#------------------------------------------------------------------------------ #$Date: 2011-06-23 21:33:16 +0300 (Thu, 23 Jun 2011) $ #$Revision: 21579 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2000027.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2000027 loop_ _publ_author_name _publ_author_address 'C. D. W. Jones' ; Department of Chemistry Cornell University Ithaca, NY 14853 ; 'F. J. DiSalvo' ; Department of Chemistry Cornell University Ithaca, NY 14853 ; 'R. C. Haushalter' ; NEC Research Institute 4 Independence Way Princeton, NJ 08540 Current Address: Symyx Technologies 420 Oakmead Parkway Sunnyvale, CA 94086 ; _publ_section_title ; Synthesis and X-Ray Crystal Structure of K~4~PbTe~3~.2(en) ; _journal_name_full 'Inorganic Chemistry' _journal_volume 37 _journal_page_first 821 _journal_page_last 823 _journal_year 1998 _publ_contact_author ; Dr. R.C Haushalter Symyx Technologies 420 Oakmead Parkway Sunnyvale, CA 94086 ; _publ_contact_author_phone '408-764-2050' _publ_contact_author_fax '408-732-3949' _publ_contact_author_email 'bhaushalter@symyx.com' _chemical_formula_sum 'C4 H16 K4 N4 Pb Te3' _[local]_cod_chemical_formula_sum_orig 'C4 H16 K4 N4 Pb1 Te3' _cell_volume 1017.609 _exptl_crystal_colour 'silver' _exptl_crystal_density_diffrn 2.828 _exptl_crystal_description 'columnar' _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_gt 0.0384 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 9.044(2) _cell_length_b 9.325(3) _cell_length_c 13.986(5) _cell_angle_alpha 71.21(2) _cell_angle_beta 82.77(2) _cell_angle_gamma 65.69(2) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_measurement_reflns_used 19 _cell_measurement_theta_min 14.3 _cell_measurement_theta_max 19.39 _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _exptl_crystal_F_000 764.0 _exptl_absorpt_coefficient_mu 13.325 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.849 _diffrn_ambient_temperature 295 _diffrn_radiation_wavelength 0.7107 loop_ _atom_type_symbol _atom_type_radius_bond C 0.68 H 0.23 K 1.38 N 0.68 Pb 1.54 Te 1.47 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Pb(1) 0.78810(5) 0.32189(6) 0.76531(4) 0.0469(1) Uij ? ? Te(1) 0.59014(8) 0.21620(9) 0.93936(6) 0.0466(2) Uij ? ? Te(2) 0.97961(9) 0.41496(9) 0.87276(6) 0.0484(2) Uij ? ? Te(3) 1.03413(9) -0.00037(10) 0.74938(6) 0.0498(2) Uij ? ? K(1) 0.0000 0.0000 0.0000 0.0226(8) Uij ? ? K(2) 0.7349(3) 0.4028(3) 1.0848(2) 0.0622(9) Uij ? ? K(3) 0.3333(3) 0.1157(3) 0.8154(2) 0.0635(9) Uij ? ? K(4) 0.7627(3) -0.1796(3) 0.8960(2) 0.0567(9) Uij ? ? K(5) 0.0000 0.0000 0.5000 0.161(3) Uij ? ? N(1a) 0.495(7) 0.760(7) 0.758(2) 0.12(1) Uij ? ? N(1) 0.552(2) 0.788(2) 0.765(1) 0.106(7) Uij ? ? N(2) 0.613(2) 1.048(2) 0.663(1) 0.136(7) Uij ? ? N(2a) 0.802(5) 0.779(5) 0.613(5) 0.15(1) Uij ? ? N(3) 0.225(1) 0.346(1) 0.6102(9) 0.1013 Uij ? ? N(4) 0.191(1) 0.665(1) 0.6061(9) 0.1013 Uij ? ? C(1) 0.550(2) 0.827(2) 0.658(1) 0.107(5) Uij ? ? C(2) 0.656(2) 0.924(2) 0.614(1) 0.145(7) Uij ? ? C(3) 0.234(2) 0.497(2) 0.5414(10) 0.1013 Uij ? ? C(4) 0.339(1) 0.520(2) 0.610(1) 0.1013 Uij ? ? H(1) 0.6133 0.8233 0.7963 0.1275 Uij ? ? H(2) 0.4916 0.7281 0.8059 0.1275 Uij ? ? H(3) 0.5311 1.0562 0.7128 0.1633 Uij ? ? H(4) 0.6662 1.1216 0.6453 0.1633 Uij ? ? H(5) 0.2397 0.3206 0.6808 0.1216 Uij ? ? H(6) 0.2054 0.2729 0.5846 0.1216 Uij ? ? H(7) 0.1815 0.7329 0.6469 0.1216 Uij ? ? H(8) 0.1038 0.6932 0.5631 0.1216 Uij ? ? H(9) 0.5908 0.7278 0.6401 0.1282 Uij ? ? H(10) 0.4416 0.8915 0.6338 0.1282 Uij ? ? H(11) 0.6371 0.9730 0.5431 0.1736 Uij ? ? H(12) 0.7675 0.8524 0.6258 0.1736 Uij ? ? H(13) 0.2858 0.4830 0.4798 0.1216 Uij ? ? H(14) 0.1300 0.5858 0.5273 0.1216 Uij ? ? H(15) 0.4314 0.5391 0.5792 0.1216 Uij ? ? H(16) 0.3679 0.4390 0.6738 0.1216 Uij ? ? 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 Pb(1) 0.0465(3) 0.0429(3) 0.0517(3) -0.0188(2) -0.0072(2) -0.0103(2) Te(1) 0.0296(4) 0.0446(5) 0.0705(6) -0.0151(3) 0.0039(4) -0.0243(4) Te(2) 0.0408(4) 0.0417(5) 0.0717(6) -0.0197(4) 0.0011(4) -0.0242(4) Te(3) 0.0497(5) 0.0551(5) 0.0542(5) -0.0244(4) 0.0047(4) -0.0254(4) K(1) 0.018(1) 0.020(2) 0.033(2) -0.009(1) -0.001(1) -0.012(1) K(2) 0.050(2) 0.044(2) 0.087(2) -0.012(1) 0.003(1) -0.022(2) K(3) 0.046(2) 0.071(2) 0.079(2) -0.023(1) 0.001(1) -0.029(2) K(4) 0.049(2) 0.046(2) 0.080(2) -0.023(1) 0.005(1) -0.023(1) K(5) 0.189(7) 0.277(9) 0.079(4) -0.137(7) 0.032(4) -0.083(5) #------------------------------------------------------------------------------ _refine_special_details 'fixed thermal parameters C(2,3) and N(3,4)' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_number_reflns 2089 _refine_ls_number_parameters 112 _refine_ls_number_restraints 6 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.0384 _refine_ls_wR_factor_obs 0.0430 _refine_ls_goodness_of_fit_obs 2.823 _refine_ls_shift/esd_max 0.0040 _refine_diff_density_min -2.77 _refine_diff_density_max 1.23 #------------------------------------------------------------------------------ loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb(1) Te(1) 2.985(2) ? ? yes Pb(1) Te(2) 2.957(1) ? ? yes Pb(1) Te(3) 2.972(2) ? ? yes Pb(1) K(1) 3.7361(8) ? ? yes Te(1) K(1) 3.473(1) ? ? yes Te(1) K(2) 3.702(5) ? ? yes Te(1) K(2) 3.501(4) ? ? yes Te(1) K(3) 3.624(4) ? ? yes Te(1) K(3) 3.718(5) ? ? yes Te(1) K(4) 3.589(4) ? ? yes Te(1) K(4) 3.761(4) ? ? yes Te(2) K(1) 3.638(1) ? ? yes Te(2) K(2) 3.471(5) ? ? yes Te(2) K(2) 3.815(5) ? ? yes Te(2) K(3) 3.479(4) ? ? yes Te(2) K(4) 3.574(4) ? ? yes Te(2) K(4) 3.718(5) ? ? yes Te(3) K(1) 3.481(1) ? ? yes Te(3) K(2) 3.603(5) ? ? yes Te(3) K(3) 3.609(4) ? ? yes Te(3) K(4) 3.595(4) ? ? yes Te(3) K(5) 3.539(1) ? ? yes K(1) K(2) 4.000(4) ? ? yes K(1) K(2) 4.000(4) ? ? yes K(1) K(3) 3.980(4) ? ? yes K(1) K(3) 3.980(4) ? ? yes K(1) K(4) 3.852(4) ? ? yes K(1) K(4) 3.852(4) ? ? yes K(2) K(2) 4.516(9) ? ? yes K(2) K(3) 4.857(6) ? ? yes K(2) K(4) 4.028(6) ? ? yes K(2) K(4) 4.149(6) ? ? yes K(2) N(1a) 3.28(5) ? ? yes K(3) K(4) 3.773(6) ? ? yes K(3) K(4) 4.200(7) ? ? yes K(3) N(1) 3.13(3) ? ? yes K(3) N(2) 3.09(3) ? ? yes K(3) N(3) 2.97(2) ? ? yes K(4) N(1) 2.96(3) ? ? yes K(5) N(2a) 3.2(1) ? ? yes K(5) N(2a) 3.2(1) ? ? yes K(5) N(4) 2.85(2) ? ? yes K(5) N(4) 2.85(2) ? ? yes N(1a) N(1) 0.7(1) ? ? yes N(1a) C(1) 1.45(1) ? ? yes N(1) C(1) 1.42(1) ? ? yes N(2) C(2) 1.42(1) ? ? yes N(2a) C(2) 1.45(1) ? ? yes N(3) C(3) 1.46(1) ? ? yes N(4) C(4) 1.45(1) ? ? yes C(1) C(2) 1.53(1) ? ? yes C(3) C(4) 1.54(1) ? ? yes #------------------------------------------------------------------------------ _cod_database_code 2000027