# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Carrillo-Hermosilla, FERNANDO' 'Antiolo, Antonio' 'Romero-Fernandez, Javier' 'Alonso-Moreno, Carlos' 'Rodriguez, Ana' 'Lopez-Solera, Isabel' 'Otero, Antonio' _publ_contact_author_name 'Carrillo-Hermosilla, FERNANDO' _publ_contact_author_email Fernando.Carrillo@uclm.es _publ_section_title ; Oxo- and imido-alkoxide vanadium complexes as precatalysts for the guanylation of aromatic amines ; # Attachment '- xray_fin.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 768393' #TrackingRef '- xray_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H40 Cl4 N2 O2 V2' _chemical_formula_sum 'C26 H40 Cl4 N2 O2 V2' _chemical_formula_weight 656.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7453(19) _cell_length_b 9.890(2) _cell_length_c 21.010(5) _cell_angle_alpha 90.144(6) _cell_angle_beta 91.537(6) _cell_angle_gamma 115.928(5) _cell_volume 1633.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.923 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7205 _exptl_absorpt_correction_T_max 0.8369 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19261 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0805 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.43 _reflns_number_total 6624 _reflns_number_gt 3578 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1284P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6624 _refine_ls_number_parameters 335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1281 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.2349 _refine_ls_wR_factor_gt 0.1870 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.47392(10) 0.55372(9) 0.07070(4) 0.0536(3) Uani 1 1 d . . . Cl1 Cl 0.68984(18) 0.77725(17) 0.08151(9) 0.0837(5) Uani 1 1 d . . . Cl2 Cl 0.4983(2) 0.3881(2) 0.13402(10) 0.1067(7) Uani 1 1 d . . . O1 O 0.3636(4) 0.5004(5) -0.00647(17) 0.0731(11) Uani 1 1 d . . . N1 N 0.3290(5) 0.5850(4) 0.10842(17) 0.0479(9) Uani 1 1 d . . . C1 C 0.2047(6) 0.6126(6) 0.1371(2) 0.0513(12) Uani 1 1 d . . . C2 C 0.0852(6) 0.4983(6) 0.1749(2) 0.0582(13) Uani 1 1 d . B . C3 C -0.0328(8) 0.5332(8) 0.2041(3) 0.0793(18) Uani 1 1 d . . . H3 H -0.1167 0.4595 0.2292 0.095 Uiso 1 1 calc R . . C4 C -0.0322(8) 0.6715(9) 0.1979(3) 0.087(2) Uani 1 1 d . . . H4 H -0.1106 0.6940 0.2208 0.104 Uiso 1 1 calc R . . C5 C 0.0779(8) 0.7756(7) 0.1597(3) 0.0736(16) Uani 1 1 d . . . H5 H 0.0712 0.8684 0.1547 0.088 Uiso 1 1 calc R . . C6 C 0.2011(6) 0.7522(6) 0.1274(2) 0.0538(12) Uani 1 1 d . D . C7 C 0.0864(8) 0.3467(7) 0.1824(3) 0.0798(18) Uani 1 1 d . . . H7 H 0.1744 0.3409 0.1546 0.096 Uiso 1 1 calc R A 1 C8 C -0.104(2) 0.2199(19) 0.1582(8) 0.116(5) Uiso 0.50 1 d P B 1 H8A H -0.1177 0.2280 0.1122 0.175 Uiso 0.50 1 calc PR B 1 H8B H -0.1911 0.2372 0.1802 0.175 Uiso 0.50 1 calc PR B 1 H8C H -0.1150 0.1192 0.1680 0.175 Uiso 0.50 1 calc PR B 1 C9 C 0.122(2) 0.320(2) 0.2486(8) 0.110(6) Uiso 0.50 1 d P B 1 H9A H 0.1304 0.2249 0.2511 0.165 Uiso 0.50 1 calc PR B 1 H9B H 0.0296 0.3160 0.2752 0.165 Uiso 0.50 1 calc PR B 1 H9C H 0.2294 0.4025 0.2637 0.165 Uiso 0.50 1 calc PR B 1 C8A C 0.014(2) 0.245(2) 0.1314(8) 0.119(5) Uiso 0.50 1 d P B 2 H8A1 H 0.0217 0.1510 0.1408 0.178 Uiso 0.50 1 calc PR B 2 H8A2 H 0.0760 0.2882 0.0926 0.178 Uiso 0.50 1 calc PR B 2 H8A3 H -0.1054 0.2244 0.1250 0.178 Uiso 0.50 1 calc PR B 2 C9A C 0.034(2) 0.272(2) 0.2470(8) 0.110(6) Uiso 0.50 1 d P B 2 H9A1 H -0.0907 0.2214 0.2484 0.165 Uiso 0.50 1 calc PR B 2 H9A2 H 0.0793 0.3481 0.2810 0.165 Uiso 0.50 1 calc PR B 2 H9A3 H 0.0787 0.1974 0.2528 0.165 Uiso 0.50 1 calc PR B 2 C10 C 0.3220(8) 0.8696(6) 0.0845(3) 0.0705(16) Uani 1 1 d . . . H10 H 0.3712 0.8179 0.0564 0.085 Uiso 1 1 calc R C 1 C11 C 0.243(2) 0.9425(19) 0.0423(8) 0.090(5) Uiso 0.50 1 d P D 1 H11A H 0.1813 0.9843 0.0679 0.135 Uiso 0.50 1 calc PR D 1 H11B H 0.1634 0.8680 0.0118 0.135 Uiso 0.50 1 calc PR D 1 H11C H 0.3317 1.0235 0.0190 0.135 Uiso 0.50 1 calc PR D 1 C12 C 0.4746(18) 0.9953(15) 0.1230(6) 0.072(3) Uiso 0.50 1 d P D 1 H12A H 0.5477 1.0716 0.0936 0.109 Uiso 0.50 1 calc PR D 1 H12B H 0.5408 0.9504 0.1452 0.109 Uiso 0.50 1 calc PR D 1 H12C H 0.4306 1.0422 0.1541 0.109 Uiso 0.50 1 calc PR D 1 C11A C 0.213(3) 0.885(2) 0.0257(10) 0.119(7) Uiso 0.50 1 d P D 2 H11D H 0.1128 0.8933 0.0412 0.178 Uiso 0.50 1 calc PR D 2 H11E H 0.1773 0.7965 -0.0023 0.178 Uiso 0.50 1 calc PR D 2 H11F H 0.2828 0.9756 0.0020 0.178 Uiso 0.50 1 calc PR D 2 C12A C 0.411(2) 1.012(2) 0.1170(8) 0.109(6) Uiso 0.50 1 d P D 2 H12D H 0.3285 1.0472 0.1312 0.163 Uiso 0.50 1 calc PR D 2 H12E H 0.4899 1.0848 0.0881 0.163 Uiso 0.50 1 calc PR D 2 H12F H 0.4741 0.9998 0.1541 0.163 Uiso 0.50 1 calc PR D 2 C13 C 0.2018(7) 0.4924(9) -0.0261(3) 0.101(2) Uani 1 1 d . . . H13A H 0.1269 0.3902 -0.0412 0.151 Uiso 1 1 calc R . . H13B H 0.2171 0.5633 -0.0606 0.151 Uiso 1 1 calc R . . H13C H 0.1506 0.5184 0.0100 0.151 Uiso 1 1 calc R . . V2 V 0.96952(10) 0.06503(9) 0.43212(4) 0.0529(3) Uani 1 1 d . . . Cl3 Cl 1.0076(2) -0.0810(2) 0.36194(10) 0.0959(6) Uani 1 1 d . . . Cl4 Cl 1.1737(2) 0.29555(18) 0.43343(9) 0.0931(6) Uani 1 1 d . . . O2 O 1.1428(4) 0.0141(5) 0.49566(17) 0.0727(11) Uani 1 1 d . . . N2 N 0.8173(5) 0.0899(4) 0.39415(18) 0.0493(9) Uani 1 1 d . . . C14 C 0.6837(6) 0.1031(6) 0.3620(2) 0.0524(12) Uani 1 1 d . . . C15 C 0.5595(6) -0.0203(6) 0.3302(2) 0.0598(13) Uani 1 1 d . F . C16 C 0.4322(8) 0.0002(9) 0.2974(3) 0.0855(19) Uani 1 1 d . . . H16 H 0.3434 -0.0827 0.2759 0.103 Uiso 1 1 calc R . . C17 C 0.4332(10) 0.1397(11) 0.2956(3) 0.104(3) Uani 1 1 d . . . H17 H 0.3485 0.1531 0.2709 0.125 Uiso 1 1 calc R . . C18 C 0.5527(10) 0.2577(9) 0.3286(3) 0.090(2) Uani 1 1 d . . . H18 H 0.5481 0.3519 0.3274 0.108 Uiso 1 1 calc R . . C19 C 0.6803(7) 0.2456(7) 0.3636(3) 0.0671(15) Uani 1 1 d . H . C20 C 0.5577(7) -0.1747(7) 0.3314(3) 0.0750(16) Uani 1 1 d . . . H20 H 0.6421 -0.1797 0.3632 0.090 Uiso 1 1 calc R E 1 C21 C 0.370(2) -0.291(2) 0.3455(9) 0.096(6) Uiso 0.50 1 d P F 1 H21A H 0.2936 -0.2915 0.3105 0.144 Uiso 0.50 1 calc PR F 1 H21B H 0.3351 -0.2629 0.3853 0.144 Uiso 0.50 1 calc PR F 1 H21C H 0.3649 -0.3919 0.3494 0.144 Uiso 0.50 1 calc PR F 1 C22 C 0.564(3) -0.241(2) 0.2698(9) 0.100(6) Uiso 0.50 1 d P F 1 H22A H 0.4488 -0.2927 0.2509 0.149 Uiso 0.50 1 calc PR F 1 H22B H 0.6111 -0.3141 0.2759 0.149 Uiso 0.50 1 calc PR F 1 H22C H 0.6362 -0.1621 0.2413 0.149 Uiso 0.50 1 calc PR F 1 C21A C 0.413(2) -0.303(2) 0.3615(9) 0.104(6) Uiso 0.50 1 d P F 2 H21D H 0.3422 -0.3744 0.3284 0.156 Uiso 0.50 1 calc PR F 2 H21E H 0.3436 -0.2636 0.3843 0.156 Uiso 0.50 1 calc PR F 2 H21F H 0.4575 -0.3530 0.3916 0.156 Uiso 0.50 1 calc PR F 2 C22A C 0.618(2) -0.201(2) 0.2660(8) 0.083(5) Uiso 0.50 1 d P F 2 H22D H 0.6069 -0.3040 0.2634 0.124 Uiso 0.50 1 calc PR F 2 H22E H 0.7370 -0.1295 0.2610 0.124 Uiso 0.50 1 calc PR F 2 H22F H 0.5475 -0.1868 0.2320 0.124 Uiso 0.50 1 calc PR F 2 C23 C 0.8081(9) 0.3735(6) 0.4040(3) 0.0806(18) Uani 1 1 d . . . H23 H 0.9228 0.3773 0.3974 0.097 Uiso 1 1 calc R G 1 C24 C 0.812(2) 0.5258(18) 0.3791(8) 0.099(5) Uiso 0.50 1 d P H 1 H24A H 0.8884 0.6093 0.4068 0.149 Uiso 0.50 1 calc PR H 1 H24B H 0.6970 0.5196 0.3797 0.149 Uiso 0.50 1 calc PR H 1 H24C H 0.8527 0.5428 0.3355 0.149 Uiso 0.50 1 calc PR H 1 C25 C 0.7720(15) 0.3487(14) 0.4730(6) 0.066(3) Uiso 0.50 1 d P H 1 H25A H 0.8704 0.4192 0.4984 0.099 Uiso 0.50 1 calc PR H 1 H25B H 0.7494 0.2453 0.4836 0.099 Uiso 0.50 1 calc PR H 1 H25C H 0.6722 0.3652 0.4825 0.099 Uiso 0.50 1 calc PR H 1 C24A C 0.894(2) 0.527(2) 0.3784(9) 0.109(5) Uiso 0.50 1 d P H 2 H24D H 0.9872 0.5343 0.3516 0.163 Uiso 0.50 1 calc PR H 2 H24E H 0.9399 0.6001 0.4137 0.163 Uiso 0.50 1 calc PR H 2 H24F H 0.8121 0.5489 0.3529 0.163 Uiso 0.50 1 calc PR H 2 C25A C 0.721(3) 0.394(3) 0.4609(10) 0.143(8) Uiso 0.50 1 d P H 2 H25D H 0.8070 0.4550 0.4932 0.214 Uiso 0.50 1 calc PR H 2 H25E H 0.6492 0.2955 0.4785 0.214 Uiso 0.50 1 calc PR H 2 H25F H 0.6513 0.4447 0.4484 0.214 Uiso 0.50 1 calc PR H 2 C26 C 1.3124(7) 0.0447(9) 0.4792(3) 0.107(3) Uani 1 1 d . . . H26A H 1.3683 0.0181 0.5148 0.160 Uiso 1 1 calc R . . H26B H 1.3763 0.1519 0.4703 0.160 Uiso 1 1 calc R . . H26C H 1.3088 -0.0149 0.4414 0.160 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0495(5) 0.0568(6) 0.0620(6) -0.0026(4) 0.0084(4) 0.0297(4) Cl1 0.0611(9) 0.0669(9) 0.1185(13) 0.0019(9) 0.0129(8) 0.0233(7) Cl2 0.1047(13) 0.0986(13) 0.1481(17) 0.0390(12) 0.0327(12) 0.0716(11) O1 0.053(2) 0.114(3) 0.070(2) -0.025(2) -0.0040(17) 0.054(2) N1 0.053(2) 0.046(2) 0.051(2) 0.0014(18) 0.0104(17) 0.0274(18) C1 0.049(3) 0.059(3) 0.051(3) -0.001(2) 0.002(2) 0.029(2) C2 0.056(3) 0.069(3) 0.054(3) 0.007(3) 0.012(2) 0.031(3) C3 0.069(4) 0.104(5) 0.073(4) 0.016(4) 0.026(3) 0.044(4) C4 0.090(4) 0.134(6) 0.072(4) 0.006(4) 0.026(3) 0.081(5) C5 0.084(4) 0.086(4) 0.077(4) 0.002(3) 0.010(3) 0.062(4) C6 0.063(3) 0.055(3) 0.055(3) -0.003(2) 0.005(2) 0.036(3) C7 0.087(4) 0.076(4) 0.079(4) 0.025(3) 0.037(3) 0.036(3) C10 0.097(4) 0.049(3) 0.077(4) 0.007(3) 0.014(3) 0.043(3) C13 0.062(4) 0.177(8) 0.084(4) -0.034(5) -0.010(3) 0.072(5) V2 0.0455(5) 0.0503(5) 0.0620(6) 0.0057(4) 0.0007(4) 0.0200(4) Cl3 0.0829(11) 0.0913(12) 0.1288(15) -0.0222(10) -0.0030(10) 0.0528(10) Cl4 0.0660(9) 0.0598(9) 0.1336(15) 0.0050(9) -0.0146(9) 0.0100(7) O2 0.0444(19) 0.110(3) 0.071(2) 0.030(2) 0.0110(17) 0.039(2) N2 0.055(2) 0.041(2) 0.050(2) 0.0012(17) 0.0005(18) 0.0194(18) C14 0.059(3) 0.065(3) 0.042(3) 0.004(2) 0.004(2) 0.035(3) C15 0.055(3) 0.070(4) 0.058(3) -0.004(3) 0.002(2) 0.032(3) C16 0.075(4) 0.121(6) 0.074(4) -0.020(4) -0.023(3) 0.057(4) C17 0.098(5) 0.170(8) 0.085(5) -0.004(5) -0.020(4) 0.097(6) C18 0.114(6) 0.111(6) 0.085(5) 0.003(4) -0.003(4) 0.087(5) C19 0.085(4) 0.073(4) 0.065(3) 0.010(3) 0.015(3) 0.054(3) C20 0.067(4) 0.071(4) 0.078(4) -0.021(3) -0.017(3) 0.024(3) C23 0.100(5) 0.045(3) 0.098(5) 0.003(3) 0.012(4) 0.032(3) C26 0.053(3) 0.178(8) 0.105(5) 0.060(5) 0.027(3) 0.064(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N1 1.651(4) . ? V1 O1 1.818(4) . ? V1 Cl2 2.191(2) . ? V1 Cl1 2.1974(17) . ? V1 O1 2.212(3) 2_665 ? O1 C13 1.432(6) . ? O1 V1 2.212(3) 2_665 ? N1 C1 1.383(6) . ? C1 C6 1.409(7) . ? C1 C2 1.421(7) . ? C2 C3 1.380(7) . ? C2 C7 1.512(8) . ? C3 C4 1.373(9) . ? C4 C5 1.344(9) . ? C5 C6 1.391(7) . ? C6 C10 1.504(7) . ? C7 C8A 1.402(17) . ? C7 C9 1.465(18) . ? C7 C9A 1.530(18) . ? C7 C8 1.650(17) . ? C10 C12A 1.433(18) . ? C10 C11 1.481(17) . ? C10 C12 1.570(14) . ? C10 C11A 1.59(2) . ? V2 N2 1.643(4) . ? V2 O2 1.815(3) 2_756 ? V2 Cl3 2.1927(19) . ? V2 Cl4 2.1963(17) . ? V2 O2 2.212(3) . ? O2 C26 1.431(6) . ? O2 V2 1.815(3) 2_756 ? N2 C14 1.389(6) . ? C14 C15 1.383(7) . ? C14 C19 1.423(7) . ? C15 C16 1.383(7) . ? C15 C20 1.520(8) . ? C16 C17 1.377(10) . ? C17 C18 1.351(10) . ? C18 C19 1.369(8) . ? C19 C23 1.509(9) . ? C20 C22 1.46(2) . ? C20 C21A 1.501(19) . ? C20 C22A 1.546(18) . ? C20 C21 1.575(19) . ? C23 C24A 1.481(18) . ? C23 C25A 1.49(2) . ? C23 C25 1.491(13) . ? C23 C24 1.583(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 V1 O1 98.02(17) . . ? N1 V1 Cl2 99.80(14) . . ? O1 V1 Cl2 121.85(15) . . ? N1 V1 Cl1 99.47(14) . . ? O1 V1 Cl1 118.26(15) . . ? Cl2 V1 Cl1 112.54(8) . . ? N1 V1 O1 170.29(17) . 2_665 ? O1 V1 O1 72.29(15) . 2_665 ? Cl2 V1 O1 85.21(12) . 2_665 ? Cl1 V1 O1 86.10(12) . 2_665 ? C13 O1 V1 129.2(3) . . ? C13 O1 V1 123.1(3) . 2_665 ? V1 O1 V1 107.71(15) . 2_665 ? C1 N1 V1 177.1(3) . . ? N1 C1 C6 118.9(4) . . ? N1 C1 C2 118.4(4) . . ? C6 C1 C2 122.7(4) . . ? C3 C2 C1 116.1(5) . . ? C3 C2 C7 121.9(5) . . ? C1 C2 C7 122.0(4) . . ? C4 C3 C2 121.8(5) . . ? C5 C4 C3 120.9(5) . . ? C4 C5 C6 122.2(6) . . ? C5 C6 C1 116.1(5) . . ? C5 C6 C10 121.4(5) . . ? C1 C6 C10 122.5(4) . . ? C8A C7 C9 130.2(11) . . ? C8A C7 C2 115.9(9) . . ? C9 C7 C2 111.8(9) . . ? C8A C7 C9A 112.3(11) . . ? C9 C7 C9A 27.2(9) . . ? C2 C7 C9A 116.4(8) . . ? C8A C7 C8 42.0(8) . . ? C9 C7 C8 110.5(10) . . ? C2 C7 C8 106.4(8) . . ? C9A C7 C8 83.8(10) . . ? C12A C10 C11 87.7(10) . . ? C12A C10 C6 111.6(8) . . ? C11 C10 C6 114.9(8) . . ? C12A C10 C12 24.7(8) . . ? C11 C10 C12 108.6(9) . . ? C6 C10 C12 112.0(6) . . ? C12A C10 C11A 110.2(11) . . ? C11 C10 C11A 22.7(10) . . ? C6 C10 C11A 107.5(9) . . ? C12 C10 C11A 129.3(10) . . ? N2 V2 O2 98.00(17) . 2_756 ? N2 V2 Cl3 98.72(14) . . ? O2 V2 Cl3 119.99(15) 2_756 . ? N2 V2 Cl4 100.54(14) . . ? O2 V2 Cl4 119.90(15) 2_756 . ? Cl3 V2 Cl4 112.78(8) . . ? N2 V2 O2 170.40(16) . . ? O2 V2 O2 72.41(15) 2_756 . ? Cl3 V2 O2 85.93(12) . . ? Cl4 V2 O2 85.22(12) . . ? C26 O2 V2 129.5(3) . 2_756 ? C26 O2 V2 122.9(3) . . ? V2 O2 V2 107.59(15) 2_756 . ? C14 N2 V2 177.1(4) . . ? C15 C14 N2 119.8(4) . . ? C15 C14 C19 122.4(5) . . ? N2 C14 C19 117.8(5) . . ? C16 C15 C14 117.5(5) . . ? C16 C15 C20 120.0(5) . . ? C14 C15 C20 122.5(5) . . ? C17 C16 C15 120.5(6) . . ? C18 C17 C16 121.0(6) . . ? C17 C18 C19 121.9(6) . . ? C18 C19 C14 116.5(6) . . ? C18 C19 C23 122.6(6) . . ? C14 C19 C23 120.8(5) . . ? C22 C20 C21A 101.5(11) . . ? C22 C20 C15 116.8(9) . . ? C21A C20 C15 119.2(9) . . ? C22 C20 C22A 17.9(11) . . ? C21A C20 C22A 118.9(11) . . ? C15 C20 C22A 107.4(8) . . ? C22 C20 C21 95.4(11) . . ? C21A C20 C21 20.1(10) . . ? C15 C20 C21 106.8(8) . . ? C22A C20 C21 113.2(11) . . ? C24A C23 C25A 103.3(12) . . ? C24A C23 C25 121.1(9) . . ? C25A C23 C25 30.8(9) . . ? C24A C23 C19 120.8(9) . . ? C25A C23 C19 108.7(10) . . ? C25 C23 C19 111.4(7) . . ? C24A C23 C24 26.7(8) . . ? C25A C23 C24 86.7(11) . . ? C25 C23 C24 113.4(9) . . ? C19 C23 C24 108.4(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.520 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.156 #==========================================================END data_8 _database_code_depnum_ccdc_archive 'CCDC 768394' #TrackingRef '- xray_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H46 Cl2 N2 O4 V2' _chemical_formula_sum 'C28 H46 Cl2 N2 O4 V2' _chemical_formula_weight 647.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.727(4) _cell_length_b 28.197(3) _cell_length_c 7.648(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.565(6) _cell_angle_gamma 90.00 _cell_volume 1651.9(11) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 1285 _cell_measurement_theta_min 2.659 _cell_measurement_theta_max 19.538 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 0.760 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7930 _exptl_absorpt_correction_T_max 0.9143 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10448 _diffrn_reflns_av_R_equivalents 0.0570 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2910 _reflns_number_gt 2056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1024P)^2^+3.7528P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2910 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 0.851 _refine_ls_restrained_S_all 0.851 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.006 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.06202(7) 0.458358(19) 0.37364(7) 0.0273(2) Uani 1 1 d . . . Cl1 Cl -0.17155(11) 0.44971(3) 0.16821(12) 0.0399(3) Uani 1 1 d . . . N1 N 0.1336(3) 0.40272(10) 0.3928(4) 0.0285(6) Uani 1 1 d . . . O1 O 0.0330(3) 0.46923(8) 0.6054(3) 0.0298(5) Uani 1 1 d . . . O2 O 0.2389(3) 0.48688(8) 0.2901(3) 0.0374(6) Uani 1 1 d . . . C1 C 0.2002(4) 0.35719(12) 0.4162(4) 0.0302(8) Uani 1 1 d . . . C2 C 0.3584(5) 0.34917(13) 0.5259(5) 0.0350(8) Uani 1 1 d . . . C3 C 0.4204(5) 0.30318(14) 0.5410(5) 0.0472(10) Uani 1 1 d . . . H3 H 0.5262 0.2969 0.6158 0.057 Uiso 1 1 calc R . . C4 C 0.3333(6) 0.26627(14) 0.4509(6) 0.0534(11) Uani 1 1 d . . . H4 H 0.3801 0.2351 0.4615 0.064 Uiso 1 1 calc R . . C5 C 0.1785(5) 0.27464(13) 0.3456(6) 0.0489(11) Uani 1 1 d . . . H5 H 0.1190 0.2489 0.2843 0.059 Uiso 1 1 calc R . . C6 C 0.1067(5) 0.31939(13) 0.3261(5) 0.0357(8) Uani 1 1 d . . . C7 C 0.4615(5) 0.38844(14) 0.6237(5) 0.0422(9) Uani 1 1 d . . . H7 H 0.3955 0.4187 0.5982 0.051 Uiso 1 1 calc R . . C8 C 0.4832(6) 0.38026(16) 0.8240(6) 0.0589(12) Uani 1 1 d . . . H8A H 0.3679 0.3771 0.8631 0.088 Uiso 1 1 calc R . . H8B H 0.5447 0.4073 0.8841 0.088 Uiso 1 1 calc R . . H8C H 0.5507 0.3512 0.8527 0.088 Uiso 1 1 calc R . . C9 C 0.6402(5) 0.39396(16) 0.5596(7) 0.0641(13) Uani 1 1 d . . . H9A H 0.7139 0.3667 0.5990 0.096 Uiso 1 1 calc R . . H9B H 0.6960 0.4232 0.6083 0.096 Uiso 1 1 calc R . . H9C H 0.6250 0.3955 0.4305 0.096 Uiso 1 1 calc R . . C10 C -0.0606(5) 0.32878(13) 0.2035(5) 0.0415(9) Uani 1 1 d . . . H10 H -0.1164 0.3574 0.2490 0.050 Uiso 1 1 calc R . . C11 C -0.0157(6) 0.34088(17) 0.0228(5) 0.0591(12) Uani 1 1 d . . . H11A H 0.0675 0.3673 0.0321 0.089 Uiso 1 1 calc R . . H11B H -0.1221 0.3501 -0.0539 0.089 Uiso 1 1 calc R . . H11C H 0.0365 0.3132 -0.0272 0.089 Uiso 1 1 calc R . . C12 C -0.1921(6) 0.28847(17) 0.1975(7) 0.0751(16) Uani 1 1 d . . . H12A H -0.1440 0.2602 0.1471 0.113 Uiso 1 1 calc R . . H12B H -0.3004 0.2978 0.1243 0.113 Uiso 1 1 calc R . . H12C H -0.2166 0.2814 0.3173 0.113 Uiso 1 1 calc R . . C13 C 0.0606(5) 0.43863(13) 0.7546(5) 0.0373(9) Uani 1 1 d . . . H13A H 0.0576 0.4056 0.7149 0.056 Uiso 1 1 calc R . . H13B H -0.0313 0.4438 0.8294 0.056 Uiso 1 1 calc R . . H13C H 0.1747 0.4454 0.8222 0.056 Uiso 1 1 calc R . . C14 C 0.3926(6) 0.47145(17) 0.2332(7) 0.0589(12) Uani 1 1 d . . . H14A H 0.4919 0.4800 0.3208 0.088 Uiso 1 1 calc R . . H14B H 0.4057 0.4865 0.1202 0.088 Uiso 1 1 calc R . . H14C H 0.3888 0.4369 0.2185 0.088 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0268(3) 0.0284(3) 0.0266(3) -0.0002(2) 0.0030(2) 0.0026(2) Cl1 0.0357(5) 0.0434(5) 0.0377(5) -0.0029(4) -0.0062(4) 0.0047(4) N1 0.0263(14) 0.0306(15) 0.0278(15) -0.0015(12) 0.0011(11) 0.0014(11) O1 0.0372(13) 0.0289(12) 0.0236(12) 0.0063(10) 0.0048(10) 0.0059(10) O2 0.0376(14) 0.0326(14) 0.0431(15) 0.0052(11) 0.0090(11) 0.0000(10) C1 0.0323(18) 0.0315(18) 0.0271(18) 0.0028(14) 0.0047(15) 0.0026(14) C2 0.0329(19) 0.039(2) 0.033(2) 0.0033(16) 0.0020(15) 0.0043(15) C3 0.046(2) 0.041(2) 0.051(3) 0.0067(19) -0.0040(19) 0.0099(18) C4 0.066(3) 0.026(2) 0.065(3) 0.0013(19) 0.000(2) 0.0100(19) C5 0.059(3) 0.028(2) 0.058(3) -0.0025(18) -0.002(2) -0.0046(18) C6 0.042(2) 0.033(2) 0.032(2) 0.0009(16) 0.0044(16) -0.0055(15) C7 0.035(2) 0.040(2) 0.049(2) 0.0019(18) -0.0054(18) 0.0017(16) C8 0.056(3) 0.063(3) 0.053(3) -0.006(2) -0.012(2) 0.009(2) C9 0.038(2) 0.060(3) 0.094(4) 0.006(3) 0.004(2) -0.007(2) C10 0.046(2) 0.031(2) 0.045(2) -0.0016(17) -0.0046(17) -0.0035(16) C11 0.069(3) 0.063(3) 0.044(3) 0.007(2) 0.003(2) 0.015(2) C12 0.069(3) 0.061(3) 0.087(4) 0.011(3) -0.021(3) -0.026(3) C13 0.047(2) 0.033(2) 0.031(2) 0.0084(15) 0.0047(17) 0.0069(16) C14 0.047(2) 0.060(3) 0.074(3) 0.013(2) 0.022(2) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N1 1.663(3) . ? V1 O2 1.775(2) . ? V1 O1 1.842(2) . ? V1 O1 2.183(2) 3_566 ? V1 Cl1 2.2447(12) . ? N1 C1 1.386(4) . ? O1 C13 1.424(4) . ? O1 V1 2.183(2) 3_566 ? O2 C14 1.388(5) . ? C1 C2 1.407(5) . ? C1 C6 1.415(5) . ? C2 C3 1.382(5) . ? C2 C7 1.504(5) . ? C3 C4 1.375(6) . ? C4 C5 1.372(6) . ? C5 C6 1.379(5) . ? C6 C10 1.517(5) . ? C7 C9 1.533(6) . ? C7 C8 1.537(6) . ? C10 C11 1.507(6) . ? C10 C12 1.521(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 V1 O2 101.33(12) . . ? N1 V1 O1 98.82(12) . . ? O2 V1 O1 117.90(11) . . ? N1 V1 O1 170.69(12) . 3_566 ? O2 V1 O1 83.38(10) . 3_566 ? O1 V1 O1 71.88(10) . 3_566 ? N1 V1 Cl1 100.75(10) . . ? O2 V1 Cl1 112.54(9) . . ? O1 V1 Cl1 120.22(8) . . ? O1 V1 Cl1 84.59(7) 3_566 . ? C1 N1 V1 176.8(2) . . ? C13 O1 V1 130.2(2) . . ? C13 O1 V1 121.6(2) . 3_566 ? V1 O1 V1 108.12(10) . 3_566 ? C14 O2 V1 134.6(3) . . ? N1 C1 C2 120.3(3) . . ? N1 C1 C6 118.5(3) . . ? C2 C1 C6 121.2(3) . . ? C3 C2 C1 117.7(3) . . ? C3 C2 C7 119.6(3) . . ? C1 C2 C7 122.7(3) . . ? C4 C3 C2 121.8(4) . . ? C3 C4 C5 119.7(4) . . ? C6 C5 C4 121.9(4) . . ? C5 C6 C1 117.7(3) . . ? C5 C6 C10 121.6(3) . . ? C1 C6 C10 120.6(3) . . ? C2 C7 C9 110.9(3) . . ? C2 C7 C8 111.5(3) . . ? C9 C7 C8 110.5(3) . . ? C6 C10 C11 109.1(3) . . ? C6 C10 C12 113.6(3) . . ? C11 C10 C12 112.0(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.284 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.062 #==========================================================END data_12 _database_code_depnum_ccdc_archive 'CCDC 768395' #TrackingRef '- xray_fin.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H62 Cl2 N2 O4 V2' _chemical_formula_sum 'C36 H62 Cl2 N2 O4 V2' _chemical_formula_weight 759.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.8392(19) _cell_length_b 12.0336(19) _cell_length_c 14.851(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.638(3) _cell_angle_gamma 90.00 _cell_volume 2097.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prismatic _exptl_crystal_colour Red _exptl_crystal_size_max 0.726 _exptl_crystal_size_mid 0.562 _exptl_crystal_size_min 0.347 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.608 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.499089 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13776 _diffrn_reflns_av_R_equivalents 0.0433 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 26.60 _reflns_number_total 4245 _reflns_number_gt 2805 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.2787P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4245 _refine_ls_number_parameters 214 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1032 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.87471(4) 0.54172(4) 1.02084(3) 0.04016(16) Uani 1 1 d . . . Cl1 Cl 0.90084(7) 0.55920(7) 1.17174(4) 0.0630(2) Uani 1 1 d . . . O1 O 0.99443(14) 0.58556(14) 0.96076(11) 0.0448(4) Uani 1 1 d . . . O2 O 0.78329(15) 0.42913(14) 0.98428(12) 0.0481(5) Uani 1 1 d . . . N1 N 0.78820(17) 0.64817(17) 0.99066(12) 0.0394(5) Uani 1 1 d . . . C1 C 0.7252(2) 0.7407(2) 0.95898(18) 0.0443(6) Uani 1 1 d . . . C2 C 0.6907(2) 0.7542(2) 0.86545(19) 0.0538(7) Uani 1 1 d . . . C3 C 0.6332(3) 0.8510(3) 0.8372(3) 0.0771(10) Uani 1 1 d . . . H3 H 0.6099 0.8624 0.7756 0.093 Uiso 1 1 calc R . . C4 C 0.6102(3) 0.9302(3) 0.8986(3) 0.0890(13) Uani 1 1 d . . . H4 H 0.5721 0.9948 0.8780 0.107 Uiso 1 1 calc R . . C5 C 0.6425(3) 0.9153(3) 0.9899(3) 0.0786(11) Uani 1 1 d . . . H5 H 0.6254 0.9699 1.0303 0.094 Uiso 1 1 calc R . . C6 C 0.6998(2) 0.8209(2) 1.0231(2) 0.0549(7) Uani 1 1 d . . . C7 C 0.7109(3) 0.6670(3) 0.79597(18) 0.0668(9) Uani 1 1 d . . . H7 H 0.7598 0.6092 0.8269 0.080 Uiso 1 1 calc R . . C8 C 0.7710(3) 0.7147(4) 0.7189(2) 0.0952(13) Uani 1 1 d . . . H8A H 0.7218 0.7673 0.6846 0.143 Uiso 1 1 calc R . . H8B H 0.7886 0.6554 0.6798 0.143 Uiso 1 1 calc R . . H8C H 0.8401 0.7510 0.7443 0.143 Uiso 1 1 calc R . . C9 C 0.5980(3) 0.6129(4) 0.7560(2) 0.0946(12) Uani 1 1 d . . . H9A H 0.5616 0.5814 0.8041 0.142 Uiso 1 1 calc R . . H9B H 0.6126 0.5554 0.7142 0.142 Uiso 1 1 calc R . . H9C H 0.5490 0.6680 0.7246 0.142 Uiso 1 1 calc R . . C10 C 0.7314(3) 0.8011(3) 1.1236(2) 0.0666(9) Uani 1 1 d . . . H10 H 0.7991 0.7534 1.1305 0.080 Uiso 1 1 calc R . . C11 C 0.7629(4) 0.9050(3) 1.1785(3) 0.1185(16) Uani 1 1 d . . . H11A H 0.6962 0.9502 1.1797 0.178 Uiso 1 1 calc R . . H11B H 0.8190 0.9462 1.1513 0.178 Uiso 1 1 calc R . . H11C H 0.7934 0.8848 1.2394 0.178 Uiso 1 1 calc R . . C12 C 0.6390(4) 0.7375(4) 1.1615(3) 0.1176(16) Uani 1 1 d . . . H12A H 0.5715 0.7824 1.1576 0.176 Uiso 1 1 calc R . . H12B H 0.6639 0.7192 1.2238 0.176 Uiso 1 1 calc R . . H12C H 0.6227 0.6705 1.1271 0.176 Uiso 1 1 calc R . . C13 C 1.0097(2) 0.6893(2) 0.91656(18) 0.0510(7) Uani 1 1 d . . . H13A H 0.9398 0.7083 0.8778 0.061 Uiso 1 1 calc R . . H13B H 1.0694 0.6812 0.8782 0.061 Uiso 1 1 calc R . . C14 C 1.0408(3) 0.7830(2) 0.9839(2) 0.0679(9) Uani 1 1 d . . . H14A H 0.9805 0.7928 1.0214 0.082 Uiso 1 1 calc R . . H14B H 1.1102 0.7641 1.0233 0.082 Uiso 1 1 calc R . . C15 C 1.0582(4) 0.8900(3) 0.9341(3) 0.1232(18) Uani 1 1 d . . . H15A H 0.9877 0.9118 0.8990 0.185 Uiso 1 1 calc R . . H15B H 1.1150 0.8789 0.8944 0.185 Uiso 1 1 calc R . . H15C H 1.0830 0.9472 0.9773 0.185 Uiso 1 1 calc R . . C16 C 0.6631(2) 0.4246(3) 0.9601(2) 0.0578(8) Uani 1 1 d . . . H16A H 0.6450 0.3788 0.9063 0.069 Uiso 1 1 calc R . . H16B H 0.6340 0.4987 0.9458 0.069 Uiso 1 1 calc R . . C17 C 0.6066(3) 0.3771(3) 1.0365(2) 0.0738(9) Uani 1 1 d . . . H17A H 0.6241 0.4244 1.0894 0.089 Uiso 1 1 calc R . . H17B H 0.5247 0.3787 1.0191 0.089 Uiso 1 1 calc R . . C18 C 0.6417(3) 0.2605(3) 1.0622(3) 0.1093(15) Uani 1 1 d . . . H18A H 0.6298 0.2139 1.0094 0.164 Uiso 1 1 calc R . . H18B H 0.5970 0.2335 1.1070 0.164 Uiso 1 1 calc R . . H18C H 0.7209 0.2595 1.0868 0.164 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0282(3) 0.0532(3) 0.0385(3) 0.0054(2) 0.00230(18) 0.0024(2) Cl1 0.0650(5) 0.0822(5) 0.0392(4) 0.0049(3) -0.0021(3) 0.0037(4) O1 0.0313(10) 0.0519(10) 0.0514(10) 0.0161(8) 0.0063(8) 0.0040(8) O2 0.0299(11) 0.0545(10) 0.0591(11) -0.0007(9) 0.0029(8) 0.0021(8) N1 0.0285(12) 0.0536(12) 0.0360(10) 0.0001(9) 0.0035(9) 0.0027(10) C1 0.0267(15) 0.0512(15) 0.0551(16) 0.0065(13) 0.0059(12) 0.0033(12) C2 0.0316(16) 0.0719(19) 0.0575(17) 0.0158(15) 0.0046(13) 0.0050(14) C3 0.050(2) 0.097(3) 0.083(2) 0.038(2) 0.0027(18) 0.0165(19) C4 0.064(3) 0.076(2) 0.128(4) 0.042(2) 0.016(2) 0.0256(19) C5 0.067(3) 0.060(2) 0.112(3) 0.001(2) 0.024(2) 0.0140(18) C6 0.0393(17) 0.0522(16) 0.075(2) -0.0017(15) 0.0136(15) 0.0038(13) C7 0.057(2) 0.100(2) 0.0419(16) 0.0091(16) -0.0010(14) 0.0106(18) C8 0.075(3) 0.161(4) 0.0499(18) 0.023(2) 0.0082(18) 0.012(3) C9 0.081(3) 0.131(3) 0.066(2) 0.001(2) -0.015(2) -0.017(3) C10 0.063(2) 0.073(2) 0.065(2) -0.0167(16) 0.0151(17) 0.0081(17) C11 0.138(5) 0.107(3) 0.110(3) -0.042(3) 0.017(3) -0.010(3) C12 0.112(4) 0.171(4) 0.072(2) 0.009(3) 0.020(2) -0.050(3) C13 0.0369(16) 0.0586(17) 0.0575(16) 0.0217(14) 0.0061(13) 0.0050(13) C14 0.059(2) 0.0613(18) 0.085(2) 0.0021(17) 0.0167(18) 0.0003(16) C15 0.150(5) 0.062(2) 0.166(5) 0.012(3) 0.052(4) -0.004(3) C16 0.0330(17) 0.0691(18) 0.0687(19) -0.0079(15) -0.0027(14) 0.0010(14) C17 0.042(2) 0.081(2) 0.100(3) -0.009(2) 0.0134(18) -0.0071(17) C18 0.073(3) 0.091(3) 0.170(4) 0.027(3) 0.035(3) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N1 1.664(2) . ? V1 O2 1.7736(18) . ? V1 O1 1.8491(16) . ? V1 O1 2.1699(17) 3_767 ? V1 Cl1 2.2311(8) . ? O1 C13 1.433(3) . ? O1 V1 2.1698(17) 3_767 ? O2 C16 1.422(3) . ? N1 C1 1.387(3) . ? C1 C2 1.404(4) . ? C1 C6 1.416(4) . ? C2 C3 1.385(4) . ? C2 C7 1.512(4) . ? C3 C4 1.371(5) . ? C4 C5 1.371(5) . ? C5 C6 1.380(4) . ? C6 C10 1.508(4) . ? C7 C9 1.534(5) . ? C7 C8 1.536(4) . ? C10 C12 1.504(5) . ? C10 C11 1.513(5) . ? C13 C14 1.520(4) . ? C14 C15 1.513(4) . ? C16 C17 1.504(4) . ? C17 C18 1.498(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 V1 O2 100.19(9) . . ? N1 V1 O1 97.71(9) . . ? O2 V1 O1 123.09(8) . . ? N1 V1 O1 168.80(8) . 3_767 ? O2 V1 O1 84.02(8) . 3_767 ? O1 V1 O1 71.46(7) . 3_767 ? N1 V1 Cl1 101.31(7) . . ? O2 V1 Cl1 112.15(6) . . ? O1 V1 Cl1 116.41(6) . . ? O1 V1 Cl1 86.49(5) 3_767 . ? C13 O1 V1 128.38(15) . . ? C13 O1 V1 122.77(14) . 3_767 ? V1 O1 V1 108.55(7) . 3_767 ? C16 O2 V1 131.04(17) . . ? C1 N1 V1 173.35(17) . . ? N1 C1 C2 120.0(2) . . ? N1 C1 C6 118.1(2) . . ? C2 C1 C6 121.8(2) . . ? C3 C2 C1 117.6(3) . . ? C3 C2 C7 119.5(3) . . ? C1 C2 C7 122.9(2) . . ? C4 C3 C2 121.1(3) . . ? C5 C4 C3 120.8(3) . . ? C4 C5 C6 121.4(3) . . ? C5 C6 C1 117.3(3) . . ? C5 C6 C10 122.0(3) . . ? C1 C6 C10 120.7(2) . . ? C2 C7 C9 110.5(3) . . ? C2 C7 C8 112.4(3) . . ? C9 C7 C8 109.6(3) . . ? C12 C10 C6 110.7(3) . . ? C12 C10 C11 111.0(3) . . ? C6 C10 C11 114.4(3) . . ? O1 C13 C14 112.3(2) . . ? C15 C14 C13 110.3(3) . . ? O2 C16 C17 110.7(3) . . ? C18 C17 C16 114.3(3) . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 26.60 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.256 _refine_diff_density_min -0.291 _refine_diff_density_rms 0.055 #=======================================================================_eof # End of Crystallographic Information File