#======================================================================= data_global #======================================================================= _audit_creation_method 'Jana2006 Version : 11/03/2012' # 1. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_paper_category ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full 'Journal of Materials Chemistry' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #======================================================================= # 2. SUBMISSION DETAILS _publ_contact_author_name 'Tom Baikie' _publ_contact_author_address ; Energy Research Institute @ NTU, Nanyang Technological University, Singapore. ; _publ_contact_author_email tbaikie@ntu.edu.sg _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_requested_journal 'Journal of Materials Chemistry' _publ_requested_category ? _publ_contact_letter ; ? ; #======================================================================= # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis and crystal chemistry of the hybrid perovskite (CH3NH3)PbI3 for solid state sensitised solar cell applications ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address 'Tom Baikie' ;Energy Research Institute @ NTU, Research Technoplaza, Nanyang Technological University, Nanyang Drive, 637553, Singapore ; 'Fang Yanan' ;Energy Research Institute @ NTU, Research Technoplaza, Nanyang Technological University, Nanyang Drive, 637553, Singapore ; 'Jeannette M Kadro' ;Energy Research Institute @ NTU, Research Technoplaza, Nanyang Technological University, Nanyang Drive, 637553, Singapore ; 'Martin K Schreyer' ;Institute of Chemical Science, 1 Pesek Road, Jurong Island, 627833, Singapore ; 'Fengxia Wei' ;School of Materials Science and Engineering, Nanyang Technological University,Nanyang Avenue, 639798, Singapore ; 'Subodh G Mhaisalkar' ;Energy Research Institute @ NTU, Research Technoplaza, Nanyang Technological University, Nanyang Drive, 637553, Singapore ; 'Michael Graetzel' ;Laboratory of Photonics and Interfaces, Institute of Chemical Sciences and Engineering, Swiss Federal Institute of Technology, Switzerland ; 'Tim J White' ;School of Materials Science and Engineering, Nanyang Technological University,Nanyang Avenue, 639798, Singapore ; #======================================================================= data_I #======================================================================= # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_sum 'C1 H0 I3 N1 Pb1' _chemical_formula_weight 613.9 _chemical_melting_point ? _chemical_compound_source ? _chemical_absolute_configuration . #======================================================================= # 6. CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' _symmetry_space_group_name_Hall '-P -2xabc;-2yb;-2zac' _symmetry_Int_Tables_number 62 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x+1/2,-y,z+1/2 3 -x,y+1/2,-z 4 x+1/2,-y+1/2,-z+1/2 5 -x,-y,-z 6 x+1/2,y,-z+1/2 7 x,-y+1/2,z 8 -x+1/2,y+1/2,z+1/2 _cell_length_a 8.8362(11) _cell_length_b 12.5804(15) _cell_length_c 8.5551(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 951.0101 loop_ _cell_formula_units_Z 4 _cell_measurement_reflns_used 1731 _cell_measurement_theta_min 2.88 _cell_measurement_theta_max 32.08 _cell_measurement_temperature 100 _cell_special_details ; ? ; _exptl_crystal_density_diffrn 4.2864 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 27.39 _exptl_crystal_description ? _exptl_crystal_size_max 1 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_size_rad ? _exptl_crystal_colour 'black' _exptl_absorpt_correction_type 'multi scan' _exptl_absorpt_process_details ? _exptl_absorpt_correction_T_min 0.00 _exptl_absorpt_correction_T_max 0.004 #======================================================================= # 7. EXPERIMENTAL DATA _exptl_special_details ? _diffrn_ambient_temperature 100 _diffrn_source ? _diffrn_source_power ? _diffrn_source_voltage ? _diffrn_source_current ? _diffrn_radiation_type ? _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_monochromator 'three cycle diffractomter' _diffrn_measurement_device ? _diffrn_measurement_device_type ? _diffrn_detector 'CCD' _diffrn_detector_area_resol_mean ? _diffrn_measurement_method ? _diffrn_measurement_specimen_support ? _diffrn_reflns_number 17319 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 32.08 _diffrn_reflns_theta_full 32.08 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0465 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? _diffrn_radiation_probe X-ray #======================================================================= # 8. REFINEMENT DATA _refine_special_details ; ? ; _reflns_number_total 1731 _reflns_number_gt 1344 _reflns_threshold_expression 'I>3\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_gt 0.1299 _refine_ls_R_factor_all 0.0657 _refine_ls_wR_factor_all 0.1322 _refine_ls_goodness_of_fit_all 2.22 _refine_ls_goodness_of_fit_gt 2.48 _refine_ls_restrained_S_gt ? _refine_ls_restrained_S_all ? _refine_ls_number_reflns 1731 _refine_ls_number_parameters 35 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.0004I^2^)' _refine_ls_hydrogen_treatment 'constr' _refine_ls_shift/su_max 0.0042 _refine_ls_shift/su_mean 0.0008 _refine_diff_density_max 7.82 _refine_diff_density_min -9.44 _refine_ls_extinction_method 'B-C type 1 Gaussian isotropic (Becker & Coppens, 1974)' _refine_ls_extinction_coef 570(70) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_abs_structure_Rogers ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' I -0.4742 1.8119 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' Pb -3.3944 10.1111 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement ? _computing_molecular_graphics ? _computing_publication_material ? #======================================================================= # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_adp_type _atom_site_U_iso_or_equiv _atom_site_symmetry_multiplicity _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5 0 0 Uani 0.00608(16) 4 1 d . . . I1 I 0.48572(11) 0.25 -0.05291(14) Uani 0.0130(3) 4 1 d . . . I2 I 0.19020(9) 0.01719(6) 0.18615(10) Uani 0.0168(2) 8 1 d . . . N N 0.932(2) 0.75 0.029(2) Uani 0.030(5) 4 1 d . . . C C 0.913(2) 0.25 0.061(2) Uani 0.019(5) 4 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_type_symbol _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 Pb1 Pb 0.0068(3) 0.0028(3) 0.0086(3) 0.00005(16) 0.00011(18) 0.00028(18) I1 I 0.0187(5) 0.0021(4) 0.0183(6) 0 0.0021(4) 0 I2 I 0.0157(4) 0.0206(4) 0.0143(4) 0.0013(3) 0.0092(3) 0.0009(3) N N 0.035(10) 0.023(9) 0.033(10) 0 0.020(8) 0 C C 0.019(8) 0.011(8) 0.027(10) 0 -0.002(8) 0 #======================================================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Pb1 I1 . . 3.18001(18) ? Pb1 I1 . 3_645 3.18001(18) ? Pb1 I2 . . 3.1744(8) ? Pb1 I2 . 2_554 3.1750(8) ? Pb1 I2 . 5_655 3.1744(8) ? Pb1 I2 . 6_555 3.1750(8) ? N C . 3_755 1.57(3) ? 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_2 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag I1 Pb1 I1 . . 3_645 180.0(5) ? I1 Pb1 I2 . . . 88.27(2) ? I1 Pb1 I2 . . 2_554 85.75(3) ? I1 Pb1 I2 . . 5_655 91.73(2) ? I1 Pb1 I2 . . 6_555 94.25(3) ? I1 Pb1 I2 3_645 . . 91.73(2) ? I1 Pb1 I2 3_645 . 2_554 94.25(3) ? I1 Pb1 I2 3_645 . 5_655 88.27(2) ? I1 Pb1 I2 3_645 . 6_555 85.75(3) ? I2 Pb1 I2 . . 2_554 88.42(2) ? I2 Pb1 I2 . . 5_655 180.0(5) ? I2 Pb1 I2 . . 6_555 91.58(2) ? I2 Pb1 I2 2_554 . 5_655 91.58(2) ? I2 Pb1 I2 2_554 . 6_555 180.0(5) ? I2 Pb1 I2 5_655 . 6_555 88.42(2) ? Pb1 I1 Pb1 . . 3_655 163.00(4) ? Pb1 I2 Pb1 . . 2_555 151.18(3) ? #=======================================================================