#------------------------------------------------------------------------------ #$Date: 2026-05-07 23:58:41 +0100 (Thu, 07 May 2026) $ #$Revision: 305892 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720993.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_7720993 loop_ _publ_author_name 'Vosegaard, Emilie' 'Mamakhel, Aref' 'Iversen, Bo Brummerstedt' _publ_section_title ; Hybrid organic-inorganic polyoxovanadates with [M(en) n ] (M=Co, Ni, Cu, Zn) displaying (V 4 O 13 ), (V 15 O 36 ) or (V 18 O 42 ) morphologies ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT00188B _journal_year 2026 _chemical_formula_moiety 'O42 V18, Cl, 4(C4 Cu N4), 4(O)' _chemical_formula_sum 'C16 Cl Cu4 N16 O46 V18' _chemical_formula_weight 2358.85 _space_group_crystal_system orthorhombic _space_group_IT_number 34 _space_group_name_Hall 'P 2 -2n' _space_group_name_H-M_alt 'P n n 2' _audit_creation_date 2026-03-18 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2026-03-19 deposited with the CCDC. 2026-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.7171(5) _cell_length_b 18.3850(5) _cell_length_c 14.7840(5) _cell_measurement_reflns_used 26403 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 27.0430 _cell_measurement_theta_min 2.2180 _cell_volume 4000.2(2) _computing_cell_refinement 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.115a (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 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 150.15 _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 100' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 -76.00 -51.00 1.00 120.00 -- -6.23 151.00 -56.00 25 2 \w -49.00 -11.00 1.00 120.00 -- -6.23 122.00 142.00 38 3 \w -5.00 81.00 1.00 120.00 -- 6.62 38.00 90.00 86 4 \w 22.00 63.00 1.00 120.00 -- 6.62 77.00 120.00 41 5 \w 9.00 35.00 1.00 120.00 -- 6.62 -99.00-120.00 26 6 \w 0.00 46.00 1.00 120.00 -- 6.62 -99.00 0.00 46 7 \w -19.00 7.00 1.00 120.00 -- 6.62 77.00 90.00 26 8 \w 16.00 62.00 1.00 120.00 -- 6.62 77.00 90.00 46 9 \w -19.00 51.00 1.00 120.00 -- 6.62 77.00-120.00 70 10 \w -55.00 -15.00 1.00 120.00 -- 6.62 -57.00 0.00 40 11 \w -7.00 26.00 1.00 120.00 -- 6.62 -57.00 0.00 33 12 \w -64.00 26.00 1.00 120.00 -- 6.62 -57.00 -60.00 90 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix-Arc 100' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0932 _diffrn_reflns_av_unetI/netI 0.0265 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 14113 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.344 _diffrn_reflns_theta_min 2.245 _exptl_absorpt_coefficient_mu 3.149 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86977 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.958 _exptl_crystal_description block _exptl_crystal_F_000 2246 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.176 _refine_diff_density_min -0.544 _refine_diff_density_rms 0.178 _refine_ls_abs_structure_details ; Flack x determined using 3052 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.24(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 457 _refine_ls_number_reflns 14113 _refine_ls_number_restraints 109 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0677 _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^)+(0.1482P)^2^+0.9536P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1807 _refine_ls_wR_factor_ref 0.1860 _reflns_Friedel_coverage 0.918 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 13167 _reflns_number_total 14113 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 89.6580\% around [0.00 1.00 -0.00] (reciprocal) or [-0.00 1.00 0.00] (direct) ; _cod_data_source_file d6dt00188b2.cif _cod_data_source_block cuv-1-2_150k_pnn2_twin_twin1_hklf4 _cod_database_code 7720993 _shelx_shelxl_version_number 2019/1 _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_estimated_absorpt_t_max 0.744 _shelx_estimated_absorpt_t_min 0.744 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.578(3) 0.422(3) 2. Restrained distances C2-Cu11 = Cu11-C4 = C5-Cu11 = Cu11-C10 2.8 with sigma of 0.02 N1-Cu11 = Cu11-N2 = N8-Cu11 = Cu11-N7 2.1 with sigma of 0.02 N8-C5 = N7-C10 1.5 with sigma of 0.02 N1-C2 = C4-N2 1.5 with sigma of 0.02 N6-C20 = N5-C9 = C1-N4 = C17-N3 2.1 with sigma of 0.02 C10-C5 = C20-C9 = C17-C1 1.5 with sigma of 0.02 N5-C20 = C9-N6 1.5 with sigma of 0.02 N4-C17 = N3-C1 1.5 with sigma of 0.02 Cu12-C17 = Cu12-C9 = Cu12-C1 = Cu12-C20 2.8 with sigma of 0.02 Cu12-N3 = Cu12-N5 = Cu12-N4 = Cu12-N6 2.1 with sigma of 0.02 C4-C2 1.5 with sigma of 0.02 N2-C2 = C4-N1 2.2 with sigma of 0.04 N7-C5 = C10-N8 2.1 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints N7 \\sim C10 \\sim C5 \\sim N8: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A N2 \\sim C4 \\sim C2 \\sim N1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C20 \\sim N5 \\sim C9 \\sim N6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A N4 \\sim N3 \\sim C17 \\sim C1: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A ; _shelx_res_file ; TITL CuV-1-2_150K_Pnn2_twin_twin1_hklf4 in Pnn2 #34 cuv-1-2_150k_pnn2_twin_twin1_hklf4.res created by SHELXL-2019/1 at 14:34:08 on 18-Mar-2026 CELL 0.71073 14.717104 18.384992 14.784038 90 90 90 ZERR 2 0.000546 0.000512 0.000481 0 0 0 LATT -1 SYMM -X,-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SYMM 0.5+X,0.5-Y,0.5+Z SFAC C Cl Cu N O V UNIT 32 2 8 32 92 36 DFIX 2.8 C2 Cu11 Cu11 C4 C5 Cu11 Cu11 C10 DFIX 2.1 N1 Cu11 Cu11 N2 N8 Cu11 Cu11 N7 DANG 2.2 N2 C2 C4 N1 DFIX 1.5 N8 C5 N7 C10 DFIX 1.5 N1 C2 C4 N2 DANG 2.1 N7 C5 C10 N8 SIMU N7 C10 C5 N8 SIMU N2 C4 C2 N1 SIMU C20 N5 C9 N6 SIMU N4 N3 C17 C1 DFIX 2.1 N6 C20 N5 C9 C1 N4 C17 N3 DFIX 1.5 C10 C5 C20 C9 C17 C1 DFIX 1.5 N5 C20 C9 N6 DFIX 1.5 N4 C17 N3 C1 DFIX 2.8 Cu12 C17 Cu12 C9 Cu12 C1 Cu12 C20 DFIX 2.1 Cu12 N3 Cu12 N5 Cu12 N4 Cu12 N6 DFIX 1.5 C4 C2 L.S. 10 PLAN 56 SIZE 0.1 0.1 0.1 TEMP -123 CONF MORE -1 fmap 2 53 acta SHEL 10 0.83 OMIT -3 0 -1 OMIT -3 0 1 OMIT -2 0 -2 OMIT -2 0 2 OMIT -1 0 -3 OMIT -1 0 3 OMIT 0 -2 0 OMIT 1 1 7 OMIT 10 -2 0 REM REM REM WGHT 0.148200 0.953600 BASF 0.42191 FVAR 0.14953 V6 6 0.900703 0.011045 0.680212 11.00000 0.04164 0.06423 = 0.02736 0.00248 0.00330 0.01041 V8 6 0.761645 0.012117 0.543329 11.00000 0.03430 0.06912 = 0.03717 0.00081 0.00730 0.00522 V4 6 0.762519 0.022375 0.346857 11.00000 0.03106 0.07877 = 0.03435 0.00714 -0.00252 -0.00304 V2 6 0.900760 0.001435 0.208318 11.00000 0.03626 0.05205 = 0.02556 0.00237 -0.00506 -0.00322 V3 6 0.820239 -0.127797 0.379076 11.00000 0.05428 0.04733 = 0.04247 -0.00100 0.00042 -0.02695 V7 6 0.919180 -0.135368 0.605675 11.00000 0.05416 0.04772 = 0.04181 0.01884 0.00857 -0.00701 V1 6 0.949916 0.145294 0.282232 11.00000 0.05401 0.03559 = 0.04000 0.01491 -0.00373 0.00342 V5 6 0.979554 -0.209332 0.443710 11.00000 0.07326 0.01921 = 0.05511 -0.00037 0.00813 -0.00179 V10 6 0.852971 0.152336 0.509448 11.00000 0.05642 0.04388 = 0.04245 -0.00494 -0.00141 0.02719 CL10 2 1.000000 0.000000 0.443122 10.50000 0.05732 0.05405 = 0.05820 0.00000 0.00000 0.00081 CU11 3 0.718652 -0.227618 0.192587 11.00000 0.11533 0.09362 = 0.06744 -0.02468 -0.00647 -0.05913 CU12 3 0.725804 -0.234732 0.692798 11.00000 0.10456 0.07047 = 0.07047 0.02144 0.02706 -0.03484 O1 5 1.010835 0.067196 0.677047 11.00000 0.05666 0.04769 = 0.03792 -0.01457 -0.00685 0.00933 O2 5 0.996782 -0.069115 0.211045 11.00000 0.05775 0.03665 = 0.02891 -0.01396 0.00767 -0.00320 O3 5 0.849337 0.079420 0.277797 11.00000 0.03320 0.04699 = 0.03365 0.01055 0.00279 -0.00143 O4 5 0.835816 0.079603 0.603776 11.00000 0.04830 0.05700 = 0.03017 -0.00258 0.01343 0.02167 O5 5 0.829882 -0.058184 0.609015 11.00000 0.04189 0.07092 = 0.02607 0.01127 0.01175 0.01195 O6 5 0.825686 -0.057178 0.284537 11.00000 0.05163 0.05421 = 0.02688 0.01008 0.00880 -0.02243 O8 5 0.759360 -0.049228 0.440566 11.00000 0.03546 0.07103 = 0.04070 -0.00668 0.00565 -0.01654 O10 5 0.905488 0.178524 0.397207 11.00000 0.08139 0.03425 = 0.03617 0.00184 0.00099 0.02191 O11 5 0.662171 0.032060 0.302006 11.00000 0.03159 0.16787 = 0.04662 0.02245 -0.01003 -0.00215 O13 5 0.868281 -0.163583 0.489795 11.00000 0.04325 0.02866 = 0.04067 0.00597 0.00686 -0.00709 O7 5 0.773319 0.085298 0.451112 11.00000 0.03850 0.06573 = 0.03934 -0.00411 -0.00919 0.00768 O9 5 0.660979 0.015754 0.585707 11.00000 0.05296 0.13246 = 0.05397 -0.01010 -0.01252 0.01385 O12 5 0.741138 -0.183100 0.349331 11.00000 0.08465 0.07874 = 0.08785 -0.02496 0.03420 -0.05262 O14 5 0.855954 0.003128 0.106772 11.00000 0.07597 0.08893 = 0.01842 0.00798 -0.02808 0.00283 O16 5 0.970290 0.174369 0.557239 11.00000 0.07201 0.02430 = 0.05497 -0.01256 0.00371 0.01335 O17 5 0.884992 -0.193694 0.679889 11.00000 0.09460 0.07150 = 0.06211 0.04166 0.01179 -0.01694 O18 5 0.855653 0.013733 0.780312 11.00000 0.05415 0.14015 = 0.03871 0.01712 0.01105 0.01446 O15 5 0.927885 0.211553 0.212547 11.00000 0.09466 0.06007 = 0.05273 0.02668 -0.01096 0.00609 O19 5 0.932663 -0.166301 0.335585 11.00000 0.06173 0.02959 = 0.06103 -0.00184 0.00472 -0.01981 O20 5 0.974999 -0.297119 0.441376 11.00000 0.13908 0.01594 = 0.08818 0.00647 0.01959 -0.01357 O21 5 0.792094 0.221763 0.536830 11.00000 0.10029 0.06775 = 0.05950 -0.01388 -0.02006 0.05618 N1 4 0.725841 -0.125535 0.132099 11.00000 0.31944 0.17270 = 0.12820 0.05148 -0.15692 -0.15547 N2 4 0.577943 -0.208577 0.196162 11.00000 0.07267 0.13975 = 0.16343 -0.05456 -0.01779 -0.04989 C5 1 0.824189 -0.338917 0.259253 11.00000 0.31305 0.09125 = 0.16903 -0.07107 -0.08023 0.00526 C10 1 0.879180 -0.307876 0.190277 11.00000 0.19293 0.19972 = 0.14975 -0.08933 -0.04221 -0.03332 C2 1 0.632221 -0.108774 0.108155 11.00000 0.28869 0.15766 = 0.16720 -0.03793 -0.11395 -0.06336 C4 1 0.570181 -0.132271 0.177843 11.00000 0.13758 0.15535 = 0.18704 -0.08010 -0.06768 0.00914 N8 4 0.724736 -0.329217 0.245851 11.00000 0.34261 0.16232 = 0.05363 -0.00005 -0.08609 -0.11909 N7 4 0.851853 -0.232739 0.170829 11.00000 0.07959 0.24040 = 0.15013 -0.14911 -0.01254 -0.01214 N3 4 0.780402 -0.333553 0.678071 11.00000 0.13601 0.06545 = 0.34218 0.07429 0.13245 0.00197 N5 4 0.673098 -0.131501 0.714864 11.00000 0.20309 0.05934 = 0.22211 0.01552 0.11543 -0.04429 N4 4 0.706674 -0.249878 0.556530 11.00000 0.19309 0.24918 = 0.04090 0.02000 0.01814 -0.12720 N6 4 0.740892 -0.222165 0.826560 11.00000 0.29066 0.32458 = 0.07554 -0.00090 0.06971 -0.24647 C9 1 0.740903 -0.144367 0.845046 11.00000 0.34727 0.32360 = 0.13410 -0.09114 0.16994 -0.21169 C1 1 0.789253 -0.347151 0.583352 11.00000 0.20567 0.07189 = 0.28971 -0.04512 0.20260 -0.07773 C17 1 0.703270 -0.330736 0.550803 11.00000 0.23619 0.22762 = 0.18530 0.02608 0.01858 -0.09889 C20 1 0.650586 -0.129205 0.810863 11.00000 0.31905 0.17540 = 0.20609 -0.09736 0.10983 -0.11837 O22 5 0.930914 -0.450108 0.441487 11.00000 0.10273 0.04966 = 0.37284 0.00254 0.02136 0.01592 O23 5 0.729267 -0.003084 -0.071468 11.00000 0.37339 0.38154 = 0.19178 0.12455 0.24233 0.16863 HKLF 5 REM CuV-1-2_150K_Pnn2_twin_twin1_hklf4 in Pnn2 #34 REM wR2 = 0.1860, GooF = S = 1.040, Restrained GooF = 1.062 for all data REM R1 = 0.0677 for 13167 Fo > 4sig(Fo) and 0.0715 for all 14113 data REM 457 parameters refined using 109 restraints END WGHT 0.1482 0.9671 REM Highest difference peak 1.176, deepest hole -0.544, 1-sigma level 0.178 Q1 1 0.9798 0.1607 0.8377 11.00000 0.05 1.18 Q2 1 0.7684 -0.2621 0.1991 11.00000 0.05 1.15 Q3 1 0.9647 -0.1551 0.0453 11.00000 0.05 1.06 Q4 1 0.9894 0.0024 0.9421 11.00000 0.05 0.98 Q5 1 0.7687 -0.2582 0.6820 11.00000 0.05 0.92 Q6 1 0.5986 0.1644 0.4321 11.00000 0.05 0.90 Q7 1 1.0217 -0.2050 0.4295 11.00000 0.05 0.86 Q8 1 0.5000 0.0000 0.4004 10.50000 0.05 0.77 Q9 1 0.9193 0.1618 0.3313 11.00000 0.05 0.70 Q10 1 0.5000 0.0000 0.4882 10.50000 0.05 0.70 Q11 1 0.9026 0.1577 0.5420 11.00000 0.05 0.69 Q12 1 0.8567 -0.1383 0.4301 11.00000 0.05 0.67 Q13 1 0.7592 -0.2363 0.7331 11.00000 0.05 0.65 Q14 1 0.9979 0.1578 0.3259 11.00000 0.05 0.65 Q15 1 0.9583 -0.1412 0.5687 11.00000 0.05 0.63 Q16 1 0.7598 0.0031 -0.0571 11.00000 0.05 0.62 Q17 1 0.8795 -0.1599 0.5382 11.00000 0.05 0.62 Q18 1 0.5740 -0.1689 0.4624 11.00000 0.05 0.61 Q19 1 0.8622 -0.0012 0.1622 11.00000 0.05 0.61 Q20 1 0.5169 -0.0564 0.5337 11.00000 0.05 0.60 Q21 1 0.8968 -0.1647 0.4272 11.00000 0.05 0.58 Q22 1 0.4984 0.0147 0.6932 11.00000 0.05 0.58 Q23 1 0.8613 -0.1563 0.3611 11.00000 0.05 0.57 Q24 1 0.8945 -0.1662 0.4513 11.00000 0.05 0.56 Q25 1 0.8184 0.1256 0.5081 11.00000 0.05 0.56 Q26 1 0.7574 -0.0165 0.3745 11.00000 0.05 0.55 Q27 1 0.9562 -0.1402 0.6416 11.00000 0.05 0.54 Q28 1 0.5679 0.1778 0.3417 11.00000 0.05 0.54 Q29 1 1.0023 0.1576 0.2197 11.00000 0.05 0.53 Q30 1 0.9117 0.1548 0.4775 11.00000 0.05 0.52 Q31 1 0.9667 -0.4450 0.3848 11.00000 0.05 0.48 Q32 1 0.7766 -0.0850 0.4366 11.00000 0.05 0.48 Q33 1 0.9061 0.1418 0.2449 11.00000 0.05 0.48 Q34 1 0.7973 0.0045 0.3058 11.00000 0.05 0.46 Q35 1 0.7250 0.0088 0.5923 11.00000 0.05 0.46 Q36 1 0.5153 -0.0571 0.2006 11.00000 0.05 0.46 Q37 1 0.5000 0.0000 0.1982 10.50000 0.05 0.45 Q38 1 0.9350 -0.3018 0.1372 11.00000 0.05 0.41 Q39 1 0.7171 -0.3025 0.5175 11.00000 0.05 0.41 Q40 1 0.9949 0.1279 0.2353 11.00000 0.05 0.41 Q41 1 0.7761 -0.3453 0.2922 11.00000 0.05 0.41 Q42 1 0.7365 -0.1768 0.8649 11.00000 0.05 0.41 Q43 1 0.6674 -0.1561 0.6997 11.00000 0.05 0.40 Q44 1 0.5000 0.0000 0.6123 10.50000 0.05 0.40 Q45 1 0.6412 -0.2473 0.1984 11.00000 0.05 0.39 Q46 1 0.7627 -0.2619 0.8781 11.00000 0.05 0.38 Q47 1 0.6755 -0.1409 0.6782 11.00000 0.05 0.38 Q48 1 0.6830 -0.1142 0.0942 11.00000 0.05 0.38 Q49 1 0.8069 -0.3714 0.2772 11.00000 0.05 0.37 Q50 1 0.4525 -0.1599 0.2910 11.00000 0.05 0.37 Q51 1 0.8316 -0.3569 0.6545 11.00000 0.05 0.37 Q52 1 0.9365 -0.3370 0.2018 11.00000 0.05 0.37 Q53 1 0.6416 -0.2233 0.1632 11.00000 0.05 0.37 Q54 1 0.8060 0.1145 0.3981 11.00000 0.05 0.36 Q55 1 0.7102 -0.1452 0.1000 11.00000 0.05 0.36 Q56 1 0.5954 -0.0750 0.1763 11.00000 0.05 0.36 ; _shelx_res_checksum 74585 _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 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z+1/2' '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 V6 V 0.9007(2) 0.01104(19) 0.6802(2) 0.0444(7) Uani 1 1 d . . . . . V8 V 0.7616(2) 0.0121(2) 0.5433(2) 0.0469(8) Uani 1 1 d . . . . . V4 V 0.7625(2) 0.0224(2) 0.3469(2) 0.0481(8) Uani 1 1 d . . . . . V2 V 0.9008(2) 0.00144(16) 0.2083(2) 0.0380(7) Uani 1 1 d . . . . . V3 V 0.8202(2) -0.12780(17) 0.3791(2) 0.0480(8) Uani 1 1 d . . . . . V7 V 0.9192(2) -0.13537(17) 0.6057(2) 0.0479(8) Uani 1 1 d . . . . . V1 V 0.9499(2) 0.14529(16) 0.2822(2) 0.0432(7) Uani 1 1 d . . . . . V5 V 0.9796(2) -0.20933(11) 0.4437(3) 0.0492(6) Uani 1 1 d . . . . . V10 V 0.8530(2) 0.15234(16) 0.5094(2) 0.0476(8) Uani 1 1 d . . . . . Cl10 Cl 1.000000 0.000000 0.4431(9) 0.0565(11) Uani 1 2 d S T P . . Cu11 Cu 0.7187(3) -0.2276(2) 0.1926(3) 0.0921(13) Uani 1 1 d D . . . . Cu12 Cu 0.7258(3) -0.23473(18) 0.6928(3) 0.0818(10) Uani 1 1 d D . . . . O1 O 1.0108(9) 0.0672(7) 0.6770(10) 0.047(3) Uani 1 1 d . . . . . O2 O 0.9968(9) -0.0691(6) 0.2110(9) 0.041(3) Uani 1 1 d . . . . . O3 O 0.8493(9) 0.0794(7) 0.2778(8) 0.038(3) Uani 1 1 d . . . . . O4 O 0.8358(10) 0.0796(7) 0.6038(9) 0.045(3) Uani 1 1 d . . . . . O5 O 0.8299(9) -0.0582(8) 0.6090(9) 0.046(3) Uani 1 1 d . . . . . O6 O 0.8257(10) -0.0572(7) 0.2845(8) 0.044(3) Uani 1 1 d . . . . . O8 O 0.7594(7) -0.0492(7) 0.4406(10) 0.049(3) Uani 1 1 d . . . . . O10 O 0.9055(11) 0.1785(6) 0.3972(8) 0.051(3) Uani 1 1 d . . . . . O11 O 0.6622(10) 0.0321(14) 0.3020(12) 0.082(6) Uani 1 1 d . . . . . O13 O 0.8683(8) -0.1636(6) 0.4898(8) 0.038(2) Uani 1 1 d . . . . . O7 O 0.7733(8) 0.0853(7) 0.4511(10) 0.048(3) Uani 1 1 d . . . . . O9 O 0.6610(13) 0.0158(13) 0.5857(13) 0.080(6) Uani 1 1 d . . . . . O12 O 0.7411(13) -0.1831(10) 0.3493(14) 0.084(6) Uani 1 1 d . . . . . O14 O 0.8560(12) 0.0031(9) 0.1068(10) 0.061(4) Uani 1 1 d . . . . . O16 O 0.9703(10) 0.1744(6) 0.5572(9) 0.050(3) Uani 1 1 d . . . . . O17 O 0.8850(13) -0.1937(9) 0.6799(12) 0.076(5) Uani 1 1 d . . . . . O18 O 0.8557(13) 0.0137(13) 0.7803(13) 0.078(6) Uani 1 1 d . . . . . O15 O 0.9279(13) 0.2116(8) 0.2125(11) 0.069(4) Uani 1 1 d . . . . . O19 O 0.9327(10) -0.1663(6) 0.3356(10) 0.051(3) Uani 1 1 d . . . . . O20 O 0.9750(12) -0.2971(5) 0.4414(18) 0.081(4) Uani 1 1 d . . . . . O21 O 0.7921(13) 0.2218(8) 0.5368(11) 0.076(5) Uani 1 1 d . . . . . N1 N 0.726(3) -0.1255(17) 0.132(2) 0.21(2) Uani 1 1 d D U . . . N2 N 0.5779(15) -0.2086(16) 0.196(3) 0.125(12) Uani 1 1 d D U . . . C5 C 0.824(4) -0.3389(18) 0.259(3) 0.19(2) Uani 1 1 d D U . . . C10 C 0.879(3) -0.308(3) 0.190(4) 0.18(2) Uani 1 1 d D U . . . C2 C 0.632(3) -0.109(2) 0.108(3) 0.20(2) Uani 1 1 d D U . . . C4 C 0.570(3) -0.132(2) 0.178(4) 0.160(18) Uani 1 1 d D U . . . N8 N 0.725(3) -0.3292(16) 0.2459(18) 0.19(2) Uani 1 1 d D U . . . N7 N 0.8519(17) -0.233(2) 0.171(2) 0.157(19) Uani 1 1 d D U . . . N3 N 0.780(2) -0.3336(13) 0.678(3) 0.18(2) Uani 1 1 d D U . . . N5 N 0.673(2) -0.1315(12) 0.715(3) 0.162(19) Uani 1 1 d D U . . . N4 N 0.707(2) -0.250(2) 0.5565(14) 0.161(17) Uani 1 1 d D U . . . N6 N 0.741(3) -0.222(2) 0.8266(17) 0.23(3) Uani 1 1 d D U . . . C9 C 0.741(4) -0.144(3) 0.845(2) 0.27(3) Uani 1 1 d D U . . . C1 C 0.789(3) -0.3472(14) 0.583(3) 0.19(2) Uani 1 1 d D U . . . C17 C 0.703(4) -0.331(2) 0.551(3) 0.22(2) Uani 1 1 d D U . . . C20 C 0.651(4) -0.129(3) 0.811(3) 0.23(3) Uani 1 1 d D U . . . O22 O 0.9309(16) -0.4501(10) 0.441(4) 0.175(15) Uani 1 1 d . . . . . O23 O 0.729(4) -0.003(3) -0.071(3) 0.32(4) 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 V6 0.0416(16) 0.0642(18) 0.0274(17) 0.0025(12) 0.0033(13) 0.0104(14) V8 0.0343(17) 0.0691(19) 0.0372(18) 0.0008(14) 0.0073(13) 0.0052(14) V4 0.0311(15) 0.079(2) 0.0344(16) 0.0071(16) -0.0025(13) -0.0030(14) V2 0.0363(15) 0.0520(16) 0.0256(16) 0.0024(10) -0.0051(12) -0.0032(13) V3 0.0543(19) 0.0473(15) 0.0425(15) -0.0010(12) 0.0004(15) -0.0270(14) V7 0.054(2) 0.0477(16) 0.0418(16) 0.0188(13) 0.0086(15) -0.0070(13) V1 0.0540(19) 0.0356(13) 0.0400(16) 0.0149(11) -0.0037(15) 0.0034(12) V5 0.0733(18) 0.0192(10) 0.0551(15) -0.0004(14) 0.008(2) -0.0018(10) V10 0.056(2) 0.0439(15) 0.0425(16) -0.0049(12) -0.0014(15) 0.0272(14) Cl10 0.057(4) 0.054(3) 0.058(4) 0.000 0.000 0.001(2) Cu11 0.115(3) 0.094(2) 0.0674(17) -0.0247(18) -0.006(2) -0.059(2) Cu12 0.105(2) 0.0705(18) 0.0705(17) 0.0214(15) 0.0271(19) -0.0348(17) O1 0.057(8) 0.048(7) 0.038(8) -0.015(5) -0.007(6) 0.009(6) O2 0.058(8) 0.037(6) 0.029(6) -0.014(5) 0.008(5) -0.003(5) O3 0.033(6) 0.047(6) 0.034(6) 0.011(5) 0.003(5) -0.001(5) O4 0.048(7) 0.057(7) 0.030(6) -0.003(5) 0.013(5) 0.022(6) O5 0.042(7) 0.071(8) 0.026(5) 0.011(5) 0.012(5) 0.012(6) O6 0.052(7) 0.054(7) 0.027(6) 0.010(5) 0.009(5) -0.022(6) O8 0.035(5) 0.071(7) 0.041(6) -0.007(7) 0.006(6) -0.017(5) O10 0.081(10) 0.034(5) 0.036(6) 0.002(5) 0.001(6) 0.022(6) O11 0.032(8) 0.168(19) 0.047(9) 0.022(11) -0.010(6) -0.002(9) O13 0.043(6) 0.029(5) 0.041(6) 0.006(4) 0.007(5) -0.007(4) O7 0.038(6) 0.066(7) 0.039(6) -0.004(6) -0.009(6) 0.008(5) O9 0.053(10) 0.132(17) 0.054(10) -0.010(9) -0.013(8) 0.014(10) O12 0.085(11) 0.079(10) 0.088(11) -0.025(9) 0.034(10) -0.053(10) O14 0.076(11) 0.089(10) 0.018(6) 0.008(6) -0.028(7) 0.003(8) O16 0.072(9) 0.024(5) 0.055(8) -0.013(5) 0.004(7) 0.013(5) O17 0.095(13) 0.071(9) 0.062(9) 0.042(8) 0.012(9) -0.017(9) O18 0.054(9) 0.140(17) 0.039(9) 0.017(8) 0.011(7) 0.014(10) O15 0.095(12) 0.060(8) 0.053(9) 0.027(7) -0.011(8) 0.006(8) O19 0.062(8) 0.030(5) 0.061(8) -0.002(5) 0.005(6) -0.020(5) O20 0.139(13) 0.016(4) 0.088(10) 0.006(8) 0.020(14) -0.014(6) O21 0.100(13) 0.068(9) 0.059(9) -0.014(7) -0.020(9) 0.056(9) N1 0.32(5) 0.17(3) 0.13(3) 0.05(2) -0.16(3) -0.16(4) N2 0.073(16) 0.14(2) 0.16(3) -0.05(2) -0.018(18) -0.050(16) C5 0.31(6) 0.09(2) 0.17(4) -0.07(3) -0.08(4) 0.01(3) C10 0.19(5) 0.20(4) 0.15(4) -0.09(4) -0.04(3) -0.03(4) C2 0.29(6) 0.16(4) 0.17(4) -0.04(3) -0.11(4) -0.06(4) C4 0.14(3) 0.16(3) 0.19(4) -0.08(3) -0.07(3) 0.01(3) N8 0.34(6) 0.16(3) 0.054(14) 0.000(16) -0.09(3) -0.12(4) N7 0.080(17) 0.24(4) 0.15(3) -0.15(3) -0.013(17) -0.01(2) N3 0.14(3) 0.065(14) 0.34(6) 0.07(3) 0.13(3) 0.002(16) N5 0.20(4) 0.059(13) 0.22(4) 0.016(19) 0.12(3) -0.044(19) N4 0.19(3) 0.25(4) 0.041(13) 0.020(18) 0.018(15) -0.13(3) N6 0.29(5) 0.32(5) 0.08(2) 0.00(2) 0.07(3) -0.25(4) C9 0.35(6) 0.32(5) 0.13(3) -0.09(3) 0.17(4) -0.21(5) C1 0.21(3) 0.072(17) 0.29(5) -0.05(2) 0.20(3) -0.08(2) C17 0.24(5) 0.23(5) 0.19(5) 0.03(4) 0.02(4) -0.10(5) C20 0.32(6) 0.18(4) 0.21(5) -0.10(4) 0.11(5) -0.12(4) O22 0.103(14) 0.050(9) 0.37(5) 0.00(2) 0.02(3) 0.016(10) O23 0.37(7) 0.38(8) 0.19(4) 0.12(4) 0.24(5) 0.17(6) 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' 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' 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 V8 V6 V6 134.85(9) . 2_755 ? V8 V6 V7 78.89(13) . . ? V7 V6 V6 77.35(14) . 2_755 ? O1 V6 V6 40.0(4) 2_755 2_755 ? O1 V6 V6 40.4(4) . 2_755 ? O1 V6 V8 125.4(5) . . ? O1 V6 V8 117.7(5) 2_755 . ? O1 V6 V7 41.0(5) 2_755 . ? O1 V6 V7 114.0(4) . . ? O1 V6 O1 80.3(6) . 2_755 ? O1 V6 O4 142.8(6) 2_755 . ? O1 V6 O4 93.0(6) . . ? O1 V6 O5 141.9(6) . . ? O1 V6 O5 82.1(6) 2_755 . ? O4 V6 V6 125.2(5) . 2_755 ? O4 V6 V8 40.3(4) . . ? O4 V6 V7 115.1(4) . . ? O4 V6 O5 81.2(6) . . ? O5 V6 V6 116.0(4) . 2_755 ? O5 V6 V8 41.1(4) . . ? O5 V6 V7 41.1(4) . . ? O18 V6 V6 114.1(7) . 2_755 ? O18 V6 V8 110.5(7) . . ? O18 V6 V7 114.2(9) . . ? O18 V6 O1 108.6(8) . 2_755 ? O18 V6 O1 110.5(9) . . ? O18 V6 O4 108.0(8) . . ? O18 V6 O5 107.1(9) . . ? V6 V8 V4 134.34(15) . . ? V6 V8 V10 78.55(13) . . ? V4 V8 V10 76.82(14) . . ? O4 V8 V6 42.0(4) . . ? O4 V8 V4 115.4(5) . . ? O4 V8 V10 40.4(4) . . ? O4 V8 O5 84.2(7) . . ? O4 V8 O8 141.8(6) . . ? O4 V8 O7 79.8(6) . . ? O5 V8 V6 42.4(5) . . ? O5 V8 V4 123.4(4) . . ? O5 V8 V10 116.1(5) . . ? O5 V8 O7 142.2(6) . . ? O8 V8 V6 125.0(4) . . ? O8 V8 V4 40.3(5) . . ? O8 V8 V10 113.1(4) . . ? O8 V8 O5 90.8(6) . . ? O8 V8 O7 81.3(6) . . ? O7 V8 V6 116.1(4) . . ? O7 V8 V4 41.1(4) . . ? O7 V8 V10 39.4(4) . . ? O9 V8 V6 112.4(6) . . ? O9 V8 V4 112.9(7) . . ? O9 V8 V10 116.7(9) . . ? O9 V8 O4 108.8(8) . . ? O9 V8 O5 108.4(9) . . ? O9 V8 O8 108.7(8) . . ? O9 V8 O7 109.2(9) . . ? V8 V4 V2 134.13(15) . . ? V8 V4 V3 77.16(14) . . ? V2 V4 V3 77.71(13) . . ? O3 V4 V8 124.2(4) . . ? O3 V4 V2 40.7(4) . . ? O3 V4 V3 113.8(4) . . ? O3 V4 O6 81.0(5) . . ? O6 V4 V8 115.0(4) . . ? O6 V4 V2 40.6(3) . . ? O6 V4 V3 40.2(4) . . ? O8 V4 V8 39.8(4) . . ? O8 V4 V2 115.8(4) . . ? O8 V4 V3 40.5(4) . . ? O8 V4 O3 140.2(5) . . ? O8 V4 O6 80.7(5) . . ? O8 V4 O7 80.6(6) . . ? O11 V4 V8 114.2(7) . . ? O11 V4 V2 111.2(7) . . ? O11 V4 V3 115.6(9) . . ? O11 V4 O3 108.9(8) . . ? O11 V4 O6 108.7(10) . . ? O11 V4 O8 110.4(8) . . ? O11 V4 O7 109.5(9) . . ? O7 V4 V8 40.9(4) . . ? O7 V4 V2 125.6(4) . . ? O7 V4 V3 114.2(4) . . ? O7 V4 O3 92.4(6) . . ? O7 V4 O6 141.4(6) . . ? V4 V2 V2 134.49(9) . 2_755 ? V4 V2 V1 78.02(13) . . ? V2 V2 V1 76.77(13) 2_755 . ? O2 V2 V4 126.1(4) . . ? O2 V2 V4 116.1(4) 2_755 . ? O2 V2 V2 40.6(4) 2_755 2_755 ? O2 V2 V2 41.5(4) . 2_755 ? O2 V2 V1 39.9(4) 2_755 . ? O2 V2 V1 114.7(4) . . ? O2 V2 O2 82.1(5) . 2_755 ? O2 V2 O3 141.6(6) . . ? O3 V2 V4 41.4(4) . . ? O3 V2 V2 114.1(4) . 2_755 ? O3 V2 V1 39.6(4) . . ? O3 V2 O2 79.5(5) . 2_755 ? O6 V2 V4 41.9(4) . . ? O6 V2 V2 124.6(5) . 2_755 ? O6 V2 V1 115.4(4) . . ? O6 V2 O2 91.8(6) . . ? O6 V2 O2 142.4(6) . 2_755 ? O6 V2 O3 83.0(6) . . ? O14 V2 V4 111.1(7) . . ? O14 V2 V2 113.7(7) . 2_755 ? O14 V2 V1 114.9(6) . . ? O14 V2 O2 108.5(7) . 2_755 ? O14 V2 O2 109.2(7) . . ? O14 V2 O3 108.5(7) . . ? O14 V2 O6 108.5(8) . . ? V4 V3 V5 139.86(13) . . ? O6 V3 V4 41.6(4) . . ? O6 V3 V5 123.4(5) . . ? O6 V3 O8 81.7(6) . . ? O6 V3 O19 88.2(6) . . ? O8 V3 V4 40.1(5) . . ? O8 V3 V5 126.8(5) . . ? O13 V3 V4 125.1(4) . . ? O13 V3 V5 41.2(4) . . ? O13 V3 O6 148.2(5) . . ? O13 V3 O8 91.5(6) . . ? O13 V3 O19 80.8(5) . . ? O12 V3 V4 110.0(9) . . ? O12 V3 V5 110.1(9) . . ? O12 V3 O6 105.1(10) . . ? O12 V3 O8 105.5(8) . . ? O12 V3 O13 106.6(9) . . ? O12 V3 O19 107.5(8) . . ? O19 V3 V4 123.1(4) . . ? O19 V3 V5 39.7(5) . . ? O19 V3 O8 147.0(5) . . ? V5 V7 V6 140.70(13) . . ? O1 V7 V6 41.2(4) 2_755 . ? O1 V7 V5 126.3(4) 2_755 . ? O1 V7 O13 149.3(5) 2_755 . ? O5 V7 V6 41.5(5) . . ? O5 V7 V5 125.1(4) . . ? O5 V7 O1 82.7(6) . 2_755 ? O5 V7 O13 87.5(5) . . ? O13 V7 V6 122.9(3) . . ? O13 V7 V5 42.5(3) . . ? O16 V7 V6 124.4(4) 2_755 . ? O16 V7 V5 41.8(4) 2_755 . ? O16 V7 O1 89.7(6) 2_755 2_755 ? O16 V7 O5 149.4(6) 2_755 . ? O16 V7 O13 84.1(6) 2_755 . ? O17 V7 V6 109.1(8) . . ? O17 V7 V5 110.2(8) . . ? O17 V7 O1 103.0(8) . 2_755 ? O17 V7 O5 105.0(8) . . ? O17 V7 O13 107.6(8) . . ? O17 V7 O16 105.7(8) . 2_755 ? V5 V1 V2 140.14(13) 2_755 . ? O2 V1 V2 40.8(4) 2_755 . ? O2 V1 V5 127.6(4) 2_755 2_755 ? O2 V1 O10 148.9(5) 2_755 . ? O2 V1 O19 90.2(6) 2_755 2_755 ? O3 V1 V2 39.7(4) . . ? O3 V1 V5 124.8(4) . 2_755 ? O3 V1 O2 80.5(6) . 2_755 ? O3 V1 O10 88.2(6) . . ? O3 V1 O19 146.1(5) . 2_755 ? O10 V1 V2 121.9(4) . . ? O10 V1 V5 41.7(5) . 2_755 ? O10 V1 O19 83.1(7) . 2_755 ? O15 V1 V2 112.8(6) . . ? O15 V1 V5 107.0(6) . 2_755 ? O15 V1 O2 106.3(7) . 2_755 ? O15 V1 O3 107.3(8) . . ? O15 V1 O10 104.7(7) . . ? O15 V1 O19 106.6(8) . 2_755 ? O19 V1 V2 123.2(4) 2_755 . ? O19 V1 V5 41.8(5) 2_755 2_755 ? V7 V5 V3 77.56(12) . . ? V1 V5 V3 78.94(14) 2_755 . ? V1 V5 V7 127.54(11) 2_755 . ? V10 V5 V3 127.79(11) 2_755 . ? V10 V5 V7 79.08(14) 2_755 . ? V10 V5 V1 79.58(12) 2_755 2_755 ? O10 V5 V3 115.9(4) 2_755 . ? O10 V5 V7 115.5(4) 2_755 . ? O10 V5 V1 41.9(4) 2_755 2_755 ? O10 V5 V10 41.3(4) 2_755 2_755 ? O10 V5 O13 137.4(4) 2_755 . ? O10 V5 O16 82.9(6) 2_755 2_755 ? O10 V5 O19 84.0(6) 2_755 . ? O13 V5 V3 39.6(4) . . ? O13 V5 V7 41.9(4) . . ? O13 V5 V1 114.6(3) . 2_755 ? O13 V5 V10 116.5(4) . 2_755 ? O16 V5 V3 114.5(4) 2_755 . ? O16 V5 V7 41.1(4) 2_755 . ? O16 V5 V1 116.6(4) 2_755 2_755 ? O16 V5 V10 41.8(5) 2_755 2_755 ? O16 V5 O13 82.8(6) 2_755 . ? O19 V5 V3 39.7(4) . . ? O19 V5 V7 112.7(4) . . ? O19 V5 V1 42.5(4) . 2_755 ? O19 V5 V10 116.4(4) . 2_755 ? O19 V5 O13 79.2(6) . . ? O19 V5 O16 136.2(5) . 2_755 ? O20 V5 V3 118.0(8) . . ? O20 V5 V7 118.3(9) . . ? O20 V5 V1 114.1(9) . 2_755 ? O20 V5 V10 114.2(8) . 2_755 ? O20 V5 O10 109.0(8) . 2_755 ? O20 V5 O13 113.6(7) . . ? O20 V5 O16 111.4(10) . 2_755 ? O20 V5 O19 112.4(10) . . ? V5 V10 V8 140.66(13) 2_755 . ? O4 V10 V8 38.7(4) . . ? O4 V10 V5 127.5(5) . 2_755 ? O10 V10 V8 123.9(4) . . ? O10 V10 V5 41.8(5) . 2_755 ? O10 V10 O4 148.8(5) . . ? O10 V10 O7 91.1(7) . . ? O10 V10 O16 84.3(6) . . ? O7 V10 V8 39.8(4) . . ? O7 V10 V5 128.0(4) . 2_755 ? O7 V10 O4 78.5(6) . . ? O7 V10 O16 149.4(5) . . ? O16 V10 V8 122.3(4) . . ? O16 V10 V5 42.8(5) . 2_755 ? O16 V10 O4 89.9(6) . . ? O21 V10 V8 113.3(8) . . ? O21 V10 V5 106.0(8) . 2_755 ? O21 V10 O4 107.0(8) . . ? O21 V10 O10 104.2(8) . . ? O21 V10 O7 106.5(8) . . ? O21 V10 O16 104.0(8) . . ? N1 Cu11 N2 84.9(14) . . ? N8 Cu11 N1 174(2) . . ? N8 Cu11 N2 100.8(17) . . ? N7 Cu11 N1 85.6(18) . . ? N7 Cu11 N2 169.6(17) . . ? N7 Cu11 N8 88.6(17) . . ? N3 Cu12 N5 176.8(17) . . ? N3 Cu12 N4 79.9(13) . . ? N3 Cu12 N6 99.7(18) . . ? N4 Cu12 N5 103.1(16) . . ? N6 Cu12 N5 77.3(14) . . ? N6 Cu12 N4 178.1(12) . . ? V6 O1 V6 99.6(6) . 2_755 ? V6 O1 V7 144.1(8) . 2_755 ? V7 O1 V6 97.8(7) 2_755 2_755 ? V2 O2 V2 97.9(5) . 2_755 ? V2 O2 V1 143.7(8) . 2_755 ? V1 O2 V2 99.2(7) 2_755 2_755 ? V2 O3 V4 97.9(6) . . ? V1 O3 V4 146.3(8) . . ? V1 O3 V2 100.7(6) . . ? V6 O4 V10 142.9(8) . . ? V8 O4 V6 97.7(6) . . ? V8 O4 V10 100.8(6) . . ? V8 O5 V6 96.5(7) . . ? V8 O5 V7 147.5(7) . . ? V7 O5 V6 97.4(6) . . ? V2 O6 V4 97.5(6) . . ? V3 O6 V4 98.2(6) . . ? V3 O6 V2 147.1(9) . . ? V8 O8 V4 99.8(6) . . ? V8 O8 V3 144.8(8) . . ? V4 O8 V3 99.4(7) . . ? V5 O10 V1 96.4(7) 2_755 . ? V10 O10 V1 146.5(7) . . ? V10 O10 V5 97.0(6) . 2_755 ? V3 O13 V7 144.2(6) . . ? V3 O13 V5 99.2(5) . . ? V7 O13 V5 95.7(6) . . ? V8 O7 V4 98.0(6) . . ? V10 O7 V8 100.7(6) . . ? V10 O7 V4 142.9(8) . . ? V7 O16 V5 97.1(7) 2_755 2_755 ? V10 O16 V7 145.7(7) . 2_755 ? V10 O16 V5 95.4(7) . 2_755 ? V3 O19 V1 146.6(7) . 2_755 ? V3 O19 V5 100.6(7) . . ? V5 O19 V1 95.8(7) . 2_755 ? C2 N1 Cu11 104(2) . . ? C4 N2 Cu11 103.7(18) . . ? C10 C5 N8 115(3) . . ? C5 C10 N7 111(3) . . ? C4 C2 N1 111(3) . . ? N2 C4 C2 112(3) . . ? C5 N8 Cu11 102(2) . . ? C10 N7 Cu11 106(2) . . ? C1 N3 Cu12 107.6(18) . . ? C20 N5 Cu12 105(2) . . ? C17 N4 Cu12 101.3(19) . . ? C9 N6 Cu12 107.4(19) . . ? C20 C9 N6 97(3) . . ? C17 C1 N3 103(2) . . ? C1 C17 N4 100(3) . . ? C9 C20 N5 97(3) . . ? 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 V6 V6 2.951(7) 2_755 ? V6 V8 2.878(4) . ? V6 V7 2.921(5) . ? V6 O1 1.922(15) . ? V6 O1 1.941(13) 2_755 ? V6 O4 1.944(13) . ? V6 O5 1.953(15) . ? V6 O18 1.622(18) . ? V8 V4 2.911(4) . ? V8 V10 2.950(5) . ? V8 O4 1.879(15) . ? V8 O5 1.903(13) . ? V8 O8 1.892(15) . ? V8 O7 1.923(15) . ? V8 O9 1.61(2) . ? V4 V2 2.912(4) . ? V4 V3 2.928(5) . ? V4 O3 1.943(12) . ? V4 O6 1.963(15) . ? V4 O8 1.912(15) . ? V4 O11 1.629(15) . ? V4 O7 1.934(14) . ? V2 V2 2.922(6) 2_755 ? V2 V1 2.952(4) . ? V2 O2 1.919(13) . ? V2 O2 1.955(13) 2_755 ? V2 O3 1.919(13) . ? V2 O6 1.911(11) . ? V2 O14 1.640(12) . ? V3 V5 2.942(5) . ? V3 O6 1.909(12) . ? V3 O8 1.928(14) . ? V3 O13 1.901(12) . ? V3 O12 1.607(15) . ? V3 O19 1.911(15) . ? V7 V5 2.893(6) . ? V7 O1 1.935(16) 2_755 ? V7 O5 1.935(14) . ? V7 O13 1.940(13) . ? V7 O16 1.916(15) 2_755 ? V7 O17 1.615(12) . ? V1 V5 2.857(5) 2_755 ? V1 O2 1.920(14) 2_755 ? V1 O3 1.914(13) . ? V1 O10 1.921(13) . ? V1 O15 1.628(13) . ? V1 O19 1.938(14) 2_755 ? V5 V10 2.849(5) 2_755 ? V5 O10 1.912(16) 2_755 ? V5 O13 1.963(12) . ? V5 O16 1.943(15) 2_755 ? V5 O19 1.912(16) . ? V5 O20 1.616(10) . ? V10 O4 1.948(14) . ? V10 O10 1.893(14) . ? V10 O7 1.907(13) . ? V10 O16 1.909(16) . ? V10 O21 1.611(13) . ? Cu11 N1 2.08(3) . ? Cu11 N2 2.10(2) . ? Cu11 N8 2.03(3) . ? Cu11 N7 1.99(2) . ? Cu12 N3 2.00(2) . ? Cu12 N5 2.08(3) . ? Cu12 N4 2.05(2) . ? Cu12 N6 2.00(3) . ? N1 C2 1.46(3) . ? N2 C4 1.43(3) . ? C5 C10 1.42(4) . ? C5 N8 1.49(3) . ? C10 N7 1.47(3) . ? C2 C4 1.44(4) . ? N3 C1 1.43(3) . ? N5 C20 1.46(3) . ? N4 C17 1.49(3) . ? N6 C9 1.46(3) . ? C9 C20 1.45(4) . ? C1 C17 1.39(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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag V6 V8 O4 V10 147.7(9) . . . . ? V6 V8 O8 V4 -119.6(5) . . . . ? V6 V8 O8 V3 2.6(15) . . . . ? V8 V10 O10 V1 -17.5(18) . . . . ? V8 V10 O10 V5 -130.3(4) . . . 2_755 ? V4 V8 O4 V6 -128.9(4) . . . . ? V4 V8 O4 V10 18.7(7) . . . . ? V4 V8 O8 V3 122.2(14) . . . . ? V5 V10 O10 V1 112.8(17) 2_755 . . . ? V10 V8 O4 V6 -147.7(9) . . . . ? V10 V8 O8 V4 -27.6(6) . . . . ? V10 V8 O8 V3 94.6(13) . . . . ? Cu11 N1 C2 C4 39(4) . . . . ? Cu11 N2 C4 C2 41(4) . . . . ? Cu12 N3 C1 C17 -50(3) . . . . ? Cu12 N5 C20 C9 59(3) . . . . ? Cu12 N4 C17 C1 -61(3) . . . . ? Cu12 N6 C9 C20 61(3) . . . . ? O4 V8 O8 V4 -64.9(11) . . . . ? O4 V8 O8 V3 57.3(18) . . . . ? O4 V10 O10 V1 28(2) . . . . ? O4 V10 O10 V5 -85.2(13) . . . 2_755 ? O5 V8 O4 V6 -4.6(6) . . . . ? O5 V8 O4 V10 143.1(6) . . . . ? O5 V8 O8 V4 -146.6(6) . . . . ? O5 V8 O8 V3 -24.4(13) . . . . ? O8 V8 O4 V6 -88.5(10) . . . . ? O8 V8 O4 V10 59.2(11) . . . . ? O7 V8 O4 V6 -150.1(6) . . . . ? O7 V8 O4 V10 -2.4(6) . . . . ? O7 V8 O8 V4 -3.7(5) . . . . ? O7 V8 O8 V3 118.4(12) . . . . ? O7 V10 O10 V1 -41.7(16) . . . . ? O7 V10 O10 V5 -154.5(5) . . . 2_755 ? O9 V8 O4 V6 102.9(9) . . . . ? O9 V8 O4 V10 -109.4(9) . . . . ? O9 V8 O8 V4 103.7(9) . . . . ? O9 V8 O8 V3 -134.1(14) . . . . ? O16 V10 O10 V1 108.0(16) . . . . ? O16 V10 O10 V5 -4.8(4) . . . 2_755 ? O21 V10 O10 V1 -149.0(16) . . . . ? O21 V10 O10 V5 98.2(8) . . . 2_755 ? N1 C2 C4 N2 -57(5) . . . . ? C5 C10 N7 Cu11 -32(4) . . . . ? C10 C5 N8 Cu11 -37(4) . . . . ? N8 C5 C10 N7 49(5) . . . . ? N3 C1 C17 N4 74(3) . . . . ? N6 C9 C20 N5 -77(3) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.578(3) 2 0.422(3)