#------------------------------------------------------------------------------
#$Date: 2017-10-17 04:43:32 +0300 (Tue, 17 Oct 2017) $
#$Revision: 202041 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/76/1547683.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_1547683
loop_
_publ_author_name
'Lin, Haoran'
'Zhou, Chenkun'
'Tian, Yu'
'Besara, Tiglet'
'Neu, Jennifer'
'Siegrist, Theo'
'Zhou, Yan'
'Bullock, James'
'Schanze, Kirk'
'Ming, Wenmei'
'Du, Mao Hua'
'Ma, Biwu'
_publ_section_title
;
 Bulk Assembly of Organic Metal Halide Nanotubes
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03675B
_journal_year                    2017
_chemical_formula_moiety         'C18 H36 Br7 N12 Pb2'
_chemical_formula_sum            'C18 H36 Br7 N12 Pb2'
_chemical_formula_weight         1394.29
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_update_record
;
2017-08-01 deposited with the CCDC.
2017-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   24.5149(6)
_cell_length_b                   24.5149(6)
_cell_length_c                   9.7646(2)
_cell_measurement_reflns_used    3199
_cell_measurement_temperature    100
_cell_measurement_theta_max      25
_cell_measurement_theta_min      4
_cell_volume                     5082.1(2)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.094
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            69463
_diffrn_reflns_theta_full        25.066
_diffrn_reflns_theta_max         25.066
_diffrn_reflns_theta_min         2.834
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.213
_exptl_absorpt_correction_T_max  0.46
_exptl_absorpt_correction_T_min  0.35
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            transparent
_exptl_crystal_density_diffrn    2.733
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3822
_exptl_crystal_size_max          0.205
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.043
_refine_diff_density_max         5.46
_refine_diff_density_min         -7.63
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0634
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3186
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0518
_refine_ls_shift/su_max          0.0005106
_refine_ls_shift/su_mean         0.0000221
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 80.1 99.9 32.4 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0729
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0728
_reflns_limit_h_max              0
_reflns_limit_h_min              -24
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              11
_reflns_limit_l_min              0
_reflns_number_gt                2797
_reflns_number_total             3199
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0593
_oxford_refine_ls_scale          0.21171(10)
_oxford_reflns_number_all        3187
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_cod_data_source_file            c7sc03675b2.cif
_cod_data_source_block           hmtaPbCl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Other' changed to 'other'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P 63/m '
_cod_database_code               1547683
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+y,-x,z
x-y,x,-z
-y,x-y,z
y,-x+y,-z
-x,-y,z+1/2
x,y,-z+1/2
y,-x+y,z+1/2
-y,x-y,-z+1/2
-x+y,-x,-z+1/2
x-y,x,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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Pb1 Pb 0.71799(3) 0.65688(3) 0.2500 0.0234 1.0000 Uani S T
Pb2 Pb 0.65448(5) 0.78652(5) 0.2500 0.0482 1.0000 Uani S T
Br1 Br 0.62146(7) 0.52648(7) 0.2500 0.0228 1.0000 Uani S T
Br2 Br 0.51820(11) 0.73401(10) 0.2500 0.0452 1.0000 Uani S T
Br3 Br 0.64245(6) 0.68525(6) 0.44770(11) 0.0290 1.0000 Uani . .
Br4 Br 0.78504(5) 0.65075(5) 0.51749(13) 0.0319 1.0000 Uani . .
Br5 Br 0.79180(9) 0.80509(8) 0.2500 0.0377 1.0000 Uani S T
N11 N 0.5585(4) 0.4744(4) 0.6254(9) 0.0198 1.0000 Uani D .
N12 N 0.5814(6) 0.5689(6) 0.7500 0.0195 1.0000 Uani DS T
N13 N 0.6569(6) 0.5330(7) 0.7500 0.0248 1.0000 Uani DS T
C14 C 0.5519(5) 0.5301(5) 0.6270(9) 0.0171 1.0000 Uani D .
C15 C 0.6487(8) 0.5900(8) 0.7500 0.0259 1.0000 Uani DS T
C16 C 0.6251(5) 0.4941(6) 0.6245(11) 0.0273 1.0000 Uani D .
C17 C 0.5302(8) 0.4370(7) 0.7500 0.0255 1.0000 Uani DS T
N21 N 0.4580(4) 0.6748(4) 0.6261(10) 0.0251 1.0000 Uani D .
N22 N 0.5412(7) 0.7645(7) 0.7500 0.0237 1.0000 Uani DS T
N23 N 0.5360(7) 0.6624(6) 0.7500 0.0238 1.0000 Uani DS T
C24 C 0.5001(6) 0.7437(5) 0.6272(11) 0.0282 1.0000 Uani D .
C25 C 0.5793(7) 0.7339(7) 0.7500 0.0217 1.0000 Uani DS T
C26 C 0.4948(5) 0.6443(5) 0.6243(11) 0.0243 1.0000 Uani D .
C27 C 0.4194(8) 0.6568(8) 0.7500 0.0290 1.0000 Uani DS T
N31 N 0.9767(5) 0.8483(5) 0.3739(13) 0.0478 1.0000 Uani D .
N32 N 1.0524(8) 0.8302(9) 0.2500 0.0439 1.0000 Uani DS T
N33 N 0.9414(8) 0.7513(7) 0.2500 0.0350 1.0000 Uani DS T
C34 C 0.9320(6) 0.7802(6) 0.3724(12) 0.0393 1.0000 Uani D .
C35 C 1.0041(10) 0.7624(9) 0.2500 0.0393 1.0000 Uani DS T
C36 C 1.0407(6) 0.8578(7) 0.3732(14) 0.0484 1.0000 Uani D .
C37 C 0.9703(11) 0.8783(10) 0.2500 0.0521 1.0000 Uani DS T
H142 H 0.5706(17) 0.5544(13) 0.544(2) 0.022(2) 1.0000 Uiso D .
H141 H 0.5075(11) 0.5167(14) 0.628(4) 0.022(2) 1.0000 Uiso D .
H152 H 0.6681(11) 0.6150(10) 0.8313(15) 0.0340(14) 1.0000 Uiso D .
H162 H 0.6441(14) 0.5186(16) 0.541(3) 0.035(2) 1.0000 Uiso D .
H161 H 0.6298(15) 0.4572(13) 0.625(4) 0.035(2) 1.0000 Uiso D .
H171 H 0.537(2) 0.4015(15) 0.7500 0.033(2) 1.0000 Uiso DS .
H172 H 0.4853(12) 0.422(2) 0.7500 0.033(2) 1.0000 Uiso DS .
H242 H 0.4748(14) 0.7640(14) 0.627(4) 0.035(2) 1.0000 Uiso D .
H241 H 0.5257(14) 0.7558(15) 0.544(3) 0.035(2) 1.0000 Uiso D .
H252 H 0.6056(9) 0.7464(11) 0.8312(15) 0.0280(14) 1.0000 Uiso D .
H262 H 0.5208(14) 0.6572(18) 0.541(3) 0.031(2) 1.0000 Uiso D .
H261 H 0.4671(14) 0.5992(11) 0.624(4) 0.031(2) 1.0000 Uiso D .
H272 H 0.3942(18) 0.677(2) 0.7500 0.037(2) 1.0000 Uiso DS .
H271 H 0.3920(18) 0.6116(13) 0.7500 0.037(2) 1.0000 Uiso DS .
H341 H 0.9390(19) 0.7617(14) 0.455(3) 0.049(2) 1.0000 Uiso D .
H342 H 0.8895(11) 0.7732(16) 0.373(4) 0.049(2) 1.0000 Uiso D .
H352 H 1.0097(14) 0.7431(12) 0.3313(15) 0.0480(14) 1.0000 Uiso D .
H361 H 1.0707(14) 0.9025(12) 0.375(4) 0.060(2) 1.0000 Uiso D .
H362 H 1.0462(18) 0.839(2) 0.456(3) 0.060(2) 1.0000 Uiso D .
H372 H 1.002(2) 0.9223(13) 0.2500 0.067(2) 1.0000 Uiso DS .
H371 H 0.929(2) 0.874(3) 0.2500 0.067(2) 1.0000 Uiso DS .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Pb -3.3944 10.1111 31.0617 0.6902 13.0637 2.3576 18.4420 8.6180 5.9696 47.2579
13.4118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br3 8_555 Pb1 Br4 8_555 82.73(3) yes
Br3 8_555 Pb1 Br1 . 89.86(4) yes
Br4 8_555 Pb1 Br1 . 96.12(3) yes
Br3 8_555 Pb1 Br3 . 80.50(5) yes
Br4 8_555 Pb1 Br3 . 162.17(4) yes
Br1 . Pb1 Br3 . 89.86(4) yes
Br3 8_555 Pb1 Br4 . 162.17(4) yes
Br4 8_555 Pb1 Br4 . 113.15(5) yes
Br1 . Pb1 Br4 . 96.12(3) yes
Br3 . Pb1 Br4 . 82.73(3) yes
Br4 9_564 Pb2 Br4 6_566 97.57(5) yes
Br4 9_564 Pb2 Br3 8_555 91.48(3) yes
Br4 6_566 Pb2 Br3 8_555 168.82(5) yes
Br4 9_564 Pb2 Br2 . 83.55(4) yes
Br4 6_566 Pb2 Br2 . 83.55(4) yes
Br3 8_555 Pb2 Br2 . 91.01(5) yes
Br4 9_564 Pb2 Br3 . 168.82(5) yes
Br4 6_566 Pb2 Br3 . 91.48(3) yes
Br3 8_555 Pb2 Br3 . 78.82(5) yes
Br2 . Pb2 Br3 . 91.01(5) yes
Br4 9_564 Pb2 Br5 . 106.24(4) yes
Br4 6_566 Pb2 Br5 . 106.24(4) yes
Br3 8_555 Pb2 Br5 . 77.25(4) yes
Br2 . Pb2 Br5 . 164.70(6) yes
Br3 . Pb2 Br5 . 77.25(4) yes
Pb1 . Br3 Pb2 . 87.79(3) yes
Pb2 4_656 Br4 Pb1 . 171.25(5) yes
C14 . N11 C16 . 108.8(8) yes
C14 . N11 C17 . 109.6(9) yes
C16 . N11 C17 . 108.4(10) yes
C14 8_556 N12 C14 . 108.9(11) yes
C14 8_556 N12 C15 . 109.4(8) yes
C14 . N12 C15 . 109.4(8) yes
C16 8_556 N13 C15 . 108.7(8) yes
C16 8_556 N13 C16 . 108.7(13) yes
C15 . N13 C16 . 108.7(8) yes
N12 . C14 N11 . 111.3(9) yes
N12 . C14 H142 . 110.8(17) no
N11 . C14 H142 . 109.0(17) no
N12 . C14 H141 . 108.2(17) no
N11 . C14 H141 . 108.4(17) no
H142 . C14 H141 . 109.0(17) no
N13 . C15 N12 . 108.7(12) yes
N13 . C15 H152 8_556 109.6(11) no
N12 . C15 H152 8_556 109.6(11) no
N13 . C15 H152 . 109.6(11) no
N12 . C15 H152 . 109.6(11) no
H152 8_556 C15 H152 . 109.8(18) no
N13 . C16 N11 . 110.1(9) yes
N13 . C16 H162 . 110.4(17) no
N11 . C16 H162 . 108.6(17) no
N13 . C16 H161 . 109.0(17) no
N11 . C16 H161 . 109.1(17) no
H162 . C16 H161 . 109.5(17) no
N11 . C17 N11 8_556 111.6(12) yes
N11 . C17 H171 . 108.6(11) no
N11 8_556 C17 H171 . 108.6(11) no
N11 . C17 H172 . 109.3(11) no
N11 8_556 C17 H172 . 109.3(11) no
H171 . C17 H172 . 109.4(18) no
C24 . N21 C26 . 109.5(9) yes
C24 . N21 C27 . 108.5(10) yes
C26 . N21 C27 . 109.5(10) yes
C24 8_556 N22 C24 . 107.9(12) yes
C24 8_556 N22 C25 . 108.7(8) yes
C24 . N22 C25 . 108.7(8) yes
C26 8_556 N23 C25 . 108.4(8) yes
C26 8_556 N23 C26 . 108.9(12) yes
C25 . N23 C26 . 108.4(8) yes
N22 . C24 N21 . 111.5(10) yes
N22 . C24 H242 . 108.8(17) no
N21 . C24 H242 . 109.0(17) no
N22 . C24 H241 . 110.2(17) no
N21 . C24 H241 . 108.5(17) no
H242 . C24 H241 . 108.8(18) no
N23 . C25 N22 . 109.5(12) yes
N23 . C25 H252 8_556 109.5(11) no
N22 . C25 H252 8_556 109.3(11) no
N23 . C25 H252 . 109.5(11) no
N22 . C25 H252 . 109.3(11) no
H252 8_556 C25 H252 . 109.7(18) no
N23 . C26 N21 . 109.9(9) yes
N23 . C26 H262 . 110.3(17) no
N21 . C26 H262 . 108.6(17) no
N23 . C26 H261 . 109.0(17) no
N21 . C26 H261 . 109.3(17) no
H262 . C26 H261 . 109.7(17) no
N21 . C27 N21 8_556 111.8(13) yes
N21 . C27 H272 . 109.1(11) no
N21 8_556 C27 H272 . 109.1(11) no
N21 . C27 H271 . 108.7(11) no
N21 8_556 C27 H271 . 108.7(11) no
H272 . C27 H271 . 109.4(18) no
C34 . N31 C36 . 108.2(11) yes
C34 . N31 C37 . 110.8(12) yes
C36 . N31 C37 . 106.9(13) yes
C36 8_555 N32 C35 . 106.5(10) yes
C36 8_555 N32 C36 . 109.1(16) yes
C35 . N32 C36 . 106.5(10) yes
C34 8_555 N33 C34 . 109.3(14) yes
C34 8_555 N33 C35 . 108.9(10) yes
C34 . N33 C35 . 108.9(10) yes
N31 . C34 N33 . 110.4(11) yes
N31 . C34 H341 . 108.3(17) no
N33 . C34 H341 . 109.7(17) no
N31 . C34 H342 . 109.1(17) no
N33 . C34 H342 . 109.7(17) no
H341 . C34 H342 . 109.6(18) no
N32 . C35 N33 . 113.4(15) yes
N32 . C35 H352 8_555 108.5(11) no
N33 . C35 H352 8_555 108.2(11) no
N32 . C35 H352 . 108.5(11) no
N33 . C35 H352 . 108.2(11) no
H352 8_555 C35 H352 . 110.0(18) no
N32 . C36 N31 . 111.7(11) yes
N32 . C36 H361 . 108.6(17) no
N31 . C36 H361 . 109.1(17) no
N32 . C36 H362 . 110.3(17) no
N31 . C36 H362 . 108.2(17) no
H361 . C36 H362 . 108.9(18) no
N31 . C37 N31 8_555 111.4(15) yes
N31 . C37 H372 . 109.2(11) no
N31 8_555 C37 H372 . 109.2(11) no
N31 . C37 H371 . 108.6(11) no
N31 8_555 C37 H371 . 108.6(11) no
H372 . C37 H371 . 109.7(18) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pb1 Br3 8_555 2.9878(12) yes
Pb1 Br4 8_555 3.1295(13) yes
Pb1 Br1 . 2.8731(17) yes
Pb1 Br3 . 2.9878(12) yes
Pb1 Br4 . 3.1295(13) yes
Pb2 Br4 9_564 3.0182(14) yes
Pb2 Br4 6_566 3.0182(14) yes
Pb2 Br3 8_555 3.0406(14) yes
Pb2 Br2 . 2.919(3) yes
Pb2 Br3 . 3.0406(14) yes
Pb2 Br5 . 3.164(2) yes
N11 C14 . 1.456(13) yes
N11 C16 . 1.452(14) yes
N11 C17 . 1.471(12) yes
N12 C14 8_556 1.477(12) yes
N12 C14 . 1.477(12) yes
N12 C15 . 1.46(2) yes
N13 C16 8_556 1.509(13) yes
N13 C15 . 1.51(2) yes
N13 C16 . 1.509(13) yes
C14 H142 . 0.976(19) no
C14 H141 . 0.966(19) no
C15 H152 8_556 0.970(14) no
C15 H152 . 0.970(14) no
C16 H162 . 0.977(19) no
C16 H161 . 0.966(19) no
C17 H171 . 0.97(2) no
C17 H172 . 0.97(2) no
N21 C24 . 1.474(14) yes
N21 C26 . 1.433(13) yes
N21 C27 . 1.461(13) yes
N22 C24 8_556 1.483(13) yes
N22 C24 . 1.483(13) yes
N22 C25 . 1.462(19) yes
N23 C26 8_556 1.508(13) yes
N23 C25 . 1.528(19) yes
N23 C26 . 1.508(13) yes
C24 H242 . 0.971(19) no
C24 H241 . 0.977(19) no
C25 H252 8_556 0.970(14) no
C25 H252 . 0.970(14) no
C26 H262 . 0.982(19) no
C26 H261 . 0.965(19) no
C27 H272 . 0.97(2) no
C27 H271 . 0.97(2) no
N31 C34 . 1.469(16) yes
N31 C36 . 1.466(16) yes
N31 C37 . 1.465(16) yes
N32 C36 8_555 1.477(16) yes
N32 C35 . 1.48(3) yes
N32 C36 . 1.477(16) yes
N33 C34 8_555 1.466(15) yes
N33 C34 . 1.466(15) yes
N33 C35 . 1.42(2) yes
C34 H341 . 0.981(19) no
C34 H342 . 0.967(19) no
C35 H352 8_555 0.969(14) no
C35 H352 . 0.969(14) no
C36 H361 . 0.967(19) no
C36 H362 . 0.975(19) no
C37 H372 . 0.97(2) no
C37 H371 . 0.97(2) no
