#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/46/2204634.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204634 loop_ _publ_author_name 'Li-Juan Chen' 'Ming-Xing Yang' 'Shen Lin' _publ_section_title ; Isopropoxy[2'-(2-methoxybenzoyl)-2-oxidobenzohydrazidato]oxovanadium(V) ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m1881 _journal_page_last m1882 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[V (C15 H12 N2 O4) (C3 H7 O)O]' _chemical_formula_moiety 'C18 H19 N2 O6 V' _chemical_formula_sum 'C18 H19 N2 O6 V' _chemical_formula_weight 410.29 _chemical_name_systematic ; Isopropoxy[2'-(2-methoxybenzoyl)-2- oxidobenzohydrazidato](isopropoxy)oxovanadium(V) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 101.84(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 10.835(8) _cell_length_b 9.882(8) _cell_length_c 17.7300(12) _cell_measurement_reflns_used 4227 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 2.35 _cell_volume 1858(2) _computing_cell_refinement RAPID-AUTO _computing_data_collection 'RAPID-AUTO (Rigaku, 1998)' _computing_data_reduction 'CrystalStructure (Rigaku/MSC, 2002)' _computing_molecular_graphics 'SHELXTL/PC (Sheldrick, 1998)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method '\w scan' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0281 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 16277 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 1.92 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_T_max 0.843 _exptl_absorpt_correction_T_min 0.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1999)' _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.467 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 848 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _refine_diff_density_max 0.475 _refine_diff_density_min -0.262 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 244 _refine_ls_number_reflns 4226 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.081 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0386 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0660P)^2^+0.1239P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1120 _refine_ls_wR_factor_ref 0.1168 _reflns_number_gt 3336 _reflns_number_total 4226 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file ci6468.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 2204634 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol V1 0.27238(3) 0.43906(3) 0.077130(17) 0.04575(13) Uani d . 1 V N1 0.40958(14) 0.56827(13) 0.05972(8) 0.0426(3) Uani d . 1 N N2 0.36963(14) 0.65906(14) 0.00014(8) 0.0460(3) Uani d . 1 N H2N 0.4170 0.7230 -0.0106 0.055 Uiso calc R 1 H O1 0.40644(13) 0.34411(13) 0.13214(8) 0.0586(3) Uani d . 1 O O2 0.59469(13) 0.68087(15) 0.07624(9) 0.0668(4) Uani d . 1 O O3 0.19505(12) 0.54057(13) -0.01719(7) 0.0493(3) Uani d . 1 O O4 0.37230(14) 0.86614(15) -0.09145(8) 0.0624(4) Uani d . 1 O O5 0.21334(16) 0.51281(17) 0.14071(8) 0.0681(4) Uani d . 1 O O6 0.17127(14) 0.30487(15) 0.04488(8) 0.0629(4) Uani d . 1 O C1 0.51241(17) 0.38689(19) 0.17930(10) 0.0474(4) Uani d . 1 C C2 0.57721(17) 0.50189(18) 0.16365(10) 0.0451(4) Uani d . 1 C C3 0.6908(2) 0.5341(2) 0.21212(12) 0.0584(5) Uani d . 1 C H3 0.7355 0.6095 0.2013 0.070 Uiso calc R 1 H C4 0.7391(2) 0.4564(3) 0.27609(13) 0.0691(6) Uani d . 1 C H4 0.8153 0.4796 0.3081 0.083 Uiso calc R 1 H C5 0.6737(2) 0.3447(3) 0.29206(12) 0.0671(6) Uani d . 1 C H5 0.7062 0.2921 0.3350 0.081 Uiso calc R 1 H C6 0.5609(2) 0.3099(2) 0.24523(12) 0.0597(5) Uani d . 1 C H6 0.5166 0.2350 0.2572 0.072 Uiso calc R 1 H C7 0.52987(17) 0.59010(18) 0.09664(10) 0.0457(4) Uani d . 1 C C8 0.25446(16) 0.64015(18) -0.03853(9) 0.0436(4) Uani d . 1 C C9 0.19347(18) 0.72694(19) -0.10238(10) 0.0475(4) Uani d . 1 C C10 0.25239(19) 0.8387(2) -0.12852(11) 0.0530(4) Uani d . 1 C C11 0.1857(2) 0.9147(2) -0.18964(13) 0.0689(6) Uani d . 1 C H11 0.2236 0.9889 -0.2078 0.083 Uiso calc R 1 H C12 0.0639(3) 0.8802(3) -0.22314(13) 0.0790(7) Uani d . 1 C H12 0.0206 0.9310 -0.2643 0.095 Uiso calc R 1 H C13 0.0053(2) 0.7733(3) -0.19722(13) 0.0747(7) Uani d . 1 C H13 -0.0777 0.7524 -0.2201 0.090 Uiso calc R 1 H C14 0.06935(19) 0.6959(2) -0.13690(11) 0.0586(5) Uani d . 1 C H14 0.0294 0.6227 -0.1192 0.070 Uiso calc R 1 H C15 0.4381(3) 0.9760(3) -0.11858(17) 0.0842(8) Uani d . 1 C H15A 0.5212 0.9833 -0.0871 0.126 Uiso calc R 1 H H15B 0.3929 1.0587 -0.1158 0.126 Uiso calc R 1 H H15C 0.4443 0.9593 -0.1710 0.126 Uiso calc R 1 H C16 0.0279(3) 0.2434(4) -0.06850(17) 0.1165(12) Uani d . 1 C H16A 0.0249 0.3361 -0.0850 0.175 Uiso calc R 1 H H16B -0.0371 0.2275 -0.0400 0.175 Uiso calc R 1 H H16C 0.0152 0.1851 -0.1127 0.175 Uiso calc R 1 H C17 0.1508(2) 0.2153(3) -0.01941(14) 0.0749(6) Uani d . 1 C H17 0.2154 0.2339 -0.0494 0.090 Uiso calc R 1 H C18 0.1699(4) 0.0759(3) 0.0105(2) 0.1146(12) Uani d . 1 C H18A 0.2528 0.0678 0.0420 0.172 Uiso calc R 1 H H18B 0.1610 0.0137 -0.0319 0.172 Uiso calc R 1 H H18C 0.1081 0.0556 0.0407 0.172 Uiso calc R 1 H 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 V1 0.0469(2) 0.04482(19) 0.04441(19) -0.01057(13) 0.00684(13) 0.00124(12) N1 0.0433(7) 0.0396(7) 0.0428(7) -0.0026(6) 0.0039(6) 0.0045(6) N2 0.0472(8) 0.0415(8) 0.0477(8) -0.0045(6) 0.0059(6) 0.0075(6) O1 0.0611(8) 0.0443(7) 0.0637(8) -0.0096(6) -0.0024(6) 0.0091(6) O2 0.0529(8) 0.0651(9) 0.0766(9) -0.0197(7) -0.0004(7) 0.0201(8) O3 0.0451(7) 0.0502(7) 0.0503(7) -0.0062(5) 0.0042(6) 0.0049(6) O4 0.0660(9) 0.0543(8) 0.0684(9) -0.0039(7) 0.0174(7) 0.0137(7) O5 0.0742(10) 0.0775(10) 0.0565(8) -0.0058(8) 0.0229(7) -0.0069(8) O6 0.0662(9) 0.0593(8) 0.0583(8) -0.0249(7) 0.0010(7) 0.0039(7) C1 0.0509(10) 0.0430(9) 0.0474(9) 0.0039(8) 0.0078(8) -0.0006(8) C2 0.0456(9) 0.0442(9) 0.0441(9) 0.0020(7) 0.0060(7) -0.0022(8) C3 0.0512(11) 0.0614(12) 0.0583(11) -0.0037(9) 0.0014(9) 0.0003(10) C4 0.0563(12) 0.0827(16) 0.0597(12) 0.0037(11) -0.0083(10) 0.0019(12) C5 0.0732(14) 0.0715(14) 0.0516(11) 0.0154(12) 0.0012(10) 0.0086(10) C6 0.0696(13) 0.0522(11) 0.0561(11) 0.0056(9) 0.0100(10) 0.0081(9) C7 0.0452(9) 0.0424(9) 0.0483(9) -0.0036(7) 0.0067(7) -0.0020(8) C8 0.0470(9) 0.0430(9) 0.0415(8) 0.0037(7) 0.0105(7) -0.0015(7) C9 0.0529(10) 0.0495(10) 0.0411(8) 0.0084(8) 0.0116(8) 0.0024(8) C10 0.0604(11) 0.0546(11) 0.0463(9) 0.0088(9) 0.0165(8) 0.0038(8) C11 0.0836(16) 0.0678(14) 0.0584(12) 0.0144(12) 0.0215(12) 0.0176(11) C12 0.0903(18) 0.0893(18) 0.0539(12) 0.0309(15) 0.0067(12) 0.0192(13) C13 0.0605(12) 0.0966(18) 0.0614(12) 0.0183(13) -0.0004(10) 0.0118(13) C14 0.0526(10) 0.0691(13) 0.0522(10) 0.0095(10) 0.0065(9) 0.0028(10) C15 0.0934(19) 0.0630(14) 0.0998(19) -0.0162(13) 0.0282(16) 0.0199(14) C16 0.134(3) 0.105(2) 0.0839(19) -0.005(2) -0.0391(19) -0.0115(17) C17 0.0763(15) 0.0750(15) 0.0742(14) -0.0169(13) 0.0171(12) -0.0136(13) C18 0.137(3) 0.0715(18) 0.129(3) 0.0173(18) 0.012(2) -0.0103(18) 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O5 V1 O6 105.40(9) yes O5 V1 O1 104.39(8) yes O6 V1 O1 99.29(9) yes O5 V1 O3 101.83(8) yes O6 V1 O3 88.84(7) yes O1 V1 O3 149.26(6) yes O5 V1 N1 103.54(9) yes O6 V1 N1 149.35(7) yes O1 V1 N1 82.98(8) yes O3 V1 N1 75.49(7) yes C7 N1 N2 112.67(14) ? C7 N1 V1 133.68(12) ? N2 N1 V1 113.52(11) ? C8 N2 N1 114.98(14) ? C8 N2 H2N 122.5 ? N1 N2 H2N 122.5 ? C1 O1 V1 130.79(13) ? C8 O3 V1 119.28(11) ? C10 O4 C15 118.73(18) ? C17 O6 V1 136.13(14) ? O1 C1 C2 122.30(16) ? O1 C1 C6 118.30(18) ? C2 C1 C6 119.36(18) ? C3 C2 C1 118.91(17) ? C3 C2 C7 118.73(18) ? C1 C2 C7 122.36(16) ? C4 C3 C2 121.3(2) ? C4 C3 H3 119.3 ? C2 C3 H3 119.3 ? C5 C4 C3 119.5(2) ? C5 C4 H4 120.2 ? C3 C4 H4 120.2 ? C4 C5 C6 120.7(2) ? C4 C5 H5 119.7 ? C6 C5 H5 119.7 ? C5 C6 C1 120.1(2) ? C5 C6 H6 119.9 ? C1 C6 H6 119.9 ? O2 C7 N1 121.54(17) ? O2 C7 C2 122.55(17) ? N1 C7 C2 115.89(16) ? O3 C8 N2 116.11(15) ? O3 C8 C9 120.39(16) ? N2 C8 C9 123.50(17) ? C14 C9 C10 119.51(17) ? C14 C9 C8 116.90(18) ? C10 C9 C8 123.58(18) ? O4 C10 C11 124.2(2) ? O4 C10 C9 116.92(16) ? C11 C10 C9 118.9(2) ? C12 C11 C10 120.1(2) ? C12 C11 H11 119.9 ? C10 C11 H11 119.9 ? C13 C12 C11 121.3(2) ? C13 C12 H12 119.3 ? C11 C12 H12 119.3 ? C12 C13 C14 119.8(2) ? C12 C13 H13 120.1 ? C14 C13 H13 120.1 ? C13 C14 C9 120.4(2) ? C13 C14 H14 119.8 ? C9 C14 H14 119.8 ? O4 C15 H15A 109.5 ? O4 C15 H15B 109.5 ? H15A C15 H15B 109.5 ? O4 C15 H15C 109.5 ? H15A C15 H15C 109.5 ? H15B C15 H15C 109.5 ? C17 C16 H16A 109.5 ? C17 C16 H16B 109.5 ? H16A C16 H16B 109.5 ? C17 C16 H16C 109.5 ? H16A C16 H16C 109.5 ? H16B C16 H16C 109.5 ? O6 C17 C16 109.4(2) ? O6 C17 C18 107.8(2) ? C16 C17 C18 115.8(3) ? O6 C17 H17 107.9 ? C16 C17 H17 107.9 ? C18 C17 H17 107.9 ? C17 C18 H18A 109.5 ? C17 C18 H18B 109.5 ? H18A C18 H18B 109.5 ? C17 C18 H18C 109.5 ? H18A C18 H18C 109.5 ? H18B C18 H18C 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag V1 O5 1.5834(16) yes V1 O6 1.7402(16) yes V1 O1 1.8331(16) yes V1 O3 1.9824(14) yes V1 N1 2.0307(18) yes N1 C7 1.350(2) ? N1 N2 1.386(2) ? N2 C8 1.308(2) ? N2 H2N 0.86 ? O1 C1 1.342(2) ? O2 C7 1.238(2) ? O3 C8 1.275(2) ? O4 C10 1.358(3) ? O4 C15 1.435(3) ? O6 C17 1.424(3) ? C1 C2 1.393(3) ? C1 C6 1.404(3) ? C2 C3 1.386(3) ? C2 C7 1.478(3) ? C3 C4 1.380(3) ? C3 H3 0.93 ? C4 C5 1.371(3) ? C4 H4 0.93 ? C5 C6 1.373(3) ? C5 H5 0.93 ? C6 H6 0.93 ? C8 C9 1.465(2) ? C9 C14 1.393(3) ? C9 C10 1.402(3) ? C10 C11 1.392(3) ? C11 C12 1.375(4) ? C11 H11 0.93 ? C12 C13 1.360(4) ? C12 H12 0.93 ? C13 C14 1.380(3) ? C13 H13 0.93 ? C14 H14 0.93 ? C15 H15A 0.96 ? C15 H15B 0.96 ? C15 H15C 0.96 ? C16 C17 1.460(4) ? C16 H16A 0.96 ? C16 H16B 0.96 ? C16 H16C 0.96 ? C17 C18 1.475(4) ? C17 H17 0.98 ? C18 H18A 0.96 ? C18 H18B 0.96 ? C18 H18C 0.96 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O5 V1 N1 C7 82.69(18) O6 V1 N1 C7 -116.90(19) O1 V1 N1 C7 -20.49(17) O3 V1 N1 C7 -178.36(18) O5 V1 N1 N2 -92.74(13) O6 V1 N1 N2 67.68(18) O1 V1 N1 N2 164.08(12) O3 V1 N1 N2 6.21(11) C7 N1 N2 C8 178.55(15) V1 N1 N2 C8 -5.04(18) O5 V1 O1 C1 -63.09(18) O6 V1 O1 C1 -171.74(16) O3 V1 O1 C1 84.7(2) N1 V1 O1 C1 39.15(16) O5 V1 O3 C8 93.90(14) O6 V1 O3 C8 -160.60(13) O1 V1 O3 C8 -54.22(18) N1 V1 O3 C8 -7.21(12) O5 V1 O6 C17 164.9(2) O1 V1 O6 C17 -87.3(2) O3 V1 O6 C17 62.9(2) N1 V1 O6 C17 4.6(3) V1 O1 C1 C2 -39.2(3) V1 O1 C1 C6 142.87(16) O1 C1 C2 C3 -175.31(17) C6 C1 C2 C3 2.6(3) O1 C1 C2 C7 4.0(3) C6 C1 C2 C7 -178.13(17) C1 C2 C3 C4 -1.5(3) C7 C2 C3 C4 179.2(2) C2 C3 C4 C5 0.2(4) C3 C4 C5 C6 -0.2(4) C4 C5 C6 C1 1.3(3) O1 C1 C6 C5 175.42(18) C2 C1 C6 C5 -2.6(3) N2 N1 C7 O2 -1.5(3) V1 N1 C7 O2 -176.95(14) N2 N1 C7 C2 176.85(14) V1 N1 C7 C2 1.4(3) C3 C2 C7 O2 9.7(3) C1 C2 C7 O2 -169.61(18) C3 C2 C7 N1 -168.65(17) C1 C2 C7 N1 12.1(3) V1 O3 C8 N2 6.7(2) V1 O3 C8 C9 -172.59(12) N1 N2 C8 O3 -0.8(2) N1 N2 C8 C9 178.49(15) O3 C8 C9 C14 0.7(3) N2 C8 C9 C14 -178.57(16) O3 C8 C9 C10 179.40(16) N2 C8 C9 C10 0.1(3) C15 O4 C10 C11 -3.2(3) C15 O4 C10 C9 177.23(19) C14 C9 C10 O4 178.39(17) C8 C9 C10 O4 -0.3(3) C14 C9 C10 C11 -1.2(3) C8 C9 C10 C11 -179.89(18) O4 C10 C11 C12 -179.2(2) C9 C10 C11 C12 0.4(3) C10 C11 C12 C13 0.8(4) C11 C12 C13 C14 -1.0(4) C12 C13 C14 C9 0.1(3) C10 C9 C14 C13 1.0(3) C8 C9 C14 C13 179.75(19) V1 O6 C17 C16 -112.2(3) V1 O6 C17 C18 121.1(3)