#------------------------------------------------------------------------------
#$Date: 2017-05-04 12:03:30 +0300 (Thu, 04 May 2017) $
#$Revision: 196000 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/58/4345838.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_4345838
loop_
_publ_author_name
'García-Fernández, A'
'Bermúdez-García, J M'
'Castro-García, S'
'Llamas-Saiz, A L'
'Artiaga, R.'
'López-Beceiro, J'
'Hu, S.'
'Ren, W.'
'Stroppa, A.'
'Sánchez-Andújar, M'
'Señarís-Rodríguez, M A'
_publ_section_title
;
 Phase Transition, Dielectric Properties, and Ionic Transport in the
 [(CH3)2NH2]PbI3 Organic-Inorganic Hybrid with 2H-Hexagonal Perovskite
 Structure.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4918
_journal_page_last               4927
_journal_paper_doi               10.1021/acs.inorgchem.6b03095
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C2 H8 I3 N Pb'
_chemical_formula_sum            'C2 H8 I3 N Pb'
_chemical_formula_weight         633.98
_chemical_name_systematic        DMAPbI3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     other
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2016-01-28T12:55:02-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 95.994(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9303(6)
_cell_length_b                   14.6910(9)
_cell_length_c                   7.9790(5)
_cell_measurement_reflns_used    1615
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      3.78
_cell_measurement_wavelength     0.71073
_cell_volume                     1041.08(12)
_computing_cell_refinement       'SAINT V8.34A integration software'
_computing_data_collection       'Bruker APEX2 software'
_computing_data_reduction        'SORTAV (Blessing, 1995)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_orient_matrix_UB_11      0.032928
_diffrn_orient_matrix_UB_12      -0.000062
_diffrn_orient_matrix_UB_13      -0.116002
_diffrn_orient_matrix_UB_21      -0.107468
_diffrn_orient_matrix_UB_22      0.004156
_diffrn_orient_matrix_UB_23      -0.04915
_diffrn_orient_matrix_UB_31      0.006604
_diffrn_orient_matrix_UB_32      0.067942
_diffrn_orient_matrix_UB_33      0.002901
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.083
_diffrn_reflns_av_unetI/netI     0.1175
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            52099
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.634
_diffrn_reflns_theta_min         2.293
_diffrn_source                   'sealed x-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    25.027
_exptl_absorpt_correction_T_max  0.084
_exptl_absorpt_correction_T_min  0.009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.045
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         5.125
_refine_diff_density_min         -3.603
_refine_diff_density_rms         0.638
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     68
_refine_ls_number_reflns         52099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.096
_refine_ls_R_factor_gt           0.073
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0513P)²+72.2747P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1901
_reflns_Friedel_coverage         0
_reflns_number_gt                40756
_reflns_number_total             52099
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b03095_si_003.cif
_cod_data_source_block           DMAPbI3LT
_cod_database_code               4345838
_shelx_estimated_absorpt_t_min   0.021
_shelx_estimated_absorpt_t_max   0.315
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Pb1 Pb 0.27276(11) 0.24550(6) 0.47417(10) 0.0142(2) Uani 1 1 d . .
I2 I 0.28046(19) 0.42139(12) 0.69098(18) 0.0166(4) Uani 1 1 d . .
I3 I 0.04096(19) 0.34945(12) 0.20902(19) 0.0180(4) Uani 1 1 d . .
I4 I 0.52725(19) 0.32625(12) 0.26937(19) 0.0193(4) Uani 1 1 d . .
N5 N 0.297(3) 0.5559(15) 0.299(2) 0.020(5) Uani 1 1 d . .
H5A H 0.3866 0.5739 0.3528 0.024 Uiso 1 1 calc R U
H5B H 0.2806 0.4972 0.3286 0.024 Uiso 1 1 calc R U
C6 C 0.304(3) 0.560(2) 0.114(3) 0.026(7) Uani 1 1 d . .
H6A H 0.3844 0.5201 0.0831 0.039 Uiso 1 1 calc R U
H6B H 0.3258 0.6231 0.0819 0.039 Uiso 1 1 calc R U
H6C H 0.2077 0.5411 0.0553 0.039 Uiso 1 1 calc R U
C7 C 0.175(3) 0.614(2) 0.353(3) 0.034(7) Uani 1 1 d . .
H7A H 0.1723 0.6722 0.2918 0.051 Uiso 1 1 calc R U
H7B H 0.1941 0.6262 0.4746 0.051 Uiso 1 1 calc R U
H7C H 0.0778 0.5833 0.3297 0.051 Uiso 1 1 calc R U
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 0 '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'
N N 0.0061 0.0033 '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
I2 Pb1 I4 90.02(5) . .
I2 Pb1 I3 86.92(5) . .
I4 Pb1 I3 85.95(5) . .
I2 Pb1 I3 90.82(5) . 4_566
I4 Pb1 I3 173.68(5) . 4_566
I3 Pb1 I3 100.35(6) . 4_566
I2 Pb1 I4 83.90(5) . 4_566
I4 Pb1 I4 90.58(5) . 4_566
I3 Pb1 I4 170.18(5) . 4_566
I3 Pb1 I4 83.28(5) 4_566 4_566
I2 Pb1 I2 170.62(5) . 4_565
I4 Pb1 I2 81.91(5) . 4_565
I3 Pb1 I2 87.74(4) . 4_565
I3 Pb1 I2 97.73(5) 4_566 4_565
I4 Pb1 I2 100.88(5) 4_566 4_565
Pb1 I2 Pb1 76.42(4) . 4_566
Pb1 I3 Pb1 76.62(4) . 4_565
Pb1 I4 Pb1 76.63(4) . 4_565
C6 N5 C7 112.1(19) . .
C6 N5 H5A 109.2 . .
C7 N5 H5A 109.2 . .
C6 N5 H5B 109.2 . .
C7 N5 H5B 109.2 . .
H5A N5 H5B 107.9 . .
N5 C6 H6A 109.5 . .
N5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
N5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N5 C7 H7A 109.5 . .
N5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
N5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pb1 I2 3.1065(18) .
Pb1 I4 3.1651(19) .
Pb1 I3 3.1904(18) .
Pb1 I3 3.2485(19) 4_566
Pb1 I4 3.2719(18) 4_566
Pb1 I2 3.3398(18) 4_565
I2 Pb1 3.3398(18) 4_566
I3 Pb1 3.2485(19) 4_565
I4 Pb1 3.2720(18) 4_565
N5 C6 1.48(3) .
N5 C7 1.49(3) .
N5 H5A 0.91 .
N5 H5B 0.91 .
C6 H6A 0.98 .
C6 H6B 0.98 .
C6 H6C 0.98 .
C7 H7A 0.98 .
C7 H7B 0.98 .
C7 H7C 0.98 .
