#------------------------------------------------------------------------------ #$Date: 2011-09-17 21:27:16 +0100 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: svn://www.crystallography.net/cod/cif/2/2206901.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_2206901 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M 'P 21/c' loop_ _publ_author_name 'Fowkes, Adrian' 'Harrison, William T. A.' _publ_section_title ; A monoclinic polymorph of dichlorobis(cyanoguanidine)zinc(II) ; _journal_coeditor_code CF6454 _journal_issue 10 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m2021 _journal_page_last m2022 _journal_volume 61 _journal_year 2005 _chemical_formula_iupac '[Cn Cl2 (C4 H8 N8)]' _chemical_formula_moiety 'C4 H8 Cl2 N8 Zn' _chemical_formula_sum 'C4 H8 Cl2 N8 Zn' _chemical_formula_weight 304.45 _chemical_name_systematic ; dichlorobis(cyanoguanidine)zinc(II) ; _symmetry_cell_setting monoclinic _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 93.928(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 4.9315(3) _cell_length_b 14.6161(10) _cell_length_c 15.5026(11) _cell_measurement_reflns_used 2094 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.82 _cell_measurement_theta_min 2.63 _cell_volume 1114.79(13) _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_data_reduction SAINT _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method \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 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 7331 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 1.92 _diffrn_standards_decay_% 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.664 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_correction_T_min 0.495 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 1999)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.814 _exptl_crystal_density_method 'not measured' _exptl_crystal_description bar _exptl_crystal_F_000 608 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.382 _refine_diff_density_min -0.336 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 2444 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.908 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0353 _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^)+(0.0345P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0692 _refine_ls_wR_factor_ref 0.0768 _reflns_number_gt 1610 _reflns_number_total 2444 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cf6454.cif 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_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' 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_ _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 0.57190(7) 0.26684(3) 0.41448(2) 0.03114(12) Uani d . 1 Zn Cl1 0.77571(18) 0.35115(6) 0.31465(5) 0.0421(2) Uani d . 1 Cl Cl2 0.35476(17) 0.35081(7) 0.50813(6) 0.0427(2) Uani d . 1 Cl N1 0.8270(5) 0.1795(2) 0.47356(17) 0.0377(7) Uani d . 1 N C1 1.0125(7) 0.1372(2) 0.4988(2) 0.0305(7) Uani d . 1 C N2 1.2201(5) 0.0859(2) 0.52099(17) 0.0358(7) Uani d . 1 N C2 1.3399(7) 0.0944(2) 0.6013(2) 0.0324(8) Uani d . 1 C N3 1.2696(6) 0.1547(2) 0.65774(19) 0.0515(9) Uani d . 1 N H1 1.3542 0.1569 0.7081 0.062 Uiso calc R 1 H H2 1.1387 0.1921 0.6446 0.062 Uiso calc R 1 H N4 1.5405(6) 0.0377(2) 0.62248(18) 0.0463(8) Uani d . 1 N H3 1.6237 0.0405 0.6730 0.056 Uiso calc R 1 H H4 1.5885 -0.0023 0.5858 0.056 Uiso calc R 1 H N5 0.3319(6) 0.1889(2) 0.33726(18) 0.0390(7) Uani d . 1 N C3 0.2135(7) 0.1398(2) 0.2928(2) 0.0328(8) Uani d . 1 C N6 0.1010(6) 0.0754(2) 0.2464(2) 0.0501(9) Uani d . 1 N C4 -0.0951(7) 0.0945(3) 0.1849(2) 0.0374(8) Uani d . 1 C N7 -0.2052(6) 0.1752(2) 0.17497(18) 0.0440(8) Uani d . 1 N H5 -0.3277 0.1847 0.1338 0.053 Uiso calc R 1 H H6 -0.1555 0.2189 0.2097 0.053 Uiso calc R 1 H N8 -0.1731(7) 0.0286(2) 0.1315(2) 0.0587(10) Uani d . 1 N H7 -0.2957 0.0388 0.0905 0.070 Uiso calc R 1 H H8 -0.1016 -0.0249 0.1375 0.070 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 Zn1 0.0351(2) 0.0310(2) 0.02591(19) 0.00114(19) -0.00776(14) 0.00054(18) Cl1 0.0544(5) 0.0371(6) 0.0336(5) -0.0095(4) -0.0057(4) 0.0064(4) Cl2 0.0458(5) 0.0462(6) 0.0349(5) 0.0078(4) -0.0073(4) -0.0088(4) N1 0.0362(15) 0.0371(19) 0.0380(16) 0.0058(14) -0.0092(13) 0.0066(14) C1 0.0336(17) 0.033(2) 0.0238(16) -0.0042(15) -0.0018(14) 0.0007(14) N2 0.0376(15) 0.0360(18) 0.0323(15) 0.0105(13) -0.0083(12) -0.0020(13) C2 0.0345(16) 0.033(2) 0.0289(17) 0.0001(15) -0.0026(14) 0.0023(15) N3 0.0550(18) 0.063(3) 0.0347(17) 0.0247(17) -0.0107(15) -0.0110(16) N4 0.0561(18) 0.044(2) 0.0356(17) 0.0196(16) -0.0203(14) -0.0042(14) N5 0.0400(15) 0.040(2) 0.0350(16) -0.0022(14) -0.0094(13) -0.0020(14) C3 0.0372(17) 0.031(2) 0.0291(17) 0.0031(15) -0.0086(15) 0.0076(15) N6 0.065(2) 0.0292(19) 0.0513(19) 0.0025(15) -0.0324(17) -0.0066(15) C4 0.0428(19) 0.034(2) 0.0335(18) -0.0035(16) -0.0102(16) -0.0018(16) N7 0.0536(17) 0.038(2) 0.0375(17) 0.0079(15) -0.0196(14) -0.0067(14) N8 0.072(2) 0.037(2) 0.061(2) 0.0068(17) -0.0378(19) -0.0153(17) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Zn1 N1 1.974(3) y Zn1 N5 1.984(3) y Zn1 Cl2 2.2302(10) y Zn1 Cl1 2.2664(10) y N1 C1 1.150(4) ? C1 N2 1.296(4) ? N2 C2 1.347(4) ? C2 N3 1.305(4) ? C2 N4 1.315(4) ? N3 H1 0.860 ? N3 H2 0.860 ? N4 H3 0.860 ? N4 H4 0.860 ? N5 C3 1.130(4) ? C3 N6 1.287(4) ? N6 C4 1.340(4) ? C4 N7 1.303(5) ? C4 N8 1.310(4) ? N7 H5 0.860 ? N7 H6 0.860 ? N8 H7 0.860 ? N8 H8 0.860 ? 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 N5 104.10(13) ? N1 Zn1 Cl2 111.92(9) ? N5 Zn1 Cl2 114.55(9) ? N1 Zn1 Cl1 111.74(9) ? N5 Zn1 Cl1 100.03(9) ? Cl2 Zn1 Cl1 113.61(4) ? C1 N1 Zn1 166.5(3) y N1 C1 N2 175.1(4) ? C1 N2 C2 118.7(3) ? N3 C2 N4 119.2(3) ? N3 C2 N2 124.2(3) ? N4 C2 N2 116.5(3) ? C2 N3 H1 120.0 ? C2 N3 H2 120.0 ? H1 N3 H2 120.0 ? C2 N4 H3 120.0 ? C2 N4 H4 120.0 ? H3 N4 H4 120.0 ? C3 N5 Zn1 174.2(3) y N5 C3 N6 172.2(4) ? C3 N6 C4 120.5(3) ? N7 C4 N8 119.3(3) ? N7 C4 N6 123.1(3) ? N8 C4 N6 117.5(3) ? C4 N7 H5 120.0 ? C4 N7 H6 120.0 ? H5 N7 H6 120.0 ? C4 N8 H7 120.0 ? C4 N8 H8 120.0 ? H7 N8 H8 120.0 ? 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 N5 Zn1 N1 C1 112.9(12) Cl2 Zn1 N1 C1 -122.8(12) Cl1 Zn1 N1 C1 5.9(13) C1 N2 C2 N3 -3.6(5) C1 N2 C2 N4 176.5(3) C3 N6 C4 N8 170.1(4) 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 N4 H3 N6 3_756 0.86 2.46 3.082(4) 130 yes N4 H4 N2 3_856 0.86 2.31 3.156(4) 168 yes N3 H1 Cl1 4_666 0.86 2.57 3.365(3) 155 yes N4 H3 Cl1 4_666 0.86 2.77 3.520(3) 147 yes N7 H5 Cl2 4_465 0.86 2.47 3.282(3) 158 yes N7 H6 Cl1 1_455 0.86 2.56 3.368(3) 156 yes N8 H7 Cl2 4_465 0.86 2.63 3.402(3) 151 yes N8 H8 Cl1 2_645 0.86 2.50 3.322(3) 160 yes _cod_database_code 2206901