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#$Date: 2025-04-05 05:34:10 +0300 (Sat, 05 Apr 2025) $
#$Revision: 298836 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/99/7249975.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_7249975
loop_
_publ_author_name
'Fan, Chang-Chun'
'Fang, Zi-Han'
'Jiao, Shu-Lin'
'Yu, Jing-Xue'
'Liu, Cheng-Dong'
'Wang, Wei'
'Jin, Ming-Liang'
'Liang, Bei-Dou'
'Han, Xiang-Bin'
_publ_section_title
;
 Enhanced luminescence in 1D corrugated lead bromides via reduced
 flexibility of trivalent cations
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              1997
_journal_page_last               2003
_journal_paper_doi               10.1039/D5CE00003C
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'Br5 Pb, 0.5(H4 O2), C7 H20 N3'
_chemical_formula_sum            'C7 H22 Br5 N3 O Pb'
_chemical_formula_weight         771.01
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-21 deposited with the CCDC.	2025-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.9020(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.2495(2)
_cell_length_b                   8.7968(2)
_cell_length_c                   10.3341(2)
_cell_measurement_reflns_used    4042
_cell_measurement_temperature    282.00
_cell_measurement_theta_max      68.112
_cell_measurement_theta_min      4.372
_cell_volume                     911.72(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      282.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7544
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.233
_diffrn_reflns_theta_min         4.372
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    30.770
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.5335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0924 before and 0.0522 after correction.
The Ratio of minimum to maximum transmission is 0.7084.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic light white'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    2.809
_exptl_crystal_description       plate
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.926
_refine_diff_density_min         -1.074
_refine_diff_density_rms         0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1786
_refine_ls_number_restraints     61
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0301
_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)+(0.0120P)²+3.5358P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1676
_reflns_number_total             1786
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d5ce00003c2.cif
_cod_data_source_block           MPMA
_cod_depositor_comments
'Adding full bibliography for 7249974--7249975.cif.'
_cod_database_code               7249975
_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.
;
_shelx_estimated_absorpt_t_max   0.063
_shelx_estimated_absorpt_t_min   0.063
_olex2_refinement_description
;
1. Restrained distances
 C3-C4
 2.5 with sigma of 0.01
 C5-C4
 1.53 with sigma of 0.01
 N3-C5
 1.49 with sigma of 0.01
 C5-N2
 2.48 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(N2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N1, N2, C1, C2, C3, N3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: H1D(0.5) H1E(0.5) H1A(0.5) H1B(0.5) H1C(0.5) N3(0.5) H3C(0.5)
 H3D(0.5) H3E(0.5) C4(0.5) H4A(0.5) H4B(0.5) C5(0.5) H5A(0.5) H5B(0.5)
5.a Free rotating group:
 O1(H1D,H1E)
5.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B)
5.d Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
5.e Idealised Me refined as rotating group:
 N3(H3C,H3D,H3E)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'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 0.18836(3) 0.750000 0.59911(3) 0.02549(12) Uani 1 2 d S T P . .
Br1 Br 0.11352(9) 0.750000 0.87535(9) 0.0435(2) Uani 1 2 d S T P . .
Br2 Br 0.41393(7) 0.52807(8) 0.70488(7) 0.04535(19) Uani 1 1 d . . . . .
Br3 Br 0.26515(10) 0.750000 0.33886(9) 0.0425(2) Uani 1 2 d S T P . .
Br4 Br 0.000000 1.000000 0.500000 0.0533(3) Uani 1 2 d S . P . .
O1 O 0.5795(7) 1.250000 0.9333(8) 0.0564(18) Uani 1 2 d GS T P . .
H1D H 0.611625 1.286067 0.870302 0.085 Uiso 0.5 1 d G U P . .
H1E H 0.642405 1.216409 0.993342 0.085 Uiso 0.5 1 d G U P . .
N1 N 0.7261(9) 0.750000 1.0889(7) 0.0438(17) Uani 1 2 d S T P . .
H1 H 0.668651 0.749999 1.153851 0.053 Uiso 1 2 calc R U P . .
N2 N 0.7132(8) 0.750000 0.8048(7) 0.063(2) Uani 1 2 d DS TU P . .
H2 H 0.615532 0.749999 0.780839 0.075 Uiso 1 2 calc R U P B .
C1 C 0.8688(15) 0.750000 1.1654(13) 0.079(4) Uani 1 2 d S T P . .
H1A H 0.885555 0.841299 1.217093 0.119 Uiso 0.5 1 calc R U P A -1
H1B H 0.883312 0.663264 1.223000 0.119 Uiso 0.5 1 calc R U P A -1
H1C H 0.928184 0.745437 1.104808 0.119 Uiso 0.5 1 calc R U P A -1
C2 C 0.6927(8) 0.8893(8) 1.0059(8) 0.0505(16) Uani 1 1 d . . . . .
H2A H 0.596886 0.894200 0.974209 0.061 Uiso 1 1 calc R U . . .
H2B H 0.719597 0.978356 1.060127 0.061 Uiso 1 1 calc R U . . .
C3 C 0.7563(8) 0.8921(10) 0.8952(7) 0.0621(19) Uani 1 1 d D . . . .
H3A H 0.852355 0.891747 0.926030 0.075 Uiso 1 1 calc R U . . .
H3B H 0.731874 0.984322 0.844555 0.075 Uiso 1 1 calc R U . . .
N3 N 0.5739(8) 0.7232(16) 0.5085(9) 0.032(4) Uani 0.5 1 d D . P B -1
H3C H 0.548179 0.653687 0.445807 0.038 Uiso 0.5 1 calc R U P B -1
H3D H 0.562949 0.815603 0.472838 0.038 Uiso 0.5 1 calc R U P B -1
H3E H 0.524960 0.714361 0.569912 0.038 Uiso 0.5 1 calc R U P B -1
C4 C 0.7685(11) 0.8110(13) 0.6753(9) 0.039(2) Uani 0.5 1 d D U P B -1
H4A H 0.735185 0.912309 0.650206 0.047 Uiso 0.5 1 calc R U P B -1
H4B H 0.865153 0.813093 0.693704 0.047 Uiso 0.5 1 calc R U P B -1
C5 C 0.7162(9) 0.6997(12) 0.5697(8) 0.039(3) Uani 0.5 1 d D U P B -1
H5A H 0.768431 0.706570 0.501628 0.047 Uiso 0.5 1 calc R U P B -1
H5B H 0.727456 0.598062 0.606700 0.047 Uiso 0.5 1 calc R U P B -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -4.0753 8.5060 '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
Br2 Pb1 Br1 89.04(2) . . ?
Br2 Pb1 Br1 89.04(2) 4_575 . ?
Br2 Pb1 Br2 79.57(3) . 4_575 ?
Br3 Pb1 Br1 178.88(3) . . ?
Br3 Pb1 Br2 90.10(2) . 4_575 ?
Br3 Pb1 Br2 90.10(2) . . ?
Br3 Pb1 Br4 87.838(15) . 2_546 ?
Br3 Pb1 Br4 87.838(14) . . ?
Br4 Pb1 Br1 92.914(13) 2_546 . ?
Br4 Pb1 Br1 92.914(13) . . ?
Br4 Pb1 Br2 92.318(15) 2_546 . ?
Br4 Pb1 Br2 92.318(15) . 4_575 ?
Br4 Pb1 Br2 171.625(16) 2_546 4_575 ?
Br4 Pb1 Br2 171.625(16) . . ?
Br4 Pb1 Br4 95.713(8) 2_546 . ?
Pb1 Br4 Pb1 180.0 . 3_576 ?
H1D O1 H1D 43.9 . 4_585 ?
H1D O1 H1E 109.5 . . ?
H1D O1 H1E 109.5 4_585 4_585 ?
H1D O1 H1E 94.2 . 4_585 ?
H1E O1 H1D 94.2 . 4_585 ?
H1E O1 H1E 40.7 . 4_585 ?
C1 N1 H1 107.1 . . ?
C2 N1 H1 107.1 . . ?
C2 N1 H1 107.1 4_575 . ?
C2 N1 C1 112.5(6) 4_575 . ?
C2 N1 C1 112.5(6) . . ?
C2 N1 C2 110.1(8) 4_575 . ?
C3 N2 H2 107.4 4_575 . ?
C3 N2 H2 107.4 . . ?
C3 N2 C3 105.7(7) 4_575 . ?
C3 N2 C4 97.0(5) . . ?
C3 N2 C4 129.9(7) . 4_575 ?
C3 N2 C4 129.9(7) 4_575 . ?
C3 N2 C4 97.0(5) 4_575 4_575 ?
C4 N2 H2 107.4 . . ?
C4 N2 H2 107.4 4_575 . ?
C4 N2 C4 38.0(8) 4_575 . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.1 . . ?
N1 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
C3 C2 N1 112.7(6) . . ?
C3 C2 H2A 109.1 . . ?
C3 C2 H2B 109.1 . . ?
N2 C3 H3A 109.6 . . ?
N2 C3 H3B 109.6 . . ?
C2 C3 N2 110.1(7) . . ?
C2 C3 H3A 109.6 . . ?
C2 C3 H3B 109.6 . . ?
H3A C3 H3B 108.2 . . ?
H3C N3 H3D 109.5 . . ?
H3C N3 H3E 109.5 . . ?
H3D N3 H3E 109.5 . . ?
C5 N3 H3C 109.5 . . ?
C5 N3 H3D 109.5 . . ?
C5 N3 H3E 109.5 . . ?
N2 C4 H4A 110.9 . . ?
N2 C4 H4B 110.9 . . ?
H4A C4 H4B 108.9 . . ?
C5 C4 N2 104.5(8) . . ?
C5 C4 H4A 110.9 . . ?
C5 C4 H4B 110.9 . . ?
N3 C5 C4 113.4(9) . . ?
N3 C5 H5A 108.9 . . ?
N3 C5 H5B 108.9 . . ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?
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 3.1050(10) . ?
Pb1 Br2 3.0511(7) 4_575 ?
Pb1 Br2 3.0511(7) . ?
Pb1 Br3 2.9538(10) . ?
Pb1 Br4 2.96601(19) 2_546 ?
Pb1 Br4 2.96601(19) . ?
O1 H1D 0.8496 . ?
O1 H1D 0.85(14) 4_585 ?
O1 H1E 0.8499 . ?
O1 H1E 0.85(13) 4_585 ?
N1 H1 0.9800 . ?
N1 C1 1.513(16) . ?
N1 C2 1.494(8) . ?
N1 C2 1.494(8) 4_575 ?
N2 H2 0.9800 . ?
N2 C3 1.568(10) 4_575 ?
N2 C3 1.568(10) . ?
N2 C4 1.647(13) . ?
N2 C4 1.647(13) 4_575 ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.429(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N3 H3C 0.8900 . ?
N3 H3D 0.8900 . ?
N3 H3E 0.8900 . ?
N3 C5 1.480(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.482(9) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
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 C2 C3 N2 59.4(9) . . . . ?
N2 C4 C5 N3 78.3(11) . . . . ?
C1 N1 C2 C3 70.8(10) . . . . ?
C2 N1 C2 C3 -55.6(11) 4_575 . . . ?
C3 N2 C3 C2 -59.1(9) 4_575 . . . ?
C3 N2 C4 C5 71.6(11) 4_575 . . . ?
C3 N2 C4 C5 -171.1(7) . . . . ?
C4 N2 C3 C2 166.0(7) . . . . ?
C4 N2 C3 C2 -172.7(7) 4_575 . . . ?
C4 N2 C4 C5 35.8(8) 4_575 . . . ?
