#------------------------------------------------------------------------------ #$Date: 2019-05-18 04:09:11 +0300 (Sat, 18 May 2019) $ #$Revision: 215288 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/12/34/7123490.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_7123490 loop_ _publ_author_name 'Gharpure, Santosh J.' 'Vishwakarma, Dharmendra S.' 'Patel, Raj Kumar' _publ_section_title ; TMSOTf Mediated ‘5/6-endo-dig’ Reductive Hydroamination for the Stereoselective Synthesis of Pyrrolidine and Piperidine derivatives ; _journal_name_full 'Chemical Communications' _journal_paper_doi 10.1039/C9CC03127H _journal_year 2019 _chemical_absolute_configuration unk _chemical_formula_moiety '4(C18 H21 N O2 S)' _chemical_formula_sum 'C72 H84 N4 O8 S4' _chemical_formula_weight 1261.67 _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 dual _audit_creation_date 2018-10-24 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-04-02 deposited with the CCDC. 2019-05-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.315(3) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 17.8848(4) _cell_length_b 7.37022(15) _cell_length_c 25.6676(6) _cell_measurement_reflns_used 10463 _cell_measurement_temperature 150 _cell_measurement_theta_max 72.2580 _cell_measurement_theta_min 2.5710 _cell_volume 3230.05(13) _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_collection 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 150 _diffrn_detector CCD _diffrn_detector_area_resol_mean 28.5714 _diffrn_detector_type 'Rigaku Saturn724+' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -191.00 -42.00 1.00 8.00 -- -101.00 0.00-108.00 149 2 \w -122.00 2.00 1.00 8.00 -- -32.00 -72.00 108.00 124 3 \w -191.00 -77.00 1.00 8.00 -- -101.00 -72.00 36.00 114 4 \w -135.00 -68.00 1.00 8.00 -- -101.00 72.00-180.00 67 5 \w -64.00 33.00 1.00 8.00 -- -32.00 0.00-108.00 97 6 \w -44.00 -14.00 1.00 8.00 -- -101.00 72.00 -36.00 30 7 \w -53.00 -23.00 1.00 8.00 -- -101.00 72.00 108.00 30 8 \w -191.00-161.00 1.00 8.00 -- -101.00 -72.00-180.00 30 9 \w -80.00 -18.00 1.00 8.00 -- -101.00 72.00-108.00 62 10 \w -135.00 -18.00 1.00 8.00 -- -101.00 72.00 36.00 117 11 \w -191.00 -67.00 1.00 8.00 -- -101.00 -72.00 -36.00 124 12 \w -169.00 -67.00 1.00 8.00 -- -101.00 -72.00-108.00 102 13 \w -98.00 40.00 1.00 8.00 -- -32.00 0.00-180.00 138 14 \w -138.00 -74.00 1.00 8.00 -- -101.00 0.00 108.00 64 15 \w -66.00 58.00 1.00 8.00 -- -32.00 72.00-180.00 124 16 \w -191.00 -67.00 1.00 8.00 -- -101.00 -72.00 108.00 124 17 \w -147.00-116.00 1.00 8.00 -- -101.00 0.00 -36.00 31 18 \w -30.00 0.00 1.00 8.00 -- -32.00 -72.00 36.00 30 19 \w -191.00 -42.00 1.00 8.00 -- -101.00 0.00 36.00 149 20 \w -66.00 -33.00 1.00 8.00 -- -32.00 72.00-108.00 33 ; _diffrn_measurement_device 'AFC12 (Right): Kappa 3 circle' _diffrn_measurement_device_type 'Rigaku Saturn724+ (2x2 bin mode)' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_measurement_specimen_support 'Mitegen 50um' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0831101000 _diffrn_orient_matrix_UB_12 -0.0689287000 _diffrn_orient_matrix_UB_13 0.0048343000 _diffrn_orient_matrix_UB_21 -0.0075069000 _diffrn_orient_matrix_UB_22 0.0737314000 _diffrn_orient_matrix_UB_23 -0.0574856000 _diffrn_orient_matrix_UB_31 0.0343415000 _diffrn_orient_matrix_UB_32 0.1831158000 _diffrn_orient_matrix_UB_33 0.0249358000 _diffrn_radiation_collimation 0.3 _diffrn_radiation_monochromator Confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0975 _diffrn_reflns_av_unetI/netI 0.0798 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 35767 _diffrn_reflns_point_group_measured_fraction_full 0.919 _diffrn_reflns_point_group_measured_fraction_max 0.919 _diffrn_reflns_theta_full 64.995 _diffrn_reflns_theta_max 64.995 _diffrn_reflns_theta_min 1.803 _diffrn_source 'Rotating Anode' _diffrn_source_current 24.0 _diffrn_source_power 1.2 _diffrn_source_target Mo _diffrn_source_type 'Rotating Anode' _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 1.829 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.39927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.297 _exptl_crystal_description block _exptl_crystal_F_000 1344 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.278 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.099 _refine_ls_abs_structure_details ; Flack x determined using 2400 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.028(15) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 789 _refine_ls_number_reflns 10110 _refine_ls_number_restraints 44 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0818 _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^)+(0.1496P)^2^+1.7551P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2130 _refine_ls_wR_factor_ref 0.2400 _reflns_Friedel_coverage 0.691 _reflns_Friedel_fraction_full 0.822 _reflns_Friedel_fraction_max 0.822 _reflns_number_gt 8044 _reflns_number_total 10110 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9cc03127h2.cif _cod_data_source_block sjg-rp-02-163_cu _cod_original_cell_volume 3230.06(13) _cod_database_code 7123490 _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_max 0.711 _shelx_estimated_absorpt_t_min 0.711 _reflns_odcompleteness_completeness 98.09 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 72.79 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C9-C8 1.7 with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001 Uanis(C8) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005 4.a Ternary CH refined with riding coordinates: C44(H44), C65(H65), C47(H47), C62(H62), C29(H29), C25(H25), C9(H9), C12(H12) 4.b Secondary CH2 refined with riding coordinates: C46(H46A,H46B), C64(H64A,H64B), C45(H45A,H45B), C63(H63A,H63B), C27(H27A, H27B), C28(H28A,H28B), C10(H10A,H10B), C11(H11A,H11B) 4.c Aromatic/amide H refined with riding coordinates: C59(H59), C41(H41), C53(H53), C3(H3), C71(H71), C69(H69), C67(H67), C012(H012), C21(H21), C56(H56), C42(H42), C68(H68), C51(H51), C52(H52), C38(H38), C32(H32), C6(H6), C50(H50), C39(H39), C49(H49), C31(H31), C60(H60), C70(H70), C4(H4), C35(H35), C7(H7), C22(H22), C33(H33), C57(H57), C34(H34), C24(H24), C15(H15), C16(H16), C17(H17), C18(H18), C14(H14) 4.d Fitted hexagon refined as free rotating group: C15(C16,C17,C18,C13,C14) 4.e Idealised Me refined as rotating group: C61(H61A,H61B,H61C), C43(H43A,H43B,H43C), C36(H36A,H36B,H36C), C54(H54A,H54B, H54C), C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C1(H1A,H1B,H1C), C8(H8A,H8B, H8C) ; _shelx_res_file ; TITL sjg-rp-02-163_cu_a.res in P2(1) sjg-rp-02-163_cu.res created by SHELXL-2018/3 at 14:49:18 on 24-Oct-2018 REM Old TITL sjg-rp-02-163_cu_a.res in P2(1) REM SHELXT solution in P2(1) REM R1 0.186, Rweak 0.019, Alpha 0.012, Orientation as input REM Flack x = 0.229 ( 0.030 ) from Parsons' quotients REM Formula found by SHELXT: C68 N7 O8 S4 CELL 1.54184 17.884826 7.37022 25.667594 90 107.3145 90 ZERR 2 0.000404 0.000152 0.000598 0 0.0025 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O S UNIT 144 168 8 16 8 DFIX 1.7 C9 C8 ISOR 0.001 0.001 C13 C14 C15 C16 C17 C18 ISOR 0.005 0.005 C8 L.S. 100 PLAN 2 SIZE 0.2 0.2 0.2 TEMP -123.15 BOND $H list 4 fmap 2 acta OMIT -3 130 REM REM REM WGHT 0.149600 1.755100 FVAR 2.57451 S3 5 0.694683 0.528710 0.549524 11.00000 0.02566 0.03554 = 0.03968 0.00651 0.01431 0.00086 S2 5 0.686818 0.540045 0.302573 11.00000 0.03744 0.04422 = 0.05264 0.01198 0.02413 0.00727 S4 5 0.708702 0.573604 0.808138 11.00000 0.03497 0.03655 = 0.04155 0.00215 0.01915 -0.00042 S1 5 0.714885 0.396954 0.077566 11.00000 0.05073 0.04857 = 0.06159 -0.01245 0.03432 -0.00638 O4 4 0.679202 0.587796 0.598754 11.00000 0.03645 0.06217 = 0.03457 0.00676 0.01743 -0.00070 O6 4 0.688685 0.639343 0.854880 11.00000 0.04954 0.04890 = 0.04245 -0.00658 0.02528 -0.00316 O5 4 0.723208 0.350291 0.546640 11.00000 0.02941 0.02977 = 0.07400 0.01312 0.02226 0.00470 O7 4 0.740687 0.397361 0.809025 11.00000 0.03556 0.03654 = 0.05824 0.00935 0.01896 0.00009 O2 4 0.672040 0.610492 0.350841 11.00000 0.05073 0.08217 = 0.04672 0.01293 0.02802 0.01218 N00A 3 0.759298 0.668032 0.538939 11.00000 0.02976 0.03164 = 0.03734 0.00303 0.01444 0.00345 O00B 4 0.752007 0.568388 0.085827 11.00000 0.07680 0.05036 = 0.10742 -0.02948 0.05377 -0.01198 O3 4 0.715222 0.359965 0.302677 11.00000 0.04340 0.03651 = 0.10777 0.02042 0.03717 0.00957 O1 4 0.687472 0.321782 0.119996 11.00000 0.05221 0.09670 = 0.05511 -0.00273 0.03292 -0.00407 N00E 3 0.750547 0.675691 0.289061 11.00000 0.03157 0.03791 = 0.04492 0.00779 0.01930 0.00462 N00F 3 0.771875 0.717725 0.797940 11.00000 0.03651 0.02949 = 0.03735 -0.00280 0.01818 -0.00011 C30 1 0.856009 0.490583 0.269158 11.00000 0.03352 0.03701 = 0.06114 0.00027 0.02774 -0.00316 N00H 3 0.775659 0.257542 0.063290 11.00000 0.04477 0.04423 = 0.04702 -0.00582 0.02237 -0.00148 C48 1 0.852793 0.479908 0.504773 11.00000 0.03198 0.02729 = 0.04259 0.00591 0.02049 -0.00675 C23 1 0.598275 0.554830 0.248645 11.00000 0.03780 0.03730 = 0.04954 0.00019 0.02400 -0.00052 C44 1 0.745926 0.868876 0.545404 11.00000 0.02419 0.03408 = 0.05299 0.00343 0.01614 0.00245 AFIX 13 H44 2 0.688916 0.893578 0.538999 11.00000 -1.20000 AFIX 0 C37 1 0.464987 0.555348 0.412257 11.00000 0.03109 0.03999 = 0.04840 0.00446 0.01277 -0.00893 C65 1 0.802911 0.693296 0.749956 11.00000 0.02529 0.03766 = 0.03461 -0.00114 0.01316 -0.00064 AFIX 13 H65 2 0.758297 0.686267 0.715544 11.00000 -1.20000 AFIX 0 C47 1 0.795935 0.633580 0.494721 11.00000 0.02696 0.03915 = 0.03623 0.00153 0.01626 0.00292 AFIX 13 H47 2 0.753768 0.612013 0.459657 11.00000 -1.20000 AFIX 0 C59 1 0.622048 0.492400 0.703855 11.00000 0.03538 0.04675 = 0.05903 -0.00522 0.02925 -0.00979 AFIX 43 H59 2 0.668662 0.440806 0.699778 11.00000 -1.20000 AFIX 0 C58 1 0.623170 0.576507 0.752474 11.00000 0.03546 0.03043 = 0.04263 0.00012 0.01969 -0.00077 C62 1 0.761075 0.914419 0.807084 11.00000 0.03510 0.03924 = 0.04487 -0.00005 0.01654 0.00551 AFIX 13 H62 2 0.704396 0.941261 0.801402 11.00000 -1.20000 AFIX 0 C40 1 0.606647 0.546818 0.496218 11.00000 0.02647 0.02892 = 0.04200 0.00274 0.01551 -0.00323 C20 1 0.457911 0.572684 0.164574 11.00000 0.04625 0.03971 = 0.05684 0.00664 0.02610 -0.01532 C41 1 0.601873 0.474277 0.445775 11.00000 0.03466 0.04449 = 0.04617 -0.00715 0.02268 -0.00404 AFIX 43 H41 2 0.646682 0.420299 0.439538 11.00000 -1.20000 AFIX 0 C66 1 0.856364 0.531943 0.753577 11.00000 0.03234 0.02472 = 0.03757 -0.00171 0.01608 -0.00554 C53 1 0.904046 0.449793 0.556621 11.00000 0.03401 0.03402 = 0.04704 0.00314 0.01388 0.00370 AFIX 43 H53 2 0.900361 0.520459 0.586713 11.00000 -1.20000 AFIX 0 C3 1 0.500733 0.329848 -0.030551 11.00000 0.04773 0.04253 = 0.08571 -0.00111 0.02758 0.00040 AFIX 43 H3 2 0.453262 0.269639 -0.031807 11.00000 -1.20000 AFIX 0 C71 1 0.852975 0.438370 0.706121 11.00000 0.03859 0.03276 = 0.04520 -0.00277 0.01798 -0.00359 AFIX 43 H71 2 0.813692 0.469098 0.673293 11.00000 -1.20000 AFIX 0 C69 1 0.962279 0.258604 0.752272 11.00000 0.04007 0.03271 = 0.08633 -0.00623 0.03263 -0.00570 AFIX 43 H69 2 0.999444 0.166846 0.751950 11.00000 -1.20000 AFIX 0 C55 1 0.483615 0.556442 0.666240 11.00000 0.03794 0.03482 = 0.05437 0.00514 0.01581 -0.01023 C29 1 0.789174 0.619504 0.248101 11.00000 0.03044 0.05652 = 0.04726 0.00158 0.01926 0.00053 AFIX 13 H29 2 0.749658 0.565613 0.215669 11.00000 -1.20000 AFIX 0 C67 1 0.913588 0.484708 0.800699 11.00000 0.03305 0.03678 = 0.04970 0.00149 0.01368 -0.00116 AFIX 43 H67 2 0.916905 0.546612 0.833775 11.00000 -1.20000 AFIX 0 C012 1 0.591285 0.466597 0.200438 11.00000 0.04054 0.04832 = 0.06859 -0.00749 0.03520 -0.00245 AFIX 43 H012 2 0.633580 0.396978 0.195843 11.00000 -1.20000 AFIX 0 C21 1 0.465487 0.659514 0.213254 11.00000 0.03905 0.04102 = 0.06192 0.01307 0.02059 0.00782 AFIX 43 H21 2 0.422316 0.725508 0.217942 11.00000 -1.20000 AFIX 0 C46 1 0.833768 0.819650 0.492240 11.00000 0.03235 0.04022 = 0.05288 0.01375 0.01938 0.00344 AFIX 23 H46A 2 0.884009 0.831676 0.521599 11.00000 -1.20000 H46B 2 0.843246 0.838047 0.456523 11.00000 -1.20000 AFIX 0 C64 1 0.846174 0.874724 0.752100 11.00000 0.02943 0.03358 = 0.04495 0.00569 0.01711 -0.00083 AFIX 23 H64A 2 0.896880 0.874422 0.781322 11.00000 -1.20000 H64B 2 0.855491 0.901847 0.716769 11.00000 -1.20000 AFIX 0 C56 1 0.485811 0.642432 0.715718 11.00000 0.03681 0.03641 = 0.06550 0.00301 0.02172 0.00147 AFIX 43 H56 2 0.439155 0.692269 0.720251 11.00000 -1.20000 AFIX 0 C45 1 0.773551 0.953572 0.500178 11.00000 0.03636 0.03461 = 0.06420 0.01311 0.01975 0.00431 AFIX 23 H45A 2 0.729524 0.967200 0.466257 11.00000 -1.20000 H45B 2 0.797506 1.074005 0.511301 11.00000 -1.20000 AFIX 0 C63 1 0.789073 1.010178 0.764417 11.00000 0.03774 0.02323 = 0.04979 0.00716 0.00989 -0.00166 AFIX 23 H63A 2 0.815748 1.125462 0.778723 11.00000 -1.20000 H63B 2 0.744946 1.035954 0.731366 11.00000 -1.20000 AFIX 0 C42 1 0.531821 0.480246 0.404336 11.00000 0.04235 0.04507 = 0.04144 -0.00964 0.01861 -0.01632 AFIX 43 H42 2 0.529413 0.431710 0.369587 11.00000 -1.20000 AFIX 0 C68 1 0.966523 0.347221 0.800259 11.00000 0.03225 0.05121 = 0.06635 0.01044 0.00933 -0.00134 AFIX 43 H68 2 1.005550 0.314456 0.832997 11.00000 -1.20000 AFIX 0 C51 1 0.966420 0.210852 0.519698 11.00000 0.04447 0.03782 = 0.11907 0.00380 0.05585 0.00640 AFIX 43 H51 2 1.004961 0.118479 0.524686 11.00000 -1.20000 AFIX 0 C52 1 0.960614 0.315492 0.563952 11.00000 0.03236 0.04218 = 0.08211 0.01936 0.02079 0.00875 AFIX 43 H52 2 0.995738 0.294243 0.599285 11.00000 -1.20000 AFIX 0 C25 1 0.737362 0.874074 0.289165 11.00000 0.02777 0.04582 = 0.06258 0.00985 0.01359 0.00708 AFIX 13 H25 2 0.681424 0.898757 0.286675 11.00000 -1.20000 AFIX 0 C38 1 0.470044 0.627582 0.463273 11.00000 0.03038 0.03151 = 0.05488 0.00701 0.01426 0.00446 AFIX 43 H38 2 0.424523 0.677248 0.469630 11.00000 -1.20000 AFIX 0 C32 1 0.938501 0.254257 0.252755 11.00000 0.06470 0.05504 = 0.12340 -0.03847 0.06403 -0.00322 AFIX 43 H32 2 0.951546 0.172780 0.228125 11.00000 -1.20000 AFIX 0 C6 1 0.639058 0.510511 -0.026283 11.00000 0.06390 0.03865 = 0.07102 0.00403 0.04671 0.00520 AFIX 43 H6 2 0.685683 0.574947 -0.024710 11.00000 -1.20000 AFIX 0 C50 1 0.915000 0.244887 0.468794 11.00000 0.06281 0.04137 = 0.08925 -0.00724 0.05337 -0.01052 AFIX 43 H50 2 0.918324 0.175316 0.438404 11.00000 -1.20000 AFIX 0 C39 1 0.540323 0.628516 0.505087 11.00000 0.03671 0.02936 = 0.04612 -0.00074 0.01976 0.00240 AFIX 43 H39 2 0.543594 0.683474 0.539174 11.00000 -1.20000 AFIX 0 C49 1 0.859327 0.377255 0.461429 11.00000 0.04304 0.04299 = 0.05064 -0.00718 0.03110 -0.01166 AFIX 43 H49 2 0.824651 0.398853 0.425966 11.00000 -1.20000 AFIX 0 C31 1 0.875597 0.363801 0.234418 11.00000 0.04253 0.06563 = 0.07385 -0.03072 0.03162 -0.01695 AFIX 43 H31 2 0.844099 0.355062 0.197480 11.00000 -1.20000 AFIX 0 C60 1 0.554310 0.483771 0.662058 11.00000 0.04189 0.05354 = 0.04286 -0.01027 0.02284 -0.01647 AFIX 43 H60 2 0.554756 0.426793 0.628953 11.00000 -1.20000 AFIX 0 C61 1 0.809226 0.968500 0.864982 11.00000 0.05704 0.03470 = 0.04808 -0.00690 0.01602 0.00205 AFIX 137 H61A 2 0.796515 0.887412 0.891400 11.00000 -1.50000 H61B 2 0.796809 1.093834 0.872120 11.00000 -1.50000 H61C 2 0.865155 0.958847 0.868462 11.00000 -1.50000 AFIX 0 C70 1 0.905747 0.300511 0.705428 11.00000 0.05055 0.03394 = 0.07170 -0.01299 0.03362 -0.00713 AFIX 43 H70 2 0.902258 0.236639 0.672640 11.00000 -1.20000 AFIX 0 C5 1 0.634065 0.409158 0.018153 11.00000 0.05197 0.03727 = 0.06381 -0.00707 0.03468 0.00030 C4 1 0.565154 0.318252 0.016977 11.00000 0.05661 0.04676 = 0.06080 -0.00064 0.03209 -0.00276 AFIX 43 H4 2 0.561727 0.249962 0.047574 11.00000 -1.20000 AFIX 0 C43 1 0.791858 0.929710 0.601227 11.00000 0.04045 0.04913 = 0.05357 -0.00423 0.00987 -0.00036 AFIX 137 H43A 2 0.772582 0.867411 0.628428 11.00000 -1.50000 H43B 2 0.785835 1.061051 0.604380 11.00000 -1.50000 H43C 2 0.847313 0.900604 0.607522 11.00000 -1.50000 AFIX 0 C2 1 0.505654 0.427173 -0.075155 11.00000 0.05829 0.05575 = 0.06491 -0.00443 0.02696 0.02392 C35 1 0.902711 0.491728 0.323563 11.00000 0.03571 0.05004 = 0.05299 0.00582 0.02117 0.00845 AFIX 43 H35 2 0.890963 0.573944 0.348540 11.00000 -1.20000 AFIX 0 C36 1 0.388148 0.544314 0.367739 11.00000 0.03778 0.06031 = 0.05972 0.00982 0.00536 -0.00458 AFIX 137 H36A 2 0.397667 0.549994 0.332096 11.00000 -1.50000 H36B 2 0.354698 0.646065 0.371241 11.00000 -1.50000 H36C 2 0.362059 0.429699 0.370897 11.00000 -1.50000 AFIX 0 C7 1 0.574906 0.516927 -0.073345 11.00000 0.07275 0.05475 = 0.06942 0.00648 0.04102 0.02347 AFIX 43 H7 2 0.578556 0.582912 -0.104289 11.00000 -1.20000 AFIX 0 C22 1 0.535734 0.652707 0.256218 11.00000 0.04141 0.03763 = 0.05446 -0.00329 0.02395 -0.00104 AFIX 43 H22 2 0.540473 0.713497 0.289685 11.00000 -1.20000 AFIX 0 C54 1 0.407998 0.533955 0.621226 11.00000 0.04527 0.05391 = 0.05779 0.00733 0.00863 -0.01239 AFIX 137 H54A 2 0.387448 0.411438 0.622731 11.00000 -1.50000 H54B 2 0.417392 0.552310 0.585879 11.00000 -1.50000 H54C 2 0.369875 0.623463 0.625732 11.00000 -1.50000 AFIX 0 C19 1 0.382125 0.578162 0.118621 11.00000 0.06137 0.07266 = 0.06404 0.01286 0.01551 -0.02298 AFIX 137 H19A 2 0.347085 0.668668 0.126817 11.00000 -1.50000 H19B 2 0.357108 0.458564 0.114640 11.00000 -1.50000 H19C 2 0.392977 0.610812 0.084571 11.00000 -1.50000 AFIX 0 C33 1 0.983802 0.258289 0.306087 11.00000 0.04676 0.05021 = 0.10623 0.00574 0.03356 0.00639 AFIX 43 H33 2 1.027668 0.179668 0.318137 11.00000 -1.20000 AFIX 0 C57 1 0.554560 0.654989 0.757414 11.00000 0.04387 0.03443 = 0.05101 0.00026 0.02706 0.00271 AFIX 43 H57 2 0.555482 0.717660 0.789941 11.00000 -1.20000 AFIX 0 C34 1 0.966307 0.374111 0.341805 11.00000 0.04304 0.06104 = 0.06982 0.01527 0.02215 0.01064 AFIX 43 H34 2 0.997137 0.375198 0.379007 11.00000 -1.20000 AFIX 0 C27 1 0.753754 0.939012 0.237389 11.00000 0.05434 0.04493 = 0.08479 0.02811 0.02593 0.00401 AFIX 23 H27A 2 0.773398 1.065389 0.241204 11.00000 -1.20000 H27B 2 0.706383 0.930908 0.205447 11.00000 -1.20000 AFIX 0 C24 1 0.520899 0.480384 0.157974 11.00000 0.05113 0.06270 = 0.05397 -0.00958 0.02552 -0.02443 AFIX 43 H24 2 0.516837 0.424472 0.123893 11.00000 -1.20000 AFIX 0 C28 1 0.817244 0.804657 0.232575 11.00000 0.04461 0.06303 = 0.08189 0.02737 0.03085 0.00234 AFIX 23 H28A 2 0.868977 0.837463 0.257954 11.00000 -1.20000 H28B 2 0.821055 0.802161 0.194885 11.00000 -1.20000 AFIX 0 C9 1 0.766898 0.056774 0.072898 11.00000 0.04683 0.05203 = 0.09204 0.01410 0.01977 0.00033 AFIX 13 H9 2 0.733277 0.031241 0.096972 11.00000 -1.20000 AFIX 0 C26 1 0.790470 0.957643 0.340926 11.00000 0.06808 0.06425 = 0.07179 -0.00992 -0.00820 0.01851 AFIX 137 H26A 2 0.783112 0.894853 0.372698 11.00000 -1.50000 H26B 2 0.777499 1.086361 0.342388 11.00000 -1.50000 H26C 2 0.845151 0.945769 0.341173 11.00000 -1.50000 AFIX 0 C1 1 0.438576 0.434146 -0.125834 11.00000 0.10063 0.06500 = 0.07732 -0.01973 0.02440 0.02641 AFIX 137 H1A 2 0.403920 0.330473 -0.126690 11.00000 -1.50000 H1B 2 0.458116 0.429365 -0.157656 11.00000 -1.50000 H1C 2 0.409425 0.547202 -0.126603 11.00000 -1.50000 AFIX 66 C15 1 0.874798 0.569924 -0.040278 11.00000 0.10349 0.10348 = 0.10333 0.00051 0.03066 0.00091 AFIX 43 H15 2 0.847865 0.578322 -0.078159 11.00000 -1.20000 AFIX 65 C16 1 0.938553 0.682008 -0.017150 11.00000 0.09654 0.09671 = 0.09742 0.00059 0.03047 0.00087 AFIX 43 H16 2 0.955194 0.767011 -0.039224 11.00000 -1.20000 AFIX 65 C17 1 0.977960 0.669719 0.038277 11.00000 0.08241 0.08305 = 0.08541 -0.00090 0.02624 0.00009 AFIX 43 H17 2 1.021533 0.746324 0.054084 11.00000 -1.20000 AFIX 65 C18 1 0.953611 0.545345 0.070576 11.00000 0.08761 0.08716 = 0.08730 -0.00069 0.02668 0.00219 AFIX 43 H18 2 0.980544 0.536947 0.108458 11.00000 -1.20000 AFIX 65 C13 1 0.889856 0.433260 0.047449 11.00000 0.07598 0.07656 = 0.07815 0.00111 0.02683 0.00030 C14 1 0.850449 0.445547 -0.007978 11.00000 0.09469 0.09579 = 0.09677 -0.00098 0.02874 0.00079 AFIX 43 H14 2 0.806875 0.368942 -0.023784 11.00000 -1.20000 AFIX 0 C12 1 0.862070 0.303980 0.081118 11.00000 0.07131 0.11843 = 0.08998 0.03430 0.03312 0.00435 AFIX 13 H12 2 0.877715 0.347563 0.119759 11.00000 -1.20000 AFIX 0 C10 1 0.844729 -0.012554 0.094062 11.00000 0.06976 0.05214 = 0.23532 0.02097 0.05157 -0.01323 AFIX 23 H10A 2 0.847555 -0.135741 0.079386 11.00000 -1.20000 H10B 2 0.858906 -0.021137 0.134320 11.00000 -1.20000 AFIX 0 C11 1 0.899341 0.106754 0.078730 11.00000 0.08652 0.12503 = 0.15038 0.05201 0.04725 0.05240 AFIX 23 H11A 2 0.901862 0.078887 0.041559 11.00000 -1.20000 H11B 2 0.952544 0.097444 0.104862 11.00000 -1.20000 AFIX 0 C8 1 0.730631 -0.022111 0.011236 11.00000 0.20600 0.18497 = 0.19219 -0.00420 0.04319 0.00626 AFIX 137 H8A 2 0.689963 0.060484 -0.009981 11.00000 -1.50000 H8B 2 0.707769 -0.142100 0.012770 11.00000 -1.50000 H8C 2 0.772340 -0.032182 -0.006184 11.00000 -1.50000 AFIX 0 HKLF 4 REM sjg-rp-02-163_cu_a.res in P2(1) REM wR2 = 0.2400, GooF = S = 1.038, Restrained GooF = 1.040 for all data REM R1 = 0.0818 for 8044 Fo > 4sig(Fo) and 0.1003 for all 10110 data REM 789 parameters refined using 44 restraints END WGHT 0.1495 1.7533 REM Highest difference peak 1.278, deepest hole -0.429, 1-sigma level 0.099 Q1 1 0.8325 0.0861 0.0143 11.00000 0.05 1.28 Q2 1 0.8665 0.4215 0.0260 11.00000 0.05 1.18 ; _shelx_res_checksum 90817 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.012 _oxdiff_exptl_absorpt_empirical_full_min 0.617 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 S3 S 0.69468(10) 0.5287(3) 0.54952(7) 0.0326(5) Uani 1 1 d . . S2 S 0.68682(11) 0.5400(3) 0.30257(8) 0.0424(5) Uani 1 1 d . . S4 S 0.70870(11) 0.5736(3) 0.80814(7) 0.0360(5) Uani 1 1 d . . S1 S 0.71488(13) 0.3970(3) 0.07757(9) 0.0498(6) Uani 1 1 d . . O4 O 0.6792(3) 0.5878(9) 0.59875(19) 0.0429(14) Uani 1 1 d . . O6 O 0.6887(3) 0.6393(8) 0.8549(2) 0.0444(14) Uani 1 1 d . . O5 O 0.7232(3) 0.3503(8) 0.5466(2) 0.0429(14) Uani 1 1 d . . O7 O 0.7407(3) 0.3974(8) 0.8090(2) 0.0424(13) Uani 1 1 d . . O2 O 0.6720(3) 0.6105(10) 0.3508(2) 0.0569(18) Uani 1 1 d . . N00A N 0.7593(3) 0.6680(9) 0.5389(2) 0.0319(14) Uani 1 1 d . . O00B O 0.7520(4) 0.5684(11) 0.0858(3) 0.072(2) Uani 1 1 d . . O3 O 0.7152(4) 0.3600(9) 0.3027(3) 0.0594(18) Uani 1 1 d . . O1 O 0.6875(4) 0.3218(11) 0.1200(3) 0.064(2) Uani 1 1 d . . N00E N 0.7505(4) 0.6757(9) 0.2891(3) 0.0364(15) Uani 1 1 d . . N00F N 0.7719(4) 0.7177(9) 0.7979(2) 0.0329(14) Uani 1 1 d . . C30 C 0.8560(5) 0.4906(12) 0.2692(3) 0.0409(19) Uani 1 1 d . . N00H N 0.7757(4) 0.2575(10) 0.0633(3) 0.0434(17) Uani 1 1 d . . C48 C 0.8528(4) 0.4799(10) 0.5048(3) 0.0319(16) Uani 1 1 d . . C23 C 0.5983(4) 0.5548(12) 0.2486(3) 0.0392(18) Uani 1 1 d . . C44 C 0.7459(4) 0.8689(11) 0.5454(3) 0.0361(18) Uani 1 1 d . . H44 H 0.688916 0.893578 0.538999 0.043 Uiso 1 1 calc R . C37 C 0.4650(4) 0.5553(13) 0.4123(3) 0.0396(18) Uani 1 1 d . . C65 C 0.8029(4) 0.6933(11) 0.7500(3) 0.0316(16) Uani 1 1 d . . H65 H 0.758297 0.686267 0.715544 0.038 Uiso 1 1 calc R . C47 C 0.7959(4) 0.6336(11) 0.4947(3) 0.0326(17) Uani 1 1 d . . H47 H 0.753768 0.612013 0.459657 0.039 Uiso 1 1 calc R . C59 C 0.6220(5) 0.4924(12) 0.7039(3) 0.044(2) Uani 1 1 d . . H59 H 0.668662 0.440806 0.699778 0.052 Uiso 1 1 calc R . C58 C 0.6232(4) 0.5765(12) 0.7525(3) 0.0344(16) Uani 1 1 d . . C62 C 0.7611(5) 0.9144(12) 0.8071(3) 0.0387(18) Uani 1 1 d . . H62 H 0.704396 0.941261 0.801402 0.046 Uiso 1 1 calc R . C40 C 0.6066(4) 0.5468(11) 0.4962(3) 0.0313(16) Uani 1 1 d . . C20 C 0.4579(5) 0.5727(13) 0.1646(3) 0.045(2) Uani 1 1 d . . C41 C 0.6019(5) 0.4743(12) 0.4458(3) 0.0395(19) Uani 1 1 d . . H41 H 0.646682 0.420299 0.439538 0.047 Uiso 1 1 calc R . C66 C 0.8564(4) 0.5319(10) 0.7536(3) 0.0303(15) Uani 1 1 d . . C53 C 0.9040(4) 0.4498(12) 0.5566(3) 0.0380(18) Uani 1 1 d . . H53 H 0.900361 0.520459 0.586713 0.046 Uiso 1 1 calc R . C3 C 0.5007(6) 0.3298(14) -0.0306(4) 0.057(2) Uani 1 1 d . . H3 H 0.453262 0.269639 -0.031807 0.068 Uiso 1 1 calc R . C71 C 0.8530(5) 0.4384(11) 0.7061(3) 0.0377(17) Uani 1 1 d . . H71 H 0.813692 0.469098 0.673293 0.045 Uiso 1 1 calc R . C69 C 0.9623(5) 0.2586(13) 0.7523(4) 0.050(2) Uani 1 1 d . . H69 H 0.999444 0.166846 0.751950 0.060 Uiso 1 1 calc R . C55 C 0.4836(5) 0.5564(12) 0.6662(3) 0.0419(19) Uani 1 1 d . . C29 C 0.7892(4) 0.6195(13) 0.2481(3) 0.043(2) Uani 1 1 d . . H29 H 0.749658 0.565613 0.215669 0.052 Uiso 1 1 calc R . C67 C 0.9136(4) 0.4847(12) 0.8007(3) 0.0395(19) Uani 1 1 d . . H67 H 0.916905 0.546612 0.833775 0.047 Uiso 1 1 calc R . C012 C 0.5913(5) 0.4666(13) 0.2004(4) 0.048(2) Uani 1 1 d . . H012 H 0.633580 0.396978 0.195843 0.058 Uiso 1 1 calc R . C21 C 0.4655(5) 0.6595(13) 0.2133(4) 0.046(2) Uani 1 1 d . . H21 H 0.422316 0.725508 0.217942 0.055 Uiso 1 1 calc R . C46 C 0.8338(4) 0.8196(12) 0.4922(3) 0.0404(19) Uani 1 1 d . . H46A H 0.884009 0.831676 0.521599 0.048 Uiso 1 1 calc R . H46B H 0.843246 0.838047 0.456523 0.048 Uiso 1 1 calc R . C64 C 0.8462(4) 0.8747(11) 0.7521(3) 0.0347(17) Uani 1 1 d . . H64A H 0.896880 0.874422 0.781322 0.042 Uiso 1 1 calc R . H64B H 0.855491 0.901847 0.716769 0.042 Uiso 1 1 calc R . C56 C 0.4858(5) 0.6424(12) 0.7157(4) 0.045(2) Uani 1 1 d . . H56 H 0.439155 0.692269 0.720251 0.054 Uiso 1 1 calc R . C45 C 0.7736(5) 0.9536(13) 0.5002(4) 0.044(2) Uani 1 1 d . . H45A H 0.729524 0.967200 0.466257 0.053 Uiso 1 1 calc R . H45B H 0.797506 1.074005 0.511301 0.053 Uiso 1 1 calc R . C63 C 0.7891(5) 1.0102(11) 0.7644(3) 0.0376(17) Uani 1 1 d . . H63A H 0.815748 1.125462 0.778723 0.045 Uiso 1 1 calc R . H63B H 0.744946 1.035954 0.731366 0.045 Uiso 1 1 calc R . C42 C 0.5318(5) 0.4802(12) 0.4043(3) 0.042(2) Uani 1 1 d . . H42 H 0.529413 0.431710 0.369587 0.050 Uiso 1 1 calc R . C68 C 0.9665(5) 0.3472(14) 0.8003(4) 0.051(2) Uani 1 1 d . . H68 H 1.005550 0.314456 0.832997 0.061 Uiso 1 1 calc R . C51 C 0.9664(5) 0.2109(14) 0.5197(5) 0.060(3) Uani 1 1 d . . H51 H 1.004961 0.118479 0.524686 0.072 Uiso 1 1 calc R . C52 C 0.9606(5) 0.3155(13) 0.5640(4) 0.051(2) Uani 1 1 d . . H52 H 0.995738 0.294243 0.599285 0.062 Uiso 1 1 calc R . C25 C 0.7374(5) 0.8741(13) 0.2892(4) 0.045(2) Uani 1 1 d . . H25 H 0.681424 0.898757 0.286675 0.054 Uiso 1 1 calc R . C38 C 0.4700(4) 0.6276(11) 0.4633(3) 0.0386(18) Uani 1 1 d . . H38 H 0.424523 0.677248 0.469630 0.046 Uiso 1 1 calc R . C32 C 0.9385(6) 0.2543(16) 0.2528(6) 0.073(4) Uani 1 1 d . . H32 H 0.951546 0.172780 0.228125 0.088 Uiso 1 1 calc R . C6 C 0.6391(6) 0.5105(13) -0.0263(4) 0.052(2) Uani 1 1 d . . H6 H 0.685683 0.574947 -0.024710 0.062 Uiso 1 1 calc R . C50 C 0.9150(6) 0.2449(14) 0.4688(5) 0.058(3) Uani 1 1 d . . H50 H 0.918324 0.175316 0.438404 0.069 Uiso 1 1 calc R . C39 C 0.5403(4) 0.6285(11) 0.5051(3) 0.0358(17) Uani 1 1 d . . H39 H 0.543594 0.683474 0.539174 0.043 Uiso 1 1 calc R . C49 C 0.8593(5) 0.3773(13) 0.4614(3) 0.0418(19) Uani 1 1 d . . H49 H 0.824651 0.398853 0.425966 0.050 Uiso 1 1 calc R . C31 C 0.8756(5) 0.3638(15) 0.2344(4) 0.058(3) Uani 1 1 d . . H31 H 0.844099 0.355062 0.197480 0.069 Uiso 1 1 calc R . C60 C 0.5543(5) 0.4838(13) 0.6621(3) 0.044(2) Uani 1 1 d . . H60 H 0.554756 0.426793 0.628953 0.053 Uiso 1 1 calc R . C61 C 0.8092(5) 0.9685(12) 0.8650(3) 0.047(2) Uani 1 1 d . . H61A H 0.796515 0.887412 0.891400 0.070 Uiso 1 1 calc GR . H61B H 0.796809 1.093834 0.872120 0.070 Uiso 1 1 calc GR . H61C H 0.865155 0.958847 0.868462 0.070 Uiso 1 1 calc GR . C70 C 0.9057(5) 0.3005(12) 0.7054(4) 0.049(2) Uani 1 1 d . . H70 H 0.902258 0.236639 0.672640 0.058 Uiso 1 1 calc R . C5 C 0.6341(5) 0.4092(13) 0.0182(4) 0.047(2) Uani 1 1 d . . C4 C 0.5652(5) 0.3183(13) 0.0170(4) 0.052(2) Uani 1 1 d . . H4 H 0.561727 0.249962 0.047574 0.062 Uiso 1 1 calc R . C43 C 0.7919(5) 0.9297(14) 0.6012(3) 0.049(2) Uani 1 1 d . . H43A H 0.772582 0.867411 0.628428 0.073 Uiso 1 1 calc GR . H43B H 0.785835 1.061051 0.604380 0.073 Uiso 1 1 calc GR . H43C H 0.847313 0.900604 0.607522 0.073 Uiso 1 1 calc GR . C2 C 0.5057(6) 0.4272(15) -0.0752(4) 0.058(3) Uani 1 1 d . . C35 C 0.9027(5) 0.4917(13) 0.3236(3) 0.045(2) Uani 1 1 d . . H35 H 0.890963 0.573944 0.348540 0.053 Uiso 1 1 calc R . C36 C 0.3881(5) 0.5443(16) 0.3677(4) 0.055(2) Uani 1 1 d . . H36A H 0.397667 0.549994 0.332096 0.082 Uiso 1 1 calc GR . H36B H 0.354698 0.646065 0.371241 0.082 Uiso 1 1 calc GR . H36C H 0.362059 0.429699 0.370897 0.082 Uiso 1 1 calc GR . C7 C 0.5749(6) 0.5169(15) -0.0733(4) 0.061(3) Uani 1 1 d . . H7 H 0.578556 0.582912 -0.104289 0.074 Uiso 1 1 calc R . C22 C 0.5357(5) 0.6527(12) 0.2562(4) 0.0424(19) Uani 1 1 d . . H22 H 0.540473 0.713497 0.289685 0.051 Uiso 1 1 calc R . C54 C 0.4080(5) 0.5340(15) 0.6212(4) 0.054(2) Uani 1 1 d . . H54A H 0.387448 0.411438 0.622731 0.081 Uiso 1 1 calc GR . H54B H 0.417392 0.552310 0.585879 0.081 Uiso 1 1 calc GR . H54C H 0.369875 0.623463 0.625732 0.081 Uiso 1 1 calc GR . C19 C 0.3821(6) 0.5782(18) 0.1186(4) 0.067(3) Uani 1 1 d . . H19A H 0.347085 0.668668 0.126817 0.100 Uiso 1 1 calc GR . H19B H 0.357108 0.458564 0.114640 0.100 Uiso 1 1 calc GR . H19C H 0.392977 0.610812 0.084571 0.100 Uiso 1 1 calc GR . C33 C 0.9838(6) 0.2583(15) 0.3061(5) 0.065(3) Uani 1 1 d . . H33 H 1.027668 0.179668 0.318137 0.078 Uiso 1 1 calc R . C57 C 0.5546(5) 0.6550(12) 0.7574(3) 0.0403(19) Uani 1 1 d . . H57 H 0.555482 0.717660 0.789941 0.048 Uiso 1 1 calc R . C34 C 0.9663(5) 0.3741(15) 0.3418(4) 0.057(2) Uani 1 1 d . . H34 H 0.997137 0.375198 0.379007 0.068 Uiso 1 1 calc R . C27 C 0.7538(6) 0.9390(15) 0.2374(4) 0.060(3) Uani 1 1 d . . H27A H 0.773398 1.065389 0.241204 0.072 Uiso 1 1 calc R . H27B H 0.706383 0.930908 0.205447 0.072 Uiso 1 1 calc R . C24 C 0.5209(5) 0.4804(14) 0.1580(4) 0.054(2) Uani 1 1 d . . H24 H 0.516837 0.424472 0.123893 0.065 Uiso 1 1 calc R . C28 C 0.8172(5) 0.8047(15) 0.2326(4) 0.061(3) Uani 1 1 d . . H28A H 0.868977 0.837463 0.257954 0.073 Uiso 1 1 calc R . H28B H 0.821055 0.802161 0.194885 0.073 Uiso 1 1 calc R . C9 C 0.7669(6) 0.0568(16) 0.0729(5) 0.064(3) Uani 1 1 d D . H9 H 0.733277 0.031241 0.096972 0.077 Uiso 1 1 calc R . C26 C 0.7905(7) 0.9576(17) 0.3409(4) 0.074(3) Uani 1 1 d . . H26A H 0.783112 0.894853 0.372698 0.112 Uiso 1 1 calc GR . H26B H 0.777499 1.086361 0.342388 0.112 Uiso 1 1 calc GR . H26C H 0.845151 0.945769 0.341173 0.112 Uiso 1 1 calc GR . C1 C 0.4386(8) 0.4341(19) -0.1258(5) 0.081(4) Uani 1 1 d . . H1A H 0.403920 0.330473 -0.126690 0.122 Uiso 1 1 calc GR . H1B H 0.458116 0.429365 -0.157656 0.122 Uiso 1 1 calc GR . H1C H 0.409425 0.547202 -0.126603 0.122 Uiso 1 1 calc GR . C15 C 0.8748(5) 0.5699(14) -0.0403(2) 0.103(4) Uani 1 1 d . U H15 H 0.847865 0.578322 -0.078159 0.124 Uiso 1 1 calc R . C16 C 0.9386(5) 0.6820(13) -0.0171(3) 0.097(4) Uani 1 1 d G U H16 H 0.955194 0.767011 -0.039224 0.116 Uiso 1 1 calc R . C17 C 0.9780(4) 0.6697(12) 0.0383(3) 0.083(3) Uani 1 1 d G U H17 H 1.021533 0.746324 0.054084 0.100 Uiso 1 1 calc R . C18 C 0.9536(5) 0.5453(14) 0.0706(2) 0.087(4) Uani 1 1 d G U H18 H 0.980544 0.536947 0.108458 0.105 Uiso 1 1 calc R . C13 C 0.8899(5) 0.4333(12) 0.0474(3) 0.076(3) Uani 1 1 d G U C14 C 0.8504(4) 0.4455(13) -0.0080(3) 0.096(4) Uani 1 1 d G U H14 H 0.806875 0.368942 -0.023784 0.115 Uiso 1 1 calc R . C12 C 0.8621(7) 0.304(2) 0.0811(6) 0.091(4) Uani 1 1 d . . H12 H 0.877715 0.347563 0.119759 0.110 Uiso 1 1 calc R . C10 C 0.8447(8) -0.0126(19) 0.0941(9) 0.118(6) Uani 1 1 d . . H10A H 0.847555 -0.135741 0.079386 0.141 Uiso 1 1 calc R . H10B H 0.858906 -0.021137 0.134320 0.141 Uiso 1 1 calc R . C11 C 0.8993(8) 0.107(3) 0.0787(7) 0.118(6) Uani 1 1 d . . H11A H 0.901862 0.078887 0.041559 0.142 Uiso 1 1 calc R . H11B H 0.952544 0.097444 0.104862 0.142 Uiso 1 1 calc R . C8 C 0.7306(14) -0.022(4) 0.0112(8) 0.198(11) Uani 1 1 d D U H8A H 0.689963 0.060484 -0.009981 0.297 Uiso 1 1 calc GR . H8B H 0.707769 -0.142100 0.012770 0.297 Uiso 1 1 calc GR . H8C H 0.772340 -0.032182 -0.006184 0.297 Uiso 1 1 calc GR . 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 S3 0.0257(8) 0.0355(12) 0.0397(8) 0.0065(8) 0.0143(7) 0.0009(8) S2 0.0374(10) 0.0442(13) 0.0526(10) 0.0120(9) 0.0241(8) 0.0073(10) S4 0.0350(9) 0.0366(12) 0.0416(9) 0.0021(8) 0.0191(7) -0.0004(9) S1 0.0507(12) 0.0486(14) 0.0616(12) -0.0124(10) 0.0343(10) -0.0064(11) O4 0.036(3) 0.062(4) 0.035(2) 0.007(3) 0.017(2) -0.001(3) O6 0.050(3) 0.049(4) 0.042(3) -0.007(2) 0.025(3) -0.003(3) O5 0.029(3) 0.030(3) 0.074(4) 0.013(3) 0.022(3) 0.005(2) O7 0.036(3) 0.037(3) 0.058(3) 0.009(3) 0.019(2) 0.000(3) O2 0.051(3) 0.082(5) 0.047(3) 0.013(3) 0.028(3) 0.012(4) N00A 0.030(3) 0.032(4) 0.037(3) 0.003(3) 0.014(3) 0.003(3) O00B 0.077(5) 0.050(5) 0.107(6) -0.029(4) 0.054(4) -0.012(4) O3 0.043(3) 0.037(4) 0.108(5) 0.020(4) 0.037(3) 0.010(3) O1 0.052(4) 0.097(6) 0.055(4) -0.003(4) 0.033(3) -0.004(4) N00E 0.032(3) 0.038(4) 0.045(3) 0.008(3) 0.019(3) 0.005(3) N00F 0.037(3) 0.029(4) 0.037(3) -0.003(3) 0.018(3) 0.000(3) C30 0.034(4) 0.037(5) 0.061(5) 0.000(4) 0.028(4) -0.003(3) N00H 0.045(4) 0.044(5) 0.047(4) -0.006(3) 0.022(3) -0.001(3) C48 0.032(4) 0.027(4) 0.043(4) 0.006(3) 0.020(3) -0.007(3) C23 0.038(4) 0.037(5) 0.050(4) 0.000(4) 0.024(3) -0.001(4) C44 0.024(3) 0.034(5) 0.053(4) 0.003(3) 0.016(3) 0.002(3) C37 0.031(4) 0.040(5) 0.048(4) 0.004(4) 0.013(3) -0.009(4) C65 0.025(3) 0.038(5) 0.035(3) -0.001(3) 0.013(3) -0.001(3) C47 0.027(3) 0.039(5) 0.036(4) 0.002(3) 0.016(3) 0.003(3) C59 0.035(4) 0.047(6) 0.059(5) -0.005(4) 0.029(4) -0.010(4) C58 0.035(4) 0.030(4) 0.043(4) 0.000(3) 0.020(3) -0.001(4) C62 0.035(4) 0.039(5) 0.045(4) 0.000(3) 0.017(3) 0.006(4) C40 0.026(3) 0.029(4) 0.042(3) 0.003(3) 0.016(3) -0.003(3) C20 0.046(4) 0.040(5) 0.057(5) 0.007(4) 0.026(4) -0.015(4) C41 0.035(4) 0.044(5) 0.046(4) -0.007(4) 0.023(3) -0.004(4) C66 0.032(4) 0.025(4) 0.038(3) -0.002(3) 0.016(3) -0.006(3) C53 0.034(4) 0.034(5) 0.047(4) 0.003(3) 0.014(3) 0.004(4) C3 0.048(5) 0.043(6) 0.086(7) -0.001(5) 0.028(5) 0.000(5) C71 0.039(4) 0.033(5) 0.045(4) -0.003(3) 0.018(3) -0.004(4) C69 0.040(5) 0.033(5) 0.086(7) -0.006(4) 0.033(5) -0.006(4) C55 0.038(4) 0.035(5) 0.054(4) 0.005(4) 0.016(3) -0.010(4) C29 0.030(4) 0.057(6) 0.047(4) 0.002(4) 0.019(3) 0.001(4) C67 0.033(4) 0.037(5) 0.050(4) 0.001(4) 0.014(3) -0.001(4) C012 0.041(4) 0.048(6) 0.069(5) -0.007(4) 0.035(4) -0.002(4) C21 0.039(4) 0.041(5) 0.062(5) 0.013(4) 0.021(4) 0.008(4) C46 0.032(4) 0.040(5) 0.053(4) 0.014(4) 0.019(3) 0.003(4) C64 0.029(4) 0.034(5) 0.045(4) 0.006(3) 0.017(3) -0.001(3) C56 0.037(4) 0.036(5) 0.066(5) 0.003(4) 0.022(4) 0.001(4) C45 0.036(4) 0.035(5) 0.064(5) 0.013(4) 0.020(4) 0.004(4) C63 0.038(4) 0.023(4) 0.050(4) 0.007(3) 0.010(3) -0.002(3) C42 0.042(4) 0.045(5) 0.041(4) -0.010(4) 0.019(3) -0.016(4) C68 0.032(4) 0.051(6) 0.066(5) 0.010(4) 0.009(4) -0.001(4) C51 0.044(5) 0.038(6) 0.119(9) 0.004(5) 0.056(6) 0.006(4) C52 0.032(4) 0.042(6) 0.082(6) 0.019(5) 0.021(4) 0.009(4) C25 0.028(4) 0.046(6) 0.063(5) 0.010(4) 0.014(3) 0.007(4) C38 0.030(4) 0.032(5) 0.055(4) 0.007(3) 0.014(3) 0.004(3) C32 0.065(7) 0.055(7) 0.123(10) -0.038(7) 0.064(7) -0.003(6) C6 0.064(6) 0.039(5) 0.071(5) 0.004(4) 0.047(5) 0.005(4) C50 0.063(6) 0.041(6) 0.089(7) -0.007(5) 0.053(6) -0.011(5) C39 0.037(4) 0.029(5) 0.046(4) -0.001(3) 0.020(3) 0.002(3) C49 0.043(4) 0.043(5) 0.051(4) -0.007(4) 0.031(4) -0.012(4) C31 0.043(5) 0.066(7) 0.074(6) -0.031(5) 0.032(4) -0.017(5) C60 0.042(4) 0.054(6) 0.043(4) -0.010(4) 0.023(3) -0.016(4) C61 0.057(5) 0.035(5) 0.048(4) -0.007(4) 0.016(4) 0.002(4) C70 0.051(5) 0.034(5) 0.072(6) -0.013(4) 0.034(5) -0.007(4) C5 0.052(5) 0.037(5) 0.064(5) -0.007(4) 0.035(4) 0.000(4) C4 0.057(5) 0.047(6) 0.061(5) -0.001(4) 0.032(4) -0.003(5) C43 0.040(4) 0.049(6) 0.054(5) -0.004(4) 0.010(4) 0.000(4) C2 0.058(6) 0.056(7) 0.065(6) -0.004(5) 0.027(5) 0.024(5) C35 0.036(4) 0.050(6) 0.053(4) 0.006(4) 0.021(4) 0.008(4) C36 0.038(4) 0.060(7) 0.060(5) 0.010(5) 0.005(4) -0.005(5) C7 0.073(6) 0.055(7) 0.069(6) 0.006(5) 0.041(5) 0.023(6) C22 0.041(4) 0.038(5) 0.054(5) -0.003(4) 0.024(4) -0.001(4) C54 0.045(5) 0.054(6) 0.058(5) 0.007(5) 0.009(4) -0.012(5) C19 0.061(6) 0.073(8) 0.064(6) 0.013(6) 0.016(5) -0.023(6) C33 0.047(5) 0.050(7) 0.106(9) 0.006(6) 0.034(6) 0.006(5) C57 0.044(4) 0.034(5) 0.051(4) 0.000(4) 0.027(4) 0.003(4) C34 0.043(5) 0.061(7) 0.070(6) 0.015(5) 0.022(4) 0.011(5) C27 0.054(5) 0.045(6) 0.085(7) 0.028(5) 0.026(5) 0.004(5) C24 0.051(5) 0.063(7) 0.054(5) -0.010(4) 0.026(4) -0.024(5) C28 0.045(5) 0.063(7) 0.082(7) 0.027(5) 0.031(5) 0.002(5) C9 0.047(5) 0.052(7) 0.092(7) 0.014(6) 0.020(5) 0.000(5) C26 0.068(7) 0.064(8) 0.072(6) -0.010(6) -0.008(5) 0.019(6) C1 0.101(9) 0.065(8) 0.077(7) -0.020(6) 0.024(6) 0.026(7) C15 0.103(5) 0.103(5) 0.103(4) 0.0005(14) 0.0307(18) 0.0009(14) C16 0.097(4) 0.097(4) 0.097(4) 0.0006(14) 0.0305(18) 0.0009(14) C17 0.082(4) 0.083(4) 0.085(4) -0.0009(14) 0.0262(17) 0.0001(14) C18 0.088(4) 0.087(4) 0.087(4) -0.0007(14) 0.0267(17) 0.0022(14) C13 0.076(3) 0.077(3) 0.078(3) 0.0011(14) 0.0268(16) 0.0003(14) C14 0.095(4) 0.096(4) 0.097(4) -0.0010(14) 0.0287(18) 0.0008(14) C12 0.071(7) 0.118(12) 0.090(8) 0.034(8) 0.033(6) 0.004(8) C10 0.070(8) 0.052(9) 0.235(19) 0.021(10) 0.052(11) -0.013(7) C11 0.087(9) 0.125(15) 0.150(14) 0.052(12) 0.047(9) 0.052(10) C8 0.206(12) 0.185(13) 0.192(12) -0.004(7) 0.043(7) 0.006(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 '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 O4 S3 N00A 106.7(3) O4 S3 C40 107.4(3) O5 S3 O4 119.5(4) O5 S3 N00A 106.9(3) O5 S3 C40 106.4(4) N00A S3 C40 109.8(3) O2 S2 N00E 106.3(4) O2 S2 C23 107.5(4) O3 S2 O2 119.5(4) O3 S2 N00E 107.5(3) O3 S2 C23 107.2(4) N00E S2 C23 108.4(4) O6 S4 N00F 105.8(3) O6 S4 C58 107.6(3) O7 S4 O6 119.8(4) O7 S4 N00F 107.7(3) O7 S4 C58 105.9(4) N00F S4 C58 109.9(3) O00B S1 O1 118.9(5) O00B S1 N00H 106.6(4) O00B S1 C5 108.2(5) O1 S1 N00H 109.4(4) O1 S1 C5 107.4(4) N00H S1 C5 105.7(4) C44 N00A S3 117.0(5) C47 N00A S3 120.9(5) C47 N00A C44 111.6(6) C29 N00E S2 118.9(6) C29 N00E C25 112.7(6) C25 N00E S2 118.9(5) C65 N00F S4 119.8(5) C62 N00F S4 118.7(5) C62 N00F C65 110.0(6) C31 C30 C29 121.1(8) C35 C30 C29 122.2(7) C35 C30 C31 116.7(8) C9 N00H S1 118.4(6) C12 N00H S1 118.9(8) C12 N00H C9 108.5(8) C53 C48 C47 120.5(7) C49 C48 C47 119.6(7) C49 C48 C53 119.6(8) C012 C23 S2 119.8(6) C012 C23 C22 120.7(8) C22 C23 S2 119.5(6) N00A C44 H44 110.2 N00A C44 C45 102.7(6) C45 C44 H44 110.2 C43 C44 N00A 109.8(7) C43 C44 H44 110.2 C43 C44 C45 113.4(7) C42 C37 C38 118.3(7) C42 C37 C36 120.0(8) C38 C37 C36 121.6(7) N00F C65 H65 109.7 N00F C65 C66 115.1(6) N00F C65 C64 99.8(6) C66 C65 H65 109.7 C66 C65 C64 112.3(5) C64 C65 H65 109.7 N00A C47 C48 115.4(6) N00A C47 H47 109.1 N00A C47 C46 100.2(6) C48 C47 H47 109.1 C48 C47 C46 113.5(6) C46 C47 H47 109.1 C58 C59 H59 120.0 C60 C59 H59 120.0 C60 C59 C58 120.1(7) C59 C58 S4 120.1(6) C59 C58 C57 119.3(7) C57 C58 S4 120.5(6) N00F C62 H62 110.0 N00F C62 C63 104.7(6) N00F C62 C61 110.1(7) C63 C62 H62 110.0 C63 C62 C61 111.7(7) C61 C62 H62 110.0 C41 C40 S3 119.5(6) C41 C40 C39 119.8(7) C39 C40 S3 120.6(6) C21 C20 C19 121.4(9) C24 C20 C21 118.8(8) C24 C20 C19 119.8(9) C40 C41 H41 120.0 C40 C41 C42 119.9(7) C42 C41 H41 120.0 C71 C66 C65 118.4(6) C67 C66 C65 123.0(6) C67 C66 C71 118.2(7) C48 C53 H53 120.3 C52 C53 C48 119.3(8) C52 C53 H53 120.3 C4 C3 H3 119.5 C2 C3 H3 119.5 C2 C3 C4 120.9(9) C66 C71 H71 119.2 C66 C71 C70 121.5(8) C70 C71 H71 119.2 C68 C69 H69 119.6 C70 C69 H69 119.6 C70 C69 C68 120.9(9) C56 C55 C54 121.3(8) C60 C55 C56 117.1(7) C60 C55 C54 121.5(8) N00E C29 C30 114.4(6) N00E C29 H29 109.8 N00E C29 C28 101.1(7) C30 C29 H29 109.8 C30 C29 C28 111.6(6) C28 C29 H29 109.8 C66 C67 H67 119.7 C66 C67 C68 120.5(8) C68 C67 H67 119.7 C23 C012 H012 120.4 C23 C012 C24 119.1(8) C24 C012 H012 120.4 C20 C21 H21 119.3 C20 C21 C22 121.4(8) C22 C21 H21 119.3 C47 C46 H46A 111.0 C47 C46 H46B 111.0 H46A C46 H46B 109.0 C45 C46 C47 103.6(6) C45 C46 H46A 111.0 C45 C46 H46B 111.0 C65 C64 H64A 111.3 C65 C64 H64B 111.3 H64A C64 H64B 109.2 C63 C64 C65 102.4(5) C63 C64 H64A 111.3 C63 C64 H64B 111.3 C55 C56 H56 119.6 C57 C56 C55 120.8(8) C57 C56 H56 119.6 C44 C45 H45A 111.0 C44 C45 H45B 111.0 C46 C45 C44 103.9(7) C46 C45 H45A 111.0 C46 C45 H45B 111.0 H45A C45 H45B 109.0 C62 C63 C64 103.4(6) C62 C63 H63A 111.1 C62 C63 H63B 111.1 C64 C63 H63A 111.1 C64 C63 H63B 111.1 H63A C63 H63B 109.1 C37 C42 H42 119.2 C41 C42 C37 121.6(7) C41 C42 H42 119.2 C69 C68 C67 119.8(8) C69 C68 H68 120.1 C67 C68 H68 120.1 C52 C51 H51 120.7 C50 C51 H51 120.7 C50 C51 C52 118.6(9) C53 C52 C51 120.6(9) C53 C52 H52 119.7 C51 C52 H52 119.7 N00E C25 H25 109.6 N00E C25 C27 103.7(7) N00E C25 C26 110.1(7) C27 C25 H25 109.6 C26 C25 H25 109.6 C26 C25 C27 113.9(9) C37 C38 H38 119.3 C39 C38 C37 121.3(7) C39 C38 H38 119.3 C31 C32 H32 119.3 C31 C32 C33 121.3(9) C33 C32 H32 119.3 C5 C6 H6 120.3 C5 C6 C7 119.4(9) C7 C6 H6 120.3 C51 C50 H50 119.5 C49 C50 C51 120.9(9) C49 C50 H50 119.5 C40 C39 H39 120.5 C38 C39 C40 119.0(7) C38 C39 H39 120.5 C48 C49 H49 119.6 C50 C49 C48 120.9(9) C50 C49 H49 119.6 C30 C31 H31 119.5 C32 C31 C30 121.0(10) C32 C31 H31 119.5 C59 C60 C55 122.1(7) C59 C60 H60 118.9 C55 C60 H60 118.9 C62 C61 H61A 109.5 C62 C61 H61B 109.5 C62 C61 H61C 109.5 H61A C61 H61B 109.5 H61A C61 H61C 109.5 H61B C61 H61C 109.5 C71 C70 H70 120.5 C69 C70 C71 119.0(8) C69 C70 H70 120.5 C6 C5 S1 120.1(7) C6 C5 C4 120.9(9) C4 C5 S1 119.0(7) C3 C4 H4 120.7 C5 C4 C3 118.6(9) C5 C4 H4 120.7 C44 C43 H43A 109.5 C44 C43 H43B 109.5 C44 C43 H43C 109.5 H43A C43 H43B 109.5 H43A C43 H43C 109.5 H43B C43 H43C 109.5 C3 C2 C7 119.8(9) C3 C2 C1 120.8(10) C7 C2 C1 119.4(10) C30 C35 H35 119.5 C34 C35 C30 121.1(8) C34 C35 H35 119.5 C37 C36 H36A 109.5 C37 C36 H36B 109.5 C37 C36 H36C 109.5 H36A C36 H36B 109.5 H36A C36 H36C 109.5 H36B C36 H36C 109.5 C6 C7 H7 119.8 C2 C7 C6 120.4(9) C2 C7 H7 119.8 C23 C22 C21 118.5(8) C23 C22 H22 120.8 C21 C22 H22 120.8 C55 C54 H54A 109.5 C55 C54 H54B 109.5 C55 C54 H54C 109.5 H54A C54 H54B 109.5 H54A C54 H54C 109.5 H54B C54 H54C 109.5 C20 C19 H19A 109.5 C20 C19 H19B 109.5 C20 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C32 C33 H33 119.9 C34 C33 C32 120.2(10) C34 C33 H33 119.9 C58 C57 H57 119.7 C56 C57 C58 120.6(8) C56 C57 H57 119.7 C35 C34 H34 120.2 C33 C34 C35 119.6(10) C33 C34 H34 120.2 C25 C27 H27A 111.4 C25 C27 H27B 111.4 C25 C27 C28 101.9(7) H27A C27 H27B 109.3 C28 C27 H27A 111.4 C28 C27 H27B 111.4 C20 C24 C012 121.4(8) C20 C24 H24 119.3 C012 C24 H24 119.3 C29 C28 H28A 110.9 C29 C28 H28B 110.9 C27 C28 C29 104.1(7) C27 C28 H28A 110.9 C27 C28 H28B 110.9 H28A C28 H28B 109.0 N00H C9 H9 113.2 N00H C9 C8 102.8(12) C10 C9 N00H 105.9(9) C10 C9 H9 113.2 C10 C9 C8 107.6(14) C8 C9 H9 113.2 C25 C26 H26A 109.5 C25 C26 H26B 109.5 C25 C26 H26C 109.5 H26A C26 H26B 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C2 C1 H1A 109.5 C2 C1 H1B 109.5 C2 C1 H1C 109.5 H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C16 C15 H15 120.0 C16 C15 C14 120.0 C14 C15 H15 120.0 C15 C16 H16 120.0 C17 C16 C15 120.0 C17 C16 H16 120.0 C16 C17 H17 120.0 C16 C17 C18 120.0 C18 C17 H17 120.0 C17 C18 H18 120.0 C13 C18 C17 120.0 C13 C18 H18 120.0 C18 C13 C12 120.8(8) C14 C13 C18 120.0 C14 C13 C12 119.2(8) C15 C14 H14 120.0 C13 C14 C15 120.0 C13 C14 H14 120.0 N00H C12 H12 109.4 N00H C12 C11 100.5(11) C13 C12 N00H 117.5(10) C13 C12 H12 109.4 C13 C12 C11 110.3(10) C11 C12 H12 109.4 C9 C10 H10A 109.7 C9 C10 H10B 109.7 C9 C10 C11 109.7(12) H10A C10 H10B 108.2 C11 C10 H10A 109.7 C11 C10 H10B 109.7 C12 C11 H11A 111.3 C12 C11 H11B 111.3 C10 C11 C12 102.5(11) C10 C11 H11A 111.3 C10 C11 H11B 111.3 H11A C11 H11B 109.2 C9 C8 H8A 109.5 C9 C8 H8B 109.5 C9 C8 H8C 109.5 H8A C8 H8B 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S3 O4 1.439(5) S3 O5 1.420(6) S3 N00A 1.628(6) S3 C40 1.757(7) S2 O2 1.438(6) S2 O3 1.421(7) S2 N00E 1.629(7) S2 C23 1.769(8) S4 O6 1.435(5) S4 O7 1.417(6) S4 N00F 1.628(7) S4 C58 1.755(8) S1 O00B 1.414(8) S1 O1 1.432(6) S1 N00H 1.615(7) S1 C5 1.764(10) N00A C44 1.516(11) N00A C47 1.492(8) N00E C29 1.479(9) N00E C25 1.481(12) N00F C65 1.505(8) N00F C62 1.490(11) C30 C29 1.496(12) C30 C31 1.406(12) C30 C35 1.398(12) N00H C9 1.516(13) N00H C12 1.515(14) C48 C47 1.492(10) C48 C53 1.391(11) C48 C49 1.379(11) C23 C012 1.370(12) C23 C22 1.392(11) C44 H44 1.0000 C44 C45 1.524(11) C44 C43 1.493(11) C37 C42 1.386(12) C37 C38 1.391(11) C37 C36 1.505(10) C65 H65 1.0000 C65 C66 1.511(10) C65 C64 1.538(11) C47 H47 1.0000 C47 C46 1.539(11) C59 H59 0.9500 C59 C58 1.388(11) C59 C60 1.360(11) C58 C57 1.396(11) C62 H62 1.0000 C62 C63 1.508(11) C62 C61 1.532(11) C40 C41 1.380(10) C40 C39 1.408(10) C20 C21 1.374(13) C20 C19 1.509(12) C20 C24 1.369(13) C41 H41 0.9500 C41 C42 1.382(11) C66 C71 1.385(10) C66 C67 1.376(11) C53 H53 0.9500 C53 C52 1.388(11) C3 H3 0.9500 C3 C4 1.409(13) C3 C2 1.376(14) C71 H71 0.9500 C71 C70 1.390(12) C69 H69 0.9500 C69 C68 1.376(13) C69 C70 1.356(13) C55 C56 1.409(12) C55 C60 1.406(12) C55 C54 1.504(11) C29 H29 1.0000 C29 C28 1.547(13) C67 H67 0.9500 C67 C68 1.389(12) C012 H012 0.9500 C012 C24 1.402(13) C21 H21 0.9500 C21 C22 1.404(12) C46 H46A 0.9900 C46 H46B 0.9900 C46 C45 1.519(11) C64 H64A 0.9900 C64 H64B 0.9900 C64 C63 1.527(11) C56 H56 0.9500 C56 C57 1.372(12) C45 H45A 0.9900 C45 H45B 0.9900 C63 H63A 0.9900 C63 H63B 0.9900 C42 H42 0.9500 C68 H68 0.9500 C51 H51 0.9500 C51 C52 1.402(15) C51 C50 1.379(15) C52 H52 0.9500 C25 H25 1.0000 C25 C27 1.521(12) C25 C26 1.515(13) C38 H38 0.9500 C38 C39 1.389(11) C32 H32 0.9500 C32 C31 1.351(15) C32 C33 1.368(16) C6 H6 0.9500 C6 C5 1.388(12) C6 C7 1.397(14) C50 H50 0.9500 C50 C49 1.366(13) C39 H39 0.9500 C49 H49 0.9500 C31 H31 0.9500 C60 H60 0.9500 C61 H61A 0.9800 C61 H61B 0.9800 C61 H61C 0.9800 C70 H70 0.9500 C5 C4 1.395(12) C4 H4 0.9500 C43 H43A 0.9800 C43 H43B 0.9800 C43 H43C 0.9800 C2 C7 1.393(15) C2 C1 1.485(15) C35 H35 0.9500 C35 C34 1.395(12) C36 H36A 0.9800 C36 H36B 0.9800 C36 H36C 0.9800 C7 H7 0.9500 C22 H22 0.9500 C54 H54A 0.9800 C54 H54B 0.9800 C54 H54C 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C33 H33 0.9500 C33 C34 1.356(15) C57 H57 0.9500 C34 H34 0.9500 C27 H27A 0.9900 C27 H27B 0.9900 C27 C28 1.539(14) C24 H24 0.9500 C28 H28A 0.9900 C28 H28B 0.9900 C9 H9 1.0000 C9 C10 1.430(17) C9 C8 1.629(19) C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C1 H1A 0.9800 C1 H1B 0.9800 C1 H1C 0.9800 C15 H15 0.9500 C15 C16 1.3900 C15 C14 1.3900 C16 H16 0.9500 C16 C17 1.3900 C17 H17 0.9500 C17 C18 1.3900 C18 H18 0.9500 C18 C13 1.3900 C13 C14 1.3900 C13 C12 1.469(13) C14 H14 0.9500 C12 H12 1.0000 C12 C11 1.61(2) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.453(19) C11 H11A 0.9900 C11 H11B 0.9900 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800