#------------------------------------------------------------------------------
#$Date: 2025-03-22 01:36:20 +0200 (Sat, 22 Mar 2025) $
#$Revision: 298556 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/25/01/7250167.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_7250167
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(I K0.33), 2(C3 H7 N)'
_chemical_formula_sum            'C6 H14 I3 K N2'
_chemical_formula_weight         533.99
_space_group_crystal_system      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2025-03-19 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                   9.6698(7)
_cell_length_b                   9.6698(7)
_cell_length_c                   12.2899(9)
_cell_measurement_reflns_used    3301
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      30.4760
_cell_measurement_theta_min      2.9080
_cell_volume                     995.21(13)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0871
_diffrn_reflns_av_unetI/netI     0.0395
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.902
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.905
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.897
_diffrn_reflns_theta_min         2.943
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.342
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.673
_exptl_crystal_description       plate
_exptl_crystal_F_000             726
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.049
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.954
_refine_diff_density_min         -2.508
_refine_diff_density_rms         0.360
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         608
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0254P)²+89.3544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1542
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                594
_reflns_number_total             608
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00907j2.cif
_cod_data_source_block           DKI3
_cod_original_cell_volume        995.21(16)
_cod_database_code               7250167
_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 hj098f_lt_auto_a.res in R32
    shelx.res
    created by SHELXL-2018/3 at 10:00:14 on 05-Mar-2025
CELL  0.71073   9.6698   9.6698  12.2899   90.000   90.000  120.000
ZERR     3.00   0.0007   0.0007   0.0009    0.000    0.000    0.000
LATT  -3
SYMM  - Y,   X - Y,   Z
SYMM  - X + Y, - X,   Z
SYMM    Y,   X, - Z
SYMM    X - Y, - Y, - Z
SYMM  - X, - X + Y, - Z
SFAC  C    H    I    K    N
UNIT  18 42 9 3 6
MERG   2
TWIN    0.68  0.37 -0.63  0.32 -0.37  0.63 -0.68 -1.37 -0.37  -4
EADP C1 N1
EQIV $10 x-2/3, y-1/3, z-1/3
HTAB C1 I1_$10
HTAB C1 I1
HTAB C1 I1_$10
HTAB C1 I1
FMAP   2
PLAN   10
ACTA
L.S.   4
TEMP  -120.00
WGHT    0.025400   89.354401
BASF   0.09379   0.26557  -0.07636
FVAR       0.21788
I1    3    0.528408    0.528408    0.500000    10.50000    0.02735    0.02735 =
         0.04595   -0.01630    0.01630    0.00338
K1    4    0.666667    0.333333    0.333333    10.16667    0.01806    0.01806 =
         0.02281    0.00000    0.00000    0.00903
N1    5    0.333333    0.666667    0.268019    10.33333    0.02798    0.02798 =
         0.03755    0.00000    0.00000    0.01399
AFIX  13
H1    2    0.333334    0.666667    0.349387    10.33333   -1.20000
AFIX   0
C1    1    0.319793    0.515966    0.228792    11.00000    0.02798    0.02798 =
         0.03755    0.00000    0.00000    0.01399
AFIX  23
H1A   2    0.212575    0.425103    0.245889    11.00000   -1.20000
H1B   2    0.400656    0.497495    0.264920    11.00000   -1.20000
AFIX   0
HKLF    4




REM  hj098f_lt_auto_a.res in R32
REM wR2 = 0.1553, GooF = S = 1.296, Restrained GooF = 1.296 for all data
REM R1 = 0.0667 for 594 Fo > 4sig(Fo) and 0.0693 for all 608 data
REM 17 parameters refined using 0 restraints

END

WGHT      0.0255     89.3230

REM Highest difference peak  1.954,  deepest hole -2.508,  1-sigma level  0.360
Q1    1   0.4339  0.4779  0.4475  11.00000  0.05    1.95
Q2    1   0.5699  0.4755  0.4966  11.00000  0.05    1.72
Q3    1   0.3333  0.5759  0.1667  10.50000  0.05    1.69
Q4    1   0.4771  0.5807  0.4128  11.00000  0.05    1.68
Q5    1   0.6027  0.5699  0.4098  11.00000  0.05    1.38
Q6    1   0.4638  0.4127  0.4009  11.00000  0.05    0.99
Q7    1   0.1133  0.3333  0.3333  10.50000  0.05    0.97
Q8    1   0.2349  0.5082  0.2599  11.00000  0.05    0.90
Q9    1   0.5437  0.3750  0.3920  11.00000  0.05    0.88
Q10   1   0.2375  0.3333  0.3333  10.50000  0.05    0.85
;
_shelx_res_checksum              81562
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'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+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'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+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
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
I1 I 0.52841(18) 0.52841(18) 0.500000 0.0381(7) Uani 1 2 d S T P . .
K1 K 0.666667 0.333333 0.333333 0.0196(18) Uani 1 6 d S T P . .
N1 N 0.333333 0.666667 0.268(2) 0.031(4) Uani 1 3 d S T P . .
H1 H 0.333334 0.666667 0.349387 0.037 Uiso 1 3 calc R U P . .
C1 C 0.320(3) 0.516(3) 0.2288(16) 0.031(4) Uani 1 1 d . . . . .
H1A H 0.212575 0.425103 0.245889 0.037 Uiso 1 1 calc R U . . .
H1B H 0.400656 0.497495 0.264920 0.037 Uiso 1 1 calc R U . . .
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
I1 0.0274(7) 0.0274(7) 0.0459(11) -0.0163(5) 0.0163(5) 0.0034(8)
K1 0.018(3) 0.018(3) 0.023(4) 0.000 0.000 0.0090(14)
N1 0.028(5) 0.028(5) 0.038(9) 0.000 0.000 0.014(3)
C1 0.028(5) 0.028(5) 0.038(9) 0.000 0.000 0.014(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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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_
_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
K1 I1 K1 170.93(6) . 7_455 ?
I1 K1 I1 97.93(4) 3_665 14_654 ?
I1 K1 I1 170.93(6) 3_665 15_554 ?
I1 K1 I1 88.756(5) 14_654 15_554 ?
I1 K1 I1 88.756(5) 3_665 2_655 ?
I1 K1 I1 170.93(6) 14_654 2_655 ?
I1 K1 I1 85.29(4) 15_554 2_655 ?
I1 K1 I1 88.756(5) 3_665 . ?
I1 K1 I1 85.29(4) 14_654 . ?
I1 K1 I1 97.94(4) 15_554 . ?
I1 K1 I1 88.757(5) 2_655 . ?
I1 K1 I1 85.29(4) 3_665 13_544 ?
I1 K1 I1 88.755(5) 14_654 13_544 ?
I1 K1 I1 88.755(5) 15_554 13_544 ?
I1 K1 I1 97.93(4) 2_655 13_544 ?
I1 K1 I1 170.93(6) . 13_544 ?
C1 N1 C1 109.9(13) 3_565 2_665 ?
C1 N1 C1 109.9(13) 3_565 . ?
C1 N1 C1 109.9(13) 2_665 . ?
N1 C1 C1 108.1(14) . 12 ?
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
I1 K1 3.4732(2) . ?
I1 K1 3.4733(2) 7_455 ?
N1 C1 1.48(2) 3_565 ?
N1 C1 1.48(2) 2_665 ?
N1 C1 1.48(2) . ?
C1 C1 1.54(4) 12 ?
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
C1 H1A I1 0.99 3.14 4.01(2) 147.6 13_444 yes
C1 H1B I1 0.99 3.10 3.87(2) 135.5 . yes
C1 H1A I1 0.99 3.14 4.01(2) 147.6 13_444 yes
C1 H1B I1 0.99 3.10 3.87(2) 135.5 . yes
