#------------------------------------------------------------------------------
#$Date: 2019-11-17 06:09:59 +0100 (dom 17 de nov de 2019) $
#$Revision: 228584 $
#$URL: svn://www.crystallography.net/cod/cif/1/54/91/1549184.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_1549184
loop_
_publ_author_name
'Xue, Chen'
'Yao, Zhi-Yuan'
'Zhang, Jin'
'Liu, Wen-Long'
'Liu, Jian-Lan'
'Ren, Xiao-Ming'
_publ_section_title
;
 Extra thermo- and water-stable one-dimensional organic-inorganic hybrid
 perovskite [N-methyldabconium]PbI₃ showing switchable
 dielectric behaviour, conductivity and bright yellow-green emission.
;
_journal_issue                   34
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4321
_journal_page_last               4324
_journal_paper_doi               10.1039/c8cc00786a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_sum            'C7 H15 I3 N2 Pb'
_chemical_formula_weight         715.10
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_symmetry_space_group_name_Hall  '-P 6c 2c'
_symmetry_space_group_name_H-M   'P 63/m m c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-01-28 deposited with the CCDC.
2018-04-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.4821(3)
_cell_length_b                   10.4821(3)
_cell_length_c                   8.1053(5)
_cell_measurement_reflns_used    371
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      27.443
_cell_measurement_theta_min      3.370
_cell_volume                     771.25(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0169
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6660
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.443
_diffrn_reflns_theta_min         3.370
_exptl_absorpt_coefficient_mu    16.913
_exptl_absorpt_correction_T_max  0.429
_exptl_absorpt_correction_T_min  0.308
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    3.079
_exptl_crystal_description       rod
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.557
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     25
_refine_ls_number_reflns         371
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0323
_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)+(0.0331P)²+2.3685P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0740
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                291
_reflns_number_total             371
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8cc00786a2.cif
_cod_data_source_block           2-auto
_cod_depositor_comments
'Adding full bibliography for 1549184--1549185.cif.'
_cod_original_cell_volume        771.25(7)
_cod_database_code               1549184
_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_res_file
;

    2-auto.res created by SHELXL-2014/7


TITL 2_a.res in P6(3)/mmc
CELL 0.71073 10.4821 10.4821 8.1053 90.000 90.000 120.000
ZERR 2.00 0.0003 0.0003 0.0005 0.000 0.000 0.000
LATT 1
SYMM x-y, x, z+1/2
SYMM y, -x+y, z+1/2
SYMM -y, x-y, z
SYMM -x+y, -x, z
SYMM x-y, -y, -z
SYMM -x, -x+y, -z
SYMM -x, -y, z+1/2
SYMM y, x, -z
SYMM -y, -x, -z+1/2
SYMM -x+y, y, -z+1/2
SYMM x, x-y, -z+1/2
SFAC C  H  N  I  Pb

UNIT 14 30 4 6 2
LIST 4
L.S. 20
ACTA
BOND $H
FMAP 2
Eqiv $1 1-x+y, 1-x, +z
EQIV $2 1-y, +x-y, +z
EQIV $3 1-y, 1-x, 1/2-z
PLAN -6
DFIX 1.5 0.1 C1 C1_$3
TEMP 100.000
WGHT    0.033100    2.368500
FVAR       0.40675
PB1   5    1.000000    1.000000    0.500000    10.08333    0.08335    0.08335 =
         0.04984    0.00000    0.00000    0.04167
I01   4    0.723753    0.861877    0.250000    10.25000    0.07753    0.13339 =
         0.08578    0.00000    0.00000    0.03877
simu C2 > N1
delu C2 > N1
SADI N1 C1 N1 C2 N1 C1_$1 C1_$2 N1
sadi C2 C1 C2 C1_$1 C2 C1_$2 C1 C1_$1 C1_$2 C1
part -1
C2    1    0.666677    0.333324    0.569190    10.08333    0.26057    0.26057 =
         0.42430    0.03649   -0.03649   -0.00843
AFIX   3
H2A   2    0.741198    0.313231    0.608698    10.08333   -1.50000
H2B   2    0.572048    0.258802    0.608664    10.08333   -1.50000
H2C   2    0.686769    0.427952    0.608648    10.08333   -1.50000
AFIX   0
part 0
C1    1    0.592881    0.407119    0.337255    10.50000    0.24817    0.24817 =
         0.44809   -0.02605    0.02605    0.19007
AFIX  23
H1A   2    0.492411    0.357566    0.377992    10.50000   -1.20000
H1B   2    0.642434    0.507589    0.377992    10.50000   -1.20000
AFIX   0
N1    3    0.666667    0.333333    0.393904    10.16667    0.16861    0.16861 =
         0.42439    0.00000    0.00000    0.08431
HKLF 4 1 1 0 0 0 1 0 0 0 1

REM  2_a.res in P6(3)/mmc
REM R1 =  0.0323 for     291 Fo > 4sig(Fo)  and  0.0461 for all     371 data
REM     25 parameters refined using     32 restraints

END

WGHT      0.0338      2.4217

REM Highest difference peak  0.460,  deepest hole -0.557,  1-sigma level  0.110
Q1    1   0.7890  0.9538  0.2500  10.50000  0.05    0.46
Q2    1   0.4669  0.2334  0.3588  10.50000  0.05    0.40
Q3    1   0.9645  0.9291  0.2500  10.25000  0.05    0.39
Q4    1   0.5677  0.4323  0.3912  10.50000  0.05    0.36
Q5    1   0.4012  0.2006  0.2500  10.25000  0.05    0.25
Q6    1   0.6663  0.8332  0.1700  10.50000  0.05    0.23
;
_shelx_res_checksum              96873
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'y, -x+y, z+1/2'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-x, -y, z+1/2'
'y, x, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'-y, x-y, -z-1/2'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'x, y, -z-1/2'
'-y, -x, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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
Pb1 Pb 1.0000 1.0000 0.5000 0.0722(4) Uani 1 12 d S T P . .
I01 I 0.72375(12) 0.86188(6) 0.2500 0.1051(5) Uani 1 4 d S T P . .
C2 C 0.667(2) 0.333(2) 0.569(3) 0.38(5) Uani 0.0833 1 d D U P A -1
H2A H 0.7412 0.3132 0.6087 0.565 Uiso 0.0833 1 d R U P A -1
H2B H 0.5720 0.2588 0.6087 0.565 Uiso 0.0833 1 d R U P A -1
H2C H 0.6868 0.4280 0.6086 0.565 Uiso 0.0833 1 d R U P A -1
C1 C 0.5929(8) 0.4071(8) 0.337(2) 0.285(16) Uani 1 2 d DS TU P A .
H1A H 0.4924 0.3576 0.3780 0.343 Uiso 0.5 1 calc R U P . .
H1B H 0.6424 0.5076 0.3780 0.343 Uiso 0.5 1 calc R U P . .
N1 N 0.6667 0.3333 0.394(2) 0.254(16) Uani 1 6 d DS TU P . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Pb1 0.0833(5) 0.0833(5) 0.0498(4) 0.000 0.000 0.0417(2)
I01 0.0775(7) 0.1334(8) 0.0858(7) 0.000 0.000 0.0388(3)
C2 0.26(7) 0.26(7) 0.42(5) 0.04(6) -0.04(6) -0.01(7)
C1 0.248(14) 0.248(14) 0.45(5) -0.026(8) 0.026(8) 0.190(15)
N1 0.169(11) 0.169(11) 0.42(5) 0.000 0.000 0.084(6)
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
I01 Pb1 I01 95.309(18) 13_776 15_766
I01 Pb1 I01 84.691(18) 13_776 3_565
I01 Pb1 I01 180.0 15_766 3_565
I01 Pb1 I01 84.691(18) 13_776 2_655
I01 Pb1 I01 95.309(18) 15_766 2_655
I01 Pb1 I01 84.691(18) 3_565 2_655
I01 Pb1 I01 95.309(18) 13_776 14_676
I01 Pb1 I01 84.691(18) 15_766 14_676
I01 Pb1 I01 95.309(18) 3_565 14_676
I01 Pb1 I01 180.00(3) 2_655 14_676
I01 Pb1 I01 180.00(3) 13_776 .
I01 Pb1 I01 84.691(18) 15_766 .
I01 Pb1 I01 95.309(18) 3_565 .
I01 Pb1 I01 95.309(18) 2_655 .
I01 Pb1 I01 84.691(18) 14_676 .
Pb1 I01 Pb1 77.88(2) . 2_654
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 . .
C1 C1 N1 108.9(7) 10_665 .
C1 C1 H1A 109.9 10_665 .
N1 C1 H1A 109.9 . .
C1 C1 H1B 109.9 10_665 .
N1 C1 H1B 109.9 . .
H1A C1 H1B 108.3 . .
C1 N1 C1 110.0(6) 4_655 5_665
C1 N1 C1 110.0(6) 4_655 .
C1 N1 C1 110.0(6) 5_665 .
C1 N1 C2 108.9(11) 4_655 .
C1 N1 C2 108.9(11) 5_665 .
C1 N1 C2 108.9(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I01 3.2240(8) 13_776
Pb1 I01 3.2240(8) 15_766
Pb1 I01 3.2240(8) 3_565
Pb1 I01 3.2240(8) 2_655
Pb1 I01 3.2240(8) 14_676
Pb1 I01 3.2241(8) .
I01 Pb1 3.2241(8) 2_654
C2 N1 1.42(2) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C1 C1 1.41(3) 10_665
C1 N1 1.416(17) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
N1 C1 1.416(17) 4_655
N1 C1 1.416(17) 5_665
