#------------------------------------------------------------------------------ #$Date: 2018-01-16 04:34:49 +0200 (Tue, 16 Jan 2018) $ #$Revision: 205237 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229966.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_7229966 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 Cl2 Cu2 N4 O6' _chemical_formula_sum 'C26 H30 Cl2 Cu2 N4 O6' _chemical_formula_weight 692.54 _chemical_name_common '[CuL30aCl]' _chemical_name_systematic ; ? ; _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -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 _audit_update_record ; 2018-01-11 deposited with the CCDC. 2018-01-15 downloaded from the CCDC. ; _cell_angle_alpha 94.110(6) _cell_angle_beta 96.016(6) _cell_angle_gamma 105.895(6) _cell_formula_units_Z 1 _cell_length_a 7.3859(5) _cell_length_b 9.1298(7) _cell_length_c 10.3252(7) _cell_measurement_reflns_used 5999 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 28.40 _cell_measurement_theta_min 2.00 _cell_volume 662.26(8) _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 0.976 _diffrn_measured_fraction_theta_max 0.913 _diffrn_measurement_device_type STOE-STADIVARI _diffrn_measurement_method omega-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.0820 _diffrn_reflns_av_unetI/netI 0.0707 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.913 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 6277 _diffrn_reflns_point_group_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.913 _diffrn_reflns_theta_full 25.240 _diffrn_reflns_theta_max 28.497 _diffrn_reflns_theta_min 1.994 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.858 _exptl_absorpt_correction_type none _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.736 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 354 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.105 _exptl_crystal_size_min 0.093 _refine_diff_density_max 1.343 _refine_diff_density_min -1.727 _refine_diff_density_rms 0.147 _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 181 _refine_ls_number_reflns 3054 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0701 _refine_ls_R_factor_gt 0.0609 _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^)+(0.1157P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1635 _refine_ls_wR_factor_ref 0.1742 _reflns_number_gt 2501 _reflns_number_total 3054 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02007d2.cif _cod_data_source_block cl100 _cod_database_code 7229966 _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. ; _shelxl_version_number 2014-3 _shelx_res_file ; TITL cl100 in P -1 CELL 0.71069 7.3859 9.1298 10.3252 94.110 96.016 105.895 ZERR 2.00 0.0005 0.0007 0.0007 0.006 0.006 0.006 LATT 1 SFAC C H N O CL CU UNIT 26 30 4 6 2 2 MERG 2 FMAP 2 PLAN 10 ACTA BOND $H CONF LIST 4 L.S. 20 HTAB TEMP -140.00 WGHT 0.115700 FVAR 0.58965 C1 1 0.420384 0.275610 0.664393 11.00000 0.04014 0.03605 = 0.02176 0.00515 0.00107 0.01746 AFIX 43 H1 2 0.476512 0.208638 0.709570 11.00000 -1.20000 AFIX 0 C2 1 0.454557 0.424290 0.718599 11.00000 0.04060 0.04184 = 0.02085 0.00518 0.00006 0.01670 AFIX 43 H2 2 0.531871 0.458928 0.800485 11.00000 -1.20000 AFIX 0 C3 1 0.374851 0.522816 0.652309 11.00000 0.04585 0.03259 = 0.02646 0.00458 0.00423 0.01480 AFIX 43 H3 2 0.398114 0.626193 0.687715 11.00000 -1.20000 AFIX 0 C4 1 0.261399 0.469234 0.534396 11.00000 0.04109 0.03814 = 0.02371 0.00784 0.00263 0.02067 AFIX 43 H4 2 0.204900 0.534952 0.487753 11.00000 -1.20000 AFIX 0 C5 1 0.230893 0.317855 0.484788 11.00000 0.03551 0.03271 = 0.02254 0.00592 0.00441 0.01521 C6 1 0.110083 0.251916 0.356279 11.00000 0.03975 0.03225 = 0.02535 0.00711 -0.00143 0.01813 AFIX 23 H6A 2 -0.020528 0.259310 0.360138 11.00000 -1.20000 H6B 2 0.162676 0.310931 0.285290 11.00000 -1.20000 AFIX 0 C7 1 -0.006796 0.015946 0.225551 11.00000 0.03959 0.03496 = 0.02250 0.00945 0.00310 0.01783 AFIX 43 H7 2 -0.079540 0.070180 0.177760 11.00000 -1.20000 AFIX 0 C8 1 -0.032577 -0.139437 0.176672 11.00000 0.03576 0.03349 = 0.02265 0.00425 0.00027 0.01361 C9 1 0.065930 -0.231544 0.240423 11.00000 0.03596 0.02965 = 0.02081 0.00147 0.00088 0.00998 C10 1 0.043555 -0.394662 0.188743 11.00000 0.04333 0.02971 = 0.03359 0.00308 -0.00045 0.01596 AFIX 133 H10A 2 0.117519 -0.440362 0.249807 11.00000 -1.50000 H10B 2 0.089310 -0.396870 0.103099 11.00000 -1.50000 H10C 2 -0.090739 -0.453027 0.179653 11.00000 -1.50000 AFIX 0 C11 1 -0.169130 -0.201163 0.058293 11.00000 0.03989 0.03569 = 0.02338 0.00687 0.00094 0.01362 C12 1 -0.424725 -0.154769 -0.080123 11.00000 0.04594 0.04099 = 0.02242 0.00469 -0.00404 0.01781 AFIX 23 H12A 2 -0.380449 -0.213315 -0.148428 11.00000 -1.20000 H12B 2 -0.447566 -0.063334 -0.117065 11.00000 -1.20000 AFIX 0 C13 1 -0.607088 -0.252813 -0.042475 11.00000 0.04959 0.04164 = 0.03016 0.00426 0.00238 0.01807 AFIX 133 H13A 2 -0.589266 -0.350203 -0.018115 11.00000 -1.50000 H13B 2 -0.707570 -0.272580 -0.116851 11.00000 -1.50000 H13C 2 -0.643156 -0.199490 0.032050 11.00000 -1.50000 AFIX 0 N1 3 0.309208 0.221847 0.548633 11.00000 0.03593 0.03398 = 0.02319 0.00913 0.00426 0.01803 N2 3 0.105713 0.091474 0.328628 11.00000 0.03824 0.03266 = 0.02605 0.00688 0.00063 0.01785 O1 4 0.179052 -0.185073 0.347706 11.00000 0.04402 0.03356 = 0.03117 0.00610 -0.00317 0.02054 O2 4 -0.190647 -0.319949 -0.009707 11.00000 0.05821 0.04265 = 0.03301 -0.00685 -0.01048 0.02623 O3 4 -0.279610 -0.106901 0.032211 11.00000 0.04552 0.04020 = 0.02479 0.00244 -0.00786 0.02119 CL1 5 0.380398 -0.092751 0.622336 11.00000 0.04124 0.03417 = 0.02480 0.01093 0.00302 0.01841 CU1 6 0.257898 0.011829 0.452336 11.00000 0.03797 0.02971 = 0.02347 0.00635 -0.00108 0.01666 HKLF 4 REM cl100 in P -1 REM R1 = 0.0609 for 2501 Fo > 4sig(Fo) and 0.0701 for all 3054 data REM 181 parameters refined using 0 restraints END WGHT 0.1157 0.0000 REM Instructions for potential hydrogen bonds HTAB C1 Cl1 EQIV $1 -x, -y, -z+1 HTAB C6 Cl1_$1 EQIV $2 x-1, y, z-1 HTAB C12 Cl1_$2 REM Highest difference peak 1.343, deepest hole -1.727, 1-sigma level 0.147 Q1 1 0.3970 0.0275 0.4546 11.00000 0.05 1.34 Q2 1 0.1172 -0.0124 0.4507 11.00000 0.05 1.11 Q3 1 0.5107 -0.0792 0.6180 11.00000 0.05 0.91 Q4 1 0.2305 -0.1146 0.6163 11.00000 0.05 0.88 Q5 1 0.1567 -0.0764 0.5193 11.00000 0.05 0.63 Q6 1 0.1683 -0.1635 0.4244 11.00000 0.05 0.62 Q7 1 0.3621 0.1856 0.4859 11.00000 0.05 0.57 Q8 1 0.0313 -0.0679 0.5133 11.00000 0.05 0.53 Q9 1 0.3124 0.1036 0.3669 11.00000 0.05 0.51 Q10 1 0.3213 -0.1142 0.4395 11.00000 0.05 0.51 ; _shelx_res_checksum 68399 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 C1 C 0.4204(6) 0.2756(5) 0.6644(4) 0.0314(8) Uani 1 1 d . . H1 H 0.4765 0.2086 0.7096 0.038 Uiso 1 1 calc R U C2 C 0.4546(6) 0.4243(5) 0.7186(4) 0.0336(9) Uani 1 1 d . . H2 H 0.5319 0.4589 0.8005 0.040 Uiso 1 1 calc R U C3 C 0.3749(6) 0.5228(5) 0.6523(4) 0.0342(9) Uani 1 1 d . . H3 H 0.3981 0.6262 0.6877 0.041 Uiso 1 1 calc R U C4 C 0.2614(6) 0.4692(5) 0.5344(4) 0.0323(8) Uani 1 1 d . . H4 H 0.2049 0.5350 0.4878 0.039 Uiso 1 1 calc R U C5 C 0.2309(6) 0.3179(5) 0.4848(4) 0.0289(8) Uani 1 1 d . . C6 C 0.1101(6) 0.2519(5) 0.3563(4) 0.0311(8) Uani 1 1 d . . H6A H -0.0205 0.2593 0.3601 0.037 Uiso 1 1 calc R U H6B H 0.1627 0.3109 0.2853 0.037 Uiso 1 1 calc R U C7 C -0.0068(6) 0.0159(5) 0.2256(4) 0.0306(8) Uani 1 1 d . . H7 H -0.0795 0.0702 0.1778 0.037 Uiso 1 1 calc R U C8 C -0.0326(6) -0.1394(5) 0.1767(4) 0.0301(8) Uani 1 1 d . . C9 C 0.0659(6) -0.2315(5) 0.2404(4) 0.0289(8) Uani 1 1 d . . C10 C 0.0436(6) -0.3947(5) 0.1887(4) 0.0348(9) Uani 1 1 d . . H10A H 0.1175 -0.4404 0.2498 0.052 Uiso 1 1 calc R U H10B H 0.0893 -0.3969 0.1031 0.052 Uiso 1 1 calc R U H10C H -0.0907 -0.4530 0.1797 0.052 Uiso 1 1 calc R U C11 C -0.1691(6) -0.2012(5) 0.0583(4) 0.0324(8) Uani 1 1 d . . C12 C -0.4247(6) -0.1548(5) -0.0801(4) 0.0359(9) Uani 1 1 d . . H12A H -0.3804 -0.2133 -0.1484 0.043 Uiso 1 1 calc R U H12B H -0.4476 -0.0633 -0.1171 0.043 Uiso 1 1 calc R U C13 C -0.6071(7) -0.2528(6) -0.0425(4) 0.0396(10) Uani 1 1 d . . H13A H -0.5893 -0.3502 -0.0181 0.059 Uiso 1 1 calc R U H13B H -0.7076 -0.2726 -0.1169 0.059 Uiso 1 1 calc R U H13C H -0.6432 -0.1995 0.0321 0.059 Uiso 1 1 calc R U N1 N 0.3092(5) 0.2218(4) 0.5486(3) 0.0291(7) Uani 1 1 d . . N2 N 0.1057(5) 0.0915(4) 0.3286(3) 0.0308(7) Uani 1 1 d . . O1 O 0.1791(4) -0.1851(4) 0.3477(3) 0.0348(6) Uani 1 1 d . . O2 O -0.1906(5) -0.3199(4) -0.0097(3) 0.0440(8) Uani 1 1 d . . O3 O -0.2796(4) -0.1069(4) 0.0322(3) 0.0360(7) Uani 1 1 d . . Cl1 Cl 0.38040(14) -0.09275(12) 0.62234(9) 0.0316(2) Uani 1 1 d . . Cu1 Cu 0.25790(7) 0.01183(6) 0.45234(4) 0.0292(2) 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 0.040(2) 0.036(2) 0.0218(17) 0.0051(15) 0.0011(14) 0.0175(17) C2 0.041(2) 0.042(2) 0.0208(17) 0.0052(16) 0.0001(14) 0.0167(17) C3 0.046(2) 0.033(2) 0.0265(19) 0.0046(16) 0.0042(16) 0.0148(17) C4 0.041(2) 0.038(2) 0.0237(18) 0.0078(16) 0.0026(15) 0.0207(17) C5 0.0355(19) 0.033(2) 0.0225(17) 0.0059(15) 0.0044(14) 0.0152(15) C6 0.040(2) 0.032(2) 0.0254(18) 0.0071(15) -0.0014(14) 0.0181(16) C7 0.040(2) 0.035(2) 0.0225(17) 0.0094(15) 0.0031(14) 0.0178(16) C8 0.0358(19) 0.033(2) 0.0227(17) 0.0043(15) 0.0003(14) 0.0136(16) C9 0.0360(19) 0.030(2) 0.0208(17) 0.0015(15) 0.0009(13) 0.0100(15) C10 0.043(2) 0.030(2) 0.034(2) 0.0031(17) -0.0005(16) 0.0160(17) C11 0.040(2) 0.036(2) 0.0234(18) 0.0069(16) 0.0009(14) 0.0136(17) C12 0.046(2) 0.041(2) 0.0224(18) 0.0047(17) -0.0040(15) 0.0178(18) C13 0.050(2) 0.042(3) 0.030(2) 0.0043(18) 0.0024(17) 0.018(2) N1 0.0359(16) 0.0340(19) 0.0232(15) 0.0091(13) 0.0043(12) 0.0180(14) N2 0.0382(17) 0.0327(19) 0.0260(16) 0.0069(13) 0.0006(12) 0.0178(14) O1 0.0440(16) 0.0336(16) 0.0312(15) 0.0061(12) -0.0032(12) 0.0205(13) O2 0.058(2) 0.043(2) 0.0330(16) -0.0069(14) -0.0105(14) 0.0262(16) O3 0.0455(16) 0.0402(18) 0.0248(14) 0.0024(12) -0.0079(11) 0.0212(13) Cl1 0.0412(5) 0.0342(5) 0.0248(5) 0.0109(4) 0.0030(3) 0.0184(4) Cu1 0.0380(3) 0.0297(3) 0.0235(3) 0.00635(19) -0.00108(18) 0.0167(2) 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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C1 C2 122.0(4) N1 C1 H1 119.0 C2 C1 H1 119.0 C1 C2 C3 119.2(4) C1 C2 H2 120.4 C3 C2 H2 120.4 C4 C3 C2 119.3(4) C4 C3 H3 120.4 C2 C3 H3 120.4 C3 C4 C5 119.0(4) C3 C4 H4 120.5 C5 C4 H4 120.5 N1 C5 C4 121.9(4) N1 C5 C6 116.2(4) C4 C5 C6 122.0(3) N2 C6 C5 109.7(3) 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 127.0(4) N2 C7 H7 116.5 C8 C7 H7 116.5 C9 C8 C7 121.5(4) C9 C8 C11 121.1(4) C7 C8 C11 117.4(4) O1 C9 C8 123.3(4) O1 C9 C10 114.5(4) C8 C9 C10 122.2(4) 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 121.5(4) O2 C11 C8 127.7(4) O3 C11 C8 110.8(4) O3 C12 C13 110.9(3) O3 C12 H12A 109.5 C13 C12 H12A 109.5 O3 C12 H12B 109.5 C13 C12 H12B 109.5 H12A C12 H12B 108.0 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 118.6(4) C5 N1 Cu1 114.7(3) C1 N1 Cu1 126.6(3) C7 N2 C6 116.4(3) C7 N2 Cu1 126.8(3) C6 N2 Cu1 116.7(3) C9 O1 Cu1 130.9(3) C11 O3 C12 117.2(4) N2 Cu1 O1 90.36(14) N2 Cu1 N1 82.52(14) O1 Cu1 N1 172.41(12) N2 Cu1 Cl1 167.34(11) O1 Cu1 Cl1 90.67(9) N1 Cu1 Cl1 95.70(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.354(5) C1 C2 1.376(6) C1 H1 0.9500 C2 C3 1.385(5) C2 H2 0.9500 C3 C4 1.378(6) C3 H3 0.9500 C4 C5 1.388(6) C4 H4 0.9500 C5 N1 1.348(5) C5 C6 1.504(6) C6 N2 1.463(5) C6 H6A 0.9900 C6 H6B 0.9900 C7 N2 1.302(5) C7 C8 1.426(6) C7 H7 0.9500 C8 C9 1.408(5) C8 C11 1.470(6) C9 O1 1.284(5) C9 C10 1.504(6) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 O2 1.211(6) C11 O3 1.360(5) C12 O3 1.448(5) C12 C13 1.505(6) C12 H12A 0.9900 C12 H12B 0.9900 C13 H13A 0.9800 C13 H13B 0.9800 C13 H13C 0.9800 N1 Cu1 2.015(4) N2 Cu1 1.924(3) O1 Cu1 1.938(3) Cl1 Cu1 2.2785(9) 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 -0.8(6) C1 C2 C3 C4 0.8(6) C2 C3 C4 C5 -0.4(6) C3 C4 C5 N1 -0.1(6) C3 C4 C5 C6 -179.5(4) N1 C5 C6 N2 -0.2(5) C4 C5 C6 N2 179.3(3) N2 C7 C8 C9 0.8(6) N2 C7 C8 C11 179.6(4) C7 C8 C9 O1 2.5(6) C11 C8 C9 O1 -176.3(4) C7 C8 C9 C10 -178.7(4) C11 C8 C9 C10 2.5(6) C9 C8 C11 O2 -13.5(7) C7 C8 C11 O2 167.7(4) C9 C8 C11 O3 165.1(4) C7 C8 C11 O3 -13.7(5) C4 C5 N1 C1 0.1(6) C6 C5 N1 C1 179.5(3) C4 C5 N1 Cu1 -176.4(3) C6 C5 N1 Cu1 3.1(4) C2 C1 N1 C5 0.3(6) C2 C1 N1 Cu1 176.3(3) C8 C7 N2 C6 178.4(4) C8 C7 N2 Cu1 -4.5(6) C5 C6 N2 C7 174.4(3) C5 C6 N2 Cu1 -3.0(4) C8 C9 O1 Cu1 -1.8(6) C10 C9 O1 Cu1 179.3(3) O2 C11 O3 C12 0.2(6) C8 C11 O3 C12 -178.5(4) C13 C12 O3 C11 88.7(4)