#------------------------------------------------------------------------------ #$Date: 2018-01-16 04:34:49 +0200 (Tue, 16 Jan 2018) $ #$Revision: 205237 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229983.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_7229983 loop_ _publ_author_name 'Dankhoff, Katja' 'Weber, Birgit' _publ_section_title ; Novel Cu(II) complexes with NNO-Schiff base-like ligands -- structures and magnetic properties ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C7CE02007D _journal_year 2018 _chemical_formula_moiety 'C26 H30 Cu2 I2 N4 O6' _chemical_formula_sum 'C13 H15 Cu I N2 O3' _chemical_formula_weight 437.71 _chemical_name_common '[CuL30aI]' _chemical_name_systematic ; ? ; _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_date 2017-07-27 _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-01-11 deposited with the CCDC. 2018-01-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.391(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.8179(3) _cell_length_b 14.6683(6) _cell_length_c 13.0905(4) _cell_measurement_reflns_used 8349 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 27.62 _cell_measurement_theta_min 2.08 _cell_volume 1499.85(10) _computing_cell_refinement X-AREA-STOE _computing_data_collection X-AREA-STOE _computing_data_reduction X-AREA-STOE _computing_molecular_graphics ORTEP-III _computing_publication_material PLATON _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution SIR97 _diffrn_ambient_temperature 133(2) _diffrn_detector_area_resol_mean 9 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measurement_device_type STOE-STADIVARI _diffrn_measurement_method omega-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0355 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 0.927 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 9126 _diffrn_reflns_point_group_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 0.927 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.465 _diffrn_reflns_theta_min 2.086 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 3.522 _exptl_absorpt_correction_type none _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.938 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 852 _exptl_crystal_size_max 0.101 _exptl_crystal_size_mid 0.077 _exptl_crystal_size_min 0.063 _refine_diff_density_max 0.502 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.091 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 181 _refine_ls_number_reflns 3516 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.936 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0205 _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^)+(0.0209P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0458 _refine_ls_wR_factor_ref 0.0468 _reflns_number_gt 2940 _reflns_number_total 3516 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02007d2.cif _cod_data_source_block cl099 _cod_database_code 7229983 _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_res_file ; shelx.res created by SHELXL-2014/7 TITL SIR97 run in space group P 21/c CELL 0.71073 7.8179 14.6683 13.0905 90.000 92.391 90.000 ZERR 4.00 0.0003 0.0006 0.0004 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CU I UNIT 52 60 8 12 4 4 MERG 2 FMAP 2 PLAN 10 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -140.00 WGHT 0.020900 FVAR 0.25756 C1 1 0.647567 0.364021 0.330482 11.00000 0.02726 0.02758 = 0.01893 -0.00141 -0.00809 0.00336 AFIX 43 H1 2 0.588142 0.414845 0.301324 11.00000 -1.20000 AFIX 0 C2 1 0.636467 0.281413 0.280880 11.00000 0.02654 0.03342 = 0.02188 -0.00560 -0.00598 0.00103 AFIX 43 H2 2 0.572544 0.275886 0.217859 11.00000 -1.20000 AFIX 0 C3 1 0.719625 0.206303 0.323896 11.00000 0.02412 0.02606 = 0.02577 -0.01091 0.00031 0.00024 AFIX 43 H3 2 0.710351 0.148140 0.292226 11.00000 -1.20000 AFIX 0 C4 1 0.816321 0.217817 0.413838 11.00000 0.02260 0.02071 = 0.02466 -0.00374 -0.00203 0.00109 AFIX 43 H4 2 0.876624 0.167875 0.444325 11.00000 -1.20000 AFIX 0 C5 1 0.823944 0.303526 0.458937 11.00000 0.01654 0.01985 = 0.01682 -0.00148 -0.00003 -0.00108 C6 1 0.927800 0.319235 0.556316 11.00000 0.02958 0.01642 = 0.02057 -0.00094 -0.00948 0.00190 AFIX 23 H6A 2 0.894697 0.274467 0.608528 11.00000 -1.20000 H6B 2 1.050836 0.310654 0.543979 11.00000 -1.20000 AFIX 0 C7 1 0.971134 0.433463 0.681505 11.00000 0.01634 0.01873 = 0.01739 0.00200 -0.00313 -0.00315 AFIX 43 H7 2 1.040161 0.388280 0.714956 11.00000 -1.20000 AFIX 0 C8 1 0.956584 0.518492 0.732392 11.00000 0.02125 0.01938 = 0.01467 -0.00093 -0.00128 -0.00368 C9 1 0.857985 0.590566 0.689271 11.00000 0.02206 0.01815 = 0.01999 -0.00096 0.00060 -0.00433 C10 1 0.840183 0.681532 0.740883 11.00000 0.03486 0.02172 = 0.02834 -0.00586 -0.00671 0.00208 AFIX 133 H10A 2 0.760443 0.719854 0.700208 11.00000 -1.50000 H10B 2 0.952272 0.711412 0.746868 11.00000 -1.50000 H10C 2 0.796239 0.672578 0.809188 11.00000 -1.50000 AFIX 0 C11 1 1.055987 0.531059 0.828737 11.00000 0.02707 0.02315 = 0.01831 0.00089 -0.00211 -0.00533 C12 1 1.248917 0.461071 0.949699 11.00000 0.03827 0.03457 = 0.02145 0.00072 -0.01552 -0.00314 AFIX 23 H12A 2 1.185746 0.480412 1.010004 11.00000 -1.20000 H12B 2 1.338282 0.507038 0.936992 11.00000 -1.20000 AFIX 0 C13 1 1.328318 0.369893 0.968135 11.00000 0.03600 0.04475 = 0.03283 0.00174 -0.01504 0.00383 AFIX 133 H13A 2 1.239851 0.326179 0.986393 11.00000 -1.50000 H13B 2 1.415043 0.374246 1.024174 11.00000 -1.50000 H13C 2 1.382287 0.349281 0.905966 11.00000 -1.50000 AFIX 0 N1 3 0.739615 0.375530 0.418909 11.00000 0.02007 0.01966 = 0.01681 -0.00003 -0.00351 -0.00080 N2 3 0.899006 0.411427 0.593415 11.00000 0.01914 0.01641 = 0.01943 0.00008 -0.00396 -0.00168 O1 4 0.776311 0.585216 0.603345 11.00000 0.03290 0.01945 = 0.02218 -0.00302 -0.01030 0.00203 O2 4 1.072383 0.600752 0.877049 11.00000 0.06063 0.02440 = 0.02879 -0.00545 -0.01990 0.00075 O3 4 1.132882 0.452674 0.861110 11.00000 0.03244 0.02555 = 0.01835 0.00000 -0.01093 -0.00026 CU1 5 0.746656 0.485850 0.508915 11.00000 0.02232 0.01575 = 0.01729 -0.00060 -0.00670 0.00181 I1 6 0.582065 0.598388 0.384530 11.00000 0.02164 0.02136 = 0.02228 0.00587 -0.00445 0.00192 HKLF 4 REM SIR97 run in space group P 21/c REM R1 = 0.0205 for 2940 Fo > 4sig(Fo) and 0.0273 for all 3516 data REM 181 parameters refined using 0 restraints END WGHT 0.0209 0.0000 REM Highest difference peak 0.502, deepest hole -0.527, 1-sigma level 0.091 Q1 1 0.5777 0.5341 0.3833 11.00000 0.05 0.50 Q2 1 0.6027 0.6585 0.4000 11.00000 0.05 0.43 Q3 1 0.5560 0.6542 0.3613 11.00000 0.05 0.43 Q4 1 0.6470 0.3164 0.3190 11.00000 0.05 0.43 Q5 1 0.9122 0.5523 0.7186 11.00000 0.05 0.38 Q6 1 0.9340 0.4732 0.7137 11.00000 0.05 0.37 Q7 1 0.8173 0.2664 0.4277 11.00000 0.05 0.34 Q8 1 0.8110 0.5869 0.6409 11.00000 0.05 0.33 Q9 1 0.8256 0.6299 0.7182 11.00000 0.05 0.33 Q10 1 0.6923 0.3644 0.3791 11.00000 0.05 0.33 ; _shelx_res_checksum 85840 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 C1 C 0.6476(3) 0.36402(18) 0.33048(19) 0.0248(5) Uani 1 1 d . . H1 H 0.5881 0.4148 0.3013 0.030 Uiso 1 1 calc R U C2 C 0.6365(3) 0.28141(19) 0.2809(2) 0.0275(6) Uani 1 1 d . . H2 H 0.5725 0.2759 0.2179 0.033 Uiso 1 1 calc R U C3 C 0.7196(3) 0.20630(19) 0.3239(2) 0.0253(5) Uani 1 1 d . . H3 H 0.7104 0.1481 0.2922 0.030 Uiso 1 1 calc R U C4 C 0.8163(3) 0.21782(17) 0.41384(19) 0.0227(5) Uani 1 1 d . . H4 H 0.8766 0.1679 0.4443 0.027 Uiso 1 1 calc R U C5 C 0.8239(3) 0.30353(16) 0.45894(17) 0.0178(5) Uani 1 1 d . . C6 C 0.9278(3) 0.31923(17) 0.55632(18) 0.0225(5) Uani 1 1 d . . H6A H 0.8947 0.2745 0.6085 0.027 Uiso 1 1 calc R U H6B H 1.0508 0.3107 0.5440 0.027 Uiso 1 1 calc R U C7 C 0.9711(3) 0.43346(16) 0.68151(18) 0.0176(4) Uani 1 1 d . . H7 H 1.0402 0.3883 0.7150 0.021 Uiso 1 1 calc R U C8 C 0.9566(3) 0.51849(16) 0.73239(17) 0.0185(5) Uani 1 1 d . . C9 C 0.8580(3) 0.59057(16) 0.68927(18) 0.0201(5) Uani 1 1 d . . C10 C 0.8402(4) 0.68153(18) 0.7409(2) 0.0285(6) Uani 1 1 d . . H10A H 0.7604 0.7199 0.7002 0.043 Uiso 1 1 calc R U H10B H 0.9523 0.7114 0.7469 0.043 Uiso 1 1 calc R U H10C H 0.7962 0.6726 0.8092 0.043 Uiso 1 1 calc R U C11 C 1.0560(3) 0.53106(17) 0.82874(19) 0.0229(5) Uani 1 1 d . . C12 C 1.2489(4) 0.4611(2) 0.9497(2) 0.0319(6) Uani 1 1 d . . H12A H 1.1857 0.4804 1.0100 0.038 Uiso 1 1 calc R U H12B H 1.3383 0.5070 0.9370 0.038 Uiso 1 1 calc R U C13 C 1.3283(4) 0.3699(2) 0.9681(2) 0.0383(7) Uani 1 1 d . . H13A H 1.2399 0.3262 0.9864 0.057 Uiso 1 1 calc R U H13B H 1.4150 0.3742 1.0242 0.057 Uiso 1 1 calc R U H13C H 1.3823 0.3493 0.9060 0.057 Uiso 1 1 calc R U N1 N 0.7396(3) 0.37553(14) 0.41891(15) 0.0190(4) Uani 1 1 d . . N2 N 0.8990(2) 0.41143(13) 0.59341(15) 0.0185(4) Uani 1 1 d . . O1 O 0.7763(2) 0.58522(12) 0.60334(13) 0.0252(4) Uani 1 1 d . . O2 O 1.0724(3) 0.60075(14) 0.87705(15) 0.0385(5) Uani 1 1 d . . O3 O 1.1329(2) 0.45267(12) 0.86111(13) 0.0258(4) Uani 1 1 d . . Cu1 Cu 0.74666(4) 0.48585(2) 0.50892(2) 0.01866(7) Uani 1 1 d . . I1 I 0.58207(2) 0.59839(2) 0.38453(2) 0.02191(5) 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 C1 0.0273(12) 0.0276(13) 0.0189(12) -0.0014(10) -0.0081(10) 0.0034(11) C2 0.0265(12) 0.0334(15) 0.0219(13) -0.0056(10) -0.0060(10) 0.0010(11) C3 0.0241(12) 0.0261(13) 0.0258(13) -0.0109(10) 0.0003(10) 0.0002(11) C4 0.0226(11) 0.0207(12) 0.0247(13) -0.0037(9) -0.0020(10) 0.0011(10) C5 0.0165(10) 0.0199(12) 0.0168(11) -0.0015(8) 0.0000(9) -0.0011(9) C6 0.0296(12) 0.0164(11) 0.0206(12) -0.0009(9) -0.0095(10) 0.0019(10) C7 0.0163(10) 0.0187(11) 0.0174(11) 0.0020(8) -0.0031(9) -0.0032(9) C8 0.0213(11) 0.0194(11) 0.0147(11) -0.0009(8) -0.0013(9) -0.0037(9) C9 0.0221(11) 0.0182(11) 0.0200(11) -0.0010(9) 0.0006(9) -0.0043(10) C10 0.0349(14) 0.0217(13) 0.0283(14) -0.0059(10) -0.0067(11) 0.0021(11) C11 0.0271(12) 0.0232(12) 0.0183(12) 0.0009(9) -0.0021(10) -0.0053(10) C12 0.0383(15) 0.0346(15) 0.0215(13) 0.0007(10) -0.0155(12) -0.0031(12) C13 0.0360(15) 0.0447(18) 0.0328(16) 0.0017(13) -0.0150(13) 0.0038(14) N1 0.0201(9) 0.0197(10) 0.0168(9) 0.0000(7) -0.0035(8) -0.0008(8) N2 0.0191(9) 0.0164(10) 0.0194(10) 0.0001(7) -0.0040(8) -0.0017(8) O1 0.0329(9) 0.0195(9) 0.0222(9) -0.0030(7) -0.0103(7) 0.0020(8) O2 0.0606(13) 0.0244(10) 0.0288(10) -0.0054(8) -0.0199(10) 0.0008(10) O3 0.0324(9) 0.0255(9) 0.0183(9) 0.0000(7) -0.0109(8) -0.0003(8) Cu1 0.02232(14) 0.01575(14) 0.01729(14) -0.00060(10) -0.00670(11) 0.00181(12) I1 0.02164(8) 0.02136(8) 0.02228(8) 0.00587(6) -0.00445(6) 0.00192(7) 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' O O 0.0106 0.0060 '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 N1 C1 C2 122.4(2) N1 C1 H1 118.8 C2 C1 H1 118.8 C1 C2 C3 119.3(2) C1 C2 H2 120.4 C3 C2 H2 120.4 C4 C3 C2 118.6(2) C4 C3 H3 120.7 C2 C3 H3 120.7 C3 C4 C5 119.0(2) C3 C4 H4 120.5 C5 C4 H4 120.5 N1 C5 C4 122.4(2) N1 C5 C6 116.8(2) C4 C5 C6 120.8(2) N2 C6 C5 109.87(19) N2 C6 H6A 109.7 C5 C6 H6A 109.7 N2 C6 H6B 109.7 C5 C6 H6B 109.7 H6A C6 H6B 108.2 N2 C7 C8 126.3(2) N2 C7 H7 116.8 C8 C7 H7 116.8 C9 C8 C7 121.5(2) C9 C8 C11 120.7(2) C7 C8 C11 117.6(2) O1 C9 C8 123.5(2) O1 C9 C10 113.5(2) C8 C9 C10 122.9(2) C9 C10 H10A 109.5 C9 C10 H10B 109.5 H10A C10 H10B 109.5 C9 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 O2 C11 O3 121.2(2) O2 C11 C8 126.8(2) O3 C11 C8 112.0(2) O3 C12 C13 107.2(2) O3 C12 H12A 110.3 C13 C12 H12A 110.3 O3 C12 H12B 110.3 C13 C12 H12B 110.3 H12A C12 H12B 108.5 C12 C13 H13A 109.5 C12 C13 H13B 109.5 H13A C13 H13B 109.5 C12 C13 H13C 109.5 H13A C13 H13C 109.5 H13B C13 H13C 109.5 C5 N1 C1 118.3(2) C5 N1 Cu1 113.96(15) C1 N1 Cu1 127.41(17) C7 N2 C6 117.25(19) C7 N2 Cu1 126.93(17) C6 N2 Cu1 115.73(14) C9 O1 Cu1 131.22(16) C11 O3 C12 115.6(2) O1 Cu1 N2 90.31(8) O1 Cu1 N1 173.28(8) N2 Cu1 N1 83.18(8) O1 Cu1 I1 87.98(5) N2 Cu1 I1 171.32(6) N1 Cu1 I1 98.22(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.348(3) C1 C2 1.376(4) C1 H1 0.9500 C2 C3 1.387(4) C2 H2 0.9500 C3 C4 1.383(3) C3 H3 0.9500 C4 C5 1.389(3) C4 H4 0.9500 C5 N1 1.340(3) C5 C6 1.500(3) C6 N2 1.458(3) C6 H6A 0.9900 C6 H6B 0.9900 C7 N2 1.303(3) C7 C8 1.421(3) C7 H7 0.9500 C8 C9 1.412(3) C8 C11 1.465(3) C9 O1 1.272(3) C9 C10 1.505(3) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 O2 1.206(3) C11 O3 1.357(3) C12 O3 1.447(3) C12 C13 1.490(4) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 N1 Cu1 2.001(2) N2 Cu1 1.9298(19) O1 Cu1 1.9189(17) Cu1 I1 2.6186(3) 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 N1 C1 C2 C3 1.4(4) C1 C2 C3 C4 -2.3(4) C2 C3 C4 C5 1.3(4) C3 C4 C5 N1 0.6(4) C3 C4 C5 C6 -179.8(2) N1 C5 C6 N2 6.0(3) C4 C5 C6 N2 -173.6(2) N2 C7 C8 C9 -0.3(4) N2 C7 C8 C11 -176.7(2) C7 C8 C9 O1 -0.1(4) C11 C8 C9 O1 176.2(2) C7 C8 C9 C10 -179.8(2) C11 C8 C9 C10 -3.6(4) C9 C8 C11 O2 -4.0(4) C7 C8 C11 O2 172.4(3) C9 C8 C11 O3 176.0(2) C7 C8 C11 O3 -7.6(3) C4 C5 N1 C1 -1.5(4) C6 C5 N1 C1 178.9(2) C4 C5 N1 Cu1 171.99(19) C6 C5 N1 Cu1 -7.6(3) C2 C1 N1 C5 0.5(4) C2 C1 N1 Cu1 -172.0(2) C8 C7 N2 C6 -178.5(2) C8 C7 N2 Cu1 -2.1(4) C5 C6 N2 C7 175.3(2) C5 C6 N2 Cu1 -1.5(3) C8 C9 O1 Cu1 3.1(4) C10 C9 O1 Cu1 -177.15(18) O2 C11 O3 C12 -6.6(4) C8 C11 O3 C12 173.5(2) C13 C12 O3 C11 -176.1(2)