#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:00:03 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293750 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571927.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_1571927 loop_ _publ_author_name 'Biswas, Soumen' 'Empel, Claire' 'Sanchez-Palestino, Luis Mario' 'Arman, Hadi' 'Koenigs, Rene M.' 'Doyle, Michael P.' _publ_section_title ; Denitrogenative dismantling of heteroaromatics by nucleophilic substitution reactions with diazomethyl compounds. ; _journal_issue 28 _journal_name_full 'Chemical science' _journal_page_first 11065 _journal_page_last 11071 _journal_paper_doi 10.1039/d4sc01578a _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C20 H17 N5 O4' _chemical_formula_sum 'C20 H17 N5 O4' _chemical_formula_weight 391.39 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2023-07-20 _audit_creation_method ; Olex2 1.5 (compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748) ; _audit_update_record ; 2023-07-29 deposited with the CCDC. 2024-06-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.256(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.4348(2) _cell_length_b 9.9373(2) _cell_length_c 18.8362(3) _cell_measurement_reflns_used 8976 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 75.4380 _cell_measurement_theta_min 4.5540 _cell_volume 1927.76(6) _computing_cell_refinement 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _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 293(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.973 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 33.00 71.00 0.50 1.45 -- 106.29 -61.00 60.00 76 2 \w 33.00 71.00 0.50 1.45 -- 106.29 -61.00 150.00 76 3 \w 92.00 178.00 0.50 1.45 -- 106.29 45.00 90.00 172 4 \w 90.00 178.00 0.50 1.45 -- 106.29 59.00 172.00 176 5 \w 30.00 120.00 0.50 0.36 -- 46.90 59.00 172.00 180 6 \w 33.00 68.00 0.50 1.45 -- 106.29 -59.00 32.00 70 7 \w 33.00 65.00 0.50 1.45 -- 106.29 -61.00 0.00 64 8 \w -25.00 64.00 0.50 0.36 -- 46.90 -59.00 32.00 178 9 \w 35.00 61.00 0.50 1.45 -- 106.29 -61.00-180.00 52 10 \w 33.00 105.00 0.50 1.45 -- 106.29 -94.00 -30.00 144 11 \w -63.00 26.00 0.50 0.36 -- -46.90 59.00 172.00 178 12 \w -68.00 -19.00 0.50 1.45 -- -91.75 59.00 172.00 98 13 \w -71.00 -19.00 0.50 1.45 -- -91.75 61.00 120.00 104 14 \w -71.00 -19.00 0.50 1.45 -- -91.75 61.00 30.00 104 15 \w -51.00 -19.00 0.50 1.45 -- -91.75 45.00 30.00 64 16 \w -51.00 -19.00 0.50 1.45 -- -91.75 45.00 0.00 64 17 \w -51.00 -19.00 0.50 1.45 -- -91.75 45.00 -60.00 64 18 \w -51.00 -19.00 0.50 1.45 -- -91.75 45.00 -90.00 64 19 \w -51.00 -19.00 0.50 1.45 -- -91.75 45.00 150.00 64 20 \w -164.00 -91.00 0.50 1.45 -- -91.75 -61.00 120.00 146 21 \w -164.00-100.00 0.50 1.45 -- -91.75 -94.00 150.00 128 22 \w -164.00 -75.00 0.50 1.45 -- -91.75 -59.00 32.00 178 23 \w -119.00 -30.00 0.50 0.36 -- -46.90 -59.00 32.00 178 24 \w -119.00 -87.00 0.50 0.36 -- -46.90-125.00-150.00 64 25 \w -119.00 -87.00 0.50 0.36 -- -46.90-125.00-180.00 64 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0856504000 _diffrn_orient_matrix_UB_12 -0.0240940000 _diffrn_orient_matrix_UB_13 -0.0734819000 _diffrn_orient_matrix_UB_21 0.0793563000 _diffrn_orient_matrix_UB_22 0.1052097000 _diffrn_orient_matrix_UB_23 -0.0344811000 _diffrn_orient_matrix_UB_31 0.0935328000 _diffrn_orient_matrix_UB_32 -0.1112539000 _diffrn_orient_matrix_UB_33 -0.0166933000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_unetI/netI 0.0353 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18614 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.362 _diffrn_reflns_theta_min 4.561 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.470 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear dark yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.349 _exptl_crystal_description plate _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.233 _exptl_crystal_size_mid 0.135 _exptl_crystal_size_min 0.082 _refine_diff_density_max 0.341 _refine_diff_density_min -0.222 _refine_diff_density_rms 0.039 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 275 _refine_ls_number_reflns 3713 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0464 _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^)+(0.0519P)^2^+0.7248P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1182 _refine_ls_wR_factor_ref 0.1231 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3170 _reflns_number_total 3713 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc01578a2.cif _cod_data_source_block hpd630b2 _cod_depositor_comments 'Adding full bibliography for 1571926--1571927.cif.' _cod_database_code 1571927 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H N O' _chemical_oxdiff_usercomment 'SB2-104B try 2' _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_max 0.937 _shelx_estimated_absorpt_t_min 0.834 _reflns_odcompleteness_completeness 99.92 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances N5-O1B 1.2 with sigma of 0.02 3. Others Fixed Sof: O1A(0.85) O1B(0.15) 4.a Ternary CH refined with riding coordinates: C4(H4) 4.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B) 4.c Aromatic/amide H refined with riding coordinates: C20(H20), C9(H9), C13(H13), C16(H16), C12(H12), C11(H11), C10(H10), C19(H19), C18(H18), C17(H17) 4.d Idealised Me refined as rotating group: C7(H7A,H7B,H7C) ; _shelx_res_file ; TITL hpd630b2_a.res in P2(1)/n hpd630b2.res created by SHELXL-2018/3 at 15:45:15 on 20-Jul-2023 REM Old TITL HPD630B2 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.157, Rweak 0.205, Alpha 0.027 REM 0.745 for 238 systematic absences, Orientation as input REM Formula found by SHELXT: C21 N4 O4 CELL 1.54184 10.4348 9.9373 18.8362 90 99.256 90 ZERR 4 0.0002 0.0002 0.0003 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O UNIT 80 68 20 16 DFIX 1.2 N5 O1B L.S. 9 PLAN 5 SIZE 0.082 0.135 0.233 CONF BOND list 4 MORE -1 BOND $H fmap 2 53 acta OMIT -3 145 OMIT 0 1 6 REM REM REM WGHT 0.051900 0.724800 FVAR 0.58084 O3 4 0.041236 0.531578 0.177357 11.00000 0.07473 0.04518 = 0.04428 0.00186 -0.01308 -0.00171 O4 4 0.552217 0.650050 0.463969 11.00000 0.06142 0.06238 = 0.04373 -0.00935 0.00528 -0.01137 O2 4 0.088969 0.319550 0.213765 11.00000 0.06620 0.04042 = 0.05387 -0.00633 -0.00041 -0.00334 N1 3 0.245292 0.644300 0.368810 11.00000 0.04799 0.03078 = 0.04159 -0.00545 0.00382 0.00143 N2 3 0.174374 0.625824 0.300758 11.00000 0.04441 0.03442 = 0.04170 0.00222 0.00427 -0.00107 N3 3 0.343591 0.333100 0.327769 11.00000 0.04669 0.03544 = 0.05177 -0.00818 0.00649 0.00080 N4 3 0.456278 0.404900 0.336591 11.00000 0.04432 0.04146 = 0.04782 -0.00274 0.00494 0.00193 C1 1 0.169109 0.499104 0.289214 11.00000 0.04011 0.03354 = 0.03700 0.00332 0.00728 -0.00194 C4 1 0.312747 0.521709 0.397630 11.00000 0.04501 0.03405 = 0.03367 -0.00014 0.00566 -0.00033 AFIX 13 H4 2 0.312379 0.508764 0.449174 11.00000 -1.20000 AFIX 0 C2 1 0.237703 0.410587 0.349945 11.00000 0.04438 0.02958 = 0.03623 0.00011 0.00555 0.00134 C3 1 0.446148 0.508114 0.376635 11.00000 0.04282 0.03813 = 0.03649 0.00100 0.00348 0.00111 C14 1 0.555507 0.597302 0.405606 11.00000 0.04420 0.04001 = 0.03945 0.00295 -0.00037 0.00182 C5 1 0.095646 0.438882 0.222351 11.00000 0.04495 0.03833 = 0.04013 0.00116 0.00585 -0.00187 C8 1 0.140777 0.328166 0.383421 11.00000 0.04960 0.03781 = 0.03881 0.00507 0.00280 -0.00426 C15 1 0.661344 0.627177 0.364007 11.00000 0.04080 0.04371 = 0.05096 0.00320 0.00415 0.00343 C20 1 0.772606 0.690397 0.399258 11.00000 0.04625 0.05954 = 0.06834 0.00125 0.00148 -0.00154 AFIX 43 H20 2 0.783234 0.703769 0.448724 11.00000 -1.20000 AFIX 0 C9 1 0.154171 0.192053 0.394304 11.00000 0.07169 0.03992 = 0.06785 0.00769 0.01506 -0.00277 AFIX 43 H9 2 0.224968 0.146744 0.381431 11.00000 -1.20000 AFIX 0 C13 1 0.034554 0.392692 0.403633 11.00000 0.06362 0.05209 = 0.07536 0.01489 0.02704 0.00501 AFIX 43 H13 2 0.024338 0.484896 0.396375 11.00000 -1.20000 AFIX 0 C16 1 0.648140 0.607583 0.290372 11.00000 0.05661 0.09024 = 0.05671 -0.00083 0.01304 -0.00900 AFIX 43 H16 2 0.574943 0.564465 0.266002 11.00000 -1.20000 AFIX 0 C6 1 -0.040755 0.481938 0.112159 11.00000 0.09289 0.06649 = 0.05071 -0.00569 -0.02133 -0.00378 AFIX 23 H6A 2 0.008912 0.423135 0.085729 11.00000 -1.20000 H6B 2 -0.113515 0.431477 0.124664 11.00000 -1.20000 AFIX 0 C12 1 -0.056353 0.321887 0.434414 11.00000 0.06563 0.08305 = 0.08512 0.02045 0.02989 -0.00020 AFIX 43 H12 2 -0.126941 0.366600 0.447916 11.00000 -1.20000 AFIX 0 C11 1 -0.042898 0.187525 0.444970 11.00000 0.07022 0.07809 = 0.07528 0.01741 0.01815 -0.02068 AFIX 43 H11 2 -0.104035 0.140061 0.465852 11.00000 -1.20000 AFIX 0 C10 1 0.060225 0.121908 0.424988 11.00000 0.10388 0.04456 = 0.08390 0.01628 0.02102 -0.01578 AFIX 43 H10 2 0.068383 0.029418 0.431793 11.00000 -1.20000 AFIX 0 C19 1 0.867059 0.733236 0.361106 11.00000 0.04572 0.07438 = 0.10831 0.00542 0.01338 -0.00720 AFIX 43 H19 2 0.941386 0.774979 0.385084 11.00000 -1.20000 AFIX 0 C18 1 0.852580 0.714978 0.288368 11.00000 0.05836 0.09493 = 0.10796 0.02075 0.03615 0.00030 AFIX 43 H18 2 0.916298 0.745075 0.262871 11.00000 -1.20000 AFIX 0 C17 1 0.743819 0.652159 0.253171 11.00000 0.07602 0.12770 = 0.06986 0.00714 0.03050 -0.00828 AFIX 43 H17 2 0.734251 0.639360 0.203690 11.00000 -1.20000 AFIX 0 C7 1 -0.087443 0.598718 0.068277 11.00000 0.09638 0.09535 = 0.05692 0.00612 -0.01486 0.01349 AFIX 137 H7A 2 -0.144639 0.569340 0.026041 11.00000 -1.50000 H7B 2 -0.014921 0.645525 0.054358 11.00000 -1.50000 H7C 2 -0.133426 0.657965 0.095619 11.00000 -1.50000 AFIX 0 PART 1 H3 2 0.335921 0.282242 0.289412 11.00000 -1.20000 PART 0 N5 3 0.250013 0.759549 0.405009 11.00000 0.07104 0.04086 = 0.07919 -0.01317 0.02486 0.00013 O1A 4 0.193298 0.852627 0.373887 10.85000 0.07191 0.04068 = 0.09653 -0.00985 0.01068 0.01204 O1B 4 0.275764 0.772728 0.459703 10.15000 0.11032 0.08929 = 0.04296 -0.03718 0.01222 0.00791 HKLF 4 REM hpd630b2_a.res in P2(1)/n REM wR2 = 0.1231, GooF = S = 1.025, Restrained GooF = 1.035 for all data REM R1 = 0.0464 for 3170 Fo > 4sig(Fo) and 0.0534 for all 3713 data REM 275 parameters refined using 1 restraints END WGHT 0.0559 0.6893 REM Highest difference peak 0.341, deepest hole -0.222, 1-sigma level 0.039 Q1 1 -0.1450 0.5195 0.0940 11.00000 0.05 0.34 Q2 1 0.0204 0.5215 0.0867 11.00000 0.05 0.18 Q3 1 0.1284 0.7131 0.2943 11.00000 0.05 0.15 Q4 1 0.1144 0.0673 0.3993 11.00000 0.05 0.15 Q5 1 0.2013 0.1462 0.3501 11.00000 0.05 0.13 ; _shelx_res_checksum 64862 _shelx_hkl_file ; 0 0 1 0.16 0.15 0 0 2 1213.47 67.18 0 0 -3 0.53 0.65 0 0 3 0.25 0.63 0 0 -4 9879.60 548.43 0 0 4 9999.00 548.49 0 0 5 -0.45 1.11 0 0 6 1879.99 107.70 0 0 -6 1983.49 107.53 0 0 7 0.17 1.17 0 0 -7 -0.13 0.79 0 0 8 6.82 1.65 0 0 -8 6.74 1.20 0 0 9 0.91 1.59 0 0 -9 0.70 1.08 0 0 10 472.22 27.63 0 0 -10 415.38 28.50 0 0 -10 483.30 27.28 0 0 10 477.91 26.47 0 0 -11 0.51 2.10 0 0 11 0.89 1.49 0 0 -11 -1.14 1.35 0 0 11 -0.23 0.75 0 0 -12 552.77 30.40 0 0 -12 525.78 29.21 0 0 -12 525.58 30.61 0 0 12 513.47 30.80 0 0 -12 483.19 31.72 0 0 12 515.54 29.35 0 0 -13 -0.66 1.41 0 0 13 0.29 0.84 0 0 -13 2.23 2.29 0 0 13 -1.84 1.78 0 0 -13 -0.43 0.63 0 0 -14 14.88 2.53 0 0 -14 14.23 1.36 0 0 14 17.97 2.88 0 0 14 15.70 1.64 0 0 15 -1.27 1.98 0 0 15 -0.22 1.04 0 0 -15 0.77 1.45 0 0 -15 0.17 0.71 0 0 -16 46.36 3.23 0 0 -16 48.00 4.66 0 0 16 51.68 5.08 0 0 16 49.34 3.43 0 0 -17 -1.20 1.82 0 0 -17 -0.55 0.77 0 0 17 -0.44 2.04 0 0 17 0.57 1.07 0 0 -18 41.80 2.92 0 0 18 43.17 3.11 0 0 19 -0.40 0.87 0 0 -19 -0.83 0.76 0 0 20 0.17 0.75 0 0 -20 -0.29 0.67 0 0 -20 -0.41 0.47 0 0 21 -0.57 0.64 0 0 -21 -0.04 0.36 0 0 -21 0.84 0.60 0 0 -22 0.99 0.44 0 0 -22 2.04 0.50 0 0 22 1.79 0.58 0 0 -23 -0.93 0.35 0 -1 0 0.66 0.54 0 -1 0 0.49 0.90 0 -1 1 1443.15 76.36 0 -1 1 1469.96 77.13 0 1 1 1491.82 76.37 0 -1 -1 1415.87 77.07 0 -1 -1 1374.05 76.34 0 1 -1 1263.09 76.32 0 1 2 559.93 30.05 0 -1 2 548.71 30.04 0 -1 -2 518.32 31.07 0 -1 2 552.72 30.47 0 -1 -2 535.00 29.99 0 1 -2 522.73 29.98 0 -1 -3 1768.22 106.52 0 1 3 1938.06 105.48 0 -1 3 1864.63 105.47 0 1 -3 1944.61 105.39 0 -1 -3 1902.69 105.39 0 -1 4 1012.73 56.28 0 1 4 990.09 56.28 0 -1 -4 985.25 57.34 0 -1 -4 1029.28 56.17 0 1 -4 1013.79 56.16 0 -1 5 11.14 1.46 0 1 5 10.63 1.49 0 1 -5 10.95 1.25 0 -1 -5 11.32 1.23 0 -1 -6 23.79 2.95 0 1 6 17.92 2.09 0 -1 6 21.85 2.16 0 1 -6 22.34 1.91 0 -1 -6 23.91 1.95 0 1 7 254.96 15.13 0 -1 -7 263.52 15.87 0 -1 7 263.27 15.16 0 1 -7 253.87 14.91 0 -1 -7 251.09 14.90 0 -1 8 613.44 36.53 0 1 8 621.85 36.53 0 1 -8 680.43 36.33 0 1 9 151.78 9.68 0 -1 9 142.86 9.61 0 -1 -9 134.34 10.97 0 1 -9 158.62 9.35 0 1 -10 1963.35 103.42 0 -1 10 1841.62 102.57 0 1 10 1840.91 102.58 0 1 10 1878.20 103.77 0 -1 -10 1750.25 105.45 0 -1 10 1817.24 103.72 0 1 -11 42.83 3.57 0 -1 11 46.01 2.79 0 -1 -11 31.29 4.96 0 1 -11 26.94 3.93 0 -1 11 43.13 3.97 0 1 11 39.38 3.90 0 1 11 38.99 2.78 0 -1 11 41.74 2.80 0 -1 12 7.07 1.07 0 1 12 5.36 1.04 0 -1 12 4.00 1.84 0 -1 -12 4.67 3.05 0 1 12 4.01 1.94 0 1 -12 6.67 1.69 0 1 -12 7.19 0.85 0 -1 -12 5.71 0.82 0 1 -12 3.88 1.46 0 -1 -12 5.68 1.65 0 1 -13 46.59 2.84 0 -1 -13 41.54 2.80 0 -1 13 42.10 4.25 0 1 13 42.59 4.33 0 -1 -13 42.53 5.61 0 1 13 39.97 2.99 0 -1 13 39.65 2.97 0 1 -13 41.48 4.04 0 -1 -13 42.58 4.08 0 -1 -14 26.40 2.05 0 1 -14 26.92 2.07 0 1 14 23.81 3.50 0 -1 14 32.20 2.33 0 -1 14 26.50 3.59 0 1 14 30.67 2.31 0 -1 -14 24.26 3.36 0 1 -14 33.95 3.55 0 -1 -14 20.44 4.25 0 1 -15 1.14 1.84 0 -1 -15 1.15 1.48 0 -1 -15 1.98 0.85 0 1 -15 2.74 0.87 0 1 15 1.67 2.02 0 -1 15 2.93 1.07 0 1 15 3.61 1.09 0 -1 15 0.42 2.04 0 1 -16 75.11 4.81 0 -1 -16 78.47 4.84 0 1 16 82.11 5.04 0 -1 16 80.45 5.03 0 1 -16 85.53 6.56 0 -1 -16 73.08 6.38 0 1 16 66.05 6.41 0 -1 16 62.79 6.30 0 1 -17 114.46 6.71 0 1 17 113.14 6.86 0 -1 17 112.65 6.85 0 -1 -17 100.76 8.15 0 1 -17 101.73 8.17 0 -1 17 106.94 8.41 0 1 17 108.22 8.50 0 1 -18 53.83 3.64 0 -1 18 57.62 3.83 0 1 18 56.83 3.85 0 1 -19 19.84 1.46 0 -1 19 24.55 1.91 0 1 19 18.77 1.79 0 1 -19 19.24 1.67 0 1 20 40.15 2.81 0 -1 20 40.13 2.79 0 -1 -20 38.37 2.68 0 1 -20 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19.46 2.38 11 1 3 22.47 1.83 11 1 3 16.70 1.51 11 -1 3 23.47 1.86 11 1 4 57.66 3.99 11 -1 4 56.07 4.47 11 1 4 66.06 4.04 11 -1 4 63.07 4.02 11 1 5 1.65 0.79 11 -1 5 2.39 0.74 11 -1 5 2.19 1.57 11 1 5 2.34 0.76 11 1 6 0.99 0.67 11 -1 6 0.17 0.59 11 -1 6 0.62 1.32 11 1 6 0.41 0.61 11 -1 7 -0.14 1.25 11 1 7 0.29 0.56 11 -1 7 0.22 0.56 -11 -1 -7 0.25 0.56 -11 1 -7 1.77 0.59 -11 -1 -8 7.56 0.83 -11 1 -8 8.50 0.84 11 1 8 8.98 1.41 -11 -1 -9 0.06 0.37 -11 1 -9 -0.06 0.38 11 1 9 0.18 0.80 11 2 -15 7.54 0.73 11 2 -14 2.59 0.59 11 -2 -14 1.90 0.49 11 2 -13 24.63 1.74 11 -2 -13 20.67 1.66 11 2 -13 26.03 1.73 11 2 -12 6.12 0.89 11 -2 -12 6.20 0.90 11 -2 -12 5.92 0.81 11 2 -12 5.74 0.85 11 2 -11 1.78 0.75 11 -2 -11 1.22 0.72 11 -2 -11 2.42 0.69 11 2 -11 1.48 0.76 11 2 -10 0.80 0.78 11 -2 -10 0.18 0.78 11 -2 -10 -0.07 0.64 11 2 -10 0.26 0.75 -11 -2 9 3.84 1.49 11 2 -9 5.96 1.03 11 -2 -9 5.15 1.02 11 -2 -9 6.82 0.92 11 2 -9 7.28 1.11 -11 -2 8 5.21 1.72 11 -2 -8 5.45 1.12 11 2 -8 7.05 1.16 11 -2 -8 7.03 0.97 -11 -2 7 -0.19 1.73 11 -2 -7 0.12 0.99 11 2 -7 1.07 0.89 11 -2 -7 1.59 0.72 -11 -2 6 28.14 3.17 11 2 -6 30.54 2.49 11 -2 -6 31.97 2.28 11 2 -6 35.49 2.52 11 2 -5 0.81 0.96 11 -2 -5 1.43 1.03 11 2 -5 0.51 1.01 11 2 -5 2.40 0.89 11 -2 -5 0.76 0.64 11 2 -4 1.56 1.11 11 2 -4 0.94 0.99 11 2 -4 0.42 0.84 11 -2 -4 0.39 0.98 11 2 -4 0.26 1.01 11 -2 -3 54.31 3.79 11 2 -3 51.76 3.62 11 2 -3 57.24 3.83 11 2 -3 51.85 3.82 11 2 -2 0.97 1.04 11 2 -2 1.22 0.88 11 -2 -2 1.65 1.04 11 2 -2 1.13 1.03 11 -2 -1 9.64 1.35 11 2 -1 8.53 1.34 11 2 -1 9.63 1.41 11 2 0 3.53 1.06 11 -2 0 5.25 1.08 11 2 0 4.47 1.17 11 2 1 11.38 1.62 11 -2 1 14.65 2.02 11 2 1 19.99 1.71 11 -2 1 16.61 1.61 11 2 2 3.51 1.02 11 -2 2 5.93 1.10 11 -2 2 5.56 1.62 11 2 2 6.38 1.12 11 2 3 4.07 0.95 11 -2 3 4.22 0.94 11 -2 3 5.41 1.64 11 2 3 5.78 1.07 11 2 4 2.95 0.89 11 -2 4 3.08 0.85 11 -2 5 0.16 1.32 11 2 5 1.25 0.67 11 -2 5 1.27 0.72 11 -2 6 4.29 1.41 11 2 6 3.78 0.75 11 -2 6 2.47 0.70 11 -2 7 0.63 1.13 -11 -2 -7 0.38 0.51 -11 2 -7 0.93 0.51 -11 -2 -8 3.26 0.50 -11 2 -8 3.89 0.53 11 2 9 -0.45 0.69 11 3 -14 4.23 0.59 11 3 -13 0.37 0.50 11 3 -12 11.40 1.07 -11 -3 12 9.47 0.72 11 3 -11 1.50 0.65 11 3 -11 1.96 0.68 -11 -3 11 1.31 0.30 11 -3 -10 3.54 0.60 11 3 -10 4.83 0.85 11 3 -10 4.39 0.81 -11 -3 10 2.92 0.41 11 3 -9 2.67 0.80 11 3 -9 3.59 0.86 -11 -3 9 2.51 1.53 11 3 -8 1.98 1.07 11 3 -8 1.51 0.86 11 3 -8 1.61 0.80 -11 -3 8 -0.51 1.53 11 3 -7 2.96 1.10 11 3 -7 1.86 0.79 11 3 -7 1.59 0.85 -11 -3 7 1.11 1.76 11 3 -6 3.17 1.12 11 3 -6 2.31 0.87 11 3 -6 3.02 0.91 -11 -3 6 3.57 1.94 11 3 -5 1.89 0.86 -11 -3 5 2.08 1.85 11 3 -5 3.89 1.18 11 3 -4 2.02 1.06 11 -3 -4 3.60 1.04 11 3 -4 2.60 0.98 -11 -3 4 2.58 2.03 11 3 -3 2.55 1.05 -11 -3 3 1.98 1.94 11 -3 -3 1.27 0.94 11 3 -3 2.48 0.99 11 3 -3 2.95 0.94 11 3 -2 0.27 0.99 -11 -3 2 -1.33 2.00 11 -3 -2 0.34 0.88 11 3 -2 -0.22 0.87 11 -3 -1 17.20 1.71 11 3 -1 19.29 1.77 11 -3 0 0.86 0.88 11 3 0 -0.31 0.82 11 -3 1 1.21 1.14 11 3 1 -0.89 0.82 11 -3 1 0.10 0.82 11 -3 2 1.14 1.24 11 3 2 1.58 0.80 11 -3 2 0.57 0.75 11 -3 3 5.61 1.56 11 3 3 6.80 0.98 11 -3 3 7.83 1.05 11 3 4 13.82 1.42 11 -3 4 13.65 1.78 11 3 4 14.69 1.28 11 -3 4 11.90 1.27 11 -3 5 1.55 0.62 -11 -3 -5 1.61 1.33 11 3 6 5.12 0.83 11 -3 6 5.75 1.32 -11 -3 -6 3.98 0.61 -11 3 -6 4.39 0.60 11 -3 7 1.33 0.98 -11 -3 -7 1.23 0.36 -11 3 -7 1.46 0.39 11 -3 8 16.57 1.52 -11 -4 12 1.46 0.26 11 4 -12 2.17 0.49 -11 -4 11 0.15 0.25 11 4 -11 -0.10 0.45 11 4 -10 -0.06 0.57 -11 -4 10 -0.24 0.31 11 4 -10 0.46 0.53 11 4 -9 0.98 0.64 -11 -4 9 1.24 0.34 11 4 -9 1.40 0.63 -11 -4 8 -0.16 1.53 11 4 -8 0.15 0.67 -11 -4 8 1.10 0.34 11 4 -8 0.07 0.65 -11 -4 8 0.20 1.64 11 4 -7 2.59 0.99 11 4 -7 3.50 0.85 -11 -4 7 4.11 0.47 11 4 -7 3.45 0.78 -11 -4 7 4.19 1.68 -11 -4 7 5.25 2.21 11 4 -6 0.82 0.88 -11 -4 6 0.19 1.74 11 4 -6 1.62 0.75 11 4 -5 1.91 0.97 -11 -4 5 3.72 1.84 11 4 -5 0.97 0.77 11 4 -4 7.61 1.30 -11 -4 4 6.03 2.03 11 4 -4 7.75 1.08 11 4 -3 3.75 1.09 -11 -4 3 7.35 2.14 11 4 -3 5.34 0.99 11 4 -2 10.55 1.36 11 4 -1 -0.23 0.97 11 -4 -1 1.89 0.76 11 -4 0 0.41 0.70 11 4 0 0.34 0.88 -11 -4 0 2.51 1.74 11 -4 1 3.07 0.81 -11 -4 -1 7.67 1.92 11 4 1 6.30 1.11 -11 -4 -2 -0.84 1.56 11 -4 2 1.94 0.96 11 4 2 0.82 0.80 -11 -4 -3 1.49 1.45 11 4 3 1.24 0.80 11 -4 3 0.74 0.99 11 4 4 1.22 0.73 11 -4 4 1.76 0.92 -11 -4 -4 0.60 0.36 11 4 5 3.80 0.76 11 -4 5 3.67 0.96 11 -4 6 0.59 0.76 -11 -5 10 4.20 0.39 -11 -5 9 1.86 0.33 11 5 -8 0.76 0.55 -11 -5 8 1.01 0.30 -11 -5 8 1.59 1.31 -11 -5 7 2.69 1.48 11 5 -7 2.38 0.68 -11 -5 7 2.01 0.37 -11 -5 7 2.62 1.57 -11 -5 6 -1.13 1.62 11 5 -6 -0.37 0.75 11 5 -6 0.07 0.61 -11 -5 6 0.40 0.31 -11 -5 6 0.65 1.86 11 5 -5 -0.10 0.76 11 5 -5 -0.14 0.64 -11 -5 5 0.07 0.28 -11 -5 5 2.57 1.68 -11 -5 5 2.40 2.13 11 5 -4 1.34 0.66 -11 -5 4 1.58 1.60 -11 -5 4 1.28 2.20 11 5 -4 0.20 0.81 11 5 -3 0.30 0.63 -11 -5 3 -1.85 2.13 11 5 -3 -0.60 0.84 11 5 -2 3.94 0.79 11 5 -2 4.74 0.99 -11 -5 2 5.85 2.42 11 5 -1 25.96 2.04 -11 -5 1 24.58 2.72 11 5 0 12.66 1.30 -11 -5 0 12.16 2.03 -11 -5 0 7.67 2.40 11 5 1 2.94 0.84 -11 -5 -1 5.10 1.66 -11 -5 -1 4.31 1.97 11 5 2 3.49 0.81 12 0 -12 1.63 0.55 12 0 -9 1.00 0.55 12 0 -8 0.81 0.56 12 0 -7 -0.06 0.57 12 0 -6 0.40 0.59 12 0 -5 1.69 0.81 12 0 -5 0.79 0.60 12 0 -4 14.49 1.46 12 0 -4 14.47 1.29 12 0 -4 17.92 1.61 12 0 -3 0.55 0.73 12 0 -3 0.18 0.57 12 0 -3 1.34 0.86 12 0 -2 16.02 1.32 12 0 -2 16.79 1.54 12 0 -1 0.17 0.67 12 0 -1 -0.39 0.78 12 0 0 2.42 0.72 12 0 0 1.52 0.84 12 0 1 -0.09 0.74 12 0 1 0.29 0.85 12 0 2 26.74 1.87 12 0 2 19.47 1.92 12 0 3 0.30 0.94 12 0 3 0.98 0.61 12 0 4 1.02 0.87 -12 0 -5 -0.21 0.41 -12 0 -6 0.43 0.34 12 1 -12 3.94 0.63 12 1 -11 1.30 0.60 12 1 -10 6.10 0.75 12 1 -10 4.09 0.79 12 1 -9 1.64 0.59 12 1 -9 0.45 0.70 12 1 -8 0.52 0.56 12 1 -8 0.40 0.79 12 1 -7 0.07 0.61 12 1 -6 0.89 0.80 -12 -1 6 -1.14 1.21 12 1 -6 0.42 0.62 12 1 -5 2.11 0.84 -12 -1 5 0.84 1.39 12 1 -5 2.13 0.66 12 1 -4 8.56 1.17 12 1 -4 8.65 0.98 12 -1 -4 8.67 1.19 12 1 -3 -0.10 0.76 12 1 -3 1.30 0.65 12 -1 -3 0.80 0.82 12 1 -3 1.00 0.85 12 1 -2 1.84 0.82 12 1 -2 3.28 0.69 12 1 -2 3.13 0.89 12 1 -1 1.59 0.81 12 1 -1 -0.06 0.54 12 -1 -1 0.19 0.75 12 1 -1 -0.57 0.76 12 1 0 0.88 0.72 12 -1 0 0.09 0.72 12 1 0 0.27 0.71 12 1 1 -0.33 0.66 12 -1 1 0.52 0.70 12 1 1 -0.86 0.69 12 -1 1 0.42 0.76 12 -1 2 2.01 0.73 12 1 2 2.71 0.76 12 -1 2 1.60 0.83 12 -1 3 14.84 1.52 12 1 3 16.41 1.66 12 -1 3 17.11 1.41 12 1 3 17.39 1.41 12 -1 4 0.33 0.79 12 1 4 1.84 0.88 12 1 5 3.06 0.87 -12 -1 -5 4.68 0.55 -12 1 -5 2.62 0.50 12 2 -12 6.51 0.67 12 2 -11 1.51 0.53 12 2 -10 4.78 0.76 12 2 -9 4.81 0.80 12 2 -8 6.36 0.83 12 2 -7 2.87 0.71 -12 -2 6 1.04 1.34 12 2 -6 1.36 0.81 12 2 -6 1.59 0.65 -12 -2 5 -0.14 1.38 12 2 -5 -0.30 0.79 12 2 -5 -0.28 0.61 -12 -2 4 2.98 1.50 12 2 -4 3.78 0.94 12 2 -4 5.06 0.80 12 -2 -3 0.91 0.80 12 2 -3 0.99 0.81 12 2 -3 0.83 0.61 12 -2 -2 6.80 1.02 12 2 -2 6.56 1.00 -12 -2 2 4.53 1.64 12 2 -2 6.00 1.01 12 2 -2 5.84 0.85 12 -2 -1 0.35 0.70 12 2 -1 -0.08 0.73 12 2 -1 0.56 0.73 12 2 -1 -0.19 0.56 12 -2 0 1.57 0.70 12 2 0 -0.08 0.65 -12 -2 0 1.51 1.41 12 2 0 0.27 0.69 12 2 0 0.23 0.52 12 -2 1 11.92 1.19 12 2 1 13.19 1.27 12 2 1 11.44 1.17 -12 -2 -2 4.06 1.38 -12 -2 -4 1.61 0.45 -12 2 -4 1.46 0.41 12 3 -6 3.77 0.85 -12 -3 6 3.10 1.39 12 3 -5 3.02 0.69 -12 -3 5 1.61 1.29 12 3 -4 6.89 0.87 -12 -3 4 5.76 1.51 12 3 -3 0.96 0.57 -12 -3 3 3.60 1.46 12 3 -2 5.30 0.78 -12 -3 2 4.62 1.52 12 3 -1 0.24 0.52 -12 -3 1 -0.28 1.37 12 3 0 13.29 1.29 0 0 0 0.00 0.00 TITL HPD630B2 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 1.54184 10.434788 9.937295 18.836188 90.0000 99.2560 90.0000 ZERR 36.00 0.000176 0.000164 0.000267 0.0000 0.0015 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 36.00 36.00 36.00 36.00 SIZE 0.08 0.14 0.23 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 85308 _olex2_exptl_crystal_mounting_method 'nylon loop' _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 3.461 _oxdiff_exptl_absorpt_empirical_full_min 0.380 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -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 O3 O 0.04124(14) 0.53158(13) 0.17736(6) 0.0572(4) Uani 1 1 d . . . . . O4 O 0.55222(13) 0.65005(14) 0.46397(6) 0.0562(3) Uani 1 1 d . . . . . O2 O 0.08897(13) 0.31955(13) 0.21377(7) 0.0546(3) Uani 1 1 d . . . . . N1 N 0.24529(13) 0.64430(13) 0.36881(7) 0.0405(3) Uani 1 1 d . . . . . N2 N 0.17437(13) 0.62582(13) 0.30076(7) 0.0405(3) Uani 1 1 d . . . . . N3 N 0.34359(14) 0.33310(14) 0.32777(8) 0.0448(3) Uani 1 1 d . . . . . N4 N 0.45628(14) 0.40490(14) 0.33659(7) 0.0448(3) Uani 1 1 d . . . . . C1 C 0.16911(15) 0.49910(15) 0.28921(8) 0.0368(3) Uani 1 1 d . . . . . C4 C 0.31275(15) 0.52171(15) 0.39763(8) 0.0377(3) Uani 1 1 d . . . . . H4 H 0.312379 0.508764 0.449174 0.045 Uiso 1 1 calc R U . . . C2 C 0.23770(15) 0.41059(15) 0.34995(8) 0.0368(3) Uani 1 1 d . . . . . C3 C 0.44615(15) 0.50811(16) 0.37663(8) 0.0395(4) Uani 1 1 d . . . . . C14 C 0.55551(16) 0.59730(17) 0.40561(8) 0.0420(4) Uani 1 1 d . . . . . C5 C 0.09565(16) 0.43888(17) 0.22235(8) 0.0412(4) Uani 1 1 d . . . . . C8 C 0.14078(17) 0.32817(17) 0.38342(8) 0.0425(4) Uani 1 1 d . . . . . C15 C 0.66134(16) 0.62718(18) 0.36401(9) 0.0455(4) Uani 1 1 d . . . . . C20 C 0.77261(18) 0.6904(2) 0.39926(12) 0.0589(5) Uani 1 1 d . . . . . H20 H 0.783234 0.703769 0.448724 0.071 Uiso 1 1 calc R U . . . C9 C 0.1542(2) 0.19205(19) 0.39430(11) 0.0594(5) Uani 1 1 d . . . . . H9 H 0.224968 0.146744 0.381431 0.071 Uiso 1 1 calc R U . . . C13 C 0.0346(2) 0.3927(2) 0.40363(12) 0.0619(5) Uani 1 1 d . . . . . H13 H 0.024338 0.484896 0.396375 0.074 Uiso 1 1 calc R U . . . C16 C 0.6481(2) 0.6076(3) 0.29037(11) 0.0674(6) Uani 1 1 d . . . . . H16 H 0.574943 0.564465 0.266002 0.081 Uiso 1 1 calc R U . . . C6 C -0.0408(3) 0.4819(2) 0.11216(11) 0.0737(6) Uani 1 1 d . . . . . H6A H 0.008912 0.423135 0.085729 0.088 Uiso 1 1 calc R U . . . H6B H -0.113515 0.431477 0.124664 0.088 Uiso 1 1 calc R U . . . C12 C -0.0564(2) 0.3219(3) 0.43441(14) 0.0760(7) Uani 1 1 d . . . . . H12 H -0.126941 0.366600 0.447916 0.091 Uiso 1 1 calc R U . . . C11 C -0.0429(2) 0.1875(3) 0.44497(13) 0.0738(6) Uani 1 1 d . . . . . H11 H -0.104035 0.140061 0.465852 0.089 Uiso 1 1 calc R U . . . C10 C 0.0602(3) 0.1219(2) 0.42499(14) 0.0768(7) Uani 1 1 d . . . . . H10 H 0.068383 0.029418 0.431793 0.092 Uiso 1 1 calc R U . . . C19 C 0.8671(2) 0.7332(3) 0.36111(16) 0.0760(7) Uani 1 1 d . . . . . H19 H 0.941386 0.774979 0.385084 0.091 Uiso 1 1 calc R U . . . C18 C 0.8526(2) 0.7150(3) 0.28837(17) 0.0846(8) Uani 1 1 d . . . . . H18 H 0.916298 0.745075 0.262871 0.101 Uiso 1 1 calc R U . . . C17 C 0.7438(3) 0.6522(3) 0.25317(15) 0.0891(8) Uani 1 1 d . . . . . H17 H 0.734251 0.639360 0.203690 0.107 Uiso 1 1 calc R U . . . C7 C -0.0874(3) 0.5987(3) 0.06828(13) 0.0859(8) Uani 1 1 d . . . . . H7A H -0.144639 0.569340 0.026041 0.129 Uiso 1 1 calc R U . . . H7B H -0.014921 0.645525 0.054358 0.129 Uiso 1 1 calc R U . . . H7C H -0.133426 0.657965 0.095619 0.129 Uiso 1 1 calc R U . . . H3 H 0.336(3) 0.282(3) 0.2894(17) 0.103 Uiso 1 1 d . U . A 1 N5 N 0.25001(18) 0.75955(17) 0.40501(11) 0.0623(5) Uani 1 1 d D . . . . O1A O 0.19330(18) 0.85263(17) 0.37389(11) 0.0700(5) Uani 0.85 1 d . . P . . O1B O 0.2758(12) 0.7727(12) 0.4597(5) 0.081(3) Uani 0.15 1 d D . P . . 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 O3 0.0747(9) 0.0452(7) 0.0443(6) 0.0019(5) -0.0131(6) -0.0017(6) O4 0.0614(8) 0.0624(8) 0.0437(7) -0.0093(6) 0.0053(6) -0.0114(6) O2 0.0662(8) 0.0404(7) 0.0539(7) -0.0063(5) -0.0004(6) -0.0033(6) N1 0.0480(8) 0.0308(7) 0.0416(7) -0.0054(5) 0.0038(6) 0.0014(6) N2 0.0444(7) 0.0344(7) 0.0417(7) 0.0022(5) 0.0043(6) -0.0011(6) N3 0.0467(8) 0.0354(7) 0.0518(8) -0.0082(6) 0.0065(6) 0.0008(6) N4 0.0443(8) 0.0415(8) 0.0478(7) -0.0027(6) 0.0049(6) 0.0019(6) C1 0.0401(8) 0.0335(8) 0.0370(7) 0.0033(6) 0.0073(6) -0.0019(6) C4 0.0450(8) 0.0341(8) 0.0337(7) -0.0001(6) 0.0057(6) -0.0003(7) C2 0.0444(8) 0.0296(8) 0.0362(7) 0.0001(6) 0.0056(6) 0.0013(6) C3 0.0428(8) 0.0381(8) 0.0365(7) 0.0010(6) 0.0035(6) 0.0011(7) C14 0.0442(9) 0.0400(9) 0.0395(8) 0.0030(7) -0.0004(6) 0.0018(7) C5 0.0450(9) 0.0383(9) 0.0401(8) 0.0012(6) 0.0059(6) -0.0019(7) C8 0.0496(9) 0.0378(9) 0.0388(8) 0.0051(6) 0.0028(7) -0.0043(7) C15 0.0408(9) 0.0437(9) 0.0510(9) 0.0032(7) 0.0041(7) 0.0034(7) C20 0.0462(10) 0.0595(12) 0.0683(12) 0.0012(10) 0.0015(9) -0.0015(9) C9 0.0717(13) 0.0399(10) 0.0678(12) 0.0077(9) 0.0151(10) -0.0028(9) C13 0.0636(12) 0.0521(11) 0.0754(13) 0.0149(10) 0.0270(10) 0.0050(9) C16 0.0566(12) 0.0902(17) 0.0567(11) -0.0008(11) 0.0130(9) -0.0090(11) C6 0.0929(16) 0.0665(14) 0.0507(11) -0.0057(10) -0.0213(10) -0.0038(12) C12 0.0656(14) 0.0830(17) 0.0851(16) 0.0204(13) 0.0299(12) -0.0002(12) C11 0.0702(14) 0.0781(16) 0.0753(14) 0.0174(12) 0.0181(11) -0.0207(12) C10 0.1039(19) 0.0446(12) 0.0839(15) 0.0163(10) 0.0210(14) -0.0158(12) C19 0.0457(11) 0.0744(15) 0.108(2) 0.0054(14) 0.0134(12) -0.0072(11) C18 0.0584(14) 0.0949(19) 0.108(2) 0.0207(16) 0.0361(14) 0.0003(13) C17 0.0760(16) 0.128(2) 0.0699(14) 0.0071(15) 0.0305(12) -0.0083(16) C7 0.0964(18) 0.0953(19) 0.0569(12) 0.0061(12) -0.0149(12) 0.0135(15) N5 0.0710(11) 0.0409(9) 0.0792(13) -0.0132(8) 0.0249(9) 0.0001(8) O1A 0.0719(11) 0.0407(9) 0.0965(13) -0.0098(8) 0.0107(10) 0.0120(8) O1B 0.110(9) 0.089(8) 0.043(5) -0.037(5) 0.012(5) 0.008(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 -5 -8 0.0927 -6 1 -4 0.0546 0 5 8 0.0542 6 -1 4 0.0228 6 -1 -8 0.0637 -5 0 9 0.0199 1 5 -6 0.0906 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 C5 O3 C6 115.93(15) . . ? N2 N1 C4 112.67(12) . . ? N5 N1 N2 123.97(15) . . ? N5 N1 C4 123.34(15) . . ? C1 N2 N1 106.86(13) . . ? N4 N3 C2 111.50(13) . . ? N4 N3 H3 111(2) . . ? C2 N3 H3 125(2) . . ? C3 N4 N3 109.76(14) . . ? N2 C1 C2 115.99(14) . . ? N2 C1 C5 122.81(14) . . ? C5 C1 C2 121.14(13) . . ? N1 C4 H4 113.4 . . ? N1 C4 C2 102.07(12) . . ? N1 C4 C3 112.60(13) . . ? C2 C4 H4 113.4 . . ? C3 C4 H4 113.4 . . ? C3 C4 C2 100.65(12) . . ? N3 C2 C1 111.97(12) . . ? N3 C2 C4 101.88(12) . . ? N3 C2 C8 114.83(13) . . ? C1 C2 C4 98.95(12) . . ? C8 C2 C1 111.06(13) . . ? C8 C2 C4 116.85(12) . . ? N4 C3 C4 112.95(14) . . ? N4 C3 C14 124.24(15) . . ? C14 C3 C4 122.55(14) . . ? O4 C14 C3 117.20(15) . . ? O4 C14 C15 121.32(16) . . ? C3 C14 C15 121.41(14) . . ? O3 C5 C1 111.89(14) . . ? O2 C5 O3 126.59(16) . . ? O2 C5 C1 121.51(15) . . ? C9 C8 C2 122.43(16) . . ? C9 C8 C13 118.81(17) . . ? C13 C8 C2 118.76(15) . . ? C20 C15 C14 118.25(16) . . ? C16 C15 C14 122.56(17) . . ? C16 C15 C20 118.83(18) . . ? C15 C20 H20 119.9 . . ? C19 C20 C15 120.2(2) . . ? C19 C20 H20 119.9 . . ? C8 C9 H9 120.3 . . ? C8 C9 C10 119.4(2) . . ? C10 C9 H9 120.3 . . ? C8 C13 H13 119.6 . . ? C12 C13 C8 120.9(2) . . ? C12 C13 H13 119.6 . . ? C15 C16 H16 120.0 . . ? C17 C16 C15 119.9(2) . . ? C17 C16 H16 120.0 . . ? O3 C6 H6A 110.2 . . ? O3 C6 H6B 110.2 . . ? H6A C6 H6B 108.5 . . ? C7 C6 O3 107.65(19) . . ? C7 C6 H6A 110.2 . . ? C7 C6 H6B 110.2 . . ? C13 C12 H12 119.9 . . ? C11 C12 C13 120.1(2) . . ? C11 C12 H12 119.9 . . ? C12 C11 H11 120.0 . . ? C12 C11 C10 120.0(2) . . ? C10 C11 H11 120.0 . . ? C9 C10 H10 119.6 . . ? C11 C10 C9 120.8(2) . . ? C11 C10 H10 119.6 . . ? C20 C19 H19 119.7 . . ? C18 C19 C20 120.6(2) . . ? C18 C19 H19 119.7 . . ? C19 C18 H18 120.2 . . ? C19 C18 C17 119.7(2) . . ? C17 C18 H18 120.2 . . ? C16 C17 H17 119.6 . . ? C18 C17 C16 120.7(2) . . ? C18 C17 H17 119.6 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O1A N5 N1 116.0(2) . . ? O1B N5 N1 127.2(7) . . ? O1B N5 O1A 114.8(7) . . ? 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 O3 C5 1.317(2) . ? O3 C6 1.465(2) . ? O4 C14 1.223(2) . ? O2 C5 1.197(2) . ? N1 N2 1.3854(18) . ? N1 C4 1.467(2) . ? N1 N5 1.330(2) . ? N2 C1 1.278(2) . ? N3 N4 1.363(2) . ? N3 C2 1.462(2) . ? N3 H3 0.87(3) . ? N4 C3 1.288(2) . ? C1 C2 1.527(2) . ? C1 C5 1.490(2) . ? C4 H4 0.9800 . ? C4 C2 1.553(2) . ? C4 C3 1.513(2) . ? C2 C8 1.515(2) . ? C3 C14 1.478(2) . ? C14 C15 1.483(2) . ? C8 C9 1.372(3) . ? C8 C13 1.386(3) . ? C15 C20 1.391(3) . ? C15 C16 1.385(3) . ? C20 H20 0.9300 . ? C20 C19 1.377(3) . ? C9 H9 0.9300 . ? C9 C10 1.401(3) . ? C13 H13 0.9300 . ? C13 C12 1.381(3) . ? C16 H16 0.9300 . ? C16 C17 1.382(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C7 1.462(3) . ? C12 H12 0.9300 . ? C12 C11 1.354(4) . ? C11 H11 0.9300 . ? C11 C10 1.362(4) . ? C10 H10 0.9300 . ? C19 H19 0.9300 . ? C19 C18 1.366(4) . ? C18 H18 0.9300 . ? C18 C17 1.369(4) . ? C17 H17 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? N5 O1A 1.199(2) . ? N5 O1B 1.030(9) . ? 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 O4 C14 C15 C20 15.1(3) . . . . ? O4 C14 C15 C16 -158.0(2) . . . . ? N1 N2 C1 C2 0.18(18) . . . . ? N1 N2 C1 C5 177.33(13) . . . . ? N1 C4 C2 N3 131.06(12) . . . . ? N1 C4 C2 C1 16.21(14) . . . . ? N1 C4 C2 C8 -102.97(15) . . . . ? N1 C4 C3 N4 -116.15(15) . . . . ? N1 C4 C3 C14 69.53(18) . . . . ? N2 N1 C4 C2 -18.75(16) . . . . ? N2 N1 C4 C3 88.33(15) . . . . ? N2 N1 N5 O1A -3.6(3) . . . . ? N2 N1 N5 O1B 159.5(9) . . . . ? N2 C1 C2 N3 -117.90(15) . . . . ? N2 C1 C2 C4 -11.15(17) . . . . ? N2 C1 C2 C8 112.26(16) . . . . ? N2 C1 C5 O3 1.5(2) . . . . ? N2 C1 C5 O2 -177.71(16) . . . . ? N3 N4 C3 C4 -3.13(19) . . . . ? N3 N4 C3 C14 171.07(14) . . . . ? N3 C2 C8 C9 2.2(2) . . . . ? N3 C2 C8 C13 -177.67(16) . . . . ? N4 N3 C2 C1 86.28(16) . . . . ? N4 N3 C2 C4 -18.58(16) . . . . ? N4 N3 C2 C8 -145.87(14) . . . . ? N4 C3 C14 O4 -148.57(17) . . . . ? N4 C3 C14 C15 34.5(2) . . . . ? C1 C2 C8 C9 130.50(17) . . . . ? C1 C2 C8 C13 -49.4(2) . . . . ? C4 N1 N2 C1 12.37(17) . . . . ? C4 N1 N5 O1A 177.83(17) . . . . ? C4 N1 N5 O1B -19.1(9) . . . . ? C4 C2 C8 C9 -117.05(18) . . . . ? C4 C2 C8 C13 63.1(2) . . . . ? C4 C3 C14 O4 25.1(2) . . . . ? C4 C3 C14 C15 -151.84(15) . . . . ? C2 N3 N4 C3 14.44(18) . . . . ? C2 C1 C5 O3 178.56(14) . . . . ? C2 C1 C5 O2 -0.7(2) . . . . ? C2 C4 C3 N4 -8.17(17) . . . . ? C2 C4 C3 C14 177.52(14) . . . . ? C2 C8 C9 C10 -179.46(18) . . . . ? C2 C8 C13 C12 -179.94(19) . . . . ? C3 C4 C2 N3 14.94(14) . . . . ? C3 C4 C2 C1 -99.90(13) . . . . ? C3 C4 C2 C8 140.92(13) . . . . ? C3 C14 C15 C20 -168.10(16) . . . . ? C3 C14 C15 C16 18.8(3) . . . . ? C14 C15 C20 C19 -172.90(19) . . . . ? C14 C15 C16 C17 172.2(2) . . . . ? C5 O3 C6 C7 -177.76(19) . . . . ? C5 C1 C2 N3 64.89(18) . . . . ? C5 C1 C2 C4 171.64(13) . . . . ? C5 C1 C2 C8 -64.95(18) . . . . ? C8 C9 C10 C11 -0.9(4) . . . . ? C8 C13 C12 C11 -0.3(4) . . . . ? C15 C20 C19 C18 0.3(4) . . . . ? C15 C16 C17 C18 0.5(4) . . . . ? C20 C15 C16 C17 -0.8(3) . . . . ? C20 C19 C18 C17 -0.7(4) . . . . ? C9 C8 C13 C12 0.2(3) . . . . ? C13 C8 C9 C10 0.4(3) . . . . ? C13 C12 C11 C10 -0.2(4) . . . . ? C16 C15 C20 C19 0.4(3) . . . . ? C6 O3 C5 O2 3.3(3) . . . . ? C6 O3 C5 C1 -175.89(16) . . . . ? C12 C11 C10 C9 0.8(4) . . . . ? C19 C18 C17 C16 0.3(5) . . . . ? N5 N1 N2 C1 -166.33(15) . . . . ? N5 N1 C4 C2 159.95(15) . . . . ? N5 N1 C4 C3 -92.97(18) . . . . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.7652 -4.7790 -8.2136 0.6532 -0.1589 0.7404 -5.8005 1.3297 -4.0265 0.7606 -0.1816 -0.6233 -0.2857 4.6297 8.4717 -0.7096 0.1723 -0.6832 5.7315 -1.0681 4.4456 -0.7918 0.1892 0.5807 5.5845 -0.9886 -8.1961 0.1478 0.6218 0.7691 -5.4689 0.0751 8.7064 -0.1732 -0.7263 -0.6652 1.4279 5.4273 -6.4211 0.2188 0.9057 -0.3631