#------------------------------------------------------------------------------ #$Date: 2018-04-15 02:00:10 +0300 (Sun, 15 Apr 2018) $ #$Revision: 207341 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/60/7046038.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_7046038 loop_ _publ_author_name 'Ojelere, Olusola Oyedele' 'Graf, David' 'Ludwig, Tim' 'Vogt, Nicolas' 'Klein, Axel' 'Mathur, Sanjay' _publ_section_title ; Reductive Transformation of V(III) Precursors into Vanadium (II) oxide Nanowires ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/C8DT00848E _journal_year 2018 _chemical_formula_moiety 'C21 H12 F9 N6 O3 V' _chemical_formula_sum 'C21 H12 F9 N6 O3 V' _chemical_formula_weight 618.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_block_doi 10.5517/ccdc.csd.cc1zbrdg _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2018-03-05 deposited with the CCDC. 2018-04-13 downloaded from the CCDC. ; _cell_angle_alpha 73.757(15) _cell_angle_beta 88.851(15) _cell_angle_gamma 66.864(14) _cell_formula_units_Z 2 _cell_length_a 9.5584(18) _cell_length_b 10.2431(19) _cell_length_c 14.555(3) _cell_measurement_reflns_used 2000 _cell_measurement_temperature 170(2) _cell_measurement_theta_max 29.682 _cell_measurement_theta_min 1.465 _cell_volume 1251.6(5) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 170(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measurement_device_type 'IPDS 2T (Stoe & Cie)' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1641 _diffrn_reflns_av_unetI/netI 0.1295 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _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 24426 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.682 _diffrn_reflns_theta_min 1.465 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.500 _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.641 _exptl_crystal_description polyhedron _exptl_crystal_F_000 616 _exptl_crystal_recrystallization_method Sublimation _refine_diff_density_max 0.751 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.135 _refine_ls_extinction_coef 0.026(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.236 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 389 _refine_ls_number_reflns 6980 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.236 _refine_ls_R_factor_all 0.2513 _refine_ls_R_factor_gt 0.1362 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3886 _refine_ls_wR_factor_ref 0.4433 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2727 _reflns_number_total 6980 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt00848e2.cif _cod_data_source_block shelx_CCDC2 _cod_original_cell_volume 1251.6(4) _cod_database_code 7046038 _shelx_shelxl_version_number 2014/7 _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_res_file ; shelx.res created by SHELXL-2014/7 TITL SIR92 run in space group P -1 CELL 0.71073 9.5584 10.2431 14.5553 73.757 88.851 66.864 ZERR 2.00 0.0018 0.0019 0.0028 0.015 0.015 0.014 LATT 1 SFAC C H N F V O UNIT 42 24 12 18 2 6 MERG 2 FMAP 2 PLAN 25 ACTA BOND $H CONF LIST 6 L.S. 10 TEMP -103.00 WGHT 0.200000 EXTI 0.026285 FVAR 0.57252 V1 5 0.794213 0.445016 0.766495 11.00000 0.07279 0.06083 = 0.06234 -0.02317 0.01683 -0.03753 O3 6 1.006073 0.308815 0.793980 11.00000 0.08719 0.06959 = 0.07321 -0.02286 0.00911 -0.04073 O2 6 0.721210 0.351720 0.880552 11.00000 0.10154 0.06826 = 0.06925 -0.03091 0.02780 -0.04662 C14 1 0.721299 0.151957 1.007611 11.00000 0.09916 0.09341 = 0.05808 -0.01319 0.01324 -0.06190 O1 6 0.849453 0.550797 0.646600 11.00000 0.07291 0.05764 = 0.07904 -0.02498 0.02229 -0.03145 N4 3 1.116040 0.468161 0.820420 11.00000 0.06411 0.07050 = 0.08118 -0.02972 0.01066 -0.03288 N6 3 0.731297 0.133331 0.849725 11.00000 0.09094 0.06706 = 0.07733 -0.01889 0.01232 -0.04515 C9 1 0.993416 0.558148 0.856903 11.00000 0.07394 0.06008 = 0.06565 -0.01728 0.00979 -0.03508 N3 3 0.847981 0.569702 0.842445 11.00000 0.07209 0.06578 = 0.06302 -0.02452 0.01132 -0.03261 N1 3 0.575335 0.621701 0.713995 11.00000 0.07590 0.07262 = 0.05897 -0.02206 0.01733 -0.04405 N5 3 0.742536 0.305304 0.700507 11.00000 0.09254 0.07309 = 0.08036 -0.03722 0.03219 -0.05560 N2 3 0.673710 0.794140 0.616939 11.00000 0.06281 0.07152 = 0.08545 -0.01447 -0.00045 -0.03303 C18 1 0.670884 0.139655 0.601226 11.00000 0.13488 0.10275 = 0.09531 -0.05444 0.02264 -0.07199 AFIX 43 H18 2 0.651049 0.079848 0.568172 11.00000 -1.20000 AFIX 0 C16 1 0.721123 0.183417 0.749197 11.00000 0.08224 0.06606 = 0.08282 -0.03014 0.01875 -0.03454 F7 4 0.632963 0.251165 1.048995 11.00000 0.25978 0.15461 = 0.11352 -0.03624 0.08400 -0.06728 F9 4 0.668169 0.050294 1.026295 11.00000 0.29760 0.19659 = 0.08862 -0.03159 0.04628 -0.20141 C15 1 0.725705 0.220116 0.899100 11.00000 0.05964 0.05630 = 0.07490 -0.01241 0.00625 -0.02589 C6 1 0.304089 0.711288 0.727091 11.00000 0.07667 0.11694 = 0.06450 -0.02838 0.02037 -0.05215 AFIX 43 H6 2 0.219540 0.690758 0.751339 11.00000 -1.20000 AFIX 0 C3 1 0.552606 0.759815 0.661625 11.00000 0.06879 0.07252 = 0.06699 -0.02672 0.01690 -0.04006 C10 1 1.026284 0.643244 0.907238 11.00000 0.07843 0.07006 = 0.07615 -0.02804 0.00504 -0.03984 AFIX 43 H10 2 1.127664 0.635962 0.915668 11.00000 -1.20000 AFIX 0 C12 1 0.761626 0.745062 0.932991 11.00000 0.08930 0.07748 = 0.07759 -0.03564 0.00328 -0.03092 AFIX 43 H12 2 0.679805 0.807732 0.959372 11.00000 -1.20000 AFIX 0 C7 1 0.446600 0.601282 0.744816 11.00000 0.07718 0.09609 = 0.07301 -0.03128 0.01990 -0.05855 AFIX 43 H7 2 0.458167 0.504038 0.780782 11.00000 -1.20000 AFIX 0 F6 4 1.266570 0.152799 0.746892 11.00000 0.12454 0.17310 = 0.38211 -0.18888 0.11652 -0.06926 C19 1 0.681218 0.267462 0.553022 11.00000 0.16299 0.13378 = 0.06145 -0.04857 0.03099 -0.10673 AFIX 43 H19 2 0.661547 0.302828 0.484909 11.00000 -1.20000 AFIX 0 C025 1 1.259589 0.270756 0.760567 11.00000 0.07481 0.07003 = 0.10870 -0.02798 0.00085 -0.02135 C11 1 0.907281 0.738324 0.944443 11.00000 0.11071 0.07814 = 0.10084 -0.04773 0.02014 -0.05227 AFIX 43 H11 2 0.926375 0.798366 0.977614 11.00000 -1.20000 AFIX 0 C2 1 0.802199 0.692398 0.612275 11.00000 0.06441 0.07511 = 0.07413 -0.01841 0.00220 -0.03569 C1 1 0.914629 0.742134 0.560795 11.00000 0.09638 0.08227 = 0.09891 0.00077 0.00894 -0.05189 C8 1 1.112260 0.359814 0.795641 11.00000 0.07129 0.07186 = 0.06973 -0.02285 0.01898 -0.03441 C13 1 0.736764 0.659307 0.882606 11.00000 0.07653 0.07682 = 0.06670 -0.03114 0.01369 -0.03652 AFIX 43 H13 2 0.636355 0.663418 0.875776 11.00000 -1.20000 AFIX 0 PART 1 F3B 4 1.050866 0.678081 0.596288 10.50000 0.07769 0.28556 = 0.17207 0.16047 -0.07713 -0.12114 PART 0 C20 1 0.720601 0.348285 0.602400 11.00000 0.13172 0.09008 = 0.07580 -0.03598 0.02680 -0.07278 AFIX 43 H20 2 0.732582 0.435793 0.566932 11.00000 -1.20000 AFIX 0 F4 4 1.304140 0.343636 0.693246 11.00000 0.20799 0.12458 = 0.21631 -0.00862 0.15913 -0.00728 C17 1 0.690459 0.097068 0.702631 11.00000 0.13040 0.08605 = 0.09370 -0.03849 0.02640 -0.06752 AFIX 43 H17 2 0.682312 0.007924 0.738827 11.00000 -1.20000 AFIX 0 F5 4 1.375420 0.216600 0.830780 11.00000 0.09431 0.26050 = 0.24084 -0.13998 0.00008 0.00092 C4 1 0.409638 0.878562 0.640126 11.00000 0.06390 0.07546 = 0.10716 -0.03455 0.01732 -0.02467 AFIX 43 H4 2 0.399855 0.974811 0.603231 11.00000 -1.20000 AFIX 0 PART 2 F2B 4 0.880983 0.879480 0.525934 10.50000 0.07168 0.09288 = 0.23769 0.02980 0.03856 -0.02508 PART 0 C5 1 0.282429 0.855225 0.672850 11.00000 0.07594 0.09550 = 0.09687 -0.02856 0.01876 -0.03272 AFIX 43 H5 2 0.183632 0.934147 0.659020 11.00000 -1.20000 AFIX 0 F1B 4 0.906158 0.721466 0.470029 10.50000 0.19653 0.24096 = 0.09206 -0.05827 0.03548 -0.12831 F8 4 0.845867 0.103517 1.054626 11.00000 0.17524 0.31544 = 0.09656 0.03154 -0.02318 -0.13975 F2A 4 0.852929 0.850036 0.480625 10.50000 0.23285 0.35702 = 0.12443 0.02485 0.01273 -0.25039 F10 4 1.033476 0.640741 0.552963 10.50000 0.10305 0.10614 = 0.30150 -0.07495 0.13637 -0.04512 F11 4 0.952865 0.823630 0.606582 10.50000 0.08549 0.15346 = 0.31445 -0.10416 0.04015 -0.07602 HKLF 4 REM SIR92 run in space group P -1 REM R1 = 0.1362 for 2727 Fo > 4sig(Fo) and 0.2513 for all 6980 data REM 389 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.751, deepest hole -0.600, 1-sigma level 0.135 Q1 1 1.2189 0.2778 0.6612 11.00000 0.05 0.75 Q2 1 0.3603 0.5727 0.8456 11.00000 0.05 0.65 Q3 1 1.0192 0.5609 0.6206 11.00000 0.05 0.63 Q4 1 0.5788 0.1760 1.0236 11.00000 0.05 0.50 Q5 1 0.6601 0.2627 0.9478 11.00000 0.05 0.48 Q6 1 0.8895 0.3165 0.8576 11.00000 0.05 0.48 Q7 1 0.7227 0.4080 0.8583 11.00000 0.05 0.48 Q8 1 0.7818 0.3159 0.8420 11.00000 0.05 0.47 Q9 1 1.0172 0.2984 0.8444 11.00000 0.05 0.45 Q10 1 1.1283 0.6070 0.5111 11.00000 0.05 0.45 Q11 1 0.8997 0.7408 0.8696 11.00000 0.05 0.44 Q12 1 1.3568 0.1423 0.7910 11.00000 0.05 0.43 Q13 1 1.0490 0.2389 0.8040 11.00000 0.05 0.42 Q14 1 0.6838 0.5651 0.6608 11.00000 0.05 0.42 Q15 1 1.2583 0.1225 0.7594 11.00000 0.05 0.41 Q16 1 1.1384 0.1961 0.7881 11.00000 0.05 0.41 Q17 1 0.8924 0.6155 0.9206 11.00000 0.05 0.41 Q18 1 0.8970 0.2752 0.7945 11.00000 0.05 0.40 Q19 1 1.0814 0.7738 0.8162 11.00000 0.05 0.40 Q20 1 1.1755 0.4155 0.7240 11.00000 0.05 0.40 Q21 1 0.8001 0.0216 1.0280 11.00000 0.05 0.40 Q22 1 0.5491 0.7655 0.6263 11.00000 0.05 0.38 Q23 1 0.8651 0.5434 0.9977 11.00000 0.05 0.37 Q24 1 0.7200 0.6151 0.7342 11.00000 0.05 0.37 Q25 1 0.6264 0.7457 0.9553 11.00000 0.05 0.36 ; _shelx_res_checksum 23663 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 V1 V 0.79421(16) 0.44502(14) 0.76649(10) 0.0609(5) Uani 1 1 d . . . . . O3 O 1.0061(7) 0.3088(6) 0.7940(4) 0.0733(16) Uani 1 1 d . . . . . O2 O 0.7212(7) 0.3517(6) 0.8806(4) 0.0736(16) Uani 1 1 d . . . . . C14 C 0.7213(13) 0.1520(12) 1.0076(7) 0.078(3) Uani 1 1 d . . . . . O1 O 0.8495(6) 0.5508(6) 0.6466(4) 0.0674(14) Uani 1 1 d . . . . . N4 N 1.1160(8) 0.4682(8) 0.8204(5) 0.0685(18) Uani 1 1 d . . . . . N6 N 0.7313(9) 0.1333(8) 0.8497(6) 0.0747(19) Uani 1 1 d . . . . . C9 C 0.9934(10) 0.5581(9) 0.8569(6) 0.064(2) Uani 1 1 d . . . . . N3 N 0.8480(8) 0.5697(7) 0.8424(5) 0.0643(16) Uani 1 1 d . . . . . N1 N 0.5753(8) 0.6217(7) 0.7140(5) 0.0642(17) Uani 1 1 d . . . . . N5 N 0.7425(9) 0.3053(8) 0.7005(5) 0.0719(19) Uani 1 1 d . . . . . N2 N 0.6737(8) 0.7941(8) 0.6169(6) 0.0731(19) Uani 1 1 d . . . . . C18 C 0.6709(14) 0.1397(12) 0.6012(8) 0.098(3) Uani 1 1 d . . . . . H18 H 0.6510 0.0798 0.5682 0.117 Uiso 1 1 calc R U . . . C16 C 0.7211(11) 0.1834(9) 0.7492(7) 0.074(2) Uani 1 1 d . . . . . F7 F 0.6330(15) 0.2512(11) 1.0490(7) 0.183(4) Uani 1 1 d . . . . . F9 F 0.6682(13) 0.0503(10) 1.0263(5) 0.164(4) Uani 1 1 d . . . . . C15 C 0.7257(9) 0.2201(9) 0.8991(6) 0.064(2) Uani 1 1 d . . . . . C6 C 0.3041(11) 0.7113(12) 0.7271(7) 0.082(3) Uani 1 1 d . . . . . H6 H 0.2195 0.6908 0.7513 0.098 Uiso 1 1 calc R U . . . C3 C 0.5526(10) 0.7598(9) 0.6616(6) 0.064(2) Uani 1 1 d . . . . . C10 C 1.0263(11) 0.6432(9) 0.9072(6) 0.070(2) Uani 1 1 d . . . . . H10 H 1.1277 0.6360 0.9157 0.084 Uiso 1 1 calc R U . . . C12 C 0.7616(12) 0.7451(10) 0.9330(7) 0.079(2) Uani 1 1 d . . . . . H12 H 0.6798 0.8077 0.9594 0.095 Uiso 1 1 calc R U . . . C7 C 0.4466(11) 0.6013(11) 0.7448(6) 0.073(2) Uani 1 1 d . . . . . H7 H 0.4582 0.5040 0.7808 0.088 Uiso 1 1 calc R U . . . F6 F 1.2666(10) 0.1528(11) 0.7469(10) 0.201(5) Uani 1 1 d . . . . . C19 C 0.6812(14) 0.2675(13) 0.5530(7) 0.100(4) Uani 1 1 d . . . . . H19 H 0.6615 0.3028 0.4849 0.120 Uiso 1 1 calc R U . . . C025 C 1.2596(12) 0.2708(11) 0.7606(9) 0.087(3) Uani 1 1 d . . . . . C11 C 0.9073(13) 0.7383(11) 0.9444(8) 0.087(3) Uani 1 1 d . . . . . H11 H 0.9264 0.7984 0.9776 0.105 Uiso 1 1 calc R U . . . C2 C 0.8022(10) 0.6924(10) 0.6123(6) 0.069(2) Uani 1 1 d . . . . . C1 C 0.9146(14) 0.7421(13) 0.5608(9) 0.093(3) Uani 1 1 d . . . . . C8 C 1.1123(10) 0.3598(9) 0.7956(6) 0.069(2) Uani 1 1 d . . . . . C13 C 0.7368(11) 0.6593(9) 0.8826(6) 0.069(2) Uani 1 1 d . . . . . H13 H 0.6364 0.6634 0.8758 0.083 Uiso 1 1 calc R U . . . F3B F 1.051(3) 0.678(4) 0.596(2) 0.21(2) Uani 0.5 1 d . . P A 1 C20 C 0.7206(13) 0.3483(11) 0.6024(7) 0.088(3) Uani 1 1 d . . . . . H20 H 0.7326 0.4358 0.5669 0.105 Uiso 1 1 calc R U . . . F4 F 1.3041(13) 0.3436(10) 0.6932(8) 0.214(6) Uani 1 1 d . . . . . C17 C 0.6905(13) 0.0971(11) 0.7026(8) 0.093(3) Uani 1 1 d . . . . . H17 H 0.6823 0.0079 0.7388 0.112 Uiso 1 1 calc R U . . . F5 F 1.3754(10) 0.2166(15) 0.8308(9) 0.207(6) Uani 1 1 d . . . . . C4 C 0.4096(10) 0.8786(11) 0.6401(8) 0.082(3) Uani 1 1 d . . . . . H4 H 0.3999 0.9748 0.6032 0.098 Uiso 1 1 calc R U . . . F2B F 0.881(3) 0.879(2) 0.526(3) 0.155(15) Uani 0.5 1 d . . P A 2 C5 C 0.2824(12) 0.8552(12) 0.6729(8) 0.090(3) Uani 1 1 d . . . . . H5 H 0.1836 0.9341 0.6590 0.108 Uiso 1 1 calc R U . . . F1B F 0.906(4) 0.721(4) 0.4700(17) 0.162(9) Uani 0.5 1 d . . P A . F8 F 0.8459(13) 0.1035(15) 1.0546(6) 0.202(5) Uani 1 1 d . . . . . F2A F 0.853(5) 0.850(6) 0.481(3) 0.22(2) Uani 0.5 1 d . . P A . F10 F 1.033(3) 0.641(2) 0.553(3) 0.168(15) Uani 0.5 1 d . . P A . F11 F 0.953(3) 0.824(4) 0.607(3) 0.168(10) Uani 0.5 1 d . . P A . 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 V1 0.0728(10) 0.0608(8) 0.0623(9) -0.0232(6) 0.0168(7) -0.0375(7) O3 0.087(4) 0.070(3) 0.073(4) -0.023(3) 0.009(3) -0.041(3) O2 0.102(4) 0.068(3) 0.069(3) -0.031(3) 0.028(3) -0.047(3) C14 0.099(7) 0.093(6) 0.058(5) -0.013(5) 0.013(5) -0.062(6) O1 0.073(4) 0.058(3) 0.079(4) -0.025(3) 0.022(3) -0.031(3) N4 0.064(4) 0.071(4) 0.081(5) -0.030(4) 0.011(4) -0.033(3) N6 0.091(5) 0.067(4) 0.077(5) -0.019(4) 0.012(4) -0.045(4) C9 0.074(5) 0.060(4) 0.066(5) -0.017(4) 0.010(4) -0.035(4) N3 0.072(4) 0.066(4) 0.063(4) -0.025(3) 0.011(3) -0.033(3) N1 0.076(4) 0.073(4) 0.059(4) -0.022(3) 0.017(3) -0.044(4) N5 0.093(5) 0.073(4) 0.080(5) -0.037(4) 0.032(4) -0.056(4) N2 0.063(4) 0.072(4) 0.085(5) -0.014(4) 0.000(4) -0.033(4) C18 0.135(9) 0.103(7) 0.095(8) -0.054(6) 0.023(7) -0.072(7) C16 0.082(6) 0.066(5) 0.083(6) -0.030(4) 0.019(5) -0.035(5) F7 0.260(12) 0.155(7) 0.114(6) -0.036(6) 0.084(7) -0.067(8) F9 0.298(12) 0.197(8) 0.089(5) -0.032(5) 0.046(6) -0.201(9) C15 0.060(5) 0.056(4) 0.075(5) -0.012(4) 0.006(4) -0.026(4) C6 0.077(6) 0.117(8) 0.064(5) -0.028(5) 0.020(5) -0.052(6) C3 0.069(5) 0.073(5) 0.067(5) -0.027(4) 0.017(4) -0.040(4) C10 0.078(6) 0.070(5) 0.076(5) -0.028(4) 0.005(4) -0.040(5) C12 0.089(7) 0.077(6) 0.078(6) -0.036(5) 0.003(5) -0.031(5) C7 0.077(6) 0.096(6) 0.073(5) -0.031(5) 0.020(4) -0.059(5) F6 0.125(6) 0.173(8) 0.382(17) -0.189(10) 0.117(9) -0.069(6) C19 0.163(11) 0.134(9) 0.061(5) -0.049(6) 0.031(6) -0.107(9) C025 0.075(6) 0.070(6) 0.109(8) -0.028(6) 0.001(6) -0.021(5) C11 0.111(8) 0.078(6) 0.101(7) -0.048(5) 0.020(6) -0.052(6) C2 0.064(5) 0.075(5) 0.074(5) -0.018(4) 0.002(4) -0.036(5) C1 0.096(8) 0.082(7) 0.099(8) 0.001(6) 0.009(6) -0.052(7) C8 0.071(5) 0.072(5) 0.070(5) -0.023(4) 0.019(4) -0.034(4) C13 0.077(5) 0.077(5) 0.067(5) -0.031(4) 0.014(4) -0.037(5) F3B 0.078(13) 0.29(4) 0.172(19) 0.16(2) -0.077(15) -0.12(2) C20 0.132(9) 0.090(6) 0.076(6) -0.036(5) 0.027(6) -0.073(7) F4 0.208(10) 0.125(6) 0.216(10) -0.009(6) 0.159(9) -0.007(6) C17 0.130(9) 0.086(6) 0.094(7) -0.038(6) 0.026(6) -0.068(7) F5 0.094(6) 0.260(12) 0.241(12) -0.140(11) 0.000(7) 0.001(7) C4 0.064(5) 0.075(6) 0.107(7) -0.035(5) 0.017(5) -0.025(5) F2B 0.072(12) 0.093(11) 0.24(4) 0.030(16) 0.039(15) -0.025(11) C5 0.076(6) 0.096(7) 0.097(7) -0.029(6) 0.019(6) -0.033(5) F1B 0.20(2) 0.24(3) 0.092(12) -0.058(17) 0.035(13) -0.13(2) F8 0.175(10) 0.315(14) 0.097(6) 0.032(7) -0.023(6) -0.140(10) F2A 0.23(4) 0.36(5) 0.12(2) 0.02(3) 0.013(19) -0.25(4) F10 0.103(16) 0.106(12) 0.30(4) -0.07(2) 0.14(2) -0.045(12) F11 0.085(14) 0.153(19) 0.31(4) -0.10(2) 0.040(17) -0.076(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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 '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 O3 V1 O2 97.5(3) O3 V1 O1 87.5(2) O2 V1 O1 175.0(3) O3 V1 N3 87.2(3) O2 V1 N3 89.8(2) O1 V1 N3 91.2(2) O3 V1 N1 168.7(2) O2 V1 N1 93.7(3) O1 V1 N1 81.4(2) N3 V1 N1 90.8(3) O3 V1 N5 91.2(3) O2 V1 N5 86.0(2) O1 V1 N5 93.1(2) N3 V1 N5 175.4(3) N1 V1 N5 91.6(3) C8 O3 V1 119.7(5) C15 O2 V1 123.2(5) F8 C14 F9 109.4(11) F8 C14 F7 102.2(11) F9 C14 F7 104.6(10) F8 C14 C15 113.0(9) F9 C14 C15 113.8(8) F7 C14 C15 112.9(9) C2 O1 V1 125.6(5) C8 N4 C9 121.7(7) C15 N6 C16 120.1(7) N3 C9 N4 122.9(7) N3 C9 C10 121.4(8) N4 C9 C10 115.7(7) C13 N3 C9 118.1(7) C13 N3 V1 119.4(6) C9 N3 V1 122.4(5) C3 N1 C7 115.7(8) C3 N1 V1 124.7(5) C7 N1 V1 119.0(6) C16 N5 C20 118.1(7) C16 N5 V1 124.2(6) C20 N5 V1 117.6(5) C2 N2 C3 121.7(7) C19 C18 C17 117.8(9) C19 C18 H18 121.1 C17 C18 H18 121.1 N5 C16 C17 121.4(9) N5 C16 N6 123.4(8) C17 C16 N6 115.2(8) N6 C15 O2 135.5(8) N6 C15 C14 112.9(7) O2 C15 C14 111.6(8) C7 C6 C5 119.5(9) C7 C6 H6 120.2 C5 C6 H6 120.2 N1 C3 C4 123.6(8) N1 C3 N2 121.7(8) C4 C3 N2 114.5(8) C11 C10 C9 118.6(8) C11 C10 H10 120.7 C9 C10 H10 120.7 C11 C12 C13 118.8(9) C11 C12 H12 120.6 C13 C12 H12 120.6 C6 C7 N1 124.1(9) C6 C7 H7 118.0 N1 C7 H7 118.0 C18 C19 C20 120.2(10) C18 C19 H19 119.9 C20 C19 H19 119.9 F4 C025 F6 111.8(12) F4 C025 F5 102.5(11) F6 C025 F5 100.8(10) F4 C025 C8 115.0(9) F6 C025 C8 115.6(9) F5 C025 C8 109.3(10) C12 C11 C10 119.7(8) C12 C11 H11 120.1 C10 C11 H11 120.1 N2 C2 O1 129.5(8) N2 C2 C1 116.4(9) O1 C2 C1 114.1(9) F10 C1 F3B 41(2) F10 C1 F2B 126.2(16) F10 C1 F2A 115(3) F3B C1 F2A 129.4(18) F2B C1 F2A 40(2) F10 C1 F11 107.8(19) F3B C1 F11 68(2) F2B C1 F11 56.2(18) F2A C1 F11 96(2) F10 C1 F1B 70(2) F3B C1 F1B 109(2) F2B C1 F1B 93(2) F2A C1 F1B 55(2) F11 C1 F1B 142(2) F10 C1 C2 114.4(12) F3B C1 C2 118.1(12) F2B C1 C2 119.3(14) F2A C1 C2 112.5(16) F11 C1 C2 109.8(15) F1B C1 C2 104.5(14) N4 C8 O3 133.1(8) N4 C8 C025 114.0(8) O3 C8 C025 112.9(8) N3 C13 C12 123.3(8) N3 C13 H13 118.4 C12 C13 H13 118.4 F10 F3B C1 68.3(17) F10 F3B F11 125(3) C1 F3B F11 59.3(15) N5 C20 C19 121.8(9) N5 C20 H20 119.1 C19 C20 H20 119.1 C16 C17 C18 120.4(9) C16 C17 H17 119.8 C18 C17 H17 119.8 C5 C4 C3 119.5(10) C5 C4 H4 120.3 C3 C4 H4 120.3 F2A F2B F11 138(4) F2A F2B C1 73(4) F11 F2B C1 65.7(15) C4 C5 C6 117.6(10) C4 C5 H5 121.2 C6 C5 H5 121.2 F2A F1B C1 58.7(19) F2A F1B F10 100(3) C1 F1B F10 49.5(11) F2B F2A F1B 128(6) F2B F2A C1 67(3) F1B F2A C1 66(3) F3B F10 C1 70(2) F3B F10 F1B 126(3) C1 F10 F1B 60.1(15) F2B F11 C1 58.1(17) C1 F11 F3B 52.4(12) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance V1 O3 1.925(6) V1 O2 1.936(6) V1 O1 1.963(6) V1 N3 2.109(7) V1 N1 2.133(7) V1 N5 2.135(6) O3 C8 1.315(10) O2 C15 1.282(9) C14 F8 1.229(13) C14 F9 1.291(11) C14 F7 1.325(13) C14 C15 1.545(12) O1 C2 1.283(10) N4 C8 1.272(10) N4 C9 1.380(10) N6 C15 1.276(10) N6 C16 1.400(11) C9 N3 1.364(10) C9 C10 1.406(11) N3 C13 1.350(10) N1 C3 1.338(10) N1 C7 1.374(10) N5 C16 1.343(10) N5 C20 1.366(11) N2 C2 1.277(11) N2 C3 1.431(10) C18 C19 1.342(14) C18 C17 1.411(15) C18 H18 0.9500 C16 C17 1.369(12) C6 C7 1.355(13) C6 C5 1.398(14) C6 H6 0.9500 C3 C4 1.394(12) C10 C11 1.391(13) C10 H10 0.9500 C12 C11 1.378(15) C12 C13 1.377(11) C12 H12 0.9500 C7 H7 0.9500 F6 C025 1.255(12) C19 C20 1.390(12) C19 H19 0.9500 C025 F4 1.234(13) C025 F5 1.350(14) C025 C8 1.516(13) C11 H11 0.9500 C2 C1 1.470(13) C1 F10 1.231(19) C1 F3B 1.25(2) C1 F2B 1.26(2) C1 F2A 1.31(4) C1 F11 1.35(2) C1 F1B 1.40(2) C13 H13 0.9500 F3B F10 0.87(4) F3B F11 1.46(4) C20 H20 0.9500 C17 H17 0.9500 C4 C5 1.380(13) C4 H4 0.9500 F2B F2A 0.88(5) F2B F11 1.23(4) C5 H5 0.9500 F1B F2A 1.27(5) F1B F10 1.53(4) 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 C8 N4 C9 N3 -20.8(13) C8 N4 C9 C10 161.8(8) N4 C9 N3 C13 179.0(7) C10 C9 N3 C13 -3.7(12) N4 C9 N3 V1 2.3(11) C10 C9 N3 V1 179.6(6) C20 N5 C16 C17 5.3(14) V1 N5 C16 C17 -179.0(7) C20 N5 C16 N6 -176.1(9) V1 N5 C16 N6 -0.4(13) C15 N6 C16 N5 16.7(14) C15 N6 C16 C17 -164.6(9) C16 N6 C15 O2 -5.2(16) C16 N6 C15 C14 173.9(8) V1 O2 C15 N6 -23.1(14) V1 O2 C15 C14 157.7(6) F8 C14 C15 N6 101.3(12) F9 C14 C15 N6 -24.3(13) F7 C14 C15 N6 -143.3(10) F8 C14 C15 O2 -79.3(13) F9 C14 C15 O2 155.1(10) F7 C14 C15 O2 36.0(13) C7 N1 C3 C4 1.3(12) V1 N1 C3 C4 -170.2(7) C7 N1 C3 N2 -173.8(7) V1 N1 C3 N2 14.6(11) C2 N2 C3 N1 10.9(13) C2 N2 C3 C4 -164.6(8) N3 C9 C10 C11 1.4(13) N4 C9 C10 C11 178.9(8) C5 C6 C7 N1 1.2(14) C3 N1 C7 C6 -1.6(12) V1 N1 C7 C6 170.5(7) C17 C18 C19 C20 4.4(19) C13 C12 C11 C10 -1.5(15) C9 C10 C11 C12 1.2(14) C3 N2 C2 O1 -3.0(15) C3 N2 C2 C1 177.4(9) V1 O1 C2 N2 -33.3(13) V1 O1 C2 C1 146.4(8) N2 C2 C1 F10 -176(3) O1 C2 C1 F10 4(3) N2 C2 C1 F3B 138(3) O1 C2 C1 F3B -42(3) N2 C2 C1 F2B 1(3) O1 C2 C1 F2B -179(3) N2 C2 C1 F2A -43(3) O1 C2 C1 F2A 137(3) N2 C2 C1 F11 63(2) O1 C2 C1 F11 -117(2) N2 C2 C1 F1B -101(2) O1 C2 C1 F1B 79(2) C9 N4 C8 O3 2.2(15) C9 N4 C8 C025 -178.0(8) V1 O3 C8 N4 33.4(13) V1 O3 C8 C025 -146.5(7) F4 C025 C8 N4 -55.8(15) F6 C025 C8 N4 171.5(11) F5 C025 C8 N4 58.7(13) F4 C025 C8 O3 124.1(12) F6 C025 C8 O3 -8.6(15) F5 C025 C8 O3 -121.4(11) C9 N3 C13 C12 3.5(12) V1 N3 C13 C12 -179.7(7) C11 C12 C13 N3 -0.9(14) F2A C1 F3B F10 -83(4) F11 C1 F3B F10 -163(3) F1B C1 F3B F10 -23(3) C2 C1 F3B F10 96(2) F10 C1 F3B F11 163(3) F2A C1 F3B F11 80(4) F1B C1 F3B F11 140(2) C2 C1 F3B F11 -101.5(19) C16 N5 C20 C19 -1.7(15) V1 N5 C20 C19 -177.7(9) C18 C19 C20 N5 -3.2(18) N5 C16 C17 C18 -4.1(16) N6 C16 C17 C18 177.2(10) C19 C18 C17 C16 -0.9(18) N1 C3 C4 C5 -0.7(14) N2 C3 C4 C5 174.7(9) F10 C1 F2B F2A 86(4) F11 C1 F2B F2A 174(4) F1B C1 F2B F2A 18(4) C2 C1 F2B F2A -91(4) F10 C1 F2B F11 -88(3) F2A C1 F2B F11 -174(4) F1B C1 F2B F11 -156.1(18) C2 C1 F2B F11 95(2) C3 C4 C5 C6 0.2(15) C7 C6 C5 C4 -0.5(15) F10 C1 F1B F2A -141(2) F3B C1 F1B F2A -126(2) F2B C1 F1B F2A -14(2) F11 C1 F1B F2A -47(4) C2 C1 F1B F2A 108(2) F3B C1 F1B F10 15.8(18) F2B C1 F1B F10 127.4(17) F2A C1 F1B F10 141(2) F11 C1 F1B F10 94(3) C2 C1 F1B F10 -111.2(13) F11 F2B F2A F1B -17(9) C1 F2B F2A F1B -26(4) F11 F2B F2A C1 8(5) C1 F1B F2A F2B 26(4) F10 F1B F2A F2B -3(6) F10 F1B F2A C1 -28.8(16) F10 C1 F2A F2B -118(3) F11 C1 F2A F2B -5(3) F1B C1 F2A F2B -158(4) C2 C1 F2A F2B 109(3) F10 C1 F2A F1B 40(2) F3B C1 F2A F1B 86(4) F2B C1 F2A F1B 158(4) F11 C1 F2A F1B 153(2) C2 C1 F2A F1B -93(3) F11 F3B F10 C1 -18(3) C1 F3B F10 F1B 25(2) F11 F3B F10 F1B 6(5) F2A C1 F10 F3B 123(3) F11 C1 F10 F3B 17(3) F1B C1 F10 F3B 157(3) C2 C1 F10 F3B -105(2) F3B C1 F10 F1B -157(3) F2B C1 F10 F1B -79(3) F2A C1 F10 F1B -34.4(19) F11 C1 F10 F1B -140(2) C2 C1 F10 F1B 97.6(17) F2A F1B F10 F3B 6(4) C1 F1B F10 F3B -27(3) F2A F1B F10 C1 32.8(19) F2A F2B F11 C1 -9(5) F10 C1 F11 F2B 122(2) F2A C1 F11 F2B 4(3) F1B C1 F11 F2B 41(3) C2 C1 F11 F2B -112.7(18) F10 C1 F11 F3B -12(2) F2A C1 F11 F3B -130(2) F1B C1 F11 F3B -93(3) C2 C1 F11 F3B 113.3(14) F10 F3B F11 C1 20(3)