#------------------------------------------------------------------------------ #$Date: 2026-05-07 23:58:41 +0100 (Thu, 07 May 2026) $ #$Revision: 305892 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/09/7720994.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_7720994 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, 4(C6 N6 Ni), Cl, 13.25(O)' _chemical_formula_sum 'C24 Cl N24 Ni4 O55.26 V18' _chemical_formula_weight 2695.81 _space_group_crystal_system tetragonal _space_group_IT_number 138 _space_group_name_Hall '-P 4ac 2ac' _space_group_name_H-M_alt 'P 42/n c m :2' _audit_creation_date 2026-03-16 _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 4 _cell_length_a 24.6487(10) _cell_length_b 24.6487(10) _cell_length_c 16.6483(17) _cell_measurement_reflns_used 4982 _cell_measurement_temperature 100(1) _cell_measurement_theta_max 25.4950 _cell_measurement_theta_min 2.3320 _cell_volume 10114.8(12) _computing_cell_refinement 'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)' _computing_data_collection 'CrysAlisPro system (CCD 43.95a 64-bit (release 03-11-2023))' _computing_data_reduction 'CrysAlisPro 1.171.43.107a (Rigaku OD, 2024)' _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 'XT (Sheldrick, 2015)' _diffrn_ambient_temperature 100(1) _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type 'HyPix-Arc 100' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 -11.00 16.00 1.00 360.00 -- -11.67 58.00 -86.00 27 2 \w -22.00 16.00 1.00 360.00 -- 12.07 96.00 143.00 38 3 \w -97.00 -43.00 1.00 360.00 -- -11.67-178.00 90.00 54 4 \w 23.00 53.00 1.00 360.00 -- -11.67 19.00 120.00 30 5 \w -90.00 -43.00 1.00 360.00 -- -11.67-178.00 -60.00 47 6 \w -80.00 -42.00 1.00 360.00 -- -11.67-178.00-120.00 38 ; _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 0.0818 _diffrn_reflns_av_unetI/netI 0.0857 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 19047 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.349 _diffrn_reflns_theta_min 2.216 _exptl_absorpt_coefficient_mu 2.416 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.44373 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.107a (Rigaku Oxford Diffraction, 2024) 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 1.770 _exptl_crystal_description block _exptl_crystal_F_000 5188 _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 1.353 _refine_diff_density_min -0.727 _refine_diff_density_rms 0.187 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 304 _refine_ls_number_reflns 19047 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.024 _refine_ls_R_factor_all 0.1496 _refine_ls_R_factor_gt 0.0972 _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^)+(0.1179P)^2^+94.1205P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2369 _refine_ls_wR_factor_ref 0.2722 _reflns_Friedel_coverage 0.000 _reflns_number_gt 12157 _reflns_number_total 19047 _reflns_threshold_expression 'I > 2\s(I)' _twin_special_details ; Component 2 rotated by 87.8585\% around [0.71 0.70 0.00] (reciprocal) or [0.71 0.70 -0.00] (direct) ; _cod_data_source_file d6dt00188b2.cif _cod_data_source_block niv-1-2_100k_02_tp_twin1_hklf4 _cod_original_cell_volume 10114.8(13) _cod_original_sg_symbol_H-M 'P 42/n c m' _cod_database_code 7720994 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.499(3) 0.501(3) 2. Restrained distances N00T-C013 = N00V-C012 = N00Q-C00W = N00S-C00U = N00O-C00Z = N00R-C00X 1.5 with sigma of 0.02 Ni00-N00O = Ni00-N00Q = Ni00-N00R = Ni00-N00S = Ni00-N00T = Ni00-N00V 2.1 with sigma of 0.02 ; _shelx_res_file ; TITL niv-1-2_100k_02_tp_twin1_hklf4_a.res in P4(2)/ncm niv-1-2_100k_02_tp_twin1_hklf4.res created by SHELXL-2019/1 at 21:01:07 on 16-Mar-2026 REM Old TITL NiV-1-2_100K_02_tP_twin1_hklf4 in P4(2)/ncm REM SHELXT solution in P4(2)/ncm: R1 0.286, Rweak 0.040, Alpha 0.051 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C48 N10 O50 Cl V6 Ni16 CELL 0.71073 24.6487 24.6487 16.6483 90 90 90 ZERR 4 0.001 0.001 0.0017 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM 0.5-Y,+X,0.5+Z SYMM +Y,0.5-X,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SYMM 0.5+Y,0.5+X,-Z SYMM -Y,-X,-Z SFAC C Cl N Ni O V UNIT 96 4 96 16 221.03 72 DFIX 1.5 N00T C013 N00V C012 N00Q C00W N00S C00U N00O C00Z N00R C00X DFIX 2.1 Ni00 N00O Ni00 N00Q Ni00 N00R Ni00 N00S Ni00 N00T Ni00 N00V L.S. 10 0 0 PLAN 39 TEMP -173 CONF list 4 MORE -1 fmap 2 53 acta SHEL 10 0.83 REM REM REM WGHT 0.117900 94.120499 BASF 0.50088 FVAR 0.04541 V01 6 0.646339 0.498614 0.523345 11.00000 0.01515 0.02629 = 0.03951 -0.00203 -0.00039 0.00062 V02 6 0.611409 0.388591 0.500000 10.50000 0.02603 0.02603 = 0.03934 -0.00030 -0.00030 0.00693 V03 6 0.583809 0.583809 0.370199 10.50000 0.02407 0.02407 = 0.04286 0.01018 0.01018 0.00470 V04 6 0.584680 0.437597 0.346251 11.00000 0.02710 0.02677 = 0.02744 -0.00285 0.00445 0.00446 V05 6 0.438735 0.438735 0.323213 10.50000 0.02907 0.02907 = 0.03541 -0.01053 -0.01053 0.00727 V06 6 0.609422 0.609422 0.530383 10.50000 0.02646 0.02646 = 0.06201 -0.00490 -0.00490 -0.00521 V1 6 0.514436 0.514436 0.269457 10.50000 0.05002 0.05002 = 0.03330 0.00189 0.00189 0.01200 NI00 4 0.490930 0.271175 0.199120 11.00000 0.13088 0.05699 = 0.09995 -0.04936 0.00849 0.02018 CL09 2 0.500000 0.500000 0.500000 10.25000 0.03664 0.03664 = 0.04169 0.00058 0.00058 0.00506 O00A 5 0.631240 0.557161 0.451840 11.00000 0.01710 0.01594 = 0.04798 0.00170 0.00154 -0.00170 O00B 5 0.632497 0.450460 0.435093 11.00000 0.02304 0.02406 = 0.03208 0.00106 -0.00092 0.00614 O00C 5 0.620287 0.440070 0.586569 11.00000 0.02160 0.02369 = 0.03715 0.00053 -0.00590 0.00288 O00D 5 0.379519 0.451857 0.397684 11.00000 0.01958 0.02569 = 0.04094 -0.00377 -0.00193 0.00506 O00E 5 0.584663 0.513083 0.323179 11.00000 0.02596 0.02692 = 0.03070 0.00288 0.00696 0.00544 O00F 5 0.513828 0.439347 0.300353 11.00000 0.02907 0.03416 = 0.02548 -0.00572 -0.00285 0.00757 O00G 5 0.711293 0.498058 0.534815 11.00000 0.01590 0.03872 = 0.05945 0.00188 -0.00323 -0.00060 O00H 5 0.622675 0.409679 0.279396 11.00000 0.04818 0.04255 = 0.04745 -0.00410 0.01094 0.01601 O00I 5 0.657446 0.342554 0.500000 10.50000 0.03068 0.03068 = 0.04862 0.00247 0.00247 0.00746 O00J 5 0.620773 0.620773 0.313986 10.50000 0.03685 0.03685 = 0.06413 0.01447 0.01447 0.00802 O00K 5 0.410551 0.410551 0.245585 10.50000 0.04223 0.04223 = 0.05745 -0.02259 -0.02259 0.01421 O00L 5 0.655566 0.655566 0.543591 10.50000 0.03846 0.03846 = 0.09013 -0.00737 -0.00737 -0.00771 O00M 5 0.521327 0.521327 0.171351 10.50000 0.08234 0.08234 = 0.03604 0.00170 0.00170 0.02870 N00O 3 0.557948 0.248004 0.125199 11.00000 0.10190 0.07329 = 0.09287 -0.05692 0.00054 0.00477 N00Q 3 0.427459 0.288757 0.280245 11.00000 0.14549 0.04396 = 0.12395 -0.04764 0.01974 0.00111 N00R 3 0.554004 0.293729 0.279386 11.00000 0.15751 0.09600 = 0.10387 -0.06700 0.01944 -0.06206 N00S 3 0.484935 0.194245 0.254415 11.00000 0.08236 0.04924 = 0.14920 -0.04588 -0.03112 0.00263 N00T 3 0.430878 0.252749 0.110301 11.00000 0.14078 0.19033 = 0.10992 -0.08545 -0.03090 0.11565 C00U 1 0.450024 0.197526 0.327001 11.00000 0.08466 0.05245 = 0.13913 -0.04634 -0.01008 -0.00991 N00V 3 0.489464 0.349126 0.144024 11.00000 0.26489 0.08977 = 0.13449 0.01527 0.09026 0.10391 C00W 1 0.404955 0.235935 0.312162 11.00000 0.09549 0.07598 = 0.15858 -0.05631 0.00606 -0.00170 C00X 1 0.606539 0.273281 0.247975 11.00000 0.14445 0.17354 = 0.08968 -0.07073 0.00663 -0.03847 C00Z 1 0.607305 0.274216 0.158294 11.00000 0.12395 0.12022 = 0.13246 -0.06403 0.03580 -0.05443 C012 1 0.461795 0.345232 0.063725 11.00000 0.25754 0.23522 = 0.22832 0.08656 0.05465 0.14497 C013 1 0.416502 0.305807 0.068110 11.00000 0.21615 0.27677 = 0.14027 -0.02753 -0.00142 0.19035 O1 5 0.670659 0.232810 0.446788 11.00000 0.08628 0.05930 = 0.08235 -0.00913 -0.00671 0.01436 O3 5 0.575094 0.436588 0.082360 11.00000 0.18177 0.19677 = 0.13168 -0.05969 0.01632 0.07335 O4 5 0.579658 0.178484 0.402094 11.00000 0.14344 0.24685 = 0.32186 0.11379 -0.08796 -0.07947 O2 5 0.750000 0.250000 0.330706 0.31240 0.05201 0.14840 = 0.03128 0.00000 0.00000 -0.00676 HKLF 5 REM niv-1-2_100k_02_tp_twin1_hklf4_a.res in P4(2)/ncm REM wR2 = 0.2722, GooF = S = 1.023, Restrained GooF = 1.024 for all data REM R1 = 0.0972 for 12157 Fo > 4sig(Fo) and 0.1496 for all 19047 data REM 304 parameters refined using 12 restraints END WGHT 0.1180 94.0149 REM Highest difference peak 1.353, deepest hole -0.727, 1-sigma level 0.187 Q1 1 0.5030 0.2585 0.2365 11.00000 0.05 1.35 Q2 1 0.2957 0.2957 0.1973 10.50000 0.05 1.30 Q3 1 0.2832 0.2832 0.2150 10.50000 0.05 1.29 Q4 1 0.7252 0.7252 0.6372 10.50000 0.05 1.06 Q5 1 0.5025 0.2866 0.1774 11.00000 0.05 0.96 Q6 1 0.7006 0.6777 0.3749 11.00000 0.05 0.93 Q7 1 0.6401 0.5199 0.4834 11.00000 0.05 0.92 Q8 1 0.5841 0.4242 0.3941 11.00000 0.05 0.90 Q9 1 0.4224 0.4224 0.3353 10.50000 0.05 0.86 Q10 1 0.4623 0.2722 0.2050 11.00000 0.05 0.85 Q11 1 0.5965 0.5837 0.3174 11.00000 0.05 0.75 Q12 1 0.6208 0.4227 0.4587 11.00000 0.05 0.75 Q13 1 0.7406 0.7406 0.3574 10.50000 0.05 0.73 Q14 1 0.2623 0.2623 0.1759 10.50000 0.05 0.69 Q15 1 0.6232 0.4204 0.5442 11.00000 0.05 0.67 Q16 1 0.5951 0.4179 0.3049 11.00000 0.05 0.61 Q17 1 0.7589 0.7026 0.5517 11.00000 0.05 0.59 Q18 1 0.7198 0.7198 0.4368 10.50000 0.05 0.59 Q19 1 0.5673 0.1993 0.4133 11.00000 0.05 0.58 Q20 1 0.4162 0.4162 0.2780 10.50000 0.05 0.58 Q21 1 0.5193 0.2987 0.2410 11.00000 0.05 0.58 Q22 1 0.6176 0.3588 0.5369 11.00000 0.05 0.57 Q23 1 0.5577 0.2737 0.3309 11.00000 0.05 0.57 Q24 1 0.4800 0.2000 0.3696 11.00000 0.05 0.56 Q25 1 0.5791 0.6045 0.4126 11.00000 0.05 0.55 Q26 1 0.5026 0.5132 0.5384 11.00000 0.05 0.54 Q27 1 0.6262 0.5855 0.4859 11.00000 0.05 0.53 Q28 1 0.6290 0.5152 0.5636 11.00000 0.05 0.53 Q29 1 0.7599 0.2625 0.3578 11.00000 0.05 0.52 Q30 1 0.3826 0.4237 0.4222 11.00000 0.05 0.52 Q31 1 0.6732 0.4970 0.4852 11.00000 0.05 0.52 Q32 1 0.4821 0.4573 0.3371 11.00000 0.05 0.52 Q33 1 0.5616 0.4509 0.3280 11.00000 0.05 0.50 Q34 1 0.4998 0.1802 0.2963 11.00000 0.05 0.50 Q35 1 0.4607 0.3402 0.1191 11.00000 0.05 0.50 Q36 1 0.5614 0.3043 0.1169 11.00000 0.05 0.50 Q37 1 0.5971 0.4758 0.0596 11.00000 0.05 0.50 Q38 1 0.5823 0.4651 0.3020 11.00000 0.05 0.50 Q39 1 0.6401 0.4617 0.5611 11.00000 0.05 0.49 ; _shelx_res_checksum 14215 _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+1/2, -y+1/2, z' '-y+1/2, x, z+1/2' 'y, -x+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z' '-y, -x, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z-1/2' '-y, x-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z' 'y, x, 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group V01 V 0.64634(8) 0.49861(8) 0.52334(13) 0.0270(5) Uani 1 1 d . . . . . V02 V 0.61141(8) 0.38859(8) 0.500000 0.0305(7) Uani 1 2 d S T P . . V03 V 0.58381(9) 0.58381(9) 0.37020(19) 0.0303(7) Uani 1 2 d S T P . . V04 V 0.58468(8) 0.43760(8) 0.34625(12) 0.0271(5) Uani 1 1 d . . . . . V05 V 0.43874(9) 0.43874(9) 0.32321(19) 0.0312(7) Uani 1 2 d S T P . . V06 V 0.60942(9) 0.60942(9) 0.5304(2) 0.0383(8) Uani 1 2 d S T P . . V1 V 0.51444(12) 0.51444(12) 0.2695(2) 0.0444(9) Uani 1 2 d S T P . . Ni00 Ni 0.49093(14) 0.27118(11) 0.19912(19) 0.0959(11) Uani 1 1 d D . . . . Cl09 Cl 0.500000 0.500000 0.500000 0.0383(14) Uani 1 4 d S T P . . O00A O 0.6312(3) 0.5572(3) 0.4518(5) 0.0270(19) Uani 1 1 d . . . . . O00B O 0.6325(3) 0.4505(3) 0.4351(5) 0.0264(18) Uani 1 1 d . . . . . O00C O 0.6203(3) 0.4401(3) 0.5866(5) 0.0275(18) Uani 1 1 d . . . . . O00D O 0.3795(3) 0.4519(3) 0.3977(5) 0.0287(19) Uani 1 1 d . . . . . O00E O 0.5847(3) 0.5131(3) 0.3232(5) 0.0279(18) Uani 1 1 d . . . . . O00F O 0.5138(3) 0.4393(3) 0.3004(5) 0.0296(19) Uani 1 1 d . . . . . O00G O 0.7113(3) 0.4981(4) 0.5348(6) 0.038(2) Uani 1 1 d . . . . . O00H O 0.6227(4) 0.4097(4) 0.2794(6) 0.046(2) Uani 1 1 d . . . . . O00I O 0.6574(3) 0.3426(3) 0.500000 0.037(3) Uani 1 2 d S T P . . O00J O 0.6208(4) 0.6208(4) 0.3140(9) 0.046(4) Uani 1 2 d S T P . . O00K O 0.4106(4) 0.4106(4) 0.2456(9) 0.047(4) Uani 1 2 d S T P . . O00L O 0.6556(4) 0.6556(4) 0.5436(10) 0.056(4) Uani 1 2 d S T P . . O00M O 0.5213(6) 0.5213(6) 0.1714(9) 0.067(5) Uani 1 2 d S T P . . N00O N 0.5579(7) 0.2480(7) 0.1252(11) 0.089(6) Uani 1 1 d D . . . . N00Q N 0.4275(8) 0.2888(7) 0.2802(12) 0.104(7) Uani 1 1 d D . . . . N00R N 0.5540(9) 0.2937(8) 0.2794(12) 0.119(8) Uani 1 1 d D . . . . N00S N 0.4849(7) 0.1942(6) 0.2544(13) 0.094(6) Uani 1 1 d D . . . . N00T N 0.4309(9) 0.2527(11) 0.1103(13) 0.147(12) Uani 1 1 d D . . . . C00U C 0.4500(9) 0.1975(8) 0.3270(16) 0.092(7) Uani 1 1 d D . . . . N00V N 0.4895(14) 0.3491(9) 0.1440(18) 0.163(14) Uani 1 1 d D . . . . C00W C 0.4050(11) 0.2359(9) 0.3122(17) 0.110(9) Uani 1 1 d D . . . . C00X C 0.6065(12) 0.2733(14) 0.2480(17) 0.136(12) Uani 1 1 d D . . . . C00Z C 0.6073(11) 0.2742(12) 0.1583(18) 0.126(11) Uani 1 1 d D . . . . C012 C 0.462(2) 0.345(2) 0.064(3) 0.24(4) Uani 1 1 d D . . . . C013 C 0.417(2) 0.306(2) 0.068(3) 0.21(3) Uani 1 1 d D . . . . O1 O 0.6707(6) 0.2328(5) 0.4468(8) 0.076(4) Uani 1 1 d . . . . . O3 O 0.5751(10) 0.4366(11) 0.0824(14) 0.170(10) Uani 1 1 d . . . . . O4 O 0.5797(11) 0.1785(14) 0.402(2) 0.237(17) Uani 1 1 d . . . . . O2 O 0.750000 0.250000 0.3307(15) 0.077(13) Uani 0.62(5) 2 d S T . . . 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 V01 0.0151(9) 0.0263(11) 0.0395(12) -0.0020(9) -0.0004(9) 0.0006(8) V02 0.0260(10) 0.0260(10) 0.0393(17) -0.0003(10) -0.0003(10) 0.0069(12) V03 0.0241(9) 0.0241(9) 0.0429(18) 0.0102(10) 0.0102(10) 0.0047(12) V04 0.0271(11) 0.0268(11) 0.0274(11) -0.0028(8) 0.0044(8) 0.0045(9) V05 0.0291(10) 0.0291(10) 0.0354(17) -0.0105(10) -0.0105(10) 0.0073(13) V06 0.0265(10) 0.0265(10) 0.062(2) -0.0049(10) -0.0049(10) -0.0052(13) V1 0.0500(13) 0.0500(13) 0.0333(19) 0.0019(12) 0.0019(12) 0.0120(17) Ni00 0.131(3) 0.0570(16) 0.100(2) -0.0494(15) 0.0085(18) 0.0202(16) Cl09 0.037(2) 0.037(2) 0.042(4) 0.001(2) 0.001(2) 0.005(3) O00A 0.017(4) 0.016(4) 0.048(5) 0.002(4) 0.002(4) -0.002(3) O00B 0.023(4) 0.024(4) 0.032(5) 0.001(4) -0.001(3) 0.006(3) O00C 0.022(4) 0.024(4) 0.037(5) 0.001(4) -0.006(3) 0.003(3) O00D 0.020(4) 0.026(5) 0.041(5) -0.004(4) -0.002(3) 0.005(3) O00E 0.026(4) 0.027(4) 0.031(5) 0.003(3) 0.007(4) 0.005(4) O00F 0.029(5) 0.034(5) 0.025(4) -0.006(4) -0.003(3) 0.008(4) O00G 0.016(4) 0.039(5) 0.059(6) 0.002(4) -0.003(4) -0.001(4) O00H 0.048(6) 0.043(6) 0.047(6) -0.004(4) 0.011(5) 0.016(5) O00I 0.031(4) 0.031(4) 0.049(8) 0.002(4) 0.002(4) 0.007(5) O00J 0.037(5) 0.037(5) 0.064(9) 0.014(5) 0.014(5) 0.008(6) O00K 0.042(5) 0.042(5) 0.057(9) -0.023(5) -0.023(5) 0.014(6) O00L 0.038(5) 0.038(5) 0.090(12) -0.007(5) -0.007(5) -0.008(6) O00M 0.082(8) 0.082(8) 0.036(9) 0.002(6) 0.002(6) 0.029(10) N00O 0.102(13) 0.073(11) 0.093(13) -0.057(10) 0.001(10) 0.005(10) N00Q 0.145(19) 0.044(10) 0.124(16) -0.048(10) 0.020(13) 0.001(10) N00R 0.16(2) 0.096(15) 0.104(15) -0.067(12) 0.019(14) -0.062(14) N00S 0.082(12) 0.049(9) 0.149(18) -0.046(11) -0.031(12) 0.003(8) N00T 0.14(2) 0.19(3) 0.110(17) -0.085(17) -0.031(14) 0.116(19) C00U 0.085(16) 0.052(12) 0.14(2) -0.046(13) -0.010(15) -0.010(11) N00V 0.26(4) 0.090(16) 0.13(2) 0.015(15) 0.09(2) 0.10(2) C00W 0.095(18) 0.076(17) 0.16(3) -0.056(17) 0.006(16) -0.002(13) C00X 0.14(3) 0.17(3) 0.090(19) -0.07(2) 0.007(18) -0.04(2) C00Z 0.12(2) 0.12(2) 0.13(2) -0.064(19) 0.036(18) -0.054(18) C012 0.26(7) 0.24(7) 0.23(6) 0.09(5) 0.05(6) 0.14(6) C013 0.22(5) 0.28(7) 0.14(3) -0.03(4) 0.00(3) 0.19(5) O1 0.086(9) 0.059(8) 0.082(9) -0.009(7) -0.007(7) 0.014(7) O3 0.18(2) 0.20(2) 0.132(17) -0.060(17) 0.016(16) 0.073(18) O4 0.14(2) 0.25(3) 0.32(4) 0.11(3) -0.09(2) -0.08(2) O2 0.052(18) 0.15(3) 0.031(16) 0.000 0.000 -0.007(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' Cl Cl 0.1484 0.1585 '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' Ni Ni 0.3393 1.1124 '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 V02 V01 V06 143.71(10) . . ? O00A V01 V02 124.9(3) . . ? O00A V01 V06 41.1(3) . . ? O00A V01 O00B 87.4(3) . . ? O00B V01 V02 42.2(2) . . ? O00B V01 V06 124.1(3) . . ? O00C V01 V02 41.9(2) . . ? O00C V01 V06 126.2(3) . . ? O00C V01 O00A 148.8(3) . . ? O00C V01 O00B 83.9(3) . . ? O00C V01 O00D 89.5(4) . 9_666 ? O00D V01 V02 126.8(3) 9_666 . ? O00D V01 V06 42.1(3) 9_666 . ? O00D V01 O00A 83.1(4) 9_666 . ? O00D V01 O00B 150.0(3) 9_666 . ? O00G V01 V02 107.8(3) . . ? O00G V01 V06 108.5(3) . . ? O00G V01 O00A 105.9(4) . . ? O00G V01 O00B 105.2(4) . . ? O00G V01 O00C 105.3(4) . . ? O00G V01 O00D 104.8(4) . 9_666 ? V01 V02 V01 125.77(13) . 8_666 ? V01 V02 V04 78.15(7) 8_666 8_666 ? V01 V02 V04 77.95(7) . 8_666 ? V01 V02 V04 78.15(7) . . ? V01 V02 V04 77.96(7) 8_666 . ? V04 V02 V04 125.97(12) 8_666 . ? O00B V02 V01 114.4(2) . 8_666 ? O00B V02 V01 41.6(2) . . ? O00B V02 V01 41.6(2) 8_666 8_666 ? O00B V02 V01 114.4(2) 8_666 . ? O00B V02 V04 40.8(2) . . ? O00B V02 V04 115.1(2) . 8_666 ? O00B V02 V04 40.8(2) 8_666 8_666 ? O00B V02 V04 115.1(2) 8_666 . ? O00B V02 O00B 137.0(5) . 8_666 ? O00C V02 V01 113.9(3) . 8_666 ? O00C V02 V01 113.9(3) 8_666 . ? O00C V02 V01 41.0(2) 8_666 8_666 ? O00C V02 V01 41.0(2) . . ? O00C V02 V04 40.7(2) 8_666 . ? O00C V02 V04 40.7(2) . 8_666 ? O00C V02 V04 114.2(3) 8_666 8_666 ? O00C V02 V04 114.2(3) . . ? O00C V02 O00B 82.5(4) . . ? O00C V02 O00B 81.3(3) 8_666 . ? O00C V02 O00B 81.3(3) . 8_666 ? O00C V02 O00B 82.5(4) 8_666 8_666 ? O00C V02 O00C 134.8(5) . 8_666 ? O00I V02 V01 117.11(6) . 8_666 ? O00I V02 V01 117.11(6) . . ? O00I V02 V04 117.02(6) . 8_666 ? O00I V02 V04 117.02(6) . . ? O00I V02 O00B 111.5(2) . . ? O00I V02 O00B 111.5(2) . 8_666 ? O00I V02 O00C 112.6(2) . 8_666 ? O00I V02 O00C 112.6(2) . . ? V06 V03 V1 143.25(14) . . ? O00A V03 V06 42.7(2) 16 . ? O00A V03 V06 42.7(2) . . ? O00A V03 V1 124.2(2) . . ? O00A V03 V1 124.2(2) 16 . ? O00A V03 O00A 85.1(5) . 16 ? O00A V03 O00E 148.6(4) . 16 ? O00A V03 O00E 88.3(3) 16 16 ? O00A V03 O00E 88.3(3) . . ? O00A V03 O00E 148.6(4) 16 . ? O00E V03 V06 126.2(3) 16 . ? O00E V03 V06 126.2(3) . . ? O00E V03 V1 40.8(2) 16 . ? O00E V03 V1 40.8(3) . . ? O00E V03 O00E 81.5(5) . 16 ? O00J V03 V06 107.5(6) . . ? O00J V03 V1 109.3(6) . . ? O00J V03 O00A 105.4(5) . 16 ? O00J V03 O00A 105.4(5) . . ? O00J V03 O00E 106.0(5) . . ? O00J V03 O00E 106.0(5) . 16 ? V1 V04 V02 143.54(11) . . ? O00B V04 V02 41.4(2) . . ? O00B V04 V1 127.3(3) . . ? O00C V04 V02 41.2(2) 8_666 . ? O00C V04 V1 124.1(3) 8_666 . ? O00C V04 O00B 82.4(3) 8_666 . ? O00E V04 V02 125.8(3) . . ? O00E V04 V1 42.5(3) . . ? O00E V04 O00B 89.7(4) . . ? O00E V04 O00C 148.1(3) . 8_666 ? O00E V04 O00F 84.1(4) . . ? O00F V04 V02 124.8(3) . . ? O00F V04 V1 41.7(3) . . ? O00F V04 O00B 150.3(3) . . ? O00F V04 O00C 87.7(4) . 8_666 ? O00H V04 V02 107.4(4) . . ? O00H V04 V1 109.0(4) . . ? O00H V04 O00B 104.3(4) . . ? O00H V04 O00C 105.7(4) . 8_666 ? O00H V04 O00E 106.2(4) . . ? O00H V04 O00F 105.4(5) . . ? V1 V05 V06 143.29(15) . 9_666 ? O00D V05 V06 40.5(2) . 9_666 ? O00D V05 V06 40.5(2) 16 9_666 ? O00D V05 V1 126.6(3) 16 . ? O00D V05 V1 126.6(3) . . ? O00D V05 O00D 81.0(5) . 16 ? O00F V05 V06 124.2(3) 16 9_666 ? O00F V05 V06 124.2(3) . 9_666 ? O00F V05 V1 43.5(3) . . ? O00F V05 V1 43.5(3) 16 . ? O00F V05 O00D 88.4(4) . 16 ? O00F V05 O00D 149.7(4) 16 16 ? O00F V05 O00D 88.4(4) 16 . ? O00F V05 O00D 149.7(4) . . ? O00F V05 O00F 86.8(5) . 16 ? O00K V05 V06 108.2(6) . 9_666 ? O00K V05 V1 108.5(6) . . ? O00K V05 O00D 104.9(5) . . ? O00K V05 O00D 104.9(5) . 16 ? O00K V05 O00F 105.2(5) . 16 ? O00K V05 O00F 105.2(5) . . ? V01 V06 V01 126.66(13) 16 . ? V01 V06 V05 77.29(9) . 9_666 ? V01 V06 V05 77.29(9) 16 9_666 ? V03 V06 V01 79.60(8) . 16 ? V03 V06 V01 79.60(8) . . ? V03 V06 V05 126.93(14) . 9_666 ? O00A V06 V01 116.8(3) 16 . ? O00A V06 V01 116.8(3) . 16 ? O00A V06 V01 41.0(2) . . ? O00A V06 V01 41.0(2) 16 16 ? O00A V06 V03 42.6(2) 16 . ? O00A V06 V03 42.6(2) . . ? O00A V06 V05 113.9(3) 16 9_666 ? O00A V06 V05 113.9(3) . 9_666 ? O00A V06 O00A 84.9(5) 16 . ? O00A V06 O00D 137.1(4) . 8_666 ? O00A V06 O00D 137.1(4) 16 9_666 ? O00A V06 O00D 81.9(3) . 9_666 ? O00A V06 O00D 81.9(3) 16 8_666 ? O00D V06 V01 113.8(3) 9_666 16 ? O00D V06 V01 113.8(3) 8_666 . ? O00D V06 V01 41.0(2) 8_666 16 ? O00D V06 V01 41.0(2) 9_666 . ? O00D V06 V03 116.1(3) 9_666 . ? O00D V06 V03 116.1(3) 8_666 . ? O00D V06 V05 40.4(2) 8_666 9_666 ? O00D V06 V05 40.4(2) 9_666 9_666 ? O00D V06 O00D 80.7(5) 8_666 9_666 ? O00L V06 V01 116.64(7) . 16 ? O00L V06 V01 116.64(7) . . ? O00L V06 V03 116.3(6) . . ? O00L V06 V05 116.8(6) . 9_666 ? O00L V06 O00A 111.6(5) . . ? O00L V06 O00A 111.6(5) . 16 ? O00L V06 O00D 111.2(5) . 8_666 ? O00L V06 O00D 111.2(5) . 9_666 ? V04 V1 V03 77.22(9) . . ? V04 V1 V03 77.22(9) 16 . ? V04 V1 V04 126.80(15) . 16 ? V05 V1 V03 126.52(15) . . ? V05 V1 V04 79.56(9) . 16 ? V05 V1 V04 79.56(9) . . ? O00E V1 V03 39.8(2) . . ? O00E V1 V03 39.8(2) 16 . ? O00E V1 V04 113.1(3) 16 . ? O00E V1 V04 113.1(3) . 16 ? O00E V1 V04 41.2(2) 16 16 ? O00E V1 V04 41.2(2) . . ? O00E V1 V05 115.8(3) 16 . ? O00E V1 V05 115.8(3) . . ? O00E V1 O00E 79.6(5) . 16 ? O00F V1 V03 114.3(3) . . ? O00F V1 V03 114.3(3) 16 . ? O00F V1 V04 117.2(3) 16 . ? O00F V1 V04 41.3(2) . . ? O00F V1 V04 117.2(3) . 16 ? O00F V1 V04 41.3(2) 16 16 ? O00F V1 V05 42.6(3) 16 . ? O00F V1 V05 42.6(3) . . ? O00F V1 O00E 82.4(3) . . ? O00F V1 O00E 137.1(4) . 16 ? O00F V1 O00E 137.1(4) 16 . ? O00F V1 O00E 82.4(3) 16 16 ? O00F V1 O00F 85.0(5) . 16 ? O00M V1 V03 116.4(7) . . ? O00M V1 V04 116.55(8) . 16 ? O00M V1 V04 116.55(8) . . ? O00M V1 V05 117.1(7) . . ? O00M V1 O00E 111.4(6) . 16 ? O00M V1 O00E 111.4(6) . . ? O00M V1 O00F 111.4(6) . 16 ? O00M V1 O00F 111.4(6) . . ? N00O Ni00 N00T 94.6(7) . . ? N00Q Ni00 N00O 174.6(8) . . ? N00Q Ni00 N00R 94.9(9) . . ? N00Q Ni00 N00S 81.6(7) . . ? N00Q Ni00 N00T 88.5(8) . . ? N00Q Ni00 N00V 94.5(8) . . ? N00R Ni00 N00O 82.3(8) . . ? N00R Ni00 N00T 174.9(11) . . ? N00R Ni00 N00V 92.7(13) . . ? N00S Ni00 N00O 93.7(8) . . ? N00S Ni00 N00R 90.7(8) . . ? N00S Ni00 N00T 93.6(10) . . ? N00S Ni00 N00V 175.0(11) . . ? N00V Ni00 N00O 90.4(8) . . ? N00V Ni00 N00T 83.2(13) . . ? V01 O00A V03 145.5(4) . . ? V01 O00A V06 97.9(4) . . ? V03 O00A V06 94.8(3) . . ? V01 O00B V02 96.2(4) . . ? V04 O00B V01 143.3(4) . . ? V04 O00B V02 97.8(4) . . ? V01 O00C V02 97.1(4) . . ? V01 O00C V04 145.0(4) . 8_666 ? V04 O00C V02 98.2(4) 8_666 . ? V01 O00D V05 143.0(5) 9_666 . ? V01 O00D V06 96.9(4) 9_666 9_666 ? V05 O00D V06 99.1(3) . 9_666 ? V03 O00E V1 99.4(4) . . ? V04 O00E V03 144.1(5) . . ? V04 O00E V1 96.3(4) . . ? V04 O00F V1 97.0(4) . . ? V05 O00F V04 144.7(5) . . ? V05 O00F V1 94.0(4) . . ? C00Z N00O Ni00 107.7(13) . . ? C00W N00Q Ni00 108.7(12) . . ? C00X N00R Ni00 109.1(13) . . ? C00U N00S Ni00 110.2(12) . . ? C013 N00T Ni00 107(3) . . ? C00W C00U N00S 109(2) . . ? C012 N00V Ni00 109(3) . . ? C00U C00W N00Q 110(2) . . ? N00R C00X C00Z 111(3) . . ? N00O C00Z C00X 111(2) . . ? C013 C012 N00V 110(5) . . ? C012 C013 N00T 114(4) . . ? 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 V01 V02 2.872(2) . ? V01 V06 2.881(2) . ? V01 O00A 1.907(8) . ? V01 O00B 1.919(8) . ? V01 O00C 1.898(8) . ? V01 O00D 1.904(8) 9_666 ? V01 O00G 1.612(8) . ? V02 V04 2.906(3) 8_666 ? V02 V04 2.906(3) . ? V02 O00B 1.940(8) 8_666 ? V02 O00B 1.940(8) . ? V02 O00C 1.933(8) 8_666 ? V02 O00C 1.933(8) . ? V02 O00I 1.605(12) . ? V03 V06 2.812(5) . ? V03 V1 2.943(5) . ? V03 O00A 1.909(8) 16 ? V03 O00A 1.909(8) . ? V03 O00E 1.911(8) 16 ? V03 O00E 1.911(8) . ? V03 O00J 1.592(13) . ? V04 V1 2.867(3) . ? V04 O00B 1.918(8) . ? V04 O00C 1.913(9) 8_666 ? V04 O00E 1.900(8) . ? V04 O00F 1.907(8) . ? V04 O00H 1.609(9) . ? V05 V06 2.960(5) 9_666 ? V05 V1 2.786(5) . ? V05 O00D 1.942(8) 16 ? V05 O00D 1.942(8) . ? V05 O00F 1.890(9) . ? V05 O00F 1.890(9) 16 ? V05 O00K 1.623(13) . ? V06 O00A 1.913(8) 16 ? V06 O00A 1.913(8) . ? V06 O00D 1.947(8) 8_666 ? V06 O00D 1.947(8) 9_666 ? V06 O00L 1.623(14) . ? V1 O00E 1.949(9) 16 ? V1 O00E 1.949(9) . ? V1 O00F 1.921(9) 16 ? V1 O00F 1.921(9) . ? V1 O00M 1.651(16) . ? Ni00 N00O 2.138(16) . ? Ni00 N00Q 2.112(18) . ? Ni00 N00R 2.124(19) . ? Ni00 N00S 2.113(18) . ? Ni00 N00T 2.14(2) . ? Ni00 N00V 2.13(2) . ? N00O C00Z 1.48(2) . ? N00Q C00W 1.51(3) . ? N00R C00X 1.48(3) . ? N00S C00U 1.49(2) . ? N00T C013 1.53(3) . ? C00U C00W 1.48(3) . ? N00V C012 1.50(4) . ? C00X C00Z 1.49(4) . ? C012 C013 1.48(7) . ? 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 V02 V01 O00C V04 -115.3(9) . . . 8_666 ? V02 V04 O00E V03 -17.3(9) . . . . ? V02 V04 O00E V1 -132.9(2) . . . . ? V06 V01 O00C V02 132.8(2) . . . . ? V06 V01 O00C V04 17.5(9) . . . 8_666 ? V06 V05 O00F V04 -25.8(10) 9_666 . . . ? V06 V05 O00F V1 -133.8(2) 9_666 . . . ? V1 V04 O00E V03 115.6(9) . . . . ? V1 V05 O00F V04 108.0(9) . . . . ? Ni00 N00O C00Z C00X 39(3) . . . . ? Ni00 N00Q C00W C00U 40(2) . . . . ? Ni00 N00R C00X C00Z 34(3) . . . . ? Ni00 N00S C00U C00W 36.6(18) . . . . ? Ni00 N00T C013 C012 31(4) . . . . ? Ni00 N00V C012 C013 36(5) . . . . ? O00A V01 O00C V02 79.2(7) . . . . ? O00A V01 O00C V04 -36.2(12) . . . 8_666 ? O00B V01 O00C V02 4.3(3) . . . . ? O00B V01 O00C V04 -111.0(8) . . . 8_666 ? O00B V04 O00E V03 -39.0(8) . . . . ? O00B V04 O00E V1 -154.6(4) . . . . ? O00C V04 O00E V03 36.1(12) 8_666 . . . ? O00C V04 O00E V1 -79.6(7) 8_666 . . . ? O00D V01 O00C V02 155.0(4) 9_666 . . . ? O00D V01 O00C V04 39.6(8) 9_666 . . 8_666 ? O00D V05 O00F V04 23.0(13) . . . . ? O00D V05 O00F V04 -45.9(8) 16 . . . ? O00D V05 O00F V1 -85.0(8) . . . . ? O00D V05 O00F V1 -153.9(4) 16 . . . ? O00F V04 O00E V03 111.9(8) . . . . ? O00F V04 O00E V1 -3.7(4) . . . . ? O00F V05 O00F V04 104.2(8) 16 . . . ? O00F V05 O00F V1 -3.8(5) 16 . . . ? O00G V01 O00C V02 -99.8(5) . . . . ? O00G V01 O00C V04 144.9(8) . . . 8_666 ? O00H V04 O00E V03 -143.8(8) . . . . ? O00H V04 O00E V1 100.6(5) . . . . ? O00K V05 O00F V04 -150.9(9) . . . . ? O00K V05 O00F V1 101.0(5) . . . . ? N00R C00X C00Z N00O -50(3) . . . . ? N00S C00U C00W N00Q -51(2) . . . . ? N00V C012 C013 N00T -46(6) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.499(3) 2 0.501(3)