#------------------------------------------------------------------------------ #$Date: 2026-05-10 01:35:23 +0100 (Sun, 10 May 2026) $ #$Revision: 305917 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064406.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_7064406 loop_ _publ_author_name 'Li, Bing-Yu' 'Tong, Jin' 'Wang, Ji' 'Yu, Shu-Yan' _publ_section_title ; Self-Assembly of Tetraphenylethylene-Cored Metallacycles Linked by Stereo-isomerizable Ligands: Photo-induced E to Z isomerization within Supramolecular Structures ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D6NJ01109H _journal_year 2026 _chemical_absolute_configuration ad _chemical_formula_moiety 'C32 H24 N4' _chemical_formula_sum 'C32 H24 N4' _chemical_formula_weight 464.55 _space_group_crystal_system orthorhombic _space_group_IT_number 36 _space_group_name_Hall 'C 2c -2' _space_group_name_H-M_alt 'C m c 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2021-07-28 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2026-03-04 deposited with the CCDC. 2026-05-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 39.366(10) _cell_length_b 18.683(5) _cell_length_c 9.677(2) _cell_measurement_reflns_used 9798 _cell_measurement_temperature 193.0 _cell_measurement_theta_max 53.724 _cell_measurement_theta_min 2.277 _cell_volume 7117(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 0.972 _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 0.0732 _diffrn_reflns_av_unetI/netI 0.0525 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 54151 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.953 _diffrn_reflns_theta_full 53.594 _diffrn_reflns_theta_max 60.171 _diffrn_reflns_theta_min 1.953 _diffrn_source_current 2.86 _diffrn_source_power 0.1993706 _diffrn_source_voltage 69.71 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_T_max 0.7518 _exptl_absorpt_correction_T_min 0.6684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1490 before and 0.0788 after correction. The Ratio of minimum to maximum transmission is 0.8891. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 0.867 _exptl_crystal_description block _exptl_crystal_F_000 1952 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.184 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details ; Flack x determined using 1859 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.4(2) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 417 _refine_ls_number_reflns 7813 _refine_ls_number_restraints 158 _refine_ls_restrained_S_all 1.057 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0653 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1399P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1900 _refine_ls_wR_factor_ref 0.2174 _reflns_Friedel_coverage 0.847 _reflns_Friedel_fraction_full 0.993 _reflns_Friedel_fraction_max 0.932 _reflns_number_gt 5081 _reflns_number_total 7813 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6nj01109h2.cif _cod_data_source_block a1_sq _cod_database_code 7064406 _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 0.975 _shelx_estimated_absorpt_t_min 0.970 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All N(H) groups 2. Restrained distances N4A-N3A \\sim N4-N3 with sigma of 0.02 3. Rigid body (RIGU) restrains N3, C27, C30, C32, C31, N3A, N4A, N4, C31A, C30A, C32A with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 C18, N1A, C22, C21, N2, C23, C23A, N2A, C21A, N1, C22A with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 4. Others Sof(N3A)=Sof(H3AA)=Sof(N4A)=Sof(C31A)=Sof(H31A)=Sof(C30A)=Sof(C32A)=Sof(H32A)= 1-FVAR(1) Sof(N3)=Sof(H3)=Sof(C30)=Sof(C32)=Sof(H32)=Sof(C31)=Sof(H31)=Sof(N4)=FVAR(1) Sof(N1A)=Sof(C23A)=Sof(H23A)=Sof(N2A)=Sof(H2A)=Sof(C21A)=Sof(C22A)=Sof(H22A)= 1-FVAR(2) Sof(C22)=Sof(H22)=Sof(C21)=Sof(N2)=Sof(C23)=Sof(H23)=Sof(N1)=Sof(H1A)=FVAR(2) 5.a Aromatic/amide H refined with riding coordinates: C17(H17), C16(H16), C14(H14), C4(H4), C5(H5), C10(H10), C20(H20), C1(H1), C26(H26), C25(H25), C29(H29), N3(H3), C28(H28), C2(H2), C22(H22), C3(H3A), C11(H11), C19(H19), C13(H13), C32(H32), C12(H12), C31(H31), C23(H23), N3A(H3AA), C31A(H31A), C32A(H32A), C23A(H23A), N2A(H2A), N1(H1A), C22A(H22A) ; _shelx_res_file ; TITL a1_a.res in Cmc2(1) a1_sq.res created by SHELXL-2018/3 at 16:53:57 on 28-Jul-2021 REM Old TITL A1 in Cmcm REM SHELXT solution in Cmc2(1): R1 0.267, Rweak 0.041, Alpha 0.012 REM 0.370 for 121 systematic absences, Orientation as input REM Flack x = 0.228 ( 0.185 ) from 1924 Parsons' quotients REM Formula found by SHELXT: C31 N9 O CELL 1.34139 39.366 18.683 9.677 90 90 90 ZERR 8 0.0097 0.0045 0.0023 0 0 0 LATT -7 SYMM -X,-Y,0.5+Z SYMM +X,-Y,0.5+Z SYMM -X,+Y,+Z SFAC C H N DISP C 0.0137 0.0067 57.1 DISP H 0 0 0.6 DISP N 0.0241 0.0134 109.9 UNIT 256 192 32 SADI N4A N3A N4 N3 RIGU 0.002 0.002 N3 C27 C30 C32 C31 N3A N4A N4 C31A C30A C32A RIGU 0.002 0.002 C18 N1A C22 C21 N2 C23 C23A N2A C21A N1 C22A L.S. 10 0 109 PLAN 20 SIZE 0.1 0.12 0.1 TEMP -80.15 CONF BOND MORE -1 HTAB ABIN fmap 2 acta BOND $H REM REM REM WGHT 0.139900 FVAR 0.33402 0.70135 0.46439 C17 1 0.649928 0.614770 0.642317 11.00000 0.04282 0.04338 = 0.05778 -0.00838 0.00209 -0.00153 AFIX 43 H17 2 0.650156 0.654485 0.703615 11.00000 -1.20000 AFIX 0 C16 1 0.678792 0.573406 0.629843 11.00000 0.04163 0.04309 = 0.05418 -0.00251 -0.00424 -0.00122 AFIX 43 H16 2 0.698415 0.585750 0.681777 11.00000 -1.20000 AFIX 0 C6 1 0.740777 0.352433 0.497058 11.00000 0.04021 0.03472 = 0.04938 -0.00074 0.00122 0.00072 C14 1 0.746674 0.571891 0.439801 11.00000 0.04602 0.04211 = 0.06334 0.00657 0.00708 0.00035 AFIX 43 H14 2 0.727669 0.586829 0.386612 11.00000 -1.20000 AFIX 0 C9 1 0.743859 0.510593 0.523930 11.00000 0.04068 0.03926 = 0.04796 -0.00691 0.00241 0.00043 C15 1 0.679887 0.513958 0.542958 11.00000 0.03822 0.03579 = 0.05167 0.00187 0.00131 0.00067 C4 1 0.786373 0.315291 0.347292 11.00000 0.04840 0.05821 = 0.05803 -0.00990 0.00713 -0.00543 AFIX 43 H4 2 0.798991 0.321678 0.264521 11.00000 -1.20000 AFIX 0 C5 1 0.760427 0.361180 0.376300 11.00000 0.04917 0.04397 = 0.05040 -0.00018 0.00247 0.00260 AFIX 43 H5 2 0.755528 0.399393 0.314677 11.00000 -1.20000 AFIX 0 C7 1 0.710596 0.397148 0.528077 11.00000 0.03946 0.03795 = 0.04733 -0.00135 0.00111 0.00071 C10 1 0.771560 0.492758 0.600888 11.00000 0.04830 0.04663 = 0.05965 0.00013 0.00084 -0.00033 AFIX 43 H10 2 0.770261 0.452330 0.660196 11.00000 -1.20000 AFIX 0 C24 1 0.679742 0.353839 0.560423 11.00000 0.04222 0.03938 = 0.04427 0.00277 -0.00305 -0.00328 C20 1 0.650588 0.498889 0.467127 11.00000 0.04987 0.04598 = 0.05375 -0.00366 -0.00247 -0.00095 AFIX 43 H20 2 0.650396 0.459067 0.406087 11.00000 -1.20000 AFIX 0 C1 1 0.749416 0.295757 0.584472 11.00000 0.04475 0.04550 = 0.05257 0.00006 0.00223 -0.00317 AFIX 43 H1 2 0.736533 0.288303 0.666228 11.00000 -1.20000 AFIX 0 C26 1 0.632617 0.321998 0.710678 11.00000 0.04887 0.05748 = 0.06209 0.00436 0.00714 0.00055 AFIX 43 H26 2 0.619761 0.330713 0.792037 11.00000 -1.20000 AFIX 0 C25 1 0.660135 0.365750 0.680460 11.00000 0.04582 0.04490 = 0.05452 0.00141 0.00314 -0.00250 AFIX 43 H25 2 0.665817 0.403969 0.740947 11.00000 -1.20000 AFIX 0 C29 1 0.670751 0.296797 0.475092 11.00000 0.04918 0.03941 = 0.05801 0.00325 -0.00121 -0.00136 AFIX 43 H29 2 0.683954 0.286859 0.395189 11.00000 -1.20000 AFIX 0 C8 1 0.711468 0.470023 0.530215 11.00000 0.04062 0.03695 = 0.04587 0.00282 0.00017 -0.00042 C18 1 0.620725 0.600253 0.568507 11.00000 0.04390 0.04413 = 0.06835 -0.00066 0.00275 -0.00053 PART 1 N3 3 0.551070 0.159095 0.747727 21.00000 0.05617 0.05937 = 0.10195 0.00588 0.01421 -0.01195 AFIX 43 H3 2 0.537476 0.142292 0.812217 21.00000 -1.20000 AFIX 0 PART 0 C27 1 0.623478 0.265737 0.624465 11.00000 0.04501 0.04564 = 0.07969 0.01098 -0.00041 -0.00208 C28 1 0.642440 0.253769 0.505527 11.00000 0.04935 0.04545 = 0.07623 0.00335 -0.00241 -0.00253 AFIX 43 H28 2 0.636217 0.216224 0.444354 11.00000 -1.20000 AFIX 0 C2 1 0.776098 0.250317 0.555545 11.00000 0.05573 0.04292 = 0.07751 0.00612 -0.00209 0.00302 AFIX 43 H2 2 0.781555 0.212839 0.618068 11.00000 -1.20000 AFIX 0 PART 2 N1A 3 0.554665 0.726310 0.667415 -31.00000 0.05350 0.06045 = 0.13289 -0.02080 -0.01379 0.00131 PART 1 C22 1 0.584498 0.710482 0.627853 31.00000 0.04026 0.04880 = 0.05222 0.00175 0.00067 0.00458 AFIX 43 H22 2 0.601448 0.735074 0.679127 31.00000 -1.20000 AFIX 0 PART 0 C3 1 0.794944 0.258935 0.436262 11.00000 0.05430 0.05221 = 0.08103 -0.00881 -0.00179 0.01151 AFIX 43 H3A 2 0.813201 0.227535 0.415147 11.00000 -1.20000 AFIX 0 C11 1 0.801158 0.530899 0.595906 11.00000 0.04930 0.06325 = 0.07341 -0.00338 -0.00113 -0.00417 AFIX 43 H11 2 0.819978 0.516111 0.650325 11.00000 -1.20000 AFIX 0 PART 1 C21 1 0.589818 0.645983 0.560320 31.00000 0.03675 0.03961 = 0.05949 0.00337 0.00906 -0.00293 PART 0 C19 1 0.621916 0.540814 0.479294 11.00000 0.04107 0.05646 = 0.07640 -0.00848 -0.00723 0.00017 AFIX 43 H19 2 0.602415 0.529249 0.425948 11.00000 -1.20000 AFIX 0 C13 1 0.776383 0.610540 0.433130 11.00000 0.06415 0.04682 = 0.07934 -0.00102 0.01041 -0.00712 AFIX 43 H13 2 0.778044 0.650974 0.373986 11.00000 -1.20000 AFIX 0 PART 1 N2 3 0.537262 0.683091 0.527939 31.00000 0.04839 0.07256 = 0.09590 -0.00720 -0.01116 0.01044 C30 1 0.593135 0.219366 0.640926 21.00000 0.04238 0.04722 = 0.06918 0.00773 -0.00586 -0.00261 C32 1 0.576320 0.209766 0.767814 21.00000 0.05554 0.05708 = 0.07279 0.00676 0.00285 -0.00534 AFIX 43 H32 2 0.581351 0.233667 0.852012 21.00000 -1.20000 AFIX 0 PART 0 C12 1 0.804018 0.589885 0.513851 11.00000 0.05490 0.05563 = 0.08731 -0.00706 0.00329 -0.01359 AFIX 43 H12 2 0.824561 0.616546 0.511707 11.00000 -1.20000 AFIX 0 PART 1 C31 1 0.576426 0.174291 0.548948 21.00000 0.05555 0.06233 = 0.07801 -0.01002 0.00337 -0.00879 AFIX 43 H31 2 0.582213 0.168538 0.454290 21.00000 -1.20000 AFIX 0 C23 1 0.559002 0.637859 0.499558 31.00000 0.04772 0.05724 = 0.07614 -0.00448 -0.00550 0.00153 AFIX 43 H23 2 0.554400 0.599323 0.438307 31.00000 -1.20000 AFIX 0 PART 2 N3A 3 0.552925 0.174485 0.812592 -21.00000 0.06520 0.07799 = 0.07547 0.00456 0.01673 -0.02440 AFIX 43 H3AA 2 0.538146 0.164131 0.877826 -21.00000 -1.20000 AFIX 0 N4A 3 0.552619 0.144261 0.686871 -21.00000 0.04176 0.07081 = 0.07803 0.00113 0.00032 -0.01344 PART 1 N4 3 0.550683 0.139738 0.613890 21.00000 0.06305 0.05698 = 0.11252 -0.00109 0.00567 -0.00977 PART 2 C31A 1 0.578603 0.173123 0.612680 -21.00000 0.04838 0.06772 = 0.06039 -0.00989 0.00246 -0.01480 AFIX 43 H31A 2 0.584071 0.161626 0.519674 -21.00000 -1.20000 AFIX 0 C30A 1 0.595229 0.220354 0.691907 -21.00000 0.03158 0.04009 = 0.05100 0.00750 -0.00742 0.00360 C32A 1 0.578532 0.222942 0.828775 -21.00000 0.06106 0.05706 = 0.06347 -0.00721 0.00933 -0.00959 AFIX 43 H32A 2 0.584170 0.251007 0.907361 -21.00000 -1.20000 AFIX 0 C23A 1 0.556165 0.623699 0.556770 -31.00000 0.04398 0.07081 = 0.11310 -0.03443 -0.00441 -0.00098 AFIX 43 H23A 2 0.549315 0.581292 0.510319 -31.00000 -1.20000 AFIX 0 N2A 3 0.536109 0.682072 0.591076 -31.00000 0.04367 0.09523 = 0.12809 -0.04557 -0.00912 0.00896 AFIX 43 H2A 2 0.514811 0.688641 0.566540 -31.00000 -1.20000 AFIX 0 C21A 1 0.589815 0.641300 0.607009 -31.00000 0.03748 0.06346 = 0.07773 -0.01355 0.00442 -0.00356 PART 1 N1 3 0.552008 0.734345 0.611782 31.00000 0.03750 0.05144 = 0.08689 -0.00030 0.00353 0.01409 AFIX 43 H1A 2 0.542645 0.773148 0.646516 31.00000 -1.20000 AFIX 0 PART 2 C22A 1 0.586204 0.706475 0.677230 -31.00000 0.05176 0.06701 = 0.07644 -0.01592 -0.00214 -0.00195 AFIX 43 H22A 2 0.603744 0.731718 0.723829 -31.00000 -1.20000 AFIX 0 HKLF 4 REM a1_a.res in Cmc2(1) REM wR2 = 0.2174, GooF = S = 1.064, Restrained GooF = 1.057 for all data REM R1 = 0.0653 for 5081 Fo > 4sig(Fo) and 0.1036 for all 7813 data REM 417 parameters refined using 158 restraints END WGHT 0.1400 0.0000 REM Instructions for potential hydrogen bonds EQIV $1 -x+1, y, z HTAB N2A N2A_$1 REM Highest difference peak 0.184, deepest hole -0.215, 1-sigma level 0.046 Q1 1 0.8528 0.3852 0.4746 11.00000 0.05 0.18 Q2 1 0.6775 0.3517 0.5995 11.00000 0.05 0.18 Q3 1 0.5000 0.1452 0.8317 10.50000 0.05 0.18 Q4 1 0.6124 0.1074 1.0414 11.00000 0.05 0.17 Q5 1 0.5000 0.7117 0.9575 10.50000 0.05 0.17 Q6 1 0.5000 0.1674 0.6868 10.50000 0.05 0.16 Q7 1 0.7084 0.5960 0.8457 11.00000 0.05 0.16 Q8 1 0.5000 0.4514 0.4073 10.50000 0.05 0.15 Q9 1 0.8622 0.4396 0.4191 11.00000 0.05 0.15 Q10 1 0.6663 0.4143 0.4529 11.00000 0.05 0.15 Q11 1 0.5000 0.1955 0.8744 10.50000 0.05 0.15 Q12 1 0.5000 0.5097 0.4481 10.50000 0.05 0.14 Q13 1 0.5206 0.4435 0.4030 11.00000 0.05 0.14 Q14 1 0.5312 0.1084 0.5674 11.00000 0.05 0.14 Q15 1 0.5173 0.2108 0.8384 11.00000 0.05 0.14 Q16 1 0.5000 0.8579 0.6864 10.50000 0.05 0.14 Q17 1 0.6297 0.2065 0.7521 11.00000 0.05 0.14 Q18 1 0.5000 0.3997 0.4912 10.50000 0.05 0.14 Q19 1 0.5000 0.1777 0.4620 10.50000 0.05 0.14 Q20 1 0.5000 0.5532 0.4260 10.50000 0.05 0.14 ; _shelx_res_checksum 23694 _shelx_fab_file ; 0 2 0 227.13 -9.18 0 4 0 -138.86 5.38 0 6 0 -47.96 0.59 0 8 0 -7.70 -2.32 0 10 0 1.11 -13.31 0 12 0 -9.17 -0.17 0 14 0 0.14 -2.11 0 16 0 2.44 1.70 0 18 0 -2.11 -0.10 0 20 0 -4.62 2.54 0 22 0 2.20 -0.41 1 1 0 -139.35 12.13 1 3 0 7.78 5.12 1 5 0 66.40 7.97 1 7 0 24.19 4.98 1 9 0 41.10 3.55 1 11 0 15.41 -0.24 1 13 0 -1.69 -0.97 1 15 0 -1.43 -0.32 1 17 0 -0.97 -2.36 1 19 0 0.06 0.12 1 21 0 -6.97 0.18 2 0 0 439.02 -14.68 2 2 0 125.19 -7.85 2 4 0 -19.75 -0.50 2 6 0 -13.91 -0.19 2 8 0 -23.44 10.71 2 10 0 4.88 -4.36 2 12 0 -6.69 0.16 2 14 0 -1.95 -3.92 2 16 0 1.77 -0.34 2 18 0 1.02 -0.93 2 20 0 -3.55 4.14 2 22 0 2.75 0.28 3 1 0 167.29 2.95 3 3 0 -45.08 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0.14 23 3 10 2.32 -1.20 23 5 10 1.18 -1.73 23 7 10 -0.60 -1.78 23 9 10 -0.98 -3.26 24 0 10 -0.05 -1.38 24 2 10 -1.11 0.25 24 4 10 -0.58 0.01 24 6 10 0.71 1.42 24 8 10 1.55 0.21 25 1 10 1.77 -1.41 25 3 10 1.97 -0.35 25 5 10 1.19 -1.19 25 7 10 -1.14 -0.16 26 0 10 1.96 0.56 26 2 10 0.12 0.86 26 4 10 1.06 -1.11 26 6 10 2.05 -1.40 27 1 10 0.88 -0.17 27 3 10 -1.51 -0.60 27 5 10 -2.50 0.92 28 0 10 1.66 -1.74 28 2 10 1.89 -0.74 28 4 10 2.47 -2.03 29 1 10 -0.11 1.57 29 3 10 -2.59 0.68 30 0 10 1.19 -1.66 30 2 10 1.46 -1.92 0 2 11 -2.44 -1.39 0 4 11 -0.75 -0.03 0 6 11 1.75 0.48 0 8 11 -1.47 -2.20 0 10 11 -2.26 -1.24 1 1 11 2.70 -1.80 1 3 11 0.41 -2.06 1 5 11 0.15 -2.55 1 7 11 -0.13 1.08 1 9 11 1.02 4.18 2 2 11 -2.02 0.20 2 4 11 -0.86 -0.92 2 6 11 1.27 -0.49 2 8 11 -2.00 0.50 2 10 11 -1.11 -0.07 3 1 11 1.89 -1.04 3 3 11 0.58 -1.61 3 5 11 0.36 -0.30 3 7 11 0.17 -1.12 3 9 11 0.09 0.22 4 2 11 -1.07 1.00 4 4 11 -1.15 -0.41 4 6 11 0.93 0.22 4 8 11 -1.28 2.13 4 10 11 0.29 -0.53 5 1 11 1.28 0.29 5 3 11 0.17 -1.62 5 5 11 0.33 -2.35 5 7 11 0.16 -1.55 5 9 11 -0.07 2.47 6 2 11 0.53 1.36 6 4 11 0.68 1.91 6 6 11 1.06 1.48 6 8 11 -1.05 -1.55 6 10 11 -0.59 -2.96 7 1 11 0.61 -0.07 7 3 11 -2.20 -2.09 7 5 11 -0.98 -2.92 7 7 11 1.51 1.08 7 9 11 1.20 4.24 8 2 11 1.30 0.30 8 4 11 2.04 0.68 8 6 11 0.94 -0.71 8 8 11 -1.70 -2.15 9 1 11 0.21 0.62 9 3 11 -1.77 -0.95 9 5 11 -0.17 0.38 9 7 11 2.62 1.18 9 9 11 0.98 1.03 10 2 11 -0.42 -1.28 10 4 11 -1.33 -1.77 10 6 11 0.36 -1.09 10 8 11 -0.92 0.95 11 1 11 0.78 -0.59 11 3 11 0.88 -0.70 11 5 11 1.49 1.10 11 7 11 1.99 -1.50 11 9 11 0.15 0.33 12 2 11 -1.80 0.49 12 4 11 -2.52 -0.39 12 6 11 0.54 0.75 12 8 11 0.07 1.26 13 1 11 1.62 -1.25 13 3 11 0.80 -1.70 13 5 11 0.42 -0.84 13 7 11 1.10 -0.83 13 9 11 0.27 1.07 14 2 11 -0.81 0.07 14 4 11 -0.15 2.13 14 6 11 0.87 0.85 14 8 11 0.15 0.01 15 1 11 1.29 1.49 15 3 11 0.40 -0.70 15 5 11 0.41 -0.47 15 7 11 0.64 0.01 16 2 11 1.21 -0.74 16 4 11 0.32 1.16 16 6 11 0.29 0.75 16 8 11 -0.29 1.03 17 1 11 0.63 0.51 17 3 11 1.41 0.03 17 5 11 2.16 1.38 17 7 11 0.37 -0.77 18 2 11 1.64 0.87 18 4 11 -0.21 0.43 18 6 11 -0.58 0.80 19 1 11 0.59 -0.90 19 3 11 1.84 -0.47 19 5 11 3.03 1.11 19 7 11 0.36 0.48 20 2 11 1.26 -0.28 20 4 11 -0.45 0.72 20 6 11 -1.38 0.46 21 1 11 -0.13 0.24 21 3 11 0.61 0.05 21 5 11 2.62 1.62 22 2 11 1.32 -1.14 22 4 11 -0.37 -0.88 23 1 11 -0.19 0.02 23 3 11 -0.46 0.52 0 2 12 -2.58 4.65 0 4 12 1.50 1.07 1 1 12 -0.21 -0.74 1 3 12 -2.27 0.45 1 5 12 0.26 -1.41 2 0 12 -2.18 1.53 2 2 12 -2.48 2.43 2 4 12 0.69 0.19 3 1 12 -1.21 1.70 3 3 12 -1.38 1.52 3 5 12 -1.81 -0.31 4 0 12 0.22 -3.13 4 2 12 -1.60 0.00 4 4 12 0.12 -0.62 5 1 12 -0.42 1.30 5 3 12 -2.11 1.46 5 5 12 -0.56 0.03 6 0 12 0.49 -2.39 6 2 12 -0.22 -1.09 6 4 12 -0.41 -0.41 7 1 12 0.64 -0.29 7 3 12 -1.23 0.54 7 5 12 1.93 -2.35 8 0 12 0.79 -1.46 8 2 12 -0.10 -0.64 8 4 12 -0.47 0.02 9 1 12 1.50 -0.21 9 3 12 0.66 -1.77 9 5 12 0.39 -3.04 10 0 12 0.68 -2.38 10 2 12 -0.17 0.16 10 4 12 1.41 -1.14 11 1 12 1.54 -0.05 11 3 12 0.44 -1.20 12 0 12 1.23 -2.13 12 2 12 0.81 -1.93 13 1 12 0.64 -0.19 13 3 12 -0.30 0.72 14 0 12 1.34 -3.70 34 0 0 8.93 2.53 35 1 0 -9.07 1.25 51 1 0 -2.31 0.89 51 3 0 -2.37 0.93 49 7 0 0.35 0.58 48 8 0 -2.14 0.31 44 12 0 4.20 1.09 43 13 0 0.05 0.29 42 14 0 -0.66 0.99 34 18 0 2.07 0.15 28 20 0 0.03 0.78 23 21 0 -0.26 -2.02 25 21 0 -0.69 -1.85 6 22 0 -1.79 1.09 8 22 0 0.62 -0.70 10 22 0 1.74 -1.02 12 22 0 -1.11 -1.18 14 22 0 -5.36 -0.02 16 22 0 -3.63 1.10 18 22 0 1.53 -1.35 20 22 0 0.37 -1.83 22 22 0 -2.16 0.31 1 23 0 -3.15 0.42 3 23 0 -2.49 0.73 5 23 0 2.90 -0.06 7 23 0 4.61 -0.19 9 23 0 0.79 0.74 11 23 0 -0.88 0.85 13 23 0 0.37 -0.66 15 23 0 0.83 -2.33 17 23 0 -0.44 -1.27 51 1 1 -0.87 0.62 5 3 1 -72.00 60.20 49 7 1 -1.02 2.40 48 8 1 -1.48 -1.39 44 12 1 -2.18 0.51 43 13 1 -0.03 -1.23 38 16 1 -2.05 -0.79 34 18 1 -0.56 3.92 23 21 1 0.73 -0.63 25 21 1 -0.37 0.85 4 22 1 -0.50 -5.54 6 22 1 -0.83 -3.09 8 22 1 -0.14 -3.61 10 22 1 -0.65 -4.30 12 22 1 -0.54 -0.71 14 22 1 -0.49 -1.32 16 22 1 -1.40 -4.08 18 22 1 0.58 -2.30 20 22 1 1.87 -0.03 1 23 1 5.37 -2.85 3 23 1 2.40 0.30 5 23 1 0.57 1.99 7 23 1 -0.67 -0.18 9 23 1 -0.89 -0.25 11 23 1 -0.27 -0.72 13 23 1 -0.87 -1.88 15 23 1 0.04 0.18 0 0 2 47.85 80.67 2 0 2 33.49 20.85 50 0 2 0.12 0.85 50 2 2 2.40 -0.69 50 4 2 -0.12 0.61 47 9 2 0.09 -0.73 46 10 2 1.69 -1.20 45 11 2 -0.57 0.84 44 12 2 0.39 -1.50 38 16 2 1.82 -0.18 31 19 2 0.40 -0.84 28 20 2 -0.97 1.40 21 21 2 -3.60 0.70 23 21 2 -4.94 -0.15 0 22 2 -1.27 -1.69 2 22 2 -1.49 -0.60 4 22 2 -2.20 -0.62 6 22 2 -0.03 0.11 8 22 2 4.19 1.11 10 22 2 1.97 -0.85 12 22 2 -1.75 -1.47 14 22 2 -0.70 -0.10 16 22 2 0.42 -0.28 18 22 2 -1.40 -1.60 20 22 2 -2.49 -2.34 1 23 2 0.35 -0.45 3 23 2 0.04 -1.57 5 23 2 0.53 -1.95 7 23 2 -0.47 -2.48 9 23 2 0.30 -0.94 11 23 2 3.63 1.35 13 23 2 3.12 -0.13 15 23 2 -0.30 -2.66 49 1 3 0.17 -0.14 49 3 3 0.53 1.18 48 6 3 0.10 0.03 40 14 3 -1.29 -2.59 32 18 3 0.25 -1.60 29 19 3 2.26 -0.01 26 20 3 -1.52 2.35 19 21 3 1.00 0.67 21 21 3 0.92 -0.03 23 21 3 -0.67 0.89 10 22 3 -0.18 -3.17 12 22 3 -1.30 -1.10 14 22 3 1.49 -2.69 16 22 3 1.76 -2.36 18 22 3 0.00 -0.83 1 23 3 1.35 2.54 3 23 3 2.01 -1.19 5 23 3 -0.16 -1.37 7 23 3 -0.82 0.47 9 23 3 0.87 -0.88 11 23 3 1.46 -2.52 48 2 4 1.91 0.46 48 4 4 -1.65 1.66 44 10 4 -0.06 -0.20 37 15 4 -1.92 0.31 33 17 4 -1.07 -0.79 30 18 4 -0.01 -0.49 27 19 4 -1.35 2.66 24 20 4 -1.13 0.47 17 21 4 -0.08 2.66 0 22 4 0.60 1.81 2 22 4 -1.51 0.31 4 22 4 -2.39 -0.46 6 22 4 -0.12 2.09 8 22 4 0.05 3.44 10 22 4 -0.01 1.72 12 22 4 -0.29 1.71 14 22 4 -0.40 1.16 1 23 4 -0.63 1.58 3 23 4 2.63 3.38 5 23 4 1.67 3.10 47 1 5 -0.76 0.71 46 4 5 0.69 0.11 44 8 5 -1.66 0.24 43 9 5 -0.21 -1.13 42 10 5 0.23 1.92 41 11 5 0.15 -0.20 35 15 5 0.96 -1.27 28 18 5 -0.52 -0.58 25 19 5 2.92 -1.09 15 21 5 -1.46 0.33 0 22 5 1.15 0.02 2 22 5 0.14 1.21 4 22 5 -1.32 1.71 6 22 5 -2.47 -0.65 8 22 5 -1.51 -0.93 45 1 6 1.69 -0.01 44 4 6 1.79 -0.44 42 8 6 -0.40 1.41 41 9 6 0.07 -1.22 40 10 6 0.44 -0.20 34 14 6 -0.57 2.08 30 16 6 2.25 -0.56 27 17 6 0.51 -1.08 24 18 6 2.78 -1.33 21 19 6 2.01 1.33 16 20 6 -0.82 3.26 1 21 6 2.54 0.75 3 21 6 0.70 -0.39 5 21 6 0.46 0.25 7 21 6 0.63 0.02 9 21 6 -0.89 0.21 42 4 7 0.53 -1.13 41 5 7 1.19 0.45 34 12 7 1.40 0.76 26 16 7 -1.31 -0.67 23 17 7 -0.74 -2.70 15 19 7 2.93 1.83 0 20 7 1.49 0.07 2 20 7 2.06 -0.38 4 20 7 1.56 -0.74 6 20 7 0.26 -0.32 39 1 8 1.08 0.04 39 3 8 -0.28 0.95 37 7 8 0.52 -0.06 36 8 8 0.54 0.29 35 9 8 -0.10 1.05 30 12 8 0.30 0.20 26 14 8 -2.69 0.35 23 15 8 -1.60 -1.31 20 16 8 -0.37 -2.24 17 17 8 0.18 -0.74 10 18 8 0.25 -0.03 12 18 8 -0.23 -0.89 35 1 9 -0.82 -0.75 35 3 9 -1.14 -0.45 34 4 9 -0.64 0.54 33 7 9 0.70 0.35 27 11 9 0.45 -0.86 23 13 9 -0.42 2.18 20 14 9 -1.56 -0.96 17 15 9 1.07 0.37 12 16 9 0.02 -0.24 1 17 9 -0.89 2.52 3 17 9 -0.84 1.83 31 1 10 0.06 0.65 30 4 10 0.42 -2.59 29 5 10 -2.18 1.07 28 6 10 2.69 -2.04 27 7 10 -1.86 1.71 26 8 10 0.76 -1.85 25 9 10 -1.44 -0.13 21 11 10 -0.61 -3.77 18 12 10 -0.72 0.06 15 13 10 0.35 0.71 8 14 10 1.23 1.47 10 14 10 0.48 1.04 25 1 11 0.52 0.04 24 2 11 0.14 -0.33 23 5 11 0.93 2.21 22 6 11 -0.88 0.08 18 8 11 -0.81 1.13 15 9 11 -0.03 0.59 8 10 11 -0.74 -1.65 10 10 11 0.12 -0.79 12 10 11 -0.80 -1.54 14 10 11 -1.31 -0.01 1 11 11 -0.12 -1.42 3 11 11 -1.23 0.10 5 11 11 -0.68 0.82 7 11 11 0.09 0.22 9 11 11 -0.60 -0.72 0 12 11 -2.29 2.15 2 12 11 -1.65 0.70 0 0 12 -4.78 5.29 16 0 12 0.72 -4.50 15 1 12 0.87 -0.36 14 2 12 1.27 -2.53 12 4 12 1.74 -2.56 11 5 12 -0.77 -1.67 0 6 12 0.40 0.43 2 6 12 1.88 0.66 4 6 12 1.64 -0.08 6 6 12 -1.95 0.40 8 6 12 -0.85 0.97 10 6 12 1.84 -0.87 1 7 12 0.91 1.61 3 7 12 -1.16 1.52 5 7 12 0.05 1.74 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 140621) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.164 -0.110 1373 389 ' ' 2 0.500 0.017 0.077 1373 389 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 5 3 1 8.848 0 0 2 7.968 2 0 2 8.207 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL a1_a.res in Cmc2(1) CELL 39.3660 18.6830 9.6770 90.00 90.00 90.00 SPGR Cmc21 # Solvent Accessible Volume = 2747 # Electrons Found in S.A.V. = 776 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 1.000 0.442 0.935 ! 5.66 eA-3 Q102 1.000 0.410 0.410 ! 5.06 eA-3 C103 1.000 0.314 0.759 ! 4.71 eA-3 C104 0.895 0.379 0.748 ! 4.52 eA-3 C105 0.384 0.075 0.066 ! 4.26 eA-3 C106 0.500 0.503 0.972 ! 3.79 eA-3 C107 0.601 0.097 0.145 ! 3.35 eA-3 C108 0.845 0.364 0.621 ! 2.43 eA-3 C109 0.932 0.451 0.685 ! 2.40 eA-3 Q110 0.500 0.047 0.587 ! 2.35 eA-3 C111 1.000 0.186 0.225 ! 2.20 eA-3 C112 1.000 0.202 0.139 ! 2.11 eA-3 C113 0.555 0.393 0.461 ! 2.06 eA-3 C114 1.000 0.204 0.075 ! 2.01 eA-3 C115 0.500 0.298 0.549 ! 1.99 eA-3 C116 0.104 0.475 0.423 ! 1.94 eA-3 C117 0.629 0.058 0.940 ! 1.91 eA-3 C118 0.952 0.120 0.056 ! 1.76 eA-3 C119 0.643 0.126 0.024 ! 1.72 eA-3 C120 0.499 0.379 0.528 ! 1.55 eA-3 C121 0.052 0.094 0.146 ! 1.52 eA-3 C122 0.993 0.070 0.033 ! 1.48 eA-3 C123 0.954 0.059 0.036 ! 1.44 eA-3 C124 0.022 0.175 0.070 ! 1.43 eA-3 C125 0.540 0.470 0.653 ! 1.09 eA-3 C126 0.999 0.491 0.810 ! 0.83 eA-3 C127 1.000 0.092 0.785 ! 0.78 eA-3 Q128 0.453 0.499 0.685 ! 0.77 eA-3 C129 0.486 0.371 0.697 ! 0.74 eA-3 Q130 0.477 0.499 0.651 ! 0.74 eA-3 Q131 0.978 0.046 0.661 ! 0.71 eA-3 C132 1.000 0.058 0.298 ! 0.71 eA-3 Q133 0.530 0.279 0.604 ! 0.70 eA-3 C134 1.000 0.048 0.729 ! 0.69 eA-3 Q135 0.978 0.063 0.782 ! 0.69 eA-3 Q136 0.918 0.467 0.134 ! 0.67 eA-3 Q137 0.631 0.080 0.383 ! 0.65 eA-3 C138 0.479 0.016 0.462 ! 0.64 eA-3 C139 0.482 0.484 0.723 ! 0.63 eA-3 Q140 0.845 0.436 0.508 ! 0.63 eA-3 C141 0.978 0.404 0.585 ! 0.61 eA-3 C142 0.505 0.112 0.313 ! 0.60 eA-3 Q143 0.485 0.375 0.833 ! 0.60 eA-3 C144 0.971 0.012 0.753 ! 0.59 eA-3 C145 0.965 0.437 0.749 ! 0.58 eA-3 C146 0.617 0.052 0.412 ! 0.56 eA-3 C147 1.003 0.030 0.182 ! 0.55 eA-3 Q148 0.867 0.363 0.384 ! 0.55 eA-3 Q149 0.039 0.022 0.605 ! 0.54 eA-3 Q150 0.864 0.404 0.946 ! 0.53 eA-3 C151 0.484 0.501 0.816 ! 0.52 eA-3 Q152 0.920 0.327 0.769 ! 0.52 eA-3 Q153 0.362 0.014-0.005 ! 0.52 eA-3 Q154 0.020 0.419 0.481 ! 0.52 eA-3 Q155 0.478 0.420 0.799 ! 0.50 eA-3 C156 0.099 0.462 0.708 ! 0.50 eA-3 ) ; _shelx_fab_checksum 53807 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, z+1/2' '-x, y, z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C17 C 0.64993(10) 0.6148(2) 0.6423(5) 0.0480(9) Uani 1 1 d . . . . . H17 H 0.650156 0.654485 0.703615 0.058 Uiso 1 1 calc R U . . . C16 C 0.67879(10) 0.57341(19) 0.6298(4) 0.0463(9) Uani 1 1 d . . . . . H16 H 0.698415 0.585750 0.681777 0.056 Uiso 1 1 calc R U . . . C6 C 0.74078(9) 0.35243(18) 0.4971(4) 0.0414(8) Uani 1 1 d . . . . . C14 C 0.74667(10) 0.5719(2) 0.4398(5) 0.0505(9) Uani 1 1 d . . . . . H14 H 0.727669 0.586829 0.386612 0.061 Uiso 1 1 calc R U . . . C9 C 0.74386(9) 0.51059(19) 0.5239(4) 0.0426(8) Uani 1 1 d . . . . . C15 C 0.67989(9) 0.51396(19) 0.5430(4) 0.0419(8) Uani 1 1 d . . . . . C4 C 0.78637(11) 0.3153(2) 0.3473(5) 0.0549(10) Uani 1 1 d . . . . . H4 H 0.798991 0.321678 0.264521 0.066 Uiso 1 1 calc R U . . . C5 C 0.76043(10) 0.3612(2) 0.3763(4) 0.0478(9) Uani 1 1 d . . . . . H5 H 0.755528 0.399393 0.314677 0.057 Uiso 1 1 calc R U . . . C7 C 0.71060(9) 0.39715(18) 0.5281(4) 0.0416(7) Uani 1 1 d . . . . . C10 C 0.77156(10) 0.4928(2) 0.6009(5) 0.0515(10) Uani 1 1 d . . . . . H10 H 0.770261 0.452330 0.660196 0.062 Uiso 1 1 calc R U . . . C24 C 0.67974(9) 0.35384(19) 0.5604(4) 0.0420(8) Uani 1 1 d . . . . . C20 C 0.65059(10) 0.4989(2) 0.4671(5) 0.0499(9) Uani 1 1 d . . . . . H20 H 0.650396 0.459067 0.406087 0.060 Uiso 1 1 calc R U . . . C1 C 0.74942(10) 0.2958(2) 0.5845(4) 0.0476(9) Uani 1 1 d . . . . . H1 H 0.736533 0.288303 0.666228 0.057 Uiso 1 1 calc R U . . . C26 C 0.63262(11) 0.3220(2) 0.7107(5) 0.0561(11) Uani 1 1 d . . . . . H26 H 0.619761 0.330713 0.792037 0.067 Uiso 1 1 calc R U . . . C25 C 0.66014(10) 0.3658(2) 0.6805(4) 0.0484(9) Uani 1 1 d . . . . . H25 H 0.665817 0.403969 0.740947 0.058 Uiso 1 1 calc R U . . . C29 C 0.67075(10) 0.2968(2) 0.4751(5) 0.0489(9) Uani 1 1 d . . . . . H29 H 0.683954 0.286859 0.395189 0.059 Uiso 1 1 calc R U . . . C8 C 0.71147(9) 0.47002(17) 0.5302(4) 0.0411(7) Uani 1 1 d . . . . . C18 C 0.62072(10) 0.6003(2) 0.5685(5) 0.0521(10) Uani 1 1 d . . . . . C27 C 0.62348(10) 0.2657(2) 0.6245(5) 0.0568(10) Uani 1 1 d . . . . . C28 C 0.64244(10) 0.2538(2) 0.5055(5) 0.0570(11) Uani 1 1 d . . . . . H28 H 0.636217 0.216224 0.444354 0.068 Uiso 1 1 calc R U . . . C2 C 0.77610(11) 0.2503(2) 0.5555(5) 0.0587(11) Uani 1 1 d . . . . . H2 H 0.781555 0.212839 0.618068 0.070 Uiso 1 1 calc R U . . . N1A N 0.5547(5) 0.7263(11) 0.667(3) 0.082(6) Uani 0.54(4) 1 d . . P B 2 C3 C 0.79494(12) 0.2589(2) 0.4363(6) 0.0625(12) Uani 1 1 d . . . . . H3A H 0.813201 0.227535 0.415147 0.075 Uiso 1 1 calc R U . . . C11 C 0.80116(11) 0.5309(3) 0.5959(5) 0.0620(11) Uani 1 1 d . . . . . H11 H 0.819978 0.516111 0.650325 0.074 Uiso 1 1 calc R U . . . C19 C 0.62192(11) 0.5408(2) 0.4793(5) 0.0580(11) Uani 1 1 d . . . . . H19 H 0.602415 0.529249 0.425948 0.070 Uiso 1 1 calc R U . . . C13 C 0.77638(12) 0.6105(2) 0.4331(6) 0.0634(12) Uani 1 1 d . . . . . H13 H 0.778044 0.650974 0.373986 0.076 Uiso 1 1 calc R U . . . C12 C 0.80402(12) 0.5899(2) 0.5139(6) 0.0659(12) Uani 1 1 d . . . . . H12 H 0.824561 0.616546 0.511707 0.079 Uiso 1 1 calc R U . . . N3A N 0.5529(6) 0.1745(18) 0.813(4) 0.073(6) Uani 0.30(4) 1 d D . P A 2 H3AA H 0.538146 0.164131 0.877826 0.087 Uiso 0.30(4) 1 calc R U P A 2 N4A N 0.5526(6) 0.1443(15) 0.687(4) 0.064(7) Uani 0.30(4) 1 d D . P A 2 C31A C 0.5786(6) 0.1731(13) 0.613(4) 0.059(6) Uani 0.30(4) 1 d . . P A 2 H31A H 0.584071 0.161626 0.519674 0.071 Uiso 0.30(4) 1 calc R U P A 2 C30A C 0.5952(7) 0.2204(14) 0.692(3) 0.041(5) Uani 0.30(4) 1 d . . P A 2 C32A C 0.5785(6) 0.2229(13) 0.829(4) 0.061(5) Uani 0.30(4) 1 d . . P A 2 H32A H 0.584170 0.251007 0.907361 0.073 Uiso 0.30(4) 1 calc R U P A 2 C23A C 0.5562(4) 0.6237(12) 0.557(3) 0.076(6) Uani 0.54(4) 1 d . . P B 2 H23A H 0.549315 0.581292 0.510319 0.091 Uiso 0.54(4) 1 calc R U P B 2 N2A N 0.5361(4) 0.6821(10) 0.591(3) 0.089(6) Uani 0.54(4) 1 d . . P B 2 H2A H 0.514811 0.688641 0.566540 0.107 Uiso 0.54(4) 1 calc R U P B 2 C21A C 0.5898(5) 0.6413(13) 0.607(3) 0.060(5) Uani 0.54(4) 1 d . . P B 2 C22A C 0.5862(5) 0.7065(11) 0.677(3) 0.065(5) Uani 0.54(4) 1 d . . P B 2 H22A H 0.603744 0.731718 0.723829 0.078 Uiso 0.54(4) 1 calc R U P B 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 C17 0.043(2) 0.043(2) 0.058(2) -0.0084(17) 0.0021(18) -0.0015(16) C16 0.042(2) 0.043(2) 0.054(2) -0.0025(18) -0.0042(16) -0.0012(16) C6 0.040(2) 0.0347(18) 0.049(2) -0.0007(15) 0.0012(15) 0.0007(15) C14 0.046(2) 0.042(2) 0.063(2) 0.0066(18) 0.0071(19) 0.0004(17) C9 0.0407(19) 0.0393(19) 0.048(2) -0.0069(16) 0.0024(17) 0.0004(15) C15 0.0382(19) 0.0358(19) 0.052(2) 0.0019(16) 0.0013(16) 0.0007(14) C4 0.048(2) 0.058(3) 0.058(2) -0.0099(19) 0.0071(18) -0.0054(19) C5 0.049(2) 0.044(2) 0.050(2) -0.0002(16) 0.0025(17) 0.0026(17) C7 0.0395(18) 0.0380(17) 0.0473(17) -0.0014(17) 0.0011(14) 0.0007(16) C10 0.048(2) 0.047(2) 0.060(2) 0.0001(18) 0.0008(19) -0.0003(18) C24 0.042(2) 0.0394(19) 0.0443(19) 0.0028(15) -0.0031(15) -0.0033(15) C20 0.050(2) 0.046(2) 0.054(2) -0.0037(17) -0.0025(18) -0.0009(18) C1 0.045(2) 0.045(2) 0.053(2) 0.0001(17) 0.0022(17) -0.0032(16) C26 0.049(2) 0.057(3) 0.062(2) 0.004(2) 0.0071(19) 0.001(2) C25 0.046(2) 0.045(2) 0.055(2) 0.0014(17) 0.0031(17) -0.0025(17) C29 0.049(2) 0.039(2) 0.058(2) 0.0033(17) -0.0012(18) -0.0014(17) C8 0.0406(18) 0.0370(17) 0.0459(16) 0.0028(17) 0.0002(14) -0.0004(15) C18 0.044(2) 0.044(2) 0.068(2) -0.0007(19) 0.0027(18) -0.0005(16) C27 0.045(2) 0.046(2) 0.080(3) 0.011(2) 0.000(2) -0.0021(16) C28 0.049(2) 0.045(2) 0.076(3) 0.003(2) -0.002(2) -0.0025(18) C2 0.056(2) 0.043(2) 0.078(3) 0.006(2) -0.002(2) 0.0030(19) N1A 0.054(5) 0.060(7) 0.133(15) -0.021(8) -0.014(8) 0.001(4) C3 0.054(3) 0.052(3) 0.081(3) -0.009(2) -0.002(2) 0.012(2) C11 0.049(2) 0.063(3) 0.073(3) -0.003(2) -0.001(2) -0.004(2) C19 0.041(2) 0.056(2) 0.076(3) -0.008(2) -0.007(2) 0.0002(19) C13 0.064(3) 0.047(2) 0.079(3) -0.001(2) 0.010(2) -0.007(2) C12 0.055(3) 0.056(3) 0.087(3) -0.007(3) 0.003(2) -0.014(2) N3A 0.065(9) 0.078(12) 0.075(12) 0.005(9) 0.017(8) -0.024(8) N4A 0.042(8) 0.071(12) 0.078(15) 0.001(9) 0.000(9) -0.013(7) C31A 0.048(8) 0.068(9) 0.060(12) -0.010(9) 0.002(8) -0.015(7) C30A 0.032(7) 0.040(7) 0.051(11) 0.008(7) -0.007(7) 0.004(5) C32A 0.061(9) 0.057(10) 0.063(11) -0.007(8) 0.009(8) -0.010(7) C23A 0.044(4) 0.071(8) 0.113(14) -0.034(9) -0.004(7) -0.001(5) N2A 0.044(4) 0.095(8) 0.128(15) -0.046(9) -0.009(7) 0.009(5) C21A 0.037(4) 0.063(7) 0.078(13) -0.014(8) 0.004(6) -0.004(4) C22A 0.052(5) 0.067(7) 0.076(13) -0.016(8) -0.002(7) -0.002(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' N N 0.0241 0.0134 '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 C16 C17 H17 119.0 . . ? C16 C17 C18 122.1(4) . . ? C18 C17 H17 119.0 . . ? C17 C16 H16 119.2 . . ? C17 C16 C15 121.6(3) . . ? C15 C16 H16 119.2 . . ? C5 C6 C7 122.8(3) . . ? C1 C6 C5 117.1(3) . . ? C1 C6 C7 120.0(3) . . ? C9 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C13 C14 C9 121.4(4) . . ? C14 C9 C8 120.4(3) . . ? C10 C9 C14 116.9(4) . . ? C10 C9 C8 122.7(3) . . ? C16 C15 C20 116.9(3) . . ? C16 C15 C8 120.9(3) . . ? C20 C15 C8 122.2(3) . . ? C5 C4 H4 119.1 . . ? C5 C4 C3 121.8(4) . . ? C3 C4 H4 119.1 . . ? C6 C5 H5 119.7 . . ? C4 C5 C6 120.6(4) . . ? C4 C5 H5 119.7 . . ? C6 C7 C24 112.9(3) . . ? C8 C7 C6 123.1(3) . . ? C8 C7 C24 124.0(3) . . ? C9 C10 H10 118.8 . . ? C9 C10 C11 122.4(4) . . ? C11 C10 H10 118.8 . . ? C25 C24 C7 122.1(3) . . ? C29 C24 C7 119.8(3) . . ? C29 C24 C25 118.0(3) . . ? C15 C20 H20 119.4 . . ? C19 C20 C15 121.1(4) . . ? C19 C20 H20 119.4 . . ? C6 C1 H1 119.0 . . ? C2 C1 C6 121.9(4) . . ? C2 C1 H1 119.0 . . ? C25 C26 H26 119.3 . . ? C25 C26 C27 121.4(4) . . ? C27 C26 H26 119.3 . . ? C24 C25 H25 119.8 . . ? C26 C25 C24 120.5(4) . . ? C26 C25 H25 119.8 . . ? C24 C29 H29 119.5 . . ? C24 C29 C28 121.0(4) . . ? C28 C29 H29 119.5 . . ? C9 C8 C15 115.9(3) . . ? C7 C8 C9 122.1(3) . . ? C7 C8 C15 121.9(3) . . ? C17 C18 C19 116.4(4) . . ? C17 C18 C21A 116.8(9) . . ? C19 C18 C21A 126.0(9) . . ? C26 C27 C28 118.7(4) . . ? C26 C27 C30A 110.4(12) . . ? C28 C27 C30A 130.5(12) . . ? C29 C28 H28 119.8 . . ? C27 C28 C29 120.5(4) . . ? C27 C28 H28 119.8 . . ? C1 C2 H2 119.8 . . ? C1 C2 C3 120.4(4) . . ? C3 C2 H2 119.8 . . ? C22A N1A N2A 112.9(14) . . ? C4 C3 H3A 120.9 . . ? C2 C3 C4 118.1(4) . . ? C2 C3 H3A 120.9 . . ? C10 C11 H11 119.6 . . ? C12 C11 C10 120.8(4) . . ? C12 C11 H11 119.6 . . ? C20 C19 C18 121.9(4) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C14 C13 H13 120.3 . . ? C14 C13 C12 119.5(4) . . ? C12 C13 H13 120.3 . . ? C11 C12 C13 119.1(4) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? N4A N3A H3AA 123.5 . . ? N4A N3A C32A 113(2) . . ? C32A N3A H3AA 123.5 . . ? N3A N4A C31A 108(2) . . ? N4A C31A H31A 125.5 . . ? C30A C31A N4A 109(2) . . ? C30A C31A H31A 125.5 . . ? C31A C30A C27 118(2) . . ? C31A C30A C32A 108.5(19) . . ? C32A C30A C27 132.9(18) . . ? N3A C32A C30A 101.8(17) . . ? N3A C32A H32A 129.1 . . ? C30A C32A H32A 129.1 . . ? N2A C23A H23A 127.4 . . ? N2A C23A C21A 105.2(15) . . ? C21A C23A H23A 127.4 . . ? N1A N2A C23A 108.0(13) . . ? N1A N2A H2A 126.0 . . ? C23A N2A H2A 126.0 . . ? C23A C21A C18 123.2(16) . . ? C22A C21A C18 130.8(17) . . ? C22A C21A C23A 105.5(15) . . ? N1A C22A C21A 108.0(14) . . ? N1A C22A H22A 126.0 . . ? C21A C22A H22A 126.0 . . ? 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 C17 H17 0.9500 . ? C17 C16 1.379(5) . ? C17 C18 1.380(6) . ? C16 H16 0.9500 . ? C16 C15 1.394(5) . ? C6 C5 1.411(5) . ? C6 C7 1.483(5) . ? C6 C1 1.397(5) . ? C14 H14 0.9500 . ? C14 C9 1.409(5) . ? C14 C13 1.376(6) . ? C9 C10 1.362(5) . ? C9 C8 1.485(5) . ? C15 C20 1.396(5) . ? C15 C8 1.495(5) . ? C4 H4 0.9500 . ? C4 C5 1.363(6) . ? C4 C3 1.401(6) . ? C5 H5 0.9500 . ? C7 C24 1.493(5) . ? C7 C8 1.362(5) . ? C10 H10 0.9500 . ? C10 C11 1.367(6) . ? C24 C25 1.412(5) . ? C24 C29 1.394(5) . ? C20 H20 0.9500 . ? C20 C19 1.379(6) . ? C1 H1 0.9500 . ? C1 C2 1.379(6) . ? C26 H26 0.9500 . ? C26 C25 1.388(6) . ? C26 C27 1.389(6) . ? C25 H25 0.9500 . ? C29 H29 0.9500 . ? C29 C28 1.405(6) . ? C18 C19 1.407(6) . ? C18 C21A 1.486(19) . ? C27 C28 1.390(7) . ? C27 C30A 1.54(3) . ? C28 H28 0.9500 . ? C2 H2 0.9500 . ? C2 C3 1.382(7) . ? N1A N2A 1.328(18) . ? N1A C22A 1.30(2) . ? C3 H3A 0.9500 . ? C11 H11 0.9500 . ? C11 C12 1.363(7) . ? C19 H19 0.9500 . ? C13 H13 0.9500 . ? C13 C12 1.394(7) . ? C12 H12 0.9500 . ? N3A H3AA 0.8800 . ? N3A N4A 1.34(2) . ? N3A C32A 1.36(3) . ? N4A C31A 1.36(3) . ? C31A H31A 0.9500 . ? C31A C30A 1.34(3) . ? C30A C32A 1.48(3) . ? C32A H32A 0.9500 . ? C23A H23A 0.9500 . ? C23A N2A 1.39(2) . ? C23A C21A 1.45(2) . ? N2A H2A 0.8800 . ? C21A C22A 1.40(2) . ? C22A H22A 0.9500 . ? 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 C17 C16 C15 C20 1.1(5) . . . . ? C17 C16 C15 C8 179.7(3) . . . . ? C17 C18 C19 C20 0.6(6) . . . . ? C17 C18 C21A C23A -168.8(13) . . . . ? C17 C18 C21A C22A 21(2) . . . . ? C16 C17 C18 C19 -0.1(6) . . . . ? C16 C17 C18 C21A 170.6(13) . . . . ? C16 C15 C20 C19 -0.6(6) . . . . ? C16 C15 C8 C9 -41.3(5) . . . . ? C16 C15 C8 C7 137.1(4) . . . . ? C6 C7 C24 C25 128.5(4) . . . . ? C6 C7 C24 C29 -47.5(5) . . . . ? C6 C7 C8 C9 -10.1(6) . . . . ? C6 C7 C8 C15 171.6(3) . . . . ? C6 C1 C2 C3 -1.2(7) . . . . ? C14 C9 C10 C11 -1.4(6) . . . . ? C14 C9 C8 C15 -44.4(5) . . . . ? C14 C9 C8 C7 137.2(4) . . . . ? C14 C13 C12 C11 1.2(7) . . . . ? C9 C14 C13 C12 -1.7(6) . . . . ? C9 C10 C11 C12 1.0(7) . . . . ? C15 C20 C19 C18 -0.3(7) . . . . ? C5 C6 C7 C24 127.5(4) . . . . ? C5 C6 C7 C8 -54.1(6) . . . . ? C5 C6 C1 C2 0.5(6) . . . . ? C5 C4 C3 C2 0.5(7) . . . . ? C7 C6 C5 C4 -175.0(4) . . . . ? C7 C6 C1 C2 176.3(4) . . . . ? C7 C24 C25 C26 -176.7(4) . . . . ? C7 C24 C29 C28 178.0(4) . . . . ? C10 C9 C8 C15 133.3(4) . . . . ? C10 C9 C8 C7 -45.1(6) . . . . ? C10 C11 C12 C13 -0.8(7) . . . . ? C24 C7 C8 C9 168.1(3) . . . . ? C24 C7 C8 C15 -10.2(6) . . . . ? C24 C29 C28 C27 -2.3(6) . . . . ? C20 C15 C8 C9 137.2(4) . . . . ? C20 C15 C8 C7 -44.4(6) . . . . ? C1 C6 C5 C4 0.7(5) . . . . ? C1 C6 C7 C24 -48.0(5) . . . . ? C1 C6 C7 C8 130.3(4) . . . . ? C1 C2 C3 C4 0.7(7) . . . . ? C26 C27 C28 C29 1.5(6) . . . . ? C26 C27 C30A C31A 166.6(18) . . . . ? C26 C27 C30A C32A -5(3) . . . . ? C25 C24 C29 C28 1.8(5) . . . . ? C25 C26 C27 C28 -0.2(6) . . . . ? C25 C26 C27 C30A 172.6(12) . . . . ? C29 C24 C25 C26 -0.6(6) . . . . ? C8 C9 C10 C11 -179.1(4) . . . . ? C8 C15 C20 C19 -179.1(4) . . . . ? C8 C7 C24 C25 -49.8(6) . . . . ? C8 C7 C24 C29 134.2(4) . . . . ? C18 C17 C16 C15 -0.8(6) . . . . ? C18 C21A C22A N1A 170.1(19) . . . . ? C27 C26 C25 C24 -0.2(6) . . . . ? C27 C30A C32A N3A 172(3) . . . . ? C28 C27 C30A C31A -22(3) . . . . ? C28 C27 C30A C32A 167.2(19) . . . . ? C3 C4 C5 C6 -1.2(6) . . . . ? C19 C18 C21A C23A 1(2) . . . . ? C19 C18 C21A C22A -169.4(14) . . . . ? C13 C14 C9 C10 1.8(6) . . . . ? C13 C14 C9 C8 179.6(4) . . . . ? N3A N4A C31A C30A 1(3) . . . . ? N4A N3A C32A C30A 0(3) . . . . ? N4A C31A C30A C27 -174(2) . . . . ? N4A C31A C30A C32A 0(3) . . . . ? C31A C30A C32A N3A 0(3) . . . . ? C30A C27 C28 C29 -169.7(15) . . . . ? C32A N3A N4A C31A -1(4) . . . . ? C23A C21A C22A N1A -1(2) . . . . ? N2A N1A C22A C21A -3(2) . . . . ? N2A C23A C21A C18 -167.6(18) . . . . ? N2A C23A C21A C22A 4.7(19) . . . . ? C21A C18 C19 C20 -169.1(14) . . . . ? C21A C23A N2A N1A -6(2) . . . . ? C22A N1A N2A C23A 6(2) . . . . ?