#------------------------------------------------------------------------------ #$Date: 2012-02-03 19:16:24 +0200 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012487.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_2012487 loop_ _publ_author_name 'Ercan, Ismail' 'Ercan, Filiz' 'Arici, Cengiz' 'Atakol, Orhan' _publ_section_title Bis{[\m-N,N'-bis(salicylidene)-1,4-butanediamine-N,N',O,O'-copper(II)]-\m-chloro-chloromercury(II)} _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m137 _journal_page_last m138 _journal_volume 58 _journal_year 2002 _chemical_formula_analytical 'C18.28 H18.60 Cl2.02 Cu1.00 Hg N2.04 O2' _chemical_formula_iupac '[(Cu Hg Cl2)2(C18 H18 N2 O2)2]' _chemical_formula_moiety 'C36 H36 Cl4 Cu2 Hg2 N4 O4' _chemical_formula_sum 'C36 H36 Cl4 Cu2 Hg2 N4 O4' _chemical_formula_weight 1258.74 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_type_scat_source IntTabIV _cell_angle_alpha 72.440(2) _cell_angle_beta 69.285(3) _cell_angle_gamma 73.023(3) _cell_formula_units_Z 1 _cell_length_a 8.9927(12) _cell_length_b 9.4979(13) _cell_length_c 13.0245(14) _cell_measurement_reflns_used 25 _cell_measurement_temperature 301(2) _cell_measurement_theta_max 18.08 _cell_measurement_theta_min 10.22 _cell_volume 970.4(2) _computing_cell_refinement 'SHELXL97 (Sheldrick, 1997b)' _computing_data_collection 'CAD-4 EXPRESS(Enraf-Nonius, 1993)' _computing_molecular_graphics 'ORTEP(II) (Johnson, 1976)' _computing_publication_material 'SHELXL97 (Sheldrick, 1997b)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997b)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997a)' _diffrn_measurement_device 'CAD-4 EXPRESS (Enraf-Nonius, 1993)' _diffrn_measurement_method '\w/2\q scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .036 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 4114 _diffrn_reflns_theta_max 26.29 _diffrn_standards_decay_% .287 _diffrn_standards_interval_time 120 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 9.287 _exptl_absorpt_correction_T_max .4569 _exptl_absorpt_correction_T_min .2581 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details 'empirical via \y scans (Fair, 1990)' _exptl_crystal_colour 'dark brown' _exptl_crystal_density_diffrn 2.154 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prism _exptl_crystal_size_max .20 _exptl_crystal_size_mid .15 _exptl_crystal_size_min .10 _refine_diff_density_max .922 _refine_diff_density_min -.188 _refine_ls_extinction_coef .0026(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment 'see text' _refine_ls_matrix_type full _refine_ls_number_parameters 236 _refine_ls_number_reflns 3932 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt .0570 _refine_ls_shift/su_max .003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1197P)^2^+0.1203P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .1487 _reflns_number_gt 3482 _reflns_number_total 3932 _reflns_threshold_expression I>2sigma(I) _[local]_cod_data_source_file br1346.cif _[local]_cod_data_source_block I _cod_database_code 2012487 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol Cu .43513(11) 1.01273(9) .74407(8) .0309(2) Ueq . . Cu Hg .52245(4) .61512(3) .82450(2) .03813(18) Ueq . . Hg N1 .4372(8) 1.1446(7) .8376(6) .0335(13) Ueq . . N N2 .3329(8) 1.1690(7) .6379(6) .0368(14) Ueq . . N O1 .5871(7) .8521(6) .8092(6) .0423(13) Ueq . . O O2 .3962(7) .8529(6) .7014(5) .0364(12) Ueq . . O C1 .7126(9) .8761(9) .8245(6) .0341(16) Ueq . . C C2 .8572(10) .7649(10) .8169(7) .0420(18) Ueq . . C H2 .8634 .6734 .7987 .050 Uiso . . H C3 .9910(10) .7865(12) .8356(8) .049(2) Ueq . . C H3 1.0883 .7112 .8278 .059 Uiso . . H C4 .9836(12) .9155(12) .8650(9) .054(2) Ueq . . C H4 1.0745 .9285 .8796 .064 Uiso . . H C5 .8444(12) 1.0263(11) .8735(8) .049(2) Ueq . . C H5 .8405 1.1157 .8938 .059 Uiso . . H C6 .7081(10) 1.0102(9) .8529(7) .0365(17) Ueq . . C C7 .5621(11) 1.1275(9) .8671(7) .0394(17) Ueq . . C H7 .5600 1.2015 .9033 .047 Uiso . . H C8 .2993(11) 1.2670(11) .8772(8) .049(2) Ueq . . C H8A .2696 1.2465 .9603 .058 Uiso . . H H8B .3369 1.3636 .8471 .058 Uiso . . H C9 .1510(10) 1.2858(10) .8445(8) .046(2) Ueq . . C H9A .0559 1.3346 .8984 .056 Uiso . . H H9B .1345 1.1847 .8504 .056 Uiso . . H C10 .1582(12) 1.3805(10) .7242(9) .051(2) Ueq . . C H10A .0633 1.3751 .7047 .062 Uiso . . H H10B .1496 1.4873 .7228 .062 Uiso . . H C11 .3125(11) 1.3294(9) .6353(8) .0423(19) Ueq . . C H11A .3068 1.3910 .5599 .051 Uiso . . H H11B .4074 1.3446 .6493 .051 Uiso . . H C12 .2821(10) 1.1441(9) .5667(7) .0407(18) Ueq . . C H12 .2383 1.2306 .5182 .049 Uiso . . H C13 .2835(9) 1.0001(9) .5511(6) .0348(16) Ueq . . C C14 .2233(11) 1.0012(11) .4647(7) .0432(19) Ueq . . C H14 .1860 1.0953 .4196 .052 Uiso . . H C15 .2171(12) .8712(12) .4439(8) .049(2) Ueq . . C H15 .1750 .8737 .3858 .059 Uiso . . H C16 .2742(13) .7344(11) .5101(8) .049(2) Ueq . . C H16 .2712 .6427 .4964 .059 Uiso . . H C17 .3346(11) .7289(9) .5947(7) .0402(18) Ueq . . C H17 .3736 .6335 .6376 .048 Uiso . . H C18 .3398(9) .8611(9) .6192(7) .0323(15) Ueq . . C Cl1 .3030(3) .6226(3) .9871(2) .0550(6) Ueq . . Cl Cl2 .7183(4) .4980(3) .6866(2) .0641(7) Ueq . . Cl 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 _atom_site_aniso_type_symbol C1 .039(4) .032(4) .034(4) -.007(3) -.013(3) -.010(3) C C2 .045(4) .034(4) .047(5) -.018(4) -.014(4) .000(3) C C3 .033(4) .056(6) .053(5) -.016(4) -.012(3) .001(4) C C4 .045(5) .057(6) .071(7) -.016(5) -.022(4) -.021(4) C C5 .057(5) .047(5) .058(6) -.018(4) -.023(4) -.019(4) C C6 .045(4) .030(4) .037(4) -.009(3) -.010(3) -.013(3) C C7 .053(5) .031(4) .041(4) -.014(3) -.014(4) -.013(3) C C8 .056(5) .039(5) .049(5) -.020(4) -.007(4) -.007(4) C C9 .043(4) .034(4) .053(5) -.015(4) .000(4) -.007(4) C C10 .054(5) .028(4) .069(6) -.014(4) -.020(5) .002(4) C C11 .061(5) .016(3) .047(5) -.003(3) -.017(4) -.005(3) C C12 .046(4) .029(4) .041(4) -.006(3) -.014(3) -.001(3) C C13 .041(4) .031(4) .031(4) -.006(3) -.011(3) -.007(3) C C14 .051(5) .042(5) .034(4) -.001(3) -.014(3) -.011(4) C C15 .062(5) .056(6) .040(5) -.014(4) -.020(4) -.017(5) C C16 .070(6) .042(5) .047(5) -.016(4) -.017(4) -.022(4) C C17 .060(5) .024(4) .041(4) -.003(3) -.019(4) -.014(3) C C18 .032(3) .027(4) .039(4) -.005(3) -.010(3) -.011(3) C Cl1 .0478(12) .0631(15) .0454(12) -.0090(11) -.0130(9) -.0026(11) C Cl2 .0762(17) .0590(16) .0526(14) -.0295(12) -.0198(12) .0114(13) C Cu .0390(5) .0195(4) .0374(5) -.0077(4) -.0143(4) -.0054(3) Cu Hg .0486(2) .0258(2) .0430(2) -.01005(14) -.01545(15) -.00712(14) Hg N1 .044(4) .020(3) .039(4) -.009(3) -.014(3) -.004(3) N N2 .048(4) .022(3) .039(4) -.007(3) -.011(3) -.007(3) N O1 .054(3) .022(3) .064(4) -.014(3) -.034(3) -.002(2) O O2 .052(3) .020(2) .043(3) -.002(2) -.025(3) -.007(2) O loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 O1 . . 1.304(9) no C1 C2 . . 1.409(11) no C1 C6 . . 1.416(11) no C2 C3 . . 1.389(13) no C2 H2 . . .9500 no C3 C4 . . 1.368(14) no C3 H3 . . .9500 no C4 C5 . . 1.375(14) no C4 H4 . . .9500 no C5 C6 . . 1.402(12) no C5 H5 . . .9500 no C6 C7 . . 1.449(12) no C7 N1 . . 1.263(11) no C7 H7 . . .9500 no C8 C9 . . 1.486(13) no C8 N1 . . 1.491(11) no C8 H8A . . .9900 no C8 H8B . . .9900 no C9 C10 . . 1.543(13) no C9 H9A . . .9900 no C9 H9B . . .9900 no C10 C11 . . 1.520(13) no C10 H10A . . .9900 no C10 H10B . . .9900 no C11 N2 . . 1.471(9) no C11 H11A . . .9900 no C11 H11B . . .9900 no C12 N2 . . 1.274(11) no C12 C13 . . 1.438(12) no C12 H12 . . .9500 no C13 C14 . . 1.408(11) no C13 C18 . . 1.416(11) no C14 C15 . . 1.362(13) no C14 H14 . . .9500 no C15 C16 . . 1.394(14) no C15 H15 . . .9500 no C16 C17 . . 1.372(12) no C16 H16 . . .9500 no C17 C18 . . 1.403(11) no C17 H17 . . .9500 no C18 O2 . . 1.313(10) no Hg Cl1 . . 2.331(2) yes Hg Cl1 . 2_667 3.2997(17) yes Hg Cl2 . . 2.321(2) yes Hg O1 . . 2.420(5) yes Hg O2 . . 2.562(5) yes Cu O1 . . 1.933(6) yes Cu O2 . . 1.921(5) yes Cu N1 . . 2.001(6) yes Cu N2 . . 1.955(7) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle _geom_angle_publ_flag O1 C1 C2 . 120.3(7) no O1 C1 C6 . 122.1(7) no C2 C1 C6 . 117.5(7) no C3 C2 C1 . 121.4(8) no C3 C2 H2 . 119.3 no C1 C2 H2 . 119.3 no C4 C3 C2 . 120.4(8) no C4 C3 H3 . 119.8 no C2 C3 H3 . 119.8 no C3 C4 C5 . 119.9(8) no C3 C4 H4 . 120.0 no C5 C4 H4 . 120.0 no C4 C5 C6 . 121.4(9) no C4 C5 H5 . 119.3 no C6 C5 H5 . 119.3 no C5 C6 C1 . 119.4(8) no C5 C6 C7 . 119.3(8) no C1 C6 C7 . 121.1(7) no N1 C7 C6 . 128.6(7) no N1 C7 H7 . 115.7 no C6 C7 H7 . 115.7 no C9 C8 N1 . 115.3(8) no C9 C8 H8A . 108.5 no N1 C8 H8A . 108.5 no C9 C8 H8B . 108.5 no N1 C8 H8B . 108.5 no H8A C8 H8B . 107.5 no C8 C9 C10 . 113.8(8) no C8 C9 H9A . 108.8 no C10 C9 H9A . 108.8 no C8 C9 H9B . 108.8 no C10 C9 H9B . 108.8 no H9A C9 H9B . 107.7 no C11 C10 C9 . 113.7(7) no C11 C10 H10A . 108.8 no C9 C10 H10A . 108.8 no C11 C10 H10B . 108.8 no C9 C10 H10B . 108.8 no H10A C10 H10B . 107.7 no N2 C11 C10 . 110.4(7) no N2 C11 H11A . 109.6 no C10 C11 H11A . 109.6 no N2 C11 H11B . 109.6 no C10 C11 H11B . 109.6 no H11A C11 H11B . 108.1 no N2 C12 C13 . 127.5(7) no N2 C12 H12 . 116.3 no C13 C12 H12 . 116.3 no C14 C13 C18 . 120.0(8) no C14 C13 C12 . 117.0(7) no C18 C13 C12 . 123.0(7) no C15 C14 C13 . 121.8(8) no C15 C14 H14 . 119.1 no C13 C14 H14 . 119.1 no C14 C15 C16 . 118.2(8) no C14 C15 H15 . 120.9 no C16 C15 H15 . 120.9 no C17 C16 C15 . 121.7(8) no C17 C16 H16 . 119.2 no C15 C16 H16 . 119.2 no C16 C17 C18 . 121.3(8) no C16 C17 H17 . 119.3 no C18 C17 H17 . 119.3 no O2 C18 C17 . 120.2(7) no O2 C18 C13 . 122.7(7) no C17 C18 C13 . 117.1(7) no O2 Cu O1 . 83.6(2) yes O2 Cu N2 . 92.6(3) no O1 Cu N2 . 163.3(3) no O2 Cu N1 . 161.3(3) no O1 Cu N1 . 90.1(2) no N2 Cu N1 . 98.1(3) yes Cl2 Hg Cl1 . 153.80(12) yes Cl2 Hg O1 . 108.68(18) yes Cl1 Hg O1 . 96.99(18) yes Cl1 Hg O1 2_667 103.40(3) yes Cl2 Hg O2 . 100.32(15) yes Cl1 Hg O2 . 96.17(15) yes Cl1 Hg O2 2_667 164.36(3) yes Cl1 Hg Cl1 2_667 79.96(3) yes Cl1 Hg Cl2 2_667 88.92(3) yes O1 Hg O2 . 62.04(18) yes C7 N1 C8 . 115.1(7) no C7 N1 Cu . 120.1(5) no C8 N1 Cu . 124.8(5) no C12 N2 C11 . 115.1(7) no C12 N2 Cu . 124.9(6) no C11 N2 Cu . 120.0(6) no C1 O1 Cu . 122.5(5) no C1 O1 Hg . 129.2(5) no Cu O1 Hg . 107.7(2) no C18 O2 Cu . 128.8(5) no C18 O2 Hg . 127.8(5) no Cu O2 Hg . 102.8(2) no