#------------------------------------------------------------------------------ #$Date: 2019-11-08 04:02:53 +0200 (Fri, 08 Nov 2019) $ #$Revision: 225275 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/15/70/7157039.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_7157039 loop_ _publ_author_name 'Verma, Kamal' 'Taily, Irshad Maajid' 'Banerjee, Prabal' _publ_section_title ; Exploitation of donor-acceptor cyclopropanes and N-sulfonyl 1-azadienes towards the synthesis of spiro-cyclopentane benzofuran derivatives. ; _journal_issue 35 _journal_name_full 'Organic & biomolecular chemistry' _journal_page_first 8149 _journal_page_last 8152 _journal_paper_doi 10.1039/c9ob01369e _journal_volume 17 _journal_year 2019 _chemical_formula_sum 'C31 H30 O7' _chemical_formula_weight 514.55 _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 ; 2018-08-20 deposited with the CCDC. 2019-08-16 downloaded from the CCDC. ; _cell_angle_alpha 95.665(5) _cell_angle_beta 97.294(5) _cell_angle_gamma 99.247(5) _cell_formula_units_Z 2 _cell_length_a 9.539(5) _cell_length_b 9.870(5) _cell_length_c 15.022(5) _cell_measurement_reflns_used 6760 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 28.3 _cell_measurement_theta_min 2.2 _cell_volume 1374.4(11) _computing_cell_refinement 'APEX2 (Bruker, 2014); SAINT (Bruker, 2014)' _computing_data_collection 'APEX2 (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2014);XPREP(Sheldrick,2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 10.233 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measurement_device_type 'Bruker D8 Venture PHOTON 100 CMOS' _diffrn_measurement_method 'phi and omega scan' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_unetI/netI 0.0754 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 24174 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.312 _diffrn_reflns_theta_min 2.186 _diffrn_source 'fine-focus sealed tube' _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_meas ? _exptl_crystal_description block _exptl_crystal_F_000 544 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.314 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.043 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 343 _refine_ls_number_reflns 6760 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.037 _refine_ls_R_factor_all 0.1477 _refine_ls_R_factor_gt 0.0806 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0764P)^2^+0.7131P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1970 _refine_ls_wR_factor_ref 0.2320 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3531 _reflns_number_total 6760 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ob01369e2.cif _cod_data_source_block shelx_CCDC1 _cod_depositor_comments ; The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas Adding full bibliography for 7157038--7157039.cif. ; _cod_database_code 7157039 _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_res_file ; shelx.res created by SHELXL-2014/7 TITL PB_KV_129P-1 in P-1 CELL 0.71073 9.5390 9.8700 15.0220 95.665 97.294 99.247 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H O UNIT 62 60 14 MERG 2 FMAP 2 PLAN 25 ACTA L.S. 4 WGHT 0.076400 0.713100 FVAR 0.39400 O1 3 0.700228 -0.105309 0.239438 11.00000 0.06022 0.05155 = 0.05425 0.01377 0.01611 0.00085 O5 3 0.740081 0.230769 0.484792 11.00000 0.08310 0.07507 = 0.07338 0.00490 0.03586 0.00896 O3 3 1.013368 0.358638 0.357516 11.00000 0.09041 0.06508 = 0.07346 0.01816 0.00974 -0.01276 O6 3 0.744241 0.004692 0.477915 11.00000 0.08679 0.07410 = 0.08339 0.03752 0.02702 0.00513 O7 3 1.136680 -0.471517 0.097866 11.00000 0.11104 0.06216 = 0.11693 0.00473 0.05122 0.02029 O4 3 1.042479 0.282002 0.492186 11.00000 0.07553 0.07171 = 0.07604 0.01550 -0.01630 -0.00741 O2 3 0.827283 0.120502 0.088658 11.00000 0.10738 0.08686 = 0.06765 0.03739 0.02432 0.00707 C5 1 0.779449 0.145960 0.285363 11.00000 0.04996 0.05042 = 0.05228 0.01796 0.01204 0.00674 AFIX 13 H5 2 0.831194 0.223384 0.259767 11.00000 -1.20000 AFIX 0 C6 1 0.630273 0.177328 0.286009 11.00000 0.05407 0.05442 = 0.04454 0.00884 0.00607 0.01238 C1 1 0.873659 0.140668 0.379330 11.00000 0.04938 0.05197 = 0.04908 0.01270 0.00855 0.00792 C4 1 0.797015 0.016973 0.225960 11.00000 0.05150 0.05130 = 0.04897 0.01728 0.01357 0.00649 C3 1 0.953075 0.000736 0.258585 11.00000 0.05144 0.05128 = 0.06262 0.01698 0.01296 0.00973 AFIX 13 H3 2 1.016394 0.080107 0.242404 11.00000 -1.20000 AFIX 0 C25 1 0.769052 0.026626 0.124454 11.00000 0.06856 0.06467 = 0.05679 0.02228 0.01987 0.01795 C2 1 0.957324 0.021627 0.360904 11.00000 0.06028 0.05760 = 0.05757 0.01242 0.00319 0.01622 AFIX 23 H2A 2 1.055594 0.046245 0.391135 11.00000 -1.20000 H2B 2 0.912103 -0.062011 0.382074 11.00000 -1.20000 AFIX 0 C31 1 0.629500 -0.166155 0.156981 11.00000 0.05507 0.05803 = 0.06258 0.00113 0.01343 0.00920 C18 1 0.999439 -0.127707 0.218617 11.00000 0.05329 0.05590 = 0.05818 0.01402 0.01483 0.01200 C21 1 1.086720 -0.362584 0.139090 11.00000 0.06783 0.05952 = 0.07545 0.00716 0.02245 0.01380 C26 1 0.664396 -0.093455 0.086217 11.00000 0.06623 0.07388 = 0.05267 0.00242 0.00816 0.02357 C15 1 0.981083 0.273748 0.406628 11.00000 0.05476 0.05456 = 0.06266 0.01004 0.01108 0.01012 C20 1 1.127898 -0.236128 0.111830 11.00000 0.08258 0.06805 = 0.07431 0.01479 0.04028 0.01290 AFIX 43 H20 2 1.186103 -0.227979 0.066763 11.00000 -1.20000 AFIX 0 C11 1 0.602633 0.303837 0.264835 11.00000 0.06954 0.06585 = 0.07408 0.01846 0.01496 0.02026 AFIX 43 H11 2 0.676324 0.367606 0.250027 11.00000 -1.20000 AFIX 0 C19 1 1.084479 -0.121520 0.150072 11.00000 0.06734 0.05656 = 0.07241 0.01705 0.02541 0.00660 AFIX 43 H19 2 1.112651 -0.036807 0.129640 11.00000 -1.20000 AFIX 0 C22 1 1.000418 -0.374041 0.206598 11.00000 0.09152 0.06156 = 0.09819 0.03206 0.04398 0.01968 AFIX 43 H22 2 0.970849 -0.459488 0.225688 11.00000 -1.20000 AFIX 0 C30 1 0.531267 -0.287366 0.144849 11.00000 0.07658 0.07190 = 0.09738 -0.01028 0.03247 0.00223 AFIX 43 H30 2 0.509033 -0.334914 0.193104 11.00000 -1.20000 AFIX 0 C12 1 0.780288 0.114902 0.453503 11.00000 0.05585 0.06404 = 0.05160 0.01377 0.00689 0.00517 C7 1 0.516364 0.084964 0.306907 11.00000 0.05546 0.07044 = 0.08729 0.02076 0.01705 0.00989 AFIX 43 H7 2 0.530935 -0.002014 0.320643 11.00000 -1.20000 AFIX 0 C9 1 0.357165 0.246690 0.287001 11.00000 0.06281 0.11158 = 0.09616 0.01711 0.01162 0.03641 AFIX 43 H9 2 0.266705 0.270163 0.287856 11.00000 -1.20000 AFIX 0 C10 1 0.467086 0.338534 0.265067 11.00000 0.09057 0.08413 = 0.10405 0.02956 0.01600 0.04193 AFIX 43 H10 2 0.451063 0.424593 0.250239 11.00000 -1.20000 AFIX 0 C17 1 1.286864 0.361474 0.546055 11.00000 0.07369 0.10646 = 0.19892 0.00551 -0.00916 0.00167 AFIX 33 H17A 2 1.358091 0.440944 0.570722 11.00000 -1.50000 H17B 2 1.283544 0.294470 0.588267 11.00000 -1.50000 H17C 2 1.311098 0.321625 0.490356 11.00000 -1.50000 AFIX 0 C16 1 1.152059 0.401533 0.529700 11.00000 0.08775 0.07030 = 0.11249 0.00600 -0.01943 -0.00249 AFIX 23 H16A 2 1.155511 0.470128 0.487655 11.00000 -1.20000 H16B 2 1.127901 0.442918 0.585766 11.00000 -1.20000 AFIX 0 C27 1 0.597694 -0.145080 -0.002017 11.00000 0.09922 0.11630 = 0.05918 -0.00519 0.00337 0.03654 AFIX 43 H27 2 0.619475 -0.098308 -0.050674 11.00000 -1.20000 AFIX 0 C23 1 0.959081 -0.256338 0.245038 11.00000 0.09467 0.06716 = 0.09032 0.03135 0.05225 0.02991 AFIX 43 H23 2 0.901728 -0.264290 0.290560 11.00000 -1.20000 AFIX 0 C28 1 0.500929 -0.264406 -0.014948 11.00000 0.09708 0.12878 = 0.08699 -0.03800 -0.00864 0.01998 AFIX 43 H28 2 0.456227 -0.299795 -0.073128 11.00000 -1.20000 AFIX 0 C29 1 0.467634 -0.334427 0.057228 11.00000 0.08533 0.10130 = 0.11829 -0.04026 0.01746 -0.00598 AFIX 43 H29 2 0.400275 -0.415704 0.046264 11.00000 -1.20000 AFIX 0 C24 1 1.079576 -0.606499 0.112615 11.00000 0.14956 0.05879 = 0.11619 0.00641 0.03800 0.02068 AFIX 33 H24A 2 1.124559 -0.671539 0.079620 11.00000 -1.50000 H24B 2 1.097136 -0.615141 0.175983 11.00000 -1.50000 H24C 2 0.978041 -0.624990 0.092314 11.00000 -1.50000 AFIX 0 C8 1 0.381865 0.120089 0.307633 11.00000 0.05311 0.09921 = 0.10967 0.01978 0.01580 0.01355 AFIX 43 H8 2 0.307530 0.056916 0.322308 11.00000 -1.20000 AFIX 0 C13 1 0.640671 0.219498 0.550412 11.00000 0.13948 0.13303 = 0.13411 -0.00255 0.09487 0.00513 AFIX 23 H13A 2 0.546988 0.229766 0.521084 11.00000 -1.20000 H13B 2 0.631818 0.127255 0.568597 11.00000 -1.20000 AFIX 0 C14 1 0.675774 0.308420 0.622415 11.00000 0.17644 0.28665 = 0.10170 -0.06481 0.08080 -0.05105 AFIX 33 H14A 2 0.604253 0.293172 0.661626 11.00000 -1.50000 H14B 2 0.767047 0.297622 0.653294 11.00000 -1.50000 H14C 2 0.682033 0.400356 0.605678 11.00000 -1.50000 AFIX 0 HKLF 4 REM PB_KV_129P-1 in P-1 REM R1 = 0.0806 for 3531 Fo > 4sig(Fo) and 0.1477 for all 6760 data REM 343 parameters refined using 0 restraints END WGHT 0.0756 0.7177 REM Highest difference peak 0.314, deepest hole -0.238, 1-sigma level 0.043 Q1 1 1.2019 0.3794 0.4757 11.00000 0.05 0.31 Q2 1 1.2325 0.4187 0.6030 11.00000 0.05 0.25 Q3 1 0.5627 0.1312 0.5182 11.00000 0.05 0.23 Q4 1 0.5935 0.3411 0.5182 11.00000 0.05 0.21 Q5 1 0.7567 0.4087 0.6368 11.00000 0.05 0.18 Q6 1 0.5582 0.0042 0.3688 11.00000 0.05 0.17 Q7 1 0.4080 -0.1710 -0.1108 11.00000 0.05 0.16 Q8 1 0.7157 0.3655 0.5015 11.00000 0.05 0.15 Q9 1 0.5283 -0.0974 0.1166 11.00000 0.05 0.15 Q10 1 0.8603 0.2013 0.2456 11.00000 0.05 0.15 Q11 1 0.5623 0.2971 0.6462 11.00000 0.05 0.15 Q12 1 0.6892 -0.0468 -0.0200 11.00000 0.05 0.14 Q13 1 0.6563 -0.1168 0.3931 11.00000 0.05 0.14 Q14 1 1.1327 0.4986 0.5097 11.00000 0.05 0.14 Q15 1 0.5569 0.0449 -0.0717 11.00000 0.05 0.14 Q16 1 1.2916 0.3975 0.4520 11.00000 0.05 0.14 Q17 1 0.6470 -0.1151 0.1199 11.00000 0.05 0.14 Q18 1 1.0747 0.1784 0.4873 11.00000 0.05 0.13 Q19 1 0.5768 -0.3550 0.2292 11.00000 0.05 0.13 Q20 1 1.0818 0.2082 0.4490 11.00000 0.05 0.13 Q21 1 0.6122 -0.0572 -0.0273 11.00000 0.05 0.13 Q22 1 0.5403 0.4158 0.2697 11.00000 0.05 0.13 Q23 1 0.9971 0.3197 0.2999 11.00000 0.05 0.13 Q24 1 0.8254 -0.0923 0.3835 11.00000 0.05 0.13 Q25 1 0.6577 0.0138 -0.0752 11.00000 0.05 0.13 ; _shelx_res_checksum 99785 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 O1 O 0.7002(2) -0.1053(2) 0.23944(13) 0.0552(5) Uani 1 1 d . . O5 O 0.7401(3) 0.2308(3) 0.48479(16) 0.0759(7) Uani 1 1 d . . O3 O 1.0134(3) 0.3586(2) 0.35752(16) 0.0788(7) Uani 1 1 d . . O6 O 0.7442(3) 0.0047(3) 0.47792(17) 0.0792(7) Uani 1 1 d . . O7 O 1.1367(3) -0.4715(3) 0.0979(2) 0.0935(8) Uani 1 1 d . . O4 O 1.0425(2) 0.2820(2) 0.49219(16) 0.0787(7) Uani 1 1 d . . O2 O 0.8273(3) 0.1205(3) 0.08866(16) 0.0855(8) Uani 1 1 d . . C5 C 0.7794(3) 0.1460(3) 0.28536(18) 0.0499(7) Uani 1 1 d . . H5 H 0.8312 0.2234 0.2598 0.060 Uiso 1 1 calc R U C6 C 0.6303(3) 0.1773(3) 0.28601(18) 0.0506(7) Uani 1 1 d . . C1 C 0.8737(3) 0.1407(3) 0.37933(18) 0.0497(7) Uani 1 1 d . . C4 C 0.7970(3) 0.0170(3) 0.22596(18) 0.0496(7) Uani 1 1 d . . C3 C 0.9531(3) 0.0007(3) 0.2586(2) 0.0539(7) Uani 1 1 d . . H3 H 1.0164 0.0801 0.2424 0.065 Uiso 1 1 calc R U C25 C 0.7691(3) 0.0266(3) 0.1245(2) 0.0607(8) Uani 1 1 d . . C2 C 0.9573(3) 0.0216(3) 0.3609(2) 0.0579(7) Uani 1 1 d . . H2A H 1.0556 0.0462 0.3911 0.070 Uiso 1 1 calc R U H2B H 0.9121 -0.0620 0.3821 0.070 Uiso 1 1 calc R U C31 C 0.6295(3) -0.1662(3) 0.1570(2) 0.0586(8) Uani 1 1 d . . C18 C 0.9994(3) -0.1277(3) 0.2186(2) 0.0544(7) Uani 1 1 d . . C21 C 1.0867(3) -0.3626(3) 0.1391(2) 0.0663(8) Uani 1 1 d . . C26 C 0.6644(3) -0.0935(4) 0.0862(2) 0.0634(8) Uani 1 1 d . . C15 C 0.9811(3) 0.2737(3) 0.4066(2) 0.0568(7) Uani 1 1 d . . C20 C 1.1279(4) -0.2361(4) 0.1118(2) 0.0721(9) Uani 1 1 d . . H20 H 1.1861 -0.2280 0.0668 0.086 Uiso 1 1 calc R U C11 C 0.6026(4) 0.3038(4) 0.2648(2) 0.0678(9) Uani 1 1 d . . H11 H 0.6763 0.3676 0.2500 0.081 Uiso 1 1 calc R U C19 C 1.0845(3) -0.1215(3) 0.1501(2) 0.0639(8) Uani 1 1 d . . H19 H 1.1127 -0.0368 0.1296 0.077 Uiso 1 1 calc R U C22 C 1.0004(4) -0.3740(4) 0.2066(3) 0.0789(10) Uani 1 1 d . . H22 H 0.9708 -0.4595 0.2257 0.095 Uiso 1 1 calc R U C30 C 0.5313(4) -0.2874(4) 0.1448(3) 0.0828(11) Uani 1 1 d . . H30 H 0.5090 -0.3349 0.1931 0.099 Uiso 1 1 calc R U C12 C 0.7803(3) 0.1149(3) 0.4535(2) 0.0574(7) Uani 1 1 d . . C7 C 0.5164(3) 0.0850(4) 0.3069(2) 0.0698(9) Uani 1 1 d . . H7 H 0.5309 -0.0020 0.3206 0.084 Uiso 1 1 calc R U C9 C 0.3572(4) 0.2467(5) 0.2870(3) 0.0875(12) Uani 1 1 d . . H9 H 0.2667 0.2702 0.2879 0.105 Uiso 1 1 calc R U C10 C 0.4671(4) 0.3385(4) 0.2651(3) 0.0885(12) Uani 1 1 d . . H10 H 0.4511 0.4246 0.2502 0.106 Uiso 1 1 calc R U C17 C 1.2869(5) 0.3615(5) 0.5461(4) 0.131(2) Uani 1 1 d . . H17A H 1.3581 0.4409 0.5707 0.197 Uiso 1 1 calc R U H17B H 1.2835 0.2945 0.5883 0.197 Uiso 1 1 calc R U H17C H 1.3111 0.3216 0.4904 0.197 Uiso 1 1 calc R U C16 C 1.1521(4) 0.4015(4) 0.5297(3) 0.0954(13) Uani 1 1 d . . H16A H 1.1555 0.4701 0.4877 0.114 Uiso 1 1 calc R U H16B H 1.1279 0.4429 0.5858 0.114 Uiso 1 1 calc R U C27 C 0.5977(5) -0.1451(5) -0.0020(3) 0.0914(12) Uani 1 1 d . . H27 H 0.6195 -0.0983 -0.0507 0.110 Uiso 1 1 calc R U C23 C 0.9591(4) -0.2563(4) 0.2450(3) 0.0774(10) Uani 1 1 d . . H23 H 0.9017 -0.2643 0.2906 0.093 Uiso 1 1 calc R U C28 C 0.5009(5) -0.2644(6) -0.0149(4) 0.1097(16) Uani 1 1 d . . H28 H 0.4562 -0.2998 -0.0731 0.132 Uiso 1 1 calc R U C29 C 0.4676(5) -0.3344(5) 0.0572(4) 0.1076(16) Uani 1 1 d . . H29 H 0.4003 -0.4157 0.0463 0.129 Uiso 1 1 calc R U C24 C 1.0796(6) -0.6065(4) 0.1126(3) 0.1066(15) Uani 1 1 d . . H24A H 1.1246 -0.6715 0.0796 0.160 Uiso 1 1 calc R U H24B H 1.0971 -0.6151 0.1760 0.160 Uiso 1 1 calc R U H24C H 0.9780 -0.6250 0.0923 0.160 Uiso 1 1 calc R U C8 C 0.3819(4) 0.1201(5) 0.3076(3) 0.0865(11) Uani 1 1 d . . H8 H 0.3075 0.0569 0.3223 0.104 Uiso 1 1 calc R U C13 C 0.6407(6) 0.2195(6) 0.5504(4) 0.132(2) Uani 1 1 d . . H13A H 0.5470 0.2298 0.5211 0.159 Uiso 1 1 calc R U H13B H 0.6318 0.1273 0.5686 0.159 Uiso 1 1 calc R U C14 C 0.6758(8) 0.3084(9) 0.6224(4) 0.199(4) Uani 1 1 d . . H14A H 0.6043 0.2932 0.6616 0.299 Uiso 1 1 calc R U H14B H 0.7670 0.2976 0.6533 0.299 Uiso 1 1 calc R U H14C H 0.6820 0.4004 0.6057 0.299 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 0.0602(12) 0.0515(12) 0.0543(12) 0.0138(9) 0.0161(9) 0.0008(9) O5 0.0831(16) 0.0751(16) 0.0734(15) 0.0049(12) 0.0359(12) 0.0090(12) O3 0.0904(17) 0.0651(15) 0.0735(15) 0.0182(12) 0.0097(12) -0.0128(12) O6 0.0868(16) 0.0741(16) 0.0834(17) 0.0375(13) 0.0270(13) 0.0051(12) O7 0.111(2) 0.0622(16) 0.117(2) 0.0047(15) 0.0512(17) 0.0203(14) O4 0.0755(15) 0.0717(16) 0.0760(16) 0.0155(12) -0.0163(12) -0.0074(12) O2 0.1074(19) 0.0869(18) 0.0676(15) 0.0374(14) 0.0243(13) 0.0071(14) C5 0.0500(15) 0.0504(16) 0.0523(16) 0.0180(13) 0.0120(12) 0.0067(12) C6 0.0541(16) 0.0544(17) 0.0445(15) 0.0088(13) 0.0061(12) 0.0124(13) C1 0.0494(15) 0.0520(17) 0.0491(15) 0.0127(13) 0.0085(12) 0.0079(12) C4 0.0515(15) 0.0513(17) 0.0490(15) 0.0173(13) 0.0136(12) 0.0065(12) C3 0.0514(16) 0.0513(17) 0.0626(18) 0.0170(14) 0.0130(13) 0.0097(13) C25 0.0686(19) 0.065(2) 0.0568(18) 0.0223(16) 0.0199(15) 0.0179(16) C2 0.0603(18) 0.0576(19) 0.0576(18) 0.0124(14) 0.0032(14) 0.0162(14) C31 0.0551(17) 0.0580(19) 0.0626(19) 0.0011(15) 0.0134(14) 0.0092(14) C18 0.0533(16) 0.0559(18) 0.0582(17) 0.0140(14) 0.0148(13) 0.0120(13) C21 0.068(2) 0.060(2) 0.075(2) 0.0072(17) 0.0224(16) 0.0138(16) C26 0.0662(19) 0.074(2) 0.0527(18) 0.0024(16) 0.0082(14) 0.0236(17) C15 0.0548(17) 0.0546(18) 0.0627(19) 0.0100(15) 0.0111(14) 0.0101(13) C20 0.083(2) 0.068(2) 0.074(2) 0.0148(18) 0.0403(18) 0.0129(17) C11 0.070(2) 0.066(2) 0.074(2) 0.0185(17) 0.0150(16) 0.0203(16) C19 0.0673(19) 0.0566(19) 0.072(2) 0.0170(16) 0.0254(16) 0.0066(15) C22 0.092(2) 0.062(2) 0.098(3) 0.0321(19) 0.044(2) 0.0197(18) C30 0.077(2) 0.072(2) 0.097(3) -0.010(2) 0.032(2) 0.0022(18) C12 0.0558(17) 0.064(2) 0.0516(17) 0.0138(15) 0.0069(13) 0.0052(14) C7 0.0555(18) 0.070(2) 0.087(2) 0.0208(18) 0.0171(16) 0.0099(16) C9 0.063(2) 0.112(3) 0.096(3) 0.017(2) 0.012(2) 0.036(2) C10 0.091(3) 0.084(3) 0.104(3) 0.030(2) 0.016(2) 0.042(2) C17 0.074(3) 0.106(4) 0.199(6) 0.006(4) -0.009(3) 0.002(3) C16 0.088(3) 0.070(3) 0.112(3) 0.006(2) -0.019(2) -0.002(2) C27 0.099(3) 0.116(4) 0.059(2) -0.005(2) 0.003(2) 0.037(3) C23 0.095(3) 0.067(2) 0.090(3) 0.0313(19) 0.052(2) 0.0299(19) C28 0.097(3) 0.129(4) 0.087(3) -0.038(3) -0.009(3) 0.020(3) C29 0.085(3) 0.101(3) 0.118(4) -0.040(3) 0.017(3) -0.006(2) C24 0.150(4) 0.059(3) 0.116(4) 0.006(2) 0.038(3) 0.021(3) C8 0.053(2) 0.099(3) 0.110(3) 0.020(2) 0.0158(19) 0.0135(19) C13 0.139(4) 0.133(4) 0.134(5) -0.003(4) 0.095(4) 0.005(3) C14 0.176(6) 0.287(9) 0.102(4) -0.065(5) 0.081(4) -0.051(6) 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 C31 O1 C4 108.1(2) C12 O5 C13 116.7(3) C21 O7 C24 118.9(3) C15 O4 C16 119.0(3) C6 C5 C4 117.9(2) C6 C5 C1 118.2(2) C4 C5 C1 104.7(2) C11 C6 C7 117.1(3) C11 C6 C5 119.2(3) C7 C6 C5 123.7(3) C15 C1 C12 110.0(2) C15 C1 C2 108.3(2) C12 C1 C2 111.8(2) C15 C1 C5 110.4(2) C12 C1 C5 111.5(2) C2 C1 C5 104.6(2) O1 C4 C5 112.8(2) O1 C4 C25 105.0(2) C5 C4 C25 114.2(2) O1 C4 C3 109.2(2) C5 C4 C3 103.0(2) C25 C4 C3 112.7(2) C18 C3 C2 117.3(2) C18 C3 C4 116.0(2) C2 C3 C4 101.1(2) O2 C25 C26 130.3(3) O2 C25 C4 123.6(3) C26 C25 C4 106.0(3) C3 C2 C1 105.4(2) O1 C31 C30 123.5(3) O1 C31 C26 113.6(3) C30 C31 C26 122.9(3) C23 C18 C19 116.4(3) C23 C18 C3 123.2(3) C19 C18 C3 120.3(3) C20 C21 O7 116.7(3) C20 C21 C22 119.4(3) O7 C21 C22 123.8(3) C31 C26 C27 119.0(4) C31 C26 C25 107.1(3) C27 C26 C25 133.8(4) O3 C15 O4 123.4(3) O3 C15 C1 125.4(3) O4 C15 C1 111.2(3) C21 C20 C19 120.7(3) C6 C11 C10 121.5(3) C20 C19 C18 121.9(3) C23 C22 C21 118.9(3) C31 C30 C29 116.4(4) O6 C12 O5 124.5(3) O6 C12 C1 124.8(3) O5 C12 C1 110.7(3) C8 C7 C6 121.2(3) C8 C9 C10 119.2(3) C9 C10 C11 120.3(4) C17 C16 O4 110.2(4) C28 C27 C26 118.7(4) C18 C23 C22 122.6(3) C27 C28 C29 121.0(4) C30 C29 C28 122.1(4) C9 C8 C7 120.6(4) C14 C13 O5 115.4(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C31 1.364(4) O1 C4 1.445(3) O5 C12 1.325(4) O5 C13 1.452(5) O3 C15 1.199(4) O6 C12 1.194(4) O7 C21 1.369(4) O7 C24 1.406(5) O4 C15 1.332(4) O4 C16 1.458(4) O2 C25 1.210(4) C5 C6 1.505(4) C5 C4 1.526(4) C5 C1 1.584(4) C6 C11 1.376(4) C6 C7 1.391(4) C1 C15 1.516(4) C1 C12 1.528(4) C1 C2 1.545(4) C4 C25 1.529(4) C4 C3 1.546(4) C3 C18 1.504(4) C3 C2 1.525(4) C25 C26 1.439(5) C31 C30 1.377(5) C31 C26 1.385(4) C18 C23 1.378(4) C18 C19 1.389(4) C21 C20 1.365(5) C21 C22 1.387(5) C26 C27 1.403(5) C20 C19 1.365(5) C11 C10 1.390(5) C22 C23 1.382(5) C30 C29 1.379(6) C7 C8 1.383(5) C9 C8 1.366(5) C9 C10 1.368(5) C17 C16 1.404(6) C27 C28 1.355(6) C28 C29 1.385(7) C13 C14 1.296(7)