#------------------------------------------------------------------------------ #$Date: 2013-08-29 18:37:19 +0300 (Thu, 29 Aug 2013) $ #$Revision: 88064 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/57/2205769.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_2205769 loop_ _publ_author_name 'Shi, Jing-Min' 'Liu, Zhe' 'Lu, Jian-Jun' 'Liu, Lian-Dong' _publ_section_title ; Diiodidobis(4-methylpyridine N-oxide-\kO)zinc(II) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m856 _journal_page_last m857 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Zn (I)2 (C6 H7 N O)2]' _chemical_formula_moiety 'C12 H14 I2 N2 O2 Zn' _chemical_formula_sum 'C12 H14 I2 N2 O2 Zn' _chemical_formula_weight 537.42 _chemical_name_systematic ; Diiodidobis(4-methylpyridine N-oxide-?O)zinc(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 SHELXL97 _cell_angle_alpha 90.00 _cell_angle_beta 126.487(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 19.385(5) _cell_length_b 7.5134(19) _cell_length_c 14.859(4) _cell_measurement_reflns_used 1828 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.0 _cell_measurement_theta_min 2.6 _cell_volume 1740.0(8) _computing_cell_refinement 'SAINT (Bruker, 1997)' _computing_data_collection 'SMART (Bruker, 1997)' _computing_data_reduction SAINT _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _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 0.989 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker SMART 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 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 4279 _diffrn_reflns_theta_full 25.50 _diffrn_reflns_theta_max 25.50 _diffrn_reflns_theta_min 2.61 _exptl_absorpt_coefficient_mu 4.959 _exptl_absorpt_correction_T_max 0.637 _exptl_absorpt_correction_T_min 0.406 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Sheldrick, 1996)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.052 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.589 _refine_diff_density_min -0.491 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 88 _refine_ls_number_reflns 1597 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0301 _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^)+(0.037P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.0747 _reflns_number_gt 1371 _reflns_number_total 1597 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file ng6123.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 1739.9(8) _cod_database_code 2205769 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 Zn1 0.5000 0.07038(9) 0.7500 0.0502(2) Uani d S 1 Zn N1 0.4751(2) 0.2916(4) 0.5765(3) 0.0526(8) Uani d . 1 N C1 0.4079(3) 0.3817(6) 0.5543(5) 0.0653(13) Uani d . 1 C H1 0.4025 0.4063 0.6112 0.078 Uiso calc R 1 H C2 0.3469(3) 0.4381(6) 0.4481(5) 0.0690(13) Uani d . 1 C H2 0.2999 0.5012 0.4333 0.083 Uiso calc R 1 H C3 0.3530(3) 0.4039(6) 0.3614(4) 0.0617(12) Uani d . 1 C C4 0.2878(4) 0.4701(8) 0.2442(5) 0.1016(19) Uani d . 1 C H4A 0.3054 0.5839 0.2351 0.152 Uiso calc R 1 H H4B 0.2331 0.4814 0.2308 0.152 Uiso calc R 1 H H4C 0.2832 0.3871 0.1917 0.152 Uiso calc R 1 H C5 0.4247(3) 0.3109(6) 0.3897(4) 0.0626(12) Uani d . 1 C H5 0.4324 0.2859 0.3349 0.075 Uiso calc R 1 H C6 0.4845(3) 0.2552(5) 0.4968(4) 0.0556(11) Uani d . 1 C H6 0.5322 0.1915 0.5143 0.067 Uiso calc R 1 H O1 0.53714(19) 0.2360(4) 0.6817(3) 0.0680(9) Uani d . 1 O I1 0.368720(18) -0.09837(4) 0.59359(3) 0.06272(15) Uani d . 1 I 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 Zn1 0.0462(4) 0.0652(4) 0.0380(4) 0.000 0.0244(3) 0.000 N1 0.052(2) 0.060(2) 0.047(2) -0.0055(18) 0.0300(18) 0.0034(18) C1 0.068(3) 0.079(3) 0.063(3) 0.005(3) 0.047(3) 0.000(3) C2 0.057(3) 0.074(3) 0.080(4) 0.017(2) 0.043(3) 0.005(3) C3 0.060(3) 0.060(3) 0.053(3) 0.000(2) 0.027(2) 0.003(2) C4 0.086(4) 0.103(4) 0.071(4) 0.018(4) 0.022(3) 0.017(4) C5 0.072(3) 0.071(3) 0.051(3) 0.005(3) 0.040(3) -0.004(2) C6 0.057(3) 0.061(3) 0.056(3) 0.011(2) 0.038(2) 0.007(2) O1 0.0528(18) 0.093(2) 0.0476(18) -0.0099(17) 0.0241(15) 0.0148(17) I1 0.0448(2) 0.0832(3) 0.0528(2) -0.00856(14) 0.02497(17) -0.01277(15) 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 O1 Zn1 O1 . 2_656 102.7(2) yes O1 Zn1 I1 . . 108.34(9) yes O1 Zn1 I1 2_656 . 108.00(9) ? O1 Zn1 I1 . 2_656 108.00(9) yes O1 Zn1 I1 2_656 2_656 108.34(9) ? I1 Zn1 I1 . 2_656 120.11(3) yes C1 N1 C6 . . 121.3(4) ? C1 N1 O1 . . 120.8(4) ? C6 N1 O1 . . 117.8(4) ? N1 C1 C2 . . 119.8(5) ? N1 C1 H1 . . 120.1 ? C2 C1 H1 . . 120.1 ? C1 C2 C3 . . 121.6(5) ? C1 C2 H2 . . 119.2 ? C3 C2 H2 . . 119.2 ? C5 C3 C2 . . 116.0(5) ? C5 C3 C4 . . 121.4(5) ? C2 C3 C4 . . 122.5(5) ? C3 C4 H4A . . 109.5 ? C3 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? C3 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? C6 C5 C3 . . 121.0(4) ? C6 C5 H5 . . 119.5 ? C3 C5 H5 . . 119.5 ? N1 C6 C5 . . 120.3(4) ? N1 C6 H6 . . 119.8 ? C5 C6 H6 . . 119.8 ? N1 O1 Zn1 . . 116.1(2) ? 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 Zn1 O1 . 1.992(3) yes Zn1 O1 2_656 1.992(3) ? Zn1 I1 . 2.5399(6) yes Zn1 I1 2_656 2.5399(6) ? N1 C1 . 1.324(6) ? N1 C6 . 1.329(5) ? N1 O1 . 1.353(4) ? C1 C2 . 1.360(7) ? C1 H1 . 0.9300 ? C2 C3 . 1.387(7) ? C2 H2 . 0.9300 ? C3 C5 . 1.379(7) ? C3 C4 . 1.503(8) ? C4 H4A . 0.9600 ? C4 H4B . 0.9600 ? C4 H4C . 0.9600 ? C5 C6 . 1.363(6) ? C5 H5 . 0.9300 ? C6 H6 . 0.9300 ? 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_site_symmetry_1 _geom_torsion C6 N1 C1 C2 . 0.2(7) O1 N1 C1 C2 . 179.2(4) N1 C1 C2 C3 . -0.1(8) C1 C2 C3 C5 . -0.5(7) C1 C2 C3 C4 . -177.9(5) C2 C3 C5 C6 . 0.9(7) C4 C3 C5 C6 . 178.4(5) C1 N1 C6 C5 . 0.2(7) O1 N1 C6 C5 . -178.8(4) C3 C5 C6 N1 . -0.8(7) C1 N1 O1 Zn1 . 60.5(4) C6 N1 O1 Zn1 . -120.5(3) O1 Zn1 O1 N1 2_656 -87.2(3) I1 Zn1 O1 N1 . 26.9(3) I1 Zn1 O1 N1 2_656 158.5(2) _cod_database_fobs_code 2205769