#------------------------------------------------------------------------------ #$Date: 2018-11-10 01:21:05 +0200 (Sat, 10 Nov 2018) $ #$Revision: 211871 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/02/1550206.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_1550206 loop_ _publ_author_name 'Li, Tianyang' 'Dunlap-Shohl, Wiley' 'Reinheimer, Eric W.' 'LeMagueres, Pierre' 'Mitzi, David B.' _publ_section_title ; Melting Temperature Suppression of Layered Hybrid Lead Halide Perovskites via Organic Ammonium Cation Branching ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/C8SC03863E _journal_year 2019 _chemical_formula_moiety '0.5(I8 Pb2), 2(C5 H14 N)' _chemical_formula_sum 'C10 H28 I4 N2 Pb' _chemical_formula_weight 891.13 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _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 _audit_creation_date 2018-08-20 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2018-08-24 deposited with the CCDC. 2018-11-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 106.155(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 15.0424(8) _cell_length_b 9.2398(4) _cell_length_c 8.5756(5) _cell_measurement_reflns_used 6061 _cell_measurement_temperature 273 _cell_measurement_theta_max 26.28 _cell_measurement_theta_min 3.31 _cell_volume 1144.85(10) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 273.15 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_unetI/netI 0.0174 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_number 12771 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.430 _diffrn_reflns_theta_min 3.580 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 12.751 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'clear orange' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary orange _exptl_crystal_density_diffrn 2.585 _exptl_crystal_description plate _exptl_crystal_F_000 792 _exptl_crystal_size_max 0.101 _exptl_crystal_size_mid 0.089 _exptl_crystal_size_min 0.084 _exptl_transmission_factor_max 0.7454 _exptl_transmission_factor_min 0.6472 _refine_diff_density_max 0.811 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.152 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.270 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 82 _refine_ls_number_reflns 2354 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.270 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0314 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+11.5917P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.0724 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2125 _reflns_number_total 2354 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL 1Meba_5_P21c in P21/c #14 1meba_5_p21c.res created by SHELXL-2016/6 at 15:35:03 on 02-Jul-2018 REM reset to P21/c #14 CELL 0.71073 15.0424 9.2398 8.5756 90 106.1553 90 ZERR 2 0.0008 0.0004 0.0005 0 0.0025 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N Pb UNIT 20 56 8 4 2 L.S. 10 0 0 PLAN 5 SIZE 0.084 0.089 0.101 TEMP 0 fmap 2 53 acta OMIT 1 0 0 OMIT 2 0 0 OMIT 1 1 0 REM REM REM WGHT 0.000100 11.591701 FVAR 0.06989 PB1 5 0.500000 -0.500000 0.000000 10.50000 0.04627 0.03393 = 0.03554 0.00009 0.01236 -0.00166 I2 3 0.496138 -0.194571 0.187657 11.00000 0.06063 0.04235 = 0.04139 -0.01169 0.01637 0.00369 I3 3 0.719922 -0.471296 0.115444 11.00000 0.05131 0.05514 = 0.06349 0.00214 0.01689 0.00390 N1 4 0.686093 -0.089870 0.011209 11.00000 0.07878 0.05293 = 0.06630 0.00666 0.02547 0.01369 AFIX 137 H1A 2 0.700127 -0.058256 -0.077081 11.00000 -1.20000 H1B 2 0.631241 -0.054784 0.012741 11.00000 -1.20000 H1C 2 0.683913 -0.186132 0.009835 11.00000 -1.20000 AFIX 0 C2 1 0.754202 -0.043043 0.150812 11.00000 0.07851 0.05718 = 0.06915 0.00834 0.01016 0.01693 AFIX 13 H2 2 0.744951 -0.091209 0.246911 11.00000 -1.20000 AFIX 0 C3 1 0.849688 -0.084050 0.131251 11.00000 0.06503 0.10733 = 0.12290 0.00136 0.00394 -0.00936 AFIX 23 H3A 2 0.845625 -0.181027 0.086493 11.00000 -1.20000 H3B 2 0.863611 -0.019029 0.052397 11.00000 -1.20000 AFIX 0 C4 1 0.747028 0.122447 0.168903 11.00000 0.16662 0.04484 = 0.14075 -0.03043 0.01525 -0.01844 AFIX 137 H4A 2 0.759979 0.169717 0.077953 11.00000 -1.50000 H4B 2 0.790986 0.153414 0.267386 11.00000 -1.50000 H4C 2 0.685657 0.147122 0.172620 11.00000 -1.50000 AFIX 0 C5 1 0.926012 -0.080149 0.276509 11.00000 0.10011 0.16616 = 0.29291 0.02919 -0.00987 0.01959 AFIX 23 H5A 2 0.907702 -0.132621 0.360557 11.00000 -1.20000 H5B 2 0.935768 0.019841 0.311561 11.00000 -1.20000 AFIX 0 C6 1 1.014239 -0.138347 0.267384 11.00000 0.08119 0.26195 = 0.41717 -0.09006 0.02127 0.00496 AFIX 137 H6A 2 1.056317 -0.142832 0.374421 11.00000 -1.50000 H6B 2 1.039531 -0.076828 0.200214 11.00000 -1.50000 H6C 2 1.005116 -0.233804 0.221491 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1Meba_5_P21c in P21/c #14 REM R1 = 0.0314 for 2125 Fo > 4sig(Fo) and 0.0360 for all 2354 data REM 82 parameters refined using 0 restraints END WGHT 0.0000 11.5916 REM Highest difference peak 0.811, deepest hole -0.983, 1-sigma level 0.152 Q1 1 0.7187 -0.5602 0.0468 11.00000 0.05 0.81 Q2 1 0.7313 -0.5615 0.1814 11.00000 0.05 0.80 Q3 1 0.4927 -0.1847 0.3936 11.00000 0.05 0.65 Q4 1 0.5623 -0.5002 -0.0176 11.00000 0.05 0.64 Q5 1 0.4991 -0.2128 0.0856 11.00000 0.05 0.63 REM The information below was added by Olex2. REM REM R1 = 0.0314 for 2125 Fo > 4sig(Fo) and 0.0360 for all 13347 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.81, deepest hole -0.98 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0360 REM R1_gt = 0.0314 REM wR_ref = 0.0724 REM GOOF = 1.270 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 13347 REM Reflections_gt = 2125 REM Parameters = n/a REM Hole = -0.98 REM Peak = 0.81 REM Flack = n/a ; _cod_data_source_file c8sc03863e2.cif _cod_data_source_block 1meba_5_p21c _cod_original_cell_volume 1144.84(10) _cod_database_code 1550206 _shelx_shelxl_version_number 2016/6 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.414 _shelx_estimated_absorpt_t_min 0.359 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C2(H2) 2.b Secondary CH2 refined with riding coordinates: C3(H3a,H3b), C5(H5a,H5b) 2.c Idealised Me refined as rotating group: N1(H1a,H1b,H1c), C4(H4a,H4b,H4c), C6(H6a,H6b,H6c) ; _olex2_date_sample_data_collection 2018-06-08 _olex2_date_sample_submission 2018-06-08 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Pb1 Pb 0.500000 -0.500000 0.000000 0.03838(13) Uani 1 2 d S T P I2 I 0.49614(4) -0.19457(7) 0.18766(7) 0.04769(17) Uani 1 1 d . . . I3 I 0.71992(5) -0.47130(8) 0.11544(8) 0.05646(19) Uani 1 1 d . . . N1 N 0.6861(6) -0.0899(10) 0.0112(11) 0.065(2) Uani 1 1 d . . . H1A H 0.700127 -0.058256 -0.077081 0.078 Uiso 1 1 calc GR . . H1B H 0.631241 -0.054784 0.012741 0.078 Uiso 1 1 calc GR . . H1C H 0.683913 -0.186132 0.009835 0.078 Uiso 1 1 calc GR . . C2 C 0.7542(8) -0.0430(13) 0.1508(15) 0.070(3) Uani 1 1 d . . . H2 H 0.744951 -0.091209 0.246911 0.084 Uiso 1 1 calc R . . C3 C 0.8497(9) -0.0841(19) 0.131(2) 0.103(5) Uani 1 1 d . . . H3A H 0.845625 -0.181027 0.086493 0.123 Uiso 1 1 calc R . . H3B H 0.863611 -0.019029 0.052397 0.123 Uiso 1 1 calc R . . C4 C 0.7470(12) 0.1224(14) 0.169(2) 0.123(6) Uani 1 1 d . . . H4A H 0.759979 0.169717 0.077953 0.184 Uiso 1 1 calc GR . . H4B H 0.790986 0.153414 0.267386 0.184 Uiso 1 1 calc GR . . H4C H 0.685657 0.147122 0.172620 0.184 Uiso 1 1 calc GR . . C5 C 0.9260(14) -0.080(3) 0.277(3) 0.199(12) Uani 1 1 d . . . H5A H 0.907702 -0.132621 0.360557 0.239 Uiso 1 1 calc R . . H5B H 0.935768 0.019841 0.311561 0.239 Uiso 1 1 calc R . . C6 C 1.0142(15) -0.138(3) 0.267(4) 0.263(18) Uani 1 1 d . . . H6A H 1.056317 -0.142832 0.374421 0.395 Uiso 1 1 calc GR . . H6B H 1.039531 -0.076828 0.200214 0.395 Uiso 1 1 calc GR . . H6C H 1.005116 -0.233804 0.221491 0.395 Uiso 1 1 calc GR . . 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 Pb1 0.0463(3) 0.0339(2) 0.0355(2) 0.00009(19) 0.01236(19) -0.0017(2) I2 0.0606(4) 0.0424(4) 0.0414(3) -0.0117(3) 0.0164(3) 0.0037(3) I3 0.0513(4) 0.0551(4) 0.0635(4) 0.0021(3) 0.0169(3) 0.0039(3) N1 0.079(6) 0.053(5) 0.066(6) 0.007(5) 0.025(5) 0.014(5) C2 0.079(8) 0.057(7) 0.069(7) 0.008(6) 0.010(6) 0.017(6) C3 0.065(8) 0.107(12) 0.123(13) 0.001(10) 0.004(8) -0.009(8) C4 0.167(17) 0.045(8) 0.141(15) -0.030(9) 0.015(12) -0.018(9) C5 0.100(15) 0.17(2) 0.29(3) 0.03(2) -0.010(19) 0.020(15) C6 0.081(15) 0.26(4) 0.42(5) -0.09(3) 0.02(2) 0.005(19) 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' I I -0.4742 1.8119 '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' 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 Pb1 I2 180.00(2) 4 2_645 I2 Pb1 I2 180.0 3_645 . I2 Pb1 I2 85.895(6) 4 . I2 Pb1 I2 85.895(6) 2_645 3_645 I2 Pb1 I2 94.105(6) 4 3_645 I2 Pb1 I2 94.105(6) 2_645 . I3 Pb1 I2 93.777(17) 3_645 . I3 Pb1 I2 86.223(17) 3_645 3_645 I3 Pb1 I2 90.639(17) . 2_645 I3 Pb1 I2 89.361(17) . 4 I3 Pb1 I2 93.776(17) . 3_645 I3 Pb1 I2 86.224(17) . . I3 Pb1 I2 89.361(17) 3_645 2_645 I3 Pb1 I2 90.639(17) 3_645 4 I3 Pb1 I3 180.0 3_645 . Pb1 I2 Pb1 153.90(2) 2_655 . N1 C2 C3 108.2(10) . . N1 C2 C4 109.6(10) . . C3 C2 C4 110.4(13) . . C5 C3 C2 116.3(17) . . C3 C5 C6 118(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pb1 I2 3.2130(6) 4 Pb1 I2 3.2572(6) . Pb1 I2 3.2572(6) 3_645 Pb1 I2 3.2130(6) 2_645 Pb1 I3 3.1893(7) 3_645 Pb1 I3 3.1893(7) . N1 C2 1.410(14) . C2 C3 1.539(17) . C2 C4 1.544(17) . C3 C5 1.44(2) . C5 C6 1.45(3) .