#------------------------------------------------------------------------------ #$Date: 2020-04-24 01:50:12 +0300 (Fri, 24 Apr 2020) $ #$Revision: 251115 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/03/7240387.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_7240387 loop_ _publ_author_name 'Yang, Chih-Tung' 'Yang, Xiang-Kai' 'Hu, Ji-Hong' 'Lee, Wei-Te' 'Chen, Tsun-Ren' 'Wang, Chih-Chieh' 'Chen, Jhy-Der' _publ_section_title ; One-dimensional chains based on linear tetranuclear copper(I) units: reversible structural transformation and luminescence change ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00294A _journal_year 2020 _chemical_formula_sum 'C22 H18 Cu4 I2 N8' _chemical_formula_weight 902.40 _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_creation_method SHELXL-2014/7 _audit_update_record ; 2020-02-03 deposited with the CCDC. 2020-04-23 downloaded from the CCDC. ; _cell_angle_alpha 87.6090(10) _cell_angle_beta 79.1280(10) _cell_angle_gamma 72.9380(10) _cell_formula_units_Z 1 _cell_length_a 7.02250(10) _cell_length_b 8.3565(2) _cell_length_c 11.6598(2) _cell_measurement_reflns_used 6780 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 28.26 _cell_measurement_theta_min 2.55 _cell_volume 642.31(2) _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-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _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 0.0287 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_Laue_measured_fraction_full 1.000 _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 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 11499 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.275 _diffrn_reflns_theta_min 1.779 _exptl_absorpt_coefficient_mu 5.698 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.5386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2008/1 (Bruker AXS, 2008)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.333 _exptl_crystal_description Plate _exptl_crystal_F_000 428 _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.869 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 163 _refine_ls_number_reflns 3196 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.061 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0279 _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^)+(0.0182P)^2^+0.5628P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.0564 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2577 _reflns_number_total 3196 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00294a2.cif _cod_data_source_block 2 _cod_depositor_comments ; The following automatic conversions were performed: data item '_exptl_absorpt_correction_type' value 'multi_scan' was changed to 'multi-scan' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas ; _cod_original_cell_volume 642.32(2) _cod_database_code 7240387 _shelx_shelxl_version_number 2014/7 _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 0.395 _shelx_estimated_absorpt_t_max 0.600 _shelx_res_file ; 12023_0m.res created by SHELXL-2014/7 TITL 12023_0m in P-1 CELL 0.71073 7.0225 8.3565 11.6598 87.609 79.128 72.938 ZERR 1.00 0.0001 0.0002 0.0002 0.001 0.001 0.001 LATT 1 SFAC C H N CU I UNIT 22 18 8 4 2 TEMP 23.000 SIZE 0.10 0.10 0.20 acta L.S. 8 BOND $H FMAP 2 PLAN 20 WGHT 0.018200 0.562800 FVAR 0.13710 CU1 4 0.272237 0.362125 0.231087 11.00000 0.03821 0.02590 = 0.03531 -0.00265 -0.01369 -0.00356 CU2 4 0.014579 0.440214 0.099979 11.00000 0.06340 0.02359 = 0.04237 -0.01004 -0.02931 0.00550 I 5 0.660108 0.340164 0.238385 11.00000 0.02851 0.03586 = 0.05590 -0.00194 -0.01089 -0.00844 N1 3 0.109179 0.574905 0.311121 11.00000 0.02996 0.02754 = 0.02796 -0.00343 -0.00724 -0.00989 N2 3 -0.047340 0.666403 0.152556 11.00000 0.02710 0.02376 = 0.02769 -0.00595 -0.00765 -0.00469 N3 3 -0.146796 0.770068 -0.020139 11.00000 0.02689 0.02084 = 0.03207 -0.00288 -0.00876 -0.00400 N4 3 -0.281834 0.865177 -0.184728 11.00000 0.02391 0.02416 = 0.03268 -0.00024 -0.00572 -0.00517 C1 1 0.139978 0.598324 0.419151 11.00000 0.04151 0.03395 = 0.03355 0.00318 -0.01335 -0.01135 AFIX 43 H1A 2 0.234985 0.513892 0.449947 11.00000 -1.20000 AFIX 0 C2 1 0.039683 0.738879 0.485910 11.00000 0.05762 0.04290 = 0.02779 -0.00588 -0.01095 -0.02020 AFIX 43 H2A 2 0.064310 0.749671 0.560406 11.00000 -1.20000 AFIX 0 C3 1 -0.099183 0.864104 0.439146 11.00000 0.04956 0.03435 = 0.03643 -0.01348 -0.00333 -0.00939 AFIX 43 H3B 2 -0.170529 0.961219 0.482468 11.00000 -1.20000 AFIX 0 C4 1 -0.132527 0.846013 0.328962 11.00000 0.03280 0.03062 = 0.03641 -0.01024 -0.00913 -0.00436 AFIX 43 H4B 2 -0.225591 0.930766 0.297087 11.00000 -1.20000 AFIX 0 C5 1 -0.025358 0.698967 0.264883 11.00000 0.02609 0.02615 = 0.03121 -0.00458 -0.00470 -0.00889 C6 1 -0.127720 0.792697 0.087636 11.00000 0.02346 0.02061 = 0.03395 -0.00677 -0.00217 -0.00408 AFIX 43 H6A 2 -0.172039 0.900636 0.119106 11.00000 -1.20000 AFIX 0 C7 1 -0.236072 0.906237 -0.084830 11.00000 0.02119 0.02311 = 0.03222 -0.00177 -0.00253 -0.00710 C8 1 -0.279431 1.075441 -0.053010 11.00000 0.03210 0.02449 = 0.03895 -0.00374 -0.00545 -0.00741 AFIX 43 H8A 2 -0.248684 1.103675 0.016194 11.00000 -1.20000 AFIX 0 C9 1 -0.366899 1.198303 -0.124086 11.00000 0.03376 0.02244 = 0.05399 0.00295 -0.00530 -0.00853 AFIX 43 H9A 2 -0.397786 1.310199 -0.102475 11.00000 -1.20000 AFIX 0 C10 1 -0.409294 1.157000 -0.227296 11.00000 0.03374 0.02943 = 0.04745 0.01185 -0.00940 -0.00720 AFIX 43 H10A 2 -0.465911 1.239055 -0.277478 11.00000 -1.20000 AFIX 0 C11 1 -0.364648 0.989075 -0.253659 11.00000 0.02912 0.03584 = 0.03573 0.00109 -0.00720 -0.00770 AFIX 43 H11A 2 -0.393493 0.959818 -0.323154 11.00000 -1.20000 AFIX 0 HKLF 4 REM 12023_0m in P-1 REM R1 = 0.0279 for 2577 Fo > 4sig(Fo) and 0.0405 for all 3196 data REM 163 parameters refined using 0 restraints END WGHT 0.0182 0.5629 REM Highest difference peak 0.869, deepest hole -0.589, 1-sigma level 0.100 Q1 1 0.6289 0.3667 0.1809 11.00000 0.05 0.87 Q2 1 0.5749 0.3505 0.3046 11.00000 0.05 0.81 Q3 1 0.6949 0.2840 0.2408 11.00000 0.05 0.46 Q4 1 0.1484 0.3729 0.2967 11.00000 0.05 0.40 Q5 1 0.7893 0.3329 0.1746 11.00000 0.05 0.39 Q6 1 -0.3319 1.1961 -0.2399 11.00000 0.05 0.37 Q7 1 0.1545 0.3497 0.2455 11.00000 0.05 0.36 Q8 1 0.2975 0.3525 0.3229 11.00000 0.05 0.36 Q9 1 -0.2342 0.7370 -0.0045 11.00000 0.05 0.35 Q10 1 -0.2059 0.7728 0.0403 11.00000 0.05 0.35 Q11 1 -0.0306 0.6905 0.1996 11.00000 0.05 0.34 Q12 1 0.3009 0.3626 0.1458 11.00000 0.05 0.34 Q13 1 0.4620 0.2719 0.3294 11.00000 0.05 0.33 Q14 1 -0.2021 0.8859 -0.1591 11.00000 0.05 0.32 Q15 1 -0.0531 0.4415 0.1847 11.00000 0.05 0.32 Q16 1 -0.1037 0.8329 0.3780 11.00000 0.05 0.32 Q17 1 0.0877 0.3776 0.1606 11.00000 0.05 0.32 Q18 1 -0.0838 0.3372 0.2044 11.00000 0.05 0.32 Q19 1 0.3394 0.3587 0.0809 11.00000 0.05 0.32 Q20 1 -0.0302 0.4449 -0.0104 11.00000 0.05 0.32 ; _shelx_res_checksum 15873 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 Cu1 Cu 0.27224(6) 0.36213(5) 0.23109(3) 0.03336(11) Uani 1 1 d . . . . . Cu2 Cu 0.01458(7) 0.44021(5) 0.09998(4) 0.04409(13) Uani 1 1 d . . . . . I I 0.66011(3) 0.34016(3) 0.23838(2) 0.03979(8) Uani 1 1 d . . . . . N1 N 0.1092(4) 0.5749(3) 0.3111(2) 0.0278(6) Uani 1 1 d . . . . . N2 N -0.0473(4) 0.6664(3) 0.1526(2) 0.0262(5) Uani 1 1 d . . . . . N3 N -0.1468(4) 0.7701(3) -0.0201(2) 0.0267(5) Uani 1 1 d . . . . . N4 N -0.2818(4) 0.8652(3) -0.1847(2) 0.0272(5) Uani 1 1 d . . . . . C1 C 0.1400(5) 0.5983(4) 0.4192(3) 0.0355(7) Uani 1 1 d . . . . . H1A H 0.2350 0.5139 0.4499 0.043 Uiso 1 1 calc R U . . . C2 C 0.0397(6) 0.7389(4) 0.4859(3) 0.0410(8) Uani 1 1 d . . . . . H2A H 0.0643 0.7497 0.5604 0.049 Uiso 1 1 calc R U . . . C3 C -0.0992(6) 0.8641(4) 0.4391(3) 0.0409(8) Uani 1 1 d . . . . . H3B H -0.1705 0.9612 0.4825 0.049 Uiso 1 1 calc R U . . . C4 C -0.1325(5) 0.8460(4) 0.3290(3) 0.0336(7) Uani 1 1 d . . . . . H4B H -0.2256 0.9308 0.2971 0.040 Uiso 1 1 calc R U . . . C5 C -0.0254(4) 0.6990(4) 0.2649(3) 0.0275(6) Uani 1 1 d . . . . . C6 C -0.1277(4) 0.7927(3) 0.0876(3) 0.0267(6) Uani 1 1 d . . . . . H6A H -0.1720 0.9006 0.1191 0.032 Uiso 1 1 calc R U . . . C7 C -0.2361(4) 0.9062(3) -0.0848(3) 0.0256(6) Uani 1 1 d . . . . . C8 C -0.2794(5) 1.0754(4) -0.0530(3) 0.0321(7) Uani 1 1 d . . . . . H8A H -0.2487 1.1037 0.0162 0.038 Uiso 1 1 calc R U . . . C9 C -0.3669(5) 1.1983(4) -0.1241(3) 0.0371(8) Uani 1 1 d . . . . . H9A H -0.3978 1.3102 -0.1025 0.045 Uiso 1 1 calc R U . . . C10 C -0.4093(5) 1.1570(4) -0.2273(3) 0.0374(8) Uani 1 1 d . . . . . H10A H -0.4659 1.2391 -0.2775 0.045 Uiso 1 1 calc R U . . . C11 C -0.3646(5) 0.9891(4) -0.2537(3) 0.0338(7) Uani 1 1 d . . . . . H11A H -0.3935 0.9598 -0.3232 0.041 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 Cu1 0.0382(2) 0.02590(19) 0.0353(2) -0.00265(16) -0.01369(18) -0.00356(16) Cu2 0.0634(3) 0.0236(2) 0.0424(3) -0.01004(17) -0.0293(2) 0.00550(19) I 0.02851(12) 0.03586(12) 0.05590(16) -0.00194(10) -0.01089(10) -0.00844(9) N1 0.0300(14) 0.0275(13) 0.0280(14) -0.0034(10) -0.0072(11) -0.0099(11) N2 0.0271(13) 0.0238(12) 0.0277(14) -0.0059(10) -0.0076(11) -0.0047(10) N3 0.0269(13) 0.0208(12) 0.0321(15) -0.0029(10) -0.0088(11) -0.0040(10) N4 0.0239(13) 0.0242(12) 0.0327(15) -0.0002(11) -0.0057(11) -0.0052(10) C1 0.0415(19) 0.0339(17) 0.0336(19) 0.0032(14) -0.0134(15) -0.0113(14) C2 0.058(2) 0.043(2) 0.0278(18) -0.0059(15) -0.0109(16) -0.0202(17) C3 0.050(2) 0.0344(18) 0.036(2) -0.0135(15) -0.0033(16) -0.0094(16) C4 0.0328(17) 0.0306(16) 0.0364(19) -0.0102(14) -0.0091(14) -0.0044(13) C5 0.0261(15) 0.0262(14) 0.0312(17) -0.0046(12) -0.0047(13) -0.0089(12) C6 0.0235(15) 0.0206(14) 0.0340(18) -0.0068(12) -0.0022(13) -0.0041(11) C7 0.0212(14) 0.0231(14) 0.0322(17) -0.0018(12) -0.0025(12) -0.0071(11) C8 0.0321(17) 0.0245(15) 0.0390(19) -0.0037(13) -0.0054(14) -0.0074(13) C9 0.0338(18) 0.0224(15) 0.054(2) 0.0029(15) -0.0053(16) -0.0085(13) C10 0.0337(18) 0.0294(16) 0.047(2) 0.0118(15) -0.0094(16) -0.0072(14) C11 0.0291(16) 0.0358(17) 0.0357(19) 0.0011(14) -0.0072(14) -0.0077(14) 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' 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_ _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 N4 147.17(10) . 2_565 ? N1 Cu1 Cu2 83.43(7) . . ? N4 Cu1 Cu2 81.21(7) 2_565 . ? N1 Cu1 I 105.55(7) . . ? N4 Cu1 I 104.31(7) 2_565 . ? Cu2 Cu1 I 142.43(2) . . ? N2 Cu2 N3 162.52(11) . 2_565 ? N2 Cu2 Cu1 87.71(7) . . ? N3 Cu2 Cu1 88.14(7) 2_565 . ? N2 Cu2 Cu2 86.23(8) . 2_565 ? N3 Cu2 Cu2 85.70(8) 2_565 2_565 ? Cu1 Cu2 Cu2 138.62(4) . 2_565 ? N2 Cu2 I 100.97(8) . 1_455 ? N3 Cu2 I 96.51(8) 2_565 1_455 ? Cu1 Cu2 I 103.155(19) . 1_455 ? Cu2 Cu2 I 118.19(3) 2_565 1_455 ? Cu1 I Cu2 140.318(15) . 1_655 ? C1 N1 C5 118.3(3) . . ? C1 N1 Cu1 116.6(2) . . ? C5 N1 Cu1 125.1(2) . . ? C6 N2 C5 119.2(2) . . ? C6 N2 Cu2 120.8(2) . . ? C5 N2 Cu2 119.74(19) . . ? C6 N3 C7 120.1(2) . . ? C6 N3 Cu2 121.00(19) . 2_565 ? C7 N3 Cu2 118.07(19) . 2_565 ? C11 N4 C7 118.5(3) . . ? C11 N4 Cu1 115.3(2) . 2_565 ? C7 N4 Cu1 125.6(2) . 2_565 ? N1 C1 C2 123.8(3) . . ? N1 C1 H1A 118.1 . . ? C2 C1 H1A 118.1 . . ? C1 C2 C3 117.7(3) . . ? C1 C2 H2A 121.1 . . ? C3 C2 H2A 121.1 . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3B 119.9 . . ? C2 C3 H3B 119.9 . . ? C3 C4 C5 119.4(3) . . ? C3 C4 H4B 120.3 . . ? C5 C4 H4B 120.3 . . ? N1 C5 N2 115.0(2) . . ? N1 C5 C4 120.5(3) . . ? N2 C5 C4 124.5(3) . . ? N3 C6 N2 121.9(2) . . ? N3 C6 H6A 119.0 . . ? N2 C6 H6A 119.0 . . ? N4 C7 N3 114.7(2) . . ? N4 C7 C8 120.1(3) . . ? N3 C7 C8 125.2(3) . . ? C9 C8 C7 119.8(3) . . ? C9 C8 H8A 120.1 . . ? C7 C8 H8A 120.1 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9A 119.9 . . ? C10 C9 H9A 119.9 . . ? C9 C10 C11 117.4(3) . . ? C9 C10 H10A 121.3 . . ? C11 C10 H10A 121.3 . . ? N4 C11 C10 123.8(3) . . ? N4 C11 H11A 118.1 . . ? C10 C11 H11A 118.1 . . ? 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 1.971(2) . ? Cu1 N4 1.975(2) 2_565 ? Cu1 Cu2 2.5108(6) . ? Cu1 I 2.6931(5) . ? Cu2 N2 1.911(2) . ? Cu2 N3 1.916(2) 2_565 ? Cu2 Cu2 2.5183(9) 2_565 ? Cu2 I 3.0155(6) 1_455 ? I Cu2 3.0155(6) 1_655 ? N1 C1 1.349(4) . ? N1 C5 1.352(4) . ? N2 C6 1.323(4) . ? N2 C5 1.394(4) . ? N3 C6 1.316(4) . ? N3 C7 1.395(4) . ? N3 Cu2 1.916(2) 2_565 ? N4 C11 1.345(4) . ? N4 C7 1.348(4) . ? N4 Cu1 1.975(2) 2_565 ? C1 C2 1.366(5) . ? C1 H1A 0.9300 . ? C2 C3 1.377(5) . ? C2 H2A 0.9300 . ? C3 C4 1.371(4) . ? C3 H3B 0.9300 . ? C4 C5 1.399(4) . ? C4 H4B 0.9300 . ? C6 H6A 0.9300 . ? C7 C8 1.406(4) . ? C8 C9 1.367(5) . ? C8 H8A 0.9300 . ? C9 C10 1.373(5) . ? C9 H9A 0.9300 . ? C10 C11 1.380(4) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ?