#Supplementary Material (ESI) for Journal of Materials Chemistry #This journal is (c) The Royal Society of Chemistry 2010 data_sken19 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 N4 O4 S' _chemical_formula_sum 'C22 H24 N4 O4 S' _chemical_formula_weight 440.51 _chemical_compound_source 'Synthesized by the authors. See text' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_hall '-P 2ybc' 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 13.7006(3) _cell_length_b 16.7642(4) _cell_length_c 20.2638(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.8690(10) _cell_angle_gamma 90.00 _cell_volume 4554.68(19) _cell_formula_units_Z 8 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 21925 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 71.99 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.558 _exptl_absorpt_correction_Type multi-scan _exptl_absorpt_correction_T_min 0.6950 _exptl_absorpt_correction_T_max 0.7550 _exptl_absorpt_process_details 'Sadabs (Sheldrick,1996)' _exptl_special_details ; X-ray crystallographic data for I were collected from a single crystal sample, which was mounted on a loop fiber. Data were collected using a Bruker Platform diffractometer, equipped with a Bruker SMART 2K Charged-Coupled Device (CCD) Area Detector using the program SMART and normal focus sealed tube source graphite monochromated Cu-K\a radiation. The crystal-to-detector distance was 4.908 cm, and the data collection was carried out in 512 x 512 pixel mode, utilizing 4 x 4 pixel binning. The initial unit cell parameters were determined by a least-squares fit of the angular setting of strong reflections, collected by a 9.0 degree scan in 30 frames over four different parts of the reciprocal space (120 frames total). One complete sphere of data was collected, to better than 0.8\%A resolution. Upon completion of the data collection, the first 101 frames were recollected in order to improve the decay correction analysis. ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'X-ray Sealed Tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Bruker Smart 2000' _diffrn_measurement_method '\w' _diffrn_detector_area_resol_mean 5.5 _diffrn_standards_number 258 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -0.27 _diffrn_reflns_number 49416 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 71.98 _reflns_number_total 8910 _reflns_number_gt 7601 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'UdMX (local program)' _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^)+(0.0878P)^2^+0.9192P] 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 8910 _refine_ls_number_parameters 567 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 S1 S -0.06310(3) 0.90727(3) 0.02534(2) 0.03755(12) Uani 1 1 d . . . O11 O 0.28413(10) 0.92203(10) 0.04527(7) 0.0566(4) Uani 1 1 d . . . O12 O 0.27363(10) 0.89768(11) 0.15184(7) 0.0617(4) Uani 1 1 d . . . O13 O 0.18234(13) 1.05498(11) 0.18052(8) 0.0703(5) Uani 1 1 d . . . O14 O 0.10316(12) 0.97809(10) 0.24086(7) 0.0618(4) Uani 1 1 d . . . N11 N 0.12950(14) 0.75170(10) -0.14665(8) 0.0514(4) Uani 1 1 d . . . N12 N 0.08957(11) 0.84902(8) -0.03101(7) 0.0388(3) Uani 1 1 d . . . N13 N -0.09449(10) 0.98418(9) 0.14001(7) 0.0374(3) Uani 1 1 d . . . N14 N -0.25275(12) 1.03715(11) 0.21061(8) 0.0480(4) Uani 1 1 d . . . C11 C 0.1127(2) 0.71055(16) -0.20579(12) 0.0700(7) Uani 1 1 d . . . H11 H 0.1608 0.6808 -0.2222 0.084 Uiso 1 1 calc R . . C12 C 0.0154(2) 0.71899(17) -0.23766(12) 0.0737(7) Uani 1 1 d . . . H12 H -0.0151 0.6961 -0.2791 0.088 Uiso 1 1 calc R . . C13 C -0.03018(18) 0.76758(14) -0.19746(10) 0.0586(5) Uani 1 1 d . . . H13 H -0.0972 0.7840 -0.2069 0.070 Uiso 1 1 calc R . . C14 C 0.04147(15) 0.78762(11) -0.14051(9) 0.0435(4) Uani 1 1 d . . . C15 C 0.02436(14) 0.83378(10) -0.08506(9) 0.0408(4) Uani 1 1 d . . . H15 H -0.0399 0.8550 -0.0881 0.049 Uiso 1 1 calc R . . C16 C 0.06132(12) 0.89123(10) 0.02037(8) 0.0352(3) Uani 1 1 d . . . C17 C 0.12502(12) 0.92077(10) 0.07658(8) 0.0342(3) Uani 1 1 d . . . C18 C 0.07430(12) 0.95548(9) 0.12446(8) 0.0336(3) Uani 1 1 d . . . C19 C -0.02754(12) 0.95379(10) 0.10441(8) 0.0343(3) Uani 1 1 d . . . C110 C -0.18283(13) 1.00501(10) 0.10913(8) 0.0375(4) Uani 1 1 d . . . H110 H -0.1976 1.0024 0.0618 0.045 Uiso 1 1 calc R . . C111 C -0.25949(13) 1.03161(10) 0.14182(9) 0.0392(4) Uani 1 1 d . . . C112 C -0.35569(15) 1.05309(13) 0.11120(10) 0.0505(5) Uani 1 1 d . . . H112 H -0.3816 1.0548 0.0645 0.061 Uiso 1 1 calc R . . C113 C -0.40739(16) 1.07165(16) 0.16135(12) 0.0627(6) Uani 1 1 d . . . H113 H -0.4743 1.0881 0.1551 0.075 Uiso 1 1 calc R . . C114 C -0.34211(16) 1.06139(17) 0.22186(11) 0.0640(6) Uani 1 1 d . . . H114 H -0.3571 1.0699 0.2645 0.077 Uiso 1 1 calc R . . C115 C 0.22462(18) 0.75311(16) -0.09876(13) 0.0668(6) Uani 1 1 d . . . H11A H 0.2367 0.8063 -0.0800 0.100 Uiso 1 1 calc R . . H11B H 0.2777 0.7386 -0.1216 0.100 Uiso 1 1 calc R . . H11C H 0.2228 0.7154 -0.0627 0.100 Uiso 1 1 calc R . . C116 C 0.23524(13) 0.91425(11) 0.08728(9) 0.0398(4) Uani 1 1 d . . . C117 C 0.38161(17) 0.8961(2) 0.17142(13) 0.0915(11) Uani 1 1 d . . . H11D H 0.4101 0.9435 0.1543 0.110 Uiso 1 1 calc R . . H11E H 0.4080 0.8486 0.1529 0.110 Uiso 1 1 calc R . . C118 C 0.4072(3) 0.8946(6) 0.24464(18) 0.296(6) Uani 1 1 d . . . H11F H 0.3758 0.9394 0.2624 0.443 Uiso 1 1 calc R . . H11G H 0.4790 0.8983 0.2596 0.443 Uiso 1 1 calc R . . H11H H 0.3837 0.8452 0.2608 0.443 Uiso 1 1 calc R . . C119 C 0.12673(12) 1.00118(10) 0.18435(8) 0.0367(3) Uani 1 1 d . . . C120 C 0.1507(2) 1.0228(2) 0.30081(11) 0.0857(9) Uani 1 1 d . . . H12A H 0.2194 1.0040 0.3159 0.103 Uiso 1 1 calc R . . H12B H 0.1532 1.0794 0.2892 0.103 Uiso 1 1 calc R . . C121 C 0.1014(2) 1.0147(4) 0.35176(19) 0.162(3) Uani 1 1 d . . . H12C H 0.0332 1.0330 0.3370 0.243 Uiso 1 1 calc R . . H12D H 0.1342 1.0462 0.3901 0.243 Uiso 1 1 calc R . . H12E H 0.1013 0.9590 0.3648 0.243 Uiso 1 1 calc R . . C122 C -0.16419(17) 1.02570(18) 0.26334(10) 0.0676(7) Uani 1 1 d . . . H12F H -0.1163 1.0676 0.2605 0.101 Uiso 1 1 calc R . . H12G H -0.1347 0.9742 0.2575 0.101 Uiso 1 1 calc R . . H12H H -0.1825 1.0277 0.3071 0.101 Uiso 1 1 calc R . . S2 S 0.57851(3) 0.46638(3) 0.08297(2) 0.04066(13) Uani 1 1 d . . . O21 O 0.60445(13) 0.34702(14) -0.12440(9) 0.0804(6) Uani 1 1 d . . . O22 O 0.76216(11) 0.35915(9) -0.06939(8) 0.0574(4) Uani 1 1 d . . . O23 O 0.71847(14) 0.53462(11) -0.11182(8) 0.0721(5) Uani 1 1 d . . . O24 O 0.80174(13) 0.59774(11) -0.02030(9) 0.0735(5) Uani 1 1 d . . . N21 N 0.43046(11) 0.16729(9) 0.01559(7) 0.0420(3) Uani 1 1 d . . . N22 N 0.54112(11) 0.32186(9) 0.01632(7) 0.0409(3) Uani 1 1 d . . . N23 N 0.67782(11) 0.60796(9) 0.07661(8) 0.0423(3) Uani 1 1 d . . . N24 N 0.73516(13) 0.76073(10) 0.14614(9) 0.0512(4) Uani 1 1 d . . . C21 C 0.36949(15) 0.11032(13) 0.03253(11) 0.0515(5) Uani 1 1 d . . . H21 H 0.3586 0.0597 0.0124 0.062 Uiso 1 1 calc R . . C22 C 0.32624(15) 0.13779(13) 0.08342(11) 0.0539(5) Uani 1 1 d . . . H22 H 0.2813 0.1100 0.1043 0.065 Uiso 1 1 calc R . . C23 C 0.36165(14) 0.21466(13) 0.09807(10) 0.0483(4) Uani 1 1 d . . . H23 H 0.3446 0.2486 0.1309 0.058 Uiso 1 1 calc R . . C24 C 0.42682(13) 0.23275(11) 0.05567(9) 0.0402(4) Uani 1 1 d . . . C25 C 0.47928(13) 0.30614(11) 0.05458(9) 0.0417(4) Uani 1 1 d . . . H25 H 0.4677 0.3464 0.0843 0.050 Uiso 1 1 calc R . . C26 C 0.58513(13) 0.39609(11) 0.02010(9) 0.0394(4) Uani 1 1 d . . . C27 C 0.64230(13) 0.42408(11) -0.02297(9) 0.0414(4) Uani 1 1 d . . . C28 C 0.68116(13) 0.50219(12) -0.00658(9) 0.0414(4) Uani 1 1 d . . . C29 C 0.65301(13) 0.53395(11) 0.04930(9) 0.0393(4) Uani 1 1 d . . . C210 C 0.63677(14) 0.63485(11) 0.12353(9) 0.0440(4) Uani 1 1 d . . . H210 H 0.5863 0.6040 0.1361 0.053 Uiso 1 1 calc R . . C211 C 0.66273(14) 0.70875(11) 0.15810(10) 0.0461(4) Uani 1 1 d . . . C212 C 0.62205(18) 0.74055(14) 0.20904(11) 0.0595(5) Uani 1 1 d . . . H212 H 0.5711 0.7176 0.2276 0.071 Uiso 1 1 calc R . . C213 C 0.6701(2) 0.81299(14) 0.22826(12) 0.0665(6) Uani 1 1 d . . . H213 H 0.6575 0.8478 0.2619 0.080 Uiso 1 1 calc R . . C214 C 0.73870(19) 0.82358(13) 0.18895(12) 0.0631(6) Uani 1 1 d . . . H214 H 0.7818 0.8676 0.1911 0.076 Uiso 1 1 calc R . . C215 C 0.48692(16) 0.15832(13) -0.03768(10) 0.0511(5) Uani 1 1 d . . . H21A H 0.4726 0.1067 -0.0591 0.077 Uiso 1 1 calc R . . H21B H 0.5577 0.1622 -0.0184 0.077 Uiso 1 1 calc R . . H21C H 0.4680 0.2001 -0.0710 0.077 Uiso 1 1 calc R . . C216 C 0.66443(14) 0.37340(12) -0.07853(10) 0.0477(4) Uani 1 1 d . . . C217 C 0.7941(2) 0.30609(16) -0.11715(14) 0.0714(7) Uani 1 1 d . . . H21D H 0.7705 0.3257 -0.1632 0.086 Uiso 1 1 calc R . . H21E H 0.7668 0.2526 -0.1138 0.086 Uiso 1 1 calc R . . C218 C 0.9052(2) 0.3034(2) -0.10080(16) 0.0868(9) Uani 1 1 d . . . H21F H 0.9315 0.3560 -0.1067 0.130 Uiso 1 1 calc R . . H21G H 0.9285 0.2660 -0.1307 0.130 Uiso 1 1 calc R . . H21H H 0.9279 0.2864 -0.0544 0.130 Uiso 1 1 calc R . . C219 C 0.73539(15) 0.54500(12) -0.05202(10) 0.0479(4) Uani 1 1 d . . . C220 C 0.8587(2) 0.64255(18) -0.06133(15) 0.0770(7) Uani 1 1 d . . . H22A H 0.8181 0.6502 -0.1067 0.092 Uiso 1 1 calc R . . H22B H 0.8756 0.6952 -0.0412 0.092 Uiso 1 1 calc R . . C221 C 0.9484(3) 0.6005(2) -0.0656(2) 0.0997(11) Uani 1 1 d . . . H22C H 0.9890 0.5938 -0.0207 0.150 Uiso 1 1 calc R . . H22D H 0.9854 0.6307 -0.0931 0.150 Uiso 1 1 calc R . . H22E H 0.9315 0.5486 -0.0858 0.150 Uiso 1 1 calc R . . C222 C 0.79669(19) 0.75355(15) 0.09580(13) 0.0656(6) Uani 1 1 d . . . H22F H 0.8389 0.8003 0.0976 0.098 Uiso 1 1 calc R . . H22G H 0.7542 0.7493 0.0513 0.098 Uiso 1 1 calc R . . H22H H 0.8381 0.7063 0.1049 0.098 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 S1 0.0366(2) 0.0431(2) 0.0322(2) -0.00288(15) 0.00530(16) -0.00504(16) O11 0.0429(7) 0.0824(10) 0.0471(8) 0.0066(7) 0.0157(6) 0.0048(7) O12 0.0386(7) 0.1088(13) 0.0351(7) -0.0067(7) 0.0019(5) 0.0148(7) O13 0.0815(11) 0.0761(11) 0.0558(9) -0.0167(8) 0.0201(8) -0.0421(9) O14 0.0637(9) 0.0897(11) 0.0289(6) -0.0048(6) 0.0024(6) -0.0299(8) N11 0.0617(10) 0.0500(9) 0.0420(8) -0.0062(7) 0.0097(7) 0.0075(8) N12 0.0470(8) 0.0362(7) 0.0333(7) -0.0010(6) 0.0084(6) 0.0000(6) N13 0.0368(7) 0.0430(7) 0.0325(7) -0.0008(6) 0.0073(6) -0.0015(6) N14 0.0392(8) 0.0684(11) 0.0361(8) -0.0083(7) 0.0069(6) 0.0029(7) C11 0.0851(17) 0.0723(15) 0.0537(13) -0.0215(11) 0.0170(12) 0.0130(13) C12 0.0897(18) 0.0828(17) 0.0443(11) -0.0240(11) 0.0040(11) 0.0015(14) C13 0.0655(13) 0.0650(13) 0.0415(10) -0.0104(9) 0.0019(9) -0.0009(11) C14 0.0544(10) 0.0396(9) 0.0353(9) -0.0016(7) 0.0066(8) 0.0013(8) C15 0.0481(10) 0.0370(8) 0.0368(9) 0.0002(7) 0.0078(7) 0.0003(7) C16 0.0403(8) 0.0331(8) 0.0322(8) 0.0025(6) 0.0075(6) -0.0001(7) C17 0.0361(8) 0.0341(8) 0.0318(8) 0.0008(6) 0.0061(6) -0.0002(6) C18 0.0369(8) 0.0334(8) 0.0301(8) 0.0011(6) 0.0060(6) -0.0017(6) C19 0.0375(8) 0.0363(8) 0.0289(7) 0.0017(6) 0.0066(6) -0.0025(6) C110 0.0393(8) 0.0398(8) 0.0330(8) 0.0012(7) 0.0064(7) -0.0014(7) C111 0.0386(9) 0.0425(9) 0.0354(8) -0.0006(7) 0.0052(7) 0.0002(7) C112 0.0437(10) 0.0604(12) 0.0444(10) -0.0027(9) 0.0019(8) 0.0099(9) C113 0.0392(10) 0.0839(16) 0.0640(13) -0.0130(12) 0.0082(9) 0.0122(10) C114 0.0476(11) 0.0964(18) 0.0508(12) -0.0180(12) 0.0164(9) 0.0071(11) C115 0.0595(13) 0.0739(15) 0.0635(14) -0.0098(12) 0.0042(11) 0.0184(12) C116 0.0393(9) 0.0430(9) 0.0364(9) -0.0046(7) 0.0061(7) 0.0019(7) C117 0.0395(11) 0.179(3) 0.0504(13) -0.0254(16) -0.0035(10) 0.0243(15) C118 0.066(2) 0.760(19) 0.0492(18) -0.069(5) -0.0147(16) 0.105(5) C119 0.0353(8) 0.0411(9) 0.0337(8) -0.0030(7) 0.0071(6) -0.0009(7) C120 0.0766(17) 0.142(3) 0.0353(11) -0.0265(13) 0.0045(11) -0.0412(17) C121 0.0651(19) 0.323(7) 0.100(3) -0.130(4) 0.0220(18) -0.044(3) C122 0.0502(12) 0.115(2) 0.0341(10) -0.0151(11) 0.0015(9) 0.0105(12) S2 0.0417(2) 0.0461(2) 0.0345(2) 0.00698(16) 0.00843(17) -0.00434(17) O21 0.0575(9) 0.1289(17) 0.0562(9) -0.0292(10) 0.0148(8) -0.0185(10) O22 0.0499(8) 0.0605(9) 0.0637(9) -0.0056(7) 0.0164(7) 0.0059(7) O23 0.0889(12) 0.0869(12) 0.0455(9) 0.0037(8) 0.0261(8) -0.0252(10) O24 0.0720(11) 0.0917(12) 0.0614(10) 0.0024(8) 0.0241(8) -0.0385(9) N21 0.0404(8) 0.0467(8) 0.0385(7) 0.0025(6) 0.0075(6) -0.0019(6) N22 0.0374(7) 0.0456(8) 0.0389(7) 0.0070(6) 0.0060(6) -0.0003(6) N23 0.0386(7) 0.0447(8) 0.0414(8) 0.0097(6) 0.0033(6) -0.0035(6) N24 0.0547(9) 0.0446(9) 0.0520(9) 0.0100(7) 0.0055(7) -0.0066(7) C21 0.0470(10) 0.0492(10) 0.0567(12) 0.0012(9) 0.0068(9) -0.0102(9) C22 0.0428(10) 0.0608(12) 0.0596(12) 0.0109(10) 0.0141(9) -0.0101(9) C23 0.0471(10) 0.0571(11) 0.0439(10) 0.0029(8) 0.0170(8) -0.0006(9) C24 0.0379(8) 0.0455(9) 0.0374(9) 0.0039(7) 0.0083(7) -0.0013(7) C25 0.0420(9) 0.0459(9) 0.0368(8) 0.0037(7) 0.0074(7) -0.0003(8) C26 0.0345(8) 0.0461(9) 0.0364(8) 0.0061(7) 0.0040(7) 0.0019(7) C27 0.0355(8) 0.0508(10) 0.0378(9) 0.0080(7) 0.0069(7) 0.0008(7) C28 0.0345(8) 0.0514(10) 0.0373(9) 0.0088(8) 0.0051(7) -0.0029(7) C29 0.0335(8) 0.0474(10) 0.0353(8) 0.0106(7) 0.0025(6) -0.0032(7) C210 0.0409(9) 0.0474(10) 0.0424(9) 0.0085(8) 0.0056(7) -0.0046(8) C211 0.0466(10) 0.0440(10) 0.0452(10) 0.0088(8) 0.0037(8) -0.0024(8) C212 0.0668(13) 0.0577(12) 0.0554(12) 0.0018(10) 0.0162(10) -0.0026(10) C213 0.0846(17) 0.0550(13) 0.0576(13) -0.0046(10) 0.0093(12) 0.0014(12) C214 0.0746(15) 0.0453(11) 0.0637(13) 0.0035(10) 0.0004(11) -0.0089(10) C215 0.0569(11) 0.0561(11) 0.0434(10) -0.0003(8) 0.0173(9) 0.0052(9) C216 0.0463(10) 0.0563(11) 0.0421(9) 0.0027(8) 0.0127(8) -0.0080(9) C217 0.0821(17) 0.0594(13) 0.0814(17) -0.0070(12) 0.0373(14) 0.0059(12) C218 0.0829(19) 0.090(2) 0.099(2) 0.0128(17) 0.0463(17) 0.0287(16) C219 0.0465(10) 0.0543(11) 0.0449(10) 0.0097(8) 0.0141(8) -0.0022(8) C220 0.0775(17) 0.0784(17) 0.0850(18) 0.0111(14) 0.0394(14) -0.0219(14) C221 0.086(2) 0.095(2) 0.130(3) 0.021(2) 0.048(2) -0.0087(17) C222 0.0650(14) 0.0650(14) 0.0700(14) 0.0081(11) 0.0212(11) -0.0200(11) _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_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag S1 C16 . . 1.7490(17) Y S1 C19 . . 1.7583(16) Y O11 C116 . . 1.194(2) Y O12 C116 . . 1.335(2) Y O12 C117 . . 1.451(3) Y O13 C119 . . 1.193(2) Y O14 C119 . . 1.310(2) Y O14 C120 . . 1.462(3) Y N11 C11 . . 1.361(3) Y N11 C14 . . 1.376(3) Y N11 C115 . . 1.456(3) Y N12 C15 . . 1.289(2) Y N12 C16 . . 1.379(2) Y N13 C110 . . 1.291(2) Y N13 C19 . . 1.376(2) Y N14 C114 . . 1.353(3) Y N14 C111 . . 1.381(2) Y N14 C122 . . 1.455(2) Y C11 C12 . . 1.364(4) Y C11 H11 . . 0.94 ? C12 C13 . . 1.388(3) Y C12 H12 . . 0.94 ? C13 C14 . . 1.394(3) Y C13 H13 . . 0.94 ? C14 C15 . . 1.423(2) Y C15 H15 . . 0.94 ? C16 C17 . . 1.377(2) Y C17 C18 . . 1.428(2) Y C17 C116 . . 1.485(2) Y C18 C19 . . 1.371(2) Y C18 C119 . . 1.489(2) Y C110 C111 . . 1.424(2) Y C110 H110 . . 0.94 ? C111 C112 . . 1.384(3) Y C112 C113 . . 1.388(3) Y C112 H112 . . 0.94 ? C113 C114 . . 1.372(3) Y C113 H113 . . 0.94 ? C114 H114 . . 0.94 ? C115 H11a . . 0.97 ? C115 H11b . . 0.97 ? C115 H11c . . 0.97 ? C117 C118 . . 1.453(4) Y C117 H11d . . 0.98 ? C117 H11e . . 0.98 ? C118 H11f . . 0.97 ? C118 H11g . . 0.97 ? C118 H11h . . 0.97 ? C120 C121 . . 1.352(4) Y C120 H12a . . 0.98 ? C120 H12b . . 0.98 ? C121 H12c . . 0.97 ? C121 H12d . . 0.97 ? C121 H12e . . 0.97 ? C122 H12f . . 0.97 ? C122 H12g . . 0.97 ? C122 H12h . . 0.97 ? S2 C26 . . 1.7513(19) Y S2 C29 . . 1.7540(17) Y O21 C216 . . 1.192(2) Y O22 C216 . . 1.335(2) Y O22 C217 . . 1.447(3) Y O23 C219 . . 1.199(3) Y O24 C219 . . 1.334(3) Y O24 C220 . . 1.460(3) Y N21 C21 . . 1.359(2) Y N21 C24 . . 1.372(2) Y N21 C215 . . 1.459(2) Y N22 C25 . . 1.288(2) Y N22 C26 . . 1.378(2) Y N23 C210 . . 1.282(2) Y N23 C29 . . 1.372(2) Y N24 C214 . . 1.359(3) Y N24 C211 . . 1.379(2) Y N24 C222 . . 1.456(3) Y C21 C22 . . 1.370(3) Y C21 H21 . . 0.94 ? C22 C23 . . 1.387(3) Y C22 H22 . . 0.94 ? C23 C24 . . 1.394(2) Y C23 H23 . . 0.94 ? C24 C25 . . 1.427(3) Y C25 H25 . . 0.94 ? C26 C27 . . 1.370(2) Y C27 C28 . . 1.427(3) Y C27 C216 . . 1.491(3) Y C28 C29 . . 1.376(3) Y C28 C219 . . 1.482(2) Y C210 C211 . . 1.432(3) Y C210 H210 . . 0.94 ? C211 C212 . . 1.377(3) Y C212 C213 . . 1.398(3) Y C212 H212 . . 0.94 ? C213 C214 . . 1.363(4) Y C213 H213 . . 0.94 ? C214 H214 . . 0.94 ? C215 H21a . . 0.97 ? C215 H21b . . 0.97 ? C215 H21c . . 0.97 ? C217 C218 . . 1.490(4) Y C217 H21d . . 0.98 ? C217 H21e . . 0.98 ? C218 H21f . . 0.97 ? C218 H21g . . 0.97 ? C218 H21h . . 0.97 ? C220 C221 . . 1.435(4) Y C220 H22a . . 0.98 ? C220 H22b . . 0.98 ? C221 H22c . . 0.97 ? C221 H22d . . 0.97 ? C221 H22e . . 0.97 ? C222 H22f . . 0.97 ? C222 H22g . . 0.97 ? C222 H22h . . 0.97 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C16 S1 C19 . . . 91.72(8) Y C116 O12 C117 . . . 116.47(17) Y C119 O14 C120 . . . 115.26(17) Y C11 N11 C14 . . . 107.98(18) Y C11 N11 C115 . . . 124.15(19) Y C14 N11 C115 . . . 127.83(17) Y C15 N12 C16 . . . 119.36(16) Y C110 N13 C19 . . . 120.38(14) Y C114 N14 C111 . . . 108.38(16) Y C114 N14 C122 . . . 124.24(17) Y C111 N14 C122 . . . 127.21(16) Y N11 C11 C12 . . . 109.6(2) Y N11 C11 H11 . . . 125.2 ? C12 C11 H11 . . . 125.2 ? C11 C12 C13 . . . 107.3(2) Y C11 C12 H12 . . . 126.4 ? C13 C12 H12 . . . 126.4 ? C12 C13 C14 . . . 107.6(2) Y C12 C13 H13 . . . 126.2 ? C14 C13 H13 . . . 126.2 ? N11 C14 C13 . . . 107.50(17) Y N11 C14 C15 . . . 126.80(17) Y C13 C14 C15 . . . 125.64(19) Y N12 C15 C14 . . . 125.52(18) Y N12 C15 H15 . . . 117.2 ? C14 C15 H15 . . . 117.2 ? C17 C16 N12 . . . 125.52(16) Y C17 C16 S1 . . . 110.88(12) Y N12 C16 S1 . . . 123.42(13) Y C16 C17 C18 . . . 113.24(15) Y C16 C17 C116 . . . 123.15(15) Y C18 C17 C116 . . . 123.58(14) Y C19 C18 C17 . . . 113.44(14) Y C19 C18 C119 . . . 122.90(15) Y C17 C18 C119 . . . 122.87(15) Y C18 C19 N13 . . . 125.76(15) Y C18 C19 S1 . . . 110.71(12) Y N13 C19 S1 . . . 123.53(12) Y N13 C110 C111 . . . 124.55(16) Y N13 C110 H110 . . . 117.7 ? C111 C110 H110 . . . 117.7 ? N14 C111 C112 . . . 107.14(16) Y N14 C111 C110 . . . 126.02(16) Y C112 C111 C110 . . . 126.77(17) Y C111 C112 C113 . . . 108.20(18) Y C111 C112 H112 . . . 125.9 ? C113 C112 H112 . . . 125.9 ? C114 C113 C112 . . . 106.81(18) Y C114 C113 H113 . . . 126.6 ? C112 C113 H113 . . . 126.6 ? N14 C114 C113 . . . 109.47(19) Y N14 C114 H114 . . . 125.3 ? C113 C114 H114 . . . 125.3 ? N11 C115 H11A . . . 109.5 ? N11 C115 H11B . . . 109.5 ? H11A C115 H11B . . . 109.5 ? N11 C115 H11C . . . 109.5 ? H11A C115 H11C . . . 109.5 ? H11B C115 H11C . . . 109.5 ? O11 C116 O12 . . . 123.77(17) Y O11 C116 C17 . . . 126.22(16) Y O12 C116 C17 . . . 110.01(15) Y O12 C117 C118 . . . 107.3(2) Y O12 C117 H11D . . . 110.3 ? C118 C117 H11D . . . 110.3 ? O12 C117 H11E . . . 110.3 ? C118 C117 H11E . . . 110.3 ? H11D C117 H11E . . . 108.5 ? C117 C118 H11F . . . 109.5 ? C117 C118 H11G . . . 109.5 ? H11F C118 H11G . . . 109.5 ? C117 C118 H11H . . . 109.5 ? H11F C118 H11H . . . 109.5 ? H11G C118 H11H . . . 109.5 ? O13 C119 O14 . . . 123.75(16) Y O13 C119 C18 . . . 122.90(16) Y O14 C119 C18 . . . 113.32(15) Y C121 C120 O14 . . . 112.0(2) Y C121 C120 H12A . . . 109.2 ? O14 C120 H12A . . . 109.2 ? C121 C120 H12B . . . 109.2 ? O14 C120 H12B . . . 109.2 ? H12A C120 H12B . . . 107.9 ? C120 C121 H12C . . . 109.5 ? C120 C121 H12D . . . 109.5 ? H12C C121 H12D . . . 109.5 ? C120 C121 H12E . . . 109.5 ? H12C C121 H12E . . . 109.5 ? H12D C121 H12E . . . 109.5 ? N14 C122 H12F . . . 109.5 ? N14 C122 H12G . . . 109.5 ? H12F C122 H12G . . . 109.5 ? N14 C122 H12H . . . 109.5 ? H12F C122 H12H . . . 109.5 ? H12G C122 H12H . . . 109.5 ? C26 S2 C29 . . . 91.73(9) Y C216 O22 C217 . . . 116.75(18) Y C219 O24 C220 . . . 117.24(19) Y C21 N21 C24 . . . 108.27(16) Y C21 N21 C215 . . . 124.15(17) Y C24 N21 C215 . . . 127.56(16) Y C25 N22 C26 . . . 119.07(16) Y C210 N23 C29 . . . 120.45(16) Y C214 N24 C211 . . . 108.07(19) Y C214 N24 C222 . . . 124.15(19) Y C211 N24 C222 . . . 127.75(18) Y N21 C21 C22 . . . 109.72(18) Y N21 C21 H21 . . . 125.1 ? C22 C21 H21 . . . 125.1 ? C21 C22 C23 . . . 106.67(17) Y C21 C22 H22 . . . 126.7 ? C23 C22 H22 . . . 126.7 ? C22 C23 C24 . . . 108.08(18) Y C22 C23 H23 . . . 126 ? C24 C23 H23 . . . 126 ? N21 C24 C23 . . . 107.26(16) Y N21 C24 C25 . . . 126.90(16) Y C23 C24 C25 . . . 125.84(17) Y N22 C25 C24 . . . 125.55(18) Y N22 C25 H25 . . . 117.2 ? C24 C25 H25 . . . 117.2 ? C27 C26 N22 . . . 125.10(17) Y C27 C26 S2 . . . 110.78(14) Y N22 C26 S2 . . . 124.09(13) Y C26 C27 C28 . . . 113.64(17) Y C26 C27 C216 . . . 121.18(17) Y C28 C27 C216 . . . 125.09(16) Y C29 C28 C27 . . . 113.09(15) Y C29 C28 C219 . . . 125.81(18) Y C27 C28 C219 . . . 120.71(17) Y N23 C29 C28 . . . 126.39(16) Y N23 C29 S2 . . . 122.86(14) Y C28 C29 S2 . . . 110.74(14) Y N23 C210 C211 . . . 124.37(17) Y N23 C210 H210 . . . 117.8 ? C211 C210 H210 . . . 117.8 ? C212 C211 N24 . . . 107.69(18) Y C212 C211 C210 . . . 127.13(18) Y N24 C211 C210 . . . 125.18(18) Y C211 C212 C213 . . . 107.8(2) Y C211 C212 H212 . . . 126.1 ? C213 C212 H212 . . . 126.1 ? C214 C213 C212 . . . 107.0(2) Y C214 C213 H213 . . . 126.5 ? C212 C213 H213 . . . 126.5 ? N24 C214 C213 . . . 109.5(2) Y N24 C214 H214 . . . 125.3 ? C213 C214 H214 . . . 125.3 ? N21 C215 H21A . . . 109.5 ? N21 C215 H21B . . . 109.5 ? H21A C215 H21B . . . 109.5 ? N21 C215 H21C . . . 109.5 ? H21A C215 H21C . . . 109.5 ? H21B C215 H21C . . . 109.5 ? O21 C216 O22 . . . 123.6(2) Y O21 C216 C27 . . . 125.87(19) Y O22 C216 C27 . . . 110.56(16) Y O22 C217 C218 . . . 107.8(2) Y O22 C217 H21D . . . 110.1 ? C218 C217 H21D . . . 110.1 ? O22 C217 H21E . . . 110.1 ? C218 C217 H21E . . . 110.1 ? H21D C217 H21E . . . 108.5 ? C217 C218 H21F . . . 109.5 ? C217 C218 H21G . . . 109.5 ? H21F C218 H21G . . . 109.5 ? C217 C218 H21H . . . 109.5 ? H21F C218 H21H . . . 109.5 ? H21G C218 H21H . . . 109.5 ? O23 C219 O24 . . . 123.64(18) Y O23 C219 C28 . . . 122.71(19) Y O24 C219 C28 . . . 113.62(17) Y C221 C220 O24 . . . 110.3(2) Y C221 C220 H22A . . . 109.6 ? O24 C220 H22A . . . 109.6 ? C221 C220 H22B . . . 109.6 ? O24 C220 H22B . . . 109.6 ? H22A C220 H22B . . . 108.1 ? C220 C221 H22C . . . 109.5 ? C220 C221 H22D . . . 109.5 ? H22C C221 H22D . . . 109.5 ? C220 C221 H22E . . . 109.5 ? H22C C221 H22E . . . 109.5 ? H22D C221 H22E . . . 109.5 ? N24 C222 H22F . . . 109.5 ? N24 C222 H22G . . . 109.5 ? H22F C222 H22G . . . 109.5 ? N24 C222 H22H . . . 109.5 ? H22F C222 H22H . . . 109.5 ? H22G C222 H22H . . . 109.5 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C14 N11 C11 C12 . . . . -0.3(3) Y C115 N11 C11 C12 . . . . 177.6(2) Y N11 C11 C12 C13 . . . . 0.5(3) Y C11 C12 C13 C14 . . . . -0.5(3) Y C11 N11 C14 C13 . . . . 0.0(2) Y C115 N11 C14 C13 . . . . -177.9(2) Y C11 N11 C14 C15 . . . . 177.3(2) Y C115 N11 C14 C15 . . . . -0.6(3) Y C12 C13 C14 N11 . . . . 0.3(3) Y C12 C13 C14 C15 . . . . -177.0(2) Y C16 N12 C15 C14 . . . . -176.65(16) Y N11 C14 C15 N12 . . . . -0.4(3) Y C13 C14 C15 N12 . . . . 176.5(2) Y C15 N12 C16 C17 . . . . -170.84(16) Y C15 N12 C16 S1 . . . . 14.5(2) Y C19 S1 C16 C17 . . . . -0.30(13) Y C19 S1 C16 N12 . . . . 175.07(14) Y N12 C16 C17 C18 . . . . -174.41(15) Y S1 C16 C17 C18 . . . . 0.84(18) Y N12 C16 C17 C116 . . . . 3.4(3) Y S1 C16 C17 C116 . . . . 178.63(13) Y C16 C17 C18 C19 . . . . -1.1(2) Y C116 C17 C18 C19 . . . . -178.91(15) Y C16 C17 C18 C119 . . . . -171.22(15) Y C116 C17 C18 C119 . . . . 11.0(2) Y C17 C18 C19 N13 . . . . -178.82(15) Y C119 C18 C19 N13 . . . . -8.7(3) Y C17 C18 C19 S1 . . . . 0.87(18) Y C119 C18 C19 S1 . . . . 170.96(13) Y C110 N13 C19 C18 . . . . 155.71(17) Y C110 N13 C19 S1 . . . . -23.9(2) Y C16 S1 C19 C18 . . . . -0.33(13) Y C16 S1 C19 N13 . . . . 179.36(14) Y C19 N13 C110 C111 . . . . 175.30(16) Y C114 N14 C111 C112 . . . . -0.1(2) Y C122 N14 C111 C112 . . . . -175.5(2) Y C114 N14 C111 C110 . . . . -177.3(2) Y C122 N14 C111 C110 . . . . 7.3(3) Y N13 C110 C111 N14 . . . . -1.9(3) Y N13 C110 C111 C112 . . . . -178.66(19) Y N14 C111 C112 C113 . . . . 0.0(2) Y C110 C111 C112 C113 . . . . 177.2(2) Y C111 C112 C113 C114 . . . . 0.1(3) Y C111 N14 C114 C113 . . . . 0.1(3) Y C122 N14 C114 C113 . . . . 175.7(2) Y C112 C113 C114 N14 . . . . -0.1(3) Y C117 O12 C116 O11 . . . . 5.3(3) Y C117 O12 C116 C17 . . . . -175.0(2) Y C16 C17 C116 O11 . . . . 39.6(3) Y C18 C17 C116 O11 . . . . -142.9(2) Y C16 C17 C116 O12 . . . . -140.12(17) Y C18 C17 C116 O12 . . . . 37.4(2) Y C116 O12 C117 C118 . . . . 167.8(5) Y C120 O14 C119 O13 . . . . -0.4(3) Y C120 O14 C119 C18 . . . . -178.3(2) Y C19 C18 C119 O13 . . . . -117.5(2) Y C17 C18 C119 O13 . . . . 51.7(3) Y C19 C18 C119 O14 . . . . 60.4(2) Y C17 C18 C119 O14 . . . . -130.42(18) Y C119 O14 C120 C121 . . . . 160.2(4) Y C24 N21 C21 C22 . . . . -0.2(2) Y C215 N21 C21 C22 . . . . -178.86(18) Y N21 C21 C22 C23 . . . . 0.3(2) Y C21 C22 C23 C24 . . . . -0.3(2) Y C21 N21 C24 C23 . . . . 0.0(2) Y C215 N21 C24 C23 . . . . 178.63(17) Y C21 N21 C24 C25 . . . . -179.81(18) Y C215 N21 C24 C25 . . . . -1.2(3) Y C22 C23 C24 N21 . . . . 0.2(2) Y C22 C23 C24 C25 . . . . 179.98(18) Y C26 N22 C25 C24 . . . . 178.96(16) Y N21 C24 C25 N22 . . . . -1.9(3) Y C23 C24 C25 N22 . . . . 178.35(18) Y C25 N22 C26 C27 . . . . -171.59(17) Y C25 N22 C26 S2 . . . . 10.6(2) Y C29 S2 C26 C27 . . . . 0.56(14) Y C29 S2 C26 N22 . . . . 178.61(15) Y N22 C26 C27 C28 . . . . -178.34(16) Y S2 C26 C27 C28 . . . . -0.32(19) Y N22 C26 C27 C216 . . . . -1.7(3) Y S2 C26 C27 C216 . . . . 176.34(14) Y C26 C27 C28 C29 . . . . -0.2(2) Y C216 C27 C28 C29 . . . . -176.71(17) Y C26 C27 C28 C219 . . . . -173.36(16) Y C216 C27 C28 C219 . . . . 10.1(3) Y C210 N23 C29 C28 . . . . 171.04(17) Y C210 N23 C29 S2 . . . . -8.8(2) Y C27 C28 C29 N23 . . . . -179.25(16) Y C219 C28 C29 N23 . . . . -6.5(3) Y C27 C28 C29 S2 . . . . 0.62(19) Y C219 C28 C29 S2 . . . . 173.37(15) Y C26 S2 C29 N23 . . . . 179.20(15) Y C26 S2 C29 C28 . . . . -0.67(14) Y C29 N23 C210 C211 . . . . 175.58(17) Y C214 N24 C211 C212 . . . . -0.2(2) Y C222 N24 C211 C212 . . . . -178.4(2) Y C214 N24 C211 C210 . . . . -179.50(19) Y C222 N24 C211 C210 . . . . 2.3(3) Y N23 C210 C211 C212 . . . . -179.5(2) Y N23 C210 C211 N24 . . . . -0.3(3) Y N24 C211 C212 C213 . . . . 0.2(2) Y C210 C211 C212 C213 . . . . 179.5(2) Y C211 C212 C213 C214 . . . . -0.1(3) Y C211 N24 C214 C213 . . . . 0.1(3) Y C222 N24 C214 C213 . . . . 178.4(2) Y C212 C213 C214 N24 . . . . 0.0(3) Y C217 O22 C216 O21 . . . . -2.5(3) Y C217 O22 C216 C27 . . . . 175.95(18) Y C26 C27 C216 O21 . . . . 61.9(3) Y C28 C27 C216 O21 . . . . -121.8(2) Y C26 C27 C216 O22 . . . . -116.48(19) Y C28 C27 C216 O22 . . . . 59.8(2) Y C216 O22 C217 C218 . . . . 175.9(2) Y C220 O24 C219 O23 . . . . -2.3(4) Y C220 O24 C219 C28 . . . . 179.9(2) Y C29 C28 C219 O23 . . . . -142.7(2) Y C27 C28 C219 O23 . . . . 29.5(3) Y C29 C28 C219 O24 . . . . 35.0(3) Y C27 C28 C219 O24 . . . . -152.73(19) Y C219 O24 C220 C221 . . . . -89.6(3) Y _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 71.98 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.470 _refine_diff_density_min -0.492 _refine_diff_density_rms 0.055