# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Wright, Dominic' _publ_contact_author_name 'Dr Dominic Wright' _publ_contact_author_email DSW1000@CAM.AC.UK _publ_section_title ; Group 11 complexes containing the [C5(CN)5]- ligand; 'coordination-analogues' of molecular organometallic systems ; # Attachment '- Compound3.cif' data_dw1137 _database_code_depnum_ccdc_archive 'CCDC 866130' #TrackingRef '- Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C93 H63 Cu2 N11 O2 P4' _chemical_formula_weight 1617.50 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' 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' P P 0.1023 0.0942 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0066(2) _cell_length_b 12.5966(2) _cell_length_c 16.6026(3) _cell_angle_alpha 98.7170(10) _cell_angle_beta 100.8340(10) _cell_angle_gamma 113.5480(10) _cell_volume 2005.84(6) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 31460 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.668 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 34368 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 30.07 _reflns_number_total 11695 _reflns_number_gt 8414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.2691P] 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 11695 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1203 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 Cu1 Cu 0.08700(3) 0.61532(2) 0.211383(16) 0.02290(7) Uani 1 1 d . . . P1 P 0.26816(5) 0.76199(5) 0.31591(3) 0.02185(11) Uani 1 1 d . . . P2 P -0.11368(6) 0.48423(5) 0.23395(4) 0.02435(12) Uani 1 1 d . . . N1 N -0.01971(19) 0.31130(16) -0.12286(12) 0.0274(4) Uani 1 1 d . . . N2 N 0.14163(19) 0.49848(17) 0.14526(12) 0.0275(4) Uani 1 1 d . . . N3 N 0.3006(2) 0.2879(2) 0.28531(15) 0.0470(6) Uani 1 1 d . . . N4 N 0.2535(2) -0.0245(2) 0.10477(16) 0.0460(6) Uani 1 1 d . . . N5 N 0.0696(2) -0.0121(2) -0.15479(14) 0.0422(5) Uani 1 1 d . . . C1 C 0.0337(2) 0.27921(19) -0.07234(14) 0.0250(4) Uani 1 1 d . . . C2 C 0.1454(2) 0.41202(19) 0.11555(13) 0.0244(4) Uani 1 1 d . . . C3 C 0.2589(2) 0.2671(2) 0.21330(15) 0.0303(5) Uani 1 1 d . . . C4 C 0.2273(2) 0.0491(2) 0.08602(15) 0.0302(5) Uani 1 1 d . . . C5 C 0.0961(2) 0.0578(2) -0.09314(15) 0.0297(5) Uani 1 1 d . . . C11 C 0.1006(2) 0.24368(19) -0.00737(13) 0.0236(4) Uani 1 1 d . . . C12 C 0.1491(2) 0.30419(18) 0.07934(13) 0.0238(4) Uani 1 1 d . . . C13 C 0.2052(2) 0.23997(19) 0.12400(14) 0.0243(4) Uani 1 1 d . . . C14 C 0.1915(2) 0.14066(19) 0.06495(14) 0.0249(4) Uani 1 1 d . . . C15 C 0.1274(2) 0.14261(19) -0.01628(13) 0.0244(4) Uani 1 1 d . . . C21 C 0.3393(2) 0.71007(19) 0.40151(13) 0.0233(4) Uani 1 1 d . . . C22 C 0.4521(2) 0.7873(2) 0.46978(14) 0.0294(5) Uani 1 1 d . . . H22 H 0.4942 0.8706 0.4732 0.035 Uiso 1 1 calc R . . C23 C 0.5030(3) 0.7433(2) 0.53252(15) 0.0349(5) Uani 1 1 d . . . H23 H 0.5787 0.7966 0.5795 0.042 Uiso 1 1 calc R . . C24 C 0.4440(3) 0.6216(2) 0.52716(16) 0.0371(6) Uani 1 1 d . . . H24 H 0.4792 0.5917 0.5704 0.044 Uiso 1 1 calc R . . C25 C 0.3341(3) 0.5439(2) 0.45897(17) 0.0378(6) Uani 1 1 d . . . H25 H 0.2945 0.4604 0.4549 0.045 Uiso 1 1 calc R . . C26 C 0.2812(2) 0.5880(2) 0.39617(15) 0.0288(5) Uani 1 1 d . . . H26 H 0.2052 0.5344 0.3495 0.035 Uiso 1 1 calc R . . C31 C 0.2211(2) 0.87336(18) 0.36668(14) 0.0243(4) Uani 1 1 d . . . C32 C 0.2292(2) 0.9006(2) 0.45222(14) 0.0283(5) Uani 1 1 d . . . H32 H 0.2648 0.8626 0.4889 0.034 Uiso 1 1 calc R . . C33 C 0.1852(3) 0.9836(2) 0.48462(16) 0.0346(5) Uani 1 1 d . . . H33 H 0.1911 1.0022 0.5433 0.042 Uiso 1 1 calc R . . C34 C 0.1330(3) 1.0387(2) 0.43138(18) 0.0404(6) Uani 1 1 d . . . H34 H 0.1030 1.0952 0.4535 0.048 Uiso 1 1 calc R . . C35 C 0.1244(3) 1.0119(2) 0.34600(18) 0.0431(6) Uani 1 1 d . . . H35 H 0.0883 1.0499 0.3096 0.052 Uiso 1 1 calc R . . C36 C 0.1680(3) 0.9301(2) 0.31342(15) 0.0340(5) Uani 1 1 d . . . H36 H 0.1620 0.9122 0.2547 0.041 Uiso 1 1 calc R . . C41 C 0.4235(2) 0.8549(2) 0.28802(13) 0.0259(4) Uani 1 1 d . . . C42 C 0.4939(3) 0.9784(2) 0.31911(16) 0.0364(5) Uani 1 1 d . . . H42 H 0.4589 1.0192 0.3542 0.044 Uiso 1 1 calc R . . C43 C 0.6147(3) 1.0423(3) 0.29925(19) 0.0473(7) Uani 1 1 d . . . H43 H 0.6625 1.1268 0.3207 0.057 Uiso 1 1 calc R . . C44 C 0.6659(3) 0.9834(3) 0.24830(19) 0.0502(7) Uani 1 1 d . . . H44 H 0.7488 1.0274 0.2347 0.060 Uiso 1 1 calc R . . C45 C 0.5975(3) 0.8617(3) 0.21736(19) 0.0490(7) Uani 1 1 d . . . H45 H 0.6333 0.8214 0.1826 0.059 Uiso 1 1 calc R . . C46 C 0.4758(3) 0.7969(2) 0.23664(16) 0.0371(5) Uani 1 1 d . . . H46 H 0.4281 0.7126 0.2145 0.045 Uiso 1 1 calc R . . C51 C -0.0914(2) 0.39821(19) 0.31015(14) 0.0263(4) Uani 1 1 d . . . C52 C -0.0317(3) 0.3218(2) 0.29195(17) 0.0355(5) Uani 1 1 d . . . H52 H -0.0118 0.3105 0.2389 0.043 Uiso 1 1 calc R . . C53 C -0.0012(3) 0.2624(2) 0.35024(19) 0.0417(6) Uani 1 1 d . . . H53 H 0.0402 0.2111 0.3373 0.050 Uiso 1 1 calc R . . C54 C -0.0306(3) 0.2775(2) 0.42715(17) 0.0385(6) Uani 1 1 d . . . H54 H -0.0081 0.2376 0.4676 0.046 Uiso 1 1 calc R . . C55 C -0.0926(3) 0.3504(2) 0.44523(16) 0.0377(6) Uani 1 1 d . . . H55 H -0.1150 0.3593 0.4976 0.045 Uiso 1 1 calc R . . C56 C -0.1224(2) 0.4112(2) 0.38721(15) 0.0318(5) Uani 1 1 d . . . H56 H -0.1644 0.4620 0.4004 0.038 Uiso 1 1 calc R . . C61 C -0.2319(2) 0.3653(2) 0.14019(15) 0.0298(5) Uani 1 1 d . . . C62 C -0.3344(3) 0.2587(2) 0.14553(18) 0.0407(6) Uani 1 1 d . . . H62 H -0.3462 0.2469 0.1992 0.049 Uiso 1 1 calc R . . C63 C -0.4187(3) 0.1704(2) 0.0725(2) 0.0483(7) Uani 1 1 d . . . H63 H -0.4894 0.0986 0.0764 0.058 Uiso 1 1 calc R . . C64 C -0.4016(3) 0.1850(3) -0.0060(2) 0.0525(7) Uani 1 1 d . . . H64 H -0.4595 0.1235 -0.0557 0.063 Uiso 1 1 calc R . . C65 C -0.2999(3) 0.2896(3) -0.01150(19) 0.0518(7) Uani 1 1 d . . . H65 H -0.2878 0.3001 -0.0654 0.062 Uiso 1 1 calc R . . C66 C -0.2154(3) 0.3793(2) 0.06052(16) 0.0378(6) Uani 1 1 d . . . H66 H -0.1455 0.4510 0.0559 0.045 Uiso 1 1 calc R . . C71 C -0.2128(2) 0.5561(2) 0.27394(14) 0.0282(5) Uani 1 1 d . . . C72 C -0.3510(3) 0.4977(3) 0.2703(2) 0.0497(7) Uani 1 1 d . . . H72 H -0.4023 0.4154 0.2416 0.060 Uiso 1 1 calc R . . C73 C -0.4153(3) 0.5578(3) 0.3078(2) 0.0554(8) Uani 1 1 d . . . H73 H -0.5102 0.5164 0.3048 0.067 Uiso 1 1 calc R . . C74 C -0.3435(3) 0.6760(3) 0.34913(19) 0.0487(7) Uani 1 1 d . . . H74 H -0.3877 0.7168 0.3753 0.058 Uiso 1 1 calc R . . C75 C -0.2068(3) 0.7355(3) 0.3527(2) 0.0653(10) Uani 1 1 d . . . H75 H -0.1561 0.8178 0.3814 0.078 Uiso 1 1 calc R . . C76 C -0.1424(3) 0.6756(3) 0.3145(2) 0.0500(7) Uani 1 1 d . . . H76 H -0.0481 0.7180 0.3165 0.060 Uiso 1 1 calc R . . C1S C -0.5210(12) 0.4603(9) -0.0381(5) 0.200(4) Uiso 0.50 1 d P . 1 N1S N -0.5210(12) 0.4603(9) -0.0381(5) 0.200(4) Uiso 0.50 1 d P . 2 O1S O -0.6293(12) 0.3800(10) -0.0656(7) 0.167(4) Uiso 0.50 1 d P . . O2S O -0.4450(10) 0.4766(9) -0.0887(7) 0.155(3) Uiso 0.50 1 d P . . H1A H -0.4473 0.4925 -0.0657 0.233 Uiso 0.50 1 d P A 1 H1B H -0.5381 0.3845 -0.0339 0.233 Uiso 0.50 1 d P B 1 H1C H -0.6013 0.4641 -0.0712 0.233 Uiso 0.50 1 d P C 1 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 Cu1 0.02672(13) 0.02033(13) 0.02058(13) 0.00418(10) 0.00523(10) 0.01022(11) P1 0.0251(3) 0.0194(3) 0.0199(3) 0.0034(2) 0.0046(2) 0.0099(2) P2 0.0266(3) 0.0218(3) 0.0253(3) 0.0060(2) 0.0085(2) 0.0106(2) N1 0.0335(10) 0.0229(9) 0.0242(10) 0.0053(8) 0.0057(8) 0.0121(8) N2 0.0312(9) 0.0255(10) 0.0251(10) 0.0032(8) 0.0067(8) 0.0135(8) N3 0.0517(14) 0.0496(14) 0.0317(12) 0.0090(10) -0.0001(10) 0.0201(12) N4 0.0503(13) 0.0413(13) 0.0583(15) 0.0196(12) 0.0148(12) 0.0295(12) N5 0.0479(13) 0.0411(13) 0.0366(12) -0.0001(10) 0.0143(10) 0.0209(11) C1 0.0295(11) 0.0202(10) 0.0238(11) 0.0030(8) 0.0083(9) 0.0099(9) C2 0.0256(10) 0.0243(11) 0.0213(10) 0.0061(8) 0.0051(8) 0.0096(9) C3 0.0295(11) 0.0270(11) 0.0307(12) 0.0066(9) 0.0031(9) 0.0112(10) C4 0.0303(11) 0.0285(12) 0.0333(12) 0.0084(10) 0.0070(10) 0.0149(10) C5 0.0332(12) 0.0278(12) 0.0303(12) 0.0073(10) 0.0097(10) 0.0152(10) C11 0.0266(10) 0.0226(10) 0.0215(10) 0.0057(8) 0.0053(8) 0.0112(9) C12 0.0274(10) 0.0208(10) 0.0228(10) 0.0045(8) 0.0062(8) 0.0110(9) C13 0.0249(10) 0.0223(10) 0.0242(11) 0.0061(8) 0.0044(8) 0.0097(9) C14 0.0260(10) 0.0222(10) 0.0280(11) 0.0071(9) 0.0071(9) 0.0121(9) C15 0.0273(10) 0.0219(10) 0.0239(11) 0.0039(8) 0.0076(8) 0.0111(9) C21 0.0254(10) 0.0243(10) 0.0215(10) 0.0045(8) 0.0070(8) 0.0124(9) C22 0.0305(11) 0.0287(12) 0.0266(11) 0.0032(9) 0.0034(9) 0.0141(10) C23 0.0349(12) 0.0421(14) 0.0248(12) 0.0031(10) -0.0010(10) 0.0201(11) C24 0.0430(14) 0.0468(15) 0.0306(13) 0.0153(11) 0.0069(11) 0.0282(13) C25 0.0411(13) 0.0338(13) 0.0437(15) 0.0187(12) 0.0102(12) 0.0190(12) C26 0.0292(11) 0.0256(11) 0.0277(12) 0.0049(9) 0.0021(9) 0.0114(9) C31 0.0244(10) 0.0194(10) 0.0272(11) 0.0042(8) 0.0056(8) 0.0090(8) C32 0.0324(11) 0.0267(11) 0.0269(11) 0.0062(9) 0.0091(9) 0.0136(10) C33 0.0424(13) 0.0321(13) 0.0316(13) 0.0037(10) 0.0144(11) 0.0184(11) C34 0.0494(15) 0.0310(13) 0.0458(16) 0.0033(11) 0.0125(12) 0.0252(12) C35 0.0565(16) 0.0339(14) 0.0445(16) 0.0082(12) 0.0049(13) 0.0300(13) C36 0.0464(14) 0.0303(12) 0.0263(12) 0.0044(10) 0.0045(10) 0.0214(11) C41 0.0275(10) 0.0272(11) 0.0203(10) 0.0061(9) 0.0046(8) 0.0101(9) C42 0.0368(13) 0.0296(13) 0.0345(13) 0.0046(10) 0.0124(11) 0.0065(11) C43 0.0434(15) 0.0365(15) 0.0491(17) 0.0127(13) 0.0153(13) 0.0030(12) C44 0.0363(14) 0.0574(19) 0.0489(17) 0.0175(15) 0.0210(13) 0.0075(14) C45 0.0441(15) 0.0589(19) 0.0453(17) 0.0097(14) 0.0224(13) 0.0207(14) C46 0.0370(13) 0.0362(14) 0.0352(14) 0.0047(11) 0.0132(11) 0.0133(11) C51 0.0262(10) 0.0223(11) 0.0298(12) 0.0083(9) 0.0087(9) 0.0093(9) C52 0.0451(14) 0.0314(13) 0.0436(15) 0.0178(11) 0.0251(12) 0.0217(11) C53 0.0490(15) 0.0355(14) 0.0582(18) 0.0238(13) 0.0265(14) 0.0265(13) C54 0.0425(14) 0.0329(13) 0.0454(15) 0.0212(12) 0.0126(12) 0.0174(12) C55 0.0460(14) 0.0386(14) 0.0314(13) 0.0145(11) 0.0148(11) 0.0177(12) C56 0.0396(13) 0.0281(12) 0.0328(13) 0.0080(10) 0.0144(10) 0.0178(11) C61 0.0288(11) 0.0251(11) 0.0319(12) 0.0034(9) 0.0059(9) 0.0108(10) C62 0.0391(13) 0.0289(13) 0.0455(16) 0.0073(11) 0.0128(12) 0.0066(11) C63 0.0416(15) 0.0254(13) 0.061(2) 0.0017(12) 0.0099(14) 0.0035(11) C64 0.0503(17) 0.0372(15) 0.0469(18) -0.0066(13) -0.0015(14) 0.0090(13) C65 0.0560(18) 0.0432(16) 0.0333(15) 0.0003(12) 0.0021(13) 0.0072(14) C66 0.0377(13) 0.0312(13) 0.0316(13) 0.0051(10) 0.0039(11) 0.0060(11) C71 0.0304(11) 0.0292(12) 0.0303(12) 0.0103(9) 0.0100(9) 0.0168(10) C72 0.0349(13) 0.0326(14) 0.086(2) 0.0142(14) 0.0260(15) 0.0152(12) C73 0.0429(15) 0.0531(19) 0.092(3) 0.0301(18) 0.0374(17) 0.0296(15) C74 0.0544(17) 0.0616(19) 0.0517(18) 0.0151(15) 0.0229(14) 0.0427(16) C75 0.0452(17) 0.0536(19) 0.082(3) -0.0245(17) 0.0076(16) 0.0261(15) C76 0.0312(13) 0.0407(15) 0.067(2) -0.0104(14) 0.0105(13) 0.0147(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.0280(18) 2_565 ? Cu1 N2 2.0491(18) . ? Cu1 P1 2.2770(6) . ? Cu1 P2 2.3088(6) . ? P1 C31 1.825(2) . ? P1 C21 1.826(2) . ? P1 C41 1.836(2) . ? P2 C71 1.824(2) . ? P2 C61 1.826(2) . ? P2 C51 1.829(2) . ? N1 C1 1.149(3) . ? N1 Cu1 2.0280(18) 2_565 ? N2 C2 1.146(3) . ? N3 C3 1.145(3) . ? N4 C4 1.142(3) . ? N5 C5 1.148(3) . ? C1 C11 1.420(3) . ? C2 C12 1.419(3) . ? C3 C13 1.421(3) . ? C4 C14 1.429(3) . ? C5 C15 1.419(3) . ? C11 C15 1.411(3) . ? C11 C12 1.411(3) . ? C12 C13 1.412(3) . ? C13 C14 1.404(3) . ? C14 C15 1.408(3) . ? C21 C26 1.391(3) . ? C21 C22 1.394(3) . ? C22 C23 1.382(3) . ? C22 H22 0.9500 . ? C23 C24 1.385(4) . ? C23 H23 0.9500 . ? C24 C25 1.381(4) . ? C24 H24 0.9500 . ? C25 C26 1.393(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.387(3) . ? C31 C36 1.402(3) . ? C32 C33 1.397(3) . ? C32 H32 0.9500 . ? C33 C34 1.380(3) . ? C33 H33 0.9500 . ? C34 C35 1.382(4) . ? C34 H34 0.9500 . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C46 1.386(3) . ? C41 C42 1.390(3) . ? C42 C43 1.384(4) . ? C42 H42 0.9500 . ? C43 C44 1.381(4) . ? C43 H43 0.9500 . ? C44 C45 1.369(4) . ? C44 H44 0.9500 . ? C45 C46 1.389(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.388(3) . ? C51 C52 1.393(3) . ? C52 C53 1.381(3) . ? C52 H52 0.9500 . ? C53 C54 1.379(4) . ? C53 H53 0.9500 . ? C54 C55 1.376(4) . ? C54 H54 0.9500 . ? C55 C56 1.388(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C62 1.394(3) . ? C61 C66 1.396(3) . ? C62 C63 1.383(4) . ? C62 H62 0.9500 . ? C63 C64 1.379(4) . ? C63 H63 0.9500 . ? C64 C65 1.376(4) . ? C64 H64 0.9500 . ? C65 C66 1.380(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.373(3) . ? C71 C72 1.384(3) . ? C72 C73 1.383(4) . ? C72 H72 0.9500 . ? C73 C74 1.363(4) . ? C73 H73 0.9500 . ? C74 C75 1.372(4) . ? C74 H74 0.9500 . ? C75 C76 1.386(4) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C1S O1S 1.160(12) . ? C1S O2S 1.275(12) . ? C1S C1S 1.357(16) 2_465 ? C1S H1A 0.982(12) . ? C1S H1B 0.914(10) . ? C1S H1C 0.972(10) . ? O1S H1B 1.018(11) . ? O1S H1C 1.002(11) . ? O2S H1A 0.413(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 Cu1 N2 104.07(7) 2_565 . ? N1 Cu1 P1 109.59(5) 2_565 . ? N2 Cu1 P1 112.52(6) . . ? N1 Cu1 P2 103.50(6) 2_565 . ? N2 Cu1 P2 100.97(5) . . ? P1 Cu1 P2 124.13(2) . . ? C31 P1 C21 105.74(10) . . ? C31 P1 C41 102.36(10) . . ? C21 P1 C41 101.87(9) . . ? C31 P1 Cu1 111.67(7) . . ? C21 P1 Cu1 114.87(7) . . ? C41 P1 Cu1 118.76(7) . . ? C71 P2 C61 106.47(11) . . ? C71 P2 C51 103.95(10) . . ? C61 P2 C51 101.54(10) . . ? C71 P2 Cu1 113.95(8) . . ? C61 P2 Cu1 114.16(8) . . ? C51 P2 Cu1 115.44(7) . . ? C1 N1 Cu1 171.95(18) . 2_565 ? C2 N2 Cu1 161.72(18) . . ? N1 C1 C11 177.7(2) . . ? N2 C2 C12 179.3(2) . . ? N3 C3 C13 179.1(3) . . ? N4 C4 C14 177.8(3) . . ? N5 C5 C15 179.0(3) . . ? C15 C11 C12 107.97(18) . . ? C15 C11 C1 127.3(2) . . ? C12 C11 C1 124.73(19) . . ? C13 C12 C11 107.97(18) . . ? C13 C12 C2 125.7(2) . . ? C11 C12 C2 126.32(18) . . ? C14 C13 C12 107.83(19) . . ? C14 C13 C3 125.94(19) . . ? C12 C13 C3 126.1(2) . . ? C13 C14 C15 108.46(17) . . ? C13 C14 C4 124.8(2) . . ? C15 C14 C4 126.5(2) . . ? C11 C15 C14 107.77(18) . . ? C11 C15 C5 126.39(19) . . ? C14 C15 C5 125.83(19) . . ? C26 C21 C22 119.15(19) . . ? C26 C21 P1 118.20(16) . . ? C22 C21 P1 122.61(16) . . ? C23 C22 C21 120.4(2) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 120.2(2) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 120.0(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.3(2) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C32 C31 C36 119.1(2) . . ? C32 C31 P1 124.45(16) . . ? C36 C31 P1 116.42(17) . . ? C31 C32 C33 120.3(2) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 120.0(2) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.1(2) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C31 120.3(2) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C46 C41 C42 119.1(2) . . ? C46 C41 P1 117.57(18) . . ? C42 C41 P1 123.28(18) . . ? C43 C42 C41 120.3(2) . . ? C43 C42 H42 119.9 . . ? C41 C42 H42 119.9 . . ? C44 C43 C42 120.0(3) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C45 C44 C43 120.2(2) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.2(3) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C41 C46 C45 120.3(2) . . ? C41 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? C56 C51 C52 118.6(2) . . ? C56 C51 P2 123.35(16) . . ? C52 C51 P2 117.90(17) . . ? C53 C52 C51 120.6(2) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C54 C53 C52 120.2(2) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 119.8(2) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C56 120.2(2) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C55 C56 C51 120.5(2) . . ? C55 C56 H56 119.8 . . ? C51 C56 H56 119.8 . . ? C62 C61 C66 118.8(2) . . ? C62 C61 P2 122.36(19) . . ? C66 C61 P2 118.81(18) . . ? C63 C62 C61 119.9(3) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? C62 C63 C64 120.9(3) . . ? C62 C63 H63 119.5 . . ? C64 C63 H63 119.5 . . ? C65 C64 C63 119.4(3) . . ? C65 C64 H64 120.3 . . ? C63 C64 H64 120.3 . . ? C64 C65 C66 120.6(3) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C65 C66 C61 120.4(2) . . ? C65 C66 H66 119.8 . . ? C61 C66 H66 119.8 . . ? C76 C71 C72 118.0(2) . . ? C76 C71 P2 117.04(18) . . ? C72 C71 P2 124.84(19) . . ? C71 C72 C73 120.8(3) . . ? C71 C72 H72 119.6 . . ? C73 C72 H72 119.6 . . ? C74 C73 C72 120.4(3) . . ? C74 C73 H73 119.8 . . ? C72 C73 H73 119.8 . . ? C73 C74 C75 119.5(3) . . ? C73 C74 H74 120.3 . . ? C75 C74 H74 120.3 . . ? C76 C75 C74 120.1(3) . . ? C76 C75 H75 119.9 . . ? C74 C75 H75 119.9 . . ? C71 C76 C75 121.1(3) . . ? C71 C76 H76 119.5 . . ? C75 C76 H76 119.5 . . ? O1S C1S O2S 114.6(11) . . ? O1S C1S C1S 124.5(16) . 2_465 ? O2S C1S C1S 120.6(15) . 2_465 ? O1S C1S H1A 129.3(11) . . ? O2S C1S H1A 15.0(5) . . ? C1S C1S H1A 105.7(13) 2_465 . ? O1S C1S H1B 57.3(8) . . ? O2S C1S H1B 102.0(10) . . ? C1S C1S H1B 113.3(12) 2_465 . ? H1A C1S H1B 111.5(10) . . ? O1S C1S H1C 55.3(8) . . ? O2S C1S H1C 101.2(9) . . ? C1S C1S H1C 106.8(12) 2_465 . ? H1A C1S H1C 106.7(9) . . ? H1B C1S H1C 112.4(11) . . ? C1S O1S H1B 49.1(7) . . ? C1S O1S H1C 52.8(8) . . ? H1B O1S H1C 101.8(11) . . ? C1S O2S H1A 37.9(12) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 30.07 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.749 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.070 # Attachment '- Compound4.cif' data_dw1201 _database_code_depnum_ccdc_archive 'CCDC 866131' #TrackingRef '- Compound4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H45 Ag N5 P3' _chemical_formula_sum 'C64 H45 Ag N5 P3' _chemical_formula_weight 1084.83 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' Ag Ag -0.8971 1.1015 '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 P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6870(1) _cell_length_b 25.7466(2) _cell_length_c 16.6696(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.4460(10) _cell_angle_gamma 90.00 _cell_volume 5435.23(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 42260 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 0.504 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 53107 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 30.03 _reflns_number_total 15813 _reflns_number_gt 11336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+1.6079P] 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 15813 _refine_ls_number_parameters 658 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0830 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Ag1 Ag 0.756512(10) 0.132237(6) 0.244900(8) 0.02600(5) Uani 1 1 d . . . N1 N 0.61349(16) 0.09279(8) 0.31882(11) 0.0470(5) Uani 1 1 d . . . C1 C 0.54902(17) 0.06746(9) 0.34301(12) 0.0346(5) Uani 1 1 d . . . C10 C 0.46886(15) 0.03359(8) 0.36856(12) 0.0309(4) Uani 1 1 d . . . N2 N 0.44466(16) 0.10251(8) 0.55427(12) 0.0469(5) Uani 1 1 d . . . C2 C 0.43133(16) 0.07349(8) 0.50267(13) 0.0326(5) Uani 1 1 d . . . C20 C 0.41453(15) 0.03651(8) 0.43958(12) 0.0289(4) Uani 1 1 d . . . N3 N 0.22480(16) -0.02918(8) 0.55291(12) 0.0483(5) Uani 1 1 d . . . C3 C 0.27671(16) -0.01804(8) 0.50194(13) 0.0334(5) Uani 1 1 d . . . C30 C 0.34278(15) -0.00490(8) 0.43891(12) 0.0289(4) Uani 1 1 d . . . N4 N 0.24790(17) -0.11437(8) 0.32159(13) 0.0532(6) Uani 1 1 d . . . C4 C 0.29406(17) -0.07848(9) 0.34297(13) 0.0360(5) Uani 1 1 d . . . C40 C 0.35207(15) -0.03328(8) 0.36761(12) 0.0296(4) Uani 1 1 d . . . N5 N 0.49917(18) -0.03964(10) 0.19028(13) 0.0604(6) Uani 1 1 d . . . C5 C 0.46791(17) -0.02657(9) 0.24978(13) 0.0395(5) Uani 1 1 d . . . C50 C 0.43032(16) -0.00963(8) 0.32417(12) 0.0310(4) Uani 1 1 d . . . P1 P 0.62666(4) 0.18265(2) 0.15464(3) 0.02551(11) Uani 1 1 d . . . C11 C 0.53208(14) 0.22375(8) 0.20334(11) 0.0274(4) Uani 1 1 d . . . C12 C 0.56285(16) 0.24639(9) 0.27628(12) 0.0360(5) Uani 1 1 d . . . H12 H 0.6301 0.2385 0.3014 0.043 Uiso 1 1 calc R . . C13 C 0.49615(18) 0.28052(9) 0.31302(13) 0.0416(5) Uani 1 1 d . . . H13 H 0.5181 0.2961 0.3629 0.050 Uiso 1 1 calc R . . C14 C 0.39808(17) 0.29175(9) 0.27721(14) 0.0404(5) Uani 1 1 d . . . H14 H 0.3524 0.3152 0.3022 0.048 Uiso 1 1 calc R . . C15 C 0.36650(17) 0.26894(9) 0.20513(14) 0.0420(6) Uani 1 1 d . . . H15 H 0.2987 0.2766 0.1806 0.050 Uiso 1 1 calc R . . C16 C 0.43246(15) 0.23496(9) 0.16801(13) 0.0352(5) Uani 1 1 d . . . H16 H 0.4098 0.2192 0.1184 0.042 Uiso 1 1 calc R . . C21 C 0.54248(14) 0.14383(8) 0.08528(12) 0.0283(4) Uani 1 1 d . . . C22 C 0.52256(16) 0.15651(9) 0.00485(12) 0.0348(5) Uani 1 1 d . . . H22 H 0.5530 0.1870 -0.0161 0.042 Uiso 1 1 calc R . . C23 C 0.45857(18) 0.12513(9) -0.04517(14) 0.0405(5) Uani 1 1 d . . . H23 H 0.4460 0.1340 -0.1002 0.049 Uiso 1 1 calc R . . C24 C 0.41352(18) 0.08150(10) -0.01526(15) 0.0475(6) Uani 1 1 d . . . H24 H 0.3698 0.0600 -0.0496 0.057 Uiso 1 1 calc R . . C25 C 0.4316(2) 0.06880(10) 0.06478(16) 0.0541(7) Uani 1 1 d . . . H25 H 0.3993 0.0389 0.0858 0.065 Uiso 1 1 calc R . . C26 C 0.49672(18) 0.09953(9) 0.11451(14) 0.0425(5) Uani 1 1 d . . . H26 H 0.5101 0.0901 0.1693 0.051 Uiso 1 1 calc R . . C31 C 0.69304(15) 0.22769(8) 0.08964(12) 0.0278(4) Uani 1 1 d . . . C32 C 0.66956(17) 0.28008(8) 0.08294(13) 0.0366(5) Uani 1 1 d . . . H32 H 0.6145 0.2943 0.1122 0.044 Uiso 1 1 calc R . . C33 C 0.72586(19) 0.31192(9) 0.03375(15) 0.0472(6) Uani 1 1 d . . . H33 H 0.7095 0.3479 0.0298 0.057 Uiso 1 1 calc R . . C34 C 0.80512(19) 0.29172(10) -0.00928(15) 0.0468(6) Uani 1 1 d . . . H34 H 0.8430 0.3136 -0.0432 0.056 Uiso 1 1 calc R . . C35 C 0.82971(18) 0.23975(10) -0.00327(14) 0.0459(6) Uani 1 1 d . . . H35 H 0.8844 0.2257 -0.0332 0.055 Uiso 1 1 calc R . . C36 C 0.77457(17) 0.20803(9) 0.04638(14) 0.0393(5) Uani 1 1 d . . . H36 H 0.7926 0.1723 0.0510 0.047 Uiso 1 1 calc R . . P2 P 0.85968(4) 0.06670(2) 0.17019(3) 0.02842(11) Uani 1 1 d . . . C41 C 0.84013(15) 0.07049(8) 0.06077(12) 0.0297(4) Uani 1 1 d . . . C42 C 0.73913(16) 0.06055(8) 0.02685(13) 0.0356(5) Uani 1 1 d . . . H42 H 0.6853 0.0494 0.0601 0.043 Uiso 1 1 calc R . . C43 C 0.71632(19) 0.06678(9) -0.05481(14) 0.0444(6) Uani 1 1 d . . . H43 H 0.6473 0.0598 -0.0774 0.053 Uiso 1 1 calc R . . C44 C 0.7942(2) 0.08324(10) -0.10327(14) 0.0489(6) Uani 1 1 d . . . H44 H 0.7783 0.0882 -0.1592 0.059 Uiso 1 1 calc R . . C45 C 0.8947(2) 0.09251(10) -0.07102(14) 0.0474(6) Uani 1 1 d . . . H45 H 0.9483 0.1032 -0.1049 0.057 Uiso 1 1 calc R . . C46 C 0.91817(17) 0.08633(9) 0.01072(13) 0.0378(5) Uani 1 1 d . . . H46 H 0.9877 0.0929 0.0327 0.045 Uiso 1 1 calc R . . C51 C 1.00202(16) 0.07585(9) 0.18791(12) 0.0338(5) Uani 1 1 d . . . C52 C 1.07329(19) 0.03526(11) 0.19794(18) 0.0578(7) Uani 1 1 d . . . H52 H 1.0490 0.0004 0.1952 0.069 Uiso 1 1 calc R . . C53 C 1.1802(2) 0.04562(13) 0.2119(2) 0.0826(11) Uani 1 1 d . . . H53 H 1.2289 0.0177 0.2180 0.099 Uiso 1 1 calc R . . C54 C 1.2162(2) 0.09598(13) 0.2171(2) 0.0696(9) Uani 1 1 d . . . H54 H 1.2893 0.1027 0.2276 0.083 Uiso 1 1 calc R . . C55 C 1.14659(19) 0.13648(11) 0.20706(16) 0.0502(6) Uani 1 1 d . . . H55 H 1.1715 0.1713 0.2098 0.060 Uiso 1 1 calc R . . C56 C 1.03985(17) 0.12654(9) 0.19299(13) 0.0384(5) Uani 1 1 d . . . H56 H 0.9918 0.1547 0.1867 0.046 Uiso 1 1 calc R . . C61 C 0.83370(16) -0.00161(8) 0.19035(12) 0.0320(4) Uani 1 1 d . . . C62 C 0.85079(18) -0.04094(9) 0.13553(14) 0.0411(5) Uani 1 1 d . . . H62 H 0.8785 -0.0328 0.0853 0.049 Uiso 1 1 calc R . . C63 C 0.8275(2) -0.09175(10) 0.15399(17) 0.0528(7) Uani 1 1 d . . . H63 H 0.8395 -0.1185 0.1163 0.063 Uiso 1 1 calc R . . C64 C 0.7873(2) -0.10402(11) 0.22629(19) 0.0585(7) Uani 1 1 d . . . H64 H 0.7715 -0.1391 0.2386 0.070 Uiso 1 1 calc R . . C65 C 0.7699(2) -0.06524(11) 0.28074(18) 0.0612(7) Uani 1 1 d . . . H65 H 0.7417 -0.0736 0.3307 0.073 Uiso 1 1 calc R . . C66 C 0.7931(2) -0.01432(10) 0.26305(14) 0.0462(6) Uani 1 1 d . . . H66 H 0.7812 0.0122 0.3010 0.055 Uiso 1 1 calc R . . P3 P 0.84672(4) 0.17713(2) 0.36441(3) 0.02527(11) Uani 1 1 d . . . C71 C 0.76289(15) 0.21276(8) 0.43126(11) 0.0272(4) Uani 1 1 d . . . C72 C 0.68125(16) 0.18574(9) 0.46540(13) 0.0355(5) Uani 1 1 d . . . H72 H 0.6696 0.1502 0.4524 0.043 Uiso 1 1 calc R . . C73 C 0.61730(17) 0.21022(10) 0.51788(14) 0.0429(6) Uani 1 1 d . . . H73 H 0.5623 0.1914 0.5410 0.051 Uiso 1 1 calc R . . C74 C 0.63308(18) 0.26196(10) 0.53693(14) 0.0433(6) Uani 1 1 d . . . H74 H 0.5892 0.2787 0.5732 0.052 Uiso 1 1 calc R . . C75 C 0.71270(18) 0.28935(9) 0.50314(13) 0.0405(5) Uani 1 1 d . . . H75 H 0.7231 0.3250 0.5158 0.049 Uiso 1 1 calc R . . C76 C 0.77784(16) 0.26483(8) 0.45057(12) 0.0326(5) Uani 1 1 d . . . H76 H 0.8329 0.2838 0.4278 0.039 Uiso 1 1 calc R . . C81 C 0.92768(15) 0.13749(7) 0.43514(12) 0.0272(4) Uani 1 1 d . . . C82 C 0.92563(16) 0.14251(9) 0.51783(12) 0.0351(5) Uani 1 1 d . . . H82 H 0.8847 0.1692 0.5400 0.042 Uiso 1 1 calc R . . C83 C 0.98314(18) 0.10861(10) 0.56846(14) 0.0426(6) Uani 1 1 d . . . H83 H 0.9805 0.1119 0.6251 0.051 Uiso 1 1 calc R . . C84 C 1.04384(18) 0.07035(9) 0.53684(15) 0.0449(6) Uani 1 1 d . . . H84 H 1.0833 0.0473 0.5715 0.054 Uiso 1 1 calc R . . C85 C 1.04736(18) 0.06551(9) 0.45492(15) 0.0447(6) Uani 1 1 d . . . H85 H 1.0901 0.0394 0.4332 0.054 Uiso 1 1 calc R . . C86 C 0.98923(17) 0.09838(9) 0.40409(13) 0.0371(5) Uani 1 1 d . . . H86 H 0.9912 0.0943 0.3476 0.045 Uiso 1 1 calc R . . C91 C 0.93572(15) 0.22624(8) 0.32717(12) 0.0277(4) Uani 1 1 d . . . C92 C 0.89916(17) 0.25594(9) 0.26156(13) 0.0378(5) Uani 1 1 d . . . H92 H 0.8294 0.2510 0.2389 0.045 Uiso 1 1 calc R . . C93 C 0.9642(2) 0.29285(9) 0.22894(15) 0.0476(6) Uani 1 1 d . . . H93 H 0.9385 0.3134 0.1846 0.057 Uiso 1 1 calc R . . C94 C 1.0657(2) 0.29964(10) 0.26086(15) 0.0513(6) Uani 1 1 d . . . H94 H 1.1103 0.3247 0.2383 0.062 Uiso 1 1 calc R . . C95 C 1.10287(18) 0.27017(10) 0.32544(15) 0.0482(6) Uani 1 1 d . . . H95 H 1.1731 0.2749 0.3472 0.058 Uiso 1 1 calc R . . C96 C 1.03823(16) 0.23356(9) 0.35898(13) 0.0360(5) Uani 1 1 d . . . H96 H 1.0642 0.2135 0.4037 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.02411(7) 0.02702(8) 0.02670(8) -0.00220(6) 0.00012(5) 0.00198(6) N1 0.0480(11) 0.0583(14) 0.0346(10) 0.0008(9) 0.0014(9) -0.0207(10) C1 0.0372(11) 0.0415(13) 0.0246(10) 0.0015(9) -0.0008(9) -0.0074(10) C10 0.0300(10) 0.0331(12) 0.0293(11) 0.0026(9) -0.0004(8) -0.0030(9) N2 0.0572(12) 0.0382(12) 0.0448(12) -0.0064(10) -0.0009(10) 0.0015(10) C2 0.0351(10) 0.0277(11) 0.0351(11) 0.0039(9) 0.0019(9) 0.0004(9) C20 0.0299(9) 0.0285(11) 0.0280(10) 0.0020(8) -0.0018(8) 0.0000(8) N3 0.0473(11) 0.0564(14) 0.0421(12) 0.0011(10) 0.0110(10) -0.0059(10) C3 0.0331(10) 0.0352(12) 0.0320(11) -0.0006(9) 0.0018(9) -0.0011(9) C30 0.0272(9) 0.0299(11) 0.0296(10) 0.0009(8) 0.0010(8) 0.0012(8) N4 0.0573(13) 0.0482(13) 0.0553(13) -0.0113(10) 0.0124(11) -0.0201(11) C4 0.0371(11) 0.0375(13) 0.0341(12) -0.0019(10) 0.0085(9) -0.0060(10) C40 0.0291(9) 0.0293(11) 0.0302(11) 0.0010(8) -0.0003(8) -0.0022(8) N5 0.0626(14) 0.0792(17) 0.0399(12) -0.0161(12) 0.0078(11) -0.0090(13) C5 0.0380(11) 0.0474(14) 0.0328(12) -0.0029(10) 0.0015(10) -0.0076(10) C50 0.0318(10) 0.0342(12) 0.0268(10) 0.0011(8) 0.0002(8) -0.0031(9) P1 0.0236(2) 0.0261(3) 0.0266(3) -0.0003(2) -0.0006(2) 0.00394(19) C11 0.0257(9) 0.0284(11) 0.0283(10) 0.0009(8) 0.0023(8) 0.0024(8) C12 0.0312(10) 0.0441(13) 0.0324(11) -0.0052(10) -0.0016(9) 0.0096(9) C13 0.0430(12) 0.0496(15) 0.0320(12) -0.0114(10) 0.0012(10) 0.0066(11) C14 0.0361(11) 0.0416(13) 0.0442(13) -0.0079(11) 0.0095(10) 0.0111(10) C15 0.0312(11) 0.0465(14) 0.0475(14) -0.0061(11) -0.0030(10) 0.0148(10) C16 0.0300(10) 0.0400(13) 0.0347(11) -0.0088(10) -0.0051(9) 0.0079(9) C21 0.0241(9) 0.0287(11) 0.0317(11) -0.0033(8) -0.0022(8) 0.0045(8) C22 0.0387(11) 0.0328(12) 0.0324(11) -0.0012(9) -0.0033(9) 0.0068(9) C23 0.0454(12) 0.0410(14) 0.0339(12) -0.0070(10) -0.0083(10) 0.0101(10) C24 0.0427(13) 0.0481(15) 0.0503(15) -0.0152(12) -0.0082(11) -0.0020(11) C25 0.0571(15) 0.0495(16) 0.0552(16) -0.0022(13) -0.0014(13) -0.0247(13) C26 0.0460(13) 0.0443(14) 0.0364(12) 0.0040(10) -0.0026(10) -0.0101(11) C31 0.0272(9) 0.0285(11) 0.0271(10) -0.0004(8) -0.0026(8) 0.0016(8) C32 0.0349(11) 0.0317(12) 0.0433(13) -0.0008(10) 0.0043(10) 0.0026(9) C33 0.0515(14) 0.0302(13) 0.0601(16) 0.0067(11) 0.0050(12) -0.0036(11) C34 0.0477(13) 0.0455(15) 0.0476(14) 0.0057(11) 0.0063(11) -0.0155(12) C35 0.0417(12) 0.0487(15) 0.0492(14) -0.0023(11) 0.0179(11) -0.0039(11) C36 0.0381(11) 0.0340(12) 0.0468(13) 0.0012(10) 0.0120(10) 0.0026(10) P2 0.0285(2) 0.0293(3) 0.0274(3) -0.0032(2) 0.0013(2) 0.0062(2) C41 0.0324(10) 0.0284(11) 0.0284(10) -0.0035(8) 0.0025(8) 0.0072(8) C42 0.0357(11) 0.0343(12) 0.0364(12) -0.0068(9) -0.0004(9) 0.0073(9) C43 0.0484(13) 0.0431(14) 0.0401(13) -0.0113(11) -0.0113(11) 0.0117(11) C44 0.0701(17) 0.0491(15) 0.0271(12) -0.0017(11) -0.0008(12) 0.0170(13) C45 0.0538(14) 0.0529(16) 0.0367(13) 0.0027(11) 0.0135(11) 0.0071(12) C46 0.0375(11) 0.0414(13) 0.0351(12) -0.0003(10) 0.0059(9) 0.0069(10) C51 0.0320(10) 0.0383(13) 0.0310(11) -0.0036(9) -0.0001(9) 0.0064(9) C52 0.0409(13) 0.0420(15) 0.088(2) -0.0121(14) -0.0168(14) 0.0111(11) C53 0.0409(15) 0.067(2) 0.137(3) -0.015(2) -0.0240(18) 0.0173(15) C54 0.0335(13) 0.080(2) 0.093(2) -0.0140(19) -0.0112(14) -0.0009(14) C55 0.0412(13) 0.0518(16) 0.0579(16) -0.0077(13) 0.0054(12) -0.0097(12) C56 0.0352(11) 0.0404(14) 0.0399(13) -0.0006(10) 0.0047(10) 0.0042(10) C61 0.0317(10) 0.0303(11) 0.0335(11) 0.0000(9) -0.0012(9) 0.0039(9) C62 0.0460(12) 0.0348(13) 0.0426(13) -0.0057(10) 0.0040(10) 0.0047(10) C63 0.0586(15) 0.0332(14) 0.0654(18) -0.0102(12) -0.0075(13) 0.0014(12) C64 0.0594(16) 0.0380(15) 0.077(2) 0.0150(14) -0.0057(15) -0.0059(13) C65 0.079(2) 0.0486(17) 0.0570(17) 0.0185(14) 0.0110(15) -0.0016(15) C66 0.0618(15) 0.0426(15) 0.0347(12) 0.0056(10) 0.0060(11) 0.0074(12) P3 0.0254(2) 0.0252(3) 0.0250(3) -0.0012(2) -0.0002(2) -0.0018(2) C71 0.0270(9) 0.0306(11) 0.0236(10) -0.0006(8) -0.0025(8) -0.0004(8) C72 0.0351(11) 0.0362(13) 0.0355(12) -0.0048(9) 0.0046(9) -0.0060(9) C73 0.0345(11) 0.0551(16) 0.0399(13) -0.0052(11) 0.0085(10) -0.0038(11) C74 0.0404(12) 0.0528(16) 0.0372(13) -0.0096(11) 0.0055(10) 0.0079(11) C75 0.0493(13) 0.0324(12) 0.0393(13) -0.0090(10) -0.0012(10) 0.0049(10) C76 0.0361(10) 0.0310(12) 0.0303(11) -0.0015(9) -0.0004(9) -0.0018(9) C81 0.0269(9) 0.0244(10) 0.0299(10) 0.0021(8) -0.0009(8) -0.0044(8) C82 0.0366(11) 0.0391(13) 0.0291(11) 0.0009(9) -0.0020(9) 0.0014(9) C83 0.0466(13) 0.0507(15) 0.0300(12) 0.0095(10) -0.0028(10) -0.0025(11) C84 0.0434(12) 0.0422(14) 0.0478(14) 0.0143(11) -0.0070(11) 0.0018(11) C85 0.0440(13) 0.0393(14) 0.0505(15) 0.0017(11) -0.0003(11) 0.0089(11) C86 0.0413(12) 0.0367(13) 0.0331(12) -0.0008(10) -0.0009(10) 0.0056(10) C91 0.0296(9) 0.0267(11) 0.0272(10) -0.0033(8) 0.0041(8) -0.0039(8) C92 0.0393(11) 0.0366(13) 0.0373(12) 0.0060(10) 0.0001(10) -0.0021(10) C93 0.0606(15) 0.0392(14) 0.0436(14) 0.0116(11) 0.0083(12) -0.0028(12) C94 0.0545(15) 0.0479(16) 0.0533(16) 0.0044(12) 0.0179(13) -0.0187(12) C95 0.0368(12) 0.0553(16) 0.0528(15) -0.0008(12) 0.0051(11) -0.0167(11) C96 0.0324(10) 0.0414(13) 0.0337(12) 0.0002(10) -0.0005(9) -0.0071(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.4721(19) . ? Ag1 P2 2.5115(5) . ? Ag1 P3 2.5181(5) . ? Ag1 P1 2.5228(5) . ? N1 C1 1.139(3) . ? C1 C10 1.424(3) . ? C10 C20 1.407(3) . ? C10 C50 1.408(3) . ? N2 C2 1.144(3) . ? C2 C20 1.425(3) . ? C20 C30 1.401(3) . ? N3 C3 1.142(3) . ? C3 C30 1.424(3) . ? C30 C40 1.406(3) . ? N4 C4 1.140(3) . ? C4 C40 1.424(3) . ? C40 C50 1.403(3) . ? N5 C5 1.141(3) . ? C5 C50 1.424(3) . ? P1 C21 1.824(2) . ? P1 C11 1.8265(19) . ? P1 C31 1.827(2) . ? C11 C12 1.383(3) . ? C11 C16 1.392(3) . ? C12 C13 1.388(3) . ? C12 H12 0.9500 . ? C13 C14 1.378(3) . ? C13 H13 0.9500 . ? C14 C15 1.375(3) . ? C14 H14 0.9500 . ? C15 C16 1.382(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C21 C26 1.382(3) . ? C21 C22 1.388(3) . ? C22 C23 1.388(3) . ? C22 H22 0.9500 . ? C23 C24 1.368(3) . ? C23 H23 0.9500 . ? C24 C25 1.380(4) . ? C24 H24 0.9500 . ? C25 C26 1.383(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C31 C32 1.384(3) . ? C31 C36 1.391(3) . ? C32 C33 1.387(3) . ? C32 H32 0.9500 . ? C33 C34 1.372(3) . ? C33 H33 0.9500 . ? C34 C35 1.376(3) . ? C34 H34 0.9500 . ? C35 C36 1.382(3) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? P2 C61 1.824(2) . ? P2 C51 1.828(2) . ? P2 C41 1.828(2) . ? C41 C42 1.393(3) . ? C41 C46 1.394(3) . ? C42 C43 1.384(3) . ? C42 H42 0.9500 . ? C43 C44 1.380(3) . ? C43 H43 0.9500 . ? C44 C45 1.374(3) . ? C44 H44 0.9500 . ? C45 C46 1.386(3) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C52 1.385(3) . ? C51 C56 1.391(3) . ? C52 C53 1.388(4) . ? C52 H52 0.9500 . ? C53 C54 1.376(4) . ? C53 H53 0.9500 . ? C54 C55 1.370(4) . ? C54 H54 0.9500 . ? C55 C56 1.384(3) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C66 1.384(3) . ? C61 C62 1.390(3) . ? C62 C63 1.380(3) . ? C62 H62 0.9500 . ? C63 C64 1.374(4) . ? C63 H63 0.9500 . ? C64 C65 1.376(4) . ? C64 H64 0.9500 . ? C65 C66 1.379(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? P3 C81 1.828(2) . ? P3 C91 1.8284(19) . ? P3 C71 1.832(2) . ? C71 C76 1.389(3) . ? C71 C72 1.397(3) . ? C72 C73 1.381(3) . ? C72 H72 0.9500 . ? C73 C74 1.381(3) . ? C73 H73 0.9500 . ? C74 C75 1.380(3) . ? C74 H74 0.9500 . ? C75 C76 1.392(3) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C82 1.386(3) . ? C81 C86 1.393(3) . ? C82 C83 1.390(3) . ? C82 H82 0.9500 . ? C83 C84 1.375(3) . ? C83 H83 0.9500 . ? C84 C85 1.375(3) . ? C84 H84 0.9500 . ? C85 C86 1.380(3) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C91 C96 1.388(3) . ? C91 C92 1.391(3) . ? C92 C93 1.391(3) . ? C92 H92 0.9500 . ? C93 C94 1.375(3) . ? C93 H93 0.9500 . ? C94 C95 1.377(3) . ? C94 H94 0.9500 . ? C95 C96 1.389(3) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 P2 113.03(5) . . ? N1 Ag1 P3 96.11(5) . . ? P2 Ag1 P3 118.368(17) . . ? N1 Ag1 P1 92.07(5) . . ? P2 Ag1 P1 113.019(17) . . ? P3 Ag1 P1 119.021(18) . . ? C1 N1 Ag1 167.47(19) . . ? N1 C1 C10 176.1(2) . . ? C20 C10 C50 108.19(17) . . ? C20 C10 C1 127.85(19) . . ? C50 C10 C1 123.96(18) . . ? N2 C2 C20 178.8(2) . . ? C30 C20 C10 107.67(17) . . ? C30 C20 C2 125.61(18) . . ? C10 C20 C2 126.68(18) . . ? N3 C3 C30 178.9(3) . . ? C20 C30 C40 108.34(17) . . ? C20 C30 C3 125.86(19) . . ? C40 C30 C3 125.68(19) . . ? N4 C4 C40 178.5(2) . . ? C50 C40 C30 107.97(18) . . ? C50 C40 C4 125.13(19) . . ? C30 C40 C4 126.89(18) . . ? N5 C5 C50 179.0(3) . . ? C40 C50 C10 107.83(17) . . ? C40 C50 C5 127.0(2) . . ? C10 C50 C5 125.18(19) . . ? C21 P1 C11 102.94(9) . . ? C21 P1 C31 104.18(9) . . ? C11 P1 C31 103.56(9) . . ? C21 P1 Ag1 115.63(7) . . ? C11 P1 Ag1 117.12(6) . . ? C31 P1 Ag1 111.87(6) . . ? C12 C11 C16 119.06(18) . . ? C12 C11 P1 118.46(14) . . ? C16 C11 P1 122.41(15) . . ? C11 C12 C13 120.49(19) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 120.0(2) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 119.8(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.6(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C15 C16 C11 120.0(2) . . ? C15 C16 H16 120.0 . . ? C11 C16 H16 120.0 . . ? C26 C21 C22 118.60(19) . . ? C26 C21 P1 118.11(16) . . ? C22 C21 P1 123.29(16) . . ? C23 C22 C21 120.6(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C22 120.1(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 119.9(2) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.2(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C21 C26 C25 120.6(2) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C32 C31 C36 118.39(19) . . ? C32 C31 P1 124.18(15) . . ? C36 C31 P1 117.39(16) . . ? C31 C32 C33 120.5(2) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C34 C33 C32 120.3(2) . . ? C34 C33 H33 119.9 . . ? C32 C33 H33 119.9 . . ? C33 C34 C35 120.0(2) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 C36 119.8(2) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 120.9(2) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C61 P2 C51 106.39(10) . . ? C61 P2 C41 102.71(9) . . ? C51 P2 C41 103.17(9) . . ? C61 P2 Ag1 116.81(7) . . ? C51 P2 Ag1 111.87(7) . . ? C41 P2 Ag1 114.54(6) . . ? C42 C41 C46 118.69(19) . . ? C42 C41 P2 117.48(15) . . ? C46 C41 P2 123.65(16) . . ? C43 C42 C41 120.7(2) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 119.8(2) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 120.3(2) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.3(2) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 120.3(2) . . ? C45 C46 H46 119.9 . . ? C41 C46 H46 119.9 . . ? C52 C51 C56 118.7(2) . . ? C52 C51 P2 123.62(18) . . ? C56 C51 P2 117.69(16) . . ? C51 C52 C53 120.0(3) . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 120.6(3) . . ? C54 C53 H53 119.7 . . ? C52 C53 H53 119.7 . . ? C55 C54 C53 120.1(2) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 119.8(2) . . ? C54 C55 H55 120.1 . . ? C56 C55 H55 120.1 . . ? C55 C56 C51 120.9(2) . . ? C55 C56 H56 119.5 . . ? C51 C56 H56 119.5 . . ? C66 C61 C62 119.0(2) . . ? C66 C61 P2 118.04(17) . . ? C62 C61 P2 122.97(17) . . ? C63 C62 C61 120.0(2) . . ? C63 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C64 C63 C62 120.6(2) . . ? C64 C63 H63 119.7 . . ? C62 C63 H63 119.7 . . ? C63 C64 C65 119.6(3) . . ? C63 C64 H64 120.2 . . ? C65 C64 H64 120.2 . . ? C64 C65 C66 120.2(3) . . ? C64 C65 H65 119.9 . . ? C66 C65 H65 119.9 . . ? C65 C66 C61 120.5(2) . . ? C65 C66 H66 119.8 . . ? C61 C66 H66 119.8 . . ? C81 P3 C91 105.70(9) . . ? C81 P3 C71 102.22(9) . . ? C91 P3 C71 104.66(9) . . ? C81 P3 Ag1 117.71(7) . . ? C91 P3 Ag1 108.02(6) . . ? C71 P3 Ag1 117.27(6) . . ? C76 C71 C72 118.71(18) . . ? C76 C71 P3 123.23(15) . . ? C72 C71 P3 118.04(15) . . ? C73 C72 C71 120.6(2) . . ? C73 C72 H72 119.7 . . ? C71 C72 H72 119.7 . . ? C72 C73 C74 120.2(2) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C75 C74 C73 119.9(2) . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.1(2) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C71 C76 C75 120.4(2) . . ? C71 C76 H76 119.8 . . ? C75 C76 H76 119.8 . . ? C82 C81 C86 118.79(19) . . ? C82 C81 P3 123.08(16) . . ? C86 C81 P3 118.02(15) . . ? C81 C82 C83 120.3(2) . . ? C81 C82 H82 119.9 . . ? C83 C82 H82 119.9 . . ? C84 C83 C82 120.2(2) . . ? C84 C83 H83 119.9 . . ? C82 C83 H83 119.9 . . ? C85 C84 C83 119.9(2) . . ? C85 C84 H84 120.1 . . ? C83 C84 H84 120.1 . . ? C84 C85 C86 120.4(2) . . ? C84 C85 H85 119.8 . . ? C86 C85 H85 119.8 . . ? C85 C86 C81 120.4(2) . . ? C85 C86 H86 119.8 . . ? C81 C86 H86 119.8 . . ? C96 C91 C92 119.10(19) . . ? C96 C91 P3 123.23(16) . . ? C92 C91 P3 117.61(15) . . ? C91 C92 C93 120.3(2) . . ? C91 C92 H92 119.8 . . ? C93 C92 H92 119.8 . . ? C94 C93 C92 120.0(2) . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.1(2) . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C94 C95 C96 120.4(2) . . ? C94 C95 H95 119.8 . . ? C96 C95 H95 119.8 . . ? C91 C96 C95 120.1(2) . . ? C91 C96 H96 120.0 . . ? C95 C96 H96 120.0 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.378 _refine_diff_density_min -0.699 _refine_diff_density_rms 0.069 # Attachment '- Compound5.cif' data_dw1175 _database_code_depnum_ccdc_archive 'CCDC 866132' #TrackingRef '- Compound5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H60 Ag2 N10 P4, C H Cl3' _chemical_formula_sum 'C93 H61 Ag2 Cl3 N10 P4' _chemical_formula_weight 1764.49 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' 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 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 10.9813(1) _cell_length_b 12.7250(2) _cell_length_c 16.8652(3) _cell_angle_alpha 97.866(1) _cell_angle_beta 100.456(1) _cell_angle_gamma 112.374(1) _cell_volume 2087.41(5) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23903 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 33.14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 894 _exptl_absorpt_coefficient_mu 0.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.857 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; The chloroform solvate molecule is disordered about an inversion centre: for the rerfinement, a common isotropic displacement parameter plus bond length constraints were applied to the C and Cl atoms of this group (JED). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 39087 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.56 _diffrn_reflns_theta_max 33.19 _reflns_number_total 15808 _reflns_number_gt 10572 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+0.3282P] 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 15808 _refine_ls_number_parameters 501 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0939 _refine_ls_R_factor_gt 0.0541 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1299 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Ag1 Ag 0.097680(19) 0.117596(16) 0.219703(12) 0.02699(6) Uani 1 1 d . . . P1 P -0.11316(7) -0.02516(6) 0.24138(4) 0.02711(14) Uani 1 1 d . . . P2 P 0.28842(6) 0.27579(5) 0.32121(4) 0.02370(13) Uani 1 1 d . . . N1 N 0.0097(3) 0.1965(2) 0.11572(16) 0.0431(6) Uani 1 1 d . . . N2 N -0.1628(3) 0.0100(2) -0.13748(18) 0.0429(6) Uani 1 1 d . . . N3 N -0.3091(3) 0.2259(3) -0.28164(18) 0.0565(8) Uani 1 1 d . . . N4 N -0.2610(3) 0.5353(3) -0.1097(2) 0.0529(7) Uani 1 1 d . . . N5 N -0.0751(3) 0.5182(3) 0.14799(18) 0.0498(7) Uani 1 1 d . . . C11 C -0.1080(3) 0.2684(2) 0.00398(16) 0.0282(5) Uani 1 1 d . . . C12 C -0.1574(3) 0.2093(2) -0.07987(16) 0.0285(5) Uani 1 1 d . . . C13 C -0.2114(3) 0.2744(2) -0.12368(17) 0.0303(5) Uani 1 1 d . . . C14 C -0.1972(3) 0.3728(2) -0.06724(18) 0.0305(5) Uani 1 1 d . . . C15 C -0.1326(3) 0.3697(2) 0.01184(17) 0.0296(5) Uani 1 1 d . . . C21 C -0.0427(3) 0.2308(2) 0.06772(18) 0.0328(6) Uani 1 1 d . . . C22 C -0.1590(3) 0.0997(2) -0.11202(17) 0.0321(5) Uani 1 1 d . . . C23 C -0.2668(3) 0.2466(3) -0.21131(19) 0.0369(6) Uani 1 1 d . . . C24 C -0.2329(3) 0.4638(3) -0.0895(2) 0.0368(6) Uani 1 1 d . . . C25 C -0.1009(3) 0.4522(2) 0.08726(19) 0.0345(6) Uani 1 1 d . . . C31 C -0.2243(3) -0.1405(2) 0.15122(19) 0.0334(6) Uani 1 1 d . . . C32 C -0.3229(3) -0.2451(3) 0.1572(2) 0.0443(7) Uani 1 1 d . . . H32 H -0.3357 -0.2574 0.2100 0.053 Uiso 1 1 calc R . . C33 C -0.4028(4) -0.3315(3) 0.0867(3) 0.0561(10) Uani 1 1 d . . . H33 H -0.4715 -0.4018 0.0913 0.067 Uiso 1 1 calc R . . C34 C -0.3835(4) -0.3163(3) 0.0105(3) 0.0637(11) Uani 1 1 d . . . H34 H -0.4377 -0.3765 -0.0374 0.076 Uiso 1 1 calc R . . C35 C -0.2852(4) -0.2133(4) 0.0030(2) 0.0621(11) Uani 1 1 d . . . H35 H -0.2729 -0.2024 -0.0501 0.075 Uiso 1 1 calc R . . C36 C -0.2045(3) -0.1260(3) 0.0731(2) 0.0431(7) Uani 1 1 d . . . H36 H -0.1357 -0.0561 0.0680 0.052 Uiso 1 1 calc R . . C41 C -0.0820(3) -0.1045(2) 0.31937(18) 0.0300(5) Uani 1 1 d . . . C42 C -0.1192(3) -0.0965(2) 0.39379(18) 0.0347(6) Uani 1 1 d . . . H42 H -0.1708 -0.0531 0.4040 0.042 Uiso 1 1 calc R . . C43 C -0.0816(3) -0.1513(3) 0.4532(2) 0.0412(7) Uani 1 1 d . . . H43 H -0.1076 -0.1453 0.5038 0.049 Uiso 1 1 calc R . . C44 C -0.0061(3) -0.2148(3) 0.4390(2) 0.0426(7) Uani 1 1 d . . . H44 H 0.0199 -0.2522 0.4798 0.051 Uiso 1 1 calc R . . C45 C 0.0310(4) -0.2233(3) 0.3655(2) 0.0477(8) Uani 1 1 d . . . H45 H 0.0830 -0.2664 0.3557 0.057 Uiso 1 1 calc R . . C46 C -0.0067(3) -0.1696(3) 0.3062(2) 0.0403(7) Uani 1 1 d . . . H46 H 0.0189 -0.1767 0.2556 0.048 Uiso 1 1 calc R . . C51 C -0.2141(3) 0.0462(2) 0.27939(18) 0.0318(5) Uani 1 1 d . . . C52 C -0.1485(3) 0.1649(3) 0.3129(2) 0.0453(8) Uani 1 1 d . . . H52 H -0.0553 0.2056 0.3141 0.054 Uiso 1 1 calc R . . C53 C -0.2176(4) 0.2254(3) 0.3450(3) 0.0601(10) Uani 1 1 d . . . H53 H -0.1721 0.3073 0.3667 0.072 Uiso 1 1 calc R . . C54 C -0.3516(4) 0.1668(3) 0.3453(2) 0.0510(8) Uani 1 1 d . . . H54 H -0.3978 0.2075 0.3691 0.061 Uiso 1 1 calc R . . C55 C -0.4190(4) 0.0483(3) 0.3109(3) 0.0515(9) Uani 1 1 d . . . H55 H -0.5123 0.0080 0.3096 0.062 Uiso 1 1 calc R . . C56 C -0.3503(3) -0.0124(3) 0.2778(2) 0.0436(7) Uani 1 1 d . . . H56 H -0.3969 -0.0938 0.2542 0.052 Uiso 1 1 calc R . . C61 C 0.4395(3) 0.3693(2) 0.29307(16) 0.0285(5) Uani 1 1 d . . . C62 C 0.4885(3) 0.3195(3) 0.2353(2) 0.0420(7) Uani 1 1 d . . . H62 H 0.4399 0.2392 0.2088 0.050 Uiso 1 1 calc R . . C63 C 0.6068(4) 0.3853(3) 0.2156(3) 0.0563(10) Uani 1 1 d . . . H63 H 0.6400 0.3498 0.1765 0.068 Uiso 1 1 calc R . . C64 C 0.6770(4) 0.5024(3) 0.2527(3) 0.0560(9) Uani 1 1 d . . . H64 H 0.7583 0.5473 0.2388 0.067 Uiso 1 1 calc R . . C65 C 0.6300(3) 0.5551(3) 0.3102(2) 0.0478(8) Uani 1 1 d . . . H65 H 0.6789 0.6356 0.3360 0.057 Uiso 1 1 calc R . . C66 C 0.5101(3) 0.4882(3) 0.3295(2) 0.0396(7) Uani 1 1 d . . . H66 H 0.4760 0.5240 0.3679 0.048 Uiso 1 1 calc R . . C71 C 0.3586(3) 0.2244(2) 0.40637(15) 0.0249(5) Uani 1 1 d . . . C72 C 0.4708(3) 0.2981(2) 0.47097(17) 0.0314(5) Uani 1 1 d . . . H72 H 0.5132 0.3789 0.4719 0.038 Uiso 1 1 calc R . . C73 C 0.5211(3) 0.2545(3) 0.53400(18) 0.0367(6) Uani 1 1 d . . . H73 H 0.5967 0.3057 0.5783 0.044 Uiso 1 1 calc R . . C74 C 0.4610(3) 0.1362(3) 0.53237(19) 0.0402(7) Uani 1 1 d . . . H74 H 0.4961 0.1063 0.5753 0.048 Uiso 1 1 calc R . . C75 C 0.3506(3) 0.0621(3) 0.4684(2) 0.0412(7) Uani 1 1 d . . . H75 H 0.3095 -0.0188 0.4674 0.049 Uiso 1 1 calc R . . C76 C 0.2990(3) 0.1053(2) 0.40543(18) 0.0319(5) Uani 1 1 d . . . H76 H 0.2228 0.0538 0.3615 0.038 Uiso 1 1 calc R . . C81 C 0.2274(3) 0.3779(2) 0.36751(16) 0.0260(5) Uani 1 1 d . . . C82 C 0.1665(3) 0.4287(2) 0.31385(19) 0.0365(6) Uani 1 1 d . . . H82 H 0.1634 0.4125 0.2566 0.044 Uiso 1 1 calc R . . C83 C 0.1111(3) 0.5018(3) 0.3430(2) 0.0413(7) Uani 1 1 d . . . H83 H 0.0689 0.5351 0.3059 0.050 Uiso 1 1 calc R . . C84 C 0.1169(3) 0.5271(3) 0.4270(2) 0.0412(7) Uani 1 1 d . . . H84 H 0.0798 0.5786 0.4472 0.049 Uiso 1 1 calc R . . C85 C 0.1761(3) 0.4779(3) 0.48063(19) 0.0375(6) Uani 1 1 d . . . H85 H 0.1793 0.4949 0.5378 0.045 Uiso 1 1 calc R . . C86 C 0.2315(3) 0.4028(2) 0.45140(17) 0.0300(5) Uani 1 1 d . . . H86 H 0.2722 0.3688 0.4887 0.036 Uiso 1 1 calc R . . C01 C -0.4394(14) -0.0020(11) 0.0052(8) 0.1406(8) Uiso 0.50 1 d PD A -1 H01 H -0.3520 -0.0089 0.0039 0.169 Uiso 0.50 1 calc PR A -1 Cl1 Cl -0.5075(5) 0.0058(4) -0.0899(3) 0.1406(8) Uiso 0.50 1 d PD A -1 Cl2 Cl -0.5392(5) -0.1212(4) 0.0362(3) 0.1406(8) Uiso 0.50 1 d PD A -1 Cl3 Cl -0.3993(5) 0.1236(4) 0.0841(3) 0.1406(8) Uiso 0.50 1 d PD A -1 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 Ag1 0.02867(10) 0.02380(9) 0.02460(10) 0.00395(7) 0.00456(7) 0.00830(7) P1 0.0264(3) 0.0233(3) 0.0302(3) 0.0064(3) 0.0080(3) 0.0084(2) P2 0.0256(3) 0.0217(3) 0.0218(3) 0.0041(2) 0.0044(2) 0.0088(2) N1 0.0498(15) 0.0384(13) 0.0368(14) 0.0141(12) 0.0033(12) 0.0155(12) N2 0.0490(15) 0.0380(13) 0.0427(15) 0.0028(12) 0.0122(12) 0.0211(12) N3 0.0553(18) 0.066(2) 0.0337(16) 0.0077(14) -0.0057(13) 0.0182(16) N4 0.0584(18) 0.0475(16) 0.067(2) 0.0245(15) 0.0161(16) 0.0336(15) N5 0.0547(17) 0.0511(16) 0.0427(16) 0.0018(13) 0.0207(14) 0.0202(14) C11 0.0318(13) 0.0276(12) 0.0241(12) 0.0061(10) 0.0059(10) 0.0118(10) C12 0.0332(13) 0.0259(12) 0.0258(13) 0.0044(10) 0.0063(10) 0.0127(10) C13 0.0282(12) 0.0296(12) 0.0300(13) 0.0081(11) 0.0043(10) 0.0098(10) C14 0.0267(12) 0.0310(13) 0.0344(14) 0.0088(11) 0.0074(11) 0.0122(10) C15 0.0333(13) 0.0255(11) 0.0286(13) 0.0050(10) 0.0090(11) 0.0105(10) C21 0.0382(14) 0.0294(13) 0.0295(14) 0.0071(11) 0.0075(11) 0.0132(11) C22 0.0326(13) 0.0350(14) 0.0290(14) 0.0056(11) 0.0070(11) 0.0154(11) C23 0.0338(14) 0.0372(15) 0.0346(16) 0.0094(13) 0.0018(12) 0.0121(12) C24 0.0334(14) 0.0367(14) 0.0422(17) 0.0126(13) 0.0100(12) 0.0153(12) C25 0.0365(14) 0.0345(14) 0.0341(15) 0.0086(12) 0.0129(12) 0.0146(12) C31 0.0307(13) 0.0266(12) 0.0355(15) 0.0014(11) 0.0063(11) 0.0070(10) C32 0.0407(16) 0.0318(14) 0.051(2) 0.0073(14) 0.0116(15) 0.0058(13) C33 0.0425(18) 0.0311(16) 0.072(3) -0.0037(17) 0.0063(18) 0.0003(14) C34 0.056(2) 0.051(2) 0.058(3) -0.0133(19) 0.0029(19) 0.0087(18) C35 0.055(2) 0.063(2) 0.039(2) -0.0110(18) 0.0047(17) 0.0042(19) C36 0.0395(16) 0.0431(17) 0.0360(17) 0.0047(14) 0.0080(13) 0.0083(13) C41 0.0294(12) 0.0247(11) 0.0359(15) 0.0104(11) 0.0110(11) 0.0090(10) C42 0.0402(15) 0.0317(13) 0.0363(15) 0.0105(12) 0.0123(12) 0.0172(12) C43 0.0529(18) 0.0355(15) 0.0370(16) 0.0117(13) 0.0149(14) 0.0176(14) C44 0.0505(18) 0.0343(15) 0.0489(19) 0.0212(14) 0.0144(15) 0.0191(14) C45 0.060(2) 0.0408(16) 0.061(2) 0.0246(16) 0.0264(18) 0.0316(16) C46 0.0526(18) 0.0357(14) 0.0493(18) 0.0197(14) 0.0271(15) 0.0262(14) C51 0.0340(13) 0.0308(13) 0.0349(15) 0.0113(11) 0.0095(11) 0.0165(11) C52 0.0354(15) 0.0409(16) 0.059(2) 0.0010(15) 0.0131(15) 0.0186(13) C53 0.055(2) 0.0475(19) 0.078(3) -0.0045(19) 0.017(2) 0.0272(18) C54 0.051(2) 0.067(2) 0.055(2) 0.0176(18) 0.0202(17) 0.0410(18) C55 0.0419(17) 0.061(2) 0.072(3) 0.032(2) 0.0302(18) 0.0307(17) C56 0.0360(15) 0.0388(15) 0.065(2) 0.0214(16) 0.0192(15) 0.0188(13) C61 0.0296(12) 0.0307(12) 0.0262(13) 0.0111(11) 0.0075(10) 0.0118(10) C62 0.0446(17) 0.0421(16) 0.0450(18) 0.0131(14) 0.0210(14) 0.0186(14) C63 0.052(2) 0.064(2) 0.065(2) 0.022(2) 0.0372(19) 0.0254(18) C64 0.0427(18) 0.063(2) 0.065(2) 0.031(2) 0.0264(18) 0.0147(17) C65 0.0459(18) 0.0394(16) 0.0442(19) 0.0151(15) 0.0102(15) 0.0017(14) C66 0.0441(16) 0.0326(14) 0.0357(16) 0.0092(12) 0.0151(13) 0.0064(12) C71 0.0288(12) 0.0269(11) 0.0229(12) 0.0057(10) 0.0069(10) 0.0153(10) C72 0.0320(13) 0.0293(12) 0.0286(13) 0.0031(11) 0.0027(11) 0.0117(11) C73 0.0359(14) 0.0421(15) 0.0276(14) 0.0018(12) -0.0023(11) 0.0183(13) C74 0.0444(16) 0.0482(17) 0.0337(16) 0.0174(14) 0.0043(13) 0.0251(14) C75 0.0433(16) 0.0344(14) 0.0485(19) 0.0181(14) 0.0103(14) 0.0165(13) C76 0.0302(13) 0.0281(12) 0.0344(14) 0.0079(11) 0.0031(11) 0.0111(11) C81 0.0275(12) 0.0212(10) 0.0275(13) 0.0046(10) 0.0056(10) 0.0093(9) C82 0.0459(16) 0.0298(13) 0.0349(15) 0.0073(12) 0.0067(13) 0.0185(12) C83 0.0501(18) 0.0336(14) 0.0446(18) 0.0090(13) 0.0070(14) 0.0244(14) C84 0.0430(16) 0.0327(14) 0.056(2) 0.0104(14) 0.0190(15) 0.0210(13) C85 0.0455(16) 0.0364(14) 0.0347(15) 0.0063(12) 0.0170(13) 0.0187(13) C86 0.0324(13) 0.0304(12) 0.0320(14) 0.0107(11) 0.0126(11) 0.0149(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.371(3) . ? Ag1 N2 2.387(2) 2 ? Ag1 P2 2.4322(7) . ? Ag1 P1 2.4661(7) . ? P1 C31 1.819(3) . ? P1 C51 1.825(3) . ? P1 C41 1.825(3) . ? P2 C81 1.823(2) . ? P2 C71 1.823(3) . ? P2 C61 1.825(3) . ? N1 C21 1.138(4) . ? N2 C22 1.146(4) . ? N2 Ag1 2.387(2) 2 ? N3 C23 1.146(4) . ? N4 C24 1.140(4) . ? N5 C25 1.146(4) . ? C11 C12 1.407(4) . ? C11 C15 1.408(4) . ? C11 C21 1.422(4) . ? C12 C13 1.403(4) . ? C12 C22 1.417(4) . ? C13 C14 1.403(4) . ? C13 C23 1.430(4) . ? C14 C15 1.405(4) . ? C14 C24 1.431(4) . ? C15 C25 1.427(4) . ? C31 C32 1.391(4) . ? C31 C36 1.399(4) . ? C32 C33 1.386(5) . ? C32 H32 0.9500 . ? C33 C34 1.367(6) . ? C33 H33 0.9500 . ? C34 C35 1.384(5) . ? C34 H34 0.9500 . ? C35 C36 1.389(5) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C42 1.392(4) . ? C41 C46 1.398(4) . ? C42 C43 1.386(4) . ? C42 H42 0.9500 . ? C43 C44 1.389(4) . ? C43 H43 0.9500 . ? C44 C45 1.377(5) . ? C44 H44 0.9500 . ? C45 C46 1.374(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C52 1.381(4) . ? C51 C56 1.388(4) . ? C52 C53 1.394(4) . ? C52 H52 0.9500 . ? C53 C54 1.375(5) . ? C53 H53 0.9500 . ? C54 C55 1.383(5) . ? C54 H54 0.9500 . ? C55 C56 1.399(4) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C62 1.387(4) . ? C61 C66 1.395(4) . ? C62 C63 1.380(4) . ? C62 H62 0.9500 . ? C63 C64 1.379(6) . ? C63 H63 0.9500 . ? C64 C65 1.387(5) . ? C64 H64 0.9500 . ? C65 C66 1.394(4) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C72 1.392(4) . ? C71 C76 1.400(3) . ? C72 C73 1.387(4) . ? C72 H72 0.9500 . ? C73 C74 1.389(4) . ? C73 H73 0.9500 . ? C74 C75 1.379(5) . ? C74 H74 0.9500 . ? C75 C76 1.389(4) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C86 1.395(4) . ? C81 C82 1.397(4) . ? C82 C83 1.376(4) . ? C82 H82 0.9500 . ? C83 C84 1.393(5) . ? C83 H83 0.9500 . ? C84 C85 1.373(4) . ? C84 H84 0.9500 . ? C85 C86 1.396(4) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C01 Cl1 1.676(13) . ? C01 Cl2 1.713(13) . ? C01 Cl3 1.785(13) . ? C01 H01 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ag1 N2 99.91(10) . 2 ? N1 Ag1 P2 108.70(7) . . ? N2 Ag1 P2 113.66(7) 2 . ? N1 Ag1 P1 101.56(7) . . ? N2 Ag1 P1 100.22(7) 2 . ? P2 Ag1 P1 128.73(2) . . ? C31 P1 C51 107.53(13) . . ? C31 P1 C41 103.47(13) . . ? C51 P1 C41 104.78(12) . . ? C31 P1 Ag1 115.56(9) . . ? C51 P1 Ag1 111.39(9) . . ? C41 P1 Ag1 113.25(9) . . ? C81 P2 C71 105.95(11) . . ? C81 P2 C61 103.70(12) . . ? C71 P2 C61 103.20(12) . . ? C81 P2 Ag1 108.65(9) . . ? C71 P2 Ag1 112.00(8) . . ? C61 P2 Ag1 122.04(9) . . ? C21 N1 Ag1 174.2(3) . . ? C22 N2 Ag1 153.0(2) . 2 ? C12 C11 C15 108.1(2) . . ? C12 C11 C21 124.6(2) . . ? C15 C11 C21 127.3(2) . . ? C13 C12 C11 107.8(2) . . ? C13 C12 C22 126.9(3) . . ? C11 C12 C22 125.2(2) . . ? C14 C13 C12 108.3(2) . . ? C14 C13 C23 126.3(3) . . ? C12 C13 C23 125.4(3) . . ? C13 C14 C15 108.1(2) . . ? C13 C14 C24 124.6(3) . . ? C15 C14 C24 127.1(3) . . ? C14 C15 C11 107.8(2) . . ? C14 C15 C25 126.4(2) . . ? C11 C15 C25 125.8(3) . . ? N1 C21 C11 176.5(3) . . ? N2 C22 C12 178.5(3) . . ? N3 C23 C13 178.8(4) . . ? N4 C24 C14 177.8(4) . . ? N5 C25 C15 179.7(4) . . ? C32 C31 C36 118.7(3) . . ? C32 C31 P1 122.7(2) . . ? C36 C31 P1 118.6(2) . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.5(3) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 120.1(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.3(3) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C42 C41 C46 118.3(3) . . ? C42 C41 P1 123.8(2) . . ? C46 C41 P1 117.8(2) . . ? C43 C42 C41 120.5(3) . . ? C43 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C42 C43 C44 120.2(3) . . ? C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C45 C44 C43 119.6(3) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C46 C45 C44 120.4(3) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C41 121.1(3) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? C52 C51 C56 119.2(3) . . ? C52 C51 P1 117.1(2) . . ? C56 C51 P1 123.6(2) . . ? C51 C52 C53 120.7(3) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C54 C53 C52 120.1(3) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 119.7(3) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C54 C55 C56 120.2(3) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 120.0(3) . . ? C51 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C62 C61 C66 118.7(3) . . ? C62 C61 P2 118.7(2) . . ? C66 C61 P2 122.5(2) . . ? C63 C62 C61 120.8(3) . . ? C63 C62 H62 119.6 . . ? C61 C62 H62 119.6 . . ? C64 C63 C62 120.1(3) . . ? C64 C63 H63 120.0 . . ? C62 C63 H63 120.0 . . ? C63 C64 C65 120.5(3) . . ? C63 C64 H64 119.7 . . ? C65 C64 H64 119.7 . . ? C64 C65 C66 119.1(3) . . ? C64 C65 H65 120.5 . . ? C66 C65 H65 120.5 . . ? C65 C66 C61 120.7(3) . . ? C65 C66 H66 119.6 . . ? C61 C66 H66 119.6 . . ? C72 C71 C76 118.8(2) . . ? C72 C71 P2 122.74(19) . . ? C76 C71 P2 118.4(2) . . ? C73 C72 C71 120.5(3) . . ? C73 C72 H72 119.7 . . ? C71 C72 H72 119.7 . . ? C72 C73 C74 120.1(3) . . ? C72 C73 H73 120.0 . . ? C74 C73 H73 120.0 . . ? C75 C74 C73 119.9(3) . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 120.3(3) . . ? C74 C75 H75 119.9 . . ? C76 C75 H75 119.9 . . ? C75 C76 C71 120.3(3) . . ? C75 C76 H76 119.8 . . ? C71 C76 H76 119.8 . . ? C86 C81 C82 118.9(2) . . ? C86 C81 P2 124.1(2) . . ? C82 C81 P2 116.9(2) . . ? C83 C82 C81 120.7(3) . . ? C83 C82 H82 119.7 . . ? C81 C82 H82 119.7 . . ? C82 C83 C84 120.0(3) . . ? C82 C83 H83 120.0 . . ? C84 C83 H83 120.0 . . ? C85 C84 C83 120.1(3) . . ? C85 C84 H84 119.9 . . ? C83 C84 H84 119.9 . . ? C84 C85 C86 120.2(3) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C81 C86 C85 120.1(3) . . ? C81 C86 H86 120.0 . . ? C85 C86 H86 120.0 . . ? Cl1 C01 Cl2 113.5(8) . . ? Cl1 C01 Cl3 114.2(8) . . ? Cl2 C01 Cl3 107.3(7) . . ? Cl1 C01 H01 107.1 . . ? Cl2 C01 H01 107.1 . . ? Cl3 C01 H01 107.1 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 33.19 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.739 _refine_diff_density_min -1.133 _refine_diff_density_rms 0.103 # Attachment '- Compound6(check).cif' data_dw1171 _database_code_depnum_ccdc_archive 'CCDC 866133' #TrackingRef '- Compound6(check).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100.50 H78 Cu2 N10 P6' _chemical_formula_weight 1738.63 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.7176(2) _cell_length_b 14.3620(2) _cell_length_c 15.2562(2) _cell_angle_alpha 114.1120(10) _cell_angle_beta 101.5560(10) _cell_angle_gamma 106.3640(10) _cell_volume 2276.61(6) _cell_formula_units_Z 1 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 15509 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 30.03 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 899 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.894 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 30211 _diffrn_reflns_av_R_equivalents 0.0387 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 30.04 _reflns_number_total 13093 _reflns_number_gt 8561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Low rsidual electron density was interpreted 1/4 n-pentane solvate in the asymmetric unit. Restraints were applied to the parameters of the solvate. ; _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^)+(0.0841P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13093 _refine_ls_number_parameters 539 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1441 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.002 _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 Cu1 Cu 0.96265(2) 0.24779(2) 0.296461(19) 0.02960(9) Uani 1 1 d . . . N1 N 0.94632(17) 0.34102(15) 0.23144(14) 0.0360(4) Uani 1 1 d . . . N2 N 0.5903(2) 0.2525(2) 0.0704(2) 0.0606(6) Uani 1 1 d . . . N3 N 0.5723(2) 0.46112(19) -0.0786(2) 0.0570(6) Uani 1 1 d . . . N4 N 0.9387(2) 0.7097(2) 0.0266(2) 0.0621(7) Uani 1 1 d . . . N5 N 1.1767(2) 0.6219(2) 0.2056(2) 0.0621(6) Uani 1 1 d . . . C1 C 0.8824(2) 0.43320(18) 0.13085(17) 0.0355(5) Uani 1 1 d . . . C01 C 0.9209(2) 0.38249(18) 0.18587(17) 0.0349(5) Uani 1 1 d . . . C02 C 0.6658(2) 0.3181(2) 0.07067(19) 0.0422(5) Uani 1 1 d . . . C2 C 0.7636(2) 0.40330(18) 0.07687(17) 0.0356(5) Uani 1 1 d . . . C03 C 0.6569(2) 0.4673(2) -0.0273(2) 0.0432(6) Uani 1 1 d . . . C3 C 0.7601(2) 0.47355(19) 0.03499(18) 0.0366(5) Uani 1 1 d . . . C04 C 0.9112(2) 0.6375(2) 0.04299(19) 0.0433(6) Uani 1 1 d . . . C4 C 0.8762(2) 0.54776(18) 0.06421(17) 0.0359(5) Uani 1 1 d . . . C05 C 1.0771(2) 0.5788(2) 0.16887(19) 0.0428(5) Uani 1 1 d . . . C5 C 0.9530(2) 0.52322(18) 0.12323(17) 0.0353(5) Uani 1 1 d . . . P1 P 1.13384(5) 0.22412(4) 0.31195(4) 0.02962(13) Uani 1 1 d . . . P2 P 0.86257(5) 0.07003(4) 0.16036(4) 0.03095(13) Uani 1 1 d . . . C11 C 1.07921(19) 0.07085(17) 0.23959(17) 0.0343(5) Uani 1 1 d . . . H11A H 1.1442 0.0490 0.2270 0.041 Uiso 1 1 calc R . . H11B H 1.0475 0.0386 0.2798 0.041 Uiso 1 1 calc R . . C12 C 0.98217(19) 0.02655(18) 0.13658(17) 0.0356(5) Uani 1 1 d . . . H12A H 0.9509 -0.0560 0.0973 0.043 Uiso 1 1 calc R . . H12B H 1.0151 0.0562 0.0952 0.043 Uiso 1 1 calc R . . C111 C 1.22443(18) 0.27399(17) 0.24856(16) 0.0310(4) Uani 1 1 d . . . C112 C 1.2294(2) 0.37225(19) 0.24884(18) 0.0372(5) Uani 1 1 d . . . H112 H 1.1842 0.4092 0.2790 0.045 Uiso 1 1 calc R . . C113 C 1.3004(2) 0.4161(2) 0.20497(19) 0.0415(5) Uani 1 1 d . . . H113 H 1.3046 0.4839 0.2063 0.050 Uiso 1 1 calc R . . C114 C 1.3645(2) 0.3626(2) 0.15971(18) 0.0407(5) Uani 1 1 d . . . H114 H 1.4135 0.3934 0.1304 0.049 Uiso 1 1 calc R . . C115 C 1.3577(2) 0.2640(2) 0.15686(18) 0.0414(5) Uani 1 1 d . . . H115 H 1.4009 0.2260 0.1242 0.050 Uiso 1 1 calc R . . C116 C 1.2882(2) 0.21969(19) 0.20147(18) 0.0384(5) Uani 1 1 d . . . H116 H 1.2844 0.1519 0.1996 0.046 Uiso 1 1 calc R . . C121 C 1.24025(19) 0.26983(19) 0.43575(17) 0.0351(5) Uani 1 1 d . . . C122 C 1.3088(2) 0.3832(2) 0.49967(19) 0.0465(6) Uani 1 1 d . . . H122 H 1.3027 0.4340 0.4761 0.056 Uiso 1 1 calc R . . C123 C 1.3861(2) 0.4232(2) 0.5979(2) 0.0565(7) Uani 1 1 d . . . H123 H 1.4327 0.5011 0.6406 0.068 Uiso 1 1 calc R . . C124 C 1.3958(3) 0.3516(3) 0.6338(2) 0.0581(7) Uani 1 1 d . . . H124 H 1.4486 0.3794 0.7011 0.070 Uiso 1 1 calc R . . C125 C 1.3292(3) 0.2404(3) 0.5719(2) 0.0587(7) Uani 1 1 d . . . H125 H 1.3358 0.1906 0.5966 0.070 Uiso 1 1 calc R . . C126 C 1.2515(2) 0.1981(2) 0.4732(2) 0.0482(6) Uani 1 1 d . . . H126 H 1.2060 0.1199 0.4311 0.058 Uiso 1 1 calc R . . C211 C 0.78013(19) 0.05532(17) 0.03966(16) 0.0332(5) Uani 1 1 d . . . C212 C 0.6588(2) -0.00224(19) -0.00547(17) 0.0385(5) Uani 1 1 d . . . H212 H 0.6177 -0.0411 0.0231 0.046 Uiso 1 1 calc R . . C213 C 0.5974(2) -0.0032(2) -0.0923(2) 0.0490(6) Uani 1 1 d . . . H213 H 0.5144 -0.0427 -0.1228 0.059 Uiso 1 1 calc R . . C214 C 0.6565(3) 0.0532(2) -0.1345(2) 0.0522(6) Uani 1 1 d . . . H214 H 0.6143 0.0520 -0.1941 0.063 Uiso 1 1 calc R . . C215 C 0.7764(2) 0.1109(2) -0.0900(2) 0.0472(6) Uani 1 1 d . . . H215 H 0.8170 0.1497 -0.1190 0.057 Uiso 1 1 calc R . . C216 C 0.8385(2) 0.11285(19) -0.00294(18) 0.0391(5) Uani 1 1 d . . . H216 H 0.9213 0.1536 0.0278 0.047 Uiso 1 1 calc R . . C221 C 0.76457(19) -0.03796(18) 0.17470(16) 0.0352(5) Uani 1 1 d . . . C222 C 0.7436(2) -0.15005(19) 0.12069(18) 0.0426(5) Uani 1 1 d . . . H222 H 0.7835 -0.1736 0.0750 0.051 Uiso 1 1 calc R . . C223 C 0.6638(3) -0.2280(2) 0.1338(2) 0.0557(7) Uani 1 1 d . . . H223 H 0.6500 -0.3046 0.0974 0.067 Uiso 1 1 calc R . . C224 C 0.6045(3) -0.1942(2) 0.1997(2) 0.0583(8) Uani 1 1 d . . . H224 H 0.5503 -0.2477 0.2082 0.070 Uiso 1 1 calc R . . C225 C 0.6237(3) -0.0846(3) 0.2521(2) 0.0664(8) Uani 1 1 d . . . H225 H 0.5821 -0.0616 0.2962 0.080 Uiso 1 1 calc R . . C226 C 0.7052(2) -0.0061(2) 0.2404(2) 0.0544(7) Uani 1 1 d . . . H226 H 0.7200 0.0706 0.2784 0.065 Uiso 1 1 calc R . . P3 P 0.93515(5) 0.31773(4) 0.44736(4) 0.03023(13) Uani 1 1 d . . . C31 C 1.0206(2) 0.46969(17) 0.52640(17) 0.0354(5) Uani 1 1 d . . . H31A H 1.0116 0.4965 0.5943 0.043 Uiso 1 1 calc R . . H31B H 1.1049 0.4869 0.5380 0.043 Uiso 1 1 calc R . . C311 C 0.7885(2) 0.30785(18) 0.44534(18) 0.0367(5) Uani 1 1 d . . . C312 C 0.7066(2) 0.2825(2) 0.3557(2) 0.0468(6) Uani 1 1 d . . . H312 H 0.7256 0.2657 0.2955 0.056 Uiso 1 1 calc R . . C313 C 0.5965(3) 0.2813(3) 0.3528(3) 0.0710(9) Uani 1 1 d . . . H313 H 0.5400 0.2637 0.2909 0.085 Uiso 1 1 calc R . . C314 C 0.5696(3) 0.3063(3) 0.4416(3) 0.0852(12) Uani 1 1 d . . . H314 H 0.4942 0.3050 0.4403 0.102 Uiso 1 1 calc R . . C315 C 0.6504(3) 0.3323(3) 0.5293(3) 0.0853(12) Uani 1 1 d . . . H315 H 0.6315 0.3503 0.5897 0.102 Uiso 1 1 calc R . . C316 C 0.7602(3) 0.3334(3) 0.5334(2) 0.0632(8) Uani 1 1 d . . . H316 H 0.8160 0.3514 0.5958 0.076 Uiso 1 1 calc R . . C321 C 0.9813(2) 0.2655(2) 0.53267(19) 0.0460(6) Uani 1 1 d . . . C322 C 1.0806(2) 0.3258(2) 0.62072(19) 0.0499(6) Uani 1 1 d . . . H322 H 1.1271 0.4010 0.6415 0.060 Uiso 1 1 calc R . . C323 C 1.1140(3) 0.2806(3) 0.6791(2) 0.0611(8) Uani 1 1 d . . . H323 H 1.1822 0.3249 0.7400 0.073 Uiso 1 1 calc R . . C324 C 1.0523(4) 0.1757(4) 0.6515(4) 0.1223(19) Uani 1 1 d . . . H324 H 1.0721 0.1460 0.6947 0.147 Uiso 1 1 calc R . . C325 C 0.9608(6) 0.1113(5) 0.5612(6) 0.242(5) Uani 1 1 d . . . H325 H 0.9229 0.0334 0.5359 0.291 Uiso 1 1 calc R . . C326 C 0.9212(4) 0.1588(4) 0.5041(4) 0.169(3) Uani 1 1 d . . . H326 H 0.8512 0.1146 0.4449 0.203 Uiso 1 1 calc R . . C1X C 0.2857(13) -0.091(3) 0.3878(18) 0.178(5) Uiso 0.25 1 d PD A -1 H1X1 H 0.2408 -0.1274 0.3140 0.266 Uiso 0.25 1 calc PR A -1 H1X2 H 0.2704 -0.0253 0.4249 0.266 Uiso 0.25 1 calc PR A -1 H1X3 H 0.2620 -0.1434 0.4130 0.266 Uiso 0.25 1 calc PR A -1 C2X C 0.4139(14) -0.056(2) 0.4054(13) 0.163(5) Uiso 0.25 1 d PD A -1 H2X1 H 0.4240 -0.1117 0.3468 0.195 Uiso 0.25 1 calc PR A -1 H2X2 H 0.4433 0.0162 0.4059 0.195 Uiso 0.25 1 calc PR A -1 C3X C 0.4874(13) -0.0421(17) 0.5028(15) 0.148(4) Uiso 0.25 1 d PD A -1 H3X1 H 0.4498 -0.0228 0.5547 0.178 Uiso 0.25 1 calc PR A -1 H3X2 H 0.4942 -0.1132 0.4898 0.178 Uiso 0.25 1 calc PR A -1 C4X C 0.6076(14) 0.049(2) 0.5429(16) 0.163(5) Uiso 0.25 1 d PD A -1 H4X1 H 0.5992 0.1190 0.5548 0.195 Uiso 0.25 1 calc PR A -1 H4X2 H 0.6432 0.0291 0.4895 0.195 Uiso 0.25 1 calc PR A -1 C5X C 0.6894(15) 0.069(2) 0.6404(17) 0.178(5) Uiso 0.25 1 d PD A -1 H5X1 H 0.7686 0.0849 0.6382 0.266 Uiso 0.25 1 calc PR A -1 H5X2 H 0.6626 0.0027 0.6478 0.266 Uiso 0.25 1 calc PR A -1 H5X3 H 0.6905 0.1330 0.6990 0.266 Uiso 0.25 1 calc PR A -1 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 Cu1 0.02969(15) 0.02604(14) 0.02984(15) 0.01103(11) 0.01056(11) 0.01140(11) N1 0.0390(11) 0.0322(10) 0.0349(10) 0.0148(9) 0.0138(8) 0.0143(9) N2 0.0550(15) 0.0535(14) 0.0870(18) 0.0427(14) 0.0374(14) 0.0199(12) N3 0.0433(13) 0.0547(14) 0.0756(16) 0.0443(14) 0.0113(12) 0.0121(11) N4 0.0559(15) 0.0562(15) 0.0807(17) 0.0480(14) 0.0189(13) 0.0139(12) N5 0.0447(14) 0.0641(16) 0.0622(16) 0.0257(13) 0.0109(12) 0.0159(12) C1 0.0449(13) 0.0333(11) 0.0329(11) 0.0178(10) 0.0170(10) 0.0175(10) C01 0.0392(12) 0.0296(11) 0.0332(11) 0.0117(10) 0.0156(10) 0.0146(10) C02 0.0442(14) 0.0407(13) 0.0513(15) 0.0274(12) 0.0222(12) 0.0193(12) C2 0.0397(13) 0.0333(11) 0.0383(12) 0.0199(10) 0.0183(10) 0.0146(10) C03 0.0430(14) 0.0369(13) 0.0533(15) 0.0293(12) 0.0163(12) 0.0112(11) C3 0.0374(12) 0.0357(12) 0.0387(12) 0.0205(10) 0.0145(10) 0.0139(10) C04 0.0379(13) 0.0440(14) 0.0481(14) 0.0267(12) 0.0133(11) 0.0121(11) C4 0.0408(13) 0.0328(11) 0.0370(12) 0.0192(10) 0.0165(10) 0.0141(10) C05 0.0457(15) 0.0400(13) 0.0413(13) 0.0202(12) 0.0145(12) 0.0164(12) C5 0.0387(12) 0.0329(11) 0.0339(11) 0.0157(10) 0.0141(10) 0.0146(10) P1 0.0276(3) 0.0276(3) 0.0315(3) 0.0128(2) 0.0105(2) 0.0114(2) P2 0.0301(3) 0.0255(3) 0.0299(3) 0.0091(2) 0.0107(2) 0.0087(2) C11 0.0347(12) 0.0291(11) 0.0392(12) 0.0153(10) 0.0148(10) 0.0145(9) C12 0.0358(12) 0.0284(11) 0.0358(12) 0.0093(10) 0.0145(10) 0.0127(10) C111 0.0267(10) 0.0315(11) 0.0307(11) 0.0144(9) 0.0080(9) 0.0098(9) C112 0.0325(11) 0.0355(12) 0.0438(13) 0.0181(11) 0.0153(10) 0.0154(10) C113 0.0400(13) 0.0373(12) 0.0516(14) 0.0261(12) 0.0167(11) 0.0152(11) C114 0.0357(12) 0.0472(14) 0.0400(13) 0.0236(11) 0.0155(10) 0.0137(11) C115 0.0409(13) 0.0425(13) 0.0433(13) 0.0189(12) 0.0218(11) 0.0190(11) C116 0.0401(13) 0.0356(12) 0.0452(13) 0.0210(11) 0.0199(11) 0.0184(10) C121 0.0301(11) 0.0409(12) 0.0339(11) 0.0165(10) 0.0125(9) 0.0166(10) C122 0.0445(14) 0.0418(14) 0.0417(14) 0.0192(12) 0.0051(11) 0.0118(12) C123 0.0480(16) 0.0518(16) 0.0441(15) 0.0147(13) 0.0032(12) 0.0090(13) C124 0.0476(16) 0.077(2) 0.0425(15) 0.0306(16) 0.0068(12) 0.0214(15) C125 0.0641(19) 0.0635(19) 0.0514(16) 0.0352(16) 0.0098(14) 0.0273(16) C126 0.0529(16) 0.0443(14) 0.0479(15) 0.0261(13) 0.0129(12) 0.0188(12) C211 0.0354(12) 0.0279(10) 0.0281(10) 0.0079(9) 0.0107(9) 0.0116(9) C212 0.0356(12) 0.0349(12) 0.0357(12) 0.0111(10) 0.0114(10) 0.0125(10) C213 0.0379(13) 0.0509(15) 0.0437(14) 0.0142(12) 0.0073(11) 0.0183(12) C214 0.0583(17) 0.0585(17) 0.0407(14) 0.0248(13) 0.0119(13) 0.0287(14) C215 0.0590(17) 0.0443(14) 0.0445(14) 0.0241(12) 0.0235(13) 0.0226(13) C216 0.0397(13) 0.0338(12) 0.0381(12) 0.0151(10) 0.0146(10) 0.0111(10) C221 0.0323(11) 0.0315(11) 0.0312(11) 0.0134(10) 0.0062(9) 0.0058(9) C222 0.0472(14) 0.0338(12) 0.0393(13) 0.0170(11) 0.0097(11) 0.0123(11) C223 0.0595(17) 0.0346(13) 0.0565(17) 0.0243(13) 0.0044(14) 0.0060(13) C224 0.0583(18) 0.0480(16) 0.0459(15) 0.0263(14) 0.0071(14) -0.0050(13) C225 0.067(2) 0.0580(18) 0.0582(18) 0.0235(16) 0.0335(16) 0.0050(16) C226 0.0577(17) 0.0381(14) 0.0525(16) 0.0152(13) 0.0256(14) 0.0065(13) P3 0.0305(3) 0.0268(3) 0.0281(3) 0.0097(2) 0.0087(2) 0.0116(2) C31 0.0332(11) 0.0275(11) 0.0339(11) 0.0082(9) 0.0071(9) 0.0110(9) C311 0.0313(11) 0.0286(11) 0.0401(12) 0.0096(10) 0.0153(10) 0.0083(9) C312 0.0353(13) 0.0447(14) 0.0537(15) 0.0199(13) 0.0119(11) 0.0169(11) C313 0.0381(16) 0.0600(19) 0.091(2) 0.0223(18) 0.0090(16) 0.0215(15) C314 0.0388(17) 0.064(2) 0.120(3) 0.015(2) 0.037(2) 0.0181(16) C315 0.054(2) 0.080(2) 0.078(2) 0.0017(19) 0.0425(19) 0.0118(18) C316 0.0464(16) 0.0667(19) 0.0484(16) 0.0107(15) 0.0238(14) 0.0083(15) C321 0.0516(15) 0.0431(14) 0.0396(13) 0.0236(12) 0.0088(12) 0.0152(12) C322 0.0561(16) 0.0565(16) 0.0397(14) 0.0227(13) 0.0141(12) 0.0302(14) C323 0.0665(19) 0.085(2) 0.0429(15) 0.0319(16) 0.0194(14) 0.0450(18) C324 0.110(3) 0.127(4) 0.127(4) 0.105(4) -0.011(3) 0.017(3) C325 0.180(6) 0.156(5) 0.262(8) 0.181(6) -0.126(6) -0.077(4) C326 0.144(4) 0.097(3) 0.168(5) 0.108(4) -0.084(4) -0.050(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.9948(18) . ? Cu1 P3 2.2500(6) . ? Cu1 P1 2.2777(6) . ? Cu1 P2 2.2865(6) . ? N1 C01 1.140(3) . ? N2 C02 1.138(3) . ? N3 C03 1.154(3) . ? N4 C04 1.141(3) . ? N5 C05 1.137(3) . ? C1 C2 1.411(3) . ? C1 C01 1.418(3) . ? C1 C5 1.415(3) . ? C02 C2 1.434(3) . ? C2 C3 1.403(3) . ? C03 C3 1.413(3) . ? C3 C4 1.406(3) . ? C04 C4 1.428(3) . ? C4 C5 1.410(3) . ? C05 C5 1.417(3) . ? P1 C121 1.814(2) . ? P1 C111 1.823(2) . ? P1 C11 1.842(2) . ? P2 C221 1.818(2) . ? P2 C211 1.822(2) . ? P2 C12 1.846(2) . ? C11 C12 1.537(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C111 C116 1.383(3) . ? C111 C112 1.393(3) . ? C112 C113 1.388(3) . ? C112 H112 0.9500 . ? C113 C114 1.371(3) . ? C113 H113 0.9500 . ? C114 C115 1.376(3) . ? C114 H114 0.9500 . ? C115 C116 1.388(3) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C126 1.393(3) . ? C121 C122 1.387(3) . ? C122 C123 1.389(4) . ? C122 H122 0.9500 . ? C123 C124 1.370(4) . ? C123 H123 0.9500 . ? C124 C125 1.359(4) . ? C124 H124 0.9500 . ? C125 C126 1.389(4) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C211 C212 1.389(3) . ? C211 C216 1.394(3) . ? C212 C213 1.389(3) . ? C212 H212 0.9500 . ? C213 C214 1.383(4) . ? C213 H213 0.9500 . ? C214 C215 1.373(4) . ? C214 H214 0.9500 . ? C215 C216 1.388(3) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C226 1.381(3) . ? C221 C222 1.389(3) . ? C222 C223 1.396(3) . ? C222 H222 0.9500 . ? C223 C224 1.388(4) . ? C223 H223 0.9500 . ? C224 C225 1.361(4) . ? C224 H224 0.9500 . ? C225 C226 1.399(4) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? P3 C311 1.823(2) . ? P3 C321 1.828(2) . ? P3 C31 1.840(2) . ? C31 C31 1.530(4) 2_766 ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C311 C312 1.377(3) . ? C311 C316 1.391(4) . ? C312 C313 1.387(4) . ? C312 H312 0.9500 . ? C313 C314 1.392(5) . ? C313 H313 0.9500 . ? C314 C315 1.345(5) . ? C314 H314 0.9500 . ? C315 C316 1.381(4) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? C321 C326 1.336(4) . ? C321 C322 1.379(4) . ? C322 C323 1.369(4) . ? C322 H322 0.9500 . ? C323 C324 1.321(5) . ? C323 H323 0.9500 . ? C324 C325 1.348(6) . ? C324 H324 0.9500 . ? C325 C326 1.407(5) . ? C325 H325 0.9500 . ? C326 H326 0.9500 . ? C1X C2X 1.494(10) . ? C1X H1X1 0.9800 . ? C1X H1X2 0.9800 . ? C1X H1X3 0.9800 . ? C2X C3X 1.491(10) . ? C2X H2X1 0.9900 . ? C2X H2X2 0.9900 . ? C3X C4X 1.505(10) . ? C3X H3X1 0.9900 . ? C3X H3X2 0.9900 . ? C4X C5X 1.494(10) . ? C4X H4X1 0.9900 . ? C4X H4X2 0.9900 . ? C5X H5X1 0.9800 . ? C5X H5X2 0.9800 . ? C5X H5X3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 P3 109.54(5) . . ? N1 Cu1 P1 113.44(6) . . ? P3 Cu1 P1 112.65(2) . . ? N1 Cu1 P2 102.69(6) . . ? P3 Cu1 P2 127.00(2) . . ? P1 Cu1 P2 90.28(2) . . ? C01 N1 Cu1 170.04(19) . . ? C2 C1 C01 124.5(2) . . ? C2 C1 C5 108.39(19) . . ? C01 C1 C5 127.1(2) . . ? N1 C01 C1 176.1(2) . . ? N2 C02 C2 176.9(3) . . ? C3 C2 C1 107.99(19) . . ? C3 C2 C02 127.4(2) . . ? C1 C2 C02 124.6(2) . . ? N3 C03 C3 179.3(2) . . ? C2 C3 C4 107.9(2) . . ? C2 C3 C03 125.1(2) . . ? C4 C3 C03 127.05(19) . . ? N4 C04 C4 179.4(3) . . ? C3 C4 C5 108.82(18) . . ? C3 C4 C04 125.9(2) . . ? C5 C4 C04 125.2(2) . . ? N5 C05 C5 179.0(3) . . ? C4 C5 C1 106.9(2) . . ? C4 C5 C05 127.3(2) . . ? C1 C5 C05 125.8(2) . . ? C121 P1 C111 103.11(10) . . ? C121 P1 C11 106.44(10) . . ? C111 P1 C11 105.22(10) . . ? C121 P1 Cu1 122.29(7) . . ? C111 P1 Cu1 116.78(7) . . ? C11 P1 Cu1 101.44(7) . . ? C221 P2 C211 105.10(10) . . ? C221 P2 C12 105.43(10) . . ? C211 P2 C12 105.61(10) . . ? C221 P2 Cu1 120.17(7) . . ? C211 P2 Cu1 116.56(7) . . ? C12 P2 Cu1 102.50(7) . . ? C12 C11 P1 108.78(14) . . ? C12 C11 H11A 109.9 . . ? P1 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? P1 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C11 C12 P2 109.79(15) . . ? C11 C12 H12A 109.7 . . ? P2 C12 H12A 109.7 . . ? C11 C12 H12B 109.7 . . ? P2 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? C116 C111 C112 119.10(19) . . ? C116 C111 P1 123.31(16) . . ? C112 C111 P1 117.59(16) . . ? C113 C112 C111 120.0(2) . . ? C113 C112 H112 120.0 . . ? C111 C112 H112 120.0 . . ? C114 C113 C112 120.5(2) . . ? C114 C113 H113 119.7 . . ? C112 C113 H113 119.7 . . ? C115 C114 C113 119.8(2) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 120.3(2) . . ? C114 C115 H115 119.8 . . ? C116 C115 H115 119.8 . . ? C111 C116 C115 120.2(2) . . ? C111 C116 H116 119.9 . . ? C115 C116 H116 119.9 . . ? C126 C121 C122 118.0(2) . . ? C126 C121 P1 123.52(19) . . ? C122 C121 P1 118.36(17) . . ? C121 C122 C123 120.6(2) . . ? C121 C122 H122 119.7 . . ? C123 C122 H122 119.7 . . ? C124 C123 C122 120.7(3) . . ? C124 C123 H123 119.7 . . ? C122 C123 H123 119.7 . . ? C125 C124 C123 119.2(3) . . ? C125 C124 H124 120.4 . . ? C123 C124 H124 120.4 . . ? C124 C125 C126 121.3(2) . . ? C124 C125 H125 119.3 . . ? C126 C125 H125 119.3 . . ? C121 C126 C125 120.2(3) . . ? C121 C126 H126 119.9 . . ? C125 C126 H126 119.9 . . ? C212 C211 C216 118.9(2) . . ? C212 C211 P2 121.69(17) . . ? C216 C211 P2 119.11(17) . . ? C213 C212 C211 120.3(2) . . ? C213 C212 H212 119.9 . . ? C211 C212 H212 119.9 . . ? C214 C213 C212 120.3(2) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C213 C214 C215 119.9(2) . . ? C213 C214 H214 120.1 . . ? C215 C214 H214 120.1 . . ? C214 C215 C216 120.3(2) . . ? C214 C215 H215 119.9 . . ? C216 C215 H215 119.9 . . ? C215 C216 C211 120.4(2) . . ? C215 C216 H216 119.8 . . ? C211 C216 H216 119.8 . . ? C226 C221 C222 118.9(2) . . ? C226 C221 P2 117.47(18) . . ? C222 C221 P2 123.54(18) . . ? C221 C222 C223 119.8(2) . . ? C221 C222 H222 120.1 . . ? C223 C222 H222 120.1 . . ? C224 C223 C222 120.3(3) . . ? C224 C223 H223 119.8 . . ? C222 C223 H223 119.8 . . ? C225 C224 C223 120.2(2) . . ? C225 C224 H224 119.9 . . ? C223 C224 H224 119.9 . . ? C224 C225 C226 119.5(3) . . ? C224 C225 H225 120.2 . . ? C226 C225 H225 120.2 . . ? C221 C226 C225 121.2(3) . . ? C221 C226 H226 119.4 . . ? C225 C226 H226 119.4 . . ? C311 P3 C321 104.67(11) . . ? C311 P3 C31 100.80(10) . . ? C321 P3 C31 103.35(11) . . ? C311 P3 Cu1 118.49(8) . . ? C321 P3 Cu1 115.79(9) . . ? C31 P3 Cu1 111.71(8) . . ? C31 C31 P3 110.9(2) 2_766 . ? C31 C31 H31A 109.5 2_766 . ? P3 C31 H31A 109.5 . . ? C31 C31 H31B 109.5 2_766 . ? P3 C31 H31B 109.5 . . ? H31A C31 H31B 108.0 . . ? C312 C311 C316 119.3(2) . . ? C312 C311 P3 118.63(18) . . ? C316 C311 P3 121.9(2) . . ? C311 C312 C313 120.4(3) . . ? C311 C312 H312 119.8 . . ? C313 C312 H312 119.8 . . ? C312 C313 C314 119.3(3) . . ? C312 C313 H313 120.3 . . ? C314 C313 H313 120.3 . . ? C315 C314 C313 120.0(3) . . ? C315 C314 H314 120.0 . . ? C313 C314 H314 120.0 . . ? C314 C315 C316 121.4(3) . . ? C314 C315 H315 119.3 . . ? C316 C315 H315 119.3 . . ? C315 C316 C311 119.5(3) . . ? C315 C316 H316 120.3 . . ? C311 C316 H316 120.3 . . ? C326 C321 C322 116.9(3) . . ? C326 C321 P3 118.3(2) . . ? C322 C321 P3 124.5(2) . . ? C323 C322 C321 122.0(3) . . ? C323 C322 H322 119.0 . . ? C321 C322 H322 119.0 . . ? C324 C323 C322 120.5(3) . . ? C324 C323 H323 119.8 . . ? C322 C323 H323 119.8 . . ? C323 C324 C325 119.2(3) . . ? C323 C324 H324 120.4 . . ? C325 C324 H324 120.4 . . ? C324 C325 C326 120.4(5) . . ? C324 C325 H325 119.8 . . ? C326 C325 H325 119.8 . . ? C321 C326 C325 120.4(4) . . ? C321 C326 H326 119.8 . . ? C325 C326 H326 119.8 . . ? C2X C1X H1X1 109.5 . . ? C2X C1X H1X2 109.5 . . ? H1X1 C1X H1X2 109.5 . . ? C2X C1X H1X3 109.5 . . ? H1X1 C1X H1X3 109.5 . . ? H1X2 C1X H1X3 109.5 . . ? C3X C2X C1X 114.8(10) . . ? C3X C2X H2X1 108.6 . . ? C1X C2X H2X1 108.6 . . ? C3X C2X H2X2 108.6 . . ? C1X C2X H2X2 108.6 . . ? H2X1 C2X H2X2 107.6 . . ? C4X C3X C2X 109.6(9) . . ? C4X C3X H3X1 109.7 . . ? C2X C3X H3X1 109.7 . . ? C4X C3X H3X2 109.7 . . ? C2X C3X H3X2 109.7 . . ? H3X1 C3X H3X2 108.2 . . ? C3X C4X C5X 114.3(10) . . ? C3X C4X H4X1 108.7 . . ? C5X C4X H4X1 108.7 . . ? C3X C4X H4X2 108.7 . . ? C5X C4X H4X2 108.7 . . ? H4X1 C4X H4X2 107.6 . . ? C4X C5X H5X1 109.5 . . ? C4X C5X H5X2 109.5 . . ? H5X1 C5X H5X2 109.5 . . ? C4X C5X H5X3 109.5 . . ? H5X1 C5X H5X3 109.5 . . ? H5X2 C5X H5X3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.818 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.072 # Attachment '- Compound7.cif' data_dw1164 _database_code_depnum_ccdc_archive 'CCDC 866134' #TrackingRef '- Compound7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Au P2 1+, C10 N5 1-' _chemical_formula_sum 'C46 H30 Au N5 P2' _chemical_formula_weight 911.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3138(2) _cell_length_b 12.4831(2) _cell_length_c 15.4936(4) _cell_angle_alpha 69.145(1) _cell_angle_beta 81.391(1) _cell_angle_gamma 69.918(1) _cell_volume 1919.56(7) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 26362 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 32.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 3.956 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.692 _exptl_absorpt_correction_T_max 0.931 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 29144 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 32.03 _reflns_number_total 13234 _reflns_number_gt 10043 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V. 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0242P)^2^+3.7216P] 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 13234 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.249456(15) 0.354460(14) -0.208494(12) 0.02806(5) Uani 1 1 d . . . P1 P 0.44584(9) 0.37768(9) -0.21729(7) 0.0250(2) Uani 1 1 d . . . P2 P 0.04300(9) 0.36017(9) -0.20868(7) 0.0240(2) Uani 1 1 d . . . C31 C 0.5505(4) 0.3232(3) -0.3049(3) 0.0266(8) Uani 1 1 d . . . C32 C 0.5033(4) 0.3610(4) -0.3925(3) 0.0335(9) Uani 1 1 d . . . H32 H 0.4178 0.4094 -0.4032 0.040 Uiso 1 1 calc R . . C33 C 0.5783(5) 0.3293(4) -0.4638(3) 0.0411(11) Uani 1 1 d . . . H33 H 0.5450 0.3561 -0.5234 0.049 Uiso 1 1 calc R . . C34 C 0.7034(5) 0.2578(4) -0.4481(3) 0.0411(11) Uani 1 1 d . . . H34 H 0.7564 0.2359 -0.4968 0.049 Uiso 1 1 calc R . . C35 C 0.7496(4) 0.2191(4) -0.3610(3) 0.0374(10) Uani 1 1 d . . . H35 H 0.8346 0.1695 -0.3500 0.045 Uiso 1 1 calc R . . C36 C 0.6748(4) 0.2508(4) -0.2899(3) 0.0311(9) Uani 1 1 d . . . H36 H 0.7083 0.2231 -0.2303 0.037 Uiso 1 1 calc R . . C41 C 0.5274(4) 0.3008(4) -0.1090(3) 0.0276(8) Uani 1 1 d . . . C42 C 0.5542(5) 0.1759(4) -0.0720(3) 0.0362(10) Uani 1 1 d . . . H42 H 0.5305 0.1340 -0.1035 0.043 Uiso 1 1 calc R . . C43 C 0.6155(5) 0.1128(4) 0.0107(3) 0.0429(12) Uani 1 1 d . . . H43 H 0.6352 0.0275 0.0353 0.051 Uiso 1 1 calc R . . C44 C 0.6481(5) 0.1737(5) 0.0577(3) 0.0436(12) Uani 1 1 d . . . H44 H 0.6897 0.1301 0.1147 0.052 Uiso 1 1 calc R . . C45 C 0.6206(5) 0.2969(5) 0.0225(3) 0.0467(13) Uani 1 1 d . . . H45 H 0.6424 0.3383 0.0555 0.056 Uiso 1 1 calc R . . C46 C 0.5609(5) 0.3614(4) -0.0613(3) 0.0380(10) Uani 1 1 d . . . H46 H 0.5431 0.4465 -0.0859 0.046 Uiso 1 1 calc R . . C51 C 0.4361(4) 0.5355(4) -0.2513(3) 0.0272(8) Uani 1 1 d . . . C52 C 0.5449(4) 0.5695(4) -0.2705(3) 0.0342(9) Uani 1 1 d . . . H52 H 0.6251 0.5095 -0.2648 0.041 Uiso 1 1 calc R . . C53 C 0.5368(5) 0.6903(4) -0.2978(3) 0.0414(11) Uani 1 1 d . . . H53 H 0.6113 0.7129 -0.3109 0.050 Uiso 1 1 calc R . . C54 C 0.4203(5) 0.7778(4) -0.3059(4) 0.0427(11) Uani 1 1 d . . . H54 H 0.4147 0.8605 -0.3239 0.051 Uiso 1 1 calc R . . C55 C 0.3122(5) 0.7450(4) -0.2879(4) 0.0399(11) Uani 1 1 d . . . H55 H 0.2322 0.8053 -0.2944 0.048 Uiso 1 1 calc R . . C56 C 0.3199(4) 0.6233(4) -0.2601(3) 0.0307(9) Uani 1 1 d . . . H56 H 0.2452 0.6011 -0.2472 0.037 Uiso 1 1 calc R . . C61 C 0.0193(4) 0.2167(3) -0.1896(3) 0.0262(8) Uani 1 1 d . . . C62 C -0.0598(4) 0.1704(4) -0.1190(3) 0.0303(9) Uani 1 1 d . . . H62 H -0.1053 0.2149 -0.0794 0.036 Uiso 1 1 calc R . . C63 C -0.0720(5) 0.0584(4) -0.1069(3) 0.0381(10) Uani 1 1 d . . . H63 H -0.1252 0.0264 -0.0585 0.046 Uiso 1 1 calc R . . C64 C -0.0072(5) -0.0061(4) -0.1647(3) 0.0388(11) Uani 1 1 d . . . H64 H -0.0148 -0.0829 -0.1556 0.047 Uiso 1 1 calc R . . C65 C 0.0684(5) 0.0409(4) -0.2355(3) 0.0398(11) Uani 1 1 d . . . H65 H 0.1109 -0.0023 -0.2766 0.048 Uiso 1 1 calc R . . C66 C 0.0833(4) 0.1515(4) -0.2476(3) 0.0320(9) Uani 1 1 d . . . H66 H 0.1375 0.1823 -0.2958 0.038 Uiso 1 1 calc R . . C71 C -0.0268(4) 0.4593(4) -0.3186(3) 0.0278(8) Uani 1 1 d . . . C72 C 0.0145(5) 0.5584(4) -0.3692(3) 0.0385(10) Uani 1 1 d . . . H72 H 0.0837 0.5692 -0.3491 0.046 Uiso 1 1 calc R . . C73 C -0.0463(6) 0.6404(4) -0.4486(4) 0.0509(14) Uani 1 1 d . . . H73 H -0.0185 0.7078 -0.4830 0.061 Uiso 1 1 calc R . . C74 C -0.1461(5) 0.6261(5) -0.4786(3) 0.0517(14) Uani 1 1 d . . . H74 H -0.1885 0.6844 -0.5325 0.062 Uiso 1 1 calc R . . C75 C -0.1847(5) 0.5268(5) -0.4304(3) 0.0485(13) Uani 1 1 d . . . H75 H -0.2517 0.5146 -0.4521 0.058 Uiso 1 1 calc R . . C76 C -0.1252(4) 0.4451(4) -0.3502(3) 0.0366(10) Uani 1 1 d . . . H76 H -0.1533 0.3777 -0.3164 0.044 Uiso 1 1 calc R . . C81 C -0.0560(4) 0.4208(4) -0.1231(3) 0.0259(8) Uani 1 1 d . . . C82 C -0.0222(4) 0.3664(4) -0.0304(3) 0.0348(10) Uani 1 1 d . . . H82 H 0.0525 0.2998 -0.0138 0.042 Uiso 1 1 calc R . . C83 C -0.0961(5) 0.4086(5) 0.0368(3) 0.0412(11) Uani 1 1 d . . . H83 H -0.0739 0.3700 0.0998 0.049 Uiso 1 1 calc R . . C84 C -0.2036(5) 0.5083(5) 0.0120(3) 0.0424(11) Uani 1 1 d . . . H84 H -0.2542 0.5382 0.0582 0.051 Uiso 1 1 calc R . . C85 C -0.2373(5) 0.5636(4) -0.0785(4) 0.0404(11) Uani 1 1 d . . . H85 H -0.3109 0.6316 -0.0947 0.048 Uiso 1 1 calc R . . C86 C -0.1645(4) 0.5206(4) -0.1461(3) 0.0323(9) Uani 1 1 d . . . H86 H -0.1884 0.5592 -0.2087 0.039 Uiso 1 1 calc R . . N1 N 0.3705(4) 0.1035(3) -0.2078(3) 0.0412(9) Uani 1 1 d . . . N2 N 0.4232(4) 0.1473(4) -0.4918(3) 0.0499(11) Uani 1 1 d . . . N3 N 0.8351(5) -0.0421(5) -0.5461(3) 0.0672(15) Uani 1 1 d . . . N4 N 1.0105(4) -0.2374(4) -0.2722(3) 0.0497(11) Uani 1 1 d . . . N5 N 0.7314(4) -0.1434(4) -0.0619(3) 0.0468(10) Uani 1 1 d . . . C11 C 0.5761(4) -0.0007(4) -0.2791(3) 0.0296(8) Uani 1 1 d . . . C12 C 0.5969(4) 0.0160(4) -0.3737(3) 0.0301(9) Uani 1 1 d . . . C13 C 0.7228(4) -0.0471(4) -0.3891(3) 0.0315(9) Uani 1 1 d . . . C14 C 0.7806(4) -0.1048(4) -0.3030(3) 0.0319(9) Uani 1 1 d . . . C15 C 0.6910(4) -0.0772(4) -0.2343(3) 0.0300(9) Uani 1 1 d . . . C21 C 0.4623(4) 0.0553(4) -0.2388(3) 0.0306(9) Uani 1 1 d . . . C22 C 0.5018(4) 0.0879(4) -0.4409(3) 0.0344(9) Uani 1 1 d . . . C23 C 0.7832(5) -0.0458(4) -0.4766(3) 0.0426(11) Uani 1 1 d . . . C24 C 0.9082(4) -0.1773(4) -0.2864(3) 0.0345(9) Uani 1 1 d . . . C25 C 0.7126(4) -0.1143(4) -0.1385(3) 0.0331(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 Au1 0.02194(8) 0.02938(8) 0.03396(8) -0.01050(6) -0.00021(5) -0.00954(6) P1 0.0196(5) 0.0245(5) 0.0306(5) -0.0079(4) -0.0019(4) -0.0072(4) P2 0.0204(5) 0.0251(5) 0.0277(5) -0.0096(4) -0.0002(4) -0.0081(4) C31 0.0232(19) 0.0249(18) 0.031(2) -0.0080(16) -0.0005(15) -0.0082(15) C32 0.036(2) 0.029(2) 0.030(2) -0.0060(17) -0.0088(18) -0.0054(18) C33 0.055(3) 0.039(2) 0.030(2) -0.0087(19) -0.003(2) -0.017(2) C34 0.052(3) 0.042(3) 0.035(2) -0.019(2) 0.010(2) -0.020(2) C35 0.027(2) 0.041(2) 0.045(3) -0.019(2) 0.0034(19) -0.0092(19) C36 0.026(2) 0.035(2) 0.034(2) -0.0108(18) -0.0033(17) -0.0119(17) C41 0.0227(19) 0.031(2) 0.030(2) -0.0097(16) 0.0005(15) -0.0100(16) C42 0.048(3) 0.035(2) 0.025(2) -0.0073(17) 0.0003(19) -0.016(2) C43 0.058(3) 0.033(2) 0.029(2) -0.0020(18) 0.000(2) -0.013(2) C44 0.043(3) 0.052(3) 0.029(2) -0.003(2) -0.008(2) -0.016(2) C45 0.060(3) 0.052(3) 0.035(2) -0.010(2) -0.013(2) -0.026(3) C46 0.043(3) 0.032(2) 0.039(2) -0.0062(19) -0.008(2) -0.014(2) C51 0.027(2) 0.0268(19) 0.030(2) -0.0096(16) -0.0012(16) -0.0109(16) C52 0.026(2) 0.029(2) 0.045(3) -0.0067(19) -0.0047(18) -0.0092(17) C53 0.039(3) 0.036(2) 0.050(3) -0.005(2) -0.004(2) -0.021(2) C54 0.049(3) 0.027(2) 0.053(3) -0.009(2) -0.009(2) -0.015(2) C55 0.035(3) 0.029(2) 0.056(3) -0.017(2) -0.005(2) -0.0049(18) C56 0.026(2) 0.028(2) 0.036(2) -0.0093(17) 0.0001(17) -0.0078(16) C61 0.025(2) 0.0245(18) 0.0286(19) -0.0074(15) -0.0054(15) -0.0071(15) C62 0.033(2) 0.030(2) 0.029(2) -0.0104(17) 0.0007(17) -0.0125(17) C63 0.042(3) 0.037(2) 0.036(2) -0.0040(19) -0.002(2) -0.021(2) C64 0.046(3) 0.030(2) 0.044(3) -0.010(2) -0.012(2) -0.014(2) C65 0.049(3) 0.028(2) 0.040(2) -0.0148(19) -0.005(2) -0.003(2) C66 0.029(2) 0.034(2) 0.031(2) -0.0123(17) 0.0018(17) -0.0063(17) C71 0.027(2) 0.0273(19) 0.0264(19) -0.0100(16) 0.0020(15) -0.0050(16) C72 0.047(3) 0.031(2) 0.036(2) -0.0083(19) 0.001(2) -0.015(2) C73 0.063(4) 0.030(2) 0.039(3) 0.001(2) 0.007(2) -0.006(2) C74 0.049(3) 0.049(3) 0.031(2) -0.005(2) -0.001(2) 0.009(2) C75 0.042(3) 0.058(3) 0.039(3) -0.015(2) -0.010(2) -0.004(2) C76 0.032(2) 0.041(2) 0.033(2) -0.0072(19) -0.0073(18) -0.0101(19) C81 0.026(2) 0.0284(19) 0.0281(19) -0.0129(16) 0.0002(15) -0.0111(16) C82 0.036(2) 0.038(2) 0.033(2) -0.0114(19) -0.0081(19) -0.0122(19) C83 0.050(3) 0.056(3) 0.028(2) -0.020(2) 0.003(2) -0.025(2) C84 0.047(3) 0.054(3) 0.038(2) -0.029(2) 0.014(2) -0.022(2) C85 0.035(3) 0.040(2) 0.051(3) -0.026(2) 0.004(2) -0.008(2) C86 0.029(2) 0.032(2) 0.035(2) -0.0116(18) -0.0010(17) -0.0080(17) N1 0.039(2) 0.0315(19) 0.045(2) -0.0082(17) -0.0027(18) -0.0056(17) N2 0.048(3) 0.045(2) 0.046(2) -0.011(2) -0.016(2) 0.000(2) N3 0.079(4) 0.058(3) 0.041(3) -0.007(2) 0.010(3) -0.008(3) N4 0.035(2) 0.052(3) 0.060(3) -0.028(2) -0.008(2) 0.000(2) N5 0.047(3) 0.047(2) 0.043(2) -0.017(2) -0.011(2) -0.005(2) C11 0.030(2) 0.0238(18) 0.034(2) -0.0087(16) -0.0038(17) -0.0076(16) C12 0.031(2) 0.0231(18) 0.034(2) -0.0075(16) -0.0056(17) -0.0057(16) C13 0.033(2) 0.028(2) 0.030(2) -0.0090(17) -0.0020(17) -0.0059(17) C14 0.030(2) 0.030(2) 0.036(2) -0.0108(18) -0.0073(18) -0.0080(17) C15 0.026(2) 0.0269(19) 0.036(2) -0.0107(17) -0.0033(17) -0.0054(16) C21 0.034(2) 0.028(2) 0.029(2) -0.0047(16) -0.0061(17) -0.0116(18) C22 0.036(2) 0.032(2) 0.035(2) -0.0111(18) -0.0020(19) -0.0091(19) C23 0.043(3) 0.037(2) 0.038(3) -0.010(2) 0.000(2) -0.003(2) C24 0.034(2) 0.036(2) 0.034(2) -0.0158(19) -0.0019(18) -0.0072(19) C25 0.027(2) 0.031(2) 0.038(2) -0.0135(18) -0.0055(18) -0.0028(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P2 2.3127(10) . ? Au1 P1 2.3158(10) . ? P1 C41 1.815(4) . ? P1 C51 1.817(4) . ? P1 C31 1.825(4) . ? P2 C81 1.809(4) . ? P2 C71 1.813(4) . ? P2 C61 1.815(4) . ? C31 C36 1.387(6) . ? C31 C32 1.392(6) . ? C32 C33 1.378(7) . ? C32 H32 0.9500 . ? C33 C34 1.393(7) . ? C33 H33 0.9500 . ? C34 C35 1.378(7) . ? C34 H34 0.9500 . ? C35 C36 1.375(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C41 C46 1.393(6) . ? C41 C42 1.394(6) . ? C42 C43 1.384(6) . ? C42 H42 0.9500 . ? C43 C44 1.382(7) . ? C43 H43 0.9500 . ? C44 C45 1.373(7) . ? C44 H44 0.9500 . ? C45 C46 1.390(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C51 C56 1.381(6) . ? C51 C52 1.394(6) . ? C52 C53 1.388(6) . ? C52 H52 0.9500 . ? C53 C54 1.381(7) . ? C53 H53 0.9500 . ? C54 C55 1.379(7) . ? C54 H54 0.9500 . ? C55 C56 1.398(6) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C61 C66 1.384(6) . ? C61 C62 1.394(6) . ? C62 C63 1.395(6) . ? C62 H62 0.9500 . ? C63 C64 1.379(7) . ? C63 H63 0.9500 . ? C64 C65 1.373(7) . ? C64 H64 0.9500 . ? C65 C66 1.390(6) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C71 C76 1.368(6) . ? C71 C72 1.401(6) . ? C72 C73 1.382(7) . ? C72 H72 0.9500 . ? C73 C74 1.370(8) . ? C73 H73 0.9500 . ? C74 C75 1.379(8) . ? C74 H74 0.9500 . ? C75 C76 1.384(6) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C81 C86 1.397(6) . ? C81 C82 1.401(6) . ? C82 C83 1.374(7) . ? C82 H82 0.9500 . ? C83 C84 1.391(7) . ? C83 H83 0.9500 . ? C84 C85 1.371(7) . ? C84 H84 0.9500 . ? C85 C86 1.379(6) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? N1 C21 1.140(6) . ? N2 C22 1.142(6) . ? N3 C23 1.140(7) . ? N4 C24 1.146(6) . ? N5 C25 1.141(6) . ? C11 C12 1.400(6) . ? C11 C21 1.410(6) . ? C11 C15 1.424(6) . ? C12 C13 1.402(6) . ? C12 C22 1.433(6) . ? C13 C14 1.407(6) . ? C13 C23 1.422(7) . ? C14 C15 1.406(6) . ? C14 C24 1.421(6) . ? C15 C25 1.421(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Au1 P1 172.03(3) . . ? C41 P1 C51 106.93(19) . . ? C41 P1 C31 107.05(19) . . ? C51 P1 C31 104.37(19) . . ? C41 P1 Au1 113.28(13) . . ? C51 P1 Au1 111.86(14) . . ? C31 P1 Au1 112.77(13) . . ? C81 P2 C71 105.28(18) . . ? C81 P2 C61 106.13(19) . . ? C71 P2 C61 105.59(19) . . ? C81 P2 Au1 112.51(13) . . ? C71 P2 Au1 110.64(14) . . ? C61 P2 Au1 115.91(14) . . ? C36 C31 C32 118.8(4) . . ? C36 C31 P1 123.7(3) . . ? C32 C31 P1 117.5(3) . . ? C33 C32 C31 121.1(4) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C33 C34 119.5(4) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C35 C34 C33 119.3(5) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? C36 C35 C34 121.2(4) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 119.4 . . ? C35 C36 C31 120.1(4) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C46 C41 C42 119.4(4) . . ? C46 C41 P1 123.0(3) . . ? C42 C41 P1 117.6(3) . . ? C43 C42 C41 120.1(4) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C44 C43 C42 120.1(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 120.3(4) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 120.3(5) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? C45 C46 C41 119.9(4) . . ? C45 C46 H46 120.1 . . ? C41 C46 H46 120.1 . . ? C56 C51 C52 119.4(4) . . ? C56 C51 P1 119.9(3) . . ? C52 C51 P1 120.7(3) . . ? C53 C52 C51 120.4(4) . . ? C53 C52 H52 119.8 . . ? C51 C52 H52 119.8 . . ? C54 C53 C52 120.0(4) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 119.9(4) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 120.3(4) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C51 C56 C55 120.0(4) . . ? C51 C56 H56 120.0 . . ? C55 C56 H56 120.0 . . ? C66 C61 C62 119.3(4) . . ? C66 C61 P2 118.1(3) . . ? C62 C61 P2 122.6(3) . . ? C61 C62 C63 119.7(4) . . ? C61 C62 H62 120.2 . . ? C63 C62 H62 120.2 . . ? C64 C63 C62 120.5(4) . . ? C64 C63 H63 119.8 . . ? C62 C63 H63 119.8 . . ? C65 C64 C63 119.8(4) . . ? C65 C64 H64 120.1 . . ? C63 C64 H64 120.1 . . ? C64 C65 C66 120.5(4) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C61 C66 C65 120.2(4) . . ? C61 C66 H66 119.9 . . ? C65 C66 H66 119.9 . . ? C76 C71 C72 119.0(4) . . ? C76 C71 P2 121.7(3) . . ? C72 C71 P2 119.1(3) . . ? C73 C72 C71 119.3(5) . . ? C73 C72 H72 120.3 . . ? C71 C72 H72 120.3 . . ? C74 C73 C72 121.0(5) . . ? C74 C73 H73 119.5 . . ? C72 C73 H73 119.5 . . ? C73 C74 C75 119.7(5) . . ? C73 C74 H74 120.1 . . ? C75 C74 H74 120.1 . . ? C74 C75 C76 119.6(5) . . ? C74 C75 H75 120.2 . . ? C76 C75 H75 120.2 . . ? C71 C76 C75 121.3(5) . . ? C71 C76 H76 119.3 . . ? C75 C76 H76 119.3 . . ? C86 C81 C82 118.7(4) . . ? C86 C81 P2 122.5(3) . . ? C82 C81 P2 118.9(3) . . ? C83 C82 C81 120.6(4) . . ? C83 C82 H82 119.7 . . ? C81 C82 H82 119.7 . . ? C82 C83 C84 119.5(4) . . ? C82 C83 H83 120.2 . . ? C84 C83 H83 120.2 . . ? C85 C84 C83 120.7(4) . . ? C85 C84 H84 119.7 . . ? C83 C84 H84 119.7 . . ? C84 C85 C86 120.1(5) . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C85 C86 C81 120.4(4) . . ? C85 C86 H86 119.8 . . ? C81 C86 H86 119.8 . . ? C12 C11 C21 124.6(4) . . ? C12 C11 C15 107.7(4) . . ? C21 C11 C15 127.6(4) . . ? C11 C12 C13 108.8(4) . . ? C11 C12 C22 123.5(4) . . ? C13 C12 C22 127.7(4) . . ? C12 C13 C14 107.7(4) . . ? C12 C13 C23 126.0(4) . . ? C14 C13 C23 126.1(4) . . ? C15 C14 C13 108.5(4) . . ? C15 C14 C24 124.7(4) . . ? C13 C14 C24 126.8(4) . . ? C14 C15 C25 126.3(4) . . ? C14 C15 C11 107.3(4) . . ? C25 C15 C11 126.3(4) . . ? N1 C21 C11 178.2(5) . . ? N2 C22 C12 177.2(5) . . ? N3 C23 C13 176.9(6) . . ? N4 C24 C14 178.9(6) . . ? N5 C25 C15 179.0(5) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 32.03 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.262 _refine_diff_density_min -1.306 _refine_diff_density_rms 0.150