#------------------------------------------------------------------------------
#$Date: 2016-07-14 12:03:03 +0300 (Thu, 14 Jul 2016) $
#$Revision: 184455 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/26/4002667.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_4002667
loop_
_publ_author_name
'Kamminga, Machteld E.'
'Fang, Hong-Hua'
'Filip, Marina R.'
'Giustino, Feliciano'
'Baas, Jacob'
'Blake, Graeme R.'
'Loi, Maria Antonietta'
'Palstra, Thomas T. M.'
_publ_section_title
;
 Confinement Effects in Low-Dimensional Lead Iodide Perovskite Hybrids
;
_journal_issue                   13
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4554
_journal_paper_doi               10.1021/acs.chemmater.6b00809
_journal_volume                  28
_journal_year                    2016
_chemical_formula_sum            'C14 H20 I4 N2 Pb'
_chemical_formula_weight         917.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.1111(3)
_cell_length_b                   8.6338(3)
_cell_length_c                   28.4080(10)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.33
_cell_measurement_theta_min      2.87
_cell_volume                     2234.67(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_av_unetI/netI     0.0131
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            30920
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.868
_exptl_absorpt_coefficient_mu    13.069
_exptl_absorpt_correction_T_max  0.7800
_exptl_absorpt_correction_T_min  0.1209
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.726
_exptl_crystal_description       Rectangular
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.392
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0173
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0217P)²+4.0456P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0428
_refine_ls_wR_factor_ref         0.0435
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2202
_reflns_number_total             2287
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            PMAPbI4.cif
_cod_data_source_block           PMAPbI4
_cod_database_code               4002667
_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   0.121
_shelx_estimated_absorpt_t_max   0.780
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.0000 0.0000 0.5000 0.01318(6) Uani 1 2 d S . P . .
I02 I 0.29488(2) 0.20141(2) 0.50752(2) 0.01611(7) Uani 1 1 d . . . . .
I03 I 0.04300(3) 0.02154(2) 0.38860(2) 0.01894(7) Uani 1 1 d . . . . .
N1 N 0.5848(3) 0.0676(3) 0.58635(10) 0.0206(6) Uani 1 1 d . . . . .
H1A H 0.5922 0.0540 0.5547 0.031 Uiso 1 1 calc R U . . .
H1B H 0.6747 0.0558 0.5998 0.031 Uiso 1 1 calc R U . . .
H1C H 0.5502 0.1644 0.5925 0.031 Uiso 1 1 calc R U . . .
C2 C 0.4804(5) -0.0511(4) 0.60644(13) 0.0258(8) Uani 1 1 d . . . . .
H2A H 0.3892 -0.0529 0.5875 0.031 Uiso 1 1 calc R U . . .
H2B H 0.5258 -0.1551 0.6047 0.031 Uiso 1 1 calc R U . . .
C3 C 0.4438(4) -0.0143(4) 0.65654(13) 0.0201(7) Uani 1 1 d . . . . .
C4 C 0.5181(4) -0.0837(5) 0.69354(13) 0.0266(8) Uani 1 1 d . . . . .
H4 H 0.5955 -0.1543 0.6872 0.032 Uiso 1 1 calc R U . . .
C5 C 0.4805(5) -0.0509(5) 0.73980(14) 0.0282(8) Uani 1 1 d . . . . .
H5 H 0.5319 -0.0989 0.7650 0.034 Uiso 1 1 calc R U . . .
C6 C 0.3687(5) 0.0511(4) 0.74912(14) 0.0305(8) Uani 1 1 d . . . . .
H6 H 0.3415 0.0721 0.7808 0.037 Uiso 1 1 calc R U . . .
C7 C 0.2957(4) 0.1231(5) 0.71264(15) 0.0324(9) Uani 1 1 d . . . . .
H7 H 0.2200 0.1955 0.7193 0.039 Uiso 1 1 calc R U . . .
C8 C 0.3323(4) 0.0903(4) 0.66654(14) 0.0275(8) Uani 1 1 d . . . . .
H8 H 0.2810 0.1395 0.6416 0.033 Uiso 1 1 calc R U . . .
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'
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
I02 Pb1 I02 180.0 8_655 4_456
I02 Pb1 I03 92.378(6) 8_655 .
I02 Pb1 I03 87.622(6) 4_456 .
I02 Pb1 I03 87.623(6) 8_655 5_556
I02 Pb1 I03 92.377(6) 4_456 5_556
I03 Pb1 I03 180.0 . 5_556
I02 Pb1 I02 86.731(3) 8_655 .
I02 Pb1 I02 93.269(3) 4_456 .
I03 Pb1 I02 86.082(6) . .
I03 Pb1 I02 93.918(6) 5_556 .
I02 Pb1 I02 93.269(3) 8_655 5_556
I02 Pb1 I02 86.731(3) 4_456 5_556
I03 Pb1 I02 93.920(6) . 5_556
I03 Pb1 I02 86.081(6) 5_556 5_556
I02 Pb1 I02 180.0 . 5_556
Pb1 I02 Pb1 157.525(7) 4_556 .
C2 N1 H1A 109.5 . .
C2 N1 H1B 109.5 . .
H1A N1 H1B 109.5 . .
C2 N1 H1C 109.5 . .
H1A N1 H1C 109.5 . .
H1B N1 H1C 109.5 . .
C3 C2 N1 110.8(3) . .
C3 C2 H2A 109.5 . .
N1 C2 H2A 109.5 . .
C3 C2 H2B 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 108.1 . .
C4 C3 C8 118.9(4) . .
C4 C3 C2 121.4(3) . .
C8 C3 C2 119.7(3) . .
C3 C4 C5 120.6(4) . .
C3 C4 H4 119.7 . .
C5 C4 H4 119.7 . .
C6 C5 C4 119.8(4) . .
C6 C5 H5 120.1 . .
C4 C5 H5 120.1 . .
C5 C6 C7 120.1(4) . .
C5 C6 H6 119.9 . .
C7 C6 H6 119.9 . .
C6 C7 C8 120.2(4) . .
C6 C7 H7 119.9 . .
C8 C7 H7 119.9 . .
C7 C8 C3 120.3(4) . .
C7 C8 H8 119.9 . .
C3 C8 H8 119.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I02 3.1912(2) 8_655
Pb1 I02 3.1912(2) 4_456
Pb1 I03 3.1942(2) .
Pb1 I03 3.1943(2) 5_556
Pb1 I02 3.2075(2) .
Pb1 I02 3.2075(2) 5_556
I02 Pb1 3.1912(2) 4_556
N1 C2 1.510(5) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
C2 C3 1.496(5) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 C4 1.386(5) .
C3 C8 1.389(5) .
C4 C5 1.387(5) .
C4 H4 0.9500 .
C5 C6 1.372(6) .
C5 H5 0.9500 .
C6 C7 1.379(6) .
C6 H6 0.9500 .
C7 C8 1.381(6) .
C7 H7 0.9500 .
C8 H8 0.9500 .
