#------------------------------------------------------------------------------ #$Date: 2017-04-22 05:09:35 +0300 (Sat, 22 Apr 2017) $ #$Revision: 195681 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042750.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_7042750 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_sum 'C40 H26 Cl2 N3 O6 P3' _chemical_formula_weight 808.45 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -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 93.834(4) _cell_angle_beta 96.273(4) _cell_angle_gamma 106.767(5) _cell_formula_units_Z 2 _cell_length_a 8.8960(5) _cell_length_b 13.1019(6) _cell_length_c 16.2731(7) _cell_measurement_reflns_used 4255 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 29.2 _cell_measurement_theta_min 3.1 _cell_volume 1795.52(16) _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Rigaku saturn 724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_unetI/netI 0.0562 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 16019 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 24.999 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.959 _exptl_absorpt_coefficient_mu 0.369 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_correction_T_min 0.926 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'Numabs Rigaku 1999' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.495 _exptl_crystal_description prism _exptl_crystal_F_000 828 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.711 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.088 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 487 _refine_ls_number_reflns 6317 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0480 _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^)+(0.0640P)^2^+1.6230P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1183 _refine_ls_wR_factor_ref 0.1273 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5463 _reflns_number_total 6317 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7dt00737j2.cif _cod_data_source_block msb-vsk-233_mo _cod_original_cell_volume 1795.51(16) _cod_database_code 7042750 _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-134_mo.res created by SHELXL-2014/7 TITL msb-vsk-134_mo_a.res in P-1 REM Old TITL MSB-VSK-134_Mo in P-1 #2 REM SHELXT solution in P-1 REM R1 0.157, Rweak 0.007, Alpha 0.033, Orientation as input REM Formula found by SHELXT: C40 N3 O6 P Cl4 CELL 0.71073 8.895963 13.101914 16.273114 93.8337 96.273 106.7674 ZERR 2 0.000474 0.000636 0.000684 0.0037 0.0039 0.0045 LATT 1 SFAC C H Cl N O P UNIT 80 52 4 6 12 6 L.S. 5 PLAN 20 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 OMIT -3 50 OMIT 1 -1 2 OMIT -1 2 0 OMIT 1 -2 1 OMIT 0 1 0 OMIT 0 -1 2 OMIT 0 2 0 OMIT 0 1 1 OMIT -3 1 7 REM REM REM WGHT 0.064000 1.623000 FVAR 0.32463 P2 6 0.326873 0.714418 0.319574 11.00000 0.01644 0.01663 = 0.01631 0.00353 0.00639 0.00562 P1 6 0.660627 0.820713 0.154416 11.00000 0.01633 0.01445 = 0.01650 0.00430 0.00525 0.00342 P3 6 0.609503 0.507894 0.274228 11.00000 0.01908 0.01565 = 0.01913 0.00319 0.00492 0.00742 CL1 3 -0.041080 0.815983 0.672378 11.00000 0.04922 0.07111 = 0.04003 -0.00052 -0.00159 0.03741 CL2 3 0.287461 0.896674 0.643913 11.00000 0.06477 0.04004 = 0.03605 0.00267 0.01374 0.00499 O5 5 0.441597 0.811633 0.020946 11.00000 0.02277 0.02133 = 0.02531 0.01022 0.00057 0.00622 O6 5 0.354877 0.341739 0.203664 11.00000 0.02136 0.01578 = 0.03410 0.00907 0.00496 0.00359 O1 5 0.609535 0.348584 0.375328 11.00000 0.03691 0.02914 = 0.02713 0.01025 0.01176 0.02100 O4 5 0.738270 1.031357 0.124143 11.00000 0.03003 0.01676 = 0.03316 0.00679 0.01779 0.00347 O2 5 0.113648 0.662891 0.433362 11.00000 0.03217 0.03206 = 0.03892 0.01689 0.02351 0.01827 O3 5 0.087439 0.807047 0.321342 11.00000 0.02526 0.04641 = 0.03808 0.02340 0.01656 0.01966 N3 4 0.465587 0.590959 0.125829 11.00000 0.01355 0.01557 = 0.01926 0.00349 0.00914 0.00560 N2 4 0.369682 0.518014 0.378357 11.00000 0.01975 0.01598 = 0.01993 0.00367 0.00367 0.00636 N1 4 0.425163 0.896739 0.224859 11.00000 0.01785 0.01620 = 0.01447 0.00223 0.00368 0.00475 C34 1 0.395963 0.485312 0.122209 11.00000 0.01676 0.01550 = 0.02225 0.00369 0.00860 0.00571 C33 1 0.434510 0.431911 0.195761 11.00000 0.01733 0.01593 = 0.02307 0.00258 0.00882 0.00852 C9 1 0.445714 1.062127 0.166518 11.00000 0.02479 0.01651 = 0.02594 0.00645 0.00632 0.00416 AFIX 43 H9 2 0.496081 1.112883 0.133270 11.00000 -1.20000 AFIX 0 C21 1 0.261909 0.542130 0.420352 11.00000 0.01711 0.01753 = 0.01994 0.00412 0.00391 0.00341 C20 1 0.215091 0.639457 0.399696 11.00000 0.01629 0.01859 = 0.02034 0.00307 0.00558 0.00364 C14 1 0.502139 0.792763 0.390576 11.00000 0.02016 0.01261 = 0.01764 0.00654 0.00265 0.00403 C22 1 0.195793 0.483008 0.482304 11.00000 0.01760 0.02857 = 0.02223 0.00589 0.00781 0.00833 AFIX 43 H22 2 0.123598 0.503757 0.511654 11.00000 -1.20000 AFIX 0 C38 1 0.418457 0.641109 0.063451 11.00000 0.01429 0.01743 = 0.01762 0.00393 0.00788 0.00440 C39 1 0.490726 0.759436 0.069654 11.00000 0.01495 0.01974 = 0.01824 0.00638 0.00938 0.00669 C10 1 0.318559 1.073132 0.203204 11.00000 0.02869 0.01728 = 0.02929 0.00387 0.00139 0.01050 AFIX 43 H10 2 0.282985 1.132523 0.196155 11.00000 -1.20000 AFIX 0 C29 1 0.834896 0.297294 0.187002 11.00000 0.02511 0.01896 = 0.02192 0.00165 0.00328 0.00851 AFIX 43 H29 2 0.812172 0.224104 0.172229 11.00000 -1.20000 AFIX 0 C23 1 0.239140 0.393453 0.499296 11.00000 0.02458 0.02554 = 0.02254 0.00989 0.00648 0.00607 AFIX 43 H23 2 0.193325 0.350729 0.538734 11.00000 -1.20000 AFIX 0 C1 1 0.818056 0.823687 0.090582 11.00000 0.01697 0.01248 = 0.01648 -0.00073 0.00457 0.00095 C19 1 0.651772 0.794561 0.372551 11.00000 0.02072 0.01940 = 0.01872 0.00672 0.00698 0.00765 AFIX 43 H19 2 0.662298 0.755486 0.324806 11.00000 -1.20000 AFIX 0 C15 1 0.487905 0.850228 0.463160 11.00000 0.02370 0.02015 = 0.02357 0.00379 0.00682 0.01076 AFIX 43 H15 2 0.388254 0.849086 0.476189 11.00000 -1.20000 AFIX 0 C12 1 0.300838 0.908177 0.259178 11.00000 0.01826 0.01951 = 0.01243 0.00053 0.00015 0.00490 C18 1 0.785322 0.854333 0.425423 11.00000 0.01914 0.02505 = 0.02558 0.01048 0.00567 0.00675 AFIX 43 H18 2 0.885447 0.856105 0.412788 11.00000 -1.20000 AFIX 0 C28 1 0.719533 0.337870 0.212447 11.00000 0.02122 0.02031 = 0.02005 0.00388 0.00416 0.00590 AFIX 43 H28 2 0.619069 0.291800 0.214979 11.00000 -1.20000 AFIX 0 C11 1 0.243827 0.994824 0.250829 11.00000 0.02261 0.02185 = 0.02260 0.00075 0.00416 0.00811 AFIX 43 H11 2 0.157695 1.000537 0.276427 11.00000 -1.20000 AFIX 0 C6 1 0.934795 0.780758 0.123077 11.00000 0.01885 0.02106 = 0.02038 0.00374 0.00293 0.00462 AFIX 43 H6 2 0.928028 0.752448 0.173924 11.00000 -1.20000 AFIX 0 C17 1 0.770143 0.911203 0.496737 11.00000 0.02467 0.02390 = 0.02403 0.00558 -0.00032 0.00343 AFIX 43 H17 2 0.860122 0.951271 0.532164 11.00000 -1.20000 AFIX 0 C7 1 0.640351 0.957961 0.147191 11.00000 0.02393 0.01502 = 0.01832 0.00185 0.00497 0.00312 C4 1 1.074140 0.823682 0.006820 11.00000 0.01739 0.02206 = 0.02505 -0.00339 0.00832 0.00051 AFIX 43 H4 2 1.161132 0.825376 -0.020574 11.00000 -1.20000 AFIX 0 C2 1 0.830592 0.865936 0.014595 11.00000 0.02023 0.01646 = 0.02100 0.00413 0.00563 0.00415 AFIX 43 H2 2 0.752966 0.894430 -0.008178 11.00000 -1.20000 AFIX 0 C8 1 0.497443 0.973399 0.180206 11.00000 0.01984 0.01533 = 0.01759 0.00174 0.00300 0.00276 C37 1 0.306799 0.589057 -0.003575 11.00000 0.02629 0.02450 = 0.01988 0.00600 0.00318 0.00615 AFIX 43 H37 2 0.275673 0.627442 -0.044818 11.00000 -1.20000 AFIX 0 C3 1 0.957006 0.865887 -0.027140 11.00000 0.02509 0.01497 = 0.02179 0.00136 0.01197 0.00102 AFIX 43 H3 2 0.964334 0.894022 -0.078037 11.00000 -1.20000 AFIX 0 C16 1 0.622715 0.908963 0.515716 11.00000 0.03351 0.01933 = 0.02129 0.00055 0.00300 0.00871 AFIX 43 H16 2 0.613306 0.947133 0.564178 11.00000 -1.20000 AFIX 0 C26 1 0.545186 0.413981 0.354927 11.00000 0.02566 0.01710 = 0.01908 0.00235 0.00576 0.00862 C5 1 1.060492 0.779658 0.080807 11.00000 0.01940 0.02655 = 0.02641 -0.00040 0.00108 0.00815 AFIX 43 H5 2 1.136306 0.748963 0.102523 11.00000 -1.20000 AFIX 0 C27 1 0.751481 0.447437 0.234527 11.00000 0.01809 0.01924 = 0.01726 0.00225 0.00426 0.00756 C25 1 0.415148 0.433245 0.398120 11.00000 0.02126 0.01960 = 0.01785 0.00385 0.00284 0.00669 C32 1 0.903458 0.514991 0.231337 11.00000 0.02071 0.01704 = 0.02391 0.00117 0.00160 0.00375 AFIX 43 H32 2 0.927516 0.588094 0.246926 11.00000 -1.20000 AFIX 0 C35 1 0.287180 0.426692 0.055648 11.00000 0.02625 0.01463 = 0.02577 0.00093 0.00834 0.00275 AFIX 43 H35 2 0.245165 0.352764 0.054316 11.00000 -1.20000 AFIX 0 C13 1 0.219530 0.816591 0.305481 11.00000 0.01936 0.02273 = 0.01614 0.00384 0.00523 0.00763 C30 1 0.985303 0.365307 0.183295 11.00000 0.02165 0.02857 = 0.02676 0.00086 0.00563 0.01140 AFIX 43 H30 2 1.063438 0.337763 0.166147 11.00000 -1.20000 AFIX 0 C24 1 0.351704 0.367708 0.457011 11.00000 0.02450 0.02065 = 0.02451 0.00728 0.00370 0.00683 AFIX 43 H24 2 0.384177 0.307940 0.467735 11.00000 -1.20000 AFIX 0 C36 1 0.242818 0.479996 -0.008189 11.00000 0.03100 0.02704 = 0.01935 -0.00067 -0.00148 0.00057 AFIX 43 H36 2 0.170713 0.442745 -0.053677 11.00000 -1.20000 AFIX 0 C31 1 1.018557 0.473351 0.204991 11.00000 0.01581 0.02759 = 0.03054 0.00163 0.00432 0.00149 AFIX 43 H31 2 1.119151 0.518912 0.201968 11.00000 -1.20000 AFIX 0 C40 1 0.112083 0.791534 0.620737 11.00000 0.04514 0.04418 = 0.02780 -0.00404 -0.00076 0.02126 AFIX 23 H40A 2 0.130867 0.725931 0.637054 11.00000 -1.20000 H40B 2 0.078958 0.781704 0.561208 11.00000 -1.20000 AFIX 0 HKLF 4 REM msb-vsk-134_mo_a.res in P-1 REM R1 = 0.0480 for 5463 Fo > 4sig(Fo) and 0.0576 for all 6317 data REM 487 parameters refined using 0 restraints END WGHT 0.0595 1.7111 REM Highest difference peak 0.711, deepest hole -0.522, 1-sigma level 0.088 Q1 1 0.1901 0.9017 0.6113 11.00000 0.05 0.71 Q2 1 0.3744 0.4388 0.0748 11.00000 0.05 0.38 Q3 1 0.2581 0.7630 0.3078 11.00000 0.05 0.38 Q4 1 0.1440 0.8549 0.3579 11.00000 0.05 0.36 Q5 1 0.3446 0.6251 0.0289 11.00000 0.05 0.35 Q6 1 0.5606 0.7784 0.1115 11.00000 0.05 0.34 Q7 1 0.6598 0.8038 0.2182 11.00000 0.05 0.33 Q8 1 0.2756 1.0820 0.1836 11.00000 0.05 0.32 Q9 1 0.3009 0.3979 0.0497 11.00000 0.05 0.32 Q10 1 0.6953 0.5613 0.3043 11.00000 0.05 0.32 Q11 1 0.2550 0.5213 0.4686 11.00000 0.05 0.31 Q12 1 0.2708 0.5439 0.0146 11.00000 0.05 0.31 Q13 1 0.8203 0.9915 0.5358 11.00000 0.05 0.31 Q14 1 0.2802 0.2775 0.1306 11.00000 0.05 0.30 Q15 1 0.6428 0.8944 0.1626 11.00000 0.05 0.30 Q16 1 0.4251 0.7632 0.3559 11.00000 0.05 0.30 Q17 1 0.4344 0.6990 0.0628 11.00000 0.05 0.30 Q18 1 0.6426 1.0193 0.4762 11.00000 0.05 0.29 Q19 1 0.1990 0.3343 0.5925 11.00000 0.05 0.29 Q20 1 0.4169 0.8489 0.6056 11.00000 0.05 0.29 ; _shelx_res_checksum 46105 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 P2 P 0.32687(7) 0.71442(5) 0.31957(4) 0.01590(16) Uani 1 1 d . . P1 P 0.66063(7) 0.82071(5) 0.15442(4) 0.01565(16) Uani 1 1 d . . P3 P 0.60950(8) 0.50789(5) 0.27423(4) 0.01723(16) Uani 1 1 d . . Cl1 Cl -0.04108(11) 0.81598(8) 0.67238(5) 0.0502(2) Uani 1 1 d . . Cl2 Cl 0.28746(11) 0.89667(7) 0.64391(5) 0.0487(2) Uani 1 1 d . . O5 O 0.4416(2) 0.81163(14) 0.02095(11) 0.0231(4) Uani 1 1 d . . O6 O 0.3549(2) 0.34174(13) 0.20366(12) 0.0238(4) Uani 1 1 d . . O1 O 0.6095(2) 0.34858(15) 0.37533(12) 0.0278(4) Uani 1 1 d . . O4 O 0.7383(2) 1.03136(14) 0.12414(12) 0.0261(4) Uani 1 1 d . . O2 O 0.1136(2) 0.66289(15) 0.43336(13) 0.0305(5) Uani 1 1 d . . O3 O 0.0874(2) 0.80705(17) 0.32134(13) 0.0328(5) Uani 1 1 d . . N3 N 0.4656(2) 0.59096(15) 0.12583(13) 0.0152(4) Uani 1 1 d . . N2 N 0.3697(2) 0.51801(16) 0.37836(13) 0.0182(5) Uani 1 1 d . . N1 N 0.4252(2) 0.89674(15) 0.22486(12) 0.0161(4) Uani 1 1 d . . C34 C 0.3960(3) 0.48531(19) 0.12221(16) 0.0174(5) Uani 1 1 d . . C33 C 0.4345(3) 0.43191(19) 0.19576(16) 0.0175(5) Uani 1 1 d . . C9 C 0.4457(3) 1.0621(2) 0.16652(17) 0.0224(6) Uani 1 1 d . . H9 H 0.4961 1.1129 0.1333 0.027 Uiso 1 1 calc R U C21 C 0.2619(3) 0.54213(19) 0.42035(16) 0.0184(5) Uani 1 1 d . . C20 C 0.2151(3) 0.63946(19) 0.39970(16) 0.0184(5) Uani 1 1 d . . C14 C 0.5021(3) 0.79276(18) 0.39058(15) 0.0167(5) Uani 1 1 d . . C22 C 0.1958(3) 0.4830(2) 0.48230(16) 0.0219(6) Uani 1 1 d . . H22 H 0.1236 0.5038 0.5117 0.026 Uiso 1 1 calc R U C38 C 0.4185(3) 0.64111(19) 0.06345(15) 0.0160(5) Uani 1 1 d . . C39 C 0.4907(3) 0.75944(19) 0.06965(15) 0.0166(5) Uani 1 1 d . . C10 C 0.3186(3) 1.0731(2) 0.20320(17) 0.0244(6) Uani 1 1 d . . H10 H 0.2830 1.1325 0.1962 0.029 Uiso 1 1 calc R U C29 C 0.8349(3) 0.2973(2) 0.18700(16) 0.0216(6) Uani 1 1 d . . H29 H 0.8122 0.2241 0.1722 0.026 Uiso 1 1 calc R U C23 C 0.2391(3) 0.3935(2) 0.49930(17) 0.0239(6) Uani 1 1 d . . H23 H 0.1933 0.3507 0.5387 0.029 Uiso 1 1 calc R U C1 C 0.8181(3) 0.82369(18) 0.09058(15) 0.0160(5) Uani 1 1 d . . C19 C 0.6518(3) 0.7946(2) 0.37255(16) 0.0187(5) Uani 1 1 d . . H19 H 0.6623 0.7555 0.3248 0.022 Uiso 1 1 calc R U C15 C 0.4879(3) 0.8502(2) 0.46316(16) 0.0212(6) Uani 1 1 d . . H15 H 0.3883 0.8491 0.4762 0.025 Uiso 1 1 calc R U C12 C 0.3008(3) 0.90818(19) 0.25918(15) 0.0171(5) Uani 1 1 d . . C18 C 0.7853(3) 0.8543(2) 0.42542(17) 0.0226(6) Uani 1 1 d . . H18 H 0.8854 0.8561 0.4128 0.027 Uiso 1 1 calc R U C28 C 0.7195(3) 0.3379(2) 0.21245(16) 0.0204(5) Uani 1 1 d . . H28 H 0.6191 0.2918 0.2150 0.024 Uiso 1 1 calc R U C11 C 0.2438(3) 0.9948(2) 0.25083(16) 0.0220(6) Uani 1 1 d . . H11 H 0.1577 1.0005 0.2764 0.026 Uiso 1 1 calc R U C6 C 0.9348(3) 0.7808(2) 0.12308(16) 0.0203(5) Uani 1 1 d . . H6 H 0.9280 0.7524 0.1739 0.024 Uiso 1 1 calc R U C17 C 0.7701(3) 0.9112(2) 0.49674(17) 0.0251(6) Uani 1 1 d . . H17 H 0.8601 0.9513 0.5322 0.030 Uiso 1 1 calc R U C7 C 0.6404(3) 0.95796(19) 0.14719(16) 0.0195(5) Uani 1 1 d . . C4 C 1.0741(3) 0.8237(2) 0.00682(17) 0.0225(6) Uani 1 1 d . . H4 H 1.1611 0.8254 -0.0206 0.027 Uiso 1 1 calc R U C2 C 0.8306(3) 0.86594(19) 0.01459(16) 0.0192(5) Uani 1 1 d . . H2 H 0.7530 0.8944 -0.0082 0.023 Uiso 1 1 calc R U C8 C 0.4974(3) 0.97340(19) 0.18021(15) 0.0181(5) Uani 1 1 d . . C37 C 0.3068(3) 0.5891(2) -0.00358(16) 0.0237(6) Uani 1 1 d . . H37 H 0.2757 0.6274 -0.0448 0.028 Uiso 1 1 calc R U C3 C 0.9570(3) 0.86589(19) -0.02714(16) 0.0210(6) Uani 1 1 d . . H3 H 0.9643 0.8940 -0.0780 0.025 Uiso 1 1 calc R U C16 C 0.6227(3) 0.9090(2) 0.51572(17) 0.0247(6) Uani 1 1 d . . H16 H 0.6133 0.9471 0.5642 0.030 Uiso 1 1 calc R U C26 C 0.5452(3) 0.41398(19) 0.35493(16) 0.0199(5) Uani 1 1 d . . C5 C 1.0605(3) 0.7797(2) 0.08081(17) 0.0241(6) Uani 1 1 d . . H5 H 1.1363 0.7490 0.1025 0.029 Uiso 1 1 calc R U C27 C 0.7515(3) 0.44744(19) 0.23453(15) 0.0176(5) Uani 1 1 d . . C25 C 0.4151(3) 0.4332(2) 0.39812(16) 0.0193(5) Uani 1 1 d . . C32 C 0.9035(3) 0.5150(2) 0.23134(16) 0.0211(6) Uani 1 1 d . . H32 H 0.9275 0.5881 0.2469 0.025 Uiso 1 1 calc R U C35 C 0.2872(3) 0.4267(2) 0.05565(16) 0.0226(6) Uani 1 1 d . . H35 H 0.2452 0.3528 0.0543 0.027 Uiso 1 1 calc R U C13 C 0.2195(3) 0.8166(2) 0.30548(15) 0.0188(5) Uani 1 1 d . . C30 C 0.9853(3) 0.3653(2) 0.18329(17) 0.0247(6) Uani 1 1 d . . H30 H 1.0634 0.3378 0.1661 0.030 Uiso 1 1 calc R U C24 C 0.3517(3) 0.3677(2) 0.45701(17) 0.0229(6) Uani 1 1 d . . H24 H 0.3842 0.3079 0.4677 0.028 Uiso 1 1 calc R U C36 C 0.2428(3) 0.4800(2) -0.00819(17) 0.0280(6) Uani 1 1 d . . H36 H 0.1707 0.4427 -0.0537 0.034 Uiso 1 1 calc R U C31 C 1.0186(3) 0.4734(2) 0.20499(17) 0.0257(6) Uani 1 1 d . . H31 H 1.1192 0.5189 0.2020 0.031 Uiso 1 1 calc R U C40 C 0.1121(4) 0.7915(3) 0.6207(2) 0.0382(8) Uani 1 1 d . . H40A H 0.1309 0.7259 0.6371 0.046 Uiso 1 1 calc R U H40B H 0.0790 0.7817 0.5612 0.046 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 P2 0.0164(3) 0.0166(3) 0.0163(3) 0.0035(2) 0.0064(2) 0.0056(3) P1 0.0163(3) 0.0145(3) 0.0165(3) 0.0043(2) 0.0052(2) 0.0034(2) P3 0.0191(3) 0.0156(3) 0.0191(3) 0.0032(3) 0.0049(3) 0.0074(3) Cl1 0.0492(5) 0.0711(6) 0.0400(5) -0.0005(4) -0.0016(4) 0.0374(5) Cl2 0.0648(6) 0.0400(5) 0.0361(5) 0.0027(4) 0.0137(4) 0.0050(4) O5 0.0228(10) 0.0213(9) 0.0253(10) 0.0102(8) 0.0006(8) 0.0062(8) O6 0.0214(10) 0.0158(9) 0.0341(11) 0.0091(8) 0.0050(8) 0.0036(7) O1 0.0369(11) 0.0291(10) 0.0271(11) 0.0103(8) 0.0118(8) 0.0210(9) O4 0.0300(11) 0.0168(9) 0.0332(11) 0.0068(8) 0.0178(8) 0.0035(8) O2 0.0322(11) 0.0321(11) 0.0389(12) 0.0169(9) 0.0235(9) 0.0183(9) O3 0.0253(11) 0.0464(12) 0.0381(12) 0.0234(10) 0.0166(9) 0.0197(9) N3 0.0136(10) 0.0156(10) 0.0193(11) 0.0035(8) 0.0091(8) 0.0056(8) N2 0.0197(11) 0.0160(10) 0.0199(11) 0.0037(8) 0.0037(9) 0.0064(9) N1 0.0178(11) 0.0162(10) 0.0145(10) 0.0022(8) 0.0037(8) 0.0048(8) C34 0.0168(12) 0.0155(12) 0.0222(13) 0.0037(10) 0.0086(10) 0.0057(10) C33 0.0173(13) 0.0159(13) 0.0231(14) 0.0026(10) 0.0088(10) 0.0085(10) C9 0.0248(14) 0.0165(13) 0.0259(15) 0.0064(10) 0.0063(11) 0.0042(10) C21 0.0171(13) 0.0175(12) 0.0199(13) 0.0041(10) 0.0039(10) 0.0034(10) C20 0.0163(13) 0.0186(13) 0.0203(13) 0.0031(10) 0.0056(10) 0.0036(10) C14 0.0202(13) 0.0126(12) 0.0176(13) 0.0065(9) 0.0026(10) 0.0040(10) C22 0.0176(13) 0.0286(14) 0.0222(14) 0.0059(11) 0.0078(10) 0.0083(11) C38 0.0143(12) 0.0174(12) 0.0176(13) 0.0039(10) 0.0079(9) 0.0044(10) C39 0.0150(12) 0.0197(12) 0.0182(13) 0.0064(10) 0.0094(10) 0.0067(10) C10 0.0287(15) 0.0173(13) 0.0293(15) 0.0039(11) 0.0014(11) 0.0105(11) C29 0.0251(14) 0.0190(13) 0.0219(14) 0.0016(10) 0.0033(11) 0.0085(11) C23 0.0246(14) 0.0255(14) 0.0225(14) 0.0099(11) 0.0065(11) 0.0061(11) C1 0.0170(12) 0.0125(11) 0.0165(13) -0.0007(9) 0.0046(9) 0.0009(9) C19 0.0207(13) 0.0194(12) 0.0187(13) 0.0067(10) 0.0070(10) 0.0077(10) C15 0.0237(14) 0.0201(13) 0.0236(14) 0.0038(10) 0.0068(11) 0.0108(11) C12 0.0183(13) 0.0195(12) 0.0124(12) 0.0005(10) 0.0001(10) 0.0049(10) C18 0.0191(13) 0.0251(14) 0.0256(15) 0.0105(11) 0.0057(11) 0.0068(11) C28 0.0212(13) 0.0203(13) 0.0200(13) 0.0039(10) 0.0042(10) 0.0059(10) C11 0.0226(14) 0.0219(13) 0.0226(14) 0.0008(11) 0.0042(10) 0.0081(11) C6 0.0189(13) 0.0211(13) 0.0204(13) 0.0037(10) 0.0029(10) 0.0046(10) C17 0.0247(15) 0.0239(14) 0.0240(15) 0.0056(11) -0.0003(11) 0.0034(11) C7 0.0239(14) 0.0150(12) 0.0183(13) 0.0019(10) 0.0050(10) 0.0031(11) C4 0.0174(13) 0.0221(13) 0.0250(14) -0.0034(11) 0.0083(11) 0.0005(10) C2 0.0202(13) 0.0165(12) 0.0210(14) 0.0041(10) 0.0056(10) 0.0042(10) C8 0.0198(13) 0.0153(12) 0.0176(13) 0.0017(10) 0.0030(10) 0.0028(10) C37 0.0263(14) 0.0245(14) 0.0199(14) 0.0060(11) 0.0032(11) 0.0061(11) C3 0.0251(14) 0.0150(12) 0.0218(14) 0.0014(10) 0.0120(11) 0.0010(10) C16 0.0335(16) 0.0193(13) 0.0213(14) 0.0006(11) 0.0030(11) 0.0087(11) C26 0.0257(14) 0.0171(13) 0.0191(13) 0.0024(10) 0.0058(10) 0.0086(11) C5 0.0194(14) 0.0266(14) 0.0264(15) -0.0004(11) 0.0011(11) 0.0081(11) C27 0.0181(13) 0.0192(12) 0.0173(13) 0.0023(10) 0.0043(10) 0.0076(10) C25 0.0213(13) 0.0196(13) 0.0179(13) 0.0039(10) 0.0028(10) 0.0067(10) C32 0.0207(13) 0.0170(12) 0.0239(14) 0.0012(10) 0.0016(10) 0.0037(10) C35 0.0262(14) 0.0146(12) 0.0258(15) 0.0009(10) 0.0083(11) 0.0028(10) C13 0.0194(14) 0.0227(13) 0.0161(13) 0.0038(10) 0.0052(10) 0.0076(10) C30 0.0216(14) 0.0286(14) 0.0268(15) 0.0009(11) 0.0056(11) 0.0114(11) C24 0.0245(14) 0.0206(13) 0.0245(14) 0.0073(11) 0.0037(11) 0.0068(11) C36 0.0310(16) 0.0270(15) 0.0193(14) -0.0007(11) -0.0015(11) 0.0006(12) C31 0.0158(13) 0.0276(15) 0.0305(16) 0.0016(12) 0.0043(11) 0.0015(11) C40 0.0451(19) 0.0442(18) 0.0278(17) -0.0040(14) -0.0008(14) 0.0213(15) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C14 P2 C13 100.58(11) C14 P2 C20 97.11(11) C13 P2 C20 99.35(11) C1 P1 C7 101.19(11) C1 P1 C39 96.47(11) C7 P1 C39 92.51(11) C27 P3 C26 98.11(11) C27 P3 C33 96.52(11) C26 P3 C33 92.46(11) C34 N3 C38 116.6(2) C21 N2 C25 117.3(2) C12 N1 C8 117.9(2) N3 C34 C35 123.3(2) N3 C34 C33 116.6(2) C35 C34 C33 120.1(2) O6 C33 C34 120.0(2) O6 C33 P3 122.03(19) C34 C33 P3 117.97(17) C10 C9 C8 118.5(2) C10 C9 H9 120.7 C8 C9 H9 120.7 N2 C21 C22 123.1(2) N2 C21 C20 117.0(2) C22 C21 C20 119.9(2) O2 C20 C21 120.0(2) O2 C20 P2 126.17(19) C21 C20 P2 113.81(18) C19 C14 C15 119.3(2) C19 C14 P2 119.66(19) C15 C14 P2 121.01(19) C23 C22 C21 118.7(2) C23 C22 H22 120.6 C21 C22 H22 120.6 N3 C38 C37 123.5(2) N3 C38 C39 116.5(2) C37 C38 C39 120.0(2) O5 C39 C38 120.3(2) O5 C39 P1 122.73(19) C38 C39 P1 116.98(17) C9 C10 C11 119.3(2) C9 C10 H10 120.3 C11 C10 H10 120.3 C28 C29 C30 120.1(2) C28 C29 H29 119.9 C30 C29 H29 119.9 C22 C23 C24 119.0(2) C22 C23 H23 120.5 C24 C23 H23 120.5 C6 C1 C2 118.7(2) C6 C1 P1 115.57(19) C2 C1 P1 125.68(19) C18 C19 C14 120.2(2) C18 C19 H19 119.9 C14 C19 H19 119.9 C16 C15 C14 119.7(2) C16 C15 H15 120.1 C14 C15 H15 120.1 N1 C12 C11 123.4(2) N1 C12 C13 115.4(2) C11 C12 C13 121.1(2) C17 C18 C19 120.1(2) C17 C18 H18 120.0 C19 C18 H18 120.0 C29 C28 C27 120.7(2) C29 C28 H28 119.7 C27 C28 H28 119.7 C12 C11 C10 118.1(2) C12 C11 H11 120.9 C10 C11 H11 120.9 C5 C6 C1 120.8(2) C5 C6 H6 119.6 C1 C6 H6 119.6 C16 C17 C18 120.2(3) C16 C17 H17 119.9 C18 C17 H17 119.9 O4 C7 C8 121.6(2) O4 C7 P1 124.3(2) C8 C7 P1 113.92(17) C5 C4 C3 119.7(2) C5 C4 H4 120.1 C3 C4 H4 120.1 C3 C2 C1 120.5(2) C3 C2 H2 119.8 C1 C2 H2 119.8 N1 C8 C9 122.7(2) N1 C8 C7 114.9(2) C9 C8 C7 122.4(2) C36 C37 C38 118.9(2) C36 C37 H37 120.5 C38 C37 H37 120.5 C2 C3 C4 120.1(2) C2 C3 H3 120.0 C4 C3 H3 120.0 C17 C16 C15 120.4(3) C17 C16 H16 119.8 C15 C16 H16 119.8 O1 C26 C25 121.6(2) O1 C26 P3 123.9(2) C25 C26 P3 114.25(17) C4 C5 C6 120.2(2) C4 C5 H5 119.9 C6 C5 H5 119.9 C28 C27 C32 118.8(2) C28 C27 P3 123.86(19) C32 C27 P3 117.25(18) N2 C25 C24 123.5(2) N2 C25 C26 115.8(2) C24 C25 C26 120.7(2) C31 C32 C27 120.1(2) C31 C32 H32 120.0 C27 C32 H32 120.0 C36 C35 C34 118.8(2) C36 C35 H35 120.6 C34 C35 H35 120.6 O3 C13 C12 120.0(2) O3 C13 P2 124.9(2) C12 C13 P2 114.46(17) C31 C30 C29 119.9(2) C31 C30 H30 120.1 C29 C30 H30 120.1 C23 C24 C25 118.3(2) C23 C24 H24 120.9 C25 C24 H24 120.9 C37 C36 C35 118.8(2) C37 C36 H36 120.6 C35 C36 H36 120.6 C30 C31 C32 120.5(2) C30 C31 H31 119.8 C32 C31 H31 119.8 Cl2 C40 Cl1 111.76(17) Cl2 C40 H40A 109.3 Cl1 C40 H40A 109.3 Cl2 C40 H40B 109.3 Cl1 C40 H40B 109.3 H40A C40 H40B 107.9 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance P2 C14 1.829(2) P2 C13 1.867(3) P2 C20 1.883(3) P1 C1 1.826(3) P1 C7 1.868(3) P1 C39 1.878(3) P3 C27 1.824(3) P3 C26 1.881(3) P3 C33 1.883(3) Cl1 C40 1.770(3) Cl2 C40 1.742(3) O5 C39 1.207(3) O6 C33 1.213(3) O1 C26 1.205(3) O4 C7 1.209(3) O2 C20 1.206(3) O3 C13 1.204(3) N3 C34 1.338(3) N3 C38 1.339(3) N2 C21 1.332(3) N2 C25 1.334(3) N1 C12 1.333(3) N1 C8 1.333(3) C34 C35 1.389(4) C34 C33 1.483(3) C9 C10 1.374(4) C9 C8 1.391(4) C9 H9 0.9300 C21 C22 1.390(4) C21 C20 1.499(3) C14 C19 1.388(4) C14 C15 1.395(4) C22 C23 1.372(4) C22 H22 0.9300 C38 C37 1.384(4) C38 C39 1.489(3) C10 C11 1.386(4) C10 H10 0.9300 C29 C28 1.373(4) C29 C30 1.387(4) C29 H29 0.9300 C23 C24 1.380(4) C23 H23 0.9300 C1 C6 1.390(4) C1 C2 1.391(3) C19 C18 1.384(4) C19 H19 0.9300 C15 C16 1.385(4) C15 H15 0.9300 C12 C11 1.379(3) C12 C13 1.507(3) C18 C17 1.377(4) C18 H18 0.9300 C28 C27 1.394(3) C28 H28 0.9300 C11 H11 0.9300 C6 C5 1.378(4) C6 H6 0.9300 C17 C16 1.373(4) C17 H17 0.9300 C7 C8 1.493(4) C4 C5 1.372(4) C4 C3 1.394(4) C4 H4 0.9300 C2 C3 1.376(4) C2 H2 0.9300 C37 C36 1.371(4) C37 H37 0.9300 C3 H3 0.9300 C16 H16 0.9300 C26 C25 1.489(4) C5 H5 0.9300 C27 C32 1.395(4) C25 C24 1.387(4) C32 C31 1.384(4) C32 H32 0.9300 C35 C36 1.374(4) C35 H35 0.9300 C30 C31 1.373(4) C30 H30 0.9300 C24 H24 0.9300 C36 H36 0.9300 C31 H31 0.9300 C40 H40A 0.9700 C40 H40B 0.9700 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 C38 N3 C34 C35 4.0(3) C38 N3 C34 C33 -173.2(2) N3 C34 C33 O6 166.3(2) C35 C34 C33 O6 -11.0(4) N3 C34 C33 P3 -14.2(3) C35 C34 C33 P3 168.47(19) C27 P3 C33 O6 82.4(2) C26 P3 C33 O6 -16.1(2) C27 P3 C33 C34 -97.15(19) C26 P3 C33 C34 164.40(19) C25 N2 C21 C22 -0.4(4) C25 N2 C21 C20 178.1(2) N2 C21 C20 O2 177.1(2) C22 C21 C20 O2 -4.3(4) N2 C21 C20 P2 -2.6(3) C22 C21 C20 P2 176.03(19) C14 P2 C20 O2 96.8(2) C13 P2 C20 O2 -5.2(3) C14 P2 C20 C21 -83.50(19) C13 P2 C20 C21 174.49(18) C13 P2 C14 C19 -129.7(2) C20 P2 C14 C19 129.3(2) C13 P2 C14 C15 50.8(2) C20 P2 C14 C15 -50.1(2) N2 C21 C22 C23 -2.3(4) C20 C21 C22 C23 179.2(2) C34 N3 C38 C37 -1.6(3) C34 N3 C38 C39 177.3(2) N3 C38 C39 O5 -171.7(2) C37 C38 C39 O5 7.2(4) N3 C38 C39 P1 9.3(3) C37 C38 C39 P1 -171.80(19) C1 P1 C39 O5 -83.1(2) C7 P1 C39 O5 18.5(2) C1 P1 C39 C38 95.92(19) C7 P1 C39 C38 -162.51(19) C8 C9 C10 C11 -1.5(4) C21 C22 C23 C24 2.8(4) C7 P1 C1 C6 136.10(19) C39 P1 C1 C6 -130.03(19) C7 P1 C1 C2 -42.9(2) C39 P1 C1 C2 50.9(2) C15 C14 C19 C18 -1.1(4) P2 C14 C19 C18 179.41(18) C19 C14 C15 C16 0.6(4) P2 C14 C15 C16 -179.92(19) C8 N1 C12 C11 0.0(3) C8 N1 C12 C13 177.3(2) C14 C19 C18 C17 0.8(4) C30 C29 C28 C27 0.2(4) N1 C12 C11 C10 1.0(4) C13 C12 C11 C10 -176.1(2) C9 C10 C11 C12 -0.2(4) C2 C1 C6 C5 -0.2(4) P1 C1 C6 C5 -179.31(19) C19 C18 C17 C16 0.0(4) C1 P1 C7 O4 -16.7(3) C39 P1 C7 O4 -113.8(2) C1 P1 C7 C8 168.75(18) C39 P1 C7 C8 71.65(19) C6 C1 C2 C3 -0.5(3) P1 C1 C2 C3 178.50(18) C12 N1 C8 C9 -1.8(4) C12 N1 C8 C7 177.1(2) C10 C9 C8 N1 2.6(4) C10 C9 C8 C7 -176.3(2) O4 C7 C8 N1 -161.4(2) P1 C7 C8 N1 13.3(3) O4 C7 C8 C9 17.5(4) P1 C7 C8 C9 -167.8(2) N3 C38 C37 C36 -1.6(4) C39 C38 C37 C36 179.5(2) C1 C2 C3 C4 -0.3(4) C5 C4 C3 C2 1.8(4) C18 C17 C16 C15 -0.5(4) C14 C15 C16 C17 0.2(4) C27 P3 C26 O1 9.8(3) C33 P3 C26 O1 106.8(2) C27 P3 C26 C25 -175.45(18) C33 P3 C26 C25 -78.50(19) C3 C4 C5 C6 -2.5(4) C1 C6 C5 C4 1.7(4) C29 C28 C27 C32 -0.8(4) C29 C28 C27 P3 -176.64(19) C26 P3 C27 C28 48.1(2) C33 P3 C27 C28 -45.3(2) C26 P3 C27 C32 -127.8(2) C33 P3 C27 C32 138.8(2) C21 N2 C25 C24 2.7(4) C21 N2 C25 C26 -175.1(2) O1 C26 C25 N2 170.4(2) P3 C26 C25 N2 -4.5(3) O1 C26 C25 C24 -7.5(4) P3 C26 C25 C24 177.7(2) C28 C27 C32 C31 1.3(4) P3 C27 C32 C31 177.4(2) N3 C34 C35 C36 -3.0(4) C33 C34 C35 C36 174.1(2) N1 C12 C13 O3 -162.4(2) C11 C12 C13 O3 14.9(4) N1 C12 C13 P2 8.9(3) C11 C12 C13 P2 -173.78(19) C14 P2 C13 O3 -121.6(2) C20 P2 C13 O3 -22.5(3) C14 P2 C13 C12 67.57(19) C20 P2 C13 C12 166.68(17) C28 C29 C30 C31 -0.1(4) C22 C23 C24 C25 -0.7(4) N2 C25 C24 C23 -2.1(4) C26 C25 C24 C23 175.6(2) C38 C37 C36 C35 2.6(4) C34 C35 C36 C37 -0.4(4) C29 C30 C31 C32 0.6(4) C27 C32 C31 C30 -1.2(4)