# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 440/121 data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32 H41 Cl N P2 S Tc' _chemical_formula_weight 667.11 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tc' 'Tc' -1.4390 0.7593 '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 12.437(4) _cell_length_b 13.441(4) _cell_length_c 19.060(6) _cell_angle_alpha 90.00 _cell_angle_beta 102.05(3) _cell_angle_gamma 90.00 _cell_volume 3116(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 50 _cell_measurement_theta_min 8.3 _cell_measurement_theta_max 14.6 _exptl_crystal_description 'rectangular plates' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method ? _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.452 _exptl_absorpt_correction_T_max 0.763 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nicolet R3m/V' _diffrn_measurement_method theta-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.7 _diffrn_reflns_number 4563 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0571 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 24.07 _reflns_number_total 4323 _reflns_number_observed 3107 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P3/P4-PC Vers.4.27 (1991)' _computing_cell_refinement " " _computing_data_reduction 'SHELXTL/PC V.5.3 (Sheldrick, 1994)' _computing_structure_solution " " _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC V.5.3 (Sheldrick, 1994)' _computing_publication_material " " _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+0.0486P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom method' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0003(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4320 _refine_ls_number_parameters 339 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_obs 0.0433 _refine_ls_wR_factor_all 0.1183 _refine_ls_wR_factor_obs 0.0993 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.049 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.049 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tc Tc 0.51777(4) 0.17949(4) 0.12348(2) 0.0333(2) Uani 1 d . . Cl Cl 0.59206(13) 0.26938(12) 0.22995(7) 0.0486(4) Uani 1 d . . S1 S 0.38624(13) 0.06040(12) 0.08302(9) 0.0462(4) Uani 1 d . . P1 P 0.62510(13) 0.03838(11) 0.17117(8) 0.0395(4) Uani 1 d . . P2 P 0.36655(13) 0.29719(11) 0.10997(7) 0.0346(4) Uani 1 d . . N1 N 0.5749(4) 0.2106(4) 0.0596(2) 0.0455(13) Uiso 1 d . . C1 C 0.5666(5) -0.0666(5) 0.1162(3) 0.049(2) Uani 1 d . . H1A H 0.5939(5) -0.0667(5) 0.0722(3) 0.058 Uiso 1 calc R . H1B H 0.5901(5) -0.1280(5) 0.1417(3) 0.058 Uiso 1 calc R . C2 C 0.4457(6) -0.0632(4) 0.0986(4) 0.057(2) Uani 1 d . . H2A H 0.4184(6) -0.0937(4) 0.1376(4) 0.068 Uiso 1 calc R . H2B H 0.4200(6) -0.1031(4) 0.0560(4) 0.068 Uiso 1 calc R . C1A C 0.6187(5) 0.0132(4) 0.2643(3) 0.042(2) Uani 1 d . . H1AA H 0.6601(5) 0.0669(4) 0.2926(3) 0.050 Uiso 1 calc R . C2A C 0.6746(7) -0.0823(6) 0.2938(4) 0.075(2) Uani 1 d . . H2AA H 0.6360(7) -0.1385(6) 0.2683(4) 0.090 Uiso 1 calc R . H2AB H 0.7494(7) -0.0829(6) 0.2864(4) 0.090 Uiso 1 calc R . C3A C 0.6757(7) -0.0917(7) 0.3722(4) 0.088(3) Uani 1 d . . H3AA H 0.7094(7) -0.1545(7) 0.3896(4) 0.105 Uiso 1 calc R . H3AB H 0.7202(7) -0.0386(7) 0.3979(4) 0.105 Uiso 1 calc R . C4A C 0.5642(7) -0.0868(6) 0.3875(4) 0.078(2) Uani 1 d . . H4AA H 0.5694(7) -0.0886(6) 0.4390(4) 0.093 Uiso 1 calc R . H4AB H 0.5222(7) -0.1443(6) 0.3668(4) 0.093 Uiso 1 calc R . C5A C 0.5055(6) 0.0063(6) 0.3574(4) 0.070(2) Uani 1 d . . H5AA H 0.5415(6) 0.0633(6) 0.3834(4) 0.084 Uiso 1 calc R . H5AB H 0.4305(6) 0.0042(6) 0.3645(4) 0.084 Uiso 1 calc R . C6A C 0.5038(5) 0.0190(6) 0.2786(3) 0.060(2) Uani 1 d . . H6AA H 0.4715(5) 0.0828(6) 0.2625(3) 0.072 Uiso 1 calc R . H6AB H 0.4586(5) -0.0327(6) 0.2516(3) 0.072 Uiso 1 calc R . C1B C 0.7698(5) 0.0358(5) 0.1687(3) 0.050(2) Uani 1 d . . H1BA H 0.7981(5) -0.0293(5) 0.1872(3) 0.061 Uiso 1 calc R . C2B C 0.8343(5) 0.1129(6) 0.2166(4) 0.067(2) Uani 1 d . . H2BA H 0.8240(5) 0.1032(6) 0.2652(4) 0.080 Uiso 1 calc R . H2BB H 0.8063(5) 0.1784(6) 0.2009(4) 0.080 Uiso 1 calc R . C3B C 0.9551(6) 0.1089(8) 0.2165(5) 0.091(3) Uani 1 d . . H3BA H 0.9920(6) 0.1640(8) 0.2445(5) 0.109 Uiso 1 calc R . H3BB H 0.9857(6) 0.0476(8) 0.2392(5) 0.109 Uiso 1 calc R . C4B C 0.9766(7) 0.1139(6) 0.1423(5) 0.083(2) Uani 1 d . . H4BA H 0.9577(7) 0.1798(6) 0.1227(5) 0.099 Uiso 1 calc R . H4BB H 1.0543(7) 0.1034(6) 0.1443(5) 0.099 Uiso 1 calc R . C5B C 0.9126(7) 0.0389(7) 0.0940(5) 0.088(3) Uani 1 d . . H5BA H 0.9391(7) -0.0270(7) 0.1095(5) 0.106 Uiso 1 calc R . H5BB H 0.9241(7) 0.0489(7) 0.0457(5) 0.106 Uiso 1 calc R . C6B C 0.7911(6) 0.0452(6) 0.0934(4) 0.067(2) Uani 1 d . . H6BA H 0.7527(6) -0.0075(6) 0.0635(4) 0.080 Uiso 1 calc R . H6BB H 0.7626(6) 0.1084(6) 0.0729(4) 0.080 Uiso 1 calc R . C1C C 0.3131(5) 0.2984(4) 0.1908(3) 0.0377(14) Uani 1 d . . C2C C 0.2768(5) 0.2116(5) 0.2150(3) 0.050(2) Uani 1 d . . H2CA H 0.2725(5) 0.1545(5) 0.1871(3) 0.059 Uiso 1 calc R . C3C C 0.2465(6) 0.2082(6) 0.2802(4) 0.064(2) Uani 1 d . . H3CA H 0.2215(6) 0.1486(6) 0.2957(4) 0.077 Uiso 1 calc R . C4C C 0.2524(6) 0.2893(6) 0.3219(4) 0.065(2) Uani 1 d . . H4CA H 0.2326(6) 0.2860(6) 0.3663(4) 0.078 Uiso 1 calc R . C5C C 0.2876(6) 0.3761(6) 0.2983(4) 0.065(2) Uani 1 d . . H5CA H 0.2917(6) 0.4328(6) 0.3266(4) 0.078 Uiso 1 calc R . C6C C 0.3175(5) 0.3810(5) 0.2326(3) 0.051(2) Uani 1 d . . H6CA H 0.3409(5) 0.4412(5) 0.2169(3) 0.062 Uiso 1 calc R . C1D C 0.3978(5) 0.4252(4) 0.0939(3) 0.0388(15) Uani 1 d . . C2D C 0.5052(6) 0.4561(5) 0.1038(3) 0.047(2) Uani 1 d . . H2DA H 0.5624(6) 0.4114(5) 0.1189(3) 0.057 Uiso 1 calc R . C3D C 0.5273(7) 0.5541(5) 0.0909(4) 0.061(2) Uani 1 d . . H3DA H 0.5998(7) 0.5755(5) 0.0969(4) 0.073 Uiso 1 calc R . C4D C 0.4445(7) 0.6192(5) 0.0697(3) 0.060(2) Uani 1 d . . H4DA H 0.4604(7) 0.6855(5) 0.0621(3) 0.072 Uiso 1 calc R . C5D C 0.3395(7) 0.5898(5) 0.0596(3) 0.060(2) Uani 1 d . . H5DA H 0.2832(7) 0.6354(5) 0.0443(3) 0.072 Uiso 1 calc R . C6D C 0.3145(6) 0.4927(5) 0.0716(3) 0.052(2) Uani 1 d . . H6DA H 0.2416(6) 0.4725(5) 0.0647(3) 0.063 Uiso 1 calc R . C1E C 0.2521(5) 0.2710(4) 0.0368(3) 0.0400(15) Uani 1 d . . C2E C 0.2762(5) 0.2560(5) -0.0295(3) 0.047(2) Uani 1 d . . H2EA H 0.3490(5) 0.2559(5) -0.0346(3) 0.056 Uiso 1 calc R . C3E C 0.1942(6) 0.2414(5) -0.0874(3) 0.056(2) Uani 1 d . . H3EA H 0.2110(6) 0.2345(5) -0.1325(3) 0.067 Uiso 1 calc R . C4E C 0.0881(6) 0.2367(5) -0.0809(4) 0.058(2) Uani 1 d . . H4EA H 0.0328(6) 0.2238(5) -0.1209(4) 0.069 Uiso 1 calc R . C5E C 0.0629(6) 0.2507(6) -0.0158(4) 0.062(2) Uani 1 d . . H5EA H -0.0099(6) 0.2482(6) -0.0109(4) 0.075 Uiso 1 calc R . C6E C 0.1458(6) 0.2688(5) 0.0431(3) 0.049(2) Uani 1 d . . H6EA H 0.1285(6) 0.2797(5) 0.0876(3) 0.059 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 Tc 0.0370(4) 0.0299(3) 0.0324(3) 0.0011(2) 0.0058(2) -0.0003(2) Cl 0.0553(11) 0.0449(9) 0.0401(8) -0.0031(7) -0.0025(7) -0.0035(8) S1 0.0424(11) 0.0413(9) 0.0517(9) -0.0096(7) 0.0023(8) -0.0041(8) P1 0.0401(11) 0.0315(8) 0.0467(9) 0.0045(7) 0.0090(7) 0.0028(7) P2 0.0383(10) 0.0328(9) 0.0330(8) -0.0004(6) 0.0083(7) -0.0010(7) C1 0.046(5) 0.037(4) 0.065(4) -0.013(3) 0.016(3) 0.000(3) C2 0.068(6) 0.031(4) 0.071(5) -0.013(3) 0.013(4) -0.008(3) C1A 0.048(5) 0.031(3) 0.045(3) 0.006(3) 0.008(3) 0.000(3) C2A 0.083(6) 0.063(5) 0.083(5) 0.033(4) 0.027(4) 0.030(4) C3A 0.090(7) 0.093(7) 0.084(6) 0.052(5) 0.026(5) 0.023(5) C4A 0.099(7) 0.071(5) 0.068(5) 0.028(4) 0.030(5) -0.003(5) C5A 0.076(6) 0.074(5) 0.071(5) 0.015(4) 0.038(4) 0.005(4) C6A 0.044(5) 0.076(5) 0.066(4) 0.010(4) 0.025(4) 0.004(4) C1B 0.047(5) 0.041(4) 0.064(4) 0.014(3) 0.014(3) 0.007(3) C2B 0.041(5) 0.099(6) 0.061(4) -0.001(4) 0.012(3) -0.013(4) C3B 0.048(6) 0.126(8) 0.095(6) 0.009(6) 0.010(5) -0.008(5) C4B 0.062(6) 0.072(6) 0.121(7) 0.002(5) 0.035(5) -0.010(5) C5B 0.071(7) 0.088(6) 0.123(7) -0.014(6) 0.057(5) -0.005(5) C6B 0.055(5) 0.079(5) 0.074(5) -0.014(4) 0.032(4) -0.012(4) C1C 0.036(4) 0.043(4) 0.035(3) 0.001(3) 0.009(3) -0.002(3) C2C 0.049(5) 0.051(4) 0.051(4) 0.002(3) 0.017(3) -0.003(3) C3C 0.066(5) 0.068(5) 0.065(5) 0.023(4) 0.032(4) 0.001(4) C4C 0.081(6) 0.073(5) 0.050(4) 0.007(4) 0.032(4) 0.014(4) C5C 0.082(6) 0.065(5) 0.054(4) -0.019(4) 0.028(4) 0.013(4) C6C 0.062(5) 0.046(4) 0.050(4) -0.006(3) 0.022(3) -0.001(3) C1D 0.050(5) 0.035(3) 0.033(3) 0.000(3) 0.012(3) -0.002(3) C2D 0.053(5) 0.039(4) 0.049(4) 0.008(3) 0.011(3) -0.002(3) C3D 0.071(6) 0.049(5) 0.066(5) 0.003(4) 0.023(4) -0.017(4) C4D 0.099(7) 0.033(4) 0.047(4) 0.006(3) 0.014(4) -0.003(5) C5D 0.077(6) 0.040(4) 0.059(4) 0.005(3) 0.006(4) 0.018(4) C6D 0.056(5) 0.044(4) 0.059(4) 0.003(3) 0.017(3) 0.008(4) C1E 0.038(5) 0.041(3) 0.041(3) 0.000(3) 0.009(3) 0.001(3) C2E 0.044(4) 0.056(4) 0.039(3) -0.001(3) 0.007(3) 0.004(3) C3E 0.064(6) 0.062(5) 0.038(4) 0.000(3) 0.003(3) 0.010(4) C4E 0.056(6) 0.055(4) 0.052(4) -0.002(3) -0.011(4) 0.002(4) C5E 0.038(4) 0.084(6) 0.060(5) 0.003(4) -0.003(3) -0.009(4) C6E 0.042(5) 0.064(4) 0.043(4) -0.005(3) 0.010(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tc N1 1.590(5) . ? Tc S1 2.303(2) . ? Tc Cl 2.377(2) . ? Tc P1 2.387(2) . ? Tc P2 2.430(2) . ? S1 C2 1.817(6) . ? P1 C1B 1.810(7) . ? P1 C1 1.817(6) . ? P1 C1A 1.826(6) . ? P2 C1C 1.802(6) . ? P2 C1D 1.804(6) . ? P2 C1E 1.807(6) . ? C1 C2 1.471(9) . ? C1A C6A 1.511(8) . ? C1A C2A 1.511(8) . ? C2A C3A 1.497(10) . ? C3A C4A 1.477(10) . ? C4A C5A 1.500(10) . ? C5A C6A 1.508(9) . ? C1B C2B 1.499(9) . ? C1B C6B 1.520(9) . ? C2B C3B 1.504(10) . ? C3B C4B 1.496(11) . ? C4B C5B 1.480(11) . ? C5B C6B 1.511(10) . ? C1C C6C 1.361(8) . ? C1C C2C 1.365(8) . ? C2C C3C 1.372(8) . ? C3C C4C 1.343(9) . ? C4C C5C 1.356(10) . ? C5C C6C 1.379(8) . ? C1D C2D 1.374(8) . ? C1D C6D 1.375(8) . ? C2D C3D 1.378(9) . ? C3D C4D 1.348(9) . ? C4D C5D 1.339(9) . ? C5D C6D 1.372(9) . ? C1E C6E 1.352(8) . ? C1E C2E 1.375(8) . ? C2E C3E 1.351(8) . ? C3E C4E 1.352(9) . ? C4E C5E 1.356(9) . ? C5E C6E 1.378(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Tc S1 109.0(2) . . ? N1 Tc Cl 111.4(2) . . ? S1 Tc Cl 139.59(6) . . ? N1 Tc P1 101.4(2) . . ? S1 Tc P1 82.93(6) . . ? Cl Tc P1 89.54(6) . . ? N1 Tc P2 102.0(2) . . ? S1 Tc P2 86.39(6) . . ? Cl Tc P2 85.06(6) . . ? P1 Tc P2 156.43(6) . . ? C2 S1 Tc 110.1(2) . . ? C1B P1 C1 104.6(3) . . ? C1B P1 C1A 105.5(3) . . ? C1 P1 C1A 108.8(3) . . ? C1B P1 Tc 119.0(2) . . ? C1 P1 Tc 105.8(2) . . ? C1A P1 Tc 112.5(2) . . ? C1C P2 C1D 105.5(3) . . ? C1C P2 C1E 106.8(3) . . ? C1D P2 C1E 102.6(3) . . ? C1C P2 Tc 109.3(2) . . ? C1D P2 Tc 116.7(2) . . ? C1E P2 Tc 115.0(2) . . ? C2 C1 P1 112.0(4) . . ? C1 C2 S1 115.3(4) . . ? C6A C1A C2A 110.9(6) . . ? C6A C1A P1 113.6(4) . . ? C2A C1A P1 114.1(5) . . ? C3A C2A C1A 110.5(6) . . ? C4A C3A C2A 112.4(7) . . ? C3A C4A C5A 111.3(6) . . ? C4A C5A C6A 112.3(6) . . ? C5A C6A C1A 110.9(6) . . ? C2B C1B C6B 109.9(6) . . ? C2B C1B P1 112.3(5) . . ? C6B C1B P1 113.2(5) . . ? C1B C2B C3B 112.5(7) . . ? C4B C3B C2B 112.0(7) . . ? C5B C4B C3B 112.3(7) . . ? C4B C5B C6B 111.9(7) . . ? C5B C6B C1B 111.1(6) . . ? C6C C1C C2C 118.4(5) . . ? C6C C1C P2 122.1(5) . . ? C2C C1C P2 119.2(5) . . ? C1C C2C C3C 120.5(6) . . ? C4C C3C C2C 121.1(7) . . ? C3C C4C C5C 118.9(6) . . ? C4C C5C C6C 120.6(7) . . ? C1C C6C C5C 120.4(6) . . ? C2D C1D C6D 119.3(6) . . ? C2D C1D P2 120.2(5) . . ? C6D C1D P2 120.4(5) . . ? C1D C2D C3D 119.3(7) . . ? C4D C3D C2D 120.4(7) . . ? C5D C4D C3D 120.8(7) . . ? C4D C5D C6D 120.3(7) . . ? C5D C6D C1D 119.8(7) . . ? C6E C1E C2E 118.9(6) . . ? C6E C1E P2 124.3(5) . . ? C2E C1E P2 116.8(5) . . ? C3E C2E C1E 120.0(6) . . ? C2E C3E C4E 121.1(6) . . ? C3E C4E C5E 119.6(6) . . ? C4E C5E C6E 119.5(7) . . ? C1E C6E C5E 120.7(6) . . ? _refine_diff_density_max 0.700 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.084 data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C28 H52 N P2 S2 Tc' _chemical_formula_weight 626.77 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Tc' 'Tc' -1.4390 0.7593 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.528(9) _cell_length_b 11.731(9) _cell_length_c 24.25(1) _cell_angle_alpha 90.00 _cell_angle_beta 95.32(8) _cell_angle_gamma 90.00 _cell_volume 2982(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 7.6 _cell_measurement_theta_max 14.2 _exptl_crystal_description rhomboids _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method ? _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.563 _exptl_absorpt_correction_T_max 0.813 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nicolet R3m/V' _diffrn_measurement_method theta-2theta _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.1 _diffrn_reflns_number 2718 _diffrn_reflns_av_R_equivalents 0.0666 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 20.04 _reflns_number_total 1409 _reflns_number_observed 1100 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'P3/P4-PC Vers.4.27 (1991)' _computing_cell_refinement " " _computing_data_reduction 'SHELXTL/PC V.5.3 (Sheldrick, 1994)' _computing_structure_solution " " _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL/PC V.5.3 (Sheldrick, 1994)' _computing_publication_material " " _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+49.7908P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'heavy-atom methods' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1404 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1039 _refine_ls_R_factor_obs 0.0779 _refine_ls_wR_factor_all 0.2364 _refine_ls_wR_factor_obs 0.2038 _refine_ls_goodness_of_fit_all 1.102 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_restrained_S_all 1.140 _refine_ls_restrained_S_obs 1.137 _refine_ls_shift/esd_max -0.618 _refine_ls_shift/esd_mean 0.011 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Tc Tc 0.0000 0.1689(2) 0.2500 0.0344(9) Uani 0.67 d SP . Tc' Tc 0.0000 0.0317(4) 0.2500 0.0458(13) Uani 0.33 d SP . S1 S 0.1652(5) 0.0826(6) 0.2053(2) 0.050(2) Uiso 0.67 d P . S1' S 0.1689(8) 0.1300(10) 0.2046(4) 0.029(3) Uiso 0.33 d P . P1 P 0.1418(4) 0.1309(5) 0.3306(2) 0.0377(14) Uiso 0.67 d P . P1' P 0.1438(9) 0.0667(12) 0.3298(4) 0.045(3) Uiso 0.33 d P . N1' N 0.0000 -0.1072(48) 0.2500 0.091(17) Uiso 0.33 d SP . N1 N 0.0000 0.3091(24) 0.2500 0.092(9) Uiso 0.67 d SP . C1' C 0.3036(38) 0.0667(41) 0.3094(18) 0.052(12) Uiso 0.33 d P . C1 C 0.3034(20) 0.1227(20) 0.3068(9) 0.052(6) Uiso 0.67 d P . C2 C 0.3056(21) 0.0617(22) 0.2538(10) 0.073(6) Uiso 0.67 d P . C2' C 0.3120(29) 0.1377(29) 0.2564(14) 0.031(8) Uiso 0.33 d P . C3 C 0.1108(18) -0.0011(17) 0.3687(8) 0.044(5) Uiso 0.67 d P . C3' C 0.1536(48) -0.0415(44) 0.3842(22) 0.069(14) Uiso 0.33 d P . C4 C 0.1111(19) -0.1058(17) 0.3306(9) 0.057(5) Uiso 0.67 d P . C4' C 0.1770(52) -0.1603(47) 0.3569(24) 0.094(16) Uiso 0.33 d P . C5 C 0.0722(23) -0.2127(21) 0.3625(11) 0.082(7) Uiso 0.67 d P . C5' C 0.1767(55) -0.2485(52) 0.4022(27) 0.074(19) Uiso 0.33 d P . C6 C 0.1612(34) -0.2257(31) 0.4200(16) 0.094(12) Uiso 0.67 d P . C6' C 0.0724(42) -0.2573(37) 0.4340(19) 0.066(12) Uiso 0.33 d P . C7 C 0.1497(27) -0.1238(22) 0.4534(11) 0.091(8) Uiso 0.67 d P . C7' C 0.0521(43) -0.1276(36) 0.4572(18) 0.067(12) Uiso 0.33 d P . C8 C 0.1975(20) -0.0161(18) 0.4238(9) 0.063(6) Uiso 0.67 d P . C8' C 0.0342(42) -0.0389(39) 0.4110(19) 0.075(13) Uiso 0.33 d P . C9 C 0.1545(21) 0.2364(18) 0.3846(10) 0.048(6) Uiso 0.67 d P . C9' C 0.1129(45) 0.1999(44) 0.3660(22) 0.069(14) Uiso 0.33 d P . C10 C 0.0296(18) 0.2475(16) 0.4106(8) 0.056(5) Uiso 0.67 d P . C10' C 0.2121(35) 0.2095(31) 0.4181(16) 0.047(10) Uiso 0.33 d P . C11 C 0.0450(20) 0.3347(18) 0.4594(9) 0.069(6) Uiso 0.67 d P . C11' C 0.1724(65) 0.3197(57) 0.4567(30) 0.134(23) Uiso 0.33 d P . C12 C 0.0848(23) 0.4527(21) 0.4369(11) 0.084(7) Uiso 0.67 d P . C12' C 0.2302(47) 0.4261(39) 0.4167(19) 0.050(14) Uiso 0.33 d P . C13 C 0.1820(33) 0.4438(28) 0.4097(14) 0.093(12) Uiso 0.67 d P . C13' C 0.0841(45) 0.4026(41) 0.3582(21) 0.082(14) Uiso 0.33 d P . C14 C 0.1955(20) 0.3545(17) 0.3618(9) 0.062(6) Uiso 0.67 d P . C14' C 0.1129(39) 0.3114(36) 0.3294(18) 0.064(11) Uiso 0.33 d P . 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 Tc 0.0264(13) 0.0291(14) 0.048(2) 0.000 0.0053(9) 0.000 Tc' 0.037(3) 0.051(3) 0.048(3) 0.000 0.000(2) 0.000 _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 Tc Tc' 1.609(5) . ? Tc N1 1.64(3) . ? Tc S1' 2.223(9) 2 ? Tc S1' 2.223(9) . ? Tc S1 2.362(6) 2 ? Tc S1 2.362(6) . ? Tc P1 2.389(5) . ? Tc P1 2.389(5) 2 ? Tc P1' 2.633(11) . ? Tc P1' 2.633(11) 2 ? Tc' N1' 1.63(6) . ? Tc' S1 2.216(6) 2 ? Tc' S1 2.216(6) . ? Tc' P1' 2.380(10) . ? Tc' P1' 2.380(10) 2 ? Tc' S1' 2.463(10) 2 ? Tc' S1' 2.463(10) . ? Tc' P1 2.619(6) . ? Tc' P1 2.619(6) 2 ? S1 S1' 0.558(10) . ? S1 C2 1.82(2) . ? S1 C2' 2.00(3) . ? S1' C2' 1.87(3) . ? S1' C2 1.95(2) . ? P1 P1' 0.753(11) . ? P1 C9' 1.24(5) . ? P1 C9 1.80(2) . ? P1 C3 1.85(2) . ? P1 C1 1.85(2) . ? P1 C1' 1.97(4) . ? P1 C14' 2.14(4) . ? P1 C10' 2.37(4) . ? P1' C3 1.30(2) . ? P1' C1' 1.80(4) . ? P1' C3' 1.83(5) . ? P1' C9' 1.84(5) . ? P1' C1 1.93(2) . ? P1' C4 2.05(2) . ? C1' C1 0.66(4) . ? C1' C2 1.35(5) . ? C1' C2' 1.54(6) . ? C1 C2' 1.25(4) . ? C1 C2 1.47(3) . ? C2 C2' 0.90(3) . ? C3 C3' 0.73(5) . ? C3 C8' 1.43(5) . ? C3 C4 1.54(3) . ? C3 C8 1.56(3) . ? C3 C4' 2.02(6) . ? C3' C8 1.07(5) . ? C3' C8' 1.47(6) . ? C3' C4 1.53(5) . ? C3' C4' 1.57(7) . ? C3' C7 1.94(6) . ? C4 C4' 1.10(5) . ? C4 C5 1.55(3) . ? C4' C5 1.28(5) . ? C4' C5' 1.51(8) . ? C4' C6 1.73(7) . ? C5 C5' 1.45(6) . ? C5 C6 1.61(4) . ? C5 C6' 1.81(5) . ? C5' C6 0.55(7) . ? C5' C6' 1.40(8) . ? C5' C7 1.96(7) . ? C6 C6' 1.09(5) . ? C6 C7 1.46(4) . ? C6 C7' 1.91(6) . ? C6' C7' 1.64(6) . ? C6' C7 1.81(5) . ? C7 C7' 1.04(4) . ? C7 C8 1.56(3) . ? C7 C8' 1.82(5) . ? C7' C8' 1.53(6) . ? C8 C8' 1.74(5) . ? C9 C9' 0.74(5) . ? C9 C10' 1.02(4) . ? C9 C10 1.51(3) . ? C9 C14 1.57(3) . ? C9 C14' 1.63(5) . ? C9 C11' 2.00(7) . ? C9' C10 1.56(5) . ? C9' C10' 1.57(6) . ? C9' C14' 1.58(6) . ? C9' C14 2.02(5) . ? C10 C11 1.56(3) . ? C10 C10' 1.96(4) . ? C10 C11' 1.98(7) . ? C10' C11' 1.67(7) . ? C11 C11' 1.36(7) . ? C11 C12 1.56(3) . ? C11' C12' 1.73(8) . ? C11' C12 1.85(7) . ? C11' C13 1.86(7) . ? C12 C13 1.27(4) . ? C12 C12' 1.68(5) . ? C12 C13' 2.00(5) . ? C12' C13 0.56(5) . ? C12' C14 1.59(5) . ? C12' C13' 2.01(7) . ? C13 C14 1.58(4) . ? C13 C13' 1.62(6) . ? C13' C14 1.30(5) . ? C13' C14' 1.33(6) . ? C14 C14' 1.23(4) . ? 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 Tc' Tc N1 180.000(5) . . ? Tc' Tc S1' 78.2(3) . 2 ? N1 Tc S1' 101.8(3) . 2 ? Tc' Tc S1' 78.2(3) . . ? N1 Tc S1' 101.8(3) . . ? S1' Tc S1' 156.3(6) 2 . ? Tc' Tc S1 64.6(2) . 2 ? N1 Tc S1 115.4(2) . 2 ? S1' Tc S1 13.6(3) 2 2 ? S1' Tc S1 142.8(4) . 2 ? Tc' Tc S1 64.6(2) . . ? N1 Tc S1 115.4(2) . . ? S1' Tc S1 142.8(4) 2 . ? S1' Tc S1 13.6(3) . . ? S1 Tc S1 129.2(3) 2 . ? Tc' Tc P1 79.2(2) . . ? N1 Tc P1 100.8(2) . . ? S1' Tc P1 91.4(3) 2 . ? S1' Tc P1 84.2(3) . . ? S1 Tc P1 88.6(2) 2 . ? S1 Tc P1 82.2(2) . . ? Tc' Tc P1 79.2(2) . 2 ? N1 Tc P1 100.8(2) . 2 ? S1' Tc P1 84.2(3) 2 2 ? S1' Tc P1 91.4(3) . 2 ? S1 Tc P1 82.2(2) 2 2 ? S1 Tc P1 88.6(2) . 2 ? P1 Tc P1 158.5(3) . 2 ? Tc' Tc P1' 62.9(3) . . ? N1 Tc P1' 117.1(3) . . ? S1' Tc P1' 88.5(3) 2 . ? S1' Tc P1' 80.7(3) . . ? S1 Tc P1' 82.2(3) 2 . ? S1 Tc P1' 75.2(3) . . ? P1 Tc P1' 16.3(2) . . ? P1 Tc P1' 142.2(4) 2 . ? Tc' Tc P1' 62.9(3) . 2 ? N1 Tc P1' 117.1(3) . 2 ? S1' Tc P1' 80.7(3) 2 2 ? S1' Tc P1' 88.5(3) . 2 ? S1 Tc P1' 75.2(3) 2 2 ? S1 Tc P1' 82.2(3) . 2 ? P1 Tc P1' 142.2(4) . 2 ? P1 Tc P1' 16.3(2) 2 2 ? P1' Tc P1' 125.9(6) . 2 ? Tc Tc' N1' 180.000(8) . . ? Tc Tc' S1 74.4(2) . 2 ? N1' Tc' S1 105.6(2) . 2 ? Tc Tc' S1 74.4(2) . . ? N1' Tc' S1 105.6(2) . . ? S1 Tc' S1 148.7(4) 2 . ? Tc Tc' P1' 80.1(3) . . ? N1' Tc' P1' 99.9(3) . . ? S1 Tc' P1' 91.4(3) 2 . ? S1 Tc' P1' 83.3(3) . . ? Tc Tc' P1' 80.1(3) . 2 ? N1' Tc' P1' 99.9(3) . 2 ? S1 Tc' P1' 83.3(3) 2 2 ? S1 Tc' P1' 91.4(3) . 2 ? P1' Tc' P1' 160.1(7) . 2 ? Tc Tc' S1' 62.1(3) . 2 ? N1' Tc' S1' 117.9(3) . 2 ? S1 Tc' S1' 12.3(2) 2 2 ? S1 Tc' S1' 136.4(4) . 2 ? P1' Tc' S1' 89.2(3) . 2 ? P1' Tc' S1' 81.5(3) 2 2 ? Tc Tc' S1' 62.1(3) . . ? N1' Tc' S1' 117.9(3) . . ? S1 Tc' S1' 136.4(4) 2 . ? S1 Tc' S1' 12.3(2) . . ? P1' Tc' S1' 81.5(3) . . ? P1' Tc' S1' 89.2(3) 2 . ? S1' Tc' S1' 124.1(5) 2 . ? Tc Tc' P1 63.6(2) . . ? N1' Tc' P1 116.4(2) . . ? S1 Tc' P1 86.2(2) 2 . ? S1 Tc' P1 80.0(2) . . ? P1' Tc' P1 16.4(3) . . ? P1' Tc' P1 143.7(5) 2 . ? S1' Tc' P1 81.0(3) 2 . ? S1' Tc' P1 74.9(3) . . ? Tc Tc' P1 63.6(2) . 2 ? N1' Tc' P1 116.4(2) . 2 ? S1 Tc' P1 80.0(2) 2 2 ? S1 Tc' P1 86.2(2) . 2 ? P1' Tc' P1 143.7(5) . 2 ? P1' Tc' P1 16.4(3) 2 2 ? S1' Tc' P1 74.9(3) 2 2 ? S1' Tc' P1 81.0(3) . 2 ? P1 Tc' P1 127.2(3) . 2 ? S1' S1 C2 95.6(15) . . ? S1' S1 C2' 69.1(16) . . ? C2 S1 C2' 26.6(10) . . ? S1' S1 Tc' 110.0(13) . . ? C2 S1 Tc' 106.0(8) . . ? C2' S1 Tc' 112.4(10) . . ? S1' S1 Tc 69.0(12) . . ? C2 S1 Tc 110.5(8) . . ? C2' S1 Tc 97.8(10) . . ? Tc' S1 Tc 41.0(2) . . ? S1 S1' C2' 94.8(17) . . ? S1 S1' C2 67.9(14) . . ? C2' S1' C2 27.0(10) . . ? S1 S1' Tc 97.5(13) . . ? C2' S1' Tc 106.8(11) . . ? C2 S1' Tc 111.1(8) . . ? S1 S1' Tc' 57.7(11) . . ? C2' S1' Tc' 107.0(11) . . ? C2 S1' Tc' 93.3(8) . . ? Tc S1' Tc' 39.8(2) . . ? P1' P1 C9' 132.8(25) . . ? P1' P1 C9 134.8(12) . . ? C9' P1 C9 18.5(23) . . ? P1' P1 C3 35.0(11) . . ? C9' P1 C3 97.8(23) . . ? C9 P1 C3 102.6(9) . . ? P1' P1 C1 85.0(12) . . ? C9' P1 C1 122.9(25) . . ? C9 P1 C1 104.7(10) . . ? C3 P1 C1 108.8(10) . . ? P1' P1 C1' 65.5(16) . . ? C9' P1 C1' 134.7(27) . . ? C9 P1 C1' 116.4(15) . . ? C3 P1 C1' 90.4(15) . . ? C1 P1 C1' 19.5(13) . . ? P1' P1 C14' 173.3(15) . . ? C9' P1 C14' 47.0(25) . . ? C9 P1 C14' 47.9(14) . . ? C3 P1 C14' 143.6(13) . . ? C1 P1 C14' 100.4(14) . . ? C1' P1 C14' 119.9(18) . . ? P1' P1 C10' 113.8(13) . . ? C9' P1 C10' 36.9(24) . . ? C9 P1 C10' 23.5(9) . . ? C3 P1 C10' 86.2(11) . . ? C1 P1 C10' 94.6(11) . . ? C1' P1 C10' 100.2(16) . . ? C14' P1 C10' 70.1(15) . . ? P1' P1 Tc 100.6(10) . . ? C9' P1 Tc 105.7(23) . . ? C9 P1 Tc 117.8(8) . . ? C3 P1 Tc 116.1(7) . . ? C1 P1 Tc 106.1(7) . . ? C1' P1 Tc 110.3(13) . . ? C14' P1 Tc 74.2(12) . . ? C10' P1 Tc 141.3(10) . . ? P1' P1 Tc' 63.5(9) . . ? C9' P1 Tc' 130.4(23) . . ? C9 P1 Tc' 148.0(8) . . ? C3 P1 Tc' 83.4(6) . . ? C1 P1 Tc' 102.8(7) . . ? C1' P1 Tc' 94.7(13) . . ? C14' P1 Tc' 111.1(12) . . ? C10' P1 Tc' 161.9(9) . . ? Tc P1 Tc' 37.13(13) . . ? P1 P1' C3 125.6(16) . . ? P1 P1' C1' 92.0(19) . . ? C3 P1' C1' 121.2(19) . . ? P1 P1' C3' 132.7(20) . . ? C3 P1' C3' 19.2(17) . . ? C1' P1' C3' 102.0(22) . . ? P1 P1' C9' 29.7(17) . . ? C3 P1' C9' 96.0(18) . . ? C1' P1' C9' 110.1(23) . . ? C3' P1' C9' 104.4(22) . . ? P1 P1' C1 72.2(11) . . ? C3 P1' C1 135.4(13) . . ? C1' P1' C1 19.9(14) . . ? C3' P1' C1 116.9(18) . . ? C9' P1' C1 92.6(18) . . ? P1 P1' C4 168.4(13) . . ? C3 P1' C4 48.4(11) . . ? C1' P1' C4 99.4(18) . . ? C3' P1' C4 46.1(17) . . ? C9' P1' C4 142.9(17) . . ? C1 P1' C4 119.2(10) . . ? P1 P1' Tc' 100.1(10) . . ? C3 P1' Tc' 106.9(11) . . ? C1' P1' Tc' 108.4(15) . . ? C3' P1' Tc' 117.1(17) . . ? C9' P1' Tc' 114.1(17) . . ? C1 P1' Tc' 109.1(8) . . ? C4 P1' Tc' 75.1(7) . . ? P1 P1' Tc 63.1(9) . . ? C3 P1' Tc 129.5(11) . . ? C1' P1' Tc 106.6(15) . . ? C3' P1' Tc 146.9(17) . . ? C9' P1' Tc 81.3(16) . . ? C1 P1' Tc 95.1(8) . . ? C4 P1' Tc 111.7(7) . . ? Tc' P1' Tc 37.0(2) . . ? C1 C1' C2 87.1(55) . . ? C1 C1' C2' 52.0(45) . . ? C2 C1' C2' 35.3(17) . . ? C1 C1' P1' 91.7(50) . . ? C2 C1' P1' 112.1(27) . . ? C2' C1' P1' 111.0(27) . . ? C1 C1' P1 69.4(45) . . ? C2 C1' P1 111.7(27) . . ? C2' C1' P1 97.4(25) . . ? P1' C1' P1 22.4(6) . . ? C1' C1 C2' 103.4(55) . . ? C1' C1 C2 66.3(49) . . ? C2' C1 C2 37.3(16) . . ? C1' C1 P1 91.1(48) . . ? C2' C1 P1 116.8(20) . . ? C2 C1 P1 112.8(15) . . ? C1' C1 P1' 68.4(46) . . ? C2' C1 P1' 118.4(20) . . ? C2 C1 P1' 99.9(15) . . ? P1 C1 P1' 22.8(4) . . ? C2' C2 C1' 83.9(34) . . ? C2' C2 C1 57.5(27) . . ? C1' C2 C1 26.5(19) . . ? C2' C2 S1 87.9(28) . . ? C1' C2 S1 123.6(23) . . ? C1 C2 S1 114.9(16) . . ? C2' C2 S1' 71.4(27) . . ? C1' C2 S1' 120.8(23) . . ? C1 C2 S1' 105.2(16) . . ? S1 C2 S1' 16.5(4) . . ? C2 C2' C1 85.3(33) . . ? C2 C2' C1' 60.8(29) . . ? C1 C2' C1' 24.6(19) . . ? C2 C2' S1' 81.6(28) . . ? C1 C2' S1' 121.6(23) . . ? C1' C2' S1' 115.4(24) . . ? C2 C2' S1 65.5(26) . . ? C1 C2' S1 116.1(23) . . ? C1' C2' S1 104.0(23) . . ? S1' C2' S1 16.2(4) . . ? C3' C3 P1' 125.0(48) . . ? C3' C3 C8' 78.0(47) . . ? P1' C3 C8' 155.6(26) . . ? C3' C3 C4 75.8(47) . . ? P1' C3 C4 92.2(15) . . ? C8' C3 C4 102.5(23) . . ? C3' C3 C8 37.3(44) . . ? P1' C3 C8 121.0(16) . . ? C8' C3 C8 71.0(22) . . ? C4 C3 C8 113.1(18) . . ? C3' C3 P1 132.1(47) . . ? P1' C3 P1 19.4(6) . . ? C8' C3 P1 139.0(23) . . ? C4 C3 P1 111.1(14) . . ? C8 C3 P1 114.0(13) . . ? C3' C3 C4' 43.3(47) . . ? P1' C3 C4' 110.1(21) . . ? C8' C3 C4' 92.3(26) . . ? C4 C3 C4' 32.6(17) . . ? C8 C3 C4' 80.5(21) . . ? P1 C3 C4' 128.6(19) . . ? C3 C3' C8 118.3(65) . . ? C3 C3' C8' 72.8(47) . . ? C8 C3' C8' 85.0(39) . . ? C3 C3' C4 76.5(49) . . ? C8 C3' C4 165.2(53) . . ? C8' C3' C4 101.1(35) . . ? C3 C3' C4' 118.1(63) . . ? C8 C3' C4' 123.6(52) . . ? C8' C3' C4' 112.3(40) . . ? C4 C3' C4' 41.6(24) . . ? C3 C3' P1' 35.8(35) . . ? C8 C3' P1' 116.4(39) . . ? C8' C3' P1' 108.2(37) . . ? C4 C3' P1' 74.8(25) . . ? C4' C3' P1' 108.3(36) . . ? C3 C3' C7 134.8(56) . . ? C8 C3' C7 53.4(28) . . ? C8' C3' C7 62.5(27) . . ? C4 C3' C7 117.5(31) . . ? C4' C3' C7 86.5(33) . . ? P1' C3' C7 165.0(32) . . ? C4' C4 C3' 71.2(37) . . ? C4' C4 C3 98.8(34) . . ? C3' C4 C3 27.6(19) . . ? C4' C4 C5 54.7(30) . . ? C3' C4 C5 92.6(24) . . ? C3 C4 C5 109.4(17) . . ? C4' C4 P1' 118.7(34) . . ? C3' C4 P1' 59.1(21) . . ? C3 C4 P1' 39.4(9) . . ? C5 C4 P1' 148.8(16) . . ? C4 C4' C5 80.7(39) . . ? C4 C4' C5' 140.8(53) . . ? C5 C4' C5' 62.2(34) . . ? C4 C4' C3' 67.3(37) . . ? C5 C4' C3' 102.1(40) . . ? C5' C4' C3' 106.9(46) . . ? C4 C4' C6 131.3(46) . . ? C5 C4' C6 62.6(29) . . ? C5' C4' C6 17.7(27) . . ? C3' C4' C6 89.4(35) . . ? C4 C4' C3 48.6(25) . . ? C5 C4' C3 96.7(33) . . ? C5' C4' C3 120.4(41) . . ? C3' C4' C3 18.6(22) . . ? C6 C4' C3 102.8(30) . . ? C4' C5 C5' 66.6(35) . . ? C4' C5 C4 44.6(26) . . ? C5' C5 C4 110.2(29) . . ? C4' C5 C6 72.6(31) . . ? C5' C5 C6 19.6(27) . . ? C4 C5 C6 110.4(22) . . ? C4' C5 C6' 108.4(34) . . ? C5' C5 C6' 49.4(30) . . ? C4 C5 C6' 137.4(23) . . ? C6 C5 C6' 36.5(16) . . ? C6 C5' C6' 45.1(78) . . ? C6 C5' C5 96.8(94) . . ? C6' C5' C5 78.6(35) . . ? C6 C5' C4' 105.0(100) . . ? C6' C5' C4' 120.3(48) . . ? C5 C5' C4' 51.2(29) . . ? C6 C5' C7 19.8(78) . . ? C6' C5' C7 62.5(32) . . ? C5 C5' C7 93.3(33) . . ? C4' C5' C7 87.7(36) . . ? C5' C6 C6' 114.1(100) . . ? C5' C6 C7 152.9(100) . . ? C6' C6 C7 89.3(38) . . ? C5' C6 C5 63.6(85) . . ? C6' C6 C5 81.7(34) . . ? C7 C6 C5 109.4(26) . . ? C5' C6 C4' 57.3(88) . . ? C6' C6 C4' 125.6(42) . . ? C7 C6 C4' 98.5(31) . . ? C5 C6 C4' 44.9(21) . . ? C5' C6 C7' 155.0(99) . . ? C6' C6 C7' 59.1(33) . . ? C7 C6 C7' 32.6(17) . . ? C5 C6 C7' 91.4(24) . . ? C4' C6 C7' 105.2(30) . . ? C6 C6' C5' 20.8(36) . . ? C6 C6' C7' 86.2(38) . . ? C5' C6' C7' 104.6(43) . . ? C6 C6' C7 53.6(29) . . ? C5' C6' C7 73.9(37) . . ? C7' C6' C7 34.7(18) . . ? C6 C6' C5 61.8(31) . . ? C5' C6' C5 52.0(28) . . ? C7' C6' C5 94.1(27) . . ? C7 C6' C5 87.6(23) . . ? C7' C7 C6 98.5(36) . . ? C7' C7 C8 116.0(34) . . ? C6 C7 C8 111.2(25) . . ? C7' C7 C6' 64.0(31) . . ? C6 C7 C6' 37.1(19) . . ? C8 C7 C6' 137.7(24) . . ? C7' C7 C8' 57.2(31) . . ? C6 C7 C8' 102.8(25) . . ? C8 C7 C8' 61.5(18) . . ? C6' C7 C8' 93.8(24) . . ? C7' C7 C3' 101.4(36) . . ? C6 C7 C3' 85.2(25) . . ? C8 C7 C3' 33.4(15) . . ? C6' C7 C3' 104.5(25) . . ? C8' C7 C3' 45.9(21) . . ? C7' C7 C5' 103.1(37) . . ? C6 C7 C5' 7.3(29) . . ? C8 C7 C5' 104.0(24) . . ? C6' C7 C5' 43.6(25) . . ? C8' C7 C5' 100.4(26) . . ? C3' C7 C5' 78.9(25) . . ? C7 C7' C8' 87.9(38) . . ? C7 C7' C6' 81.3(35) . . ? C8' C7' C6' 113.1(36) . . ? C7 C7' C6 48.9(27) . . ? C8' C7' C6 95.9(31) . . ? C6' C7' C6 34.7(18) . . ? C3' C8 C3 24.5(29) . . ? C3' C8 C7 93.2(33) . . ? C3 C8 C7 107.3(18) . . ? C3' C8 C8' 57.2(32) . . ? C3 C8 C8' 51.2(18) . . ? C7 C8 C8' 66.5(20) . . ? C3 C8' C3' 29.2(22) . . ? C3 C8' C7' 134.1(38) . . ? C3' C8' C7' 105.0(39) . . ? C3 C8' C8 57.8(20) . . ? C3' C8' C8 37.8(22) . . ? C7' C8' C8 85.5(29) . . ? C3 C8' C7 100.6(28) . . ? C3' C8' C7 71.6(30) . . ? C7' C8' C7 34.9(19) . . ? C8 C8' C7 52.0(17) . . ? C9' C9 C10' 125.8(55) . . ? C9' C9 C10 79.3(46) . . ? C10' C9 C10 99.9(28) . . ? C9' C9 C14 117.7(50) . . ? C10' C9 C14 113.1(30) . . ? C10 C9 C14 110.4(16) . . ? C9' C9 C14' 73.2(48) . . ? C10' C9 C14' 156.8(34) . . ? C10 C9 C14' 96.7(20) . . ? C14 C9 C14' 45.1(16) . . ? C9' C9 P1 32.1(42) . . ? C10' C9 P1 111.5(26) . . ? C10 C9 P1 110.6(16) . . ? C14 C9 P1 110.8(15) . . ? C14' C9 P1 77.1(19) . . ? C9' C9 C11' 145.5(52) . . ? C10' C9 C11' 56.8(31) . . ? C10 C9 C11' 67.0(22) . . ? C14 C9 C11' 82.5(23) . . ? C14' C9 C11' 116.9(27) . . ? P1 C9 C11' 165.8(23) . . ? C9 C9' P1 129.4(59) . . ? C9 C9' C10 73.0(47) . . ? P1 C9' C10 155.0(43) . . ? C9 C9' C10' 31.7(35) . . ? P1 C9' C10' 114.7(34) . . ? C10 C9' C10' 77.9(29) . . ? C9 C9' C14' 80.4(51) . . ? P1 C9' C14' 98.0(35) . . ? C10 C9' C14' 97.0(32) . . ? C10' C9' C14' 111.0(41) . . ? C9 C9' P1' 131.8(54) . . ? P1 C9' P1' 17.5(11) . . ? C10 C9' P1' 140.6(33) . . ? C10' C9' P1' 108.2(29) . . ? C14' C9' P1' 115.3(35) . . ? C9 C9' C14 43.4(39) . . ? P1 C9' C14 114.7(31) . . ? C10 C9' C14 89.2(27) . . ? C10' C9' C14 73.6(28) . . ? C14' C9' C14 37.4(20) . . ? P1' C9' C14 130.2(27) . . ? C9 C10 C9' 27.7(18) . . ? C9 C10 C11 109.8(17) . . ? C9' C10 C11 137.4(25) . . ? C9 C10 C10' 30.7(12) . . ? C9' C10 C10' 51.3(23) . . ? C11 C10 C10' 92.7(16) . . ? C9 C10 C11' 68.2(23) . . ? C9' C10 C11' 95.7(29) . . ? C11 C10 C11' 43.2(21) . . ? C10' C10 C11' 50.2(22) . . ? C9 C10' C9' 22.4(24) . . ? C9 C10' C11' 92.6(38) . . ? C9' C10' C11' 108.9(39) . . ? C9 C10' C10 49.5(21) . . ? C9' C10' C10 50.8(22) . . ? C11' C10' C10 65.4(27) . . ? C9 C10' P1 45.0(20) . . ? C9' C10' P1 28.4(19) . . ? C11' C10' P1 136.8(33) . . ? C10 C10' P1 77.5(14) . . ? C11' C11 C12 78.4(32) . . ? C11' C11 C10 84.9(33) . . ? C12 C11 C10 109.1(18) . . ? C11 C11' C10' 115.2(48) . . ? C11 C11' C12' 109.6(47) . . ? C10' C11' C12' 97.2(41) . . ? C11 C11' C12 55.6(27) . . ? C10' C11' C12 130.5(45) . . ? C12' C11' C12 55.8(27) . . ? C11 C11' C13 92.3(40) . . ? C10' C11' C13 103.4(41) . . ? C12' C11' C13 17.5(19) . . ? C12 C11' C13 40.1(18) . . ? C11 C11' C10 51.9(26) . . ? C10' C11' C10 64.4(27) . . ? C12' C11' C10 106.3(39) . . ? C12 C11' C10 83.1(29) . . ? C13 C11' C10 94.0(33) . . ? C11 C11' C9 95.3(40) . . ? C10' C11' C9 30.6(18) . . ? C12' C11' C9 82.6(33) . . ? C12 C11' C9 100.4(34) . . ? C13 C11' C9 81.5(30) . . ? C10 C11' C9 44.8(18) . . ? C13 C12 C11 111.3(24) . . ? C13 C12 C12' 15.1(24) . . ? C11 C12 C12' 102.7(22) . . ? C13 C12 C11' 70.1(28) . . ? C11 C12 C11' 46.0(22) . . ? C12' C12 C11' 58.3(26) . . ? C13 C12 C13' 54.0(22) . . ? C11 C12 C13' 95.5(20) . . ? C12' C12 C13' 65.7(23) . . ? C11' C12 C13' 87.6(28) . . ? C13 C12' C14 79.0(71) . . ? C13 C12' C12 36.4(61) . . ? C14 C12' C12 101.4(29) . . ? C13 C12' C11' 94.7(76) . . ? C14 C12' C11' 91.3(33) . . ? C12 C12' C11' 65.9(30) . . ? C13 C12' C13' 39.2(64) . . ? C14 C12' C13' 40.1(19) . . ? C12 C12' C13' 64.8(23) . . ? C11' C12' C13' 90.6(33) . . ? C12' C13 C12 128.5(81) . . ? C12' C13 C14 80.6(71) . . ? C12 C13 C14 124.6(28) . . ? C12' C13 C13' 128.2(79) . . ? C12 C13 C13' 86.6(28) . . ? C14 C13 C13' 47.8(20) . . ? C12' C13 C11' 67.8(70) . . ? C12 C13 C11' 69.8(28) . . ? C14 C13 C11' 86.9(28) . . ? C13' C13 C11' 100.0(32) . . ? C14 C13' C14' 55.7(27) . . ? C14 C13' C13 64.5(25) . . ? C14' C13' C13 119.1(39) . . ? C14 C13' C12 98.0(30) . . ? C14' C13' C12 139.4(38) . . ? C13 C13' C12 39.5(17) . . ? C14 C13' C12' 52.0(23) . . ? C14' C13' C12' 106.5(35) . . ? C13 C13' C12' 12.6(20) . . ? C12 C13' C12' 49.5(20) . . ? C14' C14 C13' 63.4(29) . . ? C14' C14 C9 70.1(24) . . ? C13' C14 C9 97.6(26) . . ? C14' C14 C13 129.6(28) . . ? C13' C14 C13 67.7(26) . . ? C9 C14 C13 106.3(19) . . ? C14' C14 C12' 148.2(32) . . ? C13' C14 C12' 87.9(30) . . ? C9 C14 C12' 102.8(22) . . ? C13 C14 C12' 20.3(19) . . ? C14' C14 C9' 51.6(26) . . ? C13' C14 C9' 90.2(27) . . ? C9 C14 C9' 18.9(16) . . ? C13 C14 C9' 119.4(23) . . ? C12' C14 C9' 120.0(25) . . ? C14 C14' C13' 60.9(29) . . ? C14 C14' C9' 91.0(34) . . ? C13' C14' C9' 111.1(41) . . ? C14 C14' C9 64.8(24) . . ? C13' C14' C9 93.4(34) . . ? C9' C14' C9 26.5(19) . . ? C14 C14' P1 107.9(27) . . ? C13' C14' P1 146.1(36) . . ? C9' C14' P1 35.0(21) . . ? C9 C14' P1 55.0(15) . . ? _refine_diff_density_max 0.584 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.120