#------------------------------------------------------------------------------ #$Date: 2016-03-22 21:53:30 +0200 (Tue, 22 Mar 2016) $ #$Revision: 179027 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/12/25/4122504.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_4122504 loop_ _publ_author_name 'Cherney, Emily C.' 'Lopchuk, Justin M.' 'Green, Jason C.' 'Baran, Phil S.' _publ_section_title ; A unified approach to ent-atisane diterpenes and related alkaloids: synthesis of (-)-methyl atisenoate, (-)-isoatisine, and the hetidine skeleton. ; _journal_issue 36 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 12592 _journal_page_last 12595 _journal_paper_doi 10.1021/ja507321j _journal_volume 136 _journal_year 2014 _chemical_absolute_configuration ad _chemical_formula_moiety 'C21 H30 O3' _chemical_formula_sum 'C21 H30 O3' _chemical_formula_weight 330.45 _chemical_name_systematic ECC-9-020-1 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary dimap _audit_creation_date 2013-11-04 _audit_creation_method ; Olex2 1.2-beta (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.3107(3) _cell_length_b 9.0733(3) _cell_length_c 26.4224(10) _cell_measurement_reflns_used 8115 _cell_measurement_temperature 100 _cell_measurement_theta_max 68.255 _cell_measurement_theta_min 3.345 _cell_volume 1752.66(11) _computing_cell_refinement 'Bruker Saint' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker Saint' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _diffrn_ambient_temperature 100.0 _diffrn_detector 'Bruker APEX CCD' _diffrn_detector_area_resol_mean 8.0 _diffrn_detector_type 'CCD Area Detector' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device 'Kappa Four-Circle Diffractometer' _diffrn_measurement_device_type 'Bruker X8 APEX' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Double Bounce Multilayer Mirrors' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_xray_symbol K-L~3~ _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 11352 _diffrn_reflns_point_group_measured_fraction_full 0.985 _diffrn_reflns_point_group_measured_fraction_max 0.984 _diffrn_reflns_theta_full 68.000 _diffrn_reflns_theta_max 68.250 _diffrn_reflns_theta_min 3.345 _diffrn_source 'Micro Focus Rotating Anode' _diffrn_source_type 'Bruker FR-591' _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.643 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.6619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1239 before and 0.0376 after correction. The Ratio of minimum to maximum transmission is 0.8789. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour Colorless _exptl_crystal_colour_primary Colorless _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'Not measured' _exptl_crystal_description plate _exptl_crystal_F_000 720 _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.184 _refine_diff_density_min -0.135 _refine_diff_density_rms 0.030 _refine_ls_abs_structure_details ; Flack x determined using 1279 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.00(5) _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 220 _refine_ls_number_reflns 3152 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0270 _refine_ls_R_factor_gt 0.0263 _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^)+(0.0340P)^2^+0.4395P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0679 _refine_ls_wR_factor_ref 0.0687 _reflns_Friedel_coverage 0.701 _reflns_Friedel_fraction_full 0.977 _reflns_Friedel_fraction_max 0.976 _reflns_number_gt 3093 _reflns_number_total 3152 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja507321j_si_003.cif _cod_data_source_block Baran336 _cod_depositor_comments ; The following automatic conversions were performed: '_chemical_absolute_configuration' value 'AD' changed to 'ad' according to /home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. '_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according to /home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26. Automatic conversion script Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius Adding full bibliography for 4122504--4122507.cif. ; _cod_database_code 4122504 #BEGIN Tags that were not found in dictionaries: _shelxl_version_number 2013-3 _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 0.975 _shelx_estimated_absorpt_t_min 0.893 _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.a Ternary CH refined with riding coordinates: C6(H6), C12(H12), C14(H14) 2.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A, H10B), C13(H13A,H13B), C16(H16A,H16B) 2.c X=CH2 refined with riding coordinates: C21(H21A,H21B) 2.d Idealised Me refined as rotating group: C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C) ; _shelx_res_file ; TITL baran336a in P2(1)2(1)2(1) CELL 1.54178 7.3107 9.0733 26.4224 90 90 90 ZERR 4 0.0003 0.0003 0.001 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H O UNIT 84 120 12 L.S. 30 PLAN 20 SIZE 0.04 0.09 0.18 TEMP -173.15 REM Solution 1 R1 0.096 Rweak 0.026, Alpha = 0.0092 in P2(1)2(1)2(1) REM Flack x = 0.066 ( 0.052 ) from Parsons' quotients REM Formula: C21 O3 BOND $H MORE -1 fmap 2 acta 136 CONF REM C:/Documents%20and%20Settings/Daley%20Group/Desktop/Frames/baran336/w REM ork/baran336a_a.hkl WGHT 0.034000 0.439500 FVAR 0.95668 O1 3 0.530619 0.365343 -0.031991 11.00000 0.03548 0.03341 = 0.01773 -0.00825 -0.00256 0.00897 O2 3 0.747041 -0.151987 0.188435 11.00000 0.02497 0.01595 = 0.03233 0.00280 0.00345 -0.00039 O3 3 0.947998 0.005947 0.154641 11.00000 0.01623 0.01618 = 0.02177 -0.00317 0.00249 0.00064 C1 1 0.530087 0.413825 0.010964 11.00000 0.02512 0.01427 = 0.01619 0.00199 0.00067 0.00075 C2 1 0.695576 0.416047 0.045005 11.00000 0.01748 0.01631 = 0.01609 0.00202 0.00384 -0.00003 AFIX 23 H2A 2 0.790588 0.480834 0.030246 11.00000 -1.20000 H2B 2 0.746851 0.315387 0.047797 11.00000 -1.20000 AFIX 0 C3 1 0.642470 0.472851 0.098015 11.00000 0.01252 0.01466 = 0.01400 0.00018 0.00063 -0.00109 C4 1 0.803759 0.473332 0.134745 11.00000 0.01260 0.01521 = 0.01931 0.00040 -0.00110 -0.00264 AFIX 23 H4A 2 0.772132 0.534662 0.164473 11.00000 -1.20000 H4B 2 0.910676 0.518987 0.117924 11.00000 -1.20000 AFIX 0 C5 1 0.856263 0.318944 0.152839 11.00000 0.01049 0.01560 = 0.01686 0.00018 -0.00096 -0.00095 AFIX 23 H5A 2 0.959659 0.325637 0.176925 11.00000 -1.20000 H5B 2 0.895908 0.258582 0.123617 11.00000 -1.20000 AFIX 0 C6 1 0.691700 0.245129 0.178853 11.00000 0.01264 0.01258 = 0.01347 -0.00136 0.00021 0.00071 AFIX 13 H6 2 0.647472 0.320835 0.203486 11.00000 -1.20000 AFIX 0 C7 1 0.731328 0.106645 0.212267 11.00000 0.01531 0.01701 = 0.01381 0.00130 -0.00038 0.00106 C8 1 0.553902 0.064059 0.239701 11.00000 0.01900 0.02209 = 0.01703 0.00582 0.00314 0.00261 AFIX 23 H8A 2 0.575804 -0.026910 0.259483 11.00000 -1.20000 H8B 2 0.521704 0.143325 0.263859 11.00000 -1.20000 AFIX 0 C9 1 0.392394 0.038461 0.204266 11.00000 0.01523 0.02074 = 0.02394 0.00660 0.00367 -0.00131 AFIX 23 H9A 2 0.281435 0.016850 0.224422 11.00000 -1.20000 H9B 2 0.417667 -0.047747 0.182389 11.00000 -1.20000 AFIX 0 C10 1 0.358803 0.174236 0.171327 11.00000 0.01167 0.01877 = 0.01884 0.00241 0.00029 -0.00093 AFIX 23 H10A 2 0.316838 0.256099 0.193208 11.00000 -1.20000 H10B 2 0.259336 0.151960 0.147079 11.00000 -1.20000 AFIX 0 C11 1 0.528909 0.225508 0.141444 11.00000 0.01175 0.01394 = 0.01409 0.00044 -0.00077 -0.00198 C12 1 0.481626 0.381751 0.120313 11.00000 0.01099 0.01412 = 0.01358 -0.00110 0.00010 -0.00039 AFIX 13 H12 2 0.438828 0.439325 0.150334 11.00000 -1.20000 AFIX 0 C13 1 0.317817 0.383592 0.082740 11.00000 0.01492 0.01720 = 0.01841 0.00289 -0.00238 0.00010 AFIX 23 H13A 2 0.290329 0.281653 0.071756 11.00000 -1.20000 H13B 2 0.208147 0.423210 0.100004 11.00000 -1.20000 AFIX 0 C14 1 0.361972 0.479525 0.035885 11.00000 0.01737 0.01739 = 0.01473 0.00063 -0.00362 0.00182 AFIX 13 H14 2 0.256275 0.482644 0.011886 11.00000 -1.20000 AFIX 0 C15 1 0.414921 0.632408 0.052993 11.00000 0.01876 0.01855 = 0.01282 -0.00044 0.00275 0.00113 C16 1 0.569121 0.629994 0.090507 11.00000 0.01655 0.01569 = 0.01931 0.00100 -0.00017 -0.00084 AFIX 23 H16A 2 0.525631 0.669171 0.123341 11.00000 -1.20000 H16B 2 0.669182 0.694448 0.078362 11.00000 -1.20000 AFIX 0 C17 1 0.804182 -0.028291 0.183955 11.00000 0.01306 0.01780 = 0.01626 0.00198 -0.00421 0.00075 C18 1 1.022767 -0.112807 0.124998 11.00000 0.02113 0.02062 = 0.02289 -0.00452 0.00125 0.00376 AFIX 137 H18A 2 0.933769 -0.142777 0.099242 11.00000 -1.50000 H18B 2 1.049905 -0.196675 0.147131 11.00000 -1.50000 H18C 2 1.135516 -0.079796 0.108447 11.00000 -1.50000 AFIX 0 C19 1 0.876235 0.144346 0.252870 11.00000 0.02253 0.02153 = 0.01744 0.00116 -0.00530 0.00318 AFIX 137 H19A 2 0.994477 0.161856 0.236463 11.00000 -1.50000 H19B 2 0.887462 0.061935 0.276642 11.00000 -1.50000 H19C 2 0.838619 0.233145 0.271241 11.00000 -1.50000 AFIX 0 C20 1 0.572114 0.111234 0.099797 11.00000 0.01663 0.01416 = 0.01623 -0.00113 -0.00369 -0.00121 AFIX 137 H20A 2 0.696808 0.126872 0.087287 11.00000 -1.50000 H20B 2 0.485214 0.122699 0.071833 11.00000 -1.50000 H20C 2 0.561734 0.011626 0.113848 11.00000 -1.50000 AFIX 0 C21 1 0.333837 0.754606 0.035364 11.00000 0.02514 0.02013 = 0.02350 -0.00085 -0.00417 0.00424 AFIX 93 H21A 2 0.373433 0.848767 0.046641 11.00000 -1.20000 H21B 2 0.236789 0.747028 0.011596 11.00000 -1.20000 AFIX 0 HKLF 4 REM baran336a in P2(1)2(1)2(1) REM R1 = 0.0263 for 3093 Fo > 4sig(Fo) and 0.0270 for all 3152 data REM 220 parameters refined using 0 restraints END WGHT 0.0288 0.4299 REM Highest difference peak 0.184, deepest hole -0.135, 1-sigma level 0.030 Q1 1 0.5684 0.4208 0.1069 11.00000 0.05 0.18 Q2 1 0.7215 0.1697 0.1945 11.00000 0.05 0.18 Q3 1 0.3408 0.4339 0.0583 11.00000 0.05 0.18 Q4 1 0.4443 0.2010 0.1551 11.00000 0.05 0.17 Q5 1 0.4436 0.4519 0.0224 11.00000 0.05 0.17 Q6 1 0.5169 0.2999 0.1279 11.00000 0.05 0.17 Q7 1 0.6445 0.0919 0.2258 11.00000 0.05 0.17 Q8 1 0.7232 0.4748 0.1150 11.00000 0.05 0.16 Q9 1 0.6126 0.2255 0.1594 11.00000 0.05 0.15 Q10 1 0.3883 0.1022 0.1863 11.00000 0.05 0.15 Q11 1 0.6728 0.4563 0.0709 11.00000 0.05 0.15 Q12 1 0.7550 0.0465 0.1960 11.00000 0.05 0.14 Q13 1 0.5516 0.1809 0.1186 11.00000 0.05 0.14 Q14 1 0.7978 0.1265 0.2301 11.00000 0.05 0.14 Q15 1 0.4694 0.0558 0.2218 11.00000 0.05 0.14 Q16 1 0.6068 0.5467 0.0935 11.00000 0.05 0.14 Q17 1 0.4303 0.6945 0.0316 11.00000 0.05 0.14 Q18 1 0.7725 0.2828 0.1649 11.00000 0.05 0.13 Q19 1 0.8251 0.3966 0.1444 11.00000 0.05 0.13 Q20 1 0.4907 0.6355 0.0698 11.00000 0.05 0.13 ; _shelx_res_checksum 70646 _shelx_hkl_file ; 1 0 0 -0.80 0.20 -1 0 0 -0.50 0.30 2 0 0 460.75 13.50 -2 0 0 476.75 13.50 -4 0 0 201.08 7.70 -5 0 0 2.10 1.70 6 0 0 163.98 7.80 -7 0 0 -2.40 1.00 1 -1 0 447.76 12.50 -1 -1 0 443.66 12.90 -2 -1 0 34.90 1.80 -2 1 0 35.20 1.30 2 -1 0 34.10 1.20 2 1 0 34.30 1.80 -3 -1 0 1.10 0.70 -4 -1 0 60.09 4.20 -5 -1 0 688.63 20.20 -6 -1 0 736.23 22.90 6 -1 0 795.02 21.80 7 1 0 3.30 2.10 7 -1 0 6.00 2.30 -7 1 0 0.40 1.70 -8 1 0 17.90 2.80 8 1 0 21.50 2.50 0 -2 0 3502.55 97.59 -1 -2 0 580.74 17.00 -2 -2 0 252.67 8.20 -3 -2 0 11.90 1.40 -3 -2 0 13.00 2.30 -3 -2 0 11.10 2.00 -4 -2 0 18.60 3.00 -5 -2 0 551.84 17.30 -6 -2 0 130.39 7.90 -6 2 0 139.39 5.40 -6 2 0 123.69 5.00 -6 2 0 136.99 7.40 6 -2 0 143.69 7.00 6 2 0 135.09 6.40 7 2 0 322.17 10.70 -7 2 0 321.57 9.30 7 -2 0 299.87 12.30 -7 2 0 312.47 12.80 8 2 0 82.09 4.10 -8 2 0 78.29 5.20 0 -3 0 -0.60 0.50 -1 -3 0 389.96 11.90 1 -3 0 377.56 11.40 -2 -3 0 6.30 1.20 -3 -3 0 1381.86 33.20 -3 -3 0 1344.97 35.30 -4 -3 0 166.08 7.30 -4 -3 0 163.58 7.30 -5 -3 0 10.10 3.00 -6 3 0 21.30 2.30 -6 3 0 20.90 2.60 -6 3 0 26.10 3.70 -6 -3 0 25.50 4.30 6 -3 0 22.40 3.30 6 3 0 22.20 3.10 -7 3 0 373.46 10.50 7 3 0 363.66 11.60 -7 3 0 378.66 14.10 -8 3 0 88.09 5.60 8 3 0 101.59 4.20 0 -4 0 1409.06 40.40 -1 -4 0 386.16 12.40 -2 4 0 1148.89 38.80 2 4 0 1268.67 37.10 -2 -4 0 1213.68 30.70 -3 -4 0 61.29 3.90 -3 -4 0 64.09 3.80 3 4 0 61.09 4.40 -4 -4 0 791.52 22.70 -4 -4 0 748.03 21.20 4 4 0 760.52 25.50 -5 -4 0 6.10 2.60 5 4 0 2.10 1.50 -6 4 0 268.37 8.60 -6 4 0 247.28 8.00 6 4 0 256.97 9.10 6 -4 0 284.97 9.90 -6 4 0 278.87 11.10 -6 -4 0 277.17 11.10 6 4 0 262.07 8.80 6 4 0 249.28 8.90 -6 4 0 271.87 7.60 -7 4 0 339.37 9.70 7 4 0 332.07 10.10 -7 4 0 351.16 12.90 -8 4 0 93.09 4.80 0 5 0 0.40 2.00 -1 5 0 442.76 18.40 1 5 0 452.15 17.50 -2 5 0 638.34 25.40 -2 -5 0 695.43 18.30 2 5 0 688.73 23.80 3 5 0 77.19 5.90 -3 -5 0 79.39 4.50 4 5 0 348.87 15.00 4 5 0 344.57 10.70 -4 -5 0 353.16 12.70 -4 -5 0 357.16 12.00 -5 5 0 408.16 10.50 5 5 0 414.06 12.60 -5 -5 0 388.46 14.90 -5 5 0 402.96 11.50 5 5 0 436.86 12.50 -6 5 0 82.69 4.50 6 5 0 78.69 4.20 -6 5 0 86.39 3.50 6 5 0 83.19 4.60 6 5 0 84.89 4.40 -7 5 0 257.27 9.70 -7 5 0 241.48 6.40 0 6 0 189.78 11.70 1 6 0 85.79 7.40 -1 6 0 85.79 8.20 -2 6 0 28.20 5.90 -2 -6 0 23.50 2.20 2 6 0 25.60 4.80 3 6 0 31.70 5.50 3 6 0 23.00 2.90 -3 -6 0 28.10 3.30 4 6 0 292.97 14.90 4 6 0 306.17 8.50 -4 -6 0 306.07 11.80 4 6 0 296.87 10.10 4 6 0 309.67 11.70 -4 6 0 314.27 8.30 4 6 0 315.37 9.30 4 6 0 317.77 10.30 5 6 0 457.45 13.70 -5 6 0 491.15 11.70 -5 -6 0 464.45 16.20 5 6 0 454.95 13.70 5 6 0 476.35 12.60 6 6 0 54.89 3.60 6 6 0 58.29 3.90 -6 6 0 52.89 2.60 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0 26 64.19 3.50 -5 0 -26 28.40 1.90 0 -1 26 301.17 9.30 0 -1 26 291.97 10.00 0 1 -26 291.57 8.50 0 1 26 276.97 10.10 0 1 26 288.97 9.40 0 -1 -26 272.27 8.50 -1 1 26 110.49 6.00 1 -1 26 111.89 5.00 -1 -1 -26 108.19 4.90 1 1 -26 108.39 4.30 -1 1 26 106.19 5.40 -1 1 -26 105.29 4.50 1 -1 -26 105.79 4.80 -1 -1 26 106.79 5.10 1 1 26 100.49 5.50 1 1 26 102.09 5.20 -1 -1 26 102.39 5.50 -2 1 26 15.60 2.60 -2 -1 -26 13.80 2.50 -2 1 26 17.00 2.60 2 1 26 9.50 2.00 -2 -1 26 10.40 2.30 -2 -1 26 14.40 2.50 -3 1 26 27.20 3.00 -3 1 26 21.30 2.40 -3 -1 -26 23.90 2.70 -3 1 -26 23.60 3.60 3 1 26 18.50 3.00 -3 -1 26 17.50 2.40 -3 1 -26 24.10 2.50 -3 -1 26 22.60 2.60 -4 -1 -26 109.89 4.60 4 -1 26 110.39 4.60 -4 -1 26 105.79 4.70 -4 1 -26 106.79 4.30 -4 -1 26 113.59 4.40 -4 1 -26 106.29 6.00 5 -1 26 56.39 2.90 0 -2 -26 8.20 2.00 0 2 26 6.50 2.30 0 -2 26 5.60 1.60 0 2 -26 7.90 1.60 0 2 26 5.50 2.00 0 -2 26 7.80 1.90 1 2 -26 253.07 7.60 -1 -2 -26 254.47 8.00 -1 2 26 247.88 8.50 -1 2 26 266.27 9.50 -1 -2 26 246.68 8.90 -1 2 -26 250.97 7.70 1 2 26 248.38 8.70 1 2 26 239.98 9.40 -1 -2 26 244.18 8.20 1 -2 -26 243.18 7.60 -2 2 26 145.49 5.90 -2 -2 -26 144.89 5.80 -2 2 26 146.59 6.50 2 2 -26 153.58 5.10 -2 2 -26 154.88 5.30 -2 -2 26 150.68 6.00 -2 -2 26 139.39 6.40 2 2 26 142.09 6.00 2 -2 -26 148.99 5.20 -3 2 26 3.40 1.50 -3 -2 -26 10.20 1.90 -3 -2 26 7.30 1.80 -3 2 -26 7.20 2.10 3 2 26 9.40 2.30 -3 -2 26 10.70 2.00 -4 -2 -26 27.40 2.40 4 -2 26 23.90 2.40 -4 2 -26 24.00 3.00 -4 -2 26 27.40 2.30 4 2 26 27.20 2.80 -4 -2 26 26.10 2.40 -4 2 -26 28.10 2.00 0 -3 -26 537.45 13.40 0 3 -26 493.25 13.40 0 3 26 520.85 15.80 0 3 26 531.45 14.40 -1 3 26 534.25 14.70 1 3 -26 551.74 14.10 -1 -3 -26 545.25 13.90 -1 3 26 558.14 16.20 -1 -3 26 546.35 15.40 1 -3 -26 553.94 13.70 1 3 26 521.25 16.10 1 3 26 544.45 15.00 -1 3 -26 561.74 14.00 -2 3 26 110.59 4.80 -2 -3 -26 106.99 4.50 -2 3 26 111.89 5.40 2 3 -26 105.99 4.20 -2 3 -26 105.59 5.90 2 -3 -26 113.59 4.40 2 3 26 108.19 5.40 -2 -3 26 96.99 4.50 2 3 26 103.49 5.30 2 3 26 102.09 4.90 -2 -3 26 110.69 5.20 -2 3 -26 104.49 4.10 -3 -3 -26 263.27 7.70 -3 -3 26 253.77 8.50 3 -3 -26 249.08 7.10 -3 3 -26 256.67 9.90 3 3 26 269.47 9.20 3 3 26 253.47 8.00 -3 -3 26 264.37 7.80 4 -3 26 2.90 1.30 -4 -3 -26 2.60 0.90 -4 -3 26 -0.20 0.90 -4 -3 26 0.80 1.10 4 3 26 -0.80 1.30 -4 3 -26 1.80 0.90 0 4 26 58.89 4.30 0 -4 -26 61.19 3.30 0 4 26 67.99 4.10 0 4 -26 52.89 2.80 -1 4 26 2.30 1.60 -1 4 26 5.70 1.60 1 4 -26 4.70 1.30 -1 -4 -26 9.20 1.70 1 4 26 7.60 2.10 1 4 26 6.50 1.90 -1 4 -26 4.80 1.10 1 -4 -26 6.10 1.40 -2 4 26 45.40 3.30 -2 -4 -26 46.80 2.80 2 4 -26 48.40 2.70 -2 4 -26 48.40 3.70 -2 -4 26 49.90 2.90 -2 4 -26 44.70 2.40 2 4 26 52.79 3.70 2 4 26 47.10 3.60 2 4 26 47.60 3.30 -2 -4 26 48.80 3.10 2 -4 -26 50.09 2.90 3 4 -26 35.50 2.00 3 4 26 39.10 2.70 -3 -4 26 38.10 2.60 -3 -4 26 40.50 2.50 3 -4 -26 38.90 2.30 3 4 26 40.60 3.00 0 5 26 196.78 6.60 0 5 -26 191.58 5.70 0 5 26 200.38 7.50 0 -5 -26 194.38 5.90 1 5 -26 204.08 6.00 -1 -5 -26 199.68 5.90 -1 5 26 200.28 7.20 1 -5 -26 204.38 6.00 -1 5 -26 199.78 5.80 1 5 26 202.18 7.60 1 5 26 205.38 6.70 2 5 -26 10.80 1.30 2 5 26 11.70 1.90 2 -5 -26 8.30 1.20 2 5 26 6.00 1.60 3 5 -26 17.20 1.30 3 -5 -26 18.80 1.50 3 5 26 19.10 1.80 0 6 26 35.40 2.50 1 6 26 107.09 4.50 0 0 27 2.20 1.80 0 0 -27 1.50 1.00 0 0 27 -2.60 1.50 -1 0 27 0.00 1.70 -1 0 -27 -1.20 1.50 1 0 27 0.90 1.50 -1 0 27 1.00 1.80 -2 0 27 133.49 6.20 -2 0 27 132.89 5.70 -2 0 -27 129.19 5.20 -3 0 27 19.60 2.30 -3 0 -27 14.00 2.40 -3 0 -27 24.60 2.50 -3 0 27 20.00 2.50 -4 0 -27 0.00 0.90 -4 0 27 0.70 0.70 -4 0 -27 -0.80 1.10 -4 0 27 -1.60 0.90 0 1 27 28.20 3.50 0 -1 27 29.50 3.30 0 1 27 27.60 2.90 0 -1 27 28.20 2.80 0 1 -27 23.40 2.20 0 -1 -27 31.00 2.90 -1 -1 -27 146.09 5.70 1 1 -27 149.39 5.10 -1 1 27 143.59 6.70 -1 1 27 149.99 6.20 -1 -1 27 142.59 5.90 -1 -1 27 139.09 6.50 1 1 27 139.79 6.00 1 1 27 144.19 6.50 -1 1 -27 141.59 5.20 -2 -1 -27 108.89 4.90 -2 1 27 107.49 5.00 -2 1 27 117.19 5.60 -2 -1 27 106.59 4.90 -2 -1 27 106.79 5.50 -3 -1 -27 97.99 4.50 -3 1 27 97.19 4.70 -3 1 27 97.59 4.30 -3 1 -27 96.49 5.70 3 1 27 100.99 5.10 -3 -1 27 93.69 4.70 -3 -1 27 93.99 4.50 -3 1 -27 93.99 4.00 -4 -1 -27 29.90 2.40 -4 -1 27 32.80 2.40 -4 -1 27 30.30 2.30 -4 1 -27 29.00 3.00 -4 1 -27 32.70 2.20 0 2 27 1363.06 32.20 0 2 -27 1338.47 31.50 0 2 27 1347.47 34.30 0 -2 -27 1403.56 30.40 -1 2 27 16.90 2.80 -1 2 27 9.60 2.10 1 2 -27 18.10 1.90 -1 -2 -27 21.20 2.50 -1 -2 27 21.50 2.50 1 -2 -27 16.30 2.10 1 2 27 15.90 2.40 -1 -2 27 19.90 2.60 1 2 27 15.80 2.50 -1 2 -27 13.30 1.80 -2 -2 -27 52.49 3.50 -2 2 27 53.69 3.90 -2 2 27 57.29 3.50 2 2 -27 52.39 2.80 -2 -2 27 52.29 3.40 -2 -2 27 52.19 3.80 2 -2 -27 51.49 2.90 2 2 27 47.90 4.00 2 2 27 57.29 3.60 -2 2 -27 57.29 4.40 -3 2 27 53.59 3.30 -3 -2 -27 48.40 3.10 3 2 27 52.49 3.90 -3 -2 27 56.99 3.50 -3 2 -27 51.29 4.00 -3 -2 27 51.19 3.50 -4 -2 -27 126.79 4.30 -4 2 -27 119.89 5.70 -4 -2 27 127.89 4.70 4 2 27 127.29 5.20 -4 -2 27 124.59 4.30 0 3 27 3.80 1.70 0 -3 -27 4.00 1.50 0 3 27 3.80 1.90 0 3 -27 5.90 1.40 1 3 -27 160.08 5.40 -1 -3 -27 157.08 5.70 -1 3 27 155.08 6.80 -1 3 27 161.38 6.20 -1 -3 27 159.58 6.10 1 3 27 155.98 6.20 1 -3 -27 152.68 5.40 1 3 27 154.28 6.80 -1 3 -27 163.18 5.30 -2 -3 -27 88.49 4.00 -2 3 27 96.69 4.80 2 3 -27 90.79 3.60 -2 3 27 92.59 4.20 -2 -3 27 89.49 4.60 -2 3 -27 86.39 5.00 2 3 27 81.69 4.40 2 3 27 88.89 4.30 -2 -3 27 89.69 4.00 2 3 27 97.69 4.90 2 -3 -27 83.59 3.60 -3 -3 -27 15.90 1.70 3 -3 -27 20.20 1.70 -3 3 -27 19.00 2.40 3 3 27 15.00 2.20 -3 -3 27 19.60 2.00 -3 -3 27 17.60 2.00 0 4 -27 26.70 2.00 0 -4 -27 31.60 2.40 0 4 27 34.20 2.90 0 4 27 30.80 3.10 -1 4 27 443.16 13.10 1 4 -27 437.56 11.30 -1 4 27 430.66 11.70 -1 -4 -27 448.86 11.30 1 4 27 435.56 12.10 1 4 27 452.05 13.40 1 -4 -27 445.26 11.20 1 4 27 447.56 12.60 -1 4 -27 437.76 11.20 2 4 -27 30.40 2.00 -2 -4 -27 26.60 2.10 -2 4 27 29.70 2.50 -2 -4 27 29.70 2.30 2 4 27 32.30 2.70 2 4 27 28.80 2.50 2 4 27 25.80 2.50 2 -4 -27 29.40 2.20 3 4 27 2.20 1.00 -3 -4 27 0.90 0.80 3 4 27 1.00 1.10 -3 -4 27 0.80 0.90 3 -4 -27 2.00 0.80 0 5 27 319.27 9.90 0 5 27 319.57 8.70 0 -5 -27 304.17 8.20 0 5 -27 320.27 8.30 1 5 -27 18.60 1.40 -1 5 27 27.00 2.50 -1 -5 -27 21.10 1.70 1 5 27 20.00 2.00 1 5 27 18.20 2.20 1 -5 -27 17.70 1.60 2 5 -27 65.39 2.60 2 5 27 68.79 3.20 2 -5 -27 63.69 2.60 2 5 27 62.59 3.30 0 0 28 109.19 4.90 0 0 28 112.69 5.40 -1 0 -28 55.69 3.20 -1 0 28 57.99 3.60 1 0 28 51.39 3.30 -1 0 28 55.89 4.10 -2 0 28 252.27 8.90 -2 0 28 273.37 8.40 -2 0 -28 257.27 7.70 -3 0 28 0.20 1.10 -3 0 -28 -0.60 1.10 -3 0 28 -1.80 1.10 -3 0 -28 1.70 1.20 -4 0 -28 19.80 1.80 0 1 28 86.39 5.00 0 1 28 87.19 4.50 0 -1 28 93.89 4.60 0 -1 -28 100.09 4.20 0 -1 28 90.99 4.30 0 1 -28 90.69 3.90 -1 1 28 65.69 4.50 -1 1 28 74.59 4.20 -1 -1 -28 74.49 3.70 1 1 -28 66.19 3.10 1 1 28 68.09 3.90 1 1 28 64.39 4.00 -1 -1 28 63.89 3.80 -1 -1 28 66.59 4.20 -2 -1 -28 192.88 6.40 -2 1 28 195.68 6.70 -2 1 28 195.48 7.40 -2 -1 28 202.58 6.80 -2 -1 28 203.48 7.50 -2 1 -28 184.58 8.40 2 1 28 190.98 7.50 -3 -1 -28 54.09 3.10 -3 1 28 55.29 3.30 -3 1 28 52.09 3.00 -3 1 -28 49.30 3.90 -3 -1 28 50.49 3.20 -3 -1 28 52.29 3.40 -3 1 -28 47.10 2.70 -4 -1 -28 13.00 1.40 -4 1 -28 8.20 1.30 0 2 -28 113.99 4.50 0 2 28 121.89 5.40 0 2 28 125.89 6.00 0 -2 -28 127.19 4.90 1 2 -28 143.59 4.90 -1 -2 -28 150.98 5.40 -1 2 28 155.98 6.00 -1 2 28 147.49 6.40 1 2 28 150.58 6.40 1 -2 -28 144.89 5.00 -1 -2 28 140.89 5.40 -1 2 -28 142.89 5.10 -1 -2 28 140.59 6.00 1 2 28 146.09 5.80 -2 2 28 37.90 3.10 -2 -2 -28 39.50 2.90 -2 2 28 36.60 2.90 2 2 28 37.70 2.90 2 2 28 40.00 3.40 -2 -2 28 38.10 2.80 -2 -2 28 36.30 3.10 -2 2 -28 36.40 3.50 2 -2 -28 38.80 2.40 -3 -2 -28 6.70 1.30 -3 2 28 4.30 1.10 -3 2 -28 6.90 1.80 -3 -2 28 7.30 1.50 -3 -2 28 8.60 1.60 3 2 28 6.90 1.70 0 3 28 542.45 15.60 0 3 28 534.45 14.30 0 3 -28 543.45 13.60 0 -3 -28 557.54 13.50 -1 -3 -28 13.70 2.00 -1 3 28 12.80 2.00 -1 3 28 12.30 2.20 1 3 -28 10.60 1.40 1 3 28 7.90 2.00 -1 3 -28 14.40 1.60 1 3 28 13.80 2.00 1 -3 -28 13.00 1.80 -1 3 -28 12.20 2.20 -2 3 28 36.70 2.70 2 3 -28 36.00 2.00 -2 -3 -28 36.40 2.50 -2 3 28 34.10 2.50 -2 -3 28 35.30 2.70 -2 -3 28 36.60 2.40 2 3 28 39.10 3.30 2 3 28 35.20 2.60 -2 3 -28 31.90 2.80 2 -3 -28 37.80 2.30 -3 -3 -28 1.70 0.90 -3 -3 28 2.70 0.90 3 3 28 0.60 1.30 -3 -3 28 0.90 0.80 -3 3 -28 1.60 0.80 0 4 28 340.37 10.60 0 -4 -28 347.27 9.00 0 4 28 347.37 9.60 0 4 -28 346.27 9.00 -1 -4 -28 4.80 1.20 -1 4 28 8.00 1.50 -1 4 28 4.10 1.40 1 4 -28 5.10 1.10 1 4 28 3.50 1.50 1 4 28 6.00 1.50 -1 4 -28 5.30 1.00 1 4 28 3.20 1.40 1 -4 -28 6.20 1.30 2 4 -28 51.19 2.30 -2 -4 -28 50.69 2.50 2 4 28 54.49 3.00 2 4 28 47.60 2.70 2 4 28 47.60 3.00 2 -4 -28 50.69 2.40 0 -5 -28 497.55 11.80 0 5 28 507.45 13.60 1 5 -28 16.20 1.10 1 -5 -28 19.00 1.40 1 5 28 23.40 2.10 0 0 29 0.90 1.30 0 0 29 1.20 1.30 -1 0 29 3.40 1.40 -1 0 29 4.00 1.60 1 0 29 2.80 1.20 -2 0 29 89.29 4.20 -2 0 -29 81.09 4.80 -2 0 -29 82.29 3.70 -2 0 29 82.79 4.30 -3 0 29 21.90 2.00 -3 0 -29 23.30 1.90 -3 0 -29 19.00 2.30 -3 0 29 23.90 2.10 0 -1 29 219.08 7.00 0 1 -29 221.78 6.50 0 1 29 209.08 7.90 0 1 29 218.28 7.30 0 -1 -29 215.68 6.50 -1 1 29 509.55 13.30 -1 1 29 502.85 14.40 -1 -1 -29 491.65 12.30 1 1 -29 489.35 12.50 -1 -1 29 500.35 13.00 1 1 29 501.85 13.20 -1 -1 29 488.35 14.00 -2 1 29 55.69 3.60 -2 -1 -29 47.70 3.20 -2 1 29 52.19 3.30 -2 -1 -29 56.49 3.20 -2 -1 29 55.19 3.50 2 1 29 56.79 3.50 -2 1 -29 50.69 4.00 -2 -1 29 51.29 3.20 -3 -1 -29 21.90 1.90 -3 1 29 22.60 1.90 -3 1 29 21.50 2.00 -3 -1 29 19.50 2.00 -3 1 -29 16.30 2.20 -3 -1 29 16.20 1.90 0 2 29 128.79 5.30 0 -2 -29 124.69 4.60 0 2 -29 120.19 4.40 0 2 29 118.69 5.60 -1 2 29 25.70 2.90 1 2 -29 31.20 2.10 -1 -2 -29 36.60 2.70 -1 2 29 36.20 3.00 -1 -2 29 34.50 2.50 1 -2 -29 30.90 2.40 1 2 29 32.70 2.80 1 2 29 27.40 2.40 -1 -2 29 36.80 2.70 -2 -2 -29 24.50 2.30 -2 2 29 24.10 2.20 -2 2 29 23.30 2.50 2 2 29 16.00 1.70 -2 2 -29 23.90 2.80 -2 -2 29 24.40 2.20 2 2 29 23.10 2.50 -2 -2 29 20.80 2.30 -3 -2 -29 27.60 2.10 -3 -2 29 24.20 2.00 -3 2 -29 26.30 2.40 3 2 29 18.70 2.00 -3 -2 29 25.10 2.10 0 3 29 192.28 7.20 0 3 29 207.08 6.80 0 3 -29 193.78 5.90 0 -3 -29 210.38 6.10 1 3 -29 33.80 2.10 -1 -3 -29 37.00 2.60 -1 3 29 38.80 2.70 -1 3 29 37.90 3.00 1 -3 -29 36.10 2.30 -1 3 -29 34.50 2.00 -1 3 -29 39.60 2.80 1 3 29 39.10 3.00 1 3 29 34.50 2.80 1 3 29 30.40 2.60 -2 -3 -29 3.40 1.00 -2 3 29 2.80 1.10 2 3 -29 1.50 0.60 -2 -3 29 0.80 0.90 2 3 29 4.40 1.20 2 -3 -29 1.70 0.70 2 3 29 1.40 1.30 -2 -3 29 1.00 0.80 -2 3 -29 2.10 0.80 0 4 29 28.30 2.30 0 4 29 29.30 2.20 0 4 -29 29.10 1.60 0 4 29 32.00 2.50 0 -4 -29 25.20 1.90 1 4 -29 1.20 0.70 -1 -4 -29 1.00 0.80 -1 4 29 0.90 0.90 1 4 29 1.90 1.10 1 -4 -29 2.00 0.90 1 4 29 0.30 0.90 1 4 29 0.30 0.80 0 0 30 59.19 3.30 0 0 30 62.09 3.50 -1 0 30 3.80 1.30 -1 0 30 3.90 1.40 -2 0 30 56.59 3.30 -2 0 -30 56.69 3.50 -2 0 30 63.29 3.20 0 -1 -30 -0.30 0.90 0 1 30 -0.20 1.30 0 1 30 -1.30 1.00 0 -1 30 0.70 0.90 -1 1 30 411.86 11.00 -1 1 30 390.36 11.60 -1 -1 -30 402.76 10.10 1 1 30 394.46 10.70 -1 -1 30 408.16 10.70 -1 -1 30 401.36 11.50 -2 -1 -30 47.70 2.50 -2 1 30 50.09 2.90 -2 1 30 43.40 2.80 -2 -1 30 41.20 2.50 -2 1 -30 40.20 3.20 -2 -1 30 36.70 2.70 0 2 -30 37.60 2.20 0 2 30 40.60 2.80 0 2 30 35.30 2.90 0 -2 -30 38.60 2.30 1 2 -30 20.90 1.40 -1 2 30 26.80 2.70 -1 2 30 18.50 2.00 -1 -2 -30 24.00 2.10 -1 2 -30 19.80 2.20 1 2 30 16.60 1.80 -2 -2 -30 16.10 1.60 -2 2 30 14.70 1.70 -2 2 30 18.30 1.70 2 2 30 13.70 1.80 -2 -2 30 14.00 1.60 -2 -2 30 12.00 1.50 -2 2 -30 13.50 1.80 0 -3 -30 72.19 3.00 0 3 30 69.29 3.40 0 3 30 72.09 3.60 0 3 -30 64.49 2.70 -1 -3 -30 11.30 1.50 1 3 -30 10.80 1.20 -1 3 30 14.90 1.60 -1 3 30 11.60 1.60 1 3 30 15.10 1.80 1 3 30 9.80 1.50 1 -3 -30 12.20 1.30 1 3 30 11.90 1.70 0 0 31 1.00 0.90 -1 0 31 287.07 8.00 -1 0 31 291.77 8.70 -2 0 31 0.50 0.70 -2 0 31 0.10 0.90 0 1 31 186.18 5.90 0 1 31 181.38 6.30 -1 1 31 70.69 3.60 -1 1 31 76.09 3.50 -1 1 -31 67.79 3.80 -1 -1 31 73.39 3.10 0 2 31 6.20 1.30 0 2 31 3.00 1.10 -1 2 31 26.60 2.20 -1 2 31 33.40 2.20 -1 2 -31 27.00 2.10 1 2 31 29.60 2.20 ; _shelx_hkl_checksum 5765 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -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 O1 O 0.5306(2) 0.36534(16) -0.03199(5) 0.0289(3) Uani 1 1 d . . O2 O 0.74704(18) -0.15199(14) 0.18843(5) 0.0244(3) Uani 1 1 d . . O3 O 0.94800(16) 0.00595(13) 0.15464(4) 0.0181(3) Uani 1 1 d . . C1 C 0.5301(3) 0.41382(18) 0.01096(6) 0.0185(4) Uani 1 1 d . . C2 C 0.6956(2) 0.41605(19) 0.04500(6) 0.0166(3) Uani 1 1 d . . H2A H 0.7906 0.4808 0.0302 0.020 Uiso 1 1 calc R U H2B H 0.7469 0.3154 0.0478 0.020 Uiso 1 1 calc R U C3 C 0.6425(2) 0.47285(18) 0.09801(6) 0.0137(3) Uani 1 1 d . . C4 C 0.8038(2) 0.47333(18) 0.13475(6) 0.0157(3) Uani 1 1 d . . H4A H 0.7721 0.5347 0.1645 0.019 Uiso 1 1 calc R U H4B H 0.9107 0.5190 0.1179 0.019 Uiso 1 1 calc R U C5 C 0.8563(2) 0.31894(18) 0.15284(6) 0.0143(3) Uani 1 1 d . . H5A H 0.9597 0.3256 0.1769 0.017 Uiso 1 1 calc R U H5B H 0.8959 0.2586 0.1236 0.017 Uiso 1 1 calc R U C6 C 0.6917(2) 0.24513(17) 0.17885(6) 0.0129(3) Uani 1 1 d . . H6 H 0.6475 0.3208 0.2035 0.015 Uiso 1 1 calc R U C7 C 0.7313(2) 0.10665(19) 0.21227(6) 0.0154(3) Uani 1 1 d . . C8 C 0.5539(2) 0.06406(19) 0.23970(6) 0.0194(4) Uani 1 1 d . . H8A H 0.5758 -0.0269 0.2595 0.023 Uiso 1 1 calc R U H8B H 0.5217 0.1433 0.2639 0.023 Uiso 1 1 calc R U C9 C 0.3924(2) 0.0385(2) 0.20427(7) 0.0200(4) Uani 1 1 d . . H9A H 0.2814 0.0169 0.2244 0.024 Uiso 1 1 calc R U H9B H 0.4177 -0.0477 0.1824 0.024 Uiso 1 1 calc R U C10 C 0.3588(2) 0.17424(19) 0.17133(6) 0.0164(3) Uani 1 1 d . . H10A H 0.3168 0.2561 0.1932 0.020 Uiso 1 1 calc R U H10B H 0.2593 0.1520 0.1471 0.020 Uiso 1 1 calc R U C11 C 0.5289(2) 0.22551(18) 0.14144(6) 0.0133(3) Uani 1 1 d . . C12 C 0.4816(2) 0.38175(17) 0.12031(5) 0.0129(3) Uani 1 1 d . . H12 H 0.4388 0.4393 0.1503 0.015 Uiso 1 1 calc R U C13 C 0.3178(2) 0.38359(19) 0.08274(6) 0.0168(3) Uani 1 1 d . . H13A H 0.2903 0.2817 0.0718 0.020 Uiso 1 1 calc R U H13B H 0.2081 0.4232 0.1000 0.020 Uiso 1 1 calc R U C14 C 0.3620(2) 0.47952(19) 0.03589(6) 0.0165(3) Uani 1 1 d . . H14 H 0.2563 0.4826 0.0119 0.020 Uiso 1 1 calc R U C15 C 0.4149(2) 0.63241(19) 0.05299(6) 0.0167(3) Uani 1 1 d . . C16 C 0.5691(2) 0.62999(19) 0.09051(6) 0.0172(3) Uani 1 1 d . . H16A H 0.5256 0.6692 0.1233 0.021 Uiso 1 1 calc R U H16B H 0.6692 0.6944 0.0784 0.021 Uiso 1 1 calc R U C17 C 0.8042(2) -0.02829(18) 0.18395(6) 0.0157(3) Uani 1 1 d . . C18 C 1.0228(3) -0.1128(2) 0.12500(6) 0.0215(4) Uani 1 1 d . . H18A H 0.9338 -0.1428 0.0992 0.032 Uiso 1 1 calc R U H18B H 1.0499 -0.1967 0.1471 0.032 Uiso 1 1 calc R U H18C H 1.1355 -0.0798 0.1084 0.032 Uiso 1 1 calc R U C19 C 0.8762(2) 0.1443(2) 0.25287(6) 0.0205(4) Uani 1 1 d . . H19A H 0.9945 0.1619 0.2365 0.031 Uiso 1 1 calc R U H19B H 0.8875 0.0619 0.2766 0.031 Uiso 1 1 calc R U H19C H 0.8386 0.2331 0.2712 0.031 Uiso 1 1 calc R U C20 C 0.5721(2) 0.11123(18) 0.09980(6) 0.0157(3) Uani 1 1 d . . H20A H 0.6968 0.1269 0.0873 0.024 Uiso 1 1 calc R U H20B H 0.4852 0.1227 0.0718 0.024 Uiso 1 1 calc R U H20C H 0.5617 0.0116 0.1138 0.024 Uiso 1 1 calc R U C21 C 0.3338(3) 0.7546(2) 0.03536(7) 0.0229(4) Uani 1 1 d . . H21A H 0.3734 0.8488 0.0466 0.028 Uiso 1 1 calc R U H21B H 0.2368 0.7470 0.0116 0.028 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 O1 0.0355(8) 0.0334(7) 0.0177(6) -0.0082(5) -0.0026(6) 0.0090(7) O2 0.0250(7) 0.0159(6) 0.0323(7) 0.0028(5) 0.0034(5) -0.0004(5) O3 0.0162(6) 0.0162(6) 0.0218(6) -0.0032(5) 0.0025(5) 0.0006(5) C1 0.0251(9) 0.0143(8) 0.0162(8) 0.0020(6) 0.0007(7) 0.0007(7) C2 0.0175(8) 0.0163(8) 0.0161(8) 0.0020(6) 0.0038(6) 0.0000(7) C3 0.0125(7) 0.0147(8) 0.0140(7) 0.0002(6) 0.0006(6) -0.0011(6) C4 0.0126(8) 0.0152(8) 0.0193(8) 0.0004(6) -0.0011(6) -0.0026(6) C5 0.0105(7) 0.0156(8) 0.0169(7) 0.0002(6) -0.0010(6) -0.0010(6) C6 0.0126(8) 0.0126(8) 0.0135(7) -0.0014(6) 0.0002(6) 0.0007(6) C7 0.0153(8) 0.0170(8) 0.0138(7) 0.0013(6) -0.0004(6) 0.0011(6) C8 0.0190(9) 0.0221(9) 0.0170(8) 0.0058(6) 0.0031(7) 0.0026(7) C9 0.0152(8) 0.0207(9) 0.0239(9) 0.0066(7) 0.0037(7) -0.0013(7) C10 0.0117(8) 0.0188(9) 0.0188(8) 0.0024(6) 0.0003(6) -0.0009(6) C11 0.0118(8) 0.0139(8) 0.0141(7) 0.0004(6) -0.0008(6) -0.0020(6) C12 0.0110(7) 0.0141(8) 0.0136(7) -0.0011(6) 0.0001(6) -0.0004(6) C13 0.0149(8) 0.0172(8) 0.0184(8) 0.0029(6) -0.0024(6) 0.0001(6) C14 0.0174(8) 0.0174(8) 0.0147(7) 0.0006(7) -0.0036(6) 0.0018(7) C15 0.0188(8) 0.0186(8) 0.0128(7) -0.0004(6) 0.0028(6) 0.0011(7) C16 0.0165(8) 0.0157(8) 0.0193(8) 0.0010(6) -0.0002(7) -0.0008(7) C17 0.0131(8) 0.0178(8) 0.0163(8) 0.0020(6) -0.0042(6) 0.0008(6) C18 0.0211(9) 0.0206(9) 0.0229(8) -0.0045(7) 0.0012(7) 0.0038(7) C19 0.0225(9) 0.0215(9) 0.0174(8) 0.0012(7) -0.0053(7) 0.0032(7) C20 0.0166(8) 0.0142(8) 0.0162(8) -0.0011(6) -0.0037(6) -0.0012(6) C21 0.0251(10) 0.0201(9) 0.0235(8) -0.0009(7) -0.0042(8) 0.0042(8) 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' O O 0.0492 0.0322 '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 C17 O3 C18 115.98(13) O1 C1 C2 123.95(16) O1 C1 C14 123.34(16) C2 C1 C14 112.71(13) C1 C2 H2A 109.6 C1 C2 H2B 109.6 C1 C2 C3 110.14(14) H2A C2 H2B 108.1 C3 C2 H2A 109.6 C3 C2 H2B 109.6 C2 C3 C12 110.93(13) C4 C3 C2 112.57(13) C4 C3 C12 110.18(12) C4 C3 C16 110.42(13) C16 C3 C2 106.31(13) C16 C3 C12 106.18(13) C3 C4 H4A 109.0 C3 C4 H4B 109.0 C3 C4 C5 112.95(13) H4A C4 H4B 107.8 C5 C4 H4A 109.0 C5 C4 H4B 109.0 C4 C5 H5A 109.7 C4 C5 H5B 109.7 C4 C5 C6 110.00(13) H5A C5 H5B 108.2 C6 C5 H5A 109.7 C6 C5 H5B 109.7 C5 C6 H6 104.2 C5 C6 C7 117.21(13) C5 C6 C11 111.33(12) C7 C6 H6 104.2 C11 C6 H6 104.2 C11 C6 C7 114.10(13) C8 C7 C6 108.21(13) C8 C7 C19 107.88(13) C17 C7 C6 115.57(13) C17 C7 C8 108.87(14) C17 C7 C19 106.12(13) C19 C7 C6 109.95(14) C7 C8 H8A 108.8 C7 C8 H8B 108.8 H8A C8 H8B 107.7 C9 C8 C7 113.75(13) C9 C8 H8A 108.8 C9 C8 H8B 108.8 C8 C9 H9A 109.5 C8 C9 H9B 109.5 C8 C9 C10 110.57(14) H9A C9 H9B 108.1 C10 C9 H9A 109.5 C10 C9 H9B 109.5 C9 C10 H10A 108.8 C9 C10 H10B 108.8 C9 C10 C11 113.86(14) H10A C10 H10B 107.7 C11 C10 H10A 108.8 C11 C10 H10B 108.8 C6 C11 C12 106.99(12) C10 C11 C6 108.98(12) C10 C11 C12 106.13(13) C20 C11 C6 111.88(13) C20 C11 C10 109.06(13) C20 C11 C12 113.56(12) C3 C12 C11 116.80(13) C3 C12 H12 105.1 C3 C12 C13 109.57(12) C11 C12 H12 105.1 C13 C12 C11 114.09(12) C13 C12 H12 105.1 C12 C13 H13A 109.5 C12 C13 H13B 109.5 H13A C13 H13B 108.1 C14 C13 C12 110.86(13) C14 C13 H13A 109.5 C14 C13 H13B 109.5 C1 C14 C13 107.18(13) C1 C14 H14 111.2 C13 C14 H14 111.2 C15 C14 C1 106.47(14) C15 C14 C13 109.32(13) C15 C14 H14 111.2 C16 C15 C14 112.14(14) C21 C15 C14 122.86(15) C21 C15 C16 124.99(16) C3 C16 H16A 109.4 C3 C16 H16B 109.4 C15 C16 C3 111.16(14) C15 C16 H16A 109.4 C15 C16 H16B 109.4 H16A C16 H16B 108.0 O2 C17 O3 122.99(15) O2 C17 C7 125.25(15) O3 C17 C7 111.68(14) O3 C18 H18A 109.5 O3 C18 H18B 109.5 O3 C18 H18C 109.5 H18A C18 H18B 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C7 C19 H19A 109.5 C7 C19 H19B 109.5 C7 C19 H19C 109.5 H19A C19 H19B 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C11 C20 H20A 109.5 C11 C20 H20B 109.5 C11 C20 H20C 109.5 H20A C20 H20B 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 C15 C21 H21A 120.0 C15 C21 H21B 120.0 H21A C21 H21B 120.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C1 1.217(2) O2 C17 1.203(2) O3 C17 1.342(2) O3 C18 1.440(2) C1 C2 1.508(2) C1 C14 1.516(2) C2 H2A 0.9900 C2 H2B 0.9900 C2 C3 1.542(2) C3 C4 1.527(2) C3 C12 1.553(2) C3 C16 1.536(2) C4 H4A 0.9900 C4 H4B 0.9900 C4 C5 1.529(2) C5 H5A 0.9900 C5 H5B 0.9900 C5 C6 1.539(2) C6 H6 1.0000 C6 C7 1.563(2) C6 C11 1.557(2) C7 C8 1.535(2) C7 C17 1.530(2) C7 C19 1.546(2) C8 H8A 0.9900 C8 H8B 0.9900 C8 C9 1.525(2) C9 H9A 0.9900 C9 H9B 0.9900 C9 C10 1.528(2) C10 H10A 0.9900 C10 H10B 0.9900 C10 C11 1.545(2) C11 C12 1.562(2) C11 C20 1.545(2) C12 H12 1.0000 C12 C13 1.556(2) C13 H13A 0.9900 C13 H13B 0.9900 C13 C14 1.547(2) C14 H14 1.0000 C14 C15 1.509(2) C15 C16 1.501(2) C15 C21 1.341(2) C16 H16A 0.9900 C16 H16B 0.9900 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 H21A 0.9500 C21 H21B 0.9500 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion O1 C1 C2 C3 -175.30(17) O1 C1 C14 C13 118.52(18) O1 C1 C14 C15 -124.58(18) C1 C2 C3 C4 178.32(13) C1 C2 C3 C12 54.34(17) C1 C2 C3 C16 -60.67(16) C1 C14 C15 C16 -60.72(17) C1 C14 C15 C21 118.05(18) C2 C1 C14 C13 -61.81(17) C2 C1 C14 C15 55.10(17) C2 C3 C4 C5 -73.96(17) C2 C3 C12 C11 76.44(16) C2 C3 C12 C13 -55.23(17) C2 C3 C16 C15 55.49(17) C3 C4 C5 C6 -58.33(17) C3 C12 C13 C14 -2.07(18) C4 C3 C12 C11 -48.89(17) C4 C3 C12 C13 179.44(12) C4 C3 C16 C15 177.87(13) C4 C5 C6 C7 -164.01(13) C4 C5 C6 C11 62.07(16) C5 C6 C7 C8 172.71(13) C5 C6 C7 C17 -64.95(19) C5 C6 C7 C19 55.12(18) C5 C6 C11 C10 -171.15(13) C5 C6 C11 C12 -56.80(16) C5 C6 C11 C20 68.17(16) C6 C7 C8 C9 55.39(19) C6 C7 C17 O2 -131.90(17) C6 C7 C17 O3 51.11(18) C6 C11 C12 C3 51.59(16) C6 C11 C12 C13 -178.85(12) C7 C6 C11 C10 53.42(17) C7 C6 C11 C12 167.76(12) C7 C6 C11 C20 -67.27(17) C7 C8 C9 C10 -56.1(2) C8 C7 C17 O2 -9.9(2) C8 C7 C17 O3 173.08(13) C8 C9 C10 C11 54.47(19) C9 C10 C11 C6 -52.73(18) C9 C10 C11 C12 -167.64(13) C9 C10 C11 C20 69.67(17) C10 C11 C12 C3 167.85(13) C10 C11 C12 C13 -62.59(16) C11 C6 C7 C8 -54.60(17) C11 C6 C7 C17 67.74(18) C11 C6 C7 C19 -172.19(13) C11 C12 C13 C14 -135.15(14) C12 C3 C4 C5 50.44(17) C12 C3 C16 C15 -62.70(16) C12 C13 C14 C1 59.27(17) C12 C13 C14 C15 -55.74(17) C13 C14 C15 C16 54.75(18) C13 C14 C15 C21 -126.49(18) C14 C1 C2 C3 5.03(19) C14 C15 C16 C3 4.79(19) C16 C3 C4 C5 167.41(13) C16 C3 C12 C11 -168.47(12) C16 C3 C12 C13 59.86(16) C17 C7 C8 C9 -70.95(17) C18 O3 C17 O2 5.0(2) C18 O3 C17 C7 -177.93(13) C19 C7 C8 C9 174.30(14) C19 C7 C17 O2 105.96(19) C19 C7 C17 O3 -71.03(16) C20 C11 C12 C3 -72.35(17) C20 C11 C12 C13 57.21(17) C21 C15 C16 C3 -173.94(17)