#------------------------------------------------------------------------------ #$Date: 2016-02-19 14:29:56 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176759 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/85/2008547.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_2008547 loop_ _publ_author_name 'Yang, Shi-Ping' 'Long, La-Sheng' 'Chen, Xiao-Ming' 'Ji, Liang-Nian' _publ_section_title ; Dichlorobis(2-hydroxymethyl-1-methylimidazole-N^3^)zinc(II) ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 869 _journal_page_last 871 _journal_paper_doi 10.1107/S0108270199002309 _journal_volume 55 _journal_year 1999 _chemical_formula_iupac '[Zn Cl2 (C5 H8 N2 O)2]' _chemical_formula_moiety '[Zn Cl2 (C5 H8 N2 O)2]' _chemical_formula_sum 'C10 H16 Cl2 N4 O2 Zn' _chemical_formula_weight 360.54 _chemical_name_systematic ; Dichloro-bis[2-(2-hydroxymethyl)-1-methylimidazole-N^3^]zinc(II) ; _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' _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 100.51(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.281(2) _cell_length_b 16.084(7) _cell_length_c 12.849(6) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15 _cell_measurement_theta_min 7.5 _cell_volume 1479.5(10) _computing_cell_refinement 'R3m Software' _computing_data_collection 'R3m Software (Siemens, 1990)' _computing_data_reduction 'SHELXTL-Plus (Sheldrick, 1990)' _computing_molecular_graphics 'ORTEP3 for Windows (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997b)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.964 _diffrn_measured_fraction_theta_max 0.964 _diffrn_measurement_device_type 'Siemens R3m' _diffrn_measurement_method '\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 0.025 _diffrn_reflns_av_sigmaI/netI 0.042 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 3127 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26 _diffrn_reflns_theta_min 2.05 _diffrn_standards_decay_% 1.1 _diffrn_standards_interval_count 118 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 2.024 _exptl_absorpt_correction_T_max 0.603 _exptl_absorpt_correction_T_min 0.458 _exptl_absorpt_correction_type 'empirical via \y-scans' _exptl_absorpt_process_details '(North et al. 1968)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 736 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _refine_diff_density_max 0.865 _refine_diff_density_min -0.570 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 2894 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.099 _refine_ls_R_factor_gt 0.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0740P)^2^+2.7045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.166 _reflns_number_gt 1924 _reflns_number_total 2894 _reflns_threshold_expression I>2\s(I) _cod_data_source_file cf1299.cif _cod_data_source_block zn _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: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0740P)^2^+2.7045P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0740P)^2^+2.7045P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2008547 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_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 Zn1 .19749(10) .86759(4) .80310(6) .0542(3) Uani d . 1 . . Zn Cl1 -.0056(3) .76202(11) .79958(18) .0848(6) Uani d . 1 . . Cl Cl2 .4597(3) .85371(12) .92223(14) .0771(5) Uani d . 1 . . Cl N1 .0567(6) .9677(3) .8369(4) .0484(11) Uani d . 1 . . N N2 -.0163(8) 1.0931(3) .8763(4) .0621(14) Uani d . 1 . . N N3 .2753(6) .8794(3) .6620(4) .0517(12) Uani d . 1 . . N N4 .2841(7) .8896(3) .4951(4) .0563(13) Uani d . 1 . . N O1 .2509(8) 1.1120(4) .7154(4) .105(2) Uani d . 1 . . O H1 .3456 1.1628 .7107 .080 Uiso d R 1 . . H O2 -.1249(9) .9302(5) .4943(7) .138(3) Uani d . 1 . . O H2 -.0842 .9609 .4304 .080 Uiso d R 1 . . H C1 -.1138(8) .9665(4) .8678(5) .0560(15) Uani d . 1 . . C H1A -.1879 .9173 .8694 .080 Uiso d R 1 . . H C2 -.1603(9) 1.0434(5) .8908(5) .0662(18) Uani d . 1 . . C H2A -.2730 1.0611 .9131 .080 Uiso d R 1 . . H C3 .1116(8) 1.0462(4) .8439(4) .0519(14) Uani d . 1 . . C C4 .2886(9) 1.0761(4) .8163(5) .0666(18) Uani d . 1 . . C H4A .3493 1.1152 .8677 .080 Uiso d R 1 . . H H4B .3696 1.0292 .8141 .080 Uiso d R 1 . . H C5 -.0058(12) 1.1824(5) .8942(7) .093(3) Uani d . 1 . . C H5A .1108 1.2027 .8796 .080 Uiso d R 1 . . H H5B -.1071 1.2092 .8481 .080 Uiso d R 1 . . H H5C -.0137 1.1943 .9665 .080 Uiso d R 1 . . H C6 .4564(9) .8928(4) .6500(5) .0615(16) Uani d . 1 . . C H6A .5610 .8958 .7074 .080 Uiso d R 1 . . H C7 .4589(9) .8994(5) .5475(6) .0689(18) Uani d . 1 . . C H7A .5639 .9095 .5136 .080 Uiso d R 1 . . H C8 .2218(11) .8939(5) .3798(5) .084(2) Uani d . 1 . . C H8A .0893 .8850 .3622 .080 Uiso d R 1 . . H H8B .2513 .9479 .3556 .080 Uiso d R 1 . . H H8C .2850 .8521 .3463 .080 Uiso d R 1 . . H C9 .1745(8) .8770(4) .5669(5) .0528(14) Uani d . 1 . . C C10 -.0302(9) .8626(4) .5391(6) .0676(18) Uani d . 1 . . C H10A -.0759 .8575 .6043 .080 Uiso d R 1 . . H H10B -.0615 .8126 .4990 .080 Uiso d 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 Zn1 .0554(4) .0528(4) .0567(4) -.0027(3) .0165(3) -.0028(3) Cl1 .0844(13) .0579(10) .1219(17) -.0157(9) .0447(12) -.0116(10) Cl2 .0685(11) .0930(13) .0666(11) .0080(10) .0039(8) .0143(9) N1 .047(3) .049(3) .048(3) .002(2) .007(2) -.002(2) N2 .074(4) .055(3) .053(3) .014(3) -.001(3) -.006(2) N3 .045(3) .060(3) .052(3) -.004(2) .013(2) -.007(2) N4 .049(3) .065(3) .056(3) .011(2) .016(2) -.003(2) O1 .096(4) .134(5) .080(4) -.054(4) .001(3) .026(3) O2 .078(4) .127(6) .206(8) .008(4) .017(5) -.015(5) C1 .053(4) .067(4) .047(3) -.003(3) .007(3) -.001(3) C2 .056(4) .091(5) .051(4) .013(4) .009(3) -.005(3) C3 .057(4) .054(3) .041(3) .000(3) -.002(3) -.001(3) C4 .066(4) .068(4) .062(4) -.020(3) .002(3) .005(3) C5 .115(7) .068(5) .092(6) .014(5) .009(5) -.021(4) C6 .046(3) .077(4) .061(4) -.007(3) .009(3) .004(3) C7 .047(4) .090(5) .074(5) .008(3) .021(3) .012(4) C8 .084(5) .122(6) .049(4) .037(5) .016(4) .003(4) C9 .048(3) .054(3) .058(4) .004(3) .013(3) -.009(3) C10 .046(4) .071(4) .083(5) .002(3) .005(3) .001(4) 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 N1 Zn1 N3 111.15(19) yes N1 Zn1 Cl2 109.90(14) yes N3 Zn1 Cl2 106.42(15) yes N1 Zn1 Cl1 104.56(15) yes N3 Zn1 Cl1 110.31(15) yes Cl2 Zn1 Cl1 114.59(8) yes C3 N1 C1 105.7(5) ? C3 N1 Zn1 128.6(4) yes C1 N1 Zn1 125.4(4) yes C3 N2 C2 108.2(5) ? C3 N2 C5 126.4(7) ? C2 N2 C5 125.4(6) ? C9 N3 C6 106.7(5) ? C9 N3 Zn1 129.8(4) yes C6 N3 Zn1 123.5(4) yes C7 N4 C9 107.6(5) ? C7 N4 C8 126.4(6) ? C9 N4 C8 126.0(6) ? C2 C1 N1 109.4(6) ? C1 C2 N2 106.4(6) ? N1 C3 N2 110.2(6) ? N1 C3 C4 124.0(6) ? N2 C3 C4 125.8(6) ? O1 C4 C3 108.9(5) ? C7 C6 N3 108.2(6) ? C6 C7 N4 107.8(6) ? N3 C9 N4 109.6(5) ? N3 C9 C10 126.7(6) ? N4 C9 C10 123.7(6) ? O2 C10 C9 112.7(6) ? 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 N1 . 1.998(5) yes Zn1 N3 . 2.005(5) yes Zn1 Cl2 . 2.230(2) yes Zn1 Cl1 . 2.247(2) yes N1 C3 . 1.323(7) ? N1 C1 . 1.371(7) ? N2 C3 . 1.323(8) ? N2 C2 . 1.358(9) ? N2 C5 . 1.454(9) ? N3 C9 . 1.306(8) ? N3 C6 . 1.372(7) ? N4 C7 . 1.336(8) ? N4 C9 . 1.341(7) ? N4 C8 . 1.470(8) ? O1 C4 . 1.401(8) ? O2 C10 . 1.358(9) ? C1 C2 . 1.330(9) ? C3 C4 . 1.478(9) ? C6 C7 . 1.325(9) ? C9 C10 . 1.486(8) ? 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 _geom_hbond_publ_flag O1 H1 Cl1 2_556 1.08 1.99 3.071(7) 176.0 yes O2 H2 O1 3_576 1.05 2.35 2.767(10) 102.1 yes O2 H2 O2 3_576 1.05 2.41 2.877(14) 106.1 yes