -0.017(4) 0.013(4) 0.087(4) F2 0.068(3) 0.100(4) 0.045(3) 0.007(2) -0.010(2) 0.020(3) F3 0.051(3) 0.080(3) 0.097(4) 0.041(3) 0.006(3) -0.006(2) F4 0.049(3) 0.104(5) 0.245(9) 0.101(5) 0.012(4) 0.027(3) F5 0.153(6) 0.068(3) 0.115(5) 0.040(3) -0.001(4) 0.048(4) F6 0.317(13) 0.078(5) 0.111(6) -0.035(4) -0.094(7) 0.017(6) F7 0.060(2) 0.0311(17) 0.102(3) 0.0191(19) 0.039(2) 0.0277(17) F8 0.039(2) 0.051(2) 0.055(3) 0.009(2) 0.0159(18) 0.0101(19) F9 0.039(2) 0.051(2) 0.055(3) 0.009(2) 0.0159(18) 0.0101(19) F8B 0.039(2) 0.051(2) 0.055(3) 0.009(2) 0.0159(18) 0.0101(19) F9B 0.039(2) 0.051(2) 0.055(3) 0.009(2) 0.0159(18) 0.0101(19) P1 0.0397(7) 0.0555(8) 0.0128(5) -0.0107(5) -0.0074(5) 0.0355(7) P2 0.0404(7) 0.0394(7) 0.0159(5) -0.0043(5) -0.0030(5) 0.0301(6) P3 0.0213(5) 0.0160(4) 0.0135(5) -0.0026(4) -0.0021(4) 0.0109(4) P4 0.0226(6) 0.0185(5) 0.0206(5) -0.0036(4) -0.0079(4) 0.0137(4) S1 0.0497(8) 0.0248(6) 0.0330(7) 0.0048(5) 0.0084(6) 0.0143(6) S2 0.0787(13) 0.1072(16) 0.0308(8) 0.0003(9) 0.0024(8) 0.0753(13) S3 0.0281(10) 0.0240(8) 0.0316(10) 0.0052(7) 0.0119(7) 0.0138(8) S3B 0.0281(10) 0.0240(8) 0.0316(10) 0.0052(7) 0.0119(7) 0.0138(8) Au1 0.03911(15) 0.03708(14) 0.01255(11) -0.00621(9) -0.00832(10) 0.02676(12) Au2 0.04315(12) 0.05750(13) 0.01496(8) -0.00813(8) -0.00686(8) 0.03778(11) Au3 0.01617(10) 0.01327(9) 0.01330(10) -0.00173(7) -0.00179(8) 0.00926(8) Au4 0.01974(8) 0.01648(7) 0.01569(7) -0.00199(5) -0.00217(6) 0.01103(6) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.307(7) . ? C1 N1 1.369(5) . ? C1 Au1 2.068(5) . ? C2 C3 1.322(8) . ? C2 N1 1.399(8) . ? C2 H2 0.9500 . ? C3 N2 1.408(7) . ? C3 H3 0.9500 . ? C4 C7 1.491(11) . ? C4 C5 1.503(10) . ? C4 C6 1.544(11) . ? C4 P1 1.861(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.510(10) . ? C8 C10 1.522(8) . ? C8 C11 1.534(9) . ? C8 P1 1.863(6) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C14 1.525(8) . ? C12 C15 1.540(7) . ? C12 C13 1.544(9) . ? C12 P2 1.852(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.525(10) . ? C16 C18 1.536(8) . ? C16 C19 1.537(9) . ? C16 P2 1.849(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N3 1.353(5) . ? C20 N4 1.356(5) . ? C20 Au3 2.045(4) . ? C21 C22 1.328(6) . ? C21 N3 1.398(5) . ? C21 H21 0.9500 . ? C22 N4 1.401(5) . ? C22 H22 0.9500 . ? C23 C24 1.512(9) . ? C23 C26 1.530(8) . ? C23 C25 1.541(8) . ? C23 P3 1.857(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.526(8) . ? C27 C29 1.530(7) . ? C27 C30 1.535(7) . ? C27 P3 1.854(5) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.526(9) . ? C31 C32 1.533(8) . ? C31 C34 1.533(7) . ? C31 P4 1.850(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C37 1.512(10) . ? C35 C36 1.529(7) . ? C35 C38 1.532(8) . ? C35 P4 1.859(5) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 F3 1.300(9) . ? C39 F1 1.309(9) . ? C39 F2 1.332(8) . ? C39 S1 1.812(8) . ? C40 F6 1.287(10) . ? C40 F4 1.303(12) . ? C40 F5 1.318(10) . ? C40 S2 1.809(11) . ? C41 F9 1.318(13) . ? C41 F8 1.331(13) . ? C41 F7 1.340(11) . ? C41 S3 1.835(11) . ? C41B F9B 1.344(13) . ? C41B F8B 1.355(13) . ? C41B F7 1.365(11) . ? C41B S3B 1.810(11) . ? C42 N5 1.110(9) . ? C42 C43 1.416(10) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 N6 1.130(12) . ? C44 C45 1.459(14) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? N1 P1 1.743(5) . ? N2 P2 1.757(4) 2_655 ? N3 P3 1.754(4) . ? N4 P4 1.753(4) . ? O1 S1 1.426(5) . ? O2 S1 1.427(5) . ? O3 S1 1.431(4) . ? O4 S2 1.414(6) . ? O5 S2 1.429(6) . ? O6 S2 1.402(6) . ? O7 S3B 1.347(5) . ? O7 S3 1.395(5) . ? O8 S3 1.428(5) . ? O8 S3B 1.535(5) . ? O9 S3 1.436(9) . ? O9B S3B 1.453(9) . ? P1 Au2 2.3141(15) . ? P2 N2 1.757(4) 2_655 ? P2 Au2 2.3168(14) . ? P3 Au4 2.3168(10) . ? P4 Au4 2.3183(11) 2_666 ? Au1 C1 2.068(5) 2_655 ? Au1 Au2 2.7584(2) . ? Au1 Au2 2.7584(2) 2_655 ? Au3 C20 2.045(4) 2_666 ? Au3 Au4 2.76278(19) 2_666 ? Au3 Au4 2.76278(19) . ? Au4 P4 2.3183(11) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 108.9(4) . . ? N2 C1 Au1 127.8(3) . . ? N1 C1 Au1 123.3(4) . . ? C3 C2 N1 108.2(5) . . ? C3 C2 H2 125.9 . . ? N1 C2 H2 125.9 . . ? C2 C3 N2 107.3(6) . . ? C2 C3 H3 126.3 . . ? N2 C3 H3 126.3 . . ? C7 C4 C5 108.8(6) . . ? C7 C4 C6 109.7(9) . . ? C5 C4 C6 108.9(9) . . ? C7 C4 P1 107.4(6) . . ? C5 C4 P1 116.7(5) . . ? C6 C4 P1 105.2(4) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C10 110.9(8) . . ? C9 C8 C11 109.5(7) . . ? C10 C8 C11 108.3(6) . . ? C9 C8 P1 106.8(5) . . ? C10 C8 P1 105.2(4) . . ? C11 C8 P1 116.1(5) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C14 C12 C15 108.8(5) . . ? C14 C12 C13 109.7(5) . . ? C15 C12 C13 109.5(5) . . ? C14 C12 P2 117.0(4) . . ? C15 C12 P2 106.3(4) . . ? C13 C12 P2 105.3(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 107.4(6) . . ? C17 C16 C19 111.1(6) . . ? C18 C16 C19 109.8(5) . . ? C17 C16 P2 116.8(4) . . ? C18 C16 P2 106.1(4) . . ? C19 C16 P2 105.4(5) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 N4 107.3(3) . . ? N3 C20 Au3 126.2(3) . . ? N4 C20 Au3 126.4(3) . . ? C22 C21 N3 107.6(4) . . ? C22 C21 H21 126.2 . . ? N3 C21 H21 126.2 . . ? C21 C22 N4 107.9(4) . . ? C21 C22 H22 126.0 . . ? N4 C22 H22 126.0 . . ? C24 C23 C26 111.2(6) . . ? C24 C23 C25 109.1(5) . . ? C26 C23 C25 107.5(5) . . ? C24 C23 P3 106.2(4) . . ? C26 C23 P3 116.4(4) . . ? C25 C23 P3 106.3(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 108.9(5) . . ? C28 C27 C30 109.7(5) . . ? C29 C27 C30 109.7(4) . . ? C28 C27 P3 105.4(3) . . ? C29 C27 P3 107.9(4) . . ? C30 C27 P3 115.0(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 110.4(6) . . ? C33 C31 C34 108.5(5) . . ? C32 C31 C34 108.5(5) . . ? C33 C31 P4 105.7(4) . . ? C32 C31 P4 115.6(5) . . ? C34 C31 P4 107.9(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C37 C35 C36 109.3(5) . . ? C37 C35 C38 110.7(7) . . ? C36 C35 C38 108.2(5) . . ? C37 C35 P4 105.5(4) . . ? C36 C35 P4 106.4(4) . . ? C38 C35 P4 116.4(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F3 C39 F1 108.4(7) . . ? F3 C39 F2 106.9(6) . . ? F1 C39 F2 107.7(7) . . ? F3 C39 S1 112.2(5) . . ? F1 C39 S1 110.0(6) . . ? F2 C39 S1 111.5(6) . . ? F6 C40 F4 106.2(10) . . ? F6 C40 F5 107.1(7) . . ? F4 C40 F5 107.4(10) . . ? F6 C40 S2 112.6(10) . . ? F4 C40 S2 111.6(5) . . ? F5 C40 S2 111.7(7) . . ? F9 C41 F8 107.9(9) . . ? F9 C41 F7 111.6(9) . . ? F8 C41 F7 104.2(9) . . ? F9 C41 S3 111.4(8) . . ? F8 C41 S3 111.0(8) . . ? F7 C41 S3 110.5(7) . . ? F9B C41B F8B 108.1(10) . . ? F9B C41B F7 110.4(8) . . ? F8B C41B F7 108.3(8) . . ? F9B C41B S3B 110.5(7) . . ? F8B C41B S3B 110.5(7) . . ? F7 C41B S3B 109.0(7) . . ? N5 C42 C43 178.2(9) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N6 C44 C45 178.8(10) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C1 N1 C2 106.8(5) . . ? C1 N1 P1 127.9(4) . . ? C2 N1 P1 125.1(3) . . ? C1 N2 C3 108.8(4) . . ? C1 N2 P2 125.7(3) . 2_655 ? C3 N2 P2 125.5(4) . 2_655 ? C20 N3 C21 108.8(3) . . ? C20 N3 P3 125.5(3) . . ? C21 N3 P3 125.4(3) . . ? C20 N4 C22 108.4(3) . . ? C20 N4 P4 125.8(3) . . ? C22 N4 P4 125.8(3) . . ? C41 F7 C41B 45.1(6) . . ? N1 P1 C4 103.2(3) . . ? N1 P1 C8 104.3(3) . . ? C4 P1 C8 118.3(3) . . ? N1 P1 Au2 107.77(15) . . ? C4 P1 Au2 111.6(2) . . ? C8 P1 Au2 110.6(2) . . ? N2 P2 C16 104.0(2) 2_655 . ? N2 P2 C12 103.3(2) 2_655 . ? C16 P2 C12 119.8(3) . . ? N2 P2 Au2 107.53(17) 2_655 . ? C16 P2 Au2 111.8(2) . . ? C12 P2 Au2 109.34(19) . . ? N3 P3 C27 103.7(2) . . ? N3 P3 C23 105.9(2) . . ? C27 P3 C23 116.8(2) . . ? N3 P3 Au4 107.76(11) . . ? C27 P3 Au4 111.12(16) . . ? C23 P3 Au4 110.82(17) . . ? N4 P4 C31 104.4(2) . . ? N4 P4 C35 104.9(2) . . ? C31 P4 C35 117.9(3) . . ? N4 P4 Au4 107.46(12) . 2_666 ? C31 P4 Au4 110.51(18) . 2_666 ? C35 P4 Au4 110.87(17) . 2_666 ? O1 S1 O2 114.7(3) . . ? O1 S1 O3 113.6(3) . . ? O2 S1 O3 114.5(3) . . ? O1 S1 C39 104.1(3) . . ? O2 S1 C39 103.0(3) . . ? O3 S1 C39 105.2(3) . . ? O6 S2 O4 118.1(6) . . ? O6 S2 O5 114.5(5) . . ? O4 S2 O5 114.3(4) . . ? O6 S2 C40 102.5(4) . . ? O4 S2 C40 101.0(6) . . ? O5 S2 C40 103.3(4) . . ? O7 S3 O8 115.6(3) . . ? O7 S3 O9 108.6(5) . . ? O8 S3 O9 122.9(5) . . ? O7 S3 C41 105.2(4) . . ? O8 S3 C41 98.6(4) . . ? O9 S3 C41 102.9(6) . . ? O7 S3B O9B 110.4(5) . . ? O7 S3B O8 111.8(3) . . ? O9B S3B O8 122.7(5) . . ? O7 S3B C41B 109.4(5) . . ? O9B S3B C41B 101.8(5) . . ? O8 S3B C41B 98.8(4) . . ? C1 Au1 C1 180.00(19) . 2_655 ? C1 Au1 Au2 91.10(13) . . ? C1 Au1 Au2 88.90(13) 2_655 . ? C1 Au1 Au2 88.90(13) . 2_655 ? C1 Au1 Au2 91.10(13) 2_655 2_655 ? Au2 Au1 Au2 180.000(19) . 2_655 ? P1 Au2 P2 178.69(5) . . ? P1 Au2 Au1 89.80(4) . . ? P2 Au2 Au1 90.09(3) . . ? C20 Au3 C20 180.000(2) 2_666 . ? C20 Au3 Au4 90.14(10) 2_666 2_666 ? C20 Au3 Au4 89.86(10) . 2_666 ? C20 Au3 Au4 89.86(10) 2_666 . ? C20 Au3 Au4 90.14(10) . . ? Au4 Au3 Au4 180.0 2_666 . ? P3 Au4 P4 179.59(4) . 2_666 ? P3 Au4 Au3 89.65(3) . . ? P4 Au4 Au3 89.99(3) 2_666 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C2 C3 N2 -0.8(7) . . . . ? N3 C21 C22 N4 -0.1(6) . . . . ? N2 C1 N1 C2 1.1(6) . . . . ? Au1 C1 N1 C2 -179.7(4) . . . . ? N2 C1 N1 P1 178.1(4) . . . . ? Au1 C1 N1 P1 -2.6(6) . . . . ? C3 C2 N1 C1 -0.1(7) . . . . ? C3 C2 N1 P1 -177.3(4) . . . . ? N1 C1 N2 C3 -1.6(6) . . . . ? Au1 C1 N2 C3 179.2(4) . . . . ? N1 C1 N2 P2 179.4(3) . . . 2_655 ? Au1 C1 N2 P2 0.2(6) . . . 2_655 ? C2 C3 N2 C1 1.5(7) . . . . ? C2 C3 N2 P2 -179.5(4) . . . 2_655 ? N4 C20 N3 C21 -0.2(5) . . . . ? Au3 C20 N3 C21 175.8(3) . . . . ? N4 C20 N3 P3 174.2(3) . . . . ? Au3 C20 N3 P3 -9.8(5) . . . . ? C22 C21 N3 C20 0.2(5) . . . . ? C22 C21 N3 P3 -174.2(4) . . . . ? N3 C20 N4 C22 0.1(5) . . . . ? Au3 C20 N4 C22 -175.9(3) . . . . ? N3 C20 N4 P4 -176.9(3) . . . . ? Au3 C20 N4 P4 7.1(6) . . . . ? C21 C22 N4 C20 0.0(6) . . . . ? C21 C22 N4 P4 177.0(4) . . . . ? F9 C41 F7 C41B -169.6(14) . . . . ? F8 C41 F7 C41B 74.2(10) . . . . ? S3 C41 F7 C41B -45.0(8) . . . . ? F9B C41B F7 C41 159.6(14) . . . . ? F8B C41B F7 C41 -82.3(11) . . . . ? S3B C41B F7 C41 38.0(8) . . . . ? C1 N1 P1 C4 -115.0(5) . . . . ? C2 N1 P1 C4 61.6(5) . . . . ? C1 N1 P1 C8 120.8(5) . . . . ? C2 N1 P1 C8 -62.6(6) . . . . ? C1 N1 P1 Au2 3.3(5) . . . . ? C2 N1 P1 Au2 179.8(5) . . . . ? C7 C4 P1 N1 167.7(6) . . . . ? C5 C4 P1 N1 -69.9(6) . . . . ? C6 C4 P1 N1 50.9(8) . . . . ? C7 C4 P1 C8 -77.8(7) . . . . ? C5 C4 P1 C8 44.6(7) . . . . ? C6 C4 P1 C8 165.4(8) . . . . ? C7 C4 P1 Au2 52.3(6) . . . . ? C5 C4 P1 Au2 174.7(5) . . . . ? C6 C4 P1 Au2 -64.6(8) . . . . ? C9 C8 P1 N1 -176.6(6) . . . . ? C10 C8 P1 N1 -58.7(5) . . . . ? C11 C8 P1 N1 61.0(6) . . . . ? C9 C8 P1 C4 69.5(7) . . . . ? C10 C8 P1 C4 -172.5(5) . . . . ? C11 C8 P1 C4 -52.9(7) . . . . ? C9 C8 P1 Au2 -61.0(6) . . . . ? C10 C8 P1 Au2 56.9(5) . . . . ? C11 C8 P1 Au2 176.6(5) . . . . ? C17 C16 P2 N2 -75.3(5) . . . 2_655 ? C18 C16 P2 N2 165.1(4) . . . 2_655 ? C19 C16 P2 N2 48.7(5) . . . 2_655 ? C17 C16 P2 C12 39.2(6) . . . . ? C18 C16 P2 C12 -80.4(5) . . . . ? C19 C16 P2 C12 163.2(4) . . . . ? C17 C16 P2 Au2 169.0(4) . . . . ? C18 C16 P2 Au2 49.4(5) . . . . ? C19 C16 P2 Au2 -67.0(4) . . . . ? C14 C12 P2 N2 66.5(5) . . . 2_655 ? C15 C12 P2 N2 -171.8(4) . . . 2_655 ? C13 C12 P2 N2 -55.6(4) . . . 2_655 ? C14 C12 P2 C16 -48.4(5) . . . . ? C15 C12 P2 C16 73.4(5) . . . . ? C13 C12 P2 C16 -170.5(4) . . . . ? C14 C12 P2 Au2 -179.3(4) . . . . ? C15 C12 P2 Au2 -57.5(4) . . . . ? C13 C12 P2 Au2 58.6(4) . . . . ? C20 N3 P3 C27 -107.2(4) . . . . ? C21 N3 P3 C27 66.2(4) . . . . ? C20 N3 P3 C23 129.3(4) . . . . ? C21 N3 P3 C23 -57.2(4) . . . . ? C20 N3 P3 Au4 10.7(4) . . . . ? C21 N3 P3 Au4 -175.9(3) . . . . ? C28 C27 P3 N3 63.5(4) . . . . ? C29 C27 P3 N3 179.8(3) . . . . ? C30 C27 P3 N3 -57.4(5) . . . . ? C28 C27 P3 C23 179.5(4) . . . . ? C29 C27 P3 C23 -64.2(4) . . . . ? C30 C27 P3 C23 58.6(5) . . . . ? C28 C27 P3 Au4 -52.0(4) . . . . ? C29 C27 P3 Au4 64.3(4) . . . . ? C30 C27 P3 Au4 -173.0(4) . . . . ? C24 C23 P3 N3 -52.4(4) . . . . ? C26 C23 P3 N3 71.9(6) . . . . ? C25 C23 P3 N3 -168.4(4) . . . . ? C24 C23 P3 C27 -167.3(4) . . . . ? C26 C23 P3 C27 -42.9(6) . . . . ? C25 C23 P3 C27 76.7(4) . . . . ? C24 C23 P3 Au4 64.2(4) . . . . ? C26 C23 P3 Au4 -171.5(5) . . . . ? C25 C23 P3 Au4 -51.9(4) . . . . ? C20 N4 P4 C31 108.8(4) . . . . ? C22 N4 P4 C31 -67.7(5) . . . . ? C20 N4 P4 C35 -126.6(4) . . . . ? C22 N4 P4 C35 56.9(5) . . . . ? C20 N4 P4 Au4 -8.6(4) . . . 2_666 ? C22 N4 P4 Au4 174.9(4) . . . 2_666 ? C33 C31 P4 N4 -56.7(4) . . . . ? C32 C31 P4 N4 65.7(6) . . . . ? C34 C31 P4 N4 -172.6(4) . . . . ? C33 C31 P4 C35 -172.5(4) . . . . ? C32 C31 P4 C35 -50.1(6) . . . . ? C34 C31 P4 C35 71.6(4) . . . . ? C33 C31 P4 Au4 58.5(4) . . . 2_666 ? C32 C31 P4 Au4 -179.0(5) . . . 2_666 ? C34 C31 P4 Au4 -57.3(4) . . . 2_666 ? C37 C35 P4 N4 61.7(4) . . . . ? C36 C35 P4 N4 177.8(4) . . . . ? C38 C35 P4 N4 -61.6(7) . . . . ? C37 C35 P4 C31 177.3(4) . . . . ? C36 C35 P4 C31 -66.6(4) . . . . ? C38 C35 P4 C31 54.0(7) . . . . ? C37 C35 P4 Au4 -54.0(4) . . . 2_666 ? C36 C35 P4 Au4 62.1(4) . . . 2_666 ? C38 C35 P4 Au4 -177.3(6) . . . 2_666 ? F3 C39 S1 O1 -60.2(6) . . . . ? F1 C39 S1 O1 179.0(6) . . . . ? F2 C39 S1 O1 59.5(6) . . . . ? F3 C39 S1 O2 59.8(6) . . . . ? F1 C39 S1 O2 -61.0(6) . . . . ? F2 C39 S1 O2 179.6(5) . . . . ? F3 C39 S1 O3 180.0(6) . . . . ? F1 C39 S1 O3 59.2(7) . . . . ? F2 C39 S1 O3 -60.2(6) . . . . ? F6 C40 S2 O6 -172.7(8) . . . . ? F4 C40 S2 O6 -53.3(8) . . . . ? F5 C40 S2 O6 66.8(8) . . . . ? F6 C40 S2 O4 65.1(8) . . . . ? F4 C40 S2 O4 -175.6(7) . . . . ? F5 C40 S2 O4 -55.4(8) . . . . ? F6 C40 S2 O5 -53.4(8) . . . . ? F4 C40 S2 O5 65.9(8) . . . . ? F5 C40 S2 O5 -173.9(7) . . . . ? S3B O7 S3 O8 -66.1(4) . . . . ? S3B O7 S3 O9 151.0(5) . . . . ? S3B O7 S3 C41 41.5(5) . . . . ? S3B O8 S3 O7 59.8(4) . . . . ? S3B O8 S3 O9 -163.2(6) . . . . ? S3B O8 S3 C41 -51.7(4) . . . . ? F9 C41 S3 O7 -66.3(8) . . . . ? F8 C41 S3 O7 54.0(9) . . . . ? F7 C41 S3 O7 169.1(7) . . . . ? F9 C41 S3 O8 53.4(8) . . . . ? F8 C41 S3 O8 173.7(8) . . . . ? F7 C41 S3 O8 -71.3(8) . . . . ? F9 C41 S3 O9 -179.9(8) . . . . ? F8 C41 S3 O9 -59.6(9) . . . . ? F7 C41 S3 O9 55.4(9) . . . . ? S3 O7 S3B O9B -163.9(5) . . . . ? S3 O7 S3B O8 55.7(3) . . . . ? S3 O7 S3B C41B -52.7(4) . . . . ? S3 O8 S3B O7 -60.4(4) . . . . ? S3 O8 S3B O9B 164.8(6) . . . . ? S3 O8 S3B C41B 54.6(4) . . . . ? F9B C41B S3B O7 64.8(8) . . . . ? F8B C41B S3B O7 -54.7(8) . . . . ? F7 C41B S3B O7 -173.6(6) . . . . ? F9B C41B S3B O9B -178.4(8) . . . . ? F8B C41B S3B O9B 62.1(9) . . . . ? F7 C41B S3B O9B -56.8(8) . . . . ? F9B C41B S3B O8 -52.1(8) . . . . ? F8B C41B S3B O8 -171.7(7) . . . . ? F7 C41B S3B O8 69.4(7) . . . . ? N2 C1 Au1 Au2 179.6(4) . . . . ? N1 C1 Au1 Au2 0.5(4) . . . . ? N2 C1 Au1 Au2 -0.4(4) . . . 2_655 ? N1 C1 Au1 Au2 -179.5(4) . . . 2_655 ? N1 P1 Au2 Au1 -1.96(17) . . . . ? C4 P1 Au2 Au1 110.7(3) . . . . ? C8 P1 Au2 Au1 -115.38(19) . . . . ? N2 P2 Au2 Au1 0.36(15) 2_655 . . . ? C16 P2 Au2 Au1 113.9(2) . . . . ? C12 P2 Au2 Au1 -111.1(2) . . . . ? C1 Au1 Au2 P1 0.95(12) . . . . ? C1 Au1 Au2 P1 -179.05(12) 2_655 . . . ? C1 Au1 Au2 P2 179.65(12) . . . . ? C1 Au1 Au2 P2 -0.35(12) 2_655 . . . ? N3 C20 Au3 Au4 -176.8(4) . . . 2_666 ? N4 C20 Au3 Au4 -1.6(4) . . . 2_666 ? N3 C20 Au3 Au4 3.2(4) . . . . ? N4 C20 Au3 Au4 178.4(4) . . . . ? N3 P3 Au4 Au3 -5.95(14) . . . . ? C27 P3 Au4 Au3 107.07(17) . . . . ? C23 P3 Au4 Au3 -121.3(2) . . . . ? C20 Au3 Au4 P3 -177.73(12) 2_666 . . . ? C20 Au3 Au4 P3 2.27(12) . . . . ? C20 Au3 Au4 P4 2.47(12) 2_666 . . 2_666 ? C20 Au3 Au4 P4 -177.53(12) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 31.24 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 3.030 _refine_diff_density_min -4.035 _refine_diff_density_rms 0.165 _database_code_depnum_ccdc_archive 'CCDC 963089'