#------------------------------------------------------------------------------ #$Date: 2020-02-03 10:52:46 +0200 (Mon, 03 Feb 2020) $ #$Revision: 247458 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/72/1557212.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1557212 loop_ _publ_author_name 'Polamo, Mika' 'Leskela, Markku' _publ_section_title ; Syntheses and Crystal Structures of Bis[2-(benzylamino)-4-methylpyridinato]trichlorotantalum(V) and Bis[2-(benzylamino)-6-methylpyridinato]trichlorotantalum(V) ; _journal_name_full 'Acta Chemica Scandinavica' _journal_page_first 709 _journal_page_last 713 _journal_paper_doi 10.3891/acta.chem.scand.51-0709 _journal_volume 51 _journal_year 1997 _chemical_formula_moiety 'C26 H26 Cl3 N4 Ta, C8 H10' _chemical_formula_sum 'C34 H36 Cl3 N4 Ta' _chemical_formula_weight 787.97 _chemical_name_common ; Bis[2-(benzylamino)-6-methylpyridinato]trichlorotantalum(V) ; _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 106.53(6) _cell_angle_beta 100.51(5) _cell_angle_gamma 90.15(7) _cell_formula_units_Z 2 _cell_length_a 10.066(7) _cell_length_b 12.113(11) _cell_length_c 14.329(9) _cell_volume 1644(2) _diffrn_ambient_temperature 193 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 3.616 _exptl_crystal_density_diffrn 1.592 _exptl_crystal_F_000 784 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_number_parameters 380 _refine_ls_number_reflns 5113 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_gt 0.1372 _cod_data_source_file Acta-Chem-Scand-1997-51-709-2.cif _cod_data_source_block 2 _cod_database_code 1557212 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta Ta Uiso -0.1655(2) 0.32290(10) 0.08910(10) 1.000 0.0300(10) . . . . Cl1 Cl Uiso -0.3209(2) 0.2243(2) -0.0620(2) 1.000 0.0420(10) . . . . Cl3 Cl Uiso -0.3440(2) 0.3058(2) 0.1765(2) 1.000 0.0440(10) . . . . Cl2 Cl Uiso -0.0182(2) 0.3446(2) -0.0175(2) 1.000 0.0390(10) . . . . N1 N Uiso -0.1374(7) 0.1370(6) 0.0941(5) 1.000 0.036(2) . . . . N7 N Uiso 0.0057(7) 0.2837(6) 0.1719(5) 1.000 0.034(2) . . . . N15 N Uiso -0.2545(7) 0.4860(6) 0.0572(5) 1.000 0.035(2) . . . . N21 N Uiso -0.1221(8) 0.4786(6) 0.1942(5) 1.000 0.036(2) . . . . C2 C Uiso -0.0100(9) 0.1644(7) 0.1444(6) 1.000 0.033(2) . . . . C3 C Uiso 0.0815(9) 0.0830(8) 0.1609(7) 1.000 0.038(2) . . . . C4 C Uiso 0.0329(10) -0.0305(8) 0.1266(7) 1.000 0.042(2) . . . . C5 C Uiso -0.0997(10) -0.0590(8) 0.0795(7) 1.000 0.041(2) . . . . C6 C Uiso -0.1865(9) 0.0260(8) 0.0634(6) 1.000 0.037(2) . . . . C6M C Uiso -0.3318(9) -0.0031(8) 0.0156(8) 1.000 0.047(2) . . . . C8 C Uiso 0.1430(9) 0.3379(8) 0.2041(7) 1.000 0.037(2) . . . . C9 C Uiso 0.2154(10) 0.3332(8) 0.3061(7) 1.000 0.041(2) . . . . C10 C Uiso 0.1505(11) 0.3050(8) 0.3741(7) 1.000 0.047(2) . . . . C11 C Uiso 0.2206(13) 0.3077(10) 0.4669(8) 1.000 0.060(3) . . . . C12 C Uiso 0.3573(15) 0.3361(11) 0.4917(9) 1.000 0.073(4) . . . . C13 C Uiso 0.4237(14) 0.3629(11) 0.4252(11) 1.000 0.075(4) . . . . C14 C Uiso 0.3542(11) 0.3611(10) 0.3322(10) 1.000 0.060(3) . . . . C16 C Uiso -0.2022(9) 0.5504(8) 0.1516(7) 1.000 0.037(2) . . . . C17 C Uiso -0.2330(10) 0.6630(8) 0.1916(8) 1.000 0.045(2) . . . . C18 C Uiso -0.3146(10) 0.7124(8) 0.1274(8) 1.000 0.046(2) . . . . C19 C Uiso -0.3597(9) 0.6502(8) 0.0297(8) 1.000 0.043(2) . . . . C20 C Uiso -0.3276(9) 0.5374(8) -0.0065(7) 1.000 0.036(2) . . . . C20M C Uiso -0.3711(10) 0.4707(8) -0.1130(7) 1.000 0.043(2) . . . . C22 C Uiso -0.0812(10) 0.5118(8) 0.3021(6) 1.000 0.039(2) . . . . C23 C Uiso 0.0408(9) 0.5964(8) 0.3447(7) 1.000 0.040(2) . . . . C24 C Uiso 0.0929(11) 0.6230(10) 0.4459(8) 1.000 0.053(3) . . . . C25 C Uiso 0.2036(12) 0.6994(11) 0.4890(9) 1.000 0.065(3) . . . . C26 C Uiso 0.2646(12) 0.7507(10) 0.4332(10) 1.000 0.064(3) . . . . C27 C Uiso 0.2161(12) 0.7253(10) 0.3325(10) 1.000 0.061(3) . . . . C28 C Uiso 0.1037(10) 0.6485(8) 0.2888(7) 1.000 0.045(2) . . . . C31 C Uiso 0.4677(12) 0.9946(9) 0.6656(8) 1.000 0.054(3) . . . . C32 C Uiso 0.4010(13) 1.0643(10) 0.6115(9) 1.000 0.062(3) . . . . C33 C Uiso 0.2635(13) 1.0764(10) 0.6023(8) 1.000 0.059(3) . . . . C34 C Uiso 0.1828(14) 1.0206(11) 0.6462(8) 1.000 0.062(3) . . . . C35 C Uiso 0.2484(15) 0.9503(11) 0.6997(9) 1.000 0.066(3) . . . . C36 C Uiso 0.3883(16) 0.9396(10) 0.7093(8) 1.000 0.070(4) . . . . C37 C Uiso 0.6171(14) 0.9825(12) 0.6761(11) 1.000 0.080(4) . . . . C38 C Uiso 0.0336(16) 1.0349(15) 0.6382(11) 1.000 0.088(4) . . . . 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' Cl Cl 0.1484 0.1585 ' 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' Ta Ta -0.7052 6.5227 ' 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_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ta Cl3 87.19(12) . . . yes Cl1 Ta Cl2 85.29(11) . . . yes Cl1 Ta N1 81.1(2) . . . yes Cl1 Ta N7 136.1(2) . . . yes Cl1 Ta N15 83.7(2) . . . yes Cl1 Ta N21 142.5(2) . . . yes Cl3 Ta Cl2 170.61(11) . . . yes Cl3 Ta N1 81.6(2) . . . yes Cl3 Ta N7 105.1(2) . . . yes Cl3 Ta N15 90.4(2) . . . yes Cl3 Ta N21 83.8(2) . . . yes Cl2 Ta N1 102.7(2) . . . yes Cl2 Ta N7 84.3(2) . . . yes Cl2 Ta N15 83.2(2) . . . yes Cl2 Ta N21 98.8(2) . . . yes N1 Ta N7 60.0(3) . . . yes N1 Ta N15 163.1(3) . . . yes N1 Ta N21 132.8(3) . . . yes N7 Ta N15 136.8(3) . . . yes N7 Ta N21 81.2(3) . . . yes N15 Ta N21 60.2(3) . . . yes Ta N1 C2 91.4(5) . . . yes Ta N1 C6 148.2(6) . . . yes C2 N1 C6 120.0(8) . . . yes Ta N7 C2 101.1(5) . . . yes Ta N7 C8 132.2(6) . . . yes C2 N7 C8 118.5(7) . . . yes Ta N15 C16 91.0(6) . . . yes Ta N15 C20 149.7(6) . . . yes C16 N15 C20 119.3(8) . . . yes Ta N21 C16 102.3(6) . . . yes Ta N21 C22 132.9(6) . . . yes C16 N21 C22 118.6(8) . . . yes N1 C2 N7 106.1(7) . . . yes N1 C2 C3 123.5(8) . . . yes N7 C2 C3 130.4(8) . . . yes C2 C3 C4 116.3(9) . . . no C3 C4 C5 120.5(9) . . . no C4 C5 C6 120.8(9) . . . no N1 C6 C5 118.7(8) . . . yes N1 C6 C6M 120.0(8) . . . yes C5 C6 C6M 121.4(9) . . . no N7 C8 C9 115.1(8) . . . yes C8 C9 C10 123.7(9) . . . no C8 C9 C14 117.7(9) . . . no C10 C9 C14 118.6(10) . . . no C9 C10 C11 120.8(11) . . . no C10 C11 C12 119.8(11) . . . no C11 C12 C13 120.3(12) . . . no C12 C13 C14 120.3(13) . . . no C9 C14 C13 120.1(12) . . . no N15 C16 N21 105.8(8) . . . yes N15 C16 C17 123.7(9) . . . yes N21 C16 C17 130.4(9) . . . yes C16 C17 C18 116.1(10) . . . no C17 C18 C19 120.3(10) . . . no C18 C19 C20 121.5(9) . . . no N15 C20 C19 118.6(9) . . . yes N15 C20 C20M 119.4(8) . . . yes C19 C20 C20M 122.0(9) . . . no N21 C22 C23 115.3(8) . . . yes C22 C23 C24 118.2(9) . . . no C22 C23 C28 123.8(8) . . . no C24 C23 C28 118.1(9) . . . no C23 C24 C25 120.9(11) . . . no C24 C25 C26 120.6(11) . . . no C25 C26 C27 119.9(12) . . . no C26 C27 C28 119.6(11) . . . no C23 C28 C27 121.0(10) . . . no C32 C31 C36 116.1(12) . . . no C32 C31 C37 121.5(11) . . . no C36 C31 C37 122.4(12) . . . no C31 C32 C33 121.7(12) . . . no C32 C33 C34 122.4(12) . . . no C33 C34 C35 116.3(13) . . . no C33 C34 C38 122.8(12) . . . no C35 C34 C38 120.9(13) . . . no C34 C35 C36 120.8(13) . . . no C31 C36 C35 122.8(12) . . . no 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 Ta Cl1 2.418(4) . . yes Ta Cl3 2.410(4) . . yes Ta Cl2 2.378(4) . . yes Ta N1 2.290(8) . . yes Ta N7 2.045(8) . . yes Ta N15 2.300(8) . . yes Ta N21 2.038(8) . . yes N1 C2 1.341(11) . . yes N1 C6 1.351(12) . . yes N7 C2 1.386(12) . . yes N7 C8 1.464(12) . . yes N15 C16 1.361(12) . . yes N15 C20 1.358(12) . . yes N21 C16 1.380(12) . . yes N21 C22 1.461(11) . . yes C2 C3 1.391(13) . . no C3 C4 1.377(14) . . no C4 C5 1.376(14) . . no C5 C6 1.394(14) . . no C6 C6M 1.492(13) . . no C8 C9 1.526(14) . . no C9 C10 1.383(14) . . no C9 C14 1.393(15) . . no C10 C11 1.378(15) . . no C11 C12 1.37(2) . . no C12 C13 1.37(2) . . no C13 C14 1.38(2) . . no C16 C17 1.381(14) . . no C17 C18 1.385(15) . . no C18 C19 1.378(15) . . no C19 C20 1.379(14) . . no C20 C20M 1.492(13) . . no C22 C23 1.515(14) . . no C23 C24 1.392(14) . . no C23 C28 1.383(14) . . no C24 C25 1.378(17) . . no C25 C26 1.365(18) . . no C26 C27 1.380(19) . . no C27 C28 1.394(16) . . no C31 C32 1.396(17) . . no C31 C36 1.376(18) . . no C31 C37 1.496(19) . . no C32 C33 1.378(19) . . no C33 C34 1.392(18) . . no C34 C35 1.392(19) . . no C34 C38 1.50(2) . . no C35 C36 1.40(2) . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Ta N1 C2 151.3(5) . . . . no Cl1 Ta N1 C6 -20.1(11) . . . . no Cl3 Ta N1 C2 -120.3(5) . . . . no Cl3 Ta N1 C6 68.3(11) . . . . no Cl2 Ta N1 C2 68.2(5) . . . . no Cl2 Ta N1 C6 -103.2(11) . . . . no N7 Ta N1 C2 -7.5(5) . . . . no N7 Ta N1 C6 -178.9(12) . . . . no N21 Ta N1 C2 -46.8(7) . . . . no N21 Ta N1 C6 141.8(10) . . . . no Cl1 Ta N7 C2 -23.7(7) . . . . no Cl1 Ta N7 C8 122.8(7) . . . . no Cl3 Ta N7 C2 78.2(5) . . . . no Cl3 Ta N7 C8 -135.3(7) . . . . no Cl2 Ta N7 C2 -100.9(5) . . . . no Cl2 Ta N7 C8 45.7(7) . . . . no N1 Ta N7 C2 7.4(5) . . . . no N1 Ta N7 C8 153.9(8) . . . . no N15 Ta N7 C2 -174.6(5) . . . . no N15 Ta N7 C8 -28.1(9) . . . . no N21 Ta N7 C2 159.3(6) . . . . no N21 Ta N7 C8 -54.2(8) . . . . no Cl1 Ta N15 C16 164.5(5) . . . . no Cl1 Ta N15 C20 -14.6(12) . . . . no Cl3 Ta N15 C16 77.4(5) . . . . no Cl3 Ta N15 C20 -101.7(12) . . . . no Cl2 Ta N15 C16 -109.5(5) . . . . no Cl2 Ta N15 C20 71.4(12) . . . . no N7 Ta N15 C16 -35.3(7) . . . . no N7 Ta N15 C20 145.6(11) . . . . no N21 Ta N15 C16 -5.2(5) . . . . no N21 Ta N15 C20 175.7(13) . . . . no Cl1 Ta N21 C16 -11.6(8) . . . . no Cl1 Ta N21 C22 138.8(7) . . . . no Cl3 Ta N21 C16 -88.8(6) . . . . no Cl3 Ta N21 C22 61.7(8) . . . . no Cl2 Ta N21 C16 82.1(6) . . . . no Cl2 Ta N21 C22 -127.4(8) . . . . no N1 Ta N21 C16 -161.3(5) . . . . no N1 Ta N21 C22 -10.9(11) . . . . no N7 Ta N21 C16 164.9(6) . . . . no N7 Ta N21 C22 -44.6(9) . . . . no N15 Ta N21 C16 5.3(5) . . . . no N15 Ta N21 C22 155.7(10) . . . . no Ta N1 C2 N7 10.0(6) . . . . no Ta N1 C2 C3 -169.3(8) . . . . no C6 N1 C2 N7 -175.2(7) . . . . no C6 N1 C2 C3 5.5(13) . . . . no Ta N1 C6 C5 166.0(8) . . . . no Ta N1 C6 C6M -15.5(16) . . . . no C2 N1 C6 C5 -4.1(12) . . . . no C2 N1 C6 C6M 174.5(8) . . . . no Ta N7 C2 N1 -11.4(7) . . . . no Ta N7 C2 C3 167.8(9) . . . . no C8 N7 C2 N1 -163.7(7) . . . . no C8 N7 C2 C3 15.5(13) . . . . no Ta N7 C8 C9 145.7(7) . . . . no C2 N7 C8 C9 -72.4(10) . . . . no Ta N15 C16 N21 7.0(7) . . . . no Ta N15 C16 C17 -170.8(9) . . . . no C20 N15 C16 N21 -173.6(8) . . . . no C20 N15 C16 C17 8.7(14) . . . . no Ta N15 C20 C19 171.6(8) . . . . no Ta N15 C20 C20M -8.3(17) . . . . no C16 N15 C20 C19 -7.4(13) . . . . no C16 N15 C20 C20M 172.8(8) . . . . no Ta N21 C16 N15 -8.1(8) . . . . no Ta N21 C16 C17 169.5(10) . . . . no C22 N21 C16 N15 -163.7(8) . . . . no C22 N21 C16 C17 13.8(15) . . . . no Ta N21 C22 C23 130.6(8) . . . . no C16 N21 C22 C23 -82.8(11) . . . . no N1 C2 C3 C4 -3.1(13) . . . . no N7 C2 C3 C4 177.8(9) . . . . no C2 C3 C4 C5 -0.5(14) . . . . no C3 C4 C5 C6 1.6(15) . . . . no C4 C5 C6 N1 0.7(13) . . . . no C4 C5 C6 C6M -177.8(9) . . . . no N7 C8 C9 C10 -14.3(14) . . . . no N7 C8 C9 C14 166.9(9) . . . . no C8 C9 C10 C11 -176.8(10) . . . . no C14 C9 C10 C11 1.9(16) . . . . no C8 C9 C14 C13 177.3(11) . . . . no C10 C9 C14 C13 -1.5(17) . . . . no C9 C10 C11 C12 -1.5(18) . . . . no C10 C11 C12 C13 1(2) . . . . no C11 C12 C13 C14 0(2) . . . . no C12 C13 C14 C9 1(2) . . . . no N15 C16 C17 C18 -4.6(15) . . . . no N21 C16 C17 C18 178.2(10) . . . . no C16 C17 C18 C19 -0.4(15) . . . . no C17 C18 C19 C20 1.2(15) . . . . no C18 C19 C20 N15 2.7(14) . . . . no C18 C19 C20 C20M -177.5(9) . . . . no N21 C22 C23 C24 -173.9(9) . . . . no N21 C22 C23 C28 5.9(14) . . . . no C22 C23 C24 C25 -179.9(11) . . . . no C28 C23 C24 C25 0.3(17) . . . . no C22 C23 C28 C27 -179.7(10) . . . . no C24 C23 C28 C27 0.1(16) . . . . no C23 C24 C25 C26 0.0(19) . . . . no C24 C25 C26 C27 -1(2) . . . . no C25 C26 C27 C28 0.9(19) . . . . no C26 C27 C28 C23 -0.7(17) . . . . no C36 C31 C32 C33 -0.3(17) . . . . no C37 C31 C32 C33 -179.5(12) . . . . no C32 C31 C36 C35 1.0(17) . . . . no C37 C31 C36 C35 -179.9(12) . . . . no C31 C32 C33 C34 0.2(19) . . . . no C32 C33 C34 C35 -0.6(18) . . . . no C32 C33 C34 C38 178.8(12) . . . . no C33 C34 C35 C36 1.2(18) . . . . no C38 C34 C35 C36 -178.2(12) . . . . no C34 C35 C36 C31 -1.5(19) . . . . no