# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1170 data_s92 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53 H39 Cr N O13 S32' _chemical_formula_weight 1975.99 _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' 'O' 'O' 0.0106 0.0060 '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' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.371(2) _cell_length_b 19.518(3) _cell_length_c 35.646(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7216(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.137 _exptl_crystal_density_method ? _exptl_crystal_F_000 4728 _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST TV Area detector' _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24400 _diffrn_reflns_av_R_equivalents 0.2159 _diffrn_reflns_av_sigmaI/netI 0.3233 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.06 _reflns_number_total 5599 _reflns_number_observed 2195 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Pflugrath, 1989)' _computing_cell_refinement MADNES _computing_data_reduction ABSURD _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Pearce, Watkin, 1995)' _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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^)+(0.0000P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5599 _refine_ls_number_parameters 462 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1764 _refine_ls_R_factor_obs 0.0655 _refine_ls_wR_factor_all 0.1243 _refine_ls_wR_factor_obs 0.1033 _refine_ls_goodness_of_fit_all 0.731 _refine_ls_goodness_of_fit_obs 1.041 _refine_ls_restrained_S_all 0.733 _refine_ls_restrained_S_obs 1.042 _refine_ls_shift/esd_max -0.007 _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 Cr1 Cr 0.5000 0.19088(12) 0.2500 0.0167(6) Uani 1 d S . S1 S 0.4782(2) 0.57287(13) 0.05776(6) 0.0188(6) Uani 1 d . . S2 S 0.2748(2) 0.48158(14) 0.03070(6) 0.0217(6) Uani 1 d . . S3 S 0.4700(2) 0.51738(14) 0.13647(6) 0.0226(7) Uani 1 d . . S4 S 0.2360(3) 0.40874(14) 0.10065(6) 0.0279(7) Uani 1 d . . S5 S 0.4865(2) 0.64333(13) -0.02650(6) 0.0210(6) Uani 1 d . . S6 S 0.2829(2) 0.54876(13) -0.04895(6) 0.0195(6) Uani 1 d . . S7 S 0.5058(3) 0.71331(13) -0.09926(6) 0.0254(7) Uani 1 d . . S8 S 0.2508(3) 0.60236(14) -0.12488(6) 0.0245(7) Uani 1 d . . S9 S 1.0099(2) 0.61254(14) 0.02009(6) 0.0239(7) Uani 1 d . . S10 S 0.7782(2) 0.69501(14) 0.03821(6) 0.0217(6) Uani 1 d . . S11 S 0.9807(3) 0.52564(14) 0.08942(6) 0.0253(7) Uani 1 d . . S12 S 0.7186(2) 0.61967(15) 0.10796(6) 0.0257(7) Uani 1 d . . S13 S 1.0177(2) 0.68646(14) -0.06288(6) 0.0229(7) Uani 1 d . . S14 S 0.7884(2) 0.76699(14) -0.04141(6) 0.0233(7) Uani 1 d . . S15 S 1.0116(3) 0.72535(14) -0.14287(6) 0.0238(7) Uani 1 d . . S16 S 0.7484(2) 0.82901(13) -0.11567(6) 0.0218(7) Uani 1 d . . O1 O 0.6654(6) 0.1959(3) 0.22226(14) 0.020(2) Uani 1 d . . O2 O 0.4393(6) 0.1143(4) 0.21845(14) 0.018(2) Uani 1 d . . O3 O 0.4223(6) 0.2638(3) 0.21942(15) 0.021(2) Uani 1 d . . O4 O 0.8454(7) 0.2584(4) 0.2214(2) 0.030(2) Uani 1 d . . O5 O 0.4378(8) 0.0006(4) 0.2155(2) 0.052(3) Uani 1 d . . O6 O 0.2583(7) 0.3379(4) 0.2222(2) 0.035(2) Uani 1 d . . C1 C 0.7397(11) 0.2450(5) 0.2340(2) 0.024(3) Uani 1 d . . C2 C 0.4637(10) 0.0538(6) 0.2305(2) 0.022(3) Uani 1 d . . C3 C 0.3148(10) 0.2880(6) 0.2333(2) 0.020(3) Uani 1 d . . C4 C 0.3826(9) 0.5457(5) 0.0212(2) 0.015(2) Uani 1 d . . C5 C 0.3872(9) 0.5772(5) -0.0135(2) 0.017(2) Uani 1 d . . C6 C 0.4148(9) 0.5144(5) 0.0897(2) 0.014(2) Uani 1 d . . C7 C 0.3226(9) 0.4733(5) 0.0782(2) 0.018(2) Uani 1 d . . C8 C 0.3189(10) 0.4945(6) 0.1590(2) 0.029(3) Uani 1 d . . H8A H 0.3279(10) 0.4998(6) 0.1859(2) 0.035 Uiso 1 calc R . H8B H 0.2519(10) 0.5257(6) 0.1506(2) 0.035 Uiso 1 calc R . C9 C 0.2782(10) 0.4216(6) 0.1503(2) 0.043(4) Uani 1 d . . H9A H 0.2044(10) 0.4099(6) 0.1658(2) 0.051 Uiso 1 calc R . H9B H 0.3480(10) 0.3908(6) 0.1569(2) 0.051 Uiso 1 calc R . C10 C 0.4317(9) 0.6497(5) -0.0721(2) 0.018(2) Uani 1 d . . C11 C 0.3349(9) 0.6068(5) -0.0822(2) 0.021(2) Uani 1 d U . C13 C 0.3478(10) 0.6570(6) -0.1541(2) 0.030(3) Uani 1 d . . H13A H 0.4238(10) 0.6316(6) -0.1617(2) 0.035 Uiso 1 calc R . H13B H 0.2991(10) 0.6675(6) -0.1766(2) 0.035 Uiso 1 calc R . C16 C 0.8956(9) 0.6727(5) 0.0048(2) 0.018(3) Uani 1 d . . C14 C 0.3906(10) 0.7228(5) -0.1368(2) 0.028(3) Uani 1 d . . H14A H 0.3154(10) 0.7466(5) -0.1272(2) 0.033 Uiso 1 calc R . H14B H 0.4284(10) 0.7513(5) -0.1562(2) 0.033 Uiso 1 calc R . C15 C 0.8996(9) 0.7036(5) -0.0283(2) 0.019(2) Uani 1 d . . C17 C 0.9191(9) 0.5903(5) 0.0607(2) 0.022(3) Uani 1 d . . C18 C 0.8168(9) 0.6279(5) 0.0683(2) 0.016(2) Uani 1 d . . C19 C 0.9593(9) 0.5718(6) 0.1333(2) 0.032(3) Uani 1 d . . H19A H 1.0013(9) 0.5463(6) 0.1532(2) 0.039 Uiso 1 calc R . H19B H 1.0022(9) 0.6158(6) 0.1313(2) 0.039 Uiso 1 calc R . C20 C 0.8214(10) 0.5836(6) 0.1440(2) 0.034(3) Uani 1 d . . H20A H 0.8198(10) 0.6140(6) 0.1656(2) 0.041 Uiso 1 calc R . H20B H 0.7847(10) 0.5402(6) 0.1519(2) 0.041 Uiso 1 calc R . C21 C 0.9403(9) 0.7345(5) -0.0981(2) 0.021(3) Uani 1 d . . C22 C 0.8375(9) 0.7721(5) -0.0883(2) 0.014(2) Uani 1 d . . C23 C 0.9384(10) 0.7957(6) -0.1677(2) 0.034(3) Uani 1 d . . H23A H 0.9785(10) 0.8381(6) -0.1596(2) 0.041 Uiso 1 calc R . H23B H 0.9552(10) 0.7904(6) -0.1943(2) 0.041 Uiso 1 calc R . C24 C 0.7904(10) 0.8012(5) -0.1615(2) 0.027(3) Uani 1 d . . H24A H 0.7517(10) 0.7567(5) -0.1660(2) 0.033 Uiso 1 calc R . H24B H 0.7549(10) 0.8330(5) -0.1797(2) 0.033 Uiso 1 calc R . N01 N 0.2036(16) 0.4455(10) 0.2933(4) 0.035(5) Uani 0.50 d P . C01 C 0.2933(20) 0.4673(10) 0.2789(5) 0.015(5) Uani 0.50 d P . C02 C 0.3941(11) 0.4932(6) 0.2639(2) 0.036(3) Uani 1 d . . C03 C 0.3966(12) 0.5648(6) 0.2635(3) 0.047(4) Uani 1 d U . H03 H 0.3263(12) 0.5892(6) 0.2727(3) 0.056 Uiso 1 calc R . C04 C 0.5000 0.5993(10) 0.2500 0.059(5) Uani 1 d SU . H04 H 0.5000 0.6470(10) 0.2500 0.071 Uiso 1 calc SR . C05 C 0.5000 0.4570(8) 0.2500 0.022(4) Uani 1 d SU . H05 H 0.5000 0.4094(8) 0.2500 0.027 Uiso 1 calc SR . O01 O 0.5000 -0.1293(6) 0.2500 0.057(4) Uani 1 d S . 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 Cr1 0.0135(14) 0.0194(14) 0.0172(12) 0.000 0.0002(9) 0.000 S1 0.019(2) 0.022(2) 0.0163(14) 0.0001(10) 0.0002(11) -0.0036(13) S2 0.017(2) 0.023(2) 0.0245(15) 0.0031(11) -0.0043(11) -0.0031(14) S3 0.017(2) 0.034(2) 0.0167(14) 0.0034(12) -0.0020(11) -0.0003(14) S4 0.023(2) 0.025(2) 0.036(2) 0.0138(12) -0.0048(13) -0.0084(14) S5 0.021(2) 0.022(2) 0.0204(14) 0.0006(11) 0.0011(12) -0.0028(13) S6 0.017(2) 0.022(2) 0.0196(13) 0.0036(11) -0.0020(11) -0.0032(13) S7 0.020(2) 0.025(2) 0.031(2) 0.0086(11) 0.0012(12) -0.0029(15) S8 0.021(2) 0.035(2) 0.0180(13) 0.0056(11) -0.0055(12) -0.0023(15) S9 0.014(2) 0.033(2) 0.0244(15) 0.0052(12) 0.0050(11) 0.0046(15) S10 0.016(2) 0.024(2) 0.0242(14) 0.0014(11) 0.0004(11) 0.0059(14) S11 0.021(2) 0.031(2) 0.025(2) 0.0071(12) 0.0011(12) 0.0042(14) S12 0.016(2) 0.041(2) 0.0207(15) -0.0004(11) 0.0011(11) -0.0017(15) S13 0.019(2) 0.032(2) 0.0177(14) 0.0040(11) -0.0019(11) 0.0061(14) S14 0.019(2) 0.030(2) 0.0206(15) -0.0004(11) 0.0017(11) 0.0054(14) S15 0.018(2) 0.033(2) 0.0205(15) 0.0028(12) 0.0011(12) 0.0054(14) S16 0.016(2) 0.023(2) 0.0264(14) 0.0055(11) -0.0009(12) 0.0001(13) O1 0.017(4) 0.027(5) 0.017(4) 0.001(3) 0.008(3) 0.006(4) O2 0.016(4) 0.023(5) 0.016(4) -0.004(3) -0.000(3) 0.002(3) O3 0.017(4) 0.026(5) 0.021(4) 0.003(3) 0.004(3) -0.001(4) O4 0.017(5) 0.034(6) 0.039(4) -0.007(3) 0.011(3) -0.006(4) O5 0.097(8) 0.014(6) 0.046(5) -0.008(4) -0.029(5) -0.006(5) O6 0.042(5) 0.032(5) 0.031(4) 0.011(3) 0.008(4) 0.021(4) C1 0.029(7) 0.022(8) 0.021(6) 0.004(5) -0.017(5) 0.002(6) C2 0.028(7) 0.013(8) 0.024(6) 0.006(5) -0.006(5) -0.013(6) C3 0.023(7) 0.024(8) 0.013(6) -0.002(5) -0.002(5) -0.006(6) C4 0.022(6) 0.007(6) 0.017(6) 0.000(4) -0.001(4) 0.004(5) C5 0.011(6) 0.028(7) 0.012(6) -0.005(4) -0.005(4) -0.001(5) C6 0.016(6) 0.012(6) 0.013(5) -0.003(4) 0.005(4) 0.002(5) C7 0.016(6) 0.025(7) 0.012(5) 0.001(4) -0.001(4) -0.001(5) C8 0.037(8) 0.031(8) 0.019(6) 0.007(5) 0.014(5) 0.003(6) C9 0.029(8) 0.085(11) 0.014(6) 0.022(6) 0.006(5) -0.023(7) C10 0.019(6) 0.021(7) 0.014(5) 0.002(4) 0.001(4) -0.004(5) C11 0.020(5) 0.013(5) 0.030(5) 0.004(4) 0.001(4) 0.006(4) C13 0.028(7) 0.040(8) 0.020(6) 0.013(5) 0.001(5) 0.007(6) C16 0.014(6) 0.032(8) 0.009(5) -0.007(5) 0.002(4) 0.004(5) C14 0.027(7) 0.030(8) 0.026(6) 0.013(5) 0.002(5) 0.005(6) C15 0.017(6) 0.018(7) 0.021(6) -0.009(5) 0.000(4) 0.001(5) C17 0.016(6) 0.036(8) 0.012(6) -0.000(5) 0.006(4) -0.011(6) C18 0.021(7) 0.013(7) 0.013(5) -0.006(4) -0.001(4) -0.005(5) C19 0.021(7) 0.065(9) 0.011(6) -0.004(5) -0.003(5) -0.005(6) C20 0.032(8) 0.053(9) 0.018(6) 0.005(5) -0.005(5) -0.002(6) C21 0.016(6) 0.031(7) 0.016(6) 0.004(5) -0.008(4) 0.001(5) C22 0.019(6) 0.007(6) 0.015(5) -0.006(4) -0.001(4) 0.006(5) C23 0.044(8) 0.039(9) 0.018(6) 0.004(5) 0.011(5) 0.004(7) C24 0.037(8) 0.037(8) 0.009(5) -0.008(4) -0.009(5) 0.009(6) N01 0.012(12) 0.055(16) 0.038(12) -0.003(9) -0.004(9) 0.001(10) C01 0.025(14) 0.004(13) 0.017(12) -0.000(9) -0.016(10) 0.004(11) C02 0.040(9) 0.050(10) 0.018(6) 0.012(5) -0.007(5) 0.003(7) C03 0.056(6) 0.051(7) 0.034(5) -0.010(5) -0.014(5) 0.011(5) C04 0.068(8) 0.056(8) 0.053(7) 0.000 -0.021(6) 0.000 C05 0.022(6) 0.018(6) 0.027(6) 0.000 0.001(5) 0.000 O01 0.039(8) 0.070(10) 0.061(7) 0.000 -0.003(6) 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 Cr1 O3 1.966(7) 3_655 ? Cr1 O3 1.966(6) . ? Cr1 O2 1.973(6) 3_655 ? Cr1 O2 1.973(7) . ? Cr1 O1 1.982(6) 3_655 ? Cr1 O1 1.982(6) . ? S1 C4 1.722(9) . ? S1 C6 1.741(9) . ? S2 C4 1.713(10) . ? S2 C7 1.771(8) . ? S3 C6 1.764(8) . ? S3 C8 1.816(9) . ? S4 C7 1.742(10) . ? S4 C9 1.842(8) . ? S5 C5 1.715(10) . ? S5 C10 1.728(8) . ? S6 C11 1.727(9) . ? S6 C5 1.752(8) . ? S7 C10 1.751(9) . ? S7 C14 1.804(9) . ? S8 C11 1.754(9) . ? S8 C13 1.798(10) . ? S9 C16 1.756(10) . ? S9 C17 1.779(8) . ? S10 C18 1.740(9) . ? S10 C16 1.757(9) . ? S11 C17 1.747(10) . ? S11 C19 1.817(9) . ? S12 C18 1.750(9) . ? S12 C20 1.813(9) . ? S13 C21 1.760(9) . ? S13 C15 1.769(9) . ? S14 C22 1.749(8) . ? S14 C15 1.754(10) . ? S15 C21 1.769(9) . ? S15 C23 1.801(10) . ? S16 C22 1.745(9) . ? S16 C24 1.777(8) . ? O1 C1 1.299(12) . ? O2 C2 1.282(11) . ? O3 C3 1.307(11) . ? O4 C1 1.212(12) . ? O5 C2 1.200(11) . ? O6 C3 1.204(11) . ? C1 C3 1.545(13) 3_655 ? C2 C2 1.58(2) 3_655 ? C3 C1 1.545(13) 3_655 ? C4 C5 1.382(11) . ? C6 C7 1.314(12) . ? C8 C9 1.516(15) . ? C10 C11 1.356(13) . ? C13 C14 1.492(13) . ? C16 C15 1.327(11) . ? C17 C18 1.318(13) . ? C19 C20 1.499(13) . ? C21 C22 1.341(12) . ? C23 C24 1.554(13) . ? N01 C01 1.14(2) . ? C01 C02 1.28(2) . ? C02 C05 1.397(13) . ? C02 C03 1.399(15) . ? C03 C04 1.354(14) . ? C04 C03 1.354(14) 3_655 ? C05 C02 1.397(13) 3_655 ? 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 O3 Cr1 O3 87.2(4) 3_655 . ? O3 Cr1 O2 95.8(2) 3_655 3_655 ? O3 Cr1 O2 174.4(3) . 3_655 ? O3 Cr1 O2 174.4(3) 3_655 . ? O3 Cr1 O2 95.8(2) . . ? O2 Cr1 O2 81.5(4) 3_655 . ? O3 Cr1 O1 92.4(3) 3_655 3_655 ? O3 Cr1 O1 83.5(3) . 3_655 ? O2 Cr1 O1 91.6(3) 3_655 3_655 ? O2 Cr1 O1 92.6(2) . 3_655 ? O3 Cr1 O1 83.5(3) 3_655 . ? O3 Cr1 O1 92.4(3) . . ? O2 Cr1 O1 92.6(2) 3_655 . ? O2 Cr1 O1 91.6(3) . . ? O1 Cr1 O1 174.4(4) 3_655 . ? C4 S1 C6 94.3(4) . . ? C4 S2 C7 94.2(4) . . ? C6 S3 C8 97.5(4) . . ? C7 S4 C9 102.8(5) . . ? C5 S5 C10 96.3(4) . . ? C11 S6 C5 95.4(5) . . ? C10 S7 C14 101.1(5) . . ? C11 S8 C13 101.2(4) . . ? C16 S9 C17 93.3(5) . . ? C18 S10 C16 94.1(5) . . ? C17 S11 C19 95.8(5) . . ? C18 S12 C20 105.4(4) . . ? C21 S13 C15 94.5(5) . . ? C22 S14 C15 95.9(4) . . ? C21 S15 C23 101.0(4) . . ? C22 S16 C24 101.0(4) . . ? C1 O1 Cr1 112.9(6) . . ? C2 O2 Cr1 116.3(6) . . ? C3 O3 Cr1 113.6(6) . . ? O4 C1 O1 125.3(9) . . ? O4 C1 C3 119.5(10) . 3_655 ? O1 C1 C3 115.2(10) . 3_655 ? O5 C2 O2 127.1(9) . . ? O5 C2 C2 120.0(6) . 3_655 ? O2 C2 C2 112.9(5) . 3_655 ? O6 C3 O3 125.7(9) . . ? O6 C3 C1 120.6(10) . 3_655 ? O3 C3 C1 113.7(9) . 3_655 ? C5 C4 S2 121.6(7) . . ? C5 C4 S1 121.5(7) . . ? S2 C4 S1 116.8(5) . . ? C4 C5 S5 126.6(7) . . ? C4 C5 S6 118.9(7) . . ? S5 C5 S6 114.5(5) . . ? C7 C6 S1 118.2(7) . . ? C7 C6 S3 123.4(7) . . ? S1 C6 S3 118.3(5) . . ? C6 C7 S4 132.4(7) . . ? C6 C7 S2 116.5(7) . . ? S4 C7 S2 111.2(5) . . ? C9 C8 S3 112.4(7) . . ? C8 C9 S4 112.9(7) . . ? C11 C10 S5 116.7(7) . . ? C11 C10 S7 128.0(7) . . ? S5 C10 S7 115.2(5) . . ? C10 C11 S6 117.0(7) . . ? C10 C11 S8 128.9(7) . . ? S6 C11 S8 114.0(6) . . ? C14 C13 S8 116.0(6) . . ? C15 C16 S9 124.0(7) . . ? C15 C16 S10 120.8(8) . . ? S9 C16 S10 115.0(5) . . ? C13 C14 S7 114.5(7) . . ? C16 C15 S14 122.4(7) . . ? C16 C15 S13 123.7(8) . . ? S14 C15 S13 113.8(5) . . ? C18 C17 S11 125.1(7) . . ? C18 C17 S9 117.3(8) . . ? S11 C17 S9 117.3(6) . . ? C17 C18 S10 118.5(7) . . ? C17 C18 S12 125.7(7) . . ? S10 C18 S12 115.7(6) . . ? C20 C19 S11 114.4(7) . . ? C19 C20 S12 116.1(6) . . ? C22 C21 S13 117.9(7) . . ? C22 C21 S15 128.6(7) . . ? S13 C21 S15 113.5(5) . . ? C21 C22 S16 128.6(7) . . ? C21 C22 S14 116.7(7) . . ? S16 C22 S14 114.6(5) . . ? C24 C23 S15 113.5(7) . . ? C23 C24 S16 113.2(6) . . ? N01 C01 C02 178.0(20) . . ? C01 C02 C05 126.3(14) . . ? C01 C02 C03 114.5(13) . . ? C05 C02 C03 119.2(12) . . ? C04 C03 C02 121.0(14) . . ? C03 C04 C03 120.4(20) . 3_655 ? C02 C05 C02 119.3(15) . 3_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Cr1 O1 C1 -5.0(6) 3_655 . . . ? O3 Cr1 O1 C1 81.9(6) . . . . ? O2 Cr1 O1 C1 -100.6(6) 3_655 . . . ? O2 Cr1 O1 C1 177.8(6) . . . . ? O1 Cr1 O1 C1 38.6(6) 3_655 . . . ? O3 Cr1 O2 C2 62.2(29) 3_655 . . . ? O3 Cr1 O2 C2 -175.5(7) . . . . ? O2 Cr1 O2 C2 -0.5(5) 3_655 . . . ? O1 Cr1 O2 C2 -91.8(7) 3_655 . . . ? O1 Cr1 O2 C2 91.9(7) . . . . ? O3 Cr1 O3 C3 -83.6(6) 3_655 . . . ? O2 Cr1 O3 C3 39.1(30) 3_655 . . . ? O2 Cr1 O3 C3 101.1(6) . . . . ? O1 Cr1 O3 C3 9.2(6) 3_655 . . . ? O1 Cr1 O3 C3 -167.0(6) . . . . ? Cr1 O1 C1 O4 -179.9(8) . . . . ? Cr1 O1 C1 C3 0.5(10) . . . 3_655 ? Cr1 O2 C2 O5 -178.4(9) . . . . ? Cr1 O2 C2 C2 1.2(13) . . . 3_655 ? Cr1 O3 C3 O6 170.5(8) . . . . ? Cr1 O3 C3 C1 -11.0(10) . . . 3_655 ? C7 S2 C4 C5 -177.1(8) . . . . ? C7 S2 C4 S1 -1.1(6) . . . . ? C6 S1 C4 C5 177.5(8) . . . . ? C6 S1 C4 S2 1.5(6) . . . . ? S2 C4 C5 S5 178.1(6) . . . . ? S1 C4 C5 S5 2.2(13) . . . . ? S2 C4 C5 S6 -1.9(11) . . . . ? S1 C4 C5 S6 -177.7(5) . . . . ? C10 S5 C5 C4 179.5(9) . . . . ? C10 S5 C5 S6 -0.6(6) . . . . ? C11 S6 C5 C4 179.4(8) . . . . ? C11 S6 C5 S5 -0.6(6) . . . . ? C4 S1 C6 C7 -1.5(9) . . . . ? C4 S1 C6 S3 -177.2(6) . . . . ? C8 S3 C6 C7 -30.6(10) . . . . ? C8 S3 C6 S1 144.9(6) . . . . ? S1 C6 C7 S4 179.5(6) . . . . ? S3 C6 C7 S4 -5.0(15) . . . . ? S1 C6 C7 S2 1.0(11) . . . . ? S3 C6 C7 S2 176.5(5) . . . . ? C9 S4 C7 C6 12.1(12) . . . . ? C9 S4 C7 S2 -169.3(5) . . . . ? C4 S2 C7 C6 0.0(9) . . . . ? C4 S2 C7 S4 -178.8(5) . . . . ? C6 S3 C8 C9 66.7(8) . . . . ? S3 C8 C9 S4 -66.9(9) . . . . ? C7 S4 C9 C8 24.9(9) . . . . ? C5 S5 C10 C11 1.9(9) . . . . ? C5 S5 C10 S7 179.9(6) . . . . ? C14 S7 C10 C11 16.2(11) . . . . ? C14 S7 C10 S5 -161.6(6) . . . . ? S5 C10 C11 S6 -2.7(11) . . . . ? S7 C10 C11 S6 179.6(6) . . . . ? S5 C10 C11 S8 176.2(5) . . . . ? S7 C10 C11 S8 -1.5(15) . . . . ? C5 S6 C11 C10 1.9(9) . . . . ? C5 S6 C11 S8 -177.1(5) . . . . ? C13 S8 C11 C10 11.0(11) . . . . ? C13 S8 C11 S6 -170.1(6) . . . . ? C11 S8 C13 C14 -44.1(9) . . . . ? C17 S9 C16 C15 -171.5(9) . . . . ? C17 S9 C16 S10 13.0(6) . . . . ? C18 S10 C16 C15 171.5(9) . . . . ? C18 S10 C16 S9 -12.9(6) . . . . ? S8 C13 C14 S7 68.4(10) . . . . ? C10 S7 C14 C13 -48.4(8) . . . . ? S9 C16 C15 S14 -176.3(5) . . . . ? S10 C16 C15 S14 -1.1(12) . . . . ? S9 C16 C15 S13 2.4(13) . . . . ? S10 C16 C15 S13 177.7(5) . . . . ? C22 S14 C15 C16 -171.4(9) . . . . ? C22 S14 C15 S13 9.7(6) . . . . ? C21 S13 C15 C16 170.7(9) . . . . ? C21 S13 C15 S14 -10.4(6) . . . . ? C19 S11 C17 C18 -41.4(10) . . . . ? C19 S11 C17 S9 132.4(6) . . . . ? C16 S9 C17 C18 -8.3(8) . . . . ? C16 S9 C17 S11 177.4(6) . . . . ? S11 C17 C18 S10 174.4(5) . . . . ? S9 C17 C18 S10 0.6(11) . . . . ? S11 C17 C18 S12 -1.9(14) . . . . ? S9 C17 C18 S12 -175.7(5) . . . . ? C16 S10 C18 C17 7.4(8) . . . . ? C16 S10 C18 S12 -175.9(5) . . . . ? C20 S12 C18 C17 26.8(10) . . . . ? C20 S12 C18 S10 -149.7(6) . . . . ? C17 S11 C19 C20 67.1(9) . . . . ? S11 C19 C20 S12 -49.8(12) . . . . ? C18 S12 C20 C19 1.9(10) . . . . ? C15 S13 C21 C22 7.5(9) . . . . ? C15 S13 C21 S15 -172.1(5) . . . . ? C23 S15 C21 C22 14.6(11) . . . . ? C23 S15 C21 S13 -165.7(6) . . . . ? S13 C21 C22 S16 175.0(6) . . . . ? S15 C21 C22 S16 -5.4(16) . . . . ? S13 C21 C22 S14 -2.0(12) . . . . ? S15 C21 C22 S14 177.7(6) . . . . ? C24 S16 C22 C21 20.0(11) . . . . ? C24 S16 C22 S14 -163.0(5) . . . . ? C15 S14 C22 C21 -4.8(9) . . . . ? C15 S14 C22 S16 177.8(6) . . . . ? C21 S15 C23 C24 -46.1(8) . . . . ? S15 C23 C24 S16 71.2(9) . . . . ? C22 S16 C24 C23 -51.5(9) . . . . ? N01 C01 C02 C05 129.3(627) . . . . ? N01 C01 C02 C03 -47.4(635) . . . . ? C01 C02 C03 C04 177.0(11) . . . . ? C05 C02 C03 C04 -0.1(13) . . . . ? C02 C03 C04 C03 0.0(7) . . . 3_655 ? C01 C02 C05 C02 -176.6(15) . . . 3_655 ? C03 C02 C05 C02 0.0(6) . . . 3_655 ? _refine_diff_density_max 0.627 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.131 #=END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C53 H37 Cr N O13 S32' _chemical_formula_weight 1973.76 _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' 'O' 'O' 0.0106 0.0060 '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' 'Cr' 'Cr' 0.3209 0.6236 '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 10.278(3) _cell_length_b 20.130(4) _cell_length_c 35.078(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.040(9) _cell_angle_gamma 90.00 _cell_volume 7247.3(40) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 'All reflections from 10 deg phi rotation' _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Thick needle' _exptl_crystal_colour Dark _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method ? _exptl_crystal_F_000 4008 _exptl_absorpt_coefficient_mu 1.141 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST TV Area detector' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8640 _diffrn_reflns_av_R_equivalents 0.2393 _diffrn_reflns_av_sigmaI/netI 0.2055 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4281 _reflns_number_observed 2482 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Pflugrath, 1989)' _computing_cell_refinement MADNES _computing_data_reduction ABSURD _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics CAMERON _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 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^)+(0.0311P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4272 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_obs 0.0622 _refine_ls_wR_factor_all 0.1149 _refine_ls_wR_factor_obs 0.0945 _refine_ls_goodness_of_fit_all 0.841 _refine_ls_goodness_of_fit_obs 1.055 _refine_ls_restrained_S_all 0.941 _refine_ls_restrained_S_obs 1.055 _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 Cr1 Cr 0.0000 0.08374(7) 0.2500 0.0364(4) Uani 1 d S . S1 S -0.1152(2) 0.04397(8) -0.03743(5) 0.0364(5) Uani 1 d . . S2 S -0.3507(2) 0.11859(8) -0.06129(5) 0.0382(5) Uani 1 d . . S3 S 0.0204(2) 0.07306(8) -0.10802(5) 0.0414(5) Uani 1 d . . S4 S -0.2565(2) 0.15839(9) -0.13618(5) 0.0500(6) Uani 1 d . . S5 S -0.2407(2) 0.01210(8) 0.04341(5) 0.0361(5) Uani 1 d . . S6 S -0.4733(2) 0.08832(9) 0.01870(5) 0.0387(5) Uani 1 d . . S7 S -0.3286(2) -0.01845(9) 0.12023(5) 0.0459(5) Uani 1 d . . S8 S -0.6076(2) 0.06989(10) 0.08938(6) 0.0544(6) Uani 1 d . . S9 S -0.5423(2) 0.25363(8) 0.07394(5) 0.0393(5) Uani 1 d . . S10 S -0.7802(2) 0.32612(8) 0.04991(5) 0.0376(5) Uani 1 d . . S11 S -0.6200(2) 0.22458(9) 0.15119(5) 0.0538(6) Uani 1 d . . S12 S -0.9088(2) 0.30657(9) 0.12202(6) 0.0480(6) Uani 1 d . . S13 S -0.4233(2) 0.28558(8) -0.00816(5) 0.0385(5) Uani 1 d . . S14 S -0.6640(2) 0.35673(8) -0.03105(5) 0.0365(5) Uani 1 d . . S15 S -0.2957(2) 0.30764(9) -0.07968(5) 0.0446(5) Uani 1 d . . S16 S -0.5860(2) 0.39020(9) -0.10828(5) 0.0429(5) Uani 1 d . . N1 N 0.0000 -0.1260(5) 0.2500 0.097(4) Uani 1 d S . O1 O 0.1490(5) 0.0728(2) 0.21723(12) 0.0427(13) Uani 1 d . . O2 O -0.0967(4) 0.0188(2) 0.21813(12) 0.0410(12) Uani 1 d . . O3 O -0.0804(4) 0.1585(2) 0.22052(13) 0.0470(13) Uani 1 d . . O4 O 0.3141(5) 0.0012(3) 0.20980(14) 0.063(2) Uani 1 d . . O5 O -0.2771(5) -0.0437(3) 0.2167(2) 0.061(2) Uani 1 d . . O6 O -0.0922(5) 0.2689(2) 0.2200(2) 0.067(2) Uani 1 d . . O7 O -0.5000 -0.0981(4) 0.2500 0.087(3) Uani 1 d S . C1 C 0.2244(7) 0.0247(4) 0.2277(2) 0.041(2) Uani 1 d . . C2 C -0.2005(8) -0.0033(3) 0.2325(2) 0.041(2) Uani 1 d . . C3 C -0.0497(7) 0.2166(4) 0.2328(2) 0.044(2) Uani 1 d . . C4 C -0.2666(6) 0.0736(3) -0.0256(2) 0.031(2) Uani 1 d . . C5 C -0.1165(6) 0.0847(3) -0.0818(2) 0.033(2) Uani 1 d . . C6 C -0.2245(6) 0.1183(3) -0.0929(2) 0.030(2) Uani 1 d . . C7 C -0.0637(9) 0.0696(4) -0.1548(2) 0.085(3) Uani 1 d . . H7A H 0.0012(9) 0.0633(4) -0.1735(2) 0.103 Uiso 1 calc R . H7B H -0.1189(9) 0.0305(4) -0.1556(2) 0.103 Uiso 1 calc R . C8 C -0.1404(8) 0.1238(4) -0.1662(2) 0.067(3) Uani 1 d . . H8A H -0.1872(8) 0.1114(4) -0.1899(2) 0.080 Uiso 1 calc R . H8B H -0.0814(8) 0.1594(4) -0.1724(2) 0.080 Uiso 1 calc R . C9 C -0.3195(6) 0.0593(3) 0.0077(2) 0.031(2) Uani 1 d . . C10 C -0.3637(6) 0.0191(3) 0.0758(2) 0.027(2) Uani 1 d . . C11 C -0.4688(6) 0.0541(3) 0.0647(2) 0.031(2) Uani 1 d . . C12 C -0.4751(8) -0.0066(5) 0.1431(2) 0.095(4) Uani 1 d . . H12A H -0.5312(8) -0.0439(5) 0.1363(2) 0.114 Uiso 1 calc R . H12B H -0.4545(8) -0.0098(5) 0.1704(2) 0.114 Uiso 1 calc R . C13 C -0.5484(9) 0.0500(4) 0.1373(2) 0.085(3) Uani 1 d . . H13A H -0.4966(9) 0.0873(4) 0.1469(2) 0.101 Uiso 1 calc R . H13B H -0.6232(9) 0.0467(4) 0.1529(2) 0.101 Uiso 1 calc R . C14 C -0.6263(6) 0.2989(3) 0.0381(2) 0.030(2) Uani 1 d . . C15 C -0.6647(7) 0.2596(3) 0.1065(2) 0.033(2) Uani 1 d . . C16 C -0.7725(7) 0.2918(3) 0.0956(2) 0.034(2) Uani 1 d . . C17 C -0.7653(8) 0.2377(4) 0.1767(2) 0.062(2) Uani 1 d . . H17A H -0.8262(8) 0.2021(4) 0.1703(2) 0.074 Uiso 1 calc R . H17B H -0.7427(8) 0.2348(4) 0.2039(2) 0.074 Uiso 1 calc R . C18 C -0.8313(8) 0.3021(4) 0.1689(2) 0.066(3) Uani 1 d . . H18A H -0.7676(8) 0.3376(4) 0.1718(2) 0.079 Uiso 1 calc R . H18B H -0.8961(8) 0.3091(4) 0.1876(2) 0.079 Uiso 1 calc R . C19 C -0.5767(6) 0.3123(3) 0.0043(2) 0.031(2) Uani 1 d . . C20 C -0.4340(6) 0.3208(3) -0.0539(2) 0.030(2) Uani 1 d . . C21 C -0.5429(6) 0.3532(3) -0.0647(2) 0.031(2) Uani 1 d . . C22 C -0.3550(7) 0.3311(3) -0.1273(2) 0.041(2) Uani 1 d . . H22A H -0.2811(7) 0.3352(3) -0.1432(2) 0.050 Uiso 1 calc R . H22B H -0.4098(7) 0.2956(3) -0.1378(2) 0.050 Uiso 1 calc R . C23 C -0.4303(6) 0.3943(3) -0.1294(2) 0.039(2) Uani 1 d . . H23A H -0.4442(6) 0.4068(3) -0.1560(2) 0.047 Uiso 1 calc R . H23B H -0.3787(6) 0.4289(3) -0.1168(2) 0.047 Uiso 1 calc R . C24 C 0.0000 -0.1831(7) 0.2500 0.067(4) Uani 1 d S . C25 C 0.0000 -0.2522(5) 0.2500 0.053(3) Uani 1 d S . C26 C 0.0934(8) -0.2860(4) 0.2303(2) 0.066(2) Uani 1 d . . H26 H 0.1563(8) -0.2631(4) 0.2174(2) 0.079 Uiso 1 calc R . C27 C 0.0899(9) -0.3556(5) 0.2302(3) 0.092(3) Uani 1 d . . H27 H 0.1497(9) -0.3792(5) 0.2166(3) 0.110 Uiso 1 calc R . C28 C 0.0000 -0.3894(7) 0.2500 0.097(6) Uani 1 d S . H28 H 0.0000 -0.4356(7) 0.2500 0.116 Uiso 1 calc SR . 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 Cr1 0.0468(11) 0.0363(10) 0.0267(10) 0.000 0.0069(8) 0.000 S1 0.0328(11) 0.0427(11) 0.0344(11) 0.0052(7) 0.0076(9) 0.0099(8) S2 0.0332(12) 0.0551(12) 0.0271(11) 0.0065(8) 0.0082(9) 0.0150(9) S3 0.0339(12) 0.0468(12) 0.0450(12) 0.0027(8) 0.0164(10) 0.0078(9) S4 0.0628(15) 0.0575(13) 0.0312(12) 0.0127(8) 0.0164(11) 0.0228(11) S5 0.0311(11) 0.0474(11) 0.0305(11) 0.0079(7) 0.0071(9) 0.0117(8) S6 0.0322(11) 0.0552(12) 0.0291(11) 0.0078(8) 0.0052(9) 0.0145(9) S7 0.0340(12) 0.0601(12) 0.0445(13) 0.0254(9) 0.0113(10) 0.0084(9) S8 0.0376(13) 0.086(2) 0.0407(13) 0.0192(10) 0.0157(11) 0.0257(11) S9 0.0354(11) 0.0466(11) 0.0362(12) 0.0078(8) 0.0042(10) 0.0102(9) S10 0.0314(11) 0.0458(11) 0.0360(12) 0.0065(8) 0.0054(9) 0.0068(8) S11 0.0663(15) 0.0639(14) 0.0307(12) 0.0112(9) -0.0014(11) 0.0071(11) S12 0.0459(13) 0.0476(12) 0.0528(14) 0.0059(9) 0.0245(11) 0.0053(9) S13 0.0311(12) 0.0515(12) 0.0333(12) 0.0046(8) 0.0056(9) 0.0105(9) S14 0.0302(11) 0.0478(11) 0.0323(11) 0.0079(8) 0.0082(9) 0.0083(8) S15 0.0332(12) 0.0594(13) 0.0421(13) 0.0030(9) 0.0112(10) 0.0109(9) S16 0.0381(12) 0.0561(12) 0.0354(12) 0.0125(8) 0.0091(10) 0.0075(9) N1 0.136(11) 0.071(8) 0.087(9) 0.000 0.045(8) 0.000 O1 0.048(3) 0.048(3) 0.033(3) 0.002(2) 0.009(3) -0.010(3) O2 0.044(3) 0.040(3) 0.040(3) -0.006(2) 0.017(3) -0.011(2) O3 0.060(4) 0.042(3) 0.040(3) 0.006(2) 0.006(3) 0.004(3) O4 0.056(4) 0.085(4) 0.052(4) -0.008(3) 0.027(3) 0.002(3) O5 0.050(4) 0.066(4) 0.069(4) -0.008(3) 0.007(3) -0.017(3) O6 0.075(4) 0.042(4) 0.085(4) 0.015(3) 0.010(3) 0.009(3) O7 0.091(6) 0.073(6) 0.100(7) 0.000 0.034(6) 0.000 C1 0.041(5) 0.050(5) 0.032(5) -0.006(4) 0.007(4) -0.007(4) C2 0.045(5) 0.046(5) 0.032(5) -0.001(3) 0.007(4) -0.001(4) C3 0.057(6) 0.036(5) 0.042(5) 0.006(3) 0.019(4) 0.003(4) C4 0.028(4) 0.036(4) 0.030(4) -0.003(3) 0.003(4) 0.004(3) C5 0.034(5) 0.034(4) 0.033(4) -0.006(3) 0.011(4) 0.003(3) C6 0.033(4) 0.033(4) 0.024(4) -0.004(3) 0.010(3) 0.007(3) C7 0.108(8) 0.109(8) 0.042(6) -0.013(5) 0.030(6) 0.040(6) C8 0.075(7) 0.098(7) 0.028(5) -0.005(4) 0.005(5) 0.028(5) C9 0.025(4) 0.031(4) 0.036(5) -0.001(3) -0.000(3) 0.008(3) C10 0.024(4) 0.037(4) 0.022(4) 0.001(3) 0.003(3) 0.001(3) C11 0.031(4) 0.043(4) 0.020(4) 0.004(3) 0.007(3) 0.004(3) C12 0.092(8) 0.149(9) 0.048(6) 0.030(6) 0.042(6) 0.052(7) C13 0.126(9) 0.089(7) 0.043(6) 0.023(4) 0.036(6) 0.062(6) C14 0.024(4) 0.034(4) 0.032(4) -0.002(3) -0.003(3) 0.000(3) C15 0.042(5) 0.033(4) 0.026(4) -0.002(3) 0.010(4) 0.000(3) C16 0.039(5) 0.034(4) 0.030(4) -0.002(3) 0.010(4) 0.000(3) C17 0.075(6) 0.086(7) 0.024(5) 0.010(4) 0.001(5) -0.016(5) C18 0.066(6) 0.067(6) 0.065(7) -0.023(4) 0.025(5) -0.012(5) C19 0.029(4) 0.032(4) 0.032(4) 0.001(3) 0.004(4) 0.004(3) C20 0.034(5) 0.033(4) 0.024(4) -0.000(3) 0.007(4) 0.008(3) C21 0.026(4) 0.037(4) 0.032(4) -0.008(3) 0.008(4) -0.006(3) C22 0.041(5) 0.043(5) 0.042(5) 0.002(3) 0.017(4) 0.007(3) C23 0.041(5) 0.041(5) 0.037(4) -0.002(3) 0.016(4) -0.007(4) C24 0.105(11) 0.052(8) 0.045(8) 0.000 0.016(8) 0.000 C25 0.066(9) 0.039(8) 0.052(8) 0.000 -0.017(7) 0.000 C26 0.066(6) 0.073(7) 0.057(6) -0.000(4) -0.019(5) 0.019(5) C27 0.082(8) 0.056(8) 0.130(10) -0.021(6) -0.058(7) 0.024(6) C28 0.078(12) 0.041(10) 0.166(17) 0.000 -0.048(12) 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 Cr1 O2 1.957(4) . ? Cr1 O2 1.957(4) 2 ? Cr1 O1 1.976(4) . ? Cr1 O1 1.976(4) 2 ? Cr1 O3 1.982(5) 2 ? Cr1 O3 1.982(5) . ? S1 C4 1.737(6) . ? S1 C5 1.759(7) . ? S2 C4 1.737(7) . ? S2 C6 1.751(6) . ? S3 C5 1.738(6) . ? S3 C7 1.814(9) . ? S4 C6 1.734(7) . ? S4 C8 1.776(7) . ? S5 C9 1.736(7) . ? S5 C10 1.750(5) . ? S6 C9 1.747(6) . ? S6 C11 1.752(6) . ? S7 C10 1.753(6) . ? S7 C12 1.761(7) . ? S8 C11 1.737(6) . ? S8 C13 1.802(9) . ? S9 C14 1.744(7) . ? S9 C15 1.748(6) . ? S10 C16 1.743(7) . ? S10 C14 1.745(6) . ? S11 C15 1.757(7) . ? S11 C17 1.801(7) . ? S12 C16 1.746(6) . ? S12 C18 1.790(9) . ? S13 C19 1.743(6) . ? S13 C20 1.751(6) . ? S14 C19 1.738(7) . ? S14 C21 1.762(6) . ? S15 C20 1.746(6) . ? S15 C22 1.810(7) . ? S16 C21 1.735(7) . ? S16 C23 1.801(5) . ? N1 C24 1.149(13) . ? O1 C1 1.282(8) . ? O2 C2 1.284(7) . ? O3 C3 1.280(7) . ? O4 C1 1.235(7) . ? O5 C2 1.243(8) . ? O6 C3 1.217(7) . ? C1 C2 1.538(9) 2 ? C2 C1 1.538(9) 2 ? C3 C3 1.537(15) 2 ? C4 C9 1.348(8) . ? C5 C6 1.340(8) . ? C7 C8 1.393(10) . ? C10 C11 1.331(8) . ? C12 C13 1.375(9) . ? C14 C19 1.344(7) . ? C15 C16 1.323(9) . ? C17 C18 1.483(10) . ? C20 C21 1.334(9) . ? C22 C23 1.489(8) . ? C24 C25 1.391(15) . ? C25 C26 1.391(8) . ? C25 C26 1.391(8) 2 ? C26 C27 1.401(12) . ? C27 C28 1.365(10) . ? C28 C27 1.365(10) 2 ? 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 O2 Cr1 O2 96.1(3) . 2 ? O2 Cr1 O1 88.8(2) . . ? O2 Cr1 O1 82.6(2) 2 . ? O2 Cr1 O1 82.6(2) . 2 ? O2 Cr1 O1 88.8(2) 2 2 ? O1 Cr1 O1 167.2(3) . 2 ? O2 Cr1 O3 172.2(2) . 2 ? O2 Cr1 O3 91.4(2) 2 2 ? O1 Cr1 O3 94.2(2) . 2 ? O1 Cr1 O3 95.5(2) 2 2 ? O2 Cr1 O3 91.4(2) . . ? O2 Cr1 O3 172.2(2) 2 . ? O1 Cr1 O3 95.5(2) . . ? O1 Cr1 O3 94.2(2) 2 . ? O3 Cr1 O3 81.2(3) 2 . ? C4 S1 C5 94.9(3) . . ? C4 S2 C6 95.6(3) . . ? C5 S3 C7 97.1(3) . . ? C6 S4 C8 103.6(3) . . ? C9 S5 C10 95.6(3) . . ? C9 S6 C11 95.2(3) . . ? C10 S7 C12 101.9(4) . . ? C11 S8 C13 100.3(4) . . ? C14 S9 C15 95.1(3) . . ? C16 S10 C14 95.5(3) . . ? C15 S11 C17 101.6(3) . . ? C16 S12 C18 98.5(4) . . ? C19 S13 C20 95.2(3) . . ? C19 S14 C21 95.8(3) . . ? C20 S15 C22 101.3(3) . . ? C21 S16 C23 101.1(3) . . ? C1 O1 Cr1 113.2(4) . . ? C2 O2 Cr1 114.5(4) . . ? C3 O3 Cr1 115.4(5) . . ? O4 C1 O1 126.9(7) . . ? O4 C1 C2 118.7(8) . 2 ? O1 C1 C2 114.4(6) . 2 ? O5 C2 O2 124.8(6) . . ? O5 C2 C1 121.2(6) . 2 ? O2 C2 C1 114.0(7) . 2 ? O6 C3 O3 126.0(7) . . ? O6 C3 C3 120.0(5) . 2 ? O3 C3 C3 114.0(4) . 2 ? C9 C4 S2 121.9(5) . . ? C9 C4 S1 122.8(5) . . ? S2 C4 S1 115.1(3) . . ? C6 C5 S3 126.6(5) . . ? C6 C5 S1 117.4(4) . . ? S3 C5 S1 115.9(4) . . ? C5 C6 S4 127.3(5) . . ? C5 C6 S2 116.6(5) . . ? S4 C6 S2 116.1(4) . . ? C8 C7 S3 117.8(6) . . ? C7 C8 S4 121.5(6) . . ? C4 C9 S5 123.2(5) . . ? C4 C9 S6 122.1(5) . . ? S5 C9 S6 114.7(3) . . ? C11 C10 S5 117.1(5) . . ? C11 C10 S7 127.9(4) . . ? S5 C10 S7 114.9(4) . . ? C10 C11 S8 128.8(5) . . ? C10 C11 S6 117.3(4) . . ? S8 C11 S6 113.9(4) . . ? C13 C12 S7 121.3(6) . . ? C12 C13 S8 118.5(6) . . ? C19 C14 S9 123.0(5) . . ? C19 C14 S10 122.5(5) . . ? S9 C14 S10 114.4(3) . . ? C16 C15 S9 117.8(5) . . ? C16 C15 S11 129.0(5) . . ? S9 C15 S11 113.1(4) . . ? C15 C16 S10 117.2(5) . . ? C15 C16 S12 127.8(5) . . ? S10 C16 S12 115.0(4) . . ? C18 C17 S11 114.7(5) . . ? C17 C18 S12 113.1(5) . . ? C14 C19 S14 121.8(5) . . ? C14 C19 S13 123.3(5) . . ? S14 C19 S13 114.8(3) . . ? C21 C20 S15 128.3(5) . . ? C21 C20 S13 118.1(4) . . ? S15 C20 S13 113.6(4) . . ? C20 C21 S16 129.3(4) . . ? C20 C21 S14 116.1(5) . . ? S16 C21 S14 114.6(4) . . ? C23 C22 S15 114.7(5) . . ? C22 C23 S16 114.3(4) . . ? N1 C24 C25 180.000(1) . . ? C26 C25 C26 121.4(12) . 2 ? C26 C25 C24 119.3(6) . . ? C26 C25 C24 119.3(6) 2 . ? C25 C26 C27 118.1(9) . . ? C28 C27 C26 121.0(11) . . ? C27 C28 C27 120.3(14) . 2 ? _refine_diff_density_max 0.657 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.114