#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:34:41 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232892 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/83/4348372.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_4348372
loop_
_publ_author_name
'Liu, Guangfeng'
'Liu, Jie'
'Sun, Zhihua'
'Zhang, Zhenyi'
'Chang, Lei'
'Wang, Junling'
'Tao, Xutang'
'Zhang, Qichun'
_publ_section_title
;
 Thermally Induced Reversible Double Phase Transitions in an
 Organic-Inorganic Hybrid Iodoplumbate C4H12NPbI3 with Symmetry Breaking.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8025
_journal_page_last               8030
_journal_paper_doi               10.1021/acs.inorgchem.6b01143
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C4 H12 I3 N Pb'
_chemical_formula_weight         662.04
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.798(3)
_cell_length_b                   9.798(3)
_cell_length_c                   7.953(3)
_cell_measurement_reflns_used    5523
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.40
_cell_volume                     661.2(4)
_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-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7502
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.583
_diffrn_reflns_theta_min         2.400
_exptl_absorpt_coefficient_mu    19.710
_exptl_absorpt_correction_T_max  0.0182
_exptl_absorpt_correction_T_min  0.0042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.325
_exptl_crystal_description       prism
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.495
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.214
_refine_diff_density_max         2.580
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.214
_refine_ls_extinction_coef       0.0059(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   0.943
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     33
_refine_ls_number_reflns         557
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0304
_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)+(0.0584P)²+2.5940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                544
_reflns_number_total             557
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b01143_si_004.cif
_cod_data_source_block           02_a
_cod_original_cell_volume        661.2(5)
_cod_database_code               4348372
_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   0.037
_shelx_estimated_absorpt_t_max   0.101
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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
Pb01 Pb 0.0000 0.0000 0.5000 0.0405(2) Uani 1 6 d S T P . .
N1 N 0.3333 0.6667 0.7500 0.042(3) Uani 1 6 d DS T P . .
I002 I 0.29949(9) 0.17206(11) 0.7500 0.0545(3) Uani 1 2 d S T P . .
C1 C 0.467(3) 0.647(4) 0.715(6) 0.058(19) Uani 0.25 1 d D U P A -1
H1A H 0.4398 0.5704 0.6272 0.087 Uiso 0.25 1 calc R U P A -1
H1B H 0.4957 0.6126 0.8143 0.087 Uiso 0.25 1 calc R U P A -1
H1C H 0.5539 0.7462 0.6785 0.087 Uiso 0.25 1 calc R U P A -1
C2 C 0.245(6) 0.582(6) 0.601(4) 0.081(14) Uani 0.25 1 d D U P A -1
H2A H 0.3156 0.6073 0.5077 0.122 Uiso 0.25 1 calc R U P A -1
H2B H 0.1678 0.6122 0.5752 0.122 Uiso 0.25 1 calc R U P A -1
H2C H 0.1926 0.4706 0.6219 0.122 Uiso 0.25 1 calc R U P A -1
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
I002 Pb01 I002 180.00(2) 9_556 3
I002 Pb01 I002 86.17(2) 9_556 7_556
I002 Pb01 I002 93.83(2) 3 7_556
I002 Pb01 I002 93.83(2) 9_556 .
I002 Pb01 I002 86.17(2) 3 .
I002 Pb01 I002 180.0 7_556 .
I002 Pb01 I002 86.16(2) 9_556 8_556
I002 Pb01 I002 93.84(2) 3 8_556
I002 Pb01 I002 86.16(2) 7_556 8_556
I002 Pb01 I002 93.83(2) . 8_556
I002 Pb01 I002 93.84(2) 9_556 2
I002 Pb01 I002 86.16(2) 3 2
I002 Pb01 I002 93.84(2) 7_556 2
I002 Pb01 I002 86.17(2) . 2
I002 Pb01 I002 180.0 8_556 2
C1 N1 C2 95(3) . .
Pb01 I002 Pb01 75.87(3) . 4
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 . .
N1 C2 H2A 109.5 . .
N1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
N1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb01 I002 3.2340(10) 9_556
Pb01 I002 3.2340(10) 3
Pb01 I002 3.2340(10) 7_556
Pb01 I002 3.2341(10) .
Pb01 I002 3.2341(10) 8_556
Pb01 I002 3.2341(10) 2
N1 C1 1.44(2) .
N1 C2 1.46(2) .
I002 Pb01 3.2341(10) 4
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
