#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:16:50 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193829 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/17/7041763.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_7041763
loop_
_publ_author_name
'Duan, Hai-Bao'
'Yu, Shan-Shan'
'Liu, Shao-Xian'
'Zhang, Hui'
_publ_section_title
;
 An inorganic-organic hybrid crystal with a two-step dielectric response
 and thermochromic luminescence.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2220
_journal_page_last               2227
_journal_paper_doi               10.1039/c6dt03691k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C7 H11 I3 N2 Pb'
_chemical_formula_sum            'C7 H11 I3 N2 Pb'
_chemical_formula_weight         711.07
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-01-15 deposited with the CCDC.
2017-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.8382(6)
_cell_length_b                   10.3922(7)
_cell_length_c                   18.2707(13)
_cell_measurement_reflns_used    6350
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      25.7823
_cell_measurement_theta_min      2.4635
_cell_volume                     1488.26(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.2793
_diffrn_reflns_av_unetI/netI     0.0793
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16469
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.425
_exptl_absorpt_coefficient_mu    17.528
_exptl_absorpt_correction_T_max  0.168
_exptl_absorpt_correction_T_min  0.160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.174
_exptl_crystal_description       needele
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.533
_refine_diff_density_min         -2.710
_refine_diff_density_rms         0.541
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1393
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0666
_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)+(0.1381P)²+6.2294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1249
_reflns_number_total             1393
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt03691k2.cif
_cod_data_source_block           1-300K
_cod_depositor_comments
'Adding full bibliography for 7041760--7041764.cif.'
_cod_database_code               7041763
_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.
;
_shelx_estimated_absorpt_t_min   0.249
_shelx_estimated_absorpt_t_max   0.273
_structure_special_details
;
 This structure is part of a multi-temperature experiment.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z'
'-x-1/2, 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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4579(19) 0.250000 0.6518(12) 0.047(5) Uani 1 2 d S T P . .
C2 C 0.530(2) 0.1335(15) 0.6266(8) 0.062(4) Uani 1 1 d . . . . .
H2 H 0.488765 0.054629 0.642835 0.074 Uiso 1 1 calc R U . . .
C3 C 0.659(2) 0.1396(16) 0.5789(8) 0.065(4) Uani 1 1 d . . . . .
H3 H 0.703781 0.063019 0.561087 0.078 Uiso 1 1 calc R U . . .
C4A C 0.874(4) 0.287(7) 0.5035(18) 0.073(6) Uani 0.37(2) 1 d D U P A -1
H4A1 H 0.854709 0.247941 0.456055 0.088 Uiso 0.37(2) 1 calc R U P A -1
H4A2 H 0.874753 0.379698 0.496874 0.088 Uiso 0.37(2) 1 calc R U P A -1
C5A C 1.034(3) 0.248(19) 0.5295(17) 0.073(7) Uani 0.37(2) 1 d D U P A -1
H5A1 H 1.061772 0.296081 0.572918 0.110 Uiso 0.37(2) 1 calc R U P A -1
H5A2 H 1.119086 0.264277 0.492729 0.110 Uiso 0.37(2) 1 calc R U P A -1
H5A3 H 1.031465 0.158129 0.540728 0.110 Uiso 0.37(2) 1 calc R U P A -1
C4B C 0.850(13) 0.223(14) 0.492(4) 0.073(6) Uani 0.13(2) 1 d D U P A -2
H4B1 H 0.785681 0.200446 0.448221 0.087 Uiso 0.13(2) 1 calc R U P A -2
H4B2 H 0.914882 0.300323 0.481013 0.087 Uiso 0.13(2) 1 calc R U P A -2
C5B C 0.963(10) 0.123(12) 0.508(6) 0.075(8) Uani 0.13(2) 1 d D U P A -2
H5B1 H 1.072225 0.138812 0.486270 0.112 Uiso 0.13(2) 1 d R U P A -2
H5B2 H 0.917814 0.043184 0.490196 0.112 Uiso 0.13(2) 1 d R U P A -2
H5B3 H 0.976594 0.117108 0.560611 0.112 Uiso 0.13(2) 1 d R U P A -2
I1 I 0.95827(10) 0.03946(9) 0.31848(5) 0.0522(4) Uani 1 1 d . . . . .
I2 I 0.44858(13) 0.250000 0.38895(6) 0.0453(4) Uani 1 2 d S T P . .
N1 N 0.334(2) 0.250000 0.7028(10) 0.064(4) Uani 1 2 d S T P . .
H1A H 0.297799 0.321584 0.720520 0.076 Uiso 0.5 1 calc R U P . .
H1B H 0.291437 0.178416 0.717677 0.076 Uiso 0.5 1 calc R U P . .
N2 N 0.7252(18) 0.250000 0.5557(8) 0.072(5) Uani 1 2 d DS TU P . .
Pb1 Pb 0.70892(7) 0.250000 0.24918(3) 0.0357(4) Uani 1 2 d S T P . .
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'
I I -0.4742 1.8119 '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
N1 C1 C2 121.0(10) . 7_565
N1 C1 C2 121.0(10) . .
C2 C1 C2 117.9(19) 7_565 .
C3 C2 C1 118.4(15) . .
C3 C2 H2 120.8 . .
C1 C2 H2 120.8 . .
N2 C3 C2 123.1(15) . .
N2 C3 H3 118.5 . .
C2 C3 H3 118.5 . .
C5A C4A N2 113(2) . .
C5A C4A H4A1 108.9 . .
N2 C4A H4A1 108.9 . .
C5A C4A H4A2 108.9 . .
N2 C4A H4A2 108.9 . .
H4A1 C4A H4A2 107.8 . .
C4A C5A H5A1 109.5 . .
C4A C5A H5A2 109.5 . .
H5A1 C5A H5A2 109.5 . .
C4A C5A H5A3 109.5 . .
H5A1 C5A H5A3 109.5 . .
H5A2 C5A H5A3 109.5 . .
C5B C4B N2 112(3) . .
C5B C4B H4B1 109.3 . .
N2 C4B H4B1 109.3 . .
C5B C4B H4B2 109.3 . .
N2 C4B H4B2 109.3 . .
H4B1 C4B H4B2 108.0 . .
C4B C5B H5B1 109.9 . .
C4B C5B H5B2 109.2 . .
H5B1 C5B H5B2 109.5 . .
C4B C5B H5B3 109.3 . .
H5B1 C5B H5B3 109.5 . .
H5B2 C5B H5B3 109.5 . .
Pb1 I1 Pb1 75.73(2) 6_656 .
Pb1 I2 Pb1 75.29(3) 6_556 .
C1 N1 H1A 120.0 . .
C1 N1 H1B 120.0 . .
H1A N1 H1B 120.0 . .
C3 N2 C3 119.3(16) . 7_565
C3 N2 C4B 109(6) . .
C3 N2 C4B 130(5) 7_565 .
C3 N2 C4A 135(3) . .
C3 N2 C4A 106(3) 7_565 .
I2 Pb1 I1 93.26(2) 6_656 6_556
I2 Pb1 I1 93.26(2) 6_656 4_455
I1 Pb1 I1 86.62(4) 6_556 4_455
I2 Pb1 I1 87.29(2) 6_656 .
I1 Pb1 I1 93.47(3) 6_556 .
I1 Pb1 I1 179.44(2) 4_455 .
I2 Pb1 I1 87.29(2) 6_656 7_565
I1 Pb1 I1 179.44(2) 6_556 7_565
I1 Pb1 I1 93.47(3) 4_455 7_565
I1 Pb1 I1 86.43(4) . 7_565
I2 Pb1 I2 178.03(3) 6_656 .
I1 Pb1 I2 85.31(2) 6_556 .
I1 Pb1 I2 85.31(2) 4_455 .
I1 Pb1 I2 94.14(2) . .
I1 Pb1 I2 94.14(2) 7_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.34(3) .
C1 C2 1.413(17) 7_565
C1 C2 1.413(17) .
C2 C3 1.33(2) .
C2 H2 0.9300 .
C3 N2 1.330(17) .
C3 H3 0.9300 .
C4A C5A 1.40(2) .
C4A N2 1.557(18) .
C4A H4A1 0.9700 .
C4A H4A2 0.9700 .
C5A H5A1 0.9600 .
C5A H5A2 0.9600 .
C5A H5A3 0.9600 .
C4B C5B 1.40(2) .
C4B N2 1.55(2) .
C4B H4B1 0.9700 .
C4B H4B2 0.9700 .
C5B H5B1 0.9600 .
C5B H5B2 0.9600 .
C5B H5B3 0.9600 .
I1 Pb1 3.1900(9) 6_656
I1 Pb1 3.1954(9) .
I2 Pb1 3.1461(12) 6_556
I2 Pb1 3.2688(12) .
N1 H1A 0.8600 .
N1 H1B 0.8600 .
