#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/85/2008553.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_2008553 loop_ _publ_author_name 'Nakagawa, Hiroo' 'Kani, Yoshiyuki' 'Tsuchimoto, Masanobu' 'Ohba, Shigeru' 'Hideaki, Matsushima' 'Tokii, Tadashi' _publ_section_title ; A monomeric and a dimeric copper(II) trigonelline adduct with chloride, and a dimeric copper(II) 1-methyl-2-pyrrolecarboxylate adduct with 3-methylpyridine ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 882 _journal_page_last 886 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Cu Cl2 (C7 H7 N O2)2]' _chemical_formula_moiety 'C14 H14 Cl2 Cu N2 O4' _chemical_formula_structural 'Cu (C7 H7 N O2)2 Cl2' _chemical_formula_sum 'C14 H14 Cl2 Cu N2 O4' _chemical_formula_weight 408.73 _chemical_name_systematic ; Bis(trigonelline)-dichlorocopper(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_type_scat_source IntTabIV _cell_angle_alpha 90.00 _cell_angle_beta 104.960(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 8.4010(10) _cell_length_b 10.7040(10) _cell_length_c 9.3250(10) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295 _cell_measurement_theta_max 15 _cell_measurement_theta_min 14 _cell_volume 810.12(15) _computing_cell_refinement 'AFC/MSC Diffractometer Control System' _computing_data_collection 'AFC/MSC Diffractometer Control System (Rigaku Corporation, 1993)' _computing_data_reduction 'local programs' _computing_molecular_graphics CRYSTAN-GM _computing_publication_material CRYSTAN-GM _computing_structure_refinement CRYSTAN-GM _computing_structure_solution 'CRYSTAN-GM (Edwards et al., 1996)' _diffrn_measurement_device_type 'Rigaku AFC-5' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.041 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 2489 _diffrn_reflns_theta_max 30 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 100 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.697 _exptl_absorpt_correction_T_max 0.834 _exptl_absorpt_correction_T_min 0.539 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Coppens et al., 1965)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 414 _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _refine_diff_density_max 1.09 _refine_diff_density_min -0.55 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_obs 1.23 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 106 _refine_ls_number_reflns 1927 _refine_ls_R_factor_obs .044 _refine_ls_shift/esd_max 0.03 _refine_ls_shift/esd_mean 0.0059 _refine_ls_structure_factor_coef F _refine_ls_weighting_details 'w = 1/[\s^2^(F) + 0.000225F^2^]' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_obs .045 _reflns_number_observed 1927 _reflns_number_total 2348 _reflns_threshold_expression |F~o~|>3\s(|F~o~|) _[local]_cod_data_source_file da1057.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius The following automatic conversions were performed: '_atom_site_thermal_displace_type' tag value 'Uij' was replaced with 'Uani' value 12 times. Automatic conversion script Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana ; _cod_original_cell_volume 810.1(2) _cod_database_code 2008553 loop_ _symmetry_equiv_pos_as_xyz +x,+y,+z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z 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 Cu1 .0305(2) .02300(10) .02450(10) .00300(10) .00070(10) -.00350(10) Cl2 .0468(3) .0370(2) .0413(3) .0007(2) .0159(2) .0001(2) O3 .0393(7) .0241(6) .0357(7) .0055(5) -.0003(5) -.0053(5) O4 .0540(9) .0360(7) .0455(8) .0007(6) -.0138(7) -.0096(6) N5 .0340(7) .0278(7) .0282(7) -.0026(6) .0080(6) -.0019(5) C6 .0353(9) .0271(8) .0308(9) .0002(7) .0072(7) -.0022(7) C7 .0284(8) .0250(8) .0283(9) .0003(6) .0055(7) .0003(6) C8 .0334(9) .0353(9) .0340(10) .0018(8) .0027(7) .0023(8) C9 .0400(10) .0370(10) .0440(10) .0080(10) .0010(10) .0070(10) C10 .0430(10) .0260(10) .0430(10) .0060(10) .0090(10) .0040(10) C11 .0540(10) .0360(10) .0350(10) -.0070(10) .0010(10) -.0090(10) C12 .0310(9) .0270(8) .0274(9) .0021(7) .0074(7) .0016(7) 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_occupancy Cu1 1.00000 .00000 .00000 .02800(10) Uani 1.000 Cl2 .84175(6) -.07606(4) .14543(6) .0438(2) Uani 1.000 O3 .9775(2) .16860(10) .07100(10) .0358(4) Uani 1.000 O4 .7554(2) .16890(10) -.1191(2) .0493(5) Uani 1.000 N5 .9061(2) .53350(10) .1702(2) .0318(4) Uani 1.000 C6 .8514(2) .2197(2) -.0126(2) .0331(5) Uani 1.000 C7 .8249(2) .3552(2) .0205(2) .0285(5) Uani 1.000 C8 .7021(2) .4248(2) -.0741(2) .0354(6) Uani 1.000 C9 .6858(2) .5499(2) -.0443(2) .0413(7) Uani 1.000 C10 .7888(2) .6025(2) .0807(2) .0388(6) Uani 1.000 C11 1.0110(3) .5913(2) .3072(2) .0457(7) Uani 1.000 C12 .9262(2) .4119(2) .1435(2) .0296(5) Uani 1.000 H8 .62913 .38589 -.15870 .10 Uiso 1.000 H9 .60346 .60014 -.10979 .10 Uiso 1.000 H10 .77659 .68874 .10420 .10 Uiso 1.000 H11A 1.09530 .54128 .37066 .10 Uiso 1.000 H11B .93870 .61898 .36536 .10 Uiso 1.000 H11C 1.06410 .66258 .27756 .10 Uiso 1.000 H12 1.01109 .36452 .20995 .10 Uiso 1.000 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 Cu1 Cl2 . . 2.2800(10) yes Cu1 O3 . . 1.948(2) yes Cu1 O4 . . 2.7470(10) yes O3 C6 . . 1.266(3) yes O4 C6 . . 1.232(3) yes N5 C10 . . 1.337(3) no N5 C11 . . 1.486(3) no N5 C12 . . 1.344(3) no C6 C7 . . 1.511(3) no C7 C8 . . 1.388(3) no C7 C12 . . 1.380(3) no C8 C9 . . 1.382(3) no C9 C10 . . 1.380(3) no C8 H8 . . .960 no C9 H9 . . .960 no C10 H10 . . .960 no C11 H11A . . .960 no C11 H11B . . .960 no C11 H11C . . .960 no C12 H12 . . .960 no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl2 Cu1 O3 90.40(10) yes Cl2 Cu1 O4 89.2(2) yes O3 Cu1 O4 53.10(10) yes Cu1 O3 C6 109.3(2) yes C10 N5 C11 119.0(2) no C10 N5 C12 121.8(2) no C11 N5 C12 119.1(2) no O3 C6 O4 125.1(2) yes O3 C6 C7 115.6(2) no O4 C6 C7 119.2(2) no C6 C7 C8 120.6(2) no C6 C7 C12 120.0(2) no C8 C7 C12 119.3(2) no C7 C8 C9 119.2(2) no C8 C9 C10 119.5(2) no N5 C10 C9 120.1(2) no N5 C12 C7 120.0(2) no C7 C8 H8 120.1 no C9 C8 H8 120.7 no C8 C9 H9 120.5 no C10 C9 H9 120.0 no N5 C10 H10 119.6 no C9 C10 H10 120.3 no N5 C11 H11A 118.5 no N5 C11 H11B 107.0 no N5 C11 H11C 107.5 no H11A C11 H11B 107.3 no H11A C11 H11C 107.3 no H11B C11 H11C 109.0 no N5 C12 H12 120.0 no C7 C12 H12 120.0 no