#------------------------------------------------------------------------------ #$Date: 2020-07-06 06:31:08 +0300 (Mon, 06 Jul 2020) $ #$Revision: 253953 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/05/96/7059671.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_7059671 loop_ _publ_author_name 'Ling, Irene' 'Skelton, Brian W.' 'Sobolev, Alexandre N.' 'Alias, Yatimah' 'Khor, Zong Chin' 'Raston, Colin L.' _publ_section_title ; Effect of anions on the solid-state interplay of symmetric and unsymmetric phosphonium cations ; _journal_issue 25 _journal_name_full 'New Journal of Chemistry' _journal_page_first 10220 _journal_paper_doi 10.1039/D0NJ01975E _journal_volume 44 _journal_year 2020 _chemical_formula_moiety 'C25 H22 P, C N S' _chemical_formula_sum 'C26 H22 N P S' _chemical_formula_weight 411.47 _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 geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-12-02 deposited with the CCDC. 2020-05-22 downloaded from the CCDC. ; _cell_angle_alpha 70.204(4) _cell_angle_beta 84.593(4) _cell_angle_gamma 76.784(4) _cell_formula_units_Z 4 _cell_length_a 9.8950(4) _cell_length_b 12.8564(5) _cell_length_c 18.7165(9) _cell_measurement_reflns_used 3679 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.2460 _cell_measurement_theta_min 2.9320 _cell_volume 2180.59(17) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'X-Seed v. 4.0 (Barbour, 2001)' _computing_publication_material 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2015/1 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0009 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur-S' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0488276 _diffrn_orient_matrix_UB_12 -0.0475322 _diffrn_orient_matrix_UB_13 0.0214141 _diffrn_orient_matrix_UB_21 -0.0183861 _diffrn_orient_matrix_UB_22 0.0164907 _diffrn_orient_matrix_UB_23 0.0327484 _diffrn_orient_matrix_UB_31 -0.0519747 _diffrn_orient_matrix_UB_32 -0.0326427 _diffrn_orient_matrix_UB_33 0.0095796 _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_unetI/netI 0.0938 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 18157 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 2.911 _exptl_absorpt_coefficient_mu 0.234 _exptl_absorpt_correction_T_max 0.990 _exptl_absorpt_correction_T_min 0.965 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET) (compiled Jan 14 2014,18:38:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.253 _exptl_crystal_description needle _exptl_crystal_F_000 864 _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.050 _refine_diff_density_max 1.287 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 523 _refine_ls_number_reflns 8913 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.002 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0625 _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^)+(0.0450P)^2^+1.5000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1234 _refine_ls_wR_factor_ref 0.1434 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5838 _reflns_number_total 8913 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0nj01975e1.cif _cod_data_source_block 090604j _cod_depositor_comments 'Adding full bibliography for 7059666--7059672.cif.' _cod_original_cell_volume 2180.60(17) _cod_database_code 7059671 _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 0.942 _shelx_estimated_absorpt_t_max 0.988 _shelx_res_file ; TITL 090604j in P-1, C25 H22 P, S C N 090604j.res created by SHELXL-2018/3 at 15:09:46 on 08-Jul-2018 CELL 0.71073 9.8950 12.8564 18.7165 70.204 84.593 76.784 ZERR 4.00 0.0004 0.0005 0.0009 0.004 0.004 0.004 LATT 1 SFAC C H N P S UNIT 104 88 4 4 4 SHEL 100 0.8 OMIT -1 -1 1 OMIT 0 2 2 ACTA TEMP -173 SIZE 0.26 0.09 0.05 BOND $H L.S. 6 WGHT 0.045000 1.500000 FVAR 0.17815 P1 4 0.329077 0.197613 0.360789 11.00000 0.02443 0.02374 = 0.02255 -0.00749 -0.00217 -0.00042 C1 1 0.197601 0.272641 0.289603 11.00000 0.02181 0.02828 = 0.02374 -0.00842 -0.00386 -0.00026 AFIX 23 H1A 2 0.179077 0.219439 0.265759 11.00000 -1.20000 H1B 2 0.110521 0.298927 0.314949 11.00000 -1.20000 AFIX 0 C111 1 0.236847 0.373370 0.227978 11.00000 0.01960 0.02706 = 0.02194 -0.00214 -0.00713 -0.00047 C112 1 0.302594 0.358428 0.162374 11.00000 0.02211 0.02829 = 0.02680 -0.00787 -0.00617 0.00001 AFIX 43 H112 2 0.326901 0.285013 0.157841 11.00000 -1.20000 AFIX 0 C113 1 0.332945 0.450032 0.103474 11.00000 0.02254 0.04335 = 0.02372 0.00070 -0.00401 -0.00383 AFIX 43 H113 2 0.377688 0.439368 0.058533 11.00000 -1.20000 AFIX 0 C114 1 0.298435 0.557003 0.109749 11.00000 0.02684 0.03472 = 0.03337 0.00773 -0.00897 -0.01022 AFIX 43 H114 2 0.318808 0.619759 0.068964 11.00000 -1.20000 AFIX 0 C115 1 0.234388 0.572896 0.175182 11.00000 0.02671 0.02577 = 0.04303 -0.00265 -0.01464 -0.00633 AFIX 43 H115 2 0.212119 0.646262 0.179816 11.00000 -1.20000 AFIX 0 C116 1 0.202670 0.481324 0.234146 11.00000 0.02648 0.02842 = 0.02995 -0.00793 -0.00624 -0.00082 AFIX 43 H116 2 0.157457 0.492309 0.278905 11.00000 -1.20000 AFIX 0 C121 1 0.349722 0.281092 0.417241 11.00000 0.02734 0.02714 = 0.02362 -0.01074 -0.00175 -0.00442 C122 1 0.230970 0.344284 0.440641 11.00000 0.02487 0.03413 = 0.02839 -0.01128 -0.00092 -0.00340 AFIX 43 H122 2 0.142971 0.350150 0.421513 11.00000 -1.20000 AFIX 0 C123 1 0.241217 0.398281 0.491548 11.00000 0.03449 0.03845 = 0.03447 -0.01901 0.00511 -0.00685 AFIX 43 H123 2 0.160251 0.441310 0.507586 11.00000 -1.20000 AFIX 0 C124 1 0.369964 0.389795 0.519423 11.00000 0.04543 0.03958 = 0.02900 -0.01833 0.00325 -0.01189 AFIX 43 H124 2 0.376921 0.427781 0.554085 11.00000 -1.20000 AFIX 0 C125 1 0.488089 0.326270 0.496928 11.00000 0.03411 0.04421 = 0.02738 -0.01246 -0.00659 -0.00774 AFIX 43 H125 2 0.575749 0.320695 0.516318 11.00000 -1.20000 AFIX 0 C126 1 0.479222 0.271051 0.446544 11.00000 0.02538 0.03596 = 0.02560 -0.01111 -0.00376 0.00044 AFIX 43 H126 2 0.560208 0.226505 0.431756 11.00000 -1.20000 AFIX 0 C131 1 0.266931 0.076710 0.422485 11.00000 0.02839 0.02286 = 0.02403 -0.00431 -0.00030 -0.00091 C132 1 0.269204 0.052149 0.501162 11.00000 0.03334 0.03021 = 0.02919 -0.00426 -0.00585 -0.00289 AFIX 43 H132 2 0.309198 0.095847 0.521956 11.00000 -1.20000 AFIX 0 C133 1 0.212421 -0.036645 0.548304 11.00000 0.03593 0.03395 = 0.02523 -0.00149 -0.00358 -0.00341 AFIX 43 H133 2 0.212596 -0.053295 0.601777 11.00000 -1.20000 AFIX 0 C134 1 0.155986 -0.100784 0.518766 11.00000 0.03208 0.02193 = 0.02952 -0.00032 0.00574 0.00187 AFIX 43 H134 2 0.118457 -0.161906 0.552114 11.00000 -1.20000 AFIX 0 C135 1 0.152722 -0.077907 0.440780 11.00000 0.03430 0.02624 = 0.03383 -0.00948 0.00321 -0.00571 AFIX 43 H135 2 0.113514 -0.122944 0.420792 11.00000 -1.20000 AFIX 0 C136 1 0.207832 0.012105 0.392321 11.00000 0.03756 0.02636 = 0.02403 -0.00634 0.00298 -0.00390 AFIX 43 H136 2 0.205209 0.029496 0.338862 11.00000 -1.20000 AFIX 0 C141 1 0.492483 0.158649 0.315882 11.00000 0.02318 0.02966 = 0.01970 -0.01203 -0.00709 0.00358 C142 1 0.538848 0.050093 0.312439 11.00000 0.02961 0.03619 = 0.03671 -0.01939 -0.00600 -0.00329 AFIX 43 H142 2 0.484310 -0.005356 0.334057 11.00000 -1.20000 AFIX 0 C143 1 0.665753 0.023026 0.277108 11.00000 0.03203 0.03709 = 0.04905 -0.02839 -0.00621 0.00449 AFIX 43 H143 2 0.697303 -0.050849 0.273911 11.00000 -1.20000 AFIX 0 C144 1 0.746167 0.103156 0.246625 11.00000 0.02946 0.04779 = 0.02373 -0.01635 -0.00334 -0.00455 AFIX 43 H144 2 0.833160 0.083775 0.223054 11.00000 -1.20000 AFIX 0 C145 1 0.701185 0.210483 0.250183 11.00000 0.03147 0.03580 = 0.01965 -0.00050 -0.00061 -0.00402 AFIX 43 H145 2 0.757488 0.264851 0.229625 11.00000 -1.20000 AFIX 0 C146 1 0.574076 0.239568 0.283638 11.00000 0.03160 0.02828 = 0.01985 -0.00177 -0.00257 -0.00070 AFIX 43 H146 2 0.541926 0.314505 0.284793 11.00000 -1.20000 AFIX 0 P2 4 0.679776 0.738921 0.157500 11.00000 0.01553 0.01948 = 0.02130 -0.00650 -0.00169 -0.00292 C2 1 0.611320 0.861040 0.077410 11.00000 0.02155 0.01971 = 0.02072 -0.00405 -0.00205 -0.00446 AFIX 23 H2A 2 0.578677 0.926805 0.095402 11.00000 -1.20000 H2B 2 0.687843 0.877968 0.040149 11.00000 -1.20000 AFIX 0 C211 1 0.492647 0.848377 0.036981 11.00000 0.01979 0.01441 = 0.01989 0.00011 -0.00332 -0.00362 C212 1 0.355173 0.879921 0.058740 11.00000 0.02282 0.02443 = 0.02126 -0.00624 -0.00066 0.00105 AFIX 43 H212 2 0.334019 0.905473 0.101356 11.00000 -1.20000 AFIX 0 C213 1 0.248112 0.873715 0.017310 11.00000 0.01558 0.02711 = 0.02721 -0.00622 0.00161 -0.00024 AFIX 43 H213 2 0.154091 0.894506 0.032197 11.00000 -1.20000 AFIX 0 C214 1 0.278676 0.837548 -0.044987 11.00000 0.02124 0.02585 = 0.02611 -0.00213 -0.00779 -0.00471 AFIX 43 H214 2 0.205691 0.834272 -0.073178 11.00000 -1.20000 AFIX 0 C215 1 0.415653 0.805995 -0.066501 11.00000 0.02835 0.02534 = 0.02077 -0.00809 -0.00178 -0.00239 AFIX 43 H215 2 0.436527 0.780699 -0.109235 11.00000 -1.20000 AFIX 0 C216 1 0.522529 0.811360 -0.025542 11.00000 0.01748 0.02184 = 0.02459 -0.00503 -0.00054 -0.00310 AFIX 43 H216 2 0.616371 0.789632 -0.040358 11.00000 -1.20000 AFIX 0 C221 1 0.745493 0.617156 0.128732 11.00000 0.01867 0.01799 = 0.01601 -0.00183 -0.00143 -0.00251 C222 1 0.887943 0.581905 0.119738 11.00000 0.02158 0.02956 = 0.02671 -0.00929 -0.00378 -0.00478 AFIX 43 H222 2 0.949974 0.622324 0.128920 11.00000 -1.20000 AFIX 0 C223 1 0.939204 0.487814 0.097382 11.00000 0.02129 0.03587 = 0.03193 -0.01201 -0.00394 0.00419 AFIX 43 H223 2 1.036505 0.463678 0.091381 11.00000 -1.20000 AFIX 0 C224 1 0.849646 0.429054 0.083805 11.00000 0.03536 0.02136 = 0.02385 -0.00852 -0.00162 0.00492 AFIX 43 H224 2 0.885221 0.364652 0.068370 11.00000 -1.20000 AFIX 0 C225 1 0.707113 0.464075 0.092708 11.00000 0.03631 0.02140 = 0.02158 -0.00688 -0.00498 -0.00700 AFIX 43 H225 2 0.645637 0.422811 0.084024 11.00000 -1.20000 AFIX 0 C226 1 0.654672 0.558376 0.114073 11.00000 0.02212 0.02211 = 0.02312 -0.00647 -0.00228 -0.00370 AFIX 43 H226 2 0.557199 0.583274 0.118806 11.00000 -1.20000 AFIX 0 C231 1 0.815769 0.773232 0.196584 11.00000 0.01722 0.02151 = 0.02942 -0.01349 -0.00189 -0.00127 C232 1 0.886259 0.856281 0.152545 11.00000 0.01909 0.02865 = 0.03551 -0.01273 0.00055 -0.00373 AFIX 43 H232 2 0.866058 0.893259 0.100241 11.00000 -1.20000 AFIX 0 C233 1 0.986189 0.884592 0.185636 11.00000 0.02147 0.03128 = 0.05419 -0.01976 0.00271 -0.00935 AFIX 43 H233 2 1.035086 0.940796 0.155918 11.00000 -1.20000 AFIX 0 C234 1 1.014455 0.830985 0.261787 11.00000 0.02394 0.04159 = 0.05645 -0.02722 -0.01321 -0.00345 AFIX 43 H234 2 1.080934 0.852388 0.284439 11.00000 -1.20000 AFIX 0 C235 1 0.947821 0.747069 0.305342 11.00000 0.03268 0.03956 = 0.03841 -0.01009 -0.01713 -0.00386 AFIX 43 H235 2 0.969840 0.709487 0.357376 11.00000 -1.20000 AFIX 0 C236 1 0.848005 0.717601 0.272709 11.00000 0.02660 0.03073 = 0.03165 -0.00825 -0.00869 -0.00359 AFIX 43 H236 2 0.801847 0.659493 0.302400 11.00000 -1.20000 AFIX 0 C241 1 0.548039 0.710609 0.229412 11.00000 0.01669 0.02706 = 0.01759 -0.00863 -0.00522 -0.00286 C242 1 0.463748 0.802401 0.247324 11.00000 0.02059 0.02627 = 0.02723 -0.00930 -0.00452 -0.00268 AFIX 43 H242 2 0.474472 0.877327 0.220160 11.00000 -1.20000 AFIX 0 C243 1 0.365059 0.782884 0.304786 11.00000 0.02069 0.04518 = 0.02752 -0.02154 -0.00069 0.00052 AFIX 43 H243 2 0.309094 0.844834 0.317675 11.00000 -1.20000 AFIX 0 C244 1 0.346441 0.674738 0.343804 11.00000 0.02279 0.05040 = 0.01923 -0.01388 0.00363 -0.01171 AFIX 43 H244 2 0.276216 0.662646 0.382175 11.00000 -1.20000 AFIX 0 C245 1 0.430084 0.584593 0.326839 11.00000 0.02763 0.03894 = 0.01999 -0.00318 -0.00163 -0.01051 AFIX 43 H245 2 0.418634 0.509965 0.354338 11.00000 -1.20000 AFIX 0 C246 1 0.531438 0.601815 0.269673 11.00000 0.02331 0.02445 = 0.02235 -0.00788 -0.00148 -0.00470 AFIX 43 H246 2 0.589039 0.539144 0.258312 11.00000 -1.20000 AFIX 0 S1 5 0.095660 0.163568 0.063074 11.00000 0.02229 0.03741 = 0.03808 -0.01117 -0.00130 -0.00109 C11 1 0.180259 0.106707 0.143961 11.00000 0.03103 0.02166 = 0.03537 -0.01196 0.00852 -0.01022 N11 3 0.240396 0.065987 0.200138 11.00000 0.05972 0.03975 = 0.03199 -0.00932 -0.00242 -0.01552 S2 5 0.149731 0.594456 0.647511 11.00000 0.03741 0.03453 = 0.05205 -0.00005 -0.00215 0.00138 C21 1 0.128287 0.632031 0.554900 11.00000 0.02641 0.02873 = 0.05665 -0.01804 0.00824 -0.00690 N21 3 0.108795 0.661248 0.489361 11.00000 0.04711 0.04443 = 0.05467 -0.02201 0.01575 -0.01551 HKLF 4 REM 090604j in P-1, C25 H22 P, S C N REM wR2 = 0.1434, GooF = S = 1.002, Restrained GooF = 1.002 for all data REM R1 = 0.0625 for 5838 Fo > 4sig(Fo) and 0.1054 for all 8913 data REM 523 parameters refined using 0 restraints END WGHT 0.0606 0.4922 REM Highest difference peak 1.287, deepest hole -0.541, 1-sigma level 0.069 Q1 1 0.1725 0.6347 0.6873 11.00000 0.05 1.29 Q2 1 0.3285 0.2753 0.3184 11.00000 0.05 0.55 Q3 1 0.2782 0.1411 0.3823 11.00000 0.05 0.48 Q4 1 0.0611 0.5184 0.6088 11.00000 0.05 0.38 Q5 1 0.3227 0.2321 0.4028 11.00000 0.05 0.36 Q6 1 0.4191 0.1798 0.3365 11.00000 0.05 0.36 Q7 1 0.5951 0.7304 0.1898 11.00000 0.05 0.35 Q8 1 0.0829 0.6283 0.4460 11.00000 0.05 0.34 Q9 1 0.6036 0.8060 0.1196 11.00000 0.05 0.34 Q10 1 0.1238 0.5629 0.5975 11.00000 0.05 0.33 Q11 1 0.2379 0.1042 0.4643 11.00000 0.05 0.31 Q12 1 0.6211 0.6891 0.1909 11.00000 0.05 0.31 Q13 1 0.7628 0.7838 0.1547 11.00000 0.05 0.30 Q14 1 0.1587 0.2035 0.0227 11.00000 0.05 0.29 Q15 1 0.5964 0.5814 0.1204 11.00000 0.05 0.29 Q16 1 0.8225 0.8400 0.1721 11.00000 0.05 0.29 Q17 1 0.1625 0.2806 0.4656 11.00000 0.05 0.28 Q18 1 0.4227 0.2226 0.4646 11.00000 0.05 0.28 Q19 1 0.6877 0.7991 0.1040 11.00000 0.05 0.28 Q20 1 0.5394 0.7482 0.2580 11.00000 0.05 0.27 ; _shelx_res_checksum 49160 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 P1 P 0.32908(8) 0.19761(7) 0.36079(5) 0.0243(2) Uani 1 1 d . . . . . C1 C 0.1976(3) 0.2726(3) 0.28960(17) 0.0252(7) Uani 1 1 d . . . . . H1A H 0.179077 0.219439 0.265759 0.030 Uiso 1 1 calc R U . . . H1B H 0.110521 0.298927 0.314949 0.030 Uiso 1 1 calc R U . . . C111 C 0.2368(3) 0.3734(3) 0.22798(17) 0.0247(7) Uani 1 1 d . . . . . C112 C 0.3026(3) 0.3584(3) 0.16237(17) 0.0265(7) Uani 1 1 d . . . . . H112 H 0.326901 0.285013 0.157841 0.032 Uiso 1 1 calc R U . . . C113 C 0.3329(3) 0.4500(3) 0.10347(19) 0.0332(9) Uani 1 1 d . . . . . H113 H 0.377688 0.439368 0.058533 0.040 Uiso 1 1 calc R U . . . C114 C 0.2984(3) 0.5570(3) 0.1097(2) 0.0353(9) Uani 1 1 d . . . . . H114 H 0.318808 0.619759 0.068964 0.042 Uiso 1 1 calc R U . . . C115 C 0.2344(3) 0.5729(3) 0.1752(2) 0.0330(8) Uani 1 1 d . . . . . H115 H 0.212119 0.646262 0.179816 0.040 Uiso 1 1 calc R U . . . C116 C 0.2027(3) 0.4813(3) 0.23415(19) 0.0292(8) Uani 1 1 d . . . . . H116 H 0.157457 0.492309 0.278905 0.035 Uiso 1 1 calc R U . . . C121 C 0.3497(3) 0.2811(3) 0.41724(17) 0.0255(7) Uani 1 1 d . . . . . C122 C 0.2310(3) 0.3443(3) 0.44064(18) 0.0293(8) Uani 1 1 d . . . . . H122 H 0.142971 0.350150 0.421513 0.035 Uiso 1 1 calc R U . . . C123 C 0.2412(4) 0.3983(3) 0.49155(19) 0.0345(8) Uani 1 1 d . . . . . H123 H 0.160251 0.441310 0.507586 0.041 Uiso 1 1 calc R U . . . C124 C 0.3700(4) 0.3898(3) 0.5194(2) 0.0359(9) Uani 1 1 d . . . . . H124 H 0.376921 0.427781 0.554085 0.043 Uiso 1 1 calc R U . . . C125 C 0.4881(4) 0.3263(3) 0.49693(19) 0.0347(9) Uani 1 1 d . . . . . H125 H 0.575749 0.320695 0.516318 0.042 Uiso 1 1 calc R U . . . C126 C 0.4792(3) 0.2711(3) 0.44654(18) 0.0297(8) Uani 1 1 d . . . . . H126 H 0.560208 0.226505 0.431756 0.036 Uiso 1 1 calc R U . . . C131 C 0.2669(3) 0.0767(3) 0.42249(18) 0.0267(7) Uani 1 1 d . . . . . C132 C 0.2692(3) 0.0521(3) 0.50116(19) 0.0326(8) Uani 1 1 d . . . . . H132 H 0.309198 0.095847 0.521956 0.039 Uiso 1 1 calc R U . . . C133 C 0.2124(3) -0.0366(3) 0.5483(2) 0.0343(9) Uani 1 1 d . . . . . H133 H 0.212596 -0.053295 0.601777 0.041 Uiso 1 1 calc R U . . . C134 C 0.1560(3) -0.1008(3) 0.51877(19) 0.0317(8) Uani 1 1 d . . . . . H134 H 0.118457 -0.161906 0.552114 0.038 Uiso 1 1 calc R U . . . C135 C 0.1527(3) -0.0779(3) 0.44078(19) 0.0319(8) Uani 1 1 d . . . . . H135 H 0.113514 -0.122944 0.420792 0.038 Uiso 1 1 calc R U . . . C136 C 0.2078(3) 0.0121(3) 0.39232(19) 0.0305(8) Uani 1 1 d . . . . . H136 H 0.205209 0.029496 0.338862 0.037 Uiso 1 1 calc R U . . . C141 C 0.4925(3) 0.1586(3) 0.31588(17) 0.0242(7) Uani 1 1 d . . . . . C142 C 0.5388(3) 0.0501(3) 0.31244(19) 0.0325(8) Uani 1 1 d . . . . . H142 H 0.484310 -0.005356 0.334057 0.039 Uiso 1 1 calc R U . . . C143 C 0.6658(3) 0.0230(3) 0.2771(2) 0.0373(9) Uani 1 1 d . . . . . H143 H 0.697303 -0.050849 0.273911 0.045 Uiso 1 1 calc R U . . . C144 C 0.7462(3) 0.1032(3) 0.24662(18) 0.0329(8) Uani 1 1 d . . . . . H144 H 0.833160 0.083775 0.223054 0.039 Uiso 1 1 calc R U . . . C145 C 0.7012(3) 0.2105(3) 0.25018(17) 0.0317(8) Uani 1 1 d . . . . . H145 H 0.757488 0.264851 0.229625 0.038 Uiso 1 1 calc R U . . . C146 C 0.5741(3) 0.2396(3) 0.28364(17) 0.0290(8) Uani 1 1 d . . . . . H146 H 0.541926 0.314505 0.284793 0.035 Uiso 1 1 calc R U . . . P2 P 0.67978(7) 0.73892(7) 0.15750(4) 0.01885(19) Uani 1 1 d . . . . . C2 C 0.6113(3) 0.8610(2) 0.07741(16) 0.0212(7) Uani 1 1 d . . . . . H2A H 0.578677 0.926805 0.095402 0.025 Uiso 1 1 calc R U . . . H2B H 0.687843 0.877968 0.040149 0.025 Uiso 1 1 calc R U . . . C211 C 0.4926(3) 0.8484(2) 0.03698(16) 0.0193(7) Uani 1 1 d . . . . . C212 C 0.3552(3) 0.8799(3) 0.05874(17) 0.0242(7) Uani 1 1 d . . . . . H212 H 0.334019 0.905473 0.101356 0.029 Uiso 1 1 calc R U . . . C213 C 0.2481(3) 0.8737(3) 0.01731(17) 0.0249(7) Uani 1 1 d . . . . . H213 H 0.154091 0.894506 0.032197 0.030 Uiso 1 1 calc R U . . . C214 C 0.2787(3) 0.8375(3) -0.04499(18) 0.0256(7) Uani 1 1 d . . . . . H214 H 0.205691 0.834272 -0.073178 0.031 Uiso 1 1 calc R U . . . C215 C 0.4157(3) 0.8060(3) -0.06650(17) 0.0251(7) Uani 1 1 d . . . . . H215 H 0.436527 0.780699 -0.109235 0.030 Uiso 1 1 calc R U . . . C216 C 0.5225(3) 0.8114(2) -0.02554(17) 0.0221(7) Uani 1 1 d . . . . . H216 H 0.616371 0.789632 -0.040358 0.027 Uiso 1 1 calc R U . . . C221 C 0.7455(3) 0.6172(2) 0.12873(16) 0.0187(7) Uani 1 1 d . . . . . C222 C 0.8879(3) 0.5819(3) 0.11974(17) 0.0258(7) Uani 1 1 d . . . . . H222 H 0.949974 0.622324 0.128920 0.031 Uiso 1 1 calc R U . . . C223 C 0.9392(3) 0.4878(3) 0.09738(19) 0.0310(8) Uani 1 1 d . . . . . H223 H 1.036505 0.463678 0.091381 0.037 Uiso 1 1 calc R U . . . C224 C 0.8496(3) 0.4291(3) 0.08380(17) 0.0283(8) Uani 1 1 d . . . . . H224 H 0.885221 0.364652 0.068370 0.034 Uiso 1 1 calc R U . . . C225 C 0.7071(3) 0.4641(3) 0.09271(17) 0.0260(7) Uani 1 1 d . . . . . H225 H 0.645637 0.422811 0.084024 0.031 Uiso 1 1 calc R U . . . C226 C 0.6547(3) 0.5584(3) 0.11407(17) 0.0227(7) Uani 1 1 d . . . . . H226 H 0.557199 0.583274 0.118806 0.027 Uiso 1 1 calc R U . . . C231 C 0.8158(3) 0.7732(3) 0.19658(17) 0.0217(7) Uani 1 1 d . . . . . C232 C 0.8863(3) 0.8563(3) 0.15255(19) 0.0275(8) Uani 1 1 d . . . . . H232 H 0.866058 0.893259 0.100241 0.033 Uiso 1 1 calc R U . . . C233 C 0.9862(3) 0.8846(3) 0.1856(2) 0.0337(8) Uani 1 1 d . . . . . H233 H 1.035086 0.940796 0.155918 0.040 Uiso 1 1 calc R U . . . C234 C 1.0145(3) 0.8310(3) 0.2618(2) 0.0375(9) Uani 1 1 d . . . . . H234 H 1.080934 0.852388 0.284439 0.045 Uiso 1 1 calc R U . . . C235 C 0.9478(3) 0.7471(3) 0.3053(2) 0.0371(9) Uani 1 1 d . . . . . H235 H 0.969840 0.709487 0.357376 0.045 Uiso 1 1 calc R U . . . C236 C 0.8480(3) 0.7176(3) 0.27271(19) 0.0300(8) Uani 1 1 d . . . . . H236 H 0.801847 0.659493 0.302400 0.036 Uiso 1 1 calc R U . . . C241 C 0.5480(3) 0.7106(3) 0.22941(16) 0.0201(7) Uani 1 1 d . . . . . C242 C 0.4637(3) 0.8024(3) 0.24732(18) 0.0247(7) Uani 1 1 d . . . . . H242 H 0.474472 0.877327 0.220160 0.030 Uiso 1 1 calc R U . . . C243 C 0.3651(3) 0.7829(3) 0.30479(18) 0.0299(8) Uani 1 1 d . . . . . H243 H 0.309094 0.844834 0.317675 0.036 Uiso 1 1 calc R U . . . C244 C 0.3464(3) 0.6747(3) 0.34380(18) 0.0297(8) Uani 1 1 d . . . . . H244 H 0.276216 0.662646 0.382175 0.036 Uiso 1 1 calc R U . . . C245 C 0.4301(3) 0.5846(3) 0.32684(17) 0.0299(8) Uani 1 1 d . . . . . H245 H 0.418634 0.509965 0.354338 0.036 Uiso 1 1 calc R U . . . C246 C 0.5314(3) 0.6018(3) 0.26967(17) 0.0233(7) Uani 1 1 d . . . . . H246 H 0.589039 0.539144 0.258312 0.028 Uiso 1 1 calc R U . . . S1 S 0.09566(8) 0.16357(8) 0.06307(5) 0.0337(2) Uani 1 1 d . . . . . C11 C 0.1803(3) 0.1067(3) 0.1440(2) 0.0285(8) Uani 1 1 d . . . . . N11 N 0.2404(3) 0.0660(3) 0.20014(18) 0.0435(8) Uani 1 1 d . . . . . S2 S 0.14973(10) 0.59446(8) 0.64751(6) 0.0464(3) Uani 1 1 d . . . . . C21 C 0.1283(3) 0.6320(3) 0.5549(2) 0.0366(9) Uani 1 1 d . . . . . N21 N 0.1088(3) 0.6612(3) 0.4894(2) 0.0474(9) 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 P1 0.0244(4) 0.0237(4) 0.0226(4) -0.0075(4) -0.0022(3) -0.0004(3) C1 0.0218(16) 0.0283(18) 0.0237(17) -0.0084(14) -0.0039(13) -0.0003(13) C111 0.0196(15) 0.0271(18) 0.0219(16) -0.0021(14) -0.0071(12) -0.0005(13) C112 0.0221(16) 0.0283(18) 0.0268(18) -0.0079(14) -0.0062(13) 0.0000(13) C113 0.0225(17) 0.043(2) 0.0237(18) 0.0007(16) -0.0040(13) -0.0038(15) C114 0.0268(18) 0.035(2) 0.033(2) 0.0077(16) -0.0090(15) -0.0102(15) C115 0.0267(18) 0.0258(18) 0.043(2) -0.0027(16) -0.0146(15) -0.0063(14) C116 0.0265(17) 0.0284(19) 0.0300(18) -0.0079(15) -0.0062(14) -0.0008(14) C121 0.0273(17) 0.0271(18) 0.0236(17) -0.0107(14) -0.0017(13) -0.0044(14) C122 0.0249(17) 0.0341(19) 0.0284(18) -0.0113(15) -0.0009(14) -0.0034(14) C123 0.0345(19) 0.038(2) 0.034(2) -0.0190(17) 0.0051(15) -0.0068(16) C124 0.045(2) 0.040(2) 0.0290(19) -0.0183(16) 0.0033(16) -0.0119(17) C125 0.0341(19) 0.044(2) 0.0274(18) -0.0125(16) -0.0066(15) -0.0077(16) C126 0.0254(17) 0.036(2) 0.0256(18) -0.0111(15) -0.0038(14) 0.0004(14) C131 0.0284(17) 0.0229(17) 0.0240(17) -0.0043(14) -0.0003(13) -0.0009(14) C132 0.0333(19) 0.0302(19) 0.0292(19) -0.0043(15) -0.0059(15) -0.0029(15) C133 0.0359(19) 0.034(2) 0.0252(18) -0.0015(16) -0.0036(15) -0.0034(16) C134 0.0321(18) 0.0219(17) 0.0295(19) -0.0003(15) 0.0057(15) 0.0019(14) C135 0.0343(19) 0.0262(18) 0.034(2) -0.0095(15) 0.0032(15) -0.0057(15) C136 0.0376(19) 0.0264(18) 0.0240(18) -0.0063(15) 0.0030(14) -0.0039(15) C141 0.0232(16) 0.0297(18) 0.0197(16) -0.0120(14) -0.0071(13) 0.0036(14) C142 0.0296(18) 0.036(2) 0.037(2) -0.0194(16) -0.0060(15) -0.0033(15) C143 0.0320(19) 0.037(2) 0.049(2) -0.0284(18) -0.0062(16) 0.0045(16) C144 0.0295(18) 0.048(2) 0.0237(18) -0.0164(16) -0.0033(14) -0.0045(16) C145 0.0315(18) 0.036(2) 0.0196(17) -0.0005(15) -0.0006(14) -0.0040(15) C146 0.0316(18) 0.0283(18) 0.0199(17) -0.0018(14) -0.0026(14) -0.0007(15) P2 0.0155(4) 0.0195(4) 0.0213(4) -0.0065(3) -0.0017(3) -0.0029(3) C2 0.0215(15) 0.0197(16) 0.0207(16) -0.0041(13) -0.0020(12) -0.0045(12) C211 0.0198(15) 0.0144(15) 0.0199(15) 0.0001(12) -0.0033(12) -0.0036(12) C212 0.0228(16) 0.0244(17) 0.0213(16) -0.0062(13) -0.0007(13) 0.0011(13) C213 0.0156(15) 0.0271(17) 0.0272(18) -0.0062(14) 0.0016(13) -0.0002(13) C214 0.0212(16) 0.0258(17) 0.0261(17) -0.0021(14) -0.0078(13) -0.0047(13) C215 0.0284(17) 0.0253(17) 0.0208(16) -0.0081(14) -0.0018(13) -0.0024(14) C216 0.0175(15) 0.0218(16) 0.0246(17) -0.0050(13) -0.0005(12) -0.0031(12) C221 0.0187(15) 0.0180(15) 0.0160(15) -0.0018(12) -0.0014(11) -0.0025(12) C222 0.0216(16) 0.0296(18) 0.0267(17) -0.0093(14) -0.0038(13) -0.0048(14) C223 0.0213(16) 0.036(2) 0.0319(19) -0.0120(16) -0.0039(14) 0.0042(15) C224 0.0354(19) 0.0214(17) 0.0239(17) -0.0085(14) -0.0016(14) 0.0049(14) C225 0.0363(19) 0.0214(17) 0.0216(17) -0.0069(13) -0.0050(14) -0.0070(14) C226 0.0221(16) 0.0221(16) 0.0231(17) -0.0065(13) -0.0023(13) -0.0037(13) C231 0.0172(15) 0.0215(16) 0.0294(17) -0.0135(14) -0.0019(13) -0.0013(12) C232 0.0191(16) 0.0287(18) 0.0355(19) -0.0127(15) 0.0005(14) -0.0037(13) C233 0.0215(17) 0.0313(19) 0.054(2) -0.0198(18) 0.0027(16) -0.0093(14) C234 0.0239(18) 0.042(2) 0.056(2) -0.0272(19) -0.0132(16) -0.0035(16) C235 0.0327(19) 0.040(2) 0.038(2) -0.0101(17) -0.0171(16) -0.0039(16) C236 0.0266(17) 0.0307(19) 0.0317(19) -0.0083(15) -0.0087(14) -0.0036(14) C241 0.0167(15) 0.0271(17) 0.0176(15) -0.0086(13) -0.0052(12) -0.0029(13) C242 0.0206(16) 0.0263(17) 0.0272(17) -0.0093(14) -0.0045(13) -0.0027(13) C243 0.0207(16) 0.045(2) 0.0275(18) -0.0215(16) -0.0007(13) 0.0005(15) C244 0.0228(17) 0.050(2) 0.0192(17) -0.0139(16) 0.0036(13) -0.0117(15) C245 0.0276(17) 0.039(2) 0.0200(17) -0.0032(15) -0.0016(13) -0.0105(15) C246 0.0233(16) 0.0244(17) 0.0223(17) -0.0079(14) -0.0015(13) -0.0047(13) S1 0.0223(4) 0.0374(5) 0.0381(5) -0.0112(4) -0.0013(4) -0.0011(4) C11 0.0310(18) 0.0217(17) 0.035(2) -0.0120(15) 0.0085(15) -0.0102(14) N11 0.060(2) 0.0397(19) 0.0320(18) -0.0093(15) -0.0024(15) -0.0155(16) S2 0.0374(5) 0.0345(5) 0.0521(6) 0.0000(5) -0.0021(4) 0.0014(4) C21 0.0264(18) 0.029(2) 0.057(3) -0.0180(19) 0.0082(17) -0.0069(15) N21 0.047(2) 0.044(2) 0.055(2) -0.0220(18) 0.0157(17) -0.0155(16) 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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 0 1 0.0263 -0.0000 -0.0000 1.0000 0.0214 0.0327 0.0096 0 0 -1 0.0185 0.0000 0.0000 -1.0000 -0.0214 -0.0327 -0.0096 -1 -1 0 0.1093 -1.0000 -1.0000 0.0000 -0.0013 0.0019 0.0846 1 1 0 0.0969 1.0000 1.0000 -0.0000 0.0013 -0.0019 -0.0846 0 -1 0 0.0572 -0.0000 -1.0000 0.0000 0.0475 -0.0165 0.0326 -1 0 0 0.1295 -1.0000 -0.0000 -0.0000 -0.0488 0.0184 0.0520 1 0 0 0.1230 1.0000 0.0000 0.0000 0.0488 -0.0184 -0.0520 0 1 1 0.0284 -0.0000 1.0000 1.0000 -0.0261 0.0492 -0.0231 0 -1 -1 0.0406 0.0000 -1.0000 -1.0000 0.0261 -0.0492 0.0231 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 C131 P1 C121 107.60(15) . . ? C131 P1 C141 112.23(15) . . ? C121 P1 C141 109.23(15) . . ? C131 P1 C1 106.03(15) . . ? C121 P1 C1 111.80(15) . . ? C141 P1 C1 109.93(14) . . ? C111 C1 P1 113.9(2) . . ? C111 C1 H1A 108.8 . . ? P1 C1 H1A 108.8 . . ? C111 C1 H1B 108.8 . . ? P1 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C112 C111 C116 119.3(3) . . ? C112 C111 C1 119.0(3) . . ? C116 C111 C1 121.6(3) . . ? C113 C112 C111 120.2(3) . . ? C113 C112 H112 119.9 . . ? C111 C112 H112 119.9 . . ? C114 C113 C112 120.2(3) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C115 C114 C113 120.1(3) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C114 C115 C116 119.8(3) . . ? C114 C115 H115 120.1 . . ? C116 C115 H115 120.1 . . ? C115 C116 C111 120.3(3) . . ? C115 C116 H116 119.9 . . ? C111 C116 H116 119.9 . . ? C122 C121 C126 119.9(3) . . ? C122 C121 P1 118.3(2) . . ? C126 C121 P1 121.2(2) . . ? C123 C122 C121 120.0(3) . . ? C123 C122 H122 120.0 . . ? C121 C122 H122 120.0 . . ? C122 C123 C124 120.0(3) . . ? C122 C123 H123 120.0 . . ? C124 C123 H123 120.0 . . ? C125 C124 C123 120.3(4) . . ? C125 C124 H124 119.9 . . ? C123 C124 H124 119.9 . . ? C126 C125 C124 120.3(3) . . ? C126 C125 H125 119.8 . . ? C124 C125 H125 119.8 . . ? C125 C126 C121 119.5(3) . . ? C125 C126 H126 120.2 . . ? C121 C126 H126 120.2 . . ? C136 C131 C132 120.1(3) . . ? C136 C131 P1 120.3(2) . . ? C132 C131 P1 119.4(3) . . ? C133 C132 C131 119.1(4) . . ? C133 C132 H132 120.4 . . ? C131 C132 H132 120.4 . . ? C134 C133 C132 120.8(3) . . ? C134 C133 H133 119.6 . . ? C132 C133 H133 119.6 . . ? C133 C134 C135 121.1(3) . . ? C133 C134 H134 119.5 . . ? C135 C134 H134 119.5 . . ? C134 C135 C136 119.0(4) . . ? C134 C135 H135 120.5 . . ? C136 C135 H135 120.5 . . ? C135 C136 C131 119.9(3) . . ? C135 C136 H136 120.0 . . ? C131 C136 H136 120.0 . . ? C142 C141 C146 119.6(3) . . ? C142 C141 P1 121.1(3) . . ? C146 C141 P1 119.3(2) . . ? C141 C142 C143 119.5(3) . . ? C141 C142 H142 120.2 . . ? C143 C142 H142 120.2 . . ? C144 C143 C142 120.3(3) . . ? C144 C143 H143 119.9 . . ? C142 C143 H143 119.9 . . ? C145 C144 C143 120.4(3) . . ? C145 C144 H144 119.8 . . ? C143 C144 H144 119.8 . . ? C144 C145 C146 120.1(3) . . ? C144 C145 H145 120.0 . . ? C146 C145 H145 120.0 . . ? C145 C146 C141 120.1(3) . . ? C145 C146 H146 120.0 . . ? C141 C146 H146 120.0 . . ? C241 P2 C221 109.89(14) . . ? C241 P2 C231 107.83(14) . . ? C221 P2 C231 110.37(13) . . ? C241 P2 C2 110.21(13) . . ? C221 P2 C2 111.05(14) . . ? C231 P2 C2 107.42(14) . . ? C211 C2 P2 115.2(2) . . ? C211 C2 H2A 108.5 . . ? P2 C2 H2A 108.5 . . ? C211 C2 H2B 108.5 . . ? P2 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C216 C211 C212 119.8(3) . . ? C216 C211 C2 119.1(3) . . ? C212 C211 C2 121.0(3) . . ? C211 C212 C213 119.5(3) . . ? C211 C212 H212 120.2 . . ? C213 C212 H212 120.2 . . ? C214 C213 C212 120.3(3) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C213 C214 C215 120.1(3) . . ? C213 C214 H214 119.9 . . ? C215 C214 H214 119.9 . . ? C214 C215 C216 120.0(3) . . ? C214 C215 H215 120.0 . . ? C216 C215 H215 120.0 . . ? C211 C216 C215 120.3(3) . . ? C211 C216 H216 119.9 . . ? C215 C216 H216 119.9 . . ? C222 C221 C226 119.8(3) . . ? C222 C221 P2 119.7(2) . . ? C226 C221 P2 120.5(2) . . ? C223 C222 C221 119.9(3) . . ? C223 C222 H222 120.0 . . ? C221 C222 H222 120.0 . . ? C224 C223 C222 120.3(3) . . ? C224 C223 H223 119.9 . . ? C222 C223 H223 119.9 . . ? C223 C224 C225 120.0(3) . . ? C223 C224 H224 120.0 . . ? C225 C224 H224 120.0 . . ? C226 C225 C224 120.3(3) . . ? C226 C225 H225 119.8 . . ? C224 C225 H225 119.8 . . ? C225 C226 C221 119.7(3) . . ? C225 C226 H226 120.1 . . ? C221 C226 H226 120.1 . . ? C236 C231 C232 120.0(3) . . ? C236 C231 P2 118.9(2) . . ? C232 C231 P2 121.1(2) . . ? C233 C232 C231 119.5(3) . . ? C233 C232 H232 120.2 . . ? C231 C232 H232 120.2 . . ? C234 C233 C232 119.9(3) . . ? C234 C233 H233 120.0 . . ? C232 C233 H233 120.0 . . ? C235 C234 C233 121.0(3) . . ? C235 C234 H234 119.5 . . ? C233 C234 H234 119.5 . . ? C234 C235 C236 119.6(3) . . ? C234 C235 H235 120.2 . . ? C236 C235 H235 120.2 . . ? C235 C236 C231 120.0(3) . . ? C235 C236 H236 120.0 . . ? C231 C236 H236 120.0 . . ? C246 C241 C242 119.6(3) . . ? C246 C241 P2 122.3(2) . . ? C242 C241 P2 118.0(2) . . ? C243 C242 C241 119.4(3) . . ? C243 C242 H242 120.3 . . ? C241 C242 H242 120.3 . . ? C242 C243 C244 121.0(3) . . ? C242 C243 H243 119.5 . . ? C244 C243 H243 119.5 . . ? C245 C244 C243 119.6(3) . . ? C245 C244 H244 120.2 . . ? C243 C244 H244 120.2 . . ? C244 C245 C246 120.5(3) . . ? C244 C245 H245 119.7 . . ? C246 C245 H245 119.7 . . ? C241 C246 C245 119.8(3) . . ? C241 C246 H246 120.1 . . ? C245 C246 H246 120.1 . . ? N11 C11 S1 179.2(3) . . ? N21 C21 S2 177.7(3) . . ? 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 P1 C131 1.793(3) . ? P1 C121 1.794(3) . ? P1 C141 1.797(3) . ? P1 C1 1.811(3) . ? C1 C111 1.514(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C111 C112 1.386(4) . ? C111 C116 1.393(5) . ? C112 C113 1.383(4) . ? C112 H112 0.9500 . ? C113 C114 1.382(5) . ? C113 H113 0.9500 . ? C114 C115 1.381(5) . ? C114 H114 0.9500 . ? C115 C116 1.388(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C121 C122 1.393(4) . ? C121 C126 1.403(4) . ? C122 C123 1.378(5) . ? C122 H122 0.9500 . ? C123 C124 1.389(5) . ? C123 H123 0.9500 . ? C124 C125 1.384(5) . ? C124 H124 0.9500 . ? C125 C126 1.378(5) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C131 C136 1.397(5) . ? C131 C132 1.399(4) . ? C132 C133 1.384(5) . ? C132 H132 0.9500 . ? C133 C134 1.369(5) . ? C133 H133 0.9500 . ? C134 C135 1.390(5) . ? C134 H134 0.9500 . ? C135 C136 1.394(4) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? C141 C142 1.387(5) . ? C141 C146 1.402(5) . ? C142 C143 1.391(5) . ? C142 H142 0.9500 . ? C143 C144 1.382(5) . ? C143 H143 0.9500 . ? C144 C145 1.372(5) . ? C144 H144 0.9500 . ? C145 C146 1.382(4) . ? C145 H145 0.9500 . ? C146 H146 0.9500 . ? P2 C241 1.788(3) . ? P2 C221 1.790(3) . ? P2 C231 1.793(3) . ? P2 C2 1.812(3) . ? C2 C211 1.522(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C211 C216 1.390(4) . ? C211 C212 1.391(4) . ? C212 C213 1.402(4) . ? C212 H212 0.9500 . ? C213 C214 1.380(5) . ? C213 H213 0.9500 . ? C214 C215 1.386(4) . ? C214 H214 0.9500 . ? C215 C216 1.390(4) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? C221 C222 1.391(4) . ? C221 C226 1.397(4) . ? C222 C223 1.385(5) . ? C222 H222 0.9500 . ? C223 C224 1.378(5) . ? C223 H223 0.9500 . ? C224 C225 1.391(4) . ? C224 H224 0.9500 . ? C225 C226 1.379(4) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C231 C236 1.391(4) . ? C231 C232 1.394(4) . ? C232 C233 1.388(5) . ? C232 H232 0.9500 . ? C233 C234 1.381(5) . ? C233 H233 0.9500 . ? C234 C235 1.375(5) . ? C234 H234 0.9500 . ? C235 C236 1.391(5) . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? C241 C246 1.385(4) . ? C241 C242 1.402(4) . ? C242 C243 1.380(4) . ? C242 H242 0.9500 . ? C243 C244 1.380(5) . ? C243 H243 0.9500 . ? C244 C245 1.375(5) . ? C244 H244 0.9500 . ? C245 C246 1.392(4) . ? C245 H245 0.9500 . ? C246 H246 0.9500 . ? S1 C11 1.654(4) . ? C11 N11 1.156(4) . ? S2 C21 1.655(4) . ? C21 N21 1.176(5) . ?