#------------------------------------------------------------------------------ #$Date: 2020-05-23 04:22:48 +0300 (Sat, 23 May 2020) $ #$Revision: 252294 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/05/7240567.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_7240567 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 'C56 H98 N16 Ni2 O13 V4' _chemical_formula_weight 1524.68 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yc' _space_group_name_H-M_alt 'P 1 2/c 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 107.071(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 14.6250(12) _cell_length_b 16.5741(14) _cell_length_c 16.2669(14) _cell_measurement_reflns_used 1024 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 26.312 _cell_measurement_theta_min 2.458 _cell_volume 3769.3(6) _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.1036 _diffrn_reflns_av_unetI/netI 0.1486 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 18504 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.020 _diffrn_reflns_theta_max 25.020 _diffrn_reflns_theta_min 2.458 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_T_max 26.312 _exptl_absorpt_correction_T_min 2.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour green _exptl_crystal_density_diffrn 1.343 _exptl_crystal_description block _exptl_crystal_F_000 1596 _exptl_crystal_size_max 0.220 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.180 _refine_diff_density_max 0.867 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.108 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.853 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 423 _refine_ls_number_reflns 6667 _refine_ls_number_restraints 495 _refine_ls_restrained_S_all 0.940 _refine_ls_R_factor_all 0.1794 _refine_ls_R_factor_gt 0.0755 _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^)+(0.1237P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1968 _refine_ls_wR_factor_ref 0.2369 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2556 _reflns_number_total 6667 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0ce00660b2.cif _cod_data_source_block 181109a _cod_original_sg_symbol_H-M 'P 2/c' _cod_database_code 7240567 _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 0.805 _shelx_estimated_absorpt_t_max 0.837 _shelx_res_file ; TITL 181109a in P2/c 181109a.res created by SHELXL-2018/3 at 21:47:30 on 09-May-2019 CELL 0.71073 14.6250 16.5741 16.2669 90.000 107.071 90.000 ZERR 2 0.0012 0.0014 0.0014 0.000 0.003 0.000 LATT 1 SYMM - X , Y , 0.50000 - Z SFAC C H N O V Ni UNIT 112 196 32 26 8 4 OMIT -1.00 50.04 L.S. 16 ACTA BOND $H FMAP 2 PLAN 20 htab delu 0.002 0.001 c13 c14 c26 c27 c28 dfix 2.54 0.02 c18 c20 c19 c21 c25 c27 c26 c28 dfix 2.54 0.02 c4 c6 c5 c7 c11 c13 c12 c14 dfix 1.53 0.01 c18 c19 c19 c20 c20 c21 c25 c26 c26 c27 c27 c28 dfix 1.53 0.01 c4 c5 c5 c6 c6 c7 c11 c12 c12 c13 c13 c14 dfix 3.67 0.02 c25 c28 simu 0.02 0.04 3.8 $o $c dfix 2.16 0.01 h28c h28c_$1 h28b h28c_$1 eqiv $1 -x,y,1/2-z size 0.22 0.20 0.18 htab BIND C12 C11 FREE C26 C28 FREE C14 C12 TEMP 25 WGHT 0.123700 FVAR 0.17828 NI1 6 0.500000 1.000000 0.500000 10.50000 0.07370 0.03534 = 0.04349 -0.00708 0.02446 -0.00063 NI2 6 0.500000 0.500000 0.500000 10.50000 0.08043 0.03826 = 0.04445 0.01032 0.02529 0.00390 V1 5 0.445896 0.843520 0.330332 11.00000 0.09882 0.04169 = 0.04510 -0.01182 0.02903 -0.00416 V2 5 0.547050 0.660247 0.358776 11.00000 0.10355 0.04038 = 0.04496 0.00773 0.02953 -0.00575 N1 3 0.383539 0.892603 0.677612 11.00000 0.12052 0.06601 = 0.05745 0.00455 0.04441 -0.00415 N2 3 0.452997 0.924774 0.581546 11.00000 0.08645 0.04814 = 0.05031 0.00097 0.01452 -0.00208 N3 3 0.769977 0.888966 0.540900 11.00000 0.09931 0.09167 = 0.11622 -0.00518 0.05158 0.03033 N4 3 0.638715 0.955489 0.540264 11.00000 0.08423 0.06044 = 0.04780 -0.00141 0.02655 0.00683 N5 3 0.626338 0.602044 0.740142 11.00000 0.15594 0.05652 = 0.04718 0.00336 0.03656 0.00808 N6 3 0.547847 0.573436 0.605823 11.00000 0.10719 0.03636 = 0.06389 0.00822 0.03565 0.00277 N7 3 0.225901 0.608063 0.407755 11.00000 0.11088 0.12324 = 0.08708 0.01718 0.03079 0.06079 N8 3 0.359635 0.541829 0.469655 11.00000 0.08842 0.04954 = 0.05948 0.01002 0.03570 0.01755 O1 4 0.488224 0.749889 0.376575 11.00000 0.19628 0.04634 = 0.06926 0.00143 0.05975 0.01031 O2 4 0.470464 0.912723 0.405071 11.00000 0.10483 0.04257 = 0.05179 -0.01002 0.04101 -0.00200 O3 4 0.500000 0.869479 0.250000 10.50000 0.19930 0.05163 = 0.06168 0.00000 0.06822 0.00000 O4 4 0.332283 0.838727 0.293486 11.00000 0.10588 0.18136 = 0.15923 -0.09324 0.01312 -0.01679 O5 4 0.526002 0.588097 0.420903 11.00000 0.12131 0.04495 = 0.04956 0.01638 0.03718 0.00525 O6 4 0.660246 0.674519 0.383780 11.00000 0.12127 0.16826 = 0.15911 0.06373 0.04044 -0.04000 O7 4 0.500000 0.631485 0.250000 10.50000 0.19050 0.04672 = 0.05797 0.00000 0.05714 0.00000 O8 4 0.198787 0.741475 0.178755 10.50000 0.04927 0.12083 = 0.08147 -0.05741 0.02617 -0.01103 AFIX 3 H8C 2 0.232807 0.773565 0.216135 10.50000 -1.20000 H8D 2 0.235377 0.716785 0.155125 10.50000 -1.20000 AFIX 0 C1 1 0.419296 0.951277 0.642935 11.00000 0.10540 0.04612 = 0.06084 -0.00258 0.05038 0.00113 AFIX 43 H1 2 0.420666 1.005023 0.659677 11.00000 -1.20000 AFIX 0 C2 1 0.432977 0.844588 0.572286 11.00000 0.15590 0.04553 = 0.07410 -0.00611 0.05933 -0.00307 AFIX 43 H2 2 0.445507 0.810750 0.531277 11.00000 -1.20000 AFIX 0 C3 1 0.391151 0.822385 0.633887 11.00000 0.19145 0.04887 = 0.10045 -0.01151 0.07174 -0.00364 AFIX 43 H3 2 0.371854 0.770869 0.644237 11.00000 -1.20000 AFIX 0 C4 1 0.337546 0.900955 0.745750 11.00000 0.13981 0.08579 = 0.07785 -0.00417 0.06259 -0.01371 AFIX 23 H4A 2 0.355444 0.952324 0.774551 11.00000 -1.20000 H4B 2 0.360080 0.858490 0.787872 11.00000 -1.20000 AFIX 0 C5 1 0.229860 0.896344 0.710679 11.00000 0.15107 0.12798 = 0.11417 -0.00214 0.07741 -0.02300 AFIX 23 H5A 2 0.202280 0.891260 0.757871 11.00000 -1.20000 H5B 2 0.212014 0.849021 0.674415 11.00000 -1.20000 AFIX 0 C6 1 0.190575 0.971916 0.658506 11.00000 0.12802 0.17502 = 0.13596 0.02157 0.05765 -0.00266 AFIX 23 H6A 2 0.218792 1.019289 0.691208 11.00000 -1.20000 H6B 2 0.208833 0.971494 0.605797 11.00000 -1.20000 AFIX 0 C7 1 0.083052 0.977188 0.636522 11.00000 0.17777 0.32701 = 0.23194 0.00791 0.01282 -0.00644 AFIX 137 H7A 2 0.054529 0.936186 0.595280 11.00000 -1.50000 H7B 2 0.062185 1.029342 0.612644 11.00000 -1.50000 H7C 2 0.064054 0.969390 0.687660 11.00000 -1.50000 AFIX 0 C8 1 0.673558 0.888082 0.516687 11.00000 0.11619 0.06704 = 0.09274 -0.00922 0.04168 0.01964 AFIX 43 H8 2 0.636215 0.845792 0.487288 11.00000 -1.20000 AFIX 0 C9 1 0.717753 0.999178 0.581559 11.00000 0.08859 0.05759 = 0.09263 -0.00645 0.04012 -0.00557 AFIX 43 H9 2 0.716430 1.049564 0.606343 11.00000 -1.20000 AFIX 0 C10 1 0.798388 0.959260 0.581580 11.00000 0.10045 0.08813 = 0.11564 -0.00385 0.04929 0.00390 AFIX 43 H10 2 0.861009 0.976918 0.605056 11.00000 -1.20000 AFIX 0 C11 1 0.832792 0.822172 0.525652 11.00000 0.14139 0.13540 = 0.16779 -0.01433 0.05940 0.04099 AFIX 23 H11A 2 0.890888 0.844589 0.517724 11.00000 -1.20000 H11B 2 0.799644 0.792487 0.474133 11.00000 -1.20000 AFIX 0 C12 1 0.857449 0.765780 0.603317 11.00000 0.18227 0.14997 = 0.19797 -0.00139 0.03568 0.09141 AFIX 23 H12A 2 0.879557 0.799294 0.654193 11.00000 -1.20000 H12B 2 0.798165 0.740946 0.605541 11.00000 -1.20000 AFIX 0 C13 1 0.929175 0.699317 0.611705 11.00000 0.24962 0.22908 = 0.26338 -0.02101 -0.00220 0.07585 AFIX 23 H13A 2 0.917548 0.658619 0.650307 11.00000 -1.20000 H13B 2 0.992592 0.721162 0.637913 11.00000 -1.20000 AFIX 0 C14 1 0.927756 0.658904 0.527400 11.00000 0.29495 0.27573 = 0.29439 -0.05859 0.02654 0.04839 AFIX 137 H14A 2 0.950367 0.604437 0.538399 11.00000 -1.50000 H14B 2 0.968434 0.688156 0.501093 11.00000 -1.50000 H14C 2 0.863569 0.658611 0.489495 11.00000 -1.50000 AFIX 0 C15 1 0.579100 0.547044 0.684193 11.00000 0.12286 0.04661 = 0.05315 0.01039 0.03477 0.00079 AFIX 43 H15 2 0.569353 0.494482 0.699795 11.00000 -1.20000 AFIX 0 C16 1 0.577815 0.651273 0.610417 11.00000 0.17422 0.05640 = 0.06734 0.00121 0.03409 0.00449 AFIX 43 H16 2 0.567089 0.686417 0.563981 11.00000 -1.20000 AFIX 0 C17 1 0.626186 0.670187 0.693707 11.00000 0.20241 0.07368 = 0.07626 -0.00189 0.02766 -0.00401 AFIX 43 H17 2 0.653428 0.719648 0.714341 11.00000 -1.20000 AFIX 0 C18 1 0.679154 0.592156 0.831992 11.00000 0.15334 0.08340 = 0.06153 -0.00890 0.03283 -0.00489 AFIX 23 H18A 2 0.653759 0.545931 0.854635 11.00000 -1.20000 H18B 2 0.669176 0.639523 0.863315 11.00000 -1.20000 AFIX 0 C19 1 0.785477 0.580326 0.846760 11.00000 0.17429 0.13251 = 0.08923 -0.00258 0.00338 -0.01920 AFIX 23 H19A 2 0.817741 0.584242 0.907915 11.00000 -1.20000 H19B 2 0.809146 0.623649 0.818460 11.00000 -1.20000 AFIX 0 C20 1 0.811204 0.500224 0.814092 11.00000 0.17023 0.15238 = 0.12198 -0.00978 0.00316 0.00210 AFIX 23 H20A 2 0.788725 0.501321 0.751756 11.00000 -1.20000 H20B 2 0.775761 0.458211 0.832941 11.00000 -1.20000 AFIX 0 C21 1 0.916430 0.475744 0.840825 11.00000 0.14623 0.28943 = 0.24017 0.00287 0.01316 0.00055 AFIX 137 H21A 2 0.929012 0.443559 0.796286 11.00000 -1.50000 H21B 2 0.930779 0.445026 0.893101 11.00000 -1.50000 H21C 2 0.955690 0.523248 0.849905 11.00000 -1.50000 AFIX 0 C22 1 0.322653 0.610055 0.430949 11.00000 0.13574 0.07232 = 0.09595 0.01871 0.05927 0.02766 AFIX 43 H22 2 0.358485 0.653375 0.421120 11.00000 -1.20000 AFIX 0 C23 1 0.201744 0.538142 0.431367 11.00000 0.12409 0.09814 = 0.10920 0.01322 0.04627 0.00777 AFIX 43 H23 2 0.139597 0.519920 0.423388 11.00000 -1.20000 AFIX 0 C24 1 0.281868 0.497017 0.469126 11.00000 0.10643 0.06841 = 0.09924 0.01042 0.04525 0.00432 AFIX 43 H24 2 0.283903 0.445270 0.491700 11.00000 -1.20000 AFIX 0 C25 1 0.163357 0.674028 0.365232 11.00000 0.16398 0.13319 = 0.15440 0.02295 0.02510 0.03740 AFIX 23 H25A 2 0.100945 0.652314 0.335012 11.00000 -1.20000 H25B 2 0.189599 0.698669 0.322997 11.00000 -1.20000 AFIX 0 C26 1 0.151579 0.739629 0.429489 11.00000 0.20165 0.17474 = 0.21376 0.00651 0.03058 0.06969 AFIX 23 H26A 2 0.142163 0.712156 0.479030 11.00000 -1.20000 H26B 2 0.211680 0.768616 0.449278 11.00000 -1.20000 AFIX 0 C27 1 0.073335 0.801063 0.400170 11.00000 0.24282 0.19511 = 0.29092 0.05376 0.02959 0.09371 AFIX 23 H27A 2 0.014983 0.770874 0.375046 11.00000 -1.20000 H27B 2 0.066329 0.826014 0.451923 11.00000 -1.20000 AFIX 0 C28 1 0.073454 0.868582 0.339096 11.00000 0.33889 0.24245 = 0.35562 0.11386 -0.01327 0.05525 AFIX 137 H28A 2 0.128690 0.901917 0.362370 11.00000 -1.50000 H28B 2 0.016596 0.900371 0.330851 11.00000 -1.50000 H28C 2 0.075155 0.846763 0.284896 11.00000 -1.50000 AFIX 0 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 0.0000 -1.0000 0.0000 -1.0000 0.0000 REM 181109a in P2/c REM wR2 = 0.2369, GooF = S = 0.853, Restrained GooF = 0.940 for all data REM R1 = 0.0755 for 2556 Fo > 4sig(Fo) and 0.1794 for all 6667 data REM 423 parameters refined using 495 restraints END WGHT 0.1243 0.0000 REM Instructions for potential hydrogen bonds HTAB O8 O4 EQIV $2 -x+1, y, -z+1/2 HTAB O8 O6_$2 EQIV $3 -x+1, -y+2, -z+1 HTAB C1 O2_$3 HTAB C1 O3_$3 HTAB C11 O8_$2 EQIV $4 -x+1, -y+1, -z+1 HTAB C15 O5_$4 HTAB C15 O7_$4 HTAB C25 O8 REM Highest difference peak 0.867, deepest hole -0.682, 1-sigma level 0.108 Q1 1 0.2065 0.7761 0.1669 11.00000 0.05 0.76 Q2 1 0.2233 0.7047 0.1917 11.00000 0.05 0.60 Q3 1 0.0838 0.6943 0.4114 11.00000 0.05 0.59 Q4 1 0.2235 0.7331 0.2190 11.00000 0.05 0.58 Q5 1 0.5540 0.7459 0.3934 11.00000 0.05 0.51 Q6 1 0.8070 0.7319 0.5516 11.00000 0.05 0.48 Q7 1 0.5452 0.6669 0.6646 11.00000 0.05 0.46 Q8 1 0.4415 0.8349 0.8282 11.00000 0.05 0.44 Q9 1 0.2075 0.7703 0.4132 11.00000 0.05 0.43 Q10 1 0.4567 0.8309 0.6498 11.00000 0.05 0.42 Q11 1 0.8401 0.5563 0.7936 11.00000 0.05 0.42 Q12 1 0.5572 0.6575 0.8639 11.00000 0.05 0.41 Q13 1 0.1250 0.8267 0.3797 11.00000 0.05 0.40 Q14 1 0.2000 0.7173 0.3827 11.00000 0.05 0.40 Q15 1 0.1763 0.8261 0.4541 11.00000 0.05 0.38 Q16 1 0.9201 0.8037 0.6041 11.00000 0.05 0.38 Q17 1 0.3580 0.8772 0.2582 11.00000 0.05 0.37 Q18 1 0.1649 0.9173 0.6237 11.00000 0.05 0.35 Q19 1 0.4404 0.7408 0.3518 11.00000 0.05 0.35 Q20 1 0.5560 0.8659 0.2812 11.00000 0.05 0.35 ; _shelx_res_checksum 27643 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, 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 0.500000 1.000000 0.500000 0.0493(4) Uani 1 2 d S . P . . Ni2 Ni 0.500000 0.500000 0.500000 0.0529(5) Uani 1 2 d S . P . . V1 V 0.44590(12) 0.84352(8) 0.33033(8) 0.0602(5) Uani 1 1 d . . . . . V2 V 0.54705(12) 0.66025(8) 0.35878(8) 0.0613(5) Uani 1 1 d . . . . . N1 N 0.3835(6) 0.8926(5) 0.6776(4) 0.077(2) Uani 1 1 d . . . . . N2 N 0.4530(5) 0.9248(4) 0.5815(4) 0.0628(19) Uani 1 1 d . . . . . N3 N 0.7700(7) 0.8890(6) 0.5409(6) 0.098(3) Uani 1 1 d . . . . . N4 N 0.6387(5) 0.9555(4) 0.5403(4) 0.063(2) Uani 1 1 d . . . . . N5 N 0.6263(7) 0.6020(5) 0.7401(5) 0.085(3) Uani 1 1 d . . . . . N6 N 0.5478(5) 0.5734(4) 0.6058(4) 0.067(2) Uani 1 1 d . . . . . N7 N 0.2259(8) 0.6081(7) 0.4078(6) 0.107(3) Uani 1 1 d . . . . . N8 N 0.3596(5) 0.5418(4) 0.4697(4) 0.063(2) Uani 1 1 d . . . . . O1 O 0.4882(6) 0.7499(4) 0.3766(4) 0.0995(19) Uani 1 1 d . U . . . O2 O 0.4705(4) 0.9127(3) 0.4051(3) 0.0625(15) Uani 1 1 d . U . . . O3 O 0.500000 0.8695(5) 0.250000 0.098(3) Uani 1 2 d S TU P . . O4 O 0.3323(6) 0.8387(6) 0.2935(6) 0.154(3) Uani 1 1 d . U . . . O5 O 0.5260(4) 0.5881(3) 0.4209(3) 0.0693(16) Uani 1 1 d . U . . . O6 O 0.6602(6) 0.6745(6) 0.3838(6) 0.150(3) Uani 1 1 d . U . . . O7 O 0.500000 0.6315(5) 0.250000 0.094(3) Uani 1 2 d S TU P . . O8 O 0.1988(7) 0.7415(7) 0.1788(7) 0.082(4) Uani 0.5 1 d . U P . . H8C H 0.232807 0.773565 0.216135 0.099 Uiso 0.5 1 d R U P . . H8D H 0.235377 0.716785 0.155125 0.099 Uiso 0.5 1 d R U P . . C1 C 0.4193(6) 0.9513(5) 0.6429(5) 0.065(2) Uani 1 1 d . U . . . H1 H 0.420666 1.005023 0.659677 0.078 Uiso 1 1 calc R U . . . C2 C 0.4330(8) 0.8446(5) 0.5723(6) 0.086(3) Uani 1 1 d . U . . . H2 H 0.445507 0.810750 0.531277 0.104 Uiso 1 1 calc R U . . . C3 C 0.3912(9) 0.8224(6) 0.6339(7) 0.107(3) Uani 1 1 d . U . . . H3 H 0.371854 0.770869 0.644237 0.129 Uiso 1 1 calc R U . . . C4 C 0.3375(7) 0.9010(6) 0.7458(6) 0.095(3) Uani 1 1 d D U . . . H4A H 0.355444 0.952324 0.774551 0.114 Uiso 1 1 calc R U . . . H4B H 0.360080 0.858490 0.787872 0.114 Uiso 1 1 calc R U . . . C5 C 0.2299(8) 0.8963(7) 0.7107(7) 0.123(3) Uani 1 1 d D U . . . H5A H 0.202280 0.891260 0.757871 0.147 Uiso 1 1 calc R U . . . H5B H 0.212014 0.849021 0.674415 0.147 Uiso 1 1 calc R U . . . C6 C 0.1906(8) 0.9719(8) 0.6585(9) 0.142(4) Uani 1 1 d D U . . . H6A H 0.218792 1.019289 0.691208 0.171 Uiso 1 1 calc R U . . . H6B H 0.208833 0.971494 0.605797 0.171 Uiso 1 1 calc R U . . . C7 C 0.0831(9) 0.9772(12) 0.6365(12) 0.256(9) Uani 1 1 d D U . . . H7A H 0.054529 0.936186 0.595280 0.384 Uiso 1 1 calc R U . . . H7B H 0.062185 1.029342 0.612644 0.384 Uiso 1 1 calc R U . . . H7C H 0.064054 0.969390 0.687660 0.384 Uiso 1 1 calc R U . . . C8 C 0.6736(9) 0.8881(6) 0.5167(6) 0.090(3) Uani 1 1 d . U . . . H8 H 0.636215 0.845792 0.487288 0.108 Uiso 1 1 calc R U . . . C9 C 0.7178(8) 0.9992(6) 0.5816(6) 0.077(3) Uani 1 1 d . U . . . H9 H 0.716430 1.049564 0.606343 0.092 Uiso 1 1 calc R U . . . C10 C 0.7984(9) 0.9593(7) 0.5816(7) 0.098(3) Uani 1 1 d . U . . . H10 H 0.861009 0.976918 0.605056 0.117 Uiso 1 1 calc R U . . . C11 C 0.8328(10) 0.8222(8) 0.5257(9) 0.145(4) Uani 1 1 d D U . . . H11A H 0.890888 0.844589 0.517724 0.174 Uiso 1 1 calc R U . . . H11B H 0.799644 0.792487 0.474133 0.174 Uiso 1 1 calc R U . . . C12 C 0.8574(11) 0.7658(8) 0.6033(9) 0.181(5) Uani 1 1 d D U . . . H12A H 0.879557 0.799294 0.654193 0.217 Uiso 1 1 calc R U . . . H12B H 0.798165 0.740946 0.605541 0.217 Uiso 1 1 calc R U . . . C13 C 0.9292(14) 0.6993(11) 0.6117(11) 0.264(7) Uani 1 1 d D U . . . H13A H 0.917548 0.658619 0.650307 0.317 Uiso 1 1 calc R U . . . H13B H 0.992592 0.721162 0.637913 0.317 Uiso 1 1 calc R U . . . C14 C 0.9278(17) 0.6589(14) 0.5274(13) 0.301(10) Uani 1 1 d D U . . . H14A H 0.950367 0.604437 0.538399 0.452 Uiso 1 1 calc R U . . . H14B H 0.968434 0.688156 0.501093 0.452 Uiso 1 1 calc R U . . . H14C H 0.863569 0.658611 0.489495 0.452 Uiso 1 1 calc R U . . . C15 C 0.5791(7) 0.5470(5) 0.6842(6) 0.072(2) Uani 1 1 d . U . . . H15 H 0.569353 0.494482 0.699795 0.087 Uiso 1 1 calc R U . . . C16 C 0.5778(9) 0.6513(6) 0.6104(6) 0.100(3) Uani 1 1 d . U . . . H16 H 0.567089 0.686417 0.563981 0.120 Uiso 1 1 calc R U . . . C17 C 0.6262(10) 0.6702(7) 0.6937(7) 0.120(3) Uani 1 1 d . U . . . H17 H 0.653428 0.719648 0.714341 0.144 Uiso 1 1 calc R U . . . C18 C 0.6792(8) 0.5922(6) 0.8320(6) 0.099(3) Uani 1 1 d D U . . . H18A H 0.653759 0.545931 0.854635 0.119 Uiso 1 1 calc R U . . . H18B H 0.669176 0.639523 0.863315 0.119 Uiso 1 1 calc R U . . . C19 C 0.7855(8) 0.5803(7) 0.8468(7) 0.140(4) Uani 1 1 d D U . . . H19A H 0.817741 0.584242 0.907915 0.167 Uiso 1 1 calc R U . . . H19B H 0.809146 0.623649 0.818460 0.167 Uiso 1 1 calc R U . . . C20 C 0.8112(9) 0.5002(8) 0.8141(9) 0.157(5) Uani 1 1 d D U . . . H20A H 0.788725 0.501321 0.751756 0.188 Uiso 1 1 calc R U . . . H20B H 0.775761 0.458211 0.832941 0.188 Uiso 1 1 calc R U . . . C21 C 0.9164(10) 0.4757(11) 0.8408(12) 0.235(8) Uani 1 1 d D U . . . H21A H 0.929012 0.443559 0.796286 0.352 Uiso 1 1 calc R U . . . H21B H 0.930779 0.445026 0.893101 0.352 Uiso 1 1 calc R U . . . H21C H 0.955690 0.523248 0.849905 0.352 Uiso 1 1 calc R U . . . C22 C 0.3227(10) 0.6101(7) 0.4309(7) 0.096(3) Uani 1 1 d . U . . . H22 H 0.358485 0.653375 0.421120 0.115 Uiso 1 1 calc R U . . . C23 C 0.2017(10) 0.5381(8) 0.4314(8) 0.108(3) Uani 1 1 d . U . . . H23 H 0.139597 0.519920 0.423388 0.129 Uiso 1 1 calc R U . . . C24 C 0.2819(9) 0.4970(6) 0.4691(7) 0.088(3) Uani 1 1 d . U . . . H24 H 0.283903 0.445270 0.491700 0.106 Uiso 1 1 calc R U . . . C25 C 0.1634(11) 0.6740(8) 0.3652(9) 0.155(4) Uani 1 1 d D U . . . H25A H 0.100945 0.652314 0.335012 0.186 Uiso 1 1 calc R U . . . H25B H 0.189599 0.698669 0.322997 0.186 Uiso 1 1 calc R U . . . C26 C 0.1516(12) 0.7396(9) 0.4295(9) 0.203(5) Uani 1 1 d D U . . . H26A H 0.142163 0.712156 0.479030 0.244 Uiso 1 1 calc R U . . . H26B H 0.211680 0.768616 0.449278 0.244 Uiso 1 1 calc R U . . . C27 C 0.0733(13) 0.8011(10) 0.4002(12) 0.253(7) Uani 1 1 d D U . . . H27A H 0.014983 0.770874 0.375046 0.304 Uiso 1 1 calc R U . . . H27B H 0.066329 0.826014 0.451923 0.304 Uiso 1 1 calc R U . . . C28 C 0.0735(10) 0.8686(9) 0.3391(10) 0.337(11) Uani 1 1 d D U . . . H28A H 0.128690 0.901917 0.362370 0.505 Uiso 1 1 calc R U . . . H28B H 0.016596 0.900371 0.330851 0.505 Uiso 1 1 calc DR U . . . H28C H 0.075155 0.846763 0.284896 0.505 Uiso 1 1 calc DR 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 0.0737(11) 0.0353(8) 0.0435(8) -0.0071(6) 0.0245(7) -0.0006(7) Ni2 0.0804(12) 0.0383(8) 0.0444(9) 0.0103(6) 0.0253(8) 0.0039(8) V1 0.0988(14) 0.0417(8) 0.0451(9) -0.0118(7) 0.0290(8) -0.0042(8) V2 0.1035(14) 0.0404(8) 0.0450(9) 0.0077(7) 0.0295(8) -0.0057(8) N1 0.121(7) 0.066(5) 0.057(5) 0.005(4) 0.044(5) -0.004(5) N2 0.086(6) 0.048(4) 0.050(4) 0.001(3) 0.015(4) -0.002(4) N3 0.099(8) 0.092(7) 0.116(7) -0.005(6) 0.052(6) 0.030(6) N4 0.084(6) 0.060(5) 0.048(4) -0.001(3) 0.027(4) 0.007(4) N5 0.156(8) 0.057(5) 0.047(5) 0.003(4) 0.037(5) 0.008(5) N6 0.107(6) 0.036(4) 0.064(5) 0.008(3) 0.036(4) 0.003(4) N7 0.111(8) 0.123(9) 0.087(7) 0.017(6) 0.031(6) 0.061(7) N8 0.088(6) 0.050(5) 0.059(5) 0.010(3) 0.036(4) 0.018(4) O1 0.196(6) 0.046(3) 0.069(4) 0.001(3) 0.060(4) 0.010(4) O2 0.105(4) 0.043(3) 0.052(3) -0.010(2) 0.041(3) -0.002(3) O3 0.199(8) 0.052(5) 0.062(5) 0.000 0.068(5) 0.000 O4 0.106(6) 0.181(8) 0.159(7) -0.093(6) 0.013(5) -0.017(6) O5 0.121(5) 0.045(3) 0.050(3) 0.016(2) 0.037(3) 0.005(3) O6 0.121(7) 0.168(8) 0.159(7) 0.064(6) 0.040(5) -0.040(6) O7 0.190(8) 0.047(5) 0.058(5) 0.000 0.057(5) 0.000 O8 0.049(7) 0.121(9) 0.081(8) -0.057(7) 0.026(6) -0.011(7) C1 0.105(6) 0.046(5) 0.061(5) -0.003(4) 0.050(5) 0.001(4) C2 0.156(7) 0.046(5) 0.074(5) -0.006(4) 0.059(5) -0.003(5) C3 0.191(8) 0.049(5) 0.100(6) -0.012(5) 0.072(6) -0.004(6) C4 0.140(7) 0.086(6) 0.078(6) -0.004(5) 0.063(6) -0.014(6) C5 0.151(8) 0.128(8) 0.114(7) -0.002(6) 0.077(7) -0.023(7) C6 0.128(8) 0.175(9) 0.136(8) 0.022(8) 0.058(7) -0.003(8) C7 0.178(16) 0.33(2) 0.232(18) 0.008(17) 0.013(15) -0.006(17) C8 0.116(7) 0.067(5) 0.093(6) -0.009(5) 0.042(5) 0.020(5) C9 0.089(7) 0.058(5) 0.093(6) -0.006(5) 0.040(5) -0.006(5) C10 0.100(7) 0.088(7) 0.116(7) -0.004(6) 0.049(6) 0.004(6) C11 0.141(8) 0.135(8) 0.168(8) -0.014(7) 0.059(7) 0.041(7) C12 0.182(9) 0.150(9) 0.198(10) -0.001(8) 0.036(8) 0.091(7) C13 0.250(13) 0.229(13) 0.263(13) -0.021(11) -0.002(12) 0.076(11) C14 0.295(19) 0.276(19) 0.294(16) -0.059(15) 0.027(17) 0.048(17) C15 0.123(7) 0.047(5) 0.053(5) 0.010(4) 0.035(5) 0.001(5) C16 0.174(8) 0.056(5) 0.067(6) 0.001(5) 0.034(6) 0.004(6) C17 0.202(9) 0.074(6) 0.076(6) -0.002(5) 0.028(6) -0.004(7) C18 0.153(8) 0.083(6) 0.062(6) -0.009(5) 0.033(6) -0.005(6) C19 0.174(9) 0.133(8) 0.089(7) -0.003(6) 0.003(7) -0.019(8) C20 0.170(10) 0.152(9) 0.122(8) -0.010(8) 0.003(8) 0.002(9) C21 0.146(14) 0.29(2) 0.240(18) 0.003(15) 0.013(14) 0.001(15) C22 0.136(7) 0.072(6) 0.096(6) 0.019(5) 0.059(6) 0.028(6) C23 0.124(8) 0.098(7) 0.109(7) 0.013(6) 0.046(6) 0.008(7) C24 0.106(8) 0.068(6) 0.099(7) 0.010(5) 0.045(6) 0.004(6) C25 0.164(8) 0.133(8) 0.154(8) 0.023(7) 0.025(7) 0.037(7) C26 0.202(10) 0.175(9) 0.214(10) 0.007(8) 0.031(9) 0.070(8) C27 0.243(12) 0.195(12) 0.291(13) 0.054(10) 0.030(12) 0.094(9) C28 0.34(2) 0.242(16) 0.356(19) 0.114(13) -0.013(17) 0.055(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 O2 Ni1 O2 180.0 3_676 . ? O2 Ni1 N4 87.6(3) 3_676 3_676 ? O2 Ni1 N4 92.4(3) . 3_676 ? O2 Ni1 N4 92.4(3) 3_676 . ? O2 Ni1 N4 87.6(3) . . ? N4 Ni1 N4 180.0 3_676 . ? O2 Ni1 N2 88.8(2) 3_676 . ? O2 Ni1 N2 91.2(2) . . ? N4 Ni1 N2 86.5(3) 3_676 . ? N4 Ni1 N2 93.5(3) . . ? O2 Ni1 N2 91.2(2) 3_676 3_676 ? O2 Ni1 N2 88.8(2) . 3_676 ? N4 Ni1 N2 93.5(3) 3_676 3_676 ? N4 Ni1 N2 86.5(3) . 3_676 ? N2 Ni1 N2 180.0 . 3_676 ? O5 Ni2 O5 180.0 3_666 . ? O5 Ni2 N6 91.3(2) 3_666 3_666 ? O5 Ni2 N6 88.7(2) . 3_666 ? O5 Ni2 N6 88.7(2) 3_666 . ? O5 Ni2 N6 91.3(2) . . ? N6 Ni2 N6 180.0(3) 3_666 . ? O5 Ni2 N8 88.0(3) 3_666 3_666 ? O5 Ni2 N8 92.0(3) . 3_666 ? N6 Ni2 N8 94.1(3) 3_666 3_666 ? N6 Ni2 N8 85.9(3) . 3_666 ? O5 Ni2 N8 92.0(3) 3_666 . ? O5 Ni2 N8 88.0(3) . . ? N6 Ni2 N8 85.9(3) 3_666 . ? N6 Ni2 N8 94.1(3) . . ? N8 Ni2 N8 180.0 3_666 . ? O4 V1 O2 107.0(4) . . ? O4 V1 O1 108.3(5) . . ? O2 V1 O1 109.2(3) . . ? O4 V1 O3 112.2(4) . . ? O2 V1 O3 109.3(3) . . ? O1 V1 O3 110.7(3) . . ? O6 V2 O5 108.4(4) . . ? O6 V2 O7 111.3(4) . . ? O5 V2 O7 109.3(3) . . ? O6 V2 O1 110.3(5) . . ? O5 V2 O1 108.6(3) . . ? O7 V2 O1 108.9(3) . . ? C1 N1 C3 107.5(7) . . ? C1 N1 C4 126.0(8) . . ? C3 N1 C4 126.4(8) . . ? C1 N2 C2 107.1(7) . . ? C1 N2 Ni1 123.6(6) . . ? C2 N2 Ni1 128.0(6) . . ? C10 N3 C8 107.4(9) . . ? C10 N3 C11 127.1(11) . . ? C8 N3 C11 125.5(11) . . ? C8 N4 C9 104.3(9) . . ? C8 N4 Ni1 129.0(8) . . ? C9 N4 Ni1 125.2(6) . . ? C15 N5 C17 105.9(8) . . ? C15 N5 C18 129.0(8) . . ? C17 N5 C18 124.8(9) . . ? C15 N6 C16 104.6(8) . . ? C15 N6 Ni2 123.9(6) . . ? C16 N6 Ni2 129.3(6) . . ? C23 N7 C22 106.9(10) . . ? C23 N7 C25 128.2(13) . . ? C22 N7 C25 124.8(12) . . ? C22 N8 C24 103.8(10) . . ? C22 N8 Ni2 129.1(8) . . ? C24 N8 Ni2 125.8(7) . . ? V1 O1 V2 142.5(4) . . ? V1 O2 Ni1 179.3(3) . . ? V1 O3 V1 151.8(5) 2_655 . ? V2 O5 Ni2 178.9(3) . . ? V2 O7 V2 148.7(5) . 2_655 ? H8C O8 H8D 108.1 . . ? N1 C1 N2 111.5(8) . . ? N1 C1 H1 124.3 . . ? N2 C1 H1 124.3 . . ? N2 C2 C3 108.0(8) . . ? N2 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? C2 C3 N1 105.7(9) . . ? C2 C3 H3 127.2 . . ? N1 C3 H3 127.2 . . ? N1 C4 C5 111.7(8) . . ? N1 C4 H4A 109.3 . . ? C5 C4 H4A 109.3 . . ? N1 C4 H4B 109.3 . . ? C5 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C4 C5 C6 110.4(9) . . ? C4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? C4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C7 C6 C5 112.0(10) . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 N3 111.3(10) . . ? N4 C8 H8 124.4 . . ? N3 C8 H8 124.4 . . ? C10 C9 N4 110.7(10) . . ? C10 C9 H9 124.6 . . ? N4 C9 H9 124.6 . . ? N3 C10 C9 106.3(11) . . ? N3 C10 H10 126.9 . . ? C9 C10 H10 126.9 . . ? N3 C11 C12 108.7(10) . . ? N3 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? N3 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C13 C12 C11 120.9(11) . . ? C13 C12 H12A 107.1 . . ? C11 C12 H12A 107.1 . . ? C13 C12 H12B 107.1 . . ? C11 C12 H12B 107.1 . . ? H12A C12 H12B 106.8 . . ? C12 C13 C14 114.7(11) . . ? C12 C13 H13A 108.6 . . ? C14 C13 H13A 108.6 . . ? C12 C13 H13B 108.6 . . ? C14 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N6 C15 N5 113.8(8) . . ? N6 C15 H15 123.1 . . ? N5 C15 H15 123.1 . . ? N6 C16 C17 109.7(9) . . ? N6 C16 H16 125.2 . . ? C17 C16 H16 125.2 . . ? N5 C17 C16 106.0(10) . . ? N5 C17 H17 127.0 . . ? C16 C17 H17 127.0 . . ? N5 C18 C19 112.5(8) . . ? N5 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? N5 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 114.0(9) . . ? C18 C19 H19A 108.8 . . ? C20 C19 H19A 108.8 . . ? C18 C19 H19B 108.8 . . ? C20 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C19 C20 C21 117.8(11) . . ? C19 C20 H20A 107.9 . . ? C21 C20 H20A 107.9 . . ? C19 C20 H20B 107.9 . . ? C21 C20 H20B 107.9 . . ? H20A C20 H20B 107.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N8 C22 N7 111.0(11) . . ? N8 C22 H22 124.5 . . ? N7 C22 H22 124.5 . . ? N7 C23 C24 108.2(13) . . ? N7 C23 H23 125.9 . . ? C24 C23 H23 125.9 . . ? C23 C24 N8 110.1(11) . . ? C23 C24 H24 125.0 . . ? N8 C24 H24 125.0 . . ? N7 C25 C26 112.5(10) . . ? N7 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N7 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 119.1(11) . . ? C27 C26 H26A 107.5 . . ? C25 C26 H26A 107.5 . . ? C27 C26 H26B 107.5 . . ? C25 C26 H26B 107.5 . . ? H26A C26 H26B 107.0 . . ? C28 C27 C26 124.7(13) . . ? C28 C27 H27A 106.2 . . ? C26 C27 H27A 106.2 . . ? C28 C27 H27B 106.2 . . ? C26 C27 H27B 106.2 . . ? H27A C27 H27B 106.4 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 O2 2.067(5) 3_676 ? Ni1 O2 2.067(5) . ? Ni1 N4 2.076(7) 3_676 ? Ni1 N4 2.076(7) . ? Ni1 N2 2.079(7) . ? Ni1 N2 2.079(7) 3_676 ? Ni2 O5 2.054(5) 3_666 ? Ni2 O5 2.054(5) . ? Ni2 N6 2.056(7) 3_666 ? Ni2 N6 2.056(7) . ? Ni2 N8 2.084(7) 3_666 ? Ni2 N8 2.084(7) . ? V1 O4 1.594(8) . ? V1 O2 1.633(5) . ? V1 O1 1.756(6) . ? V1 O3 1.768(2) . ? V2 O6 1.602(8) . ? V2 O5 1.652(5) . ? V2 O7 1.765(3) . ? V2 O1 1.783(6) . ? N1 C1 1.308(10) . ? N1 C3 1.385(11) . ? N1 C4 1.462(10) . ? N2 C1 1.312(9) . ? N2 C2 1.360(10) . ? N3 C10 1.344(13) . ? N3 C8 1.348(12) . ? N3 C11 1.505(13) . ? N4 C8 1.330(11) . ? N4 C9 1.362(11) . ? N5 C15 1.329(11) . ? N5 C17 1.358(12) . ? N5 C18 1.476(11) . ? N6 C15 1.297(9) . ? N6 C16 1.357(11) . ? N7 C23 1.302(14) . ? N7 C22 1.354(13) . ? N7 C25 1.463(13) . ? N8 C22 1.330(11) . ? N8 C24 1.356(11) . ? O8 H8C 0.8500 . ? O8 H8D 0.8499 . ? C1 H1 0.9300 . ? C2 C3 1.369(13) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.511(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.527(9) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.509(9) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8 0.9300 . ? C9 C10 1.352(13) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.527(9) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.499(9) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.521(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15 0.9300 . ? C16 C17 1.368(13) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.515(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.518(9) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.526(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22 0.9300 . ? C23 C24 1.339(14) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C26 1.552(9) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.501(9) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.497(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ?