#------------------------------------------------------------------------------
#$Date: 2015-12-04 03:39:04 +0200 (Fri, 04 Dec 2015) $
#$Revision: 170697 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/72/2107272.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2107272
loop_
_publ_author_name
'Weber, Oliver J.'
'Marshall, Kayleigh L.'
'Dyson, Lewis M.'
'Weller, Mark T.'
_publ_section_title
;
 Structural diversity in hybrid organic--inorganic lead iodide materials
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              668
_journal_page_last               678
_journal_paper_doi               10.1107/S2052520615019885
_journal_volume                  71
_journal_year                    2015
_chemical_formula_sum            'C3 H5 I3 N2 Pb'
_chemical_formula_weight         656.98
_chemical_name_common            'imidazolium lead iodide'
_chemical_name_systematic
;
 ?
;
_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'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.5643(6)
_cell_length_b                   15.5643(6)
_cell_length_c                   8.0123(5)
_cell_measurement_temperature    150(2)
_cell_volume                     1680.92(14)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.820
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0341
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3203
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.721
_diffrn_reflns_theta_min         3.650
_exptl_absorpt_coefficient_mu    23.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24599
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.894
_exptl_crystal_description       needle
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.092
_refine_diff_density_min         -10.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         1277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1182
_refine_ls_R_factor_gt           0.0956
_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)+(0.0564P)²+177.1023P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2107
_refine_ls_wR_factor_ref         0.2254
_reflns_number_gt                977
_reflns_number_total             1277
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ps5046sup1.cif
_cod_data_source_block           shelx6
_cod_original_cell_volume        1680.92(17)
_cod_database_code               2107272
_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.
;
_shelxl_version_number           201.4
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
C C3 0.399(4) 0.354(4) 0.7500 0.069(13) Uiso d 1
H H3 0.4650 0.3691 0.7500 0.083 Uiso calc 1
N N1 0.334(3) 0.339(3) 0.611(8) 0.123(16) Uiso d 1
H H1 0.3457 0.3378 0.5069 0.148 Uiso calc 1
C C1 0.262(3) 0.330(3) 0.670(5) 0.086(12) Uiso d 1
H H1A 0.2086 0.3234 0.6071 0.103 Uiso calc 1
Pb Pb1 0.0000 0.0000 0.5000 0.0370(6) Uani d 1
Pb Pb2 0.3333 0.6667 0.5034(2) 0.0355(5) Uani d 1
I I3 0.1587(2) 0.5134(3) 0.7500 0.0687(10) Uani d 1
I I4 0.4986(2) 0.1806(2) 0.7500 0.0544(8) Uani d 1
I I5 -0.02512(19) 0.14913(18) 0.7500 0.0391(6) Uani d 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'
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'
H H 0.0000 0.0000 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C3 N1 . 10_557 100(5)
C1 N1 C3 . . 105(6)
N1 C1 C1 . 10_557 114(4)
I5 Pb1 I5 9_556 3 180.0
I5 Pb1 I5 9_556 7_556 85.68(4)
I5 Pb1 I5 3 7_556 94.32(4)
I5 Pb1 I5 9_556 2 94.32(4)
I5 Pb1 I5 3 2 85.68(4)
I5 Pb1 I5 7_556 2 94.32(4)
I5 Pb1 I5 9_556 8_556 85.68(4)
I5 Pb1 I5 3 8_556 94.32(4)
I5 Pb1 I5 7_556 8_556 85.68(4)
I5 Pb1 I5 2 8_556 180.0
I5 Pb1 I5 9_556 . 94.32(4)
I5 Pb1 I5 3 . 85.68(4)
I5 Pb1 I5 7_556 . 180.00(9)
I5 Pb1 I5 2 . 85.68(4)
I5 Pb1 I5 8_556 . 94.32(4)
I4 Pb2 I4 8_566 7_666 84.57(5)
I4 Pb2 I4 8_566 9_556 84.57(5)
I4 Pb2 I4 7_666 9_556 84.57(5)
I4 Pb2 I3 8_566 3_565 95.28(7)
I4 Pb2 I3 7_666 3_565 93.46(7)
I4 Pb2 I3 9_556 3_565 178.04(8)
I4 Pb2 I3 8_566 2_665 178.04(8)
I4 Pb2 I3 7_666 2_665 95.28(8)
I4 Pb2 I3 9_556 2_665 93.46(7)
I3 Pb2 I3 3_565 2_665 86.68(6)
I4 Pb2 I3 8_566 . 93.46(7)
I4 Pb2 I3 7_666 . 178.04(8)
I4 Pb2 I3 9_556 . 95.28(8)
I3 Pb2 I3 3_565 . 86.68(6)
I3 Pb2 I3 2_665 . 86.68(6)
Pb2 I3 Pb2 10_557 . 75.16(8)
Pb2 I4 Pb2 4_665 7_666 78.04(7)
Pb1 I5 Pb1 . 4 76.54(5)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C3 N1 . 1.45(6)
C3 N1 10_557 1.45(6)
N1 C1 . 1.16(5)
C1 C1 10_557 1.28(8)
Pb1 I5 9_556 3.2342(18)
Pb1 I5 3 3.2342(18)
Pb1 I5 7_556 3.2342(18)
Pb1 I5 2 3.2342(18)
Pb1 I5 8_556 3.2342(18)
Pb1 I5 . 3.2342(18)
Pb2 I4 8_566 3.225(2)
Pb2 I4 7_666 3.225(2)
Pb2 I4 9_556 3.225(2)
Pb2 I3 3_565 3.240(3)
Pb2 I3 2_665 3.240(3)
Pb2 I3 . 3.240(3)
I3 Pb2 10_557 3.240(3)
I4 Pb2 4_665 3.225(2)
I4 Pb2 7_666 3.225(2)
I5 Pb1 4 3.2342(18)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C3 H3 I4 . 0.93 3.23 3.73(5) 115.6
C3 H3 I4 3_665 0.93 2.95 3.81(5) 155.3
N1 H1 I3 8_556 0.86 3.23 3.95(6) 142.8

_cod_database_fobs_code 2107272
