#------------------------------------------------------------------------------ #$Date: 2023-10-27 04:20:56 +0300 (Fri, 27 Oct 2023) $ #$Revision: 287134 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247588.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_7247588 loop_ _publ_author_name 'Lim, Ae Ran' 'Kim, Sun Ha' _publ_section_title ; Processing on crystal growth, structure, thermal property, and nuclear magnetic resonance of organic--inorganic hybrid perovskite type [NH3(CH2)6NH3]ZnCl4 crystal ; _journal_issue 44 _journal_name_full 'RSC Advances' _journal_page_first 31027 _journal_page_last 31035 _journal_paper_doi 10.1039/D3RA05752F _journal_volume 13 _journal_year 2023 _chemical_formula_moiety 'C6 H18 N2, Cl4 Zn' _chemical_formula_sum 'C6 H18 Cl4 N2 Zn' _chemical_formula_weight 325.39 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc2ghbt4 _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-10-21 deposited with the CCDC. 2023-10-24 downloaded from the CCDC. ; _cell_angle_alpha 75.028(2) _cell_angle_beta 86.496(2) _cell_angle_gamma 88.354(2) _cell_formula_units_Z 2 _cell_length_a 7.2757(4) _cell_length_b 10.0165(6) _cell_length_c 10.0348(6) _cell_measurement_reflns_used 7784 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 28.40 _cell_measurement_theta_min 2.57 _cell_volume 705.10(7) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 250(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0242 _diffrn_reflns_av_unetI/netI 0.0204 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 14848 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.452 _diffrn_reflns_theta_min 2.565 _exptl_absorpt_coefficient_mu 2.465 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.533 _exptl_crystal_description BLOCK _exptl_crystal_F_000 332 _exptl_crystal_size_max 0.285 _exptl_crystal_size_mid 0.095 _exptl_crystal_size_min 0.090 _refine_diff_density_max 0.484 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.053 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 3539 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0369 _refine_ls_R_factor_gt 0.0283 _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/[\s^2^(Fo^2^)+(0.0322P)^2^+0.3207P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.0740 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2961 _reflns_number_total 3539 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra05752f1.cif _cod_data_source_block NH3CH26NH3ZnCl4_250K_a _cod_database_code 7247588 _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_estimated_absorpt_t_min 0.540 _shelx_estimated_absorpt_t_max 0.809 _shelx_res_file ; TITL NH3CH26NH3ZnCl4_250K_a.res in P-1 NH3CH26NH3ZnCl4_250K_a.res created by SHELXL-2018/3 at 14:29:24 on 23-Dec-2022 REM Old TITL NH3CH26NH3ZnCl4_250K in P-1 REM SHELXT solution in P-1 REM R1 0.109, Rweak 0.007, Alpha 0.031, Orientation as input REM Formula found by SHELXT: C6 Cl4 N2 Zn CELL 0.71073 7.2757 10.0165 10.0348 75.028 86.496 88.354 ZERR 2.000 0.0004 0.0006 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H CL N ZN UNIT 12 36 8 4 2 TEMP -23.000 SIZE 0.09 0.095 0.285 L.S. 10 BOND $H LIST 4 FMAP 2 PLAN 20 ACTA omit -1 2 1 omit 0 1 0 omit 2 1 1 omit 1 -1 1 omit -2 -1 1 OMIT 0 1 2 WGHT 0.032200 0.320700 FVAR 1.01163 ZN1 5 0.739159 0.559340 0.706229 11.00000 0.03604 0.04152 = 0.04508 -0.00585 -0.00097 -0.00103 CL1 3 0.760536 0.619048 0.474268 11.00000 0.08853 0.04976 = 0.04234 -0.00174 -0.00005 0.00272 CL2 3 0.498494 0.669216 0.791038 11.00000 0.03554 0.04614 = 0.05875 -0.01298 -0.00191 0.00279 CL3 3 0.689888 0.327881 0.789308 11.00000 0.04485 0.04009 = 0.04655 -0.00354 0.00019 -0.00014 CL4 3 0.993180 0.622107 0.794441 11.00000 0.03400 0.06194 = 0.05602 -0.01378 -0.00105 -0.00529 N1 4 0.277788 0.365433 0.918390 11.00000 0.04231 0.04295 = 0.05339 -0.00425 0.00252 -0.00656 AFIX 33 H1NA 2 0.228641 0.449086 0.880319 11.00000 -1.50000 H1NB 2 0.294111 0.357421 1.008317 11.00000 -1.50000 H1NC 2 0.387103 0.356015 0.874474 11.00000 -1.50000 AFIX 0 N2 4 0.745045 0.283246 0.484478 11.00000 0.06315 0.03926 = 0.04560 -0.00647 -0.00012 -0.00701 AFIX 33 H2NA 2 0.823825 0.340040 0.424984 11.00000 -1.50000 H2NB 2 0.635401 0.286485 0.446733 11.00000 -1.50000 H2NC 2 0.730663 0.310232 0.563396 11.00000 -1.50000 AFIX 0 C1 1 0.152004 0.256531 0.905333 11.00000 0.05439 0.04922 = 0.04641 -0.00404 -0.00723 -0.01103 AFIX 23 H1A 2 0.032425 0.268518 0.951608 11.00000 -1.20000 H1AB 2 0.132655 0.267003 0.807348 11.00000 -1.20000 AFIX 0 C2 1 0.224090 0.115771 0.965891 11.00000 0.06075 0.05307 = 0.09681 0.00088 -0.01263 -0.00213 AFIX 23 H2A 2 0.247454 0.106083 1.063107 11.00000 -1.20000 H2AB 2 0.341436 0.102332 0.917389 11.00000 -1.20000 AFIX 0 C3 1 0.087285 0.002605 0.955994 11.00000 0.07984 0.04654 = 0.10658 -0.01206 -0.00320 -0.00797 AFIX 23 H3A 2 0.055935 0.018478 0.859494 11.00000 -1.20000 H3AB 2 0.149513 -0.087678 0.982464 11.00000 -1.20000 AFIX 0 C4 1 0.819821 0.139437 0.514756 11.00000 0.05468 0.04593 = 0.08795 -0.01086 -0.01081 0.00089 AFIX 23 H4A 2 0.940349 0.136917 0.553987 11.00000 -1.20000 H4AB 2 0.837668 0.111321 0.428238 11.00000 -1.20000 AFIX 0 C5 1 0.694678 0.038249 0.614076 11.00000 0.09428 0.04160 = 0.07548 -0.00118 -0.01729 -0.00093 AFIX 23 H5A 2 0.680838 0.065494 0.701226 11.00000 -1.20000 H5AB 2 0.754119 -0.053259 0.633444 11.00000 -1.20000 AFIX 0 C6 1 0.500711 0.026544 0.563223 11.00000 0.06516 0.03992 = 0.07547 -0.00413 0.00485 -0.00254 AFIX 23 H6A 2 0.427023 -0.035030 0.637894 11.00000 -1.20000 H6AB 2 0.441093 0.117990 0.543795 11.00000 -1.20000 AFIX 0 HKLF 4 REM NH3CH26NH3ZnCl4_250K_a.res in P-1 REM wR2 = 0.074025, GooF = S = 1.03920, Restrained GooF = 1.03920 for all data REM R1 = 0.028293 for 2961 Fo > 4sig(Fo) and 0.036932 for all 3539 data REM 118 parameters refined using 0 restraints END WGHT 0.0322 0.3207 REM Highest difference peak 0.484, deepest hole -0.387, 1-sigma level 0.053 Q1 1 0.0708 0.1720 1.0144 11.00000 0.05 0.48 Q2 1 0.6805 0.5831 0.4571 11.00000 0.05 0.43 Q3 1 0.7232 0.0423 0.4576 11.00000 0.05 0.41 Q4 1 0.0169 -0.0543 1.0278 11.00000 0.05 0.36 Q5 1 0.4616 -0.0493 0.5345 11.00000 0.05 0.33 Q6 1 0.2522 0.2097 0.9083 11.00000 0.05 0.33 Q7 1 0.5593 0.0393 0.6496 11.00000 0.05 0.30 Q8 1 0.9879 0.6389 0.7026 11.00000 0.05 0.27 Q9 1 0.2095 0.0081 0.9073 11.00000 0.05 0.27 Q10 1 0.8334 0.5843 0.4752 11.00000 0.05 0.26 Q11 1 0.5258 0.7403 0.7798 11.00000 0.05 0.24 Q12 1 0.7592 0.6822 0.4838 11.00000 0.05 0.24 Q13 1 0.6201 0.3307 0.7426 11.00000 0.05 0.21 Q14 1 0.5076 0.6125 0.8593 11.00000 0.05 0.20 Q15 1 0.7706 0.5499 0.5768 11.00000 0.05 0.20 Q16 1 0.7181 0.5927 0.5806 11.00000 0.05 0.20 Q17 1 0.9699 0.5399 0.8182 11.00000 0.05 0.19 Q18 1 0.8836 0.5656 0.7670 11.00000 0.05 0.19 Q19 1 1.0127 0.5371 0.7871 11.00000 0.05 0.19 Q20 1 0.7388 0.4248 0.7808 11.00000 0.05 0.17 ; _shelx_res_checksum 80788 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Zn1 Zn 0.73916(3) 0.55934(2) 0.70623(3) 0.04190(9) Uani 1 1 d . . . . . Cl1 Cl 0.76054(11) 0.61905(6) 0.47427(6) 0.06230(17) Uani 1 1 d . . . . . Cl2 Cl 0.49849(7) 0.66922(6) 0.79104(6) 0.04700(13) Uani 1 1 d . . . . . Cl3 Cl 0.68989(7) 0.32788(5) 0.78931(6) 0.04536(13) Uani 1 1 d . . . . . Cl4 Cl 0.99318(7) 0.62211(6) 0.79444(6) 0.05088(14) Uani 1 1 d . . . . . N1 N 0.2778(3) 0.36543(19) 0.9184(2) 0.0478(4) Uani 1 1 d . . . . . H1NA H 0.228641 0.449086 0.880319 0.072 Uiso 1 1 calc R U . . . H1NB H 0.294111 0.357421 1.008317 0.072 Uiso 1 1 calc R U . . . H1NC H 0.387103 0.356015 0.874474 0.072 Uiso 1 1 calc R U . . . N2 N 0.7450(3) 0.28325(19) 0.4845(2) 0.0502(5) Uani 1 1 d . . . . . H2NA H 0.823825 0.340040 0.424984 0.075 Uiso 1 1 calc R U . . . H2NB H 0.635401 0.286485 0.446733 0.075 Uiso 1 1 calc R U . . . H2NC H 0.730663 0.310232 0.563396 0.075 Uiso 1 1 calc R U . . . C1 C 0.1520(3) 0.2565(2) 0.9053(2) 0.0511(5) Uani 1 1 d . . . . . H1A H 0.032425 0.268518 0.951608 0.061 Uiso 1 1 calc R U . . . H1AB H 0.132655 0.267003 0.807348 0.061 Uiso 1 1 calc R U . . . C2 C 0.2241(4) 0.1158(3) 0.9659(4) 0.0736(8) Uani 1 1 d . . . . . H2A H 0.247454 0.106083 1.063107 0.088 Uiso 1 1 calc R U . . . H2AB H 0.341436 0.102332 0.917389 0.088 Uiso 1 1 calc R U . . . C3 C 0.0873(4) 0.0026(3) 0.9560(4) 0.0790(9) Uani 1 1 d . . . . . H3A H 0.055935 0.018478 0.859494 0.095 Uiso 1 1 calc R U . . . H3AB H 0.149513 -0.087678 0.982464 0.095 Uiso 1 1 calc R U . . . C4 C 0.8198(4) 0.1394(3) 0.5148(3) 0.0638(7) Uani 1 1 d . . . . . H4A H 0.940349 0.136917 0.553987 0.077 Uiso 1 1 calc R U . . . H4AB H 0.837668 0.111321 0.428238 0.077 Uiso 1 1 calc R U . . . C5 C 0.6947(5) 0.0382(3) 0.6141(3) 0.0725(8) Uani 1 1 d . . . . . H5A H 0.680838 0.065494 0.701226 0.087 Uiso 1 1 calc R U . . . H5AB H 0.754119 -0.053259 0.633444 0.087 Uiso 1 1 calc R U . . . C6 C 0.5007(4) 0.0265(3) 0.5632(3) 0.0625(7) Uani 1 1 d . . . . . H6A H 0.427023 -0.035030 0.637894 0.075 Uiso 1 1 calc R U . . . H6AB H 0.441093 0.117990 0.543795 0.075 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 Zn1 0.03604(13) 0.04152(14) 0.04508(15) -0.00585(10) -0.00097(10) -0.00103(10) Cl1 0.0885(5) 0.0498(3) 0.0423(3) -0.0017(2) -0.0001(3) 0.0027(3) Cl2 0.0355(2) 0.0461(3) 0.0587(3) -0.0130(2) -0.0019(2) 0.0028(2) Cl3 0.0448(3) 0.0401(3) 0.0466(3) -0.0035(2) 0.0002(2) -0.0001(2) Cl4 0.0340(3) 0.0619(3) 0.0560(3) -0.0138(3) -0.0011(2) -0.0053(2) N1 0.0423(10) 0.0430(10) 0.0534(11) -0.0043(8) 0.0025(8) -0.0066(8) N2 0.0631(12) 0.0393(10) 0.0456(10) -0.0065(8) -0.0001(9) -0.0070(9) C1 0.0544(13) 0.0492(13) 0.0464(12) -0.0040(10) -0.0072(10) -0.0110(10) C2 0.0607(17) 0.0531(15) 0.097(2) 0.0009(15) -0.0126(16) -0.0021(13) C3 0.080(2) 0.0465(15) 0.107(3) -0.0121(15) -0.0032(18) -0.0080(14) C4 0.0547(15) 0.0459(13) 0.088(2) -0.0109(13) -0.0108(14) 0.0009(11) C5 0.094(2) 0.0416(13) 0.0755(19) -0.0012(12) -0.0173(17) -0.0009(14) C6 0.0652(16) 0.0399(12) 0.0755(18) -0.0041(11) 0.0048(14) -0.0025(11) 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' Cl Cl 0.1484 0.1585 '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' Zn Zn 0.2839 1.4301 '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 Zn1 Cl4 111.39(3) . . ? Cl1 Zn1 Cl2 111.72(3) . . ? Cl4 Zn1 Cl2 105.40(2) . . ? Cl1 Zn1 Cl3 110.77(2) . . ? Cl4 Zn1 Cl3 110.71(2) . . ? Cl2 Zn1 Cl3 106.64(2) . . ? C1 N1 H1NA 109.5 . . ? C1 N1 H1NB 109.5 . . ? H1NA N1 H1NB 109.5 . . ? C1 N1 H1NC 109.5 . . ? H1NA N1 H1NC 109.5 . . ? H1NB N1 H1NC 109.5 . . ? C4 N2 H2NA 109.5 . . ? C4 N2 H2NB 109.5 . . ? H2NA N2 H2NB 109.5 . . ? C4 N2 H2NC 109.5 . . ? H2NA N2 H2NC 109.5 . . ? H2NB N2 H2NC 109.5 . . ? C2 C1 N1 112.5(2) . . ? C2 C1 H1A 109.1 . . ? N1 C1 H1A 109.1 . . ? C2 C1 H1AB 109.1 . . ? N1 C1 H1AB 109.1 . . ? H1A C1 H1AB 107.8 . . ? C1 C2 C3 111.9(2) . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2AB 109.2 . . ? C3 C2 H2AB 109.2 . . ? H2A C2 H2AB 107.9 . . ? C3 C3 C2 114.8(3) 2_557 . ? C3 C3 H3A 108.6 2_557 . ? C2 C3 H3A 108.6 . . ? C3 C3 H3AB 108.6 2_557 . ? C2 C3 H3AB 108.6 . . ? H3A C3 H3AB 107.6 . . ? N2 C4 C5 112.4(2) . . ? N2 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? N2 C4 H4AB 109.1 . . ? C5 C4 H4AB 109.1 . . ? H4A C4 H4AB 107.8 . . ? C4 C5 C6 115.0(2) . . ? C4 C5 H5A 108.5 . . ? C6 C5 H5A 108.5 . . ? C4 C5 H5AB 108.5 . . ? C6 C5 H5AB 108.5 . . ? H5A C5 H5AB 107.5 . . ? C6 C6 C5 114.6(3) 2_656 . ? C6 C6 H6A 108.6 2_656 . ? C5 C6 H6A 108.6 . . ? C6 C6 H6AB 108.6 2_656 . ? C5 C6 H6AB 108.6 . . ? H6A C6 H6AB 107.6 . . ? 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 Zn1 Cl1 2.2454(7) . ? Zn1 Cl4 2.2691(6) . ? Zn1 Cl2 2.2787(6) . ? Zn1 Cl3 2.2828(6) . ? N1 C1 1.480(3) . ? N1 H1NA 0.9000 . ? N1 H1NB 0.9000 . ? N1 H1NC 0.9000 . ? N2 C4 1.487(3) . ? N2 H2NA 0.9000 . ? N2 H2NB 0.9000 . ? N2 H2NC 0.9000 . ? C1 C2 1.479(4) . ? C1 H1A 0.9800 . ? C1 H1AB 0.9800 . ? C2 C3 1.556(4) . ? C2 H2A 0.9800 . ? C2 H2AB 0.9800 . ? C3 C3 1.496(6) 2_557 ? C3 H3A 0.9800 . ? C3 H3AB 0.9800 . ? C4 C5 1.507(4) . ? C4 H4A 0.9800 . ? C4 H4AB 0.9800 . ? C5 C6 1.547(4) . ? C5 H5A 0.9800 . ? C5 H5AB 0.9800 . ? C6 C6 1.498(6) 2_656 ? C6 H6A 0.9800 . ? C6 H6AB 0.9800 . ?