#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2102943.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_2102943 loop_ _publ_author_name 'Billing, David G.' 'Lemmerer, Andreas' _publ_section_title ; Synthesis, characterization and phase transitions in the inorganic--organic layered perovskite-type hybrids [(C~n~H~2n~ + 1NH~3~)~2~PbI~4~], n = 4, 5 and 6 ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 735 _journal_page_last 747 _journal_volume 63 _journal_year 2007 _chemical_formula_moiety '2(C6 H16 N), I4 Pb' _chemical_formula_sum 'C12 H32 I4 N2 Pb' _chemical_formula_weight 919.19 _chemical_name_systematic ; bis(hexylammonium)tetraiodoplumbate(II) ; _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M Pbca _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_creation_method 'WinGX routine CIF_UPDATE' _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.9413(2) _cell_length_b 8.6874(2) _cell_length_c 32.7027(10) _cell_measurement_reflns_used 5270 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.94 _cell_measurement_theta_min 2.6 _cell_volume 2540.24(11) _computing_cell_refinement 'SAINT-Plus (Bruker, 2004)' _computing_data_collection 'APEX2 (Bruker, 2005)' _computing_data_reduction 'SAINT-Plus and XPREP (Bruker 2004)' _computing_molecular_graphics ; Ortep-3 for Windows (Farrugia, 1997) and DIAMOND (Brandenburg, 1999) ; _computing_publication_material ; WinGX publication routines (Farrugia, 1999) and PLATON (Spek, 2003) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX II CCD area detector' _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 0.0447 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_number 12552 _diffrn_reflns_theta_full 28 _diffrn_reflns_theta_max 28 _diffrn_reflns_theta_min 2.6 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.498 _exptl_absorpt_correction_T_max 0.5361 _exptl_absorpt_correction_T_min 0.0582 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'Bruker XPREP (Bruker, 2004)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.403 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 1648 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.651 _refine_diff_density_min -1.693 _refine_ls_extinction_coef 0.00037(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.335 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 89 _refine_ls_number_reflns 3056 _refine_ls_number_restraints 56 _refine_ls_restrained_S_all 1.33 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0814 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+101.7161P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1636 _refine_ls_wR_factor_ref 0.1682 _reflns_number_gt 2421 _reflns_number_total 3056 _reflns_threshold_expression >2sigma(I) _[local]_cod_data_source_file bs5044.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.025 0 0 -1 0.025 1 0 0 0.14 -1 0 0 0.14 0 -1 0 0.23 0 1 0 0.23 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 0 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 '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 C C1 0.970(4) 0.463(4) 0.9038(6) 0.120(8) Uani d DU 1 H H1D 0.8689 0.4845 0.913 0.144 Uiso calc R 1 H H1E 0.9957 0.358 0.9111 0.144 Uiso calc R 1 C C2 0.985(4) 0.489(4) 0.8585(6) 0.136(8) Uani d DU 1 H H2A 1.0882 0.4693 0.8508 0.163 Uiso calc R 1 H H2B 0.9647 0.5967 0.8528 0.163 Uiso calc R 1 C C3 0.883(4) 0.391(4) 0.8320(6) 0.148(8) Uani d DU 1 H H3A 0.7796 0.4145 0.8379 0.177 Uiso calc R 1 H H3B 0.8999 0.2824 0.8379 0.177 Uiso calc R 1 C C4 0.917(4) 0.423(4) 0.7872(6) 0.164(9) Uani d DU 1 H H4A 0.8935 0.5296 0.7813 0.197 Uiso calc R 1 H H4B 1.0236 0.409 0.7825 0.197 Uiso calc R 1 C C5 0.832(4) 0.321(4) 0.7578(7) 0.177(10) Uani d DU 1 H H5A 0.7256 0.3351 0.762 0.213 Uiso calc R 1 H H5B 0.8561 0.2144 0.7632 0.213 Uiso calc R 1 C C6 0.871(5) 0.360(5) 0.7136(7) 0.202(15) Uani d DU 1 H H6A 0.8147 0.294 0.6956 0.303 Uiso calc R 1 H H6B 0.9758 0.3435 0.7091 0.303 Uiso calc R 1 H H6C 0.8463 0.4652 0.7081 0.303 Uiso calc R 1 N N1 1.078(2) 0.574(2) 0.9216(7) 0.086(5) Uani d U 1 H H1A 1.0749 0.5688 0.9488 0.129 Uiso calc R 1 H H1B 1.055 0.6691 0.9136 0.129 Uiso calc R 1 H H1C 1.1703 0.5512 0.9131 0.129 Uiso calc R 1 I I1 1.03252(17) 0.98288(17) 0.90247(5) 0.0689(4) Uani d . 1 I I2 0.69807(13) 1.19581(14) 0.99628(5) 0.0637(4) Uani d . 1 Pb Pb1 1 1 1 0.0443(3) Uani d S 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 C1 0.112(16) 0.122(17) 0.127(12) -0.016(13) -0.005(15) -0.027(16) C2 0.137(17) 0.145(18) 0.126(12) 0.005(15) -0.008(14) -0.028(15) C3 0.149(18) 0.164(19) 0.130(12) 0.012(17) -0.022(15) -0.035(16) C4 0.17(2) 0.19(2) 0.129(12) 0.02(2) -0.022(16) -0.032(17) C5 0.18(2) 0.22(2) 0.132(14) 0.02(2) -0.029(18) -0.041(19) C6 0.22(3) 0.26(4) 0.126(13) 0.05(3) -0.03(2) -0.03(2) N1 0.057(10) 0.082(13) 0.120(13) 0.016(9) -0.003(10) -0.003(11) I1 0.0759(9) 0.0620(8) 0.0687(9) 0.0080(8) -0.0078(7) 0.0020(7) I2 0.0451(6) 0.0439(6) 0.1019(11) 0.0175(5) -0.0117(7) -0.0073(7) Pb1 0.0328(4) 0.0322(4) 0.0679(6) 0.0001(3) -0.0003(4) 0.0003(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance C1 N1 . 1.49(3) C1 C2 . 1.504(10) C1 H1D . 0.97 C1 H1E . 0.97 C2 C3 . 1.522(10) C2 H2A . 0.97 C2 H2B . 0.97 C3 C4 . 1.525(10) C3 H3A . 0.97 C3 H3B . 0.97 C4 C5 . 1.510(10) C4 H4A . 0.97 C4 H4B . 0.97 C5 C6 . 1.523(10) C5 H5A . 0.97 C5 H5B . 0.97 C6 H6A . 0.96 C6 H6B . 0.96 C6 H6C . 0.96 N1 H1A . 0.89 N1 H1B . 0.89 N1 H1C . 0.89 I1 Pb1 . 3.2062(15) I2 Pb1 4_477 3.1835(11) I2 Pb1 . 3.1932(11) Pb1 I2 8_755 3.1835(11) Pb1 I2 4_577 3.1835(11) Pb1 I2 5_777 3.1932(11) Pb1 I1 5_777 3.2062(15) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle N1 C1 C2 . . 103(2) N1 C1 H1D . . 111.1 C2 C1 H1D . . 111.1 N1 C1 H1E . . 111.1 C2 C1 H1E . . 111.1 H1D C1 H1E . . 109.1 C1 C2 C3 . . 114.9(14) C1 C2 H2A . . 108.5 C3 C2 H2A . . 108.5 C1 C2 H2B . . 108.5 C3 C2 H2B . . 108.5 H2A C2 H2B . . 107.5 C2 C3 C4 . . 109.0(13) C2 C3 H3A . . 109.9 C4 C3 H3A . . 109.9 C2 C3 H3B . . 109.9 C4 C3 H3B . . 109.9 H3A C3 H3B . . 108.3 C5 C4 C3 . . 113.8(14) C5 C4 H4A . . 108.8 C3 C4 H4A . . 108.8 C5 C4 H4B . . 108.8 C3 C4 H4B . . 108.8 H4A C4 H4B . . 107.7 C4 C5 C6 . . 111.2(14) C4 C5 H5A . . 109.4 C6 C5 H5A . . 109.4 C4 C5 H5B . . 109.4 C6 C5 H5B . . 109.4 H5A C5 H5B . . 108 C5 C6 H6A . . 109.5 C5 C6 H6B . . 109.5 H6A C6 H6B . . 109.5 C5 C6 H6C . . 109.5 H6A C6 H6C . . 109.5 H6B C6 H6C . . 109.5 C1 N1 H1A . . 109.5 C1 N1 H1B . . 109.5 H1A N1 H1B . . 109.5 C1 N1 H1C . . 109.5 H1A N1 H1C . . 109.5 H1B N1 H1C . . 109.5 Pb1 I2 Pb1 4_477 . 155.65(5) I2 Pb1 I2 8_755 4_577 180 I2 Pb1 I2 8_755 5_777 91.695(9) I2 Pb1 I2 4_577 5_777 88.305(9) I2 Pb1 I2 8_755 . 88.305(9) I2 Pb1 I2 4_577 . 91.695(9) I2 Pb1 I2 5_777 . 180.0000(10) I2 Pb1 I1 8_755 5_777 91.50(4) I2 Pb1 I1 4_577 5_777 88.50(4) I2 Pb1 I1 5_777 5_777 93.64(4) I2 Pb1 I1 . 5_777 86.36(4) I2 Pb1 I1 8_755 . 88.50(4) I2 Pb1 I1 4_577 . 91.50(4) I2 Pb1 I1 5_777 . 86.36(4) I2 Pb1 I1 . . 93.64(4) I1 Pb1 I1 5_777 . 180.0000(10) 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_site_symmetry_1 _geom_torsion_site_symmetry_4 _geom_torsion N1 C1 C2 C3 . . -179(3) C1 C2 C3 C4 . . -177(3) C2 C3 C4 C5 . . 175(3) C3 C4 C5 C6 . . 180(4) Pb1 I2 Pb1 I2 4_477 8_755 171.92(11) Pb1 I2 Pb1 I2 4_477 4_577 -8.08(11) Pb1 I2 Pb1 I1 4_477 5_777 80.32(14) Pb1 I2 Pb1 I1 4_477 . -99.68(14) 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 N1 H1A I2 8_755 0.89 3.1 3.63(2) 121 N1 H1B I1 . 0.89 2.76 3.63(2) 166 N1 H1C I1 8_855 0.89 2.74 3.622(18) 169 _cod_database_code 2102943