#------------------------------------------------------------------------------ #$Date: 2024-09-06 03:52:59 +0300 (Fri, 06 Sep 2024) $ #$Revision: 294573 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/66/7716687.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_7716687 loop_ _publ_author_name 'Deng, Qing-Song' 'Zhang, Yu-Shuang' 'Wang, Ye-Xin' 'Xie, Yi' 'Fu, Peng-Xiang' 'Gao, Song' 'Liu, Zheng' 'Jiang, Shang-Da' _publ_section_title ; Orthogonal magnetic orbitals in high spin Cu-VO units: structure, magnetism and EPR study of anisotropic heterometallic complexes. ; _journal_issue 31 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 13207 _journal_page_last 13215 _journal_paper_doi 10.1039/d4dt01346h _journal_volume 53 _journal_year 2024 _chemical_formula_moiety 'C40 H32 Cu2 N4 O14 V2' _chemical_formula_sum 'C40 H32 Cu2 N4 O14 V2' _chemical_formula_weight 1021.65 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2023-08-31 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2023-09-05 deposited with the CCDC. 2024-07-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.576(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.1187(8) _cell_length_b 10.8875(4) _cell_length_c 18.4955(7) _cell_measurement_reflns_used 6108 _cell_measurement_temperature 303.58(17) _cell_measurement_theta_max 30.7900 _cell_measurement_theta_min 2.1400 _cell_volume 3817.1(3) _computing_cell_refinement 'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_environment air _diffrn_ambient_temperature 303.58(17) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.807 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -63.00 17.00 0.50 4.57 -- -4.92 0.00 60.00 160 2 \w -16.00 27.00 0.50 4.57 -- -4.92 -99.00 60.00 86 3 \w 0.00 34.00 0.50 4.57 -- 3.98 -99.00 -90.00 68 4 \w -61.00 -5.00 0.50 4.57 -- 3.98 -57.00-120.00 112 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0080965000 _diffrn_orient_matrix_UB_12 0.0611549000 _diffrn_orient_matrix_UB_13 -0.0133045000 _diffrn_orient_matrix_UB_21 0.0079560000 _diffrn_orient_matrix_UB_22 -0.0146227000 _diffrn_orient_matrix_UB_23 -0.0335483000 _diffrn_orient_matrix_UB_31 -0.0356595000 _diffrn_orient_matrix_UB_32 -0.0171477000 _diffrn_orient_matrix_UB_33 -0.0187850000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.807 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 14216 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.807 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.837 _diffrn_reflns_theta_min 2.149 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.653 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.66266 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.30a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.778 _exptl_crystal_description block _exptl_crystal_F_000 2064 _refine_diff_density_max 0.392 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 282 _refine_ls_number_reflns 4840 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0390 _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^)+(0.0542P)^2^+4.3266P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0993 _refine_ls_wR_factor_ref 0.1088 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3619 _reflns_number_total 4840 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4dt01346h2.cif _cod_data_source_block 8-14-t4-z_auto _cod_depositor_comments 'Adding full bibliography for 7716686--7716689.cif.' _cod_database_code 7716687 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula CHONCuV _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. ; _reflns_odcompleteness_completeness 99.90 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C10(H10A,H10B), C11(H11A,H11B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C12(H12), C8(H8), C9(H9), C14(H14), C17(H17) 2.c Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C16(H16A,H16B,H16C) ; _shelx_res_file ; TITL 8-14-t4-z_auto_a.res in C2/c 8-14-t4-z_auto.res created by SHELXL-2018/3 at 10:08:22 on 31-Aug-2023 REM Old TITL 8-14-t4-z_auto in C2/c REM SHELXT solution in C2/c: R1 0.138, Rweak 0.007, Alpha 0.026 REM 0.605 for 217 systematic absences, Orientation as input REM Formula found by SHELXT: C20 N2 O7 V1 Cu1 CELL 0.71073 20.1187 10.8875 18.4955 90 109.576 90 ZERR 4 0.0008 0.0004 0.0007 0 0.004 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cu N O V UNIT 160 128 8 16 56 8 L.S. 10 PLAN 5 TEMP 30 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta REM REM REM WGHT 0.054200 4.326600 FVAR 0.17124 CU1 3 0.386720 0.355634 0.570398 11.00000 0.06117 0.05012 = 0.03428 0.00114 0.02460 -0.01111 V1 6 0.364621 0.438806 0.408052 11.00000 0.04361 0.04602 = 0.03423 0.00487 0.01604 -0.00601 O3 5 0.431823 0.555385 0.391999 11.00000 0.05436 0.05339 = 0.03967 -0.00007 0.02345 -0.01303 O1 5 0.402783 0.494871 0.516001 11.00000 0.06998 0.04348 = 0.03578 -0.00187 0.02516 -0.01339 O2 5 0.355656 0.292504 0.467274 11.00000 0.06583 0.04441 = 0.03365 0.00125 0.02035 -0.01271 O4 5 0.377332 0.325682 0.333555 11.00000 0.06389 0.05429 = 0.04139 0.00050 0.02490 -0.00870 O5 5 0.498069 0.719333 0.402897 11.00000 0.05772 0.05081 = 0.06153 0.00711 0.03203 -0.00800 O6 5 0.362164 0.162319 0.259930 11.00000 0.08536 0.07064 = 0.04079 -0.00773 0.02514 -0.00759 O7 5 0.288705 0.496128 0.370430 11.00000 0.04885 0.06870 = 0.07120 0.01551 0.02032 -0.00046 N1 4 0.390979 0.444622 0.660199 11.00000 0.05732 0.06236 = 0.03583 0.00145 0.02373 -0.00401 N2 4 0.353961 0.219085 0.612562 11.00000 0.05398 0.05917 = 0.04027 0.00925 0.02431 -0.00468 C20 1 0.338345 0.176179 0.446143 11.00000 0.03587 0.04260 = 0.04226 0.00364 0.01125 -0.00491 C5 1 0.460804 0.654030 0.427811 11.00000 0.03925 0.04319 = 0.04392 0.00795 0.01390 -0.00069 C6 1 0.425671 0.605738 0.544853 11.00000 0.04123 0.04508 = 0.03888 -0.00012 0.01493 -0.00068 C4 1 0.450854 0.688879 0.502526 11.00000 0.03940 0.04462 = 0.04288 0.00383 0.01359 0.00054 C3 1 0.471571 0.806657 0.532052 11.00000 0.04393 0.04482 = 0.05526 0.00352 0.01343 0.00026 AFIX 43 H3 2 0.488702 0.861229 0.503827 11.00000 -1.20000 AFIX 0 C13 1 0.321954 0.093792 0.497587 11.00000 0.03852 0.04786 = 0.04638 0.00682 0.01462 -0.00573 C18 1 0.336675 0.135113 0.374060 11.00000 0.03758 0.04893 = 0.03912 -0.00041 0.00802 -0.00097 C7 1 0.424942 0.639841 0.618476 11.00000 0.04613 0.05142 = 0.04216 -0.00465 0.01781 -0.00002 C19 1 0.359407 0.211474 0.317905 11.00000 0.04459 0.05850 = 0.03403 0.00219 0.01062 0.00161 C12 1 0.328921 0.121450 0.577065 11.00000 0.04735 0.05562 = 0.05362 0.01209 0.02540 -0.00897 AFIX 43 H12 2 0.313555 0.061881 0.603879 11.00000 -1.20000 AFIX 0 C2 1 0.467368 0.844470 0.601934 11.00000 0.04507 0.04627 = 0.05835 -0.00611 0.01250 0.00317 C8 1 0.444646 0.759657 0.643713 11.00000 0.04916 0.05481 = 0.04867 -0.01009 0.01595 0.00406 AFIX 43 H8 2 0.442293 0.783295 0.691114 11.00000 -1.20000 AFIX 0 C9 1 0.404965 0.559350 0.671090 11.00000 0.05668 0.06490 = 0.03621 -0.00639 0.02082 -0.00112 AFIX 43 H9 2 0.402198 0.594117 0.715923 11.00000 -1.20000 AFIX 0 C14 1 0.300505 -0.025326 0.471506 11.00000 0.05075 0.04849 = 0.06475 0.00990 0.01732 -0.00875 AFIX 43 H14 2 0.288441 -0.079029 0.504205 11.00000 -1.20000 AFIX 0 C17 1 0.315351 0.013781 0.352505 11.00000 0.04960 0.05404 = 0.05335 -0.00741 0.01462 -0.00196 AFIX 43 H17 2 0.313980 -0.013212 0.304320 11.00000 -1.20000 AFIX 0 C15 1 0.296389 -0.066995 0.399481 11.00000 0.05006 0.04577 = 0.06935 -0.00276 0.01363 -0.00573 C1 1 0.488647 0.972593 0.632415 11.00000 0.06633 0.05119 = 0.07732 -0.01243 0.01404 0.00257 AFIX 137 H1A 2 0.539130 0.977527 0.653749 11.00000 -1.50000 H1B 2 0.468556 0.990795 0.671517 11.00000 -1.50000 H1C 2 0.471767 1.030821 0.591335 11.00000 -1.50000 AFIX 0 C10 1 0.366545 0.369994 0.713709 11.00000 0.09908 0.08447 = 0.04662 0.00411 0.04096 -0.00809 AFIX 23 H10A 2 0.397679 0.383338 0.765929 11.00000 -1.20000 H10B 2 0.319469 0.395778 0.710419 11.00000 -1.20000 AFIX 0 C11 1 0.365768 0.238705 0.694835 11.00000 0.10241 0.07849 = 0.04270 0.00923 0.03749 -0.01205 AFIX 23 H11A 2 0.328721 0.198052 0.708465 11.00000 -1.20000 H11B 2 0.410422 0.202038 0.724900 11.00000 -1.20000 AFIX 0 C16 1 0.273751 -0.197561 0.374631 11.00000 0.08947 0.05191 = 0.09635 -0.01106 0.02749 -0.01771 AFIX 137 H16A 2 0.311042 -0.239307 0.363134 11.00000 -1.50000 H16B 2 0.232268 -0.196189 0.329748 11.00000 -1.50000 H16C 2 0.263608 -0.239850 0.415278 11.00000 -1.50000 AFIX 0 HKLF 4 REM 8-14-t4-z_auto_a.res in C2/c REM wR2 = 0.1088, GooF = S = 1.017, Restrained GooF = 1.017 for all data REM R1 = 0.0390 for 3619 Fo > 4sig(Fo) and 0.0578 for all 4840 data REM 282 parameters refined using 0 restraints END WGHT 0.0542 4.3263 REM Highest difference peak 0.392, deepest hole -0.269, 1-sigma level 0.069 Q1 1 0.4422 0.3527 0.5994 11.00000 0.05 0.39 Q2 1 0.3370 0.3576 0.5675 11.00000 0.05 0.37 Q3 1 0.4035 0.4053 0.4359 11.00000 0.05 0.35 Q4 1 0.4070 0.3466 0.7187 11.00000 0.05 0.35 Q5 1 0.3109 0.4430 0.4057 11.00000 0.05 0.30 ; _shelx_res_checksum 66792 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.530 _oxdiff_exptl_absorpt_empirical_full_min 0.723 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.38672(2) 0.35563(3) 0.57040(2) 0.04636(12) Uani 1 1 d . . . . . V1 V 0.36462(2) 0.43881(4) 0.40805(2) 0.04053(13) Uani 1 1 d . . . . . O3 O 0.43182(10) 0.55538(17) 0.39200(10) 0.0472(4) Uani 1 1 d . . . . . O1 O 0.40278(10) 0.49487(17) 0.51600(10) 0.0479(4) Uani 1 1 d . . . . . O2 O 0.35566(10) 0.29250(17) 0.46727(10) 0.0470(4) Uani 1 1 d . . . . . O4 O 0.37733(11) 0.32568(19) 0.33356(11) 0.0514(5) Uani 1 1 d . . . . . O5 O 0.49807(10) 0.71933(18) 0.40290(12) 0.0537(5) Uani 1 1 d . . . . . O6 O 0.36216(13) 0.1623(2) 0.25993(12) 0.0646(6) Uani 1 1 d . . . . . O7 O 0.28871(10) 0.4961(2) 0.37043(13) 0.0629(6) Uani 1 1 d . . . . . N1 N 0.39098(12) 0.4446(2) 0.66020(12) 0.0498(6) Uani 1 1 d . . . . . N2 N 0.35396(12) 0.2191(2) 0.61256(13) 0.0490(5) Uani 1 1 d . . . . . C20 C 0.33834(13) 0.1762(2) 0.44614(15) 0.0407(5) Uani 1 1 d . . . . . C5 C 0.46080(13) 0.6540(2) 0.42781(15) 0.0421(6) Uani 1 1 d . . . . . C6 C 0.42567(13) 0.6057(2) 0.54485(14) 0.0413(5) Uani 1 1 d . . . . . C4 C 0.45085(13) 0.6889(2) 0.50253(15) 0.0423(5) Uani 1 1 d . . . . . C3 C 0.47157(14) 0.8067(3) 0.53205(17) 0.0488(6) Uani 1 1 d . . . . . H3 H 0.488702 0.861229 0.503827 0.059 Uiso 1 1 calc R U . . . C13 C 0.32195(13) 0.0938(3) 0.49759(15) 0.0442(6) Uani 1 1 d . . . . . C18 C 0.33668(13) 0.1351(2) 0.37406(15) 0.0431(6) Uani 1 1 d . . . . . C7 C 0.42494(14) 0.6398(3) 0.61848(15) 0.0458(6) Uani 1 1 d . . . . . C19 C 0.35941(14) 0.2115(3) 0.31790(15) 0.0464(6) Uani 1 1 d . . . . . C12 C 0.32892(14) 0.1215(3) 0.57706(17) 0.0501(7) Uani 1 1 d . . . . . H12 H 0.313555 0.061881 0.603879 0.060 Uiso 1 1 calc R U . . . C2 C 0.46737(15) 0.8445(3) 0.60193(18) 0.0511(6) Uani 1 1 d . . . . . C8 C 0.44465(14) 0.7597(3) 0.64371(17) 0.0510(6) Uani 1 1 d . . . . . H8 H 0.442293 0.783295 0.691114 0.061 Uiso 1 1 calc R U . . . C9 C 0.40497(15) 0.5594(3) 0.67109(15) 0.0513(7) Uani 1 1 d . . . . . H9 H 0.402198 0.594117 0.715923 0.062 Uiso 1 1 calc R U . . . C14 C 0.30050(15) -0.0253(3) 0.47151(18) 0.0552(7) Uani 1 1 d . . . . . H14 H 0.288441 -0.079029 0.504205 0.066 Uiso 1 1 calc R U . . . C17 C 0.31535(14) 0.0138(3) 0.35250(17) 0.0530(7) Uani 1 1 d . . . . . H17 H 0.313980 -0.013212 0.304320 0.064 Uiso 1 1 calc R U . . . C15 C 0.29639(15) -0.0670(3) 0.3995(2) 0.0567(7) Uani 1 1 d . . . . . C1 C 0.48865(18) 0.9726(3) 0.6324(2) 0.0675(9) Uani 1 1 d . . . . . H1A H 0.539130 0.977527 0.653749 0.101 Uiso 1 1 calc R U . . . H1B H 0.468556 0.990795 0.671517 0.101 Uiso 1 1 calc R U . . . H1C H 0.471767 1.030821 0.591335 0.101 Uiso 1 1 calc R U . . . C10 C 0.3665(2) 0.3700(3) 0.71371(19) 0.0726(10) Uani 1 1 d . . . . . H10A H 0.397679 0.383338 0.765929 0.087 Uiso 1 1 calc R U . . . H10B H 0.319469 0.395778 0.710419 0.087 Uiso 1 1 calc R U . . . C11 C 0.3658(2) 0.2387(3) 0.69484(18) 0.0712(10) Uani 1 1 d . . . . . H11A H 0.328721 0.198052 0.708465 0.085 Uiso 1 1 calc R U . . . H11B H 0.410422 0.202038 0.724900 0.085 Uiso 1 1 calc R U . . . C16 C 0.2738(2) -0.1976(3) 0.3746(2) 0.0802(11) Uani 1 1 d . . . . . H16A H 0.311042 -0.239307 0.363134 0.120 Uiso 1 1 calc R U . . . H16B H 0.232268 -0.196189 0.329748 0.120 Uiso 1 1 calc R U . . . H16C H 0.263608 -0.239850 0.415278 0.120 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 0.0612(2) 0.0501(2) 0.03428(17) 0.00114(13) 0.02460(15) -0.01111(15) V1 0.0436(2) 0.0460(2) 0.0342(2) 0.00487(18) 0.01604(18) -0.00601(18) O3 0.0544(10) 0.0534(11) 0.0397(9) -0.0001(8) 0.0235(8) -0.0130(8) O1 0.0700(12) 0.0435(10) 0.0358(9) -0.0019(8) 0.0252(9) -0.0134(9) O2 0.0658(11) 0.0444(10) 0.0336(9) 0.0013(7) 0.0204(8) -0.0127(8) O4 0.0639(12) 0.0543(11) 0.0414(10) 0.0005(9) 0.0249(9) -0.0087(9) O5 0.0577(11) 0.0508(11) 0.0615(12) 0.0071(9) 0.0320(10) -0.0080(9) O6 0.0854(15) 0.0706(14) 0.0408(11) -0.0077(10) 0.0251(11) -0.0076(12) O7 0.0488(11) 0.0687(14) 0.0712(14) 0.0155(11) 0.0203(10) -0.0005(10) N1 0.0573(14) 0.0624(15) 0.0358(11) 0.0014(10) 0.0237(10) -0.0040(11) N2 0.0540(13) 0.0592(14) 0.0403(11) 0.0092(10) 0.0243(10) -0.0047(11) C20 0.0359(12) 0.0426(13) 0.0423(13) 0.0036(11) 0.0112(10) -0.0049(10) C5 0.0392(12) 0.0432(14) 0.0439(13) 0.0079(11) 0.0139(11) -0.0007(10) C6 0.0412(13) 0.0451(13) 0.0389(13) -0.0001(11) 0.0149(10) -0.0007(10) C4 0.0394(12) 0.0446(14) 0.0429(13) 0.0038(11) 0.0136(11) 0.0005(10) C3 0.0439(14) 0.0448(14) 0.0553(16) 0.0035(12) 0.0134(12) 0.0003(11) C13 0.0385(13) 0.0479(14) 0.0464(14) 0.0068(12) 0.0146(11) -0.0057(11) C18 0.0376(12) 0.0489(14) 0.0391(13) -0.0004(11) 0.0080(10) -0.0010(10) C7 0.0461(14) 0.0514(15) 0.0422(13) -0.0046(12) 0.0178(11) 0.0000(11) C19 0.0446(14) 0.0585(17) 0.0340(12) 0.0022(12) 0.0106(11) 0.0016(12) C12 0.0474(14) 0.0556(17) 0.0536(16) 0.0121(13) 0.0254(13) -0.0090(12) C2 0.0451(14) 0.0463(15) 0.0583(17) -0.0061(13) 0.0125(13) 0.0032(11) C8 0.0492(15) 0.0548(16) 0.0487(15) -0.0101(13) 0.0160(12) 0.0041(12) C9 0.0567(16) 0.0649(19) 0.0362(13) -0.0064(12) 0.0208(12) -0.0011(13) C14 0.0507(15) 0.0485(16) 0.0648(18) 0.0099(14) 0.0173(14) -0.0088(12) C17 0.0496(15) 0.0540(17) 0.0534(16) -0.0074(13) 0.0146(13) -0.0020(12) C15 0.0501(16) 0.0458(16) 0.069(2) -0.0028(14) 0.0136(14) -0.0057(12) C1 0.066(2) 0.0512(18) 0.077(2) -0.0124(16) 0.0140(17) 0.0026(15) C10 0.099(3) 0.084(3) 0.0466(17) 0.0041(16) 0.0410(18) -0.008(2) C11 0.102(3) 0.078(2) 0.0427(16) 0.0092(16) 0.0375(17) -0.012(2) C16 0.089(3) 0.052(2) 0.096(3) -0.0111(19) 0.027(2) -0.0177(18) 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' Cu Cu 0.3201 1.2651 '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' V V 0.3005 0.5294 '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 O1 Cu1 V1 39.82(5) . . ? O1 Cu1 O2 79.46(7) . . ? O1 Cu1 O5 93.30(8) . 5_666 ? O2 Cu1 V1 39.79(5) . . ? O2 Cu1 O5 93.11(8) . 5_666 ? O5 Cu1 V1 96.85(5) 5_666 . ? N1 Cu1 V1 131.62(8) . . ? N1 Cu1 O1 95.16(9) . . ? N1 Cu1 O2 162.43(10) . . ? N1 Cu1 O5 103.95(9) . 5_666 ? N2 Cu1 V1 133.43(7) . . ? N2 Cu1 O1 169.82(9) . . ? N2 Cu1 O2 94.90(9) . . ? N2 Cu1 O5 95.48(9) . 5_666 ? N2 Cu1 N1 87.73(10) . . ? O3 V1 Cu1 117.90(6) . . ? O3 V1 O1 84.17(7) . . ? O3 V1 O2 143.78(8) . . ? O1 V1 Cu1 38.05(5) . . ? O2 V1 Cu1 38.56(5) . . ? O2 V1 O1 76.47(7) . . ? O4 V1 Cu1 120.52(6) . . ? O4 V1 O3 92.42(8) . . ? O4 V1 O1 144.89(9) . . ? O4 V1 O2 86.55(8) . . ? O7 V1 Cu1 110.77(8) . . ? O7 V1 O3 107.06(10) . . ? O7 V1 O1 108.27(11) . . ? O7 V1 O2 107.97(10) . . ? O7 V1 O4 106.13(11) . . ? C5 O3 V1 132.81(17) . . ? Cu1 O1 V1 102.12(8) . . ? C6 O1 Cu1 127.14(16) . . ? C6 O1 V1 130.22(16) . . ? Cu1 O2 V1 101.65(8) . . ? C20 O2 Cu1 126.48(16) . . ? C20 O2 V1 131.69(16) . . ? C19 O4 V1 132.60(17) . . ? C5 O5 Cu1 113.77(17) . 5_666 ? C9 N1 Cu1 125.29(19) . . ? C9 N1 C10 122.2(3) . . ? C10 N1 Cu1 112.0(2) . . ? C12 N2 Cu1 125.41(19) . . ? C12 N2 C11 123.8(2) . . ? C11 N2 Cu1 110.6(2) . . ? O2 C20 C13 119.8(2) . . ? O2 C20 C18 120.2(2) . . ? C18 C20 C13 120.0(2) . . ? O3 C5 C4 120.1(2) . . ? O5 C5 O3 121.0(2) . . ? O5 C5 C4 118.8(2) . . ? O1 C6 C4 120.1(2) . . ? O1 C6 C7 120.5(2) . . ? C4 C6 C7 119.4(3) . . ? C6 C4 C5 122.3(2) . . ? C6 C4 C3 119.4(2) . . ? C3 C4 C5 118.3(2) . . ? C4 C3 H3 118.9 . . ? C2 C3 C4 122.2(3) . . ? C2 C3 H3 118.9 . . ? C20 C13 C12 125.2(3) . . ? C14 C13 C20 117.8(3) . . ? C14 C13 C12 116.9(2) . . ? C20 C18 C19 124.2(2) . . ? C20 C18 C17 118.7(2) . . ? C17 C18 C19 117.1(2) . . ? C6 C7 C9 125.2(3) . . ? C8 C7 C6 118.2(3) . . ? C8 C7 C9 116.6(2) . . ? O4 C19 C18 119.8(2) . . ? O6 C19 O4 121.7(3) . . ? O6 C19 C18 118.4(3) . . ? N2 C12 C13 125.7(2) . . ? N2 C12 H12 117.1 . . ? C13 C12 H12 117.1 . . ? C3 C2 C1 121.6(3) . . ? C8 C2 C3 117.4(3) . . ? C8 C2 C1 121.0(3) . . ? C7 C8 H8 118.3 . . ? C2 C8 C7 123.3(3) . . ? C2 C8 H8 118.3 . . ? N1 C9 C7 125.1(2) . . ? N1 C9 H9 117.5 . . ? C7 C9 H9 117.5 . . ? C13 C14 H14 118.4 . . ? C15 C14 C13 123.2(3) . . ? C15 C14 H14 118.4 . . ? C18 C17 H17 118.5 . . ? C15 C17 C18 123.0(3) . . ? C15 C17 H17 118.5 . . ? C14 C15 C16 121.0(3) . . ? C17 C15 C14 117.3(3) . . ? C17 C15 C16 121.7(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? C11 C10 N1 110.7(3) . . ? C11 C10 H10A 109.5 . . ? C11 C10 H10B 109.5 . . ? N2 C11 H11A 109.3 . . ? N2 C11 H11B 109.3 . . ? C10 C11 N2 111.8(3) . . ? C10 C11 H11A 109.3 . . ? C10 C11 H11B 109.3 . . ? H11A C11 H11B 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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 V1 3.0231(5) . ? Cu1 O1 1.9059(17) . ? Cu1 O2 1.9241(18) . ? Cu1 O5 2.349(2) 5_666 ? Cu1 N1 1.900(2) . ? Cu1 N2 1.897(2) . ? V1 O3 1.9484(17) . ? V1 O1 1.9802(18) . ? V1 O2 1.9753(18) . ? V1 O4 1.928(2) . ? V1 O7 1.579(2) . ? O3 C5 1.294(3) . ? O1 C6 1.338(3) . ? O2 C20 1.337(3) . ? O4 C19 1.300(3) . ? O5 C5 1.229(3) . ? O6 C19 1.216(3) . ? N1 C9 1.281(4) . ? N1 C10 1.486(4) . ? N2 C12 1.262(4) . ? N2 C11 1.475(4) . ? C20 C13 1.424(3) . ? C20 C18 1.396(4) . ? C5 C4 1.510(4) . ? C6 C4 1.398(4) . ? C6 C7 1.416(4) . ? C4 C3 1.401(4) . ? C3 H3 0.9300 . ? C3 C2 1.386(4) . ? C13 C12 1.461(4) . ? C13 C14 1.400(4) . ? C18 C19 1.516(4) . ? C18 C17 1.405(4) . ? C7 C8 1.397(4) . ? C7 C9 1.462(4) . ? C12 H12 0.9300 . ? C2 C8 1.377(4) . ? C2 C1 1.512(4) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C14 H14 0.9300 . ? C14 C15 1.383(5) . ? C17 H17 0.9300 . ? C17 C15 1.377(4) . ? C15 C16 1.516(4) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.470(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 O1 C6 C4 164.64(18) . . . . ? Cu1 O1 C6 C7 -15.1(4) . . . . ? Cu1 O2 C20 C13 18.4(3) . . . . ? Cu1 O2 C20 C18 -161.23(18) . . . . ? Cu1 O5 C5 O3 -79.4(3) 5_666 . . . ? Cu1 O5 C5 C4 98.9(2) 5_666 . . . ? Cu1 N1 C9 C7 -4.5(4) . . . . ? Cu1 N1 C10 C11 16.9(4) . . . . ? Cu1 N2 C12 C13 1.6(4) . . . . ? Cu1 N2 C11 C10 27.2(4) . . . . ? V1 Cu1 N1 C9 -21.4(3) . . . . ? V1 Cu1 N1 C10 150.8(2) . . . . ? V1 Cu1 N2 C12 18.0(3) . . . . ? V1 Cu1 N2 C11 -165.59(18) . . . . ? V1 O3 C5 O5 -173.93(19) . . . . ? V1 O3 C5 C4 7.8(4) . . . . ? V1 O1 C6 C4 -25.1(4) . . . . ? V1 O1 C6 C7 155.20(19) . . . . ? V1 O2 C20 C13 -167.32(18) . . . . ? V1 O2 C20 C18 13.0(4) . . . . ? V1 O4 C19 O6 167.6(2) . . . . ? V1 O4 C19 C18 -14.5(4) . . . . ? O3 C5 C4 C6 15.5(4) . . . . ? O3 C5 C4 C3 -168.2(2) . . . . ? O1 Cu1 N1 C9 -3.5(3) . . . . ? O1 Cu1 N1 C10 168.7(2) . . . . ? O1 Cu1 N2 C12 62.6(6) . . . . ? O1 Cu1 N2 C11 -121.0(5) . . . . ? O1 C6 C4 C5 -6.7(4) . . . . ? O1 C6 C4 C3 177.1(2) . . . . ? O1 C6 C7 C8 -175.5(2) . . . . ? O1 C6 C7 C9 4.4(4) . . . . ? O2 Cu1 N1 C9 -74.6(4) . . . . ? O2 Cu1 N1 C10 97.6(4) . . . . ? O2 Cu1 N2 C12 6.8(3) . . . . ? O2 Cu1 N2 C11 -176.8(2) . . . . ? O2 C20 C13 C12 -6.4(4) . . . . ? O2 C20 C13 C14 176.7(2) . . . . ? O2 C20 C18 C19 5.3(4) . . . . ? O2 C20 C18 C17 -177.3(2) . . . . ? O5 Cu1 N1 C9 91.2(3) 5_666 . . . ? O5 Cu1 N1 C10 -96.6(2) 5_666 . . . ? O5 Cu1 N2 C12 -86.8(2) 5_666 . . . ? O5 Cu1 N2 C11 89.6(2) 5_666 . . . ? O5 C5 C4 C6 -162.8(2) . . . . ? O5 C5 C4 C3 13.4(4) . . . . ? N1 Cu1 N2 C12 169.4(3) . . . . ? N1 Cu1 N2 C11 -14.2(2) . . . . ? N1 C10 C11 N2 -28.4(4) . . . . ? N2 Cu1 N1 C9 -173.7(3) . . . . ? N2 Cu1 N1 C10 -1.5(2) . . . . ? C20 C13 C12 N2 -4.2(5) . . . . ? C20 C13 C14 C15 1.8(4) . . . . ? C20 C18 C19 O4 -5.0(4) . . . . ? C20 C18 C19 O6 173.0(3) . . . . ? C20 C18 C17 C15 -0.4(4) . . . . ? C5 C4 C3 C2 -177.0(2) . . . . ? C6 C4 C3 C2 -0.6(4) . . . . ? C6 C7 C8 C2 -2.7(4) . . . . ? C6 C7 C9 N1 6.0(5) . . . . ? C4 C6 C7 C8 4.8(4) . . . . ? C4 C6 C7 C9 -175.3(3) . . . . ? C4 C3 C2 C8 2.7(4) . . . . ? C4 C3 C2 C1 -178.9(3) . . . . ? C3 C2 C8 C7 -1.0(4) . . . . ? C13 C20 C18 C19 -174.3(2) . . . . ? C13 C20 C18 C17 3.0(4) . . . . ? C13 C14 C15 C17 0.8(4) . . . . ? C13 C14 C15 C16 179.2(3) . . . . ? C18 C20 C13 C12 173.2(3) . . . . ? C18 C20 C13 C14 -3.7(4) . . . . ? C18 C17 C15 C14 -1.5(4) . . . . ? C18 C17 C15 C16 -179.9(3) . . . . ? C7 C6 C4 C5 173.0(2) . . . . ? C7 C6 C4 C3 -3.2(4) . . . . ? C19 C18 C17 C15 177.1(3) . . . . ? C12 N2 C11 C10 -156.3(3) . . . . ? C12 C13 C14 C15 -175.4(3) . . . . ? C8 C7 C9 N1 -174.1(3) . . . . ? C9 N1 C10 C11 -170.6(3) . . . . ? C9 C7 C8 C2 177.4(3) . . . . ? C14 C13 C12 N2 172.7(3) . . . . ? C17 C18 C19 O4 177.6(2) . . . . ? C17 C18 C19 O6 -4.4(4) . . . . ? C1 C2 C8 C7 -179.5(3) . . . . ? C10 N1 C9 C7 -176.0(3) . . . . ? C11 N2 C12 C13 -174.4(3) . . . . ?