#------------------------------------------------------------------------------ #$Date: 2020-02-12 12:42:01 +0200 (Wed, 12 Feb 2020) $ #$Revision: 248077 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/73/1557308.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_1557308 loop_ _publ_author_name 'Kivekas, Raikko' 'Pajunen, Aarne' 'Colacio, Enrique' 'Dominguez-Vera, Jose M.' 'Moreno, Jose Maria' 'Romerosa, Antonio' _publ_section_title ; Structural Characterization of Closely Related Mononuclear CuII Complexes of 5-Nitrosooxime Pyrimidines. A Combined X-Ray and EPR Study ; _journal_name_full 'Acta Chemica Scandinavica' _journal_page_first 1051 _journal_page_last 1057 _journal_paper_doi 10.3891/acta.chem.scand.51-1051 _journal_volume 51 _journal_year 1997 _chemical_formula_sum 'C16 H19 Cl Cu N6 O9' _chemical_formula_weight 538.36 _chemical_name_common ; [Cu(1L)(bipy)(H2O)]ClO4.H2O ; _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90. _cell_angle_beta 93.49(3) _cell_angle_gamma 90. _cell_formula_units_Z 4 _cell_length_a 7.915(2) _cell_length_b 13.165(3) _cell_length_c 20.065(4) _cell_volume 2086.9(8) _diffrn_ambient_temperature 293 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu 1.239 _exptl_crystal_density_diffrn 1.713 _exptl_crystal_F_000 1100 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_number_parameters 314 _refine_ls_number_reflns 1965 _refine_ls_R_factor_gt 0.0743 _refine_ls_wR_factor_gt 0.1581 _cod_data_source_file Acta-Chem-Scand-1997-51-1051-1.cif _cod_data_source_block 1 _cod_depositor_comments ; The paper contains selected atomic coordinates...! ; _cod_original_sg_symbol_H-M 'P 21/c' _cod_database_code 1557308 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,1/2+y,1/2-z 3 -x,-y,-z 4 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 Cu1 Cu Uiso 0.21210(10) 0.06590(10) 0.22440(10) 1.000 0.0330(10) . . . . O5A O Uiso 0.3001(19) 0.2764(10) 0.2652(6) 0.43(2) 0.027(5) . . . . O5B O Uiso 0.2282(15) 0.1982(9) 0.2673(6) 0.57(2) 0.048(4) . . . . O19 O Uiso 0.4351(8) 0.0913(5) 0.1614(3) 1.000 0.044(2) . . . . N5A N Uiso 0.208(2) 0.2226(13) 0.2243(10) 0.43(2) 0.030(5) . . . . N5B N Uiso 0.189(2) 0.2806(12) 0.2411(7) 0.57(2) 0.042(4) . . . . N6 N Uiso 0.0302(10) 0.1059(6) 0.1611(4) 1.000 0.041(2) . . . . N7 N Uiso 0.2087(9) -0.0849(5) 0.2080(3) 1.000 0.026(2) . . . . N18 N Uiso 0.3591(8) 0.0222(5) 0.3041(3) 1.000 0.032(2) . . . . O2 O Uiso -0.1990(8) 0.3526(5) 0.0190(3) 1.000 0.042(2) . . . . C5 C Uiso 0.0980(10) 0.2784(7) 0.1816(4) 1.000 0.034(2) . . . . C6 C Uiso 0.0073(11) 0.1997(7) 0.1442(4) 1.000 0.033(2) . . . . C12 C Uiso 0.2986(11) -0.1382(6) 0.2536(4) 1.000 0.031(2) . . . . C13 C Uiso 0.3851(11) -0.0805(7) 0.3088(4) 1.000 0.032(2) . . . . O4 O Uiso 0.1392(9) 0.4550(5) 0.1979(3) 1.000 0.057(2) . . . . O20 O Uiso 0.2971(10) 0.4639(5) 0.3314(3) 1.000 0.051(2) . . . . 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' Cu Cu 0.3201 1.2651 ' 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 O5B Cu1 O19 94.8(4) . . . yes O5B Cu1 N5B 20.5(5) . . . yes O5B Cu1 N6 94.2(4) . . . yes O5B Cu1 N7 163.0(4) . . . yes O5B Cu1 N18 83.4(4) . . . yes O19 Cu1 N5B 88.7(4) . . . yes O19 Cu1 N6 99.7(3) . . . yes O19 Cu1 N7 93.3(3) . . . yes O19 Cu1 N18 93.1(2) . . . yes O19 Cu1 N5A 82.2(5) . . . yes N5B Cu1 N6 75.9(4) . . . yes N5B Cu1 N7 175.0(4) . . . yes N5B Cu1 N18 103.2(4) . . . yes N6 Cu1 N7 99.2(3) . . . yes N6 Cu1 N18 167.2(3) . . . yes N5A Cu1 N6 73.5(6) . . . yes N7 Cu1 N18 81.3(3) . . . yes N5A Cu1 N7 170.5(6) . . . yes N5A Cu1 N18 107.2(6) . . . yes Cu1 O5B N5B 126.1(11) . . . yes O5A N5A C5 114.4(14) . . . yes Cu1 N5A O5A 123.0(13) . . . yes Cu1 N5A C5 122.5(12) . . . yes Cu1 N5B O5B 33.4(7) . . . yes Cu1 N5B C5 84.8(8) . . . yes O5B N5B C5 117.5(14) . . . yes Cu1 N6 C6 121.3(6) . . . yes Cu1 N7 C12 114.1(5) . . . yes Cu1 N18 C13 114.6(5) . . . yes N5A C5 C6 102.3(10) . . . yes N5B C5 C6 133.9(10) . . . yes N6 C6 C5 119.5(8) . . . yes N7 C12 C13 116.8(7) . . . yes N18 C13 C12 113.3(7) . . . 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 Cu1 O5B 1.944(12) . . yes Cu1 O19 2.258(6) . . yes Cu1 N5B 2.854(16) . . yes Cu1 N6 1.934(8) . . yes Cu1 N7 2.012(7) . . yes Cu1 N18 2.004(6) . . yes Cu1 N5A 2.063(17) . . yes O5A N5A 1.28(2) . . yes O5B N5B 1.24(2) . . yes N5A C5 1.39(2) . . yes N5B C5 1.357(17) . . yes N6 C6 1.291(12) . . yes N7 C12 1.325(10) . . yes N18 C13 1.370(11) . . yes C5 C6 1.444(12) . . no C12 C13 1.477(12) . . 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 O19 Cu1 O5B N5B 73.2(13) . . . . no N6 Cu1 O5B N5B -26.9(13) . . . . no N18 Cu1 O5B N5B 165.8(13) . . . . no O5B Cu1 N5B C5 -168.4(18) . . . . no O19 Cu1 N5B O5B -107.4(13) . . . . no O19 Cu1 N5B C5 84.2(7) . . . . no N6 Cu1 N5B O5B 152.3(14) . . . . no N6 Cu1 N5B C5 -16.1(7) . . . . no N18 Cu1 N5B O5B -14.5(14) . . . . no N18 Cu1 N5B C5 177.1(7) . . . . no O5B Cu1 N6 C6 24.6(8) . . . . no O19 Cu1 N6 C6 -71.0(7) . . . . no N5B Cu1 N6 C6 15.2(7) . . . . no N7 Cu1 N6 C6 -166.0(7) . . . . no O19 Cu1 N7 C12 92.3(6) . . . . no N6 Cu1 N7 C12 -167.4(6) . . . . no N18 Cu1 N7 C12 -0.3(6) . . . . no O5B Cu1 N18 C13 172.9(7) . . . . no O19 Cu1 N18 C13 -92.7(6) . . . . no N5B Cu1 N18 C13 177.9(6) . . . . no N7 Cu1 N18 C13 0.2(6) . . . . no Cu1 O5B N5B C5 13(2) . . . . no Cu1 N5B C5 C6 19.8(12) . . . . no O5B N5B C5 C6 13(2) . . . . no Cu1 N6 C6 C5 -11.4(11) . . . . no Cu1 N7 C12 C13 0.4(9) . . . . no Cu1 N18 C13 C12 0.0(9) . . . . no N5B C5 C6 N6 -13.3(17) . . . . no N7 C12 C13 N18 -0.3(11) . . . . no