#------------------------------------------------------------------------------
#$Date: 2019-11-24 21:47:49 +0200 (Sun, 24 Nov 2019) $
#$Revision: 239511 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/67/4516752.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_4516752
loop_
_publ_author_name
'Jaffe, Adam'
'Lin, Yu'
'Beavers, Christine M.'
'Voss, Johannes'
'Mao, Wendy L.'
'Karunadasa, Hemamala I.'
_publ_section_title
;
 High-Pressure Single-Crystal Structures of 3D Lead-Halide Hybrid
 Perovskites and Pressure Effects on their Electronic and Optical
 Properties.
;
_journal_issue                   4
_journal_name_full               'ACS central science'
_journal_page_first              201
_journal_page_last               209
_journal_paper_doi               10.1021/acscentsci.6b00055
_journal_volume                  2
_journal_year                    2016
_chemical_formula_sum            'C H6 I3 N Pb'
_chemical_formula_weight         619.96
_space_group_crystal_system      orthorhombic
_space_group_IT_number           69
_space_group_name_Hall           '-F 2 2'
_space_group_name_H-M_alt        'F m m m'
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.4984(7)
_cell_length_b                   12.5181(7)
_cell_length_c                   12.6012(8)
_cell_measurement_reflns_used    3332
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      33.4
_cell_measurement_theta_min      3.15
_cell_volume                     1971.5(2)
_computing_cell_refinement       'SAINT V8.34A(Bruker, 2013)'
_computing_data_collection       'Apex2 v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
     	SHELXTL 5.1, XP (Sheldrick, 1994)
	ShelXle Rev 699 (Hubschle, 2011)
;
_computing_publication_material  SHELXL-2014/7
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2012)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6888
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0322
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7622
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.411
_diffrn_reflns_theta_max         35.039
_diffrn_reflns_theta_min         2.727
_diffrn_source
;
Advanced Light Source, station 11.3.1
;
_exptl_absorpt_coefficient_mu    26.187
_exptl_absorpt_correction_T_max  0.4371
_exptl_absorpt_correction_T_min  0.2919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/5 (Sheldrick, 2015)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.177
_exptl_crystal_description       'rhombic dodecahedron'
_exptl_crystal_F_000             2080
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         3.255
_refine_diff_density_min         -5.657
_refine_diff_density_rms         0.498
_refine_ls_extinction_coef       0.00025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         1326
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0555
_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/[σ²(Fo²)+(0.0724P)²+241.6893P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1831
_refine_ls_wR_factor_ref         0.1948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                962
_reflns_number_total             1326
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            oc6b00055_si_003.cif
_cod_data_source_block           MAPbI3_RT
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4516752
_shelx_shelxl_version_number     2014/7
_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_min   0.354
_shelx_estimated_absorpt_t_max   0.354
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
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 0.2500 0.2500 0.5000 0.0324(3) Uani 1 4 d S T P
I1 I 0.2241(5) 0.5000 0.5000 0.0860(17) Uani 1 4 d S T P
I2A I 0.5000 0.2981(6) 0.5000 0.0530(10) Uani 0.75 4 d S T P
I2B I 0.5000 0.267(2) 0.462(2) 0.0530(10) Uani 0.125 2 d S T P
I3A I 0.2500 0.2500 0.2500 0.0672(19) Uani 0.75 4 d S T P
I3B I 0.294(3) 0.2500 0.2500 0.0672(19) Uani 0.125 2 d S T P
C1 C 0.5000 0.44269(8) 0.216(5) 0.15(3) Uiso 0.5 2 d S . P
N1 N 0.5000 0.44269(8) 0.216(5) 0.15(3) Uiso 0.5 2 d DS . P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'ShelXle using methods of  L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
H H 0.0000 0.0000
'ShelXle using methods of  L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
N N 0.0066 0.0034
'ShelXle using methods of  L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
I I -0.4371 1.8409
'ShelXle using methods of  L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
Pb Pb -3.4194 10.2008
'ShelXle using methods of  L.Kissel & R.H.Pratt Acta Cryst A46 170 1990'
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
I1 Pb1 I1 180.0 29_556 .
I1 Pb1 I3A 90.0 29_556 29_556
I1 Pb1 I3A 90.0 . 29_556
I1 Pb1 I3A 90.0 29_556 .
I1 Pb1 I3A 90.0 . .
I3A Pb1 I3A 180.0 29_556 .
I1 Pb1 I2B 88.1(5) 29_556 18_556
I1 Pb1 I2B 91.9(5) . 18_556
I3A Pb1 I2B 81.3(5) 29_556 18_556
I3A Pb1 I2B 98.7(5) . 18_556
I1 Pb1 I2B 91.9(5) 29_556 14
I1 Pb1 I2B 88.1(5) . 14
I3A Pb1 I2B 98.7(5) 29_556 14
I3A Pb1 I2B 81.3(5) . 14
I2B Pb1 I2B 180.0 18_556 14
I1 Pb1 I2B 91.9(5) 29_556 29_556
I1 Pb1 I2B 88.1(5) . 29_556
I3A Pb1 I2B 81.3(5) 29_556 29_556
I3A Pb1 I2B 98.7(5) . 29_556
I2B Pb1 I2B 162.6(9) 18_556 29_556
I2B Pb1 I2B 17.4(9) 14 29_556
I1 Pb1 I2B 88.1(5) 29_556 .
I1 Pb1 I2B 91.9(5) . .
I3A Pb1 I2B 98.7(5) 29_556 .
I3A Pb1 I2B 81.3(5) . .
I2B Pb1 I2B 17.4(9) 18_556 .
I2B Pb1 I2B 162.6(9) 14 .
I2B Pb1 I2B 180.0(9) 29_556 .
I1 Pb1 I2A 85.0(2) 29_556 29_556
I1 Pb1 I2A 95.0(2) . 29_556
I3A Pb1 I2A 90.0 29_556 29_556
I3A Pb1 I2A 90.0 . 29_556
I2B Pb1 I2A 168.9(4) 18_556 29_556
I2B Pb1 I2A 11.1(4) 14 29_556
I2B Pb1 I2A 11.1(4) 29_556 29_556
I2B Pb1 I2A 168.9(4) . 29_556
I1 Pb1 I2A 95.0(2) 29_556 .
I1 Pb1 I2A 85.0(2) . .
I3A Pb1 I2A 90.0 29_556 .
I3A Pb1 I2A 90.0 . .
I2B Pb1 I2A 11.1(4) 18_556 .
I2B Pb1 I2A 168.9(4) 14 .
I2B Pb1 I2A 168.9(4) 29_556 .
I2B Pb1 I2A 11.1(4) . .
I2A Pb1 I2A 180.0 29_556 .
I1 Pb1 I3B 88.98(7) 29_556 .
I1 Pb1 I3B 91.02(7) . .
I3A Pb1 I3B 170.0(6) 29_556 .
I3A Pb1 I3B 10.0(6) . .
I2B Pb1 I3B 88.8(8) 18_556 .
I2B Pb1 I3B 91.2(8) 14 .
I2B Pb1 I3B 108.7(8) 29_556 .
I2B Pb1 I3B 71.3(8) . .
I2A Pb1 I3B 99.8(6) 29_556 .
I2A Pb1 I3B 80.2(6) . .
I1 Pb1 I3B 88.98(7) 29_556 18_556
I1 Pb1 I3B 91.02(7) . 18_556
I3A Pb1 I3B 10.0(6) 29_556 18_556
I3A Pb1 I3B 170.0(6) . 18_556
I2B Pb1 I3B 71.3(8) 18_556 18_556
I2B Pb1 I3B 108.7(8) 14 18_556
I2B Pb1 I3B 91.2(8) 29_556 18_556
I2B Pb1 I3B 88.8(8) . 18_556
I2A Pb1 I3B 99.8(6) 29_556 18_556
I2A Pb1 I3B 80.2(6) . 18_556
I3B Pb1 I3B 160.0(12) . 18_556
Pb1 I1 Pb1 168.2(2) 15_556 .
I2B I2A I2B 103(6) 18_556 .
I2B I2A Pb1 83.2(5) 18_556 .
I2B I2A Pb1 83.2(5) . .
I2B I2A Pb1 83.2(5) 18_556 3_656
I2B I2A Pb1 83.2(5) . 3_656
Pb1 I2A Pb1 158.2(2) . 3_656
I2A I2B I2B 39(3) . 18_556
I2A I2B Pb1 85.7(6) . 3_656
I2B I2B Pb1 81.3(5) 18_556 3_656
I2A I2B Pb1 85.7(6) . .
I2B I2B Pb1 81.3(5) 18_556 .
Pb1 I2B Pb1 160.8(10) 3_656 .
I3B I3A I3B 180.0 . 14
I3B I3A Pb1 90.000(1) . .
I3B I3A Pb1 90.000(1) 14 .
I3B I3A Pb1 90.0 . 11
I3B I3A Pb1 90.000(1) 14 11
Pb1 I3A Pb1 180.0 . 11
I3A I3B I3B 0.000(1) . 14
I3A I3B Pb1 80.0(6) . 11
I3B I3B Pb1 80.0(6) 14 11
I3A I3B Pb1 80.0(6) . .
I3B I3B Pb1 80.0(6) 14 .
Pb1 I3B Pb1 160.0(12) 11 .
N1 C1 C1 0.0 2_665 19_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I1 3.1462(7) 29_556
Pb1 I1 3.1462(7) .
Pb1 I3A 3.1503(2) 29_556
Pb1 I3A 3.1503(2) .
Pb1 I2B 3.169(5) 18_556
Pb1 I2B 3.169(5) 14
Pb1 I2B 3.169(5) 29_556
Pb1 I2B 3.169(5) .
Pb1 I2A 3.1820(14) 29_556
Pb1 I2A 3.1820(14) .
Pb1 I3B 3.199(6) .
Pb1 I3B 3.199(6) 18_556
I1 Pb1 3.1462(7) 15_556
I2A I2B 0.61(2) 18_556
I2A I2B 0.61(2) .
I2A Pb1 3.1820(13) 3_656
I2B I2B 0.96(5) 18_556
I2B Pb1 3.169(5) 3_656
I3A I3B 0.55(3) .
I3A I3B 0.55(3) 14
I3A Pb1 3.1503(2) 11
I3B I3B 1.11(7) 14
I3B Pb1 3.199(6) 11
C1 N1 1.435(2) 2_665
C1 C1 1.435(2) 19_565
