#------------------------------------------------------------------------------
#$Date: 2019-11-25 23:49:47 +0200 (Mon, 25 Nov 2019) $
#$Revision: 242094 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/20/4132052.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_4132052
loop_
_publ_author_name
'Spanopoulos, Ioannis'
'Ke, Weijun'
'Stoumpos, Constantinos C.'
'Schueller, Emily C.'
'Kontsevoi, Oleg Y.'
'Seshadri, Ram'
'Kanatzidis, Mercouri G.'
_publ_section_title
;
 Unraveling the Chemical Nature of the 3D "Hollow" Hybrid Halide
 Perovskites.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5728
_journal_page_last               5742
_journal_paper_doi               10.1021/jacs.8b01034
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         (H3NCH2CH2NH3)PbI4
_chemical_formula_sum            'C2 H12 I4 N2 O2 Pb'
_chemical_formula_weight         810.9
_chemical_name_common            'ethylenediamonium lead iodide'
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_cell_angle_alpha                90
_cell_angle_beta                 113.907(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.492(3)
_cell_length_b                   4.7532(11)
_cell_length_c                   10.4165(18)
_cell_measurement_reflns_used    3357
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.00
_cell_measurement_theta_min      2.14
_cell_volume                     746.5(3)
_diffrn_ambient_temperature      293
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'IPDS Stoe'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3610
_diffrn_reflns_theta_full        29.25
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         2.14
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    19.546
_exptl_absorpt_correction_T_max  0.3446
_exptl_absorpt_correction_T_min  0.0901
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   X-Shape
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.6077
_exptl_crystal_description       'yellow block'
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.1275
_exptl_crystal_size_mid          0.0389
_exptl_crystal_size_min          0.0304
_refine_diff_density_max         4.41
_refine_diff_density_min         -4.77
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_gt    3.61
_refine_ls_goodness_of_fit_ref   3.36
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_constraints    0
_refine_ls_number_parameters     42
_refine_ls_number_reflns         1119
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.0684
_refine_ls_shift/su_mean         0.0057
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/(σ²(I)+0.0004I²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1326
_refine_ls_wR_factor_ref         0.1332
_reflns_number_gt                964
_reflns_number_total             1119
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ja8b01034_si_005.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_formula_sum        'C2 H12 I4 N2 O2 Pb1'
_cod_database_code               4132052
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,y,-z
3 -x,-y,-z
4 x,-y,z
5 x+1/2,y+1/2,z
6 -x+1/2,y+1/2,-z
7 -x+1/2,-y+1/2,-z
8 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_adp_type
_atom_site_U_iso_or_equiv
_atom_site_site_symmetry_multiplicity
_atom_site_occupancy
_atom_site_calc_flag
Pb Pb 0.5 0 0.5 Uani 0.0337(5) 2 1 d
I1 I 0.36043(11) 0 0.17986(16) Uani 0.0413(6) 4 1 d
I2 I 0.11205(11) 0 0.43235(17) Uani 0.0407(7) 4 1 d
N N 0.12512(11) 0 0.075(4) Uiso 0.121(10) 4 1 d
C C 0.0341(8) 0 0.0743(6) Uiso 0.121(10) 4 1 d
O O 0.1977(13) 0.5 0.230(2) Uiso 0.058(5) 4 1 d
H1n H 0.156766 -0.164418 0.122506 Uiso 0.1454 8 0.5 d
H2n H 0.120286 0 -0.02048 Uiso 0.1454 4 1 d
H3n H 0.156551 0.165392 0.121664 Uiso 0.1454 8 0.5 d
H1c H 0.026819 -0.164908 0.121763 Uiso 0.1454 8 0.5 d
H2c H 0.026819 0.164908 0.121763 Uiso 0.1454 8 0.5 d
H1o H 0.218569 0.643838 0.274302 Uiso 0.0692 8 0.5 d
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'
O 0.0106 0.0060 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-11 1 30 0.0304
5 1 -30 0.0311
-6 30 -3 0.1275
15 -30 -2 0.1193
30 0 -8 0.0376
-30 0 9 0.0389
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
I1 Pb I1 . 2_656 180.0(5)
I1 Pb I2 . 5_545 90.35(4)
I1 Pb I2 . 5_555 90.35(4)
I1 Pb I2 . 6_546 89.65(4)
I1 Pb I2 . 6_556 89.65(4)
I1 Pb I2 2_656 5_545 89.65(4)
I1 Pb I2 2_656 5_555 89.65(4)
I1 Pb I2 2_656 6_546 90.35(4)
I1 Pb I2 2_656 6_556 90.35(4)
I2 Pb I2 5_545 5_555 93.68(4)
I2 Pb I2 5_545 6_546 86.32(4)
I2 Pb I2 5_545 6_556 180.0(5)
I2 Pb I2 5_555 6_546 180.0(5)
I2 Pb I2 5_555 6_556 86.32(4)
I2 Pb I2 6_546 6_556 93.68(4)
Pb I1 N . . 123.5(7)
Pb I1 N . 6_545 121.9(3)
Pb I1 N . 6_555 121.9(3)
N I1 N . 6_545 99.2(5)
N I1 N . 6_555 99.2(5)
N I1 N 6_545 6_555 81.5(6)
Pb I2 Pb 5_445 5_455 93.68(6)
Pb I2 N 5_445 . 118.19(4)
Pb I2 N 5_455 . 118.19(4)
I1 N I1 . 6_545 80.8(5)
I1 N I1 . 6_555 80.8(5)
I1 N I2 . . 100.7(7)
I1 N C . . 164(2)
I1 N H1n . . 63.0(5)
I1 N H1n . 4_555 63.0(5)
I1 N H2n . . 86.6(9)
I1 N H3n . . 63.2(5)
I1 N H3n . 4_555 63.2(5)
I1 N I1 6_545 6_555 81.5(9)
I1 N I2 6_545 . 139.2(4)
I1 N C 6_545 . 111.0(10)
I1 N H1n 6_545 . 70.2(19)
I1 N H1n 6_545 4_555 137(2)
I1 N H2n 6_545 . 41.5(5)
I1 N H3n 6_545 . 136(2)
I1 N H3n 6_545 4_555 69.7(19)
I1 N I2 6_555 . 139.2(4)
I1 N C 6_555 . 111.0(10)
I1 N H1n 6_555 . 137(2)
I1 N H1n 6_555 4_555 70.2(19)
I1 N H2n 6_555 . 41.5(5)
I1 N H3n 6_555 . 69.7(19)
I1 N H3n 6_555 4_555 136(2)
I2 N C . . 63.4(14)
I2 N H1n . . 74(2)
I2 N H1n . 4_555 74(2)
I2 N H2n . . 172.7(2)
I2 N H3n . . 75(2)
I2 N H3n . 4_555 75(2)
C N H1n . . 110(2)
C N H1n . 4_555 110(2)
C N H2n . . 109.3(13)
C N H3n . . 110(2)
C N H3n . 4_555 110(2)
H1n N H1n . 4_555 109(2)
H1n N H2n . . 109(2)
H1n N H3n . . 110(2)
H1n N H3n . 4_555 0.553(7)
H1n N H2n 4_555 . 109(2)
H1n N H3n 4_555 . 0.553(7)
H1n N H3n 4_555 4_555 110(2)
H2n N H3n . . 109(2)
H2n N H3n . 4_555 109(2)
H3n N H3n . 4_555 110(2)
N C C . 2_555 109.6(17)
N C H1c . . 109.4(10)
N C H1c . 4_555 109.4(10)
C C H1c 2_555 . 109.5(7)
C C H1c 2_555 4_555 109.5(7)
H1c C H1c . 4_555 109.5(10)
H1o O H1o . 4_565 113.3(19)
N H1n H3n . 4_555 90(2)
N H3n H1n . 4_555 89(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pb I1 . 3.193(2)
Pb I1 2_656 3.193(2)
Pb I2 5_545 3.2581(17)
Pb I2 5_555 3.2581(17)
Pb I2 6_546 3.2581(17)
Pb I2 6_556 3.2581(17)
I1 N . 3.580(6)
I1 N 6_545 3.64(3)
I1 N 6_555 3.64(3)
I2 N . 3.81(4)
N C . 1.50(2)
N H1n . 0.958(12)
N H1n 4_555 0.958(12)
N H2n . 0.97(4)
N H3n . 0.959(12)
N H3n 4_555 0.959(12)
C C 2_555 1.500(9)
C H1c . 0.960(6)
C H1c 4_555 0.960(6)
O H1o . 0.819(9)
O H1o 4_565 0.819(9)
H1n H3n 4_555 0.0093
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N H1n O 1_545 0.958(12) 1.908(10) 2.850(19) 166.8(19)
N H3n O . 0.959(12) 1.909(10) 2.850(19) 166.6(19)
