#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/21/16/2211656.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_2211656 loop_ _publ_author_name 'Ya-Qian Cheng' 'Lu-Ping Lv' 'Jian-Wu Xie' 'Hai-Bin Wang' 'Zhi-Min Jin' _publ_section_title ; Ammonium trichloro(hexamethylenetetramine)zincate(II) sesquihydrate ; _journal_coeditor_code WM2072 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m3591 _journal_page_last m3593 _journal_volume 62 _journal_year 2006 _chemical_formula_iupac '(N H4) [Zn Cl3 (C6 H12 N4)], 1.5H 2O' _chemical_formula_moiety 'N H4 +, C6 H12 Cl3 N4 Zn -, 1.5(H2 O)' _chemical_formula_sum 'C6 H19 Cl3 N5 O1.5 Zn' _chemical_formula_weight 357.96 _chemical_name_systematic ; Ammonium trichloro(hexamethylenetetramine)zincate 1.5-hydrate ; _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 _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 94.842(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.7692(19) _cell_length_b 9.621(2) _cell_length_c 17.137(4) _cell_measurement_reflns_used 3136 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 27.0 _cell_measurement_theta_min 2.3 _cell_volume 1440.7(5) _computing_cell_refinement SMART _computing_data_collection 'SMART (Bruker, 2002)' _computing_data_reduction 'SAINT (Bruker, 2002)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXTL (Bruker, 2002)' _diffrn_ambient_temperature 273(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker SMART APEX CCD 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 0.0254 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 8538 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_min 2.33 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.258 _exptl_absorpt_correction_T_max 0.499 _exptl_absorpt_correction_T_min 0.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS; Bruker, 2002)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.32 _refine_diff_density_max 0.334 _refine_diff_density_min -0.347 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 187 _refine_ls_number_reflns 3136 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all 0.0484 _refine_ls_R_factor_gt 0.0395 _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^)+(0.0367P)^2^+0.9695P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0890 _refine_ls_wR_factor_ref 0.0931 _reflns_number_gt 2694 _reflns_number_total 3136 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wm2072.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_chemical_formula_sum_orig 'C6 H19 Cl3 N5 O1.50 Zn' _cod_original_cell_volume 1440.6(5) _cod_database_code 2211656 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' 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_ _atom_site_type_symbol _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_group Zn Zn1 0.64545(3) 0.04267(3) 0.83373(2) 0.03070(12) Uani d . 1 . Cl Cl1 0.69797(10) 0.04665(9) 0.70755(5) 0.0479(2) Uani d . 1 . Cl Cl2 0.72682(9) -0.15574(8) 0.89069(5) 0.0429(2) Uani d . 1 . Cl Cl3 0.73478(10) 0.23086(10) 0.90084(6) 0.0576(3) Uani d . 1 . O O1 0.1794(3) 0.4063(3) 0.97510(14) 0.0424(5) Uani d D 1 . N N5 0.0184(3) 0.6316(3) 0.89970(17) 0.0352(6) Uani d . 1 . O O2 0.4684(18) 0.511(2) 1.0414(10) 0.078(4) Uani d P 0.25 1 O O2' 0.4768(19) 0.5626(16) 0.9878(16) 0.079(4) Uani d P 0.25 2 N N1 0.4053(2) 0.0394(2) 0.83495(13) 0.0243(5) Uani d . 1 . N N2 0.1795(3) -0.0946(2) 0.86587(15) 0.0317(5) Uani d . 1 . N N3 0.1616(3) 0.0665(3) 0.75544(14) 0.0341(6) Uani d . 1 . N N4 0.1887(3) 0.1553(2) 0.88907(14) 0.0321(5) Uani d . 1 . C C1 0.3468(3) -0.0951(3) 0.86481(17) 0.0311(6) Uani d . 1 . H H1A 0.3767 -0.1705 0.8318 0.037 Uiso calc R 1 . H H1B 0.3931 -0.1115 0.9174 0.037 Uiso calc R 1 . C C2 0.1113(3) -0.0675(3) 0.78613(18) 0.0358(7) Uani d . 1 . H H2A 0.0007 -0.0674 0.7862 0.043 Uiso calc R 1 . H H2B 0.1395 -0.1417 0.7518 0.043 Uiso calc R 1 . C C3 0.1198(3) 0.1767(3) 0.80870(19) 0.0376(7) Uani d . 1 . H H3A 0.0093 0.1797 0.8091 0.045 Uiso calc R 1 . H H3B 0.1532 0.2656 0.7895 0.045 Uiso calc R 1 . C C4 0.3553(3) 0.1522(3) 0.88707(17) 0.0297(6) Uani d . 1 . H H4A 0.4025 0.1380 0.9397 0.036 Uiso calc R 1 . H H4B 0.3898 0.2412 0.8686 0.036 Uiso calc R 1 . C C5 0.3289(3) 0.0635(3) 0.75469(17) 0.0331(6) Uani d . 1 . H H5A 0.3638 0.1511 0.7345 0.040 Uiso calc R 1 . H H5B 0.3577 -0.0100 0.7200 0.040 Uiso calc R 1 . C C6 0.1358(3) 0.0197(3) 0.91692(17) 0.0330(6) Uani d . 1 . H H6A 0.1802 0.0036 0.9699 0.040 Uiso calc R 1 . H H6B 0.0254 0.0214 0.9179 0.040 Uiso calc R 1 . H H5F -0.047(4) 0.638(4) 0.935(2) 0.052(11) Uiso d . 1 . H H5E 0.078(4) 0.567(4) 0.912(2) 0.042(10) Uiso d . 1 . H H5C -0.034(5) 0.611(4) 0.849(3) 0.075(13) Uiso d . 1 . H H1WA 0.178(5) 0.333(3) 0.950(3) 0.11(2) Uiso d D 1 . H H1WB 0.267(4) 0.426(5) 0.997(3) 0.15(3) Uiso d D 1 . H H5D 0.064(5) 0.715(5) 0.891(3) 0.088(15) Uiso d . 1 . 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 0.02226(18) 0.0319(2) 0.0383(2) 0.00374(13) 0.00418(13) 0.00107(14) Cl1 0.0440(5) 0.0569(5) 0.0454(5) 0.0089(4) 0.0193(4) 0.0106(4) Cl2 0.0416(4) 0.0394(4) 0.0460(4) 0.0145(3) -0.0051(3) 0.0039(3) Cl3 0.0395(5) 0.0479(5) 0.0851(7) -0.0072(4) 0.0043(4) -0.0217(5) O1 0.0507(15) 0.0371(13) 0.0405(13) 0.0130(11) 0.0104(11) 0.0021(10) N5 0.0349(15) 0.0373(16) 0.0339(15) 0.0104(13) 0.0057(12) 0.0075(12) O2 0.085(10) 0.072(10) 0.073(11) 0.013(9) -0.019(8) -0.023(11) O2' 0.071(9) 0.082(11) 0.079(12) 0.001(8) -0.013(8) -0.027(11) N1 0.0208(11) 0.0245(12) 0.0277(11) 0.0008(9) 0.0026(9) -0.0002(9) N2 0.0244(12) 0.0294(12) 0.0414(14) -0.0029(10) 0.0038(10) 0.0020(11) N3 0.0230(12) 0.0462(15) 0.0325(13) -0.0001(10) -0.0014(10) 0.0042(11) N4 0.0214(11) 0.0328(13) 0.0426(14) 0.0015(10) 0.0048(10) -0.0070(11) C1 0.0294(14) 0.0244(14) 0.0395(16) 0.0012(11) 0.0026(12) 0.0040(12) C2 0.0266(14) 0.0386(17) 0.0417(17) -0.0054(12) -0.0007(12) -0.0085(13) C3 0.0237(14) 0.0339(16) 0.0549(19) 0.0052(12) 0.0019(13) 0.0081(14) C4 0.0219(13) 0.0297(15) 0.0375(15) 0.0013(11) 0.0016(11) -0.0064(12) C5 0.0250(14) 0.0459(18) 0.0281(14) -0.0007(12) 0.0016(11) 0.0034(12) C6 0.0259(14) 0.0408(17) 0.0328(15) -0.0013(12) 0.0052(11) 0.0010(13) 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 . 2.108(2) yes Zn1 Cl2 . 2.2335(9) yes Zn1 Cl1 . 2.2487(10) yes Zn1 Cl3 . 2.2500(10) yes O1 H1WA . 0.823(18) ? O1 H1WB . 0.842(19) ? N5 H5F . 0.87(4) ? N5 H5E . 0.82(4) ? N5 H5C . 0.97(4) ? N5 H5D . 0.92(5) ? O2 O2 3_667 1.58(3) ? O2' O2' 3_667 1.33(3) ? N1 C4 . 1.494(3) yes N1 C5 . 1.496(3) yes N1 C1 . 1.498(3) yes N2 C2 . 1.468(4) yes N2 C1 . 1.469(3) yes N2 C6 . 1.476(4) yes N3 C3 . 1.466(4) yes N3 C5 . 1.469(3) yes N3 C2 . 1.474(4) yes N4 C4 . 1.464(3) yes N4 C3 . 1.471(4) yes N4 C6 . 1.477(4) yes C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? 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 Cl2 105.41(6) yes N1 Zn1 Cl1 107.20(6) yes Cl2 Zn1 Cl1 110.54(3) yes N1 Zn1 Cl3 108.17(6) yes Cl2 Zn1 Cl3 112.32(4) yes Cl1 Zn1 Cl3 112.77(4) yes H1WA O1 H1WB 113(3) ? H5F N5 H5E 109(3) ? H5F N5 H5C 110(3) ? H5E N5 H5C 108(3) ? H5F N5 H5D 112(4) ? H5E N5 H5D 115(3) ? H5C N5 H5D 103(4) ? C4 N1 C5 107.8(2) ? C4 N1 C1 107.3(2) ? C5 N1 C1 107.9(2) ? C4 N1 Zn1 109.81(15) yes C5 N1 Zn1 111.01(16) yes C1 N1 Zn1 112.80(15) yes C2 N2 C1 108.5(2) ? C2 N2 C6 108.3(2) ? C1 N2 C6 108.6(2) ? C3 N3 C5 108.8(2) ? C3 N3 C2 108.2(2) ? C5 N3 C2 108.4(2) ? C4 N4 C3 108.2(2) ? C4 N4 C6 109.4(2) ? C3 N4 C6 108.1(2) ? N2 C1 N1 111.9(2) ? N2 C1 H1A 109.2 ? N1 C1 H1A 109.2 ? N2 C1 H1B 109.2 ? N1 C1 H1B 109.2 ? H1A C1 H1B 107.9 ? N2 C2 N3 112.2(2) ? N2 C2 H2A 109.2 ? N3 C2 H2A 109.2 ? N2 C2 H2B 109.2 ? N3 C2 H2B 109.2 ? H2A C2 H2B 107.9 ? N3 C3 N4 112.1(2) ? N3 C3 H3A 109.2 ? N4 C3 H3A 109.2 ? N3 C3 H3B 109.2 ? N4 C3 H3B 109.2 ? H3A C3 H3B 107.9 ? N4 C4 N1 111.8(2) ? N4 C4 H4A 109.2 ? N1 C4 H4A 109.2 ? N4 C4 H4B 109.2 ? N1 C4 H4B 109.2 ? H4A C4 H4B 107.9 ? N3 C5 N1 111.4(2) ? N3 C5 H5A 109.3 ? N1 C5 H5A 109.3 ? N3 C5 H5B 109.3 ? N1 C5 H5B 109.3 ? H5A C5 H5B 108.0 ? N2 C6 N4 111.2(2) ? N2 C6 H6A 109.4 ? N4 C6 H6A 109.4 ? N2 C6 H6B 109.4 ? N4 C6 H6B 109.4 ? H6A C6 H6B 108.0 ? 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 H1WA N4 1_555 0.823(18) 2.012(19) 2.834(3) 176(3) yes O1 H1WB O2 1_555 0.842(19) 2.040(19) 2.871(17) 169(3) yes O1 H1WB O2' 1_555 0.842(19) 2.279(19) 3.002(16) 144(3) yes O1 H1WB O2 3_667 0.842(19) 2.538(19) 3.225(17) 139(3) yes O1 H1WB O2' 3_667 0.842(19) 2.245(19) 3.043(17) 158(3) yes N5 H5E O1 1_555 0.82(4) 2.05(4) 2.838(4) 160(3) yes N5 H5F O1 3_567 0.87(4) 2.05(4) 2.894(4) 163 yes N5 H5C N3 2_556 0.97(4) 2.08(4) 3.040(4) 176(3) yes N5 H5D N2 1_565 0.92(5) 2.15(5) 3.067(4) 177(4) yes C1 H1A Cl1 2_646 0.97 2.87 3.673(3) 141 yes C5 H5A Cl2 2_656 0.97 2.90 3.679(3) 138 yes C6 H6A Cl2 3_657 0.97 2.86 3.655(3) 140 yes _cod_database_fobs_code 2211656 _journal_paper_doi 10.1107/S1600536806050550