#------------------------------------------------------------------------------
#$Date: 2016-02-13 21:28:24 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176429 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/64/7036473.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_7036473
loop_
_publ_author_name
'Tong, Yuan-Bo'
'Ren, Li-Te'
'Duan, Hai-Bao'
'Liu, Jian-Lan'
'Ren, Xiao-Ming'
_publ_section_title
;
 An amphidynamic inorganic-organic hybrid crystal of bromoplumbate with
 1,5-bis(1-methylimidazolium)pentane exhibiting multi-functionality of a
 dielectric anomaly and temperature-dependent dual band emissions.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              17850
_journal_page_last               17858
_journal_paper_doi               10.1039/c5dt02739j
_journal_volume                  44
_journal_year                    2015
_chemical_formula_sum            'C6.5 H11 Br3 N2 Pb'
_chemical_formula_weight         564.09
_chemical_name_systematic
'[1, 5-bis(1-methylimidazolium)pentane]- [PbBr3]2'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/cc1jd88g
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-08 deposited with the CCDC.
2015-09-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   29.942(5)
_cell_length_b                   22.309(4)
_cell_length_c                   7.8155(11)
_cell_measurement_reflns_used    3630
_cell_measurement_temperature    413(2)
_cell_measurement_theta_max      24.4849
_cell_measurement_theta_min      2.2793
_cell_volume                     5220.6(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      413(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1061
_diffrn_reflns_av_unetI/netI     0.0847
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9453
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.277
_exptl_absorpt_coefficient_mu    22.073
_exptl_absorpt_correction_T_max  0.102
_exptl_absorpt_correction_T_min  0.047
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.871
_exptl_crystal_description       needle
_exptl_crystal_F_000             4016
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.733
_refine_diff_density_min         -1.880
_refine_diff_density_rms         0.303
_refine_ls_abs_structure_details
;
 Flack x determined using 524 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.00091(8)
_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   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     116
_refine_ls_number_reflns         2390
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0599
_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)+(0.0919P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1436
_refine_ls_wR_factor_ref         0.1681
_reflns_Friedel_coverage         0.812
_reflns_Friedel_fraction_full    0.951
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                1501
_reflns_number_total             2390
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c5dt02739j2.cif
_cod_data_source_block           140d
_cod_depositor_comments
'Adding full bibliography for 7036471--7036473.cif.'
_cod_original_cell_volume        5220.6(14)
_cod_original_formula_sum        'C6.50 H11 Br3 N2 Pb'
_cod_database_code               7036473
#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, z'
'-x+1/4, y+1/4, z+1/4'
'x+3/4, -y+3/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x+1/4, y+3/4, z+3/4'
'x+3/4, -y+5/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+3/4, y+1/4, z+3/4'
'x+5/4, -y+3/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+3/4, y+3/4, z+1/4'
'x+5/4, -y+5/4, z+1/4'
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
Pb1 Pb 0.24994(3) 0.50046(4) 0.7635(10) 0.0629(5) Uani 1 1 d . . .
Br1 Br 0.17675(8) 0.46089(13) 0.5418(3) 0.0776(9) Uani 1 1 d . . .
Br2 Br 0.19100(9) 0.56804(14) 0.9952(4) 0.0935(11) Uani 1 1 d . . .
Br3 Br 0.23836(11) 0.39757(14) 1.0159(4) 0.0931(10) Uani 1 1 d . . .
N1 N 0.1677(9) 0.7498(9) 0.198(4) 0.092(9) Uani 1 1 d . . .
N2 N 0.1478(7) 0.6746(11) 0.360(3) 0.077(6) Uani 1 1 d . . .
C1 C 0.2500 0.7500 -0.012(18) 0.27(7) Uani 1 2 d S T P
H1A H 0.2618 0.7804 0.0646 0.325 Uiso 0.5 1 calc R U P
H1B H 0.2382 0.7196 0.0646 0.325 Uiso 0.5 1 calc R U P
C2 C 0.215(3) 0.774(3) -0.054(10) 0.31(6) Uani 1 1 d . . .
H2A H 0.2051 0.7515 -0.1527 0.366 Uiso 1 1 calc R U .
H2B H 0.2244 0.8129 -0.0991 0.366 Uiso 1 1 calc R U .
C3 C 0.1729(13) 0.7873(14) 0.048(6) 0.137(16) Uani 1 1 d . . .
H3A H 0.1733 0.8290 0.0836 0.164 Uiso 1 1 calc R U .
H3B H 0.1472 0.7817 -0.0258 0.164 Uiso 1 1 calc R U .
C4 C 0.1470(9) 0.6993(13) 0.206(4) 0.078(7) Uani 1 1 d . . .
H4 H 0.1329 0.6818 0.1130 0.094 Uiso 1 1 calc R U .
C5 C 0.1715(12) 0.715(2) 0.456(5) 0.126(15) Uani 1 1 d . . .
H5 H 0.1784 0.7099 0.5707 0.151 Uiso 1 1 calc R U .
C6 C 0.1828(13) 0.7596(16) 0.364(6) 0.106(12) Uani 1 1 d . . .
H6 H 0.1984 0.7931 0.4015 0.127 Uiso 1 1 calc R U .
C7 C 0.1299(11) 0.6179(14) 0.419(5) 0.122(13) Uani 1 1 d . . .
H7A H 0.1075 0.6250 0.5041 0.183 Uiso 1 1 calc R U .
H7B H 0.1535 0.5941 0.4668 0.183 Uiso 1 1 calc R U .
H7C H 0.1168 0.5969 0.3238 0.183 Uiso 1 1 calc R U .
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'
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'
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
Br1 Pb1 Br2 93.99(8) . .
Br1 Pb1 Br3 86.2(2) . 10_564
Br2 Pb1 Br3 94.49(9) . 10_564
Br1 Pb1 Br3 94.06(8) . .
Br2 Pb1 Br3 85.4(2) . .
Br3 Pb1 Br3 179.7(2) 10_564 .
Br1 Pb1 Br2 83.09(19) . 10_564
Br2 Pb1 Br2 176.0(2) . 10_564
Br3 Pb1 Br2 82.69(19) 10_564 10_564
Br3 Pb1 Br2 97.46(9) . 10_564
Br1 Pb1 Br1 173.6(2) . 10_565
Br2 Pb1 Br1 81.69(18) . 10_565
Br3 Pb1 Br1 98.81(8) 10_564 10_565
Br3 Pb1 Br1 80.88(19) . 10_565
Br2 Pb1 Br1 101.44(7) 10_564 10_565
Pb1 Br1 Pb1 78.94(6) . 10_564
Pb1 Br2 Pb1 79.86(7) . 10_565
Pb1 Br3 Pb1 80.41(7) 10_565 .
C4 N1 C6 104(3) . .
C4 N1 C3 127(3) . .
C6 N1 C3 129(3) . .
C4 N2 C5 104(3) . .
C4 N2 C7 130(3) . .
C5 N2 C7 126(3) . .
C2 C1 C2 148(10) 14_565 .
C2 C1 H1A 99.7 14_565 .
C2 C1 H1A 99.7 . .
C2 C1 H1B 99.7 14_565 .
C2 C1 H1B 99.7 . .
H1A C1 H1B 104.1 . .
C1 C2 C3 130(9) . .
C1 C2 H2A 104.6 . .
C3 C2 H2A 104.6 . .
C1 C2 H2B 104.6 . .
C3 C2 H2B 104.6 . .
H2A C2 H2B 105.7 . .
N1 C3 C2 114(3) . .
N1 C3 H3A 108.8 . .
C2 C3 H3A 108.8 . .
N1 C3 H3B 108.8 . .
C2 C3 H3B 108.8 . .
H3A C3 H3B 107.7 . .
N1 C4 N2 114(3) . .
N1 C4 H4 123.2 . .
N2 C4 H4 123.2 . .
C6 C5 N2 110(4) . .
C6 C5 H5 124.9 . .
N2 C5 H5 124.9 . .
C5 C6 N1 108(3) . .
C5 C6 H6 125.9 . .
N1 C6 H6 125.9 . .
N2 C7 H7A 109.5 . .
N2 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N2 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 Br1 2.930(5) .
Pb1 Br2 2.944(6) .
Pb1 Br3 3.007(6) 10_564
Pb1 Br3 3.046(6) .
Pb1 Br2 3.140(6) 10_564
Pb1 Br1 3.208(6) 10_565
Br1 Pb1 3.208(6) 10_564
Br2 Pb1 3.140(6) 10_565
Br3 Pb1 3.007(6) 10_565
N1 C4 1.29(3) .
N1 C6 1.39(5) .
N1 C3 1.45(5) .
N2 C4 1.32(3) .
N2 C5 1.36(4) .
N2 C7 1.45(4) .
C1 C2 1.22(8) 14_565
C1 C2 1.22(8) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 C3 1.53(8) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C4 H4 0.9300 .
C5 C6 1.28(6) .
C5 H5 0.9300 .
C6 H6 0.9300 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
