#------------------------------------------------------------------------------ #$Date: 2008-03-30 11:21:05 +0100 (Sun, 30 Mar 2008) $ #$Revision: 321 $ #$URL: svn://www.crystallography.net/cod/cif/2/2204342.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_2204342 loop_ _publ_author_name 'Jun Luo' 'Bao-Shu Liu' 'Xi-Geng Zhou' 'Lin-Hong Weng' 'Yan-Rong Li' 'Rui-Fang Cai' _publ_section_title ; catena-Poly[[bis(1H-1,2,3-benzotriazole\-kN^3^)cobalt(II)]-di-\m-dicyanamido- \k^4^N^1^:N^3^] ; _journal_issue 10 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m1391 _journal_page_last m1393 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[Co (C2 N3)2 (C6 H5 N3)2]' _chemical_formula_moiety 'C16 H10 Co N12' _chemical_formula_sum 'C16 H10 Co N12' _chemical_formula_weight 429.29 _chemical_name_systematic ; catena-Poly[[bis(1H-1,2,3-benzotriazole\-kN^3^)cobalt(II)]-di-\m-dicyanamido- \k^4^N^1^:N^3^] ; _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 114.002(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 17.259(6) _cell_length_b 7.249(3) _cell_length_c 8.030(3) _cell_measurement_reflns_used 701 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 22.901 _cell_measurement_theta_min 2.583 _cell_volume 917.8(6) _computing_cell_refinement 'SAINT (Bruker, 2000)' _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT ' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2000)' _computing_publication_material 'SHELXTL ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _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 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 1920 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_min 2.58 _diffrn_standards_decay_% 4.38 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 434 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.422 _refine_diff_density_min -0.268 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 83 _refine_ls_number_reflns 878 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0543 _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^)+(0.0489P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1005 _refine_ls_wR_factor_ref 0.1092 _reflns_number_gt 678 _reflns_number_total 878 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file hb6087.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Co1 0.0000 0.0000 0.0000 0.0293(4) Uani d S 1 Co N1 0.0278(2) 0.2062(5) -0.1530(4) 0.0409(9) Uani d . 1 N N2 0.0729(3) 0.5000 -0.2424(6) 0.0399(12) Uani d S 1 N N3 0.1306(3) 0.0000 0.1942(6) 0.0347(11) Uani d S 1 N N4 0.1927(3) 0.0000 0.1395(6) 0.0396(12) Uani d S 1 N N5 0.2657(3) 0.0000 0.2872(6) 0.0438(13) Uani d S 1 N H5A 0.3148 0.0000 0.2839 0.053 Uiso calc SR 1 H C1 0.0474(2) 0.3456(6) -0.1923(4) 0.0311(9) Uani d . 1 C C2 0.2531(3) 0.0000 0.4438(7) 0.0358(13) Uani d S 1 C C3 0.1658(3) 0.0000 0.3844(7) 0.0320(13) Uani d S 1 C C4 0.1273(4) 0.0000 0.5087(7) 0.0450(15) Uani d S 1 C H4A 0.0687 0.0000 0.4699 0.054 Uiso calc SR 1 H C5 0.1807(4) 0.0000 0.6899(8) 0.0542(17) Uani d S 1 C H5B 0.1577 0.0000 0.7765 0.065 Uiso calc SR 1 H C6 0.2694(4) 0.0000 0.7482(9) 0.0601(19) Uani d S 1 C H6A 0.3034 0.0000 0.8726 0.072 Uiso calc SR 1 H C7 0.3075(4) 0.0000 0.6279(8) 0.0535(17) Uani d S 1 C H7A 0.3661 0.0000 0.6671 0.064 Uiso calc SR 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 Co1 0.0251(7) 0.0270(7) 0.0352(7) 0.000 0.0116(5) 0.000 N1 0.041(2) 0.033(2) 0.051(2) -0.0001(16) 0.0212(17) 0.0043(16) N2 0.047(3) 0.028(3) 0.056(3) 0.000 0.032(3) 0.000 N3 0.031(3) 0.039(3) 0.038(3) 0.000 0.018(2) 0.000 N4 0.032(3) 0.054(3) 0.038(3) 0.000 0.019(2) 0.000 N5 0.023(3) 0.059(3) 0.053(3) 0.000 0.019(2) 0.000 C1 0.025(2) 0.035(3) 0.031(2) 0.0078(18) 0.0098(17) -0.0045(17) C2 0.032(3) 0.039(3) 0.038(3) 0.000 0.016(3) 0.000 C3 0.031(3) 0.038(3) 0.031(3) 0.000 0.017(3) 0.000 C4 0.040(4) 0.054(4) 0.043(4) 0.000 0.019(3) 0.000 C5 0.058(5) 0.071(5) 0.037(4) 0.000 0.024(3) 0.000 C6 0.058(5) 0.076(5) 0.035(4) 0.000 0.006(3) 0.000 C7 0.032(4) 0.071(5) 0.048(4) 0.000 0.006(3) 0.000 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 Co1 N1 2 2.110(3) N Co1 N1 6 2.110(3) N Co1 N1 . 2.110(3) Y Co1 N1 5 2.110(3) N Co1 N3 . 2.157(4) Y Co1 N3 5 2.157(4) N N1 C1 . 1.150(5) y N2 C1 6_565 1.324(5) N N2 C1 . 1.324(5) y N3 N4 . 1.314(6) N N3 C3 . 1.395(6) N N4 N5 . 1.333(6) N N5 C2 . 1.360(6) N N5 H5A . 0.8600 N C2 C3 . 1.383(7) N C2 C7 . 1.392(7) N C3 C4 . 1.405(7) N C4 C5 . 1.369(7) N C4 H4A . 0.9300 N C5 C6 . 1.407(9) N C5 H5B . 0.9300 N C6 C7 . 1.371(8) N C6 H6A . 0.9300 N C7 H7A . 0.9300 N 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 Co1 N1 2 6 180.00(16) Y N1 Co1 N1 2 . 89.81(17) Y N1 Co1 N1 6 . 90.19(17) N N1 Co1 N1 2 5 90.19(17) Y N1 Co1 N1 6 5 89.81(17) N N1 Co1 N1 . 5 180.0(2) N N1 Co1 N3 2 . 89.83(12) Y N1 Co1 N3 6 . 90.17(12) Y N1 Co1 N3 . . 90.17(12) Y N1 Co1 N3 5 . 89.83(12) N N1 Co1 N3 2 5 90.17(12) N N1 Co1 N3 6 5 89.83(12) N N1 Co1 N3 . 5 89.83(12) Y N1 Co1 N3 5 5 90.17(12) N N3 Co1 N3 . 5 180.0(3) Y C1 N1 Co1 . . 160.8(3) y C1 N2 C1 6_565 . 115.5(4) y N4 N3 C3 . . 108.3(4) N N4 N3 Co1 . . 120.8(3) N C3 N3 Co1 . . 130.8(3) N N3 N4 N5 . . 107.9(4) N N4 N5 C2 . . 112.0(4) N N4 N5 H5A . . 124.0 N C2 N5 H5A . . 124.0 N N1 C1 N2 . . 176.3(4) y N5 C2 C3 . . 104.0(4) N N5 C2 C7 . . 133.6(5) N C3 C2 C7 . . 122.4(5) N C2 C3 N3 . . 107.8(5) N C2 C3 C4 . . 121.2(5) N N3 C3 C4 . . 131.0(5) N C5 C4 C3 . . 116.6(6) N C5 C4 H4A . . 121.7 N C3 C4 H4A . . 121.7 N C4 C5 C6 . . 121.6(6) N C4 C5 H5B . . 119.2 N C6 C5 H5B . . 119.2 N C7 C6 C5 . . 122.3(6) N C7 C6 H6A . . 118.9 N C5 C6 H6A . . 118.9 N C6 C7 C2 . . 116.0(6) N C6 C7 H7A . . 122.0 N C2 C7 H7A . . 122.0 N loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N5 H5A N2 7 0.86 2.10 2.951(6) 173