#------------------------------------------------------------------------------ #$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 '\w 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/[\s^2^(Fo^2^)+(0.0254P)^2^+89.3544P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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