#------------------------------------------------------------------------------ #$Date: 2019-11-17 09:06:29 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229011 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229967.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_7229967 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_issue 6 _journal_name_full CrystEngComm _journal_page_first 818 _journal_paper_doi 10.1039/C7CE02007D _journal_volume 20 _journal_year 2018 _chemical_formula_moiety 'C24 H26 Cl2 Cu2 N4 O6' _chemical_formula_sum 'C24 H26 Cl2 Cu2 N4 O6' _chemical_formula_weight 664.46 _chemical_name_common '[CuL30iCl]' _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 90.393(5) _cell_angle_beta 96.377(5) _cell_angle_gamma 110.150(5) _cell_formula_units_Z 1 _cell_length_a 7.5941(5) _cell_length_b 9.0685(6) _cell_length_c 10.0399(6) _cell_measurement_reflns_used 5836 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 28.44 _cell_measurement_theta_min 2.05 _cell_volume 644.33(7) _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 0.981 _diffrn_measured_fraction_theta_max 0.929 _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 0.0786 _diffrn_reflns_av_unetI/netI 0.0715 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.929 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 7133 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.929 _diffrn_reflns_theta_full 25.240 _diffrn_reflns_theta_max 28.488 _diffrn_reflns_theta_min 2.043 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.906 _exptl_absorpt_correction_type none _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 338 _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.105 _exptl_crystal_size_min 0.082 _refine_diff_density_max 0.801 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.106 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 172 _refine_ls_number_reflns 3031 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.942 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0470 _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^)+(0.0725P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1161 _refine_ls_wR_factor_ref 0.1218 _reflns_number_gt 2347 _reflns_number_total 3031 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02007d2.cif _cod_data_source_block cl094 _cod_depositor_comments 'Adding full bibliography for 7229962--7229987.cif.' _cod_database_code 7229967 _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 cl094 in P -1 CELL 0.71069 7.5941 9.0685 10.0399 90.393 96.377 110.150 ZERR 2.00 0.0005 0.0006 0.0006 0.005 0.005 0.005 LATT 1 SFAC C H N O CL CU UNIT 24 26 4 6 2 2 MERG 2 FMAP 2 PLAN 10 ACTA BOND $H CONF LIST 4 L.S. 20 TEMP -140.00 WGHT 0.072500 FVAR 0.63881 C1 1 0.578056 0.235904 -0.163954 11.00000 0.04722 0.02813 = 0.02998 0.00103 -0.00451 0.01280 AFIX 43 H1 2 0.520082 0.303176 -0.207425 11.00000 -1.20000 AFIX 0 C2 1 0.550025 0.091772 -0.224291 11.00000 0.05145 0.02559 = 0.03171 -0.00239 -0.00257 0.00753 AFIX 43 H2 2 0.474184 0.060137 -0.308438 11.00000 -1.20000 AFIX 0 C3 1 0.633906 -0.006854 -0.160717 11.00000 0.05391 0.02155 = 0.03629 -0.00281 0.00156 0.01114 AFIX 43 H3 2 0.616873 -0.106455 -0.201452 11.00000 -1.20000 AFIX 0 C4 1 0.742135 0.040419 -0.038094 11.00000 0.04721 0.02485 = 0.03899 0.00014 0.00129 0.01271 AFIX 43 H4 2 0.799490 -0.026134 0.007303 11.00000 -1.20000 AFIX 0 C5 1 0.765529 0.188098 0.017798 11.00000 0.03903 0.02366 = 0.03157 0.00120 -0.00051 0.00902 C6 1 0.877010 0.245244 0.152187 11.00000 0.04894 0.02236 = 0.03857 -0.00284 -0.00760 0.01196 AFIX 23 H6A 2 0.814737 0.177323 0.222453 11.00000 -1.20000 H6B 2 1.005504 0.240739 0.152765 11.00000 -1.20000 AFIX 0 C7 1 1.010545 0.485245 0.280229 11.00000 0.04316 0.02801 = 0.03026 0.00099 -0.00208 0.01212 AFIX 43 H7 2 1.089860 0.434176 0.323456 11.00000 -1.20000 AFIX 0 C8 1 1.035487 0.638651 0.331042 11.00000 0.04187 0.02922 = 0.03222 -0.00486 -0.00463 0.01000 C9 1 0.924727 0.724846 0.274978 11.00000 0.04604 0.02575 = 0.03906 -0.00438 0.00073 0.00933 C10 1 0.938547 0.882847 0.332850 11.00000 0.05953 0.03450 = 0.04755 -0.00918 -0.00901 0.01922 AFIX 133 H10A 2 0.856506 0.925209 0.275024 11.00000 -1.50000 H10B 2 1.069538 0.955126 0.338268 11.00000 -1.50000 H10C 2 0.898581 0.870910 0.422874 11.00000 -1.50000 AFIX 0 C11 1 1.185266 0.705699 0.443182 11.00000 0.04480 0.03561 = 0.03189 -0.00015 -0.00082 0.01084 C12 1 1.455702 0.683762 0.565886 11.00000 0.06497 0.06036 = 0.04057 -0.01357 -0.02222 0.02876 AFIX 133 H12A 2 1.535452 0.791113 0.549357 11.00000 -1.50000 H12B 2 1.532065 0.615689 0.571979 11.00000 -1.50000 H12C 2 1.402038 0.683863 0.650248 11.00000 -1.50000 AFIX 0 N1 3 0.685270 0.284472 -0.045063 11.00000 0.04099 0.02349 = 0.02877 0.00068 -0.00163 0.01077 N2 3 0.888999 0.408269 0.179891 11.00000 0.04400 0.02067 = 0.03429 -0.00138 -0.00553 0.01213 O1 4 0.805484 0.677838 0.169916 11.00000 0.04973 0.02756 = 0.04060 -0.00808 -0.01295 0.01504 O2 4 1.206261 0.819435 0.515589 11.00000 0.06558 0.04258 = 0.03921 -0.01511 -0.01041 0.02141 O3 4 1.305481 0.626019 0.457487 11.00000 0.05383 0.04143 = 0.03203 -0.00758 -0.01542 0.01901 CL1 5 0.633540 0.610222 -0.118693 11.00000 0.04799 0.02571 = 0.03465 0.00477 -0.00023 0.01531 CU1 6 0.734638 0.488443 0.056652 11.00000 0.04396 0.02188 = 0.03174 -0.00223 -0.00596 0.01238 HKLF 4 REM cl094 in P -1 REM R1 = 0.0470 for 2347 Fo > 4sig(Fo) and 0.0606 for all 3031 data REM 172 parameters refined using 0 restraints END WGHT 0.0725 0.0000 REM Highest difference peak 0.801, deepest hole -0.564, 1-sigma level 0.106 Q1 1 0.5745 0.4590 0.0892 11.00000 0.05 0.80 Q2 1 0.8792 0.5113 0.0196 11.00000 0.05 0.59 Q3 1 0.8453 0.4579 0.1406 11.00000 0.05 0.47 Q4 1 0.7127 0.5372 -0.0708 11.00000 0.05 0.46 Q5 1 0.4558 0.3937 -0.1772 11.00000 0.05 0.41 Q6 1 1.0041 0.6626 0.1585 11.00000 0.05 0.41 Q7 1 0.6703 0.5555 -0.0345 11.00000 0.05 0.40 Q8 1 1.0000 0.0000 0.0000 10.50000 0.05 0.35 Q9 1 0.6705 0.5398 0.1577 11.00000 0.05 0.35 Q10 1 0.7722 0.3910 -0.0205 11.00000 0.05 0.35 ; _shelx_res_checksum 22789 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 0.5781(5) 0.2359(4) -0.1640(3) 0.0359(7) Uani 1 1 d . . H1 H 0.5201 0.3032 -0.2074 0.043 Uiso 1 1 calc R U C2 C 0.5500(5) 0.0918(4) -0.2243(3) 0.0384(7) Uani 1 1 d . . H2 H 0.4742 0.0601 -0.3084 0.046 Uiso 1 1 calc R U C3 C 0.6339(5) -0.0069(4) -0.1607(3) 0.0381(7) Uani 1 1 d . . H3 H 0.6169 -0.1065 -0.2015 0.046 Uiso 1 1 calc R U C4 C 0.7421(5) 0.0404(4) -0.0381(3) 0.0373(7) Uani 1 1 d . . H4 H 0.7995 -0.0261 0.0073 0.045 Uiso 1 1 calc R U C5 C 0.7655(5) 0.1881(4) 0.0178(3) 0.0323(6) Uani 1 1 d . . C6 C 0.8770(5) 0.2452(4) 0.1522(3) 0.0378(7) Uani 1 1 d . . H6A H 0.8147 0.1773 0.2225 0.045 Uiso 1 1 calc R U H6B H 1.0055 0.2407 0.1528 0.045 Uiso 1 1 calc R U C7 C 1.0105(5) 0.4852(4) 0.2802(3) 0.0344(7) Uani 1 1 d . . H7 H 1.0899 0.4342 0.3235 0.041 Uiso 1 1 calc R U C8 C 1.0355(5) 0.6387(4) 0.3310(3) 0.0358(7) Uani 1 1 d . . C9 C 0.9247(5) 0.7248(4) 0.2750(3) 0.0382(7) Uani 1 1 d . . C10 C 0.9385(6) 0.8828(4) 0.3328(4) 0.0477(9) Uani 1 1 d . . H10A H 0.8565 0.9252 0.2750 0.072 Uiso 1 1 calc R U H10B H 1.0695 0.9551 0.3383 0.072 Uiso 1 1 calc R U H10C H 0.8986 0.8709 0.4229 0.072 Uiso 1 1 calc R U C11 C 1.1853(5) 0.7057(4) 0.4432(3) 0.0387(7) Uani 1 1 d . . C12 C 1.4557(7) 0.6838(5) 0.5659(4) 0.0558(11) Uani 1 1 d . . H12A H 1.5355 0.7911 0.5494 0.084 Uiso 1 1 calc R U H12B H 1.5321 0.6157 0.5720 0.084 Uiso 1 1 calc R U H12C H 1.4020 0.6839 0.6502 0.084 Uiso 1 1 calc R U N1 N 0.6853(4) 0.2845(3) -0.0451(3) 0.0317(5) Uani 1 1 d . . N2 N 0.8890(4) 0.4083(3) 0.1799(3) 0.0336(6) Uani 1 1 d . . O1 O 0.8055(4) 0.6778(3) 0.1699(2) 0.0404(5) Uani 1 1 d . . O2 O 1.2063(4) 0.8194(3) 0.5156(3) 0.0499(7) Uani 1 1 d . . O3 O 1.3055(4) 0.6260(3) 0.4575(2) 0.0435(6) Uani 1 1 d . . Cl1 Cl 0.63354(12) 0.61022(9) -0.11869(8) 0.0359(2) Uani 1 1 d . . Cu1 Cu 0.73464(6) 0.48844(4) 0.05665(4) 0.03314(15) 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 0.0472(19) 0.0281(16) 0.0300(15) 0.0010(12) -0.0045(13) 0.0128(14) C2 0.051(2) 0.0256(16) 0.0317(16) -0.0024(13) -0.0026(14) 0.0075(14) C3 0.054(2) 0.0215(15) 0.0363(16) -0.0028(12) 0.0016(15) 0.0111(14) C4 0.0472(19) 0.0248(16) 0.0390(17) 0.0001(13) 0.0013(14) 0.0127(14) C5 0.0390(17) 0.0237(14) 0.0316(15) 0.0012(12) -0.0005(13) 0.0090(12) C6 0.049(2) 0.0224(15) 0.0386(17) -0.0028(13) -0.0076(14) 0.0120(14) C7 0.0432(18) 0.0280(16) 0.0303(15) 0.0010(12) -0.0021(13) 0.0121(13) C8 0.0419(18) 0.0292(16) 0.0322(15) -0.0049(13) -0.0046(13) 0.0100(13) C9 0.0460(19) 0.0257(16) 0.0391(17) -0.0044(13) 0.0007(15) 0.0093(14) C10 0.060(2) 0.0345(19) 0.048(2) -0.0092(15) -0.0090(17) 0.0192(17) C11 0.0448(19) 0.0356(18) 0.0319(16) -0.0001(13) -0.0008(14) 0.0108(15) C12 0.065(3) 0.060(3) 0.041(2) -0.0136(18) -0.0222(18) 0.029(2) N1 0.0410(15) 0.0235(13) 0.0288(12) 0.0007(10) -0.0016(11) 0.0108(11) N2 0.0440(15) 0.0207(12) 0.0343(13) -0.0014(10) -0.0055(11) 0.0121(11) O1 0.0497(14) 0.0276(12) 0.0406(13) -0.0081(10) -0.0129(11) 0.0150(10) O2 0.0656(18) 0.0426(15) 0.0392(13) -0.0151(11) -0.0104(12) 0.0214(13) O3 0.0538(15) 0.0414(14) 0.0320(12) -0.0076(10) -0.0154(11) 0.0190(12) Cl1 0.0480(5) 0.0257(4) 0.0346(4) 0.0048(3) -0.0002(3) 0.0153(3) Cu1 0.0440(3) 0.0219(2) 0.0317(2) -0.00223(14) -0.00596(16) 0.01238(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' 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 121.9(3) N1 C1 H1 119.1 C2 C1 H1 119.1 C1 C2 C3 119.1(3) C1 C2 H2 120.4 C3 C2 H2 120.4 C4 C3 C2 119.6(3) C4 C3 H3 120.2 C2 C3 H3 120.2 C3 C4 C5 118.5(3) C3 C4 H4 120.7 C5 C4 H4 120.7 N1 C5 C4 121.7(3) N1 C5 C6 117.0(3) C4 C5 C6 121.3(3) N2 C6 C5 109.0(3) N2 C6 H6A 109.9 C5 C6 H6A 109.9 N2 C6 H6B 109.9 C5 C6 H6B 109.9 H6A C6 H6B 108.3 N2 C7 C8 126.0(3) N2 C7 H7 117.0 C8 C7 H7 117.0 C9 C8 C7 121.8(3) C9 C8 C11 121.2(3) C7 C8 C11 117.1(3) O1 C9 C8 123.4(3) O1 C9 C10 113.7(3) C8 C9 C10 122.9(3) 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 121.6(3) O2 C11 C8 126.8(3) O3 C11 C8 111.6(3) O3 C12 H12A 109.5 O3 C12 H12B 109.5 H12A C12 H12B 109.5 O3 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C1 N1 C5 119.1(3) C1 N1 Cu1 126.5(2) C5 N1 Cu1 114.4(2) C7 N2 C6 116.5(3) C7 N2 Cu1 127.1(2) C6 N2 Cu1 116.3(2) C9 O1 Cu1 130.8(2) C11 O3 C12 115.0(3) N2 Cu1 O1 90.01(10) N2 Cu1 N1 82.71(10) O1 Cu1 N1 172.67(10) N2 Cu1 Cl1 162.75(9) O1 Cu1 Cl1 90.71(7) N1 Cu1 Cl1 96.00(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.346(4) C1 C2 1.375(4) C1 H1 0.9500 C2 C3 1.387(5) C2 H2 0.9500 C3 C4 1.378(5) C3 H3 0.9500 C4 C5 1.394(4) C4 H4 0.9500 C5 N1 1.350(4) C5 C6 1.497(4) C6 N2 1.472(4) C6 H6A 0.9900 C6 H6B 0.9900 C7 N2 1.302(4) C7 C8 1.421(4) C7 H7 0.9500 C8 C9 1.410(5) C8 C11 1.470(5) C9 O1 1.277(4) C9 C10 1.508(5) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 O2 1.212(4) C11 O3 1.343(4) C12 O3 1.437(4) C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 N1 Cu1 2.004(3) N2 Cu1 1.926(3) O1 Cu1 1.932(2) Cl1 Cu1 2.2845(8) 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 0.3(5) C1 C2 C3 C4 0.6(5) C2 C3 C4 C5 -0.7(5) C3 C4 C5 N1 0.0(5) C3 C4 C5 C6 178.4(3) N1 C5 C6 N2 -5.7(4) C4 C5 C6 N2 175.8(3) N2 C7 C8 C9 0.4(6) N2 C7 C8 C11 -178.3(3) C7 C8 C9 O1 -5.4(6) C11 C8 C9 O1 173.2(3) C7 C8 C9 C10 175.5(3) C11 C8 C9 C10 -5.9(5) C9 C8 C11 O2 15.9(6) C7 C8 C11 O2 -165.4(4) C9 C8 C11 O3 -163.1(3) C7 C8 C11 O3 15.6(4) C2 C1 N1 C5 -1.0(5) C2 C1 N1 Cu1 -178.7(3) C4 C5 N1 C1 0.8(5) C6 C5 N1 C1 -177.7(3) C4 C5 N1 Cu1 178.8(3) C6 C5 N1 Cu1 0.3(4) C8 C7 N2 C6 -174.9(3) C8 C7 N2 Cu1 9.4(5) C5 C6 N2 C7 -167.3(3) C5 C6 N2 Cu1 8.9(4) C8 C9 O1 Cu1 0.2(5) C10 C9 O1 Cu1 179.4(3) O2 C11 O3 C12 1.4(5) C8 C11 O3 C12 -179.6(3)