#------------------------------------------------------------------------------ #$Date: 2020-01-30 12:45:04 +0200 (Thu, 30 Jan 2020) $ #$Revision: 247378 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/71/1557192.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_1557192 loop_ _publ_author_name 'Romero, Jaime' 'Garcia-Vazquez, Jose A.' 'Duran, Maria L.' 'Castineiras, Alfonso' 'Sousa, Antonio' 'Garnovskii, Alexander D.' 'Garnovskii, D. A.' _publ_section_title ; Electrochemical Synthesis of Zinc and Cadmium Complexes with N-[(2-pyrrolyl)methylidyne]-N'-tosylbenzene-1,2-diamine. The Crystal Structure of Bis-{N-[(2-pyrrolyl)methylidene]-N'-tosylbenzene-1,2-diaminato}zinc(II) ; _journal_name_full 'Acta Chemica Scandinavica' _journal_page_first 672 _journal_page_last 675 _journal_paper_doi 10.3891/acta.chem.scand.51-0672 _journal_volume 51 _journal_year 1997 _chemical_formula_sum 'C36 H32 N6 O4 S2 Zn' _chemical_formula_weight 742.19 _chemical_name_common ; Bis-{N-[(2-pyrrolyl)methylidene]-N'-tosylbenzene-1,2-diaminato}zinc(II) ; _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 15 _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _cell_angle_alpha 90. _cell_angle_beta 98.64(2) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 21.811(7) _cell_length_b 11.523(2) _cell_length_c 14.063(4) _cell_volume 3494.3(16) _diffrn_ambient_temperature 293 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 0.88 _exptl_crystal_density_diffrn 1.411 _exptl_crystal_F_000 1536 _refine_ls_goodness_of_fit_ref 3.52 _refine_ls_number_parameters 223 _refine_ls_number_reflns 2034 _refine_ls_R_factor_gt 0.053 _refine_ls_wR_factor_gt 0.057 _cod_data_source_file Acta-Chem-Scand-1997-51-672.cif _cod_data_source_block 1 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 1557192 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,y,1/2-z 3 -x,-y,-z 4 x,-y,1/2+z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,1/2-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,1/2+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 Zn Zn Uiso 0.50000 0.09262(9) 0.75000 1.000 0.0346(3) . . . . S S Uiso 0.40184(7) 0.25980(10) 0.81890(10) 1.000 0.0415(4) . . . . O1 O Uiso 0.3501(2) 0.2238(4) 0.8644(3) 1.000 0.0557(13) . . . . O2 O Uiso 0.4596(2) 0.2817(4) 0.8816(3) 1.000 0.0557(13) . . . . N1 N Uiso 0.4189(2) 0.1684(4) 0.7421(3) 1.000 0.0393(13) . . . . N2 N Uiso 0.5428(2) 0.0016(4) 0.8666(3) 1.000 0.0329(11) . . . . N3 N Uiso 0.4089(3) -0.1189(6) 0.8345(4) 1.000 0.074(3) . . . . C1 C Uiso 0.3262(3) 0.4462(5) 0.7704(4) 1.000 0.0443(13) . . . . C2 C Uiso 0.3087(3) 0.5471(6) 0.7193(5) 1.000 0.0545(13) . . . . C3 C Uiso 0.3435(3) 0.5931(6) 0.6541(4) 1.000 0.0519(13) . . . . C4 C Uiso 0.3962(3) 0.5332(7) 0.6409(5) 1.000 0.065(3) . . . . C5 C Uiso 0.4149(3) 0.4330(6) 0.6904(5) 1.000 0.058(3) . . . . C6 C Uiso 0.3795(3) 0.3892(5) 0.7558(4) 1.000 0.0405(13) . . . . C7 C Uiso 0.3749(2) 0.1272(5) 0.6663(4) 1.000 0.0367(13) . . . . C8 C Uiso 0.3133(3) 0.1662(6) 0.6454(5) 1.000 0.0456(13) . . . . C9 C Uiso 0.2732(3) 0.1213(6) 0.5685(5) 1.000 0.0519(13) . . . . C10 C Uiso 0.2930(3) 0.0366(6) 0.5124(5) 1.000 0.0545(13) . . . . C11 C Uiso 0.3530(3) -0.0038(5) 0.5309(4) 1.000 0.0443(13) . . . . C12 C Uiso 0.6054(2) 0.0395(5) 0.8918(4) 1.000 0.0342(13) . . . . C13 C Uiso 0.5235(3) -0.0856(6) 0.9123(4) 1.000 0.0405(13) . . . . C14 C Uiso 0.4635(3) -0.1375(5) 0.8970(4) 1.000 0.0393(13) . . . . C15 C Uiso 0.4534(2) -0.2319(5) 0.9515(4) 1.000 0.0367(13) . . . . C16 C Uiso 0.3960(3) -0.2711(7) 0.9266(5) 1.000 0.063(3) . . . . C17 C Uiso 0.3668(3) -0.2041(6) 0.8534(5) 1.000 0.058(3) . . . . C30 C Uiso 0.3240(5) 0.7025(7) 0.6011(6) 1.000 0.086(3) . . . . 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' 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' S S 0.1246 0.1234 ' International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 ' 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 N1 Zn N2 124.88(17) . . . yes N1 Zn N1 127.1(2) . . 2_656 yes N1 Zn N2 83.34(18) . . 2_656 yes N1 Zn N2 83.34(18) 2_656 . . yes N2 Zn N2 118.44(19) . . 2_656 yes N1 Zn N2 124.88(17) 2_656 . 2_656 yes O1 S O2 116.6(3) . . . yes O1 S N1 112.9(3) . . . yes O1 S C6 106.9(3) . . . yes O2 S N1 104.9(3) . . . yes O2 S C6 108.0(3) . . . yes N1 S C6 107.0(3) . . . yes Zn N1 S 123.8(3) . . . yes Zn N1 C7 113.6(3) . . . yes S N1 C7 122.4(4) . . . yes Zn N2 C12 110.2(3) . . . yes Zn N2 C13 130.6(4) . . . yes C12 N2 C13 119.0(5) . . . yes C14 N3 C17 107.3(6) . . . yes C2 C1 C6 119.6(6) . . . no C1 C2 C3 121.9(6) . . . no C2 C3 C4 116.8(6) . . . no C2 C3 C30 120.8(7) . . . no C4 C3 C30 122.5(7) . . . no C3 C4 C5 122.8(6) . . . no C4 C5 C6 119.3(6) . . . no S C6 C1 120.2(5) . . . yes S C6 C5 120.2(5) . . . yes C1 C6 C5 119.6(6) . . . no N1 C7 C8 125.0(5) . . . yes N1 C7 C12 116.7(4) . . 2_656 yes C8 C7 C12 118.3(5) . . 2_656 no C7 C8 C9 121.0(6) . . . no C8 C9 C10 120.1(6) . . . no C9 C10 C11 120.5(6) . . . no C10 C11 C12 120.9(5) . . 2_656 no N2 C12 C7 116.1(5) . . 2_656 yes N2 C12 C11 124.7(5) . . 2_656 yes C7 C12 C11 119.2(5) 2_656 . 2_656 no N2 C13 C14 127.5(6) . . . yes N3 C14 C13 135.4(6) . . . yes N3 C14 C15 106.4(5) . . . yes C13 C14 C15 118.1(5) . . . no C14 C15 C16 110.4(6) . . . no C15 C16 C17 108.7(6) . . . no N3 C17 C16 107.2(6) . . . yes 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 Zn N1 1.961(5) . . yes Zn N2 2.050(4) . . yes Zn N1 1.961(5) . 2_656 yes Zn N2 2.050(4) . 2_656 yes S O1 1.439(5) . . yes S O2 1.447(5) . . yes S N1 1.592(5) . . yes S C6 1.766(6) . . yes N1 C7 1.406(7) . . yes N2 C12 1.427(6) . . yes N2 C13 1.297(8) . . yes N3 C14 1.386(9) . . yes N3 C17 1.397(10) . . yes C1 C2 1.390(9) . . no C1 C6 1.377(9) . . no C2 C3 1.381(9) . . no C3 C4 1.377(10) . . no C3 C30 1.493(11) . . no C4 C5 1.378(10) . . no C5 C6 1.382(9) . . no C7 C8 1.405(8) . . no C7 C12 1.407(8) . 2_656 no C8 C9 1.385(10) . . no C9 C10 1.365(10) . . no C10 C11 1.377(9) . . no C11 C12 1.399(8) . 2_656 no C13 C14 1.426(9) . . no C14 C15 1.368(8) . . no C15 C16 1.328(8) . . no C16 C17 1.365(10) . . 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 N2 Zn N1 S 54.3(4) . . . . no N2 Zn N1 C7 -120.6(4) . . . . no N1 Zn N1 S -56.2(4) 2_656 . . . no N1 Zn N1 C7 129.0(4) 2_656 . . . no N2 Zn N1 S 174.5(3) 2_656 . . . no N2 Zn N1 C7 -0.4(4) 2_656 . . . no N1 Zn N2 C12 -130.7(3) . . . . no N1 Zn N2 C13 55.2(6) . . . . no N1 Zn N2 C12 0.6(3) 2_656 . . . no N1 Zn N2 C13 -173.6(5) 2_656 . . . no N2 Zn N2 C12 126.8(3) 2_656 . . . no N2 Zn N2 C13 -47.4(6) 2_656 . . . no O1 S N1 Zn -120.7(3) . . . . no O1 S N1 C7 53.7(5) . . . . no O2 S N1 Zn 7.4(4) . . . . no O2 S N1 C7 -178.2(4) . . . . no C6 S N1 Zn 121.9(3) . . . . no C6 S N1 C7 -63.7(5) . . . . no O1 S C6 C1 11.2(6) . . . . no O1 S C6 C5 -167.9(5) . . . . no O2 S C6 C1 -115.0(5) . . . . no O2 S C6 C5 65.9(6) . . . . no N1 S C6 C1 132.5(5) . . . . no N1 S C6 C5 -46.6(6) . . . . no Zn N1 C7 C8 179.4(5) . . . . no Zn N1 C7 C12 0.1(6) . . . 2_656 no S N1 C7 C8 4.5(8) . . . . no S N1 C7 C12 -174.8(4) . . . 2_656 no Zn N2 C12 C7 -0.7(6) . . . 2_656 no Zn N2 C12 C11 178.9(5) . . . 2_656 no C13 N2 C12 C7 174.3(5) . . . 2_656 no C13 N2 C12 C11 -6.1(8) . . . 2_656 no Zn N2 C13 C14 -5.1(10) . . . . no C12 N2 C13 C14 -178.9(6) . . . . no C17 N3 C14 C13 177.3(7) . . . . no C17 N3 C14 C15 -0.1(7) . . . . no C14 N3 C17 C16 0.6(8) . . . . no C6 C1 C2 C3 -0.4(10) . . . . no C2 C1 C6 S -179.1(5) . . . . no C2 C1 C6 C5 -0.1(9) . . . . no C1 C2 C3 C4 0.9(10) . . . . no C1 C2 C3 C30 -179.2(7) . . . . no C2 C3 C4 C5 -1.0(10) . . . . no C30 C3 C4 C5 179.2(7) . . . . no C3 C4 C5 C6 0.5(11) . . . . no C4 C5 C6 S 179.1(5) . . . . no C4 C5 C6 C1 0.0(10) . . . . no N1 C7 C8 C9 179.4(6) . . . . no C12 C7 C8 C9 -1.2(9) 2_656 . . . no N1 C7 C12 C11 -179.2(5) . . 2_656 . no N1 C7 C12 N2 0.4(7) . . 2_656 2_656 no C8 C7 C12 C11 1.4(8) . . 2_656 . no C8 C7 C12 N2 -179.0(5) . . 2_656 2_656 no C7 C8 C9 C10 1.0(10) . . . . no C8 C9 C10 C11 -0.8(10) . . . . no C9 C10 C11 C12 1.0(10) . . . 2_656 no C10 C11 C12 C7 -1.3(9) . . 2_656 . no C10 C11 C12 N2 179.1(6) . . 2_656 2_656 no N2 C13 C14 N3 0.8(12) . . . . no N2 C13 C14 C15 177.9(6) . . . . no N3 C14 C15 C16 -0.5(7) . . . . no C13 C14 C15 C16 -178.4(6) . . . . no C14 C15 C16 C17 0.9(8) . . . . no C15 C16 C17 N3 -0.9(8) . . . . no