# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_email PARKIN@COLUMBIA.EDU _publ_contact_author 'Prof. G. Parkin ' _publ_contact_author_name 'Prof. G. Parkin' loop_ _publ_author_name 'G. Parkin ' 'Keliang Pang.' 'Stephanie M. Quan' data_pdoacs10 _database_code_depnum_ccdc_archive 'CCDC 617723' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H78 B2 N14 O4 Pd S6' _chemical_formula_weight 1259.64 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' 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' Pd Pd -0.9988 1.0072 '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)/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 10.7707(5) _cell_length_b 16.3500(8) _cell_length_c 18.0972(9) _cell_angle_alpha 90.00 _cell_angle_beta 99.8880(10) _cell_angle_gamma 90.00 _cell_volume 3139.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 6711 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.51 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9224 _exptl_absorpt_correction_T_max 0.9224 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21988 _diffrn_reflns_av_R_equivalents 0.0410 _diffrn_reflns_av_sigmaI/netI 0.0582 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7407 _reflns_number_gt 4824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0487P)^2^+1.3428P] 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 0.0005(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7407 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1108 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.0000 0.5000 0.0000 0.03185(10) Uani 1 2 d S . . S1 S 0.01153(7) 0.44109(5) 0.11757(4) 0.0404(2) Uani 1 1 d . . . S2 S 0.21282(7) 0.47242(5) -0.00944(5) 0.03632(19) Uani 1 1 d . . . S3 S -0.04876(9) 0.19596(7) 0.14319(6) 0.0616(3) Uani 1 1 d . . . O1 O 0.1732(2) 0.19250(12) 0.04743(13) 0.0437(5) Uani 1 1 d . . . O2 O 0.0332(3) 0.11898(17) -0.03116(17) 0.0791(9) Uani 1 1 d . . . N11 N 0.1896(2) 0.32400(14) 0.10433(14) 0.0335(6) Uani 1 1 d . . . N12 N 0.2434(2) 0.40565(15) 0.20137(14) 0.0359(6) Uani 1 1 d . . . N21 N 0.1778(2) 0.30738(15) -0.03741(14) 0.0360(6) Uani 1 1 d . . . N22 N 0.2703(2) 0.37016(16) -0.12067(14) 0.0397(6) Uani 1 1 d . . . N31 N -0.0177(2) 0.28210(15) 0.01943(14) 0.0355(6) Uani 1 1 d . . . N32 N -0.2175(2) 0.26646(16) 0.02786(15) 0.0409(6) Uani 1 1 d . . . B B 0.1257(3) 0.2759(2) 0.0336(2) 0.0359(8) Uani 1 1 d . . . C1 C 0.1176(4) 0.1235(3) 0.0235(3) 0.0659(11) Uani 1 1 d . . . C2 C 0.1707(5) 0.0481(3) 0.0663(3) 0.0975(17) Uani 1 1 d . . . H2A H 0.1236 0.0003 0.0458 0.146 Uiso 1 1 calc R . . H2B H 0.1638 0.0541 0.1188 0.146 Uiso 1 1 calc R . . H2C H 0.2586 0.0417 0.0618 0.146 Uiso 1 1 calc R . . C11 C 0.1524(3) 0.38935(18) 0.14080(16) 0.0334(7) Uani 1 1 d . . . C12 C 0.3069(3) 0.30016(19) 0.14255(17) 0.0378(7) Uani 1 1 d . . . H12A H 0.3552 0.2565 0.1290 0.045 Uiso 1 1 calc R . . C13 C 0.3402(3) 0.34940(19) 0.20196(18) 0.0398(7) Uani 1 1 d . . . H13A H 0.4150 0.3464 0.2373 0.048 Uiso 1 1 calc R . . C14 C 0.2435(3) 0.4719(2) 0.25848(18) 0.0419(7) Uani 1 1 d . . . C15 C 0.3632(4) 0.4631(2) 0.3175(2) 0.0625(10) Uani 1 1 d . . . H15A H 0.3625 0.4106 0.3424 0.094 Uiso 1 1 calc R . . H15B H 0.3661 0.5067 0.3542 0.094 Uiso 1 1 calc R . . H15C H 0.4367 0.4666 0.2933 0.094 Uiso 1 1 calc R . . C16 C 0.2438(4) 0.5545(2) 0.2202(2) 0.0580(10) Uani 1 1 d . . . H16A H 0.1673 0.5604 0.1835 0.087 Uiso 1 1 calc R . . H16B H 0.3165 0.5583 0.1953 0.087 Uiso 1 1 calc R . . H16C H 0.2477 0.5976 0.2574 0.087 Uiso 1 1 calc R . . C17 C 0.1294(3) 0.4623(2) 0.29754(19) 0.0541(9) Uani 1 1 d . . . H17A H 0.0527 0.4682 0.2610 0.081 Uiso 1 1 calc R . . H17B H 0.1320 0.5040 0.3359 0.081 Uiso 1 1 calc R . . H17C H 0.1312 0.4086 0.3205 0.081 Uiso 1 1 calc R . . C21 C 0.2198(3) 0.38107(18) -0.05685(17) 0.0343(7) Uani 1 1 d . . . C22 C 0.1965(3) 0.2515(2) -0.0919(2) 0.0522(9) Uani 1 1 d . . . H22A H 0.1731 0.1960 -0.0933 0.063 Uiso 1 1 calc R . . C23 C 0.2534(4) 0.2895(2) -0.1423(2) 0.0559(10) Uani 1 1 d . . . H23A H 0.2776 0.2655 -0.1848 0.067 Uiso 1 1 calc R . . C24 C 0.3345(3) 0.4316(2) -0.16424(19) 0.0465(8) Uani 1 1 d . . . C25 C 0.4421(4) 0.4726(3) -0.1117(2) 0.0663(11) Uani 1 1 d . . . H25A H 0.4088 0.5019 -0.0728 0.099 Uiso 1 1 calc R . . H25B H 0.4848 0.5107 -0.1400 0.099 Uiso 1 1 calc R . . H25C H 0.5013 0.4314 -0.0890 0.099 Uiso 1 1 calc R . . C26 C 0.3885(4) 0.3859(2) -0.2249(2) 0.0671(11) Uani 1 1 d . . . H26A H 0.3206 0.3600 -0.2590 0.101 Uiso 1 1 calc R . . H26B H 0.4472 0.3445 -0.2019 0.101 Uiso 1 1 calc R . . H26C H 0.4321 0.4242 -0.2524 0.101 Uiso 1 1 calc R . . C27 C 0.2389(4) 0.4928(3) -0.2004(3) 0.0829(15) Uani 1 1 d . . . H27A H 0.1722 0.4647 -0.2336 0.124 Uiso 1 1 calc R . . H27B H 0.2793 0.5318 -0.2290 0.124 Uiso 1 1 calc R . . H27C H 0.2035 0.5214 -0.1619 0.124 Uiso 1 1 calc R . . C31 C -0.0966(3) 0.24894(19) 0.06277(18) 0.0407(7) Uani 1 1 d . . . C32 C -0.0894(3) 0.31995(18) -0.04206(17) 0.0383(7) Uani 1 1 d . . . H32A H -0.0579 0.3477 -0.0804 0.046 Uiso 1 1 calc R . . C33 C -0.2106(3) 0.31025(19) -0.03735(19) 0.0427(8) Uani 1 1 d . . . H33A H -0.2795 0.3296 -0.0720 0.051 Uiso 1 1 calc R . . C34 C -0.3364(3) 0.2347(3) 0.0486(2) 0.0596(10) Uani 1 1 d . . . C35 C -0.3443(4) 0.2605(4) 0.1289(2) 0.0922(16) Uani 1 1 d . . . H35A H -0.3439 0.3197 0.1321 0.138 Uiso 1 1 calc R . . H35B H -0.2725 0.2387 0.1629 0.138 Uiso 1 1 calc R . . H35C H -0.4215 0.2395 0.1425 0.138 Uiso 1 1 calc R . . C36 C -0.3379(4) 0.1419(3) 0.0379(3) 0.0917(16) Uani 1 1 d . . . H36A H -0.3327 0.1292 -0.0138 0.138 Uiso 1 1 calc R . . H36B H -0.4154 0.1197 0.0501 0.138 Uiso 1 1 calc R . . H36C H -0.2664 0.1180 0.0707 0.138 Uiso 1 1 calc R . . C37 C -0.4490(3) 0.2724(3) -0.0039(2) 0.0840(15) Uani 1 1 d . . . H37A H -0.4462 0.2565 -0.0553 0.126 Uiso 1 1 calc R . . H37B H -0.4451 0.3315 0.0002 0.126 Uiso 1 1 calc R . . H37C H -0.5268 0.2530 0.0101 0.126 Uiso 1 1 calc R . . N1S N -0.3775(4) 0.3157(3) 0.3151(2) 0.1023(15) Uani 1 1 d . . . C1S C -0.2733(4) 0.3176(3) 0.3121(2) 0.0717(12) Uani 1 1 d . . . C2S C -0.1405(4) 0.3206(3) 0.3080(3) 0.0800(14) Uani 1 1 d . . . H2S1 H -0.1265 0.3603 0.2704 0.120 Uiso 1 1 calc R . . H2S2 H -0.1128 0.2671 0.2944 0.120 Uiso 1 1 calc R . . H2S3 H -0.0932 0.3365 0.3564 0.120 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 Pd 0.03319(16) 0.02943(18) 0.03264(19) -0.00066(15) 0.00477(12) 0.00662(14) S1 0.0399(4) 0.0464(5) 0.0354(4) 0.0029(4) 0.0078(3) 0.0148(3) S2 0.0352(4) 0.0309(4) 0.0435(5) -0.0021(3) 0.0086(3) 0.0029(3) S3 0.0534(5) 0.0810(7) 0.0530(6) 0.0326(5) 0.0168(4) 0.0136(5) O1 0.0488(12) 0.0300(12) 0.0521(14) -0.0041(10) 0.0078(11) 0.0004(10) O2 0.091(2) 0.068(2) 0.071(2) -0.0007(16) -0.0066(18) -0.0159(16) N11 0.0338(12) 0.0338(14) 0.0336(14) 0.0023(11) 0.0078(11) 0.0042(10) N12 0.0366(13) 0.0383(15) 0.0324(14) 0.0006(11) 0.0045(11) 0.0021(11) N21 0.0389(13) 0.0341(14) 0.0361(15) -0.0054(11) 0.0097(11) -0.0042(11) N22 0.0427(14) 0.0412(15) 0.0380(15) 0.0000(12) 0.0146(12) -0.0014(12) N31 0.0394(13) 0.0345(14) 0.0327(14) 0.0060(11) 0.0068(11) -0.0005(11) N32 0.0354(13) 0.0444(16) 0.0436(16) 0.0058(13) 0.0085(12) 0.0023(12) B 0.0379(17) 0.0334(19) 0.037(2) 0.0009(15) 0.0080(15) 0.0021(15) C1 0.073(3) 0.061(3) 0.062(3) 0.003(2) 0.005(2) -0.003(2) C2 0.121(4) 0.060(3) 0.102(4) 0.018(3) -0.006(3) 0.002(3) C11 0.0343(14) 0.0352(17) 0.0318(17) 0.0034(13) 0.0089(13) 0.0029(13) C12 0.0344(15) 0.0385(18) 0.0408(19) 0.0038(14) 0.0075(13) 0.0091(13) C13 0.0329(15) 0.0438(19) 0.0412(19) 0.0018(15) 0.0018(13) 0.0035(13) C14 0.0508(18) 0.0381(17) 0.0365(18) -0.0059(14) 0.0067(15) -0.0004(14) C15 0.066(2) 0.061(2) 0.055(2) -0.019(2) -0.0070(19) 0.000(2) C16 0.076(2) 0.038(2) 0.063(3) -0.0002(17) 0.017(2) -0.0060(18) C17 0.063(2) 0.063(2) 0.039(2) -0.0029(18) 0.0170(17) 0.0004(19) C21 0.0294(14) 0.0375(18) 0.0362(17) -0.0021(13) 0.0068(13) 0.0014(12) C22 0.070(2) 0.044(2) 0.048(2) -0.0174(17) 0.0232(18) -0.0119(18) C23 0.075(2) 0.052(2) 0.047(2) -0.0175(18) 0.0286(19) -0.0130(19) C24 0.0486(18) 0.048(2) 0.048(2) 0.0100(16) 0.0233(16) 0.0061(15) C25 0.065(2) 0.063(3) 0.077(3) 0.006(2) 0.030(2) -0.016(2) C26 0.077(3) 0.068(3) 0.067(3) 0.004(2) 0.046(2) -0.002(2) C27 0.080(3) 0.095(3) 0.083(3) 0.046(3) 0.040(3) 0.038(3) C31 0.0429(17) 0.0391(18) 0.0414(19) 0.0043(15) 0.0109(15) 0.0029(14) C32 0.0471(18) 0.0328(17) 0.0339(18) 0.0038(13) 0.0034(14) -0.0055(14) C33 0.0442(18) 0.0423(19) 0.0392(19) 0.0059(15) 0.0009(15) 0.0039(15) C34 0.0397(18) 0.087(3) 0.054(2) 0.016(2) 0.0128(17) -0.0027(19) C35 0.053(2) 0.164(5) 0.064(3) 0.010(3) 0.022(2) 0.015(3) C36 0.082(3) 0.085(4) 0.106(4) 0.026(3) 0.013(3) -0.032(3) C37 0.0381(19) 0.140(5) 0.074(3) 0.025(3) 0.0087(19) 0.006(2) N1S 0.063(2) 0.168(5) 0.072(3) 0.022(3) 0.003(2) 0.023(3) C1S 0.069(3) 0.087(3) 0.054(3) 0.020(2) -0.003(2) 0.011(2) C2S 0.058(2) 0.096(4) 0.083(3) 0.027(3) 0.002(2) 0.002(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 Pd S1 2.3193(8) 3_565 ? Pd S1 2.3193(8) . ? Pd S2 2.3710(7) . ? Pd S2 2.3710(7) 3_565 ? S1 C11 1.725(3) . ? S2 C21 1.730(3) . ? S3 C31 1.696(3) . ? O1 C1 1.316(5) . ? O1 B 1.463(4) . ? O2 C1 1.225(5) . ? N11 C11 1.352(4) . ? N11 C12 1.388(4) . ? N11 B 1.558(4) . ? N12 C11 1.366(4) . ? N12 C13 1.389(4) . ? N12 C14 1.497(4) . ? N21 C21 1.355(4) . ? N21 C22 1.385(4) . ? N21 B 1.575(4) . ? N22 C21 1.370(4) . ? N22 C23 1.379(4) . ? N22 C24 1.515(4) . ? N31 C31 1.365(4) . ? N31 C32 1.387(4) . ? N31 B 1.525(4) . ? N32 C31 1.376(4) . ? N32 C33 1.393(4) . ? N32 C34 1.488(4) . ? C1 C2 1.514(6) . ? C12 C13 1.342(4) . ? C14 C16 1.519(5) . ? C14 C17 1.527(5) . ? C14 C15 1.534(5) . ? C22 C23 1.335(5) . ? C24 C27 1.503(5) . ? C24 C25 1.523(5) . ? C24 C26 1.523(5) . ? C32 C33 1.333(4) . ? C34 C36 1.528(6) . ? C34 C35 1.530(6) . ? C34 C37 1.536(5) . ? N1S C1S 1.133(5) . ? C1S C2S 1.446(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Pd S1 180.0 3_565 . ? S1 Pd S2 85.01(3) 3_565 . ? S1 Pd S2 94.99(3) . . ? S1 Pd S2 94.99(3) 3_565 3_565 ? S1 Pd S2 85.01(3) . 3_565 ? S2 Pd S2 180.00(4) . 3_565 ? C11 S1 Pd 109.49(10) . . ? C21 S2 Pd 108.95(10) . . ? C1 O1 B 128.1(3) . . ? C11 N11 C12 107.4(2) . . ? C11 N11 B 132.3(2) . . ? C12 N11 B 120.2(2) . . ? C11 N12 C13 108.2(2) . . ? C11 N12 C14 127.6(2) . . ? C13 N12 C14 124.2(2) . . ? C21 N21 C22 107.8(3) . . ? C21 N21 B 133.2(2) . . ? C22 N21 B 118.8(3) . . ? C21 N22 C23 108.1(3) . . ? C21 N22 C24 129.4(3) . . ? C23 N22 C24 122.4(3) . . ? C31 N31 C32 108.8(2) . . ? C31 N31 B 126.1(3) . . ? C32 N31 B 125.0(3) . . ? C31 N32 C33 108.2(3) . . ? C31 N32 C34 126.8(3) . . ? C33 N32 C34 124.5(3) . . ? O1 B N31 113.9(3) . . ? O1 B N11 103.8(2) . . ? N31 B N11 113.4(3) . . ? O1 B N21 106.3(2) . . ? N31 B N21 109.4(2) . . ? N11 B N21 109.7(2) . . ? O2 C1 O1 123.4(4) . . ? O2 C1 C2 121.8(4) . . ? O1 C1 C2 114.7(4) . . ? N11 C11 N12 108.3(2) . . ? N11 C11 S1 126.2(2) . . ? N12 C11 S1 125.5(2) . . ? C13 C12 N11 109.0(3) . . ? C12 C13 N12 107.1(3) . . ? N12 C14 C16 109.2(3) . . ? N12 C14 C17 109.9(3) . . ? C16 C14 C17 111.5(3) . . ? N12 C14 C15 108.3(3) . . ? C16 C14 C15 109.5(3) . . ? C17 C14 C15 108.3(3) . . ? N21 C21 N22 107.6(3) . . ? N21 C21 S2 126.4(2) . . ? N22 C21 S2 126.0(2) . . ? C23 C22 N21 108.6(3) . . ? C22 C23 N22 107.8(3) . . ? C27 C24 N22 109.2(3) . . ? C27 C24 C25 111.7(3) . . ? N22 C24 C25 109.5(3) . . ? C27 C24 C26 109.3(3) . . ? N22 C24 C26 108.4(3) . . ? C25 C24 C26 108.8(3) . . ? N31 C31 N32 106.7(3) . . ? N31 C31 S3 124.6(2) . . ? N32 C31 S3 128.6(2) . . ? C33 C32 N31 108.2(3) . . ? C32 C33 N32 108.1(3) . . ? N32 C34 C36 107.8(3) . . ? N32 C34 C35 109.5(3) . . ? C36 C34 C35 113.1(4) . . ? N32 C34 C37 109.0(3) . . ? C36 C34 C37 109.3(4) . . ? C35 C34 C37 108.0(3) . . ? N1S C1S C2S 179.6(6) . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 0.449 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.072 # Attachment 'PDPMES10.CIF' data_pdpmes10 _database_code_depnum_ccdc_archive 'CCDC 617724' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 B N6 P Pd S3' _chemical_formula_weight 737.10 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' 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' Pd Pd -0.9988 1.0072 '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 13.5495(14) _cell_length_b 13.3193(13) _cell_length_c 21.005(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.513(2) _cell_angle_gamma 90.00 _cell_volume 3594.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 2313 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 19.51 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9275 _exptl_absorpt_correction_T_max 0.9849 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24957 _diffrn_reflns_av_R_equivalents 0.1621 _diffrn_reflns_av_sigmaI/netI 0.2663 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.30 _reflns_number_total 8406 _reflns_number_gt 3177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0380P)^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 8406 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2375 _refine_ls_R_factor_gt 0.0667 _refine_ls_wR_factor_ref 0.1434 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _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 Pd Pd 0.33068(5) 0.28264(4) 0.13850(3) 0.03437(19) Uani 1 1 d . . . S1 S 0.35220(18) 0.14048(12) 0.07975(10) 0.0439(6) Uani 1 1 d . . . S2 S 0.15948(15) 0.37376(12) 0.12003(10) 0.0354(5) Uani 1 1 d . . . S3 S 0.44110(15) 0.36040(12) 0.24402(9) 0.0353(5) Uani 1 1 d . . . P P 0.39382(18) 0.38896(13) 0.07027(10) 0.0427(6) Uani 1 1 d . . . N11 N 0.2925(4) 0.0722(3) 0.1800(3) 0.0279(14) Uani 1 1 d . . . N12 N 0.3291(4) -0.0525(3) 0.1220(3) 0.0304(15) Uani 1 1 d . . . N21 N 0.1623(4) 0.2052(4) 0.1916(3) 0.0298(14) Uani 1 1 d . . . N22 N 0.0136(4) 0.2881(4) 0.1698(3) 0.0396(15) Uani 1 1 d . . . N31 N 0.3438(4) 0.2014(4) 0.2749(3) 0.0340(15) Uani 1 1 d . . . N32 N 0.4482(4) 0.2743(4) 0.3656(3) 0.0330(14) Uani 1 1 d . . . B B 0.2799(7) 0.1865(5) 0.1977(4) 0.029(2) Uani 1 1 d . . . C11 C 0.3258(6) 0.0503(4) 0.1283(3) 0.0297(18) Uani 1 1 d . . . C12 C 0.2767(6) -0.0185(4) 0.2093(3) 0.0345(19) Uani 1 1 d . . . H12A H 0.2547 -0.0250 0.2472 0.041 Uiso 1 1 calc R . . C13 C 0.2981(6) -0.0929(5) 0.1745(4) 0.0357(19) Uani 1 1 d . . . H13A H 0.2935 -0.1616 0.1833 0.043 Uiso 1 1 calc R . . C14 C 0.3617(7) -0.1096(5) 0.0710(4) 0.044(2) Uani 1 1 d . . . C15 C 0.3571(7) -0.2220(5) 0.0850(4) 0.071(3) Uani 1 1 d . . . H15A H 0.2862 -0.2407 0.0810 0.107 Uiso 1 1 calc R . . H15B H 0.4023 -0.2367 0.1300 0.107 Uiso 1 1 calc R . . H15C H 0.3800 -0.2598 0.0528 0.107 Uiso 1 1 calc R . . C16 C 0.4739(7) -0.0830(6) 0.0766(5) 0.074(3) Uani 1 1 d . . . H16A H 0.4784 -0.0121 0.0673 0.110 Uiso 1 1 calc R . . H16B H 0.4955 -0.1223 0.0444 0.110 Uiso 1 1 calc R . . H16C H 0.5192 -0.0978 0.1216 0.110 Uiso 1 1 calc R . . C17 C 0.2876(8) -0.0856(5) 0.0021(4) 0.086(3) Uani 1 1 d . . . H17A H 0.2918 -0.0147 -0.0071 0.129 Uiso 1 1 calc R . . H17B H 0.2171 -0.1022 0.0005 0.129 Uiso 1 1 calc R . . H17C H 0.3064 -0.1247 -0.0313 0.129 Uiso 1 1 calc R . . C21 C 0.1098(6) 0.2878(5) 0.1609(3) 0.0339(17) Uani 1 1 d . . . C22 C 0.0983(7) 0.1527(5) 0.2184(4) 0.045(2) Uani 1 1 d . . . H22A H 0.1153 0.0913 0.2414 0.054 Uiso 1 1 calc R . . C23 C 0.0097(7) 0.2005(5) 0.2074(4) 0.057(2) Uani 1 1 d . . . H23A H -0.0463 0.1803 0.2218 0.069 Uiso 1 1 calc R . . C24 C -0.0723(6) 0.3610(6) 0.1471(5) 0.054(2) Uani 1 1 d . . . C25 C -0.1637(7) 0.3318(6) 0.1689(5) 0.093(4) Uani 1 1 d . . . H25A H -0.1896 0.2669 0.1500 0.139 Uiso 1 1 calc R . . H25B H -0.2182 0.3817 0.1533 0.139 Uiso 1 1 calc R . . H25C H -0.1422 0.3280 0.2175 0.139 Uiso 1 1 calc R . . C26 C -0.1054(7) 0.3687(7) 0.0716(4) 0.088(3) Uani 1 1 d . . . H26A H -0.1301 0.3039 0.0520 0.132 Uiso 1 1 calc R . . H26B H -0.0466 0.3895 0.0579 0.132 Uiso 1 1 calc R . . H26C H -0.1608 0.4178 0.0564 0.132 Uiso 1 1 calc R . . C27 C -0.0349(7) 0.4630(5) 0.1761(4) 0.069(3) Uani 1 1 d . . . H27A H -0.0142 0.4598 0.2248 0.103 Uiso 1 1 calc R . . H27B H -0.0907 0.5115 0.1599 0.103 Uiso 1 1 calc R . . H27C H 0.0241 0.4833 0.1625 0.103 Uiso 1 1 calc R . . C31 C 0.4119(5) 0.2783(5) 0.2968(3) 0.0327(17) Uani 1 1 d . . . C32 C 0.3399(6) 0.1505(5) 0.3320(4) 0.045(2) Uani 1 1 d . . . H32A H 0.2991 0.0933 0.3315 0.054 Uiso 1 1 calc R . . C33 C 0.4020(6) 0.1941(4) 0.3871(4) 0.039(2) Uani 1 1 d . . . H33A H 0.4124 0.1744 0.4318 0.047 Uiso 1 1 calc R . . C34 C 0.5288(6) 0.3416(5) 0.4121(4) 0.040(2) Uani 1 1 d . . . C35 C 0.4927(6) 0.4490(5) 0.4022(4) 0.057(2) Uani 1 1 d . . . H35A H 0.4285 0.4558 0.4130 0.085 Uiso 1 1 calc R . . H35B H 0.4807 0.4682 0.3558 0.085 Uiso 1 1 calc R . . H35C H 0.5455 0.4921 0.4314 0.085 Uiso 1 1 calc R . . C36 C 0.5461(6) 0.3129(5) 0.4853(3) 0.060(3) Uani 1 1 d . . . H36A H 0.4815 0.3208 0.4955 0.090 Uiso 1 1 calc R . . H36B H 0.5990 0.3561 0.5145 0.090 Uiso 1 1 calc R . . H36C H 0.5687 0.2435 0.4925 0.090 Uiso 1 1 calc R . . C37 C 0.6308(6) 0.3299(6) 0.3963(4) 0.071(3) Uani 1 1 d . . . H37A H 0.6201 0.3489 0.3500 0.106 Uiso 1 1 calc R . . H37B H 0.6535 0.2605 0.4029 0.106 Uiso 1 1 calc R . . H37C H 0.6835 0.3728 0.4258 0.106 Uiso 1 1 calc R . . C41 C 0.5316(7) 0.3708(6) 0.0809(5) 0.089(3) Uani 1 1 d . . . H41A H 0.5526 0.4165 0.0517 0.134 Uiso 1 1 calc R . . H41B H 0.5431 0.3021 0.0696 0.134 Uiso 1 1 calc R . . H41C H 0.5723 0.3841 0.1272 0.134 Uiso 1 1 calc R . . C42 C 0.3339(8) 0.3790(6) -0.0190(4) 0.090(4) Uani 1 1 d . . . H42A H 0.3665 0.4261 -0.0414 0.135 Uiso 1 1 calc R . . H42B H 0.2603 0.3944 -0.0306 0.135 Uiso 1 1 calc R . . H42C H 0.3425 0.3113 -0.0334 0.135 Uiso 1 1 calc R . . C43 C 0.3872(7) 0.5230(5) 0.0849(4) 0.069(3) Uani 1 1 d . . . H43A H 0.4151 0.5597 0.0545 0.103 Uiso 1 1 calc R . . H43B H 0.4277 0.5385 0.1309 0.103 Uiso 1 1 calc R . . H43C H 0.3153 0.5424 0.0770 0.103 Uiso 1 1 calc R . . C1S C 0.8512(8) 0.6104(9) 0.3104(6) 0.089(4) Uani 1 1 d . . . H1SA H 0.9132 0.6133 0.3467 0.107 Uiso 1 1 calc R . . C2S C 0.8344(10) 0.6774(8) 0.2592(7) 0.083(3) Uani 1 1 d . . . H2SA H 0.8851 0.7261 0.2600 0.100 Uiso 1 1 calc R . . C3S C 0.7447(11) 0.6739(9) 0.2073(6) 0.101(4) Uani 1 1 d . . . H3SA H 0.7314 0.7211 0.1723 0.121 Uiso 1 1 calc R . . C4S C 0.6729(9) 0.5997(10) 0.2063(6) 0.096(4) Uani 1 1 d . . . H4SA H 0.6120 0.5955 0.1692 0.115 Uiso 1 1 calc R . . C5S C 0.6869(10) 0.5345(8) 0.2559(6) 0.075(3) Uani 1 1 d . . . H5SA H 0.6356 0.4863 0.2547 0.090 Uiso 1 1 calc R . . C6S C 0.7774(10) 0.5379(8) 0.3092(7) 0.094(4) Uani 1 1 d . . . H6SA H 0.7891 0.4915 0.3445 0.113 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 Pd 0.0525(4) 0.0213(2) 0.0359(3) 0.0004(3) 0.0234(3) -0.0043(3) S1 0.0797(18) 0.0224(8) 0.0399(13) 0.0011(9) 0.0336(13) -0.0028(10) S2 0.0346(13) 0.0307(9) 0.0402(12) 0.0047(9) 0.0107(10) 0.0065(9) S3 0.0394(13) 0.0329(9) 0.0290(11) 0.0007(8) 0.0043(10) -0.0128(9) P 0.0657(17) 0.0295(10) 0.0383(14) 0.0000(9) 0.0240(13) -0.0106(11) N11 0.036(4) 0.013(2) 0.038(4) -0.002(3) 0.016(3) -0.005(3) N12 0.041(4) 0.020(3) 0.030(4) 0.001(3) 0.010(3) 0.003(3) N21 0.038(4) 0.023(3) 0.029(3) -0.001(3) 0.012(3) -0.001(3) N22 0.024(4) 0.037(3) 0.057(4) -0.006(3) 0.013(3) 0.001(3) N31 0.045(4) 0.022(3) 0.039(4) 0.001(3) 0.019(3) -0.004(3) N32 0.035(4) 0.033(3) 0.028(4) 0.004(3) 0.005(3) 0.003(3) B 0.031(6) 0.026(4) 0.028(5) -0.010(4) 0.008(4) 0.001(4) C11 0.026(5) 0.030(4) 0.028(5) 0.000(3) 0.002(4) 0.007(4) C12 0.054(6) 0.022(3) 0.036(5) -0.002(3) 0.026(4) -0.005(4) C13 0.042(5) 0.023(3) 0.038(5) 0.002(3) 0.006(4) -0.001(3) C14 0.075(7) 0.030(4) 0.038(5) -0.009(4) 0.031(5) 0.008(4) C15 0.120(8) 0.030(4) 0.085(7) -0.001(5) 0.062(6) 0.009(5) C16 0.082(8) 0.054(5) 0.108(9) -0.010(5) 0.062(7) 0.012(5) C17 0.154(11) 0.047(5) 0.046(6) -0.022(5) 0.016(7) 0.004(6) C21 0.033(5) 0.034(4) 0.034(4) -0.011(4) 0.009(4) -0.004(4) C22 0.053(6) 0.033(4) 0.060(6) 0.013(4) 0.034(5) 0.005(4) C23 0.054(7) 0.046(5) 0.083(7) 0.003(5) 0.039(6) -0.014(5) C24 0.029(6) 0.060(5) 0.065(7) -0.001(5) 0.005(5) 0.005(5) C25 0.045(7) 0.088(7) 0.158(11) -0.002(7) 0.050(7) 0.006(6) C26 0.037(6) 0.139(9) 0.059(7) -0.020(6) -0.026(5) 0.029(6) C27 0.064(7) 0.057(5) 0.091(8) 0.006(5) 0.033(6) 0.030(5) C31 0.042(5) 0.022(3) 0.035(5) -0.004(4) 0.013(4) -0.001(4) C32 0.061(7) 0.029(4) 0.050(6) 0.003(4) 0.027(5) -0.010(4) C33 0.055(6) 0.031(4) 0.029(5) 0.005(4) 0.012(4) -0.003(4) C34 0.032(5) 0.047(4) 0.030(5) -0.003(4) -0.003(4) -0.004(4) C35 0.059(6) 0.052(5) 0.042(5) -0.013(4) -0.008(5) -0.007(5) C36 0.064(7) 0.068(6) 0.032(5) 0.001(4) -0.007(5) -0.004(5) C37 0.040(6) 0.107(7) 0.054(6) -0.008(5) 0.000(5) -0.002(5) C41 0.083(8) 0.066(6) 0.143(10) 0.020(6) 0.071(8) -0.007(6) C42 0.149(11) 0.067(6) 0.044(6) -0.014(5) 0.018(7) -0.060(6) C43 0.100(8) 0.039(4) 0.076(7) 0.010(5) 0.042(6) -0.003(5) C1S 0.056(8) 0.086(8) 0.101(10) -0.033(7) -0.010(7) -0.011(7) C2S 0.079(10) 0.072(7) 0.102(10) -0.021(7) 0.035(8) -0.041(7) C3S 0.105(11) 0.132(10) 0.075(9) 0.001(8) 0.042(9) -0.032(9) C4S 0.084(10) 0.137(11) 0.066(9) -0.037(8) 0.023(7) -0.044(8) C5S 0.091(10) 0.083(7) 0.068(8) -0.023(6) 0.051(8) -0.028(7) C6S 0.088(10) 0.080(8) 0.111(11) -0.008(7) 0.027(9) -0.012(7) _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 B 2.050(8) . ? Pd S1 2.3285(18) . ? Pd P 2.3601(19) . ? Pd S3 2.4734(19) . ? Pd S2 2.5362(19) . ? S1 C11 1.686(7) . ? S2 C21 1.693(7) . ? S3 C31 1.692(7) . ? P C42 1.797(8) . ? P C43 1.819(7) . ? P C41 1.824(9) . ? N11 C11 1.333(7) . ? N11 C12 1.403(7) . ? N11 B 1.590(8) . ? N12 C11 1.377(7) . ? N12 C13 1.404(8) . ? N12 C14 1.492(8) . ? N21 C21 1.356(8) . ? N21 C22 1.367(8) . ? N21 B 1.577(9) . ? N22 C21 1.375(8) . ? N22 C23 1.419(8) . ? N22 C24 1.473(9) . ? N31 C31 1.358(8) . ? N31 C32 1.392(8) . ? N31 B 1.588(9) . ? N32 C31 1.372(8) . ? N32 C33 1.384(8) . ? N32 C34 1.508(8) . ? C12 C13 1.317(8) . ? C14 C17 1.510(10) . ? C14 C16 1.529(10) . ? C14 C15 1.531(8) . ? C22 C23 1.313(9) . ? C24 C25 1.501(10) . ? C24 C27 1.509(10) . ? C24 C26 1.509(11) . ? C32 C33 1.330(9) . ? C34 C35 1.504(9) . ? C34 C36 1.529(9) . ? C34 C37 1.530(10) . ? C1S C2S 1.359(13) . ? C1S C6S 1.384(12) . ? C2S C3S 1.352(13) . ? C3S C4S 1.382(13) . ? C4S C5S 1.322(13) . ? C5S C6S 1.373(13) . ? 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 B Pd S1 86.4(2) . . ? B Pd P 177.9(2) . . ? S1 Pd P 92.04(7) . . ? B Pd S3 86.7(2) . . ? S1 Pd S3 132.34(8) . . ? P Pd S3 93.45(7) . . ? B Pd S2 85.7(2) . . ? S1 Pd S2 124.78(8) . . ? P Pd S2 96.33(7) . . ? S3 Pd S2 101.56(6) . . ? C11 S1 Pd 99.9(2) . . ? C21 S2 Pd 95.2(3) . . ? C31 S3 Pd 96.7(2) . . ? C42 P C43 102.6(4) . . ? C42 P C41 103.0(5) . . ? C43 P C41 102.3(4) . . ? C42 P Pd 117.3(3) . . ? C43 P Pd 116.1(3) . . ? C41 P Pd 113.6(3) . . ? C11 N11 C12 107.9(5) . . ? C11 N11 B 119.4(5) . . ? C12 N11 B 132.8(5) . . ? C11 N12 C13 106.2(5) . . ? C11 N12 C14 127.0(6) . . ? C13 N12 C14 126.8(5) . . ? C21 N21 C22 107.8(6) . . ? C21 N21 B 122.0(6) . . ? C22 N21 B 129.9(6) . . ? C21 N22 C23 106.1(6) . . ? C21 N22 C24 130.1(6) . . ? C23 N22 C24 123.8(6) . . ? C31 N31 C32 106.4(6) . . ? C31 N31 B 122.1(5) . . ? C32 N31 B 131.3(6) . . ? C31 N32 C33 109.0(6) . . ? C31 N32 C34 127.1(6) . . ? C33 N32 C34 123.9(6) . . ? N21 B N31 105.8(5) . . ? N21 B N11 108.3(5) . . ? N31 B N11 107.1(5) . . ? N21 B Pd 112.1(5) . . ? N31 B Pd 111.2(5) . . ? N11 B Pd 111.9(5) . . ? N11 C11 N12 109.0(6) . . ? N11 C11 S1 121.9(5) . . ? N12 C11 S1 129.1(6) . . ? C13 C12 N11 108.3(6) . . ? C12 C13 N12 108.6(5) . . ? N12 C14 C17 108.8(6) . . ? N12 C14 C16 110.0(6) . . ? C17 C14 C16 111.5(7) . . ? N12 C14 C15 108.8(6) . . ? C17 C14 C15 109.6(7) . . ? C16 C14 C15 108.1(7) . . ? N21 C21 N22 108.3(6) . . ? N21 C21 S2 123.8(5) . . ? N22 C21 S2 127.9(6) . . ? C23 C22 N21 110.1(6) . . ? C22 C23 N22 107.6(7) . . ? N22 C24 C25 112.0(7) . . ? N22 C24 C27 109.5(6) . . ? C25 C24 C27 108.2(7) . . ? N22 C24 C26 109.0(7) . . ? C25 C24 C26 109.8(8) . . ? C27 C24 C26 108.2(7) . . ? N31 C31 N32 107.8(6) . . ? N31 C31 S3 122.7(5) . . ? N32 C31 S3 129.5(5) . . ? C33 C32 N31 110.6(6) . . ? C32 C33 N32 106.2(6) . . ? C35 C34 N32 109.8(6) . . ? C35 C34 C36 108.5(6) . . ? N32 C34 C36 110.5(6) . . ? C35 C34 C37 110.1(6) . . ? N32 C34 C37 108.5(6) . . ? C36 C34 C37 109.4(7) . . ? C2S C1S C6S 120.4(11) . . ? C3S C2S C1S 119.8(10) . . ? C2S C3S C4S 119.0(11) . . ? C5S C4S C3S 122.2(11) . . ? C4S C5S C6S 119.2(11) . . ? C5S C6S C1S 119.4(11) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.658 _refine_diff_density_min -0.933 _refine_diff_density_rms 0.129 # Attachment 'TMPDOS10.CIF' data_tmpdos10 _database_code_depnum_ccdc_archive 'CCDC 617725' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H78 B2 N14 O4 Pd S6' _chemical_formula_weight 1259.64 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' 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8342(4) _cell_length_b 11.2770(5) _cell_length_c 13.6177(6) _cell_angle_alpha 93.8670(10) _cell_angle_beta 92.8400(10) _cell_angle_gamma 106.2340(10) _cell_volume 1589.73(12) _cell_formula_units_Z 1 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 5252 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.23 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 660 _exptl_absorpt_coefficient_mu 0.541 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8996 _exptl_absorpt_correction_T_max 0.9479 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11445 _diffrn_reflns_av_R_equivalents 0.0202 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.32 _reflns_number_total 7200 _reflns_number_gt 5694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0359P)^2^+0.6216P] 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 7200 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0531 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0780 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 Pd Pd 0.5000 1.0000 0.0000 0.02902(8) Uani 1 2 d S . . S1 S 0.70711(5) 0.96855(5) 0.00512(4) 0.03246(13) Uani 1 1 d . . . S2 S 0.50630(6) 1.05986(6) 0.16696(4) 0.03973(15) Uani 1 1 d . . . S3 S 0.38906(7) 0.81739(8) 0.35834(5) 0.0558(2) Uani 1 1 d . . . O1 O 0.60052(16) 0.70284(15) 0.26014(12) 0.0398(4) Uani 1 1 d . . . O2 O 0.4372(2) 0.5292(2) 0.22652(16) 0.0662(6) Uani 1 1 d . . . N11 N 0.62875(17) 0.74377(17) 0.08702(14) 0.0327(4) Uani 1 1 d . . . N12 N 0.73601(17) 0.73613(17) -0.04519(14) 0.0331(4) Uani 1 1 d . . . N21 N 0.65636(16) 0.91415(17) 0.22684(13) 0.0312(4) Uani 1 1 d . . . N22 N 0.73386(17) 1.10990(18) 0.28234(14) 0.0334(4) Uani 1 1 d . . . N31 N 0.42999(17) 0.76826(19) 0.16636(14) 0.0356(4) Uani 1 1 d . . . N32 N 0.22522(18) 0.7429(2) 0.19006(15) 0.0416(5) Uani 1 1 d . . . B B 0.5737(2) 0.7826(3) 0.18483(19) 0.0331(6) Uani 1 1 d . . . C1 C 0.5208(3) 0.5957(3) 0.2829(2) 0.0502(7) Uani 1 1 d . . . C2 C 0.5495(4) 0.5675(3) 0.3860(2) 0.0780(11) Uani 1 1 d . . . H2A H 0.5096 0.4803 0.3930 0.117 Uiso 1 1 calc R . . H2B H 0.5156 0.6175 0.4322 0.117 Uiso 1 1 calc R . . H2C H 0.6421 0.5863 0.3994 0.117 Uiso 1 1 calc R . . C11 C 0.69021(19) 0.8124(2) 0.01632(16) 0.0310(5) Uani 1 1 d . . . C12 C 0.6315(2) 0.6231(2) 0.06578(19) 0.0423(6) Uani 1 1 d . . . H12A H 0.5938 0.5555 0.1018 0.051 Uiso 1 1 calc R . . C13 C 0.6967(2) 0.6182(2) -0.01435(19) 0.0417(6) Uani 1 1 d . . . H13A H 0.7129 0.5471 -0.0444 0.050 Uiso 1 1 calc R . . C14 C 0.8188(2) 0.7679(2) -0.13087(18) 0.0378(5) Uani 1 1 d . . . C15 C 0.9380(2) 0.8748(3) -0.0976(2) 0.0502(7) Uani 1 1 d . . . H15A H 0.9851 0.8518 -0.0431 0.075 Uiso 1 1 calc R . . H15B H 0.9119 0.9475 -0.0765 0.075 Uiso 1 1 calc R . . H15C H 0.9928 0.8931 -0.1521 0.075 Uiso 1 1 calc R . . C16 C 0.8621(3) 0.6546(3) -0.1645(2) 0.0558(7) Uani 1 1 d . . . H16A H 0.9078 0.6308 -0.1096 0.084 Uiso 1 1 calc R . . H16B H 0.9189 0.6747 -0.2177 0.084 Uiso 1 1 calc R . . H16C H 0.7873 0.5865 -0.1876 0.084 Uiso 1 1 calc R . . C17 C 0.7398(3) 0.7986(3) -0.21572(19) 0.0506(7) Uani 1 1 d . . . H17A H 0.6655 0.7282 -0.2349 0.076 Uiso 1 1 calc R . . H17B H 0.7924 0.8172 -0.2714 0.076 Uiso 1 1 calc R . . H17C H 0.7113 0.8700 -0.1951 0.076 Uiso 1 1 calc R . . C21 C 0.6352(2) 1.0264(2) 0.22622(16) 0.0318(5) Uani 1 1 d . . . C22 C 0.7723(2) 0.9284(2) 0.28132(17) 0.0377(5) Uani 1 1 d . . . H22A H 0.8111 0.8651 0.2922 0.045 Uiso 1 1 calc R . . C23 C 0.8188(2) 1.0469(2) 0.31535(18) 0.0394(6) Uani 1 1 d . . . H23A H 0.8958 1.0818 0.3549 0.047 Uiso 1 1 calc R . . C24 C 0.7460(2) 1.2438(2) 0.3108(2) 0.0432(6) Uani 1 1 d . . . C25 C 0.8656(3) 1.2976(3) 0.3818(2) 0.0615(8) Uani 1 1 d . . . H25A H 0.9414 1.2903 0.3497 0.092 Uiso 1 1 calc R . . H25B H 0.8569 1.2523 0.4404 0.092 Uiso 1 1 calc R . . H25C H 0.8743 1.3843 0.4003 0.092 Uiso 1 1 calc R . . C26 C 0.6280(3) 1.2509(3) 0.3651(2) 0.0601(8) Uani 1 1 d . . . H26A H 0.5521 1.2256 0.3194 0.090 Uiso 1 1 calc R . . H26B H 0.6400 1.3353 0.3925 0.090 Uiso 1 1 calc R . . H26C H 0.6171 1.1961 0.4180 0.090 Uiso 1 1 calc R . . C27 C 0.7606(3) 1.3144(3) 0.2183(2) 0.0681(9) Uani 1 1 d . . . H27A H 0.6814 1.2863 0.1763 0.102 Uiso 1 1 calc R . . H27B H 0.8310 1.2993 0.1829 0.102 Uiso 1 1 calc R . . H27C H 0.7788 1.4024 0.2371 0.102 Uiso 1 1 calc R . . C31 C 0.3467(2) 0.7754(2) 0.23730(18) 0.0391(5) Uani 1 1 d . . . C32 C 0.3594(2) 0.7306(2) 0.07642(18) 0.0396(6) Uani 1 1 d . . . H32A H 0.3932 0.7172 0.0158 0.048 Uiso 1 1 calc R . . C33 C 0.2352(2) 0.7164(2) 0.09055(19) 0.0447(6) Uani 1 1 d . . . H33A H 0.1667 0.6927 0.0416 0.054 Uiso 1 1 calc R . . C34 C 0.1006(2) 0.7335(3) 0.2381(2) 0.0499(7) Uani 1 1 d . . . C35 C 0.1039(3) 0.8601(3) 0.2863(3) 0.0738(10) Uani 1 1 d . . . H35A H 0.1006 0.9158 0.2357 0.111 Uiso 1 1 calc R . . H35B H 0.1828 0.8931 0.3283 0.111 Uiso 1 1 calc R . . H35C H 0.0303 0.8520 0.3258 0.111 Uiso 1 1 calc R . . C36 C -0.0112(3) 0.6923(4) 0.1584(3) 0.0823(11) Uani 1 1 d . . . H36A H -0.0160 0.6100 0.1294 0.123 Uiso 1 1 calc R . . H36B H 0.0029 0.7500 0.1076 0.123 Uiso 1 1 calc R . . H36C H -0.0914 0.6907 0.1878 0.123 Uiso 1 1 calc R . . C37 C 0.0825(3) 0.6364(3) 0.3126(3) 0.0692(9) Uani 1 1 d . . . H37A H 0.0749 0.5560 0.2786 0.104 Uiso 1 1 calc R . . H37B H 0.0049 0.6331 0.3462 0.104 Uiso 1 1 calc R . . H37C H 0.1563 0.6581 0.3605 0.104 Uiso 1 1 calc R . . N1S N 0.8932(4) 0.8326(5) 0.5206(3) 0.1420(19) Uani 1 1 d . . . C1S C 0.8026(3) 0.8600(4) 0.5224(3) 0.0799(11) Uani 1 1 d . . . C2S C 0.6860(3) 0.8963(4) 0.5250(3) 0.0844(11) Uani 1 1 d . . . H2S1 H 0.7069 0.9861 0.5312 0.127 Uiso 1 1 calc R . . H2S2 H 0.6398 0.8637 0.5811 0.127 Uiso 1 1 calc R . . H2S3 H 0.6324 0.8638 0.4646 0.127 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 Pd 0.02651(12) 0.03413(14) 0.02798(14) 0.00379(10) -0.00193(9) 0.01154(10) S1 0.0278(3) 0.0355(3) 0.0354(3) 0.0054(2) 0.0014(2) 0.0107(2) S2 0.0392(3) 0.0543(4) 0.0321(3) -0.0019(3) -0.0050(2) 0.0265(3) S3 0.0473(4) 0.0919(6) 0.0316(4) -0.0036(4) 0.0013(3) 0.0279(4) O1 0.0454(9) 0.0421(10) 0.0334(9) 0.0080(7) 0.0030(7) 0.0138(8) O2 0.0726(14) 0.0553(13) 0.0574(13) 0.0084(10) 0.0110(11) -0.0053(11) N11 0.0345(9) 0.0329(10) 0.0296(10) 0.0021(8) 0.0032(8) 0.0077(8) N12 0.0317(9) 0.0361(11) 0.0311(10) -0.0008(8) 0.0046(8) 0.0095(8) N21 0.0286(9) 0.0394(11) 0.0272(10) 0.0005(8) -0.0015(7) 0.0135(8) N22 0.0323(9) 0.0386(11) 0.0294(10) -0.0003(8) -0.0004(8) 0.0114(8) N31 0.0325(9) 0.0449(12) 0.0279(10) 0.0005(8) 0.0015(8) 0.0095(8) N32 0.0320(10) 0.0536(13) 0.0378(12) 0.0059(10) 0.0014(8) 0.0097(9) B 0.0331(12) 0.0393(15) 0.0277(13) 0.0021(11) 0.0035(10) 0.0116(11) C1 0.0663(17) 0.0463(16) 0.0417(15) 0.0087(13) 0.0139(14) 0.0192(14) C2 0.127(3) 0.062(2) 0.0502(19) 0.0229(16) 0.009(2) 0.029(2) C11 0.0253(10) 0.0383(13) 0.0290(12) -0.0004(9) -0.0006(8) 0.0094(9) C12 0.0516(14) 0.0314(13) 0.0420(14) 0.0022(11) 0.0099(12) 0.0075(11) C13 0.0468(13) 0.0354(13) 0.0419(14) -0.0044(11) 0.0098(11) 0.0106(11) C14 0.0327(11) 0.0462(14) 0.0346(13) 0.0002(11) 0.0093(10) 0.0110(10) C15 0.0337(12) 0.0598(18) 0.0536(17) 0.0028(14) 0.0108(11) 0.0067(12) C16 0.0516(15) 0.0614(18) 0.0610(19) 0.0010(15) 0.0241(14) 0.0242(14) C17 0.0494(14) 0.0718(19) 0.0333(14) 0.0055(13) 0.0043(11) 0.0213(14) C21 0.0304(10) 0.0414(13) 0.0252(11) 0.0006(9) 0.0008(9) 0.0134(9) C22 0.0310(11) 0.0488(15) 0.0367(13) 0.0018(11) -0.0042(10) 0.0184(10) C23 0.0288(11) 0.0510(15) 0.0373(13) -0.0006(11) -0.0051(10) 0.0120(10) C24 0.0464(13) 0.0375(14) 0.0438(15) -0.0009(11) 0.0018(11) 0.0102(11) C25 0.0593(17) 0.0489(17) 0.065(2) -0.0110(14) -0.0113(15) 0.0031(14) C26 0.0657(18) 0.0634(19) 0.0545(18) -0.0167(15) 0.0056(15) 0.0285(15) C27 0.074(2) 0.0542(19) 0.070(2) 0.0205(16) -0.0001(17) 0.0066(16) C31 0.0353(11) 0.0489(15) 0.0337(13) 0.0063(11) 0.0019(10) 0.0124(11) C32 0.0412(12) 0.0441(14) 0.0295(12) 0.0026(10) -0.0003(10) 0.0060(11) C33 0.0394(13) 0.0525(16) 0.0361(14) 0.0021(12) -0.0065(11) 0.0047(11) C34 0.0322(12) 0.0565(17) 0.0596(18) 0.0011(14) 0.0069(12) 0.0106(12) C35 0.0496(17) 0.066(2) 0.112(3) -0.001(2) 0.0066(18) 0.0277(15) C36 0.0349(14) 0.121(3) 0.084(3) 0.000(2) -0.0022(15) 0.0137(17) C37 0.0628(18) 0.068(2) 0.076(2) 0.0193(18) 0.0317(17) 0.0106(16) N1S 0.094(3) 0.262(6) 0.102(3) 0.037(3) 0.004(2) 0.099(3) C1S 0.063(2) 0.130(3) 0.050(2) 0.020(2) -0.0030(16) 0.030(2) C2S 0.068(2) 0.124(3) 0.062(2) -0.003(2) -0.0032(17) 0.033(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 Pd S2 2.3198(6) 2_675 ? Pd S2 2.3198(6) . ? Pd S1 2.3661(5) . ? Pd S1 2.3661(5) 2_675 ? S1 C11 1.737(2) . ? S2 C21 1.723(2) . ? S3 C31 1.688(2) . ? O1 C1 1.340(3) . ? O1 B 1.478(3) . ? O2 C1 1.202(3) . ? N11 C11 1.358(3) . ? N11 C12 1.382(3) . ? N11 B 1.571(3) . ? N12 C11 1.368(3) . ? N12 C13 1.379(3) . ? N12 C14 1.508(3) . ? N21 C21 1.348(3) . ? N21 C22 1.390(3) . ? N21 B 1.556(3) . ? N22 C21 1.368(3) . ? N22 C23 1.386(3) . ? N22 C24 1.501(3) . ? N31 C31 1.368(3) . ? N31 C32 1.386(3) . ? N31 B 1.526(3) . ? N32 C31 1.377(3) . ? N32 C33 1.384(3) . ? N32 C34 1.509(3) . ? C1 C2 1.496(4) . ? C12 C13 1.335(3) . ? C14 C17 1.519(3) . ? C14 C15 1.524(3) . ? C14 C16 1.530(4) . ? C22 C23 1.331(3) . ? C24 C27 1.526(4) . ? C24 C26 1.527(4) . ? C24 C25 1.529(4) . ? C32 C33 1.335(3) . ? C34 C35 1.520(4) . ? C34 C37 1.522(4) . ? C34 C36 1.533(4) . ? N1S C1S 1.109(5) . ? C1S C2S 1.434(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 S2 Pd S2 180.00(3) 2_675 . ? S2 Pd S1 84.290(19) 2_675 . ? S2 Pd S1 95.71(2) . . ? S2 Pd S1 95.71(2) 2_675 2_675 ? S2 Pd S1 84.290(19) . 2_675 ? S1 Pd S1 180.0 . 2_675 ? C11 S1 Pd 108.53(7) . . ? C21 S2 Pd 108.68(8) . . ? C1 O1 B 126.5(2) . . ? C11 N11 C12 107.70(19) . . ? C11 N11 B 131.24(19) . . ? C12 N11 B 120.75(19) . . ? C11 N12 C13 108.03(19) . . ? C11 N12 C14 129.02(19) . . ? C13 N12 C14 122.92(19) . . ? C21 N21 C22 108.01(19) . . ? C21 N21 B 132.04(18) . . ? C22 N21 B 119.84(19) . . ? C21 N22 C23 107.72(19) . . ? C21 N22 C24 127.33(19) . . ? C23 N22 C24 124.80(19) . . ? C31 N31 C32 108.49(19) . . ? C31 N31 B 125.72(19) . . ? C32 N31 B 125.3(2) . . ? C31 N32 C33 108.62(19) . . ? C31 N32 C34 126.2(2) . . ? C33 N32 C34 125.1(2) . . ? O1 B N31 112.52(19) . . ? O1 B N21 102.67(18) . . ? N31 B N21 115.0(2) . . ? O1 B N11 106.92(19) . . ? N31 B N11 109.58(19) . . ? N21 B N11 109.68(18) . . ? O2 C1 O1 123.8(3) . . ? O2 C1 C2 124.0(3) . . ? O1 C1 C2 112.1(3) . . ? N11 C11 N12 107.64(19) . . ? N11 C11 S1 126.41(17) . . ? N12 C11 S1 125.95(17) . . ? C13 C12 N11 108.7(2) . . ? C12 C13 N12 107.9(2) . . ? N12 C14 C17 109.39(19) . . ? N12 C14 C15 109.52(19) . . ? C17 C14 C15 112.1(2) . . ? N12 C14 C16 108.4(2) . . ? C17 C14 C16 108.7(2) . . ? C15 C14 C16 108.6(2) . . ? N21 C21 N22 107.91(18) . . ? N21 C21 S2 126.51(17) . . ? N22 C21 S2 125.57(17) . . ? C23 C22 N21 108.3(2) . . ? C22 C23 N22 108.1(2) . . ? N22 C24 C27 109.1(2) . . ? N22 C24 C26 108.3(2) . . ? C27 C24 C26 112.9(3) . . ? N22 C24 C25 109.0(2) . . ? C27 C24 C25 109.3(2) . . ? C26 C24 C25 108.1(2) . . ? N31 C31 N32 106.5(2) . . ? N31 C31 S3 125.39(17) . . ? N32 C31 S3 128.09(19) . . ? C33 C32 N31 108.4(2) . . ? C32 C33 N32 107.9(2) . . ? N32 C34 C35 109.2(2) . . ? N32 C34 C37 109.2(2) . . ? C35 C34 C37 111.8(3) . . ? N32 C34 C36 108.7(2) . . ? C35 C34 C36 109.2(3) . . ? C37 C34 C36 108.7(3) . . ? N1S C1S C2S 179.6(6) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.407 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.057 # Attachment 'TMPDS10.CIF' data_tmpds10 _database_code_depnum_ccdc_archive 'CCDC 617726' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H72 B2 N14 Pd2 S6' _chemical_formula_weight 1247.96 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' Pd Pd -0.9988 1.0072 '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)/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 12.6473(6) _cell_length_b 18.2555(9) _cell_length_c 12.4059(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.6250(10) _cell_angle_gamma 90.00 _cell_volume 2805.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 4722 _cell_measurement_theta_min 2.77 _cell_measurement_theta_max 25.66 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8755 _exptl_absorpt_correction_T_max 0.9820 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19957 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0760 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 28.35 _reflns_number_total 6611 _reflns_number_gt 4207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.0246P)^2^+2.5115P] 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 6611 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0916 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd -0.09746(2) -0.036352(16) 0.55805(2) 0.02879(9) Uani 1 1 d . . . S1 S 0.02876(8) -0.12142(6) 0.52817(8) 0.0360(2) Uani 1 1 d . . . S2 S -0.24207(8) 0.00687(6) 0.63631(8) 0.0383(2) Uani 1 1 d . . . S3 S 0.20875(7) 0.04229(5) 0.63997(7) 0.0306(2) Uani 1 1 d . . . N11 N 0.0855(2) -0.08397(15) 0.7398(2) 0.0295(7) Uani 1 1 d . . . N12 N 0.2026(2) -0.16098(16) 0.6936(3) 0.0323(7) Uani 1 1 d . . . N21 N -0.0877(2) -0.04405(15) 0.7974(2) 0.0299(7) Uani 1 1 d . . . N22 N -0.2421(3) -0.03942(17) 0.8522(2) 0.0361(7) Uani 1 1 d . . . N31 N 0.0380(2) 0.05080(15) 0.7452(2) 0.0272(7) Uani 1 1 d . . . N32 N 0.1288(2) 0.15400(15) 0.7519(2) 0.0297(7) Uani 1 1 d . . . B B -0.0086(3) -0.0284(2) 0.7174(3) 0.0278(9) Uani 1 1 d . . . C11 C 0.1087(3) -0.12453(19) 0.6563(3) 0.0279(8) Uani 1 1 d . . . C12 C 0.1689(3) -0.0940(2) 0.8301(3) 0.0364(9) Uani 1 1 d . . . H12A H 0.1745 -0.0714 0.8991 0.044 Uiso 1 1 calc R . . C13 C 0.2395(3) -0.1409(2) 0.8029(3) 0.0409(10) Uani 1 1 d . . . H13A H 0.3032 -0.1575 0.8492 0.049 Uiso 1 1 calc R . . C14 C 0.2597(3) -0.2093(2) 0.6253(3) 0.0368(10) Uani 1 1 d . . . C15 C 0.3609(3) -0.2397(2) 0.6985(4) 0.0565(13) Uani 1 1 d . . . H15A H 0.3410 -0.2698 0.7557 0.085 Uiso 1 1 calc R . . H15B H 0.4062 -0.1996 0.7319 0.085 Uiso 1 1 calc R . . H15C H 0.4002 -0.2692 0.6546 0.085 Uiso 1 1 calc R . . C16 C 0.2896(4) -0.1623(3) 0.5349(4) 0.0631(14) Uani 1 1 d . . . H16A H 0.3371 -0.1230 0.5676 0.095 Uiso 1 1 calc R . . H16B H 0.2247 -0.1416 0.4902 0.095 Uiso 1 1 calc R . . H16C H 0.3262 -0.1923 0.4891 0.095 Uiso 1 1 calc R . . C17 C 0.1853(3) -0.2721(2) 0.5791(4) 0.0534(12) Uani 1 1 d . . . H17A H 0.1683 -0.3007 0.6392 0.080 Uiso 1 1 calc R . . H17B H 0.2210 -0.3030 0.5337 0.080 Uiso 1 1 calc R . . H17C H 0.1193 -0.2526 0.5348 0.080 Uiso 1 1 calc R . . C21 C -0.1928(3) -0.02652(19) 0.7654(3) 0.0313(9) Uani 1 1 d . . . C22 C -0.0699(3) -0.0676(2) 0.9058(3) 0.0360(9) Uani 1 1 d . . . H22A H -0.0035 -0.0828 0.9483 0.043 Uiso 1 1 calc R . . C23 C -0.1636(3) -0.0649(2) 0.9391(3) 0.0394(10) Uani 1 1 d . . . H23A H -0.1748 -0.0779 1.0092 0.047 Uiso 1 1 calc R . . C24 C -0.3588(3) -0.0260(2) 0.8549(3) 0.0437(11) Uani 1 1 d . . . C25 C -0.3812(4) -0.0555(3) 0.9639(4) 0.0631(15) Uani 1 1 d . . . H25A H -0.3366 -0.0295 1.0248 0.095 Uiso 1 1 calc R . . H25B H -0.3643 -0.1073 0.9699 0.095 Uiso 1 1 calc R . . H25C H -0.4567 -0.0482 0.9660 0.095 Uiso 1 1 calc R . . C26 C -0.3803(4) 0.0554(2) 0.8476(4) 0.0569(13) Uani 1 1 d . . . H26A H -0.3663 0.0739 0.7785 0.085 Uiso 1 1 calc R . . H26B H -0.3332 0.0800 0.9083 0.085 Uiso 1 1 calc R . . H26C H -0.4550 0.0647 0.8513 0.085 Uiso 1 1 calc R . . C27 C -0.4311(4) -0.0673(3) 0.7613(4) 0.0606(14) Uani 1 1 d . . . H27A H -0.4179 -0.0498 0.6914 0.091 Uiso 1 1 calc R . . H27B H -0.5061 -0.0592 0.7646 0.091 Uiso 1 1 calc R . . H27C H -0.4152 -0.1193 0.7684 0.091 Uiso 1 1 calc R . . C31 C 0.1241(3) 0.08331(19) 0.7133(3) 0.0267(8) Uani 1 1 d . . . C32 C -0.0116(3) 0.1028(2) 0.7990(3) 0.0346(9) Uani 1 1 d . . . H32A H -0.0742 0.0954 0.8275 0.042 Uiso 1 1 calc R . . C33 C 0.0440(3) 0.1653(2) 0.8038(3) 0.0374(10) Uani 1 1 d . . . H33A H 0.0279 0.2092 0.8369 0.045 Uiso 1 1 calc R . . C34 C 0.2081(3) 0.2130(2) 0.7368(3) 0.0344(9) Uani 1 1 d . . . C35 C 0.1829(4) 0.2822(2) 0.7948(4) 0.0537(13) Uani 1 1 d . . . H35A H 0.1896 0.2724 0.8727 0.081 Uiso 1 1 calc R . . H35B H 0.1098 0.2980 0.7639 0.081 Uiso 1 1 calc R . . H35C H 0.2332 0.3206 0.7848 0.081 Uiso 1 1 calc R . . C36 C 0.1976(3) 0.2290(2) 0.6145(3) 0.0406(10) Uani 1 1 d . . . H36A H 0.1246 0.2451 0.5839 0.061 Uiso 1 1 calc R . . H36B H 0.2133 0.1849 0.5770 0.061 Uiso 1 1 calc R . . H36C H 0.2482 0.2672 0.6049 0.061 Uiso 1 1 calc R . . C37 C 0.3217(3) 0.1877(2) 0.7900(3) 0.0485(11) Uani 1 1 d . . . H37A H 0.3252 0.1782 0.8675 0.073 Uiso 1 1 calc R . . H37B H 0.3733 0.2256 0.7819 0.073 Uiso 1 1 calc R . . H37C H 0.3388 0.1432 0.7543 0.073 Uiso 1 1 calc R . . N1S N 0.5210(5) -0.2578(4) 0.4505(5) 0.102(2) Uani 1 1 d . . . C1S C 0.5368(5) -0.1980(5) 0.4530(5) 0.0759(19) Uani 1 1 d . . . C2S C 0.5528(5) -0.1191(4) 0.4538(5) 0.101(2) Uani 1 1 d . . . H2S1 H 0.5857 -0.1053 0.3925 0.151 Uiso 1 1 calc R . . H2S2 H 0.5997 -0.1047 0.5223 0.151 Uiso 1 1 calc R . . H2S3 H 0.4837 -0.0947 0.4470 0.151 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 Pd 0.03085(15) 0.02912(15) 0.02691(15) -0.00026(14) 0.00699(11) 0.00208(14) S1 0.0345(6) 0.0400(6) 0.0327(6) -0.0079(4) 0.0046(4) 0.0060(5) S2 0.0366(6) 0.0443(6) 0.0362(6) 0.0068(5) 0.0128(5) 0.0069(5) S3 0.0290(5) 0.0322(5) 0.0319(5) -0.0037(4) 0.0089(4) 0.0006(4) N11 0.0364(18) 0.0236(17) 0.0277(17) 0.0005(13) 0.0047(14) 0.0005(14) N12 0.0318(18) 0.0264(17) 0.039(2) 0.0007(14) 0.0068(15) 0.0033(14) N21 0.0357(18) 0.0241(17) 0.0307(17) 0.0007(14) 0.0084(13) -0.0001(14) N22 0.0449(19) 0.0302(17) 0.0381(19) -0.0003(16) 0.0198(16) -0.0017(16) N31 0.0339(17) 0.0221(17) 0.0274(16) -0.0016(12) 0.0106(13) 0.0004(13) N32 0.0372(18) 0.0226(16) 0.0318(18) -0.0013(13) 0.0129(14) -0.0018(14) B 0.034(2) 0.023(2) 0.026(2) 0.0028(18) 0.0052(18) 0.0012(19) C11 0.031(2) 0.0239(19) 0.030(2) 0.0000(16) 0.0097(17) -0.0027(16) C12 0.042(2) 0.039(2) 0.027(2) 0.0011(17) 0.0009(18) 0.0073(19) C13 0.043(3) 0.040(2) 0.034(2) 0.0055(19) -0.0042(19) 0.005(2) C14 0.034(2) 0.030(2) 0.050(3) 0.0021(19) 0.0177(19) 0.0065(18) C15 0.046(3) 0.047(3) 0.075(3) -0.001(2) 0.006(2) 0.013(2) C16 0.058(3) 0.063(3) 0.080(4) 0.018(3) 0.043(3) 0.017(3) C17 0.053(3) 0.039(3) 0.073(3) -0.016(2) 0.023(2) 0.003(2) C21 0.039(2) 0.025(2) 0.032(2) -0.0033(16) 0.0141(17) -0.0016(17) C22 0.052(3) 0.029(2) 0.025(2) 0.0019(17) 0.0034(18) -0.0046(19) C23 0.056(3) 0.039(2) 0.028(2) 0.0026(18) 0.018(2) -0.005(2) C24 0.049(3) 0.036(2) 0.053(3) -0.001(2) 0.027(2) -0.002(2) C25 0.068(3) 0.060(3) 0.074(4) 0.008(3) 0.044(3) 0.003(3) C26 0.061(3) 0.042(3) 0.076(3) 0.000(2) 0.035(3) 0.008(2) C27 0.049(3) 0.065(3) 0.074(4) -0.016(3) 0.027(3) -0.020(2) C31 0.032(2) 0.027(2) 0.0199(18) 0.0018(15) 0.0029(15) 0.0000(16) C32 0.041(2) 0.032(2) 0.036(2) -0.0029(17) 0.0214(19) 0.0027(18) C33 0.049(3) 0.027(2) 0.043(2) -0.0054(18) 0.022(2) -0.0008(19) C34 0.039(2) 0.026(2) 0.039(2) 0.0004(17) 0.0094(19) -0.0078(17) C35 0.076(3) 0.030(2) 0.064(3) -0.010(2) 0.033(3) -0.017(2) C36 0.050(3) 0.033(2) 0.040(2) 0.0066(18) 0.011(2) -0.0079(19) C37 0.047(3) 0.045(3) 0.048(3) 0.002(2) -0.005(2) -0.014(2) N1S 0.096(4) 0.117(5) 0.089(4) -0.002(4) 0.007(3) 0.036(4) C1S 0.043(3) 0.129(6) 0.056(4) -0.012(5) 0.009(3) 0.015(4) C2S 0.074(4) 0.140(7) 0.099(5) -0.047(5) 0.042(4) -0.035(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd B 2.073(4) . ? Pd S1 2.3099(10) . ? Pd S2 2.3720(10) . ? Pd S3 2.5757(10) 3_556 ? S1 C11 1.704(4) . ? S2 C21 1.710(4) . ? S3 C31 1.711(3) . ? S3 Pd 2.5757(10) 3_556 ? N11 C11 1.353(4) . ? N11 C12 1.387(4) . ? N11 B 1.546(5) . ? N12 C11 1.360(4) . ? N12 C13 1.390(5) . ? N12 C14 1.504(4) . ? N21 C21 1.346(4) . ? N21 C22 1.386(4) . ? N21 B 1.570(5) . ? N22 C21 1.369(4) . ? N22 C23 1.390(5) . ? N22 C24 1.503(5) . ? N31 C31 1.366(4) . ? N31 C32 1.382(4) . ? N31 B 1.574(5) . ? N32 C31 1.373(4) . ? N32 C33 1.374(4) . ? N32 C34 1.509(4) . ? C12 C13 1.329(5) . ? C14 C15 1.518(5) . ? C14 C16 1.520(5) . ? C14 C17 1.520(5) . ? C22 C23 1.332(5) . ? C24 C26 1.511(5) . ? C24 C27 1.525(6) . ? C24 C25 1.533(5) . ? C32 C33 1.334(5) . ? C34 C35 1.520(5) . ? C34 C36 1.524(5) . ? C34 C37 1.526(5) . ? N1S C1S 1.110(8) . ? C1S C2S 1.453(9) . ? 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 B Pd S1 86.60(11) . . ? B Pd S2 84.30(11) . . ? S1 Pd S2 154.70(4) . . ? B Pd S3 178.40(12) . 3_556 ? S1 Pd S3 94.65(3) . 3_556 ? S2 Pd S3 94.94(3) . 3_556 ? C11 S1 Pd 99.90(12) . . ? C21 S2 Pd 95.70(12) . . ? C31 S3 Pd 104.20(12) . 3_556 ? C11 N11 C12 107.4(3) . . ? C11 N11 B 120.0(3) . . ? C12 N11 B 131.6(3) . . ? C11 N12 C13 107.6(3) . . ? C11 N12 C14 125.5(3) . . ? C13 N12 C14 126.8(3) . . ? C21 N21 C22 108.5(3) . . ? C21 N21 B 119.2(3) . . ? C22 N21 B 132.0(3) . . ? C21 N22 C23 107.5(3) . . ? C21 N22 C24 126.5(3) . . ? C23 N22 C24 126.0(3) . . ? C31 N31 C32 107.8(3) . . ? C31 N31 B 128.4(3) . . ? C32 N31 B 123.4(3) . . ? C31 N32 C33 108.8(3) . . ? C31 N32 C34 127.6(3) . . ? C33 N32 C34 123.5(3) . . ? N11 B N21 109.5(3) . . ? N11 B N31 108.8(3) . . ? N21 B N31 106.7(3) . . ? N11 B Pd 112.0(2) . . ? N21 B Pd 107.3(2) . . ? N31 B Pd 112.3(2) . . ? N11 C11 N12 108.4(3) . . ? N11 C11 S1 121.1(3) . . ? N12 C11 S1 130.4(3) . . ? C13 C12 N11 108.7(3) . . ? C12 C13 N12 107.9(3) . . ? N12 C14 C15 108.7(3) . . ? N12 C14 C16 107.7(3) . . ? C15 C14 C16 110.0(3) . . ? N12 C14 C17 108.9(3) . . ? C15 C14 C17 109.4(3) . . ? C16 C14 C17 112.0(4) . . ? N21 C21 N22 107.9(3) . . ? N21 C21 S2 120.8(3) . . ? N22 C21 S2 131.3(3) . . ? C23 C22 N21 108.0(4) . . ? C22 C23 N22 108.2(3) . . ? N22 C24 C26 108.9(3) . . ? N22 C24 C27 110.0(3) . . ? C26 C24 C27 111.6(4) . . ? N22 C24 C25 108.6(4) . . ? C26 C24 C25 109.6(3) . . ? C27 C24 C25 108.0(4) . . ? N31 C31 N32 106.8(3) . . ? N31 C31 S3 125.7(3) . . ? N32 C31 S3 127.5(3) . . ? C33 C32 N31 108.9(3) . . ? C32 C33 N32 107.7(3) . . ? N32 C34 C35 109.1(3) . . ? N32 C34 C36 109.4(3) . . ? C35 C34 C36 109.1(3) . . ? N32 C34 C37 108.8(3) . . ? C35 C34 C37 108.4(3) . . ? C36 C34 C37 112.0(3) . . ? N1S C1S C2S 177.6(8) . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.589 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.091