#------------------------------------------------------------------------------ #$Date: 2024-12-03 04:54:58 +0200 (Tue, 03 Dec 2024) $ #$Revision: 296194 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/31/27/2312700.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2312700 loop_ _publ_author_name 'Kanagavel, Manimurugan' 'Balasubramanian, Sridhar' 'Nechipadappu, Sunil Kumar' _publ_section_title ; Variable stoichiometry and a salt-cocrystal intermediate in multicomponent systems of flucytosine: structural elucidation and their impact on stability. ; _journal_coeditor_code YH5039 _journal_issue 6 _journal_name_full 'Acta crystallographica Section B, Structural science, crystal engineering and materials' _journal_paper_doi 10.1107/S2052520624010278 _journal_volume 80 _journal_year 2024 _chemical_formula_moiety 'C9 H8 O4, C4 H4 F N3 O' _chemical_formula_sum 'C13 H12 F N3 O5' _chemical_formula_weight 309.26 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2019/3 _cell_angle_alpha 81.8901(9) _cell_angle_beta 81.0672(9) _cell_angle_gamma 86.6887(9) _cell_formula_units_Z 2 _cell_length_a 6.5047(2) _cell_length_b 7.1710(2) _cell_length_c 13.9389(4) _cell_measurement_reflns_used 6023 _cell_measurement_temperature 294(2) _cell_measurement_theta_max 30.48 _cell_measurement_theta_min 2.37 _cell_volume 635.45(3) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL2014 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _diffrn_ambient_temperature 294(2) _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON-III' _diffrn_measurement_method '\w and \f' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_unetI/netI 0.0309 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 10092 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.247 _diffrn_reflns_theta_min 2.871 _exptl_absorpt_coefficient_mu 0.135 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6460 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_crystal_density_diffrn 1.616 _exptl_crystal_description block _exptl_crystal_F_000 320 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.140 _refine_diff_density_max 0.246 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.041 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 228 _refine_ls_number_reflns 2520 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0423 _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^)+(0.0601P)^2^+0.2350P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1151 _refine_ls_wR_factor_ref 0.1233 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2031 _reflns_number_total 2520 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file yh5039sup1.cif _cod_data_source_block FCY-CAF _cod_database_code 2312700 _shelx_shelxl_version_number 2019/3 _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 0.976 _shelx_estimated_absorpt_t_max 0.981 _shelx_res_file ; TITL FCY-CAF_a.res in P-1 FCY-CAF.res created by SHELXL-2018/3 at 14:28:06 on 14-Aug-2024 CELL 0.71073 6.5047 7.1710 13.9389 81.8901 81.0672 86.6887 ZERR 2.00 0.0002 0.0002 0.0004 0.0009 0.0009 0.0009 LATT 1 SFAC C H N O F UNIT 26 24 6 10 2 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP 21 OMIT -3 52.5 OMIT 0 2 1 OMIT 0 0 1 OMIT 0 6 6 OMIT 3 6 0 OMIT 3 6 6 OMIT 0 -2 2 DFIX 1.43 0.02 C10 O4D L.S. 10 ACTA FMAP 2 PLAN 5 SIZE 0.18 0.16 0.14 EQIV $1 -x+1, -y+2, -z EQIV $2 -x, -y+2, -z+1 EQIV $3 -x+2, -y+1, -z+1 EQIV $4 -x+2, -y+1, -z+2 HTAB N1 O1_$1 HTAB N3 O2_$2 HTAB O5 O1_$3 HTAB O4 O5_$4 HTAB O3 N2 HTAB N3 O2 HTAB BOND $H CONF WGHT 0.060100 0.235000 FVAR 1.85368 0.90912 MOLE 1 C1 1 0.384476 0.959015 0.150330 11.00000 0.02691 0.03304 = 0.02523 -0.00243 -0.00372 0.00390 C2 1 0.108957 1.004694 0.276266 11.00000 0.02633 0.02694 = 0.02644 -0.00332 -0.00314 -0.00057 C3 1 -0.016302 1.085047 0.204548 11.00000 0.02198 0.03374 = 0.03083 -0.00462 -0.00385 0.00471 C4 1 0.061269 1.101604 0.109770 11.00000 0.03035 0.04156 = 0.02865 -0.00203 -0.00957 0.00832 AFIX 43 H4 2 -0.019152 1.155187 0.062653 11.00000 -1.20000 AFIX 0 F1 5 -0.211619 1.145894 0.235990 11.00000 0.02686 0.06141 = 0.03923 -0.00927 -0.00328 0.01363 N1 3 0.260670 1.038613 0.083030 11.00000 0.03152 0.04914 = 0.02066 -0.00077 -0.00194 0.00931 H1N 2 0.320214 1.047281 0.019215 11.00000 0.05503 N2 3 0.305495 0.944520 0.247190 11.00000 0.02592 0.03274 = 0.02181 -0.00173 -0.00379 0.00420 N3 3 0.034133 0.989834 0.370433 11.00000 0.02877 0.05140 = 0.02494 -0.00278 -0.00044 0.00788 H3N 2 0.123667 0.935830 0.417793 11.00000 0.04365 H4N 2 -0.094984 1.031025 0.389032 11.00000 0.05097 O1 4 0.565327 0.903175 0.120458 11.00000 0.02793 0.05508 = 0.02780 -0.00253 -0.00045 0.01203 MOLE 2 C5 1 0.480315 0.779974 0.471450 11.00000 0.03124 0.03481 = 0.02566 -0.00260 -0.00279 0.00460 C6 1 0.632010 0.695229 0.534013 11.00000 0.02989 0.04367 = 0.03020 -0.00184 -0.00391 0.00879 AFIX 43 H6 2 0.767569 0.670267 0.504957 11.00000 -1.20000 AFIX 0 C7 1 0.583836 0.652927 0.629977 11.00000 0.02930 0.03454 = 0.02979 -0.00280 -0.00491 0.00600 AFIX 43 H7 2 0.447168 0.680710 0.656497 11.00000 -1.20000 AFIX 0 C8 1 0.720999 0.567257 0.699439 11.00000 0.03158 0.02947 = 0.02743 -0.00170 -0.00597 0.00213 C9 1 0.926417 0.509552 0.668909 11.00000 0.03582 0.04209 = 0.02564 -0.00123 -0.00068 0.00901 AFIX 43 H9 2 0.978807 0.523927 0.602412 11.00000 -1.20000 AFIX 0 C10 1 1.052963 0.431394 0.736089 11.00000 0.02994 0.04016 = 0.03673 -0.00246 -0.00335 0.00772 PART 1 AFIX 43 H10 2 1.189134 0.392725 0.714413 21.00000 -1.20000 AFIX 0 PART 0 C11 1 0.978944 0.410230 0.835120 11.00000 0.03399 0.03173 = 0.03285 -0.00176 -0.01195 0.00240 C12 1 0.774122 0.467794 0.867632 11.00000 0.03527 0.04047 = 0.02475 -0.00227 -0.00414 0.00065 PART 2 AFIX 43 H12 2 0.723249 0.454551 0.934283 -21.00000 -1.20000 AFIX 0 PART 0 C13 1 0.647776 0.544518 0.800026 11.00000 0.02689 0.03865 = 0.02892 -0.00519 -0.00265 0.00385 AFIX 43 H13 2 0.511199 0.581826 0.821843 11.00000 -1.20000 AFIX 0 O2 4 0.299706 0.821555 0.503116 11.00000 0.03346 0.06795 = 0.02714 -0.00022 -0.00221 0.01644 O3 4 0.556868 0.808477 0.377879 11.00000 0.03593 0.06510 = 0.02331 0.00200 -0.00238 0.01355 H3O 2 0.452405 0.854409 0.335052 11.00000 0.06792 PART 1 O4 4 0.705277 0.443033 0.966110 21.00000 0.03916 0.10178 = 0.02305 -0.00513 -0.00498 0.00286 AFIX 147 H4O 2 0.787962 0.487726 0.994638 21.00000 -1.50000 AFIX 0 PART 2 O4D 4 1.246010 0.384209 0.733033 -21.00000 0.02204 0.07810 = 0.04692 -0.01452 -0.01081 0.02433 AFIX 147 H4DO 2 1.258390 0.273133 0.756053 -21.00000 -1.50000 AFIX 0 PART 0 O5 4 1.098944 0.337001 0.904619 11.00000 0.04076 0.06119 = 0.03482 -0.00102 -0.01402 0.01539 AFIX 147 H5O 2 1.205757 0.287634 0.878221 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM KB780_0m_a.res in P-1 REM wR2 = 0.1233, GooF = S = 1.047, Restrained GooF = 1.058 for all data REM R1 = 0.0423 for 2031 Fo > 4sig(Fo) and 0.0529 for all 2520 data REM 228 parameters refined using 1 restraints END WGHT 0.0601 0.2352 REM Instructions for potential hydrogen bonds EQIV $5 x-1, y+1, z-1 HTAB C4 O5_$5 HTAB N1 O1_$1 HTAB N3 O2 HTAB N3 O2_$2 HTAB C10 O3_$3 HTAB O3 N2 HTAB O4 O5_$4 HTAB O4D O1_$3 HTAB O5 O1_$3 REM Highest difference peak 0.246, deepest hole -0.199, 1-sigma level 0.041 Q1 1 0.5559 0.4856 0.9872 11.00000 0.05 0.25 Q2 1 0.0407 1.0301 0.2394 11.00000 0.05 0.23 Q3 1 0.0606 1.0861 0.2408 11.00000 0.05 0.23 Q4 1 0.3906 0.9301 0.2840 11.00000 0.05 0.22 Q5 1 0.0478 1.1720 0.1624 11.00000 0.05 0.22 ; _shelx_res_checksum 71730 _shelx_hkl_file ; -1 0 0 123.86 5.97 -1 0 0 114.61 5.90 -1 0 0 118.54 5.74 1 0 0 118.15 5.54 1 0 0 113.04 5.88 1 0 0 121.59 5.96 1 0 0 127.56 5.78 -2 0 0 357.83 15.75 -2 0 0 341.30 16.21 -2 0 0 381.23 16.20 -2 0 0 350.55 16.44 2 0 0 356.91 16.39 2 0 0 357.41 15.69 2 0 0 353.61 16.16 2 0 0 348.06 16.24 -3 0 0 3505.41 147.33 -3 0 0 3517.55 146.91 3 0 0 3613.72 147.13 3 0 0 3436.64 146.09 3 0 0 3601.06 146.98 -4 0 0 907.06 38.68 -4 0 0 829.84 38.69 -4 0 0 836.54 37.71 -4 0 0 833.33 39.33 4 0 0 833.20 38.54 4 0 0 899.99 39.14 4 0 0 828.29 37.64 4 0 0 960.65 39.00 -5 0 0 20.84 3.59 -5 0 0 27.32 4.36 5 0 0 29.28 4.82 5 0 0 28.65 5.36 5 0 0 27.83 4.62 -6 0 0 263.08 16.03 -6 0 0 274.85 15.23 6 0 0 267.33 15.73 6 0 0 264.46 16.99 -7 0 0 9.98 4.53 -7 0 0 -0.90 3.16 7 0 0 4.15 4.43 7 0 0 3.71 5.42 -8 0 0 34.13 6.69 8 0 0 13.46 5.76 8 0 0 21.56 7.99 9 0 0 0.45 6.14 9 0 0 -4.68 7.27 9 -1 0 7.15 6.19 9 -1 0 0.44 7.38 -9 1 0 0.14 5.53 8 -1 0 1.76 5.88 8 -1 0 -4.74 3.96 -8 1 0 0.99 4.74 7 -1 0 -3.44 3.68 7 -1 0 -6.55 4.72 -7 1 0 -1.15 3.18 -7 1 0 -1.49 3.84 6 -1 0 0.32 3.40 6 -1 0 8.10 5.12 -6 1 0 1.11 2.87 -6 1 0 5.49 3.90 5 -1 0 193.46 13.37 5 -1 0 245.23 12.72 -5 1 0 214.65 13.65 -5 1 0 200.71 12.00 4 -1 0 3.69 1.84 4 -1 0 3.76 2.35 4 -1 0 7.58 3.31 4 -1 0 8.76 2.08 -4 1 0 5.15 3.07 -4 1 0 7.61 2.88 -4 1 0 3.36 1.97 -4 1 0 3.02 2.37 3 -1 0 3654.06 150.78 -3 1 0 3573.59 150.53 -3 1 0 3636.48 150.63 2 -1 0 59.70 3.84 2 -1 0 66.17 4.71 2 -1 0 63.85 4.77 2 -1 0 68.12 4.07 -2 1 0 69.57 4.64 -2 1 0 64.73 4.85 -2 1 0 60.16 4.04 -2 1 0 59.08 4.25 1 -1 0 64.73 4.47 1 -1 0 72.75 4.54 1 -1 0 76.05 3.77 -1 1 0 65.58 4.45 -1 1 0 73.80 3.83 0 -1 0 1195.06 50.04 0 1 0 1229.69 50.04 -1 -1 0 342.12 14.86 -1 -1 0 351.33 15.89 -1 -1 0 354.71 15.12 -1 -1 0 360.47 14.74 1 1 0 333.95 14.76 1 1 0 359.20 15.44 1 1 0 354.71 14.87 -2 -1 0 802.84 36.56 -2 -1 0 849.78 35.28 -2 -1 0 818.46 35.88 2 1 0 860.42 35.37 2 1 0 849.56 35.45 2 1 0 836.13 36.63 2 1 0 869.32 36.05 -3 -1 0 4582.66 192.36 -3 -1 0 4490.03 191.41 3 1 0 4705.28 191.66 3 1 0 4737.59 192.25 -4 -1 0 259.99 14.93 -4 -1 0 246.55 13.84 -4 -1 0 269.59 13.26 -4 -1 0 264.09 13.26 4 1 0 288.21 14.69 4 1 0 263.19 14.67 4 1 0 256.06 13.31 4 1 0 266.20 13.06 -5 -1 0 1.97 2.70 -5 -1 0 1.58 1.87 5 1 0 -2.08 3.28 5 1 0 -0.58 3.02 5 1 0 0.54 1.41 5 1 0 2.79 1.83 -6 -1 0 3.34 3.40 -6 -1 0 0.26 2.41 6 1 0 -1.08 3.67 6 1 0 0.78 3.83 -7 -1 0 282.30 15.86 7 1 0 257.94 16.94 7 1 0 250.75 17.45 8 1 0 1.15 5.58 8 1 0 3.72 6.26 9 1 0 5.69 7.60 9 1 0 3.92 6.17 8 -2 0 8.19 7.31 8 -2 0 8.35 4.87 -8 2 0 4.32 5.73 -8 2 0 -2.65 4.54 7 -2 0 10.53 4.17 7 -2 0 5.18 5.59 -7 2 0 15.16 5.06 -7 2 0 5.62 3.99 6 -2 0 267.80 15.42 6 -2 0 280.71 17.96 -6 2 0 287.07 16.03 -6 2 0 297.06 18.15 5 -2 0 74.79 6.60 5 -2 0 77.26 8.13 -5 2 0 91.24 7.14 -5 2 0 77.05 8.79 4 -2 0 35.95 5.26 4 -2 0 21.96 4.98 4 -2 0 38.53 3.87 -4 2 0 30.62 4.60 -4 2 0 32.00 3.84 -4 2 0 22.03 3.86 -4 2 0 28.92 3.89 -4 2 0 32.21 4.83 3 -2 0 3805.21 150.53 3 -2 0 3346.13 151.08 -3 2 0 3494.84 149.29 -3 2 0 3636.56 150.27 -3 2 0 3765.39 149.98 2 -2 0 362.72 16.70 2 -2 0 334.65 15.69 2 -2 0 346.47 17.44 2 -2 0 356.03 15.70 -2 2 0 344.29 16.09 -2 2 0 348.75 16.49 -2 2 0 341.55 17.46 -2 2 0 387.17 16.04 -2 2 0 362.61 15.90 1 -2 0 50.44 4.14 1 -2 0 53.75 3.02 1 -2 0 53.27 3.65 -1 2 0 55.43 4.48 -1 2 0 51.72 3.06 -1 2 0 50.43 3.58 -1 2 0 55.75 3.63 -1 2 0 52.68 3.12 -2 -2 0 104.54 5.64 -2 -2 0 101.94 6.76 -2 -2 0 96.42 5.21 -2 -2 0 102.54 5.84 2 2 0 103.43 5.89 2 2 0 97.54 5.15 2 2 0 93.24 5.45 2 2 0 102.93 7.10 2 2 0 104.05 5.00 -3 -2 0 1478.75 64.44 -3 -2 0 1430.86 65.72 -3 -2 0 1531.07 63.85 -3 -2 0 1592.40 63.09 3 2 0 1526.79 63.56 3 2 0 1518.51 64.68 3 2 0 1576.22 63.89 3 2 0 1536.64 66.06 -4 -2 0 557.44 24.77 -4 -2 0 559.49 25.27 4 2 0 538.56 24.99 4 2 0 587.95 27.90 4 2 0 591.78 26.61 4 2 0 558.01 25.18 -5 -2 0 206.40 11.90 -5 -2 0 222.94 11.66 5 2 0 224.87 13.73 5 2 0 240.31 14.66 5 2 0 214.61 11.76 -6 -2 0 0.86 3.05 6 2 0 -5.03 4.02 6 2 0 5.87 4.91 7 2 0 0.14 4.80 7 2 0 2.77 5.36 8 2 0 -7.62 5.86 8 2 0 -2.64 5.84 9 2 0 1.58 7.23 9 2 0 6.69 7.47 8 -3 0 133.52 10.80 -8 3 0 136.57 13.03 -8 3 0 126.80 15.33 7 -3 0 16.41 6.65 7 -3 0 18.60 4.41 -7 3 0 9.84 4.78 -7 3 0 15.46 5.55 6 -3 0 176.00 13.44 6 -3 0 159.28 10.30 -6 3 0 160.58 11.44 -6 3 0 162.48 13.87 5 -3 0 141.08 10.88 5 -3 0 135.27 8.72 -5 3 0 143.10 9.73 -5 3 0 139.57 12.18 4 -3 0 660.57 30.36 4 -3 0 645.55 28.41 -4 3 0 593.54 29.74 -4 3 0 594.08 29.40 -4 3 0 672.51 31.83 -4 3 0 658.07 28.93 3 -3 0 753.43 32.13 3 -3 0 696.34 34.55 3 -3 0 767.08 33.55 3 -3 0 683.75 32.13 -3 3 0 779.39 32.49 -3 3 0 742.39 32.70 -3 3 0 779.74 35.27 -3 3 0 737.34 33.28 2 -3 0 409.95 18.95 2 -3 0 443.12 21.41 -2 3 0 414.65 19.17 -2 3 0 401.96 19.59 -2 3 0 441.28 19.87 -2 3 0 451.59 21.68 -2 3 0 464.15 19.22 1 -3 0 396.33 17.61 1 -3 0 422.23 18.51 1 -3 0 398.17 18.09 -1 3 0 400.36 17.96 -1 3 0 421.49 17.73 -1 3 0 428.57 18.19 -1 3 0 393.83 18.54 -1 3 0 438.73 20.16 -1 3 0 411.12 18.46 0 -3 0 135.77 7.24 0 -3 0 132.58 7.12 0 -3 0 140.45 5.78 0 -3 0 121.56 5.67 0 -3 0 136.86 7.16 0 3 0 142.11 7.93 0 3 0 127.22 6.91 0 3 0 135.12 5.93 0 3 0 129.46 7.06 0 3 0 129.37 6.99 0 3 0 140.37 5.77 -1 -3 0 527.78 23.28 -1 -3 0 504.52 23.09 -1 -3 0 534.95 23.50 -1 -3 0 518.32 21.99 -1 -3 0 534.15 21.94 1 3 0 527.58 23.31 1 3 0 519.67 23.35 1 3 0 560.51 24.62 1 3 0 508.98 22.09 1 3 0 551.77 23.53 1 3 0 506.98 22.93 1 3 0 569.61 22.00 -2 -3 0 193.63 10.14 -2 -3 0 184.17 9.16 -2 -3 0 188.05 9.44 2 3 0 207.14 9.22 2 3 0 189.36 9.90 2 3 0 208.35 11.67 2 3 0 199.80 9.52 -3 -3 0 8.76 1.92 -3 -3 0 11.03 3.01 -3 -3 0 7.90 2.07 -3 -3 0 4.65 2.66 -3 -3 0 7.70 1.77 3 3 0 6.82 1.17 3 3 0 10.54 1.80 3 3 0 8.64 2.51 3 3 0 5.57 3.70 -4 -3 0 584.94 26.07 -4 -3 0 552.58 24.88 -4 -3 0 534.31 24.03 4 3 0 580.55 28.28 4 3 0 537.21 24.16 4 3 0 591.26 26.27 4 3 0 539.56 24.84 -5 -3 0 105.75 7.52 -5 -3 0 97.63 8.31 -5 -3 0 105.91 6.05 5 3 0 104.86 9.18 5 3 0 115.46 10.77 6 3 0 9.96 4.89 6 3 0 13.74 5.81 7 3 0 37.71 8.23 7 3 0 52.60 8.25 -8 -3 0 110.07 13.08 8 3 0 104.23 14.22 8 3 0 87.15 11.80 -8 4 0 -3.12 5.95 -8 4 0 -6.50 5.27 7 -4 0 159.50 10.85 -7 4 0 166.93 16.53 -7 4 0 167.26 13.21 6 -4 0 4.11 2.78 -6 4 0 -2.28 3.68 -6 4 0 0.67 3.80 5 -4 0 80.66 6.26 5 -4 0 70.10 8.78 -5 4 0 72.25 7.41 -5 4 0 77.01 10.55 4 -4 0 118.67 7.78 4 -4 0 134.67 10.05 -4 4 0 136.30 8.80 -4 4 0 140.55 12.01 3 -4 0 24.83 4.00 -3 4 0 20.63 3.30 -3 4 0 29.38 3.68 -3 4 0 26.46 4.66 -3 4 0 24.83 3.86 2 -4 0 26.21 3.40 2 -4 0 21.27 2.42 2 -4 0 20.84 3.10 -2 4 0 22.99 2.77 -2 4 0 16.15 3.58 -2 4 0 20.79 3.05 -2 4 0 26.46 3.11 -2 4 0 22.46 2.79 1 -4 0 427.25 19.39 1 -4 0 402.30 17.95 -1 4 0 438.89 18.57 -1 4 0 432.67 21.21 -1 4 0 396.25 19.14 -1 4 0 425.81 18.09 -1 4 0 417.03 18.64 0 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49.88 9.57 -3 4 15 39.35 8.34 -3 4 15 31.65 8.26 2 -4 -15 -1.06 3.41 2 -4 -15 -6.69 5.11 -2 4 15 3.81 5.89 -2 4 15 -1.92 4.75 1 -4 -15 -2.76 4.71 -1 4 15 0.06 5.08 -1 4 15 -5.43 4.63 0 -4 -15 122.12 11.18 0 4 15 112.73 13.12 0 4 15 111.88 11.61 -1 -4 -15 -3.07 4.07 1 4 15 -1.52 4.58 -2 -4 -15 20.65 5.43 2 4 15 17.98 6.30 -3 -4 -15 10.16 4.26 3 4 15 12.35 5.88 4 4 15 8.82 6.12 4 4 15 16.98 7.91 5 4 15 7.74 5.99 5 4 15 3.84 7.66 6 4 15 13.14 6.68 6 4 15 0.02 9.35 3 -5 -15 11.51 4.65 -3 5 15 1.73 7.02 -3 5 15 -11.73 5.76 2 -5 -15 18.10 4.87 -2 5 15 11.37 6.29 -2 5 15 13.90 7.17 -1 5 15 0.50 5.47 -1 5 15 -0.21 5.37 0 5 15 188.38 16.64 0 5 15 197.80 15.01 1 5 15 52.53 8.58 2 5 15 -0.07 5.36 3 5 15 589.50 31.34 4 5 15 269.55 21.49 4 5 15 253.63 18.95 5 5 15 8.08 6.13 5 5 15 8.48 8.81 6 5 15 9.49 6.41 6 5 15 11.54 9.52 2 -6 -15 31.54 6.19 -2 6 15 18.49 7.04 -2 6 15 17.37 7.95 1 -6 -15 0.82 4.03 -1 6 15 -4.77 5.73 -1 6 15 -2.22 6.03 0 6 15 25.47 6.68 0 6 15 18.24 6.55 1 6 15 -4.49 5.01 2 6 15 41.89 8.13 3 6 15 32.69 7.92 4 6 15 62.97 12.62 4 6 15 57.94 9.55 5 6 15 9.05 8.81 5 6 15 5.77 5.77 1 -7 -15 -1.35 4.71 -1 7 15 -2.98 5.82 0 7 15 18.65 6.96 1 7 15 60.73 9.55 2 7 15 -2.64 5.72 3 7 15 13.58 6.64 4 7 15 333.43 26.57 4 7 15 330.08 21.84 1 4 -16 283.20 17.31 -1 -4 16 298.68 19.78 0 4 -16 -0.30 3.91 0 -4 16 1.30 5.92 -1 4 -16 -2.77 3.42 1 -4 16 -0.27 6.00 -2 4 -16 39.32 6.26 2 -4 16 42.76 8.41 3 -4 16 18.86 7.18 2 3 -16 59.03 7.82 1 3 -16 0.07 3.88 -1 -3 16 6.30 6.40 0 3 -16 74.72 9.12 0 -3 16 86.05 11.25 -1 3 -16 21.76 5.58 1 -3 16 28.67 7.29 -2 3 -16 -2.65 3.63 2 -3 16 -0.32 5.44 -3 3 -16 84.76 9.04 3 -3 16 57.46 8.81 -4 3 -16 80.56 10.30 3 2 -16 6.29 5.07 -3 -2 16 15.86 7.34 2 2 -16 -2.99 4.27 -2 -2 16 -5.40 5.45 1 2 -16 30.90 6.09 -1 -2 16 29.56 6.99 0 2 -16 1.41 3.90 0 -2 16 0.80 4.98 -1 2 -16 78.51 9.04 1 -2 16 98.40 10.20 -2 2 -16 24.88 5.39 2 -2 16 27.99 6.33 -3 2 -16 66.18 8.59 3 -2 16 83.79 10.09 -5 2 -16 5.93 4.71 3 1 -16 -1.21 4.95 2 1 -16 46.07 7.80 1 1 -16 63.99 7.92 0 1 -16 8.58 4.31 0 -1 16 16.09 5.68 -1 1 -16 45.86 6.97 1 -1 16 48.33 7.28 -2 1 -16 31.41 5.99 2 -1 16 22.17 5.78 -3 1 -16 503.55 26.20 3 -1 16 501.66 25.35 -4 1 -16 10.03 4.44 -5 1 -16 7.16 4.92 -6 1 -16 168.23 14.71 4 0 -16 -6.01 5.47 3 0 -16 3.36 5.58 2 0 -16 14.00 5.62 1 0 -16 -2.81 3.52 0 0 -16 7.36 4.54 0 0 16 16.11 8.87 -1 0 -16 254.20 15.47 1 0 16 219.33 14.03 -2 0 -16 -4.91 3.82 2 0 16 -1.86 4.37 2 0 16 1.35 5.01 -3 0 -16 38.65 6.23 3 0 16 48.77 6.66 3 0 16 37.52 7.25 -4 0 -16 236.85 15.74 4 0 16 242.56 18.17 5 0 16 219.45 24.81 -6 0 -16 14.91 5.84 4 -1 -16 49.82 9.78 3 -1 -16 30.43 7.45 2 -1 -16 47.47 8.09 -2 1 16 52.02 8.56 1 -1 -16 16.33 5.77 -1 1 16 1.04 5.30 0 -1 -16 81.50 8.70 0 1 16 89.07 10.14 -1 -1 -16 1.20 3.81 1 1 16 -1.85 3.94 -2 -1 -16 70.04 8.98 2 1 16 88.63 10.72 -3 -1 -16 27.84 6.04 3 1 16 22.81 6.16 -4 -1 -16 323.29 19.33 4 1 16 352.19 22.14 5 1 16 238.20 18.86 -6 -1 -16 48.68 8.46 6 1 16 53.47 10.21 4 -2 -16 146.50 15.79 -4 2 16 125.45 14.67 -4 2 16 162.48 18.34 3 -2 -16 128.74 14.02 -3 2 16 118.31 13.49 -3 2 16 159.56 17.30 2 -2 -16 -1.27 4.67 -2 2 16 -4.80 5.38 -2 2 16 1.93 5.08 1 -2 -16 4.66 4.88 -1 2 16 1.79 5.51 0 -2 -16 4.51 3.95 0 2 16 -3.34 4.34 -1 -2 -16 0.27 3.98 1 2 16 8.68 5.11 -2 -2 -16 0.63 3.94 2 2 16 -2.62 4.83 -3 -2 -16 182.60 13.34 3 2 16 168.92 14.50 -4 -2 -16 138.77 11.76 4 2 16 162.07 14.79 5 2 16 10.15 6.27 -6 -2 -16 24.86 6.31 6 2 16 24.60 8.14 3 -3 -16 10.83 7.17 -3 3 16 4.47 6.44 -3 3 16 9.71 6.50 2 -3 -16 8.51 5.59 -2 3 16 -0.22 5.72 -2 3 16 6.04 5.68 1 -3 -16 6.69 5.45 -1 3 16 0.90 4.74 -1 3 16 10.65 5.44 0 -3 -16 87.63 10.02 0 3 16 86.61 10.49 -1 -3 -16 7.72 4.65 1 3 16 2.19 5.30 -2 -3 -16 52.36 8.02 2 3 16 37.85 7.68 -3 -3 -16 42.79 6.88 3 3 16 70.86 9.73 -4 -3 -16 10.80 5.20 4 3 16 0.56 5.00 5 3 16 6.01 6.16 6 3 16 0.84 6.17 3 -4 -16 63.90 13.93 -3 4 16 53.39 9.93 -3 4 16 47.84 9.82 2 -4 -16 45.49 8.83 -2 4 16 34.03 7.76 -2 4 16 28.68 7.87 1 -4 -16 8.67 5.59 -1 4 16 13.79 6.67 -1 4 16 10.66 5.79 0 -4 -16 133.72 11.85 0 4 16 117.45 12.44 -1 -4 -16 29.35 6.37 1 4 16 26.73 7.17 -2 -4 -16 0.05 4.55 2 4 16 2.09 5.20 3 4 16 -0.18 5.55 4 4 16 8.69 7.36 4 4 16 9.56 5.67 5 4 16 0.24 7.54 5 4 16 5.95 6.27 6 4 16 3.09 5.82 -2 5 16 -0.81 6.02 -2 5 16 2.45 6.35 -1 5 16 1.38 5.81 -1 5 16 3.49 6.12 0 5 16 39.15 8.08 0 5 16 29.51 6.75 1 5 16 15.38 6.59 2 5 16 -2.86 5.27 3 5 16 9.68 6.08 4 5 16 34.00 10.45 4 5 16 16.05 7.09 5 5 16 11.92 9.02 5 5 16 6.93 6.13 -1 6 16 -0.32 5.93 -1 6 16 -4.14 5.93 0 6 16 4.29 5.78 0 6 16 6.01 5.42 1 6 16 100.77 12.56 2 6 16 -3.74 5.00 3 6 16 -2.02 6.08 4 6 16 10.72 8.78 4 6 16 8.43 6.20 1 7 16 0.63 6.02 2 7 16 31.03 8.10 -1 4 -17 11.60 4.87 1 -4 17 18.91 7.31 1 3 -17 10.09 4.97 -1 -3 17 14.34 7.34 0 3 -17 2.61 4.39 0 -3 17 3.37 6.23 -1 3 -17 48.72 7.31 1 -3 17 30.35 7.13 -2 3 -17 8.71 4.77 2 -3 17 9.65 6.28 -3 3 -17 69.38 8.60 3 -3 17 44.27 8.33 2 2 -17 154.33 13.33 -2 -2 17 188.38 15.75 1 2 -17 9.55 4.87 -1 -2 17 15.28 6.97 0 2 -17 412.71 23.11 0 -2 17 431.36 23.44 -1 2 -17 57.26 7.88 1 -2 17 62.42 8.84 -2 2 -17 -1.63 4.07 2 -2 17 2.11 5.39 -3 2 -17 150.62 12.31 3 -2 17 138.89 12.77 3 1 -17 3.91 5.98 2 1 -17 27.99 7.06 1 1 -17 3.14 4.33 -1 -1 17 -4.08 5.15 0 1 -17 2.25 4.63 0 -1 17 6.81 6.09 -1 1 -17 41.32 6.91 1 -1 17 38.86 7.41 -2 1 -17 10.27 5.09 2 -1 17 13.18 5.33 -3 1 -17 7.63 4.89 3 -1 17 3.45 4.55 -4 1 -17 12.95 5.07 -5 1 -17 112.28 12.12 3 0 -17 283.77 19.48 2 0 -17 25.73 7.05 1 0 -17 1.83 4.60 0 0 -17 160.50 12.68 -1 0 -17 120.61 11.33 1 0 17 122.82 11.14 -2 0 -17 11.07 4.71 2 0 17 10.11 5.40 -3 0 -17 6.35 4.87 -4 0 -17 26.06 6.31 3 -1 -17 75.61 10.91 2 -1 -17 -1.62 4.95 1 -1 -17 1.94 5.18 -1 1 17 3.39 4.94 0 -1 -17 0.75 4.50 0 1 17 -0.25 5.16 -1 -1 -17 3.26 4.49 1 1 17 3.24 4.87 -2 -1 -17 57.89 8.34 2 1 17 52.85 8.39 2 1 17 40.54 6.50 -3 -1 -17 3.92 4.79 3 1 17 2.11 5.75 -4 -1 -17 267.34 17.12 4 1 17 261.60 19.96 5 1 17 8.93 6.80 3 -2 -17 -10.40 5.60 -3 2 17 -9.53 6.13 2 -2 -17 -6.36 5.25 -2 2 17 1.86 6.32 1 -2 -17 -1.35 5.13 -1 2 17 2.49 5.43 0 -2 -17 0.97 4.62 0 2 17 -0.26 5.32 -1 -2 -17 17.73 5.88 1 2 17 15.62 6.17 -2 -2 -17 64.74 9.04 2 2 17 48.29 8.51 -3 -2 -17 2.26 4.88 3 2 17 -3.91 5.15 -4 -2 -17 23.99 5.99 4 2 17 23.86 7.96 5 2 17 31.65 8.63 3 -3 -17 118.46 14.92 -3 3 17 157.07 18.46 -3 3 17 107.70 13.99 2 -3 -17 18.99 6.71 -2 3 17 27.27 7.63 -2 3 17 16.21 7.79 1 -3 -17 -1.88 5.37 -1 3 17 0.11 5.93 0 -3 -17 16.57 6.00 0 3 17 8.76 5.89 -1 -3 -17 8.72 5.22 1 3 17 19.44 6.93 -2 -3 -17 12.71 5.42 2 3 17 8.93 6.26 -3 -3 -17 15.34 5.68 3 3 17 16.94 7.19 -4 -3 -17 17.66 6.27 4 3 17 12.04 6.68 -5 -3 -17 195.85 15.35 5 3 17 206.36 18.19 2 -4 -17 12.52 8.63 -2 4 17 1.12 6.65 -2 4 17 18.44 7.01 1 -4 -17 -1.33 5.54 -1 4 17 -0.96 5.38 0 -4 -17 8.54 5.68 0 4 17 -4.53 5.01 -1 -4 -17 0.57 4.51 1 4 17 1.40 5.84 -2 -4 -17 7.44 6.56 2 4 17 9.45 6.52 3 4 17 -5.98 5.43 4 4 17 25.92 12.49 4 4 17 27.01 7.54 5 4 17 88.71 12.25 -1 5 17 3.59 6.27 -1 5 17 16.02 6.45 0 5 17 0.32 5.69 1 5 17 8.44 6.54 2 5 17 3.24 5.94 3 5 17 15.35 7.06 4 5 17 15.46 7.26 4 5 17 26.64 9.42 0 6 17 14.03 7.04 0 6 17 37.17 12.17 1 6 17 13.07 7.06 2 6 17 12.26 7.09 3 6 17 1.93 6.16 1 -3 18 27.83 7.53 1 2 -18 40.28 7.27 -1 -2 18 32.00 8.27 0 2 -18 42.55 7.45 0 -2 18 71.91 9.91 -1 2 -18 11.82 5.04 1 -2 18 10.84 6.03 -2 2 -18 4.45 4.35 2 -2 18 12.62 6.08 -3 2 -18 16.36 5.47 3 -2 18 11.37 7.25 2 1 -18 87.41 11.21 -2 -1 18 84.84 10.87 1 1 -18 15.13 5.72 -1 -1 18 3.97 6.08 0 1 -18 47.97 7.55 0 -1 18 58.38 9.05 -1 1 -18 7.52 5.03 1 -1 18 3.85 5.68 -2 1 -18 3.82 4.47 2 -1 18 6.12 5.62 -3 1 -18 6.20 4.89 -4 1 -18 115.38 11.78 2 0 -18 168.74 14.87 1 0 -18 92.41 11.08 0 0 -18 73.11 9.43 -1 0 -18 143.82 12.32 1 0 18 160.32 12.85 -2 0 -18 34.93 7.02 2 0 18 45.70 7.37 -3 0 -18 -0.12 4.32 -4 0 -18 100.47 11.23 2 -1 -18 3.51 5.68 1 -1 -18 116.18 12.10 0 -1 -18 0.01 4.28 -1 -1 -18 0.42 4.96 1 1 18 -1.76 4.95 -2 -1 -18 4.72 4.91 2 1 18 -6.33 4.88 2 1 18 1.07 5.62 -3 -1 -18 -0.70 4.29 3 1 18 1.56 5.84 -4 -1 -18 13.00 5.68 4 1 18 17.42 7.49 5 1 18 1.02 7.36 2 -2 -18 283.21 19.94 -2 2 18 282.74 20.93 1 -2 -18 75.14 10.37 -1 2 18 62.51 9.87 0 -2 -18 5.61 5.01 0 2 18 -2.83 5.74 -1 -2 -18 88.55 11.17 1 2 18 104.43 11.90 -2 -2 -18 216.34 15.53 2 2 18 221.14 17.76 -3 -2 -18 17.48 6.03 3 2 18 5.63 6.85 -4 -2 -18 19.60 6.29 4 2 18 17.79 8.21 5 2 18 91.08 12.95 2 -3 -18 29.12 8.04 -2 3 18 29.49 9.44 1 -3 -18 1.82 5.51 -1 3 18 -6.07 6.39 0 -3 -18 13.54 6.32 0 3 18 17.99 7.40 -1 -3 -18 8.42 5.40 1 3 18 9.44 6.85 -2 -3 -18 -3.01 4.85 2 3 18 -0.44 5.44 -3 -3 -18 27.46 7.38 3 3 18 16.90 6.90 -4 -3 -18 25.73 7.27 4 3 18 31.46 8.13 -1 4 18 29.58 8.73 0 -4 -18 0.17 10.69 0 4 18 1.07 6.45 1 4 18 -2.93 6.06 2 4 18 32.07 8.22 3 4 18 -1.10 5.65 4 4 18 2.64 5.93 0 5 18 -0.96 5.48 1 5 18 1.04 6.34 2 5 18 3.05 6.47 3 5 18 11.58 7.34 0 1 -19 3.68 5.03 0 -1 19 -6.07 5.63 -1 1 -19 153.44 13.26 1 -1 19 171.28 13.77 -2 1 -19 9.66 5.43 2 -1 19 9.14 6.07 1 0 -19 43.40 8.50 0 0 -19 20.61 6.13 0 0 19 33.10 7.44 -1 0 -19 170.60 14.20 1 0 19 179.68 13.94 -2 0 -19 -0.17 4.73 2 0 19 2.03 5.42 -3 0 -19 6.36 5.23 1 -1 -19 36.46 7.52 0 -1 -19 5.51 5.72 -1 -1 -19 56.32 9.01 -2 -1 -19 28.85 6.62 -3 -1 -19 4.44 5.23 -4 -1 -19 1.98 5.36 1 -2 -19 4.87 5.36 -1 2 19 1.66 8.82 0 -2 -19 10.48 6.09 0 2 19 17.27 7.57 -1 -2 -19 150.58 14.10 1 2 19 155.90 15.77 -2 -2 -19 -3.79 4.93 2 2 19 0.59 6.97 -3 -2 -19 10.13 6.05 3 2 19 6.16 6.78 -4 -2 -19 11.66 6.48 4 2 19 2.57 6.80 0 -3 -19 105.65 12.28 0 3 19 92.72 12.43 -1 -3 -19 2.32 5.78 1 3 19 -3.30 6.62 -2 -3 -19 21.01 7.05 2 3 19 19.22 7.60 -3 -3 -19 3.25 5.57 3 3 19 9.29 7.37 1 4 19 6.12 7.01 2 4 19 11.70 7.04 0 0 0 0.00 0.00 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6460 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71155 6.495 7.149 13.920 81.976 81.046 86.520 ) _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 39971 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 C1 C 0.3845(2) 0.9590(2) 0.15033(11) 0.0288(4) Uani 1 1 d . . . . . C2 C 0.1090(2) 1.0047(2) 0.27627(11) 0.0267(3) Uani 1 1 d . . . . . C3 C -0.0163(2) 1.0850(2) 0.20455(12) 0.0291(4) Uani 1 1 d . . . . . C4 C 0.0613(3) 1.1016(2) 0.10977(12) 0.0336(4) Uani 1 1 d . . . . . H4 H -0.019152 1.155187 0.062653 0.040 Uiso 1 1 calc R U . . . F1 F -0.21162(14) 1.14589(15) 0.23599(7) 0.0430(3) Uani 1 1 d . . . . . N1 N 0.2607(2) 1.0386(2) 0.08303(10) 0.0348(4) Uani 1 1 d . . . . . H1N H 0.320(3) 1.047(3) 0.0192(18) 0.055(6) Uiso 1 1 d . . . . . N2 N 0.30550(19) 0.94452(18) 0.24719(9) 0.0272(3) Uani 1 1 d . . . . . N3 N 0.0341(2) 0.9898(2) 0.37043(10) 0.0360(4) Uani 1 1 d . . . . . H3N H 0.124(3) 0.936(3) 0.4178(15) 0.044(5) Uiso 1 1 d . . . . . H4N H -0.095(4) 1.031(3) 0.3890(16) 0.051(6) Uiso 1 1 d . . . . . O1 O 0.56533(17) 0.90317(18) 0.12046(8) 0.0382(3) Uani 1 1 d . . . . . C5 C 0.4803(2) 0.7800(2) 0.47145(12) 0.0311(4) Uani 1 1 d . . . . . C6 C 0.6320(3) 0.6952(2) 0.53401(12) 0.0353(4) Uani 1 1 d . . . . . H6 H 0.767569 0.670267 0.504957 0.042 Uiso 1 1 calc R U . . . C7 C 0.5838(3) 0.6529(2) 0.62998(12) 0.0316(4) Uani 1 1 d . . . . . H7 H 0.447168 0.680710 0.656497 0.038 Uiso 1 1 calc R U . . . C8 C 0.7210(2) 0.5673(2) 0.69944(11) 0.0297(4) Uani 1 1 d . . . . . C9 C 0.9264(3) 0.5096(2) 0.66891(12) 0.0357(4) Uani 1 1 d . . . . . H9 H 0.978807 0.523927 0.602412 0.043 Uiso 1 1 calc R U . . . C10 C 1.0530(3) 0.4314(2) 0.73609(13) 0.0364(4) Uani 1 1 d D . . . . H10 H 1.189134 0.392725 0.714413 0.044 Uiso 0.909(4) 1 calc R U P A 1 C11 C 0.9789(3) 0.4102(2) 0.83512(12) 0.0325(4) Uani 1 1 d . . . . . C12 C 0.7741(3) 0.4678(2) 0.86763(12) 0.0338(4) Uani 1 1 d . . . . . H12 H 0.723249 0.454551 0.934283 0.041 Uiso 0.091(4) 1 calc R U P A 2 C13 C 0.6478(2) 0.5445(2) 0.80003(12) 0.0318(4) Uani 1 1 d . . . . . H13 H 0.511199 0.581826 0.821843 0.038 Uiso 1 1 calc R U . . . O2 O 0.29971(18) 0.82156(19) 0.50312(8) 0.0444(4) Uani 1 1 d . . . . . O3 O 0.55687(19) 0.8085(2) 0.37788(9) 0.0430(3) Uani 1 1 d . . . . . H3O H 0.452(4) 0.854(3) 0.3351(18) 0.068(7) Uiso 1 1 d . . . . . O4 O 0.7053(2) 0.4430(3) 0.96611(10) 0.0552(6) Uani 0.909(4) 1 d . . P A 1 H4O H 0.787962 0.487726 0.994638 0.083 Uiso 0.909(4) 1 calc R U P A 1 O4D O 1.2460(17) 0.384(2) 0.7330(11) 0.049(5) Uani 0.091(4) 1 d D . P A 2 H4DO H 1.258390 0.273133 0.756053 0.073 Uiso 0.091(4) 1 calc R U P A 2 O5 O 1.0989(2) 0.3370(2) 0.90462(9) 0.0459(4) Uani 1 1 d . . . . . H5O H 1.205757 0.287634 0.878221 0.069 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 C1 0.0269(8) 0.0330(8) 0.0252(8) -0.0024(6) -0.0037(6) 0.0039(6) C2 0.0263(8) 0.0269(8) 0.0264(8) -0.0033(6) -0.0031(6) -0.0006(6) C3 0.0220(8) 0.0337(8) 0.0308(8) -0.0046(6) -0.0038(6) 0.0047(6) C4 0.0303(8) 0.0416(9) 0.0286(8) -0.0020(7) -0.0096(7) 0.0083(7) F1 0.0269(5) 0.0614(7) 0.0392(6) -0.0093(5) -0.0033(4) 0.0136(4) N1 0.0315(7) 0.0491(9) 0.0207(7) -0.0008(6) -0.0019(6) 0.0093(6) N2 0.0259(7) 0.0327(7) 0.0218(6) -0.0017(5) -0.0038(5) 0.0042(5) N3 0.0288(8) 0.0514(9) 0.0249(7) -0.0028(6) -0.0004(6) 0.0079(7) O1 0.0279(6) 0.0551(8) 0.0278(6) -0.0025(5) -0.0005(5) 0.0120(5) C5 0.0312(8) 0.0348(9) 0.0257(8) -0.0026(6) -0.0028(6) 0.0046(7) C6 0.0299(8) 0.0437(9) 0.0302(9) -0.0018(7) -0.0039(7) 0.0088(7) C7 0.0293(8) 0.0345(9) 0.0298(8) -0.0028(7) -0.0049(6) 0.0060(6) C8 0.0316(8) 0.0295(8) 0.0274(8) -0.0017(6) -0.0060(6) 0.0021(6) C9 0.0358(9) 0.0421(9) 0.0256(8) -0.0012(7) -0.0007(7) 0.0090(7) C10 0.0299(8) 0.0402(9) 0.0367(9) -0.0025(7) -0.0034(7) 0.0077(7) C11 0.0340(9) 0.0317(8) 0.0329(9) -0.0018(7) -0.0120(7) 0.0024(7) C12 0.0353(9) 0.0405(9) 0.0247(8) -0.0023(7) -0.0041(7) 0.0006(7) C13 0.0269(8) 0.0386(9) 0.0289(8) -0.0052(7) -0.0026(6) 0.0038(7) O2 0.0335(7) 0.0679(9) 0.0271(6) -0.0002(6) -0.0022(5) 0.0164(6) O3 0.0359(7) 0.0651(8) 0.0233(6) 0.0020(5) -0.0024(5) 0.0135(6) O4 0.0392(8) 0.1018(14) 0.0231(8) -0.0051(8) -0.0050(6) 0.0029(8) O4D 0.022(7) 0.078(11) 0.047(9) -0.015(8) -0.011(6) 0.024(7) O5 0.0408(7) 0.0612(9) 0.0348(7) -0.0010(6) -0.0140(5) 0.0154(6) 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' 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 O1 C1 N2 122.44(14) . . ? O1 C1 N1 118.88(14) . . ? N2 C1 N1 118.68(13) . . ? N3 C2 N2 119.98(14) . . ? N3 C2 C3 120.61(14) . . ? N2 C2 C3 119.41(14) . . ? C4 C3 F1 121.77(14) . . ? C4 C3 C2 120.20(14) . . ? F1 C3 C2 118.01(13) . . ? C3 C4 N1 118.76(15) . . ? C3 C4 H4 120.6 . . ? N1 C4 H4 120.6 . . ? C4 N1 C1 122.39(14) . . ? C4 N1 H1N 121.8(14) . . ? C1 N1 H1N 115.8(14) . . ? C2 N2 C1 120.56(13) . . ? C2 N3 H3N 118.8(12) . . ? C2 N3 H4N 119.4(14) . . ? H3N N3 H4N 121.7(18) . . ? O2 C5 O3 122.96(15) . . ? O2 C5 C6 123.44(15) . . ? O3 C5 C6 113.60(14) . . ? C7 C6 C5 122.66(15) . . ? C7 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? C6 C7 C8 127.48(15) . . ? C6 C7 H7 116.3 . . ? C8 C7 H7 116.3 . . ? C9 C8 C13 118.01(15) . . ? C9 C8 C7 122.14(14) . . ? C13 C8 C7 119.84(14) . . ? C10 C9 C8 120.89(15) . . ? C10 C9 H9 119.6 . . ? C8 C9 H9 119.6 . . ? O4D C10 C11 103.3(7) . . ? O4D C10 C9 135.7(7) . . ? C11 C10 C9 120.51(15) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? O5 C11 C10 122.78(15) . . ? O5 C11 C12 117.49(15) . . ? C10 C11 C12 119.72(15) . . ? O4 C12 C13 122.31(16) . . ? O4 C12 C11 118.18(15) . . ? C13 C12 C11 119.50(15) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C8 121.37(15) . . ? C12 C13 H13 119.3 . . ? C8 C13 H13 119.3 . . ? C5 O3 H3O 113.8(14) . . ? C12 O4 H4O 109.5 . . ? C10 O4D H4DO 109.5 . . ? C11 O5 H5O 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 C1 O1 1.2482(19) . ? C1 N2 1.360(2) . ? C1 N1 1.373(2) . ? C2 N3 1.319(2) . ? C2 N2 1.3452(19) . ? C2 C3 1.425(2) . ? C3 C4 1.330(2) . ? C3 F1 1.3467(17) . ? C4 N1 1.362(2) . ? C4 H4 0.9300 . ? N1 H1N 0.91(2) . ? N3 H3N 0.97(2) . ? N3 H4N 0.89(2) . ? C5 O2 1.2246(19) . ? C5 O3 1.3137(19) . ? C5 C6 1.467(2) . ? C6 C7 1.321(2) . ? C6 H6 0.9300 . ? C7 C8 1.466(2) . ? C7 H7 0.9300 . ? C8 C9 1.395(2) . ? C8 C13 1.399(2) . ? C9 C10 1.381(2) . ? C9 H9 0.9300 . ? C10 O4D 1.277(11) . ? C10 C11 1.380(2) . ? C10 H10 0.9300 . ? C11 O5 1.367(2) . ? C11 C12 1.397(2) . ? C12 O4 1.366(2) . ? C12 C13 1.381(2) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? O3 H3O 0.99(3) . ? O4 H4O 0.8200 . ? O4D H4DO 0.8200 . ? O5 H5O 0.8200 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1N O1 0.91(2) 1.96(2) 2.8678(18) 173(2) 2_675 yes N3 H4N O2 0.89(2) 2.19(2) 2.9658(19) 145.3(19) 2_576 yes O5 H5O O1 0.82 1.96 2.7122(17) 151.4 2_766 yes O4^a H4O^a O5 0.82 2.24 3.017(2) 158.3 2_767 yes O3 H3O N2 0.99(3) 1.70(3) 2.6801(17) 171(2) . yes N3 H3N O2 0.97(2) 1.85(2) 2.8253(19) 176.5(18) . yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 C2 C3 C4 179.17(16) . . . . ? N2 C2 C3 C4 -0.5(2) . . . . ? N3 C2 C3 F1 0.4(2) . . . . ? N2 C2 C3 F1 -179.27(13) . . . . ? F1 C3 C4 N1 179.43(14) . . . . ? C2 C3 C4 N1 0.7(3) . . . . ? C3 C4 N1 C1 -0.1(3) . . . . ? O1 C1 N1 C4 179.50(15) . . . . ? N2 C1 N1 C4 -0.7(2) . . . . ? N3 C2 N2 C1 179.99(15) . . . . ? C3 C2 N2 C1 -0.3(2) . . . . ? O1 C1 N2 C2 -179.31(14) . . . . ? N1 C1 N2 C2 0.9(2) . . . . ? O2 C5 C6 C7 1.6(3) . . . . ? O3 C5 C6 C7 -178.86(16) . . . . ? C5 C6 C7 C8 179.55(16) . . . . ? C6 C7 C8 C9 -3.4(3) . . . . ? C6 C7 C8 C13 175.38(17) . . . . ? C13 C8 C9 C10 0.4(3) . . . . ? C7 C8 C9 C10 179.18(16) . . . . ? C8 C9 C10 O4D -171.4(11) . . . . ? C8 C9 C10 C11 -0.5(3) . . . . ? O4D C10 C11 O5 -5.3(8) . . . . ? C9 C10 C11 O5 -178.75(16) . . . . ? O4D C10 C11 C12 173.6(8) . . . . ? C9 C10 C11 C12 0.2(3) . . . . ? O5 C11 C12 O4 -1.6(3) . . . . ? C10 C11 C12 O4 179.35(17) . . . . ? O5 C11 C12 C13 179.32(15) . . . . ? C10 C11 C12 C13 0.3(3) . . . . ? O4 C12 C13 C8 -179.49(17) . . . . ? C11 C12 C13 C8 -0.5(3) . . . . ? C9 C8 C13 C12 0.2(3) . . . . ? C7 C8 C13 C12 -178.69(15) . . . . ? _cod_database_fobs_code 2312700