#------------------------------------------------------------------------------ #$Date: 2012-02-03 17:16:24 +0000 (Fri, 03 Feb 2012) $ #$Revision: 32112 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/25/2012565.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_2012565 loop_ _publ_author_name 'Zhu, Miaoli' 'Lu, Liping' 'Jin, Xianglin' 'Yang, Pin' _publ_section_title ; Trichloro(1,1-dimethylbiguanidium-\kN^3^)zinc(II) ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m158 _journal_page_last m159 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Zn (C4 H12 N5) Cl3]' _chemical_formula_moiety 'C4 H12 Cl3 N5 Zn' _chemical_formula_sum 'C4 H12 Cl3 N5 Zn' _chemical_formula_weight 301.91 _chemical_name_common 'Trichloro(N, N-dimethylbiguanidium)zinc(II)' _chemical_name_systematic ; Trichloro(1,1-dimethylbiguanidium-\kN^3^)zinc(II) ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_method SHELXL97 _cell_angle_alpha 90 _cell_angle_beta 113.237(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.5040(7) _cell_length_b 7.5170(5) _cell_length_c 13.0894(5) _cell_measurement_reflns_used 10407 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 27.48 _cell_measurement_theta_min 3.14 _cell_volume 1130.50(11) _computing_cell_refinement 'Please provide missing details' _computing_data_collection 'Please provide missing details' _computing_data_reduction 'Please provide missing details' _computing_molecular_graphics 'Please provide missing details' _computing_publication_material 'Please provide missing details' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean '100 \\times 100 microns' _diffrn_measured_fraction_theta_full .923 _diffrn_measured_fraction_theta_max .923 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID image-plate' _diffrn_measurement_method oscillation _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .029 _diffrn_reflns_av_sigmaI/netI .033 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 10407 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_min 3.14 _diffrn_standards_decay_% +/-1 _diffrn_standards_interval_time 60 _exptl_absorpt_coefficient_mu 2.847 _exptl_absorpt_correction_T_max .566 _exptl_absorpt_correction_T_min .402 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.774 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 608 _exptl_crystal_size_max .4 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .2 _refine_diff_density_max .36 _refine_diff_density_min -.56 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref .943 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 138 _refine_ls_number_reflns 2574 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all .943 _refine_ls_R_factor_all .031 _refine_ls_R_factor_gt .022 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_scheme 'calc w = 1/[\s^2^(Fo^2^)+(0.0243P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_wR_factor_gt .046 _refine_ls_wR_factor_ref .048 _reflns_number_gt 2107 _reflns_number_total 2574 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file de1178.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/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 1130.50(10) _cod_database_code 2012565 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 .282952(17) .13965(3) .297150(16) .01607(6) Uani d . 1 . . Zn Cl2 .13650(4) .15467(6) .12736(3) .02258(11) Uani d . 1 . . Cl Cl3 .46377(4) .10263(6) .30140(4) .02117(10) Uani d . 1 . . Cl Cl4 .24484(4) -.07610(6) .39974(4) .02573(11) Uani d . 1 . . Cl N1 .37182(15) .5511(2) .53957(14) .0223(4) Uani d . 1 . . N N2 .28448(12) .37208(18) .38125(11) .0151(3) Uani d . 1 . . N N3 .17053(12) .5575(2) .23638(12) .0181(3) Uani d . 1 . . N N4 .11663(14) .5076(2) .38315(14) .0210(3) Uani d . 1 . . N N5 .41223(15) .2538(2) .54696(13) .0236(4) Uani d . 1 . . N C1 .35440(14) .3930(2) .49044(14) .0156(3) Uani d . 1 . . C C2 .19093(14) .4857(2) .33386(13) .0144(3) Uani d . 1 . . C C3 .05951(18) .6452(3) .17234(17) .0310(5) Uani d . 1 . . C H3A -.0031 .5759 .1765 .047 Uiso calc R 1 . . H H3B .0499 .6557 .0961 .047 Uiso calc R 1 . . H H3C .0590 .7615 .2024 .047 Uiso calc R 1 . . H C4 .26062(18) .5749(3) .19237(16) .0280(4) Uani d . 1 . . C H4A .3297 .5144 .2405 .042 Uiso calc R 1 . . H H4B .2777 .6985 .1882 .042 Uiso calc R 1 . . H H4C .2337 .5233 .1194 .042 Uiso calc R 1 . . H H11A .408(3) .560(4) .612(3) .080 Uiso d . 1 . . H H11B .349(3) .641(4) .508(3) .080 Uiso d . 1 . . H H14A .130(3) .455(4) .443(3) .080 Uiso d . 1 . . H H14B .071(3) .590(4) .363(3) .080 Uiso d . 1 . . H H15A .393(3) .157(4) .521(3) .080 Uiso d . 1 . . H H15B .464(3) .268(4) .619(2) .080 Uiso d . 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 .01686(11) .01453(11) .01636(11) .00090(8) .00607(8) -.00130(8) Cl2 .0184(2) .0303(3) .0166(2) -.00188(19) .00421(17) -.00273(18) Cl3 .0171(2) .0266(2) .0195(2) .00454(18) .00692(16) .00075(18) Cl4 .0347(3) .0171(2) .0251(2) -.0039(2) .0115(2) .00226(18) N1 .0289(9) .0171(8) .0167(8) -.0012(7) .0045(7) -.0016(6) N2 .0179(7) .0116(7) .0135(7) .0021(6) .0038(6) .0001(6) N3 .0199(7) .0158(8) .0166(7) .0025(6) .0052(6) .0029(6) N4 .0196(8) .0235(9) .0222(8) .0015(7) .0110(7) .0011(7) N5 .0286(9) .0198(9) .0167(8) .0066(7) .0028(7) .0020(7) C1 .0143(8) .0182(9) .0146(8) .0000(7) .0060(6) .0009(7) C2 .0141(8) .0100(8) .0179(8) -.0029(7) .0050(7) -.0025(7) C3 .0276(11) .0291(11) .0278(11) .0085(9) .0018(8) .0081(9) C4 .0353(11) .0290(11) .0267(10) .0001(9) .0197(9) .0063(9) 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 N2 . 2.0611(14) y Zn1 Cl3 . 2.2568(7) y Zn1 Cl2 . 2.2570(5) y Zn1 Cl4 . 2.2728(6) y N1 C1 . 1.328(2) y N2 C1 . 1.359(2) y N2 C2 . 1.382(2) y N3 C2 . 1.314(2) y N3 C4 . 1.459(2) y N3 C3 . 1.465(2) y N4 C2 . 1.334(2) y N5 C1 . 1.320(2) y N1 H11A . .88(3) ? N1 H11B . .78(3) ? N4 H14A . .83(3) ? N4 H14B . .81(3) ? N5 H15A . .80(3) ? N5 H15B . .92(3) ? C3 H3A . .9600 ? C3 H3B . .9600 ? C3 H3C . .9600 ? C4 H4A . .9600 ? C4 H4B . .9600 ? C4 H4C . .9600 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .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 N2 Zn1 Cl3 107.05(4) y N2 Zn1 Cl2 108.45(4) y Cl3 Zn1 Cl2 116.50(3) y N2 Zn1 Cl4 104.43(4) y Cl3 Zn1 Cl4 109.82(3) y Cl2 Zn1 Cl4 109.86(2) y C1 N2 C2 118.68(14) y C1 N2 Zn1 121.78(11) y C2 N2 Zn1 117.15(11) y C2 N3 C4 122.38(15) y C2 N3 C3 121.16(16) y C4 N3 C3 116.02(15) y N5 C1 N1 119.29(16) y N5 C1 N2 118.71(16) y N1 C1 N2 121.86(15) y N3 C2 N4 120.89(16) y N3 C2 N2 119.69(15) y N4 C2 N2 119.13(15) y C1 N1 H11A 121(2) ? C1 N1 H11B 124(2) ? H11A N1 H11B 116(3) ? C2 N4 H14A 118(2) ? C2 N4 H14B 118(2) ? H14A N4 H14B 122(3) ? C1 N5 H15A 118(2) ? C1 N5 H15B 120(2) ? H15A N5 H15B 121(3) ? N3 C3 H3A 109.5 ? N3 C3 H3B 109.5 ? H3A C3 H3B 109.5 ? N3 C3 H3C 109.5 ? H3A C3 H3C 109.5 ? H3B C3 H3C 109.5 ? N3 C4 H4A 109.5 ? N3 C4 H4B 109.5 ? H4A C4 H4B 109.5 ? N3 C4 H4C 109.5 ? H4A C4 H4C 109.5 ? H4B C4 H4C 109.5 ? 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 _geom_torsion_publ_flag Zn1 N2 C1 N5 -8.2(2) y Zn1 N2 C1 N1 167.41(13) y Zn1 N2 C2 N4 111.06(16) y Zn1 N2 C2 N3 -62.77(19) y Cl4 Zn1 N2 C2 -107.20(12) y Cl2 Zn1 N2 C2 9.91(13) y Cl3 Zn1 N2 C2 136.37(11) y C4 N3 C2 N4 164.46(17) y C3 N3 C2 N4 -7.6(3) y N3 C2 N2 C1 134.46(17) y N1 C1 N2 C2 -30.7(2) y N5 C1 N2 C2 153.77(16) y N3 C2 N4 N2 173.8(3) y N2 C1 N1 N5 -175.5(3) y