#------------------------------------------------------------------------------
#$Date: 2022-05-03 01:12:52 +0200 (mar 03 de may de 2022) $
#$Revision: 274812 $
#$URL: svn://www.crystallography.net/cod/cif/7/71/01/7710135.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_7710135
loop_
_publ_author_name
'Han, Keke'
'Wei, Zhenhong'
'Ye, Xing'
'Li, Bo'
'Wang, Pan'
'Cai, Hu'
_publ_section_title
;
 A lead bromide organic-inorganic hybrid perovskite material showing
 reversible dual phase transition and robust SHG switching
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01040B
_journal_year                    2022
_chemical_formula_moiety         '2(C3 N), Br3 Pb'
_chemical_formula_sum            'C6 Br3 N2 Pb'
_chemical_formula_weight         546.98
_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'
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-03-24
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-03-30 deposited with the CCDC.	2022-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.7659(16)
_cell_length_b                   9.7659(16)
_cell_length_c                   7.9042(7)
_cell_measurement_reflns_used    473
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.2560
_cell_measurement_theta_min      2.4070
_cell_volume                     652.85(16)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1012
_diffrn_reflns_av_unetI/netI     0.0595
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2622
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.688
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    22.058
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            color
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_description       block
_exptl_crystal_F_000             474
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.430
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     14
_refine_ls_number_reflns         385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.430
_refine_ls_R_factor_all          0.3405
_refine_ls_R_factor_gt           0.1935
_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)+(0.0599P)²+11.3213P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3019
_refine_ls_wR_factor_ref         0.3389
_reflns_Friedel_coverage         0.000
_reflns_number_gt                156
_reflns_number_total             419
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01040b2.cif
_cod_data_source_block           t
_cod_original_cell_volume        652.8(2)
_cod_database_code               7710135
_shelx_shelxl_version_number     2017/1
_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.
;
_olex2_refinement_description
;
1. Others
 Fixed Sof: N1(0.16667) C1(0.33333)
;
_shelx_res_file
;
TITL t R = New: P63/mmc
    t.res
    created by SHELXL-2017/1 at 21:57:40 on 23-Mar-2022
CELL 0.71073 9.7659 9.7659 7.9042 90 90 120
ZERR 2 0.0016 0.0016 0.0007 0 0 0
LATT 1
SYMM -Y+X,+X,0.5+Z
SYMM -Y,+X-Y,+Z
SYMM -X,-Y,0.5+Z
SYMM +Y-X,-X,+Z
SYMM +Y,-X+Y,0.5+Z
SYMM -Y,-X,0.5-Z
SYMM -Y+X,-Y,-Z
SYMM +X,+X-Y,0.5-Z
SYMM +Y,+X,-Z
SYMM +Y-X,+Y,0.5-Z
SYMM -X,-X+Y,-Z
SFAC C Br N Pb
UNIT 16 6 6 2

L.S. 15
PLAN  2
CONF
fmap 2
acta
MORE -1
REM <olex2.extras>
REM <HklSrc "%.\\t.hkl">
REM </olex2.extras>

WGHT    0.059900   11.321301
FVAR       0.52540
PB1   4    1.000000    1.000000    0.500000    10.08333    0.23814    0.23814 =
         0.07181    0.00000    0.00000    0.11907
BR1   2    0.731610    0.865805    0.750000    10.25000    0.22854    0.41900 =
         0.14781    0.00000    0.00000    0.11427
N1    3    0.270161    0.729839    1.250000    10.16667    0.35156
C1    1    0.407804    0.815607    1.102076    10.33333    0.34413
C2    1    0.333333    0.666667    1.044236    10.16667    0.41445
HKLF 4




REM  t R = New: P63/mmc
REM R1 =  0.1935 for     156 Fo > 4sig(Fo)  and  0.3405 for all     385 data
REM     14 parameters refined using      0 restraints

END

WGHT      0.0599     11.3203

REM Highest difference peak  0.716,  deepest hole -0.688,  1-sigma level  0.125
Q1    1   1.0000  1.0000  0.6527  10.16667  0.05    0.72
Q2    1   1.0531  0.9469  0.5987  10.50000  0.05    0.64
;
_shelx_res_checksum              29800
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x-y, x, z+1/2'
'-y, x-y, z'
'-x, -y, z+1/2'
'-x+y, -x, z'
'y, -x+y, z+1/2'
'-y, -x, -z+1/2'
'x-y, -y, -z'
'x, x-y, -z+1/2'
'y, x, -z'
'-x+y, y, -z+1/2'
'-x, -x+y, -z'
'-x, -y, -z'
'-x+y, -x, -z-1/2'
'y, -x+y, -z'
'x, y, -z-1/2'
'x-y, x, -z'
'-y, x-y, -z-1/2'
'y, x, z-1/2'
'-x+y, y, z'
'-x, -x+y, z-1/2'
'-y, -x, z'
'x-y, -y, z-1/2'
'x, x-y, z'
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 1.000000 1.000000 0.500000 0.183(3) Uani 1 12 d S T P . .
Br1 Br 0.7316(14) 0.8658(7) 0.750000 0.286(7) Uani 1 4 d S T P . .
N1 N 0.270(9) 0.730(9) 1.250000 0.35(10) Uiso 0.6667 4 d S . P . .
C1 C 0.408(8) 0.816(16) 1.102(14) 0.34(7) Uiso 0.6667 2 d S . P . .
C2 C 0.333333 0.666667 1.04(3) 0.41(13) Uiso 1 6 d S . 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 0.238(5) 0.238(5) 0.072(2) 0.000 0.000 0.119(2)
Br1 0.229(11) 0.419(16) 0.148(6) 0.000 0.000 0.114(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'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
Br1 Pb1 Br1 180.0 14_677 2_654 ?
Br1 Pb1 Br1 98.4(2) 2_654 . ?
Br1 Pb1 Br1 98.4(2) 14_677 15_566 ?
Br1 Pb1 Br1 98.4(2) . 15_566 ?
Br1 Pb1 Br1 180.0 13_776 . ?
Br1 Pb1 Br1 81.6(2) . 3_765 ?
Br1 Pb1 Br1 81.6(2) 14_677 3_765 ?
Br1 Pb1 Br1 98.4(2) 14_677 13_776 ?
Br1 Pb1 Br1 98.4(2) 13_776 3_765 ?
Br1 Pb1 Br1 98.4(2) 2_654 3_765 ?
Br1 Pb1 Br1 180.0 15_566 3_765 ?
Br1 Pb1 Br1 81.6(2) 2_654 13_776 ?
Br1 Pb1 Br1 81.6(2) 2_654 15_566 ?
Br1 Pb1 Br1 81.6(2) 13_776 15_566 ?
Br1 Pb1 Br1 81.6(2) 14_677 . ?
Pb1 Br1 Pb1 82.1(3) 2_655 . ?
N1 N1 N1 60.00(6) 3_665 14_568 ?
N1 N1 C2 62(5) 3_665 . ?
N1 N1 C2 62(5) 14_568 14_568 ?
N1 N1 C2 62(5) 3_665 14_568 ?
N1 N1 C2 62(5) 14_568 . ?
C1 N1 N1 56(6) 16_558 14_568 ?
C1 N1 N1 56(6) 18_668 3_665 ?
C1 N1 N1 96(7) 16_558 3_665 ?
C1 N1 N1 96(7) 18_668 14_568 ?
C1 N1 N1 56(6) . 14_568 ?
C1 N1 N1 96(7) . 3_665 ?
C1 N1 N1 96(7) 3_665 14_568 ?
C1 N1 N1 56(6) 3_665 3_665 ?
C1 N1 C1 82(9) 16_558 18_668 ?
C1 N1 C1 90(7) 3_665 18_668 ?
C1 N1 C1 82(9) . 3_665 ?
C1 N1 C1 90(7) 16_558 . ?
C1 N1 C1 149(10) . 18_668 ?
C1 N1 C1 149(10) 16_558 3_665 ?
C1 N1 C2 43(5) . . ?
C1 N1 C2 116(7) 18_668 . ?
C1 N1 C2 116(7) 3_665 14_568 ?
C1 N1 C2 43(5) 18_668 14_568 ?
C1 N1 C2 116(7) . 14_568 ?
C1 N1 C2 116(7) 16_558 . ?
C1 N1 C2 43(5) 16_558 14_568 ?
C1 N1 C2 43(5) 3_665 . ?
C2 N1 C2 113(10) . 14_568 ?
N1 C1 N1 68(10) . 14_568 ?
C2 C1 N1 80(10) . 14_568 ?
C2 C1 N1 80(10) . . ?
N1 C2 N1 57(9) . 3_665 ?
N1 C2 N1 57(9) 14_568 3_665 ?
N1 C2 N1 57(9) . 14_568 ?
C1 C2 N1 57(10) . . ?
C1 C2 N1 57(10) 3_665 3_665 ?
C1 C2 N1 57(10) . 14_568 ?
C1 C2 N1 103(10) . 3_665 ?
C1 C2 N1 57(10) 3_665 . ?
C1 C2 N1 57(10) 5_565 3_665 ?
C1 C2 N1 103(10) 5_565 . ?
C1 C2 N1 103(10) 3_665 14_568 ?
C1 C2 N1 57(10) 5_565 14_568 ?
C1 C2 C1 109(10) . 3_665 ?
C1 C2 C1 109(10) . 5_565 ?
C1 C2 C1 109(10) 3_665 5_565 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 Br1 3.010(9) 14_677 ?
Pb1 Br1 3.010(9) 15_566 ?
Pb1 Br1 3.010(9) 13_776 ?
Pb1 Br1 3.010(9) 3_765 ?
Pb1 Br1 3.010(9) . ?
Pb1 Br1 3.010(9) 2_654 ?
N1 N1 1.9(3) 14_568 ?
N1 N1 1.9(3) 3_665 ?
N1 C1 1.66(10) 3_665 ?
N1 C1 1.66(10) 18_668 ?
N1 C1 1.66(10) . ?
N1 C1 1.66(10) 16_558 ?
N1 C2 1.9(2) . ?
N1 C2 1.9(2) 14_568 ?
C1 C2 1.34(15) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 N1 C1 N1 -48(4) 3_665 . . 14_568 ?
N1 N1 C1 C2 83(8) 14_568 . . . ?
N1 N1 C1 C2 36(8) 3_665 . . . ?
N1 C1 C2 N1 69(10) 14_568 . . . ?
N1 C1 C2 N1 -69(10) . . . 14_568 ?
N1 C1 C2 N1 34(5) 14_568 . . 3_665 ?
N1 C1 C2 N1 -34(5) . . . 3_665 ?
N1 C1 C2 C1 -25(18) 14_568 . . 5_565 ?
N1 C1 C2 C1 94(17) 14_568 . . 3_665 ?
N1 C1 C2 C1 -94(17) . . . 5_565 ?
N1 C1 C2 C1 25(18) . . . 3_665 ?
C1 N1 C1 N1 -102(4) 3_665 . . 14_568 ?
C1 N1 C1 N1 -26(3) 18_668 . . 14_568 ?
C1 N1 C1 N1 48(10) 16_558 . . 14_568 ?
C1 N1 C1 C2 57(7) 18_668 . . . ?
C1 N1 C1 C2 -19(10) 3_665 . . . ?
C1 N1 C1 C2 131(10) 16_558 . . . ?
C2 N1 C1 N1 13(10) 14_568 . . 14_568 ?
C2 N1 C1 N1 -83(8) . . . 14_568 ?
C2 N1 C1 C2 97(12) 14_568 . . . ?
