#------------------------------------------------------------------------------ #$Date: 2014-07-12 07:06:18 +0300 (Sat, 12 Jul 2014) $ #$Revision: 120112 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/01/54/7015496.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_7015496 loop_ _publ_author_name 'Yong, Guo-Ping' 'Li, Ying-Zhou' 'Li, Chong-Fu' 'Zhang, Yi-Man' 'She, Wen-Long' _publ_section_title ; New metal-anion radical framework materials: Co(II) compounds showing ferromagnetic to antiferromagnetic phase transition at about 344 K, and Zn(II) compounds exhibiting terminal anion ligand induced direct white-light-emission. ; _journal_issue 16 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 4131 _journal_page_last 4139 _journal_volume 40 _journal_year 2011 _chemical_formula_sum 'C14 H9 Br Co N4 O' _chemical_formula_weight 388.09 _chemical_name_systematic ; ? ; _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_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 94.20(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.189(2) _cell_length_b 8.0372(16) _cell_length_c 15.294(3) _cell_measurement_temperature 293(2) _cell_volume 1371.7(5) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.864 _diffrn_measured_fraction_theta_max 0.864 _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 0.0729 _diffrn_reflns_av_sigmaI/netI 0.0957 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 5766 _diffrn_reflns_theta_full 24.23 _diffrn_reflns_theta_max 24.23 _diffrn_reflns_theta_min 11.72 _exptl_absorpt_coefficient_mu 4.166 _exptl_absorpt_correction_T_max 0.353 _exptl_absorpt_correction_T_min 0.220 _exptl_absorpt_correction_type multi-scan _exptl_crystal_density_diffrn 1.879 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.748 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.127 _refine_ls_extinction_coef 0.22(5) _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 1.067 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 199 _refine_ls_number_reflns 1913 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.067 _refine_ls_R_factor_all 0.1387 _refine_ls_R_factor_gt 0.1010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2716 _refine_ls_wR_factor_ref 0.2951 _reflns_number_gt 1198 _reflns_number_total 1913 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file c0dt01667e.txt _[local]_cod_data_source_block 2 _[local]_cod_cif_authors_sg_H-M P2(1)/n _cod_database_code 7015496 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Co1 Co 0.11346(12) 0.21441(18) 0.25066(9) 0.0521(9) Uani 1 1 d . . . O1 O 0.2289(6) 0.0351(9) 0.2646(4) 0.0508(18) Uani 1 1 d . . . N4 N 0.3301(7) -0.0276(9) 0.4826(5) 0.0417(18) Uani 1 1 d . . . C14 C 0.2731(9) -0.0043(11) 0.3400(6) 0.043(2) Uani 1 1 d . . . C7 C 0.2168(8) 0.2361(11) 0.4394(6) 0.041(2) Uani 1 1 d . . . N2 N 0.1664(7) 0.4797(10) 0.4862(6) 0.045(2) Uani 1 1 d . . . C8 C 0.2656(8) 0.0740(11) 0.4230(6) 0.040(2) Uani 1 1 d . . . N1 N 0.1495(7) 0.3148(9) 0.3706(5) 0.0434(19) Uani 1 1 d . . . C1 C 0.1240(8) 0.4647(12) 0.4019(6) 0.042(2) Uani 1 1 d . . . C5 C 0.1473(8) 0.6224(14) 0.5342(8) 0.056(3) Uani 1 1 d . . . H5A H 0.1758 0.6303 0.5927 0.067 Uiso 1 1 calc R . . C2 C 0.0621(10) 0.6018(14) 0.3596(8) 0.060(3) Uani 1 1 d . . . H2A H 0.0340 0.5953 0.3009 0.072 Uiso 1 1 calc R . . C3 C 0.0456(11) 0.7398(14) 0.4062(9) 0.062(3) Uani 1 1 d . . . H3A H 0.0061 0.8301 0.3792 0.075 Uiso 1 1 calc R . . C6 C 0.2251(8) 0.3367(12) 0.5099(6) 0.044(2) Uani 1 1 d . . . H6A H 0.2636 0.3130 0.5644 0.053 Uiso 1 1 calc R . . C4 C 0.0858(11) 0.7511(14) 0.4936(10) 0.064(3) Uani 1 1 d . . . H4A H 0.0708 0.8470 0.5251 0.077 Uiso 1 1 calc R . . Br1 Br -0.0999(4) 0.1479(6) 0.2412(2) 0.1587(15) Uani 1 1 d . . . C11 C 0.4603(10) -0.2683(14) 0.5731(8) 0.057(3) Uani 1 1 d . . . H11A H 0.5054 -0.3486 0.6043 0.068 Uiso 1 1 calc R . . C12 C 0.4465(9) -0.2786(12) 0.4853(7) 0.046(2) Uani 1 1 d . . . H12A H 0.4827 -0.3643 0.4562 0.055 Uiso 1 1 calc R . . C13 C 0.3765(8) -0.1584(11) 0.4373(6) 0.040(2) Uani 1 1 d . . . C9 C 0.3437(10) -0.0203(13) 0.5709(6) 0.051(2) Uani 1 1 d . . . H9A H 0.3091 0.0665 0.6004 0.061 Uiso 1 1 calc R . . C10 C 0.4087(10) -0.1407(14) 0.6179(7) 0.053(3) Uani 1 1 d . . . H10A H 0.4176 -0.1361 0.6787 0.064 Uiso 1 1 calc R . . N3 N 0.3444(7) -0.1436(10) 0.3518(5) 0.0427(18) Uani 1 1 d . . . Br1A Br -0.130(2) 0.288(3) 0.2535(13) 0.339(7) Uiso 1 1 d . . . Br1B Br -0.022(3) 0.056(3) 0.2383(14) 0.345(7) Uiso 1 1 d . . . 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 Co1 0.0577(11) 0.0522(12) 0.0469(11) 0.0014(6) 0.0079(6) -0.0011(6) O1 0.064(4) 0.052(4) 0.037(4) -0.003(3) 0.008(3) 0.016(3) N4 0.046(4) 0.038(4) 0.041(4) 0.000(3) 0.005(3) -0.009(3) C14 0.056(5) 0.036(5) 0.038(5) -0.002(4) 0.012(4) -0.011(4) C7 0.043(4) 0.040(5) 0.041(5) -0.002(4) 0.009(4) -0.002(4) N2 0.035(4) 0.040(4) 0.061(5) -0.009(3) 0.011(3) -0.006(3) C8 0.047(5) 0.036(4) 0.038(4) -0.002(4) 0.011(3) -0.002(4) N1 0.046(4) 0.040(4) 0.045(4) -0.002(3) 0.011(3) 0.002(3) C1 0.047(5) 0.047(5) 0.035(5) 0.005(4) 0.014(4) -0.001(4) C5 0.031(5) 0.059(7) 0.078(7) -0.027(5) 0.013(4) -0.007(4) C2 0.059(6) 0.053(6) 0.068(7) 0.003(5) 0.010(5) 0.010(5) C3 0.062(6) 0.045(6) 0.082(9) 0.001(5) 0.026(6) 0.004(5) C6 0.043(4) 0.047(5) 0.042(5) -0.005(4) 0.002(4) 0.001(4) C4 0.056(6) 0.042(6) 0.097(10) -0.024(6) 0.031(6) -0.009(5) Br1 0.161(3) 0.173(3) 0.139(2) -0.0036(18) -0.0087(18) -0.003(2) C11 0.049(5) 0.053(6) 0.067(7) 0.004(5) -0.001(5) -0.009(5) C12 0.043(5) 0.045(5) 0.049(5) 0.005(4) 0.001(4) 0.005(4) C13 0.041(4) 0.040(5) 0.040(5) -0.004(4) 0.009(4) -0.007(4) C9 0.062(6) 0.052(6) 0.038(5) -0.006(4) 0.004(4) -0.011(5) C10 0.060(6) 0.060(6) 0.040(5) 0.007(4) -0.005(4) -0.008(5) N3 0.044(4) 0.043(4) 0.042(4) -0.006(3) 0.006(3) -0.003(3) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 O1 Co1 Br1B 91.7(9) . . ? O1 Co1 N1 96.4(3) . . ? Br1B Co1 N1 116.5(7) . . ? O1 Co1 N3 108.3(3) . 2 ? Br1B Co1 N3 120.6(7) . 2 ? N1 Co1 N3 115.9(3) . 2 ? O1 Co1 Br1 119.0(3) . . ? Br1B Co1 Br1 27.7(9) . . ? N1 Co1 Br1 105.7(2) . . ? N3 Co1 Br1 111.1(2) 2 . ? O1 Co1 Br1A 143.0(6) . . ? Br1B Co1 Br1A 52.8(11) . . ? N1 Co1 Br1A 91.8(5) . . ? N3 Co1 Br1A 100.2(5) 2 . ? Br1 Co1 Br1A 25.2(5) . . ? C14 O1 Co1 120.1(6) . . ? C9 N4 C13 121.1(8) . . ? C9 N4 C8 130.4(8) . . ? C13 N4 C8 108.4(7) . . ? O1 C14 N3 120.6(8) . . ? O1 C14 C8 131.2(9) . . ? N3 C14 C8 108.2(8) . . ? C6 C7 N1 109.4(8) . . ? C6 C7 C8 132.7(9) . . ? N1 C7 C8 117.8(8) . . ? C1 N2 C6 108.0(7) . . ? C1 N2 C5 121.6(9) . . ? C6 N2 C5 130.4(9) . . ? N4 C8 C14 105.3(7) . . ? N4 C8 C7 127.1(8) . . ? C14 C8 C7 127.1(8) . . ? C1 N1 C7 104.8(7) . . ? C1 N1 Co1 130.8(6) . . ? C7 N1 Co1 124.3(6) . . ? N1 C1 N2 110.8(8) . . ? N1 C1 C2 130.0(9) . . ? N2 C1 C2 119.3(9) . . ? C4 C5 N2 118.5(11) . . ? C3 C2 C1 118.6(12) . . ? C2 C3 C4 121.5(11) . . ? C7 C6 N2 106.9(8) . . ? C5 C4 C3 120.5(9) . . ? Br1B Br1 Br1A 147.0(16) . . ? Br1B Br1 Co1 53.0(12) . . ? Br1A Br1 Co1 94.2(11) . . ? C12 C11 C10 121.3(10) . . ? C11 C12 C13 119.7(9) . . ? N3 C13 N4 109.8(8) . . ? N3 C13 C12 131.8(8) . . ? N4 C13 C12 118.3(8) . . ? N4 C9 C10 120.5(10) . . ? C9 C10 C11 119.1(9) . . ? C13 N3 C14 108.2(7) . . ? C13 N3 Co1 130.4(6) . 2_545 ? C14 N3 Co1 121.4(6) . 2_545 ? Br1 Br1A Br1B 16.2(8) . . ? Br1 Br1A Co1 60.6(10) . . ? Br1B Br1A Co1 44.5(8) . . ? Br1 Br1B Co1 99.3(16) . . ? Br1 Br1B Br1A 16.8(9) . . ? Co1 Br1B Br1A 82.6(12) . . ? 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 Co1 O1 1.936(7) . ? Co1 Br1B 1.98(2) . ? Co1 N1 2.018(8) . ? Co1 N3 2.022(7) 2 ? Co1 Br1 2.440(4) . ? Co1 Br1A 2.79(2) . ? O1 C14 1.262(12) . ? N4 C9 1.351(13) . ? N4 C13 1.380(12) . ? N4 C8 1.387(13) . ? C14 N3 1.379(13) . ? C14 C8 1.425(13) . ? C7 C6 1.345(14) . ? C7 N1 1.399(13) . ? C7 C8 1.442(13) . ? N2 C1 1.346(13) . ? N2 C6 1.359(14) . ? N2 C5 1.387(13) . ? N1 C1 1.334(13) . ? C1 C2 1.431(16) . ? C5 C4 1.37(2) . ? C2 C3 1.339(18) . ? C3 C4 1.38(2) . ? Br1 Br1B 1.15(3) . ? Br1 Br1A 1.19(3) . ? C11 C12 1.342(16) . ? C11 C10 1.384(18) . ? C12 C13 1.415(15) . ? C13 N3 1.335(13) . ? C9 C10 1.379(16) . ? N3 Co1 2.022(7) 2_545 ? Br1A Br1B 2.25(4) . ? _journal_paper_doi 10.1039/c0dt01667e