#------------------------------------------------------------------------------ #$Date: 2016-03-26 11:46:54 +0000 (Sat, 26 Mar 2016) $ #$Revision: 180235 $ #$URL: svn://www.crystallography.net/cod/cif/7/11/21/7112111.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_7112111 loop_ _publ_author_name 'Daisuke Uraguchi' 'Shinji Nakamura' 'Hitoshi Sasaki' 'Yuki Konakade' 'Takashi Ooi' _publ_section_title ; Enantioselective formal alpha-allylation of nitroalkanes through a chiral iminophosphorane-catalyzed Michael reaction-Julia-Kocienski olefination sequence ; _journal_name_full Chem.Commun. _journal_page_first 3491 _journal_paper_doi 10.1039/C3CC49477B _journal_volume 50 _journal_year 2014 _chemical_absolute_configuration ad _chemical_formula_moiety 'C17 H17 N5 O4 S' _chemical_formula_sum 'C17 H17 N5 O4 S' _chemical_formula_weight 387.41 _chemical_name_systematic ; ? ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 103.085(7) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.949(2) _cell_length_b 24.489(9) _cell_length_c 10.960(4) _cell_measurement_reflns_used 5616 _cell_measurement_temperature 103(2) _cell_measurement_theta_max 27.4816 _cell_measurement_theta_min 3.1416 _cell_volume 1816.7(11) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 103(2) _diffrn_detector_area_resol_mean 28.5714 _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.976 _diffrn_measurement_device ; Saturn724+ (4x4 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_radiation_detector CCD _diffrn_radiation_monochromator Confocal _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_unetI/netI 0.0784 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.976 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 14634 _diffrn_reflns_point_group_measured_fraction_full 0.954 _diffrn_reflns_point_group_measured_fraction_max 0.936 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.480 _diffrn_reflns_theta_min 3.142 _exptl_absorpt_coefficient_mu 0.213 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.8751 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour Colorless _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 808 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.308 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.049 _refine_ls_abs_structure_details ; Flack x determined using 2524 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.06(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 489 _refine_ls_number_reflns 7772 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.008 _refine_ls_R_factor_all 0.0456 _refine_ls_R_factor_gt 0.0378 _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^)+(0.0374P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.0904 _reflns_Friedel_coverage 0.873 _reflns_Friedel_fraction_full 0.925 _reflns_Friedel_fraction_max 0.893 _reflns_number_gt 6174 _reflns_number_total 7772 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c3cc49477b3.cif _cod_data_source_block shelxs _cod_original_cell_volume 1816.6(11) _cod_database_code 7112111 #BEGIN Tags that were not found in dictionaries: _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 0.939 _shelx_estimated_absorpt_t_max 0.979 _shelxl_version_number 2013-3 _shelx_res_file ; TITL 3X01nakamura_abs1 CELL 0.71075 6.9490 24.4887 10.9598 90.000 103.085 90.000 ZERR 4 0.0024 0.0085 0.0039 0.000 0.007 0.000 LATT -1 SYMM -X, .50+Y, -Z SFAC C H N O S UNIT 68 68 20 16 4 L.S. 4 ACTA bond $h FMAP 2 PLAN 5 size 0.3 0.1 0.1 FREE N9 C28 temp -170 WGHT 0.037400 FVAR 3.23909 MOLE 1 S1 5 0.920528 0.151678 0.645007 11.00000 0.02051 0.01494 = 0.01873 0.00086 0.00414 0.00200 N7 3 1.069858 0.051867 0.755826 11.00000 0.01607 0.01268 = 0.01974 0.00006 0.00450 0.00259 C18 1 0.680065 0.127826 0.574558 11.00000 0.01271 0.02103 = 0.01644 0.00127 0.00419 0.00157 AFIX 23 H18A 2 0.648816 0.096313 0.623265 11.00000 -1.20000 H18B 2 0.583572 0.157077 0.579051 11.00000 -1.20000 AFIX 0 O7 4 0.998042 0.183063 0.557137 11.00000 0.02865 0.02072 = 0.02934 0.00668 0.00814 -0.00208 O8 4 0.912886 0.174479 0.764051 11.00000 0.02851 0.02221 = 0.02264 -0.00488 0.00321 0.00691 N9 3 1.310492 0.037618 0.669390 11.00000 0.02195 0.03022 = 0.02355 0.00060 0.00894 0.00665 C28 1 1.075425 0.092805 0.674971 11.00000 0.01467 0.01691 = 0.01409 -0.00102 0.00335 -0.00163 N8 3 1.219397 0.017255 0.750850 11.00000 0.01918 0.02286 = 0.02688 -0.00206 0.00701 0.00632 N10 3 1.225438 0.085061 0.621273 11.00000 0.01641 0.02654 = 0.01898 -0.00176 0.00436 0.00206 O5 4 0.493643 0.121474 0.169941 11.00000 0.03832 0.04454 = 0.02407 0.00320 0.01292 -0.00961 C29 1 0.937248 0.040446 0.837084 11.00000 0.01972 0.01647 = 0.01842 0.00541 0.00703 0.00396 N6 3 0.415067 0.093536 0.237916 11.00000 0.01735 0.03403 = 0.01991 0.00085 0.00187 -0.00196 C30 1 0.820693 -0.006014 0.813998 11.00000 0.02519 0.02076 = 0.02248 0.00183 0.00561 -0.00024 AFIX 43 H30 2 0.828501 -0.029786 0.746789 11.00000 -1.20000 AFIX 0 C25 1 0.896723 0.049145 0.363290 11.00000 0.02045 0.03077 = 0.01758 -0.00337 0.00657 -0.00347 AFIX 43 H25 2 0.944714 0.080412 0.328297 11.00000 -1.20000 AFIX 0 C34 1 0.932432 0.075479 0.934622 11.00000 0.03050 0.01968 = 0.02577 0.00118 0.01110 -0.00023 AFIX 43 H34 2 1.015641 0.106689 0.949635 11.00000 -1.20000 AFIX 0 C20 1 0.744153 0.054729 0.424730 11.00000 0.01391 0.02158 = 0.01372 -0.00166 0.00006 -0.00044 C19 1 0.654963 0.110333 0.436607 11.00000 0.01774 0.02051 = 0.01314 0.00214 0.00644 0.00096 AFIX 13 H19 2 0.725687 0.137569 0.394663 11.00000 -1.20000 AFIX 0 C23 1 0.910684 -0.047508 0.401901 11.00000 0.03170 0.02413 = 0.03116 -0.00666 0.00432 0.00752 AFIX 43 H23 2 0.966299 -0.082344 0.393302 11.00000 -1.20000 AFIX 0 C22 1 0.759079 -0.042430 0.464372 11.00000 0.03374 0.02350 = 0.03111 0.00191 0.01010 0.00029 AFIX 43 H22 2 0.712393 -0.073778 0.499814 11.00000 -1.20000 AFIX 0 C31 1 0.692712 -0.017012 0.890986 11.00000 0.02125 0.02939 = 0.03476 0.00982 0.00529 -0.00543 AFIX 43 H31 2 0.611719 -0.048680 0.877198 11.00000 -1.20000 AFIX 0 O6 4 0.324506 0.051757 0.204254 11.00000 0.05215 0.05038 = 0.03137 -0.00784 0.00770 -0.02671 C26 1 0.433081 0.112809 0.372131 11.00000 0.01786 0.03146 = 0.01206 0.00344 0.00694 0.00291 AFIX 13 H26 2 0.358202 0.087357 0.415717 11.00000 -1.20000 AFIX 0 C24 1 0.980676 -0.001788 0.352187 11.00000 0.02277 0.03593 = 0.02658 -0.00786 0.01079 -0.00086 AFIX 43 H24 2 1.085969 -0.005045 0.310451 11.00000 -1.20000 AFIX 0 C21 1 0.675440 0.008056 0.475356 11.00000 0.02153 0.02752 = 0.02613 0.00164 0.01283 0.00269 AFIX 43 H21 2 0.570616 0.011106 0.517546 11.00000 -1.20000 AFIX 0 C32 1 0.682943 0.018472 0.988764 11.00000 0.02428 0.03734 = 0.03315 0.01282 0.01447 0.00448 AFIX 43 H32 2 0.593357 0.011260 1.040656 11.00000 -1.20000 AFIX 0 C33 1 0.802040 0.063802 1.010551 11.00000 0.03972 0.02835 = 0.02761 0.00055 0.01779 0.00684 AFIX 43 H33 2 0.795372 0.087451 1.078181 11.00000 -1.20000 AFIX 0 C27 1 0.343250 0.169073 0.367240 11.00000 0.02673 0.04230 = 0.02631 0.00325 0.00171 0.01681 AFIX 137 H27A 2 0.429589 0.195383 0.338445 11.00000 -1.50000 H27B 2 0.328449 0.179426 0.451004 11.00000 -1.50000 H27C 2 0.213357 0.168961 0.309094 11.00000 -1.50000 AFIX 0 MOLE 2 S2 5 0.859356 0.227875 0.142942 11.00000 0.01898 0.01594 = 0.02079 -0.00071 0.00451 -0.00026 O3 4 0.868535 0.202106 0.261391 11.00000 0.02421 0.02414 = 0.02785 0.00841 0.00216 -0.00300 N5 3 1.180009 0.288433 0.121262 11.00000 0.01769 0.02663 = 0.02545 -0.00017 0.00698 -0.00037 O4 4 0.910316 0.198110 0.042534 11.00000 0.03130 0.02359 = 0.03218 -0.00990 0.01114 0.00211 N3 3 1.190134 0.356835 0.252617 11.00000 0.01832 0.02606 = 0.02680 0.00013 0.00925 -0.00473 N2 3 1.032450 0.324848 0.256120 11.00000 0.01636 0.01521 = 0.01987 0.00141 0.00645 -0.00038 C11 1 1.029825 0.283614 0.173856 11.00000 0.01646 0.01687 = 0.01739 0.00087 0.00390 0.00064 C12 1 0.906748 0.336590 0.340731 11.00000 0.01904 0.01635 = 0.01870 -0.00214 0.00622 -0.00352 C13 1 0.915302 0.302065 0.442521 11.00000 0.03025 0.01955 = 0.02462 0.00266 0.00990 0.00398 AFIX 43 H13 2 1.002516 0.271677 0.456512 11.00000 -1.20000 AFIX 0 O1 4 0.277973 0.290177 -0.263833 11.00000 0.04512 0.06981 = 0.03136 -0.01053 -0.00373 0.03528 O2 4 0.466299 0.244903 -0.357340 11.00000 0.04127 0.03942 = 0.02405 0.00042 0.01146 0.00430 C17 1 0.784430 0.382038 0.319146 11.00000 0.02023 0.02042 = 0.02061 -0.00197 0.00408 -0.00161 AFIX 43 H17 2 0.783394 0.405368 0.249746 11.00000 -1.20000 AFIX 0 C1 1 0.621134 0.256929 0.094442 11.00000 0.01577 0.02044 = 0.01935 0.00023 0.00460 -0.00191 AFIX 23 H1A 2 0.524425 0.229058 0.107284 11.00000 -1.20000 H1B 2 0.612732 0.287535 0.152022 11.00000 -1.20000 AFIX 0 N4 3 1.277891 0.334339 0.172119 11.00000 0.02005 0.02977 = 0.02928 0.00009 0.00843 -0.00254 C2 1 0.552026 0.278564 -0.039889 11.00000 0.01955 0.02374 = 0.01822 -0.00174 0.00323 0.00050 AFIX 13 H2 2 0.417266 0.294020 -0.044879 11.00000 -1.20000 AFIX 0 C3 1 0.677777 0.326350 -0.066519 11.00000 0.02417 0.02034 = 0.01399 0.00024 0.00209 -0.00137 N1 3 0.414591 0.259289 -0.263025 11.00000 0.02346 0.03461 = 0.02100 -0.00312 0.00010 0.00045 C15 1 0.667301 0.358132 0.502243 11.00000 0.02775 0.03607 = 0.03014 -0.00706 0.01718 -0.00287 AFIX 43 H15 2 0.583096 0.365300 0.557628 11.00000 -1.20000 AFIX 0 C16 1 0.663983 0.392553 0.401175 11.00000 0.01962 0.02838 = 0.03090 -0.00452 0.00686 0.00677 AFIX 43 H16 2 0.578860 0.423395 0.388272 11.00000 -1.20000 AFIX 0 C8 1 0.838582 0.320617 -0.120386 11.00000 0.03278 0.02318 = 0.02332 0.00123 0.00841 0.00240 AFIX 43 H8 2 0.872062 0.285536 -0.146265 11.00000 -1.20000 AFIX 0 C10 1 0.403613 0.185004 -0.115724 11.00000 0.03587 0.03230 = 0.02703 -0.00487 -0.00010 -0.01093 AFIX 137 H10A 2 0.278137 0.197629 -0.099168 11.00000 -1.50000 H10B 2 0.477359 0.164662 -0.043047 11.00000 -1.50000 H10C 2 0.377370 0.161183 -0.189490 11.00000 -1.50000 AFIX 0 C9 1 0.524783 0.234015 -0.139758 11.00000 0.02148 0.02362 = 0.02153 -0.00167 0.00038 0.00069 AFIX 13 H9 2 0.657454 0.221202 -0.148859 11.00000 -1.20000 AFIX 0 C6 1 0.904602 0.416461 -0.098289 11.00000 0.04215 0.02955 = 0.02483 0.00843 0.00309 -0.01394 AFIX 43 H6A 2 0.982964 0.447252 -0.107964 11.00000 -1.20000 AFIX 0 C5 1 0.743258 0.422838 -0.045193 11.00000 0.04879 0.02272 = 0.03452 -0.00308 0.00823 -0.00407 AFIX 43 H5 2 0.709789 0.458019 -0.019885 11.00000 -1.20000 AFIX 0 C14 1 0.792581 0.313373 0.522953 11.00000 0.04517 0.02627 = 0.02633 0.00129 0.02127 -0.00200 AFIX 43 H14 2 0.794351 0.290265 0.592823 11.00000 -1.20000 AFIX 0 C4 1 0.630929 0.378024 -0.029018 11.00000 0.03533 0.02700 = 0.03004 -0.00317 0.01312 0.00083 AFIX 43 H4 2 0.520829 0.382510 0.007995 11.00000 -1.20000 AFIX 0 C7 1 0.952158 0.365907 -0.137081 11.00000 0.02851 0.03987 = 0.02617 0.00828 0.00824 -0.00267 AFIX 43 H7 2 1.061455 0.361767 -0.174980 11.00000 -1.20000 AFIX 0 HKLF 4 REM 3X01nakamura_abs1 REM R1 = 0.0378 for 6174 Fo > 4sig(Fo) and 0.0456 for all 7772 data REM 489 parameters refined using 1 restraints END WGHT 0.0374 0.0000 REM Highest difference peak 0.308, deepest hole -0.251, 1-sigma level 0.049 Q1 1 0.4181 0.2589 -0.1167 11.00000 0.05 0.31 Q2 1 0.7385 0.2487 0.1016 11.00000 0.05 0.26 Q3 1 0.9661 0.2594 0.1796 11.00000 0.05 0.25 Q4 1 0.9942 0.1183 0.6664 11.00000 0.05 0.25 Q5 1 0.7111 0.0813 0.4365 11.00000 0.05 0.24 ; _shelx_res_checksum 52450 _shelx_hkl_file ; 0 0 210543.60 376.35 0 0 -210310.02 381.37 0 0 2 9723.05 361.15 0 0 -2 9838.56 360.71 0 0 3 48.27 68.43 0 0 -3 97.38 66.57 0 0 3 53.15 50.89 0 0 -3 95.92 50.70 0 0 420000.67 724.92 0 0 -419066.76 696.96 0 0 420147.80 721.94 0 0 -423457.55 819.74 0 0 5 2800.74 213.39 0 0 5 2475.61 188.40 0 0 -5 2599.00 180.58 0 0 6 -14.03 74.96 0 0 6 43.94 38.02 0 0 -6 17.96 36.59 0 0 7 45.58 45.19 0 0 7 46.80 82.35 0 0 819736.29 683.34 0 0 818565.05 648.85 0 0 9 333.03 186.27 0 0 9 357.78 187.54 0 0 1029098.16 1566.12 0 0 1029406.29 794.94 0 0 11 334.91 292.98 0 0 11 420.22 151.85 0 0 12 1249.73 386.59 0 0 12 1282.70 438.62 0 0 13 1921.83 216.60 0 1 211850.27 439.80 0 1 213128.41 460.69 0 1 -215055.75 529.27 0 1 -213073.03 464.18 0 -1 213134.43 485.31 0 -1 -214066.30 498.69 0 -1 212967.02 459.59 0 -1 -213163.31 467.56 0 -1 336964.09 1270.80 0 1 418447.75 667.22 0 1 418733.63 695.37 0 1 -419169.56 687.60 0 1 -418687.26 677.17 0 -1 -420580.21 734.03 0 -1 418847.66 685.66 0 -1 419277.79 688.26 0 1 5 9463.53 375.40 0 1 5 9184.58 426.42 0 1 -5 9137.14 349.77 0 -1 510191.24 402.23 0 -1 5 9482.91 377.83 0 -1 -5 9736.15 371.44 0 1 6 1787.05 186.85 0 1 6 1862.50 172.59 0 1 -6 1805.43 162.80 0 -1 6 1608.61 157.66 0 -1 6 1667.87 178.64 0 -1 -6 1818.29 152.35 0 1 7 1202.87 167.08 0 1 7 1166.07 149.52 0 -1 7 1093.35 162.34 0 -1 7 1062.30 125.83 0 1 8 5348.03 471.49 0 1 8 5791.65 293.78 0 -1 8 5161.30 462.75 0 -1 8 5524.52 523.01 0 1 9 1121.36 148.78 0 1 9 1201.74 173.30 0 -1 9 1028.74 187.83 0 -1 9 1037.69 329.21 0 1 10 331.35 223.82 0 1 10 345.96 196.56 0 -1 10 302.23 377.04 0 -1 10 102.64 158.22 0 1 11 2805.93 231.88 0 1 11 2722.55 266.74 0 -1 11 2881.58 310.33 0 -1 11 2664.00 354.96 0 1 12 215.91 212.60 0 -1 12 331.90 296.38 0 -1 12 260.29 212.86 0 1 13 1279.54 188.12 0 -1 13 1464.90 505.13 0 2 -333173.96 1146.20 0 -2 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2391.50 261.79 -7 -15 1 2252.43 229.09 7 15 0 581.41 131.88 7 -15 0 323.84 495.17 -7 -15 0 496.77 149.14 7 15 1 2675.95 203.07 7 -15 1 3206.93 305.17 -7 -15 -1 2589.09 411.26 7 15 2 1295.49 241.26 7 -15 2 1437.17 288.86 -7 -15 -2 1343.77 229.80 7 15 3 178.60 231.22 7 -15 3 308.09 392.01 -7 -15 -3 333.70 316.50 -7 -16 7 2896.81 428.81 -7 -16 6 25.42 53.86 -7 -16 5 2721.14 540.41 -7 -16 4 8361.94 926.46 7 -16 -4 9038.57 702.67 -7 -16 4 9037.57 719.13 -7 -16 3 3104.84 310.94 7 -16 -3 3338.98 420.15 -7 -16 3 3646.82 325.54 7 16 -2 351.64 415.61 7 -16 -2 569.52 209.25 -7 -16 2 427.64 176.65 7 16 -1 928.52 369.69 7 -16 -1 1014.78 310.26 -7 -16 1 1036.51 196.39 7 16 0 523.15 391.49 7 -16 0 729.45 188.54 -7 -16 0 409.85 357.33 7 16 1 2590.98 300.90 7 -16 1 2635.37 348.00 -7 -16 -1 2607.01 340.62 7 16 2 59.98 70.36 7 -16 2 0.40 179.21 -7 -16 -2 87.45 91.24 -7 -17 7 347.62 440.46 -7 -17 6 1965.19 274.16 -7 -17 5 1500.75 233.96 -7 -17 4 193.21 271.29 7 -17 -4 195.23 174.60 -7 -17 4 144.16 187.33 -7 -17 3 111.02 138.12 7 -17 -3 98.50 192.77 7 17 -2 2781.44 290.62 7 -17 -2 2692.47 212.44 -7 -17 2 3115.76 211.60 7 17 -1 2461.55 202.72 7 -17 -1 2567.80 230.20 -7 -17 1 1698.61 242.96 7 17 0 24.65 40.85 7 -17 0 80.17 81.55 -7 -17 0 28.79 57.21 7 17 1 86.84 115.13 7 -17 1 19.48 110.80 -7 -17 -1 69.98 130.55 7 17 2 1245.64 314.55 7 -17 2 1500.26 229.59 -7 -17 -2 1247.30 323.06 -7 -18 6 4321.27 342.14 -7 -18 5 979.05 161.24 -7 -18 4 2401.65 380.45 -7 -18 4 3213.32 346.13 -7 -18 3 624.67 262.94 7 -18 -3 564.85 424.50 -7 -18 3 699.98 232.79 7 18 -2 29.10 134.11 -7 -18 2 28.15 98.63 7 18 -1 743.73 422.69 7 -18 -1 543.98 436.17 -7 -18 1 626.78 124.84 7 18 0 1450.38 169.62 7 -18 0 1151.30 363.47 -7 -18 0 1231.04 164.54 7 18 1 211.39 243.61 7 -18 1 43.91 148.65 -7 -18 -1 70.81 79.09 -7 -19 5 655.62 169.36 -7 -19 4 322.54 477.75 -7 -19 4 506.35 318.98 -7 -19 3 838.08 241.82 7 -19 -3 1262.29 153.33 -7 -19 3 1414.80 152.97 7 19 -2 7342.77 434.22 7 -19 -2 7626.57 499.51 -7 -19 2 6202.51 660.22 7 19 -1 311.95 460.22 7 -19 -1 317.44 359.84 -7 -19 1 349.14 373.83 7 19 0 700.39 123.56 7 -19 0 915.96 166.00 -7 -19 0 345.56 383.22 8 0 -3 1771.18 177.00 8 0 -2 265.65 188.24 8 0 0 3565.69 347.98 8 0 1 79.08 117.68 8 0 2 1096.03 681.41 8 0 3 596.53 368.27 8 1 -3 57.43 127.09 8 -1 -3 36.27 60.98 8 1 -2 1190.72 152.19 8 -1 -2 1027.38 123.90 8 1 -1 4828.98 562.73 8 -1 -1 5108.00 591.58 8 1 0 3477.89 328.21 8 -1 0 3510.20 370.05 8 1 1 2349.88 355.43 8 -1 1 2390.16 276.58 8 1 2 242.95 172.11 8 -1 2 163.69 236.58 8 1 3 762.27 371.95 8 -1 3 747.88 551.45 8 2 -3 3523.63 383.12 8 -2 -3 3788.97 451.12 8 2 -2 567.68 288.33 8 -2 -2 546.27 367.28 8 2 -1 1020.43 177.40 8 -2 -1 965.98 135.13 8 2 0 1518.73 206.59 8 -2 0 1808.80 198.39 8 2 1 5881.98 322.32 8 -2 1 5844.17 393.04 8 2 2 158.13 168.04 8 -2 2 135.96 192.00 8 2 3 1426.85 455.52 8 -2 3 1230.38 239.47 8 -3 -3 1078.55 140.81 8 3 -2 920.60 120.59 8 -3 -2 889.24 210.19 8 3 -1 47.81 67.64 8 -3 -1 7.08 85.01 8 3 0 142.75 202.86 8 -3 0 131.81 236.62 8 3 1 265.09 363.50 8 -3 1 267.76 245.73 8 3 2 740.47 191.00 8 -3 2 681.53 312.09 8 3 3 97.71 158.64 8 -3 3 22.75 86.80 8 -4 -3 128.20 201.74 -8 -4 3 181.79 134.57 8 4 -2 1054.74 122.57 8 -4 -2 1156.22 224.94 8 4 -1 3707.59 414.09 8 -4 -1 3849.47 435.61 8 4 0 3831.13 357.01 8 -4 0 3510.40 533.73 8 4 1 7158.42 346.37 8 -4 1 6854.53 720.19 8 4 2 48.95 125.32 8 -4 2 107.45 151.39 8 4 3 170.17 159.72 8 -4 3 342.23 263.66 8 -5 -3 1353.98 146.56 8 -5 -2 75.19 89.22 -8 -5 2 107.34 145.25 8 5 -1 545.09 313.50 8 -5 -1 485.28 462.20 8 5 0 3536.76 431.40 8 -5 0 4094.31 384.57 8 5 1 2456.96 232.63 8 -5 1 1708.70 303.29 8 5 2 1577.08 193.65 8 -5 2 1265.67 194.12 8 5 3 62.71 138.20 8 -5 3 261.91 371.43 -8 -6 8 100.38 139.64 8 -6 -3 6.69 42.94 8 -6 -2 3486.56 331.27 -8 -6 2 3069.19 289.92 8 -6 -1 278.19 238.88 -8 -6 1 351.95 348.91 8 6 0 2612.09 276.64 8 -6 0 2756.22 286.32 8 6 1 39.94 144.88 8 -6 1 68.43 111.21 8 6 2 6366.64 732.16 8 -6 2 6599.95 689.56 -8 -7 8 384.67 353.73 -8 -7 7 121.50 219.86 8 -7 -3 453.24 313.03 8 -7 -2 503.13 418.19 -8 -7 2 998.25 289.04 8 -7 -1 42.72 111.09 -8 -7 1 63.54 114.10 8 -7 0 1125.80 153.05 -8 -7 0 924.31 367.01 8 7 1 590.08 320.38 8 -7 1 792.67 323.75 8 7 2 1280.06 161.05 8 -7 2 1465.13 286.60 -8 -8 8 298.12 402.25 -8 -8 7 177.69 316.97 -8 -8 6 6512.32 301.88 8 -8 -3 142.88 136.50 -8 -8 3 105.21 205.07 8 -8 -2 3112.54 302.38 -8 -8 2 2970.13 324.82 8 -8 -1 1323.73 262.24 -8 -8 1 1435.65 460.81 8 -8 0 1718.27 180.64 -8 -8 0 1708.82 217.19 8 -8 1 3786.39 427.29 -8 -8 -1 3941.29 454.73 8 8 2 1206.57 216.30 8 -8 2 1028.72 564.63 -8 -9 7 578.10 304.58 -8 -9 6 749.97 207.08 -8 -9 5 1073.98 328.10 8 -9 -3 218.33 264.12 8 -9 -2 464.52 287.76 -8 -9 2 614.29 161.63 8 -9 -1 2214.94 263.87 -8 -9 1 2292.42 403.56 8 -9 0 1184.73 158.02 -8 -9 0 1708.33 196.36 8 -9 1 154.97 177.15 -8 -9 -1 162.94 183.00 8 -9 2 2689.15 304.39 -8 -9 -2 2329.18 235.34 -8 -10 7 117.98 115.96 -8 -10 6 749.49 346.22 -8 -10 5 678.43 114.67 -8 -10 4 5.21 45.58 8 -10 -2 3867.87 304.37 -8 -10 2 3252.71 243.03 8 -10 -1 1604.84 216.52 -8 -10 1 1509.28 156.37 8 -10 0 256.71 250.36 -8 -10 0 106.48 173.10 8 -10 1 3108.17 275.19 -8 -10 -1 3312.48 296.28 -8 -11 7 330.11 345.99 -8 -11 6 449.63 492.94 -8 -11 5 124.47 266.90 -8 -11 4 11.46 102.98 8 -11 -2 415.43 234.80 -8 -11 2 570.51 179.73 8 -11 -1 4738.88 516.95 -8 -11 1 4232.60 555.08 8 -11 0 47.87 93.47 -8 -11 0 -10.04 81.92 8 -11 1 403.37 417.30 -8 -11 -1 297.88 274.84 -8 -12 6 265.33 404.70 -8 -12 5 820.17 324.67 -8 -12 4 881.95 410.12 -8 -12 3 1776.28 231.45 8 -12 -2 68.62 123.17 -8 -12 2 80.97 77.42 8 -12 -1 64.69 119.80 -8 -12 1 65.58 53.15 8 -12 0 43.38 70.98 -8 -12 0 76.85 85.47 -8 -13 5 651.19 109.68 -8 -13 4 414.40 184.53 -8 -13 3 147.57 132.59 -8 -13 2 820.90 285.35 8 -13 -2 1110.49 160.91 -8 -13 2 749.91 121.29 8 -13 -1 973.57 473.89 -8 -13 1 1076.07 143.63 8 -13 0 586.40 277.57 -8 -13 0 739.86 160.90 -8 -14 4 328.21 162.74 -8 -14 3 869.51 432.43 -8 -14 2 128.22 254.01 -8 -14 2 325.98 353.55 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 20931 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 S1 S 0.92053(11) 0.15168(3) 0.64501(7) 0.01811(18) Uani 1 1 d . . N7 N 1.0699(3) 0.05187(10) 0.7558(2) 0.0161(5) Uani 1 1 d . . C18 C 0.6801(4) 0.12783(13) 0.5746(3) 0.0166(6) Uani 1 1 d . . H18A H 0.6488 0.0963 0.6233 0.020 Uiso 1 1 calc R U H18B H 0.5836 0.1571 0.5791 0.020 Uiso 1 1 calc R U O7 O 0.9980(3) 0.18306(9) 0.5571(2) 0.0260(5) Uani 1 1 d . . O8 O 0.9129(3) 0.17448(9) 0.7641(2) 0.0249(5) Uani 1 1 d . . N9 N 1.3105(4) 0.03762(12) 0.6694(3) 0.0246(6) Uani 1 1 d . . C28 C 1.0754(4) 0.09281(13) 0.6750(3) 0.0152(6) Uani 1 1 d . . N8 N 1.2194(4) 0.01725(12) 0.7508(3) 0.0227(6) Uani 1 1 d . . N10 N 1.2254(4) 0.08506(12) 0.6213(3) 0.0206(6) Uani 1 1 d . . O5 O 0.4936(4) 0.12147(12) 0.1699(2) 0.0347(6) Uani 1 1 d . . C29 C 0.9372(4) 0.04045(12) 0.8371(3) 0.0178(7) Uani 1 1 d . . N6 N 0.4151(4) 0.09354(12) 0.2379(3) 0.0241(6) Uani 1 1 d . . C30 C 0.8207(5) -0.00601(14) 0.8140(3) 0.0228(7) Uani 1 1 d . . H30 H 0.8285 -0.0298 0.7468 0.027 Uiso 1 1 calc R U C25 C 0.8967(5) 0.04914(15) 0.3633(3) 0.0226(7) Uani 1 1 d . . H25 H 0.9447 0.0804 0.3283 0.027 Uiso 1 1 calc R U C34 C 0.9324(5) 0.07548(14) 0.9346(3) 0.0246(8) Uani 1 1 d . . H34 H 1.0156 0.1067 0.9496 0.029 Uiso 1 1 calc R U C20 C 0.7442(4) 0.05473(13) 0.4247(3) 0.0169(6) Uani 1 1 d . . C19 C 0.6550(4) 0.11033(13) 0.4366(3) 0.0167(6) Uani 1 1 d . . H19 H 0.7257 0.1376 0.3947 0.020 Uiso 1 1 calc R U C23 C 0.9107(5) -0.04751(15) 0.4019(3) 0.0294(8) Uani 1 1 d . . H23 H 0.9663 -0.0823 0.3933 0.035 Uiso 1 1 calc R U C22 C 0.7591(5) -0.04243(16) 0.4644(4) 0.0290(8) Uani 1 1 d . . H22 H 0.7124 -0.0738 0.4998 0.035 Uiso 1 1 calc R U C31 C 0.6927(5) -0.01701(15) 0.8910(4) 0.0286(8) Uani 1 1 d . . H31 H 0.6117 -0.0487 0.8772 0.034 Uiso 1 1 calc R U O6 O 0.3245(4) 0.05176(12) 0.2043(3) 0.0449(7) Uani 1 1 d . . C26 C 0.4331(5) 0.11281(14) 0.3721(3) 0.0199(7) Uani 1 1 d . . H26 H 0.3582 0.0874 0.4157 0.024 Uiso 1 1 calc R U C24 C 0.9807(5) -0.00179(15) 0.3522(3) 0.0276(8) Uani 1 1 d . . H24 H 1.0860 -0.0050 0.3105 0.033 Uiso 1 1 calc R U C21 C 0.6754(5) 0.00806(15) 0.4754(3) 0.0239(7) Uani 1 1 d . . H21 H 0.5706 0.0111 0.5175 0.029 Uiso 1 1 calc R U C32 C 0.6829(5) 0.01847(16) 0.9888(4) 0.0303(9) Uani 1 1 d . . H32 H 0.5934 0.0113 1.0407 0.036 Uiso 1 1 calc R U C33 C 0.8020(6) 0.06380(15) 1.0106(4) 0.0303(9) Uani 1 1 d . . H33 H 0.7954 0.0875 1.0782 0.036 Uiso 1 1 calc R U C27 C 0.3433(5) 0.16907(16) 0.3672(3) 0.0325(9) Uani 1 1 d . . H27A H 0.4296 0.1954 0.3384 0.049 Uiso 1 1 calc R U H27B H 0.3284 0.1794 0.4510 0.049 Uiso 1 1 calc R U H27C H 0.2134 0.1690 0.3091 0.049 Uiso 1 1 calc R U S2 S 0.85936(11) 0.22788(3) 0.14294(7) 0.01857(17) Uani 1 1 d . . O3 O 0.8685(3) 0.20211(10) 0.2614(2) 0.0260(5) Uani 1 1 d . . N5 N 1.1800(4) 0.28843(12) 0.1213(3) 0.0229(6) Uani 1 1 d . . O4 O 0.9103(4) 0.19811(10) 0.0425(2) 0.0284(6) Uani 1 1 d . . N3 N 1.1901(4) 0.35684(12) 0.2526(3) 0.0231(6) Uani 1 1 d . . N2 N 1.0325(4) 0.32485(10) 0.2561(2) 0.0168(6) Uani 1 1 d . . C11 C 1.0298(4) 0.28361(13) 0.1739(3) 0.0169(6) Uani 1 1 d . . C12 C 0.9067(5) 0.33659(13) 0.3407(3) 0.0177(7) Uani 1 1 d . . C13 C 0.9153(5) 0.30206(14) 0.4425(3) 0.0242(8) Uani 1 1 d . . H13 H 1.0025 0.2717 0.4565 0.029 Uiso 1 1 calc R U O1 O 0.2780(4) 0.29018(14) -0.2638(3) 0.0507(9) Uani 1 1 d . . O2 O 0.4663(4) 0.24490(11) -0.3573(2) 0.0343(6) Uani 1 1 d . . C17 C 0.7844(5) 0.38204(13) 0.3191(3) 0.0205(7) Uani 1 1 d . . H17 H 0.7834 0.4054 0.2497 0.025 Uiso 1 1 calc R U C1 C 0.6211(4) 0.25693(13) 0.0944(3) 0.0184(6) Uani 1 1 d . . H1A H 0.5244 0.2291 0.1073 0.022 Uiso 1 1 calc R U H1B H 0.6127 0.2875 0.1520 0.022 Uiso 1 1 calc R U N4 N 1.2779(4) 0.33434(12) 0.1721(3) 0.0259(7) Uani 1 1 d . . C2 C 0.5520(5) 0.27856(13) -0.0399(3) 0.0207(7) Uani 1 1 d . . H2 H 0.4173 0.2940 -0.0449 0.025 Uiso 1 1 calc R U C3 C 0.6778(5) 0.32635(13) -0.0665(3) 0.0199(7) Uani 1 1 d . . N1 N 0.4146(4) 0.25929(13) -0.2630(3) 0.0271(7) Uani 1 1 d . . C15 C 0.6673(5) 0.35813(16) 0.5022(3) 0.0296(8) Uani 1 1 d . . H15 H 0.5831 0.3653 0.5576 0.036 Uiso 1 1 calc R U C16 C 0.6640(5) 0.39255(15) 0.4012(3) 0.0261(8) Uani 1 1 d . . H16 H 0.5789 0.4234 0.3883 0.031 Uiso 1 1 calc R U C8 C 0.8386(5) 0.32062(15) -0.1204(3) 0.0261(8) Uani 1 1 d . . H8 H 0.8721 0.2855 -0.1463 0.031 Uiso 1 1 calc R U C10 C 0.4036(6) 0.18500(15) -0.1157(4) 0.0329(9) Uani 1 1 d . . H10A H 0.2781 0.1976 -0.0992 0.049 Uiso 1 1 calc R U H10B H 0.4774 0.1647 -0.0430 0.049 Uiso 1 1 calc R U H10C H 0.3774 0.1612 -0.1895 0.049 Uiso 1 1 calc R U C9 C 0.5248(5) 0.23402(14) -0.1398(3) 0.0229(7) Uani 1 1 d . . H9 H 0.6575 0.2212 -0.1489 0.028 Uiso 1 1 calc R U C6 C 0.9046(6) 0.41646(16) -0.0983(3) 0.0329(9) Uani 1 1 d . . H6A H 0.9830 0.4473 -0.1080 0.039 Uiso 1 1 calc R U C5 C 0.7433(6) 0.42284(16) -0.0452(4) 0.0355(9) Uani 1 1 d . . H5 H 0.7098 0.4580 -0.0199 0.043 Uiso 1 1 calc R U C14 C 0.7926(6) 0.31337(15) 0.5230(4) 0.0305(9) Uani 1 1 d . . H14 H 0.7944 0.2903 0.5928 0.037 Uiso 1 1 calc R U C4 C 0.6309(6) 0.37802(15) -0.0290(4) 0.0299(8) Uani 1 1 d . . H4 H 0.5208 0.3825 0.0080 0.036 Uiso 1 1 calc R U C7 C 0.9522(5) 0.36591(17) -0.1371(3) 0.0312(8) Uani 1 1 d . . H7 H 1.0615 0.3618 -0.1750 0.037 Uiso 1 1 calc R U 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 S1 0.0205(4) 0.0149(4) 0.0187(4) 0.0009(3) 0.0041(3) 0.0020(3) N7 0.0161(13) 0.0127(13) 0.0197(14) 0.0001(11) 0.0045(10) 0.0026(10) C18 0.0127(15) 0.0210(16) 0.0164(16) 0.0013(12) 0.0042(12) 0.0016(12) O7 0.0286(13) 0.0207(13) 0.0293(13) 0.0067(10) 0.0081(10) -0.0021(10) O8 0.0285(13) 0.0222(12) 0.0226(13) -0.0049(10) 0.0032(10) 0.0069(10) N9 0.0220(14) 0.0302(16) 0.0235(15) 0.0006(12) 0.0089(12) 0.0067(12) C28 0.0147(15) 0.0169(15) 0.0141(15) -0.0010(12) 0.0034(12) -0.0016(12) N8 0.0192(14) 0.0229(15) 0.0269(16) -0.0021(12) 0.0070(12) 0.0063(11) N10 0.0164(13) 0.0265(15) 0.0190(14) -0.0018(12) 0.0044(11) 0.0021(11) O5 0.0383(15) 0.0445(16) 0.0241(14) 0.0032(12) 0.0129(11) -0.0096(12) C29 0.0197(16) 0.0165(16) 0.0184(17) 0.0054(12) 0.0070(13) 0.0040(12) N6 0.0174(14) 0.0340(17) 0.0199(14) 0.0009(12) 0.0019(11) -0.0020(12) C30 0.0252(17) 0.0208(17) 0.0225(18) 0.0018(14) 0.0056(14) -0.0002(14) C25 0.0205(17) 0.0308(19) 0.0176(16) -0.0034(14) 0.0066(13) -0.0035(14) C34 0.0305(19) 0.0197(17) 0.0258(19) 0.0012(14) 0.0111(15) -0.0002(14) C20 0.0139(15) 0.0216(16) 0.0137(15) -0.0017(12) 0.0001(12) -0.0004(13) C19 0.0177(15) 0.0205(16) 0.0131(15) 0.0021(12) 0.0064(12) 0.0010(13) C23 0.032(2) 0.0241(19) 0.031(2) -0.0067(15) 0.0043(16) 0.0075(15) C22 0.034(2) 0.0235(18) 0.031(2) 0.0019(16) 0.0101(16) 0.0003(15) C31 0.0213(18) 0.029(2) 0.035(2) 0.0098(16) 0.0053(15) -0.0054(14) O6 0.0521(17) 0.0504(19) 0.0314(15) -0.0078(13) 0.0077(13) -0.0267(15) C26 0.0179(16) 0.0315(18) 0.0121(15) 0.0034(13) 0.0069(12) 0.0029(14) C24 0.0228(18) 0.036(2) 0.0266(19) -0.0079(16) 0.0108(15) -0.0009(15) C21 0.0215(17) 0.0275(18) 0.0261(18) 0.0016(15) 0.0128(14) 0.0027(14) C32 0.0243(19) 0.037(2) 0.033(2) 0.0128(17) 0.0145(16) 0.0045(16) C33 0.040(2) 0.028(2) 0.028(2) 0.0005(16) 0.0178(17) 0.0068(16) C27 0.0267(19) 0.042(2) 0.0263(19) 0.0032(16) 0.0017(15) 0.0168(17) S2 0.0190(4) 0.0159(4) 0.0208(4) -0.0007(3) 0.0045(3) -0.0003(3) O3 0.0242(12) 0.0241(13) 0.0278(13) 0.0084(10) 0.0022(10) -0.0030(10) N5 0.0177(14) 0.0266(16) 0.0255(16) -0.0002(13) 0.0070(12) -0.0004(12) O4 0.0313(13) 0.0236(13) 0.0322(14) -0.0099(11) 0.0111(11) 0.0021(11) N3 0.0183(15) 0.0261(16) 0.0268(16) 0.0001(12) 0.0093(12) -0.0047(12) N2 0.0164(13) 0.0152(13) 0.0199(14) 0.0014(11) 0.0065(11) -0.0004(10) C11 0.0165(15) 0.0169(15) 0.0174(16) 0.0009(12) 0.0039(12) 0.0006(12) C12 0.0190(16) 0.0163(15) 0.0187(17) -0.0021(12) 0.0062(13) -0.0035(12) C13 0.0303(19) 0.0196(17) 0.0246(19) 0.0027(14) 0.0099(15) 0.0040(14) O1 0.0451(17) 0.070(2) 0.0314(16) -0.0105(15) -0.0037(13) 0.0353(16) O2 0.0413(15) 0.0394(16) 0.0240(13) 0.0004(11) 0.0115(11) 0.0043(12) C17 0.0202(17) 0.0204(17) 0.0206(17) -0.0020(13) 0.0041(13) -0.0016(13) C1 0.0158(15) 0.0204(16) 0.0193(16) 0.0002(12) 0.0046(12) -0.0019(13) N4 0.0200(15) 0.0298(16) 0.0293(17) 0.0001(13) 0.0084(13) -0.0025(12) C2 0.0195(16) 0.0237(17) 0.0182(16) -0.0017(13) 0.0032(13) 0.0005(13) C3 0.0242(17) 0.0203(16) 0.0140(16) 0.0002(13) 0.0021(13) -0.0014(13) N1 0.0235(15) 0.0346(17) 0.0210(15) -0.0031(13) 0.0001(12) 0.0005(13) C15 0.028(2) 0.036(2) 0.030(2) -0.0071(17) 0.0172(16) -0.0029(16) C16 0.0196(17) 0.0284(19) 0.031(2) -0.0045(15) 0.0069(15) 0.0068(14) C8 0.033(2) 0.0232(18) 0.0233(18) 0.0012(14) 0.0084(16) 0.0024(15) C10 0.036(2) 0.032(2) 0.0270(19) -0.0049(15) -0.0001(15) -0.0109(16) C9 0.0215(16) 0.0236(17) 0.0215(16) -0.0017(13) 0.0004(13) 0.0007(14) C6 0.042(2) 0.030(2) 0.025(2) 0.0084(16) 0.0031(17) -0.0139(17) C5 0.049(2) 0.0227(19) 0.035(2) -0.0031(17) 0.0082(19) -0.0041(17) C14 0.045(2) 0.0263(19) 0.026(2) 0.0013(15) 0.0213(17) -0.0020(16) C4 0.035(2) 0.027(2) 0.030(2) -0.0032(15) 0.0131(16) 0.0008(16) C7 0.029(2) 0.040(2) 0.0262(19) 0.0083(17) 0.0082(15) -0.0027(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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O7 S1 O8 120.12(15) O7 S1 C18 110.21(15) O8 S1 C18 107.44(14) O7 S1 C28 104.76(14) O8 S1 C28 107.02(14) C18 S1 C28 106.48(15) C28 N7 N8 107.7(2) C28 N7 C29 131.9(3) N8 N7 C29 120.4(2) C19 C18 S1 113.9(2) C19 C18 H18A 108.8 S1 C18 H18A 108.8 C19 C18 H18B 108.8 S1 C18 H18B 108.8 H18A C18 H18B 107.7 N8 N9 N10 110.9(2) N10 C28 N7 109.3(3) N10 C28 S1 122.5(2) N7 C28 S1 128.1(2) N9 N8 N7 106.5(3) C28 N10 N9 105.6(3) C34 C29 C30 122.5(3) C34 C29 N7 119.2(3) C30 C29 N7 118.3(3) O6 N6 O5 123.8(3) O6 N6 C26 118.6(3) O5 N6 C26 117.6(3) C31 C30 C29 118.6(3) C31 C30 H30 120.7 C29 C30 H30 120.7 C20 C25 C24 120.8(3) C20 C25 H25 119.6 C24 C25 H25 119.6 C29 C34 C33 118.0(3) C29 C34 H34 121.0 C33 C34 H34 121.0 C25 C20 C21 118.6(3) C25 C20 C19 120.3(3) C21 C20 C19 121.1(3) C20 C19 C18 112.1(2) C20 C19 C26 112.4(2) C18 C19 C26 108.5(2) C20 C19 H19 107.9 C18 C19 H19 107.9 C26 C19 H19 107.9 C24 C23 C22 119.8(3) C24 C23 H23 120.1 C22 C23 H23 120.1 C21 C22 C23 120.3(3) C21 C22 H22 119.8 C23 C22 H22 119.8 C30 C31 C32 119.8(3) C30 C31 H31 120.1 C32 C31 H31 120.1 C27 C26 N6 107.8(3) C27 C26 C19 114.5(3) N6 C26 C19 106.6(2) C27 C26 H26 109.3 N6 C26 H26 109.3 C19 C26 H26 109.3 C23 C24 C25 120.0(3) C23 C24 H24 120.0 C25 C24 H24 120.0 C22 C21 C20 120.5(3) C22 C21 H21 119.8 C20 C21 H21 119.8 C33 C32 C31 120.4(3) C33 C32 H32 119.8 C31 C32 H32 119.8 C32 C33 C34 120.7(3) C32 C33 H33 119.6 C34 C33 H33 119.6 C26 C27 H27A 109.5 C26 C27 H27B 109.5 H27A C27 H27B 109.5 C26 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 O4 S2 O3 120.34(15) O4 S2 C1 110.59(15) O3 S2 C1 107.23(14) O4 S2 C11 105.43(15) O3 S2 C11 105.84(15) C1 S2 C11 106.53(15) C11 N5 N4 105.5(3) N4 N3 N2 106.3(3) C11 N2 N3 107.6(3) C11 N2 C12 131.4(3) N3 N2 C12 121.0(3) N5 C11 N2 109.6(3) N5 C11 S2 123.1(2) N2 C11 S2 127.2(2) C17 C12 C13 122.5(3) C17 C12 N2 119.2(3) C13 C12 N2 118.3(3) C14 C13 C12 117.9(3) C14 C13 H13 121.0 C12 C13 H13 121.0 C16 C17 C12 118.4(3) C16 C17 H17 120.8 C12 C17 H17 120.8 C2 C1 S2 119.7(2) C2 C1 H1A 107.4 S2 C1 H1A 107.4 C2 C1 H1B 107.4 S2 C1 H1B 107.4 H1A C1 H1B 106.9 N3 N4 N5 111.0(3) C9 C2 C3 113.2(3) C9 C2 C1 113.7(3) C3 C2 C1 112.3(3) C9 C2 H2 105.6 C3 C2 H2 105.6 C1 C2 H2 105.6 C8 C3 C4 118.9(3) C8 C3 C2 123.8(3) C4 C3 C2 117.3(3) O1 N1 O2 123.6(3) O1 N1 C9 119.7(3) O2 N1 C9 116.6(3) C14 C15 C16 120.5(3) C14 C15 H15 119.8 C16 C15 H15 119.8 C17 C16 C15 120.1(3) C17 C16 H16 119.9 C15 C16 H16 119.9 C3 C8 C7 120.7(3) C3 C8 H8 119.7 C7 C8 H8 119.7 C9 C10 H10A 109.5 C9 C10 H10B 109.5 H10A C10 H10B 109.5 C9 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 C10 C9 N1 106.7(3) C10 C9 C2 115.0(3) N1 C9 C2 107.5(3) C10 C9 H9 109.2 N1 C9 H9 109.2 C2 C9 H9 109.2 C7 C6 C5 120.4(3) C7 C6 H6A 119.8 C5 C6 H6A 119.8 C4 C5 C6 120.0(4) C4 C5 H5 120.0 C6 C5 H5 120.0 C15 C14 C13 120.5(3) C15 C14 H14 119.7 C13 C14 H14 119.7 C5 C4 C3 120.5(3) C5 C4 H4 119.7 C3 C4 H4 119.7 C6 C7 C8 119.5(3) C6 C7 H7 120.3 C8 C7 H7 120.3 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 O7 1.429(2) S1 O8 1.431(2) S1 C18 1.774(3) S1 C28 1.785(3) N7 C28 1.344(4) N7 N8 1.352(3) N7 C29 1.446(4) C18 C19 1.543(4) C18 H18A 0.9900 C18 H18B 0.9900 N9 N8 1.305(4) N9 N10 1.355(4) C28 N10 1.322(4) O5 N6 1.227(4) C29 C34 1.377(5) C29 C30 1.386(4) N6 O6 1.214(4) N6 C26 1.523(4) C30 C31 1.384(5) C30 H30 0.9500 C25 C20 1.385(4) C25 C24 1.394(5) C25 H25 0.9500 C34 C33 1.392(5) C34 H34 0.9500 C20 C21 1.401(4) C20 C19 1.514(4) C19 C26 1.545(4) C19 H19 1.0000 C23 C24 1.381(5) C23 C22 1.386(5) C23 H23 0.9500 C22 C21 1.383(5) C22 H22 0.9500 C31 C32 1.393(5) C31 H31 0.9500 C26 C27 1.509(5) C26 H26 1.0000 C24 H24 0.9500 C21 H21 0.9500 C32 C33 1.373(5) C32 H32 0.9500 C33 H33 0.9500 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 S2 O4 1.430(2) S2 O3 1.432(2) S2 C1 1.769(3) S2 C11 1.789(3) N5 C11 1.307(4) N5 N4 1.366(4) N3 N4 1.303(4) N3 N2 1.355(4) N2 C11 1.351(4) N2 C12 1.440(4) C12 C17 1.388(4) C12 C13 1.390(5) C13 C14 1.386(5) C13 H13 0.9500 O1 N1 1.212(4) O2 N1 1.221(4) C17 C16 1.384(5) C17 H17 0.9500 C1 C2 1.536(4) C1 H1A 0.9900 C1 H1B 0.9900 C2 C9 1.526(4) C2 C3 1.528(5) C2 H2 1.0000 C3 C8 1.384(5) C3 C4 1.392(5) N1 C9 1.525(4) C15 C14 1.386(5) C15 C16 1.388(5) C15 H15 0.9500 C16 H16 0.9500 C8 C7 1.397(5) C8 H8 0.9500 C10 C9 1.523(5) C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 C9 H9 1.0000 C6 C7 1.373(6) C6 C5 1.384(6) C6 H6A 0.9500 C5 C4 1.381(5) C5 H5 0.9500 C14 H14 0.9500 C4 H4 0.9500 C7 H7 0.9500