#------------------------------------------------------------------------------ #$Date: 2017-04-22 05:09:35 +0300 (Sat, 22 Apr 2017) $ #$Revision: 195681 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042749.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_7042749 loop_ _publ_author_name 'Kashid, Vitthal S.' 'Radhakrishna, Latchupatula' 'Balakrishna, Maravanji Shivaramaiah' _publ_section_title ; First examples of tri- and tetraphosphametacyclophanes: synthesis and isolation of an unusual hexapalladium complex containing pincer units with Pd---P covalent bonds ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00737J _journal_year 2017 _chemical_formula_moiety 'C56 H42 N4 O9 P4' _chemical_formula_sum 'C56 H42 N4 O9 P4' _chemical_formula_weight 1038.81 _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' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-09-24 deposited with the CCDC. 2017-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 97.725(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.9200(3) _cell_length_b 19.0391(8) _cell_length_c 20.9881(6) _cell_measurement_reflns_used 9587 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 72.6190 _cell_measurement_theta_min 3.1250 _cell_volume 5115.9(3) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.965 _diffrn_measurement_device_type 'Rigaku saturn 724' _diffrn_measurement_method \w _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1084 _diffrn_reflns_av_unetI/netI 0.1054 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.965 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 28013 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.965 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.767 _diffrn_reflns_theta_min 3.147 _exptl_absorpt_coefficient_mu 1.877 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.61938 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Numabs Rigaku 1999' _exptl_crystal_colour brown _exptl_crystal_density_diffrn 1.349 _exptl_crystal_description block _exptl_crystal_F_000 2152 _exptl_crystal_size_max 0.129 _exptl_crystal_size_mid 0.116 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.798 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.117 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 660 _refine_ls_number_reflns 9815 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.099 _refine_ls_R_factor_all 0.1322 _refine_ls_R_factor_gt 0.0819 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1449P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2069 _refine_ls_wR_factor_ref 0.2652 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6159 _reflns_number_total 9815 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00737j2.cif _cod_data_source_block MSB-VSK-292 _cod_database_code 7042749 _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_res_file ; msb-vsk-293-a_cu.res created by SHELXL-2014/7 TITL msb-vsk-293-a_cu_a.res in P2(1)/c REM Old TITL MSB-VSK-293-A_Cu in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.542, Rweak 0.126, Alpha 0.029, Orientation as input REM Formula found by SHELXT: C53 N5 O8 P4 CELL 1.54184 12.919977 19.039089 20.98807 90 97.7251 90 ZERR 4 0.000305 0.000769 0.000574 0 0.0022 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O P UNIT 224 168 16 36 16 L.S. 5 PLAN 50 TEMP -123.15 BOND $H LIST 6 MORE -1 CONF fmap 2 acta OMIT 0 4 5 OMIT 12 14 2 OMIT 12 12 7 OMIT 13 12 1 OMIT -2 16 2 OMIT 12 12 8 OMIT 4 3 4 OMIT 11 11 11 OMIT -11 16 2 OMIT 13 11 3 OMIT 12 11 6 OMIT 10 17 0 OMIT 13 11 5 OMIT -2 8 16 OMIT -4 18 2 OMIT -1 11 14 OMIT -14 11 4 OMIT 10 17 1 OMIT 11 12 9 OMIT -3 10 23 OMIT 4 1 2 OMIT 2 3 4 OMIT -1 11 13 OMIT 4 1 0 OMIT 3 2 3 OMIT -1 5 6 OMIT 3 4 3 OMIT 3 3 3 OMIT 5 0 0 OMIT -2 5 5 OMIT 4 2 2 OMIT -1 6 6 OMIT 5 1 2 OMIT 0 5 5 OMIT 2 4 4 OMIT 3 4 4 OMIT 0 5 4 OMIT 0 6 5 OMIT 5 1 1 OMIT 4 3 3 OMIT -1 5 5 OMIT 12 13 6 OMIT -1 5 4 OMIT -1 4 5 OMIT 0 5 6 OMIT 2 5 4 OMIT 4 1 1 OMIT -1 6 5 OMIT 5 0 2 OMIT 2 5 5 OMIT 4 3 2 OMIT 12 11 9 OMIT -1 9 16 OMIT 12 11 8 OMIT -2 6 5 OMIT 11 11 10 OMIT 1 4 25 OMIT 4 2 1 OMIT 11 16 0 OMIT 11 14 3 OMIT 13 11 4 OMIT -2 10 13 OMIT -2 9 14 OMIT -5 12 21 REM REM REM WGHT 0.144900 FVAR 0.34944 P4 5 0.128105 0.473095 0.229441 11.00000 0.02292 0.04727 = 0.02351 0.00027 0.00021 -0.00002 P2 5 0.485108 0.553940 0.333226 11.00000 0.01864 0.04557 = 0.02688 0.00075 -0.00268 0.00047 P3 5 0.214904 0.591030 0.429095 11.00000 0.01889 0.04705 = 0.02165 -0.00202 -0.00264 -0.00187 P1 5 0.353040 0.557000 0.098014 11.00000 0.02258 0.04578 = 0.02314 0.00024 -0.00110 -0.00023 O7 4 -0.034228 0.546518 0.162946 11.00000 0.02475 0.06163 = 0.02109 -0.00038 -0.00661 -0.00011 O3 4 0.549844 0.687233 0.366969 11.00000 0.02523 0.05021 = 0.03018 -0.00101 -0.00729 -0.00409 O2 4 0.180842 0.640489 0.099175 11.00000 0.02427 0.05616 = 0.02997 -0.00615 -0.00378 0.00245 O6 4 0.307481 0.713953 0.397109 11.00000 0.02632 0.04868 = 0.03407 -0.00025 -0.00360 -0.01066 O4 4 0.663225 0.519236 0.413662 11.00000 0.02142 0.05448 = 0.03731 0.00745 -0.00228 0.00527 O5 4 0.240357 0.650874 0.549515 11.00000 0.02505 0.06330 = 0.02565 -0.00847 -0.00117 -0.00065 O1 4 0.278260 0.551582 -0.030271 11.00000 0.04341 0.06353 = 0.02756 -0.00012 0.00350 -0.00988 O8 4 0.002760 0.365665 0.176651 11.00000 0.05712 0.06083 = 0.03065 -0.00330 0.00811 -0.02292 N1 3 0.384946 0.644876 0.224546 11.00000 0.01718 0.04727 = 0.02517 0.00428 -0.00110 -0.00010 N4 3 0.153599 0.474130 0.090899 11.00000 0.02433 0.03709 = 0.02563 -0.00264 -0.00298 -0.00159 N3 3 0.140257 0.614686 0.289475 11.00000 0.01922 0.04798 = 0.01936 0.00152 -0.00061 0.00072 N2 3 0.438266 0.591463 0.463455 11.00000 0.01745 0.04487 = 0.02598 0.00434 -0.00463 -0.00152 O9 4 0.354456 0.297217 0.276203 11.00000 0.03983 0.07816 = 0.05450 -0.00689 -0.00115 0.00460 C47 1 0.428212 0.686166 0.272024 11.00000 0.01633 0.04021 = 0.02271 0.00021 -0.00153 -0.00105 C39 1 0.578858 0.548625 0.410317 11.00000 0.01779 0.03159 = 0.03710 0.00093 -0.00234 -0.00176 C11 1 0.016884 0.395184 0.046625 11.00000 0.02293 0.04563 = 0.02937 0.00064 -0.00226 0.00237 AFIX 43 H11 2 -0.037591 0.363910 0.053939 11.00000 -1.20000 AFIX 0 C22 1 0.029544 0.681064 0.210304 11.00000 0.02225 0.04030 = 0.02675 0.00122 -0.00223 0.00348 AFIX 43 H22 2 -0.021142 0.680906 0.173052 11.00000 -1.20000 AFIX 0 C52 1 0.269535 0.629204 0.124324 11.00000 0.02227 0.04850 = 0.02096 0.00315 0.00141 -0.00394 C13 1 0.057041 0.415014 0.165107 11.00000 0.02871 0.04079 = 0.03048 -0.00073 0.00314 0.00103 C9 1 0.118691 0.453638 -0.023343 11.00000 0.02260 0.05210 = 0.02428 -0.00250 -0.00222 0.00738 AFIX 43 H9 2 0.135806 0.463147 -0.065117 11.00000 -1.20000 AFIX 0 C34 1 0.400761 0.615898 0.515258 11.00000 0.02142 0.04070 = 0.02764 -0.00789 -0.00119 -0.00183 C7 1 0.262407 0.534145 0.022839 11.00000 0.02528 0.04393 = 0.02420 -0.00048 0.00184 0.00388 C23 1 0.062312 0.743157 0.240048 11.00000 0.03196 0.03969 = 0.02603 0.00776 0.00105 0.01010 AFIX 43 H23 2 0.035018 0.786781 0.223448 11.00000 -1.20000 AFIX 0 C12 1 0.076397 0.429228 0.097614 11.00000 0.02491 0.04337 = 0.02626 -0.00213 -0.00096 0.00299 C32 1 0.006987 0.561983 0.430252 11.00000 0.02687 0.04194 = 0.02890 -0.00011 0.00277 -0.00454 AFIX 43 H32 2 0.029684 0.514744 0.427570 11.00000 -1.20000 AFIX 0 C1 1 0.444093 0.611366 0.059663 11.00000 0.02205 0.04379 = 0.02812 0.00392 0.00121 0.00424 C21 1 0.072058 0.619078 0.235878 11.00000 0.01732 0.04554 = 0.02362 -0.00268 -0.00058 -0.00264 C8 1 0.173879 0.485683 0.030976 11.00000 0.02286 0.04599 = 0.01947 -0.00018 -0.00369 0.00582 C25 1 0.171293 0.675290 0.317820 11.00000 0.02171 0.04527 = 0.02075 -0.00364 0.00124 -0.00069 C38 1 0.541000 0.577152 0.469226 11.00000 0.01778 0.04514 = 0.03006 0.00342 -0.00380 -0.00098 C20 1 0.040910 0.550964 0.204197 11.00000 0.02382 0.05157 = 0.01986 -0.00003 0.00366 0.00121 C28 1 0.044996 0.684305 0.440835 11.00000 0.02298 0.04190 = 0.03627 -0.00176 -0.00181 -0.00280 AFIX 43 H28 2 0.094382 0.721511 0.446391 11.00000 -1.20000 AFIX 0 C27 1 0.078857 0.616002 0.435392 11.00000 0.02553 0.04666 = 0.02011 0.00397 -0.00305 -0.00239 C35 1 0.462061 0.627512 0.573369 11.00000 0.02764 0.04619 = 0.03168 -0.00051 -0.00360 -0.00372 AFIX 43 H35 2 0.432147 0.645194 0.609085 11.00000 -1.20000 AFIX 0 C29 1 -0.060953 0.698911 0.438228 11.00000 0.02909 0.04173 = 0.03815 0.00304 0.00513 0.00936 AFIX 43 H29 2 -0.084158 0.746071 0.440586 11.00000 -1.20000 AFIX 0 C46 1 0.495201 0.651897 0.327106 11.00000 0.01799 0.05017 = 0.02434 0.00191 0.00063 0.00090 C24 1 0.135950 0.740991 0.294739 11.00000 0.02752 0.04639 = 0.02440 -0.00435 0.00078 -0.00023 AFIX 43 H24 2 0.161462 0.782944 0.315779 11.00000 -1.20000 AFIX 0 C14 1 0.065868 0.439436 0.295774 11.00000 0.02470 0.04204 = 0.02554 -0.00095 -0.00112 -0.00050 C19 1 -0.041279 0.441300 0.298816 11.00000 0.02528 0.04290 = 0.02502 -0.00297 -0.00011 -0.00107 AFIX 43 H19 2 -0.086057 0.464943 0.266081 11.00000 -1.20000 AFIX 0 C26 1 0.242956 0.669908 0.380802 11.00000 0.01822 0.04922 = 0.02717 -0.00364 0.00271 0.00079 C10 1 0.038934 0.407962 -0.014729 11.00000 0.02318 0.05202 = 0.02817 -0.00644 -0.00764 0.00306 AFIX 43 H10 2 -0.000276 0.385610 -0.050617 11.00000 -1.20000 AFIX 0 C40 1 0.573733 0.528341 0.275929 11.00000 0.02978 0.04950 = 0.02732 0.00496 -0.00053 0.01235 C51 1 0.320128 0.674866 0.177259 11.00000 0.01817 0.04449 = 0.02218 -0.00182 0.00050 -0.00097 C2 1 0.416186 0.673227 0.025646 11.00000 0.02313 0.05165 = 0.03262 -0.00153 0.00109 -0.00391 AFIX 43 H2 2 0.347512 0.691330 0.024888 11.00000 -1.20000 AFIX 0 C37 1 0.607766 0.586929 0.526162 11.00000 0.02025 0.05043 = 0.03577 0.00347 -0.00705 -0.00118 AFIX 43 H37 2 0.679884 0.575801 0.528724 11.00000 -1.20000 AFIX 0 C50 1 0.297919 0.745829 0.175014 11.00000 0.02590 0.05035 = 0.02156 0.00128 -0.00086 0.00281 AFIX 43 H50 2 0.250050 0.764642 0.140972 11.00000 -1.20000 AFIX 0 C17 1 -0.019332 0.373707 0.396455 11.00000 0.04270 0.05185 = 0.02682 -0.00114 0.00516 -0.00386 AFIX 43 H17 2 -0.047965 0.350954 0.430386 11.00000 -1.20000 AFIX 0 C41 1 0.670201 0.561718 0.273685 11.00000 0.02659 0.05651 = 0.04141 0.00924 0.00083 0.00773 AFIX 43 H41 2 0.692214 0.598565 0.302914 11.00000 -1.20000 AFIX 0 C48 1 0.413102 0.758907 0.272970 11.00000 0.02201 0.04892 = 0.03097 -0.00287 -0.00245 -0.00586 AFIX 43 H48 2 0.447564 0.786884 0.306851 11.00000 -1.20000 AFIX 0 C36 1 0.567429 0.613035 0.578752 11.00000 0.02768 0.05468 = 0.03281 0.00102 -0.01196 0.00139 AFIX 43 H36 2 0.611433 0.620958 0.618123 11.00000 -1.20000 AFIX 0 C15 1 0.129312 0.404731 0.344637 11.00000 0.02848 0.06264 = 0.02710 0.00087 -0.00091 0.00536 AFIX 43 H15 2 0.202711 0.403606 0.344144 11.00000 -1.20000 AFIX 0 C18 1 -0.083565 0.409367 0.348605 11.00000 0.02817 0.05507 = 0.03253 -0.00556 0.00140 -0.00244 AFIX 43 H18 2 -0.156637 0.411801 0.350116 11.00000 -1.20000 AFIX 0 C30 1 -0.132398 0.644359 0.432180 11.00000 0.02198 0.06663 = 0.03819 -0.00121 -0.00066 0.00332 AFIX 43 H30 2 -0.204868 0.654101 0.430246 11.00000 -1.20000 AFIX 0 C33 1 0.283862 0.626384 0.507423 11.00000 0.02121 0.04934 = 0.03001 -0.00192 -0.00063 -0.00415 C49 1 0.346189 0.789204 0.222915 11.00000 0.02784 0.06055 = 0.03120 0.00117 0.00118 0.00336 AFIX 43 H49 2 0.334007 0.838423 0.221701 11.00000 -1.20000 AFIX 0 C3 1 0.486190 0.708357 -0.006720 11.00000 0.03109 0.05199 = 0.03497 0.00005 0.00053 0.00371 AFIX 43 H3 2 0.466021 0.750204 -0.029753 11.00000 -1.20000 AFIX 0 C16 1 0.087243 0.371976 0.393723 11.00000 0.03821 0.05209 = 0.02758 -0.00355 -0.00080 0.00772 AFIX 43 H16 2 0.131903 0.347845 0.426184 11.00000 -1.20000 AFIX 0 C43 1 0.703281 0.486776 0.187329 11.00000 0.04999 0.07794 = 0.03426 0.00130 0.00972 0.02660 AFIX 43 H43 2 0.747952 0.472033 0.157449 11.00000 -1.20000 AFIX 0 C42 1 0.732941 0.540694 0.228748 11.00000 0.03089 0.09066 = 0.04665 0.01902 0.01132 0.01950 AFIX 43 H42 2 0.797405 0.564009 0.226652 11.00000 -1.20000 AFIX 0 C31 1 -0.099099 0.576808 0.428996 11.00000 0.02481 0.06319 = 0.04345 -0.00948 0.00498 -0.00504 AFIX 43 H31 2 -0.148343 0.539498 0.425900 11.00000 -1.20000 AFIX 0 C4 1 0.586078 0.682135 -0.005364 11.00000 0.03313 0.05665 = 0.04815 0.00333 0.01662 0.00058 AFIX 43 H4 2 0.635025 0.706029 -0.027534 11.00000 -1.20000 AFIX 0 C6 1 0.543367 0.586532 0.060107 11.00000 0.02810 0.05455 = 0.06090 0.01019 0.00633 0.01084 AFIX 43 H6 2 0.563931 0.544543 0.082799 11.00000 -1.20000 AFIX 0 C44 1 0.608736 0.453723 0.188784 11.00000 0.06887 0.06139 = 0.03095 -0.00147 -0.00513 0.02529 AFIX 43 H44 2 0.587973 0.416473 0.159743 11.00000 -1.20000 AFIX 0 C54 1 0.287867 0.290568 0.217191 11.00000 0.03922 0.07677 = 0.04858 -0.01093 -0.00411 0.01104 AFIX 23 H54A 2 0.214365 0.297142 0.224494 11.00000 -1.20000 H54B 2 0.294811 0.242881 0.199444 11.00000 -1.20000 AFIX 0 C53 1 0.315430 0.343708 0.170657 11.00000 0.04943 0.10242 = 0.05405 -0.00399 0.00388 0.02729 AFIX 137 H53A 2 0.311863 0.390736 0.189219 11.00000 -1.50000 H53B 2 0.266197 0.340608 0.130940 11.00000 -1.50000 H53C 2 0.386450 0.334909 0.161051 11.00000 -1.50000 AFIX 0 C56 1 0.255278 0.219725 0.338252 11.00000 0.06330 0.09954 = 0.10929 0.00825 0.03483 0.01858 AFIX 137 H56A 2 0.237955 0.256713 0.367523 11.00000 -1.50000 H56B 2 0.260062 0.174523 0.360792 11.00000 -1.50000 H56C 2 0.200675 0.217215 0.301089 11.00000 -1.50000 AFIX 0 C45 1 0.543392 0.475181 0.233162 11.00000 0.04411 0.04800 = 0.03302 0.00343 -0.00204 0.01138 AFIX 43 H45 2 0.477736 0.452893 0.233730 11.00000 -1.20000 AFIX 0 C55 1 0.357406 0.236036 0.315971 11.00000 0.05054 0.07094 = 0.05454 -0.00447 0.00163 0.00668 AFIX 23 H55A 2 0.410694 0.242909 0.353988 11.00000 -1.20000 H55B 2 0.379181 0.195311 0.291624 11.00000 -1.20000 AFIX 0 C5 1 0.614701 0.621946 0.027760 11.00000 0.03151 0.07398 = 0.07288 0.01982 0.01885 0.01534 AFIX 43 H5 2 0.683612 0.604198 0.028709 11.00000 -1.20000 AFIX 0 HKLF 4 REM msb-vsk-293-a_cu_a.res in P2(1)/c REM R1 = 0.0819 for 6159 Fo > 4sig(Fo) and 0.1322 for all 9815 data REM 660 parameters refined using 0 restraints END WGHT 0.1449 0.0000 REM Highest difference peak 0.798, deepest hole -0.797, 1-sigma level 0.117 Q1 1 0.1192 0.4372 0.2704 11.00000 0.05 0.80 Q2 1 0.5552 0.5580 0.3045 11.00000 0.05 0.64 Q3 1 0.4139 0.5597 0.0673 11.00000 0.05 0.62 Q4 1 0.2318 0.6253 0.3945 11.00000 0.05 0.60 Q5 1 0.5018 0.5212 0.2992 11.00000 0.05 0.59 Q6 1 0.5007 0.5945 0.2983 11.00000 0.05 0.56 Q7 1 0.4418 0.6013 0.3276 11.00000 0.05 0.55 Q8 1 0.0718 0.4806 0.2611 11.00000 0.05 0.54 Q9 1 0.1360 0.4362 0.1916 11.00000 0.05 0.53 Q10 1 0.1989 0.4784 0.2021 11.00000 0.05 0.53 Q11 1 0.3171 0.5921 0.1278 11.00000 0.05 0.53 Q12 1 0.0785 0.5201 0.2188 11.00000 0.05 0.52 Q13 1 0.3387 0.5210 0.1367 11.00000 0.05 0.52 Q14 1 0.4043 0.6024 0.0946 11.00000 0.05 0.52 Q15 1 0.1156 0.5091 0.2782 11.00000 0.05 0.51 Q16 1 0.2595 0.6420 0.4313 11.00000 0.05 0.49 Q17 1 0.2942 0.6035 0.0918 11.00000 0.05 0.49 Q18 1 0.4770 0.5186 0.3763 11.00000 0.05 0.49 Q19 1 0.2318 0.5594 0.3884 11.00000 0.05 0.48 Q20 1 0.1999 0.5528 0.4684 11.00000 0.05 0.47 Q21 1 0.2987 0.5577 0.0448 11.00000 0.05 0.47 Q22 1 0.2790 0.5855 0.3943 11.00000 0.05 0.46 Q23 1 0.3623 0.5206 0.0579 11.00000 0.05 0.45 Q24 1 0.2986 0.5154 0.0808 11.00000 0.05 0.45 Q25 1 0.1631 0.6757 0.1275 11.00000 0.05 0.44 Q26 1 0.1864 0.4222 0.2366 11.00000 0.05 0.43 Q27 1 0.1895 0.4844 0.2770 11.00000 0.05 0.43 Q28 1 0.5413 0.5626 0.3804 11.00000 0.05 0.43 Q29 1 0.0129 0.5631 0.2223 11.00000 0.05 0.43 Q30 1 0.1371 0.5106 0.1918 11.00000 0.05 0.43 Q31 1 0.1847 0.4424 0.0111 11.00000 0.05 0.42 Q32 1 0.6754 0.4792 0.3851 11.00000 0.05 0.42 Q33 1 0.4236 0.5992 0.2324 11.00000 0.05 0.42 Q34 1 0.0415 0.4018 0.0536 11.00000 0.05 0.42 Q35 1 0.6577 0.5540 0.3801 11.00000 0.05 0.41 Q36 1 0.2210 0.6245 0.4759 11.00000 0.05 0.41 Q37 1 0.4157 0.5528 0.3648 11.00000 0.05 0.40 Q38 1 0.4262 0.5527 0.2835 11.00000 0.05 0.40 Q39 1 0.4644 0.5968 0.3615 11.00000 0.05 0.40 Q40 1 0.4367 0.5123 0.3204 11.00000 0.05 0.40 Q41 1 0.4018 0.5546 0.1495 11.00000 0.05 0.39 Q42 1 0.2921 0.2536 0.2628 11.00000 0.05 0.39 Q43 1 0.0867 0.4530 0.1187 11.00000 0.05 0.39 Q44 1 0.0390 0.5298 0.1402 11.00000 0.05 0.39 Q45 1 0.5044 0.5789 0.3878 11.00000 0.05 0.38 Q46 1 0.5593 0.5133 0.2019 11.00000 0.05 0.38 Q47 1 0.0735 0.3836 0.1436 11.00000 0.05 0.38 Q48 1 0.0602 0.4495 0.1249 11.00000 0.05 0.37 Q49 1 0.4104 0.5133 0.1069 11.00000 0.05 0.37 Q50 1 0.1446 0.5583 0.3303 11.00000 0.05 0.37 ; _shelx_res_checksum 20955 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 P4 P 0.12810(7) 0.47309(7) 0.22944(5) 0.0315(3) Uani 1 1 d . . P2 P 0.48511(7) 0.55394(7) 0.33323(5) 0.0309(3) Uani 1 1 d . . P3 P 0.21490(7) 0.59103(7) 0.42909(5) 0.0297(3) Uani 1 1 d . . P1 P 0.35304(7) 0.55700(7) 0.09801(5) 0.0309(3) Uani 1 1 d . . O7 O -0.0342(2) 0.54652(19) 0.16295(13) 0.0367(8) Uani 1 1 d . . O3 O 0.5498(2) 0.68723(18) 0.36697(14) 0.0362(8) Uani 1 1 d . . O2 O 0.1808(2) 0.64049(18) 0.09918(14) 0.0375(8) Uani 1 1 d . . O6 O 0.3075(2) 0.71395(18) 0.39711(14) 0.0371(8) Uani 1 1 d . . O4 O 0.66323(19) 0.51924(18) 0.41366(14) 0.0383(8) Uani 1 1 d . . O5 O 0.24036(19) 0.65087(19) 0.54952(13) 0.0384(8) Uani 1 1 d . . O1 O 0.2783(2) 0.5516(2) -0.03027(15) 0.0449(9) Uani 1 1 d . . O8 O 0.0028(3) 0.3657(2) 0.17665(15) 0.0493(9) Uani 1 1 d . . N1 N 0.3849(2) 0.6449(2) 0.22455(15) 0.0302(9) Uani 1 1 d . . N4 N 0.1536(2) 0.4741(2) 0.09090(16) 0.0296(8) Uani 1 1 d . . N3 N 0.1403(2) 0.6147(2) 0.28947(15) 0.0291(8) Uani 1 1 d . . N2 N 0.4383(2) 0.5915(2) 0.46346(16) 0.0301(9) Uani 1 1 d . . O9 O 0.3545(2) 0.2972(2) 0.27620(18) 0.0582(11) Uani 1 1 d . . C47 C 0.4282(3) 0.6862(2) 0.27202(18) 0.0268(9) Uani 1 1 d . . C39 C 0.5789(3) 0.5486(2) 0.4103(2) 0.0294(10) Uani 1 1 d . . C11 C 0.0169(3) 0.3952(3) 0.0466(2) 0.0332(11) Uani 1 1 d . . H11 H -0.0376 0.3639 0.0539 0.040 Uiso 1 1 calc R U C22 C 0.0295(3) 0.6811(3) 0.2103(2) 0.0303(10) Uani 1 1 d . . H22 H -0.0211 0.6809 0.1731 0.036 Uiso 1 1 calc R U C52 C 0.2695(3) 0.6292(3) 0.12432(18) 0.0307(10) Uani 1 1 d . . C13 C 0.0570(3) 0.4150(3) 0.1651(2) 0.0334(10) Uani 1 1 d . . C9 C 0.1187(3) 0.4536(3) -0.0233(2) 0.0335(11) Uani 1 1 d . . H9 H 0.1358 0.4631 -0.0651 0.040 Uiso 1 1 calc R U C34 C 0.4008(3) 0.6159(2) 0.51526(19) 0.0303(10) Uani 1 1 d . . C7 C 0.2624(3) 0.5341(3) 0.02284(19) 0.0313(10) Uani 1 1 d . . C23 C 0.0623(3) 0.7432(3) 0.2400(2) 0.0328(10) Uani 1 1 d . . H23 H 0.0350 0.7868 0.2234 0.039 Uiso 1 1 calc R U C12 C 0.0764(3) 0.4292(3) 0.0976(2) 0.0319(10) Uani 1 1 d . . C32 C 0.0070(3) 0.5620(3) 0.43025(19) 0.0327(10) Uani 1 1 d . . H32 H 0.0297 0.5147 0.4276 0.039 Uiso 1 1 calc R U C1 C 0.4441(3) 0.6114(3) 0.0597(2) 0.0315(10) Uani 1 1 d . . C21 C 0.0721(3) 0.6191(3) 0.23588(19) 0.0291(10) Uani 1 1 d . . C8 C 0.1739(3) 0.4857(3) 0.03098(18) 0.0300(10) Uani 1 1 d . . C25 C 0.1713(3) 0.6753(3) 0.31782(19) 0.0294(10) Uani 1 1 d . . C38 C 0.5410(3) 0.5772(3) 0.4692(2) 0.0316(10) Uani 1 1 d . . C20 C 0.0409(3) 0.5510(3) 0.20420(19) 0.0317(11) Uani 1 1 d . . C28 C 0.0450(3) 0.6843(3) 0.4408(2) 0.0342(10) Uani 1 1 d . . H28 H 0.0944 0.7215 0.4464 0.041 Uiso 1 1 calc R U C27 C 0.0789(3) 0.6160(3) 0.43539(18) 0.0313(10) Uani 1 1 d . . C35 C 0.4621(3) 0.6275(3) 0.5734(2) 0.0359(11) Uani 1 1 d . . H35 H 0.4321 0.6452 0.6091 0.043 Uiso 1 1 calc R U C29 C -0.0610(3) 0.6989(3) 0.4382(2) 0.0363(11) Uani 1 1 d . . H29 H -0.0842 0.7461 0.4406 0.044 Uiso 1 1 calc R U C46 C 0.4952(3) 0.6519(3) 0.32711(19) 0.0310(10) Uani 1 1 d . . C24 C 0.1360(3) 0.7410(3) 0.29474(19) 0.0330(10) Uani 1 1 d . . H24 H 0.1615 0.7829 0.3158 0.040 Uiso 1 1 calc R U C14 C 0.0659(3) 0.4394(3) 0.2958(2) 0.0312(10) Uani 1 1 d . . C19 C -0.0413(3) 0.4413(3) 0.2988(2) 0.0314(10) Uani 1 1 d . . H19 H -0.0861 0.4649 0.2661 0.038 Uiso 1 1 calc R U C26 C 0.2430(3) 0.6699(3) 0.38080(19) 0.0316(10) Uani 1 1 d . . C10 C 0.0389(3) 0.4080(3) -0.0147(2) 0.0355(11) Uani 1 1 d . . H10 H -0.0003 0.3856 -0.0506 0.043 Uiso 1 1 calc R U C40 C 0.5737(3) 0.5283(3) 0.2759(2) 0.0359(11) Uani 1 1 d . . C51 C 0.3201(3) 0.6749(3) 0.17726(18) 0.0285(10) Uani 1 1 d . . C2 C 0.4162(3) 0.6732(3) 0.0256(2) 0.0360(11) Uani 1 1 d . . H2 H 0.3475 0.6913 0.0249 0.043 Uiso 1 1 calc R U C37 C 0.6078(3) 0.5869(3) 0.5262(2) 0.0365(11) Uani 1 1 d . . H37 H 0.6799 0.5758 0.5287 0.044 Uiso 1 1 calc R U C50 C 0.2979(3) 0.7458(3) 0.17501(19) 0.0330(11) Uani 1 1 d . . H50 H 0.2500 0.7646 0.1410 0.040 Uiso 1 1 calc R U C17 C -0.0193(3) 0.3737(3) 0.3965(2) 0.0404(12) Uani 1 1 d . . H17 H -0.0480 0.3510 0.4304 0.048 Uiso 1 1 calc R U C41 C 0.6702(3) 0.5617(3) 0.2737(2) 0.0418(12) Uani 1 1 d . . H41 H 0.6922 0.5986 0.3029 0.050 Uiso 1 1 calc R U C48 C 0.4131(3) 0.7589(3) 0.2730(2) 0.0345(11) Uani 1 1 d . . H48 H 0.4476 0.7869 0.3069 0.041 Uiso 1 1 calc R U C36 C 0.5674(3) 0.6130(3) 0.5788(2) 0.0399(12) Uani 1 1 d . . H36 H 0.6114 0.6210 0.6181 0.048 Uiso 1 1 calc R U C15 C 0.1293(3) 0.4047(3) 0.3446(2) 0.0398(12) Uani 1 1 d . . H15 H 0.2027 0.4036 0.3441 0.048 Uiso 1 1 calc R U C18 C -0.0836(3) 0.4094(3) 0.3486(2) 0.0388(12) Uani 1 1 d . . H18 H -0.1566 0.4118 0.3501 0.047 Uiso 1 1 calc R U C30 C -0.1324(3) 0.6444(3) 0.4322(2) 0.0427(13) Uani 1 1 d . . H30 H -0.2049 0.6541 0.4302 0.051 Uiso 1 1 calc R U C33 C 0.2839(3) 0.6264(3) 0.5074(2) 0.0339(11) Uani 1 1 d . . C49 C 0.3462(3) 0.7892(3) 0.2229(2) 0.0401(12) Uani 1 1 d . . H49 H 0.3340 0.8384 0.2217 0.048 Uiso 1 1 calc R U C3 C 0.4862(3) 0.7084(3) -0.0067(2) 0.0397(12) Uani 1 1 d . . H3 H 0.4660 0.7502 -0.0298 0.048 Uiso 1 1 calc R U C16 C 0.0872(3) 0.3720(3) 0.3937(2) 0.0398(12) Uani 1 1 d . . H16 H 0.1319 0.3478 0.4262 0.048 Uiso 1 1 calc R U C43 C 0.7033(4) 0.4868(3) 0.1873(2) 0.0537(15) Uani 1 1 d . . H43 H 0.7480 0.4720 0.1574 0.064 Uiso 1 1 calc R U C42 C 0.7329(4) 0.5407(4) 0.2287(3) 0.0555(16) Uani 1 1 d . . H42 H 0.7974 0.5640 0.2267 0.067 Uiso 1 1 calc R U C31 C -0.0991(3) 0.5768(3) 0.4290(2) 0.0438(13) Uani 1 1 d . . H31 H -0.1483 0.5395 0.4259 0.053 Uiso 1 1 calc R U C4 C 0.5861(3) 0.6821(3) -0.0054(2) 0.0450(13) Uani 1 1 d . . H4 H 0.6350 0.7060 -0.0275 0.054 Uiso 1 1 calc R U C6 C 0.5434(3) 0.5865(3) 0.0601(3) 0.0478(13) Uani 1 1 d . . H6 H 0.5639 0.5445 0.0828 0.057 Uiso 1 1 calc R U C44 C 0.6087(4) 0.4537(3) 0.1888(2) 0.0548(15) Uani 1 1 d . . H44 H 0.5880 0.4165 0.1597 0.066 Uiso 1 1 calc R U C54 C 0.2879(4) 0.2906(4) 0.2172(3) 0.0558(16) Uani 1 1 d . . H54A H 0.2144 0.2971 0.2245 0.067 Uiso 1 1 calc R U H54B H 0.2948 0.2429 0.1994 0.067 Uiso 1 1 calc R U C53 C 0.3154(4) 0.3437(4) 0.1707(3) 0.0689(19) Uani 1 1 d . . H53A H 0.3119 0.3907 0.1892 0.103 Uiso 1 1 calc R U H53B H 0.2662 0.3406 0.1309 0.103 Uiso 1 1 calc R U H53C H 0.3864 0.3349 0.1611 0.103 Uiso 1 1 calc R U C56 C 0.2553(5) 0.2197(4) 0.3383(4) 0.089(2) Uani 1 1 d . . H56A H 0.2380 0.2567 0.3675 0.133 Uiso 1 1 calc R U H56B H 0.2601 0.1745 0.3608 0.133 Uiso 1 1 calc R U H56C H 0.2007 0.2172 0.3011 0.133 Uiso 1 1 calc R U C45 C 0.5434(4) 0.4752(3) 0.2332(2) 0.0424(12) Uani 1 1 d . . H45 H 0.4777 0.4529 0.2337 0.051 Uiso 1 1 calc R U C55 C 0.3574(4) 0.2360(4) 0.3160(3) 0.0592(16) Uani 1 1 d . . H55A H 0.4107 0.2429 0.3540 0.071 Uiso 1 1 calc R U H55B H 0.3792 0.1953 0.2916 0.071 Uiso 1 1 calc R U C5 C 0.6147(4) 0.6219(3) 0.0278(3) 0.0584(16) Uani 1 1 d . . H5 H 0.6836 0.6042 0.0287 0.070 Uiso 1 1 calc R U 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 P4 0.0229(5) 0.0473(8) 0.0235(5) 0.0003(5) 0.0002(4) 0.0000(4) P2 0.0186(5) 0.0456(8) 0.0269(6) 0.0008(5) -0.0027(4) 0.0005(4) P3 0.0189(5) 0.0471(8) 0.0217(5) -0.0020(5) -0.0026(4) -0.0019(4) P1 0.0226(5) 0.0458(8) 0.0231(5) 0.0002(5) -0.0011(4) -0.0002(4) O7 0.0247(13) 0.062(2) 0.0211(14) -0.0004(15) -0.0066(11) -0.0001(13) O3 0.0252(13) 0.050(2) 0.0302(16) -0.0010(15) -0.0073(11) -0.0041(13) O2 0.0243(13) 0.056(2) 0.0300(15) -0.0061(16) -0.0038(11) 0.0025(13) O6 0.0263(14) 0.049(2) 0.0341(16) -0.0003(16) -0.0036(12) -0.0107(14) O4 0.0214(13) 0.054(2) 0.0373(17) 0.0074(16) -0.0023(11) 0.0053(13) O5 0.0251(13) 0.063(2) 0.0256(15) -0.0085(16) -0.0012(11) -0.0007(14) O1 0.0434(17) 0.064(3) 0.0276(16) -0.0001(17) 0.0035(13) -0.0099(16) O8 0.0571(19) 0.061(3) 0.0307(17) -0.0033(17) 0.0081(15) -0.0229(18) N1 0.0172(14) 0.047(3) 0.0252(17) 0.0043(17) -0.0011(12) -0.0001(14) N4 0.0243(15) 0.037(2) 0.0256(17) -0.0026(17) -0.0030(13) -0.0016(15) N3 0.0192(14) 0.048(3) 0.0194(16) 0.0015(17) -0.0006(12) 0.0007(15) N2 0.0174(14) 0.045(3) 0.0260(18) 0.0043(17) -0.0046(12) -0.0015(14) O9 0.0398(18) 0.078(3) 0.054(2) -0.007(2) -0.0011(16) 0.0046(18) C47 0.0163(16) 0.040(3) 0.0227(19) 0.0002(19) -0.0015(14) -0.0011(16) C39 0.0178(17) 0.032(3) 0.037(2) 0.001(2) -0.0023(15) -0.0018(16) C11 0.0229(18) 0.046(3) 0.029(2) 0.001(2) -0.0023(15) 0.0024(18) C22 0.0222(17) 0.040(3) 0.027(2) 0.001(2) -0.0022(15) 0.0035(17) C52 0.0223(18) 0.049(3) 0.0210(19) 0.003(2) 0.0014(14) -0.0039(18) C13 0.0287(19) 0.041(3) 0.030(2) -0.001(2) 0.0031(16) 0.0010(19) C9 0.0226(18) 0.052(3) 0.024(2) -0.002(2) -0.0022(15) 0.0074(19) C34 0.0214(18) 0.041(3) 0.028(2) -0.008(2) -0.0012(15) -0.0018(17) C7 0.0253(18) 0.044(3) 0.024(2) 0.000(2) 0.0018(15) 0.0039(18) C23 0.032(2) 0.040(3) 0.026(2) 0.008(2) 0.0011(16) 0.0101(19) C12 0.0249(18) 0.043(3) 0.026(2) -0.002(2) -0.0010(15) 0.0030(18) C32 0.0269(19) 0.042(3) 0.029(2) 0.000(2) 0.0028(16) -0.0045(18) C1 0.0220(18) 0.044(3) 0.028(2) 0.004(2) 0.0012(15) 0.0042(18) C21 0.0173(16) 0.046(3) 0.024(2) -0.003(2) -0.0006(14) -0.0026(17) C8 0.0229(17) 0.046(3) 0.0195(19) 0.000(2) -0.0037(14) 0.0058(18) C25 0.0217(17) 0.045(3) 0.0207(19) -0.004(2) 0.0012(14) -0.0007(18) C38 0.0178(17) 0.045(3) 0.030(2) 0.003(2) -0.0038(15) -0.0010(17) C20 0.0238(18) 0.052(3) 0.0199(19) 0.000(2) 0.0037(15) 0.0012(18) C28 0.0230(18) 0.042(3) 0.036(2) -0.002(2) -0.0018(16) -0.0028(18) C27 0.0255(18) 0.047(3) 0.0201(19) 0.004(2) -0.0030(15) -0.0024(19) C35 0.0276(19) 0.046(3) 0.032(2) -0.001(2) -0.0036(16) -0.0037(19) C29 0.029(2) 0.042(3) 0.038(2) 0.003(2) 0.0051(17) 0.0094(19) C46 0.0180(16) 0.050(3) 0.024(2) 0.002(2) 0.0006(14) 0.0009(18) C24 0.0275(19) 0.046(3) 0.024(2) -0.004(2) 0.0008(15) -0.0002(19) C14 0.0247(18) 0.042(3) 0.026(2) -0.001(2) -0.0011(15) -0.0005(18) C19 0.0253(18) 0.043(3) 0.025(2) -0.003(2) -0.0001(15) -0.0011(18) C26 0.0182(17) 0.049(3) 0.027(2) -0.004(2) 0.0027(14) 0.0008(18) C10 0.0232(19) 0.052(3) 0.028(2) -0.006(2) -0.0076(16) 0.0031(19) C40 0.030(2) 0.049(3) 0.027(2) 0.005(2) -0.0005(16) 0.0123(19) C51 0.0182(16) 0.044(3) 0.0222(19) -0.002(2) 0.0005(14) -0.0010(17) C2 0.0231(18) 0.052(3) 0.033(2) -0.002(2) 0.0011(16) -0.0039(19) C37 0.0203(18) 0.050(3) 0.036(2) 0.003(2) -0.0070(16) -0.0012(19) C50 0.0259(18) 0.050(3) 0.022(2) 0.001(2) -0.0009(15) 0.0028(19) C17 0.043(2) 0.052(3) 0.027(2) -0.001(2) 0.0052(18) -0.004(2) C41 0.027(2) 0.057(4) 0.041(3) 0.009(3) 0.0008(18) 0.008(2) C48 0.0220(18) 0.049(3) 0.031(2) -0.003(2) -0.0025(15) -0.0059(19) C36 0.028(2) 0.055(3) 0.033(2) 0.001(2) -0.0120(17) 0.001(2) C15 0.028(2) 0.063(4) 0.027(2) 0.001(2) -0.0009(17) 0.005(2) C18 0.028(2) 0.055(4) 0.033(2) -0.006(2) 0.0014(17) -0.002(2) C30 0.0220(19) 0.067(4) 0.038(3) -0.001(3) -0.0007(17) 0.003(2) C33 0.0212(18) 0.049(3) 0.030(2) -0.002(2) -0.0006(16) -0.0042(18) C49 0.028(2) 0.061(4) 0.031(2) 0.001(2) 0.0012(17) 0.003(2) C3 0.031(2) 0.052(3) 0.035(2) 0.000(2) 0.0005(17) 0.004(2) C16 0.038(2) 0.052(3) 0.028(2) -0.004(2) -0.0008(17) 0.008(2) C43 0.050(3) 0.078(5) 0.034(3) 0.001(3) 0.010(2) 0.027(3) C42 0.031(2) 0.091(5) 0.047(3) 0.019(3) 0.011(2) 0.019(3) C31 0.025(2) 0.063(4) 0.043(3) -0.009(3) 0.0050(18) -0.005(2) C4 0.033(2) 0.057(4) 0.048(3) 0.003(3) 0.017(2) 0.001(2) C6 0.028(2) 0.055(4) 0.061(3) 0.010(3) 0.006(2) 0.011(2) C44 0.069(3) 0.061(4) 0.031(3) -0.001(3) -0.005(2) 0.025(3) C54 0.039(3) 0.077(5) 0.049(3) -0.011(3) -0.004(2) 0.011(3) C53 0.049(3) 0.102(6) 0.054(3) -0.004(4) 0.004(3) 0.027(3) C56 0.063(4) 0.100(6) 0.109(6) 0.008(5) 0.035(4) 0.019(4) C45 0.044(2) 0.048(3) 0.033(2) 0.003(2) -0.0020(19) 0.011(2) C55 0.051(3) 0.071(5) 0.055(3) -0.004(3) 0.002(2) 0.007(3) C5 0.032(2) 0.074(4) 0.073(4) 0.020(3) 0.019(2) 0.015(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 '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 C14 P4 C13 96.8(2) C14 P4 C20 100.53(19) C13 P4 C20 92.6(2) C40 P2 C46 99.4(2) C40 P2 C39 99.35(18) C46 P2 C39 93.98(19) C27 P3 C26 95.03(19) C27 P3 C33 100.88(18) C26 P3 C33 94.7(2) C1 P1 C52 98.3(2) C1 P1 C7 97.24(19) C52 P1 C7 95.65(18) C47 N1 C51 117.5(4) C12 N4 C8 116.6(4) C25 N3 C21 116.5(4) C34 N2 C38 117.4(3) C54 O9 C55 113.8(4) N1 C47 C48 123.3(4) N1 C47 C46 117.5(4) C48 C47 C46 119.2(4) O4 C39 C38 120.6(4) O4 C39 P2 122.6(3) C38 C39 P2 116.5(3) C10 C11 C12 118.3(4) C10 C11 H11 120.8 C12 C11 H11 120.8 C23 C22 C21 118.4(4) C23 C22 H22 120.8 C21 C22 H22 120.8 O2 C52 C51 120.9(4) O2 C52 P1 123.2(3) C51 C52 P1 115.8(3) O8 C13 C12 120.2(4) O8 C13 P4 123.3(3) C12 C13 P4 116.4(3) C10 C9 C8 118.4(4) C10 C9 H9 120.8 C8 C9 H9 120.8 N2 C34 C35 123.3(3) N2 C34 C33 115.2(3) C35 C34 C33 121.5(4) O1 C7 C8 120.1(4) O1 C7 P1 123.1(3) C8 C7 P1 116.4(3) C22 C23 C24 118.9(4) C22 C23 H23 120.5 C24 C23 H23 120.5 N4 C12 C11 124.1(4) N4 C12 C13 116.0(4) C11 C12 C13 119.9(4) C27 C32 C31 120.0(5) C27 C32 H32 120.0 C31 C32 H32 120.0 C6 C1 C2 118.2(4) C6 C1 P1 117.3(4) C2 C1 P1 124.3(3) N3 C21 C22 124.4(4) N3 C21 C20 115.5(4) C22 C21 C20 120.1(4) N4 C8 C9 123.5(4) N4 C8 C7 117.3(4) C9 C8 C7 119.3(4) N3 C25 C24 123.7(4) N3 C25 C26 116.3(4) C24 C25 C26 119.8(4) N2 C38 C37 122.8(4) N2 C38 C39 115.4(3) C37 C38 C39 121.8(3) O7 C20 C21 121.5(4) O7 C20 P4 122.2(4) C21 C20 P4 116.2(3) C27 C28 C29 120.4(4) C27 C28 H28 119.8 C29 C28 H28 119.8 C32 C27 C28 119.4(4) C32 C27 P3 116.1(4) C28 C27 P3 124.4(3) C36 C35 C34 118.9(4) C36 C35 H35 120.5 C34 C35 H35 120.5 C30 C29 C28 119.6(5) C30 C29 H29 120.2 C28 C29 H29 120.2 O3 C46 C47 120.6(4) O3 C46 P2 122.7(3) C47 C46 P2 116.6(3) C23 C24 C25 118.0(4) C23 C24 H24 121.0 C25 C24 H24 121.0 C15 C14 C19 117.9(4) C15 C14 P4 117.1(3) C19 C14 P4 124.8(3) C18 C19 C14 121.2(4) C18 C19 H19 119.4 C14 C19 H19 119.4 O6 C26 C25 121.5(4) O6 C26 P3 125.7(3) C25 C26 P3 112.8(3) C11 C10 C9 119.1(4) C11 C10 H10 120.5 C9 C10 H10 120.5 C45 C40 C41 119.2(4) C45 C40 P2 118.4(3) C41 C40 P2 122.4(4) N1 C51 C50 123.3(4) N1 C51 C52 118.2(4) C50 C51 C52 118.5(4) C3 C2 C1 121.3(4) C3 C2 H2 119.3 C1 C2 H2 119.3 C36 C37 C38 118.7(4) C36 C37 H37 120.6 C38 C37 H37 120.6 C51 C50 C49 119.2(4) C51 C50 H50 120.4 C49 C50 H50 120.4 C16 C17 C18 118.8(4) C16 C17 H17 120.6 C18 C17 H17 120.6 C42 C41 C40 119.7(5) C42 C41 H41 120.1 C40 C41 H41 120.1 C49 C48 C47 118.2(4) C49 C48 H48 120.9 C47 C48 H48 120.9 C37 C36 C35 118.9(4) C37 C36 H36 120.6 C35 C36 H36 120.6 C16 C15 C14 120.9(4) C16 C15 H15 119.5 C14 C15 H15 119.5 C19 C18 C17 120.1(4) C19 C18 H18 119.9 C17 C18 H18 119.9 C31 C30 C29 120.2(4) C31 C30 H30 119.9 C29 C30 H30 119.9 O5 C33 C34 122.0(4) O5 C33 P3 124.5(3) C34 C33 P3 113.3(3) C50 C49 C48 118.3(5) C50 C49 H49 120.8 C48 C49 H49 120.8 C2 C3 C4 119.3(5) C2 C3 H3 120.4 C4 C3 H3 120.4 C15 C16 C17 121.0(4) C15 C16 H16 119.5 C17 C16 H16 119.5 C42 C43 C44 120.2(5) C42 C43 H43 119.9 C44 C43 H43 119.9 C43 C42 C41 120.8(5) C43 C42 H42 119.6 C41 C42 H42 119.6 C30 C31 C32 120.4(5) C30 C31 H31 119.8 C32 C31 H31 119.8 C5 C4 C3 120.2(4) C5 C4 H4 119.9 C3 C4 H4 119.9 C1 C6 C5 120.8(5) C1 C6 H6 119.6 C5 C6 H6 119.6 C43 C44 C45 119.8(5) C43 C44 H44 120.1 C45 C44 H44 120.1 O9 C54 C53 110.1(5) O9 C54 H54A 109.6 C53 C54 H54A 109.6 O9 C54 H54B 109.6 C53 C54 H54B 109.6 H54A C54 H54B 108.2 C54 C53 H53A 109.5 C54 C53 H53B 109.5 H53A C53 H53B 109.5 C54 C53 H53C 109.5 H53A C53 H53C 109.5 H53B C53 H53C 109.5 C55 C56 H56A 109.5 C55 C56 H56B 109.5 H56A C56 H56B 109.5 C55 C56 H56C 109.5 H56A C56 H56C 109.5 H56B C56 H56C 109.5 C40 C45 C44 120.3(5) C40 C45 H45 119.8 C44 C45 H45 119.8 O9 C55 C56 113.4(5) O9 C55 H55A 108.9 C56 C55 H55A 108.9 O9 C55 H55B 108.9 C56 C55 H55B 108.9 H55A C55 H55B 107.7 C4 C5 C6 120.2(4) C4 C5 H5 119.9 C6 C5 H5 119.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P4 C14 1.816(4) P4 C13 1.886(5) P4 C20 1.894(5) P2 C40 1.834(4) P2 C46 1.875(5) P2 C39 1.889(4) P3 C27 1.843(4) P3 C26 1.874(5) P3 C33 1.886(4) P1 C1 1.832(4) P1 C52 1.876(5) P1 C7 1.885(4) O7 C20 1.214(5) O3 C46 1.222(5) O2 C52 1.215(4) O6 C26 1.199(5) O4 C39 1.219(5) O5 C33 1.203(5) O1 C7 1.207(5) O8 C13 1.216(5) N1 C47 1.332(5) N1 C51 1.337(5) N4 C12 1.335(5) N4 C8 1.337(5) N3 C25 1.335(6) N3 C21 1.335(5) N2 C34 1.332(5) N2 C38 1.344(5) O9 C54 1.416(6) O9 C55 1.431(7) C47 C48 1.399(7) C47 C46 1.497(5) C39 C38 1.492(6) C11 C10 1.377(6) C11 C12 1.391(6) C11 H11 0.9500 C22 C23 1.377(7) C22 C21 1.380(6) C22 H22 0.9500 C52 C51 1.491(6) C13 C12 1.496(6) C9 C10 1.379(6) C9 C8 1.401(6) C9 H9 0.9500 C34 C35 1.380(5) C34 C33 1.510(5) C7 C8 1.497(6) C23 C24 1.390(5) C23 H23 0.9500 C32 C27 1.380(6) C32 C31 1.396(6) C32 H32 0.9500 C1 C6 1.366(6) C1 C2 1.399(7) C21 C20 1.488(6) C25 C24 1.396(7) C25 C26 1.512(5) C38 C37 1.389(6) C28 C27 1.382(7) C28 C29 1.391(5) C28 H28 0.9500 C35 C36 1.379(6) C35 H35 0.9500 C29 C30 1.384(7) C29 H29 0.9500 C24 H24 0.9500 C14 C15 1.391(6) C14 C19 1.395(5) C19 C18 1.383(6) C19 H19 0.9500 C10 H10 0.9500 C40 C45 1.374(7) C40 C41 1.405(6) C51 C50 1.381(7) C2 C3 1.376(6) C2 H2 0.9500 C37 C36 1.375(6) C37 H37 0.9500 C50 C49 1.383(6) C50 H50 0.9500 C17 C16 1.386(6) C17 C18 1.391(6) C17 H17 0.9500 C41 C42 1.383(7) C41 H41 0.9500 C48 C49 1.393(6) C48 H48 0.9500 C36 H36 0.9500 C15 C16 1.377(6) C15 H15 0.9500 C18 H18 0.9500 C30 C31 1.361(7) C30 H30 0.9500 C49 H49 0.9500 C3 C4 1.380(6) C3 H3 0.9500 C16 H16 0.9500 C43 C42 1.366(8) C43 C44 1.378(8) C43 H43 0.9500 C42 H42 0.9500 C31 H31 0.9500 C4 C5 1.365(8) C4 H4 0.9500 C6 C5 1.390(7) C6 H6 0.9500 C44 C45 1.399(7) C44 H44 0.9500 C54 C53 1.483(9) C54 H54A 0.9900 C54 H54B 0.9900 C53 H53A 0.9800 C53 H53B 0.9800 C53 H53C 0.9800 C56 C55 1.491(8) C56 H56A 0.9800 C56 H56B 0.9800 C56 H56C 0.9800 C45 H45 0.9500 C55 H55A 0.9900 C55 H55B 0.9900 C5 H5 0.9500 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion C51 N1 C47 C48 -3.2(5) C51 N1 C47 C46 176.1(3) C40 P2 C39 O4 -14.6(4) C46 P2 C39 O4 -114.9(4) C40 P2 C39 C38 170.4(3) C46 P2 C39 C38 70.2(3) C1 P1 C52 O2 107.9(4) C7 P1 C52 O2 9.7(4) C1 P1 C52 C51 -69.8(3) C7 P1 C52 C51 -168.0(3) C14 P4 C13 O8 -10.0(4) C20 P4 C13 O8 -111.0(4) C14 P4 C13 C12 174.2(3) C20 P4 C13 C12 73.3(3) C38 N2 C34 C35 0.6(7) C38 N2 C34 C33 -176.0(4) C1 P1 C7 O1 4.2(5) C52 P1 C7 O1 103.3(4) C1 P1 C7 C8 177.6(3) C52 P1 C7 C8 -83.3(3) C21 C22 C23 C24 -0.5(6) C8 N4 C12 C11 -0.6(6) C8 N4 C12 C13 178.0(4) C10 C11 C12 N4 0.4(7) C10 C11 C12 C13 -178.1(4) O8 C13 C12 N4 -166.1(4) P4 C13 C12 N4 9.8(5) O8 C13 C12 C11 12.6(7) P4 C13 C12 C11 -171.5(3) C52 P1 C1 C6 150.1(4) C7 P1 C1 C6 -113.1(4) C52 P1 C1 C2 -35.4(4) C7 P1 C1 C2 61.4(4) C25 N3 C21 C22 -2.8(5) C25 N3 C21 C20 178.4(3) C23 C22 C21 N3 2.9(6) C23 C22 C21 C20 -178.4(3) C12 N4 C8 C9 0.2(6) C12 N4 C8 C7 -178.1(4) C10 C9 C8 N4 0.3(7) C10 C9 C8 C7 178.6(4) O1 C7 C8 N4 -173.2(4) P1 C7 C8 N4 13.2(5) O1 C7 C8 C9 8.4(7) P1 C7 C8 C9 -165.2(3) C21 N3 C25 C24 0.5(5) C21 N3 C25 C26 176.1(3) C34 N2 C38 C37 -0.1(7) C34 N2 C38 C39 178.9(4) O4 C39 C38 N2 -163.2(4) P2 C39 C38 N2 11.9(5) O4 C39 C38 C37 15.8(7) P2 C39 C38 C37 -169.2(4) N3 C21 C20 O7 165.7(3) C22 C21 C20 O7 -13.2(6) N3 C21 C20 P4 -16.7(4) C22 C21 C20 P4 164.4(3) C14 P4 C20 O7 -92.1(3) C13 P4 C20 O7 5.3(3) C14 P4 C20 C21 90.3(3) C13 P4 C20 C21 -172.2(3) C31 C32 C27 C28 1.6(6) C31 C32 C27 P3 -174.6(3) C29 C28 C27 C32 -2.9(6) C29 C28 C27 P3 172.9(3) C26 P3 C27 C32 140.8(3) C33 P3 C27 C32 -123.4(3) C26 P3 C27 C28 -35.1(4) C33 P3 C27 C28 60.7(4) N2 C34 C35 C36 -0.3(8) C33 C34 C35 C36 176.1(5) C27 C28 C29 C30 2.0(7) N1 C47 C46 O3 168.6(3) C48 C47 C46 O3 -12.1(5) N1 C47 C46 P2 -14.3(4) C48 C47 C46 P2 165.0(3) C40 P2 C46 O3 -100.6(3) C39 P2 C46 O3 -0.4(3) C40 P2 C46 C47 82.4(3) C39 P2 C46 C47 -177.4(3) C22 C23 C24 C25 -1.6(5) N3 C25 C24 C23 1.7(6) C26 C25 C24 C23 -173.8(3) C13 P4 C14 C15 115.3(4) C20 P4 C14 C15 -150.8(4) C13 P4 C14 C19 -59.7(4) C20 P4 C14 C19 34.2(5) C15 C14 C19 C18 -0.3(7) P4 C14 C19 C18 174.6(4) N3 C25 C26 O6 149.1(4) C24 C25 C26 O6 -35.1(5) N3 C25 C26 P3 -33.3(4) C24 C25 C26 P3 142.6(3) C27 P3 C26 O6 118.1(4) C33 P3 C26 O6 16.7(4) C27 P3 C26 C25 -59.5(3) C33 P3 C26 C25 -160.9(3) C12 C11 C10 C9 0.1(7) C8 C9 C10 C11 -0.4(7) C46 P2 C40 C45 -136.2(4) C39 P2 C40 C45 128.2(4) C46 P2 C40 C41 42.9(4) C39 P2 C40 C41 -52.8(4) C47 N1 C51 C50 1.1(5) C47 N1 C51 C52 -178.9(3) O2 C52 C51 N1 144.5(4) P1 C52 C51 N1 -37.8(4) O2 C52 C51 C50 -35.6(5) P1 C52 C51 C50 142.1(3) C6 C1 C2 C3 0.1(7) P1 C1 C2 C3 -174.3(4) N2 C38 C37 C36 -0.7(7) C39 C38 C37 C36 -179.6(5) N1 C51 C50 C49 1.5(6) C52 C51 C50 C49 -178.4(3) C45 C40 C41 C42 0.0(7) P2 C40 C41 C42 -179.1(4) N1 C47 C48 C49 2.6(6) C46 C47 C48 C49 -176.7(3) C38 C37 C36 C35 1.0(8) C34 C35 C36 C37 -0.5(8) C19 C14 C15 C16 1.4(7) P4 C14 C15 C16 -174.0(4) C14 C19 C18 C17 -0.9(7) C16 C17 C18 C19 1.1(7) C28 C29 C30 C31 0.2(7) N2 C34 C33 O5 -176.9(5) C35 C34 C33 O5 6.5(8) N2 C34 C33 P3 7.7(5) C35 C34 C33 P3 -169.0(4) C27 P3 C33 O5 6.8(5) C26 P3 C33 O5 102.9(5) C27 P3 C33 C34 -177.8(3) C26 P3 C33 C34 -81.8(4) C51 C50 C49 C48 -2.1(6) C47 C48 C49 C50 0.2(6) C1 C2 C3 C4 -0.3(7) C14 C15 C16 C17 -1.1(8) C18 C17 C16 C15 -0.1(8) C44 C43 C42 C41 1.7(8) C40 C41 C42 C43 -1.4(8) C29 C30 C31 C32 -1.5(7) C27 C32 C31 C30 0.6(7) C2 C3 C4 C5 0.1(8) C2 C1 C6 C5 0.2(8) P1 C1 C6 C5 175.0(5) C42 C43 C44 C45 -0.5(8) C55 O9 C54 C53 -160.8(5) C41 C40 C45 C44 1.2(7) P2 C40 C45 C44 -179.7(4) C43 C44 C45 C40 -1.0(8) C54 O9 C55 C56 -64.3(7) C3 C4 C5 C6 0.3(9) C1 C6 C5 C4 -0.4(9)