#------------------------------------------------------------------------------ #$Date: 2026-05-20 01:40:27 +0100 (Wed, 20 May 2026) $ #$Revision: 306001 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064413.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_7064413 loop_ _publ_author_name '\/Lyczko, Krzysztof' 'Lyczko, Monika' 'Bednarek, El\.zbieta' 'Khalaj, Mehdi' 'W\;egrzy\'nska, Karolina' 'Baraniak, Anna' 'Persson, Ingmar' _publ_section_title ; Synthesis, structural and spectroscopic characterization of zinc(II) iodide complex with 2-[(4-iodophenyl)iminomethyl]pyridine in the solid state and solution † ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ01605G _journal_year 2026 _chemical_formula_moiety 'C12 H9 I3 N2 Zn' _chemical_formula_sum 'C12 H9 I3 N2 Zn' _chemical_formula_weight 627.28 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2026-03-30 _audit_creation_method ; Olex2 1.5 (compiled 2025.07.13 svn.rb7424aed for OlexSys, GUI svn.r7314) ; _audit_update_record ; 2026-04-29 deposited with the CCDC. 2026-05-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 113.799(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 15.4748(3) _cell_length_b 7.92606(11) _cell_length_c 14.2411(3) _cell_measurement_reflns_used 12654 _cell_measurement_temperature 100.0(1) _cell_measurement_theta_max 71.0940 _cell_measurement_theta_min 3.0960 _cell_volume 1598.20(6) _computing_cell_refinement 'CrysAlisPro (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2017/1 (Sheldrick, 2015)' _computing_structure_solution 'SHELXS (Sheldrick, 2008)' _diffrn_ambient_temperature 100.0(1) _diffrn_detector_area_resol_mean 16.0131 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Eos' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0509 _diffrn_reflns_av_unetI/netI 0.0236 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 22487 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.891 _diffrn_reflns_theta_min 3.121 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 47.509 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.10422 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro (Rigaku OD, 2022)' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.607 _exptl_crystal_description plate _exptl_crystal_F_000 1136 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.03 _refine_diff_density_max 1.628 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.205 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 3060 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.046 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0322 _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^)+(0.0611P)^2^+2.4292P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.0882 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2880 _reflns_number_total 3060 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj01605g2.cif _cod_data_source_block '[zni2(pycnphi)]' _cod_original_cell_volume 1598.19(5) _cod_database_code 7064413 _shelx_shelxl_version_number 2017/1 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12) ; _shelx_res_file ; TITL [ZnI2(pyCNPhI)]_auto in P21/c #14 [zni2(pycnphi)].res created by SHELXL-2017/1 at 15:33:57 on 30-Mar-2026 REM reset to P21/c #14 CELL 1.54184 15.474762 7.926059 14.241092 90 113.7992 90 ZERR 4 0.000279 0.000106 0.000275 0 0.0021 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N Zn UNIT 48 36 12 8 4 L.S. 20 PLAN 1 TEMP -173 CONF MORE -1 BOND $H fmap 2 acta MERG 2 REM REM REM WGHT 0.061100 2.429200 FVAR 1.52741 I1 3 0.663944 -0.261892 0.238251 11.00000 0.02163 0.01504 = 0.02450 -0.00217 0.00807 -0.00219 I2 3 0.920577 -0.228113 0.502558 11.00000 0.02056 0.01968 = 0.02405 0.00584 0.00806 0.00540 I3 3 0.524309 0.273715 0.652257 11.00000 0.01518 0.02520 = 0.02211 -0.00382 0.00710 -0.00021 ZN1 5 0.796470 -0.070515 0.351791 11.00000 0.01821 0.01264 = 0.02301 0.00164 0.00923 0.00161 N1 4 0.849175 0.073358 0.266884 11.00000 0.01376 0.01634 = 0.01960 0.00244 0.00436 0.00102 N2 4 0.757663 0.167079 0.382853 11.00000 0.01248 0.01294 = 0.02056 -0.00112 0.00217 0.00221 C1 1 0.893402 0.024700 0.208238 11.00000 0.01909 0.01461 = 0.02647 -0.00022 0.00978 0.00234 AFIX 43 H1 2 0.904446 -0.092242 0.203420 11.00000 -1.20000 AFIX 0 C2 1 0.924025 0.138440 0.153807 11.00000 0.01939 0.02440 = 0.02236 0.00127 0.00730 0.00046 AFIX 43 H2 2 0.956263 0.100076 0.113474 11.00000 -1.20000 AFIX 0 C3 1 0.906818 0.306714 0.159474 11.00000 0.01680 0.02348 = 0.02407 0.00085 0.00439 -0.00446 AFIX 43 H3 2 0.927032 0.386631 0.122864 11.00000 -1.20000 AFIX 0 C4 1 0.859889 0.359817 0.218719 11.00000 0.01794 0.01536 = 0.02727 -0.00152 0.00633 0.00090 AFIX 43 H4 2 0.846410 0.475930 0.222510 11.00000 -1.20000 AFIX 0 C5 1 0.832905 0.239742 0.272532 11.00000 0.01008 0.02009 = 0.02085 0.00025 0.00153 -0.00032 C6 1 0.782445 0.285570 0.337015 11.00000 0.01123 0.02009 = 0.02162 0.00136 0.00247 0.00134 AFIX 43 H6 2 0.768445 0.400140 0.344670 11.00000 -1.20000 AFIX 0 C7 1 0.706212 0.203305 0.444025 11.00000 0.01120 0.01979 = 0.01670 -0.00110 0.00141 0.00045 C8 1 0.692550 0.364265 0.474412 11.00000 0.02613 0.02019 = 0.02555 -0.00077 0.01102 -0.00193 AFIX 43 H8 2 0.718170 0.459586 0.454236 11.00000 -1.20000 AFIX 0 C9 1 0.641334 0.385379 0.534360 11.00000 0.02273 0.01734 = 0.02451 -0.00343 0.00685 0.00092 AFIX 43 H9 2 0.632636 0.495012 0.556082 11.00000 -1.20000 AFIX 0 C10 1 0.602792 0.245493 0.562522 11.00000 0.01199 0.02163 = 0.02460 -0.00152 0.00795 0.00190 C11 1 0.615642 0.085184 0.531797 11.00000 0.01394 0.02069 = 0.02618 0.00032 0.00554 -0.00144 AFIX 43 H11 2 0.589100 -0.009759 0.551166 11.00000 -1.20000 AFIX 0 C12 1 0.667345 0.063526 0.472687 11.00000 0.01669 0.01407 = 0.02276 -0.00354 0.00638 0.00051 AFIX 43 H12 2 0.676369 -0.046417 0.451638 11.00000 -1.20000 AFIX 0 HKLF 4 REM [ZnI2(pyCNPhI)]_auto in P21/c #14 REM R1 = 0.0322 for 2880 Fo > 4sig(Fo) and 0.0340 for all 3060 data REM 163 parameters refined using 0 restraints END WGHT 0.0611 2.4292 REM Highest difference peak 1.628, deepest hole -1.294, 1-sigma level 0.205 Q1 1 0.7577 -0.2497 0.2934 11.00000 0.05 1.63 ; _shelx_res_checksum 23936 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, 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 I1 I 0.66394(2) -0.26189(4) 0.23825(2) 0.02079(11) Uani 1 1 d . . . . . I2 I 0.92058(2) -0.22811(4) 0.50256(2) 0.02174(12) Uani 1 1 d . . . . . I3 I 0.52431(2) 0.27372(4) 0.65226(2) 0.02096(11) Uani 1 1 d . . . . . Zn1 Zn 0.79647(4) -0.07052(8) 0.35179(4) 0.01766(15) Uani 1 1 d . . . . . N1 N 0.8492(2) 0.0734(5) 0.2669(3) 0.0173(8) Uani 1 1 d . . . . . N2 N 0.7577(2) 0.1671(5) 0.3829(3) 0.0168(8) Uani 1 1 d . . . . . C1 C 0.8934(3) 0.0247(6) 0.2082(3) 0.0199(9) Uani 1 1 d . . . . . H1 H 0.904446 -0.092242 0.203420 0.024 Uiso 1 1 calc R U . . . C2 C 0.9240(3) 0.1384(7) 0.1538(4) 0.0224(10) Uani 1 1 d . . . . . H2 H 0.956263 0.100076 0.113474 0.027 Uiso 1 1 calc R U . . . C3 C 0.9068(3) 0.3067(7) 0.1595(4) 0.0227(10) Uani 1 1 d . . . . . H3 H 0.927032 0.386631 0.122864 0.027 Uiso 1 1 calc R U . . . C4 C 0.8599(3) 0.3598(6) 0.2187(4) 0.0211(9) Uani 1 1 d . . . . . H4 H 0.846410 0.475930 0.222510 0.025 Uiso 1 1 calc R U . . . C5 C 0.8329(3) 0.2397(6) 0.2725(4) 0.0185(10) Uani 1 1 d . . . . . C6 C 0.7824(3) 0.2856(6) 0.3370(4) 0.0190(9) Uani 1 1 d . . . . . H6 H 0.768445 0.400140 0.344670 0.023 Uiso 1 1 calc R U . . . C7 C 0.7062(3) 0.2033(6) 0.4440(3) 0.0173(9) Uani 1 1 d . . . . . C8 C 0.6926(3) 0.3643(7) 0.4744(4) 0.0238(10) Uani 1 1 d . . . . . H8 H 0.718170 0.459586 0.454236 0.029 Uiso 1 1 calc R U . . . C9 C 0.6413(3) 0.3854(6) 0.5344(4) 0.0224(10) Uani 1 1 d . . . . . H9 H 0.632636 0.495012 0.556082 0.027 Uiso 1 1 calc R U . . . C10 C 0.6028(3) 0.2455(6) 0.5625(4) 0.0192(10) Uani 1 1 d . . . . . C11 C 0.6156(3) 0.0852(6) 0.5318(4) 0.0211(10) Uani 1 1 d . . . . . H11 H 0.589100 -0.009759 0.551166 0.025 Uiso 1 1 calc R U . . . C12 C 0.6673(3) 0.0635(6) 0.4727(3) 0.0183(9) Uani 1 1 d . . . . . H12 H 0.676369 -0.046417 0.451638 0.022 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 0.02163(18) 0.01504(18) 0.0245(2) -0.00217(10) 0.00807(14) -0.00219(9) I2 0.02056(18) 0.01968(19) 0.02405(19) 0.00584(11) 0.00806(13) 0.00540(10) I3 0.01518(17) 0.0252(2) 0.02211(19) -0.00382(11) 0.00710(13) -0.00021(10) Zn1 0.0182(3) 0.0126(3) 0.0230(3) 0.0016(2) 0.0092(2) 0.0016(2) N1 0.0138(16) 0.016(2) 0.0196(18) 0.0024(14) 0.0044(13) 0.0010(13) N2 0.0125(16) 0.0129(19) 0.0206(18) -0.0011(15) 0.0022(13) 0.0022(13) C1 0.019(2) 0.015(2) 0.026(2) -0.0002(18) 0.0098(17) 0.0023(16) C2 0.019(2) 0.024(3) 0.022(2) 0.001(2) 0.0073(17) 0.0005(18) C3 0.017(2) 0.023(3) 0.024(2) 0.001(2) 0.0044(18) -0.0045(18) C4 0.018(2) 0.015(2) 0.027(2) -0.0015(19) 0.0063(17) 0.0009(16) C5 0.010(2) 0.020(3) 0.021(2) 0.0002(17) 0.0015(19) -0.0003(14) C6 0.0112(19) 0.020(2) 0.022(2) 0.0014(19) 0.0025(17) 0.0013(16) C7 0.0112(19) 0.020(2) 0.017(2) -0.0011(18) 0.0014(16) 0.0004(16) C8 0.026(2) 0.020(3) 0.026(2) -0.0008(19) 0.0110(19) -0.0019(18) C9 0.023(2) 0.017(2) 0.025(2) -0.0034(19) 0.0069(17) 0.0009(18) C10 0.012(2) 0.022(3) 0.025(3) -0.0015(17) 0.0080(19) 0.0019(15) C11 0.0139(19) 0.021(2) 0.026(2) 0.0003(19) 0.0055(17) -0.0014(16) C12 0.0167(19) 0.014(2) 0.023(2) -0.0035(18) 0.0064(16) 0.0005(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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 Zn1 I2 112.53(2) . . ? N1 Zn1 I1 111.54(10) . . ? N1 Zn1 I2 115.05(10) . . ? N1 Zn1 N2 80.78(15) . . ? N2 Zn1 I1 116.65(10) . . ? N2 Zn1 I2 116.61(10) . . ? C1 N1 Zn1 129.4(3) . . ? C1 N1 C5 118.4(4) . . ? C5 N1 Zn1 112.3(3) . . ? C6 N2 Zn1 112.5(3) . . ? C6 N2 C7 121.1(4) . . ? C7 N2 Zn1 126.4(3) . . ? N1 C1 H1 118.7 . . ? N1 C1 C2 122.6(4) . . ? C2 C1 H1 118.7 . . ? C1 C2 H2 120.6 . . ? C3 C2 C1 118.7(5) . . ? C3 C2 H2 120.6 . . ? C2 C3 H3 120.2 . . ? C2 C3 C4 119.7(5) . . ? C4 C3 H3 120.2 . . ? C3 C4 H4 120.7 . . ? C3 C4 C5 118.5(5) . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 122.1(5) . . ? N1 C5 C6 115.9(4) . . ? C4 C5 C6 122.0(4) . . ? N2 C6 C5 118.6(4) . . ? N2 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C8 C7 N2 124.6(5) . . ? C8 C7 C12 119.9(5) . . ? C12 C7 N2 115.5(4) . . ? C7 C8 H8 120.1 . . ? C9 C8 C7 119.9(5) . . ? C9 C8 H8 120.1 . . ? C8 C9 H9 120.1 . . ? C8 C9 C10 119.9(5) . . ? C10 C9 H9 120.1 . . ? C9 C10 I3 120.7(3) . . ? C11 C10 I3 118.8(4) . . ? C11 C10 C9 120.5(5) . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.8(5) . . ? C12 C11 H11 120.1 . . ? C7 C12 H12 120.0 . . ? C11 C12 C7 120.1(4) . . ? C11 C12 H12 120.0 . . ? 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 Zn1 2.5387(6) . ? I2 Zn1 2.5555(6) . ? I3 C10 2.100(5) . ? Zn1 N1 2.055(4) . ? Zn1 N2 2.078(4) . ? N1 C1 1.333(6) . ? N1 C5 1.351(6) . ? N2 C6 1.287(6) . ? N2 C7 1.427(6) . ? C1 H1 0.9500 . ? C1 C2 1.391(7) . ? C2 H2 0.9500 . ? C2 C3 1.369(8) . ? C3 H3 0.9500 . ? C3 C4 1.382(7) . ? C4 H4 0.9500 . ? C4 C5 1.388(7) . ? C5 C6 1.471(7) . ? C6 H6 0.9500 . ? C7 C8 1.390(7) . ? C7 C12 1.398(6) . ? C8 H8 0.9500 . ? C8 C9 1.390(7) . ? C9 H9 0.9500 . ? C9 C10 1.392(7) . ? C10 C11 1.384(7) . ? C11 H11 0.9500 . ? C11 C12 1.386(7) . ? C12 H12 0.9500 . ? 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 I3 C10 C11 C12 -179.9(3) . . . . ? Zn1 N1 C1 C2 179.1(3) . . . . ? Zn1 N1 C5 C4 -178.0(3) . . . . ? Zn1 N1 C5 C6 0.3(5) . . . . ? Zn1 N2 C6 C5 -0.4(5) . . . . ? Zn1 N2 C7 C8 170.9(3) . . . . ? Zn1 N2 C7 C12 -9.8(5) . . . . ? N1 C1 C2 C3 -1.0(6) . . . . ? N1 C5 C6 N2 0.0(6) . . . . ? N2 C7 C8 C9 -179.8(4) . . . . ? N2 C7 C12 C11 -179.7(4) . . . . ? C1 N1 C5 C4 0.6(6) . . . . ? C1 N1 C5 C6 179.0(4) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 1.1(6) . . . . ? C3 C4 C5 N1 -1.5(7) . . . . ? C3 C4 C5 C6 -179.8(4) . . . . ? C4 C5 C6 N2 178.4(4) . . . . ? C5 N1 C1 C2 0.6(6) . . . . ? C6 N2 C7 C8 -11.6(6) . . . . ? C6 N2 C7 C12 167.7(4) . . . . ? C7 N2 C6 C5 -178.2(4) . . . . ? C7 C8 C9 C10 -0.9(7) . . . . ? C8 C7 C12 C11 -0.3(6) . . . . ? C8 C9 C10 I3 -179.6(3) . . . . ? C8 C9 C10 C11 0.4(7) . . . . ? C9 C10 C11 C12 0.1(7) . . . . ? C10 C11 C12 C7 -0.1(6) . . . . ? C12 C7 C8 C9 0.9(7) . . . . ?