#------------------------------------------------------------------------------
#$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/(\s^2^(I)+0.0004I^2^)
_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>2\s(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_site_aniso_label
_atom_site_aniso_type_symbol
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pb Pb 0.0357(8) 0.0370(7) 0.0264(7) 0 0.0104(6) 0
I1 I 0.0362(9) 0.0547(10) 0.0289(9) 0 0.0090(7) 0
I2 I 0.0447(10) 0.0414(9) 0.0405(10) 0 0.0220(8) 0
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)
loop_
_refln_index_h
_refln_index_k
_refln_index_l
_refln_F_squared_calc
_refln_F_squared_meas
_refln_F_squared_sigma
_refln_observed_status
2 0 0 16738.00 21679.90 422.96 o
4 0 0 44567.20 39685.20 380.98 o
6 0 0 21736.40 23281.50 269.02 o
8 0 0 84997.70 86674.30 421.41 o
10 0 0 6687.22 6723.84 189.71 o
12 0 0 404.32 814.82 171.05 o
14 0 0 4191.54 4008.80 199.04 o
16 0 0 3848.70 3702.46 213.04 o
18 0 0 562.40 522.48 233.25 o
20 0 0 1030.39 1124.27 259.69 o
1 1 0 10868.30 8662.92 129.07 o
3 1 0 4683.63 3955.93 116.62 o
5 1 0 57381.40 48712.00 245.69 o
7 1 0 33373.40 30904.10 217.70 o
9 1 0 646.71 645.33 129.07 o
11 1 0 225.96 363.87 146.17 o
13 1 0 20516.20 21516.60 192.82 o
15 1 0 12512.00 13320.20 181.93 o
17 1 0 475.10 531.81 208.37 o
19 1 0 55.36 216.15 172.60 <
0 2 0 183606.00 149007.00 413.63 o
2 2 0 10209.60 8529.20 99.52 o
4 2 0 19304.40 20759.30 136.84 o
6 2 0 10796.80 11435.50 127.51 o
8 2 0 51707.70 51030.60 199.04 o
10 2 0 4855.90 5521.82 121.29 o
12 2 0 257.64 352.99 122.85 o
14 2 0 2831.26 3279.50 143.06 o
16 2 0 2655.85 3268.62 161.72 o
18 2 0 398.74 608.01 188.15 o
1 3 0 4899.91 6196.69 87.08 o
3 3 0 3431.39 3881.29 83.97 o
5 3 0 22213.20 22973.60 133.73 o
7 3 0 14158.20 16714.70 127.51 o
9 3 0 135.94 237.92 104.18 o
11 3 0 56.31 287.68 113.51 o
13 3 0 9506.40 10717.10 155.50 o
15 3 0 5745.07 5871.69 158.61 o
17 3 0 175.32 435.40 161.72 o
0 4 0 38849.40 41411.30 214.59 o
2 4 0 3010.66 3456.77 93.30 o
4 4 0 3430.90 3531.41 96.41 o
6 4 0 2824.21 2253.20 105.74 o
8 4 0 13516.40 8983.26 135.29 o
10 4 0 1996.68 1550.34 122.85 o
12 4 0 35.32 130.62 139.95 <
14 4 0 807.66 897.24 166.38 o
16 4 0 1097.16 1054.29 169.49 o
1 5 0 1129.87 1253.33 91.75 o
3 5 0 1352.68 1458.59 101.07 o
5 5 0 5137.91 5436.29 121.29 o
7 5 0 2843.63 3027.59 124.40 o
9 5 0 30.88 13.99 135.29 <
11 5 0 48.53 213.04 155.50 <
13 5 0 1995.56 1225.34 166.38 o
0 6 0 5107.31 5342.99 303.23 o
2 6 0 731.23 562.91 119.74 o
4 6 0 194.01 499.16 133.73 o
6 6 0 468.39 564.47 147.73 o
8 6 0 2396.88 1783.59 261.24 o
-20 0 1 119.23 -18.66 259.69 <
-18 0 1 6004.22 6033.41 231.70 o
-16 0 1 13606.00 13858.20 230.14 o
-14 0 1 599.57 489.83 169.49 o
-12 0 1 2648.21 2271.86 169.49 o
-10 0 1 49590.90 48569.00 315.67 o
-8 0 1 66904.40 66924.20 379.42 o
-6 0 1 3649.66 5865.47 222.37 o
-4 0 1 547.05 500.71 228.59 o
-2 0 1 65123.80 49427.30 663.99 o
0 0 1 44755.80 33488.60 629.78 o
2 0 1 15818.90 11905.10 269.02 o
4 0 1 15300.70 13318.60 227.03 o
6 0 1 7860.90 8028.48 197.49 o
8 0 1 820.14 1076.06 161.72 o
10 0 1 19445.60 21928.70 250.36 o
12 0 1 19544.30 21395.30 253.47 o
14 0 1 201.17 362.32 213.04 <
16 0 1 147.49 216.15 217.70 <
18 0 1 5323.50 6209.13 477.39 o
-21 1 1 352.54 586.24 315.67 <
-19 1 1 45.19 214.59 167.94 <
-17 1 1 1721.58 2013.73 153.95 o
-15 1 1 3590.26 3683.80 153.95 o
-13 1 1 3001.46 2851.88 136.84 o
-11 1 1 12957.70 12898.80 175.71 o
-9 1 1 14090.10 16237.30 172.60 o
-7 1 1 2158.15 1778.92 125.96 o
-5 1 1 11617.90 11741.80 146.17 o
-3 1 1 183107.00 124436.00 359.21 o
-1 1 1 20750.70 22721.70 174.16 o
1 1 1 27539.80 26907.80 194.38 o
3 1 1 12360.30 12418.30 203.71 o
5 1 1 148932.00 126565.00 413.63 o
7 1 1 12471.40 13082.20 174.16 o
9 1 1 9615.07 10454.30 217.70 o
11 1 1 6577.37 6792.26 214.59 o
13 1 1 18860.40 19827.90 247.25 o
15 1 1 1002.29 1030.97 153.95 o
17 1 1 69.55 129.07 177.27 <
19 1 1 1027.59 962.55 191.26 o
-20 2 1 41.37 393.42 202.15 <
-18 2 1 4351.84 4887.38 185.04 o
-16 2 1 8779.50 10034.40 188.15 o
-14 2 1 239.47 404.30 183.49 o
-12 2 1 1333.70 1472.59 152.39 o
-10 2 1 30267.10 29837.40 214.59 o
-8 2 1 44120.40 44092.10 183.49 o
-6 2 1 965.88 1024.75 96.41 o
-4 2 1 253.59 715.30 83.97 o
-2 2 1 37595.80 39035.30 191.26 o
0 2 1 28697.60 31156.10 147.73 o
2 2 1 9229.39 10689.10 108.85 o
4 2 1 10003.70 13772.70 153.95 o
6 2 1 5145.62 5779.95 111.96 o
8 2 1 886.27 803.94 97.97 o
10 2 1 13842.10 15592.00 153.95 o
12 2 1 12418.30 14051.00 155.50 o
14 2 1 117.29 157.05 136.84 <
16 2 1 43.58 216.15 155.50 <
18 2 1 3574.43 4772.31 195.93 o
-19 3 1 52.56 82.42 514.71 <
-17 3 1 781.81 855.25 157.05 o
-15 3 1 1697.88 2128.80 144.62 o
-13 3 1 1901.17 2615.52 136.84 o
-11 3 1 5904.85 6579.22 125.96 o
-9 3 1 4606.51 5147.06 107.29 o
-7 3 1 580.41 772.84 90.19 o
-5 3 1 5711.84 6437.71 96.41 o
-3 3 1 56999.80 53798.50 195.93 o
-1 3 1 6074.06 6719.17 88.64 o
1 3 1 7987.38 9207.18 94.86 o
3 3 1 5681.97 5414.52 91.75 o
5 3 1 53209.10 52804.80 185.04 o
7 3 1 4771.62 4298.03 110.40 o
9 3 1 2967.46 3270.17 115.07 o
11 3 1 2882.71 3760.00 121.29 o
13 3 1 8272.60 9889.82 160.16 o
15 3 1 710.40 1110.27 144.62 o
17 3 1 68.09 334.33 177.27 <
-16 4 1 2860.07 2999.60 164.83 o
-14 4 1 48.86 300.12 139.95 o
-12 4 1 248.57 342.10 124.40 o
-10 4 1 8984.87 9255.38 130.62 o
-8 4 1 12912.40 9994.01 129.07 o
-6 4 1 67.01 13.99 87.08 <
-4 4 1 178.36 118.18 85.53 <
-2 4 1 9586.33 11765.20 124.40 o
0 4 1 10084.70 11413.70 108.85 o
2 4 1 3851.91 4251.38 93.30 o
4 4 1 2637.57 3282.61 116.62 o
6 4 1 1642.64 990.54 102.63 o
8 4 1 832.44 338.99 110.40 o
10 4 1 4399.62 2980.94 138.40 o
12 4 1 3610.45 2711.93 153.95 o
14 4 1 28.54 244.14 157.05 <
-13 5 1 784.17 458.73 171.05 o
-11 5 1 1602.66 914.34 147.73 o
-9 5 1 873.63 485.16 129.07 o
-7 5 1 53.05 37.32 118.18 <
-5 5 1 1771.92 2071.26 111.96 o
-3 5 1 10019.60 11192.90 111.96 o
-1 5 1 1117.95 1394.84 113.51 o
1 5 1 909.62 1289.10 99.52 o
3 5 1 1428.36 1617.20 127.51 o
5 5 1 9802.64 10751.30 135.29 o
7 5 1 1332.51 1262.66 125.96 o
9 5 1 288.93 329.66 138.40 o
11 5 1 739.39 642.22 158.61 o
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