#------------------------------------------------------------------------------ #$Date: 2024-08-05 21:12:58 +0300 (Mon, 05 Aug 2024) $ #$Revision: 293778 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572028.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_1572028 loop_ _publ_author_name 'Nascimento, Mitchell A.' 'LaPierre, Etienne A.' 'Patrick, Brian O.' 'Watson, Jade E. T.' 'Watanabe, Lara' 'Rawson, Jeremy' 'Hering-Junghans, Christian' 'Manners, Ian' _publ_section_title ; 1,3-Dipolar cyclisation reactions of nitriles with sterically encumbered cyclic triphosphanes: synthesis and electronic structure of phosphorus-rich heterocycles with tunable colour. ; _journal_issue 30 _journal_name_full 'Chemical science' _journal_page_first 12006 _journal_page_last 12016 _journal_paper_doi 10.1039/d4sc02497d _journal_volume 15 _journal_year 2024 _chemical_formula_moiety 'C43 H57 N P3, C F3 O3 S' _chemical_formula_sum 'C44 H57 F3 N O3 P3 S' _chemical_formula_weight 829.87 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2023-09-05 deposited with the CCDC. 2024-07-01 downloaded from the CCDC. ; _cell_angle_alpha 106.573(2) _cell_angle_beta 104.787(2) _cell_angle_gamma 94.530(3) _cell_formula_units_Z 2 _cell_length_a 10.8554(10) _cell_length_b 11.7203(11) _cell_length_c 18.4078(16) _cell_measurement_reflns_used 9849 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 26.45 _cell_measurement_theta_min 2.41 _cell_volume 2141.1(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'LinXTL v. 5.9.9 (Spasyuk, 2009)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_unetI/netI 0.0553 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 34614 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.459 _diffrn_reflns_theta_min 1.838 _exptl_absorpt_coefficient_mu 0.241 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6240 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Sadabs (Sheldrick, 1996)' _exptl_crystal_colour Purple _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 880 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _refine_diff_density_max 0.560 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.073 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 512 _refine_ls_number_reflns 8818 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.018 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0515 _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^)+(0.0520P)^2^+3.3467P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1183 _refine_ls_wR_factor_ref 0.1376 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6336 _reflns_number_total 8818 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02497d4.cif _cod_data_source_block im022_a _cod_depositor_comments ; The following automatic conversions were performed: data item '_refine_ls_hydrogen_treatment' value 'Mixed' was changed to 'mixed' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas Adding full bibliography for 1572027--1572043.cif. ; _cod_database_code 1572028 _shelx_shelxl_version_number 2018/3 _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 0.953 _shelx_estimated_absorpt_t_max 0.972 _shelx_res_file ; TITL im022_a.res in P-1 im022_a.res created by SHELXL-2018/3 at 12:23:14 on 11-Mar-2020 REM Old TITL im022 in P-1 REM SHELXT solution in P-1: R1 0.138, Rweak 0.004, Alpha 0.052 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C42 O3 F3 P1 CELL 0.71073 10.8554 11.7203 18.4078 106.573 104.787 94.53 ZERR 2 0.001 0.0011 0.0016 0.002 0.002 0.003 LATT 1 SFAC C H N O F P S UNIT 88 114 2 6 6 6 2 L.S. 10 PLAN 20 SIZE 0.12 0.17 0.2 TEMP -173 BOND LIST 6 FMAP 2 ACTA REM REM REM WGHT 0.052000 3.346700 FVAR 0.51414 C1 1 0.320519 0.393349 0.351468 11.00000 0.01347 0.01556 = 0.02091 0.00448 0.00433 0.00759 C2 1 0.335364 0.489894 0.426223 11.00000 0.01353 0.01599 = 0.02128 0.00303 0.00327 0.00410 C3 1 0.349426 0.611667 0.429811 11.00000 0.01798 0.01836 = 0.02302 0.00585 0.00597 0.00424 AFIX 43 H3 2 0.348343 0.632981 0.383606 11.00000 -1.20000 AFIX 0 C4 1 0.364846 0.700242 0.501000 11.00000 0.01982 0.01584 = 0.02912 0.00217 0.00733 0.00309 AFIX 43 H4 2 0.374699 0.782734 0.503667 11.00000 -1.20000 AFIX 0 C5 1 0.366067 0.669677 0.568807 11.00000 0.01756 0.02074 = 0.02056 -0.00449 0.00456 0.00439 AFIX 43 H5 2 0.377350 0.731514 0.617479 11.00000 -1.20000 AFIX 0 C6 1 0.350936 0.549523 0.566028 11.00000 0.01675 0.02461 = 0.02088 0.00513 0.00574 0.00629 AFIX 43 H6 2 0.350841 0.528928 0.612331 11.00000 -1.20000 AFIX 0 C7 1 0.335925 0.459732 0.494635 11.00000 0.01592 0.01521 = 0.02296 0.00222 0.00436 0.00470 AFIX 43 H7 2 0.325986 0.377375 0.492278 11.00000 -1.20000 AFIX 0 C8 1 0.320239 0.357322 0.127192 11.00000 0.01826 0.01181 = 0.02047 0.00044 0.00589 -0.00096 C9 1 0.208882 0.411665 0.111097 11.00000 0.01951 0.01342 = 0.01924 -0.00018 0.00473 -0.00068 C10 1 0.176467 0.443361 0.041987 11.00000 0.02407 0.01420 = 0.02567 0.00490 0.00680 0.00420 AFIX 43 H10 2 0.103297 0.482005 0.031328 11.00000 -1.20000 AFIX 0 C11 1 0.247712 0.420193 -0.011496 11.00000 0.03032 0.02035 = 0.02352 0.00781 0.00829 0.00245 AFIX 43 H11 2 0.221664 0.439982 -0.059133 11.00000 -1.20000 AFIX 0 C12 1 0.356608 0.368284 0.004695 11.00000 0.02774 0.01894 = 0.02691 0.00325 0.01368 0.00040 AFIX 43 H12 2 0.405698 0.353125 -0.032017 11.00000 -1.20000 AFIX 0 C13 1 0.396316 0.337538 0.073710 11.00000 0.02161 0.00899 = 0.02582 -0.00034 0.00861 -0.00031 C14 1 0.121118 0.439759 0.164224 11.00000 0.02164 0.02037 = 0.02254 0.00808 0.00834 0.00889 AFIX 13 H14 2 0.146703 0.399399 0.205624 11.00000 -1.20000 AFIX 0 C15 1 -0.019445 0.388507 0.118040 11.00000 0.02155 0.04940 = 0.03297 0.02012 0.00846 0.00738 AFIX 137 H15A 2 -0.044072 0.418188 0.072546 11.00000 -1.50000 H15B 2 -0.074347 0.414122 0.152504 11.00000 -1.50000 H15C 2 -0.030480 0.300190 0.099314 11.00000 -1.50000 AFIX 0 C16 1 0.138630 0.575709 0.206944 11.00000 0.04586 0.02396 = 0.03522 0.00770 0.02055 0.01703 AFIX 137 H16A 2 0.230221 0.606646 0.234923 11.00000 -1.50000 H16B 2 0.088482 0.590069 0.245106 11.00000 -1.50000 H16C 2 0.108372 0.617240 0.168086 11.00000 -1.50000 AFIX 0 C17 1 0.517663 0.280294 0.085336 11.00000 0.02134 0.01926 = 0.02745 0.00049 0.01218 0.00385 AFIX 13 H17 2 0.545087 0.279633 0.141348 11.00000 -1.20000 AFIX 0 C18 1 0.489727 0.149521 0.030809 11.00000 0.03146 0.02373 = 0.03992 -0.00386 0.01342 0.00808 AFIX 137 H18A 2 0.425841 0.102372 0.044612 11.00000 -1.50000 H18B 2 0.569668 0.115062 0.037246 11.00000 -1.50000 H18C 2 0.455782 0.147389 -0.024349 11.00000 -1.50000 AFIX 0 C19 1 0.629222 0.350598 0.071344 11.00000 0.02839 0.03621 = 0.03499 0.00527 0.01625 0.00031 AFIX 137 H19A 2 0.606637 0.348086 0.015792 11.00000 -1.50000 H19B 2 0.706977 0.314173 0.083631 11.00000 -1.50000 H19C 2 0.645606 0.434628 0.105636 11.00000 -1.50000 AFIX 0 C20 1 0.227199 0.022939 0.175942 11.00000 0.02179 0.01284 = 0.01615 0.00276 0.00785 0.00189 C21 1 0.111048 -0.056437 0.125565 11.00000 0.02646 0.01699 = 0.01932 0.00455 0.00897 0.00188 C22 1 0.118055 -0.177489 0.092235 11.00000 0.03115 0.01634 = 0.03206 -0.00190 0.01118 -0.00516 AFIX 43 H22 2 0.041604 -0.231476 0.058747 11.00000 -1.20000 AFIX 0 C23 1 0.232798 -0.220717 0.106600 11.00000 0.04280 0.01232 = 0.04121 -0.00121 0.01921 0.00344 AFIX 43 H23 2 0.235511 -0.302997 0.081371 11.00000 -1.20000 AFIX 0 C24 1 0.343827 -0.145336 0.157383 11.00000 0.02934 0.01599 = 0.03709 0.00385 0.01654 0.00737 AFIX 43 H24 2 0.421998 -0.177020 0.167933 11.00000 -1.20000 AFIX 0 C25 1 0.343948 -0.022839 0.193840 11.00000 0.02408 0.01381 = 0.02371 0.00307 0.01231 0.00488 C26 1 -0.021565 -0.017375 0.110339 11.00000 0.02115 0.01911 = 0.02910 0.00370 0.00316 -0.00064 AFIX 13 H26 2 -0.008387 0.069076 0.112489 11.00000 -1.20000 AFIX 0 C27 1 -0.082579 -0.024242 0.176113 11.00000 0.02501 0.04076 = 0.03486 0.00107 0.00935 0.00176 AFIX 137 H27A 2 -0.096001 -0.108008 0.175932 11.00000 -1.50000 H27B 2 -0.165762 0.004504 0.166707 11.00000 -1.50000 H27C 2 -0.024833 0.026406 0.227593 11.00000 -1.50000 AFIX 0 C28 1 -0.115309 -0.089058 0.029174 11.00000 0.03142 0.02623 = 0.03427 0.00700 -0.00060 -0.00578 AFIX 137 H28A 2 -0.070610 -0.096892 -0.011585 11.00000 -1.50000 H28B 2 -0.188515 -0.046672 0.017531 11.00000 -1.50000 H28C 2 -0.146778 -0.169471 0.029651 11.00000 -1.50000 AFIX 0 C29 1 0.471999 0.048580 0.251573 11.00000 0.02223 0.01547 = 0.02580 0.00304 0.00741 0.00712 AFIX 13 H29 2 0.458763 0.133288 0.274673 11.00000 -1.20000 AFIX 0 C30 1 0.577286 0.052640 0.210504 11.00000 0.02831 0.02484 = 0.04360 0.00462 0.01396 0.00460 AFIX 137 H30A 2 0.597219 -0.028714 0.191276 11.00000 -1.50000 H30B 2 0.655179 0.106402 0.248199 11.00000 -1.50000 H30C 2 0.547013 0.082837 0.165687 11.00000 -1.50000 AFIX 0 C31 1 0.517698 -0.002881 0.319746 11.00000 0.03158 0.03512 = 0.03772 0.01228 0.00875 0.01769 AFIX 137 H31A 2 0.456501 0.006011 0.351205 11.00000 -1.50000 H31B 2 0.603258 0.040977 0.353460 11.00000 -1.50000 H31C 2 0.522573 -0.088559 0.298192 11.00000 -1.50000 AFIX 0 C32 1 0.129944 0.209656 0.372925 11.00000 0.01990 0.01625 = 0.01483 0.00100 0.00469 0.00092 C33 1 0.032005 0.281581 0.376951 11.00000 0.01803 0.02059 = 0.02044 0.00338 0.00688 0.00328 C34 1 -0.060637 0.253363 0.412476 11.00000 0.02448 0.03018 = 0.02759 0.00885 0.01353 0.00801 AFIX 43 H34 2 -0.123392 0.304412 0.419188 11.00000 -1.20000 AFIX 0 C35 1 -0.063775 0.154094 0.437992 11.00000 0.03057 0.03903 = 0.03691 0.01459 0.02038 0.00354 AFIX 43 H35 2 -0.127177 0.137786 0.462573 11.00000 -1.20000 AFIX 0 C36 1 0.026114 0.077932 0.427644 11.00000 0.03566 0.02458 = 0.03572 0.01562 0.01524 0.00457 AFIX 43 H36 2 0.020355 0.006488 0.442063 11.00000 -1.20000 AFIX 0 C37 1 0.124354 0.104538 0.396538 11.00000 0.02757 0.01898 = 0.02289 0.00581 0.00787 0.00428 C38 1 0.011743 0.382589 0.340682 11.00000 0.02046 0.02389 = 0.02689 0.00725 0.01066 0.00874 AFIX 13 H38 2 0.081979 0.391472 0.315596 11.00000 -1.20000 AFIX 0 C39 1 0.015828 0.504486 0.401426 11.00000 0.02703 0.02492 = 0.03287 0.01008 0.01279 0.01250 AFIX 137 H39A 2 -0.059593 0.501069 0.421234 11.00000 -1.50000 H39B 2 0.014818 0.567789 0.376242 11.00000 -1.50000 H39C 2 0.094873 0.522581 0.445663 11.00000 -1.50000 AFIX 0 C40 1 -0.117850 0.347383 0.275640 11.00000 0.02717 0.03573 = 0.03082 0.01161 0.00860 0.01191 AFIX 137 H40A 2 -0.115734 0.274918 0.233476 11.00000 -1.50000 H40B 2 -0.133273 0.413724 0.253722 11.00000 -1.50000 H40C 2 -0.187399 0.331000 0.298136 11.00000 -1.50000 AFIX 0 C41 1 0.222321 0.018183 0.389308 11.00000 0.03511 0.01645 = 0.03235 0.00950 0.01400 0.00835 AFIX 13 H41 2 0.270152 0.036946 0.353240 11.00000 -1.20000 AFIX 0 C42 1 0.159489 -0.114756 0.352918 11.00000 0.05528 0.01941 = 0.04442 0.00510 0.01121 0.00810 AFIX 137 H42A 2 0.118980 -0.138416 0.389445 11.00000 -1.50000 H42B 2 0.225541 -0.164751 0.343358 11.00000 -1.50000 H42C 2 0.093734 -0.126176 0.302663 11.00000 -1.50000 AFIX 0 C43 1 0.320375 0.041218 0.469367 11.00000 0.03528 0.02870 = 0.04020 0.01151 0.01176 0.00918 AFIX 137 H43A 2 0.364975 0.124885 0.488822 11.00000 -1.50000 H43B 2 0.383454 -0.013670 0.463977 11.00000 -1.50000 H43C 2 0.275995 0.027309 0.506983 11.00000 -1.50000 AFIX 0 C44 1 0.742698 0.711684 0.329039 11.00000 0.02286 0.01795 = 0.04572 0.00762 0.00846 0.00475 F1 5 0.772043 0.689484 0.397996 11.00000 0.04203 0.03125 = 0.03685 0.00610 0.00090 0.00251 F2 5 0.839517 0.690332 0.297957 11.00000 0.02563 0.04203 = 0.06704 0.01797 0.01942 0.00921 F3 5 0.737985 0.830214 0.345336 11.00000 0.03866 0.01587 = 0.06798 0.00747 0.00999 0.00297 N1 3 0.362525 0.414780 0.295109 11.00000 0.01716 0.01180 = 0.02236 0.00245 0.00698 0.00257 O1 4 0.619071 0.498245 0.250645 11.00000 0.03677 0.01612 = 0.03308 0.00563 0.00790 0.00653 O2 4 0.498539 0.646010 0.306388 11.00000 0.02573 0.02570 = 0.04229 0.00577 0.01553 0.00306 O3 4 0.571181 0.660787 0.193755 11.00000 0.03635 0.03262 = 0.04144 0.01885 0.01396 0.00874 P1 6 0.375936 0.299522 0.210841 11.00000 0.01717 0.01261 = 0.02013 0.00209 0.00727 0.00440 P2 6 0.201042 0.181695 0.208721 11.00000 0.01618 0.01241 = 0.01911 0.00180 0.00573 0.00360 P3 6 0.272769 0.234922 0.339419 11.00000 0.01802 0.01290 = 0.01939 0.00268 0.00683 0.00498 S3 7 0.590881 0.619501 0.261454 11.00000 0.02329 0.01859 = 0.03019 0.00656 0.01004 0.00378 H1 2 0.402540 0.485439 0.299648 11.00000 0.02995 HKLF 4 REM im022_a.res in P-1 REM wR2 = 0.1376, GooF = S = 1.018, Restrained GooF = 1.018 for all data REM R1 = 0.0515 for 6336 Fo > 4sig(Fo) and 0.0823 for all 8818 data REM 512 parameters refined using 0 restraints END WGHT 0.0463 3.4600 REM Highest difference peak 0.560, deepest hole -0.465, 1-sigma level 0.073 Q1 1 0.1962 0.2207 0.3590 11.00000 0.05 0.56 Q2 1 0.2352 0.1998 0.2756 11.00000 0.05 0.53 Q3 1 0.2918 0.2501 0.2141 11.00000 0.05 0.50 Q4 1 0.1044 0.1736 0.2049 11.00000 0.05 0.50 Q5 1 0.3407 0.3182 0.1594 11.00000 0.05 0.45 Q6 1 0.3734 0.2580 0.3501 11.00000 0.05 0.44 Q7 1 0.4734 0.3003 0.2282 11.00000 0.05 0.42 Q8 1 0.1606 -0.0178 0.1707 11.00000 0.05 0.41 Q9 1 0.4974 0.6103 0.2586 11.00000 0.05 0.39 Q10 1 0.2816 0.3189 0.3226 11.00000 0.05 0.38 Q11 1 0.6036 0.6613 0.3259 11.00000 0.05 0.36 Q12 1 0.6655 0.6673 0.3877 11.00000 0.05 0.36 Q13 1 0.5433 0.6011 0.2044 11.00000 0.05 0.35 Q14 1 0.0484 -0.0391 0.1228 11.00000 0.05 0.35 Q15 1 0.4646 0.3250 0.0886 11.00000 0.05 0.33 Q16 1 -0.0596 -0.0567 0.0696 11.00000 0.05 0.33 Q17 1 0.2559 0.3686 0.1109 11.00000 0.05 0.33 Q18 1 0.7519 0.7194 0.2539 11.00000 0.05 0.33 Q19 1 0.3951 0.0297 0.2334 11.00000 0.05 0.32 Q20 1 0.6567 0.6660 0.3112 11.00000 0.05 0.32 ; _shelx_res_checksum 4538 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3205(2) 0.3933(2) 0.35147(16) 0.0168(5) Uani 1 1 d . . . . . C2 C 0.3354(3) 0.4899(2) 0.42622(16) 0.0178(6) Uani 1 1 d . . . . . C3 C 0.3494(3) 0.6117(2) 0.42981(17) 0.0199(6) Uani 1 1 d . . . . . H3 H 0.348343 0.632981 0.383606 0.024 Uiso 1 1 calc R U . . . C4 C 0.3648(3) 0.7002(3) 0.50100(17) 0.0226(6) Uani 1 1 d . . . . . H4 H 0.374699 0.782734 0.503667 0.027 Uiso 1 1 calc R U . . . C5 C 0.3661(3) 0.6697(3) 0.56881(17) 0.0222(6) Uani 1 1 d . . . . . H5 H 0.377350 0.731514 0.617479 0.027 Uiso 1 1 calc R U . . . C6 C 0.3509(3) 0.5495(3) 0.56603(17) 0.0210(6) Uani 1 1 d . . . . . H6 H 0.350841 0.528928 0.612331 0.025 Uiso 1 1 calc R U . . . C7 C 0.3359(3) 0.4597(2) 0.49463(16) 0.0190(6) Uani 1 1 d . . . . . H7 H 0.325986 0.377375 0.492278 0.023 Uiso 1 1 calc R U . . . C8 C 0.3202(3) 0.3573(2) 0.12719(16) 0.0180(6) Uani 1 1 d . . . . . C9 C 0.2089(3) 0.4117(2) 0.11110(16) 0.0189(6) Uani 1 1 d . . . . . C10 C 0.1765(3) 0.4434(2) 0.04199(17) 0.0216(6) Uani 1 1 d . . . . . H10 H 0.103297 0.482005 0.031328 0.026 Uiso 1 1 calc R U . . . C11 C 0.2477(3) 0.4202(3) -0.01150(18) 0.0245(6) Uani 1 1 d . . . . . H11 H 0.221664 0.439982 -0.059133 0.029 Uiso 1 1 calc R U . . . C12 C 0.3566(3) 0.3683(3) 0.00469(17) 0.0245(6) Uani 1 1 d . . . . . H12 H 0.405698 0.353125 -0.032017 0.029 Uiso 1 1 calc R U . . . C13 C 0.3963(3) 0.3375(2) 0.07371(17) 0.0199(6) Uani 1 1 d . . . . . C14 C 0.1211(3) 0.4398(2) 0.16422(17) 0.0205(6) Uani 1 1 d . . . . . H14 H 0.146703 0.399399 0.205624 0.025 Uiso 1 1 calc R U . . . C15 C -0.0194(3) 0.3885(3) 0.11804(19) 0.0329(7) Uani 1 1 d . . . . . H15A H -0.044072 0.418188 0.072546 0.049 Uiso 1 1 calc R U . . . H15B H -0.074347 0.414122 0.152504 0.049 Uiso 1 1 calc R U . . . H15C H -0.030480 0.300190 0.099314 0.049 Uiso 1 1 calc R U . . . C16 C 0.1386(3) 0.5757(3) 0.2069(2) 0.0330(7) Uani 1 1 d . . . . . H16A H 0.230221 0.606646 0.234923 0.050 Uiso 1 1 calc R U . . . H16B H 0.088482 0.590069 0.245106 0.050 Uiso 1 1 calc R U . . . H16C H 0.108372 0.617240 0.168086 0.050 Uiso 1 1 calc R U . . . C17 C 0.5177(3) 0.2803(2) 0.08534(18) 0.0232(6) Uani 1 1 d . . . . . H17 H 0.545087 0.279633 0.141348 0.028 Uiso 1 1 calc R U . . . C18 C 0.4897(3) 0.1495(3) 0.0308(2) 0.0340(8) Uani 1 1 d . . . . . H18A H 0.425841 0.102372 0.044612 0.051 Uiso 1 1 calc R U . . . H18B H 0.569668 0.115062 0.037246 0.051 Uiso 1 1 calc R U . . . H18C H 0.455782 0.147389 -0.024349 0.051 Uiso 1 1 calc R U . . . C19 C 0.6292(3) 0.3506(3) 0.0713(2) 0.0334(7) Uani 1 1 d . . . . . H19A H 0.606637 0.348086 0.015792 0.050 Uiso 1 1 calc R U . . . H19B H 0.706977 0.314173 0.083631 0.050 Uiso 1 1 calc R U . . . H19C H 0.645606 0.434628 0.105636 0.050 Uiso 1 1 calc R U . . . C20 C 0.2272(3) 0.0229(2) 0.17594(15) 0.0169(5) Uani 1 1 d . . . . . C21 C 0.1110(3) -0.0564(2) 0.12557(16) 0.0208(6) Uani 1 1 d . . . . . C22 C 0.1181(3) -0.1775(3) 0.09223(18) 0.0288(7) Uani 1 1 d . . . . . H22 H 0.041604 -0.231476 0.058747 0.035 Uiso 1 1 calc R U . . . C23 C 0.2328(3) -0.2207(3) 0.1066(2) 0.0329(8) Uani 1 1 d . . . . . H23 H 0.235511 -0.302997 0.081371 0.040 Uiso 1 1 calc R U . . . C24 C 0.3438(3) -0.1453(3) 0.15738(19) 0.0269(7) Uani 1 1 d . . . . . H24 H 0.421998 -0.177020 0.167933 0.032 Uiso 1 1 calc R U . . . C25 C 0.3439(3) -0.0228(2) 0.19384(16) 0.0200(6) Uani 1 1 d . . . . . C26 C -0.0216(3) -0.0174(3) 0.11034(18) 0.0250(6) Uani 1 1 d . . . . . H26 H -0.008387 0.069076 0.112489 0.030 Uiso 1 1 calc R U . . . C27 C -0.0826(3) -0.0242(3) 0.1761(2) 0.0360(8) Uani 1 1 d . . . . . H27A H -0.096001 -0.108008 0.175932 0.054 Uiso 1 1 calc R U . . . H27B H -0.165762 0.004504 0.166707 0.054 Uiso 1 1 calc R U . . . H27C H -0.024833 0.026406 0.227593 0.054 Uiso 1 1 calc R U . . . C28 C -0.1153(3) -0.0891(3) 0.02917(19) 0.0338(8) Uani 1 1 d . . . . . H28A H -0.070610 -0.096892 -0.011585 0.051 Uiso 1 1 calc R U . . . H28B H -0.188515 -0.046672 0.017531 0.051 Uiso 1 1 calc R U . . . H28C H -0.146778 -0.169471 0.029651 0.051 Uiso 1 1 calc R U . . . C29 C 0.4720(3) 0.0486(2) 0.25157(17) 0.0216(6) Uani 1 1 d . . . . . H29 H 0.458763 0.133288 0.274673 0.026 Uiso 1 1 calc R U . . . C30 C 0.5773(3) 0.0526(3) 0.2105(2) 0.0329(7) Uani 1 1 d . . . . . H30A H 0.597219 -0.028714 0.191276 0.049 Uiso 1 1 calc R U . . . H30B H 0.655179 0.106402 0.248199 0.049 Uiso 1 1 calc R U . . . H30C H 0.547013 0.082837 0.165687 0.049 Uiso 1 1 calc R U . . . C31 C 0.5177(3) -0.0029(3) 0.3197(2) 0.0342(8) Uani 1 1 d . . . . . H31A H 0.456501 0.006011 0.351205 0.051 Uiso 1 1 calc R U . . . H31B H 0.603258 0.040977 0.353460 0.051 Uiso 1 1 calc R U . . . H31C H 0.522573 -0.088559 0.298192 0.051 Uiso 1 1 calc R U . . . C32 C 0.1299(3) 0.2097(2) 0.37293(15) 0.0180(6) Uani 1 1 d . . . . . C33 C 0.0320(3) 0.2816(2) 0.37695(16) 0.0201(6) Uani 1 1 d . . . . . C34 C -0.0606(3) 0.2534(3) 0.41248(18) 0.0261(7) Uani 1 1 d . . . . . H34 H -0.123392 0.304412 0.419188 0.031 Uiso 1 1 calc R U . . . C35 C -0.0638(3) 0.1541(3) 0.43799(19) 0.0330(7) Uani 1 1 d . . . . . H35 H -0.127177 0.137786 0.462573 0.040 Uiso 1 1 calc R U . . . C36 C 0.0261(3) 0.0779(3) 0.42764(19) 0.0297(7) Uani 1 1 d . . . . . H36 H 0.020355 0.006488 0.442063 0.036 Uiso 1 1 calc R U . . . C37 C 0.1244(3) 0.1045(3) 0.39654(17) 0.0232(6) Uani 1 1 d . . . . . C38 C 0.0117(3) 0.3826(3) 0.34068(17) 0.0229(6) Uani 1 1 d . . . . . H38 H 0.081979 0.391472 0.315596 0.027 Uiso 1 1 calc R U . . . C39 C 0.0158(3) 0.5045(3) 0.40143(18) 0.0268(7) Uani 1 1 d . . . . . H39A H -0.059593 0.501069 0.421234 0.040 Uiso 1 1 calc R U . . . H39B H 0.014818 0.567789 0.376242 0.040 Uiso 1 1 calc R U . . . H39C H 0.094873 0.522581 0.445663 0.040 Uiso 1 1 calc R U . . . C40 C -0.1179(3) 0.3474(3) 0.27564(19) 0.0306(7) Uani 1 1 d . . . . . H40A H -0.115734 0.274918 0.233476 0.046 Uiso 1 1 calc R U . . . H40B H -0.133273 0.413724 0.253722 0.046 Uiso 1 1 calc R U . . . H40C H -0.187399 0.331000 0.298136 0.046 Uiso 1 1 calc R U . . . C41 C 0.2223(3) 0.0182(3) 0.38931(18) 0.0265(7) Uani 1 1 d . . . . . H41 H 0.270152 0.036946 0.353240 0.032 Uiso 1 1 calc R U . . . C42 C 0.1595(4) -0.1148(3) 0.3529(2) 0.0413(9) Uani 1 1 d . . . . . H42A H 0.118980 -0.138416 0.389445 0.062 Uiso 1 1 calc R U . . . H42B H 0.225541 -0.164751 0.343358 0.062 Uiso 1 1 calc R U . . . H42C H 0.093734 -0.126176 0.302663 0.062 Uiso 1 1 calc R U . . . C43 C 0.3204(3) 0.0412(3) 0.4694(2) 0.0342(7) Uani 1 1 d . . . . . H43A H 0.364975 0.124885 0.488822 0.051 Uiso 1 1 calc R U . . . H43B H 0.383454 -0.013670 0.463977 0.051 Uiso 1 1 calc R U . . . H43C H 0.275995 0.027309 0.506983 0.051 Uiso 1 1 calc R U . . . C44 C 0.7427(3) 0.7117(3) 0.3290(2) 0.0296(7) Uani 1 1 d . . . . . F1 F 0.77204(19) 0.68948(17) 0.39800(11) 0.0400(5) Uani 1 1 d . . . . . F2 F 0.83952(18) 0.69033(18) 0.29796(13) 0.0434(5) Uani 1 1 d . . . . . F3 F 0.73798(19) 0.83021(16) 0.34534(13) 0.0433(5) Uani 1 1 d . . . . . N1 N 0.3625(2) 0.4148(2) 0.29511(13) 0.0175(5) Uani 1 1 d . . . . . O1 O 0.6191(2) 0.49825(17) 0.25064(13) 0.0294(5) Uani 1 1 d . . . . . O2 O 0.4985(2) 0.64601(19) 0.30639(13) 0.0313(5) Uani 1 1 d . . . . . O3 O 0.5712(2) 0.6608(2) 0.19376(14) 0.0345(5) Uani 1 1 d . . . . . P1 P 0.37594(7) 0.29952(6) 0.21084(4) 0.01684(16) Uani 1 1 d . . . . . P2 P 0.20104(7) 0.18169(6) 0.20872(4) 0.01641(16) Uani 1 1 d . . . . . P3 P 0.27277(7) 0.23492(6) 0.33942(4) 0.01689(16) Uani 1 1 d . . . . . S3 S 0.59088(7) 0.61950(6) 0.26145(4) 0.02382(17) Uani 1 1 d . . . . . H1 H 0.403(3) 0.485(3) 0.2996(19) 0.030(9) Uiso 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 0.0135(13) 0.0156(13) 0.0209(14) 0.0045(11) 0.0043(11) 0.0076(10) C2 0.0135(13) 0.0160(13) 0.0213(14) 0.0030(11) 0.0033(11) 0.0041(10) C3 0.0180(14) 0.0184(14) 0.0230(14) 0.0059(11) 0.0060(11) 0.0042(11) C4 0.0198(15) 0.0158(13) 0.0291(16) 0.0022(12) 0.0073(12) 0.0031(11) C5 0.0176(14) 0.0207(14) 0.0206(14) -0.0045(11) 0.0046(11) 0.0044(11) C6 0.0167(14) 0.0246(15) 0.0209(14) 0.0051(12) 0.0057(11) 0.0063(11) C7 0.0159(13) 0.0152(13) 0.0230(14) 0.0022(11) 0.0044(11) 0.0047(11) C8 0.0183(14) 0.0118(12) 0.0205(14) 0.0004(10) 0.0059(11) -0.0010(10) C9 0.0195(14) 0.0134(13) 0.0192(14) -0.0002(11) 0.0047(11) -0.0007(11) C10 0.0241(15) 0.0142(13) 0.0257(15) 0.0049(11) 0.0068(12) 0.0042(11) C11 0.0303(17) 0.0203(14) 0.0235(15) 0.0078(12) 0.0083(13) 0.0025(12) C12 0.0277(16) 0.0189(14) 0.0269(16) 0.0033(12) 0.0137(13) 0.0004(12) C13 0.0216(15) 0.0090(12) 0.0258(15) -0.0003(11) 0.0086(12) -0.0003(11) C14 0.0216(15) 0.0204(14) 0.0225(14) 0.0081(11) 0.0083(12) 0.0089(11) C15 0.0215(16) 0.049(2) 0.0330(18) 0.0201(16) 0.0085(14) 0.0074(15) C16 0.046(2) 0.0240(16) 0.0352(18) 0.0077(14) 0.0205(16) 0.0170(15) C17 0.0213(15) 0.0193(14) 0.0275(16) 0.0005(12) 0.0122(12) 0.0039(11) C18 0.0315(18) 0.0237(16) 0.0399(19) -0.0039(14) 0.0134(15) 0.0081(13) C19 0.0284(17) 0.0362(18) 0.0350(18) 0.0053(15) 0.0162(14) 0.0003(14) C20 0.0218(14) 0.0128(12) 0.0161(13) 0.0028(10) 0.0078(11) 0.0019(11) C21 0.0265(16) 0.0170(13) 0.0193(14) 0.0046(11) 0.0090(12) 0.0019(11) C22 0.0311(17) 0.0163(14) 0.0321(17) -0.0019(12) 0.0112(14) -0.0052(12) C23 0.043(2) 0.0123(14) 0.0412(19) -0.0012(13) 0.0192(16) 0.0034(13) C24 0.0293(17) 0.0160(14) 0.0371(18) 0.0038(12) 0.0165(14) 0.0074(12) C25 0.0241(15) 0.0138(13) 0.0237(14) 0.0031(11) 0.0123(12) 0.0049(11) C26 0.0212(15) 0.0191(14) 0.0291(16) 0.0037(12) 0.0032(12) -0.0006(12) C27 0.0250(17) 0.041(2) 0.0349(18) 0.0011(15) 0.0093(14) 0.0018(14) C28 0.0314(18) 0.0262(17) 0.0343(18) 0.0070(14) -0.0006(14) -0.0058(14) C29 0.0222(15) 0.0155(13) 0.0258(15) 0.0030(11) 0.0074(12) 0.0071(11) C30 0.0283(17) 0.0248(16) 0.044(2) 0.0046(14) 0.0140(15) 0.0046(13) C31 0.0316(18) 0.0351(18) 0.0377(19) 0.0123(15) 0.0087(15) 0.0177(15) C32 0.0199(14) 0.0163(13) 0.0148(13) 0.0010(10) 0.0047(11) 0.0009(11) C33 0.0180(14) 0.0206(14) 0.0204(14) 0.0034(11) 0.0069(11) 0.0033(11) C34 0.0245(16) 0.0302(16) 0.0276(16) 0.0088(13) 0.0135(13) 0.0080(13) C35 0.0306(18) 0.0390(19) 0.0369(19) 0.0146(15) 0.0204(15) 0.0035(15) C36 0.0357(18) 0.0246(16) 0.0357(18) 0.0156(14) 0.0152(14) 0.0046(13) C37 0.0276(16) 0.0190(14) 0.0229(15) 0.0058(12) 0.0079(12) 0.0043(12) C38 0.0205(15) 0.0239(15) 0.0269(15) 0.0072(12) 0.0107(12) 0.0087(12) C39 0.0270(16) 0.0249(15) 0.0329(17) 0.0101(13) 0.0128(13) 0.0125(13) C40 0.0272(17) 0.0357(18) 0.0308(17) 0.0116(14) 0.0086(14) 0.0119(14) C41 0.0351(18) 0.0165(14) 0.0323(17) 0.0095(12) 0.0140(14) 0.0084(13) C42 0.055(2) 0.0194(16) 0.044(2) 0.0051(15) 0.0112(18) 0.0081(15) C43 0.0353(19) 0.0287(17) 0.0402(19) 0.0115(15) 0.0118(15) 0.0092(14) C44 0.0229(16) 0.0180(14) 0.046(2) 0.0076(14) 0.0085(14) 0.0048(12) F1 0.0420(12) 0.0312(10) 0.0368(11) 0.0061(9) 0.0009(9) 0.0025(9) F2 0.0256(10) 0.0420(12) 0.0670(14) 0.0180(11) 0.0194(10) 0.0092(9) F3 0.0387(12) 0.0159(9) 0.0680(14) 0.0075(9) 0.0100(10) 0.0030(8) N1 0.0172(12) 0.0118(11) 0.0224(12) 0.0024(9) 0.0070(10) 0.0026(9) O1 0.0368(13) 0.0161(10) 0.0331(12) 0.0056(9) 0.0079(10) 0.0065(9) O2 0.0257(12) 0.0257(11) 0.0423(13) 0.0058(10) 0.0155(10) 0.0031(9) O3 0.0364(13) 0.0326(12) 0.0414(14) 0.0188(11) 0.0140(11) 0.0087(10) P1 0.0172(4) 0.0126(3) 0.0201(4) 0.0021(3) 0.0073(3) 0.0044(3) P2 0.0162(4) 0.0124(3) 0.0191(4) 0.0018(3) 0.0057(3) 0.0036(3) P3 0.0180(4) 0.0129(3) 0.0194(4) 0.0027(3) 0.0068(3) 0.0050(3) S3 0.0233(4) 0.0186(3) 0.0302(4) 0.0066(3) 0.0100(3) 0.0038(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.0(2) . . ? N1 C1 P3 115.82(19) . . ? C2 C1 P3 122.2(2) . . ? C7 C2 C3 119.6(2) . . ? C7 C2 C1 119.5(2) . . ? C3 C2 C1 120.9(2) . . ? C4 C3 C2 119.5(3) . . ? C3 C4 C5 120.5(3) . . ? C6 C5 C4 120.6(3) . . ? C5 C6 C7 119.2(3) . . ? C6 C7 C2 120.5(3) . . ? C9 C8 C13 119.8(3) . . ? C9 C8 P1 126.0(2) . . ? C13 C8 P1 114.1(2) . . ? C10 C9 C8 118.3(2) . . ? C10 C9 C14 116.8(2) . . ? C8 C9 C14 124.9(2) . . ? C11 C10 C9 121.9(3) . . ? C12 C11 C10 119.6(3) . . ? C11 C12 C13 121.4(3) . . ? C12 C13 C8 118.9(3) . . ? C12 C13 C17 116.9(2) . . ? C8 C13 C17 124.1(3) . . ? C15 C14 C9 111.3(2) . . ? C15 C14 C16 111.3(3) . . ? C9 C14 C16 111.4(2) . . ? C13 C17 C19 112.5(3) . . ? C13 C17 C18 110.5(2) . . ? C19 C17 C18 109.8(2) . . ? C25 C20 C21 120.1(2) . . ? C25 C20 P2 127.9(2) . . ? C21 C20 P2 111.9(2) . . ? C22 C21 C20 118.2(3) . . ? C22 C21 C26 118.2(3) . . ? C20 C21 C26 123.5(2) . . ? C23 C22 C21 121.6(3) . . ? C22 C23 C24 120.3(3) . . ? C23 C24 C25 121.3(3) . . ? C24 C25 C20 118.4(3) . . ? C24 C25 C29 115.7(2) . . ? C20 C25 C29 125.9(2) . . ? C21 C26 C28 113.9(3) . . ? C21 C26 C27 110.6(3) . . ? C28 C26 C27 109.8(3) . . ? C25 C29 C30 111.9(2) . . ? C25 C29 C31 111.5(2) . . ? C30 C29 C31 109.4(3) . . ? C33 C32 C37 119.9(2) . . ? C33 C32 P3 127.4(2) . . ? C37 C32 P3 112.7(2) . . ? C34 C33 C32 117.9(3) . . ? C34 C33 C38 116.1(2) . . ? C32 C33 C38 125.8(2) . . ? C35 C34 C33 122.1(3) . . ? C34 C35 C36 119.6(3) . . ? C35 C36 C37 120.9(3) . . ? C36 C37 C32 119.1(3) . . ? C36 C37 C41 117.9(3) . . ? C32 C37 C41 123.0(3) . . ? C33 C38 C39 113.3(2) . . ? C33 C38 C40 109.1(2) . . ? C39 C38 C40 109.8(2) . . ? C43 C41 C37 110.1(2) . . ? C43 C41 C42 111.3(3) . . ? C37 C41 C42 113.2(3) . . ? F2 C44 F1 107.9(3) . . ? F2 C44 F3 107.3(2) . . ? F1 C44 F3 106.9(3) . . ? F2 C44 S3 110.9(2) . . ? F1 C44 S3 111.6(2) . . ? F3 C44 S3 112.0(2) . . ? C1 N1 P1 124.01(19) . . ? N1 P1 C8 104.74(11) . . ? N1 P1 P2 91.24(8) . . ? C8 P1 P2 104.65(9) . . ? C20 P2 P3 103.55(9) . . ? C20 P2 P1 107.61(9) . . ? P3 P2 P1 88.53(4) . . ? C1 P3 C32 112.40(12) . . ? C1 P3 P2 93.98(9) . . ? C32 P3 P2 105.80(9) . . ? O3 S3 O1 116.70(13) . . ? O3 S3 O2 115.58(14) . . ? O1 S3 O2 112.24(13) . . ? O3 S3 C44 103.70(14) . . ? O1 S3 C44 102.41(13) . . ? O2 S3 C44 103.89(14) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.311(3) . ? C1 C2 1.473(4) . ? C1 P3 1.822(3) . ? C2 C7 1.400(4) . ? C2 C3 1.404(4) . ? C3 C4 1.381(4) . ? C4 C5 1.391(4) . ? C5 C6 1.390(4) . ? C6 C7 1.391(4) . ? C8 C9 1.415(4) . ? C8 C13 1.421(4) . ? C8 P1 1.838(3) . ? C9 C10 1.394(4) . ? C9 C14 1.521(4) . ? C10 C11 1.382(4) . ? C11 C12 1.376(4) . ? C12 C13 1.391(4) . ? C13 C17 1.519(4) . ? C14 C15 1.521(4) . ? C14 C16 1.534(4) . ? C17 C19 1.528(4) . ? C17 C18 1.530(4) . ? C20 C25 1.413(4) . ? C20 C21 1.429(4) . ? C20 P2 1.854(3) . ? C21 C22 1.393(4) . ? C21 C26 1.527(4) . ? C22 C23 1.373(5) . ? C23 C24 1.376(4) . ? C24 C25 1.400(4) . ? C25 C29 1.522(4) . ? C26 C28 1.532(4) . ? C26 C27 1.539(4) . ? C29 C30 1.527(4) . ? C29 C31 1.532(4) . ? C32 C33 1.412(4) . ? C32 C37 1.420(4) . ? C32 P3 1.842(3) . ? C33 C34 1.398(4) . ? C33 C38 1.521(4) . ? C34 C35 1.374(4) . ? C35 C36 1.386(4) . ? C36 C37 1.387(4) . ? C37 C41 1.529(4) . ? C38 C39 1.532(4) . ? C38 C40 1.533(4) . ? C41 C43 1.518(5) . ? C41 C42 1.531(4) . ? C44 F2 1.327(4) . ? C44 F1 1.332(4) . ? C44 F3 1.343(3) . ? C44 S3 1.827(3) . ? N1 P1 1.790(2) . ? O1 S3 1.446(2) . ? O2 S3 1.453(2) . ? O3 S3 1.434(2) . ? P1 P2 2.2428(10) . ? P2 P3 2.2123(10) . ?