#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:52:33 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257544 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705286.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_7705286
loop_
_publ_author_name
'Guo, Yuan-Yuan'
'Lightfoot, Philip'
_publ_section_title
;
Structural diversity of lead halide chain compounds, APbX3,
templated by isomeric molecular cations.
;
_journal_issue 36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first 12767
_journal_page_last 12775
_journal_paper_doi 10.1039/d0dt02782k
_journal_volume 49
_journal_year 2020
_chemical_formula_moiety 'Br3 Pb, C9 H8 N'
_chemical_formula_sum 'C9 H8 Br3 N Pb'
_chemical_formula_weight 577.08
_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'
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary dual
_atom_sites_solution_secondary dual
_audit_creation_method SHELXL-2018/3
_audit_update_record
;
2020-08-07 deposited with the CCDC. 2020-08-27 downloaded from the CCDC.
;
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_formula_units_Z 16
_cell_length_a 21.3526(15)
_cell_length_b 7.7783(5)
_cell_length_c 31.1680(2)
_cell_measurement_reflns_used 958
_cell_measurement_temperature 298(2)
_cell_measurement_theta_max 27.5
_cell_measurement_theta_min 2
_cell_volume 5176.6(5)
_computing_molecular_graphics 'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material 'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution 'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature 298(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
;
Rigaku Mercury2 (2x2 bin mode)
;
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71075
_diffrn_reflns_av_R_equivalents 0.1305
_diffrn_reflns_av_unetI/netI 0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 25
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 9
_diffrn_reflns_limit_k_min -9
_diffrn_reflns_limit_l_max 37
_diffrn_reflns_limit_l_min -37
_diffrn_reflns_number 39543
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 24.995
_diffrn_reflns_theta_max 24.995
_diffrn_reflns_theta_min 2.312
_diffrn_source 'Sealed Tube'
_exptl_absorpt_coefficient_mu 22.263
_exptl_absorpt_correction_T_max 1
_exptl_absorpt_correction_T_min 0.399
_exptl_absorpt_correction_type multi-scan
_exptl_crystal_colour Colorless
_exptl_crystal_density_diffrn 2.962
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description Chip
_exptl_crystal_F_000 4096
_exptl_crystal_size_max 0.32
_exptl_crystal_size_mid 0.24
_exptl_crystal_size_min 0.09
_refine_diff_density_max 1.925
_refine_diff_density_min -2.313
_refine_diff_density_rms 0.284
_refine_ls_extinction_coef 0.00124(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref 0.912
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 254
_refine_ls_number_reflns 4554
_refine_ls_number_restraints 24
_refine_ls_restrained_S_all 0.919
_refine_ls_R_factor_all 0.0692
_refine_ls_R_factor_gt 0.0412
_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/[\s^2^(Fo^2^)+(0.0576P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0979
_refine_ls_wR_factor_ref 0.1120
_reflns_Friedel_coverage 0.000
_reflns_number_gt 2807
_reflns_number_total 4554
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file d0dt02782k2.cif
_cod_data_source_block shelx_CCDC4
_cod_depositor_comments
;
The following automatic conversions were performed:
data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 7556 2019-12-06 15:28:31Z antanas
Adding full bibliography for 7705282--7705287.cif.
;
_cod_database_code 7705286
_shelx_shelxl_version_number 2018/3
_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_res_file
;
TITL shelxt_a.res in Pbca
shelx.res
created by SHELXL-2018/3 at 16:11:44 on 10-Jun-2020
REM Old TITL YGPL155
REM SHELXT solution in Pbca: R1 0.173, Rweak 0.001, Alpha 0.022
REM 0.298 for 661 systematic absences, Orientation a'=b, b'=a, c'=-c
REM Formula found by SHELXT: Pb2 Br6 N C2
CELL 0.71075 21.3526 7.7783 31.1680 90.000 90.000 90.000
ZERR 16.000 0.0015 0.0005 0.0002 0.000 0.000 0.000
LATT 1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC PB BR N C H
UNIT 16 48 16 144 128
L.S. 10
BOND
EQIV $1 -x+1/2, y-1/2, z
BIND Pb2 Br5_$1
HTAB
EQIV $2 -x+1/2, y+1/2, z
HTAB N1 Br1_$2
EQIV $3 x, -y+1/2, z+1/2
HTAB N1 Br6_$3
HTAB N1 Br1
HTAB N2 Br3
HTAB N2 Br4
OMIT -3 50
OMIT 1 0 24
ISOR 0.01 0.01 N2 C2 C11 C16
LIST 6
FMAP 2
ACTA
PLAN 10
WGHT 0.057600
EXTI 0.001235
FVAR 0.09022
PB1 1 0.249925 0.481576 0.804180 11.00000 0.04642 0.02360 =
0.03944 0.00170 -0.00066 0.00057
PB2 1 0.250151 -0.345389 0.553878 11.00000 0.04613 0.02284 =
0.03994 0.00047 0.00080 -0.00063
BR1 2 0.296859 0.239000 0.871909 11.00000 0.04958 0.04240 =
0.04302 0.00230 -0.00989 -0.00031
BR2 2 0.140018 0.196446 0.806613 11.00000 0.04218 0.04785 =
0.07053 -0.00539 -0.00494 0.00212
BR4 2 0.204645 -0.088043 0.622379 11.00000 0.05504 0.04427 =
0.04070 0.00373 0.00888 0.00429
BR3 2 0.298353 0.240233 0.738976 11.00000 0.06779 0.04410 =
0.04159 0.00036 0.01423 -0.00241
BR5 2 0.360512 -0.141039 0.553458 11.00000 0.04364 0.04620 =
0.06521 0.00000 0.00153 -0.00356
BR6 2 0.200621 -0.089747 0.488867 11.00000 0.06258 0.04436 =
0.04263 -0.00444 -0.01322 0.00545
N1 3 0.347839 0.612989 0.929387 11.00000 0.05670 0.13137 =
0.06284 -0.03977 0.00613 -0.04715
AFIX 43
H2 5 0.309104 0.584742 0.926657 11.00000 -1.20000
AFIX 0
C1 4 0.364011 0.767353 0.921245 11.00000 0.03587 0.11862 =
0.07142 -0.03904 -0.00684 -0.00881
AFIX 43
H1 5 0.333634 0.844319 0.911848 11.00000 -1.20000
AFIX 0
C2 4 0.390390 0.488930 0.942482 11.00000 0.10812 0.07553 =
0.06822 -0.00232 0.01082 -0.02989
AFIX 43
H3 5 0.377353 0.376494 0.947299 11.00000 -1.20000
AFIX 0
C3 4 0.450426 0.532864 0.948107 11.00000 0.10229 0.05703 =
0.06676 0.00452 -0.01007 -0.02038
AFIX 43
H4 5 0.479055 0.450378 0.957155 11.00000 -1.20000
AFIX 0
C4 4 0.470947 0.703212 0.940470 11.00000 0.05913 0.03713 =
0.04411 0.00253 -0.00396 -0.00704
C5 4 0.531141 0.761027 0.945556 11.00000 0.04940 0.05498 =
0.10813 0.00699 -0.01448 0.01363
AFIX 43
H5 5 0.561943 0.684776 0.954662 11.00000 -1.20000
AFIX 0
C6 4 0.546616 0.925603 0.937664 11.00000 0.03662 0.09944 =
0.09534 0.00100 0.00952 -0.00629
AFIX 43
H6 5 0.587607 0.961977 0.942060 11.00000 -1.20000
AFIX 0
C7 4 0.502742 1.040316 0.923228 11.00000 0.06280 0.06228 =
0.12149 0.01183 0.00115 -0.00544
AFIX 43
H7 5 0.514771 1.152934 0.917525 11.00000 -1.20000
AFIX 0
C8 4 0.443076 0.994452 0.917134 11.00000 0.07872 0.05603 =
0.07912 0.00307 -0.01596 0.01859
AFIX 43
H8 5 0.414008 1.074185 0.907243 11.00000 -1.20000
AFIX 0
C9 4 0.424760 0.824769 0.925814 11.00000 0.04139 0.06887 =
0.04261 -0.00741 -0.00451 0.01103
N2 3 0.354913 -0.068873 0.669962 11.00000 0.07945 0.13111 =
0.07511 -0.03564 -0.01198 0.03909
AFIX 43
H10 5 0.317090 -0.032445 0.667267 11.00000 -1.20000
AFIX 0
C10 4 0.361674 -0.233990 0.682565 11.00000 0.06927 0.14378 =
0.07818 -0.06400 0.01368 -0.03309
AFIX 43
H9 5 0.327937 -0.307207 0.687281 11.00000 -1.20000
AFIX 0
C11 4 0.401706 0.048244 0.660900 11.00000 0.13575 0.10955 =
0.09783 -0.00866 0.00263 0.03203
AFIX 43
H11 5 0.392735 0.158605 0.651204 11.00000 -1.20000
AFIX 0
C12 4 0.458859 -0.003808 0.666627 11.00000 0.09457 0.09060 =
0.08060 -0.01015 0.01649 0.02256
AFIX 43
H12 5 0.491560 0.071585 0.660759 11.00000 -1.20000
AFIX 0
C13 4 0.473139 -0.170645 0.681434 11.00000 0.04847 0.05644 =
0.05983 -0.00622 0.00258 0.00064
C14 4 0.534690 -0.228913 0.687381 11.00000 0.05765 0.06304 =
0.10158 -0.01916 0.01794 -0.00874
AFIX 43
H13 5 0.568215 -0.155386 0.682267 11.00000 -1.20000
AFIX 0
C15 4 0.544991 -0.387254 0.700167 11.00000 0.06687 0.08712 =
0.10227 -0.01792 -0.02421 0.02991
AFIX 43
H14 5 0.585995 -0.424475 0.704029 11.00000 -1.20000
AFIX 0
C16 4 0.494856 -0.503019 0.708237 11.00000 0.10093 0.07691 =
0.09197 0.00527 -0.00221 0.00464
AFIX 43
H15 5 0.503301 -0.613587 0.718007 11.00000 -1.20000
AFIX 0
C17 4 0.438416 -0.456006 0.702148 11.00000 0.07905 0.09864 =
0.08620 -0.01366 0.02971 -0.03224
AFIX 43
H16 5 0.405938 -0.533275 0.706986 11.00000 -1.20000
AFIX 0
C18 4 0.424565 -0.285284 0.687925 11.00000 0.04487 0.07658 =
0.04509 -0.03718 0.00730 0.00493
HKLF 4
REM shelxt_a.res in Pbca
REM wR2 = 0.1120, GooF = S = 0.912, Restrained GooF = 0.919 for all data
REM R1 = 0.0412 for 2807 Fo > 4sig(Fo) and 0.0692 for all 4554 data
REM 254 parameters refined using 24 restraints
END
WGHT 0.0576 0.0000
REM Instructions for potential hydrogen bonds
HTAB N1 Br1_$2
HTAB N1 Br6_$3
HTAB C2 Br1
EQIV $4 -x+1/2, -y, z+1/2
HTAB C2 Br6_$4
HTAB N2 Br4
HTAB C10 Br4_$1
HTAB C11 Br4_$2
REM Highest difference peak 1.925, deepest hole -2.313, 1-sigma level 0.284
Q1 1 0.2518 -0.2855 0.5879 11.00000 0.05 1.92
Q2 1 0.2503 0.4124 0.8382 11.00000 0.05 1.64
Q3 1 0.2517 0.5421 0.8423 11.00000 0.05 1.59
Q4 1 0.2515 -0.2838 0.5190 11.00000 0.05 1.53
Q5 1 0.2494 -0.4460 0.5213 11.00000 0.05 1.50
Q6 1 0.2490 0.4051 0.7701 11.00000 0.05 1.46
Q7 1 0.2910 -0.4882 0.5550 11.00000 0.05 1.40
Q8 1 0.2977 -0.0976 0.6225 11.00000 0.05 1.39
Q9 1 0.6430 -0.3172 0.6946 11.00000 0.05 1.32
Q10 1 0.2513 0.5519 0.7702 11.00000 0.05 1.31
;
_shelx_res_checksum 33301
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 0.24993(2) 0.48158(4) 0.80418(2) 0.03649(15) Uani 1 1 d . . . . .
Pb2 Pb 0.25015(2) -0.34539(4) 0.55388(2) 0.03630(15) Uani 1 1 d . . . . .
Br1 Br 0.29686(5) 0.23900(12) 0.87191(4) 0.0450(3) Uani 1 1 d . . . . .
Br2 Br 0.14002(5) 0.19645(14) 0.80661(4) 0.0535(3) Uani 1 1 d . . . . .
Br4 Br 0.20464(5) -0.08804(13) 0.62238(3) 0.0467(3) Uani 1 1 d . . . . .
Br3 Br 0.29835(6) 0.24023(13) 0.73898(4) 0.0512(3) Uani 1 1 d . . . . .
Br5 Br 0.36051(5) -0.14104(14) 0.55346(4) 0.0517(3) Uani 1 1 d . . . . .
Br6 Br 0.20062(6) -0.08975(13) 0.48887(4) 0.0499(3) Uani 1 1 d . . . . .
N1 N 0.3478(5) 0.6130(19) 0.9294(4) 0.084(4) Uani 1 1 d . . . . .
H2 H 0.309104 0.584742 0.926657 0.100 Uiso 1 1 calc R U . . .
C1 C 0.3640(6) 0.767(2) 0.9212(4) 0.075(4) Uani 1 1 d . . . . .
H1 H 0.333634 0.844319 0.911848 0.090 Uiso 1 1 calc R U . . .
C2 C 0.3904(9) 0.489(2) 0.9425(4) 0.084(4) Uani 1 1 d . U . . .
H3 H 0.377353 0.376494 0.947299 0.101 Uiso 1 1 calc R U . . .
C3 C 0.4504(8) 0.5329(17) 0.9481(4) 0.075(4) Uani 1 1 d . . . . .
H4 H 0.479055 0.450378 0.957155 0.090 Uiso 1 1 calc R U . . .
C4 C 0.4709(5) 0.7032(13) 0.9405(3) 0.047(3) Uani 1 1 d . . . . .
C5 C 0.5311(6) 0.7610(15) 0.9456(5) 0.071(4) Uani 1 1 d . . . . .
H5 H 0.561943 0.684776 0.954662 0.085 Uiso 1 1 calc R U . . .
C6 C 0.5466(6) 0.9256(19) 0.9377(5) 0.077(4) Uani 1 1 d . . . . .
H6 H 0.587607 0.961977 0.942060 0.093 Uiso 1 1 calc R U . . .
C7 C 0.5027(6) 1.0403(18) 0.9232(5) 0.082(4) Uani 1 1 d . . . . .
H7 H 0.514771 1.152934 0.917525 0.099 Uiso 1 1 calc R U . . .
C8 C 0.4431(7) 0.9945(16) 0.9171(4) 0.071(4) Uani 1 1 d . . . . .
H8 H 0.414008 1.074185 0.907243 0.086 Uiso 1 1 calc R U . . .
C9 C 0.4248(5) 0.8248(15) 0.9258(4) 0.051(3) Uani 1 1 d . . . . .
N2 N 0.3549(6) -0.069(2) 0.6700(4) 0.095(4) Uani 1 1 d . U . . .
H10 H 0.317090 -0.032445 0.667267 0.114 Uiso 1 1 calc R U . . .
C10 C 0.3617(7) -0.234(2) 0.6826(5) 0.097(6) Uani 1 1 d . . . . .
H9 H 0.327937 -0.307207 0.687281 0.116 Uiso 1 1 calc R U . . .
C11 C 0.4017(10) 0.048(2) 0.6609(6) 0.114(6) Uani 1 1 d . U . . .
H11 H 0.392735 0.158605 0.651204 0.137 Uiso 1 1 calc R U . . .
C12 C 0.4589(8) -0.004(2) 0.6666(5) 0.089(5) Uani 1 1 d . . . . .
H12 H 0.491560 0.071585 0.660759 0.106 Uiso 1 1 calc R U . . .
C13 C 0.4731(6) -0.1706(15) 0.6814(4) 0.055(3) Uani 1 1 d . . . . .
C14 C 0.5347(6) -0.2289(17) 0.6874(5) 0.074(4) Uani 1 1 d . . . . .
H13 H 0.568215 -0.155386 0.682267 0.089 Uiso 1 1 calc R U . . .
C15 C 0.5450(7) -0.387(2) 0.7002(5) 0.085(5) Uani 1 1 d . . . . .
H14 H 0.585995 -0.424475 0.704029 0.103 Uiso 1 1 calc R U . . .
C16 C 0.4949(9) -0.503(2) 0.7082(5) 0.090(5) Uani 1 1 d . U . . .
H15 H 0.503301 -0.613587 0.718007 0.108 Uiso 1 1 calc R U . . .
C17 C 0.4384(7) -0.456(2) 0.7021(5) 0.088(5) Uani 1 1 d . . . . .
H16 H 0.405938 -0.533275 0.706986 0.106 Uiso 1 1 calc R U . . .
C18 C 0.4246(5) -0.2853(17) 0.6879(4) 0.056(3) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0464(3) 0.0236(2) 0.0394(3) 0.00170(15) -0.00066(16) 0.00057(15)
Pb2 0.0461(3) 0.0228(2) 0.0399(3) 0.00047(14) 0.00080(18) -0.00063(15)
Br1 0.0496(6) 0.0424(6) 0.0430(7) 0.0023(4) -0.0099(5) -0.0003(4)
Br2 0.0422(6) 0.0479(6) 0.0705(8) -0.0054(6) -0.0049(6) 0.0021(5)
Br4 0.0550(7) 0.0443(6) 0.0407(6) 0.0037(5) 0.0089(5) 0.0043(5)
Br3 0.0678(8) 0.0441(6) 0.0416(7) 0.0004(5) 0.0142(6) -0.0024(5)
Br5 0.0436(6) 0.0462(6) 0.0652(8) 0.0000(5) 0.0015(6) -0.0036(5)
Br6 0.0626(7) 0.0444(6) 0.0426(7) -0.0044(5) -0.0132(6) 0.0054(5)
N1 0.057(7) 0.131(11) 0.063(8) -0.040(8) 0.006(6) -0.047(8)
C1 0.036(7) 0.119(13) 0.071(10) -0.039(9) -0.007(6) -0.009(7)
C2 0.108(8) 0.076(7) 0.068(7) -0.002(6) 0.011(7) -0.030(7)
C3 0.102(12) 0.057(8) 0.067(9) 0.005(7) -0.010(8) -0.020(8)
C4 0.059(7) 0.037(5) 0.044(7) 0.003(5) -0.004(5) -0.007(5)
C5 0.049(8) 0.055(8) 0.108(12) 0.007(7) -0.014(8) 0.014(6)
C6 0.037(7) 0.099(11) 0.095(11) 0.001(9) 0.010(7) -0.006(7)
C7 0.063(9) 0.062(9) 0.121(14) 0.012(9) 0.001(9) -0.005(7)
C8 0.079(10) 0.056(8) 0.079(11) 0.003(7) -0.016(8) 0.019(7)
C9 0.041(6) 0.069(8) 0.043(7) -0.007(6) -0.005(5) 0.011(6)
N2 0.079(7) 0.131(8) 0.075(7) -0.036(7) -0.012(6) 0.039(7)
C10 0.069(10) 0.144(16) 0.078(11) -0.064(11) 0.014(8) -0.033(10)
C11 0.136(10) 0.110(9) 0.098(9) -0.009(8) 0.003(8) 0.032(8)
C12 0.095(12) 0.091(11) 0.081(11) -0.010(9) 0.016(9) 0.023(9)
C13 0.048(7) 0.056(8) 0.060(8) -0.006(6) 0.003(6) 0.001(6)
C14 0.058(8) 0.063(8) 0.102(12) -0.019(8) 0.018(8) -0.009(7)
C15 0.067(10) 0.087(11) 0.102(12) -0.018(10) -0.024(9) 0.030(8)
C16 0.101(9) 0.077(8) 0.092(8) 0.005(7) -0.002(7) 0.005(7)
C17 0.079(12) 0.099(12) 0.086(11) -0.014(10) 0.030(9) -0.032(10)
C18 0.045(7) 0.077(8) 0.045(7) -0.037(7) 0.007(5) 0.005(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
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'
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
_geom_angle_publ_flag
Br2 Pb1 Br3 95.80(3) 8_665 . ?
Br2 Pb1 Br1 94.23(3) 8_665 . ?
Br3 Pb1 Br1 88.14(3) . . ?
Br2 Pb1 Br3 84.86(3) 8_665 8_665 ?
Br3 Pb1 Br3 94.55(4) . 8_665 ?
Br1 Pb1 Br3 177.23(3) . 8_665 ?
Br2 Pb1 Br1 82.50(3) 8_665 8_665 ?
Br3 Pb1 Br1 178.30(3) . 8_665 ?
Br1 Pb1 Br1 92.00(3) . 8_665 ?
Br3 Pb1 Br1 85.29(3) 8_665 8_665 ?
Br2 Pb1 Br2 171.54(4) 8_665 . ?
Br3 Pb1 Br2 80.45(3) . . ?
Br1 Pb1 Br2 78.14(3) . . ?
Br3 Pb1 Br2 102.93(3) 8_665 . ?
Br1 Pb1 Br2 101.24(3) 8_665 . ?
Br5 Pb2 Br6 93.52(3) . 8_655 ?
Br5 Pb2 Br4 95.05(3) . 8_655 ?
Br6 Pb2 Br4 88.23(3) 8_655 8_655 ?
Br5 Pb2 Br6 85.37(3) . . ?
Br6 Pb2 Br6 95.01(4) 8_655 . ?
Br4 Pb2 Br6 176.71(3) 8_655 . ?
Br5 Pb2 Br4 84.34(3) . . ?
Br6 Pb2 Br4 177.64(3) 8_655 . ?
Br4 Pb2 Br4 90.97(3) 8_655 . ?
Br6 Pb2 Br4 85.81(3) . . ?
Br5 Pb2 Br5 169.77(3) . 8_655 ?
Br6 Pb2 Br5 78.73(3) 8_655 8_655 ?
Br4 Pb2 Br5 78.18(3) 8_655 8_655 ?
Br6 Pb2 Br5 101.83(3) . 8_655 ?
Br4 Pb2 Br5 103.28(3) . 8_655 ?
Pb1 Br1 Pb1 79.53(3) . 8_655 ?
Pb1 Br2 Pb1 78.77(3) 8_655 . ?
Pb2 Br4 Pb2 79.33(3) 8_665 . ?
Pb1 Br3 Pb1 80.90(3) . 8_655 ?
Pb2 Br6 Pb2 80.81(3) 8_665 . ?
C1 N1 C2 122.4(12) . . ?
N1 C1 C9 122.6(14) . . ?
C3 C2 N1 119.2(14) . . ?
C2 C3 C4 120.9(15) . . ?
C5 C4 C3 125.3(12) . . ?
C5 C4 C9 117.6(10) . . ?
C3 C4 C9 117.1(12) . . ?
C6 C5 C4 121.4(12) . . ?
C5 C6 C7 120.8(13) . . ?
C8 C7 C6 121.7(13) . . ?
C7 C8 C9 119.3(12) . . ?
C1 C9 C8 123.2(12) . . ?
C1 C9 C4 117.7(12) . . ?
C8 C9 C4 119.2(11) . . ?
C10 N2 C11 127.5(14) . . ?
N2 C10 C18 113.9(14) . . ?
C12 C11 N2 116.5(17) . . ?
C11 C12 C13 122.4(17) . . ?
C18 C13 C14 118.4(12) . . ?
C18 C13 C12 118.6(13) . . ?
C14 C13 C12 122.9(13) . . ?
C15 C14 C13 120.0(13) . . ?
C14 C15 C16 121.5(14) . . ?
C17 C16 C15 120.3(15) . . ?
C16 C17 C18 120.5(14) . . ?
C13 C18 C10 121.0(14) . . ?
C13 C18 C17 119.3(12) . . ?
C10 C18 C17 119.7(14) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br2 2.8848(12) 8_665 ?
Pb1 Br3 2.9535(11) . ?
Pb1 Br1 3.0034(11) . ?
Pb1 Br3 3.0399(11) 8_665 ?
Pb1 Br1 3.0763(11) 8_665 ?
Pb1 Br2 3.2299(12) . ?
Pb2 Br5 2.8425(11) . ?
Pb2 Br6 2.9703(11) 8_655 ?
Pb2 Br4 3.0087(11) 8_655 ?
Pb2 Br6 3.0295(11) . ?
Pb2 Br4 3.0837(11) . ?
Pb2 Br5 3.2973(12) 8_655 ?
N1 C1 1.275(17) . ?
N1 C2 1.387(18) . ?
C1 C9 1.379(15) . ?
C2 C3 1.34(2) . ?
C3 C4 1.416(16) . ?
C4 C5 1.371(16) . ?
C4 C9 1.441(15) . ?
C5 C6 1.345(17) . ?
C6 C7 1.370(18) . ?
C7 C8 1.337(17) . ?
C8 C9 1.403(17) . ?
N2 C10 1.351(18) . ?
N2 C11 1.38(2) . ?
C10 C18 1.411(18) . ?
C11 C12 1.30(2) . ?
C12 C13 1.411(18) . ?
C13 C18 1.383(16) . ?
C13 C14 1.403(17) . ?
C14 C15 1.313(18) . ?
C15 C16 1.42(2) . ?
C16 C17 1.274(19) . ?
C17 C18 1.431(18) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H2 Br1 0.86 3.08 3.704(13) 131.5 8_665 yes
N1 H2 Br6 0.86 3.02 3.654(11) 132.1 7_566 yes
N1 H2 Br1 0.86 3.20 3.586(11) 110.3 . yes
N2 H10 Br3 0.86 3.11 3.445(12) 106.0 . yes
N2 H10 Br4 0.86 2.81 3.538(13) 143.1 . yes