Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 1145 loop_ _publ_author_name 'Samina Rashid' 'Scott T. Turner' 'Peter Day' 'Judith A. K. Howard' 'Philippe Guionneau' 'Eric. J. L. Innes' 'Frank E. Mabbs' 'Robin J. Clark' 'Steven Firth' 'Tim Biggs' _publ_contact_author_name 'Dr Samina Rashid' _publ_contact_author_address ; Davy-Faraday Research Laboratory The Royal Institution of Great Britain 21 Albemarle Street London W1X 4BS UNITED KINGDOM ; _publ_contact_author_email samina@ri.ac.uk data_sad _database_code_CSD 157874 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ET4NH4Fe(OX)3C6H5NO2 _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H20.50 Fe0.50 N O7 S16' _chemical_formula_weight 999.82 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.2732(2) _cell_length_b 19.9494(3) _cell_length_c 35.0304(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.9690(10) _cell_angle_gamma 90.00 _cell_volume 7169.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method ? _exptl_crystal_F_000 4068 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8140 _exptl_absorpt_correction_T_max 0.9488 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30838 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8238 _reflns_number_observed 6799 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 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^)+(0.0124P)^2^+25.2618P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8230 _refine_ls_number_parameters 462 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0527 _refine_ls_R_factor_obs 0.0378 _refine_ls_wR_factor_all 0.0800 _refine_ls_wR_factor_obs 0.0724 _refine_ls_goodness_of_fit_all 1.130 _refine_ls_goodness_of_fit_obs 1.141 _refine_ls_restrained_S_all 1.138 _refine_ls_restrained_S_obs 1.141 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_mean 0.001 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 Fe1 Fe 1.0000 0.07500(3) -0.2500 0.01621(12) Uani 1 d S . S8 S 1.25701(6) 0.48968(4) 0.04437(2) 0.01469(14) Uani 1 d . . S6 S 1.02466(6) 0.41242(4) 0.01919(2) 0.01561(14) Uani 1 d . . S7 S 1.38660(6) 0.45692(3) -0.03611(2) 0.01479(14) Uani 1 d . . S16 S 0.78373(6) 0.32548(3) -0.04888(2) 0.01511(14) Uani 1 d . . S5 S 1.15122(6) 0.38130(4) -0.06070(2) 0.01548(14) Uani 1 d . . S14 S 0.42118(6) 0.28660(4) 0.00751(2) 0.01557(14) Uani 1 d . . S4 S 1.52663(6) 0.42537(4) -0.10629(2) 0.01652(14) Uani 1 d . . S15 S 0.66445(6) 0.35664(4) 0.03125(2) 0.01488(14) Uani 1 d . . S13 S 0.54535(6) 0.25334(3) -0.07480(2) 0.01508(14) Uani 1 d . . S11 S 0.29081(6) 0.30907(4) 0.07897(2) 0.01797(15) Uani 1 d . . S10 S 0.91908(7) 0.30488(4) -0.12029(2) 0.01754(15) Uani 1 d . . S2 S 1.16840(6) 0.51937(4) 0.12171(2) 0.01836(15) Uani 1 d . . S12 S 0.58513(6) 0.38987(4) 0.10901(2) 0.01706(14) Uani 1 d . . S3 S 0.88677(7) 0.43080(4) 0.08970(2) 0.0227(2) Uani 1 d . . S1 S 1.24998(7) 0.33821(4) -0.13474(2) 0.0199(2) Uani 1 d . . S9 S 0.62855(7) 0.22486(4) -0.15205(2) 0.0203(2) Uani 1 d . . C10 C 1.2807(3) 0.38016(14) -0.09148(7) 0.0144(5) Uani 1 d . . C19 C 0.7805(3) 0.29064(13) -0.09482(7) 0.0138(5) Uani 1 d . . C13 C 0.7760(3) 0.2382(2) -0.17744(8) 0.0240(6) Uani 1 d . . H13A H 0.8360(3) 0.2017(2) -0.17143(8) 0.029 Uiso 1 calc R . H13B H 0.7541(3) 0.2367(2) -0.20470(8) 0.029 Uiso 1 calc R . C8 C 1.3892(3) 0.41427(13) -0.07978(7) 0.0134(5) Uani 1 d . . C20 C 0.4311(3) 0.32135(14) 0.05368(7) 0.0142(5) Uani 1 d . . C9 C 1.1339(3) 0.48214(14) 0.07708(7) 0.0138(5) Uani 1 d . . C18 C 0.6699(3) 0.25905(13) -0.10709(7) 0.0134(5) Uani 1 d . . C17 C 0.5763(3) 0.31203(14) -0.00427(7) 0.0142(5) Uani 1 d . . C16 C 0.5437(3) 0.35322(14) 0.06468(7) 0.0141(5) Uani 1 d . . C5 C 1.2340(2) 0.42730(13) -0.02485(7) 0.0135(5) Uani 1 d . . C15 C 0.6280(2) 0.29821(13) -0.03841(7) 0.0137(5) Uani 1 d . . C6 C 1.0266(3) 0.44702(14) 0.06497(7) 0.0148(5) Uani 1 d . . C7 C 1.1791(2) 0.44106(13) 0.00909(7) 0.0131(5) Uani 1 d . . C4 C 1.0115(3) 0.5160(2) 0.14253(8) 0.0211(6) Uani 1 d . . H4A H 1.0227(3) 0.5266(2) 0.16951(8) 0.025 Uiso 1 calc R . H4B H 0.9555(3) 0.5500(2) 0.13060(8) 0.025 Uiso 1 calc R . C14 C 0.4261(3) 0.39740(14) 0.12854(8) 0.0158(5) Uani 1 d . . H14A H 0.4373(3) 0.41188(14) 0.15494(8) 0.019 Uiso 1 calc R . H14B H 0.3774(3) 0.43197(14) 0.11455(8) 0.019 Uiso 1 calc R . C2 C 1.3708(3) 0.3710(2) -0.16561(9) 0.0314(8) Uani 1 d . . H2A H 1.4355(3) 0.3363(2) -0.16894(9) 0.038 Uiso 1 calc R . H2B H 1.3283(3) 0.3795(2) -0.19050(9) 0.038 Uiso 1 calc R . C12 C 0.8440(3) 0.3039(2) -0.16806(8) 0.0230(6) Uani 1 d . . H12A H 0.7811(3) 0.3402(2) -0.17060(8) 0.028 Uiso 1 calc R . H12B H 0.9103(3) 0.3117(2) -0.18630(8) 0.028 Uiso 1 calc R . C3 C 0.9450(3) 0.4488(2) 0.13824(8) 0.0234(6) Uani 1 d . . H3A H 0.8719(3) 0.4476(2) 0.15467(8) 0.028 Uiso 1 calc R . H3B H 1.0058(3) 0.4140(2) 0.14677(8) 0.028 Uiso 1 calc R . C11 C 0.3470(3) 0.33348(14) 0.12709(8) 0.0184(6) Uani 1 d . . H11A H 0.2720(3) 0.33925(14) 0.14247(8) 0.022 Uiso 1 calc R . H11B H 0.3997(3) 0.29753(14) 0.13837(8) 0.022 Uiso 1 calc R . C1 C 1.4402(3) 0.4329(2) -0.15302(8) 0.0316(8) Uani 1 d . . H1A H 1.3775(3) 0.4691(2) -0.15205(8) 0.038 Uiso 1 calc R . H1B H 1.5023(3) 0.4447(2) -0.17184(8) 0.038 Uiso 1 calc R . N1 N 1.5000 0.3176(2) -0.2500 0.0316(9) Uani 1 d S . C27 C 1.5000 0.2435(2) -0.2500 0.0261(10) Uani 1 d S . C24 C 1.5000 0.1079(3) -0.2500 0.052(2) Uani 1 d S . H24 H 1.5000 0.0613(3) -0.2500 0.062 Uiso 2.00 calc SPR . O30 O 1.6057(3) 0.34618(13) -0.24577(7) 0.0430(7) Uani 1 d . . C26 C 1.4001(3) 0.2113(2) -0.23237(9) 0.0309(8) Uani 1 d . . H26 H 1.3343(3) 0.2351(2) -0.22114(9) 0.037 Uiso 1 calc R . C25 C 1.4024(4) 0.1417(2) -0.23221(12) 0.0423(10) Uani 1 d . . H25 H 1.3384(4) 0.1179(2) -0.22015(12) 0.051 Uiso 1 calc R . O2 O 1.1473(2) 0.05776(10) -0.28428(5) 0.0193(4) Uani 1 d . . O1 O 0.8929(2) 0.01257(10) -0.28395(5) 0.0180(4) Uani 1 d . . O3 O 0.9231(2) 0.15256(10) -0.28048(6) 0.0231(5) Uani 1 d . . O6 O 1.3155(2) -0.01248(11) -0.29036(6) 0.0293(5) Uani 1 d . . O5 O 0.7068(2) -0.04554(11) -0.28648(6) 0.0228(4) Uani 1 d . . O4 O 0.9074(2) 0.26449(11) -0.28065(7) 0.0321(5) Uani 1 d . . C22 C 0.7889(3) -0.00996(14) -0.26983(8) 0.0162(5) Uani 1 d . . C21 C 1.2293(3) 0.01265(15) -0.27219(8) 0.0191(6) Uani 1 d . . C23 C 0.9507(3) 0.2113(2) -0.26783(8) 0.0229(6) Uani 1 d . . N2 N 1.0000 0.3938(2) -0.2500 0.0313(9) Uani 1 d SD . H22A H 1.0000 0.3391(5) -0.2500 0.050 Uiso 1 d SD . H22B H 0.9157(24) 0.4176(17) -0.2386(10) 0.050 Uiso 1 d D . 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 Fe1 0.0202(3) 0.0164(3) 0.0122(3) 0.000 0.0025(2) 0.000 S8 0.0123(3) 0.0193(4) 0.0126(3) -0.0035(2) 0.0018(2) -0.0039(3) S6 0.0129(3) 0.0219(4) 0.0121(3) -0.0036(3) 0.0014(2) -0.0049(3) S7 0.0128(3) 0.0178(4) 0.0138(3) -0.0023(3) 0.0016(2) -0.0042(3) S16 0.0125(3) 0.0184(3) 0.0145(3) -0.0036(3) 0.0015(2) -0.0034(3) S5 0.0126(3) 0.0220(4) 0.0120(3) -0.0028(3) 0.0022(2) -0.0052(3) S14 0.0129(3) 0.0200(4) 0.0138(3) -0.0024(3) 0.0013(2) -0.0035(3) S4 0.0131(3) 0.0178(3) 0.0191(3) 0.0002(3) 0.0055(2) -0.0030(3) S15 0.0115(3) 0.0199(4) 0.0134(3) -0.0036(3) 0.0023(2) -0.0032(3) S13 0.0123(3) 0.0190(4) 0.0139(3) -0.0024(3) 0.0010(2) -0.0037(3) S11 0.0128(3) 0.0239(4) 0.0175(3) -0.0020(3) 0.0040(2) -0.0049(3) S10 0.0148(3) 0.0195(4) 0.0189(3) -0.0014(3) 0.0060(3) -0.0021(3) S2 0.0123(3) 0.0257(4) 0.0174(3) -0.0106(3) 0.0027(2) -0.0025(3) S12 0.0135(3) 0.0231(4) 0.0147(3) -0.0054(3) 0.0020(2) -0.0023(3) S3 0.0158(3) 0.0352(4) 0.0178(3) -0.0095(3) 0.0062(3) -0.0112(3) S1 0.0232(4) 0.0235(4) 0.0133(3) -0.0048(3) 0.0048(3) -0.0078(3) S9 0.0219(4) 0.0257(4) 0.0131(3) -0.0046(3) -0.0006(3) -0.0028(3) C10 0.0152(13) 0.0164(14) 0.0119(12) -0.0005(10) 0.0042(10) -0.0015(11) C19 0.0154(13) 0.0146(13) 0.0116(12) -0.0009(10) 0.0023(10) 0.0007(11) C13 0.024(2) 0.033(2) 0.0144(13) -0.0036(12) 0.0030(11) 0.0044(14) C8 0.0146(13) 0.0128(13) 0.0129(12) 0.0015(10) 0.0031(10) -0.0006(10) C20 0.0140(13) 0.0155(14) 0.0133(12) 0.0010(10) 0.0028(10) -0.0001(11) C9 0.0130(12) 0.0162(14) 0.0124(12) -0.0027(10) 0.0025(10) 0.0006(10) C18 0.0158(13) 0.0134(13) 0.0113(12) 0.0010(10) 0.0015(10) 0.0009(10) C17 0.0131(12) 0.0148(13) 0.0146(12) 0.0008(10) -0.0005(10) -0.0007(10) C16 0.0143(13) 0.0159(14) 0.0123(12) -0.0014(10) 0.0021(10) 0.0018(11) C5 0.0124(12) 0.0157(13) 0.0121(12) -0.0001(10) -0.0014(9) -0.0031(10) C15 0.0127(12) 0.0133(13) 0.0148(12) -0.0010(10) -0.0008(10) -0.0022(10) C6 0.0138(13) 0.0172(14) 0.0136(12) -0.0024(10) 0.0025(10) -0.0018(11) C7 0.0116(12) 0.0155(13) 0.0117(12) -0.0007(10) -0.0022(9) -0.0011(10) C4 0.0170(14) 0.028(2) 0.0191(14) -0.0056(12) 0.0043(11) -0.0013(12) C14 0.0127(13) 0.0168(14) 0.0183(13) -0.0017(11) 0.0039(10) 0.0021(11) C2 0.028(2) 0.048(2) 0.0182(15) 0.0026(14) 0.0040(12) -0.009(2) C12 0.0228(15) 0.027(2) 0.0191(14) 0.0067(12) 0.0047(11) 0.0025(13) C3 0.026(2) 0.028(2) 0.0166(14) -0.0051(12) 0.0039(12) -0.0078(13) C11 0.0200(14) 0.0208(15) 0.0151(13) 0.0000(11) 0.0064(11) -0.0014(12) C1 0.039(2) 0.038(2) 0.0181(15) 0.0039(14) 0.0053(13) -0.012(2) N1 0.051(3) 0.024(2) 0.020(2) 0.000 0.000(2) 0.000 C27 0.036(3) 0.018(2) 0.023(2) 0.000 -0.014(2) 0.000 C24 0.047(3) 0.011(2) 0.094(5) 0.000 -0.041(3) 0.000 O30 0.060(2) 0.0296(14) 0.0395(14) -0.0020(11) 0.0012(13) -0.0155(13) C26 0.030(2) 0.030(2) 0.031(2) 0.0029(14) -0.0172(14) -0.0011(14) C25 0.037(2) 0.029(2) 0.058(2) 0.011(2) -0.026(2) -0.010(2) O2 0.0221(10) 0.0223(11) 0.0139(9) 0.0008(8) 0.0047(8) -0.0027(9) O1 0.0188(10) 0.0218(11) 0.0138(9) -0.0020(8) 0.0035(7) -0.0020(8) O3 0.0311(12) 0.0190(11) 0.0191(10) 0.0018(8) 0.0011(9) 0.0035(9) O6 0.0286(12) 0.0335(13) 0.0271(11) -0.0003(10) 0.0146(9) 0.0037(10) O5 0.0193(10) 0.0280(12) 0.0211(10) 0.0025(9) 0.0004(8) -0.0019(9) O4 0.0377(13) 0.0206(12) 0.0391(13) 0.0077(10) 0.0126(11) 0.0052(10) C22 0.0169(13) 0.0147(14) 0.0170(13) 0.0017(11) 0.0014(10) 0.0049(11) C21 0.0201(14) 0.022(2) 0.0152(13) -0.0029(11) 0.0046(11) -0.0067(12) C23 0.028(2) 0.022(2) 0.0208(15) 0.0043(12) 0.0131(12) 0.0032(13) N2 0.031(2) 0.015(2) 0.051(3) 0.000 0.024(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 Fe1 O2 2.010(2) 2_754 ? Fe1 O2 2.010(2) . ? Fe1 O1 2.010(2) 2_754 ? Fe1 O1 2.010(2) . ? Fe1 O3 2.018(2) 2_754 ? Fe1 O3 2.018(2) . ? S8 C7 1.734(3) . ? S8 C9 1.757(3) . ? S6 C7 1.740(3) . ? S6 C6 1.745(3) . ? S7 C5 1.740(3) . ? S7 C8 1.752(3) . ? S16 C15 1.746(3) . ? S16 C19 1.752(3) . ? S5 C5 1.741(3) . ? S5 C10 1.755(3) . ? S14 C17 1.742(3) . ? S14 C20 1.758(3) . ? S4 C8 1.743(3) . ? S4 C1 1.828(3) . ? S15 C17 1.745(3) . ? S15 C16 1.750(3) . ? S13 C15 1.742(3) . ? S13 C18 1.755(3) . ? S11 C20 1.748(3) . ? S11 C11 1.820(3) . ? S10 C19 1.742(3) . ? S10 C12 1.806(3) . ? S2 C9 1.750(3) . ? S2 C4 1.804(3) . ? S12 C16 1.749(3) . ? S12 C14 1.810(3) . ? S3 C6 1.746(3) . ? S3 C3 1.809(3) . ? S1 C10 1.745(3) . ? S1 C2 1.810(3) . ? S9 C18 1.748(3) . ? S9 C13 1.815(3) . ? C10 C8 1.352(4) . ? C19 C18 1.350(4) . ? C13 C12 1.514(4) . ? C20 C16 1.358(4) . ? C9 C6 1.355(4) . ? C17 C15 1.362(4) . ? C5 C7 1.369(3) . ? C4 C3 1.508(4) . ? C14 C11 1.511(4) . ? C2 C1 1.481(5) . ? N1 O30 1.229(3) . ? N1 O30 1.229(3) 2_854 ? N1 C27 1.477(6) . ? C27 C26 1.384(4) . ? C27 C26 1.384(4) 2_854 ? C24 C25 1.384(5) . ? C24 C25 1.384(5) 2_854 ? C26 C25 1.387(5) . ? O2 C21 1.289(4) . ? O1 C22 1.281(3) . ? O3 C23 1.280(4) . ? O6 C21 1.224(3) . ? O5 C22 1.227(3) . ? O4 C23 1.226(4) . ? C22 C21 1.560(4) 2_754 ? C21 C22 1.560(4) 2_754 ? C23 C23 1.567(6) 2_754 ? 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 Fe1 O2 160.29(12) 2_754 . ? O2 Fe1 O1 86.94(8) 2_754 2_754 ? O2 Fe1 O1 80.88(8) . 2_754 ? O2 Fe1 O1 80.88(8) 2_754 . ? O2 Fe1 O1 86.93(8) . . ? O1 Fe1 O1 103.44(12) 2_754 . ? O2 Fe1 O3 95.82(8) 2_754 2_754 ? O2 Fe1 O3 99.27(8) . 2_754 ? O1 Fe1 O3 88.55(8) 2_754 2_754 ? O1 Fe1 O3 167.30(9) . 2_754 ? O2 Fe1 O3 99.27(8) 2_754 . ? O2 Fe1 O3 95.82(8) . . ? O1 Fe1 O3 167.30(9) 2_754 . ? O1 Fe1 O3 88.55(8) . . ? O3 Fe1 O3 79.85(12) 2_754 . ? C7 S8 C9 95.51(12) . . ? C7 S6 C6 95.15(12) . . ? C5 S7 C8 95.05(12) . . ? C15 S16 C19 95.47(12) . . ? C5 S5 C10 95.32(12) . . ? C17 S14 C20 95.33(12) . . ? C8 S4 C1 96.78(14) . . ? C17 S15 C16 95.60(12) . . ? C15 S13 C18 95.40(12) . . ? C20 S11 C11 101.63(13) . . ? C19 S10 C12 98.73(13) . . ? C9 S2 C4 101.61(13) . . ? C16 S12 C14 100.82(13) . . ? C6 S3 C3 100.89(13) . . ? C10 S1 C2 104.29(14) . . ? C18 S9 C13 102.38(13) . . ? C8 C10 S1 127.9(2) . . ? C8 C10 S5 116.5(2) . . ? S1 C10 S5 115.53(15) . . ? C18 C19 S10 127.6(2) . . ? C18 C19 S16 117.0(2) . . ? S10 C19 S16 115.39(15) . . ? C12 C13 S9 114.1(2) . . ? C10 C8 S4 125.5(2) . . ? C10 C8 S7 117.3(2) . . ? S4 C8 S7 116.94(15) . . ? C16 C20 S11 129.4(2) . . ? C16 C20 S14 117.0(2) . . ? S11 C20 S14 113.64(15) . . ? C6 C9 S2 128.5(2) . . ? C6 C9 S8 116.2(2) . . ? S2 C9 S8 115.28(15) . . ? C19 C18 S9 129.1(2) . . ? C19 C18 S13 117.1(2) . . ? S9 C18 S13 113.83(15) . . ? C15 C17 S14 123.5(2) . . ? C15 C17 S15 121.2(2) . . ? S14 C17 S15 115.28(15) . . ? C20 C16 S12 127.7(2) . . ? C20 C16 S15 116.8(2) . . ? S12 C16 S15 115.45(15) . . ? C7 C5 S7 123.0(2) . . ? C7 C5 S5 121.6(2) . . ? S7 C5 S5 115.31(14) . . ? C17 C15 S13 123.3(2) . . ? C17 C15 S16 121.7(2) . . ? S13 C15 S16 115.06(14) . . ? C9 C6 S6 117.6(2) . . ? C9 C6 S3 128.1(2) . . ? S6 C6 S3 114.34(15) . . ? C5 C7 S8 122.4(2) . . ? C5 C7 S6 122.1(2) . . ? S8 C7 S6 115.52(14) . . ? C3 C4 S2 113.7(2) . . ? C11 C14 S12 114.3(2) . . ? C1 C2 S1 117.2(2) . . ? C13 C12 S10 112.3(2) . . ? C4 C3 S3 113.3(2) . . ? C14 C11 S11 113.7(2) . . ? C2 C1 S4 113.7(2) . . ? O30 N1 O30 124.6(4) . 2_854 ? O30 N1 C27 117.7(2) . . ? O30 N1 C27 117.7(2) 2_854 . ? C26 C27 C26 124.6(4) . 2_854 ? C26 C27 N1 117.7(2) . . ? C26 C27 N1 117.7(2) 2_854 . ? C25 C24 C25 121.6(5) . 2_854 ? C27 C26 C25 117.0(4) . . ? C24 C25 C26 119.9(4) . . ? C21 O2 Fe1 115.0(2) . . ? C22 O1 Fe1 115.5(2) . . ? C23 O3 Fe1 116.5(2) . . ? O5 C22 O1 125.9(3) . . ? O5 C22 C21 120.1(2) . 2_754 ? O1 C22 C21 114.0(2) . 2_754 ? O6 C21 O2 126.4(3) . . ? O6 C21 C22 119.9(3) . 2_754 ? O2 C21 C22 113.8(2) . 2_754 ? O4 C23 O3 126.5(3) . . ? O4 C23 C23 120.0(2) . 2_754 ? O3 C23 C23 113.5(2) . 2_754 ? _refine_diff_density_max 1.129 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.121 #===END data_etcrnobt _database_code_CSD 157875 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H20.50 Cr0.50 N O7 S16' _chemical_formula_weight 997.89 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.28340(10) _cell_length_b 19.91720(10) _cell_length_c 34.9399(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.2990(10) _cell_angle_gamma 90.00 _cell_volume 7144.41(9) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method ? _exptl_crystal_F_000 4060 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25199 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0828 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8179 _reflns_number_observed 5249 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 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^)+(0.0395P)^2^+7.7070P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8172 _refine_ls_number_parameters 458 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0960 _refine_ls_R_factor_obs 0.0470 _refine_ls_wR_factor_all 0.1109 _refine_ls_wR_factor_obs 0.0902 _refine_ls_goodness_of_fit_all 1.028 _refine_ls_goodness_of_fit_obs 1.065 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.065 _refine_ls_shift/esd_max -0.012 _refine_ls_shift/esd_mean 0.001 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 0.07563(5) 0.2500 0.0150(2) Uani 1 d S . S8 S 0.74145(10) 0.01038(5) -0.54449(3) 0.0150(2) Uani 1 d . . S6 S 0.97455(10) 0.08752(5) -0.51917(3) 0.0162(2) Uani 1 d . . S7 S 0.61413(10) 0.04308(5) -0.46376(3) 0.0152(2) Uani 1 d . . S14 S 0.78300(10) 0.17425(5) -0.04902(3) 0.0157(2) Uani 1 d . . S5 S 0.85059(10) 0.11834(5) -0.43902(3) 0.0162(2) Uani 1 d . . S15 S 0.54436(10) 0.24684(5) -0.07507(3) 0.0157(2) Uani 1 d . . S4 S 0.47616(10) 0.07480(5) -0.39341(3) 0.0167(2) Uani 1 d . . S10 S 0.29286(10) 0.19065(5) 0.07899(3) 0.0183(2) Uani 1 d . . S16 S 0.66524(10) 0.14336(5) 0.03122(3) 0.0153(2) Uani 1 d . . S13 S 0.42163(10) 0.21350(5) 0.00738(3) 0.0162(2) Uani 1 d . . S11 S 0.91738(10) 0.19508(5) -0.12040(3) 0.0178(2) Uani 1 d . . S3 S 1.11080(10) 0.06872(6) -0.58987(3) 0.0224(3) Uani 1 d . . S9 S 0.58755(10) 0.10976(6) 0.10905(3) 0.0175(2) Uani 1 d . . S1 S 0.75393(11) 0.16152(6) -0.36474(3) 0.0205(2) Uani 1 d . . S2 S 0.82832(10) -0.02003(6) -0.62175(3) 0.0186(2) Uani 1 d . . S12 S 0.62633(11) 0.27505(6) -0.15251(3) 0.0211(3) Uani 1 d . . C20 C 0.7796(4) 0.2090(2) -0.09500(11) 0.0142(9) Uani 1 d . . C8 C 0.6127(4) 0.0855(2) -0.42000(11) 0.0147(9) Uani 1 d . . C13 C 0.7736(4) 0.2623(2) -0.17774(12) 0.0235(10) Uani 1 d . . H13A H 0.7512(4) 0.2642(2) -0.20566(12) 0.028 Uiso 1 calc R . H13B H 0.8345(4) 0.2998(2) -0.17135(12) 0.028 Uiso 1 calc R . C28 C 0.5449(4) 0.1463(2) 0.06443(11) 0.0136(8) Uani 1 d . . C19 C 0.4322(4) 0.1786(2) 0.05359(11) 0.0143(9) Uani 1 d . . C16 C 0.6678(4) 0.2410(2) -0.10740(11) 0.0144(9) Uani 1 d . . C10 C 0.7227(4) 0.1197(2) -0.40806(11) 0.0138(9) Uani 1 d . . O3 O 0.6469(3) 0.06467(14) 0.21636(7) 0.0170(6) Uani 1 d . . C17 C 0.6280(4) 0.2020(2) -0.03853(11) 0.0143(9) Uani 1 d . . C5 C 0.7663(4) 0.0727(2) -0.47515(11) 0.0139(9) Uani 1 d . . C9 C 0.9718(4) 0.0527(2) -0.56511(11) 0.0143(9) Uani 1 d . . C15 C 0.5761(4) 0.1879(2) -0.00425(11) 0.0142(9) Uani 1 d . . O2 O 0.4185(3) 0.15086(14) 0.22032(8) 0.0213(7) Uani 1 d . . C6 C 0.8639(4) 0.0174(2) -0.57694(11) 0.0139(9) Uani 1 d . . C7 C 0.8205(4) 0.0591(2) -0.50883(11) 0.0135(8) Uani 1 d . . O4 O 0.8132(3) -0.0074(2) 0.20874(8) 0.0271(7) Uani 1 d . . C4 C 0.9829(4) -0.0146(2) -0.64324(12) 0.0228(10) Uani 1 d . . H4A H 1.0414(4) -0.0496(2) -0.63183(12) 0.027 Uiso 1 calc R . H4B H 0.9695(4) -0.0243(2) -0.67097(12) 0.027 Uiso 1 calc R . O1 O 0.4012(3) 0.00973(14) 0.21802(7) 0.0173(6) Uani 1 d . . C2 C 0.6342(5) 0.1284(2) -0.33386(12) 0.0297(12) Uani 1 d . . H2A H 0.6786(5) 0.1190(2) -0.30854(12) 0.036 Uiso 1 calc R . H2B H 0.5691(5) 0.1641(2) -0.33003(12) 0.036 Uiso 1 calc R . O5 O 0.2118(3) -0.04638(15) 0.21513(8) 0.0223(7) Uani 1 d . . C12 C 0.8430(4) 0.1964(2) -0.16856(11) 0.0217(10) Uani 1 d . . H12A H 0.9111(4) 0.1892(2) -0.18706(11) 0.026 Uiso 1 calc R . H12B H 0.7797(4) 0.1591(2) -0.17158(11) 0.026 Uiso 1 calc R . C14 C 0.4296(4) 0.1027(2) 0.12901(11) 0.0161(9) Uani 1 d . . H14A H 0.3795(4) 0.0670(2) 0.11511(11) 0.019 Uiso 1 calc R . H14B H 0.4422(4) 0.0887(2) 0.15614(11) 0.019 Uiso 1 calc R . C3 C 1.0492(4) 0.0527(2) -0.63840(11) 0.0222(10) Uani 1 d . . H3A H 0.9864(4) 0.0885(2) -0.64634(11) 0.027 Uiso 1 calc R . H3B H 1.1223(4) 0.0549(2) -0.65559(11) 0.027 Uiso 1 calc R . C23 C 0.7260(4) 0.0170(2) 0.22743(12) 0.0204(10) Uani 1 d . . C11 C 0.3498(4) 0.1666(2) 0.12721(11) 0.0186(9) Uani 1 d . . H11A H 0.4032(4) 0.2036(2) 0.13871(11) 0.022 Uiso 1 calc R . H11B H 0.2734(4) 0.1606(2) 0.14290(11) 0.022 Uiso 1 calc R . C1 C 0.5633(5) 0.0671(2) -0.34669(12) 0.0311(12) Uani 1 d . . H1A H 0.5002(5) 0.0554(2) -0.32743(12) 0.037 Uiso 1 calc R . H1B H 0.6263(5) 0.0297(2) -0.34770(12) 0.037 Uiso 1 calc R . C22 C 0.2935(4) -0.0102(2) 0.23171(12) 0.0160(9) Uani 1 d . . O6 O 0.4071(3) 0.2634(2) 0.21934(9) 0.0306(8) Uani 1 d . . C21 C 0.4489(4) 0.2101(2) 0.23252(12) 0.0214(10) Uani 1 d . . O30 O 0.8947(4) 0.3447(2) 0.24623(10) 0.0447(10) Uani 1 d . . N1 N 1.0000 0.3161(3) 0.2500 0.0322(14) Uani 1 d S . C27 C 1.0000 0.2424(3) 0.2500 0.028(2) Uani 1 d S . C26 C 1.0987(5) 0.2101(2) 0.23193(13) 0.0312(12) Uani 1 d . . H26A H 1.1652(5) 0.2346(2) 0.22028(13) 0.037 Uiso 1 calc R . C24 C 1.0000 0.1054(4) 0.2500 0.049(2) Uani 1 d S . H24A H 1.0000 0.0577(4) 0.2500 0.074 Uiso 1 calc SR . C25 C 1.0963(5) 0.1397(3) 0.2316(2) 0.043(2) Uani 1 d . . H25A H 1.1604(5) 0.1154(3) 0.2188(2) 0.051 Uiso 1 calc R . N2 N 0.0000 -0.1058(3) 0.2500 0.0310(14) 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 0.0153(5) 0.0164(5) 0.0135(5) 0.000 0.0018(4) 0.000 S8 0.0108(5) 0.0203(6) 0.0139(5) -0.0031(4) 0.0011(4) -0.0038(4) S6 0.0119(5) 0.0236(6) 0.0132(5) -0.0038(4) 0.0013(4) -0.0049(4) S7 0.0114(5) 0.0190(6) 0.0152(5) -0.0024(4) 0.0009(4) -0.0043(4) S14 0.0114(5) 0.0195(6) 0.0164(5) 0.0036(4) 0.0011(4) 0.0027(4) S5 0.0116(5) 0.0238(6) 0.0134(5) -0.0034(4) 0.0019(4) -0.0056(4) S15 0.0123(5) 0.0201(6) 0.0149(5) 0.0021(4) 0.0008(4) 0.0041(4) S4 0.0113(5) 0.0201(6) 0.0192(5) 0.0001(4) 0.0048(4) -0.0022(4) S10 0.0112(5) 0.0248(6) 0.0193(5) 0.0016(5) 0.0041(4) 0.0044(4) S16 0.0106(5) 0.0216(6) 0.0139(5) 0.0037(4) 0.0019(4) 0.0026(4) S13 0.0110(5) 0.0217(6) 0.0158(5) 0.0019(4) 0.0014(4) 0.0038(4) S11 0.0136(5) 0.0209(6) 0.0194(5) 0.0008(4) 0.0048(4) 0.0009(4) S3 0.0145(6) 0.0342(7) 0.0190(5) -0.0078(5) 0.0057(4) -0.0106(5) S9 0.0124(5) 0.0241(6) 0.0160(5) 0.0055(4) 0.0014(4) 0.0024(4) S1 0.0221(6) 0.0258(6) 0.0138(5) -0.0054(4) 0.0040(4) -0.0090(5) S2 0.0112(5) 0.0263(6) 0.0184(5) -0.0104(5) 0.0018(4) -0.0026(4) S12 0.0218(6) 0.0274(6) 0.0138(5) 0.0044(5) -0.0018(4) 0.0038(5) C20 0.014(2) 0.013(2) 0.016(2) -0.001(2) 0.003(2) -0.002(2) C8 0.017(2) 0.013(2) 0.015(2) -0.001(2) 0.002(2) -0.001(2) C13 0.023(2) 0.032(3) 0.015(2) 0.004(2) 0.001(2) -0.005(2) C28 0.011(2) 0.017(2) 0.013(2) 0.000(2) 0.002(2) -0.001(2) C19 0.015(2) 0.016(2) 0.012(2) 0.002(2) -0.001(2) -0.002(2) C16 0.014(2) 0.016(2) 0.013(2) -0.001(2) 0.001(2) 0.000(2) C10 0.014(2) 0.016(2) 0.012(2) -0.001(2) 0.002(2) -0.001(2) O3 0.0142(15) 0.022(2) 0.0153(14) 0.0018(12) 0.0039(12) -0.0025(13) C17 0.010(2) 0.016(2) 0.016(2) 0.000(2) -0.002(2) 0.000(2) C5 0.012(2) 0.016(2) 0.014(2) 0.000(2) 0.000(2) -0.003(2) C9 0.013(2) 0.017(2) 0.013(2) -0.004(2) 0.003(2) -0.004(2) C15 0.010(2) 0.015(2) 0.017(2) -0.001(2) -0.001(2) 0.002(2) O2 0.025(2) 0.018(2) 0.021(2) 0.0011(13) 0.0005(13) 0.0047(13) C6 0.013(2) 0.016(2) 0.013(2) -0.003(2) 0.000(2) 0.000(2) C7 0.011(2) 0.015(2) 0.014(2) -0.003(2) -0.003(2) -0.001(2) O4 0.021(2) 0.034(2) 0.027(2) -0.0029(15) 0.0078(14) 0.0026(15) C4 0.017(2) 0.031(3) 0.021(2) -0.008(2) 0.003(2) -0.006(2) O1 0.016(2) 0.021(2) 0.0151(14) -0.0015(12) 0.0029(12) -0.0025(12) C2 0.030(3) 0.045(3) 0.015(2) 0.002(2) 0.006(2) -0.010(2) O5 0.015(2) 0.027(2) 0.024(2) 0.0007(14) -0.0006(13) -0.0046(13) C12 0.020(2) 0.026(3) 0.019(2) -0.005(2) 0.001(2) -0.001(2) C14 0.014(2) 0.023(2) 0.012(2) 0.000(2) 0.004(2) 0.000(2) C3 0.025(2) 0.025(3) 0.017(2) -0.004(2) 0.005(2) -0.006(2) C23 0.020(2) 0.023(3) 0.018(2) -0.004(2) 0.003(2) -0.006(2) C11 0.015(2) 0.023(2) 0.018(2) 0.004(2) 0.005(2) 0.003(2) C1 0.038(3) 0.039(3) 0.017(2) 0.004(2) 0.005(2) -0.010(2) C22 0.019(2) 0.009(2) 0.020(2) 0.004(2) 0.003(2) 0.005(2) O6 0.035(2) 0.021(2) 0.038(2) 0.011(2) 0.014(2) 0.0083(15) C21 0.022(2) 0.021(2) 0.023(2) 0.001(2) 0.014(2) 0.002(2) O30 0.061(3) 0.033(2) 0.039(2) 0.002(2) 0.001(2) 0.014(2) N1 0.048(4) 0.026(3) 0.022(3) 0.000 -0.002(3) 0.000 C27 0.037(4) 0.022(4) 0.022(3) 0.000 -0.014(3) 0.000 C26 0.028(3) 0.033(3) 0.030(3) -0.003(2) -0.016(2) 0.002(2) C24 0.035(5) 0.024(4) 0.085(7) 0.000 -0.036(5) 0.000 C25 0.039(3) 0.030(3) 0.055(4) -0.013(3) -0.031(3) 0.013(2) N2 0.027(3) 0.021(3) 0.048(4) 0.000 0.020(3) 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 O1 1.968(3) . ? Cr1 O1 1.968(3) 2_655 ? Cr1 O3 1.979(3) . ? Cr1 O3 1.979(3) 2_655 ? Cr1 O2 1.981(3) . ? Cr1 O2 1.981(3) 2_655 ? S8 C7 1.744(4) . ? S8 C6 1.748(4) . ? S6 C7 1.739(4) . ? S6 C9 1.747(4) . ? S7 C5 1.740(4) . ? S7 C8 1.748(4) . ? S14 C17 1.746(4) . ? S14 C20 1.747(4) . ? S5 C5 1.745(4) . ? S5 C10 1.750(4) . ? S15 C17 1.744(4) . ? S15 C16 1.751(4) . ? S4 C8 1.741(4) . ? S4 C1 1.823(4) . ? S10 C19 1.745(4) . ? S10 C11 1.816(4) . ? S16 C15 1.741(4) . ? S16 C28 1.745(4) . ? S13 C15 1.739(4) . ? S13 C19 1.755(4) . ? S11 C20 1.737(4) . ? S11 C12 1.808(4) . ? S3 C9 1.742(4) . ? S3 C3 1.804(4) . ? S9 C28 1.753(4) . ? S9 C14 1.810(4) . ? S1 C10 1.741(4) . ? S1 C2 1.808(4) . ? S2 C6 1.753(4) . ? S2 C4 1.800(4) . ? S12 C16 1.746(4) . ? S12 C13 1.814(4) . ? C20 C16 1.363(5) . ? C8 C10 1.364(5) . ? C13 C12 1.520(6) . ? C28 C19 1.360(5) . ? O3 C23 1.295(5) . ? C17 C15 1.368(5) . ? C5 C7 1.358(5) . ? C9 C6 1.359(5) . ? O2 C21 1.287(5) . ? O4 C23 1.238(5) . ? C4 C3 1.509(6) . ? O1 C22 1.294(5) . ? C2 C1 1.478(6) . ? O5 C22 1.227(5) . ? C14 C11 1.512(5) . ? C23 C22 1.550(6) 2_655 ? C22 C23 1.550(6) 2_655 ? O6 C21 1.225(5) . ? C21 C21 1.565(9) 2_655 ? O30 N1 1.224(4) . ? N1 O30 1.224(4) 2_755 ? N1 C27 1.469(8) . ? C27 C26 1.384(6) 2_755 ? C27 C26 1.384(6) . ? C26 C25 1.403(7) . ? C24 C25 1.391(7) . ? C24 C25 1.391(7) 2_755 ? 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 O1 Cr1 O1 96.3(2) . 2_655 ? O1 Cr1 O3 88.63(11) . . ? O1 Cr1 O3 82.92(11) 2_655 . ? O1 Cr1 O3 82.92(11) . 2_655 ? O1 Cr1 O3 88.63(11) 2_655 2_655 ? O3 Cr1 O3 167.3(2) . 2_655 ? O1 Cr1 O2 91.04(12) . . ? O1 Cr1 O2 172.27(12) 2_655 . ? O3 Cr1 O2 95.00(12) . . ? O3 Cr1 O2 94.57(12) 2_655 . ? O1 Cr1 O2 172.27(12) . 2_655 ? O1 Cr1 O2 91.04(12) 2_655 2_655 ? O3 Cr1 O2 94.57(12) . 2_655 ? O3 Cr1 O2 95.00(12) 2_655 2_655 ? O2 Cr1 O2 81.7(2) . 2_655 ? C7 S8 C6 95.5(2) . . ? C7 S6 C9 95.5(2) . . ? C5 S7 C8 95.1(2) . . ? C17 S14 C20 95.6(2) . . ? C5 S5 C10 95.5(2) . . ? C17 S15 C16 95.3(2) . . ? C8 S4 C1 96.8(2) . . ? C19 S10 C11 101.8(2) . . ? C15 S16 C28 95.3(2) . . ? C15 S13 C19 95.1(2) . . ? C20 S11 C12 99.2(2) . . ? C9 S3 C3 100.4(2) . . ? C28 S9 C14 101.0(2) . . ? C10 S1 C2 104.3(2) . . ? C6 S2 C4 101.7(2) . . ? C16 S12 C13 102.5(2) . . ? C16 C20 S11 127.6(3) . . ? C16 C20 S14 116.7(3) . . ? S11 C20 S14 115.7(2) . . ? C10 C8 S4 125.3(3) . . ? C10 C8 S7 117.4(3) . . ? S4 C8 S7 117.1(2) . . ? C12 C13 S12 114.4(3) . . ? C19 C28 S16 117.1(3) . . ? C19 C28 S9 127.5(3) . . ? S16 C28 S9 115.3(2) . . ? C28 C19 S10 129.4(3) . . ? C28 C19 S13 116.8(3) . . ? S10 C19 S13 113.8(2) . . ? C20 C16 S12 128.8(3) . . ? C20 C16 S15 117.1(3) . . ? S12 C16 S15 114.1(2) . . ? C8 C10 S1 127.8(3) . . ? C8 C10 S5 116.3(3) . . ? S1 C10 S5 115.9(2) . . ? C23 O3 Cr1 113.0(2) . . ? C15 C17 S15 123.1(3) . . ? C15 C17 S14 121.7(3) . . ? S15 C17 S14 115.2(2) . . ? C7 C5 S7 123.4(3) . . ? C7 C5 S5 121.3(3) . . ? S7 C5 S5 115.3(2) . . ? C6 C9 S3 128.5(3) . . ? C6 C9 S6 117.0(3) . . ? S3 C9 S6 114.4(2) . . ? C17 C15 S13 123.5(3) . . ? C17 C15 S16 120.8(3) . . ? S13 C15 S16 115.7(2) . . ? C21 O2 Cr1 115.6(3) . . ? C9 C6 S8 116.8(3) . . ? C9 C6 S2 128.1(3) . . ? S8 C6 S2 115.1(2) . . ? C5 C7 S6 122.7(3) . . ? C5 C7 S8 122.2(3) . . ? S6 C7 S8 115.2(2) . . ? C3 C4 S2 114.3(3) . . ? C22 O1 Cr1 114.8(2) . . ? C1 C2 S1 117.5(3) . . ? C13 C12 S11 112.1(3) . . ? C11 C14 S9 114.6(3) . . ? C4 C3 S3 113.2(3) . . ? O4 C23 O3 126.2(4) . . ? O4 C23 C22 119.0(4) . 2_655 ? O3 C23 C22 114.7(4) . 2_655 ? C14 C11 S10 113.9(3) . . ? C2 C1 S4 114.2(3) . . ? O5 C22 O1 125.7(4) . . ? O5 C22 C23 121.2(4) . 2_655 ? O1 C22 C23 113.1(4) . 2_655 ? O6 C21 O2 126.6(4) . . ? O6 C21 C21 119.9(3) . 2_655 ? O2 C21 C21 113.5(2) . 2_655 ? O30 N1 O30 124.6(6) . 2_755 ? O30 N1 C27 117.7(3) . . ? O30 N1 C27 117.7(3) 2_755 . ? C26 C27 C26 124.7(7) 2_755 . ? C26 C27 N1 117.7(3) 2_755 . ? C26 C27 N1 117.7(3) . . ? C27 C26 C25 117.1(5) . . ? C25 C24 C25 121.2(7) . 2_755 ? C24 C25 C26 120.0(6) . . ? _refine_diff_density_max 0.771 _refine_diff_density_min -0.518 _refine_diff_density_rms 0.115 #===END data_etcrno _database_code_CSD 157876 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H20.50 Cr0.50 N O7 S16' _chemical_formula_weight 997.89 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 10.3039(2) _cell_length_b 20.0908(3) _cell_length_c 35.2508(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.7010(10) _cell_angle_gamma 90.00 _cell_volume 7289.3(2) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4060 _exptl_absorpt_coefficient_mu 1.137 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34583 _diffrn_reflns_av_R_equivalents 0.1170 _diffrn_reflns_av_sigmaI/netI 0.1172 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8365 _reflns_number_gt 4188 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0642P)^2^+1.3023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8365 _refine_ls_number_parameters 472 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1637 _refine_ls_R_factor_gt 0.0646 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 1.0000 0.42207(6) -0.2500 0.0344(3) Uani 1 2 d S . . S8 S 1.25685(14) 0.01188(8) 0.04381(4) 0.0380(4) Uani 1 1 d . . . S7 S 1.38372(14) 0.04290(8) -0.03665(4) 0.0385(4) Uani 1 1 d . . . S6 S 1.02560(15) 0.08849(8) 0.01930(4) 0.0400(4) Uani 1 1 d . . . S16 S 0.78063(14) 0.17438(8) -0.04950(4) 0.0376(4) Uani 1 1 d . . . S5 S 1.15042(15) 0.11844(8) -0.06066(4) 0.0402(4) Uani 1 1 d . . . S15 S 0.66373(14) 0.14363(8) 0.03115(4) 0.0373(4) Uani 1 1 d . . . S14 S 0.42295(14) 0.21414(8) 0.00821(5) 0.0392(4) Uani 1 1 d . . . S13 S 0.54317(15) 0.24575(8) -0.07388(4) 0.0392(4) Uani 1 1 d . . . S4 S 1.52326(15) 0.07253(8) -0.10624(5) 0.0443(4) Uani 1 1 d . . . S3 S 0.89134(16) 0.07156(10) 0.08993(5) 0.0572(5) Uani 1 1 d . . . S12 S 0.58517(15) 0.11061(8) 0.10822(5) 0.0428(4) Uani 1 1 d . . . S11 S 0.29483(15) 0.19267(8) 0.07953(5) 0.0462(4) Uani 1 1 d . . . S2 S 1.16976(15) -0.01692(9) 0.12078(5) 0.0468(5) Uani 1 1 d . . . S10 S 0.91119(16) 0.19290(8) -0.12112(5) 0.0476(5) Uani 1 1 d . . . S1 S 1.24904(18) 0.15804(9) -0.13502(5) 0.0524(5) Uani 1 1 d . . . S9 S 0.62258(19) 0.27354(9) -0.15108(5) 0.0548(5) Uani 1 1 d . . . C20 C 0.4329(5) 0.1802(3) 0.05395(16) 0.0322(13) Uani 1 1 d . . . C10 C 1.2788(5) 0.1177(3) -0.09179(16) 0.0343(14) Uani 1 1 d . . . C19 C 0.7745(6) 0.2075(3) -0.09534(16) 0.0330(14) Uani 1 1 d . . . C9 C 1.1353(5) 0.0202(3) 0.07608(16) 0.0329(14) Uani 1 1 d . . . C18 C 0.6650(6) 0.2398(3) -0.10675(16) 0.0345(14) Uani 1 1 d . . . C8 C 1.3852(5) 0.0839(3) -0.08047(16) 0.0319(13) Uani 1 1 d . . . C17 C 0.5772(5) 0.1884(3) -0.00391(16) 0.0299(13) Uani 1 1 d . . . C16 C 0.5443(5) 0.1473(3) 0.06439(16) 0.0323(14) Uani 1 1 d . . . C7 C 1.1778(5) 0.0594(3) 0.00881(16) 0.0311(13) Uani 1 1 d . . . C6 C 1.0290(5) 0.0548(3) 0.06486(16) 0.0337(14) Uani 1 1 d . . . C5 C 1.2321(5) 0.0729(3) -0.02517(16) 0.0328(14) Uani 1 1 d . . . C15 C 0.6283(5) 0.2017(3) -0.03855(16) 0.0329(14) Uani 1 1 d . . . C14 C 0.7695(7) 0.2618(4) -0.17621(19) 0.063(2) Uani 1 1 d . . . H14A H 0.7482 0.2643 -0.2033 0.075 Uiso 1 1 calc R . . H14B H 0.8288 0.2979 -0.1697 0.075 Uiso 1 1 calc R . . C13 C 0.4305(6) 0.1057(3) 0.12934(18) 0.0433(16) Uani 1 1 d . . . H13A H 0.3800 0.0706 0.1168 0.052 Uiso 1 1 calc R . . H13B H 0.4444 0.0933 0.1558 0.052 Uiso 1 1 calc R . . C4 C 1.0217(8) -0.0064(5) 0.1434(2) 0.093(3) Uani 1 1 d . . . H4A H 0.9674 -0.0443 0.1364 0.112 Uiso 1 1 calc R . . H4B H 1.0413 -0.0096 0.1705 0.112 Uiso 1 1 calc R . . C12 C 0.3522(6) 0.1695(3) 0.12722(17) 0.0443(16) Uani 1 1 d . . . H12A H 0.4054 0.2054 0.1378 0.053 Uiso 1 1 calc R . . H12B H 0.2779 0.1647 0.1429 0.053 Uiso 1 1 calc R . . C3 C 0.9455(8) 0.0506(4) 0.1375(2) 0.079(3) Uani 1 1 d . . . H3A H 0.9944 0.0882 0.1478 0.095 Uiso 1 1 calc R . . H3B H 0.8691 0.0459 0.1523 0.095 Uiso 1 1 calc R . . C2 C 1.3565(8) 0.1162(5) -0.1646(2) 0.102(3) Uani 1 1 d . . . H2A H 1.3019 0.0919 -0.1829 0.122 Uiso 1 1 calc R . . H2B H 1.3990 0.1507 -0.1787 0.122 Uiso 1 1 calc R . . C11 C 0.8378(7) 0.1969(3) -0.1679(2) 0.061(2) Uani 1 1 d . . . H11A H 0.9043 0.1905 -0.1861 0.073 Uiso 1 1 calc R . . H11B H 0.7757 0.1608 -0.1711 0.073 Uiso 1 1 calc R . . C1 C 1.4497(10) 0.0743(5) -0.1529(2) 0.117(4) Uani 1 1 d . . . H1A H 1.5200 0.0804 -0.1700 0.140 Uiso 1 1 calc R . . H1B H 1.4157 0.0300 -0.1578 0.140 Uiso 1 1 calc R . . O1 O 0.8499(4) 0.4329(2) -0.21761(11) 0.0392(10) Uani 1 1 d . . . O2 O 1.0788(4) 0.3472(2) -0.22031(12) 0.0454(11) Uani 1 1 d . . . O3 O 1.0964(4) 0.48710(18) -0.21800(11) 0.0373(10) Uani 1 1 d . . . O4 O 1.2836(4) 0.5433(2) -0.21451(12) 0.0494(12) Uani 1 1 d . . . O5 O 0.6804(4) 0.5015(2) -0.21148(13) 0.0594(13) Uani 1 1 d . . . N2 N 1.0000 -0.1014(5) 0.2500 0.059(2) Uani 1 2 d SD . . C23 C 1.2038(6) 0.5067(3) -0.23106(16) 0.0322(14) Uani 1 1 d . . . C27 C 0.5000 0.2516(5) -0.2500 0.061(3) Uani 1 2 d S . . O6 O 1.0885(5) 0.2362(2) -0.21915(15) 0.0655(15) Uani 1 1 d . . . C22 C 0.7707(6) 0.4790(3) -0.22925(18) 0.0391(15) Uani 1 1 d . . . C21 C 1.0483(6) 0.2890(3) -0.23271(17) 0.0438(16) Uani 1 1 d . . . N1 N 0.5000 0.1788(6) -0.2500 0.086(4) Uani 1 2 d S . . C26 C 0.5981(7) 0.2832(4) -0.2679(2) 0.062(2) Uani 1 1 d . . . H26A H 0.6631 0.2594 -0.2793 0.075 Uiso 1 1 calc R . . C25 C 0.5958(8) 0.3521(4) -0.2680(3) 0.087(3) Uani 1 1 d . . . H25A H 0.6593 0.3754 -0.2804 0.105 Uiso 1 1 calc R . . C24 C 0.5000 0.3867(6) -0.2500 0.099(5) Uani 1 2 d S . . H24A H 0.5000 0.4330 -0.2500 0.118 Uiso 1 2 calc SR . . O30 O 0.6044(8) 0.1502(3) -0.2491(2) 0.129(3) Uani 1 1 d . . . H124 H 0.944(9) -0.125(6) 0.235(3) 0.04(4) Uiso 0.50 1 d PD . . H121 H 1.068(11) -0.082(7) 0.239(5) 0.07(5) Uiso 0.50 1 d PD . . H123 H 1.0000 -0.1464(11) 0.2500 0.18(9) Uiso 1 2 d SD . . H122 H 0.96(2) -0.070(6) 0.235(5) 0.11(7) Uiso 0.50 1 d PD . . 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 0.0402(8) 0.0355(8) 0.0277(7) 0.000 0.0051(6) 0.000 S8 0.0331(8) 0.0473(10) 0.0340(9) 0.0084(7) 0.0047(7) 0.0112(7) S7 0.0346(8) 0.0448(10) 0.0363(9) 0.0048(7) 0.0050(7) 0.0122(7) S6 0.0344(8) 0.0548(10) 0.0309(9) 0.0073(7) 0.0031(7) 0.0129(8) S16 0.0332(8) 0.0435(10) 0.0363(9) 0.0064(7) 0.0024(7) 0.0067(7) S5 0.0352(9) 0.0562(11) 0.0294(9) 0.0065(7) 0.0053(7) 0.0138(8) S15 0.0320(8) 0.0478(10) 0.0327(9) 0.0094(7) 0.0066(7) 0.0082(7) S14 0.0314(8) 0.0510(10) 0.0353(9) 0.0036(7) 0.0030(7) 0.0097(8) S13 0.0365(8) 0.0461(10) 0.0351(9) 0.0067(7) 0.0014(7) 0.0092(8) S4 0.0373(9) 0.0456(10) 0.0514(11) 0.0002(8) 0.0166(8) 0.0083(8) S3 0.0406(10) 0.0880(14) 0.0442(11) 0.0224(10) 0.0161(8) 0.0281(10) S12 0.0385(9) 0.0532(10) 0.0372(9) 0.0132(8) 0.0071(7) 0.0070(8) S11 0.0347(9) 0.0571(11) 0.0477(10) 0.0042(8) 0.0124(8) 0.0112(8) S2 0.0330(9) 0.0632(11) 0.0446(10) 0.0257(9) 0.0061(8) 0.0086(8) S10 0.0464(10) 0.0465(10) 0.0512(11) 0.0037(8) 0.0174(8) 0.0020(8) S1 0.0604(12) 0.0631(12) 0.0347(10) 0.0138(8) 0.0116(8) 0.0182(10) S9 0.0675(12) 0.0623(12) 0.0339(10) 0.0098(8) -0.0027(9) 0.0073(10) C20 0.032(3) 0.034(3) 0.031(3) -0.004(3) 0.007(3) 0.001(3) C10 0.035(3) 0.043(4) 0.025(3) -0.001(3) 0.006(3) 0.004(3) C19 0.042(4) 0.025(3) 0.032(3) -0.004(3) 0.007(3) -0.004(3) C9 0.029(3) 0.036(3) 0.034(3) 0.009(3) 0.005(3) -0.002(3) C18 0.045(4) 0.031(3) 0.028(3) 0.000(3) 0.004(3) 0.000(3) C8 0.034(3) 0.030(3) 0.032(3) 0.000(3) 0.007(3) -0.003(3) C17 0.028(3) 0.029(3) 0.032(3) 0.001(3) 0.001(2) -0.004(3) C16 0.032(3) 0.030(3) 0.035(3) -0.001(3) 0.007(3) -0.004(3) C7 0.030(3) 0.033(3) 0.031(3) 0.000(3) 0.000(3) 0.005(3) C6 0.033(3) 0.042(4) 0.026(3) 0.011(3) 0.002(3) 0.007(3) C5 0.029(3) 0.042(4) 0.027(3) -0.005(3) 0.002(3) 0.003(3) C15 0.036(3) 0.031(3) 0.031(3) 0.005(3) -0.001(3) 0.004(3) C14 0.064(5) 0.094(6) 0.031(4) 0.009(4) 0.001(3) -0.021(5) C13 0.040(4) 0.048(4) 0.043(4) 0.002(3) 0.013(3) -0.004(3) C4 0.070(6) 0.159(9) 0.052(5) 0.029(6) 0.023(4) 0.054(6) C12 0.044(4) 0.051(4) 0.038(4) 0.005(3) 0.013(3) 0.007(3) C3 0.107(7) 0.082(6) 0.052(5) 0.033(4) 0.034(5) 0.055(5) C2 0.080(6) 0.177(10) 0.047(5) -0.023(6) 0.003(5) 0.047(7) C11 0.069(5) 0.063(5) 0.051(5) -0.015(4) 0.017(4) -0.013(4) C1 0.149(9) 0.169(10) 0.033(5) -0.006(5) 0.023(5) 0.101(8) O1 0.042(2) 0.047(3) 0.028(2) 0.0031(19) 0.0073(19) -0.005(2) O2 0.055(3) 0.040(3) 0.041(3) 0.004(2) 0.002(2) 0.006(2) O3 0.038(2) 0.040(2) 0.035(2) -0.0020(19) 0.0105(19) -0.005(2) O4 0.040(3) 0.059(3) 0.049(3) -0.005(2) -0.002(2) -0.010(2) O5 0.047(3) 0.076(3) 0.057(3) -0.006(3) 0.017(2) 0.001(3) N2 0.056(7) 0.032(6) 0.091(9) 0.000 0.021(7) 0.000 C23 0.037(4) 0.027(3) 0.032(3) 0.007(3) 0.003(3) 0.004(3) C27 0.086(9) 0.039(7) 0.054(7) 0.000 -0.028(6) 0.000 O6 0.079(4) 0.037(3) 0.081(4) 0.017(3) 0.012(3) 0.010(3) C22 0.035(4) 0.047(4) 0.037(4) -0.011(3) 0.012(3) -0.012(3) C21 0.054(4) 0.037(4) 0.042(4) 0.004(3) 0.019(3) 0.006(3) N1 0.145(12) 0.071(9) 0.042(6) 0.000 -0.008(7) 0.000 C26 0.063(5) 0.060(5) 0.062(5) 0.002(4) -0.024(4) 0.001(4) C25 0.074(6) 0.061(6) 0.121(8) 0.020(6) -0.054(6) -0.024(5) C24 0.085(10) 0.046(8) 0.157(15) 0.000 -0.070(10) 0.000 O30 0.197(9) 0.068(5) 0.121(6) 0.008(4) 0.001(6) 0.047(5) _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 1.965(4) . ? Cr1 O3 1.965(4) 2_754 ? Cr1 O1 1.977(4) . ? Cr1 O1 1.977(4) 2_754 ? Cr1 O2 1.984(4) 2_754 ? Cr1 O2 1.984(4) . ? S8 C7 1.733(6) . ? S8 C9 1.739(6) . ? S7 C5 1.740(5) . ? S7 C8 1.751(6) . ? S6 C7 1.730(6) . ? S6 C6 1.742(5) . ? S16 C15 1.724(6) . ? S16 C19 1.746(6) . ? S5 C5 1.735(6) . ? S5 C10 1.758(5) . ? S15 C17 1.741(6) . ? S15 C16 1.740(6) . ? S14 C17 1.743(5) . ? S14 C20 1.749(6) . ? S13 C15 1.732(6) . ? S13 C18 1.752(6) . ? S4 C8 1.739(6) . ? S4 C1 1.780(9) . ? S3 C6 1.739(6) . ? S3 C3 1.790(7) . ? S12 C16 1.746(6) . ? S12 C13 1.793(6) . ? S11 C20 1.738(6) . ? S11 C12 1.816(6) . ? S2 C9 1.764(6) . ? S2 C4 1.767(7) . ? S10 C19 1.737(6) . ? S10 C11 1.782(7) . ? S1 C10 1.741(6) . ? S1 C2 1.768(8) . ? S9 C18 1.740(6) . ? S9 C14 1.805(7) . ? C20 C16 1.360(8) . ? C10 C8 1.335(7) . ? C19 C18 1.346(8) . ? C9 C6 1.342(7) . ? C17 C15 1.379(7) . ? C7 C5 1.373(7) . ? C14 C11 1.503(9) . ? C13 C12 1.514(8) . ? C4 C3 1.399(9) . ? C2 C1 1.328(10) . ? O1 C22 1.288(7) . ? O2 C21 1.283(7) . ? O3 C23 1.281(6) . ? O4 C23 1.230(6) . ? O5 C22 1.232(7) . ? C23 C22 1.540(8) 2_754 ? C27 C26 1.371(8) . ? C27 C26 1.371(8) 2_654 ? C27 N1 1.462(14) . ? O6 C21 1.227(7) . ? C22 C23 1.540(8) 2_754 ? C21 C21 1.537(13) 2_754 ? N1 O30 1.219(7) 2_654 ? N1 O30 1.219(7) . ? C26 C25 1.385(10) . ? C25 C24 1.386(10) . ? C24 C25 1.386(10) 2_654 ? 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 96.6(2) . 2_754 ? O3 Cr1 O1 89.05(16) . . ? O3 Cr1 O1 82.56(16) 2_754 . ? O3 Cr1 O1 82.56(16) . 2_754 ? O3 Cr1 O1 89.05(16) 2_754 2_754 ? O1 Cr1 O1 167.4(2) . 2_754 ? O3 Cr1 O2 171.96(18) . 2_754 ? O3 Cr1 O2 91.03(17) 2_754 2_754 ? O1 Cr1 O2 94.36(17) . 2_754 ? O1 Cr1 O2 95.19(17) 2_754 2_754 ? O3 Cr1 O2 91.03(17) . . ? O3 Cr1 O2 171.96(18) 2_754 . ? O1 Cr1 O2 95.19(17) . . ? O1 Cr1 O2 94.36(16) 2_754 . ? O2 Cr1 O2 81.4(3) 2_754 . ? C7 S8 C9 94.8(3) . . ? C5 S7 C8 95.0(3) . . ? C7 S6 C6 95.0(3) . . ? C15 S16 C19 95.3(3) . . ? C5 S5 C10 95.3(3) . . ? C17 S15 C16 95.8(3) . . ? C17 S14 C20 95.5(3) . . ? C15 S13 C18 94.9(3) . . ? C8 S4 C1 99.1(4) . . ? C6 S3 C3 101.8(3) . . ? C16 S12 C13 102.0(3) . . ? C20 S11 C12 101.8(3) . . ? C9 S2 C4 102.2(3) . . ? C19 S10 C11 99.0(3) . . ? C10 S1 C2 101.8(4) . . ? C18 S9 C14 102.0(3) . . ? C16 C20 S11 129.1(5) . . ? C16 C20 S14 116.8(4) . . ? S11 C20 S14 114.1(3) . . ? C8 C10 S1 127.4(4) . . ? C8 C10 S5 116.7(4) . . ? S1 C10 S5 115.8(3) . . ? C18 C19 S10 127.9(5) . . ? C18 C19 S16 117.0(4) . . ? S10 C19 S16 115.1(3) . . ? C6 C9 S8 117.4(4) . . ? C6 C9 S2 127.6(4) . . ? S8 C9 S2 115.0(3) . . ? C19 C18 S9 128.9(5) . . ? C19 C18 S13 116.9(4) . . ? S9 C18 S13 114.2(3) . . ? C10 C8 S4 126.3(4) . . ? C10 C8 S7 117.5(4) . . ? S4 C8 S7 116.1(3) . . ? C15 C17 S15 121.7(4) . . ? C15 C17 S14 123.4(4) . . ? S15 C17 S14 114.9(3) . . ? C20 C16 S15 117.0(4) . . ? C20 C16 S12 127.6(4) . . ? S15 C16 S12 115.4(3) . . ? C5 C7 S6 122.1(4) . . ? C5 C7 S8 122.2(4) . . ? S6 C7 S8 115.7(3) . . ? C9 C6 S3 128.7(4) . . ? C9 C6 S6 117.0(4) . . ? S3 C6 S6 114.4(3) . . ? C7 C5 S5 122.0(4) . . ? C7 C5 S7 122.8(4) . . ? S5 C5 S7 115.2(3) . . ? C17 C15 S16 121.8(4) . . ? C17 C15 S13 122.3(4) . . ? S16 C15 S13 115.9(3) . . ? C11 C14 S9 114.4(5) . . ? C12 C13 S12 114.5(4) . . ? C3 C4 S2 121.4(6) . . ? C13 C12 S11 114.3(4) . . ? C4 C3 S3 118.7(6) . . ? C1 C2 S1 125.7(7) . . ? C14 C11 S10 113.2(5) . . ? C2 C1 S4 124.7(6) . . ? C22 O1 Cr1 113.3(4) . . ? C21 O2 Cr1 115.1(4) . . ? C23 O3 Cr1 114.8(4) . . ? O4 C23 O3 125.7(6) . . ? O4 C23 C22 120.6(5) . 2_754 ? O3 C23 C22 113.7(5) . 2_754 ? C26 C27 C26 124.9(10) . 2_654 ? C26 C27 N1 117.6(5) . . ? C26 C27 N1 117.6(5) 2_654 . ? O5 C22 O1 125.7(6) . . ? O5 C22 C23 119.6(6) . 2_754 ? O1 C22 C23 114.7(5) . 2_754 ? O6 C21 O2 125.7(6) . . ? O6 C21 C21 120.2(4) . 2_754 ? O2 C21 C21 114.2(3) . 2_754 ? O30 N1 O30 123.7(14) 2_654 . ? O30 N1 C27 118.1(7) 2_654 . ? O30 N1 C27 118.1(7) . . ? C27 C26 C25 116.9(9) . . ? C24 C25 C26 120.9(10) . . ? C25 C24 C25 119.7(12) 2_654 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.915 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.164