#------------------------------------------------------------------------------
#$Date: 2019-10-29 23:48:20 +0200 (Tue, 29 Oct 2019) $
#$Revision: 220495 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/30/4003081.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_4003081
loop_
_publ_author_name
'Febriansyah, Benny'
'Koh, Teck Ming'
'Lekina, Yulia'
'Jamaludin, Nur Fadilah'
'Bruno, Annalisa'
'Ganguly, Rakesh'
'Shen, Ze Xiang'
'Mhaisalkar, Subodh G.'
'England, Jason'
_publ_section_title
;
 Improved Photovoltaic Efficiency and Amplified Photocurrent Generation in
 Mesoporous n = 1 Two-Dimensional Lead--Iodide Perovskite Solar Cells
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              890
_journal_paper_doi               10.1021/acs.chemmater.8b04064
_journal_volume                  31
_journal_year                    2019
_chemical_formula_sum            'C10 H24 I10 N6 O2 Pb3'
_chemical_formula_weight         2150.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_update_record
;
2018-05-07 deposited with the CCDC.
2018-08-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.7582(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.6609(6)
_cell_length_b                   8.9123(3)
_cell_length_c                   22.7613(6)
_cell_measurement_reflns_used    9787
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      40.7198
_cell_measurement_theta_min      2.1889
_cell_volume                     3774.7(2)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'APEX3 (Bruker AXS Inc., 2017)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_publication_material  'APEX3 (Bruker AXS Inc., 2017)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'XT, VERSION 2014/5'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Photon II CPADs detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Multilayer Mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            58051
_diffrn_reflns_theta_full        32.00
_diffrn_reflns_theta_max         32.00
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'Incoatec microfocus source'
_diffrn_source_type              'Bruker D8 Quest'
_exptl_absorpt_coefficient_mu    21.545
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.26
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.785
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3672
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         2.007
_refine_diff_density_min         -1.157
_refine_ls_extinction_coef       0.000254(6)
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         6551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0050P)²+13.2962P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0422
_refine_ls_wR_factor_ref         0.0437
_reflns_number_gt                6012
_reflns_number_total             6551
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cm8b04064_si_002.cif
_cod_data_source_block           (PyrzEA)[Pb2I6]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-Scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4003081
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
C C1 0.3241(2) 0.6453(4) 0.69455(19) 0.0150(7) Uani d . . . 1
H H1 0.362051 0.57632 0.716596 0.018 Uiso calc U . R 1
C C2 0.3315(2) 0.7859(5) 0.6723(2) 0.0177(8) Uani d . . . 1
H H2 0.37454 0.831567 0.675843 0.021 Uiso calc U . R 1
C C3 0.2631(2) 0.8460(4) 0.64404(19) 0.0160(8) Uani d . . . 1
H H3 0.250613 0.94232 0.624477 0.019 Uiso calc U . R 1
C C4 0.1391(2) 0.7538(4) 0.62391(19) 0.0147(7) Uani d . . . 1
H H4A 0.124836 0.860414 0.621825 0.018 Uiso calc U . R 1
H H4B 0.12487 0.702317 0.655011 0.018 Uiso calc U . R 1
C C5 0.0987(2) 0.6841(4) 0.55707(19) 0.0150(7) Uani d . . . 1
H H5A 0.118186 0.582617 0.557165 0.018 Uiso calc U . R 1
H H5B 0.047484 0.673068 0.547856 0.018 Uiso calc U . R 1
I I1 0.48307(2) -0.01054(3) 0.63099(2) 0.01159(5) Uani d . . . 1
I I2 0.48509(2) 0.48499(3) 0.65051(2) 0.01246(5) Uani d . . . 1
I I3 0.40526(2) 0.32943(3) 0.45181(2) 0.01278(5) Uani d . . . 1
I I4 0.25261(2) -0.01508(3) 0.48455(2) 0.01089(5) Uani d . . . 1
I I5 0.33049(2) 0.22242(3) 0.69365(2) 0.01097(5) Uani d . . . 1
N N1 0.25434(18) 0.6224(3) 0.67978(16) 0.0130(6) Uani d . . . 1
N N2 0.21715(18) 0.7457(3) 0.64873(16) 0.0119(6) Uani d . . . 1
N N3 0.10374(18) 0.7752(3) 0.50398(15) 0.0122(6) Uani d . . . 1
H H3A 0.09013 0.87128 0.506223 0.018 Uiso calc U . R 1
H H3B 0.074302 0.735206 0.464537 0.018 Uiso calc U . R 1
H H3C 0.149865 0.774336 0.50889 0.018 Uiso calc U . R 1
O O1 0.17507(16) 0.3988(3) 0.69136(15) 0.0183(6) Uani d . . . 1
H H1O 0.137032 0.417716 0.694546 0.027 Uiso d U . R 1
H H2O 0.177231 0.331365 0.665937 0.027 Uiso d U . R 1
Pb Pb1 0.36379(2) 0.25293(2) 0.56520(2) 0.00968(3) Uani d . . . 1
Pb Pb2 0.5 0.22921(2) 0.75 0.00955(4) Uani d T P S 1
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'
Pb Pb -3.3944 10.1111 '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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 C2 . . 108.8(4)
N1 C1 H1 . . 125.6
C2 C1 H1 . . 125.6
C3 C2 C1 . . 105.6(4)
C3 C2 H2 . . 127.2
C1 C2 H2 . . 127.2
N2 C3 C2 . . 108.7(3)
N2 C3 H3 . . 125.6
C2 C3 H3 . . 125.6
N2 C4 C5 . . 113.8(3)
N2 C4 H4A . . 108.8
C5 C4 H4A . . 108.8
N2 C4 H4B . . 108.8
C5 C4 H4B . . 108.8
H4A C4 H4B . . 107.7
N3 C5 C4 . . 112.8(3)
N3 C5 H5A . . 109.0
C4 C5 H5A . . 109.0
N3 C5 H5B . . 109.0
C4 C5 H5B . . 109.0
H5A C5 H5B . . 107.8
Pb1 I1 Pb2 . . 72.790(6)
Pb2 I2 Pb1 . . 76.808(6)
Pb1 I4 Pb1 7_556 . 84.344(7)
Pb2 I5 Pb1 . . 74.740(6)
C1 N1 N2 . . 108.1(3)
C3 N2 N1 . . 108.8(3)
C3 N2 C4 . . 129.6(3)
N1 N2 C4 . . 121.6(3)
C5 N3 H3A . . 109.5
C5 N3 H3B . . 109.5
H3A N3 H3B . . 109.5
C5 N3 H3C . . 109.5
H3A N3 H3C . . 109.5
H3B N3 H3C . . 109.5
H1O O1 H2O . . 122.1
I3 Pb1 I2 . . 86.342(7)
I3 Pb1 I4 . 7_556 88.969(7)
I2 Pb1 I4 . 7_556 90.742(7)
I3 Pb1 I1 . . 96.463(7)
I2 Pb1 I1 . . 87.137(8)
I4 Pb1 I1 7_556 . 174.027(7)
I3 Pb1 I4 . . 94.216(7)
I2 Pb1 I4 . . 173.586(8)
I4 Pb1 I4 7_556 . 95.655(7)
I1 Pb1 I4 . . 86.451(7)
I3 Pb1 I5 . . 171.311(8)
I2 Pb1 I5 . . 85.689(7)
I4 Pb1 I5 7_556 . 87.678(7)
I1 Pb1 I5 . . 86.595(7)
I4 Pb1 I5 . . 94.089(7)
I2 Pb2 I2 2_656 . 86.612(10)
I2 Pb2 I5 2_656 . 92.909(7)
I2 Pb2 I5 . . 88.688(7)
I2 Pb2 I5 2_656 2_656 88.688(7)
I2 Pb2 I5 . 2_656 92.909(7)
I5 Pb2 I5 . 2_656 177.807(11)
I2 Pb2 I1 2_656 2_656 86.367(6)
I2 Pb2 I1 . 2_656 172.973(8)
I5 Pb2 I1 . 2_656 91.365(6)
I5 Pb2 I1 2_656 2_656 87.234(6)
I2 Pb2 I1 2_656 . 172.972(8)
I2 Pb2 I1 . . 86.366(7)
I5 Pb2 I1 . . 87.234(6)
I5 Pb2 I1 2_656 . 91.366(6)
I1 Pb2 I1 2_656 . 100.656(10)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.346(5)
C1 C2 . 1.384(6)
C1 H1 . 0.95
C2 C3 . 1.381(6)
C2 H2 . 0.95
C3 N2 . 1.341(5)
C3 H3 . 0.95
C4 N2 . 1.460(5)
C4 C5 . 1.515(6)
C4 H4A . 0.99
C4 H4B . 0.99
C5 N3 . 1.496(5)
C5 H5A . 0.99
C5 H5B . 0.99
I1 Pb1 . 3.2591(3)
I1 Pb2 . 3.3470(3)
I2 Pb2 . 3.1326(3)
I2 Pb1 . 3.1780(3)
I3 Pb1 . 3.1277(3)
I4 Pb1 7_556 3.1870(3)
I4 Pb1 . 3.2691(3)
I5 Pb2 . 3.1638(3)
I5 Pb1 . 3.2929(3)
N1 N2 . 1.352(4)
N3 H3A . 0.91
N3 H3B . 0.91
N3 H3C . 0.91
O1 H1O . 0.837
O1 H2O . 0.8491
