#------------------------------------------------------------------------------
#$Date: 2024-12-06 18:57:51 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296429 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/26/1572606.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_1572606
loop_
_publ_author_name
'Liu, Jiu-Yang'
'Lun, Meng-Meng'
'Wang, Zhi-Jie'
'Li, Jun-Yi'
'Ding, Kun'
'Fu, Da-Wei'
'Lu, Hai-Feng'
'Zhang, Yi'
_publ_section_title
;
 The H/F substitution strategy can achieve large spontaneous polarization
 in 1D hybrid perovskite ferroelectrics.
;
_journal_issue                   40
_journal_name_full               'Chemical science'
_journal_page_first              16612
_journal_page_last               16617
_journal_paper_doi               10.1039/d4sc03571b
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'Br5 Pb1.5, 2(C10 N)'
_chemical_formula_sum            'C20 Br5 N2 Pb1.5'
_chemical_formula_weight         978.56
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2024-04-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2024-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.990(14)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.110(3)
_cell_length_b                   9.6090(13)
_cell_length_c                   26.851(4)
_cell_measurement_reflns_used    1790
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.9200
_cell_measurement_theta_min      1.8880
_cell_volume                     5702.4(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -74.00 -10.00   0.50    1.00    --   20.00  54.00 -90.00  128
  2  ω     22.00  57.00   0.50    1.00    --   20.00  54.00 -90.00   70
  3  ω     80.00 105.00   0.50    1.00    --   20.00  54.00 -90.00   50
  4  ω    -53.00 103.00   0.50    1.00    --   20.00  54.00 120.00  312
  5  ω    -59.00   7.00   0.50    1.00    --   20.00  54.00  90.00  132
  6  ω     69.00  94.00   0.50    1.00    --   20.00  54.00  90.00   50
  7  ω    -32.00  -7.00   0.50    1.00    --   20.00  54.00-150.00   50
  8  ω     16.00  49.00   0.50    1.00    --   20.00  54.00-150.00   66
  9  ω    -63.00   1.00   0.50    1.00    --   20.00  54.00 -60.00  128
 10  ω    -32.00  46.00   0.50    1.00    --   20.00  54.00-180.00  156
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini II'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0271698000
_diffrn_orient_matrix_UB_12      0.0144498000
_diffrn_orient_matrix_UB_13      0.0199373000
_diffrn_orient_matrix_UB_21      -0.0169366000
_diffrn_orient_matrix_UB_22      0.0121837000
_diffrn_orient_matrix_UB_23      0.0177495000
_diffrn_orient_matrix_UB_31      0.0026238000
_diffrn_orient_matrix_UB_32      -0.0713562000
_diffrn_orient_matrix_UB_33      0.0070121000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1032
_diffrn_reflns_av_unetI/netI     0.1209
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            19381
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.843
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    15.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.10805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    2.280
_exptl_crystal_description       block
_exptl_crystal_F_000             3456
_refine_diff_density_max         1.683
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.260
_refine_ls_extinction_coef       0.00100(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     193
_refine_ls_number_reflns         5021
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.1246
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0559P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3063
_reflns_number_total             5021
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc03571b2.cif
_cod_data_source_block           (BTAB)PbBr3-293
_cod_depositor_comments
'Adding full bibliography for 1572604--1572606.cif.'
_cod_original_cell_volume        5702.4(13)
_cod_original_formula_sum        'C20 Br5 N2 Pb1.50'
_cod_database_code               1572606
_shelx_shelxl_version_number     2018/3
_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.
;
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Restrained distances
 Pb2-Br8
 3.2 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C11) = Uanis(C24) = Uanis(C12) = Uanis(C16) = Uanis(C13)
Uanis(C19) = Uanis(C37) = Uanis(C8)
3.a Fitted hexagon refined as free rotating group:
 C20(C14,C9,C17,C6,C10), C11(C24,C12,C16,C13,C5)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.606
_oxdiff_exptl_absorpt_empirical_full_min 0.378
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.500000 0.04926(9) 0.250000 0.0327(3) Uani 1 2 d S T P . .
Pb2 Pb 0.31941(2) 0.04807(6) 0.22010(2) 0.0307(2) Uani 1 1 d D . . . .
Br3 Br 0.23915(7) 0.03537(18) 0.11779(7) 0.0474(5) Uani 1 1 d . . . . .
Br4 Br 0.56931(7) 0.02711(19) 0.17068(6) 0.0464(5) Uani 1 1 d . . . . .
Br5 Br 0.39994(7) -0.14580(17) 0.18759(7) 0.0462(5) Uani 1 1 d . . . . .
Br6 Br 0.41051(7) 0.26109(17) 0.19476(7) 0.0484(5) Uani 1 1 d . . . . .
N7 N 0.0638(5) 0.0475(13) 0.1605(5) 0.037(3) Uani 1 1 d . . . . .
Br8 Br 0.25487(8) -0.18709(18) 0.25595(7) 0.0555(5) Uani 1 1 d D . . . .
C8 C 0.0700(9) -0.099(2) 0.1445(8) 0.077(4) Uani 1 1 d . . . . .
C15 C -0.0023(6) 0.0834(19) 0.1550(8) 0.066(6) Uani 1 1 d . . . . .
C20 C -0.0899(5) 0.2264(11) 0.0214(5) 0.068(6) Uani 1 1 d G . . . .
C14 C -0.0520(5) 0.2172(10) 0.0721(5) 0.055(5) Uani 1 1 d G . . . .
C9 C -0.0410(5) 0.0887(13) 0.0969(4) 0.055(5) Uani 1 1 d G . . . .
C17 C -0.0678(5) -0.0306(10) 0.0709(5) 0.077(7) Uani 1 1 d G . . . .
C6 C -0.1057(5) -0.0214(12) 0.0202(5) 0.066(6) Uani 1 1 d G . . . .
C10 C -0.1168(4) 0.1071(15) -0.0046(4) 0.058(5) Uani 1 1 d G . . . .
C37 C 0.0876(8) 0.153(2) 0.1276(8) 0.077(4) Uani 1 1 d . . . . .
C3 C 0.2671(7) 0.0856(16) -0.0839(7) 0.049(5) Uani 1 1 d . . . . .
C19 C 0.1019(9) 0.0656(19) 0.2164(8) 0.077(4) Uani 1 1 d . . . . .
N1 N 0.2493(5) -0.0616(13) -0.1053(5) 0.039(3) Uani 1 1 d . . . . .
C2 C 0.1942(7) -0.0474(19) -0.1528(7) 0.067(6) Uani 1 1 d . . . . .
C7 C 0.2997(7) -0.1240(19) -0.1233(7) 0.059(5) Uani 1 1 d . . . . .
C4 C 0.2355(7) -0.1503(19) -0.0643(7) 0.064(6) Uani 1 1 d . . . . .
C11 C 0.3182(4) 0.0885(12) 0.0124(5) 0.059(2) Uani 1 1 d G . . . .
C24 C 0.3692(6) 0.0938(12) 0.0555(3) 0.059(2) Uani 1 1 d G . . . .
C12 C 0.4264(4) 0.1039(12) 0.0487(4) 0.059(2) Uani 1 1 d G . . . .
C16 C 0.4326(4) 0.1087(11) -0.0012(5) 0.059(2) Uani 1 1 d G . . . .
C13 C 0.3817(6) 0.1034(11) -0.0443(3) 0.059(2) Uani 1 1 d G . . . .
C5 C 0.3244(4) 0.0933(12) -0.0375(4) 0.059(2) Uani 1 1 d G . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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
Br4 Pb1 Br4 171.93(8) . 2_655 ?
Br4 Pb1 Br5 92.41(5) 2_655 2_655 ?
Br4 Pb1 Br5 92.41(5) . . ?
Br4 Pb1 Br5 82.64(5) . 2_655 ?
Br4 Pb1 Br5 82.64(5) 2_655 . ?
Br5 Pb1 Br5 104.64(7) 2_655 . ?
Br6 Pb1 Br4 88.00(5) . 2_655 ?
Br6 Pb1 Br4 97.54(5) . . ?
Br6 Pb1 Br4 97.55(5) 2_655 2_655 ?
Br6 Pb1 Br4 88.00(5) 2_655 . ?
Br6 Pb1 Br5 80.92(5) . . ?
Br6 Pb1 Br5 174.43(5) . 2_655 ?
Br6 Pb1 Br5 174.43(5) 2_655 . ?
Br6 Pb1 Br5 80.92(5) 2_655 2_655 ?
Br6 Pb1 Br6 93.51(7) . 2_655 ?
Br3 Pb2 Br5 88.67(5) . . ?
Br3 Pb2 Br6 96.21(5) . . ?
Br3 Pb2 Br8 91.86(5) . . ?
Br3 Pb2 Br8 89.52(5) . 4 ?
Br5 Pb2 Br6 80.02(5) . . ?
Br5 Pb2 Br8 92.01(5) . . ?
Br5 Pb2 Br8 167.25(5) . 4 ?
Br6 Pb2 Br8 87.64(5) . 4 ?
Br8 Pb2 Br6 168.49(5) . . ?
Br8 Pb2 Br8 100.667(18) . 4 ?
Pb2 Br5 Pb1 83.81(4) . . ?
Pb1 Br6 Pb2 81.87(4) . . ?
C8 N7 C15 111.2(13) . . ?
C8 N7 C37 112.0(13) . . ?
C8 N7 C19 108.5(13) . . ?
C15 N7 C37 108.0(13) . . ?
C19 N7 C15 110.2(13) . . ?
C19 N7 C37 106.8(13) . . ?
Pb2 Br8 Pb2 173.06(7) . 4_545 ?
N7 C15 C9 111.6(13) . . ?
C14 C20 C10 120.0 . . ?
C20 C14 C9 120.0 . . ?
C14 C9 C15 118.7(11) . . ?
C17 C9 C15 121.1(11) . . ?
C17 C9 C14 120.0 . . ?
C9 C17 C6 120.0 . . ?
C10 C6 C17 120.0 . . ?
C6 C10 C20 120.0 . . ?
C5 C3 N1 115.0(11) . . ?
C2 N1 C3 107.4(12) . . ?
C7 N1 C3 109.7(12) . . ?
C7 N1 C2 107.6(13) . . ?
C4 N1 C3 109.9(13) . . ?
C4 N1 C2 111.2(12) . . ?
C4 N1 C7 111.0(13) . . ?
C24 C11 C5 120.0 . . ?
C11 C24 C12 120.0 . . ?
C16 C12 C24 120.0 . . ?
C13 C16 C12 120.0 . . ?
C16 C13 C5 120.0 . . ?
C11 C5 C3 118.3(11) . . ?
C13 C5 C3 121.7(11) . . ?
C13 C5 C11 120.0 . . ?
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 Br4 3.0234(16) . ?
Pb1 Br4 3.0236(16) 2_655 ?
Pb1 Br5 3.0665(17) . ?
Pb1 Br5 3.0665(17) 2_655 ?
Pb1 Br6 2.9712(17) 2_655 ?
Pb1 Br6 2.9712(17) . ?
Pb2 Br3 2.8325(18) . ?
Pb2 Br5 2.9403(16) . ?
Pb2 Br6 3.1499(18) . ?
Pb2 Br8 3.2376(17) 4 ?
Pb2 Br8 3.0161(18) . ?
N7 C8 1.49(2) . ?
N7 C15 1.531(17) . ?
N7 C37 1.55(2) . ?
N7 C19 1.51(2) . ?
C15 C9 1.56(2) . ?
C20 C14 1.3900 . ?
C20 C10 1.3900 . ?
C14 C9 1.3900 . ?
C9 C17 1.3900 . ?
C17 C6 1.3900 . ?
C6 C10 1.3900 . ?
C3 N1 1.537(18) . ?
C3 C5 1.533(17) . ?
N1 C2 1.522(18) . ?
N1 C7 1.510(17) . ?
N1 C4 1.499(18) . ?
C11 C24 1.3900 . ?
C11 C5 1.3900 . ?
C24 C12 1.3900 . ?
C12 C16 1.3900 . ?
C16 C13 1.3900 . ?
C13 C5 1.3900 . ?
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
N7 C15 C9 C14 -97.7(13) . . . . ?
N7 C15 C9 C17 87.0(14) . . . . ?
C8 N7 C15 C9 -68.7(18) . . . . ?
C15 C9 C17 C6 175.2(11) . . . . ?
C20 C14 C9 C15 -175.4(11) . . . . ?
C20 C14 C9 C17 0.0 . . . . ?
C14 C20 C10 C6 0.0 . . . . ?
C14 C9 C17 C6 0.0 . . . . ?
C9 C17 C6 C10 0.0 . . . . ?
C17 C6 C10 C20 0.0 . . . . ?
C10 C20 C14 C9 0.0 . . . . ?
C37 N7 C15 C9 54.6(17) . . . . ?
C19 N7 C15 C9 171.0(13) . . . . ?
N1 C3 C5 C11 -92.7(13) . . . . ?
N1 C3 C5 C13 86.7(14) . . . . ?
C11 C24 C12 C16 0.0 . . . . ?
C24 C11 C5 C3 179.3(11) . . . . ?
C24 C11 C5 C13 0.0 . . . . ?
C24 C12 C16 C13 0.0 . . . . ?
C12 C16 C13 C5 0.0 . . . . ?
C16 C13 C5 C3 -179.3(11) . . . . ?
C16 C13 C5 C11 0.0 . . . . ?
C5 C3 N1 C2 -176.6(13) . . . . ?
C5 C3 N1 C7 -60.0(17) . . . . ?
C5 C3 N1 C4 62.3(16) . . . . ?
C5 C11 C24 C12 0.0 . . . . ?
