#------------------------------------------------------------------------------ #$Date: 2023-10-27 04:20:56 +0300 (Fri, 27 Oct 2023) $ #$Revision: 287134 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/75/7247589.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_7247589 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.cc2h9bsy _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 74.3060(10) _cell_angle_beta 85.9270(10) _cell_angle_gamma 88.0170(10) _cell_formula_units_Z 2 _cell_length_a 7.2844(2) _cell_length_b 10.1024(3) _cell_length_c 10.1051(3) _cell_measurement_reflns_used 9931 _cell_measurement_temperature 300(2) _cell_measurement_theta_max 25.89 _cell_measurement_theta_min 2.53 _cell_volume 714.01(4) _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 300(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _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 0.0272 _diffrn_reflns_av_unetI/netI 0.0164 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _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 26702 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.294 _diffrn_reflns_theta_min 2.098 _exptl_absorpt_coefficient_mu 2.435 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6723 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.513 _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 0.716 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 118 _refine_ls_number_reflns 3538 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0359 _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^)+(0.0502P)^2^+0.4098P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.1046 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2812 _reflns_number_total 3538 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ra05752f1.cif _cod_data_source_block NH3CH26NH3ZnCl4_300K_a _cod_database_code 7247589 _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 0.544 _shelx_estimated_absorpt_t_max 0.811 _shelx_res_file ; TITL NH3CH26NH3ZnCl4_300K_a.res in P-1 NH3CH26NH3ZnCl4_300K_a.res created by SHELXL-2018/3 at 14:33:43 on 23-Dec-2022 REM Old TITL NH3CH26NH3ZnCl4_300K in P-1 REM SHELXT solution in P-1 REM R1 0.119, Rweak 0.009, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C6 Cl4 N2 Zn CELL 0.71073 7.2844 10.1024 10.1051 74.306 85.927 88.017 ZERR 2.000 0.0002 0.0003 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H CL N ZN UNIT 12 36 8 4 2 TEMP 27.000 SIZE 0.09 0.095 0.285 L.S. 10 BOND $H LIST 4 FMAP 2 PLAN 20 ACTA omit 0 1 0 WGHT 0.050200 0.409800 FVAR 0.97901 ZN1 5 0.738992 0.558371 0.706649 11.00000 0.04542 0.05595 = 0.05792 -0.00903 -0.00283 -0.00102 CL1 3 0.690589 0.328128 0.789355 11.00000 0.06017 0.05423 = 0.06111 -0.00525 -0.00034 0.00036 CL2 3 0.498025 0.666761 0.792028 11.00000 0.04513 0.06380 = 0.07677 -0.01997 -0.00427 0.00442 CL3 3 0.992937 0.618485 0.793032 11.00000 0.04214 0.08764 = 0.07318 -0.02175 -0.00263 -0.00732 CL4 3 0.759187 0.620475 0.475490 11.00000 0.10734 0.06626 = 0.05355 -0.00349 -0.00102 0.00200 N1 4 0.740590 0.285412 0.485624 11.00000 0.07955 0.05391 = 0.06114 -0.01146 -0.00265 -0.00848 AFIX 33 H1NA 2 0.819754 0.341400 0.427509 11.00000 -1.50000 H1NB 2 0.633601 0.289061 0.447277 11.00000 -1.50000 H1NC 2 0.723610 0.311458 0.563053 11.00000 -1.50000 AFIX 0 N2 4 0.277660 0.363155 0.922245 11.00000 0.05318 0.05962 = 0.07044 -0.00819 0.00326 -0.00961 AFIX 33 H2NA 2 0.229304 0.444924 0.881579 11.00000 -1.50000 H2NB 2 0.287118 0.356290 1.011188 11.00000 -1.50000 H2NC 2 0.388829 0.354247 0.882687 11.00000 -1.50000 AFIX 0 C1 1 0.815045 0.143029 0.517253 11.00000 0.07377 0.06244 = 0.11683 -0.01197 -0.01955 0.00149 AFIX 23 H1A 2 0.933041 0.140641 0.556765 11.00000 -1.20000 H1AB 2 0.836035 0.116503 0.431989 11.00000 -1.20000 AFIX 0 C2 1 0.692941 0.041312 0.613686 11.00000 0.14071 0.06271 = 0.11302 -0.00501 -0.03444 0.00321 AFIX 23 H2A 2 0.674582 0.067170 0.699454 11.00000 -1.20000 H2AB 2 0.755014 -0.047727 0.633655 11.00000 -1.20000 AFIX 0 C3 1 0.498424 0.026208 0.560378 11.00000 0.09264 0.06219 = 0.12173 -0.00752 0.00288 0.00233 AFIX 23 H3A 2 0.425146 -0.034760 0.634429 11.00000 -1.20000 H3AB 2 0.437167 0.115559 0.539140 11.00000 -1.20000 AFIX 0 C4 1 0.158499 0.254342 0.907867 11.00000 0.08351 0.06949 = 0.06790 -0.00851 -0.01145 -0.01749 AFIX 23 H4A 2 0.036915 0.266453 0.949133 11.00000 -1.20000 H4AB 2 0.146521 0.264252 0.810659 11.00000 -1.20000 AFIX 0 C5 1 0.224650 0.117832 0.970315 11.00000 0.10791 0.08101 = 0.14156 -0.00458 -0.03503 -0.00101 AFIX 23 H5A 2 0.242113 0.108665 1.066675 11.00000 -1.20000 H5AB 2 0.343282 0.103452 0.925890 11.00000 -1.20000 AFIX 0 C6 1 0.087767 0.003488 0.959140 11.00000 0.12763 0.06815 = 0.15611 -0.01860 -0.02418 -0.01061 AFIX 23 H6A 2 0.061922 0.019319 0.863199 11.00000 -1.20000 H6AB 2 0.149700 -0.085298 0.987118 11.00000 -1.20000 AFIX 0 HKLF 4 REM NH3CH26NH3ZnCl4_300K_a.res in P-1 REM wR2 = 0.104568, GooF = S = 1.04244, Restrained GooF = 1.04244 for all data REM R1 = 0.035942 for 2812 Fo > 4sig(Fo) and 0.047954 for all 3538 data REM 118 parameters refined using 0 restraints END WGHT 0.0502 0.4098 REM Highest difference peak 0.716, deepest hole -0.367, 1-sigma level 0.060 Q1 1 0.0674 0.1670 1.0125 11.00000 0.05 0.72 Q2 1 0.7305 0.0531 0.4562 11.00000 0.05 0.70 Q3 1 0.6731 0.5906 0.4517 11.00000 0.05 0.39 Q4 1 0.2688 0.2099 0.9138 11.00000 0.05 0.39 Q5 1 0.4579 -0.0573 0.5441 11.00000 0.05 0.35 Q6 1 0.0240 -0.0649 1.0361 11.00000 0.05 0.34 Q7 1 0.5363 0.0409 0.6552 11.00000 0.05 0.32 Q8 1 0.2189 0.0000 0.9167 11.00000 0.05 0.29 Q9 1 0.7551 0.6958 0.4631 11.00000 0.05 0.28 Q10 1 0.9661 0.5369 0.8118 11.00000 0.05 0.25 Q11 1 0.9854 0.6430 0.7060 11.00000 0.05 0.23 Q12 1 0.5838 0.7159 0.7588 11.00000 0.05 0.23 Q13 1 0.8335 0.5973 0.4629 11.00000 0.05 0.23 Q14 1 0.7474 0.5570 0.5752 11.00000 0.05 0.21 Q15 1 0.5401 0.7449 0.7873 11.00000 0.05 0.21 Q16 1 0.5110 0.6197 0.8624 11.00000 0.05 0.18 Q17 1 0.7728 0.6383 0.6857 11.00000 0.05 0.18 Q18 1 0.6170 0.5834 0.7997 11.00000 0.05 0.17 Q19 1 0.1521 0.1426 0.8585 11.00000 0.05 0.17 Q20 1 0.7003 0.4329 0.7599 11.00000 0.05 0.16 ; _shelx_res_checksum 12580 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 0.73899(4) 0.55837(3) 0.70665(3) 0.05434(13) Uani 1 1 d . . . . . Cl1 Cl 0.69059(11) 0.32813(7) 0.78936(8) 0.06071(19) Uani 1 1 d . . . . . Cl2 Cl 0.49803(10) 0.66676(8) 0.79203(8) 0.0618(2) Uani 1 1 d . . . . . Cl3 Cl 0.99294(10) 0.61848(9) 0.79303(9) 0.0675(2) Uani 1 1 d . . . . . Cl4 Cl 0.75919(15) 0.62047(9) 0.47549(8) 0.0785(3) Uani 1 1 d . . . . . N1 N 0.7406(4) 0.2854(3) 0.4856(3) 0.0656(7) Uani 1 1 d . . . . . H1NA H 0.819754 0.341400 0.427509 0.098 Uiso 1 1 calc R U . . . H1NB H 0.633601 0.289061 0.447277 0.098 Uiso 1 1 calc R U . . . H1NC H 0.723610 0.311458 0.563053 0.098 Uiso 1 1 calc R U . . . N2 N 0.2777(3) 0.3632(3) 0.9222(3) 0.0630(6) Uani 1 1 d . . . . . H2NA H 0.229304 0.444924 0.881579 0.095 Uiso 1 1 calc R U . . . H2NB H 0.287118 0.356290 1.011188 0.095 Uiso 1 1 calc R U . . . H2NC H 0.388829 0.354247 0.882687 0.095 Uiso 1 1 calc R U . . . C1 C 0.8150(6) 0.1430(4) 0.5173(5) 0.0861(11) Uani 1 1 d . . . . . H1A H 0.933041 0.140641 0.556765 0.103 Uiso 1 1 calc R U . . . H1AB H 0.836035 0.116503 0.431989 0.103 Uiso 1 1 calc R U . . . C2 C 0.6929(8) 0.0413(4) 0.6137(6) 0.1079(16) Uani 1 1 d . . . . . H2A H 0.674582 0.067170 0.699454 0.130 Uiso 1 1 calc R U . . . H2AB H 0.755014 -0.047727 0.633655 0.130 Uiso 1 1 calc R U . . . C3 C 0.4984(7) 0.0262(4) 0.5604(5) 0.0961(13) Uani 1 1 d . . . . . H3A H 0.425146 -0.034760 0.634429 0.115 Uiso 1 1 calc R U . . . H3AB H 0.437167 0.115559 0.539140 0.115 Uiso 1 1 calc R U . . . C4 C 0.1585(6) 0.2543(4) 0.9079(4) 0.0749(9) Uani 1 1 d . . . . . H4A H 0.036915 0.266453 0.949133 0.090 Uiso 1 1 calc R U . . . H4AB H 0.146521 0.264252 0.810659 0.090 Uiso 1 1 calc R U . . . C5 C 0.2246(8) 0.1178(5) 0.9703(6) 0.1138(17) Uani 1 1 d . . . . . H5A H 0.242113 0.108665 1.066675 0.137 Uiso 1 1 calc R U . . . H5AB H 0.343282 0.103452 0.925890 0.137 Uiso 1 1 calc R U . . . C6 C 0.0878(7) 0.0035(5) 0.9591(7) 0.1186(18) Uani 1 1 d . . . . . H6A H 0.061922 0.019319 0.863199 0.142 Uiso 1 1 calc R U . . . H6AB H 0.149700 -0.085298 0.987118 0.142 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 0.04542(19) 0.0560(2) 0.0579(2) -0.00903(15) -0.00283(14) -0.00102(14) Cl1 0.0602(4) 0.0542(4) 0.0611(4) -0.0053(3) -0.0003(3) 0.0004(3) Cl2 0.0451(3) 0.0638(4) 0.0768(5) -0.0200(4) -0.0043(3) 0.0044(3) Cl3 0.0421(3) 0.0876(5) 0.0732(5) -0.0218(4) -0.0026(3) -0.0073(3) Cl4 0.1073(7) 0.0663(5) 0.0535(4) -0.0035(3) -0.0010(4) 0.0020(5) N1 0.0795(18) 0.0539(14) 0.0611(15) -0.0115(11) -0.0027(13) -0.0085(12) N2 0.0532(14) 0.0596(14) 0.0704(16) -0.0082(12) 0.0033(12) -0.0096(11) C1 0.074(2) 0.062(2) 0.117(3) -0.012(2) -0.020(2) 0.0015(17) C2 0.141(4) 0.063(2) 0.113(4) -0.005(2) -0.034(3) 0.003(3) C3 0.093(3) 0.062(2) 0.122(4) -0.008(2) 0.003(3) 0.002(2) C4 0.084(2) 0.069(2) 0.068(2) -0.0085(16) -0.0114(17) -0.0175(18) C5 0.108(4) 0.081(3) 0.142(5) -0.005(3) -0.035(3) -0.001(3) C6 0.128(4) 0.068(2) 0.156(5) -0.019(3) -0.024(4) -0.011(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' 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 Cl4 Zn1 Cl3 111.62(4) . . ? Cl4 Zn1 Cl2 111.39(4) . . ? Cl3 Zn1 Cl2 105.62(3) . . ? Cl4 Zn1 Cl1 110.65(3) . . ? Cl3 Zn1 Cl1 110.55(3) . . ? Cl2 Zn1 Cl1 106.80(3) . . ? 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 . . ? N1 C1 C2 113.7(4) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1AB 108.8 . . ? C2 C1 H1AB 108.8 . . ? H1A C1 H1AB 107.7 . . ? C1 C2 C3 115.1(4) . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2AB 108.5 . . ? C3 C2 H2AB 108.5 . . ? H2A C2 H2AB 107.5 . . ? C3 C3 C2 115.3(5) 2_656 . ? C3 C3 H3A 108.4 2_656 . ? C2 C3 H3A 108.4 . . ? C3 C3 H3AB 108.4 2_656 . ? C2 C3 H3AB 108.4 . . ? H3A C3 H3AB 107.5 . . ? C5 C4 N2 113.9(4) . . ? C5 C4 H4A 108.8 . . ? N2 C4 H4A 108.8 . . ? C5 C4 H4AB 108.8 . . ? N2 C4 H4AB 108.8 . . ? H4A C4 H4AB 107.7 . . ? C4 C5 C6 112.4(4) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5AB 109.1 . . ? C6 C5 H5AB 109.1 . . ? H5A C5 H5AB 107.9 . . ? C6 C6 C5 115.9(6) 2_557 . ? C6 C6 H6A 108.3 2_557 . ? C5 C6 H6A 108.3 . . ? C6 C6 H6AB 108.3 2_557 . ? C5 C6 H6AB 108.3 . . ? H6A C6 H6AB 107.4 . . ? 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 Zn1 Cl4 2.2442(9) . ? Zn1 Cl3 2.2686(8) . ? Zn1 Cl2 2.2776(8) . ? Zn1 Cl1 2.2795(8) . ? N1 C1 1.479(4) . ? N1 H1NA 0.8900 . ? N1 H1NB 0.8900 . ? N1 H1NC 0.8900 . ? N2 C4 1.467(4) . ? N2 H2NA 0.8900 . ? N2 H2NB 0.8900 . ? N2 H2NC 0.8900 . ? C1 C2 1.482(6) . ? C1 H1A 0.9700 . ? C1 H1AB 0.9700 . ? C2 C3 1.578(7) . ? C2 H2A 0.9700 . ? C2 H2AB 0.9700 . ? C3 C3 1.454(9) 2_656 ? C3 H3A 0.9700 . ? C3 H3AB 0.9700 . ? C4 C5 1.435(6) . ? C4 H4A 0.9700 . ? C4 H4AB 0.9700 . ? C5 C6 1.584(7) . ? C5 H5A 0.9700 . ? C5 H5AB 0.9700 . ? C6 C6 1.465(11) 2_557 ? C6 H6A 0.9700 . ? C6 H6AB 0.9700 . ?