#------------------------------------------------------------------------------ #$Date: 2016-08-07 11:19:22 +0300 (Sun, 07 Aug 2016) $ #$Revision: 185212 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/22/51/7225198.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_7225198 loop_ _publ_author_name 'Veerakanellore, Giri Babu' 'Captain, Burjor' 'Ramamurthy, V.' _publ_section_title ; Solid-state photochemistry of cis-cinnamic acids: a competition between [2 + 2] addition and cis--trans isomerization ; _journal_issue 25 _journal_name_full CrystEngComm _journal_page_first 4708 _journal_paper_doi 10.1039/C6CE00682E _journal_volume 18 _journal_year 2016 _chemical_formula_sum 'C27.5 H28 O6' _chemical_formula_weight 454.50 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2016-03-10 deposited with the CCDC. 2016-05-11 downloaded from the CCDC. ; _cell_angle_alpha 82.4210(8) _cell_angle_beta 83.5482(9) _cell_angle_gamma 82.2157(9) _cell_formula_units_Z 2 _cell_length_a 9.9527(5) _cell_length_b 10.3401(5) _cell_length_c 12.2625(6) _cell_measurement_reflns_used 5207 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 31.23 _cell_measurement_theta_min 2.46 _cell_volume 1233.65(11) _computing_cell_refinement 'SAINT+ V8.34A (Bruker, 2015)' _computing_data_collection 'APEX2 v2.2-0 (Bruker, 2007)' _computing_data_reduction 'SAINT+ V8.34A (Bruker, 2015)' _computing_molecular_graphics 'XSHELL v6.3.1 (Bruker, 2004)' _computing_publication_material 'XCIF v2014/2 (Bruker, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS/SHELXTL V6.14 (Bruker, 2015)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker SMART APEX2 CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_unetI/netI 0.0176 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10135 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 24.999 _diffrn_reflns_theta_min 1.683 _exptl_absorpt_coefficient_mu 0.086 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_correction_T_min 0.6854 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SADABS 2014/5 Bruker)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.224 _exptl_crystal_description block _exptl_crystal_F_000 482 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.543 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 325 _refine_ls_number_reflns 4339 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0746 _refine_ls_R_factor_gt 0.0668 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1141P)^2^+0.5344P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1925 _refine_ls_wR_factor_ref 0.2028 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3690 _reflns_number_total 4339 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c6ce00682e2.cif _cod_data_source_block collect_0m _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_absorpt_correction_type' value 'Multi-scan' changed to 'multi-scan' according to /usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/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 4268 2015-11-12 08:31:59Z antanas Adding full bibliography for 7225194--7225202.cif. ; _cod_original_formula_sum 'C27.50 H28 O6' _cod_database_code 7225198 _shelx_shelxl_version_number 2014/7 _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 0.950 _shelx_estimated_absorpt_t_max 0.983 _shelx_res_file ; collect_0m.res created by SHELXL-2014/7 TITL collect_0m in P-1 CELL 0.71073 9.9527 10.3401 12.2625 82.4210 83.5482 82.2157 ZERR 2.00 0.0005 0.0005 0.0006 0.0008 0.0009 0.0009 LATT 1 SFAC C H O UNIT 55 56 12 OMIT -3 50 L.S. 4 ACTA BOND FMAP 2 PLAN 20 SIZE 0.20 0.40 0.60 SADI 0.0125 C52 C57 C56 C57 DFIX 1.5 C51 C57 TEMP 23.000 WGHT 0.114100 0.534400 FVAR 0.34168 PART 1 MOLE 1 O1 3 0.432510 0.140725 0.045358 11.00000 0.06856 0.05497 = 0.07120 -0.01862 0.02553 -0.01107 O2 3 0.393452 -0.060797 0.119849 11.00000 0.08284 0.04989 = 0.07251 -0.01913 0.02482 -0.00242 AFIX 147 H2 2 0.446131 -0.082006 0.067037 11.00000 -1.50000 AFIX 0 O3 3 0.176364 0.512556 0.092584 11.00000 0.12426 0.06044 = 0.10233 0.01113 -0.00337 -0.00085 O4 3 0.118265 0.077171 0.033446 11.00000 0.08173 0.10160 = 0.03501 -0.00824 -0.00010 -0.04513 O5 3 -0.019461 -0.036469 0.149849 11.00000 0.09132 0.09984 = 0.04124 -0.00577 -0.00503 -0.05337 AFIX 147 H5 2 -0.053402 -0.042103 0.093003 11.00000 -1.50000 AFIX 0 O6 3 -0.091569 0.428811 0.308057 11.00000 0.07718 0.07043 = 0.06223 -0.01106 0.00337 0.01590 C1 1 0.273216 0.364814 0.235904 11.00000 0.05491 0.04994 = 0.05879 -0.01974 0.01815 -0.00918 C2 1 0.255627 0.494579 0.180396 11.00000 0.08156 0.05303 = 0.09844 -0.02397 0.03040 -0.01301 C3 1 0.315084 0.590953 0.216819 11.00000 0.11381 0.06401 = 0.13859 -0.03612 0.04068 -0.03010 AFIX 43 H3 2 0.303970 0.676222 0.180997 11.00000 -1.20000 AFIX 0 C4 1 0.390607 0.562751 0.305392 11.00000 0.09893 0.08887 = 0.17543 -0.08464 0.04939 -0.04930 AFIX 43 H4 2 0.433059 0.628822 0.326831 11.00000 -1.20000 AFIX 0 C5 1 0.405708 0.437820 0.364383 11.00000 0.07503 0.11318 = 0.11992 -0.07085 0.01076 -0.02829 AFIX 43 H5A 2 0.454045 0.420660 0.426408 11.00000 -1.20000 AFIX 0 C6 1 0.345771 0.339082 0.327235 11.00000 0.06305 0.07203 = 0.08002 -0.03635 0.00596 -0.01641 AFIX 43 H6 2 0.355035 0.254630 0.364803 11.00000 -1.20000 AFIX 0 C7 1 0.211048 0.260573 0.192142 11.00000 0.05221 0.04685 = 0.03697 -0.00754 0.00573 -0.00228 AFIX 13 H7 2 0.200627 0.287348 0.113554 11.00000 -1.20000 AFIX 0 C8 1 0.276261 0.116684 0.206271 11.00000 0.04688 0.04628 = 0.03859 -0.01176 -0.00217 -0.00252 AFIX 13 H8 2 0.319817 0.099543 0.275416 11.00000 -1.20000 AFIX 0 C9 1 0.374312 0.065865 0.115474 11.00000 0.04644 0.04849 = 0.04837 -0.01488 0.00073 -0.00477 C10 1 0.145523 0.640677 0.035388 11.00000 0.13279 0.07529 = 0.15085 0.02128 0.00746 0.01181 AFIX 23 H10A 2 0.124445 0.703124 0.089197 11.00000 -1.20000 H10B 2 0.064579 0.642038 -0.002243 11.00000 -1.20000 AFIX 0 C11 1 0.252408 0.683100 -0.043896 11.00000 0.20386 0.12016 = 0.12164 0.02979 0.01280 -0.05999 AFIX 43 H11 2 0.230688 0.771537 -0.069008 11.00000 -1.20000 AFIX 0 C12 1 0.350541 0.646749 -0.084707 11.00000 0.24000 0.51553 = 0.29912 -0.26903 0.17131 -0.25735 AFIX 93 H12A 2 0.386897 0.559494 -0.068487 11.00000 -1.20000 H12B 2 0.397988 0.702960 -0.135778 11.00000 -1.20000 AFIX 0 C21 1 0.038004 0.232437 0.369734 11.00000 0.04152 0.05745 = 0.03925 -0.01359 0.00477 -0.01011 C22 1 -0.050278 0.343480 0.395960 11.00000 0.05321 0.06038 = 0.05136 -0.01173 0.00678 -0.00767 C23 1 -0.089226 0.361780 0.506097 11.00000 0.07707 0.07377 = 0.06074 -0.02525 0.01886 -0.00193 AFIX 43 H23 2 -0.150174 0.434255 0.523472 11.00000 -1.20000 AFIX 0 C24 1 -0.037650 0.272814 0.589098 11.00000 0.09377 0.09124 = 0.04295 -0.02216 0.01841 -0.01848 AFIX 43 H24 2 -0.064220 0.285698 0.662429 11.00000 -1.20000 AFIX 0 C25 1 0.051506 0.166403 0.565636 11.00000 0.07614 0.08098 = 0.03895 -0.00907 0.00315 -0.01601 AFIX 43 H25 2 0.087412 0.107697 0.622308 11.00000 -1.20000 AFIX 0 C26 1 0.088386 0.146292 0.456207 11.00000 0.05519 0.06558 = 0.04095 -0.00980 0.00019 -0.00703 AFIX 43 H26 2 0.148730 0.072804 0.440372 11.00000 -1.20000 AFIX 0 C27 1 0.073356 0.212959 0.249765 11.00000 0.04350 0.05505 = 0.03670 -0.00945 -0.00212 -0.00098 AFIX 13 H27 2 -0.003101 0.246798 0.205944 11.00000 -1.20000 AFIX 0 C28 1 0.133456 0.069832 0.227009 11.00000 0.05013 0.04988 = 0.03274 -0.00776 0.00008 -0.00712 AFIX 13 H28 2 0.123356 0.004050 0.291705 11.00000 -1.20000 AFIX 0 C29 1 0.078681 0.036337 0.127089 11.00000 0.05199 0.05059 = 0.03789 -0.00983 0.00193 -0.01048 C30 1 -0.198848 0.531754 0.326240 11.00000 0.07697 0.06953 = 0.09996 -0.01570 0.00470 0.01045 AFIX 23 H30A 2 -0.175201 0.585420 0.378710 11.00000 -1.20000 H30B 2 -0.281805 0.495100 0.356331 11.00000 -1.20000 AFIX 0 C31 1 -0.219866 0.612051 0.220533 11.00000 0.14909 0.08857 = 0.11984 -0.01494 -0.03583 0.04975 AFIX 43 H31 2 -0.201440 0.562923 0.161117 11.00000 -1.20000 AFIX 0 C32 1 -0.253247 0.719868 0.193615 11.00000 0.16723 0.14416 = 0.15495 0.02854 0.01836 0.02753 AFIX 93 H32A 2 -0.274452 0.778634 0.246043 11.00000 -1.20000 H32B 2 -0.259382 0.749404 0.119142 11.00000 -1.20000 PART -1 AFIX 66 C51 1 0.432602 0.946647 0.529892 10.50000 0.14956 0.09538 = 0.32986 0.04987 -0.11494 0.00081 C52 1 0.476670 1.039392 0.585567 10.50000 0.14649 0.15877 = 0.13463 -0.01123 -0.05876 0.07125 AFIX 43 H52 2 0.438132 1.052122 0.656613 10.50000 -1.20000 AFIX 65 C53 1 0.578337 1.113111 0.535057 10.50000 0.17444 0.12308 = 0.22305 -0.06903 -0.11059 0.05641 AFIX 43 H53 2 0.607821 1.175164 0.572308 10.50000 -1.20000 AFIX 65 C54 1 0.635937 1.094085 0.428871 10.50000 0.14749 0.15466 = 0.36727 0.10311 -0.08069 0.02879 AFIX 43 H54 2 0.703959 1.143408 0.395077 10.50000 -1.20000 AFIX 65 C55 1 0.591870 1.001341 0.373195 10.50000 0.21435 0.15738 = 0.26303 -0.06420 -0.13685 0.07929 AFIX 43 H55 2 0.630408 0.988611 0.302149 10.50000 -1.20000 AFIX 65 C56 1 0.490203 0.927621 0.423704 10.50000 0.11977 0.21744 = 0.32405 0.12348 -0.05306 -0.00587 AFIX 43 H56 2 0.460719 0.865568 0.386452 10.50000 -1.20000 PART 0 AFIX 0 C57 1 0.331188 0.865557 0.585393 10.50000 0.13833 0.20071 = 0.81728 0.17729 -0.04074 0.01399 AFIX 137 H57A 2 0.370961 0.804330 0.642269 10.50000 -1.50000 H57B 2 0.299872 0.818264 0.532815 10.50000 -1.50000 H57C 2 0.255698 0.920477 0.617783 10.50000 -1.50000 AFIX 0 HKLF 4 REM collect_0m in P-1 REM R1 = 0.0668 for 3690 Fo > 4sig(Fo) and 0.0746 for all 4339 data REM 325 parameters refined using 2 restraints END WGHT 0.1120 0.5454 REM Highest difference peak 0.543, deepest hole -0.406, 1-sigma level 0.051 Q1 1 0.2826 0.5229 0.1038 11.00000 0.05 0.54 Q2 1 0.2665 0.6554 0.0591 11.00000 0.05 0.41 Q3 1 0.3703 0.6198 -0.0686 11.00000 0.05 0.39 Q4 1 -0.1314 0.6316 0.1412 11.00000 0.05 0.39 Q5 1 0.2862 0.7780 -0.0909 11.00000 0.05 0.27 Q6 1 0.3347 0.4896 0.2054 11.00000 0.05 0.25 Q7 1 0.6103 1.0267 0.3935 11.00000 0.05 0.21 Q8 1 0.4336 0.5401 0.3776 11.00000 0.05 0.20 Q9 1 0.1455 0.0072 0.0539 11.00000 0.05 0.18 Q10 1 0.2037 0.0760 0.2174 11.00000 0.05 0.17 Q11 1 0.2736 0.7047 -0.1657 11.00000 0.05 0.16 Q12 1 0.2539 0.3115 0.2182 11.00000 0.05 0.16 Q13 1 0.2428 0.6022 -0.0696 11.00000 0.05 0.16 Q14 1 0.2445 0.4511 0.1783 11.00000 0.05 0.16 Q15 1 0.0577 0.1199 0.0724 11.00000 0.05 0.15 Q16 1 0.1627 0.1153 0.0158 11.00000 0.05 0.15 Q17 1 -0.0443 0.0592 0.1397 11.00000 0.05 0.15 Q18 1 -0.1412 0.6541 0.2383 11.00000 0.05 0.14 Q19 1 -0.3241 0.6344 0.1536 11.00000 0.05 0.14 Q20 1 0.0894 0.1183 0.2457 11.00000 0.05 0.14 ; _shelx_res_checksum 47376 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.43251(18) 0.14073(16) 0.04536(15) 0.0661(5) Uani 1 1 d . . . A 1 O2 O 0.3935(2) -0.06080(16) 0.11985(15) 0.0704(5) Uani 1 1 d . . . A 1 H2 H 0.4461 -0.0820 0.0670 0.106 Uiso 1 1 calc R U . A 1 O3 O 0.1764(3) 0.5126(2) 0.0926(2) 0.0991(7) Uani 1 1 d . . . A 1 O4 O 0.11827(19) 0.0772(2) 0.03345(12) 0.0700(5) Uani 1 1 d . . . A 1 O5 O -0.0195(2) -0.0365(2) 0.14985(13) 0.0739(6) Uani 1 1 d . . . A 1 H5 H -0.0534 -0.0421 0.0930 0.111 Uiso 1 1 calc R U . A 1 O6 O -0.0916(2) 0.42881(19) 0.30806(15) 0.0728(5) Uani 1 1 d . . . A 1 C1 C 0.2732(2) 0.3648(2) 0.23590(19) 0.0549(6) Uani 1 1 d . . . A 1 C2 C 0.2556(3) 0.4946(3) 0.1804(3) 0.0789(9) Uani 1 1 d . . . A 1 C3 C 0.3151(5) 0.5910(3) 0.2168(4) 0.1056(13) Uani 1 1 d . . . A 1 H3 H 0.3040 0.6762 0.1810 0.127 Uiso 1 1 calc R U . A 1 C4 C 0.3906(4) 0.5628(4) 0.3054(5) 0.1161(17) Uani 1 1 d . . . A 1 H4 H 0.4331 0.6288 0.3268 0.139 Uiso 1 1 calc R U . A 1 C5 C 0.4057(3) 0.4378(4) 0.3644(3) 0.0975(12) Uani 1 1 d . . . A 1 H5A H 0.4540 0.4207 0.4264 0.117 Uiso 1 1 calc R U . A 1 C6 C 0.3458(3) 0.3391(3) 0.3272(2) 0.0695(7) Uani 1 1 d . . . A 1 H6 H 0.3550 0.2546 0.3648 0.083 Uiso 1 1 calc R U . A 1 C7 C 0.2110(2) 0.2606(2) 0.19214(16) 0.0462(5) Uani 1 1 d . . . A 1 H7 H 0.2006 0.2873 0.1136 0.055 Uiso 1 1 calc R U . A 1 C8 C 0.2763(2) 0.1167(2) 0.20627(16) 0.0438(5) Uani 1 1 d . . . A 1 H8 H 0.3198 0.0995 0.2754 0.053 Uiso 1 1 calc R U . A 1 C9 C 0.3743(2) 0.0659(2) 0.11547(18) 0.0474(5) Uani 1 1 d . . . A 1 C10 C 0.1455(5) 0.6407(4) 0.0354(4) 0.1267(16) Uani 1 1 d . . . A 1 H10A H 0.1244 0.7031 0.0892 0.152 Uiso 1 1 calc R U . A 1 H10B H 0.0646 0.6420 -0.0022 0.152 Uiso 1 1 calc R U . A 1 C11 C 0.2524(8) 0.6831(6) -0.0439(5) 0.151(2) Uani 1 1 d . . . A 1 H11 H 0.2307 0.7715 -0.0690 0.181 Uiso 1 1 calc R U . A 1 C12 C 0.3505(10) 0.6467(13) -0.0847(8) 0.327(9) Uani 1 1 d . . . A 1 H12A H 0.3869 0.5595 -0.0685 0.393 Uiso 1 1 calc R U . A 1 H12B H 0.3980 0.7030 -0.1358 0.393 Uiso 1 1 calc R U . A 1 C21 C 0.0380(2) 0.2324(2) 0.36973(16) 0.0457(5) Uani 1 1 d . . . A 1 C22 C -0.0503(2) 0.3435(2) 0.39596(19) 0.0554(6) Uani 1 1 d . . . A 1 C23 C -0.0892(3) 0.3618(3) 0.5061(2) 0.0716(7) Uani 1 1 d . . . A 1 H23 H -0.1502 0.4343 0.5235 0.086 Uiso 1 1 calc R U . A 1 C24 C -0.0376(3) 0.2728(3) 0.5891(2) 0.0760(8) Uani 1 1 d . . . A 1 H24 H -0.0642 0.2857 0.6624 0.091 Uiso 1 1 calc R U . A 1 C25 C 0.0515(3) 0.1664(3) 0.56564(19) 0.0653(7) Uani 1 1 d . . . A 1 H25 H 0.0874 0.1077 0.6223 0.078 Uiso 1 1 calc R U . A 1 C26 C 0.0884(2) 0.1463(2) 0.45621(17) 0.0540(5) Uani 1 1 d . . . A 1 H26 H 0.1487 0.0728 0.4404 0.065 Uiso 1 1 calc R U . A 1 C27 C 0.0734(2) 0.2130(2) 0.24977(16) 0.0453(5) Uani 1 1 d . . . A 1 H27 H -0.0031 0.2468 0.2059 0.054 Uiso 1 1 calc R U . A 1 C28 C 0.1335(2) 0.0698(2) 0.22701(15) 0.0442(5) Uani 1 1 d . . . A 1 H28 H 0.1234 0.0041 0.2917 0.053 Uiso 1 1 calc R U . A 1 C29 C 0.0787(2) 0.0363(2) 0.12709(16) 0.0465(5) Uani 1 1 d . . . A 1 C30 C -0.1988(3) 0.5318(3) 0.3262(3) 0.0845(9) Uani 1 1 d . . . A 1 H30A H -0.1752 0.5854 0.3787 0.101 Uiso 1 1 calc R U . A 1 H30B H -0.2818 0.4951 0.3563 0.101 Uiso 1 1 calc R U . A 1 C31 C -0.2199(5) 0.6121(4) 0.2205(4) 0.1232(16) Uani 1 1 d . . . A 1 H31 H -0.2014 0.5629 0.1611 0.148 Uiso 1 1 calc R U . A 1 C32 C -0.2532(6) 0.7199(6) 0.1936(5) 0.167(2) Uani 1 1 d . . . A 1 H32A H -0.2745 0.7786 0.2460 0.200 Uiso 1 1 calc R U . A 1 H32B H -0.2594 0.7494 0.1191 0.200 Uiso 1 1 calc R U . A 1 C51 C 0.4326(16) 0.9466(14) 0.530(2) 0.193(11) Uani 0.5 1 d DG . P B -1 C52 C 0.4767(18) 1.0394(16) 0.5856(14) 0.152(8) Uani 0.5 1 d DG . P B -1 H52 H 0.4381 1.0521 0.6566 0.182 Uiso 0.5 1 calc R U P B -1 C53 C 0.5783(18) 1.1131(11) 0.535(2) 0.169(10) Uani 0.5 1 d G . P B -1 H53 H 0.6078 1.1752 0.5723 0.203 Uiso 0.5 1 calc R U P B -1 C54 C 0.6359(16) 1.0941(17) 0.429(2) 0.235(17) Uani 0.5 1 d G . P B -1 H54 H 0.7040 1.1434 0.3951 0.282 Uiso 0.5 1 calc R U P B -1 C55 C 0.592(2) 1.001(2) 0.3732(15) 0.209(13) Uani 0.5 1 d G . P B -1 H55 H 0.6304 0.9886 0.3021 0.251 Uiso 0.5 1 calc R U P B -1 C56 C 0.490(2) 0.9276(14) 0.4237(19) 0.233(16) Uani 0.5 1 d DG . P B -1 H56 H 0.4607 0.8656 0.3865 0.280 Uiso 0.5 1 calc R U P B -1 C57 C 0.331(3) 0.866(3) 0.585(3) 0.41(4) Uani 0.5 1 d D . P . . H57A H 0.3710 0.8043 0.6423 0.616 Uiso 0.5 1 calc R U P B . H57B H 0.2999 0.8183 0.5328 0.616 Uiso 0.5 1 calc R U P . . H57C H 0.2557 0.9205 0.6178 0.616 Uiso 0.5 1 calc R U P . . 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 0.0686(11) 0.0550(10) 0.0712(11) -0.0186(8) 0.0255(9) -0.0111(8) O2 0.0828(12) 0.0499(9) 0.0725(12) -0.0191(8) 0.0248(9) -0.0024(8) O3 0.1243(19) 0.0604(12) 0.1023(17) 0.0111(11) -0.0034(15) -0.0009(12) O4 0.0817(12) 0.1016(14) 0.0350(8) -0.0082(8) -0.0001(7) -0.0451(10) O5 0.0913(13) 0.0998(14) 0.0412(9) -0.0058(9) -0.0050(8) -0.0534(11) O6 0.0772(12) 0.0704(11) 0.0622(11) -0.0111(9) 0.0034(9) 0.0159(9) C1 0.0549(13) 0.0499(12) 0.0588(13) -0.0197(10) 0.0181(10) -0.0092(9) C2 0.0816(19) 0.0530(15) 0.098(2) -0.0240(14) 0.0304(17) -0.0130(13) C3 0.114(3) 0.064(2) 0.139(3) -0.036(2) 0.041(3) -0.0301(19) C4 0.099(3) 0.089(3) 0.175(4) -0.085(3) 0.049(3) -0.049(2) C5 0.0750(19) 0.113(3) 0.120(3) -0.071(2) 0.0108(18) -0.0283(18) C6 0.0630(15) 0.0720(16) 0.0800(18) -0.0363(14) 0.0060(13) -0.0164(12) C7 0.0522(11) 0.0469(11) 0.0370(10) -0.0075(8) 0.0057(8) -0.0023(9) C8 0.0469(11) 0.0463(11) 0.0386(10) -0.0118(8) -0.0022(8) -0.0025(8) C9 0.0464(11) 0.0485(12) 0.0484(11) -0.0149(9) 0.0007(9) -0.0048(9) C10 0.133(3) 0.075(2) 0.151(4) 0.021(2) 0.007(3) 0.012(2) C11 0.204(6) 0.120(4) 0.122(4) 0.030(3) 0.013(4) -0.060(4) C12 0.240(9) 0.516(19) 0.299(12) -0.269(13) 0.171(9) -0.257(12) C21 0.0415(10) 0.0574(12) 0.0392(10) -0.0136(9) 0.0048(8) -0.0101(9) C22 0.0532(12) 0.0604(14) 0.0514(13) -0.0117(10) 0.0068(10) -0.0077(10) C23 0.0771(17) 0.0738(17) 0.0607(15) -0.0253(13) 0.0189(13) -0.0019(13) C24 0.094(2) 0.091(2) 0.0429(13) -0.0222(13) 0.0184(13) -0.0185(16) C25 0.0761(16) 0.0810(17) 0.0389(12) -0.0091(11) 0.0032(11) -0.0160(13) C26 0.0552(12) 0.0656(14) 0.0410(11) -0.0098(10) 0.0002(9) -0.0070(10) C27 0.0435(11) 0.0550(12) 0.0367(10) -0.0094(8) -0.0021(8) -0.0010(9) C28 0.0501(11) 0.0499(11) 0.0327(9) -0.0078(8) 0.0001(8) -0.0071(9) C29 0.0520(11) 0.0506(11) 0.0379(11) -0.0098(8) 0.0019(8) -0.0105(9) C30 0.0770(18) 0.0695(17) 0.100(2) -0.0157(16) 0.0047(16) 0.0104(14) C31 0.149(4) 0.089(3) 0.120(3) -0.015(2) -0.036(3) 0.050(3) C32 0.167(5) 0.144(5) 0.155(5) 0.029(4) 0.018(4) 0.028(4) C51 0.15(2) 0.095(11) 0.33(3) 0.050(18) -0.11(2) 0.001(11) C52 0.146(15) 0.159(19) 0.135(12) -0.011(12) -0.059(12) 0.071(14) C53 0.174(19) 0.123(13) 0.22(2) -0.069(15) -0.111(16) 0.056(12) C54 0.15(3) 0.15(3) 0.37(5) 0.10(3) -0.08(3) 0.03(2) C55 0.21(2) 0.157(18) 0.26(3) -0.064(18) -0.14(2) 0.079(16) C56 0.120(15) 0.22(2) 0.32(4) 0.12(2) -0.053(17) -0.006(15) C57 0.138(16) 0.20(2) 0.82(10) 0.18(4) -0.04(3) 0.014(17) 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' O O 0.0106 0.0060 '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 C2 O3 C10 120.1(3) C22 O6 C30 119.1(2) C6 C1 C2 119.5(3) C6 C1 C7 122.4(2) C2 C1 C7 118.1(2) C3 C2 O3 125.3(3) C3 C2 C1 119.2(4) O3 C2 C1 115.5(2) C4 C3 C2 120.5(4) C3 C4 C5 121.8(3) C4 C5 C6 117.8(4) C1 C6 C5 121.1(3) C1 C7 C8 120.54(19) C1 C7 C27 120.76(16) C8 C7 C27 88.27(15) C9 C8 C7 119.26(17) C9 C8 C28 118.92(16) C7 C8 C28 90.39(15) O1 C9 O2 124.25(19) O1 C9 C8 121.35(19) O2 C9 C8 114.38(19) O3 C10 C11 114.5(4) C12 C11 C10 141.3(9) C26 C21 C22 117.77(19) C26 C21 C27 123.64(19) C22 C21 C27 118.59(19) O6 C22 C23 124.3(2) O6 C22 C21 115.62(19) C23 C22 C21 120.0(2) C24 C23 C22 120.0(2) C25 C24 C23 121.0(2) C24 C25 C26 119.2(2) C21 C26 C25 121.9(2) C21 C27 C28 115.49(17) C21 C27 C7 116.92(17) C28 C27 C7 88.08(14) C29 C28 C8 115.10(16) C29 C28 C27 109.88(17) C8 C28 C27 88.31(15) O4 C29 O5 122.81(19) O4 C29 C28 123.42(19) O5 C29 C28 113.71(17) O6 C30 C31 108.5(3) C32 C31 C30 135.4(6) C52 C51 C56 120.0 C52 C51 C57 119.6(5) C56 C51 C57 120.4(5) C53 C52 C51 120.0 C52 C53 C54 120.0 C55 C54 C53 120.0 C54 C55 C56 120.0 C55 C56 C51 120.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C9 1.228(3) O2 C9 1.293(3) O3 C2 1.384(4) O3 C10 1.426(4) O4 C29 1.211(2) O5 C29 1.297(3) O6 C22 1.364(3) O6 C30 1.423(3) C1 C6 1.378(4) C1 C2 1.420(4) C1 C7 1.497(3) C2 C3 1.371(5) C3 C4 1.368(7) C4 C5 1.393(7) C5 C6 1.398(4) C7 C8 1.536(3) C7 C27 1.579(3) C8 C9 1.496(3) C8 C28 1.547(3) C10 C11 1.432(7) C11 C12 1.089(10) C21 C26 1.385(3) C21 C22 1.398(3) C21 C27 1.507(3) C22 C23 1.393(3) C23 C24 1.374(4) C24 C25 1.357(4) C25 C26 1.386(3) C27 C28 1.568(3) C28 C29 1.494(3) C30 C31 1.464(5) C31 C32 1.136(6) C51 C52 1.3900 C51 C56 1.3900 C51 C57 1.452(18) C52 C53 1.3900 C53 C54 1.3900 C54 C55 1.3900 C55 C56 1.3900