#------------------------------------------------------------------------------
#$Date: 2019-04-03 04:58:53 +0300 (Wed, 03 Apr 2019) $
#$Revision: 214462 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/25/7232563.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_7232563
loop_
_publ_author_name
'Huang, Yuan'
'Yang, Jie'
'Li, Zi-jian'
'Qian, Kun'
'Sao, Feng'
_publ_section_title
;
 High-temperature ferroelastic phase transition in a perovskite-like
 complex: [Et4N]2[PbBr3]2
;
_journal_issue                   18
_journal_name_full               'RSC Advances'
_journal_page_first              10364
_journal_paper_doi               10.1039/C9RA00804G
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C16 H40 Br6 N2 Pb2'
_chemical_formula_weight         1154.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-09-11 deposited with the CCDC.    2019-03-26 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.712(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.892(3)
_cell_length_b                   35.883(10)
_cell_length_c                   7.838(2)
_cell_measurement_reflns_used    4543
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.54
_cell_measurement_theta_min      2.27
_cell_volume                     3010.0(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0762
_diffrn_reflns_av_sigmaI/netI    0.0735
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            20649
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.13
_exptl_absorpt_coefficient_mu    19.142
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.1873
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.547
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       strip
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.889
_refine_diff_density_min         -6.167
_refine_diff_density_rms         0.471
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5305
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1002
_refine_ls_R_factor_gt           0.0640
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0690P)²+29.1059P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                3680
_reflns_number_total             5305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ra00804g2.cif
_cod_data_source_block           hy-pb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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.

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' 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_cell_volume        3010.1(14)
_cod_original_sg_symbol_H-M      'P2(1)/c  '
_cod_database_code               7232563
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pb1 Pb 0.49287(2) 0.250001(6) 0.91039(3) 0.02545(6) Uani 1 1 d .
Br2 Br 0.49419(6) 0.185273(16) 1.14244(8) 0.03362(18) Uani 1 1 d .
Br1 Br 0.30887(7) 0.21764(2) 0.61986(10) 0.0465(2) Uani 1 1 d .
Br3 Br 0.68044(7) 0.21711(2) 0.71512(10) 0.0564(2) Uani 1 1 d .
Pb2 Pb 0.0000 0.0000 0.5000 0.02753(9) Uani 1 2 d S
Pb3 Pb 0.0000 0.0000 0.0000 0.02692(9) Uani 1 2 d S
Br5 Br -0.20654(6) 0.022121(18) 0.19546(10) 0.0402(2) Uani 1 1 d .
Br6 Br 0.15395(6) 0.047056(19) 0.29009(9) 0.0409(2) Uani 1 1 d .
Br4 Br -0.04717(7) 0.061778(18) 0.73672(9) 0.0423(2) Uani 1 1 d .
N1 N 0.4328(4) 0.08386(12) 0.7881(6) 0.0240(14) Uani 1 1 d .
C5 C 0.4992(6) 0.08368(18) 0.9726(8) 0.037(2) Uani 1 1 d .
H5A H 0.4878 0.1078 1.0237 0.044 Uiso 1 1 calc R
H5B H 0.5879 0.0804 0.9749 0.044 Uiso 1 1 calc R
C7 C 0.2920(6) 0.08662(17) 0.7726(9) 0.037(2) Uani 1 1 d .
H7A H 0.2616 0.0639 0.8176 0.044 Uiso 1 1 calc R
H7B H 0.2540 0.0885 0.6508 0.044 Uiso 1 1 calc R
C3 C 0.4554(5) 0.04770(15) 0.6947(8) 0.0285(17) Uani 1 1 d .
H3A H 0.4229 0.0271 0.7533 0.034 Uiso 1 1 calc R
H3B H 0.4073 0.0488 0.5775 0.034 Uiso 1 1 calc R
C1 C 0.4817(6) 0.11779(16) 0.7003(8) 0.037(2) Uani 1 1 d .
H1A H 0.4626 0.1402 0.7597 0.045 Uiso 1 1 calc R
H1B H 0.5719 0.1159 0.7156 0.045 Uiso 1 1 calc R
C8 C 0.2509(6) 0.1199(2) 0.8695(11) 0.061(3) Uani 1 1 d .
H8A H 0.2949 0.1197 0.9876 0.092 Uiso 1 1 calc R
H8B H 0.1626 0.1184 0.8677 0.092 Uiso 1 1 calc R
H8C H 0.2691 0.1426 0.8142 0.092 Uiso 1 1 calc R
C4 C 0.5874(7) 0.0391(2) 0.6837(11) 0.055(3) Uani 1 1 d .
H4A H 0.6202 0.0587 0.6215 0.082 Uiso 1 1 calc R
H4B H 0.5908 0.0159 0.6239 0.082 Uiso 1 1 calc R
H4C H 0.6363 0.0373 0.7987 0.082 Uiso 1 1 calc R
C6 C 0.4558(7) 0.0537(2) 1.0829(10) 0.063(3) Uani 1 1 d .
H6A H 0.3722 0.0590 1.0981 0.094 Uiso 1 1 calc R
H6B H 0.5103 0.0529 1.1942 0.094 Uiso 1 1 calc R
H6C H 0.4574 0.0300 1.0264 0.094 Uiso 1 1 calc R
C2 C 0.4290(8) 0.1221(2) 0.5077(9) 0.058(3) Uani 1 1 d .
H2A H 0.4373 0.0990 0.4494 0.088 Uiso 1 1 calc R
H2B H 0.4742 0.1413 0.4601 0.088 Uiso 1 1 calc R
H2C H 0.3423 0.1288 0.4921 0.088 Uiso 1 1 calc R
N2 N 0.9284(4) 0.16209(13) 1.2864(6) 0.0283(15) Uani 1 1 d .
C9 C 0.8445(7) 0.1658(2) 1.1156(9) 0.050(2) Uani 1 1 d .
H9A H 0.8628 0.1893 1.0642 0.060 Uiso 1 1 calc R
H9B H 0.7591 0.1671 1.1346 0.060 Uiso 1 1 calc R
C15 C 0.8966(6) 0.1276(2) 1.3767(10) 0.057(2) Uani 1 1 d .
H15A H 0.9118 0.1062 1.3080 0.068 Uiso 1 1 calc R
H15B H 0.9534 0.1259 1.4875 0.068 Uiso 1 1 calc R
C16 C 0.7668(6) 0.1251(2) 1.4089(11) 0.064(3) Uani 1 1 d .
H16A H 0.7442 0.1483 1.4562 0.095 Uiso 1 1 calc R
H16B H 0.7615 0.1054 1.4898 0.095 Uiso 1 1 calc R
H16C H 0.7107 0.1201 1.3016 0.095 Uiso 1 1 calc R
C11 C 1.0619(6) 0.1603(2) 1.2613(11) 0.054(3) Uani 1 1 d .
H11A H 1.1140 0.1584 1.3757 0.064 Uiso 1 1 calc R
H11B H 1.0716 0.1371 1.2013 0.064 Uiso 1 1 calc R
C12 C 1.1132(7) 0.1893(2) 1.1709(10) 0.062(3) Uani 1 1 d .
H12A H 1.0748 0.1887 1.0504 0.093 Uiso 1 1 calc R
H12B H 1.2017 0.1856 1.1820 0.093 Uiso 1 1 calc R
H12C H 1.0977 0.2130 1.2196 0.093 Uiso 1 1 calc R
C13 C 0.9043(7) 0.1952(2) 1.3900(11) 0.079(3) Uani 1 1 d .
H13A H 0.8154 0.1966 1.3906 0.095 Uiso 1 1 calc R
H13B H 0.9273 0.2175 1.3332 0.095 Uiso 1 1 calc R
C10 C 0.8524(9) 0.1354(3) 0.9882(12) 0.105(4) Uani 1 1 d .
H10A H 0.9385 0.1298 0.9880 0.158 Uiso 1 1 calc R
H10B H 0.8126 0.1434 0.8743 0.158 Uiso 1 1 calc R
H10C H 0.8111 0.1136 1.0202 0.158 Uiso 1 1 calc R
C14 C 0.9753(9) 0.1950(4) 1.5787(12) 0.132(5) Uani 1 1 d .
H14A H 0.9629 0.1715 1.6314 0.198 Uiso 1 1 calc R
H14B H 0.9446 0.2147 1.6421 0.198 Uiso 1 1 calc R
H14C H 1.0629 0.1986 1.5803 0.198 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'
N N 0.0061 0.0033 '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'
Pb Pb -3.3944 10.1111 '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
Br2 Pb1 Br1 95.17(3) . .
Br2 Pb1 Br3 94.52(3) . .
Br1 Pb1 Br3 83.23(3) . .
Br2 Pb1 Br1 84.04(3) . 4_566
Br1 Pb1 Br1 98.29(3) . 4_566
Br3 Pb1 Br1 177.98(2) . 4_566
Br2 Pb1 Br3 84.08(3) . 4_566
Br1 Pb1 Br3 179.02(2) . 4_566
Br3 Pb1 Br3 97.45(3) . 4_566
Br1 Pb1 Br3 81.01(3) 4_566 4_566
Br2 Pb1 Br2 175.83(2) . 4_565
Br1 Pb1 Br2 82.10(2) . 4_565
Br3 Pb1 Br2 82.05(3) . 4_565
Br1 Pb1 Br2 99.45(2) 4_566 4_565
Br3 Pb1 Br2 98.69(3) 4_566 4_565
Pb1 Br2 Pb1 80.18(3) . 4_566
Pb1 Br1 Pb1 81.19(3) . 4_565
Pb1 Br3 Pb1 80.15(3) . 4_565
Br4 Pb2 Br4 180.0 . 3_556
Br4 Pb2 Br5 96.04(2) . .
Br4 Pb2 Br5 83.96(2) 3_556 .
Br4 Pb2 Br5 83.96(2) . 3_556
Br4 Pb2 Br5 96.04(2) 3_556 3_556
Br5 Pb2 Br5 180.0 . 3_556
Br4 Pb2 Br6 84.33(3) . 3_556
Br4 Pb2 Br6 95.67(3) 3_556 3_556
Br5 Pb2 Br6 99.51(3) . 3_556
Br5 Pb2 Br6 80.49(3) 3_556 3_556
Br4 Pb2 Br6 95.67(3) . .
Br4 Pb2 Br6 84.33(3) 3_556 .
Br5 Pb2 Br6 80.49(3) . .
Br5 Pb2 Br6 99.51(3) 3_556 .
Br6 Pb2 Br6 180.0 3_556 .
Br4 Pb3 Br4 180.000(16) 3_556 1_554
Br4 Pb3 Br5 96.02(2) 3_556 3
Br4 Pb3 Br5 83.98(2) 1_554 3
Br4 Pb3 Br5 83.98(2) 3_556 .
Br4 Pb3 Br5 96.02(2) 1_554 .
Br5 Pb3 Br5 180.0 3 .
Br4 Pb3 Br6 95.91(3) 3_556 3
Br4 Pb3 Br6 84.09(3) 1_554 3
Br5 Pb3 Br6 80.63(3) 3 3
Br5 Pb3 Br6 99.37(3) . 3
Br4 Pb3 Br6 84.09(3) 3_556 .
Br4 Pb3 Br6 95.91(3) 1_554 .
Br5 Pb3 Br6 99.37(3) 3 .
Br5 Pb3 Br6 80.63(3) . .
Br6 Pb3 Br6 180.0 3 .
Pb3 Br5 Pb2 79.68(3) . .
Pb2 Br6 Pb3 79.43(2) . .
Pb2 Br4 Pb3 81.52(3) . 1_556
C5 N1 C7 112.2(5) . .
C5 N1 C3 111.5(4) . .
C7 N1 C3 105.5(4) . .
C5 N1 C1 106.9(4) . .
C7 N1 C1 109.9(4) . .
C3 N1 C1 110.8(5) . .
N1 C5 C6 114.3(5) . .
N1 C7 C8 113.4(5) . .
C4 C3 N1 116.5(5) . .
C2 C1 N1 115.2(5) . .
C9 N2 C13 106.2(5) . .
C9 N2 C15 110.2(5) . .
C13 N2 C15 108.7(6) . .
C9 N2 C11 109.6(5) . .
C13 N2 C11 112.2(5) . .
C15 N2 C11 109.9(5) . .
N2 C9 C10 115.9(6) . .
C16 C15 N2 116.2(6) . .
C12 C11 N2 120.7(6) . .
N2 C13 C14 114.3(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br2 2.9485(9) .
Pb1 Br1 2.9756(9) .
Pb1 Br3 3.0119(10) .
Pb1 Br1 3.0470(10) 4_566
Pb1 Br3 3.0753(9) 4_566
Pb1 Br2 3.1331(9) 4_565
Br2 Pb1 3.1332(9) 4_566
Br1 Pb1 3.0469(10) 4_565
Br3 Pb1 3.0753(9) 4_565
Pb2 Br4 2.9959(9) .
Pb2 Br4 2.9959(9) 3_556
Pb2 Br5 3.0647(9) .
Pb2 Br5 3.0648(9) 3_556
Pb2 Br6 3.0652(9) 3_556
Pb2 Br6 3.0652(9) .
Pb3 Br4 3.0072(9) 3_556
Pb3 Br4 3.0072(9) 1_554
Pb3 Br5 3.0527(9) 3
Pb3 Br5 3.0527(9) .
Pb3 Br6 3.0685(8) 3
Pb3 Br6 3.0685(8) .
Br4 Pb3 3.0071(9) 1_556
N1 C5 1.492(7) .
N1 C7 1.518(8) .
N1 C3 1.533(7) .
N1 C1 1.541(8) .
C5 C6 1.511(10) .
C7 C8 1.527(10) .
C3 C4 1.488(9) .
C1 C2 1.520(9) .
N2 C9 1.479(8) .
N2 C13 1.490(9) .
N2 C15 1.497(9) .
N2 C11 1.505(8) .
C9 C10 1.493(13) .
C15 C16 1.484(10) .
C11 C12 1.430(11) .
C13 C14 1.536(12) .
