#------------------------------------------------------------------------------ #$Date: 2016-03-23 21:54:53 +0200 (Wed, 23 Mar 2016) $ #$Revision: 179459 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/33/56/4335641.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_4335641 loop_ _publ_author_name 'Constantinos C. Stoumpos' 'Christos D. Malliakas' 'Mercouri G. Kanatzidis' _publ_contact_author_address ; Department of Chemistry 2145 Sheridan Road Northwestern University Evanston, IL 60208-3113 USA ; _publ_contact_author_email m-kanatzidis@northwestern.edu _publ_contact_author_fax 847-491-5937 _publ_contact_author_name 'Mercouri G. Kanatzidis' _publ_contact_author_phone 847-467-1541 _publ_section_title ; Semiconducting Tin and Lead Iodide Perovskites with Organic Cations: Phase Transitions, High Mobilities, and Near-Infrared Photoluminescent Properties ; _journal_name_full 'Inorganic Chemistry' _journal_page_first 9019 _journal_page_last 9038 _journal_paper_doi 10.1021/ic401215x _journal_volume 52 _journal_year 2013 _chemical_formula_moiety CH3NH3Sn0.43Pb0.57I3 _chemical_formula_sum 'C H3 I3 N Pb0.57 Sn0.43' _chemical_formula_weight 575.78 _chemical_name_common beta-Methylammonium_Tin_Lead_Iodide _chemical_name_systematic ; ? ; _space_group_IT_number 108 _symmetry_cell_setting tetragonal _symmetry_space_group_name_Hall 'I 4 -2c' _symmetry_space_group_name_H-M 'I 4 c m' _atom_sites_solution_hydrogens none _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.8552(6) _cell_length_b 8.8552(6) _cell_length_c 12.5353(12) _cell_measurement_reflns_used 3302 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.15 _cell_measurement_theta_min 2.82 _cell_volume 982.95(13) _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector_type STOE _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 4728 _diffrn_reflns_theta_full 29.01 _diffrn_reflns_theta_max 29.01 _diffrn_reflns_theta_min 2.82 _diffrn_source 'sealed x-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_current 30 _diffrn_source_power 1.20 _diffrn_source_voltage 40 _exptl_absorpt_coefficient_mu 20.260 _exptl_absorpt_correction_T_max 0.0869 _exptl_absorpt_correction_T_min 0.0296 _exptl_absorpt_correction_type integration _exptl_crystal_colour black _exptl_crystal_density_diffrn 3.930 _exptl_crystal_description 'rhombic dodecahedron' _exptl_crystal_F_000 964 _exptl_crystal_size_max 0.191 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.109 _refine_diff_density_max 2.980 _refine_diff_density_min -2.175 _refine_diff_density_rms 0.365 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_extinction_coef 0.00084(10) _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 1.162 _refine_ls_hydrogen_treatment none _refine_ls_matrix_type full _refine_ls_number_parameters 22 _refine_ls_number_reflns 788 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.160 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0678 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1089P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1732 _refine_ls_wR_factor_ref 0.1809 _reflns_number_gt 633 _reflns_number_total 788 _reflns_threshold_expression >2sigma(I) _cod_data_source_file ic401215x_si_004_3.cif _cod_data_source_block 5b_293K _cod_database_code 4335641 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x, -y, z+1/2' '-x, y, z+1/2' '-y, -x, z+1/2' 'y, x, z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, z+1' '-x+1/2, y+1/2, z+1' '-y+1/2, -x+1/2, z+1' 'y+1/2, x+1/2, z+1' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags Pb Pb 0.0000 0.0000 0.0002 0.0419(3) Uani 0.569(7) 4 d SP Sn Sn 0.0000 0.0000 0.0002 0.0419(3) Uani 0.431(7) 4 d SP I1 I 0.2269(2) 0.7269(2) -0.0007(5) 0.1017(7) Uani 1 2 d S I2 I 0.0000 0.0000 0.2548(4) 0.131(2) Uani 1 4 d S C C 0.5000 0.0000 0.2227(19) 0.051(12) Uiso 1 4 d SD N N 0.5000 0.0000 0.332(3) 0.28(10) Uiso 1 4 d SD loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.0380(4) 0.0380(4) 0.0496(8) 0.000 0.000 0.000 Sn 0.0380(4) 0.0380(4) 0.0496(8) 0.000 0.000 0.000 I1 0.0838(7) 0.0838(7) 0.1374(16) -0.0412(12) -0.0412(12) 0.0477(10) I2 0.179(3) 0.179(3) 0.0363(15) 0.000 0.000 0.000 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' Sn Sn -0.6537 1.4246 '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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 I2 Pb I1 89.79(11) 5_554 4_455 I2 Pb I1 89.79(11) 5_554 3_655 I1 Pb I1 179.6(2) 4_455 3_655 I2 Pb I1 89.79(11) 5_554 1_545 I1 Pb I1 89.999(1) 4_455 1_545 I1 Pb I1 89.999(1) 3_655 1_545 I2 Pb I1 89.79(11) 5_554 2_565 I1 Pb I1 89.999(1) 4_455 2_565 I1 Pb I1 89.999(1) 3_655 2_565 I1 Pb I1 179.6(2) 1_545 2_565 I2 Pb I2 180.0 5_554 . I1 Pb I2 90.21(11) 4_455 . I1 Pb I2 90.21(11) 3_655 . I1 Pb I2 90.21(11) 1_545 . I1 Pb I2 90.21(11) 2_565 . Sn I1 Pb 0.0 13_554 13_554 Sn I1 Pb 169.44(9) 13_554 1_565 Pb I1 Pb 169.44(9) 13_554 1_565 Sn I1 Sn 169.44(9) 13_554 1_565 Pb I1 Sn 169.44(9) 13_554 1_565 Pb I1 Sn 0.0 1_565 1_565 Sn I2 Pb 0.0 5 5 Sn I2 Pb 180.0 5 . Pb I2 Pb 180.0 5 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pb I2 3.076(6) 5_554 Pb I1 3.1441(3) 4_455 Pb I1 3.1441(3) 3_655 Pb I1 3.1441(3) 1_545 Pb I1 3.1441(3) 2_565 Pb I2 3.192(6) . I1 Sn 3.1441(3) 13_554 I1 Pb 3.1441(3) 13_554 I1 Pb 3.1441(3) 1_565 I1 Sn 3.1441(3) 1_565 I2 Sn 3.076(6) 5 I2 Pb 3.076(6) 5 C N 1.37(4) .