#------------------------------------------------------------------------------
#$Date: 2025-08-04 10:03:09 +0300 (Mon, 04 Aug 2025) $
#$Revision: 301442 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/57/7055738.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_7055738
loop_
_publ_author_name
'Wan, Kun-Ming'
'Tong, Yuan-Bo'
'Li, Li'
'Zou, Yang'
'Duan, Hai-Bao'
'Liu, Jian-Lan'
'Ren, XiaoMing'
_publ_section_title
;
 Investigation of thermochromic photoluminescent, dielectric and crystal
 structural properties for an inorganic-organic hybrid solid of
 [1-hexyl-3-methylimidazolium][PbBr3]
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              8664
_journal_page_last               8672
_journal_paper_doi               10.1039/C6NJ01508E
_journal_volume                  40
_journal_year                    2016
_chemical_formula_sum            'C10 H19 Br3 N2 Pb'
_chemical_formula_weight         614.19
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-09 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.062(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4917(6)
_cell_length_b                   7.9842(5)
_cell_length_c                   23.0848(12)
_cell_measurement_reflns_used    9869
_cell_measurement_temperature    313(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.97
_cell_volume                     1653.52(17)
_computing_cell_refinement       'Bruker APEXII'
_computing_data_collection       'Bruker APEXII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      313(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0642
_diffrn_reflns_Laue_measured_fraction_full 0.917
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6076
_diffrn_reflns_point_group_measured_fraction_full 0.917
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         3.162
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    17.433
_exptl_absorpt_correction_T_max  0.175
_exptl_absorpt_correction_T_min  0.021
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.467
_exptl_crystal_description       bulk
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.897
_refine_diff_density_min         -5.440
_refine_diff_density_rms         0.498
_refine_ls_extinction_coef       0.0072(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         2674
_refine_ls_number_restraints     203
_refine_ls_restrained_S_all      2.814
_refine_ls_R_factor_all          0.1130
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2622
_refine_ls_wR_factor_ref         0.2773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2049
_reflns_number_total             2674
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6nj01508e2.cif
_cod_data_source_block           313k
_cod_database_code               7055738
#BEGIN Tags that were not found in dictionaries:
_shelx_shelxl_version_number     2014/7
_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.
;
#END Tags that were not found in dictionaries
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
N1 N 0.063(3) 0.658(3) 0.8395(12) 0.073(3) Uani 1 1 d . U
N2 N 0.078(3) 0.425(3) 0.8851(12) 0.074(3) Uani 1 1 d . U
C1 C 0.100(3) 0.795(3) 0.8049(14) 0.075(4) Uani 1 1 d . U
H1A H 0.1869 0.7651 0.7945 0.113 Uiso 1 1 calc R U
H1B H 0.1197 0.8944 0.8294 0.113 Uiso 1 1 calc R U
H1C H 0.0180 0.8140 0.7681 0.113 Uiso 1 1 calc R U
C2 C -0.060(3) 0.646(3) 0.8559(15) 0.074(3) Uani 1 1 d . U
H2 H -0.1354 0.7248 0.8483 0.089 Uiso 1 1 calc R U
C3 C -0.054(3) 0.501(3) 0.8849(14) 0.074(3) Uani 1 1 d . U
H3 H -0.1235 0.4585 0.9015 0.089 Uiso 1 1 calc R U
C4 C 0.146(3) 0.522(3) 0.8590(13) 0.074(3) Uani 1 1 d . U
H4 H 0.2381 0.5005 0.8544 0.089 Uiso 1 1 calc R U
C5 C 0.133(3) 0.253(3) 0.9116(14) 0.077(3) Uani 1 1 d . U
H5A H 0.0626 0.1685 0.8892 0.093 Uiso 1 1 calc R U
H5B H 0.2280 0.2305 0.9063 0.093 Uiso 1 1 calc R U
C6 C 0.149(3) 0.242(3) 0.9775(14) 0.079(3) Uani 1 1 d . U
H6A H 0.2292 0.3160 0.9997 0.095 Uiso 1 1 calc R U
H6B H 0.0581 0.2849 0.9826 0.095 Uiso 1 1 calc R U
C7 C 0.178(3) 0.080(3) 1.0068(15) 0.084(3) Uani 1 1 d D U
H7A H 0.0862 0.0163 0.9914 0.101 Uiso 1 1 calc R U
H7B H 0.1945 0.0988 1.0500 0.101 Uiso 1 1 calc DR U
C8 C 0.301(3) -0.033(3) 1.0032(14) 0.085(3) Uani 1 1 d D U
H8A H 0.3953 0.0146 1.0273 0.102 Uiso 1 1 calc R U
H8B H 0.2986 -0.0382 0.9609 0.102 Uiso 1 1 calc R U
C9 C 0.291(3) -0.213(3) 1.0257(15) 0.089(3) Uani 1 1 d D U
H9A H 0.3070 -0.2111 1.0694 0.107 Uiso 1 1 calc R U
H9B H 0.1923 -0.2575 1.0052 0.107 Uiso 1 1 calc R U
C10 C 0.407(3) -0.326(3) 1.0130(17) 0.096(5) Uani 1 1 d D U
H10A H 0.3730 -0.3584 0.9706 0.144 Uiso 1 1 calc R U
H10B H 0.4207 -0.4244 1.0382 0.144 Uiso 1 1 calc R U
H10C H 0.4996 -0.2671 1.0222 0.144 Uiso 1 1 calc R U
Pb1 Pb 0.50621(8) 0.39563(9) 0.75194(4) 0.0358(5) Uani 1 1 d . .
Br1 Br 0.5408(3) 0.6476(3) 0.85329(11) 0.0492(7) Uani 1 1 d . .
Br2 Br 0.2487(2) 0.5863(3) 0.68929(13) 0.0547(8) Uani 1 1 d . .
Br3 Br 0.3235(3) 0.1683(3) 0.79694(13) 0.0545(8) Uani 1 1 d . .
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'
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'
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
C4 N1 C2 109(2) . .
C4 N1 C1 125(2) . .
C2 N1 C1 126(2) . .
C4 N2 C3 109(2) . .
C4 N2 C5 125(2) . .
C3 N2 C5 126(2) . .
N1 C1 H1A 109.5 . .
N1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
N1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C3 C2 N1 108(3) . .
C3 C2 H2 126.1 . .
N1 C2 H2 126.1 . .
C2 C3 N2 106(2) . .
C2 C3 H3 127.1 . .
N2 C3 H3 127.1 . .
N2 C4 N1 108(3) . .
N2 C4 H4 125.9 . .
N1 C4 H4 125.9 . .
C6 C5 N2 112(2) . .
C6 C5 H5A 109.2 . .
N2 C5 H5A 109.2 . .
C6 C5 H5B 109.2 . .
N2 C5 H5B 109.2 . .
H5A C5 H5B 107.9 . .
C7 C6 C5 118(3) . .
C7 C6 H6A 107.7 . .
C5 C6 H6A 107.7 . .
C7 C6 H6B 107.7 . .
C5 C6 H6B 107.7 . .
H6A C6 H6B 107.1 . .
C6 C7 C8 123(2) . .
C6 C7 H7A 106.5 . .
C8 C7 H7A 106.5 . .
C6 C7 H7B 106.5 . .
C8 C7 H7B 106.5 . .
H7A C7 H7B 106.5 . .
C7 C8 C9 114.3(16) . .
C7 C8 H8A 108.7 . .
C9 C8 H8A 108.7 . .
C7 C8 H8B 108.7 . .
C9 C8 H8B 108.7 . .
H8A C8 H8B 107.6 . .
C10 C9 C8 111(2) . .
C10 C9 H9A 109.4 . .
C8 C9 H9A 109.4 . .
C10 C9 H9B 109.4 . .
C8 C9 H9B 109.4 . .
H9A C9 H9B 108.0 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
Br2 Pb1 Br3 90.10(7) . .
Br2 Pb1 Br1 83.99(7) . .
Br3 Pb1 Br1 93.73(7) . .
Br2 Pb1 Br1 93.71(7) . 2_646
Br3 Pb1 Br1 86.02(7) . 2_646
Br1 Pb1 Br1 177.68(4) . 2_646
Br2 Pb1 Br3 84.47(7) . 2_656
Br3 Pb1 Br3 173.92(6) . 2_656
Br1 Pb1 Br3 82.98(6) . 2_656
Br1 Pb1 Br3 97.05(7) 2_646 2_656
Pb1 Br1 Pb1 82.24(6) . 2_656
Pb1 Br3 Pb1 82.41(5) . 2_646
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 C4 1.33(3) .
N1 C2 1.34(3) .
N1 C1 1.46(3) .
N2 C4 1.28(3) .
N2 C3 1.38(3) .
N2 C5 1.53(3) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.33(3) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 H4 0.9300 .
C5 C6 1.48(4) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C6 C7 1.44(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C8 1.498(17) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 C9 1.536(18) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C10 1.523(18) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
Pb1 Br2 2.842(2) .
Pb1 Br3 2.925(2) .
Pb1 Br1 3.021(2) .
Pb1 Br1 3.052(2) 2_646
Pb1 Br3 3.133(2) 2_656
Br1 Pb1 3.052(2) 2_656
Br3 Pb1 3.133(2) 2_646
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C4 N1 C2 C3 -1(4)
C1 N1 C2 C3 178(3)
N1 C2 C3 N2 0(4)
C4 N2 C3 C2 1(4)
C5 N2 C3 C2 -178(3)
C3 N2 C4 N1 -2(4)
C5 N2 C4 N1 178(3)
C2 N1 C4 N2 2(4)
C1 N1 C4 N2 -177(3)
C4 N2 C5 C6 123(3)
C3 N2 C5 C6 -58(4)
N2 C5 C6 C7 171(2)
C5 C6 C7 C8 51(4)
C6 C7 C8 C9 -168(3)
C7 C8 C9 C10 173(3)
