#------------------------------------------------------------------------------ #$Date: 2019-11-17 11:31:23 +0200 (Sun, 17 Nov 2019) $ #$Revision: 229605 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/60/7046037.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_7046037 loop_ _publ_author_name 'Ojelere, Olusola' 'Graf, David' 'Ludwig, Tim' 'Vogt, Nicholas' 'Klein, Axel' 'Mathur, Sanjay' _publ_section_title ; Reductive transformation of V(iii) precursors into vanadium(ii) oxide nanowires. ; _journal_issue 19 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 6842 _journal_page_last 6849 _journal_paper_doi 10.1039/c8dt00848e _journal_volume 47 _journal_year 2018 _chemical_formula_moiety 'C24 H15 F9 N3 O3 V' _chemical_formula_sum 'C24 H15 F9 N3 O3 V' _chemical_formula_weight 615.33 _chemical_name_common V(PyTFP)3 _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.cc1zbrfh _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 87.461(9) _cell_angle_beta 73.130(9) _cell_angle_gamma 82.194(9) _cell_formula_units_Z 2 _cell_length_a 9.3944(11) _cell_length_b 10.6399(13) _cell_length_c 13.4756(15) _cell_measurement_reflns_used 2000 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.848 _cell_measurement_theta_min 1.932 _cell_volume 1277.0(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.961 _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 0.1231 _diffrn_reflns_av_unetI/netI 0.0997 _diffrn_reflns_Laue_measured_fraction_full 0.977 _diffrn_reflns_Laue_measured_fraction_max 0.961 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11718 _diffrn_reflns_point_group_measured_fraction_full 0.977 _diffrn_reflns_point_group_measured_fraction_max 0.961 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.848 _diffrn_reflns_theta_min 1.932 _exptl_absorpt_coefficient_mu 0.486 _exptl_absorpt_correction_T_max 0.9656 _exptl_absorpt_correction_T_min 0.7645 _exptl_absorpt_correction_type numerical _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description polyhedron _exptl_crystal_F_000 616 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.558 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.156 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 361 _refine_ls_number_reflns 5268 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.094 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0745 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2285 _refine_ls_wR_factor_ref 0.3039 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3233 _reflns_number_total 5268 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c8dt00848e2.cif _cod_data_source_block shelx_CCDC1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 7046036--7046038.cif. ; _cod_database_code 7046037 _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 9.3944 10.6399 13.4756 87.461 73.130 82.194 ZERR 2.00 0.0011 0.0013 0.0015 0.009 0.009 0.009 LATT 1 SFAC C H N O F V UNIT 48 30 6 6 18 2 MERG 2 FMAP 2 PLAN 25 ACTA BOND $H CONF L.S. 10 WGHT 0.200000 FVAR 0.65513 V001 6 0.491609 0.286901 0.266756 11.00000 0.04896 0.05070 = 0.04500 -0.00013 -0.00531 -0.00843 O1 4 0.330075 0.424303 0.305652 11.00000 0.05969 0.05664 = 0.04647 -0.00164 -0.00586 -0.00269 O2 4 0.654568 0.387158 0.248165 11.00000 0.05905 0.06485 = 0.05381 -0.00273 -0.01140 -0.01813 F1 5 0.226632 0.679739 0.317897 11.00000 0.10900 0.06960 = 0.08587 0.01574 -0.00523 0.00570 O3 4 0.635398 0.135158 0.227324 11.00000 0.05672 0.06239 = 0.06199 -0.00664 -0.01067 -0.00616 N3 3 0.328278 0.154283 0.283136 11.00000 0.05494 0.04965 = 0.05292 0.00482 -0.00830 -0.00994 F3 5 0.112651 0.660199 0.476246 11.00000 0.14301 0.09590 = 0.07786 -0.02412 0.00134 0.04069 N2 3 0.500573 0.321912 0.108215 11.00000 0.05047 0.04627 = 0.04895 0.00055 -0.00761 -0.00693 F2 5 0.050767 0.564552 0.364133 11.00000 0.07203 0.11305 = 0.19239 -0.02266 -0.05033 0.00415 C16 1 0.377015 0.317880 0.078343 11.00000 0.05617 0.05409 = 0.05583 0.00588 -0.01553 -0.01102 AFIX 43 H16 2 0.288777 0.304338 0.128632 11.00000 -1.20000 AFIX 0 C1 1 0.166939 0.596124 0.389988 11.00000 0.06061 0.06753 = 0.07025 -0.00749 0.00142 0.00334 C19 1 0.499693 0.013121 0.153761 11.00000 0.07189 0.05801 = 0.05835 -0.00501 -0.01120 -0.00751 AFIX 43 H19 2 0.507782 -0.041822 0.100049 11.00000 -1.20000 AFIX 0 N1 3 0.486024 0.261923 0.426799 11.00000 0.06454 0.05753 = 0.05117 0.00302 -0.01195 -0.01312 F7 5 0.774890 -0.084209 0.025910 11.00000 0.10904 0.16651 = 0.15013 -0.09579 0.01761 -0.00994 C12 1 0.628905 0.343720 0.036037 11.00000 0.05489 0.05412 = 0.04381 -0.00239 -0.00718 -0.00705 C5 1 0.413108 0.320305 0.605012 11.00000 0.11121 0.09170 = 0.04960 -0.00427 -0.01578 -0.01401 AFIX 43 H5 2 0.359767 0.377804 0.656858 11.00000 -1.20000 AFIX 0 C20 1 0.353066 0.052765 0.221857 11.00000 0.06799 0.05352 = 0.05179 0.00030 -0.01566 -0.01430 C13 1 0.632897 0.357058 -0.067990 11.00000 0.07519 0.06405 = 0.04499 -0.00450 -0.00769 -0.01483 AFIX 43 H13 2 0.722416 0.369119 -0.117499 11.00000 -1.20000 AFIX 0 F5 5 1.021667 0.403841 0.098549 11.00000 0.05555 0.26029 = 0.11122 -0.02413 -0.00495 -0.04181 F4 5 0.891027 0.542372 0.198183 11.00000 0.10918 0.12229 = 0.22009 -0.02618 -0.06113 -0.04837 C2 1 0.278244 0.483216 0.395142 11.00000 0.04907 0.05346 = 0.05641 -0.00197 0.00283 -0.00593 C4 1 0.406105 0.341391 0.504326 11.00000 0.07454 0.06542 = 0.04713 -0.00149 -0.00529 -0.01807 C15 1 0.374368 0.332853 -0.023448 11.00000 0.07668 0.06176 = 0.06325 0.00258 -0.02679 -0.01154 AFIX 43 H15 2 0.286683 0.329823 -0.041646 11.00000 -1.20000 AFIX 0 F6 5 0.935834 0.363510 0.258010 11.00000 0.10505 0.19298 = 0.15038 0.07072 -0.07578 -0.05368 C11 1 0.760905 0.361672 0.066203 11.00000 0.05025 0.06811 = 0.05601 0.00274 -0.00367 -0.01212 AFIX 43 H11 2 0.851556 0.356816 0.014116 11.00000 -1.20000 AFIX 0 C24 1 0.193245 0.180229 0.353068 11.00000 0.05944 0.06604 = 0.06931 -0.00218 -0.00210 -0.01393 AFIX 43 H24 2 0.177289 0.249213 0.396752 11.00000 -1.20000 AFIX 0 C10 1 0.763708 0.384648 0.162570 11.00000 0.04995 0.05806 = 0.05878 0.00240 -0.00764 -0.00739 C18 1 0.626427 0.051019 0.163238 11.00000 0.06893 0.05094 = 0.05280 -0.00252 -0.00294 -0.00374 C8 1 0.572646 0.160592 0.451546 11.00000 0.10104 0.08405 = 0.05897 0.00155 -0.03163 -0.00836 AFIX 43 H8 2 0.629293 0.105480 0.398799 11.00000 -1.20000 AFIX 0 C17 1 0.777267 -0.011466 0.100673 11.00000 0.07449 0.06763 = 0.09795 -0.01869 -0.00491 0.00598 F9 5 0.841763 -0.085642 0.155194 11.00000 0.15739 0.27759 = 0.15901 -0.02074 -0.03106 0.14382 C14 1 0.507506 0.352651 -0.097954 11.00000 0.08835 0.06582 = 0.04843 -0.00261 -0.01656 -0.01165 AFIX 43 H14 2 0.510512 0.362734 -0.167409 11.00000 -1.20000 AFIX 0 C7 1 0.581541 0.134618 0.550302 11.00000 0.12491 0.08141 = 0.07480 0.01193 -0.04216 -0.00985 AFIX 43 H7 2 0.642974 0.063738 0.563734 11.00000 -1.20000 AFIX 0 C21 1 0.236219 -0.018880 0.226502 11.00000 0.07956 0.07020 = 0.08974 -0.00676 -0.02320 -0.02298 AFIX 43 H21 2 0.252128 -0.086111 0.181108 11.00000 -1.20000 AFIX 0 C3 1 0.308928 0.451467 0.484088 11.00000 0.07992 0.07292 = 0.04904 -0.01215 -0.00183 -0.01536 AFIX 43 H3 2 0.262864 0.506015 0.539533 11.00000 -1.20000 AFIX 0 F8 5 0.867477 0.067741 0.059217 11.00000 0.10777 0.11186 = 0.31477 -0.08373 0.09946 -0.02830 C9 1 0.904079 0.419391 0.178626 11.00000 0.06277 0.09864 = 0.08230 0.00925 -0.01009 -0.02510 C6 1 0.499056 0.214200 0.628309 11.00000 0.13225 0.10821 = 0.05910 0.01154 -0.03930 -0.03004 AFIX 43 H6 2 0.500729 0.197170 0.696279 11.00000 -1.20000 AFIX 0 C23 1 0.078290 0.110010 0.363002 11.00000 0.06146 0.08171 = 0.10393 0.00103 0.00258 -0.02191 AFIX 43 H23 2 -0.012931 0.129642 0.413357 11.00000 -1.20000 AFIX 0 C22 1 0.100493 0.009529 0.296803 11.00000 0.07338 0.08316 = 0.10814 -0.00219 -0.02285 -0.03398 AFIX 43 H22 2 0.023229 -0.038201 0.300349 11.00000 -1.20000 AFIX 0 HKLF 4 REM SIR92 run in space group P -1 REM R1 = 0.0745 for 3233 Fo > 4sig(Fo) and 0.1066 for all 5268 data REM 361 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.558, deepest hole -0.744, 1-sigma level 0.156 Q1 1 0.2125 0.2162 0.4514 11.00000 0.05 0.56 Q2 1 0.6019 0.3845 0.3630 11.00000 0.05 0.55 Q3 1 0.7717 -0.1334 0.1159 11.00000 0.05 0.54 Q4 1 0.0999 0.1833 0.5000 11.00000 0.05 0.54 Q5 1 0.4400 0.0018 0.1836 11.00000 0.05 0.49 Q6 1 0.8947 -0.0179 0.1325 11.00000 0.05 0.48 Q7 1 0.5245 0.3990 0.5819 11.00000 0.05 0.47 Q8 1 0.0918 0.6200 0.2985 11.00000 0.05 0.47 Q9 1 0.2267 0.2799 0.3167 11.00000 0.05 0.46 Q10 1 0.1966 0.2748 0.3435 11.00000 0.05 0.46 Q11 1 0.6258 0.4758 0.2451 11.00000 0.05 0.46 Q12 1 0.7150 -0.0044 0.5795 11.00000 0.05 0.46 Q13 1 0.5217 0.2148 0.7169 11.00000 0.05 0.45 Q14 1 0.5855 0.4044 0.2126 11.00000 0.05 0.45 Q15 1 0.7955 0.0598 0.5787 11.00000 0.05 0.45 Q16 1 0.3886 0.3535 0.2856 11.00000 0.05 0.45 Q17 1 0.4697 0.0373 0.0350 11.00000 0.05 0.43 Q18 1 0.6689 0.4581 0.2069 11.00000 0.05 0.41 Q19 1 0.4157 0.0373 0.0821 11.00000 0.05 0.41 Q20 1 0.0262 0.1357 0.5030 11.00000 0.05 0.41 Q21 1 0.6252 0.2391 0.2733 11.00000 0.05 0.41 Q22 1 0.5513 0.4199 0.2587 11.00000 0.05 0.41 Q23 1 0.2633 0.3781 0.1346 11.00000 0.05 0.41 Q24 1 0.5909 0.3489 0.4625 11.00000 0.05 0.40 Q25 1 1.0289 0.2673 0.1607 11.00000 0.05 0.40 ; _shelx_res_checksum 86683 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 V001 V 0.49161(7) 0.28690(6) 0.26676(5) 0.0498(3) Uani 1 1 d . . O1 O 0.3301(3) 0.4243(3) 0.3057(2) 0.0567(7) Uani 1 1 d . . O2 O 0.6546(3) 0.3872(3) 0.2482(2) 0.0592(8) Uani 1 1 d . . F1 F 0.2266(4) 0.6797(3) 0.3179(3) 0.0952(11) Uani 1 1 d . . O3 O 0.6354(3) 0.1352(3) 0.2273(3) 0.0617(8) Uani 1 1 d . . N3 N 0.3283(4) 0.1543(3) 0.2831(3) 0.0539(8) Uani 1 1 d . . F3 F 0.1127(6) 0.6602(4) 0.4762(3) 0.1173(16) Uani 1 1 d . . N2 N 0.5006(4) 0.3219(3) 0.1082(3) 0.0499(8) Uani 1 1 d . . F2 F 0.0508(4) 0.5646(5) 0.3641(5) 0.1241(16) Uani 1 1 d . . C16 C 0.3770(5) 0.3179(4) 0.0783(3) 0.0553(9) Uani 1 1 d . . H16 H 0.2888 0.3043 0.1286 0.066 Uiso 1 1 calc R U C1 C 0.1669(6) 0.5961(5) 0.3900(4) 0.0713(13) Uani 1 1 d . . C19 C 0.4997(6) 0.0131(5) 0.1538(4) 0.0643(11) Uani 1 1 d . . H19 H 0.5078 -0.0418 0.1000 0.077 Uiso 1 1 calc R U N1 N 0.4860(4) 0.2619(4) 0.4268(3) 0.0583(9) Uani 1 1 d . . F7 F 0.7749(6) -0.0842(6) 0.0259(5) 0.151(2) Uani 1 1 d . . C12 C 0.6289(5) 0.3437(4) 0.0360(3) 0.0524(9) Uani 1 1 d . . C5 C 0.4131(8) 0.3203(7) 0.6050(4) 0.0855(17) Uani 1 1 d . . H5 H 0.3598 0.3778 0.6569 0.103 Uiso 1 1 calc R U C20 C 0.3531(5) 0.0528(4) 0.2219(3) 0.0575(10) Uani 1 1 d . . C13 C 0.6329(6) 0.3571(5) -0.0680(3) 0.0627(11) Uani 1 1 d . . H13 H 0.7224 0.3691 -0.1175 0.075 Uiso 1 1 calc R U F5 F 1.0217(4) 0.4038(7) 0.0985(4) 0.144(2) Uani 1 1 d . . F4 F 0.8910(6) 0.5424(5) 0.1982(6) 0.144(2) Uani 1 1 d . . C2 C 0.2782(5) 0.4832(4) 0.3951(4) 0.0568(10) Uani 1 1 d . . C4 C 0.4061(6) 0.3414(5) 0.5043(3) 0.0640(12) Uani 1 1 d . . C15 C 0.3744(6) 0.3329(5) -0.0234(4) 0.0656(11) Uani 1 1 d . . H15 H 0.2867 0.3298 -0.0416 0.079 Uiso 1 1 calc R U F6 F 0.9358(5) 0.3635(6) 0.2580(4) 0.140(2) Uani 1 1 d . . C11 C 0.7609(5) 0.3617(5) 0.0662(3) 0.0602(11) Uani 1 1 d . . H11 H 0.8516 0.3568 0.0141 0.072 Uiso 1 1 calc R U C24 C 0.1932(5) 0.1802(5) 0.3531(4) 0.0678(12) Uani 1 1 d . . H24 H 0.1773 0.2492 0.3968 0.081 Uiso 1 1 calc R U C10 C 0.7637(5) 0.3846(4) 0.1626(4) 0.0573(10) Uani 1 1 d . . C18 C 0.6264(5) 0.0510(4) 0.1632(4) 0.0610(11) Uani 1 1 d . . C8 C 0.5726(7) 0.1606(6) 0.4515(4) 0.0799(15) Uani 1 1 d . . H8 H 0.6293 0.1055 0.3988 0.096 Uiso 1 1 calc R U C17 C 0.7773(7) -0.0115(6) 0.1007(5) 0.0851(17) Uani 1 1 d . . F9 F 0.8418(8) -0.0856(9) 0.1552(6) 0.217(4) Uani 1 1 d . . C14 C 0.5075(6) 0.3527(5) -0.0980(4) 0.0679(12) Uani 1 1 d . . H14 H 0.5105 0.3627 -0.1674 0.082 Uiso 1 1 calc R U C7 C 0.5815(9) 0.1346(7) 0.5503(5) 0.0915(18) Uani 1 1 d . . H7 H 0.6430 0.0637 0.5637 0.110 Uiso 1 1 calc R U C21 C 0.2362(7) -0.0189(6) 0.2265(5) 0.0786(15) Uani 1 1 d . . H21 H 0.2521 -0.0861 0.1811 0.094 Uiso 1 1 calc R U C3 C 0.3089(6) 0.4515(5) 0.4841(4) 0.0699(13) Uani 1 1 d . . H3 H 0.2629 0.5060 0.5395 0.084 Uiso 1 1 calc R U F8 F 0.8675(6) 0.0677(5) 0.0592(7) 0.208(4) Uani 1 1 d . . C9 C 0.9041(6) 0.4194(7) 0.1786(5) 0.0824(16) Uani 1 1 d . . C6 C 0.4991(9) 0.2142(8) 0.6283(5) 0.096(2) Uani 1 1 d . . H6 H 0.5007 0.1972 0.6963 0.116 Uiso 1 1 calc R U C23 C 0.0783(6) 0.1100(6) 0.3630(6) 0.0868(18) Uani 1 1 d . . H23 H -0.0129 0.1296 0.4134 0.104 Uiso 1 1 calc R U C22 C 0.1005(7) 0.0095(6) 0.2968(6) 0.0866(17) Uani 1 1 d . . H22 H 0.0232 -0.0382 0.3003 0.104 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 V001 0.0490(4) 0.0507(5) 0.0450(4) -0.0001(3) -0.0053(3) -0.0084(3) O1 0.0597(16) 0.0566(17) 0.0465(15) -0.0016(13) -0.0059(12) -0.0027(13) O2 0.0590(16) 0.0648(19) 0.0538(16) -0.0027(14) -0.0114(13) -0.0181(14) F1 0.109(3) 0.070(2) 0.086(2) 0.0157(17) -0.0052(19) 0.0057(17) O3 0.0567(16) 0.0624(19) 0.0620(18) -0.0066(15) -0.0107(13) -0.0062(13) N3 0.0549(18) 0.0496(19) 0.0529(18) 0.0048(15) -0.0083(14) -0.0099(14) F3 0.143(4) 0.096(3) 0.078(2) -0.024(2) 0.001(2) 0.041(3) N2 0.0505(17) 0.0463(18) 0.0490(17) 0.0006(14) -0.0076(13) -0.0069(13) F2 0.072(2) 0.113(3) 0.192(5) -0.023(3) -0.050(3) 0.004(2) C16 0.056(2) 0.054(2) 0.056(2) 0.0059(18) -0.0155(17) -0.0110(17) C1 0.061(3) 0.068(3) 0.070(3) -0.007(2) 0.001(2) 0.003(2) C19 0.072(3) 0.058(3) 0.058(2) -0.005(2) -0.011(2) -0.008(2) N1 0.065(2) 0.058(2) 0.0512(19) 0.0030(16) -0.0120(15) -0.0131(16) F7 0.109(3) 0.167(5) 0.150(4) -0.096(4) 0.018(3) -0.010(3) C12 0.055(2) 0.054(2) 0.0438(19) -0.0024(16) -0.0072(15) -0.0071(16) C5 0.111(4) 0.092(4) 0.050(3) -0.004(3) -0.016(3) -0.014(3) C20 0.068(2) 0.054(2) 0.052(2) 0.0003(18) -0.0157(18) -0.0143(18) C13 0.075(3) 0.064(3) 0.045(2) -0.0045(19) -0.0077(19) -0.015(2) F5 0.0555(19) 0.260(7) 0.111(3) -0.024(4) -0.0049(19) -0.042(3) F4 0.109(3) 0.122(4) 0.220(6) -0.026(4) -0.061(4) -0.048(3) C2 0.049(2) 0.053(2) 0.056(2) -0.0020(18) 0.0028(16) -0.0059(16) C4 0.075(3) 0.065(3) 0.047(2) -0.001(2) -0.0053(19) -0.018(2) C15 0.077(3) 0.062(3) 0.063(3) 0.003(2) -0.027(2) -0.012(2) F6 0.105(3) 0.193(5) 0.150(4) 0.071(4) -0.076(3) -0.054(3) C11 0.050(2) 0.068(3) 0.056(2) 0.003(2) -0.0037(17) -0.0121(18) C24 0.059(2) 0.066(3) 0.069(3) -0.002(2) -0.002(2) -0.014(2) C10 0.050(2) 0.058(2) 0.059(2) 0.0024(19) -0.0076(17) -0.0074(17) C18 0.069(3) 0.051(2) 0.053(2) -0.0025(19) -0.0029(19) -0.0037(18) C8 0.101(4) 0.084(4) 0.059(3) 0.002(3) -0.032(3) -0.008(3) C17 0.074(3) 0.068(3) 0.098(4) -0.019(3) -0.005(3) 0.006(3) F9 0.157(6) 0.278(9) 0.159(6) -0.021(6) -0.031(4) 0.144(6) C14 0.088(3) 0.066(3) 0.048(2) -0.003(2) -0.017(2) -0.012(2) C7 0.125(5) 0.081(4) 0.075(4) 0.012(3) -0.042(3) -0.010(4) C21 0.080(3) 0.070(3) 0.090(4) -0.007(3) -0.023(3) -0.023(3) C3 0.080(3) 0.073(3) 0.049(2) -0.012(2) -0.002(2) -0.015(2) F8 0.108(3) 0.112(4) 0.315(9) -0.084(5) 0.099(5) -0.028(3) C9 0.063(3) 0.099(4) 0.082(4) 0.009(3) -0.010(3) -0.025(3) C6 0.132(6) 0.108(5) 0.059(3) 0.012(3) -0.039(3) -0.030(4) C23 0.061(3) 0.082(4) 0.104(4) 0.001(3) 0.003(3) -0.022(3) C22 0.073(3) 0.083(4) 0.108(5) -0.002(3) -0.023(3) -0.034(3) 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' 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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1 V001 O2 97.07(14) O1 V001 O3 172.83(13) O2 V001 O3 90.04(14) O1 V001 N2 89.15(13) O2 V001 N2 88.74(13) O3 V001 N2 90.12(14) O1 V001 N1 89.42(15) O2 V001 N1 88.62(14) O3 V001 N1 91.64(15) N2 V001 N1 176.83(13) O1 V001 N3 89.75(14) O2 V001 N3 173.18(14) O3 V001 N3 83.14(14) N2 V001 N3 91.56(13) N1 V001 N3 91.27(14) C2 O1 V001 127.7(3) C10 O2 V001 122.0(3) C18 O3 V001 123.7(3) C20 N3 C24 118.6(4) C20 N3 V001 122.9(3) C24 N3 V001 118.4(3) C16 N2 C12 118.9(4) C16 N2 V001 119.2(3) C12 N2 V001 121.8(3) N2 C16 C15 123.2(4) N2 C16 H16 118.4 C15 C16 H16 118.4 F3 C1 F2 106.8(5) F3 C1 F1 105.5(5) F2 C1 F1 105.6(5) F3 C1 C2 114.5(5) F2 C1 C2 112.0(5) F1 C1 C2 111.8(4) C18 C19 C20 123.7(5) C18 C19 H19 118.1 C20 C19 H19 118.1 C4 N1 C8 117.2(5) C4 N1 V001 125.2(4) C8 N1 V001 117.5(4) N2 C12 C13 120.1(4) N2 C12 C11 120.7(4) C13 C12 C11 119.0(4) C6 C5 C4 119.9(6) C6 C5 H5 120.0 C4 C5 H5 120.0 N3 C20 C21 120.1(4) N3 C20 C19 120.8(4) C21 C20 C19 119.1(5) C14 C13 C12 120.7(4) C14 C13 H13 119.6 C12 C13 H13 119.6 O1 C2 C3 128.4(4) O1 C2 C1 111.4(4) C3 C2 C1 120.2(5) N1 C4 C5 121.4(5) N1 C4 C3 120.5(4) C5 C4 C3 118.1(5) C16 C15 C14 117.7(5) C16 C15 H15 121.1 C14 C15 H15 121.1 C10 C11 C12 125.7(4) C10 C11 H11 117.1 C12 C11 H11 117.1 N3 C24 C23 123.1(5) N3 C24 H24 118.4 C23 C24 H24 118.4 O2 C10 C11 128.3(4) O2 C10 C9 112.5(4) C11 C10 C9 119.1(4) O3 C18 C19 126.6(4) O3 C18 C17 113.0(5) C19 C18 C17 120.3(5) N1 C8 C7 123.5(6) N1 C8 H8 118.3 C7 C8 H8 118.3 F9 C17 F8 106.4(8) F9 C17 F7 103.1(7) F8 C17 F7 106.2(7) F9 C17 C18 112.2(6) F8 C17 C18 112.9(5) F7 C17 C18 115.2(6) C13 C14 C15 119.2(5) C13 C14 H14 120.4 C15 C14 H14 120.4 C6 C7 C8 118.9(6) C6 C7 H7 120.5 C8 C7 H7 120.5 C22 C21 C20 120.3(6) C22 C21 H21 119.9 C20 C21 H21 119.9 C2 C3 C4 127.4(5) C2 C3 H3 116.3 C4 C3 H3 116.3 F6 C9 F5 109.2(6) F6 C9 F4 104.5(7) F5 C9 F4 102.7(6) F6 C9 C10 113.0(5) F5 C9 C10 115.2(6) F4 C9 C10 111.2(5) C7 C6 C5 118.9(6) C7 C6 H6 120.5 C5 C6 H6 120.5 C24 C23 C22 118.6(5) C24 C23 H23 120.7 C22 C23 H23 120.7 C21 C22 C23 119.2(5) C21 C22 H22 120.4 C23 C22 H22 120.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance V001 O1 1.928(3) V001 O2 1.934(3) V001 O3 1.944(3) V001 N2 2.132(4) V001 N1 2.148(4) V001 N3 2.181(4) O1 C2 1.314(5) O2 C10 1.300(5) F1 C1 1.339(6) O3 C18 1.298(6) N3 C20 1.342(6) N3 C24 1.344(6) F3 C1 1.307(6) N2 C16 1.341(6) N2 C12 1.352(5) F2 C1 1.325(7) C16 C15 1.381(7) C16 H16 0.9300 C1 C2 1.495(7) C19 C18 1.349(7) C19 C20 1.435(7) C19 H19 0.9300 N1 C4 1.349(6) N1 C8 1.350(7) F7 C17 1.304(8) C12 C13 1.393(6) C12 C11 1.450(6) C5 C6 1.376(10) C5 C4 1.384(8) C5 H5 0.9300 C20 C21 1.405(7) C13 C14 1.359(8) C13 H13 0.9300 F5 C9 1.299(7) F4 C9 1.328(9) C2 C3 1.331(7) C4 C3 1.451(8) C15 C14 1.393(7) C15 H15 0.9300 F6 C9 1.291(8) C11 C10 1.340(7) C11 H11 0.9300 C24 C23 1.367(7) C24 H24 0.9300 C10 C9 1.492(7) C18 C17 1.504(7) C8 C7 1.371(8) C8 H8 0.9300 C17 F9 1.268(9) C17 F8 1.272(8) C14 H14 0.9300 C7 C6 1.360(11) C7 H7 0.9300 C21 C22 1.354(9) C21 H21 0.9300 C3 H3 0.9300 C6 H6 0.9300 C23 C22 1.378(10) C23 H23 0.9300 C22 H22 0.9300 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 C12 N2 C16 C15 1.1(7) V001 N2 C16 C15 -176.6(4) C16 N2 C12 C13 -2.3(6) V001 N2 C12 C13 175.3(3) C16 N2 C12 C11 173.7(4) V001 N2 C12 C11 -8.7(5) C24 N3 C20 C21 4.4(7) V001 N3 C20 C21 -171.1(4) C24 N3 C20 C19 -173.3(5) V001 N3 C20 C19 11.2(6) C18 C19 C20 N3 16.9(8) C18 C19 C20 C21 -160.8(5) N2 C12 C13 C14 2.2(7) C11 C12 C13 C14 -173.9(5) V001 O1 C2 C3 -10.6(7) V001 O1 C2 C1 172.0(3) F3 C1 C2 O1 -179.0(4) F2 C1 C2 O1 59.3(6) F1 C1 C2 O1 -59.1(6) F3 C1 C2 C3 3.4(7) F2 C1 C2 C3 -118.3(6) F1 C1 C2 C3 123.3(5) C8 N1 C4 C5 0.3(8) V001 N1 C4 C5 -177.7(4) C8 N1 C4 C3 -179.2(5) V001 N1 C4 C3 2.8(6) C6 C5 C4 N1 -2.2(9) C6 C5 C4 C3 177.3(6) N2 C16 C15 C14 0.2(7) N2 C12 C11 C10 -14.4(7) C13 C12 C11 C10 161.6(5) C20 N3 C24 C23 -1.8(8) V001 N3 C24 C23 173.8(5) V001 O2 C10 C11 28.7(7) V001 O2 C10 C9 -154.8(4) C12 C11 C10 O2 5.0(8) C12 C11 C10 C9 -171.2(5) V001 O3 C18 C19 -36.0(6) V001 O3 C18 C17 147.9(4) C20 C19 C18 O3 -6.3(8) C20 C19 C18 C17 169.6(5) C4 N1 C8 C7 0.7(9) V001 N1 C8 C7 178.9(5) O3 C18 C17 F9 71.1(8) C19 C18 C17 F9 -105.4(8) O3 C18 C17 F8 -49.1(9) C19 C18 C17 F8 134.5(8) O3 C18 C17 F7 -171.3(6) C19 C18 C17 F7 12.2(9) C12 C13 C14 C15 -0.9(8) C16 C15 C14 C13 -0.3(7) N1 C8 C7 C6 0.2(11) N3 C20 C21 C22 -3.8(9) C19 C20 C21 C22 173.9(6) O1 C2 C3 C4 -1.3(8) C1 C2 C3 C4 175.9(5) N1 C4 C3 C2 4.8(8) C5 C4 C3 C2 -174.7(5) O2 C10 C9 F6 45.6(8) C11 C10 C9 F6 -137.6(6) O2 C10 C9 F5 172.1(6) C11 C10 C9 F5 -11.1(9) O2 C10 C9 F4 -71.6(7) C11 C10 C9 F4 105.2(6) C8 C7 C6 C5 -2.0(11) C4 C5 C6 C7 3.0(11) N3 C24 C23 C22 -1.5(10) C20 C21 C22 C23 0.5(11) C24 C23 C22 C21 2.0(11)