#------------------------------------------------------------------------------ #$Date: 2021-08-05 04:20:23 +0300 (Thu, 05 Aug 2021) $ #$Revision: 267955 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/79/7707955.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_7707955 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 'C48 H72 B6 Nd O3 P3' _chemical_formula_sum 'C48 H72 B6 Nd O3 P3' _chemical_formula_weight 999.06 _chemical_name_common Pr(Ph-PDB)3(THF)3 _chemical_name_systematic Nd(BH3Ph2BH3)3(THF)3 _chemical_properties_physical Air-sensitive,Moisture-sensitive,Heat-sensitive,Oxygen-sensitive _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-09-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 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 97.233(5) _cell_angle_beta 96.868(5) _cell_angle_gamma 111.125(5) _cell_formula_units_Z 2 _cell_length_a 11.5469(19) _cell_length_b 14.970(3) _cell_length_c 17.592(3) _cell_measurement_reflns_used 8654 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 2.3015 _cell_measurement_theta_min 23.25 _cell_volume 2768.9(9) _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 0.0877 _diffrn_reflns_av_unetI/netI 0.1038 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 37473 _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 26.352 _diffrn_reflns_theta_min 2.061 _exptl_absorpt_coefficient_mu 1.059 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0728 before and 0.0623 after correction. The Ratio of minimum to maximum transmission is 0.8367. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour 'pale blue' _exptl_crystal_density_diffrn 1.198 _exptl_crystal_description lath-like _exptl_crystal_F_000 1038 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _refine_diff_density_max 2.474 _refine_diff_density_min -1.268 _refine_diff_density_rms 0.130 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 493 _refine_ls_number_reflns 11206 _refine_ls_number_restraints 24 _refine_ls_restrained_S_all 1.033 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0658 _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^)+(0.0876P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1452 _refine_ls_wR_factor_ref 0.1634 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7897 _reflns_number_total 11206 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01932e2.cif _cod_data_source_block dal1924 _cod_database_code 7707955 _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 0.969 _shelx_estimated_absorpt_t_min 0.832 _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 C31-C32 = C32-C33 = C33-C34 = C34-C35 = C35-C36 = C36-C31 1.39 with sigma of 0.01 C31A-C32A = C32A-C33A = C33A-C34A = C34A-C35A = C35A-C36A = C36A-C31A 1.39 with sigma of 0.01 C51-C52 = C52-C53 = C53-C54 = C54-C55 = C55-C56 = C56-C51 1.39 with sigma of 0.01 C51A-C52A = C52A-C53A = C53A-C54A = C54A-C55A = C55A-C56A = C56A-C51A 1.39 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(C31A) = Uanis(C32A) = Uanis(C33A) = Uanis(C34A) = Uanis(C35A) = Uanis(C36A) Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56) = Uanis(C51A) = Uanis(C52A) = Uanis(C53A) = Uanis(C54A) = Uanis(C55A) = Uanis(C56A) Uanis(O1) = Uanis(C71) = Uanis(C72) = Uanis(C73) = Uanis(C74) = Uanis(O1A) = Uanis(C71A) = Uanis(C72A) = Uanis(C73A) = Uanis(C74A) 4. Others Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34A)=Sof(C35A)= Sof(H35A)=Sof(C36A)=Sof(H36A)=Sof(C31A)=1-FVAR(1) Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)= Sof(H35)=Sof(C36)=Sof(H36)=FVAR(1) Sof(C51A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(H53A)=Sof(C54A)=Sof(H54A)= Sof(C55A)=Sof(H55A)=Sof(C56A)=Sof(H56A)=1-FVAR(2) Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)= Sof(H55)=Sof(C56)=Sof(H56)=FVAR(2) Sof(O1A)=Sof(C71A)=Sof(H71C)=Sof(H71D)=Sof(C72A)=Sof(H72C)=Sof(H72D)= Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74C)=Sof(H74D)=1-FVAR(3) Sof(O1)=Sof(C71)=Sof(H71A)=Sof(H71B)=Sof(C72)=Sof(H72A)=Sof(H72B)=Sof(C73)= Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=FVAR(3) 5.a Free rotating group: C32A(C33A,C34A,C35A,C36A,C31A) 5.b Secondary CH2 refined with riding coordinates: C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B), C74(H74A,H74B), C71A(H71C, H71D), C72A(H72C,H72D), C73A(H73C,H73D), C74A(H74C,H74D), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B), C94(H94A,H94B) 5.c Aromatic/amide H refined with riding coordinates: C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C32A(H32A), C33A(H33A), C34A(H34A), C35A(H35A), C36A(H36A), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C52A(H52A), C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66) 5.d Fitted pentagon refined as free rotating group: O1A(C71A,C72A,C73A,C74A) 5.e Fitted hexagon refined as free rotating group: C51A(C52A,C53A,C54A,C55A,C56A) 5.f Idealised Me refined as rotating group: B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), B5(H5A, H5B,H5C), B6(H6A,H6B,H6C) ; _shelx_res_file ; TITL dal1924_a.res in P-1 dal1924.res created by SHELXL-2018/3 at 17:42:45 on 04-Sep-2019 REM Old TITL Dal19_24 in P1 sample #19121 TVF_Nd(PDB) REM SHELXT solution in P-1 REM R1 0.140, Rweak 0.028, Alpha 0.038, Orientation as input REM Formula found by SHELXT: C53 O6 P3 Nd CELL 0.71073 11.5469 14.97 17.592 97.233 96.868 111.125 ZERR 2 0.0019 0.003 0.003 0.005 0.005 0.005 LATT 1 SFAC C H B Nd O P UNIT 96 144 12 2 6 6 DFIX 1.39 0.01 C31 C32 C32 C33 C33 C34 C34 C35 C35 C36 C36 C31 DFIX 1.39 0.01 C31A C32A C32A C33A C33A C34A C34A C35A C35A C36A C36A C31A DFIX 1.39 0.01 C51 C52 C52 C53 C53 C54 C54 C55 C55 C56 C56 C51 DFIX 1.39 0.01 C51A C52A C52A C53A C53A C54A C54A C55A C55A C56A C56A C51A EADP C31 C32 C33 C34 C35 C36 C31A C32A C33A C34A C35A C36A EADP C51 C52 C53 C54 C55 C56 C51A C52A C53A C54A C55A C56A EADP O1 C71 C72 C73 C74 O1A C71A C72A C73A C74A L.S. 10 0 0 PLAN 20 SIZE 0.03 0.07 0.18 TEMP -123 FREE B1 Nd1 FREE B3 Nd1 FREE B2 Nd1 FREE B5 Nd1 list 4 ABIN fmap 2 53 acta OMIT 0 0 1 OMIT 0 -1 1 OMIT 0 1 0 OMIT -1 0 1 OMIT -1 1 0 OMIT 1 0 0 REM REM REM WGHT 0.087600 FVAR 0.35872 0.72069 0.75318 0.67005 B1 3 0.529978 0.515030 0.690258 11.00000 0.02948 0.03690 = 0.04202 0.00891 0.00962 0.01527 AFIX 137 1.2000 H1A 2 0.541676 0.439423 0.695339 11.00000 -1.50000 H1B 2 0.608750 0.561946 0.656751 11.00000 -1.50000 H1C 2 0.427039 0.498902 0.654678 11.00000 -1.50000 AFIX 0 B2 3 0.717107 0.610449 0.847157 11.00000 0.02896 0.05146 = 0.03200 0.00834 0.01144 0.02112 AFIX 137 1.2000 H2A 2 0.730143 0.649608 0.913222 11.00000 -1.50000 H2B 2 0.794649 0.661977 0.815366 11.00000 -1.50000 H2C 2 0.730165 0.534401 0.846578 11.00000 -1.50000 AFIX 0 C11 1 0.532639 0.702649 0.790783 11.00000 0.04785 0.03915 = 0.03260 0.00907 0.01624 0.02029 C12 1 0.417365 0.705630 0.764219 11.00000 0.06147 0.04524 = 0.07094 -0.00694 -0.01658 0.02736 AFIX 43 H12 2 0.345268 0.646893 0.747143 11.00000 -1.20000 AFIX 0 C13 1 0.406866 0.794961 0.762480 11.00000 0.07888 0.06418 = 0.08934 -0.00698 -0.03458 0.04213 AFIX 43 H13 2 0.326803 0.796726 0.744871 11.00000 -1.20000 AFIX 0 C14 1 0.508762 0.879616 0.785445 11.00000 0.09486 0.04755 = 0.05674 0.02121 0.01257 0.03554 AFIX 43 H14 2 0.500567 0.940019 0.782333 11.00000 -1.20000 AFIX 0 C15 1 0.622722 0.877624 0.812948 11.00000 0.07158 0.03977 = 0.13030 0.02927 0.02742 0.01282 AFIX 43 H15 2 0.694180 0.936755 0.830203 11.00000 -1.20000 AFIX 0 C16 1 0.634465 0.789041 0.815766 11.00000 0.04497 0.04467 = 0.12624 0.01814 0.02184 0.01438 AFIX 43 H16 2 0.714291 0.788126 0.835309 11.00000 -1.20000 AFIX 0 C21 1 0.429810 0.516778 0.843536 11.00000 0.02632 0.04323 = 0.05373 0.02243 0.00882 0.01957 C22 1 0.339688 0.427508 0.807223 11.00000 0.04350 0.06179 = 0.05193 0.02401 0.00733 0.01205 AFIX 43 H22 2 0.340297 0.402171 0.755038 11.00000 -1.20000 AFIX 0 C23 1 0.247138 0.373746 0.846564 11.00000 0.04812 0.08236 = 0.06873 0.04370 0.01140 0.00734 AFIX 43 H23 2 0.184736 0.312798 0.820627 11.00000 -1.20000 AFIX 0 C24 1 0.246268 0.408130 0.921041 11.00000 0.03706 0.09906 = 0.09226 0.07090 0.03236 0.02877 AFIX 43 H24 2 0.183251 0.371170 0.947252 11.00000 -1.20000 AFIX 0 C25 1 0.336486 0.496864 0.959599 11.00000 0.06404 0.09021 = 0.06372 0.04174 0.03778 0.03494 AFIX 43 H25 2 0.336187 0.520714 1.012209 11.00000 -1.20000 AFIX 0 C26 1 0.427794 0.550793 0.920256 11.00000 0.04531 0.07056 = 0.05745 0.02289 0.02564 0.02717 AFIX 43 H26 2 0.489661 0.611853 0.946428 11.00000 -1.20000 AFIX 0 P1 6 0.549957 0.586838 0.792811 11.00000 0.02781 0.03646 = 0.03732 0.01103 0.00958 0.01340 B3 3 0.735114 0.345138 0.771472 11.00000 0.05020 0.02981 = 0.04032 0.01393 0.01025 0.01593 AFIX 137 1.2000 H3A 2 0.784806 0.348796 0.715173 11.00000 -1.50000 H3B 2 0.798132 0.413570 0.821673 11.00000 -1.50000 H3C 2 0.632383 0.347116 0.754486 11.00000 -1.50000 AFIX 0 B4 3 0.877482 0.218639 0.849021 11.00000 0.05565 0.06235 = 0.05307 0.01649 0.00849 0.03155 AFIX 137 1.2000 H4A 2 0.857866 0.140469 0.867004 11.00000 -1.50000 H4B 2 0.930054 0.281426 0.905201 11.00000 -1.50000 H4C 2 0.942865 0.229075 0.800078 11.00000 -1.50000 AFIX 0 B5 3 0.881916 0.673999 0.646506 11.00000 0.04872 0.03121 = 0.03142 0.01305 0.00379 0.01756 AFIX 137 1.2000 H5A 2 0.794979 0.693489 0.663268 11.00000 -1.50000 H5B 2 0.938001 0.661257 0.703412 11.00000 -1.50000 H5C 2 0.842962 0.601266 0.597878 11.00000 -1.50000 AFIX 0 B6 3 1.139964 0.760826 0.580398 11.00000 0.02800 0.06025 = 0.06261 -0.01179 0.01344 0.00466 AFIX 137 1.2000 H6A 2 1.110012 0.695927 0.525422 11.00000 -1.50000 H6B 2 1.193088 0.741053 0.634751 11.00000 -1.50000 H6C 2 1.209328 0.834774 0.564364 11.00000 -1.50000 AFIX 0 PART 1 C31 1 0.627121 0.130143 0.724543 21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 C32 1 0.684907 0.078896 0.682641 21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H32 2 0.771870 0.092113 0.698773 21.00000 -1.20000 AFIX 0 C33 1 0.617015 0.008304 0.617209 21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H33 2 0.656971 -0.027009 0.589033 21.00000 -1.20000 AFIX 0 C34 1 0.489838 -0.010003 0.593488 21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H34 2 0.443098 -0.058063 0.548829 21.00000 -1.20000 AFIX 0 C35 1 0.430697 0.041026 0.634235 21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H35 2 0.343834 0.027925 0.617828 21.00000 -1.20000 AFIX 0 C36 1 0.500043 0.112025 0.699761 21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H36 2 0.460463 0.148047 0.727499 21.00000 -1.20000 AFIX 6 PART 0 PART 2 C32A 1 0.738640 0.112607 0.681330 -21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H32A 2 0.826603 0.144898 0.700561 -21.00000 -1.20000 AFIX 5 C33A 1 0.695830 0.043238 0.613179 -21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H33A 2 0.754513 0.028052 0.585899 -21.00000 -1.20000 AFIX 5 C34A 1 0.567110 -0.003840 0.585028 -21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H34A 2 0.537823 -0.051135 0.538434 -21.00000 -1.20000 AFIX 5 C35A 1 0.481220 0.018231 0.624999 -21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H35A 2 0.393255 -0.014050 0.605771 -21.00000 -1.20000 AFIX 5 C36A 1 0.524031 0.087529 0.693100 -21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 43 H36A 2 0.465324 0.102673 0.720383 -21.00000 -1.20000 AFIX 5 C31A 1 0.652741 0.134687 0.721300 -21.00000 0.06492 0.04521 = 0.04047 0.00206 0.01194 0.01386 AFIX 0 PART 0 C41 1 0.608722 0.207608 0.876934 11.00000 0.04371 0.02893 = 0.03910 0.00511 0.00271 0.00404 C42 1 0.522587 0.251391 0.877635 11.00000 0.06591 0.05518 = 0.05053 0.01260 0.01680 0.02388 AFIX 43 H42 2 0.521588 0.295229 0.843166 11.00000 -1.20000 AFIX 0 C43 1 0.435594 0.231600 0.929275 11.00000 0.06750 0.06515 = 0.08710 0.01419 0.03304 0.02977 AFIX 43 H43 2 0.374762 0.260648 0.929111 11.00000 -1.20000 AFIX 0 C44 1 0.440447 0.170163 0.979292 11.00000 0.10129 0.06188 = 0.07388 0.01264 0.04141 0.01291 AFIX 43 H44 2 0.382205 0.156882 1.014217 11.00000 -1.20000 AFIX 0 C45 1 0.525841 0.127344 0.980799 11.00000 0.12735 0.04564 = 0.06114 0.02087 0.03587 0.01615 AFIX 43 H45 2 0.527880 0.085667 1.017002 11.00000 -1.20000 AFIX 0 C46 1 0.610301 0.144546 0.929310 11.00000 0.08451 0.03997 = 0.05055 0.01886 0.02010 0.01502 AFIX 43 H46 2 0.669148 0.113627 0.929542 11.00000 -1.20000 AFIX 0 PART 1 C51 1 0.898082 0.796978 0.519695 31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 C52 1 0.959447 0.867124 0.478087 31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H52 2 1.045738 0.907462 0.496560 31.00000 -1.20000 AFIX 0 C53 1 0.898487 0.879623 0.410907 31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H53 2 0.941954 0.928986 0.383868 31.00000 -1.20000 AFIX 0 C54 1 0.773584 0.820207 0.382602 31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H54 2 0.730933 0.828395 0.335980 31.00000 -1.20000 AFIX 0 C55 1 0.710850 0.748499 0.422715 31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H55 2 0.624966 0.707637 0.403481 31.00000 -1.20000 AFIX 0 C56 1 0.772756 0.736221 0.490576 31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H56 2 0.729753 0.686332 0.517310 31.00000 -1.20000 AFIX 66 PART 0 PART 2 C51A 1 0.936018 0.810668 0.527941 -31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 C52A 1 1.024745 0.869310 0.489890 -31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H52A 2 1.112201 0.890085 0.510053 -31.00000 -1.20000 AFIX 65 C53A 1 0.985511 0.897553 0.422338 -31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H53A 2 1.046153 0.937632 0.396332 -31.00000 -1.20000 AFIX 65 C54A 1 0.857550 0.867156 0.392836 -31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H54A 2 0.830736 0.886459 0.346667 -31.00000 -1.20000 AFIX 65 C55A 1 0.768821 0.808515 0.430886 -31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H55A 2 0.681366 0.787740 0.410723 -31.00000 -1.20000 AFIX 65 C56A 1 0.808054 0.780271 0.498439 -31.00000 0.05449 0.04481 = 0.04347 0.01694 0.00315 0.01875 AFIX 43 H56A 2 0.747412 0.740192 0.524445 -31.00000 -1.20000 AFIX 0 PART 0 C61 1 1.031186 0.884841 0.682115 11.00000 0.05433 0.02886 = 0.04085 0.01238 0.02587 0.00919 C62 1 1.154852 0.935184 0.720013 11.00000 0.06200 0.04273 = 0.04917 -0.00045 0.02284 0.01506 AFIX 43 H62 2 1.218842 0.913861 0.705988 11.00000 -1.20000 AFIX 0 C63 1 1.186875 1.016395 0.778232 11.00000 0.08633 0.04746 = 0.05766 -0.00474 0.02392 0.01060 AFIX 43 H63 2 1.271802 1.050319 0.804074 11.00000 -1.20000 AFIX 0 C64 1 1.092978 1.046774 0.797757 11.00000 0.11601 0.04316 = 0.05532 0.00169 0.04334 0.02211 AFIX 43 H64 2 1.113963 1.102156 0.837445 11.00000 -1.20000 AFIX 0 C65 1 0.969839 0.998486 0.760919 11.00000 0.08937 0.04669 = 0.07392 0.01550 0.04570 0.03549 AFIX 43 H65 2 0.906204 1.020364 0.774746 11.00000 -1.20000 AFIX 0 C66 1 0.939578 0.917651 0.703468 11.00000 0.07575 0.03859 = 0.05345 0.01205 0.02864 0.02643 AFIX 43 H66 2 0.854360 0.883898 0.678105 11.00000 -1.20000 AFIX 0 PART 1 O1 5 0.977227 0.581506 0.823198 41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 C71 1 1.098530 0.660627 0.819065 41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H71A 2 1.090381 0.724632 0.824564 41.00000 -1.20000 H71B 2 1.126568 0.648042 0.769200 41.00000 -1.20000 AFIX 0 C72 1 1.190979 0.657143 0.888392 41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H72A 2 1.237720 0.616583 0.871235 41.00000 -1.20000 H72B 2 1.252502 0.723521 0.911839 41.00000 -1.20000 AFIX 0 C73 1 1.115696 0.615547 0.943245 41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H73A 2 1.115295 0.667732 0.983696 41.00000 -1.20000 H73B 2 1.150872 0.573468 0.969045 41.00000 -1.20000 AFIX 0 C74 1 0.988539 0.558597 0.902096 41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H74A 2 0.927036 0.574560 0.930078 41.00000 -1.20000 H74B 2 0.970652 0.488271 0.898996 41.00000 -1.20000 AFIX 56 PART 0 PART 2 O1A 5 0.985678 0.596466 0.829425 -41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 C71A 1 1.055959 0.696718 0.831166 -41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H71C 2 1.098362 0.704852 0.785357 -41.00000 -1.20000 H71D 2 0.999138 0.732901 0.829842 -41.00000 -1.20000 AFIX 55 C72A 1 1.147026 0.733072 0.900863 -41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H72C 2 1.233073 0.758629 0.888456 -41.00000 -1.20000 H72D 2 1.133850 0.786678 0.932942 -41.00000 -1.20000 AFIX 55 C73A 1 1.133029 0.655289 0.942198 -41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H73C 2 1.113144 0.671618 0.994086 -41.00000 -1.20000 H73D 2 1.212368 0.643569 0.949601 -41.00000 -1.20000 AFIX 55 C74A 1 1.033310 0.570862 0.898047 -41.00000 0.04110 0.07787 = 0.03853 0.00510 -0.00681 0.02284 AFIX 23 H74C 2 1.064859 0.518680 0.884290 -41.00000 -1.20000 H74D 2 0.965635 0.546729 0.928776 -41.00000 -1.20000 AFIX 0 PART 0 C81 1 1.004543 0.487503 0.597079 11.00000 0.05513 0.03880 = 0.03018 0.01255 0.01898 0.01715 AFIX 23 H81A 2 1.040899 0.556869 0.592056 11.00000 -1.20000 H81B 2 0.930811 0.452809 0.554812 11.00000 -1.20000 AFIX 0 C82 1 1.101135 0.442722 0.592940 11.00000 0.04342 0.06244 = 0.04617 0.00347 0.01837 0.02398 AFIX 23 H82A 2 1.187630 0.492806 0.609476 11.00000 -1.20000 H82B 2 1.092986 0.408461 0.539444 11.00000 -1.20000 AFIX 0 C83 1 1.071390 0.371562 0.648962 11.00000 0.05208 0.05949 = 0.04482 0.00269 0.00985 0.04041 AFIX 23 H83A 2 0.997915 0.310902 0.625676 11.00000 -1.20000 H83B 2 1.144804 0.355346 0.666824 11.00000 -1.20000 AFIX 0 C84 1 1.041764 0.431785 0.714222 11.00000 0.05957 0.05819 = 0.03979 0.01358 0.00977 0.04011 AFIX 23 H84A 2 0.992696 0.389845 0.747760 11.00000 -1.20000 H84B 2 1.120154 0.481157 0.746725 11.00000 -1.20000 AFIX 0 C91 1 0.621012 0.431601 0.524276 11.00000 0.06367 0.03818 = 0.03457 0.00642 -0.00324 0.01989 AFIX 23 H91A 2 0.673175 0.496518 0.514626 11.00000 -1.20000 H91B 2 0.539517 0.432681 0.535570 11.00000 -1.20000 AFIX 0 C92 1 0.600258 0.354070 0.455446 11.00000 0.12336 0.06783 = 0.04952 0.00466 -0.01567 0.02562 AFIX 23 H92A 2 0.525815 0.346270 0.416928 11.00000 -1.20000 H92B 2 0.675140 0.369692 0.429794 11.00000 -1.20000 AFIX 0 C93 1 0.579010 0.264848 0.489480 11.00000 0.06199 0.04199 = 0.04872 0.00004 0.00326 0.00530 AFIX 23 H93A 2 0.604043 0.217920 0.457456 11.00000 -1.20000 H93B 2 0.489356 0.232832 0.494080 11.00000 -1.20000 AFIX 0 C94 1 0.661842 0.302211 0.568067 11.00000 0.05493 0.02489 = 0.05022 0.00723 0.00829 0.01437 AFIX 23 H94A 2 0.619362 0.266689 0.607125 11.00000 -1.20000 H94B 2 0.742191 0.292790 0.566689 11.00000 -1.20000 AFIX 0 ND1 4 0.789480 0.512921 0.718434 11.00000 0.03021 0.02922 = 0.02563 0.00868 0.00679 0.01180 O2 5 0.967047 0.478330 0.673542 11.00000 0.03950 0.04467 = 0.02880 0.01484 0.01813 0.02297 O3 5 0.686045 0.405587 0.588419 11.00000 0.03986 0.03274 = 0.02576 0.00643 0.00606 0.01503 P2 6 0.719142 0.226602 0.808414 11.00000 0.04564 0.03018 = 0.03411 0.01120 0.00525 0.01411 P3 6 0.991924 0.777985 0.607043 11.00000 0.03784 0.02537 = 0.03893 0.01015 0.01424 0.01057 HKLF 4 REM dal1924_a.res in P-1 REM wR2 = 0.1634, GooF = S = 1.034, Restrained GooF = 1.033 for all data REM R1 = 0.0658 for 7897 Fo > 4sig(Fo) and 0.1038 for all 11206 data REM 493 parameters refined using 24 restraints END WGHT 0.0876 0.0000 REM Highest difference peak 2.474, deepest hole -1.268, 1-sigma level 0.130 Q1 1 0.8001 0.5810 0.7167 11.00000 0.05 2.47 Q2 1 0.7705 0.4472 0.7206 11.00000 0.05 2.28 Q3 1 0.7018 0.4813 0.6811 11.00000 0.05 1.13 Q4 1 0.8792 0.5412 0.7540 11.00000 0.05 1.11 Q5 1 0.5131 0.3571 0.4897 11.00000 0.05 0.95 Q6 1 0.7173 0.2850 0.7938 11.00000 0.05 0.89 Q7 1 0.5256 0.6380 0.7846 11.00000 0.05 0.87 Q8 1 0.9804 0.7149 0.6189 11.00000 0.05 0.72 Q9 1 1.1237 0.7359 0.9409 11.00000 0.05 0.71 Q10 1 1.1616 0.6459 0.9204 11.00000 0.05 0.65 Q11 1 0.9774 0.8382 0.5939 11.00000 0.05 0.64 Q12 1 0.7106 0.1466 0.8022 11.00000 0.05 0.63 Q13 1 0.5393 0.5189 0.7894 11.00000 0.05 0.60 Q14 1 1.0626 0.6613 0.9394 11.00000 0.05 0.59 Q15 1 0.5770 0.1419 0.8845 11.00000 0.05 0.56 Q16 1 0.9813 0.7156 0.6550 11.00000 0.05 0.51 Q17 1 0.8061 0.2317 0.8366 11.00000 0.05 0.49 Q18 1 1.0447 0.8567 0.6194 11.00000 0.05 0.49 Q19 1 0.8658 0.7992 0.6321 11.00000 0.05 0.48 Q20 1 0.6303 0.2880 0.4591 11.00000 0.05 0.47 ; _shelx_res_checksum 9497 _shelx_hkl_file ; -1 0 0 0.30 1.10 -1 0 0 -2.00 1.30 -1 0 0 -0.40 1.30 -1 0 0 -2.00 2.20 1 0 0 0.40 1.70 1 0 0 5.30 1.80 1 0 0 2.20 2.40 -2 0 0 624.64 26.20 -2 0 0 509.85 24.00 -2 0 0 535.15 27.20 2 0 0 622.64 25.00 2 0 0 509.35 26.90 2 0 0 525.95 25.30 -3 0 0 34.40 5.10 -3 0 0 8.30 8.30 -3 0 0 2.30 7.00 3 0 0 23.60 8.70 3 0 0 28.60 6.40 3 0 0 23.70 6.30 -4 0 0 898.21 46.60 -4 0 0 908.91 40.20 -4 0 0 957.30 44.50 4 0 0 959.80 42.10 4 0 0 947.21 42.60 4 0 0 865.31 45.70 -5 0 0 884.11 40.00 -5 0 0 924.71 45.70 -5 0 0 954.60 49.50 5 0 0 896.51 42.80 -6 0 0 13.50 13.30 -6 0 0 12.10 5.00 -6 0 0 -12.10 9.10 6 0 0 11.50 7.80 -7 0 0 109.79 21.80 -7 0 0 89.99 16.40 -8 0 0 -23.90 15.80 -8 0 0 -7.60 13.20 -9 0 0 398.76 43.20 -9 0 0 360.46 33.20 -10 0 0 163.48 33.00 -11 0 0 -16.40 26.20 -12 0 0 124.59 34.60 -13 0 0 -51.99 27.20 -13 1 0 5.20 33.10 -12 1 0 213.58 45.40 -11 1 0 -1.20 27.10 -10 1 0 -3.40 23.10 -9 1 0 312.97 36.40 -9 1 0 335.87 32.80 -8 1 0 -5.00 12.10 -8 1 0 6.60 16.80 -7 1 0 441.26 29.00 -7 1 0 472.85 34.70 6 -1 0 109.39 12.00 -6 1 0 108.69 10.10 -6 1 0 117.99 15.40 -6 1 0 180.08 22.30 5 -1 0 264.67 19.10 5 -1 0 280.97 17.30 -5 1 0 255.37 19.40 -5 1 0 269.57 24.00 -5 1 0 244.98 14.80 4 -1 0 796.12 37.60 4 -1 0 873.01 39.50 -4 1 0 771.22 41.60 -4 1 0 790.72 36.60 -4 1 0 900.81 39.00 3 -1 0 24.00 5.60 3 -1 0 19.10 7.20 -3 1 0 13.70 8.70 -3 1 0 33.20 6.40 2 -1 0 4009.40 165.08 2 -1 0 4469.15 166.48 -2 1 0 3735.13 166.78 -2 1 0 3916.61 166.78 -2 1 0 4019.40 165.08 1 -1 0 -1.10 2.50 1 -1 0 8.60 2.30 1 -1 0 -1.00 1.60 -1 1 0 0.50 1.90 -1 1 0 0.10 2.40 -1 1 0 0.50 1.40 0 -1 0 -2.20 1.10 0 -1 0 -0.80 1.50 0 -1 0 -2.80 1.60 0 -1 0 -3.60 1.40 0 1 0 -0.80 1.60 0 1 0 -1.50 1.10 -1 -1 0 14.90 5.00 -1 -1 0 9.60 3.30 -1 -1 0 8.00 3.60 1 1 0 12.10 4.70 -2 -1 0 310.67 18.90 -2 -1 0 332.47 18.50 -2 -1 0 333.37 16.00 2 1 0 309.87 18.50 2 1 0 279.37 13.60 -3 -1 0 139.19 11.00 -3 -1 0 166.08 16.10 -3 -1 0 203.98 16.70 3 1 0 177.18 13.80 3 1 0 189.38 15.80 -4 -1 0 613.34 33.00 -4 -1 0 530.25 32.90 -4 -1 0 536.35 26.70 4 1 0 553.04 29.30 4 1 0 586.74 33.20 -5 -1 0 1696.93 82.39 -5 -1 0 1626.14 74.29 -5 -1 0 1877.41 80.99 5 1 0 1811.62 77.39 5 1 0 1709.03 81.49 -6 -1 0 7.30 13.90 -6 -1 0 -10.70 5.50 -6 -1 0 3.20 11.50 6 1 0 -3.20 12.00 6 1 0 -4.30 6.80 -7 -1 0 119.29 21.30 -7 -1 0 109.09 18.90 -8 -1 0 350.76 34.00 -8 -1 0 381.06 38.70 -9 -1 0 668.03 51.59 -9 -1 0 540.75 43.90 -10 -1 0 107.69 29.80 -11 -1 0 25.10 30.00 -12 -1 0 37.70 35.70 -13 2 0 -37.10 25.90 -12 2 0 148.09 36.30 -11 2 0 81.89 31.00 -10 2 0 20.00 20.90 -9 2 0 199.98 31.50 -8 2 0 217.28 29.10 -8 2 0 139.89 17.90 -7 2 0 999.70 46.90 -7 2 0 1047.60 51.09 -7 2 0 1159.58 59.39 6 -2 0 18.10 10.70 6 -2 0 18.40 7.20 -6 2 0 27.20 9.10 -6 2 0 10.30 6.60 -6 2 0 21.10 12.60 5 -2 0 299.87 18.90 5 -2 0 350.06 23.60 -5 2 0 361.76 20.60 -5 2 0 356.66 26.30 4 -2 0 762.72 35.90 4 -2 0 809.82 39.70 -4 2 0 817.82 36.50 -4 2 0 796.12 41.00 3 -2 0 33.80 8.90 3 -2 0 20.80 6.60 3 -2 0 22.70 5.50 -3 2 0 19.00 8.80 -3 2 0 23.90 4.90 2 -2 0 95.19 7.80 2 -2 0 99.19 9.50 2 -2 0 99.49 10.30 -2 2 0 78.29 9.20 -2 2 0 79.79 8.70 1 -2 0 251.27 14.10 1 -2 0 261.77 13.70 1 -2 0 303.57 14.60 1 -2 0 268.67 13.00 -1 2 0 236.68 12.90 -1 2 0 229.98 13.70 0 -2 0 1764.22 73.79 0 -2 0 1697.83 72.99 0 -2 0 1765.72 73.79 0 -2 0 1765.72 73.59 0 2 0 1790.22 73.99 0 2 0 1700.03 73.19 -1 -2 0 896.41 44.00 -1 -2 0 1036.30 45.60 -1 -2 0 1050.09 44.30 1 2 0 996.20 44.90 -2 -2 0 117.39 11.10 -2 -2 0 126.89 12.00 -2 -2 0 108.59 13.70 -2 -2 0 126.39 14.00 2 2 0 102.19 12.90 -3 -2 0 1024.10 47.50 -3 -2 0 897.61 46.70 -3 -2 0 943.61 43.10 3 2 0 925.71 46.90 -4 -2 0 136.19 12.70 -4 -2 0 118.79 17.10 -4 -2 0 126.89 17.70 4 2 0 135.69 17.20 -5 -2 0 1046.60 49.30 -5 -2 0 1065.49 55.49 -5 -2 0 1094.89 57.59 5 2 0 1083.89 56.09 5 2 0 1106.49 51.99 -6 -2 0 -0.20 7.10 -6 -2 0 24.70 14.30 -6 -2 0 3.10 12.60 6 2 0 14.20 13.70 6 2 0 9.00 9.30 -7 -2 0 451.95 36.30 -7 -2 0 427.56 35.00 7 2 0 488.95 36.50 -8 -2 0 298.67 32.70 -8 -2 0 329.47 37.80 8 2 0 320.77 36.10 -9 -2 0 263.97 36.30 -9 -2 0 305.87 35.30 -10 -2 0 38.40 29.20 -10 -2 0 21.70 26.20 -11 -2 0 64.29 30.50 -12 -2 0 84.39 37.50 -13 3 0 -3.80 31.90 -12 3 0 256.27 42.30 -11 3 0 25.00 24.80 -10 3 0 202.88 33.00 -9 3 0 232.18 30.10 -8 3 0 -10.60 12.50 -8 3 0 2.10 8.70 7 -3 0 364.46 26.40 -7 3 0 320.47 21.00 -7 3 0 304.27 20.10 -7 3 0 312.17 27.60 6 -3 0 19.80 6.90 6 -3 0 21.50 11.70 -6 3 0 27.40 14.00 -6 3 0 30.20 7.90 5 -3 0 524.35 27.10 5 -3 0 604.64 33.00 -5 3 0 538.35 26.90 -5 3 0 535.95 32.30 4 -3 0 583.44 32.20 4 -3 0 561.54 27.90 4 -3 0 621.34 29.40 -4 3 0 515.25 26.30 -4 3 0 628.64 32.80 -4 3 0 599.34 32.60 3 -3 0 122.69 14.40 3 -3 0 146.39 12.60 3 -3 0 127.79 10.80 -3 3 0 149.59 13.80 -3 3 0 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12 -5 6 0.0634 -0.0066 12 -5 7 -0.2762 -0.0152 12 -5 8 0.0085 -0.0349 12 -5 9 0.8197 -0.0506 12 -4 0 -0.2246 0.0009 12 -4 1 -1.3927 0.0211 12 -4 2 -1.5490 0.0228 12 -4 3 -1.1833 0.0184 12 -4 4 -1.3037 0.0220 12 -4 5 -2.1526 0.0280 12 -4 6 -2.8697 0.0181 12 -4 7 -2.5398 -0.0147 12 -4 8 -1.3159 -0.0548 12 -4 9 -0.2393 -0.0784 12 -3 0 -0.1579 -0.0040 12 -3 1 -0.1589 -0.0019 12 -3 2 -0.0189 -0.0011 12 -3 3 -0.5566 0.0156 12 -3 4 -1.8132 0.0450 12 -3 5 -2.7885 0.0641 12 -3 6 -2.4929 0.0538 12 -3 7 -1.0949 0.0163 12 -3 8 0.2313 -0.0298 12 -2 0 -0.0330 0.0050 12 -2 1 -0.0822 -0.0124 12 -2 2 -0.8829 -0.0169 12 -2 3 -2.2928 -0.0013 12 -2 4 -3.2037 0.0202 12 -2 5 -2.5874 0.0278 12 -2 6 -0.6495 0.0132 12 -2 7 1.2834 -0.0186 12 -1 0 0.3566 -0.0278 12 -1 1 -1.1126 -0.0575 12 -1 2 -3.0815 -0.0683 12 -1 3 -4.3766 -0.0654 12 -1 4 -3.9463 -0.0621 12 -1 5 -1.9602 -0.0668 12 -1 6 0.2470 -0.0803 12 -1 7 1.3954 -0.0988 12 0 0 -0.5249 -0.0839 12 0 1 -2.5393 -0.1066 12 0 2 -3.8337 -0.1097 12 0 3 -3.5107 -0.1051 12 0 4 -1.7802 -0.1032 12 0 5 0.0976 -0.1092 12 0 6 0.9192 -0.1228 12 1 0 -2.7193 -0.0769 12 1 1 -3.2441 -0.0709 12 1 2 -2.2437 -0.0516 12 1 3 -0.0976 -0.0342 12 1 4 1.9286 -0.0317 12 2 0 -3.5216 -0.0816 12 2 1 -2.2827 -0.0387 12 2 2 0.0098 0.0102 12 2 3 2.1921 0.0424 12 3 0 -2.0501 -0.1877 12 3 1 -0.4586 -0.1186 13 -13 0 -1.7217 0.1453 13 -13 1 -0.4835 0.0566 13 -13 2 -0.1900 -0.0625 13 -12 0 -3.1773 0.0302 13 -12 1 -2.6958 -0.0267 13 -12 2 -2.7307 -0.0803 13 -12 3 -2.7096 -0.1136 13 -12 4 -2.2038 -0.1150 13 -11 0 -2.8182 -0.0374 13 -11 1 -3.3078 -0.0407 13 -11 2 -3.3867 -0.0377 13 -11 3 -2.7372 -0.0225 13 -11 4 -1.7461 0.0134 13 -11 5 -1.0574 0.0604 13 -10 0 -1.3139 -0.0395 13 -10 1 -1.9082 -0.0310 13 -10 2 -1.6963 -0.0209 13 -10 3 -1.0879 0.0055 13 -10 4 -0.7866 0.0486 13 -10 5 -0.8995 0.0824 13 -10 6 -0.8341 0.0782 13 -9 0 -0.1541 -0.0188 13 -9 1 -0.0485 -0.0334 13 -9 2 0.2883 -0.0359 13 -9 3 0.1423 -0.0125 13 -9 4 -0.5454 0.0171 13 -9 5 -1.0043 0.0185 13 -9 6 -0.5654 -0.0183 13 -8 0 1.0354 -0.0098 13 -8 1 1.5053 -0.0314 13 -8 2 1.3082 -0.0273 13 -8 3 0.3873 -0.0047 13 -8 4 -0.3530 0.0053 13 -8 5 -0.0385 -0.0144 13 -8 6 1.1022 -0.0460 13 -7 0 1.7527 -0.0051 13 -7 1 1.5954 -0.0049 13 -7 2 0.5460 0.0138 13 -7 3 -0.3927 0.0255 13 -7 4 -0.1037 0.0132 13 -7 5 1.3679 -0.0088 13 -7 6 2.7936 -0.0109 13 -6 0 1.4679 0.0089 13 -6 1 0.2547 0.0286 13 -6 2 -1.1731 0.0454 13 -6 3 -1.4738 0.0382 13 -6 4 -0.3342 0.0153 13 -6 5 1.2253 0.0039 13 -6 6 1.9673 0.0180 13 -5 0 1.3441 -0.0051 13 -5 1 -0.1976 0.0165 13 -5 2 -1.1425 0.0278 13 -5 3 -0.9076 0.0271 13 -5 4 -0.1323 0.0307 13 -5 5 0.1666 0.0473 13 -5 6 -0.2799 0.0642 13 -4 0 1.3765 -0.0432 13 -4 1 0.6802 -0.0278 13 -4 2 0.6616 -0.0114 13 -4 3 0.9302 0.0174 13 -4 4 0.7442 0.0636 13 -4 5 -0.0529 0.1108 13 -3 0 0.9821 -0.0288 13 -3 1 1.1469 -0.0318 13 -3 2 1.3687 -0.0257 13 -3 3 1.1697 0.0046 13 -3 4 0.5352 0.0558 13 -3 5 -0.0294 0.1062 13 -2 0 1.3341 0.0071 13 -2 1 1.0229 -0.0360 13 -2 2 0.3154 -0.0697 13 -2 3 -0.5457 -0.0750 13 -2 4 -1.0001 -0.0498 13 -1 0 1.9536 -0.0270 13 -1 1 0.6600 -0.1095 13 -1 2 -0.6993 -0.1750 13 -1 3 -1.4904 -0.1993 13 0 0 0.4771 -0.0644 13 0 1 -0.4184 -0.1499 14 -10 0 0.1074 -0.0552 14 -10 1 0.3045 -0.0526 14 -9 0 0.4450 -0.0371 14 -9 1 1.1437 -0.0623 14 -9 2 1.6446 -0.0746 14 -8 0 1.1507 -0.0240 14 -8 1 1.8489 -0.0338 14 -8 2 1.7966 -0.0229 14 -7 0 1.5201 0.0042 14 -7 1 1.6568 0.0278 14 -7 2 1.0131 0.0545 14 -6 0 1.3667 0.0199 14 -6 1 0.9300 0.0555 14 -6 2 0.1710 0.0775 14 -5 0 1.1727 -0.0263 14 -5 1 0.7830 0.0072 14 -4 0 0.4733 -0.0654 0 0 0 0.0 0.0 ; _shelx_fab_checksum 58740 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 B1 B 0.5300(7) 0.5150(5) 0.6903(4) 0.0349(16) Uani 1 1 d . . . . . H1A H 0.541676 0.439423 0.695339 0.052 Uiso 1 1 calc GR . . . . H1B H 0.608750 0.561946 0.656751 0.052 Uiso 1 1 calc GR . . . . H1C H 0.427039 0.498902 0.654678 0.052 Uiso 1 1 calc GR . . . . B2 B 0.7171(7) 0.6104(6) 0.8472(4) 0.0352(17) Uani 1 1 d . . . . . H2A H 0.730143 0.649608 0.913222 0.053 Uiso 1 1 calc GR . . . . H2B H 0.794649 0.661977 0.815366 0.053 Uiso 1 1 calc GR . . . . H2C H 0.730165 0.534401 0.846578 0.053 Uiso 1 1 calc GR . . . . C11 C 0.5326(6) 0.7026(5) 0.7908(3) 0.0378(15) Uani 1 1 d . . . . . C12 C 0.4174(8) 0.7056(5) 0.7642(5) 0.061(2) Uani 1 1 d . . . . . H12 H 0.345268 0.646893 0.747143 0.074 Uiso 1 1 calc R . . . . C13 C 0.4069(9) 0.7950(6) 0.7625(5) 0.080(3) Uani 1 1 d . . . . . H13 H 0.326803 0.796726 0.744871 0.096 Uiso 1 1 calc R . . . . C14 C 0.5088(9) 0.8796(6) 0.7854(4) 0.063(2) Uani 1 1 d . . . . . H14 H 0.500567 0.940019 0.782333 0.076 Uiso 1 1 calc R . . . . C15 C 0.6227(9) 0.8776(6) 0.8129(6) 0.081(3) Uani 1 1 d . . . . . H15 H 0.694180 0.936755 0.830203 0.097 Uiso 1 1 calc R . . . . C16 C 0.6345(8) 0.7890(6) 0.8158(6) 0.072(3) Uani 1 1 d . . . . . H16 H 0.714291 0.788126 0.835309 0.086 Uiso 1 1 calc R . . . . C21 C 0.4298(6) 0.5168(5) 0.8435(4) 0.0379(15) Uani 1 1 d . . . . . C22 C 0.3397(7) 0.4275(5) 0.8072(4) 0.054(2) Uani 1 1 d . . . . . H22 H 0.340297 0.402171 0.755038 0.064 Uiso 1 1 calc R . . . . C23 C 0.2471(7) 0.3737(7) 0.8466(5) 0.069(3) Uani 1 1 d . . . . . H23 H 0.184736 0.312798 0.820627 0.082 Uiso 1 1 calc R . . . . C24 C 0.2463(7) 0.4081(7) 0.9210(5) 0.068(3) Uani 1 1 d . . . . . H24 H 0.183251 0.371170 0.947252 0.082 Uiso 1 1 calc R . . . . C25 C 0.3365(8) 0.4969(7) 0.9596(5) 0.066(2) Uani 1 1 d . . . . . H25 H 0.336187 0.520714 1.012209 0.079 Uiso 1 1 calc R . . . . C26 C 0.4278(7) 0.5508(6) 0.9203(4) 0.0538(19) Uani 1 1 d . . . . . H26 H 0.489661 0.611853 0.946428 0.065 Uiso 1 1 calc R . . . . P1 P 0.54996(15) 0.58684(12) 0.79281(9) 0.0328(4) Uani 1 1 d . . . . . B3 B 0.7351(8) 0.3451(5) 0.7715(4) 0.0390(18) Uani 1 1 d . . . . . H3A H 0.784806 0.348796 0.715173 0.059 Uiso 1 1 calc GR . . . . H3B H 0.798132 0.413570 0.821673 0.059 Uiso 1 1 calc GR . . . . H3C H 0.632383 0.347116 0.754486 0.059 Uiso 1 1 calc GR . . . . B4 B 0.8775(8) 0.2186(7) 0.8490(5) 0.054(2) Uani 1 1 d . . . . . H4A H 0.857866 0.140469 0.867004 0.081 Uiso 1 1 calc GR . . . . H4B H 0.930054 0.281426 0.905201 0.081 Uiso 1 1 calc GR . . . . H4C H 0.942865 0.229075 0.800078 0.081 Uiso 1 1 calc GR . . . . B5 B 0.8819(7) 0.6740(5) 0.6465(4) 0.0361(17) Uani 1 1 d . . . . . H5A H 0.794979 0.693489 0.663268 0.054 Uiso 1 1 calc GR . . . . H5B H 0.938001 0.661257 0.703412 0.054 Uiso 1 1 calc GR . . . . H5C H 0.842962 0.601266 0.597878 0.054 Uiso 1 1 calc GR . . . . B6 B 1.1400(8) 0.7608(7) 0.5804(5) 0.055(2) Uani 1 1 d . . . . . H6A H 1.110012 0.695927 0.525422 0.083 Uiso 1 1 calc GR . . . . H6B H 1.193088 0.741053 0.634751 0.083 Uiso 1 1 calc GR . . . . H6C H 1.209328 0.834774 0.564364 0.083 Uiso 1 1 calc GR . . . . C31 C 0.6271(10) 0.1301(8) 0.7245(6) 0.0525(12) Uani 0.721(9) 1 d D . P A 1 C32 C 0.6849(11) 0.0789(7) 0.6826(5) 0.0525(12) Uani 0.721(9) 1 d D . P A 1 H32 H 0.771870 0.092113 0.698773 0.063 Uiso 0.721(9) 1 calc R . P A 1 C33 C 0.6170(9) 0.0083(7) 0.6172(5) 0.0525(12) Uani 0.721(9) 1 d D . P A 1 H33 H 0.656971 -0.027009 0.589033 0.063 Uiso 0.721(9) 1 calc R . P A 1 C34 C 0.4898(9) -0.0100(7) 0.5935(6) 0.0525(12) Uani 0.721(9) 1 d D . P A 1 H34 H 0.443098 -0.058063 0.548829 0.063 Uiso 0.721(9) 1 calc R . P A 1 C35 C 0.4307(11) 0.0410(7) 0.6342(5) 0.0525(12) Uani 0.721(9) 1 d D . P A 1 H35 H 0.343834 0.027925 0.617828 0.063 Uiso 0.721(9) 1 calc R . P A 1 C36 C 0.5000(10) 0.1120(7) 0.6998(6) 0.0525(12) Uani 0.721(9) 1 d D . P A 1 H36 H 0.460463 0.148047 0.727499 0.063 Uiso 0.721(9) 1 calc R . P A 1 C32A C 0.7386(15) 0.1126(15) 0.6813(11) 0.0525(12) Uani 0.279(9) 1 d D . P A 2 H32A H 0.826603 0.144898 0.700561 0.063 Uiso 0.279(9) 1 calc R . P A 2 C33A C 0.6958(18) 0.0432(14) 0.6132(10) 0.0525(12) Uani 0.279(9) 1 d DG . P A 2 H33A H 0.754513 0.028052 0.585899 0.063 Uiso 0.279(9) 1 calc R . P A 2 C34A C 0.567(2) -0.0038(12) 0.5850(9) 0.0525(12) Uani 0.279(9) 1 d DG . P A 2 H34A H 0.537823 -0.051135 0.538434 0.063 Uiso 0.279(9) 1 calc R . P A 2 C35A C 0.4812(15) 0.0182(14) 0.6250(11) 0.0525(12) Uani 0.279(9) 1 d DG . P A 2 H35A H 0.393255 -0.014050 0.605771 0.063 Uiso 0.279(9) 1 calc R . P A 2 C36A C 0.5240(18) 0.0875(15) 0.6931(12) 0.0525(12) Uani 0.279(9) 1 d DG . P A 2 H36A H 0.465324 0.102673 0.720383 0.063 Uiso 0.279(9) 1 calc R . P A 2 C31A C 0.653(2) 0.1347(13) 0.7213(10) 0.0525(12) Uani 0.279(9) 1 d DG . P A 2 C41 C 0.6087(6) 0.2076(4) 0.8769(4) 0.0406(16) Uani 1 1 d . . . . . C42 C 0.5226(8) 0.2514(5) 0.8776(4) 0.056(2) Uani 1 1 d . . . . . H42 H 0.521588 0.295229 0.843166 0.067 Uiso 1 1 calc R . . . . C43 C 0.4356(8) 0.2316(6) 0.9293(5) 0.070(2) Uani 1 1 d . . . . . H43 H 0.374762 0.260648 0.929111 0.084 Uiso 1 1 calc R . . . . C44 C 0.4404(10) 0.1702(7) 0.9793(5) 0.082(3) Uani 1 1 d . . . . . H44 H 0.382205 0.156882 1.014217 0.098 Uiso 1 1 calc R . . . . C45 C 0.5258(11) 0.1273(6) 0.9808(5) 0.080(3) Uani 1 1 d . . . . . H45 H 0.527880 0.085667 1.017002 0.096 Uiso 1 1 calc R . . . . C46 C 0.6103(8) 0.1445(5) 0.9293(4) 0.059(2) Uani 1 1 d . . . . . H46 H 0.669148 0.113627 0.929542 0.071 Uiso 1 1 calc R . . . . C51 C 0.8981(9) 0.7970(7) 0.5197(6) 0.0473(11) Uani 0.753(8) 1 d D . P B 1 C52 C 0.9594(9) 0.8671(6) 0.4781(5) 0.0473(11) Uani 0.753(8) 1 d D . P B 1 H52 H 1.045738 0.907462 0.496560 0.057 Uiso 0.753(8) 1 calc R . P B 1 C53 C 0.8985(8) 0.8796(7) 0.4109(5) 0.0473(11) Uani 0.753(8) 1 d D . P B 1 H53 H 0.941954 0.928986 0.383868 0.057 Uiso 0.753(8) 1 calc R . P B 1 C54 C 0.7736(8) 0.8202(6) 0.3826(5) 0.0473(11) Uani 0.753(8) 1 d D . P B 1 H54 H 0.730933 0.828395 0.335980 0.057 Uiso 0.753(8) 1 calc R . P B 1 C55 C 0.7108(9) 0.7485(7) 0.4227(5) 0.0473(11) Uani 0.753(8) 1 d D . P B 1 H55 H 0.624966 0.707637 0.403481 0.057 Uiso 0.753(8) 1 calc R . P B 1 C56 C 0.7728(8) 0.7362(7) 0.4906(5) 0.0473(11) Uani 0.753(8) 1 d D . P B 1 H56 H 0.729753 0.686332 0.517310 0.057 Uiso 0.753(8) 1 calc R . P B 1 C51A C 0.9360(19) 0.8107(17) 0.5279(11) 0.0473(11) Uani 0.247(8) 1 d D . P B 2 C52A C 1.0247(14) 0.8693(16) 0.4899(11) 0.0473(11) Uani 0.247(8) 1 d DG . P B 2 H52A H 1.112201 0.890085 0.510053 0.057 Uiso 0.247(8) 1 calc R . P B 2 C53A C 0.9855(17) 0.8976(14) 0.4223(11) 0.0473(11) Uani 0.247(8) 1 d DG . P B 2 H53A H 1.046153 0.937632 0.396332 0.057 Uiso 0.247(8) 1 calc R . P B 2 C54A C 0.8576(19) 0.8672(17) 0.3928(9) 0.0473(11) Uani 0.247(8) 1 d DG . P B 2 H54A H 0.830736 0.886459 0.346667 0.057 Uiso 0.247(8) 1 calc R . P B 2 C55A C 0.7688(14) 0.8085(17) 0.4309(11) 0.0473(11) Uani 0.247(8) 1 d DG . P B 2 H55A H 0.681366 0.787740 0.410723 0.057 Uiso 0.247(8) 1 calc R . P B 2 C56A C 0.8081(17) 0.7803(15) 0.4984(11) 0.0473(11) Uani 0.247(8) 1 d DG . P B 2 H56A H 0.747412 0.740192 0.524445 0.057 Uiso 0.247(8) 1 calc R . P B 2 C61 C 1.0312(7) 0.8848(4) 0.6821(4) 0.0411(16) Uani 1 1 d . . . . . C62 C 1.1549(8) 0.9352(5) 0.7200(4) 0.0524(19) Uani 1 1 d . . . . . H62 H 1.218842 0.913861 0.705988 0.063 Uiso 1 1 calc R . . . . C63 C 1.1869(9) 1.0164(6) 0.7782(5) 0.068(2) Uani 1 1 d . . . . . H63 H 1.271802 1.050319 0.804074 0.082 Uiso 1 1 calc R . . . . C64 C 1.0930(10) 1.0468(6) 0.7978(5) 0.072(3) Uani 1 1 d . . . . . H64 H 1.113963 1.102156 0.837445 0.086 Uiso 1 1 calc R . . . . C65 C 0.9698(9) 0.9985(6) 0.7609(5) 0.064(2) Uani 1 1 d . . . . . H65 H 0.906204 1.020364 0.774746 0.077 Uiso 1 1 calc R . . . . C66 C 0.9396(8) 0.9177(5) 0.7035(4) 0.0527(19) Uani 1 1 d . . . . . H66 H 0.854360 0.883898 0.678105 0.063 Uiso 1 1 calc R . . . . O1 O 0.9772(10) 0.5815(8) 0.8232(6) 0.0542(11) Uani 0.670(8) 1 d . . P C 1 C71 C 1.0985(10) 0.6606(9) 0.8191(6) 0.0542(11) Uani 0.670(8) 1 d . . P C 1 H71A H 1.090381 0.724632 0.824564 0.065 Uiso 0.670(8) 1 calc R . P C 1 H71B H 1.126568 0.648042 0.769200 0.065 Uiso 0.670(8) 1 calc R . P C 1 C72 C 1.1910(10) 0.6571(9) 0.8884(6) 0.0542(11) Uani 0.670(8) 1 d . . P C 1 H72A H 1.237720 0.616583 0.871235 0.065 Uiso 0.670(8) 1 calc R . P C 1 H72B H 1.252502 0.723521 0.911839 0.065 Uiso 0.670(8) 1 calc R . P C 1 C73 C 1.1157(11) 0.6155(9) 0.9432(6) 0.0542(11) Uani 0.670(8) 1 d . . P C 1 H73A H 1.115295 0.667732 0.983696 0.065 Uiso 0.670(8) 1 calc R . P C 1 H73B H 1.150872 0.573468 0.969045 0.065 Uiso 0.670(8) 1 calc R . P C 1 C74 C 0.9885(11) 0.5586(10) 0.9021(7) 0.0542(11) Uani 0.670(8) 1 d . . P C 1 H74A H 0.927036 0.574560 0.930078 0.065 Uiso 0.670(8) 1 calc R . P C 1 H74B H 0.970652 0.488271 0.898996 0.065 Uiso 0.670(8) 1 calc R . P C 1 O1A O 0.9857(18) 0.5965(13) 0.8294(11) 0.0542(11) Uani 0.330(8) 1 d . . P C 2 C71A C 1.0560(17) 0.6967(13) 0.8312(8) 0.0542(11) Uani 0.330(8) 1 d G . P C 2 H71C H 1.098362 0.704852 0.785357 0.065 Uiso 0.330(8) 1 calc R . P C 2 H71D H 0.999138 0.732901 0.829842 0.065 Uiso 0.330(8) 1 calc R . P C 2 C72A C 1.1470(15) 0.7331(11) 0.9009(9) 0.0542(11) Uani 0.330(8) 1 d G . P C 2 H72C H 1.233073 0.758629 0.888456 0.065 Uiso 0.330(8) 1 calc R . P C 2 H72D H 1.133850 0.786678 0.932942 0.065 Uiso 0.330(8) 1 calc R . P C 2 C73A C 1.1330(17) 0.6553(13) 0.9422(9) 0.0542(11) Uani 0.330(8) 1 d G . P C 2 H73C H 1.113144 0.671618 0.994086 0.065 Uiso 0.330(8) 1 calc R . P C 2 H73D H 1.212368 0.643569 0.949601 0.065 Uiso 0.330(8) 1 calc R . P C 2 C74A C 1.0333(18) 0.5709(11) 0.8980(12) 0.0542(11) Uani 0.330(8) 1 d G . P C 2 H74C H 1.064859 0.518680 0.884290 0.065 Uiso 0.330(8) 1 calc R . P C 2 H74D H 0.965635 0.546729 0.928776 0.065 Uiso 0.330(8) 1 calc R . P C 2 C81 C 1.0045(7) 0.4875(5) 0.5971(3) 0.0400(16) Uani 1 1 d . . . . . H81A H 1.040899 0.556869 0.592056 0.048 Uiso 1 1 calc R . . . . H81B H 0.930811 0.452809 0.554812 0.048 Uiso 1 1 calc R . . . . C82 C 1.1011(7) 0.4427(5) 0.5929(4) 0.0493(18) Uani 1 1 d . . . . . H82A H 1.187630 0.492806 0.609476 0.059 Uiso 1 1 calc R . . . . H82B H 1.092986 0.408461 0.539444 0.059 Uiso 1 1 calc R . . . . C83 C 1.0714(7) 0.3716(5) 0.6490(4) 0.0472(18) Uani 1 1 d . . . . . H83A H 0.997915 0.310902 0.625676 0.057 Uiso 1 1 calc R . . . . H83B H 1.144804 0.355346 0.666824 0.057 Uiso 1 1 calc R . . . . C84 C 1.0418(7) 0.4318(5) 0.7142(4) 0.0470(18) Uani 1 1 d . . . . . H84A H 0.992696 0.389845 0.747760 0.056 Uiso 1 1 calc R . . . . H84B H 1.120154 0.481157 0.746725 0.056 Uiso 1 1 calc R . . . . C91 C 0.6210(7) 0.4316(5) 0.5243(4) 0.0464(18) Uani 1 1 d . . . . . H91A H 0.673175 0.496518 0.514626 0.056 Uiso 1 1 calc R . . . . H91B H 0.539517 0.432681 0.535570 0.056 Uiso 1 1 calc R . . . . C92 C 0.6003(11) 0.3541(6) 0.4554(5) 0.087(3) Uani 1 1 d . . . . . H92A H 0.525815 0.346270 0.416928 0.104 Uiso 1 1 calc R . . . . H92B H 0.675140 0.369692 0.429794 0.104 Uiso 1 1 calc R . . . . C93 C 0.5790(7) 0.2648(5) 0.4895(4) 0.056(2) Uani 1 1 d . . . . . H93A H 0.604043 0.217920 0.457456 0.068 Uiso 1 1 calc R . . . . H93B H 0.489356 0.232832 0.494080 0.068 Uiso 1 1 calc R . . . . C94 C 0.6618(7) 0.3022(4) 0.5681(4) 0.0436(17) Uani 1 1 d . . . . . H94A H 0.619362 0.266689 0.607125 0.052 Uiso 1 1 calc R . . . . H94B H 0.742191 0.292790 0.566689 0.052 Uiso 1 1 calc R . . . . Nd1 Nd 0.78948(3) 0.51292(2) 0.71843(2) 0.02771(12) Uani 1 1 d . . . . . O2 O 0.9670(4) 0.4783(3) 0.6735(2) 0.0338(10) Uani 1 1 d . . . . . O3 O 0.6860(4) 0.4056(3) 0.5884(2) 0.0323(9) Uani 1 1 d . . . . . P2 P 0.71914(17) 0.22660(11) 0.80841(9) 0.0364(4) Uani 1 1 d . . . . . P3 P 0.99192(16) 0.77799(11) 0.60704(9) 0.0334(4) Uani 1 1 d . . . . . 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 B1 0.029(4) 0.037(4) 0.042(4) 0.009(3) 0.010(3) 0.015(3) B2 0.029(4) 0.051(5) 0.032(4) 0.008(3) 0.011(3) 0.021(4) C11 0.048(4) 0.039(4) 0.033(3) 0.009(3) 0.016(3) 0.020(3) C12 0.061(6) 0.045(4) 0.071(5) -0.007(4) -0.017(4) 0.027(4) C13 0.079(7) 0.064(6) 0.089(7) -0.007(5) -0.035(5) 0.042(5) C14 0.095(7) 0.048(5) 0.057(5) 0.021(4) 0.013(5) 0.036(5) C15 0.072(7) 0.040(5) 0.130(9) 0.029(5) 0.027(6) 0.013(4) C16 0.045(5) 0.045(5) 0.126(8) 0.018(5) 0.022(5) 0.014(4) C21 0.026(4) 0.043(4) 0.054(4) 0.022(3) 0.009(3) 0.020(3) C22 0.043(5) 0.062(5) 0.052(4) 0.024(4) 0.007(3) 0.012(4) C23 0.048(5) 0.082(6) 0.069(6) 0.044(5) 0.011(4) 0.007(4) C24 0.037(5) 0.099(7) 0.092(7) 0.071(6) 0.032(4) 0.029(5) C25 0.064(6) 0.090(7) 0.064(5) 0.042(5) 0.038(4) 0.035(5) C26 0.045(5) 0.071(5) 0.057(5) 0.023(4) 0.026(4) 0.027(4) P1 0.0278(9) 0.0365(9) 0.0373(9) 0.0110(7) 0.0096(7) 0.0134(7) B3 0.050(5) 0.030(4) 0.040(4) 0.014(3) 0.010(4) 0.016(4) B4 0.056(6) 0.062(6) 0.053(5) 0.016(4) 0.008(4) 0.032(5) B5 0.049(5) 0.031(4) 0.031(4) 0.013(3) 0.004(3) 0.018(3) B6 0.028(5) 0.060(6) 0.063(6) -0.012(4) 0.013(4) 0.005(4) C31 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C32 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C33 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C34 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C35 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C36 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C32A 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C33A 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C34A 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C35A 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C36A 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C31A 0.065(3) 0.045(2) 0.040(2) 0.0021(16) 0.012(2) 0.014(2) C41 0.044(4) 0.029(3) 0.039(4) 0.005(3) 0.003(3) 0.004(3) C42 0.066(6) 0.055(5) 0.051(4) 0.013(4) 0.017(4) 0.024(4) C43 0.068(6) 0.065(6) 0.087(6) 0.014(5) 0.033(5) 0.030(5) C44 0.101(8) 0.062(6) 0.074(6) 0.013(5) 0.041(6) 0.013(6) C45 0.127(9) 0.046(5) 0.061(5) 0.021(4) 0.036(6) 0.016(5) C46 0.085(6) 0.040(4) 0.051(4) 0.019(3) 0.020(4) 0.015(4) C51 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C52 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C53 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C54 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C55 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C56 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C51A 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C52A 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C53A 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C54A 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C55A 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C56A 0.054(3) 0.045(2) 0.043(2) 0.0169(18) 0.003(2) 0.019(2) C61 0.054(5) 0.029(3) 0.041(4) 0.012(3) 0.026(3) 0.009(3) C62 0.062(5) 0.043(4) 0.049(4) 0.000(3) 0.023(4) 0.015(4) C63 0.086(7) 0.047(5) 0.058(5) -0.005(4) 0.024(5) 0.011(5) C64 0.116(9) 0.043(5) 0.055(5) 0.002(4) 0.043(5) 0.022(5) C65 0.089(7) 0.047(5) 0.074(6) 0.015(4) 0.046(5) 0.035(5) C66 0.076(6) 0.039(4) 0.053(4) 0.012(3) 0.029(4) 0.026(4) O1 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C71 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C72 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C73 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C74 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) O1A 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C71A 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C72A 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C73A 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C74A 0.041(2) 0.078(3) 0.0385(18) 0.005(2) -0.0068(17) 0.023(2) C81 0.055(5) 0.039(4) 0.030(3) 0.013(3) 0.019(3) 0.017(3) C82 0.043(4) 0.062(5) 0.046(4) 0.003(3) 0.018(3) 0.024(4) C83 0.052(5) 0.059(5) 0.045(4) 0.003(3) 0.010(3) 0.040(4) C84 0.060(5) 0.058(4) 0.040(4) 0.014(3) 0.010(3) 0.040(4) C91 0.064(5) 0.038(4) 0.035(4) 0.006(3) -0.003(3) 0.020(4) C92 0.123(9) 0.068(6) 0.050(5) 0.005(4) -0.016(5) 0.026(6) C93 0.062(5) 0.042(4) 0.049(4) 0.000(3) 0.003(4) 0.005(4) C94 0.055(5) 0.025(3) 0.050(4) 0.007(3) 0.008(3) 0.014(3) Nd1 0.0302(2) 0.02922(18) 0.02563(17) 0.00868(12) 0.00679(13) 0.01180(14) O2 0.039(3) 0.045(2) 0.029(2) 0.0148(18) 0.0181(19) 0.023(2) O3 0.040(3) 0.033(2) 0.026(2) 0.0064(17) 0.0061(18) 0.0150(19) P2 0.0456(11) 0.0302(9) 0.0341(8) 0.0112(7) 0.0053(7) 0.0141(8) P3 0.0378(10) 0.0254(8) 0.0389(9) 0.0102(7) 0.0142(7) 0.0106(7) 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' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' 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 C12 C11 P1 120.8(5) . . ? C16 C11 C12 118.5(7) . . ? C16 C11 P1 120.7(6) . . ? C11 C12 C13 119.7(7) . . ? C14 C13 C12 121.2(8) . . ? C13 C14 C15 119.6(7) . . ? C14 C15 C16 119.8(8) . . ? C11 C16 C15 121.1(8) . . ? C22 C21 C26 118.2(6) . . ? C22 C21 P1 120.8(6) . . ? C26 C21 P1 120.9(5) . . ? C21 C22 C23 120.6(8) . . ? C24 C23 C22 120.3(8) . . ? C23 C24 C25 120.5(7) . . ? C24 C25 C26 119.2(8) . . ? C21 C26 C25 121.1(8) . . ? B1 P1 B2 107.5(3) . . ? C11 P1 B1 112.6(3) . . ? C11 P1 B2 109.3(3) . . ? C21 P1 B1 109.7(3) . . ? C21 P1 B2 110.8(3) . . ? C21 P1 C11 107.0(3) . . ? C32 C31 C36 119.5(9) . . ? C32 C31 P2 120.4(7) . . ? C36 C31 P2 120.0(7) . . ? C31 C32 C33 120.8(10) . . ? C32 C33 C34 119.3(10) . . ? C35 C34 C33 120.8(10) . . ? C34 C35 C36 119.4(10) . . ? C31 C36 C35 120.3(9) . . ? C31A C32A C33A 120.0 . . ? C34A C33A C32A 119.9 . . ? C35A C34A C33A 120.0 . . ? C36A C35A C34A 120.0 . . ? C35A C36A C31A 120.0 . . ? C32A C31A C36A 120.0 . . ? C32A C31A P2 116.1(12) . . ? C36A C31A P2 123.9(12) . . ? C42 C41 C46 118.9(7) . . ? C42 C41 P2 122.2(5) . . ? C46 C41 P2 118.8(6) . . ? C41 C42 C43 120.4(7) . . ? C44 C43 C42 118.8(8) . . ? C45 C44 C43 122.0(9) . . ? C44 C45 C46 119.8(8) . . ? C45 C46 C41 120.0(8) . . ? C52 C51 C56 118.6(8) . . ? C52 C51 P3 118.8(6) . . ? C56 C51 P3 122.2(6) . . ? C53 C52 C51 121.5(8) . . ? C52 C53 C54 119.8(8) . . ? C53 C54 C55 119.6(8) . . ? C56 C55 C54 120.4(8) . . ? C55 C56 C51 120.0(8) . . ? C52A C51A C56A 120.0 . . ? C52A C51A P3 116.6(12) . . ? C56A C51A P3 123.4(12) . . ? C53A C52A C51A 120.0 . . ? C52A C53A C54A 120.0 . . ? C55A C54A C53A 120.0 . . ? C54A C55A C56A 120.0 . . ? C55A C56A C51A 120.0 . . ? C62 C61 C66 118.3(6) . . ? C62 C61 P3 120.1(5) . . ? C66 C61 P3 121.6(6) . . ? C61 C62 C63 121.1(8) . . ? C64 C63 C62 118.8(9) . . ? C65 C64 C63 121.3(8) . . ? C64 C65 C66 119.2(8) . . ? C65 C66 C61 121.3(8) . . ? C71 O1 Nd1 125.1(7) . . ? C74 O1 C71 107.2(8) . . ? C74 O1 Nd1 127.6(8) . . ? O1 C71 C72 103.6(9) . . ? C73 C72 C71 106.1(9) . . ? C72 C73 C74 108.4(9) . . ? C73 C74 O1 108.4(9) . . ? C71A O1A Nd1 115.8(9) . . ? C74A O1A C71A 108.0 . . ? C74A O1A Nd1 135.4(9) . . ? C72A C71A O1A 108.0 . . ? C73A C72A C71A 108.0 . . ? C72A C73A C74A 108.0 . . ? O1A C74A C73A 108.0 . . ? O2 C81 C82 106.1(5) . . ? C81 C82 C83 103.8(5) . . ? C84 C83 C82 100.0(5) . . ? O2 C84 C83 104.0(5) . . ? O3 C91 C92 105.1(6) . . ? C93 C92 C91 103.8(6) . . ? C92 C93 C94 103.5(6) . . ? O3 C94 C93 107.5(5) . . ? O1 Nd1 O2 70.2(3) . . ? O1 Nd1 O3 147.6(3) . . ? O2 Nd1 O1A 72.5(6) . . ? O2 Nd1 O3 77.98(13) . . ? O3 Nd1 O1A 150.4(6) . . ? C81 O2 Nd1 126.3(4) . . ? C84 O2 C81 107.5(5) . . ? C84 O2 Nd1 125.7(3) . . ? C91 O3 C94 107.6(4) . . ? C91 O3 Nd1 125.3(3) . . ? C94 O3 Nd1 126.4(3) . . ? B3 P2 B4 114.6(4) . . ? C31 P2 B3 104.2(5) . . ? C31 P2 B4 113.2(5) . . ? C31A P2 B3 103.4(8) . . ? C31A P2 B4 105.9(8) . . ? C31A P2 C41 110.5(7) . . ? C41 P2 B3 108.4(3) . . ? C41 P2 B4 113.6(3) . . ? C41 P2 C31 101.9(4) . . ? B5 P3 B6 115.1(4) . . ? C51 P3 B5 107.6(3) . . ? C51 P3 B6 110.4(4) . . ? C51A P3 B5 118.8(7) . . ? C51A P3 B6 102.7(9) . . ? C51A P3 C61 102.9(9) . . ? C61 P3 B5 104.8(3) . . ? C61 P3 B6 112.0(4) . . ? C61 P3 C51 106.5(4) . . ? 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 B1 P1 1.923(7) . ? B2 P1 1.935(7) . ? C11 C12 1.375(10) . ? C11 C16 1.373(10) . ? C11 P1 1.820(6) . ? C12 C13 1.389(10) . ? C13 C14 1.355(11) . ? C14 C15 1.359(12) . ? C15 C16 1.387(11) . ? C21 C22 1.379(10) . ? C21 C26 1.387(10) . ? C21 P1 1.818(6) . ? C22 C23 1.402(10) . ? C23 C24 1.349(12) . ? C24 C25 1.384(12) . ? C25 C26 1.394(10) . ? B3 P2 1.921(7) . ? B4 P2 1.932(9) . ? B5 P3 1.891(7) . ? B6 P3 1.920(9) . ? C31 C32 1.386(8) . ? C31 C36 1.395(8) . ? C31 P2 1.837(10) . ? C32 C33 1.392(8) . ? C33 C34 1.393(8) . ? C34 C35 1.385(8) . ? C35 C36 1.399(8) . ? C32A C33A 1.3910 . ? C32A C31A 1.3900 . ? C33A C34A 1.3900 . ? C34A C35A 1.3898 . ? C35A C36A 1.3898 . ? C36A C31A 1.3901 . ? C31A P2 1.805(13) . ? C41 C42 1.375(10) . ? C41 C46 1.403(9) . ? C41 P2 1.831(7) . ? C42 C43 1.412(11) . ? C43 C44 1.361(12) . ? C44 C45 1.356(13) . ? C45 C46 1.388(12) . ? C51 C52 1.386(8) . ? C51 C56 1.393(8) . ? C51 P3 1.884(9) . ? C52 C53 1.371(8) . ? C53 C54 1.382(8) . ? C54 C55 1.388(8) . ? C55 C56 1.384(8) . ? C51A C52A 1.3900 . ? C51A C56A 1.3900 . ? C51A P3 1.666(12) . ? C52A C53A 1.3900 . ? C53A C54A 1.3900 . ? C54A C55A 1.3900 . ? C55A C56A 1.3900 . ? C61 C62 1.386(10) . ? C61 C66 1.387(10) . ? C61 P3 1.820(7) . ? C62 C63 1.391(10) . ? C63 C64 1.380(13) . ? C64 C65 1.373(12) . ? C65 C66 1.382(10) . ? O1 C71 1.490(15) . ? O1 C74 1.473(12) . ? O1 Nd1 2.473(9) . ? C71 C72 1.541(13) . ? C72 C73 1.427(16) . ? C73 C74 1.447(14) . ? O1A C71A 1.4200 . ? O1A C74A 1.4200 . ? O1A Nd1 2.607(12) . ? C71A C72A 1.4200 . ? C72A C73A 1.4200 . ? C73A C74A 1.4200 . ? C81 C82 1.498(9) . ? C81 O2 1.469(7) . ? C82 C83 1.518(9) . ? C83 C84 1.518(9) . ? C84 O2 1.467(7) . ? C91 C92 1.499(11) . ? C91 O3 1.452(7) . ? C92 C93 1.484(10) . ? C93 C94 1.497(9) . ? C94 O3 1.458(7) . ? Nd1 O2 2.479(4) . ? Nd1 O3 2.506(4) . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 0.000 222.7 48.0 ? 2 0.344 0.206 0.360 16.2 0.0 ? 3 0.656 0.794 0.640 16.2 0.0 ?