#------------------------------------------------------------------------------
#$Date: 2026-04-22 03:09:01 +0200 (Wed, 22 Apr 2026) $
#$Revision: 305594 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/7/25/19/7251904.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_7251904
loop_
_publ_author_name
'Ben Mahmoud, Iteb'
'Alghamdi, Mashael A.'
'Lazreg Aref, Houda'
'Mhadhbi, Noureddine'
'Nasrallah, Hossam H.'
'Guesmi, Ahlem'
'Ben Hamadi, Naoufel'
'Walha, Sandra'
'Costantino, Ferdinando'
'Naïli, Houcine'
_publ_section_title
;
 Diethylenetriamine-driven assembly of a dimeric cadmium bromide hybrid
 and an organic bromide salt: structural, vibrational, optical, in silico
 study and biological insights
;
_journal_issue                   23
_journal_name_full               'RSC Advances'
_journal_page_first              20526
_journal_page_last               20543
_journal_paper_doi               10.1039/D6RA02827F
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         'C4 H16 N3, 3(Br)'
_chemical_formula_sum            'C4 H16 Br3 N3'
_chemical_formula_weight         345.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2026-04-12
_audit_creation_method
;
Olex2 1.5
(compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314)
;
_audit_update_record
;
2026-04-12 deposited with the CCDC.	2026-04-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.211(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.2138(5)
_cell_length_b                   19.5497(16)
_cell_length_c                   8.9715(9)
_cell_measurement_reflns_used    6710
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      26.369
_cell_measurement_theta_min      3.085
_cell_volume                     1088.13(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_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      150.15
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -21.00  39.00   1.00    7.03    --   11.34  77.00 -30.00   60
  2  ω    -17.00  84.00   1.00    7.03    --   11.34  57.00 -30.00  101
  3  ω    -62.00  39.00   1.00    7.03    --   11.34 -57.00-180.00  101
  4  ω    -98.00 -35.00   1.00    7.03    --  -10.40 178.00-120.00   63
  5  ω    -43.00  31.00   1.00    7.03    --  -10.40  77.00  60.00   74
  6  ω    -13.00  86.00   1.00    7.03    --   11.34  37.00-180.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0692
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14524
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         3.085
_exptl_absorpt_coefficient_mu    11.070
_exptl_absorpt_correction_T_max  0.08500
_exptl_absorpt_correction_T_min  0.00900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_description       block
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.469
_exptl_crystal_size_mid          0.382
_exptl_crystal_size_min          0.223
_refine_diff_density_max         0.84
_refine_diff_density_min         -1.04
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.0138(12)
_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   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         2221
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0674P)²+7.2133P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1977
_reflns_number_total             2221
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6ra02827f2.cif
_cod_data_source_block           DETBR_publish
_cod_database_code               7251904
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups, All N(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C1(H1D,H1E), C2(H2C,H2D), C3(H3D,H3E), C4(H4A,H4B)
3.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C), N3(H3A,H3B,H3C)
;
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a nylon loop in perfluoroether oil'
_olex2_submission_original_sample_id DETZnBr
_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
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Br1 Br -0.18236(7) 0.34366(2) 0.03655(5) 0.02044(16) Uani 1 1 d . . . . .
Br2 Br 0.34182(7) 0.23927(2) 0.24856(5) 0.01848(16) Uani 1 1 d . . . . .
Br3 Br 0.83582(7) 0.53055(2) 0.29965(5) 0.01948(16) Uani 1 1 d . . . . .
N1 N 0.3116(5) 0.38664(18) 0.0113(4) 0.0169(8) Uani 1 1 d . . . . .
H1A H 0.445875 0.367883 0.016816 0.020 Uiso 1 1 calc R U . . .
H1B H 0.281969 0.403429 -0.082219 0.020 Uiso 1 1 calc R U . . .
H1C H 0.212883 0.354065 0.031646 0.020 Uiso 1 1 calc R U . . .
N2 N 0.5458(5) 0.39255(17) 0.3218(4) 0.0137(7) Uani 1 1 d . . . . .
H2A H 0.568395 0.354547 0.266218 0.016 Uiso 1 1 calc R U . . .
H2B H 0.644201 0.424542 0.297357 0.016 Uiso 1 1 calc R U . . .
N3 N 0.8422(6) 0.32187(19) 0.6646(4) 0.0187(8) Uani 1 1 d . . . . .
H3A H 0.964028 0.296072 0.674609 0.022 Uiso 1 1 calc R U . . .
H3B H 0.727758 0.296820 0.692611 0.022 Uiso 1 1 calc R U . . .
H3C H 0.857395 0.359614 0.723633 0.022 Uiso 1 1 calc R U . . .
C1 C 0.3022(7) 0.4430(2) 0.1215(5) 0.0180(9) Uani 1 1 d . . . . .
H1D H 0.163104 0.467255 0.104834 0.022 Uiso 1 1 calc R U . . .
H1E H 0.418817 0.476012 0.104055 0.022 Uiso 1 1 calc R U . . .
C2 C 0.3240(6) 0.4195(2) 0.2811(5) 0.0172(9) Uani 1 1 d . . . . .
H2C H 0.292866 0.458211 0.347577 0.021 Uiso 1 1 calc R U . . .
H2D H 0.216808 0.383086 0.296825 0.021 Uiso 1 1 calc R U . . .
C3 C 0.5836(7) 0.3749(2) 0.4825(5) 0.0190(9) Uani 1 1 d . U . . .
H3D H 0.472326 0.342269 0.512676 0.023 Uiso 1 1 calc R U . . .
H3E H 0.574045 0.416669 0.544193 0.023 Uiso 1 1 calc R U . . .
C4 C 0.8052(7) 0.3432(2) 0.5069(5) 0.0217(10) Uani 1 1 d . . . . .
H4A H 0.817013 0.302934 0.440821 0.026 Uiso 1 1 calc R U . . .
H4B H 0.916556 0.376743 0.481201 0.026 Uiso 1 1 calc R 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'
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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 0 -12 0.1115
2 0 12 0.1115
2 -27 0 0.2098
-2 27 0 0.2098
-3 -26 2 0.1571
-7 17 3 0.1833
7 15 0 0.1498
8 6 -6 0.1017
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
C1 N1 H1A 109.5 . . ?
C1 N1 H1B 109.5 . . ?
H1A N1 H1B 109.5 . . ?
C1 N1 H1C 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C3 N2 C2 114.2(3) . . ?
C3 N2 H2A 108.7 . . ?
C2 N2 H2A 108.7 . . ?
C3 N2 H2B 108.7 . . ?
C2 N2 H2B 108.7 . . ?
H2A N2 H2B 107.6 . . ?
C4 N3 H3A 109.5 . . ?
C4 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
C4 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
N1 C1 C2 113.8(3) . . ?
N1 C1 H1D 108.8 . . ?
C2 C1 H1D 108.8 . . ?
N1 C1 H1E 108.8 . . ?
C2 C1 H1E 108.8 . . ?
H1D C1 H1E 107.7 . . ?
N2 C2 C1 111.8(3) . . ?
N2 C2 H2C 109.3 . . ?
C1 C2 H2C 109.3 . . ?
N2 C2 H2D 109.3 . . ?
C1 C2 H2D 109.3 . . ?
H2C C2 H2D 107.9 . . ?
N2 C3 C4 109.1(3) . . ?
N2 C3 H3D 109.9 . . ?
C4 C3 H3D 109.9 . . ?
N2 C3 H3E 109.9 . . ?
C4 C3 H3E 109.9 . . ?
H3D C3 H3E 108.3 . . ?
N3 C4 C3 110.1(4) . . ?
N3 C4 H4A 109.6 . . ?
C3 C4 H4A 109.6 . . ?
N3 C4 H4B 109.6 . . ?
C3 C4 H4B 109.6 . . ?
H4A C4 H4B 108.1 . . ?
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
N1 C1 1.483(6) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 H1C 0.9100 . ?
N2 C3 1.488(5) . ?
N2 C2 1.501(5) . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 C4 1.481(6) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
C1 C2 1.503(6) . ?
C1 H1D 0.9900 . ?
C1 H1E 0.9900 . ?
C2 H2C 0.9900 . ?
C2 H2D 0.9900 . ?
C3 C4 1.515(6) . ?
C3 H3D 0.9900 . ?
C3 H3E 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1C Br1 0.91 2.47 3.203(3) 138.1 . yes
N1 H1A Br1 0.91 2.36 3.250(3) 167.8 1_655 yes
N1 H1B Br3 0.91 2.42 3.310(4) 166.6 3_665 yes
N2 H2A Br1 0.91 2.65 3.286(4) 127.3 1_655 yes
N2 H2A Br2 0.91 2.66 3.305(3) 128.9 . yes
N2 H2B Br3 0.91 2.39 3.257(3) 159.3 . yes
N3 H3B Br2 0.91 2.58 3.453(4) 162.0 4_566 yes
N3 H3A Br2 0.91 2.50 3.372(4) 160.5 4_666 yes
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
C3 N2 C2 C1 174.3(4) . . . . ?
N1 C1 C2 N2 68.0(5) . . . . ?
C2 N2 C3 C4 175.5(4) . . . . ?
N2 C3 C4 N3 -177.1(3) . . . . ?
