#------------------------------------------------------------------------------
#$Date: 2017-03-05 07:16:50 +0200 (Sun, 05 Mar 2017) $
#$Revision: 193829 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/17/7041761.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_7041761
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                   7.8530(15)
_cell_length_b                   10.418(2)
_cell_length_c                   18.343(4)
_cell_measurement_reflns_used    6350
_cell_measurement_temperature    350(2)
_cell_measurement_theta_max      25.7823
_cell_measurement_theta_min      2.4635
_cell_volume                     1500.7(5)
_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      350(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.5734
_diffrn_reflns_av_unetI/netI     0.1456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_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            15166
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.822
_exptl_absorpt_coefficient_mu    17.384
_exptl_absorpt_correction_T_max  0.240
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Bruker,2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.147
_exptl_crystal_description       needle
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.040
_refine_diff_density_min         -2.370
_refine_diff_density_rms         0.463
_refine_ls_extinction_coef       0.0034(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0729
_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)+(0.1074P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1928
_refine_ls_wR_factor_ref         0.2016
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1102
_reflns_number_total             1403
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c6dt03691k2.cif
_cod_data_source_block           15
_cod_depositor_comments
'Adding full bibliography for 7041760--7041764.cif.'
_cod_original_cell_volume        1500.6(5)
_cod_database_code               7041761
_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.
;
_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
C1 C 0.460(3) 0.250000 0.6509(12) 0.057(5) Uani 1 2 d S T P
C2 C 0.538(3) 0.1349(18) 0.6240(11) 0.088(6) Uani 1 1 d . . .
H2 H 0.499358 0.055408 0.640081 0.105 Uiso 1 1 calc R U .
C3 C 0.658(2) 0.1403(17) 0.5794(10) 0.080(5) Uani 1 1 d . . .
H3 H 0.706125 0.064256 0.562663 0.096 Uiso 1 1 calc R U .
C4 C 0.865(3) 0.250000 0.5020(16) 0.128(14) Uani 1 2 d S T P
H4A H 0.853371 0.175023 0.470994 0.153 Uiso 0.5 1 calc R U P
H4B H 0.853371 0.324977 0.470994 0.153 Uiso 0.5 1 calc R U P
C5 C 1.032(3) 0.250000 0.5320(19) 0.17(2) Uani 1 2 d S T P
H5A H 1.047141 0.174009 0.562882 0.252 Uiso 0.5 1 d R U P
H5B H 1.048582 0.327602 0.561422 0.252 Uiso 0.5 1 d R U P
H5C H 1.116534 0.250000 0.492563 0.252 Uiso 1 2 d R U P
I1 I 0.95724(12) 0.04008(10) 0.31816(5) 0.0640(5) Uani 1 1 d . . .
I2 I 0.44821(16) 0.250000 0.38854(7) 0.0562(5) Uani 1 2 d S T P
N1 N 0.338(3) 0.250000 0.7005(12) 0.080(6) Uani 1 2 d S T P
H1A H 0.301701 0.321381 0.718257 0.095 Uiso 0.5 1 calc R U P
H1B H 0.294392 0.178619 0.714963 0.095 Uiso 0.5 1 calc R U P
N2 N 0.718(3) 0.250000 0.5552(9) 0.090(7) Uani 1 2 d S T P
Pb1 Pb 0.70833(9) 0.250000 0.24909(3) 0.0448(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 123.2(11) . 7_565
N1 C1 C2 123.2(11) . .
C2 C1 C2 113(2) 7_565 .
C3 C2 C1 120.7(18) . .
C3 C2 H2 119.7 . .
C1 C2 H2 119.7 . .
C2 C3 N2 122.1(18) . .
C2 C3 H3 119.0 . .
N2 C3 H3 119.0 . .
C5 C4 N2 117(2) . .
C5 C4 H4A 108.0 . .
N2 C4 H4A 108.0 . .
C5 C4 H4B 108.0 . .
N2 C4 H4B 108.0 . .
H4A C4 H4B 107.3 . .
C4 C5 H5A 109.4 . .
C4 C5 H5B 109.4 . .
H5A C5 H5B 109.5 . .
C4 C5 H5C 109.7 . .
H5A C5 H5C 110.3 . .
H5B C5 H5C 108.6 . .
Pb1 I1 Pb1 75.87(3) 6_656 .
Pb1 I2 Pb1 75.34(3) 6_556 .
C1 N1 H1A 120.0 . .
C1 N1 H1B 120.0 . .
H1A N1 H1B 120.0 . .
C3 N2 C3 121(2) 7_565 .
C3 N2 C4 119.5(11) 7_565 .
C3 N2 C4 119.4(11) . .
I2 Pb1 I1 93.42(3) 6_656 6_556
I2 Pb1 I1 93.42(3) 6_656 4_455
I1 Pb1 I1 86.47(4) 6_556 4_455
I2 Pb1 I1 87.24(3) 6_656 .
I1 Pb1 I1 93.57(4) 6_556 .
I1 Pb1 I1 179.33(3) 4_455 .
I2 Pb1 I1 87.24(3) 6_656 7_565
I1 Pb1 I1 179.33(3) 6_556 7_565
I1 Pb1 I1 93.57(4) 4_455 7_565
I1 Pb1 I1 86.39(4) . 7_565
I2 Pb1 I2 178.12(4) 6_656 .
I1 Pb1 I2 85.21(3) 6_556 .
I1 Pb1 I2 85.21(3) 4_455 .
I1 Pb1 I2 94.13(3) . .
I1 Pb1 I2 94.13(3) 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 1.32(3) .
C1 C2 1.44(2) 7_565
C1 C2 1.44(2) .
C2 C3 1.25(2) .
C2 H2 0.9300 .
C3 N2 1.313(19) .
C3 H3 0.9300 .
C4 C5 1.43(4) .
C4 N2 1.51(3) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 H5A 0.9800 .
C5 H5B 0.9800 .
C5 H5C 0.9799 .
I1 Pb1 3.1925(11) 6_656
I1 Pb1 3.1950(11) .
I2 Pb1 3.1500(15) 6_556
I2 Pb1 3.2734(15) .
N1 H1A 0.8600 .
N1 H1B 0.8600 .
