#------------------------------------------------------------------------------
#$Date: 2019-11-03 17:30:44 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221974 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/89/4128939.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_4128939
loop_
_publ_author_name
'Tremblay, Marie-Hélène'
'Thouin, Félix'
'Leisen, Johannes'
'Bacsa, John'
'Srimath Kandada, Ajay Ram'
'Hoffman, Justin M.'
'Kanatzidis, Mercouri G.'
'Mohite, Aditya D.'
'Silva, Carlos'
'Barlow, Stephen'
'Marder, Seth R.'
_publ_section_title
;
 (4NPEA)₂PbI₄ (4NPEA = 4-Nitrophenylethylammonium):
 Structural, NMR, and Optical Properties of a 3 × 3 Corrugated 2D
 Hybrid Perovskite.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4521
_journal_page_last               4525
_journal_paper_doi               10.1021/jacs.8b13207
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         '(I4 Pb), 2(C8 H11 N2 O2)'
_chemical_formula_sum            'C16 H22 I4 N4 O4 Pb'
_chemical_formula_weight         1049.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-20
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2018.07.26 svn.r3523 for OlexSys, GUI svn.r5532)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.2252(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.0976(4)
_cell_length_b                   19.8255(3)
_cell_length_c                   12.6149(2)
_cell_measurement_reflns_used    32454
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.7420
_cell_measurement_theta_min      1.9140
_cell_volume                     5222.16(15)
_computing_cell_refinement       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.43c (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 HyPix
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω     -2.00  80.00   0.50   25.00    --   15.69  38.00 -60.00  164
  2  ω     57.00  85.00   0.50   25.00    --   15.69   0.00 -30.00   56
  3  ω      4.00  34.00   0.50   25.00    --   15.69  57.00-150.00   60
  4  ω    -34.00  -1.00   0.50   25.00    --   15.69   0.00 -30.00   66
  5  ω    -24.00   5.00   0.50   25.00    --   15.69 -57.00-120.00   58
  6  ω    -56.00  34.00   0.50   25.00    --   15.69 -57.00-150.00  180
  7  ω    -24.00  59.00   0.50   25.00    --  -15.84  38.00-180.00  166
  8  ω    -59.00  34.00   0.50   25.00    --   15.69 -38.00 -60.00  186
  9  ω    -86.00 -32.00   0.50   25.00    --  -15.84 -57.00  60.00  108
 10  ω    -89.00 -21.00   0.50   25.00    --  -15.84 -57.00-180.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0144901000
_diffrn_orient_matrix_UB_12      -0.0293935000
_diffrn_orient_matrix_UB_13      0.0248131000
_diffrn_orient_matrix_UB_21      -0.0307133000
_diffrn_orient_matrix_UB_22      -0.0134875000
_diffrn_orient_matrix_UB_23      0.0038903000
_diffrn_orient_matrix_UB_31      -0.0007337000
_diffrn_orient_matrix_UB_32      -0.0153028000
_diffrn_orient_matrix_UB_33      -0.0509651000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            90640
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         1.928
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.218
_exptl_absorpt_correction_T_max  0.908
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.43c (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.669
_exptl_crystal_description       plate
_exptl_crystal_F_000             3776
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.019
_refine_diff_density_max         3.260
_refine_diff_density_min         -2.533
_refine_diff_density_rms         0.238
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         14658
_refine_ls_number_restraints     603
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0521
_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)+(0.0421P)²+85.4699P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11561
_reflns_number_total             14658
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja8b13207_si_002.cif
_cod_data_source_block           mht-iii-53
_cod_original_cell_volume        5222.17(16)
_cod_database_code               4128939
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C180  I32  N12  O8  Pb8  '
_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.
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
2. Restrained distances
 N2_4-C8_4
 1.48 with sigma of 0.005
 C8_1-C7_1
 1.52 with sigma of 0.005
 N1_3-C1_3
 1.47 with sigma of 0.005
 Pb1-I2B \\sim Pb1-I2A
 with sigma of 0.005
 Pb2-I4A \\sim Pb2-I4B
 with sigma of 0.002
 O2_4-N1_4 \\sim O1_4-N1_4
 with sigma of 0.002
 C6_2-C1_2 \\sim C2_2-C1_2
 with sigma of 0.002
 C3_2-C2_2 \\sim C6_2-C5_2
 with sigma of 0.002
 C5_2-C4_2 \\sim C4_2-C3_2
 with sigma of 0.002
3. Restrained planarity
 C2_3, C1_3, C6_3, C5_3, C4_3, C3_3, N1_3
 with sigma of 0.002
4. Uiso/Uaniso restraints and constraints
I4A \\sim I4B: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
I7B \\sim I7A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008
Uanis(I7B) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C6_4) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1_2) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1_1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(C1_3) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
Uanis(I8A) = Uanis(I8B)
Uanis(I2A) = Uanis(I2B)
5. Rigid body (RIGU) restrains
 Pb2, I4A
 with sigma for 1-2 distances of 0.0002 and sigma for 1-3 distances of 0.0002
 O1_4, N1_4, O2_4, C1_4, C2_4, C6_4, C3_4, C5_4, C4_4, C7_4, C8_4, N2_4
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C7_2, O1_2, N1_2, O2_2, C1_2, C2_2, C6_2, C3_2, C5_2, C4_2, C8_2, N2_2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C7_1, O1_1, N1_1, O2_1, C1_1, C2_1, C6_1, C3_1, C5_1, C4_1, C8_1, N2_1
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C1_3, O1_3, N1_3, O2_3, C2_3, C6_3, C3_3, C5_3, C4_3, C7_3, C8_3, N2_3
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
6. Same fragment restrains
{O1_2, O2_2, N1_2, N2_2, C1_2, C2_2, C3_2, C4_2, C5_2, C6_2, C7_2, C8_2}
{O1_3, O2_3, N1_3, N2_3, C1_3, C2_3, C3_3, C4_3, C5_3, C6_3, C7_3, C8_3}
{O1_4, O2_4, N1_4, N2_4, C1_4, C2_4, C3_4, C4_4, C5_4, C6_4, C7_4, C8_4}
as
{O1_1, O2_1, N1_1, N2_1, C1_1, C2_1, C3_1, C4_1, C5_1, C6_1, C7_1, C8_1} sigma
for 1-2: 0.002 1-3: 0.004
7. Others
 Sof(I8B)=Sof(I4A)=Sof(I7B)=Sof(I2B)=1-FVAR(1)
 Sof(I2A)=Sof(I8A)=Sof(I7A)=Sof(I4B)=FVAR(1)
8.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B), C7(H7A,H7B), C8(H8A,H8B),
 C7(H7A,H7B), C8(H8A,H8B)
8.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6), C2(H2),
 C3(H3), C5(H5), C6(H6), C2(H2), C3(H3), C5(H5), C6(H6)
8.c Idealised Me refined as rotating group:
 N2(H2A,H2B,H2C), N2(H2A,H2B,H2C), N2(H2A,H2B,H2C), N2(H2A,H2B,H2C)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a loop with paratone oil'
_olex2_submission_original_sample_id MHT-III-53
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.235
_oxdiff_exptl_absorpt_empirical_full_min 0.860
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
I1 I 0.62079(3) 0.59502(3) 0.99335(5) 0.04032(15) Uani 1 1 d . . . . .
I8B I 0.81514(8) 0.16864(8) 0.53886(15) 0.0389(2) Uani 0.4076(13) 1 d . . . A 2
I3 I 0.47827(3) 0.47757(4) 0.74536(4) 0.04070(15) Uani 1 1 d . . . . .
I5 I 0.56080(3) 0.35279(3) 0.49787(6) 0.04766(17) Uani 1 1 d . . . . .
I6 I 0.78379(4) 0.37647(3) 0.50661(6) 0.0540(2) Uani 1 1 d . . . . .
Pb1 Pb 0.500000 0.500000 1.000000 0.02431(9) Uani 1 2 d DS T P . .
Pb2 Pb 0.500000 0.500000 0.500000 0.02238(9) Uani 1 2 d DS TU P . .
Pb3 Pb 0.69303(2) 0.25864(2) 0.52252(2) 0.02703(7) Uani 1 1 d . . . . .
I2A I 0.41670(8) 0.63569(7) 0.98525(15) 0.0348(3) Uani 0.5924(13) 1 d D . . A 1
I4A I 0.64063(9) 0.5509(2) 0.5705(3) 0.0408(8) Uani 0.4076(13) 1 d D U . A 1
I7B I 0.67603(14) 0.27640(13) 0.7732(2) 0.0445(5) Uani 0.4076(13) 1 d . U . A 2
I8A I 0.79559(5) 0.15395(6) 0.58059(10) 0.0389(2) Uani 0.5924(13) 1 d . . . A 1
I7A I 0.69130(11) 0.25220(8) 0.77454(13) 0.0487(4) Uani 0.5924(13) 1 d . U . A
1
I2B I 0.40070(12) 0.62166(11) 0.9621(2) 0.0348(3) Uani 0.4076(13) 1 d D . . A 2
I4B I 0.63170(7) 0.56370(14) 0.59626(18) 0.0343(4) Uani 0.5924(13) 1 d D U . A
2
O1_1 O 0.8387(5) 0.6923(6) 0.9924(8) 0.099(3) Uani 1 1 d D U . . .
O2_1 O 0.8057(4) 0.7692(5) 1.0914(6) 0.077(2) Uani 1 1 d D U . . .
N1_1 N 0.8008(4) 0.7333(4) 1.0142(6) 0.0623(16) Uani 1 1 d D U . . .
N2_1 N 0.5175(5) 0.6721(4) 0.7741(8) 0.0580(19) Uani 1 1 d D U . . .
H2A_1 H 0.514621 0.650985 0.711296 0.070 Uiso 1 1 calc GR . . . .
H2B_1 H 0.484995 0.659595 0.807578 0.070 Uiso 1 1 calc GR . . . .
H2C_1 H 0.554312 0.661252 0.814050 0.070 Uiso 1 1 calc GR . . . .
C1_1 C 0.7421(4) 0.7420(5) 0.9355(7) 0.0642(14) Uani 1 1 d D U . . .
C2_1 C 0.6974(4) 0.7874(5) 0.9555(7) 0.0545(15) Uani 1 1 d D U . . .
H2_1 H 0.703976 0.812441 1.018399 0.065 Uiso 1 1 calc R . . . .
C3_1 C 0.6435(4) 0.7967(5) 0.8857(6) 0.0537(15) Uani 1 1 d D U . . .
H3_1 H 0.612907 0.827502 0.901360 0.064 Uiso 1 1 calc R . . . .
C4_1 C 0.6334(4) 0.7600(4) 0.7889(6) 0.0547(11) Uani 1 1 d D U . . .
C5_1 C 0.6815(4) 0.7136(5) 0.7710(7) 0.0557(16) Uani 1 1 d D U . . .
H5_1 H 0.676601 0.688127 0.708395 0.067 Uiso 1 1 calc R . . . .
C6_1 C 0.7343(4) 0.7058(5) 0.8436(7) 0.0604(18) Uani 1 1 d D U . . .
H6_1 H 0.765770 0.675295 0.830528 0.072 Uiso 1 1 calc R . . . .
C7_1 C 0.5747(4) 0.7692(5) 0.7139(6) 0.0581(11) Uani 1 1 d D U . . .
H7A_1 H 0.578504 0.744441 0.648781 0.070 Uiso 1 1 calc R . . . .
H7B_1 H 0.570336 0.816643 0.695310 0.070 Uiso 1 1 calc R . . . .
C8_1 C 0.5150(4) 0.7463(4) 0.7562(9) 0.0571(15) Uani 1 1 d D U . . .
H8A_1 H 0.511501 0.769262 0.823080 0.069 Uiso 1 1 calc R . . . .
H8B_1 H 0.477566 0.757665 0.705273 0.069 Uiso 1 1 calc R . . . .
O1_2 O 1.0292(5) 0.6067(9) 0.9098(10) 0.155(5) Uani 1 1 d D U . . .
O2_2 O 0.9991(6) 0.6464(9) 0.7520(10) 0.153(4) Uani 1 1 d D U . . .
N1_2 N 0.9908(5) 0.6166(7) 0.8316(8) 0.120(3) Uani 1 1 d D U . . .
N2_2 N 0.6514(4) 0.4414(7) 0.7926(10) 0.102(3) Uani 1 1 d D U . . .
H2A_2 H 0.635159 0.462480 0.732576 0.123 Uiso 1 1 calc GR . . . .
H2B_2 H 0.623052 0.442231 0.838579 0.123 Uiso 1 1 calc GR . . . .
H2C_2 H 0.660086 0.398759 0.777812 0.123 Uiso 1 1 calc GR . . . .
C1_2 C 0.9293(4) 0.5797(6) 0.8257(10) 0.0980(18) Uani 1 1 d D U . . .
C2_2 C 0.8805(4) 0.5958(6) 0.7481(9) 0.084(2) Uani 1 1 d D U . . .
H2_2 H 0.885234 0.631388 0.701886 0.101 Uiso 1 1 calc R . . . .
C3_2 C 0.8252(5) 0.5607(7) 0.7370(12) 0.117(3) Uani 1 1 d D U . . .
H3_2 H 0.790521 0.574637 0.687917 0.141 Uiso 1 1 calc R . . . .
C4_2 C 0.8202(5) 0.5028(6) 0.8004(10) 0.117(2) Uani 1 1 d D U . . .
C5_2 C 0.8683(6) 0.4938(7) 0.8893(11) 0.114(3) Uani 1 1 d D U . . .
H5_2 H 0.862509 0.462620 0.942143 0.136 Uiso 1 1 calc R . . . .
C6_2 C 0.9226(5) 0.5304(6) 0.8974(9) 0.092(2) Uani 1 1 d D U . . .
H6_2 H 0.955761 0.521700 0.952706 0.110 Uiso 1 1 calc R . . . .
C7_2 C 0.7648(4) 0.4584(6) 0.7784(11) 0.113(2) Uani 1 1 d D U . . .
H7A_2 H 0.778352 0.412379 0.795053 0.136 Uiso 1 1 calc R . . . .
H7B_2 H 0.748550 0.460409 0.702557 0.136 Uiso 1 1 calc R . . . .
C8_2 C 0.7113(5) 0.4759(7) 0.8411(10) 0.108(3) Uani 1 1 d D U . . .
H8A_2 H 0.722575 0.461715 0.914976 0.130 Uiso 1 1 calc R . . . .
H8B_2 H 0.704719 0.524315 0.840192 0.130 Uiso 1 1 calc R . . . .
O1_3 O 1.0357(8) 0.5588(10) 0.5821(13) 0.242(6) Uani 1 1 d D U . . .
O2_3 O 1.1138(5) 0.5554(5) 0.7118(8) 0.103(3) Uani 1 1 d D U . . .
N1_3 N 1.0627(4) 0.5379(5) 0.6657(8) 0.147(3) Uani 1 1 d D U . . .
N2_3 N 0.8838(6) 0.2119(6) 0.8317(11) 0.102(3) Uani 1 1 d D U . . .
H2A_3 H 0.856685 0.188040 0.785871 0.122 Uiso 1 1 calc GR . . . .
H2B_3 H 0.865552 0.221855 0.889154 0.122 Uiso 1 1 calc GR . . . .
H2C_3 H 0.919192 0.187933 0.851508 0.122 Uiso 1 1 calc GR . . . .
C1_3 C 1.0343(3) 0.4778(4) 0.7108(5) 0.0919(18) Uani 1 1 d D U . . .
C2_3 C 1.0654(4) 0.4494(4) 0.8011(6) 0.0742(18) Uani 1 1 d D U . . .
H2_3 H 1.103887 0.467899 0.833356 0.089 Uiso 1 1 calc R . . . .
C3_3 C 1.0414(4) 0.3948(4) 0.8449(7) 0.082(2) Uani 1 1 d D U . . .
H3_3 H 1.063362 0.375910 0.907019 0.098 Uiso 1 1 calc R . . . .
C4_3 C 0.9830(4) 0.3662(5) 0.7968(7) 0.102(3) Uani 1 1 d D U . . .
C5_3 C 0.9523(5) 0.3975(5) 0.7028(8) 0.086(2) Uani 1 1 d D U . . .
H5_3 H 0.913678 0.380242 0.668518 0.103 Uiso 1 1 calc R . . . .
C6_3 C 0.9783(4) 0.4521(4) 0.6622(7) 0.087(3) Uani 1 1 d D U . . .
H6_3 H 0.957553 0.472183 0.600161 0.105 Uiso 1 1 calc R . . . .
C7_3 C 0.9545(8) 0.3106(8) 0.8492(11) 0.144(3) Uani 1 1 d D U . . .
H7A_3 H 0.938531 0.327824 0.912287 0.173 Uiso 1 1 calc R . . . .
H7B_3 H 0.987677 0.277832 0.872902 0.173 Uiso 1 1 calc R . . . .
C8_3 C 0.9006(11) 0.2755(10) 0.7793(15) 0.196(5) Uani 1 1 d D U . . .
H8A_3 H 0.863526 0.304836 0.767484 0.235 Uiso 1 1 calc R . . . .
H8B_3 H 0.913541 0.265236 0.710241 0.235 Uiso 1 1 calc R . . . .
O1_4 O 0.9546(7) 0.7532(7) 0.3758(13) 0.176(5) Uani 1 1 d D U . . .
O2_4 O 0.9839(6) 0.6840(7) 0.5051(11) 0.148(4) Uani 1 1 d D U . . .
N1_4 N 0.9484(5) 0.7040(6) 0.4289(10) 0.109(3) Uani 1 1 d D U . . .
N2_4 N 0.6805(8) 0.4368(6) 0.2630(16) 0.147(6) Uani 1 1 d D U . . .
H2A_4 H 0.649630 0.437195 0.206982 0.177 Uiso 1 1 calc GR . . . .
H2B_4 H 0.663940 0.446771 0.322145 0.177 Uiso 1 1 calc GR . . . .
H2C_4 H 0.698232 0.395988 0.269674 0.177 Uiso 1 1 calc GR . . . .
C1_4 C 0.8911(5) 0.6619(5) 0.3948(8) 0.085(2) Uani 1 1 d D U . . .
C2_4 C 0.8788(5) 0.6086(6) 0.4558(9) 0.093(3) Uani 1 1 d D U . . .
H2_4 H 0.908171 0.596913 0.515156 0.112 Uiso 1 1 calc R . . . .
C3_4 C 0.8247(5) 0.5723(6) 0.4317(9) 0.088(2) Uani 1 1 d D U . . .
H3_4 H 0.816321 0.536532 0.475339 0.106 Uiso 1 1 calc R . . . .
C4_4 C 0.7807(5) 0.5885(5) 0.3402(8) 0.0901(17) Uani 1 1 d D U . . .
C5_4 C 0.7979(5) 0.6410(5) 0.2743(8) 0.082(2) Uani 1 1 d D U . . .
H5_4 H 0.772289 0.650352 0.209643 0.099 Uiso 1 1 calc R . . . .
C6_4 C 0.8511(6) 0.6777(7) 0.3046(10) 0.1026(19) Uani 1 1 d D U . . .
H6_4 H 0.860513 0.714169 0.263207 0.123 Uiso 1 1 calc R . . . .
C7_4 C 0.7221(5) 0.5493(5) 0.3134(10) 0.0926(17) Uani 1 1 d D U . . .
H7A_4 H 0.689392 0.577969 0.274532 0.111 Uiso 1 1 calc R . . . .
H7B_4 H 0.707066 0.535380 0.379166 0.111 Uiso 1 1 calc R . . . .
C8_4 C 0.7301(6) 0.4876(6) 0.2467(12) 0.097(3) Uani 1 1 d D U . . .
H8A_4 H 0.725973 0.499920 0.171634 0.116 Uiso 1 1 calc R . . . .
H8B_4 H 0.772452 0.468568 0.267472 0.116 Uiso 1 1 calc R . . . .
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'
I I -0.4742 1.8119 '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'
O O 0.0106 0.0060 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -4 -5 0.0476
-1 4 5 0.0476
0 -5 2 0.0438
0 5 -2 0.0438
1 0 0 0.0095
-1 0 0 0.0095
0 -5 -1 0.0488
0 5 1 0.0488
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
Pb1 I3 Pb2 157.22(2) . .
Pb2 I5 Pb3 147.53(3) . .
I1 Pb1 I1 180.0 3_667 .
I1 Pb1 I3 86.794(16) 3_667 .
I1 Pb1 I3 93.206(16) . .
I1 Pb1 I3 93.205(16) 3_667 3_667
I1 Pb1 I3 86.794(16) . 3_667
I1 Pb1 I2A 86.33(3) . .
I1 Pb1 I2A 93.67(3) 3_667 .
I1 Pb1 I2A 86.33(3) 3_667 3_667
I1 Pb1 I2A 93.67(3) . 3_667
I1 Pb1 I2B 93.43(5) . .
I1 Pb1 I2B 93.43(5) 3_667 3_667
I1 Pb1 I2B 86.57(5) . 3_667
I1 Pb1 I2B 86.57(5) 3_667 .
I3 Pb1 I3 180.00(2) 3_667 .
I2A Pb1 I3 93.42(4) 3_667 3_667
I2A Pb1 I3 93.42(4) . .
I2A Pb1 I3 86.58(4) 3_667 .
I2A Pb1 I3 86.58(4) . 3_667
I2A Pb1 I2A 180.00(6) 3_667 .
I2B Pb1 I3 92.40(6) 3_667 .
I2B Pb1 I3 87.60(6) . .
I2B Pb1 I2B 180.00(9) 3_667 .
I3 Pb2 I3 180.0 . 3_666
I5 Pb2 I3 89.681(19) 3_666 3_666
I5 Pb2 I3 89.682(19) . .
I5 Pb2 I3 90.318(19) . 3_666
I5 Pb2 I3 90.318(19) 3_666 .
I5 Pb2 I5 180.0 3_666 .
I4A Pb2 I3 91.76(7) 3_666 3_666
I4A Pb2 I3 91.77(7) . .
I4A Pb2 I3 88.23(7) 3_666 .
I4A Pb2 I3 88.24(7) . 3_666
I4A Pb2 I5 86.09(8) 3_666 3_666
I4A Pb2 I5 86.09(8) . .
I4A Pb2 I5 93.91(8) 3_666 .
I4A Pb2 I5 93.91(8) . 3_666
I4A Pb2 I4A 180.00(12) . 3_666
I4B Pb2 I3 85.62(5) . .
I4B Pb2 I3 94.38(5) 3_666 .
I4B Pb2 I5 92.10(5) . .
I4B Pb2 I5 87.90(5) 3_666 .
I4B Pb2 I4B 180.0 3_666 .
I8B Pb3 I5 178.26(4) . .
I8B Pb3 I7B 101.70(6) . .
I5 Pb3 I2A 80.75(3) . 2_646
I5 Pb3 I2B 88.09(5) . 2_646
I6 Pb3 I8B 85.52(4) . .
I6 Pb3 I5 95.16(2) . .
I6 Pb3 I2A 173.52(3) . 2_646
I6 Pb3 I7B 97.98(5) . .
I6 Pb3 I7B 94.88(5) . 4_565
I6 Pb3 I7A 84.51(4) . 4_565
I6 Pb3 I7A 101.16(4) . .
I6 Pb3 I2B 176.65(5) . 2_646
I2A Pb3 I2B 8.47(4) 2_646 2_646
I7B Pb3 I5 93.18(6) 4_565 .
I7B Pb3 I5 79.80(5) . .
I7B Pb3 I7B 165.83(10) 4_565 .
I8A Pb3 I5 166.14(3) . .
I8A Pb3 I6 96.20(3) . .
I8A Pb3 I2A 88.58(3) . 2_646
I8A Pb3 I7B 93.74(6) . 4_565
I8A Pb3 I7A 80.80(4) . .
I8A Pb3 I7A 95.80(4) . 4_565
I8A Pb3 I2B 80.70(5) . 2_646
I7A Pb3 I5 93.16(4) 4_565 .
I7A Pb3 I5 89.23(4) . .
I7A Pb3 I2A 83.90(5) . 2_646
I7A Pb3 I2A 90.67(5) 4_565 2_646
I7A Pb3 I7B 163.50(5) . 4_565
I7A Pb3 I7B 10.42(4) 4_565 4_565
I7A Pb3 I7A 173.63(2) 4_565 .
I7A Pb3 I2B 94.52(6) 4_565 2_646
I7A Pb3 I2B 79.66(6) . 2_646
Pb1 I2A Pb3 169.29(6) . 2_656
Pb3 I7B Pb3 157.28(9) 4_566 .
Pb3 I7A Pb3 177.90(7) 4_566 .
Pb1 I2B Pb3 167.69(9) . 2_656
O1_1 N1_1 C1_1 116.5(6) . .
O2_1 N1_1 O1_1 127.3(7) . .
O2_1 N1_1 C1_1 116.2(6) . .
C2_1 C1_1 N1_1 119.4(5) . .
C2_1 C1_1 C6_1 120.7(7) . .
C6_1 C1_1 N1_1 120.0(5) . .
C3_1 C2_1 C1_1 121.0(7) . .
C2_1 C3_1 C4_1 120.2(7) . .
C3_1 C4_1 C5_1 116.9(8) . .
C3_1 C4_1 C7_1 120.4(6) . .
C5_1 C4_1 C7_1 122.7(6) . .
C6_1 C5_1 C4_1 120.6(7) . .
C5_1 C6_1 C1_1 120.6(7) . .
C4_1 C7_1 C8_1 114.0(5) . .
N2_1 C8_1 C7_1 109.7(5) . .
O1_2 N1_2 C1_2 116.3(6) . .
O2_2 N1_2 O1_2 127.3(8) . .
O2_2 N1_2 C1_2 115.7(6) . .
C2_2 C1_2 N1_2 119.3(5) . .
C6_2 C1_2 N1_2 119.8(5) . .
C6_2 C1_2 C2_2 120.9(7) . .
C3_2 C2_2 C1_2 120.7(7) . .
C2_2 C3_2 C4_2 119.6(7) . .
C3_2 C4_2 C5_2 116.7(8) . .
C3_2 C4_2 C7_2 120.4(6) . .
C5_2 C4_2 C7_2 122.7(6) . .
C6_2 C5_2 C4_2 120.0(7) . .
C5_2 C6_2 C1_2 120.4(7) . .
C4_2 C7_2 C8_2 113.7(6) . .
N2_2 C8_2 C7_2 109.5(6) . .
O1_3 N1_3 O2_3 127.3(8) . .
O1_3 N1_3 C1_3 116.7(6) . .
O2_3 N1_3 C1_3 115.5(6) . .
C2_3 C1_3 N1_3 118.9(5) . .
C6_3 C1_3 N1_3 120.3(5) . .
C6_3 C1_3 C2_3 120.8(7) . .
C3_3 C2_3 C1_3 121.0(7) . .
C2_3 C3_3 C4_3 120.1(7) . .
C3_3 C4_3 C7_3 119.9(6) . .
C5_3 C4_3 C3_3 117.0(8) . .
C5_3 C4_3 C7_3 122.9(6) . .
C6_3 C5_3 C4_3 120.5(7) . .
C5_3 C6_3 C1_3 120.6(7) . .
C4_3 C7_3 C8_3 114.2(5) . .
N2_3 C8_3 C7_3 109.8(6) . .
O1_4 N1_4 C1_4 116.5(6) . .
O2_4 N1_4 O1_4 127.6(8) . .
O2_4 N1_4 C1_4 115.9(6) . .
C2_4 C1_4 N1_4 119.3(5) . .
C6_4 C1_4 N1_4 119.8(5) . .
C6_4 C1_4 C2_4 120.9(7) . .
C3_4 C2_4 C1_4 120.9(7) . .
C2_4 C3_4 C4_4 120.0(7) . .
C3_4 C4_4 C5_4 117.1(8) . .
C3_4 C4_4 C7_4 120.3(6) . .
C5_4 C4_4 C7_4 122.5(6) . .
C6_4 C5_4 C4_4 120.3(7) . .
C5_4 C6_4 C1_4 120.5(7) . .
C4_4 C7_4 C8_4 113.7(5) . .
N2_4 C8_4 C7_4 109.5(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I1 Pb1 3.1797(6) .
I8B Pb3 3.1162(16) .
I3 Pb1 3.2102(5) .
I3 Pb2 3.2240(5) .
I5 Pb2 3.1896(6) .
I5 Pb3 3.3340(7) .
I6 Pb3 3.0453(7) .
Pb1 I2A 3.2041(14) .
Pb1 I2A 3.2040(14) 3_667
Pb1 I2B 3.186(2) 3_667
Pb1 I2B 3.186(2) .
Pb2 I4A 3.1398(15) .
Pb2 I4A 3.1399(15) 3_666
Pb2 I4B 3.1343(10) 3_666
Pb2 I4B 3.1343(10) .
Pb3 I2A 3.3535(15) 2_646
Pb3 I7B 3.253(3) .
Pb3 I7B 3.190(2) 4_565
Pb3 I8A 3.0122(11) .
Pb3 I7A 3.1306(17) 4_565
Pb3 I7A 3.1872(17) .
Pb3 I2B 3.381(2) 2_646
O1_1 N1_1 1.200(5) .
O2_1 N1_1 1.199(5) .
N1_1 C1_1 1.482(5) .
N2_1 C8_1 1.489(5) .
C1_1 C2_1 1.352(6) .
C1_1 C6_1 1.353(6) .
C2_1 C3_1 1.348(7) .
C3_1 C4_1 1.411(7) .
C4_1 C5_1 1.411(7) .
C4_1 C7_1 1.458(10) .
C5_1 C6_1 1.348(7) .
C7_1 C8_1 1.508(5) .
O1_2 N1_2 1.200(5) .
O2_2 N1_2 1.200(5) .
N1_2 C1_2 1.482(5) .
N2_2 C8_2 1.490(5) .
C1_2 C2_2 1.353(6) .
C1_2 C6_2 1.352(6) .
C2_2 C3_2 1.349(7) .
C3_2 C4_2 1.412(7) .
C4_2 C5_2 1.412(7) .
C4_2 C7_2 1.458(10) .
C5_2 C6_2 1.348(7) .
C7_2 C8_2 1.508(5) .
O1_3 N1_3 1.200(5) .
O2_3 N1_3 1.201(5) .
N1_3 C1_3 1.482(5) .
N2_3 C8_3 1.489(5) .
C1_3 C2_3 1.353(6) .
C1_3 C6_3 1.352(6) .
C2_3 C3_3 1.347(7) .
C3_3 C4_3 1.412(7) .
C4_3 C5_3 1.411(7) .
C4_3 C7_3 1.458(10) .
C5_3 C6_3 1.348(7) .
C7_3 C8_3 1.507(5) .
O1_4 N1_4 1.200(5) .
O2_4 N1_4 1.199(5) .
N1_4 C1_4 1.482(5) .
N2_4 C8_4 1.489(5) .
C1_4 C2_4 1.353(6) .
C1_4 C6_4 1.352(6) .
C2_4 C3_4 1.348(7) .
C3_4 C4_4 1.411(7) .
C4_4 C5_4 1.411(7) .
C4_4 C7_4 1.459(10) .
C5_4 C6_4 1.347(7) .
C7_4 C8_4 1.508(5) .
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
1.0066 -3.9919 -4.9978 0.0079 0.0035 0.3151
-1.0066 3.9919 4.9978 -0.0079 -0.0035 -0.3151
0.0126 -5.0048 1.9973 0.1969 0.0749 -0.0252
-0.0126 5.0048 -1.9973 -0.1969 -0.0749 0.0252
1.0009 0.0013 -0.0006 0.0145 -0.0308 -0.0007
-1.0009 -0.0013 0.0006 -0.0145 0.0308 0.0007
0.0106 -5.0000 -1.0004 0.1223 0.0632 0.1275
-0.0106 5.0000 1.0004 -0.1223 -0.0632 -0.1275
