#------------------------------------------------------------------------------ #$Date: 2023-11-18 01:40:34 +0200 (Sat, 18 Nov 2023) $ #$Revision: 287678 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247750.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_7247750 loop_ _publ_author_name 'Liu, Jian-Qiang' 'Duqingcuo, Li' 'Liu, Yichen' 'Xiang, Ruifang' 'Li, Yuyan' 'Qin, Tianrui' 'Dong, Xiuyan' 'Sakiyama, Hiroshi' 'Muddassir, Mohd.' _publ_section_title ; Synthesis, structural, and investigation of unique magnetic properties in two Mn-based coordination polymers ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE01060K _journal_year 2023 _chemical_formula_moiety 'C30 H18 Mn N4 O4' _chemical_formula_sum 'C30 H18 Mn N4 O4' _chemical_formula_weight 553.42 _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_Hall '-P 2yac' _space_group_name_H-M_alt 'P 1 2/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-07-25 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2023-10-23 deposited with the CCDC. 2023-11-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.461(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.9590(6) _cell_length_b 10.7872(8) _cell_length_c 29.582(2) _cell_measurement_reflns_used 9916 _cell_measurement_temperature 193.0 _cell_measurement_theta_max 59.611 _cell_measurement_theta_min 3.796 _cell_volume 2535.1(3) _computing_cell_refinement 'SAINT V8.40A (Bruker, 2019)' _computing_data_reduction 'SAINT V8.40A (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 193.0 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Bruker D8 VENTURE Metaljet PHOTON II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_unetI/netI 0.0456 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_number 24117 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.046 _diffrn_reflns_theta_min 3.795 _diffrn_source_current 2.86 _diffrn_source_power 0.1993706 _diffrn_source_voltage 69.71 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.146 _exptl_absorpt_correction_T_max 0.7518 _exptl_absorpt_correction_T_min 0.6221 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1036 before and 0.0710 after correction. The Ratio of minimum to maximum transmission is 0.8275. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 1.450 _exptl_crystal_description block _exptl_crystal_F_000 1132 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.264 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.048 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 398 _refine_ls_number_reflns 5632 _refine_ls_number_restraints 126 _refine_ls_restrained_S_all 1.026 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0360 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+0.7458P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.0943 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4562 _reflns_number_total 5632 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d3ce01060k2.cif _cod_data_source_block dongxy80 _cod_database_code 7247750 _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. ; _shelx_estimated_absorpt_t_max 0.744 _shelx_estimated_absorpt_t_min 0.704 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Uiso/Uaniso restraints and constraints C23A \\sim C22A \\sim N5 \\sim C21A \\sim C20A: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A Uanis(C23A) \\sim Ueq, Uanis(C22A) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(C21A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Rigid body (RIGU) restrains N3, C20, C23, C21, N4, C22, N5, C22A, C21A, C23A, C20A with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 4. Others Sof(N5)=Sof(C22A)=Sof(H22A)=Sof(C21A)=Sof(H21A)=Sof(C23A)=Sof(C20A)=1-FVAR(1) Sof(C20)=Sof(C23)=Sof(C21)=Sof(H21)=Sof(N4)=Sof(C22)=Sof(H22)=FVAR(1) 5.a Aromatic/amide H refined with riding coordinates: C15(H15), C18(H18), C19(H19), C16(H16), C26(H26), C28(H28), C29(H29), C1(H1), C12(H12), C9(H9), C3(H3), C25(H25), C2(H2), C8(H8), C11(H11), C10(H10), C21(H21), C22(H22), C22A(H22A), C21A(H21A) ; _shelx_res_file ; TITL a_a.res in P2/n a.res created by SHELXL-2018/3 at 13:05:54 on 25-Jul-2021 REM Old TITL A in P2/n REM SHELXT solution in P2/n: R1 0.109, Rweak 0.005, Alpha 0.037 REM 0.367 for 283 systematic absences, Orientation as input REM Formula found by SHELXT: C21A N3 O4 Mn CELL 1.34139 7.959 10.7872 29.5817 90 93.461 90 ZERR 4 0.0006 0.0008 0.0023 0 0.004 0 LATT 1 SYMM 0.5-X,+Y,0.5-Z SFAC C H Mn N O DISP C 0.0137 0.0067 57.1 DISP H 0 0 0.6 DISP Mn -0.0162 2.2332 17004.7 DISP N 0.0241 0.0134 109.9 DISP O 0.0389 0.0241 193.4 UNIT 120 72 4 16 16 RIGU 0.002 0.002 N3 C20 C23 C21 N4 C22 N5 C22A C21A C23A C20A SIMU 0.005 0.01 2 C23A C22A N5 C21A C20A ISOR 0.01 0.02 C23A C22A N5 C21A C20A L.S. 20 PLAN 1 SIZE 0.1 0.12 0.1 TEMP -80.15 CONF BOND list 4 fmap 2 MORE -1 HTAB BOND $H ACTA REM REM REM WGHT 0.040900 0.745800 FVAR 0.58934 0.87407 MN1 3 0.935689 0.114264 0.300447 11.00000 0.02843 0.02696 = 0.02202 0.00067 -0.00225 -0.00060 O3 5 0.683736 0.173710 0.298171 11.00000 0.03492 0.03865 = 0.03511 -0.00277 -0.00389 0.00949 O1 5 0.818625 0.915977 0.658172 11.00000 0.03285 0.05047 = 0.02674 -0.01120 -0.00200 0.00063 O4 5 0.485615 0.242459 0.248100 11.00000 0.04177 0.04134 = 0.02614 -0.00844 -0.00815 0.01101 O2 5 1.009237 0.792151 0.631776 11.00000 0.03354 0.04367 = 0.03407 -0.00715 -0.00847 0.00541 N1 4 0.990013 -0.057877 0.258352 11.00000 0.02508 0.03280 = 0.02488 -0.00047 -0.00021 0.00017 N3 4 0.444782 0.629529 0.450245 11.00000 0.02974 0.03799 = 0.02206 -0.00437 -0.00189 0.00233 N2 4 0.841496 -0.052759 0.337866 11.00000 0.02763 0.03262 = 0.02743 0.00154 0.00280 0.00097 C27 1 0.754937 0.823215 0.586370 11.00000 0.02951 0.03388 = 0.02258 -0.00017 -0.00027 -0.00245 C5 1 0.948993 -0.168142 0.277021 11.00000 0.02029 0.02935 = 0.02941 -0.00031 -0.00355 0.00201 C15 1 0.339764 0.380562 0.316594 11.00000 0.03028 0.03010 = 0.02269 -0.00072 -0.00377 -0.00131 AFIX 43 H15 2 0.268807 0.361254 0.290569 11.00000 -1.20000 AFIX 0 C14 1 0.499663 0.328840 0.321795 11.00000 0.02996 0.02358 = 0.02353 0.00168 -0.00184 -0.00167 C18 1 0.544824 0.435952 0.392844 11.00000 0.02795 0.03479 = 0.02498 -0.00299 -0.00527 -0.00248 AFIX 43 H18 2 0.615448 0.454608 0.418998 11.00000 -1.20000 AFIX 0 C6 1 0.871241 -0.165337 0.319872 11.00000 0.02191 0.02855 = 0.03053 0.00355 -0.00249 0.00024 C19 1 0.601147 0.355445 0.360841 11.00000 0.02770 0.02994 = 0.02809 -0.00034 -0.00423 -0.00024 AFIX 43 H19 2 0.708930 0.318048 0.365324 11.00000 -1.20000 AFIX 0 C17 1 0.386136 0.490369 0.387468 11.00000 0.02777 0.03541 = 0.02345 -0.00276 -0.00217 -0.00110 C30 1 0.868395 0.845978 0.627807 11.00000 0.03197 0.03399 = 0.02459 0.00051 0.00060 -0.00469 C13 1 0.561451 0.242607 0.286902 11.00000 0.02968 0.02620 = 0.02794 -0.00114 -0.00277 0.00001 C16 1 0.283443 0.459904 0.349065 11.00000 0.02751 0.03847 = 0.02604 -0.00124 -0.00323 0.00255 AFIX 43 H16 2 0.173559 0.494194 0.345253 11.00000 -1.20000 AFIX 0 C4 1 0.981252 -0.282979 0.256951 11.00000 0.02613 0.03455 = 0.03804 -0.00708 -0.00580 0.00393 C7 1 0.829779 -0.276533 0.341062 11.00000 0.02801 0.03437 = 0.04000 0.00863 -0.00344 -0.00152 C26 1 0.599801 0.880871 0.581210 11.00000 0.03914 0.04206 = 0.03159 -0.01364 -0.00449 0.00666 AFIX 43 H26 2 0.571251 0.943187 0.602105 11.00000 -1.20000 AFIX 0 C28 1 0.798682 0.737668 0.553851 11.00000 0.02731 0.04368 = 0.03035 -0.00558 -0.00012 0.00338 AFIX 43 H28 2 0.907938 0.701870 0.555643 11.00000 -1.20000 AFIX 0 PART 1 C20 1 0.326040 0.572118 0.423005 21.00000 0.03029 0.03914 = 0.02474 -0.00548 -0.00246 0.00205 PART 0 C29 1 0.683900 0.704473 0.518925 11.00000 0.03524 0.04646 = 0.02689 -0.01129 -0.00072 0.00589 AFIX 43 H29 2 0.714949 0.645344 0.497138 11.00000 -1.20000 AFIX 0 C1 1 1.065836 -0.060100 0.219443 11.00000 0.02862 0.04452 = 0.02777 0.00121 0.00255 0.00191 AFIX 43 H1 2 1.096302 0.016438 0.206321 11.00000 -1.20000 AFIX 0 C12 1 0.771050 -0.048149 0.377343 11.00000 0.03915 0.04149 = 0.03199 0.00130 0.00964 0.00063 AFIX 43 H12 2 0.749521 0.030749 0.390037 11.00000 -1.20000 AFIX 0 C24 1 0.524009 0.756399 0.515291 11.00000 0.03256 0.04263 = 0.02215 -0.00597 -0.00176 0.00407 C9 1 0.935691 -0.394737 0.279072 11.00000 0.03934 0.02845 = 0.05347 -0.00428 -0.00920 0.00308 AFIX 43 H9 2 0.956220 -0.472349 0.265265 11.00000 -1.20000 AFIX 0 C3 1 1.058938 -0.280696 0.215334 11.00000 0.03688 0.04513 = 0.04162 -0.01390 -0.00159 0.01018 AFIX 43 H3 2 1.080806 -0.355957 0.200080 11.00000 -1.20000 AFIX 0 C25 1 0.485450 0.848937 0.545961 11.00000 0.03585 0.04991 = 0.03450 -0.01195 -0.00781 0.01319 AFIX 43 H25 2 0.380066 0.890324 0.542648 11.00000 -1.20000 AFIX 0 C2 1 1.102554 -0.169885 0.197074 11.00000 0.03565 0.05544 = 0.03064 -0.00679 0.00432 0.00669 AFIX 43 H2 2 1.157329 -0.167504 0.169430 11.00000 -1.20000 AFIX 0 PART 1 C23 1 0.392054 0.701261 0.483055 21.00000 0.03352 0.04537 = 0.02561 -0.00943 -0.00341 0.00665 PART 0 C8 1 0.863691 -0.391860 0.319416 11.00000 0.03857 0.02931 = 0.05465 0.00848 -0.00499 -0.00173 AFIX 43 H8 2 0.835283 -0.467462 0.333552 11.00000 -1.20000 AFIX 0 C11 1 0.727241 -0.153740 0.401012 11.00000 0.04803 0.05558 = 0.03545 0.00745 0.01204 -0.00297 AFIX 43 H11 2 0.677214 -0.146524 0.429249 11.00000 -1.20000 AFIX 0 C10 1 0.756938 -0.267328 0.383214 11.00000 0.04328 0.04698 = 0.04280 0.01586 0.00420 -0.00511 AFIX 43 H10 2 0.728713 -0.340195 0.399121 11.00000 -1.20000 AFIX 0 PART 1 C21 1 0.155475 0.590779 0.429203 21.00000 0.03106 0.07178 = 0.04144 -0.02594 -0.00480 0.00226 AFIX 43 H21 2 0.074907 0.549706 0.409487 21.00000 -1.20000 AFIX 0 N4 4 0.100809 0.663450 0.461460 21.00000 0.03141 0.10353 = 0.06055 -0.04672 -0.00386 0.00805 C22 1 0.219729 0.718470 0.488246 21.00000 0.03609 0.08703 = 0.04818 -0.03813 -0.00201 0.00726 AFIX 43 H22 2 0.186144 0.771357 0.511743 21.00000 -1.20000 AFIX 0 PART 2 N5 4 0.149057 0.766088 0.433646 -21.00000 0.05057 0.05981 = 0.05237 -0.02131 -0.01816 0.01431 C22A 1 0.266209 0.805354 0.466048 -21.00000 0.04401 0.05301 = 0.04672 -0.01853 -0.01361 0.01345 AFIX 43 H22A 2 0.246926 0.879980 0.481982 -21.00000 -1.20000 AFIX 0 C21A 1 0.193046 0.672838 0.408054 -21.00000 0.04782 0.05596 = 0.04716 -0.01843 -0.02001 0.01136 AFIX 43 H21A 2 0.118691 0.649261 0.383210 -21.00000 -1.20000 AFIX 0 C23A 1 0.408904 0.740760 0.476030 -21.00000 0.04069 0.04755 = 0.04269 -0.01505 -0.00787 0.01103 C20A 1 0.339843 0.608397 0.415388 -21.00000 0.04682 0.05328 = 0.04155 -0.01499 -0.01889 0.00969 HKLF 4 REM a_a.res in P2/n REM wR2 = 0.0943, GooF = S = 1.032, Restrained GooF = 1.026 for all data REM R1 = 0.0360 for 4562 Fo > 4sig(Fo) and 0.0500 for all 5632 data REM 398 parameters refined using 126 restraints END WGHT 0.0409 0.7453 REM Instructions for potential hydrogen bonds EQIV $3 x+1/2, -y+1, z-1/2 HTAB C1 O1_$3 REM Highest difference peak 0.264, deepest hole -0.465, 1-sigma level 0.048 Q1 1 1.0721 0.1242 0.2829 11.00000 0.05 0.26 ; _shelx_res_checksum 4545 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, 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 Mn1 Mn 0.93569(3) 0.11426(2) 0.30045(2) 0.02596(9) Uani 1 1 d . . . . . O3 O 0.68374(16) 0.17371(12) 0.29817(4) 0.0365(3) Uani 1 1 d . . . . . O1 O 0.81862(16) 0.91598(13) 0.65817(4) 0.0368(3) Uani 1 1 d . . . . . O4 O 0.48562(16) 0.24246(12) 0.24810(4) 0.0368(3) Uani 1 1 d . . . . . O2 O 1.00924(16) 0.79215(12) 0.63178(4) 0.0375(3) Uani 1 1 d . . . . . N1 N 0.99001(17) -0.05788(14) 0.25835(5) 0.0277(3) Uani 1 1 d . . . . . N3 N 0.44478(19) 0.62953(14) 0.45025(5) 0.0301(3) Uani 1 1 d . . . . . N2 N 0.84150(18) -0.05276(14) 0.33787(5) 0.0292(3) Uani 1 1 d . . . . . C27 C 0.7549(2) 0.82321(16) 0.58637(6) 0.0287(4) Uani 1 1 d . . . . . C5 C 0.9490(2) -0.16814(16) 0.27702(6) 0.0266(4) Uani 1 1 d . . . . . C15 C 0.3398(2) 0.38056(15) 0.31659(6) 0.0279(4) Uani 1 1 d . . . . . H15 H 0.268807 0.361254 0.290569 0.033 Uiso 1 1 calc R U . . . C14 C 0.4997(2) 0.32884(15) 0.32179(5) 0.0258(4) Uani 1 1 d . . . . . C18 C 0.5448(2) 0.43595(17) 0.39284(6) 0.0295(4) Uani 1 1 d . . . . . H18 H 0.615448 0.454608 0.418998 0.035 Uiso 1 1 calc R U . . . C6 C 0.8712(2) -0.16534(16) 0.31987(6) 0.0272(4) Uani 1 1 d . . . . . C19 C 0.6011(2) 0.35545(16) 0.36084(6) 0.0288(4) Uani 1 1 d . . . . . H19 H 0.708930 0.318048 0.365324 0.035 Uiso 1 1 calc R U . . . C17 C 0.3861(2) 0.49037(16) 0.38747(5) 0.0290(4) Uani 1 1 d . . . . . C30 C 0.8684(2) 0.84598(17) 0.62781(6) 0.0302(4) Uani 1 1 d . . . . . C13 C 0.5615(2) 0.24261(16) 0.28690(6) 0.0281(4) Uani 1 1 d . . . . . C16 C 0.2834(2) 0.45990(17) 0.34907(6) 0.0309(4) Uani 1 1 d . . . . . H16 H 0.173559 0.494194 0.345253 0.037 Uiso 1 1 calc R U . . . C4 C 0.9813(2) -0.28298(17) 0.25695(6) 0.0332(4) Uani 1 1 d . . . . . C7 C 0.8298(2) -0.27653(17) 0.34106(6) 0.0344(4) Uani 1 1 d . . . . . C26 C 0.5998(3) 0.88087(18) 0.58121(6) 0.0379(5) Uani 1 1 d . . . . . H26 H 0.571251 0.943187 0.602105 0.045 Uiso 1 1 calc R U . . . C28 C 0.7987(2) 0.73767(18) 0.55385(6) 0.0339(4) Uani 1 1 d . . . . . H28 H 0.907938 0.701870 0.555643 0.041 Uiso 1 1 calc R U . . . C20 C 0.3260(4) 0.5721(3) 0.42300(10) 0.0316(6) Uani 0.874(3) 1 d . . P A 1 C29 C 0.6839(2) 0.70447(19) 0.51893(6) 0.0363(4) Uani 1 1 d . . . . . H29 H 0.714949 0.645344 0.497138 0.044 Uiso 1 1 calc R U . . . C1 C 1.0658(2) -0.06010(19) 0.21944(6) 0.0336(4) Uani 1 1 d . . . . . H1 H 1.096302 0.016438 0.206321 0.040 Uiso 1 1 calc R U . . . C12 C 0.7711(2) -0.04815(19) 0.37734(6) 0.0372(4) Uani 1 1 d . . . . . H12 H 0.749521 0.030749 0.390037 0.045 Uiso 1 1 calc R U . . . C24 C 0.5240(2) 0.75640(18) 0.51529(6) 0.0326(4) Uani 1 1 d . . . . . C9 C 0.9357(3) -0.39474(17) 0.27907(8) 0.0409(5) Uani 1 1 d . . . . . H9 H 0.956220 -0.472349 0.265265 0.049 Uiso 1 1 calc R U . . . C3 C 1.0589(2) -0.2807(2) 0.21533(7) 0.0414(5) Uani 1 1 d . . . . . H3 H 1.080806 -0.355957 0.200080 0.050 Uiso 1 1 calc R U . . . C25 C 0.4854(3) 0.8489(2) 0.54596(6) 0.0405(5) Uani 1 1 d . . . . . H25 H 0.380066 0.890324 0.542648 0.049 Uiso 1 1 calc R U . . . C2 C 1.1026(2) -0.1699(2) 0.19707(6) 0.0405(5) Uani 1 1 d . . . . . H2 H 1.157329 -0.167504 0.169430 0.049 Uiso 1 1 calc R U . . . C23 C 0.3921(4) 0.7013(2) 0.48305(10) 0.0350(7) Uani 0.874(3) 1 d . . P A 1 C8 C 0.8637(3) -0.39186(18) 0.31942(8) 0.0412(5) Uani 1 1 d . . . . . H8 H 0.835283 -0.467462 0.333552 0.049 Uiso 1 1 calc R U . . . C11 C 0.7272(3) -0.1537(2) 0.40101(7) 0.0460(5) Uani 1 1 d . . . . . H11 H 0.677214 -0.146524 0.429249 0.055 Uiso 1 1 calc R U . . . C10 C 0.7569(3) -0.2673(2) 0.38321(7) 0.0443(5) Uani 1 1 d . . . . . H10 H 0.728713 -0.340195 0.399121 0.053 Uiso 1 1 calc R U . . . C21 C 0.1555(3) 0.5908(3) 0.42920(8) 0.0484(7) Uani 0.874(3) 1 d . . P A 1 H21 H 0.074907 0.549706 0.409487 0.058 Uiso 0.874(3) 1 calc R U P A 1 N4 N 0.1008(3) 0.6634(3) 0.46146(8) 0.0654(9) Uani 0.874(3) 1 d . . P A 1 C22 C 0.2197(3) 0.7185(3) 0.48825(9) 0.0573(9) Uani 0.874(3) 1 d . . P A 1 H22 H 0.186144 0.771357 0.511743 0.069 Uiso 0.874(3) 1 calc R U P A 1 N5 N 0.149(2) 0.7661(15) 0.4336(5) 0.055(3) Uani 0.126(3) 1 d . U P A 2 C22A C 0.266(2) 0.8054(18) 0.4660(6) 0.049(3) Uani 0.126(3) 1 d . U P A 2 H22A H 0.246926 0.879980 0.481982 0.058 Uiso 0.126(3) 1 calc R U P A 2 C21A C 0.193(2) 0.6728(19) 0.4081(6) 0.051(3) Uani 0.126(3) 1 d . U P A 2 H21A H 0.118691 0.649261 0.383210 0.061 Uiso 0.126(3) 1 calc R U P A 2 C23A C 0.409(4) 0.741(2) 0.4760(10) 0.044(3) Uani 0.126(3) 1 d . U P A 2 C20A C 0.340(4) 0.608(2) 0.4154(10) 0.048(3) Uani 0.126(3) 1 d . U P A 2 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 Mn1 0.02843(16) 0.02696(15) 0.02202(14) 0.00067(10) -0.00225(10) -0.00060(11) O3 0.0349(7) 0.0387(7) 0.0351(7) -0.0028(6) -0.0039(6) 0.0095(6) O1 0.0328(7) 0.0505(8) 0.0267(7) -0.0112(6) -0.0020(5) 0.0006(6) O4 0.0418(8) 0.0413(7) 0.0261(6) -0.0084(5) -0.0082(5) 0.0110(6) O2 0.0335(7) 0.0437(7) 0.0341(7) -0.0072(6) -0.0085(5) 0.0054(6) N1 0.0251(7) 0.0328(8) 0.0249(7) -0.0005(6) -0.0002(6) 0.0002(6) N3 0.0297(8) 0.0380(8) 0.0221(7) -0.0044(6) -0.0019(6) 0.0023(6) N2 0.0276(8) 0.0326(8) 0.0274(7) 0.0015(6) 0.0028(6) 0.0010(6) C27 0.0295(9) 0.0339(9) 0.0226(8) -0.0002(7) -0.0003(7) -0.0025(7) C5 0.0203(8) 0.0293(9) 0.0294(9) -0.0003(7) -0.0036(6) 0.0020(7) C15 0.0303(9) 0.0301(9) 0.0227(8) -0.0007(7) -0.0038(7) -0.0013(7) C14 0.0300(9) 0.0236(8) 0.0235(8) 0.0017(7) -0.0018(7) -0.0017(7) C18 0.0280(9) 0.0348(9) 0.0250(8) -0.0030(7) -0.0053(7) -0.0025(8) C6 0.0219(8) 0.0285(9) 0.0305(9) 0.0035(7) -0.0025(7) 0.0002(7) C19 0.0277(9) 0.0299(9) 0.0281(9) -0.0003(7) -0.0042(7) -0.0002(7) C17 0.0278(9) 0.0354(9) 0.0234(8) -0.0028(7) -0.0022(7) -0.0011(7) C30 0.0320(10) 0.0340(9) 0.0246(9) 0.0005(7) 0.0006(7) -0.0047(8) C13 0.0297(9) 0.0262(8) 0.0279(9) -0.0011(7) -0.0028(7) 0.0000(7) C16 0.0275(9) 0.0385(10) 0.0260(9) -0.0012(7) -0.0032(7) 0.0026(8) C4 0.0261(9) 0.0346(10) 0.0380(10) -0.0071(8) -0.0058(7) 0.0039(8) C7 0.0280(10) 0.0344(10) 0.0400(10) 0.0086(8) -0.0034(8) -0.0015(8) C26 0.0391(11) 0.0421(11) 0.0316(10) -0.0136(8) -0.0045(8) 0.0067(9) C28 0.0273(9) 0.0437(11) 0.0304(9) -0.0056(8) -0.0001(7) 0.0034(8) C20 0.0303(11) 0.0391(16) 0.0247(12) -0.0055(10) -0.0025(9) 0.0020(12) C29 0.0352(10) 0.0465(11) 0.0269(9) -0.0113(8) -0.0007(8) 0.0059(9) C1 0.0286(9) 0.0445(11) 0.0278(9) 0.0012(8) 0.0026(7) 0.0019(8) C12 0.0391(11) 0.0415(11) 0.0320(10) 0.0013(8) 0.0096(8) 0.0006(9) C24 0.0326(10) 0.0426(10) 0.0222(8) -0.0060(8) -0.0018(7) 0.0041(8) C9 0.0393(11) 0.0284(10) 0.0535(13) -0.0043(9) -0.0092(9) 0.0031(8) C3 0.0369(11) 0.0451(12) 0.0416(11) -0.0139(9) -0.0016(9) 0.0102(9) C25 0.0359(11) 0.0499(12) 0.0345(10) -0.0119(9) -0.0078(8) 0.0132(9) C2 0.0356(11) 0.0554(13) 0.0306(10) -0.0068(9) 0.0043(8) 0.0067(9) C23 0.0335(13) 0.0454(17) 0.0256(12) -0.0094(12) -0.0034(9) 0.0067(13) C8 0.0386(11) 0.0293(10) 0.0547(13) 0.0085(9) -0.0050(9) -0.0017(8) C11 0.0480(13) 0.0556(13) 0.0354(11) 0.0074(10) 0.0120(9) -0.0030(10) C10 0.0433(12) 0.0470(12) 0.0428(12) 0.0159(10) 0.0042(9) -0.0051(10) C21 0.0311(12) 0.0718(19) 0.0414(13) -0.0259(13) -0.0048(10) 0.0023(12) N4 0.0314(11) 0.104(2) 0.0605(15) -0.0467(15) -0.0039(10) 0.0081(12) C22 0.0361(13) 0.087(2) 0.0482(15) -0.0381(15) -0.0020(11) 0.0073(13) N5 0.051(4) 0.060(5) 0.052(5) -0.021(4) -0.018(4) 0.014(4) C22A 0.044(5) 0.053(5) 0.047(5) -0.019(4) -0.014(4) 0.013(4) C21A 0.048(4) 0.056(5) 0.047(5) -0.018(4) -0.020(4) 0.011(4) C23A 0.041(5) 0.048(5) 0.043(5) -0.015(4) -0.008(4) 0.011(4) C20A 0.047(5) 0.053(6) 0.042(5) -0.015(4) -0.019(4) 0.010(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0137 0.0067 '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' Mn Mn -0.0162 2.2332 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0389 0.0241 '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 O3 Mn1 O1 148.33(5) . 3_766 ? O3 Mn1 O4 95.73(5) . 2_655 ? O3 Mn1 O2 91.47(5) . 3_766 ? O3 Mn1 N1 116.14(5) . . ? O3 Mn1 N2 85.13(5) . . ? O3 Mn1 C30 120.07(5) . 3_766 ? O1 Mn1 N1 89.54(5) 3_766 . ? O1 Mn1 C30 28.97(5) 3_766 3_766 ? O4 Mn1 O1 100.34(5) 2_655 3_766 ? O4 Mn1 O2 105.09(5) 2_655 3_766 ? O4 Mn1 N1 95.02(5) 2_655 . ? O4 Mn1 N2 166.33(5) 2_655 . ? O4 Mn1 C30 105.04(5) 2_655 3_766 ? O2 Mn1 O1 58.09(4) 3_766 3_766 ? O2 Mn1 N1 144.08(5) 3_766 . ? O2 Mn1 N2 88.51(5) 3_766 . ? O2 Mn1 C30 29.12(5) 3_766 3_766 ? N1 Mn1 C30 117.07(6) . 3_766 ? N2 Mn1 O1 85.52(5) . 3_766 ? N2 Mn1 N1 72.54(5) . . ? N2 Mn1 C30 86.10(5) . 3_766 ? C13 O3 Mn1 155.92(13) . . ? C30 O1 Mn1 90.04(11) . 3_766 ? C13 O4 Mn1 118.20(11) . 2_655 ? C30 O2 Mn1 90.04(10) . 3_766 ? C5 N1 Mn1 115.50(11) . . ? C1 N1 Mn1 126.48(13) . . ? C1 N1 C5 117.89(16) . . ? C23 N3 C20 117.5(2) . . ? C20A N3 C23A 114.8(18) . . ? C6 N2 Mn1 116.79(11) . . ? C12 N2 Mn1 124.76(13) . . ? C12 N2 C6 118.26(16) . . ? C26 C27 C30 120.44(16) . . ? C26 C27 C28 118.73(16) . . ? C28 C27 C30 120.69(16) . . ? N1 C5 C6 117.67(15) . . ? N1 C5 C4 123.07(16) . . ? C4 C5 C6 119.25(16) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C16 C15 C14 120.35(15) . . ? C15 C14 C19 119.24(16) . . ? C15 C14 C13 120.71(15) . . ? C19 C14 C13 120.02(15) . . ? C19 C18 H18 119.4 . . ? C19 C18 C17 121.12(15) . . ? C17 C18 H18 119.4 . . ? N2 C6 C5 117.31(15) . . ? N2 C6 C7 122.73(16) . . ? C7 C6 C5 119.96(16) . . ? C14 C19 H19 120.0 . . ? C18 C19 C14 120.04(16) . . ? C18 C19 H19 120.0 . . ? C18 C17 C16 118.38(16) . . ? C18 C17 C20 120.11(18) . . ? C18 C17 C20A 121.4(11) . . ? C16 C17 C20 121.42(19) . . ? C16 C17 C20A 118.2(10) . . ? O1 C30 Mn1 60.99(9) . 3_766 ? O1 C30 O2 121.81(16) . . ? O1 C30 C27 118.90(16) . . ? O2 C30 Mn1 60.84(9) . 3_766 ? O2 C30 C27 119.27(16) . . ? C27 C30 Mn1 179.88(16) . 3_766 ? O3 C13 O4 124.13(16) . . ? O3 C13 C14 117.90(15) . . ? O4 C13 C14 117.96(15) . . ? C15 C16 C17 120.82(16) . . ? C15 C16 H16 119.6 . . ? C17 C16 H16 119.6 . . ? C5 C4 C9 119.52(18) . . ? C5 C4 C3 117.04(18) . . ? C3 C4 C9 123.44(18) . . ? C6 C7 C8 119.17(18) . . ? C6 C7 C10 117.10(18) . . ? C10 C7 C8 123.72(18) . . ? C27 C26 H26 119.6 . . ? C27 C26 C25 120.85(17) . . ? C25 C26 H26 119.6 . . ? C27 C28 H28 119.8 . . ? C29 C28 C27 120.38(17) . . ? C29 C28 H28 119.8 . . ? N3 C20 C17 116.9(2) . . ? N3 C20 C21 120.4(3) . . ? C21 C20 C17 122.7(2) . . ? C28 C29 H29 119.5 . . ? C28 C29 C24 120.92(17) . . ? C24 C29 H29 119.5 . . ? N1 C1 H1 118.5 . . ? N1 C1 C2 122.93(19) . . ? C2 C1 H1 118.5 . . ? N2 C12 H12 118.5 . . ? N2 C12 C11 122.96(19) . . ? C11 C12 H12 118.5 . . ? C29 C24 C25 118.34(16) . . ? C29 C24 C23 119.54(19) . . ? C29 C24 C23A 123.3(12) . . ? C25 C24 C23 121.6(2) . . ? C25 C24 C23A 116.9(11) . . ? C4 C9 H9 119.5 . . ? C8 C9 C4 121.10(18) . . ? C8 C9 H9 119.5 . . ? C4 C3 H3 120.1 . . ? C2 C3 C4 119.72(18) . . ? C2 C3 H3 120.1 . . ? C26 C25 C24 120.46(18) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C1 C2 H2 120.3 . . ? C3 C2 C1 119.32(18) . . ? C3 C2 H2 120.3 . . ? N3 C23 C24 117.1(3) . . ? N3 C23 C22 120.8(3) . . ? C22 C23 C24 122.0(2) . . ? C7 C8 H8 119.5 . . ? C9 C8 C7 120.98(18) . . ? C9 C8 H8 119.5 . . ? C12 C11 H11 120.4 . . ? C10 C11 C12 119.19(19) . . ? C10 C11 H11 120.4 . . ? C7 C10 H10 120.1 . . ? C11 C10 C7 119.75(19) . . ? C11 C10 H10 120.1 . . ? C20 C21 H21 118.6 . . ? N4 C21 C20 122.9(2) . . ? N4 C21 H21 118.6 . . ? C21 N4 C22 115.9(2) . . ? C23 C22 H22 118.7 . . ? N4 C22 C23 122.6(2) . . ? N4 C22 H22 118.7 . . ? C21A N5 C22A 116.5(15) . . ? N5 C22A H22A 119.2 . . ? C23A C22A N5 121.6(18) . . ? C23A C22A H22A 119.2 . . ? N5 C21A H21A 118.3 . . ? N5 C21A C20A 123.5(18) . . ? C20A C21A H21A 118.3 . . ? C24 C23A N3 112.4(18) . . ? C22A C23A N3 120(2) . . ? C22A C23A C24 127(2) . . ? N3 C20A C17 113(2) . . ? N3 C20A C21A 122(2) . . ? C21A C20A C17 124(2) . . ? 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 Mn1 O3 2.1025(13) . ? Mn1 O1 2.2670(13) 3_766 ? Mn1 O4 2.1156(12) 2_655 ? Mn1 O2 2.2638(12) 3_766 ? Mn1 N1 2.2914(15) . ? Mn1 N2 2.2658(15) . ? Mn1 C30 2.5924(17) 3_766 ? O3 C13 1.254(2) . ? O1 C30 1.256(2) . ? O4 C13 1.264(2) . ? O2 C30 1.262(2) . ? N1 C5 1.359(2) . ? N1 C1 1.332(2) . ? N3 C20 1.354(3) . ? N3 C23 1.329(3) . ? N3 C23A 1.46(3) . ? N3 C20A 1.31(3) . ? N2 C6 1.353(2) . ? N2 C12 1.327(2) . ? C27 C30 1.498(2) . ? C27 C26 1.383(3) . ? C27 C28 1.392(2) . ? C5 C6 1.444(2) . ? C5 C4 1.404(2) . ? C15 H15 0.9500 . ? C15 C14 1.390(2) . ? C15 C16 1.381(2) . ? C14 C19 1.399(2) . ? C14 C13 1.495(2) . ? C18 H18 0.9500 . ? C18 C19 1.379(2) . ? C18 C17 1.393(2) . ? C6 C7 1.402(2) . ? C19 H19 0.9500 . ? C17 C16 1.398(2) . ? C17 C20 1.474(4) . ? C17 C20A 1.57(3) . ? C16 H16 0.9500 . ? C4 C9 1.429(3) . ? C4 C3 1.411(3) . ? C7 C8 1.432(3) . ? C7 C10 1.410(3) . ? C26 H26 0.9500 . ? C26 C25 1.386(3) . ? C28 H28 0.9500 . ? C28 C29 1.384(2) . ? C20 C21 1.395(4) . ? C29 H29 0.9500 . ? C29 C24 1.389(3) . ? C1 H1 0.9500 . ? C1 C2 1.396(3) . ? C12 H12 0.9500 . ? C12 C11 1.392(3) . ? C24 C25 1.395(3) . ? C24 C23 1.498(4) . ? C24 C23A 1.45(3) . ? C9 H9 0.9500 . ? C9 C8 1.355(3) . ? C3 H3 0.9500 . ? C3 C2 1.365(3) . ? C25 H25 0.9500 . ? C2 H2 0.9500 . ? C23 C22 1.402(4) . ? C8 H8 0.9500 . ? C11 H11 0.9500 . ? C11 C10 1.360(3) . ? C10 H10 0.9500 . ? C21 H21 0.9500 . ? C21 N4 1.328(3) . ? N4 C22 1.336(3) . ? C22 H22 0.9500 . ? N5 C22A 1.36(2) . ? N5 C21A 1.32(2) . ? C22A H22A 0.9500 . ? C22A C23A 1.35(3) . ? C21A H21A 0.9500 . ? C21A C20A 1.37(3) . ? 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 Mn1 O3 C13 O4 76.0(4) . . . . ? Mn1 O3 C13 C14 -105.0(3) . . . . ? Mn1 O1 C30 O2 1.78(18) 3_766 . . . ? Mn1 O1 C30 C27 -179.97(15) 3_766 . . . ? Mn1 O4 C13 O3 2.0(2) 2_655 . . . ? Mn1 O4 C13 C14 -176.93(11) 2_655 . . . ? Mn1 O2 C30 O1 -1.79(18) 3_766 . . . ? Mn1 O2 C30 C27 179.97(15) 3_766 . . . ? Mn1 N1 C5 C6 2.16(19) . . . . ? Mn1 N1 C5 C4 -176.78(13) . . . . ? Mn1 N1 C1 C2 176.38(13) . . . . ? Mn1 N2 C6 C5 -4.33(19) . . . . ? Mn1 N2 C6 C7 175.70(13) . . . . ? Mn1 N2 C12 C11 -174.62(15) . . . . ? N1 C5 C6 N2 1.4(2) . . . . ? N1 C5 C6 C7 -178.62(15) . . . . ? N1 C5 C4 C9 179.34(16) . . . . ? N1 C5 C4 C3 -0.4(3) . . . . ? N1 C1 C2 C3 0.3(3) . . . . ? N3 C20 C21 N4 -0.4(4) . . . . ? N3 C23 C22 N4 1.0(5) . . . . ? N2 C6 C7 C8 179.23(16) . . . . ? N2 C6 C7 C10 -1.1(3) . . . . ? N2 C12 C11 C10 -0.2(3) . . . . ? C27 C26 C25 C24 0.9(3) . . . . ? C27 C28 C29 C24 0.7(3) . . . . ? C5 N1 C1 C2 0.8(2) . . . . ? C5 C6 C7 C8 -0.7(3) . . . . ? C5 C6 C7 C10 178.90(16) . . . . ? C5 C4 C9 C8 -0.8(3) . . . . ? C5 C4 C3 C2 1.5(3) . . . . ? C15 C14 C19 C18 -2.5(3) . . . . ? C15 C14 C13 O3 -161.29(16) . . . . ? C15 C14 C13 O4 17.7(2) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C18 C17 C16 C15 -1.8(3) . . . . ? C18 C17 C20 N3 25.2(3) . . . . ? C18 C17 C20 C21 -154.5(2) . . . . ? C18 C17 C20A N3 -16(3) . . . . ? C18 C17 C20A C21A 172.9(19) . . . . ? C6 N2 C12 C11 0.3(3) . . . . ? C6 C5 C4 C9 0.4(3) . . . . ? C6 C5 C4 C3 -179.37(16) . . . . ? C6 C7 C8 C9 0.3(3) . . . . ? C6 C7 C10 C11 1.2(3) . . . . ? C19 C14 C13 O3 16.8(2) . . . . ? C19 C14 C13 O4 -164.17(16) . . . . ? C19 C18 C17 C16 1.0(3) . . . . ? C19 C18 C17 C20 177.52(18) . . . . ? C19 C18 C17 C20A -162.4(13) . . . . ? C17 C18 C19 C14 1.1(3) . . . . ? C17 C20 C21 N4 179.3(3) . . . . ? C30 C27 C26 C25 -171.89(19) . . . . ? C30 C27 C28 C29 171.10(18) . . . . ? C13 C14 C19 C18 179.38(16) . . . . ? C16 C15 C14 C19 1.7(3) . . . . ? C16 C15 C14 C13 179.82(16) . . . . ? C16 C17 C20 N3 -158.44(19) . . . . ? C16 C17 C20 C21 21.8(3) . . . . ? C16 C17 C20A N3 -179.2(13) . . . . ? C16 C17 C20A C21A 9(3) . . . . ? C4 C5 C6 N2 -179.61(15) . . . . ? C4 C5 C6 C7 0.4(2) . . . . ? C4 C9 C8 C7 0.5(3) . . . . ? C4 C3 C2 C1 -1.5(3) . . . . ? C26 C27 C30 O1 1.6(3) . . . . ? C26 C27 C30 O2 179.89(18) . . . . ? C26 C27 C28 C29 -4.7(3) . . . . ? C28 C27 C30 O1 -174.14(17) . . . . ? C28 C27 C30 O2 4.2(3) . . . . ? C28 C27 C26 C25 3.9(3) . . . . ? C28 C29 C24 C25 4.2(3) . . . . ? C28 C29 C24 C23 -168.0(2) . . . . ? C28 C29 C24 C23A 169.8(13) . . . . ? C20 N3 C23 C24 175.30(19) . . . . ? C20 N3 C23 C22 -1.5(4) . . . . ? C20 C17 C16 C15 -178.27(18) . . . . ? C20 C21 N4 C22 -0.2(5) . . . . ? C29 C24 C25 C26 -5.0(3) . . . . ? C29 C24 C23 N3 -19.2(3) . . . . ? C29 C24 C23 C22 157.6(3) . . . . ? C29 C24 C23A N3 24(2) . . . . ? C29 C24 C23A C22A -167(2) . . . . ? C1 N1 C5 C6 178.24(15) . . . . ? C1 N1 C5 C4 -0.7(2) . . . . ? C12 N2 C6 C5 -179.61(16) . . . . ? C12 N2 C6 C7 0.4(2) . . . . ? C12 C11 C10 C7 -0.6(3) . . . . ? C24 C23 C22 N4 -175.7(3) . . . . ? C9 C4 C3 C2 -178.23(18) . . . . ? C3 C4 C9 C8 178.93(19) . . . . ? C25 C24 C23 N3 169.0(2) . . . . ? C25 C24 C23 C22 -14.3(4) . . . . ? C25 C24 C23A N3 -170.5(12) . . . . ? C25 C24 C23A C22A -1(3) . . . . ? C23 N3 C20 C17 -178.52(19) . . . . ? C23 N3 C20 C21 1.2(3) . . . . ? C23 C24 C25 C26 167.0(2) . . . . ? C8 C7 C10 C11 -179.18(19) . . . . ? C10 C7 C8 C9 -179.3(2) . . . . ? C21 N4 C22 C23 -0.1(5) . . . . ? N5 C22A C23A N3 3(4) . . . . ? N5 C22A C23A C24 -166(2) . . . . ? N5 C21A C20A N3 4(4) . . . . ? N5 C21A C20A C17 175(2) . . . . ? C22A N5 C21A C20A 6(3) . . . . ? C21A N5 C22A C23A -10(3) . . . . ? C23A N3 C20A C17 178.0(16) . . . . ? C23A N3 C20A C21A -10(3) . . . . ? C23A C24 C25 C26 -171.5(13) . . . . ? C20A N3 C23A C24 177.3(18) . . . . ? C20A N3 C23A C22A 7(3) . . . . ? C20A C17 C16 C15 162.1(13) . . . . ?