#------------------------------------------------------------------------------ #$Date: 2023-11-05 01:56:22 +0200 (Sun, 05 Nov 2023) $ #$Revision: 287262 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/76/7247668.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_7247668 loop_ _publ_author_name 'Lu, Kuang-Lieh' 'Sie, Shu-Ling' 'Kamal, Surabhi' 'Zong-Zhan, Lu' 'Wei, Ling-Fang' 'Luo, Tzuoo-Tsair' 'Liu, Yen-Hsiang' 'Chang, Chao-Wan' 'Chi, Kai-Ming' _publ_section_title ; Fine-tuning synthesis of a novel CuI/CuII mixed-valence coordination polymer ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE01001E _journal_year 2023 _chemical_formula_moiety 'C6 H4 Cl Cu2 N5' _chemical_formula_sum 'C6 H4 Cl Cu2 N5' _chemical_formula_weight 308.67 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difma; _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-10-21 deposited with the CCDC. 2023-10-27 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 102.953(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 19.689(5) _cell_length_b 3.6236(9) _cell_length_c 11.631(3) _cell_measurement_reflns_used 2199 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 24.59 _cell_measurement_theta_min 2.05 _cell_volume 808.7(4) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _diffrn_ambient_temperature 200(2) _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Bruker APEX2' _diffrn_measurement_method 'phi & omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0173 _diffrn_reflns_av_unetI/netI 0.0335 _diffrn_reflns_Laue_measured_fraction_full 0.978 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 1437 _diffrn_reflns_point_group_measured_fraction_full 0.838 _diffrn_reflns_point_group_measured_fraction_max 0.838 _diffrn_reflns_theta_full 25.069 _diffrn_reflns_theta_max 25.069 _diffrn_reflns_theta_min 2.123 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 5.543 _exptl_absorpt_correction_T_max 0.8087 _exptl_absorpt_correction_T_min 0.3752 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.535 _exptl_crystal_description prism _exptl_crystal_F_000 600 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.040 _refine_diff_density_max 0.645 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.312 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.38(4) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 128 _refine_ls_number_reflns 1200 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.068 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0240 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0805P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.1018 _reflns_Friedel_coverage 0.712 _reflns_Friedel_fraction_full 0.699 _reflns_Friedel_fraction_max 0.698 _reflns_number_gt 1156 _reflns_number_total 1200 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01001e2.cif _cod_data_source_block shelx _cod_original_cell_volume 808.7(3) _cod_original_sg_symbol_H-M 'C c' _cod_database_code 7247668 _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 0.375 _shelx_estimated_absorpt_t_max 0.809 _shelx_res_file ; TITL a11935_0m in Cc shelx.res created by SHELXL-2018/3 at 10:22:13 on 19-Oct-2023 CELL 0.71073 19.6891 3.6236 11.6313 90.000 102.953 90.000 ZERR 4.00 0.0047 0.0009 0.0028 0.000 0.003 0.000 LATT -7 SYMM X, - Y, 1/2 + Z SFAC CU CL C H N UNIT 8 4 24 16 20 MERG 2 TWIN FMAP 2 PLAN 20 SIZE 0.040 0.100 0.220 ACTA BOND $H L.S. 80 TEMP -73.00 WGHT 0.080500 BASF 0.38015 FVAR 0.44755 CU1 1 -0.143583 -0.155305 0.647645 11.00000 0.00959 0.03562 = 0.01896 -0.00108 0.00234 -0.00392 CU2 1 -0.049997 -0.989012 0.466080 11.00000 0.01882 0.03244 = 0.00716 -0.00107 0.00454 0.00077 CL1 2 -0.134766 -0.498620 0.466734 11.00000 0.01619 0.01718 = 0.01474 -0.00215 0.00131 0.00123 C1 3 0.056674 0.140818 0.714196 11.00000 0.01788 0.01421 = 0.00602 -0.00344 0.00111 -0.00061 C2 3 0.124392 0.221550 0.687094 11.00000 0.00754 0.01675 = 0.01157 0.00685 0.00207 -0.00280 C3 3 0.175328 0.385273 0.773514 11.00000 0.01152 0.01821 = 0.00891 -0.00016 0.00382 0.00285 AFIX 43 H3 4 0.164467 0.463987 0.845212 11.00000 -1.20000 AFIX 0 C4 3 0.241099 0.434291 0.756302 11.00000 0.01091 0.02100 = 0.01690 -0.00193 -0.00123 -0.00067 AFIX 43 H4 4 0.275057 0.550338 0.816363 11.00000 -1.20000 AFIX 0 C5 3 0.209401 0.173135 0.571456 11.00000 0.01538 0.01675 = 0.00894 0.00261 0.00258 -0.00177 AFIX 43 H5 4 0.221407 0.099052 0.500210 11.00000 -1.20000 AFIX 0 C6 3 0.141837 0.121152 0.581822 11.00000 0.01555 0.02000 = 0.00492 0.00121 0.00164 0.00237 AFIX 43 H6 4 0.107895 0.019203 0.518676 11.00000 -1.20000 AFIX 0 N1 5 -0.047586 -0.030270 0.709595 11.00000 0.01329 0.02148 = 0.01048 -0.00069 0.00292 -0.00251 N2 5 -0.002736 0.031559 0.640294 11.00000 0.01353 0.01956 = 0.00461 0.00119 0.00136 -0.00079 N3 5 0.049463 0.149417 0.826880 11.00000 0.01022 0.02374 = 0.01097 -0.00045 0.00216 -0.00227 N4 5 -0.015938 0.040210 0.820759 11.00000 0.01039 0.02481 = 0.00878 0.00214 -0.00029 0.00183 N5 5 0.259413 0.323086 0.656636 11.00000 0.01143 0.02104 = 0.01364 0.00287 0.00450 -0.00026 HKLF 4 REM a11935_0m in Cc REM wR2 = 0.1018, GooF = S = 1.069, Restrained GooF = 1.068 for all data REM R1 = 0.0240 for 1156 Fo > 4sig(Fo) and 0.0305 for all 1200 data REM 128 parameters refined using 2 restraints END WGHT 0.0610 0.0000 REM Highest difference peak 0.645, deepest hole -0.894, 1-sigma level 0.312 Q1 1 0.1543 0.2011 0.7217 11.00000 0.05 0.63 Q2 1 0.1891 -0.0280 0.4395 11.00000 0.05 0.60 Q3 1 0.2161 0.1910 0.5473 11.00000 0.05 0.60 Q4 1 0.2065 0.4442 0.7424 11.00000 0.05 0.60 Q5 1 0.1946 0.2009 0.8159 11.00000 0.05 0.58 Q6 1 0.1892 0.4875 0.7234 11.00000 0.05 0.58 Q7 1 0.1339 0.1815 0.6400 11.00000 0.05 0.58 Q8 1 0.1624 0.4860 0.9333 11.00000 0.05 0.58 Q9 1 0.1195 0.3570 0.6614 11.00000 0.05 0.57 Q10 1 0.1630 -0.1367 0.6781 11.00000 0.05 0.57 Q11 1 0.1899 0.8154 0.8554 11.00000 0.05 0.57 Q12 1 0.1632 0.0793 0.3876 11.00000 0.05 0.56 Q13 1 0.1616 0.4624 0.8032 11.00000 0.05 0.56 Q14 1 0.1275 0.2372 0.5485 11.00000 0.05 0.56 Q15 1 0.1690 0.5209 0.5210 11.00000 0.05 0.56 Q16 1 0.1307 -0.1232 0.6370 11.00000 0.05 0.55 Q17 1 0.0993 0.1863 0.6946 11.00000 0.05 0.55 Q18 1 0.1764 0.2095 0.6345 11.00000 0.05 0.55 Q19 1 0.1832 -0.1172 0.4977 11.00000 0.05 0.53 Q20 1 0.1888 0.5004 0.9797 11.00000 0.05 0.53 ; _shelx_res_checksum 65718 loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -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 Cu1 Cu -0.14358(8) -0.1553(4) 0.64765(14) 0.0215(4) Uani 1 1 d . . . . . Cu2 Cu -0.05000(6) -0.9890(3) 0.46608(9) 0.0192(4) Uani 1 1 d . . . . . Cl1 Cl -0.13477(13) -0.4986(6) 0.4667(2) 0.0164(6) Uani 1 1 d . . . . . C1 C 0.0567(5) 0.141(3) 0.7142(8) 0.013(2) Uani 1 1 d . . . . . C2 C 0.1244(5) 0.222(3) 0.6871(9) 0.0120(18) Uani 1 1 d . . . . . C3 C 0.1753(5) 0.385(3) 0.7735(9) 0.0126(19) Uani 1 1 d . . . . . H3 H 0.164467 0.463987 0.845212 0.015 Uiso 1 1 calc R U . . . C4 C 0.2411(5) 0.434(3) 0.7563(10) 0.017(2) Uani 1 1 d . . . . . H4 H 0.275057 0.550338 0.816363 0.020 Uiso 1 1 calc R U . . . C5 C 0.2094(5) 0.173(2) 0.5715(9) 0.0137(19) Uani 1 1 d . . . . . H5 H 0.221407 0.099052 0.500210 0.016 Uiso 1 1 calc R U . . . C6 C 0.1418(5) 0.121(3) 0.5818(9) 0.0136(19) Uani 1 1 d . . . . . H6 H 0.107895 0.019203 0.518676 0.016 Uiso 1 1 calc R U . . . N1 N -0.0476(5) -0.030(2) 0.7096(10) 0.0150(17) Uani 1 1 d . . . . . N2 N -0.0027(4) 0.032(2) 0.6403(8) 0.0127(17) Uani 1 1 d . . . . . N3 N 0.0495(4) 0.149(2) 0.8269(7) 0.0150(17) Uani 1 1 d . . . . . N4 N -0.0159(4) 0.040(2) 0.8208(8) 0.0150(19) Uani 1 1 d . . . . . N5 N 0.2594(4) 0.323(2) 0.6566(8) 0.0151(17) Uani 1 1 d . . . . . 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 Cu1 0.0096(6) 0.0356(7) 0.0190(6) -0.0011(7) 0.0023(4) -0.0039(5) Cu2 0.0188(7) 0.0324(7) 0.0072(6) -0.0011(5) 0.0045(5) 0.0008(5) Cl1 0.0162(12) 0.0172(10) 0.0147(15) -0.0021(9) 0.0013(10) 0.0012(8) C1 0.018(5) 0.014(4) 0.006(4) -0.003(4) 0.001(4) -0.001(3) C2 0.008(4) 0.017(4) 0.012(4) 0.007(4) 0.002(4) -0.003(3) C3 0.012(5) 0.018(4) 0.009(5) 0.000(4) 0.004(4) 0.003(4) C4 0.011(5) 0.021(4) 0.017(6) -0.002(4) -0.001(4) -0.001(4) C5 0.015(5) 0.017(4) 0.009(5) 0.003(4) 0.003(4) -0.002(4) C6 0.016(5) 0.020(4) 0.005(4) 0.001(4) 0.002(4) 0.002(4) N1 0.013(4) 0.021(4) 0.010(4) -0.001(4) 0.003(3) -0.003(3) N2 0.014(4) 0.020(4) 0.005(4) 0.001(3) 0.001(3) -0.001(3) N3 0.010(4) 0.024(4) 0.011(4) 0.000(4) 0.002(3) -0.002(3) N4 0.010(4) 0.025(4) 0.009(5) 0.002(3) 0.000(3) 0.002(3) N5 0.011(4) 0.021(4) 0.014(4) 0.003(3) 0.005(4) 0.000(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Cu Cu 0.3201 1.2651 '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' 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' 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 N1 Cu1 N5 152.7(4) . 3_445 ? N1 Cu1 Cl1 100.7(3) . . ? N5 Cu1 Cl1 106.4(3) 3_445 . ? N4 Cu2 N2 133.9(3) 2_544 1_545 ? N4 Cu2 Cl1 116.0(3) 2_544 . ? N2 Cu2 Cl1 97.5(2) 1_545 . ? N4 Cu2 Cl1 106.9(3) 2_544 1_545 ? N2 Cu2 Cl1 100.5(2) 1_545 1_545 ? Cl1 Cu2 Cl1 94.63(9) . 1_545 ? Cu2 Cl1 Cu1 123.05(11) . . ? Cu2 Cl1 Cu2 94.63(9) . 1_565 ? Cu1 Cl1 Cu2 78.78(8) . 1_565 ? N2 C1 N3 111.2(9) . . ? N2 C1 C2 128.5(9) . . ? N3 C1 C2 120.2(8) . . ? C3 C2 C6 118.0(9) . . ? C3 C2 C1 118.4(8) . . ? C6 C2 C1 123.5(9) . . ? C4 C3 C2 120.4(9) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? N5 C4 C3 122.1(9) . . ? N5 C4 H4 118.9 . . ? C3 C4 H4 118.9 . . ? N5 C5 C6 123.6(9) . . ? N5 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C5 C6 C2 118.4(9) . . ? C5 C6 H6 120.8 . . ? C2 C6 H6 120.8 . . ? N4 N1 N2 108.9(8) . . ? N4 N1 Cu1 128.2(8) . . ? N2 N1 Cu1 122.6(8) . . ? N1 N2 C1 105.1(9) . . ? N1 N2 Cu2 112.2(6) . 1_565 ? C1 N2 Cu2 141.7(7) . 1_565 ? N4 N3 C1 104.6(8) . . ? N1 N4 N3 110.2(9) . . ? N1 N4 Cu2 130.1(7) . 2_545 ? N3 N4 Cu2 119.6(6) . 2_545 ? C5 N5 C4 117.4(9) . . ? C5 N5 Cu1 123.0(7) . 3 ? C4 N5 Cu1 119.4(7) . 3 ? 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 Cu1 N1 1.920(10) . ? Cu1 N5 1.938(8) 3_445 ? Cu1 Cl1 2.484(3) . ? Cu2 N4 1.962(9) 2_544 ? Cu2 N2 2.033(9) 1_545 ? Cu2 Cl1 2.439(2) . ? Cu2 Cl1 2.490(2) 1_545 ? C1 N2 1.347(13) . ? C1 N3 1.350(13) . ? C1 C2 1.467(13) . ? C2 C3 1.384(14) . ? C2 C6 1.392(14) . ? C3 C4 1.366(15) . ? C3 H3 0.9500 . ? C4 N5 1.350(15) . ? C4 H4 0.9500 . ? C5 N5 1.345(13) . ? C5 C6 1.375(15) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? N1 N4 1.328(14) . ? N1 N2 1.341(14) . ? N3 N4 1.334(12) . ?