Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry data_CroxalateBEDTTTF18crown6 _database_code_CSD 166475 # For publication in Chemical Communications # S.Turner and Mark Light # Royal Institution of Great Britain # 21 Albemarle Street # London # W1S 4BS _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Clark, Robin J. H.' 'Day, P.' 'Firth, Steven' 'Hursthouse, Michael B.' 'Light, Mark E.' 'Rashid, Samina' 'Turner, Scott S.' _publ_contact_author_name 'Prof P Day' _publ_contact_author_address ; Royal Institution 21 Albemarle Street London W1X 4BS UNITED KINGDOM ; _publ_contact_author_email 'PDAY@RI.AC.UK' _publ_section_title 'The First Molecular Charge Transfer Salt Containing Proton Channels' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H28 Cr N0 O19.50 S16' _chemical_formula_weight 1289.50 ~ 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2212(5) _cell_length_b 11.2266(5) _cell_length_c 24.0998(15) _cell_angle_alpha 88.433(3) _cell_angle_beta 88.391(2) _cell_angle_gamma 63.780(3) _cell_volume 2479.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used na _cell_measurement_theta_min na _cell_measurement_theta_max na _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.00 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.727 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type 'Empirical, SORTAV' _exptl_absorpt_correction_T_min 0.9086 _exptl_absorpt_correction_T_max 0.9990 _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_type 'Enraf Nonius KappaCCD area detector' _diffrn_measurement_method 'Phi and Omega scans to fill Ewald sphere' _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number 'not measured' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% na _diffrn_reflns_number 19985 _diffrn_reflns_av_R_equivalents 0.1264 _diffrn_reflns_av_sigmaI/netI 0.2233 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 25.03 _reflns_number_total 8722 _reflns_number_gt 3550 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; ? ; _computing_cell_refinement 'DENZO and COLLECT' _computing_data_reduction 'DENZO and COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP _computing_publication_material CIFTAB _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 w=1/[\s^2^(Fo^2^)+(0.0677P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8722 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1901 _refine_ls_R_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1222 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.810 _refine_ls_shift/su_max 0.619 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S4 S 0.5612(2) 0.58315(18) 0.05375(9) 0.0262(5) Uani 1 d . . . S8 S 0.8928(2) 0.45681(19) -0.17216(10) 0.0295(6) Uani 1 d . . . S5 S 0.8930(2) 0.67739(18) -0.02612(9) 0.0247(5) Uani 1 d . . . S6 S 0.7515(2) 0.51499(18) -0.06088(9) 0.0255(5) Uani 1 d . . . S3 S 0.7099(2) 0.73982(19) 0.08834(9) 0.0261(5) Uani 1 d . . . S7 S 1.0621(3) 0.6495(2) -0.12920(10) 0.0415(7) Uani 1 d . . . S13 S 0.9792(2) 1.14909(18) -0.07591(9) 0.0229(5) Uani 1 d . . . S10 S 0.4606(2) 1.11111(19) 0.10660(9) 0.0259(5) Uani 1 d . . . S11 S 0.8041(2) 1.20906(18) 0.04126(9) 0.0236(5) Uani 1 d . . . S2 S 0.3690(2) 0.64433(18) 0.15401(9) 0.0267(6) Uani 1 d . . . S14 S 0.8155(2) 1.00696(18) -0.11189(9) 0.0231(5) Uani 1 d . . . S12 S 0.6375(2) 1.06947(18) 0.00493(9) 0.0238(5) Uani 1 d . . . S1 S 0.5468(2) 0.82316(19) 0.19435(9) 0.0296(6) Uani 1 d . . . S9 S 0.6643(2) 1.27261(18) 0.15287(9) 0.0257(5) Uani 1 d . . . Cr1 Cr 0.47963(14) 1.31381(12) 0.34773(6) 0.0280(4) Uani 1 d . . . S15 S 1.1505(2) 1.11085(18) -0.18048(10) 0.0276(6) Uani 1 d . . . S16 S 0.9467(2) 0.94920(19) -0.22375(9) 0.0298(6) Uani 1 d . . . C24 C 0.9444(7) 1.0173(6) -0.1593(3) 0.0184(18) Uani 1 d . . . O3 O 0.6286(6) 1.3423(5) 0.3020(2) 0.0326(15) Uani 1 d . . . C12 C 0.7660(8) 0.6156(6) -0.0111(3) 0.0199(19) Uani 1 d . . . O12 O 0.0836(6) 1.5882(5) 0.3124(3) 0.0383(16) Uani 1 d . . . C22 C 0.8475(7) 1.0941(6) -0.0598(3) 0.0163(18) Uani 1 d . . . C11 C 0.6873(8) 0.6439(6) 0.0375(3) 0.0180(18) Uani 1 d . . . C19 C 0.6742(7) 1.2002(6) 0.0885(3) 0.0171(18) Uani 1 d . . . C20 C 0.5983(7) 1.1366(6) 0.0717(3) 0.0178(18) Uani 1 d . . . C10 C 0.5030(8) 0.6685(7) 0.1163(3) 0.0201(19) Uani 1 d . . . C14 C 0.8725(8) 0.5344(7) -0.1083(3) 0.024(2) Uani 1 d . . . C26 C 1.0847(8) 0.9784(7) -0.2624(3) 0.028(2) Uani 1 d . . . H26A H 1.1816 0.9049 -0.2543 0.033 Uiso 1 calc R . . H26B H 1.0678 0.9773 -0.3026 0.033 Uiso 1 calc R . . C23 C 1.0198(7) 1.0812(6) -0.1415(3) 0.0181(19) Uani 1 d . . . C16 C 1.0429(9) 0.4736(8) -0.2028(4) 0.042(3) Uani 1 d . . . H16A H 1.1332 0.4057 -0.1859 0.050 Uiso 1 calc R . . H16B H 1.0474 0.4534 -0.2428 0.050 Uiso 1 calc R . . C13 C 0.9378(7) 0.6091(7) -0.0919(3) 0.0215(19) Uani 1 d . . . C17 C 0.4901(7) 1.2879(6) 0.1782(3) 0.0204(19) Uani 1 d . . . H17A H 0.4758 1.3182 0.2171 0.025 Uiso 1 calc R . . H17B H 0.4123 1.3571 0.1559 0.025 Uiso 1 calc R . . C21 C 0.7721(8) 1.1203(6) -0.0111(3) 0.0210(19) Uani 1 d . . . O4 O 0.4939(6) 1.4478(5) 0.3949(2) 0.0348(16) Uani 1 d . . . C18 C 0.4733(8) 1.1611(6) 0.1762(3) 0.023(2) Uani 1 d . . . H18A H 0.3844 1.1730 0.1976 0.028 Uiso 1 calc R . . H18B H 0.5578 1.0890 0.1945 0.028 Uiso 1 calc R . . C9 C 0.5706(8) 0.7394(7) 0.1320(3) 0.026(2) Uani 1 d . . . O2 O 0.6297(6) 1.1687(5) 0.3914(2) 0.0322(15) Uani 1 d . . . O6 O 0.3226(6) 1.4535(5) 0.3054(2) 0.0301(14) Uani 1 d . . . O11 O 0.0801(6) 1.4490(5) 0.4094(3) 0.0461(18) Uani 1 d . . . O10 O 0.5827(6) 1.5980(5) 0.3930(3) 0.0455(18) Uani 1 d . . . O1 O 0.4828(6) 1.1669(5) 0.3040(2) 0.0375(16) Uani 1 d . . . C15 C 1.0427(11) 0.6033(8) -0.1979(4) 0.052(3) Uani 1 d . . . H15A H 0.9501 0.6719 -0.2130 0.063 Uiso 1 calc R . . H15B H 1.1230 0.6043 -0.2215 0.063 Uiso 1 calc R . . C3 C 0.6558(9) 1.4354(8) 0.3198(4) 0.034(2) Uani 1 d . . . C7 C 0.4598(11) 0.7467(8) 0.2394(4) 0.050(3) Uani 1 d . . . H7A H 0.5181 0.7162 0.2735 0.060 Uiso 1 calc R . . H7B H 0.3632 0.8172 0.2505 0.060 Uiso 1 calc R . . C5 C 0.1942(10) 1.4166(8) 0.3815(4) 0.034(2) Uani 1 d . . . O8 O 0.7629(7) 0.9483(5) 0.3889(3) 0.056(2) Uani 1 d . . . C1 C 0.5710(10) 1.0492(8) 0.3229(4) 0.038(2) Uani 1 d . . . C8 C 0.4375(11) 0.6380(9) 0.2204(4) 0.061(3) Uani 1 d . . . H8A H 0.3704 0.6240 0.2473 0.074 Uiso 1 calc R . . H8B H 0.5322 0.5579 0.2224 0.074 Uiso 1 calc R . . O9 O 0.7404(6) 1.4746(6) 0.2986(3) 0.0482(18) Uani 1 d . . . O7 O 0.5837(6) 0.9442(5) 0.3057(3) 0.0466(18) Uani 1 d . . . C25 C 1.0865(9) 1.1094(7) -0.2491(3) 0.031(2) Uani 1 d . . . H25A H 0.9866 1.1820 -0.2526 0.037 Uiso 1 calc R . . H25B H 1.1500 1.1268 -0.2766 0.037 Uiso 1 calc R . . C4 C 0.5716(9) 1.5019(8) 0.3734(4) 0.036(2) Uani 1 d . . . C6 C 0.1957(10) 1.4952(8) 0.3287(4) 0.027(2) Uani 1 d . . . C2 C 0.6634(10) 1.0526(9) 0.3710(4) 0.040(3) Uani 1 d . . . O5 O 0.3175(6) 1.3196(5) 0.3949(2) 0.0318(15) Uani 1 d . . . C27 C 0.7759(10) 1.0808(10) -0.3713(4) 0.062(3) Uani 1 d . . . H27A H 0.7574 1.0740 -0.3310 0.074 Uiso 1 calc R . . H27B H 0.6945 1.0790 -0.3919 0.074 Uiso 1 calc R . . C32 C -0.0586(12) 1.2530(9) 0.3978(5) 0.058(3) Uani 1 d . . . H32A H -0.0766 1.3431 0.3846 0.070 Uiso 1 calc R . . H32B H -0.1387 1.2343 0.3849 0.070 Uiso 1 calc R . . C31 C -0.1819(11) 1.3520(8) 0.4813(5) 0.067(4) Uani 1 d . . . H31A H -0.2710 1.3516 0.4665 0.080 Uiso 1 calc R . . H31B H -0.1829 1.4388 0.4718 0.080 Uiso 1 calc R . . C28 C 0.9160(11) 0.8471(9) -0.3754(4) 0.056(3) Uani 1 d . . . H28A H 0.8344 0.8387 -0.3933 0.067 Uiso 1 calc R . . H28B H 0.9088 0.8343 -0.3349 0.067 Uiso 1 calc R . . C29 C 0.2106(12) 1.7949(10) 0.3843(5) 0.076(4) Uani 1 d . . . H29A H 0.1207 1.7997 0.3679 0.091 Uiso 1 calc R . . H29B H 0.2952 1.7181 0.3683 0.091 Uiso 1 calc R . . C30 C 0.1789(13) 1.6677(10) 0.4583(6) 0.080(4) Uani 1 d . . . H30A H 0.2541 1.5869 0.4407 0.096 Uiso 1 calc R . . H30B H 0.0825 1.6823 0.4445 0.096 Uiso 1 calc R . . O13 O 0.9107(6) 0.9746(5) -0.3877(3) 0.0479(18) Uani 1 d . . . O14 O 0.2055(7) 1.7788(6) 0.4431(3) 0.057(2) Uani 1 d . . . O15 O -0.0534(7) 1.2455(5) 0.4571(3) 0.0516(19) Uani 1 d . . . O1W O 0.8043(7) 0.6821(6) 0.3690(3) 0.068(2) Uani 1 d . . . O2W O 0.2029(7) 1.2861(6) 0.5108(3) 0.072(2) Uani 1 d . . . O3W O 0.5060(10) 1.7384(9) 0.4950(4) 0.125(3) Uani 1 d . . . O4W O 1.0701(16) 1.0051(12) -0.4800(6) 0.075(5) Uani 0.50 d P . . O5WA O 0.7552(19) 0.9896(13) 0.4963(7) 0.088(5) Uani 0.50 d P . . O5WB O 0.562(2) 0.999(2) 0.5151(9) 0.123(8) Uani 0.50 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S4 0.0277(13) 0.0257(11) 0.0328(16) -0.0067(10) 0.0095(11) -0.0189(10) S8 0.0271(13) 0.0372(12) 0.0311(16) -0.0167(11) 0.0117(11) -0.0202(11) S5 0.0246(12) 0.0315(11) 0.0237(15) -0.0039(10) 0.0037(10) -0.0178(10) S6 0.0302(13) 0.0260(11) 0.0262(15) -0.0069(10) 0.0083(11) -0.0180(10) S3 0.0291(13) 0.0366(12) 0.0225(15) -0.0062(10) 0.0059(10) -0.0236(11) S7 0.0538(16) 0.0611(15) 0.0334(17) -0.0174(13) 0.0205(13) -0.0472(14) S13 0.0218(12) 0.0270(11) 0.0246(14) -0.0050(9) 0.0046(10) -0.0152(10) S10 0.0270(13) 0.0340(11) 0.0243(14) -0.0034(10) 0.0052(10) -0.0205(10) S11 0.0229(12) 0.0295(11) 0.0234(14) -0.0040(10) 0.0039(10) -0.0161(10) S2 0.0299(13) 0.0300(11) 0.0281(15) -0.0083(10) 0.0129(11) -0.0208(10) S14 0.0248(12) 0.0268(11) 0.0225(14) -0.0045(10) 0.0054(10) -0.0158(10) S12 0.0227(12) 0.0288(11) 0.0243(15) -0.0062(10) 0.0045(10) -0.0152(10) S1 0.0393(14) 0.0368(12) 0.0236(15) -0.0078(10) 0.0085(11) -0.0269(11) S9 0.0254(12) 0.0297(11) 0.0263(15) -0.0075(10) 0.0065(10) -0.0160(10) Cr1 0.0349(9) 0.0229(7) 0.0250(10) 0.0003(6) 0.0033(7) -0.0119(7) S15 0.0260(12) 0.0270(11) 0.0334(16) -0.0035(10) 0.0096(11) -0.0153(10) S16 0.0395(14) 0.0341(12) 0.0219(15) -0.0060(10) 0.0053(11) -0.0219(11) C24 0.016(4) 0.021(4) 0.016(5) -0.004(3) 0.004(4) -0.006(4) O3 0.032(3) 0.031(3) 0.031(4) 0.000(3) 0.005(3) -0.011(3) C12 0.025(5) 0.021(4) 0.022(5) -0.006(4) 0.004(4) -0.017(4) O12 0.032(4) 0.032(3) 0.046(5) 0.007(3) -0.009(3) -0.010(3) C22 0.017(4) 0.020(4) 0.012(5) 0.001(3) 0.003(4) -0.008(4) C11 0.017(4) 0.023(4) 0.018(5) 0.002(4) -0.008(4) -0.011(4) C19 0.017(4) 0.019(4) 0.015(5) -0.004(3) 0.009(4) -0.008(4) C20 0.015(4) 0.020(4) 0.019(5) 0.000(3) -0.002(4) -0.008(4) C10 0.027(5) 0.022(4) 0.014(5) 0.002(3) 0.000(4) -0.013(4) C14 0.024(5) 0.026(4) 0.025(6) -0.006(4) 0.007(4) -0.013(4) C26 0.028(5) 0.035(5) 0.019(6) 0.001(4) 0.010(4) -0.013(4) C23 0.018(4) 0.014(4) 0.019(5) -0.005(3) 0.007(4) -0.003(4) C16 0.049(6) 0.063(6) 0.033(7) -0.006(5) 0.008(5) -0.042(5) C13 0.011(4) 0.028(4) 0.021(6) 0.006(4) 0.000(4) -0.005(4) C17 0.019(5) 0.019(4) 0.018(5) -0.011(4) 0.011(4) -0.004(4) C21 0.024(5) 0.018(4) 0.020(6) 0.003(4) -0.002(4) -0.009(4) O4 0.040(4) 0.031(3) 0.038(4) -0.012(3) 0.012(3) -0.019(3) C18 0.018(5) 0.016(4) 0.035(6) -0.004(4) 0.006(4) -0.007(4) C9 0.025(5) 0.025(4) 0.030(6) 0.001(4) 0.004(4) -0.014(4) O2 0.036(4) 0.024(3) 0.033(4) 0.003(3) 0.003(3) -0.011(3) O6 0.026(3) 0.027(3) 0.029(4) 0.009(3) 0.002(3) -0.005(3) O11 0.041(4) 0.042(4) 0.056(5) -0.003(3) 0.020(4) -0.021(3) O10 0.050(4) 0.043(3) 0.059(5) -0.005(3) 0.001(4) -0.035(3) O1 0.040(4) 0.025(3) 0.041(5) -0.002(3) 0.006(3) -0.009(3) C15 0.085(8) 0.046(6) 0.036(7) -0.014(5) 0.027(6) -0.039(6) C3 0.022(5) 0.044(5) 0.029(6) 0.009(5) -0.001(4) -0.008(5) C7 0.091(8) 0.054(6) 0.025(7) -0.002(5) 0.009(6) -0.052(6) C5 0.042(6) 0.033(5) 0.036(7) -0.005(5) 0.006(5) -0.025(5) O8 0.043(4) 0.029(3) 0.085(6) 0.006(4) -0.005(4) -0.005(3) C1 0.045(6) 0.034(5) 0.036(7) -0.006(5) 0.017(5) -0.020(5) C8 0.097(9) 0.093(8) 0.038(8) 0.016(6) -0.013(6) -0.081(7) O9 0.039(4) 0.072(4) 0.039(5) 0.009(4) 0.009(3) -0.030(4) O7 0.061(4) 0.029(3) 0.050(5) -0.008(3) 0.012(4) -0.020(3) C25 0.037(5) 0.032(5) 0.027(6) -0.003(4) 0.014(4) -0.020(4) C4 0.037(6) 0.040(5) 0.035(7) 0.011(5) -0.008(5) -0.020(5) C6 0.035(6) 0.022(4) 0.027(6) -0.004(4) -0.006(5) -0.014(4) C2 0.033(6) 0.033(5) 0.049(8) 0.001(5) 0.020(5) -0.011(5) O5 0.040(4) 0.025(3) 0.031(4) 0.004(3) 0.005(3) -0.016(3) C27 0.044(7) 0.092(8) 0.037(8) -0.005(6) 0.011(6) -0.018(7) C32 0.083(9) 0.043(6) 0.060(9) 0.019(6) -0.032(7) -0.037(6) C31 0.073(8) 0.008(5) 0.098(11) 0.022(6) -0.023(8) 0.001(5) C28 0.071(8) 0.081(8) 0.036(8) 0.005(6) 0.000(6) -0.052(7) C29 0.069(9) 0.066(8) 0.058(10) -0.035(7) -0.007(7) 0.004(7) C30 0.082(9) 0.043(7) 0.103(13) -0.023(7) 0.006(9) -0.015(7) O13 0.041(4) 0.036(4) 0.062(5) -0.013(3) -0.003(4) -0.012(3) O14 0.049(4) 0.040(4) 0.070(6) -0.014(4) -0.001(4) -0.008(3) O15 0.067(5) 0.029(3) 0.055(6) 0.005(3) -0.009(4) -0.018(4) O1W 0.060(5) 0.055(4) 0.094(7) 0.007(4) 0.001(4) -0.031(4) O2W 0.088(6) 0.091(5) 0.047(6) 0.014(4) 0.007(4) -0.051(5) O3W 0.119(8) 0.173(9) 0.070(8) -0.023(7) 0.003(6) -0.053(7) O4W 0.100(13) 0.034(7) 0.077(13) 0.000(7) -0.021(10) -0.015(8) O5WA 0.147(16) 0.066(10) 0.061(12) 0.011(8) -0.038(11) -0.054(11) O5WB 0.16(3) 0.113(12) 0.09(2) -0.033(13) 0.028(16) -0.059(17) _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 S4 C11 1.736(7) . ? S4 C10 1.753(8) . ? S8 C14 1.751(8) . ? S8 C16 1.767(7) . ? S5 C13 1.740(8) . ? S5 C12 1.747(6) . ? S6 C12 1.722(7) . ? S6 C14 1.741(7) . ? S3 C11 1.739(7) . ? S3 C9 1.748(7) . ? S7 C13 1.747(7) . ? S7 C15 1.791(9) . ? S13 C23 1.731(8) . ? S13 C22 1.742(6) . ? S10 C20 1.745(7) . ? S10 C18 1.809(8) . ? S11 C21 1.752(8) . ? S11 C19 1.759(7) . ? S2 C10 1.737(7) . ? S2 C8 1.750(10) . ? S14 C22 1.735(7) . ? S14 C24 1.760(7) . ? S12 C21 1.738(7) . ? S12 C20 1.755(8) . ? S1 C9 1.749(8) . ? S1 C7 1.811(8) . ? S9 C19 1.751(7) . ? S9 C17 1.802(6) . ? Cr1 O5 1.961(5) . ? Cr1 O6 1.964(5) . ? Cr1 O4 1.968(5) . ? Cr1 O1 1.969(5) . ? Cr1 O2 1.976(5) . ? Cr1 O3 1.987(5) . ? S15 C23 1.756(7) . ? S15 C25 1.798(9) . ? S16 C24 1.746(8) . ? S16 C26 1.812(7) . ? C24 C23 1.348(9) . ? O3 C3 1.282(9) . ? C12 C11 1.365(10) . ? O12 C6 1.226(9) . ? C22 C21 1.353(10) . ? C19 C20 1.341(9) . ? C10 C9 1.330(9) . ? C14 C13 1.353(9) . ? C26 C25 1.521(9) . ? C16 C15 1.464(9) . ? C17 C18 1.509(8) . ? O4 C4 1.286(8) . ? O2 C2 1.299(9) . ? O6 C6 1.286(9) . ? O11 C5 1.240(9) . ? O10 C4 1.239(9) . ? O1 C1 1.306(9) . ? C3 O9 1.225(9) . ? C3 C4 1.547(12) . ? C7 C8 1.426(10) . ? C5 O5 1.292(9) . ? C5 C6 1.532(11) . ? O8 C2 1.239(10) . ? C1 O7 1.212(8) . ? C1 C2 1.528(13) . ? C27 O13 1.422(10) . ? C27 C29 1.485(12) 2_685 ? C32 O15 1.432(11) . ? C32 C28 1.489(12) 2_675 ? C31 O15 1.450(11) . ? C31 C30 1.465(14) 2_586 ? C28 O13 1.432(9) . ? C28 C32 1.489(12) 2_675 ? C29 O14 1.426(12) . ? C29 C27 1.485(12) 2_685 ? C30 O14 1.425(11) . ? C30 C31 1.465(14) 2_586 ? O5WB O5WB 1.47(4) 2_676 ? 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 C11 S4 C10 94.9(3) . . ? C14 S8 C16 102.3(4) . . ? C13 S5 C12 94.7(3) . . ? C12 S6 C14 95.8(3) . . ? C11 S3 C9 95.0(4) . . ? C13 S7 C15 101.2(4) . . ? C23 S13 C22 95.3(3) . . ? C20 S10 C18 101.7(3) . . ? C21 S11 C19 95.5(3) . . ? C10 S2 C8 97.8(4) . . ? C22 S14 C24 95.5(3) . . ? C21 S12 C20 95.6(3) . . ? C9 S1 C7 103.0(4) . . ? C19 S9 C17 100.2(3) . . ? O5 Cr1 O6 83.3(2) . . ? O5 Cr1 O4 89.2(2) . . ? O6 Cr1 O4 90.7(2) . . ? O5 Cr1 O1 92.3(2) . . ? O6 Cr1 O1 94.8(2) . . ? O4 Cr1 O1 174.4(3) . . ? O5 Cr1 O2 93.9(2) . . ? O6 Cr1 O2 176.7(2) . . ? O4 Cr1 O2 91.0(2) . . ? O1 Cr1 O2 83.5(2) . . ? O5 Cr1 O3 169.9(2) . . ? O6 Cr1 O3 90.6(2) . . ? O4 Cr1 O3 82.8(2) . . ? O1 Cr1 O3 96.3(2) . . ? O2 Cr1 O3 92.5(2) . . ? C23 S15 C25 99.3(4) . . ? C24 S16 C26 102.8(4) . . ? C23 C24 S16 130.3(6) . . ? C23 C24 S14 115.9(6) . . ? S16 C24 S14 113.7(4) . . ? C3 O3 Cr1 113.4(5) . . ? C11 C12 S6 123.2(5) . . ? C11 C12 S5 121.4(5) . . ? S6 C12 S5 115.4(4) . . ? C21 C22 S14 122.1(5) . . ? C21 C22 S13 122.8(6) . . ? S14 C22 S13 115.1(4) . . ? C12 C11 S4 122.5(5) . . ? C12 C11 S3 122.3(5) . . ? S4 C11 S3 115.2(4) . . ? C20 C19 S9 128.1(6) . . ? C20 C19 S11 116.7(6) . . ? S9 C19 S11 115.1(4) . . ? C19 C20 S10 129.2(6) . . ? C19 C20 S12 117.4(5) . . ? S10 C20 S12 113.4(4) . . ? C9 C10 S2 126.2(6) . . ? C9 C10 S4 117.3(6) . . ? S2 C10 S4 116.4(4) . . ? C13 C14 S6 116.4(6) . . ? C13 C14 S8 127.8(6) . . ? S6 C14 S8 115.8(4) . . ? C25 C26 S16 113.6(5) . . ? C24 C23 S13 118.1(5) . . ? C24 C23 S15 125.7(6) . . ? S13 C23 S15 116.0(4) . . ? C15 C16 S8 116.3(6) . . ? C14 C13 S5 117.6(6) . . ? C14 C13 S7 128.1(6) . . ? S5 C13 S7 114.3(4) . . ? C18 C17 S9 114.2(4) . . ? C22 C21 S12 123.3(6) . . ? C22 C21 S11 121.9(5) . . ? S12 C21 S11 114.7(4) . . ? C4 O4 Cr1 114.0(5) . . ? C17 C18 S10 113.8(5) . . ? C10 C9 S1 127.6(6) . . ? C10 C9 S3 117.3(6) . . ? S1 C9 S3 115.0(4) . . ? C2 O2 Cr1 112.4(6) . . ? C6 O6 Cr1 114.2(5) . . ? C1 O1 Cr1 113.9(6) . . ? C16 C15 S7 115.9(7) . . ? O9 C3 O3 126.4(9) . . ? O9 C3 C4 118.7(8) . . ? O3 C3 C4 114.9(7) . . ? C8 C7 S1 120.1(7) . . ? O11 C5 O5 123.7(8) . . ? O11 C5 C6 120.3(8) . . ? O5 C5 C6 116.0(7) . . ? O7 C1 O1 126.1(9) . . ? O7 C1 C2 120.5(9) . . ? O1 C1 C2 113.5(7) . . ? C7 C8 S2 120.0(7) . . ? C26 C25 S15 112.9(6) . . ? O10 C4 O4 124.9(8) . . ? O10 C4 C3 120.9(7) . . ? O4 C4 C3 114.2(7) . . ? O12 C6 O6 126.0(8) . . ? O12 C6 C5 120.7(8) . . ? O6 C6 C5 113.3(7) . . ? O8 C2 O2 123.7(10) . . ? O8 C2 C1 120.1(8) . . ? O2 C2 C1 116.2(8) . . ? C5 O5 Cr1 112.4(5) . . ? O13 C27 C29 106.3(8) . 2_685 ? O15 C32 C28 108.1(8) . 2_675 ? O15 C31 C30 108.7(8) . 2_586 ? O13 C28 C32 106.4(7) . 2_675 ? O14 C29 C27 108.9(8) . 2_685 ? O14 C30 C31 111.0(9) . 2_586 ? C27 O13 C28 112.6(7) . . ? C30 O14 C29 111.6(9) . . ? C32 O15 C31 110.7(8) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.569 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.104