#------------------------------------------------------------------------------ #$Date: 2021-08-05 04:20:23 +0300 (Thu, 05 Aug 2021) $ #$Revision: 267955 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/79/7707954.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_7707954 loop_ _publ_author_name 'Fetrow, Taylor V.' 'Daly, Scott R.' _publ_section_title ; Mechanochemical synthesis and structural analysis of trivalent lanthanide and uranium diphenylphosphinodiboranates ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01932E _journal_year 2021 _chemical_formula_moiety 'C72 H96 B12 P6 U2' _chemical_formula_sum 'C72 H96 B12 P6 U2' _chemical_formula_weight 1753.08 _chemical_name_common U(Ph-PDB)3_dimer _chemical_name_systematic U2(BH3Ph2BH3)6 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-09-04 _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2021-06-09 deposited with the CCDC. 2021-07-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.622(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 18.8498(19) _cell_length_b 9.6187(10) _cell_length_c 23.960(2) _cell_measurement_reflns_used 6131 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 21.745 _cell_measurement_theta_min 2.3015 _cell_volume 4091.9(7) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker Nonius Kappa Apex II' _diffrn_measurement_method 'CCD Phi and Omega Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_unetI/netI 0.0674 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 47507 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.446 _diffrn_reflns_theta_min 2.396 _exptl_absorpt_coefficient_mu 4.107 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0648 before and 0.0528 after correction. The Ratio of minimum to maximum transmission is 0.8731. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour orange-red _exptl_crystal_density_diffrn 1.423 _exptl_crystal_description plate-like _exptl_crystal_F_000 1724 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.076 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.662 _refine_diff_density_min -1.989 _refine_diff_density_rms 0.143 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 399 _refine_ls_number_reflns 8365 _refine_ls_number_restraints 625 _refine_ls_restrained_S_all 1.074 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0474 _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^)+(0.0407P)^2^+16.1993P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.1143 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5566 _reflns_number_total 8365 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01932e2.cif _cod_data_source_block dal1929 _cod_database_code 7707954 _shelx_shelxl_version_number 2014/7 _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 0.922 _shelx_estimated_absorpt_t_min 0.661 _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 B(H,H,H) groups 2. Restrained distances P2A-C19A = P2A-C13A = P2-C13 1.9 with sigma of 0.01 C31-C32 \\sim C32-C33 \\sim C33-C34 \\sim C34-C35 \\sim C36-C31 \\sim C25-C26 \\sim C26-C27 \\sim C27-C28 \\sim C28-C29 \\sim C29-C30 \\sim C25-C30 \\sim C25-C26A \\sim C26A-C27A \\sim C27A-C28 \\sim C28-C29A ~ C29A-C30A \\sim C25-C30A \\sim C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C1-C6 \\sim C7-C8A \\sim C8A-C9A \\sim C9A-C10A \\sim C10A-C11A \\sim C11A-C12A \\sim C7-C12A \\sim C19-C20 \\sim C20-C21 ~ C21-C22 \\sim C22-C23 \\sim C23-C24 \\sim C19-C24 with sigma of 0.02 3. Restrained planarity C13, C14, C15, C16, C17, C18 with sigma of 0.02 C13A, C14A, C15A, C16A, C17A, C18A with sigma of 0.02 C25, C28, C26, C27, C29, C30 with sigma of 0.02 C25, C28, C26A, C27A, C29A, C30A with sigma of 0.02 C7, C8A, C9A, C10A, C11A, C12A with sigma of 0.02 4. Uiso/Uaniso restraints and constraints B3 \\sim B4 \\sim B3A \\sim B4A: within 1.7A with sigma of 0.05 and sigma for terminal atoms of 0.1 Uanis(B3) = Uanis(B4) = Uanis(B3A) = Uanis(B4A) Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24) Uanis(C19A) = Uanis(C20A) = Uanis(C21A) = Uanis(C22A) = Uanis(C23A) = Uanis(C24A) Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C13A) = Uanis(C14A) = Uanis(C15A) = Uanis(C16A) = Uanis(C17A) = Uanis(C18A) Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6) Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C8A) = Uanis(C9A) = Uanis(C10A) = Uanis(C11A) = Uanis(C12A) 5. Others Sof(H28A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(H27A)=Sof(C29A)=Sof(H29A)= Sof(C30A)=Sof(H30A)=1-FVAR(1) Sof(H28)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C29)=Sof(H29)=Sof(C30)= Sof(H30)=FVAR(1) Sof(C13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)= Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=1-FVAR(2) Sof(C13)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)= Sof(H17)=Sof(C18)=Sof(H18)=FVAR(2) Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)= Sof(C12A)=Sof(H12A)=1-FVAR(3) Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(C12)= Sof(H12)=FVAR(3) Sof(P2A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)= Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(B3A)=Sof(H3AA)=Sof(H3AB)= Sof(H3AC)=Sof(B4A)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=1-FVAR(4) Sof(P2)=Sof(C19)=Sof(C20)=Sof(H20)=Sof(C21)=Sof(H21)=Sof(C22)=Sof(H22)= Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(B3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=Sof(B4)= Sof(H4A)=Sof(H4B)=Sof(H4C)=FVAR(4) 6.a : C1(C2,C3,C4,C5,C6), C31(C32,C33,C34,C35,C36) 6.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C28(H28), C28(H28A), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C14A(H14A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A), C24A(H24A), C26A(H26A), C27A(H27A), C29A(H29A), C30A(H30A) 6.c Idealised Me refined as rotating group: B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B5(H5A,H5B,H5C), B6(H6A,H6B,H6C), B3(H3A, H3B,H3C), B4(H4A,H4B,H4C), B3A(H3AA,H3AB,H3AC), B4A(H4AA,H4AB,H4AC) ; _shelx_res_file ; dal1929.res created by SHELXL-2014/7 TITL dal1929_a.res in P2(1)/c REM Old TITL dal1929_a.res in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.218, Rweak 0.006, Alpha 0.092, Orientation as input REM Formula found by SHELXT: C39 O7 P3 U CELL 0.71073 18.8498 9.6187 23.96 90 109.622 90 ZERR 2 0.0019 0.001 0.002 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B P U UNIT 144 192 24 12 4 EQIV $1 1-X,1-Y,1-Z DFIX 1.9 0.01 P2A C19A P2A C13A P2 C13 SADI C31 C32 C32 C33 C33 C34 C34 C35 C36 C31 C25 C26 C26 C27 C27 C28 C28 = C29 C29 C30 C25 C30 C25 C26A C26A C27A C27A C28 C28 C29A C29A C30A C25 C30A = C1 C2 C2 C3 C3 C4 C4 C5 C5 C6 C1 C6 C7 C8A C8A C9A C9A C10A C10A C11A C11A = C12A C7 C12A C19 C20 C20 C21 C21 C22 C22 C23 C23 C24 C19 C24 FLAT 0.02 C13 C14 C15 C16 C17 C18 FLAT 0.02 C13A C14A C15A C16A C17A C18A FLAT 0.02 C25 C28 C26 C27 C29 C30 FLAT 0.02 C25 C28 C26A C27A C29A C30A FLAT 0.02 C7 C8A C9A C10A C11A C12A SIMU 0.05 0.1 1.7 B3 B4 B3A B4A EADP B3 B4 B3A B4A EADP C19 C20 C21 C22 C23 C24 EADP C19A C20A C21A C22A C23A C24A EADP C13 C14 C15 C16 C17 C18 C13A C14A C15A C16A C17A C18A EADP C1 C2 C3 C4 C5 C6 EADP C7 C8 C9 C10 C11 C12 C8A C9A C10A C11A C12A L.S. 10 PLAN 40 SIZE 0.02 0.076 0.11 TEMP -123 FREE B4A U1 FREE B3 U1 FREE B6 U1_$1 FREE B1 U1 FREE B5 U1 FREE B2 U1 FREE B3A U1 FREE B4 U1 BOND $H list 4 fmap 2 acta OMIT 0 0 2 OMIT 1 0 0 OMIT -1 0 2 REM REM REM WGHT 0.040700 16.199301 FVAR 0.22116 0.55535 0.51722 0.66519 0.46108 U1 5 0.303306 0.511807 0.441765 11.00000 0.01639 0.02458 = 0.04751 -0.00084 -0.00332 0.00200 P1 4 0.195003 0.314398 0.311135 11.00000 0.03443 0.03006 = 0.05325 0.00332 -0.01654 -0.00385 P3 4 0.509334 0.724631 0.419278 11.00000 0.01935 0.02526 = 0.03334 -0.00381 0.00146 0.00368 AFIX 9 1.3900 C1 1 0.108768 0.383242 0.257500 11.00000 0.06268 0.09068 = 0.11524 0.03812 -0.02357 -0.00055 C2 1 0.113456 0.477810 0.215887 11.00000 0.06268 0.09068 = 0.11524 0.03812 -0.02357 -0.00055 AFIX 43 H2 2 0.161286 0.510009 0.216327 11.00000 -1.20000 AFIX 5 1.3900 C3 1 0.048973 0.525838 0.173626 11.00000 0.06268 0.09068 = 0.11524 0.03812 -0.02357 -0.00055 AFIX 43 H3 2 0.052240 0.591167 0.144851 11.00000 -1.20000 AFIX 5 1.3900 C4 1 -0.020268 0.479298 0.173009 11.00000 0.06268 0.09068 = 0.11524 0.03812 -0.02357 -0.00055 AFIX 43 H4 2 -0.064845 0.512533 0.143829 11.00000 -1.20000 AFIX 5 1.3900 C5 1 -0.024966 0.384700 0.214612 11.00000 0.06268 0.09068 = 0.11524 0.03812 -0.02357 -0.00055 AFIX 43 H5 2 -0.072799 0.352498 0.214163 11.00000 -1.20000 AFIX 5 1.3900 C6 1 0.039507 0.336652 0.256873 11.00000 0.06268 0.09068 = 0.11524 0.03812 -0.02357 -0.00055 AFIX 43 H6 2 0.036238 0.271294 0.285637 11.00000 -1.20000 AFIX 0 C7 1 0.212742 0.146133 0.283307 11.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 C25 1 0.511218 0.673664 0.346498 11.00000 0.02438 0.02928 = 0.03843 -0.00389 0.00193 0.00474 C28 1 0.514793 0.587020 0.237834 11.00000 0.08483 0.06742 = 0.07166 -0.02655 0.04978 -0.00913 PART 1 AFIX 43 H28 2 0.515396 0.555913 0.200365 21.00000 -1.20000 AFIX 43 PART 0 PART 2 H28A 2 0.516245 0.559648 0.200137 -21.00000 -1.20000 AFIX 9 PART 0 C31 1 0.505718 0.913440 0.418680 11.00000 0.02559 0.02342 = 0.03481 -0.00725 0.00882 -0.00030 C32 1 0.437019 0.980103 0.401100 11.00000 0.02652 0.03238 = 0.05087 0.00092 0.00800 0.00473 AFIX 43 H32 2 0.391885 0.927587 0.392166 11.00000 -1.20000 AFIX 5 C33 1 0.433791 1.122913 0.396480 11.00000 0.04182 0.03100 = 0.06516 -0.00208 0.02196 0.01212 AFIX 43 H33 2 0.386435 1.168870 0.384400 11.00000 -1.20000 AFIX 5 C34 1 0.499242 1.199059 0.409380 11.00000 0.07567 0.02470 = 0.08071 -0.01556 0.04512 -0.01032 AFIX 43 H34 2 0.497018 1.297518 0.406142 11.00000 -1.20000 AFIX 5 C35 1 0.567931 1.132396 0.426980 11.00000 0.03653 0.03828 = 0.10899 -0.03494 0.03587 -0.01499 AFIX 43 H35 2 0.613065 1.184914 0.435916 11.00000 -1.20000 AFIX 5 C36 1 0.571169 0.989607 0.431619 11.00000 0.02431 0.03631 = 0.08716 -0.02379 0.01379 -0.00412 AFIX 43 H36 2 0.618531 0.943666 0.443741 11.00000 -1.20000 AFIX 0 B1 3 0.187005 0.302432 0.388230 11.00000 0.03982 0.03798 = 0.06291 -0.00215 -0.00844 -0.00928 AFIX 137 1.2000 H1A 2 0.246713 0.269069 0.423275 11.00000 0.04627 H1B 2 0.140413 0.217241 0.388035 11.00000 0.05905 H1C 2 0.168854 0.413454 0.401903 11.00000 0.02433 AFIX 0 B2 3 0.278104 0.438555 0.318619 11.00000 0.03478 0.03957 = 0.04549 -0.00264 -0.00887 -0.00499 AFIX 137 1.2000 H2A 2 0.262937 0.552583 0.331543 11.00000 0.04943 H2B 2 0.289668 0.443719 0.272372 11.00000 0.08990 H2C 2 0.333386 0.396576 0.356595 11.00000 0.05751 AFIX 0 B5 3 0.419906 0.650015 0.427900 11.00000 0.02379 0.02348 = 0.04145 -0.00276 0.00256 0.00097 AFIX 137 1.2000 H5A 2 0.413288 0.692278 0.473019 11.00000 0.05620 H5B 2 0.423725 0.525463 0.429466 11.00000 0.04662 H5C 2 0.366403 0.685329 0.386644 11.00000 0.03414 AFIX 0 B6 3 0.597962 0.651599 0.477020 11.00000 0.02201 0.03564 = 0.03563 -0.00576 0.00485 0.01082 AFIX 137 1.2000 H6A 2 0.596964 0.527015 0.474214 11.00000 0.05165 H6B 2 0.600040 0.687110 0.525557 11.00000 0.05887 H6C 2 0.652579 0.694777 0.467578 11.00000 0.04726 AFIX 0 PART 1 P2 4 0.194042 0.730610 0.514178 51.00000 0.01668 0.02831 = 0.03415 -0.00046 0.00511 0.00468 C8 1 0.197366 0.132553 0.227147 41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H8 2 0.177951 0.207686 0.200680 41.00000 -1.20000 AFIX 0 C9 1 0.210449 0.002707 0.206830 41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H9 2 0.204680 -0.008189 0.166131 41.00000 -1.20000 AFIX 0 C10 1 0.231350 -0.109569 0.243714 41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H10 2 0.238591 -0.197799 0.228635 41.00000 -1.20000 AFIX 0 C11 1 0.241725 -0.093082 0.302799 41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H11 2 0.258452 -0.168910 0.329394 41.00000 -1.20000 AFIX 0 C12 1 0.227596 0.035289 0.323457 41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H12 2 0.227992 0.047288 0.362916 41.00000 -1.20000 AFIX 0 C13 1 0.091218 0.716775 0.502261 31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 C14 1 0.072803 0.675342 0.552158 31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H14 2 0.110693 0.654847 0.588927 31.00000 -1.20000 AFIX 0 C15 1 -0.002051 0.665983 0.545247 31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H15 2 -0.016177 0.639422 0.578241 31.00000 -1.20000 AFIX 0 C16 1 -0.053561 0.691720 0.495984 31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H16 2 -0.104371 0.679801 0.494029 31.00000 -1.20000 AFIX 0 C17 1 -0.040393 0.737151 0.443559 31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H17 2 -0.079108 0.759799 0.407517 31.00000 -1.20000 AFIX 0 C18 1 0.037707 0.744241 0.452014 31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H18 2 0.052191 0.770581 0.419166 31.00000 -1.20000 AFIX 0 C19 1 0.226843 0.871665 0.562176 51.00000 0.03180 0.04672 = 0.07790 -0.02134 0.01830 0.00416 C20 1 0.213344 1.010115 0.545332 51.00000 0.03180 0.04672 = 0.07790 -0.02134 0.01830 0.00416 AFIX 43 H20 2 0.185312 1.030170 0.505127 51.00000 -1.20000 AFIX 0 C21 1 0.238644 1.120288 0.584120 51.00000 0.03180 0.04672 = 0.07790 -0.02134 0.01830 0.00416 AFIX 43 H21 2 0.229522 1.213776 0.570855 51.00000 -1.20000 AFIX 0 C22 1 0.277919 1.089381 0.643246 51.00000 0.03180 0.04672 = 0.07790 -0.02134 0.01830 0.00416 AFIX 43 H22 2 0.294219 1.163954 0.670572 51.00000 -1.20000 AFIX 0 C23 1 0.294290 0.954272 0.663990 51.00000 0.03180 0.04672 = 0.07790 -0.02134 0.01830 0.00416 AFIX 43 H23 2 0.321476 0.934538 0.704391 51.00000 -1.20000 AFIX 0 C24 1 0.268439 0.849604 0.621983 51.00000 0.03180 0.04672 = 0.07790 -0.02134 0.01830 0.00416 AFIX 43 H24 2 0.279858 0.756276 0.634835 51.00000 -1.20000 AFIX 0 C26 1 0.571771 0.611978 0.336080 21.00000 0.06437 0.08899 = 0.03287 -0.00956 0.00993 0.04177 AFIX 43 H26 2 0.615365 0.598566 0.369947 21.00000 -1.20000 AFIX 0 C27 1 0.577238 0.567578 0.283320 21.00000 0.09100 0.10092 = 0.04924 -0.01052 0.02108 0.04782 AFIX 43 H27 2 0.621470 0.526914 0.279800 21.00000 -1.20000 AFIX 0 C29 1 0.447928 0.648318 0.238763 21.00000 0.05334 0.11706 = 0.03106 -0.01555 0.00845 -0.01385 AFIX 43 H29 2 0.405285 0.660472 0.204051 21.00000 -1.20000 AFIX 0 C30 1 0.448871 0.690255 0.294838 21.00000 0.04876 0.10024 = 0.04504 -0.01760 0.02007 0.00351 AFIX 43 H30 2 0.404830 0.732307 0.298103 21.00000 -1.20000 AFIX 0 B3 3 0.254274 0.567852 0.548153 51.00000 0.01938 0.03809 = 0.02998 -0.00225 -0.00904 0.00565 AFIX 137 1.2000 H3A 2 0.317718 0.585330 0.549138 51.00000 -1.50000 H3B 2 0.228118 0.467610 0.518586 51.00000 -1.50000 H3C 2 0.254154 0.550183 0.597701 51.00000 -1.50000 AFIX 0 B4 3 0.214459 0.765010 0.441147 51.00000 0.01938 0.03809 = 0.02998 -0.00225 -0.00904 0.00565 AFIX 137 1.2000 H4A 2 0.188876 0.672019 0.406903 51.00000 -1.50000 H4B 2 0.281242 0.771496 0.451542 51.00000 -1.50000 H4C 2 0.185874 0.872769 0.419872 51.00000 -1.50000 AFIX 0 PART 0 PART 2 P2A 4 0.186569 0.732163 0.489971 -51.00000 0.02300 0.03152 = 0.04323 0.00076 0.01183 0.00499 C8A 1 0.257632 0.129626 0.246190 -41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H8A 2 0.276476 0.214907 0.236851 -41.00000 -1.20000 AFIX 0 C9A 1 0.279558 0.013670 0.220758 -41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H9A 2 0.310411 0.020759 0.196640 -41.00000 -1.20000 AFIX 0 C10A 1 0.253350 -0.109776 0.233196 -41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H10A 2 0.264810 -0.194633 0.217798 -41.00000 -1.20000 AFIX 0 C11A 1 0.209693 -0.107261 0.268846 -41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H11A 2 0.190954 -0.192465 0.278361 -41.00000 -1.20000 AFIX 0 C12A 1 0.192129 0.014659 0.291298 -41.00000 0.06368 0.04411 = 0.06022 -0.01004 0.00503 0.00433 AFIX 43 H12A 2 0.161571 0.005467 0.315562 -41.00000 -1.20000 AFIX 0 C13A 1 0.083554 0.705214 0.473650 -31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 C14A 1 0.046116 0.789593 0.501167 -31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H14A 2 0.071796 0.860495 0.527946 -31.00000 -1.20000 AFIX 0 C15A 1 -0.030017 0.767153 0.488341 -31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H15A 2 -0.058815 0.822563 0.505670 -31.00000 -1.20000 AFIX 0 C16A 1 -0.024465 0.580890 0.422160 -31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H16A 2 -0.048481 0.510335 0.394528 -31.00000 -1.20000 AFIX 0 C17A 1 -0.064296 0.656064 0.447512 -31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H17A 2 -0.116325 0.636521 0.438667 -31.00000 -1.20000 AFIX 0 C18A 1 0.050669 0.604435 0.435575 -31.00000 0.03459 0.07910 = 0.12857 -0.00491 0.03553 -0.00305 AFIX 43 H18A 2 0.079362 0.549557 0.417964 -31.00000 -1.20000 AFIX 0 C19A 1 0.212762 0.894016 0.536197 -51.00000 0.05072 0.04476 = 0.07633 -0.00431 0.01736 0.01417 C20A 1 0.205625 1.016960 0.507648 -51.00000 0.05072 0.04476 = 0.07633 -0.00431 0.01736 0.01417 AFIX 43 H20A 2 0.189046 1.019451 0.465583 -51.00000 -1.20000 AFIX 0 C21A 1 0.222531 1.139533 0.539822 -51.00000 0.05072 0.04476 = 0.07633 -0.00431 0.01736 0.01417 AFIX 43 H21A 2 0.216245 1.227260 0.520553 -51.00000 -1.20000 AFIX 0 C22A 1 0.249211 1.129554 0.601746 -51.00000 0.05072 0.04476 = 0.07633 -0.00431 0.01736 0.01417 AFIX 43 H22A 2 0.261793 1.211945 0.624847 -51.00000 -1.20000 AFIX 0 C23A 1 0.257438 1.004223 0.629404 -51.00000 0.05072 0.04476 = 0.07633 -0.00431 0.01736 0.01417 AFIX 43 H23A 2 0.275987 0.997108 0.671385 -51.00000 -1.20000 AFIX 0 C24A 1 0.237183 0.884719 0.592981 -51.00000 0.05072 0.04476 = 0.07633 -0.00431 0.01736 0.01417 AFIX 43 H24A 2 0.241759 0.795610 0.610950 -51.00000 -1.20000 AFIX 0 C26A 1 0.545786 0.754091 0.319270 -21.00000 0.06717 0.03834 = 0.06116 -0.01781 0.04218 -0.02099 AFIX 43 H26A 2 0.568750 0.839318 0.335913 -21.00000 -1.20000 AFIX 0 C27A 1 0.546613 0.707264 0.265368 -21.00000 0.11782 0.09356 = 0.05716 -0.02136 0.06475 -0.05731 AFIX 43 H27A 2 0.571681 0.763811 0.245313 -21.00000 -1.20000 AFIX 0 C29A 1 0.479014 0.505922 0.271010 -21.00000 0.05011 0.03936 = 0.03458 -0.01449 0.01942 -0.00838 AFIX 43 H29A 2 0.456535 0.419952 0.254898 -21.00000 -1.20000 AFIX 0 C30A 1 0.475709 0.547186 0.325529 -21.00000 0.03021 0.01991 = 0.02125 -0.00287 0.01015 -0.00875 AFIX 43 H30A 2 0.451202 0.493634 0.346985 -21.00000 -1.20000 AFIX 0 B3A 3 0.240760 0.571362 0.530134 -51.00000 0.01938 0.03809 = 0.02998 -0.00225 -0.00904 0.00565 AFIX 137 1.2000 H3AA 2 0.307206 0.592893 0.544641 -51.00000 -1.50000 H3AB 2 0.224826 0.472970 0.497484 -51.00000 -1.50000 H3AC 2 0.224049 0.547926 0.573328 -51.00000 -1.50000 AFIX 0 B4A 3 0.206515 0.754899 0.418797 -51.00000 0.01938 0.03809 = 0.02998 -0.00225 -0.00904 0.00565 AFIX 137 1.2000 H4AA 2 0.184912 0.654463 0.388060 -51.00000 -1.50000 H4AB 2 0.273043 0.768524 0.429438 -51.00000 -1.50000 H4AC 2 0.174333 0.856236 0.393421 -51.00000 -1.50000 AFIX 0 HKLF 4 REM dal1929_a.res in P2(1)/c REM R1 = 0.0474 for 5566 Fo > 4sig(Fo) and 0.0913 for all 8365 data REM 399 parameters refined using 625 restraints END WGHT 0.0407 16.2044 REM Highest difference peak 1.662, deepest hole -1.989, 1-sigma level 0.143 Q1 1 0.0033 0.5035 0.1593 11.00000 0.05 1.01 Q2 1 0.1996 0.1521 0.2907 11.00000 0.05 0.91 Q3 1 0.0943 0.3263 0.1939 11.00000 0.05 0.77 Q4 1 0.0890 0.4932 0.2664 11.00000 0.05 0.72 Q5 1 0.2310 0.0200 0.3038 11.00000 0.05 0.68 Q6 1 0.0363 0.4107 0.1512 11.00000 0.05 0.66 Q7 1 -0.0374 0.6234 0.3890 11.00000 0.05 0.65 Q8 1 0.2630 -0.0076 0.2081 11.00000 0.05 0.63 Q9 1 0.2915 0.1179 0.2558 11.00000 0.05 0.62 Q10 1 0.1592 0.0348 0.2715 11.00000 0.05 0.61 Q11 1 0.2174 0.9561 0.6376 11.00000 0.05 0.58 Q12 1 0.2080 0.8432 0.5208 11.00000 0.05 0.57 Q13 1 0.3185 0.5367 0.4696 11.00000 0.05 0.57 Q14 1 -0.0549 0.4128 0.3498 11.00000 0.05 0.55 Q15 1 0.5731 0.5943 0.2732 11.00000 0.05 0.54 Q16 1 0.3474 0.5082 0.4416 11.00000 0.05 0.54 Q17 1 -0.0206 0.6750 0.4327 11.00000 0.05 0.54 Q18 1 -0.0441 0.8041 0.4528 11.00000 0.05 0.52 Q19 1 0.5040 0.8385 0.4110 11.00000 0.05 0.52 Q20 1 0.2724 -0.0347 0.2638 11.00000 0.05 0.51 Q21 1 0.0035 0.3622 0.1655 11.00000 0.05 0.51 Q22 1 -0.0214 0.5630 0.4520 11.00000 0.05 0.50 Q23 1 0.3390 0.5512 0.4396 11.00000 0.05 0.49 Q24 1 0.3631 0.9435 0.3170 11.00000 0.05 0.49 Q25 1 0.2563 0.4413 0.4707 11.00000 0.05 0.49 Q26 1 0.2469 -0.0960 0.2765 11.00000 0.05 0.48 Q27 1 0.2682 0.4568 0.3964 11.00000 0.05 0.48 Q28 1 0.3097 0.4769 0.5104 11.00000 0.05 0.47 Q29 1 0.0119 0.8368 0.4010 11.00000 0.05 0.47 Q30 1 -0.1247 0.5043 0.3652 11.00000 0.05 0.47 Q31 1 0.5820 0.6176 0.3237 11.00000 0.05 0.47 Q32 1 0.0565 0.5596 0.4589 11.00000 0.05 0.47 Q33 1 0.2300 -0.1017 0.3124 11.00000 0.05 0.46 Q34 1 0.5623 0.4909 0.2069 11.00000 0.05 0.46 Q35 1 0.1632 0.0237 0.1122 11.00000 0.05 0.45 Q36 1 0.0795 0.7015 0.5639 11.00000 0.05 0.45 Q37 1 -0.0575 0.5147 0.3625 11.00000 0.05 0.45 Q38 1 0.2576 0.4991 0.4393 11.00000 0.05 0.45 Q39 1 0.0316 0.5712 0.2283 11.00000 0.05 0.45 Q40 1 0.2080 1.0970 0.6007 11.00000 0.05 0.45 ; _shelx_res_checksum 45514 _shelx_hkl_file ; 1 0 0 -0.10 0.50 1 0 0 1.30 1.40 1 0 0 -2.40 1.10 -1 0 0 -0.70 1.10 -1 0 0 1.50 1.50 -1 0 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35.90 -5 -3 27 41.20 38.00 -5 -3 27 70.09 38.10 -5 3 27 71.59 39.40 5 3 -27 18.20 35.80 -5 3 27 32.50 33.40 -4 -3 27 -45.70 32.10 -4 -3 27 6.50 34.30 4 3 -27 3.90 32.70 -4 3 27 18.70 36.60 -4 3 27 -44.20 27.80 -3 -3 27 8.40 29.90 -3 -3 27 82.89 41.80 3 -3 -27 25.10 36.90 -3 3 27 88.39 38.50 3 3 -27 39.80 29.20 -3 3 27 86.89 40.80 -2 -3 27 -37.80 33.90 2 -3 -27 16.30 35.80 -2 -3 27 1.00 26.90 2 3 -27 55.79 36.20 -2 3 27 30.70 35.90 -2 3 27 34.80 37.30 -1 -3 27 33.40 39.10 -1 -3 27 1.90 25.50 1 -3 -27 -23.30 36.10 -1 3 27 -6.70 38.50 -1 3 27 78.89 34.40 1 3 -27 43.90 37.60 0 -3 -27 42.90 40.40 0 -3 27 145.89 51.69 0 -3 27 95.99 35.70 0 3 27 75.49 42.90 0 3 27 88.09 35.70 -13 -4 27 -62.89 36.20 -13 -4 27 14.50 38.60 -13 4 27 41.60 43.10 13 4 -27 -9.50 25.50 -12 -4 27 -19.10 36.90 -12 -4 27 0.70 37.30 12 4 -27 -15.20 36.80 -12 4 27 65.69 42.50 -11 -4 27 -17.90 36.60 -11 -4 27 -0.50 38.30 11 4 -27 -25.90 33.20 -11 4 27 -20.40 36.70 -11 4 27 22.90 33.30 -10 -4 27 -10.80 27.80 -10 -4 27 31.70 38.80 10 4 -27 24.20 39.30 -10 4 27 -29.30 32.30 -10 4 27 -22.10 35.90 -9 -4 27 -9.80 36.20 -9 -4 27 49.40 39.50 -9 4 27 7.60 30.80 -9 4 27 12.10 33.70 9 4 -27 41.30 39.60 -8 -4 27 16.10 36.60 -8 -4 27 44.40 39.60 -8 4 27 25.40 33.10 8 4 -27 24.00 35.50 -8 4 27 -70.59 29.70 -7 -4 27 -9.70 36.10 -7 -4 27 -28.40 33.30 -7 4 27 -6.10 34.40 -7 4 27 11.80 37.90 7 4 -27 -2.60 35.90 -6 -4 27 7.00 35.40 -6 -4 27 46.20 37.00 -6 4 27 -20.50 35.80 6 4 -27 -20.20 35.10 -6 4 27 -19.60 28.00 -5 -4 27 10.20 38.20 -5 -4 27 20.50 37.50 -5 4 27 -6.00 29.40 -5 4 27 -12.90 34.00 5 4 -27 -22.10 34.10 -4 -4 27 72.19 41.60 -4 -4 27 71.59 41.30 4 4 -27 33.30 38.60 -4 4 27 0.80 30.20 -4 4 27 70.79 39.50 -3 -4 27 13.40 31.70 -3 -4 27 -41.80 35.20 -3 4 27 -35.20 33.90 -3 4 27 24.70 30.40 3 4 -27 38.20 32.10 -2 -4 27 118.09 43.40 -2 -4 27 -29.40 35.40 2 4 -27 30.90 37.20 -2 4 27 72.69 40.50 -2 4 27 -15.90 32.50 -1 -4 27 7.60 29.50 1 -4 -27 -12.80 34.80 1 4 -27 -11.80 34.20 -1 4 27 -20.80 32.30 -10 -5 27 14.00 38.60 -9 -5 27 100.69 43.80 -9 -5 27 31.90 39.10 9 5 -27 2.90 37.80 -9 5 27 26.00 39.40 -8 -5 27 31.80 39.30 -8 -5 27 138.39 45.10 -8 5 27 67.19 41.40 8 5 -27 47.60 38.50 -7 -5 27 17.00 38.50 -7 -5 27 -2.00 38.40 -7 5 27 -6.40 29.00 7 5 -27 46.70 37.60 -7 5 27 29.40 39.10 -6 -5 27 36.60 39.90 -6 -5 27 48.70 32.60 6 5 -27 -24.60 24.60 -6 5 27 25.90 32.10 -6 5 27 33.10 37.50 -5 -5 27 -2.50 38.90 -5 -5 27 79.29 41.30 5 5 -27 27.00 29.90 -5 5 27 -26.00 28.20 -5 5 27 89.19 44.60 15 0 -28 68.89 43.90 -15 0 28 19.80 40.30 -15 0 28 42.40 34.30 14 0 -28 36.60 40.10 -14 0 28 -77.39 29.80 -14 0 28 -27.00 35.30 -13 0 28 -26.80 37.10 -13 0 28 2.20 36.10 13 0 -28 35.90 35.30 -12 0 28 14.30 38.80 -12 0 28 -41.50 32.90 12 0 -28 -15.60 35.60 -11 0 28 47.00 40.20 -11 0 28 8.20 35.00 11 0 -28 18.70 37.30 -10 0 28 44.60 41.40 -10 0 28 32.40 35.60 10 0 -28 79.89 38.30 -9 0 28 39.40 30.10 -9 0 28 -13.00 32.90 9 0 -28 -27.00 53.39 -8 0 28 -12.60 33.30 -8 0 28 51.89 36.90 -7 0 28 14.70 37.20 -7 0 28 -16.70 34.40 -6 0 28 137.99 45.10 -6 0 28 120.99 35.80 -5 0 28 89.19 40.00 -5 0 28 123.99 41.70 -4 0 28 12.00 33.70 -4 0 28 23.00 37.00 -3 0 28 84.09 41.60 -3 0 28 6.80 34.00 -2 0 28 46.50 36.50 -2 0 28 -35.40 23.90 -1 0 28 60.79 41.30 -1 0 28 -15.80 35.30 0 0 28 35.90 42.40 -15 -1 28 -15.70 35.60 -15 -1 28 35.60 46.70 15 -1 -28 -27.90 33.70 15 1 -28 28.00 38.40 -15 1 28 6.20 36.70 -14 -1 28 -25.20 36.80 14 -1 -28 -13.30 26.80 -14 -1 28 65.29 41.30 -14 1 28 -10.00 35.50 -14 1 28 49.30 43.40 14 1 -28 25.30 29.80 -13 -1 28 29.10 29.40 13 -1 -28 38.40 47.20 -13 -1 28 42.80 40.70 -13 1 28 27.80 38.30 -13 1 28 -19.60 36.40 13 1 -28 -37.40 34.90 -12 -1 28 2.50 37.20 -12 -1 28 8.10 37.90 -12 1 28 -23.90 38.00 -12 1 28 -20.70 34.60 12 1 -28 -4.70 36.60 -11 -1 28 -57.89 22.30 -11 -1 28 7.60 35.60 -11 1 28 10.20 39.70 11 1 -28 -11.50 34.40 -11 1 28 -16.40 33.20 -10 -1 28 -40.30 33.70 -10 -1 28 -23.40 34.70 -10 1 28 9.30 36.40 10 1 -28 -12.40 24.50 -10 1 28 2.60 37.60 -9 -1 28 22.90 37.30 -9 -1 28 27.00 36.50 -9 1 28 10.90 29.20 -9 1 28 49.80 36.20 9 1 -28 -51.69 31.40 -8 -1 28 -54.69 31.80 -8 -1 28 49.50 39.40 -8 1 28 -32.70 35.20 -8 1 28 -18.80 31.80 8 1 -28 -53.49 31.20 -7 -1 28 -68.49 32.00 -7 -1 28 -21.50 32.20 -7 1 28 41.40 35.20 -7 1 28 43.70 41.30 7 1 -28 35.80 36.40 -6 -1 28 45.40 38.80 -6 -1 28 -25.80 25.70 -6 1 28 56.69 35.50 -6 1 28 -7.50 35.50 -5 -1 28 -40.90 32.20 -5 -1 28 6.60 26.70 -5 1 28 -52.19 30.00 -5 1 28 3.10 36.90 -4 -1 28 17.90 29.30 -4 -1 28 14.40 34.50 -4 1 28 -46.20 30.40 -4 1 28 -7.50 36.60 -3 -1 28 -14.80 35.70 -3 -1 28 -6.30 34.30 -3 1 28 17.80 35.10 -3 1 28 -7.00 37.50 -2 -1 28 44.60 39.20 -2 -1 28 29.40 38.90 -2 1 28 16.70 34.50 -2 1 28 65.49 40.70 -1 -1 28 57.89 41.80 -1 1 28 -27.00 35.30 -1 1 28 6.60 31.20 0 -1 -28 -33.10 35.50 0 -1 28 26.70 41.70 0 1 28 28.50 41.90 -14 -2 28 33.30 41.10 -14 -2 28 15.30 38.70 14 2 -28 8.00 38.20 -14 2 28 18.30 42.30 -13 -2 28 74.89 43.30 -13 -2 28 63.59 41.20 13 2 -28 71.49 41.30 -13 2 28 71.39 46.40 -13 2 28 39.50 42.50 -12 -2 28 -17.40 35.50 -12 -2 28 38.30 40.30 12 2 -28 36.80 38.20 -12 2 28 -18.40 34.50 -12 2 28 -19.80 29.30 -11 -2 28 -38.40 36.40 -11 -2 28 44.20 39.70 -11 2 28 43.10 37.90 -11 2 28 40.60 41.20 11 2 -28 -38.10 33.30 -10 -2 28 56.09 41.30 -10 -2 28 18.70 38.00 -10 2 28 5.70 34.10 -10 2 28 -1.80 40.10 10 2 -28 13.70 29.80 -9 -2 28 45.80 31.30 -9 -2 28 108.09 42.70 -9 2 28 8.90 41.70 -9 2 28 137.39 41.40 9 2 -28 45.60 37.80 -8 -2 28 71.69 38.10 -8 -2 28 24.70 29.80 -8 2 28 58.99 40.90 8 2 -28 91.79 39.10 -8 2 28 85.89 39.20 -7 -2 28 22.80 36.70 -7 -2 28 44.50 40.10 -7 2 28 79.29 36.70 7 2 -28 -14.30 33.70 -7 2 28 10.80 29.60 -6 -2 28 28.60 37.40 -6 -2 28 9.30 36.30 -6 2 28 21.90 33.70 -6 2 28 39.30 38.70 6 2 -28 4.40 34.50 -5 -2 28 0.20 27.10 -5 -2 28 75.59 37.90 -5 2 28 7.10 33.10 5 2 -28 72.69 39.10 -5 2 28 21.00 38.30 4 -2 -28 66.89 39.90 -4 -2 28 85.39 42.80 -4 -2 28 62.19 38.90 4 2 -28 34.20 40.10 -4 2 28 27.40 38.70 -4 2 28 7.90 33.10 -3 -2 28 66.69 40.60 -3 -2 28 156.58 47.10 3 -2 -28 29.90 39.50 -3 2 28 74.09 35.90 -3 2 28 83.49 42.50 2 -2 -28 -72.79 32.80 -2 -2 28 -23.60 36.80 -2 -2 28 -27.90 26.20 -2 2 28 69.39 40.00 -2 2 28 36.40 40.10 -1 -2 28 10.80 29.60 1 -2 -28 24.20 37.90 -1 2 28 149.59 47.60 -13 -3 28 29.40 42.50 13 3 -28 7.60 38.40 -12 -3 28 -72.99 34.80 -12 -3 28 -27.50 35.60 -12 3 28 -1.30 42.40 12 3 -28 -26.50 27.00 -11 -3 28 2.30 39.50 -11 -3 28 -54.69 24.20 11 3 -28 -83.09 31.30 -11 3 28 74.39 37.20 -10 -3 28 -15.40 27.20 -10 -3 28 2.00 39.60 -10 3 28 -15.70 33.50 -10 3 28 26.20 40.10 10 3 -28 27.60 38.00 -9 -3 28 -12.80 36.70 -9 -3 28 -49.20 30.80 -9 3 28 22.40 40.30 9 3 -28 -22.80 33.90 -9 3 28 -3.30 32.10 -8 -3 28 23.10 38.10 -8 -3 28 -40.50 33.10 -8 3 28 30.20 42.00 -8 3 28 -38.20 32.10 8 3 -28 46.00 39.70 -7 -3 28 21.50 30.00 -7 -3 28 31.10 42.20 -7 3 28 -28.40 26.90 -7 3 28 -10.10 32.80 7 3 -28 21.40 35.70 -6 -3 28 62.49 40.20 -6 -3 28 -5.30 26.30 -6 3 28 4.40 38.40 -6 3 28 -19.00 33.90 6 3 -28 -15.60 37.30 -5 -3 28 -36.20 35.40 -5 -3 28 61.99 41.10 -5 3 28 -58.99 33.80 5 3 -28 7.40 36.70 -5 3 28 -8.60 30.50 -4 -3 28 93.49 42.10 -4 -3 28 -5.20 35.60 4 3 -28 -35.90 32.90 -4 3 28 -29.90 30.10 -4 3 28 1.80 38.10 3 -3 -28 9.90 41.10 -3 -3 28 -23.10 25.70 -3 -3 28 9.10 41.00 3 3 -28 -23.60 34.50 -3 3 28 -5.20 31.00 -3 3 28 -53.49 34.40 2 -3 -28 40.60 37.80 -2 -3 28 -1.40 38.70 2 3 -28 -1.90 59.09 -2 3 28 6.90 38.50 -10 -4 28 -42.10 37.70 -10 -4 28 9.40 39.20 10 4 -28 41.80 39.20 -10 4 28 -37.90 37.30 -9 -4 28 12.70 38.90 -9 -4 28 23.40 40.20 9 4 -28 -11.70 27.30 -9 4 28 66.99 43.00 -8 -4 28 -33.90 36.70 -8 -4 28 54.49 41.40 -8 4 28 115.49 44.30 8 4 -28 -3.60 36.50 -7 -4 28 -20.60 36.40 -7 -4 28 10.00 38.10 -7 4 28 5.50 38.40 7 4 -28 80.69 41.30 -6 -4 28 69.09 42.40 -6 -4 28 -1.00 38.10 -6 4 28 198.48 50.89 6 4 -28 48.40 40.80 -5 -4 28 23.00 38.80 -5 -4 28 36.30 40.30 -5 4 28 27.10 40.30 5 4 -28 34.00 40.50 -13 0 29 57.89 39.30 -13 0 29 53.19 46.00 13 0 -29 63.49 39.40 -12 0 29 -24.30 36.10 -12 0 29 -2.40 39.80 12 0 -29 2.60 26.50 11 0 -29 67.19 45.70 -11 0 29 -45.40 34.40 -11 0 29 7.00 38.70 -10 0 29 12.20 40.00 -10 0 29 -69.49 32.00 -9 0 29 -31.90 34.50 -9 0 29 -20.30 25.90 -8 0 29 36.90 41.20 -8 0 29 -43.20 30.60 -7 0 29 31.50 42.40 -7 0 29 20.00 37.90 -6 0 29 84.99 41.60 -6 0 29 19.70 38.10 -5 0 29 29.80 37.80 -5 0 29 -50.89 31.60 -4 0 29 11.10 39.60 -3 0 29 -62.29 24.20 -13 -1 29 110.59 43.70 13 1 -29 26.30 41.20 -12 -1 29 88.69 44.10 -12 -1 29 35.10 41.90 -12 1 29 18.00 40.70 12 1 -29 -1.80 37.80 -11 -1 29 9.80 38.50 -11 -1 29 41.40 42.70 11 1 -29 19.70 38.50 -11 1 29 90.99 46.70 -11 1 29 52.19 43.10 -10 -1 29 52.89 40.30 -10 -1 29 59.89 40.30 -10 1 29 39.30 39.10 -10 1 29 78.49 45.80 10 1 -29 -44.30 33.10 -9 -1 29 101.89 41.90 -9 -1 29 43.30 31.70 -9 1 29 -22.50 35.20 9 1 -29 19.60 35.60 -9 1 29 -21.00 26.70 -8 -1 29 41.20 41.60 -8 -1 29 46.90 40.80 8 1 -29 -31.60 36.80 -8 1 29 1.40 39.80 -8 1 29 -6.00 32.90 -7 -1 29 -10.80 27.20 -7 -1 29 42.20 38.90 -7 1 29 77.49 40.10 -7 1 29 53.99 43.70 -6 -1 29 -12.70 34.60 -6 -1 29 15.10 40.20 -6 1 29 61.49 41.90 -6 1 29 27.70 38.80 -5 -1 29 28.70 38.70 -5 -1 29 1.60 28.60 -5 1 29 -18.00 38.60 -5 1 29 78.99 45.70 -4 -1 29 63.79 42.10 -4 1 29 47.20 42.50 -3 -1 29 110.09 45.50 -3 1 29 77.39 41.90 12 2 -29 15.50 41.20 -11 -2 29 -39.50 37.50 -11 -2 29 10.70 37.60 -11 2 29 -7.70 42.80 11 2 -29 24.30 38.90 -10 -2 29 37.60 44.00 -10 -2 29 -58.79 33.20 -10 2 29 -15.60 39.10 10 2 -29 7.60 37.30 -9 -2 29 -46.00 33.30 -9 -2 29 -24.50 37.60 -9 2 29 18.80 43.00 9 2 -29 -43.90 33.50 -8 -2 29 25.30 39.90 -8 -2 29 -17.10 38.40 8 2 -29 11.50 36.60 -8 2 29 1.30 40.20 -7 -2 29 1.50 38.30 -7 -2 29 -28.90 36.00 7 2 -29 14.70 37.50 -7 2 29 -10.60 39.90 -6 -2 29 -4.90 37.20 -6 -2 29 -11.40 36.80 6 2 -29 22.00 35.40 -6 2 29 114.29 48.60 -5 -2 29 53.49 40.60 -5 -2 29 -30.30 37.60 -5 2 29 -19.10 36.80 -4 -2 29 44.90 42.60 -4 2 29 2.40 38.30 -9 -3 29 -49.99 34.90 9 3 -29 10.50 40.00 -8 -3 29 47.20 42.30 8 3 -29 78.49 43.20 -7 -3 29 -63.89 35.80 7 3 -29 15.90 37.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 51295 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 U1 U 0.30331(2) 0.51181(2) 0.44177(2) 0.03303(10) Uani 1 1 d . . . . . P1 P 0.19500(11) 0.3144(2) 0.31114(10) 0.0471(6) Uani 1 1 d . . . . . P3 P 0.50933(9) 0.72463(17) 0.41928(8) 0.0278(4) Uani 1 1 d . . . . . C1 C 0.1088(4) 0.3832(8) 0.2575(3) 0.1030(18) Uani 1 1 d D . . . . C2 C 0.1135(3) 0.4778(8) 0.2159(3) 0.1030(18) Uani 1 1 d DG . . . . H2 H 0.1613 0.5100 0.2163 0.124 Uiso 1 1 calc R . . . . C3 C 0.0490(4) 0.5258(7) 0.1736(3) 0.1030(18) Uani 1 1 d DG . . . . H3 H 0.0522 0.5912 0.1449 0.124 Uiso 1 1 calc R . . . . C4 C -0.0203(3) 0.4793(8) 0.1730(3) 0.1030(18) Uani 1 1 d DG . . . . H4 H -0.0648 0.5125 0.1438 0.124 Uiso 1 1 calc R . . . . C5 C -0.0250(3) 0.3847(8) 0.2146(3) 0.1030(18) Uani 1 1 d DG . . . . H5 H -0.0728 0.3525 0.2142 0.124 Uiso 1 1 calc R . . . . C6 C 0.0395(4) 0.3367(8) 0.2569(3) 0.1030(18) Uani 1 1 d DG . . . . H6 H 0.0362 0.2713 0.2856 0.124 Uiso 1 1 calc R . . . . C7 C 0.2127(5) 0.1461(8) 0.2833(4) 0.0600(14) Uani 1 1 d D . . . . C25 C 0.5112(3) 0.6737(6) 0.3465(3) 0.0329(17) Uani 1 1 d D . . . . C28 C 0.5148(5) 0.5870(8) 0.2378(4) 0.069(3) Uani 1 1 d D . . . . H28 H 0.5154 0.5559 0.2004 0.082 Uiso 0.555(9) 1 calc R . P A 1 H28A H 0.5162 0.5596 0.2001 0.082 Uiso 0.445(9) 1 calc R . P A 2 C31 C 0.5057(2) 0.9134(4) 0.4187(2) 0.0283(16) Uani 1 1 d D . . . . C32 C 0.4370(2) 0.9801(4) 0.4011(2) 0.0378(17) Uani 1 1 d DG . . . . H32 H 0.3919 0.9276 0.3922 0.045 Uiso 1 1 calc R . . . . C33 C 0.4338(3) 1.1229(4) 0.3965(2) 0.045(2) Uani 1 1 d DG . . . . H33 H 0.3864 1.1689 0.3844 0.054 Uiso 1 1 calc R . . . . C34 C 0.4992(3) 1.1991(4) 0.4094(3) 0.056(2) Uani 1 1 d DG . . . . H34 H 0.4970 1.2975 0.4061 0.067 Uiso 1 1 calc R . . . . C35 C 0.5679(3) 1.1324(5) 0.4270(3) 0.058(3) Uani 1 1 d DG . . . . H35 H 0.6131 1.1849 0.4359 0.070 Uiso 1 1 calc R . . . . C36 C 0.5712(2) 0.9896(5) 0.4316(3) 0.051(2) Uani 1 1 d DG . . . . H36 H 0.6185 0.9437 0.4437 0.061 Uiso 1 1 calc R . . . . B1 B 0.1870(5) 0.3024(9) 0.3882(4) 0.053(3) Uani 1 1 d . . . . . H1A H 0.2467 0.2691 0.4233 0.05(2) Uiso 1 1 calc GR . . . . H1B H 0.1404 0.2172 0.3880 0.06(2) Uiso 1 1 calc GR . . . . H1C H 0.1689 0.4135 0.4019 0.024(16) Uiso 1 1 calc GR . . . . B2 B 0.2781(5) 0.4386(9) 0.3186(4) 0.046(2) Uani 1 1 d . . . . . H2A H 0.2629 0.5526 0.3315 0.05(2) Uiso 1 1 calc GR . . . . H2B H 0.2897 0.4437 0.2724 0.09(3) Uiso 1 1 calc GR . . . . H2C H 0.3334 0.3966 0.3566 0.06(2) Uiso 1 1 calc GR . . . . B5 B 0.4199(4) 0.6500(7) 0.4279(4) 0.0317(19) Uani 1 1 d . . . . . H5A H 0.4133 0.6923 0.4730 0.06(2) Uiso 1 1 calc GR . . . . H5B H 0.4237 0.5255 0.4295 0.05(2) Uiso 1 1 calc GR . . . . H5C H 0.3664 0.6853 0.3866 0.034(18) Uiso 1 1 calc GR . . . . B6 B 0.5980(4) 0.6516(8) 0.4770(4) 0.0323(19) Uani 1 1 d . . . . . H6A H 0.5970 0.5270 0.4742 0.05(2) Uiso 1 1 calc GR . . . . H6B H 0.6000 0.6871 0.5256 0.06(2) Uiso 1 1 calc GR . . . . H6C H 0.6526 0.6948 0.4676 0.05(2) Uiso 1 1 calc GR . . . . P2 P 0.1940(6) 0.7306(11) 0.5142(5) 0.0272(18) Uani 0.461(15) 1 d D . P B 1 C8 C 0.1974(8) 0.1326(13) 0.2271(6) 0.0600(14) Uani 0.665(7) 1 d . . P C 1 H8 H 0.1780 0.2077 0.2007 0.072 Uiso 0.665(7) 1 calc R . P C 1 C9 C 0.2104(8) 0.0027(12) 0.2068(6) 0.0600(14) Uani 0.665(7) 1 d . . P C 1 H9 H 0.2047 -0.0082 0.1661 0.072 Uiso 0.665(7) 1 calc R . P C 1 C10 C 0.2314(9) -0.1096(16) 0.2437(7) 0.0600(14) Uani 0.665(7) 1 d . . P C 1 H10 H 0.2386 -0.1978 0.2286 0.072 Uiso 0.665(7) 1 calc R . P C 1 C11 C 0.2417(8) -0.0931(13) 0.3028(7) 0.0600(14) Uani 0.665(7) 1 d . . P C 1 H11 H 0.2585 -0.1689 0.3294 0.072 Uiso 0.665(7) 1 calc R . P C 1 C12 C 0.2276(8) 0.0353(12) 0.3235(7) 0.0600(14) Uani 0.665(7) 1 d . . P C 1 H12 H 0.2280 0.0473 0.3629 0.072 Uiso 0.665(7) 1 calc R . P C 1 C13 C 0.0912(7) 0.7168(18) 0.5023(11) 0.079(2) Uani 0.517(7) 1 d D . P B 1 C14 C 0.0728(10) 0.6753(16) 0.5522(11) 0.079(2) Uani 0.517(7) 1 d . . P B 1 H14 H 0.1107 0.6548 0.5889 0.094 Uiso 0.517(7) 1 calc R . P B 1 C15 C -0.0021(10) 0.6660(15) 0.5452(11) 0.079(2) Uani 0.517(7) 1 d . . P B 1 H15 H -0.0162 0.6394 0.5782 0.094 Uiso 0.517(7) 1 calc R . P B 1 C16 C -0.0536(11) 0.6917(16) 0.4960(11) 0.079(2) Uani 0.517(7) 1 d . . P B 1 H16 H -0.1044 0.6798 0.4940 0.094 Uiso 0.517(7) 1 calc R . P B 1 C17 C -0.0404(11) 0.7372(18) 0.4436(12) 0.079(2) Uani 0.517(7) 1 d . . P B 1 H17 H -0.0791 0.7598 0.4075 0.094 Uiso 0.517(7) 1 calc R . P B 1 C18 C 0.0377(10) 0.7442(17) 0.4520(11) 0.079(2) Uani 0.517(7) 1 d . . P B 1 H18 H 0.0522 0.7706 0.4192 0.094 Uiso 0.517(7) 1 calc R . P B 1 C19 C 0.2268(12) 0.8717(17) 0.5622(9) 0.052(4) Uani 0.461(15) 1 d D . P B 1 C20 C 0.2133(9) 1.0101(15) 0.5453(10) 0.052(4) Uani 0.461(15) 1 d D . P B 1 H20 H 0.1853 1.0302 0.5051 0.063 Uiso 0.461(15) 1 calc R . P B 1 C21 C 0.2386(13) 1.120(2) 0.5841(9) 0.052(4) Uani 0.461(15) 1 d D . P B 1 H21 H 0.2295 1.2138 0.5709 0.063 Uiso 0.461(15) 1 calc R . P B 1 C22 C 0.2779(10) 1.0894(17) 0.6432(9) 0.052(4) Uani 0.461(15) 1 d D . P B 1 H22 H 0.2942 1.1640 0.6706 0.063 Uiso 0.461(15) 1 calc R . P B 1 C23 C 0.2943(10) 0.9543(15) 0.6640(9) 0.052(4) Uani 0.461(15) 1 d D . P B 1 H23 H 0.3215 0.9345 0.7044 0.063 Uiso 0.461(15) 1 calc R . P B 1 C24 C 0.2684(10) 0.8496(19) 0.6220(8) 0.052(4) Uani 0.461(15) 1 d D . P B 1 H24 H 0.2799 0.7563 0.6348 0.063 Uiso 0.461(15) 1 calc R . P B 1 C26 C 0.5718(7) 0.6120(11) 0.3361(6) 0.064(5) Uani 0.555(9) 1 d D . P A 1 H26 H 0.6154 0.5986 0.3699 0.076 Uiso 0.555(9) 1 calc R . P A 1 C27 C 0.5772(8) 0.5676(13) 0.2833(6) 0.081(7) Uani 0.555(9) 1 d D . P A 1 H27 H 0.6215 0.5269 0.2798 0.097 Uiso 0.555(9) 1 calc R . P A 1 C29 C 0.4479(7) 0.6483(13) 0.2388(6) 0.069(6) Uani 0.555(9) 1 d D . P A 1 H29 H 0.4053 0.6605 0.2041 0.082 Uiso 0.555(9) 1 calc R . P A 1 C30 C 0.4489(7) 0.6903(13) 0.2948(5) 0.064(5) Uani 0.555(9) 1 d D . P A 1 H30 H 0.4048 0.7323 0.2981 0.076 Uiso 0.555(9) 1 calc R . P A 1 B3 B 0.2543(17) 0.568(4) 0.5482(13) 0.034(4) Uani 0.461(15) 1 d . U P B 1 H3A H 0.3177 0.5853 0.5491 0.050 Uiso 0.461(15) 1 calc GR . P B 1 H3B H 0.2281 0.4676 0.5186 0.050 Uiso 0.461(15) 1 calc GR . P B 1 H3C H 0.2542 0.5502 0.5977 0.050 Uiso 0.461(15) 1 calc GR . P B 1 B4 B 0.2145(17) 0.765(3) 0.4411(11) 0.034(4) Uani 0.461(15) 1 d . U P B 1 H4A H 0.1889 0.6720 0.4069 0.050 Uiso 0.461(15) 1 calc GR . P B 1 H4B H 0.2812 0.7715 0.4515 0.050 Uiso 0.461(15) 1 calc GR . P B 1 H4C H 0.1859 0.8728 0.4199 0.050 Uiso 0.461(15) 1 calc GR . P B 1 P2A P 0.1866(5) 0.7322(9) 0.4900(4) 0.0324(17) Uani 0.539(15) 1 d D . P B 2 C8A C 0.2576(9) 0.130(2) 0.2462(7) 0.0600(14) Uani 0.335(7) 1 d D . P C 2 H8A H 0.2765 0.2149 0.2369 0.072 Uiso 0.335(7) 1 calc R . P C 2 C9A C 0.2796(12) 0.014(2) 0.2208(9) 0.0600(14) Uani 0.335(7) 1 d D . P C 2 H9A H 0.3104 0.0208 0.1966 0.072 Uiso 0.335(7) 1 calc R . P C 2 C10A C 0.2534(13) -0.110(3) 0.2332(11) 0.0600(14) Uani 0.335(7) 1 d D . P C 2 H10A H 0.2648 -0.1946 0.2178 0.072 Uiso 0.335(7) 1 calc R . P C 2 C11A C 0.2097(14) -0.107(2) 0.2688(11) 0.0600(14) Uani 0.335(7) 1 d D . P C 2 H11A H 0.1910 -0.1925 0.2784 0.072 Uiso 0.335(7) 1 calc R . P C 2 C12A C 0.1921(12) 0.0147(15) 0.2913(10) 0.0600(14) Uani 0.335(7) 1 d D . P C 2 H12A H 0.1616 0.0055 0.3156 0.072 Uiso 0.335(7) 1 calc R . P C 2 C13A C 0.0836(7) 0.705(2) 0.4736(9) 0.079(2) Uani 0.483(7) 1 d D . P B 2 C14A C 0.0461(10) 0.790(2) 0.5012(10) 0.079(2) Uani 0.483(7) 1 d . . P B 2 H14A H 0.0718 0.8605 0.5279 0.094 Uiso 0.483(7) 1 calc R . P B 2 C15A C -0.0300(11) 0.767(2) 0.4883(10) 0.079(2) Uani 0.483(7) 1 d . . P B 2 H15A H -0.0588 0.8226 0.5057 0.094 Uiso 0.483(7) 1 calc R . P B 2 C16A C -0.0245(10) 0.581(2) 0.4222(9) 0.079(2) Uani 0.483(7) 1 d . . P B 2 H16A H -0.0485 0.5103 0.3945 0.094 Uiso 0.483(7) 1 calc R . P B 2 C17A C -0.0643(12) 0.656(2) 0.4475(10) 0.079(2) Uani 0.483(7) 1 d . . P B 2 H17A H -0.1163 0.6365 0.4387 0.094 Uiso 0.483(7) 1 calc R . P B 2 C18A C 0.0507(10) 0.604(2) 0.4356(9) 0.079(2) Uani 0.483(7) 1 d . . P B 2 H18A H 0.0794 0.5496 0.4180 0.094 Uiso 0.483(7) 1 calc R . P B 2 C19A C 0.2128(11) 0.8940(14) 0.5362(8) 0.058(3) Uani 0.539(15) 1 d D . P B 2 C20A C 0.2056(10) 1.0170(16) 0.5076(10) 0.058(3) Uani 0.539(15) 1 d . . P B 2 H20A H 0.1890 1.0195 0.4656 0.070 Uiso 0.539(15) 1 calc R . P B 2 C21A C 0.2225(9) 1.1395(17) 0.5398(9) 0.058(3) Uani 0.539(15) 1 d . . P B 2 H21A H 0.2162 1.2273 0.5206 0.070 Uiso 0.539(15) 1 calc R . P B 2 C22A C 0.2492(14) 1.130(2) 0.6017(9) 0.058(3) Uani 0.539(15) 1 d . . P B 2 H22A H 0.2618 1.2119 0.6248 0.070 Uiso 0.539(15) 1 calc R . P B 2 C23A C 0.2574(10) 1.0042(17) 0.6294(9) 0.058(3) Uani 0.539(15) 1 d . . P B 2 H23A H 0.2760 0.9971 0.6714 0.070 Uiso 0.539(15) 1 calc R . P B 2 C24A C 0.2372(12) 0.8847(18) 0.5930(10) 0.058(3) Uani 0.539(15) 1 d . . P B 2 H24A H 0.2418 0.7956 0.6109 0.070 Uiso 0.539(15) 1 calc R . P B 2 C26A C 0.5458(6) 0.7541(14) 0.3193(6) 0.050(5) Uani 0.445(9) 1 d D . P A 2 H26A H 0.5688 0.8393 0.3359 0.060 Uiso 0.445(9) 1 calc R . P A 2 C27A C 0.5466(8) 0.7073(14) 0.2654(6) 0.081(9) Uani 0.445(9) 1 d D . P A 2 H27A H 0.5717 0.7638 0.2453 0.097 Uiso 0.445(9) 1 calc R . P A 2 C29A C 0.4790(7) 0.5059(14) 0.2710(5) 0.040(4) Uani 0.445(9) 1 d D . P A 2 H29A H 0.4565 0.4200 0.2549 0.048 Uiso 0.445(9) 1 calc R . P A 2 C30A C 0.4757(6) 0.5472(10) 0.3255(5) 0.023(4) Uani 0.445(9) 1 d D . P A 2 H30A H 0.4512 0.4936 0.3470 0.028 Uiso 0.445(9) 1 calc R . P A 2 B3A B 0.2408(14) 0.571(3) 0.5301(11) 0.034(4) Uani 0.539(15) 1 d . U P B 2 H3AA H 0.3072 0.5929 0.5446 0.050 Uiso 0.539(15) 1 calc GR . P B 2 H3AB H 0.2248 0.4730 0.4975 0.050 Uiso 0.539(15) 1 calc GR . P B 2 H3AC H 0.2240 0.5479 0.5733 0.050 Uiso 0.539(15) 1 calc GR . P B 2 B4A B 0.2065(14) 0.755(3) 0.4188(9) 0.034(4) Uani 0.539(15) 1 d . U P B 2 H4AA H 0.1849 0.6545 0.3881 0.050 Uiso 0.539(15) 1 calc GR . P B 2 H4AB H 0.2730 0.7685 0.4294 0.050 Uiso 0.539(15) 1 calc GR . P B 2 H4AC H 0.1743 0.8562 0.3934 0.050 Uiso 0.539(15) 1 calc GR . 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 U1 0.01639(12) 0.02458(14) 0.04751(17) -0.00084(13) -0.00332(10) 0.00200(11) P1 0.0344(11) 0.0301(10) 0.0532(14) 0.0033(9) -0.0165(10) -0.0039(8) P3 0.0193(9) 0.0253(8) 0.0333(10) -0.0038(7) 0.0015(8) 0.0037(7) C1 0.063(3) 0.091(3) 0.115(4) 0.038(3) -0.024(3) -0.001(3) C2 0.063(3) 0.091(3) 0.115(4) 0.038(3) -0.024(3) -0.001(3) C3 0.063(3) 0.091(3) 0.115(4) 0.038(3) -0.024(3) -0.001(3) C4 0.063(3) 0.091(3) 0.115(4) 0.038(3) -0.024(3) -0.001(3) C5 0.063(3) 0.091(3) 0.115(4) 0.038(3) -0.024(3) -0.001(3) C6 0.063(3) 0.091(3) 0.115(4) 0.038(3) -0.024(3) -0.001(3) C7 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C25 0.024(4) 0.029(4) 0.038(4) -0.004(3) 0.002(3) 0.005(3) C28 0.085(8) 0.067(6) 0.072(7) -0.027(5) 0.050(7) -0.009(6) C31 0.026(4) 0.023(3) 0.035(4) -0.007(3) 0.009(3) 0.000(3) C32 0.027(4) 0.032(4) 0.051(5) 0.001(3) 0.008(3) 0.005(3) C33 0.042(5) 0.031(4) 0.065(6) -0.002(4) 0.022(4) 0.012(3) C34 0.076(7) 0.025(4) 0.081(7) -0.016(4) 0.045(5) -0.010(4) C35 0.037(5) 0.038(4) 0.109(8) -0.035(5) 0.036(5) -0.015(4) C36 0.024(4) 0.036(4) 0.087(6) -0.024(4) 0.014(4) -0.004(3) B1 0.040(5) 0.038(5) 0.063(7) -0.002(5) -0.008(5) -0.009(4) B2 0.035(5) 0.040(5) 0.045(6) -0.003(4) -0.009(4) -0.005(4) B5 0.024(4) 0.023(4) 0.041(5) -0.003(3) 0.003(4) 0.001(3) B6 0.022(4) 0.036(4) 0.036(5) -0.006(4) 0.005(4) 0.011(3) P2 0.017(3) 0.028(2) 0.034(5) 0.000(4) 0.005(4) 0.0047(18) C8 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C9 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C10 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C11 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C12 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C13 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C14 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C15 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C16 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C17 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C18 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C19 0.032(5) 0.047(5) 0.078(9) -0.021(5) 0.018(5) 0.004(4) C20 0.032(5) 0.047(5) 0.078(9) -0.021(5) 0.018(5) 0.004(4) C21 0.032(5) 0.047(5) 0.078(9) -0.021(5) 0.018(5) 0.004(4) C22 0.032(5) 0.047(5) 0.078(9) -0.021(5) 0.018(5) 0.004(4) C23 0.032(5) 0.047(5) 0.078(9) -0.021(5) 0.018(5) 0.004(4) C24 0.032(5) 0.047(5) 0.078(9) -0.021(5) 0.018(5) 0.004(4) C26 0.064(11) 0.089(13) 0.033(9) -0.010(8) 0.010(8) 0.042(10) C27 0.091(15) 0.101(15) 0.049(12) -0.011(10) 0.021(11) 0.048(12) C29 0.053(11) 0.117(16) 0.031(9) -0.016(9) 0.008(8) -0.014(10) C30 0.049(10) 0.100(14) 0.045(10) -0.018(9) 0.020(8) 0.004(9) B3 0.019(7) 0.038(4) 0.030(13) -0.002(8) -0.009(8) 0.006(4) B4 0.019(7) 0.038(4) 0.030(13) -0.002(8) -0.009(8) 0.006(4) P2A 0.023(3) 0.032(2) 0.043(5) 0.001(4) 0.012(4) 0.0050(18) C8A 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C9A 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C10A 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C11A 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C12A 0.064(3) 0.044(2) 0.060(3) -0.010(2) 0.005(3) 0.004(2) C13A 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C14A 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C15A 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C16A 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C17A 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C18A 0.035(3) 0.079(4) 0.129(7) -0.005(4) 0.036(4) -0.003(3) C19A 0.051(5) 0.045(4) 0.076(6) -0.004(4) 0.017(4) 0.014(4) C20A 0.051(5) 0.045(4) 0.076(6) -0.004(4) 0.017(4) 0.014(4) C21A 0.051(5) 0.045(4) 0.076(6) -0.004(4) 0.017(4) 0.014(4) C22A 0.051(5) 0.045(4) 0.076(6) -0.004(4) 0.017(4) 0.014(4) C23A 0.051(5) 0.045(4) 0.076(6) -0.004(4) 0.017(4) 0.014(4) C24A 0.051(5) 0.045(4) 0.076(6) -0.004(4) 0.017(4) 0.014(4) C26A 0.067(14) 0.038(10) 0.061(13) -0.018(9) 0.042(11) -0.021(9) C27A 0.12(2) 0.094(18) 0.057(15) -0.021(13) 0.065(15) -0.057(16) C29A 0.050(10) 0.039(9) 0.035(9) -0.014(8) 0.019(8) -0.008(8) C30A 0.030(8) 0.020(7) 0.021(8) -0.003(6) 0.010(6) -0.009(6) B3A 0.019(7) 0.038(4) 0.030(13) -0.002(8) -0.009(8) 0.006(4) B4A 0.019(7) 0.038(4) 0.030(13) -0.002(8) -0.009(8) 0.006(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 '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 C1 P1 B1 111.3(4) . . ? C1 P1 B2 110.1(4) . . ? C7 P1 C1 107.1(4) . . ? C7 P1 B1 112.6(4) . . ? C7 P1 B2 109.9(4) . . ? B1 P1 B2 105.9(4) . . ? C25 P3 B5 107.7(3) . . ? C25 P3 B6 107.5(3) . . ? C31 P3 C25 105.9(3) . . ? C31 P3 B5 110.2(3) . . ? C31 P3 B6 113.2(3) . . ? B5 P3 B6 111.9(4) . . ? C2 C1 P1 119.5(4) . . ? C2 C1 C6 120.0 . . ? C6 C1 P1 120.5(4) . . ? C1 C2 H2 120.0 . . ? C1 C2 C3 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 H3 120.0 . . ? C2 C3 C4 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 120.0 . . ? C4 C5 C6 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 H6 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 P1 118.0(8) . . ? C8 C7 C12 124.4(10) . . ? C12 C7 P1 116.3(8) . . ? C8A C7 P1 123.1(11) . . ? C12A C7 P1 132.8(13) . . ? C12A C7 C8A 104.0(16) . . ? C26 C25 P3 124.8(7) . . ? C26 C25 C30 112.8(10) . . ? C30 C25 P3 122.3(7) . . ? C26A C25 P3 119.2(8) . . ? C26A C25 C30A 126.2(10) . . ? C30A C25 P3 114.6(7) . . ? C27 C28 H28 116.4 . . ? C27 C28 C29 127.2(11) . . ? C29 C28 H28 116.4 . . ? C27A C28 H28A 123.1 . . ? C27A C28 C29A 113.9(11) . . ? C29A C28 H28A 123.1 . . ? C32 C31 P3 119.8(2) . . ? C36 C31 P3 120.1(2) . . ? C36 C31 C32 120.0 . . ? C31 C32 H32 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 H34 120.0 . . ? C33 C34 C35 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C35 H35 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 H36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? H1A B1 H1B 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? P1 B2 H2A 109.5 . . ? P1 B2 H2B 109.5 . . ? P1 B2 H2C 109.5 . . ? H2A B2 H2B 109.5 . . ? H2A B2 H2C 109.5 . . ? H2B B2 H2C 109.5 . . ? P3 B5 H5A 109.5 . . ? P3 B5 H5B 109.5 . . ? P3 B5 H5C 109.5 . . ? H5A B5 H5B 109.5 . . ? H5A B5 H5C 109.5 . . ? H5B B5 H5C 109.5 . . ? P3 B6 H6A 109.5 . . ? P3 B6 H6B 109.5 . . ? P3 B6 H6C 109.5 . . ? H6A B6 H6B 109.5 . . ? H6A B6 H6C 109.5 . . ? H6B B6 H6C 109.5 . . ? C13 P2 B3 115.9(14) . . ? C13 P2 B4 112.6(12) . . ? C19 P2 C13 106.0(10) . . ? C19 P2 B3 108.7(11) . . ? C19 P2 B4 109.1(13) . . ? B4 P2 B3 104.5(15) . . ? C7 C8 H8 121.5 . . ? C7 C8 C9 117.0(12) . . ? C9 C8 H8 121.5 . . ? C8 C9 H9 119.0 . . ? C10 C9 C8 121.9(14) . . ? C10 C9 H9 119.0 . . ? C9 C10 H10 120.5 . . ? C9 C10 C11 119.1(14) . . ? C11 C10 H10 120.5 . . ? C10 C11 H11 120.2 . . ? C10 C11 C12 119.5(13) . . ? C12 C11 H11 120.2 . . ? C7 C12 H12 121.6 . . ? C11 C12 C7 116.8(13) . . ? C11 C12 H12 121.6 . . ? C14 C13 P2 115.4(16) . . ? C18 C13 P2 124.4(19) . . ? C18 C13 C14 120.2(16) . . ? C13 C14 H14 121.5 . . ? C15 C14 C13 117(2) . . ? C15 C14 H14 121.5 . . ? C14 C15 H15 118.9 . . ? C16 C15 C14 122(2) . . ? C16 C15 H15 118.9 . . ? C15 C16 H16 117.6 . . ? C15 C16 C17 125(2) . . ? C17 C16 H16 117.6 . . ? C16 C17 H17 124.2 . . ? C18 C17 C16 112(2) . . ? C18 C17 H17 124.2 . . ? C13 C18 C17 124(2) . . ? C13 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? C20 C19 P2 124.2(14) . . ? C20 C19 C24 115.3(17) . . ? C24 C19 P2 120.5(12) . . ? C19 C20 H20 118.3 . . ? C21 C20 C19 123.4(19) . . ? C21 C20 H20 118.3 . . ? C20 C21 H21 121.1 . . ? C20 C21 C22 117.7(19) . . ? C22 C21 H21 121.1 . . ? C21 C22 H22 118.6 . . ? C23 C22 C21 122.8(17) . . ? C23 C22 H22 118.6 . . ? C22 C23 H23 122.1 . . ? C22 C23 C24 115.9(17) . . ? C24 C23 H23 122.1 . . ? C19 C24 H24 117.6 . . ? C23 C24 C19 124.8(18) . . ? C23 C24 H24 117.6 . . ? C25 C26 H26 115.7 . . ? C27 C26 C25 128.5(13) . . ? C27 C26 H26 115.7 . . ? C28 C27 C26 113.2(13) . . ? C28 C27 H27 123.4 . . ? C26 C27 H27 123.4 . . ? C28 C29 H29 122.7 . . ? C30 C29 C28 114.6(12) . . ? C30 C29 H29 122.7 . . ? C25 C30 H30 118.2 . . ? C29 C30 C25 123.6(12) . . ? C29 C30 H30 118.2 . . ? P2 B3 H3A 109.5 . . ? P2 B3 H3B 109.5 . . ? P2 B3 H3C 109.5 . . ? H3A B3 H3B 109.5 . . ? H3A B3 H3C 109.5 . . ? H3B B3 H3C 109.5 . . ? P2 B4 H4A 109.5 . . ? P2 B4 H4B 109.5 . . ? P2 B4 H4C 109.5 . . ? H4A B4 H4B 109.5 . . ? H4A B4 H4C 109.5 . . ? H4B B4 H4C 109.5 . . ? C13A P2A C19A 106.7(11) . . ? C13A P2A B3A 109.5(12) . . ? C13A P2A B4A 109.7(10) . . ? C19A P2A B3A 112.4(10) . . ? C19A P2A B4A 110.2(11) . . ? B4A P2A B3A 108.3(13) . . ? C7 C8A H8A 113.4 . . ? C9A C8A C7 133(2) . . ? C9A C8A H8A 113.4 . . ? C8A C9A H9A 122.6 . . ? C10A C9A C8A 115(2) . . ? C10A C9A H9A 122.6 . . ? C9A C10A H10A 121.3 . . ? C9A C10A C11A 117(3) . . ? C11A C10A H10A 121.3 . . ? C10A C11A H11A 118.9 . . ? C10A C11A C12A 122(3) . . ? C12A C11A H11A 118.9 . . ? C7 C12A C11A 128(2) . . ? C7 C12A H12A 115.8 . . ? C11A C12A H12A 115.8 . . ? C14A C13A P2A 118.8(18) . . ? C18A C13A P2A 117.2(17) . . ? C18A C13A C14A 124.1(16) . . ? C13A C14A H14A 121.2 . . ? C13A C14A C15A 118(2) . . ? C15A C14A H14A 121.2 . . ? C14A C15A H15A 121.3 . . ? C14A C15A C17A 117(2) . . ? C17A C15A H15A 121.3 . . ? C17A C16A H16A 119.8 . . ? C17A C16A C18A 120(2) . . ? C18A C16A H16A 119.8 . . ? C15A C17A H17A 119.4 . . ? C16A C17A C15A 121(2) . . ? C16A C17A H17A 119.4 . . ? C13A C18A C16A 119(2) . . ? C13A C18A H18A 120.3 . . ? C16A C18A H18A 120.3 . . ? C20A C19A P2A 117.7(14) . . ? C24A C19A P2A 119.8(13) . . ? C24A C19A C20A 122.5(14) . . ? C19A C20A H20A 120.1 . . ? C19A C20A C21A 119.9(17) . . ? C21A C20A H20A 120.1 . . ? C20A C21A H21A 121.2 . . ? C20A C21A C22A 117.7(18) . . ? C22A C21A H21A 121.2 . . ? C21A C22A H22A 119.4 . . ? C23A C22A C21A 121.2(18) . . ? C23A C22A H22A 119.4 . . ? C22A C23A H23A 121.4 . . ? C22A C23A C24A 117.2(18) . . ? C24A C23A H23A 121.4 . . ? C19A C24A C23A 121.5(16) . . ? C19A C24A H24A 119.2 . . ? C23A C24A H24A 119.2 . . ? C25 C26A H26A 122.0 . . ? C25 C26A C27A 115.9(13) . . ? C27A C26A H26A 122.0 . . ? C28 C27A C26A 126.2(15) . . ? C28 C27A H27A 116.9 . . ? C26A C27A H27A 116.9 . . ? C28 C29A H29A 118.5 . . ? C30A C29A C28 123.0(12) . . ? C30A C29A H29A 118.5 . . ? C25 C30A H30A 122.6 . . ? C29A C30A C25 114.8(11) . . ? C29A C30A H30A 122.6 . . ? P2A B3A H3AA 109.5 . . ? P2A B3A H3AB 109.5 . . ? P2A B3A H3AC 109.5 . . ? H3AA B3A H3AB 109.5 . . ? H3AA B3A H3AC 109.5 . . ? H3AB B3A H3AC 109.5 . . ? P2A B4A H4AA 109.5 . . ? P2A B4A H4AB 109.5 . . ? P2A B4A H4AC 109.5 . . ? H4AA B4A H4AB 109.5 . . ? H4AA B4A H4AC 109.5 . . ? H4AB B4A H4AC 109.5 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 B6 2.700(7) 3_666 ? P1 C1 1.825(6) . ? P1 C7 1.824(9) . ? P1 B1 1.907(11) . ? P1 B2 1.930(9) . ? P3 C25 1.823(7) . ? P3 C31 1.817(4) . ? P3 B5 1.906(8) . ? P3 B6 1.909(7) . ? C1 C2 1.374(4) . ? C1 C6 1.376(4) . ? C2 H2 0.9500 . ? C2 C3 1.375(4) . ? C3 H3 0.9500 . ? C3 C4 1.375(4) . ? C4 H4 0.9500 . ? C4 C5 1.374(4) . ? C5 H5 0.9500 . ? C5 C6 1.375(4) . ? C6 H6 0.9500 . ? C7 C8 1.284(15) . ? C7 C12 1.400(16) . ? C7 C8A 1.427(13) . ? C7 C12A 1.355(13) . ? C25 C26 1.382(11) . ? C25 C30 1.401(11) . ? C25 C26A 1.317(11) . ? C25 C30A 1.398(10) . ? C28 H28 0.9500 . ? C28 H28A 0.9500 . ? C28 C27 1.322(12) . ? C28 C29 1.398(11) . ? C28 C27A 1.366(12) . ? C28 C29A 1.434(11) . ? C31 C32 1.378(3) . ? C31 C36 1.378(3) . ? C32 H32 0.9500 . ? C32 C33 1.378(3) . ? C33 H33 0.9500 . ? C33 C34 1.378(3) . ? C34 H34 0.9500 . ? C34 C35 1.378(3) . ? C35 H35 0.9500 . ? C35 C36 1.378(3) . ? C36 H36 0.9500 . ? B1 H1A 1.2000 . ? B1 H1B 1.2000 . ? B1 H1C 1.2000 . ? B2 H2A 1.2000 . ? B2 H2B 1.2000 . ? B2 H2C 1.2000 . ? B5 H5A 1.2000 . ? B5 H5B 1.2000 . ? B5 H5C 1.2000 . ? B6 H6A 1.2000 . ? B6 H6B 1.2000 . ? B6 H6C 1.2000 . ? P2 C13 1.867(9) . ? P2 C19 1.75(2) . ? P2 B3 1.94(3) . ? P2 B4 1.94(3) . ? C8 H8 0.9500 . ? C8 C9 1.392(16) . ? C9 H9 0.9500 . ? C9 C10 1.367(19) . ? C10 H10 0.9500 . ? C10 C11 1.37(2) . ? C11 H11 0.9500 . ? C11 C12 1.389(17) . ? C12 H12 0.9500 . ? C13 C14 1.41(3) . ? C13 C18 1.31(3) . ? C14 H14 0.9500 . ? C14 C15 1.37(2) . ? C15 H15 0.9500 . ? C15 C16 1.28(3) . ? C16 H16 0.9500 . ? C16 C17 1.43(4) . ? C17 H17 0.9500 . ? C17 C18 1.42(2) . ? C18 H18 0.9500 . ? C19 C20 1.390(13) . ? C19 C24 1.400(13) . ? C20 H20 0.9500 . ? C20 C21 1.384(13) . ? C21 H21 0.9500 . ? C21 C22 1.392(14) . ? C22 H22 0.9500 . ? C22 C23 1.389(13) . ? C23 H23 0.9500 . ? C23 C24 1.391(13) . ? C24 H24 0.9500 . ? C26 H26 0.9500 . ? C26 C27 1.371(12) . ? C27 H27 0.9500 . ? C29 H29 0.9500 . ? C29 C30 1.397(12) . ? C30 H30 0.9500 . ? B3 H3A 1.2000 . ? B3 H3B 1.2000 . ? B3 H3C 1.2000 . ? B4 H4A 1.2000 . ? B4 H4B 1.2000 . ? B4 H4C 1.2000 . ? P2A C13A 1.866(9) . ? P2A C19A 1.878(9) . ? P2A B3A 1.92(3) . ? P2A B4A 1.88(3) . ? C8A H8A 0.9500 . ? C8A C9A 1.398(13) . ? C9A H9A 0.9500 . ? C9A C10A 1.357(14) . ? C10A H10A 0.9500 . ? C10A C11A 1.371(14) . ? C11A H11A 0.9500 . ? C11A C12A 1.376(14) . ? C12A H12A 0.9500 . ? C13A C14A 1.38(3) . ? C13A C18A 1.33(3) . ? C14A H14A 0.9500 . ? C14A C15A 1.38(3) . ? C15A H15A 0.9500 . ? C15A C17A 1.45(4) . ? C16A H16A 0.9500 . ? C16A C17A 1.33(3) . ? C16A C18A 1.36(2) . ? C17A H17A 0.9500 . ? C18A H18A 0.9500 . ? C19A C20A 1.35(2) . ? C19A C24A 1.28(2) . ? C20A H20A 0.9500 . ? C20A C21A 1.39(2) . ? C21A H21A 0.9500 . ? C21A C22A 1.40(2) . ? C22A H22A 0.9500 . ? C22A C23A 1.36(2) . ? C23A H23A 0.9500 . ? C23A C24A 1.42(2) . ? C24A H24A 0.9500 . ? C26A H26A 0.9500 . ? C26A C27A 1.373(12) . ? C27A H27A 0.9500 . ? C29A H29A 0.9500 . ? C29A C30A 1.387(12) . ? C30A H30A 0.9500 . ? B3A H3AA 1.2000 . ? B3A H3AB 1.2000 . ? B3A H3AC 1.2000 . ? B4A H4AA 1.2000 . ? B4A H4AB 1.2000 . ? B4A H4AC 1.2000 . ?