#------------------------------------------------------------------------------ #$Date: 2013-08-29 16:37:19 +0100 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/36/2203692.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_2203692 loop_ _publ_author_name 'Jian Zhang' 'Yao Kang' 'Yi-Hang Wen' 'Zhao-Ji Li' 'Ye-Yan Qin' 'Yuan-Gen Yao' _publ_section_title ; Dichlorobis[2-(chloromethyl)pyridine]copper(II) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m599 _journal_page_last m600 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Cu Cl2 (C12 H12 Cl2 N2)]' _chemical_formula_moiety 'C12 H12 Cl4 Cu N2' _chemical_formula_sum 'C12 H12 Cl4 Cu N2' _chemical_formula_weight 389.58 _chemical_name_systematic ; dichlorobis(2-chloromethylpyridine)copper(II) ; _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 117.311(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.292(2) _cell_length_b 7.7844(11) _cell_length_c 14.306(2) _cell_measurement_reflns_used 1734 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.0 _cell_measurement_theta_min 3.0 _cell_volume 1513.1(4) _computing_cell_refinement 'SMART and SAINT (Siemens,1994)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_data_reduction 'XPREP in SHELXTL (Siemens, 1994)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement SHELXTL _computing_structure_solution SHELXTL _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Bruker SMART CCD area-detector' _diffrn_measurement_method '\f and \w' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.027 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 2252 _diffrn_reflns_theta_full 25.0 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_theta_min 3.0 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.13 _exptl_absorpt_correction_T_max 0.626 _exptl_absorpt_correction_T_min .435 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.710 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 780 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.74 _refine_diff_density_min -0.69 _refine_ls_extinction_coef 0.0122(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXTL _refine_ls_goodness_of_fit_ref 1.08 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 1324 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.08 _refine_ls_R_factor_gt 0.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0661P)^2^+3.161P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.101 _refine_ls_wR_factor_ref 0.110 _reflns_number_gt 1187 _reflns_number_total 1324 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ya6203.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _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: '_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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_cell_volume 1513.2(4) _cod_database_code 2203692 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cu1 0.2500 0.2500 0.0000 0.0294(3) Uani d S 1 Cu Cl2 0.25899(6) 0.52023(11) 0.06378(7) 0.0403(3) Uani d . 1 Cl Cl1 0.36172(7) 0.11129(15) 0.21919(8) 0.0577(4) Uani d . 1 Cl N1 0.14710(19) 0.1955(4) 0.0458(2) 0.0311(6) Uani d . 1 N C1 0.1603(3) 0.0943(4) 0.1270(3) 0.0355(7) Uani d . 1 C C2 0.0876(3) 0.0795(5) 0.1588(3) 0.0473(9) Uani d . 1 C H2A 0.0983 0.0111 0.2164 0.057 Uiso calc R 1 H C5 0.0611(3) 0.2784(5) -0.0059(3) 0.0375(8) Uani d . 1 C H5A 0.0519 0.3480 -0.0625 0.045 Uiso calc R 1 H C3 -0.0002(3) 0.1650(6) 0.1058(3) 0.0534(10) Uani d . 1 C H3A -0.0492 0.1553 0.1269 0.064 Uiso calc R 1 H C4 -0.0141(3) 0.2645(5) 0.0216(4) 0.0466(10) Uani d . 1 C H4A -0.0733 0.3220 -0.0167 0.056 Uiso calc R 1 H C6 0.2513(3) -0.0130(5) 0.1793(3) 0.0442(9) Uani d . 1 C H6A 0.2495 -0.1023 0.1311 0.053 Uiso calc R 1 H H6B 0.2524 -0.0684 0.2406 0.053 Uiso calc R 1 H 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 0.0244(4) 0.0336(4) 0.0335(4) 0.0003(2) 0.0162(3) 0.0018(2) Cl2 0.0380(5) 0.0385(5) 0.0500(5) -0.0030(3) 0.0250(4) -0.0057(4) Cl1 0.0340(5) 0.0728(8) 0.0537(6) 0.0005(4) 0.0093(4) 0.0079(5) N1 0.0276(13) 0.0350(14) 0.0346(14) -0.0003(11) 0.0176(11) -0.0005(12) C1 0.0352(17) 0.0355(18) 0.0378(17) -0.0038(14) 0.0184(14) -0.0013(14) C2 0.047(2) 0.057(2) 0.048(2) -0.0090(18) 0.0304(18) -0.0029(18) C5 0.0280(17) 0.0389(19) 0.0449(19) 0.0038(14) 0.0161(15) -0.0019(15) C3 0.037(2) 0.071(3) 0.066(3) -0.013(2) 0.0356(19) -0.011(2) C4 0.0272(18) 0.052(2) 0.062(3) -0.0003(15) 0.0213(17) -0.0122(18) C6 0.045(2) 0.044(2) 0.0447(19) 0.0023(16) 0.0215(16) 0.0115(16) 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' H H 0.0000 0.0000 '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' Cl Cl 0.1484 0.1585 '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' 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_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 Cu1 N1 . 7 180.00(11) no N1 Cu1 Cl2 . . 88.65(8) yes N1 Cu1 Cl2 7 . 91.35(8) no N1 Cu1 Cl2 . 7 91.35(8) no N1 Cu1 Cl2 7 7 88.65(8) no Cl2 Cu1 Cl2 . 7 180.00(4) no N1 Cu1 Cl1 . . 74.84(8) yes N1 Cu1 Cl1 7 . 105.16(8) no Cl2 Cu1 Cl1 . . 90.74(3) yes Cl2 Cu1 Cl1 7 . 89.26(3) no C6 Cl1 Cu1 . . 81.98(12) no C1 N1 C5 . . 118.7(3) no C1 N1 Cu1 . . 125.4(2) no C5 N1 Cu1 . . 115.8(2) no N1 C1 C2 . . 120.7(3) no N1 C1 C6 . . 119.8(3) no C2 C1 C6 . . 119.4(3) no C3 C2 C1 . . 120.4(4) no C3 C2 H2A . . 119.8 no C1 C2 H2A . . 119.8 no N1 C5 C4 . . 122.6(4) no N1 C5 H5A . . 118.7 no C4 C5 H5A . . 118.7 no C4 C3 C2 . . 118.7(3) no C4 C3 H3A . . 120.7 no C2 C3 H3A . . 120.7 no C3 C4 C5 . . 118.9(4) no C3 C4 H4A . . 120.6 no C5 C4 H4A . . 120.6 no C1 C6 Cl1 . . 112.4(3) no C1 C6 H6A . . 109.1 no Cl1 C6 H6A . . 109.1 no C1 C6 H6B . . 109.1 no Cl1 C6 H6B . . 109.1 no H6A C6 H6B . . 107.9 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 N1 . 2.008(2) yes Cu1 N1 7 2.008(2) no Cu1 Cl2 . 2.2719(9) yes Cu1 Cl2 7 2.2719(9) no Cu1 Cl1 . 3.0003(10) yes Cl1 C6 . 1.797(4) no N1 C1 . 1.339(4) no N1 C5 . 1.341(5) no C1 C2 . 1.386(5) no C1 C6 . 1.497(5) no C2 C3 . 1.373(6) no C2 H2A . 0.9300 no C5 C4 . 1.381(5) no C5 H5A . 0.9300 no C3 C4 . 1.365(6) no C3 H3A . 0.9300 no C4 H4A . 0.9300 no C6 H6A . 0.9700 no C6 H6B . 0.9700 no _cod_database_fobs_code 2203692