Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Maravanji Balakrishna' _publ_contact_author_address ; Department of Chemistry Indian Institute of Technology Bombay Powai Mumbai 400076 INDIA ; _publ_contact_author_email KRISHNA@CHEM.IITB.AC.IN _publ_section_title ; Water-soluble Cyclodiphosphazanes: Synthesis, Gold(I) Metal Complexes and their In Vitro Antitumor Studies ; loop_ _publ_author_name 'Maravanji Balakrishna' 'Shaikh M Mobin' 'Dulal Panda' 'Krishnan Rathinasamy' 'D. Suresh' data_msb026 _database_code_depnum_ccdc_archive 'CCDC 675638' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H41 I N4 P2' _chemical_formula_weight 490.38 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.090(3) _cell_length_b 25.9449(18) _cell_length_c 27.452(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10036(3) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16145 _cell_measurement_theta_min 2.9777 _cell_measurement_theta_max 32.2703 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4064 _exptl_absorpt_coefficient_mu 1.411 _exptl_absorpt_correction_T_min 0.6532 _exptl_absorpt_correction_T_max 0.8835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61951 _diffrn_reflns_av_R_equivalents 0.0596 _diffrn_reflns_av_sigmaI/netI 0.0621 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8818 _reflns_number_gt 5439 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0309P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8818 _refine_ls_number_parameters 506 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0576 _refine_ls_goodness_of_fit_ref 0.831 _refine_ls_restrained_S_all 0.831 _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 I2 I 0.166125(15) 0.002970(10) 0.358271(8) 0.03845(7) Uani 1 1 d . . . I1 I 0.278375(14) -0.176094(9) 0.151982(8) 0.03390(7) Uani 1 1 d . . . P1 P 0.27882(6) -0.18387(3) 0.32237(3) 0.02228(19) Uani 1 1 d . . . P2 P 0.28032(6) -0.18709(3) 0.41517(3) 0.0249(2) Uani 1 1 d . . . P3 P -0.15468(6) 0.01379(3) 0.38724(3) 0.0237(2) Uani 1 1 d . . . P4 P -0.33404(6) 0.01287(3) 0.39705(3) 0.0273(2) Uani 1 1 d . . . N1 N 0.20027(16) -0.19128(10) 0.36589(9) 0.0233(6) Uani 1 1 d . . . N2 N 0.35962(15) -0.18926(10) 0.36552(9) 0.0235(6) Uani 1 1 d . . . N3 N 0.28075(18) -0.22345(11) 0.27737(10) 0.0257(7) Uani 1 1 d . . . N4 N 0.2841(2) -0.24485(12) 0.43961(11) 0.0302(8) Uani 1 1 d . A . N5 N -0.23065(17) 0.02382(10) 0.43179(9) 0.0256(6) Uani 1 1 d . . . N6 N -0.24780(16) 0.01466(9) 0.35136(9) 0.0215(6) Uani 1 1 d . . . N7 N -0.06924(19) 0.05379(11) 0.37973(10) 0.0274(7) Uani 1 1 d . . . N8 N -0.3880(2) 0.06895(12) 0.39350(12) 0.0371(8) Uani 1 1 d . . . C1 C 0.0942(2) -0.18740(13) 0.36707(12) 0.0294(9) Uani 1 1 d . . . C2 C 0.0533(2) -0.24066(13) 0.37423(13) 0.0419(10) Uani 1 1 d . . . H2A H 0.0722 -0.2624 0.3476 0.063 Uiso 1 1 calc R . . H2B H -0.0147 -0.2386 0.3754 0.063 Uiso 1 1 calc R . . H2C H 0.0765 -0.2549 0.4043 0.063 Uiso 1 1 calc R . . C3 C 0.0659(2) -0.15258(13) 0.40909(13) 0.0393(9) Uani 1 1 d . . . H3A H 0.0867 -0.1676 0.4392 0.059 Uiso 1 1 calc R . . H3B H -0.0018 -0.1487 0.4096 0.059 Uiso 1 1 calc R . . H3C H 0.0951 -0.1194 0.4050 0.059 Uiso 1 1 calc R . . C4 C 0.0597(2) -0.16462(15) 0.31913(13) 0.0488(11) Uani 1 1 d . . . H4A H 0.0830 -0.1300 0.3159 0.073 Uiso 1 1 calc R . . H4B H -0.0085 -0.1643 0.3187 0.073 Uiso 1 1 calc R . . H4C H 0.0827 -0.1852 0.2926 0.073 Uiso 1 1 calc R . . C5 C 0.4624(2) -0.17545(13) 0.36593(11) 0.0289(8) Uani 1 1 d . . . C6 C 0.4735(3) -0.11845(17) 0.3770(2) 0.0887(17) Uani 1 1 d . . . H6A H 0.4393 -0.0986 0.3533 0.133 Uiso 1 1 calc R . . H6B H 0.5396 -0.1093 0.3759 0.133 Uiso 1 1 calc R . . H6C H 0.4489 -0.1113 0.4089 0.133 Uiso 1 1 calc R . . C7 C 0.5109(3) -0.2064(2) 0.40396(18) 0.0913(18) Uani 1 1 d . . . H7A H 0.4826 -0.1994 0.4351 0.137 Uiso 1 1 calc R . . H7B H 0.5770 -0.1973 0.4049 0.137 Uiso 1 1 calc R . . H7C H 0.5046 -0.2424 0.3965 0.137 Uiso 1 1 calc R . . C8 C 0.5038(2) -0.1861(2) 0.31631(14) 0.0885(18) Uani 1 1 d . . . H8A H 0.5001 -0.2224 0.3096 0.133 Uiso 1 1 calc R . . H8B H 0.5689 -0.1753 0.3157 0.133 Uiso 1 1 calc R . . H8C H 0.4686 -0.1675 0.2921 0.133 Uiso 1 1 calc R . . C9 C 0.2778(2) -0.12297(12) 0.29285(11) 0.0328(8) Uani 1 1 d . . . H9A H 0.3379 -0.1173 0.2773 0.049 Uiso 1 1 calc R . . H9B H 0.2668 -0.0963 0.3165 0.049 Uiso 1 1 calc R . . H9C H 0.2283 -0.1224 0.2689 0.049 Uiso 1 1 calc R . . C10 C 0.2803(2) -0.28061(12) 0.27290(11) 0.0290(8) Uani 1 1 d . . . C11 C 0.2875(2) -0.30605(12) 0.32215(11) 0.0329(8) Uani 1 1 d . . . H11A H 0.3452 -0.2955 0.3378 0.049 Uiso 1 1 calc R . . H11B H 0.2877 -0.3428 0.3182 0.049 Uiso 1 1 calc R . . H11C H 0.2342 -0.2961 0.3418 0.049 Uiso 1 1 calc R . . C12 C 0.3643(2) -0.29560(13) 0.24106(13) 0.0416(10) Uani 1 1 d . . . H12A H 0.3585 -0.2792 0.2099 0.062 Uiso 1 1 calc R . . H12B H 0.3651 -0.3323 0.2368 0.062 Uiso 1 1 calc R . . H12C H 0.4221 -0.2848 0.2564 0.062 Uiso 1 1 calc R . . C13 C 0.1875(2) -0.29584(13) 0.24797(13) 0.0420(10) Uani 1 1 d . . . H13A H 0.1349 -0.2862 0.2682 0.063 Uiso 1 1 calc R . . H13B H 0.1866 -0.3324 0.2428 0.063 Uiso 1 1 calc R . . H13C H 0.1828 -0.2785 0.2172 0.063 Uiso 1 1 calc R . . C14 C 0.2811(2) -0.25967(13) 0.49143(12) 0.0320(8) Uani 1 1 d U . . C15 C 0.2204(11) -0.3070(5) 0.4967(4) 0.110(7) Uani 0.609(16) 1 d PU A 2 H15A H 0.2575 -0.3371 0.4894 0.165 Uiso 0.609(16) 1 calc PR A 2 H15B H 0.1677 -0.3050 0.4746 0.165 Uiso 0.609(16) 1 calc PR A 2 H15C H 0.1972 -0.3092 0.5296 0.165 Uiso 0.609(16) 1 calc PR A 2 C16 C 0.3812(6) -0.2743(6) 0.5077(3) 0.081(5) Uani 0.609(16) 1 d PU A 2 H16A H 0.3793 -0.2869 0.5406 0.122 Uiso 0.609(16) 1 calc PR A 2 H16B H 0.4216 -0.2446 0.5062 0.122 Uiso 0.609(16) 1 calc PR A 2 H16C H 0.4057 -0.3007 0.4867 0.122 Uiso 0.609(16) 1 calc PR A 2 C17 C 0.2454(11) -0.2179(4) 0.5218(3) 0.086(6) Uani 0.609(16) 1 d PU A 2 H17A H 0.1849 -0.2067 0.5098 0.128 Uiso 0.609(16) 1 calc PR A 2 H17B H 0.2893 -0.1896 0.5210 0.128 Uiso 0.609(16) 1 calc PR A 2 H17C H 0.2386 -0.2298 0.5548 0.128 Uiso 0.609(16) 1 calc PR A 2 C15` C 0.1823(11) -0.2456(10) 0.5105(6) 0.095(8) Uani 0.391(16) 1 d PU A 1 H15D H 0.1354 -0.2661 0.4941 0.142 Uiso 0.391(16) 1 calc PR A 1 H15E H 0.1702 -0.2098 0.5045 0.142 Uiso 0.391(16) 1 calc PR A 1 H15F H 0.1794 -0.2522 0.5449 0.142 Uiso 0.391(16) 1 calc PR A 1 C16` C 0.3529(16) -0.2274(10) 0.5185(5) 0.116(12) Uani 0.391(16) 1 d PU A 1 H16D H 0.3566 -0.2388 0.5517 0.174 Uiso 0.391(16) 1 calc PR A 1 H16E H 0.3338 -0.1919 0.5176 0.174 Uiso 0.391(16) 1 calc PR A 1 H16F H 0.4139 -0.2310 0.5033 0.174 Uiso 0.391(16) 1 calc PR A 1 C17` C 0.299(2) -0.3129(6) 0.4956(7) 0.132(14) Uani 0.391(16) 1 d PU A 1 H17D H 0.2858 -0.3239 0.5283 0.199 Uiso 0.391(16) 1 calc PR A 1 H17E H 0.3641 -0.3198 0.4879 0.199 Uiso 0.391(16) 1 calc PR A 1 H17F H 0.2586 -0.3314 0.4734 0.199 Uiso 0.391(16) 1 calc PR A 1 C18 C -0.2214(2) 0.01533(13) 0.48508(11) 0.0320(8) Uani 1 1 d . . . C19 C -0.2292(3) -0.04126(14) 0.49794(13) 0.0480(10) Uani 1 1 d . . . H19A H -0.2887 -0.0545 0.4864 0.072 Uiso 1 1 calc R . . H19B H -0.2258 -0.0453 0.5327 0.072 Uiso 1 1 calc R . . H19C H -0.1780 -0.0599 0.4830 0.072 Uiso 1 1 calc R . . C20 C -0.2997(2) 0.04557(15) 0.51051(12) 0.0476(11) Uani 1 1 d . . . H20A H -0.2952 0.0813 0.5016 0.071 Uiso 1 1 calc R . . H20B H -0.2928 0.0422 0.5452 0.071 Uiso 1 1 calc R . . H20C H -0.3604 0.0323 0.5008 0.071 Uiso 1 1 calc R . . C21 C -0.1261(2) 0.03711(16) 0.50158(12) 0.0507(11) Uani 1 1 d . . . H21A H -0.0758 0.0205 0.4839 0.076 Uiso 1 1 calc R . . H21B H -0.1180 0.0310 0.5358 0.076 Uiso 1 1 calc R . . H21C H -0.1244 0.0735 0.4954 0.076 Uiso 1 1 calc R . . C22 C -0.2608(2) 0.00758(12) 0.29784(11) 0.0276(8) Uani 1 1 d . . . C23 C -0.1703(2) -0.01344(14) 0.27522(12) 0.0414(10) Uani 1 1 d . . . H23A H -0.1188 0.0098 0.2817 0.062 Uiso 1 1 calc R . . H23B H -0.1787 -0.0168 0.2407 0.062 Uiso 1 1 calc R . . H23C H -0.1563 -0.0466 0.2890 0.062 Uiso 1 1 calc R . . C24 C -0.2861(3) 0.05973(13) 0.27547(12) 0.0450(10) Uani 1 1 d . . . H24A H -0.3421 0.0730 0.2909 0.067 Uiso 1 1 calc R . . H24B H -0.2976 0.0556 0.2412 0.067 Uiso 1 1 calc R . . H24C H -0.2345 0.0833 0.2802 0.067 Uiso 1 1 calc R . . C25 C -0.3423(2) -0.03042(13) 0.28991(12) 0.0348(9) Uani 1 1 d . . . H25A H -0.3271 -0.0627 0.3051 0.052 Uiso 1 1 calc R . . H25B H -0.3517 -0.0356 0.2556 0.052 Uiso 1 1 calc R . . H25C H -0.3993 -0.0168 0.3041 0.052 Uiso 1 1 calc R . . C26 C -0.0953(2) -0.04657(12) 0.39000(12) 0.0322(9) Uani 1 1 d . . . H26A H -0.0557 -0.0505 0.3618 0.048 Uiso 1 1 calc R . . H26B H -0.1413 -0.0739 0.3908 0.048 Uiso 1 1 calc R . . H26C H -0.0569 -0.0479 0.4189 0.048 Uiso 1 1 calc R . . C27 C -0.0619(2) 0.11071(12) 0.37439(12) 0.0313(8) Uani 1 1 d . . . C28 C 0.0097(2) 0.12916(14) 0.41229(13) 0.0476(10) Uani 1 1 d . . . H28A H -0.0152 0.1233 0.4444 0.071 Uiso 1 1 calc R . . H28B H 0.0213 0.1653 0.4079 0.071 Uiso 1 1 calc R . . H28C H 0.0680 0.1105 0.4085 0.071 Uiso 1 1 calc R . . C29 C -0.0248(2) 0.12215(13) 0.32338(12) 0.0396(9) Uani 1 1 d . . . H29A H 0.0360 0.1061 0.3191 0.059 Uiso 1 1 calc R . . H29B H -0.0187 0.1587 0.3192 0.059 Uiso 1 1 calc R . . H29C H -0.0684 0.1088 0.2997 0.059 Uiso 1 1 calc R . . C30 C -0.1582(2) 0.13578(12) 0.38246(12) 0.0371(9) Uani 1 1 d . . . H30A H -0.2031 0.1220 0.3596 0.056 Uiso 1 1 calc R . . H30B H -0.1529 0.1724 0.3779 0.056 Uiso 1 1 calc R . . H30C H -0.1795 0.1288 0.4150 0.056 Uiso 1 1 calc R . . C31 C -0.4923(2) 0.07966(15) 0.39571(16) 0.0482(11) Uani 1 1 d . . . C32 C -0.5221(3) 0.1039(2) 0.3481(2) 0.110(2) Uani 1 1 d . . . H32A H -0.5887 0.1116 0.3491 0.166 Uiso 1 1 calc R . . H32B H -0.5098 0.0803 0.3219 0.166 Uiso 1 1 calc R . . H32C H -0.4869 0.1351 0.3430 0.166 Uiso 1 1 calc R . . C33 C -0.5453(3) 0.03042(18) 0.4017(2) 0.0903(17) Uani 1 1 d . . . H33A H -0.5301 0.0155 0.4327 0.135 Uiso 1 1 calc R . . H33B H -0.5277 0.0070 0.3762 0.135 Uiso 1 1 calc R . . H33C H -0.6122 0.0371 0.4001 0.135 Uiso 1 1 calc R . . C34 C -0.5122(3) 0.1142(2) 0.4370(2) 0.131(3) Uani 1 1 d . . . H34A H -0.5778 0.1242 0.4364 0.197 Uiso 1 1 calc R . . H34B H -0.4731 0.1444 0.4346 0.197 Uiso 1 1 calc R . . H34C H -0.4987 0.0967 0.4670 0.197 Uiso 1 1 calc R . . H4N H 0.287(2) -0.2656(11) 0.4237(10) 0.005(10) Uiso 1 1 d . . . H3N H 0.277(2) -0.2094(12) 0.2492(12) 0.040(11) Uiso 1 1 d . . . H7N H -0.0186(18) 0.0397(11) 0.3745(9) 0.011(8) Uiso 1 1 d . . . H8N H -0.360(2) 0.0963(13) 0.3920(12) 0.036(12) Uiso 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 I2 0.03308(12) 0.05682(17) 0.02543(12) 0.00193(12) 0.00471(10) 0.00463(12) I1 0.02441(11) 0.04819(15) 0.02909(13) 0.00284(12) 0.00050(10) -0.00257(11) P1 0.0204(4) 0.0247(5) 0.0216(5) 0.0019(4) 0.0009(4) 0.0014(4) P2 0.0244(4) 0.0288(5) 0.0214(5) -0.0006(4) 0.0007(4) -0.0007(4) P3 0.0266(5) 0.0233(5) 0.0212(5) -0.0009(4) 0.0008(4) 0.0001(4) P4 0.0235(4) 0.0303(6) 0.0282(5) 0.0010(4) 0.0010(4) -0.0012(4) N1 0.0224(15) 0.0273(16) 0.0203(15) 0.0006(12) 0.0008(11) 0.0033(11) N2 0.0185(14) 0.0315(17) 0.0205(16) 0.0004(13) 0.0014(11) -0.0020(11) N3 0.0271(15) 0.0285(18) 0.0215(17) 0.0029(14) -0.0013(13) 0.0027(14) N4 0.0423(18) 0.027(2) 0.0207(18) -0.0024(16) 0.0017(14) 0.0017(16) N5 0.0281(15) 0.0271(16) 0.0216(16) 0.0009(12) 0.0031(12) -0.0030(13) N6 0.0236(14) 0.0231(15) 0.0176(14) -0.0028(12) 0.0002(10) -0.0046(11) N7 0.0224(16) 0.0286(19) 0.0311(18) -0.0017(14) 0.0025(13) 0.0021(14) N8 0.0277(17) 0.028(2) 0.056(2) -0.0001(17) 0.0067(15) 0.0017(15) C1 0.0161(17) 0.035(2) 0.037(2) 0.0021(18) 0.0033(15) 0.0035(15) C2 0.0235(18) 0.043(2) 0.060(3) -0.001(2) 0.0020(17) -0.0022(17) C3 0.032(2) 0.040(2) 0.047(2) 0.004(2) 0.0136(17) 0.0105(17) C4 0.0240(19) 0.081(3) 0.041(2) 0.014(2) -0.0020(16) 0.011(2) C5 0.0179(16) 0.043(2) 0.025(2) 0.0046(18) 0.0008(13) -0.0086(16) C6 0.056(3) 0.073(4) 0.137(5) -0.033(3) 0.008(3) -0.035(3) C7 0.027(2) 0.138(5) 0.108(4) 0.073(4) -0.014(2) -0.008(3) C8 0.025(2) 0.193(6) 0.048(3) -0.014(3) 0.006(2) -0.021(3) C9 0.036(2) 0.031(2) 0.032(2) 0.0047(16) 0.0017(17) 0.0001(17) C10 0.0313(19) 0.0222(19) 0.034(2) -0.0067(16) -0.0025(17) 0.0020(17) C11 0.048(2) 0.0209(19) 0.030(2) -0.0021(16) 0.0004(17) 0.0051(17) C12 0.048(2) 0.038(2) 0.039(2) -0.0040(19) 0.0065(18) 0.0108(18) C13 0.044(2) 0.033(2) 0.049(3) -0.0100(19) -0.0097(18) 0.0000(17) C14 0.0398(19) 0.035(2) 0.021(2) 0.0017(16) -0.0006(16) 0.0047(19) C15 0.198(15) 0.096(12) 0.035(6) 0.015(6) -0.003(8) -0.089(12) C16 0.069(5) 0.132(13) 0.043(6) 0.039(7) 0.001(4) 0.033(7) C17 0.165(16) 0.071(7) 0.021(5) 0.005(4) 0.017(6) 0.048(8) C15` 0.070(9) 0.18(2) 0.038(9) 0.030(11) 0.026(7) 0.033(12) C16` 0.14(2) 0.17(2) 0.033(9) 0.050(12) -0.053(11) -0.094(19) C17` 0.31(4) 0.033(9) 0.057(11) 0.041(9) 0.099(19) 0.070(18) C18 0.041(2) 0.033(2) 0.0215(19) 0.0000(16) 0.0018(16) -0.0037(18) C19 0.074(3) 0.042(3) 0.027(2) 0.0083(19) 0.005(2) -0.002(2) C20 0.068(3) 0.051(3) 0.025(2) -0.0023(19) 0.0147(18) -0.002(2) C21 0.054(3) 0.075(3) 0.023(2) 0.011(2) -0.0080(18) -0.016(2) C22 0.041(2) 0.024(2) 0.0181(18) -0.0076(16) -0.0033(14) -0.0038(16) C23 0.045(2) 0.050(3) 0.029(2) -0.0118(18) 0.0018(17) -0.0089(19) C24 0.073(3) 0.034(2) 0.029(2) 0.0014(18) -0.0121(19) -0.006(2) C25 0.038(2) 0.037(2) 0.029(2) -0.0058(18) -0.0065(16) -0.0028(18) C26 0.031(2) 0.029(2) 0.036(2) -0.0006(18) -0.0020(16) 0.0050(16) C27 0.034(2) 0.024(2) 0.035(2) 0.0025(17) -0.0033(16) -0.0062(16) C28 0.057(3) 0.039(3) 0.048(3) -0.002(2) -0.009(2) -0.0163(19) C29 0.033(2) 0.041(2) 0.044(2) 0.0081(19) 0.0029(17) -0.0058(17) C30 0.046(2) 0.019(2) 0.046(2) -0.0033(17) 0.0016(18) -0.0037(17) C31 0.029(2) 0.050(3) 0.066(3) 0.006(2) 0.011(2) 0.0119(19) C32 0.046(3) 0.147(5) 0.139(5) 0.078(4) 0.010(3) 0.037(3) C33 0.029(2) 0.078(4) 0.164(6) 0.018(4) 0.009(3) -0.006(2) C34 0.062(3) 0.155(6) 0.177(7) -0.097(5) 0.015(4) 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 N3 1.607(3) . ? P1 N1 1.640(2) . ? P1 N2 1.649(2) . ? P1 C9 1.776(3) . ? P1 P2 2.5488(11) . ? P2 N4 1.643(3) . ? P2 N2 1.763(2) . ? P2 N1 1.765(2) . ? P3 N7 1.603(3) . ? P3 N6 1.641(2) . ? P3 N5 1.646(2) . ? P3 C26 1.777(3) . ? P3 P4 2.5416(13) . ? P4 N8 1.645(3) . ? P4 N6 1.747(2) . ? P4 N5 1.764(3) . ? N1 C1 1.499(3) . ? N2 C5 1.492(3) . ? N3 C10 1.488(4) . ? N3 H3N 0.86(3) . ? N4 C14 1.474(4) . ? N4 H4N 0.69(3) . ? N5 C18 1.485(4) . ? N6 C22 1.492(4) . ? N7 C27 1.488(4) . ? N7 H7N 0.81(2) . ? N8 C31 1.497(4) . ? N8 H8N 0.81(3) . ? C1 C2 1.510(4) . ? C1 C3 1.518(4) . ? C1 C4 1.522(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C7 1.484(5) . ? C5 C8 1.507(5) . ? C5 C6 1.518(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.508(4) . ? C10 C12 1.522(4) . ? C10 C13 1.527(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C17` 1.409(15) . ? C14 C17 1.458(8) . ? C14 C15 1.504(10) . ? C14 C16` 1.508(13) . ? C14 C16 1.528(8) . ? C14 C15` 1.531(13) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C15` H15D 0.9600 . ? C15` H15E 0.9600 . ? C15` H15F 0.9600 . ? C16` H16D 0.9600 . ? C16` H16E 0.9600 . ? C16` H16F 0.9600 . ? C17` H17D 0.9600 . ? C17` H17E 0.9600 . ? C17` H17F 0.9600 . ? C18 C19 1.514(5) . ? C18 C20 1.524(4) . ? C18 C21 1.525(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.519(4) . ? C22 C24 1.528(4) . ? C22 C25 1.529(4) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C30 1.521(4) . ? C27 C29 1.524(4) . ? C27 C28 1.526(4) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C34 1.473(6) . ? C31 C33 1.489(5) . ? C31 C32 1.511(6) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? 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 N3 P1 N1 119.78(14) . . ? N3 P1 N2 119.11(14) . . ? N1 P1 N2 86.15(12) . . ? N3 P1 C9 102.58(15) . . ? N1 P1 C9 115.56(14) . . ? N2 P1 C9 114.13(14) . . ? N3 P1 P2 138.37(11) . . ? N1 P1 P2 43.42(9) . . ? N2 P1 P2 43.41(8) . . ? C9 P1 P2 119.03(11) . . ? N4 P2 N2 105.42(14) . . ? N4 P2 N1 106.12(14) . . ? N2 P2 N1 79.08(11) . . ? N4 P2 P1 116.00(12) . . ? N2 P2 P1 39.99(8) . . ? N1 P2 P1 39.70(8) . . ? N7 P3 N6 120.97(14) . . ? N7 P3 N5 118.79(14) . . ? N6 P3 N5 85.63(12) . . ? N7 P3 C26 102.87(15) . . ? N6 P3 C26 114.46(14) . . ? N5 P3 C26 114.44(14) . . ? N7 P3 P4 140.05(12) . . ? N6 P3 P4 43.00(9) . . ? N5 P3 P4 43.63(9) . . ? C26 P3 P4 117.07(11) . . ? N8 P4 N6 104.79(14) . . ? N8 P4 N5 105.72(15) . . ? N6 P4 N5 79.02(11) . . ? N8 P4 P3 116.41(12) . . ? N6 P4 P3 39.83(8) . . ? N5 P4 P3 40.07(8) . . ? C1 N1 P1 132.9(2) . . ? C1 N1 P2 128.08(19) . . ? P1 N1 P2 96.88(12) . . ? C5 N2 P1 130.94(19) . . ? C5 N2 P2 126.99(19) . . ? P1 N2 P2 96.60(12) . . ? C10 N3 P1 134.4(2) . . ? C10 N3 H3N 110(2) . . ? P1 N3 H3N 115(2) . . ? C14 N4 P2 129.1(3) . . ? C14 N4 H4N 114(3) . . ? P2 N4 H4N 117(3) . . ? C18 N5 P3 130.6(2) . . ? C18 N5 P4 125.6(2) . . ? P3 N5 P4 96.30(13) . . ? C22 N6 P3 133.4(2) . . ? C22 N6 P4 128.21(19) . . ? P3 N6 P4 97.17(13) . . ? C27 N7 P3 135.0(2) . . ? C27 N7 H7N 111(2) . . ? P3 N7 H7N 113(2) . . ? C31 N8 P4 128.0(3) . . ? C31 N8 H8N 108(2) . . ? P4 N8 H8N 124(2) . . ? N1 C1 C2 108.8(2) . . ? N1 C1 C3 108.5(2) . . ? C2 C1 C3 110.2(3) . . ? N1 C1 C4 109.0(2) . . ? C2 C1 C4 110.3(3) . . ? C3 C1 C4 110.0(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 N2 108.8(3) . . ? C7 C5 C8 111.0(3) . . ? N2 C5 C8 108.9(2) . . ? C7 C5 C6 109.7(4) . . ? N2 C5 C6 109.6(3) . . ? C8 C5 C6 108.7(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C9 H9A 109.5 . . ? P1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 C11 111.2(3) . . ? N3 C10 C12 107.4(3) . . ? C11 C10 C12 110.5(3) . . ? N3 C10 C13 107.4(3) . . ? C11 C10 C13 110.3(3) . . ? C12 C10 C13 110.0(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C17` C14 C17 138.1(7) . . ? C17` C14 N4 109.2(8) . . ? C17 C14 N4 111.6(4) . . ? C17` C14 C15 44.9(10) . . ? C17 C14 C15 110.8(6) . . ? N4 C14 C15 108.8(5) . . ? C17` C14 C16` 112.7(11) . . ? C17 C14 C16` 62.4(9) . . ? N4 C14 C16` 108.1(5) . . ? C15 C14 C16` 141.9(7) . . ? C17` C14 C16 64.4(10) . . ? C17 C14 C16 109.6(6) . . ? N4 C14 C16 108.7(4) . . ? C15 C14 C16 107.0(7) . . ? C16` C14 C16 51.3(8) . . ? C17` C14 C15` 111.5(10) . . ? C17 C14 C15` 46.6(7) . . ? N4 C14 C15` 107.1(6) . . ? C15 C14 C15` 69.2(8) . . ? C16` C14 C15` 108.0(10) . . ? C16 C14 C15` 142.9(7) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C15` H15D 109.5 . . ? C14 C15` H15E 109.5 . . ? C14 C15` H15F 109.5 . . ? C14 C16` H16D 109.5 . . ? C14 C16` H16E 109.5 . . ? C14 C16` H16F 109.5 . . ? C14 C17` H17D 109.5 . . ? C14 C17` H17E 109.5 . . ? C14 C17` H17F 109.5 . . ? N5 C18 C19 111.5(3) . . ? N5 C18 C20 108.1(3) . . ? C19 C18 C20 109.9(3) . . ? N5 C18 C21 108.4(3) . . ? C19 C18 C21 110.7(3) . . ? C20 C18 C21 108.1(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N6 C22 C23 110.1(2) . . ? N6 C22 C24 108.4(2) . . ? C23 C22 C24 110.4(3) . . ? N6 C22 C25 108.2(2) . . ? C23 C22 C25 109.9(3) . . ? C24 C22 C25 109.8(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? P3 C26 H26A 109.5 . . ? P3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? P3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N7 C27 C30 110.4(3) . . ? N7 C27 C29 107.9(3) . . ? C30 C27 C29 110.9(3) . . ? N7 C27 C28 106.9(3) . . ? C30 C27 C28 110.9(3) . . ? C29 C27 C28 109.8(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C34 C31 C33 110.0(4) . . ? C34 C31 N8 109.4(3) . . ? C33 C31 N8 109.7(3) . . ? C34 C31 C32 111.1(4) . . ? C33 C31 C32 108.2(4) . . ? N8 C31 C32 108.4(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 P1 P2 N4 -0.2(2) . . . . ? N1 P1 P2 N4 84.04(18) . . . . ? N2 P1 P2 N4 -83.05(18) . . . . ? C9 P1 P2 N4 -178.41(17) . . . . ? N3 P1 P2 N2 82.9(2) . . . . ? N1 P1 P2 N2 167.09(19) . . . . ? C9 P1 P2 N2 -95.37(18) . . . . ? N3 P1 P2 N1 -84.2(2) . . . . ? N2 P1 P2 N1 -167.09(19) . . . . ? C9 P1 P2 N1 97.55(18) . . . . ? N7 P3 P4 N8 2.6(2) . . . . ? N6 P3 P4 N8 -81.35(18) . . . . ? N5 P3 P4 N8 83.08(19) . . . . ? C26 P3 P4 N8 -179.03(18) . . . . ? N7 P3 P4 N6 84.0(2) . . . . ? N5 P3 P4 N6 164.43(19) . . . . ? C26 P3 P4 N6 -97.68(18) . . . . ? N7 P3 P4 N5 -80.5(2) . . . . ? N6 P3 P4 N5 -164.43(19) . . . . ? C26 P3 P4 N5 97.88(18) . . . . ? N3 P1 N1 C1 -65.7(3) . . . . ? N2 P1 N1 C1 172.8(3) . . . . ? C9 P1 N1 C1 57.8(3) . . . . ? P2 P1 N1 C1 163.9(3) . . . . ? N3 P1 N1 P2 130.41(15) . . . . ? N2 P1 N1 P2 8.86(13) . . . . ? C9 P1 N1 P2 -106.10(15) . . . . ? N4 P2 N1 C1 83.4(3) . . . . ? N2 P2 N1 C1 -173.5(3) . . . . ? P1 P2 N1 C1 -165.1(3) . . . . ? N4 P2 N1 P1 -111.48(15) . . . . ? N2 P2 N1 P1 -8.41(12) . . . . ? N3 P1 N2 C5 74.5(3) . . . . ? N1 P1 N2 C5 -163.3(3) . . . . ? C9 P1 N2 C5 -47.0(3) . . . . ? P2 P1 N2 C5 -154.5(3) . . . . ? N3 P1 N2 P2 -131.02(15) . . . . ? N1 P1 N2 P2 -8.86(13) . . . . ? C9 P1 N2 P2 107.48(15) . . . . ? N4 P2 N2 C5 -91.8(3) . . . . ? N1 P2 N2 C5 164.3(3) . . . . ? P1 P2 N2 C5 155.9(3) . . . . ? N4 P2 N2 P1 112.25(15) . . . . ? N1 P2 N2 P1 8.36(12) . . . . ? N1 P1 N3 C10 -48.9(4) . . . . ? N2 P1 N3 C10 54.4(3) . . . . ? C9 P1 N3 C10 -178.4(3) . . . . ? P2 P1 N3 C10 3.1(4) . . . . ? N2 P2 N4 C14 141.8(3) . . . . ? N1 P2 N4 C14 -135.3(3) . . . . ? P1 P2 N4 C14 -176.7(2) . . . . ? N7 P3 N5 C18 -76.3(3) . . . . ? N6 P3 N5 C18 160.5(3) . . . . ? C26 P3 N5 C18 45.6(3) . . . . ? P4 P3 N5 C18 149.9(3) . . . . ? N7 P3 N5 P4 133.73(14) . . . . ? N6 P3 N5 P4 10.58(13) . . . . ? C26 P3 N5 P4 -104.34(15) . . . . ? N8 P4 N5 C18 95.3(3) . . . . ? N6 P4 N5 C18 -162.2(3) . . . . ? P3 P4 N5 C18 -152.1(3) . . . . ? N8 P4 N5 P3 -112.53(15) . . . . ? N6 P4 N5 P3 -10.08(12) . . . . ? N7 P3 N6 C22 60.3(3) . . . . ? N5 P3 N6 C22 -178.6(3) . . . . ? C26 P3 N6 C22 -63.7(3) . . . . ? P4 P3 N6 C22 -167.9(3) . . . . ? N7 P3 N6 P4 -131.87(15) . . . . ? N5 P3 N6 P4 -10.70(13) . . . . ? C26 P3 N6 P4 104.20(15) . . . . ? N8 P4 N6 C22 -77.5(3) . . . . ? N5 P4 N6 C22 178.9(3) . . . . ? P3 P4 N6 C22 168.8(3) . . . . ? N8 P4 N6 P3 113.68(15) . . . . ? N5 P4 N6 P3 10.14(12) . . . . ? N6 P3 N7 C27 51.0(4) . . . . ? N5 P3 N7 C27 -52.2(4) . . . . ? C26 P3 N7 C27 -179.8(3) . . . . ? P4 P3 N7 C27 -1.3(4) . . . . ? N6 P4 N8 C31 136.2(3) . . . . ? N5 P4 N8 C31 -141.3(3) . . . . ? P3 P4 N8 C31 177.1(3) . . . . ? P1 N1 C1 C2 110.3(3) . . . . ? P2 N1 C1 C2 -90.1(3) . . . . ? P1 N1 C1 C3 -129.8(3) . . . . ? P2 N1 C1 C3 29.8(4) . . . . ? P1 N1 C1 C4 -10.0(4) . . . . ? P2 N1 C1 C4 149.6(3) . . . . ? P1 N2 C5 C7 -157.0(3) . . . . ? P2 N2 C5 C7 55.4(4) . . . . ? P1 N2 C5 C8 -35.8(4) . . . . ? P2 N2 C5 C8 176.6(3) . . . . ? P1 N2 C5 C6 83.0(4) . . . . ? P2 N2 C5 C6 -64.6(4) . . . . ? P1 N3 C10 C11 -5.9(4) . . . . ? P1 N3 C10 C12 -126.9(3) . . . . ? P1 N3 C10 C13 114.9(3) . . . . ? P2 N4 C14 C17` -172.4(14) . . . . ? P2 N4 C14 C17 17.4(8) . . . . ? P2 N4 C14 C15 140.0(8) . . . . ? P2 N4 C14 C16` -49.4(14) . . . . ? P2 N4 C14 C16 -103.7(7) . . . . ? P2 N4 C14 C15` 66.8(12) . . . . ? P3 N5 C18 C19 -75.9(4) . . . . ? P4 N5 C18 C19 66.3(4) . . . . ? P3 N5 C18 C20 163.2(2) . . . . ? P4 N5 C18 C20 -54.6(3) . . . . ? P3 N5 C18 C21 46.2(4) . . . . ? P4 N5 C18 C21 -171.5(2) . . . . ? P3 N6 C22 C23 12.0(4) . . . . ? P4 N6 C22 C23 -152.6(2) . . . . ? P3 N6 C22 C24 -108.9(3) . . . . ? P4 N6 C22 C24 86.5(3) . . . . ? P3 N6 C22 C25 132.1(3) . . . . ? P4 N6 C22 C25 -32.4(4) . . . . ? P3 N7 C27 C30 6.3(4) . . . . ? P3 N7 C27 C29 -115.0(3) . . . . ? P3 N7 C27 C28 127.0(3) . . . . ? P4 N8 C31 C34 120.5(4) . . . . ? P4 N8 C31 C33 -0.2(5) . . . . ? P4 N8 C31 C32 -118.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.649 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.067 # Attachment 'Compound_7.cif' data_msb028b _database_code_depnum_ccdc_archive 'CCDC 679232' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H41 Au Cl I N4 P2' _chemical_formula_weight 722.79 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.5625(7) _cell_length_b 11.9084(13) _cell_length_c 15.895(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.376(3) _cell_angle_gamma 90.00 _cell_volume 2591.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.852 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 7.103 _exptl_absorpt_correction_T_min 0.2027 _exptl_absorpt_correction_T_max 0.3170 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET) (compiled Mar 23 2006,23:39:28) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14699 _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4359 _reflns_number_gt 3809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0833P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4359 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1229 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 0.152842(17) 0.18752(2) 0.167065(18) 0.02200(14) Uani 1 1 d . . . Cl1 Cl 0.49169(11) -0.16739(13) 0.33788(13) 0.0216(4) Uani 1 1 d . . . I1 I 0.04557(3) 0.35490(4) 0.07914(3) 0.02723(16) Uani 1 1 d . . . P1 P 0.25067(11) 0.04101(15) 0.23700(12) 0.0194(4) Uani 1 1 d . . . P2 P 0.20404(12) -0.16200(15) 0.23015(12) 0.0197(4) Uani 1 1 d . . . N1 N 0.2337(4) -0.0746(5) 0.1671(4) 0.0210(12) Uani 1 1 d . . . N2 N 0.2212(4) -0.0522(5) 0.3004(4) 0.0211(12) Uani 1 1 d . . . N3 N 0.3662(4) 0.0710(5) 0.2932(4) 0.0235(12) Uani 1 1 d . . . H3 H 0.4037 0.0134 0.3147 0.028 Uiso 1 1 calc R . . N4 N 0.2792(4) -0.2626(5) 0.2739(4) 0.0258(13) Uani 1 1 d . . . H4 H 0.3375 -0.2385 0.2917 0.031 Uiso 1 1 calc R . . C1 C 0.2332(5) -0.0841(6) 0.0723(5) 0.0282(16) Uani 1 1 d . . . C2 C 0.1337(6) -0.0498(8) -0.0068(6) 0.040(2) Uani 1 1 d . . . H2A H 0.0848 -0.0992 -0.0071 0.060 Uiso 1 1 calc R . . H2B H 0.1334 -0.0543 -0.0673 0.060 Uiso 1 1 calc R . . H2C H 0.1199 0.0259 0.0038 0.060 Uiso 1 1 calc R . . C3 C 0.2549(7) -0.2069(7) 0.0597(6) 0.0350(19) Uani 1 1 d . . . H3A H 0.3149 -0.2297 0.1138 0.052 Uiso 1 1 calc R . . H3B H 0.2606 -0.2141 0.0025 0.052 Uiso 1 1 calc R . . H3C H 0.2026 -0.2538 0.0551 0.052 Uiso 1 1 calc R . . C4 C 0.3133(6) -0.0111(7) 0.0748(6) 0.0392(19) Uani 1 1 d . . . H4A H 0.3017 0.0656 0.0850 0.059 Uiso 1 1 calc R . . H4B H 0.3143 -0.0172 0.0150 0.059 Uiso 1 1 calc R . . H4C H 0.3750 -0.0351 0.1258 0.059 Uiso 1 1 calc R . . C5 C 0.1970(5) -0.0323(7) 0.3802(5) 0.0279(16) Uani 1 1 d . . . C6 C 0.2154(5) -0.1404(7) 0.4364(5) 0.0302(17) Uani 1 1 d . . . H6A H 0.1701 -0.1968 0.3967 0.045 Uiso 1 1 calc R . . H6B H 0.2067 -0.1275 0.4915 0.045 Uiso 1 1 calc R . . H6C H 0.2809 -0.1654 0.4565 0.045 Uiso 1 1 calc R . . C7 C 0.0894(5) 0.0010(7) 0.3383(6) 0.0370(19) Uani 1 1 d . . . H7A H 0.0763 0.0646 0.2968 0.055 Uiso 1 1 calc R . . H7B H 0.0755 0.0202 0.3893 0.055 Uiso 1 1 calc R . . H7C H 0.0489 -0.0608 0.3026 0.055 Uiso 1 1 calc R . . C8 C 0.2615(6) 0.0620(7) 0.4416(6) 0.0358(19) Uani 1 1 d . . . H8A H 0.3288 0.0433 0.4631 0.054 Uiso 1 1 calc R . . H8B H 0.2511 0.0726 0.4960 0.054 Uiso 1 1 calc R . . H8C H 0.2457 0.1300 0.4049 0.054 Uiso 1 1 calc R . . C9 C 0.0806(5) -0.2078(6) 0.1729(6) 0.0282(16) Uani 1 1 d . . . H9A H 0.0700 -0.2578 0.1215 0.042 Uiso 1 1 calc R . . H9B H 0.0382 -0.1440 0.1480 0.042 Uiso 1 1 calc R . . H9C H 0.0670 -0.2463 0.2183 0.042 Uiso 1 1 calc R . . C10 C 0.2821(5) -0.3852(6) 0.2943(5) 0.0283(16) Uani 1 1 d . . . C11 C 0.3675(6) -0.4029(7) 0.3946(5) 0.0346(18) Uani 1 1 d . . . H11A H 0.4277 -0.3855 0.3945 0.052 Uiso 1 1 calc R . . H11B H 0.3685 -0.4797 0.4135 0.052 Uiso 1 1 calc R . . H11C H 0.3598 -0.3545 0.4389 0.052 Uiso 1 1 calc R . . C12 C 0.3022(6) -0.4472(7) 0.2214(6) 0.040(2) Uani 1 1 d . . . H12A H 0.2510 -0.4314 0.1581 0.061 Uiso 1 1 calc R . . H12B H 0.3047 -0.5265 0.2331 0.061 Uiso 1 1 calc R . . H12C H 0.3636 -0.4227 0.2272 0.061 Uiso 1 1 calc R . . C13 C 0.1877(6) -0.4267(7) 0.2901(6) 0.0384(19) Uani 1 1 d . . . H13A H 0.1727 -0.3817 0.3315 0.058 Uiso 1 1 calc R . . H13B H 0.1953 -0.5037 0.3103 0.058 Uiso 1 1 calc R . . H13C H 0.1355 -0.4209 0.2257 0.058 Uiso 1 1 calc R . . C14 C 0.4191(5) 0.1807(6) 0.3145(6) 0.0283(17) Uani 1 1 d . . . C15 C 0.3907(6) 0.2552(7) 0.3757(5) 0.0377(19) Uani 1 1 d . . . H15A H 0.3977 0.2136 0.4304 0.057 Uiso 1 1 calc R . . H15B H 0.3240 0.2788 0.3386 0.057 Uiso 1 1 calc R . . H15C H 0.4324 0.3199 0.3967 0.057 Uiso 1 1 calc R . . C16 C 0.3968(5) 0.2424(6) 0.2226(5) 0.0292(16) Uani 1 1 d . . . H16A H 0.4323 0.3119 0.2378 0.044 Uiso 1 1 calc R . . H16B H 0.3281 0.2576 0.1874 0.044 Uiso 1 1 calc R . . H16C H 0.4160 0.1967 0.1846 0.044 Uiso 1 1 calc R . . C17 C 0.5254(6) 0.1509(8) 0.3679(8) 0.053(3) Uani 1 1 d . . . H17A H 0.5396 0.1164 0.4277 0.079 Uiso 1 1 calc R . . H17B H 0.5640 0.2178 0.3797 0.079 Uiso 1 1 calc R . . H17C H 0.5409 0.0995 0.3305 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.02416(19) 0.0188(2) 0.0204(2) 0.00139(10) 0.00843(14) 0.00146(9) Cl1 0.0166(7) 0.0164(8) 0.0365(10) 0.0012(7) 0.0164(7) 0.0012(6) I1 0.0291(3) 0.0224(3) 0.0262(3) 0.00291(19) 0.0098(2) 0.00361(18) P1 0.0219(8) 0.0170(9) 0.0176(9) -0.0015(7) 0.0079(7) -0.0008(7) P2 0.0254(8) 0.0175(9) 0.0142(9) -0.0027(7) 0.0079(7) -0.0025(7) N1 0.030(3) 0.017(3) 0.013(3) -0.001(2) 0.008(2) -0.005(2) N2 0.026(3) 0.016(3) 0.023(3) -0.001(2) 0.012(2) 0.004(2) N3 0.024(3) 0.015(3) 0.025(3) 0.003(2) 0.007(2) 0.004(2) N4 0.035(3) 0.018(3) 0.031(3) -0.004(3) 0.020(3) -0.004(3) C1 0.043(4) 0.027(4) 0.014(3) -0.005(3) 0.013(3) -0.006(3) C2 0.047(4) 0.043(5) 0.022(4) 0.005(4) 0.010(4) -0.002(4) C3 0.061(5) 0.034(4) 0.025(4) -0.005(3) 0.033(4) -0.006(4) C4 0.055(5) 0.033(5) 0.037(4) -0.009(4) 0.027(4) -0.015(4) C5 0.037(4) 0.033(4) 0.020(4) -0.004(3) 0.018(3) -0.002(3) C6 0.037(4) 0.038(5) 0.017(4) -0.002(3) 0.015(3) -0.001(3) C7 0.037(4) 0.045(5) 0.038(5) -0.003(4) 0.025(4) 0.005(4) C8 0.055(5) 0.037(5) 0.028(4) -0.017(4) 0.030(4) -0.011(4) C9 0.026(3) 0.024(4) 0.030(4) -0.004(3) 0.009(3) -0.006(3) C10 0.042(4) 0.018(4) 0.026(4) -0.002(3) 0.017(3) 0.004(3) C11 0.045(4) 0.030(4) 0.026(4) 0.005(3) 0.014(3) 0.006(4) C12 0.057(5) 0.032(5) 0.045(5) -0.005(4) 0.034(4) 0.003(4) C13 0.047(5) 0.020(4) 0.052(5) 0.002(4) 0.027(4) -0.004(3) C14 0.032(4) 0.019(4) 0.030(4) -0.008(3) 0.012(3) -0.008(3) C15 0.055(5) 0.031(5) 0.024(4) -0.009(3) 0.016(4) -0.015(4) C16 0.034(4) 0.025(4) 0.033(4) -0.001(3) 0.020(3) -0.003(3) C17 0.029(4) 0.037(5) 0.069(7) 0.005(5) 0.005(4) -0.009(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 P1 2.2336(17) . ? Au1 I1 2.5487(5) . ? P1 N3 1.622(6) . ? P1 N2 1.701(6) . ? P1 N1 1.709(6) . ? P1 P2 2.512(2) . ? P2 N4 1.585(6) . ? P2 N1 1.656(6) . ? P2 N2 1.657(6) . ? P2 C9 1.775(7) . ? N1 C1 1.506(9) . ? N2 C5 1.504(9) . ? N3 C14 1.495(9) . ? N3 H3 0.8600 . ? N4 C10 1.492(10) . ? N4 H4 0.8600 . ? C1 C4 1.505(10) . ? C1 C2 1.515(10) . ? C1 C3 1.535(11) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 C8 1.514(11) . ? C5 C6 1.515(11) . ? C5 C7 1.531(10) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C13 1.521(10) . ? C10 C12 1.526(10) . ? C10 C11 1.530(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C17 1.500(11) . ? C14 C16 1.521(11) . ? C14 C15 1.531(11) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 I1 176.13(5) . . ? N3 P1 N2 110.9(3) . . ? N3 P1 N1 108.9(3) . . ? N2 P1 N1 81.8(3) . . ? N3 P1 Au1 114.7(2) . . ? N2 P1 Au1 119.49(19) . . ? N1 P1 Au1 116.6(2) . . ? N3 P1 P2 117.2(2) . . ? N2 P1 P2 40.92(19) . . ? N1 P1 P2 40.91(19) . . ? Au1 P1 P2 128.00(8) . . ? N4 P2 N1 112.3(3) . . ? N4 P2 N2 116.9(3) . . ? N1 P2 N2 84.8(3) . . ? N4 P2 C9 112.7(3) . . ? N1 P2 C9 115.3(3) . . ? N2 P2 C9 112.1(3) . . ? N4 P2 P1 124.8(2) . . ? N1 P2 P1 42.5(2) . . ? N2 P2 P1 42.3(2) . . ? C9 P2 P1 122.5(3) . . ? C1 N1 P2 133.4(5) . . ? C1 N1 P1 129.5(5) . . ? P2 N1 P1 96.5(3) . . ? C5 N2 P2 131.9(5) . . ? C5 N2 P1 130.0(5) . . ? P2 N2 P1 96.8(3) . . ? C14 N3 P1 131.6(5) . . ? C14 N3 H3 114.2 . . ? P1 N3 H3 114.2 . . ? C10 N4 P2 140.7(5) . . ? C10 N4 H4 109.6 . . ? P2 N4 H4 109.6 . . ? C4 C1 N1 108.7(6) . . ? C4 C1 C2 111.9(7) . . ? N1 C1 C2 109.1(6) . . ? C4 C1 C3 108.8(7) . . ? N1 C1 C3 107.7(6) . . ? C2 C1 C3 110.5(7) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C8 107.8(6) . . ? N2 C5 C6 108.1(6) . . ? C8 C5 C6 111.6(6) . . ? N2 C5 C7 109.6(6) . . ? C8 C5 C7 110.0(7) . . ? C6 C5 C7 109.7(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P2 C9 H9A 109.5 . . ? P2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N4 C10 C13 112.3(6) . . ? N4 C10 C12 107.7(6) . . ? C13 C10 C12 110.6(7) . . ? N4 C10 C11 106.4(6) . . ? C13 C10 C11 110.1(6) . . ? C12 C10 C11 109.6(6) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N3 C14 C17 105.3(6) . . ? N3 C14 C16 110.8(6) . . ? C17 C14 C16 110.2(7) . . ? N3 C14 C15 110.8(6) . . ? C17 C14 C15 110.6(7) . . ? C16 C14 C15 109.1(6) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag I1 Au1 P1 N3 70.4(7) . . . . ? I1 Au1 P1 N2 -154.2(6) . . . . ? I1 Au1 P1 N1 -58.5(7) . . . . ? I1 Au1 P1 P2 -105.5(6) . . . . ? N3 P1 P2 N4 -2.0(4) . . . . ? N2 P1 P2 N4 -93.1(4) . . . . ? N1 P1 P2 N4 85.9(4) . . . . ? Au1 P1 P2 N4 173.9(3) . . . . ? N3 P1 P2 N1 -87.8(4) . . . . ? N2 P1 P2 N1 -179.0(4) . . . . ? Au1 P1 P2 N1 88.0(3) . . . . ? N3 P1 P2 N2 91.1(4) . . . . ? N1 P1 P2 N2 179.0(4) . . . . ? Au1 P1 P2 N2 -93.0(3) . . . . ? N3 P1 P2 C9 179.0(4) . . . . ? N2 P1 P2 C9 87.8(4) . . . . ? N1 P1 P2 C9 -93.2(4) . . . . ? Au1 P1 P2 C9 -5.2(4) . . . . ? N4 P2 N1 C1 70.2(7) . . . . ? N2 P2 N1 C1 -172.8(6) . . . . ? C9 P2 N1 C1 -60.8(7) . . . . ? P1 P2 N1 C1 -172.1(8) . . . . ? N4 P2 N1 P1 -117.6(3) . . . . ? N2 P2 N1 P1 -0.7(3) . . . . ? C9 P2 N1 P1 111.3(3) . . . . ? N3 P1 N1 C1 -77.3(6) . . . . ? N2 P1 N1 C1 173.3(6) . . . . ? Au1 P1 N1 C1 54.3(6) . . . . ? P2 P1 N1 C1 172.6(7) . . . . ? N3 P1 N1 P2 110.1(3) . . . . ? N2 P1 N1 P2 0.7(3) . . . . ? Au1 P1 N1 P2 -118.3(2) . . . . ? N4 P2 N2 C5 -79.2(6) . . . . ? N1 P2 N2 C5 168.3(6) . . . . ? C9 P2 N2 C5 53.0(7) . . . . ? P1 P2 N2 C5 167.6(7) . . . . ? N4 P2 N2 P1 113.1(3) . . . . ? N1 P2 N2 P1 0.7(3) . . . . ? C9 P2 N2 P1 -114.6(4) . . . . ? N3 P1 N2 C5 84.2(6) . . . . ? N1 P1 N2 C5 -168.6(6) . . . . ? Au1 P1 N2 C5 -52.7(6) . . . . ? P2 P1 N2 C5 -168.0(7) . . . . ? N3 P1 N2 P2 -107.9(3) . . . . ? N1 P1 N2 P2 -0.7(3) . . . . ? Au1 P1 N2 P2 115.3(2) . . . . ? N2 P1 N3 C14 -132.7(6) . . . . ? N1 P1 N3 C14 139.0(6) . . . . ? Au1 P1 N3 C14 6.3(7) . . . . ? P2 P1 N3 C14 -177.2(6) . . . . ? N1 P2 N4 C10 -142.5(7) . . . . ? N2 P2 N4 C10 121.9(7) . . . . ? C9 P2 N4 C10 -10.1(9) . . . . ? P1 P2 N4 C10 170.7(6) . . . . ? P2 N1 C1 C4 -149.6(6) . . . . ? P1 N1 C1 C4 40.5(8) . . . . ? P2 N1 C1 C2 88.2(8) . . . . ? P1 N1 C1 C2 -81.7(7) . . . . ? P2 N1 C1 C3 -31.8(9) . . . . ? P1 N1 C1 C3 158.3(5) . . . . ? P2 N2 C5 C8 158.9(6) . . . . ? P1 N2 C5 C8 -37.2(8) . . . . ? P2 N2 C5 C6 38.1(8) . . . . ? P1 N2 C5 C6 -158.0(5) . . . . ? P2 N2 C5 C7 -81.4(8) . . . . ? P1 N2 C5 C7 82.4(8) . . . . ? P2 N4 C10 C13 -15.5(11) . . . . ? P2 N4 C10 C12 106.6(8) . . . . ? P2 N4 C10 C11 -136.0(7) . . . . ? P1 N3 C14 C17 -179.3(7) . . . . ? P1 N3 C14 C16 -60.2(9) . . . . ? P1 N3 C14 C15 61.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 2.787 _refine_diff_density_min -1.169 _refine_diff_density_rms 0.231