#------------------------------------------------------------------------------ #$Date: 2019-08-14 03:06:28 +0300 (Wed, 14 Aug 2019) $ #$Revision: 217510 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/39/7123980.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_7123980 loop_ _publ_author_name 'Ho, Luong Phong' 'Zaretzke, Marc-Kevin' 'Bannenberg, Thomas' 'Tamm, Matthias' _publ_section_title ; Heteroleptic diphosphenes and arsaphosphenes bearing neutral and anionic N-heterocyclic carbenes ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC05739K _journal_year 2019 _chemical_formula_moiety 'C72 H71 B Cl F15 N4 P2, 0.5(C6 D6)' _chemical_formula_sum 'C75 H71 B Cl D3 F15 N4 P2' _chemical_formula_weight 1427.60 _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 ; 2019-07-23 deposited with the CCDC. 2019-08-13 downloaded from the CCDC. ; _cell_angle_alpha 99.475(4) _cell_angle_beta 93.788(4) _cell_angle_gamma 109.582(4) _cell_formula_units_Z 2 _cell_length_a 13.5450(6) _cell_length_b 14.3760(10) _cell_length_c 19.5043(8) _cell_measurement_reflns_used 17925 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 76.0020 _cell_measurement_theta_min 3.3220 _cell_volume 3499.3(3) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_publication_material ; WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.) ; _computing_structure_refinement ; SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst. (2008), A64, 112-122)' ; _computing_structure_solution ; SHELXT-2014/7 (G. M. Sheldrick, Acta Cryst., 2008, A64, 112-122) ; _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.3543 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0707 _diffrn_reflns_av_unetI/netI 0.0473 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 70864 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 76.204 _diffrn_reflns_theta_min 3.329 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'Nova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.657 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_correction_T_min 0.951 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.355 _exptl_crystal_description irregular _exptl_crystal_F_000 1478 _exptl_crystal_size_max 0.391 _exptl_crystal_size_mid 0.157 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.692 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.061 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 899 _refine_ls_number_reflns 14515 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.039 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0579 _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^)+(0.0854P)^2^+1.6738P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1521 _refine_ls_wR_factor_ref 0.1668 _reflns_Friedel_coverage 0.000 _reflns_number_gt 11103 _reflns_number_total 14515 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc05739k3.cif _cod_data_source_block ph08ph _cod_database_code 7123980 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.563 _shelx_estimated_absorpt_t_max 0.879 _oxdiff_exptl_absorpt_empirical_full_min 0.507 _oxdiff_exptl_absorpt_empirical_full_max 2.155 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P-1 CELL 1.54184 13.5450 14.3760 19.5043 99.475 93.788 109.582 ZERR 2.00 0.0006 0.0010 0.0008 0.004 0.004 0.004 LATT 1 SFAC C H B N F P CL D UNIT 150 142 2 8 30 4 2 6 MERG 2 FMAP 2 PLAN 20 SIZE 0.080 0.157 0.391 ACTA CONF LIST 6 L.S. 30 TEMP -173.00 WGHT 0.085400 1.673800 FVAR 3.60089 C1 1 0.399160 0.620948 0.736401 11.00000 0.02529 0.02466 = 0.02388 0.00381 0.00296 0.00840 C2 1 0.520386 0.754093 0.702904 11.00000 0.02179 0.02723 = 0.02516 0.00429 0.00291 0.00782 C101 1 1.070781 0.957836 1.020112 11.00000 0.08873 0.08751 = 0.16065 0.03281 -0.05928 0.00890 AFIX 43 D101 8 1.120749 0.929391 1.034521 11.00000 -1.20000 AFIX 0 C102 1 1.033984 1.013950 1.070517 11.00000 0.11937 0.09242 = 0.12770 0.01460 -0.05068 0.02228 AFIX 43 D102 8 1.057611 1.022032 1.118814 11.00000 -1.20000 AFIX 0 C100 1 1.035939 0.942628 0.949267 11.00000 0.09681 0.08734 = 0.14294 0.02078 -0.04112 0.00749 AFIX 43 D100 8 1.060191 0.902907 0.915314 11.00000 -1.20000 AFIX 0 C3 1 0.523962 0.665354 0.668036 11.00000 0.02628 0.03007 = 0.02712 0.00501 0.00705 0.01153 AFIX 43 H3 2 0.570626 0.659654 0.634623 11.00000 -1.20000 AFIX 0 C4 1 0.387070 0.788028 0.782099 11.00000 0.03294 0.02440 = 0.02892 0.00436 0.00962 0.01106 C5 1 0.298768 0.795192 0.743821 11.00000 0.03790 0.03281 = 0.03591 0.01036 0.01364 0.01870 C6 1 0.252673 0.861643 0.776034 11.00000 0.05632 0.04997 = 0.05171 0.01632 0.02098 0.03730 AFIX 43 H6 2 0.192544 0.867606 0.751850 11.00000 -1.20000 AFIX 0 C7 1 0.293142 0.918951 0.842604 11.00000 0.07900 0.04942 = 0.05300 0.01004 0.02949 0.04195 AFIX 43 H7 2 0.263063 0.966335 0.862669 11.00000 -1.20000 AFIX 0 C8 1 0.376801 0.907502 0.879805 11.00000 0.07320 0.04222 = 0.03852 -0.00044 0.01766 0.02786 AFIX 43 H8 2 0.402716 0.946317 0.925828 11.00000 -1.20000 AFIX 0 C9 1 0.424662 0.839932 0.851395 11.00000 0.04535 0.03036 = 0.03184 0.00232 0.01069 0.01253 C10 1 0.506858 0.822243 0.899914 11.00000 0.04205 0.03990 = 0.02666 0.00144 0.00512 0.00710 AFIX 13 H10 2 0.533979 0.772712 0.872723 11.00000 -1.20000 AFIX 0 C11 1 0.454521 0.777839 0.960334 11.00000 0.05097 0.05293 = 0.03203 0.00806 0.00961 0.01508 AFIX 137 H11A 2 0.428486 0.826165 0.987787 11.00000 -1.50000 H11B 2 0.506392 0.763848 0.990547 11.00000 -1.50000 H11C 2 0.395252 0.715140 0.941265 11.00000 -1.50000 AFIX 0 C12 1 0.600882 0.918898 0.931634 11.00000 0.06064 0.04606 = 0.03385 -0.00443 0.00683 0.00002 AFIX 137 H12A 2 0.640400 0.944320 0.894235 11.00000 -1.50000 H12B 2 0.647391 0.904089 0.965528 11.00000 -1.50000 H12C 2 0.574809 0.969918 0.955367 11.00000 -1.50000 AFIX 0 C13 1 0.250873 0.734241 0.671018 11.00000 0.02985 0.04218 = 0.03887 0.01016 0.00602 0.01944 AFIX 13 H13 2 0.303747 0.706601 0.650992 11.00000 -1.20000 AFIX 0 C14 1 0.151558 0.644828 0.675015 11.00000 0.03431 0.04625 = 0.06612 0.01242 0.00637 0.01605 AFIX 137 H14A 2 0.170484 0.601450 0.703289 11.00000 -1.50000 H14B 2 0.121107 0.606097 0.627636 11.00000 -1.50000 H14C 2 0.099669 0.669846 0.696673 11.00000 -1.50000 AFIX 0 C15 1 0.223645 0.796704 0.620637 11.00000 0.04038 0.05626 = 0.04924 0.01788 0.00028 0.02415 AFIX 137 H15A 2 0.164613 0.816578 0.635403 11.00000 -1.50000 H15B 2 0.203608 0.756163 0.572956 11.00000 -1.50000 H15C 2 0.285392 0.857111 0.621499 11.00000 -1.50000 AFIX 0 C16 1 0.431895 0.482012 0.653638 11.00000 0.04453 0.02566 = 0.04284 0.00716 0.02125 0.01387 C17 1 0.358321 0.442993 0.592886 11.00000 0.04377 0.03208 = 0.04038 -0.00518 0.01993 0.00245 C18 1 0.335291 0.342611 0.561735 11.00000 0.06531 0.03377 = 0.06791 -0.01101 0.03172 0.00482 AFIX 43 H18 2 0.284451 0.312796 0.521167 11.00000 -1.20000 AFIX 0 C19 1 0.385736 0.287082 0.589475 11.00000 0.08645 0.03586 = 0.09351 -0.00545 0.03985 0.01822 AFIX 43 H19 2 0.366604 0.217735 0.569008 11.00000 -1.20000 AFIX 0 C20 1 0.462812 0.327719 0.645664 11.00000 0.08862 0.04952 = 0.09736 0.02833 0.04880 0.04774 AFIX 43 H20 2 0.498191 0.287039 0.662018 11.00000 -1.20000 AFIX 0 C21 1 0.491036 0.429790 0.680108 11.00000 0.06406 0.04878 = 0.05694 0.01986 0.03057 0.03599 C22 1 0.583548 0.480146 0.737166 11.00000 0.08001 0.07769 = 0.05348 0.03027 0.02459 0.06036 AFIX 13 H22 2 0.573796 0.540972 0.764527 11.00000 -1.20000 AFIX 0 C23 1 0.686555 0.515336 0.704383 11.00000 0.06296 0.08023 = 0.05910 0.01958 0.01197 0.04755 AFIX 137 H23A 2 0.694400 0.457626 0.673775 11.00000 -1.50000 H23B 2 0.746713 0.544887 0.741632 11.00000 -1.50000 H23C 2 0.684225 0.565930 0.676841 11.00000 -1.50000 AFIX 0 C24 1 0.594001 0.412609 0.788216 11.00000 0.12198 0.13835 = 0.08828 0.07144 0.05128 0.10116 AFIX 137 H24A 2 0.527831 0.388467 0.808328 11.00000 -1.50000 H24B 2 0.651897 0.451213 0.825874 11.00000 -1.50000 H24C 2 0.608963 0.354934 0.763111 11.00000 -1.50000 AFIX 0 C25 1 0.306938 0.504573 0.558116 11.00000 0.04421 0.04712 = 0.03125 -0.00317 0.00384 0.00619 AFIX 13 H25 2 0.318835 0.568561 0.592239 11.00000 -1.20000 AFIX 0 C26 1 0.360299 0.532507 0.493264 11.00000 0.06509 0.06312 = 0.04128 0.00564 0.01623 0.00998 AFIX 137 H26A 2 0.436206 0.568735 0.507337 11.00000 -1.50000 H26B 2 0.329174 0.575561 0.472464 11.00000 -1.50000 H26C 2 0.349435 0.470980 0.458770 11.00000 -1.50000 AFIX 0 C27 1 0.187906 0.452310 0.537076 11.00000 0.04778 0.07124 = 0.05205 0.00894 -0.00047 0.00251 AFIX 137 H27A 2 0.174188 0.391267 0.501447 11.00000 -1.50000 H27B 2 0.158797 0.497977 0.517945 11.00000 -1.50000 H27C 2 0.154334 0.434143 0.578332 11.00000 -1.50000 AFIX 0 C28 1 0.617966 0.964603 0.745905 11.00000 0.03216 0.02960 = 0.03412 0.00542 0.00865 0.00355 C29 1 0.533632 0.998110 0.739888 11.00000 0.04064 0.02675 = 0.03505 0.00578 0.00616 0.00608 C30 1 0.529928 1.085804 0.779596 11.00000 0.05056 0.03559 = 0.04976 0.00998 0.01422 0.02007 C31 1 0.615224 1.145439 0.828585 11.00000 0.06142 0.02856 = 0.04267 -0.00102 0.01124 0.01103 C32 1 0.702291 1.118713 0.835455 11.00000 0.04267 0.03674 = 0.04064 -0.00040 0.00669 0.00274 C33 1 0.703441 1.031059 0.794353 11.00000 0.03526 0.03491 = 0.03714 0.00107 0.00766 0.00371 C34 1 0.720425 0.830784 0.704417 11.00000 0.02379 0.03459 = 0.03791 0.00138 0.00502 0.00436 C35 1 0.746194 0.807395 0.768342 11.00000 0.02575 0.04988 = 0.03900 0.00366 0.00418 0.01168 C36 1 0.826106 0.771723 0.783718 11.00000 0.03488 0.07336 = 0.04616 0.01182 0.00357 0.02253 C37 1 0.887688 0.757222 0.732363 11.00000 0.03145 0.08253 = 0.05846 0.00879 0.00131 0.02907 C38 1 0.866440 0.777124 0.668118 11.00000 0.02837 0.06045 = 0.04816 -0.00057 0.00931 0.01527 C39 1 0.784538 0.812636 0.654963 11.00000 0.03018 0.04082 = 0.03505 -0.00015 0.00480 0.00851 C40 1 0.596087 0.884651 0.613590 11.00000 0.03397 0.03011 = 0.03315 0.00733 0.01137 0.01240 C41 1 0.510231 0.836658 0.562374 11.00000 0.03685 0.03420 = 0.03366 0.01066 0.01243 0.01671 C42 1 0.501912 0.864023 0.497954 11.00000 0.04229 0.04832 = 0.03309 0.00826 0.00593 0.02546 C43 1 0.583497 0.942825 0.482761 11.00000 0.06366 0.04744 = 0.04114 0.02335 0.02497 0.03632 C44 1 0.669460 0.993497 0.531365 11.00000 0.05351 0.03445 = 0.05189 0.01624 0.02493 0.01755 C45 1 0.674529 0.965812 0.595446 11.00000 0.04465 0.03538 = 0.04278 0.01100 0.01661 0.01478 C46 1 0.126383 0.357603 0.778398 11.00000 0.03349 0.03522 = 0.03487 0.00797 0.00209 0.00728 C47 1 -0.025505 0.235518 0.788295 11.00000 0.03713 0.05263 = 0.04900 0.01156 0.00503 -0.00704 AFIX 43 H47 2 -0.087848 0.177385 0.776445 11.00000 -1.20000 AFIX 0 C48 1 0.011548 0.294226 0.851781 11.00000 0.04371 0.06198 = 0.04611 0.01530 0.01153 -0.00269 AFIX 43 H48 2 -0.020121 0.285823 0.893442 11.00000 -1.20000 AFIX 0 C49 1 0.033948 0.232333 0.669371 11.00000 0.02827 0.03318 = 0.03800 0.00469 -0.00127 0.00207 C50 1 0.077461 0.158194 0.650158 11.00000 0.02974 0.03375 = 0.05989 0.00608 0.00274 0.00344 C51 1 0.070476 0.119523 0.579101 11.00000 0.05024 0.03543 = 0.06753 -0.00102 0.01304 0.00754 AFIX 43 H51 2 0.100043 0.069360 0.564512 11.00000 -1.20000 AFIX 0 C52 1 0.021845 0.152695 0.530343 11.00000 0.05933 0.04437 = 0.04995 -0.00589 0.00428 0.00142 AFIX 43 H52 2 0.019293 0.126663 0.481960 11.00000 -1.20000 AFIX 0 C53 1 -0.024413 0.224517 0.550405 11.00000 0.05166 0.05012 = 0.04430 0.00753 -0.01163 0.00547 AFIX 43 H53 2 -0.059655 0.245374 0.515462 11.00000 -1.20000 AFIX 0 C54 1 -0.019857 0.266136 0.620654 11.00000 0.03265 0.03484 = 0.04794 0.00235 -0.01102 0.00469 C55 1 -0.072862 0.341108 0.644839 11.00000 0.04396 0.04607 = 0.06666 0.00380 -0.01203 0.01724 AFIX 13 H55 2 -0.028097 0.389165 0.687478 11.00000 -1.20000 AFIX 0 C56 1 -0.182476 0.286096 0.665598 11.00000 0.05933 0.07710 = 0.09789 0.02338 0.01817 0.04066 AFIX 137 H56A 2 -0.227385 0.237510 0.624757 11.00000 -1.50000 H56B 2 -0.215438 0.335366 0.682086 11.00000 -1.50000 H56C 2 -0.174068 0.250549 0.703107 11.00000 -1.50000 AFIX 0 C57 1 -0.086858 0.402123 0.590601 11.00000 0.04836 0.05869 = 0.09924 0.02470 -0.01223 0.02135 AFIX 137 H57A 2 -0.019474 0.430983 0.572844 11.00000 -1.50000 H57B 2 -0.109917 0.456511 0.612314 11.00000 -1.50000 H57C 2 -0.140200 0.358175 0.551710 11.00000 -1.50000 AFIX 0 C58 1 0.126883 0.117157 0.705159 11.00000 0.04331 0.04164 = 0.08404 0.01813 -0.00405 0.01314 AFIX 13 H58 2 0.142102 0.165689 0.750915 11.00000 -1.20000 AFIX 0 C59 1 0.229525 0.103000 0.687838 11.00000 0.04678 0.09913 = 0.19681 0.08897 0.02651 0.03188 AFIX 137 H59A 2 0.217892 0.061360 0.640842 11.00000 -1.50000 H59B 2 0.252912 0.069662 0.722259 11.00000 -1.50000 H59C 2 0.283847 0.168867 0.689261 11.00000 -1.50000 AFIX 0 C60 1 0.048468 0.016002 0.713846 11.00000 0.05539 0.06228 = 0.10312 0.04097 0.01673 0.02099 AFIX 137 H60A 2 -0.017359 0.024541 0.726223 11.00000 -1.50000 H60B 2 0.078871 -0.008259 0.751135 11.00000 -1.50000 H60C 2 0.033668 -0.033067 0.669742 11.00000 -1.50000 AFIX 0 C61 1 0.172095 0.438001 0.906835 11.00000 0.04039 0.04373 = 0.03064 0.01016 0.00804 0.00260 C62 1 0.237679 0.401782 0.945307 11.00000 0.05446 0.04328 = 0.03422 0.01250 0.00606 0.00760 C63 1 0.298301 0.465968 1.006242 11.00000 0.06626 0.04660 = 0.03497 0.01132 -0.00316 0.01381 AFIX 43 H63 2 0.344117 0.444572 1.033591 11.00000 -1.20000 AFIX 0 C64 1 0.292606 0.559878 1.027256 11.00000 0.07808 0.04588 = 0.03236 0.01083 0.00355 0.00988 AFIX 43 H64 2 0.335247 0.602973 1.068627 11.00000 -1.20000 AFIX 0 C65 1 0.225228 0.592600 0.988733 11.00000 0.06473 0.04314 = 0.03909 0.01212 0.01445 0.01226 AFIX 43 H65 2 0.221325 0.657203 1.004747 11.00000 -1.20000 AFIX 0 C66 1 0.163293 0.532124 0.926974 11.00000 0.04555 0.05180 = 0.03714 0.01762 0.01570 0.01311 C67 1 0.088275 0.566781 0.884584 11.00000 0.04695 0.06822 = 0.04796 0.02304 0.01649 0.02122 AFIX 13 H67 2 0.082117 0.533822 0.834387 11.00000 -1.20000 AFIX 0 C68 1 0.128680 0.680533 0.888467 11.00000 0.06633 0.07381 = 0.05940 0.02641 0.02174 0.03812 AFIX 137 H68A 2 0.129325 0.715005 0.936317 11.00000 -1.50000 H68B 2 0.082129 0.697423 0.855905 11.00000 -1.50000 H68C 2 0.200510 0.702150 0.875673 11.00000 -1.50000 AFIX 0 C69 1 -0.022824 0.531895 0.906988 11.00000 0.05385 0.11179 = 0.09039 0.05110 0.03228 0.03391 AFIX 137 H69A 2 -0.049919 0.458324 0.900989 11.00000 -1.50000 H69B 2 -0.070050 0.552952 0.877931 11.00000 -1.50000 H69C 2 -0.019372 0.562155 0.956336 11.00000 -1.50000 AFIX 0 C70 1 0.242269 0.296423 0.924085 11.00000 0.06807 0.04530 = 0.04678 0.01275 0.00234 0.01820 AFIX 13 H70 2 0.184329 0.258623 0.884632 11.00000 -1.20000 AFIX 0 C71 1 0.223036 0.238379 0.983723 11.00000 0.13150 0.05938 = 0.07727 0.03440 0.02936 0.03019 AFIX 137 H71A 2 0.281909 0.270373 1.021715 11.00000 -1.50000 H71B 2 0.217795 0.168700 0.966389 11.00000 -1.50000 H71C 2 0.157058 0.238806 1.001347 11.00000 -1.50000 AFIX 0 C72 1 0.345604 0.299794 0.897529 11.00000 0.08721 0.05790 = 0.11575 0.02899 0.02466 0.03868 AFIX 137 H72A 2 0.351648 0.328016 0.854900 11.00000 -1.50000 H72B 2 0.347538 0.231428 0.886967 11.00000 -1.50000 H72C 2 0.404571 0.342123 0.933516 11.00000 -1.50000 AFIX 0 B1 3 0.612189 0.860803 0.692813 11.00000 0.02437 0.02776 = 0.03192 0.00473 0.00673 0.00603 N1 4 0.439478 0.724104 0.745133 11.00000 0.02461 0.02449 = 0.02526 0.00371 0.00514 0.00893 N2 4 0.451515 0.585800 0.687567 11.00000 0.02837 0.02545 = 0.02668 0.00312 0.00504 0.01212 N3 4 0.104897 0.369847 0.845748 11.00000 0.03728 0.04592 = 0.03650 0.01121 0.00587 -0.00105 N4 4 0.044307 0.275629 0.743179 11.00000 0.03194 0.03924 = 0.03665 0.00837 0.00144 0.00129 F1 5 0.449390 0.944021 0.691904 11.00000 0.03809 0.03565 = 0.04159 0.00831 0.00376 0.01452 F2 5 0.445219 1.112988 0.770607 11.00000 0.06795 0.04456 = 0.06907 0.00464 0.00684 0.03296 F3 5 0.611708 1.229976 0.869046 11.00000 0.08192 0.03678 = 0.05932 -0.00779 0.01241 0.02063 F4 5 0.785879 1.176245 0.883562 11.00000 0.04947 0.04856 = 0.05112 -0.01322 0.00128 -0.00006 F5 5 0.794794 1.012566 0.804084 11.00000 0.02897 0.05026 = 0.04865 -0.00534 0.00312 0.00594 F6 5 0.687506 0.817529 0.820501 11.00000 0.03528 0.06741 = 0.03818 0.01323 0.00790 0.02242 F7 5 0.842535 0.748317 0.846434 11.00000 0.05633 0.11221 = 0.05167 0.02520 0.00389 0.04994 F8 5 0.965566 0.722174 0.745978 11.00000 0.05259 0.14479 = 0.07187 0.02240 0.00846 0.06642 F9 5 0.924779 0.761322 0.617215 11.00000 0.04017 0.08144 = 0.05542 0.00186 0.01463 0.02915 F10 5 0.769945 0.826454 0.588877 11.00000 0.04216 0.05334 = 0.03693 0.00253 0.01193 0.01924 F11 5 0.426775 0.759059 0.572458 11.00000 0.03109 0.04696 = 0.03460 0.01125 0.00259 0.00953 F12 5 0.415788 0.813590 0.450616 11.00000 0.05099 0.07598 = 0.03788 0.01751 0.00593 0.03442 F13 5 0.576727 0.967087 0.418845 11.00000 0.08103 0.07137 = 0.04606 0.03365 0.02803 0.04793 F14 5 0.748956 1.070030 0.516276 11.00000 0.07173 0.04617 = 0.06623 0.02847 0.03355 0.01218 F15 5 0.762295 1.018180 0.641223 11.00000 0.04500 0.03681 = 0.05099 0.00549 0.01371 -0.00281 P1 6 0.311648 0.557912 0.796761 11.00000 0.02957 0.02822 = 0.02816 0.00672 0.00658 0.00861 P2 6 0.236470 0.411555 0.731750 11.00000 0.03141 0.02854 = 0.03224 0.00524 0.00483 0.00586 CL1 7 0.442902 0.554071 0.864701 11.00000 0.04053 0.04275 = 0.03415 0.00976 -0.00021 0.01281 HKLF 4 REM shelxt_a.res in P-1 REM R1 = 0.0579 for 11103 Fo > 4sig(Fo) and 0.0773 for all 14515 data REM 899 parameters refined using 0 restraints END WGHT 0.0854 1.6760 REM Highest difference peak 0.692, deepest hole -0.440, 1-sigma level 0.061 Q1 1 0.0197 0.2021 0.9381 11.00000 0.05 0.69 Q2 1 0.5064 0.9084 0.3946 11.00000 0.05 0.59 Q3 1 0.6816 1.0411 0.4832 11.00000 0.05 0.56 Q4 1 0.8595 0.8329 0.8580 11.00000 0.05 0.48 Q5 1 0.5599 1.2407 0.8321 11.00000 0.05 0.45 Q6 1 0.3751 1.0845 0.7505 11.00000 0.05 0.44 Q7 1 0.3663 0.7521 0.4422 11.00000 0.05 0.44 Q8 1 0.6855 0.8788 0.8204 11.00000 0.05 0.44 Q9 1 0.7518 1.2178 0.8448 11.00000 0.05 0.43 Q10 1 0.7788 1.0568 0.7722 11.00000 0.05 0.40 Q11 1 0.7080 1.0250 0.6183 11.00000 0.05 0.40 Q12 1 0.1852 0.4320 0.7231 11.00000 0.05 0.39 Q13 1 0.3187 0.3131 0.7663 11.00000 0.05 0.36 Q14 1 0.5585 0.7996 0.7014 11.00000 0.05 0.36 Q15 1 -0.0419 0.1580 0.5335 11.00000 0.05 0.36 Q16 1 -0.0828 0.2149 0.5738 11.00000 0.05 0.36 Q17 1 0.5398 0.8708 0.5934 11.00000 0.05 0.35 Q18 1 -0.1810 0.1421 0.7764 11.00000 0.05 0.34 Q19 1 0.6671 1.1389 0.8012 11.00000 0.05 0.32 Q20 1 0.9141 0.8039 0.5828 11.00000 0.05 0.32 ; _shelx_res_checksum 65855 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 C1 C 0.39916(17) 0.62095(17) 0.73640(11) 0.0248(4) Uani 1 1 d . . C2 C 0.52039(17) 0.75409(18) 0.70290(11) 0.0251(4) Uani 1 1 d . . C101 C 1.0708(5) 0.9578(5) 1.0201(4) 0.121(3) Uani 1 1 d . . D101 D 1.1207 0.9294 1.0345 0.145 Uiso 1 1 calc R U C102 C 1.0340(6) 1.0139(5) 1.0705(4) 0.121(2) Uani 1 1 d . . D102 D 1.0576 1.0220 1.1188 0.145 Uiso 1 1 calc R U C100 C 1.0359(5) 0.9426(5) 0.9493(4) 0.118(2) Uani 1 1 d . . D100 D 1.0602 0.9029 0.9153 0.142 Uiso 1 1 calc R U C3 C 0.52396(18) 0.66535(18) 0.66804(12) 0.0273(4) Uani 1 1 d . . H3 H 0.5706 0.6597 0.6346 0.033 Uiso 1 1 calc R U C4 C 0.38707(19) 0.78803(18) 0.78210(12) 0.0283(5) Uani 1 1 d . . C5 C 0.2988(2) 0.7952(2) 0.74382(13) 0.0331(5) Uani 1 1 d . . C6 C 0.2527(3) 0.8616(2) 0.77603(16) 0.0464(7) Uani 1 1 d . . H6 H 0.1925 0.8676 0.7519 0.056 Uiso 1 1 calc R U C7 C 0.2931(3) 0.9190(3) 0.84260(17) 0.0545(8) Uani 1 1 d . . H7 H 0.2631 0.9663 0.8627 0.065 Uiso 1 1 calc R U C8 C 0.3768(3) 0.9075(2) 0.87981(16) 0.0499(7) Uani 1 1 d . . H8 H 0.4027 0.9463 0.9258 0.060 Uiso 1 1 calc R U C9 C 0.4247(2) 0.8399(2) 0.85140(13) 0.0362(5) Uani 1 1 d . . C10 C 0.5069(2) 0.8222(2) 0.89991(13) 0.0387(6) Uani 1 1 d . . H10 H 0.5340 0.7727 0.8727 0.046 Uiso 1 1 calc R U C11 C 0.4545(3) 0.7778(3) 0.96033(14) 0.0460(7) Uani 1 1 d . . H11A H 0.4285 0.8262 0.9878 0.069 Uiso 1 1 calc R U H11B H 0.5064 0.7638 0.9905 0.069 Uiso 1 1 calc R U H11C H 0.3953 0.7151 0.9413 0.069 Uiso 1 1 calc R U C12 C 0.6009(3) 0.9189(3) 0.93163(15) 0.0532(8) Uani 1 1 d . . H12A H 0.6404 0.9443 0.8942 0.080 Uiso 1 1 calc R U H12B H 0.6474 0.9041 0.9655 0.080 Uiso 1 1 calc R U H12C H 0.5748 0.9699 0.9554 0.080 Uiso 1 1 calc R U C13 C 0.2509(2) 0.7342(2) 0.67102(14) 0.0349(5) Uani 1 1 d . . H13 H 0.3037 0.7066 0.6510 0.042 Uiso 1 1 calc R U C14 C 0.1516(2) 0.6448(2) 0.67501(18) 0.0483(7) Uani 1 1 d . . H14A H 0.1705 0.6015 0.7033 0.072 Uiso 1 1 calc R U H14B H 0.1211 0.6061 0.6276 0.072 Uiso 1 1 calc R U H14C H 0.0997 0.6698 0.6967 0.072 Uiso 1 1 calc R U C15 C 0.2236(2) 0.7967(3) 0.62064(16) 0.0461(7) Uani 1 1 d . . H15A H 0.1646 0.8166 0.6354 0.069 Uiso 1 1 calc R U H15B H 0.2036 0.7562 0.5730 0.069 Uiso 1 1 calc R U H15C H 0.2854 0.8571 0.6215 0.069 Uiso 1 1 calc R U C16 C 0.4319(2) 0.48201(19) 0.65364(14) 0.0365(6) Uani 1 1 d . . C17 C 0.3583(2) 0.4430(2) 0.59289(15) 0.0424(6) Uani 1 1 d . . C18 C 0.3353(3) 0.3426(2) 0.5617(2) 0.0604(10) Uani 1 1 d . . H18 H 0.2845 0.3128 0.5212 0.072 Uiso 1 1 calc R U C19 C 0.3857(4) 0.2871(3) 0.5895(3) 0.0737(12) Uani 1 1 d . . H19 H 0.3666 0.2177 0.5690 0.088 Uiso 1 1 calc R U C20 C 0.4628(4) 0.3277(3) 0.6457(2) 0.0690(12) Uani 1 1 d . . H20 H 0.4982 0.2870 0.6620 0.083 Uiso 1 1 calc R U C21 C 0.4910(3) 0.4298(3) 0.68011(18) 0.0502(8) Uani 1 1 d . . C22 C 0.5835(3) 0.4801(3) 0.73717(18) 0.0591(9) Uani 1 1 d . . H22 H 0.5738 0.5410 0.7645 0.071 Uiso 1 1 calc R U C23 C 0.6866(3) 0.5153(3) 0.70438(19) 0.0607(9) Uani 1 1 d . . H23A H 0.6944 0.4576 0.6738 0.091 Uiso 1 1 calc R U H23B H 0.7467 0.5449 0.7416 0.091 Uiso 1 1 calc R U H23C H 0.6842 0.5659 0.6768 0.091 Uiso 1 1 calc R U C24 C 0.5940(4) 0.4126(4) 0.7882(3) 0.0941(18) Uani 1 1 d . . H24A H 0.5278 0.3885 0.8083 0.141 Uiso 1 1 calc R U H24B H 0.6519 0.4512 0.8259 0.141 Uiso 1 1 calc R U H24C H 0.6090 0.3549 0.7631 0.141 Uiso 1 1 calc R U C25 C 0.3069(2) 0.5046(2) 0.55812(14) 0.0448(7) Uani 1 1 d . . H25 H 0.3188 0.5686 0.5922 0.054 Uiso 1 1 calc R U C26 C 0.3603(3) 0.5325(3) 0.49326(17) 0.0599(9) Uani 1 1 d . . H26A H 0.4362 0.5687 0.5073 0.090 Uiso 1 1 calc R U H26B H 0.3292 0.5756 0.4725 0.090 Uiso 1 1 calc R U H26C H 0.3494 0.4710 0.4588 0.090 Uiso 1 1 calc R U C27 C 0.1879(3) 0.4523(3) 0.53708(19) 0.0625(9) Uani 1 1 d . . H27A H 0.1742 0.3913 0.5014 0.094 Uiso 1 1 calc R U H27B H 0.1588 0.4980 0.5179 0.094 Uiso 1 1 calc R U H27C H 0.1543 0.4341 0.5783 0.094 Uiso 1 1 calc R U C28 C 0.6180(2) 0.96460(19) 0.74590(13) 0.0338(5) Uani 1 1 d . . C29 C 0.5336(2) 0.99811(19) 0.73989(13) 0.0356(5) Uani 1 1 d . . C30 C 0.5299(2) 1.0858(2) 0.77960(16) 0.0435(6) Uani 1 1 d . . C31 C 0.6152(3) 1.1454(2) 0.82859(16) 0.0462(7) Uani 1 1 d . . C32 C 0.7023(2) 1.1187(2) 0.83545(15) 0.0438(6) Uani 1 1 d . . C33 C 0.7034(2) 1.0311(2) 0.79435(14) 0.0386(6) Uani 1 1 d . . C34 C 0.72043(19) 0.8308(2) 0.70442(14) 0.0343(5) Uani 1 1 d . . C35 C 0.7462(2) 0.8074(2) 0.76834(14) 0.0393(6) Uani 1 1 d . . C36 C 0.8261(2) 0.7717(3) 0.78372(17) 0.0506(7) Uani 1 1 d . . C37 C 0.8877(2) 0.7572(3) 0.73236(18) 0.0560(9) Uani 1 1 d . . C38 C 0.8664(2) 0.7771(3) 0.66812(16) 0.0469(7) Uani 1 1 d . . C39 C 0.7845(2) 0.8126(2) 0.65496(14) 0.0373(6) Uani 1 1 d . . C40 C 0.5961(2) 0.88465(19) 0.61359(13) 0.0317(5) Uani 1 1 d . . C41 C 0.5102(2) 0.8367(2) 0.56237(13) 0.0330(5) Uani 1 1 d . . C42 C 0.5019(2) 0.8640(2) 0.49795(14) 0.0387(6) Uani 1 1 d . . C43 C 0.5835(3) 0.9428(2) 0.48276(15) 0.0438(7) Uani 1 1 d . . C44 C 0.6695(3) 0.9935(2) 0.53136(16) 0.0443(7) Uani 1 1 d . . C45 C 0.6745(2) 0.9658(2) 0.59545(15) 0.0398(6) Uani 1 1 d . . C46 C 0.1264(2) 0.3576(2) 0.77840(13) 0.0358(5) Uani 1 1 d . . C47 C -0.0255(2) 0.2355(3) 0.78829(17) 0.0520(8) Uani 1 1 d . . H47 H -0.0878 0.1774 0.7764 0.062 Uiso 1 1 calc R U C48 C 0.0115(3) 0.2942(3) 0.85178(17) 0.0553(8) Uani 1 1 d . . H48 H -0.0201 0.2858 0.8934 0.066 Uiso 1 1 calc R U C49 C 0.0339(2) 0.2323(2) 0.66937(14) 0.0360(5) Uani 1 1 d . . C50 C 0.0775(2) 0.1582(2) 0.65016(17) 0.0437(6) Uani 1 1 d . . C51 C 0.0705(3) 0.1195(2) 0.57910(19) 0.0541(8) Uani 1 1 d . . H51 H 0.1000 0.0694 0.5645 0.065 Uiso 1 1 calc R U C52 C 0.0218(3) 0.1527(3) 0.53034(18) 0.0576(8) Uani 1 1 d . . H52 H 0.0193 0.1267 0.4820 0.069 Uiso 1 1 calc R U C53 C -0.0244(3) 0.2245(3) 0.55040(17) 0.0530(8) Uani 1 1 d . . H53 H -0.0597 0.2454 0.5155 0.064 Uiso 1 1 calc R U C54 C -0.0199(2) 0.2661(2) 0.62065(16) 0.0418(6) Uani 1 1 d . . C55 C -0.0729(3) 0.3411(3) 0.64484(19) 0.0537(8) Uani 1 1 d . . H55 H -0.0281 0.3892 0.6875 0.064 Uiso 1 1 calc R U C56 C -0.1825(3) 0.2861(3) 0.6656(3) 0.0727(11) Uani 1 1 d . . H56A H -0.2274 0.2375 0.6248 0.109 Uiso 1 1 calc R U H56B H -0.2154 0.3354 0.6821 0.109 Uiso 1 1 calc R U H56C H -0.1741 0.2505 0.7031 0.109 Uiso 1 1 calc R U C57 C -0.0869(3) 0.4021(3) 0.5906(2) 0.0681(11) Uani 1 1 d . . H57A H -0.0195 0.4310 0.5728 0.102 Uiso 1 1 calc R U H57B H -0.1099 0.4565 0.6123 0.102 Uiso 1 1 calc R U H57C H -0.1402 0.3582 0.5517 0.102 Uiso 1 1 calc R U C58 C 0.1269(3) 0.1172(3) 0.7052(2) 0.0567(8) Uani 1 1 d . . H58 H 0.1421 0.1657 0.7509 0.068 Uiso 1 1 calc R U C59 C 0.2295(3) 0.1030(4) 0.6878(4) 0.105(2) Uani 1 1 d . . H59A H 0.2179 0.0614 0.6408 0.157 Uiso 1 1 calc R U H59B H 0.2529 0.0697 0.7223 0.157 Uiso 1 1 calc R U H59C H 0.2838 0.1689 0.6893 0.157 Uiso 1 1 calc R U C60 C 0.0485(3) 0.0160(3) 0.7138(3) 0.0702(11) Uani 1 1 d . . H60A H -0.0174 0.0245 0.7262 0.105 Uiso 1 1 calc R U H60B H 0.0789 -0.0083 0.7511 0.105 Uiso 1 1 calc R U H60C H 0.0337 -0.0331 0.6697 0.105 Uiso 1 1 calc R U C61 C 0.1721(2) 0.4380(2) 0.90684(14) 0.0409(6) Uani 1 1 d . . C62 C 0.2377(3) 0.4018(2) 0.94531(15) 0.0459(7) Uani 1 1 d . . C63 C 0.2983(3) 0.4660(2) 1.00624(15) 0.0509(7) Uani 1 1 d . . H63 H 0.3441 0.4446 1.0336 0.061 Uiso 1 1 calc R U C64 C 0.2926(3) 0.5599(3) 1.02726(15) 0.0550(8) Uani 1 1 d . . H64 H 0.3352 0.6030 1.0686 0.066 Uiso 1 1 calc R U C65 C 0.2252(3) 0.5926(3) 0.98873(16) 0.0499(7) Uani 1 1 d . . H65 H 0.2213 0.6572 1.0047 0.060 Uiso 1 1 calc R U C66 C 0.1633(2) 0.5321(2) 0.92697(15) 0.0443(6) Uani 1 1 d . . C67 C 0.0883(3) 0.5668(3) 0.88458(17) 0.0522(8) Uani 1 1 d . . H67 H 0.0821 0.5338 0.8344 0.063 Uiso 1 1 calc R U C68 C 0.1287(3) 0.6805(3) 0.8885(2) 0.0608(9) Uani 1 1 d . . H68A H 0.1293 0.7150 0.9363 0.091 Uiso 1 1 calc R U H68B H 0.0821 0.6974 0.8559 0.091 Uiso 1 1 calc R U H68C H 0.2005 0.7022 0.8757 0.091 Uiso 1 1 calc R U C69 C -0.0228(3) 0.5319(4) 0.9070(3) 0.0792(13) Uani 1 1 d . . H69A H -0.0499 0.4583 0.9010 0.119 Uiso 1 1 calc R U H69B H -0.0701 0.5530 0.8779 0.119 Uiso 1 1 calc R U H69C H -0.0194 0.5622 0.9563 0.119 Uiso 1 1 calc R U C70 C 0.2423(3) 0.2964(3) 0.92409(17) 0.0536(8) Uani 1 1 d . . H70 H 0.1843 0.2586 0.8846 0.064 Uiso 1 1 calc R U C71 C 0.2230(5) 0.2384(3) 0.9837(2) 0.0870(15) Uani 1 1 d . . H71A H 0.2819 0.2704 1.0217 0.130 Uiso 1 1 calc R U H71B H 0.2178 0.1687 0.9664 0.130 Uiso 1 1 calc R U H71C H 0.1571 0.2388 1.0013 0.130 Uiso 1 1 calc R U C72 C 0.3456(4) 0.2998(3) 0.8975(3) 0.0816(13) Uani 1 1 d . . H72A H 0.3516 0.3280 0.8549 0.122 Uiso 1 1 calc R U H72B H 0.3475 0.2314 0.8870 0.122 Uiso 1 1 calc R U H72C H 0.4046 0.3421 0.9335 0.122 Uiso 1 1 calc R U B1 B 0.6122(2) 0.8608(2) 0.69281(14) 0.0288(5) Uani 1 1 d . . N1 N 0.43948(15) 0.72410(14) 0.74513(9) 0.0248(4) Uani 1 1 d . . N2 N 0.45152(15) 0.58580(15) 0.68757(10) 0.0263(4) Uani 1 1 d . . N3 N 0.10490(19) 0.3698(2) 0.84575(12) 0.0435(5) Uani 1 1 d . . N4 N 0.04431(18) 0.27563(18) 0.74318(12) 0.0389(5) Uani 1 1 d . . F1 F 0.44939(12) 0.94402(12) 0.69190(8) 0.0380(3) Uani 1 1 d . . F2 F 0.44522(17) 1.11299(14) 0.77061(11) 0.0580(5) Uani 1 1 d . . F3 F 0.61171(18) 1.22998(14) 0.86905(11) 0.0614(5) Uani 1 1 d . . F4 F 0.78588(15) 1.17624(15) 0.88356(10) 0.0573(5) Uani 1 1 d . . F5 F 0.79479(12) 1.01257(14) 0.80408(9) 0.0466(4) Uani 1 1 d . . F6 F 0.68751(12) 0.81753(15) 0.82050(8) 0.0453(4) Uani 1 1 d . . F7 F 0.84254(16) 0.7483(2) 0.84643(10) 0.0672(6) Uani 1 1 d . . F8 F 0.96557(17) 0.7222(2) 0.74598(12) 0.0814(8) Uani 1 1 d . . F9 F 0.92478(14) 0.76132(17) 0.61721(10) 0.0580(5) Uani 1 1 d . . F10 F 0.76994(13) 0.82645(14) 0.58888(8) 0.0440(4) Uani 1 1 d . . F11 F 0.42678(12) 0.75906(13) 0.57246(8) 0.0383(3) Uani 1 1 d . . F12 F 0.41579(14) 0.81359(16) 0.45062(9) 0.0511(4) Uani 1 1 d . . F13 F 0.57673(17) 0.96709(16) 0.41884(9) 0.0571(5) Uani 1 1 d . . F14 F 0.74896(17) 1.07003(15) 0.51628(11) 0.0603(5) Uani 1 1 d . . F15 F 0.76230(14) 1.01818(13) 0.64122(9) 0.0488(4) Uani 1 1 d . . P1 P 0.31165(5) 0.55791(5) 0.79676(3) 0.02878(13) Uani 1 1 d . . P2 P 0.23647(5) 0.41156(5) 0.73175(3) 0.03200(14) Uani 1 1 d . . Cl1 Cl 0.44290(5) 0.55407(5) 0.86470(3) 0.03961(15) Uani 1 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0253(10) 0.0247(11) 0.0239(9) 0.0038(8) 0.0030(8) 0.0084(9) C2 0.0218(10) 0.0272(11) 0.0252(10) 0.0043(8) 0.0029(8) 0.0078(9) C101 0.089(4) 0.088(4) 0.161(6) 0.033(4) -0.059(4) 0.009(3) C102 0.119(5) 0.092(4) 0.128(5) 0.015(4) -0.051(4) 0.022(4) C100 0.097(4) 0.087(4) 0.143(6) 0.021(4) -0.041(4) 0.007(3) C3 0.0263(10) 0.0301(12) 0.0271(10) 0.0050(9) 0.0070(8) 0.0115(9) C4 0.0329(11) 0.0244(11) 0.0289(11) 0.0044(9) 0.0096(9) 0.0111(9) C5 0.0379(13) 0.0328(13) 0.0359(12) 0.0104(10) 0.0136(10) 0.0187(11) C6 0.0563(17) 0.0500(17) 0.0517(16) 0.0163(14) 0.0210(14) 0.0373(15) C7 0.079(2) 0.0494(18) 0.0530(17) 0.0100(14) 0.0295(16) 0.0420(18) C8 0.073(2) 0.0422(16) 0.0385(14) -0.0004(12) 0.0177(14) 0.0279(16) C9 0.0454(14) 0.0304(13) 0.0318(12) 0.0023(10) 0.0107(10) 0.0125(11) C10 0.0420(14) 0.0399(14) 0.0267(11) 0.0014(10) 0.0051(10) 0.0071(12) C11 0.0510(16) 0.0529(18) 0.0320(13) 0.0081(12) 0.0096(12) 0.0151(14) C12 0.0606(19) 0.0461(17) 0.0339(13) -0.0044(12) 0.0068(13) 0.0000(15) C13 0.0298(12) 0.0422(14) 0.0389(13) 0.0102(11) 0.0060(10) 0.0194(11) C14 0.0343(14) 0.0463(17) 0.0661(19) 0.0124(14) 0.0064(13) 0.0161(13) C15 0.0404(15) 0.0563(18) 0.0492(15) 0.0179(14) 0.0003(12) 0.0241(14) C16 0.0445(14) 0.0257(12) 0.0428(13) 0.0072(10) 0.0212(11) 0.0139(11) C17 0.0438(14) 0.0321(14) 0.0404(13) -0.0052(11) 0.0199(12) 0.0025(12) C18 0.065(2) 0.0338(16) 0.068(2) -0.0110(15) 0.0317(17) 0.0048(15) C19 0.086(3) 0.0359(18) 0.094(3) -0.0054(19) 0.040(3) 0.0182(19) C20 0.089(3) 0.050(2) 0.097(3) 0.028(2) 0.049(3) 0.048(2) C21 0.0641(19) 0.0488(18) 0.0569(17) 0.0199(14) 0.0306(15) 0.0360(16) C22 0.080(2) 0.078(2) 0.0535(18) 0.0303(17) 0.0246(17) 0.060(2) C23 0.063(2) 0.080(3) 0.0591(19) 0.0196(18) 0.0120(16) 0.048(2) C24 0.122(4) 0.138(5) 0.088(3) 0.071(3) 0.051(3) 0.101(4) C25 0.0442(15) 0.0471(17) 0.0312(12) -0.0032(11) 0.0038(11) 0.0062(13) C26 0.065(2) 0.063(2) 0.0413(16) 0.0056(15) 0.0162(15) 0.0100(18) C27 0.0478(18) 0.071(2) 0.0521(18) 0.0089(17) -0.0005(14) 0.0025(17) C28 0.0322(12) 0.0296(12) 0.0341(12) 0.0054(10) 0.0086(10) 0.0036(10) C29 0.0406(13) 0.0267(12) 0.0351(12) 0.0058(10) 0.0062(10) 0.0061(11) C30 0.0506(16) 0.0356(14) 0.0498(15) 0.0100(12) 0.0142(13) 0.0201(13) C31 0.0614(18) 0.0286(13) 0.0427(14) -0.0010(11) 0.0112(13) 0.0110(13) C32 0.0427(15) 0.0367(15) 0.0406(14) -0.0004(11) 0.0067(11) 0.0027(12) C33 0.0353(13) 0.0349(14) 0.0371(13) 0.0011(11) 0.0077(10) 0.0037(11) C34 0.0238(11) 0.0346(13) 0.0379(12) 0.0014(10) 0.0050(9) 0.0044(10) C35 0.0257(11) 0.0499(16) 0.0390(13) 0.0037(12) 0.0042(10) 0.0117(11) C36 0.0349(14) 0.073(2) 0.0462(15) 0.0118(15) 0.0036(12) 0.0225(15) C37 0.0314(14) 0.083(3) 0.0585(18) 0.0088(17) 0.0013(13) 0.0291(16) C38 0.0284(13) 0.0605(19) 0.0482(15) -0.0006(14) 0.0093(11) 0.0153(13) C39 0.0302(12) 0.0408(14) 0.0350(12) -0.0001(11) 0.0048(10) 0.0085(11) C40 0.0340(12) 0.0301(12) 0.0332(11) 0.0073(10) 0.0114(9) 0.0124(10) C41 0.0369(12) 0.0342(13) 0.0337(12) 0.0107(10) 0.0124(10) 0.0167(11) C42 0.0423(14) 0.0483(16) 0.0331(12) 0.0083(11) 0.0059(10) 0.0255(13) C43 0.0637(18) 0.0474(16) 0.0411(14) 0.0233(12) 0.0250(13) 0.0363(15) C44 0.0535(17) 0.0344(14) 0.0519(16) 0.0162(12) 0.0249(14) 0.0175(13) C45 0.0447(14) 0.0354(14) 0.0428(14) 0.0110(11) 0.0166(12) 0.0148(12) C46 0.0335(12) 0.0352(13) 0.0349(12) 0.0080(10) 0.0021(10) 0.0073(11) C47 0.0371(14) 0.0526(19) 0.0490(16) 0.0116(14) 0.0050(12) -0.0070(13) C48 0.0437(16) 0.062(2) 0.0461(16) 0.0153(15) 0.0115(13) -0.0027(15) C49 0.0283(11) 0.0332(13) 0.0380(13) 0.0047(10) -0.0013(10) 0.0021(10) C50 0.0297(12) 0.0337(14) 0.0599(17) 0.0061(13) 0.0027(12) 0.0034(11) C51 0.0502(17) 0.0354(15) 0.068(2) -0.0010(14) 0.0130(15) 0.0075(14) C52 0.0593(19) 0.0444(18) 0.0499(17) -0.0059(14) 0.0043(15) 0.0014(15) C53 0.0517(17) 0.0501(18) 0.0443(15) 0.0075(14) -0.0116(13) 0.0055(15) C54 0.0327(13) 0.0348(14) 0.0479(15) 0.0024(12) -0.0110(11) 0.0047(11) C55 0.0440(16) 0.0461(17) 0.067(2) 0.0038(15) -0.0120(14) 0.0172(14) C56 0.059(2) 0.077(3) 0.098(3) 0.023(2) 0.018(2) 0.041(2) C57 0.0484(18) 0.059(2) 0.099(3) 0.025(2) -0.0122(19) 0.0213(17) C58 0.0433(16) 0.0416(17) 0.084(2) 0.0181(17) -0.0040(16) 0.0131(14) C59 0.047(2) 0.099(4) 0.197(6) 0.089(4) 0.027(3) 0.032(2) C60 0.055(2) 0.062(2) 0.103(3) 0.041(2) 0.017(2) 0.0210(19) C61 0.0404(14) 0.0437(15) 0.0306(12) 0.0102(11) 0.0080(10) 0.0026(12) C62 0.0545(17) 0.0433(16) 0.0342(13) 0.0125(12) 0.0061(12) 0.0076(14) C63 0.066(2) 0.0466(17) 0.0350(14) 0.0113(13) -0.0032(13) 0.0138(15) C64 0.078(2) 0.0459(17) 0.0324(13) 0.0108(12) 0.0035(14) 0.0099(16) C65 0.0647(19) 0.0431(16) 0.0391(14) 0.0121(12) 0.0145(14) 0.0123(15) C66 0.0456(15) 0.0518(17) 0.0371(13) 0.0176(12) 0.0157(12) 0.0131(13) C67 0.0470(16) 0.068(2) 0.0480(16) 0.0230(15) 0.0165(13) 0.0212(16) C68 0.066(2) 0.074(2) 0.059(2) 0.0264(18) 0.0217(17) 0.038(2) C69 0.054(2) 0.112(4) 0.090(3) 0.051(3) 0.032(2) 0.034(2) C70 0.068(2) 0.0453(17) 0.0468(16) 0.0128(14) 0.0023(15) 0.0182(16) C71 0.132(4) 0.059(2) 0.077(3) 0.034(2) 0.029(3) 0.030(3) C72 0.087(3) 0.058(2) 0.116(4) 0.029(2) 0.025(3) 0.039(2) B1 0.0244(11) 0.0278(13) 0.0319(12) 0.0047(10) 0.0067(10) 0.0060(10) N1 0.0246(9) 0.0245(9) 0.0253(8) 0.0037(7) 0.0051(7) 0.0089(8) N2 0.0284(9) 0.0254(10) 0.0267(9) 0.0031(7) 0.0050(7) 0.0121(8) N3 0.0373(12) 0.0459(14) 0.0365(11) 0.0112(10) 0.0059(9) -0.0010(11) N4 0.0319(11) 0.0392(12) 0.0367(11) 0.0084(9) 0.0014(9) 0.0013(9) F1 0.0381(8) 0.0357(8) 0.0416(8) 0.0083(6) 0.0038(6) 0.0145(7) F2 0.0680(12) 0.0446(10) 0.0691(12) 0.0046(9) 0.0068(10) 0.0330(10) F3 0.0819(14) 0.0368(10) 0.0593(11) -0.0078(8) 0.0124(10) 0.0206(10) F4 0.0495(10) 0.0486(11) 0.0511(10) -0.0132(8) 0.0013(8) -0.0001(8) F5 0.0290(7) 0.0503(10) 0.0486(9) -0.0053(8) 0.0031(6) 0.0059(7) F6 0.0353(8) 0.0674(12) 0.0382(8) 0.0132(8) 0.0079(6) 0.0224(8) F7 0.0563(11) 0.1122(19) 0.0517(10) 0.0252(11) 0.0039(9) 0.0499(13) F8 0.0526(12) 0.145(2) 0.0719(14) 0.0224(15) 0.0085(10) 0.0664(15) F9 0.0402(9) 0.0814(14) 0.0554(10) 0.0019(10) 0.0146(8) 0.0291(10) F10 0.0422(8) 0.0533(10) 0.0369(8) 0.0025(7) 0.0119(7) 0.0192(8) F11 0.0311(7) 0.0470(9) 0.0346(7) 0.0112(6) 0.0026(6) 0.0095(7) F12 0.0510(10) 0.0760(13) 0.0379(8) 0.0175(8) 0.0059(7) 0.0344(10) F13 0.0810(13) 0.0714(13) 0.0461(9) 0.0337(9) 0.0280(9) 0.0479(11) F14 0.0717(13) 0.0462(10) 0.0662(12) 0.0285(9) 0.0335(10) 0.0122(10) F15 0.0450(9) 0.0368(9) 0.0510(9) 0.0055(7) 0.0137(7) -0.0028(7) P1 0.0296(3) 0.0282(3) 0.0282(3) 0.0067(2) 0.0066(2) 0.0086(2) P2 0.0314(3) 0.0285(3) 0.0322(3) 0.0052(2) 0.0048(2) 0.0059(2) Cl1 0.0405(3) 0.0428(3) 0.0341(3) 0.0098(2) -0.0002(2) 0.0128(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' B B 0.0090 0.0039 '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' F F 0.0727 0.0534 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' D D 0.0000 0.0000 '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 N2 C1 N1 105.93(19) . N2 C1 P1 131.52(18) . N1 C1 P1 121.44(16) . C3 C2 N1 103.63(19) . C3 C2 B1 118.05(19) . N1 C2 B1 137.9(2) . C100 C101 C102 121.3(6) . C100 C102 C101 120.2(7) 2_777 C102 C100 C101 118.5(7) 2_777 C2 C3 N2 110.78(19) . C9 C4 C5 122.4(2) . C9 C4 N1 121.2(2) . C5 C4 N1 116.4(2) . C6 C5 C4 117.4(2) . C6 C5 C13 118.8(2) . C4 C5 C13 123.8(2) . C7 C6 C5 121.1(3) . C8 C7 C6 120.2(3) . C7 C8 C9 121.5(3) . C8 C9 C4 117.1(3) . C8 C9 C10 117.6(2) . C4 C9 C10 125.1(2) . C9 C10 C11 109.3(2) . C9 C10 C12 113.2(3) . C11 C10 C12 108.1(2) . C5 C13 C14 110.2(2) . C5 C13 C15 113.4(2) . C14 C13 C15 109.6(2) . C21 C16 C17 123.9(3) . C21 C16 N2 119.1(3) . C17 C16 N2 116.8(2) . C18 C17 C16 117.4(3) . C18 C17 C25 118.7(3) . C16 C17 C25 123.8(2) . C19 C18 C17 119.9(4) . C18 C19 C20 122.2(3) . C19 C20 C21 121.1(4) . C16 C21 C20 115.0(4) . C16 C21 C22 122.5(3) . C20 C21 C22 122.4(3) . C21 C22 C24 113.5(4) . C21 C22 C23 109.8(3) . C24 C22 C23 109.1(3) . C17 C25 C27 113.6(3) . C17 C25 C26 109.9(3) . C27 C25 C26 109.7(3) . C29 C28 C33 113.4(2) . C29 C28 B1 118.6(2) . C33 C28 B1 127.8(2) . F1 C29 C30 116.5(3) . F1 C29 C28 119.1(2) . C30 C29 C28 124.4(3) . F2 C30 C31 120.2(3) . F2 C30 C29 120.8(3) . C31 C30 C29 119.0(3) . F3 C31 C32 120.7(3) . F3 C31 C30 119.7(3) . C32 C31 C30 119.6(3) . F4 C32 C31 120.0(3) . F4 C32 C33 120.2(3) . C31 C32 C33 119.7(3) . F5 C33 C32 115.1(2) . F5 C33 C28 121.2(2) . C32 C33 C28 123.8(3) . C39 C34 C35 112.2(2) . C39 C34 B1 128.3(2) . C35 C34 B1 118.9(2) . F6 C35 C36 115.3(3) . F6 C35 C34 118.6(2) . C36 C35 C34 126.0(3) . F7 C36 C37 120.0(3) . F7 C36 C35 121.5(3) . C37 C36 C35 118.5(3) . F8 C37 C38 121.4(3) . F8 C37 C36 119.6(3) . C38 C37 C36 118.9(3) . F9 C38 C37 119.4(3) . F9 C38 C39 120.2(3) . C37 C38 C39 120.4(3) . F10 C39 C34 121.6(2) . F10 C39 C38 114.5(2) . C34 C39 C38 123.9(3) . C41 C40 C45 114.1(2) . C41 C40 B1 127.5(2) . C45 C40 B1 118.3(2) . F11 C41 C40 121.4(2) . F11 C41 C42 114.9(2) . C40 C41 C42 123.6(3) . F12 C42 C43 120.5(2) . F12 C42 C41 120.2(3) . C43 C42 C41 119.2(3) . F13 C43 C44 121.2(3) . F13 C43 C42 119.0(3) . C44 C43 C42 119.8(3) . F14 C44 C43 119.6(3) . F14 C44 C45 120.7(3) . C43 C44 C45 119.7(3) . F15 C45 C44 116.9(3) . F15 C45 C40 119.5(2) . C44 C45 C40 123.6(3) . N3 C46 N4 105.0(2) . N3 C46 P2 136.6(2) . N4 C46 P2 118.0(2) . C48 C47 N4 106.9(3) . C47 C48 N3 107.6(3) . C50 C49 C54 123.0(3) . C50 C49 N4 118.2(3) . C54 C49 N4 118.8(3) . C51 C50 C49 117.9(3) . C51 C50 C58 120.8(3) . C49 C50 C58 121.3(3) . C52 C51 C50 120.7(3) . C51 C52 C53 120.8(3) . C54 C53 C52 121.2(3) . C53 C54 C49 116.4(3) . C53 C54 C55 122.8(3) . C49 C54 C55 120.8(3) . C54 C55 C57 114.0(3) . C54 C55 C56 110.1(3) . C57 C55 C56 108.6(3) . C59 C58 C50 113.6(3) . C59 C58 C60 108.7(3) . C50 C58 C60 109.7(3) . C66 C61 C62 123.9(3) . C66 C61 N3 118.8(3) . C62 C61 N3 117.2(3) . C63 C62 C61 116.9(3) . C63 C62 C70 120.0(3) . C61 C62 C70 123.0(3) . C64 C63 C62 120.8(3) . C63 C64 C65 120.8(3) . C64 C65 C66 121.1(3) . C61 C66 C65 116.5(3) . C61 C66 C67 121.9(3) . C65 C66 C67 121.5(3) . C66 C67 C68 113.1(3) . C66 C67 C69 111.0(3) . C68 C67 C69 110.3(3) . C72 C70 C62 111.7(3) . C72 C70 C71 110.5(4) . C62 C70 C71 112.0(3) . C28 B1 C40 104.1(2) . C28 B1 C2 116.42(19) . C40 B1 C2 112.42(19) . C28 B1 C34 113.6(2) . C40 B1 C34 110.91(19) . C2 B1 C34 99.72(19) . C1 N1 C2 110.58(18) . C1 N1 C4 121.79(18) . C2 N1 C4 126.42(19) . C1 N2 C3 109.04(19) . C1 N2 C16 128.6(2) . C3 N2 C16 122.13(19) . C46 N3 C48 109.9(2) . C46 N3 C61 128.1(2) . C48 N3 C61 121.3(2) . C46 N4 C47 110.7(2) . C46 N4 C49 125.0(2) . C47 N4 C49 124.3(2) . C1 P1 P2 99.79(8) . C1 P1 Cl1 92.78(7) . P2 P1 Cl1 108.25(4) . C46 P2 P1 101.43(9) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 C1 N2 1.355(3) . C1 N1 1.374(3) . C1 P1 1.851(2) . C2 C3 1.361(3) . C2 N1 1.409(3) . C2 B1 1.671(3) . C101 C100 1.387(9) . C101 C102 1.392(10) . C102 C100 1.365(9) 2_777 C100 C102 1.365(9) 2_777 C3 N2 1.363(3) . C4 C9 1.402(3) . C4 C5 1.410(4) . C4 N1 1.468(3) . C5 C6 1.397(3) . C5 C13 1.514(4) . C6 C7 1.384(5) . C7 C8 1.376(5) . C8 C9 1.401(4) . C9 C10 1.526(4) . C10 C11 1.534(4) . C10 C12 1.537(4) . C13 C14 1.535(4) . C13 C15 1.540(4) . C16 C21 1.396(4) . C16 C17 1.401(4) . C16 N2 1.456(3) . C17 C18 1.390(4) . C17 C25 1.509(5) . C18 C19 1.362(6) . C19 C20 1.364(7) . C20 C21 1.420(5) . C21 C22 1.508(5) . C22 C24 1.532(5) . C22 C23 1.537(5) . C25 C27 1.527(4) . C25 C26 1.542(4) . C28 C29 1.386(4) . C28 C33 1.401(4) . C28 B1 1.645(4) . C29 F1 1.344(3) . C29 C30 1.385(4) . C30 F2 1.340(3) . C30 C31 1.380(4) . C31 F3 1.353(3) . C31 C32 1.362(5) . C32 F4 1.350(3) . C32 C33 1.383(4) . C33 F5 1.358(3) . C34 C39 1.390(3) . C34 C35 1.396(4) . C34 B1 1.673(4) . C35 F6 1.350(3) . C35 C36 1.380(4) . C36 F7 1.345(4) . C36 C37 1.379(4) . C37 F8 1.342(4) . C37 C38 1.364(5) . C38 F9 1.346(3) . C38 C39 1.394(4) . C39 F10 1.348(3) . C40 C41 1.381(4) . C40 C45 1.404(4) . C40 B1 1.653(4) . C41 F11 1.348(3) . C41 C42 1.386(3) . C42 F12 1.345(3) . C42 C43 1.381(4) . C43 F13 1.354(3) . C43 C44 1.358(5) . C44 F14 1.346(3) . C44 C45 1.377(4) . C45 F15 1.347(3) . C46 N3 1.360(3) . C46 N4 1.360(3) . C46 P2 1.814(3) . C47 C48 1.337(5) . C47 N4 1.383(4) . C48 N3 1.391(4) . C49 C50 1.394(4) . C49 C54 1.403(4) . C49 N4 1.449(3) . C50 C51 1.390(5) . C50 C58 1.525(4) . C51 C52 1.358(5) . C52 C53 1.395(5) . C53 C54 1.390(4) . C54 C55 1.515(4) . C55 C57 1.521(5) . C55 C56 1.546(5) . C58 C59 1.522(5) . C58 C60 1.530(5) . C61 C66 1.392(4) . C61 C62 1.405(4) . C61 N3 1.443(4) . C62 C63 1.393(4) . C62 C70 1.526(5) . C63 C64 1.374(5) . C64 C65 1.390(5) . C65 C66 1.394(4) . C66 C67 1.526(4) . C67 C68 1.528(5) . C67 C69 1.536(5) . C70 C72 1.513(6) . C70 C71 1.527(5) . P1 P2 2.1416(9) . P1 Cl1 2.1676(9) . 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 _geom_torsion_site_symmetry_4 C100 C101 C102 C100 -1.5(12) 2_777 C102 C101 C100 C102 1.5(12) 2_777 N1 C2 C3 N2 -0.6(2) . B1 C2 C3 N2 173.40(19) . C9 C4 C5 C6 3.9(4) . N1 C4 C5 C6 -175.2(2) . C9 C4 C5 C13 -175.1(2) . N1 C4 C5 C13 5.8(4) . C4 C5 C6 C7 0.8(4) . C13 C5 C6 C7 179.8(3) . C5 C6 C7 C8 -3.3(5) . C6 C7 C8 C9 1.4(5) . C7 C8 C9 C4 3.1(5) . C7 C8 C9 C10 -172.0(3) . C5 C4 C9 C8 -5.7(4) . N1 C4 C9 C8 173.3(2) . C5 C4 C9 C10 169.0(2) . N1 C4 C9 C10 -12.0(4) . C8 C9 C10 C11 61.5(3) . C4 C9 C10 C11 -113.2(3) . C8 C9 C10 C12 -59.1(3) . C4 C9 C10 C12 126.3(3) . C6 C5 C13 C14 -78.3(3) . C4 C5 C13 C14 100.7(3) . C6 C5 C13 C15 45.0(3) . C4 C5 C13 C15 -136.0(3) . C21 C16 C17 C18 7.1(4) . N2 C16 C17 C18 -177.2(2) . C21 C16 C17 C25 -170.2(3) . N2 C16 C17 C25 5.6(4) . C16 C17 C18 C19 -1.7(5) . C25 C17 C18 C19 175.8(3) . C17 C18 C19 C20 -3.1(6) . C18 C19 C20 C21 2.8(6) . C17 C16 C21 C20 -7.2(4) . N2 C16 C21 C20 177.1(3) . C17 C16 C21 C22 168.2(3) . N2 C16 C21 C22 -7.5(4) . C19 C20 C21 C16 2.2(5) . C19 C20 C21 C22 -173.2(3) . C16 C21 C22 C24 144.3(3) . C20 C21 C22 C24 -40.7(4) . C16 C21 C22 C23 -93.3(3) . C20 C21 C22 C23 81.8(4) . C18 C17 C25 C27 48.1(4) . C16 C17 C25 C27 -134.7(3) . C18 C17 C25 C26 -75.3(3) . C16 C17 C25 C26 101.9(3) . C33 C28 C29 F1 175.9(2) . B1 C28 C29 F1 1.1(3) . C33 C28 C29 C30 -3.0(4) . B1 C28 C29 C30 -177.8(2) . F1 C29 C30 F2 1.1(4) . C28 C29 C30 F2 -180.0(3) . F1 C29 C30 C31 -178.6(2) . C28 C29 C30 C31 0.3(4) . F2 C30 C31 F3 2.0(4) . C29 C30 C31 F3 -178.3(3) . F2 C30 C31 C32 -177.7(3) . C29 C30 C31 C32 2.0(4) . F3 C31 C32 F4 0.7(5) . C30 C31 C32 F4 -179.6(3) . F3 C31 C32 C33 178.9(3) . C30 C31 C32 C33 -1.4(5) . F4 C32 C33 F5 -3.3(4) . C31 C32 C33 F5 178.5(3) . F4 C32 C33 C28 176.6(3) . C31 C32 C33 C28 -1.6(5) . C29 C28 C33 F5 -176.5(2) . B1 C28 C33 F5 -2.3(4) . C29 C28 C33 C32 3.7(4) . B1 C28 C33 C32 177.8(3) . C39 C34 C35 F6 -177.4(2) . B1 C34 C35 F6 -5.1(4) . C39 C34 C35 C36 0.9(4) . B1 C34 C35 C36 173.2(3) . F6 C35 C36 F7 0.5(5) . C34 C35 C36 F7 -177.9(3) . F6 C35 C36 C37 178.5(3) . C34 C35 C36 C37 0.1(5) . F7 C36 C37 F8 -1.7(6) . C35 C36 C37 F8 -179.7(3) . F7 C36 C37 C38 177.0(3) . C35 C36 C37 C38 -1.0(6) . F8 C37 C38 F9 0.0(6) . C36 C37 C38 F9 -178.7(3) . F8 C37 C38 C39 179.4(3) . C36 C37 C38 C39 0.7(6) . C35 C34 C39 F10 177.3(2) . B1 C34 C39 F10 6.0(4) . C35 C34 C39 C38 -1.2(4) . B1 C34 C39 C38 -172.5(3) . F9 C38 C39 F10 1.3(4) . C37 C38 C39 F10 -178.2(3) . F9 C38 C39 C34 179.9(3) . C37 C38 C39 C34 0.4(5) . C45 C40 C41 F11 -178.1(2) . B1 C40 C41 F11 -1.6(4) . C45 C40 C41 C42 1.2(4) . B1 C40 C41 C42 177.7(2) . F11 C41 C42 F12 -0.7(3) . C40 C41 C42 F12 179.9(2) . F11 C41 C42 C43 180.0(2) . C40 C41 C42 C43 0.6(4) . F12 C42 C43 F13 -1.6(4) . C41 C42 C43 F13 177.7(2) . F12 C42 C43 C44 179.4(2) . C41 C42 C43 C44 -1.3(4) . F13 C43 C44 F14 0.8(4) . C42 C43 C44 F14 179.8(2) . F13 C43 C44 C45 -179.0(2) . C42 C43 C44 C45 0.0(4) . F14 C44 C45 F15 -0.5(4) . C43 C44 C45 F15 179.3(2) . F14 C44 C45 C40 -177.8(2) . C43 C44 C45 C40 2.0(4) . C41 C40 C45 F15 -179.7(2) . B1 C40 C45 F15 3.4(4) . C41 C40 C45 C44 -2.5(4) . B1 C40 C45 C44 -179.4(2) . N4 C47 C48 N3 -0.7(4) . C54 C49 C50 C51 2.7(4) . N4 C49 C50 C51 -177.8(2) . C54 C49 C50 C58 -174.6(3) . N4 C49 C50 C58 4.9(4) . C49 C50 C51 C52 -0.6(5) . C58 C50 C51 C52 176.8(3) . C50 C51 C52 C53 -1.5(5) . C51 C52 C53 C54 1.6(5) . C52 C53 C54 C49 0.4(5) . C52 C53 C54 C55 -177.4(3) . C50 C49 C54 C53 -2.6(4) . N4 C49 C54 C53 177.9(3) . C50 C49 C54 C55 175.3(3) . N4 C49 C54 C55 -4.2(4) . C53 C54 C55 C57 -26.4(4) . C49 C54 C55 C57 155.9(3) . C53 C54 C55 C56 95.9(4) . C49 C54 C55 C56 -81.8(4) . C51 C50 C58 C59 44.8(5) . C49 C50 C58 C59 -138.0(4) . C51 C50 C58 C60 -77.1(4) . C49 C50 C58 C60 100.1(4) . C66 C61 C62 C63 -1.3(4) . N3 C61 C62 C63 -176.7(3) . C66 C61 C62 C70 177.0(3) . N3 C61 C62 C70 1.6(4) . C61 C62 C63 C64 0.5(5) . C70 C62 C63 C64 -178.0(3) . C62 C63 C64 C65 0.8(5) . C63 C64 C65 C66 -1.4(5) . C62 C61 C66 C65 0.8(4) . N3 C61 C66 C65 176.1(2) . C62 C61 C66 C67 -178.0(3) . N3 C61 C66 C67 -2.7(4) . C64 C65 C66 C61 0.6(4) . C64 C65 C66 C67 179.4(3) . C61 C66 C67 C68 -148.6(3) . C65 C66 C67 C68 32.6(4) . C61 C66 C67 C69 86.8(4) . C65 C66 C67 C69 -91.9(4) . C63 C62 C70 C72 -72.5(4) . C61 C62 C70 C72 109.1(4) . C63 C62 C70 C71 52.0(5) . C61 C62 C70 C71 -126.4(4) . C29 C28 B1 C40 57.8(3) . C33 C28 B1 C40 -116.1(3) . C29 C28 B1 C2 -66.5(3) . C33 C28 B1 C2 119.6(3) . C29 C28 B1 C34 178.5(2) . C33 C28 B1 C34 4.6(4) . C41 C40 B1 C28 -116.2(3) . C45 C40 B1 C28 60.3(3) . C41 C40 B1 C2 10.7(3) . C45 C40 B1 C2 -172.9(2) . C41 C40 B1 C34 121.4(3) . C45 C40 B1 C34 -62.2(3) . C3 C2 B1 C28 -169.7(2) . N1 C2 B1 C28 1.6(4) . C3 C2 B1 C40 70.4(3) . N1 C2 B1 C40 -118.3(3) . C3 C2 B1 C34 -47.2(3) . N1 C2 B1 C34 124.2(3) . C39 C34 B1 C28 -125.4(3) . C35 C34 B1 C28 63.7(3) . C39 C34 B1 C40 -8.7(4) . C35 C34 B1 C40 -179.5(2) . C39 C34 B1 C2 110.0(3) . C35 C34 B1 C2 -60.8(3) . N2 C1 N1 C2 -1.9(2) . P1 C1 N1 C2 167.40(15) . N2 C1 N1 C4 166.32(19) . P1 C1 N1 C4 -24.4(3) . C3 C2 N1 C1 1.6(2) . B1 C2 N1 C1 -170.6(2) . C3 C2 N1 C4 -166.0(2) . B1 C2 N1 C4 21.9(4) . C9 C4 N1 C1 102.1(3) . C5 C4 N1 C1 -78.8(3) . C9 C4 N1 C2 -91.6(3) . C5 C4 N1 C2 87.4(3) . N1 C1 N2 C3 1.4(2) . P1 C1 N2 C3 -166.31(18) . N1 C1 N2 C16 -172.9(2) . P1 C1 N2 C16 19.4(4) . C2 C3 N2 C1 -0.5(3) . C2 C3 N2 C16 174.2(2) . C21 C16 N2 C1 -96.6(3) . C17 C16 N2 C1 87.5(3) . C21 C16 N2 C3 89.8(3) . C17 C16 N2 C3 -86.2(3) . N4 C46 N3 C48 1.4(3) . P2 C46 N3 C48 -170.2(3) . N4 C46 N3 C61 171.8(3) . P2 C46 N3 C61 0.1(5) . C47 C48 N3 C46 -0.5(4) . C47 C48 N3 C61 -171.6(3) . C66 C61 N3 C46 93.4(4) . C62 C61 N3 C46 -90.9(4) . C66 C61 N3 C48 -97.2(4) . C62 C61 N3 C48 78.5(4) . N3 C46 N4 C47 -1.9(3) . P2 C46 N4 C47 171.7(2) . N3 C46 N4 C49 -178.6(3) . P2 C46 N4 C49 -5.0(4) . C48 C47 N4 C46 1.6(4) . C48 C47 N4 C49 178.3(3) . C50 C49 N4 C46 89.4(3) . C54 C49 N4 C46 -91.0(3) . C50 C49 N4 C47 -86.8(4) . C54 C49 N4 C47 92.7(4) . N2 C1 P1 P2 -34.5(2) . N1 C1 P1 P2 159.28(16) . N2 C1 P1 Cl1 74.5(2) . N1 C1 P1 Cl1 -91.65(17) . N3 C46 P2 P1 -26.9(3) . N4 C46 P2 P1 162.2(2) .