#------------------------------------------------------------------------------ #$Date: 2011-06-21 23:01:37 +0300 (Tue, 21 Jun 2011) $ #$Revision: 21180 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/7015519.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_7015519 loop_ _publ_author_name 'Herringer, Susan N.' 'Turnbull, Mark M.' 'Landee, Christopher P.' 'Wikaira, Jan L.' _publ_section_title ; Copper(II) complexes of 2-halo-3-methylpyridine: synthesis, structure, and magnetic behaviour of Cu(2-X-3-CH(3)py)2X'2 [X, X' = chlorine or bromine; py = pyridine]. ; _journal_issue 16 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4242 _journal_page_last 4252 _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C12 H12 Br4 Cu N2' _chemical_formula_weight 567.42 _chemical_name_systematic ; bis(2-bromo-3-methylpyridine)dibromocopper (II) ; _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 _audit_creation_method SHELXL-97 _cell_angle_alpha 104.777(2) _cell_angle_beta 90.043(2) _cell_angle_gamma 114.151(2) _cell_formula_units_Z 1 _cell_length_a 6.2440(2) _cell_length_b 7.4588(3) _cell_length_c 9.5897(4) _cell_measurement_reflns_used 6170 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 30.00 _cell_measurement_theta_min 2.21 _cell_volume 391.24(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _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 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 9966 _diffrn_reflns_theta_full 30.00 _diffrn_reflns_theta_max 30.00 _diffrn_reflns_theta_min 2.21 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.595 _exptl_absorpt_correction_T_max 0.2936 _exptl_absorpt_correction_T_min 0.1004 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'via SADABS' _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.408 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 267 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.641 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 2270 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.086 _refine_ls_R_factor_all 0.0214 _refine_ls_R_factor_gt 0.0186 _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^)+(0.0166P)^2^+0.5302P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0454 _reflns_number_gt 2105 _reflns_number_total 2270 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0dt01696a.txt _[local]_cod_data_source_block snhc _[local]_cod_cif_authors_sg_H-M P-1 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' 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 1555 2011-01-17 13:19:09Z saulius ; _cod_database_code 7015519 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.0000 0.5000 0.01466(7) Uani 1 2 d S . . Br1 Br 0.41397(4) 0.27905(3) 0.63431(2) 0.01982(6) Uani 1 1 d . . . N1 N 0.3802(3) -0.1458(3) 0.64915(18) 0.0162(3) Uani 1 1 d . . . C2 C 0.5319(4) -0.1271(3) 0.7558(2) 0.0163(4) Uani 1 1 d . . . Br2 Br 0.84955(4) 0.05327(3) 0.75217(2) 0.02063(6) Uani 1 1 d . . . C3 C 0.4700(4) -0.2307(3) 0.8622(2) 0.0192(4) Uani 1 1 d . . . C4 C 0.2318(4) -0.3604(3) 0.8517(2) 0.0233(4) Uani 1 1 d . . . H4 H 0.1788 -0.4363 0.9205 0.028 Uiso 1 1 calc R . . C5 C 0.0704(4) -0.3813(4) 0.7431(3) 0.0243(4) Uani 1 1 d . . . H5 H -0.0922 -0.4695 0.7380 0.029 Uiso 1 1 calc R . . C6 C 0.1476(4) -0.2728(3) 0.6424(2) 0.0190(4) Uani 1 1 d . . . H6 H 0.0374 -0.2869 0.5674 0.023 Uiso 1 1 calc R . . C7 C 0.6490(5) -0.2086(4) 0.9775(2) 0.0266(5) Uani 1 1 d . . . H7A H 0.5675 -0.2758 1.0498 0.032 Uiso 1 1 calc R . . H7B H 0.7453 -0.0630 1.0248 0.032 Uiso 1 1 calc R . . H7C H 0.7511 -0.2724 0.9331 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01590(16) 0.01806(17) 0.01221(15) 0.00469(12) 0.00315(12) 0.00905(13) Br1 0.02367(11) 0.02046(11) 0.01863(10) 0.00500(8) 0.00673(7) 0.01281(8) N1 0.0165(8) 0.0183(8) 0.0155(7) 0.0040(6) 0.0039(6) 0.0095(7) C2 0.0167(9) 0.0180(9) 0.0159(8) 0.0044(7) 0.0038(7) 0.0091(8) Br2 0.01553(10) 0.02436(11) 0.02188(10) 0.00826(8) 0.00015(7) 0.00730(8) C3 0.0276(11) 0.0195(10) 0.0151(9) 0.0057(8) 0.0061(8) 0.0139(9) C4 0.0304(12) 0.0197(10) 0.0234(10) 0.0081(8) 0.0113(9) 0.0128(9) C5 0.0201(10) 0.0192(10) 0.0294(11) 0.0042(9) 0.0101(9) 0.0057(8) C6 0.0180(10) 0.0185(10) 0.0187(9) -0.0001(8) 0.0041(7) 0.0091(8) C7 0.0382(14) 0.0333(13) 0.0185(10) 0.0103(9) 0.0054(9) 0.0233(11) 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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_3 _geom_angle_publ_flag N1 Cu1 N1 180.0 2_656 . ? N1 Cu1 Br1 89.73(5) 2_656 . ? N1 Cu1 Br1 90.27(5) . . ? N1 Cu1 Br1 90.27(5) 2_656 2_656 ? N1 Cu1 Br1 89.73(5) . 2_656 ? Br1 Cu1 Br1 180.0 . 2_656 ? Cu1 Br1 Br2 106.450(8) . 1_455 ? Cu1 Br1 Cu1 103.016(7) . 1_455 ? Br2 Br1 Cu1 34.964(4) 1_455 1_455 ? C2 N1 C6 118.76(18) . . ? C2 N1 Cu1 119.45(14) . . ? C6 N1 Cu1 121.72(14) . . ? N1 C2 C3 124.6(2) . . ? N1 C2 Br2 114.44(15) . . ? C3 C2 Br2 120.99(16) . . ? C2 Br2 Br1 161.64(6) . 1_655 ? C4 C3 C2 115.3(2) . . ? C4 C3 C7 122.3(2) . . ? C2 C3 C7 122.4(2) . . ? C5 C4 C3 121.4(2) . . ? C6 C5 C4 119.3(2) . . ? N1 C6 C5 120.7(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.9793(17) 2_656 ? Cu1 N1 1.9793(17) . ? Cu1 Br1 2.4141(2) . ? Cu1 Br1 2.4141(2) 2_656 ? Br1 Br2 3.5572(3) 1_455 ? Br1 Cu1 5.2403(3) 1_455 ? N1 C2 1.334(3) . ? N1 C6 1.361(3) . ? C2 C3 1.396(3) . ? C2 Br2 1.893(2) . ? Br2 Br1 3.5572(3) 1_655 ? C3 C4 1.390(3) . ? C3 C7 1.500(3) . ? C4 C5 1.382(3) . ? C5 C6 1.379(3) . ? 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 N1 Cu1 Br1 Br2 137.05(5) 2_656 . . 1_455 ? N1 Cu1 Br1 Br2 -42.95(5) . . . 1_455 ? Br1 Cu1 Br1 Br2 -164(100) 2_656 . . 1_455 ? N1 Cu1 Br1 Cu1 101.02(5) 2_656 . . 1_455 ? N1 Cu1 Br1 Cu1 -78.98(5) . . . 1_455 ? Br1 Cu1 Br1 Cu1 160(100) 2_656 . . 1_455 ? N1 Cu1 N1 C2 -117(100) 2_656 . . . ? Br1 Cu1 N1 C2 -95.30(15) . . . . ? Br1 Cu1 N1 C2 84.70(15) 2_656 . . . ? N1 Cu1 N1 C6 66(100) 2_656 . . . ? Br1 Cu1 N1 C6 87.80(15) . . . . ? Br1 Cu1 N1 C6 -92.20(15) 2_656 . . . ? C6 N1 C2 C3 0.6(3) . . . . ? Cu1 N1 C2 C3 -176.44(16) . . . . ? C6 N1 C2 Br2 179.75(14) . . . . ? Cu1 N1 C2 Br2 2.8(2) . . . . ? N1 C2 Br2 Br1 -59.0(3) . . . 1_655 ? C3 C2 Br2 Br1 120.22(19) . . . 1_655 ? N1 C2 C3 C4 -0.1(3) . . . . ? Br2 C2 C3 C4 -179.20(15) . . . . ? N1 C2 C3 C7 178.2(2) . . . . ? Br2 C2 C3 C7 -0.9(3) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C7 C3 C4 C5 -178.9(2) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C2 N1 C6 C5 -0.4(3) . . . . ? Cu1 N1 C6 C5 176.48(16) . . . . ? C4 C5 C6 N1 -0.1(3) . . . . ?