Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_[[V2(O)(phen)4Cl2]Cl2_(CH3)2CO (1)] _database_code_CSD 167774 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C54 H44 Cl4 N8 O3 V2 ' _chemical_formula_moiety '?' _chemical_formula_weight 1096.65 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pbcn' _symmetry_Int_Tables_number 60 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2-y,1/2+z 1/2+x,1/2-y,-z -x,y,1/2-z -x,-y,-z 1/2+x,1/2+y,1/2-z 1/2-x,1/2+y,z x,-y,1/2+z _cell_length_a 18.209(8) _cell_length_b 10.673(3) _cell_length_c 25.087(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4876(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 6.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'brick' _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 0.999 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w _diffrn_reflns_number 3310 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 24.98 _diffrn_measured_fraction_theta_max 0.7732 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.7732 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 0 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.95 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3310 _reflns_number_gt 1535 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.0696 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 1535 _refine_ls_number_parameters 321 _refine_ls_goodness_of_fit_ref 1.435 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00090|Fo|^2^]' _refine_ls_shift/su_max 0.0015 _refine_diff_density_max 0.57 _refine_diff_density_min -0.28 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 V(1) V 0.91222(9) 0.0418(1) 0.21984(7) 0.0395(5) Uani 1.00 d . . . Cl(1) Cl 0.8490(1) 0.2143(2) 0.2557(1) 0.0554(8) Uani 1.00 d . . . Cl(2) Cl 0.3645(2) 0.0112(3) 0.0539(1) 0.087(1) Uani 1.00 d . . . O(1) O 1.0000 0.0592(7) 0.2500 0.039(3) Uani 1.00 d S . . O(2) O 0.0761(6) 0.016(1) 0.0608(5) 0.143(5) Uani 1.00 d . . . N(1) N 0.8184(4) 0.0109(7) 0.1673(3) 0.042(3) Uani 1.00 d . . . N(2) N 0.9378(4) 0.1482(7) 0.1518(3) 0.043(3) Uani 1.00 d . . . N(3) N 0.8678(4) -0.0882(7) 0.2750(3) 0.045(3) Uani 1.00 d . . . N(4) N 0.9429(4) -0.1341(7) 0.1878(3) 0.045(3) Uani 1.00 d . . . C(1) C 0.7593(6) -0.0575(10) 0.1745(4) 0.053(4) Uani 1.00 d . . . C(2) C 0.7036(6) -0.069(1) 0.1367(5) 0.060(4) Uani 1.00 d . . . C(3) C 0.7086(6) -0.007(1) 0.0905(5) 0.062(4) Uani 1.00 d . . . C(4) C 0.7703(6) 0.0659(9) 0.0811(4) 0.049(4) Uani 1.00 d . . . C(5) C 0.7816(7) 0.134(1) 0.0337(5) 0.071(5) Uani 1.00 d . . . C(6) C 0.8402(7) 0.207(1) 0.0267(4) 0.066(4) Uani 1.00 d . . . C(7) C 0.8951(6) 0.216(1) 0.0664(4) 0.048(4) Uani 1.00 d . . . C(8) C 0.9580(7) 0.2938(10) 0.0626(5) 0.062(4) Uani 1.00 d . . . C(9) C 1.0080(7) 0.299(1) 0.1031(5) 0.059(4) Uani 1.00 d . . . C(10) C 0.9963(6) 0.2211(10) 0.1465(4) 0.053(3) Uani 1.00 d . . . C(11) C 0.8883(5) 0.1471(9) 0.1124(4) 0.040(3) Uani 1.00 d . . . C(12) C 0.8243(5) 0.0727(9) 0.1199(4) 0.042(3) Uani 1.00 d . . . C(13) C 0.8303(6) -0.062(1) 0.3188(5) 0.063(4) Uani 1.00 d . . . C(14) C 0.8045(7) -0.156(2) 0.3523(5) 0.080(5) Uani 1.00 d . . . C(15) C 0.8154(7) -0.275(2) 0.3404(6) 0.076(5) Uani 1.00 d . . . C(16) C 0.8545(6) -0.3091(10) 0.2937(5) 0.064(4) Uani 1.00 d . . . C(17) C 0.8704(7) -0.432(1) 0.2775(7) 0.084(5) Uani 1.00 d . . . C(18) C 0.9082(8) -0.456(1) 0.2334(6) 0.077(5) Uani 1.00 d . . . C(19) C 0.9342(6) -0.358(1) 0.2001(5) 0.061(4) Uani 1.00 d . . . C(20) C 0.9742(7) -0.375(1) 0.1538(6) 0.074(5) Uani 1.00 d . . . C(21) C 0.9977(6) -0.275(1) 0.1258(5) 0.065(4) Uani 1.00 d . . . C(22) C 0.9818(6) -0.154(1) 0.1436(5) 0.057(4) Uani 1.00 d . . . C(23) C 0.9200(5) -0.2343(8) 0.2151(5) 0.046(3) Uani 1.00 d . . . C(24) C 0.8795(5) -0.2094(10) 0.2623(5) 0.050(4) Uani 1.00 d . . . C(25) C 0.115(1) 0.097(2) 0.0365(7) 0.104(7) Uani 1.00 d . . . C(26) C 0.092(1) 0.137(2) -0.0147(7) 0.149(8) Uani 1.00 d . . . C(27) C 0.1761(8) 0.155(2) 0.0622(6) 0.118(7) Uani 1.00 d . . . H(1) H 0.7541 -0.1017 0.2073 0.0633 Uiso 1.00 calc . . . H(2) H 0.6623 -0.1210 0.1435 0.0721 Uiso 1.00 calc . . . H(3) H 0.6705 -0.0121 0.0647 0.0739 Uiso 1.00 calc . . . H(4) H 0.7463 0.1280 0.0059 0.0843 Uiso 1.00 calc . . . H(5) H 0.8450 0.2541 -0.0054 0.0795 Uiso 1.00 calc . . . H(6) H 0.9654 0.3435 0.0316 0.0749 Uiso 1.00 calc . . . H(7) H 1.0494 0.3529 0.1015 0.0709 Uiso 1.00 calc . . . H(8) H 1.0321 0.2200 0.1741 0.0644 Uiso 1.00 calc . . . H(9) H 0.8208 0.0234 0.3275 0.0754 Uiso 1.00 calc . . . H(10) H 0.7787 -0.1338 0.3840 0.0960 Uiso 1.00 calc . . . H(11) H 0.7968 -0.3380 0.3634 0.0903 Uiso 1.00 calc . . . H(12) H 0.8535 -0.5000 0.2987 0.0995 Uiso 1.00 calc . . . H(13) H 0.9180 -0.5409 0.2240 0.0924 Uiso 1.00 calc . . . H(14) H 0.9850 -0.4572 0.1417 0.0884 Uiso 1.00 calc . . . H(15) H 1.0250 -0.2863 0.0938 0.0785 Uiso 1.00 calc . . . H(16) H 0.9994 -0.0839 0.1237 0.0675 Uiso 1.00 calc . . . H(17) H 0.1273 0.1964 -0.0277 0.1771 Uiso 1.00 calc . . . H(18) H 0.0906 0.0674 -0.0378 0.1771 Uiso 1.00 calc . . . H(19) H 0.0458 0.1752 -0.0121 0.1771 Uiso 1.00 calc . . . H(20) H 0.2107 0.0924 0.0722 0.1411 Uiso 1.00 calc . . . H(21) H 0.1988 0.2121 0.0382 0.1411 Uiso 1.00 calc . . . H(22) H 0.1598 0.1983 0.0929 0.1411 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V(1) 0.0373(9) 0.0367(9) 0.045(1) -0.0027(9) -0.0028(9) 0.0039(9) Cl(1) 0.050(2) 0.047(1) 0.069(2) 0.009(1) -0.001(1) -0.004(2) Cl(2) 0.093(2) 0.072(2) 0.097(3) 0.013(2) -0.038(2) 0.006(2) O(1) 0.039(5) 0.034(5) 0.045(5) 0.0000 0.002(4) 0.0000 O(2) 0.14(1) 0.124(10) 0.16(1) -0.004(9) 0.028(9) 0.006(8) N(1) 0.031(5) 0.044(5) 0.050(6) -0.006(4) -0.002(4) -0.004(4) N(2) 0.036(5) 0.036(5) 0.056(6) -0.002(4) 0.003(4) 0.007(4) N(3) 0.039(5) 0.053(6) 0.042(6) -0.009(4) -0.008(4) 0.008(5) N(4) 0.046(5) 0.042(5) 0.046(5) 0.002(4) -0.002(5) -0.001(5) C(1) 0.056(7) 0.056(7) 0.048(7) -0.008(6) -0.004(6) 0.008(6) C(2) 0.047(7) 0.064(8) 0.070(8) -0.011(6) -0.011(6) 0.000(7) C(3) 0.048(8) 0.069(8) 0.068(9) -0.008(7) -0.022(7) -0.015(7) C(4) 0.052(7) 0.054(7) 0.040(7) 0.009(6) -0.006(5) 0.001(6) C(5) 0.073(9) 0.068(9) 0.071(9) 0.013(8) -0.019(7) -0.017(7) C(6) 0.081(9) 0.071(9) 0.047(8) 0.010(8) 0.000(7) 0.009(7) C(7) 0.055(7) 0.055(7) 0.035(7) 0.007(6) 0.003(5) -0.003(6) C(8) 0.079(9) 0.053(7) 0.055(8) 0.005(7) 0.029(7) 0.009(7) C(9) 0.057(8) 0.045(7) 0.076(9) -0.005(6) 0.021(7) 0.002(7) C(10) 0.053(7) 0.042(6) 0.066(8) 0.008(6) 0.006(6) 0.005(6) C(11) 0.042(7) 0.045(6) 0.032(6) 0.002(5) 0.003(5) 0.000(5) C(12) 0.043(6) 0.041(7) 0.042(7) 0.010(5) -0.007(5) -0.003(5) C(13) 0.060(8) 0.066(8) 0.063(8) -0.014(6) 0.000(7) 0.003(8) C(14) 0.077(10) 0.10(1) 0.063(9) -0.032(9) 0.003(7) 0.012(10) C(15) 0.064(9) 0.10(1) 0.064(10) -0.038(9) -0.014(7) 0.028(9) C(16) 0.058(8) 0.043(8) 0.09(1) -0.021(6) -0.023(8) 0.013(7) C(17) 0.078(10) 0.045(8) 0.13(1) -0.022(7) -0.038(10) 0.020(10) C(18) 0.081(9) 0.039(7) 0.11(1) -0.007(8) -0.031(9) 0.002(9) C(19) 0.071(9) 0.037(7) 0.076(9) 0.000(6) -0.028(7) -0.011(7) C(20) 0.08(1) 0.053(8) 0.09(1) 0.009(8) -0.032(8) -0.034(8) C(21) 0.057(7) 0.065(8) 0.074(8) 0.010(7) -0.004(7) -0.020(8) C(22) 0.053(8) 0.056(7) 0.061(8) 0.009(6) -0.016(7) 0.002(6) C(23) 0.036(6) 0.029(6) 0.072(8) 0.004(5) -0.017(6) 0.004(6) C(24) 0.037(6) 0.037(7) 0.077(9) -0.007(6) -0.025(6) 0.002(6) C(25) 0.13(2) 0.09(1) 0.10(1) 0.01(1) 0.02(1) 0.00(1) C(26) 0.16(2) 0.20(2) 0.08(1) 0.07(2) 0.00(1) -0.02(1) C(27) 0.08(1) 0.14(1) 0.13(1) -0.03(1) -0.021(10) 0.03(1) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V(1) Cl(1) 2.351(3) . . yes V(1) O(1) 1.778(2) . . yes V(1) N(1) 2.183(7) . . yes V(1) N(2) 2.103(8) . . yes V(1) N(3) 2.119(8) . . yes V(1) N(4) 2.118(8) . . yes O(2) C(25) 1.27(2) . . yes N(1) C(1) 1.31(1) . . yes N(1) C(12) 1.36(1) . . yes N(2) C(10) 1.33(1) . . yes N(2) C(11) 1.34(1) . . yes N(3) C(13) 1.33(1) . . yes N(3) C(24) 1.35(1) . . yes N(4) C(22) 1.33(1) . . yes N(4) C(23) 1.34(1) . . yes C(1) C(2) 1.39(1) . . yes C(1) H(1) 0.953 . . no C(2) C(3) 1.34(1) . . yes C(2) H(2) 0.951 . . no C(3) C(4) 1.38(1) . . yes C(3) H(3) 0.952 . . no C(4) C(5) 1.41(1) . . yes C(4) C(12) 1.39(1) . . yes C(5) C(6) 1.33(2) . . yes C(5) H(4) 0.952 . . no C(6) C(7) 1.41(1) . . yes C(6) H(5) 0.953 . . no C(7) C(8) 1.42(1) . . yes C(7) C(11) 1.37(1) . . yes C(8) C(9) 1.37(1) . . yes C(8) H(6) 0.952 . . no C(9) C(10) 1.38(1) . . yes C(9) H(7) 0.951 . . no C(10) H(8) 0.952 . . no C(11) C(12) 1.42(1) . . yes C(13) C(14) 1.39(2) . . yes C(13) H(9) 0.952 . . no C(14) C(15) 1.32(2) . . yes C(14) H(10) 0.951 . . no C(15) C(16) 1.42(2) . . yes C(15) H(11) 0.951 . . no C(16) C(17) 1.40(2) . . yes C(16) C(24) 1.40(1) . . yes C(17) C(18) 1.33(2) . . yes C(17) H(12) 0.953 . . no C(18) C(19) 1.42(2) . . yes C(18) H(13) 0.950 . . no C(19) C(20) 1.38(2) . . yes C(19) C(23) 1.40(1) . . yes C(20) C(21) 1.35(2) . . yes C(20) H(14) 0.951 . . no C(21) C(22) 1.39(1) . . yes C(21) H(15) 0.952 . . no C(22) H(16) 0.953 . . no C(23) C(24) 1.42(1) . . yes C(25) C(26) 1.42(2) . . yes C(25) C(27) 1.43(2) . . yes C(26) H(17) 0.950 . . no C(26) H(18) 0.946 . . no C(26) H(19) 0.943 . . no C(27) H(20) 0.950 . . no C(27) H(21) 0.953 . . no C(27) H(22) 0.947 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) V(1) O(1) 101.3(2) . . . yes Cl(1) V(1) N(1) 88.1(2) . . . yes Cl(1) V(1) N(2) 89.8(2) . . . yes Cl(1) V(1) N(3) 94.3(3) . . . yes Cl(1) V(1) N(4) 165.7(2) . . . yes O(1) V(1) N(1) 167.5(2) . . . yes O(1) V(1) N(2) 95.2(3) . . . yes O(1) V(1) N(3) 97.7(3) . . . yes O(1) V(1) N(4) 90.9(3) . . . yes N(1) V(1) N(2) 76.4(3) . . . yes N(1) V(1) N(3) 89.8(3) . . . yes N(1) V(1) N(4) 81.0(3) . . . yes N(2) V(1) N(3) 165.5(3) . . . yes N(2) V(1) N(4) 96.4(3) . . . yes N(3) V(1) N(4) 76.6(3) . . . yes V(1) O(1) V(1) 168.0(5) . . 4_755 yes C(1) N(1) C(12) 116.9(8) . . . yes C(10) N(2) C(11) 118.2(9) . . . yes C(13) N(3) C(24) 118.6(9) . . . yes C(22) N(4) C(23) 117.7(9) . . . yes N(1) C(1) C(2) 123.5(10) . . . yes N(1) C(1) H(1) 118.3 . . . no C(2) C(1) H(1) 118.2 . . . no C(1) C(2) C(3) 119(1) . . . yes C(1) C(2) H(2) 120.3 . . . no C(3) C(2) H(2) 120.0 . . . no C(2) C(3) C(4) 118.7(10) . . . yes C(2) C(3) H(3) 120.7 . . . no C(4) C(3) H(3) 120.6 . . . no C(3) C(4) C(5) 123(1) . . . yes C(3) C(4) C(12) 119(1) . . . yes C(5) C(4) C(12) 117(1) . . . yes C(4) C(5) C(6) 122(1) . . . yes C(4) C(5) H(4) 118.8 . . . no C(6) C(5) H(4) 119.1 . . . no C(5) C(6) C(7) 120(1) . . . yes C(5) C(6) H(5) 119.4 . . . no C(7) C(6) H(5) 119.7 . . . no C(6) C(7) C(8) 124(1) . . . yes C(6) C(7) C(11) 119(1) . . . yes C(8) C(7) C(11) 116.2(10) . . . yes C(7) C(8) C(9) 120(1) . . . yes C(7) C(8) H(6) 119.6 . . . no C(9) C(8) H(6) 119.6 . . . no C(8) C(9) C(10) 117(1) . . . yes C(8) C(9) H(7) 121.3 . . . no C(10) C(9) H(7) 121.3 . . . no N(2) C(10) C(9) 123(1) . . . yes N(2) C(10) H(8) 118.1 . . . no C(9) C(10) H(8) 118.2 . . . no N(2) C(11) C(7) 123.7(9) . . . yes N(2) C(11) C(12) 117.4(9) . . . yes C(7) C(11) C(12) 118.9(10) . . . yes N(1) C(12) C(4) 122.0(9) . . . yes N(1) C(12) C(11) 116.7(9) . . . yes C(4) C(12) C(11) 121.2(10) . . . yes N(3) C(13) C(14) 121(1) . . . yes N(3) C(13) H(9) 119.1 . . . no C(14) C(13) H(9) 119.2 . . . no C(13) C(14) C(15) 120(1) . . . yes C(13) C(14) H(10) 119.8 . . . no C(15) C(14) H(10) 119.9 . . . no C(14) C(15) C(16) 120(1) . . . yes C(14) C(15) H(11) 119.5 . . . no C(16) C(15) H(11) 119.8 . . . no C(15) C(16) C(17) 125(1) . . . yes C(15) C(16) C(24) 115(1) . . . yes C(17) C(16) C(24) 118(1) . . . yes C(16) C(17) C(18) 122(1) . . . yes C(16) C(17) H(12) 119.0 . . . no C(18) C(17) H(12) 118.8 . . . no C(17) C(18) C(19) 121(1) . . . yes C(17) C(18) H(13) 119.3 . . . no C(19) C(18) H(13) 119.6 . . . no C(18) C(19) C(20) 124(1) . . . yes C(18) C(19) C(23) 118(1) . . . yes C(20) C(19) C(23) 116(1) . . . yes C(19) C(20) C(21) 120(1) . . . yes C(19) C(20) H(14) 119.8 . . . no C(21) C(20) H(14) 120.1 . . . no C(20) C(21) C(22) 120(1) . . . yes C(20) C(21) H(15) 120.0 . . . no C(22) C(21) H(15) 120.0 . . . no N(4) C(22) C(21) 121(1) . . . yes N(4) C(22) H(16) 119.3 . . . no C(21) C(22) H(16) 119.2 . . . no N(4) C(23) C(19) 124(1) . . . yes N(4) C(23) C(24) 116.1(9) . . . yes C(19) C(23) C(24) 119(1) . . . yes N(3) C(24) C(16) 123(1) . . . yes N(3) C(24) C(23) 117.2(9) . . . yes C(16) C(24) C(23) 119(1) . . . yes O(2) C(25) C(26) 118(1) . . . yes O(2) C(25) C(27) 120(1) . . . yes C(26) C(25) C(27) 120(1) . . . yes C(25) C(26) H(17) 108.7 . . . no C(25) C(26) H(18) 108.9 . . . no C(25) C(26) H(19) 109.1 . . . no H(17) C(26) H(18) 109.8 . . . no H(17) C(26) H(19) 110.0 . . . no H(18) C(26) H(19) 110.4 . . . no C(25) C(27) H(20) 109.4 . . . no C(25) C(27) H(21) 109.3 . . . no C(25) C(27) H(22) 109.6 . . . no H(20) C(27) H(21) 109.2 . . . no H(20) C(27) H(22) 109.7 . . . no H(21) C(27) H(22) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #=END #------------------------------------------------------------------------------ data_V2(bpyam)4Cl4 _database_code_CSD 167775 _audit_creation_date 'Mon Feb 4 18:36:13 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C40 H36 Cl4 N12 O V2 ' _chemical_formula_moiety '?' _chemical_formula_weight 944.50 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 35.158(8) _cell_length_b 16.984(4) _cell_length_c 20.180(8) _cell_angle_alpha 90 _cell_angle_beta 112.09(3) _cell_angle_gamma 90 _cell_volume 11165(5) _cell_formula_units_Z 8 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 11.4 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'violet' _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.563 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.811 _exptl_absorpt_correction_T_max 0.945 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 13537 _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.9995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.9995 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 9.84 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 12839 _reflns_number_gt 4786 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.1031 _refine_ls_wR_factor_ref 0.1675 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4786 _refine_ls_number_parameters 534 _refine_ls_goodness_of_fit_ref 2.739 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00203|Fo|^2^]' _refine_ls_shift/su_max 0.0002 _refine_diff_density_max 2.58 _refine_diff_density_min -0.53 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 V(1) V 0.15927(7) 0.7945(1) 0.1560(1) 0.0378(6) Uani 1.00 d . . . V(2) V 0.14026(7) 0.9700(1) 0.0523(1) 0.0405(6) Uani 1.00 d . . . Cl(1) Cl 0.1834(1) 0.7095(2) 0.0851(2) 0.057(1) Uani 1.00 d . . . Cl(2) Cl 0.0940(1) 0.9079(3) -0.0536(2) 0.063(1) Uani 1.00 d . . . Cl(3) Cl 0.7500 0.2500 0.5000 0.064(2) Uani 1.00 d S . . Cl(4) Cl 1.0000 0.2333(5) 0.7500 0.093(3) Uani 1.00 d S . . Cl(5) Cl 0.5971(3) 0.2094(6) 0.6644(8) 0.259(6) Uani 1.00 d . . . O(1) O 0.1548(3) 0.8811(5) 0.1049(4) 0.039(2) Uani 1.00 d . . . N(1) N 0.1639(3) 0.6938(7) 0.2260(6) 0.046(4) Uani 1.00 d . . . N(2) N 0.2103(4) 0.7620(8) 0.3274(6) 0.057(4) Uani 1.00 d . . . N(3) N 0.2215(3) 0.8081(7) 0.2285(6) 0.044(3) Uani 1.00 d . . . N(4) N 0.1374(3) 0.8607(6) 0.2248(5) 0.041(3) Uani 1.00 d . . . N(5) N 0.0779(3) 0.7825(7) 0.2024(6) 0.049(4) Uani 1.00 d . . . N(6) N 0.0959(3) 0.7630(6) 0.1031(6) 0.043(3) Uani 1.00 d . . . N(7) N 0.1248(3) 1.0789(7) -0.0106(6) 0.051(4) Uani 1.00 d . . . N(8) N 0.1947(4) 1.1050(7) 0.0089(6) 0.053(4) Uani 1.00 d . . . N(9) N 0.1878(3) 0.9669(7) 0.0114(6) 0.049(4) Uani 1.00 d . . . N(10) N 0.1762(3) 1.0445(7) 0.1396(6) 0.045(3) Uani 1.00 d . . . N(11) N 0.1208(4) 1.1203(8) 0.1372(8) 0.069(5) Uani 1.00 d . . . N(12) N 0.0923(3) 0.9983(8) 0.0902(6) 0.050(4) Uani 1.00 d . . . C(1) C 0.1423(5) 0.6267(9) 0.2005(8) 0.054(5) Uani 1.00 d . . . C(2) C 0.1365(6) 0.570(1) 0.2394(10) 0.073(6) Uani 1.00 d . . . C(3) C 0.1538(7) 0.575(1) 0.312(1) 0.089(8) Uani 1.00 d . . . C(4) C 0.1775(6) 0.640(1) 0.3425(9) 0.076(7) Uani 1.00 d . . . C(5) C 0.1829(5) 0.6982(9) 0.2966(8) 0.055(5) Uani 1.00 d . . . C(6) C 0.2344(4) 0.7985(9) 0.2977(8) 0.049(4) Uani 1.00 d . . . C(7) C 0.2730(6) 0.822(1) 0.3445(8) 0.073(6) Uani 1.00 d . . . C(8) C 0.2995(6) 0.853(1) 0.319(1) 0.087(7) Uani 1.00 d . . . C(9) C 0.2873(5) 0.860(1) 0.244(1) 0.077(7) Uani 1.00 d . . . C(10) C 0.2487(4) 0.8365(9) 0.2014(8) 0.053(5) Uani 1.00 d . . . C(11) C 0.1598(5) 0.9252(9) 0.2567(8) 0.053(5) Uani 1.00 d . . . C(12) C 0.1486(5) 0.9728(9) 0.3021(8) 0.062(5) Uani 1.00 d . . . C(13) C 0.1134(6) 0.960(1) 0.3120(9) 0.073(6) Uani 1.00 d . . . C(14) C 0.0914(5) 0.896(1) 0.2819(9) 0.065(6) Uani 1.00 d . . . C(15) C 0.1029(4) 0.8455(9) 0.2349(7) 0.048(4) Uani 1.00 d . . . C(16) C 0.0689(4) 0.7564(9) 0.1352(7) 0.047(4) Uani 1.00 d . . . C(17) C 0.0316(5) 0.722(1) 0.1047(9) 0.073(6) Uani 1.00 d . . . C(18) C 0.0194(6) 0.701(1) 0.030(1) 0.104(8) Uani 1.00 d . . . C(19) C 0.0453(6) 0.710(1) -0.0052(9) 0.087(7) Uani 1.00 d . . . C(20) C 0.0837(5) 0.7413(10) 0.0331(8) 0.057(5) Uani 1.00 d . . . C(21) C 0.0845(4) 1.103(1) -0.0398(9) 0.067(6) Uani 1.00 d . . . C(22) C 0.0725(5) 1.174(1) -0.066(1) 0.079(6) Uani 1.00 d . . . C(23) C 0.1024(7) 1.228(1) -0.061(1) 0.109(9) Uani 1.00 d . . . C(24) C 0.1430(6) 1.208(1) -0.037(1) 0.093(7) Uani 1.00 d . . . C(25) C 0.1531(5) 1.1296(9) -0.0133(8) 0.054(5) Uani 1.00 d . . . C(26) C 0.2088(4) 1.0298(9) 0.0013(7) 0.048(4) Uani 1.00 d . . . C(27) C 0.2430(5) 1.024(1) -0.0172(9) 0.060(5) Uani 1.00 d . . . C(28) C 0.2557(5) 0.954(1) -0.027(1) 0.082(7) Uani 1.00 d . . . C(29) C 0.2343(6) 0.886(1) -0.021(1) 0.081(7) Uani 1.00 d . . . C(30) C 0.2012(5) 0.8924(10) -0.0014(9) 0.061(5) Uani 1.00 d . . . C(31) C 0.2171(4) 1.0268(9) 0.1721(8) 0.055(5) Uani 1.00 d . . . C(32) C 0.2431(5) 1.067(1) 0.2285(9) 0.066(5) Uani 1.00 d . . . C(33) C 0.2280(6) 1.131(1) 0.2566(10) 0.078(7) Uani 1.00 d . . . C(34) C 0.1878(6) 1.148(1) 0.224(1) 0.082(7) Uani 1.00 d . . . C(35) C 0.1609(5) 1.1031(9) 0.1649(9) 0.057(5) Uani 1.00 d . . . C(36) C 0.0887(5) 1.067(1) 0.1164(9) 0.064(6) Uani 1.00 d . . . C(37) C 0.0523(7) 1.089(1) 0.125(1) 0.103(9) Uani 1.00 d . . . C(38) C 0.0210(5) 1.036(2) 0.108(1) 0.101(8) Uani 1.00 d . . . C(39) C 0.0262(5) 0.960(1) 0.085(1) 0.081(7) Uani 1.00 d . . . C(40) C 0.0609(4) 0.9443(10) 0.0752(9) 0.060(5) Uani 1.00 d . . . H(1) H 0.2117 0.7807 0.3726 0.0690 Uiso 1.00 calc . . . H(2) H 0.0658 0.7548 0.2304 0.0593 Uiso 1.00 calc . . . H(3) H 0.2150 1.1436 0.0313 0.0630 Uiso 1.00 calc . . . H(4) H 0.1137 1.1745 0.1311 0.0828 Uiso 1.00 calc . . . H(5) H 0.1304 0.6204 0.1501 0.0647 Uiso 1.00 calc . . . H(6) H 0.1203 0.5256 0.2174 0.0871 Uiso 1.00 calc . . . H(7) H 0.1497 0.5351 0.3410 0.1074 Uiso 1.00 calc . . . H(8) H 0.1897 0.6461 0.3930 0.0917 Uiso 1.00 calc . . . H(9) H 0.2804 0.8158 0.3946 0.0873 Uiso 1.00 calc . . . H(10) H 0.3257 0.8712 0.3508 0.1041 Uiso 1.00 calc . . . H(11) H 0.3057 0.8796 0.2233 0.0930 Uiso 1.00 calc . . . H(12) H 0.2406 0.8403 0.1510 0.0634 Uiso 1.00 calc . . . H(13) H 0.1837 0.9379 0.2477 0.0634 Uiso 1.00 calc . . . H(14) H 0.1659 1.0150 0.3264 0.0742 Uiso 1.00 calc . . . H(15) H 0.1043 0.9948 0.3396 0.0874 Uiso 1.00 calc . . . H(16) H 0.0678 0.8829 0.2918 0.0784 Uiso 1.00 calc . . . H(17) H 0.0145 0.7123 0.1307 0.0877 Uiso 1.00 calc . . . H(18) H -0.0073 0.6798 0.0054 0.1242 Uiso 1.00 calc . . . H(19) H 0.0373 0.6952 -0.0540 0.1048 Uiso 1.00 calc . . . H(20) H 0.1024 0.7480 0.0096 0.0689 Uiso 1.00 calc . . . H(21) H 0.0639 1.0661 -0.0415 0.0807 Uiso 1.00 calc . . . H(22) H 0.0443 1.1878 -0.0866 0.0945 Uiso 1.00 calc . . . H(23) H 0.0948 1.2810 -0.0742 0.1312 Uiso 1.00 calc . . . H(24) H 0.1634 1.2448 -0.0369 0.1112 Uiso 1.00 calc . . . H(25) H 0.2569 1.0704 -0.0228 0.0722 Uiso 1.00 calc . . . H(26) H 0.2796 0.9497 -0.0379 0.0979 Uiso 1.00 calc . . . H(27) H 0.2429 0.8353 -0.0300 0.0970 Uiso 1.00 calc . . . H(28) H 0.1871 0.8464 0.0035 0.0737 Uiso 1.00 calc . . . H(29) H 0.2277 0.9839 0.1542 0.0661 Uiso 1.00 calc . . . H(30) H 0.2713 1.0534 0.2491 0.0791 Uiso 1.00 calc . . . H(31) H 0.2454 1.1594 0.2969 0.0936 Uiso 1.00 calc . . . H(32) H 0.1771 1.1924 0.2403 0.0983 Uiso 1.00 calc . . . H(33) H 0.0495 1.1403 0.1420 0.1240 Uiso 1.00 calc . . . H(34) H -0.0043 1.0505 0.1109 0.1214 Uiso 1.00 calc . . . H(35) H 0.0056 0.9210 0.0772 0.0972 Uiso 1.00 calc . . . H(36) H 0.0640 0.8941 0.0572 0.0725 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V(1) 0.038(1) 0.043(1) 0.035(1) 0.000(1) 0.0163(10) 0.004(1) V(2) 0.032(1) 0.045(1) 0.043(1) -0.004(1) 0.0133(10) 0.007(1) Cl(1) 0.067(2) 0.060(2) 0.052(2) 0.007(2) 0.031(2) -0.004(2) Cl(2) 0.057(2) 0.074(3) 0.049(2) -0.017(2) 0.009(2) 0.003(2) Cl(3) 0.070(4) 0.076(4) 0.040(3) 0.039(3) 0.014(3) -0.002(3) Cl(4) 0.057(4) 0.148(7) 0.089(5) 0.0000 0.044(4) 0.0000 Cl(5) 0.159(8) 0.140(8) 0.47(2) -0.028(6) 0.11(1) 0.10(1) O(1) 0.039(5) 0.043(5) 0.036(5) 0.001(4) 0.016(4) 0.009(4) N(1) 0.055(7) 0.057(8) 0.030(6) 0.009(6) 0.020(5) 0.010(6) N(2) 0.066(8) 0.068(9) 0.033(7) 0.003(7) 0.012(6) -0.002(6) N(3) 0.041(6) 0.049(7) 0.040(7) 0.005(5) 0.012(5) 0.008(5) N(4) 0.043(6) 0.048(7) 0.032(6) 0.003(5) 0.014(5) 0.008(5) N(5) 0.043(6) 0.065(8) 0.050(7) -0.007(6) 0.027(6) 0.000(6) N(6) 0.047(7) 0.045(7) 0.040(7) -0.009(5) 0.020(5) 0.001(5) N(7) 0.031(6) 0.055(8) 0.064(8) -0.003(6) 0.015(6) 0.012(6) N(8) 0.050(7) 0.046(8) 0.061(8) -0.013(6) 0.020(6) 0.005(6) N(9) 0.051(7) 0.045(7) 0.053(7) 0.000(6) 0.024(6) 0.004(6) N(10) 0.040(6) 0.052(8) 0.038(6) -0.008(6) 0.011(5) 0.004(6) N(11) 0.056(9) 0.060(9) 0.09(1) 0.004(7) 0.028(8) -0.015(8) N(12) 0.038(6) 0.057(8) 0.056(8) 0.004(6) 0.021(6) 0.008(6) C(1) 0.060(10) 0.050(10) 0.046(9) -0.001(8) 0.014(7) 0.010(8) C(2) 0.09(1) 0.06(1) 0.06(1) -0.011(10) 0.016(10) 0.008(9) C(3) 0.11(2) 0.07(1) 0.10(2) -0.01(1) 0.05(1) 0.03(1) C(4) 0.10(1) 0.08(1) 0.06(1) 0.02(1) 0.05(1) 0.03(1) C(5) 0.060(9) 0.052(10) 0.058(10) 0.023(8) 0.028(8) 0.015(8) C(6) 0.038(7) 0.063(10) 0.046(8) -0.008(7) 0.015(7) 0.000(7) C(7) 0.08(1) 0.09(1) 0.046(10) 0.00(1) 0.017(9) -0.010(9) C(8) 0.06(1) 0.08(1) 0.09(2) -0.02(1) 0.00(1) 0.00(1) C(9) 0.05(1) 0.09(1) 0.09(1) -0.010(10) 0.03(1) 0.00(1) C(10) 0.038(8) 0.062(10) 0.057(9) 0.004(7) 0.017(7) 0.007(8) C(11) 0.061(9) 0.049(9) 0.046(9) -0.005(8) 0.018(7) -0.004(7) C(12) 0.08(1) 0.06(1) 0.051(9) -0.005(9) 0.029(9) -0.010(8) C(13) 0.08(1) 0.08(1) 0.06(1) 0.00(1) 0.036(10) -0.024(10) C(14) 0.056(10) 0.09(1) 0.06(1) 0.016(10) 0.038(8) -0.009(10) C(15) 0.050(9) 0.058(10) 0.036(8) 0.016(8) 0.017(7) 0.011(7) C(16) 0.042(8) 0.061(10) 0.042(8) -0.011(7) 0.018(7) 0.000(7) C(17) 0.049(10) 0.11(1) 0.06(1) -0.007(10) 0.013(8) 0.00(1) C(18) 0.05(1) 0.13(2) 0.13(2) -0.03(1) 0.03(1) -0.02(2) C(19) 0.08(1) 0.12(2) 0.05(1) -0.02(1) 0.017(10) -0.01(1) C(20) 0.056(10) 0.07(1) 0.049(9) -0.010(8) 0.018(8) -0.004(8) C(21) 0.040(9) 0.07(1) 0.09(1) 0.007(8) 0.017(8) 0.027(10) C(22) 0.045(10) 0.09(1) 0.10(1) 0.014(10) 0.016(9) 0.04(1) C(23) 0.09(2) 0.07(1) 0.16(2) 0.04(1) 0.04(2) 0.06(1) C(24) 0.07(1) 0.06(1) 0.14(2) 0.01(1) 0.04(1) 0.06(1) C(25) 0.050(9) 0.053(10) 0.06(1) -0.004(8) 0.026(8) 0.008(8) C(26) 0.047(8) 0.050(9) 0.041(8) -0.004(7) 0.011(6) 0.011(7) C(27) 0.046(9) 0.06(1) 0.08(1) -0.003(8) 0.030(8) 0.006(9) C(28) 0.05(1) 0.10(2) 0.12(2) 0.00(1) 0.05(1) 0.01(1) C(29) 0.08(1) 0.08(1) 0.11(2) 0.03(1) 0.06(1) 0.00(1) C(30) 0.07(1) 0.05(1) 0.07(1) 0.006(8) 0.029(9) 0.009(8) C(31) 0.044(8) 0.055(10) 0.059(10) -0.008(8) 0.011(7) 0.002(8) C(32) 0.043(9) 0.07(1) 0.07(1) -0.018(9) 0.009(8) 0.005(10) C(33) 0.08(1) 0.07(1) 0.07(1) -0.03(1) 0.02(1) -0.02(1) C(34) 0.09(1) 0.06(1) 0.10(2) -0.01(1) 0.04(1) -0.02(1) C(35) 0.06(1) 0.045(9) 0.07(1) -0.007(8) 0.032(9) -0.013(8) C(36) 0.046(9) 0.08(1) 0.07(1) 0.010(9) 0.028(8) -0.008(10) C(37) 0.07(1) 0.12(2) 0.12(2) 0.02(1) 0.04(1) -0.02(2) C(38) 0.039(10) 0.17(2) 0.10(2) 0.00(1) 0.026(10) 0.00(2) C(39) 0.06(1) 0.09(2) 0.10(1) -0.02(1) 0.04(1) 0.00(1) C(40) 0.038(8) 0.08(1) 0.07(1) 0.000(8) 0.024(8) 0.023(9) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V(1) Cl(1) 2.400(4) . . yes V(1) O(1) 1.768(8) . . yes V(1) N(1) 2.18(1) . . yes V(1) N(3) 2.14(1) . . yes V(1) N(4) 2.14(1) . . yes V(1) N(6) 2.14(1) . . yes V(2) Cl(2) 2.390(4) . . yes V(2) O(1) 1.805(8) . . yes V(2) N(7) 2.19(1) . . yes V(2) N(9) 2.12(1) . . yes V(2) N(10) 2.15(1) . . yes V(2) N(12) 2.15(1) . . yes N(1) C(1) 1.36(2) . . yes N(1) C(5) 1.33(2) . . yes N(2) C(5) 1.43(2) . . yes N(2) C(6) 1.36(2) . . yes N(2) H(1) 0.969 . . no N(3) C(6) 1.30(2) . . yes N(3) C(10) 1.36(2) . . yes N(4) C(11) 1.36(2) . . yes N(4) C(15) 1.33(2) . . yes N(5) C(15) 1.38(2) . . yes N(5) C(16) 1.35(2) . . yes N(5) H(2) 0.959 . . no N(6) C(16) 1.34(2) . . yes N(6) C(20) 1.36(2) . . yes N(7) C(21) 1.38(2) . . yes N(7) C(25) 1.33(2) . . yes N(8) C(25) 1.42(2) . . yes N(8) C(26) 1.40(2) . . yes N(8) H(3) 0.935 . . no N(9) C(26) 1.36(2) . . yes N(9) C(30) 1.41(2) . . yes N(10) C(31) 1.37(2) . . yes N(10) C(35) 1.32(2) . . yes N(11) C(35) 1.34(2) . . yes N(11) C(36) 1.39(2) . . yes N(11) H(4) 0.961 . . no N(12) C(36) 1.30(2) . . yes N(12) C(40) 1.38(2) . . yes C(1) C(2) 1.30(2) . . yes C(1) H(5) 0.964 . . no C(2) C(3) 1.36(3) . . yes C(2) H(6) 0.943 . . no C(3) C(4) 1.38(3) . . yes C(3) H(7) 0.956 . . no C(4) C(5) 1.41(2) . . yes C(4) H(8) 0.951 . . no C(6) C(7) 1.39(2) . . yes C(7) C(8) 1.33(2) . . yes C(7) H(9) 0.957 . . no C(8) C(9) 1.43(3) . . yes C(8) H(10) 0.985 . . no C(9) C(10) 1.36(2) . . yes C(9) H(11) 0.973 . . no C(10) H(12) 0.941 . . no C(11) C(12) 1.38(2) . . yes C(11) H(13) 0.942 . . no C(12) C(13) 1.34(2) . . yes C(12) H(14) 0.974 . . no C(13) C(14) 1.34(2) . . yes C(13) H(15) 0.986 . . no C(14) C(15) 1.44(2) . . yes C(14) H(16) 0.967 . . no C(16) C(17) 1.36(2) . . yes C(17) C(18) 1.45(3) . . yes C(17) H(17) 0.916 . . no C(18) C(19) 1.36(3) . . yes C(18) H(18) 0.974 . . no C(19) C(20) 1.39(2) . . yes C(19) H(19) 0.948 . . no C(20) H(20) 0.926 . . no C(21) C(22) 1.32(2) . . yes C(21) H(21) 0.948 . . no C(22) C(23) 1.37(3) . . yes C(22) H(22) 0.970 . . no C(23) C(24) 1.37(3) . . yes C(23) H(23) 0.934 . . no C(24) C(25) 1.41(2) . . yes C(24) H(24) 0.937 . . no C(26) C(27) 1.39(2) . . yes C(27) C(28) 1.31(2) . . yes C(27) H(25) 0.943 . . no C(28) C(29) 1.42(3) . . yes C(28) H(26) 0.956 . . no C(29) C(30) 1.36(2) . . yes C(29) H(27) 0.960 . . no C(30) H(28) 0.924 . . no C(31) C(32) 1.35(2) . . yes C(31) H(29) 0.956 . . no C(32) C(33) 1.40(3) . . yes C(32) H(30) 0.973 . . no C(33) C(34) 1.35(3) . . yes C(33) H(31) 0.932 . . no C(34) C(35) 1.43(2) . . yes C(34) H(32) 0.962 . . no C(36) C(37) 1.41(2) . . yes C(37) C(38) 1.36(3) . . yes C(37) H(33) 0.955 . . no C(38) C(39) 1.40(3) . . yes C(38) H(34) 0.958 . . no C(39) C(40) 1.33(2) . . yes C(39) H(35) 0.970 . . no C(40) H(36) 0.924 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl(1) V(1) O(1) 97.3(3) . . . yes Cl(1) V(1) N(1) 87.6(3) . . . yes Cl(1) V(1) N(3) 88.5(3) . . . yes Cl(1) V(1) N(4) 174.6(3) . . . yes Cl(1) V(1) N(6) 95.0(3) . . . yes O(1) V(1) N(1) 175.1(4) . . . yes O(1) V(1) N(3) 98.8(4) . . . yes O(1) V(1) N(4) 88.1(4) . . . yes O(1) V(1) N(6) 94.0(4) . . . yes N(1) V(1) N(3) 80.4(4) . . . yes N(1) V(1) N(4) 87.1(4) . . . yes N(1) V(1) N(6) 86.4(4) . . . yes N(3) V(1) N(4) 91.3(4) . . . yes N(3) V(1) N(6) 166.2(4) . . . yes N(4) V(1) N(6) 84.0(4) . . . yes Cl(2) V(2) O(1) 96.0(3) . . . yes Cl(2) V(2) N(7) 85.3(3) . . . yes Cl(2) V(2) N(9) 90.7(3) . . . yes Cl(2) V(2) N(10) 170.0(3) . . . yes Cl(2) V(2) N(12) 93.2(4) . . . yes O(1) V(2) N(7) 178.1(4) . . . yes O(1) V(2) N(9) 96.8(4) . . . yes O(1) V(2) N(10) 93.5(4) . . . yes O(1) V(2) N(12) 93.7(4) . . . yes N(7) V(2) N(9) 81.7(4) . . . yes N(7) V(2) N(10) 85.4(4) . . . yes N(7) V(2) N(12) 87.7(4) . . . yes N(9) V(2) N(10) 91.5(4) . . . yes N(9) V(2) N(12) 168.4(5) . . . yes N(10) V(2) N(12) 82.8(5) . . . yes V(1) O(1) V(2) 169.0(5) . . . yes C(1) N(1) C(5) 115(1) . . . yes C(5) N(2) C(6) 125(1) . . . yes C(5) N(2) H(1) 113.6 . . . no C(6) N(2) H(1) 120.6 . . . no C(6) N(3) C(10) 117(1) . . . yes C(11) N(4) C(15) 118(1) . . . yes C(15) N(5) C(16) 126(1) . . . yes C(15) N(5) H(2) 116.7 . . . no C(16) N(5) H(2) 116.6 . . . no C(16) N(6) C(20) 118(1) . . . yes C(21) N(7) C(25) 117(1) . . . yes C(25) N(8) C(26) 126(1) . . . yes C(25) N(8) H(3) 116.1 . . . no C(26) N(8) H(3) 117.1 . . . no C(26) N(9) C(30) 116(1) . . . yes C(31) N(10) C(35) 118(1) . . . yes C(35) N(11) C(36) 126(1) . . . yes C(35) N(11) H(4) 116.6 . . . no C(36) N(11) H(4) 117.0 . . . no C(36) N(12) C(40) 119(1) . . . yes N(1) C(1) C(2) 125(1) . . . yes N(1) C(1) H(5) 114.5 . . . no C(2) C(1) H(5) 119.9 . . . no C(1) C(2) C(3) 119(1) . . . yes C(1) C(2) H(6) 123.1 . . . no C(3) C(2) H(6) 117.4 . . . no C(2) C(3) C(4) 119(1) . . . yes C(2) C(3) H(7) 126.5 . . . no C(4) C(3) H(7) 114.4 . . . no C(3) C(4) C(5) 117(1) . . . yes C(3) C(4) H(8) 123.3 . . . no C(5) C(4) H(8) 118.8 . . . no N(1) C(5) N(2) 119(1) . . . yes N(1) C(5) C(4) 121(1) . . . yes N(2) C(5) C(4) 118(1) . . . yes N(2) C(6) N(3) 120(1) . . . yes N(2) C(6) C(7) 116(1) . . . yes N(3) C(6) C(7) 123(1) . . . yes C(6) C(7) C(8) 120(1) . . . yes C(6) C(7) H(9) 122.8 . . . no C(8) C(7) H(9) 117.1 . . . no C(7) C(8) C(9) 117(1) . . . yes C(7) C(8) H(10) 124.2 . . . no C(9) C(8) H(10) 117.9 . . . no C(8) C(9) C(10) 118(1) . . . yes C(8) C(9) H(11) 119.7 . . . no C(10) C(9) H(11) 121.5 . . . no N(3) C(10) C(9) 122(1) . . . yes N(3) C(10) H(12) 119.8 . . . no C(9) C(10) H(12) 117.7 . . . no N(4) C(11) C(12) 121(1) . . . yes N(4) C(11) H(13) 119.1 . . . no C(12) C(11) H(13) 119.0 . . . no C(11) C(12) C(13) 120(1) . . . yes C(11) C(12) H(14) 118.0 . . . no C(13) C(12) H(14) 121.3 . . . no C(12) C(13) C(14) 118(1) . . . yes C(12) C(13) H(15) 124.2 . . . no C(14) C(13) H(15) 117.4 . . . no C(13) C(14) C(15) 121(1) . . . yes C(13) C(14) H(16) 122.5 . . . no C(15) C(14) H(16) 116.1 . . . no N(4) C(15) N(5) 122(1) . . . yes N(4) C(15) C(14) 119(1) . . . yes N(5) C(15) C(14) 118(1) . . . yes N(5) C(16) N(6) 121(1) . . . yes N(5) C(16) C(17) 114(1) . . . yes N(6) C(16) C(17) 123(1) . . . yes C(16) C(17) C(18) 115(1) . . . yes C(16) C(17) H(17) 125.1 . . . no C(18) C(17) H(17) 118.9 . . . no C(17) C(18) C(19) 121(1) . . . yes C(17) C(18) H(18) 119.5 . . . no C(19) C(18) H(18) 119.0 . . . no C(18) C(19) C(20) 117(1) . . . yes C(18) C(19) H(19) 121.4 . . . no C(20) C(19) H(19) 121.4 . . . no N(6) C(20) C(19) 122(1) . . . yes N(6) C(20) H(20) 120.2 . . . no C(19) C(20) H(20) 116.9 . . . no N(7) C(21) C(22) 124(1) . . . yes N(7) C(21) H(21) 117.4 . . . no C(22) C(21) H(21) 118.2 . . . no C(21) C(22) C(23) 117(1) . . . yes C(21) C(22) H(22) 121.8 . . . no C(23) C(22) H(22) 120.7 . . . no C(22) C(23) C(24) 122(1) . . . yes C(22) C(23) H(23) 118.0 . . . no C(24) C(23) H(23) 119.3 . . . no C(23) C(24) C(25) 116(1) . . . yes C(23) C(24) H(24) 122.7 . . . no C(25) C(24) H(24) 120.5 . . . no N(7) C(25) N(8) 119(1) . . . yes N(7) C(25) C(24) 121(1) . . . yes N(8) C(25) C(24) 118(1) . . . yes N(8) C(26) N(9) 117(1) . . . yes N(8) C(26) C(27) 117(1) . . . yes N(9) C(26) C(27) 124(1) . . . yes C(26) C(27) C(28) 118(1) . . . yes C(26) C(27) H(25) 121.7 . . . no C(28) C(27) H(25) 119.6 . . . no C(27) C(28) C(29) 120(1) . . . yes C(27) C(28) H(26) 122.8 . . . no C(29) C(28) H(26) 115.5 . . . no C(28) C(29) C(30) 119(1) . . . yes C(28) C(29) H(27) 125.0 . . . no C(30) C(29) H(27) 115.5 . . . no N(9) C(30) C(29) 120(1) . . . yes N(9) C(30) H(28) 118.4 . . . no C(29) C(30) H(28) 120.9 . . . no N(10) C(31) C(32) 123(1) . . . yes N(10) C(31) H(29) 119.0 . . . no C(32) C(31) H(29) 117.8 . . . no C(31) C(32) C(33) 119(1) . . . yes C(31) C(32) H(30) 120.0 . . . no C(33) C(32) H(30) 120.4 . . . no C(32) C(33) C(34) 117(1) . . . yes C(32) C(33) H(31) 123.6 . . . no C(34) C(33) H(31) 119.2 . . . no C(33) C(34) C(35) 121(1) . . . yes C(33) C(34) H(32) 119.1 . . . no C(35) C(34) H(32) 119.1 . . . no N(10) C(35) N(11) 121(1) . . . yes N(10) C(35) C(34) 119(1) . . . yes N(11) C(35) C(34) 119(1) . . . yes N(11) C(36) N(12) 121(1) . . . yes N(11) C(36) C(37) 117(1) . . . yes N(12) C(36) C(37) 121(1) . . . yes C(36) C(37) C(38) 118(2) . . . yes C(36) C(37) H(33) 119.6 . . . no C(38) C(37) H(33) 122.1 . . . no C(37) C(38) C(39) 120(1) . . . yes C(37) C(38) H(34) 118.0 . . . no C(39) C(38) H(34) 121.6 . . . no C(38) C(39) C(40) 117(1) . . . yes C(38) C(39) H(35) 119.4 . . . no C(40) C(39) H(35) 122.5 . . . no N(12) C(40) C(39) 122(1) . . . yes N(12) C(40) H(36) 118.1 . . . no C(39) C(40) H(36) 119.6 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #=END #------------------------------------------------------------------------------ data_V2(M-O)(NCS)(DPYA) _database_code_CSD 167776 _audit_creation_date 'Fri Nov 30 16:31:40 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C42 H43 N13 O3 S4 V2 ' _chemical_formula_moiety '?' _chemical_formula_weight 1008.01 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 16.980(2) _cell_length_b 17.057(4) _cell_length_c 18.199(2) _cell_angle_alpha 90 _cell_angle_beta 103.592(9) _cell_angle_gamma 90 _cell_volume 5123(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.1 _cell_measurement_theta_max 16.0 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'BROWN' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.294 _exptl_absorpt_correction_T_max 0.891 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 12725 _diffrn_reflns_av_R_equivalents 0.016 _diffrn_reflns_theta_max 27.56 _diffrn_measured_fraction_theta_max 0.9992 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.9992 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 19.89 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 11842 _reflns_number_gt 4596 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0800 _refine_ls_wR_factor_ref 0.1007 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4596 _refine_ls_number_parameters 532 _refine_ls_goodness_of_fit_ref 3.608 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00008|Fo|^2^]' _refine_ls_shift/su_max 0.0012 _refine_diff_density_max 1.25 _refine_diff_density_min -0.39 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 V(1) V 0.50338(10) 0.33991(10) 0.15832(9) 0.0469(5) Uani 1.00 d . . . V(2) V 0.37062(10) 0.18162(10) 0.09176(9) 0.0527(5) Uani 1.00 d . . . S(1) S 0.7339(2) 0.2620(3) 0.0677(3) 0.125(2) Uani 1.00 d . . . S(2) S 0.3331(2) 0.2076(2) -0.1790(2) 0.084(1) Uani 1.00 d . . . S(3) S 0.1394(2) 0.3499(2) 0.0755(2) 0.112(1) Uani 1.00 d . . . S(4) S 0.2077(2) -0.0449(2) -0.0009(2) 0.119(2) Uani 1.00 d . . . O(1) O 0.4357(3) 0.2629(3) 0.1198(3) 0.047(2) Uani 1.00 d . . . O(2) O 0.0799(6) 0.1884(6) 0.3389(5) 0.066(3) Uiso 0.70 d P . . O(3) O 0.4476 0.0812 0.6994 0.096(4) Uiso 0.70 d P . . O(4) O 0.0171(8) 0.1351(8) 0.9987(8) 0.087(4) Uiso 0.60 d P . . N(1) N 0.4524(4) 0.4194(5) 0.0706(4) 0.050(3) Uani 1.00 d . . . N(2) N 0.4766(5) 0.5324(4) 0.1463(5) 0.059(3) Uani 1.00 d . . . N(3) N 0.5781(5) 0.4412(5) 0.2025(4) 0.051(3) Uani 1.00 d . . . N(4) N 0.4249(5) 0.3818(4) 0.2252(4) 0.051(3) Uani 1.00 d . . . N(5) N 0.5183(5) 0.3596(5) 0.3425(4) 0.066(3) Uani 1.00 d . . . N(6) N 0.5599(5) 0.2739(5) 0.2556(4) 0.054(3) Uani 1.00 d . . . N(7) N 0.5934(5) 0.3097(5) 0.1066(4) 0.057(3) Uani 1.00 d . . . N(8) N 0.3841(5) 0.1461(5) 0.2065(5) 0.062(3) Uani 1.00 d . . . N(9) N 0.4502(6) 0.0264(5) 0.1944(6) 0.076(3) Uani 1.00 d . . . N(10) N 0.4723(5) 0.1076(5) 0.0964(4) 0.051(3) Uani 1.00 d . . . N(11) N 0.3555(5) 0.1984(5) -0.0225(5) 0.064(3) Uani 1.00 d . . . N(12) N 0.2673(5) 0.2441(6) 0.0904(5) 0.074(3) Uani 1.00 d . . . N(13) N 0.3010(5) 0.0807(5) 0.0660(5) 0.071(3) Uani 1.00 d . . . C(1) C 0.4159(6) 0.3868(6) 0.0036(5) 0.057(3) Uani 1.00 d . . . C(2) C 0.3658(7) 0.4267(7) -0.0531(6) 0.069(4) Uani 1.00 d . . . C(3) C 0.3522(7) 0.5046(9) -0.0415(6) 0.079(4) Uani 1.00 d . . . C(4) C 0.3895(6) 0.5409(6) 0.0243(7) 0.072(4) Uani 1.00 d . . . C(5) C 0.4397(6) 0.4951(6) 0.0793(6) 0.054(3) Uani 1.00 d . . . C(6) C 0.5519(6) 0.5141(6) 0.1962(5) 0.055(3) Uani 1.00 d . . . C(7) C 0.5975(8) 0.5770(6) 0.2374(6) 0.074(4) Uani 1.00 d . . . C(8) C 0.6718(8) 0.5614(8) 0.2820(7) 0.082(5) Uani 1.00 d . . . C(9) C 0.7002(7) 0.4870(8) 0.2851(7) 0.081(4) Uani 1.00 d . . . C(10) C 0.6545(6) 0.4288(7) 0.2456(6) 0.067(4) Uani 1.00 d . . . C(11) C 0.3500(6) 0.4070(6) 0.1903(6) 0.058(3) Uani 1.00 d . . . C(12) C 0.2974(7) 0.4412(7) 0.2248(7) 0.072(4) Uani 1.00 d . . . C(13) C 0.3180(8) 0.4506(8) 0.3011(8) 0.088(5) Uani 1.00 d . . . C(14) C 0.3928(8) 0.4243(7) 0.3397(6) 0.082(4) Uani 1.00 d . . . C(15) C 0.4446(7) 0.3885(6) 0.3013(6) 0.061(4) Uani 1.00 d . . . C(16) C 0.5637(6) 0.2956(6) 0.3279(6) 0.061(4) Uani 1.00 d . . . C(17) C 0.6147(7) 0.2591(8) 0.3891(6) 0.086(5) Uani 1.00 d . . . C(18) C 0.6577(8) 0.1951(8) 0.3761(7) 0.093(5) Uani 1.00 d . . . C(19) C 0.6501(7) 0.1699(7) 0.3044(7) 0.075(4) Uani 1.00 d . . . C(20) C 0.6014(6) 0.2091(6) 0.2469(5) 0.058(3) Uani 1.00 d . . . C(21) C 0.6522(7) 0.2906(6) 0.0902(6) 0.061(4) Uani 1.00 d . . . C(22) C 0.3575(7) 0.1950(7) 0.2517(7) 0.077(4) Uani 1.00 d . . . C(23) C 0.3570(10) 0.179(1) 0.3249(9) 0.114(7) Uani 1.00 d . . . C(24) C 0.383(1) 0.106(1) 0.3516(9) 0.134(8) Uani 1.00 d . . . C(25) C 0.4119(9) 0.0537(9) 0.3073(8) 0.112(6) Uani 1.00 d . . . C(26) C 0.4135(7) 0.0770(8) 0.2345(7) 0.071(4) Uani 1.00 d . . . C(27) C 0.4900(7) 0.0430(6) 0.1384(6) 0.060(4) Uani 1.00 d . . . C(28) C 0.5513(7) -0.0085(7) 0.1304(6) 0.070(4) Uani 1.00 d . . . C(29) C 0.5959(7) 0.0085(7) 0.0799(7) 0.074(4) Uani 1.00 d . . . C(30) C 0.5829(6) 0.0773(7) 0.0389(6) 0.064(4) Uani 1.00 d . . . C(31) C 0.5205(6) 0.1241(6) 0.0484(6) 0.059(3) Uani 1.00 d . . . C(32) C 0.3458(5) 0.2015(6) -0.0870(6) 0.051(3) Uani 1.00 d . . . C(33) C 0.2152(7) 0.2879(7) 0.0848(6) 0.069(4) Uani 1.00 d . . . C(34) C 0.2627(6) 0.0287(7) 0.0393(6) 0.064(4) Uani 1.00 d . . . C(35) C 0.066(1) 0.260(1) 0.3700(9) 0.083(5) Uiso 0.70 d P . . C(36) C 0.111(1) 0.318(1) 0.344(1) 0.100(6) Uiso 0.70 d P . . C(37) C 0.166(1) 0.282(1) 0.316(1) 0.113(7) Uiso 0.70 d P . . C(38) C 0.153(1) 0.195(1) 0.319(1) 0.108(6) Uiso 0.70 d P . . C(39) C 0.3845 0.0418 0.6539 0.122(7) Uiso 0.70 d P . . C(40) C 0.3783 0.0463 0.5756 0.130(8) Uiso 0.70 d P . . C(41) C 0.4187 0.1121 0.5756 0.160(10) Uiso 0.70 d P . . C(42) C 0.4492 0.1322 0.6553 0.152(9) Uiso 0.70 d P . . C(43) C -0.033(1) 0.188(1) 1.022(1) 0.070(5) Uiso 0.60 d P . . C(44) C -0.033(1) 0.175(1) 1.099(1) 0.111(8) Uiso 0.60 d P . . C(45) C 0.017(2) 0.110(2) 1.110(2) 0.130(9) Uiso 0.60 d P . . C(46) C 0.058(1) 0.105(1) 1.055(1) 0.090(6) Uiso 0.60 d P . . H(1) H 0.4259 0.3330 -0.0042 0.0686 Uiso 1.00 calc . . . H(2) H 0.3409 0.4015 -0.0993 0.0823 Uiso 1.00 calc . . . H(3) H 0.3164 0.5337 -0.0799 0.0947 Uiso 1.00 calc . . . H(4) H 0.3816 0.5951 0.0322 0.0861 Uiso 1.00 calc . . . H(5) H 0.4479 0.5755 0.1604 0.0703 Uiso 1.00 calc . . . H(6) H 0.5762 0.6288 0.2336 0.0887 Uiso 1.00 calc . . . H(7) H 0.7033 0.6019 0.3106 0.0979 Uiso 1.00 calc . . . H(8) H 0.7526 0.4755 0.3151 0.0966 Uiso 1.00 calc . . . H(9) H 0.6766 0.3775 0.2479 0.0807 Uiso 1.00 calc . . . H(10) H 0.3332 0.3998 0.1371 0.0700 Uiso 1.00 calc . . . H(11) H 0.2462 0.4588 0.1962 0.0869 Uiso 1.00 calc . . . H(12) H 0.2818 0.4746 0.3269 0.1054 Uiso 1.00 calc . . . H(13) H 0.4091 0.4306 0.3930 0.0988 Uiso 1.00 calc . . . H(14) H 0.5413 0.3876 0.3875 0.0797 Uiso 1.00 calc . . . H(15) H 0.6195 0.2782 0.4390 0.1034 Uiso 1.00 calc . . . H(16) H 0.6926 0.1686 0.4170 0.1114 Uiso 1.00 calc . . . H(17) H 0.6789 0.1249 0.2946 0.0899 Uiso 1.00 calc . . . H(18) H 0.5962 0.1895 0.1971 0.0696 Uiso 1.00 calc . . . H(19) H 0.3375 0.2445 0.2318 0.0924 Uiso 1.00 calc . . . H(20) H 0.3394 0.2165 0.3560 0.1366 Uiso 1.00 calc . . . H(21) H 0.3809 0.0915 0.4016 0.1603 Uiso 1.00 calc . . . H(22) H 0.4302 0.0032 0.3257 0.1343 Uiso 1.00 calc . . . H(23) H 0.4480 -0.0274 0.2070 0.0911 Uiso 1.00 calc . . . H(24) H 0.5616 -0.0548 0.1601 0.0836 Uiso 1.00 calc . . . H(25) H 0.6364 -0.0271 0.0725 0.0891 Uiso 1.00 calc . . . H(26) H 0.6159 0.0917 0.0056 0.0764 Uiso 1.00 calc . . . H(27) H 0.5102 0.1710 0.0196 0.0710 Uiso 1.00 calc . . . H(28) H 0.3897 -0.0120 0.6678 0.1469 Uiso 0.70 calc P . . H(29) H 0.3357 0.0621 0.6633 0.1469 Uiso 0.70 calc P . . H(30) H 0.4037 0.0033 0.5573 0.1565 Uiso 0.70 calc P . . H(31) H 0.3238 0.0504 0.5475 0.1565 Uiso 0.70 calc P . . H(32) H 0.3840 0.1522 0.5501 0.1926 Uiso 0.70 calc P . . H(33) H 0.4623 0.1048 0.5518 0.1926 Uiso 0.70 calc P . . H(34) H 0.4176 0.1745 0.6665 0.1821 Uiso 0.70 calc P . . H(35) H 0.5039 0.1486 0.6620 0.1821 Uiso 0.70 calc P . . H(36) H 0.0829 0.2568 0.4236 0.0995 Uiso 0.70 calc P . . H(37) H 0.0100 0.2719 0.3556 0.0995 Uiso 0.70 calc P . . H(38) H 0.0758 0.3483 0.3053 0.1200 Uiso 0.70 calc P . . H(39) H 0.1359 0.3516 0.3839 0.1200 Uiso 0.70 calc P . . H(40) H 0.1607 0.2979 0.2645 0.1351 Uiso 0.70 calc P . . H(41) H 0.2184 0.2955 0.3444 0.1351 Uiso 0.70 calc P . . H(42) H 0.1501 0.1715 0.2713 0.1292 Uiso 0.70 calc P . . H(43) H 0.1949 0.1715 0.3560 0.1292 Uiso 0.70 calc P . . H(44) H -0.0142 0.2400 1.0167 0.0843 Uiso 0.60 calc P . . H(45) H -0.0865 0.1827 0.9922 0.0843 Uiso 0.60 calc P . . H(46) H -0.0853 0.1637 1.1059 0.1334 Uiso 0.60 calc P . . H(47) H -0.0102 0.2177 1.1305 0.1334 Uiso 0.60 calc P . . H(48) H -0.0149 0.0641 1.1085 0.1560 Uiso 0.60 calc P . . H(49) H 0.0546 0.1139 1.1572 0.1560 Uiso 0.60 calc P . . H(50) H 0.0681 0.0515 1.0451 0.1075 Uiso 0.60 calc P . . H(51) H 0.1086 0.1318 1.0700 0.1075 Uiso 0.60 calc 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V(1) 0.0459(10) 0.0491(10) 0.0433(9) 0.0023(8) 0.0053(7) -0.0029(8) V(2) 0.049(1) 0.056(1) 0.052(1) -0.0026(9) 0.0092(8) -0.0083(9) S(1) 0.078(3) 0.142(4) 0.168(4) 0.022(3) 0.058(3) -0.017(3) S(2) 0.091(2) 0.100(3) 0.057(2) 0.001(2) 0.006(2) 0.003(2) S(3) 0.073(2) 0.135(3) 0.116(3) 0.032(2) -0.004(2) -0.042(3) S(4) 0.118(3) 0.133(3) 0.119(3) -0.075(3) 0.055(3) -0.057(3) O(1) 0.049(4) 0.047(4) 0.045(4) -0.001(3) 0.013(3) -0.003(3) N(1) 0.049(5) 0.049(5) 0.047(5) 0.000(4) 0.006(4) 0.004(4) N(2) 0.053(5) 0.051(5) 0.073(6) 0.014(4) 0.016(5) -0.003(5) N(3) 0.050(5) 0.049(5) 0.050(5) 0.002(4) 0.001(4) -0.002(4) N(4) 0.049(5) 0.051(5) 0.050(5) 0.001(4) 0.008(4) -0.003(4) N(5) 0.072(6) 0.075(7) 0.046(5) 0.009(5) 0.001(5) -0.011(5) N(6) 0.054(5) 0.052(5) 0.051(5) 0.004(4) 0.003(4) -0.004(4) N(7) 0.058(6) 0.057(5) 0.059(5) 0.005(5) 0.016(5) -0.001(4) N(8) 0.066(6) 0.066(6) 0.060(6) -0.017(5) 0.023(5) -0.008(5) N(9) 0.093(7) 0.060(6) 0.077(7) -0.003(6) 0.025(6) 0.015(5) N(10) 0.055(5) 0.046(5) 0.050(5) -0.006(4) 0.009(4) -0.007(4) N(11) 0.065(6) 0.069(6) 0.050(5) -0.003(5) 0.000(5) -0.005(5) N(12) 0.051(6) 0.082(7) 0.087(7) 0.006(5) 0.015(5) -0.025(6) N(13) 0.065(6) 0.066(6) 0.078(7) -0.018(5) 0.009(5) -0.017(5) C(1) 0.059(7) 0.068(7) 0.042(6) 0.001(6) 0.006(5) -0.001(6) C(2) 0.068(8) 0.076(8) 0.058(7) -0.009(7) 0.008(6) 0.007(7) C(3) 0.054(7) 0.11(1) 0.059(8) 0.009(8) -0.008(6) 0.029(8) C(4) 0.062(7) 0.070(8) 0.074(8) 0.009(6) -0.003(6) 0.024(7) C(5) 0.045(6) 0.062(7) 0.054(7) -0.003(6) 0.008(5) 0.004(6) C(6) 0.062(7) 0.059(7) 0.044(6) -0.010(6) 0.011(5) -0.005(5) C(7) 0.092(9) 0.054(7) 0.075(8) -0.009(7) 0.017(7) -0.015(6) C(8) 0.066(8) 0.10(1) 0.074(8) -0.021(8) 0.000(7) -0.026(8) C(9) 0.066(8) 0.085(9) 0.079(9) -0.016(8) -0.005(7) -0.009(8) C(10) 0.051(7) 0.079(8) 0.065(7) 0.001(6) 0.000(6) -0.003(6) C(11) 0.052(7) 0.065(7) 0.058(7) 0.002(6) 0.013(6) -0.010(6) C(12) 0.059(7) 0.081(9) 0.075(9) 0.016(6) 0.012(6) -0.002(7) C(13) 0.086(10) 0.11(1) 0.080(10) 0.030(8) 0.036(8) -0.012(8) C(14) 0.11(1) 0.083(9) 0.060(8) 0.013(8) 0.026(8) -0.023(7) C(15) 0.073(8) 0.053(7) 0.054(7) 0.002(6) 0.012(6) -0.005(6) C(16) 0.061(7) 0.064(7) 0.056(7) 0.003(6) 0.011(6) -0.005(6) C(17) 0.087(9) 0.12(1) 0.040(7) 0.023(9) 0.001(6) 0.019(7) C(18) 0.092(10) 0.11(1) 0.071(9) 0.045(9) 0.009(8) 0.028(8) C(19) 0.072(8) 0.081(9) 0.068(8) 0.019(7) 0.009(6) 0.021(7) C(20) 0.062(7) 0.060(7) 0.051(6) 0.016(6) 0.014(5) -0.008(5) C(21) 0.062(7) 0.057(7) 0.066(7) 0.002(6) 0.016(6) -0.003(6) C(22) 0.082(9) 0.089(9) 0.067(8) -0.015(7) 0.030(7) -0.004(7) C(23) 0.12(1) 0.15(2) 0.08(1) -0.01(1) 0.043(10) -0.01(1) C(24) 0.12(1) 0.22(2) 0.08(1) 0.00(1) 0.050(10) 0.02(1) C(25) 0.12(1) 0.14(1) 0.08(1) 0.02(1) 0.040(9) 0.041(10) C(26) 0.069(8) 0.085(9) 0.062(8) -0.013(7) 0.019(6) 0.015(7) C(27) 0.061(7) 0.049(7) 0.065(8) -0.007(6) 0.005(6) -0.001(6) C(28) 0.079(8) 0.066(8) 0.060(7) 0.013(7) 0.008(7) 0.009(6) C(29) 0.056(7) 0.085(9) 0.071(8) 0.013(7) -0.007(6) -0.021(7) C(30) 0.060(7) 0.070(8) 0.061(7) -0.003(6) 0.014(6) -0.004(6) C(31) 0.059(7) 0.061(7) 0.052(6) 0.004(6) 0.002(6) -0.007(6) C(32) 0.038(6) 0.048(6) 0.068(7) -0.002(5) 0.014(5) -0.007(6) C(33) 0.057(7) 0.092(10) 0.057(7) -0.012(7) 0.010(6) -0.020(7) C(34) 0.061(8) 0.081(9) 0.055(7) -0.006(7) 0.023(6) -0.005(6) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V(1) O(1) 1.778(6) . . yes V(1) N(1) 2.118(8) . . yes V(1) N(3) 2.182(8) . . yes V(1) N(4) 2.128(8) . . yes V(1) N(6) 2.128(8) . . yes V(1) N(7) 2.041(9) . . yes V(2) O(1) 1.771(6) . . yes V(2) N(8) 2.135(9) . . yes V(2) N(10) 2.125(8) . . yes V(2) N(11) 2.055(9) . . yes V(2) N(12) 2.048(9) . . yes V(2) N(13) 2.079(9) . . yes S(1) C(21) 1.61(1) . . yes S(2) C(32) 1.64(1) . . yes S(3) C(33) 1.64(1) . . yes S(4) C(34) 1.63(1) . . yes O(2) C(35) 1.38(2) . . yes O(2) C(38) 1.37(2) . . yes O(3) C(39) 1.366 . . yes O(3) C(42) 1.189 . . yes O(4) C(43) 1.38(2) . . yes O(4) C(46) 1.21(2) . . yes N(1) C(1) 1.35(1) . . yes N(1) C(5) 1.33(1) . . yes N(2) C(5) 1.39(1) . . yes N(2) C(6) 1.42(1) . . yes N(2) H(5) 0.950 . . no N(3) C(6) 1.32(1) . . yes N(3) C(10) 1.37(1) . . yes N(4) C(11) 1.35(1) . . yes N(4) C(15) 1.35(1) . . yes N(5) C(15) 1.39(1) . . yes N(5) C(16) 1.40(1) . . yes N(5) H(14) 0.950 . . no N(6) C(16) 1.35(1) . . yes N(6) C(20) 1.34(1) . . yes N(7) C(21) 1.15(1) . . yes N(8) C(22) 1.32(1) . . yes N(8) C(26) 1.33(1) . . yes N(9) C(26) 1.37(1) . . yes N(9) C(27) 1.38(1) . . yes N(9) H(23) 0.950 . . no N(10) C(27) 1.33(1) . . yes N(10) C(31) 1.36(1) . . yes N(11) C(32) 1.15(1) . . yes N(12) C(33) 1.14(1) . . yes N(13) C(34) 1.14(1) . . yes C(1) C(2) 1.36(1) . . yes C(1) H(1) 0.950 . . no C(2) C(3) 1.37(2) . . yes C(2) H(2) 0.950 . . no C(3) C(4) 1.36(1) . . yes C(3) H(3) 0.950 . . no C(4) C(5) 1.39(1) . . yes C(4) H(4) 0.950 . . no C(6) C(7) 1.43(1) . . yes C(7) C(8) 1.36(1) . . yes C(7) H(6) 0.950 . . no C(8) C(9) 1.35(2) . . yes C(8) H(7) 0.950 . . no C(9) C(10) 1.36(1) . . yes C(9) H(8) 0.950 . . no C(10) H(9) 0.950 . . no C(11) C(12) 1.34(1) . . yes C(11) H(10) 0.950 . . no C(12) C(13) 1.36(1) . . yes C(12) H(11) 0.950 . . no C(13) C(14) 1.38(2) . . yes C(13) H(12) 0.950 . . no C(14) C(15) 1.39(1) . . yes C(14) H(13) 0.950 . . no C(16) C(17) 1.39(1) . . yes C(17) C(18) 1.37(2) . . yes C(17) H(15) 0.950 . . no C(18) C(19) 1.35(2) . . yes C(18) H(16) 0.950 . . no C(19) C(20) 1.35(1) . . yes C(19) H(17) 0.950 . . no C(20) H(18) 0.950 . . no C(22) C(23) 1.36(2) . . yes C(22) H(19) 0.950 . . no C(23) C(24) 1.37(2) . . yes C(23) H(20) 0.950 . . no C(24) C(25) 1.37(2) . . yes C(24) H(21) 0.950 . . no C(25) C(26) 1.39(2) . . yes C(25) H(22) 0.950 . . no C(27) C(28) 1.40(1) . . yes C(28) C(29) 1.35(1) . . yes C(28) H(24) 0.950 . . no C(29) C(30) 1.38(1) . . yes C(29) H(25) 0.950 . . no C(30) C(31) 1.37(1) . . yes C(30) H(26) 0.950 . . no C(31) H(27) 0.950 . . no C(35) C(36) 1.40(2) . . yes C(35) H(36) 0.950 . . no C(35) H(37) 0.950 . . no C(36) C(37) 1.32(2) . . yes C(36) H(38) 0.950 . . no C(36) H(39) 0.950 . . no C(37) C(38) 1.51(2) . . yes C(37) H(40) 0.950 . . no C(37) H(41) 0.950 . . no C(38) H(42) 0.950 . . no C(38) H(43) 0.950 . . no C(39) C(40) 1.406 . . yes C(39) H(28) 0.950 . . no C(39) H(29) 0.950 . . no C(40) C(41) 1.314 . . yes C(40) H(30) 0.950 . . no C(40) H(31) 0.950 . . no C(41) C(42) 1.461 . . yes C(41) H(32) 0.950 . . no C(41) H(33) 0.950 . . no C(42) H(34) 0.950 . . no C(42) H(35) 0.950 . . no C(43) C(44) 1.41 . . yes C(43) H(44) 0.950 . . no C(43) H(45) 0.950 . . no C(44) C(45) 1.38(3) . . yes C(44) H(46) 0.950 . . no C(44) H(47) 0.950 . . no C(45) C(46) 1.35(3) . . yes C(45) H(48) 0.950 . . no C(45) H(49) 0.950 . . no C(46) H(50) 0.950 . . no C(46) H(51) 0.950 . . no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O(1) V(1) N(1) 93.7(3) . . . yes O(1) V(1) N(3) 175.3(3) . . . yes O(1) V(1) N(4) 92.3(3) . . . yes O(1) V(1) N(6) 93.4(3) . . . yes O(1) V(1) N(7) 96.7(3) . . . yes N(1) V(1) N(3) 82.6(3) . . . yes N(1) V(1) N(4) 90.9(3) . . . yes N(1) V(1) N(6) 172.2(3) . . . yes N(1) V(1) N(7) 91.9(3) . . . yes N(3) V(1) N(4) 84.9(3) . . . yes N(3) V(1) N(6) 90.2(3) . . . yes N(3) V(1) N(7) 86.4(3) . . . yes N(4) V(1) N(6) 85.5(3) . . . yes N(4) V(1) N(7) 170.4(3) . . . yes N(6) V(1) N(7) 90.6(3) . . . yes O(1) V(2) N(8) 91.4(3) . . . yes O(1) V(2) N(10) 90.4(3) . . . yes O(1) V(2) N(11) 96.0(3) . . . yes O(1) V(2) N(12) 94.1(3) . . . yes O(1) V(2) N(13) 175.1(3) . . . yes N(8) V(2) N(10) 83.9(3) . . . yes N(8) V(2) N(11) 171.5(4) . . . yes N(8) V(2) N(12) 93.1(4) . . . yes N(8) V(2) N(13) 84.8(3) . . . yes N(10) V(2) N(11) 91.7(3) . . . yes N(10) V(2) N(12) 174.6(4) . . . yes N(10) V(2) N(13) 86.0(3) . . . yes N(11) V(2) N(12) 90.7(4) . . . yes N(11) V(2) N(13) 87.6(3) . . . yes N(12) V(2) N(13) 89.3(4) . . . yes V(1) O(1) V(2) 173.6(4) . . . yes C(35) O(2) C(38) 106(1) . . . yes C(39) O(3) C(42) 95.138 . . . yes C(43) O(4) C(46) 107(1) . . . yes C(1) N(1) C(5) 117.1(8) . . . yes C(5) N(2) C(6) 127.9(8) . . . yes C(5) N(2) H(5) 116.1 . . . no C(6) N(2) H(5) 116.0 . . . no C(6) N(3) C(10) 116.9(9) . . . yes C(11) N(4) C(15) 115.7(9) . . . yes C(15) N(5) C(16) 130.0(9) . . . yes C(15) N(5) H(14) 115.0 . . . no C(16) N(5) H(14) 115.0 . . . no C(16) N(6) C(20) 115.8(8) . . . yes C(22) N(8) C(26) 118(1) . . . yes C(26) N(9) C(27) 128.9(10) . . . yes C(26) N(9) H(23) 115.5 . . . no C(27) N(9) H(23) 115.5 . . . no C(27) N(10) C(31) 116.8(9) . . . yes N(1) C(1) C(2) 123.6(10) . . . yes N(1) C(1) H(1) 118.2 . . . no C(2) C(1) H(1) 118.2 . . . no C(1) C(2) C(3) 117(1) . . . yes C(1) C(2) H(2) 121.1 . . . no C(3) C(2) H(2) 121.1 . . . no C(2) C(3) C(4) 120(1) . . . yes C(2) C(3) H(3) 119.5 . . . no C(4) C(3) H(3) 119.5 . . . no C(3) C(4) C(5) 117(1) . . . yes C(3) C(4) H(4) 121.4 . . . no C(5) C(4) H(4) 121.4 . . . no N(1) C(5) N(2) 120.0(9) . . . yes N(1) C(5) C(4) 123.4(10) . . . yes N(2) C(5) C(4) 116.6(10) . . . yes N(2) C(6) N(3) 120.0(9) . . . yes N(2) C(6) C(7) 117.8(10) . . . yes N(3) C(6) C(7) 122.3(10) . . . yes C(6) C(7) C(8) 118(1) . . . yes C(6) C(7) H(6) 120.7 . . . no C(8) C(7) H(6) 120.7 . . . no C(7) C(8) C(9) 118(1) . . . yes C(7) C(8) H(7) 120.7 . . . no C(9) C(8) H(7) 120.7 . . . no C(8) C(9) C(10) 120(1) . . . yes C(8) C(9) H(8) 119.6 . . . no C(10) C(9) H(8) 119.6 . . . no N(3) C(10) C(9) 122(1) . . . yes N(3) C(10) H(9) 118.7 . . . no C(9) C(10) H(9) 118.7 . . . no N(4) C(11) C(12) 125.1(10) . . . yes N(4) C(11) H(10) 117.4 . . . no C(12) C(11) H(10) 117.4 . . . no C(11) C(12) C(13) 119(1) . . . yes C(11) C(12) H(11) 120.3 . . . no C(13) C(12) H(11) 120.3 . . . no C(12) C(13) C(14) 118(1) . . . yes C(12) C(13) H(12) 121.0 . . . no C(14) C(13) H(12) 121.0 . . . no C(13) C(14) C(15) 120(1) . . . yes C(13) C(14) H(13) 119.9 . . . no C(15) C(14) H(13) 119.8 . . . no N(4) C(15) N(5) 119.8(9) . . . yes N(4) C(15) C(14) 121(1) . . . yes N(5) C(15) C(14) 118(1) . . . yes N(5) C(16) N(6) 119.7(9) . . . yes N(5) C(16) C(17) 117(1) . . . yes N(6) C(16) C(17) 122(1) . . . yes C(16) C(17) C(18) 118(1) . . . yes C(16) C(17) H(15) 120.7 . . . no C(18) C(17) H(15) 120.7 . . . no C(17) C(18) C(19) 119(1) . . . yes C(17) C(18) H(16) 120.4 . . . no C(19) C(18) H(16) 120.4 . . . no C(18) C(19) C(20) 119(1) . . . yes C(18) C(19) H(17) 120.2 . . . no C(20) C(19) H(17) 120.2 . . . no N(6) C(20) C(19) 124.1(10) . . . yes N(6) C(20) H(18) 118.0 . . . no C(19) C(20) H(18) 118.0 . . . no S(1) C(21) N(7) 178(1) . . . yes N(8) C(22) C(23) 124(1) . . . yes N(8) C(22) H(19) 118.0 . . . no C(23) C(22) H(19) 118.0 . . . no C(22) C(23) C(24) 117(1) . . . yes C(22) C(23) H(20) 121.4 . . . no C(24) C(23) H(20) 121.4 . . . no C(23) C(24) C(25) 120(1) . . . yes C(23) C(24) H(21) 119.6 . . . no C(25) C(24) H(21) 119.6 . . . no C(24) C(25) C(26) 117(1) . . . yes C(24) C(25) H(22) 121.1 . . . no C(26) C(25) H(22) 121.1 . . . no N(8) C(26) N(9) 121(1) . . . yes N(8) C(26) C(25) 121(1) . . . yes N(9) C(26) C(25) 116(1) . . . yes N(9) C(27) N(10) 120(1) . . . yes N(9) C(27) C(28) 117(1) . . . yes N(10) C(27) C(28) 122(1) . . . yes C(27) C(28) C(29) 119(1) . . . yes C(27) C(28) H(24) 120.5 . . . no C(29) C(28) H(24) 120.5 . . . no C(28) C(29) C(30) 120(1) . . . yes C(28) C(29) H(25) 119.8 . . . no C(30) C(29) H(25) 119.8 . . . no C(29) C(30) C(31) 117(1) . . . yes C(29) C(30) H(26) 121.4 . . . no C(31) C(30) H(26) 121.4 . . . no N(10) C(31) C(30) 124.1(10) . . . yes N(10) C(31) H(27) 118.0 . . . no C(30) C(31) H(27) 118.0 . . . no S(2) C(32) N(11) 178.8(10) . . . yes S(3) C(33) N(12) 178(1) . . . yes S(4) C(34) N(13) 178(1) . . . yes O(2) C(35) C(36) 109(1) . . . yes O(2) C(35) H(36) 109.5 . . . no O(2) C(35) H(37) 109.5 . . . no C(36) C(35) H(36) 109.6 . . . no C(36) C(35) H(37) 109.6 . . . no H(36) C(35) H(37) 109.5 . . . no C(35) C(36) C(37) 106(1) . . . yes C(35) C(36) H(38) 110.1 . . . no C(35) C(36) H(39) 110.1 . . . no C(37) C(36) H(38) 110.1 . . . no C(37) C(36) H(39) 110.1 . . . no H(38) C(36) H(39) 109.5 . . . no C(36) C(37) C(38) 108(1) . . . yes C(36) C(37) H(40) 109.8 . . . no C(36) C(37) H(41) 109.8 . . . no C(38) C(37) H(40) 109.7 . . . no C(38) C(37) H(41) 109.7 . . . no H(40) C(37) H(41) 109.4 . . . no O(2) C(38) C(37) 104(1) . . . yes O(2) C(38) H(42) 110.8 . . . no O(2) C(38) H(43) 110.8 . . . no C(37) C(38) H(42) 110.8 . . . no C(37) C(38) H(43) 110.8 . . . no H(42) C(38) H(43) 109.5 . . . no O(3) C(39) C(40) 116.680(2) . . . yes O(3) C(39) H(28) 107.6 . . . no O(3) C(39) H(29) 107.6 . . . no C(40) C(39) H(28) 107.6 . . . no C(40) C(39) H(29) 107.6 . . . no H(28) C(39) H(29) 109.5 . . . no C(39) C(40) C(41) 97.567 . . . yes C(39) C(40) H(30) 112.4 . . . no C(39) C(40) H(31) 112.4 . . . no C(41) C(40) H(30) 112.4 . . . no C(41) C(40) H(31) 112.4 . . . no H(30) C(40) H(31) 109.5 . . . no C(40) C(41) C(42) 105.33 . . . yes C(40) C(41) H(32) 110.5 . . . no C(40) C(41) H(33) 110.5 . . . no C(42) C(41) H(32) 110.5 . . . no C(42) C(41) H(33) 110.5 . . . no H(32) C(41) H(33) 109.5 . . . no O(3) C(42) C(41) 116.038 . . . yes O(3) C(42) H(34) 107.8 . . . no O(3) C(42) H(35) 107.8 . . . no C(41) C(42) H(34) 107.8 . . . no C(41) C(42) H(35) 107.8 . . . no H(34) C(42) H(35) 109.5 . . . no O(4) C(43) C(44) 110(1) . . . yes O(4) C(43) H(44) 109.3 . . . no O(4) C(43) H(45) 109.3 . . . no C(44) C(43) H(44) 109.3 . . . no C(44) C(43) H(45) 109.3 . . . no H(44) C(43) H(45) 109.5 . . . no C(43) C(44) C(45) 97(2) . . . yes C(43) C(44) H(46) 112.4 . . . no C(43) C(44) H(47) 112.4 . . . no C(45) C(44) H(46) 112.5 . . . no C(45) C(44) H(47) 112.5 . . . no H(46) C(44) H(47) 109.5 . . . no C(44) C(45) C(46) 110(2) . . . yes C(44) C(45) H(48) 109.1 . . . no C(44) C(45) H(49) 109.1 . . . no C(46) C(45) H(48) 109.2 . . . no C(46) C(45) H(49) 109.1 . . . no H(48) C(45) H(49) 109.5 . . . no O(4) C(46) C(45) 107(2) . . . yes O(4) C(46) H(50) 110.0 . . . no O(4) C(46) H(51) 110.0 . . . no C(45) C(46) H(50) 110.0 . . . no C(45) C(46) H(51) 110.0 . . . no H(50) C(46) H(51) 109.5 . . . no #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #=END #------------------------------------------------------------------------------ data_V(NCS)(dpya) _database_code_CSD 167777 _audit_creation_date 'Mon Feb 4 19:19:54 2002' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C28 H27 N10 O S4 V ' _chemical_formula_moiety '?' _chemical_formula_weight 698.77 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _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 13.331(3) _cell_length_b 17.890(2) _cell_length_c 8.405(1) _cell_angle_alpha 93.41(1) _cell_angle_beta 91.08(1) _cell_angle_gamma 107.11(1) _cell_volume 1911.1(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.2 _cell_measurement_theta_max 13.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.512 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.866 _exptl_absorpt_correction_T_max 0.950 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_reflns_number 9206 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_theta_max 27.56 _diffrn_measured_fraction_theta_max 1.0010 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 1.0010 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 1.33 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 3.0 sigma(F^2^). The weighted R-factor (wR), goodness of fit (S) and R-factor (gt) are based on F, with F set to zero for negative F. The threshold expression of F^2^ > 3.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8827 _reflns_number_gt 3407 _reflns_threshold_expression F^2^>3.0\s(F^2^) _refine_ls_structure_factor_coef F _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.1583 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3407 _refine_ls_number_parameters 368 _refine_ls_goodness_of_fit_ref 1.891 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00490|Fo|^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max 1.13 _refine_diff_density_min -0.43 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 V(1) V 0.0358(1) -0.2293(1) 0.0256(2) 0.0512(5) Uani 1.00 d . . . S(1) S 0.3517(3) -0.0392(3) -0.1041(7) 0.123(2) Uani 1.00 d . . . S(2) S -0.1064(3) -0.1999(2) -0.4851(3) 0.0750(10) Uani 1.00 d . . . S(3) S -0.2966(3) -0.3990(3) 0.1659(5) 0.105(1) Uani 1.00 d . . . S(4) S 0.1718(5) -0.4322(3) -0.1800(5) 0.130(2) Uani 1.00 d . . . O(1) O 0.285(1) 0.037(1) 0.433(2) 0.087(5) Uiso 0.50 d P . . O(2) O 0.5794(10) 0.2965(7) 0.819(1) 0.051(3) Uiso 0.50 d P . . N(1) N 0.0948(7) -0.2316(5) 0.2577(9) 0.056(3) Uani 1.00 d . . . N(2) N 0.1310(8) -0.0957(5) 0.309(1) 0.070(3) Uani 1.00 d . . . N(3) N -0.0132(7) -0.1366(5) 0.1282(9) 0.054(3) Uani 1.00 d . . . N(4) N 0.0919(7) -0.3165(6) -0.056(1) 0.068(3) Uani 1.00 d . . . N(5) N -0.0273(7) -0.2185(5) -0.190(1) 0.063(3) Uani 1.00 d . . . N(6) N -0.1010(8) -0.3064(5) 0.084(1) 0.064(3) Uani 1.00 d . . . N(7) N 0.1723(7) -0.1501(6) -0.021(1) 0.063(3) Uani 1.00 d . . . N(8) N 0.2569(8) 0.4818(6) 0.496(1) 0.069(3) Uani 1.00 d . . . N(9) N 0.3826(10) 0.5914(6) 0.408(1) 0.084(4) Uani 1.00 d . . . N(10) N 0.4409(8) 0.5509(6) 0.640(1) 0.074(3) Uani 1.00 d . . . C(1) C 0.098(1) -0.3011(7) 0.315(1) 0.075(4) Uani 1.00 d . . . C(2) C 0.146(1) -0.3086(9) 0.454(2) 0.087(5) Uani 1.00 d . . . C(3) C 0.199(1) -0.240(1) 0.547(2) 0.097(6) Uani 1.00 d . . . C(4) C 0.196(1) -0.1714(10) 0.493(1) 0.088(5) Uani 1.00 d . . . C(5) C 0.1414(8) -0.1667(7) 0.351(1) 0.062(3) Uani 1.00 d . . . C(6) C 0.0449(9) -0.0816(6) 0.234(1) 0.058(3) Uani 1.00 d . . . C(7) C 0.024(1) -0.0117(7) 0.274(1) 0.073(4) Uani 1.00 d . . . C(8) C -0.061(1) 0.0009(7) 0.209(2) 0.087(5) Uani 1.00 d . . . C(9) C -0.128(1) -0.0556(9) 0.109(2) 0.090(5) Uani 1.00 d . . . C(10) C -0.1035(8) -0.1251(7) 0.069(1) 0.065(4) Uani 1.00 d . . . C(11) C 0.129(1) -0.3629(7) -0.108(1) 0.074(4) Uani 1.00 d . . . C(12) C -0.0599(8) -0.2108(5) -0.312(1) 0.051(3) Uani 1.00 d . . . C(13) C -0.1832(10) -0.3441(7) 0.119(1) 0.062(4) Uani 1.00 d . . . C(14) C 0.2462(9) -0.1044(7) -0.054(1) 0.064(4) Uani 1.00 d . . . C(15) C 0.1653(10) 0.4219(6) 0.477(1) 0.072(4) Uani 1.00 d . . . C(16) C 0.104(1) 0.4163(8) 0.345(2) 0.089(5) Uani 1.00 d . . . C(17) C 0.134(1) 0.4699(9) 0.232(2) 0.098(5) Uani 1.00 d . . . C(18) C 0.226(1) 0.5302(7) 0.248(2) 0.085(4) Uani 1.00 d . . . C(19) C 0.288(1) 0.5343(7) 0.386(1) 0.071(4) Uani 1.00 d . . . C(20) C 0.4597(10) 0.6003(7) 0.524(1) 0.067(4) Uani 1.00 d . . . C(21) C 0.558(1) 0.6589(8) 0.512(2) 0.086(5) Uani 1.00 d . . . C(22) C 0.634(1) 0.6667(9) 0.626(2) 0.095(5) Uani 1.00 d . . . C(23) C 0.614(1) 0.6137(9) 0.749(2) 0.086(5) Uani 1.00 d . . . C(24) C 0.519(1) 0.5591(8) 0.751(1) 0.079(4) Uani 1.00 d . . . C(25) C 0.3239 0.0874 0.5456 0.096(8) Uiso 0.50 d P . . C(26) C 0.4379 0.1196 0.5086 0.18(2) Uiso 0.50 d P . . C(27) C 0.4362 0.0892 0.3537 0.21(2) Uiso 0.50 d P . . C(28) C 0.3495 0.0626 0.3348 0.24(2) Uiso 0.50 d P . . C(29) C 0.5270 0.3025 0.9256 0.13(1) Uiso 0.50 d P . . C(30) C 0.4957 0.2456 1.0260 0.15(1) Uiso 0.50 d P . . C(31) C 0.5561 0.2127 0.9903 0.18(2) Uiso 0.50 d P . . C(32) C 0.6159 0.2409 0.8564 0.067(6) Uiso 0.50 d P . . H(1) H 0.0632 -0.3480 0.2515 0.0895 Uiso 1.00 calc . . . H(2) H 0.1435 -0.3587 0.4884 0.1056 Uiso 1.00 calc . . . H(3) H 0.2365 -0.2410 0.6442 0.1163 Uiso 1.00 calc . . . H(4) H 0.2307 -0.1235 0.5538 0.1032 Uiso 1.00 calc . . . H(5) H 0.1736 -0.0512 0.3991 0.1078 Uiso 1.00 calc . . . H(6) H 0.0690 0.0269 0.3465 0.0872 Uiso 1.00 calc . . . H(7) H -0.0736 0.0497 0.2311 0.1051 Uiso 1.00 calc . . . H(8) H -0.1898 -0.0473 0.0672 0.1063 Uiso 1.00 calc . . . H(9) H -0.1499 -0.1648 -0.0005 0.0775 Uiso 1.00 calc . . . H(10) H 0.1448 0.3845 0.5553 0.0845 Uiso 1.00 calc . . . H(11) H 0.0401 0.3747 0.3301 0.1065 Uiso 1.00 calc . . . H(12) H 0.0873 0.4648 0.1428 0.1193 Uiso 1.00 calc . . . H(13) H 0.2478 0.5661 0.1667 0.1027 Uiso 1.00 calc . . . H(14) H 0.3652 0.6392 0.4174 0.1007 Uiso 1.00 calc . . . H(15) H 0.4171 0.5884 0.3107 0.1007 Uiso 1.00 calc . . . H(16) H 0.5699 0.6916 0.4241 0.1029 Uiso 1.00 calc . . . H(17) H 0.6995 0.7070 0.6212 0.1136 Uiso 1.00 calc . . . H(18) H 0.6661 0.6164 0.8298 0.1022 Uiso 1.00 calc . . . H(19) H 0.5056 0.5248 0.8361 0.0942 Uiso 1.00 calc . . . H(20) H 0.3167 0.0635 0.6444 0.1133 Uiso 0.50 calc P . . H(21) H 0.2909 0.1278 0.5496 0.1133 Uiso 0.50 calc P . . H(22) H 0.4817 0.1012 0.5769 0.2188 Uiso 0.50 calc P . . H(23) H 0.4602 0.1753 0.5155 0.2188 Uiso 0.50 calc P . . H(24) H 0.4639 0.1289 0.2826 0.2508 Uiso 0.50 calc P . . H(25) H 0.4728 0.0511 0.3444 0.2508 Uiso 0.50 calc P . . H(26) H 0.3263 0.1019 0.2876 0.2797 Uiso 0.50 calc P . . H(27) H 0.3421 0.0197 0.2588 0.2797 Uiso 0.50 calc P . . H(28) H 0.5645 0.3485 0.9887 0.1558 Uiso 0.50 calc P . . H(29) H 0.4650 0.3098 0.8804 0.1558 Uiso 0.50 calc P . . H(30) H 0.5043 0.2651 1.1346 0.1693 Uiso 0.50 calc P . . H(31) H 0.4251 0.2144 1.0045 0.1693 Uiso 0.50 calc P . . H(32) H 0.6034 0.2174 1.0788 0.2164 Uiso 0.50 calc P . . H(33) H 0.5189 0.1590 0.9664 0.2164 Uiso 0.50 calc P . . H(34) H 0.6888 0.2597 0.8841 0.0809 Uiso 0.50 calc P . . H(35) H 0.6041 0.2014 0.7716 0.0809 Uiso 0.50 calc 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V(1) 0.055(1) 0.052(1) 0.0484(10) 0.0186(8) 0.0027(7) 0.0021(7) S(1) 0.076(3) 0.100(3) 0.194(5) 0.019(2) 0.046(3) 0.046(3) S(2) 0.077(2) 0.086(2) 0.057(2) 0.013(2) -0.004(1) 0.016(2) S(3) 0.063(2) 0.138(3) 0.108(3) 0.011(2) 0.005(2) 0.056(3) S(4) 0.204(5) 0.149(4) 0.088(3) 0.136(4) -0.011(3) -0.012(3) N(1) 0.061(5) 0.063(5) 0.049(5) 0.026(4) 0.003(4) 0.010(4) N(2) 0.082(7) 0.061(6) 0.059(6) 0.012(5) -0.004(5) -0.004(4) N(3) 0.055(5) 0.058(5) 0.051(5) 0.019(4) 0.006(4) 0.008(4) N(4) 0.069(6) 0.066(6) 0.073(6) 0.027(5) -0.003(5) -0.009(5) N(5) 0.073(6) 0.070(6) 0.047(5) 0.022(5) -0.001(5) 0.000(4) N(6) 0.067(6) 0.058(6) 0.066(6) 0.016(5) 0.000(5) 0.008(4) N(7) 0.059(6) 0.071(6) 0.061(5) 0.021(5) 0.010(5) 0.010(5) N(8) 0.098(8) 0.061(6) 0.056(5) 0.032(6) 0.008(5) 0.010(5) N(9) 0.112(9) 0.069(7) 0.068(6) 0.020(6) -0.006(6) 0.010(5) N(10) 0.084(7) 0.077(7) 0.058(6) 0.019(5) 0.004(5) 0.011(5) C(1) 0.093(9) 0.082(8) 0.066(7) 0.048(7) 0.013(6) 0.018(6) C(2) 0.10(1) 0.12(1) 0.068(8) 0.061(9) -0.001(7) 0.017(8) C(3) 0.10(1) 0.14(1) 0.070(9) 0.06(1) -0.004(8) 0.025(9) C(4) 0.074(9) 0.12(1) 0.057(7) 0.022(8) -0.021(6) -0.015(7) C(5) 0.056(7) 0.077(8) 0.054(6) 0.022(6) 0.001(5) -0.003(6) C(6) 0.063(7) 0.063(7) 0.050(6) 0.017(6) 0.013(5) 0.016(5) C(7) 0.100(10) 0.056(7) 0.067(7) 0.027(7) 0.007(7) 0.004(6) C(8) 0.12(1) 0.051(7) 0.091(10) 0.027(8) 0.029(9) 0.002(7) C(9) 0.10(1) 0.11(1) 0.093(9) 0.074(9) 0.030(8) 0.031(9) C(10) 0.053(7) 0.071(7) 0.074(7) 0.020(6) 0.003(5) 0.008(6) C(11) 0.099(10) 0.079(8) 0.057(7) 0.047(8) -0.021(6) 0.003(6) C(12) 0.051(6) 0.043(5) 0.053(6) 0.004(4) 0.008(5) 0.000(5) C(13) 0.070(8) 0.068(7) 0.054(6) 0.028(7) 0.004(6) 0.009(5) C(14) 0.058(7) 0.066(7) 0.070(7) 0.023(6) 0.010(6) 0.008(6) C(15) 0.071(8) 0.051(6) 0.082(8) 0.001(6) -0.016(6) 0.002(6) C(16) 0.090(10) 0.088(10) 0.084(9) 0.020(8) -0.015(8) 0.001(8) C(17) 0.13(1) 0.085(10) 0.077(9) 0.035(10) -0.053(9) -0.019(8) C(18) 0.11(1) 0.064(8) 0.070(8) 0.022(8) -0.028(8) -0.002(6) C(19) 0.082(9) 0.056(7) 0.075(8) 0.021(7) -0.011(7) -0.013(6) C(20) 0.083(9) 0.059(7) 0.063(7) 0.026(6) 0.003(6) 0.005(6) C(21) 0.10(1) 0.074(8) 0.082(9) 0.015(8) 0.009(8) 0.010(7) C(22) 0.074(9) 0.09(1) 0.11(1) 0.012(8) -0.006(8) -0.010(9) C(23) 0.082(10) 0.10(1) 0.076(9) 0.025(8) -0.014(7) -0.008(8) C(24) 0.088(10) 0.087(9) 0.058(7) 0.024(8) -0.013(7) 0.003(6) #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution 'DIRDIF94 (PATTY)' _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag V(1) N(1) 2.098(8) . . yes V(1) N(3) 2.099(8) . . yes V(1) N(4) 2.011(10) . . yes V(1) N(5) 2.028(9) . . yes V(1) N(6) 2.03(1) . . yes V(1) N(7) 2.01(1) . . yes S(1) C(14) 1.62(1) . . yes S(2) C(12) 1.61(1) . . yes S(3) C(13) 1.61(1) . . yes S(4) C(11) 1.60(1) . . yes O(1) C(25) 1.3 . . yes O(1) C(28) 1.2 . . yes O(2) C(29) 1.2 . . yes O(2) C(32) 1.3 . . yes N(1) C(1) 1.37(1) . . yes N(1) C(5) 1.34(1) . . yes N(2) C(5) 1.38(1) . . yes N(2) C(6) 1.39(1) . . yes N(3) C(6) 1.33(1) . . yes N(3) C(10) 1.37(1) . . yes N(4) C(11) 1.15(1) . . yes N(5) C(12) 1.14(1) . . yes N(6) C(13) 1.16(1) . . yes N(7) C(14) 1.13(1) . . yes N(8) C(15) 1.37(1) . . yes N(8) C(19) 1.34(1) . . yes N(9) C(19) 1.37(2) . . yes N(9) C(20) 1.37(1) . . yes N(10) C(20) 1.33(1) . . yes N(10) C(24) 1.35(1) . . yes C(1) C(2) 1.36(2) . . yes C(2) C(3) 1.41(2) . . yes C(3) C(4) 1.34(2) . . yes C(4) C(5) 1.41(2) . . yes C(6) C(7) 1.38(2) . . yes C(7) C(8) 1.33(2) . . yes C(8) C(9) 1.36(2) . . yes C(9) C(10) 1.40(2) . . yes C(15) C(16) 1.34(2) . . yes C(16) C(17) 1.37(2) . . yes C(17) C(18) 1.37(2) . . yes C(18) C(19) 1.40(2) . . yes C(20) C(21) 1.43(2) . . yes C(21) C(22) 1.35(2) . . yes C(22) C(23) 1.42(2) . . yes C(23) C(24) 1.36(2) . . yes C(25) C(26) 1.505 . . yes C(26) C(27) 1.378 . . yes C(27) C(28) 1.117 . . yes C(29) C(30) 1.337 . . yes C(30) C(31) 1.162 . . yes C(31) C(32) 1.422 . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N(1) V(1) N(3) 83.1(3) . . . yes N(1) V(1) N(4) 92.0(3) . . . yes N(1) V(1) N(5) 174.3(3) . . . yes N(1) V(1) N(6) 88.7(3) . . . yes N(1) V(1) N(7) 89.0(4) . . . yes N(3) V(1) N(4) 174.8(4) . . . yes N(3) V(1) N(5) 91.2(3) . . . yes N(3) V(1) N(6) 89.9(3) . . . yes N(3) V(1) N(7) 88.1(3) . . . yes N(4) V(1) N(5) 93.7(4) . . . yes N(4) V(1) N(6) 91.7(4) . . . yes N(4) V(1) N(7) 90.1(4) . . . yes N(5) V(1) N(6) 91.0(4) . . . yes N(5) V(1) N(7) 91.2(4) . . . yes N(6) V(1) N(7) 177.1(4) . . . yes C(25) O(1) C(28) 97 . . . yes C(29) O(2) C(32) 103 . . . yes C(1) N(1) C(5) 116.4(10) . . . yes C(5) N(2) C(6) 127.9(9) . . . yes C(6) N(3) C(10) 117.0(9) . . . yes C(15) N(8) C(19) 121(1) . . . yes C(19) N(9) C(20) 128(1) . . . yes C(20) N(10) C(24) 117(1) . . . yes N(1) C(1) C(2) 125(1) . . . yes C(1) C(2) C(3) 117(1) . . . yes C(2) C(3) C(4) 117(1) . . . yes C(3) C(4) C(5) 122(1) . . . yes N(1) C(5) N(2) 119.0(9) . . . yes N(1) C(5) C(4) 120(1) . . . yes N(2) C(5) C(4) 120(1) . . . yes N(2) C(6) N(3) 118.1(9) . . . yes N(2) C(6) C(7) 118(1) . . . yes N(3) C(6) C(7) 123(1) . . . yes C(6) C(7) C(8) 118(1) . . . yes C(7) C(8) C(9) 120(1) . . . yes C(8) C(9) C(10) 119(1) . . . yes N(3) C(10) C(9) 120(1) . . . yes S(4) C(11) N(4) 175(1) . . . yes S(2) C(12) N(5) 179.8(10) . . . yes S(3) C(13) N(6) 178(1) . . . yes S(1) C(14) N(7) 179(1) . . . yes N(8) C(15) C(16) 118(1) . . . yes C(15) C(16) C(17) 120(1) . . . yes C(16) C(17) C(18) 121(1) . . . yes C(17) C(18) C(19) 116(1) . . . yes N(8) C(19) N(9) 119(1) . . . yes N(8) C(19) C(18) 120(1) . . . yes N(9) C(19) C(18) 119(1) . . . yes N(9) C(20) N(10) 118(1) . . . yes N(9) C(20) C(21) 119(1) . . . yes N(10) C(20) C(21) 122(1) . . . yes C(20) C(21) C(22) 118(1) . . . yes C(21) C(22) C(23) 118(1) . . . yes C(22) C(23) C(24) 118(1) . . . yes N(10) C(24) C(23) 123(1) . . . yes O(1) C(25) C(26) 105 . . . yes C(25) C(26) C(27) 100.405 . . . yes C(26) C(27) C(28) 98.75 . . . yes O(1) C(28) C(27) 129 . . . yes O(2) C(29) C(30) 121 . . . yes C(29) C(30) C(31) 96.52 . . . yes C(30) C(31) C(32) 114.78 . . . yes O(2) C(32) C(31) 102 . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? #------------------------------------------------------------------------------ loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_site_distance_DH _geom_hbond_site_distance_HA _geom_hbond_site_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag ? ? ? ? ? ? ? ? ? ? ? #------------------------------------------------------------------------------