Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Clara Vinas' _publ_contact_author_address ; Campus de la UAB Institut de Ciencia de Materials de Barcelona Bellaterra E-08193 SPAIN ; _publ_contact_author_email CLARA@ICMAB.ES _publ_section_title ; Synthesis, Reactivity and Complexation Studies of N,S Exo-heterodisubstituted o-Carborane Ligands. Carborane as a platform to produce the uncommon bidentate chelating (pyridine)N-C-C-C-S(H) motif ; loop_ _publ_author_name 'Clara Vinas' 'H. Horakova' 'R. Kivekas' 'Anna Laromaine' 'Reijo Sillanpaa' ; F.Teixidor ; 'Radim Vespalec' data_[NMe4]5 _database_code_depnum_ccdc_archive 'CCDC 663535' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C10 H21 B9 N S, C4 H12 N' _chemical_formula_sum 'C14 H33 B9 N2 S' _chemical_formula_weight 358.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.0020(9) _cell_length_b 14.9136(14) _cell_length_c 15.8719(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2130.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3878 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 26.022 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.152 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_type Mok\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_decay_% <1 _diffrn_reflns_number 7361 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 26.01 _reflns_number_total 4147 _reflns_number_gt 3519 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowsky & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowsky & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0641P)^2^+0.7899P] 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 SHELXL _refine_ls_extinction_coef 0.021(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(9) _refine_ls_number_reflns 4147 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0618 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.12638(7) 0.42835(4) 0.88623(4) 0.03317(18) Uani 1 d . . . B1 B 0.0740(4) 0.3626(2) 0.6236(2) 0.0426(8) Uani 1 d . . . H1 H 0.1335 0.3196 0.5766 0.051 Uiso 1 calc R . . B2 B -0.1000(4) 0.3310(2) 0.6671(2) 0.0386(8) Uani 1 d . . . H2 H -0.1554 0.2660 0.6506 0.046 Uiso 1 calc R . . B3 B 0.0607(4) 0.3346(2) 0.7305(2) 0.0435(8) Uani 1 d . . . H3 H 0.1100 0.2719 0.7573 0.052 Uiso 1 calc R . . B4 B 0.1708(3) 0.4249(2) 0.6999(2) 0.0394(7) Uani 1 d . . . H4 H 0.2949 0.4221 0.7043 0.047 Uiso 1 calc R . . B5 B 0.0779(4) 0.4828(2) 0.6179(2) 0.0420(8) Uani 1 d . . . H5 H 0.1409 0.5190 0.5675 0.050 Uiso 1 calc R . . B6 B -0.0932(4) 0.4224(2) 0.5984(2) 0.0410(7) Uani 1 d . . . H6 H -0.1461 0.4176 0.5347 0.049 Uiso 1 calc R . . C7 C -0.1022(3) 0.38441(16) 0.76295(16) 0.0293(5) Uani 1 d . . . C8 C 0.0513(3) 0.43482(18) 0.78222(16) 0.0329(6) Uani 1 d . . . B9 B 0.0676(4) 0.5254(2) 0.7235(2) 0.0361(7) Uani 1 d . . . H9 H 0.127(3) 0.5819(19) 0.7486(17) 0.043 Uiso 1 d . . . B10 B -0.0940(4) 0.5267(2) 0.6533(2) 0.0385(7) Uani 1 d . . . H10A H -0.137(3) 0.5894(19) 0.6262(18) 0.046 Uiso 1 d . . . H10B H -0.092(3) 0.5107(19) 0.7436(18) 0.046 Uiso 1 d . . . B11 B -0.1990(3) 0.4314(2) 0.68973(19) 0.0340(6) Uani 1 d . . . H11 H -0.326(3) 0.4286(19) 0.6908(17) 0.041 Uiso 1 d . . . C13 C -0.1847(3) 0.34306(16) 0.83612(16) 0.0297(6) Uani 1 d . . . N14 N -0.2955(3) 0.39346(15) 0.86736(14) 0.0371(5) Uani 1 d . . . C15 C -0.3729(3) 0.36042(18) 0.93214(18) 0.0425(7) Uani 1 d . . . H15 H -0.4507 0.3961 0.9548 0.051 Uiso 1 calc R . . C16 C -0.3469(3) 0.27811(18) 0.96808(19) 0.0416(7) Uani 1 d . . . H16 H -0.4055 0.2572 1.0138 0.050 Uiso 1 calc R . . C17 C -0.2330(3) 0.22681(18) 0.93558(19) 0.0389(7) Uani 1 d . . . H17 H -0.2112 0.1697 0.9590 0.047 Uiso 1 calc R . . C18 C -0.1514(3) 0.25927(16) 0.86892(17) 0.0335(6) Uani 1 d . . . H18 H -0.0730 0.2246 0.8456 0.040 Uiso 1 calc R . . C19 C 0.0001(3) 0.49928(17) 0.94768(17) 0.0354(6) Uani 1 d . . . H19 H -0.1000 0.4971 0.9205 0.042 Uiso 1 calc R . . C20 C -0.0133(3) 0.4588(2) 1.03546(18) 0.0439(7) Uani 1 d . . . H20A H 0.0846 0.4580 1.0625 0.066 Uiso 1 calc R . . H20B H -0.0513 0.3974 1.0311 0.066 Uiso 1 calc R . . H20C H -0.0819 0.4950 1.0693 0.066 Uiso 1 calc R . . C21 C 0.0490(4) 0.59658(18) 0.9515(2) 0.0475(7) Uani 1 d . . . H21A H -0.0245 0.6315 0.9830 0.071 Uiso 1 calc R . . H21B H 0.0573 0.6205 0.8941 0.071 Uiso 1 calc R . . H21C H 0.1456 0.6006 0.9796 0.071 Uiso 1 calc R . . N22 N 0.5409(3) 0.65666(15) 0.82315(15) 0.0378(5) Uani 1 d . . . C23 C 0.5141(5) 0.7411(2) 0.8699(4) 0.0959(17) Uani 1 d . . . H23A H 0.5965 0.7827 0.8598 0.144 Uiso 1 calc R . . H23B H 0.5070 0.7282 0.9303 0.144 Uiso 1 calc R . . H23C H 0.4211 0.7683 0.8505 0.144 Uiso 1 calc R . . C24 C 0.5315(6) 0.6674(4) 0.7320(2) 0.1069(19) Uani 1 d . . . H24A H 0.5404 0.6086 0.7049 0.160 Uiso 1 calc R . . H24B H 0.6122 0.7064 0.7127 0.160 Uiso 1 calc R . . H24C H 0.4357 0.6943 0.7173 0.160 Uiso 1 calc R . . C25 C 0.6960(4) 0.6269(2) 0.8447(2) 0.0510(8) Uani 1 d . . . H25A H 0.7127 0.5664 0.8227 0.076 Uiso 1 calc R . . H25B H 0.7086 0.6267 0.9060 0.076 Uiso 1 calc R . . H25C H 0.7678 0.6684 0.8193 0.076 Uiso 1 calc R . . C26 C 0.4378(4) 0.5857(2) 0.8540(3) 0.0663(10) Uani 1 d . . . H26A H 0.3352 0.6028 0.8409 0.099 Uiso 1 calc R . . H26B H 0.4489 0.5791 0.9151 0.099 Uiso 1 calc R . . H26C H 0.4613 0.5287 0.8264 0.099 Uiso 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 S 0.0293(3) 0.0348(3) 0.0354(3) 0.0027(3) -0.0016(3) 0.0035(3) B1 0.0406(17) 0.0490(18) 0.0381(18) 0.0005(15) 0.0077(15) 0.0034(14) B2 0.0391(19) 0.0381(16) 0.0386(17) -0.0083(14) 0.0027(14) 0.0004(14) B3 0.0412(18) 0.0430(18) 0.046(2) -0.0021(15) 0.0046(16) 0.0066(15) B4 0.0316(15) 0.0465(17) 0.0402(17) 0.0021(15) 0.0077(12) 0.0040(15) B5 0.0390(17) 0.0500(18) 0.0371(16) 0.0060(16) 0.0066(15) -0.0030(14) B6 0.0426(17) 0.0470(17) 0.0333(16) -0.0057(15) 0.0031(12) -0.0018(16) C7 0.0263(13) 0.0283(12) 0.0333(13) -0.0035(10) 0.0030(10) 0.0011(10) C8 0.0277(12) 0.0337(13) 0.0372(14) 0.0010(12) 0.0030(11) 0.0003(12) B9 0.0319(15) 0.0362(16) 0.0402(17) 0.0077(14) -0.0015(14) -0.0046(13) B10 0.0401(19) 0.0382(16) 0.0372(16) 0.0044(14) 0.0006(14) 0.0001(14) B11 0.0338(15) 0.0347(14) 0.0335(15) -0.0016(14) -0.0009(12) 0.0009(14) C13 0.0305(13) 0.0265(12) 0.0322(13) -0.0011(11) 0.0001(10) -0.0035(11) N14 0.0373(12) 0.0315(10) 0.0424(14) 0.0008(10) 0.0110(10) 0.0026(10) C15 0.0408(15) 0.0395(14) 0.0473(16) 0.0020(12) 0.0131(15) 0.0024(14) C16 0.0440(18) 0.0389(15) 0.0418(16) 0.0025(12) 0.0053(13) -0.0072(13) C17 0.0402(15) 0.0316(13) 0.0449(17) 0.0065(12) -0.0014(13) -0.0063(12) C18 0.0318(13) 0.0278(12) 0.0409(15) -0.0002(10) -0.0016(12) 0.0000(11) C19 0.0312(13) 0.0360(13) 0.0388(14) 0.0009(11) -0.0036(11) 0.0020(11) C20 0.0421(16) 0.0512(16) 0.0384(15) -0.0020(13) 0.0066(13) 0.0052(13) C21 0.0512(18) 0.0371(15) 0.0541(18) -0.0063(13) -0.0003(15) 0.0030(13) N22 0.0350(12) 0.0401(12) 0.0384(13) 0.0013(10) -0.0021(10) -0.0013(11) C23 0.064(2) 0.047(2) 0.176(5) -0.015(3) 0.014(3) 0.0127(19) C24 0.091(4) 0.184(6) 0.046(3) 0.034(3) -0.016(2) -0.010(4) C25 0.0399(16) 0.0551(18) 0.058(2) 0.0064(16) 0.0001(15) 0.0034(15) C26 0.0524(19) 0.069(2) 0.078(2) 0.0088(19) -0.0067(18) -0.0256(18) _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 S C8 1.786(3) . ? S C19 1.834(3) . ? B1 B3 1.751(5) . ? B1 B4 1.758(5) . ? B1 B2 1.775(5) . ? B1 B6 1.795(5) . ? B1 B5 1.795(5) . ? B1 H1 1.1200 . ? B2 C7 1.717(4) . ? B2 B6 1.747(5) . ? B2 B3 1.763(5) . ? B2 B11 1.780(4) . ? B2 H2 1.1200 . ? B3 C8 1.707(4) . ? B3 C7 1.722(4) . ? B3 B4 1.741(5) . ? B3 H3 1.1200 . ? B4 C8 1.699(4) . ? B4 B5 1.771(5) . ? B4 B9 1.802(5) . ? B4 H4 1.1200 . ? B5 B10 1.772(5) . ? B5 B9 1.794(5) . ? B5 B6 1.810(5) . ? B5 H5 1.1200 . ? B6 B11 1.739(4) . ? B6 B10 1.783(5) . ? B6 H6 1.1200 . ? C7 C13 1.510(3) . ? C7 C8 1.603(3) . ? C7 B11 1.613(4) . ? C8 B9 1.648(4) . ? B9 B10 1.832(5) . ? B9 H9 1.07(3) . ? B9 H10B 1.49(3) . ? B10 B11 1.802(4) . ? B10 H10A 1.10(3) . ? B10 H10B 1.45(3) . ? B11 H11 1.15(3) . ? C13 N14 1.343(3) . ? C13 C18 1.387(3) . ? N14 C15 1.336(3) . ? C15 C16 1.374(4) . ? C15 H15 0.9500 . ? C16 C17 1.379(4) . ? C16 H16 0.9500 . ? C17 C18 1.376(4) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C21 1.517(4) . ? C19 C20 1.523(4) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? N22 C24 1.457(4) . ? N22 C23 1.482(5) . ? N22 C26 1.490(4) . ? N22 C25 1.504(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 C8 S C19 103.05(12) . . ? B3 B1 B4 59.5(2) . . ? B3 B1 B2 60.0(2) . . ? B4 B1 B2 108.1(2) . . ? B3 B1 B6 106.1(2) . . ? B4 B1 B6 107.8(2) . . ? B2 B1 B6 58.60(18) . . ? B3 B1 B5 106.7(3) . . ? B4 B1 B5 59.78(19) . . ? B2 B1 B5 107.6(2) . . ? B6 B1 B5 60.56(19) . . ? B3 B1 H1 122.8 . . ? B4 B1 H1 121.6 . . ? B2 B1 H1 122.0 . . ? B6 B1 H1 122.5 . . ? B5 B1 H1 121.9 . . ? C7 B2 B6 101.0(2) . . ? C7 B2 B3 59.30(17) . . ? B6 B2 B3 107.6(2) . . ? C7 B2 B1 103.4(2) . . ? B6 B2 B1 61.26(19) . . ? B3 B2 B1 59.3(2) . . ? C7 B2 B11 54.90(16) . . ? B6 B2 B11 59.08(18) . . ? B3 B2 B11 105.6(2) . . ? B1 B2 B11 107.3(2) . . ? C7 B2 H2 127.1 . . ? B6 B2 H2 123.0 . . ? B3 B2 H2 121.7 . . ? B1 B2 H2 122.1 . . ? B11 B2 H2 123.5 . . ? C8 B3 C7 55.73(15) . . ? C8 B3 B4 59.03(18) . . ? C7 B3 B4 103.6(2) . . ? C8 B3 B1 105.1(2) . . ? C7 B3 B1 104.2(2) . . ? B4 B3 B1 60.4(2) . . ? C8 B3 B2 105.1(2) . . ? C7 B3 B2 59.03(18) . . ? B4 B3 B2 109.4(3) . . ? B1 B3 B2 60.7(2) . . ? C8 B3 H3 124.7 . . ? C7 B3 H3 125.7 . . ? B4 B3 H3 121.8 . . ? B1 B3 H3 122.7 . . ? B2 B3 H3 121.1 . . ? C8 B4 B3 59.47(18) . . ? C8 B4 B1 105.2(2) . . ? B3 B4 B1 60.0(2) . . ? C8 B4 B5 102.9(2) . . ? B3 B4 B5 108.2(2) . . ? B1 B4 B5 61.16(19) . . ? C8 B4 B9 56.06(17) . . ? B3 B4 B9 106.9(2) . . ? B1 B4 B9 109.1(2) . . ? B5 B4 B9 60.28(19) . . ? C8 B4 H4 125.9 . . ? B3 B4 H4 121.4 . . ? B1 B4 H4 121.1 . . ? B5 B4 H4 122.4 . . ? B9 B4 H4 122.2 . . ? B4 B5 B10 111.1(2) . . ? B4 B5 B9 60.72(19) . . ? B10 B5 B9 61.81(18) . . ? B4 B5 B1 59.06(19) . . ? B10 B5 B1 109.6(2) . . ? B9 B5 B1 107.8(2) . . ? B4 B5 B6 106.6(2) . . ? B10 B5 B6 59.68(18) . . ? B9 B5 B6 107.0(2) . . ? B1 B5 B6 59.71(19) . . ? B4 B5 H5 121.4 . . ? B10 B5 H5 119.4 . . ? B9 B5 H5 121.5 . . ? B1 B5 H5 121.8 . . ? B6 B5 H5 123.3 . . ? B11 B6 B2 61.38(18) . . ? B11 B6 B10 61.52(18) . . ? B2 B6 B10 112.1(2) . . ? B11 B6 B1 108.2(2) . . ? B2 B6 B1 60.14(19) . . ? B10 B6 B1 109.2(2) . . ? B11 B6 B5 106.6(2) . . ? B2 B6 B5 108.1(2) . . ? B10 B6 B5 59.09(18) . . ? B1 B6 B5 59.73(18) . . ? B11 B6 H6 121.6 . . ? B2 B6 H6 119.8 . . ? B10 B6 H6 119.8 . . ? B1 B6 H6 121.7 . . ? B5 B6 H6 123.3 . . ? C13 C7 C8 118.0(2) . . ? C13 C7 B11 117.8(2) . . ? C8 C7 B11 113.5(2) . . ? C13 C7 B2 119.8(2) . . ? C8 C7 B2 112.1(2) . . ? B11 C7 B2 64.52(18) . . ? C13 C7 B3 118.2(2) . . ? C8 C7 B3 61.64(18) . . ? B11 C7 B3 115.6(2) . . ? B2 C7 B3 61.67(18) . . ? C7 C8 B9 110.7(2) . . ? C7 C8 B4 111.0(2) . . ? B9 C8 B4 65.14(19) . . ? C7 C8 B3 62.63(17) . . ? B9 C8 B3 116.2(2) . . ? B4 C8 B3 61.50(19) . . ? C7 C8 S 118.51(18) . . ? B9 C8 S 122.2(2) . . ? B4 C8 S 117.80(18) . . ? B3 C8 S 112.23(19) . . ? C8 B9 B5 104.0(2) . . ? C8 B9 B4 58.79(17) . . ? B5 B9 B4 59.00(18) . . ? C8 B9 B10 106.4(2) . . ? B5 B9 B10 58.49(18) . . ? B4 B9 B10 107.0(2) . . ? C8 B9 H9 118.6(15) . . ? B5 B9 H9 126.8(15) . . ? B4 B9 H9 118.4(16) . . ? B10 B9 H9 127.6(15) . . ? C8 B9 H10B 70.8(11) . . ? B5 B9 H10B 101.4(12) . . ? B4 B9 H10B 114.8(11) . . ? B10 B9 H10B 50.6(11) . . ? H9 B9 H10B 121(2) . . ? B5 B10 B6 61.23(18) . . ? B5 B10 B11 105.5(2) . . ? B6 B10 B11 58.04(17) . . ? B5 B10 B9 59.69(19) . . ? B6 B10 B9 106.5(2) . . ? B11 B10 B9 102.3(2) . . ? B5 B10 H10A 119.9(16) . . ? B6 B10 H10A 123.5(15) . . ? B11 B10 H10A 127.6(16) . . ? B9 B10 H10A 121.8(16) . . ? B5 B10 H10B 103.9(12) . . ? B6 B10 H10B 109.8(12) . . ? B11 B10 H10B 64.0(12) . . ? B9 B10 H10B 52.3(12) . . ? H10A B10 H10B 122.1(19) . . ? C7 B11 B6 105.7(2) . . ? C7 B11 B2 60.59(18) . . ? B6 B11 B2 59.54(18) . . ? C7 B11 B10 106.9(2) . . ? B6 B11 B10 60.44(18) . . ? B2 B11 B10 109.7(2) . . ? C7 B11 H11 120.9(14) . . ? B6 B11 H11 123.8(14) . . ? B2 B11 H11 118.2(15) . . ? B10 B11 H11 123.9(15) . . ? N14 C13 C18 121.7(2) . . ? N14 C13 C7 114.9(2) . . ? C18 C13 C7 123.4(2) . . ? C15 N14 C13 117.7(2) . . ? N14 C15 C16 124.1(3) . . ? N14 C15 H15 118.0 . . ? C16 C15 H15 118.0 . . ? C15 C16 C17 117.8(3) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C18 C17 C16 119.3(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C13 119.4(3) . . ? C17 C18 H18 120.3 . . ? C13 C18 H18 120.3 . . ? C21 C19 C20 111.5(2) . . ? C21 C19 S 113.2(2) . . ? C20 C19 S 107.89(18) . . ? C21 C19 H19 108.1 . . ? C20 C19 H19 108.1 . . ? S C19 H19 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 N22 C23 113.2(4) . . ? C24 N22 C26 111.6(3) . . ? C23 N22 C26 109.7(3) . . ? C24 N22 C25 108.1(3) . . ? C23 N22 C25 106.7(3) . . ? C26 N22 C25 107.1(2) . . ? N22 C23 H23A 109.5 . . ? N22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N22 C24 H24A 109.5 . . ? N22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N22 C25 H25A 109.5 . . ? N22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N22 C26 H26A 109.5 . . ? N22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 S C7 C8 C13 -7.0(3) . . . . ? N14 C13 C7 C8 97.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C19 H19 N14 1.00 2.49 3.346(4) 143.5 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.437 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.046 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 663536' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C25 H29 B10 Cl N P Pd S' _chemical_formula_sum 'C25 H29 B10 Cl N P Pd S' _chemical_formula_weight 656.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3314(4) _cell_length_b 11.9503(6) _cell_length_c 15.2810(4) _cell_angle_alpha 104.695(2) _cell_angle_beta 98.904(2) _cell_angle_gamma 111.702(2) _cell_volume 1471.71(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4435 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 24.407 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 2003)' _exptl_absorpt_correction_T_min 0.778 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_type Mok\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_decay_% <1 _diffrn_reflns_number 13045 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 24.37 _reflns_number_total 4805 _reflns_number_gt 3910 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0183P)^2^+1.3958P] 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 4805 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0693 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.63560(3) 0.37632(2) 0.195573(16) 0.01641(9) Uani 1 d . . . Cl Cl 0.62469(10) 0.35032(8) 0.03770(5) 0.0240(2) Uani 1 d . . . S S 0.62440(10) 0.39501(8) 0.34792(5) 0.0202(2) Uani 1 d . . . P P 0.75492(9) 0.58938(8) 0.23925(5) 0.01524(19) Uani 1 d . . . C1 C 0.3178(4) 0.1567(3) 0.2435(2) 0.0202(8) Uani 1 d . . . C2 C 0.4136(4) 0.3073(3) 0.3242(2) 0.0192(7) Uani 1 d . . . B3 B 0.2878(5) 0.2800(4) 0.2174(3) 0.0213(9) Uani 1 d . . . H3 H 0.3314 0.3179 0.1619 0.026 Uiso 1 calc R . . B4 B 0.1267(5) 0.1282(4) 0.1882(3) 0.0269(10) Uani 1 d . . . H4 H 0.0625 0.0661 0.1130 0.032 Uiso 1 calc R . . B5 B 0.1623(5) 0.0627(4) 0.2776(3) 0.0270(10) Uani 1 d . . . H5 H 0.1209 -0.0429 0.2615 0.032 Uiso 1 calc R . . B6 B 0.3475(5) 0.1757(4) 0.3617(2) 0.0236(9) Uani 1 d . . . H6 H 0.4299 0.1451 0.4005 0.028 Uiso 1 calc R . . B7 B 0.2880(5) 0.3817(4) 0.3251(3) 0.0230(9) Uani 1 d . . . H7 H 0.3298 0.4872 0.3406 0.028 Uiso 1 calc R . . B8 B 0.1035(5) 0.2677(4) 0.2407(3) 0.0289(10) Uani 1 d . . . H8 H 0.0222 0.2980 0.2006 0.035 Uiso 1 calc R . . B9 B 0.0263(5) 0.1335(4) 0.2780(3) 0.0337(11) Uani 1 d . . . H9 H -0.1058 0.0749 0.2626 0.040 Uiso 1 calc R . . B10 B 0.1650(5) 0.1640(4) 0.3856(3) 0.0293(10) Uani 1 d . . . H10 H 0.1248 0.1258 0.4416 0.035 Uiso 1 calc R . . B11 B 0.3261(5) 0.3167(4) 0.4146(3) 0.0242(9) Uani 1 d . . . H11 H 0.3936 0.3794 0.4893 0.029 Uiso 1 calc R . . B12 B 0.1264(5) 0.2904(4) 0.3628(3) 0.0313(10) Uani 1 d . . . H12 H 0.0603 0.3355 0.4036 0.038 Uiso 1 calc R . . C13 C 0.4187(4) 0.1009(3) 0.1957(2) 0.0226(8) Uani 1 d . . . N14 N 0.5323(3) 0.1731(3) 0.16448(18) 0.0211(6) Uani 1 d . . . C15 C 0.6206(4) 0.1211(4) 0.1223(2) 0.0287(9) Uani 1 d . . . H15 H 0.7012 0.1722 0.0998 0.034 Uiso 1 calc R . . C16 C 0.5993(5) -0.0021(4) 0.1104(2) 0.0349(10) Uani 1 d . . . H16 H 0.6627 -0.0361 0.0797 0.042 Uiso 1 calc R . . C17 C 0.4843(5) -0.0753(4) 0.1439(3) 0.0424(11) Uani 1 d . . . H17 H 0.4678 -0.1606 0.1377 0.051 Uiso 1 calc R . . C18 C 0.3929(5) -0.0231(4) 0.1867(3) 0.0362(10) Uani 1 d . . . H18 H 0.3123 -0.0726 0.2100 0.043 Uiso 1 calc R . . C19 C 0.8353(4) 0.6554(3) 0.1528(2) 0.0167(7) Uani 1 d . . . C20 C 0.9541(4) 0.6253(4) 0.1229(2) 0.0263(8) Uani 1 d . . . H20 H 0.9903 0.5722 0.1478 0.032 Uiso 1 calc R . . C21 C 1.0202(4) 0.6719(4) 0.0572(2) 0.0295(9) Uani 1 d . . . H21 H 1.1022 0.6518 0.0378 0.035 Uiso 1 calc R . . C22 C 0.9661(4) 0.7477(4) 0.0203(2) 0.0277(8) Uani 1 d . . . H22 H 1.0111 0.7800 -0.0247 0.033 Uiso 1 calc R . . C23 C 0.8470(4) 0.7765(3) 0.0485(2) 0.0282(9) Uani 1 d . . . H23 H 0.8095 0.8280 0.0223 0.034 Uiso 1 calc R . . C24 C 0.7816(4) 0.7311(3) 0.1147(2) 0.0229(8) Uani 1 d . . . H24 H 0.6998 0.7518 0.1340 0.027 Uiso 1 calc R . . C25 C 0.9273(4) 0.6661(3) 0.3420(2) 0.0180(7) Uani 1 d . . . C26 C 0.9913(4) 0.5931(3) 0.3777(2) 0.0226(8) Uani 1 d . . . H26 H 0.9426 0.5025 0.3495 0.027 Uiso 1 calc R . . C27 C 1.1267(4) 0.6530(4) 0.4548(2) 0.0302(9) Uani 1 d . . . H27 H 1.1706 0.6031 0.4789 0.036 Uiso 1 calc R . . C28 C 1.1970(4) 0.7833(4) 0.4961(2) 0.0347(10) Uani 1 d . . . H28 H 1.2875 0.8233 0.5497 0.042 Uiso 1 calc R . . C29 C 1.1369(4) 0.8571(4) 0.4602(2) 0.0333(9) Uani 1 d . . . H29 H 1.1873 0.9476 0.4886 0.040 Uiso 1 calc R . . C30 C 1.0032(4) 0.7992(3) 0.3826(2) 0.0243(8) Uani 1 d . . . H30 H 0.9635 0.8502 0.3572 0.029 Uiso 1 calc R . . C31 C 0.6048(4) 0.6463(3) 0.2611(2) 0.0163(7) Uani 1 d . . . C32 C 0.6145(4) 0.7293(3) 0.3460(2) 0.0228(8) Uani 1 d . . . H32 H 0.7078 0.7637 0.3974 0.027 Uiso 1 calc R . . C33 C 0.4892(4) 0.7621(4) 0.3566(2) 0.0295(9) Uani 1 d . . . H33 H 0.4976 0.8200 0.4148 0.035 Uiso 1 calc R . . C34 C 0.3527(4) 0.7115(4) 0.2832(2) 0.0287(9) Uani 1 d . . . H34 H 0.2667 0.7339 0.2910 0.034 Uiso 1 calc R . . C35 C 0.3404(4) 0.6277(4) 0.1980(2) 0.0271(8) Uani 1 d . . . H35 H 0.2460 0.5929 0.1474 0.033 Uiso 1 calc R . . C36 C 0.4651(4) 0.5948(3) 0.1863(2) 0.0220(8) Uani 1 d . . . H36 H 0.4564 0.5373 0.1278 0.026 Uiso 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 Pd 0.01598(14) 0.01883(15) 0.01688(14) 0.00821(10) 0.00667(10) 0.00777(11) Cl 0.0290(5) 0.0273(5) 0.0137(4) 0.0064(3) 0.0096(3) 0.0089(4) S 0.0178(4) 0.0238(5) 0.0161(4) 0.0094(4) 0.0039(3) 0.0046(4) P 0.0121(4) 0.0199(5) 0.0166(4) 0.0097(4) 0.0055(3) 0.0069(4) C1 0.0207(18) 0.0167(18) 0.0187(17) 0.0072(14) 0.0044(14) 0.0027(15) C2 0.0193(17) 0.0201(19) 0.0154(16) 0.0075(14) 0.0050(14) 0.0044(15) B3 0.021(2) 0.022(2) 0.022(2) 0.0100(17) 0.0051(16) 0.0086(18) B4 0.019(2) 0.029(2) 0.026(2) 0.0125(19) 0.0020(17) 0.0032(18) B5 0.024(2) 0.023(2) 0.026(2) 0.0125(18) 0.0056(18) -0.0010(18) B6 0.028(2) 0.023(2) 0.017(2) 0.0119(17) 0.0054(17) 0.0046(18) B7 0.026(2) 0.026(2) 0.023(2) 0.0115(18) 0.0129(17) 0.0132(19) B8 0.020(2) 0.038(3) 0.032(2) 0.017(2) 0.0093(18) 0.012(2) B9 0.024(2) 0.037(3) 0.033(2) 0.015(2) 0.0066(19) 0.004(2) B10 0.029(2) 0.029(2) 0.026(2) 0.0127(19) 0.0104(18) 0.005(2) B11 0.026(2) 0.027(2) 0.020(2) 0.0106(18) 0.0107(17) 0.0092(19) B12 0.026(2) 0.036(3) 0.035(2) 0.017(2) 0.0171(19) 0.010(2) C13 0.0285(19) 0.0176(19) 0.0173(17) 0.0056(14) 0.0020(15) 0.0073(16) N14 0.0238(15) 0.0203(16) 0.0224(15) 0.0086(12) 0.0071(12) 0.0115(13) C15 0.031(2) 0.032(2) 0.031(2) 0.0125(17) 0.0123(17) 0.0194(18) C16 0.050(3) 0.036(2) 0.030(2) 0.0091(18) 0.0146(19) 0.031(2) C17 0.066(3) 0.026(2) 0.041(2) 0.0109(19) 0.017(2) 0.025(2) C18 0.049(3) 0.022(2) 0.038(2) 0.0126(18) 0.0176(19) 0.0105(19) C19 0.0132(16) 0.0195(18) 0.0169(16) 0.0091(14) 0.0043(13) 0.0046(14) C20 0.0204(18) 0.036(2) 0.033(2) 0.0218(17) 0.0114(16) 0.0150(17) C21 0.0220(19) 0.044(2) 0.032(2) 0.0196(18) 0.0167(16) 0.0157(18) C22 0.028(2) 0.037(2) 0.0223(18) 0.0176(17) 0.0134(15) 0.0112(18) C23 0.034(2) 0.031(2) 0.0297(19) 0.0202(17) 0.0113(17) 0.0170(18) C24 0.0250(19) 0.029(2) 0.0252(18) 0.0148(16) 0.0128(15) 0.0164(17) C25 0.0096(15) 0.030(2) 0.0164(16) 0.0122(15) 0.0059(13) 0.0065(15) C26 0.0172(17) 0.031(2) 0.0251(18) 0.0170(16) 0.0094(15) 0.0102(16) C27 0.0222(19) 0.053(3) 0.030(2) 0.0283(19) 0.0123(16) 0.0204(19) C28 0.0163(19) 0.058(3) 0.0230(19) 0.0121(19) 0.0020(15) 0.0113(19) C29 0.0212(19) 0.035(2) 0.030(2) 0.0022(17) 0.0032(16) 0.0041(18) C30 0.0185(18) 0.027(2) 0.0280(19) 0.0117(16) 0.0087(15) 0.0087(16) C31 0.0140(16) 0.0215(19) 0.0225(17) 0.0163(15) 0.0098(13) 0.0096(15) C32 0.0219(18) 0.028(2) 0.0227(18) 0.0125(16) 0.0105(15) 0.0111(16) C33 0.032(2) 0.031(2) 0.032(2) 0.0120(17) 0.0183(17) 0.0170(18) C34 0.026(2) 0.040(2) 0.044(2) 0.0278(19) 0.0230(17) 0.0241(18) C35 0.0188(18) 0.044(2) 0.032(2) 0.0259(18) 0.0111(15) 0.0164(17) C36 0.0200(18) 0.031(2) 0.0214(17) 0.0153(15) 0.0089(14) 0.0116(16) _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 Pd N14 2.143(3) . ? Pd P 2.2314(9) . ? Pd S 2.3041(8) . ? Pd Cl 2.3339(8) . ? S C2 1.778(3) . ? P C31 1.809(3) . ? P C25 1.814(3) . ? P C19 1.825(3) . ? C1 C13 1.516(5) . ? C1 C2 1.703(4) . ? C1 B4 1.717(5) . ? C1 B5 1.722(5) . ? C1 B3 1.725(5) . ? C1 B6 1.727(4) . ? C2 B11 1.710(5) . ? C2 B7 1.712(5) . ? C2 B3 1.733(4) . ? C2 B6 1.741(5) . ? B3 B4 1.765(5) . ? B3 B8 1.771(6) . ? B3 B7 1.780(5) . ? B3 H3 1.1200 . ? B4 B8 1.765(6) . ? B4 B9 1.779(6) . ? B4 B5 1.785(5) . ? B4 H4 1.1200 . ? B5 B9 1.767(6) . ? B5 B10 1.773(6) . ? B5 B6 1.780(5) . ? B5 H5 1.1200 . ? B6 B10 1.760(6) . ? B6 B11 1.773(6) . ? B6 H6 1.1200 . ? B7 B12 1.780(6) . ? B7 B8 1.780(6) . ? B7 B11 1.787(5) . ? B7 H7 1.1200 . ? B8 B9 1.776(6) . ? B8 B12 1.783(5) . ? B8 H8 1.1200 . ? B9 B12 1.779(6) . ? B9 B10 1.788(6) . ? B9 H9 1.1200 . ? B10 B11 1.772(6) . ? B10 B12 1.777(6) . ? B10 H10 1.1200 . ? B11 B12 1.783(6) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 N14 1.336(4) . ? C13 C18 1.377(5) . ? N14 C15 1.350(4) . ? C15 C16 1.370(5) . ? C15 H15 0.9500 . ? C16 C17 1.372(6) . ? C16 H16 0.9500 . ? C17 C18 1.379(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.386(4) . ? C19 C20 1.392(5) . ? C20 C21 1.384(5) . ? C20 H20 0.9500 . ? C21 C22 1.380(5) . ? C21 H21 0.9500 . ? C22 C23 1.377(5) . ? C22 H22 0.9500 . ? C23 C24 1.384(5) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.393(5) . ? C25 C30 1.396(5) . ? C26 C27 1.393(5) . ? C26 H26 0.9500 . ? C27 C28 1.368(5) . ? C27 H27 0.9500 . ? C28 C29 1.381(5) . ? C28 H28 0.9500 . ? C29 C30 1.389(5) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.386(4) . ? C31 C36 1.404(4) . ? C32 C33 1.383(5) . ? C32 H32 0.9500 . ? C33 C34 1.374(5) . ? C33 H33 0.9500 . ? C34 C35 1.386(5) . ? C34 H34 0.9500 . ? C35 C36 1.381(5) . ? C35 H35 0.9500 . ? C36 H36 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 N14 Pd P 175.31(7) . . ? N14 Pd S 87.23(7) . . ? P Pd S 89.10(3) . . ? N14 Pd Cl 91.08(7) . . ? P Pd Cl 92.80(3) . . ? S Pd Cl 175.44(3) . . ? C2 S Pd 98.32(10) . . ? C31 P C25 110.08(15) . . ? C31 P C19 105.79(14) . . ? C25 P C19 102.74(14) . . ? C31 P Pd 107.16(11) . . ? C25 P Pd 114.43(11) . . ? C19 P Pd 116.26(11) . . ? C13 C1 C2 117.8(3) . . ? C13 C1 B4 123.6(3) . . ? C2 C1 B4 110.0(3) . . ? C13 C1 B5 120.5(3) . . ? C2 C1 B5 110.4(2) . . ? B4 C1 B5 62.5(2) . . ? C13 C1 B3 119.9(3) . . ? C2 C1 B3 60.71(19) . . ? B4 C1 B3 61.7(2) . . ? B5 C1 B3 113.0(3) . . ? C13 C1 B6 115.0(3) . . ? C2 C1 B6 61.02(19) . . ? B4 C1 B6 113.4(3) . . ? B5 C1 B6 62.2(2) . . ? B3 C1 B6 112.7(3) . . ? C1 C2 B11 109.7(2) . . ? C1 C2 B7 109.9(2) . . ? B11 C2 B7 62.9(2) . . ? C1 C2 B3 60.25(19) . . ? B11 C2 B3 113.4(3) . . ? B7 C2 B3 62.2(2) . . ? C1 C2 B6 60.15(19) . . ? B11 C2 B6 61.8(2) . . ? B7 C2 B6 113.0(3) . . ? B3 C2 B6 111.6(2) . . ? C1 C2 S 120.1(2) . . ? B11 C2 S 119.7(2) . . ? B7 C2 S 121.4(2) . . ? B3 C2 S 119.6(2) . . ? B6 C2 S 117.3(2) . . ? C1 B3 C2 59.03(19) . . ? C1 B3 B4 58.9(2) . . ? C2 B3 B4 106.5(3) . . ? C1 B3 B8 105.3(3) . . ? C2 B3 B8 105.3(3) . . ? B4 B3 B8 59.9(2) . . ? C1 B3 B7 105.8(3) . . ? C2 B3 B7 58.3(2) . . ? B4 B3 B7 108.3(3) . . ? B8 B3 B7 60.2(2) . . ? C1 B3 H3 123.6 . . ? C2 B3 H3 123.5 . . ? B4 B3 H3 121.7 . . ? B8 B3 H3 122.9 . . ? B7 B3 H3 122.1 . . ? C1 B4 B8 105.9(3) . . ? C1 B4 B3 59.4(2) . . ? B8 B4 B3 60.2(2) . . ? C1 B4 B9 105.2(3) . . ? B8 B4 B9 60.1(2) . . ? B3 B4 B9 108.2(3) . . ? C1 B4 B5 58.9(2) . . ? B8 B4 B5 107.8(3) . . ? B3 B4 B5 108.1(3) . . ? B9 B4 B5 59.4(2) . . ? C1 B4 H4 123.9 . . ? B8 B4 H4 122.0 . . ? B3 B4 H4 121.2 . . ? B9 B4 H4 122.4 . . ? B5 B4 H4 121.8 . . ? C1 B5 B9 105.5(3) . . ? C1 B5 B10 105.2(3) . . ? B9 B5 B10 60.7(2) . . ? C1 B5 B6 59.1(2) . . ? B9 B5 B6 108.1(3) . . ? B10 B5 B6 59.4(2) . . ? C1 B5 B4 58.6(2) . . ? B9 B5 B4 60.1(2) . . ? B10 B5 B4 108.2(3) . . ? B6 B5 B4 107.6(3) . . ? C1 B5 H5 124.3 . . ? B9 B5 H5 121.8 . . ? B10 B5 H5 122.2 . . ? B6 B5 H5 121.8 . . ? B4 B5 H5 121.6 . . ? C1 B6 C2 58.83(18) . . ? C1 B6 B10 105.6(3) . . ? C2 B6 B10 105.3(3) . . ? C1 B6 B11 105.8(3) . . ? C2 B6 B11 58.2(2) . . ? B10 B6 B11 60.2(2) . . ? C1 B6 B5 58.8(2) . . ? C2 B6 B5 106.0(2) . . ? B10 B6 B5 60.1(2) . . ? B11 B6 B5 108.3(3) . . ? C1 B6 H6 123.5 . . ? C2 B6 H6 123.8 . . ? B10 B6 H6 122.7 . . ? B11 B6 H6 122.1 . . ? B5 B6 H6 121.8 . . ? C2 B7 B3 59.5(2) . . ? C2 B7 B12 105.4(3) . . ? B3 B7 B12 107.7(3) . . ? C2 B7 B8 105.8(3) . . ? B3 B7 B8 59.7(2) . . ? B12 B7 B8 60.1(2) . . ? C2 B7 B11 58.5(2) . . ? B3 B7 B11 107.6(3) . . ? B12 B7 B11 60.0(2) . . ? B8 B7 B11 107.9(3) . . ? C2 B7 H7 123.9 . . ? B3 B7 H7 121.7 . . ? B12 B7 H7 122.3 . . ? B8 B7 H7 122.1 . . ? B11 B7 H7 121.8 . . ? B4 B8 B3 59.9(2) . . ? B4 B8 B9 60.3(2) . . ? B3 B8 B9 108.1(3) . . ? B4 B8 B7 108.3(3) . . ? B3 B8 B7 60.2(2) . . ? B9 B8 B7 108.2(3) . . ? B4 B8 B12 108.2(3) . . ? B3 B8 B12 107.9(3) . . ? B9 B8 B12 60.0(2) . . ? B7 B8 B12 59.9(2) . . ? B4 B8 H8 121.5 . . ? B3 B8 H8 121.8 . . ? B9 B8 H8 121.6 . . ? B7 B8 H8 121.6 . . ? B12 B8 H8 121.8 . . ? B5 B9 B8 108.1(3) . . ? B5 B9 B4 60.4(2) . . ? B8 B9 B4 59.5(2) . . ? B5 B9 B12 108.0(3) . . ? B8 B9 B12 60.2(2) . . ? B4 B9 B12 107.8(3) . . ? B5 B9 B10 59.8(2) . . ? B8 B9 B10 107.8(3) . . ? B4 B9 B10 107.8(3) . . ? B12 B9 B10 59.8(2) . . ? B5 B9 H9 121.5 . . ? B8 B9 H9 121.8 . . ? B4 B9 H9 121.8 . . ? B12 B9 H9 121.8 . . ? B10 B9 H9 122.0 . . ? B6 B10 B5 60.5(2) . . ? B6 B10 B11 60.2(2) . . ? B5 B10 B11 108.6(3) . . ? B6 B10 B12 108.4(3) . . ? B5 B10 B12 107.8(3) . . ? B11 B10 B12 60.3(2) . . ? B6 B10 B9 108.0(3) . . ? B5 B10 B9 59.5(2) . . ? B11 B10 B9 108.2(3) . . ? B12 B10 B9 59.9(2) . . ? B6 B10 H10 121.4 . . ? B5 B10 H10 121.7 . . ? B11 B10 H10 121.3 . . ? B12 B10 H10 121.7 . . ? B9 B10 H10 122.0 . . ? C2 B11 B10 106.1(3) . . ? C2 B11 B6 60.0(2) . . ? B10 B11 B6 59.5(2) . . ? C2 B11 B12 105.3(3) . . ? B10 B11 B12 60.0(2) . . ? B6 B11 B12 107.5(3) . . ? C2 B11 B7 58.6(2) . . ? B10 B11 B7 107.9(3) . . ? B6 B11 B7 108.0(3) . . ? B12 B11 B7 59.8(2) . . ? C2 B11 H11 123.6 . . ? B10 B11 H11 122.2 . . ? B6 B11 H11 121.5 . . ? B12 B11 H11 122.5 . . ? B7 B11 H11 121.8 . . ? B10 B12 B9 60.4(2) . . ? B10 B12 B7 107.9(3) . . ? B9 B12 B7 108.0(3) . . ? B10 B12 B11 59.7(2) . . ? B9 B12 B11 108.2(3) . . ? B7 B12 B11 60.2(2) . . ? B10 B12 B8 107.9(3) . . ? B9 B12 B8 59.8(2) . . ? B7 B12 B8 59.9(2) . . ? B11 B12 B8 108.0(3) . . ? B10 B12 H12 121.7 . . ? B9 B12 H12 121.6 . . ? B7 B12 H12 121.7 . . ? B11 B12 H12 121.7 . . ? B8 B12 H12 121.9 . . ? N14 C13 C18 121.3(3) . . ? N14 C13 C1 119.6(3) . . ? C18 C13 C1 119.1(3) . . ? C13 N14 C15 118.4(3) . . ? C13 N14 Pd 129.3(2) . . ? C15 N14 Pd 110.9(2) . . ? N14 C15 C16 122.9(4) . . ? N14 C15 H15 118.5 . . ? C16 C15 H15 118.5 . . ? C15 C16 C17 118.5(4) . . ? C15 C16 H16 120.8 . . ? C17 C16 H16 120.8 . . ? C16 C17 C18 119.0(4) . . ? C16 C17 H17 120.5 . . ? C18 C17 H17 120.5 . . ? C13 C18 C17 119.9(4) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C24 C19 C20 119.1(3) . . ? C24 C19 P 123.3(2) . . ? C20 C19 P 117.7(2) . . ? C21 C20 C19 120.7(3) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C22 C21 C20 119.6(3) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C23 C22 C21 120.1(3) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.5(3) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C23 C24 C19 120.0(3) . . ? C23 C24 H24 120.0 . . ? C19 C24 H24 120.0 . . ? C26 C25 C30 119.3(3) . . ? C26 C25 P 120.3(3) . . ? C30 C25 P 120.4(2) . . ? C27 C26 C25 119.9(3) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.3(3) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.4(3) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C28 C29 C30 120.1(4) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C29 C30 C25 119.9(3) . . ? C29 C30 H30 120.0 . . ? C25 C30 H30 120.0 . . ? C32 C31 C36 119.1(3) . . ? C32 C31 P 125.1(2) . . ? C36 C31 P 115.7(2) . . ? C33 C32 C31 120.4(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.3(3) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.0(3) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 120.2(3) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C35 C36 C31 119.9(3) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? 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 S C2 C1 C13 1.5(4) . . . . ? C2 C1 C13 N14 -44.1(4) . . . . ? N14 C13 C1 C2 -44.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.434 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.076 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 663537' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C25 H29 Au B10 N P S' _chemical_formula_sum 'C25 H29 Au B10 N P S' _chemical_formula_weight 711.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8012(2) _cell_length_b 13.3513(4) _cell_length_c 17.1365(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.541(2) _cell_angle_gamma 90.00 _cell_volume 2847.43(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5389 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 25.682 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.660 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 5.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Sheldrick, G. M., 2003' _exptl_absorpt_correction_T_min 0.686768 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_type Mok\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_standards_decay_% <1 _diffrn_reflns_number 26385 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.51 _reflns_number_total 5259 _reflns_number_gt 4220 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowsky & Minor, 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowsky & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+1.8773P] 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 SHELXL _refine_ls_extinction_coef 0.00076(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5259 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0591 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au Au 0.663588(12) 0.166700(13) 0.114691(10) 0.01575(7) Uani 1 d . . . S S 0.84727(8) 0.14480(8) 0.14973(7) 0.0177(2) Uani 1 d . . . P P 0.48429(8) 0.19197(9) 0.09193(7) 0.0160(3) Uani 1 d . . . C1 C 0.9022(3) 0.3182(3) 0.0504(3) 0.0150(9) Uani 1 d . . . C2 C 0.9019(3) 0.1916(3) 0.0709(3) 0.0146(9) Uani 1 d . . . B3 B 0.8247(4) 0.2369(4) -0.0167(3) 0.0151(11) Uani 1 d . . . H3 H 0.7348 0.2362 -0.0303 0.018 Uiso 1 calc R . . B4 B 0.8987(4) 0.3365(4) -0.0477(3) 0.0200(11) Uani 1 d . . . H4 H 0.8571 0.4013 -0.0835 0.024 Uiso 1 calc R . . B5 B 1.0200(4) 0.3520(4) 0.0271(3) 0.0220(12) Uani 1 d . . . H5 H 1.0594 0.4269 0.0410 0.026 Uiso 1 calc R . . B6 B 1.0186(4) 0.2617(4) 0.1036(3) 0.0181(11) Uani 1 d . . . H6 H 1.0554 0.2772 0.1684 0.022 Uiso 1 calc R . . B7 B 0.9001(4) 0.1249(4) -0.0148(3) 0.0172(11) Uani 1 d . . . H7 H 0.8604 0.0502 -0.0289 0.021 Uiso 1 calc R . . B8 B 0.9008(4) 0.2152(4) -0.0908(3) 0.0232(12) Uani 1 d . . . H8 H 0.8616 0.2002 -0.1553 0.028 Uiso 1 calc R . . B9 B 1.0214(4) 0.2862(4) -0.0627(3) 0.0242(12) Uani 1 d . . . H9 H 1.0619 0.3178 -0.1085 0.029 Uiso 1 calc R . . B10 B 1.0959(4) 0.2396(4) 0.0316(3) 0.0219(12) Uani 1 d . . . H10 H 1.1859 0.2401 0.0483 0.026 Uiso 1 calc R . . B11 B 1.0207(4) 0.1406(4) 0.0616(3) 0.0183(12) Uani 1 d . . . H11 H 1.0606 0.0762 0.0987 0.022 Uiso 1 calc R . . B12 B 1.0224(4) 0.1551(4) -0.0417(3) 0.0231(12) Uani 1 d . . . H12 H 1.0639 0.1000 -0.0735 0.028 Uiso 1 calc R . . C13 C 0.8463(3) 0.3893(3) 0.0950(3) 0.0154(9) Uani 1 d . . . N14 N 0.7391(3) 0.3936(3) 0.0701(2) 0.0203(9) Uani 1 d . . . C15 C 0.6877(3) 0.4593(4) 0.1070(3) 0.0239(11) Uani 1 d . . . H15 H 0.6115 0.4624 0.0903 0.029 Uiso 1 calc R . . C16 C 0.7382(4) 0.5226(3) 0.1676(3) 0.0260(11) Uani 1 d . . . H16 H 0.6985 0.5685 0.1917 0.031 Uiso 1 calc R . . C17 C 0.8478(4) 0.5169(4) 0.1919(3) 0.0297(12) Uani 1 d . . . H17 H 0.8857 0.5591 0.2337 0.036 Uiso 1 calc R . . C18 C 0.9030(3) 0.4497(3) 0.1554(3) 0.0235(11) Uani 1 d . . . H18 H 0.9791 0.4451 0.1717 0.028 Uiso 1 calc R . . C19 C 0.4572(3) 0.3150(3) 0.1267(3) 0.0190(10) Uani 1 d . . . C20 C 0.3907(3) 0.3846(4) 0.0785(3) 0.0222(10) Uani 1 d . . . H20 H 0.3537 0.3671 0.0255 0.027 Uiso 1 calc R . . C21 C 0.3786(3) 0.4797(4) 0.1080(3) 0.0266(11) Uani 1 d . . . H21 H 0.3338 0.5273 0.0748 0.032 Uiso 1 calc R . . C22 C 0.4309(3) 0.5057(4) 0.1850(3) 0.0259(11) Uani 1 d . . . H22 H 0.4229 0.5713 0.2042 0.031 Uiso 1 calc R . . C23 C 0.4949(4) 0.4370(4) 0.2344(3) 0.0268(11) Uani 1 d . . . H23 H 0.5288 0.4546 0.2880 0.032 Uiso 1 calc R . . C24 C 0.5095(3) 0.3430(4) 0.2057(3) 0.0231(10) Uani 1 d . . . H24 H 0.5551 0.2965 0.2394 0.028 Uiso 1 calc R . . C25 C 0.4203(3) 0.1874(3) -0.0140(3) 0.0156(9) Uani 1 d . . . C26 C 0.3277(3) 0.1306(4) -0.0451(3) 0.0218(10) Uani 1 d . . . H26 H 0.2952 0.0926 -0.0103 0.026 Uiso 1 calc R . . C27 C 0.2842(4) 0.1306(4) -0.1271(3) 0.0268(11) Uani 1 d . . . H27 H 0.2220 0.0916 -0.1486 0.032 Uiso 1 calc R . . C28 C 0.3299(4) 0.1865(4) -0.1781(3) 0.0251(11) Uani 1 d . . . H28 H 0.2983 0.1867 -0.2341 0.030 Uiso 1 calc R . . C29 C 0.4218(4) 0.2425(3) -0.1479(3) 0.0241(11) Uani 1 d . . . H29 H 0.4537 0.2803 -0.1832 0.029 Uiso 1 calc R . . C30 C 0.4668(3) 0.2431(3) -0.0665(3) 0.0213(10) Uani 1 d . . . H30 H 0.5296 0.2815 -0.0459 0.026 Uiso 1 calc R . . C31 C 0.4126(3) 0.1046(3) 0.1419(3) 0.0164(10) Uani 1 d . . . C32 C 0.4248(3) 0.0020(4) 0.1319(3) 0.0238(10) Uani 1 d . . . H32 H 0.4708 -0.0217 0.0997 0.029 Uiso 1 calc R . . C33 C 0.3700(4) -0.0652(4) 0.1688(3) 0.0295(12) Uani 1 d . . . H33 H 0.3765 -0.1351 0.1604 0.035 Uiso 1 calc R . . C34 C 0.3061(4) -0.0318(4) 0.2177(3) 0.0319(13) Uani 1 d . . . H34 H 0.2691 -0.0784 0.2434 0.038 Uiso 1 calc R . . C35 C 0.2959(4) 0.0694(4) 0.2291(3) 0.0330(13) Uani 1 d . . . H35 H 0.2525 0.0925 0.2635 0.040 Uiso 1 calc R . . C36 C 0.3481(3) 0.1378(4) 0.1911(3) 0.0255(11) Uani 1 d . . . H36 H 0.3398 0.2076 0.1987 0.031 Uiso 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 Au 0.01335(10) 0.01857(11) 0.01617(10) 0.00100(8) 0.00514(6) 0.00013(7) S 0.0143(5) 0.0235(7) 0.0157(6) 0.0062(5) 0.0042(4) 0.0033(4) P 0.0122(5) 0.0199(7) 0.0162(6) -0.0003(5) 0.0037(4) -0.0003(4) C1 0.019(2) 0.013(2) 0.014(2) -0.0002(18) 0.0050(17) -0.0024(17) C2 0.014(2) 0.015(3) 0.015(2) 0.0020(18) 0.0041(17) 0.0016(16) B3 0.016(2) 0.012(3) 0.016(3) -0.001(2) 0.000(2) -0.0001(19) B4 0.025(3) 0.015(3) 0.021(3) 0.000(2) 0.006(2) -0.002(2) B5 0.019(3) 0.019(3) 0.029(3) 0.003(2) 0.007(2) -0.005(2) B6 0.014(2) 0.016(3) 0.022(3) 0.001(2) -0.002(2) 0.0018(19) B7 0.018(2) 0.019(3) 0.016(3) -0.006(2) 0.006(2) 0.004(2) B8 0.027(3) 0.023(3) 0.019(3) -0.002(2) 0.005(2) -0.003(2) B9 0.024(3) 0.026(3) 0.026(3) 0.001(3) 0.012(2) 0.000(2) B10 0.015(3) 0.022(3) 0.032(3) 0.002(2) 0.011(2) 0.001(2) B11 0.015(2) 0.017(3) 0.024(3) 0.000(2) 0.006(2) 0.0011(19) B12 0.024(3) 0.023(3) 0.026(3) -0.005(3) 0.013(2) -0.002(2) C13 0.019(2) 0.009(2) 0.017(2) 0.0018(19) 0.0020(18) 0.0025(17) N14 0.0188(19) 0.020(2) 0.021(2) -0.0031(17) 0.0016(16) 0.0024(16) C15 0.020(2) 0.020(3) 0.033(3) -0.003(2) 0.008(2) 0.0093(19) C16 0.037(3) 0.015(3) 0.031(3) -0.002(2) 0.016(2) 0.008(2) C17 0.042(3) 0.023(3) 0.024(3) -0.011(2) 0.007(2) 0.001(2) C18 0.025(2) 0.022(3) 0.020(3) -0.004(2) -0.0015(19) 0.002(2) C19 0.013(2) 0.024(3) 0.020(3) 0.000(2) 0.0048(18) -0.0044(18) C20 0.018(2) 0.028(3) 0.020(3) -0.002(2) 0.0004(18) 0.0004(19) C21 0.023(2) 0.027(3) 0.029(3) 0.001(2) 0.004(2) 0.009(2) C22 0.024(2) 0.022(3) 0.037(3) -0.007(2) 0.016(2) 0.000(2) C23 0.029(3) 0.030(3) 0.022(3) -0.005(2) 0.006(2) -0.004(2) C24 0.024(2) 0.024(3) 0.020(3) 0.001(2) 0.0028(19) -0.005(2) C25 0.017(2) 0.017(3) 0.012(2) -0.0021(18) 0.0021(17) 0.0039(17) C26 0.022(2) 0.027(3) 0.017(3) 0.001(2) 0.0063(19) -0.0029(19) C27 0.022(2) 0.035(3) 0.019(3) -0.004(2) -0.0021(19) -0.003(2) C28 0.029(3) 0.029(3) 0.016(3) -0.001(2) 0.0024(19) 0.007(2) C29 0.034(3) 0.020(3) 0.022(3) 0.000(2) 0.013(2) 0.001(2) C30 0.018(2) 0.020(3) 0.026(3) 0.000(2) 0.006(2) -0.0024(19) C31 0.011(2) 0.025(3) 0.011(2) 0.0027(19) -0.0026(16) -0.0025(17) C32 0.022(2) 0.027(3) 0.024(3) -0.002(2) 0.0092(19) 0.002(2) C33 0.029(3) 0.022(3) 0.036(3) 0.003(2) 0.005(2) -0.006(2) C34 0.027(3) 0.039(3) 0.029(3) 0.004(2) 0.004(2) -0.017(2) C35 0.027(3) 0.048(4) 0.029(3) -0.005(3) 0.018(2) -0.013(2) C36 0.022(2) 0.028(3) 0.030(3) -0.007(2) 0.013(2) -0.007(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 Au P 2.2616(10) . ? Au S 2.3052(10) . ? S C2 1.774(4) . ? P C19 1.808(5) . ? P C25 1.810(4) . ? P C31 1.817(4) . ? C1 C13 1.501(6) . ? C1 B4 1.690(6) . ? C1 B5 1.709(6) . ? C1 B3 1.717(6) . ? C1 C2 1.725(6) . ? C1 B6 1.727(6) . ? C2 B3 1.703(6) . ? C2 B11 1.707(6) . ? C2 B7 1.713(6) . ? C2 B6 1.740(6) . ? B3 B7 1.776(7) . ? B3 B4 1.785(7) . ? B3 B8 1.796(7) . ? B3 H3 1.1200 . ? B4 B5 1.779(7) . ? B4 B9 1.781(7) . ? B4 B8 1.782(7) . ? B4 H4 1.1200 . ? B5 B9 1.775(8) . ? B5 B10 1.781(7) . ? B5 B6 1.785(7) . ? B5 H5 1.1200 . ? B6 B11 1.772(7) . ? B6 B10 1.777(7) . ? B6 H6 1.1200 . ? B7 B8 1.777(8) . ? B7 B12 1.779(7) . ? B7 B11 1.786(7) . ? B7 H7 1.1200 . ? B8 B12 1.779(7) . ? B8 B9 1.779(7) . ? B8 H8 1.1200 . ? B9 B10 1.786(8) . ? B9 B12 1.788(8) . ? B9 H9 1.1200 . ? B10 B11 1.780(7) . ? B10 B12 1.784(8) . ? B10 H10 1.1200 . ? B11 B12 1.785(7) . ? B11 H11 1.1200 . ? B12 H12 1.1200 . ? C13 N14 1.340(5) . ? C13 C18 1.377(6) . ? N14 C15 1.341(6) . ? C15 C16 1.377(6) . ? C15 H15 0.9500 . ? C16 C17 1.368(6) . ? C16 H16 0.9500 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.393(6) . ? C19 C24 1.413(6) . ? C20 C21 1.389(6) . ? C20 H20 0.9500 . ? C21 C22 1.376(6) . ? C21 H21 0.9500 . ? C22 C23 1.379(7) . ? C22 H22 0.9500 . ? C23 C24 1.377(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.403(6) . ? C25 C26 1.403(6) . ? C26 C27 1.385(6) . ? C26 H26 0.9500 . ? C27 C28 1.378(7) . ? C27 H27 0.9500 . ? C28 C29 1.389(6) . ? C28 H28 0.9500 . ? C29 C30 1.378(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C36 1.383(6) . ? C31 C32 1.394(7) . ? C32 C33 1.381(6) . ? C32 H32 0.9500 . ? C33 C34 1.375(7) . ? C33 H33 0.9500 . ? C34 C35 1.376(7) . ? C34 H34 0.9500 . ? C35 C36 1.383(7) . ? C35 H35 0.9500 . ? C36 H36 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 P Au S 174.86(4) . . ? C2 S Au 108.48(14) . . ? C19 P C25 106.5(2) . . ? C19 P C31 105.7(2) . . ? C25 P C31 106.92(19) . . ? C19 P Au 110.12(14) . . ? C25 P Au 111.75(13) . . ? C31 P Au 115.27(14) . . ? C13 C1 B4 120.7(4) . . ? C13 C1 B5 120.2(4) . . ? B4 C1 B5 63.1(3) . . ? C13 C1 B3 118.1(3) . . ? B4 C1 B3 63.2(3) . . ? B5 C1 B3 114.4(3) . . ? C13 C1 C2 119.5(3) . . ? B4 C1 C2 110.1(3) . . ? B5 C1 C2 110.5(3) . . ? B3 C1 C2 59.3(3) . . ? C13 C1 B6 117.6(4) . . ? B4 C1 B6 114.0(3) . . ? B5 C1 B6 62.6(3) . . ? B3 C1 B6 111.6(3) . . ? C2 C1 B6 60.5(2) . . ? B3 C2 B11 113.8(3) . . ? B3 C2 B7 62.6(3) . . ? B11 C2 B7 62.9(3) . . ? B3 C2 C1 60.1(2) . . ? B11 C2 C1 109.1(3) . . ? B7 C2 C1 109.6(3) . . ? B3 C2 B6 111.7(3) . . ? B11 C2 B6 61.9(3) . . ? B7 C2 B6 113.2(3) . . ? C1 C2 B6 59.8(2) . . ? B3 C2 S 123.0(3) . . ? B11 C2 S 116.7(3) . . ? B7 C2 S 122.7(3) . . ? C1 C2 S 121.3(3) . . ? B6 C2 S 114.0(3) . . ? C2 B3 C1 60.6(3) . . ? C2 B3 B7 59.0(3) . . ? C1 B3 B7 107.1(3) . . ? C2 B3 B4 106.7(3) . . ? C1 B3 B4 57.7(3) . . ? B7 B3 B4 108.0(3) . . ? C2 B3 B8 105.5(3) . . ? C1 B3 B8 104.5(3) . . ? B7 B3 B8 59.7(3) . . ? B4 B3 B8 59.7(3) . . ? C2 B3 H3 122.5 . . ? C1 B3 H3 123.3 . . ? B7 B3 H3 121.7 . . ? B4 B3 H3 122.3 . . ? B8 B3 H3 123.5 . . ? C1 B4 B5 59.0(3) . . ? C1 B4 B9 105.7(4) . . ? B5 B4 B9 59.8(3) . . ? C1 B4 B8 106.3(4) . . ? B5 B4 B8 108.0(4) . . ? B9 B4 B8 59.9(3) . . ? C1 B4 B3 59.2(3) . . ? B5 B4 B3 107.9(4) . . ? B9 B4 B3 108.1(4) . . ? B8 B4 B3 60.5(3) . . ? C1 B4 H4 123.7 . . ? B5 B4 H4 121.8 . . ? B9 B4 H4 122.3 . . ? B8 B4 H4 121.8 . . ? B3 B4 H4 121.4 . . ? C1 B5 B9 105.1(3) . . ? C1 B5 B4 57.9(3) . . ? B9 B5 B4 60.1(3) . . ? C1 B5 B10 105.6(3) . . ? B9 B5 B10 60.3(3) . . ? B4 B5 B10 108.0(4) . . ? C1 B5 B6 59.2(3) . . ? B9 B5 B6 107.8(4) . . ? B4 B5 B6 107.0(3) . . ? B10 B5 B6 59.8(3) . . ? C1 B5 H5 124.3 . . ? B9 B5 H5 122.1 . . ? B4 B5 H5 122.1 . . ? B10 B5 H5 122.0 . . ? B6 B5 H5 121.8 . . ? C1 B6 C2 59.7(2) . . ? C1 B6 B11 106.1(3) . . ? C2 B6 B11 58.2(3) . . ? C1 B6 B10 105.0(4) . . ? C2 B6 B10 105.3(4) . . ? B11 B6 B10 60.2(3) . . ? C1 B6 B5 58.2(3) . . ? C2 B6 B5 106.4(3) . . ? B11 B6 B5 108.3(4) . . ? B10 B6 B5 60.0(3) . . ? C1 B6 H6 123.6 . . ? C2 B6 H6 123.3 . . ? B11 B6 H6 122.0 . . ? B10 B6 H6 123.0 . . ? B5 B6 H6 121.9 . . ? C2 B7 B3 58.4(3) . . ? C2 B7 B8 105.9(4) . . ? B3 B7 B8 60.7(3) . . ? C2 B7 B12 105.6(3) . . ? B3 B7 B12 108.2(4) . . ? B8 B7 B12 60.0(3) . . ? C2 B7 B11 58.4(3) . . ? B3 B7 B11 106.7(4) . . ? B8 B7 B11 107.8(4) . . ? B12 B7 B11 60.1(3) . . ? C2 B7 H7 124.2 . . ? B3 B7 H7 121.8 . . ? B8 B7 H7 121.7 . . ? B12 B7 H7 121.9 . . ? B11 B7 H7 122.3 . . ? B12 B8 B7 60.0(3) . . ? B12 B8 B9 60.3(3) . . ? B7 B8 B9 108.4(4) . . ? B12 B8 B4 108.1(4) . . ? B7 B8 B4 108.0(4) . . ? B9 B8 B4 60.0(3) . . ? B12 B8 B3 107.3(4) . . ? B7 B8 B3 59.6(3) . . ? B9 B8 B3 107.6(4) . . ? B4 B8 B3 59.8(3) . . ? B12 B8 H8 121.8 . . ? B7 B8 H8 121.6 . . ? B9 B8 H8 121.5 . . ? B4 B8 H8 121.6 . . ? B3 B8 H8 122.3 . . ? B5 B9 B8 108.3(4) . . ? B5 B9 B4 60.0(3) . . ? B8 B9 B4 60.0(3) . . ? B5 B9 B10 60.0(3) . . ? B8 B9 B10 107.7(4) . . ? B4 B9 B10 107.6(4) . . ? B5 B9 B12 108.1(4) . . ? B8 B9 B12 59.8(3) . . ? B4 B9 B12 107.7(4) . . ? B10 B9 B12 59.9(3) . . ? B5 B9 H9 121.5 . . ? B8 B9 H9 121.7 . . ? B4 B9 H9 121.9 . . ? B10 B9 H9 122.0 . . ? B12 B9 H9 121.8 . . ? B6 B10 B11 59.8(3) . . ? B6 B10 B5 60.2(3) . . ? B11 B10 B5 108.2(3) . . ? B6 B10 B12 107.8(3) . . ? B11 B10 B12 60.1(3) . . ? B5 B10 B12 108.1(4) . . ? B6 B10 B9 107.7(3) . . ? B11 B10 B9 108.0(4) . . ? B5 B10 B9 59.7(3) . . ? B12 B10 B9 60.1(3) . . ? B6 B10 H10 121.9 . . ? B11 B10 H10 121.6 . . ? B5 B10 H10 121.6 . . ? B12 B10 H10 121.7 . . ? B9 B10 H10 121.9 . . ? C2 B11 B6 60.0(3) . . ? C2 B11 B10 106.5(3) . . ? B6 B11 B10 60.0(3) . . ? C2 B11 B12 105.6(3) . . ? B6 B11 B12 108.0(4) . . ? B10 B11 B12 60.1(3) . . ? C2 B11 B7 58.7(3) . . ? B6 B11 B7 108.2(3) . . ? B10 B11 B7 108.0(4) . . ? B12 B11 B7 59.7(3) . . ? C2 B11 H11 123.5 . . ? B6 B11 H11 121.2 . . ? B10 B11 H11 121.9 . . ? B12 B11 H11 122.4 . . ? B7 B11 H11 121.8 . . ? B8 B12 B7 59.9(3) . . ? B8 B12 B10 107.8(4) . . ? B7 B12 B10 108.1(4) . . ? B8 B12 B11 107.7(4) . . ? B7 B12 B11 60.1(3) . . ? B10 B12 B11 59.8(3) . . ? B8 B12 B9 59.9(3) . . ? B7 B12 B9 108.0(4) . . ? B10 B12 B9 60.0(3) . . ? B11 B12 B9 107.7(4) . . ? B8 B12 H12 121.9 . . ? B7 B12 H12 121.6 . . ? B10 B12 H12 121.7 . . ? B11 B12 H12 121.9 . . ? B9 B12 H12 121.8 . . ? N14 C13 C18 122.4(4) . . ? N14 C13 C1 116.1(4) . . ? C18 C13 C1 121.5(4) . . ? C13 N14 C15 117.2(4) . . ? N14 C15 C16 124.1(4) . . ? N14 C15 H15 117.9 . . ? C16 C15 H15 117.9 . . ? C17 C16 C15 117.6(4) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C18 119.7(4) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C13 C18 C17 119.1(4) . . ? C13 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C24 118.5(4) . . ? C20 C19 P 123.3(4) . . ? C24 C19 P 118.1(3) . . ? C21 C20 C19 120.0(4) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 120.5(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C24 C23 C22 119.9(5) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.6(4) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C30 C25 C26 119.4(4) . . ? C30 C25 P 117.7(3) . . ? C26 C25 P 122.9(3) . . ? C27 C26 C25 119.3(4) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C28 C27 C26 120.9(4) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.3(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C30 C29 C28 119.8(4) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C25 120.4(4) . . ? C29 C30 H30 119.8 . . ? C25 C30 H30 119.8 . . ? C36 C31 C32 119.3(4) . . ? C36 C31 P 121.4(4) . . ? C32 C31 P 119.3(3) . . ? C33 C32 C31 119.9(4) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C34 C33 C32 120.5(5) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 119.7(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.6(5) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 120.0(5) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? 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 S C2 C1 C13 -5.6(5) . . . . ? C2 C1 C13 N14 -78.2(5) . . . . ? C2 C1 C13 C18 104.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.51 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.809 _refine_diff_density_min -0.974 _refine_diff_density_rms 0.129 #===END