#------------------------------------------------------------------------------ #$Date: 2021-08-05 04:20:23 +0300 (Thu, 05 Aug 2021) $ #$Revision: 267955 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/79/7707953.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_7707953 loop_ _publ_author_name 'Fetrow, Taylor V.' 'Daly, Scott R.' _publ_section_title ; Mechanochemical synthesis and structural analysis of trivalent lanthanide and uranium diphenylphosphinodiboranates ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01932E _journal_year 2021 _chemical_formula_moiety 'C72 H96 B12 P6 U2' _chemical_formula_sum 'C72 H96 B12 P6 U2' _chemical_formula_weight 1753.08 _chemical_name_common U(Ph-PDB)3_polymer _chemical_name_systematic U(BH3Ph2BH3)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 2020-02-26 _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 104.030(5) _cell_angle_beta 100.044(5) _cell_angle_gamma 107.371(5) _cell_formula_units_Z 1 _cell_length_a 11.4764(14) _cell_length_b 12.8102(15) _cell_length_c 15.1334(18) _cell_measurement_reflns_used 9322 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.155 _cell_measurement_theta_min 2.5205 _cell_volume 1985.5(4) _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 149.97 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker Ventere Duo' _diffrn_measurement_method 'Photon 3 Phi and Omega Scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_unetI/netI 0.0710 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 20675 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.407 _diffrn_reflns_theta_min 2.521 _exptl_absorpt_coefficient_mu 4.232 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0567 before and 0.0449 after correction. The Ratio of minimum to maximum transmission is 0.8797. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'dark red' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_description plate-like _exptl_crystal_F_000 862 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.025 _refine_diff_density_max 1.916 _refine_diff_density_min -1.872 _refine_diff_density_rms 0.141 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 367 _refine_ls_number_reflns 8109 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.005 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0384 _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^)+(0.0358P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.0787 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6722 _reflns_number_total 8109 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01932e2.cif _cod_data_source_block dal2011 _cod_database_code 7707953 _shelx_shelxl_version_number 2016/4 _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 0.902 _shelx_estimated_absorpt_t_min 0.677 _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. Uiso/Uaniso restraints and constraints Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) Uanis(C22) = Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) 3.a 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), C42(H42), C43(H43), C44(H44), C45(H45), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C46(H46) 3.b 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 dal2011_a.res in P-1 dal2011.res created by SHELXL-2016/4 at 21:30:42 on 26-Feb-2020 REM Old TITL Dal20_11 in P-1 sample 20042 2TVF_4 REM SHELXT solution in P-1 REM R1 0.071, Rweak 0.013, Alpha 0.022, Orientation as input REM Formula found by SHELXT: C42 P3 U CELL 0.71073 11.4764 12.8102 15.1334 104.03 100.044 107.371 ZERR 1 0.0014 0.0015 0.0018 0.005 0.005 0.005 LATT 1 SFAC C H B P U UNIT 72 96 12 6 2 EQIV $1 -X,1-Y,1-Z EQIV $2 1-X,1-Y,1-Z EADP C41 C42 C43 C44 C45 C46 EADP C22 C22 C23 C24 C25 C26 L.S. 4 0 0 PLAN 20 SIZE 0.025 0.1 0.1 TEMP -123.18 FREE B4 U1_$1 FREE B3 U1 FREE B5 U1 FREE B6 U1_$2 FREE B1 U1 FREE B2 U1 CONN 12 1.98 U1 BOND $H list 4 fmap 2 53 acta OMIT 1 0 0 OMIT 0 1 0 OMIT 0 -1 1 OMIT 0 0 1 OMIT -1 1 0 OMIT -1 0 1 OMIT 1 0 1 OMIT -1 -1 1 REM REM REM WGHT 0.035800 FVAR 0.39600 B1 3 0.451786 0.596524 0.815407 11.00000 0.03484 0.02261 = 0.02408 0.00802 0.00625 0.00914 AFIX 137 1.2000 H1A 2 0.510485 0.610012 0.758186 11.00000 -1.50000 H1B 2 0.345659 0.530782 0.775804 11.00000 -1.50000 H1C 2 0.501916 0.557939 0.869221 11.00000 -1.50000 AFIX 0 B2 3 0.362521 0.801317 0.795833 11.00000 0.02683 0.02376 = 0.01850 0.00497 0.00612 0.00979 AFIX 137 1.2000 H2A 2 0.357022 0.891407 0.837687 11.00000 -1.50000 H2B 2 0.257361 0.733268 0.756555 11.00000 -1.50000 H2C 2 0.420809 0.815343 0.738460 11.00000 -1.50000 AFIX 0 B3 3 0.086432 0.486539 0.620220 11.00000 0.02318 0.02440 = 0.02947 0.01368 0.00744 0.00126 AFIX 137 1.2000 H3A 2 0.084900 0.575669 0.608828 11.00000 -1.50000 H3B 2 0.100984 0.427977 0.551102 11.00000 -1.50000 H3C 2 0.171928 0.505922 0.687312 11.00000 -1.50000 AFIX 0 B4 3 -0.225383 0.352288 0.541344 11.00000 0.02477 0.03525 = 0.02799 0.01717 0.00368 0.00914 AFIX 137 1.2000 H4A 2 -0.311912 0.296724 0.564700 11.00000 -1.50000 H4B 2 -0.213218 0.293297 0.471312 11.00000 -1.50000 H4C 2 -0.246635 0.433184 0.525634 11.00000 -1.50000 AFIX 0 B5 3 0.391118 0.420939 0.563895 11.00000 0.03669 0.01666 = 0.02641 0.00474 0.01290 0.00753 AFIX 137 1.2000 H5A 2 0.329125 0.424419 0.619990 11.00000 -1.50000 H5B 2 0.367850 0.474407 0.512514 11.00000 -1.50000 H5C 2 0.501607 0.462293 0.605074 11.00000 -1.50000 AFIX 0 B6 3 0.433373 0.237438 0.391517 11.00000 0.02090 0.01922 = 0.02217 0.01022 0.00556 0.00227 AFIX 137 1.2000 H6A 2 0.542285 0.253638 0.425641 11.00000 -1.50000 H6B 2 0.427760 0.302560 0.347127 11.00000 -1.50000 H6C 2 0.381809 0.140056 0.340077 11.00000 -1.50000 AFIX 0 C11 1 0.607305 0.844205 0.944560 11.00000 0.03067 0.02347 = 0.02319 0.00736 0.00483 0.00782 C12 1 0.656285 0.880872 1.041920 11.00000 0.03613 0.04744 = 0.02190 0.00927 0.00422 0.01297 AFIX 43 H12 2 0.604890 0.852202 1.079819 11.00000 -1.20000 AFIX 0 C13 1 0.778232 0.958192 1.084744 11.00000 0.03612 0.05386 = 0.02897 -0.00574 -0.00400 0.01716 AFIX 43 H13 2 0.809161 0.983279 1.151623 11.00000 -1.20000 AFIX 0 C14 1 0.855121 0.999084 1.031376 11.00000 0.02442 0.04609 = 0.04981 0.00228 -0.00306 0.00496 AFIX 43 H14 2 0.939403 1.051672 1.060677 11.00000 -1.20000 AFIX 0 C15 1 0.807704 0.962347 0.934022 11.00000 0.03481 0.05053 = 0.05309 0.02144 0.01318 0.00949 AFIX 43 H15 2 0.859912 0.990682 0.896476 11.00000 -1.20000 AFIX 0 C16 1 0.685674 0.885151 0.890747 11.00000 0.03249 0.04558 = 0.03024 0.00918 0.00491 0.00984 AFIX 43 H16 2 0.655197 0.859937 0.823834 11.00000 -1.20000 AFIX 0 C21 1 0.367669 0.727566 0.976543 11.00000 0.03462 0.03592 = 0.02201 0.01106 0.00222 0.00366 C22 1 0.341613 0.818675 1.029680 11.00000 0.08402 0.05512 = 0.04313 0.02307 0.03181 0.01663 AFIX 43 H22 2 0.364691 0.889963 1.016764 11.00000 -1.20000 AFIX 0 C23 1 0.282362 0.807310 1.101408 11.00000 0.08402 0.05512 = 0.04313 0.02307 0.03181 0.01663 AFIX 43 H23 2 0.267966 0.871043 1.138741 11.00000 -1.20000 AFIX 0 C24 1 0.244889 0.702743 1.117622 11.00000 0.08402 0.05512 = 0.04313 0.02307 0.03181 0.01663 AFIX 43 H24 2 0.203188 0.693827 1.165775 11.00000 -1.20000 AFIX 0 C25 1 0.267301 0.611817 1.064918 11.00000 0.08402 0.05512 = 0.04313 0.02307 0.03181 0.01663 AFIX 43 H25 2 0.240358 0.539826 1.076403 11.00000 -1.20000 AFIX 0 C26 1 0.329123 0.623104 0.994533 11.00000 0.08402 0.05512 = 0.04313 0.02307 0.03181 0.01663 AFIX 43 H26 2 0.344948 0.559285 0.958784 11.00000 -1.20000 AFIX 0 C31 1 -0.089988 0.505965 0.742699 11.00000 0.02064 0.02898 = 0.03029 0.01556 0.01115 0.00345 C32 1 0.010489 0.567870 0.822861 11.00000 0.02131 0.09702 = 0.04024 -0.00872 0.00471 0.01285 AFIX 43 H32 2 0.088163 0.554726 0.826791 11.00000 -1.20000 AFIX 0 C33 1 -0.000955 0.647817 0.896509 11.00000 0.04271 0.10725 = 0.04981 -0.02331 0.01304 -0.00550 AFIX 43 H33 2 0.068675 0.687686 0.951048 11.00000 -1.20000 AFIX 0 C34 1 -0.108360 0.671299 0.893540 11.00000 0.06388 0.03843 = 0.05939 0.00963 0.03319 0.00711 AFIX 43 H34 2 -0.113483 0.728691 0.944339 11.00000 -1.20000 AFIX 0 C35 1 -0.208453 0.611847 0.817146 11.00000 0.06116 0.06055 = 0.05079 0.03064 0.02974 0.04044 AFIX 43 H35 2 -0.285555 0.625772 0.814835 11.00000 -1.20000 AFIX 0 C36 1 -0.199023 0.529888 0.741456 11.00000 0.04835 0.05281 = 0.02753 0.01669 0.01031 0.02648 AFIX 43 H36 2 -0.269875 0.489734 0.687803 11.00000 -1.20000 AFIX 0 PART 1 C41 1 -0.053966 0.286384 0.681935 11.00000 0.04732 0.04588 = 0.06765 0.03732 0.01092 0.01328 C42 1 0.062778 0.288384 0.724384 11.00000 0.04732 0.04588 = 0.06765 0.03732 0.01092 0.01328 AFIX 43 H42 2 0.136168 0.353566 0.734610 11.00000 -1.20000 AFIX 0 C43 1 0.074455 0.195244 0.752662 11.00000 0.04732 0.04588 = 0.06765 0.03732 0.01092 0.01328 AFIX 43 H43 2 0.156325 0.196709 0.779739 11.00000 -1.20000 AFIX 0 C44 1 -0.027208 0.104061 0.742414 11.00000 0.04732 0.04588 = 0.06765 0.03732 0.01092 0.01328 AFIX 43 H44 2 -0.018321 0.042380 0.763960 11.00000 -1.20000 AFIX 0 C45 1 -0.142381 0.101084 0.701061 11.00000 0.04732 0.04588 = 0.06765 0.03732 0.01092 0.01328 AFIX 43 H45 2 -0.215322 0.036324 0.692706 11.00000 -1.20000 AFIX 0 PART 0 C51 1 0.382521 0.183432 0.570427 11.00000 0.01578 0.01990 = 0.02354 0.01102 0.00463 0.00252 C52 1 0.416979 0.235238 0.667212 11.00000 0.06590 0.03564 = 0.02891 0.01608 0.01107 0.02582 AFIX 43 H52 2 0.421661 0.312334 0.692471 11.00000 -1.20000 AFIX 0 C53 1 0.444876 0.174222 0.727777 11.00000 0.09526 0.06235 = 0.02574 0.02703 0.01198 0.04066 AFIX 43 H53 2 0.468769 0.210039 0.794248 11.00000 -1.20000 AFIX 0 C54 1 0.437927 0.062368 0.691626 11.00000 0.04483 0.05255 = 0.04540 0.03757 0.00698 0.01566 AFIX 43 H54 2 0.455641 0.020662 0.733048 11.00000 -1.20000 AFIX 0 C55 1 0.405740 0.011895 0.596763 11.00000 0.05849 0.02628 = 0.05347 0.02166 0.00826 0.01483 AFIX 43 H55 2 0.402566 -0.064791 0.571917 11.00000 -1.20000 AFIX 0 C56 1 0.377287 0.071587 0.535439 11.00000 0.05321 0.02533 = 0.03688 0.01383 0.00067 0.01396 AFIX 43 H56 2 0.354122 0.035099 0.469089 11.00000 -1.20000 AFIX 0 C61 1 0.179290 0.206657 0.437132 11.00000 0.01428 0.01850 = 0.02176 0.00469 0.00384 0.00505 C62 1 0.094270 0.154070 0.482462 11.00000 0.02977 0.03257 = 0.02603 0.01021 0.00874 0.00886 AFIX 43 H62 2 0.124177 0.141176 0.539995 11.00000 -1.20000 AFIX 0 C63 1 -0.035221 0.120671 0.442205 11.00000 0.02584 0.03334 = 0.04230 0.01137 0.01518 0.00388 AFIX 43 H63 2 -0.093794 0.081937 0.471327 11.00000 -1.20000 AFIX 0 C64 1 -0.079392 0.142888 0.361138 11.00000 0.01906 0.03177 = 0.03974 0.00698 0.00409 0.00793 AFIX 43 H64 2 -0.167876 0.121376 0.335226 11.00000 -1.20000 AFIX 0 C65 1 0.005388 0.196646 0.317441 11.00000 0.03357 0.03826 = 0.03312 0.01685 0.00467 0.01702 AFIX 43 H65 2 -0.024499 0.211698 0.260963 11.00000 -1.20000 AFIX 0 C66 1 0.133613 0.228429 0.356043 11.00000 0.02496 0.02770 = 0.03119 0.01185 0.00375 0.00543 AFIX 43 H66 2 0.191548 0.266133 0.325987 11.00000 -1.20000 AFIX 0 P1 4 0.447438 0.742833 0.884682 11.00000 0.02835 0.02334 = 0.01755 0.00745 0.00407 0.00515 P2 4 -0.071517 0.406454 0.641736 11.00000 0.01758 0.02519 = 0.02388 0.01390 0.00498 0.00418 P3 4 0.350618 0.263128 0.490219 11.00000 0.01974 0.01532 = 0.01898 0.00780 0.00518 0.00556 U1 5 0.328332 0.609565 0.633837 11.00000 0.01670 0.01511 = 0.01883 0.00680 0.00512 0.00393 C46 1 -0.155710 0.191892 0.670419 11.00000 0.04732 0.04588 = 0.06765 0.03732 0.01092 0.01328 AFIX 43 H46 2 -0.237821 0.187676 0.640784 11.00000 -1.20000 AFIX 0 HKLF 4 REM dal2011_a.res in P-1 REM R1 = 0.0384 for 6722 Fo > 4sig(Fo) and 0.0534 for all 8109 data REM 367 parameters refined using 0 restraints END WGHT 0.0358 0.0000 REM Highest difference peak 1.916, deepest hole -1.872, 1-sigma level 0.141 Q1 1 0.0816 0.2384 0.8017 11.00000 0.05 1.00 Q2 1 0.3854 0.5920 0.5995 11.00000 0.05 0.99 Q3 1 0.2998 0.8352 1.1022 11.00000 0.05 0.83 Q4 1 -0.0859 0.0922 0.7161 11.00000 0.05 0.80 Q5 1 -0.1821 0.1012 0.6980 11.00000 0.05 0.79 Q6 1 0.0537 0.3291 0.7678 11.00000 0.05 0.78 Q7 1 0.3363 0.6208 1.0874 11.00000 0.05 0.72 Q8 1 0.2658 0.7648 1.1007 11.00000 0.05 0.64 Q9 1 0.2573 0.6258 0.6601 11.00000 0.05 0.63 Q10 1 -0.0394 0.1795 0.5220 11.00000 0.05 0.62 Q11 1 0.0333 0.1482 0.7070 11.00000 0.05 0.59 Q12 1 0.3949 0.6230 1.0032 11.00000 0.05 0.59 Q13 1 0.2368 0.6183 0.5844 11.00000 0.05 0.56 Q14 1 0.0231 0.1354 0.7745 11.00000 0.05 0.55 Q15 1 0.0590 0.2595 0.6806 11.00000 0.05 0.54 Q16 1 0.1567 0.5642 0.6243 11.00000 0.05 0.54 Q17 1 0.4258 0.6761 0.6634 11.00000 0.05 0.53 Q18 1 -0.2052 0.4235 0.5388 11.00000 0.05 0.51 Q19 1 0.3021 0.0667 0.4147 11.00000 0.05 0.51 Q20 1 0.0011 0.4398 0.6177 11.00000 0.05 0.50 ; 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294.67 58.29 -1 0 17 194.28 58.79 0 0 -17 22.40 52.89 0 0 -17 76.49 61.59 0 0 17 4.20 49.99 -1 0 -17 171.68 56.39 1 0 17 128.49 59.39 8 -1 -17 -89.09 54.09 8 -1 -17 -4.00 51.49 7 -1 -17 348.97 68.19 6 -1 -17 392.36 68.49 5 -1 -17 44.80 52.69 4 -1 -17 446.36 73.89 3 -1 -17 535.85 73.19 -3 1 17 457.25 77.99 2 -1 -17 9.20 50.19 2 -1 -17 27.10 58.29 -2 1 17 -42.30 53.09 1 -1 -17 220.88 61.59 1 -1 -17 167.58 61.69 -1 1 17 269.97 63.59 0 -1 -17 261.07 60.99 0 1 17 362.66 69.79 7 -2 -17 113.19 60.09 6 -2 -17 699.73 81.29 5 -2 -17 30.60 59.39 4 -2 -17 20.20 53.09 -4 2 17 53.19 52.39 3 -2 -17 662.23 79.69 -3 2 17 573.34 77.59 2 -2 -17 165.18 65.59 2 -2 -17 115.59 52.19 -2 2 17 113.09 62.59 1 -2 -17 54.29 57.79 -1 2 17 143.09 58.19 6 -3 -17 149.69 63.69 5 -3 -17 256.07 67.29 4 -3 -17 4.60 56.99 -4 3 17 83.49 58.39 3 -3 -17 113.59 81.29 3 -3 -17 160.98 65.59 -3 3 17 150.88 60.99 2 8 -18 410.16 70.19 1 8 -18 -13.20 56.19 0 8 -18 211.68 69.99 4 7 -18 105.09 53.69 3 7 -18 158.58 56.39 2 7 -18 451.45 76.09 1 7 -18 94.79 60.99 0 7 -18 134.19 63.69 0 7 -18 127.09 60.79 -1 7 -18 423.56 75.59 -1 7 -18 404.86 81.09 5 6 -18 21.30 58.59 5 6 -18 86.89 54.19 4 6 -18 282.97 58.49 3 6 -18 -1.50 47.40 2 6 -18 121.19 59.39 1 6 -18 92.79 103.89 1 6 -18 79.89 60.89 0 6 -18 -12.70 51.69 0 6 -18 -25.60 50.59 -1 6 -18 388.06 73.09 -1 6 -18 366.76 70.29 5 5 -18 9.70 51.89 5 5 -18 -18.00 50.89 4 5 -18 253.07 65.39 4 5 -18 397.26 63.39 3 5 -18 248.38 57.69 2 5 -18 40.90 50.19 1 5 -18 389.16 63.99 1 5 -18 469.55 72.69 0 5 -18 263.57 65.59 0 5 -18 229.88 61.79 -1 5 -18 48.10 56.69 -1 5 -18 80.79 57.39 1 -5 18 132.49 64.79 -2 5 -18 352.76 70.89 6 4 -18 252.57 59.99 6 4 -18 272.37 65.29 5 4 -18 4.30 51.19 5 4 -18 81.29 54.09 4 4 -18 152.38 54.89 4 4 -18 147.59 56.89 3 4 -18 422.96 70.39 2 4 -18 29.40 49.10 1 4 -18 143.59 59.39 1 4 -18 165.68 55.69 0 4 -18 478.65 71.79 0 4 -18 485.75 69.99 0 -4 18 480.65 74.29 -1 4 -18 28.60 61.09 -1 4 -18 -5.00 57.89 1 -4 18 59.09 64.39 6 3 -18 49.50 58.49 6 3 -18 80.99 50.79 5 3 -18 156.38 60.59 5 3 -18 259.27 64.09 4 3 -18 21.90 52.69 3 3 -18 366.76 66.09 2 3 -18 293.67 65.59 1 3 -18 16.90 51.89 1 3 -18 -12.50 50.29 -1 -3 18 15.50 55.29 0 3 -18 286.07 67.19 0 3 -18 182.48 63.59 0 -3 18 236.18 64.79 -1 3 -18 236.38 66.89 -1 3 -18 244.98 65.39 1 -3 18 114.09 61.59 6 2 -18 19.20 49.00 6 2 -18 105.29 56.39 5 2 -18 358.36 64.89 4 2 -18 332.07 63.39 3 2 -18 206.88 63.79 2 2 -18 401.36 68.69 1 2 -18 361.26 67.79 1 2 -18 247.08 58.09 -1 -2 18 273.77 64.49 0 2 -18 11.70 48.70 0 2 -18 8.20 55.29 0 -2 18 -44.50 52.79 6 1 -18 53.69 54.39 5 1 -18 86.69 57.09 4 1 -18 309.87 69.79 3 1 -18 27.10 53.39 2 1 -18 208.18 61.69 -2 -1 18 251.87 64.79 1 1 -18 464.15 72.99 1 1 -18 422.86 77.19 -1 -1 18 480.55 74.59 0 1 -18 25.80 57.39 0 1 -18 39.00 53.49 0 -1 18 15.70 57.69 6 0 -18 333.97 67.79 5 0 -18 -0.80 57.59 4 0 -18 194.38 62.59 3 0 -18 312.67 68.89 2 0 -18 30.20 52.99 2 0 -18 11.20 56.99 -2 0 18 14.40 54.89 1 0 -18 9.90 57.99 1 0 -18 87.19 53.89 -1 0 18 -4.20 55.39 4 -1 -18 10.70 60.59 -3 1 18 397.86 73.99 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 30886 _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 0.4518(6) 0.5965(5) 0.8154(4) 0.0275(14) Uani 1 1 d . . . . . H1A H 0.510485 0.610012 0.758186 0.041 Uiso 1 1 calc GR . . . . H1B H 0.345659 0.530782 0.775804 0.041 Uiso 1 1 calc GR . . . . H1C H 0.501916 0.557939 0.869221 0.041 Uiso 1 1 calc GR . . . . B2 B 0.3625(6) 0.8013(5) 0.7958(4) 0.0232(13) Uani 1 1 d . . . . . H2A H 0.357022 0.891407 0.837687 0.035 Uiso 1 1 calc GR . . . . H2B H 0.257361 0.733268 0.756555 0.035 Uiso 1 1 calc GR . . . . H2C H 0.420809 0.815343 0.738460 0.035 Uiso 1 1 calc GR . . . . B3 B 0.0864(5) 0.4865(5) 0.6202(4) 0.0264(14) Uani 1 1 d . . . . . H3A H 0.084900 0.575669 0.608828 0.040 Uiso 1 1 calc GR . . . . H3B H 0.100984 0.427977 0.551102 0.040 Uiso 1 1 calc GR . . . . H3C H 0.171928 0.505922 0.687312 0.040 Uiso 1 1 calc GR . . . . B4 B -0.2254(6) 0.3523(5) 0.5413(4) 0.0288(15) Uani 1 1 d . . . . . H4A H -0.311912 0.296724 0.564700 0.043 Uiso 1 1 calc GR . . . . H4B H -0.213218 0.293297 0.471312 0.043 Uiso 1 1 calc GR . . . . H4C H -0.246635 0.433184 0.525634 0.043 Uiso 1 1 calc GR . . . . B5 B 0.3911(6) 0.4209(5) 0.5639(4) 0.0268(14) Uani 1 1 d . . . . . H5A H 0.329125 0.424419 0.619990 0.040 Uiso 1 1 calc GR . . . . H5B H 0.367850 0.474407 0.512514 0.040 Uiso 1 1 calc GR . . . . H5C H 0.501607 0.462293 0.605074 0.040 Uiso 1 1 calc GR . . . . B6 B 0.4334(5) 0.2374(5) 0.3915(4) 0.0212(13) Uani 1 1 d . . . . . H6A H 0.542285 0.253638 0.425641 0.032 Uiso 1 1 calc GR . . . . H6B H 0.427760 0.302560 0.347127 0.032 Uiso 1 1 calc GR . . . . H6C H 0.381809 0.140056 0.340077 0.032 Uiso 1 1 calc GR . . . . C11 C 0.6073(5) 0.8442(4) 0.9446(4) 0.0265(12) Uani 1 1 d . . . . . C12 C 0.6563(5) 0.8809(5) 1.0419(4) 0.0364(14) Uani 1 1 d . . . . . H12 H 0.604890 0.852202 1.079819 0.044 Uiso 1 1 calc R . . . . C13 C 0.7782(6) 0.9582(5) 1.0847(4) 0.0447(17) Uani 1 1 d . . . . . H13 H 0.809161 0.983279 1.151623 0.054 Uiso 1 1 calc R . . . . C14 C 0.8551(6) 0.9991(5) 1.0314(5) 0.0461(17) Uani 1 1 d . . . . . H14 H 0.939403 1.051672 1.060677 0.055 Uiso 1 1 calc R . . . . C15 C 0.8077(6) 0.9623(5) 0.9340(5) 0.0463(17) Uani 1 1 d . . . . . H15 H 0.859912 0.990682 0.896476 0.056 Uiso 1 1 calc R . . . . C16 C 0.6857(5) 0.8852(5) 0.8907(4) 0.0381(15) Uani 1 1 d . . . . . H16 H 0.655197 0.859937 0.823834 0.046 Uiso 1 1 calc R . . . . C21 C 0.3677(5) 0.7276(5) 0.9765(4) 0.0333(14) Uani 1 1 d . . . . . C22 C 0.3416(7) 0.8187(6) 1.0297(5) 0.0592(9) Uani 1 1 d . . . . . H22 H 0.364691 0.889963 1.016764 0.071 Uiso 1 1 calc R . . . . C23 C 0.2824(7) 0.8073(6) 1.1014(5) 0.0592(9) Uani 1 1 d . . . . . H23 H 0.267966 0.871043 1.138741 0.071 Uiso 1 1 calc R . . . . C24 C 0.2449(7) 0.7027(6) 1.1176(5) 0.0592(9) Uani 1 1 d . . . . . H24 H 0.203188 0.693827 1.165775 0.071 Uiso 1 1 calc R . . . . C25 C 0.2673(7) 0.6118(6) 1.0649(5) 0.0592(9) Uani 1 1 d . . . . . H25 H 0.240358 0.539826 1.076403 0.071 Uiso 1 1 calc R . . . . C26 C 0.3291(7) 0.6231(6) 0.9945(5) 0.0592(9) Uani 1 1 d . . . . . H26 H 0.344948 0.559285 0.958784 0.071 Uiso 1 1 calc R . . . . C31 C -0.0900(5) 0.5060(4) 0.7427(4) 0.0261(12) Uani 1 1 d . . . . . C32 C 0.0105(6) 0.5679(7) 0.8229(5) 0.061(2) Uani 1 1 d . . . . . H32 H 0.088163 0.554726 0.826791 0.073 Uiso 1 1 calc R . . . . C33 C -0.0010(7) 0.6478(8) 0.8965(6) 0.083(3) Uani 1 1 d . . . . . H33 H 0.068675 0.687686 0.951048 0.100 Uiso 1 1 calc R . . . . C34 C -0.1084(7) 0.6713(6) 0.8935(5) 0.0554(19) Uani 1 1 d . . . . . H34 H -0.113483 0.728691 0.944339 0.066 Uiso 1 1 calc R . . . . C35 C -0.2085(7) 0.6118(6) 0.8171(5) 0.0485(17) Uani 1 1 d . . . . . H35 H -0.285555 0.625772 0.814835 0.058 Uiso 1 1 calc R . . . . C36 C -0.1990(6) 0.5299(5) 0.7415(4) 0.0401(15) Uani 1 1 d . . . . . H36 H -0.269875 0.489734 0.687803 0.048 Uiso 1 1 calc R . . . . C41 C -0.0540(6) 0.2864(5) 0.6819(5) 0.0513(7) Uani 1 1 d . . . A 1 C42 C 0.0628(6) 0.2884(6) 0.7244(5) 0.0513(7) Uani 1 1 d . . . A 1 H42 H 0.136168 0.353566 0.734610 0.062 Uiso 1 1 calc R . . A 1 C43 C 0.0745(6) 0.1952(5) 0.7527(5) 0.0513(7) Uani 1 1 d . . . A 1 H43 H 0.156325 0.196709 0.779739 0.062 Uiso 1 1 calc R . . A 1 C44 C -0.0272(6) 0.1041(6) 0.7424(5) 0.0513(7) Uani 1 1 d . . . A 1 H44 H -0.018321 0.042380 0.763960 0.062 Uiso 1 1 calc R . . A 1 C45 C -0.1424(6) 0.1011(5) 0.7011(5) 0.0513(7) Uani 1 1 d . . . A 1 H45 H -0.215322 0.036324 0.692706 0.062 Uiso 1 1 calc R . . A 1 C51 C 0.3825(4) 0.1834(4) 0.5704(4) 0.0199(11) Uani 1 1 d . . . . . C52 C 0.4170(6) 0.2352(5) 0.6672(4) 0.0407(15) Uani 1 1 d . . . . . H52 H 0.421661 0.312334 0.692471 0.049 Uiso 1 1 calc R . . . . C53 C 0.4449(7) 0.1742(6) 0.7278(5) 0.056(2) Uani 1 1 d . . . . . H53 H 0.468769 0.210039 0.794248 0.067 Uiso 1 1 calc R . . . . C54 C 0.4379(6) 0.0624(6) 0.6916(5) 0.0444(16) Uani 1 1 d . . . . . H54 H 0.455641 0.020662 0.733048 0.053 Uiso 1 1 calc R . . . . C55 C 0.4057(6) 0.0119(5) 0.5968(5) 0.0453(17) Uani 1 1 d . . . . . H55 H 0.402566 -0.064791 0.571917 0.054 Uiso 1 1 calc R . . . . C56 C 0.3773(6) 0.0716(5) 0.5354(4) 0.0392(15) Uani 1 1 d . . . . . H56 H 0.354122 0.035099 0.469089 0.047 Uiso 1 1 calc R . . . . C61 C 0.1793(4) 0.2067(4) 0.4371(3) 0.0188(11) Uani 1 1 d . . . . . C62 C 0.0943(5) 0.1541(4) 0.4825(4) 0.0296(13) Uani 1 1 d . . . . . H62 H 0.124177 0.141176 0.539995 0.036 Uiso 1 1 calc R . . . . C63 C -0.0352(5) 0.1207(5) 0.4422(4) 0.0347(14) Uani 1 1 d . . . . . H63 H -0.093794 0.081937 0.471327 0.042 Uiso 1 1 calc R . . . . C64 C -0.0794(5) 0.1429(5) 0.3611(4) 0.0318(13) Uani 1 1 d . . . . . H64 H -0.167876 0.121376 0.335226 0.038 Uiso 1 1 calc R . . . . C65 C 0.0054(5) 0.1966(5) 0.3174(4) 0.0335(14) Uani 1 1 d . . . . . H65 H -0.024499 0.211698 0.260963 0.040 Uiso 1 1 calc R . . . . C66 C 0.1336(5) 0.2284(4) 0.3560(4) 0.0289(13) Uani 1 1 d . . . . . H66 H 0.191548 0.266133 0.325987 0.035 Uiso 1 1 calc R . . . . P1 P 0.44744(13) 0.74283(11) 0.88468(10) 0.0241(3) Uani 1 1 d . . . . . P2 P -0.07152(12) 0.40645(11) 0.64174(10) 0.0219(3) Uani 1 1 d . . . . . P3 P 0.35062(12) 0.26313(10) 0.49022(9) 0.0177(3) Uani 1 1 d . . . . . U1 U 0.32833(2) 0.60957(2) 0.63384(2) 0.01696(6) Uani 1 1 d . . . . . C46 C -0.1557(6) 0.1919(5) 0.6704(5) 0.0513(7) Uani 1 1 d . . . . . H46 H -0.237821 0.187676 0.640784 0.062 Uiso 1 1 calc R . . A . 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 0.035(4) 0.023(3) 0.024(3) 0.008(3) 0.006(3) 0.009(3) B2 0.027(3) 0.024(3) 0.018(3) 0.005(3) 0.006(3) 0.010(3) B3 0.023(3) 0.024(3) 0.029(4) 0.014(3) 0.007(3) 0.001(3) B4 0.025(3) 0.035(4) 0.028(4) 0.017(3) 0.004(3) 0.009(3) B5 0.037(4) 0.017(3) 0.026(4) 0.005(3) 0.013(3) 0.008(3) B6 0.021(3) 0.019(3) 0.022(3) 0.010(3) 0.006(3) 0.002(2) C11 0.031(3) 0.023(3) 0.023(3) 0.007(2) 0.005(2) 0.008(2) C12 0.036(3) 0.047(4) 0.022(3) 0.009(3) 0.004(3) 0.013(3) C13 0.036(4) 0.054(4) 0.029(4) -0.006(3) -0.004(3) 0.017(3) C14 0.024(3) 0.046(4) 0.050(4) 0.002(3) -0.003(3) 0.005(3) C15 0.035(4) 0.051(4) 0.053(5) 0.021(4) 0.013(3) 0.009(3) C16 0.032(3) 0.046(4) 0.030(4) 0.009(3) 0.005(3) 0.010(3) C21 0.035(3) 0.036(3) 0.022(3) 0.011(3) 0.002(3) 0.004(3) C22 0.084(2) 0.055(2) 0.0431(19) 0.0231(17) 0.0318(17) 0.0166(19) C23 0.084(2) 0.055(2) 0.0431(19) 0.0231(17) 0.0318(17) 0.0166(19) C24 0.084(2) 0.055(2) 0.0431(19) 0.0231(17) 0.0318(17) 0.0166(19) C25 0.084(2) 0.055(2) 0.0431(19) 0.0231(17) 0.0318(17) 0.0166(19) C26 0.084(2) 0.055(2) 0.0431(19) 0.0231(17) 0.0318(17) 0.0166(19) C31 0.021(3) 0.029(3) 0.030(3) 0.016(3) 0.011(2) 0.003(2) C32 0.021(3) 0.097(6) 0.040(4) -0.009(4) 0.005(3) 0.013(4) C33 0.043(5) 0.107(7) 0.050(5) -0.023(5) 0.013(4) -0.005(5) C34 0.064(5) 0.038(4) 0.059(5) 0.010(4) 0.033(4) 0.007(4) C35 0.061(4) 0.061(4) 0.051(4) 0.031(4) 0.030(4) 0.040(4) C36 0.048(4) 0.053(4) 0.028(3) 0.017(3) 0.010(3) 0.026(3) C41 0.0473(16) 0.0459(16) 0.068(2) 0.0373(15) 0.0109(15) 0.0133(13) C42 0.0473(16) 0.0459(16) 0.068(2) 0.0373(15) 0.0109(15) 0.0133(13) C43 0.0473(16) 0.0459(16) 0.068(2) 0.0373(15) 0.0109(15) 0.0133(13) C44 0.0473(16) 0.0459(16) 0.068(2) 0.0373(15) 0.0109(15) 0.0133(13) C45 0.0473(16) 0.0459(16) 0.068(2) 0.0373(15) 0.0109(15) 0.0133(13) C51 0.016(2) 0.020(2) 0.024(3) 0.011(2) 0.005(2) 0.003(2) C52 0.066(4) 0.036(3) 0.029(3) 0.016(3) 0.011(3) 0.026(3) C53 0.095(6) 0.062(5) 0.026(4) 0.027(3) 0.012(4) 0.041(4) C54 0.045(4) 0.053(4) 0.045(4) 0.038(4) 0.007(3) 0.016(3) C55 0.058(4) 0.026(3) 0.053(5) 0.022(3) 0.008(4) 0.015(3) C56 0.053(4) 0.025(3) 0.037(4) 0.014(3) 0.001(3) 0.014(3) C61 0.014(2) 0.019(2) 0.022(3) 0.005(2) 0.004(2) 0.005(2) C62 0.030(3) 0.033(3) 0.026(3) 0.010(3) 0.009(3) 0.009(3) C63 0.026(3) 0.033(3) 0.042(4) 0.011(3) 0.015(3) 0.004(3) C64 0.019(3) 0.032(3) 0.040(4) 0.007(3) 0.004(3) 0.008(2) C65 0.034(3) 0.038(3) 0.033(3) 0.017(3) 0.005(3) 0.017(3) C66 0.025(3) 0.028(3) 0.031(3) 0.012(3) 0.004(3) 0.005(2) P1 0.0284(7) 0.0233(7) 0.0176(7) 0.0074(6) 0.0041(6) 0.0051(6) P2 0.0176(7) 0.0252(7) 0.0239(7) 0.0139(6) 0.0050(6) 0.0042(6) P3 0.0197(7) 0.0153(6) 0.0190(7) 0.0078(5) 0.0052(6) 0.0056(5) U1 0.01670(10) 0.01511(9) 0.01883(10) 0.00680(7) 0.00512(7) 0.00393(7) C46 0.0473(16) 0.0459(16) 0.068(2) 0.0373(15) 0.0109(15) 0.0133(13) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1A B1 H1B 109.5 . . ? H1A B1 H1C 109.5 . . ? C44a C43a C42 121.3(6) . . ? C41a C42a H42 119.8 . . ? C43a C42a H42 119.8 . . ? C41a C42a C43 120.4(6) . . ? C42a C43a H43 119.3 . . ? H1B B1 H1C 109.5 . . ? P1 B1 H1A 109.5 . . ? P1 B1 H1B 109.5 . . ? P1 B1 H1C 109.5 . . ? C44a C43a H43 119.3 . . ? C43a C44a H44 120.6 . . ? H2A B2 H2B 109.5 . . ? H2A B2 H2C 109.5 . . ? C45a C44a H44 120.6 . . ? C43a C44a C45 118.9(6) . . ? C44a C45a H45 119.7 . . ? C42a C41a P2 121.2(5) . . ? C44a C45a C46 120.6(6) . . ? 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 . . ? C41a P2 B3 108.0(3) . . ? C41a P2 B4 109.9(3) . . ? C41a C46 C45 121.4(6) . . ? C45a C46 H46 119.3 . . ? C41a C46 H46 119.3 . . ? H3B B3 H3C 109.5 . . ? P2 B3 H3A 109.5 . . ? P2 B3 H3B 109.5 . . ? P2 B3 H3C 109.5 . . ? H4A B4 H4B 109.5 . . ? H4A B4 H4C 109.5 . . ? H4B B4 H4C 109.5 . . ? P2 B4 H4A 109.5 . . ? P2 B4 H4B 109.5 . . ? P2 B4 H4C 109.5 . . ? H5A B5 H5B 109.5 . . ? H5A B5 H5C 109.5 . . ? H5B B5 H5C 109.5 . . ? P3 B5 H5A 109.5 . . ? P3 B5 H5B 109.5 . . ? P3 B5 H5C 109.5 . . ? H6A B6 H6B 109.5 . . ? H6A B6 H6C 109.5 . . ? H6B B6 H6C 109.5 . . ? P3 B6 H6A 109.5 . . ? P3 B6 H6B 109.5 . . ? P3 B6 H6C 109.5 . . ? C12 C11 C16 118.1(5) . . ? C12 C11 P1 123.0(4) . . ? C16 C11 P1 118.8(4) . . ? C11 C12 H12 119.4 . . ? C13 C12 C11 121.3(6) . . ? C13 C12 H12 119.4 . . ? C12 C13 H13 119.8 . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 119.8 . . ? C13 C14 H14 120.6 . . ? C13 C14 C15 118.8(6) . . ? C15 C14 H14 120.6 . . ? C14 C15 H15 119.5 . . ? C16 C15 C14 121.0(6) . . ? C16 C15 H15 119.5 . . ? C11 C16 H16 119.8 . . ? C15 C16 C11 120.3(6) . . ? C15 C16 H16 119.8 . . ? C22 C21 P1 121.4(5) . . ? C26 C21 C22 118.3(6) . . ? C26 C21 P1 120.3(5) . . ? C21 C22 H22 119.4 . . ? C21 C22 C23 121.2(6) . . ? C23 C22 H22 119.4 . . ? C22 C23 H23 120.4 . . ? C24 C23 C22 119.2(7) . . ? C24 C23 H23 120.4 . . ? C23 C24 H24 119.8 . . ? C25 C24 C23 120.3(7) . . ? C25 C24 H24 119.8 . . ? C24 C25 H25 119.6 . . ? C24 C25 C26 120.9(7) . . ? C26 C25 H25 119.6 . . ? C21 C26 C25 120.0(7) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C32 C31 P2 120.8(4) . . ? C36 C31 C32 116.5(5) . . ? C36 C31 P2 122.5(4) . . ? C31 C32 H32 119.6 . . ? C33 C32 C31 120.9(6) . . ? C33 C32 H32 119.6 . . ? C32 C33 H33 119.1 . . ? C34 C33 C32 121.8(7) . . ? C34 C33 H33 119.1 . . ? C33 C34 H34 120.6 . . ? C33 C34 C35 118.9(7) . . ? C35 C34 H34 120.6 . . ? C34 C35 H35 119.9 . . ? C34 C35 C36 120.2(6) . . ? C36 C35 H35 119.9 . . ? C31 C36 C35 121.7(6) . . ? C31 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C52 C51 P3 120.6(4) . . ? C56 C51 C52 118.9(5) . . ? C56 C51 P3 120.4(4) . . ? C51 C52 H52 120.0 . . ? C51 C52 C53 120.0(5) . . ? C53 C52 H52 120.0 . . ? C52 C53 H53 119.9 . . ? C54 C53 C52 120.3(6) . . ? C54 C53 H53 119.9 . . ? C53 C54 H54 120.1 . . ? C55 C54 C53 119.8(6) . . ? C55 C54 H54 120.1 . . ? C54 C55 H55 119.7 . . ? C54 C55 C56 120.5(6) . . ? C56 C55 H55 119.7 . . ? C51 C56 C55 120.4(6) . . ? C51 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C62 C61 P3 121.6(4) . . ? C66 C61 C62 119.2(5) . . ? C66 C61 P3 118.8(4) . . ? C61 C62 H62 120.5 . . ? C63 C62 C61 119.0(5) . . ? C63 C62 H62 120.5 . . ? C62 C63 H63 119.5 . . ? C64 C63 C62 121.0(5) . . ? C64 C63 H63 119.5 . . ? C63 C64 H64 120.2 . . ? C63 C64 C65 119.6(5) . . ? C65 C64 H64 120.2 . . ? C64 C65 H65 120.1 . . ? C66 C65 C64 119.7(5) . . ? C66 C65 H65 120.1 . . ? C61 C66 C65 121.3(5) . . ? C61 C66 H66 119.4 . . ? C65 C66 H66 119.4 . . ? B1 P1 B2 108.4(3) . . ? C11 P1 B1 110.3(3) . . ? C11 P1 B2 110.2(2) . . ? C21 P1 B1 110.8(3) . . ? C21 P1 B2 111.1(3) . . ? C21 P1 C11 106.0(3) . . ? B3 P2 B4 119.0(3) . . ? C31 P2 B3 106.1(3) . . ? C31 P2 B4 107.5(3) . . ? C31 P2 C41 105.5(3) . . ? B6 P3 B5 116.7(3) . . ? C51 P3 B5 108.4(3) . . ? C51 P3 B6 109.8(2) . . ? C51 P3 C61 107.4(2) . . ? C61 P3 B5 105.6(2) . . ? C61 P3 B6 108.6(2) . . ? B4 U1 B6 79.97(16) 2_566 2_666 ? C46 C41a C42 117.3(6) . . ? C46 C45a H45 119.7 . . ? C46 C41a P2 121.5(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 H1A 1.2000 . ? B1 H1B 1.2000 . ? B1 H1C 1.2000 . ? C41a C42 1.371(8) . ? C42a H42 0.9500 . ? C42a C43 1.396(8) . ? C43a H43 0.9500 . ? C43a C44 1.336(8) . ? C44a H44 0.9500 . ? C44a C45 1.345(8) . ? C45a H45 0.9500 . ? B1 P1 1.933(6) . ? C41a P2 1.836(6) . ? C41a C46 1.357(8) . ? C45a C46 1.391(8) . ? B2 H2A 1.2000 . ? B2 H2B 1.2000 . ? B2 H2C 1.2000 . ? B2 P1 1.946(6) . ? B3 H3A 1.2000 . ? B3 H3B 1.2000 . ? B3 H3C 1.2000 . ? B3 P2 1.924(6) . ? B4 H4A 1.2000 . ? B4 H4B 1.2000 . ? B4 H4C 1.2000 . ? B4 P2 1.931(6) . ? B5 H5A 1.2000 . ? B5 H5B 1.2000 . ? B5 H5C 1.2000 . ? B5 P3 1.926(6) . ? B6 H6A 1.2000 . ? B6 H6B 1.2000 . ? B6 H6C 1.2000 . ? B6 P3 1.920(6) . ? C11 C12 1.388(7) . ? C11 C16 1.389(7) . ? C11 P1 1.817(5) . ? C12 H12 0.9500 . ? C12 C13 1.380(8) . ? C13 H13 0.9500 . ? C13 C14 1.372(9) . ? C14 H14 0.9500 . ? C14 C15 1.385(9) . ? C15 H15 0.9500 . ? C15 C16 1.381(8) . ? C16 H16 0.9500 . ? C21 C22 1.391(9) . ? C21 C26 1.388(8) . ? C21 P1 1.810(6) . ? C22 H22 0.9500 . ? C22 C23 1.392(9) . ? C23 H23 0.9500 . ? C23 C24 1.375(9) . ? C24 H24 0.9500 . ? C24 C25 1.363(9) . ? C25 H25 0.9500 . ? C25 C26 1.391(9) . ? C26 H26 0.9500 . ? C31 C32 1.389(8) . ? C31 C36 1.372(7) . ? C31 P2 1.826(6) . ? C32 H32 0.9500 . ? C32 C33 1.373(10) . ? C33 H33 0.9500 . ? C33 C34 1.349(10) . ? C34 H34 0.9500 . ? C34 C35 1.350(9) . ? C35 H35 0.9500 . ? C35 C36 1.398(8) . ? C36 H36 0.9500 . ? C51 C52 1.383(7) . ? C51 C56 1.381(7) . ? C51 P3 1.822(5) . ? C52 H52 0.9500 . ? C52 C53 1.396(8) . ? C53 H53 0.9500 . ? C53 C54 1.377(9) . ? C54 H54 0.9500 . ? C54 C55 1.356(9) . ? C55 H55 0.9500 . ? C55 C56 1.393(8) . ? C56 H56 0.9500 . ? C61 C62 1.393(7) . ? C61 C66 1.374(7) . ? C61 P3 1.831(5) . ? C62 H62 0.9500 . ? C62 C63 1.393(7) . ? C63 H63 0.9500 . ? C63 C64 1.372(8) . ? C64 H64 0.9500 . ? C64 C65 1.380(8) . ? C65 H65 0.9500 . ? C65 C66 1.378(7) . ? C66 H66 0.9500 . ? U1 B4 2.923(6) 2_566 ? U1 B6 3.000(6) 2_666 ? C46 H46 0.9500 . ?