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#$Date: 2025-03-22 01:36:20 +0200 (Sat, 22 Mar 2025) $
#$Revision: 298556 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/01/7250162.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_7250162
loop_
_publ_author_name
'van der Poll, Hendrik Johannes'
'Erasmus, Rudolph'
'Rademeyer, Melanie'
_publ_section_title
;
 Structures and Band Gaps of Lead-Free Dabconium-Containing Hybrid
 Alkali-Metal Halide Perovskites
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00907J
_journal_year                    2025
_chemical_formula_moiety         'Br3 Na, 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Br3 N2 Na'
_chemical_formula_weight         376.91
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-12-10 deposited with the CCDC.	2025-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   16.3508(2)
_cell_length_b                   16.3508(2)
_cell_length_c                   21.9979(2)
_cell_measurement_reflns_used    10201
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      78.7250
_cell_measurement_theta_min      3.6820
_cell_volume                     5093.19(10)
_computing_cell_refinement       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.23a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Mercury (Macrae  et al., 2008)'
_computing_publication_material  'Mercury (Macrae  et al., 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXTS (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku (Cu) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0096
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10907
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.053
_diffrn_reflns_theta_min         5.092
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.230
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.23a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    2.212
_exptl_crystal_description       Block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.185
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.355
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.000056(2)
_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   1.146
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0160
_refine_ls_R_factor_gt           0.0159
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0123P)²+22.9659P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0375
_refine_ls_wR_factor_ref         0.0375
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1203
_reflns_number_total             1207
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00907j2.cif
_cod_data_source_block           DNaBr3
_cod_original_cell_volume        5093.19(13)
_cod_database_code               7250162
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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 0.64266(2) 0.46819(2) 0.41216(2) 0.01443(8) Uani 1 1 d . . . . .
Br2 Br 0.51739(2) 0.333333 0.583333 0.01713(9) Uani 1 2 d S T P . .
Na2 Na 0.666667 0.333333 0.333333 0.0156(4) Uani 1 6 d S T P . .
Na1 Na 0.666667 0.333333 0.50166(6) 0.0190(3) Uani 1 3 d S T P . .
N1 N 0.42062(12) 0.38309(12) 0.41566(8) 0.0156(3) Uani 1 1 d . . . . .
H1 H 0.491231 0.418377 0.414972 0.019 Uiso 1 1 calc R U . . .
C1 C 0.38594(14) 0.40805(14) 0.35974(9) 0.0167(4) Uani 1 1 d . . . . .
H1A H 0.406725 0.388346 0.323051 0.020 Uiso 1 1 calc R U . . .
H1B H 0.411831 0.477176 0.357797 0.020 Uiso 1 1 calc R U . . .
C2 C 0.38857(14) 0.41219(14) 0.47092(9) 0.0168(4) Uani 1 1 d . . . . .
H2B H 0.410339 0.480562 0.469074 0.020 Uiso 1 1 calc R U . . .
H2A H 0.415569 0.400098 0.507815 0.020 Uiso 1 1 calc R U . . .
C3 C 0.38741(15) 0.28027(15) 0.41723(11) 0.0227(5) Uani 1 1 d . . . . .
H3B H 0.410405 0.264512 0.454594 0.027 Uiso 1 1 calc R U . . .
H3A H 0.412233 0.262485 0.381645 0.027 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 0.0181 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'
Na Na 0.1353 0.1239 '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'
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
Na2 Br1 Na1 74.635(19) . . ?
Na1 Br2 Na1 72.71(4) . 16_545 ?
Br1 Na2 Br1 180.0 3_665 33_545 ?
Br1 Na2 Br1 89.573(5) 3_665 2_655 ?
Br1 Na2 Br1 90.427(5) 33_545 2_655 ?
Br1 Na2 Br1 89.573(5) 3_665 . ?
Br1 Na2 Br1 90.427(5) 33_545 . ?
Br1 Na2 Br1 89.573(5) 2_655 . ?
Br1 Na2 Br1 90.427(6) 3_665 32 ?
Br1 Na2 Br1 89.573(5) 33_545 32 ?
Br1 Na2 Br1 180.0 2_655 32 ?
Br1 Na2 Br1 90.428(6) . 32 ?
Br1 Na2 Br1 90.427(5) 3_665 31_655 ?
Br1 Na2 Br1 89.573(5) 33_545 31_655 ?
Br1 Na2 Br1 90.427(6) 2_655 31_655 ?
Br1 Na2 Br1 180.0 . 31_655 ?
Br1 Na2 Br1 89.571(6) 32 31_655 ?
Br1 Na2 Na1 54.434(4) 3_665 . ?
Br1 Na2 Na1 125.566(4) 33_545 . ?
Br1 Na2 Na1 54.434(4) 2_655 . ?
Br1 Na2 Na1 54.434(4) . . ?
Br1 Na2 Na1 125.567(4) 32 . ?
Br1 Na2 Na1 125.566(4) 31_655 . ?
Br1 Na2 Na1 125.564(4) 3_665 31_655 ?
Br1 Na2 Na1 54.436(4) 33_545 31_655 ?
Br1 Na2 Na1 125.565(4) 2_655 31_655 ?
Br1 Na2 Na1 125.568(4) . 31_655 ?
Br1 Na2 Na1 54.434(4) 32 31_655 ?
Br1 Na2 Na1 54.432(4) 31_655 31_655 ?
Na1 Na2 Na1 180.0 . 31_655 ?
Br2 Na1 Br2 88.45(3) . 2_655 ?
Br2 Na1 Br2 88.45(3) . 3_665 ?
Br2 Na1 Br2 88.45(3) 2_655 3_665 ?
Br2 Na1 Br1 173.074(16) . 3_665 ?
Br2 Na1 Br1 98.048(5) 2_655 3_665 ?
Br2 Na1 Br1 89.322(5) 3_665 3_665 ?
Br2 Na1 Br1 98.047(5) . 2_655 ?
Br2 Na1 Br1 89.322(5) 2_655 2_655 ?
Br2 Na1 Br1 173.074(16) 3_665 2_655 ?
Br1 Na1 Br1 84.50(3) 3_665 2_655 ?
Br2 Na1 Br1 89.321(5) . . ?
Br2 Na1 Br1 173.074(16) 2_655 . ?
Br2 Na1 Br1 98.048(5) 3_665 . ?
Br1 Na1 Br1 84.50(3) 3_665 . ?
Br1 Na1 Br1 84.50(3) 2_655 . ?
Br2 Na1 Na1 53.65(2) . 16_545 ?
Br2 Na1 Na1 53.64(2) 2_655 16_545 ?
Br2 Na1 Na1 53.64(2) 3_665 16_545 ?
Br1 Na1 Na1 129.068(19) 3_665 16_545 ?
Br1 Na1 Na1 129.069(19) 2_655 16_545 ?
Br1 Na1 Na1 129.072(19) . 16_545 ?
Br2 Na1 Na2 126.36(2) . . ?
Br2 Na1 Na2 126.36(2) 2_655 . ?
Br2 Na1 Na2 126.36(2) 3_665 . ?
Br1 Na1 Na2 50.930(19) 3_665 . ?
Br1 Na1 Na2 50.931(19) 2_655 . ?
Br1 Na1 Na2 50.931(19) . . ?
Na1 Na1 Na2 180.0 16_545 . ?
C3 N1 C2 110.71(16) . . ?
C3 N1 C1 110.75(16) . . ?
C2 N1 C1 109.98(15) . . ?
C3 N1 H1 108.4 . . ?
C2 N1 H1 108.4 . . ?
C1 N1 H1 108.4 . . ?
N1 C1 C2 108.09(15) . 12 ?
N1 C1 H1A 110.1 . . ?
C2 C1 H1A 110.1 12 . ?
N1 C1 H1B 110.1 . . ?
C2 C1 H1B 110.1 12 . ?
H1A C1 H1B 108.4 . . ?
N1 C2 C1 108.67(16) . 12 ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 12 . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 12 . ?
H2B C2 H2A 108.3 . . ?
N1 C3 C3 108.41(10) . 12 ?
N1 C3 H3B 110.0 . . ?
C3 C3 H3B 110.0 12 . ?
N1 C3 H3A 110.0 . . ?
C3 C3 H3A 110.0 12 . ?
H3B C3 H3A 108.4 . . ?
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
Br1 Na2 2.9814(2) . ?
Br1 Na1 3.1237(9) . ?
Br2 Na1 3.0308(8) . ?
Br2 Na1 3.0308(8) 16_545 ?
Na2 Na1 3.7028(13) . ?
Na2 Na1 3.7030(13) 31_655 ?
Na1 Na1 3.593(3) 16_545 ?
N1 C3 1.486(3) . ?
N1 C2 1.493(3) . ?
N1 C1 1.494(2) . ?
N1 H1 1.0000 . ?
C1 C2 1.529(3) 12 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2B 0.9900 . ?
C2 H2A 0.9900 . ?
C3 C3 1.532(4) 12 ?
C3 H3B 0.9900 . ?
C3 H3A 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 H1 Br1 1.00 2.19 3.1734(16) 168.8 . yes
C1 H1A Br1 0.99 2.97 3.892(2) 155.8 33_545 yes
C1 H1B Br2 0.99 3.01 3.907(2) 152.0 19_666 yes
C2 H2B Br2 0.99 2.90 3.834(2) 158.4 19_666 yes
C2 H2A Br2 0.99 2.92 3.864(2) 159.2 . yes
C3 H3A Br1 0.99 3.03 3.559(2) 114.9 2_655 yes
C3 H3A Br1 0.99 3.11 3.997(2) 150.3 33_545 yes
N1 H1 Br1 1.00 2.19 3.1734(16) 168.8 . yes
C1 H1A Br1 0.99 2.97 3.892(2) 155.8 33_545 yes
C1 H1B Br2 0.99 3.01 3.907(2) 152.0 19_666 yes
C2 H2B Br2 0.99 2.90 3.834(2) 158.4 19_666 yes
C2 H2A Br2 0.99 2.92 3.864(2) 159.2 . yes
C3 H3A Br1 0.99 3.03 3.559(2) 114.9 2_655 yes
C3 H3A Br1 0.99 3.11 3.997(2) 150.3 33_545 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 N1 C1 C2 63.4(2) . . . 12 ?
C2 N1 C1 C2 -59.30(19) . . . 12 ?
C3 N1 C2 C1 -58.8(2) . . . 12 ?
C1 N1 C2 C1 63.89(18) . . . 12 ?
C2 N1 C3 C3 63.0(3) . . . 12 ?
C1 N1 C3 C3 -59.2(3) . . . 12 ?
