#------------------------------------------------------------------------------ #$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/46/2014634.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_2014634 loop_ _publ_author_name ' Zhi-Min Jin ' ' Nan Shun ' ' Ya-Ping L\"u ' ' Mao-Lin Hu ' 'Liang Shen' _publ_section_title ; Bis(2-amino-6-methylpyridinium) tetrachlorozincate(II) ; _journal_issue 1 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m43 _journal_page_last m45 _journal_paper_doi 10.1107/S0108270104030458 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '(C6 H9 N2)2 [Zn Cl4]' _chemical_formula_moiety '2C6 H9 N2 +, Cl4 Zn 2-' _chemical_formula_sum 'C12 H18 Cl4 N4 Zn' _chemical_formula_weight 425.49 _chemical_name_systematic ; Bis(2-amino-6-methylpyridinium) tetrachlorozincate(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 81.177(2) _cell_angle_beta 79.128(2) _cell_angle_gamma 89.983(2) _cell_formula_units_Z 2 _cell_length_a 7.6642(8) _cell_length_b 7.9235(8) _cell_length_c 15.6651(16) _cell_measurement_reflns_used 39 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 14.94 _cell_measurement_theta_min 2.78 _cell_volume 922.77(16) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2000)' _computing_data_reduction 'SAINT (Bruker, 2000)' _computing_molecular_graphics ; ORTEPIII for Windows (Farrugia, 1997) and SHELXTL ; _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXTL (Bruker, 2000)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Bruker Smart Apex CCD area detector' _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 0.0122 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 4948 _diffrn_reflns_theta_full 25.23 _diffrn_reflns_theta_max 25.23 _diffrn_reflns_theta_min 2.60 _exptl_absorpt_coefficient_mu 1.907 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2000)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.531 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 432.0 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _refine_diff_density_max 0.395 _refine_diff_density_min -0.286 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 192 _refine_ls_number_reflns 3272 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0333 _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^)+(0.0457P)^2^+0.1635P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0832 _refine_ls_wR_factor_ref 0.0872 _reflns_number_gt 2791 _reflns_number_total 3335 _reflns_threshold_expression I>2\s(I) _cod_data_source_file dn1068.cif _cod_data_source_block I _cod_original_formula_sum 'C12 H18 Cl4 N4 Zn1' _cod_database_code 2014634 _cod_database_fobs_code 2014634 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' 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_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Cl1 0.62077(14) 0.03528(12) 0.34772(7) 0.0989(4) Uani d . 1 . . Cl Cl2 1.04628(10) 0.29249(13) 0.29792(6) 0.0781(3) Uani d . 1 . . Cl Cl3 0.93550(11) 0.04961(12) 0.13449(6) 0.0789(3) Uani d . 1 . . Cl Cl4 0.67477(11) 0.42709(9) 0.18962(5) 0.0620(2) Uani d . 1 . . Cl Zn 0.81829(4) 0.19389(4) 0.24287(2) 0.04909(13) Uani d . 1 . . Zn N1 0.8096(3) 0.4174(3) 0.46278(16) 0.0539(6) Uani d . 1 . . N H1 0.8664 0.3668 0.4216 0.065 Uiso calc R 1 . . H N2 0.8056(4) 0.6540(3) 0.35723(17) 0.0749(8) Uani d . 1 . . N H21 0.8616 0.5979 0.3182 0.090 Uiso calc R 1 . . H H22 0.7771 0.7578 0.3421 0.090 Uiso calc R 1 . . H C1 0.7634(4) 0.5805(4) 0.44064(19) 0.0526(7) Uani d . 1 . . C C2 0.6738(4) 0.6628(4) 0.5087(2) 0.0565(7) Uani d . 1 . . C H2 0.6400 0.7755 0.4968 0.068 Uiso calc R 1 . . H C3 0.6375(4) 0.5766(4) 0.5913(2) 0.0655(8) Uani d . 1 . . C H3A 0.5796 0.6316 0.6365 0.079 Uiso calc R 1 . . H C4 0.6843(4) 0.4080(4) 0.6109(2) 0.0672(8) Uani d . 1 . . C H4 0.6554 0.3502 0.6683 0.081 Uiso calc R 1 . . H C5 0.7724(4) 0.3280(4) 0.5456(2) 0.0606(8) Uani d . 1 . . C C6 0.8322(5) 0.1475(4) 0.5559(3) 0.0832(10) Uani d . 1 . . C H6A 0.7794 0.0853 0.5188 0.125 Uiso calc R 1 . . H H6B 0.7962 0.0948 0.6162 0.125 Uiso calc R 1 . . H H6C 0.9593 0.1466 0.5394 0.125 Uiso calc R 1 . . H N3 0.6018(3) 0.2936(3) 0.01523(16) 0.0529(6) Uani d . 1 . . N H3 0.6432 0.3348 0.0554 0.064 Uiso calc R 1 . . H N4 0.3409(4) 0.2346(4) 0.1155(2) 0.0832(9) Uani d . 1 . . N H41 0.3897 0.2751 0.1535 0.100 Uiso calc R 1 . . H H42 0.2327 0.1960 0.1297 0.100 Uiso calc R 1 . . H C7 0.4326(4) 0.2317(3) 0.0348(2) 0.0552(7) Uani d . 1 . . C C8 0.3651(4) 0.1688(4) -0.0312(2) 0.0620(8) Uani d . 1 . . C H8 0.2486 0.1264 -0.0206 0.074 Uiso calc R 1 . . H C9 0.4715(5) 0.1702(4) -0.1108(2) 0.0696(9) Uani d . 1 . . C H9 0.4267 0.1288 -0.1551 0.084 Uiso calc R 1 . . H C10 0.6461(5) 0.2323(4) -0.1277(2) 0.0683(8) Uani d . 1 . . C H10 0.7177 0.2307 -0.1825 0.082 Uiso calc R 1 . . H C11 0.7114(4) 0.2948(4) -0.0644(2) 0.0556(7) Uani d . 1 . . C C12 0.8956(4) 0.3660(5) -0.0732(2) 0.0762(9) Uani d . 1 . . C H12A 0.9646 0.3512 -0.1293 0.114 Uiso calc R 1 . . H H12B 0.9498 0.3070 -0.0271 0.114 Uiso calc R 1 . . H H12C 0.8908 0.4855 -0.0687 0.114 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 Cl1 0.0849(7) 0.0693(6) 0.1105(8) 0.0064(5) 0.0310(5) 0.0249(5) Cl2 0.0510(4) 0.1244(7) 0.0711(5) 0.0065(4) -0.0133(4) -0.0512(5) Cl3 0.0546(5) 0.0959(6) 0.0971(6) 0.0014(4) -0.0042(4) -0.0614(5) Cl4 0.0708(5) 0.0528(4) 0.0609(5) 0.0095(3) -0.0109(4) -0.0068(3) Zn 0.0445(2) 0.0515(2) 0.0500(2) 0.00078(14) -0.00280(14) -0.01168(15) N1 0.0515(14) 0.0550(14) 0.0563(15) 0.0033(11) -0.0031(11) -0.0208(12) N2 0.096(2) 0.0630(16) 0.0596(17) 0.0064(15) 0.0002(14) -0.0100(13) C1 0.0506(16) 0.0547(16) 0.0544(17) -0.0010(13) -0.0083(13) -0.0170(14) C2 0.0553(17) 0.0560(16) 0.0625(19) 0.0052(13) -0.0112(14) -0.0228(15) C3 0.0567(18) 0.085(2) 0.061(2) 0.0088(16) -0.0092(15) -0.0354(18) C4 0.067(2) 0.083(2) 0.0510(18) 0.0000(17) -0.0092(15) -0.0112(17) C5 0.0512(17) 0.0638(18) 0.068(2) -0.0031(14) -0.0151(15) -0.0087(16) C6 0.080(2) 0.063(2) 0.102(3) 0.0045(18) -0.015(2) -0.002(2) N3 0.0471(14) 0.0543(13) 0.0586(15) -0.0004(11) -0.0104(11) -0.0122(11) N4 0.0521(16) 0.100(2) 0.095(2) -0.0093(15) 0.0129(15) -0.0417(18) C7 0.0442(16) 0.0484(15) 0.072(2) 0.0054(12) -0.0073(14) -0.0109(14) C8 0.0484(17) 0.0544(17) 0.087(2) 0.0055(14) -0.0254(17) -0.0074(16) C9 0.079(2) 0.071(2) 0.066(2) 0.0025(17) -0.0382(18) -0.0024(17) C10 0.072(2) 0.083(2) 0.0477(17) 0.0007(17) -0.0140(15) -0.0002(16) C11 0.0489(16) 0.0550(16) 0.0588(18) 0.0021(13) -0.0084(14) 0.0014(14) C12 0.057(2) 0.088(2) 0.076(2) -0.0113(17) -0.0034(16) -0.0011(19) 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' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag Cl1 Zn Cl3 112.41(4) y Cl1 Zn Cl2 111.75(4) y Cl3 Zn Cl2 107.77(3) y Cl1 Zn Cl4 107.17(3) y Cl3 Zn Cl4 110.74(4) y Cl2 Zn Cl4 106.88(3) y C1 N1 C5 124.4(2) ? C1 N1 H1 117.8 ? C5 N1 H1 117.8 ? C1 N2 H21 120.0 ? C1 N2 H22 120.0 ? H21 N2 H22 120.0 ? N2 C1 N1 118.9(3) ? N2 C1 C2 123.9(3) ? N1 C1 C2 117.2(3) ? C3 C2 C1 119.1(3) ? C3 C2 H2 120.4 ? C1 C2 H2 120.4 ? C2 C3 C4 121.8(3) ? C2 C3 H3A 119.1 ? C4 C3 H3A 119.1 ? C5 C4 C3 119.4(3) ? C5 C4 H4 120.3 ? C3 C4 H4 120.3 ? C4 C5 N1 118.0(3) ? C4 C5 C6 125.9(3) ? N1 C5 C6 116.1(3) ? C5 C6 H6A 109.5 ? C5 C6 H6B 109.5 ? H6A C6 H6B 109.5 ? C5 C6 H6C 109.5 ? H6A C6 H6C 109.5 ? H6B C6 H6C 109.5 ? C7 N3 C11 123.9(3) ? C7 N3 H3 118.0 ? C11 N3 H3 118.0 ? C7 N4 H41 120.0 ? C7 N4 H42 120.0 ? H41 N4 H42 120.0 ? N4 C7 N3 118.1(3) ? N4 C7 C8 124.2(3) ? N3 C7 C8 117.8(3) ? C9 C8 C7 119.1(3) ? C9 C8 H8 120.4 ? C7 C8 H8 120.4 ? C8 C9 C10 121.3(3) ? C8 C9 H9 119.4 ? C10 C9 H9 119.4 ? C11 C10 C9 119.8(3) ? C11 C10 H10 120.1 ? C9 C10 H10 120.1 ? C10 C11 N3 118.1(3) ? C10 C11 C12 125.8(3) ? N3 C11 C12 116.1(3) ? C11 C12 H12A 109.5 ? C11 C12 H12B 109.5 ? H12A C12 H12B 109.5 ? C11 C12 H12C 109.5 ? H12A C12 H12C 109.5 ? H12B C12 H12C 109.5 ? 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 Cl1 Zn . 2.2358(9) y Cl2 Zn . 2.2767(8) y Cl3 Zn . 2.2396(8) y Cl4 Zn . 2.2786(8) y N1 C1 . 1.351(4) y N1 C5 . 1.359(4) y N1 H1 . 0.8600 ? N2 C1 . 1.326(4) y N2 H21 . 0.8600 ? N2 H22 . 0.8600 ? C1 C2 . 1.403(4) y C2 C3 . 1.347(4) y C2 H2 . 0.9300 ? C3 C4 . 1.387(4) y C3 H3A . 0.9300 ? C4 C5 . 1.357(4) y C4 H4 . 0.9300 ? C5 C6 . 1.496(4) y C6 H6A . 0.9600 ? C6 H6B . 0.9600 ? C6 H6C . 0.9600 ? N3 C7 . 1.350(4) y N3 C11 . 1.365(4) y N3 H3 . 0.8600 ? N4 C7 . 1.329(4) y N4 H41 . 0.8600 ? N4 H42 . 0.8600 ? C7 C8 . 1.394(4) y C8 C9 . 1.354(5) y C8 H8 . 0.9300 ? C9 C10 . 1.389(5) y C9 H9 . 0.9300 ? C10 C11 . 1.348(4) y C10 H10 . 0.9300 ? C11 C12 . 1.495(4) y C12 H12A . 0.9600 ? C12 H12B . 0.9600 ? C12 H12C . 0.9600 ? 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 N1 H1 Cl2 . 0.86 2.31 3.155(2) 167 N2 H21 Cl2 . 0.86 2.83 3.555(3) 143 N2 H22 Cl1 1_565 0.86 2.51 3.331(3) 160 N3 H3 Cl4 . 0.86 2.38 3.218(2) 164 N4 H41 Cl4 . 0.86 2.69 3.448(3) 148 N4 H42 Cl3 1_455 0.86 2.54 3.378(3) 165 N4 H42 Cl2 1_455 0.86 2.96 3.382(3) 112 C2 H2 Cl1 1_565 0.93 2.89 3.651(3) 140 C6 H6B Cl1 2_656 0.96 3.28 3.713(4) 110 C12 H12B Cl3 . 0.96 2.98 3.851(4) 151 C8 H8 Cl3 2_655 0.93 2.97 3.632(3) 129