#------------------------------------------------------------------------------ #$Date: 2014-10-25 18:23:10 +0100 (Sat, 25 Oct 2014) $ #$Revision: 125873 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/53/2105306.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2105306 loop_ _publ_author_name 'St\"oger, Berthold' 'Kautny, Paul' 'Lumpi, Daniel' 'Zobetz, Erich' 'Fr\"ohlich, Johannes' _publ_section_title ; Solvatomorphism of 9,9'-[1,3,4-thiadiazole-2,5-diylbis(2,3-thiophendiyl-4,1-phenylene)]bis[9H-carbazole]: isostructurality, modularity and order--disorder theory ; _journal_issue 6 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 667 _journal_page_last 676 _journal_volume 68 _journal_year 2012 _chemical_formula_sum 'C52 H40 N4 O3 S3' _chemical_formula_weight 865.1 _chemical_name_systematic ' ?' _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 94.1313(18) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.5233(4) _cell_length_b 11.2845(4) _cell_length_c 29.4786(10) _cell_measurement_reflns_used 71107 _cell_measurement_temperature 100 _cell_measurement_theta_max 38.1 _cell_measurement_theta_min 2.7 _cell_volume 4155.1(2) _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _diffrn_measurement_device 'four-cycle diffractometer' _diffrn_measurement_device_type 'Bruker KAPPA APEX II CCD' _diffrn_measurement_method '\w and \p scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_number 217035 _diffrn_reflns_theta_full 38.47 _diffrn_reflns_theta_max 38.51 _diffrn_reflns_theta_min 1.39 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour 'clear yellow' _exptl_crystal_density_diffrn 1.3825 _exptl_crystal_description fragment _exptl_crystal_F_000 1808 _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.35 _refine_diff_density_max 0.67 _refine_diff_density_min -0.38 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 2.18 _refine_ls_hydrogen_treatment constr _refine_ls_number_constraints 160 _refine_ls_number_parameters 559 _refine_ls_number_reflns 22872 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0447 _refine_ls_shift/su_max 0.0406 _refine_ls_shift/su_mean 0.0019 _refine_ls_structure_factor_coef F 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0.000299 C3 0.000000 0.000071 0.000083 0.000028 0.000383 0.000422 0.000332 0.000320 0.000280 0.000289 C4 0.000000 0.000070 0.000081 0.000028 0.000371 0.000409 0.000337 0.000310 0.000279 0.000293 C5 0.000000 0.000077 0.000088 0.000031 0.000431 0.000442 0.000394 0.000346 0.000326 0.000328 C6 0.000000 0.000081 0.000091 0.000031 0.000471 0.000481 0.000388 0.000377 0.000337 0.000338 C7 0.000000 0.000070 0.000081 0.000029 0.000379 0.000398 0.000363 0.000310 0.000291 0.000299 C8 0.000000 0.000068 0.000081 0.000029 0.000356 0.000409 0.000368 0.000303 0.000284 0.000303 C9 0.000000 0.000074 0.000086 0.000033 0.000404 0.000448 0.000425 0.000337 0.000324 0.000340 C10 0.000000 0.000077 0.000089 0.000034 0.000432 0.000442 0.000479 0.000349 0.000360 0.000358 C11 0.000000 0.000071 0.000079 0.000028 0.000383 0.000399 0.000344 0.000309 0.000284 0.000287 C12 0.000000 0.000074 0.000086 0.000030 0.000402 0.000460 0.000356 0.000342 0.000299 0.000318 C13 0.000000 0.000074 0.000087 0.000030 0.000383 0.000478 0.000374 0.000335 0.000298 0.000323 C14 0.000000 0.000071 0.000083 0.000029 0.000388 0.000425 0.000348 0.000323 0.000288 0.000298 C15 0.000000 0.000073 0.000086 0.000030 0.000396 0.000460 0.000352 0.000341 0.000294 0.000316 C16 0.000000 0.000073 0.000086 0.000030 0.000377 0.000454 0.000363 0.000326 0.000292 0.000315 C17 0.000000 0.000068 0.000079 0.000028 0.000362 0.000408 0.000342 0.000301 0.000278 0.000290 C18 0.000000 0.000071 0.000086 0.000029 0.000370 0.000459 0.000354 0.000329 0.000286 0.000314 C19 0.000000 0.000073 0.000087 0.000029 0.000392 0.000465 0.000348 0.000343 0.000290 0.000315 C20 0.000000 0.000071 0.000082 0.000028 0.000380 0.000420 0.000342 0.000320 0.000283 0.000299 C21 0.000000 0.000072 0.000085 0.000029 0.000374 0.000438 0.000364 0.000324 0.000288 0.000311 C22 0.000000 0.000070 0.000084 0.000029 0.000368 0.000436 0.000351 0.000323 0.000285 0.000307 C23 0.000000 0.000071 0.000083 0.000028 0.000386 0.000423 0.000335 0.000323 0.000283 0.000294 C24 0.000000 0.000077 0.000087 0.000031 0.000422 0.000450 0.000374 0.000347 0.000314 0.000319 C25 0.000000 0.000079 0.000089 0.000032 0.000457 0.000461 0.000401 0.000362 0.000336 0.000335 C26 0.000000 0.000081 0.000089 0.000031 0.000485 0.000460 0.000390 0.000372 0.000340 0.000329 C27 0.000000 0.000080 0.000088 0.000030 0.000450 0.000464 0.000376 0.000361 0.000326 0.000321 C28 0.000000 0.000071 0.000083 0.000028 0.000384 0.000423 0.000344 0.000325 0.000287 0.000301 C29 0.000000 0.000070 0.000084 0.000029 0.000381 0.000430 0.000350 0.000324 0.000288 0.000304 C30 0.000000 0.000075 0.000092 0.000032 0.000415 0.000498 0.000400 0.000355 0.000322 0.000345 C31 0.000000 0.000078 0.000094 0.000034 0.000420 0.000499 0.000452 0.000366 0.000343 0.000369 C32 0.000000 0.000078 0.000092 0.000034 0.000430 0.000480 0.000447 0.000362 0.000345 0.000359 C33 0.000000 0.000075 0.000089 0.000032 0.000410 0.000450 0.000399 0.000344 0.000319 0.000332 C34 0.000000 0.000071 0.000082 0.000029 0.000370 0.000421 0.000357 0.000316 0.000285 0.000302 C35 0.000000 0.000070 0.000087 0.000028 0.000381 0.000464 0.000345 0.000334 0.000288 0.000311 C36 0.000000 0.000075 0.000092 0.000031 0.000422 0.000484 0.000392 0.000360 0.000320 0.000342 C37 0.000000 0.000079 0.000098 0.000032 0.000443 0.000531 0.000414 0.000387 0.000338 0.000365 C38 0.000000 0.000083 0.000102 0.000033 0.000447 0.000602 0.000413 0.000413 0.000340 0.000387 C39 0.000000 0.000079 0.000101 0.000031 0.000458 0.000579 0.000389 0.000408 0.000331 0.000368 C40 0.000000 0.000073 0.000088 0.000029 0.000402 0.000477 0.000342 0.000349 0.000292 0.000318 C41 0.000000 0.000075 0.000089 0.000029 0.000413 0.000469 0.000354 0.000350 0.000303 0.000315 C42 0.000000 0.000085 0.000096 0.000032 0.000492 0.000527 0.000408 0.000406 0.000352 0.000361 C43 0.000000 0.000086 0.000099 0.000034 0.000531 0.000531 0.000448 0.000413 0.000388 0.000377 C44 0.000000 0.000084 0.000096 0.000033 0.000475 0.000527 0.000443 0.000395 0.000365 0.000374 C45 0.000000 0.000078 0.000090 0.000031 0.000427 0.000488 0.000382 0.000362 0.000319 0.000336 C46 0.000000 0.000073 0.000084 0.000028 0.000402 0.000447 0.000340 0.000338 0.000291 0.000306 C47 0.000000 0.000100 0.000113 0.000040 0.000623 0.000699 0.000574 0.000517 0.000472 0.000489 C48 0.000000 0.000092 0.000105 0.000036 0.000581 0.000585 0.000492 0.000462 0.000422 0.000414 C49 0.000000 0.000085 0.000097 0.000035 0.000489 0.000549 0.000475 0.000410 0.000380 0.000395 C50 0.000000 0.000087 0.000099 0.000038 0.000526 0.000526 0.000559 0.000414 0.000428 0.000419 C51 0.000000 0.000111 0.000130 0.000041 0.000738 0.000842 0.000591 0.000604 0.000524 0.000534 C52 0.000000 0.000104 0.000130 0.000039 0.000699 0.000857 0.000533 0.000611 0.000482 0.000518 H5 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H6 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H9 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H10 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H12 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H13 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H15 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H16 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H18 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H19 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H21 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H22 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H24 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H25 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H26 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H27 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H30 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H31 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H32 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H33 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H36 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H37 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H38 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H39 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H42 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H43 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H44 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H45 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H471 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H472 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H481 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H482 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H491 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H492 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H501 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H502 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H511 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H512 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H521 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 H522 0.000000-0.100000-0.100000-0.100000 0.000000 0.000000 0.000000 0.000000 0.000000 0.000000 -------------------------- Saved points ---------------------------- 0 -------------------------- Fourier maxima -------------------------- 1 1 1 max1 1 1 1.000000 0.201112 0.053836 0.661643 000 0 0 0 0.48 0.77 max2 1 1 1.000000 0.479944 0.018085 0.213837 000 0 0 0 0.67 0.76 max3 1 1 1.000000 0.276208 0.011435 0.648218 000 0 0 0 0.53 0.74 max4 1 1 1.000000 0.090482 0.172267 0.135256 000 0 0 0 0.59 0.74 max5 1 1 1.000000 0.128519 0.107547 0.681543 000 0 0 0 0.65 0.74 max6 1 1 1.000000 0.367937 0.183973 0.230338 000 0 0 0 0.48 0.74 max7 1 1 1.000000 0.409060 0.079538 0.225803 000 0 0 0 0.42 0.73 max8 1 1 1.000000 0.329850 0.211080 0.918635 000 0 0 0 0.55 0.73 max9 1 1 1.000000 0.103968 0.051013 0.091644 000 0 0 0 0.42 0.72 max10 1 1 1.000000 0.952707 0.130133 0.179467 000 0 0 0 0.48 0.70 -------------------------- Fourier minima -------------------------- 1 1 1 min1 1 1 1.000000 0.578323 0.084960 0.696998 000 0 0 0 0.31 0.73 min2 1 1 1.000000 0.575389 0.033955 0.751830 000 0 0 0 0.23 0.72 min3 1 1 1.000000 0.599432 0.122551 0.686639 000 0 0 0 0.30 0.71 min4 1 1 1.000000 0.614042 0.019008 0.728618 000 0 0 0 0.26 0.70 min5 1 1 1.000000 0.639428 0.017295 0.677143 000 0 0 0 0.27 0.68 min6 1 1 1.000000 0.552072 0.154651 0.684001 000 0 0 0 0.31 0.68 min7 1 1 1.000000 0.620090 0.070040 0.749000 000 0 0 0 0.25 0.68 min8 1 1 1.000000 0.518713 0.087230 0.725321 000 0 0 0 0.24 0.66 min9 1 1 1.000000 0.426423 0.029381 0.236331 000 0 0 0 0.29 0.66 min10 1 1 1.000000 0.328780 0.248718 0.301283 000 0 0 0 0.28 0.66 ------------------------------------------------------------------------ Version Jana2006 title cell 12.5233 11.2845 29.4786 90 94.1313 90 esdcell 0.0004 0.0004 0.001 0 0.0018 0 spgroup P21/n 14 22 lattice P symmetry x y z symmetry -x+1/2 y+1/2 -z+1/2 symmetry -x -y -z symmetry x+1/2 -y+1/2 z+1/2 unitsnumb 4 chemform C52 H40 S3 N4 O3 formtab -62 atom C atradius 0.77 color 128073041 atom H atradius 0.46 color 255204204 atom S atradius 1.04 color 255250000 atom N atradius 0.74 color 176185230 atom O atradius 0.74 color 254003000 roundmethod 1 end ******************************************************************************* contour end contour dist angles 1 plane N1 N2 C1 C2 S1 plane S2 C3 C4 C5 C6 plane S3 C7 C8 C9 C10 plane C11 C12 C13 C14 C15 C16 plane C17 C18 C19 C20 C21 C22 plane N3 C23 C24 C25 C26 C27 C28 C29 C30 C31 C32 C33 C34 plane N4 C35 C36 C37 C38 C39 C40 C41 C42 C43 C44 C45 C46 end dist fourier maptype 6 intrad 1.6 end fourier refine keep hydro triang C5 2 1 C6 C4 0.96 H5 keep ADP riding C5 1.2 H5 keep hydro triang C6 2 1 C5 S2 0.96 H6 keep ADP riding C6 1.2 H6 keep hydro triang C9 2 1 C10 C8 0.96 H9 keep ADP riding C9 1.2 H9 keep hydro triang C10 2 1 C9 S3 0.96 H10 keep ADP riding C10 1.2 H10 keep hydro triang C12 2 1 C13 C11 0.96 H12 keep ADP riding C12 1.2 H12 keep hydro triang C13 2 1 C12 C14 0.96 H13 keep ADP riding C13 1.2 H13 keep hydro triang C15 2 1 C16 C14 0.96 H15 keep ADP riding C15 1.2 H15 keep hydro triang C16 2 1 C15 C11 0.96 H16 keep ADP riding C16 1.2 H16 keep hydro triang C18 2 1 C19 C17 0.96 H18 keep ADP riding C18 1.2 H18 keep hydro triang C19 2 1 C18 C20 0.96 H19 keep ADP riding C19 1.2 H19 keep hydro triang C21 2 1 C20 C22 0.96 H21 keep ADP riding C21 1.2 H21 keep hydro triang C22 2 1 C21 C17 0.96 H22 keep ADP riding C22 1.2 H22 keep hydro triang C24 2 1 C25 C23 0.96 H24 keep ADP riding C24 1.2 H24 keep hydro triang C25 2 1 C24 C26 0.96 H25 keep ADP riding C25 1.2 H25 keep hydro triang C26 2 1 C27 C25 0.96 H26 keep ADP riding C26 1.2 H26 keep hydro triang C27 2 1 C26 C28 0.96 H27 keep ADP riding C27 1.2 H27 keep hydro triang C30 2 1 C31 C29 0.96 H30 keep ADP riding C30 1.2 H30 keep hydro triang C31 2 1 C30 C32 0.96 H31 keep ADP riding C31 1.2 H31 keep hydro triang C32 2 1 C33 C31 0.96 H32 keep ADP riding C32 1.2 H32 keep hydro triang C33 2 1 C32 C34 0.96 H33 keep ADP riding C33 1.2 H33 keep hydro triang C36 2 1 C35 C37 0.96 H36 keep ADP riding C36 1.2 H36 keep hydro triang C37 2 1 C36 C38 0.96 H37 keep ADP riding C37 1.2 H37 keep hydro triang C38 2 1 C39 C37 0.96 H38 keep ADP riding C38 1.2 H38 keep hydro triang C39 2 1 C38 C40 0.96 H39 keep ADP riding C39 1.2 H39 keep hydro triang C42 2 1 C43 C41 0.96 H42 keep ADP riding C42 1.2 H42 keep hydro triang C43 2 1 C42 C44 0.96 H43 keep ADP riding C43 1.2 H43 keep hydro triang C44 2 1 C45 C43 0.96 H44 keep ADP riding C44 1.2 H44 keep hydro triang C45 2 1 C44 C46 0.96 H45 keep ADP riding C45 1.2 H45 keep hydro tetrahed C47 2 2 O1 C48 0.96 H471 H472 keep ADP riding C47 1.2 H471 H472 keep hydro tetrahed C48 2 2 O2 C47 0.96 H481 H482 keep ADP riding C48 1.2 H481 H482 keep hydro tetrahed C49 2 2 O2 C50 0.96 H491 H492 keep ADP riding C49 1.2 H491 H492 keep hydro tetrahed C50 2 2 O1 C49 0.96 H501 H502 keep ADP riding C50 1.2 H501 H502 keep hydro tetrahed C51 2 2 O3#s3t1,2,0 C52 0.96 H511 H512 keep ADP riding C51 1.2 H511 H512 keep hydro tetrahed C52 2 2 O3 C51 0.96 H521 H522 keep ADP riding C52 1.2 H521 H522 end refine ; _[local]_cod_data_source_file ry5046.cif _[local]_cod_data_source_block sesqui_dioxane _[local]_cod_cif_authors_sg_Hall '-P 2yabc' _cod_database_code 2105306 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x+1/2,y+1/2,-z+1/2 3 -x,-y,-z 4 x+1/2,-y+1/2,z+1/2 loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_symmetry_multiplicity S S1 0.071228(18) 0.38171(2) 0.193584(7) 0.01462(6) Uani d 1 4 S S2 0.19283(2) 0.18363(2) 0.079699(7) 0.01877(6) Uani d 1 4 S S3 0.20013(2) 0.74328(2) 0.197056(8) 0.01946(6) Uani d 1 4 O O1 0.87362(7) 0.21246(8) -0.03078(3) 0.0331(3) Uani d 1 4 O O2 0.88214(6) 0.43335(7) 0.01476(2) 0.0243(2) Uani d 1 4 O O3 0.44727(7) 0.95285(9) 0.03680(3) 0.0368(3) Uani d 1 4 N N1 0.18968(8) 0.41127(8) 0.12729(3) 0.0257(3) Uani d 1 4 N N2 0.19485(8) 0.51543(8) 0.15078(3) 0.0252(3) Uani d 1 4 N N3 -0.18068(6) 0.04055(7) 0.29244(2) 0.0158(2) Uani d 1 4 N N4 -0.06984(6) 0.30122(7) 0.37971(3) 0.0158(2) Uani d 1 4 C C1 0.13005(7) 0.33169(8) 0.14576(3) 0.0155(2) Uani d 1 4 C C2 0.13874(7) 0.51391(8) 0.18668(3) 0.0154(2) Uani d 1 4 C C3 0.12269(7) 0.21286(8) 0.12697(3) 0.0145(2) Uani d 1 4 C C4 0.06953(7) 0.11446(8) 0.14109(3) 0.0140(2) Uani d 1 4 C C5 0.08553(8) 0.01502(9) 0.11250(3) 0.0181(2) Uani d 1 4 C C6 0.14990(8) 0.03967(9) 0.07825(3) 0.0202(3) Uani d 1 4 C C7 0.14368(7) 0.61518(8) 0.21709(3) 0.0145(2) Uani d 1 4 C C8 0.12119(7) 0.62590(8) 0.26210(3) 0.0143(2) Uani d 1 4 C C9 0.15069(7) 0.74018(9) 0.27975(3) 0.0183(2) Uani d 1 4 C C10 0.19214(8) 0.81199(9) 0.24825(3) 0.0206(3) Uani d 1 4 C C11 0.00488(7) 0.10783(8) 0.18142(3) 0.0139(2) Uani d 1 4 C C12 -0.10631(7) 0.11745(9) 0.17662(3) 0.0168(2) Uani d 1 4 C C13 -0.16799(7) 0.09775(9) 0.21317(3) 0.0169(2) Uani d 1 4 C C14 -0.11844(7) 0.06891(8) 0.25559(3) 0.0149(2) Uani d 1 4 C C15 -0.00693(7) 0.06546(9) 0.26144(3) 0.0164(2) Uani d 1 4 C C16 0.05381(7) 0.08463(9) 0.22459(3) 0.0160(2) Uani d 1 4 C C17 0.07382(7) 0.53424(8) 0.29053(3) 0.0135(2) Uani d 1 4 C C18 0.13053(7) 0.49506(9) 0.33033(3) 0.0158(2) Uani d 1 4 C C19 0.08441(7) 0.41675(9) 0.35956(3) 0.0165(2) Uani d 1 4 C C20 -0.01962(7) 0.37677(8) 0.34910(3) 0.0146(2) Uani d 1 4 C C21 -0.07606(7) 0.41345(9) 0.30928(3) 0.0155(2) Uani d 1 4 C C22 -0.02990(7) 0.49207(8) 0.28023(3) 0.0151(2) Uani d 1 4 C C23 -0.16599(7) -0.05933(8) 0.32037(3) 0.0147(2) Uani d 1 4 C C24 -0.09571(8) -0.15407(9) 0.31718(3) 0.0176(2) Uani d 1 4 C C25 -0.09873(8) -0.24317(9) 0.34956(3) 0.0193(3) Uani d 1 4 C C26 -0.16966(8) -0.23841(9) 0.38415(3) 0.0198(3) Uani d 1 4 C C27 -0.24049(8) -0.14512(9) 0.38657(3) 0.0186(3) Uani d 1 4 C C28 -0.23974(7) -0.05505(8) 0.35411(3) 0.0150(2) Uani d 1 4 C C29 -0.30248(7) 0.05105(8) 0.34642(3) 0.0152(2) Uani d 1 4 C C30 -0.38559(8) 0.10225(9) 0.36886(3) 0.0191(3) Uani d 1 4 C C31 -0.42956(8) 0.20743(9) 0.35264(3) 0.0210(3) Uani d 1 4 C C32 -0.39197(8) 0.26290(9) 0.31427(3) 0.0205(3) Uani d 1 4 C C33 -0.30867(8) 0.21421(9) 0.29151(3) 0.0179(2) Uani d 1 4 C C34 -0.26456(7) 0.10810(8) 0.30814(3) 0.0148(2) Uani d 1 4 C C35 -0.16106(7) 0.33032(9) 0.40192(3) 0.0159(2) Uani d 1 4 C C36 -0.22360(8) 0.43152(9) 0.39787(3) 0.0188(3) Uani d 1 4 C C37 -0.30978(8) 0.43949(10) 0.42491(3) 0.0212(3) Uani d 1 4 C C38 -0.33293(8) 0.34875(10) 0.45506(3) 0.0236(3) Uani d 1 4 C C39 -0.27007(8) 0.24787(10) 0.45899(3) 0.0223(3) Uani d 1 4 C C40 -0.18233(7) 0.23819(9) 0.43240(3) 0.0170(2) Uani d 1 4 C C41 -0.10020(8) 0.14969(9) 0.42846(3) 0.0175(2) Uani d 1 4 C C42 -0.08054(9) 0.03925(10) 0.44861(3) 0.0226(3) Uani d 1 4 C C43 0.00622(9) -0.02590(10) 0.43659(3) 0.0244(3) Uani d 1 4 C C44 0.07408(8) 0.01769(10) 0.40469(3) 0.0228(3) Uani d 1 4 C C45 0.05661(8) 0.12724(9) 0.38401(3) 0.0189(3) Uani d 1 4 C C46 -0.03140(7) 0.19226(8) 0.39617(3) 0.0160(2) Uani d 1 4 C C47 0.80231(10) 0.30685(11) -0.04452(4) 0.0339(4) Uani d 1 4 C C48 0.85225(9) 0.42513(11) -0.03281(4) 0.0282(3) Uani d 1 4 C C49 0.95454(9) 0.33966(10) 0.02754(4) 0.0245(3) Uani d 1 4 C C50 0.90396(9) 0.22141(10) 0.01655(4) 0.0269(3) Uani d 1 4 C C51 0.54937(11) 1.10962(13) 0.00476(4) 0.0395(4) Uani d 1 4 C C52 0.45101(10) 1.07707(13) 0.02839(4) 0.0386(4) Uani d 1 4 H H5 0.054237 -0.061413 0.116887 0.0217 Uiso d 1 4 H H6 0.168862 -0.017139 0.055958 0.0242 Uiso d 1 4 H H9 0.142206 0.76388 0.310565 0.0219 Uiso d 1 4 H H10 0.214363 0.892253 0.254208 0.0247 Uiso d 1 4 H H12 -0.140825 0.13803 0.147554 0.0202 Uiso d 1 4 H H13 -0.244549 0.103983 0.209249 0.0203 Uiso d 1 4 H H15 0.027728 0.049831 0.290949 0.0197 Uiso d 1 4 H H16 0.130499 0.081919 0.228817 0.0192 Uiso d 1 4 H H18 0.202257 0.522667 0.337539 0.0189 Uiso d 1 4 H H19 0.123993 0.390375 0.3868 0.0198 Uiso d 1 4 H H21 -0.147196 0.384334 0.301837 0.0187 Uiso d 1 4 H H22 -0.069541 0.517607 0.252883 0.0181 Uiso d 1 4 H H24 -0.04703 -0.157654 0.293502 0.0211 Uiso d 1 4 H H25 -0.051122 -0.309554 0.3482 0.0232 Uiso d 1 4 H H26 -0.169059 -0.300584 0.406391 0.0237 Uiso d 1 4 H H27 -0.289391 -0.142268 0.410178 0.0223 Uiso d 1 4 H H30 -0.411651 0.064814 0.395144 0.023 Uiso d 1 4 H H31 -0.486708 0.243214 0.367813 0.0252 Uiso d 1 4 H H32 -0.424256 0.335755 0.30351 0.0246 Uiso d 1 4 H H33 -0.282669 0.252348 0.265366 0.0215 Uiso d 1 4 H H36 -0.208011 0.493804 0.377167 0.0226 Uiso d 1 4 H H37 -0.354396 0.508741 0.422857 0.0255 Uiso d 1 4 H H38 -0.393145 0.35658 0.473231 0.0283 Uiso d 1 4 H H39 -0.286386 0.18565 0.479594 0.0267 Uiso d 1 4 H H42 -0.126727 0.009035 0.470516 0.0271 Uiso d 1 4 H H43 0.020312 -0.10205 0.45026 0.0293 Uiso d 1 4 H H44 0.134041 -0.02928 0.396945 0.0273 Uiso d 1 4 H H45 0.103323 0.156941 0.362209 0.0226 Uiso d 1 4 H H471 0.737086 0.298688 -0.029575 0.0407 Uiso d 1 4 H H472 0.785039 0.302453 -0.076739 0.0407 Uiso d 1 4 H H481 0.914406 0.435909 -0.049611 0.0339 Uiso d 1 4 H H482 0.802331 0.487083 -0.041466 0.0339 Uiso d 1 4 H H491 0.974151 0.344194 0.059579 0.0294 Uiso d 1 4 H H492 1.018265 0.34796 0.011561 0.0294 Uiso d 1 4 H H501 0.953803 0.159442 0.025272 0.0322 Uiso d 1 4 H H502 0.841895 0.211745 0.033502 0.0322 Uiso d 1 4 H H511 0.549266 1.193304 -0.001115 0.0473 Uiso d 1 4 H H512 0.61206 1.09123 0.024149 0.0473 Uiso d 1 4 H H521 0.450999 1.119146 0.056696 0.0463 Uiso d 1 4 H H522 0.388325 1.100452 0.009894 0.0463 Uiso d 1 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol S1 0.01653(10) 0.01426(10) 0.01372(9) -0.00212(8) 0.00552(7) -0.00029(7) S S2 0.02277(11) 0.02206(12) 0.01231(9) -0.00128(9) 0.00706(8) -0.00135(8) S S3 0.02141(11) 0.01582(11) 0.02111(11) -0.00496(9) 0.00120(9) 0.00418(8) S O1 0.0365(5) 0.0257(4) 0.0376(5) -0.0007(3) 0.0055(4) -0.0097(3) O O2 0.0280(4) 0.0214(4) 0.0239(3) 0.0025(3) 0.0041(3) -0.0014(3) O O3 0.0372(5) 0.0568(6) 0.0175(3) 0.0082(4) 0.0080(3) 0.0097(4) O N1 0.0395(5) 0.0208(4) 0.0186(4) -0.0099(4) 0.0145(4) -0.0028(3) N N2 0.0391(5) 0.0190(4) 0.0192(4) -0.0107(4) 0.0146(3) -0.0024(3) N N3 0.0157(3) 0.0185(4) 0.0137(3) 0.0012(3) 0.0047(3) 0.0020(3) N N4 0.0158(3) 0.0186(4) 0.0137(3) -0.0006(3) 0.0058(3) 0.0000(3) N C1 0.0190(4) 0.0171(4) 0.0107(3) -0.0012(3) 0.0041(3) 0.0005(3) C C2 0.0181(4) 0.0145(4) 0.0138(4) -0.0022(3) 0.0023(3) 0.0025(3) C C3 0.0158(4) 0.0176(4) 0.0105(3) 0.0005(3) 0.0034(3) -0.0001(3) C C4 0.0142(4) 0.0158(4) 0.0121(3) 0.0003(3) 0.0015(3) 0.0006(3) C C5 0.0200(4) 0.0166(4) 0.0178(4) -0.0004(3) 0.0016(3) -0.0013(3) C C6 0.0243(5) 0.0206(5) 0.0156(4) 0.0018(4) 0.0019(3) -0.0039(3) C C7 0.0144(4) 0.0136(4) 0.0156(4) -0.0014(3) 0.0017(3) 0.0018(3) C C8 0.0114(4) 0.0149(4) 0.0166(4) 0.0002(3) 0.0012(3) -0.0005(3) C C9 0.0160(4) 0.0172(4) 0.0215(4) -0.0007(3) 0.0007(3) -0.0047(3) C C10 0.0184(4) 0.0146(4) 0.0283(5) -0.0016(3) -0.0016(4) -0.0019(4) C C11 0.0156(4) 0.0134(4) 0.0130(3) -0.0013(3) 0.0024(3) 0.0012(3) C C12 0.0167(4) 0.0206(5) 0.0131(4) -0.0003(3) 0.0007(3) 0.0025(3) C C13 0.0131(4) 0.0223(5) 0.0155(4) 0.0003(3) 0.0015(3) 0.0018(3) C C14 0.0158(4) 0.0164(4) 0.0130(3) -0.0006(3) 0.0039(3) 0.0001(3) C C15 0.0160(4) 0.0207(5) 0.0126(4) -0.0009(3) 0.0005(3) 0.0016(3) C C16 0.0132(4) 0.0203(5) 0.0146(4) -0.0011(3) 0.0012(3) 0.0017(3) C C17 0.0129(4) 0.0146(4) 0.0134(3) 0.0007(3) 0.0037(3) -0.0024(3) C C18 0.0123(4) 0.0213(5) 0.0138(4) -0.0017(3) 0.0020(3) -0.0023(3) C C19 0.0157(4) 0.0221(5) 0.0117(3) -0.0002(3) 0.0015(3) -0.0003(3) C C20 0.0154(4) 0.0166(4) 0.0125(3) -0.0007(3) 0.0052(3) -0.0017(3) C C21 0.0131(4) 0.0191(4) 0.0147(4) -0.0018(3) 0.0022(3) -0.0023(3) C C22 0.0129(4) 0.0188(4) 0.0136(4) 0.0002(3) 0.0010(3) -0.0016(3) C C23 0.0162(4) 0.0166(4) 0.0114(3) -0.0014(3) 0.0019(3) -0.0002(3) C C24 0.0194(4) 0.0187(4) 0.0150(4) 0.0015(3) 0.0039(3) -0.0012(3) C C25 0.0226(5) 0.0174(5) 0.0180(4) 0.0013(4) 0.0018(3) -0.0007(3) C C26 0.0266(5) 0.0171(5) 0.0157(4) -0.0025(4) 0.0020(3) 0.0016(3) C C27 0.0220(4) 0.0197(5) 0.0146(4) -0.0036(4) 0.0056(3) -0.0003(3) C C28 0.0155(4) 0.0170(4) 0.0127(3) -0.0020(3) 0.0032(3) -0.0019(3) C C29 0.0147(4) 0.0175(4) 0.0135(3) -0.0021(3) 0.0020(3) -0.0019(3) C C30 0.0166(4) 0.0234(5) 0.0179(4) -0.0016(4) 0.0047(3) -0.0041(3) C C31 0.0160(4) 0.0230(5) 0.0240(5) 0.0005(4) 0.0024(3) -0.0078(4) C C32 0.0183(4) 0.0192(5) 0.0235(4) 0.0015(4) -0.0020(3) -0.0037(4) C C33 0.0167(4) 0.0188(4) 0.0181(4) -0.0002(3) 0.0003(3) -0.0005(3) C C34 0.0135(4) 0.0163(4) 0.0145(4) -0.0010(3) 0.0016(3) -0.0029(3) C C35 0.0148(4) 0.0215(5) 0.0121(3) -0.0033(3) 0.0042(3) -0.0033(3) C C36 0.0182(4) 0.0219(5) 0.0171(4) -0.0016(4) 0.0056(3) -0.0029(3) C C37 0.0195(4) 0.0260(5) 0.0189(4) 0.0000(4) 0.0058(3) -0.0064(4) C C38 0.0190(4) 0.0353(6) 0.0175(4) -0.0023(4) 0.0080(3) -0.0048(4) C C39 0.0213(5) 0.0316(6) 0.0145(4) -0.0060(4) 0.0064(3) -0.0009(4) C C40 0.0170(4) 0.0227(5) 0.0115(3) -0.0042(3) 0.0031(3) -0.0021(3) C C41 0.0182(4) 0.0220(5) 0.0124(4) -0.0046(3) 0.0015(3) -0.0010(3) C C42 0.0252(5) 0.0256(5) 0.0169(4) -0.0054(4) 0.0003(4) 0.0038(4) C C43 0.0284(5) 0.0226(5) 0.0215(4) -0.0015(4) -0.0030(4) 0.0036(4) C C44 0.0223(5) 0.0244(5) 0.0213(4) 0.0034(4) -0.0009(4) -0.0029(4) C C45 0.0191(4) 0.0222(5) 0.0154(4) -0.0004(4) 0.0023(3) -0.0021(3) C C46 0.0178(4) 0.0188(4) 0.0114(3) -0.0028(3) 0.0009(3) -0.0017(3) C C47 0.0335(6) 0.0365(7) 0.0309(6) -0.0032(5) -0.0030(5) -0.0038(5) C C48 0.0325(6) 0.0280(6) 0.0242(5) 0.0010(5) 0.0023(4) 0.0048(4) C C49 0.0230(5) 0.0262(5) 0.0246(5) 0.0014(4) 0.0033(4) 0.0019(4) C C50 0.0260(5) 0.0220(5) 0.0338(6) 0.0028(4) 0.0108(4) 0.0043(4) C C51 0.0430(7) 0.0470(8) 0.0290(6) 0.0020(6) 0.0065(5) -0.0002(5) C C52 0.0400(7) 0.0532(9) 0.0235(5) 0.0138(6) 0.0084(5) 0.0000(5) C loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0.0033 0.0016 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' H 0.0000 0.0000 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' N 0.0061 0.0033 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' O 0.0106 0.0060 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' S 0.1246 0.1234 'International Tables Vol C tables 4.2.6.8 and 6.1.1.1' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle C1 S1 C2 . 86.86(4) C3 S2 C6 . 91.39(5) C7 S3 C10 . 91.51(5) C47 O1 C50 . 110.00(9) C48 O2 C49 . 109.16(8) C51 O3 C52 3_675 109.62(9) N2 N1 C1 . 112.77(8) N1 N2 C2 . 112.95(9) C14 N3 C23 . 125.17(8) C14 N3 C34 . 126.57(8) C23 N3 C34 . 108.24(7) C20 N4 C35 . 124.84(8) C20 N4 C46 . 126.33(8) C35 N4 C46 . 108.54(7) S1 C1 N1 . 113.78(7) S1 C1 C3 . 126.37(7) N1 C1 C3 . 119.78(8) S1 C2 N2 . 113.58(7) S1 C2 C7 . 127.19(7) N2 C2 C7 . 119.12(8) S2 C3 C1 . 117.47(7) S2 C3 C4 . 112.00(7) C1 C3 C4 . 130.51(8) C3 C4 C5 . 111.40(8) C3 C4 C11 . 125.87(8) C5 C4 C11 . 122.71(8) C4 C5 C6 . 113.10(9) C4 C5 H5 . 123.45 C6 C5 H5 . 123.45 S2 C6 C5 . 112.10(7) S2 C6 H6 . 123.95 C5 C6 H6 . 123.95 S3 C7 C2 . 116.55(7) S3 C7 C8 . 111.78(7) C2 C7 C8 . 131.29(8) C7 C8 C9 . 111.32(8) C7 C8 C17 . 126.84(8) C9 C8 C17 . 121.84(8) C8 C9 C10 . 112.92(9) C8 C9 H9 . 123.54 C10 C9 H9 . 123.54 S3 C10 C9 . 112.46(8) S3 C10 H10 . 123.77 C9 C10 H10 . 123.77 C4 C11 C12 . 120.82(7) C4 C11 C16 . 120.61(8) C12 C11 C16 . 118.46(8) C11 C12 C13 . 121.10(8) C11 C12 H12 . 119.45 C13 C12 H12 . 119.45 C12 C13 C14 . 119.81(8) C12 C13 H13 . 120.1 C14 C13 H13 . 120.1 N3 C14 C13 . 120.40(8) N3 C14 C15 . 119.95(8) C13 C14 C15 . 119.63(8) C14 C15 C16 . 119.94(8) C14 C15 H15 . 120.03 C16 C15 H15 . 120.03 C11 C16 C15 . 120.89(8) C11 C16 H16 . 119.56 C15 C16 H16 . 119.56 C8 C17 C18 . 119.68(8) C8 C17 C22 . 121.27(7) C18 C17 C22 . 118.87(8) C17 C18 C19 . 120.86(8) C17 C18 H18 . 119.57 C19 C18 H18 . 119.57 C18 C19 C20 . 119.55(8) C18 C19 H19 . 120.23 C20 C19 H19 . 120.23 N4 C20 C19 . 120.25(7) N4 C20 C21 . 119.60(8) C19 C20 C21 . 120.12(8) C20 C21 C22 . 120.19(8) C20 C21 H21 . 119.91 C22 C21 H21 . 119.91 C17 C22 C21 . 120.40(8) C17 C22 H22 . 119.8 C21 C22 H22 . 119.8 N3 C23 C24 . 129.43(8) N3 C23 C28 . 108.86(8) C24 C23 C28 . 121.67(8) C23 C24 C25 . 117.43(9) C23 C24 H24 . 121.28 C25 C24 H24 . 121.28 C24 C25 C26 . 121.51(9) C24 C25 H25 . 119.25 C26 C25 H25 . 119.25 C25 C26 C27 . 120.67(9) C25 C26 H26 . 119.67 C27 C26 H26 . 119.67 C26 C27 C28 . 118.88(9) C26 C27 H27 . 120.56 C28 C27 H27 . 120.56 C23 C28 C27 . 119.80(9) C23 C28 C29 . 107.21(8) C27 C28 C29 . 133.00(9) C28 C29 C30 . 133.25(9) C28 C29 C34 . 107.09(8) C30 C29 C34 . 119.66(9) C29 C30 C31 . 118.93(9) C29 C30 H30 . 120.54 C31 C30 H30 . 120.53 C30 C31 C32 . 120.97(9) C30 C31 H31 . 119.51 C32 C31 H31 . 119.51 C31 C32 C33 . 121.23(9) C31 C32 H32 . 119.38 C33 C32 H32 . 119.38 C32 C33 C34 . 117.47(9) C32 C33 H33 . 121.26 C34 C33 H33 . 121.26 N3 C34 C29 . 108.60(8) N3 C34 C33 . 129.67(8) C29 C34 C33 . 121.73(9) N4 C35 C36 . 129.07(9) N4 C35 C40 . 108.87(8) C36 C35 C40 . 122.05(8) C35 C36 C37 . 117.48(9) C35 C36 H36 . 121.26 C37 C36 H36 . 121.26 C36 C37 C38 . 121.44(10) C36 C37 H37 . 119.28 C38 C37 H37 . 119.28 C37 C38 C39 . 120.81(10) C37 C38 H38 . 119.6 C39 C38 H38 . 119.6 C38 C39 C40 . 118.83(10) C38 C39 H39 . 120.59 C40 C39 H39 . 120.58 C35 C40 C39 . 119.39(9) C35 C40 C41 . 106.85(8) C39 C40 C41 . 133.76(9) C40 C41 C42 . 133.51(9) C40 C41 C46 . 106.94(8) C42 C41 C46 . 119.54(9) C41 C42 C43 . 119.02(9) C41 C42 H42 . 120.49 C43 C42 H42 . 120.49 C42 C43 C44 . 120.82(10) C42 C43 H43 . 119.59 C44 C43 H43 . 119.59 C43 C44 C45 . 121.54(10) C43 C44 H44 . 119.23 C45 C44 H44 . 119.23 C44 C45 C46 . 117.30(9) C44 C45 H45 . 121.35 C46 C45 H45 . 121.35 N4 C46 C41 . 108.78(8) N4 C46 C45 . 129.41(8) C41 C46 C45 . 121.78(9) O1 C47 C48 . 110.81(9) O1 C47 H471 . 109.47 O1 C47 H472 . 109.47 C48 C47 H471 . 109.47 C48 C47 H472 . 109.47 H471 C47 H472 . 108.1 O2 C48 C47 . 111.00(9) O2 C48 H481 . 109.47 O2 C48 H482 . 109.47 C47 C48 H481 . 109.47 C47 C48 H482 . 109.47 H481 C48 H482 . 107.9 O2 C49 C50 . 110.57(8) O2 C49 H491 . 109.47 O2 C49 H492 . 109.47 C50 C49 H491 . 109.47 C50 C49 H492 . 109.47 H491 C49 H492 . 108.35 O1 C50 C49 . 110.67(9) O1 C50 H501 . 109.47 O1 C50 H502 . 109.47 C49 C50 H501 . 109.47 C49 C50 H502 . 109.47 H501 C50 H502 . 108.25 O3 C51 C52 3_675 110.82(11) O3 C51 H511 3_675 109.47 O3 C51 H512 3_675 109.47 C52 C51 H511 . 109.47 C52 C51 H512 . 109.47 H511 C51 H512 . 108.09 O3 C52 C51 . 111.05(11) O3 C52 H521 . 109.47 O3 C52 H522 . 109.47 C51 C52 H521 . 109.47 C51 C52 H522 . 109.47 H521 C52 H522 . 107.84 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance S1 C1 . 1.7315(9) S1 C2 . 1.7339(9) S2 C3 . 1.7315(9) S2 C6 . 1.7107(11) S3 C7 . 1.7316(9) S3 C10 . 1.7061(10) O1 C47 . 1.4297(15) O1 C50 . 1.4231(14) O2 C48 . 1.4280(13) O2 C49 . 1.4256(13) O3 C51 3_675 1.4166(15) O3 C52 . 1.4249(18) N1 N2 . 1.3634(13) N1 C1 . 1.3112(13) N2 C2 . 1.3119(13) N3 C14 . 1.4184(12) N3 C23 . 1.4002(12) N3 C34 . 1.4032(12) N4 C20 . 1.4207(12) N4 C35 . 1.3961(12) N4 C46 . 1.3947(12) C1 C3 . 1.4513(13) C2 C7 . 1.4510(13) C3 C4 . 1.3745(13) C4 C5 . 1.4262(13) C4 C11 . 1.4877(12) C5 C6 . 1.3652(14) C5 H5 . 0.96 C6 H6 . 0.96 C7 C8 . 1.3814(12) C8 C9 . 1.4292(13) C8 C17 . 1.4818(13) C9 C10 . 1.3630(14) C9 H9 . 0.96 C10 H10 . 0.96 C11 C12 . 1.3937(13) C11 C16 . 1.3969(12) C12 C13 . 1.3881(13) C12 H12 . 0.96 C13 C14 . 1.3938(12) C13 H13 . 0.96 C14 C15 . 1.3952(13) C15 C16 . 1.3874(13) C15 H15 . 0.96 C16 H16 . 0.96 C17 C18 . 1.3988(12) C17 C22 . 1.3961(12) C18 C19 . 1.3888(13) C18 H18 . 0.96 C19 C20 . 1.3921(13) C19 H19 . 0.96 C20 C21 . 1.3890(12) C21 C22 . 1.3878(13) C21 H21 . 0.96 C22 H22 . 0.96 C23 C24 . 1.3922(13) C23 C28 . 1.4059(13) C24 C25 . 1.3888(14) C24 H24 . 0.96 C25 C26 . 1.4008(14) C25 H25 . 0.96 C26 C27 . 1.3818(14) C26 H26 . 0.96 C27 C28 . 1.3965(13) C27 H27 . 0.96 C28 C29 . 1.4410(13) C29 C30 . 1.3979(13) C29 C34 . 1.4110(13) C30 C31 . 1.3795(14) C30 H30 . 0.96 C31 C32 . 1.4031(15) C31 H31 . 0.96 C32 C33 . 1.3932(14) C32 H32 . 0.96 C33 C34 . 1.3929(13) C33 H33 . 0.96 C35 C36 . 1.3850(14) C35 C40 . 1.4120(13) C36 C37 . 1.3900(14) C36 H36 . 0.96 C37 C38 . 1.4000(15) C37 H37 . 0.96 C38 C39 . 1.3841(16) C38 H38 . 0.96 C39 C40 . 1.3993(14) C39 H39 . 0.96 C40 C41 . 1.4442(14) C41 C42 . 1.3948(14) C41 C46 . 1.4134(13) C42 C43 . 1.3792(15) C42 H42 . 0.96 C43 C44 . 1.4014(15) C43 H43 . 0.96 C44 C45 . 1.3888(15) C44 H44 . 0.96 C45 C46 . 1.3923(14) C45 H45 . 0.96 C47 C48 . 1.5036(17) C47 H471 . 0.96 C47 H472 . 0.96 C48 H481 . 0.96 C48 H482 . 0.96 C49 C50 . 1.5024(15) C49 H491 . 0.96 C49 H492 . 0.96 C50 H501 . 0.96 C50 H502 . 0.96 C51 C52 . 1.5037(19) C51 H511 . 0.96 C51 H512 . 0.96 C52 H521 . 0.96 C52 H522 . 0.96 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA C6 H6 O1 3_655 0.96 2.37 3.1750(13) 140.63 C44 H44 N1 2_545 0.96 2.46 3.3890(14) 162.28 _cod_database_fobs_code 2105306 _journal_paper_doi 10.1107/S0108768112039651