#------------------------------------------------------------------------------ #$Date: 2025-04-10 09:33:42 +0100 (Thu, 10 Apr 2025) $ #$Revision: 299250 $ #$URL: svn://www.crystallography.net/cod/cif/3/00/05/3000560.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_3000560 loop_ _publ_author_name 'Gogoi, Diptajyoti' 'Sasaki, Toshiyuki' 'Kalita, Nabadeep' 'Sethi, Tapaswini' 'Ichiyanagi, Kouhei' 'Nakane, Takanori' 'Kawamoto, Akihiro' 'Das, Dinabandhu' 'Kurisu, Genji' 'Thakuria, Ranjit' _publ_section_title ; Tuning of a Hydrogen-Bonded Organic Framework by Liquid-Assisted Mechanosynthesis between Trans-Aconitic Acid and Isonicotinamide ; _journal_name_full 'Chemistry A European Journal' _journal_page_first e202403427(1) _journal_page_last e202403427(10) _journal_paper_doi 10.1002/chem.202403427 _journal_volume 31 _journal_year 2025 _chemical_formula_moiety 'C6 H5.762 O5.596, C6 H6 N2 O, 0.293(C N O2)' _chemical_formula_sum 'C12.29 H11.76 N2.29 O7.18' _chemical_formula_weight 306.51 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_date 2024-08-02 _audit_creation_method ; Olex2 1.5 (compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498) ; _cell_angle_alpha 90 _cell_angle_beta 109.13 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 27.933 _cell_length_b 15.206 _cell_length_c 7.146 _cell_measurement_reflns_used 2650 _cell_measurement_temperature 79 _cell_measurement_theta_max 0.8701407890883619 _cell_measurement_theta_min 0.12579614564801556 _cell_volume 2867.643 _computing_cell_refinement 'dials.two_theta_refine (Waterman et al., 2016)' _computing_data_collection 'Verlox (Thermo Fisher Scientific) and SerialEM (Mastronarde, 2005)' _computing_data_reduction 'dials.scale (Beilsten-Edmands et al., 2020)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 79.00 _diffrn_measured_fraction_theta_full 0.957 _diffrn_measured_fraction_theta_max 0.957 _diffrn_measurement_device_type ; Talos Arctica G2 ; _diffrn_radiation_type electrons _diffrn_radiation_wavelength 0.02508 _diffrn_reflns_av_R_equivalents 0.3853 _diffrn_reflns_av_unetI/netI 0.3074 _diffrn_reflns_Laue_measured_fraction_full 0.957 _diffrn_reflns_Laue_measured_fraction_max 0.957 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 18950 _diffrn_reflns_point_group_measured_fraction_full 0.957 _diffrn_reflns_point_group_measured_fraction_max 0.957 _diffrn_reflns_theta_full 0.845 _diffrn_reflns_theta_max 0.845 _diffrn_reflns_theta_min 0.139 _exptl_absorpt_coefficient_mu 0.000 _exptl_crystal_density_diffrn 1.420 _exptl_crystal_description plate _exptl_crystal_F_000 442 _refine_diff_density_max 0.130 _refine_diff_density_min -0.137 _refine_diff_density_rms 0.036 _refine_ls_extinction_coef 428(62) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 2353 _refine_ls_number_restraints 193 _refine_ls_restrained_S_all 0.961 _refine_ls_R_factor_all 0.2584 _refine_ls_R_factor_gt 0.1444 _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^)+(0.1948P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3735 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 732 _reflns_number_total 2353 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file taca-ina-meno2_fill.cif _cod_data_source_block taca-ina-meno2 _cod_depositor_comments ;Author list was corrected. Releasing structure 3000560 into public domain as published material. ; _cod_original_cell_volume 2867.8 _cod_database_code 3000560 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All O(H) groups 2. Restrained distances O11-N3 1.22 with sigma of 0.02 O12-N3 1.22 with sigma of 0.02 C17-N3 1.48 with sigma of 0.02 O11-O12 2.15 with sigma of 0.02 C17-O11 2.33 with sigma of 0.02 C17-O12 2.33 with sigma of 0.02 3. Restrained planarity O12, N3, O11, C17 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints Uanis(O7B) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Sof(O7B)=Sof(H7B)=FVAR(1) Sof(O12)=Sof(N3)=Sof(O11)=Sof(C17)=0.5*FVAR(3) 7.a Secondary CH2 refined with riding coordinates: C11(H11A,H11B) 7.b Aromatic/amide H refined with riding coordinates: C8(H8), C2(H2A), C5(H5), C4(H4A), C1(H1) 7.c X=CH2 refined with riding coordinates: N2(H2B,H2C) 7.d Idealised tetrahedral OH refined as rotating group: O7A(H7A), O7B(H7B), O4(H4), O2(H2) ; _shelx_res_file ; TITL TACA-INA-MeNO2 in C2/c #15 taca-ina-meno2.res created by SHELXL-2018/3 at 13:04:08 on 02-Aug-2024 REM Best SHELXD solution FINAL CC 80.89 REM Fragments: 11 9 REM reset to C2/c #15 CELL 0.02508 27.9334 15.2059 7.1464 90 109.132 90 ZERR 8 0 0 0 0 0 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C 0.731 36.995 1.195 11.297 0.456 2.814 0.125 0.346 0 0 0 0 0.77 12.011 SFAC H 0.375 15.495 0.141 4.126 0.022 0.025 -0.101 46.884 0 0 0 0 0.32 1.008 SFAC N 0.572 28.846 1.042 9.054 0.465 2.421 0.131 0.317 0 0 0 0 0.75 14.007 SFAC O 0.455 23.78 0.917 7.622 0.472 2.144 0.138 0.296 0 0 0 0 0.73 15.999 UNIT 98.34 94.1 18.34 57.45 RIGU ISOR 0.01 0.01 O7B O4 C3 C6 C2 O2 DFIX 1.22 O11 N3 ISOR 0.005 0.01 C8 DFIX 1.22 O12 N3 DFIX 1.48 C17 N3 FLAT O12 N3 O11 C17 DFIX 2.15 O11 O12 DFIX 2.33 C17 O11 DFIX 2.33 C17 O12 L.S. 10 PLAN 5 TEMP -194.15 CONF MORE -1 BOND $H fmap 2 acta SHEL 99 0.85 OMIT 7 1 0 OMIT -16 0 4 REM REM REM WGHT 0.194800 EXTI 427.592468 FVAR 0.60520 0.22596 0.58515 PART 1 O7A 4 -0.000544 0.347583 0.428261 0.56036 0.04225 0.14530 = 0.08495 0.03020 0.01822 -0.00176 AFIX 147 H7A 2 -0.008601 0.301295 0.474777 0.53605 -1.50000 AFIX 0 PART 2 O7B 4 0.001113 0.427098 0.448947 21.00000 0.04226 0.05031 = 0.04630 -0.00543 0.01657 -0.00278 AFIX 147 H7B 2 0.007913 0.481038 0.461229 21.00000 -1.50000 AFIX 0 PART 0 O6 4 0.044741 0.380341 0.731209 0.80939 0.06976 0.07866 = 0.07138 0.02704 0.02042 0.02143 N1 3 0.147748 0.283301 0.159760 11.00000 0.04092 0.01792 = 0.03621 0.00319 0.02134 -0.00107 O4 4 0.138967 0.547226 0.643310 11.00000 0.04346 0.00506 = 0.04387 -0.00332 0.00755 -0.00424 AFIX 147 H4 2 0.141364 0.601554 0.665738 11.00000 0.08344 AFIX 0 C6 1 0.158272 0.001208 0.197284 11.00000 0.05048 0.00820 = 0.05107 0.00226 0.01731 0.00364 O1 4 0.120721 -0.040212 0.085384 11.00000 0.07051 0.00574 = 0.04924 -0.00342 0.00923 0.00634 C3 1 0.155708 0.101019 0.187630 11.00000 0.04241 0.01155 = 0.03279 0.00395 0.01250 -0.00859 C10 1 0.176107 0.507556 0.769503 11.00000 0.04578 0.00643 = 0.05163 -0.00312 0.00642 0.00148 C7 1 0.136072 0.354825 0.639412 11.00000 0.03503 0.01641 = 0.05014 -0.00514 0.01573 0.00358 C8 1 0.173991 0.406268 0.760475 11.00000 0.04589 0.01191 = 0.04360 0.00137 0.00796 0.00069 AFIX 43 H8 2 0.202145 0.376056 0.848784 11.00000 0.04178 AFIX 0 O5 4 0.213191 0.541080 0.885695 11.00000 0.04337 0.02134 = 0.04396 -0.00716 0.01707 -0.00628 C9 1 0.146639 0.254200 0.669030 11.00000 0.04121 0.01504 = 0.03536 0.00535 0.01131 0.00419 O3 4 0.187950 0.227131 0.770400 11.00000 0.04002 0.01275 = 0.06412 -0.00282 0.00843 -0.00470 C2 1 0.109901 0.140867 0.074347 11.00000 0.04328 0.01376 = 0.06372 0.00636 -0.00542 0.00442 AFIX 43 H2A 2 0.081333 0.106502 0.003181 11.00000 0.16448 AFIX 0 N2 3 0.198051 -0.036254 0.318257 11.00000 0.04467 0.00605 = 0.07939 -0.00279 0.01491 -0.00091 AFIX 93 H2B 2 0.199925 -0.093988 0.325628 11.00000 0.05670 H2C 2 0.223210 -0.003978 0.393093 11.00000 0.05633 AFIX 0 C5 1 0.190706 0.246853 0.259803 11.00000 0.04354 0.00751 = 0.07175 -0.00949 0.00715 -0.00230 AFIX 43 H5 2 0.218704 0.284039 0.322523 11.00000 0.10583 AFIX 0 C4 1 0.197860 0.154984 0.279960 11.00000 0.03163 0.01300 = 0.07916 0.00043 0.01372 0.00033 AFIX 43 H4A 2 0.229829 0.130512 0.352890 11.00000 0.05531 AFIX 0 C1 1 0.107905 0.230853 0.070180 11.00000 0.05404 0.01130 = 0.07204 0.00457 -0.00110 0.00921 AFIX 43 H1 2 0.076522 0.257984 -0.000145 11.00000 0.09669 AFIX 0 C11 1 0.088531 0.381796 0.489338 11.00000 0.04300 0.01491 = 0.07431 0.01062 0.00794 -0.00170 AFIX 23 H11A 2 0.082032 0.342371 0.373413 11.00000 0.15464 H11B 2 0.092878 0.442053 0.444958 11.00000 0.14637 AFIX 0 C12 1 0.041553 0.380806 0.557424 11.00000 0.03655 0.15385 = 0.07126 0.02466 0.01448 0.01663 O2 4 0.108256 0.207971 0.567721 11.00000 0.05003 0.01066 = 0.05580 0.00509 0.00600 0.00372 AFIX 147 H2 2 0.116637 0.154752 0.572511 11.00000 0.05601 AFIX 0 PART 3 O12 4 0.000000 -0.111982 -0.250000 30.50000 0.16144 N3 3 0.002563 -0.041830 -0.167026 30.50000 0.09279 O11 4 0.000000 0.029403 -0.250000 30.50000 0.22941 C17 1 0.009604 -0.042813 0.048441 30.50000 0.14605 HKLF 4 REM TACA-INA-MeNO2 in C2/c #15 REM wR2 = 0.4090, GooF = S = 0.978, Restrained GooF = 0.961 for all data REM R1 = 0.1444 for 732 Fo > 4sig(Fo) and 0.2584 for all 2353 data REM 232 parameters refined using 193 restraints END WGHT 0.1950 0.0000 REM Highest difference peak 0.130, deepest hole -0.137, 1-sigma level 0.036 Q1 1 0.1011 0.2252 -0.1749 11.00000 0.05 0.13 Q2 1 0.1065 0.1592 -0.1516 11.00000 0.05 0.13 Q3 1 0.1076 0.1439 0.3525 11.00000 0.05 0.11 Q4 1 0.0037 -0.1300 0.0071 11.00000 0.05 0.11 Q5 1 0.2212 0.0269 0.5028 11.00000 0.05 0.11 ; _shelx_res_checksum 84027 _shelx_hkl_file ; -1 13 -6 3.28 55.27 1 11 -4 166.23 46.27 2 10 -3 13.92 31.53 2 -8 4 10.65 30.71 10 18 -2 4.50 56.09 11 17 -1 -3.28 53.63 13 17 0 9.42 54.04 -14 -12 -3 3.28 39.30 -13 -13 -2 10.24 38.08 -6 8 -7 0.00 40.12 -6 6 -6 0.82 31.53 -11 -13 -1 17.20 37.67 -5 5 -5 -4.50 24.57 -8 -6 -2 0.41 17.20 -10 -14 0 -5.73 41.76 -4 4 -4 1.23 18.83 -7 -7 -1 29.07 18.42 -9 -15 1 -9.01 40.12 -5 -7 0 16.79 21.70 1 13 -5 -3.68 45.04 2 14 -5 9.42 48.31 -6 -16 3 -9.83 45.86 3 15 -5 4.50 54.04 2 12 -4 54.45 41.76 -5 -15 3 -14.74 49.13 3 13 -4 -8.19 42.99 -3 -9 2 7.37 23.75 3 11 -3 -0.41 34.80 -2 -8 2 231.33 27.84 -4 -16 4 -2.46 54.04 4 12 -3 -7.37 32.75 4 10 -2 2.05 30.71 -1 -9 3 13.92 28.66 5 11 -2 11.46 28.66 5 9 -1 5.32 27.43 -1 -15 5 -24.97 52.41 6 10 -1 124.06 27.02 1 -9 4 -3.28 30.30 6 8 0 93.35 25.38 7 9 0 20.88 25.79 2 -10 5 15.97 34.39 3 -9 5 18.83 36.85 8 8 1 9.42 22.52 6 -2 4 3.28 15.97 4 -10 6 4.50 43.40 5 -9 6 18.83 37.67 10 8 2 -2.87 22.11 15 7 5 -1.64 27.02 -15 -11 -4 0.41 36.85 -15 -13 -3 -2.87 38.49 -14 -14 -2 -9.83 40.12 -13 -15 -1 0.41 40.53 -12 -14 -1 -6.14 42.99 -12 -16 0 16.79 45.04 -5 7 -6 12.69 32.34 -11 -15 0 3.28 41.35 -4 8 -6 23.75 31.53 -11 -17 1 -4.50 49.54 -3 9 -6 7.78 35.62 -4 6 -5 10.65 25.38 -8 -8 -1 0.00 19.65 -10 -16 1 9.42 44.63 -3 7 -5 7.37 25.79 -3 5 -4 36.44 19.24 -7 -9 0 13.51 21.29 -3 3 -3 32.75 13.92 -6 -8 0 77.38 22.11 -2 2 -2 45.45 9.42 -7 -17 3 1.64 47.90 -4 -10 2 1.64 28.25 4 14 -4 7.37 42.17 -3 -11 3 4.09 31.12 5 15 -4 1.23 45.86 -2 -10 3 4.50 29.07 6 16 -4 9.01 50.77 5 13 -3 12.69 36.03 6 14 -3 29.89 42.99 -1 -11 4 143.30 34.39 7 15 -3 11.87 46.67 6 12 -2 33.57 32.75 0 -10 4 53.23 34.80 8 16 -3 1.23 44.22 7 13 -2 5.73 37.26 0 -12 5 -5.73 38.49 8 14 -2 2.05 36.03 7 11 -1 20.47 29.89 1 -11 5 -5.32 34.80 8 12 -1 15.15 32.75 4 -2 3 20.06 11.46 9 13 -1 3.28 32.75 8 10 0 60.19 27.02 2 -12 6 9.42 42.99 9 11 0 21.70 29.07 3 -11 6 11.46 40.53 9 9 1 10.24 25.79 10 10 1 27.02 25.79 7 -3 5 8.19 19.65 11 9 2 2.05 24.16 12 8 3 13.10 23.34 9 -3 6 19.65 24.16 13 9 3 -1.23 25.38 14 8 4 -5.32 26.61 16 8 5 0.00 27.84 -11 1 -7 -2.05 22.52 -15 -15 -2 7.37 43.81 -14 -16 -1 5.73 45.04 -10 -6 -3 1.23 17.20 -13 -17 0 2.05 45.04 -9 -7 -2 8.19 18.01 -9 -9 -1 6.96 23.75 -2 10 -6 8.60 37.67 -8 -10 0 47.90 26.20 -1 11 -6 14.33 41.76 -2 8 -5 6.55 27.43 0 12 -6 -8.19 43.40 -1 9 -5 8.60 29.89 -2 6 -4 9.83 20.47 1 13 -6 -2.05 47.90 0 10 -5 -2.05 32.34 -1 7 -4 16.38 22.52 -2 4 -3 18.01 14.74 -1 5 -3 29.48 16.38 -1 3 -2 51.59 10.65 -5 -13 3 10.65 36.03 -4 -12 3 2.46 33.16 -4 -14 4 -15.97 40.94 -3 -13 4 7.37 37.67 -2 -12 4 70.42 34.39 -3 -15 5 -0.82 47.49 -2 -14 5 9.42 42.17 2 -2 2 35.62 8.60 -1 -13 5 2.46 40.53 9 17 -3 2.05 49.13 3 -3 3 24.97 12.28 9 15 -2 11.87 39.30 1 -13 6 -14.33 45.45 10 16 -2 4.91 42.99 4 -4 4 -3.28 16.38 11 17 -2 17.61 51.18 10 14 -1 10.65 35.62 5 -3 4 44.63 15.97 11 15 -1 20.06 42.99 10 12 0 24.97 29.89 12 16 -1 7.37 47.08 11 13 0 6.96 33.98 6 -4 5 5.73 19.24 13 17 -1 29.89 49.54 12 14 0 0.00 36.03 11 11 1 70.01 30.30 13 15 0 13.10 41.76 12 12 1 3.68 30.30 7 -5 6 1.23 24.97 14 16 0 18.01 46.27 13 13 1 9.01 34.80 12 10 2 22.93 27.02 8 -4 6 12.69 22.93 14 14 1 0.41 36.85 13 11 2 1.23 30.30 15 15 1 -6.96 45.45 14 12 2 6.14 31.94 9 -5 7 16.38 29.89 15 13 2 6.14 36.03 14 10 3 2.46 27.84 10 -4 7 7.78 27.02 15 11 3 2.46 30.30 16 12 3 1.64 36.44 15 9 4 3.68 28.66 16 10 4 3.28 30.71 17 11 4 -8.60 33.98 -10 2 -7 8.19 22.52 -9 3 -7 2.05 24.97 -10 0 -6 3.68 8.19 -11 -5 -4 1.23 15.97 -11 -7 -3 16.79 20.47 -11 -9 -2 10.65 24.16 -10 -8 -2 11.05 20.47 -11 -11 -1 52.41 31.94 -10 -10 -1 25.38 26.20 -11 -13 0 15.15 33.16 -10 -12 0 25.79 31.94 -9 -11 0 24.97 29.07 -10 -14 1 24.57 36.85 -9 -13 1 9.01 36.44 -8 -16 3 9.42 45.04 1 11 -5 25.79 38.08 0 8 -4 54.86 26.61 -7 -15 3 11.87 44.63 2 12 -5 13.10 38.90 1 9 -4 35.21 27.43 0 6 -3 34.39 19.24 -6 -14 3 20.88 37.26 3 13 -5 6.55 41.35 2 10 -4 25.79 30.30 1 7 -3 29.07 20.47 0 4 -2 350.88 18.01 -6 -16 4 -0.82 49.95 4 14 -5 4.09 45.45 3 11 -4 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29.07 15 -13 -5 3.28 34.80 32 -2 -6 3.68 36.44 31 -3 -6 0.41 32.75 30 -4 -6 -1.23 28.25 29 -5 -6 -1.23 22.52 28 -6 -6 -0.41 15.56 -30 6 6 0.00 19.24 -31 5 6 -8.19 23.75 -26 4 5 4.50 17.20 -27 3 5 0.00 22.11 -22 2 4 -2.05 16.79 -23 1 4 1.64 20.06 -17 1 3 6.14 14.33 -18 0 3 0.00 17.61 -30 -10 3 -1.23 54.45 -12 0 2 222.32 14.33 -25 -11 2 20.88 50.77 -26 -12 2 -3.28 55.68 -6 0 1 2.05 6.55 -19 -11 1 20.88 45.86 -20 -12 1 1.23 49.13 -21 -13 1 -3.68 54.45 -22 -14 1 7.37 57.73 -14 -12 0 4.91 43.40 -15 -13 0 0.00 47.90 -16 -14 0 0.82 51.59 -17 -15 0 -10.24 56.09 8 2 -1 6.96 11.46 7 1 -1 2.05 7.78 -8 -12 -1 4.09 37.26 -9 -13 -1 6.14 40.94 -10 -14 -1 0.82 46.67 -11 -15 -1 -1.64 50.36 25 13 -2 17.20 60.19 24 12 -2 20.06 53.63 23 11 -2 33.57 49.54 22 10 -2 9.83 52.41 21 9 -2 6.14 45.45 20 8 -2 5.73 41.35 19 7 -2 20.06 36.85 18 6 -2 11.46 28.25 17 5 -2 14.33 24.16 16 4 -2 3.28 20.88 15 3 -2 72.88 18.83 14 2 -2 22.93 18.01 -2 -12 -2 63.46 35.21 -3 -13 -2 -1.64 37.26 -4 -14 -2 5.32 41.35 28 10 -3 2.46 52.82 27 9 -3 8.60 46.27 26 8 -3 -1.23 42.17 25 7 -3 4.50 37.67 24 6 -3 3.68 33.98 23 5 -3 2.87 30.30 22 4 -3 -1.64 32.75 21 3 -3 -4.91 28.66 4 -12 -3 4.09 35.62 3 -13 -3 -1.23 32.75 2 -14 -3 14.74 43.40 31 7 -4 0.00 52.41 11 -11 -4 4.50 27.43 10 -12 -4 0.00 32.34 18 -10 -5 7.37 22.93 -29 7 6 -1.23 10.65 -25 5 5 2.46 12.28 -21 3 4 10.65 15.15 -31 -5 4 9.83 64.28 -32 -6 4 8.19 48.72 1 17 3 8.60 53.63 0 16 3 4.09 76.97 -1 15 3 13.92 72.88 -16 2 3 4.50 13.51 -26 -6 3 8.60 68.37 -27 -7 3 12.69 50.77 -28 -8 3 0.00 52.00 -29 -9 3 12.69 57.73 7 17 2 6.96 59.37 6 16 2 14.74 55.27 5 15 2 16.79 53.63 -11 1 2 7.37 11.46 -22 -8 2 6.14 46.67 -23 -9 2 0.82 51.18 -24 -10 2 18.83 55.27 12 16 1 5.32 61.82 11 15 1 -4.09 54.86 10 14 1 -7.37 53.23 -17 -9 1 44.22 47.08 -18 -10 1 4.09 52.41 17 15 0 20.47 62.64 16 14 0 -11.46 58.14 -11 -9 0 6.55 40.94 -12 -10 0 367.26 52.41 -13 -11 0 259.17 48.72 6 0 -1 0.41 6.55 -6 -10 -1 23.75 41.35 -7 -11 -1 233.37 45.45 13 1 -2 4.91 15.97 12 0 -2 351.29 25.79 0 -10 -2 26.20 35.21 -1 -11 -2 53.63 38.90 -9 -17 -2 -1.64 59.37 20 2 -3 9.01 24.16 19 1 -3 -5.32 27.02 6 -10 -3 83.11 39.71 5 -11 -3 11.87 31.53 -3 -17 -3 15.97 83.52 30 6 -4 -4.09 47.08 29 5 -4 11.46 42.58 28 4 -4 4.91 38.49 27 3 -4 4.09 45.45 26 2 -4 -3.68 38.08 12 -10 -4 6.55 28.25 33 3 -5 -12.28 56.91 19 -9 -5 4.50 30.30 -13 15 5 5.73 80.66 -34 -2 5 -3.28 79.84 -6 16 4 14.74 60.60 -7 15 4 2.87 59.78 -8 14 4 2.05 145.76 -9 13 4 33.16 167.86 -20 4 4 5.32 8.60 -29 -3 4 31.94 183.01 -30 -4 4 -0.82 61.00 -2 14 3 37.67 67.56 -3 13 3 6.14 86.80 -4 12 3 1.23 184.24 -24 -4 3 18.42 161.31 -25 -5 3 -7.78 81.48 4 14 2 20.06 74.11 3 13 2 18.42 84.75 2 12 2 108.50 85.16 1 11 2 85.57 94.99 -20 -6 2 20.06 85.16 -21 -7 2 11.05 68.37 -27 -11 2 45.86 284.55 9 13 1 -32.75 128.56 8 12 1 3.68 93.76 7 11 1 574.42 109.73 6 10 1 29.07 89.25 -15 -7 1 16.79 78.20 -16 -8 1 23.75 69.19 -22 -12 1 6.55 124.47 -23 -13 1 9.83 115.46 -9 -7 0 9.83 74.11 -10 -8 0 29.07 80.25 -17 -13 0 32.34 115.05 -18 -14 0 18.83 120.78 -19 -15 0 7.78 112.59 -4 -8 -1 14.74 70.42 -5 -9 -1 66.74 70.01 -12 -14 -1 -4.50 111.36 -13 -15 -1 -10.24 108.09 -14 -16 -1 11.05 106.86 26 12 -2 -9.42 113.82 25 11 -2 -7.78 116.28 24 10 -2 79.02 112.59 23 9 -2 -24.97 97.03 1 -9 -2 10.65 62.23 -7 -15 -2 22.52 105.22 -8 -16 -2 -26.20 117.51 30 10 -3 -18.42 108.09 18 0 -3 -2.05 28.25 7 -9 -3 1.23 72.47 -1 -15 -3 -38.08 252.62 -2 -16 -3 2.05 101.13 25 1 -4 1.23 36.44 24 0 -4 11.87 56.09 13 -9 -4 -1.64 59.78 4 -16 -4 0.00 90.48 32 2 -5 2.46 50.36 31 1 -5 19.65 67.96 30 0 -5 17.61 62.64 -14 14 5 -3.68 207.58 -15 13 5 0.82 123.65 -24 6 5 0.41 5.73 -32 0 5 -8.60 214.54 -33 -1 5 -14.74 126.51 -10 12 4 -5.32 241.97 -28 -2 4 -38.08 252.62 -5 11 3 17.20 156.40 -6 10 3 171.55 136.34 -15 3 3 14.74 6.96 -23 -3 3 -15.15 118.73 -30 -8 3 -14.33 280.87 -31 -9 3 12.28 292.33 9 17 2 -33.57 134.29 0 10 2 20.88 173.19 -1 9 2 83.93 213.72 -18 -4 2 90.07 220.68 -19 -5 2 125.28 205.12 -25 -9 2 -72.47 323.04 -26 -10 2 122.01 331.64 14 16 1 46.27 348.42 5 9 1 151.90 268.58 4 8 1 4.91 241.97 -13 -5 1 73.70 232.96 -14 -6 1 40.53 257.53 -20 -10 1 62.23 334.91 -21 -11 1 39.71 328.36 -15 -11 0 44.22 335.73 -16 -12 0 -70.83 354.56 16 8 -1 -21.70 302.57 15 7 -1 10.65 284.96 -3 -7 -1 27.84 212.90 -10 -12 -1 345.15 311.16 -11 -13 -1 84.34 324.67 22 8 -2 -18.83 306.66 21 7 -2 -30.30 289.87 20 6 -2 -10.65 174.82 11 -1 -2 12.28 32.75 2 -8 -2 968.70 151.49 -5 -13 -2 -2.05 318.94 -6 -14 -2 -9.01 318.53 29 9 -3 -23.34 231.33 28 8 -3 23.34 295.61 27 7 -3 43.40 287.83 26 6 -3 17.20 126.10 17 -1 -3 18.01 88.03 8 -8 -3 76.97 174.82 0 -14 -3 1.23 286.19 32 6 -4 -34.39 142.89 23 -1 -4 26.20 121.19 6 -14 -4 -2.46 124.47 5 -15 -4 -9.01 179.74 29 -1 -5 -23.75 142.48 12 -14 -5 -9.01 112.18 11 -15 -5 6.14 154.35 -16 12 5 6.96 32.75 -31 1 5 -4.09 29.89 -11 11 4 18.42 47.90 -26 0 4 10.24 27.43 -27 -1 4 -6.55 93.35 -33 -5 4 -2.46 45.04 3 17 3 3.68 54.45 2 16 3 -1.23 51.18 1 15 3 0.82 36.44 -7 9 3 24.97 23.75 -22 -2 3 -11.87 82.29 -29 -7 3 2.05 46.27 8 16 2 -9.01 56.50 7 15 2 4.91 63.87 6 14 2 -5.73 53.63 -2 8 2 219.45 43.40 -10 2 2 41.35 11.87 -17 -3 2 21.29 39.30 -23 -7 2 6.14 36.44 -24 -8 2 2.87 49.54 -29 -11 2 -2.46 40.12 13 15 1 2.87 68.37 12 14 1 -2.87 63.87 11 13 1 6.55 49.95 3 7 1 17.61 35.21 -5 1 1 237.47 13.92 -12 -4 1 126.92 34.39 -19 -9 1 4.50 65.10 -25 -13 1 -2.87 55.27 -14 -10 0 45.86 60.60 -20 -14 0 -3.28 57.32 22 12 -1 0.00 61.41 14 6 -1 13.92 42.99 13 5 -1 22.93 39.71 -2 -6 -1 22.11 33.57 -9 -11 -1 7.37 65.92 -15 -15 -1 2.05 59.78 -16 -16 -1 -0.41 63.05 27 11 -2 -2.46 58.14 19 5 -2 9.83 46.67 3 -7 -2 -2.46 88.03 -4 -12 -2 91.30 71.24 -10 -16 -2 7.78 66.74 25 5 -3 -38.49 111.77 24 4 -3 2.46 29.07 16 -2 -3 7.37 31.94 1 -13 -3 31.53 137.16 -4 -16 -3 6.14 41.76 -5 -17 -3 11.46 48.31 31 5 -4 -30.30 124.87 22 -2 -4 10.24 115.87 14 -8 -4 116.69 104.40 7 -13 -4 6.96 116.28 28 -2 -5 -7.78 55.27 13 -13 -5 -6.96 54.45 -32 -4 4 4.50 31.53 -3 -11 -2 5.32 43.40 23 3 -3 4.91 25.79 27 -3 -5 1.23 17.20 5 -1 -1 154.76 20.47 20 -8 -5 36.44 47.08 10 -2 -2 -6.14 16.38 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 31957 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, 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 O7A O -0.0005(8) 0.348(2) 0.428(4) 0.091(13) Uani 0.56(5) 1 d . . . A 1 H7A H -0.008601 0.301295 0.474777 0.137 Uiso 0.5(2) 1 calc R U . A 1 O7B O 0.0011(16) 0.427(4) 0.449(7) 0.046(9) Uani 0.23(3) 1 d . U P A 2 H7B H 0.007913 0.481038 0.461229 0.069 Uiso 0.23(3) 1 calc R U P A 2 O6 O 0.0447(6) 0.3803(9) 0.731(3) 0.074(6) Uani 0.81(4) 1 d . . . A . N1 N 0.1477(3) 0.2833(5) 0.1598(14) 0.030(2) Uani 1 1 d . . . . . O4 O 0.1390(3) 0.5472(5) 0.6433(13) 0.032(2) Uani 1 1 d . U . . . H4 H 0.141364 0.601554 0.665738 0.08(2) Uiso 1 1 calc R . . . . C6 C 0.1583(4) 0.0012(5) 0.1973(16) 0.036(3) Uani 1 1 d . U . . . O1 O 0.1207(4) -0.0402(4) 0.0854(14) 0.044(3) Uani 1 1 d . . . . . C3 C 0.1557(4) 0.1010(5) 0.1876(15) 0.029(2) Uani 1 1 d . U . . . C10 C 0.1761(4) 0.5076(5) 0.7695(16) 0.037(3) Uani 1 1 d . . . . . C7 C 0.1361(4) 0.3548(5) 0.6394(15) 0.033(3) Uani 1 1 d . . . . . C8 C 0.1740(4) 0.4063(5) 0.7605(15) 0.035(3) Uani 1 1 d . U . . . H8 H 0.202145 0.376056 0.848784 0.042(14) Uiso 1 1 calc R . . . . O5 O 0.2132(3) 0.5411(5) 0.8857(14) 0.036(2) Uani 1 1 d . . . . . C9 C 0.1466(4) 0.2542(5) 0.6690(15) 0.031(2) Uani 1 1 d . . . . . O3 O 0.1879(3) 0.2271(4) 0.7704(15) 0.041(3) Uani 1 1 d . . . . . C2 C 0.1099(4) 0.1409(5) 0.0743(16) 0.046(3) Uani 1 1 d . U . . . H2A H 0.081333 0.106502 0.003181 0.16(4) Uiso 1 1 calc R . . . . N2 N 0.1981(4) -0.0363(5) 0.3183(15) 0.045(3) Uani 1 1 d . . . . . H2B H 0.199925 -0.093988 0.325628 0.057(16) Uiso 1 1 calc R . . . . H2C H 0.223210 -0.003978 0.393093 0.056(18) Uiso 1 1 calc R . . . . C5 C 0.1907(4) 0.2469(5) 0.2598(17) 0.044(3) Uani 1 1 d . . . . . H5 H 0.218704 0.284039 0.322523 0.11(3) Uiso 1 1 calc R . . . . C4 C 0.1979(4) 0.1550(5) 0.2800(17) 0.042(3) Uani 1 1 d . . . . . H4A H 0.229829 0.130512 0.352890 0.055(16) Uiso 1 1 calc R . . . . C1 C 0.1079(4) 0.2309(5) 0.0702(16) 0.051(3) Uani 1 1 d . . . . . H1 H 0.076522 0.257984 -0.000145 0.10(2) Uiso 1 1 calc R . . . . C11 C 0.0885(4) 0.3818(6) 0.4893(19) 0.047(3) Uani 1 1 d . . . . . H11A H 0.082032 0.342371 0.373413 0.15(4) Uiso 1 1 calc R . . . . H11B H 0.092878 0.442053 0.444958 0.15(4) Uiso 1 1 calc R . . . . C12 C 0.0416(6) 0.3808(10) 0.557(3) 0.088(5) Uani 1 1 d . . . . . O2 O 0.1083(3) 0.2080(5) 0.5677(14) 0.042(3) Uani 1 1 d . U . . . H2 H 0.116637 0.154752 0.572511 0.056(17) Uiso 1 1 calc R . . . . O12 O 0.000000 -0.112(2) -0.250000 0.16(2) Uiso 0.59(5) 2 d DS . P B 3 N3 N 0.0026(10) -0.042(2) -0.167(3) 0.09(2) Uiso 0.29(3) 1 d D . P B 3 O11 O 0.000000 0.029(3) -0.250000 0.23(3) Uiso 0.59(5) 2 d DS . P B 3 C17 C 0.010(3) -0.043(2) 0.048(3) 0.15(3) Uiso 0.29(3) 1 d D . P B 3 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 O7A 0.042(11) 0.15(3) 0.085(16) 0.030(15) 0.018(10) -0.002(12) O7B 0.042(10) 0.050(13) 0.046(12) -0.005(9) 0.017(8) -0.003(8) O6 0.070(12) 0.079(11) 0.071(10) 0.027(9) 0.020(9) 0.021(7) N1 0.041(5) 0.018(4) 0.036(6) 0.003(4) 0.021(4) -0.001(3) O4 0.043(5) 0.005(4) 0.044(5) -0.003(3) 0.008(4) -0.004(3) C6 0.050(6) 0.008(4) 0.051(6) 0.002(4) 0.017(4) 0.004(3) O1 0.071(6) 0.006(4) 0.049(7) -0.003(4) 0.009(5) 0.006(3) C3 0.042(5) 0.012(4) 0.033(6) 0.004(3) 0.013(4) -0.009(3) C10 0.046(6) 0.006(4) 0.052(7) -0.003(4) 0.006(5) 0.001(3) C7 0.035(5) 0.016(4) 0.050(8) -0.005(4) 0.016(5) 0.004(3) C8 0.046(4) 0.012(3) 0.044(5) 0.001(3) 0.008(4) 0.001(3) O5 0.043(5) 0.021(4) 0.044(6) -0.007(4) 0.017(4) -0.006(4) C9 0.041(5) 0.015(4) 0.035(7) 0.005(4) 0.011(4) 0.004(3) O3 0.040(5) 0.013(4) 0.064(7) -0.003(4) 0.008(4) -0.005(3) C2 0.043(5) 0.014(4) 0.064(7) 0.006(4) -0.005(5) 0.004(4) N2 0.045(6) 0.006(4) 0.079(8) -0.003(4) 0.015(5) -0.001(4) C5 0.044(5) 0.008(4) 0.072(9) -0.009(5) 0.007(5) -0.002(4) C4 0.032(6) 0.013(4) 0.079(9) 0.000(5) 0.014(5) 0.000(4) C1 0.054(6) 0.011(4) 0.072(9) 0.005(5) -0.001(6) 0.009(4) C11 0.043(6) 0.015(5) 0.074(9) 0.011(5) 0.008(5) -0.002(4) C12 0.037(7) 0.154(13) 0.071(10) 0.025(9) 0.014(7) 0.017(7) O2 0.050(5) 0.011(4) 0.056(6) 0.005(4) 0.006(4) 0.004(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 '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 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0000 0.0000 '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 C12 O7A H7A 109.5 . . C12 O7B H7B 109.5 . . C5 N1 C1 118.5(8) . . C10 O4 H4 109.5 . . O1 C6 C3 117.0(9) . . O1 C6 N2 123.9(9) . . N2 C6 C3 119.1(9) . . C2 C3 C6 118.5(8) . . C2 C3 C4 118.8(8) . . C4 C3 C6 122.7(9) . . O4 C10 C8 115.5(9) . . O5 C10 O4 126.8(9) . . O5 C10 C8 117.6(9) . . C8 C7 C9 113.7(9) . . C8 C7 C11 129.0(8) . . C11 C7 C9 117.4(8) . . C10 C8 H8 116.3 . . C7 C8 C10 127.4(10) . . C7 C8 H8 116.3 . . O3 C9 C7 120.9(9) . . O3 C9 O2 127.1(9) . . O2 C9 C7 111.9(8) . . C3 C2 H2A 121.1 . . C1 C2 C3 117.7(9) . . C1 C2 H2A 121.1 . . C6 N2 H2B 120.0 . . C6 N2 H2C 120.0 . . H2B N2 H2C 120.0 . . N1 C5 H5 118.3 . . N1 C5 C4 123.5(9) . . C4 C5 H5 118.3 . . C3 C4 C5 117.4(9) . . C3 C4 H4A 121.3 . . C5 C4 H4A 121.3 . . N1 C1 C2 124.0(10) . . N1 C1 H1 118.0 . . C2 C1 H1 118.0 . . C7 C11 H11A 108.5 . . C7 C11 H11B 108.5 . . C7 C11 C12 115.3(10) . . H11A C11 H11B 107.5 . . C12 C11 H11A 108.5 . . C12 C11 H11B 108.5 . . O7A C12 C11 115.7(17) . . O7B C12 C11 117(2) . . O6 C12 O7A 117(2) . . O6 C12 O7B 111(2) . . O6 C12 C11 122.5(16) . . C9 O2 H2 109.5 . . N3 O12 N3 57(2) 2_554 . O12 N3 O11 123.8(19) . . O12 N3 C17 117.7(18) . . N3 N3 O12 61.7(10) 2_554 . N3 N3 O11 62.1(10) 2_554 . N3 N3 C17 179(2) 2_554 . O11 N3 C17 118.5(18) . . N3 O11 C17 124(3) . 6 N3 O11 C17 71(3) 2_554 6 C17 O11 C17 165(5) 5 6 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 O7A H7A 0.8400 . O7A C12 1.33(3) . O7B H7B 0.8400 . O7B C12 1.34(5) . O6 C12 1.216(19) . N1 C5 1.302(12) . N1 C1 1.348(12) . O4 H4 0.8400 . O4 C10 1.281(12) . C6 O1 1.260(12) . C6 C3 1.520(11) . C6 N2 1.295(13) . C3 C2 1.407(13) . C3 C4 1.409(12) . C10 C8 1.542(11) . C10 O5 1.208(12) . C7 C8 1.372(13) . C7 C9 1.560(11) . C7 C11 1.466(14) . C8 H8 0.9500 . C9 O3 1.216(12) . C9 O2 1.288(12) . C2 H2A 0.9500 . C2 C1 1.369(11) . N2 H2B 0.8800 . N2 H2C 0.8800 . C5 H5 0.9500 . C5 C4 1.412(11) . C4 H4A 0.9500 . C1 H1 0.9500 . C11 H11A 0.9900 . C11 H11B 0.9900 . C11 C12 1.542(18) . O2 H2 0.8400 . O12 N3 1.211(17) 2_554 O12 N3 1.211(17) . N3 N3 1.15(4) 2_554 N3 O11 1.226(17) . N3 C17 1.487(17) . N3 C17 1.64(6) 5 O11 C17 1.56(2) 6 O11 C17 1.56(2) 5 C17 C17 1.49(7) 5 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 N1 C5 C4 C3 -0.7(16) . . . . O4 C10 C8 C7 -3.1(15) . . . . C6 C3 C2 C1 178.8(10) . . . . C6 C3 C4 C5 179.8(9) . . . . O1 C6 C3 C2 7.5(14) . . . . O1 C6 C3 C4 -169.6(11) . . . . C3 C2 C1 N1 3.4(17) . . . . C7 C11 C12 O7A -137(2) . . . . C7 C11 C12 O7B 162(3) . . . . C7 C11 C12 O6 18(2) . . . . C8 C7 C9 O3 -9.7(14) . . . . C8 C7 C9 O2 173.6(9) . . . . C8 C7 C11 C12 -98.1(13) . . . . O5 C10 C8 C7 -179.4(10) . . . . C9 C7 C8 C10 179.6(9) . . . . C9 C7 C11 C12 82.4(12) . . . . C2 C3 C4 C5 2.8(15) . . . . N2 C6 C3 C2 -172.2(10) . . . . N2 C6 C3 C4 10.7(15) . . . . C5 N1 C1 C2 -1.3(17) . . . . C4 C3 C2 C1 -4.0(16) . . . . C1 N1 C5 C4 -0.1(16) . . . . C11 C7 C8 C10 0.1(17) . . . . C11 C7 C9 O3 169.9(11) . . . . C11 C7 C9 O2 -6.9(13) . . . . O12 N3 O11 N3 0.005(2) . . . 2_554 O12 N3 O11 C17 163(5) . . . 5 O12 N3 O11 C17 -20(5) . . . 6 O12 N3 C17 N3 -162(5) . . . 5 O12 N3 C17 O11 -117(11) . . . 5 O12 N3 C17 C17 -162(5) . . . 5 N3 O12 N3 O11 -0.005(4) 2_554 . . . N3 O12 N3 C17 114(10) 2_554 . . 5 N3 O12 N3 C17 -180(3) 2_554 . . . N3 N3 O11 C17 -20(5) 2_554 . . 6 N3 N3 O11 C17 163(5) 2_554 . . 5 O11 N3 C17 N3 19(5) . . . 5 O11 N3 C17 O11 64(11) . . . 5 O11 N3 C17 C17 19(5) . . . 5 C17 N3 O11 N3 180(3) . . . 2_554 C17 N3 O11 N3 -163(5) 5 . . 2_554 C17 N3 O11 C17 160(5) . . . 6 C17 N3 O11 C17 177.5(10) 5 . . 6 C17 N3 O11 C17 -17(5) . . . 5 C17 N3 C17 N3 0.000(4) 5 . . 5 C17 N3 C17 O11 45(8) 5 . . 5 loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code _cod_related_entry_description 1 XRDA 00264 DOI:10.51093/xrd-00264