#------------------------------------------------------------------------------ #$Date: 2019-11-17 09:06:29 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229011 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/99/7229985.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_7229985 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 Cu2 N10 O4, 2(H2O)' _chemical_formula_sum 'C24 H30 Cu2 N10 O6' _chemical_formula_weight 681.66 _chemical_name_common '[CuL30bN3]' _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-2014/7 _audit_update_record ; 2018-01-11 deposited with the CCDC. 2018-01-15 downloaded from the CCDC. ; _cell_angle_alpha 105.369(4) _cell_angle_beta 99.166(4) _cell_angle_gamma 97.860(4) _cell_formula_units_Z 1 _cell_length_a 7.3993(4) _cell_length_b 9.3862(5) _cell_length_c 10.6959(5) _cell_measurement_reflns_used 8571 _cell_measurement_temperature 133(2) _cell_measurement_theta_max 26.62 _cell_measurement_theta_min 2.02 _cell_volume 694.52(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 0.983 _diffrn_measured_fraction_theta_max 0.941 _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 0.0168 _diffrn_reflns_av_unetI/netI 0.0231 _diffrn_reflns_Laue_measured_fraction_full 0.983 _diffrn_reflns_Laue_measured_fraction_max 0.941 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 7901 _diffrn_reflns_point_group_measured_fraction_full 0.983 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.428 _diffrn_reflns_theta_min 2.017 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 1.590 _exptl_absorpt_correction_type none _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 350 _exptl_crystal_size_max 0.098 _exptl_crystal_size_mid 0.091 _exptl_crystal_size_min 0.059 _refine_diff_density_max 0.418 _refine_diff_density_min -0.692 _refine_diff_density_rms 0.072 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 190 _refine_ls_number_reflns 3289 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0256 _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^)+(0.0395P)^2^+0.2007P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.0686 _reflns_number_gt 2967 _reflns_number_total 3289 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7ce02007d2.cif _cod_data_source_block cl101 _cod_depositor_comments 'Adding full bibliography for 7229962--7229987.cif.' _cod_original_cell_volume 694.52(6) _cod_database_code 7229985 _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 -1 CELL 0.71073 7.3993 9.3862 10.6959 105.369 99.166 97.860 ZERR 2.00 0.0004 0.0005 0.0005 0.004 0.004 0.004 LATT 1 SFAC C H N O CU UNIT 24 26 10 6 2 MERG 2 FMAP 2 PLAN 10 ACTA BOND $H CONF LIST 4 L.S. 50 TEMP -140.00 WGHT 0.039500 0.200700 FVAR 0.49338 C1 1 0.504056 0.759149 0.230144 11.00000 0.01636 0.01718 = 0.01795 0.00153 0.00371 0.00008 AFIX 43 H1 2 0.454834 0.714898 0.290783 11.00000 -1.20000 AFIX 0 C2 1 0.446426 0.687587 0.096033 11.00000 0.01759 0.02114 = 0.01999 -0.00178 0.00116 -0.00072 AFIX 43 H2 2 0.361174 0.594334 0.064807 11.00000 -1.20000 AFIX 0 C3 1 0.515548 0.754605 0.007429 11.00000 0.02142 0.02664 = 0.01362 -0.00122 -0.00060 0.00335 AFIX 43 H3 2 0.475763 0.708867 -0.085363 11.00000 -1.20000 AFIX 0 C4 1 0.642671 0.888401 0.056083 11.00000 0.02250 0.02387 = 0.01379 0.00348 0.00293 0.00427 AFIX 43 H4 2 0.691853 0.935648 -0.002790 11.00000 -1.20000 AFIX 0 C5 1 0.697588 0.952880 0.192004 11.00000 0.01569 0.01624 = 0.01409 0.00302 0.00268 0.00253 C6 1 0.841736 1.095075 0.251336 11.00000 0.02313 0.02008 = 0.01236 0.00337 0.00377 -0.00294 AFIX 23 H6A 2 0.960618 1.079174 0.223546 11.00000 -1.20000 H6B 2 0.799531 1.177126 0.219257 11.00000 -1.20000 AFIX 0 C7 1 0.997422 1.253914 0.463646 11.00000 0.01404 0.01527 = 0.01756 0.00471 0.00447 0.00150 AFIX 43 H7 2 1.068688 1.301606 0.414549 11.00000 -1.20000 AFIX 0 C8 1 1.040768 1.317675 0.603619 11.00000 0.01261 0.01471 = 0.01722 0.00181 0.00157 0.00023 C9 1 0.959251 1.246059 0.688391 11.00000 0.01294 0.01756 = 0.01507 0.00134 0.00095 0.00292 C10 1 1.014285 1.304383 0.837369 11.00000 0.02128 0.02721 = 0.01386 0.00184 0.00053 -0.00032 AFIX 133 H10A 2 0.949981 1.387187 0.869540 11.00000 -1.50000 H10B 2 1.149338 1.340688 0.863760 11.00000 -1.50000 H10C 2 0.979297 1.223174 0.875612 11.00000 -1.50000 AFIX 0 C11 1 1.174174 1.460952 0.657975 11.00000 0.01642 0.01667 = 0.02086 0.00351 0.00015 0.00151 C12 1 1.314138 1.501468 0.578447 11.00000 0.01938 0.01838 = 0.02949 0.00419 0.00548 -0.00262 AFIX 133 H12A 2 1.251968 1.534479 0.506021 11.00000 -1.50000 H12B 2 1.367262 1.413233 0.541743 11.00000 -1.50000 H12C 2 1.413921 1.582959 0.636020 11.00000 -1.50000 AFIX 0 N1 3 0.628151 0.890022 0.277788 11.00000 0.01480 0.01551 = 0.01321 0.00240 0.00254 0.00188 N2 3 0.870466 1.137193 0.395910 11.00000 0.01698 0.01550 = 0.01204 0.00263 0.00318 0.00019 N3 3 0.565494 0.867064 0.535490 11.00000 0.01774 0.01658 = 0.01397 0.00482 0.00215 -0.00037 N4 3 0.620075 0.857049 0.644140 11.00000 0.01624 0.01504 = 0.01746 0.00450 0.00491 0.00053 N5 3 0.667301 0.843191 0.747589 11.00000 0.03173 0.03261 = 0.01889 0.01256 0.00270 0.00147 O1 4 0.841121 1.123598 0.645846 11.00000 0.01885 0.01970 = 0.01348 0.00328 0.00143 -0.00289 O2 4 1.175942 1.549747 0.765749 11.00000 0.03219 0.01889 = 0.02186 -0.00200 0.00312 -0.00310 O71 4 0.795794 1.574305 0.798458 11.00000 0.06293 0.06810 = 0.11441 0.04866 0.03343 0.02189 CU1 5 0.715777 1.010757 0.467678 11.00000 0.01417 0.01413 = 0.01025 0.00243 0.00222 -0.00109 HKLF 4 REM SIR97 run in space group P -1 REM R1 = 0.0256 for 2967 Fo > 4sig(Fo) and 0.0294 for all 3289 data REM 190 parameters refined using 0 restraints END WGHT 0.0395 0.2007 REM Highest difference peak 0.418, deepest hole -0.692, 1-sigma level 0.072 Q1 1 0.7673 1.0238 0.2232 11.00000 0.05 0.42 Q2 1 0.9439 1.5805 0.8057 11.00000 0.05 0.39 Q3 1 1.1050 1.3909 0.6351 11.00000 0.05 0.37 Q4 1 0.9098 1.1860 0.4246 11.00000 0.05 0.35 Q5 1 0.6619 0.9173 0.1213 11.00000 0.05 0.33 Q6 1 0.8644 1.1865 0.6572 11.00000 0.05 0.33 Q7 1 0.7630 1.6806 0.7933 11.00000 0.05 0.33 Q8 1 0.5942 0.8230 0.0358 11.00000 0.05 0.33 Q9 1 0.9926 1.2825 0.6419 11.00000 0.05 0.33 Q10 1 1.0088 1.2956 0.5365 11.00000 0.05 0.30 ; _shelx_res_checksum 1 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 0.5041(2) 0.75915(19) 0.23014(16) 0.0182(3) Uani 1 1 d . . H1 H 0.4548 0.7149 0.2908 0.022 Uiso 1 1 calc R U C2 C 0.4464(2) 0.6876(2) 0.09603(17) 0.0219(3) Uani 1 1 d . . H2 H 0.3612 0.5943 0.0648 0.026 Uiso 1 1 calc R U C3 C 0.5155(2) 0.7546(2) 0.00743(17) 0.0226(4) Uani 1 1 d . . H3 H 0.4758 0.7089 -0.0854 0.027 Uiso 1 1 calc R U C4 C 0.6427(2) 0.8884(2) 0.05608(16) 0.0206(3) Uani 1 1 d . . H4 H 0.6919 0.9356 -0.0028 0.025 Uiso 1 1 calc R U C5 C 0.6976(2) 0.95288(19) 0.19200(16) 0.0157(3) Uani 1 1 d . . C6 C 0.8417(2) 1.0951(2) 0.25134(16) 0.0195(3) Uani 1 1 d . . H6A H 0.9606 1.0792 0.2235 0.023 Uiso 1 1 calc R U H6B H 0.7995 1.1771 0.2193 0.023 Uiso 1 1 calc R U C7 C 0.9974(2) 1.25391(18) 0.46365(16) 0.0156(3) Uani 1 1 d . . H7 H 1.0687 1.3016 0.4145 0.019 Uiso 1 1 calc R U C8 C 1.0408(2) 1.31767(18) 0.60362(16) 0.0158(3) Uani 1 1 d . . C9 C 0.9593(2) 1.24606(19) 0.68839(16) 0.0161(3) Uani 1 1 d . . C10 C 1.0143(3) 1.3044(2) 0.83737(16) 0.0225(3) Uani 1 1 d . . H10A H 0.9500 1.3872 0.8695 0.034 Uiso 1 1 calc R U H10B H 1.1493 1.3407 0.8638 0.034 Uiso 1 1 calc R U H10C H 0.9793 1.2232 0.8756 0.034 Uiso 1 1 calc R U C11 C 1.1742(2) 1.46095(19) 0.65798(17) 0.0190(3) Uani 1 1 d . . C12 C 1.3141(2) 1.5015(2) 0.57845(19) 0.0235(4) Uani 1 1 d . . H12A H 1.2520 1.5345 0.5060 0.035 Uiso 1 1 calc R U H12B H 1.3673 1.4132 0.5417 0.035 Uiso 1 1 calc R U H12C H 1.4139 1.5830 0.6360 0.035 Uiso 1 1 calc R U N1 N 0.62815(19) 0.89002(16) 0.27779(13) 0.0150(3) Uani 1 1 d . . N2 N 0.87047(19) 1.13719(16) 0.39591(13) 0.0154(3) Uani 1 1 d . . N3 N 0.56549(19) 0.86706(16) 0.53549(13) 0.0165(3) Uani 1 1 d . . N4 N 0.62008(19) 0.85705(16) 0.64414(14) 0.0164(3) Uani 1 1 d . . N5 N 0.6673(2) 0.8432(2) 0.74759(15) 0.0275(3) Uani 1 1 d . . O1 O 0.84112(17) 1.12360(14) 0.64585(11) 0.0185(2) Uani 1 1 d . . O2 O 1.1759(2) 1.54975(15) 0.76575(13) 0.0270(3) Uani 1 1 d . . O71 O 0.7958(3) 1.5743(3) 0.7985(3) 0.0748(7) Uani 1 1 d . . Cu1 Cu 0.71578(3) 1.01076(2) 0.46768(2) 0.01348(7) 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 0.0164(7) 0.0172(8) 0.0179(8) 0.0015(6) 0.0037(6) 0.0001(6) C2 0.0176(8) 0.0211(8) 0.0200(8) -0.0018(7) 0.0012(6) -0.0007(6) C3 0.0214(8) 0.0266(9) 0.0136(7) -0.0012(6) -0.0006(6) 0.0034(7) C4 0.0225(8) 0.0239(8) 0.0138(7) 0.0035(6) 0.0029(6) 0.0043(7) C5 0.0157(7) 0.0162(7) 0.0141(7) 0.0030(6) 0.0027(6) 0.0025(6) C6 0.0231(8) 0.0201(8) 0.0124(7) 0.0034(6) 0.0038(6) -0.0029(6) C7 0.0140(7) 0.0153(7) 0.0176(7) 0.0047(6) 0.0045(6) 0.0015(6) C8 0.0126(7) 0.0147(7) 0.0172(7) 0.0018(6) 0.0016(6) 0.0002(6) C9 0.0129(7) 0.0176(7) 0.0151(7) 0.0013(6) 0.0010(6) 0.0029(6) C10 0.0213(8) 0.0272(9) 0.0139(7) 0.0018(7) 0.0005(6) -0.0003(7) C11 0.0164(7) 0.0167(8) 0.0209(8) 0.0035(6) 0.0001(6) 0.0015(6) C12 0.0194(8) 0.0184(8) 0.0295(9) 0.0042(7) 0.0055(7) -0.0026(6) N1 0.0148(6) 0.0155(6) 0.0132(6) 0.0024(5) 0.0025(5) 0.0019(5) N2 0.0170(6) 0.0155(6) 0.0120(6) 0.0026(5) 0.0032(5) 0.0002(5) N3 0.0177(6) 0.0166(6) 0.0140(6) 0.0048(5) 0.0021(5) -0.0004(5) N4 0.0162(6) 0.0150(6) 0.0175(7) 0.0045(5) 0.0049(5) 0.0005(5) N5 0.0317(8) 0.0326(9) 0.0189(7) 0.0126(7) 0.0027(6) 0.0015(7) O1 0.0188(5) 0.0197(6) 0.0135(5) 0.0033(4) 0.0014(4) -0.0029(5) O2 0.0322(7) 0.0189(6) 0.0219(6) -0.0020(5) 0.0031(5) -0.0031(5) O71 0.0629(14) 0.0681(15) 0.114(2) 0.0487(15) 0.0334(14) 0.0219(12) Cu1 0.01417(10) 0.01413(11) 0.01025(10) 0.00243(7) 0.00222(7) -0.00109(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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N1 C1 C2 122.06(15) N1 C1 H1 119.0 C2 C1 H1 119.0 C1 C2 C3 118.78(16) C1 C2 H2 120.6 C3 C2 H2 120.6 C4 C3 C2 119.18(16) C4 C3 H3 120.4 C2 C3 H3 120.4 C3 C4 C5 119.13(16) C3 C4 H4 120.4 C5 C4 H4 120.4 N1 C5 C4 121.82(15) N1 C5 C6 116.47(14) C4 C5 C6 121.69(15) N2 C6 C5 109.67(13) 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 126.77(15) N2 C7 H7 116.6 C8 C7 H7 116.6 C7 C8 C9 121.63(14) C7 C8 C11 117.38(14) C9 C8 C11 120.99(15) O1 C9 C8 123.21(15) O1 C9 C10 113.96(14) C8 C9 C10 122.74(15) 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 C8 122.42(16) O2 C11 C12 118.50(16) C8 C11 C12 119.08(15) C11 C12 H12A 109.5 C11 C12 H12B 109.5 H12A C12 H12B 109.5 C11 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C5 N1 C1 119.00(14) C5 N1 Cu1 114.35(11) C1 N1 Cu1 126.59(11) C7 N2 C6 117.90(14) C7 N2 Cu1 126.12(11) C6 N2 Cu1 115.98(11) N4 N3 Cu1 119.47(11) N5 N4 N3 177.56(17) C9 O1 Cu1 130.27(11) N2 Cu1 O1 91.22(5) N2 Cu1 N3 175.52(6) O1 Cu1 N3 90.56(5) N2 Cu1 N1 83.21(6) O1 Cu1 N1 170.48(5) N3 Cu1 N1 94.46(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance C1 N1 1.350(2) C1 C2 1.381(2) C1 H1 0.9500 C2 C3 1.392(3) C2 H2 0.9500 C3 C4 1.381(3) C3 H3 0.9500 C4 C5 1.387(2) C4 H4 0.9500 C5 N1 1.345(2) C5 C6 1.506(2) C6 N2 1.463(2) C6 H6A 0.9900 C6 H6B 0.9900 C7 N2 1.299(2) C7 C8 1.422(2) C7 H7 0.9500 C8 C9 1.423(2) C8 C11 1.470(2) C9 O1 1.270(2) C9 C10 1.508(2) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C11 O2 1.227(2) C11 C12 1.512(2) C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 N1 Cu1 1.9973(14) N2 Cu1 1.9233(13) N3 N4 1.200(2) N3 Cu1 1.9867(14) N4 N5 1.153(2) O1 Cu1 1.9266(12) 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 -1.5(3) C1 C2 C3 C4 1.5(3) C2 C3 C4 C5 -0.3(3) C3 C4 C5 N1 -1.1(3) C3 C4 C5 C6 177.35(16) N1 C5 C6 N2 -1.9(2) C4 C5 C6 N2 179.55(16) N2 C7 C8 C9 7.6(3) N2 C7 C8 C11 -172.63(16) C7 C8 C9 O1 -1.4(3) C11 C8 C9 O1 178.80(15) C7 C8 C9 C10 174.87(16) C11 C8 C9 C10 -4.9(3) C7 C8 C11 O2 154.96(17) C9 C8 C11 O2 -25.2(3) C7 C8 C11 C12 -24.8(2) C9 C8 C11 C12 155.06(16) C4 C5 N1 C1 1.2(2) C6 C5 N1 C1 -177.35(15) C4 C5 N1 Cu1 -176.13(13) C6 C5 N1 Cu1 5.32(19) C2 C1 N1 C5 0.1(3) C2 C1 N1 Cu1 177.10(13) C8 C7 N2 C6 176.68(16) C8 C7 N2 Cu1 -4.1(3) C5 C6 N2 C7 176.76(15) C5 C6 N2 Cu1 -2.57(18) C8 C9 O1 Cu1 -7.8(2) C10 C9 O1 Cu1 175.65(12)