#------------------------------------------------------------------------------ #$Date: 2020-05-23 04:22:48 +0300 (Sat, 23 May 2020) $ #$Revision: 252294 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240569.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_7240569 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 'C12 H50 N4 Ni2 O42 V10' _chemical_formula_weight 1549.38 _space_group_crystal_system monoclinic _space_group_IT_number 12 _space_group_name_Hall '-C 2y' _space_group_name_H-M_alt 'C 1 2/m 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 106.177(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 19.4747(16) _cell_length_b 9.2565(8) _cell_length_c 14.0833(12) _cell_measurement_reflns_used 2288 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.1791 _cell_measurement_theta_min 2.455 _cell_volume 2438.2(4) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _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 0.0575 _diffrn_reflns_av_unetI/netI 0.0590 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 6064 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.012 _diffrn_reflns_theta_max 25.011 _diffrn_reflns_theta_min 2.455 _exptl_absorpt_coefficient_mu 2.687 _exptl_crystal_colour green _exptl_crystal_density_diffrn 2.110 _exptl_crystal_description block _exptl_crystal_F_000 1544 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _refine_diff_density_max 1.580 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.157 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 2277 _refine_ls_number_restraints 145 _refine_ls_restrained_S_all 1.105 _refine_ls_R_factor_all 0.0744 _refine_ls_R_factor_gt 0.0544 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1043P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1546 _refine_ls_wR_factor_ref 0.1720 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1666 _reflns_number_total 2277 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00660b2.cif _cod_data_source_block 180720e _cod_original_sg_symbol_H-M 'C 2/m' _cod_database_code 7240569 _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 0.589 _shelx_estimated_absorpt_t_max 0.643 _shelx_res_file ; TITL 180720e in C2/m 180720e.res created by SHELXL-2018/3 at 11:26:30 on 09-Oct-2019 CELL 0.71073 19.4747 9.2565 14.0833 90.000 106.177 90.000 ZERR 2 0.0016 0.0008 0.0012 0.000 0.002 0.000 LATT 7 SYMM - X , Y , - Z SFAC C H N O V Ni UNIT 24 100 8 84 20 4 OMIT -1.00 50.04 L.S. 8 ACTA BOND $H FMAP 2 PLAN 20 htab dfix 1.39 0.01 n1 c1 c1 n2 n2 c2 c2 c3 c3 n1 dfix 2.32 0.02 n1 n2 n1 c2 c1 c2 c1 c3 n2 c3 flat 0.01 n1 n2 c1 c2 c3 c4 dfix 1.45 0.01 n1 c4 dfix 1.53 0.01 c4 c5 c5 c6 sadi 0.02 c4 c1 c4 c3 dfix 2.45 0.02 n1 c5 dfix 2.54 0.02 c4 c6 simu 0.01 0.02 3.8 n1 n2 c1 > c6 size 0.22 0.20 0.18 htab WGHT 0.104300 FVAR 0.15157 -0.25700 NI1 6 0.219420 0.500000 0.614747 10.50000 0.01662 0.01864 = 0.03735 0.00000 0.00920 0.00000 V1 5 0.408615 0.500000 0.613988 10.50000 0.01367 0.02017 = 0.02599 0.00000 0.00675 0.00000 V2 5 0.545933 0.335009 0.728921 11.00000 0.02092 0.02786 = 0.02890 0.00562 0.00617 0.00318 V3 5 0.637705 0.500000 0.615162 10.50000 0.01200 0.02353 = 0.02787 0.00000 0.00368 0.00000 V4 5 0.500000 0.675874 0.500000 10.50000 0.01309 0.01514 = 0.02814 0.00000 0.00510 0.00000 PART -1 N1 3 0.773425 0.045129 0.988295 10.50000 0.14127 0.12527 = 0.12966 -0.00066 -0.03801 0.00365 N2 3 0.665518 -0.057937 0.962208 10.50000 0.14476 0.12628 = 0.13269 -0.00106 -0.04242 0.00312 AFIX 43 H2 2 0.623895 -0.091447 0.932455 10.50000 -1.20000 PART 0 AFIX 0 O1 4 0.518907 0.500000 0.598113 10.50000 0.01557 0.01419 = 0.02997 0.00000 0.00820 0.00000 O2 4 0.445567 0.355253 0.698767 11.00000 0.01777 0.02378 = 0.02990 0.00225 0.00768 -0.00216 O3 4 0.323461 0.500000 0.610931 10.50000 0.01098 0.02828 = 0.03199 0.00000 0.00723 0.00000 O4 4 0.634492 0.353846 0.700902 11.00000 0.01673 0.02754 = 0.02981 0.00379 0.00406 0.00190 O5 4 0.519980 0.214966 0.600600 11.00000 0.02344 0.02044 = 0.03527 0.00263 0.01052 0.00126 O6 4 0.560273 0.500000 0.801603 10.50000 0.01738 0.03841 = 0.02079 0.00000 0.00077 0.00000 O7 4 0.561768 0.208078 0.808419 11.00000 0.03405 0.03923 = 0.03957 0.01391 0.00862 0.00194 O8 4 0.596623 0.633514 0.500863 11.00000 0.01333 0.01683 = 0.02661 -0.00116 0.00611 -0.00200 O9 4 0.719328 0.500000 0.613765 10.50000 0.01567 0.03595 = 0.03527 0.00000 0.00546 0.00000 O10 4 0.241653 0.660150 0.721099 11.00000 0.02450 0.02685 = 0.04893 -0.00423 0.01090 0.00392 AFIX 3 H10C 2 0.205903 0.715700 0.714799 11.00000 -1.20000 H10D 2 0.277843 0.711890 0.721799 11.00000 -1.20000 AFIX 0 O11 4 0.193171 0.656430 0.504973 11.00000 0.02608 0.02153 = 0.04872 0.00431 0.01574 0.00559 AFIX 3 H11C 2 0.159611 0.715480 0.504303 11.00000 -1.20000 H11D 2 0.229781 0.704760 0.502633 10.50000 -1.20000 H11A 2 0.180631 0.600990 0.455003 10.50000 -1.20000 AFIX 0 O12 4 0.118475 0.500000 0.629144 10.50000 0.02636 0.01793 = 0.08441 0.00000 0.02045 0.00000 AFIX 3 H12 2 0.091855 0.574350 0.621174 11.00000 -1.20000 AFIX 0 O13 4 0.353421 0.844665 0.723955 11.00000 0.04588 0.04439 = 0.22345 -0.02966 0.04728 0.00189 AFIX 3 H13C 2 0.388331 0.796535 0.715215 11.00000 -1.20000 PART 1 H13D 2 0.362521 0.934205 0.721675 10.50000 -1.20000 PART 2 H13B 2 0.328686 0.892774 0.674877 10.50000 -1.20000 PART -1 AFIX 0 C1 1 0.712273 0.005529 0.915385 10.50000 0.13944 0.12205 = 0.12370 -0.00054 -0.03807 0.00255 AFIX 43 H1 2 0.703993 0.018882 0.847676 10.50000 -1.20000 AFIX 0 C2 1 0.695899 -0.059181 1.063783 10.50000 0.14369 0.12599 = 0.12974 -0.00263 -0.03519 -0.00250 AFIX 43 H2A 2 0.675510 -0.095346 1.111267 10.50000 -1.20000 AFIX 0 C3 1 0.763705 0.005171 1.080655 10.50000 0.13728 0.12576 = 0.12421 0.00004 -0.03771 0.00201 AFIX 43 H3 2 0.796533 0.019067 1.142052 10.50000 -1.20000 AFIX 0 C4 1 0.837454 0.114900 0.978895 10.50000 0.14388 0.12868 = 0.12932 -0.00068 -0.03595 0.00223 AFIX 23 H4A 2 0.867091 0.136430 1.045035 10.50000 -1.20000 H4B 2 0.823502 0.206636 0.945861 10.50000 -1.20000 AFIX 0 C5 1 0.883526 0.037369 0.925105 10.50000 0.14695 0.13127 = 0.13940 0.00327 -0.04487 0.00300 AFIX 23 H5A 2 0.858161 0.029187 0.855498 10.50000 -1.20000 H5B 2 0.894203 -0.059282 0.951744 10.50000 -1.20000 AFIX 0 C6 1 0.953050 0.121384 0.937214 10.50000 0.18916 0.17168 = 0.18390 0.01479 -0.01975 -0.00793 AFIX 33 H6A 2 0.982352 0.071938 0.902940 10.50000 -1.50000 H6B 2 0.942248 0.216599 0.910154 10.50000 -1.50000 H6C 2 0.978197 0.128360 1.006149 10.50000 -1.50000 PART 0 AFIX 0 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 -1.0000 REM 180720e in C2/m REM wR2 = 0.1720, GooF = S = 1.105, Restrained GooF = 1.105 for all data REM R1 = 0.0544 for 1666 Fo > 4sig(Fo) and 0.0744 for all 2277 data REM 208 parameters refined using 145 restraints END WGHT 0.1044 0.0000 REM Instructions for potential hydrogen bonds EQIV $4 x, -y, z HTAB N2 O7_$4 EQIV $5 x-1/2, y+1/2, z HTAB O10 O4_$5 HTAB O10 O13 EQIV $6 x-1/2, -y+3/2, z HTAB O11 O8_$6 EQIV $7 -x+1/2, -y+3/2, -z+1 HTAB O11 O11_$7 EQIV $1 -x+1, -y+1, -z+1 HTAB O11 O9_$1 EQIV $2 x, -y+1, z HTAB O11 O11_$2 HTAB O11 O13_$7 HTAB O12 O5_$5 HTAB O13 O2_$2 EQIV $8 x, -y+2, z HTAB O13 O13_$8 HTAB O13 O9_$5 HTAB O13 O11_$7 EQIV $9 x+1/2, y-1/2, z HTAB C1 O10_$9 EQIV $10 -x+1, y-1, -z+2 HTAB C2 O13_$10 EQIV $11 -x+3/2, -y+1/2, -z+2 HTAB C3 O4_$11 HTAB C4 O6_$11 HTAB C4 O7_$11 REM Highest difference peak 1.580, deepest hole -0.869, 1-sigma level 0.157 Q1 1 0.4277 1.0000 0.6332 10.50000 0.05 1.58 Q2 1 0.3285 1.0000 0.6151 10.50000 0.05 1.43 Q3 1 0.7601 0.0000 0.9865 10.50000 0.05 1.17 Q4 1 0.8288 0.0000 0.9551 10.50000 0.05 0.74 Q5 1 0.6203 0.0000 1.0111 10.50000 0.05 0.58 Q6 1 0.6671 0.0000 1.0329 10.50000 0.05 0.58 Q7 1 0.5368 0.5000 0.8207 10.50000 0.05 0.55 Q8 1 0.8874 0.0000 0.8507 10.50000 0.05 0.53 Q9 1 0.3810 0.7995 0.8018 11.00000 0.05 0.52 Q10 1 0.6104 0.5532 0.6495 11.00000 0.05 0.49 Q11 1 0.5104 0.3195 0.5828 11.00000 0.05 0.49 Q12 1 0.6172 0.5000 0.5097 10.50000 0.05 0.49 Q13 1 0.6156 0.6253 0.5688 11.00000 0.05 0.47 Q14 1 0.1326 0.6721 0.7334 11.00000 0.05 0.47 Q15 1 0.5636 0.2175 0.7624 11.00000 0.05 0.46 Q16 1 0.2427 0.6399 0.6873 11.00000 0.05 0.46 Q17 1 0.9382 0.0000 0.9232 10.50000 0.05 0.45 Q18 1 0.6593 0.5000 0.7023 10.50000 0.05 0.45 Q19 1 0.2318 0.5000 0.6763 10.50000 0.05 0.45 Q20 1 0.3364 0.5000 0.6864 10.50000 0.05 0.44 ; _shelx_res_checksum 99538 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, 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 Ni1 Ni 0.21942(5) 0.500000 0.61475(8) 0.0239(3) Uani 1 2 d S T P . . V1 V 0.40861(7) 0.500000 0.61399(10) 0.0197(4) Uani 1 2 d S T P . . V2 V 0.54593(5) 0.33501(11) 0.72892(7) 0.0260(3) Uani 1 1 d . . . . . V3 V 0.63771(7) 0.500000 0.61516(10) 0.0215(4) Uani 1 2 d S T P . . V4 V 0.500000 0.67587(14) 0.500000 0.0189(4) Uani 1 2 d S T P . . N1 N 0.7734(7) 0.0451(15) 0.9883(10) 0.147(5) Uani 0.5 1 d D U P A -1 N2 N 0.6655(8) -0.0579(18) 0.9622(12) 0.151(5) Uani 0.5 1 d D U P A -1 H2 H 0.623895 -0.091447 0.932455 0.181 Uiso 0.5 1 calc R U P A -1 O1 O 0.5189(3) 0.500000 0.5981(4) 0.0195(12) Uani 1 2 d S T P . . O2 O 0.44557(19) 0.3553(4) 0.6988(3) 0.0236(9) Uani 1 1 d . . . . . O3 O 0.3235(3) 0.500000 0.6109(4) 0.0235(13) Uani 1 2 d S T P . . O4 O 0.63449(19) 0.3538(4) 0.7009(3) 0.0252(9) Uani 1 1 d . . . . . O5 O 0.5200(2) 0.2150(4) 0.6006(3) 0.0259(9) Uani 1 1 d . . . . . O6 O 0.5603(3) 0.500000 0.8016(4) 0.0264(13) Uani 1 2 d S T P . . O7 O 0.5618(2) 0.2081(5) 0.8084(3) 0.0379(11) Uani 1 1 d . . . . . O8 O 0.59662(18) 0.6335(4) 0.5009(3) 0.0188(8) Uani 1 1 d . . . . . O9 O 0.7193(3) 0.500000 0.6138(4) 0.0293(14) Uani 1 2 d S T P . . O10 O 0.2417(2) 0.6601(4) 0.7211(3) 0.0333(10) Uani 1 1 d . . . . . H10C H 0.205903 0.715700 0.714799 0.040 Uiso 1 1 d R U . . . H10D H 0.277843 0.711890 0.721799 0.040 Uiso 1 1 d R U . . . O11 O 0.1932(2) 0.6564(4) 0.5050(3) 0.0310(10) Uani 1 1 d . . . . . H11C H 0.159611 0.715480 0.504303 0.037 Uiso 1 1 d R U . . . H11D H 0.229781 0.704760 0.502633 0.037 Uiso 0.5 1 d R U P . . H11A H 0.180631 0.600990 0.455003 0.037 Uiso 0.5 1 d R U P . . O12 O 0.1185(3) 0.500000 0.6291(5) 0.0419(17) Uani 1 2 d S T P . . H12 H 0.091855 0.574350 0.621174 0.050 Uiso 1 1 d R U . . . O13 O 0.3534(3) 0.8447(6) 0.7240(6) 0.103(3) Uani 1 1 d . . . . . H13C H 0.388331 0.796535 0.715215 0.123 Uiso 1 1 d R U . . . H13D H 0.362521 0.934205 0.721675 0.123 Uiso 0.5 1 d R U P B 1 H13B H 0.328686 0.892774 0.674877 0.123 Uiso 0.5 1 d R U P C 2 C1 C 0.7123(9) 0.006(2) 0.9154(10) 0.143(5) Uani 0.5 1 d D U P A -1 H1 H 0.703993 0.018882 0.847676 0.172 Uiso 0.5 1 calc R U P A -1 C2 C 0.6959(10) -0.059(2) 1.0638(12) 0.148(5) Uani 0.5 1 d D U P A -1 H2A H 0.675510 -0.095346 1.111267 0.177 Uiso 0.5 1 calc R U P A -1 C3 C 0.7637(9) 0.005(3) 1.0807(10) 0.144(5) Uani 0.5 1 d D U P A -1 H3 H 0.796533 0.019067 1.142052 0.173 Uiso 0.5 1 calc R U P A -1 C4 C 0.8375(9) 0.115(2) 0.9789(15) 0.149(5) Uani 0.5 1 d D U P A -1 H4A H 0.867091 0.136430 1.045035 0.179 Uiso 0.5 1 calc R U P A -1 H4B H 0.823502 0.206636 0.945861 0.179 Uiso 0.5 1 calc R U P A -1 C5 C 0.8835(10) 0.037(3) 0.9251(15) 0.156(5) Uani 0.5 1 d D U P A -1 H5A H 0.858161 0.029187 0.855498 0.188 Uiso 0.5 1 calc R U P A -1 H5B H 0.894203 -0.059282 0.951744 0.188 Uiso 0.5 1 calc R U P A -1 C6 C 0.9531(12) 0.121(3) 0.937(2) 0.196(9) Uani 0.5 1 d D U P A -1 H6A H 0.982352 0.071938 0.902940 0.294 Uiso 0.5 1 calc R U P A -1 H6B H 0.942248 0.216599 0.910154 0.294 Uiso 0.5 1 calc R U P A -1 H6C H 0.978197 0.128360 1.006149 0.294 Uiso 0.5 1 calc R U P A -1 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 0.0166(6) 0.0186(6) 0.0373(7) 0.000 0.0092(5) 0.000 V1 0.0137(7) 0.0202(8) 0.0260(8) 0.000 0.0068(6) 0.000 V2 0.0209(6) 0.0279(7) 0.0289(6) 0.0056(4) 0.0062(4) 0.0032(4) V3 0.0120(7) 0.0235(8) 0.0279(8) 0.000 0.0037(6) 0.000 V4 0.0131(7) 0.0151(8) 0.0281(8) 0.000 0.0051(6) 0.000 N1 0.141(9) 0.125(11) 0.130(8) -0.001(8) -0.038(7) 0.004(8) N2 0.145(9) 0.126(11) 0.133(8) -0.001(8) -0.042(7) 0.003(8) O1 0.016(3) 0.014(3) 0.030(3) 0.000 0.008(2) 0.000 O2 0.018(2) 0.024(2) 0.030(2) 0.0023(17) 0.0077(17) -0.0022(16) O3 0.011(3) 0.028(3) 0.032(3) 0.000 0.007(2) 0.000 O4 0.017(2) 0.028(2) 0.030(2) 0.0038(17) 0.0041(17) 0.0019(17) O5 0.023(2) 0.020(2) 0.035(2) 0.0026(17) 0.0105(18) 0.0013(17) O6 0.017(3) 0.038(4) 0.021(3) 0.000 0.001(2) 0.000 O7 0.034(2) 0.039(3) 0.040(3) 0.014(2) 0.009(2) 0.002(2) O8 0.0133(18) 0.017(2) 0.027(2) -0.0012(15) 0.0061(16) -0.0020(15) O9 0.016(3) 0.036(4) 0.035(3) 0.000 0.005(3) 0.000 O10 0.025(2) 0.027(2) 0.049(3) -0.0042(19) 0.011(2) 0.0039(18) O11 0.026(2) 0.022(2) 0.049(3) 0.0043(18) 0.016(2) 0.0056(17) O12 0.026(3) 0.018(3) 0.084(5) 0.000 0.020(3) 0.000 O13 0.046(4) 0.044(4) 0.223(8) -0.030(5) 0.047(5) 0.002(3) C1 0.139(9) 0.122(10) 0.124(8) -0.001(9) -0.038(7) 0.003(9) C2 0.144(9) 0.126(11) 0.130(8) -0.003(9) -0.035(7) -0.002(8) C3 0.137(9) 0.126(10) 0.124(8) 0.000(9) -0.038(7) 0.002(9) C4 0.144(9) 0.129(10) 0.129(8) -0.001(8) -0.036(7) 0.002(8) C5 0.147(10) 0.131(11) 0.139(8) 0.003(9) -0.045(7) 0.003(9) C6 0.189(16) 0.172(16) 0.184(15) 0.015(15) -0.020(14) -0.008(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 O12 Ni1 O3 175.9(2) . . ? O12 Ni1 O10 86.61(18) . . ? O3 Ni1 O10 90.57(15) . . ? O12 Ni1 O10 86.61(18) . 6_565 ? O3 Ni1 O10 90.57(15) . 6_565 ? O10 Ni1 O10 91.7(2) . 6_565 ? O12 Ni1 O11 91.72(18) . 6_565 ? O3 Ni1 O11 91.19(15) . 6_565 ? O10 Ni1 O11 177.62(16) . 6_565 ? O10 Ni1 O11 89.87(17) 6_565 6_565 ? O12 Ni1 O11 91.72(18) . . ? O3 Ni1 O11 91.18(15) . . ? O10 Ni1 O11 89.87(17) . . ? O10 Ni1 O11 177.62(16) 6_565 . ? O11 Ni1 O11 88.5(2) 6_565 . ? O3 V1 O2 103.31(17) . . ? O3 V1 O2 103.31(17) . 6_565 ? O2 V1 O2 95.8(2) . 6_565 ? O3 V1 O8 98.83(18) . 5_666 ? O2 V1 O8 89.85(16) . 5_666 ? O2 V1 O8 155.16(16) 6_565 5_666 ? O3 V1 O8 98.83(18) . 2_656 ? O2 V1 O8 155.16(16) . 2_656 ? O2 V1 O8 89.85(16) 6_565 2_656 ? O8 V1 O8 75.6(2) 5_666 2_656 ? O3 V1 O1 173.0(2) . . ? O2 V1 O1 81.26(15) . . ? O2 V1 O1 81.26(15) 6_565 . ? O8 V1 O1 75.72(15) 5_666 . ? O8 V1 O1 75.72(15) 2_656 . ? O3 V1 V3 88.51(19) . 5_666 ? O2 V1 V3 129.44(12) . 5_666 ? O2 V1 V3 129.44(12) 6_565 5_666 ? O8 V1 V3 39.59(11) 5_666 5_666 ? O8 V1 V3 39.59(11) 2_656 5_666 ? O1 V1 V3 84.51(14) . 5_666 ? O3 V1 V2 136.59(14) . 6_565 ? O2 V1 V2 83.91(13) . 6_565 ? O2 V1 V2 33.46(12) 6_565 6_565 ? O8 V1 V2 124.20(11) 5_666 6_565 ? O8 V1 V2 87.74(11) 2_656 6_565 ? O1 V1 V2 48.51(11) . 6_565 ? V3 V1 V2 120.00(4) 5_666 6_565 ? O3 V1 V2 136.59(14) . . ? O2 V1 V2 33.46(12) . . ? O2 V1 V2 83.91(13) 6_565 . ? O8 V1 V2 87.74(11) 5_666 . ? O8 V1 V2 124.20(11) 2_656 . ? O1 V1 V2 48.51(11) . . ? V3 V1 V2 120.00(4) 5_666 . ? V2 V1 V2 58.76(4) 6_565 . ? O7 V2 O6 104.8(2) . . ? O7 V2 O4 101.9(2) . . ? O6 V2 O4 92.0(2) . . ? O7 V2 O2 102.5(2) . . ? O6 V2 O2 91.7(2) . . ? O4 V2 O2 153.45(18) . . ? O7 V2 O5 99.8(2) . . ? O6 V2 O5 155.40(19) . . ? O4 V2 O5 83.18(16) . . ? O2 V2 O5 82.58(16) . . ? O7 V2 O1 173.2(2) . . ? O6 V2 O1 81.97(16) . . ? O4 V2 O1 78.02(16) . . ? O2 V2 O1 76.50(16) . . ? O5 V2 O1 73.43(15) . . ? O7 V2 V2 137.54(17) . 6_565 ? O6 V2 V2 32.77(14) . 6_565 ? O4 V2 V2 84.68(12) . 6_565 ? O2 V2 V2 84.31(12) . 6_565 ? O5 V2 V2 122.63(11) . 6_565 ? O1 V2 V2 49.20(9) . 6_565 ? O7 V2 V4 130.60(17) . 5_666 ? O6 V2 V4 124.63(14) . 5_666 ? O4 V2 V4 78.49(12) . 5_666 ? O2 V2 V4 77.80(12) . 5_666 ? O5 V2 V4 30.77(11) . 5_666 ? O1 V2 V4 42.67(9) . 5_666 ? V2 V2 V4 91.86(3) 6_565 5_666 ? O7 V2 V3 134.21(16) . . ? O6 V2 V3 81.80(16) . . ? O4 V2 V3 32.35(12) . . ? O2 V2 V3 122.80(12) . . ? O5 V2 V3 81.31(11) . . ? O1 V2 V3 46.31(12) . . ? V2 V2 V3 60.62(2) 6_565 . ? V4 V2 V3 61.38(3) 5_666 . ? O7 V2 V1 134.22(16) . . ? O6 V2 V1 81.69(15) . . ? O4 V2 V1 123.39(12) . . ? O2 V2 V1 31.78(12) . . ? O5 V2 V1 80.98(11) . . ? O1 V2 V1 45.37(12) . . ? V2 V2 V1 60.62(2) 6_565 . ? V4 V2 V1 61.17(3) 5_666 . ? V3 V2 V1 91.43(4) . . ? O9 V3 O4 103.06(18) . 6_565 ? O9 V3 O4 103.06(18) . . ? O4 V3 O4 95.6(3) 6_565 . ? O9 V3 O8 99.54(19) . . ? O4 V3 O8 89.70(16) 6_565 . ? O4 V3 O8 154.92(17) . . ? O9 V3 O8 99.54(19) . 6_565 ? O4 V3 O8 154.92(17) 6_565 6_565 ? O4 V3 O8 89.70(16) . 6_565 ? O8 V3 O8 75.9(2) . 6_565 ? O9 V3 O1 173.5(3) . . ? O4 V3 O1 81.23(15) 6_565 . ? O4 V3 O1 81.23(15) . . ? O8 V3 O1 75.37(15) . . ? O8 V3 O1 75.37(15) 6_565 . ? O9 V3 V1 89.4(2) . 5_666 ? O4 V3 V1 129.41(13) 6_565 5_666 ? O4 V3 V1 129.41(13) . 5_666 ? O8 V3 V1 39.72(11) . 5_666 ? O8 V3 V1 39.72(11) 6_565 5_666 ? O1 V3 V1 84.09(14) . 5_666 ? O9 V3 V2 136.33(15) . 6_565 ? O4 V3 V2 33.46(11) 6_565 6_565 ? O4 V3 V2 83.85(12) . 6_565 ? O8 V3 V2 87.31(10) . 6_565 ? O8 V3 V2 123.80(11) 6_565 6_565 ? O1 V3 V2 48.44(10) . 6_565 ? V1 V3 V2 119.58(4) 5_666 6_565 ? O9 V3 V2 136.33(15) . . ? O4 V3 V2 83.85(13) 6_565 . ? O4 V3 V2 33.46(11) . . ? O8 V3 V2 123.80(11) . . ? O8 V3 V2 87.31(10) 6_565 . ? O1 V3 V2 48.44(10) . . ? V1 V3 V2 119.58(4) 5_666 . ? V2 V3 V2 58.77(4) 6_565 . ? O5 V4 O5 106.8(3) 6_565 5_666 ? O5 V4 O8 97.09(16) 6_565 2_656 ? O5 V4 O8 96.90(16) 5_666 2_656 ? O5 V4 O8 96.90(16) 6_565 . ? O5 V4 O8 97.10(16) 5_666 . ? O8 V4 O8 156.4(2) 2_656 . ? O5 V4 O1 87.41(17) 6_565 . ? O5 V4 O1 165.78(19) 5_666 . ? O8 V4 O1 80.66(17) 2_656 . ? O8 V4 O1 81.12(17) . . ? O5 V4 O1 165.78(19) 6_565 5_666 ? O5 V4 O1 87.41(17) 5_666 5_666 ? O8 V4 O1 81.12(17) 2_656 5_666 ? O8 V4 O1 80.66(17) . 5_666 ? O1 V4 O1 78.4(2) . 5_666 ? O5 V4 V2 145.27(15) 6_565 5_666 ? O5 V4 V2 38.46(14) 5_666 5_666 ? O8 V4 V2 89.34(10) 2_656 5_666 ? O8 V4 V2 89.90(10) . 5_666 ? O1 V4 V2 127.32(12) . 5_666 ? O1 V4 V2 48.95(11) 5_666 5_666 ? O5 V4 V2 38.46(14) 6_565 6_565 ? O5 V4 V2 145.27(15) 5_666 6_565 ? O8 V4 V2 89.90(10) 2_656 6_565 ? O8 V4 V2 89.34(10) . 6_565 ? O1 V4 V2 48.95(11) . 6_565 ? O1 V4 V2 127.32(12) 5_666 6_565 ? V2 V4 V2 176.27(6) 5_666 6_565 ? C1 N1 C3 107.7(9) . . ? C1 N1 C4 129.5(11) . . ? C3 N1 C4 122.8(10) . . ? C2 N2 C1 110.1(9) . . ? C2 N2 H2 124.9 . . ? C1 N2 H2 124.9 . . ? V4 O1 V4 101.6(2) 5_666 . ? V4 O1 V1 93.96(16) 5_666 . ? V4 O1 V1 93.96(16) . . ? V4 O1 V3 93.24(15) 5_666 . ? V4 O1 V3 93.24(15) . . ? V1 O1 V3 168.6(3) . . ? V4 O1 V2 170.0(2) 5_666 6_565 ? V4 O1 V2 88.38(4) . 6_565 ? V1 O1 V2 86.12(15) . 6_565 ? V3 O1 V2 85.25(16) . 6_565 ? V4 O1 V2 88.38(4) 5_666 . ? V4 O1 V2 170.0(2) . . ? V1 O1 V2 86.12(15) . . ? V3 O1 V2 85.25(16) . . ? V2 O1 V2 81.60(18) 6_565 . ? V1 O2 V2 114.76(19) . . ? V1 O3 Ni1 177.1(3) . . ? V3 O4 V2 114.18(19) . . ? V4 O5 V2 110.8(2) 5_666 . ? V2 O6 V2 114.5(3) . 6_565 ? V4 O8 V3 107.55(16) . . ? V4 O8 V1 106.86(17) . 5_666 ? V3 O8 V1 100.69(17) . 5_666 ? Ni1 O10 H10C 111.0 . . ? Ni1 O10 H10D 114.7 . . ? H10C O10 H10D 108.2 . . ? Ni1 O11 H11C 119.1 . . ? Ni1 O11 H11D 111.2 . . ? H11C O11 H11D 108.2 . . ? Ni1 O11 H11A 98.6 . . ? H11C O11 H11A 109.7 . . ? H11D O11 H11A 109.6 . . ? Ni1 O12 H12 123.9 . . ? Ni1 O12 H12 123.94(4) . 6_565 ? H12 O12 H12 108.1 . 6_565 ? H13C O13 H13D 108.8 . . ? H13C O13 H13B 116.9 . . ? N1 C1 N2 107.5(9) . . ? N1 C1 H1 126.3 . . ? N2 C1 H1 126.3 . . ? N2 C2 C3 106.3(9) . . ? N2 C2 H2A 126.8 . . ? C3 C2 H2A 126.8 . . ? C2 C3 N1 108.4(9) . . ? C2 C3 H3 125.8 . . ? N1 C3 H3 125.8 . . ? N1 C4 C5 118.9(12) . . ? N1 C4 H4A 107.6 . . ? C5 C4 H4A 107.6 . . ? N1 C4 H4B 107.6 . . ? C5 C4 H4B 107.6 . . ? H4A C4 H4B 107.0 . . ? C4 C5 C6 109.5(14) . . ? C4 C5 H5A 109.8 . . ? C6 C5 H5A 109.8 . . ? C4 C5 H5B 109.8 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 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 O12 2.032(6) . ? Ni1 O3 2.042(5) . ? Ni1 O10 2.066(4) . ? Ni1 O10 2.066(4) 6_565 ? Ni1 O11 2.075(4) 6_565 ? Ni1 O11 2.075(4) . ? V1 O3 1.647(5) . ? V1 O2 1.806(4) . ? V1 O2 1.806(4) 6_565 ? V1 O8 2.015(4) 5_666 ? V1 O8 2.015(4) 2_656 ? V1 O1 2.221(5) . ? V1 V3 3.0994(19) 5_666 ? V1 V2 3.1132(15) 6_565 ? V1 V2 3.1132(15) . ? V2 O7 1.593(4) . ? V2 O6 1.816(3) . ? V2 O4 1.881(4) . ? V2 O2 1.890(4) . ? V2 O5 2.061(4) . ? V2 O1 2.337(4) . ? V2 V2 3.054(2) 6_565 ? V2 V4 3.0980(10) 5_666 ? V2 V3 3.1127(14) . ? V3 O9 1.595(5) . ? V3 O4 1.826(4) 6_565 ? V3 O4 1.826(4) . ? V3 O8 2.010(4) . ? V3 O8 2.010(4) 6_565 ? V3 O1 2.258(5) . ? V4 O5 1.695(4) 6_565 ? V4 O5 1.695(4) 5_666 ? V4 O8 1.919(3) 2_656 ? V4 O8 1.919(3) . ? V4 O1 2.100(3) . ? V4 O1 2.100(3) 5_666 ? N1 C1 1.388(9) . ? N1 C3 1.415(9) . ? N1 C4 1.443(10) . ? N2 C2 1.387(9) . ? N2 C1 1.394(9) . ? N2 H2 0.8600 . ? O10 H10C 0.8500 . ? O10 H10D 0.8499 . ? O11 H11C 0.8500 . ? O11 H11D 0.8501 . ? O11 H11A 0.8500 . ? O12 H12 0.8500 . ? O12 H12 0.8501 6_565 ? O13 H13C 0.8500 . ? O13 H13D 0.8500 . ? O13 H13B 0.8500 . ? C1 H1 0.9300 . ? C2 C3 1.407(10) . ? C2 H2A 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.508(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.529(10) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ?