Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof Yoichi Sasaki' _publ_contact_author_address ; Division of Chemistry, Graduate School of Science Hokkaido University Sapporo 060-0810 JAPAN ; _publ_contact_author_email YSASAKI@SCI.HOKUDAI.AC.JP _publ_section_title ; Mononuclear oxovanadium complexes of tris(2-pyridylmethyl)amine ; loop_ _publ_author_name 'Yoichi Sasaki' 'Yasunobu Tajika' 'Kiyoshi Tsuge' data_[VO(SO4)(tpa)] _database_code_depnum_ccdc_archive 'CCDC 250590' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H26 N4 O7 S V ' _chemical_formula_moiety ? _chemical_formula_weight 517.45 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 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 11.583(3) _cell_length_b 13.466(3) _cell_length_c 15.253(4) _cell_angle_alpha 90 _cell_angle_beta 108.883(3) _cell_angle_gamma 90 _cell_volume 2251.1(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8326 _cell_measurement_theta_min 3.9 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.72 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.33 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.583 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7548 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 153.1500 _diffrn_source_power 2.5000 _diffrn_source_voltage 50.0000 _diffrn_source_current 50.0000 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6199 _diffrn_number_total 11166 _diffrn_reflns_av_R_equivalents 0.0140 _diffrn_reflns_av_sigmaI/detI 0.0294 _diffrn_reflns_theta_full 27.4835 _diffrn_measured_fraction_theta_max 27.4835 _diffrn_measured_fraction_theta_full 85.1000 _diffrn_reflns_theta_min 3.8737 _diffrn_reflns_theta_max 27.4835 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 360 Slice: -76.0000 - 104.0000 Image width: 0.5000 Exp time: 45.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 40.7558 2theta: 14.0669 scan: Number of images: 120 Slice: -16.0000 - 44.0000 Image width: 0.5000 Exp time: 45.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 40.7558 2theta: 14.0669 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using all the reflections measured. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4385 _reflns_number_gt 4085 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0448 _refine_ls_wR_factor_ref 0.1507 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4385 _refine_ls_number_parameters 298 _refine_ls_goodness_of_fit_ref 1.629 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.08000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0008 _refine_diff_density_max 0.73 _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 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) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; V V 0.300 0.529 ;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 0.43259(2) 0.08557(2) 0.32894(2) 0.0141(1) Uani 1.00 d . . . S(1) S 0.69304(4) 0.08478(3) 0.30307(3) 0.0193(1) Uani 1.00 d . . . O(1) O 0.4628(1) -0.00899(9) 0.39560(8) 0.0214(3) Uani 1.00 d . . . O(2) O 0.5526(1) 0.08383(9) 0.26380(9) 0.0215(3) Uani 1.00 d . . . O(3) O 0.7328(1) -0.0061(1) 0.2703(1) 0.0443(5) Uani 1.00 d . . . O(4) O 0.7346(1) 0.17299(10) 0.26809(9) 0.0279(3) Uani 1.00 d . . . O(5) O 0.7279(1) 0.0848(1) 0.4039(1) 0.0370(4) Uani 1.00 d . . . O(7) O 0.1121(2) 0.0179(1) 0.8292(1) 0.0396(4) Uani 1.00 d . . . O(8) O 0.8842(2) 0.2937(1) 0.0333(1) 0.0445(5) Uani 1.00 d . . . N(1) N 0.3456(1) 0.21310(10) 0.23133(9) 0.0171(3) Uani 1.00 d . . . N(2) N 0.5124(1) 0.21350(10) 0.40486(10) 0.0171(3) Uani 1.00 d . . . N(3) N 0.2823(1) 0.12858(10) 0.37266(9) 0.0163(3) Uani 1.00 d . . . N(4) N 0.3091(1) 0.0171(1) 0.21118(9) 0.0170(3) Uani 1.00 d . . . C(1) C 0.4395(2) 0.2933(1) 0.2555(1) 0.0188(4) Uani 1.00 d . . . C(2) C 0.4927(1) 0.3011(1) 0.3586(1) 0.0178(4) Uani 1.00 d . . . C(3) C 0.5258(2) 0.3907(1) 0.4044(1) 0.0224(4) Uani 1.00 d . . . C(4) C 0.5841(2) 0.3900(1) 0.4997(1) 0.0260(4) Uani 1.00 d . . . C(5) C 0.6062(2) 0.3002(1) 0.5465(1) 0.0244(4) Uani 1.00 d . . . C(6) C 0.5675(2) 0.2135(1) 0.4973(1) 0.0213(4) Uani 1.00 d . . . C(7) C 0.2300(1) 0.2464(1) 0.2438(1) 0.0204(4) Uani 1.00 d . . . C(8) C 0.2113(1) 0.2058(1) 0.3303(1) 0.0179(4) Uani 1.00 d . . . C(9) C 0.1205(2) 0.2428(1) 0.3623(1) 0.0220(4) Uani 1.00 d . . . C(10) C 0.0987(2) 0.1979(1) 0.4368(1) 0.0240(4) Uani 1.00 d . . . C(11) C 0.1707(2) 0.1175(1) 0.4798(1) 0.0228(4) Uani 1.00 d . . . C(12) C 0.2622(2) 0.0864(1) 0.4466(1) 0.0194(4) Uani 1.00 d . . . C(13) C 0.3251(2) 0.1731(1) 0.1374(1) 0.0208(4) Uani 1.00 d . . . C(14) C 0.2711(2) 0.0703(1) 0.1316(1) 0.0176(4) Uani 1.00 d . . . C(15) C 0.1923(2) 0.0307(1) 0.0502(1) 0.0238(4) Uani 1.00 d . . . C(16) C 0.1529(2) -0.0668(1) 0.0505(1) 0.0268(5) Uani 1.00 d . . . C(17) C 0.1919(2) -0.1212(1) 0.1322(1) 0.0244(4) Uani 1.00 d . . . C(18) C 0.2690(2) -0.0772(1) 0.2105(1) 0.0199(4) Uani 1.00 d . . . C(19) C 0.0237(2) -0.0559(2) 0.7905(2) 0.0348(5) Uani 1.00 d . . . C(20) C 0.9004(2) 0.3451(2) 0.1153(2) 0.0514(7) Uani 1.00 d . . . H(1) H 0.5022 0.2780 0.2301 0.0226 Uiso 1.00 calc . . . H(2) H 0.4027 0.3547 0.2309 0.0226 Uiso 1.00 calc . . . H(3) H 0.5090 0.4516 0.3713 0.0269 Uiso 1.00 calc . . . H(4) H 0.6086 0.4506 0.5324 0.0312 Uiso 1.00 calc . . . H(5) H 0.6473 0.2983 0.6114 0.0293 Uiso 1.00 calc . . . H(6) H 0.5801 0.1521 0.5297 0.0255 Uiso 1.00 calc . . . H(7) H 0.2305 0.3169 0.2470 0.0245 Uiso 1.00 calc . . . H(8) H 0.1640 0.2252 0.1918 0.0245 Uiso 1.00 calc . . . H(9) H 0.0736 0.2987 0.3331 0.0264 Uiso 1.00 calc . . . H(10) H 0.0354 0.2214 0.4585 0.0288 Uiso 1.00 calc . . . H(11) H 0.1571 0.0849 0.5309 0.0274 Uiso 1.00 calc . . . H(12) H 0.3131 0.0330 0.4770 0.0233 Uiso 1.00 calc . . . H(13) H 0.2704 0.2151 0.0930 0.0249 Uiso 1.00 calc . . . H(14) H 0.4005 0.1698 0.1254 0.0249 Uiso 1.00 calc . . . H(15) H 0.1657 0.0695 -0.0047 0.0286 Uiso 1.00 calc . . . H(16) H 0.1000 -0.0959 -0.0046 0.0322 Uiso 1.00 calc . . . H(17) H 0.1655 -0.1878 0.1338 0.0293 Uiso 1.00 calc . . . H(18) H 0.2951 -0.1145 0.2664 0.0239 Uiso 1.00 calc . . . H(19) H -0.0435 -0.0271 0.7440 0.0417 Uiso 1.00 calc . . . H(20) H 0.0586 -0.1066 0.7638 0.0417 Uiso 1.00 calc . . . H(21) H -0.0035 -0.0836 0.8376 0.0417 Uiso 1.00 calc . . . H(22) H 0.8992 0.2997 0.1627 0.0617 Uiso 1.00 calc . . . H(23) H 0.9767 0.3786 0.1328 0.0617 Uiso 1.00 calc . . . H(24) H 0.8365 0.3921 0.1066 0.0617 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) 0.0171(2) 0.0124(2) 0.0122(2) 0.00196(8) 0.0040(2) 0.00203(8) S(1) 0.0205(3) 0.0158(3) 0.0241(3) 0.0014(1) 0.0106(2) 0.0032(1) O(1) 0.0263(6) 0.0178(6) 0.0199(6) 0.0038(4) 0.0069(5) 0.0043(4) O(2) 0.0207(6) 0.0261(7) 0.0193(6) 0.0042(4) 0.0086(5) 0.0012(4) O(3) 0.0334(8) 0.0205(7) 0.088(1) -0.0007(5) 0.0326(8) -0.0114(8) O(4) 0.0381(8) 0.0210(6) 0.0244(7) -0.0103(5) 0.0096(6) 0.0018(5) O(5) 0.0264(8) 0.059(1) 0.0227(7) 0.0022(6) 0.0035(6) 0.0175(6) O(7) 0.0551(10) 0.0336(8) 0.0347(8) -0.0127(7) 0.0210(7) -0.0153(6) O(8) 0.0497(10) 0.0433(9) 0.048(1) 0.0045(7) 0.0258(8) -0.0090(7) N(1) 0.0218(7) 0.0145(6) 0.0153(7) 0.0002(5) 0.0064(6) 0.0013(5) N(2) 0.0194(7) 0.0152(6) 0.0167(7) 0.0003(5) 0.0058(5) 0.0007(5) N(3) 0.0180(6) 0.0151(6) 0.0148(6) 0.0009(5) 0.0040(5) 0.0009(5) N(4) 0.0199(7) 0.0162(7) 0.0144(6) 0.0027(5) 0.0048(5) 0.0006(5) C(1) 0.0234(8) 0.0152(7) 0.0187(8) -0.0024(6) 0.0080(7) 0.0021(6) C(2) 0.0197(8) 0.0167(8) 0.0189(8) 0.0005(5) 0.0089(7) 0.0011(6) C(3) 0.0279(9) 0.0173(7) 0.0248(9) -0.0013(6) 0.0122(7) -0.0013(7) C(4) 0.0317(9) 0.0218(8) 0.0263(9) -0.0046(7) 0.0120(8) -0.0081(7) C(5) 0.0272(9) 0.0294(9) 0.0164(8) -0.0013(7) 0.0066(7) -0.0037(7) C(6) 0.0241(8) 0.0214(8) 0.0182(8) -0.0001(6) 0.0066(7) 0.0015(6) C(7) 0.0196(8) 0.0195(8) 0.0211(8) 0.0050(6) 0.0052(7) 0.0047(6) C(8) 0.0179(8) 0.0149(7) 0.0195(8) -0.0007(5) 0.0039(7) -0.0016(6) C(9) 0.0192(8) 0.0213(8) 0.0233(8) 0.0038(6) 0.0039(7) -0.0013(6) C(10) 0.0220(8) 0.0286(9) 0.0227(9) 0.0019(6) 0.0088(7) -0.0032(7) C(11) 0.0259(9) 0.0269(9) 0.0178(8) -0.0023(7) 0.0101(7) -0.0009(7) C(12) 0.0215(9) 0.0197(8) 0.0168(8) -0.0009(5) 0.0058(7) 0.0002(5) C(13) 0.0282(9) 0.0186(8) 0.0151(7) 0.0012(6) 0.0065(7) 0.0029(6) C(14) 0.0201(8) 0.0174(7) 0.0143(8) 0.0030(6) 0.0043(7) 0.0004(6) C(15) 0.0270(9) 0.0238(8) 0.0162(8) 0.0040(7) 0.0009(7) 0.0010(6) C(16) 0.0259(9) 0.0256(9) 0.0231(9) -0.0009(7) -0.0001(8) -0.0043(7) C(17) 0.0236(8) 0.0184(8) 0.0282(9) -0.0005(6) 0.0043(7) -0.0008(7) C(18) 0.0206(9) 0.0179(8) 0.0211(8) 0.0018(6) 0.0067(7) 0.0025(6) C(19) 0.035(1) 0.035(1) 0.037(1) -0.0052(8) 0.0150(9) -0.0033(9) C(20) 0.052(1) 0.050(1) 0.039(1) 0.020(1) -0.004(1) -0.009(1) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution MULTAN88 _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) 1.596(1) . . yes V(1) O(2) 1.953(1) . . yes V(1) N(1) 2.282(1) . . yes V(1) N(2) 2.114(1) . . yes V(1) N(3) 2.136(1) . . yes V(1) N(4) 2.112(1) . . yes S(1) O(2) 1.541(1) . . yes S(1) O(3) 1.452(1) . . yes S(1) O(4) 1.447(1) . . yes S(1) O(5) 1.459(2) . . yes O(7) C(19) 1.412(3) . . yes O(8) C(20) 1.388(3) . . yes N(1) C(1) 1.492(2) . . yes N(1) C(7) 1.483(2) . . yes N(1) C(13) 1.476(2) . . yes N(2) C(2) 1.355(2) . . yes N(2) C(6) 1.347(2) . . yes N(3) C(8) 1.353(2) . . yes N(3) C(12) 1.349(2) . . yes N(4) C(14) 1.355(2) . . yes N(4) C(18) 1.350(2) . . yes C(1) C(2) 1.496(2) . . yes C(1) H(1) 0.950 . . no C(1) H(2) 0.950 . . no C(2) C(3) 1.385(2) . . yes C(3) C(4) 1.390(3) . . yes C(3) H(3) 0.950 . . no C(4) C(5) 1.386(3) . . yes C(4) H(4) 0.950 . . no C(5) C(6) 1.382(2) . . yes C(5) H(5) 0.950 . . no C(6) H(6) 0.950 . . no C(7) C(8) 1.507(2) . . yes C(7) H(7) 0.950 . . no C(7) H(8) 0.950 . . no C(8) C(9) 1.388(2) . . yes C(9) C(10) 1.382(3) . . yes C(9) H(9) 0.950 . . no C(10) C(11) 1.395(3) . . yes C(10) H(10) 0.950 . . no C(11) C(12) 1.380(2) . . yes C(11) H(11) 0.950 . . no C(12) H(12) 0.950 . . no C(13) C(14) 1.509(2) . . yes C(13) H(13) 0.950 . . no C(13) H(14) 0.950 . . no C(14) C(15) 1.388(2) . . yes C(15) C(16) 1.390(3) . . yes C(15) H(15) 0.950 . . no C(16) C(17) 1.389(3) . . yes C(16) H(16) 0.950 . . no C(17) C(18) 1.374(3) . . yes C(17) H(17) 0.950 . . no C(18) H(18) 0.950 . . no C(19) H(19) 0.950 . . no C(19) H(20) 0.950 . . no C(19) H(21) 0.950 . . no C(20) H(22) 0.950 . . no C(20) H(23) 0.950 . . no C(20) H(24) 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) O(2) 105.61(6) . . . yes O(1) V(1) N(1) 167.24(6) . . . yes O(1) V(1) N(2) 109.53(6) . . . yes O(1) V(1) N(3) 92.88(6) . . . yes O(1) V(1) N(4) 98.15(6) . . . yes O(2) V(1) N(1) 85.05(5) . . . yes O(2) V(1) N(2) 91.80(5) . . . yes O(2) V(1) N(3) 161.51(5) . . . yes O(2) V(1) N(4) 87.70(5) . . . yes N(1) V(1) N(2) 76.50(5) . . . yes N(1) V(1) N(3) 76.55(5) . . . yes N(1) V(1) N(4) 74.90(5) . . . yes N(2) V(1) N(3) 82.19(5) . . . yes N(2) V(1) N(4) 151.34(5) . . . yes N(3) V(1) N(4) 89.31(5) . . . yes O(2) S(1) O(3) 105.75(8) . . . yes O(2) S(1) O(4) 107.39(8) . . . yes O(2) S(1) O(5) 107.89(8) . . . yes O(3) S(1) O(4) 112.65(10) . . . yes O(3) S(1) O(5) 110.6(1) . . . yes O(4) S(1) O(5) 112.17(9) . . . yes V(1) O(2) S(1) 129.63(8) . . . yes V(1) N(1) C(1) 104.56(9) . . . yes V(1) N(1) C(7) 111.72(10) . . . yes V(1) N(1) C(13) 104.89(10) . . . yes C(1) N(1) C(7) 111.5(1) . . . yes C(1) N(1) C(13) 112.3(1) . . . yes C(7) N(1) C(13) 111.5(1) . . . yes V(1) N(2) C(2) 117.0(1) . . . yes V(1) N(2) C(6) 123.3(1) . . . yes C(2) N(2) C(6) 119.2(1) . . . yes V(1) N(3) C(8) 119.4(1) . . . yes V(1) N(3) C(12) 121.7(1) . . . yes C(8) N(3) C(12) 118.7(1) . . . yes V(1) N(4) C(14) 117.7(1) . . . yes V(1) N(4) C(18) 123.6(1) . . . yes C(14) N(4) C(18) 118.7(1) . . . yes N(1) C(1) C(2) 109.2(1) . . . yes N(1) C(1) H(1) 109.5 . . . no N(1) C(1) H(2) 109.5 . . . no C(2) C(1) H(1) 109.5 . . . no C(2) C(1) H(2) 109.5 . . . no H(1) C(1) H(2) 109.5 . . . no N(2) C(2) C(1) 115.4(1) . . . yes N(2) C(2) C(3) 121.5(2) . . . yes C(1) C(2) C(3) 123.0(1) . . . yes C(2) C(3) C(4) 119.0(2) . . . yes C(2) C(3) H(3) 120.5 . . . no C(4) C(3) H(3) 120.5 . . . no C(3) C(4) C(5) 119.3(2) . . . yes C(3) C(4) H(4) 120.3 . . . no C(5) C(4) H(4) 120.3 . . . no C(4) C(5) C(6) 119.0(2) . . . yes C(4) C(5) H(5) 120.5 . . . no C(6) C(5) H(5) 120.5 . . . no N(2) C(6) C(5) 121.9(2) . . . yes N(2) C(6) H(6) 119.0 . . . no C(5) C(6) H(6) 119.0 . . . no N(1) C(7) C(8) 113.2(1) . . . yes N(1) C(7) H(7) 108.5 . . . no N(1) C(7) H(8) 108.5 . . . no C(8) C(7) H(7) 108.5 . . . no C(8) C(7) H(8) 108.5 . . . no H(7) C(7) H(8) 109.5 . . . no N(3) C(8) C(7) 117.3(1) . . . yes N(3) C(8) C(9) 121.4(2) . . . yes C(7) C(8) C(9) 121.2(1) . . . yes C(8) C(9) C(10) 119.5(2) . . . yes C(8) C(9) H(9) 120.2 . . . no C(10) C(9) H(9) 120.2 . . . no C(9) C(10) C(11) 119.1(2) . . . yes C(9) C(10) H(10) 120.4 . . . no C(11) C(10) H(10) 120.4 . . . no C(10) C(11) C(12) 118.5(2) . . . yes C(10) C(11) H(11) 120.8 . . . no C(12) C(11) H(11) 120.8 . . . no N(3) C(12) C(11) 122.7(2) . . . yes N(3) C(12) H(12) 118.7 . . . no C(11) C(12) H(12) 118.6 . . . no N(1) C(13) C(14) 109.0(1) . . . yes N(1) C(13) H(13) 109.6 . . . no N(1) C(13) H(14) 109.6 . . . no C(14) C(13) H(13) 109.6 . . . no C(14) C(13) H(14) 109.6 . . . no H(13) C(13) H(14) 109.5 . . . no N(4) C(14) C(13) 115.2(1) . . . yes N(4) C(14) C(15) 121.8(2) . . . yes C(13) C(14) C(15) 123.0(2) . . . yes C(14) C(15) C(16) 118.8(2) . . . yes C(14) C(15) H(15) 120.6 . . . no C(16) C(15) H(15) 120.6 . . . no C(15) C(16) C(17) 119.3(2) . . . yes C(15) C(16) H(16) 120.4 . . . no C(17) C(16) H(16) 120.4 . . . no C(16) C(17) C(18) 119.0(2) . . . yes C(16) C(17) H(17) 120.5 . . . no C(18) C(17) H(17) 120.5 . . . no N(4) C(18) C(17) 122.5(2) . . . yes N(4) C(18) H(18) 118.8 . . . no C(17) C(18) H(18) 118.8 . . . no O(7) C(19) H(19) 109.5 . . . no O(7) C(19) H(20) 109.5 . . . no O(7) C(19) H(21) 109.5 . . . no H(19) C(19) H(20) 109.5 . . . no H(19) C(19) H(21) 109.5 . . . no H(20) C(19) H(21) 109.5 . . . no O(8) C(20) H(22) 109.5 . . . no O(8) C(20) H(23) 109.5 . . . no O(8) C(20) H(24) 109.5 . . . no H(22) C(20) H(23) 109.5 . . . no H(22) C(20) H(24) 109.5 . . . no H(23) C(20) H(24) 109.5 . . . no #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[V(O)Cl(tpa)](PF6) _database_code_depnum_ccdc_archive 'CCDC 250591' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H21 Cl F6 N5 O P V ' _chemical_formula_moiety ? _chemical_formula_weight 578.78 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 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 11.797(2) _cell_length_b 14.829(2) _cell_length_c 14.162(2) _cell_angle_alpha 90 _cell_angle_beta 99.0217(9) _cell_angle_gamma 90 _cell_volume 2446.8(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7316 _cell_measurement_theta_min 1.3730 _cell_measurement_theta_max 30.0326 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.89 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5527 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 153.1500 _diffrn_source_power 2.5000 _diffrn_source_voltage 50.0000 _diffrn_source_current 50.0000 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.7059 _diffrn_reflns_number 15597 _diffrn_number_total 15597 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/detI 0.0508 _diffrn_reflns_theta_full 30.0326 _diffrn_measured_fraction_theta_max 30.0326 _diffrn_measured_fraction_theta_full 77.4000 _diffrn_reflns_theta_min 2.0908 _diffrn_reflns_theta_max 30.0326 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 360 Slice: -76.0000 - 104.0000 Image width: 0.5000 Exp time: 30.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 40.3773 2theta: 14.2496 scan: Number of images: 120 Slice: -16.0000 - 44.0000 Image width: 0.5000 Exp time: 30.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 40.3773 2theta: 14.2496 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_orient_matrix_UB_11 0.0526 _diffrn_orient_matrix_UB_12 -0.0214 _diffrn_orient_matrix_UB_13 0.0644 _diffrn_orient_matrix_UB_21 -0.0133 _diffrn_orient_matrix_UB_22 -0.0652 _diffrn_orient_matrix_UB_23 -0.0108 _diffrn_orient_matrix_UB_31 0.0610 _diffrn_orient_matrix_UB_32 -0.0063 _diffrn_orient_matrix_UB_33 -0.0368 _diffrn_orient_matrix_type d*Trek _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using all the reflections measured. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5472 _reflns_number_gt 4377 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1397 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5472 _refine_ls_number_parameters 316 _refine_ls_goodness_of_fit_ref 1.484 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 0.64 _refine_diff_density_min -0.51 _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 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) ; V V 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;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) ; #------------------------------------------------------------------------------ # 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 0.83034(4) 0.19743(3) 0.68094(3) 0.0228(1) Uani 1.00 d . . . Cl(1) Cl 1.02572(6) 0.19267(5) 0.67289(5) 0.0299(2) Uani 1.00 d . . . P(1) P 0.27139(7) 0.10936(6) 0.98534(5) 0.0351(2) Uani 1.00 d . . . F(1) F 0.1620(2) 0.0459(2) 0.9775(2) 0.0857(8) Uani 1.00 d . . . F(2) F 0.3182(2) 0.0703(2) 1.0886(1) 0.0744(8) Uani 1.00 d . . . F(3) F 0.2063(2) 0.1865(2) 1.0314(2) 0.0848(9) Uani 1.00 d . . . F(4) F 0.3811(2) 0.1716(2) 0.9913(1) 0.0597(7) Uani 1.00 d . . . F(5) F 0.2214(2) 0.1479(1) 0.8812(1) 0.0439(5) Uani 1.00 d . . . F(6) F 0.3380(2) 0.0333(1) 0.9360(2) 0.0736(8) Uani 1.00 d . . . O(1) O 0.7803(2) 0.2333(1) 0.5764(1) 0.0351(6) Uani 1.00 d . . . N(1) N 0.8639(2) 0.1512(1) 0.8361(1) 0.0223(6) Uani 1.00 d . . . N(2) N 0.8218(2) 0.0552(1) 0.6718(1) 0.0248(6) Uani 1.00 d . . . N(3) N 0.6626(2) 0.1894(1) 0.7176(2) 0.0265(6) Uani 1.00 d . . . N(4) N 0.8540(2) 0.3176(1) 0.7610(1) 0.0242(6) Uani 1.00 d . . . N(5) N 0.6047(7) 0.3755(5) 0.9136(5) 0.216(4) Uani 1.00 d . . . C(1) C 0.9205(2) 0.0618(2) 0.8346(2) 0.0279(7) Uani 1.00 d . . . C(2) C 0.8631(2) 0.0076(2) 0.7510(2) 0.0270(7) Uani 1.00 d . . . C(3) C 0.8572(3) -0.0859(2) 0.7532(2) 0.0324(8) Uani 1.00 d . . . C(4) C 0.8089(3) -0.1307(2) 0.6715(2) 0.0408(9) Uani 1.00 d . . . C(5) C 0.7655(3) -0.0819(2) 0.5908(2) 0.0411(9) Uani 1.00 d . . . C(6) C 0.7727(3) 0.0106(2) 0.5931(2) 0.0340(8) Uani 1.00 d . . . C(7) C 0.7553(2) 0.1459(2) 0.8771(2) 0.0293(7) Uani 1.00 d . . . C(8) C 0.6491(2) 0.1631(2) 0.8064(2) 0.0287(7) Uani 1.00 d . . . C(9) C 0.5423(3) 0.1542(3) 0.8326(2) 0.046(1) Uani 1.00 d . . . C(10) C 0.4461(3) 0.1731(3) 0.7667(3) 0.060(1) Uani 1.00 d . . . C(11) C 0.4596(3) 0.1997(3) 0.6762(3) 0.056(1) Uani 1.00 d . . . C(12) C 0.5674(3) 0.2072(2) 0.6543(2) 0.0401(9) Uani 1.00 d . . . C(13) C 0.9418(2) 0.2194(2) 0.8881(2) 0.0255(7) Uani 1.00 d . . . C(14) C 0.9030(2) 0.3116(2) 0.8539(2) 0.0239(7) Uani 1.00 d . . . C(15) C 0.9188(3) 0.3874(2) 0.9113(2) 0.0313(8) Uani 1.00 d . . . C(16) C 0.8863(3) 0.4704(2) 0.8729(2) 0.0360(8) Uani 1.00 d . . . C(17) C 0.8376(3) 0.4769(2) 0.7780(2) 0.0330(8) Uani 1.00 d . . . C(18) C 0.8215(2) 0.3997(2) 0.7241(2) 0.0288(7) Uani 1.00 d . . . C(19) C 0.5533(5) 0.4038(4) 0.8500(4) 0.100(2) Uani 1.00 d . . . C(20) C 0.4921(5) 0.4336(5) 0.7657(4) 0.119(3) Uani 1.00 d . . . H(1) H 0.9991 0.0702 0.8292 0.0335 Uiso 1.00 calc . . . H(2) H 0.9149 0.0305 0.8922 0.0335 Uiso 1.00 calc . . . H(3) H 0.8860 -0.1183 0.8097 0.0389 Uiso 1.00 calc . . . H(4) H 0.8054 -0.1947 0.6707 0.0490 Uiso 1.00 calc . . . H(5) H 0.7311 -0.1119 0.5342 0.0493 Uiso 1.00 calc . . . H(6) H 0.7422 0.0440 0.5377 0.0409 Uiso 1.00 calc . . . H(7) H 0.7498 0.0873 0.9030 0.0352 Uiso 1.00 calc . . . H(8) H 0.7587 0.1894 0.9267 0.0352 Uiso 1.00 calc . . . H(9) H 0.5348 0.1352 0.8954 0.0557 Uiso 1.00 calc . . . H(10) H 0.3716 0.1678 0.7837 0.0724 Uiso 1.00 calc . . . H(11) H 0.3945 0.2127 0.6297 0.0675 Uiso 1.00 calc . . . H(12) H 0.5760 0.2258 0.5916 0.0482 Uiso 1.00 calc . . . H(13) H 0.9401 0.2147 0.9547 0.0306 Uiso 1.00 calc . . . H(14) H 1.0179 0.2094 0.8762 0.0306 Uiso 1.00 calc . . . H(15) H 0.9517 0.3822 0.9767 0.0376 Uiso 1.00 calc . . . H(16) H 0.8975 0.5230 0.9115 0.0432 Uiso 1.00 calc . . . H(17) H 0.8154 0.5339 0.7505 0.0396 Uiso 1.00 calc . . . H(18) H 0.7867 0.4039 0.6591 0.0345 Uiso 1.00 calc . . . H(19) H 0.4514 0.4868 0.7769 0.1429 Uiso 1.00 calc . . . H(20) H 0.5432 0.4464 0.7218 0.1429 Uiso 1.00 calc . . . H(21) H 0.4392 0.3884 0.7397 0.1429 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) 0.0338(3) 0.0202(2) 0.0153(2) -0.0005(2) 0.0061(2) 0.0014(2) Cl(1) 0.0367(4) 0.0245(4) 0.0307(4) -0.0014(3) 0.0122(3) -0.0017(3) P(1) 0.0356(4) 0.0377(5) 0.0313(4) -0.0066(3) 0.0030(3) 0.0071(3) F(1) 0.062(1) 0.122(2) 0.064(1) -0.055(1) -0.020(1) 0.052(1) F(2) 0.066(1) 0.105(2) 0.044(1) -0.020(1) -0.016(1) 0.032(1) F(3) 0.082(2) 0.123(2) 0.055(1) 0.036(2) 0.025(1) -0.019(1) F(4) 0.058(1) 0.073(2) 0.051(1) -0.034(1) 0.0180(10) -0.017(1) F(5) 0.054(1) 0.043(1) 0.0349(10) 0.0031(9) 0.0080(8) 0.0133(8) F(6) 0.073(2) 0.050(1) 0.088(2) 0.022(1) -0.019(1) -0.022(1) O(1) 0.047(1) 0.040(1) 0.0197(10) 0.0024(10) 0.0078(8) 0.0067(8) N(1) 0.030(1) 0.019(1) 0.019(1) -0.0003(9) 0.0042(9) 0.0017(8) N(2) 0.035(1) 0.020(1) 0.020(1) -0.0019(9) 0.0074(9) -0.0020(8) N(3) 0.032(1) 0.024(1) 0.023(1) -0.0013(10) 0.0048(9) 0.0013(9) N(4) 0.032(1) 0.021(1) 0.020(1) -0.0018(9) 0.0065(9) 0.0012(8) N(5) 0.253(8) 0.209(8) 0.140(5) -0.131(7) -0.111(6) 0.079(5) C(1) 0.039(2) 0.022(1) 0.023(1) 0.004(1) 0.004(1) 0.004(1) C(2) 0.035(1) 0.022(1) 0.026(1) 0.000(1) 0.012(1) 0.000(1) C(3) 0.042(2) 0.022(1) 0.036(2) 0.001(1) 0.014(1) 0.001(1) C(4) 0.055(2) 0.022(2) 0.050(2) -0.009(1) 0.021(2) -0.007(1) C(5) 0.053(2) 0.034(2) 0.038(2) -0.011(1) 0.009(1) -0.013(1) C(6) 0.044(2) 0.033(2) 0.026(1) -0.007(1) 0.007(1) -0.005(1) C(7) 0.037(2) 0.034(2) 0.019(1) -0.003(1) 0.009(1) 0.001(1) C(8) 0.035(2) 0.025(1) 0.028(1) 0.000(1) 0.011(1) 0.003(1) C(9) 0.037(2) 0.062(2) 0.043(2) 0.003(2) 0.016(1) 0.014(2) C(10) 0.035(2) 0.084(3) 0.064(2) 0.007(2) 0.013(2) 0.024(2) C(11) 0.032(2) 0.074(3) 0.061(2) 0.001(2) 0.000(2) 0.024(2) C(12) 0.038(2) 0.045(2) 0.035(2) 0.000(1) -0.001(1) 0.011(1) C(13) 0.034(1) 0.024(1) 0.018(1) -0.001(1) 0.002(1) -0.001(1) C(14) 0.031(1) 0.022(1) 0.020(1) -0.003(1) 0.007(1) 0.0003(10) C(15) 0.043(2) 0.028(2) 0.024(1) -0.006(1) 0.009(1) -0.003(1) C(16) 0.055(2) 0.021(1) 0.036(2) -0.008(1) 0.018(1) -0.006(1) C(17) 0.046(2) 0.021(1) 0.035(2) 0.002(1) 0.015(1) 0.004(1) C(18) 0.039(2) 0.022(1) 0.027(1) 0.002(1) 0.009(1) 0.005(1) C(19) 0.087(4) 0.118(5) 0.080(3) -0.042(3) -0.036(3) 0.038(3) C(20) 0.102(5) 0.132(6) 0.114(5) -0.002(4) -0.012(4) 0.024(4) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _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) 2.3264(9) . . yes V(1) O(1) 1.597(2) . . yes V(1) N(1) 2.276(2) . . yes V(1) N(2) 2.115(2) . . yes V(1) N(3) 2.127(2) . . yes V(1) N(4) 2.107(2) . . yes P(1) F(1) 1.587(2) . . yes P(1) F(2) 1.589(2) . . yes P(1) F(3) 1.574(2) . . yes P(1) F(4) 1.581(2) . . yes P(1) F(5) 1.604(2) . . yes P(1) F(6) 1.597(2) . . yes N(1) C(1) 1.486(3) . . yes N(1) C(7) 1.489(3) . . yes N(1) C(13) 1.483(3) . . yes N(2) C(2) 1.350(3) . . yes N(2) C(6) 1.346(3) . . yes N(3) C(8) 1.349(3) . . yes N(3) C(12) 1.349(4) . . yes N(4) C(14) 1.354(3) . . yes N(4) C(18) 1.355(3) . . yes N(5) C(19) 1.089(7) . . yes C(1) C(2) 1.502(4) . . yes C(1) H(1) 0.950 . . no C(1) H(2) 0.950 . . no C(2) C(3) 1.389(4) . . yes C(3) C(4) 1.377(4) . . yes C(3) H(3) 0.950 . . no C(4) C(5) 1.382(4) . . yes C(4) H(4) 0.950 . . no C(5) C(6) 1.374(4) . . yes C(5) H(5) 0.950 . . no C(6) H(6) 0.950 . . no C(7) C(8) 1.497(4) . . yes C(7) H(7) 0.950 . . no C(7) H(8) 0.950 . . no C(8) C(9) 1.375(4) . . yes C(9) C(10) 1.381(5) . . yes C(9) H(9) 0.950 . . no C(10) C(11) 1.373(5) . . yes C(10) H(10) 0.950 . . no C(11) C(12) 1.360(5) . . yes C(11) H(11) 0.950 . . no C(12) H(12) 0.950 . . no C(13) C(14) 1.498(4) . . yes C(13) H(13) 0.950 . . no C(13) H(14) 0.950 . . no C(14) C(15) 1.382(4) . . yes C(15) C(16) 1.376(4) . . yes C(15) H(15) 0.950 . . no C(16) C(17) 1.379(4) . . yes C(16) H(16) 0.950 . . no C(17) C(18) 1.374(4) . . yes C(17) H(17) 0.950 . . no C(18) H(18) 0.950 . . no C(19) C(20) 1.368(7) . . yes C(20) H(19) 0.950 . . no C(20) H(20) 0.950 . . no C(20) H(21) 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 Cl(1) V(1) O(1) 100.96(8) . . . yes Cl(1) V(1) N(1) 90.84(6) . . . yes Cl(1) V(1) N(2) 90.29(6) . . . yes Cl(1) V(1) N(3) 167.74(6) . . . yes Cl(1) V(1) N(4) 90.21(6) . . . yes O(1) V(1) N(1) 168.05(9) . . . yes O(1) V(1) N(2) 105.56(10) . . . yes O(1) V(1) N(3) 91.27(10) . . . yes O(1) V(1) N(4) 102.46(10) . . . yes N(1) V(1) N(2) 75.98(8) . . . yes N(1) V(1) N(3) 76.98(8) . . . yes N(1) V(1) N(4) 75.36(8) . . . yes N(2) V(1) N(3) 85.50(8) . . . yes N(2) V(1) N(4) 151.35(8) . . . yes N(3) V(1) N(4) 88.03(9) . . . yes F(1) P(1) F(2) 90.5(1) . . . yes F(1) P(1) F(3) 90.9(2) . . . yes F(1) P(1) F(4) 178.8(1) . . . yes F(1) P(1) F(5) 88.2(1) . . . yes F(1) P(1) F(6) 90.1(2) . . . yes F(2) P(1) F(3) 90.3(1) . . . yes F(2) P(1) F(4) 90.0(1) . . . yes F(2) P(1) F(5) 178.8(1) . . . yes F(2) P(1) F(6) 91.2(1) . . . yes F(3) P(1) F(4) 90.1(1) . . . yes F(3) P(1) F(5) 89.4(1) . . . yes F(3) P(1) F(6) 178.2(1) . . . yes F(4) P(1) F(5) 91.2(1) . . . yes F(4) P(1) F(6) 88.9(1) . . . yes F(5) P(1) F(6) 89.1(1) . . . yes V(1) N(1) C(1) 105.4(1) . . . yes V(1) N(1) C(7) 111.2(2) . . . yes V(1) N(1) C(13) 105.9(1) . . . yes C(1) N(1) C(7) 112.1(2) . . . yes C(1) N(1) C(13) 111.7(2) . . . yes C(7) N(1) C(13) 110.3(2) . . . yes V(1) N(2) C(2) 117.6(2) . . . yes V(1) N(2) C(6) 123.4(2) . . . yes C(2) N(2) C(6) 118.9(2) . . . yes V(1) N(3) C(8) 119.6(2) . . . yes V(1) N(3) C(12) 122.4(2) . . . yes C(8) N(3) C(12) 118.0(3) . . . yes V(1) N(4) C(14) 117.9(2) . . . yes V(1) N(4) C(18) 123.1(2) . . . yes C(14) N(4) C(18) 119.0(2) . . . yes N(1) C(1) C(2) 109.9(2) . . . yes N(1) C(1) H(1) 109.4 . . . no N(1) C(1) H(2) 109.4 . . . no C(2) C(1) H(1) 109.4 . . . no C(2) C(1) H(2) 109.4 . . . no H(1) C(1) H(2) 109.5 . . . no N(2) C(2) C(1) 115.8(2) . . . yes N(2) C(2) C(3) 121.8(3) . . . yes C(1) C(2) C(3) 122.3(2) . . . yes C(2) C(3) C(4) 118.6(3) . . . yes C(2) C(3) H(3) 120.7 . . . no C(4) C(3) H(3) 120.7 . . . no C(3) C(4) C(5) 119.6(3) . . . yes C(3) C(4) H(4) 120.2 . . . no C(5) C(4) H(4) 120.2 . . . no C(4) C(5) C(6) 119.3(3) . . . yes C(4) C(5) H(5) 120.4 . . . no C(6) C(5) H(5) 120.4 . . . no N(2) C(6) C(5) 121.8(3) . . . yes N(2) C(6) H(6) 119.1 . . . no C(5) C(6) H(6) 119.1 . . . no N(1) C(7) C(8) 114.2(2) . . . yes N(1) C(7) H(7) 108.3 . . . no N(1) C(7) H(8) 108.3 . . . no C(8) C(7) H(7) 108.3 . . . no C(8) C(7) H(8) 108.3 . . . no H(7) C(7) H(8) 109.5 . . . no N(3) C(8) C(7) 117.7(2) . . . yes N(3) C(8) C(9) 121.7(3) . . . yes C(7) C(8) C(9) 120.6(2) . . . yes C(8) C(9) C(10) 119.3(3) . . . yes C(8) C(9) H(9) 120.4 . . . no C(10) C(9) H(9) 120.4 . . . no C(9) C(10) C(11) 119.1(3) . . . yes C(9) C(10) H(10) 120.5 . . . no C(11) C(10) H(10) 120.5 . . . no C(10) C(11) C(12) 119.1(3) . . . yes C(10) C(11) H(11) 120.5 . . . no C(12) C(11) H(11) 120.5 . . . no N(3) C(12) C(11) 122.8(3) . . . yes N(3) C(12) H(12) 118.6 . . . no C(11) C(12) H(12) 118.6 . . . no N(1) C(13) C(14) 109.2(2) . . . yes N(1) C(13) H(13) 109.6 . . . no N(1) C(13) H(14) 109.6 . . . no C(14) C(13) H(13) 109.6 . . . no C(14) C(13) H(14) 109.6 . . . no H(13) C(13) H(14) 109.5 . . . no N(4) C(14) C(13) 115.9(2) . . . yes N(4) C(14) C(15) 121.0(2) . . . yes C(13) C(14) C(15) 123.1(2) . . . yes C(14) C(15) C(16) 119.4(3) . . . yes C(14) C(15) H(15) 120.3 . . . no C(16) C(15) H(15) 120.3 . . . no C(15) C(16) C(17) 119.7(3) . . . yes C(15) C(16) H(16) 120.1 . . . no C(17) C(16) H(16) 120.1 . . . no C(16) C(17) C(18) 118.9(3) . . . yes C(16) C(17) H(17) 120.6 . . . no C(18) C(17) H(17) 120.6 . . . no N(4) C(18) C(17) 121.9(2) . . . yes N(4) C(18) H(18) 119.0 . . . no C(17) C(18) H(18) 119.0 . . . no N(5) C(19) C(20) 175.1(10) . . . yes C(19) C(20) H(19) 109.5 . . . no C(19) C(20) H(20) 109.5 . . . no C(19) C(20) H(21) 109.5 . . . no H(19) C(20) H(20) 109.5 . . . no H(19) C(20) H(21) 109.5 . . . no H(20) C(20) H(21) 109.5 . . . no #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[V(O)Br(tpa)](PF6) _database_code_depnum_ccdc_archive 'CCDC 250592' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C20 H21 Br F6 N5 O P V ' _chemical_formula_moiety ? _chemical_formula_weight 623.23 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 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 11.324(2) _cell_length_b 15.280(3) _cell_length_c 14.376(3) _cell_angle_alpha 90 _cell_angle_beta 99.061(4) _cell_angle_gamma 90 _cell_volume 2456.5(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8650 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 223.2 #------------------------------------------------------------------------------ _exptl_crystal_description Plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.685 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 2.169 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7211 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 153 _diffrn_source_power 2.5000 _diffrn_source_voltage 50.0000 _diffrn_source_current 50.0000 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6199 _diffrn_number_total 14752 _diffrn_reflns_av_R_equivalents 0.0190 _diffrn_reflns_av_sigmaI/detI 0.0407 _diffrn_reflns_theta_full 27.4835 _diffrn_measured_fraction_theta_max 27.4835 _diffrn_measured_fraction_theta_full 95.4000 _diffrn_reflns_theta_min 3.1631 _diffrn_reflns_theta_max 27.4835 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 360 Slice: -76.0000 - 104.0000 Image width: 0.5000 Exp time: 40.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 40.6009 2theta: 14.0567 scan: Number of images: 120 Slice: -16.0000 - 44.0000 Image width: 0.5000 Exp time: 40.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 40.6009 2theta: 14.0567 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using all the reflections measured. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 5386 _reflns_number_gt 4545 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1269 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5386 _refine_ls_number_parameters 316 _refine_ls_goodness_of_fit_ref 1.618 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 0.99 _refine_diff_density_min -0.40 _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 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) ; V V 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Br Br -0.290 2.459 ;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 Br(1) Br 0.44844(3) 0.19521(2) 0.32790(2) 0.02570(9) Uani 1.00 d . . . V(1) V 0.66690(4) 0.20159(3) 0.32147(3) 0.0157(1) Uani 1.00 d . . . P(1) P 0.78001(8) -0.40751(6) 0.48300(6) 0.0274(2) Uani 1.00 d . . . F(1) F 0.6626(2) -0.4674(2) 0.4635(2) 0.0583(8) Uani 1.00 d . . . F(2) F 0.7149(3) -0.3441(2) 0.5446(2) 0.083(1) Uani 1.00 d . . . F(3) F 0.8989(2) -0.3500(2) 0.5022(2) 0.0518(7) Uani 1.00 d . . . F(4) F 0.8448(2) -0.4705(2) 0.4195(2) 0.0529(7) Uani 1.00 d . . . F(5) F 0.8254(2) -0.4637(2) 0.5737(2) 0.0621(8) Uani 1.00 d . . . F(6) F 0.7309(3) -0.3538(2) 0.3901(2) 0.0677(9) Uani 1.00 d . . . O(1) O 0.7115(2) 0.2382(1) 0.4251(1) 0.0259(6) Uani 1.00 d . . . N(1) N 0.6418(2) 0.1562(1) 0.1686(2) 0.0160(6) Uani 1.00 d . . . N(2) N 0.6823(2) 0.0641(2) 0.3316(2) 0.0175(6) Uani 1.00 d . . . N(3) N 0.8457(2) 0.1941(1) 0.2928(2) 0.0186(6) Uani 1.00 d . . . N(4) N 0.6404(2) 0.3170(2) 0.2406(2) 0.0168(6) Uani 1.00 d . . . N(5) N 0.8958(4) 0.1312(3) 0.5960(3) 0.063(1) Uani 1.00 d . . . C(1) C 0.5915(3) 0.0668(2) 0.1676(2) 0.0209(7) Uani 1.00 d . . . C(2) C 0.6479(3) 0.0164(2) 0.2527(2) 0.0195(7) Uani 1.00 d . . . C(3) C 0.6596(3) -0.0745(2) 0.2527(2) 0.0246(8) Uani 1.00 d . . . C(4) C 0.7082(3) -0.1159(2) 0.3352(2) 0.0324(9) Uani 1.00 d . . . C(5) C 0.7448(3) -0.0671(2) 0.4150(2) 0.0326(9) Uani 1.00 d . . . C(6) C 0.7323(3) 0.0228(2) 0.4116(2) 0.0251(8) Uani 1.00 d . . . C(7) C 0.7576(3) 0.1595(2) 0.1316(2) 0.0217(7) Uani 1.00 d . . . C(8) C 0.8647(3) 0.1687(2) 0.2073(2) 0.0192(7) Uani 1.00 d . . . C(9) C 0.9789(3) 0.1569(2) 0.1862(2) 0.0286(8) Uani 1.00 d . . . C(10) C 1.0761(3) 0.1719(3) 0.2556(3) 0.0364(10) Uani 1.00 d . . . C(11) C 1.0567(3) 0.1982(2) 0.3437(3) 0.0342(9) Uani 1.00 d . . . C(12) C 0.9414(3) 0.2080(2) 0.3605(2) 0.0265(8) Uani 1.00 d . . . C(13) C 0.5564(3) 0.2193(2) 0.1151(2) 0.0195(7) Uani 1.00 d . . . C(14) C 0.5918(3) 0.3099(2) 0.1488(2) 0.0179(7) Uani 1.00 d . . . C(15) C 0.5743(3) 0.3829(2) 0.0912(2) 0.0238(8) Uani 1.00 d . . . C(16) C 0.6049(3) 0.4645(2) 0.1284(2) 0.0261(8) Uani 1.00 d . . . C(17) C 0.6547(3) 0.4722(2) 0.2224(2) 0.0242(8) Uani 1.00 d . . . C(18) C 0.6712(3) 0.3972(2) 0.2766(2) 0.0200(7) Uani 1.00 d . . . C(19) C 0.9416(3) 0.1050(3) 0.6650(3) 0.0370(10) Uani 1.00 d . . . C(20) C 1.0018(4) 0.0733(3) 0.7554(3) 0.053(1) Uani 1.00 d . . . H(1) H 0.6062 0.0373 0.1124 0.0251 Uiso 1.00 calc . . . H(2) H 0.5077 0.0705 0.1675 0.0251 Uiso 1.00 calc . . . H(3) H 0.6346 -0.1073 0.1970 0.0295 Uiso 1.00 calc . . . H(4) H 0.7163 -0.1778 0.3370 0.0389 Uiso 1.00 calc . . . H(5) H 0.7785 -0.0951 0.4721 0.0391 Uiso 1.00 calc . . . H(6) H 0.7593 0.0564 0.4665 0.0301 Uiso 1.00 calc . . . H(7) H 0.7658 0.1070 0.0978 0.0260 Uiso 1.00 calc . . . H(8) H 0.7557 0.2081 0.0902 0.0260 Uiso 1.00 calc . . . H(9) H 0.9903 0.1387 0.1251 0.0344 Uiso 1.00 calc . . . H(10) H 1.1552 0.1643 0.2427 0.0437 Uiso 1.00 calc . . . H(11) H 1.1222 0.2094 0.3922 0.0410 Uiso 1.00 calc . . . H(12) H 0.9282 0.2251 0.4216 0.0318 Uiso 1.00 calc . . . H(13) H 0.5598 0.2146 0.0496 0.0234 Uiso 1.00 calc . . . H(14) H 0.4775 0.2070 0.1259 0.0234 Uiso 1.00 calc . . . H(15) H 0.5414 0.3768 0.0266 0.0285 Uiso 1.00 calc . . . H(16) H 0.5918 0.5152 0.0897 0.0314 Uiso 1.00 calc . . . H(17) H 0.6770 0.5278 0.2491 0.0291 Uiso 1.00 calc . . . H(18) H 0.7051 0.4020 0.3412 0.0240 Uiso 1.00 calc . . . H(19) H 0.9601 0.0928 0.8038 0.0639 Uiso 1.00 calc . . . H(20) H 1.0814 0.0951 0.7666 0.0639 Uiso 1.00 calc . . . H(21) H 1.0035 0.0111 0.7548 0.0639 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 Br(1) 0.0288(2) 0.0230(2) 0.0264(2) 0.0006(1) 0.0080(1) 0.0010(1) V(1) 0.0227(3) 0.0161(3) 0.0087(2) 0.0015(2) 0.0037(2) -0.0012(2) P(1) 0.0298(4) 0.0335(5) 0.0196(4) -0.0041(4) 0.0059(3) 0.0018(3) F(1) 0.035(1) 0.104(2) 0.034(1) -0.033(1) -0.0038(9) 0.010(1) F(2) 0.099(2) 0.081(2) 0.087(2) 0.006(2) 0.064(2) -0.025(2) F(3) 0.064(2) 0.053(1) 0.043(1) -0.036(1) 0.023(1) -0.017(1) F(4) 0.045(1) 0.053(1) 0.062(1) -0.005(1) 0.013(1) -0.028(1) F(5) 0.058(2) 0.079(2) 0.041(1) -0.029(1) -0.019(1) 0.030(1) F(6) 0.068(2) 0.084(2) 0.054(2) 0.020(2) 0.018(1) 0.041(1) O(1) 0.037(1) 0.030(1) 0.0117(9) 0.0019(10) 0.0055(9) -0.0042(8) N(1) 0.020(1) 0.016(1) 0.012(1) -0.0004(9) 0.0039(9) -0.0010(9) N(2) 0.023(1) 0.017(1) 0.013(1) 0.0004(10) 0.0058(9) 0.0007(9) N(3) 0.021(1) 0.019(1) 0.016(1) 0.0013(10) 0.0029(10) -0.0001(9) N(4) 0.020(1) 0.017(1) 0.014(1) 0.0001(9) 0.0044(9) -0.0015(9) N(5) 0.071(3) 0.064(3) 0.045(2) -0.002(2) -0.015(2) 0.001(2) C(1) 0.031(2) 0.015(1) 0.016(1) -0.005(1) 0.003(1) -0.004(1) C(2) 0.023(1) 0.018(1) 0.020(1) -0.001(1) 0.010(1) -0.002(1) C(3) 0.032(2) 0.015(1) 0.030(2) 0.000(1) 0.012(1) -0.002(1) C(4) 0.045(2) 0.018(2) 0.036(2) 0.005(1) 0.014(2) 0.004(1) C(5) 0.040(2) 0.028(2) 0.030(2) 0.010(1) 0.007(2) 0.012(1) C(6) 0.032(2) 0.024(2) 0.018(1) 0.004(1) 0.004(1) 0.004(1) C(7) 0.026(2) 0.024(2) 0.016(1) 0.001(1) 0.008(1) -0.003(1) C(8) 0.025(2) 0.015(1) 0.019(1) 0.003(1) 0.006(1) 0.000(1) C(9) 0.028(2) 0.030(2) 0.030(2) 0.005(1) 0.010(1) -0.002(1) C(10) 0.022(2) 0.038(2) 0.051(2) 0.004(1) 0.008(2) -0.004(2) C(11) 0.021(2) 0.033(2) 0.046(2) 0.002(1) -0.004(1) -0.006(2) C(12) 0.025(2) 0.027(2) 0.025(2) 0.002(1) -0.002(1) -0.007(1) C(13) 0.025(1) 0.021(1) 0.011(1) 0.001(1) -0.002(1) 0.000(1) C(14) 0.020(1) 0.019(1) 0.015(1) 0.002(1) 0.004(1) 0.000(1) C(15) 0.031(2) 0.026(2) 0.015(1) 0.003(1) 0.006(1) 0.003(1) C(16) 0.036(2) 0.019(2) 0.025(2) 0.005(1) 0.010(1) 0.005(1) C(17) 0.031(2) 0.017(1) 0.027(2) -0.002(1) 0.011(1) -0.002(1) C(18) 0.024(1) 0.019(1) 0.018(1) 0.001(1) 0.006(1) -0.005(1) C(19) 0.036(2) 0.032(2) 0.040(2) -0.001(2) -0.003(2) 0.000(2) C(20) 0.051(3) 0.059(3) 0.047(2) 0.000(2) -0.004(2) 0.015(2) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _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 Br(1) V(1) 2.4920(8) . . yes V(1) O(1) 1.597(2) . . yes V(1) N(1) 2.279(2) . . yes V(1) N(2) 2.112(2) . . yes V(1) N(3) 2.132(3) . . yes V(1) N(4) 2.107(2) . . yes P(1) F(1) 1.603(2) . . yes P(1) F(2) 1.572(3) . . yes P(1) F(3) 1.595(2) . . yes P(1) F(4) 1.585(2) . . yes P(1) F(5) 1.578(2) . . yes P(1) F(6) 1.592(2) . . yes N(1) C(1) 1.478(4) . . yes N(1) C(7) 1.492(4) . . yes N(1) C(13) 1.491(4) . . yes N(2) C(2) 1.352(4) . . yes N(2) C(6) 1.356(4) . . yes N(3) C(8) 1.339(4) . . yes N(3) C(12) 1.354(4) . . yes N(4) C(14) 1.353(4) . . yes N(4) C(18) 1.354(4) . . yes N(5) C(19) 1.118(5) . . yes C(1) C(2) 1.501(4) . . yes C(1) H(1) 0.950 . . no C(1) H(2) 0.950 . . no C(2) C(3) 1.395(4) . . yes C(3) C(4) 1.380(5) . . yes C(3) H(3) 0.950 . . no C(4) C(5) 1.376(5) . . yes C(4) H(4) 0.950 . . no C(5) C(6) 1.381(4) . . yes C(5) H(5) 0.950 . . no C(6) H(6) 0.950 . . no C(7) C(8) 1.503(4) . . yes C(7) H(7) 0.950 . . no C(7) H(8) 0.950 . . no C(8) C(9) 1.385(4) . . yes C(9) C(10) 1.384(5) . . yes C(9) H(9) 0.950 . . no C(10) C(11) 1.379(5) . . yes C(10) H(10) 0.950 . . no C(11) C(12) 1.373(5) . . yes C(11) H(11) 0.950 . . no C(12) H(12) 0.950 . . no C(13) C(14) 1.501(4) . . yes C(13) H(13) 0.950 . . no C(13) H(14) 0.950 . . no C(14) C(15) 1.384(4) . . yes C(15) C(16) 1.379(4) . . yes C(15) H(15) 0.950 . . no C(16) C(17) 1.385(4) . . yes C(16) H(16) 0.950 . . no C(17) C(18) 1.382(4) . . yes C(17) H(17) 0.950 . . no C(18) H(18) 0.950 . . no C(19) C(20) 1.453(5) . . yes C(20) H(19) 0.950 . . no C(20) H(20) 0.950 . . no C(20) H(21) 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 Br(1) V(1) O(1) 98.56(8) . . . yes Br(1) V(1) N(1) 92.87(6) . . . yes Br(1) V(1) N(2) 91.73(7) . . . yes Br(1) V(1) N(3) 169.61(7) . . . yes Br(1) V(1) N(4) 89.85(7) . . . yes O(1) V(1) N(1) 168.3(1) . . . yes O(1) V(1) N(2) 105.9(1) . . . yes O(1) V(1) N(3) 91.7(1) . . . yes O(1) V(1) N(4) 102.6(1) . . . yes N(1) V(1) N(2) 76.09(8) . . . yes N(1) V(1) N(3) 77.02(9) . . . yes N(1) V(1) N(4) 74.79(8) . . . yes N(2) V(1) N(3) 83.62(9) . . . yes N(2) V(1) N(4) 150.88(9) . . . yes N(3) V(1) N(4) 89.74(9) . . . yes F(1) P(1) F(2) 90.1(2) . . . yes F(1) P(1) F(3) 178.6(2) . . . yes F(1) P(1) F(4) 89.9(1) . . . yes F(1) P(1) F(5) 89.3(1) . . . yes F(1) P(1) F(6) 88.7(1) . . . yes F(2) P(1) F(3) 91.1(2) . . . yes F(2) P(1) F(4) 179.1(2) . . . yes F(2) P(1) F(5) 89.5(2) . . . yes F(2) P(1) F(6) 91.2(2) . . . yes F(3) P(1) F(4) 88.9(1) . . . yes F(3) P(1) F(5) 90.0(1) . . . yes F(3) P(1) F(6) 92.0(1) . . . yes F(4) P(1) F(5) 91.5(2) . . . yes F(4) P(1) F(6) 87.8(1) . . . yes F(5) P(1) F(6) 177.9(2) . . . yes V(1) N(1) C(1) 106.3(2) . . . yes V(1) N(1) C(7) 110.5(2) . . . yes V(1) N(1) C(13) 105.9(2) . . . yes C(1) N(1) C(7) 112.8(2) . . . yes C(1) N(1) C(13) 112.0(2) . . . yes C(7) N(1) C(13) 109.2(2) . . . yes V(1) N(2) C(2) 117.9(2) . . . yes V(1) N(2) C(6) 122.7(2) . . . yes C(2) N(2) C(6) 119.2(3) . . . yes V(1) N(3) C(8) 119.2(2) . . . yes V(1) N(3) C(12) 122.0(2) . . . yes C(8) N(3) C(12) 118.6(3) . . . yes V(1) N(4) C(14) 118.2(2) . . . yes V(1) N(4) C(18) 122.7(2) . . . yes C(14) N(4) C(18) 119.1(2) . . . yes N(1) C(1) C(2) 110.6(2) . . . yes N(1) C(1) H(1) 109.2 . . . no N(1) C(1) H(2) 109.2 . . . no C(2) C(1) H(1) 109.2 . . . no C(2) C(1) H(2) 109.2 . . . no H(1) C(1) H(2) 109.5 . . . no N(2) C(2) C(1) 115.9(2) . . . yes N(2) C(2) C(3) 121.4(3) . . . yes C(1) C(2) C(3) 122.7(3) . . . yes C(2) C(3) C(4) 118.8(3) . . . yes C(2) C(3) H(3) 120.6 . . . no C(4) C(3) H(3) 120.6 . . . no C(3) C(4) C(5) 119.6(3) . . . yes C(3) C(4) H(4) 120.2 . . . no C(5) C(4) H(4) 120.2 . . . no C(4) C(5) C(6) 119.6(3) . . . yes C(4) C(5) H(5) 120.2 . . . no C(6) C(5) H(5) 120.2 . . . no N(2) C(6) C(5) 121.3(3) . . . yes N(2) C(6) H(6) 119.4 . . . no C(5) C(6) H(6) 119.4 . . . no N(1) C(7) C(8) 113.6(2) . . . yes N(1) C(7) H(7) 108.4 . . . no N(1) C(7) H(8) 108.4 . . . no C(8) C(7) H(7) 108.4 . . . no C(8) C(7) H(8) 108.4 . . . no H(7) C(7) H(8) 109.5 . . . no N(3) C(8) C(7) 117.6(3) . . . yes N(3) C(8) C(9) 121.9(3) . . . yes C(7) C(8) C(9) 120.3(3) . . . yes C(8) C(9) C(10) 119.0(3) . . . yes C(8) C(9) H(9) 120.5 . . . no C(10) C(9) H(9) 120.5 . . . no C(9) C(10) C(11) 119.1(3) . . . yes C(9) C(10) H(10) 120.4 . . . no C(11) C(10) H(10) 120.4 . . . no C(10) C(11) C(12) 119.1(3) . . . yes C(10) C(11) H(11) 120.4 . . . no C(12) C(11) H(11) 120.4 . . . no N(3) C(12) C(11) 122.2(3) . . . yes N(3) C(12) H(12) 118.9 . . . no C(11) C(12) H(12) 118.9 . . . no N(1) C(13) C(14) 108.1(2) . . . yes N(1) C(13) H(13) 109.8 . . . no N(1) C(13) H(14) 109.8 . . . no C(14) C(13) H(13) 109.8 . . . no C(14) C(13) H(14) 109.8 . . . no H(13) C(13) H(14) 109.5 . . . no N(4) C(14) C(13) 115.9(2) . . . yes N(4) C(14) C(15) 121.1(3) . . . yes C(13) C(14) C(15) 123.0(3) . . . yes C(14) C(15) C(16) 119.6(3) . . . yes C(14) C(15) H(15) 120.2 . . . no C(16) C(15) H(15) 120.2 . . . no C(15) C(16) C(17) 119.5(3) . . . yes C(15) C(16) H(16) 120.2 . . . no C(17) C(16) H(16) 120.3 . . . no C(16) C(17) C(18) 118.6(3) . . . yes C(16) C(17) H(17) 120.7 . . . no C(18) C(17) H(17) 120.7 . . . no N(4) C(18) C(17) 122.1(3) . . . yes N(4) C(18) H(18) 119.0 . . . no C(17) C(18) H(18) 119.0 . . . no N(5) C(19) C(20) 178.5(5) . . . yes C(19) C(20) H(19) 109.5 . . . no C(19) C(20) H(20) 109.5 . . . no C(19) C(20) H(21) 109.5 . . . no H(19) C(20) H(20) 109.5 . . . no H(19) C(20) H(21) 109.5 . . . no H(20) C(20) H(21) 109.5 . . . no #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[V(O)(O2)(tpa)]Cl _database_code_depnum_ccdc_archive 'CCDC 250593' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18.50 H23 Cl N4 O5 V ' _chemical_formula_moiety ? _chemical_formula_weight 467.80 _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 9.0018(2) _cell_length_b 16.064(2) _cell_length_c 28.6544(9) _cell_angle_alpha 90 _cell_angle_beta 101.7140(7) _cell_angle_gamma 90 _cell_volume 4057.3(5) _cell_formula_units_Z 8 _cell_measurement_temperature 113.1500 _cell_measurement_reflns_used 8801 _cell_measurement_theta_min 1.9265 _cell_measurement_theta_max 27.1016 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_meas ? _exptl_absorpt_coefficient_mu 0.659 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0066 _exptl_absorpt_correction_T_min 0.7514 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 113.1500 _diffrn_source_power 2.0000 _diffrn_source_voltage 50.0000 _diffrn_source_current 40.0000 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 7.3153 _diffrn_number_total 17669 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_sigmaI/detI 0.0926 _diffrn_reflns_theta_full 27.1016 _diffrn_measured_fraction_theta_max 27.1016 _diffrn_measured_fraction_theta_full 0.0000 _diffrn_reflns_theta_min 1.9265 _diffrn_reflns_theta_max 27.1016 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 360 Slice: -70.0000 - 110.0000 Image width: 0.5000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 50.4576 2theta: 20.0013 scan: Number of images: 120 Slice: -10.0000 - 50.0000 Image width: 0.5000 Exp time: 60.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 50.4576 2theta: 20.0013 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using all the reflections measured. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7970 _reflns_number_gt 6464 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1654 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7970 _refine_ls_number_parameters 532 _refine_ls_goodness_of_fit_ref 1.750 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.06000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0005 _refine_diff_density_max 1.01 _refine_diff_density_min -0.70 _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) ; O O 0.011 0.006 ;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) ; Cl Cl 0.148 0.159 ;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 -0.03878(7) -0.24878(4) 0.10262(2) 0.0221(2) Uani 1.00 d . . . V(2) V 0.11852(7) -0.03237(3) 0.41368(2) 0.0200(2) Uani 1.00 d . . . Cl(1) Cl 0.0829(1) 0.14256(6) 0.16205(4) 0.0393(3) Uani 1.00 d . . . Cl(2) Cl -0.3951(1) 0.07053(6) 0.09955(4) 0.0362(3) Uani 1.00 d . . . O(1) O 0.0009(3) -0.2746(2) 0.05235(9) 0.0291(7) Uani 1.00 d . . . O(2) O -0.1277(3) -0.3422(2) 0.12415(9) 0.0298(7) Uani 1.00 d . . . O(3) O 0.0308(3) -0.3360(2) 0.14459(9) 0.0303(7) Uani 1.00 d . . . O(4) O 0.0938(3) -0.0487(2) 0.46704(8) 0.0269(7) Uani 1.00 d . . . O(5) O 0.0168(3) 0.0654(2) 0.39275(9) 0.0286(7) Uani 1.00 d . . . O(6) O 0.1758(3) 0.0783(1) 0.41125(9) 0.0277(7) Uani 1.00 d . . . O(7) O 0.5915(4) 0.1479(2) 0.1962(1) 0.051(1) Uani 1.00 d . . . O(8) O 0.2521(4) 0.1046(2) 0.0791(1) 0.0496(10) Uani 1.00 d . . . O(9) O 0.8861(4) 0.1297(2) 0.0522(1) 0.0463(9) Uani 1.00 d . . . O(10) O 0.8974(4) 0.1548(2) 0.2447(1) 0.066(1) Uani 1.00 d . . . N(1) N -0.0398(3) -0.1174(2) 0.08033(10) 0.0222(8) Uani 1.00 d . . . N(2) N -0.2708(3) -0.2226(2) 0.07029(10) 0.0222(8) Uani 1.00 d . . . N(3) N -0.0954(3) -0.1786(2) 0.16429(10) 0.0208(7) Uani 1.00 d . . . N(4) N 0.1868(3) -0.2037(2) 0.1306(1) 0.0267(8) Uani 1.00 d . . . N(5) N 0.1570(3) -0.1670(2) 0.40793(9) 0.0195(7) Uani 1.00 d . . . N(6) N 0.3607(3) -0.0476(2) 0.43264(9) 0.0204(7) Uani 1.00 d . . . N(7) N 0.1639(3) -0.0498(2) 0.34025(10) 0.0207(7) Uani 1.00 d . . . N(8) N -0.1008(3) -0.0832(2) 0.38163(10) 0.0222(8) Uani 1.00 d . . . C(1) C -0.1577(4) -0.1094(2) 0.0355(1) 0.0281(10) Uani 1.00 d . . . C(2) C -0.2973(4) -0.1557(2) 0.0411(1) 0.0236(9) Uani 1.00 d . . . C(3) C -0.4399(4) -0.1357(2) 0.0168(1) 0.0273(10) Uani 1.00 d . . . C(4) C -0.5611(4) -0.1869(3) 0.0210(1) 0.030(1) Uani 1.00 d . . . C(5) C -0.5351(4) -0.2551(2) 0.0504(1) 0.029(1) Uani 1.00 d . . . C(6) C -0.3891(4) -0.2712(2) 0.0748(1) 0.0278(10) Uani 1.00 d . . . C(7) C -0.0706(4) -0.0566(2) 0.1167(1) 0.0262(9) Uani 1.00 d . . . C(8) C -0.0997(4) -0.0953(2) 0.1616(1) 0.0205(9) Uani 1.00 d . . . C(9) C -0.1305(4) -0.0452(2) 0.1979(1) 0.0260(9) Uani 1.00 d . . . C(10) C -0.1570(4) -0.0834(3) 0.2386(1) 0.031(1) Uani 1.00 d . . . C(11) C -0.1538(4) -0.1693(3) 0.2420(1) 0.032(1) Uani 1.00 d . . . C(12) C -0.1235(4) -0.2148(2) 0.2039(1) 0.0265(10) Uani 1.00 d . . . C(13) C 0.1126(4) -0.1006(2) 0.0698(1) 0.0280(10) Uani 1.00 d . . . C(14) C 0.2295(4) -0.1352(2) 0.1093(1) 0.028(1) Uani 1.00 d . . . C(15) C 0.3742(5) -0.1012(3) 0.1236(1) 0.033(1) Uani 1.00 d . . . C(16) C 0.4761(5) -0.1409(3) 0.1586(2) 0.038(1) Uani 1.00 d . . . C(17) C 0.4362(5) -0.2115(3) 0.1791(1) 0.039(1) Uani 1.00 d . . . C(18) C 0.2890(5) -0.2418(2) 0.1649(1) 0.034(1) Uani 1.00 d . . . C(19) C 0.2901(4) -0.1877(2) 0.4468(1) 0.0224(9) Uani 1.00 d . . . C(20) C 0.4127(4) -0.1242(2) 0.4467(1) 0.0216(9) Uani 1.00 d . . . C(21) C 0.5646(4) -0.1412(2) 0.4623(1) 0.0234(9) Uani 1.00 d . . . C(22) C 0.6687(4) -0.0766(2) 0.4652(1) 0.0243(9) Uani 1.00 d . . . C(23) C 0.6152(4) 0.0026(2) 0.4498(1) 0.0238(9) Uani 1.00 d . . . C(24) C 0.4629(4) 0.0146(2) 0.4336(1) 0.0223(9) Uani 1.00 d . . . C(25) C 0.1832(4) -0.1960(2) 0.3607(1) 0.0227(9) Uani 1.00 d . . . C(26) C 0.1972(4) -0.1262(2) 0.3271(1) 0.0197(8) Uani 1.00 d . . . C(27) C 0.2382(4) -0.1411(2) 0.2834(1) 0.0270(10) Uani 1.00 d . . . C(28) C 0.2445(4) -0.0749(3) 0.2534(1) 0.031(1) Uani 1.00 d . . . C(29) C 0.2083(4) 0.0037(3) 0.2665(1) 0.031(1) Uani 1.00 d . . . C(30) C 0.1696(4) 0.0146(2) 0.3103(1) 0.0281(10) Uani 1.00 d . . . C(31) C 0.0177(4) -0.2078(2) 0.4179(1) 0.0233(9) Uani 1.00 d . . . C(32) C -0.1181(4) -0.1662(2) 0.3879(1) 0.0230(9) Uani 1.00 d . . . C(33) C -0.2514(4) -0.2072(2) 0.3693(1) 0.0262(10) Uani 1.00 d . . . C(34) C -0.3729(4) -0.1616(2) 0.3440(1) 0.0280(10) Uani 1.00 d . . . C(35) C -0.3568(4) -0.0764(2) 0.3387(1) 0.028(1) Uani 1.00 d . . . C(36) C -0.2185(4) -0.0398(2) 0.3574(1) 0.0246(9) Uani 1.00 d . . . C(37) C 0.5002(5) 0.0933(3) 0.2174(2) 0.047(1) Uani 1.00 d . . . H(1) H -0.1817 -0.0523 0.0294 0.0337 Uiso 1.00 calc . . . H(2) H -0.1200 -0.1321 0.0095 0.0337 Uiso 1.00 calc . . . H(3) H -0.4559 -0.0875 -0.0028 0.0327 Uiso 1.00 calc . . . H(4) H -0.6606 -0.1748 0.0039 0.0361 Uiso 1.00 calc . . . H(5) H -0.6164 -0.2907 0.0538 0.0349 Uiso 1.00 calc . . . H(6) H -0.3716 -0.3181 0.0955 0.0334 Uiso 1.00 calc . . . H(7) H 0.0148 -0.0209 0.1249 0.0315 Uiso 1.00 calc . . . H(8) H -0.1573 -0.0248 0.1028 0.0315 Uiso 1.00 calc . . . H(9) H -0.1332 0.0137 0.1948 0.0311 Uiso 1.00 calc . . . H(10) H -0.1775 -0.0507 0.2642 0.0372 Uiso 1.00 calc . . . H(11) H -0.1719 -0.1965 0.2698 0.0380 Uiso 1.00 calc . . . H(12) H -0.1225 -0.2738 0.2059 0.0318 Uiso 1.00 calc . . . H(13) H 0.1207 -0.1265 0.0406 0.0336 Uiso 1.00 calc . . . H(14) H 0.1269 -0.0423 0.0674 0.0336 Uiso 1.00 calc . . . H(15) H 0.4015 -0.0515 0.1095 0.0400 Uiso 1.00 calc . . . H(16) H 0.5755 -0.1189 0.1685 0.0461 Uiso 1.00 calc . . . H(17) H 0.5076 -0.2397 0.2028 0.0467 Uiso 1.00 calc . . . H(18) H 0.2599 -0.2904 0.1797 0.0411 Uiso 1.00 calc . . . H(19) H 0.2599 -0.1867 0.4767 0.0269 Uiso 1.00 calc . . . H(20) H 0.3270 -0.2415 0.4415 0.0269 Uiso 1.00 calc . . . H(21) H 0.5978 -0.1962 0.4709 0.0281 Uiso 1.00 calc . . . H(22) H 0.7737 -0.0859 0.4774 0.0291 Uiso 1.00 calc . . . H(23) H 0.6840 0.0477 0.4506 0.0286 Uiso 1.00 calc . . . H(24) H 0.4277 0.0683 0.4227 0.0268 Uiso 1.00 calc . . . H(25) H 0.2741 -0.2276 0.3658 0.0273 Uiso 1.00 calc . . . H(26) H 0.1003 -0.2302 0.3464 0.0273 Uiso 1.00 calc . . . H(27) H 0.2614 -0.1959 0.2746 0.0324 Uiso 1.00 calc . . . H(28) H 0.2737 -0.0835 0.2237 0.0377 Uiso 1.00 calc . . . H(29) H 0.2100 0.0497 0.2457 0.0371 Uiso 1.00 calc . . . H(30) H 0.1462 0.0690 0.3197 0.0337 Uiso 1.00 calc . . . H(31) H 0.0179 -0.2652 0.4101 0.0279 Uiso 1.00 calc . . . H(32) H 0.0147 -0.2018 0.4507 0.0279 Uiso 1.00 calc . . . H(33) H -0.2602 -0.2655 0.3736 0.0315 Uiso 1.00 calc . . . H(34) H -0.4657 -0.1885 0.3305 0.0336 Uiso 1.00 calc . . . H(35) H -0.4394 -0.0438 0.3225 0.0336 Uiso 1.00 calc . . . H(36) H -0.2067 0.0183 0.3529 0.0296 Uiso 1.00 calc . . . H(37) H 0.3988 0.1133 0.2115 0.0566 Uiso 1.00 calc . . . H(38) H 0.5021 0.0392 0.2040 0.0566 Uiso 1.00 calc . . . H(39) H 0.5386 0.0908 0.2508 0.0566 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) 0.0270(4) 0.0158(3) 0.0238(3) 0.0005(2) 0.0060(2) -0.0030(2) V(2) 0.0244(4) 0.0157(3) 0.0205(3) 0.0012(2) 0.0060(2) -0.0026(2) Cl(1) 0.0378(6) 0.0307(5) 0.0506(6) -0.0037(4) 0.0115(5) 0.0059(4) Cl(2) 0.0397(6) 0.0312(5) 0.0386(5) 0.0051(4) 0.0103(4) 0.0058(4) O(1) 0.034(2) 0.025(1) 0.029(1) 0.002(1) 0.008(1) -0.007(1) O(2) 0.035(2) 0.018(1) 0.035(1) -0.003(1) 0.006(1) 0.003(1) O(3) 0.031(2) 0.021(1) 0.036(1) 0.003(1) 0.000(1) 0.003(1) O(4) 0.030(1) 0.027(1) 0.025(1) -0.001(1) 0.009(1) -0.006(1) O(5) 0.025(2) 0.019(1) 0.040(1) 0.004(1) 0.003(1) -0.005(1) O(6) 0.025(2) 0.018(1) 0.038(1) 0.002(1) 0.002(1) -0.004(1) O(7) 0.049(2) 0.047(2) 0.062(2) -0.011(2) 0.023(2) -0.007(2) O(8) 0.051(2) 0.041(2) 0.054(2) 0.002(1) 0.003(2) 0.000(2) O(9) 0.065(2) 0.041(2) 0.036(2) 0.005(1) 0.017(1) 0.012(1) O(10) 0.076(3) 0.060(2) 0.061(2) 0.003(2) 0.010(2) -0.022(2) N(1) 0.025(2) 0.020(1) 0.023(1) -0.002(1) 0.009(1) -0.001(1) N(2) 0.025(2) 0.018(1) 0.024(1) -0.003(1) 0.007(1) 0.001(1) N(3) 0.022(2) 0.020(1) 0.021(1) -0.001(1) 0.004(1) 0.000(1) N(4) 0.025(2) 0.025(2) 0.031(2) 0.001(1) 0.006(1) -0.006(1) N(5) 0.021(2) 0.017(1) 0.021(1) 0.000(1) 0.004(1) 0.000(1) N(6) 0.027(2) 0.018(1) 0.017(1) 0.000(1) 0.005(1) -0.001(1) N(7) 0.019(2) 0.021(1) 0.022(1) -0.002(1) 0.006(1) 0.000(1) N(8) 0.024(2) 0.022(1) 0.022(1) 0.001(1) 0.009(1) -0.002(1) C(1) 0.039(2) 0.021(2) 0.023(2) -0.002(2) 0.005(2) 0.004(1) C(2) 0.030(2) 0.018(2) 0.023(2) -0.002(1) 0.008(1) -0.003(1) C(3) 0.033(2) 0.026(2) 0.023(2) 0.002(2) 0.005(2) 0.001(1) C(4) 0.027(2) 0.038(2) 0.025(2) 0.001(2) 0.004(2) -0.007(2) C(5) 0.028(2) 0.030(2) 0.031(2) -0.009(2) 0.011(2) -0.006(2) C(6) 0.037(2) 0.023(2) 0.025(2) -0.004(2) 0.008(2) -0.002(1) C(7) 0.037(2) 0.016(2) 0.028(2) 0.000(1) 0.012(2) -0.002(1) C(8) 0.021(2) 0.017(2) 0.023(2) 0.000(1) 0.003(1) -0.001(1) C(9) 0.027(2) 0.023(2) 0.027(2) 0.001(1) 0.006(2) -0.005(1) C(10) 0.027(2) 0.043(2) 0.023(2) -0.002(2) 0.006(2) -0.009(2) C(11) 0.029(2) 0.045(2) 0.022(2) -0.004(2) 0.007(2) 0.004(2) C(12) 0.027(2) 0.026(2) 0.027(2) -0.001(2) 0.005(2) 0.003(1) C(13) 0.030(2) 0.028(2) 0.029(2) -0.006(2) 0.015(2) -0.002(1) C(14) 0.032(2) 0.025(2) 0.031(2) 0.000(2) 0.013(2) -0.007(1) C(15) 0.028(2) 0.036(2) 0.038(2) -0.005(2) 0.011(2) -0.009(2) C(16) 0.026(2) 0.047(3) 0.042(2) 0.001(2) 0.007(2) -0.014(2) C(17) 0.030(3) 0.047(3) 0.038(2) 0.011(2) 0.002(2) -0.004(2) C(18) 0.038(3) 0.028(2) 0.036(2) 0.006(2) 0.005(2) -0.004(2) C(19) 0.022(2) 0.020(2) 0.025(2) 0.001(1) 0.004(1) 0.002(1) C(20) 0.030(2) 0.017(2) 0.020(2) -0.001(1) 0.008(1) -0.001(1) C(21) 0.026(2) 0.024(2) 0.021(2) 0.003(1) 0.006(1) 0.000(1) C(22) 0.025(2) 0.031(2) 0.018(2) 0.002(2) 0.005(1) -0.002(1) C(23) 0.029(2) 0.024(2) 0.019(2) -0.005(1) 0.008(1) -0.003(1) C(24) 0.028(2) 0.019(2) 0.020(2) -0.003(1) 0.005(1) -0.002(1) C(25) 0.029(2) 0.016(2) 0.025(2) 0.001(1) 0.010(1) -0.004(1) C(26) 0.012(2) 0.023(2) 0.023(2) 0.001(1) 0.002(1) -0.001(1) C(27) 0.024(2) 0.033(2) 0.026(2) 0.002(2) 0.007(1) -0.004(1) C(28) 0.025(2) 0.050(3) 0.021(2) 0.002(2) 0.008(1) 0.001(2) C(29) 0.027(2) 0.036(2) 0.029(2) -0.004(2) 0.005(2) 0.010(2) C(30) 0.029(2) 0.023(2) 0.032(2) -0.004(2) 0.004(2) 0.004(1) C(31) 0.025(2) 0.019(2) 0.027(2) -0.004(1) 0.008(1) 0.001(1) C(32) 0.028(2) 0.021(2) 0.023(2) -0.001(1) 0.012(1) -0.003(1) C(33) 0.029(2) 0.025(2) 0.028(2) -0.004(2) 0.012(2) -0.004(1) C(34) 0.023(2) 0.035(2) 0.027(2) -0.003(2) 0.009(2) -0.002(2) C(35) 0.026(2) 0.033(2) 0.026(2) 0.004(2) 0.007(2) 0.001(2) C(36) 0.027(2) 0.026(2) 0.022(2) 0.004(2) 0.007(1) -0.001(1) C(37) 0.047(3) 0.049(3) 0.050(3) -0.013(2) 0.020(2) -0.006(2) #------------------------------------------------------------------------------ _computing_data_collection . _computing_cell_refinement . _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution MULTAN88 _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) 1.607(2) . . yes V(1) O(2) 1.863(3) . . yes V(1) O(3) 1.870(3) . . yes V(1) N(1) 2.204(3) . . yes V(1) N(2) 2.148(3) . . yes V(1) N(3) 2.241(3) . . yes V(1) N(4) 2.152(3) . . yes V(2) O(4) 1.611(2) . . yes V(2) O(5) 1.856(3) . . yes V(2) O(6) 1.856(3) . . yes V(2) N(5) 2.202(3) . . yes V(2) N(6) 2.151(3) . . yes V(2) N(7) 2.241(3) . . yes V(2) N(8) 2.161(3) . . yes O(2) O(3) 1.431(4) . . yes O(5) O(6) 1.437(4) . . yes O(7) C(37) 1.420(5) . . yes N(1) C(1) 1.497(5) . . yes N(1) C(7) 1.495(4) . . yes N(1) C(13) 1.488(5) . . yes N(2) C(2) 1.352(4) . . yes N(2) C(6) 1.348(5) . . yes N(3) C(8) 1.340(4) . . yes N(3) C(12) 1.344(4) . . yes N(4) C(14) 1.351(5) . . yes N(4) C(18) 1.349(5) . . yes N(5) C(19) 1.497(4) . . yes N(5) C(25) 1.495(4) . . yes N(5) C(31) 1.493(4) . . yes N(6) C(20) 1.350(4) . . yes N(6) C(24) 1.354(4) . . yes N(7) C(26) 1.335(4) . . yes N(7) C(30) 1.351(4) . . yes N(8) C(32) 1.358(4) . . yes N(8) C(36) 1.339(5) . . yes C(1) C(2) 1.497(5) . . yes C(1) H(1) 0.950 . . no C(1) H(2) 0.950 . . no C(2) C(3) 1.369(5) . . yes C(3) C(4) 1.391(5) . . yes C(3) H(3) 0.950 . . no C(4) C(5) 1.371(6) . . yes C(4) H(4) 0.950 . . no C(5) C(6) 1.383(6) . . yes C(5) H(5) 0.950 . . no C(6) H(6) 0.950 . . no C(7) C(8) 1.500(5) . . yes C(7) H(7) 0.950 . . no C(7) H(8) 0.950 . . no C(8) C(9) 1.385(5) . . yes C(9) C(10) 1.382(5) . . yes C(9) H(9) 0.950 . . no C(10) C(11) 1.384(6) . . yes C(10) H(10) 0.950 . . no C(11) C(12) 1.386(5) . . yes C(11) H(11) 0.950 . . no C(12) H(12) 0.950 . . no C(13) C(14) 1.488(6) . . yes C(13) H(13) 0.950 . . no C(13) H(14) 0.950 . . no C(14) C(15) 1.396(5) . . yes C(15) C(16) 1.370(6) . . yes C(15) H(15) 0.950 . . no C(16) C(17) 1.359(6) . . yes C(16) H(16) 0.950 . . no C(17) C(18) 1.393(6) . . yes C(17) H(17) 0.950 . . no C(18) H(18) 0.950 . . no C(19) C(20) 1.503(5) . . yes C(19) H(19) 0.950 . . no C(19) H(20) 0.950 . . no C(20) C(21) 1.377(5) . . yes C(21) C(22) 1.389(5) . . yes C(21) H(21) 0.950 . . no C(22) C(23) 1.399(5) . . yes C(22) H(22) 0.950 . . no C(23) C(24) 1.369(5) . . yes C(23) H(23) 0.950 . . no C(24) H(24) 0.950 . . no C(25) C(26) 1.500(5) . . yes C(25) H(25) 0.950 . . no C(25) H(26) 0.950 . . no C(26) C(27) 1.395(5) . . yes C(27) C(28) 1.377(6) . . yes C(27) H(27) 0.950 . . no C(28) C(29) 1.376(6) . . yes C(28) H(28) 0.950 . . no C(29) C(30) 1.382(5) . . yes C(29) H(29) 0.950 . . no C(30) H(30) 0.950 . . no C(31) C(32) 1.500(5) . . yes C(31) H(31) 0.950 . . no C(31) H(32) 0.950 . . no C(32) C(33) 1.379(5) . . yes C(33) C(34) 1.391(5) . . yes C(33) H(33) 0.950 . . no C(34) C(35) 1.388(6) . . yes C(34) H(34) 0.950 . . no C(35) C(36) 1.383(5) . . yes C(35) H(35) 0.950 . . no C(36) H(36) 0.950 . . no C(37) H(37) 0.950 . . no C(37) H(38) 0.950 . . no C(37) H(39) 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) O(2) 106.1(1) . . . yes O(1) V(1) O(3) 106.1(1) . . . yes O(1) V(1) N(1) 88.6(1) . . . yes O(1) V(1) N(2) 92.2(1) . . . yes O(1) V(1) N(3) 164.6(1) . . . yes O(1) V(1) N(4) 93.2(1) . . . yes O(2) V(1) O(3) 45.1(1) . . . yes O(2) V(1) N(1) 152.9(1) . . . yes O(2) V(1) N(2) 81.7(1) . . . yes O(2) V(1) N(3) 87.8(1) . . . yes O(2) V(1) N(4) 125.8(1) . . . yes O(3) V(1) N(1) 152.2(1) . . . yes O(3) V(1) N(2) 126.4(1) . . . yes O(3) V(1) N(3) 88.3(1) . . . yes O(3) V(1) N(4) 81.1(1) . . . yes N(1) V(1) N(2) 75.0(1) . . . yes N(1) V(1) N(3) 76.0(1) . . . yes N(1) V(1) N(4) 74.6(1) . . . yes N(2) V(1) N(3) 83.4(1) . . . yes N(2) V(1) N(4) 148.9(1) . . . yes N(3) V(1) N(4) 83.4(1) . . . yes O(4) V(2) O(5) 106.9(1) . . . yes O(4) V(2) O(6) 106.5(1) . . . yes O(4) V(2) N(5) 88.0(1) . . . yes O(4) V(2) N(6) 94.0(1) . . . yes O(4) V(2) N(7) 163.3(1) . . . yes O(4) V(2) N(8) 92.9(1) . . . yes O(5) V(2) O(6) 45.5(1) . . . yes O(5) V(2) N(5) 151.9(1) . . . yes O(5) V(2) N(6) 125.9(1) . . . yes O(5) V(2) N(7) 88.5(1) . . . yes O(5) V(2) N(8) 80.5(1) . . . yes O(6) V(2) N(5) 152.7(1) . . . yes O(6) V(2) N(6) 81.0(1) . . . yes O(6) V(2) N(7) 88.8(1) . . . yes O(6) V(2) N(8) 125.6(1) . . . yes N(5) V(2) N(6) 75.0(1) . . . yes N(5) V(2) N(7) 75.3(1) . . . yes N(5) V(2) N(8) 75.0(1) . . . yes N(6) V(2) N(7) 81.6(1) . . . yes N(6) V(2) N(8) 148.9(1) . . . yes N(7) V(2) N(8) 83.0(1) . . . yes V(1) O(2) O(3) 67.7(1) . . . yes V(1) O(3) O(2) 67.2(1) . . . yes V(2) O(5) O(6) 67.2(1) . . . yes V(2) O(6) O(5) 67.2(1) . . . yes V(1) N(1) C(1) 107.0(2) . . . yes V(1) N(1) C(7) 114.5(2) . . . yes V(1) N(1) C(13) 106.4(2) . . . yes C(1) N(1) C(7) 110.0(3) . . . yes C(1) N(1) C(13) 109.4(3) . . . yes C(7) N(1) C(13) 109.4(3) . . . yes V(1) N(2) C(2) 117.1(2) . . . yes V(1) N(2) C(6) 124.2(2) . . . yes C(2) N(2) C(6) 118.5(3) . . . yes V(1) N(3) C(8) 117.8(2) . . . yes V(1) N(3) C(12) 124.1(2) . . . yes C(8) N(3) C(12) 118.1(3) . . . yes V(1) N(4) C(14) 116.1(3) . . . yes V(1) N(4) C(18) 124.8(3) . . . yes C(14) N(4) C(18) 119.0(3) . . . yes V(2) N(5) C(19) 106.0(2) . . . yes V(2) N(5) C(25) 115.4(2) . . . yes V(2) N(5) C(31) 105.4(2) . . . yes C(19) N(5) C(25) 110.8(3) . . . yes C(19) N(5) C(31) 109.7(3) . . . yes C(25) N(5) C(31) 109.3(3) . . . yes V(2) N(6) C(20) 116.8(2) . . . yes V(2) N(6) C(24) 124.8(2) . . . yes C(20) N(6) C(24) 118.3(3) . . . yes V(2) N(7) C(26) 118.3(2) . . . yes V(2) N(7) C(30) 122.5(2) . . . yes C(26) N(7) C(30) 119.0(3) . . . yes V(2) N(8) C(32) 115.7(2) . . . yes V(2) N(8) C(36) 125.6(2) . . . yes C(32) N(8) C(36) 118.7(3) . . . yes N(1) C(1) C(2) 109.2(3) . . . yes N(1) C(1) H(1) 109.6 . . . no N(1) C(1) H(2) 109.6 . . . no C(2) C(1) H(1) 109.5 . . . no C(2) C(1) H(2) 109.6 . . . no H(1) C(1) H(2) 109.5 . . . no N(2) C(2) C(1) 114.5(3) . . . yes N(2) C(2) C(3) 122.0(3) . . . yes C(1) C(2) C(3) 123.3(3) . . . yes C(2) C(3) C(4) 119.2(3) . . . yes C(2) C(3) H(3) 120.4 . . . no C(4) C(3) H(3) 120.4 . . . no C(3) C(4) C(5) 119.1(3) . . . yes C(3) C(4) H(4) 120.5 . . . no C(5) C(4) H(4) 120.5 . . . no C(4) C(5) C(6) 119.2(3) . . . yes C(4) C(5) H(5) 120.4 . . . no C(6) C(5) H(5) 120.4 . . . no N(2) C(6) C(5) 122.0(3) . . . yes N(2) C(6) H(6) 119.0 . . . no C(5) C(6) H(6) 119.0 . . . no N(1) C(7) C(8) 114.6(3) . . . yes N(1) C(7) H(7) 108.2 . . . no N(1) C(7) H(8) 108.2 . . . no C(8) C(7) H(7) 108.2 . . . no C(8) C(7) H(8) 108.2 . . . no H(7) C(7) H(8) 109.5 . . . no N(3) C(8) C(7) 117.0(3) . . . yes N(3) C(8) C(9) 123.1(3) . . . yes C(7) C(8) C(9) 119.9(3) . . . yes C(8) C(9) C(10) 118.1(3) . . . yes C(8) C(9) H(9) 121.0 . . . no C(10) C(9) H(9) 121.0 . . . no C(9) C(10) C(11) 119.8(3) . . . yes C(9) C(10) H(10) 120.1 . . . no C(11) C(10) H(10) 120.1 . . . no C(10) C(11) C(12) 118.3(3) . . . yes C(10) C(11) H(11) 120.8 . . . no C(12) C(11) H(11) 120.8 . . . no N(3) C(12) C(11) 122.6(3) . . . yes N(3) C(12) H(12) 118.7 . . . no C(11) C(12) H(12) 118.7 . . . no N(1) C(13) C(14) 108.4(3) . . . yes N(1) C(13) H(13) 109.7 . . . no N(1) C(13) H(14) 109.7 . . . no C(14) C(13) H(13) 109.7 . . . no C(14) C(13) H(14) 109.7 . . . no H(13) C(13) H(14) 109.5 . . . no N(4) C(14) C(13) 115.2(3) . . . yes N(4) C(14) C(15) 121.4(4) . . . yes C(13) C(14) C(15) 123.4(4) . . . yes C(14) C(15) C(16) 118.6(4) . . . yes C(14) C(15) H(15) 120.7 . . . no C(16) C(15) H(15) 120.7 . . . no C(15) C(16) C(17) 120.6(4) . . . yes C(15) C(16) H(16) 119.7 . . . no C(17) C(16) H(16) 119.7 . . . no C(16) C(17) C(18) 119.0(4) . . . yes C(16) C(17) H(17) 120.5 . . . no C(18) C(17) H(17) 120.5 . . . no N(4) C(18) C(17) 121.4(4) . . . yes N(4) C(18) H(18) 119.3 . . . no C(17) C(18) H(18) 119.3 . . . no N(5) C(19) C(20) 109.0(3) . . . yes N(5) C(19) H(19) 109.6 . . . no N(5) C(19) H(20) 109.6 . . . no C(20) C(19) H(19) 109.6 . . . no C(20) C(19) H(20) 109.6 . . . no H(19) C(19) H(20) 109.5 . . . no N(6) C(20) C(19) 114.1(3) . . . yes N(6) C(20) C(21) 122.6(3) . . . yes C(19) C(20) C(21) 123.2(3) . . . yes C(20) C(21) C(22) 119.1(3) . . . yes C(20) C(21) H(21) 120.5 . . . no C(22) C(21) H(21) 120.5 . . . no C(21) C(22) C(23) 118.4(3) . . . yes C(21) C(22) H(22) 120.8 . . . no C(23) C(22) H(22) 120.8 . . . no C(22) C(23) C(24) 119.4(3) . . . yes C(22) C(23) H(23) 120.3 . . . no C(24) C(23) H(23) 120.3 . . . no N(6) C(24) C(23) 122.2(3) . . . yes N(6) C(24) H(24) 118.9 . . . no C(23) C(24) H(24) 118.9 . . . no N(5) C(25) C(26) 113.5(3) . . . yes N(5) C(25) H(25) 108.5 . . . no N(5) C(25) H(26) 108.5 . . . no C(26) C(25) H(25) 108.5 . . . no C(26) C(25) H(26) 108.5 . . . no H(25) C(25) H(26) 109.5 . . . no N(7) C(26) C(25) 116.9(3) . . . yes N(7) C(26) C(27) 121.8(3) . . . yes C(25) C(26) C(27) 121.2(3) . . . yes C(26) C(27) C(28) 118.6(3) . . . yes C(26) C(27) H(27) 120.7 . . . no C(28) C(27) H(27) 120.7 . . . no C(27) C(28) C(29) 119.9(3) . . . yes C(27) C(28) H(28) 120.1 . . . no C(29) C(28) H(28) 120.1 . . . no C(28) C(29) C(30) 118.7(3) . . . yes C(28) C(29) H(29) 120.6 . . . no C(30) C(29) H(29) 120.6 . . . no N(7) C(30) C(29) 122.0(3) . . . yes N(7) C(30) H(30) 119.0 . . . no C(29) C(30) H(30) 119.0 . . . no N(5) C(31) C(32) 108.3(3) . . . yes N(5) C(31) H(31) 109.8 . . . no N(5) C(31) H(32) 109.8 . . . no C(32) C(31) H(31) 109.8 . . . no C(32) C(31) H(32) 109.8 . . . no H(31) C(31) H(32) 109.5 . . . no N(8) C(32) C(31) 114.3(3) . . . yes N(8) C(32) C(33) 122.1(3) . . . yes C(31) C(32) C(33) 123.6(3) . . . yes C(32) C(33) C(34) 118.7(3) . . . yes C(32) C(33) H(33) 120.6 . . . no C(34) C(33) H(33) 120.6 . . . no C(33) C(34) C(35) 119.2(3) . . . yes C(33) C(34) H(34) 120.4 . . . no C(35) C(34) H(34) 120.4 . . . no C(34) C(35) C(36) 118.9(3) . . . yes C(34) C(35) H(35) 120.5 . . . no C(36) C(35) H(35) 120.5 . . . no N(8) C(36) C(35) 122.3(3) . . . yes N(8) C(36) H(36) 118.9 . . . no C(35) C(36) H(36) 118.9 . . . no O(7) C(37) H(37) 109.5 . . . no O(7) C(37) H(38) 109.5 . . . no O(7) C(37) H(39) 109.5 . . . no H(37) C(37) H(38) 109.5 . . . no H(37) C(37) H(39) 109.5 . . . no H(38) C(37) H(39) 109.5 . . . no #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[V(O)2(tpa)](PF6) _database_code_depnum_ccdc_archive 'CCDC 250594' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H18 F6 N4 O2 P V ' _chemical_formula_moiety ? _chemical_formula_weight 518.27 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_Int_Tables_number 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 12.441(4) _cell_length_b 11.619(3) _cell_length_c 15.152(4) _cell_angle_alpha 90 _cell_angle_beta 111.914(4) _cell_angle_gamma 90 _cell_volume 2032(1) _cell_formula_units_Z 4 _cell_measurement_reflns_used 7283 _cell_measurement_theta_min 3.3 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.28 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.645 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7933 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 153.1500 _diffrn_source_power 2.5000 _diffrn_source_voltage 50.0000 _diffrn_source_current 50.0000 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6199 _diffrn_measurement_method dtintegrate.ref _diffrn_number_total 12129 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/detI 0.0725 _diffrn_reflns_theta_full 27.4835 _diffrn_measured_fraction_theta_max 27.4835 _diffrn_measured_fraction_theta_full 94.6000 _diffrn_reflns_theta_min 3.2751 _diffrn_reflns_theta_max 27.4835 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 360 Slice: -76.0000 - 104.0000 Image width: 0.5000 Exp time: 30.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 40.6759 2theta: 14.0254 scan: Number of images: 120 Slice: -16.0000 - 44.0000 Image width: 0.5000 Exp time: 30.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 40.6759 2theta: 14.0254 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using all the reflections measured. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4394 _reflns_number_gt 3824 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.1042 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4394 _refine_ls_number_parameters 361 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0006 _refine_diff_density_max 0.26 _refine_diff_density_min -0.33 _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 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) ; V V 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;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 0.91896(3) 0.73159(3) 0.17135(2) 0.01672(9) Uani 1.00 d . . . P(1) P 1.43892(5) 0.91483(5) 0.68883(4) 0.0245(1) Uani 1.00 d . . . F(1) F 1.4846(1) 0.9356(1) 0.60501(10) 0.0442(4) Uani 1.00 d . . . F(2) F 1.5565(1) 0.8513(1) 0.7485(1) 0.0494(5) Uani 1.00 d . . . F(3) F 1.3926(1) 0.8969(1) 0.7736(1) 0.0447(4) Uani 1.00 d . . . F(4) F 1.3195(1) 0.9796(1) 0.62867(9) 0.0423(4) Uani 1.00 d . . . F(5) F 1.4929(1) 1.0353(1) 0.7349(1) 0.0441(4) Uani 1.00 d . . . F(6) F 1.3821(1) 0.7965(1) 0.6421(1) 0.0606(5) Uani 1.00 d . . . O(1) O 0.9668(1) 0.6684(1) 0.0972(1) 0.0268(4) Uani 1.00 d . . . O(2) O 0.9154(1) 0.6354(1) 0.24848(10) 0.0237(4) Uani 1.00 d . . . N(1) N 0.8614(1) 0.8694(1) 0.2499(1) 0.0165(4) Uani 1.00 d . . . N(2) N 0.7393(1) 0.7379(1) 0.0956(1) 0.0194(4) Uani 1.00 d . . . N(3) N 0.8919(1) 0.8988(1) 0.0831(1) 0.0182(4) Uani 1.00 d . . . N(4) N 1.0715(1) 0.8094(1) 0.2630(1) 0.0189(4) Uani 1.00 d . . . C(1) C 0.7447(2) 0.8266(2) 0.2406(1) 0.0206(5) Uani 1.00 d . . . C(2) C 0.6787(2) 0.7991(2) 0.1378(1) 0.0195(5) Uani 1.00 d . . . C(3) C 0.5667(2) 0.8344(2) 0.0867(2) 0.0254(5) Uani 1.00 d . . . C(4) C 0.5157(2) 0.8050(2) -0.0086(2) 0.0304(6) Uani 1.00 d . . . C(5) C 0.5758(2) 0.7387(2) -0.0499(2) 0.0286(5) Uani 1.00 d . . . C(6) C 0.6875(2) 0.7072(2) 0.0039(1) 0.0237(5) Uani 1.00 d . . . C(7) C 0.8549(2) 0.9882(2) 0.2121(1) 0.0189(5) Uani 1.00 d . . . C(8) C 0.8467(2) 0.9897(2) 0.1108(1) 0.0176(4) Uani 1.00 d . . . C(9) C 0.7971(2) 1.0804(2) 0.0501(2) 0.0258(5) Uani 1.00 d . . . C(10) C 0.7927(2) 1.0763(2) -0.0423(2) 0.0338(6) Uani 1.00 d . . . C(11) C 0.8409(2) 0.9838(2) -0.0711(2) 0.0326(6) Uani 1.00 d . . . C(12) C 0.8900(2) 0.8977(2) -0.0065(1) 0.0252(5) Uani 1.00 d . . . C(13) C 0.9493(2) 0.8638(2) 0.3476(1) 0.0232(5) Uani 1.00 d . . . C(14) C 1.0672(2) 0.8635(2) 0.3406(1) 0.0209(5) Uani 1.00 d . . . C(15) C 1.1648(2) 0.9135(2) 0.4076(1) 0.0270(5) Uani 1.00 d . . . C(16) C 1.2684(2) 0.9106(2) 0.3934(2) 0.0310(5) Uani 1.00 d . . . C(17) C 1.2728(2) 0.8566(2) 0.3136(2) 0.0290(6) Uani 1.00 d . . . C(18) C 1.1737(2) 0.8053(2) 0.2504(1) 0.0229(5) Uani 1.00 d . . . H(1) H 0.757(2) 0.754(2) 0.278(1) 0.015(5) Uiso 1.00 calc . . . H(2) H 0.704(2) 0.882(2) 0.261(2) 0.028(6) Uiso 1.00 calc . . . H(3) H 0.531(2) 0.882(2) 0.119(2) 0.038(7) Uiso 1.00 calc . . . H(4) H 0.443(2) 0.834(2) -0.041(2) 0.030(6) Uiso 1.00 calc . . . H(5) H 0.544(2) 0.720(2) -0.112(2) 0.023(6) Uiso 1.00 calc . . . H(6) H 0.731(2) 0.664(2) -0.017(2) 0.027(6) Uiso 1.00 calc . . . H(7) H 0.790(2) 1.030(2) 0.217(1) 0.021(5) Uiso 1.00 calc . . . H(8) H 0.925(2) 1.027(2) 0.248(1) 0.020(5) Uiso 1.00 calc . . . H(9) H 0.765(2) 1.143(2) 0.074(2) 0.023(5) Uiso 1.00 calc . . . H(10) H 0.762(2) 1.137(2) -0.081(2) 0.038(7) Uiso 1.00 calc . . . H(11) H 0.838(2) 0.971(2) -0.132(2) 0.042(7) Uiso 1.00 calc . . . H(12) H 0.929(2) 0.836(2) -0.021(2) 0.027(6) Uiso 1.00 calc . . . H(13) H 0.945(2) 0.925(2) 0.382(2) 0.031(6) Uiso 1.00 calc . . . H(14) H 0.942(2) 0.798(2) 0.375(2) 0.021(5) Uiso 1.00 calc . . . H(15) H 1.162(2) 0.953(2) 0.461(2) 0.029(6) Uiso 1.00 calc . . . H(16) H 1.337(2) 0.944(2) 0.439(2) 0.027(6) Uiso 1.00 calc . . . H(17) H 1.341(2) 0.857(2) 0.302(2) 0.037(7) Uiso 1.00 calc . . . H(18) H 1.174(2) 0.764(2) 0.195(2) 0.017(5) 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) 0.0169(2) 0.0135(2) 0.0188(2) 0.0013(1) 0.0056(1) -0.0009(1) P(1) 0.0272(3) 0.0228(3) 0.0265(3) 0.0036(2) 0.0133(2) 0.0006(2) F(1) 0.0570(9) 0.0527(9) 0.0329(7) 0.0021(7) 0.0284(7) -0.0012(6) F(2) 0.0392(8) 0.065(1) 0.0488(9) 0.0274(7) 0.0224(7) 0.0156(7) F(3) 0.0449(8) 0.0552(9) 0.0471(9) 0.0178(7) 0.0325(7) 0.0213(7) F(4) 0.0415(8) 0.0486(9) 0.0293(7) 0.0177(6) 0.0044(6) -0.0021(6) F(5) 0.0473(9) 0.0401(8) 0.0496(9) -0.0109(6) 0.0235(7) -0.0197(6) F(6) 0.0551(10) 0.0315(8) 0.106(1) -0.0097(7) 0.0423(10) -0.0253(9) O(1) 0.0324(8) 0.0209(7) 0.0298(8) 0.0061(6) 0.0147(6) -0.0025(6) O(2) 0.0226(7) 0.0184(7) 0.0296(8) 0.0001(5) 0.0092(6) 0.0033(5) N(1) 0.0167(7) 0.0174(8) 0.0161(7) -0.0022(6) 0.0068(6) -0.0006(6) N(2) 0.0179(8) 0.0166(8) 0.0219(8) -0.0020(6) 0.0055(6) -0.0016(6) N(3) 0.0198(8) 0.0176(8) 0.0183(8) 0.0005(6) 0.0084(6) -0.0011(6) N(4) 0.0176(7) 0.0186(8) 0.0188(8) -0.0002(6) 0.0048(6) 0.0044(6) C(1) 0.0195(9) 0.0220(10) 0.0243(10) -0.0024(7) 0.0127(8) -0.0016(8) C(2) 0.0182(9) 0.0171(9) 0.0250(10) -0.0042(7) 0.0103(7) 0.0008(7) C(3) 0.0186(9) 0.028(1) 0.032(1) -0.0008(8) 0.0113(8) 0.0007(8) C(4) 0.0156(10) 0.039(1) 0.032(1) -0.0007(9) 0.0035(8) 0.0029(9) C(5) 0.024(1) 0.033(1) 0.024(1) -0.0068(8) 0.0028(8) -0.0028(8) C(6) 0.0258(10) 0.0197(10) 0.025(1) -0.0035(8) 0.0087(8) -0.0058(7) C(7) 0.0210(9) 0.0154(9) 0.0209(9) 0.0001(7) 0.0085(8) -0.0026(7) C(8) 0.0159(8) 0.0155(9) 0.0227(9) -0.0030(7) 0.0087(7) -0.0014(7) C(9) 0.028(1) 0.020(1) 0.034(1) 0.0052(8) 0.0163(9) 0.0043(8) C(10) 0.038(1) 0.032(1) 0.033(1) 0.0093(10) 0.016(1) 0.0161(9) C(11) 0.040(1) 0.039(1) 0.023(1) 0.0039(10) 0.0166(10) 0.0071(9) C(12) 0.031(1) 0.026(1) 0.0219(10) 0.0014(8) 0.0140(9) -0.0018(8) C(13) 0.026(1) 0.027(1) 0.0162(9) -0.0022(8) 0.0079(8) -0.0009(8) C(14) 0.0211(9) 0.0193(9) 0.0181(9) 0.0008(7) 0.0026(7) 0.0047(7) C(15) 0.026(1) 0.024(1) 0.022(1) -0.0002(8) -0.0013(8) 0.0003(8) C(16) 0.0212(10) 0.023(1) 0.036(1) -0.0025(8) -0.0038(9) 0.0047(8) C(17) 0.0186(10) 0.026(1) 0.040(1) 0.0010(8) 0.0072(9) 0.0109(9) C(18) 0.0197(9) 0.024(1) 0.025(1) 0.0031(8) 0.0085(8) 0.0089(8) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _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) 1.630(1) . . yes V(1) O(2) 1.629(1) . . yes V(1) N(1) 2.264(2) . . yes V(1) N(2) 2.099(2) . . yes V(1) N(3) 2.311(2) . . yes V(1) N(4) 2.093(2) . . yes P(1) F(1) 1.591(1) . . yes P(1) F(2) 1.586(2) . . yes P(1) F(3) 1.606(1) . . yes P(1) F(4) 1.610(1) . . yes P(1) F(5) 1.596(1) . . yes P(1) F(6) 1.586(2) . . yes N(1) C(1) 1.490(2) . . yes N(1) C(7) 1.485(2) . . yes N(1) C(13) 1.477(2) . . yes N(2) C(2) 1.358(2) . . yes N(2) C(6) 1.344(3) . . yes N(3) C(8) 1.336(2) . . yes N(3) C(12) 1.349(2) . . yes N(4) C(14) 1.352(3) . . yes N(4) C(18) 1.355(2) . . yes C(1) C(2) 1.498(3) . . yes C(1) H(1) 1.00(2) . . no C(1) H(2) 0.93(2) . . no C(2) C(3) 1.381(3) . . yes C(3) C(4) 1.386(3) . . yes C(3) H(3) 0.95(3) . . no C(4) C(5) 1.375(3) . . yes C(4) H(4) 0.92(3) . . no C(5) C(6) 1.373(3) . . yes C(5) H(5) 0.90(2) . . no C(6) H(6) 0.88(2) . . no C(7) C(8) 1.499(3) . . yes C(7) H(7) 0.96(2) . . no C(7) H(8) 0.95(2) . . no C(8) C(9) 1.384(3) . . yes C(9) C(10) 1.381(3) . . yes C(9) H(9) 0.96(2) . . no C(10) C(11) 1.379(3) . . yes C(10) H(10) 0.91(3) . . no C(11) C(12) 1.373(3) . . yes C(11) H(11) 0.92(3) . . no C(12) H(12) 0.94(2) . . no C(13) C(14) 1.510(3) . . yes C(13) H(13) 0.89(3) . . no C(13) H(14) 0.89(2) . . no C(14) C(15) 1.387(3) . . yes C(15) C(16) 1.385(3) . . yes C(15) H(15) 0.95(2) . . no C(16) C(17) 1.381(3) . . yes C(16) H(16) 0.95(2) . . no C(17) C(18) 1.382(3) . . yes C(17) H(17) 0.93(3) . . no C(18) H(18) 0.97(2) . . 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) O(2) 107.49(7) . . . yes O(1) V(1) N(1) 161.70(6) . . . yes O(1) V(1) N(2) 103.14(7) . . . yes O(1) V(1) N(3) 89.49(6) . . . yes O(1) V(1) N(4) 100.23(7) . . . yes O(2) V(1) N(1) 90.52(6) . . . yes O(2) V(1) N(2) 96.19(7) . . . yes O(2) V(1) N(3) 162.66(6) . . . yes O(2) V(1) N(4) 94.63(6) . . . yes N(1) V(1) N(2) 77.38(6) . . . yes N(1) V(1) N(3) 72.76(5) . . . yes N(1) V(1) N(4) 74.48(6) . . . yes N(2) V(1) N(3) 76.04(6) . . . yes N(2) V(1) N(4) 149.87(6) . . . yes N(3) V(1) N(4) 85.47(6) . . . yes F(1) P(1) F(2) 89.86(8) . . . yes F(1) P(1) F(3) 178.71(8) . . . yes F(1) P(1) F(4) 90.32(8) . . . yes F(1) P(1) F(5) 89.95(8) . . . yes F(1) P(1) F(6) 90.43(9) . . . yes F(2) P(1) F(3) 90.80(8) . . . yes F(2) P(1) F(4) 179.76(8) . . . yes F(2) P(1) F(5) 90.62(9) . . . yes F(2) P(1) F(6) 90.78(9) . . . yes F(3) P(1) F(4) 89.01(8) . . . yes F(3) P(1) F(5) 88.94(8) . . . yes F(3) P(1) F(6) 90.66(9) . . . yes F(4) P(1) F(5) 89.23(8) . . . yes F(4) P(1) F(6) 89.37(9) . . . yes F(5) P(1) F(6) 178.55(9) . . . yes V(1) N(1) C(1) 101.7(1) . . . yes V(1) N(1) C(7) 115.9(1) . . . yes V(1) N(1) C(13) 103.6(1) . . . yes C(1) N(1) C(7) 111.2(1) . . . yes C(1) N(1) C(13) 114.3(1) . . . yes C(7) N(1) C(13) 109.9(1) . . . yes V(1) N(2) C(2) 115.2(1) . . . yes V(1) N(2) C(6) 123.9(1) . . . yes C(2) N(2) C(6) 119.3(2) . . . yes V(1) N(3) C(8) 118.0(1) . . . yes V(1) N(3) C(12) 121.3(1) . . . yes C(8) N(3) C(12) 118.2(2) . . . yes V(1) N(4) C(14) 117.2(1) . . . yes V(1) N(4) C(18) 123.9(1) . . . yes C(14) N(4) C(18) 118.8(2) . . . yes N(1) C(1) C(2) 107.9(1) . . . yes N(1) C(1) H(1) 107(1) . . . no N(1) C(1) H(2) 111(1) . . . no C(2) C(1) H(1) 108(1) . . . no C(2) C(1) H(2) 109(1) . . . no H(1) C(1) H(2) 112(1) . . . no N(2) C(2) C(1) 114.6(2) . . . yes N(2) C(2) C(3) 120.9(2) . . . yes C(1) C(2) C(3) 124.5(2) . . . yes C(2) C(3) C(4) 119.0(2) . . . yes C(2) C(3) H(3) 116(1) . . . no C(4) C(3) H(3) 124(1) . . . no C(3) C(4) C(5) 119.8(2) . . . yes C(3) C(4) H(4) 116(1) . . . no C(5) C(4) H(4) 123(1) . . . no C(4) C(5) C(6) 118.7(2) . . . yes C(4) C(5) H(5) 120(1) . . . no C(6) C(5) H(5) 120(1) . . . no N(2) C(6) C(5) 122.1(2) . . . yes N(2) C(6) H(6) 113(1) . . . no C(5) C(6) H(6) 124(1) . . . no N(1) C(7) C(8) 112.3(1) . . . yes N(1) C(7) H(7) 110(1) . . . no N(1) C(7) H(8) 108(1) . . . no C(8) C(7) H(7) 109(1) . . . no C(8) C(7) H(8) 106(1) . . . no H(7) C(7) H(8) 108(1) . . . no N(3) C(8) C(7) 115.9(2) . . . yes N(3) C(8) C(9) 121.9(2) . . . yes C(7) C(8) C(9) 122.2(2) . . . yes C(8) C(9) C(10) 119.1(2) . . . yes C(8) C(9) H(9) 117(1) . . . no C(10) C(9) H(9) 123(1) . . . no C(9) C(10) C(11) 119.4(2) . . . yes C(9) C(10) H(10) 118(1) . . . no C(11) C(10) H(10) 121(1) . . . no C(10) C(11) C(12) 118.2(2) . . . yes C(10) C(11) H(11) 125(1) . . . no C(12) C(11) H(11) 116(1) . . . no N(3) C(12) C(11) 123.1(2) . . . yes N(3) C(12) H(12) 115(1) . . . no C(11) C(12) H(12) 121(1) . . . no N(1) C(13) C(14) 107.8(2) . . . yes N(1) C(13) H(13) 111(1) . . . no N(1) C(13) H(14) 109(1) . . . no C(14) C(13) H(13) 108(1) . . . no C(14) C(13) H(14) 107(1) . . . no H(13) C(13) H(14) 111(2) . . . no N(4) C(14) C(13) 114.7(2) . . . yes N(4) C(14) C(15) 121.6(2) . . . yes C(13) C(14) C(15) 123.8(2) . . . yes C(14) C(15) C(16) 119.2(2) . . . yes C(14) C(15) H(15) 121(1) . . . no C(16) C(15) H(15) 118(1) . . . no C(15) C(16) C(17) 119.3(2) . . . yes C(15) C(16) H(16) 120(1) . . . no C(17) C(16) H(16) 120(1) . . . no C(16) C(17) C(18) 119.1(2) . . . yes C(16) C(17) H(17) 119(1) . . . no C(18) C(17) H(17) 121(1) . . . no N(4) C(18) C(17) 121.9(2) . . . yes N(4) C(18) H(18) 116(1) . . . no C(17) C(18) H(18) 121(1) . . . no #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #===END data_[{V(tpa)Cl}2(O)](PF6)2 _database_code_depnum_ccdc_archive 'CCDC 250595' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C36 H36 Cl2 F12 N8 O P2 V2 ' _chemical_formula_moiety ? _chemical_formula_weight 1059.45 _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 8.485(3) _cell_length_b 11.126(3) _cell_length_c 12.709(3) _cell_angle_alpha 64.488(10) _cell_angle_beta 71.58(1) _cell_angle_gamma 88.72(2) _cell_volume 1018.2(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3861 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 153.1 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.05 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.768 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.7170 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 153.1500 _diffrn_source_power 2.5000 _diffrn_source_voltage 50.0000 _diffrn_source_current 50.0000 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type Molybdenum _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6199 _diffrn_number_total 5777 _diffrn_reflns_av_R_equivalents 0.0120 _diffrn_reflns_av_sigmaI/detI 0.0326 _diffrn_reflns_theta_full 27.4835 _diffrn_measured_fraction_theta_max 27.4835 _diffrn_measured_fraction_theta_full 87.2000 _diffrn_reflns_theta_min 3.5680 _diffrn_reflns_theta_max 27.4835 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 360 Slice: -76.0000 - 104.0000 Image width: 0.5000 Exp time: 50.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 40.6489 2theta: 14.0276 scan: Number of images: 120 Slice: -16.0000 - 44.0000 Image width: 0.5000 Exp time: 50.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 40.6489 2theta: 14.0276 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3-circle ; _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using all the reflections measured. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4047 _reflns_number_gt 3631 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1178 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 4047 _refine_ls_number_parameters 286 _refine_ls_goodness_of_fit_ref 1.566 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.05500(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0006 _refine_diff_density_max 0.50 _refine_diff_density_min -0.26 _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 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) ; V V 0.300 0.529 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; P P 0.102 0.094 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;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) ; #------------------------------------------------------------------------------ # 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 0.53255(4) 0.04572(3) 0.11168(3) 0.0161(1) Uani 1.00 d . . . Cl(1) Cl 0.81740(7) 0.13807(6) 0.01290(6) 0.0290(2) Uani 1.00 d . . . P(1) P 1.05351(7) 0.37775(6) 0.33918(6) 0.0225(2) Uani 1.00 d . . . F(1) F 1.1129(2) 0.3277(2) 0.4572(1) 0.0407(5) Uani 1.00 d . . . F(2) F 1.2388(2) 0.3832(2) 0.2530(2) 0.0421(4) Uani 1.00 d . . . F(3) F 0.9894(2) 0.4267(2) 0.2235(1) 0.0377(4) Uani 1.00 d . . . F(4) F 0.8645(2) 0.3699(1) 0.4263(1) 0.0300(4) Uani 1.00 d . . . F(5) F 1.0127(2) 0.2243(1) 0.3671(1) 0.0344(4) Uani 1.00 d . . . F(6) F 1.0912(2) 0.5301(2) 0.3120(2) 0.0473(5) Uani 1.00 d . . . O(1) O 0.5000 0.0000 0.0000 0.0157(5) Uani 1.00 d S . . N(1) N 0.2810(2) -0.0369(2) 0.2362(2) 0.0178(4) Uani 1.00 d . . . N(2) N 0.4146(2) 0.2180(2) 0.0467(2) 0.0174(4) Uani 1.00 d . . . N(3) N 0.5187(2) 0.1018(2) 0.2611(2) 0.0183(4) Uani 1.00 d . . . N(4) N 0.5666(2) -0.1517(2) 0.2204(2) 0.0196(5) Uani 1.00 d . . . C(1) C 0.1731(3) 0.0429(2) 0.1666(2) 0.0222(6) Uani 1.00 d . . . C(2) C 0.2461(3) 0.1898(2) 0.0870(2) 0.0199(5) Uani 1.00 d . . . C(3) C 0.1486(3) 0.2889(2) 0.0494(2) 0.0251(6) Uani 1.00 d . . . C(4) C 0.2244(3) 0.4190(2) -0.0337(2) 0.0287(6) Uani 1.00 d . . . C(5) C 0.3960(3) 0.4472(2) -0.0755(2) 0.0247(6) Uani 1.00 d . . . C(6) C 0.4874(3) 0.3448(2) -0.0330(2) 0.0211(5) Uani 1.00 d . . . C(7) C 0.2452(3) -0.0307(2) 0.3566(2) 0.0245(6) Uani 1.00 d . . . C(8) C 0.3707(3) 0.0635(2) 0.3547(2) 0.0181(5) Uani 1.00 d . . . C(9) C 0.3359(3) 0.1037(2) 0.4477(2) 0.0232(6) Uani 1.00 d . . . C(10) C 0.4573(3) 0.1862(2) 0.4455(2) 0.0275(6) Uani 1.00 d . . . C(11) C 0.6099(3) 0.2259(2) 0.3508(2) 0.0271(6) Uani 1.00 d . . . C(12) C 0.6367(3) 0.1825(2) 0.2605(2) 0.0233(6) Uani 1.00 d . . . C(13) C 0.2665(3) -0.1807(2) 0.2600(2) 0.0198(5) Uani 1.00 d . . . C(14) C 0.4238(3) -0.2393(2) 0.2788(2) 0.0197(5) Uani 1.00 d . . . C(15) C 0.4247(3) -0.3760(2) 0.3451(2) 0.0244(6) Uani 1.00 d . . . C(16) C 0.5773(3) -0.4227(2) 0.3484(2) 0.0303(6) Uani 1.00 d . . . C(17) C 0.7237(3) -0.3333(3) 0.2890(2) 0.0314(7) Uani 1.00 d . . . C(18) C 0.7134(3) -0.1988(3) 0.2261(2) 0.0268(6) Uani 1.00 d . . . H(1) H 0.1602 0.0059 0.1145 0.0266 Uiso 1.00 calc . . . H(2) H 0.0666 0.0373 0.2243 0.0266 Uiso 1.00 calc . . . H(3) H 0.0299 0.2684 0.0802 0.0302 Uiso 1.00 calc . . . H(4) H 0.1583 0.4881 -0.0616 0.0344 Uiso 1.00 calc . . . H(5) H 0.4503 0.5357 -0.1327 0.0297 Uiso 1.00 calc . . . H(6) H 0.6059 0.3642 -0.0607 0.0253 Uiso 1.00 calc . . . H(7) H 0.1381 -0.0024 0.3773 0.0294 Uiso 1.00 calc . . . H(8) H 0.2438 -0.1183 0.4184 0.0294 Uiso 1.00 calc . . . H(9) H 0.2300 0.0750 0.5121 0.0278 Uiso 1.00 calc . . . H(10) H 0.4361 0.2152 0.5084 0.0330 Uiso 1.00 calc . . . H(11) H 0.6954 0.2823 0.3476 0.0325 Uiso 1.00 calc . . . H(12) H 0.7419 0.2102 0.1955 0.0279 Uiso 1.00 calc . . . H(13) H 0.1726 -0.2303 0.3322 0.0238 Uiso 1.00 calc . . . H(14) H 0.2517 -0.1862 0.1910 0.0238 Uiso 1.00 calc . . . H(15) H 0.3234 -0.4364 0.3873 0.0293 Uiso 1.00 calc . . . H(16) H 0.5811 -0.5162 0.3916 0.0363 Uiso 1.00 calc . . . H(17) H 0.8285 -0.3640 0.2915 0.0377 Uiso 1.00 calc . . . H(18) H 0.8132 -0.1368 0.1851 0.0321 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) 0.0126(2) 0.0165(2) 0.0173(2) 0.0009(1) -0.0041(1) -0.0065(1) Cl(1) 0.0221(3) 0.0347(3) 0.0315(3) -0.0015(2) -0.0082(2) -0.0163(3) P(1) 0.0175(3) 0.0214(3) 0.0246(3) 0.0031(2) -0.0076(2) -0.0065(2) F(1) 0.0426(10) 0.052(1) 0.0405(9) 0.0242(8) -0.0279(8) -0.0238(8) F(2) 0.0181(8) 0.0488(10) 0.0383(9) 0.0037(7) -0.0010(6) -0.0068(7) F(3) 0.0347(9) 0.0483(10) 0.0271(8) 0.0114(7) -0.0147(6) -0.0115(7) F(4) 0.0222(7) 0.0368(8) 0.0309(8) 0.0085(6) -0.0055(6) -0.0176(7) F(5) 0.0342(8) 0.0256(7) 0.0387(9) 0.0037(6) -0.0061(7) -0.0147(7) F(6) 0.0377(9) 0.0259(8) 0.080(1) 0.0031(7) -0.0286(9) -0.0194(8) O(1) 0.0102(10) 0.0162(10) 0.0168(10) 0.0001(7) -0.0027(8) -0.0051(8) N(1) 0.0165(9) 0.0171(9) 0.0166(8) -0.0012(7) -0.0033(7) -0.0061(7) N(2) 0.0145(9) 0.0180(8) 0.0194(9) 0.0017(7) -0.0051(7) -0.0086(7) N(3) 0.0157(9) 0.0177(8) 0.0202(9) 0.0018(7) -0.0064(7) -0.0072(7) N(4) 0.0189(10) 0.0201(9) 0.0202(9) 0.0052(7) -0.0079(7) -0.0087(7) C(1) 0.014(1) 0.020(1) 0.029(1) 0.0000(8) -0.0062(9) -0.0092(9) C(2) 0.018(1) 0.023(1) 0.021(1) 0.0022(8) -0.0060(8) -0.0118(9) C(3) 0.018(1) 0.028(1) 0.029(1) 0.0061(9) -0.0087(9) -0.0122(10) C(4) 0.030(1) 0.026(1) 0.028(1) 0.0112(10) -0.012(1) -0.009(1) C(5) 0.030(1) 0.019(1) 0.022(1) 0.0018(9) -0.0076(9) -0.0060(9) C(6) 0.022(1) 0.019(1) 0.021(1) 0.0009(8) -0.0060(8) -0.0085(9) C(7) 0.021(1) 0.027(1) 0.020(1) -0.0046(9) -0.0001(9) -0.0112(9) C(8) 0.017(1) 0.0164(10) 0.018(1) 0.0037(8) -0.0067(8) -0.0050(8) C(9) 0.023(1) 0.025(1) 0.022(1) 0.0071(9) -0.0081(9) -0.0106(9) C(10) 0.035(1) 0.029(1) 0.029(1) 0.012(1) -0.017(1) -0.018(1) C(11) 0.028(1) 0.027(1) 0.034(1) 0.0030(9) -0.016(1) -0.016(1) C(12) 0.019(1) 0.025(1) 0.029(1) 0.0029(9) -0.0108(9) -0.0127(10) C(13) 0.017(1) 0.0171(10) 0.021(1) -0.0018(8) -0.0040(8) -0.0068(8) C(14) 0.026(1) 0.019(1) 0.0148(10) 0.0028(8) -0.0076(8) -0.0074(8) C(15) 0.035(1) 0.019(1) 0.019(1) 0.0030(9) -0.0092(9) -0.0078(9) C(16) 0.044(2) 0.023(1) 0.024(1) 0.011(1) -0.011(1) -0.0101(10) C(17) 0.031(1) 0.034(1) 0.031(1) 0.018(1) -0.014(1) -0.015(1) C(18) 0.024(1) 0.030(1) 0.028(1) 0.0088(10) -0.0121(10) -0.013(1) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SHELXS97 _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) 2.3570(9) . . yes V(1) O(1) 1.7960(3) . . yes V(1) N(1) 2.146(2) . . yes V(1) N(2) 2.105(2) . . yes V(1) N(3) 2.211(2) . . yes V(1) N(4) 2.104(2) . . yes P(1) F(1) 1.599(2) . . yes P(1) F(2) 1.592(2) . . yes P(1) F(3) 1.599(2) . . yes P(1) F(4) 1.615(2) . . yes P(1) F(5) 1.609(2) . . yes P(1) F(6) 1.595(2) . . yes N(1) C(1) 1.486(3) . . yes N(1) C(7) 1.495(3) . . yes N(1) C(13) 1.496(3) . . yes N(2) C(2) 1.351(3) . . yes N(2) C(6) 1.346(3) . . yes N(3) C(8) 1.347(3) . . yes N(3) C(12) 1.355(3) . . yes N(4) C(14) 1.353(3) . . yes N(4) C(18) 1.352(3) . . yes C(1) C(2) 1.518(3) . . yes C(1) H(1) 0.950 . . no C(1) H(2) 0.950 . . no C(2) C(3) 1.372(3) . . yes C(3) C(4) 1.386(3) . . yes C(3) H(3) 0.950 . . no C(4) C(5) 1.375(4) . . yes C(4) H(4) 0.950 . . no C(5) C(6) 1.373(3) . . yes C(5) H(5) 0.950 . . no C(6) H(6) 0.950 . . no C(7) C(8) 1.499(3) . . yes C(7) H(7) 0.950 . . no C(7) H(8) 0.950 . . no C(8) C(9) 1.383(3) . . yes C(9) C(10) 1.381(3) . . yes C(9) H(9) 0.950 . . no C(10) C(11) 1.380(4) . . yes C(10) H(10) 0.950 . . no C(11) C(12) 1.381(3) . . yes C(11) H(11) 0.950 . . no C(12) H(12) 0.950 . . no C(13) C(14) 1.514(3) . . yes C(13) H(13) 0.950 . . no C(13) H(14) 0.950 . . no C(14) C(15) 1.386(3) . . yes C(15) C(16) 1.390(4) . . yes C(15) H(15) 0.950 . . no C(16) C(17) 1.385(4) . . yes C(16) H(16) 0.950 . . no C(17) C(18) 1.376(4) . . yes C(17) H(17) 0.950 . . no C(18) H(18) 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 Cl(1) V(1) O(1) 100.48(2) . . . yes Cl(1) V(1) N(1) 167.39(5) . . . yes Cl(1) V(1) N(2) 101.25(5) . . . yes Cl(1) V(1) N(3) 89.96(5) . . . yes Cl(1) V(1) N(4) 97.72(5) . . . yes O(1) V(1) N(1) 91.85(5) . . . yes O(1) V(1) N(2) 89.95(5) . . . yes O(1) V(1) N(3) 168.73(5) . . . yes O(1) V(1) N(4) 91.89(5) . . . yes N(1) V(1) N(2) 81.25(7) . . . yes N(1) V(1) N(3) 77.96(7) . . . yes N(1) V(1) N(4) 79.07(7) . . . yes N(2) V(1) N(3) 83.80(7) . . . yes N(2) V(1) N(4) 160.28(7) . . . yes N(3) V(1) N(4) 90.90(7) . . . yes F(1) P(1) F(2) 90.68(9) . . . yes F(1) P(1) F(3) 178.57(9) . . . yes F(1) P(1) F(4) 89.69(8) . . . yes F(1) P(1) F(5) 90.02(9) . . . yes F(1) P(1) F(6) 90.28(9) . . . yes F(2) P(1) F(3) 90.69(9) . . . yes F(2) P(1) F(4) 178.94(9) . . . yes F(2) P(1) F(5) 89.68(9) . . . yes F(2) P(1) F(6) 91.05(10) . . . yes F(3) P(1) F(4) 88.92(8) . . . yes F(3) P(1) F(5) 89.62(9) . . . yes F(3) P(1) F(6) 90.05(10) . . . yes F(4) P(1) F(5) 89.33(8) . . . yes F(4) P(1) F(6) 89.93(9) . . . yes F(5) P(1) F(6) 179.20(9) . . . yes V(1) O(1) V(1) 180.0 . . 2_655 yes V(1) N(1) C(1) 104.7(1) . . . yes V(1) N(1) C(7) 113.2(1) . . . yes V(1) N(1) C(13) 104.7(1) . . . yes C(1) N(1) C(7) 111.7(2) . . . yes C(1) N(1) C(13) 113.1(2) . . . yes C(7) N(1) C(13) 109.1(2) . . . yes V(1) N(2) C(2) 112.7(1) . . . yes V(1) N(2) C(6) 127.9(1) . . . yes C(2) N(2) C(6) 119.2(2) . . . yes V(1) N(3) C(8) 115.8(1) . . . yes V(1) N(3) C(12) 126.2(1) . . . yes C(8) N(3) C(12) 117.5(2) . . . yes V(1) N(4) C(14) 113.3(1) . . . yes V(1) N(4) C(18) 127.1(2) . . . yes C(14) N(4) C(18) 119.1(2) . . . yes N(1) C(1) C(2) 112.6(2) . . . yes N(1) C(1) H(1) 108.7 . . . no N(1) C(1) H(2) 108.7 . . . no C(2) C(1) H(1) 108.7 . . . no C(2) C(1) H(2) 108.7 . . . no H(1) C(1) H(2) 109.5 . . . no N(2) C(2) C(1) 116.6(2) . . . yes N(2) C(2) C(3) 121.0(2) . . . yes C(1) C(2) C(3) 122.3(2) . . . yes C(2) C(3) C(4) 119.5(2) . . . yes C(2) C(3) H(3) 120.2 . . . no C(4) C(3) H(3) 120.2 . . . no C(3) C(4) C(5) 119.4(2) . . . yes C(3) C(4) H(4) 120.3 . . . no C(5) C(4) H(4) 120.3 . . . no C(4) C(5) C(6) 118.7(2) . . . yes C(4) C(5) H(5) 120.7 . . . no C(6) C(5) H(5) 120.7 . . . no N(2) C(6) C(5) 122.2(2) . . . yes N(2) C(6) H(6) 118.9 . . . no C(5) C(6) H(6) 118.9 . . . no N(1) C(7) C(8) 114.1(2) . . . yes N(1) C(7) H(7) 108.3 . . . no N(1) C(7) H(8) 108.3 . . . no C(8) C(7) H(7) 108.3 . . . no C(8) C(7) H(8) 108.3 . . . no H(7) C(7) H(8) 109.5 . . . no N(3) C(8) C(7) 116.5(2) . . . yes N(3) C(8) C(9) 122.7(2) . . . yes C(7) C(8) C(9) 120.7(2) . . . yes C(8) C(9) C(10) 119.1(2) . . . yes C(8) C(9) H(9) 120.5 . . . no C(10) C(9) H(9) 120.5 . . . no C(9) C(10) C(11) 119.0(2) . . . yes C(9) C(10) H(10) 120.5 . . . no C(11) C(10) H(10) 120.5 . . . no C(10) C(11) C(12) 119.1(2) . . . yes C(10) C(11) H(11) 120.4 . . . no C(12) C(11) H(11) 120.4 . . . no N(3) C(12) C(11) 122.6(2) . . . yes N(3) C(12) H(12) 118.7 . . . no C(11) C(12) H(12) 118.7 . . . no N(1) C(13) C(14) 110.0(2) . . . yes N(1) C(13) H(13) 109.3 . . . no N(1) C(13) H(14) 109.3 . . . no C(14) C(13) H(13) 109.3 . . . no C(14) C(13) H(14) 109.3 . . . no H(13) C(13) H(14) 109.5 . . . no N(4) C(14) C(13) 116.1(2) . . . yes N(4) C(14) C(15) 121.5(2) . . . yes C(13) C(14) C(15) 122.3(2) . . . yes C(14) C(15) C(16) 118.5(2) . . . yes C(14) C(15) H(15) 120.7 . . . no C(16) C(15) H(15) 120.7 . . . no C(15) C(16) C(17) 120.2(2) . . . yes C(15) C(16) H(16) 119.9 . . . no C(17) C(16) H(16) 119.9 . . . no C(16) C(17) C(18) 118.2(2) . . . yes C(16) C(17) H(17) 120.9 . . . no C(18) C(17) H(17) 120.9 . . . no N(4) C(18) C(17) 122.5(2) . . . yes N(4) C(18) H(18) 118.8 . . . no C(17) C(18) H(18) 118.8 . . . no #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ #------------------------------------------------------------------------------