#------------------------------------------------------------------------------ #$Date: 2026-06-05 20:09:37 +0100 (Fri, 05 Jun 2026) $ #$Revision: 306435 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720988.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_7720988 loop_ _publ_author_name 'Khlifi, Houyem' 'Wannassi, Jassem' 'Mhadhbi, Noureddine' 'Wahbi, Hajir' 'Erwann, Jeanneau' 'Ben Hamadi, Naoufel' 'Guesmi, Ahlem' 'Khezami, Lotfi' 'Barhoumi, Houcine' 'Naïli, Houcine' _publ_section_title ; Structural, optical, and electrochemical properties of a new 1D copper(II) halometalate for highly sensitive dopamine detection. ; _journal_issue 21 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 8243 _journal_page_last 8257 _journal_paper_doi 10.1039/d6dt00622a _journal_volume 55 _journal_year 2026 _chemical_formula_moiety 'C6 H6 Cl2 Cu I2 N4' _chemical_formula_sum 'C6 H6 Cl2 Cu I2 N4' _chemical_formula_weight 522.39 _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 dual _audit_creation_date 2025-01-25 _audit_creation_method ; Olex2 1.5-ac6-020 (compiled 2024.02.14 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6966) ; _audit_update_record ; 2026-03-01 deposited with the CCDC. 2026-05-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.599(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 4.01140(10) _cell_length_b 15.0996(6) _cell_length_c 10.0000(3) _cell_measurement_reflns_used 7693 _cell_measurement_temperature 100.0(2) _cell_measurement_theta_max 30.0050 _cell_measurement_theta_min 3.3690 _cell_volume 604.51(3) _computing_cell_refinement 'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro system (CCD 43.143a 64-bit (release 25-10-2024))' _computing_data_reduction 'CrysAlisPro 1.171.43.124a (Rigaku OD, 2024)' _computing_molecular_graphics 'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-ac6-020 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.0(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 100' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.876 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -71.00 -40.00 0.50 0.55 -- 6.58 -19.00-180.00 62 2 \w -71.00 -40.00 0.50 0.55 -- 6.58 -19.00 -90.00 62 3 \w -71.00 -40.00 0.50 0.55 -- 6.58 -19.00 -60.00 62 4 \w -71.00 -40.00 0.50 0.55 -- 6.58 -19.00 0.00 62 5 \w -71.00 -40.00 0.50 0.55 -- 6.58 -19.00 60.00 62 6 \w -71.00 -40.00 0.50 0.55 -- 6.58 -19.00 90.00 62 7 \w -71.00 -40.00 0.50 0.55 -- 6.58 -19.00 150.00 62 8 \w -83.00 -40.00 0.50 0.55 -- -5.49 -19.00 30.00 86 9 \w -59.00 6.00 0.50 0.55 -- -5.49 -57.00 150.00 130 10 \w -16.00 38.00 0.50 0.55 -- -5.49 57.00 0.00 108 11 \w -59.00 -4.00 0.50 0.55 -- -5.49 -57.00-150.00 110 12 \w -83.00 -40.00 0.50 0.55 -- -5.49 -19.00 -90.00 86 13 \w -59.00 6.00 0.50 0.55 -- -5.49 -57.00 -30.00 130 14 \w -7.00 40.00 0.50 0.55 -- 6.58 -99.00 30.00 94 15 \w -7.00 40.00 0.50 0.55 -- 6.58 -99.00 90.00 94 16 \w 8.00 54.00 0.50 0.55 -- 6.58-123.00 -34.00 92 17 \w -7.00 40.00 0.50 0.55 -- 6.58 -99.00-150.00 94 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix-Arc 100' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0124057000 _diffrn_orient_matrix_UB_12 0.0466101000 _diffrn_orient_matrix_UB_13 -0.0071994000 _diffrn_orient_matrix_UB_21 0.0349031000 _diffrn_orient_matrix_UB_22 0.0042154000 _diffrn_orient_matrix_UB_23 0.0701076000 _diffrn_orient_matrix_UB_31 0.1732465000 _diffrn_orient_matrix_UB_32 -0.0041852000 _diffrn_orient_matrix_UB_33 -0.0090555000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.876 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 1615 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.876 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.454 _diffrn_reflns_theta_min 3.384 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 7.327 _exptl_absorpt_correction_T_max 0.760 _exptl_absorpt_correction_T_min 0.380 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.124a (Rigaku Oxford Diffraction, 2024) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.870 _exptl_crystal_description plate _exptl_crystal_F_000 478 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.975 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.199 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 71 _refine_ls_number_reflns 1615 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0352 _refine_ls_R_factor_gt 0.0295 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0188P)^2^+2.5273P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.0591 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1446 _reflns_number_total 1615 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt00622a2.cif _cod_data_source_block 4icucl_autored _cod_depositor_comments 'Adding full bibliography for 7720988.cif.' _cod_database_code 7720988 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C6 H6 Cl2 Cu1 I2 N4' _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_max 0.711 _shelx_estimated_absorpt_t_min 0.272 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.8252(17) 0.1748(17) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 3.a Aromatic/amide H refined with riding coordinates: N2(H2), C1(H1), C3(H3) ; _shelx_res_file ; TITL 4icucl_autored_a.res in P2(1)/c 4icucl_autored.res created by SHELXL-2018/3 at 11:50:42 on 25-Jan-2025 REM Old TITL 4icucl_autored_a.res in P2(1) REM SHELXT solution in P2(1)/c: R1 0.134, Rweak 0.021, Alpha 0.028 REM 3.928 for 54 systematic absences, Orientation as input REM Formula found by SHELXT: C10 Cl2 Cu3 CELL 0.71073 4.0114 15.0996 10 90 93.599 90 ZERR 2 0.0001 0.0006 0.0003 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N Cl Cu I UNIT 12 12 8 4 2 4 L.S. 10 PLAN 8 SIZE 0.05 0.11 0.24 TEMP -173 CONF BOND list 4 fmap 2 53 MORE -1 BOND $H ACTA OMIT 0 4 2 REM REM REM WGHT 0.018800 2.527300 BASF 0.17480 FVAR 1.07717 I1 6 0.793027 0.357218 1.068157 11.00000 0.01259 0.01721 = 0.01142 0.00268 -0.00086 -0.00122 CU1 5 0.500000 0.500000 0.500000 10.50000 0.01491 0.00959 = 0.00996 0.00104 -0.00169 -0.00239 CL1 4 0.098574 0.403825 0.402119 11.00000 0.01538 0.01168 = 0.01266 0.00032 -0.00166 -0.00118 N1 3 0.518418 0.427007 0.665865 11.00000 0.01395 0.01155 = 0.01244 0.00055 -0.00019 0.00005 N2 3 0.360579 0.347837 0.674193 11.00000 0.01945 0.00965 = 0.01271 0.00034 -0.00049 -0.00472 AFIX 43 H2 2 0.238432 0.323539 0.607819 11.00000 -1.20000 AFIX 0 C2 1 0.614100 0.368676 0.870629 11.00000 0.01060 0.01479 = 0.01229 0.00198 0.00048 -0.00110 C1 1 0.675831 0.439949 0.785460 11.00000 0.01467 0.01077 = 0.01585 0.00012 0.00015 -0.00346 AFIX 43 H1 2 0.810020 0.489985 0.809594 11.00000 -1.20000 AFIX 0 C3 1 0.413036 0.311373 0.795071 11.00000 0.01565 0.01378 = 0.01489 0.00267 0.00291 -0.00148 AFIX 43 H3 2 0.327808 0.256290 0.823634 11.00000 -1.20000 AFIX 0 HKLF 5 REM 4icucl_autored_a.res in P2(1)/c REM wR2 = 0.0591, GooF = S = 1.074, Restrained GooF = 1.074 for all data REM R1 = 0.0295 for 1446 Fo > 4sig(Fo) and 0.0352 for all 1615 data REM 71 parameters refined using 0 restraints END WGHT 0.0187 2.5329 REM Highest difference peak 0.975, deepest hole -0.853, 1-sigma level 0.199 Q1 1 0.7922 0.3606 0.9676 11.00000 0.05 0.88 Q2 1 0.8829 0.4024 0.8513 11.00000 0.05 0.86 Q3 1 0.4850 0.3588 1.0475 11.00000 0.05 0.81 Q4 1 1.0784 0.4413 0.8231 11.00000 0.05 0.80 Q5 1 0.5993 0.3406 0.8021 11.00000 0.05 0.80 Q6 1 0.5359 0.4730 0.6930 11.00000 0.05 0.80 Q7 1 0.8743 0.4807 0.7977 11.00000 0.05 0.75 Q8 1 1.1414 0.3556 1.0590 11.00000 0.05 0.74 ; _shelx_res_checksum 33273 _olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems' _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a MITIGEN holder in perfluoroether oil' _olex2_submission_original_sample_id 4ICuCl _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.227 _oxdiff_exptl_absorpt_empirical_full_min 0.723 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 0.79303(7) 0.35722(2) 1.06816(2) 0.01381(9) Uani 1 1 d . . . . . Cu1 Cu 0.500000 0.500000 0.500000 0.01159(16) Uani 1 2 d S . P . . Cl1 Cl 0.0986(3) 0.40382(6) 0.40212(9) 0.0133(2) Uani 1 1 d . . . . . N1 N 0.5184(9) 0.4270(2) 0.6659(3) 0.0127(7) Uani 1 1 d . . . . . N2 N 0.3606(9) 0.3478(2) 0.6742(3) 0.0140(7) Uani 1 1 d . . . . . H2 H 0.238432 0.323539 0.607819 0.017 Uiso 1 1 calc R U . . . C2 C 0.6141(10) 0.3687(3) 0.8706(4) 0.0126(8) Uani 1 1 d . . . . . C1 C 0.6758(11) 0.4399(3) 0.7855(4) 0.0138(8) Uani 1 1 d . . . . . H1 H 0.810020 0.489985 0.809594 0.017 Uiso 1 1 calc R U . . . C3 C 0.4130(11) 0.3114(3) 0.7951(4) 0.0147(8) Uani 1 1 d . . . . . H3 H 0.327808 0.256290 0.823634 0.018 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 0.01259(15) 0.01721(14) 0.01142(13) 0.00268(10) -0.00086(9) -0.00122(10) Cu1 0.0149(4) 0.0096(3) 0.0100(3) 0.0010(2) -0.0017(3) -0.0024(3) Cl1 0.0154(5) 0.0117(4) 0.0127(4) 0.0003(3) -0.0017(4) -0.0012(4) N1 0.0139(18) 0.0116(16) 0.0124(16) 0.0006(13) -0.0002(13) 0.0001(13) N2 0.0194(19) 0.0096(16) 0.0127(16) 0.0003(13) -0.0005(14) -0.0047(14) C2 0.011(2) 0.015(2) 0.0123(18) 0.0020(15) 0.0005(15) -0.0011(15) C1 0.015(2) 0.0108(19) 0.0159(19) 0.0001(15) 0.0001(16) -0.0035(16) C3 0.016(2) 0.014(2) 0.0149(19) 0.0027(15) 0.0029(16) -0.0015(16) 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' N N 0.0061 0.0033 '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' Cu Cu 0.3201 1.2651 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 2 0.0372 0 -1 -2 0.0761 2 0 1 0.1054 -2 1 1 0.0960 0 20 -5 0.0180 0 -20 5 0.0249 0 -19 -7 0.0495 0 -14 11 0.0240 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 Cu1 Cl1 180.0 3_666 . ? N1 Cu1 Cl1 90.37(10) . 3_666 ? N1 Cu1 Cl1 90.37(10) 3_666 . ? N1 Cu1 Cl1 89.63(10) 3_666 3_666 ? N1 Cu1 Cl1 89.63(10) . . ? N1 Cu1 N1 180.0 . 3_666 ? N2 N1 Cu1 123.1(3) . . ? C1 N1 Cu1 131.2(3) . . ? C1 N1 N2 105.7(3) . . ? N1 N2 H2 124.1 . . ? C3 N2 N1 111.8(3) . . ? C3 N2 H2 124.1 . . ? C1 C2 I1 125.5(3) . . ? C3 C2 I1 129.0(3) . . ? C3 C2 C1 105.6(4) . . ? N1 C1 C2 109.9(4) . . ? N1 C1 H1 125.0 . . ? C2 C1 H1 125.0 . . ? N2 C3 C2 107.0(4) . . ? N2 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? 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 C2 2.066(4) . ? Cu1 Cl1 2.3371(10) . ? Cu1 Cl1 2.3371(10) 3_666 ? Cu1 N1 1.989(3) . ? Cu1 N1 1.989(3) 3_666 ? N1 N2 1.358(5) . ? N1 C1 1.331(5) . ? N2 H2 0.8800 . ? N2 C3 1.333(5) . ? C2 C1 1.404(5) . ? C2 C3 1.376(6) . ? C1 H1 0.9500 . ? C3 H3 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 I1 C2 C1 N1 -178.9(3) . . . . ? I1 C2 C3 N2 179.1(3) . . . . ? Cu1 N1 N2 C3 179.4(3) . . . . ? Cu1 N1 C1 C2 -179.6(3) . . . . ? N1 N2 C3 C2 0.1(5) . . . . ? N2 N1 C1 C2 -0.6(5) . . . . ? C1 N1 N2 C3 0.3(5) . . . . ? C1 C2 C3 N2 -0.4(5) . . . . ? C3 C2 C1 N1 0.6(5) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.8252(17) 2 0.1748(17) loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0005 1.0064 2.0007 0.0325 0.1445 -0.0222 -0.0005 -1.0064 -2.0007 -0.0325 -0.1445 0.0222 2.0009 -0.0022 0.9968 0.0175 0.1397 0.3376 -2.0005 1.0086 1.0039 0.0150 0.0048 -0.3599 0.1921 20.1040 -4.6148 0.9727 -0.2321 -0.0091 0.0007 -20.1503 4.5204 -0.9717 0.2320 0.0435 0.1417 -18.5385 -6.9334 -0.8124 -0.5593 0.1649 0.1613 -13.9936 10.5648 -0.7263 0.6873 -0.0092