#------------------------------------------------------------------------------ #$Date: 2020-01-15 17:13:04 +0200 (Wed, 15 Jan 2020) $ #$Revision: 246865 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/70/1557048.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_1557048 loop_ _publ_author_name 'Roman, Pascual' 'Guzman-Miralles, Carmen' 'Luque, Antonio' 'Beitia, Javier I.' _publ_section_title ; Synthesis, Crystal Structure and Thermal Behaviour of the Diethylenetriammonium Oxalate-Water (1/4), (H3dien)2(ox)3.4H2O ; _journal_name_full 'Acta Chemica Scandinavica' _journal_page_first 13 _journal_page_last 18 _journal_paper_doi 10.3891/acta.chem.scand.51-0013 _journal_volume 51 _journal_year 1997 _chemical_formula_sum 'C14 H40 N6 O16' _chemical_formula_weight 548.50 _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 66.02(5) _cell_angle_beta 71.95(6) _cell_angle_gamma 86.70(3) _cell_formula_units_Z 1 _cell_length_a 8.626(3) _cell_length_b 9.361(1) _cell_length_c 9.385(1) _cell_volume 656.3(4) _diffrn_ambient_temperature 293 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 0.1177 _exptl_crystal_density_diffrn 1.39 _exptl_crystal_F_000 294 _refine_ls_goodness_of_fit_ref 1.20 _refine_ls_number_parameters 227 _refine_ls_number_reflns 2846 _refine_ls_R_factor_gt 0.072 _refine_ls_wR_factor_gt 0.085 _cod_data_source_file Acta-Chem-Scand-1997-51-13.cif _cod_data_source_block 1 _cod_original_cell_volume 656.3(2) _cod_database_code 1557048 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 N1 N Uiso 0.6459(2) 0.4033(2) -0.1584(2) 1.000 0.0309(7) . . . . N4 N Uiso 0.7943(2) 0.1022(2) 0.1745(2) 1.000 0.0286(7) . . . . N7 N Uiso 0.8257(3) -0.2424(2) 0.4237(3) 1.000 0.0375(8) . . . . C2 C Uiso 0.7500(3) 0.2804(3) -0.0847(3) 1.000 0.0349(8) . . . . C3 C Uiso 0.6875(3) 0.2215(3) 0.0997(3) 1.000 0.0347(8) . . . . C5 C Uiso 0.7259(3) 0.0282(3) 0.3571(3) 1.000 0.0388(9) . . . . C6 C Uiso 0.8366(3) -0.0892(3) 0.4370(3) 1.000 0.0401(10) . . . . O10 O Uiso 0.1242(2) 0.1495(2) -0.0777(2) 1.000 0.0454(9) . . . . O20 O Uiso 0.3888(3) 0.1702(4) -0.1066(4) 1.000 0.0802(18) . . . . O30 O Uiso 0.3226(2) 0.3539(2) 0.0651(2) 1.000 0.0436(9) . . . . O40 O Uiso 0.0588(2) 0.2685(2) 0.1548(2) 1.000 0.0467(9) . . . . C10 C Uiso 0.2440(3) 0.1928(3) -0.0504(3) 1.000 0.0333(8) . . . . O11 O Uiso 0.5088(2) 0.3508(2) 0.4283(3) 1.000 0.0471(9) . . . . C20 C Uiso 0.2047(2) 0.2799(2) 0.0667(3) 1.000 0.0292(7) . . . . O21 O Uiso 0.6874(2) 0.4250(2) 0.5208(2) 1.000 0.0451(9) . . . . Ow1 O Uiso 1.0066(2) 0.4158(2) 0.3634(2) 1.000 0.0420(8) . . . . C11 C Uiso 0.5566(2) 0.4352(3) 0.4842(2) 1.000 0.0316(8) . . . . Ow2 O Uiso 0.6821(4) 0.0726(3) 0.7010(3) 1.000 0.0786(15) . . . . 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' 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 C3 N4 C5 111.60(19) . . . yes N1 C2 C3 109.7(2) . . . yes N4 C3 C2 110.1(2) . . . yes N4 C5 C6 112.6(2) . . . yes N7 C6 C5 112.6(2) . . . yes O10 C10 O20 125.5(3) . . . yes O10 C10 C20 116.9(2) . . . yes O20 C10 C20 117.7(3) . . . yes O30 C20 O40 125.8(2) . . . yes O30 C20 C10 116.9(2) . . . yes O40 C20 C10 117.3(2) . . . yes O11 C11 O21 126.1(2) . . . yes O11 C11 C11 117.95(18) . . 2_666 yes O21 C11 C11 116.0(2) . . 2_666 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 N1 C2 1.493(3) . . yes N4 C3 1.495(3) . . yes N4 C5 1.490(3) . . yes N7 C6 1.500(4) . . yes C2 C3 1.507(3) . . no C5 C6 1.528(4) . . no O10 C10 1.263(3) . . yes O20 C10 1.239(4) . . yes O30 C20 1.256(3) . . yes O40 C20 1.256(3) . . yes C10 C20 1.566(4) . . no O11 C11 1.256(3) . . yes O21 C11 1.265(3) . . yes C11 C11 1.578(4) . 2_666 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 C5 N4 C3 C2 -173.6(2) . . . . no C3 N4 C5 C6 -177.5(2) . . . . no N1 C2 C3 N4 -178.1(2) . . . . no N4 C5 C6 N7 -76.9(3) . . . . no O10 C10 C20 O30 -164.2(2) . . . . no O10 C10 C20 O40 16.4(3) . . . . no O20 C10 C20 O30 16.7(4) . . . . no O20 C10 C20 O40 -162.6(3) . . . . no O11 C11 C11 O11 -180.0(2) . . 2_666 2_666 no O11 C11 C11 O21 -1.1(3) . . 2_666 2_666 no O21 C11 C11 O11 1.1(3) . . 2_666 2_666 no O21 C11 C11 O21 180.0(2) . . 2_666 2_666 no