#------------------------------------------------------------------------------
#$Date: 2019-11-24 17:14:38 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238763 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/79/7237941.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_7237941
loop_
_publ_author_name
'García-Fernández, Alberto'
'Juarez-Perez, Emilio Jose'
'Bermúdez-García, Juan Manuel'
'Llamas-Saiz, Antonio Luis'
'Artiaga, Ramón'
'López-Beceiro, Jorge Jose'
'Señarís-Rodríguez, María Antonia'
'Sánchez-Andújar, Manuel'
'Castro-García, Socorro'
_publ_section_title
;
 Hybrid lead halide [(CH3)2NH2]PbX3 (X = Cl− and Br−)
 hexagonal perovskites with multiple functional properties
;
_journal_issue                   32
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              10008
_journal_paper_doi               10.1039/C9TC03543E
_journal_volume                  7
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'Br6 Pb2, 2(C2 H8 N)'
_chemical_formula_sum            'C4 H16 Br6 N2 Pb2'
_chemical_formula_weight         986.03
_chemical_name_common            'DMAPbBr_B - 6_T100K'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2018-07-12 deposited with the CCDC.	2019-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.7631(4)
_cell_length_b                   13.9568(6)
_cell_length_c                   14.7110(7)
_cell_measurement_reflns_used    5426
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      26.2068
_cell_measurement_theta_min      2.7052
_cell_volume                     1799.23(14)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_data_collection       'Bruker APEX3 software'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2017)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 883)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 16.6666
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'κ--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker AXS X8 APEX-II'
_diffrn_measurement_method       'φ or ω oscillation scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2072
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23098
_diffrn_reflns_theta_full        25.41
_diffrn_reflns_theta_max         25.41
_diffrn_reflns_theta_min         2.01
_diffrn_source                   'sealed x-ray tube'
_diffrn_source_type              'SIEMENS KFN MO 2K-90'
_exptl_absorpt_coefficient_mu    31.990
_exptl_absorpt_correction_T_max  0.0613
_exptl_absorpt_correction_T_min  0.0233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'TWINABS - Bruker AXS scaling for twinned crystals - Version 2012/1'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    3.640
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DMF'
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_refine_diff_density_max         4.214
_refine_diff_density_min         -2.844
_refine_ls_abs_structure_details
;

Flack x determined using 1132 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         23098
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1360
_refine_ls_R_factor_gt           0.0979
_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)+(0.1440P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2229
_refine_ls_wR_factor_ref         0.2577
_reflns_number_gt                16852
_reflns_number_total             23098
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9tc03543e2.cif
_cod_data_source_block           6_T100K_2016cg06
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7237941
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, 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_refinement_flags_adp
_atom_site_refinement_flags_posn
_atom_site_occupancy
Pb Pb1 0.2856(3) 0.31814(15) 0.37896(15) 0.0158(6) Uani d . . 1
Pb Pb2 0.3042(3) 0.33463(15) 0.11133(15) 0.0158(6) Uani d . . 1
Br Br1 0.0269(8) 0.2217(5) 0.4773(5) 0.0232(16) Uani d . . 1
Br Br2 0.2689(8) 0.4991(4) 0.4668(4) 0.0217(15) Uani d . . 1
Br Br3 0.0863(7) 0.4146(5) 0.2448(5) 0.0197(14) Uani d . . 1
Br Br4 0.5312(7) 0.3965(5) 0.2580(5) 0.0215(15) Uani d . . 1
Br Br5 0.2975(8) 0.1620(4) 0.2148(4) 0.0203(14) Uani d . . 1
Br Br6 0.0722(8) 0.2488(6) -0.0117(5) 0.0293(17) Uani d . . 1
N N11 0.297(6) 0.642(4) 0.275(3) 0.024(11) Uani d . . 1
H H11A 0.376275 0.671304 0.303479 0.029 Uiso calc U R 1
H H11B 0.286387 0.582398 0.300404 0.029 Uiso calc U R 1
C C12 0.155(7) 0.697(5) 0.293(4) 0.027(16) Uani d . . 1
H H12A 0.135488 0.699567 0.358176 0.04 Uiso calc U R 1
H H12B 0.06936 0.666519 0.261743 0.04 Uiso calc U R 1
H H12C 0.168055 0.762654 0.269432 0.04 Uiso calc U R 1
C C13 0.331(7) 0.632(4) 0.179(4) 0.022(14) Uani d . . 1
H H13A 0.242358 0.604662 0.147515 0.033 Uiso calc U R 1
H H13B 0.418803 0.589005 0.171311 0.033 Uiso calc U R 1
H H13C 0.354924 0.694743 0.153351 0.033 Uiso calc U R 1
N N21 0.683(6) 0.501(4) 0.470(4) 0.027(13) Uani d . . 1
H H21A 0.612178 0.454568 0.462442 0.033 Uiso calc U R 1
H H21B 0.651642 0.553567 0.437863 0.033 Uiso calc U R 1
C C22 0.691(9) 0.528(5) 0.569(4) 0.034(17) Uani d . . 1
H H22A 0.77749 0.570502 0.579228 0.051 Uiso calc U R 1
H H22B 0.703545 0.469314 0.605261 0.051 Uiso calc U R 1
H H22C 0.596075 0.559922 0.586654 0.051 Uiso calc U R 1
C C23 0.831(7) 0.468(5) 0.432(5) 0.030(16) Uani d . . 1
H H23A 0.912056 0.513319 0.448019 0.045 Uiso calc U R 1
H H23B 0.823547 0.462994 0.365709 0.045 Uiso calc U R 1
H H23C 0.855979 0.404638 0.457337 0.045 Uiso calc U R 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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
Br2 Pb1 Br3 . . 82.44(19)
Br2 Pb1 Br4 . . 89.02(19)
Br3 Pb1 Br4 . . 82.08(19)
Br2 Pb1 Br1 . . 98.05(19)
Br3 Pb1 Br1 . . 94.55(19)
Br4 Pb1 Br1 . . 171.7(2)
Br2 Pb1 Br1 . 2_556 83.22(19)
Br3 Pb1 Br1 . 2_556 163.15(19)
Br4 Pb1 Br1 . 2_556 88.9(2)
Br1 Pb1 Br1 . 2_556 96.19(7)
Br5 Pb2 Br3 . . 87.19(19)
Br5 Pb2 Br6 . . 88.3(2)
Br3 Pb2 Br6 . . 96.6(2)
Br5 Pb2 Br6 . 2 87.1(2)
Br3 Pb2 Br6 . 2 167.2(2)
Br6 Pb2 Br6 . 2 94.67(6)
Br5 Pb2 Br4 . . 82.84(18)
Br3 Pb2 Br4 . . 81.08(18)
Br6 Pb2 Br4 . . 170.9(2)
Br6 Pb2 Br4 2 . 86.86(19)
Br5 Pb2 Br2 . 4_564 163.7(2)
Br3 Pb2 Br2 . 4_564 92.18(18)
Br6 Pb2 Br2 . 4_564 75.6(2)
Br6 Pb2 Br2 2 4_564 96.50(19)
Br4 Pb2 Br2 . 4_564 113.13(18)
Pb1 Br1 Pb1 . 2_456 160.1(2)
Pb1 Br2 Pb2 . 4_565 162.5(2)
Pb2 Br3 Pb1 . . 83.68(16)
Pb1 Br4 Pb2 . . 81.33(16)
Pb2 Br6 Pb2 . 2_455 171.0(3)
C13 N11 C12 . . 113.(5)
C13 N11 H11A . . 109.0
C12 N11 H11A . . 109.0
C13 N11 H11B . . 109.0
C12 N11 H11B . . 109.0
H11A N11 H11B . . 107.8
N11 C12 H12A . . 109.5
N11 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
N11 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
N11 C13 H13A . . 109.5
N11 C13 H13B . . 109.5
H13A C13 H13B . . 109.5
N11 C13 H13C . . 109.5
H13A C13 H13C . . 109.5
H13B C13 H13C . . 109.5
C23 N21 C22 . . 114.(6)
C23 N21 H21A . . 108.8
C22 N21 H21A . . 108.8
C23 N21 H21B . . 108.8
C22 N21 H21B . . 108.8
H21A N21 H21B . . 107.7
N21 C22 H22A . . 109.5
N21 C22 H22B . . 109.5
H22A C22 H22B . . 109.5
N21 C22 H22C . . 109.5
H22A C22 H22C . . 109.5
H22B C22 H22C . . 109.5
N21 C23 H23A . . 109.5
N21 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
N21 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pb1 Br2 . 2.841(6)
Pb1 Br3 . 2.959(7)
Pb1 Br4 . 2.998(7)
Pb1 Br1 . 3.007(7)
Pb1 Br1 2_556 3.042(7)
Pb2 Br5 . 2.851(6)
Pb2 Br3 . 2.958(7)
Pb2 Br6 . 2.974(7)
Pb2 Br6 2 3.003(7)
Pb2 Br4 . 3.059(7)
Pb2 Br2 4_564 3.212(6)
N11 C13 . 1.46(8)
N11 C12 . 1.48(7)
N11 H11A . 0.91
N11 H11B . 0.91
C12 H12A . 0.98
C12 H12B . 0.98
C12 H12C . 0.98
C13 H13A . 0.98
C13 H13B . 0.98
C13 H13C . 0.98
N21 C23 . 1.49(8)
N21 C22 . 1.50(8)
N21 H21A . 0.91
N21 H21B . 0.91
C22 H22A . 0.98
C22 H22B . 0.98
C22 H22C . 0.98
C23 H23A . 0.98
C23 H23B . 0.98
C23 H23C . 0.98
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
N11 H11B Br2 . 0.91 2.71 3.46(5) 139.4
N11 H11B Br3 . 0.91 3.04 3.69(5) 130.5
N11 H11B Br4 . 0.91 3.42 4.00(5) 123.7
N11 H11A Br4 3_655 0.91 3.37 3.89(5) 119.1
N11 H11A Br5 3_655 0.91 2.87 3.57(5) 134.5
N11 H11A Br6 4_565 0.91 2.97 3.67(5) 134.5
N21 H21A Br1 2_556 0.91 2.72 3.49(5) 143.0
N21 H21A Br2 . 0.91 3.07 3.63(6) 121.4
N21 H21A Br4 . 0.91 3.19 3.69(6) 116.7
N21 H21B Br5 3_655 0.91 2.74 3.53(5) 144.7
N21 H21B Br6 4_565 0.91 3.47 4.15(5) 134.2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
Br2 Pb1 Br1 Pb1 . 2_456 -17.5(8)
Br3 Pb1 Br1 Pb1 . 2_456 -100.5(8)
Br4 Pb1 Br1 Pb1 . 2_456 -166.1(11)
Br1 Pb1 Br1 Pb1 2_556 2_456 66.5(8)
Br3 Pb1 Br2 Pb2 . 4_565 113.8(8)
Br4 Pb1 Br2 Pb2 . 4_565 -164.0(8)
Br1 Pb1 Br2 Pb2 . 4_565 20.3(9)
Br1 Pb1 Br2 Pb2 2_556 4_565 -75.1(8)
Br5 Pb2 Br3 Pb1 . . 42.35(18)
Br6 Pb2 Br3 Pb1 . . 130.31(19)
Br6 Pb2 Br3 Pb1 2 . -21.1(10)
Br4 Pb2 Br3 Pb1 . . -40.83(16)
Br2 Pb2 Br3 Pb1 4_564 . -153.91(17)
Br2 Pb1 Br3 Pb2 . . 131.77(19)
Br4 Pb1 Br3 Pb2 . . 41.71(16)
Br1 Pb1 Br3 Pb2 . . -130.69(17)
Br1 Pb1 Br3 Pb2 2_556 . 99.8(7)
Br2 Pb1 Br4 Pb2 . . -122.82(18)
Br3 Pb1 Br4 Pb2 . . -40.31(16)
Br1 Pb1 Br4 Pb2 . . 26.1(15)
Br1 Pb1 Br4 Pb2 2_556 . 153.94(18)
Br5 Pb2 Br4 Pb1 . . -47.81(17)
Br3 Pb2 Br4 Pb1 . . 40.45(17)
Br6 Pb2 Br4 Pb1 . . -35.3(13)
Br6 Pb2 Br4 Pb1 2 . -135.3(2)
Br2 Pb2 Br4 Pb1 4_564 . 129.01(17)
Br5 Pb2 Br6 Pb2 . 2_455 70.(2)
Br3 Pb2 Br6 Pb2 . 2_455 -17.(2)
Br6 Pb2 Br6 Pb2 2 2_455 157.(2)
Br4 Pb2 Br6 Pb2 . 2_455 57.(3)
Br2 Pb2 Br6 Pb2 4_564 2_455 -108.(2)
