Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Hughes, David L.' 'Davies, Sian C.' 'Konkol, Martin' 'Richards, R.' 'Sanders, J. Roger' 'Sobota, Piotr' _publ_contact_author_name 'David L Hughes' _publ_contact_author_address ; Department of Biological Chemistry John Innes Centre Norwich Research Pakr Colney Norwich NR4 7UH UNITED KINGDOM ; _publ_contact_author_email 'HUGHES@BBSRC.AC.UK' _publ_section_title ; Synthesis, structure and chemistry of vanadium(IV) and vanadium(V) compounds with substituted hydrazido(1-) and hydrazido(2-) ligands ; data_roger32 _database_code_CSD 180740 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'complex 1' _chemical_formula_moiety 'C7 H17 N3 S3 V' _chemical_formula_structural '[V(NMeNH2)(NS3)]' _chemical_formula_analytical ? _chemical_formula_sum 'C7 H17 N3 S3 V' _chemical_formula_weight 290.36 _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' 'S' 'S' 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M 'P 212121' #(no. 19) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 7.7299(11) _cell_length_b 9.736(2) _cell_length_c 16.638(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1252.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'flat needles' _exptl_crystal_colour 'brownish-orange' _exptl_crystal_size_max 0.76 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method ? _exptl_crystal_F_000 604 _exptl_absorpt_coefficient_mu 1.260 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.87 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count '10000 s' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1771 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.4 _diffrn_reflns_theta_max 25.0 _reflns_number_total 1288 _reflns_number_observed 1136 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(8) _refine_ls_number_reflns 1288 _refine_ls_number_parameters 132 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_obs 0.0549 _refine_ls_wR_factor_all 0.1358 _refine_ls_wR_factor_obs 0.1301 _refine_ls_goodness_of_fit_all 1.133 _refine_ls_goodness_of_fit_obs 1.163 _refine_ls_restrained_S_all 1.132 _refine_ls_restrained_S_obs 1.161 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V V 0.30474(13) 0.45915(10) 0.39800(6) 0.0261(3) Uani 1 d . . S1 S 0.1997(3) 0.5964(2) 0.49756(12) 0.0494(6) Uani 1 d . . S2 S 0.5968(2) 0.4449(2) 0.38125(12) 0.0428(5) Uani 1 d . . S3 S 0.1215(3) 0.3768(2) 0.30147(12) 0.0442(5) Uani 1 d . . N4 N 0.3208(8) 0.6428(6) 0.3250(3) 0.0314(13) Uani 1 d . . C14 C 0.2061(14) 0.7627(8) 0.4476(5) 0.053(2) Uani 1 d . . H14A H 0.1106(14) 0.8188(8) 0.4663(5) 0.063 Uiso 1 calc R . H14B H 0.3131(14) 0.8093(8) 0.4611(5) 0.063 Uiso 1 calc R . C41 C 0.1940(11) 0.7450(8) 0.3560(5) 0.047(2) Uani 1 d . . H41A H 0.0779(11) 0.7156(8) 0.3420(5) 0.056 Uiso 1 calc R . H41B H 0.2147(11) 0.8329(8) 0.3303(5) 0.056 Uiso 1 calc R . C24 C 0.6363(10) 0.5941(10) 0.3187(5) 0.051(2) Uani 1 d . . H24A H 0.7485(10) 0.6324(10) 0.3321(5) 0.061 Uiso 1 calc R . H24B H 0.6393(10) 0.5660(10) 0.2628(5) 0.061 Uiso 1 calc R . C42 C 0.4996(11) 0.7030(9) 0.3295(5) 0.049(2) Uani 1 d . . H42A H 0.5152(11) 0.7473(9) 0.3812(5) 0.059 Uiso 1 calc R . H42B H 0.5127(11) 0.7722(9) 0.2880(5) 0.059 Uiso 1 calc R . C34 C 0.1201(11) 0.5213(9) 0.2325(5) 0.050(2) Uani 1 d . . H34A H 0.1134(11) 0.4871(9) 0.1779(5) 0.060 Uiso 1 calc R . H34B H 0.0180(11) 0.5766(9) 0.2425(5) 0.060 Uiso 1 calc R . C43 C 0.2772(11) 0.6091(9) 0.2409(4) 0.047(2) Uani 1 d . . H43A H 0.3747(11) 0.5621(9) 0.2166(4) 0.057 Uiso 1 calc R . H43B H 0.2590(11) 0.6939(9) 0.2115(4) 0.057 Uiso 1 calc R . N5 N 0.2895(8) 0.2741(7) 0.4677(4) 0.0400(14) Uani 1 d D . C51 C 0.3346(12) 0.1435(9) 0.4264(5) 0.055(2) Uani 1 d . . H51A H 0.2673(64) 0.1348(34) 0.3782(22) 0.082 Uiso 1 calc R . H51B H 0.3104(83) 0.0675(9) 0.4614(17) 0.082 Uiso 1 calc R . H51C H 0.4554(22) 0.1438(31) 0.4130(36) 0.082 Uiso 1 calc R . N52 N 0.3984(10) 0.2779(8) 0.5369(4) 0.051(2) Uani 1 d D . H52 H 0.3855(143) 0.3577(64) 0.5633(50) 0.117(54) 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 V 0.0151(5) 0.0302(5) 0.0330(5) 0.0027(5) 0.0026(5) 0.0013(5) S1 0.0514(12) 0.0498(12) 0.0470(10) -0.0046(9) 0.0183(10) 0.0089(11) S2 0.0163(8) 0.0560(11) 0.0561(10) 0.0099(9) 0.0023(7) 0.0066(8) S3 0.0357(10) 0.0463(11) 0.0504(10) 0.0049(9) -0.0101(9) -0.0131(9) N4 0.021(3) 0.032(3) 0.042(3) 0.007(3) -0.001(2) -0.004(3) C14 0.055(5) 0.042(4) 0.062(5) -0.004(4) 0.008(5) 0.003(5) C41 0.037(4) 0.037(4) 0.066(5) 0.010(4) 0.000(4) 0.008(4) C24 0.021(3) 0.071(6) 0.062(5) 0.013(5) 0.009(3) -0.007(4) C42 0.034(4) 0.049(4) 0.065(5) 0.009(4) -0.005(4) -0.021(4) C34 0.044(4) 0.062(5) 0.044(4) 0.000(4) -0.021(4) -0.007(4) C43 0.041(4) 0.053(5) 0.048(4) 0.019(4) -0.005(4) -0.003(4) N5 0.025(3) 0.056(4) 0.039(3) 0.001(3) -0.002(3) 0.005(3) C51 0.049(5) 0.046(4) 0.069(5) 0.001(4) 0.005(4) 0.004(4) N52 0.037(4) 0.065(5) 0.052(4) 0.006(4) 0.001(3) -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 V N5 2.145(6) . ? V N4 2.165(6) . ? V S1 2.278(2) . ? V S2 2.279(2) . ? V S3 2.287(2) . ? S1 C14 1.821(8) . ? S2 C24 1.812(8) . ? S3 C34 1.815(8) . ? N4 C43 1.477(9) . ? N4 C41 1.489(10) . ? N4 C42 1.503(9) . ? C14 C41 1.537(11) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C41 H41A 0.97 . ? C41 H41B 0.97 . ? C24 C42 1.508(12) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C42 H42A 0.97 . ? C42 H42B 0.97 . ? C34 C43 1.492(11) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C43 H43A 0.97 . ? C43 H43B 0.97 . ? N5 N52 1.427(9) . ? N5 C51 1.487(10) . ? C51 H51A 0.96 . ? C51 H51B 0.96 . ? C51 H51C 0.96 . ? N52 H52 0.899(10) . ? 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 N5 V N4 178.6(2) . . ? N5 V S1 94.6(2) . . ? N4 V S1 86.8(2) . . ? N5 V S2 94.0(2) . . ? N4 V S2 85.7(2) . . ? S1 V S2 118.55(10) . . ? N5 V S3 92.9(2) . . ? N4 V S3 86.1(2) . . ? S1 V S3 119.71(10) . . ? S2 V S3 120.42(9) . . ? C14 S1 V 100.4(3) . . ? C24 S2 V 100.9(3) . . ? C34 S3 V 100.1(3) . . ? C43 N4 C41 109.0(6) . . ? C43 N4 C42 110.1(6) . . ? C41 N4 C42 109.1(6) . . ? C43 N4 V 109.6(5) . . ? C41 N4 V 108.7(4) . . ? C42 N4 V 110.3(5) . . ? C41 C14 S1 110.6(6) . . ? C41 C14 H14A 109.5(5) . . ? S1 C14 H14A 109.5(3) . . ? C41 C14 H14B 109.5(5) . . ? S1 C14 H14B 109.5(3) . . ? H14A C14 H14B 108.1 . . ? N4 C41 C14 112.2(7) . . ? N4 C41 H41A 109.2(4) . . ? C14 C41 H41A 109.2(6) . . ? N4 C41 H41B 109.2(4) . . ? C14 C41 H41B 109.2(4) . . ? H41A C41 H41B 107.9 . . ? C42 C24 S2 112.2(5) . . ? C42 C24 H24A 109.2(4) . . ? S2 C24 H24A 109.2(3) . . ? C42 C24 H24B 109.2(5) . . ? S2 C24 H24B 109.2(3) . . ? H24A C24 H24B 107.9 . . ? N4 C42 C24 111.4(6) . . ? N4 C42 H42A 109.4(4) . . ? C24 C42 H42A 109.4(5) . . ? N4 C42 H42B 109.4(4) . . ? C24 C42 H42B 109.4(4) . . ? H42A C42 H42B 108.0 . . ? C43 C34 S3 112.4(5) . . ? C43 C34 H34A 109.1(5) . . ? S3 C34 H34A 109.1(3) . . ? C43 C34 H34B 109.1(5) . . ? S3 C34 H34B 109.1(3) . . ? H34A C34 H34B 107.9 . . ? N4 C43 C34 113.7(6) . . ? N4 C43 H43A 108.8(4) . . ? C34 C43 H43A 108.8(5) . . ? N4 C43 H43B 108.8(4) . . ? C34 C43 H43B 108.8(4) . . ? H43A C43 H43B 107.7 . . ? N52 N5 C51 104.8(7) . . ? N52 N5 V 112.5(5) . . ? C51 N5 V 117.1(5) . . ? N5 C51 H51A 109.5(4) . . ? N5 C51 H51B 109.5(4) . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5(4) . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N5 N52 H52 110.6(22) . . ? _refine_diff_density_max 0.787 _refine_diff_density_min -1.172 _refine_diff_density_rms 0.141 #===END data_martin1 _database_code_CSD 180741 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'complex 2' _chemical_formula_moiety 'C11 H22 N3 S3 V, 0.5(C D2 Cl2)' _chemical_formula_structural '[V(NNC5H10)(NS3)].0.5CD2Cl2' _chemical_formula_analytical ? _chemical_formula_sum 'C11.50 H23 Cl N3 S3 V' _chemical_formula_weight 385.90 _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' 'S' 'S' 0.1246 0.1234 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/a' #(equiv. to no. 14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 11.4660(10) _cell_length_b 11.9468(12) _cell_length_c 12.8618(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.595(8) _cell_angle_gamma 90.00 _cell_volume 1761.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'striated plates' _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method ? _exptl_crystal_F_000 804 _exptl_absorpt_coefficient_mu 1.063 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.99 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4302 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 27.0 _reflns_number_total 3835 _reflns_number_observed 2778 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0538P)^2^+0.56P] 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 3835 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_obs 0.0388 _refine_ls_wR_factor_all 0.1165 _refine_ls_wR_factor_obs 0.1025 _refine_ls_goodness_of_fit_all 1.056 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.056 _refine_ls_restrained_S_obs 1.102 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V V 0.23319(3) 0.05236(3) 0.17669(3) 0.04478(14) Uani 1 d . . S1 S 0.30985(7) 0.08877(6) 0.02032(5) 0.0600(2) Uani 1 d . . S2 S 0.06661(7) -0.04953(6) 0.18288(7) 0.0642(2) Uani 1 d . . S3 S 0.28693(7) 0.15846(7) 0.31484(6) 0.0687(2) Uani 1 d . . C14 C 0.2225(3) 0.2060(3) -0.0266(2) 0.0696(8) Uani 1 d . . H14A H 0.2707(3) 0.2556(3) -0.0669(2) 0.083 Uiso 0.695(5) calc PR 1 H14B H 0.1599(3) 0.1785(3) -0.0721(2) 0.083 Uiso 0.695(5) calc PR 1 H14C H 0.2622(3) 0.2755(3) -0.0092(2) 0.083 Uiso 0.305(5) calc PR 2 H14D H 0.2138(3) 0.2018(3) -0.1018(2) 0.083 Uiso 0.305(5) calc PR 2 C24 C -0.0453(3) 0.0542(3) 0.1522(3) 0.0737(9) Uani 1 d . . H24A H -0.1076(3) 0.0195(3) 0.1111(3) 0.088 Uiso 0.695(5) calc PR 1 H24B H -0.0781(3) 0.0813(3) 0.2162(3) 0.088 Uiso 0.695(5) calc PR 1 H24C H -0.0669(3) 0.0497(3) 0.0789(3) 0.088 Uiso 0.305(5) calc PR 2 H24D H -0.1142(3) 0.0383(3) 0.1918(3) 0.088 Uiso 0.305(5) calc PR 2 C34 C 0.1963(3) 0.2828(3) 0.2968(3) 0.0756(9) Uani 1 d . . H34A H 0.1743(3) 0.3109(3) 0.3643(3) 0.091 Uiso 0.695(5) calc PR 1 H34B H 0.2411(3) 0.3406(3) 0.2632(3) 0.091 Uiso 0.695(5) calc PR 1 H34C H 0.1282(3) 0.2766(3) 0.3396(3) 0.091 Uiso 0.305(5) calc PR 2 H34D H 0.2400(3) 0.3482(3) 0.3197(3) 0.091 Uiso 0.305(5) calc PR 2 C41A C 0.1712(4) 0.2704(3) 0.0623(4) 0.0699(14) Uani 0.695(5) d P 1 H41A H 0.2325(4) 0.3124(3) 0.0982(4) 0.084 Uiso 0.695(5) calc PR 1 H41B H 0.1140(4) 0.3234(3) 0.0350(4) 0.084 Uiso 0.695(5) calc PR 1 C42A C 0.0036(4) 0.1518(4) 0.0927(5) 0.0722(15) Uani 0.695(5) d P 1 H42A H 0.0156(4) 0.1289(4) 0.0214(5) 0.087 Uiso 0.695(5) calc PR 1 H42B H -0.0529(4) 0.2122(4) 0.0914(5) 0.087 Uiso 0.695(5) calc PR 1 C43A C 0.0903(4) 0.2592(4) 0.2337(4) 0.077(2) Uani 0.695(5) d P 1 H43A H 0.0537(4) 0.3295(4) 0.2137(4) 0.092 Uiso 0.695(5) calc PR 1 H43B H 0.0358(4) 0.2180(4) 0.2755(4) 0.092 Uiso 0.695(5) calc PR 1 C41B C 0.1043(8) 0.2057(8) 0.0203(7) 0.056(2) Uiso 0.305(5) d P 2 H41C H 0.0584(8) 0.1444(8) -0.0086(7) 0.067 Uiso 0.305(5) calc PR 2 H41D H 0.0643(8) 0.2751(8) 0.0031(7) 0.067 Uiso 0.305(5) calc PR 2 C42B C -0.0052(8) 0.1647(7) 0.1759(8) 0.054(2) Uiso 0.305(5) d P 2 H42C H -0.0047(8) 0.1744(7) 0.2508(8) 0.065 Uiso 0.305(5) calc PR 2 H42D H -0.0608(8) 0.2178(7) 0.1462(8) 0.065 Uiso 0.305(5) calc PR 2 C43B C 0.1565(9) 0.2981(8) 0.1822(7) 0.056(2) Uiso 0.305(5) d P 2 H43C H 0.0950(9) 0.3537(8) 0.1778(7) 0.067 Uiso 0.305(5) calc PR 2 H43D H 0.2215(9) 0.3252(8) 0.1425(7) 0.067 Uiso 0.305(5) calc PR 2 N4 N 0.1142(2) 0.1933(2) 0.1377(2) 0.0509(5) Uani 1 d . . N5 N 0.3236(2) -0.0536(2) 0.2078(2) 0.0549(5) Uani 1 d . . N51 N 0.3922(2) -0.1404(2) 0.2285(2) 0.0595(6) Uani 1 d . . C52 C 0.3601(4) -0.2098(3) 0.3152(4) 0.1006(14) Uani 1 d . . H52A H 0.3889(4) -0.2852(3) 0.3050(4) 0.121 Uiso 1 calc R . H52B H 0.2758(4) -0.2131(3) 0.3186(4) 0.121 Uiso 1 calc R . C53 C 0.4091(8) -0.1646(5) 0.4128(4) 0.156(3) Uani 1 d . . H53A H 0.3914(8) -0.2149(5) 0.4695(4) 0.188 Uiso 1 calc R . H53B H 0.3734(8) -0.0927(5) 0.4269(4) 0.188 Uiso 1 calc R . C54 C 0.5406(8) -0.1503(6) 0.4071(5) 0.175(4) Uani 1 d . . H54A H 0.5709(8) -0.1172(6) 0.4712(5) 0.210 Uiso 1 calc R . H54B H 0.5772(8) -0.2228(6) 0.3987(5) 0.210 Uiso 1 calc R . C55 C 0.5682(5) -0.0770(4) 0.3178(5) 0.142(3) Uani 1 d . . H55A H 0.5381(5) -0.0023(4) 0.3297(5) 0.170 Uiso 1 calc R . H55B H 0.6521(5) -0.0717(4) 0.3116(5) 0.170 Uiso 1 calc R . C56 C 0.5159(3) -0.1226(3) 0.2204(3) 0.0803(10) Uani 1 d . . H56A H 0.5297(3) -0.0710(3) 0.1639(3) 0.096 Uiso 1 calc R . H56B H 0.5534(3) -0.1930(3) 0.2043(3) 0.096 Uiso 1 calc R . Cl61 Cl 0.3821(7) 0.4488(8) 0.4724(6) 0.102(2) Uiso 0.22 d P . Cl62 Cl 0.3745(5) 0.5070(5) 0.4494(5) 0.1029(14) Uiso 0.30 d P . Cl63 Cl 0.4202(6) 0.4052(6) 0.4606(5) 0.104(2) Uiso 0.22 d P . Cl64 Cl 0.4015(8) 0.4680(10) 0.4333(7) 0.095(2) Uiso 0.16 d P . Cl65 Cl 0.3918(15) 0.5164(15) 0.5024(14) 0.113(4) Uiso 0.10 d P . C61 C 0.4685(14) 0.5241(13) 0.5418(12) 0.106(4) Uiso 0.38 d P . C62 C 0.4771(43) 0.5544(37) 0.4861(41) 0.115(13) Uiso 0.13 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 V 0.0423(2) 0.0443(2) 0.0474(2) 0.0014(2) -0.0035(2) 0.0011(2) S1 0.0640(4) 0.0621(4) 0.0544(4) 0.0004(3) 0.0096(3) 0.0030(3) S2 0.0578(4) 0.0505(4) 0.0841(5) 0.0051(3) -0.0027(4) -0.0113(3) S3 0.0709(5) 0.0801(5) 0.0544(4) -0.0091(3) -0.0097(3) -0.0088(4) C14 0.085(2) 0.064(2) 0.059(2) 0.0156(14) -0.0052(15) -0.003(2) C24 0.0438(15) 0.070(2) 0.108(3) -0.010(2) -0.001(2) -0.0065(14) C34 0.077(2) 0.071(2) 0.079(2) -0.030(2) 0.012(2) -0.010(2) C41A 0.065(3) 0.048(2) 0.096(3) 0.014(2) -0.016(2) -0.002(2) C42A 0.045(2) 0.055(2) 0.115(4) -0.002(2) -0.023(2) 0.007(2) C43A 0.059(3) 0.067(3) 0.105(4) -0.032(3) 0.006(3) 0.005(2) N4 0.0410(11) 0.0437(11) 0.0677(13) -0.0057(10) -0.0031(9) 0.0028(9) N5 0.0547(13) 0.0525(12) 0.0571(13) 0.0041(10) -0.0080(10) 0.0064(10) N51 0.0585(13) 0.0521(12) 0.0675(14) 0.0089(11) -0.0046(11) 0.0103(11) C52 0.086(3) 0.083(2) 0.134(4) 0.053(3) 0.032(2) 0.018(2) C53 0.283(9) 0.124(4) 0.064(3) 0.025(3) 0.048(4) 0.081(5) C54 0.253(9) 0.139(5) 0.126(5) -0.017(4) -0.124(6) 0.046(6) C55 0.110(4) 0.082(3) 0.228(7) 0.008(4) -0.092(4) -0.011(3) C56 0.068(2) 0.073(2) 0.102(3) 0.024(2) 0.022(2) 0.024(2) _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 V N5 1.677(2) . ? V N4 2.216(2) . ? V S3 2.2545(9) . ? V S1 2.2595(8) . ? V S2 2.2682(8) . ? S1 C14 1.815(3) . ? S2 C24 1.820(3) . ? S3 C34 1.824(4) . ? C14 C41B 1.500(9) . ? C14 C41A 1.511(6) . ? C14 H14A 0.97 . ? C14 H14B 0.97 . ? C14 H14C 0.97 . ? C14 H14D 0.97 . ? C24 C42B 1.427(9) . ? C24 C42A 1.511(6) . ? C24 H24A 0.97 . ? C24 H24B 0.97 . ? C24 H24C 0.97 . ? C24 H24D 0.97 . ? C34 C43A 1.470(6) . ? C34 C43B 1.542(9) . ? C34 H34A 0.97 . ? C34 H34B 0.97 . ? C34 H34C 0.97 . ? C34 H34D 0.97 . ? C41A N4 1.501(5) . ? C41A H41A 0.97 . ? C41A H41B 0.97 . ? C42A N4 1.466(4) . ? C42A H42A 0.97 . ? C42A H42B 0.97 . ? C43A N4 1.496(5) . ? C43A H43A 0.97 . ? C43A H43B 0.97 . ? C41B N4 1.518(9) . ? C41B H41C 0.97 . ? C41B H41D 0.97 . ? C42B N4 1.507(9) . ? C42B H42C 0.97 . ? C42B H42D 0.97 . ? C43B N4 1.455(9) . ? C43B H43C 0.97 . ? C43B H43D 0.97 . ? N5 N51 1.324(3) . ? N51 C56 1.441(4) . ? N51 C52 1.445(4) . ? C52 C53 1.464(8) . ? C52 H52A 0.97 . ? C52 H52B 0.97 . ? C53 C54 1.521(9) . ? C53 H53A 0.97 . ? C53 H53B 0.97 . ? C54 C55 1.486(9) . ? C54 H54A 0.97 . ? C54 H54B 0.97 . ? C55 C56 1.477(6) . ? C55 H55A 0.97 . ? C55 H55B 0.97 . ? C56 H56A 0.97 . ? C56 H56B 0.97 . ? Cl61 Cl64 0.601(10) . ? Cl61 Cl63 0.700(9) . ? Cl61 Cl62 0.759(9) . ? Cl61 Cl65 0.90(2) . ? Cl61 C61 1.59(2) . ? Cl61 C62 1.67(5) . ? Cl61 C62 1.69(5) 3_666 ? Cl61 C61 1.76(2) 3_666 ? Cl62 Cl64 0.599(11) . ? Cl62 Cl65 0.71(2) . ? Cl62 Cl63 1.330(9) . ? Cl62 C62 1.38(5) . ? Cl62 C61 1.59(2) . ? Cl62 C61 1.84(2) 3_666 ? Cl62 C62 2.01(5) 3_666 ? Cl63 Cl64 0.853(12) . ? Cl63 C62 1.43(5) 3_666 ? Cl63 Cl65 1.47(2) . ? Cl63 C61 1.53(2) 3_666 ? Cl63 C61 1.84(2) . ? Cl63 C62 1.92(5) . ? Cl63 Cl65 2.39(2) 3_666 ? Cl64 Cl65 1.07(2) . ? Cl64 C62 1.50(5) . ? Cl64 C61 1.52(2) 3_666 ? Cl64 C61 1.71(2) . ? Cl64 C62 1.73(5) 3_666 ? Cl65 C61 1.01(2) . ? Cl65 C62 1.10(5) . ? Cl65 C62 1.73(5) 3_666 ? Cl65 C61 1.78(2) 3_666 ? Cl65 Cl63 2.39(2) 3_666 ? C61 C62 0.81(5) . ? C61 C62 1.19(4) 3_666 ? C61 C61 1.43(3) 3_666 ? C61 Cl64 1.52(2) 3_666 ? C61 Cl63 1.53(2) 3_666 ? C61 Cl61 1.76(2) 3_666 ? C61 Cl65 1.78(2) 3_666 ? C61 Cl62 1.84(2) 3_666 ? C62 C61 1.19(4) 3_666 ? C62 Cl63 1.43(5) 3_666 ? C62 C62 1.44(9) 3_666 ? C62 Cl61 1.69(5) 3_666 ? C62 Cl65 1.73(5) 3_666 ? C62 Cl64 1.73(5) 3_666 ? 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 N5 V N4 179.23(10) . . ? N5 V S3 94.76(8) . . ? N4 V S3 84.49(6) . . ? N5 V S1 96.00(8) . . ? N4 V S1 84.54(6) . . ? S3 V S1 119.26(3) . . ? N5 V S2 95.85(8) . . ? N4 V S2 84.37(6) . . ? S3 V S2 119.08(4) . . ? S1 V S2 118.91(3) . . ? C14 S1 V 102.71(11) . . ? C24 S2 V 102.49(10) . . ? C34 S3 V 102.45(10) . . ? C41B C14 S1 111.2(4) . . ? C41A C14 S1 111.3(2) . . ? C41A C14 H14A 109.4(2) . . ? S1 C14 H14A 109.36(11) . . ? C41A C14 H14B 109.4(2) . . ? S1 C14 H14B 109.36(11) . . ? H14A C14 H14B 108.0 . . ? C41B C14 H14C 109.4(4) . . ? S1 C14 H14C 109.40(11) . . ? C41B C14 H14D 109.4(4) . . ? S1 C14 H14D 109.40(10) . . ? H14C C14 H14D 108.0 . . ? C42B C24 S2 111.3(4) . . ? C42A C24 S2 111.5(2) . . ? C42A C24 H24A 109.3(2) . . ? S2 C24 H24A 109.33(10) . . ? C42A C24 H24B 109.3(3) . . ? S2 C24 H24B 109.33(13) . . ? H24A C24 H24B 108.0 . . ? C42B C24 H24C 109.4(4) . . ? S2 C24 H24C 109.38(13) . . ? C42B C24 H24D 109.4(4) . . ? S2 C24 H24D 109.38(11) . . ? H24C C24 H24D 108.0 . . ? C43A C34 S3 111.9(3) . . ? C43B C34 S3 111.7(4) . . ? C43A C34 H34A 109.2(2) . . ? S3 C34 H34A 109.23(11) . . ? C43A C34 H34B 109.2(3) . . ? S3 C34 H34B 109.23(11) . . ? H34A C34 H34B 107.9 . . ? C43B C34 H34C 109.3(4) . . ? S3 C34 H34C 109.27(11) . . ? C43B C34 H34D 109.3(4) . . ? S3 C34 H34D 109.27(10) . . ? H34C C34 H34D 107.9 . . ? N4 C41A C14 111.2(3) . . ? N4 C41A H41A 109.4(2) . . ? C14 C41A H41A 109.4(2) . . ? N4 C41A H41B 109.4(2) . . ? C14 C41A H41B 109.4(2) . . ? H41A C41A H41B 108.0 . . ? N4 C42A C24 112.9(4) . . ? N4 C42A H42A 109.0(3) . . ? C24 C42A H42A 109.0(3) . . ? N4 C42A H42B 109.0(2) . . ? C24 C42A H42B 109.0(2) . . ? H42A C42A H42B 107.8 . . ? C34 C43A N4 112.9(3) . . ? C34 C43A H43A 109.0(2) . . ? N4 C43A H43A 109.0(2) . . ? C34 C43A H43B 109.0(3) . . ? N4 C43A H43B 109.0(2) . . ? H43A C43A H43B 107.8 . . ? C14 C41B N4 110.9(6) . . ? C14 C41B H41C 109.5(4) . . ? N4 C41B H41C 109.5(4) . . ? C14 C41B H41D 109.5(4) . . ? N4 C41B H41D 109.5(4) . . ? H41C C41B H41D 108.0 . . ? C24 C42B N4 115.5(6) . . ? C24 C42B H42C 108.4(4) . . ? N4 C42B H42C 108.4(4) . . ? C24 C42B H42D 108.4(4) . . ? N4 C42B H42D 108.4(4) . . ? H42C C42B H42D 107.5 . . ? N4 C43B C34 111.1(6) . . ? N4 C43B H43C 109.4(4) . . ? C34 C43B H43C 109.4(4) . . ? N4 C43B H43D 109.4(4) . . ? C34 C43B H43D 109.4(4) . . ? H43C C43B H43D 108.0 . . ? C42A N4 C43A 109.1(3) . . ? C42A N4 C41A 109.8(3) . . ? C43A N4 C41A 107.7(3) . . ? C43B N4 C42B 111.3(5) . . ? C43B N4 C41B 108.8(5) . . ? C42B N4 C41B 107.6(5) . . ? C43B N4 V 111.6(4) . . ? C42A N4 V 110.7(2) . . ? C43A N4 V 109.9(2) . . ? C41A N4 V 109.6(2) . . ? C42B N4 V 108.3(4) . . ? C41B N4 V 109.1(4) . . ? N51 N5 V 177.0(2) . . ? N5 N51 C56 116.8(2) . . ? N5 N51 C52 116.2(3) . . ? C56 N51 C52 114.3(3) . . ? N51 C52 C53 110.6(4) . . ? N51 C52 H52A 109.5(2) . . ? C53 C52 H52A 109.5(3) . . ? N51 C52 H52B 109.5(2) . . ? C53 C52 H52B 109.5(3) . . ? H52A C52 H52B 108.1 . . ? C52 C53 C54 110.9(4) . . ? C52 C53 H53A 109.5(3) . . ? C54 C53 H53A 109.5(3) . . ? C52 C53 H53B 109.5(3) . . ? C54 C53 H53B 109.5(4) . . ? H53A C53 H53B 108.0 . . ? C55 C54 C53 109.6(4) . . ? C55 C54 H54A 109.7(3) . . ? C53 C54 H54A 109.7(4) . . ? C55 C54 H54B 109.7(4) . . ? C53 C54 H54B 109.7(4) . . ? H54A C54 H54B 108.2 . . ? C56 C55 C54 110.3(4) . . ? C56 C55 H55A 109.6(2) . . ? C54 C55 H55A 109.6(4) . . ? C56 C55 H55B 109.6(3) . . ? C54 C55 H55B 109.6(4) . . ? H55A C55 H55B 108.1 . . ? N51 C56 C55 111.8(4) . . ? N51 C56 H56A 109.3(2) . . ? C55 C56 H56A 109.3(3) . . ? N51 C56 H56B 109.3(2) . . ? C55 C56 H56B 109.3(2) . . ? H56A C56 H56B 107.9 . . ? Cl64 Cl61 Cl63 81.6(17) . . ? Cl64 Cl61 Cl62 50.6(13) . . ? Cl63 Cl61 Cl62 131.4(14) . . ? Cl64 Cl61 Cl65 88.4(19) . . ? Cl63 Cl61 Cl65 133.7(17) . . ? Cl62 Cl61 Cl65 50.1(11) . . ? Cl64 Cl61 C61 90.9(14) . . ? Cl63 Cl61 C61 99.2(11) . . ? Cl62 Cl61 C61 76.4(10) . . ? Cl65 Cl61 C61 35.5(13) . . ? Cl64 Cl61 C62 63.0(22) . . ? Cl63 Cl61 C62 100.1(20) . . ? Cl62 Cl61 C62 54.4(17) . . ? Cl65 Cl61 C62 37.4(20) . . ? C61 Cl61 C62 28.6(15) . . ? Cl64 Cl61 C62 84.3(22) . 3_666 ? Cl63 Cl61 C62 56.9(18) . 3_666 ? Cl62 Cl61 C62 104.1(17) . 3_666 ? Cl65 Cl61 C62 77.3(20) . 3_666 ? C61 Cl61 C62 42.3(14) . 3_666 ? C62 Cl61 C62 50.9(28) . 3_666 ? Cl64 Cl61 C61 57.3(13) . 3_666 ? Cl63 Cl61 C61 59.9(9) . 3_666 ? Cl62 Cl61 C61 83.8(9) . 3_666 ? Cl65 Cl61 C61 76.7(12) . 3_666 ? C61 Cl61 C61 50.3(9) . 3_666 ? C62 Cl61 C61 40.4(16) . 3_666 ? C62 Cl61 C61 27.1(16) 3_666 3_666 ? Cl64 Cl62 Cl65 108.7(19) . . ? Cl64 Cl62 Cl61 50.9(11) . . ? Cl65 Cl62 Cl61 75.3(14) . . ? Cl64 Cl62 Cl63 28.5(12) . . ? Cl65 Cl62 Cl63 86.7(16) . . ? Cl61 Cl62 Cl63 23.2(7) . . ? Cl64 Cl62 C62 89.7(23) . . ? Cl65 Cl62 C62 52.8(25) . . ? Cl61 Cl62 C62 98.9(20) . . ? Cl63 Cl62 C62 90.5(19) . . ? Cl64 Cl62 C61 90.7(13) . . ? Cl65 Cl62 C61 26.3(15) . . ? Cl61 Cl62 C61 76.0(10) . . ? Cl63 Cl62 C61 77.3(7) . . ? C62 Cl62 C61 30.6(19) . . ? Cl64 Cl62 C61 49.5(11) . 3_666 ? Cl65 Cl62 C61 74.1(15) . 3_666 ? Cl61 Cl62 C61 71.9(9) . 3_666 ? Cl63 Cl62 C61 55.0(6) . 3_666 ? C62 Cl62 C61 40.2(19) . 3_666 ? C61 Cl62 C61 48.7(9) . 3_666 ? Cl64 Cl62 C62 54.6(18) . 3_666 ? Cl65 Cl62 C62 56.9(22) . 3_666 ? Cl61 Cl62 C62 54.4(14) . 3_666 ? Cl63 Cl62 C62 45.2(13) . 3_666 ? C62 Cl62 C62 45.9(29) . 3_666 ? C61 Cl62 C62 36.2(12) . 3_666 ? C61 Cl62 C62 23.8(14) 3_666 3_666 ? Cl61 Cl63 Cl64 44.2(9) . . ? Cl61 Cl63 Cl62 25.3(8) . . ? Cl64 Cl63 Cl62 19.6(8) . . ? Cl61 Cl63 C62 98.9(22) . 3_666 ? Cl64 Cl63 C62 95.5(20) . 3_666 ? Cl62 Cl63 C62 93.5(19) . 3_666 ? Cl61 Cl63 Cl65 26.2(10) . . ? Cl64 Cl63 Cl65 45.7(10) . . ? Cl62 Cl63 Cl65 28.9(7) . . ? C62 Cl63 Cl65 73.0(20) 3_666 . ? Cl61 Cl63 C61 96.8(11) . 3_666 ? Cl64 Cl63 C61 73.0(10) . 3_666 ? Cl62 Cl63 C61 79.6(7) . 3_666 ? C62 Cl63 C61 31.5(19) 3_666 3_666 ? Cl65 Cl63 C61 72.7(9) . 3_666 ? Cl61 Cl63 C61 58.7(9) . . ? Cl64 Cl63 C61 67.8(9) . . ? Cl62 Cl63 C61 57.8(6) . . ? C62 Cl63 C61 40.2(18) 3_666 . ? Cl65 Cl63 C61 33.1(7) . . ? C61 Cl63 C61 49.3(9) 3_666 . ? Cl61 Cl63 C62 58.9(17) . . ? Cl64 Cl63 C62 48.4(15) . . ? Cl62 Cl63 C62 45.7(14) . . ? C62 Cl63 C62 48.3(29) 3_666 . ? Cl65 Cl63 C62 34.8(16) . . ? C61 Cl63 C62 38.1(14) 3_666 . ? C61 Cl63 C62 24.8(14) . . ? Cl61 Cl63 Cl65 103.3(9) . 3_666 ? Cl64 Cl63 Cl65 87.3(9) . 3_666 ? Cl62 Cl63 Cl65 90.8(5) . 3_666 ? C62 Cl63 Cl65 17.2(22) 3_666 3_666 ? Cl65 Cl63 Cl65 77.3(9) . 3_666 ? C61 Cl63 Cl65 16.0(7) 3_666 3_666 ? C61 Cl63 Cl65 47.7(6) . 3_666 ? C62 Cl63 Cl65 45.7(15) . 3_666 ? Cl62 Cl64 Cl61 78.5(16) . . ? Cl62 Cl64 Cl63 131.9(18) . . ? Cl61 Cl64 Cl63 54.2(15) . . ? Cl62 Cl64 Cl65 39.2(12) . . ? Cl61 Cl64 Cl65 57.4(14) . . ? Cl63 Cl64 Cl65 99.5(15) . . ? Cl62 Cl64 C62 66.8(22) . . ? Cl61 Cl64 C62 96.0(24) . . ? Cl63 Cl64 C62 106.5(20) . . ? Cl65 Cl64 C62 47.3(22) . . ? Cl62 Cl64 C61 113.0(14) . 3_666 ? Cl61 Cl64 C61 103.3(16) . 3_666 ? Cl63 Cl64 C61 74.5(11) . 3_666 ? Cl65 Cl64 C61 85.1(12) . 3_666 ? C62 Cl64 C61 46.3(17) . 3_666 ? Cl62 Cl64 C61 68.8(12) . . ? Cl61 Cl64 C61 68.5(13) . . ? Cl63 Cl64 C61 84.7(10) . . ? Cl65 Cl64 C61 33.3(10) . . ? C62 Cl64 C61 28.3(18) . . ? C61 Cl64 C61 52.2(10) 3_666 . ? Cl62 Cl64 C62 109.1(21) . 3_666 ? Cl61 Cl64 C62 75.5(22) . 3_666 ? Cl63 Cl64 C62 55.2(16) . 3_666 ? Cl65 Cl64 C62 71.7(21) . 3_666 ? C62 Cl64 C62 52.4(29) . 3_666 ? C61 Cl64 C62 27.9(16) 3_666 3_666 ? C61 Cl64 C62 40.3(15) . 3_666 ? Cl62 Cl65 Cl61 54.7(14) . . ? Cl62 Cl65 C61 135.3(24) . . ? Cl61 Cl65 C61 113.1(21) . . ? Cl62 Cl65 Cl64 32.1(11) . . ? Cl61 Cl65 Cl64 34.2(9) . . ? C61 Cl65 Cl64 111.0(19) . . ? Cl62 Cl65 C62 96.2(32) . . ? Cl61 Cl65 C62 112.8(30) . . ? C61 Cl65 C62 44.9(24) . . ? Cl64 Cl65 C62 87.3(29) . . ? Cl62 Cl65 Cl63 64.3(15) . . ? Cl61 Cl65 Cl63 20.1(8) . . ? C61 Cl65 Cl63 93.8(16) . . ? Cl64 Cl65 Cl63 34.8(9) . . ? C62 Cl65 Cl63 95.5(28) . . ? Cl62 Cl65 C62 102.9(24) . 3_666 ? Cl61 Cl65 C62 72.2(19) . 3_666 ? C61 Cl65 C62 41.9(17) . 3_666 ? Cl64 Cl65 C62 72.3(21) . 3_666 ? C62 Cl65 C62 56.2(36) . 3_666 ? Cl63 Cl65 C62 52.3(16) . 3_666 ? Cl62 Cl65 C61 83.2(15) . 3_666 ? Cl61 Cl65 C61 73.8(12) . 3_666 ? C61 Cl65 C61 53.5(15) . 3_666 ? Cl64 Cl65 C61 58.2(9) . 3_666 ? C62 Cl65 C61 40.7(24) . 3_666 ? Cl63 Cl65 C61 55.2(7) . 3_666 ? C62 Cl65 C61 26.7(16) 3_666 3_666 ? Cl62 Cl65 Cl63 118.6(17) . 3_666 ? Cl61 Cl65 Cl63 122.5(14) . 3_666 ? C61 Cl65 Cl63 24.8(12) . 3_666 ? Cl64 Cl65 Cl63 105.4(11) . 3_666 ? C62 Cl65 Cl63 22.5(28) . 3_666 ? Cl63 Cl65 Cl63 102.7(9) . 3_666 ? C62 Cl65 Cl63 52.8(16) 3_666 3_666 ? C61 Cl65 Cl63 49.8(7) 3_666 3_666 ? C62 C61 Cl65 73.8(36) . . ? C62 C61 C62 90.5(46) . 3_666 ? Cl65 C61 C62 103.6(26) . 3_666 ? C62 C61 C61 56.0(37) . 3_666 ? Cl65 C61 C61 92.2(17) . 3_666 ? C62 C61 C61 34.5(24) 3_666 3_666 ? C62 C61 Cl64 90.9(39) . 3_666 ? Cl65 C61 Cl64 161.8(18) . 3_666 ? C62 C61 Cl64 65.9(23) 3_666 3_666 ? C61 C61 Cl64 70.7(12) 3_666 3_666 ? C62 C61 Cl63 67.3(36) . 3_666 ? Cl65 C61 Cl63 139.2(18) . 3_666 ? C62 C61 Cl63 89.1(24) 3_666 3_666 ? C61 C61 Cl63 76.6(13) 3_666 3_666 ? Cl64 C61 Cl63 32.5(6) 3_666 3_666 ? C62 C61 Cl61 81.2(36) . . ? Cl65 C61 Cl61 31.3(11) . . ? C62 C61 Cl61 73.1(23) 3_666 . ? C61 C61 Cl61 70.9(12) 3_666 . ? Cl64 C61 Cl61 138.1(12) 3_666 . ? Cl63 C61 Cl61 143.7(11) 3_666 . ? C62 C61 Cl62 59.7(36) . . ? Cl65 C61 Cl62 18.3(10) . . ? C62 C61 Cl62 91.4(25) 3_666 . ? C61 C61 Cl62 74.6(12) 3_666 . ? Cl64 C61 Cl62 143.5(11) 3_666 . ? Cl63 C61 Cl62 127.0(11) 3_666 . ? Cl61 C61 Cl62 27.6(4) . . ? C62 C61 Cl64 61.2(36) . . ? Cl65 C61 Cl64 35.7(12) . . ? C62 C61 Cl64 70.9(24) 3_666 . ? C61 C61 Cl64 57.0(11) 3_666 . ? Cl64 C61 Cl64 127.8(10) 3_666 . ? Cl63 C61 Cl64 123.8(10) 3_666 . ? Cl61 C61 Cl64 20.6(4) . . ? Cl62 C61 Cl64 20.5(4) . . ? C62 C61 Cl61 71.5(38) . 3_666 ? Cl65 C61 Cl61 143.5(17) . 3_666 ? C62 C61 Cl61 65.9(23) 3_666 3_666 ? C61 C61 Cl61 58.8(11) 3_666 3_666 ? Cl64 C61 Cl61 19.4(5) 3_666 3_666 ? Cl63 C61 Cl61 23.3(4) 3_666 3_666 ? Cl61 C61 Cl61 129.7(9) . 3_666 ? Cl62 C61 Cl61 125.9(10) . 3_666 ? Cl64 C61 Cl61 113.8(9) . 3_666 ? C62 C61 Cl65 73.0(39) . 3_666 ? Cl65 C61 Cl65 126.5(15) . 3_666 ? C62 C61 Cl65 37.3(23) 3_666 3_666 ? C61 C61 Cl65 34.4(8) 3_666 3_666 ? Cl64 C61 Cl65 36.7(9) 3_666 3_666 ? Cl63 C61 Cl65 52.1(8) 3_666 3_666 ? Cl61 C61 Cl65 102.6(10) . 3_666 ? Cl62 C61 Cl65 108.8(10) . 3_666 ? Cl64 C61 Cl65 91.2(9) . 3_666 ? Cl61 C61 Cl65 29.5(7) 3_666 3_666 ? C62 C61 Cl62 90.1(40) . 3_666 ? Cl65 C61 Cl62 148.5(16) . 3_666 ? C62 C61 Cl62 48.5(23) 3_666 3_666 ? C61 C61 Cl62 56.7(11) 3_666 3_666 ? Cl64 C61 Cl62 17.4(5) 3_666 3_666 ? Cl63 C61 Cl62 45.4(5) 3_666 3_666 ? Cl61 C61 Cl62 120.9(10) . 3_666 ? Cl62 C61 Cl62 131.3(9) . 3_666 ? Cl64 C61 Cl62 112.8(9) . 3_666 ? Cl61 C61 Cl62 24.2(3) 3_666 3_666 ? Cl65 C61 Cl62 22.7(6) 3_666 3_666 ? C61 C62 Cl65 61.2(35) . . ? C61 C62 C61 89.5(46) . 3_666 ? Cl65 C62 C61 102.0(37) . 3_666 ? C61 C62 Cl62 89.7(42) . . ? Cl65 C62 Cl62 31.0(16) . . ? C61 C62 Cl62 91.3(30) 3_666 . ? C61 C62 Cl63 81.1(40) . 3_666 ? Cl65 C62 Cl63 140.3(48) . 3_666 ? C61 C62 Cl63 88.7(30) 3_666 3_666 ? Cl62 C62 Cl63 170.8(42) . 3_666 ? C61 C62 C62 55.3(36) . 3_666 ? Cl65 C62 C62 84.3(43) . 3_666 ? C61 C62 C62 34.2(24) 3_666 3_666 ? Cl62 C62 C62 90.9(41) . 3_666 ? Cl63 C62 C62 84.0(40) 3_666 3_666 ? C61 C62 Cl64 90.5(40) . . ? Cl65 C62 Cl64 45.4(20) . . ? C61 C62 Cl64 67.8(23) 3_666 . ? Cl62 C62 Cl64 23.6(9) . . ? Cl63 C62 Cl64 155.2(36) 3_666 . ? C62 C62 Cl64 72.2(35) 3_666 . ? C61 C62 Cl61 70.2(34) . . ? Cl65 C62 Cl61 29.7(16) . . ? C61 C62 Cl61 73.7(23) 3_666 . ? Cl62 C62 Cl61 26.7(9) . . ? Cl63 C62 Cl61 146.1(33) 3_666 . ? C62 C62 Cl61 65.1(33) 3_666 . ? Cl64 C62 Cl61 20.9(7) . . ? C61 C62 Cl61 81.3(39) . 3_666 ? Cl65 C62 Cl61 140.9(42) . 3_666 ? C61 C62 Cl61 64.6(22) 3_666 3_666 ? Cl62 C62 Cl61 154.1(34) . 3_666 ? Cl63 C62 Cl61 24.2(9) 3_666 3_666 ? C62 C62 Cl61 64.0(34) 3_666 3_666 ? Cl64 C62 Cl61 131.6(32) . 3_666 ? Cl61 C62 Cl61 129.1(28) . 3_666 ? C61 C62 Cl65 80.3(39) . 3_666 ? Cl65 C62 Cl65 123.8(36) . 3_666 ? C61 C62 Cl65 34.5(15) 3_666 3_666 ? Cl62 C62 Cl65 124.1(31) . 3_666 ? Cl63 C62 Cl65 54.6(18) 3_666 3_666 ? C62 C62 Cl65 39.4(28) 3_666 3_666 ? Cl64 C62 Cl65 101.1(27) . 3_666 ? Cl61 C62 Cl65 101.7(24) . 3_666 ? Cl61 C62 Cl65 30.5(10) 3_666 3_666 ? C61 C62 Cl64 61.2(34) . 3_666 ? Cl65 C62 Cl64 121.6(40) . 3_666 ? C61 C62 Cl64 68.8(24) 3_666 3_666 ? Cl62 C62 Cl64 143.7(33) . 3_666 ? Cl63 C62 Cl64 29.3(10) 3_666 3_666 ? C62 C62 Cl64 55.4(32) 3_666 3_666 ? Cl64 C62 Cl64 127.6(29) . 3_666 ? Cl61 C62 Cl64 117.1(27) . 3_666 ? Cl61 C62 Cl64 20.2(7) 3_666 3_666 ? Cl65 C62 Cl64 36.0(11) 3_666 3_666 ? C61 C62 Cl63 71.8(35) . . ? Cl65 C62 Cl63 49.7(20) . . ? C61 C62 Cl63 52.8(18) 3_666 . ? Cl62 C62 Cl63 43.8(14) . . ? Cl63 C62 Cl63 131.7(29) 3_666 . ? C62 C62 Cl63 47.7(29) 3_666 . ? Cl64 C62 Cl63 25.2(9) . . ? Cl61 C62 Cl63 21.0(6) . . ? Cl61 C62 Cl63 110.5(24) 3_666 . ? Cl65 C62 Cl63 81.4(20) 3_666 . ? Cl64 C62 Cl63 102.8(23) 3_666 . ? _refine_diff_density_max 0.302 _refine_diff_density_min -0.344 _refine_diff_density_rms 0.059 #===END data_roger56 _database_code_CSD 180742 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'complex 3' _chemical_formula_moiety 'C19 H22 N3 S3 V' _chemical_formula_structural [V(N{CH2CH2S}3)(NNCPh2)] _chemical_formula_analytical ? _chemical_formula_sum 'C19 H22 N3 S3 V' _chemical_formula_weight 439.52 _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' 'S' 'S' 0.1246 0.1234 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21 / n' #(equiv. to no. 14) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 7.5275(7) _cell_length_b 15.3503(15) _cell_length_c 17.491(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.709(8) _cell_angle_gamma 90.00 _cell_volume 1997.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10 _cell_measurement_theta_max 11 _exptl_crystal_description 'hollow square tubes' _exptl_crystal_colour 'Blood red' _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method ? _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.818 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.996 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 6583 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.5 _diffrn_reflns_theta_max 30.0 _reflns_number_total 5814 _reflns_number_observed 3978 _reflns_observed_criterion I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+0.4907P] 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 ; Coordinates were included in idealised positions and subsequently refined freely. Isotropic displacement parameters were refined freely. ; _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5814 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_obs 0.0369 _refine_ls_wR_factor_all 0.0919 _refine_ls_wR_factor_obs 0.0785 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.090 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.090 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V V 0.18242(4) 0.40817(2) 0.15845(2) 0.03121(9) Uani 1 d . . S1 S 0.35044(7) 0.52526(4) 0.13590(3) 0.04514(14) Uani 1 d . . S2 S 0.18615(8) 0.36587(4) 0.28292(3) 0.04828(15) Uani 1 d . . S3 S -0.04577(8) 0.36523(4) 0.06746(3) 0.04542(14) Uani 1 d . . N4 N -0.0125(2) 0.50745(10) 0.18679(9) 0.0320(3) Uani 1 d . . C14 C 0.2040(3) 0.61558(14) 0.15162(14) 0.0426(5) Uani 1 d . . H14A H 0.2762(33) 0.6651(16) 0.1698(14) 0.056(7) Uiso 1 d . . H14B H 0.1359(33) 0.6331(16) 0.1020(15) 0.055(7) Uiso 1 d . . C41 C 0.0828(3) 0.59049(13) 0.20917(13) 0.0390(4) Uani 1 d . . H41A H 0.1508(27) 0.5821(13) 0.2605(12) 0.034(5) Uiso 1 d . . H41B H -0.0031(30) 0.6353(15) 0.2098(13) 0.047(6) Uiso 1 d . . C24 C 0.0338(4) 0.4432(2) 0.31808(13) 0.0498(6) Uani 1 d . . H24A H -0.0220(37) 0.4144(17) 0.3549(16) 0.066(8) Uiso 1 d . . H24B H 0.1066(36) 0.4906(18) 0.3463(15) 0.068(8) Uiso 1 d . . C42 C -0.1010(3) 0.4767(2) 0.25262(14) 0.0446(5) Uani 1 d . . H42A H -0.1846(32) 0.4286(16) 0.2314(14) 0.054(7) Uiso 1 d . . H42B H -0.1674(31) 0.5253(16) 0.2669(14) 0.053(7) Uiso 1 d . . C34 C -0.2268(3) 0.4390(2) 0.0824(2) 0.0485(5) Uani 1 d . . H34A H -0.2965(37) 0.4484(18) 0.0342(17) 0.068(8) Uiso 1 d . . H34B H -0.3084(35) 0.4097(16) 0.1146(15) 0.058(7) Uiso 1 d . . C43 C -0.1525(3) 0.52320(15) 0.11780(14) 0.0424(5) Uani 1 d . . H43A H -0.0946(31) 0.5579(15) 0.0811(13) 0.047(6) Uiso 1 d . . H43B H -0.2483(34) 0.5611(16) 0.1328(14) 0.056(7) Uiso 1 d . . N5 N 0.3343(2) 0.33129(11) 0.14346(9) 0.0365(4) Uani 1 d . . N6 N 0.4657(2) 0.27458(11) 0.14845(9) 0.0365(4) Uani 1 d . . C6 C 0.4930(2) 0.22803(11) 0.08885(10) 0.0303(4) Uani 1 d . . C611 C 0.6487(2) 0.16884(12) 0.09993(10) 0.0311(4) Uani 1 d . . C612 C 0.7918(3) 0.18251(15) 0.15885(12) 0.0407(5) Uani 1 d . . H612 H 0.7906(29) 0.2323(15) 0.1884(13) 0.044(6) Uiso 1 d . . C613 C 0.9334(3) 0.1249(2) 0.17019(15) 0.0526(6) Uani 1 d . . H613 H 1.0265(38) 0.1357(18) 0.2109(16) 0.073(9) Uiso 1 d . . C614 C 0.9362(3) 0.0528(2) 0.1237(2) 0.0559(6) Uani 1 d . . H614 H 1.0273(36) 0.0104(17) 0.1327(15) 0.065(8) Uiso 1 d . . C615 C 0.7979(4) 0.0389(2) 0.0643(2) 0.0547(6) Uani 1 d . . H615 H 0.7948(33) -0.0097(18) 0.0297(15) 0.063(8) Uiso 1 d . . C616 C 0.6542(3) 0.09675(14) 0.05185(13) 0.0420(5) Uani 1 d . . H616 H 0.5643(28) 0.0884(13) 0.0116(12) 0.033(5) Uiso 1 d . . C621 C 0.3739(3) 0.22987(12) 0.01321(10) 0.0326(4) Uani 1 d . . C622 C 0.1956(3) 0.20438(14) 0.00677(13) 0.0433(5) Uani 1 d . . H622 H 0.1478(30) 0.1899(15) 0.0515(13) 0.048(7) Uiso 1 d . . C623 C 0.0916(4) 0.1985(2) -0.0655(2) 0.0546(6) Uani 1 d . . H623 H -0.0174(35) 0.1803(17) -0.0666(14) 0.057(8) Uiso 1 d . . C624 C 0.1620(4) 0.2188(2) -0.13082(14) 0.0557(7) Uani 1 d . . H624 H 0.0843(35) 0.2122(17) -0.1824(15) 0.069(8) Uiso 1 d . . C625 C 0.3367(4) 0.2478(2) -0.12453(13) 0.0584(7) Uani 1 d . . H625 H 0.3881(34) 0.2596(17) -0.1719(15) 0.064(8) Uiso 1 d . . C626 C 0.4437(3) 0.2523(2) -0.05306(13) 0.0462(5) Uani 1 d . . H626 H 0.5549(31) 0.2680(15) -0.0488(13) 0.047(7) Uiso 1 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 V 0.0327(2) 0.0298(2) 0.0316(2) -0.00203(13) 0.00643(12) 0.00568(13) S1 0.0341(3) 0.0470(3) 0.0567(3) 0.0013(3) 0.0143(2) -0.0022(2) S2 0.0612(4) 0.0461(3) 0.0382(3) 0.0092(2) 0.0098(2) 0.0166(3) S3 0.0459(3) 0.0441(3) 0.0444(3) -0.0099(2) 0.0007(2) 0.0002(2) N4 0.0298(8) 0.0300(8) 0.0376(8) 0.0010(6) 0.0091(6) 0.0045(6) C14 0.0410(11) 0.0336(10) 0.0518(13) 0.0064(9) 0.0023(10) -0.0038(9) C41 0.0426(11) 0.0287(9) 0.0458(12) -0.0027(9) 0.0072(9) 0.0047(9) C24 0.068(2) 0.0472(13) 0.0388(12) 0.0016(10) 0.0227(11) 0.0053(12) C42 0.0451(12) 0.0427(12) 0.0512(13) 0.0017(10) 0.0244(10) 0.0062(10) C34 0.0349(11) 0.0545(14) 0.0537(14) -0.0029(11) -0.0010(10) 0.0005(10) C43 0.0317(10) 0.0418(11) 0.0523(13) 0.0023(10) 0.0017(9) 0.0069(9) N5 0.0389(9) 0.0368(8) 0.0332(8) -0.0041(7) 0.0032(7) 0.0084(7) N6 0.0391(9) 0.0366(9) 0.0332(8) -0.0024(7) 0.0040(7) 0.0112(7) C6 0.0343(9) 0.0274(9) 0.0297(9) -0.0002(7) 0.0064(7) 0.0035(7) C611 0.0327(9) 0.0293(9) 0.0320(9) 0.0030(7) 0.0072(7) 0.0055(7) C612 0.0400(11) 0.0444(12) 0.0375(11) 0.0021(9) 0.0054(9) 0.0050(9) C613 0.0389(12) 0.067(2) 0.0507(13) 0.0124(12) 0.0022(10) 0.0109(11) C614 0.0445(13) 0.0530(14) 0.073(2) 0.0185(13) 0.0168(12) 0.0219(11) C615 0.061(2) 0.0388(12) 0.067(2) -0.0018(11) 0.0208(13) 0.0183(11) C616 0.0442(12) 0.0360(10) 0.0450(12) -0.0041(9) 0.0040(10) 0.0099(9) C621 0.0376(10) 0.0267(9) 0.0329(9) -0.0018(7) 0.0038(8) 0.0074(7) C622 0.0420(11) 0.0418(11) 0.0460(12) -0.0039(10) 0.0064(10) -0.0001(9) C623 0.0448(13) 0.0457(13) 0.067(2) -0.0152(12) -0.0134(12) 0.0036(11) C624 0.074(2) 0.0431(12) 0.0433(13) -0.0075(10) -0.0136(12) 0.0199(12) C625 0.077(2) 0.064(2) 0.0333(12) 0.0062(11) 0.0050(12) 0.0198(14) C626 0.0468(13) 0.0539(13) 0.0384(11) 0.0071(10) 0.0077(10) 0.0075(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V N5 1.691(2) . ? V N4 2.2229(15) . ? V S3 2.2562(7) . ? V S1 2.2665(6) . ? V S2 2.2679(7) . ? S1 C14 1.818(2) . ? S2 C24 1.821(2) . ? S3 C34 1.821(2) . ? N4 C41 1.486(3) . ? N4 C42 1.492(2) . ? N4 C43 1.497(3) . ? C14 C41 1.507(3) . ? C14 H14A 0.96(3) . ? C14 H14B 0.98(2) . ? C41 H41A 0.97(2) . ? C41 H41B 0.95(2) . ? C24 C42 1.501(3) . ? C24 H24A 0.93(3) . ? C24 H24B 1.00(3) . ? C42 H42A 1.00(2) . ? C42 H42B 0.95(2) . ? C34 C43 1.504(3) . ? C34 H34A 0.93(3) . ? C34 H34B 1.00(3) . ? C43 H43A 0.98(2) . ? C43 H43B 0.99(2) . ? N5 N6 1.311(2) . ? N6 C6 1.306(2) . ? C6 C611 1.473(2) . ? C6 C621 1.482(3) . ? C611 C612 1.389(3) . ? C611 C616 1.394(3) . ? C612 C613 1.376(3) . ? C612 H612 0.92(2) . ? C613 C614 1.375(4) . ? C613 H613 0.94(3) . ? C614 C615 1.372(4) . ? C614 H614 0.94(3) . ? C615 C616 1.390(3) . ? C615 H615 0.96(3) . ? C616 H616 0.91(2) . ? C621 C622 1.386(3) . ? C621 C626 1.386(3) . ? C622 C623 1.386(3) . ? C622 H622 0.94(2) . ? C623 C624 1.367(4) . ? C623 H623 0.86(3) . ? C624 C625 1.377(4) . ? C624 H624 1.00(3) . ? C625 C626 1.382(3) . ? C625 H625 0.98(3) . ? C626 H626 0.86(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 V N4 176.08(7) . . ? N5 V S3 98.46(6) . . ? N4 V S3 84.26(5) . . ? N5 V S1 96.79(6) . . ? N4 V S1 84.24(4) . . ? S3 V S1 119.62(3) . . ? N5 V S2 92.22(6) . . ? N4 V S2 83.97(4) . . ? S3 V S2 119.41(3) . . ? S1 V S2 117.90(3) . . ? C14 S1 V 102.20(7) . . ? C24 S2 V 102.74(8) . . ? C34 S3 V 102.93(8) . . ? C41 N4 C42 108.8(2) . . ? C41 N4 C43 109.1(2) . . ? C42 N4 C43 109.3(2) . . ? C41 N4 V 109.77(11) . . ? C42 N4 V 110.00(12) . . ? C43 N4 V 109.82(12) . . ? C41 C14 S1 110.38(15) . . ? C41 C14 H14A 110.5(15) . . ? S1 C14 H14A 109.1(15) . . ? C41 C14 H14B 112.0(14) . . ? S1 C14 H14B 108.9(14) . . ? H14A C14 H14B 105.8(20) . . ? N4 C41 C14 111.1(2) . . ? N4 C41 H41A 107.2(12) . . ? C14 C41 H41A 111.3(12) . . ? N4 C41 H41B 108.9(14) . . ? C14 C41 H41B 107.8(13) . . ? H41A C41 H41B 110.5(18) . . ? C42 C24 S2 110.7(2) . . ? C42 C24 H24A 111.4(17) . . ? S2 C24 H24A 107.2(16) . . ? C42 C24 H24B 112.7(16) . . ? S2 C24 H24B 108.5(16) . . ? H24A C24 H24B 106.1(22) . . ? N4 C42 C24 111.6(2) . . ? N4 C42 H42A 106.0(14) . . ? C24 C42 H42A 110.2(14) . . ? N4 C42 H42B 105.5(14) . . ? C24 C42 H42B 112.9(14) . . ? H42A C42 H42B 110.4(19) . . ? C43 C34 S3 110.7(2) . . ? C43 C34 H34A 111.2(17) . . ? S3 C34 H34A 107.3(17) . . ? C43 C34 H34B 112.1(14) . . ? S3 C34 H34B 109.7(14) . . ? H34A C34 H34B 105.6(22) . . ? N4 C43 C34 111.5(2) . . ? N4 C43 H43A 106.6(13) . . ? C34 C43 H43A 111.7(13) . . ? N4 C43 H43B 109.5(14) . . ? C34 C43 H43B 111.9(14) . . ? H43A C43 H43B 105.4(19) . . ? N6 N5 V 167.00(14) . . ? C6 N6 N5 121.2(2) . . ? N6 C6 C611 116.8(2) . . ? N6 C6 C621 123.8(2) . . ? C611 C6 C621 119.4(2) . . ? C612 C611 C616 118.5(2) . . ? C612 C611 C6 121.1(2) . . ? C616 C611 C6 120.4(2) . . ? C613 C612 C611 120.4(2) . . ? C613 C612 H612 121.6(14) . . ? C611 C612 H612 117.9(14) . . ? C614 C613 C612 120.9(2) . . ? C614 C613 H613 121.1(17) . . ? C612 C613 H613 118.0(17) . . ? C615 C614 C613 119.7(2) . . ? C615 C614 H614 118.0(16) . . ? C613 C614 H614 122.2(16) . . ? C614 C615 C616 120.2(2) . . ? C614 C615 H615 122.8(15) . . ? C616 C615 H615 117.0(16) . . ? C615 C616 C611 120.4(2) . . ? C615 C616 H616 120.1(13) . . ? C611 C616 H616 119.5(13) . . ? C622 C621 C626 119.1(2) . . ? C622 C621 C6 120.9(2) . . ? C626 C621 C6 119.8(2) . . ? C623 C622 C621 119.9(2) . . ? C623 C622 H622 120.7(14) . . ? C621 C622 H622 119.3(14) . . ? C624 C623 C622 120.7(2) . . ? C624 C623 H623 122.9(17) . . ? C622 C623 H623 116.4(17) . . ? C623 C624 C625 119.6(2) . . ? C623 C624 H624 118.8(15) . . ? C625 C624 H624 121.6(15) . . ? C624 C625 C626 120.5(2) . . ? C624 C625 H625 119.0(15) . . ? C626 C625 H625 120.2(15) . . ? C625 C626 C621 120.1(2) . . ? C625 C626 H626 121.1(16) . . ? C621 C626 H626 118.8(16) . . ? 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 V S1 C14 C41 28.8(2) . . . . ? S1 C14 C41 N4 -51.9(2) . . . . ? C14 C41 N4 V 48.5(2) . . . . ? V S2 C24 C42 26.5(2) . . . . ? S2 C24 C42 N4 -49.8(2) . . . . ? C24 C42 N4 V 48.2(2) . . . . ? V S3 C34 C43 26.4(2) . . . . ? S3 C34 C43 N4 -49.5(2) . . . . ? C34 C43 N4 V 47.8(2) . . . . ? V N5 N6 C6 179.1(6) . . . . ? _refine_diff_density_max 0.293 _refine_diff_density_min -0.220 _refine_diff_density_rms 0.055 #===END