Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Zofia Janas' _publ_contact_author_address ; Faculty of Chemistry University of Wroclaw F. Joliot-Curie 14 Wroclaw 50-383 POLAND ; _publ_contact_author_email ZJ@WCHUWR.CHEM.UNI.WROC.PL _publ_section_title ; Synthesis, structural studies and reactivity of vanadium complexes with tridentate (OSO) ligand ; loop_ _publ_author_name 'Zofia Janas' 'Krzysztof Drabent' 'Lucjan Jerzykiewicz' 'Piotr Sobota' 'Krzysztof Szczegot' ; D.Wisniewska ; data_(1)4CH3CN_ZJ48 _database_code_depnum_ccdc_archive 'CCDC 604895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H86 Cl2 N2 O4 S2 V2, 4(C2 H3 N)' _chemical_formula_sum 'C68 H98 Cl2 N6 O4 S2 V2' _chemical_formula_weight 1300.44 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.480(3) _cell_length_b 14.312(5) _cell_length_c 15.312(7) _cell_angle_alpha 93.17(3) _cell_angle_beta 93.88(3) _cell_angle_gamma 102.56(3) _cell_volume 1805.0(12) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 0.438 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.483 _exptl_absorpt_correction_T_max 0.833 _exptl_absorpt_process_details ; Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998) I/sigma threshold for reflections = 5.000 Delta(U)/lambda**2 = 0.000 Highest even order spherical harmonic = 6 Highest odd order spherical harmonic = 3 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Kuma KM4 automatic diffractometer' _diffrn_measurement_method 'profile data from omega-2theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.6 _diffrn_reflns_number 6873 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 25.08 _reflns_number_total 6402 _reflns_number_gt 4695 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM4 software 1996' _computing_cell_refinement 'Kuma KM4 software 1996' _computing_data_reduction 'Kuma KM4 software 1996' _computing_structure_solution 'SHELXTL-NT V5.1, Bruker AXS 1999' _computing_structure_refinement 'SHELXTL-NT V5.1, Bruker AXS 1999' _computing_molecular_graphics 'SHELXTL-NT V5.1, Bruker AXS 1999' _computing_publication_material 'SHELXTL-NT V5.1, Bruker AXS 1999' _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^)+(0.1285P)^2^+0.6258P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6402 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1723 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.14306(6) 0.94723(3) 0.50835(3) 0.01192(17) Uani 1 1 d . . . Cl1 Cl 0.32160(9) 0.90714(6) 0.61338(5) 0.0212(2) Uani 1 1 d . . . S1 S 0.28967(8) 0.91402(5) 0.37995(4) 0.01144(19) Uani 1 1 d . . . O1 O 0.0306(2) 1.01350(14) 0.42009(13) 0.0135(4) Uani 1 1 d . . . O2 O 0.0149(3) 0.82396(15) 0.47888(14) 0.0158(4) Uani 1 1 d . . . N1 N 0.2972(3) 1.08981(19) 0.52655(17) 0.0181(6) Uani 1 1 d . . . N2 N 0.4963(4) 0.1546(2) 0.8423(2) 0.0324(7) Uani 1 1 d . . . C1 C 0.3798(4) 1.1628(2) 0.5178(2) 0.0237(7) Uani 1 1 d . . . C2 C 0.4842(5) 1.2554(3) 0.5045(3) 0.0414(10) Uani 1 1 d . . . H2A H 0.5616 1.2763 0.5560 0.062 Uiso 1 1 calc R . . H2B H 0.4179 1.3028 0.4960 0.062 Uiso 1 1 calc R . . H2C H 0.5434 1.2493 0.4524 0.062 Uiso 1 1 calc R . . C3 C 0.3692(4) 0.1387(2) 0.8088(2) 0.0226(7) Uani 1 1 d . . . C4 C 0.2051(5) 0.1185(3) 0.7666(3) 0.0406(10) Uani 1 1 d . . . H4A H 0.1307 0.0804 0.8041 0.061 Uiso 1 1 calc R . . H4B H 0.2019 0.0825 0.7099 0.061 Uiso 1 1 calc R . . H4C H 0.1723 0.1790 0.7573 0.061 Uiso 1 1 calc R . . C11 C 0.2211(3) 0.99900(19) 0.31509(18) 0.0109(6) Uani 1 1 d . . . C12 C 0.0997(3) 1.0424(2) 0.34599(19) 0.0129(6) Uani 1 1 d . . . C13 C 0.0538(4) 1.1126(2) 0.2962(2) 0.0171(6) Uani 1 1 d . . . H13 H -0.0220 1.1469 0.3170 0.020 Uiso 1 1 calc R . . C14 C 0.1179(4) 1.1324(2) 0.2170(2) 0.0161(6) Uani 1 1 d . . . H14 H 0.0817 1.1788 0.1836 0.019 Uiso 1 1 calc R . . C15 C 0.2336(4) 1.0871(2) 0.18408(19) 0.0135(6) Uani 1 1 d . . . C16 C 0.2865(3) 1.0209(2) 0.23656(19) 0.0125(6) Uani 1 1 d . . . H16 H 0.3687 0.9905 0.2178 0.015 Uiso 1 1 calc R . . C21 C 0.1426(3) 0.8062(2) 0.3459(2) 0.0129(6) Uani 1 1 d . . . C22 C 0.0240(4) 0.7741(2) 0.4030(2) 0.0153(6) Uani 1 1 d . . . C23 C -0.0883(4) 0.6882(2) 0.3768(2) 0.0197(7) Uani 1 1 d . . . H23 H -0.1704 0.6636 0.4140 0.024 Uiso 1 1 calc R . . C24 C -0.0812(4) 0.6387(2) 0.2974(2) 0.0202(7) Uani 1 1 d . . . H24 H -0.1588 0.5806 0.2814 0.024 Uiso 1 1 calc R . . C25 C 0.0374(4) 0.6718(2) 0.2396(2) 0.0155(6) Uani 1 1 d . . . C26 C 0.1492(4) 0.7572(2) 0.26619(19) 0.0142(6) Uani 1 1 d . . . H26 H 0.2312 0.7821 0.2290 0.017 Uiso 1 1 calc R . . C150 C 0.2962(4) 1.1018(2) 0.09340(19) 0.0143(6) Uani 1 1 d . . . C151 C 0.4834(4) 1.1283(2) 0.0970(2) 0.0154(6) Uani 1 1 d . . . H15A H 0.5129 1.1183 0.0363 0.019 Uiso 1 1 calc R . . H15B H 0.5227 1.0803 0.1315 0.019 Uiso 1 1 calc R . . C152 C 0.5841(4) 1.2281(2) 0.1335(2) 0.0183(7) Uani 1 1 d . . . C153 C 0.2190(4) 1.1734(2) 0.0445(2) 0.0170(6) Uani 1 1 d . . . H15C H 0.1017 1.1480 0.0343 0.026 Uiso 1 1 calc R . . H15D H 0.2658 1.1834 -0.0120 0.026 Uiso 1 1 calc R . . H15E H 0.2400 1.2347 0.0798 0.026 Uiso 1 1 calc R . . C154 C 0.2430(4) 1.0036(2) 0.0394(2) 0.0206(7) Uani 1 1 d . . . H15F H 0.2984 0.9573 0.0656 0.031 Uiso 1 1 calc R . . H15G H 0.2716 1.0112 -0.0211 0.031 Uiso 1 1 calc R . . H15H H 0.1255 0.9803 0.0397 0.031 Uiso 1 1 calc R . . C155 C 0.7607(4) 1.2164(3) 0.1458(3) 0.0284(8) Uani 1 1 d . . . H15I H 0.8322 1.2785 0.1655 0.043 Uiso 1 1 calc R . . H15J H 0.7931 1.1930 0.0899 0.043 Uiso 1 1 calc R . . H15K H 0.7690 1.1702 0.1899 0.043 Uiso 1 1 calc R . . C156 C 0.5800(4) 1.3053(2) 0.0679(2) 0.0242(7) Uani 1 1 d . . . H15L H 0.4734 1.3215 0.0652 0.036 Uiso 1 1 calc R . . H15M H 0.6000 1.2806 0.0096 0.036 Uiso 1 1 calc R . . H15N H 0.6640 1.3628 0.0870 0.036 Uiso 1 1 calc R . . C157 C 0.5364(4) 1.2610(2) 0.2222(2) 0.0221(7) Uani 1 1 d . . . H15O H 0.5399 1.2114 0.2635 0.033 Uiso 1 1 calc R . . H15P H 0.4264 1.2722 0.2155 0.033 Uiso 1 1 calc R . . H15Q H 0.6123 1.3207 0.2447 0.033 Uiso 1 1 calc R . . C250 C 0.0464(4) 0.6212(2) 0.1503(2) 0.0191(7) Uani 1 1 d . . . C251 C 0.2164(4) 0.6017(2) 0.1380(2) 0.0207(7) Uani 1 1 d . . . H25A H 0.2120 0.5740 0.0770 0.025 Uiso 1 1 calc R . . H25B H 0.2918 0.6655 0.1409 0.025 Uiso 1 1 calc R . . C252 C 0.3001(4) 0.5391(3) 0.1958(3) 0.0295(8) Uani 1 1 d . . . C253 C 0.0170(5) 0.6896(3) 0.0792(2) 0.0293(8) Uani 1 1 d . . . H25C H 0.0234 0.6592 0.0210 0.044 Uiso 1 1 calc R . . H25D H 0.0997 0.7496 0.0886 0.044 Uiso 1 1 calc R . . H25E H -0.0907 0.7034 0.0830 0.044 Uiso 1 1 calc R . . C254 C -0.0871(4) 0.5288(2) 0.1322(2) 0.0243(7) Uani 1 1 d . . . H25F H -0.0817 0.4870 0.1804 0.037 Uiso 1 1 calc R . . H25G H -0.0712 0.4953 0.0771 0.037 Uiso 1 1 calc R . . H25H H -0.1935 0.5453 0.1278 0.037 Uiso 1 1 calc R . . C255 C 0.3325(8) 0.5785(4) 0.2911(3) 0.073(2) Uani 1 1 d . . . H25I H 0.2293 0.5740 0.3176 0.110 Uiso 1 1 calc R . . H25J H 0.3909 0.6459 0.2939 0.110 Uiso 1 1 calc R . . H25K H 0.3983 0.5412 0.3232 0.110 Uiso 1 1 calc R . . C256 C 0.2093(6) 0.4343(3) 0.1883(4) 0.0618(16) Uani 1 1 d . . . H25L H 0.2808 0.3945 0.2114 0.093 Uiso 1 1 calc R . . H25M H 0.1749 0.4138 0.1265 0.093 Uiso 1 1 calc R . . H25N H 0.1138 0.4272 0.2221 0.093 Uiso 1 1 calc R . . C257 C 0.4653(5) 0.5426(4) 0.1605(4) 0.0580(14) Uani 1 1 d . . . H25O H 0.5272 0.6092 0.1641 0.087 Uiso 1 1 calc R . . H25P H 0.4501 0.5166 0.0992 0.087 Uiso 1 1 calc R . . H25Q H 0.5247 0.5041 0.1955 0.087 Uiso 1 1 calc R . . N3 N 0.7410(12) 1.4625(5) 0.4619(6) 0.130(3) Uani 1 1 d . . . C5 C 0.8322(11) 1.4193(5) 0.4345(5) 0.086(2) Uani 1 1 d . . . C6 C 0.9408(10) 1.3631(5) 0.3981(4) 0.084(2) Uani 1 1 d . . . H6A H 0.9212 1.2999 0.4222 0.127 Uiso 1 1 calc R . . H6B H 1.0537 1.3968 0.4137 0.127 Uiso 1 1 calc R . . H6C H 0.9203 1.3551 0.3341 0.127 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0113(3) 0.0138(3) 0.0115(3) 0.00006(19) -0.00523(19) 0.0065(2) Cl1 0.0173(4) 0.0294(4) 0.0191(4) 0.0061(3) -0.0058(3) 0.0114(3) S1 0.0109(4) 0.0109(4) 0.0129(4) 0.0009(3) -0.0047(3) 0.0052(3) O1 0.0120(10) 0.0176(10) 0.0126(10) -0.0005(8) -0.0032(8) 0.0084(8) O2 0.0167(11) 0.0156(10) 0.0152(11) 0.0005(8) -0.0002(8) 0.0044(8) N1 0.0162(13) 0.0229(15) 0.0150(13) -0.0032(10) -0.0072(10) 0.0072(12) N2 0.0242(17) 0.0378(18) 0.0353(18) 0.0006(14) -0.0025(14) 0.0093(14) C1 0.0188(16) 0.0236(18) 0.0283(18) -0.0042(14) -0.0034(14) 0.0074(15) C2 0.036(2) 0.027(2) 0.056(3) -0.0061(18) 0.0064(19) -0.0029(17) C3 0.0264(19) 0.0182(16) 0.0233(17) -0.0003(13) -0.0014(14) 0.0067(14) C4 0.029(2) 0.046(2) 0.043(2) -0.0090(19) -0.0169(17) 0.0079(18) C11 0.0128(14) 0.0087(13) 0.0110(13) -0.0016(10) -0.0062(11) 0.0043(11) C12 0.0120(14) 0.0131(14) 0.0133(14) 0.0000(11) -0.0043(11) 0.0041(11) C13 0.0157(15) 0.0174(15) 0.0211(16) 0.0000(12) -0.0031(12) 0.0118(12) C14 0.0162(15) 0.0134(14) 0.0202(16) 0.0049(11) -0.0063(12) 0.0082(12) C15 0.0148(14) 0.0117(14) 0.0137(15) 0.0033(11) -0.0050(11) 0.0032(11) C16 0.0089(13) 0.0105(13) 0.0185(15) -0.0008(11) -0.0037(11) 0.0050(11) C21 0.0095(13) 0.0095(13) 0.0194(15) 0.0002(11) -0.0063(11) 0.0039(11) C22 0.0174(15) 0.0143(14) 0.0155(15) 0.0009(11) -0.0038(11) 0.0080(12) C23 0.0176(16) 0.0173(15) 0.0235(17) 0.0037(13) 0.0014(13) 0.0020(13) C24 0.0174(16) 0.0149(15) 0.0263(17) -0.0014(12) -0.0043(13) 0.0016(12) C25 0.0148(15) 0.0144(14) 0.0188(16) 0.0002(12) -0.0039(12) 0.0081(12) C26 0.0146(14) 0.0144(14) 0.0151(14) 0.0027(11) -0.0034(11) 0.0077(12) C150 0.0151(15) 0.0142(15) 0.0151(15) 0.0015(11) -0.0035(11) 0.0075(12) C151 0.0172(16) 0.0141(14) 0.0170(15) 0.0035(11) -0.0008(12) 0.0079(12) C152 0.0149(15) 0.0153(15) 0.0243(16) 0.0046(12) -0.0048(12) 0.0040(12) C153 0.0189(15) 0.0195(15) 0.0151(15) 0.0049(12) -0.0043(12) 0.0104(13) C154 0.0219(17) 0.0159(15) 0.0224(16) -0.0017(12) -0.0067(13) 0.0040(13) C155 0.0153(17) 0.0297(19) 0.039(2) 0.0049(15) -0.0057(14) 0.0037(14) C156 0.0224(17) 0.0163(16) 0.0314(19) 0.0094(14) -0.0039(14) -0.0013(13) C157 0.0253(17) 0.0166(15) 0.0222(17) -0.0022(12) -0.0078(13) 0.0040(13) C250 0.0196(16) 0.0161(15) 0.0209(16) -0.0014(12) -0.0057(12) 0.0052(13) C251 0.0219(17) 0.0179(15) 0.0213(16) -0.0045(12) 0.0018(13) 0.0033(13) C252 0.0276(19) 0.0244(18) 0.039(2) -0.0049(15) -0.0043(16) 0.0147(15) C253 0.044(2) 0.0266(18) 0.0183(17) -0.0007(14) -0.0085(15) 0.0143(16) C254 0.0222(17) 0.0231(17) 0.0248(17) -0.0094(13) -0.0038(13) 0.0032(14) C255 0.106(5) 0.091(4) 0.044(3) -0.013(3) -0.032(3) 0.083(4) C256 0.042(3) 0.030(2) 0.116(5) 0.022(3) -0.013(3) 0.015(2) C257 0.031(2) 0.046(3) 0.099(4) -0.002(3) 0.001(2) 0.017(2) N3 0.153(8) 0.071(4) 0.165(8) 0.042(5) 0.054(6) 0.006(5) C5 0.109(6) 0.062(4) 0.072(4) 0.022(3) -0.010(4) -0.014(4) C6 0.114(6) 0.066(4) 0.065(4) 0.020(3) -0.012(4) 0.003(4) _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 V1 O2 1.873(2) . ? V1 O1 1.999(2) . ? V1 O1 2.048(2) 2_576 ? V1 N1 2.163(3) . ? V1 Cl1 2.3148(12) . ? V1 S1 2.4741(13) . ? S1 C11 1.779(3) . ? S1 C21 1.788(3) . ? O1 C12 1.356(4) . ? O1 V1 2.048(2) 2_576 ? O2 C22 1.345(4) . ? N1 C1 1.144(4) . ? N2 C3 1.132(5) . ? C1 C2 1.459(5) . ? C3 C4 1.457(5) . ? C11 C16 1.381(4) . ? C11 C12 1.408(4) . ? C12 C13 1.399(4) . ? C13 C14 1.380(5) . ? C14 C15 1.394(4) . ? C15 C16 1.402(4) . ? C15 C150 1.529(4) . ? C21 C26 1.385(4) . ? C21 C22 1.396(4) . ? C22 C23 1.401(4) . ? C23 C24 1.385(5) . ? C24 C25 1.406(5) . ? C25 C26 1.395(4) . ? C25 C250 1.526(4) . ? C150 C153 1.534(4) . ? C150 C151 1.546(4) . ? C150 C154 1.551(4) . ? C151 C152 1.548(4) . ? C152 C157 1.522(5) . ? C152 C156 1.538(4) . ? C152 C155 1.543(4) . ? C250 C254 1.540(4) . ? C250 C253 1.547(5) . ? C250 C251 1.548(5) . ? C251 C252 1.540(5) . ? C252 C255 1.519(6) . ? C252 C256 1.524(6) . ? C252 C257 1.528(6) . ? N3 C5 1.174(11) . ? C5 C6 1.466(12) . ? 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 V1 O1 96.21(9) . . ? O2 V1 O1 92.40(9) . 2_576 ? O1 V1 O1 78.77(9) . 2_576 ? O2 V1 N1 173.34(10) . . ? O1 V1 N1 80.13(9) . . ? O1 V1 N1 92.33(10) 2_576 . ? O2 V1 Cl1 98.05(8) . . ? O1 V1 Cl1 165.39(7) . . ? O1 V1 Cl1 103.73(7) 2_576 . ? N1 V1 Cl1 85.37(8) . . ? O2 V1 S1 84.69(8) . . ? O1 V1 S1 81.63(7) . . ? O1 V1 S1 159.76(6) 2_576 . ? N1 V1 S1 89.25(8) . . ? Cl1 V1 S1 96.51(4) . . ? C11 S1 C21 101.86(13) . . ? C11 S1 V1 94.88(10) . . ? C21 S1 V1 92.49(11) . . ? C12 O1 V1 121.18(17) . . ? C12 O1 V1 134.85(18) . 2_576 ? V1 O1 V1 101.23(9) . 2_576 ? C22 O2 V1 122.27(19) . . ? C1 N1 V1 165.8(3) . . ? N1 C1 C2 178.6(4) . . ? N2 C3 C4 179.4(4) . . ? C16 C11 C12 121.6(3) . . ? C16 C11 S1 120.1(2) . . ? C12 C11 S1 118.3(2) . . ? O1 C12 C13 123.3(3) . . ? O1 C12 C11 119.5(2) . . ? C13 C12 C11 117.2(3) . . ? C14 C13 C12 120.4(3) . . ? C13 C14 C15 122.8(3) . . ? C14 C15 C16 116.7(3) . . ? C14 C15 C150 123.7(3) . . ? C16 C15 C150 119.6(3) . . ? C11 C16 C15 121.2(3) . . ? C26 C21 C22 122.3(3) . . ? C26 C21 S1 120.4(2) . . ? C22 C21 S1 117.3(2) . . ? O2 C22 C21 121.9(3) . . ? O2 C22 C23 121.2(3) . . ? C21 C22 C23 116.9(3) . . ? C24 C23 C22 120.9(3) . . ? C23 C24 C25 122.1(3) . . ? C26 C25 C24 116.8(3) . . ? C26 C25 C250 119.4(3) . . ? C24 C25 C250 123.7(3) . . ? C21 C26 C25 121.0(3) . . ? C15 C150 C153 111.8(2) . . ? C15 C150 C151 112.5(2) . . ? C153 C150 C151 112.2(2) . . ? C15 C150 C154 106.8(2) . . ? C153 C150 C154 107.0(2) . . ? C151 C150 C154 106.0(2) . . ? C150 C151 C152 122.5(2) . . ? C157 C152 C156 110.2(3) . . ? C157 C152 C155 107.9(3) . . ? C156 C152 C155 107.3(3) . . ? C157 C152 C151 113.5(3) . . ? C156 C152 C151 112.1(3) . . ? C155 C152 C151 105.4(2) . . ? C25 C250 C254 111.9(3) . . ? C25 C250 C253 107.7(3) . . ? C254 C250 C253 107.0(3) . . ? C25 C250 C251 112.6(3) . . ? C254 C250 C251 111.5(3) . . ? C253 C250 C251 105.8(3) . . ? C252 C251 C250 124.7(3) . . ? C255 C252 C256 111.3(5) . . ? C255 C252 C257 106.7(4) . . ? C256 C252 C257 107.2(3) . . ? C255 C252 C251 112.8(3) . . ? C256 C252 C251 112.5(3) . . ? C257 C252 C251 106.0(4) . . ? N3 C5 C6 177.7(9) . . ? 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 O2 V1 S1 C11 110.99(12) . . . . ? O1 V1 S1 C11 13.90(11) . . . . ? O1 V1 S1 C11 28.5(2) 2_576 . . . ? N1 V1 S1 C11 -66.24(12) . . . . ? Cl1 V1 S1 C11 -151.49(10) . . . . ? O2 V1 S1 C21 8.86(11) . . . . ? O1 V1 S1 C21 -88.23(11) . . . . ? O1 V1 S1 C21 -73.7(2) 2_576 . . . ? N1 V1 S1 C21 -168.37(11) . . . . ? Cl1 V1 S1 C21 106.38(10) . . . . ? O2 V1 O1 C12 -104.9(2) . . . . ? O1 V1 O1 C12 163.9(2) 2_576 . . . ? N1 V1 O1 C12 69.5(2) . . . . ? Cl1 V1 O1 C12 62.4(3) . . . . ? S1 V1 O1 C12 -21.24(19) . . . . ? O2 V1 O1 V1 91.22(10) . . . 2_576 ? O1 V1 O1 V1 0.0 2_576 . . 2_576 ? N1 V1 O1 V1 -94.40(10) . . . 2_576 ? Cl1 V1 O1 V1 -101.4(2) . . . 2_576 ? S1 V1 O1 V1 174.90(8) . . . 2_576 ? O1 V1 O2 C22 70.6(2) . . . . ? O1 V1 O2 C22 149.5(2) 2_576 . . . ? N1 V1 O2 C22 14.3(9) . . . . ? Cl1 V1 O2 C22 -106.2(2) . . . . ? S1 V1 O2 C22 -10.4(2) . . . . ? O2 V1 N1 C1 4.6(16) . . . . ? O1 V1 N1 C1 -52.5(10) . . . . ? O1 V1 N1 C1 -130.7(10) 2_576 . . . ? Cl1 V1 N1 C1 125.7(10) . . . . ? S1 V1 N1 C1 29.1(10) . . . . ? V1 N1 C1 C2 10(16) . . . . ? C21 S1 C11 C16 -95.4(3) . . . . ? V1 S1 C11 C16 171.0(2) . . . . ? C21 S1 C11 C12 84.5(2) . . . . ? V1 S1 C11 C12 -9.1(2) . . . . ? V1 O1 C12 C13 -160.0(2) . . . . ? V1 O1 C12 C13 -2.6(4) 2_576 . . . ? V1 O1 C12 C11 21.7(3) . . . . ? V1 O1 C12 C11 179.08(19) 2_576 . . . ? C16 C11 C12 O1 175.1(3) . . . . ? S1 C11 C12 O1 -4.8(4) . . . . ? C16 C11 C12 C13 -3.3(4) . . . . ? S1 C11 C12 C13 176.8(2) . . . . ? O1 C12 C13 C14 -173.8(3) . . . . ? C11 C12 C13 C14 4.5(4) . . . . ? C12 C13 C14 C15 -2.2(5) . . . . ? C13 C14 C15 C16 -1.5(4) . . . . ? C13 C14 C15 C150 174.9(3) . . . . ? C12 C11 C16 C15 -0.3(4) . . . . ? S1 C11 C16 C15 179.6(2) . . . . ? C14 C15 C16 C11 2.7(4) . . . . ? C150 C15 C16 C11 -173.8(3) . . . . ? C11 S1 C21 C26 76.7(2) . . . . ? V1 S1 C21 C26 172.2(2) . . . . ? C11 S1 C21 C22 -103.8(2) . . . . ? V1 S1 C21 C22 -8.3(2) . . . . ? V1 O2 C22 C21 7.7(4) . . . . ? V1 O2 C22 C23 -170.9(2) . . . . ? C26 C21 C22 O2 -177.6(3) . . . . ? S1 C21 C22 O2 3.0(4) . . . . ? C26 C21 C22 C23 1.1(4) . . . . ? S1 C21 C22 C23 -178.4(2) . . . . ? O2 C22 C23 C24 178.1(3) . . . . ? C21 C22 C23 C24 -0.6(4) . . . . ? C22 C23 C24 C25 -0.1(5) . . . . ? C23 C24 C25 C26 0.4(4) . . . . ? C23 C24 C25 C250 -178.0(3) . . . . ? C22 C21 C26 C25 -0.8(4) . . . . ? S1 C21 C26 C25 178.6(2) . . . . ? C24 C25 C26 C21 0.1(4) . . . . ? C250 C25 C26 C21 178.6(3) . . . . ? C14 C15 C150 C153 1.1(4) . . . . ? C16 C15 C150 C153 177.4(3) . . . . ? C14 C15 C150 C151 128.5(3) . . . . ? C16 C15 C150 C151 -55.2(3) . . . . ? C14 C15 C150 C154 -115.6(3) . . . . ? C16 C15 C150 C154 60.6(3) . . . . ? C15 C150 C151 C152 -72.6(3) . . . . ? C153 C150 C151 C152 54.6(4) . . . . ? C154 C150 C151 C152 171.1(3) . . . . ? C150 C151 C152 C157 48.9(4) . . . . ? C150 C151 C152 C156 -76.8(4) . . . . ? C150 C151 C152 C155 166.8(3) . . . . ? C26 C25 C250 C254 -179.6(3) . . . . ? C24 C25 C250 C254 -1.3(4) . . . . ? C26 C25 C250 C253 -62.3(4) . . . . ? C24 C25 C250 C253 116.0(3) . . . . ? C26 C25 C250 C251 53.9(4) . . . . ? C24 C25 C250 C251 -127.7(3) . . . . ? C25 C250 C251 C252 61.0(4) . . . . ? C254 C250 C251 C252 -65.7(4) . . . . ? C253 C250 C251 C252 178.4(3) . . . . ? C250 C251 C252 C255 -62.5(5) . . . . ? C250 C251 C252 C256 64.3(5) . . . . ? C250 C251 C252 C257 -178.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C6 H6A O2 0.9800 2.5200 3.429(7) 155.00 2_676 yes C13 H13 Cl1 0.9500 2.7900 3.518(4) 134.00 2_576 yes _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.836 _refine_diff_density_min -1.058 _refine_diff_density_rms 0.116 #################################END of CIF FILE