#------------------------------------------------------------------------------
#$Date: 2022-05-03 02:12:52 +0300 (Tue, 03 May 2022) $
#$Revision: 274812 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/01/7710136.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_7710136
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         'Br7 Pb2, 4(C3 N)'
_chemical_formula_sum            'C12 Br7 N4 Pb2'
_chemical_formula_weight         1173.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_primary     direct
_audit_creation_date             2022-03-27
_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                90
_cell_formula_units_Z            2
_cell_length_a                   10.1747(9)
_cell_length_b                   15.8777(17)
_cell_length_c                   7.9470(5)
_cell_measurement_reflns_used    1359
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.4830
_cell_measurement_theta_min      2.0060
_cell_volume                     1283.8(2)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5349
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         2.002
_exptl_absorpt_coefficient_mu    23.994
_exptl_crystal_colour            color
_exptl_crystal_density_diffrn    3.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1018.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         6.759
_refine_diff_density_min         -1.852
_refine_diff_density_rms         0.595
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.598
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         1221
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.533
_refine_ls_R_factor_all          0.1625
_refine_ls_R_factor_gt           0.1243
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3871
_refine_ls_wR_factor_ref         0.4280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                664
_reflns_number_total             1222
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2dt01040b2.cif
_cod_data_source_block           t_CCDC1
_cod_database_code               7710136
_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. Restrained distances
 N1A-N2A
 1.55 with sigma of 0.05
 N1A-C1
 1.55 with sigma of 0.05
 C1-C2A
 1.55 with sigma of 0.05
 C3-C2A
 1.55 with sigma of 0.05
 N2A-C3
 1.55 with sigma of 0.05
 N2A-C2A
 2.5 with sigma of 0.05
 N1A-C2A
 2.5 with sigma of 0.05
 N1-N2
 1.55 with sigma of 0.05
 N1-C1
 1.55 with sigma of 0.05
 C1-C2
 1.55 with sigma of 0.05
 C3-C2
 1.55 with sigma of 0.05
 C3-N2
 1.55 with sigma of 0.05
 N1-C2
 2.5 with sigma of 0.05
2. Rigid bond restraints
 N1, N2, C2, N1A, N2A, C2A, C3, C1
 with sigma for 1-2 distances of 0.05 and sigma for 1-3 distances of 0.05
3. Uiso/Uaniso restraints and constraints
N1 \\sim N2 \\sim C2 \\sim N1A \\sim N2A \\sim C2A \\sim C3 \\sim C1: within 2A
with sigma of 0.05 and sigma for terminal atoms of 0.1 within 2A
4. Others
 Sof(C2A)=1-FVAR(1)
 Sof(N1A)=Sof(N2A)=0.5*(1-FVAR(2))
 Sof(N1)=Sof(N2)=0.5*FVAR(2)
 Sof(C2)=FVAR(1)
 Fixed Sof: Br2(0.25)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x, y-1/2, 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 0.18999(7) 0.250000 0.500000 0.0820(3) Uani 1 2 d S T P . .
Br1 Br -0.0036(3) 0.1790(3) 0.250000 0.1852(15) Uani 1 2 d S T P . .
Br2 Br 0.4316(5) 0.250000 0.000000 0.0842(14) Uani 0.5 2 d S T P . .
Br3 Br 0.1916(4) 0.3934(3) 0.250000 0.1567(18) Uani 1 2 d S T P . .
Br4 Br 0.3832(3) 0.1739(2) 0.250000 0.1458(12) Uani 1 2 d S T P . .
N1 N 0.285(2) 0.835(2) 0.250000 0.250(9) Uani 0.58(3) 2 d DS TU P A 1
N2 N 0.146(3) 0.867(2) 0.250000 0.258(10) Uani 0.58(3) 2 d DS TU P A 1
C2 C 0.335(3) 0.932(2) 0.477(3) 0.259(8) Uani 0.58(3) 1 d D U P A 1
N1A N 0.387(3) 0.9801(16) 0.250000 0.264(9) Uani 0.42(3) 2 d DS TU P A 2
N2A N 0.237(3) 0.990(2) 0.250000 0.257(10) Uani 0.42(3) 2 d DS TU P A 2
C2A C 0.298(3) 0.8711(16) 0.448(3) 0.254(8) Uani 0.42(3) 1 d D U P A 2
C1 C 0.402(2) 0.8895(13) 0.316(2) 0.258(7) Uani 1 1 d D U . . .
C3 C 0.192(2) 0.9322(15) 0.389(3) 0.252(7) Uani 1 1 d D 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 0.0000 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Br1 Pb1 Br1 98.47(12) 7_566 . ?
Br1 Pb1 Br3 98.91(9) . 7_566 ?
Br1 Pb1 Br3 81.51(9) . . ?
Br1 Pb1 Br3 81.51(9) 7_566 7_566 ?
Br1 Pb1 Br3 98.91(9) 7_566 . ?
Br1 Pb1 Br4 80.99(8) 7_566 7_566 ?
Br1 Pb1 Br4 178.57(10) . 7_566 ?
Br1 Pb1 Br4 81.00(8) . . ?
Br1 Pb1 Br4 178.57(10) 7_566 . ?
Br2 Pb1 Br1 130.77(6) 6_556 . ?
Br2 Pb1 Br1 130.77(6) 6_556 7_566 ?
Br2 Pb1 Br3 89.68(7) 6_556 . ?
Br2 Pb1 Br3 89.68(7) 6_556 7_566 ?
Br2 Pb1 Br4 49.79(5) 6_556 7_566 ?
Br2 Pb1 Br4 49.79(5) 6_556 . ?
Br3 Pb1 Br3 179.36(15) . 7_566 ?
Br3 Pb1 Br4 82.33(8) 7_566 7_566 ?
Br3 Pb1 Br4 97.25(8) . 7_566 ?
Br3 Pb1 Br4 97.25(8) 7_566 . ?
Br3 Pb1 Br4 82.33(8) . . ?
Br4 Pb1 Br4 99.57(11) 7_566 . ?
Pb1 Br1 Pb1 82.39(8) 6_556 . ?
Br4 Br2 Pb1 78.05(13) 7_565 6_556 ?
Br4 Br2 Pb1 78.05(13) . 6_556 ?
Br4 Br2 Br4 156.1(3) 7_565 . ?
Pb1 Br3 Pb1 82.22(10) 6_556 . ?
Pb1 Br4 Pb1 81.44(8) . 6_556 ?
Br2 Br4 Pb1 118.49(15) 6_556 6_556 ?
Br2 Br4 Pb1 118.49(15) . . ?
Br2 Br4 Pb1 52.17(12) . 6_556 ?
Br2 Br4 Pb1 52.17(12) 6_556 . ?
Br2 Br4 Br2 113.39(17) 6_556 . ?
N2 N1 C1 122(2) . 6_556 ?
N2 N1 C1 122(2) . . ?
C1 N1 C1 39.0(15) 6_556 . ?
N1 N2 C3 86.5(19) . 6_556 ?
N1 N2 C3 86.5(19) . . ?
C3 N2 C3 88(2) 6_556 . ?
C1 C2 C3 92.3(17) . . ?
C1 N1A N2A 101(2) 6_556 . ?
C1 N1A N2A 101(2) . . ?
C1 N1A C1 39.6(15) . 6_556 ?
C3 N2A N1A 104.0(17) 6_556 . ?
C3 N2A N1A 104.0(17) . . ?
C3 N2A C3 94(2) . 6_556 ?
C1 C2A C3 98.9(18) . . ?
N1 C1 C2 99.8(17) . . ?
C2A C1 N1A 110.0(18) . . ?
C1 C1 N1 70.5(8) 6_556 . ?
C1 C1 C2 143.1(14) 6_556 . ?
C1 C1 N1A 70.2(8) 6_556 . ?
C1 C1 C2A 133.7(14) 6_556 . ?
N2 C3 C2 125(2) . . ?
N2A C3 C2A 114(2) . . ?
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 3.017(3) 7_566 ?
Pb1 Br1 3.017(3) . ?
Pb1 Br2 2.459(5) 6_556 ?
Pb1 Br3 3.022(3) 7_566 ?
Pb1 Br3 3.022(3) . ?
Pb1 Br4 3.046(2) 7_566 ?
Pb1 Br4 3.046(2) . ?
Br2 Br4 2.377(2) 7_565 ?
Br2 Br4 2.377(2) . ?
N1 N2 1.51(3) . ?
N1 C1 1.56(3) 6_556 ?
N1 C1 1.56(3) . ?
N2 C3 1.58(3) 6_556 ?
N2 C3 1.58(3) . ?
C2 C1 1.60(3) . ?
C2 C3 1.61(3) . ?
N1A N2A 1.53(3) . ?
N1A C1 1.54(3) 6_556 ?
N1A C1 1.54(3) . ?
N2A C3 1.50(3) . ?
N2A C3 1.50(3) 6_556 ?
C2A C1 1.52(3) . ?
C2A C3 1.52(3) . ?
C1 C1 1.04(4) 6_556 ?
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 N2 C3 C2 -7(3) . . . . ?
N2 N1 C1 C2 40(2) . . . . ?
N2 N1 C1 C1 -102.8(14) . . . 6_556 ?
N1A N2A C3 C2A -14(3) . . . . ?
N2A N1A C1 C2A -36.4(19) . . . . ?
N2A N1A C1 C1 94.1(8) . . . 6_556 ?
C1 N1 N2 C3 67.5(16) . . . 6_556 ?
C1 N1 N2 C3 -21.1(18) . . . . ?
C1 N1 N2 C3 21.1(18) 6_556 . . 6_556 ?
C1 N1 N2 C3 -67.5(16) 6_556 . . . ?
C1 N1 C1 C2 143.1(15) 6_556 . . . ?
C1 C2 C3 N2 28(3) . . . . ?
C1 N1A N2A C3 -69.4(16) . . . 6_556 ?
C1 N1A N2A C3 -28.9(18) 6_556 . . 6_556 ?
C1 N1A N2A C3 69.4(16) 6_556 . . . ?
C1 N1A N2A C3 28.9(18) . . . . ?
C1 N1A C1 C2A -130.5(15) 6_556 . . . ?
C1 C2A C3 N2A -7(3) . . . . ?
C3 N2 C3 C2 -94(3) 6_556 . . . ?
C3 C2 C1 N1 -32(2) . . . . ?
C3 C2 C1 C1 39(3) . . . 6_556 ?
C3 N2A C3 C2A 91(2) 6_556 . . . ?
C3 C2A C1 N1A 27(2) . . . . ?
C3 C2A C1 C1 -54(2) . . . 6_556 ?
