#------------------------------------------------------------------------------ #$Date: 2021-09-06 14:08:47 +0300 (Mon, 06 Sep 2021) $ #$Revision: 268752 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/79/7707957.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_7707957 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_issue 33 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 11472 _journal_page_last 11484 _journal_paper_doi 10.1039/d1dt01932e _journal_volume 50 _journal_year 2021 _chemical_formula_moiety 'C72 H96 B12 Nd2 P6' _chemical_formula_sum 'C72 H96 B12 Nd2 P6' _chemical_formula_weight 1565.50 _chemical_name_systematic Nd2(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 2019-08-31 _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 109.675(5) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 18.826(3) _cell_length_b 9.6646(17) _cell_length_c 23.904(4) _cell_measurement_reflns_used 3132 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 18.81 _cell_measurement_theta_min 2.293 _cell_volume 4095.3(12) _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 1.000 _diffrn_measured_fraction_theta_max 0.998 _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 0.1449 _diffrn_reflns_av_unetI/netI 0.1141 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 45311 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.313 _diffrn_reflns_theta_min 2.293 _exptl_absorpt_coefficient_mu 1.408 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6472 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0705 before and 0.0627 after correction. The Ratio of minimum to maximum transmission is 0.8683. The \l/2 correction factor is 0.00150. ; _exptl_crystal_colour 'pale blue' _exptl_crystal_density_diffrn 1.270 _exptl_crystal_description needle-like _exptl_crystal_F_000 1596 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.03 _refine_diff_density_max 0.775 _refine_diff_density_min -1.618 _refine_diff_density_rms 0.141 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 324 _refine_ls_number_reflns 8303 _refine_ls_number_restraints 195 _refine_ls_restrained_S_all 1.004 _refine_ls_R_factor_all 0.1427 _refine_ls_R_factor_gt 0.0679 _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^)+(0.0647P)^2^+13.5750P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1382 _refine_ls_wR_factor_ref 0.1726 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4614 _reflns_number_total 8303 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01932e2.cif _cod_data_source_block dal1923 _cod_depositor_comments 'Adding full bibliography for 7707952--7707958.cif.' _cod_database_code 7707957 _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 0.959 _shelx_estimated_absorpt_t_min 0.669 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All B(H,H,H) groups 2. Restrained distances C51-C52 = C52-C53 = C53-C54 = C54-C55 = C55-C56 = C56-C51 1.39 with sigma of 0.01 C31-C32 = C32-C33 = C33-C34 = C34-C35 = C35-C36 = C36-C31 1.39 with sigma of 0.01 C31A-C32A = C32A-C33A = C33A-C1 = C1-C35A = C35A-C36A = C36A-C31A 1.39 with sigma of 0.01 C61-C62 = C62-C63 = C63-C64 = C64-C65 = C65-C66 = C66-C61 1.39 with sigma of 0.01 C61A-C62A = C62A-C63A = C63A-C64A = C64A-C65A = C65A-C66A = C66A-C61A 1.39 with sigma of 0.01 C11-C12 \\sim C12-C13 \\sim C13-C14 \\sim C14-C15 \\sim C15-C16 \\sim C16-C11 with sigma of 0.02 C11A-C12A \\sim C12A-C13A \\sim C13A-C14A \\sim C14A-C15A \\sim C15A-C16A \\sim C16A-C11A with sigma of 0.02 C21-C22 \\sim C22-C23 \\sim C23-C24 \\sim C24-C25 \\sim C25-C26 \\sim C26-C21 with sigma of 0.02 C21A-C22A \\sim C22A-C23A \\sim C23A-C24A \\sim C24A-C25A \\sim C25A-C26A \\sim C26A-C21A with sigma of 0.02 C31-C32 \\sim C32-C33 \\sim C33-C34 \\sim C34-C35 \\sim C35-C36 \\sim C36-C31 with sigma of 0.02 P2-C31 \\sim C31-P2 with sigma of 0.02 P2-C31A \\sim C31A-P2 with sigma of 0.02 C31A-C32A \\sim C32A-C33A \\sim C33A-C1 \\sim C1-C35A \\sim C35A-C36A \\sim C36A-C31A with sigma of 0.02 C41-C42 \\sim C42-C43 \\sim C43-C44 \\sim C44-C45 \\sim C45-C46 \\sim C46-C41 with sigma of 0.02 C51-C52 \\sim C52-C53 \\sim C53-C54 \\sim C54-C55 \\sim C55-C56 \\sim C56-C51 with sigma of 0.02 C51A-C52A \\sim C52A-C53A \\sim C53A-C54A \\sim C54A-C55A \\sim C55A-C56A \\sim C56A-C51A with sigma of 0.02 P3-C51 \\sim C51-P3 with sigma of 0.02 P3-C51A \\sim C51A-P3 with sigma of 0.02 C61-C62 \\sim C62-C63 \\sim C63-C64 \\sim C64-C65 \\sim C65-C66 \\sim C66-C61 with sigma of 0.02 C61A-C62A \\sim C62A-C63A \\sim C63A-C64A \\sim C64A-C65A \\sim C65A-C66A \\sim C66A-C61A with sigma of 0.02 P3-C61 \\sim C61-P3 with sigma of 0.02 P3-C61A \\sim C61A-P3 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C11A) = Uanis(C12A) = Uanis(C13A) = Uanis(C14A) = Uanis(C15A) = Uanis(C16A) Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54) = Uanis(C55) = Uanis(C56) Uanis(C61A) = Uanis(C62A) = Uanis(C63A) = Uanis(C64A) = Uanis(C65A) = Uanis(C66A) Uanis(C31) = Uanis(C36) = Uanis(C35) = Uanis(C1) = Uanis(C34) = Uanis(C33A) = Uanis(C33) = Uanis(C32A) = Uanis(C32) = Uanis(C31A) = Uanis(C36A) = Uanis(C35A) Uanis(C31) = Uanis(C31A) = Uanis(C36) = Uanis(C36A) = Uanis(C32A) = Uanis(C32) = Uanis(C33) = Uanis(C33A) = Uanis(C34) = Uanis(C1) = Uanis(C35A) = Uanis(C35) Uanis(C21) = Uanis(C21A) = Uanis(C26A) = Uanis(C26) = Uanis(C22A) = Uanis(C25) = Uanis(C23A) = Uanis(C24) = Uanis(C23) = Uanis(C24A) = Uanis(C25A) = Uanis(C22) Uanis(C61A) = Uanis(C61) = Uanis(C62A) = Uanis(C62) = Uanis(C66A) = Uanis(C63) = Uanis(C65A) = Uanis(C64A) = Uanis(C63A) = Uanis(C64) = Uanis(C65) = Uanis(C66) Uanis(C51) = Uanis(C52) = Uanis(C56A) = Uanis(C56) = Uanis(C55A) = Uanis(C55) = Uanis(C54) = Uanis(C54A) = Uanis(C53A) = Uanis(C52A) = Uanis(C53) Uanis(C51A) = Uanis(C51) = Uanis(C52) = Uanis(C56A) = Uanis(C53) = Uanis(C55A) = Uanis(C54A) = Uanis(C54) = Uanis(C55) = Uanis(C53A) = Uanis(C52A) = Uanis(C56) 4. Others Sof(C11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)= Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=1-FVAR(1) Sof(C11)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14)=Sof(C15)= Sof(H15)=Sof(C16)=Sof(H16)=FVAR(1) Sof(C26A)=Sof(H26A)=Sof(C22A)=Sof(H22A)=Sof(C25A)=Sof(H25A)=Sof(C23A)= Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C21A)=1-FVAR(2) Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24)=Sof(C25)= Sof(H25)=Sof(C26)=Sof(H26)=FVAR(2) Sof(C31A)=Sof(C32A)=Sof(H32A)=Sof(C33A)=Sof(H33A)=Sof(C1)=Sof(H1)=Sof(C35A)= Sof(H35A)=Sof(C36A)=Sof(H36A)=1-FVAR(3) Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34)=Sof(C35)= Sof(H35)=Sof(C36)=Sof(H36)=FVAR(3) Sof(C53A)=Sof(H53A)=Sof(C52A)=Sof(H52A)=Sof(C51A)=Sof(C56A)=Sof(H56A)= Sof(C55A)=Sof(H55A)=Sof(C54A)=Sof(H54A)=1-FVAR(4) Sof(C51)=Sof(C52)=Sof(H52)=Sof(C53)=Sof(H53)=Sof(C54)=Sof(H54)=Sof(C55)= Sof(H55)=Sof(C56)=Sof(H56)=FVAR(4) Sof(C61A)=Sof(C62A)=Sof(H62A)=Sof(C63A)=Sof(H63A)=Sof(C64A)=Sof(H64A)= Sof(C65A)=Sof(H65A)=Sof(C66A)=Sof(H66A)=1-FVAR(5) Sof(C61)=Sof(C62)=Sof(H62)=Sof(C63)=Sof(H63)=Sof(C64)=Sof(H64)=Sof(C65)= Sof(H65)=Sof(C66)=Sof(H66)=FVAR(5) 5.a Free rotating group: C53A(C52A,C51A,C56A,C55A,C54A) 5.b Aromatic/amide H refined with riding coordinates: C43(H43), C46(H46), C45(H45), C44(H44), C42(H42), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C12A(H12A), C13A(H13A), C14A(H14A), C15A(H15A), C16A(H16A), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C26A(H26A), C22A(H22A), C25A(H25A), C23A(H23A), C24A(H24A), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), C32A(H32A), C33A(H33A), C1(H1), C35A(H35A), C36A(H36A), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C53A(H53A), C52A(H52A), C56A(H56A), C55A(H55A), C54A(H54A), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C62A(H62A), C63A(H63A), C64A(H64A), C65A(H65A), C66A(H66A) 5.c Idealised Me refined as rotating group: B1(H1A,H1B,H1C), B2(H2A,H2B,H2C), B3(H3A,H3B,H3C), B4(H4A,H4B,H4C), B6(H6A, H6B,H6C), B5(H5A,H5B,H5C) ; _shelx_res_file ; dal1923.res created by SHELXL-2014/7 TITL dal1923_a.res in P2(1)/c REM Old TITL Dal19_23 in P2(1)/c sample #19120 TVF_Nd(Ph-PDB) REM SHELXT solution in P2(1)/c REM R1 0.280, Rweak 0.018, Alpha 0.038, Orientation as input REM Formula found by SHELXT: C37 B4 O10 P3 Nd CELL 0.71073 18.826 9.6646 23.904 90 109.675 90 ZERR 2 0.003 0.0017 0.004 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H B Nd P UNIT 144 192 24 4 12 EQIV $1 1-X,2-Y,1-Z DFIX 1.39 0.01 C51 C52 C52 C53 C53 C54 C54 C55 C55 C56 C56 C51 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 C1 C1 C35A C35A C36A C36A C31A DFIX 1.39 0.01 C61 C62 C62 C63 C63 C64 C64 C65 C65 C66 C66 C61 DFIX 1.39 0.01 C61A C62A C62A C63A C63A C64A C64A C65A C65A C66A C66A C61A SADI C11 C12 C12 C13 C13 C14 C14 C15 C15 C16 C16 C11 SADI C11A C12A C12A C13A C13A C14A C14A C15A C15A C16A C16A C11A SADI C21 C22 C22 C23 C23 C24 C24 C25 C25 C26 C26 C21 SADI C21A C22A C22A C23A C23A C24A C24A C25A C25A C26A C26A C21A SADI C31 C32 C32 C33 C33 C34 C34 C35 C35 C36 C36 C31 SADI P2 C31 C31 P2 SADI P2 C31A C31A P2 SADI C31A C32A C32A C33A C33A C1 C1 C35A C35A C36A C36A C31A SADI C41 C42 C42 C43 C43 C44 C44 C45 C45 C46 C46 C41 SADI C51 C52 C52 C53 C53 C54 C54 C55 C55 C56 C56 C51 SADI C51A C52A C52A C53A C53A C54A C54A C55A C55A C56A C56A C51A SADI P3 C51 C51 P3 SADI P3 C51A C51A P3 SADI C61 C62 C62 C63 C63 C64 C64 C65 C65 C66 C66 C61 SADI C61A C62A C62A C63A C63A C64A C64A C65A C65A C66A C66A C61A SADI P3 C61 C61 P3 SADI P3 C61A C61A P3 EADP C11 C12 C13 C14 C15 C16 C11A C12A C13A C14A C15A C16A EADP C41 C42 C43 C44 C45 C46 EADP C51 C52 C53 C54 C55 C56 EADP C61A C62A C63A C64A C65A C66A EADP C31 C36 C35 C1 C34 C33A C33 C32A C32 C31A C36A C35A EADP C31 C31A C36 C36A C32A C32 C33 C33A C34 C1 C35A C35 EADP C21 C21A C26A C26 C22A C25 C23A C24 C23 C24A C25A C22 EADP C61A C61 C62A C62 C66A C63 C65A C64A C63A C64 C65 C66 EADP C51 C52 C56A C56 C55A C55 C54 C54A C53A C52A C53 EADP C51A C51 C52 C56A C53 C55A C54A C54 C55 C53A C52A C56 L.S. 15 0 0 PLAN 20 SIZE 0.03 0.03 0.31 TEMP -123 FREE B1 Nd1 FREE B2 Nd1 FREE B3 Nd1 FREE B4 Nd1 FREE B6 Nd1_$1 FREE B5 Nd1 BOND $H list 4 fmap 2 53 acta OMIT -1 0 2 OMIT 0 0 2 OMIT 1 0 0 REM REM REM WGHT 0.064700 13.575000 FVAR 0.24944 0.51592 0.53883 0.49367 0.63247 0.78948 B1 3 0.210085 0.742871 0.427303 11.00000 0.03638 0.03110 = 0.14233 -0.01551 0.03113 -0.00580 AFIX 137 1.2000 H1A 2 0.276775 0.730785 0.437892 11.00000 -1.50000 H1B 2 0.187423 0.840659 0.395321 11.00000 -1.50000 H1C 2 0.178592 0.640122 0.403172 11.00000 -1.50000 AFIX 0 B2 3 0.247697 0.930948 0.538391 11.00000 0.03940 0.03214 = 0.09070 0.01688 0.01860 -0.00622 AFIX 137 1.2000 H2A 2 0.242211 0.946441 0.586579 11.00000 -1.50000 H2B 2 0.223894 1.031605 0.508576 11.00000 -1.50000 H2C 2 0.312762 0.914343 0.543523 11.00000 -1.50000 AFIX 0 B3 3 0.187108 1.195738 0.389330 11.00000 0.03185 0.03472 = 0.06036 -0.01033 -0.00959 0.00774 AFIX 137 1.2000 H3A 2 0.245755 1.235113 0.424251 11.00000 -1.50000 H3B 2 0.172154 1.083834 0.404079 11.00000 -1.50000 H3C 2 0.137944 1.275897 0.388152 11.00000 -1.50000 AFIX 0 B4 3 0.279205 1.057191 0.319442 11.00000 0.03821 0.03899 = 0.05283 -0.00187 -0.00615 0.00294 AFIX 137 1.2000 H4A 2 0.290607 1.050063 0.273065 11.00000 -1.50000 H4B 2 0.263581 0.944567 0.332978 11.00000 -1.50000 H4C 2 0.334828 1.099023 0.357270 11.00000 -1.50000 AFIX 0 B6 3 0.599040 0.846738 0.477741 11.00000 0.02202 0.02978 = 0.03626 0.00193 -0.00148 0.00052 AFIX 137 1.2000 H6A 2 0.653136 0.798787 0.468956 11.00000 -1.50000 H6B 2 0.600437 0.815788 0.526718 11.00000 -1.50000 H6C 2 0.599947 0.970410 0.473557 11.00000 -1.50000 AFIX 0 B5 3 0.420557 0.851375 0.429606 11.00000 0.02345 0.01764 = 0.05976 0.00461 0.00892 0.00071 AFIX 137 1.2000 H5A 2 0.425730 0.975111 0.432627 11.00000 -1.50000 H5B 2 0.413155 0.807085 0.474220 11.00000 -1.50000 H5C 2 0.366779 0.819662 0.387681 11.00000 -1.50000 AFIX 0 C43 1 0.432506 0.378007 0.396733 11.00000 0.03561 0.02896 = 0.07386 0.01655 0.02297 0.00367 AFIX 43 H43 2 0.384833 0.333280 0.385693 11.00000 -1.20000 AFIX 0 C46 1 0.570772 0.510876 0.432280 11.00000 0.03561 0.02896 = 0.07386 0.01655 0.02297 0.00367 AFIX 43 H46 2 0.618443 0.555783 0.445105 11.00000 -1.20000 AFIX 0 C45 1 0.567071 0.368102 0.427331 11.00000 0.03561 0.02896 = 0.07386 0.01655 0.02297 0.00367 AFIX 43 H45 2 0.612154 0.315195 0.437256 11.00000 -1.20000 AFIX 0 C44 1 0.497033 0.301852 0.407740 11.00000 0.03561 0.02896 = 0.07386 0.01655 0.02297 0.00367 AFIX 43 H44 2 0.494235 0.204442 0.402093 11.00000 -1.20000 AFIX 0 C42 1 0.437129 0.520429 0.401780 11.00000 0.03561 0.02896 = 0.07386 0.01655 0.02297 0.00367 AFIX 43 H42 2 0.392115 0.573032 0.393417 11.00000 -1.20000 AFIX 0 C41 1 0.505768 0.587948 0.418717 11.00000 0.03561 0.02896 = 0.07386 0.01655 0.02297 0.00367 ND1 4 0.303454 0.987772 0.441609 11.00000 0.01728 0.02302 = 0.05529 0.00168 -0.00253 -0.00102 P1 5 0.189944 0.770260 0.500448 11.00000 0.02481 0.02812 = 0.14937 0.00132 0.03779 -0.00273 P2 5 0.509444 0.775616 0.420542 11.00000 0.01845 0.02208 = 0.04099 0.00484 0.00259 -0.00309 P3 5 0.195902 1.183472 0.311360 11.00000 0.03401 0.02807 = 0.06310 -0.00664 -0.01718 0.00278 PART 1 C11 1 0.211122 0.613173 0.531029 21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 C12 1 0.205740 0.484242 0.504115 21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H12 2 0.191734 0.478654 0.462106 21.00000 -1.20000 AFIX 0 C13 1 0.220397 0.364120 0.537372 21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H13 2 0.214071 0.277076 0.517836 21.00000 -1.20000 AFIX 0 C14 1 0.244397 0.369007 0.599349 21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H14 2 0.252357 0.286169 0.622024 21.00000 -1.20000 AFIX 0 C15 1 0.256309 0.496135 0.626983 21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H15 2 0.277509 0.502561 0.669013 21.00000 -1.20000 AFIX 0 C16 1 0.236662 0.615777 0.592117 21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H16 2 0.241181 0.702722 0.611551 21.00000 -1.20000 AFIX 0 PART 0 PART 2 C11A 1 0.228529 0.628063 0.562803 -21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 C12A 1 0.212507 0.488972 0.544106 -21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H12A 2 0.180975 0.470386 0.504501 -21.00000 -1.20000 AFIX 0 C13A 1 0.242445 0.377098 0.583136 -21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H13A 2 0.238390 0.284702 0.568836 -21.00000 -1.20000 AFIX 0 C14A 1 0.278419 0.406845 0.643792 -21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H14A 2 0.292306 0.332942 0.671570 -21.00000 -1.20000 AFIX 0 C15A 1 0.294280 0.544458 0.664175 -21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H15A 2 0.320809 0.563202 0.704899 -21.00000 -1.20000 AFIX 0 C16A 1 0.270166 0.652421 0.623238 -21.00000 0.04516 0.04435 = 0.06413 0.01883 0.02048 -0.00713 AFIX 43 H16A 2 0.282141 0.744954 0.636460 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C21 1 0.095594 0.786667 0.503364 31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 C22 1 0.072223 0.823262 0.550693 31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H22 2 0.110185 0.840459 0.587936 31.00000 -1.20000 AFIX 0 C23 1 -0.001877 0.836445 0.547608 31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H23 2 -0.014451 0.861015 0.581608 31.00000 -1.20000 AFIX 0 C24 1 -0.056258 0.813170 0.494413 31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H24 2 -0.107622 0.827990 0.490416 31.00000 -1.20000 AFIX 0 C25 1 -0.038158 0.767863 0.445449 31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H25 2 -0.076475 0.742820 0.409415 31.00000 -1.20000 AFIX 0 C26 1 0.038358 0.760415 0.451052 31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H26 2 0.051102 0.736105 0.417101 31.00000 -1.20000 AFIX 0 PART 0 PART 2 C26A 1 0.048372 0.892115 0.432224 -31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H26A 2 0.076081 0.943010 0.412483 -31.00000 -1.20000 AFIX 0 C22A 1 0.045219 0.716610 0.499798 -31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H22A 2 0.068446 0.639101 0.523298 -31.00000 -1.20000 AFIX 0 C25A 1 -0.028389 0.915508 0.415906 -31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H25A 2 -0.054614 0.974229 0.383702 -31.00000 -1.20000 AFIX 0 C23A 1 -0.030602 0.745127 0.490435 -31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H23A 2 -0.058036 0.696541 0.511083 -31.00000 -1.20000 AFIX 0 C24A 1 -0.063985 0.848085 0.449425 -31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 AFIX 43 H24A 2 -0.114564 0.873249 0.444320 -31.00000 -1.20000 AFIX 0 C21A 1 0.086890 0.799296 0.475435 -31.00000 0.03014 0.08140 = 0.09759 0.01066 0.02529 0.00894 PART 0 PART 1 C31 1 0.508337 0.829214 0.351234 41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 C32 1 0.546753 0.751455 0.322333 41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H32 2 0.571233 0.668118 0.339529 41.00000 -1.20000 AFIX 0 C33 1 0.549294 0.796310 0.267719 41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H33 2 0.570634 0.738418 0.245428 41.00000 -1.20000 AFIX 0 C34 1 0.520794 0.925283 0.245621 41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H34 2 0.528290 0.960624 0.210942 41.00000 -1.20000 AFIX 0 C35 1 0.481310 1.002246 0.274467 41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H35 2 0.458629 1.087572 0.258137 41.00000 -1.20000 AFIX 0 C36 1 0.475149 0.953804 0.327339 41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H36 2 0.448134 1.006108 0.347211 41.00000 -1.20000 AFIX 0 PART 0 PART 2 C31A 1 0.511011 0.824273 0.343375 -41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 C32A 1 0.573562 0.884513 0.334676 -41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H32A 2 0.618179 0.898357 0.367799 -41.00000 -1.20000 AFIX 0 C33A 1 0.572121 0.924785 0.278621 -41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H33A 2 0.615852 0.962204 0.272929 -41.00000 -1.20000 AFIX 0 C1 1 0.505317 0.909341 0.230781 -41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H1 2 0.502188 0.948291 0.193536 -41.00000 -1.20000 AFIX 0 C35A 1 0.443366 0.839471 0.235429 -41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H35A 2 0.400543 0.818374 0.201755 -41.00000 -1.20000 AFIX 0 C36A 1 0.448120 0.802202 0.292881 -41.00000 0.04752 0.04473 = 0.03068 0.00386 0.01174 -0.00429 AFIX 43 H36A 2 0.405476 0.758671 0.297994 -41.00000 -1.20000 AFIX 0 PART 0 PART 1 C51 1 0.208191 1.349211 0.287832 51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 C52 1 0.228707 1.461851 0.325683 51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H52 2 0.234019 1.451442 0.366413 51.00000 -1.20000 AFIX 0 C53 1 0.241550 1.589694 0.304571 51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H53 2 0.256571 1.665574 0.331230 51.00000 -1.20000 AFIX 0 C54 1 0.232825 1.608326 0.245353 51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H54 2 0.241303 1.695901 0.230682 51.00000 -1.20000 AFIX 0 C55 1 0.211307 1.494971 0.208167 51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H55 2 0.206040 1.505271 0.167441 51.00000 -1.20000 AFIX 0 C56 1 0.197189 1.367150 0.228202 51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H56 2 0.180083 1.292392 0.201195 51.00000 -1.20000 AFIX 6 PART 0 PART 2 C53A 1 0.278972 1.485021 0.216711 -51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H53A 2 0.309046 1.488861 0.191828 -51.00000 -1.20000 AFIX 5 C52A 1 0.264521 1.358510 0.238371 -51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H52A 2 0.284713 1.275856 0.228282 -51.00000 -1.20000 AFIX 5 C51A 1 0.220520 1.352901 0.274800 -51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 C56A 1 0.190960 1.473821 0.289520 -51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H56A 2 0.160903 1.470005 0.314417 -51.00000 -1.20000 AFIX 5 C55A 1 0.205351 1.600371 0.267830 -51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H55A 2 0.185080 1.683006 0.277858 -51.00000 -1.20000 AFIX 5 C54A 1 0.249392 1.605941 0.231481 -51.00000 0.05821 0.03873 = 0.05892 0.00569 0.01329 -0.00293 AFIX 43 H54A 2 0.259298 1.692430 0.216710 -51.00000 -1.20000 AFIX 0 PART 0 PART 1 C61 1 0.109440 1.117005 0.258069 61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 C62 1 0.112459 1.018088 0.217260 61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H62 2 0.160036 0.980984 0.219410 61.00000 -1.20000 AFIX 0 C63 1 0.048060 0.971327 0.173227 61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H63 2 0.051964 0.906288 0.144604 61.00000 -1.20000 AFIX 0 C64 1 -0.021809 1.019785 0.171185 61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H64 2 -0.066088 0.994122 0.139607 61.00000 -1.20000 AFIX 0 C65 1 -0.026011 1.106278 0.215961 61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H65 2 -0.074076 1.132503 0.217234 61.00000 -1.20000 AFIX 0 C66 1 0.038782 1.155802 0.259266 61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H66 2 0.034772 1.215862 0.289523 61.00000 -1.20000 AFIX 0 PART 0 PART 2 C61A 1 0.115385 1.116817 0.250414 -61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 C62A 1 0.093788 1.157062 0.191172 -61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H62A 2 0.124656 1.220860 0.179606 -61.00000 -1.20000 AFIX 0 C63A 1 0.028891 1.107695 0.148248 -61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H63A 2 0.005260 1.152728 0.111308 -61.00000 -1.20000 AFIX 0 C64A 1 0.002002 0.986171 0.164643 -61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H64A 2 -0.033769 0.935689 0.133730 -61.00000 -1.20000 AFIX 0 C65A 1 0.021690 0.930259 0.221349 -61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H65A 2 -0.001821 0.850621 0.230566 -61.00000 -1.20000 AFIX 0 C66A 1 0.079163 1.002310 0.263257 -61.00000 0.04080 0.06285 = 0.08256 -0.01535 -0.01650 -0.00318 AFIX 43 H66A 2 0.094661 0.971195 0.303270 -61.00000 -1.20000 AFIX 0 HKLF 4 REM dal1923_a.res in P2(1)/c REM R1 = 0.0679 for 4614 Fo > 4sig(Fo) and 0.1427 for all 8303 data REM 324 parameters refined using 195 restraints END WGHT 0.0645 13.6851 REM Highest difference peak 0.775, deepest hole -1.618, 1-sigma level 0.141 Q1 1 -0.0175 1.1605 0.1809 11.00000 0.05 0.68 Q2 1 0.0606 1.2112 0.2346 11.00000 0.05 0.61 Q3 1 -0.0345 0.6992 0.4593 11.00000 0.05 0.60 Q4 1 0.4594 0.9173 0.2351 11.00000 0.05 0.59 Q5 1 0.4531 0.3186 0.3982 11.00000 0.05 0.56 Q6 1 0.2953 1.0603 0.5022 11.00000 0.05 0.54 Q7 1 -0.0142 0.9458 0.4551 11.00000 0.05 0.53 Q8 1 0.0770 0.8027 0.4596 11.00000 0.05 0.53 Q9 1 0.2986 0.4841 0.6370 11.00000 0.05 0.53 Q10 1 0.2159 0.5077 0.6242 11.00000 0.05 0.53 Q11 1 0.2810 1.1403 0.4527 11.00000 0.05 0.50 Q12 1 0.1580 1.6054 0.2583 11.00000 0.05 0.49 Q13 1 0.2436 1.5965 0.2776 11.00000 0.05 0.49 Q14 1 0.5395 0.3108 0.4168 11.00000 0.05 0.48 Q15 1 0.5865 0.8510 0.2788 11.00000 0.05 0.48 Q16 1 -0.0464 0.9392 0.3596 11.00000 0.05 0.47 Q17 1 0.1767 0.9159 0.4992 11.00000 0.05 0.47 Q18 1 0.2824 1.0275 0.5052 11.00000 0.05 0.47 Q19 1 0.6432 0.8972 0.5282 11.00000 0.05 0.46 Q20 1 0.2570 0.9842 0.3769 11.00000 0.05 0.46 ; _shelx_res_checksum 15459 _shelx_hkl_file ; -1 0 0 -1.30 0.90 -1 0 0 -1.80 2.00 1 0 0 -3.40 1.40 1 0 0 0.90 1.80 -2 0 0 469.05 17.90 -3 0 0 429.16 21.80 -3 0 0 460.65 17.70 3 0 0 469.65 17.80 3 0 0 432.26 20.00 4 0 0 9798.82 198.88 4 0 0 9999.00 192.08 -4 0 0 9934.41 192.28 -4 0 0 9353.66 198.58 5 0 0 216.78 19.30 5 0 0 219.98 24.60 -5 0 0 177.88 23.20 -5 0 0 204.68 24.90 -5 0 0 213.08 19.30 6 0 0 -2.30 15.90 -6 0 0 43.30 14.10 -6 0 0 22.90 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-25.50 35.30 -7 -1 28 33.60 46.00 -7 1 28 -28.50 37.20 -6 -1 28 43.80 44.50 -6 -1 28 22.90 38.40 -6 1 28 -3.10 37.10 -5 -1 28 -17.80 42.10 -5 -1 28 -32.10 40.60 5 -1 -28 6.30 37.00 -5 1 28 36.10 39.30 4 -1 -28 -34.10 37.70 -4 -1 28 -36.70 44.80 -4 -1 28 10.80 39.50 -4 1 28 29.70 39.70 4 1 -28 4.20 43.40 -3 -1 28 90.29 49.30 3 -1 -28 -0.40 45.90 -3 -1 28 65.49 47.40 3 1 -28 -13.20 42.80 -3 1 28 -37.90 38.70 -2 -1 28 -40.70 37.20 2 -1 -28 -46.40 37.20 -2 -1 28 -22.50 39.80 -2 1 28 3.70 41.50 2 1 -28 10.60 44.10 -1 -1 28 20.40 40.50 -1 -1 28 11.50 39.60 1 -1 -28 -8.80 43.30 1 1 -28 -22.60 38.70 -1 1 28 -4.50 39.90 -14 -2 28 20.70 46.40 14 -2 -28 62.29 52.59 14 2 -28 -15.00 39.50 -14 2 28 94.09 49.10 13 -2 -28 52.99 44.00 -13 -2 28 2.50 38.90 -13 -2 28 9.10 43.50 -13 2 28 -5.20 45.50 -13 2 28 84.79 53.49 13 2 -28 2.60 37.80 -12 -2 28 -6.40 41.60 -12 -2 28 74.29 46.30 12 -2 -28 15.80 43.00 -12 2 28 -17.40 37.70 -12 2 28 9.70 46.80 -11 -2 28 -25.10 42.50 -11 -2 28 61.09 43.40 11 -2 -28 35.20 41.20 -11 2 28 -5.70 41.90 -11 2 28 -2.40 41.90 10 -2 -28 11.00 36.10 -10 -2 28 64.39 47.30 -10 -2 28 -58.89 35.30 -10 2 28 98.69 49.00 -10 2 28 64.49 53.49 -9 -2 28 53.29 44.80 -9 -2 28 13.40 40.00 -9 2 28 -19.90 41.20 -9 2 28 129.69 51.69 -8 -2 28 3.30 43.40 -8 -2 28 21.60 40.20 -8 2 28 83.09 49.60 -8 2 28 80.19 48.60 -7 -2 28 2.50 41.20 -7 -2 28 -20.80 38.70 -7 2 28 11.20 45.80 -7 2 28 57.59 42.90 -6 -2 28 -8.30 44.20 -6 -2 28 58.59 48.30 6 -2 -28 38.90 60.49 -6 2 28 21.40 42.50 -6 2 28 103.49 50.19 -5 -2 28 -16.10 36.70 -5 -2 28 10.50 38.50 5 -2 -28 -45.50 41.50 -5 2 28 26.20 46.40 -4 -2 28 -45.20 36.80 -4 -2 28 84.79 50.29 4 -2 -28 -69.39 32.40 -4 2 28 -12.40 37.40 4 2 -28 -0.90 44.70 3 -2 -28 95.09 51.79 -3 -2 28 35.60 47.20 -3 -2 28 53.39 48.10 -3 2 28 18.90 38.10 3 2 -28 21.60 46.50 -2 -2 28 -13.40 41.70 2 -2 -28 38.10 46.20 -2 -2 28 -5.90 43.60 2 2 -28 -16.60 41.40 -2 2 28 16.20 40.80 -1 -2 28 117.09 54.99 -1 -2 28 23.70 44.80 1 -2 -28 41.30 44.40 1 2 -28 94.09 54.69 -12 -3 28 -29.10 39.70 -12 -3 28 -13.90 39.60 12 -3 -28 17.10 44.50 -12 3 28 16.50 49.60 -12 3 28 88.89 52.59 -11 -3 28 -45.70 37.60 11 -3 -28 53.99 50.19 -11 -3 28 80.59 49.00 -11 3 28 -85.79 41.20 -11 3 28 8.10 44.00 -10 -3 28 16.40 43.40 -10 -3 28 -59.79 39.70 10 -3 -28 36.50 62.59 -10 3 28 130.09 57.59 -10 3 28 -4.30 50.59 -9 -3 28 27.60 45.10 -9 -3 28 50.59 46.60 -9 3 28 7.70 41.40 -9 3 28 1.50 43.50 -8 -3 28 -1.50 46.70 -8 -3 28 3.70 42.70 -8 3 28 -3.60 41.10 -8 3 28 -34.60 41.70 -7 -3 28 49.90 45.20 -7 -3 28 13.60 44.70 -7 3 28 12.70 40.40 -7 3 28 11.60 46.30 -6 -3 28 -14.40 48.20 -6 -3 28 -26.50 39.20 6 -3 -28 10.00 45.40 -6 3 28 -9.00 41.50 -6 3 28 0.40 38.20 5 -3 -28 81.29 51.19 -5 -3 28 -14.70 37.90 -5 -3 28 -9.80 45.90 -5 3 28 -43.20 37.80 -4 -3 28 20.40 42.40 -4 -3 28 15.60 43.30 4 -3 -28 2.20 43.10 -4 3 28 29.90 43.20 -3 -3 28 -13.30 41.50 -3 -3 28 10.40 41.10 3 -3 -28 20.00 45.10 -3 3 28 89.79 49.80 3 3 -28 -57.69 40.10 -9 -4 28 40.80 47.90 -9 4 28 29.70 47.20 -8 -4 28 5.50 50.49 -8 -4 28 3.60 40.60 -8 4 28 38.90 41.50 -8 4 28 -32.80 40.20 -7 -4 28 -19.20 41.30 -7 -4 28 -42.10 39.20 -7 4 28 -26.80 47.40 -7 4 28 38.70 45.60 -6 -4 28 -17.80 39.90 -6 -4 28 -37.90 41.20 -6 4 28 32.40 49.80 -12 0 29 -17.60 44.50 12 0 -29 22.30 46.10 11 0 -29 -36.30 41.00 -11 0 29 71.59 50.59 10 0 -29 15.40 41.50 -10 0 29 -62.39 35.90 -9 0 29 -18.50 39.50 -8 0 29 18.80 45.40 -7 0 29 5.30 42.50 -6 0 29 -76.99 31.60 -5 0 29 60.69 49.10 -4 0 29 72.69 48.70 4 0 -29 -10.10 38.90 -3 0 29 -7.50 47.40 3 0 -29 1.70 40.50 12 -1 -29 28.40 41.20 -12 1 29 -63.89 36.40 -12 1 29 36.10 45.50 12 1 -29 27.40 43.10 -11 -1 29 -20.80 41.70 11 -1 -29 45.20 46.10 11 1 -29 35.90 41.80 -11 1 29 -14.40 39.20 -11 1 29 -63.79 41.40 -10 -1 29 18.50 50.19 10 -1 -29 0.20 42.80 10 1 -29 -0.70 40.00 -10 1 29 -30.60 45.50 -9 -1 29 -19.10 41.80 -9 1 29 6.50 40.90 -8 -1 29 52.89 48.00 -8 1 29 -35.00 38.20 -7 -1 29 -0.30 38.60 -7 -1 29 -28.20 48.50 -7 1 29 -82.09 39.40 -6 -1 29 21.90 45.30 -6 -1 29 -0.90 42.70 -6 1 29 71.19 49.20 -5 -1 29 -21.90 41.20 -5 -1 29 -2.30 45.40 5 -1 -29 40.80 48.80 -5 1 29 -13.90 44.50 -4 -1 29 82.99 47.00 4 -1 -29 -47.20 39.70 -4 -1 29 -43.40 36.60 4 1 -29 7.50 42.40 -4 1 29 55.59 48.90 -3 -1 29 -81.29 33.00 11 -2 -29 33.30 41.90 -11 -2 29 -64.39 31.90 -11 2 29 -78.99 37.50 -11 2 29 -22.80 44.60 -10 -2 29 34.70 49.00 -10 -2 29 -11.10 40.50 -10 2 29 51.69 48.40 -10 2 29 -25.50 45.10 -9 -2 29 21.60 41.50 -9 -2 29 7.60 49.60 -9 2 29 1.50 43.60 -9 2 29 49.60 45.50 -8 -2 29 52.19 45.20 -8 -2 29 -82.39 36.70 -8 2 29 29.80 42.80 -8 2 29 63.29 54.29 -7 -2 29 -12.50 44.60 -7 -2 29 12.90 47.40 -7 2 29 -33.60 41.80 -7 2 29 37.70 44.70 -6 -2 29 51.99 46.40 -6 -2 29 -23.80 38.90 -6 2 29 -4.60 41.00 -5 -2 29 -26.20 40.40 -5 -2 29 -12.80 41.90 5 -2 -29 -9.00 38.80 -5 2 29 29.10 50.69 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 5474 _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 B1 B 0.2101(6) 0.7429(11) 0.4273(6) 0.070(4) Uani 1 1 d . . . . . H1A H 0.2768 0.7308 0.4379 0.105 Uiso 1 1 calc GR . . . . H1B H 0.1874 0.8407 0.3953 0.105 Uiso 1 1 calc GR . . . . H1C H 0.1786 0.6401 0.4032 0.105 Uiso 1 1 calc GR . . . . B2 B 0.2477(6) 0.9309(11) 0.5384(6) 0.055(3) Uani 1 1 d . . . . . H2A H 0.2422 0.9464 0.5866 0.082 Uiso 1 1 calc GR . . . . H2B H 0.2239 1.0316 0.5086 0.082 Uiso 1 1 calc GR . . . . H2C H 0.3128 0.9143 0.5435 0.082 Uiso 1 1 calc GR . . . . B3 B 0.1871(5) 1.1957(10) 0.3893(5) 0.049(3) Uani 1 1 d . . . . . H3A H 0.2458 1.2351 0.4243 0.073 Uiso 1 1 calc GR . . . . H3B H 0.1722 1.0838 0.4041 0.073 Uiso 1 1 calc GR . . . . H3C H 0.1379 1.2759 0.3882 0.073 Uiso 1 1 calc GR . . . . B4 B 0.2792(6) 1.0572(11) 0.3194(5) 0.049(3) Uani 1 1 d . . . . . H4A H 0.2906 1.0501 0.2731 0.073 Uiso 1 1 calc GR . . . . H4B H 0.2636 0.9446 0.3330 0.073 Uiso 1 1 calc GR . . . . H4C H 0.3348 1.0990 0.3573 0.073 Uiso 1 1 calc GR . . . . B6 B 0.5990(5) 0.8467(9) 0.4777(4) 0.032(2) Uani 1 1 d . . . . . H6A H 0.6531 0.7988 0.4690 0.048 Uiso 1 1 calc GR . . . . H6B H 0.6004 0.8158 0.5267 0.048 Uiso 1 1 calc GR . . . . H6C H 0.5999 0.9704 0.4736 0.048 Uiso 1 1 calc GR . . . . B5 B 0.4206(5) 0.8514(9) 0.4296(5) 0.035(2) Uani 1 1 d . . . . . H5A H 0.4257 0.9751 0.4326 0.052 Uiso 1 1 calc GR . . . . H5B H 0.4132 0.8071 0.4742 0.052 Uiso 1 1 calc GR . . . . H5C H 0.3668 0.8197 0.3877 0.052 Uiso 1 1 calc GR . . . . C43 C 0.4325(5) 0.3780(7) 0.3967(4) 0.0450(9) Uani 1 1 d D . . . . H43 H 0.3848 0.3333 0.3857 0.054 Uiso 1 1 calc R . . . . C46 C 0.5708(4) 0.5109(7) 0.4323(4) 0.0450(9) Uani 1 1 d D . . . . H46 H 0.6184 0.5558 0.4451 0.054 Uiso 1 1 calc R . . . . C45 C 0.5671(4) 0.3681(7) 0.4273(4) 0.0450(9) Uani 1 1 d D . . . . H45 H 0.6122 0.3152 0.4373 0.054 Uiso 1 1 calc R . . . . C44 C 0.4970(4) 0.3019(8) 0.4077(4) 0.0450(9) Uani 1 1 d D . . . . H44 H 0.4942 0.2044 0.4021 0.054 Uiso 1 1 calc R . . . . C42 C 0.4371(4) 0.5204(7) 0.4018(4) 0.0450(9) Uani 1 1 d D . . . . H42 H 0.3921 0.5730 0.3934 0.054 Uiso 1 1 calc R . . . . C41 C 0.5058(4) 0.5879(8) 0.4187(4) 0.0450(9) Uani 1 1 d D . . . . Nd1 Nd 0.30345(2) 0.98777(4) 0.44161(2) 0.03560(16) Uani 1 1 d . . . . . P1 P 0.18994(13) 0.7703(2) 0.50045(16) 0.0653(9) Uani 1 1 d . . . . . P2 P 0.50944(10) 0.7756(2) 0.42054(9) 0.0291(5) Uani 1 1 d D . . . . P3 P 0.19590(13) 1.1835(2) 0.31136(12) 0.0502(7) Uani 1 1 d D . . . . C11 C 0.2111(11) 0.6132(18) 0.5310(8) 0.0507(17) Uani 0.516(8) 1 d D . P A 1 C12 C 0.2057(10) 0.4842(15) 0.5041(9) 0.0507(17) Uani 0.516(8) 1 d D . P A 1 H12 H 0.1917 0.4787 0.4621 0.061 Uiso 0.516(8) 1 calc R . P A 1 C13 C 0.2204(10) 0.3641(17) 0.5374(7) 0.0507(17) Uani 0.516(8) 1 d D . P A 1 H13 H 0.2141 0.2771 0.5178 0.061 Uiso 0.516(8) 1 calc R . P A 1 C14 C 0.2444(14) 0.369(2) 0.5993(7) 0.0507(17) Uani 0.516(8) 1 d D . P A 1 H14 H 0.2524 0.2862 0.6220 0.061 Uiso 0.516(8) 1 calc R . P A 1 C15 C 0.2563(10) 0.4961(16) 0.6270(8) 0.0507(17) Uani 0.516(8) 1 d D . P A 1 H15 H 0.2775 0.5026 0.6690 0.061 Uiso 0.516(8) 1 calc R . P A 1 C16 C 0.2367(11) 0.6158(19) 0.5921(8) 0.0507(17) Uani 0.516(8) 1 d D . P A 1 H16 H 0.2412 0.7027 0.6116 0.061 Uiso 0.516(8) 1 calc R . P A 1 C11A C 0.2285(12) 0.6281(19) 0.5628(9) 0.0507(17) Uani 0.484(8) 1 d D . P A 2 C12A C 0.2125(10) 0.4890(16) 0.5441(9) 0.0507(17) Uani 0.484(8) 1 d D . P A 2 H12A H 0.1810 0.4704 0.5045 0.061 Uiso 0.484(8) 1 calc R . P A 2 C13A C 0.2424(14) 0.377(2) 0.5831(8) 0.0507(17) Uani 0.484(8) 1 d D . P A 2 H13A H 0.2384 0.2847 0.5688 0.061 Uiso 0.484(8) 1 calc R . P A 2 C14A C 0.2784(10) 0.4068(17) 0.6438(8) 0.0507(17) Uani 0.484(8) 1 d D . P A 2 H14A H 0.2923 0.3329 0.6716 0.061 Uiso 0.484(8) 1 calc R . P A 2 C15A C 0.2943(11) 0.5445(15) 0.6642(9) 0.0507(17) Uani 0.484(8) 1 d D . P A 2 H15A H 0.3208 0.5632 0.7049 0.061 Uiso 0.484(8) 1 calc R . P A 2 C16A C 0.2702(11) 0.652(2) 0.6232(8) 0.0507(17) Uani 0.484(8) 1 d D . P A 2 H16A H 0.2821 0.7450 0.6365 0.061 Uiso 0.484(8) 1 calc R . P A 2 C21 C 0.0956(11) 0.787(3) 0.5034(8) 0.069(2) Uani 0.539(7) 1 d D . P A 1 C22 C 0.0722(9) 0.823(2) 0.5507(9) 0.069(2) Uani 0.539(7) 1 d D . P A 1 H22 H 0.1102 0.8405 0.5879 0.083 Uiso 0.539(7) 1 calc R . P A 1 C23 C -0.0019(8) 0.836(2) 0.5476(9) 0.069(2) Uani 0.539(7) 1 d D . P A 1 H23 H -0.0145 0.8610 0.5816 0.083 Uiso 0.539(7) 1 calc R . P A 1 C24 C -0.0563(10) 0.813(2) 0.4944(8) 0.069(2) Uani 0.539(7) 1 d D . P A 1 H24 H -0.1076 0.8280 0.4904 0.083 Uiso 0.539(7) 1 calc R . P A 1 C25 C -0.0382(9) 0.768(2) 0.4454(9) 0.069(2) Uani 0.539(7) 1 d D . P A 1 H25 H -0.0765 0.7428 0.4094 0.083 Uiso 0.539(7) 1 calc R . P A 1 C26 C 0.0384(8) 0.760(2) 0.4511(9) 0.069(2) Uani 0.539(7) 1 d D . P A 1 H26 H 0.0511 0.7361 0.4171 0.083 Uiso 0.539(7) 1 calc R . P A 1 C26A C 0.0484(9) 0.892(2) 0.4322(10) 0.069(2) Uani 0.461(7) 1 d D . P A 2 H26A H 0.0761 0.9430 0.4125 0.083 Uiso 0.461(7) 1 calc R . P A 2 C22A C 0.0452(9) 0.717(2) 0.4998(11) 0.069(2) Uani 0.461(7) 1 d D . P A 2 H22A H 0.0684 0.6391 0.5233 0.083 Uiso 0.461(7) 1 calc R . P A 2 C25A C -0.0284(9) 0.916(2) 0.4159(11) 0.069(2) Uani 0.461(7) 1 d D . P A 2 H25A H -0.0546 0.9742 0.3837 0.083 Uiso 0.461(7) 1 calc R . P A 2 C23A C -0.0306(10) 0.745(2) 0.4904(11) 0.069(2) Uani 0.461(7) 1 d D . P A 2 H23A H -0.0580 0.6965 0.5111 0.083 Uiso 0.461(7) 1 calc R . P A 2 C24A C -0.0640(12) 0.848(2) 0.4494(10) 0.069(2) Uani 0.461(7) 1 d D . P A 2 H24A H -0.1146 0.8732 0.4443 0.083 Uiso 0.461(7) 1 calc R . P A 2 C21A C 0.0869(13) 0.799(3) 0.4754(11) 0.069(2) Uani 0.461(7) 1 d D . P A 2 C31 C 0.5083(11) 0.8292(18) 0.3512(8) 0.0413(12) Uani 0.494(6) 1 d D . P B 1 C32 C 0.5468(9) 0.7515(17) 0.3223(6) 0.0413(12) Uani 0.494(6) 1 d D . P B 1 H32 H 0.5712 0.6681 0.3395 0.050 Uiso 0.494(6) 1 calc R . P B 1 C33 C 0.5493(9) 0.7963(16) 0.2677(6) 0.0413(12) Uani 0.494(6) 1 d D . P B 1 H33 H 0.5706 0.7384 0.2454 0.050 Uiso 0.494(6) 1 calc R . P B 1 C34 C 0.5208(10) 0.9253(16) 0.2456(7) 0.0413(12) Uani 0.494(6) 1 d D . P B 1 H34 H 0.5283 0.9606 0.2109 0.050 Uiso 0.494(6) 1 calc R . P B 1 C35 C 0.4813(9) 1.0022(17) 0.2745(6) 0.0413(12) Uani 0.494(6) 1 d D . P B 1 H35 H 0.4586 1.0876 0.2581 0.050 Uiso 0.494(6) 1 calc R . P B 1 C36 C 0.4751(9) 0.9538(16) 0.3273(6) 0.0413(12) Uani 0.494(6) 1 d D . P B 1 H36 H 0.4481 1.0061 0.3472 0.050 Uiso 0.494(6) 1 calc R . P B 1 C31A C 0.5110(8) 0.824(2) 0.3434(7) 0.0413(12) Uani 0.506(6) 1 d D . P B 2 C32A C 0.5736(9) 0.8845(17) 0.3347(6) 0.0413(12) Uani 0.506(6) 1 d D . P B 2 H32A H 0.6182 0.8984 0.3678 0.050 Uiso 0.506(6) 1 calc R . P B 2 C33A C 0.5721(8) 0.9248(17) 0.2786(5) 0.0413(12) Uani 0.506(6) 1 d D . P B 2 H33A H 0.6159 0.9622 0.2729 0.050 Uiso 0.506(6) 1 calc R . P B 2 C1 C 0.5053(7) 0.9093(19) 0.2308(7) 0.0413(12) Uani 0.506(6) 1 d D . P B 2 H1 H 0.5022 0.9483 0.1935 0.050 Uiso 0.506(6) 1 calc R . P B 2 C35A C 0.4434(9) 0.8395(16) 0.2354(6) 0.0413(12) Uani 0.506(6) 1 d D . P B 2 H35A H 0.4005 0.8184 0.2018 0.050 Uiso 0.506(6) 1 calc R . P B 2 C36A C 0.4481(9) 0.8022(17) 0.2929(5) 0.0413(12) Uani 0.506(6) 1 d D . P B 2 H36A H 0.4055 0.7587 0.2980 0.050 Uiso 0.506(6) 1 calc R . P B 2 C51 C 0.2082(9) 1.3492(14) 0.2878(5) 0.0536(16) Uani 0.632(7) 1 d D . P C 1 C52 C 0.2287(9) 1.4619(11) 0.3257(6) 0.0536(16) Uani 0.632(7) 1 d D . P C 1 H52 H 0.2340 1.4514 0.3664 0.064 Uiso 0.632(7) 1 calc R . P C 1 C53 C 0.2416(9) 1.5897(13) 0.3046(6) 0.0536(16) Uani 0.632(7) 1 d D . P C 1 H53 H 0.2566 1.6656 0.3312 0.064 Uiso 0.632(7) 1 calc R . P C 1 C54 C 0.2328(10) 1.6083(14) 0.2454(5) 0.0536(16) Uani 0.632(7) 1 d D . P C 1 H54 H 0.2413 1.6959 0.2307 0.064 Uiso 0.632(7) 1 calc R . P C 1 C55 C 0.2113(8) 1.4950(11) 0.2082(6) 0.0536(16) Uani 0.632(7) 1 d D . P C 1 H55 H 0.2060 1.5053 0.1674 0.064 Uiso 0.632(7) 1 calc R . P C 1 C56 C 0.1972(8) 1.3672(13) 0.2282(6) 0.0536(16) Uani 0.632(7) 1 d D . P C 1 H56 H 0.1801 1.2924 0.2012 0.064 Uiso 0.632(7) 1 calc R . P C 1 C53A C 0.2790(9) 1.4850(17) 0.2167(7) 0.0536(16) Uani 0.368(7) 1 d D . P C 2 H53A H 0.3090 1.4889 0.1918 0.064 Uiso 0.368(7) 1 calc R . P C 2 C52A C 0.2645(10) 1.3585(14) 0.2384(8) 0.0536(16) Uani 0.368(7) 1 d DG . P C 2 H52A H 0.2847 1.2759 0.2283 0.064 Uiso 0.368(7) 1 calc R . P C 2 C51A C 0.2205(11) 1.3529(13) 0.2748(8) 0.0536(16) Uani 0.368(7) 1 d DG . P C 2 C56A C 0.1910(10) 1.4738(17) 0.2895(8) 0.0536(16) Uani 0.368(7) 1 d DG . P C 2 H56A H 0.1609 1.4700 0.3144 0.064 Uiso 0.368(7) 1 calc R . P C 2 C55A C 0.2054(10) 1.6004(14) 0.2678(9) 0.0536(16) Uani 0.368(7) 1 d DG . P C 2 H55A H 0.1851 1.6830 0.2779 0.064 Uiso 0.368(7) 1 calc R . P C 2 C54A C 0.2494(10) 1.6059(13) 0.2315(9) 0.0536(16) Uani 0.368(7) 1 d DG . P C 2 H54A H 0.2593 1.6924 0.2167 0.064 Uiso 0.368(7) 1 calc R . P C 2 C61 C 0.1094(8) 1.1170(16) 0.2581(7) 0.0715(18) Uani 0.789(7) 1 d D . P C 1 C62 C 0.1125(6) 1.0181(13) 0.2173(5) 0.0715(18) Uani 0.789(7) 1 d D . P C 1 H62 H 0.1600 0.9810 0.2194 0.086 Uiso 0.789(7) 1 calc R . P C 1 C63 C 0.0481(5) 0.9713(13) 0.1732(6) 0.0715(18) Uani 0.789(7) 1 d D . P C 1 H63 H 0.0520 0.9063 0.1446 0.086 Uiso 0.789(7) 1 calc R . P C 1 C64 C -0.0218(6) 1.0198(14) 0.1712(6) 0.0715(18) Uani 0.789(7) 1 d D . P C 1 H64 H -0.0661 0.9941 0.1396 0.086 Uiso 0.789(7) 1 calc R . P C 1 C65 C -0.0260(6) 1.1063(13) 0.2160(5) 0.0715(18) Uani 0.789(7) 1 d D . P C 1 H65 H -0.0741 1.1325 0.2172 0.086 Uiso 0.789(7) 1 calc R . P C 1 C66 C 0.0388(6) 1.1558(13) 0.2593(6) 0.0715(18) Uani 0.789(7) 1 d D . P C 1 H66 H 0.0348 1.2159 0.2895 0.086 Uiso 0.789(7) 1 calc R . P C 1 C61A C 0.115(4) 1.117(6) 0.250(2) 0.0715(18) Uani 0.211(7) 1 d D . P C 2 C62A C 0.094(2) 1.157(5) 0.1912(19) 0.0715(18) Uani 0.211(7) 1 d D . P C 2 H62A H 0.1247 1.2209 0.1796 0.086 Uiso 0.211(7) 1 calc R . P C 2 C63A C 0.029(2) 1.108(4) 0.148(2) 0.0715(18) Uani 0.211(7) 1 d D . P C 2 H63A H 0.0053 1.1527 0.1113 0.086 Uiso 0.211(7) 1 calc R . P C 2 C64A C 0.002(3) 0.986(5) 0.165(2) 0.0715(18) Uani 0.211(7) 1 d D . P C 2 H64A H -0.0338 0.9357 0.1337 0.086 Uiso 0.211(7) 1 calc R . P C 2 C65A C 0.022(2) 0.930(5) 0.2213(17) 0.0715(18) Uani 0.211(7) 1 d D . P C 2 H65A H -0.0018 0.8506 0.2306 0.086 Uiso 0.211(7) 1 calc R . P C 2 C66A C 0.079(2) 1.002(4) 0.263(2) 0.0715(18) Uani 0.211(7) 1 d D . P C 2 H66A H 0.0947 0.9712 0.3033 0.086 Uiso 0.211(7) 1 calc R . P C 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 B1 0.036(6) 0.031(6) 0.142(13) -0.016(7) 0.031(7) -0.006(5) B2 0.039(6) 0.032(6) 0.091(9) 0.017(6) 0.019(6) -0.006(5) B3 0.032(6) 0.035(6) 0.060(7) -0.010(5) -0.010(5) 0.008(4) B4 0.038(6) 0.039(6) 0.053(7) -0.002(5) -0.006(5) 0.003(5) B6 0.022(5) 0.030(5) 0.036(6) 0.002(4) -0.001(4) 0.001(4) B5 0.023(5) 0.018(4) 0.060(7) 0.005(4) 0.009(4) 0.001(4) C43 0.0356(19) 0.0290(18) 0.074(3) 0.0165(18) 0.0230(19) 0.0037(14) C46 0.0356(19) 0.0290(18) 0.074(3) 0.0165(18) 0.0230(19) 0.0037(14) C45 0.0356(19) 0.0290(18) 0.074(3) 0.0165(18) 0.0230(19) 0.0037(14) C44 0.0356(19) 0.0290(18) 0.074(3) 0.0165(18) 0.0230(19) 0.0037(14) C42 0.0356(19) 0.0290(18) 0.074(3) 0.0165(18) 0.0230(19) 0.0037(14) C41 0.0356(19) 0.0290(18) 0.074(3) 0.0165(18) 0.0230(19) 0.0037(14) Nd1 0.0173(2) 0.0230(2) 0.0553(3) 0.0017(2) -0.00253(17) -0.00102(19) P1 0.0248(12) 0.0281(13) 0.149(3) 0.0013(15) 0.0378(16) -0.0027(10) P2 0.0185(10) 0.0221(10) 0.0410(13) 0.0048(9) 0.0026(9) -0.0031(8) P3 0.0340(13) 0.0281(12) 0.0631(17) -0.0066(11) -0.0172(11) 0.0028(9) C11 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C12 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C13 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C14 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C15 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C16 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C11A 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C12A 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C13A 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C14A 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C15A 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C16A 0.045(3) 0.044(3) 0.064(5) 0.019(4) 0.020(4) -0.007(2) C21 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C22 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C23 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C24 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C25 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C26 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C26A 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C22A 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C25A 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C23A 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C24A 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C21A 0.030(3) 0.081(5) 0.098(6) 0.011(4) 0.025(4) 0.009(3) C31 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C32 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C33 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C34 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C35 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C36 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C31A 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C32A 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C33A 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C1 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C35A 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C36A 0.048(3) 0.045(3) 0.031(3) 0.004(2) 0.012(2) -0.004(2) C51 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C52 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C53 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C54 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C55 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C56 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C53A 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C52A 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C51A 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C56A 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C55A 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C54A 0.058(4) 0.039(3) 0.059(4) 0.006(3) 0.013(3) -0.003(3) C61 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C62 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C63 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C64 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C65 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C66 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C61A 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C62A 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C63A 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C64A 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C65A 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) C66A 0.041(3) 0.063(3) 0.083(4) -0.015(3) -0.016(3) -0.003(3) 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' 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 H1A B1 H1B 109.5 . . ? H1A B1 H1C 109.5 . . ? H1B B1 H1C 109.5 . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? H2A B2 H2B 109.5 . . ? H2A B2 H2C 109.5 . . ? H2B B2 H2C 109.5 . . ? P1 B2 H2A 109.5 . . ? P1 B2 H2B 109.5 . . ? P1 B2 H2C 109.5 . . ? H3A B3 H3B 109.5 . . ? H3A B3 H3C 109.5 . . ? H3B B3 H3C 109.5 . . ? P3 B3 H3A 109.5 . . ? P3 B3 H3B 109.5 . . ? P3 B3 H3C 109.5 . . ? H4A B4 H4B 109.5 . . ? H4A B4 H4C 109.5 . . ? H4B B4 H4C 109.5 . . ? P3 B4 H4A 109.5 . . ? P3 B4 H4B 109.5 . . ? P3 B4 H4C 109.5 . . ? H6A B6 H6B 109.5 . . ? H6A B6 H6C 109.5 . . ? H6B B6 H6C 109.5 . . ? P2 B6 H6A 109.5 . . ? P2 B6 H6B 109.5 . . ? P2 B6 H6C 109.5 . . ? H5A B5 H5B 109.5 . . ? H5A B5 H5C 109.5 . . ? H5B B5 H5C 109.5 . . ? P2 B5 H5A 109.5 . . ? P2 B5 H5B 109.5 . . ? P2 B5 H5C 109.5 . . ? C44 C43 H43 120.2 . . ? C44 C43 C42 119.6(8) . . ? C42 C43 H43 120.2 . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C41 C46 C45 120.3(8) . . ? C46 C45 H45 120.0 . . ? C46 C45 C44 120.0(8) . . ? C44 C45 H45 120.0 . . ? C43 C44 C45 119.6(8) . . ? C43 C44 H44 120.2 . . ? C45 C44 H44 120.2 . . ? C43 C42 H42 119.3 . . ? C41 C42 C43 121.4(7) . . ? C41 C42 H42 119.3 . . ? C46 C41 C42 118.9(7) . . ? C46 C41 P2 120.8(6) . . ? C42 C41 P2 120.2(6) . . ? B1 P1 B2 106.5(5) . . ? B1 P1 C11A 117.0(7) . . ? B2 P1 C11A 101.4(6) . . ? C11 P1 B1 100.4(7) . . ? C11 P1 B2 120.6(7) . . ? C11 P1 C21 98.9(10) . . ? C21 P1 B1 122.9(7) . . ? C21 P1 B2 108.4(8) . . ? C21A P1 B1 103.5(9) . . ? C21A P1 B2 113.1(10) . . ? C21A P1 C11A 115.4(9) . . ? B6 P2 C31A 107.8(5) . . ? B5 P2 B6 112.3(4) . . ? B5 P2 C31A 108.3(6) . . ? C41 P2 B6 113.3(4) . . ? C41 P2 B5 111.0(4) . . ? C41 P2 C31A 103.6(7) . . ? C31 P2 B6 107.5(8) . . ? C31 P2 B5 105.4(6) . . ? C31 P2 C41 106.8(7) . . ? B3 P3 B4 105.7(5) . . ? B3 P3 C51A 118.9(6) . . ? B4 P3 C51A 105.2(6) . . ? C51 P3 B3 108.7(5) . . ? C51 P3 B4 114.8(7) . . ? C51 P3 C61 106.5(7) . . ? C61 P3 B3 110.6(6) . . ? C61 P3 B4 110.5(5) . . ? C61A P3 B3 118.2(16) . . ? C61A P3 B4 106(2) . . ? C61A P3 C51A 101.2(15) . . ? C12 C11 P1 129.9(13) . . ? C16 C11 P1 113.2(12) . . ? C16 C11 C12 116.9(16) . . ? C11 C12 H12 119.4 . . ? C13 C12 C11 121.2(16) . . ? C13 C12 H12 119.4 . . ? C12 C13 H13 119.6 . . ? C12 C13 C14 120.8(18) . . ? C14 C13 H13 119.6 . . ? C13 C14 H14 120.6 . . ? C15 C14 C13 118.8(18) . . ? C15 C14 H14 120.6 . . ? C14 C15 H15 120.5 . . ? C14 C15 C16 118.9(17) . . ? C16 C15 H15 120.5 . . ? C11 C16 C15 123.0(17) . . ? C11 C16 H16 118.5 . . ? C15 C16 H16 118.5 . . ? C12A C11A P1 115.9(13) . . ? C16A C11A P1 126.3(12) . . ? C16A C11A C12A 117.8(18) . . ? C11A C12A H12A 119.3 . . ? C13A C12A C11A 121.4(18) . . ? C13A C12A H12A 119.3 . . ? C12A C13A H13A 121.0 . . ? C14A C13A C12A 118.0(19) . . ? C14A C13A H13A 121.0 . . ? C13A C14A H14A 119.3 . . ? C13A C14A C15A 121.3(18) . . ? C15A C14A H14A 119.3 . . ? C14A C15A H15A 120.7 . . ? C16A C15A C14A 118.7(18) . . ? C16A C15A H15A 120.7 . . ? C11A C16A H16A 119.0 . . ? C15A C16A C11A 122.0(18) . . ? C15A C16A H16A 119.0 . . ? C22 C21 P1 129.6(13) . . ? C26 C21 P1 115.4(13) . . ? C26 C21 C22 115.0(18) . . ? C21 C22 H22 117.6 . . ? C23 C22 C21 124.9(18) . . ? C23 C22 H22 117.6 . . ? C22 C23 H23 121.1 . . ? C24 C23 C22 117.8(18) . . ? C24 C23 H23 121.1 . . ? C23 C24 H24 119.4 . . ? C23 C24 C25 121.2(18) . . ? C25 C24 H24 119.4 . . ? C24 C25 H25 121.0 . . ? C24 C25 C26 118.0(18) . . ? C26 C25 H25 121.0 . . ? C21 C26 C25 122.9(19) . . ? C21 C26 H26 118.5 . . ? C25 C26 H26 118.5 . . ? C25A C26A H26A 118.1 . . ? C21A C26A H26A 118.1 . . ? C21A C26A C25A 124(2) . . ? C23A C22A H22A 119.5 . . ? C21A C22A H22A 119.5 . . ? C21A C22A C23A 121(2) . . ? C26A C25A H25A 122.3 . . ? C24A C25A C26A 115(2) . . ? C24A C25A H25A 122.3 . . ? C22A C23A H23A 121.6 . . ? C24A C23A C22A 117(2) . . ? C24A C23A H23A 121.6 . . ? C25A C24A C23A 124(2) . . ? C25A C24A H24A 118.0 . . ? C23A C24A H24A 118.0 . . ? C26A C21A P1 124.9(14) . . ? C26A C21A C22A 118(2) . . ? C22A C21A P1 117.4(14) . . ? C32 C31 P2 118.5(11) . . ? C32 C31 C36 120.4(17) . . ? C36 C31 P2 120.8(11) . . ? C31 C32 H32 120.3 . . ? C31 C32 C33 119.3(16) . . ? C33 C32 H32 120.3 . . ? C32 C33 H33 119.8 . . ? C34 C33 C32 120.4(16) . . ? C34 C33 H33 119.8 . . ? C33 C34 H34 120.2 . . ? C35 C34 C33 119.7(16) . . ? C35 C34 H34 120.2 . . ? C34 C35 H35 120.2 . . ? C34 C35 C36 119.6(16) . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 120.2(16) . . ? C31 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C32A C31A P2 122.4(11) . . ? C32A C31A C36A 116.7(16) . . ? C36A C31A P2 120.9(11) . . ? C31A C32A H32A 119.3 . . ? C33A C32A C31A 121.3(15) . . ? C33A C32A H32A 119.3 . . ? C32A C33A H33A 120.6 . . ? C32A C33A C1 118.8(15) . . ? C1 C33A H33A 120.6 . . ? C33A C1 H1 118.7 . . ? C35A C1 C33A 122.6(15) . . ? C35A C1 H1 118.7 . . ? C1 C35A H35A 122.3 . . ? C1 C35A C36A 115.4(15) . . ? C36A C35A H35A 122.3 . . ? C31A C36A H36A 117.7 . . ? C35A C36A C31A 124.6(15) . . ? C35A C36A H36A 117.7 . . ? C52 C51 P3 123.4(9) . . ? C56 C51 P3 117.4(9) . . ? C56 C51 C52 119.2(13) . . ? C51 C52 H52 119.8 . . ? C51 C52 C53 120.5(13) . . ? C53 C52 H52 119.8 . . ? C52 C53 H53 119.5 . . ? C54 C53 C52 120.9(13) . . ? C54 C53 H53 119.5 . . ? C53 C54 H54 121.2 . . ? C53 C54 C55 117.6(13) . . ? C55 C54 H54 121.2 . . ? C54 C55 H55 118.9 . . ? C56 C55 C54 122.3(13) . . ? C56 C55 H55 118.9 . . ? C51 C56 C55 119.4(13) . . ? C51 C56 H56 120.3 . . ? C55 C56 H56 120.3 . . ? C52A C53A H53A 120.0 . . ? C52A C53A C54A 120.0 . . ? C54A C53A H53A 120.0 . . ? C53A C52A H52A 120.0 . . ? C53A C52A C51A 120.0 . . ? C51A C52A H52A 120.0 . . ? C52A C51A P3 125.8(9) . . ? C56A C51A P3 114.2(9) . . ? C56A C51A C52A 120.0 . . ? C51A C56A H56A 120.0 . . ? C51A C56A C55A 120.0 . . ? C55A C56A H56A 120.0 . . ? C56A C55A H55A 120.0 . . ? C54A C55A C56A 120.0 . . ? C54A C55A H55A 120.0 . . ? C53A C54A H54A 120.0 . . ? C55A C54A C53A 120.0 . . ? C55A C54A H54A 120.0 . . ? C62 C61 P3 120.1(10) . . ? C62 C61 C66 117.9(14) . . ? C66 C61 P3 121.9(9) . . ? C61 C62 H62 119.0 . . ? C61 C62 C63 121.9(13) . . ? C63 C62 H62 119.0 . . ? C62 C63 H63 120.2 . . ? C64 C63 C62 119.7(12) . . ? C64 C63 H63 120.2 . . ? C63 C64 H64 120.7 . . ? C65 C64 C63 118.7(11) . . ? C65 C64 H64 120.7 . . ? C64 C65 H65 119.3 . . ? C64 C65 C66 121.3(12) . . ? C66 C65 H65 119.3 . . ? C61 C66 C65 119.8(13) . . ? C61 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C62A C61A P3 126(3) . . ? C66A C61A P3 116(3) . . ? C66A C61A C62A 117(5) . . ? C61A C62A H62A 118.7 . . ? C63A C62A C61A 123(5) . . ? C63A C62A H62A 118.7 . . ? C62A C63A H63A 123.3 . . ? C64A C63A C62A 113(4) . . ? C64A C63A H63A 123.3 . . ? C63A C64A H64A 116.5 . . ? C63A C64A C65A 127(5) . . ? C65A C64A H64A 116.5 . . ? C64A C65A H65A 123.3 . . ? C64A C65A C66A 113(5) . . ? C66A C65A H65A 123.3 . . ? C61A C66A C65A 124(5) . . ? C61A C66A H66A 117.9 . . ? C65A C66A H66A 117.9 . . ? 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 H1A 1.2000 . ? B1 H1B 1.2000 . ? B1 H1C 1.2000 . ? B1 P1 1.928(14) . ? B2 H2A 1.2000 . ? B2 H2B 1.2000 . ? B2 H2C 1.2000 . ? B2 P1 1.937(11) . ? B3 H3A 1.2000 . ? B3 H3B 1.2000 . ? B3 H3C 1.2000 . ? B3 P3 1.930(12) . ? B4 H4A 1.2000 . ? B4 H4B 1.2000 . ? B4 H4C 1.2000 . ? B4 P3 1.945(10) . ? B6 H6A 1.2000 . ? B6 H6B 1.2000 . ? B6 H6C 1.2000 . ? B6 P2 1.906(8) . ? B5 H5A 1.2000 . ? B5 H5B 1.2000 . ? B5 H5C 1.2000 . ? B5 P2 1.905(9) . ? C43 H43 0.9500 . ? C43 C44 1.368(9) . ? C43 C42 1.382(9) . ? C46 H46 0.9500 . ? C46 C45 1.385(9) . ? C46 C41 1.375(9) . ? C45 H45 0.9500 . ? C45 C44 1.397(9) . ? C44 H44 0.9500 . ? C42 H42 0.9500 . ? C42 C41 1.381(9) . ? C41 P2 1.815(8) . ? Nd1 B6 2.695(8) 3_676 ? P1 C11 1.674(18) . ? P1 C11A 1.98(2) . ? P1 C21 1.81(2) . ? P1 C21A 1.85(2) . ? P2 C31 1.729(18) . ? P2 C31A 1.913(17) . ? P3 C51 1.739(14) . ? P3 C51A 1.983(12) . ? P3 C61 1.813(16) . ? P3 C61A 1.83(6) . ? C11 C12 1.390(14) . ? C11 C16 1.375(14) . ? C12 H12 0.9500 . ? C12 C13 1.381(14) . ? C13 H13 0.9500 . ? C13 C14 1.397(14) . ? C14 H14 0.9500 . ? C14 C15 1.377(15) . ? C15 H15 0.9500 . ? C15 C16 1.400(14) . ? C16 H16 0.9500 . ? C11A C12A 1.417(15) . ? C11A C16A 1.412(14) . ? C12A H12A 0.9500 . ? C12A C13A 1.415(15) . ? C13A H13A 0.9500 . ? C13A C14A 1.408(15) . ? C14A H14A 0.9500 . ? C14A C15A 1.413(15) . ? C15A H15A 0.9500 . ? C15A C16A 1.398(14) . ? C16A H16A 0.9500 . ? C21 C22 1.391(15) . ? C21 C26 1.372(15) . ? C22 H22 0.9500 . ? C22 C23 1.378(14) . ? C23 H23 0.9500 . ? C23 C24 1.356(14) . ? C24 H24 0.9500 . ? C24 C25 1.395(14) . ? C25 H25 0.9500 . ? C25 C26 1.403(14) . ? C26 H26 0.9500 . ? C26A H26A 0.9500 . ? C26A C25A 1.383(15) . ? C26A C21A 1.376(15) . ? C22A H22A 0.9500 . ? C22A C23A 1.396(15) . ? C22A C21A 1.379(16) . ? C25A H25A 0.9500 . ? C25A C24A 1.370(15) . ? C23A H23A 0.9500 . ? C23A C24A 1.390(15) . ? C24A H24A 0.9500 . ? C31 C32 1.379(8) . ? C31 C36 1.388(8) . ? C32 H32 0.9500 . ? C32 C33 1.392(8) . ? C33 H33 0.9500 . ? C33 C34 1.389(8) . ? C34 H34 0.9500 . ? C34 C35 1.388(8) . ? C35 H35 0.9500 . ? C35 C36 1.389(8) . ? C36 H36 0.9500 . ? C31A C32A 1.391(8) . ? C31A C36A 1.394(8) . ? C32A H32A 0.9500 . ? C32A C33A 1.387(8) . ? C33A H33A 0.9500 . ? C33A C1 1.394(8) . ? C1 H1 0.9500 . ? C1 C35A 1.384(8) . ? C35A H35A 0.9500 . ? C35A C36A 1.393(8) . ? C36A H36A 0.9500 . ? C51 C52 1.385(8) . ? C51 C56 1.381(8) . ? C52 H52 0.9500 . ? C52 C53 1.386(8) . ? C53 H53 0.9500 . ? C53 C54 1.381(8) . ? C54 H54 0.9500 . ? C54 C55 1.383(8) . ? C55 H55 0.9500 . ? C55 C56 1.383(8) . ? C56 H56 0.9500 . ? C53A H53A 0.9500 . ? C53A C52A 1.3899 . ? C53A C54A 1.3903 . ? C52A H52A 0.9500 . ? C52A C51A 1.3904 . ? C51A C56A 1.3896 . ? C56A H56A 0.9500 . ? C56A C55A 1.3902 . ? C55A H55A 0.9500 . ? C55A C54A 1.3894 . ? C54A H54A 0.9500 . ? C61 C62 1.381(8) . ? C61 C66 1.392(8) . ? C62 H62 0.9500 . ? C62 C63 1.387(8) . ? C63 H63 0.9500 . ? C63 C64 1.382(8) . ? C64 H64 0.9500 . ? C64 C65 1.381(8) . ? C65 H65 0.9500 . ? C65 C66 1.392(7) . ? C66 H66 0.9500 . ? C61A C62A 1.391(9) . ? C61A C66A 1.387(9) . ? C62A H62A 0.9500 . ? C62A C63A 1.389(9) . ? C63A H63A 0.9500 . ? C63A C64A 1.387(9) . ? C64A H64A 0.9500 . ? C64A C65A 1.389(9) . ? C65A H65A 0.9500 . ? C65A C66A 1.389(9) . ? C66A H66A 0.9500 . ?