#------------------------------------------------------------------------------ #$Date: 2020-05-23 04:22:48 +0300 (Sat, 23 May 2020) $ #$Revision: 252294 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240568.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_7240568 loop_ _publ_author_name 'Dou, Ming-Yu' 'Zhong, Dan-Dan' 'Huang, Xianqiang' 'Yang, Guo-Yu' _publ_section_title ; Imidazole-induced self-assembly of polyoxovanadate cluster organic framework for efficient Knoevenagel condensation under mild conditions ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D0CE00660B _journal_year 2020 _chemical_formula_sum 'C20 H54 N8 Ni2 O38 V10' _chemical_formula_weight 1641.53 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-04-26 deposited with the CCDC. 2020-05-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.696(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 11.8760(9) _cell_length_b 12.2282(11) _cell_length_c 17.4796(14) _cell_measurement_reflns_used 1024 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 26.888 _cell_measurement_theta_min 2.409 _cell_volume 2485.7(4) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1355 _diffrn_reflns_av_unetI/netI 0.1343 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 11767 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.011 _diffrn_reflns_theta_max 25.011 _diffrn_reflns_theta_min 2.308 _exptl_absorpt_coefficient_mu 2.639 _exptl_absorpt_correction_T_max 0.647 _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour GREEN _exptl_crystal_density_diffrn 2.193 _exptl_crystal_description BLOCK _exptl_crystal_F_000 1640 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _refine_diff_density_max 1.583 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.229 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 354 _refine_ls_number_reflns 4369 _refine_ls_number_restraints 19 _refine_ls_restrained_S_all 0.999 _refine_ls_R_factor_all 0.1328 _refine_ls_R_factor_gt 0.0856 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1370P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2204 _refine_ls_wR_factor_ref 0.2432 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2657 _reflns_number_total 4369 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00660b2.cif _cod_data_source_block 180718a _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7240568 _shelx_shelxl_version_number 2018/3 _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_min 0.594 _shelx_estimated_absorpt_t_max 0.648 _shelx_res_file ; TITL 180718a in P2(1)/n 180718a.res created by SHELXL-2018/3 at 07:57:40 on 11-Oct-2019 CELL 0.71073 11.8760 12.2282 17.4796 90.000 101.696 90.000 ZERR 2.00 0.0009 0.0011 0.0014 0.000 0.003 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O V Ni UNIT 40 108 16 76 20 4 OMIT -1.00 50.04 L.S. 8 ACTA BOND $h FMAP 2 PLAN 20 HTAB C9 O4_$11 HTAB C7 O2_$11 EQIV $11 -x+1/2, y+1/2, -z+3/2 HTAB C6 O9 HTAB C6 O8 HTAB C5 O12_$1 HTAB C4 O19_$10 EQIV $10 -x+2, -y, -z+1 HTAB C4 O4_$9 EQIV $9 x+1/2, -y+1/2, z-1/2 HTAB C3 O15_$8 EQIV $8 -x+2, -y+1, -z+1 HTAB C2 O1_$7 HTAB C1 O1_$1 HTAB N4 O3_$7 EQIV $7 x+1, y, z HTAB O19 O14_$1 EQIV $1 -x+1, -y+1, -z+1 HTAB O19 O6_$6 EQIV $6 -x+3/2, y-1/2, -z+3/2 HTAB O18 O16_$5 HTAB O18 O10_$5 HTAB O17 O13_$5 HTAB O17 O4_$4 HTAB O16 O19_$4 HTAB O16 O12_$5 EQIV $5 -x+1, -y+2, -z+1 HTAB O15 O19_$4 EQIV $4 x, y+1, z HTAB O15 O7_$3 HTAB O15 O6_$3 EQIV $3 -x+3/2, y+1/2, -z+3/2 HTAB O15 O13_$2 EQIV $2 x+1/2, -y+3/2, z+1/2 HTAB O15 O8 isor 0.01 c2 c5 c4 size 0.22 0.20 0.18 htab dfix 1.436 c5 c4 FREE Ni1 H17C FREE V2 V3 FREE V1 V4 FREE V2 V4 FREE V1 V3 FREE V3 V5 FREE V1 V5 FREE V1 V2 TEMP 25 WGHT 0.137000 FVAR 0.03656 NI1 6 0.569329 0.955716 0.642413 11.00000 0.03331 0.01603 = 0.03331 -0.00085 0.00291 -0.00198 V1 5 0.380724 0.500517 0.532700 11.00000 0.02272 0.01588 = 0.03067 -0.00108 0.00465 -0.00052 V2 5 0.505906 0.718514 0.512252 11.00000 0.02830 0.01252 = 0.03094 -0.00054 0.00020 -0.00153 V3 5 0.612955 0.560522 0.641721 11.00000 0.03117 0.01615 = 0.02817 -0.00098 -0.00023 -0.00018 V4 5 0.279754 0.655321 0.399290 11.00000 0.02890 0.01719 = 0.03522 0.00104 0.00147 0.00221 V5 5 0.493789 0.342264 0.659624 11.00000 0.03606 0.01768 = 0.03214 0.00284 0.00617 -0.00123 O1 4 0.260440 0.566853 0.493836 11.00000 0.02223 0.02045 = 0.03732 0.00142 0.00215 0.00019 O2 4 0.354204 0.430308 0.608311 11.00000 0.03239 0.01729 = 0.04069 -0.00137 0.00991 -0.00375 O3 4 0.357051 0.381173 0.458012 11.00000 0.02466 0.01368 = 0.03005 0.00039 0.00390 0.00096 O4 4 0.448849 0.283949 0.727671 11.00000 0.05861 0.03702 = 0.03297 0.01077 0.01082 0.00004 O5 4 0.546266 0.431839 0.555912 11.00000 0.02197 0.01670 = 0.03252 0.00341 0.00526 -0.00186 O6 4 0.547988 0.476525 0.704596 11.00000 0.04400 0.01216 = 0.03235 -0.00004 -0.00100 0.00091 O7 4 0.742174 0.477467 0.652832 11.00000 0.02915 0.01525 = 0.03075 -0.00100 -0.00066 0.00232 O8 4 0.660861 0.662321 0.697172 11.00000 0.04309 0.00958 = 0.03161 -0.00618 0.00129 0.00049 O9 4 0.462175 0.617574 0.588737 11.00000 0.02713 0.01144 = 0.03283 -0.00050 0.00341 -0.00033 O10 4 0.554393 0.752587 0.423973 11.00000 0.03186 0.01812 = 0.03479 -0.00269 0.00601 -0.00240 O11 4 0.546740 0.823301 0.567868 11.00000 0.03904 0.01479 = 0.02556 0.00274 0.00489 0.00334 O12 4 0.359171 0.752474 0.473233 11.00000 0.02502 0.01426 = 0.02713 -0.00420 -0.00415 -0.00084 O13 4 0.359050 0.707625 0.327728 11.00000 0.03019 0.01824 = 0.03019 0.00236 -0.00094 0.00350 O14 4 0.158285 0.712654 0.375641 11.00000 0.03245 0.02909 = 0.04931 0.00156 -0.00315 0.01123 O15 4 0.720084 0.876197 0.688046 11.00000 0.04007 0.02004 = 0.03737 0.00955 0.00438 -0.00371 AFIX 3 H15A 2 0.709044 0.832667 0.723706 11.00000 -1.50000 H15C 2 0.770934 0.922947 0.707316 11.00000 -1.50000 AFIX 0 O16 4 0.664352 1.034205 0.569786 11.00000 0.03971 0.01975 = 0.04221 0.00183 0.00093 -0.00458 AFIX 3 H16A 2 0.686322 1.096415 0.588846 11.00000 -1.50000 H16B 2 0.722742 0.995436 0.566886 11.00000 -1.50000 AFIX 0 O17 4 0.613721 1.079518 0.722161 11.00000 0.04033 0.01531 = 0.04420 -0.00459 -0.00486 -0.00296 AFIX 3 H17C 2 0.565332 1.028369 0.708572 11.00000 -1.20000 H17D 2 0.593671 1.134808 0.693111 11.00000 -1.20000 AFIX 0 O18 4 0.426127 1.034299 0.583931 11.00000 0.04398 0.01574 = 0.03957 0.00508 -0.00017 0.00261 AFIX 3 H18B 2 0.436337 1.102980 0.588431 11.00000 -1.50000 H18C 2 0.414547 1.016680 0.535931 11.00000 -1.50000 AFIX 0 O19 4 0.892426 0.052771 0.642907 11.00000 0.05564 0.03074 = 0.04967 0.00560 0.00902 -0.00697 AFIX 3 H19C 2 0.905276 0.027861 0.689267 11.00000 -1.20000 H19B 2 0.910806 0.119961 0.643107 11.00000 -1.20000 AFIX 0 N1 3 0.472490 0.893753 0.713885 11.00000 0.03285 0.03774 = 0.03871 -0.00286 0.00807 -0.00186 N2 3 0.368349 0.783386 0.770970 11.00000 0.04798 0.03345 = 0.08199 0.00888 0.03129 0.00770 N3 3 0.983455 0.230644 0.417535 11.00000 0.05029 0.04137 = 0.12433 -0.02106 0.02407 -0.02108 N4 3 1.141332 0.315551 0.432852 11.00000 0.04213 0.06791 = 0.08915 -0.01344 0.02434 -0.01478 AFIX 43 H4 2 1.213445 0.329213 0.437544 11.00000 -1.20000 AFIX 0 C1 1 0.963115 0.331657 0.436340 11.00000 0.04821 0.06170 = 0.19432 -0.03998 0.04589 -0.01731 AFIX 43 H1 2 0.892454 0.359162 0.442431 11.00000 -1.20000 AFIX 0 C2 1 1.059319 0.387142 0.445067 11.00000 0.08812 0.08764 = 0.11914 -0.00945 0.03230 -0.00964 AFIX 43 H2 2 1.069431 0.460998 0.457231 11.00000 -1.20000 AFIX 0 C3 1 1.091055 0.223036 0.412864 11.00000 0.05068 0.06559 = 0.09389 -0.02515 0.03690 -0.02378 AFIX 43 H3 2 1.126219 0.161064 0.397609 11.00000 -1.20000 AFIX 0 C4 1 0.898479 0.143026 0.387855 11.00000 0.11601 0.09881 = 0.11785 -0.00052 0.02688 -0.02579 AFIX 23 H4A 2 0.849480 0.165979 0.339167 11.00000 -1.20000 H4B 2 0.938340 0.076848 0.378084 11.00000 -1.20000 AFIX 0 C5 1 0.832310 0.122905 0.443400 11.00000 0.18654 0.13645 = 0.15285 -0.06130 0.06680 -0.04826 AFIX 137 H5A 2 0.881841 0.107491 0.492814 11.00000 -1.50000 H5B 2 0.783083 0.061267 0.427436 11.00000 -1.50000 H5C 2 0.786283 0.186053 0.448331 11.00000 -1.50000 AFIX 0 C6 1 0.441911 0.791300 0.722676 11.00000 0.04986 0.01772 = 0.04774 0.00497 0.01124 0.00161 AFIX 43 H8 2 0.468424 0.731888 0.698183 11.00000 -1.20000 AFIX 0 C7 1 0.352605 0.888358 0.795021 11.00000 0.07964 0.05735 = 0.08177 -0.00621 0.04978 -0.00400 AFIX 43 H6 2 0.307055 0.910188 0.829724 11.00000 -1.20000 AFIX 0 C8 1 0.417116 0.953928 0.757810 11.00000 0.07446 0.03635 = 0.08059 -0.00877 0.04251 -0.00902 AFIX 43 H8A 2 0.421755 1.029639 0.762441 11.00000 -1.20000 AFIX 0 C9 1 0.318473 0.682227 0.793423 11.00000 0.06306 0.07374 = 0.12503 0.05214 0.04822 0.01941 AFIX 23 H9A 2 0.237544 0.679872 0.768946 11.00000 -1.20000 H9B 2 0.355858 0.620527 0.774123 11.00000 -1.20000 AFIX 0 C10 1 0.329986 0.671926 0.876150 11.00000 0.15936 0.07749 = 0.15041 0.04146 0.07735 0.02069 AFIX 137 H10A 2 0.410038 0.671423 0.900577 11.00000 -1.50000 H10B 2 0.294906 0.604888 0.887817 11.00000 -1.50000 H10C 2 0.292742 0.732553 0.895586 11.00000 -1.50000 AFIX 0 HKLF 4 REM 180718a in P2(1)/n REM wR2 = 0.2432, GooF = S = 0.996, Restrained GooF = 0.999 for all data REM R1 = 0.0856 for 2657 Fo > 4sig(Fo) and 0.1328 for all 4369 data REM 354 parameters refined using 19 restraints END WGHT 0.1367 0.0000 REM Instructions for potential hydrogen bonds HTAB O15 O8 HTAB O15 O13_$2 HTAB O15 O6_$3 HTAB O15 O7_$3 HTAB O15 O19_$4 HTAB O16 O12_$5 HTAB O16 O19_$4 HTAB O17 O4_$4 HTAB O17 O13_$5 HTAB O18 O10_$5 HTAB O18 O16_$5 HTAB O19 O6_$6 HTAB O19 O14_$1 HTAB N4 O3_$7 HTAB C1 O1_$1 HTAB C2 O1_$7 HTAB C3 O15_$8 HTAB C4 O4_$9 HTAB C4 O19_$10 HTAB C5 O12_$1 HTAB C6 O8 HTAB C6 O9 HTAB C7 O2_$11 HTAB C9 O4_$11 REM Highest difference peak 1.583, deepest hole -0.923, 1-sigma level 0.229 Q1 1 0.6567 0.9542 0.6239 11.00000 0.05 1.58 Q2 1 0.4612 0.4990 0.5275 11.00000 0.05 1.52 Q3 1 0.4256 0.6654 0.3425 11.00000 0.05 1.47 Q4 1 0.3637 0.6645 0.3819 11.00000 0.05 1.42 Q5 1 0.5619 0.9578 0.5751 11.00000 0.05 1.36 Q6 1 0.5841 0.7264 0.5094 11.00000 0.05 1.28 Q7 1 0.4914 0.9545 0.6532 11.00000 0.05 1.26 Q8 1 0.4739 0.7280 0.4443 11.00000 0.05 1.17 Q9 1 0.4213 0.7244 0.5086 11.00000 0.05 1.13 Q10 1 0.5201 0.3402 0.7317 11.00000 0.05 1.06 Q11 1 0.6261 0.5635 0.7150 11.00000 0.05 1.04 Q12 1 0.5321 0.5601 0.6619 11.00000 0.05 1.03 Q13 1 0.2666 0.6584 0.3288 11.00000 0.05 0.98 Q14 1 0.1930 0.6589 0.4127 11.00000 0.05 0.95 Q15 1 0.5954 0.9537 0.7084 11.00000 0.05 0.95 Q16 1 0.4146 0.3369 0.6843 11.00000 0.05 0.92 Q17 1 0.5211 0.7205 0.5890 11.00000 0.05 0.89 Q18 1 0.2997 0.4966 0.5272 11.00000 0.05 0.89 Q19 1 0.6917 0.5534 0.6501 11.00000 0.05 0.85 Q20 1 0.2210 0.4823 0.5900 11.00000 0.05 0.84 ; _shelx_res_checksum 21672 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 Ni1 Ni 0.56933(12) 0.95572(11) 0.64241(8) 0.0281(4) Uani 1 1 d . . . . . V1 V 0.38072(15) 0.50052(14) 0.53270(10) 0.0232(4) Uani 1 1 d . . . . . V2 V 0.50591(15) 0.71851(14) 0.51225(10) 0.0247(5) Uani 1 1 d . . . . . V3 V 0.61296(16) 0.56052(14) 0.64172(10) 0.0260(5) Uani 1 1 d . . . . . V4 V 0.27975(16) 0.65532(14) 0.39929(10) 0.0278(5) Uani 1 1 d . . . . . V5 V 0.49379(16) 0.34226(14) 0.65962(10) 0.0287(5) Uani 1 1 d . . . . . O1 O 0.2604(6) 0.5669(6) 0.4938(4) 0.0272(16) Uani 1 1 d . . . . . O2 O 0.3542(6) 0.4303(6) 0.6083(4) 0.0298(17) Uani 1 1 d . . . . . O3 O 0.3571(6) 0.3812(5) 0.4580(4) 0.0230(15) Uani 1 1 d . . . . . O4 O 0.4488(7) 0.2839(7) 0.7277(4) 0.043(2) Uani 1 1 d . . . . . O5 O 0.5463(6) 0.4318(5) 0.5559(4) 0.0238(15) Uani 1 1 d . . . . . O6 O 0.5480(6) 0.4765(6) 0.7046(4) 0.0307(18) Uani 1 1 d . . . . . O7 O 0.7422(6) 0.4775(5) 0.6528(4) 0.0260(16) Uani 1 1 d . . . . . O8 O 0.6609(6) 0.6623(5) 0.6972(4) 0.0290(17) Uani 1 1 d . . . . . O9 O 0.4622(6) 0.6176(5) 0.5887(4) 0.0242(15) Uani 1 1 d . . . . . O10 O 0.5544(6) 0.7526(6) 0.4240(4) 0.0284(17) Uani 1 1 d . . . . . O11 O 0.5467(6) 0.8233(5) 0.5679(4) 0.0267(16) Uani 1 1 d . . . . . O12 O 0.3592(6) 0.7525(5) 0.4732(4) 0.0235(15) Uani 1 1 d . . . . . O13 O 0.3591(6) 0.7076(6) 0.3277(4) 0.0272(16) Uani 1 1 d . . . . . O14 O 0.1583(6) 0.7127(6) 0.3756(4) 0.039(2) Uani 1 1 d . . . . . O15 O 0.7201(6) 0.8762(6) 0.6880(4) 0.0330(18) Uani 1 1 d . . . . . H15A H 0.709044 0.832667 0.723706 0.049 Uiso 1 1 d R U . . . H15C H 0.770934 0.922947 0.707316 0.049 Uiso 1 1 d R U . . . O16 O 0.6644(6) 1.0342(6) 0.5698(4) 0.0349(18) Uani 1 1 d . . . . . H16A H 0.686322 1.096415 0.588846 0.052 Uiso 1 1 d R U . . . H16B H 0.722742 0.995436 0.566886 0.052 Uiso 1 1 d R U . . . O17 O 0.6137(6) 1.0795(6) 0.7222(4) 0.0352(19) Uani 1 1 d . . . . . H17C H 0.565332 1.028369 0.708572 0.042 Uiso 1 1 d R U . . . H17D H 0.593671 1.134808 0.693111 0.042 Uiso 1 1 d R U . . . O18 O 0.4261(6) 1.0343(6) 0.5839(4) 0.0343(18) Uani 1 1 d . . . . . H18B H 0.436337 1.102980 0.588431 0.051 Uiso 1 1 d R U . . . H18C H 0.414547 1.016680 0.535931 0.051 Uiso 1 1 d R U . . . O19 O 0.8924(7) 0.0528(7) 0.6429(5) 0.046(2) Uani 1 1 d . . . . . H19C H 0.905276 0.027861 0.689267 0.055 Uiso 1 1 d R U . . . H19B H 0.910806 0.119961 0.643107 0.055 Uiso 1 1 d R U . . . N1 N 0.4725(8) 0.8938(8) 0.7139(5) 0.036(2) Uani 1 1 d . . . . . N2 N 0.3683(9) 0.7834(9) 0.7710(7) 0.052(3) Uani 1 1 d . . . . . N3 N 0.9835(11) 0.2306(10) 0.4175(9) 0.071(4) Uani 1 1 d . . . . . N4 N 1.1413(11) 0.3156(11) 0.4329(7) 0.065(3) Uani 1 1 d . . . . . H4 H 1.213445 0.329213 0.437544 0.078 Uiso 1 1 calc R U . . . C1 C 0.9631(15) 0.3317(15) 0.4363(13) 0.098(7) Uani 1 1 d . . . . . H1 H 0.892454 0.359162 0.442431 0.118 Uiso 1 1 calc R U . . . C2 C 1.0593(17) 0.3871(18) 0.4451(12) 0.097(6) Uani 1 1 d . U . . . H2 H 1.069431 0.460998 0.457231 0.116 Uiso 1 1 calc R U . . . C3 C 1.0911(13) 0.2230(14) 0.4129(9) 0.067(5) Uani 1 1 d . . . . . H3 H 1.126219 0.161064 0.397609 0.080 Uiso 1 1 calc R U . . . C4 C 0.8985(19) 0.1430(18) 0.3879(13) 0.110(7) Uani 1 1 d D U . . . H4A H 0.849480 0.165979 0.339167 0.133 Uiso 1 1 calc R U . . . H4B H 0.938340 0.076848 0.378084 0.133 Uiso 1 1 calc R U . . . C5 C 0.832(2) 0.123(2) 0.4434(15) 0.154(10) Uani 1 1 d D U . . . H5A H 0.881841 0.107491 0.492814 0.231 Uiso 1 1 calc R U . . . H5B H 0.783083 0.061267 0.427436 0.231 Uiso 1 1 calc R U . . . H5C H 0.786283 0.186053 0.448331 0.231 Uiso 1 1 calc R U . . . C6 C 0.4419(11) 0.7913(9) 0.7227(7) 0.038(3) Uani 1 1 d . . . . . H8 H 0.468424 0.731888 0.698183 0.046 Uiso 1 1 calc R U . . . C7 C 0.3526(14) 0.8884(13) 0.7950(9) 0.068(5) Uani 1 1 d . . . . . H6 H 0.307055 0.910188 0.829724 0.082 Uiso 1 1 calc R U . . . C8 C 0.4171(13) 0.9539(12) 0.7578(8) 0.060(4) Uani 1 1 d . . . . . H8A H 0.421755 1.029639 0.762441 0.072 Uiso 1 1 calc R U . . . C9 C 0.3185(14) 0.6822(15) 0.7934(11) 0.083(6) Uani 1 1 d . . . . . H9A H 0.237544 0.679872 0.768946 0.100 Uiso 1 1 calc R U . . . H9B H 0.355858 0.620527 0.774123 0.100 Uiso 1 1 calc R U . . . C10 C 0.330(2) 0.6719(18) 0.8761(14) 0.123(9) Uani 1 1 d . . . . . H10A H 0.410038 0.671423 0.900577 0.184 Uiso 1 1 calc R U . . . H10B H 0.294906 0.604888 0.887817 0.184 Uiso 1 1 calc R U . . . H10C H 0.292742 0.732553 0.895586 0.184 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 Ni1 0.0333(8) 0.0160(7) 0.0333(8) -0.0009(6) 0.0029(6) -0.0020(6) V1 0.0227(10) 0.0159(9) 0.0307(10) -0.0011(7) 0.0046(7) -0.0005(7) V2 0.0283(10) 0.0125(9) 0.0309(10) -0.0005(7) 0.0002(8) -0.0015(7) V3 0.0312(11) 0.0162(10) 0.0282(9) -0.0010(7) -0.0002(8) -0.0002(8) V4 0.0289(11) 0.0172(10) 0.0352(10) 0.0010(8) 0.0015(8) 0.0022(8) V5 0.0361(12) 0.0177(10) 0.0321(10) 0.0028(8) 0.0062(8) -0.0012(8) O1 0.022(4) 0.020(4) 0.037(4) 0.001(3) 0.002(3) 0.000(3) O2 0.032(4) 0.017(4) 0.041(4) -0.001(3) 0.010(3) -0.004(3) O3 0.025(4) 0.014(4) 0.030(4) 0.000(3) 0.004(3) 0.001(3) O4 0.059(6) 0.037(5) 0.033(4) 0.011(4) 0.011(4) 0.000(4) O5 0.022(4) 0.017(4) 0.033(4) 0.003(3) 0.005(3) -0.002(3) O6 0.044(5) 0.012(4) 0.032(4) 0.000(3) -0.001(3) 0.001(3) O7 0.029(4) 0.015(4) 0.031(4) -0.001(3) -0.001(3) 0.002(3) O8 0.043(5) 0.010(4) 0.032(4) -0.006(3) 0.001(3) 0.000(3) O9 0.027(4) 0.011(4) 0.033(4) 0.000(3) 0.003(3) 0.000(3) O10 0.032(4) 0.018(4) 0.035(4) -0.003(3) 0.006(3) -0.002(3) O11 0.039(4) 0.015(4) 0.026(4) 0.003(3) 0.005(3) 0.003(3) O12 0.025(4) 0.014(4) 0.027(3) -0.004(3) -0.004(3) -0.001(3) O13 0.030(4) 0.018(4) 0.030(4) 0.002(3) -0.001(3) 0.004(3) O14 0.032(5) 0.029(5) 0.049(5) 0.002(4) -0.003(4) 0.011(4) O15 0.040(5) 0.020(4) 0.037(4) 0.010(3) 0.004(3) -0.004(3) O16 0.040(5) 0.020(4) 0.042(4) 0.002(3) 0.001(4) -0.005(4) O17 0.040(5) 0.015(4) 0.044(4) -0.005(3) -0.005(4) -0.003(3) O18 0.044(5) 0.016(4) 0.040(4) 0.005(3) 0.000(4) 0.003(3) O19 0.056(6) 0.031(5) 0.050(5) 0.006(4) 0.009(4) -0.007(4) N1 0.033(6) 0.038(6) 0.039(5) -0.003(5) 0.008(4) -0.002(5) N2 0.048(7) 0.033(7) 0.082(8) 0.009(6) 0.031(6) 0.008(5) N3 0.050(8) 0.041(8) 0.124(11) -0.021(7) 0.024(7) -0.021(6) N4 0.042(7) 0.068(9) 0.089(9) -0.013(7) 0.024(6) -0.015(7) C1 0.048(10) 0.062(12) 0.19(2) -0.040(13) 0.046(12) -0.017(9) C2 0.088(9) 0.088(10) 0.119(10) -0.009(8) 0.032(8) -0.010(8) C3 0.051(10) 0.066(11) 0.094(12) -0.025(9) 0.037(9) -0.024(8) C4 0.116(10) 0.099(10) 0.118(10) -0.001(8) 0.027(8) -0.026(8) C5 0.187(18) 0.136(17) 0.153(16) -0.061(14) 0.067(15) -0.048(14) C6 0.050(8) 0.018(6) 0.048(7) 0.005(5) 0.011(6) 0.002(5) C7 0.080(12) 0.057(10) 0.082(11) -0.006(8) 0.050(10) -0.004(9) C8 0.074(11) 0.036(8) 0.081(10) -0.009(7) 0.043(9) -0.009(8) C9 0.063(11) 0.074(12) 0.125(15) 0.052(11) 0.048(10) 0.019(9) C10 0.16(2) 0.077(15) 0.15(2) 0.041(14) 0.077(18) 0.021(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 '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' 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 N1 Ni1 O18 88.0(3) . . ? N1 Ni1 O15 98.3(3) . . ? O18 Ni1 O15 172.8(3) . . ? N1 Ni1 O17 87.5(3) . . ? O18 Ni1 O17 93.8(3) . . ? O15 Ni1 O17 90.1(3) . . ? N1 Ni1 O11 94.5(3) . . ? O18 Ni1 O11 93.7(3) . . ? O15 Ni1 O11 82.2(3) . . ? O17 Ni1 O11 172.3(3) . . ? N1 Ni1 O16 174.8(4) . . ? O18 Ni1 O16 88.7(3) . . ? O15 Ni1 O16 85.3(3) . . ? O17 Ni1 O16 88.7(3) . . ? O11 Ni1 O16 89.6(3) . . ? N1 Ni1 H17C 67.9 . . ? O18 Ni1 H17C 87.3 . . ? O15 Ni1 H17C 98.4 . . ? O17 Ni1 H17C 20.4 . . ? O11 Ni1 H17C 162.4 . . ? O16 Ni1 H17C 107.9 . . ? O2 V1 O1 107.0(4) . . ? O2 V1 O9 98.0(3) . . ? O1 V1 O9 98.6(3) . . ? O2 V1 O3 97.0(3) . . ? O1 V1 O3 95.5(3) . . ? O9 V1 O3 155.4(3) . . ? O2 V1 O5 165.5(3) . 3_666 ? O1 V1 O5 87.4(3) . 3_666 ? O9 V1 O5 80.7(3) . 3_666 ? O3 V1 O5 79.9(3) . 3_666 ? O2 V1 O5 87.7(3) . . ? O1 V1 O5 165.2(3) . . ? O9 V1 O5 80.9(3) . . ? O3 V1 O5 80.3(3) . . ? O5 V1 O5 77.8(3) 3_666 . ? O11 V2 O12 101.3(3) . . ? O11 V2 O10 102.8(3) . . ? O12 V2 O10 94.3(3) . . ? O11 V2 O9 100.2(3) . . ? O12 V2 O9 91.9(3) . . ? O10 V2 O9 154.5(3) . . ? O11 V2 O3 101.3(3) . 3_666 ? O12 V2 O3 155.9(3) . 3_666 ? O10 V2 O3 88.8(3) . 3_666 ? O9 V2 O3 75.9(3) . 3_666 ? O11 V2 O5 175.8(3) . 3_666 ? O12 V2 O5 80.9(3) . 3_666 ? O10 V2 O5 80.4(3) . 3_666 ? O9 V2 O5 76.1(3) . 3_666 ? O3 V2 O5 76.1(3) 3_666 3_666 ? O11 V2 V5 135.4(2) . 3_666 ? O12 V2 V5 83.0(2) . 3_666 ? O10 V2 V5 33.0(2) . 3_666 ? O9 V2 V5 124.2(2) . 3_666 ? O3 V2 V5 86.87(19) 3_666 3_666 ? O5 V2 V5 48.12(17) 3_666 3_666 ? O8 V3 O6 102.6(3) . . ? O8 V3 O7 100.4(3) . . ? O6 V3 O7 94.2(3) . . ? O8 V3 O9 100.7(3) . . ? O6 V3 O9 91.6(3) . . ? O7 V3 O9 156.3(3) . . ? O8 V3 O3 98.5(3) . 3_666 ? O6 V3 O3 157.5(3) . 3_666 ? O7 V3 O3 89.8(3) . 3_666 ? O9 V3 O3 76.5(3) . 3_666 ? O8 V3 O5 174.4(3) . . ? O6 V3 O5 82.4(3) . . ? O7 V3 O5 81.6(3) . . ? O9 V3 O5 76.5(3) . . ? O3 V3 O5 76.3(3) 3_666 . ? O8 V3 V4 133.7(3) . 3_666 ? O6 V3 V4 84.3(2) . 3_666 ? O7 V3 V4 33.4(2) . 3_666 ? O9 V3 V4 125.0(2) . 3_666 ? O3 V3 V4 86.95(19) 3_666 3_666 ? O5 V3 V4 48.61(18) . 3_666 ? O14 V4 O13 103.6(4) . . ? O14 V4 O7 103.3(4) . 3_666 ? O13 V4 O7 90.6(3) . 3_666 ? O14 V4 O12 101.8(4) . . ? O13 V4 O12 89.6(3) . . ? O7 V4 O12 154.1(3) 3_666 . ? O14 V4 O1 101.6(4) . . ? O13 V4 O1 154.7(3) . . ? O7 V4 O1 84.6(3) 3_666 . ? O12 V4 O1 84.3(3) . . ? O14 V4 O5 175.1(4) . 3_666 ? O13 V4 O5 81.0(3) . 3_666 ? O7 V4 O5 77.9(3) 3_666 3_666 ? O12 V4 O5 76.6(3) . 3_666 ? O1 V4 O5 73.7(3) . 3_666 ? O14 V4 V5 136.3(3) . 3_666 ? O13 V4 V5 32.7(2) . 3_666 ? O7 V4 V5 83.6(2) 3_666 3_666 ? O12 V4 V5 82.6(2) . 3_666 ? O1 V4 V5 122.0(2) . 3_666 ? O5 V4 V5 48.34(17) 3_666 3_666 ? O14 V4 V3 135.9(3) . 3_666 ? O13 V4 V3 81.1(2) . 3_666 ? O7 V4 V3 32.7(2) 3_666 3_666 ? O12 V4 V3 122.2(2) . 3_666 ? O1 V4 V3 81.5(2) . 3_666 ? O5 V4 V3 45.65(17) 3_666 3_666 ? V5 V4 V3 59.85(6) 3_666 3_666 ? O4 V5 O13 102.8(4) . 3_666 ? O4 V5 O10 102.4(4) . 3_666 ? O13 V5 O10 91.2(3) 3_666 3_666 ? O4 V5 O6 102.7(4) . . ? O13 V5 O6 90.2(3) 3_666 . ? O10 V5 O6 153.9(3) 3_666 . ? O4 V5 O2 101.7(4) . . ? O13 V5 O2 155.5(3) 3_666 . ? O10 V5 O2 83.7(3) 3_666 . ? O6 V5 O2 84.3(3) . . ? O4 V5 O5 175.8(4) . . ? O13 V5 O5 81.3(3) 3_666 . ? O10 V5 O5 76.6(3) 3_666 . ? O6 V5 O5 77.9(3) . . ? O2 V5 O5 74.2(3) . . ? O4 V5 V4 135.6(3) . 3_666 ? O13 V5 V4 32.8(2) 3_666 3_666 ? O10 V5 V4 83.9(2) 3_666 3_666 ? O6 V5 V4 83.3(2) . 3_666 ? O2 V5 V4 122.7(2) . 3_666 ? O5 V5 V4 48.52(17) . 3_666 ? O4 V5 V2 133.9(3) . 3_666 ? O13 V5 V2 81.2(2) 3_666 3_666 ? O10 V5 V2 31.8(2) 3_666 3_666 ? O6 V5 V2 123.3(2) . 3_666 ? O2 V5 V2 81.9(2) . 3_666 ? O5 V5 V2 45.44(17) . 3_666 ? V4 V5 V2 60.21(6) 3_666 3_666 ? V1 O1 V4 111.3(4) . . ? V1 O2 V5 110.9(4) . . ? V1 O3 V3 107.1(3) . 3_666 ? V1 O3 V2 106.4(3) . 3_666 ? V3 O3 V2 99.5(3) 3_666 3_666 ? V1 O5 V1 102.2(3) 3_666 . ? V1 O5 V3 94.3(3) 3_666 . ? V1 O5 V3 92.2(3) . . ? V1 O5 V2 92.4(3) 3_666 3_666 ? V1 O5 V2 94.5(3) . 3_666 ? V3 O5 V2 169.2(3) . 3_666 ? V1 O5 V5 170.7(4) 3_666 . ? V1 O5 V5 87.2(2) . . ? V3 O5 V5 85.5(2) . . ? V2 O5 V5 86.4(2) 3_666 . ? V1 O5 V4 87.5(2) 3_666 3_666 ? V1 O5 V4 170.2(3) . 3_666 ? V3 O5 V4 85.7(2) . 3_666 ? V2 O5 V4 86.1(2) 3_666 3_666 ? V5 O5 V4 83.1(2) . 3_666 ? V3 O6 V5 113.5(4) . . ? V3 O7 V4 113.9(4) . 3_666 ? V1 O9 V2 107.6(3) . . ? V1 O9 V3 107.3(3) . . ? V2 O9 V3 101.6(3) . . ? V2 O10 V5 115.3(4) . 3_666 ? V2 O11 Ni1 169.8(4) . . ? V2 O12 V4 115.7(4) . . ? V5 O13 V4 114.5(4) 3_666 . ? Ni1 O15 H15A 109.3 . . ? Ni1 O15 H15C 109.2 . . ? H15A O15 H15C 109.5 . . ? Ni1 O16 H16A 109.4 . . ? Ni1 O16 H16B 109.1 . . ? H16A O16 H16B 109.5 . . ? Ni1 O17 H17C 37.0 . . ? Ni1 O17 H17D 100.3 . . ? H17C O17 H17D 109.1 . . ? Ni1 O18 H18B 109.3 . . ? Ni1 O18 H18C 109.1 . . ? H18B O18 H18C 109.5 . . ? H19C O19 H19B 110.3 . . ? C6 N1 C8 106.1(10) . . ? C6 N1 Ni1 129.4(8) . . ? C8 N1 Ni1 124.2(9) . . ? C6 N2 C7 105.8(11) . . ? C6 N2 C9 125.8(12) . . ? C7 N2 C9 128.4(12) . . ? C3 N3 C1 108.4(13) . . ? C3 N3 C4 122.1(15) . . ? C1 N3 C4 128.1(15) . . ? C3 N4 C2 107.4(14) . . ? C3 N4 H4 126.3 . . ? C2 N4 H4 126.3 . . ? C2 C1 N3 108.4(16) . . ? C2 C1 H1 125.8 . . ? N3 C1 H1 125.8 . . ? C1 C2 N4 106.5(18) . . ? C1 C2 H2 126.8 . . ? N4 C2 H2 126.8 . . ? N4 C3 N3 109.0(14) . . ? N4 C3 H3 125.5 . . ? N3 C3 H3 125.5 . . ? C5 C4 N3 108.8(19) . . ? C5 C4 H4A 109.9 . . ? N3 C4 H4A 109.9 . . ? C5 C4 H4B 109.9 . . ? N3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N1 C6 N2 111.9(11) . . ? N1 C6 H8 124.1 . . ? N2 C6 H8 124.1 . . ? C8 C7 N2 106.2(12) . . ? C8 C7 H6 126.9 . . ? N2 C7 H6 126.9 . . ? N1 C8 C7 110.0(13) . . ? N1 C8 H8A 125.0 . . ? C7 C8 H8A 125.0 . . ? C10 C9 N2 112.7(18) . . ? C10 C9 H9A 109.1 . . ? N2 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? N2 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? 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 Ni1 N1 2.010(9) . ? Ni1 O18 2.039(7) . ? Ni1 O15 2.051(7) . ? Ni1 O17 2.053(7) . ? Ni1 O11 2.062(7) . ? Ni1 O16 2.095(7) . ? Ni1 H17C 1.4667 . ? V1 O2 1.659(7) . ? V1 O1 1.663(7) . ? V1 O9 1.887(7) . ? V1 O3 1.940(7) . ? V1 O5 2.093(7) 3_666 ? V1 O5 2.100(7) . ? V2 O11 1.622(7) . ? V2 O12 1.787(7) . ? V2 O10 1.802(7) . ? V2 O9 1.965(7) . ? V2 O3 2.015(7) 3_666 ? V2 O5 2.210(7) 3_666 ? V2 V5 3.096(2) 3_666 ? V3 O8 1.609(7) . ? V3 O6 1.789(7) . ? V3 O7 1.818(7) . ? V3 O9 1.969(7) . ? V3 O3 1.981(7) 3_666 ? V3 O5 2.207(7) . ? V3 V4 3.078(2) 3_666 ? V4 O14 1.582(7) . ? V4 O13 1.827(7) . ? V4 O7 1.854(7) 3_666 ? V4 O12 1.865(6) . ? V4 O1 2.027(7) . ? V4 O5 2.316(7) 3_666 ? V4 V5 3.069(3) 3_666 ? V5 O4 1.570(7) . ? V5 O13 1.822(7) 3_666 ? V5 O10 1.863(7) 3_666 ? V5 O6 1.877(7) . ? V5 O2 2.027(7) . ? V5 O5 2.309(7) . ? O15 H15A 0.8498 . ? O15 H15C 0.8500 . ? O16 H16A 0.8500 . ? O16 H16B 0.8500 . ? O17 H17C 0.8500 . ? O17 H17D 0.8501 . ? O18 H18B 0.8499 . ? O18 H18C 0.8500 . ? O19 H19C 0.8501 . ? O19 H19B 0.8499 . ? N1 C6 1.322(14) . ? N1 C8 1.330(15) . ? N2 C6 1.336(15) . ? N2 C7 1.375(18) . ? N2 C9 1.459(19) . ? N3 C3 1.300(18) . ? N3 C1 1.31(2) . ? N3 C4 1.49(2) . ? N4 C3 1.294(18) . ? N4 C2 1.36(2) . ? N4 H4 0.8600 . ? C1 C2 1.31(2) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.389(16) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H8 0.9300 . ? C7 C8 1.362(18) . ? C7 H6 0.9300 . ? C8 H8A 0.9300 . ? C9 C10 1.43(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C9 H9A O4 0.97 2.56 3.360(18) 139.3 2_556 yes C7 H6 O2 0.93 2.40 3.291(15) 161.5 2_556 yes C6 H8 O9 0.93 2.36 3.206(14) 151.5 . yes C6 H8 O8 0.93 2.44 3.149(14) 132.9 . yes C5 H5C O12 0.96 2.53 3.31(3) 138.8 3_666 yes C4 H4B O19 0.97 2.64 3.57(3) 159.5 3_756 yes C4 H4A O4 0.97 2.55 3.11(2) 116.9 4_665 yes C3 H3 O15 0.93 2.62 3.349(16) 135.2 3_766 yes C2 H2 O1 0.93 2.58 3.23(2) 127.7 1_655 yes C1 H1 O1 0.93 2.49 3.375(19) 160.2 3_666 yes N4 H4 O3 0.86 1.79 2.635(14) 168.5 1_655 yes O19 H19B O14 0.85 2.20 2.935(11) 144.0 3_666 yes O19 H19C O6 0.85 1.93 2.777(11) 173.6 2_646 yes O18 H18C O16 0.85 1.99 2.812(10) 161.0 3_676 yes O18 H18B O10 0.85 1.79 2.622(10) 167.8 3_676 yes O17 H17D O13 0.85 2.06 2.785(10) 142.8 3_676 yes O17 H17D O4 0.85 2.66 3.189(11) 121.7 1_565 yes O16 H16B O19 0.85 2.29 2.760(11) 115.3 1_565 yes O16 H16A O12 0.85 2.16 2.713(10) 123.0 3_676 yes O15 H15C O19 0.85 2.56 3.183(11) 131.5 1_565 yes O15 H15C O7 0.85 2.57 2.994(10) 112.1 2_656 yes O15 H15C O6 0.85 2.47 3.243(11) 152.3 2_656 yes O15 H15A O13 0.85 2.33 2.846(10) 119.9 4_676 yes O15 H15A O8 0.85 2.18 2.721(10) 120.9 . yes