# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_mdau _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H22 Au Cl N2 Ni O S2' _chemical_formula_weight 541.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -4.4197 7.2980 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 '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 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 8.3017(7) _cell_length_b 8.6040(8) _cell_length_c 21.8658(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.316(5) _cell_angle_gamma 90.00 _cell_volume 1555.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 3135 _cell_measurement_theta_min 4.06 _cell_measurement_theta_max 63.50 _exptl_crystal_description 'plate ' _exptl_crystal_colour 'orange ' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1040 _exptl_absorpt_coefficient_mu 22.996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0259 _exptl_absorpt_correction_T_max 0.2331 _exptl_absorpt_process_details sadabs _exptl_special_details ; FACE absorption correction Crystal faces: H K L d(mm) 1.000 0.000 0.000 0.10000 -1.000 0.000 0.000 0.10000 0.000 1.000 0.000 0.10000 0.000 -1.000 0.000 0.10000 0.000 0.000 1.000 0.05000 0.000 0.000 -1.000 0.05000 Linear absorption coefficient set to 23.00 mm-1, giving Rint = 0.1001 Minimum and maximum transmission coefficients = 0.02603 and 0.21991 Minimum and maximum t-bar = 0.0402 and 0.1060 mm All Rint values calculated using 18859 selected reflections only ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'MWPC area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25177 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 5.53 _diffrn_reflns_theta_max 64.01 _reflns_number_total 2554 _reflns_number_gt 2268 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker FRAMBO' _computing_cell_refinement 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0400P)^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 2554 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 0.15008(3) -0.06951(2) 0.038314(9) 0.01540(9) Uani 1 1 d . . . Ni1 Ni -0.00723(10) 0.24789(10) 0.08802(4) 0.01372(19) Uani 1 1 d . . . Cl1 Cl 0.40017(18) -0.42317(17) 0.15392(6) 0.0282(3) Uani 1 1 d . . . S1 S 0.23678(15) 0.17166(14) 0.07267(5) 0.0159(3) Uani 1 1 d . . . S2 S -0.07259(15) 0.31520(14) -0.00717(5) 0.0164(3) Uani 1 1 d . . . O1ME O 0.6228(5) -0.1457(5) 0.14476(17) 0.0283(9) Uani 1 1 d . . . H1ME H 0.5635 -0.2014 0.1668 0.042 Uiso 1 1 d R . . N1 N -0.2092(5) 0.3274(5) 0.11185(18) 0.0155(9) Uani 1 1 d . . . N2 N 0.0301(5) 0.2032(5) 0.17432(18) 0.0135(8) Uani 1 1 d . . . C1 C 0.3080(6) 0.1362(7) 0.1540(2) 0.0190(11) Uani 1 1 d . . . H1A H 0.3908 0.0530 0.1570 0.023 Uiso 1 1 calc R . . H1B H 0.3576 0.2318 0.1726 0.023 Uiso 1 1 calc R . . C2 C 0.1677(6) 0.0889(6) 0.1876(2) 0.0178(11) Uani 1 1 d . . . H2A H 0.2004 0.0861 0.2323 0.021 Uiso 1 1 calc R . . H2B H 0.1317 -0.0166 0.1744 0.021 Uiso 1 1 calc R . . C3 C -0.1233(6) 0.1389(6) 0.1947(2) 0.0191(11) Uani 1 1 d . . . H3A H -0.1262 0.1558 0.2394 0.023 Uiso 1 1 calc R . . H3B H -0.1289 0.0257 0.1867 0.023 Uiso 1 1 calc R . . C4 C -0.2690(6) 0.2207(6) 0.1593(2) 0.0165(10) Uani 1 1 d . . . H4A H -0.3431 0.1422 0.1390 0.020 Uiso 1 1 calc R . . H4B H -0.3294 0.2812 0.1882 0.020 Uiso 1 1 calc R . . C5 C -0.2608(7) 0.4165(6) 0.0047(2) 0.0188(11) Uani 1 1 d . . . H5A H -0.2385 0.5280 0.0128 0.023 Uiso 1 1 calc R . . H5B H -0.3372 0.4082 -0.0327 0.023 Uiso 1 1 calc R . . C6 C -0.3351(6) 0.3448(6) 0.0586(2) 0.0192(11) Uani 1 1 d . . . H6A H -0.4240 0.4117 0.0706 0.023 Uiso 1 1 calc R . . H6B H -0.3809 0.2417 0.0468 0.023 Uiso 1 1 calc R . . C7 C -0.1654(6) 0.4822(6) 0.1399(2) 0.0182(11) Uani 1 1 d . . . H7A H -0.2654 0.5424 0.1440 0.022 Uiso 1 1 calc R . . H7B H -0.0991 0.5405 0.1123 0.022 Uiso 1 1 calc R . . C8 C -0.0710(7) 0.4667(6) 0.2032(2) 0.0198(12) Uani 1 1 d . . . H8A H -0.1461 0.4309 0.2329 0.024 Uiso 1 1 calc R . . H8B H -0.0308 0.5706 0.2166 0.024 Uiso 1 1 calc R . . C9 C 0.0728(6) 0.3543(6) 0.2054(2) 0.0177(11) Uani 1 1 d . . . H9A H 0.1619 0.4037 0.1853 0.021 Uiso 1 1 calc R . . H9B H 0.1122 0.3342 0.2488 0.021 Uiso 1 1 calc R . . C1ME C 0.6454(8) -0.1445(8) 0.0813(3) 0.0319(14) Uani 1 1 d . . . H1MA H 0.5573 -0.0862 0.0588 0.048 Uiso 1 1 calc R . . H1MB H 0.6454 -0.2515 0.0659 0.048 Uiso 1 1 calc R . . H1MC H 0.7491 -0.0951 0.0752 0.048 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 0.01665(14) 0.01255(14) 0.01708(12) -0.00147(8) 0.00203(8) -0.00025(8) Ni1 0.0137(5) 0.0121(5) 0.0154(4) -0.0001(3) 0.0021(3) -0.0003(3) Cl1 0.0295(8) 0.0346(9) 0.0214(6) -0.0039(5) 0.0064(5) -0.0140(6) S1 0.0158(6) 0.0139(7) 0.0183(5) -0.0012(5) 0.0030(5) -0.0013(5) S2 0.0196(7) 0.0127(7) 0.0168(5) 0.0001(4) 0.0012(5) -0.0007(5) O1ME 0.039(3) 0.024(2) 0.0235(19) -0.0027(16) 0.0122(17) -0.0106(18) N1 0.015(2) 0.010(2) 0.021(2) -0.0025(17) 0.0005(17) -0.0017(17) N2 0.011(2) 0.013(2) 0.0170(19) 0.0015(16) 0.0029(16) 0.0017(17) C1 0.017(3) 0.020(3) 0.020(2) -0.003(2) -0.002(2) 0.002(2) C2 0.020(3) 0.015(3) 0.019(2) 0.0011(19) 0.000(2) 0.005(2) C3 0.016(3) 0.020(3) 0.022(3) 0.005(2) 0.004(2) -0.005(2) C4 0.012(3) 0.014(3) 0.024(2) 0.004(2) 0.006(2) -0.003(2) C5 0.023(3) 0.010(3) 0.024(3) 0.001(2) 0.000(2) 0.003(2) C6 0.017(3) 0.018(3) 0.021(3) 0.003(2) -0.002(2) 0.003(2) C7 0.018(3) 0.009(3) 0.027(3) -0.003(2) 0.002(2) 0.000(2) C8 0.022(3) 0.018(3) 0.021(3) -0.007(2) 0.004(2) -0.002(2) C9 0.019(3) 0.016(3) 0.017(2) -0.002(2) 0.002(2) -0.003(2) C1ME 0.036(4) 0.033(4) 0.028(3) 0.002(3) 0.011(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 S2 2.2946(13) 3 ? Au1 S1 2.2995(12) . ? Au1 Au1 3.1103(5) 3 ? Ni1 N2 1.922(4) . ? Ni1 N1 1.926(4) . ? Ni1 S2 2.1802(14) . ? Ni1 S1 2.1845(15) . ? S1 C1 1.848(5) . ? S2 C5 1.829(5) . ? S2 Au1 2.2946(13) 3 ? O1ME C1ME 1.418(7) . ? O1ME H1ME 0.8653 . ? N1 C7 1.498(6) . ? N1 C6 1.498(6) . ? N1 C4 1.503(6) . ? N2 C3 1.494(6) . ? N2 C9 1.495(7) . ? N2 C2 1.515(6) . ? C1 C2 1.489(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.544(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.512(7) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.531(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.534(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C1ME H1MA 0.9800 . ? C1ME H1MB 0.9800 . ? C1ME H1MC 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 S2 Au1 S1 177.35(4) 3 . ? S2 Au1 Au1 90.33(3) 3 3 ? S1 Au1 Au1 92.28(3) . 3 ? N2 Ni1 N1 82.57(17) . . ? N2 Ni1 S2 173.42(13) . . ? N1 Ni1 S2 91.03(13) . . ? N2 Ni1 S1 91.34(13) . . ? N1 Ni1 S1 172.17(13) . . ? S2 Ni1 S1 94.90(6) . . ? C1 S1 Ni1 96.90(17) . . ? C1 S1 Au1 103.18(18) . . ? Ni1 S1 Au1 93.13(5) . . ? C5 S2 Ni1 97.57(17) . . ? C5 S2 Au1 105.16(17) . 3 ? Ni1 S2 Au1 94.40(5) . 3 ? C1ME O1ME H1ME 133.1 . . ? C7 N1 C6 110.8(4) . . ? C7 N1 C4 110.1(4) . . ? C6 N1 C4 110.2(4) . . ? C7 N1 Ni1 104.0(3) . . ? C6 N1 Ni1 112.8(3) . . ? C4 N1 Ni1 108.7(3) . . ? C3 N2 C9 111.1(4) . . ? C3 N2 C2 110.6(4) . . ? C9 N2 C2 109.6(4) . . ? C3 N2 Ni1 107.6(3) . . ? C9 N2 Ni1 106.4(3) . . ? C2 N2 Ni1 111.6(3) . . ? C2 C1 S1 108.9(3) . . ? C2 C1 H1A 109.9 . . ? S1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? S1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? C1 C2 N2 109.8(4) . . ? C1 C2 H2A 109.7 . . ? N2 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? N2 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 109.4(4) . . ? N2 C3 H3A 109.8 . . ? C4 C3 H3A 109.8 . . ? N2 C3 H3B 109.8 . . ? C4 C3 H3B 109.8 . . ? H3A C3 H3B 108.3 . . ? N1 C4 C3 109.3(4) . . ? N1 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? N1 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.3 . . ? C6 C5 S2 109.4(4) . . ? C6 C5 H5A 109.8 . . ? S2 C5 H5A 109.8 . . ? C6 C5 H5B 109.8 . . ? S2 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? N1 C6 C5 110.0(4) . . ? N1 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? N1 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? N1 C7 C8 112.2(4) . . ? N1 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N1 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 114.5(4) . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? C7 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N2 C9 C8 112.5(4) . . ? N2 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? N2 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? O1ME C1ME H1MA 109.5 . . ? O1ME C1ME H1MB 109.5 . . ? H1MA C1ME H1MB 109.5 . . ? O1ME C1ME H1MC 109.5 . . ? H1MA C1ME H1MC 109.5 . . ? H1MB C1ME H1MC 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 N2 Ni1 S1 C1 -4.7(2) . . . . ? N1 Ni1 S1 C1 34.1(10) . . . . ? S2 Ni1 S1 C1 173.21(18) . . . . ? N2 Ni1 S1 Au1 98.99(13) . . . . ? N1 Ni1 S1 Au1 137.8(10) . . . . ? S2 Ni1 S1 Au1 -83.10(5) . . . . ? S2 Au1 S1 C1 -31.6(10) 3 . . . ? Au1 Au1 S1 C1 139.72(17) 3 . . . ? S2 Au1 S1 Ni1 -129.4(9) 3 . . . ? Au1 Au1 S1 Ni1 41.88(4) 3 . . . ? N2 Ni1 S2 C5 -7.8(12) . . . . ? N1 Ni1 S2 C5 5.6(2) . . . . ? S1 Ni1 S2 C5 -169.27(17) . . . . ? N2 Ni1 S2 Au1 -113.7(12) . . . 3 ? N1 Ni1 S2 Au1 -100.33(13) . . . 3 ? S1 Ni1 S2 Au1 84.78(5) . . . 3 ? N2 Ni1 N1 C7 77.7(3) . . . . ? S2 Ni1 N1 C7 -100.7(3) . . . . ? S1 Ni1 N1 C7 38.5(12) . . . . ? N2 Ni1 N1 C6 -162.1(4) . . . . ? S2 Ni1 N1 C6 19.4(3) . . . . ? S1 Ni1 N1 C6 158.7(8) . . . . ? N2 Ni1 N1 C4 -39.5(3) . . . . ? S2 Ni1 N1 C4 142.0(3) . . . . ? S1 Ni1 N1 C4 -78.7(11) . . . . ? N1 Ni1 N2 C3 42.4(3) . . . . ? S2 Ni1 N2 C3 56.0(14) . . . . ? S1 Ni1 N2 C3 -142.5(3) . . . . ? N1 Ni1 N2 C9 -76.7(3) . . . . ? S2 Ni1 N2 C9 -63.1(13) . . . . ? S1 Ni1 N2 C9 98.4(3) . . . . ? N1 Ni1 N2 C2 163.9(3) . . . . ? S2 Ni1 N2 C2 177.4(10) . . . . ? S1 Ni1 N2 C2 -21.0(3) . . . . ? Ni1 S1 C1 C2 30.3(4) . . . . ? Au1 S1 C1 C2 -64.6(4) . . . . ? S1 C1 C2 N2 -50.2(5) . . . . ? C3 N2 C2 C1 166.4(4) . . . . ? C9 N2 C2 C1 -70.8(5) . . . . ? Ni1 N2 C2 C1 46.7(5) . . . . ? C9 N2 C3 C4 80.5(5) . . . . ? C2 N2 C3 C4 -157.7(4) . . . . ? Ni1 N2 C3 C4 -35.6(5) . . . . ? C7 N1 C4 C3 -85.9(5) . . . . ? C6 N1 C4 C3 151.6(4) . . . . ? Ni1 N1 C4 C3 27.4(5) . . . . ? N2 C3 C4 N1 5.2(6) . . . . ? Ni1 S2 C5 C6 -29.6(4) . . . . ? Au1 S2 C5 C6 67.1(4) 3 . . . ? C7 N1 C6 C5 72.4(5) . . . . ? C4 N1 C6 C5 -165.5(4) . . . . ? Ni1 N1 C6 C5 -43.7(5) . . . . ? S2 C5 C6 N1 47.9(5) . . . . ? C6 N1 C7 C8 165.6(4) . . . . ? C4 N1 C7 C8 43.4(6) . . . . ? Ni1 N1 C7 C8 -73.0(4) . . . . ? N1 C7 C8 C9 49.6(6) . . . . ? C3 N2 C9 C8 -47.9(5) . . . . ? C2 N2 C9 C8 -170.3(4) . . . . ? Ni1 N2 C9 C8 68.9(4) . . . . ? C7 C8 C9 N2 -47.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 64.01 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.797 _refine_diff_density_min -1.532 _refine_diff_density_rms 0.156 _database_code_depnum_ccdc_archive 'CCDC 956179' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_041213nibmedacoapph3inmeoh_0m-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H48 Au2 Cl2 N4 Ni2 O2 S4' _chemical_formula_weight 1111.14 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' S S 0.1246 0.1234 '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' Ni Ni 0.3393 1.1124 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.661(2) _cell_length_b 15.988(4) _cell_length_c 13.637(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.346(3) _cell_angle_gamma 90.00 _cell_volume 1857.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _diffrn_ambient_temperature 110(2) _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 9.265 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1676 _exptl_absorpt_correction_T_max 0.4576 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4584 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0316 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.28 _reflns_number_total 4584 _reflns_number_gt 4084 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0200P)^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 4584 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0234 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0474 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.617265(12) -0.072419(6) 0.537268(7) 0.01776(4) Uani 1 1 d . . . Ni1 Ni 0.58245(4) 0.075977(17) 0.68684(2) 0.01224(7) Uani 1 1 d . . . N1 N 0.8042(3) 0.07037(11) 0.75626(16) 0.0148(4) Uani 1 1 d . . . N2 N 0.5902(2) 0.19897(12) 0.68999(15) 0.0139(4) Uani 1 1 d . . . S1 S 0.56257(8) -0.05962(4) 0.69581(5) 0.01861(14) Uani 1 1 d . . . S2 S 0.33182(8) 0.08056(4) 0.62229(5) 0.01774(14) Uani 1 1 d . . . C1 C 0.7471(3) -0.08014(15) 0.7811(2) 0.0230(6) Uani 1 1 d . . . H1A H 0.7317 -0.0752 0.8496 0.028 Uiso 1 1 calc R . . H1B H 0.7830 -0.1364 0.7711 0.028 Uiso 1 1 calc R . . C2 C 0.8671(3) -0.01749(16) 0.7608(2) 0.0215(6) Uani 1 1 d . . . H2A H 0.9592 -0.0211 0.8129 0.026 Uiso 1 1 calc R . . H2B H 0.8989 -0.0310 0.6979 0.026 Uiso 1 1 calc R . . C3 C 0.2997(3) 0.19146(16) 0.6440(2) 0.0200(6) Uani 1 1 d . . . H3A H 0.2102 0.2118 0.5968 0.024 Uiso 1 1 calc R . . H3B H 0.2788 0.1997 0.7109 0.024 Uiso 1 1 calc R . . C4 C 0.4453(3) 0.23799(15) 0.63125(19) 0.0176(5) Uani 1 1 d . . . H4A H 0.4533 0.2386 0.5612 0.021 Uiso 1 1 calc R . . H4B H 0.4376 0.2955 0.6527 0.021 Uiso 1 1 calc R . . C5 C 0.6072(3) 0.22349(16) 0.79841(18) 0.0177(5) Uani 1 1 d . . . H5A H 0.5072 0.2446 0.8104 0.021 Uiso 1 1 calc R . . H5B H 0.6830 0.2686 0.8120 0.021 Uiso 1 1 calc R . . C6 C 0.6594(3) 0.15198(16) 0.87059(18) 0.0185(5) Uani 1 1 d . . . H6A H 0.5735 0.1122 0.8646 0.022 Uiso 1 1 calc R . . H6B H 0.6743 0.1746 0.9376 0.022 Uiso 1 1 calc R . . C7 C 0.8078(3) 0.10335(16) 0.86036(19) 0.0180(5) Uani 1 1 d . . . H7A H 0.8982 0.1397 0.8783 0.022 Uiso 1 1 calc R . . H7B H 0.8201 0.0568 0.9067 0.022 Uiso 1 1 calc R . . C8 C 0.9146(3) 0.11988(16) 0.7057(2) 0.0199(5) Uani 1 1 d . . . H8A H 0.9079 0.0990 0.6383 0.024 Uiso 1 1 calc R . . H8B H 1.0209 0.1104 0.7407 0.024 Uiso 1 1 calc R . . C9 C 0.8842(3) 0.21271(16) 0.7011(2) 0.0219(6) Uani 1 1 d . . . H9A H 0.9621 0.2396 0.6687 0.026 Uiso 1 1 calc R . . H9B H 0.8965 0.2345 0.7684 0.026 Uiso 1 1 calc R . . C10 C 0.7225(3) 0.23498(15) 0.64544(19) 0.0194(5) Uani 1 1 d . . . H10A H 0.7123 0.2954 0.6435 0.023 Uiso 1 1 calc R . . H10B H 0.7125 0.2154 0.5773 0.023 Uiso 1 1 calc R . . C11 C 0.1024(4) 0.88480(19) 0.5735(2) 0.0319(7) Uani 1 1 d . . . H11A H 0.1069 0.8851 0.6443 0.048 Uiso 1 1 calc R . . H11B H 0.0198 0.9213 0.5424 0.048 Uiso 1 1 calc R . . H11C H 0.2008 0.9038 0.5586 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.77829(8) 0.73009(4) 0.60737(5) 0.02463(14) Uani 1 1 d . . . O1 O 0.0725(2) 0.80265(13) 0.53682(15) 0.0288(5) Uani 1 1 d . . . H1 H -0.0092 0.7855 0.5521 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 Au1 0.01992(6) 0.01772(6) 0.01522(6) -0.00512(4) 0.00203(4) -0.00221(4) Ni1 0.01350(16) 0.01168(15) 0.01158(16) -0.00168(11) 0.00235(12) -0.00119(11) N1 0.0174(11) 0.0140(10) 0.0133(11) -0.0001(8) 0.0031(9) 0.0001(8) N2 0.0160(10) 0.0127(10) 0.0134(10) -0.0006(8) 0.0039(8) -0.0010(8) S1 0.0252(3) 0.0132(3) 0.0178(3) -0.0023(2) 0.0051(3) -0.0032(2) S2 0.0153(3) 0.0213(3) 0.0164(3) -0.0038(2) 0.0022(3) -0.0030(2) C1 0.0291(15) 0.0159(13) 0.0224(15) 0.0024(10) 0.0003(12) 0.0049(11) C2 0.0218(14) 0.0192(13) 0.0226(14) 0.0011(11) 0.0017(11) 0.0065(11) C3 0.0169(13) 0.0260(14) 0.0165(13) -0.0049(10) 0.0012(10) 0.0043(11) C4 0.0179(12) 0.0179(12) 0.0160(13) -0.0011(10) 0.0002(10) 0.0041(10) C5 0.0186(12) 0.0199(12) 0.0136(12) -0.0055(10) 0.0000(10) 0.0001(10) C6 0.0231(13) 0.0189(13) 0.0140(13) -0.0039(10) 0.0047(10) -0.0032(10) C7 0.0199(13) 0.0192(13) 0.0137(12) -0.0012(10) -0.0007(10) -0.0017(10) C8 0.0147(12) 0.0252(14) 0.0209(14) 0.0029(11) 0.0057(10) 0.0005(10) C9 0.0183(13) 0.0222(14) 0.0252(14) 0.0046(11) 0.0037(11) -0.0061(11) C10 0.0226(13) 0.0173(13) 0.0185(13) 0.0029(10) 0.0039(11) -0.0031(10) C11 0.0370(17) 0.0304(17) 0.0274(16) -0.0007(13) 0.0032(13) 0.0030(14) Cl1 0.0231(3) 0.0308(4) 0.0197(3) 0.0061(3) 0.0031(3) 0.0009(3) O1 0.0264(11) 0.0315(12) 0.0307(12) 0.0012(9) 0.0107(9) -0.0001(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 Au1 S2 2.3000(8) 3_656 ? Au1 S1 2.3040(8) . ? Au1 Au1 3.1273(5) 3_656 ? Au1 Ni1 3.1782(6) . ? Ni1 N2 1.968(2) . ? Ni1 N1 1.985(2) . ? Ni1 S1 2.1800(8) . ? Ni1 S2 2.1921(9) . ? N1 C8 1.500(3) . ? N1 C2 1.504(3) . ? N1 C7 1.509(3) . ? N2 C4 1.498(3) . ? N2 C10 1.504(3) . ? N2 C5 1.511(3) . ? S1 C1 1.829(3) . ? S2 C3 1.827(3) . ? S2 Au1 2.3000(8) 3_656 ? C1 C2 1.505(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.501(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.523(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.530(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.507(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.510(4) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O1 1.413(3) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? O1 H1 0.8200 . ? 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 S2 Au1 S1 177.98(2) 3_656 . ? S2 Au1 Au1 87.601(19) 3_656 3_656 ? S1 Au1 Au1 90.47(2) . 3_656 ? S2 Au1 Ni1 134.891(19) 3_656 . ? S1 Au1 Ni1 43.308(18) . . ? Au1 Au1 Ni1 61.631(14) 3_656 . ? N2 Ni1 N1 90.47(8) . . ? N2 Ni1 S1 174.46(6) . . ? N1 Ni1 S1 90.44(6) . . ? N2 Ni1 S2 90.17(6) . . ? N1 Ni1 S2 175.23(7) . . ? S1 Ni1 S2 88.47(3) . . ? N2 Ni1 Au1 138.87(6) . . ? N1 Ni1 Au1 94.42(6) . . ? S1 Ni1 Au1 46.46(2) . . ? S2 Ni1 Au1 88.20(2) . . ? C8 N1 C2 104.81(19) . . ? C8 N1 C7 109.89(19) . . ? C2 N1 C7 110.0(2) . . ? C8 N1 Ni1 113.50(16) . . ? C2 N1 Ni1 111.96(15) . . ? C7 N1 Ni1 106.71(15) . . ? C4 N2 C10 104.50(19) . . ? C4 N2 C5 109.87(18) . . ? C10 N2 C5 110.40(19) . . ? C4 N2 Ni1 112.47(15) . . ? C10 N2 Ni1 113.53(15) . . ? C5 N2 Ni1 106.12(15) . . ? C1 S1 Ni1 98.35(8) . . ? C1 S1 Au1 106.11(10) . . ? Ni1 S1 Au1 90.23(3) . . ? C3 S2 Ni1 97.82(9) . . ? C3 S2 Au1 105.62(9) . 3_656 ? Ni1 S2 Au1 91.93(3) . 3_656 ? C2 C1 S1 108.48(18) . . ? C2 C1 H1A 110.0 . . ? S1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? S1 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N1 C2 C1 111.8(2) . . ? N1 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C4 C3 S2 107.84(17) . . ? C4 C3 H3A 110.1 . . ? S2 C3 H3A 110.1 . . ? C4 C3 H3B 110.1 . . ? S2 C3 H3B 110.1 . . ? H3A C3 H3B 108.5 . . ? N2 C4 C3 111.8(2) . . ? N2 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N2 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N2 C5 C6 113.8(2) . . ? N2 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N2 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? C5 C6 C7 118.6(2) . . ? C5 C6 H6A 107.7 . . ? C7 C6 H6A 107.7 . . ? C5 C6 H6B 107.7 . . ? C7 C6 H6B 107.7 . . ? H6A C6 H6B 107.1 . . ? N1 C7 C6 112.8(2) . . ? N1 C7 H7A 109.0 . . ? C6 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C6 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N1 C8 C9 114.7(2) . . ? N1 C8 H8A 108.6 . . ? C9 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 . . ? C9 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 C10 113.1(2) . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N2 C10 C9 114.3(2) . . ? N2 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? N2 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? O1 C11 H11A 109.5 . . ? O1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C11 O1 H1 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 S2 Au1 Ni1 N2 0.88(10) 3_656 . . . ? S1 Au1 Ni1 N2 -177.80(10) . . . . ? Au1 Au1 Ni1 N2 -51.89(9) 3_656 . . . ? S2 Au1 Ni1 N1 -94.93(7) 3_656 . . . ? S1 Au1 Ni1 N1 86.40(7) . . . . ? Au1 Au1 Ni1 N1 -147.69(6) 3_656 . . . ? S2 Au1 Ni1 S1 178.67(3) 3_656 . . . ? Au1 Au1 Ni1 S1 125.91(3) 3_656 . . . ? S2 Au1 Ni1 S2 89.07(3) 3_656 . . . ? S1 Au1 Ni1 S2 -89.61(3) . . . . ? Au1 Au1 Ni1 S2 36.304(19) 3_656 . . . ? N2 Ni1 N1 C8 -53.71(17) . . . . ? S1 Ni1 N1 C8 131.75(15) . . . . ? S2 Ni1 N1 C8 -151.4(6) . . . . ? Au1 Ni1 N1 C8 85.41(16) . . . . ? N2 Ni1 N1 C2 -172.14(17) . . . . ? S1 Ni1 N1 C2 13.33(16) . . . . ? S2 Ni1 N1 C2 90.1(7) . . . . ? Au1 Ni1 N1 C2 -33.02(16) . . . . ? N2 Ni1 N1 C7 67.48(15) . . . . ? S1 Ni1 N1 C7 -107.06(14) . . . . ? S2 Ni1 N1 C7 -30.2(8) . . . . ? Au1 Ni1 N1 C7 -153.40(14) . . . . ? N1 Ni1 N2 C4 172.68(16) . . . . ? S1 Ni1 N2 C4 -87.8(7) . . . . ? S2 Ni1 N2 C4 -12.05(15) . . . . ? Au1 Ni1 N2 C4 75.40(18) . . . . ? N1 Ni1 N2 C10 54.28(17) . . . . ? S1 Ni1 N2 C10 153.8(6) . . . . ? S2 Ni1 N2 C10 -130.45(16) . . . . ? Au1 Ni1 N2 C10 -43.0(2) . . . . ? N1 Ni1 N2 C5 -67.16(16) . . . . ? S1 Ni1 N2 C5 32.3(8) . . . . ? S2 Ni1 N2 C5 108.11(14) . . . . ? Au1 Ni1 N2 C5 -164.44(11) . . . . ? N2 Ni1 S1 C1 -88.8(7) . . . . ? N1 Ni1 S1 C1 10.64(12) . . . . ? S2 Ni1 S1 C1 -164.71(10) . . . . ? Au1 Ni1 S1 C1 106.32(10) . . . . ? N2 Ni1 S1 Au1 164.8(7) . . . . ? N1 Ni1 S1 Au1 -95.68(7) . . . . ? S2 Ni1 S1 Au1 88.96(3) . . . . ? S2 Au1 S1 C1 -126.4(6) 3_656 . . . ? Au1 Au1 S1 C1 -144.22(9) 3_656 . . . ? Ni1 Au1 S1 C1 -98.76(9) . . . . ? S2 Au1 S1 Ni1 -27.6(7) 3_656 . . . ? Au1 Au1 S1 Ni1 -45.45(2) 3_656 . . . ? N2 Ni1 S2 C3 -12.30(10) . . . . ? N1 Ni1 S2 C3 85.4(7) . . . . ? S1 Ni1 S2 C3 162.33(9) . . . . ? Au1 Ni1 S2 C3 -151.19(9) . . . . ? N2 Ni1 S2 Au1 93.76(6) . . . 3_656 ? N1 Ni1 S2 Au1 -168.5(7) . . . 3_656 ? S1 Ni1 S2 Au1 -91.62(3) . . . 3_656 ? Au1 Ni1 S2 Au1 -45.134(19) . . . 3_656 ? Ni1 S1 C1 C2 -33.52(19) . . . . ? Au1 S1 C1 C2 59.15(19) . . . . ? C8 N1 C2 C1 -163.2(2) . . . . ? C7 N1 C2 C1 78.8(3) . . . . ? Ni1 N1 C2 C1 -39.7(3) . . . . ? S1 C1 C2 N1 48.8(3) . . . . ? Ni1 S2 C3 C4 35.22(18) . . . . ? Au1 S2 C3 C4 -59.01(18) 3_656 . . . ? C10 N2 C4 C3 163.2(2) . . . . ? C5 N2 C4 C3 -78.4(2) . . . . ? Ni1 N2 C4 C3 39.6(2) . . . . ? S2 C3 C4 N2 -49.9(2) . . . . ? C4 N2 C5 C6 138.4(2) . . . . ? C10 N2 C5 C6 -106.9(2) . . . . ? Ni1 N2 C5 C6 16.6(2) . . . . ? N2 C5 C6 C7 53.5(3) . . . . ? C8 N1 C7 C6 107.2(2) . . . . ? C2 N1 C7 C6 -137.9(2) . . . . ? Ni1 N1 C7 C6 -16.2(2) . . . . ? C5 C6 C7 N1 -53.2(3) . . . . ? C2 N1 C8 C9 -174.5(2) . . . . ? C7 N1 C8 C9 -56.4(3) . . . . ? Ni1 N1 C8 C9 63.0(3) . . . . ? N1 C8 C9 C10 -59.9(3) . . . . ? C4 N2 C10 C9 172.9(2) . . . . ? C5 N2 C10 C9 54.8(3) . . . . ? Ni1 N2 C10 C9 -64.2(2) . . . . ? C8 C9 C10 N2 60.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.041 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.112 _vrf_PLAT_601_041213nibmedacoapph3inmeoh_0m-sr ; Problem: Structure Contains Solvent Accessible VOIDS of . 126 A**3 RESPONSE: Disordered solvent molecules were removed by squeeze operation in PLATON ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 956180' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_datax _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H37 Au Cl N2 Ni O P S2' _chemical_formula_weight 803.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.697(3) _cell_length_b 11.0833(19) _cell_length_c 16.059(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.978(2) _cell_angle_gamma 90.00 _cell_volume 2896.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 6.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5569 _exptl_absorpt_correction_T_max 0.6442 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33863 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0278 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 28.33 _reflns_number_total 7153 _reflns_number_gt 6609 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0238P)^2^+1.5429P] 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 7153 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0517 _refine_ls_wR_factor_gt 0.0508 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.002 _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 0.292581(6) 1.132112(8) 0.334933(6) 0.01511(4) Uani 1 1 d . . . Ni1 Ni 0.273756(18) 1.15525(3) 0.512750(19) 0.01277(6) Uani 1 1 d . . . S1 S 0.28039(4) 1.29799(5) 0.42065(4) 0.01767(12) Uani 1 1 d . . . S2 S 0.40592(4) 1.13280(6) 0.53366(5) 0.02520(15) Uani 1 1 d . . . N1 N 0.15223(12) 1.15688(18) 0.47835(13) 0.0149(4) Uani 1 1 d . . . N2 N 0.26984(13) 1.04679(18) 0.60923(13) 0.0178(4) Uani 1 1 d . . . P1 P 0.29994(4) 0.96443(5) 0.25757(4) 0.01297(12) Uani 1 1 d . . . C1 C 0.17161(17) 1.3397(2) 0.39595(18) 0.0222(5) Uani 1 1 d . . . H1A H 0.1609 1.3984 0.4386 0.027 Uiso 1 1 calc R . . H1B H 0.1566 1.3778 0.3388 0.027 Uiso 1 1 calc R . . C2 C 0.12128(15) 1.2279(2) 0.39756(16) 0.0196(5) Uani 1 1 d . . . H2A H 0.1237 1.1769 0.3476 0.024 Uiso 1 1 calc R . . H2B H 0.0632 1.2506 0.3934 0.024 Uiso 1 1 calc R . . C3 C 0.41415(17) 1.0017(3) 0.60336(18) 0.0277(6) Uani 1 1 d . . . H3A H 0.3996 0.9274 0.5692 0.033 Uiso 1 1 calc R . . H3B H 0.4710 0.9935 0.6378 0.033 Uiso 1 1 calc R . . C4 C 0.35536(17) 1.0217(3) 0.66055(17) 0.0265(6) Uani 1 1 d . . . H4A H 0.3745 1.0906 0.6991 0.032 Uiso 1 1 calc R . . H4B H 0.3545 0.9491 0.6963 0.032 Uiso 1 1 calc R . . C5 C 0.12355(15) 1.0298(2) 0.45684(15) 0.0179(5) Uani 1 1 d . . . H5A H 0.1504 0.9990 0.4121 0.021 Uiso 1 1 calc R . . H5B H 0.0636 1.0313 0.4324 0.021 Uiso 1 1 calc R . . C6 C 0.14058(16) 0.9427(2) 0.53123(17) 0.0225(5) Uani 1 1 d . . . H6A H 0.1105 0.9702 0.5743 0.027 Uiso 1 1 calc R . . H6B H 0.1187 0.8624 0.5107 0.027 Uiso 1 1 calc R . . C7 C 0.23030(17) 0.9297(2) 0.57382(16) 0.0225(5) Uani 1 1 d . . . H7A H 0.2600 0.8975 0.5318 0.027 Uiso 1 1 calc R . . H7B H 0.2360 0.8705 0.6209 0.027 Uiso 1 1 calc R . . C8 C 0.11601(16) 1.2084(2) 0.54833(17) 0.0224(5) Uani 1 1 d . . . H8A H 0.0697 1.1568 0.5556 0.027 Uiso 1 1 calc R . . H8B H 0.0938 1.2897 0.5310 0.027 Uiso 1 1 calc R . . C9 C 0.17782(17) 1.2181(3) 0.63376(17) 0.0240(6) Uani 1 1 d . . . H9A H 0.2200 1.2783 0.6278 0.029 Uiso 1 1 calc R . . H9B H 0.1488 1.2496 0.6766 0.029 Uiso 1 1 calc R . . C10 C 0.22158(17) 1.1019(3) 0.66859(16) 0.0239(6) Uani 1 1 d . . . H10A H 0.2594 1.1190 0.7242 0.029 Uiso 1 1 calc R . . H10B H 0.1803 1.0428 0.6787 0.029 Uiso 1 1 calc R . . C11 C 0.21233(14) 0.9418(2) 0.16981(14) 0.0147(5) Uani 1 1 d . . . C12 C 0.13357(15) 0.9655(2) 0.18236(17) 0.0202(5) Uani 1 1 d . . . H12 H 0.1268 0.9970 0.2354 0.024 Uiso 1 1 calc R . . C13 C 0.06527(16) 0.9426(3) 0.11698(18) 0.0256(6) Uani 1 1 d . . . H13 H 0.0117 0.9578 0.1255 0.031 Uiso 1 1 calc R . . C14 C 0.07502(16) 0.8978(2) 0.03948(18) 0.0235(5) Uani 1 1 d . . . H14 H 0.0280 0.8818 -0.0048 0.028 Uiso 1 1 calc R . . C15 C 0.15305(17) 0.8759(2) 0.02605(17) 0.0204(5) Uani 1 1 d . . . H15 H 0.1595 0.8462 -0.0275 0.025 Uiso 1 1 calc R . . C16 C 0.22166(15) 0.8978(2) 0.09124(16) 0.0173(5) Uani 1 1 d . . . H16 H 0.2751 0.8828 0.0823 0.021 Uiso 1 1 calc R . . C17 C 0.38885(14) 0.9544(2) 0.21039(15) 0.0148(4) Uani 1 1 d . . . C18 C 0.43247(15) 0.8469(2) 0.21050(16) 0.0184(5) Uani 1 1 d . . . H18 H 0.4182 0.7777 0.2390 0.022 Uiso 1 1 calc R . . C19 C 0.49688(16) 0.8413(3) 0.16883(17) 0.0228(5) Uani 1 1 d . . . H19 H 0.5267 0.7683 0.1687 0.027 Uiso 1 1 calc R . . C20 C 0.51762(16) 0.9423(3) 0.12746(18) 0.0264(6) Uani 1 1 d . . . H20 H 0.5615 0.9382 0.0988 0.032 Uiso 1 1 calc R . . C21 C 0.47465(17) 1.0493(3) 0.12764(18) 0.0279(6) Uani 1 1 d . . . H21 H 0.4892 1.1183 0.0992 0.033 Uiso 1 1 calc R . . C22 C 0.41057(16) 1.0558(2) 0.16912(17) 0.0213(5) Uani 1 1 d . . . H22 H 0.3814 1.1293 0.1695 0.026 Uiso 1 1 calc R . . C23 C 0.30526(14) 0.8312(2) 0.32387(15) 0.0147(5) Uani 1 1 d . . . C24 C 0.36797(15) 0.8261(2) 0.39785(16) 0.0178(5) Uani 1 1 d . . . H24 H 0.4038 0.8930 0.4133 0.021 Uiso 1 1 calc R . . C25 C 0.37799(16) 0.7242(2) 0.44853(16) 0.0218(5) Uani 1 1 d . . . H25 H 0.4213 0.7203 0.4982 0.026 Uiso 1 1 calc R . . C26 C 0.32444(19) 0.6271(2) 0.42656(18) 0.0245(6) Uani 1 1 d . . . H26 H 0.3317 0.5564 0.4609 0.029 Uiso 1 1 calc R . . C27 C 0.26041(19) 0.6334(2) 0.35447(18) 0.0243(6) Uani 1 1 d . . . H27 H 0.2232 0.5677 0.3404 0.029 Uiso 1 1 calc R . . C28 C 0.25068(16) 0.7352(2) 0.30314(16) 0.0191(5) Uani 1 1 d . . . H28 H 0.2069 0.7395 0.2539 0.023 Uiso 1 1 calc R . . Cl1 Cl 0.94928(4) 0.04075(6) 0.26735(4) 0.02701(14) Uani 1 1 d . . . H1 H 0.984(3) 0.338(4) 0.179(3) 0.061(15) Uiso 1 1 d . . . H2 H 0.960(3) 0.227(4) 0.185(3) 0.063(14) Uiso 1 1 d . . . O1 O 0.96263(19) 0.2818(3) 0.15283(17) 0.0503(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.01958(5) 0.01068(5) 0.01551(5) -0.00020(3) 0.00489(4) -0.00105(3) Ni1 0.01334(14) 0.00999(14) 0.01381(15) -0.00056(11) 0.00059(11) -0.00159(11) S1 0.0233(3) 0.0096(3) 0.0202(3) -0.0007(2) 0.0051(2) -0.0033(2) S2 0.0149(3) 0.0271(4) 0.0315(4) 0.0022(3) 0.0006(3) -0.0010(2) N1 0.0152(9) 0.0128(9) 0.0156(10) -0.0020(8) 0.0012(8) 0.0002(8) N2 0.0218(10) 0.0151(10) 0.0143(10) -0.0002(8) -0.0009(8) -0.0034(8) P1 0.0143(3) 0.0117(3) 0.0131(3) 0.0000(2) 0.0036(2) -0.0006(2) C1 0.0279(14) 0.0123(12) 0.0248(13) 0.0014(10) 0.0024(11) 0.0047(10) C2 0.0198(12) 0.0180(12) 0.0183(12) 0.0011(9) -0.0015(10) 0.0037(10) C3 0.0237(14) 0.0230(14) 0.0300(15) -0.0001(11) -0.0071(11) 0.0050(11) C4 0.0277(14) 0.0259(14) 0.0196(13) 0.0025(11) -0.0079(11) 0.0007(11) C5 0.0182(12) 0.0175(12) 0.0159(12) -0.0021(9) -0.0004(9) -0.0059(9) C6 0.0286(14) 0.0165(12) 0.0210(13) -0.0010(10) 0.0024(11) -0.0098(10) C7 0.0345(15) 0.0115(12) 0.0198(13) 0.0016(9) 0.0023(11) -0.0043(10) C8 0.0207(12) 0.0239(13) 0.0243(13) -0.0048(11) 0.0088(11) 0.0026(10) C9 0.0277(14) 0.0249(14) 0.0210(13) -0.0071(11) 0.0086(11) -0.0022(11) C10 0.0304(14) 0.0263(14) 0.0147(12) -0.0036(10) 0.0048(11) -0.0044(11) C11 0.0150(11) 0.0130(11) 0.0155(11) 0.0019(8) 0.0020(9) -0.0017(8) C12 0.0195(12) 0.0216(13) 0.0205(12) 0.0003(10) 0.0065(10) 0.0017(10) C13 0.0166(12) 0.0293(15) 0.0304(15) 0.0025(12) 0.0043(11) 0.0005(11) C14 0.0197(12) 0.0214(13) 0.0258(14) 0.0029(11) -0.0027(11) -0.0040(10) C15 0.0240(13) 0.0194(13) 0.0175(12) 0.0003(9) 0.0036(10) -0.0032(10) C16 0.0170(11) 0.0174(12) 0.0179(12) -0.0002(9) 0.0046(9) -0.0018(9) C17 0.0132(10) 0.0180(12) 0.0128(11) 0.0003(9) 0.0021(9) -0.0023(9) C18 0.0188(12) 0.0180(12) 0.0183(12) -0.0003(9) 0.0041(10) -0.0013(9) C19 0.0185(12) 0.0284(14) 0.0203(13) -0.0052(10) 0.0021(10) 0.0005(10) C20 0.0180(12) 0.0392(17) 0.0233(13) -0.0020(12) 0.0077(11) -0.0058(11) C21 0.0246(13) 0.0319(15) 0.0297(15) 0.0073(12) 0.0112(12) -0.0063(12) C22 0.0198(12) 0.0187(12) 0.0253(13) 0.0029(10) 0.0044(10) -0.0018(10) C23 0.0170(11) 0.0126(11) 0.0157(11) 0.0003(9) 0.0063(9) 0.0012(9) C24 0.0182(12) 0.0179(12) 0.0174(12) -0.0001(9) 0.0043(10) 0.0003(9) C25 0.0247(13) 0.0226(13) 0.0188(12) 0.0042(10) 0.0061(10) 0.0068(10) C26 0.0408(16) 0.0149(13) 0.0229(13) 0.0051(10) 0.0181(12) 0.0064(11) C27 0.0365(15) 0.0152(13) 0.0252(14) 0.0014(10) 0.0152(12) -0.0019(10) C28 0.0225(12) 0.0174(12) 0.0181(12) -0.0010(9) 0.0061(10) -0.0033(10) Cl1 0.0244(3) 0.0318(4) 0.0239(3) -0.0028(3) 0.0034(3) -0.0041(3) O1 0.0711(19) 0.0481(17) 0.0318(14) 0.0028(13) 0.0117(13) -0.0188(15) _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 2.2542(7) . ? Au1 S1 2.3329(7) . ? Au1 Ni1 2.9533(6) . ? Ni1 N2 1.974(2) . ? Ni1 N1 1.980(2) . ? Ni1 S2 2.1706(8) . ? Ni1 S1 2.1854(7) . ? S1 C1 1.829(3) . ? S2 C3 1.820(3) . ? N1 C5 1.502(3) . ? N1 C8 1.503(3) . ? N1 C2 1.506(3) . ? N2 C4 1.506(3) . ? N2 C7 1.508(3) . ? N2 C10 1.509(3) . ? P1 C11 1.807(2) . ? P1 C23 1.811(2) . ? P1 C17 1.815(2) . ? C1 C2 1.501(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.504(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.508(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.524(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.523(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.394(3) . ? C11 C12 1.399(3) . ? C12 C13 1.389(4) . ? C12 H12 0.9500 . ? C13 C14 1.383(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 C16 1.389(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.393(3) . ? C17 C18 1.397(3) . ? C18 C19 1.390(4) . ? C18 H18 0.9500 . ? C19 C20 1.385(4) . ? C19 H19 0.9500 . ? C20 C21 1.387(4) . ? C20 H20 0.9500 . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C28 1.392(3) . ? C23 C24 1.397(3) . ? C24 C25 1.380(3) . ? C24 H24 0.9500 . ? C25 C26 1.393(4) . ? C25 H25 0.9500 . ? C26 C27 1.390(4) . ? C26 H26 0.9500 . ? C27 C28 1.386(3) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? O1 H1 0.79(5) . ? O1 H2 0.81(5) . ? 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 S1 176.16(2) . . ? P1 Au1 Ni1 129.446(17) . . ? S1 Au1 Ni1 47.052(17) . . ? N2 Ni1 N1 90.69(9) . . ? N2 Ni1 S2 91.18(7) . . ? N1 Ni1 S2 170.72(6) . . ? N2 Ni1 S1 171.05(6) . . ? N1 Ni1 S1 90.52(6) . . ? S2 Ni1 S1 89.05(3) . . ? N2 Ni1 Au1 137.36(6) . . ? N1 Ni1 Au1 93.21(6) . . ? S2 Ni1 Au1 79.30(2) . . ? S1 Ni1 Au1 51.385(18) . . ? C1 S1 Ni1 97.53(9) . . ? C1 S1 Au1 106.57(9) . . ? Ni1 S1 Au1 81.56(2) . . ? C3 S2 Ni1 96.92(9) . . ? C5 N1 C8 111.53(19) . . ? C5 N1 C2 105.16(18) . . ? C8 N1 C2 109.14(19) . . ? C5 N1 Ni1 108.02(15) . . ? C8 N1 Ni1 110.74(15) . . ? C2 N1 Ni1 112.15(15) . . ? C4 N2 C7 109.2(2) . . ? C4 N2 C10 107.7(2) . . ? C7 N2 C10 109.6(2) . . ? C4 N2 Ni1 110.35(16) . . ? C7 N2 Ni1 108.47(15) . . ? C10 N2 Ni1 111.47(16) . . ? C11 P1 C23 105.64(11) . . ? C11 P1 C17 105.11(11) . . ? C23 P1 C17 105.00(11) . . ? C11 P1 Au1 114.19(8) . . ? C23 P1 Au1 110.46(8) . . ? C17 P1 Au1 115.56(8) . . ? C2 C1 S1 108.65(17) . . ? C2 C1 H1A 110.0 . . ? S1 C1 H1A 110.0 . . ? C2 C1 H1B 110.0 . . ? S1 C1 H1B 110.0 . . ? H1A C1 H1B 108.3 . . ? C1 C2 N1 111.2(2) . . ? C1 C2 H2A 109.4 . . ? N1 C2 H2A 109.4 . . ? C1 C2 H2B 109.4 . . ? N1 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C4 C3 S2 106.78(19) . . ? C4 C3 H3A 110.4 . . ? S2 C3 H3A 110.4 . . ? C4 C3 H3B 110.4 . . ? S2 C3 H3B 110.4 . . ? H3A C3 H3B 108.6 . . ? C3 C4 N2 111.2(2) . . ? C3 C4 H4A 109.4 . . ? N2 C4 H4A 109.4 . . ? C3 C4 H4B 109.4 . . ? N2 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N1 C5 C6 115.0(2) . . ? N1 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? N1 C5 H5B 108.5 . . ? C6 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? C7 C6 C5 114.2(2) . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? C5 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 N2 113.3(2) . . ? C6 C7 H7A 108.9 . . ? N2 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? N2 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C9 113.3(2) . . ? N1 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N1 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C10 C9 C8 116.3(2) . . ? C10 C9 H9A 108.2 . . ? C8 C9 H9A 108.2 . . ? C10 C9 H9B 108.2 . . ? C8 C9 H9B 108.2 . . ? H9A C9 H9B 107.4 . . ? N2 C10 C9 113.0(2) . . ? N2 C10 H10A 109.0 . . ? C9 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? C9 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C16 C11 C12 119.7(2) . . ? C16 C11 P1 121.29(18) . . ? C12 C11 P1 118.96(18) . . ? C13 C12 C11 119.7(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C14 C13 C12 120.2(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.4(2) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C11 120.2(2) . . ? C15 C16 H16 119.9 . . ? C11 C16 H16 119.9 . . ? C22 C17 C18 119.8(2) . . ? C22 C17 P1 118.28(19) . . ? C18 C17 P1 121.80(18) . . ? C19 C18 C17 119.8(2) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C18 120.0(3) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.3(2) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C17 120.0(2) . . ? C21 C22 H22 120.0 . . ? C17 C22 H22 120.0 . . ? C28 C23 C24 119.8(2) . . ? C28 C23 P1 122.66(18) . . ? C24 C23 P1 117.49(18) . . ? C25 C24 C23 120.2(2) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.8(2) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 120.1(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 120.1(3) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C23 119.8(2) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? H1 O1 H2 109(4) . . ? 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 P1 Au1 Ni1 N2 4.69(9) . . . . ? S1 Au1 Ni1 N2 -177.39(9) . . . . ? P1 Au1 Ni1 N1 -89.82(6) . . . . ? S1 Au1 Ni1 N1 88.10(6) . . . . ? P1 Au1 Ni1 S2 84.65(3) . . . . ? S1 Au1 Ni1 S2 -97.43(3) . . . . ? P1 Au1 Ni1 S1 -177.92(3) . . . . ? N2 Ni1 S1 C1 -85.7(4) . . . . ? N1 Ni1 S1 C1 12.05(10) . . . . ? S2 Ni1 S1 C1 -177.23(9) . . . . ? Au1 Ni1 S1 C1 105.74(9) . . . . ? N2 Ni1 S1 Au1 168.5(4) . . . . ? N1 Ni1 S1 Au1 -93.69(6) . . . . ? S2 Ni1 S1 Au1 77.04(2) . . . . ? P1 Au1 S1 C1 -70.6(3) . . . . ? Ni1 Au1 S1 C1 -95.40(9) . . . . ? P1 Au1 S1 Ni1 24.8(3) . . . . ? N2 Ni1 S2 C3 14.69(11) . . . . ? N1 Ni1 S2 C3 -86.8(4) . . . . ? S1 Ni1 S2 C3 -174.26(10) . . . . ? Au1 Ni1 S2 C3 -123.47(10) . . . . ? N2 Ni1 N1 C5 -61.13(15) . . . . ? S2 Ni1 N1 C5 40.4(5) . . . . ? S1 Ni1 N1 C5 127.74(14) . . . . ? Au1 Ni1 N1 C5 76.39(14) . . . . ? N2 Ni1 N1 C8 61.27(17) . . . . ? S2 Ni1 N1 C8 162.8(3) . . . . ? S1 Ni1 N1 C8 -109.86(16) . . . . ? Au1 Ni1 N1 C8 -161.21(15) . . . . ? N2 Ni1 N1 C2 -176.55(16) . . . . ? S2 Ni1 N1 C2 -75.0(4) . . . . ? S1 Ni1 N1 C2 12.32(15) . . . . ? Au1 Ni1 N1 C2 -39.03(15) . . . . ? N1 Ni1 N2 C4 -177.80(17) . . . . ? S2 Ni1 N2 C4 11.30(16) . . . . ? S1 Ni1 N2 C4 -80.1(5) . . . . ? Au1 Ni1 N2 C4 86.71(17) . . . . ? N1 Ni1 N2 C7 62.66(17) . . . . ? S2 Ni1 N2 C7 -108.25(16) . . . . ? S1 Ni1 N2 C7 160.4(3) . . . . ? Au1 Ni1 N2 C7 -32.8(2) . . . . ? N1 Ni1 N2 C10 -58.14(17) . . . . ? S2 Ni1 N2 C10 130.95(16) . . . . ? S1 Ni1 N2 C10 39.6(5) . . . . ? Au1 Ni1 N2 C10 -153.63(13) . . . . ? S1 Au1 P1 C11 88.5(3) . . . . ? Ni1 Au1 P1 C11 111.89(8) . . . . ? S1 Au1 P1 C23 -30.4(4) . . . . ? Ni1 Au1 P1 C23 -6.99(9) . . . . ? S1 Au1 P1 C17 -149.4(3) . . . . ? Ni1 Au1 P1 C17 -125.98(9) . . . . ? Ni1 S1 C1 C2 -35.47(18) . . . . ? Au1 S1 C1 C2 47.93(19) . . . . ? S1 C1 C2 N1 50.1(2) . . . . ? C5 N1 C2 C1 -156.7(2) . . . . ? C8 N1 C2 C1 83.6(2) . . . . ? Ni1 N1 C2 C1 -39.5(2) . . . . ? Ni1 S2 C3 C4 -39.09(18) . . . . ? S2 C3 C4 N2 54.4(3) . . . . ? C7 N2 C4 C3 77.9(3) . . . . ? C10 N2 C4 C3 -163.2(2) . . . . ? Ni1 N2 C4 C3 -41.3(3) . . . . ? C8 N1 C5 C6 -56.3(3) . . . . ? C2 N1 C5 C6 -174.5(2) . . . . ? Ni1 N1 C5 C6 65.6(2) . . . . ? N1 C5 C6 C7 -59.3(3) . . . . ? C5 C6 C7 N2 59.5(3) . . . . ? C4 N2 C7 C6 172.3(2) . . . . ? C10 N2 C7 C6 54.5(3) . . . . ? Ni1 N2 C7 C6 -67.4(2) . . . . ? C5 N1 C8 C9 106.6(2) . . . . ? C2 N1 C8 C9 -137.6(2) . . . . ? Ni1 N1 C8 C9 -13.7(3) . . . . ? N1 C8 C9 C10 -55.9(3) . . . . ? C4 N2 C10 C9 129.4(2) . . . . ? C7 N2 C10 C9 -112.0(2) . . . . ? Ni1 N2 C10 C9 8.2(3) . . . . ? C8 C9 C10 N2 59.4(3) . . . . ? C23 P1 C11 C16 -97.5(2) . . . . ? C17 P1 C11 C16 13.3(2) . . . . ? Au1 P1 C11 C16 140.97(18) . . . . ? C23 P1 C11 C12 80.5(2) . . . . ? C17 P1 C11 C12 -168.7(2) . . . . ? Au1 P1 C11 C12 -41.1(2) . . . . ? C16 C11 C12 C13 1.3(4) . . . . ? P1 C11 C12 C13 -176.7(2) . . . . ? C11 C12 C13 C14 -0.6(4) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? C14 C15 C16 C11 -0.2(4) . . . . ? C12 C11 C16 C15 -0.9(4) . . . . ? P1 C11 C16 C15 177.04(19) . . . . ? C11 P1 C17 C22 81.2(2) . . . . ? C23 P1 C17 C22 -167.7(2) . . . . ? Au1 P1 C17 C22 -45.7(2) . . . . ? C11 P1 C17 C18 -95.3(2) . . . . ? C23 P1 C17 C18 15.9(2) . . . . ? Au1 P1 C17 C18 137.85(18) . . . . ? C22 C17 C18 C19 -0.5(4) . . . . ? P1 C17 C18 C19 175.86(19) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C18 C19 C20 C21 0.3(4) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C20 C21 C22 C17 -0.4(4) . . . . ? C18 C17 C22 C21 0.7(4) . . . . ? P1 C17 C22 C21 -175.8(2) . . . . ? C11 P1 C23 C28 1.7(2) . . . . ? C17 P1 C23 C28 -109.1(2) . . . . ? Au1 P1 C23 C28 125.64(19) . . . . ? C11 P1 C23 C24 -179.26(18) . . . . ? C17 P1 C23 C24 69.9(2) . . . . ? Au1 P1 C23 C24 -55.3(2) . . . . ? C28 C23 C24 C25 2.6(4) . . . . ? P1 C23 C24 C25 -176.46(19) . . . . ? C23 C24 C25 C26 -1.1(4) . . . . ? C24 C25 C26 C27 -0.9(4) . . . . ? C25 C26 C27 C28 1.4(4) . . . . ? C26 C27 C28 C23 0.1(4) . . . . ? C24 C23 C28 C27 -2.1(4) . . . . ? P1 C23 C28 C27 176.95(19) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.813 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.129 _database_code_depnum_ccdc_archive 'CCDC 956181' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_data_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 Au2 N6 Ni2 O4 S4' _chemical_formula_weight 1180.38 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.308(2) _cell_length_b 24.096(6) _cell_length_c 10.191(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.431(3) _cell_angle_gamma 90.00 _cell_volume 1911.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.051 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 8.880 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1759 _exptl_absorpt_correction_T_max 0.5369 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22917 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.64 _reflns_number_total 4844 _reflns_number_gt 3874 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0185P)^2^+1.4178P] 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 4844 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0418 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0545 _refine_ls_wR_factor_gt 0.0501 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.006 _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 0.356784(19) 1.011140(6) 0.562797(15) 0.02202(5) Uani 1 1 d . . . Ni1 Ni 0.63878(6) 0.917071(19) 0.71338(5) 0.01976(11) Uani 1 1 d . . . S1 S 0.52793(12) 0.98771(4) 0.78633(10) 0.02207(19) Uani 1 1 d . . . S2 S 0.83053(12) 0.96319(4) 0.65298(10) 0.0236(2) Uani 1 1 d . . . N1 N 0.4930(4) 0.87129(13) 0.7658(3) 0.0250(7) Uani 1 1 d . . . N2 N 0.7113(4) 0.85270(13) 0.6512(3) 0.0267(7) Uani 1 1 d . . . N3 N 0.0638(4) 0.85113(12) 0.1955(3) 0.0188(6) Uani 1 1 d . . . O1 O 0.3088(4) 0.85603(12) 0.8850(3) 0.0338(7) Uani 1 1 d . . . O2 O 0.8526(4) 0.81192(12) 0.5190(3) 0.0352(7) Uani 1 1 d . . . C1 C 0.3847(5) 0.94912(16) 0.8550(4) 0.0259(9) Uani 1 1 d . . . H1A H 0.4154 0.9572 0.9540 0.031 Uiso 1 1 calc R . . H1B H 0.2676 0.9617 0.8080 0.031 Uiso 1 1 calc R . . C2 C 0.3928(5) 0.88721(16) 0.8356(4) 0.0249(8) Uani 1 1 d . . . C3 C 0.9389(5) 0.90254(17) 0.6144(4) 0.0279(9) Uani 1 1 d . . . H3A H 0.9694 0.9102 0.5326 0.033 Uiso 1 1 calc R . . H3B H 1.0441 0.8957 0.6927 0.033 Uiso 1 1 calc R . . C4 C 0.8265(5) 0.85112(17) 0.5876(4) 0.0240(8) Uani 1 1 d . . . C5 C 0.6011(6) 0.80455(17) 0.6415(5) 0.0333(10) Uani 1 1 d . . . H5A H 0.6685 0.7707 0.6586 0.040 Uiso 1 1 calc R . . H5B H 0.5138 0.8024 0.5489 0.040 Uiso 1 1 calc R . . C6 C 0.5181(6) 0.81187(17) 0.7518(5) 0.0320(10) Uani 1 1 d . . . H6A H 0.4086 0.7927 0.7235 0.038 Uiso 1 1 calc R . . H6B H 0.5916 0.7966 0.8406 0.038 Uiso 1 1 calc R . . C7 C 0.2345(5) 0.87010(17) 0.2985(4) 0.0280(9) Uani 1 1 d . . . H7A H 0.2432 0.8578 0.3914 0.034 Uiso 1 1 calc R . . H7B H 0.2366 0.9104 0.2993 0.034 Uiso 1 1 calc R . . C8 C 0.3902(5) 0.8494(2) 0.2687(5) 0.0445(12) Uani 1 1 d . . . H8A H 0.3945 0.8096 0.2744 0.067 Uiso 1 1 calc R . . H8B H 0.4924 0.8646 0.3363 0.067 Uiso 1 1 calc R . . H8C H 0.3826 0.8608 0.1764 0.067 Uiso 1 1 calc R . . C9 C 0.0510(5) 0.78844(16) 0.1901(4) 0.0278(9) Uani 1 1 d . . . H9A H -0.0621 0.7784 0.1259 0.033 Uiso 1 1 calc R . . H9B H 0.1343 0.7743 0.1515 0.033 Uiso 1 1 calc R . . C10 C 0.0797(6) 0.75961(17) 0.3282(4) 0.0323(10) Uani 1 1 d . . . H10A H 0.1928 0.7681 0.3922 0.048 Uiso 1 1 calc R . . H10B H 0.0688 0.7202 0.3135 0.048 Uiso 1 1 calc R . . H10C H -0.0042 0.7722 0.3666 0.048 Uiso 1 1 calc R . . C11 C 0.0413(5) 0.87031(16) 0.0484(4) 0.0249(8) Uani 1 1 d . . . H11A H 0.1322 0.8543 0.0213 0.030 Uiso 1 1 calc R . . H11B H -0.0671 0.8561 -0.0153 0.030 Uiso 1 1 calc R . . C12 C 0.0439(5) 0.93270(17) 0.0313(4) 0.0300(9) Uani 1 1 d . . . H12A H -0.0499 0.9489 0.0523 0.045 Uiso 1 1 calc R . . H12B H 0.0327 0.9415 -0.0634 0.045 Uiso 1 1 calc R . . H12C H 0.1504 0.9473 0.0941 0.045 Uiso 1 1 calc R . . C13 C -0.0724(5) 0.87608(17) 0.2451(4) 0.0300(9) Uani 1 1 d . . . H13A H -0.0622 0.8594 0.3343 0.036 Uiso 1 1 calc R . . H13B H -0.0492 0.9154 0.2611 0.036 Uiso 1 1 calc R . . C14 C -0.2554(6) 0.8690(2) 0.1462(5) 0.0473(13) Uani 1 1 d . . . H14A H -0.2681 0.8859 0.0578 0.071 Uiso 1 1 calc R . . H14B H -0.3323 0.8865 0.1853 0.071 Uiso 1 1 calc R . . H14C H -0.2821 0.8302 0.1326 0.071 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 0.02426(8) 0.02068(8) 0.02145(8) -0.00039(6) 0.00840(6) -0.00104(7) Ni1 0.0206(2) 0.0191(2) 0.0202(2) -0.00073(19) 0.0079(2) -0.00054(19) S1 0.0238(5) 0.0214(5) 0.0214(5) -0.0024(4) 0.0083(4) -0.0022(4) S2 0.0229(5) 0.0266(5) 0.0214(5) -0.0007(4) 0.0077(4) -0.0026(4) N1 0.0300(18) 0.0181(17) 0.0285(18) -0.0011(14) 0.0121(15) -0.0014(14) N2 0.0288(19) 0.0226(18) 0.0315(19) 0.0028(14) 0.0140(16) 0.0038(14) N3 0.0198(16) 0.0186(16) 0.0202(16) -0.0017(12) 0.0096(13) -0.0013(13) O1 0.0346(17) 0.0347(17) 0.0400(18) 0.0013(14) 0.0227(14) -0.0082(14) O2 0.0462(19) 0.0303(17) 0.0338(17) 0.0001(13) 0.0201(15) 0.0139(14) C1 0.026(2) 0.030(2) 0.026(2) -0.0012(17) 0.0137(17) -0.0006(17) C2 0.023(2) 0.026(2) 0.025(2) 0.0006(16) 0.0078(17) 0.0000(16) C3 0.021(2) 0.035(2) 0.026(2) 0.0035(18) 0.0075(17) 0.0064(18) C4 0.026(2) 0.028(2) 0.0185(19) 0.0051(16) 0.0074(17) 0.0086(17) C5 0.039(3) 0.024(2) 0.038(2) -0.0010(19) 0.016(2) -0.0001(19) C6 0.035(2) 0.024(2) 0.042(3) 0.0036(18) 0.019(2) 0.0011(18) C7 0.029(2) 0.026(2) 0.023(2) 0.0004(17) 0.0010(18) -0.0035(17) C8 0.023(2) 0.058(3) 0.049(3) 0.010(2) 0.007(2) -0.003(2) C9 0.037(2) 0.018(2) 0.030(2) -0.0031(16) 0.0146(19) -0.0015(17) C10 0.046(3) 0.019(2) 0.036(2) 0.0062(18) 0.019(2) 0.0026(19) C11 0.027(2) 0.027(2) 0.0214(19) -0.0015(16) 0.0098(17) -0.0028(17) C12 0.032(2) 0.031(2) 0.026(2) 0.0047(18) 0.0089(18) -0.0063(19) C13 0.034(2) 0.029(2) 0.034(2) 0.0017(18) 0.021(2) 0.0057(18) C14 0.027(2) 0.059(3) 0.059(3) 0.004(3) 0.019(2) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Au1 S2 2.2914(11) 3_676 ? Au1 S1 2.2952(11) . ? Au1 Au1 3.1169(7) 3_676 ? Ni1 N1 1.849(3) . ? Ni1 N2 1.854(3) . ? Ni1 S1 2.1854(11) . ? Ni1 S2 2.1991(11) . ? S1 C1 1.831(4) . ? S2 C3 1.830(4) . ? S2 Au1 2.2914(11) 3_676 ? N1 C2 1.327(5) . ? N1 C6 1.461(5) . ? N2 C4 1.330(5) . ? N2 C5 1.460(5) . ? N3 C7 1.510(5) . ? N3 C9 1.514(5) . ? N3 C13 1.515(5) . ? N3 C11 1.517(4) . ? O1 C2 1.245(4) . ? O2 C4 1.239(5) . ? C1 C2 1.510(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C3 C4 1.518(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C5 C6 1.521(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.513(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.511(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.514(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.512(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 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 S2 Au1 S1 175.35(3) 3_676 . ? S2 Au1 Au1 90.72(3) 3_676 3_676 ? S1 Au1 Au1 93.90(3) . 3_676 ? N1 Ni1 N2 85.61(14) . . ? N1 Ni1 S1 88.29(10) . . ? N2 Ni1 S1 173.59(11) . . ? N1 Ni1 S2 173.52(11) . . ? N2 Ni1 S2 88.48(11) . . ? S1 Ni1 S2 97.70(4) . . ? C1 S1 Ni1 98.15(13) . . ? C1 S1 Au1 104.13(14) . . ? Ni1 S1 Au1 92.44(4) . . ? C3 S2 Ni1 96.61(14) . . ? C3 S2 Au1 103.27(13) . 3_676 ? Ni1 S2 Au1 95.12(4) . 3_676 ? C2 N1 C6 118.2(3) . . ? C2 N1 Ni1 125.4(3) . . ? C6 N1 Ni1 115.3(2) . . ? C4 N2 C5 119.0(3) . . ? C4 N2 Ni1 124.4(3) . . ? C5 N2 Ni1 114.7(3) . . ? C7 N3 C9 111.4(3) . . ? C7 N3 C13 106.1(3) . . ? C9 N3 C13 110.9(3) . . ? C7 N3 C11 110.9(3) . . ? C9 N3 C11 106.6(3) . . ? C13 N3 C11 111.1(3) . . ? C2 C1 S1 112.8(3) . . ? C2 C1 H1A 109.0 . . ? S1 C1 H1A 109.0 . . ? C2 C1 H1B 109.0 . . ? S1 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O1 C2 N1 126.0(4) . . ? O1 C2 C1 119.1(3) . . ? N1 C2 C1 114.9(3) . . ? C4 C3 S2 111.9(3) . . ? C4 C3 H3A 109.2 . . ? S2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? S2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? O2 C4 N2 126.5(4) . . ? O2 C4 C3 120.4(4) . . ? N2 C4 C3 113.0(3) . . ? N2 C5 C6 107.1(3) . . ? N2 C5 H5A 110.3 . . ? C6 C5 H5A 110.3 . . ? N2 C5 H5B 110.3 . . ? C6 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? N1 C6 C5 107.6(3) . . ? N1 C6 H6A 110.2 . . ? C5 C6 H6A 110.2 . . ? N1 C6 H6B 110.2 . . ? C5 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? N3 C7 C8 115.0(3) . . ? N3 C7 H7A 108.5 . . ? C8 C7 H7A 108.5 . . ? N3 C7 H7B 108.5 . . ? C8 C7 H7B 108.5 . . ? H7A C7 H7B 107.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C10 C9 N3 116.0(3) . . ? C10 C9 H9A 108.3 . . ? N3 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? N3 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 N3 114.5(3) . . ? C12 C11 H11A 108.6 . . ? N3 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? N3 C11 H11B 108.6 . . ? H11A C11 H11B 107.6 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 N3 115.3(3) . . ? C14 C13 H13A 108.4 . . ? N3 C13 H13A 108.4 . . ? C14 C13 H13B 108.4 . . ? N3 C13 H13B 108.4 . . ? H13A C13 H13B 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 S1 C1 3.49(17) . . . . ? N2 Ni1 S1 C1 21.3(10) . . . . ? S2 Ni1 S1 C1 -174.03(13) . . . . ? N1 Ni1 S1 Au1 -101.17(11) . . . . ? N2 Ni1 S1 Au1 -83.4(10) . . . . ? S2 Ni1 S1 Au1 81.32(4) . . . . ? S2 Au1 S1 C1 46.8(5) 3_676 . . . ? Au1 Au1 S1 C1 -140.28(13) 3_676 . . . ? S2 Au1 S1 Ni1 145.9(4) 3_676 . . . ? Au1 Au1 S1 Ni1 -41.24(3) 3_676 . . . ? N1 Ni1 S2 C3 15.6(10) . . . . ? N2 Ni1 S2 C3 -8.66(17) . . . . ? S1 Ni1 S2 C3 173.04(13) . . . . ? N1 Ni1 S2 Au1 119.6(9) . . . 3_676 ? N2 Ni1 S2 Au1 95.37(11) . . . 3_676 ? S1 Ni1 S2 Au1 -82.93(4) . . . 3_676 ? N2 Ni1 N1 C2 174.6(3) . . . . ? S1 Ni1 N1 C2 -7.3(3) . . . . ? S2 Ni1 N1 C2 150.3(8) . . . . ? N2 Ni1 N1 C6 7.1(3) . . . . ? S1 Ni1 N1 C6 -174.9(3) . . . . ? S2 Ni1 N1 C6 -17.3(11) . . . . ? N1 Ni1 N2 C4 177.6(3) . . . . ? S1 Ni1 N2 C4 159.7(8) . . . . ? S2 Ni1 N2 C4 -5.1(3) . . . . ? N1 Ni1 N2 C5 13.6(3) . . . . ? S1 Ni1 N2 C5 -4.3(12) . . . . ? S2 Ni1 N2 C5 -169.1(3) . . . . ? Ni1 S1 C1 C2 -0.8(3) . . . . ? Au1 S1 C1 C2 93.8(3) . . . . ? C6 N1 C2 O1 -4.2(6) . . . . ? Ni1 N1 C2 O1 -171.5(3) . . . . ? C6 N1 C2 C1 175.4(3) . . . . ? Ni1 N1 C2 C1 8.2(5) . . . . ? S1 C1 C2 O1 176.0(3) . . . . ? S1 C1 C2 N1 -3.8(5) . . . . ? Ni1 S2 C3 C4 20.1(3) . . . . ? Au1 S2 C3 C4 -76.8(3) 3_676 . . . ? C5 N2 C4 O2 -0.4(6) . . . . ? Ni1 N2 C4 O2 -163.7(3) . . . . ? C5 N2 C4 C3 -176.4(3) . . . . ? Ni1 N2 C4 C3 20.2(5) . . . . ? S2 C3 C4 O2 157.2(3) . . . . ? S2 C3 C4 N2 -26.4(4) . . . . ? C4 N2 C5 C6 165.7(4) . . . . ? Ni1 N2 C5 C6 -29.3(4) . . . . ? C2 N1 C6 C5 167.1(4) . . . . ? Ni1 N1 C6 C5 -24.4(4) . . . . ? N2 C5 C6 N1 32.7(5) . . . . ? C9 N3 C7 C8 58.9(4) . . . . ? C13 N3 C7 C8 179.7(3) . . . . ? C11 N3 C7 C8 -59.6(4) . . . . ? C7 N3 C9 C10 55.7(4) . . . . ? C13 N3 C9 C10 -62.3(4) . . . . ? C11 N3 C9 C10 176.7(3) . . . . ? C7 N3 C11 C12 -60.7(4) . . . . ? C9 N3 C11 C12 177.9(3) . . . . ? C13 N3 C11 C12 57.0(4) . . . . ? C7 N3 C13 C14 172.0(4) . . . . ? C9 N3 C13 C14 -67.0(4) . . . . ? C11 N3 C13 C14 51.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.64 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.814 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.138 _database_code_depnum_ccdc_archive 'CCDC 956182' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_niau _vrf_PLAT413_ALERT_2_A ; PROBLEM : Short Inter XH3 .. XHn H2DB .. H74 .. 1.84 Ang. RESPONSE : distances between H atom on a (disordered?) acetonitrile to the a H atom on the Au-Ni complex. Distance is not accurately determined. ; _vrf_PLAT364_ALERT_2B ; PROBLEM : Short C(sp3)-C(sp) Bond C1A - C2A ... 1.22 Ang. PROBLEM : Short C(sp3)-C(sp) Bond C1D - C2D ... 1.20 Ang. PROBLEM : Short C(sp3)-C(sp) Bond C1F - C2F ... 1.24 Ang. RESPONSE : Possibly disordered acetonitrile disorder was not modeled. ; _vrf_PLAT413_ALERT_2_B ; PROBLEM : Short Inter XH3 .. XHn H2DA .. H69 .. 2.07 Ang. PROBLEM : Short Inter XH3 .. XHn H2FB .. H70 .. 2.02 Ang. RESPONSE : distances between H atom on a (disordered?) acetonitrile to the a H atom on the Au-Ni complex. Distance is not accurately determined. ; _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H100 Au4 N10 Ni2 O7 P4 S4' _chemical_formula_weight 2663.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.465(2) _cell_length_b 16.178(2) _cell_length_c 25.137(4) _cell_angle_alpha 75.987(2) _cell_angle_beta 78.277(2) _cell_angle_gamma 71.395(2) _cell_volume 4987.9(13) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9813 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.32 _exptl_crystal_description 'plate ' _exptl_crystal_colour 'colorless ' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.773 _exptl_crystal_F_000 2596 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 6.436 _shelx_estimated_absorpt_T_min 0.565 _shelx_estimated_absorpt_T_max 0.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3136 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ; SADABS-2009/1 (Bruker,2009) was employed for absorption correction. wR2(int) was 0.1511 before and 0.0538 after correction. The ratio of minimum to maximum transmission factors was 0.4205. Additional spherical absorption correction applied with mu*r = 0.2000. The \l/2 correction factor of 0.0015 was applied. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 59144 _diffrn_reflns_av_unetI/netI 0.0566 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.101 _diffrn_reflns_theta_max 28.382 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 24138 _reflns_number_gt 19886 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'APEXII (Bruker, 2012a)' _computing_cell_refinement 'APEXII (Bruker, 2012a)' _computing_data_reduction 'SAINT (Bruker, 2012b)' _computing_structure_solution 'SHELXS (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'shelXLe (H\"ubschle 2011)' _computing_publication_material 'Ciftab (Sheldrick, 2008)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+26.6216P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 24138 _refine_ls_number_parameters 1159 _refine_ls_number_restraints 171 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1039 _refine_ls_wR_factor_gt 0.0993 _refine_ls_goodness_of_fit_ref 1.125 _refine_ls_restrained_S_all 1.144 _refine_ls_shift/su_max 0.057 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group N1A N -0.1497(8) 0.4258(7) 0.1876(4) 0.085(3) Uani 1 1 d D U . . . C1A C -0.1498(9) 0.4471(7) 0.1325(5) 0.068(2) Uani 1 1 d D U . . . C2A C -0.1540(9) 0.4669(7) 0.0829(4) 0.071(3) Uani 1 1 d D U . . . H2AA H -0.0920 0.4291 0.0636 0.085 Uiso 1 1 calc R U . . . H2AB H -0.1550 0.5293 0.0696 0.085 Uiso 1 1 calc R U . . . H2AC H -0.2185 0.4583 0.0756 0.085 Uiso 1 1 calc R U . . . N1B N -0.0690(8) 0.5818(6) 0.2421(5) 0.093(3) Uani 1 1 d D U . . . C1B C 0.0042(8) 0.5966(6) 0.2548(5) 0.066(2) Uani 1 1 d D U . . . C2B C 0.0831(7) 0.6123(6) 0.2720(5) 0.059(2) Uani 1 1 d D U . . . H2BA H 0.1456 0.6039 0.2438 0.071 Uiso 1 1 calc R U . . . H2BB H 0.1002 0.5710 0.3067 0.071 Uiso 1 1 calc R U . . . H2BC H 0.0612 0.6735 0.2782 0.071 Uiso 1 1 calc R U . . . N1C N 0.8988(8) -0.5942(6) 0.4800(4) 0.071(2) Uani 1 1 d D U . . . C1C C 0.8562(8) -0.6501(6) 0.4814(4) 0.060(2) Uani 1 1 d D U . . . C2C C 0.8187(10) -0.7183(7) 0.4823(5) 0.079(3) Uani 1 1 d D U . . . H2CA H 0.8558 -0.7474 0.4510 0.095 Uiso 1 1 calc R U . . . H2CB H 0.7428 -0.6959 0.4796 0.095 Uiso 1 1 calc R U . . . H2CC H 0.8302 -0.7612 0.5171 0.095 Uiso 1 1 calc R U . . . N1D N 0.9913(10) -0.3942(6) 0.0348(6) 0.112(3) Uani 1 1 d D U . . . C1D C 0.9840(9) -0.3068(7) 0.0261(5) 0.070(3) Uani 1 1 d D U . . . C2D C 0.9673(9) -0.2276(6) 0.0173(5) 0.069(3) Uani 1 1 d D U . . . H2DA H 1.0103 -0.2090 -0.0173 0.082 Uiso 1 1 calc R U . . . H2DB H 0.9858 -0.2102 0.0479 0.082 Uiso 1 1 calc R U . . . H2DC H 0.8922 -0.1990 0.0140 0.082 Uiso 1 1 calc R U . . . N1E N 0.5430(7) -0.2576(8) -0.0072(4) 0.091(3) Uani 1 1 d D U . . . C1E C 0.4770(8) -0.2700(9) 0.0330(4) 0.075(3) Uani 1 1 d D U . . . C2E C 0.4018(8) -0.2770(8) 0.0763(4) 0.072(3) Uani 1 1 d D U . . . H2EA H 0.3798 -0.3301 0.0783 0.086 Uiso 1 1 calc R U . . . H2EB H 0.3408 -0.2242 0.0719 0.086 Uiso 1 1 calc R U . . . H2EC H 0.4297 -0.2820 0.1104 0.086 Uiso 1 1 calc R U . . . N1F N -0.4007(11) 0.4880(9) 0.0523(6) 0.123(4) Uani 1 1 d D U . . . C1F C -0.3434(11) 0.4302(9) 0.0194(6) 0.096(3) Uani 1 1 d D U . . . C2F C -0.2857(11) 0.3850(8) -0.0144(6) 0.094(4) Uani 1 1 d D U . . . H2FA H -0.3036 0.4137 -0.0516 0.113 Uiso 1 1 calc R U . . . H2FB H -0.2964 0.3257 -0.0050 0.113 Uiso 1 1 calc R U . . . H2FC H -0.2116 0.3797 -0.0133 0.113 Uiso 1 1 calc R U . . . O1W O 0.5996(4) 0.5287(4) 0.1812(3) 0.0488(15) Uani 1 1 d G . . . . H1WA H 0.5467 0.5651 0.1977 0.073 Uiso 1 1 d G U . . . H1WB H 0.5778 0.4881 0.1737 0.073 Uiso 1 1 d G U . . . O2W O 0.3165(5) 0.5662(4) 0.1919(3) 0.0597(18) Uani 1 1 d G . . . . H2WA H 0.3453 0.6073 0.1919 0.090 Uiso 1 1 d G U . . . H2WB H 0.3650 0.5155 0.1923 0.090 Uiso 1 1 d G U . . . O3W O -0.0565(5) -0.0126(5) 0.3380(3) 0.0597(18) Uani 1 1 d G . . . . H3WA H -0.0254 -0.0538 0.3636 0.090 Uiso 1 1 d G U . . . H3WB H -0.1164 0.0189 0.3528 0.090 Uiso 1 1 d G U . . . Au1 Au 0.22620(2) 0.07533(2) 0.25214(2) 0.01994(6) Uani 1 1 d . . . . . Au2 Au 0.56577(2) -0.18218(2) 0.29656(2) 0.02099(6) Uani 1 1 d . . . . . Au3 Au 0.32014(2) 0.20786(2) 0.27758(2) 0.01925(6) Uani 1 1 d . . . . . Au4 Au 0.68488(2) -0.03895(2) 0.24135(2) 0.02188(6) Uani 1 1 d . . . . . Ni1 Ni 0.33763(6) -0.12649(5) 0.29386(3) 0.01800(15) Uani 1 1 d . . . . . Ni2 Ni 0.54930(6) 0.16150(5) 0.26610(3) 0.01823(15) Uani 1 1 d . . . . . S1 S 0.29921(12) -0.00954(10) 0.33140(7) 0.0206(3) Uani 1 1 d . . . . . S2 S 0.46218(11) -0.09525(10) 0.22708(7) 0.0207(3) Uani 1 1 d . . . . . S3 S 0.45208(11) 0.16661(10) 0.20398(7) 0.0208(3) Uani 1 1 d . . . . . S4 S 0.56301(12) 0.02432(10) 0.31060(7) 0.0228(3) Uani 1 1 d . . . . . P1 P 0.16420(12) 0.14826(11) 0.17099(7) 0.0216(3) Uani 1 1 d . . . . . P2 P 0.63477(12) -0.27916(10) 0.37043(7) 0.0208(3) Uani 1 1 d . . . . . P3 P 0.20698(12) 0.25837(10) 0.35002(7) 0.0184(3) Uani 1 1 d . . . . . P4 P 0.79855(13) -0.08881(11) 0.16838(7) 0.0238(3) Uani 1 1 d . . . . . O1 O 0.0890(4) -0.1365(3) 0.4108(2) 0.0381(12) Uani 1 1 d . . . . . O2 O 0.4369(4) -0.3212(3) 0.2052(2) 0.0396(13) Uani 1 1 d . . . . . O3 O 0.4857(4) 0.4075(3) 0.1752(2) 0.0299(11) Uani 1 1 d . . . . . O4 O 0.7521(4) 0.1044(3) 0.3748(2) 0.0305(11) Uani 1 1 d . . . . . N9 N 0.2372(4) -0.1657(3) 0.3480(2) 0.0230(11) Uani 1 1 d . . . . . N2 N 0.3584(4) -0.2294(3) 0.2682(2) 0.0248(12) Uani 1 1 d . . . . . N3 N 0.5450(4) 0.2791(3) 0.2349(2) 0.0232(11) Uani 1 1 d . . . . . N4 N 0.6311(4) 0.1701(3) 0.3144(2) 0.0209(11) Uani 1 1 d . . . . . C1I C 0.4648(5) -0.1769(4) 0.1873(3) 0.0248(13) Uani 1 1 d . . . . . H1IA H 0.4242 -0.1466 0.1559 0.030 Uiso 1 1 calc R U . . . H1IB H 0.5388 -0.2039 0.1720 0.030 Uiso 1 1 calc R U . . . C1J C 0.4185(5) -0.2493(4) 0.2223(3) 0.0235(13) Uani 1 1 d . . . . . C3 C 0.3132(6) -0.2962(4) 0.3070(3) 0.0323(16) Uani 1 1 d . . . . . H3A H 0.3660 -0.3373 0.3307 0.039 Uiso 1 1 calc R U . . . H3B H 0.2916 -0.3313 0.2865 0.039 Uiso 1 1 calc R U . . . C4 C 0.2185(5) -0.2466(4) 0.3418(3) 0.0297(15) Uani 1 1 d . . . . . H4A H 0.1544 -0.2315 0.3239 0.036 Uiso 1 1 calc R U . . . H4B H 0.2073 -0.2842 0.3787 0.036 Uiso 1 1 calc R U . . . C5 C 0.1686(5) -0.1169(4) 0.3810(3) 0.0242(13) Uani 1 1 d . . . . . C6 C 0.1897(5) -0.0314(4) 0.3827(3) 0.0282(14) Uani 1 1 d . . . . . H6A H 0.2057 -0.0345 0.4200 0.034 Uiso 1 1 calc R U . . . H6B H 0.1252 0.0185 0.3761 0.034 Uiso 1 1 calc R U . . . C7 C 0.4562(5) 0.2761(4) 0.1625(3) 0.0263(14) Uani 1 1 d . . . . . H7A H 0.5024 0.2684 0.1270 0.032 Uiso 1 1 calc R U . . . H7B H 0.3842 0.3110 0.1541 0.032 Uiso 1 1 calc R U . . . C8 C 0.4972(5) 0.3272(4) 0.1924(3) 0.0220(13) Uani 1 1 d . . . . . C9 C 0.6809(5) 0.1038(4) 0.3503(3) 0.0240(13) Uani 1 1 d . . . . . C10 C 0.6427(5) 0.0213(4) 0.3626(3) 0.0288(14) Uani 1 1 d . . . . . H10A H 0.5998 0.0169 0.3996 0.035 Uiso 1 1 calc R U . . . H10B H 0.7045 -0.0321 0.3633 0.035 Uiso 1 1 calc R U . . . C11 C 0.6639(5) 0.2512(4) 0.3009(3) 0.0240(13) Uani 1 1 d . . . . . H11A H 0.7353 0.2410 0.2791 0.029 Uiso 1 1 calc R U . . . H11B H 0.6662 0.2699 0.3352 0.029 Uiso 1 1 calc R U . . . C12 C 0.5835(5) 0.3229(4) 0.2672(3) 0.0309(15) Uani 1 1 d . . . . . H12A H 0.5242 0.3542 0.2922 0.037 Uiso 1 1 calc R U . . . H12B H 0.6173 0.3669 0.2424 0.037 Uiso 1 1 calc R U . . . C13 C 0.0246(5) 0.1637(4) 0.1719(3) 0.0232(13) Uani 1 1 d . . . . . C14 C -0.0295(5) 0.1154(4) 0.2142(3) 0.0268(14) Uani 1 1 d . . . . . H14 H 0.0064 0.0749 0.2431 0.032 Uiso 1 1 calc R U . . . C15 C -0.1354(6) 0.1258(5) 0.2145(3) 0.0357(17) Uani 1 1 d . . . . . H15 H -0.1724 0.0929 0.2437 0.043 Uiso 1 1 calc R U . . . C16 C -0.1866(6) 0.1830(5) 0.1730(4) 0.0381(18) Uani 1 1 d . . . . . H16 H -0.2597 0.1902 0.1737 0.046 Uiso 1 1 calc R U . . . C17 C -0.1342(6) 0.2311(5) 0.1296(3) 0.0367(17) Uani 1 1 d . . . . . H17 H -0.1705 0.2703 0.1004 0.044 Uiso 1 1 calc R U . . . C18 C -0.0281(6) 0.2211(5) 0.1294(3) 0.0335(16) Uani 1 1 d . . . . . H18 H 0.0087 0.2537 0.0999 0.040 Uiso 1 1 calc R U . . . C19 C 0.1449(5) 0.3159(4) 0.1858(3) 0.0314(15) Uani 1 1 d . . . . . H19 H 0.1177 0.2954 0.2229 0.038 Uiso 1 1 calc R U . . . C20 C 0.1518(7) 0.4014(5) 0.1692(4) 0.047(2) Uani 1 1 d . . . . . H20 H 0.1273 0.4403 0.1950 0.057 Uiso 1 1 calc R U . . . C21 C 0.1932(7) 0.4322(5) 0.1162(4) 0.053(2) Uani 1 1 d . . . . . H21 H 0.1990 0.4911 0.1060 0.063 Uiso 1 1 calc R U . . . C22 C 0.2262(7) 0.3779(6) 0.0780(4) 0.050(2) Uani 1 1 d . . . . . H22 H 0.2535 0.3994 0.0412 0.060 Uiso 1 1 calc R U . . . C23 C 0.2195(6) 0.2903(5) 0.0936(3) 0.0388(18) Uani 1 1 d . . . . . H23 H 0.2429 0.2523 0.0673 0.047 Uiso 1 1 calc R U . . . C24 C 0.1789(5) 0.2590(4) 0.1472(3) 0.0253(13) Uani 1 1 d . . . . . C25 C 0.2346(5) 0.0856(4) 0.1174(3) 0.0251(13) Uani 1 1 d . . . . . C26 C 0.1839(6) 0.0525(5) 0.0879(3) 0.0388(18) Uani 1 1 d . . . . . H26 H 0.1090 0.0661 0.0939 0.047 Uiso 1 1 calc R U . . . C27 C 0.2432(7) -0.0006(6) 0.0495(3) 0.044(2) Uani 1 1 d . . . . . H27 H 0.2082 -0.0226 0.0291 0.053 Uiso 1 1 calc R U . . . C28 C 0.3525(7) -0.0213(5) 0.0411(3) 0.0424(19) Uani 1 1 d . . . . . H28 H 0.3927 -0.0583 0.0156 0.051 Uiso 1 1 calc R U . . . C29 C 0.4029(6) 0.0121(5) 0.0700(3) 0.0373(17) Uani 1 1 d . . . . . H29 H 0.4778 -0.0010 0.0636 0.045 Uiso 1 1 calc R U . . . C30 C 0.3456(6) 0.0642(5) 0.1080(3) 0.0345(16) Uani 1 1 d . . . . . H30 H 0.3814 0.0859 0.1280 0.041 Uiso 1 1 calc R U . . . C31 C 0.7723(5) -0.2994(4) 0.3766(3) 0.0238(13) Uani 1 1 d . . . . . C32 C 0.8156(5) -0.2280(5) 0.3579(3) 0.0291(15) Uani 1 1 d . . . . . H32 H 0.7774 -0.1746 0.3366 0.035 Uiso 1 1 calc R U . . . C33 C 0.9136(6) -0.2345(6) 0.3702(4) 0.0425(19) Uani 1 1 d . . . . . H33 H 0.9428 -0.1858 0.3578 0.051 Uiso 1 1 calc R U . . . C34 C 0.9691(6) -0.3134(7) 0.4010(4) 0.051(2) Uani 1 1 d . . . . . H34 H 1.0349 -0.3173 0.4112 0.061 Uiso 1 1 calc R U . . . C35 C 0.9301(6) -0.3862(6) 0.4171(3) 0.047(2) Uani 1 1 d . . . . . H35 H 0.9706 -0.4408 0.4362 0.056 Uiso 1 1 calc R U . . . C36 C 0.8303(5) -0.3789(5) 0.4050(3) 0.0340(16) Uani 1 1 d . . . . . H36 H 0.8025 -0.4285 0.4162 0.041 Uiso 1 1 calc R U . . . C37 C 0.6140(5) -0.3867(4) 0.3741(3) 0.0229(13) Uani 1 1 d . . . . . C38 C 0.6124(5) -0.4117(4) 0.3251(3) 0.0309(15) Uani 1 1 d . . . . . H38 H 0.6258 -0.3749 0.2904 0.037 Uiso 1 1 calc R U . . . C39 C 0.5912(6) -0.4909(5) 0.3279(4) 0.0372(17) Uani 1 1 d . . . . . H39 H 0.5893 -0.5080 0.2946 0.045 Uiso 1 1 calc R U . . . C40 C 0.5727(6) -0.5456(5) 0.3780(4) 0.0373(18) Uani 1 1 d . . . . . H40 H 0.5575 -0.5995 0.3791 0.045 Uiso 1 1 calc R U . . . C41 C 0.5763(6) -0.5218(5) 0.4263(4) 0.0390(18) Uani 1 1 d . . . . . H41 H 0.5649 -0.5598 0.4609 0.047 Uiso 1 1 calc R U . . . C42 C 0.5966(6) -0.4422(5) 0.4248(3) 0.0328(16) Uani 1 1 d . . . . . H42 H 0.5987 -0.4256 0.4582 0.039 Uiso 1 1 calc R U . . . C43 C 0.5637(5) -0.2463(4) 0.4350(3) 0.0263(14) Uani 1 1 d . . . . . C44 C 0.6116(6) -0.2640(5) 0.4822(3) 0.0372(17) Uani 1 1 d . . . . . H44 H 0.6859 -0.2900 0.4804 0.045 Uiso 1 1 calc R U . . . C45 C 0.5527(7) -0.2442(6) 0.5314(3) 0.046(2) Uani 1 1 d . . . . . H45 H 0.5863 -0.2573 0.5634 0.056 Uiso 1 1 calc R U . . . C46 C 0.4444(7) -0.2054(5) 0.5345(4) 0.0427(19) Uani 1 1 d . . . . . H46 H 0.4036 -0.1921 0.5685 0.051 Uiso 1 1 calc R U . . . C47 C 0.3971(6) -0.1863(5) 0.4881(3) 0.0426(19) Uani 1 1 d . . . . . H47 H 0.3231 -0.1585 0.4901 0.051 Uiso 1 1 calc R U . . . C48 C 0.4547(6) -0.2068(5) 0.4377(3) 0.0361(17) Uani 1 1 d . . . . . H48 H 0.4204 -0.1941 0.4059 0.043 Uiso 1 1 calc R U . . . C49 C 0.2187(5) 0.1763(4) 0.4134(3) 0.0233(13) Uani 1 1 d . . . . . C50 C 0.3169(5) 0.1138(4) 0.4205(3) 0.0273(14) Uani 1 1 d . . . . . H50 H 0.3752 0.1143 0.3920 0.033 Uiso 1 1 calc R U . . . C51 C 0.3292(6) 0.0515(5) 0.4690(3) 0.0345(16) Uani 1 1 d . . . . . H51 H 0.3968 0.0107 0.4743 0.041 Uiso 1 1 calc R U . . . C52 C 0.2445(7) 0.0479(5) 0.5098(3) 0.0426(19) Uani 1 1 d . . . . . H52 H 0.2520 0.0024 0.5420 0.051 Uiso 1 1 calc R U . . . C53 C 0.1476(7) 0.1115(6) 0.5034(3) 0.047(2) Uani 1 1 d . . . . . H53 H 0.0897 0.1115 0.5322 0.057 Uiso 1 1 calc R U . . . C54 C 0.1354(6) 0.1742(5) 0.4555(3) 0.0371(17) Uani 1 1 d . . . . . H54 H 0.0686 0.2168 0.4513 0.044 Uiso 1 1 calc R U . . . C55 C 0.0691(5) 0.2925(4) 0.3423(2) 0.0205(12) Uani 1 1 d . . . . . C56 C 0.0240(5) 0.2279(4) 0.3370(3) 0.0297(15) Uani 1 1 d . . . . . H56 H 0.0667 0.1683 0.3376 0.036 Uiso 1 1 calc R U . . . C57 C -0.0814(6) 0.2502(5) 0.3308(4) 0.0384(18) Uani 1 1 d . . . . . H57 H -0.1117 0.2057 0.3285 0.046 Uiso 1 1 calc R U . . . C58 C -0.1434(6) 0.3380(5) 0.3281(4) 0.0382(18) Uani 1 1 d . . . . . H58 H -0.2156 0.3538 0.3232 0.046 Uiso 1 1 calc R U . . . C59 C -0.1000(6) 0.4020(5) 0.3325(4) 0.0371(18) Uani 1 1 d . . . . . H59 H -0.1426 0.4618 0.3306 0.045 Uiso 1 1 calc R U . . . C60 C 0.0056(5) 0.3799(4) 0.3396(3) 0.0296(15) Uani 1 1 d . . . . . H60 H 0.0347 0.4246 0.3426 0.036 Uiso 1 1 calc R U . . . C61 C 0.2319(5) 0.3542(4) 0.3656(3) 0.0219(13) Uani 1 1 d . . . . . C62 C 0.2970(5) 0.3983(4) 0.3273(3) 0.0272(14) Uani 1 1 d . . . . . H62 H 0.3259 0.3805 0.2927 0.033 Uiso 1 1 calc R U . . . C63 C 0.3193(6) 0.4685(4) 0.3402(4) 0.0357(17) Uani 1 1 d . . . . . H63 H 0.3638 0.4992 0.3143 0.043 Uiso 1 1 calc R U . . . C64 C 0.2772(6) 0.4941(5) 0.3904(3) 0.0370(17) Uani 1 1 d . . . . . H64 H 0.2941 0.5416 0.3991 0.044 Uiso 1 1 calc R U . . . C65 C 0.2113(6) 0.4520(5) 0.4280(3) 0.0359(17) Uani 1 1 d . . . . . H65 H 0.1809 0.4713 0.4621 0.043 Uiso 1 1 calc R U . . . C66 C 0.1893(6) 0.3809(5) 0.4160(3) 0.0306(15) Uani 1 1 d . . . . . H66 H 0.1451 0.3505 0.4423 0.037 Uiso 1 1 calc R U . . . C67 C 0.8013(5) 0.0044(4) 0.1119(3) 0.0268(14) Uani 1 1 d . . . . . C68 C 0.8957(6) 0.0123(5) 0.0783(3) 0.0344(16) Uani 1 1 d . . . . . H68 H 0.9598 -0.0334 0.0837 0.041 Uiso 1 1 calc R U . . . C69 C 0.8954(7) 0.0863(5) 0.0376(3) 0.0393(18) Uani 1 1 d . . . . . H69 H 0.9603 0.0918 0.0158 0.047 Uiso 1 1 calc R U . . . C70 C 0.8041(8) 0.1520(5) 0.0278(3) 0.044(2) Uani 1 1 d . . . . . H70 H 0.8055 0.2025 -0.0007 0.053 Uiso 1 1 calc R U . . . C71 C 0.7099(7) 0.1444(5) 0.0595(3) 0.0416(19) Uani 1 1 d . . . . . H71 H 0.6461 0.1896 0.0526 0.050 Uiso 1 1 calc R U . . . C72 C 0.7076(6) 0.0700(5) 0.1023(3) 0.0337(16) Uani 1 1 d . . . . . H72 H 0.6427 0.0648 0.1241 0.040 Uiso 1 1 calc R U . . . C73 C 0.9351(5) -0.1404(4) 0.1802(3) 0.0272(14) Uani 1 1 d . . . . . C74 C 1.0030(6) -0.1981(5) 0.1478(3) 0.0390(18) Uani 1 1 d . . . . . H74 H 0.9756 -0.2182 0.1229 0.047 Uiso 1 1 calc R U . . . C75 C 1.1121(6) -0.2281(6) 0.1508(4) 0.051(2) Uani 1 1 d . . . . . H75 H 1.1585 -0.2695 0.1293 0.061 Uiso 1 1 calc R U . . . C76 C 1.1497(6) -0.1951(6) 0.1863(4) 0.053(2) Uani 1 1 d . . . . . H76 H 1.2234 -0.2136 0.1885 0.063 Uiso 1 1 calc R U . . . C77 C 1.0832(6) -0.1362(6) 0.2184(4) 0.046(2) Uani 1 1 d . . . . . H77 H 1.1110 -0.1143 0.2423 0.055 Uiso 1 1 calc R U . . . C78 C 0.9751(6) -0.1090(5) 0.2157(4) 0.0376(17) Uani 1 1 d . . . . . H78 H 0.9286 -0.0690 0.2380 0.045 Uiso 1 1 calc R U . . . C79 C 0.7616(5) -0.1682(4) 0.1424(3) 0.0264(14) Uani 1 1 d . . . . . C80 C 0.7298(6) -0.1504(5) 0.0905(3) 0.0355(17) Uani 1 1 d . . . . . H80 H 0.7276 -0.0944 0.0670 0.043 Uiso 1 1 calc R U . . . C81 C 0.7011(6) -0.2135(6) 0.0724(4) 0.0431(19) Uani 1 1 d . . . . . H81 H 0.6783 -0.2001 0.0372 0.052 Uiso 1 1 calc R U . . . C82 C 0.7060(6) -0.2950(6) 0.1057(4) 0.047(2) Uani 1 1 d . . . . . H82 H 0.6869 -0.3381 0.0933 0.056 Uiso 1 1 calc R U . . . C83 C 0.7378(6) -0.3150(5) 0.1567(4) 0.042(2) Uani 1 1 d . . . . . H83 H 0.7421 -0.3721 0.1792 0.051 Uiso 1 1 calc R U . . . C84 C 0.7640(5) -0.2516(5) 0.1755(4) 0.0362(17) Uani 1 1 d . . . . . H84 H 0.7838 -0.2652 0.2115 0.043 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1A 0.080(6) 0.076(6) 0.093(6) -0.015(5) -0.017(5) -0.012(5) C1A 0.070(5) 0.048(5) 0.090(5) -0.012(5) -0.006(5) -0.026(4) C2A 0.074(6) 0.049(5) 0.087(6) -0.010(5) 0.000(5) -0.025(5) N1B 0.093(6) 0.056(5) 0.135(8) 0.015(5) -0.056(5) -0.027(4) C1B 0.067(5) 0.035(4) 0.097(6) 0.007(4) -0.035(5) -0.014(4) C2B 0.060(5) 0.044(4) 0.077(6) -0.010(4) -0.016(4) -0.017(4) N1C 0.092(6) 0.065(5) 0.046(4) -0.008(4) -0.014(4) -0.007(4) C1C 0.074(5) 0.055(5) 0.041(4) -0.003(4) -0.017(4) -0.002(4) C2C 0.083(7) 0.075(6) 0.074(6) 0.004(5) -0.027(5) -0.018(5) N1D 0.112(7) 0.076(5) 0.137(8) -0.013(6) 0.008(7) -0.032(5) C1D 0.073(5) 0.073(5) 0.068(6) -0.016(5) 0.010(5) -0.036(5) C2D 0.065(6) 0.081(5) 0.062(6) -0.018(5) 0.019(5) -0.037(5) N1E 0.056(5) 0.132(7) 0.072(6) -0.017(6) -0.014(4) -0.007(5) C1E 0.054(5) 0.114(7) 0.059(5) -0.020(5) -0.021(4) -0.015(5) C2E 0.063(5) 0.102(7) 0.063(6) -0.027(5) -0.010(4) -0.030(5) N1F 0.144(9) 0.109(8) 0.126(9) -0.021(6) -0.035(8) -0.039(7) C1F 0.123(9) 0.072(7) 0.119(9) -0.011(5) -0.059(7) -0.040(6) C2F 0.116(9) 0.070(7) 0.115(9) 0.000(6) -0.063(7) -0.035(6) O1W 0.033(3) 0.029(3) 0.089(5) -0.016(3) -0.011(3) -0.009(2) O2W 0.044(3) 0.049(4) 0.086(5) -0.021(4) 0.001(3) -0.014(3) O3W 0.039(3) 0.071(5) 0.040(4) 0.002(3) 0.000(3) 0.012(3) Au1 0.01987(11) 0.01872(11) 0.02174(12) -0.00305(9) -0.00383(9) -0.00618(8) Au2 0.01719(11) 0.02024(11) 0.02558(13) -0.00196(9) -0.00582(9) -0.00542(8) Au3 0.01517(10) 0.02053(11) 0.02277(12) -0.00423(9) -0.00214(8) -0.00627(8) Au4 0.01910(11) 0.02063(11) 0.02627(13) -0.00396(9) -0.00301(9) -0.00658(9) Ni1 0.0139(3) 0.0155(3) 0.0243(4) -0.0024(3) -0.0026(3) -0.0051(3) Ni2 0.0149(3) 0.0169(4) 0.0243(4) -0.0045(3) -0.0031(3) -0.0058(3) S1 0.0200(7) 0.0177(7) 0.0248(8) -0.0036(6) -0.0045(6) -0.0057(5) S2 0.0159(7) 0.0196(7) 0.0258(8) -0.0013(6) -0.0037(6) -0.0060(5) S3 0.0184(7) 0.0220(7) 0.0243(8) -0.0077(6) -0.0018(6) -0.0072(6) S4 0.0198(7) 0.0198(7) 0.0292(9) -0.0041(6) -0.0015(6) -0.0078(6) P1 0.0189(7) 0.0238(8) 0.0225(8) -0.0023(6) -0.0042(6) -0.0075(6) P2 0.0182(7) 0.0199(7) 0.0245(9) -0.0023(6) -0.0063(6) -0.0052(6) P3 0.0142(7) 0.0192(7) 0.0219(8) -0.0028(6) -0.0031(6) -0.0055(5) P4 0.0189(8) 0.0257(8) 0.0267(9) -0.0061(7) -0.0036(6) -0.0050(6) O1 0.028(3) 0.035(3) 0.042(3) 0.000(2) 0.012(2) -0.011(2) O2 0.037(3) 0.031(3) 0.054(4) -0.022(3) 0.001(2) -0.009(2) O3 0.032(3) 0.018(2) 0.040(3) 0.003(2) -0.010(2) -0.0107(19) O4 0.028(2) 0.034(3) 0.030(3) -0.001(2) -0.013(2) -0.009(2) N9 0.018(2) 0.022(3) 0.029(3) -0.001(2) -0.006(2) -0.006(2) N2 0.019(3) 0.022(3) 0.035(3) -0.005(2) 0.000(2) -0.012(2) N3 0.020(3) 0.015(2) 0.036(3) -0.002(2) -0.008(2) -0.0059(19) N4 0.021(3) 0.017(2) 0.026(3) -0.002(2) -0.006(2) -0.008(2) C1I 0.026(3) 0.027(3) 0.021(3) -0.009(3) -0.003(3) -0.006(3) C1J 0.019(3) 0.020(3) 0.034(4) -0.008(3) -0.008(3) -0.004(2) C3 0.033(4) 0.014(3) 0.046(5) -0.004(3) 0.004(3) -0.009(3) C4 0.029(3) 0.023(3) 0.038(4) -0.003(3) 0.000(3) -0.014(3) C5 0.018(3) 0.022(3) 0.028(4) 0.002(3) -0.003(2) -0.005(2) C6 0.027(3) 0.025(3) 0.027(4) -0.002(3) 0.002(3) -0.004(3) C7 0.028(3) 0.025(3) 0.025(4) 0.001(3) -0.005(3) -0.009(3) C8 0.017(3) 0.027(3) 0.022(3) -0.005(3) 0.000(2) -0.007(2) C9 0.019(3) 0.027(3) 0.024(3) -0.009(3) -0.001(2) -0.003(2) C10 0.033(4) 0.021(3) 0.030(4) -0.001(3) -0.007(3) -0.005(3) C11 0.024(3) 0.022(3) 0.032(4) -0.004(3) -0.006(3) -0.015(2) C12 0.027(3) 0.023(3) 0.048(5) -0.009(3) -0.012(3) -0.008(3) C13 0.020(3) 0.024(3) 0.027(4) -0.009(3) -0.003(2) -0.006(2) C14 0.021(3) 0.023(3) 0.038(4) -0.010(3) -0.002(3) -0.008(2) C15 0.031(4) 0.044(4) 0.039(4) -0.017(4) 0.004(3) -0.018(3) C16 0.022(3) 0.045(4) 0.052(5) -0.022(4) -0.004(3) -0.008(3) C17 0.027(4) 0.045(4) 0.038(4) -0.008(3) -0.014(3) -0.005(3) C18 0.030(4) 0.039(4) 0.032(4) -0.005(3) -0.008(3) -0.011(3) C19 0.029(3) 0.025(3) 0.039(4) -0.004(3) -0.008(3) -0.005(3) C20 0.041(5) 0.031(4) 0.070(6) -0.006(4) -0.015(4) -0.010(3) C21 0.047(5) 0.020(4) 0.082(7) 0.008(4) -0.008(5) -0.012(3) C22 0.046(5) 0.039(5) 0.055(6) 0.012(4) 0.000(4) -0.018(4) C23 0.039(4) 0.034(4) 0.041(5) 0.002(3) -0.003(3) -0.015(3) C24 0.020(3) 0.024(3) 0.031(4) 0.000(3) -0.008(3) -0.008(2) C25 0.026(3) 0.029(3) 0.020(3) -0.003(3) -0.004(3) -0.008(3) C26 0.027(4) 0.050(5) 0.048(5) -0.026(4) -0.006(3) -0.009(3) C27 0.050(5) 0.058(5) 0.034(4) -0.025(4) -0.005(4) -0.019(4) C28 0.056(5) 0.034(4) 0.030(4) -0.010(3) 0.003(4) -0.004(4) C29 0.030(4) 0.046(4) 0.029(4) -0.009(3) 0.003(3) -0.004(3) C30 0.028(4) 0.045(4) 0.029(4) -0.010(3) -0.005(3) -0.006(3) C31 0.020(3) 0.025(3) 0.028(4) -0.004(3) -0.006(3) -0.007(2) C32 0.028(3) 0.028(3) 0.034(4) -0.001(3) -0.007(3) -0.015(3) C33 0.030(4) 0.055(5) 0.046(5) -0.003(4) -0.002(3) -0.024(4) C34 0.022(4) 0.084(7) 0.047(5) 0.001(5) -0.008(3) -0.026(4) C35 0.019(3) 0.061(5) 0.043(5) 0.016(4) -0.009(3) -0.007(3) C36 0.022(3) 0.036(4) 0.040(4) 0.005(3) -0.008(3) -0.009(3) C37 0.017(3) 0.021(3) 0.031(4) -0.005(3) -0.005(2) -0.005(2) C38 0.030(4) 0.023(3) 0.038(4) -0.005(3) -0.009(3) -0.003(3) C39 0.039(4) 0.031(4) 0.045(5) -0.014(3) -0.009(3) -0.008(3) C40 0.035(4) 0.026(4) 0.054(5) -0.016(3) 0.000(3) -0.011(3) C41 0.040(4) 0.027(4) 0.047(5) -0.003(3) 0.001(4) -0.013(3) C42 0.037(4) 0.033(4) 0.032(4) -0.007(3) -0.002(3) -0.016(3) C43 0.028(3) 0.024(3) 0.028(4) -0.007(3) -0.004(3) -0.005(3) C44 0.034(4) 0.049(5) 0.033(4) -0.013(4) -0.005(3) -0.014(3) C45 0.063(6) 0.053(5) 0.033(5) -0.015(4) -0.011(4) -0.023(4) C46 0.053(5) 0.031(4) 0.042(5) -0.017(4) 0.011(4) -0.013(4) C47 0.039(4) 0.038(4) 0.036(5) -0.008(4) 0.004(3) 0.004(3) C48 0.029(4) 0.035(4) 0.034(4) -0.004(3) -0.002(3) 0.002(3) C49 0.022(3) 0.027(3) 0.018(3) -0.002(3) -0.005(2) -0.003(2) C50 0.024(3) 0.030(3) 0.030(4) -0.007(3) -0.007(3) -0.008(3) C51 0.031(4) 0.033(4) 0.039(4) 0.002(3) -0.018(3) -0.006(3) C52 0.053(5) 0.042(4) 0.030(4) 0.009(3) -0.016(4) -0.015(4) C53 0.046(5) 0.057(5) 0.024(4) 0.001(4) 0.010(3) -0.008(4) C54 0.033(4) 0.039(4) 0.028(4) 0.003(3) 0.001(3) -0.005(3) C55 0.026(3) 0.023(3) 0.012(3) 0.000(2) -0.002(2) -0.010(2) C56 0.021(3) 0.020(3) 0.050(5) -0.009(3) -0.010(3) -0.003(2) C57 0.027(4) 0.033(4) 0.061(5) -0.013(4) -0.014(3) -0.009(3) C58 0.023(3) 0.039(4) 0.054(5) -0.010(4) -0.012(3) -0.006(3) C59 0.026(3) 0.021(3) 0.061(5) -0.005(3) -0.015(3) 0.002(3) C60 0.022(3) 0.021(3) 0.050(5) -0.007(3) -0.011(3) -0.008(2) C61 0.017(3) 0.024(3) 0.024(3) -0.001(3) -0.008(2) -0.003(2) C62 0.029(3) 0.022(3) 0.033(4) -0.007(3) -0.005(3) -0.008(3) C63 0.037(4) 0.019(3) 0.056(5) -0.005(3) -0.010(4) -0.014(3) C64 0.036(4) 0.027(4) 0.052(5) -0.008(3) -0.014(4) -0.008(3) C65 0.043(4) 0.028(4) 0.040(4) -0.009(3) -0.009(3) -0.010(3) C66 0.033(4) 0.029(3) 0.033(4) -0.012(3) -0.002(3) -0.009(3) C67 0.031(3) 0.027(3) 0.022(3) -0.005(3) -0.005(3) -0.007(3) C68 0.040(4) 0.032(4) 0.035(4) -0.002(3) -0.004(3) -0.018(3) C69 0.053(5) 0.033(4) 0.034(4) -0.004(3) 0.000(4) -0.021(4) C70 0.078(6) 0.034(4) 0.024(4) -0.004(3) -0.011(4) -0.021(4) C71 0.055(5) 0.030(4) 0.033(4) -0.008(3) -0.017(4) 0.006(3) C72 0.033(4) 0.037(4) 0.025(4) -0.006(3) -0.008(3) -0.001(3) C73 0.017(3) 0.023(3) 0.032(4) 0.005(3) -0.006(3) 0.002(2) C74 0.022(3) 0.046(4) 0.045(5) -0.009(4) -0.006(3) -0.003(3) C75 0.027(4) 0.060(6) 0.059(6) -0.014(5) -0.005(4) -0.003(4) C76 0.024(4) 0.048(5) 0.078(7) 0.010(5) -0.020(4) -0.006(4) C77 0.038(4) 0.049(5) 0.055(6) 0.006(4) -0.026(4) -0.018(4) C78 0.034(4) 0.029(4) 0.050(5) -0.001(3) -0.012(3) -0.010(3) C79 0.020(3) 0.025(3) 0.034(4) -0.007(3) -0.003(3) -0.005(2) C80 0.031(4) 0.049(4) 0.031(4) -0.013(3) 0.003(3) -0.017(3) C81 0.038(4) 0.056(5) 0.043(5) -0.023(4) -0.004(4) -0.016(4) C82 0.027(4) 0.043(5) 0.081(7) -0.035(5) 0.001(4) -0.012(3) C83 0.034(4) 0.025(4) 0.068(6) -0.012(4) -0.001(4) -0.008(3) C84 0.022(3) 0.034(4) 0.051(5) -0.004(3) -0.006(3) -0.008(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 N1A C1A 1.344(11) . ? C1A C2A 1.218(11) . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? N1B C1B 1.202(10) . ? C1B C2B 1.340(10) . ? C2B H2BA 0.9800 . ? C2B H2BB 0.9800 . ? C2B H2BC 0.9800 . ? N1C C1C 1.208(10) . ? C1C C2C 1.345(11) . ? C2C H2CA 0.9800 . ? C2C H2CB 0.9800 . ? C2C H2CC 0.9800 . ? N1D C1D 1.351(10) . ? C1D C2D 1.200(10) . ? C2D H2DA 0.9800 . ? C2D H2DB 0.9800 . ? C2D H2DC 0.9800 . ? N1E C1E 1.225(10) . ? C1E C2E 1.338(11) . ? C2E H2EA 0.9800 . ? C2E H2EB 0.9800 . ? C2E H2EC 0.9800 . ? N1F C1F 1.343(12) . ? C1F C2F 1.237(12) . ? C2F H2FA 0.9800 . ? C2F H2FB 0.9800 . ? C2F H2FC 0.9800 . ? O1W H1WA 0.8703 . ? O1W H1WB 0.8698 . ? O2W H2WA 0.8700 . ? O2W H2WB 0.8699 . ? O3W H3WA 0.8700 . ? O3W H3WB 0.8703 . ? Au1 P1 2.2690(17) . ? Au1 S1 2.3306(16) . ? Au1 Au3 3.0543(4) . ? Au1 Ni1 3.1412(8) . ? Au2 P2 2.2656(16) . ? Au2 S2 2.3500(15) . ? Au2 Ni1 2.9228(9) . ? Au2 Au4 3.1268(4) . ? Au3 P3 2.2592(16) . ? Au3 S3 2.3516(15) . ? Au3 Ni2 2.9042(9) . ? Au4 P4 2.2683(17) . ? Au4 S4 2.3241(16) . ? Ni1 N2 1.848(5) . ? Ni1 N9 1.861(5) . ? Ni1 S1 2.1864(17) . ? Ni1 S2 2.2073(17) . ? Ni2 N4 1.852(5) . ? Ni2 N3 1.861(5) . ? Ni2 S4 2.1980(17) . ? Ni2 S3 2.2041(17) . ? S1 C6 1.817(7) . ? S2 C1I 1.828(6) . ? S3 C7 1.837(6) . ? S4 C10 1.836(7) . ? P1 C24 1.806(7) . ? P1 C25 1.808(7) . ? P1 C13 1.812(6) . ? P2 C31 1.808(6) . ? P2 C43 1.816(7) . ? P2 C37 1.826(6) . ? P3 C55 1.797(6) . ? P3 C49 1.809(7) . ? P3 C61 1.831(6) . ? P4 C79 1.808(7) . ? P4 C67 1.808(7) . ? P4 C73 1.813(6) . ? O1 C5 1.259(8) . ? O2 C1J 1.272(7) . ? O3 C8 1.234(7) . ? O4 C9 1.244(8) . ? N9 C5 1.307(8) . ? N9 C4 1.457(8) . ? N2 C1J 1.312(9) . ? N2 C3 1.470(8) . ? N3 C8 1.311(8) . ? N3 C12 1.455(8) . ? N4 C9 1.315(8) . ? N4 C11 1.458(7) . ? C1I C1J 1.509(9) . ? C1I H1IA 0.9900 . ? C1I H1IB 0.9900 . ? C3 C4 1.507(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.511(9) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.520(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C9 C10 1.522(9) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.526(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C18 1.384(10) . ? C13 C14 1.385(9) . ? C14 C15 1.380(9) . ? C14 H14 0.9500 . ? C15 C16 1.355(11) . ? C15 H15 0.9500 . ? C16 C17 1.386(11) . ? C16 H16 0.9500 . ? C17 C18 1.385(10) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.372(10) . ? C19 C24 1.408(10) . ? C19 H19 0.9500 . ? C20 C21 1.375(13) . ? C20 H20 0.9500 . ? C21 C22 1.369(13) . ? C21 H21 0.9500 . ? C22 C23 1.402(11) . ? C22 H22 0.9500 . ? C23 C24 1.385(10) . ? C23 H23 0.9500 . ? C25 C26 1.389(9) . ? C25 C30 1.405(9) . ? C26 C27 1.400(10) . ? C26 H26 0.9500 . ? C27 C28 1.385(12) . ? C27 H27 0.9500 . ? C28 C29 1.379(11) . ? C28 H28 0.9500 . ? C29 C30 1.376(10) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.383(9) . ? C31 C32 1.397(9) . ? C32 C33 1.383(10) . ? C32 H32 0.9500 . ? C33 C34 1.391(12) . ? C33 H33 0.9500 . ? C34 C35 1.380(12) . ? C34 H34 0.9500 . ? C35 C36 1.400(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.393(10) . ? C37 C38 1.392(10) . ? C38 C39 1.382(10) . ? C38 H38 0.9500 . ? C39 C40 1.381(11) . ? C39 H39 0.9500 . ? C40 C41 1.374(11) . ? C40 H40 0.9500 . ? C41 C42 1.390(10) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.391(10) . ? C43 C48 1.396(9) . ? C44 C45 1.375(11) . ? C44 H44 0.9500 . ? C45 C46 1.385(12) . ? C45 H45 0.9500 . ? C46 C47 1.366(12) . ? C46 H46 0.9500 . ? C47 C48 1.400(11) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.379(9) . ? C49 C50 1.399(9) . ? C50 C51 1.383(10) . ? C50 H50 0.9500 . ? C51 C52 1.377(11) . ? C51 H51 0.9500 . ? C52 C53 1.391(11) . ? C52 H52 0.9500 . ? C53 C54 1.376(11) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C60 1.394(9) . ? C55 C56 1.408(8) . ? C56 C57 1.380(9) . ? C56 H56 0.9500 . ? C57 C58 1.393(10) . ? C57 H57 0.9500 . ? C58 C59 1.375(10) . ? C58 H58 0.9500 . ? C59 C60 1.389(9) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? C61 C62 1.389(9) . ? C61 C66 1.390(9) . ? C62 C63 1.386(9) . ? C62 H62 0.9500 . ? C63 C64 1.378(11) . ? C63 H63 0.9500 . ? C64 C65 1.372(11) . ? C64 H64 0.9500 . ? C65 C66 1.386(9) . ? C65 H65 0.9500 . ? C66 H66 0.9500 . ? C67 C72 1.386(9) . ? C67 C68 1.400(10) . ? C68 C69 1.373(10) . ? C68 H68 0.9500 . ? C69 C70 1.366(12) . ? C69 H69 0.9500 . ? C70 C71 1.380(12) . ? C70 H70 0.9500 . ? C71 C72 1.409(11) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.376(10) . ? C73 C78 1.390(10) . ? C74 C75 1.404(10) . ? C74 H74 0.9500 . ? C75 C76 1.387(13) . ? C75 H75 0.9500 . ? C76 C77 1.376(13) . ? C76 H76 0.9500 . ? C77 C78 1.392(10) . ? C77 H77 0.9500 . ? C78 H78 0.9500 . ? C79 C80 1.390(10) . ? C79 C84 1.398(10) . ? C80 C81 1.395(10) . ? C80 H80 0.9500 . ? C81 C82 1.370(12) . ? C81 H81 0.9500 . ? C82 C83 1.365(13) . ? C82 H82 0.9500 . ? C83 C84 1.391(10) . ? C83 H83 0.9500 . ? C84 H84 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 C2A C1A N1A 177.5(13) . . ? C1A C2A H2AA 109.5 . . ? C1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? C1A C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? N1B C1B C2B 176.6(14) . . ? C1B C2B H2BA 109.5 . . ? C1B C2B H2BB 109.5 . . ? H2BA C2B H2BB 109.5 . . ? C1B C2B H2BC 109.5 . . ? H2BA C2B H2BC 109.5 . . ? H2BB C2B H2BC 109.5 . . ? N1C C1C C2C 174.1(12) . . ? C1C C2C H2CA 109.5 . . ? C1C C2C H2CB 109.5 . . ? H2CA C2C H2CB 109.5 . . ? C1C C2C H2CC 109.5 . . ? H2CA C2C H2CC 109.5 . . ? H2CB C2C H2CC 109.5 . . ? C2D C1D N1D 173.3(14) . . ? C1D C2D H2DA 109.5 . . ? C1D C2D H2DB 109.5 . . ? H2DA C2D H2DB 109.5 . . ? C1D C2D H2DC 109.5 . . ? H2DA C2D H2DC 109.5 . . ? H2DB C2D H2DC 109.5 . . ? N1E C1E C2E 175.8(15) . . ? C1E C2E H2EA 109.5 . . ? C1E C2E H2EB 109.5 . . ? H2EA C2E H2EB 109.5 . . ? C1E C2E H2EC 109.5 . . ? H2EA C2E H2EC 109.5 . . ? H2EB C2E H2EC 109.5 . . ? C2F C1F N1F 172.5(16) . . ? C1F C2F H2FA 109.5 . . ? C1F C2F H2FB 109.5 . . ? H2FA C2F H2FB 109.5 . . ? C1F C2F H2FC 109.5 . . ? H2FA C2F H2FC 109.5 . . ? H2FB C2F H2FC 109.5 . . ? H1WA O1W H1WB 109.5 . . ? H2WA O2W H2WB 109.5 . . ? H3WA O3W H3WB 109.5 . . ? P1 Au1 S1 174.95(6) . . ? P1 Au1 Au3 101.95(4) . . ? S1 Au1 Au3 80.67(4) . . ? P1 Au1 Ni1 131.22(4) . . ? S1 Au1 Ni1 44.08(4) . . ? Au3 Au1 Ni1 116.095(18) . . ? P2 Au2 S2 167.14(5) . . ? P2 Au2 Ni1 120.19(4) . . ? S2 Au2 Ni1 47.99(4) . . ? P2 Au2 Au4 114.40(4) . . ? S2 Au2 Au4 78.18(4) . . ? Ni1 Au2 Au4 116.323(18) . . ? P3 Au3 S3 172.22(5) . . ? P3 Au3 Ni2 125.69(4) . . ? S3 Au3 Ni2 48.19(4) . . ? P3 Au3 Au1 103.57(4) . . ? S3 Au3 Au1 84.18(4) . . ? Ni2 Au3 Au1 116.660(18) . . ? P4 Au4 S4 174.76(6) . . ? P4 Au4 Au2 106.91(4) . . ? S4 Au4 Au2 76.45(4) . . ? N2 Ni1 N9 85.5(2) . . ? N2 Ni1 S1 173.46(17) . . ? N9 Ni1 S1 87.93(17) . . ? N2 Ni1 S2 87.93(17) . . ? N9 Ni1 S2 173.38(17) . . ? S1 Ni1 S2 98.60(6) . . ? N2 Ni1 Au2 86.64(16) . . ? N9 Ni1 Au2 126.06(16) . . ? S1 Ni1 Au2 97.36(5) . . ? S2 Ni1 Au2 52.29(4) . . ? N2 Ni1 Au1 134.10(18) . . ? N9 Ni1 Au1 104.49(16) . . ? S1 Ni1 Au1 47.86(4) . . ? S2 Ni1 Au1 80.89(4) . . ? Au2 Ni1 Au1 118.52(2) . . ? N4 Ni2 N3 85.7(2) . . ? N4 Ni2 S4 87.70(16) . . ? N3 Ni2 S4 173.36(18) . . ? N4 Ni2 S3 173.58(16) . . ? N3 Ni2 S3 87.84(17) . . ? S4 Ni2 S3 98.72(6) . . ? N4 Ni2 Au3 127.64(16) . . ? N3 Ni2 Au3 90.29(16) . . ? S4 Ni2 Au3 92.91(5) . . ? S3 Ni2 Au3 52.67(4) . . ? C6 S1 Ni1 98.3(2) . . ? C6 S1 Au1 106.5(2) . . ? Ni1 S1 Au1 88.06(6) . . ? C1I S2 Ni1 96.1(2) . . ? C1I S2 Au2 102.5(2) . . ? Ni1 S2 Au2 79.72(6) . . ? C7 S3 Ni2 97.5(2) . . ? C7 S3 Au3 100.9(2) . . ? Ni2 S3 Au3 79.14(5) . . ? C10 S4 Ni2 98.3(2) . . ? C10 S4 Au4 104.8(2) . . ? Ni2 S4 Au4 94.17(6) . . ? C24 P1 C25 107.0(3) . . ? C24 P1 C13 104.0(3) . . ? C25 P1 C13 106.9(3) . . ? C24 P1 Au1 114.9(2) . . ? C25 P1 Au1 109.0(2) . . ? C13 P1 Au1 114.5(2) . . ? C31 P2 C43 104.2(3) . . ? C31 P2 C37 107.3(3) . . ? C43 P2 C37 104.0(3) . . ? C31 P2 Au2 119.6(2) . . ? C43 P2 Au2 111.3(2) . . ? C37 P2 Au2 109.2(2) . . ? C55 P3 C49 105.2(3) . . ? C55 P3 C61 105.6(3) . . ? C49 P3 C61 104.9(3) . . ? C55 P3 Au3 115.6(2) . . ? C49 P3 Au3 112.4(2) . . ? C61 P3 Au3 112.3(2) . . ? C79 P4 C67 106.7(3) . . ? C79 P4 C73 105.8(3) . . ? C67 P4 C73 105.4(3) . . ? C79 P4 Au4 113.8(2) . . ? C67 P4 Au4 108.8(2) . . ? C73 P4 Au4 115.7(2) . . ? C5 N9 C4 118.7(5) . . ? C5 N9 Ni1 124.4(4) . . ? C4 N9 Ni1 114.9(4) . . ? C1J N2 C3 119.8(5) . . ? C1J N2 Ni1 125.0(4) . . ? C3 N2 Ni1 114.8(4) . . ? C8 N3 C12 118.7(5) . . ? C8 N3 Ni2 125.8(4) . . ? C12 N3 Ni2 114.7(4) . . ? C9 N4 C11 117.2(5) . . ? C9 N4 Ni2 125.7(4) . . ? C11 N4 Ni2 115.0(4) . . ? C1J C1I S2 111.9(4) . . ? C1J C1I H1IA 109.2 . . ? S2 C1I H1IA 109.2 . . ? C1J C1I H1IB 109.2 . . ? S2 C1I H1IB 109.2 . . ? H1IA C1I H1IB 107.9 . . ? O2 C1J N2 125.7(6) . . ? O2 C1J C1I 119.4(6) . . ? N2 C1J C1I 114.9(5) . . ? N2 C3 C4 106.9(5) . . ? N2 C3 H3A 110.3 . . ? C4 C3 H3A 110.3 . . ? N2 C3 H3B 110.3 . . ? C4 C3 H3B 110.3 . . ? H3A C3 H3B 108.6 . . ? N9 C4 C3 108.9(5) . . ? N9 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N9 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? O1 C5 N9 125.0(6) . . ? O1 C5 C6 119.3(6) . . ? N9 C5 C6 115.7(5) . . ? C5 C6 S1 112.4(5) . . ? C5 C6 H6A 109.1 . . ? S1 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? S1 C6 H6B 109.1 . . ? H6A C6 H6B 107.9 . . ? C8 C7 S3 112.0(5) . . ? C8 C7 H7A 109.2 . . ? S3 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? S3 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O3 C8 N3 125.5(6) . . ? O3 C8 C7 119.7(6) . . ? N3 C8 C7 114.8(5) . . ? O4 C9 N4 126.1(6) . . ? O4 C9 C10 119.3(6) . . ? N4 C9 C10 114.5(5) . . ? C9 C10 S4 111.6(5) . . ? C9 C10 H10A 109.3 . . ? S4 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? S4 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? N4 C11 C12 107.7(5) . . ? N4 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? N4 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? N3 C12 C11 107.4(5) . . ? N3 C12 H12A 110.2 . . ? C11 C12 H12A 110.2 . . ? N3 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C18 C13 C14 119.3(6) . . ? C18 C13 P1 120.5(5) . . ? C14 C13 P1 120.1(5) . . ? C15 C14 C13 120.3(7) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C16 C15 C14 120.0(7) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 C17 121.1(7) . . ? C15 C16 H16 119.4 . . ? C17 C16 H16 119.4 . . ? C16 C17 C18 119.0(7) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C13 C18 C17 120.4(7) . . ? C13 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C20 C19 C24 119.2(8) . . ? C20 C19 H19 120.4 . . ? C24 C19 H19 120.4 . . ? C19 C20 C21 121.5(9) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 120.0(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 119.7(8) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.3(8) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C19 119.2(6) . . ? C23 C24 P1 123.7(6) . . ? C19 C24 P1 117.1(5) . . ? C26 C25 C30 118.7(6) . . ? C26 C25 P1 122.5(5) . . ? C30 C25 P1 118.6(5) . . ? C25 C26 C27 120.1(7) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C28 C27 C26 120.2(7) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C27 119.8(7) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.6(7) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C29 C30 C25 120.6(7) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C36 C31 C32 119.9(6) . . ? C36 C31 P2 122.0(5) . . ? C32 C31 P2 117.6(5) . . ? C33 C32 C31 120.4(7) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 119.2(7) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C35 C34 C33 121.0(7) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 119.5(7) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 119.9(7) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C42 C37 C38 120.0(6) . . ? C42 C37 P2 121.3(5) . . ? C38 C37 P2 118.7(5) . . ? C39 C38 C37 118.9(7) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 121.4(7) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C41 C40 C39 119.7(7) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C42 120.1(7) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 119.9(7) . . ? C41 C42 H42 120.0 . . ? C37 C42 H42 120.0 . . ? C44 C43 C48 119.4(7) . . ? C44 C43 P2 123.0(5) . . ? C48 C43 P2 117.5(5) . . ? C45 C44 C43 120.7(7) . . ? C45 C44 H44 119.6 . . ? C43 C44 H44 119.6 . . ? C44 C45 C46 120.4(8) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C47 C46 C45 119.2(8) . . ? C47 C46 H46 120.4 . . ? C45 C46 H46 120.4 . . ? C46 C47 C48 121.7(8) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C43 C48 C47 118.6(7) . . ? C43 C48 H48 120.7 . . ? C47 C48 H48 120.7 . . ? C54 C49 C50 118.8(6) . . ? C54 C49 P3 122.6(5) . . ? C50 C49 P3 118.6(5) . . ? C51 C50 C49 120.0(7) . . ? C51 C50 H50 120.0 . . ? C49 C50 H50 120.0 . . ? C52 C51 C50 120.6(7) . . ? C52 C51 H51 119.7 . . ? C50 C51 H51 119.7 . . ? C51 C52 C53 119.3(7) . . ? C51 C52 H52 120.3 . . ? C53 C52 H52 120.3 . . ? C54 C53 C52 120.1(7) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C49 121.0(7) . . ? C53 C54 H54 119.5 . . ? C49 C54 H54 119.5 . . ? C60 C55 C56 118.5(6) . . ? C60 C55 P3 123.3(5) . . ? C56 C55 P3 118.2(5) . . ? C57 C56 C55 120.8(6) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 119.7(7) . . ? C56 C57 H57 120.1 . . ? C58 C57 H57 120.1 . . ? C59 C58 C57 120.1(6) . . ? C59 C58 H58 120.0 . . ? C57 C58 H58 120.0 . . ? C58 C59 C60 120.6(6) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C59 C60 C55 120.3(6) . . ? C59 C60 H60 119.8 . . ? C55 C60 H60 119.8 . . ? C62 C61 C66 120.2(6) . . ? C62 C61 P3 119.2(5) . . ? C66 C61 P3 120.5(5) . . ? C63 C62 C61 119.1(7) . . ? C63 C62 H62 120.4 . . ? C61 C62 H62 120.4 . . ? C64 C63 C62 120.3(7) . . ? C64 C63 H63 119.9 . . ? C62 C63 H63 119.9 . . ? C65 C64 C63 121.0(7) . . ? C65 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C64 C65 C66 119.4(7) . . ? C64 C65 H65 120.3 . . ? C66 C65 H65 120.3 . . ? C65 C66 C61 120.0(7) . . ? C65 C66 H66 120.0 . . ? C61 C66 H66 120.0 . . ? C72 C67 C68 119.5(7) . . ? C72 C67 P4 119.0(5) . . ? C68 C67 P4 121.6(5) . . ? C69 C68 C67 119.9(7) . . ? C69 C68 H68 120.1 . . ? C67 C68 H68 120.1 . . ? C70 C69 C68 121.5(8) . . ? C70 C69 H69 119.3 . . ? C68 C69 H69 119.3 . . ? C69 C70 C71 119.5(7) . . ? C69 C70 H70 120.3 . . ? C71 C70 H70 120.3 . . ? C70 C71 C72 120.5(7) . . ? C70 C71 H71 119.8 . . ? C72 C71 H71 119.8 . . ? C67 C72 C71 119.2(7) . . ? C67 C72 H72 120.4 . . ? C71 C72 H72 120.4 . . ? C74 C73 C78 119.6(6) . . ? C74 C73 P4 120.8(6) . . ? C78 C73 P4 118.6(5) . . ? C73 C74 C75 121.3(8) . . ? C73 C74 H74 119.3 . . ? C75 C74 H74 119.3 . . ? C76 C75 C74 117.7(8) . . ? C76 C75 H75 121.2 . . ? C74 C75 H75 121.2 . . ? C77 C76 C75 121.8(7) . . ? C77 C76 H76 119.1 . . ? C75 C76 H76 119.1 . . ? C76 C77 C78 119.5(8) . . ? C76 C77 H77 120.3 . . ? C78 C77 H77 120.3 . . ? C77 C78 C73 120.1(8) . . ? C77 C78 H78 120.0 . . ? C73 C78 H78 120.0 . . ? C80 C79 C84 117.5(7) . . ? C80 C79 P4 123.2(5) . . ? C84 C79 P4 119.4(6) . . ? C79 C80 C81 121.1(8) . . ? C79 C80 H80 119.4 . . ? C81 C80 H80 119.4 . . ? C82 C81 C80 119.7(8) . . ? C82 C81 H81 120.1 . . ? C80 C81 H81 120.1 . . ? C83 C82 C81 120.7(7) . . ? C83 C82 H82 119.6 . . ? C81 C82 H82 119.6 . . ? C82 C83 C84 119.8(8) . . ? C82 C83 H83 120.1 . . ? C84 C83 H83 120.1 . . ? C83 C84 C79 121.2(8) . . ? C83 C84 H84 119.4 . . ? C79 C84 H84 119.4 . . ? 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 N2 Ni1 N9 C5 -168.1(6) . . . . ? S1 Ni1 N9 C5 11.7(5) . . . . ? Au2 Ni1 N9 C5 109.3(5) . . . . ? Au1 Ni1 N9 C5 -33.6(5) . . . . ? N2 Ni1 N9 C4 -4.6(5) . . . . ? S1 Ni1 N9 C4 175.2(4) . . . . ? Au2 Ni1 N9 C4 -87.1(5) . . . . ? Au1 Ni1 N9 C4 129.9(4) . . . . ? N9 Ni1 N2 C1J 173.3(6) . . . . ? S2 Ni1 N2 C1J -7.8(5) . . . . ? Au2 Ni1 N2 C1J -60.2(5) . . . . ? Au1 Ni1 N2 C1J 67.4(6) . . . . ? N9 Ni1 N2 C3 -14.8(5) . . . . ? S2 Ni1 N2 C3 164.2(5) . . . . ? Au2 Ni1 N2 C3 111.8(5) . . . . ? Au1 Ni1 N2 C3 -120.6(4) . . . . ? N4 Ni2 N3 C8 178.9(6) . . . . ? S3 Ni2 N3 C8 -0.7(5) . . . . ? Au3 Ni2 N3 C8 -53.3(5) . . . . ? N4 Ni2 N3 C12 -11.7(5) . . . . ? S3 Ni2 N3 C12 168.6(4) . . . . ? Au3 Ni2 N3 C12 116.0(4) . . . . ? N3 Ni2 N4 C9 -171.8(6) . . . . ? S4 Ni2 N4 C9 9.2(5) . . . . ? Au3 Ni2 N4 C9 101.1(5) . . . . ? N3 Ni2 N4 C11 -8.6(4) . . . . ? S4 Ni2 N4 C11 172.5(4) . . . . ? Au3 Ni2 N4 C11 -95.6(4) . . . . ? Ni1 S2 C1I C1J -20.5(4) . . . . ? Au2 S2 C1I C1J 60.3(5) . . . . ? C3 N2 C1J O2 5.4(10) . . . . ? Ni1 N2 C1J O2 177.1(5) . . . . ? C3 N2 C1J C1I -176.9(6) . . . . ? Ni1 N2 C1J C1I -5.3(8) . . . . ? S2 C1I C1J O2 -163.3(5) . . . . ? S2 C1I C1J N2 18.9(7) . . . . ? C1J N2 C3 C4 -158.3(6) . . . . ? Ni1 N2 C3 C4 29.2(7) . . . . ? C5 N9 C4 C3 -173.8(6) . . . . ? Ni1 N9 C4 C3 21.7(7) . . . . ? N2 C3 C4 N9 -31.0(8) . . . . ? C4 N9 C5 O1 3.9(10) . . . . ? Ni1 N9 C5 O1 166.8(5) . . . . ? C4 N9 C5 C6 -176.5(6) . . . . ? Ni1 N9 C5 C6 -13.6(8) . . . . ? O1 C5 C6 S1 -173.6(5) . . . . ? N9 C5 C6 S1 6.7(8) . . . . ? Ni1 S1 C6 C5 0.9(5) . . . . ? Au1 S1 C6 C5 91.3(5) . . . . ? Ni2 S3 C7 C8 -13.6(5) . . . . ? Au3 S3 C7 C8 66.7(5) . . . . ? C12 N3 C8 O3 3.6(10) . . . . ? Ni2 N3 C8 O3 172.5(5) . . . . ? C12 N3 C8 C7 -177.9(6) . . . . ? Ni2 N3 C8 C7 -8.9(8) . . . . ? S3 C7 C8 O3 -166.0(5) . . . . ? S3 C7 C8 N3 15.3(7) . . . . ? C11 N4 C9 O4 1.7(10) . . . . ? Ni2 N4 C9 O4 164.6(5) . . . . ? C11 N4 C9 C10 179.9(5) . . . . ? Ni2 N4 C9 C10 -17.2(8) . . . . ? O4 C9 C10 S4 -166.0(5) . . . . ? N4 C9 C10 S4 15.7(7) . . . . ? Ni2 S4 C10 C9 -8.5(5) . . . . ? Au4 S4 C10 C9 88.0(5) . . . . ? C9 N4 C11 C12 -170.1(6) . . . . ? Ni2 N4 C11 C12 25.2(7) . . . . ? C8 N3 C12 C11 -162.3(6) . . . . ? Ni2 N3 C12 C11 27.6(7) . . . . ? N4 C11 C12 N3 -32.2(7) . . . . ? C24 P1 C13 C18 41.4(6) . . . . ? C25 P1 C13 C18 -71.6(6) . . . . ? Au1 P1 C13 C18 167.6(5) . . . . ? C24 P1 C13 C14 -141.1(5) . . . . ? C25 P1 C13 C14 105.9(5) . . . . ? Au1 P1 C13 C14 -14.9(6) . . . . ? C18 C13 C14 C15 -1.3(10) . . . . ? P1 C13 C14 C15 -178.8(5) . . . . ? C13 C14 C15 C16 0.5(10) . . . . ? C14 C15 C16 C17 0.7(11) . . . . ? C15 C16 C17 C18 -1.0(12) . . . . ? C14 C13 C18 C17 1.0(10) . . . . ? P1 C13 C18 C17 178.5(6) . . . . ? C16 C17 C18 C13 0.2(11) . . . . ? C24 C19 C20 C21 -1.6(12) . . . . ? C19 C20 C21 C22 1.8(13) . . . . ? C20 C21 C22 C23 -1.3(14) . . . . ? C21 C22 C23 C24 0.6(13) . . . . ? C22 C23 C24 C19 -0.3(11) . . . . ? C22 C23 C24 P1 178.6(6) . . . . ? C20 C19 C24 C23 0.8(10) . . . . ? C20 C19 C24 P1 -178.2(6) . . . . ? C25 P1 C24 C23 11.0(7) . . . . ? C13 P1 C24 C23 -101.9(6) . . . . ? Au1 P1 C24 C23 132.2(5) . . . . ? C25 P1 C24 C19 -170.1(5) . . . . ? C13 P1 C24 C19 77.0(6) . . . . ? Au1 P1 C24 C19 -48.9(5) . . . . ? C24 P1 C25 C26 -115.5(6) . . . . ? C13 P1 C25 C26 -4.5(7) . . . . ? Au1 P1 C25 C26 119.7(6) . . . . ? C24 P1 C25 C30 69.1(6) . . . . ? C13 P1 C25 C30 -179.9(6) . . . . ? Au1 P1 C25 C30 -55.7(6) . . . . ? C30 C25 C26 C27 -0.3(12) . . . . ? P1 C25 C26 C27 -175.7(6) . . . . ? C25 C26 C27 C28 0.7(13) . . . . ? C26 C27 C28 C29 -1.2(13) . . . . ? C27 C28 C29 C30 1.4(13) . . . . ? C28 C29 C30 C25 -1.0(12) . . . . ? C26 C25 C30 C29 0.5(11) . . . . ? P1 C25 C30 C29 176.1(6) . . . . ? C43 P2 C31 C36 82.1(7) . . . . ? C37 P2 C31 C36 -27.8(7) . . . . ? Au2 P2 C31 C36 -152.8(5) . . . . ? C43 P2 C31 C32 -89.9(6) . . . . ? C37 P2 C31 C32 160.2(5) . . . . ? Au2 P2 C31 C32 35.2(6) . . . . ? C36 C31 C32 C33 -3.7(11) . . . . ? P2 C31 C32 C33 168.5(6) . . . . ? C31 C32 C33 C34 0.6(12) . . . . ? C32 C33 C34 C35 3.1(14) . . . . ? C33 C34 C35 C36 -3.8(14) . . . . ? C32 C31 C36 C35 3.0(11) . . . . ? P2 C31 C36 C35 -168.8(6) . . . . ? C34 C35 C36 C31 0.6(13) . . . . ? C31 P2 C37 C42 82.2(6) . . . . ? C43 P2 C37 C42 -27.9(6) . . . . ? Au2 P2 C37 C42 -146.8(5) . . . . ? C31 P2 C37 C38 -99.8(5) . . . . ? C43 P2 C37 C38 150.2(5) . . . . ? Au2 P2 C37 C38 31.2(5) . . . . ? C42 C37 C38 C39 1.5(10) . . . . ? P2 C37 C38 C39 -176.6(5) . . . . ? C37 C38 C39 C40 -0.7(11) . . . . ? C38 C39 C40 C41 -0.6(11) . . . . ? C39 C40 C41 C42 1.2(11) . . . . ? C40 C41 C42 C37 -0.4(11) . . . . ? C38 C37 C42 C41 -0.9(10) . . . . ? P2 C37 C42 C41 177.1(6) . . . . ? C31 P2 C43 C44 -18.6(7) . . . . ? C37 P2 C43 C44 93.7(6) . . . . ? Au2 P2 C43 C44 -148.8(6) . . . . ? C31 P2 C43 C48 165.7(5) . . . . ? C37 P2 C43 C48 -82.1(6) . . . . ? Au2 P2 C43 C48 35.4(6) . . . . ? C48 C43 C44 C45 1.0(11) . . . . ? P2 C43 C44 C45 -174.7(6) . . . . ? C43 C44 C45 C46 -0.8(12) . . . . ? C44 C45 C46 C47 -0.4(12) . . . . ? C45 C46 C47 C48 1.4(12) . . . . ? C44 C43 C48 C47 -0.1(11) . . . . ? P2 C43 C48 C47 175.8(6) . . . . ? C46 C47 C48 C43 -1.1(12) . . . . ? C55 P3 C49 C54 -25.5(7) . . . . ? C61 P3 C49 C54 85.7(6) . . . . ? Au3 P3 C49 C54 -152.0(6) . . . . ? C55 P3 C49 C50 156.1(5) . . . . ? C61 P3 C49 C50 -92.7(6) . . . . ? Au3 P3 C49 C50 29.6(6) . . . . ? C54 C49 C50 C51 0.0(10) . . . . ? P3 C49 C50 C51 178.5(5) . . . . ? C49 C50 C51 C52 2.5(11) . . . . ? C50 C51 C52 C53 -4.3(12) . . . . ? C51 C52 C53 C54 3.5(13) . . . . ? C52 C53 C54 C49 -1.0(14) . . . . ? C50 C49 C54 C53 -0.8(12) . . . . ? P3 C49 C54 C53 -179.2(7) . . . . ? C49 P3 C55 C60 120.7(6) . . . . ? C61 P3 C55 C60 10.0(7) . . . . ? Au3 P3 C55 C60 -114.7(6) . . . . ? C49 P3 C55 C56 -61.4(6) . . . . ? C61 P3 C55 C56 -172.1(5) . . . . ? Au3 P3 C55 C56 63.2(6) . . . . ? C60 C55 C56 C57 -1.9(11) . . . . ? P3 C55 C56 C57 -179.9(6) . . . . ? C55 C56 C57 C58 2.1(12) . . . . ? C56 C57 C58 C59 -1.2(13) . . . . ? C57 C58 C59 C60 0.1(13) . . . . ? C58 C59 C60 C55 0.1(12) . . . . ? C56 C55 C60 C59 0.8(11) . . . . ? P3 C55 C60 C59 178.7(6) . . . . ? C55 P3 C61 C62 -113.0(5) . . . . ? C49 P3 C61 C62 136.1(5) . . . . ? Au3 P3 C61 C62 13.7(6) . . . . ? C55 P3 C61 C66 69.2(6) . . . . ? C49 P3 C61 C66 -41.7(6) . . . . ? Au3 P3 C61 C66 -164.0(5) . . . . ? C66 C61 C62 C63 0.4(10) . . . . ? P3 C61 C62 C63 -177.3(5) . . . . ? C61 C62 C63 C64 0.0(10) . . . . ? C62 C63 C64 C65 -1.2(11) . . . . ? C63 C64 C65 C66 1.9(11) . . . . ? C64 C65 C66 C61 -1.5(11) . . . . ? C62 C61 C66 C65 0.3(10) . . . . ? P3 C61 C66 C65 178.1(5) . . . . ? C79 P4 C67 C72 83.9(6) . . . . ? C73 P4 C67 C72 -163.9(6) . . . . ? Au4 P4 C67 C72 -39.3(6) . . . . ? C79 P4 C67 C68 -96.8(6) . . . . ? C73 P4 C67 C68 15.4(7) . . . . ? Au4 P4 C67 C68 140.0(5) . . . . ? C72 C67 C68 C69 2.5(11) . . . . ? P4 C67 C68 C69 -176.8(6) . . . . ? C67 C68 C69 C70 -1.9(12) . . . . ? C68 C69 C70 C71 0.3(12) . . . . ? C69 C70 C71 C72 0.7(12) . . . . ? C68 C67 C72 C71 -1.5(11) . . . . ? P4 C67 C72 C71 177.8(6) . . . . ? C70 C71 C72 C67 -0.1(11) . . . . ? C79 P4 C73 C74 31.2(7) . . . . ? C67 P4 C73 C74 -81.6(6) . . . . ? Au4 P4 C73 C74 158.2(5) . . . . ? C79 P4 C73 C78 -160.1(6) . . . . ? C67 P4 C73 C78 87.1(6) . . . . ? Au4 P4 C73 C78 -33.1(6) . . . . ? C78 C73 C74 C75 1.7(12) . . . . ? P4 C73 C74 C75 170.3(7) . . . . ? C73 C74 C75 C76 -2.1(13) . . . . ? C74 C75 C76 C77 1.1(14) . . . . ? C75 C76 C77 C78 0.4(14) . . . . ? C76 C77 C78 C73 -0.8(12) . . . . ? C74 C73 C78 C77 -0.2(11) . . . . ? P4 C73 C78 C77 -169.0(6) . . . . ? C67 P4 C79 C80 -7.1(7) . . . . ? C73 P4 C79 C80 -119.0(6) . . . . ? Au4 P4 C79 C80 112.9(6) . . . . ? C67 P4 C79 C84 173.3(5) . . . . ? C73 P4 C79 C84 61.4(6) . . . . ? Au4 P4 C79 C84 -66.7(6) . . . . ? C84 C79 C80 C81 0.2(10) . . . . ? P4 C79 C80 C81 -179.4(6) . . . . ? C79 C80 C81 C82 -1.1(11) . . . . ? C80 C81 C82 C83 0.5(12) . . . . ? C81 C82 C83 C84 1.1(12) . . . . ? C82 C83 C84 C79 -2.1(11) . . . . ? C80 C79 C84 C83 1.4(10) . . . . ? P4 C79 C84 C83 -179.0(6) . . . . ? _refine_diff_density_max 3.615 _refine_diff_density_min -1.925 _refine_diff_density_rms 0.177 _shelxl_version_number 2013-2 _shelx_res_file ; TITL data_0m in P-1 CELL 0.71073 13.4653 16.1779 25.1373 75.987 78.277 71.395 ZERR 2 0.002 0.0023 0.0036 0.002 0.002 0.002 LATT 1 SFAC C H N O P S Ni Au UNIT 192 200 20 14 8 8 4 8 SADI N1A C1A N1B C1B N1C C1C N1D C1D N1E C1E N1F C1F SADI N1A C2A N1B C2B N1C C2C N1D C2D N1E C2E N1F C2F SADI C1A C2A C1B C2B C1C C2C C1D C2D C1E C2E C1F C2F SIMU 0.005 0.01 1.7 N1A > C2F L.S. 12 PLAN 5 SIZE 0.1 0.1 0.05 TEMP -163 BOND $H HTAB CONF WPDB -1 RIGU .005 N1A > C2F fmap 2 acta WGHT 0.026800 26.621607 FVAR 0.04623 N1A 3 -0.149706 0.425795 0.187602 11.00000 0.08000 0.07599 = 0.09321 -0.01529 -0.01686 -0.01175 C1A 1 -0.149792 0.447111 0.132501 11.00000 0.06966 0.04798 = 0.08978 -0.01176 -0.00615 -0.02582 C2A 1 -0.154023 0.466915 0.082905 11.00000 0.07407 0.04916 = 0.08710 -0.00967 0.00050 -0.02544 AFIX 137 H2AA 2 -0.091988 0.429053 0.063635 11.00000 -1.20000 H2AB 2 -0.155027 0.529303 0.069603 11.00000 -1.20000 H2AC 2 -0.218460 0.458320 0.075579 11.00000 -1.20000 AFIX 0 N1B 3 -0.068955 0.581804 0.242075 11.00000 0.09313 0.05573 = 0.13531 0.01464 -0.05607 -0.02720 C1B 1 0.004177 0.596609 0.254759 11.00000 0.06706 0.03504 = 0.09654 0.00665 -0.03545 -0.01357 C2B 1 0.083092 0.612299 0.272042 11.00000 0.05966 0.04386 = 0.07696 -0.01037 -0.01578 -0.01731 AFIX 137 H2BA 2 0.145592 0.603935 0.243843 11.00000 -1.20000 H2BB 2 0.100247 0.570959 0.306693 11.00000 -1.20000 H2BC 2 0.061153 0.673478 0.278230 11.00000 -1.20000 AFIX 0 N1C 3 0.898826 -0.594169 0.480023 11.00000 0.09158 0.06532 = 0.04552 -0.00817 -0.01423 -0.00730 C1C 1 0.856184 -0.650128 0.481368 11.00000 0.07427 0.05487 = 0.04077 -0.00255 -0.01714 -0.00189 C2C 1 0.818716 -0.718279 0.482320 11.00000 0.08328 0.07460 = 0.07395 0.00378 -0.02733 -0.01775 AFIX 137 H2CA 2 0.855824 -0.747413 0.451021 11.00000 -1.20000 H2CB 2 0.742829 -0.695939 0.479582 11.00000 -1.20000 H2CC 2 0.830187 -0.761156 0.517052 11.00000 -1.20000 AFIX 0 N1D 3 0.991296 -0.394189 0.034817 11.00000 0.11204 0.07620 = 0.13702 -0.01285 0.00822 -0.03244 C1D 1 0.984044 -0.306835 0.026112 11.00000 0.07344 0.07314 = 0.06842 -0.01565 0.01039 -0.03642 C2D 1 0.967316 -0.227634 0.017262 11.00000 0.06468 0.08140 = 0.06162 -0.01785 0.01888 -0.03721 AFIX 137 H2DA 2 1.010296 -0.208995 -0.017287 11.00000 -1.20000 H2DB 2 0.985767 -0.210233 0.047876 11.00000 -1.20000 H2DC 2 0.892224 -0.198996 0.013971 11.00000 -1.20000 AFIX 0 N1E 3 0.542976 -0.257554 -0.007236 11.00000 0.05639 0.13247 = 0.07151 -0.01669 -0.01380 -0.00670 C1E 1 0.476961 -0.269973 0.032953 11.00000 0.05369 0.11379 = 0.05924 -0.01986 -0.02070 -0.01458 C2E 1 0.401794 -0.277022 0.076301 11.00000 0.06309 0.10187 = 0.06269 -0.02728 -0.01023 -0.02977 AFIX 137 H2EA 2 0.379847 -0.330059 0.078350 11.00000 -1.20000 H2EB 2 0.340786 -0.224206 0.071911 11.00000 -1.20000 H2EC 2 0.429690 -0.281964 0.110394 11.00000 -1.20000 AFIX 0 N1F 3 -0.400652 0.487967 0.052266 11.00000 0.14372 0.10894 = 0.12568 -0.02133 -0.03508 -0.03862 C1F 1 -0.343375 0.430232 0.019407 11.00000 0.12267 0.07153 = 0.11865 -0.01124 -0.05896 -0.03951 C2F 1 -0.285738 0.384980 -0.014385 11.00000 0.11610 0.06962 = 0.11504 0.00033 -0.06317 -0.03498 AFIX 137 H2FA 2 -0.303591 0.413714 -0.051643 11.00000 -1.20000 H2FB 2 -0.296369 0.325693 -0.005007 11.00000 -1.20000 H2FC 2 -0.211597 0.379686 -0.013273 11.00000 -1.20000 AFIX 6 O1W 4 0.599572 0.528673 0.181181 11.00000 0.03280 0.02869 = 0.08882 -0.01590 -0.01148 -0.00869 H1WA 2 0.546687 0.565123 0.197685 11.00000 -1.50000 H1WB 2 0.577797 0.488149 0.173672 11.00000 -1.50000 AFIX 6 O2W 4 0.316505 0.566207 0.191901 11.00000 0.04406 0.04938 = 0.08572 -0.02087 0.00144 -0.01376 H2WA 2 0.345347 0.607259 0.191929 11.00000 -1.50000 H2WB 2 0.365009 0.515487 0.192258 11.00000 -1.50000 AFIX 6 O3W 4 -0.056492 -0.012639 0.337980 11.00000 0.03884 0.07069 = 0.04034 0.00205 -0.00044 0.01205 H3WA 2 -0.025431 -0.053781 0.363600 11.00000 -1.50000 H3WB 2 -0.116449 0.018874 0.352790 11.00000 -1.50000 AFIX 0 AU1 8 0.226198 0.075334 0.252140 11.00000 0.01987 0.01872 = 0.02174 -0.00305 -0.00383 -0.00618 AU2 8 0.565765 -0.182176 0.296560 11.00000 0.01719 0.02024 = 0.02558 -0.00196 -0.00582 -0.00542 AU3 8 0.320137 0.207858 0.277578 11.00000 0.01517 0.02053 = 0.02277 -0.00423 -0.00214 -0.00627 AU4 8 0.684885 -0.038954 0.241350 11.00000 0.01910 0.02063 = 0.02627 -0.00396 -0.00301 -0.00658 NI1 7 0.337625 -0.126495 0.293856 11.00000 0.01395 0.01554 = 0.02435 -0.00238 -0.00256 -0.00506 NI2 7 0.549305 0.161504 0.266100 11.00000 0.01490 0.01694 = 0.02425 -0.00448 -0.00312 -0.00579 S1 6 0.299210 -0.009540 0.331403 11.00000 0.01995 0.01766 = 0.02476 -0.00360 -0.00448 -0.00574 S2 6 0.462184 -0.095254 0.227079 11.00000 0.01590 0.01964 = 0.02581 -0.00127 -0.00366 -0.00599 S3 6 0.452079 0.166615 0.203982 11.00000 0.01845 0.02199 = 0.02432 -0.00775 -0.00184 -0.00720 S4 6 0.563006 0.024319 0.310599 11.00000 0.01976 0.01981 = 0.02917 -0.00407 -0.00149 -0.00782 P1 5 0.164202 0.148258 0.170987 11.00000 0.01892 0.02383 = 0.02248 -0.00226 -0.00416 -0.00749 P2 5 0.634767 -0.279164 0.370426 11.00000 0.01820 0.01993 = 0.02454 -0.00235 -0.00634 -0.00518 P3 5 0.206982 0.258368 0.350020 11.00000 0.01423 0.01924 = 0.02192 -0.00283 -0.00311 -0.00555 P4 5 0.798548 -0.088814 0.168384 11.00000 0.01885 0.02573 = 0.02669 -0.00614 -0.00361 -0.00501 O1 4 0.088999 -0.136493 0.410844 11.00000 0.02784 0.03513 = 0.04181 -0.00046 0.01224 -0.01133 O2 4 0.436915 -0.321248 0.205215 11.00000 0.03744 0.03127 = 0.05386 -0.02245 0.00115 -0.00884 O3 4 0.485696 0.407481 0.175225 11.00000 0.03224 0.01766 = 0.04021 0.00289 -0.01047 -0.01070 O4 4 0.752098 0.104399 0.374843 11.00000 0.02752 0.03448 = 0.03049 -0.00139 -0.01267 -0.00855 N9 3 0.237173 -0.165695 0.347951 11.00000 0.01780 0.02162 = 0.02873 -0.00095 -0.00566 -0.00574 N2 3 0.358365 -0.229372 0.268187 11.00000 0.01870 0.02231 = 0.03548 -0.00452 0.00020 -0.01190 N3 3 0.544953 0.279092 0.234910 11.00000 0.01960 0.01514 = 0.03590 -0.00213 -0.00786 -0.00588 N4 3 0.631139 0.170053 0.314418 11.00000 0.02129 0.01696 = 0.02631 -0.00218 -0.00556 -0.00804 C1I 1 0.464820 -0.176946 0.187310 11.00000 0.02640 0.02716 = 0.02134 -0.00872 -0.00258 -0.00571 AFIX 23 H1IA 2 0.424221 -0.146593 0.155892 11.00000 -1.20000 H1IB 2 0.538826 -0.203914 0.171962 11.00000 -1.20000 AFIX 0 C1J 1 0.418533 -0.249270 0.222340 11.00000 0.01939 0.01957 = 0.03430 -0.00842 -0.00786 -0.00427 C3 1 0.313218 -0.296239 0.307014 11.00000 0.03332 0.01449 = 0.04621 -0.00442 0.00390 -0.00949 AFIX 23 H3A 2 0.365994 -0.337286 0.330709 11.00000 -1.20000 H3B 2 0.291613 -0.331335 0.286527 11.00000 -1.20000 AFIX 0 C4 1 0.218548 -0.246606 0.341841 11.00000 0.02937 0.02304 = 0.03818 -0.00336 -0.00050 -0.01373 AFIX 23 H4A 2 0.154424 -0.231496 0.323857 11.00000 -1.20000 H4B 2 0.207303 -0.284238 0.378685 11.00000 -1.20000 AFIX 0 C5 1 0.168587 -0.116926 0.381050 11.00000 0.01789 0.02237 = 0.02830 0.00229 -0.00320 -0.00529 C6 1 0.189697 -0.031376 0.382704 11.00000 0.02684 0.02477 = 0.02655 -0.00212 0.00174 -0.00379 AFIX 23 H6A 2 0.205676 -0.034528 0.420009 11.00000 -1.20000 H6B 2 0.125186 0.018546 0.376144 11.00000 -1.20000 AFIX 0 C7 1 0.456172 0.276142 0.162531 11.00000 0.02817 0.02460 = 0.02514 0.00116 -0.00549 -0.00924 AFIX 23 H7A 2 0.502442 0.268362 0.126998 11.00000 -1.20000 H7B 2 0.384154 0.311029 0.154109 11.00000 -1.20000 AFIX 0 C8 1 0.497163 0.327227 0.192408 11.00000 0.01654 0.02703 = 0.02208 -0.00541 0.00040 -0.00704 C9 1 0.680942 0.103816 0.350283 11.00000 0.01864 0.02734 = 0.02443 -0.00887 -0.00081 -0.00278 C10 1 0.642707 0.021302 0.362623 11.00000 0.03260 0.02141 = 0.02956 -0.00066 -0.00747 -0.00509 AFIX 23 H10A 2 0.599814 0.016923 0.399637 11.00000 -1.20000 H10B 2 0.704532 -0.032137 0.363333 11.00000 -1.20000 AFIX 0 C11 1 0.663912 0.251176 0.300894 11.00000 0.02425 0.02172 = 0.03234 -0.00437 -0.00577 -0.01472 AFIX 23 H11A 2 0.735321 0.240981 0.279116 11.00000 -1.20000 H11B 2 0.666232 0.269869 0.335215 11.00000 -1.20000 AFIX 0 C12 1 0.583547 0.322869 0.267229 11.00000 0.02683 0.02281 = 0.04837 -0.00884 -0.01232 -0.00840 AFIX 23 H12A 2 0.524216 0.354154 0.292187 11.00000 -1.20000 H12B 2 0.617324 0.366925 0.242420 11.00000 -1.20000 AFIX 0 C13 1 0.024620 0.163663 0.171891 11.00000 0.01983 0.02435 = 0.02742 -0.00918 -0.00292 -0.00629 C14 1 -0.029506 0.115364 0.214195 11.00000 0.02146 0.02288 = 0.03843 -0.01016 -0.00194 -0.00768 AFIX 43 H14 2 0.006411 0.074887 0.243146 11.00000 -1.20000 AFIX 0 C15 1 -0.135415 0.125801 0.214461 11.00000 0.03072 0.04402 = 0.03860 -0.01652 0.00438 -0.01842 AFIX 43 H15 2 -0.172388 0.092903 0.243709 11.00000 -1.20000 AFIX 0 C16 1 -0.186626 0.182982 0.172994 11.00000 0.02169 0.04549 = 0.05243 -0.02239 -0.00386 -0.00808 AFIX 43 H16 2 -0.259696 0.190229 0.173695 11.00000 -1.20000 AFIX 0 C17 1 -0.134218 0.231080 0.129574 11.00000 0.02681 0.04490 = 0.03843 -0.00773 -0.01408 -0.00457 AFIX 43 H17 2 -0.170530 0.270322 0.100388 11.00000 -1.20000 AFIX 0 C18 1 -0.028078 0.221050 0.129389 11.00000 0.03044 0.03911 = 0.03187 -0.00457 -0.00756 -0.01062 AFIX 43 H18 2 0.008729 0.253750 0.099923 11.00000 -1.20000 AFIX 0 C19 1 0.144950 0.315942 0.185827 11.00000 0.02857 0.02485 = 0.03949 -0.00450 -0.00838 -0.00471 AFIX 43 H19 2 0.117683 0.295405 0.222900 11.00000 -1.20000 AFIX 0 C20 1 0.151769 0.401445 0.169245 11.00000 0.04112 0.03129 = 0.07043 -0.00563 -0.01460 -0.01015 AFIX 43 H20 2 0.127276 0.440334 0.195018 11.00000 -1.20000 AFIX 0 C21 1 0.193236 0.432183 0.116183 11.00000 0.04746 0.02006 = 0.08155 0.00838 -0.00804 -0.01157 AFIX 43 H21 2 0.199022 0.491143 0.105985 11.00000 -1.20000 AFIX 0 C22 1 0.226185 0.377851 0.078044 11.00000 0.04566 0.03869 = 0.05546 0.01176 0.00013 -0.01846 AFIX 43 H22 2 0.253465 0.399387 0.041167 11.00000 -1.20000 AFIX 0 C23 1 0.219499 0.290292 0.093639 11.00000 0.03922 0.03353 = 0.04098 0.00168 -0.00300 -0.01483 AFIX 43 H23 2 0.242940 0.252312 0.067337 11.00000 -1.20000 AFIX 0 C24 1 0.178854 0.258966 0.147236 11.00000 0.02013 0.02437 = 0.03145 0.00006 -0.00788 -0.00760 C25 1 0.234642 0.085557 0.117417 11.00000 0.02579 0.02935 = 0.01977 -0.00346 -0.00384 -0.00759 C26 1 0.183947 0.052539 0.087948 11.00000 0.02668 0.04988 = 0.04809 -0.02629 -0.00571 -0.00932 AFIX 43 H26 2 0.108993 0.066051 0.093882 11.00000 -1.20000 AFIX 0 C27 1 0.243153 -0.000630 0.049509 11.00000 0.05012 0.05795 = 0.03441 -0.02523 -0.00470 -0.01920 AFIX 43 H27 2 0.208225 -0.022590 0.029130 11.00000 -1.20000 AFIX 0 C28 1 0.352524 -0.021283 0.041124 11.00000 0.05561 0.03419 = 0.02986 -0.01046 0.00253 -0.00433 AFIX 43 H28 2 0.392701 -0.058309 0.015568 11.00000 -1.20000 AFIX 0 C29 1 0.402870 0.012090 0.070001 11.00000 0.02979 0.04632 = 0.02868 -0.00937 0.00322 -0.00411 AFIX 43 H29 2 0.477784 -0.001017 0.063604 11.00000 -1.20000 AFIX 0 C30 1 0.345621 0.064191 0.107993 11.00000 0.02800 0.04479 = 0.02948 -0.01009 -0.00507 -0.00590 AFIX 43 H30 2 0.381432 0.085919 0.128034 11.00000 -1.20000 AFIX 0 C31 1 0.772318 -0.299411 0.376644 11.00000 0.01962 0.02547 = 0.02781 -0.00442 -0.00567 -0.00728 C32 1 0.815558 -0.227970 0.357895 11.00000 0.02805 0.02803 = 0.03429 -0.00069 -0.00674 -0.01453 AFIX 43 H32 2 0.777379 -0.174574 0.336556 11.00000 -1.20000 AFIX 0 C33 1 0.913639 -0.234540 0.370224 11.00000 0.03027 0.05475 = 0.04648 -0.00345 -0.00196 -0.02418 AFIX 43 H33 2 0.942780 -0.185767 0.357806 11.00000 -1.20000 AFIX 0 C34 1 0.969104 -0.313446 0.401033 11.00000 0.02212 0.08408 = 0.04744 0.00135 -0.00816 -0.02587 AFIX 43 H34 2 1.034893 -0.317293 0.411173 11.00000 -1.20000 AFIX 0 C35 1 0.930062 -0.386198 0.417092 11.00000 0.01930 0.06149 = 0.04324 0.01597 -0.00884 -0.00675 AFIX 43 H35 2 0.970562 -0.440809 0.436217 11.00000 -1.20000 AFIX 0 C36 1 0.830299 -0.378894 0.404978 11.00000 0.02204 0.03552 = 0.03986 0.00501 -0.00797 -0.00883 AFIX 43 H36 2 0.802459 -0.428464 0.416202 11.00000 -1.20000 AFIX 0 C37 1 0.613981 -0.386706 0.374135 11.00000 0.01737 0.02114 = 0.03086 -0.00520 -0.00462 -0.00535 C38 1 0.612447 -0.411682 0.325144 11.00000 0.03042 0.02303 = 0.03758 -0.00513 -0.00936 -0.00286 AFIX 43 H38 2 0.625800 -0.374916 0.290379 11.00000 -1.20000 AFIX 0 C39 1 0.591178 -0.490859 0.327898 11.00000 0.03912 0.03100 = 0.04508 -0.01438 -0.00859 -0.00778 AFIX 43 H39 2 0.589259 -0.507974 0.294622 11.00000 -1.20000 AFIX 0 C40 1 0.572663 -0.545585 0.378023 11.00000 0.03477 0.02640 = 0.05425 -0.01574 0.00018 -0.01144 AFIX 43 H40 2 0.557467 -0.599466 0.379105 11.00000 -1.20000 AFIX 0 C41 1 0.576312 -0.521779 0.426345 11.00000 0.04013 0.02666 = 0.04747 -0.00255 0.00070 -0.01326 AFIX 43 H41 2 0.564919 -0.559804 0.460864 11.00000 -1.20000 AFIX 0 C42 1 0.596642 -0.442174 0.424787 11.00000 0.03693 0.03327 = 0.03157 -0.00711 -0.00232 -0.01554 AFIX 43 H42 2 0.598712 -0.425603 0.458223 11.00000 -1.20000 AFIX 0 C43 1 0.563671 -0.246349 0.435020 11.00000 0.02763 0.02358 = 0.02801 -0.00737 -0.00450 -0.00541 C44 1 0.611625 -0.263992 0.482191 11.00000 0.03432 0.04923 = 0.03272 -0.01339 -0.00471 -0.01396 AFIX 43 H44 2 0.685935 -0.289979 0.480426 11.00000 -1.20000 AFIX 0 C45 1 0.552651 -0.244229 0.531362 11.00000 0.06328 0.05333 = 0.03272 -0.01461 -0.01091 -0.02345 AFIX 43 H45 2 0.586348 -0.257316 0.563367 11.00000 -1.20000 AFIX 0 C46 1 0.444447 -0.205368 0.534496 11.00000 0.05277 0.03142 = 0.04247 -0.01699 0.01081 -0.01349 AFIX 43 H46 2 0.403635 -0.192094 0.568527 11.00000 -1.20000 AFIX 0 C47 1 0.397069 -0.186341 0.488096 11.00000 0.03893 0.03847 = 0.03602 -0.00780 0.00406 0.00357 AFIX 43 H47 2 0.323075 -0.158469 0.490106 11.00000 -1.20000 AFIX 0 C48 1 0.454704 -0.206840 0.437657 11.00000 0.02915 0.03452 = 0.03359 -0.00365 -0.00199 0.00249 AFIX 43 H48 2 0.420398 -0.194138 0.405905 11.00000 -1.20000 AFIX 0 C49 1 0.218701 0.176285 0.413427 11.00000 0.02245 0.02688 = 0.01765 -0.00249 -0.00502 -0.00294 C50 1 0.316945 0.113831 0.420518 11.00000 0.02430 0.02966 = 0.03039 -0.00669 -0.00691 -0.00816 AFIX 43 H50 2 0.375219 0.114278 0.391989 11.00000 -1.20000 AFIX 0 C51 1 0.329236 0.051458 0.469040 11.00000 0.03086 0.03263 = 0.03901 0.00220 -0.01794 -0.00618 AFIX 43 H51 2 0.396764 0.010741 0.474277 11.00000 -1.20000 AFIX 0 C52 1 0.244452 0.047870 0.509816 11.00000 0.05329 0.04179 = 0.02990 0.00857 -0.01607 -0.01460 AFIX 43 H52 2 0.252043 0.002428 0.541984 11.00000 -1.20000 AFIX 0 C53 1 0.147556 0.111458 0.503436 11.00000 0.04589 0.05672 = 0.02356 0.00098 0.00972 -0.00805 AFIX 43 H53 2 0.089670 0.111523 0.532247 11.00000 -1.20000 AFIX 0 C54 1 0.135387 0.174247 0.455493 11.00000 0.03251 0.03950 = 0.02779 0.00348 0.00137 -0.00535 AFIX 43 H54 2 0.068607 0.216838 0.451294 11.00000 -1.20000 AFIX 0 C55 1 0.069102 0.292469 0.342298 11.00000 0.02645 0.02296 = 0.01234 -0.00049 -0.00203 -0.00988 C56 1 0.024024 0.227924 0.336965 11.00000 0.02116 0.01960 = 0.04979 -0.00888 -0.01008 -0.00289 AFIX 43 H56 2 0.066696 0.168341 0.337585 11.00000 -1.20000 AFIX 0 C57 1 -0.081441 0.250172 0.330844 11.00000 0.02742 0.03293 = 0.06058 -0.01313 -0.01400 -0.00857 AFIX 43 H57 2 -0.111669 0.205739 0.328520 11.00000 -1.20000 AFIX 0 C58 1 -0.143351 0.338046 0.328091 11.00000 0.02332 0.03856 = 0.05429 -0.00968 -0.01198 -0.00636 AFIX 43 H58 2 -0.215622 0.353808 0.323182 11.00000 -1.20000 AFIX 0 C59 1 -0.099970 0.402002 0.332471 11.00000 0.02559 0.02086 = 0.06124 -0.00469 -0.01468 0.00152 AFIX 43 H59 2 -0.142589 0.461814 0.330611 11.00000 -1.20000 AFIX 0 C60 1 0.005632 0.379923 0.339593 11.00000 0.02163 0.02149 = 0.04996 -0.00660 -0.01138 -0.00807 AFIX 43 H60 2 0.034715 0.424648 0.342634 11.00000 -1.20000 AFIX 0 C61 1 0.231928 0.354250 0.365619 11.00000 0.01677 0.02372 = 0.02407 -0.00137 -0.00775 -0.00344 C62 1 0.297049 0.398310 0.327275 11.00000 0.02850 0.02238 = 0.03252 -0.00665 -0.00526 -0.00813 AFIX 43 H62 2 0.325942 0.380549 0.292677 11.00000 -1.20000 AFIX 0 C63 1 0.319320 0.468538 0.340161 11.00000 0.03703 0.01924 = 0.05582 -0.00534 -0.01009 -0.01385 AFIX 43 H63 2 0.363785 0.499170 0.314267 11.00000 -1.20000 AFIX 0 C64 1 0.277217 0.494109 0.390389 11.00000 0.03595 0.02690 = 0.05166 -0.00814 -0.01400 -0.00838 AFIX 43 H64 2 0.294100 0.541615 0.399057 11.00000 -1.20000 AFIX 0 C65 1 0.211285 0.451959 0.428050 11.00000 0.04320 0.02756 = 0.04013 -0.00914 -0.00922 -0.01031 AFIX 43 H65 2 0.180950 0.471287 0.462082 11.00000 -1.20000 AFIX 0 C66 1 0.189301 0.380934 0.416029 11.00000 0.03251 0.02930 = 0.03264 -0.01199 -0.00196 -0.00934 AFIX 43 H66 2 0.145077 0.350465 0.442252 11.00000 -1.20000 AFIX 0 C67 1 0.801274 0.004439 0.111948 11.00000 0.03101 0.02745 = 0.02195 -0.00515 -0.00514 -0.00712 C68 1 0.895691 0.012314 0.078336 11.00000 0.03973 0.03188 = 0.03471 -0.00208 -0.00408 -0.01832 AFIX 43 H68 2 0.959802 -0.033433 0.083707 11.00000 -1.20000 AFIX 0 C69 1 0.895445 0.086260 0.037608 11.00000 0.05295 0.03350 = 0.03367 -0.00380 -0.00021 -0.02092 AFIX 43 H69 2 0.960251 0.091840 0.015775 11.00000 -1.20000 AFIX 0 C70 1 0.804135 0.151978 0.027773 11.00000 0.07821 0.03430 = 0.02386 -0.00351 -0.01137 -0.02121 AFIX 43 H70 2 0.805500 0.202531 -0.000709 11.00000 -1.20000 AFIX 0 C71 1 0.709884 0.144351 0.059541 11.00000 0.05450 0.02969 = 0.03329 -0.00811 -0.01663 0.00615 AFIX 43 H71 2 0.646053 0.189567 0.052571 11.00000 -1.20000 AFIX 0 C72 1 0.707631 0.069959 0.102258 11.00000 0.03334 0.03744 = 0.02519 -0.00554 -0.00764 -0.00102 AFIX 43 H72 2 0.642711 0.064805 0.124134 11.00000 -1.20000 AFIX 0 C73 1 0.935057 -0.140382 0.180182 11.00000 0.01725 0.02283 = 0.03160 0.00458 -0.00608 0.00235 C74 1 1.002992 -0.198134 0.147783 11.00000 0.02230 0.04562 = 0.04512 -0.00949 -0.00566 -0.00318 AFIX 43 H74 2 0.975551 -0.218159 0.122866 11.00000 -1.20000 AFIX 0 C75 1 1.112088 -0.228058 0.150823 11.00000 0.02657 0.05978 = 0.05942 -0.01359 -0.00488 -0.00255 AFIX 43 H75 2 1.158519 -0.269457 0.129318 11.00000 -1.20000 AFIX 0 C76 1 1.149698 -0.195060 0.186321 11.00000 0.02360 0.04816 = 0.07790 0.00956 -0.01962 -0.00636 AFIX 43 H76 2 1.223405 -0.213629 0.188539 11.00000 -1.20000 AFIX 0 C77 1 1.083243 -0.136190 0.218409 11.00000 0.03849 0.04924 = 0.05512 0.00618 -0.02627 -0.01828 AFIX 43 H77 2 1.110965 -0.114275 0.242252 11.00000 -1.20000 AFIX 0 C78 1 0.975098 -0.109019 0.215652 11.00000 0.03387 0.02904 = 0.04971 -0.00058 -0.01224 -0.00963 AFIX 43 H78 2 0.928588 -0.068994 0.238033 11.00000 -1.20000 AFIX 0 C79 1 0.761628 -0.168188 0.142381 11.00000 0.01991 0.02463 = 0.03401 -0.00696 -0.00329 -0.00487 C80 1 0.729813 -0.150441 0.090532 11.00000 0.03122 0.04864 = 0.03058 -0.01275 0.00262 -0.01703 AFIX 43 H80 2 0.727570 -0.094399 0.067019 11.00000 -1.20000 AFIX 0 C81 1 0.701114 -0.213547 0.072437 11.00000 0.03824 0.05646 = 0.04278 -0.02291 -0.00360 -0.01588 AFIX 43 H81 2 0.678304 -0.200051 0.037160 11.00000 -1.20000 AFIX 0 C82 1 0.705961 -0.295040 0.105746 11.00000 0.02747 0.04350 = 0.08053 -0.03544 0.00109 -0.01237 AFIX 43 H82 2 0.686934 -0.338116 0.093253 11.00000 -1.20000 AFIX 0 C83 1 0.737836 -0.315031 0.156698 11.00000 0.03359 0.02451 = 0.06755 -0.01231 -0.00098 -0.00810 AFIX 43 H83 2 0.742132 -0.372091 0.179240 11.00000 -1.20000 AFIX 0 C84 1 0.764001 -0.251593 0.175501 11.00000 0.02243 0.03363 = 0.05061 -0.00405 -0.00623 -0.00769 AFIX 43 H84 2 0.783837 -0.265181 0.211490 11.00000 -1.20000 AFIX 0 HKLF 4 REM data_0m in P-1 REM R1 = 0.0430 for 19886 Fo > 4sig(Fo) and 0.0567 for all 24138 data REM 1159 parameters refined using 171 restraints END WGHT 0.0260 28.1437 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, -y, -z HTAB C2A N1D_$1 EQIV $2 x-1, y+1, z HTAB C2A N1D_$2 HTAB C2A N1F HTAB C2B O2W EQIV $3 -x+1, -y-1, -z+1 HTAB C2C O1_$3 HTAB C2E O2 EQIV $4 x, y+1, z HTAB O1W O2_$4 HTAB O1W O3 HTAB O2W O2_$4 HTAB O2W O3 HTAB O3W O1 EQIV $5 x-1, y, z HTAB O3W O4_$5 HTAB C12 O1W HTAB C14 O3W HTAB C30 S3 EQIV $6 x+1, y-1, z HTAB C84 N1B_$6 REM Highest difference peak 3.615, deepest hole -1.925, 1-sigma level 0.177 Q1 1 0.6819 -0.0408 0.2770 11.00000 0.05 3.61 Q2 1 0.5736 -0.1850 0.2605 11.00000 0.05 3.55 Q3 1 0.2280 0.0818 0.2180 11.00000 0.05 3.26 Q4 1 0.2210 0.0768 0.2898 11.00000 0.05 3.20 Q5 1 0.3187 0.2080 0.3113 11.00000 0.05 3.10 ; 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-3 7 0 0.24 0.52 2 -7 0 0.12 0.20 2 -7 0 0.05 0.24 -2 7 0 0.28 0.36 -2 7 0 0.42 0.25 1 -7 0 41.66 2.31 1 -7 0 41.50 2.12 -1 7 0 41.13 2.45 -1 7 0 43.03 2.50 0 -7 0 15.86 0.91 0 -7 0 15.67 0.97 0 7 0 16.20 1.03 0 7 0 15.94 1.05 -1 -7 0 38.07 1.90 -1 -7 0 36.06 2.04 1 7 0 36.61 2.21 1 7 0 37.66 2.17 -2 -7 0 262.47 12.83 -2 -7 0 259.58 13.93 2 7 0 283.53 14.73 2 7 0 259.18 15.03 -3 -7 0 24.10 1.31 3 7 0 25.86 1.51 3 7 0 23.76 1.53 -4 -7 0 153.54 8.04 -4 -7 0 181.48 8.72 4 7 0 156.81 9.41 4 7 0 171.37 9.27 -5 -7 0 0.62 0.23 -5 -7 0 1.31 0.24 5 7 0 1.07 0.38 5 7 0 0.32 0.30 -6 -7 0 59.14 3.09 -6 -7 0 54.30 2.90 6 7 0 58.34 3.42 -7 -7 0 15.10 0.93 -7 -7 0 14.51 0.91 7 7 0 12.94 1.13 -8 -7 0 4.25 0.51 -8 -7 0 5.33 0.56 8 7 0 4.91 0.70 -9 -7 0 6.41 0.65 -9 -7 0 5.64 0.61 9 7 0 5.11 0.77 -10 -7 0 97.50 4.95 -10 -7 0 105.05 5.28 10 7 0 89.07 5.68 -11 -7 0 153.79 8.14 -11 -7 0 150.83 7.62 -12 -7 0 -0.07 0.52 -12 -7 0 -0.79 0.49 -13 -7 0 39.34 2.36 -13 -7 0 36.40 2.35 13 7 0 38.94 2.47 -14 -7 0 1.80 0.76 -14 -7 0 1.26 0.69 13 -8 0 5.53 1.04 -13 8 0 3.98 1.08 12 -8 0 0.10 0.74 -12 8 0 0.67 0.86 11 -8 0 11.57 1.26 -11 8 0 14.58 1.47 10 -8 0 1.73 0.71 -10 8 0 2.34 0.79 9 -8 0 31.28 1.99 -9 8 0 28.13 2.07 8 -8 0 56.47 3.19 -8 8 0 52.20 3.35 7 -8 0 1.54 0.49 7 -8 0 2.17 0.39 -7 8 0 2.48 0.63 6 -8 0 0.19 0.30 6 -8 0 0.23 0.44 -6 8 0 -0.10 0.42 5 -8 0 8.09 0.64 5 -8 0 8.15 0.72 -5 8 0 7.21 0.83 4 -8 0 6.85 0.65 4 -8 0 7.17 0.55 -4 8 0 3.26 0.81 -4 8 0 6.18 0.68 3 -8 0 29.08 1.51 3 -8 0 24.85 1.66 -3 8 0 33.66 2.07 -3 8 0 26.19 1.77 1 -8 0 27.38 1.45 1 -8 0 27.39 1.57 -1 8 0 27.45 1.73 -1 8 0 26.92 1.68 0 -8 0 75.10 4.05 0 -8 0 78.74 3.76 0 8 0 75.46 4.31 0 8 0 74.07 4.38 -1 -8 0 73.48 3.62 -1 -8 0 70.56 3.90 1 8 0 72.43 4.23 1 8 0 75.99 4.15 -2 -8 0 5.96 0.60 -2 -8 0 5.86 0.51 2 8 0 5.58 0.58 2 8 0 6.80 0.57 -3 -8 0 10.59 0.69 -3 -8 0 8.84 0.95 3 8 0 11.30 0.78 3 8 0 10.38 0.82 -4 -8 0 21.48 1.29 -4 -8 0 26.04 1.44 4 8 0 24.18 1.48 4 8 0 22.61 1.51 -5 -8 0 0.71 0.25 -5 -8 0 0.14 0.23 5 8 0 0.93 0.35 5 8 0 0.37 0.33 -6 -8 0 44.79 2.35 -6 -8 0 37.79 2.21 6 8 0 42.80 2.59 6 8 0 45.60 2.63 -7 -8 0 19.88 1.26 -7 -8 0 22.25 1.29 7 8 0 22.72 1.47 7 8 0 21.46 1.54 -8 -8 0 0.44 0.30 -8 -8 0 0.78 0.35 8 8 0 0.71 0.43 8 8 0 1.11 0.51 -9 -8 0 83.13 4.24 -9 -8 0 87.88 4.51 9 8 0 83.69 4.88 9 8 0 77.62 4.91 -10 -8 0 21.55 1.37 -10 -8 0 21.21 1.36 10 8 0 18.18 1.62 10 8 0 21.50 1.50 -11 -8 0 36.23 2.14 -11 -8 0 38.78 2.23 11 8 0 35.88 2.37 -12 -8 0 0.55 0.55 -12 -8 0 0.80 0.54 12 8 0 0.50 0.58 -13 -8 0 5.32 0.83 13 8 0 5.54 0.82 -14 -8 0 0.87 0.68 14 8 0 -0.52 0.63 -15 -8 0 18.72 1.67 12 -9 0 0.17 0.78 -12 9 0 0.42 0.88 11 -9 0 2.86 0.86 -11 9 0 2.93 0.93 10 -9 0 12.46 1.27 -10 9 0 13.22 1.38 9 -9 0 4.02 0.78 -9 9 0 3.74 0.77 8 -9 0 21.15 1.53 -8 9 0 20.39 1.63 7 -9 0 0.18 0.50 -7 9 0 0.22 0.49 6 -9 0 10.36 0.94 6 -9 0 10.10 0.78 -6 9 0 10.25 1.02 5 -9 0 62.29 3.47 5 -9 0 64.05 3.13 -5 9 0 58.56 3.67 4 -9 0 2.79 0.50 4 -9 0 3.37 0.42 -4 9 0 3.21 0.56 3 -9 0 14.17 1.10 3 -9 0 14.96 0.95 -3 9 0 15.37 1.16 -3 9 0 18.60 1.49 1 -9 0 7.57 0.71 1 -9 0 8.21 0.65 -1 9 0 9.81 0.84 -1 9 0 9.04 0.76 0 -9 0 36.21 1.86 0 -9 0 34.68 1.99 0 9 0 36.06 2.17 0 9 0 34.80 2.12 -1 -9 0 126.13 6.93 -1 -9 0 137.29 6.42 1 9 0 128.81 7.50 1 9 0 133.11 7.35 -2 -9 0 13.63 0.85 -2 -9 0 13.68 0.96 2 9 0 12.10 0.95 2 9 0 13.60 0.94 -3 -9 0 25.39 1.41 -3 -9 0 22.80 1.68 3 9 0 26.23 1.64 3 9 0 27.18 1.59 -4 -9 0 62.67 3.24 -4 -9 0 66.29 3.60 4 9 0 60.77 3.77 4 9 0 67.89 3.70 -5 -9 0 1.51 0.30 -5 -9 0 0.37 0.27 5 9 0 0.75 0.34 5 9 0 -0.04 0.35 -6 -9 0 69.41 3.54 -6 -9 0 61.58 3.33 6 9 0 63.36 3.88 6 9 0 68.04 3.85 -7 -9 0 4.99 0.54 7 9 0 7.04 0.77 -8 -9 0 9.99 0.84 -8 -9 0 11.53 0.81 8 9 0 11.24 0.96 8 9 0 11.74 1.07 -9 -9 0 12.10 0.92 -9 -9 0 11.80 0.93 9 9 0 11.90 1.06 9 9 0 12.41 1.20 -10 -9 0 78.69 4.18 10 9 0 83.99 4.81 -11 -9 0 43.53 2.43 11 9 0 42.73 2.72 -12 -9 0 13.07 1.13 12 9 0 12.11 1.16 -13 -9 0 28.63 1.93 13 9 0 30.21 2.05 -14 -9 0 2.71 0.78 14 9 0 3.41 0.79 -15 -9 0 32.04 2.21 12 -10 0 4.31 1.00 -12 10 0 4.65 1.11 11 -10 0 3.85 0.91 -11 10 0 3.72 1.00 10 -10 0 6.46 0.97 -10 10 0 6.62 1.08 9 -10 0 0.46 0.64 -9 10 0 -0.47 0.67 8 -10 0 4.03 0.75 -8 10 0 4.64 0.84 7 -10 0 21.86 1.51 -7 10 0 19.76 1.61 6 -10 0 17.70 1.12 6 -10 0 18.77 1.33 -6 10 0 16.46 1.39 5 -10 0 33.05 2.00 5 -10 0 32.44 1.78 -5 10 0 31.93 2.13 4 -10 0 87.49 4.33 4 -10 0 89.15 4.75 -4 10 0 83.59 5.03 3 -10 0 1.23 0.45 3 -10 0 1.13 0.34 -3 10 0 1.01 0.47 -3 10 0 2.22 0.78 2 -10 0 1.79 0.47 2 -10 0 2.36 0.38 1 -10 0 50.89 2.70 1 -10 0 49.31 2.93 -1 10 0 58.34 3.22 -1 10 0 53.75 3.12 0 -10 0 9.22 0.71 0 -10 0 8.39 0.73 0 10 0 10.03 0.83 0 10 0 10.49 0.85 -1 -10 0 21.63 1.36 -1 -10 0 23.45 1.29 1 10 0 23.39 1.46 1 10 0 23.29 1.51 -2 -10 0 3.97 0.50 -2 -10 0 4.52 0.45 2 10 0 3.92 0.47 2 10 0 4.44 0.53 -3 -10 0 14.08 1.10 -3 -10 0 12.32 0.81 3 10 0 11.51 0.89 3 10 0 10.53 0.95 -4 -10 0 88.14 5.30 -4 -10 0 99.02 4.82 4 10 0 103.25 5.49 4 10 0 96.44 5.62 -5 -10 0 34.01 1.89 -5 -10 0 38.55 2.05 5 10 0 32.05 2.19 5 10 0 36.04 2.13 -6 -10 0 26.90 1.46 -6 -10 0 22.39 1.40 6 10 0 25.04 1.61 6 10 0 22.87 1.65 -7 -10 0 14.42 1.06 7 10 0 16.26 1.27 7 10 0 19.94 1.31 -8 -10 0 20.57 1.33 8 10 0 23.14 1.54 -9 -10 0 9.75 0.86 9 10 0 10.27 1.00 -10 -10 0 27.43 1.72 10 10 0 30.27 1.97 -11 -10 0 21.26 1.47 11 10 0 23.29 1.64 -12 -10 0 20.18 1.48 12 10 0 21.83 1.61 -13 -10 0 42.10 2.56 13 10 0 44.71 2.81 -14 -10 0 3.09 0.79 14 10 0 4.06 0.83 -15 -10 0 22.56 1.76 15 10 0 22.78 1.80 -16 -10 0 6.02 1.08 11 -11 0 4.62 0.97 -11 11 0 5.07 1.10 10 -11 0 3.87 0.85 -10 11 0 3.49 0.95 9 -11 0 -0.02 0.64 -9 11 0 -0.15 0.74 8 -11 0 3.82 0.77 -8 11 0 4.10 0.86 7 -11 0 19.53 1.41 -7 11 0 16.37 1.48 6 -11 0 125.31 6.53 -6 11 0 113.76 6.89 5 -11 0 9.13 0.79 5 -11 0 9.33 0.98 -5 11 0 9.16 0.94 4 -11 0 97.68 5.17 4 -11 0 96.60 4.72 -4 11 0 89.50 5.46 3 -11 0 34.66 1.90 3 -11 0 34.79 2.12 -3 11 0 35.55 2.24 2 -11 0 6.54 0.58 2 -11 0 6.02 0.62 -2 11 0 5.43 0.69 -2 11 0 7.40 0.93 1 -11 0 11.05 0.81 1 -11 0 9.89 0.83 -1 11 0 12.86 1.08 -1 11 0 10.91 0.92 0 -11 0 6.38 0.61 0 -11 0 5.79 0.62 0 11 0 6.04 0.68 0 11 0 5.37 0.62 -1 -11 0 15.07 0.96 -1 -11 0 14.77 1.02 1 11 0 16.37 1.16 1 11 0 14.88 1.12 -2 -11 0 77.66 3.81 -2 -11 0 72.00 4.13 2 11 0 76.77 4.34 2 11 0 76.01 4.44 -3 -11 0 125.94 5.93 -3 -11 0 106.70 6.50 3 11 0 120.08 6.91 3 11 0 125.57 6.75 -4 -11 0 30.04 1.60 4 11 0 29.23 1.77 4 11 0 25.72 1.85 -5 -11 0 217.82 10.66 5 11 0 230.05 12.19 5 11 0 208.50 12.46 -6 -11 0 10.12 0.82 6 11 0 10.99 0.89 6 11 0 10.04 0.98 -7 -11 0 26.23 1.56 7 11 0 27.64 1.82 -8 -11 0 2.86 0.49 8 11 0 3.10 0.61 -9 -11 0 51.70 2.78 9 11 0 51.86 3.19 -10 -11 0 16.54 1.18 10 11 0 16.44 1.35 -11 -11 0 7.51 0.82 11 11 0 8.51 1.01 -12 -11 0 2.27 0.64 12 11 0 3.20 0.74 -13 -11 0 16.88 1.39 13 11 0 18.15 1.50 -14 -11 0 27.22 1.96 14 11 0 30.93 2.12 -15 -11 0 4.27 0.90 15 11 0 3.92 0.92 -16 -11 0 10.32 1.25 10 -12 0 0.30 0.73 -10 12 0 0.88 0.86 9 -12 0 4.41 0.86 -9 12 0 2.27 0.89 8 -12 0 14.00 1.36 -8 12 0 14.41 1.42 7 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0 75.46 4.61 -13 -12 0 1.31 0.65 13 12 0 1.26 0.75 -14 -12 0 42.89 2.67 14 12 0 46.99 2.98 -15 -12 0 2.82 0.85 15 12 0 3.77 0.94 -16 -12 0 19.71 1.75 16 12 0 22.59 1.86 10 -13 0 -0.09 0.79 9 -13 0 -0.02 0.74 -9 13 0 0.10 0.82 8 -13 0 30.38 2.05 -8 13 0 28.18 2.19 7 -13 0 24.36 1.74 -7 13 0 21.15 1.79 6 -13 0 9.69 1.06 -6 13 0 9.69 1.14 5 -13 0 37.43 2.17 -5 13 0 30.56 2.23 4 -13 0 -0.12 0.51 4 -13 0 -0.44 0.41 -4 13 0 -0.21 0.58 3 -13 0 10.92 0.87 3 -13 0 9.43 0.97 -3 13 0 8.91 0.98 2 -13 0 0.84 0.41 2 -13 0 0.36 0.44 -2 13 0 0.13 0.53 1 -13 0 5.11 0.65 1 -13 0 5.58 0.61 -1 13 0 5.96 0.74 -1 13 0 6.81 0.93 0 -13 0 3.12 0.51 0 13 0 3.73 0.61 -1 -13 0 62.69 3.32 1 13 0 64.29 3.78 1 13 0 66.23 3.89 -2 -13 0 9.81 0.80 2 13 0 9.21 0.99 2 13 0 9.41 0.91 -3 -13 0 81.71 4.05 3 13 0 78.98 4.71 3 13 0 77.71 4.57 -4 -13 0 101.75 4.97 4 13 0 95.79 5.78 -5 -13 0 5.99 0.64 5 13 0 6.30 0.79 -6 -13 0 34.78 1.96 6 13 0 34.36 2.27 -7 -13 0 4.17 0.61 7 13 0 5.66 0.77 -8 -13 0 19.16 1.31 8 13 0 19.99 1.52 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10.84 0.97 7 14 0 11.63 1.18 -8 -14 0 18.72 1.32 8 14 0 20.03 1.59 -9 -14 0 8.69 0.88 9 14 0 9.11 1.05 -10 -14 0 3.47 0.68 10 14 0 5.13 0.87 -11 -14 0 6.09 0.81 11 14 0 6.24 0.98 -12 -14 0 0.87 0.60 12 14 0 1.28 0.79 -13 -14 0 6.40 0.90 13 14 0 7.58 1.07 -14 -14 0 0.85 0.70 14 14 0 2.41 0.91 -15 -14 0 6.32 1.04 15 14 0 8.74 1.20 8 -15 0 0.38 0.85 -8 15 0 -0.70 0.82 7 -15 0 11.62 1.28 -7 15 0 13.06 1.43 -6 15 0 15.49 1.48 -5 15 0 2.69 0.82 -4 15 0 4.67 0.87 3 -15 0 13.13 1.03 -3 15 0 11.67 1.20 2 -15 0 1.22 0.50 -2 15 0 1.01 0.65 1 -15 0 11.79 1.04 -1 15 0 15.25 1.24 0 -15 0 1.51 0.52 -1 -15 0 -0.07 0.44 1 15 0 1.34 0.70 1 15 0 0.96 0.59 -2 -15 0 31.51 1.93 2 15 0 34.32 2.19 2 15 0 35.65 2.30 -3 -15 0 30.53 1.78 3 15 0 29.64 2.08 -4 -15 0 11.51 1.00 4 15 0 12.75 1.21 -5 -15 0 15.76 1.15 5 15 0 16.08 1.39 -6 -15 0 26.69 1.60 6 15 0 24.09 1.86 -7 -15 0 5.05 0.72 7 15 0 7.03 0.96 -8 -15 0 23.44 1.59 8 15 0 26.05 1.88 -9 -15 0 3.32 0.67 9 15 0 4.90 0.89 -10 -15 0 2.47 0.65 10 15 0 2.72 0.84 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24.19 1.62 7 -6 9 22.45 1.55 -8 6 -9 3.61 0.79 -8 6 -9 3.97 0.73 8 -6 9 3.89 0.63 -9 6 -9 5.95 0.89 9 -6 9 5.69 0.81 -10 6 -9 11.43 1.27 10 -6 9 11.07 1.16 -11 6 -9 15.65 1.55 11 -6 9 16.23 1.42 -12 6 -9 20.83 1.87 12 -6 9 21.45 1.72 -13 6 -9 0.75 0.89 13 -6 9 0.81 0.82 16 5 -9 14.33 1.60 15 5 -9 0.33 0.97 -15 -5 9 0.99 0.86 14 5 -9 2.89 1.04 -14 -5 9 3.74 0.92 13 5 -9 1.12 0.90 -13 -5 9 1.02 0.74 12 5 -9 1.86 0.89 -12 -5 9 1.96 0.74 11 5 -9 5.09 1.00 -11 -5 9 6.08 0.87 -10 -5 9 -0.03 0.55 9 5 -9 20.35 1.46 -9 -5 9 21.67 1.55 -9 -5 9 20.65 1.51 8 5 -9 102.83 6.06 -8 -5 9 107.10 5.79 -8 -5 9 104.59 5.37 7 5 -9 47.92 2.91 -7 -5 9 46.25 2.62 -7 -5 9 49.61 2.89 6 5 -9 75.35 4.31 -6 -5 9 70.00 3.78 -6 -5 9 73.82 4.18 5 5 -9 68.30 4.05 -5 -5 9 71.66 3.99 -5 -5 9 65.90 3.51 4 5 -9 12.72 1.07 -4 -5 9 13.78 0.91 -4 -5 9 12.23 1.25 3 5 -9 0.50 0.44 -3 -5 9 0.89 0.57 -3 -5 9 0.34 0.28 2 5 -9 95.83 5.63 -2 -5 9 95.89 5.42 -2 -5 9 96.58 4.75 1 5 -9 35.01 2.36 1 5 -9 36.67 2.05 -1 -5 9 36.07 1.87 -1 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1.56 0.59 10 4 -9 29.32 2.02 -10 -4 9 29.18 1.96 9 4 -9 19.73 1.37 -9 -4 9 19.33 1.46 8 4 -9 14.49 1.10 -8 -4 9 15.53 1.20 -8 -4 9 13.49 1.19 7 4 -9 135.21 7.75 6 4 -9 1.15 0.43 -6 -4 9 1.11 0.51 -6 -4 9 0.67 0.41 5 4 -9 85.26 4.85 -5 -4 9 87.07 4.69 -5 -4 9 77.56 4.22 4 4 -9 8.09 0.83 -4 -4 9 8.08 0.91 -4 -4 9 8.70 0.70 3 4 -9 11.47 0.96 -3 -4 9 10.37 0.78 -3 -4 9 10.72 1.15 2 4 -9 2.56 0.50 -2 -4 9 1.89 0.32 -2 -4 9 2.14 0.63 1 4 -9 12.83 0.82 1 4 -9 15.52 1.22 -1 -4 9 12.23 0.83 -1 -4 9 15.65 1.24 0 4 -9 0.10 0.50 0 4 -9 0.23 0.17 0 -4 9 -0.25 0.38 0 -4 9 0.40 0.20 -1 4 -9 153.33 10.29 -1 4 -9 187.86 9.87 1 -4 9 191.17 8.61 1 -4 9 177.91 9.44 -2 4 -9 110.42 6.02 -2 4 -9 104.87 6.43 2 -4 9 103.19 5.76 2 -4 9 111.03 5.22 -3 4 -9 76.64 4.27 -3 4 -9 78.36 4.66 3 -4 9 73.02 4.09 3 -4 9 73.48 3.65 -4 4 -9 167.24 8.94 -4 4 -9 135.17 9.31 4 -4 9 161.49 7.69 4 -4 9 173.90 8.50 -5 4 -9 8.19 0.74 -5 4 -9 7.09 0.99 5 -4 9 8.67 0.73 -6 4 -9 18.15 1.25 -6 4 -9 17.02 1.48 6 -4 9 18.25 1.24 -7 4 -9 16.60 1.33 -7 4 -9 14.60 1.17 7 -4 9 13.78 1.11 -8 4 -9 38.28 2.48 -8 4 -9 37.67 2.39 8 -4 9 36.70 2.26 -9 4 -9 29.65 2.03 -9 4 -9 33.48 2.07 9 -4 9 27.10 1.87 -10 4 -9 33.60 2.30 10 -4 9 33.35 2.10 -11 4 -9 6.65 0.99 11 -4 9 6.65 0.88 -12 4 -9 32.22 2.31 12 -4 9 30.09 2.09 -13 4 -9 16.57 1.70 13 -4 9 18.49 1.56 -14 4 -9 15.58 1.72 14 -4 9 16.79 1.50 15 -4 9 4.22 1.06 15 3 -9 6.69 1.24 -15 -3 9 6.03 1.06 14 3 -9 0.77 0.91 -14 -3 9 1.29 0.82 13 3 -9 1.09 0.83 -13 -3 9 0.53 0.63 12 3 -9 12.65 1.32 -12 -3 9 11.13 1.12 11 3 -9 1.18 0.78 -11 -3 9 1.29 0.67 10 3 -9 59.50 3.34 -10 -3 9 55.42 3.35 9 3 -9 154.25 7.57 -9 -3 9 142.54 7.99 8 3 -9 21.25 1.47 8 3 -9 17.62 1.32 -8 -3 9 19.38 1.39 7 3 -9 61.46 3.55 -7 -3 9 58.69 3.42 6 3 -9 28.29 1.78 -6 -3 9 27.43 1.69 -6 -3 9 27.75 1.79 5 3 -9 9.90 0.85 -5 -3 9 9.11 0.84 -5 -3 9 10.33 0.89 -5 -3 9 10.07 0.67 4 3 -9 39.31 2.35 -4 -3 9 36.96 2.32 -4 -3 9 37.48 2.06 3 3 -9 4.04 0.55 -3 -3 9 3.53 0.70 -3 -3 9 4.56 0.46 2 3 -9 27.65 1.78 -2 -3 9 26.75 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32.55 2.35 -12 -6 10 35.72 2.36 -11 -6 10 40.35 2.60 10 6 -10 1.45 0.58 -10 -6 10 0.18 0.59 -10 -6 10 1.02 0.66 9 6 -10 1.98 0.59 -9 -6 10 1.13 0.59 -9 -6 10 2.07 0.68 8 6 -10 4.17 0.67 -8 -6 10 4.48 0.69 -8 -6 10 5.11 0.82 7 6 -10 3.07 0.60 -7 -6 10 3.24 0.73 -7 -6 10 2.13 0.54 6 6 -10 190.25 10.81 -6 -6 10 183.19 9.30 -6 -6 10 193.75 10.27 5 6 -10 162.49 9.00 -5 -6 10 160.56 7.72 -5 -6 10 144.27 8.56 4 6 -10 56.46 3.39 -4 -6 10 56.19 2.88 -4 -6 10 52.23 3.39 3 6 -10 219.62 12.98 -3 -6 10 236.34 12.28 -3 -6 10 226.87 11.05 2 6 -10 25.06 1.88 -2 -6 10 28.35 1.91 -2 -6 10 27.14 1.48 1 6 -10 1.77 0.65 -1 -6 10 2.63 0.65 -1 -6 10 2.39 0.34 0 6 -10 3.11 0.78 0 6 -10 3.53 0.41 0 -6 10 4.33 0.39 0 -6 10 4.48 0.64 -1 6 -10 0.88 0.26 -1 6 -10 0.84 0.73 1 -6 10 0.53 0.23 1 -6 10 1.13 0.45 -2 6 -10 39.85 2.37 -2 6 -10 37.14 2.82 2 -6 10 41.70 2.39 2 -6 10 41.79 2.04 -3 6 -10 89.94 5.50 -3 6 -10 87.24 5.02 3 -6 10 88.82 4.85 -4 6 -10 1.34 0.93 -4 6 -10 2.93 0.48 4 -6 10 2.65 0.55 -5 6 -10 62.97 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0.81 -5 -3 10 6.46 0.71 -5 -3 10 7.36 0.83 4 3 -10 55.33 3.26 -4 -3 10 52.73 2.84 -4 -3 10 53.87 3.22 3 3 -10 67.06 3.68 -3 -3 10 52.63 3.53 -3 -3 10 62.27 3.14 2 3 -10 32.90 2.10 -2 -3 10 31.62 1.72 -2 -3 10 29.83 2.08 1 3 -10 246.16 14.79 -1 -3 10 273.94 14.33 -1 -3 10 256.83 12.53 -1 -3 10 258.80 13.79 0 3 -10 87.91 5.75 0 -3 10 103.86 4.76 0 -3 10 97.46 5.33 -1 3 -10 20.09 1.19 -1 3 -10 16.74 1.54 1 -3 10 19.49 1.29 1 -3 10 19.04 1.05 -2 3 -10 5.70 0.53 -2 3 -10 5.32 0.88 2 -3 10 5.34 0.58 2 -3 10 5.49 0.43 -3 3 -10 11.23 0.81 -3 3 -10 9.65 1.13 3 -3 10 10.70 0.61 3 -3 10 10.62 0.80 -4 3 -10 19.18 1.70 -4 3 -10 21.15 1.38 4 -3 10 22.76 1.35 -5 3 -10 17.67 1.23 -5 3 -10 16.29 1.52 5 -3 10 19.27 1.22 -6 3 -10 3.84 0.53 -6 3 -10 3.17 0.70 6 -3 10 3.98 0.54 -7 3 -10 14.96 1.28 -7 3 -10 14.51 1.12 7 -3 10 12.20 1.04 -8 3 -10 33.31 2.20 -8 3 -10 35.15 2.29 8 -3 10 33.22 2.06 -9 3 -10 5.15 0.75 -9 3 -10 4.62 0.70 9 -3 10 3.78 0.59 -10 3 -10 24.39 1.68 -10 3 -10 22.44 1.72 10 -3 10 20.52 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