#------------------------------------------------------------------------------
#$Date: 2025-03-22 01:36:20 +0200 (Sat, 22 Mar 2025) $
#$Revision: 298556 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/01/7250161.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_7250161
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         '3(Cs0.33 I), 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 Cs I3 N2'
_chemical_formula_weight         627.80
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_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            2
_cell_length_a                   10.0382(2)
_cell_length_b                   10.0382(2)
_cell_length_c                   7.9849(2)
_cell_measurement_reflns_used    5252
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.8860
_cell_measurement_theta_min      2.3380
_cell_volume                     696.81(3)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.930
_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  0.0554
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7018
_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         30.883
_diffrn_reflns_theta_min         2.343
_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    9.267
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17877
_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    2.992
_exptl_crystal_description       Block
_exptl_crystal_F_000             556
_exptl_crystal_size_max          0.434
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.184
_refine_ls_extinction_coef       0.0102(7)
_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   1.293
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.293
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0197P)²+1.5328P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0522
_refine_ls_wR_factor_ref         0.0524
_reflns_Friedel_coverage         0.000
_reflns_number_gt                411
_reflns_number_total             424
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00907j2.cif
_cod_data_source_block           DCsI3
_cod_database_code               7250161
_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 hj011_lt_auto_a.res in P6(3)/mmc
    shelx.res
    created by SHELXL-2018/3 at 08:21:14 on 05-Dec-2024
CELL  0.71073  10.0382  10.0382   7.9849   90.000   90.000  120.000
ZERR     2.00   0.0002   0.0002   0.0002    0.000    0.000    0.000
LATT   1
SYMM  - Y,   X - Y,   Z
SYMM  - X + Y, - X,   Z
SYMM  - X, - Y, 1/2 + Z
SYMM    Y, - X + Y, 1/2 + Z
SYMM    X - Y,   X, 1/2 + Z
SYMM    Y,   X, - Z
SYMM    X - Y, - Y, - Z
SYMM  - X, - X + Y, - Z
SYMM  - Y, - X, 1/2 - Z
SYMM  - X + Y,   Y, 1/2 - Z
SYMM    X,   X - Y, 1/2 - Z
SFAC  C    H    I    N    CS
UNIT  12 28 6 4 2
MERG   2
HTAB N1 I1
EQIV $8 -y+1, x-y+1, z
HTAB N1 I1_$8
EQIV $9 -x+y, -x+1, z
HTAB N1 I1_$9
EQIV $12 y, -x+y, -z+1
HTAB C1 I1_$12
HTAB C1 I1_$9
HTAB C1 I1_$8
EQIV $13 x-y+1, x, -z+1
HTAB C1 I1_$13
FMAP   2
PLAN    4
ACTA
BOND   $H
CONF
LIST   4
L.S.  15
TEMP  -123.00
WGHT    0.019700    1.532800
EXTI    0.010181
FVAR       0.38828
CS1   5    0.000000    1.000000    0.500000    10.08333    0.01627    0.01627 =
         0.01252    0.00000    0.00000    0.00813
I1    3    0.184662    0.815338    0.250000    10.25000    0.01609    0.01609 =
         0.01403    0.00000    0.00000    0.00884
N1    4    0.333333    0.666667    0.594192    10.16667    0.01440    0.01440 =
         0.00738    0.00000    0.00000    0.00720
AFIX  13
H1    2    0.333333    0.666667    0.468956    10.16667   -1.20000
AFIX   0
C1    1    0.414438    0.585562    0.653458    10.50000    0.03382    0.03382 =
         0.01417    0.00003   -0.00003    0.02834
AFIX  23
H1A   2    0.521461    0.638476    0.611090    10.50000   -1.20000
H1B   2    0.361524    0.478539    0.611090    10.50000   -1.20000
AFIX   0
HKLF    4




REM  hj011_lt_auto_a.res in P6(3)/mmc
REM wR2 = 0.0524, GooF = S = 1.293, Restrained GooF = 1.293 for all data
REM R1 = 0.0233 for 411 Fo > 4sig(Fo) and 0.0244 for all 424 data
REM 17 parameters refined using 0 restraints

END

WGHT      0.0197      1.5328

REM Highest difference peak  0.745,  deepest hole -0.780,  1-sigma level  0.184
Q1    1   0.1987  0.8013  0.1166  10.50000  0.05    0.74
Q2    1   0.0000  1.0000  0.6301  10.16667  0.05    0.72
Q3    1   0.3564  0.7127  0.6496  10.50000  0.05    0.63
Q4    1   0.3831  0.7662  0.3960  10.50000  0.05    0.57
;
_shelx_res_checksum              92959
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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
Cs1 Cs 0.000000 1.000000 0.500000 0.01502(19) Uani 1 12 d S T P . .
I1 I 0.18466(2) 0.81534(2) 0.250000 0.01505(17) Uani 1 4 d S T P . .
N1 N 0.333333 0.666667 0.5942(7) 0.0121(11) Uani 1 6 d S T P . .
H1 H 0.333333 0.666667 0.468956 0.014 Uiso 1 6 calc R U P . .
C1 C 0.4144(2) 0.5856(2) 0.6535(5) 0.0222(9) Uani 1 2 d S T P . .
H1A H 0.521461 0.638476 0.611090 0.027 Uiso 0.5 1 calc R U P . .
H1B H 0.361524 0.478539 0.611090 0.027 Uiso 0.5 1 calc R U P . .
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 0.0163(2) 0.0163(2) 0.0125(3) 0.000 0.000 0.00813(12)
I1 0.0161(2) 0.0161(2) 0.0140(2) 0.000 0.000 0.00884(16)
N1 0.0144(17) 0.0144(17) 0.007(3) 0.000 0.000 0.0072(8)
C1 0.034(2) 0.034(2) 0.014(2) 0.0000(7) 0.0000(7) 0.028(2)
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'
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'
Cs Cs -0.3680 2.1192 '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
I1 Cs1 I1 180.0 15_666 3_465 ?
I1 Cs1 I1 94.692(4) 15_666 14_456 ?
I1 Cs1 I1 85.308(4) 3_465 14_456 ?
I1 Cs1 I1 85.308(4) 15_666 2_675 ?
I1 Cs1 I1 94.692(4) 3_465 2_675 ?
I1 Cs1 I1 180.0 14_456 2_675 ?
I1 Cs1 I1 85.308(4) 15_666 . ?
I1 Cs1 I1 94.692(4) 3_465 . ?
I1 Cs1 I1 85.308(4) 14_456 . ?
I1 Cs1 I1 94.692(4) 2_675 . ?
I1 Cs1 I1 94.692(4) 15_666 13_576 ?
I1 Cs1 I1 85.308(4) 3_465 13_576 ?
I1 Cs1 I1 94.692(4) 14_456 13_576 ?
I1 Cs1 I1 85.308(4) 2_675 13_576 ?
I1 Cs1 I1 180.0 . 13_576 ?
I1 Cs1 Cs1 58.129(3) 15_666 4_575 ?
I1 Cs1 Cs1 121.871(3) 3_465 4_575 ?
I1 Cs1 Cs1 58.129(3) 14_456 4_575 ?
I1 Cs1 Cs1 121.871(3) 2_675 4_575 ?
I1 Cs1 Cs1 121.871(3) . 4_575 ?
I1 Cs1 Cs1 58.129(3) 13_576 4_575 ?
I1 Cs1 Cs1 121.871(3) 15_666 4_574 ?
I1 Cs1 Cs1 58.129(3) 3_465 4_574 ?
I1 Cs1 Cs1 121.871(3) 14_456 4_574 ?
I1 Cs1 Cs1 58.129(3) 2_675 4_574 ?
I1 Cs1 Cs1 58.129(3) . 4_574 ?
I1 Cs1 Cs1 121.871(3) 13_576 4_574 ?
Cs1 Cs1 Cs1 180.0 4_575 4_574 ?
Cs1 I1 Cs1 63.742(6) 4_574 . ?
C1 N1 C1 110.4(3) 2_665 3_565 ?
C1 N1 C1 110.4(3) 2_665 . ?
C1 N1 C1 110.4(3) 3_565 . ?
C1 N1 H1 108.6 2_665 . ?
C1 N1 H1 108.6 3_565 . ?
C1 N1 H1 108.6 . . ?
N1 C1 C1 108.6(3) . 16_557 ?
N1 C1 H1A 110.0 . . ?
C1 C1 H1A 110.0 16_557 . ?
N1 C1 H1B 110.0 . . ?
C1 C1 H1B 110.0 16_557 . ?
H1A C1 H1B 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
Cs1 I1 3.7806(3) 15_666 ?
Cs1 I1 3.7806(3) 3_465 ?
Cs1 I1 3.7806(3) 14_456 ?
Cs1 I1 3.7806(3) 2_675 ?
Cs1 I1 3.7806(3) . ?
Cs1 I1 3.7806(3) 13_576 ?
Cs1 Cs1 3.99245(10) 4_575 ?
Cs1 Cs1 3.99245(10) 4_574 ?
N1 C1 1.487(4) 2_665 ?
N1 C1 1.487(4) 3_565 ?
N1 C1 1.487(4) . ?
N1 H1 1.0000 . ?
C1 C1 1.542(9) 16_557 ?
C1 H1A 0.9900 . ?
C1 H1B 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 I1 1.00 3.12 3.773(4) 124.1 . yes
N1 H1 I1 1.00 3.12 3.773(4) 124.1 2_665 yes
N1 H1 I1 1.00 3.12 3.773(4) 124.1 3_565 yes
C1 H1A I1 0.99 3.19 3.895(3) 129.6 14_556 yes
C1 H1A I1 0.99 3.27 3.925(4) 124.8 3_565 yes
C1 H1B I1 0.99 3.27 3.925(4) 124.8 2_665 yes
C1 H1B I1 0.99 3.19 3.895(3) 129.6 15_656 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
C1 N1 C1 C1 61.1(3) 2_665 . . 16_557 ?
C1 N1 C1 C1 -61.1(3) 3_565 . . 16_557 ?
