#------------------------------------------------------------------------------ #$Date: 2018-01-13 03:57:05 +0200 (Sat, 13 Jan 2018) $ #$Revision: 205140 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/11/7121139.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_7121139 loop_ _publ_author_name 'Koner, Abhishek' 'Kelemen, Zsolt' 'Schnakenburg, Gregor' 'Nyul\'aszi, L\'aszl\'o' 'Streubel, Rainer' _publ_section_title ; 1,4-Additions of tricyclic 1,4-diphosphinines -- a novel system to study \s-bond activation and \p--\p dispersion interactions ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C7CC09349G _journal_year 2018 _chemical_formula_moiety 'C34 H46 N4 P2 S2 Se2' _chemical_formula_sum 'C34 H46 N4 P2 S2 Se2' _chemical_formula_weight 794.73 _chemical_name_systematic ABK-466 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2017-03-30 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292) ; _audit_update_record ; 2017-12-05 deposited with the CCDC. 2018-01-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 103.2796(13) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 18.5972(7) _cell_length_b 13.2665(5) _cell_length_c 15.6185(6) _cell_measurement_reflns_used 9630 _cell_measurement_temperature 100 _cell_measurement_theta_max 23.57 _cell_measurement_theta_min 2.66 _cell_volume 3750.4(2) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker X8-KappaApexII' _diffrn_measurement_method 'fine slicing \w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0775 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 61648 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.999 _diffrn_reflns_theta_min 2.174 _diffrn_source 'sealed tube' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.197 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_correction_T_min 0.5809 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0907 before and 0.0570 after correction. The Ratio of minimum to maximum transmission is 0.7788. The \l/2 correction factor is 0.00150.' _exptl_crystal_colour 'clear yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.408 _exptl_crystal_description block _exptl_crystal_F_000 1632 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.387 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.079 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 401 _refine_ls_number_reflns 9047 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.035 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0353 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+2.7453P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0629 _refine_ls_wR_factor_ref 0.0754 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6293 _reflns_number_total 9047 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c7cc09349g2.cif _cod_data_source_block 3b _cod_database_code 7121139 _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_max 0.844 _shelx_estimated_absorpt_t_min 0.621 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints C11 \\sim C10 \\sim C9 \\sim C8: within 2A with sigma of 0.002 and sigma for terminal atoms of 0.004 3.a Secondary CH2 refined with riding coordinates: C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A, H10B), C4'(H4'A,H4'B), C5'(H5'A,H5'B), C6'(H6'A,H6'B), C8'(H8'A,H8'B), C9'(H9'A,H9'B), C10'(H10C,H10D) 3.b Aromatic/amide H refined with riding coordinates: C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C13'(H13'), C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17') 3.c Idealised Me refined as rotating group: C7(H7A,H7B,H7C), C11(H11A,H11B,H11C), C7'(H7'A,H7'B,H7'C), C11'(H11D,H11E,H11F) ; _shelx_res_file ; 5080f.res created by SHELXL-2014/7 TITL 5080f in P21/c #14 REM reset to P21/c #14 CELL 0.71073 18.5972 13.2665 15.6185 90 103.2796 90 ZERR 4 0.0007 0.0005 0.0006 0 0.0013 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N P S Se UNIT 136 184 16 8 8 8 SIMU 0.002 0.004 2 C11 C10 C9 C8 L.S. 4 0 0 PLAN 20 SIZE 0.08 0.12 0.24 TEMP -173.15 BOND fmap 2 53 acta OMIT -2 56 OMIT 3 0 0 OMIT -1 2 1 REM REM REM WGHT 0.020400 2.745300 FVAR 0.09518 SE 6 0.598232 -0.106190 0.370709 11.00000 0.02709 0.02980 = 0.02338 -0.00392 0.00865 0.00096 S 5 0.500032 0.339913 0.338070 11.00000 0.06449 0.02707 = 0.03406 0.01192 0.00444 -0.00480 P 4 0.482175 -0.068720 0.391590 11.00000 0.02291 0.02260 = 0.01531 -0.00076 0.00318 -0.00223 N1 3 0.490525 0.135376 0.353641 11.00000 0.02698 0.02382 = 0.01472 0.00357 0.00368 -0.00004 N2 3 0.513108 0.214614 0.478608 11.00000 0.02757 0.01905 = 0.02176 0.00002 0.00585 -0.00096 C1 1 0.493571 0.062994 0.418822 11.00000 0.02002 0.02109 = 0.01698 0.00253 0.00436 0.00001 C2 1 0.501469 0.229566 0.389876 11.00000 0.02625 0.02749 = 0.02396 0.00345 0.00336 -0.00295 C3 1 0.508067 0.112709 0.497555 11.00000 0.02097 0.01723 = 0.01926 0.00157 0.00434 -0.00086 C4 1 0.470180 0.117076 0.258817 11.00000 0.02929 0.03105 = 0.01764 0.00457 0.00688 0.00027 AFIX 23 H4A 2 0.489610 0.050646 0.246052 11.00000 -1.20000 H4B 2 0.493129 0.169246 0.228394 11.00000 -1.20000 AFIX 0 C5 1 0.387279 0.118949 0.223713 11.00000 0.02857 0.03281 = 0.02479 0.00020 0.00536 -0.00225 AFIX 23 H5A 2 0.364573 0.067418 0.255046 11.00000 -1.20000 H5B 2 0.368198 0.185628 0.236412 11.00000 -1.20000 AFIX 0 C6 1 0.363980 0.099227 0.125848 11.00000 0.03376 0.03478 = 0.02858 -0.00517 0.00209 -0.00048 AFIX 23 H6A 2 0.377884 0.029566 0.113616 11.00000 -1.20000 H6B 2 0.390645 0.146021 0.094630 11.00000 -1.20000 AFIX 0 C7 1 0.281253 0.112838 0.091024 11.00000 0.03669 0.06049 = 0.04662 -0.00486 -0.00706 -0.00546 AFIX 137 H7A 2 0.254667 0.066983 0.122102 11.00000 -1.50000 H7B 2 0.268125 0.097704 0.027932 11.00000 -1.50000 H7C 2 0.267638 0.182602 0.100588 11.00000 -1.50000 AFIX 0 C8 1 0.530939 0.296695 0.542424 11.00000 0.03830 0.02423 = 0.03105 -0.00673 0.01293 -0.00570 AFIX 23 H8A 2 0.517816 0.276026 0.597812 11.00000 -1.20000 H8B 2 0.500687 0.356375 0.519351 11.00000 -1.20000 AFIX 0 C9 1 0.611323 0.325365 0.561873 11.00000 0.04357 0.03909 = 0.03917 -0.00960 0.01230 -0.01338 AFIX 23 H9A 2 0.625854 0.340606 0.506126 11.00000 -1.20000 H9B 2 0.641646 0.267990 0.590364 11.00000 -1.20000 AFIX 0 C10 1 0.626007 0.416912 0.622008 11.00000 0.05756 0.05455 = 0.05500 -0.01693 0.00949 -0.02151 AFIX 23 H10A 2 0.591028 0.471128 0.596508 11.00000 -1.20000 H10B 2 0.616351 0.398680 0.679806 11.00000 -1.20000 AFIX 0 C11 1 0.702703 0.456140 0.635681 11.00000 0.08575 0.09372 = 0.08327 -0.02037 0.01109 -0.04728 AFIX 137 H11A 2 0.707700 0.517275 0.671788 11.00000 -1.50000 H11B 2 0.713415 0.472020 0.578602 11.00000 -1.50000 H11C 2 0.737543 0.404977 0.665663 11.00000 -1.50000 AFIX 0 C12 1 0.657439 -0.068060 0.483566 11.00000 0.02228 0.03623 = 0.02380 -0.00140 0.00701 0.00246 C13 1 0.679237 0.031191 0.501376 11.00000 0.02434 0.03729 = 0.03674 -0.00426 0.01020 -0.00090 AFIX 43 H13 2 0.662299 0.082122 0.458758 11.00000 -1.20000 AFIX 0 C14 1 0.725830 0.056103 0.581525 11.00000 0.02648 0.05496 = 0.04824 -0.01937 0.00968 -0.00899 AFIX 43 H14 2 0.740666 0.124088 0.593910 11.00000 -1.20000 AFIX 0 C15 1 0.750415 -0.017856 0.642867 11.00000 0.02425 0.09001 = 0.03039 -0.01125 0.00195 -0.00198 AFIX 43 H15 2 0.782380 -0.000639 0.697584 11.00000 -1.20000 AFIX 0 C16 1 0.729187 -0.116750 0.625844 11.00000 0.03241 0.07301 = 0.03075 0.01112 0.00644 0.00766 AFIX 43 H16 2 0.746760 -0.167322 0.668594 11.00000 -1.20000 AFIX 0 C17 1 0.682148 -0.142511 0.546276 11.00000 0.02607 0.04410 = 0.03547 0.00161 0.00956 0.00289 AFIX 43 H17 2 0.666914 -0.210477 0.534681 11.00000 -1.20000 AFIX 0 SE' 6 0.062978 1.202582 0.411862 11.00000 0.04341 0.02457 = 0.02949 0.00424 0.01169 -0.00602 S' 5 0.117193 0.754554 0.313238 11.00000 0.05244 0.03597 = 0.04080 -0.00932 0.01889 0.01055 P' 4 -0.029321 1.084721 0.401692 11.00000 0.02992 0.01995 = 0.01924 0.00149 0.00436 0.00216 N1' 3 0.048775 0.926168 0.349324 11.00000 0.02772 0.02265 = 0.02220 -0.00280 0.00629 -0.00104 N2' 3 0.081163 0.826610 0.461898 11.00000 0.02831 0.02014 = 0.02385 -0.00147 0.00394 0.00395 C1' 1 0.023558 0.969909 0.417923 11.00000 0.02286 0.02168 = 0.01774 -0.00147 0.00439 0.00099 C2' 1 0.082932 0.836323 0.375250 11.00000 0.02628 0.02495 = 0.02701 -0.00269 0.00605 -0.00055 C3' 1 0.044416 0.907826 0.488842 11.00000 0.02158 0.02167 = 0.01997 -0.00161 0.00332 -0.00131 C4' 1 0.041619 0.968945 0.261507 11.00000 0.03099 0.03172 = 0.01990 -0.00052 0.00861 -0.00246 AFIX 23 H4'A 2 0.078789 0.937241 0.233763 11.00000 -1.20000 H4'B 2 0.052619 1.041977 0.267183 11.00000 -1.20000 AFIX 0 C5' 1 -0.034487 0.954435 0.201793 11.00000 0.02949 0.02707 = 0.02178 -0.00466 0.00730 -0.00377 AFIX 23 H5'A 2 -0.048100 0.882243 0.201016 11.00000 -1.20000 H5'B 2 -0.071166 0.992976 0.225514 11.00000 -1.20000 AFIX 0 C6' 1 -0.037055 0.989018 0.108823 11.00000 0.03186 0.03430 = 0.02570 0.00164 0.00434 -0.00200 AFIX 23 H6'A 2 -0.001122 0.949347 0.084764 11.00000 -1.20000 H6'B 2 -0.022150 1.060732 0.109919 11.00000 -1.20000 AFIX 0 C7' 1 -0.113427 0.977237 0.048782 11.00000 0.03837 0.03000 = 0.03502 0.00422 -0.00211 0.00112 AFIX 137 H7'A 2 -0.111939 0.997586 -0.011105 11.00000 -1.50000 H7'B 2 -0.148630 1.019891 0.070139 11.00000 -1.50000 H7'C 2 -0.128966 0.906635 0.048591 11.00000 -1.50000 AFIX 0 C8' 1 0.115678 0.742722 0.517873 11.00000 0.03448 0.02084 = 0.03271 0.00228 0.00755 0.00600 AFIX 23 H8'A 2 0.121019 0.684607 0.480055 11.00000 -1.20000 H8'B 2 0.082721 0.721920 0.556260 11.00000 -1.20000 AFIX 0 C9' 1 0.190650 0.769099 0.574672 11.00000 0.03169 0.03916 = 0.03928 0.00674 -0.00007 0.00642 AFIX 23 H9'A 2 0.222999 0.793070 0.536639 11.00000 -1.20000 H9'B 2 0.185078 0.824804 0.614828 11.00000 -1.20000 AFIX 0 C10' 1 0.226888 0.680487 0.628332 11.00000 0.04523 0.05611 = 0.04094 0.01160 0.00692 0.01941 AFIX 23 H10C 2 0.192377 0.652947 0.662149 11.00000 -1.20000 H10D 2 0.235951 0.627086 0.587799 11.00000 -1.20000 AFIX 0 C11' 1 0.298511 0.705858 0.691020 11.00000 0.05293 0.10538 = 0.06556 0.01134 -0.01183 0.02497 AFIX 137 H11D 2 0.332855 0.734199 0.658301 11.00000 -1.50000 H11E 2 0.319896 0.644627 0.721725 11.00000 -1.50000 H11F 2 0.289606 0.755337 0.734019 11.00000 -1.50000 AFIX 0 C12' 1 0.113852 1.182823 0.532062 11.00000 0.02617 0.02755 = 0.03004 -0.00178 0.01142 -0.00831 C13' 1 0.165212 1.106392 0.555512 11.00000 0.02703 0.03426 = 0.03682 -0.00366 0.01146 -0.00227 AFIX 43 H13' 2 0.176941 1.063733 0.511794 11.00000 -1.20000 AFIX 0 C14' 1 0.199417 1.092655 0.643481 11.00000 0.02976 0.04175 = 0.04569 0.00636 0.00608 0.00225 AFIX 43 H14' 2 0.234464 1.039998 0.660111 11.00000 -1.20000 AFIX 0 C15' 1 0.182816 1.155090 0.707026 11.00000 0.03499 0.05221 = 0.03319 0.00157 0.00367 -0.00691 AFIX 43 H15' 2 0.206499 1.145471 0.767166 11.00000 -1.20000 AFIX 0 C16' 1 0.131882 1.231322 0.683107 11.00000 0.03842 0.04204 = 0.03591 -0.00953 0.01439 -0.00648 AFIX 43 H16' 2 0.120599 1.274370 0.726837 11.00000 -1.20000 AFIX 0 C17' 1 0.097258 1.245369 0.596059 11.00000 0.03052 0.02878 = 0.03694 -0.00308 0.00871 -0.00236 AFIX 43 H17' 2 0.062019 1.297868 0.579828 11.00000 -1.20000 AFIX 0 HKLF 4 REM 5080f in P21/c #14 REM R1 = 0.0353 for 6293 Fo > 4sig(Fo) and 0.0725 for all 9047 data REM 401 parameters refined using 18 restraints END WGHT 0.0204 2.7452 REM Highest difference peak 0.387, deepest hole -0.399, 1-sigma level 0.079 Q1 1 0.6599 0.3950 0.6456 11.00000 0.05 0.39 Q2 1 0.6288 0.4978 0.5703 11.00000 0.05 0.36 Q3 1 0.6475 0.4967 0.5923 11.00000 0.05 0.35 Q4 1 0.0170 0.9373 0.4580 11.00000 0.05 0.35 Q5 1 -0.0777 0.9823 0.0787 11.00000 0.05 0.35 Q6 1 0.6145 0.3578 0.5865 11.00000 0.05 0.35 Q7 1 0.2587 0.7036 0.6502 11.00000 0.05 0.35 Q8 1 0.5086 0.1034 0.5524 11.00000 0.05 0.34 Q9 1 0.4821 0.0179 0.4045 11.00000 0.05 0.33 Q10 1 0.4988 0.2588 0.3412 11.00000 0.05 0.32 Q11 1 0.0421 0.9055 0.5392 11.00000 0.05 0.32 Q12 1 0.4857 0.1006 0.3815 11.00000 0.05 0.32 Q13 1 0.5404 0.5245 0.5391 11.00000 0.05 0.31 Q14 1 0.2190 0.8360 0.5812 11.00000 0.05 0.30 Q15 1 0.4863 0.1146 0.5460 11.00000 0.05 0.30 Q16 1 0.5038 0.1809 0.3739 11.00000 0.05 0.29 Q17 1 0.0843 0.8423 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2.26 -24 -5 9 1.91 1.90 -24 5 8 0.86 2.15 -24 5 8 0.17 2.43 -24 -5 8 0.17 2.29 -24 5 7 1.70 2.58 -24 5 7 -1.85 1.89 -24 -5 7 -0.45 2.25 -24 5 6 1.75 2.13 -24 5 6 -0.34 2.20 -24 -5 6 -0.58 1.72 -24 -5 6 2.04 2.39 -24 5 5 1.83 1.90 -24 5 5 1.87 2.03 -24 -5 5 4.26 2.17 -24 -5 5 1.53 2.41 -24 5 4 3.05 2.03 -24 5 4 -0.99 1.64 -24 5 4 -0.14 1.68 -24 -5 4 -0.40 2.27 -24 -5 4 2.77 2.10 -24 5 3 -2.67 1.58 -24 5 3 3.48 2.34 -24 5 3 0.60 2.21 -24 -5 3 1.52 2.34 -24 -5 3 -0.40 2.25 -24 5 2 7.38 2.73 -24 5 2 0.58 2.36 -24 -5 2 3.25 2.60 -24 -5 2 4.62 2.60 -24 5 1 1.22 2.32 -24 5 1 3.11 2.50 -24 -5 1 3.64 2.57 -24 -5 1 0.79 1.84 -24 5 0 7.37 2.78 -24 5 0 4.15 2.37 -24 -5 0 1.77 1.96 -24 -5 0 0.06 2.53 -24 6 8 3.04 2.78 -24 6 8 3.41 1.93 -24 -6 8 0.02 2.44 -24 6 7 2.13 2.13 -24 6 7 2.15 2.48 -24 -6 7 4.38 2.60 -24 6 6 3.94 2.31 -24 6 6 2.97 2.17 -24 -6 6 2.65 2.32 -24 -6 6 4.81 2.61 -24 6 5 -0.55 1.76 -24 6 5 -1.50 2.07 -24 -6 5 -2.96 1.73 -24 -6 5 -1.28 2.12 -24 6 4 3.40 2.04 -24 6 4 2.49 2.40 -24 -6 4 0.92 2.51 -24 -6 4 -0.77 1.96 -24 6 3 1.49 2.21 -24 6 3 3.25 2.40 -24 -6 3 2.70 2.19 -24 -6 3 5.09 2.76 -24 6 2 -0.60 2.21 -24 6 2 3.27 2.27 -24 -6 2 2.05 2.62 -24 -6 2 1.53 2.13 -24 6 1 2.79 2.49 -24 6 1 1.50 1.87 -24 -6 1 -1.23 2.06 -24 -6 1 -0.47 1.79 -25 0 10 0.50 2.37 -25 0 9 0.81 1.59 -25 0 8 6.97 2.51 -25 0 8 8.98 2.79 -25 0 7 -2.04 1.69 -25 0 7 -2.62 1.67 -25 0 6 6.72 2.40 -25 0 6 9.75 2.55 -25 0 6 5.08 2.12 -25 0 5 -0.85 2.09 -25 0 5 0.70 1.79 -25 0 5 -0.12 1.70 -25 0 5 2.10 1.91 -25 0 5 -0.66 1.75 -25 0 4 3.88 2.34 -25 0 4 1.88 1.95 -25 0 4 1.17 1.87 -25 0 4 2.84 2.14 -25 0 3 0.27 2.03 -25 0 3 -3.34 1.87 -25 0 3 0.28 1.91 -25 0 2 -1.05 1.80 -25 0 2 1.30 2.24 -25 0 2 0.50 1.89 -25 0 1 -2.95 1.72 -25 0 1 1.36 2.19 -25 0 1 -1.13 2.09 -25 0 0 5.32 2.52 -25 0 0 4.85 2.61 -25 1 9 1.80 2.25 -25 -1 9 4.01 2.35 -25 1 8 0.31 2.13 -25 1 8 1.93 2.10 -25 -1 8 0.93 1.77 -25 -1 8 2.22 1.91 -25 -1 8 -1.05 1.82 -25 1 7 10.97 2.88 -25 1 7 4.20 2.35 -25 -1 7 4.92 2.29 -25 -1 7 6.24 2.29 -25 -1 7 4.17 2.32 -25 1 6 5.19 2.32 -25 1 6 4.40 2.31 -25 1 6 2.57 1.93 -25 -1 6 4.68 2.17 -25 -1 6 4.24 2.09 -25 1 5 -1.57 1.70 -25 1 5 0.78 1.81 -25 1 5 2.99 2.01 -25 1 5 3.24 1.99 -25 -1 5 3.34 2.03 -25 -1 5 -2.60 1.72 -25 -1 5 -1.30 1.74 -25 1 4 3.21 2.27 -25 1 4 0.75 1.91 -25 1 4 4.79 3.15 -25 1 4 2.96 2.05 -25 1 4 3.62 2.50 -25 -1 4 1.61 2.07 -25 -1 4 -0.18 1.86 -25 1 3 3.24 2.27 -25 1 3 4.96 2.42 -25 1 3 5.37 2.30 -25 1 3 4.73 2.10 -25 -1 3 1.89 2.17 -25 -1 3 0.77 2.05 -25 -1 3 4.62 2.35 -25 1 2 8.61 2.60 -25 1 2 13.15 2.88 -25 1 2 12.93 2.70 -25 1 2 11.90 2.80 -25 -1 2 19.06 3.10 -25 -1 2 8.65 2.76 -25 -1 2 12.62 2.92 -25 1 1 0.63 1.95 -25 1 1 0.69 2.12 -25 1 1 -0.99 2.01 -25 -1 1 -0.94 1.86 -25 -1 1 3.42 2.38 -25 -1 1 2.36 2.21 -25 1 0 -1.25 1.60 -25 1 0 -0.15 2.25 -25 -1 0 -0.75 2.22 -25 -1 0 0.84 2.36 -25 2 9 2.61 2.44 -25 2 9 2.99 2.30 -25 -2 9 3.59 2.10 -25 -2 9 0.60 2.16 -25 2 8 3.81 2.42 -25 2 8 3.69 1.88 -25 2 8 2.98 2.32 -25 -2 8 -1.48 1.80 -25 -2 8 1.36 1.61 -25 2 7 4.13 2.00 -25 2 7 1.58 2.21 -25 2 7 4.11 2.36 -25 -2 7 5.74 2.29 -25 -2 7 1.89 2.22 -25 2 6 2.40 2.28 -25 2 6 5.53 2.12 -25 2 6 -0.15 1.98 -25 -2 6 2.12 1.86 -25 -2 6 0.83 2.01 -25 2 5 2.13 2.16 -25 2 5 3.96 2.34 -25 2 5 0.87 1.73 -25 2 5 0.09 1.90 -25 -2 5 -0.43 1.64 -25 -2 5 -0.53 2.01 -25 -2 5 -1.95 1.78 -25 2 4 5.34 2.56 -25 2 4 5.94 2.42 -25 2 4 6.13 2.27 -25 -2 4 3.71 1.90 -25 -2 4 4.01 2.21 -25 2 3 14.60 2.94 -25 2 3 13.90 3.04 -25 2 3 13.84 2.83 -25 -2 3 10.96 2.78 -25 -2 3 16.04 3.11 -25 2 2 2.06 2.11 -25 2 2 3.39 2.18 -25 2 2 0.71 2.09 -25 -2 2 0.67 1.71 -25 -2 2 -0.67 2.00 -25 2 1 6.92 2.65 -25 2 1 5.76 2.21 -25 2 1 4.26 2.29 -25 -2 1 5.36 2.51 -25 -2 1 5.58 2.47 -25 -2 1 9.04 2.80 -25 2 0 1.54 2.25 -25 -2 0 -1.41 2.21 -25 3 9 -0.56 2.19 -25 -3 9 -2.77 1.90 -25 3 8 -0.53 2.04 -25 3 8 2.05 2.27 -25 -3 8 0.67 2.06 -25 3 7 3.32 2.21 -25 3 7 2.69 2.25 -25 -3 7 0.18 1.95 -25 3 6 3.75 2.31 -25 3 6 3.29 2.38 -25 3 6 4.55 2.20 -25 -3 6 6.25 2.54 -25 3 5 -2.21 1.53 -25 3 5 0.09 1.90 -25 3 5 -0.61 1.94 -25 -3 5 -0.72 1.75 -25 -3 5 -1.26 2.01 -25 -3 5 0.46 1.64 -25 3 4 7.06 2.49 -25 3 4 1.76 2.13 -25 3 4 7.41 2.43 -25 3 4 1.63 1.97 -25 -3 4 10.70 3.01 -25 -3 4 3.37 2.16 -25 3 3 -0.49 2.00 -25 3 3 -1.80 1.91 -25 3 3 -0.95 1.69 -25 -3 3 -1.11 2.07 -25 -3 3 -0.07 2.07 -25 3 2 5.33 2.41 -25 3 2 4.41 2.18 -25 3 2 4.56 2.48 -25 -3 2 3.92 2.37 -25 -3 2 1.89 2.34 -25 3 1 2.40 2.37 -25 3 1 1.63 1.99 -25 3 1 1.68 2.02 -25 -3 1 1.21 1.77 -25 -3 1 -0.07 2.33 -25 4 7 0.99 2.05 -25 4 7 1.23 2.40 -25 -4 7 -1.94 2.09 -25 4 6 4.60 2.66 -25 4 6 3.28 2.19 -25 -4 6 3.49 2.40 -25 4 5 0.04 2.21 -25 4 5 1.32 2.01 -25 4 5 -0.90 1.66 -25 -4 5 -2.84 1.94 -25 -4 5 0.01 1.99 -25 4 4 6.42 2.64 -25 4 4 9.09 2.76 -25 -4 4 10.80 2.69 -25 -4 4 6.84 2.81 -25 4 3 -1.09 1.96 -25 4 3 0.91 2.18 -25 -4 3 -1.43 2.15 -25 -4 3 -1.82 2.04 -25 4 2 1.29 2.00 -25 -4 2 -0.93 2.24 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 76640 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Se Se 0.59823(2) -0.10619(2) 0.37071(2) 0.02630(7) Uani 1 1 d . . S S 0.50003(5) 0.33991(6) 0.33807(5) 0.0430(2) Uani 1 1 d . . P P 0.48218(4) -0.06872(5) 0.39159(4) 0.02047(14) Uani 1 1 d . . N1 N 0.49052(11) 0.13538(15) 0.35364(13) 0.0220(5) Uani 1 1 d . . N2 N 0.51311(11) 0.21461(15) 0.47861(13) 0.0228(5) Uani 1 1 d . . C1 C 0.49357(13) 0.06299(18) 0.41882(15) 0.0193(5) Uani 1 1 d . . C2 C 0.50147(14) 0.22957(19) 0.38988(17) 0.0263(6) Uani 1 1 d . . C3 C 0.50807(13) 0.11271(18) 0.49755(15) 0.0192(5) Uani 1 1 d . . C4 C 0.47018(14) 0.1171(2) 0.25882(16) 0.0258(6) Uani 1 1 d . . H4A H 0.4896 0.0506 0.2461 0.031 Uiso 1 1 calc R . H4B H 0.4931 0.1692 0.2284 0.031 Uiso 1 1 calc R . C5 C 0.38728(14) 0.1189(2) 0.22371(17) 0.0288(6) Uani 1 1 d . . H5A H 0.3646 0.0674 0.2550 0.035 Uiso 1 1 calc R . H5B H 0.3682 0.1856 0.2364 0.035 Uiso 1 1 calc R . C6 C 0.36398(15) 0.0992(2) 0.12585(17) 0.0332(7) Uani 1 1 d . . H6A H 0.3779 0.0296 0.1136 0.040 Uiso 1 1 calc R . H6B H 0.3906 0.1460 0.0946 0.040 Uiso 1 1 calc R . C7 C 0.28125(17) 0.1128(3) 0.0910(2) 0.0506(9) Uani 1 1 d . . H7A H 0.2547 0.0670 0.1221 0.076 Uiso 1 1 calc GR . H7B H 0.2681 0.0977 0.0279 0.076 Uiso 1 1 calc GR . H7C H 0.2676 0.1826 0.1006 0.076 Uiso 1 1 calc GR . C8 C 0.53094(15) 0.2967(2) 0.54242(18) 0.0304(6) Uani 1 1 d . U H8A H 0.5178 0.2760 0.5978 0.036 Uiso 1 1 calc R . H8B H 0.5007 0.3564 0.5194 0.036 Uiso 1 1 calc R . C9 C 0.61132(17) 0.3254(2) 0.5619(2) 0.0402(6) Uani 1 1 d . U H9A H 0.6259 0.3406 0.5061 0.048 Uiso 1 1 calc R . H9B H 0.6416 0.2680 0.5904 0.048 Uiso 1 1 calc R . C10 C 0.6260(2) 0.4169(3) 0.6220(2) 0.0563(8) Uani 1 1 d . U H10A H 0.5910 0.4711 0.5965 0.068 Uiso 1 1 calc R . H10B H 0.6164 0.3987 0.6798 0.068 Uiso 1 1 calc R . C11 C 0.7027(2) 0.4561(3) 0.6357(3) 0.0889(12) Uani 1 1 d . U H11A H 0.7077 0.5173 0.6718 0.133 Uiso 1 1 calc GR . H11B H 0.7134 0.4720 0.5786 0.133 Uiso 1 1 calc GR . H11C H 0.7375 0.4050 0.6657 0.133 Uiso 1 1 calc GR . C12 C 0.65744(14) -0.0681(2) 0.48357(17) 0.0272(6) Uani 1 1 d . . C13 C 0.67924(15) 0.0312(2) 0.50138(19) 0.0323(7) Uani 1 1 d . . H13 H 0.6623 0.0821 0.4588 0.039 Uiso 1 1 calc R . C14 C 0.72583(16) 0.0561(3) 0.5815(2) 0.0431(8) Uani 1 1 d . . H14 H 0.7407 0.1241 0.5939 0.052 Uiso 1 1 calc R . C15 C 0.75042(16) -0.0179(3) 0.6429(2) 0.0489(9) Uani 1 1 d . . H15 H 0.7824 -0.0006 0.6976 0.059 Uiso 1 1 calc R . C16 C 0.72919(17) -0.1167(3) 0.6258(2) 0.0455(8) Uani 1 1 d . . H16 H 0.7468 -0.1673 0.6686 0.055 Uiso 1 1 calc R . C17 C 0.68215(15) -0.1425(2) 0.54628(19) 0.0348(7) Uani 1 1 d . . H17 H 0.6669 -0.2105 0.5347 0.042 Uiso 1 1 calc R . Se' Se 0.06298(2) 1.20258(2) 0.41186(2) 0.03196(8) Uani 1 1 d . . S' S 0.11719(5) 0.75455(6) 0.31324(5) 0.0417(2) Uani 1 1 d . . P' P -0.02932(4) 1.08472(5) 0.40169(4) 0.02325(15) Uani 1 1 d . . N1' N 0.04877(12) 0.92617(15) 0.34932(13) 0.0241(5) Uani 1 1 d . . N2' N 0.08116(12) 0.82661(15) 0.46190(14) 0.0244(5) Uani 1 1 d . . C1' C 0.02356(13) 0.96991(18) 0.41792(15) 0.0208(5) Uani 1 1 d . . C2' C 0.08293(14) 0.83632(19) 0.37525(17) 0.0261(6) Uani 1 1 d . . C3' C 0.04442(13) 0.90783(18) 0.48884(16) 0.0213(5) Uani 1 1 d . . C4' C 0.04162(14) 0.9689(2) 0.26151(16) 0.0271(6) Uani 1 1 d . . H4'A H 0.0788 0.9372 0.2338 0.033 Uiso 1 1 calc R . H4'B H 0.0526 1.0420 0.2672 0.033 Uiso 1 1 calc R . C5' C -0.03449(14) 0.9544(2) 0.20179(16) 0.0259(6) Uani 1 1 d . . H5'A H -0.0481 0.8822 0.2010 0.031 Uiso 1 1 calc R . H5'B H -0.0712 0.9930 0.2255 0.031 Uiso 1 1 calc R . C6' C -0.03705(15) 0.9890(2) 0.10882(17) 0.0310(6) Uani 1 1 d . . H6'A H -0.0011 0.9493 0.0848 0.037 Uiso 1 1 calc R . H6'B H -0.0222 1.0607 0.1099 0.037 Uiso 1 1 calc R . C7' C -0.11343(16) 0.9772(2) 0.04878(18) 0.0362(7) Uani 1 1 d . . H7'A H -0.1119 0.9976 -0.0111 0.054 Uiso 1 1 calc GR . H7'B H -0.1486 1.0199 0.0701 0.054 Uiso 1 1 calc GR . H7'C H -0.1290 0.9066 0.0486 0.054 Uiso 1 1 calc GR . C8' C 0.11568(15) 0.74272(19) 0.51787(18) 0.0294(6) Uani 1 1 d . . H8'A H 0.1210 0.6846 0.4801 0.035 Uiso 1 1 calc R . H8'B H 0.0827 0.7219 0.5563 0.035 Uiso 1 1 calc R . C9' C 0.19065(16) 0.7691(2) 0.5747(2) 0.0380(7) Uani 1 1 d . . H9'A H 0.2230 0.7931 0.5366 0.046 Uiso 1 1 calc R . H9'B H 0.1851 0.8248 0.6148 0.046 Uiso 1 1 calc R . C10' C 0.22689(18) 0.6805(3) 0.6283(2) 0.0479(9) Uani 1 1 d . . H10C H 0.1924 0.6529 0.6621 0.057 Uiso 1 1 calc R . H10D H 0.2360 0.6271 0.5878 0.057 Uiso 1 1 calc R . C11' C 0.2985(2) 0.7059(3) 0.6910(3) 0.0787(13) Uani 1 1 d . . H11D H 0.3329 0.7342 0.6583 0.118 Uiso 1 1 calc GR . H11E H 0.3199 0.6446 0.7217 0.118 Uiso 1 1 calc GR . H11F H 0.2896 0.7553 0.7340 0.118 Uiso 1 1 calc GR . C12' C 0.11385(14) 1.18282(19) 0.53206(17) 0.0271(6) Uani 1 1 d . . C13' C 0.16521(15) 1.1064(2) 0.55551(19) 0.0320(6) Uani 1 1 d . . H13' H 0.1769 1.0637 0.5118 0.038 Uiso 1 1 calc R . C14' C 0.19942(16) 1.0927(2) 0.6435(2) 0.0395(7) Uani 1 1 d . . H14' H 0.2345 1.0400 0.6601 0.047 Uiso 1 1 calc R . C15' C 0.18282(17) 1.1551(2) 0.7070(2) 0.0408(8) Uani 1 1 d . . H15' H 0.2065 1.1455 0.7672 0.049 Uiso 1 1 calc R . C16' C 0.13188(16) 1.2313(2) 0.6831(2) 0.0378(7) Uani 1 1 d . . H16' H 0.1206 1.2744 0.7268 0.045 Uiso 1 1 calc R . C17' C 0.09726(15) 1.2454(2) 0.59606(18) 0.0319(6) Uani 1 1 d . . H17' H 0.0620 1.2979 0.5798 0.038 Uiso 1 1 calc R . 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 Se 0.02709(14) 0.02980(15) 0.02338(14) -0.00392(11) 0.00865(11) 0.00096(12) S 0.0645(6) 0.0271(4) 0.0341(4) 0.0119(3) 0.0044(4) -0.0048(4) P 0.0229(3) 0.0226(3) 0.0153(3) -0.0008(3) 0.0032(3) -0.0022(3) N1 0.0270(12) 0.0238(11) 0.0147(10) 0.0036(9) 0.0037(9) 0.0000(9) N2 0.0276(12) 0.0190(11) 0.0218(11) 0.0000(9) 0.0058(9) -0.0010(9) C1 0.0200(13) 0.0211(12) 0.0170(12) 0.0025(10) 0.0044(10) 0.0000(10) C2 0.0263(15) 0.0275(14) 0.0240(14) 0.0035(11) 0.0034(12) -0.0030(11) C3 0.0210(13) 0.0172(12) 0.0193(12) 0.0016(10) 0.0043(10) -0.0009(10) C4 0.0293(14) 0.0311(14) 0.0176(13) 0.0046(11) 0.0069(11) 0.0003(12) C5 0.0286(15) 0.0328(15) 0.0248(14) 0.0002(12) 0.0054(12) -0.0022(12) C6 0.0338(16) 0.0348(16) 0.0286(15) -0.0052(12) 0.0021(13) -0.0005(13) C7 0.0367(18) 0.060(2) 0.047(2) -0.0049(17) -0.0071(15) -0.0055(16) C8 0.0383(14) 0.0242(12) 0.0311(13) -0.0067(11) 0.0129(11) -0.0057(11) C9 0.0436(13) 0.0391(13) 0.0392(13) -0.0096(11) 0.0123(11) -0.0134(11) C10 0.0576(16) 0.0546(16) 0.0550(16) -0.0169(13) 0.0095(14) -0.0215(14) C11 0.086(3) 0.094(3) 0.083(3) -0.020(2) 0.011(2) -0.047(2) C12 0.0223(14) 0.0362(15) 0.0238(14) -0.0014(12) 0.0070(11) 0.0025(12) C13 0.0243(15) 0.0373(16) 0.0367(17) -0.0043(13) 0.0102(13) -0.0009(13) C14 0.0265(16) 0.055(2) 0.048(2) -0.0194(17) 0.0097(15) -0.0090(15) C15 0.0242(16) 0.090(3) 0.0304(17) -0.0113(18) 0.0019(14) -0.0020(18) C16 0.0324(17) 0.073(2) 0.0307(17) 0.0111(17) 0.0064(14) 0.0077(17) C17 0.0261(15) 0.0441(18) 0.0355(17) 0.0016(14) 0.0096(13) 0.0029(13) Se' 0.04341(18) 0.02457(14) 0.02949(16) 0.00424(12) 0.01169(13) -0.00602(13) S' 0.0524(5) 0.0360(4) 0.0408(5) -0.0093(4) 0.0189(4) 0.0105(4) P' 0.0299(4) 0.0200(3) 0.0192(3) 0.0015(3) 0.0044(3) 0.0022(3) N1' 0.0277(12) 0.0227(11) 0.0222(11) -0.0028(9) 0.0063(10) -0.0010(9) N2' 0.0283(12) 0.0201(11) 0.0238(12) -0.0015(9) 0.0039(10) 0.0040(9) C1' 0.0229(13) 0.0217(13) 0.0177(13) -0.0015(10) 0.0044(11) 0.0010(11) C2' 0.0263(15) 0.0250(14) 0.0270(14) -0.0027(11) 0.0061(12) -0.0006(12) C3' 0.0216(13) 0.0217(13) 0.0200(13) -0.0016(10) 0.0033(11) -0.0013(11) C4' 0.0310(15) 0.0317(15) 0.0199(13) -0.0005(11) 0.0086(12) -0.0025(12) C5' 0.0295(15) 0.0271(14) 0.0218(13) -0.0047(11) 0.0073(12) -0.0038(12) C6' 0.0319(15) 0.0343(16) 0.0257(15) 0.0016(12) 0.0043(12) -0.0020(13) C7' 0.0384(17) 0.0300(15) 0.0350(17) 0.0042(13) -0.0021(14) 0.0011(13) C8' 0.0345(16) 0.0208(13) 0.0327(16) 0.0023(12) 0.0076(13) 0.0060(12) C9' 0.0317(16) 0.0392(17) 0.0393(17) 0.0067(14) -0.0001(14) 0.0064(14) C10' 0.045(2) 0.056(2) 0.0409(19) 0.0116(16) 0.0069(16) 0.0194(17) C11' 0.053(2) 0.105(3) 0.066(3) 0.011(2) -0.012(2) 0.025(2) C12' 0.0262(14) 0.0276(14) 0.0300(15) -0.0018(12) 0.0114(12) -0.0083(12) C13' 0.0270(15) 0.0343(15) 0.0368(16) -0.0037(13) 0.0115(13) -0.0023(13) C14' 0.0298(16) 0.0418(18) 0.0457(19) 0.0064(15) 0.0061(14) 0.0023(14) C15' 0.0350(17) 0.052(2) 0.0332(17) 0.0016(15) 0.0037(14) -0.0069(16) C16' 0.0384(18) 0.0420(18) 0.0359(17) -0.0095(14) 0.0144(14) -0.0065(15) C17' 0.0305(16) 0.0288(15) 0.0369(17) -0.0031(13) 0.0087(13) -0.0024(12) 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' 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' Se Se -0.0929 2.2259 '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 C12 Se P 99.85(8) . . C1 P Se 100.32(8) . . C3 P Se 100.10(8) 3_656 . C3 P C1 96.16(11) 3_656 . C1 N1 C4 125.7(2) . . C2 N1 C1 110.5(2) . . C2 N1 C4 123.4(2) . . C2 N2 C3 110.7(2) . . C2 N2 C8 122.8(2) . . C3 N2 C8 126.5(2) . . N1 C1 P 120.97(17) . . C3 C1 P 132.03(19) . . C3 C1 N1 107.0(2) . . N1 C2 S 128.0(2) . . N2 C2 S 126.8(2) . . N2 C2 N1 105.1(2) . . N2 C3 P 121.58(17) . 3_656 C1 C3 P 131.75(19) . 3_656 C1 C3 N2 106.6(2) . . N1 C4 C5 111.7(2) . . C6 C5 C4 113.3(2) . . C5 C6 C7 111.9(2) . . N2 C8 C9 112.7(2) . . C8 C9 C10 110.8(3) . . C11 C10 C9 113.5(3) . . C13 C12 Se 120.9(2) . . C13 C12 C17 119.9(3) . . C17 C12 Se 119.1(2) . . C12 C13 C14 120.0(3) . . C15 C14 C13 119.8(3) . . C14 C15 C16 120.7(3) . . C15 C16 C17 120.0(3) . . C16 C17 C12 119.6(3) . . C12' Se' P' 99.63(8) . . C1' P' Se' 100.99(9) . . C3' P' Se' 100.02(8) 3_576 . C3' P' C1' 96.45(11) 3_576 . C1' N1' C4' 125.9(2) . . C2' N1' C1' 110.6(2) . . C2' N1' C4' 123.5(2) . . C2' N2' C3' 110.6(2) . . C2' N2' C8' 123.6(2) . . C3' N2' C8' 125.8(2) . . N1' C1' P' 120.97(18) . . C3' C1' P' 132.09(19) . . C3' C1' N1' 106.9(2) . . N1' C2' S' 127.3(2) . . N2' C2' S' 127.6(2) . . N2' C2' N1' 105.1(2) . . N2' C3' P' 121.66(18) . 3_576 C1' C3' P' 131.45(19) . 3_576 C1' C3' N2' 106.9(2) . . N1' C4' C5' 113.5(2) . . C6' C5' C4' 111.8(2) . . C5' C6' C7' 112.3(2) . . N2' C8' C9' 113.1(2) . . C10' C9' C8' 112.3(2) . . C11' C10' C9' 113.8(3) . . C13' C12' Se' 121.0(2) . . C13' C12' C17' 120.1(3) . . C17' C12' Se' 118.9(2) . . C12' C13' C14' 119.4(3) . . C15' C14' C13' 120.4(3) . . C16' C15' C14' 119.9(3) . . C17' C16' C15' 120.2(3) . . C16' C17' C12' 120.0(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Se P 2.3098(7) . Se C12 1.919(3) . S C2 1.670(3) . P C1 1.799(2) . P C3 1.796(2) 3_656 N1 C1 1.391(3) . N1 C2 1.368(3) . N1 C4 1.462(3) . N2 C2 1.367(3) . N2 C3 1.392(3) . N2 C8 1.462(3) . C1 C3 1.367(3) . C3 P 1.796(2) 3_656 C4 C5 1.513(4) . C5 C6 1.513(3) . C6 C7 1.520(4) . C8 C9 1.504(4) . C9 C10 1.521(4) . C10 C11 1.487(5) . C12 C13 1.387(4) . C12 C17 1.393(4) . C13 C14 1.389(4) . C14 C15 1.374(4) . C15 C16 1.378(5) . C16 C17 1.388(4) . Se' P' 2.3003(7) . Se' C12' 1.916(3) . S' C2' 1.675(3) . P' C1' 1.799(2) . P' C3' 1.798(3) 3_576 N1' C1' 1.391(3) . N1' C2' 1.367(3) . N1' C4' 1.462(3) . N2' C2' 1.367(3) . N2' C3' 1.392(3) . N2' C8' 1.469(3) . C1' C3' 1.363(3) . C3' P' 1.798(3) 3_576 C4' C5' 1.518(4) . C5' C6' 1.513(3) . C6' C7' 1.520(4) . C8' C9' 1.512(4) . C9' C10' 1.510(4) . C10' C11' 1.499(5) . C12' C13' 1.383(4) . C12' C17' 1.387(4) . C13' C14' 1.387(4) . C14' C15' 1.381(4) . C15' C16' 1.377(4) . C16' C17' 1.377(4) .