#------------------------------------------------------------------------------
#$Date: 2025-03-22 01:36:20 +0200 (Sat, 22 Mar 2025) $
#$Revision: 298556 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/01/7250164.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_7250164
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         'Cl2 Cs I, 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Cl2 Cs I N2'
_chemical_formula_weight         444.90
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-09-02 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            3
_cell_length_a                   9.77000(10)
_cell_length_b                   9.77000(10)
_cell_length_c                   11.9653(2)
_cell_measurement_reflns_used    23797
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.0280
_cell_measurement_theta_min      2.4000
_cell_volume                     989.11(2)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_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 0.959
_diffrn_measurement_device_type  'Rigaku (Mo) X-ray Source'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31157
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.901
_diffrn_reflns_theta_min         2.407
_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    5.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38637
_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    2.241
_exptl_crystal_description       Block
_exptl_crystal_F_000             618.0
_exptl_crystal_size_max          0.349
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.512
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 749 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.004(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         2095
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0186
_refine_ls_R_factor_gt           0.0173
_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)+(0.0132P)²+0.6584P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0357
_reflns_Friedel_coverage         0.681
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.891
_reflns_number_gt                1895
_reflns_number_total             2095
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00907j2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_cell_volume        989.11(3)
_cod_database_code               7250164
_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_res_file
;
TITL hj014a_lt_auto_a.res in P3(1)21
    shelx.res
    created by SHELXL-2018/3 at 16:27:07 on 14-Apr-2021
CELL  0.71073   9.7700   9.7700  11.9653   90.000   90.000  120.000
ZERR     6.00   0.0001   0.0001   0.0002    0.000    0.000    0.000
LATT  -1
SYMM  - Y,   X - Y, 1/3 + Z
SYMM  - X + Y, - X, 2/3 + Z
SYMM    Y,   X, - Z
SYMM    X - Y, - Y, 2/3 - Z
SYMM  - X, - X + Y, 1/3 - Z
SFAC  C    H    CS   I    N    BR   CL
UNIT  36 42 6 1 1 1 1
MERG   2
FMAP   2
PLAN    4
ACTA
EQIV $8 x, y, z+1
HTAB N1 Cl1_$8
EQIV $9 y, x, -z+1
HTAB C3 Cl1_$9
EQIV $10 -x+y+1, -x+2, z+2/3
HTAB C3 I1_$10
HTAB C1 I1
EQIV $5 -y+1, x-y+1, z+1/3
HTAB C1 I1_$5
EQIV $11 -x+y, -x+1, z+2/3
HTAB C2 Cl1_$11
CONF
BOND $H
L.S.  15
TEMP  -123.00
WGHT    0.013200    0.658400
FVAR       3.03525
CS1   3    0.632523    1.000000    0.333333    10.50000    0.02116    0.02332 =
         0.02385   -0.00009   -0.00005    0.01166
I1    4    0.770181    0.770181    0.500000    10.50000    0.02221    0.02221 =
         0.02653    0.00056   -0.00056    0.01219
N1    5    0.650371    0.918202    0.919437    11.00000    0.02025    0.02655 =
         0.02460    0.00336    0.00010    0.01045
AFIX  13
H1    2    0.617141    0.852342    0.988833    11.00000   -1.20000
AFIX   0
C3    1    0.816183    0.960477    0.890779    11.00000    0.02248    0.02446 =
         0.02670   -0.00048   -0.00049    0.01416
AFIX  23
H3A   2    0.825559    0.864177    0.889249    11.00000   -1.20000
H3B   2    0.890467    1.033628    0.947542    11.00000   -1.20000
AFIX   0
C1    1    0.577682    0.934689    0.726694    11.00000    0.02321    0.04087 =
         0.02629   -0.00911   -0.00617    0.01803
AFIX  23
H1B   2    0.583542    0.882350    0.657470    11.00000   -1.20000
H1A   2    0.492728    0.961011    0.717683    11.00000   -1.20000
AFIX   0
C2    1    0.542237    0.825136    0.826115    11.00000    0.02403    0.02632 =
         0.03913   -0.00480   -0.00467    0.00596
AFIX  23
H2A   2    0.430814    0.780928    0.849559    11.00000   -1.20000
H2B   2    0.558986    0.736439    0.805546    11.00000   -1.20000
AFIX   0
CL1   7    0.544306    0.722066    0.130596    11.00000    0.02302    0.01964 =
         0.02515   -0.00303    0.00265    0.00906
HKLF    4




REM  hj014a_lt_auto_a.res in P3(1)21
REM wR2 = 0.0357, GooF = S = 1.037, Restrained GooF = 1.037 for all data
REM R1 = 0.0173 for 1895 Fo > 4sig(Fo) and 0.0186 for all 1948 data
REM 56 parameters refined using 0 restraints

END

WGHT      0.0132      0.6585

REM Highest difference peak  0.512,  deepest hole -0.733,  1-sigma level  0.090
Q1    1   0.7173  1.0000  0.3333  10.50000  0.05    0.49
Q2    1   0.6291  1.0355  0.3965  11.00000  0.05    0.44
Q3    1   0.5000  0.7442  0.1304  11.00000  0.05    0.43
Q4    1   0.5839  0.9632  0.4580  11.00000  0.05    0.35
;
_shelx_res_checksum              63018
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z+1/3'
'-x+y, -x, z+2/3'
'y, x, -z'
'x-y, -y, -z+2/3'
'-x, -x+y, -z+1/3'
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
Cs1 Cs 0.63252(3) 1.000000 0.333333 0.02254(7) Uani 1 2 d S T P . .
I1 I 0.77018(3) 0.77018(3) 0.500000 0.02317(8) Uani 1 2 d S T P . .
N1 N 0.6504(3) 0.9182(3) 0.9194(2) 0.0244(6) Uani 1 1 d . . . . .
H1 H 0.617141 0.852342 0.988833 0.029 Uiso 1 1 calc R U . . .
C3 C 0.8162(4) 0.9605(4) 0.8908(3) 0.0235(7) Uani 1 1 d . . . . .
H3A H 0.825559 0.864177 0.889249 0.028 Uiso 1 1 calc R U . . .
H3B H 0.890467 1.033628 0.947542 0.028 Uiso 1 1 calc R U . . .
C1 C 0.5777(4) 0.9347(5) 0.7267(3) 0.0292(8) Uani 1 1 d . . . . .
H1B H 0.583542 0.882350 0.657470 0.035 Uiso 1 1 calc R U . . .
H1A H 0.492728 0.961011 0.717683 0.035 Uiso 1 1 calc R U . . .
C2 C 0.5422(5) 0.8251(4) 0.8261(3) 0.0328(8) Uani 1 1 d . . . . .
H2A H 0.430814 0.780928 0.849559 0.039 Uiso 1 1 calc R U . . .
H2B H 0.558986 0.736439 0.805546 0.039 Uiso 1 1 calc R U . . .
Cl1 Cl 0.54431(10) 0.72207(9) 0.13060(6) 0.02331(15) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cs1 0.02116(10) 0.02332(14) 0.02385(13) -0.00009(11) -0.00005(5) 0.01166(7)
I1 0.02221(11) 0.02221(11) 0.02653(15) 0.00056(6) -0.00056(6) 0.01219(12)
N1 0.0202(14) 0.0265(14) 0.0246(14) 0.0034(10) 0.0001(11) 0.0104(12)
C3 0.0225(16) 0.0245(17) 0.0267(17) -0.0005(13) -0.0005(13) 0.0142(14)
C1 0.0232(17) 0.041(2) 0.0263(17) -0.0091(15) -0.0062(13) 0.0180(15)
C2 0.0240(17) 0.0263(18) 0.039(2) -0.0048(15) -0.0047(16) 0.0060(15)
Cl1 0.0230(4) 0.0196(3) 0.0251(3) -0.0030(3) 0.0026(3) 0.0091(3)
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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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'
Cl Cl 0.1484 0.1585 '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
Cl1 Cs1 Cl1 79.75(3) 6_665 2_665 ?
Cl1 Cs1 Cl1 95.132(5) 6_665 . ?
Cl1 Cs1 Cl1 97.67(2) 2_665 . ?
Cl1 Cs1 Cl1 97.67(2) 6_665 5_675 ?
Cl1 Cs1 Cl1 95.133(5) 2_665 5_675 ?
Cl1 Cs1 Cl1 163.30(3) . 5_675 ?
Cl1 Cs1 I1 171.413(15) 6_665 . ?
Cl1 Cs1 I1 91.662(14) 2_665 . ?
Cl1 Cs1 I1 85.673(14) . . ?
Cl1 Cs1 I1 83.273(14) 5_675 . ?
Cl1 Cs1 I1 91.661(14) 6_665 3_674 ?
Cl1 Cs1 I1 171.411(15) 2_665 3_674 ?
Cl1 Cs1 I1 83.273(14) . 3_674 ?
Cl1 Cs1 I1 85.674(14) 5_675 3_674 ?
I1 Cs1 I1 96.923(10) . 3_674 ?
Cs1 I1 Cs1 166.102(10) 2_765 . ?
C2 N1 C1 110.4(3) . 5_676 ?
C2 N1 C3 109.6(3) . . ?
C1 N1 C3 109.8(3) 5_676 . ?
C2 N1 H1 109.0 . . ?
C1 N1 H1 109.0 5_676 . ?
C3 N1 H1 109.0 . . ?
N1 C3 C3 108.08(17) . 5_676 ?
N1 C3 H3A 110.1 . . ?
C3 C3 H3A 110.1 5_676 . ?
N1 C3 H3B 110.1 . . ?
C3 C3 H3B 110.1 5_676 . ?
H3A C3 H3B 108.4 . . ?
N1 C1 C2 108.3(3) 5_676 . ?
N1 C1 H1B 110.0 5_676 . ?
C2 C1 H1B 110.0 . . ?
N1 C1 H1A 110.0 5_676 . ?
C2 C1 H1A 110.0 . . ?
H1B C1 H1A 108.4 . . ?
N1 C2 C1 108.3(3) . . ?
N1 C2 H2A 110.0 . . ?
C1 C2 H2A 110.0 . . ?
N1 C2 H2B 110.0 . . ?
C1 C2 H2B 110.0 . . ?
H2A C2 H2B 108.4 . . ?
Cs1 Cl1 Cs1 159.91(3) 3_564 . ?
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
Cs1 Cl1 3.3827(8) 6_665 ?
Cs1 Cl1 3.3828(8) 2_665 ?
Cs1 Cl1 3.4148(7) . ?
Cs1 Cl1 3.4148(7) 5_675 ?
Cs1 I1 3.72116(19) . ?
Cs1 I1 3.72118(19) 3_674 ?
N1 C2 1.493(4) . ?
N1 C1 1.495(5) 5_676 ?
N1 C3 1.498(4) . ?
N1 H1 1.0000 . ?
C3 C3 1.529(7) 5_676 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C1 C2 1.520(5) . ?
C1 H1B 0.9900 . ?
C1 H1A 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 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 Cl1 1.00 2.02 3.024(3) 177.9 1_556 yes
C3 H3A Cl1 0.99 2.77 3.702(3) 156.6 4_556 yes
C3 H3B I1 0.99 3.11 4.040(3) 158.0 3_675 yes
C1 H1B I1 0.99 3.17 4.062(3) 150.1 . yes
C1 H1A I1 0.99 3.10 3.969(3) 146.7 2_665 yes
C2 H2A Cl1 0.99 2.96 3.602(4) 123.7 3_565 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
C2 N1 C3 C3 52.5(4) . . . 5_676 ?
C1 N1 C3 C3 -69.0(4) 5_676 . . 5_676 ?
C1 N1 C2 C1 51.5(4) 5_676 . . . ?
C3 N1 C2 C1 -69.5(4) . . . . ?
N1 C1 C2 N1 14.3(4) 5_676 . . . ?
