#------------------------------------------------------------------------------ #$Date: 2021-10-02 02:03:01 +0300 (Sat, 02 Oct 2021) $ #$Revision: 269444 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/84/7708498.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_7708498 loop_ _publ_author_name 'Arp, Fabian Felix' 'Ashirov, Rahym' 'Bhuvanesh, Nattamai' 'Bluemel, Janet' _publ_section_title ; Di(hydroperoxy)adamantane Adducts: Synthesis, Characterization and Application as Oxidizers for the Direct Esterification of Aldehydes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT03243G _journal_year 2021 _chemical_formula_moiety 'C10 H16 O4, H2 O' _chemical_formula_sum 'C10 H18 O5' _chemical_formula_weight 218.24 _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_Hall '-P 2ac 2ab' _space_group_name_H-M_alt 'P b c a' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2020-01-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-01-29 deposited with the CCDC. 2021-09-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 10.5546(9) _cell_length_b 8.3898(7) _cell_length_c 23.5993(19) _cell_measurement_reflns_used 9255 _cell_measurement_temperature 110.0 _cell_measurement_theta_max 70.034 _cell_measurement_theta_min 3.746 _cell_volume 2089.7(3) _computing_cell_refinement 'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.' _computing_data_reduction 'SAINT V8.38 Bruker AXS Inc., Madison, WI, USA.' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 110.0 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker PHOTON II' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_unetI/netI 0.0129 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 30771 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 62.465 _diffrn_reflns_theta_max 62.465 _diffrn_reflns_theta_min 3.746 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_T_max 0.5220 _exptl_absorpt_correction_T_min 0.4283 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0764 before and 0.0546 after correction. The Ratio of minimum to maximum transmission is 0.8205. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.387 _exptl_crystal_description plate _exptl_crystal_F_000 944 _exptl_crystal_size_max 0.162 _exptl_crystal_size_mid 0.158 _exptl_crystal_size_min 0.032 _refine_diff_density_max 0.389 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.047 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 136 _refine_ls_number_reflns 1676 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.083 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0380 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+1.3767P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1007 _refine_ls_wR_factor_ref 0.1042 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1568 _reflns_number_total 1676 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt03243g2.cif _cod_data_source_block ffe406a _cod_database_code 7708498 _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 0.971 _shelx_estimated_absorpt_t_min 0.864 _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 O(H) groups, All O(H,H) groups 2.a Riding coordinates: O2(H2), O4(H4), O5(H5C,H5D) 2.b Ternary CH refined with riding coordinates: C2(H2A), C4(H4A), C6(H6), C8(H8) 2.c Secondary CH2 refined with riding coordinates: C3(H3A,H3B), C5(H5A,H5B), C7(H7B,H7A), C9(H9A,H9B), C10(H10A,H10B) ; _shelx_res_file ; TITL ffe406a_a.res in Pbca ffe406a.res created by SHELXL-2018/3 at 10:56:57 on 23-Jan-2020 REM Old TITL FFE406a in Pbca REM SHELXT solution in Pbca REM R1 0.116, Rweak 0.001, Alpha 0.015, Orientation as input REM Formula found by SHELXT: C10 O5 CELL 1.54178 10.5546 8.3898 23.5993 90 90 90 ZERR 8 0.0009 0.0007 0.0019 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 80 144 40 EQIV $1 0.5-X,-0.5+Y,+Z EQIV $2 1-X,-Y,1-Z L.S. 8 0 0 PLAN 20 SIZE 0.162 0.158 0.032 TEMP -163.15 HTAB O2 O5 HTAB O4 O5 HTAB O5 O3_$1 HTAB O5 O4_$1 HTAB O5 O1_$2 acta BOND $H more -1 wpdb -1 htab conf list 4 fmap 2 53 OMIT -4 125 OMIT 3 3 2 REM REM REM WGHT 0.054300 1.376700 FVAR 0.43489 O1 3 0.542691 0.145739 0.591175 11.00000 0.02273 0.01568 = 0.02527 0.00204 0.00069 0.00040 O2 3 0.492705 0.002124 0.618677 11.00000 0.03442 0.01511 = 0.03086 0.00645 -0.00406 -0.00328 AFIX 3 H2 2 0.450485 -0.040086 0.585427 11.00000 -1.50000 AFIX 0 O3 3 0.341550 0.257424 0.584480 11.00000 0.01919 0.02705 = 0.01808 -0.00181 0.00027 -0.00106 O4 3 0.345147 0.252165 0.522097 11.00000 0.02329 0.02102 = 0.01774 -0.00203 -0.00351 0.00250 AFIX 3 H4 2 0.343637 0.143085 0.517267 11.00000 -1.50000 AFIX 0 C1 1 0.466395 0.280688 0.605124 11.00000 0.01539 0.01656 = 0.01886 -0.00080 -0.00039 0.00156 C2 1 0.536215 0.421883 0.578432 11.00000 0.02214 0.01950 = 0.01604 0.00094 0.00118 0.00059 AFIX 13 H2A 2 0.545072 0.404717 0.536687 11.00000 -1.20000 AFIX 0 C3 1 0.458235 0.574296 0.589709 11.00000 0.02507 0.01691 = 0.02455 0.00062 -0.00310 0.00189 AFIX 23 H3A 2 0.500683 0.666980 0.571997 11.00000 -1.20000 H3B 2 0.373057 0.563295 0.572583 11.00000 -1.20000 AFIX 0 C4 1 0.445561 0.601831 0.653416 11.00000 0.02719 0.02353 = 0.02769 -0.00658 0.00160 0.00447 AFIX 13 H4A 2 0.396442 0.701830 0.660424 11.00000 -1.20000 AFIX 0 C5 1 0.577130 0.616283 0.680295 11.00000 0.02857 0.02425 = 0.02113 -0.00617 0.00038 -0.00326 AFIX 23 H5A 2 0.568570 0.634136 0.721585 11.00000 -1.20000 H5B 2 0.622391 0.708671 0.663824 11.00000 -1.20000 AFIX 0 C6 1 0.653289 0.463312 0.669542 11.00000 0.02193 0.02685 = 0.02190 -0.00147 -0.00472 -0.00183 AFIX 13 H6 2 0.739013 0.473285 0.687236 11.00000 -1.20000 AFIX 0 C7 1 0.583631 0.320763 0.695253 11.00000 0.02899 0.02575 = 0.01780 0.00197 -0.00333 -0.00038 AFIX 23 H7B 2 0.576371 0.334896 0.736775 11.00000 -1.20000 H7A 2 0.632333 0.222003 0.687997 11.00000 -1.20000 AFIX 0 C8 1 0.450079 0.305785 0.668986 11.00000 0.02537 0.02708 = 0.01704 0.00205 0.00238 -0.00374 AFIX 13 H8 2 0.404595 0.212757 0.685956 11.00000 -1.20000 AFIX 0 C9 1 0.667451 0.439628 0.605411 11.00000 0.01807 0.02077 = 0.02292 -0.00110 0.00297 -0.00188 AFIX 23 H9A 2 0.711807 0.532325 0.588670 11.00000 -1.20000 H9B 2 0.718590 0.343050 0.597804 11.00000 -1.20000 AFIX 0 C10 1 0.375171 0.459090 0.679829 11.00000 0.02278 0.03370 = 0.02223 -0.00892 0.00541 -0.00133 AFIX 23 H10A 2 0.365408 0.475882 0.721122 11.00000 -1.20000 H10B 2 0.289627 0.449839 0.662939 11.00000 -1.20000 AFIX 0 O5 3 0.367525 -0.063352 0.516304 11.00000 0.02025 0.02001 = 0.02450 -0.00462 0.00379 -0.00424 AFIX 3 H5C 2 0.302955 -0.122042 0.517364 11.00000 -1.50000 H5D 2 0.402365 -0.092342 0.485464 11.00000 -1.50000 AFIX 0 HKLF 4 REM ffe406a_a.res in Pbca REM wR2 = 0.104164, GooF = S = 1.08311, Restrained GooF = 1.08311 for all data REM R1 = 0.037965 for 1568 Fo > 4sig(Fo) and 0.040275 for all 1676 data REM 136 parameters refined using 0 restraints END WGHT 0.0543 1.3766 REM Instructions for potential hydrogen bonds HTAB O2 O5 HTAB O4 O5 HTAB O5 O3_$1 HTAB O5 O4_$1 HTAB O5 O1_$2 REM Highest difference peak 0.389, deepest hole -0.215, 1-sigma level 0.047 Q1 1 0.4051 0.1388 0.6330 11.00000 0.05 0.39 Q2 1 0.4670 0.2651 0.5431 11.00000 0.05 0.38 Q3 1 0.4587 0.2990 0.6372 11.00000 0.05 0.28 Q4 1 0.5169 0.4622 0.7186 11.00000 0.05 0.28 Q5 1 0.5646 0.6058 0.6217 11.00000 0.05 0.24 Q6 1 0.3705 0.4074 0.6277 11.00000 0.05 0.24 Q7 1 0.6025 0.3007 0.6283 11.00000 0.05 0.23 Q8 1 0.6557 0.4529 0.6346 11.00000 0.05 0.20 Q9 1 0.4410 0.5763 0.6201 11.00000 0.05 0.18 Q10 1 0.4940 0.4946 0.5824 11.00000 0.05 0.18 Q11 1 0.5207 0.3131 0.6835 11.00000 0.05 0.17 Q12 1 0.4036 0.3824 0.6802 11.00000 0.05 0.15 Q13 1 0.6057 0.4339 0.5964 11.00000 0.05 0.15 Q14 1 0.6114 0.5422 0.6794 11.00000 0.05 0.15 Q15 1 0.4997 0.3546 0.5979 11.00000 0.05 0.15 Q16 1 0.6066 0.2590 0.7025 11.00000 0.05 0.14 Q17 1 0.5409 0.3966 0.7396 11.00000 0.05 0.14 Q18 1 0.5195 0.5970 0.6776 11.00000 0.05 0.13 Q19 1 0.3950 0.6000 0.5594 11.00000 0.05 0.13 Q20 1 0.3120 0.3208 0.5037 11.00000 0.05 0.12 ; _shelx_res_checksum 43602 _shelx_hkl_file ; 0 1 0 -0.10 0.10 0 1 0 0.00 0.10 0 -1 0 0.10 0.20 0 2 0 301.57 7.50 0 2 0 292.97 8.90 0 -2 0 295.77 9.40 0 -2 0 304.17 7.50 0 -3 0 -0.20 0.40 0 3 0 -0.10 0.30 0 4 0 647.44 17.30 0 4 0 673.13 19.70 0 -4 0 679.63 21.20 0 5 0 -0.10 0.20 0 5 0 -0.40 0.60 0 -5 0 0.00 1.00 0 6 0 562.84 15.40 0 6 0 488.75 13.90 0 -6 0 503.05 20.50 0 -6 0 591.64 17.30 0 7 0 -0.10 0.10 0 7 0 -0.40 0.20 0 -7 0 0.40 0.20 0 -7 0 -0.90 1.50 0 7 0 -0.20 0.20 0 -7 0 0.00 0.30 0 -8 0 0.40 0.20 0 8 0 0.20 0.30 0 8 0 0.40 0.20 0 8 0 0.20 0.30 0 -8 0 0.20 0.20 0 -8 0 0.50 0.30 0 9 0 0.00 0.20 0 9 0 0.00 0.10 0 9 0 -0.40 0.20 0 -9 0 -0.20 0.20 0 -10 0 40.50 2.60 0 10 0 46.10 1.90 0 10 0 42.30 2.00 0 1 -1 -0.10 0.20 0 -1 -1 0.00 0.20 0 -1 -1 0.00 0.10 0 1 1 0.00 0.10 0 1 1 -0.10 0.10 0 -1 1 0.00 0.20 0 -1 1 0.30 0.30 0 -1 1 0.00 0.10 0 -2 -1 29.90 2.30 0 2 -1 29.40 2.00 0 -2 -1 33.20 1.60 0 -2 1 30.50 2.20 0 2 1 29.70 1.90 0 2 1 32.50 1.50 0 -3 -1 0.40 0.60 0 3 -1 0.00 0.30 0 3 1 0.10 0.10 0 -3 1 -0.60 0.40 0 3 1 -0.10 0.20 0 4 -1 0.70 0.60 0 4 -1 0.50 0.20 0 -4 -1 2.80 1.30 0 -4 1 0.40 0.60 0 4 1 0.70 0.60 0 5 -1 -0.10 0.20 0 5 -1 2.50 1.30 0 -5 -1 -0.60 0.80 0 -5 1 -1.20 0.70 0 5 1 -0.10 0.20 0 5 1 0.30 0.70 0 -6 -1 1333.77 40.70 0 6 -1 1265.07 32.10 0 6 -1 1298.47 33.50 0 -6 -1 1330.57 35.40 0 -6 1 1334.57 35.30 0 6 1 1286.97 32.10 0 6 1 1258.27 33.40 0 -6 1 1331.47 40.00 0 -7 -1 -0.20 0.20 0 -7 -1 -0.10 0.30 0 7 -1 -0.20 0.10 0 7 -1 0.00 0.20 0 -7 -1 0.10 0.40 0 7 -1 -0.10 0.20 0 -7 -1 0.80 1.60 0 -7 1 -0.40 0.20 0 7 1 0.10 0.10 0 7 1 0.10 0.30 0 -7 1 3.00 1.90 0 -7 1 0.00 0.30 0 -7 1 -0.30 0.20 0 7 1 0.10 0.30 0 -8 -1 23.30 1.40 0 -8 -1 21.70 1.40 0 -8 -1 19.10 2.50 0 8 -1 22.20 1.50 0 8 -1 23.50 1.60 0 8 -1 18.80 2.10 0 -8 -1 16.90 1.40 0 -8 -1 20.00 1.50 0 -8 1 17.70 2.50 0 8 1 21.80 1.50 0 -8 1 21.30 1.50 0 8 1 23.70 1.60 0 -8 1 20.90 1.40 0 8 1 20.00 2.10 0 -8 1 23.60 1.30 0 -9 -1 0.20 0.20 0 9 -1 0.00 0.10 0 9 -1 -0.20 0.30 0 9 -1 0.40 0.20 0 -9 1 -0.10 0.20 0 9 1 0.00 0.20 0 9 1 -0.10 0.20 0 9 1 -0.10 0.10 0 -10 -1 5.90 0.50 0 10 -1 6.60 0.80 0 -10 -1 4.70 1.10 0 10 -1 6.60 0.70 0 -10 1 5.50 0.70 0 -10 1 4.30 1.00 0 10 1 5.90 0.60 0 10 1 6.20 0.70 0 0 2 1535.85 35.30 0 0 2 1416.96 35.20 0 1 -2 0.10 0.20 0 -1 -2 0.00 0.10 0 1 -2 0.10 0.10 0 -1 -2 -0.10 0.20 0 -1 2 -0.10 0.20 0 -1 2 -0.10 0.30 0 1 2 0.00 0.10 0 -1 2 0.00 0.10 0 -1 2 -0.10 0.10 0 2 -2 125.79 5.10 0 -2 -2 130.09 5.40 0 -2 -2 128.99 4.50 0 2 2 121.49 4.40 0 2 2 128.89 4.40 0 -2 2 129.19 5.00 0 -2 2 129.59 4.80 0 -3 -2 -0.10 0.10 0 3 -2 -0.60 0.30 0 -3 2 1.60 0.70 0 3 2 0.00 0.10 0 3 2 -0.40 0.30 0 4 -2 204.98 6.70 0 -4 -2 209.88 9.60 0 -4 2 209.18 9.10 0 4 2 211.68 6.50 0 4 2 202.68 7.70 0 5 -2 -0.80 0.50 0 -5 -2 -0.30 0.90 0 -5 2 1.40 1.10 0 5 2 -0.20 0.20 0 5 2 -0.10 0.10 0 -6 -2 831.82 28.50 0 6 -2 780.02 20.10 0 6 -2 794.22 21.40 0 -6 -2 781.82 27.70 0 6 2 770.22 20.10 0 -6 2 803.22 27.00 0 6 2 807.72 21.50 0 7 -2 0.20 0.30 0 7 -2 -0.20 0.20 0 -7 -2 -0.30 0.30 0 -7 -2 -0.60 0.30 0 7 -2 -0.20 0.10 0 -7 -2 -0.20 0.20 0 -7 -2 1.80 1.80 0 -7 -2 -0.10 0.20 0 7 2 0.20 0.30 0 7 2 0.00 0.10 0 -7 2 -0.10 0.10 0 -7 2 0.10 0.30 0 -7 2 2.90 1.90 0 -7 2 -0.20 0.20 0 7 2 0.10 0.20 0 -8 -2 12.50 1.10 0 -8 -2 11.80 1.10 0 8 -2 12.50 1.20 0 -8 -2 10.90 2.10 0 -8 -2 11.90 1.20 0 8 -2 12.10 1.70 0 -8 -2 11.80 1.20 0 8 -2 12.50 1.20 0 -8 2 10.50 0.90 0 8 2 12.90 1.20 0 -8 2 12.60 1.10 0 8 2 12.70 1.10 0 -8 2 12.60 2.00 0 8 2 14.60 1.80 0 -8 2 12.60 1.20 0 -9 -2 -0.20 0.30 0 9 -2 0.30 0.20 0 -9 -2 -0.10 0.20 0 9 -2 -0.20 0.10 0 -9 2 0.10 0.20 0 9 2 -0.40 0.20 0 9 2 0.00 0.20 0 9 2 -0.20 0.10 0 10 -2 130.39 3.80 0 -10 -2 114.79 3.50 0 10 -2 112.19 3.70 0 -10 -2 109.69 5.60 0 10 2 123.39 3.60 0 -10 2 112.09 4.80 0 10 2 121.99 3.50 0 -10 2 118.69 3.40 0 0 -3 0.00 0.10 0 0 -3 0.00 0.10 0 0 3 0.00 0.10 0 0 3 0.00 0.10 0 0 3 -0.10 0.10 0 -1 -3 0.50 0.30 0 -1 -3 0.00 0.10 0 1 -3 0.10 0.10 0 1 3 0.00 0.10 0 -1 3 0.00 0.10 0 -1 3 0.00 0.10 0 -1 3 0.20 0.20 0 -1 3 0.10 0.30 0 2 -3 92.79 4.30 0 -2 -3 87.59 4.30 0 -2 -3 86.79 3.90 0 -2 3 89.89 5.00 0 -2 3 91.19 3.80 0 2 3 87.19 3.70 0 -2 3 88.39 2.60 0 2 3 86.49 3.40 0 -2 3 88.69 3.80 0 -3 -3 0.00 0.10 0 -3 -3 -0.10 0.70 0 3 -3 0.60 0.50 0 3 3 -0.20 0.10 0 -3 3 0.20 0.50 0 3 3 -0.20 0.30 0 -4 -3 130.39 7.30 0 4 -3 123.89 6.60 0 4 3 141.59 4.70 0 4 3 130.69 5.10 0 4 3 123.89 5.40 0 -4 3 125.49 6.60 0 5 -3 0.10 0.20 0 -5 -3 0.10 1.00 0 -5 3 0.40 0.70 0 6 -3 242.28 7.10 0 6 -3 247.88 11.90 0 -6 -3 243.38 13.30 0 6 -3 232.78 8.10 0 6 3 239.38 7.00 0 -6 3 234.18 7.20 0 6 3 235.48 8.20 0 -6 3 247.48 12.00 0 7 -3 -0.40 0.20 0 -7 -3 0.30 0.30 0 7 -3 -0.10 0.30 0 -7 -3 -0.10 0.40 0 -7 -3 0.10 0.20 0 7 -3 -0.10 0.10 0 -7 -3 0.30 0.20 0 -7 -3 -0.30 1.70 0 -7 3 -0.10 0.20 0 -7 3 2.00 1.80 0 7 3 0.00 0.10 0 7 3 0.30 0.30 0 -7 3 -0.30 0.10 0 -7 3 -0.20 0.20 0 -8 -3 218.38 6.50 0 -8 -3 205.28 6.80 0 -8 -3 221.98 6.90 0 -8 -3 209.88 6.30 0 8 -3 212.08 6.60 0 8 -3 218.88 8.00 0 8 -3 216.68 6.70 0 -8 -3 216.58 9.10 0 -8 3 220.88 6.60 0 -8 3 217.28 6.40 0 8 3 212.78 6.60 0 -8 3 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11 0.20 0.30 -11 1 11 0.20 0.20 -11 1 11 0.70 0.40 11 0 -11 -0.10 0.20 -11 0 -11 -0.10 0.20 11 0 -11 0.00 0.10 -11 0 11 -0.30 0.20 11 0 11 -0.20 0.20 -11 0 11 0.40 0.60 11 0 11 0.00 0.10 11 0 11 0.00 0.30 -11 -1 -11 0.10 0.20 11 1 -11 0.40 0.20 11 1 11 0.50 0.20 11 1 11 0.10 0.20 -11 -1 11 0.40 0.40 11 1 11 -0.20 0.20 -11 -1 11 0.00 0.20 -11 -2 -11 0.10 0.20 -11 -2 11 0.20 0.20 11 2 11 0.00 0.20 11 2 11 0.00 0.10 -11 -2 11 0.10 0.30 -11 -3 -11 24.70 1.30 -11 -3 -11 24.30 1.30 -11 -3 11 20.20 1.20 -11 -3 11 26.70 1.50 11 -3 -12 22.00 1.10 -11 3 -12 22.70 1.30 -11 3 12 22.30 1.10 11 -3 12 22.70 1.40 11 -2 -12 55.89 2.10 11 -2 -12 57.79 2.30 -11 2 -12 56.59 2.00 -11 2 12 61.39 2.60 -11 2 12 57.29 2.20 11 -2 12 60.39 2.30 11 -1 -12 12.10 0.90 -11 1 -12 11.40 0.90 -11 1 -12 10.90 0.70 11 -1 12 9.80 0.90 11 -1 12 12.00 1.00 -11 1 12 9.70 1.20 -11 1 12 11.50 1.10 -11 0 -12 104.79 3.40 11 0 -12 103.59 3.30 -11 0 12 99.29 3.40 11 0 12 105.79 3.40 -11 0 12 101.79 3.60 11 0 12 109.29 3.60 -11 -1 -12 11.20 1.00 11 1 -12 10.80 0.80 11 1 12 11.20 0.90 -11 -1 12 11.30 1.10 -11 -1 12 11.10 1.00 11 1 12 12.40 0.90 -11 -2 -12 59.89 2.30 -11 -2 12 56.89 2.40 -11 -2 12 59.39 2.70 11 2 12 61.69 2.50 11 2 12 61.09 2.40 -11 -3 -12 23.10 1.40 -11 -3 -12 26.80 1.30 -11 -3 12 25.50 1.30 -11 -3 12 23.70 1.40 11 3 12 23.40 1.40 11 -2 -13 8.00 0.70 11 -2 -13 7.80 0.80 -11 2 13 8.70 1.00 11 -1 -13 10.50 1.20 -11 1 -13 9.50 0.80 11 -1 13 9.70 0.80 -11 1 13 10.60 1.30 11 -1 13 10.80 0.90 -11 1 13 9.20 0.90 -11 0 -13 0.10 0.20 11 0 -13 0.10 0.10 11 0 13 0.20 0.20 11 0 13 0.00 0.10 -11 0 13 0.00 0.30 -11 0 13 0.10 0.30 11 1 -13 10.80 0.80 -11 -1 -13 9.60 0.90 -11 -1 13 9.80 0.90 11 1 13 11.00 1.10 -11 -1 13 9.50 1.00 11 1 13 11.30 1.20 -11 -2 -13 7.40 0.70 11 2 13 6.20 0.60 -11 -2 13 7.20 0.80 -11 -2 13 7.50 0.90 11 2 13 6.80 0.60 11 -1 -14 34.90 1.50 -11 1 -14 33.10 1.50 -11 1 14 36.40 1.80 11 -1 14 34.60 1.60 -11 1 14 33.80 1.60 -11 0 -14 105.59 3.40 11 0 -14 113.99 4.00 11 0 14 105.29 3.30 -11 0 14 95.99 3.40 11 0 14 107.89 3.40 -11 0 14 111.79 4.00 -11 -1 -14 35.10 1.50 11 1 14 34.70 1.50 11 1 14 30.90 1.70 -11 -1 14 34.10 1.50 12 -3 0 61.59 2.20 12 -3 0 51.59 2.20 -12 3 0 57.19 2.20 12 -2 0 20.00 1.20 12 -2 0 20.50 1.20 -12 2 0 19.20 1.20 12 -1 0 16.40 1.10 12 -1 0 17.70 1.10 12 -1 0 14.70 2.20 -12 1 0 16.70 1.20 -12 0 0 23.60 1.20 -12 0 0 24.00 1.40 12 0 0 26.30 1.40 12 0 0 25.00 2.00 12 1 0 15.20 1.40 -12 -1 0 18.20 1.10 12 1 0 17.60 1.10 -12 -1 0 16.70 1.20 -12 -2 0 19.80 1.60 -12 -2 0 20.90 1.20 12 2 0 20.80 1.10 -12 -3 0 54.49 2.10 -12 -3 0 61.99 2.40 12 -3 -1 2.40 0.50 12 -3 -1 2.90 0.50 -12 3 -1 3.20 0.80 12 -3 1 2.40 0.50 -12 3 1 2.50 0.60 12 -3 1 3.40 0.70 12 -2 -1 2.50 0.50 -12 2 -1 3.00 0.70 12 -2 -1 2.90 0.60 12 -2 1 3.90 0.60 12 -2 1 2.70 0.60 -12 2 1 2.20 0.70 12 -1 -1 0.20 0.10 12 -1 -1 0.20 0.30 12 -1 -1 0.10 0.20 -12 1 -1 0.30 0.30 12 -1 1 0.30 0.20 -12 1 1 0.20 0.30 12 -1 1 0.20 0.40 12 -1 1 0.10 0.10 12 0 -1 -0.10 0.10 -12 0 -1 0.30 0.30 12 0 -1 0.00 0.30 -12 0 -1 -0.20 0.20 12 0 1 0.10 0.20 -12 0 1 -0.50 0.30 12 0 1 -0.20 0.10 -12 0 1 0.10 0.30 -12 -1 -1 0.20 0.20 12 1 -1 0.00 0.10 12 1 -1 -0.20 0.20 -12 -1 -1 0.10 0.30 12 1 1 0.00 0.10 -12 -1 1 0.30 0.20 -12 -1 1 0.40 0.30 12 1 1 0.40 0.20 12 2 -1 2.30 0.50 -12 -2 -1 1.90 0.50 -12 -2 1 4.70 1.00 -12 -2 1 3.50 0.60 12 2 1 3.00 0.50 -12 -3 -1 2.10 0.40 -12 -3 -1 1.80 0.50 -12 -3 1 2.80 0.50 12 -3 -2 9.20 0.80 12 -3 -2 9.50 0.90 -12 3 -2 8.60 0.90 -12 3 2 10.30 0.90 12 -3 2 9.90 0.80 12 -3 2 9.40 0.80 12 -2 -2 28.40 1.40 12 -2 -2 27.60 1.40 -12 2 -2 28.70 1.50 12 -2 2 27.30 1.40 -12 2 2 27.20 1.60 12 -2 2 28.10 1.40 12 -1 -2 7.40 1.50 12 -1 -2 5.70 1.10 -12 1 -2 6.40 0.80 12 -1 -2 6.90 0.90 12 -1 2 9.40 1.40 12 -1 2 7.00 0.70 12 -1 2 7.20 0.80 12 0 -2 25.60 1.90 -12 0 -2 22.60 1.20 12 0 -2 22.70 2.60 -12 0 -2 21.60 1.30 12 0 2 19.60 2.10 -12 0 2 21.10 1.40 12 0 2 19.70 1.60 12 0 2 21.60 1.30 -12 0 2 21.60 1.60 12 1 -2 8.20 0.80 -12 -1 -2 6.10 1.00 -12 -1 -2 7.70 0.80 12 1 -2 5.60 0.90 -12 -1 2 8.20 0.90 12 1 2 7.70 0.80 12 1 2 6.80 1.10 -12 -1 2 8.40 0.80 -12 -2 -2 27.70 1.40 -12 -2 -2 27.60 1.40 -12 -2 2 27.80 1.40 -12 -2 2 28.00 1.50 12 2 2 27.40 1.60 -12 -3 -2 9.30 0.80 -12 -3 -2 9.10 0.60 -12 -3 2 9.70 0.90 -12 -3 2 9.20 0.80 -12 3 -3 0.40 0.30 12 -3 -3 1.50 0.60 -12 3 3 1.10 0.30 12 -3 3 2.30 0.50 12 -2 -3 20.10 1.20 -12 2 -3 15.70 1.40 12 -2 -3 20.40 1.20 12 -2 3 20.00 1.20 12 -2 3 20.30 1.20 -12 2 3 19.80 1.30 12 -1 -3 7.50 1.10 12 -1 -3 6.40 1.10 -12 1 -3 6.00 0.90 12 -1 -3 6.50 1.00 12 -1 3 5.70 1.10 -12 1 3 7.60 1.00 12 -1 3 7.50 0.80 12 -1 3 7.20 1.10 -12 0 -3 0.00 0.20 12 0 -3 -0.10 0.10 -12 0 -3 -0.20 0.30 12 0 -3 0.30 0.30 -12 0 3 0.60 0.40 -12 -1 -3 7.70 0.80 12 1 -3 8.00 1.20 12 1 -3 7.80 0.70 -12 -1 3 6.70 0.70 -12 -1 3 8.10 0.90 12 1 3 5.60 1.00 12 1 3 6.70 0.70 12 2 -3 19.60 1.00 -12 -2 -3 20.60 1.20 -12 -2 3 19.20 1.20 12 2 3 19.40 1.20 -12 -2 3 20.40 1.20 -12 -3 -3 0.20 0.20 -12 -3 -3 0.60 0.20 -12 -3 3 0.30 0.30 -12 -3 3 1.50 0.50 12 -3 -4 4.30 0.60 -12 3 -4 4.40 0.70 12 -3 -4 4.80 0.60 -12 3 4 5.20 0.70 12 -3 4 5.70 0.60 12 -2 -4 92.89 3.00 -12 2 -4 87.09 3.10 12 -2 -4 94.29 3.60 12 -2 4 91.79 3.10 -12 2 4 88.19 3.20 12 -2 4 89.49 3.20 12 -1 -4 6.90 0.80 12 -1 -4 8.10 0.80 -12 1 -4 4.40 1.00 12 -1 -4 7.40 1.00 12 -1 4 9.50 1.00 12 -1 4 5.30 1.10 -12 1 4 7.90 1.00 12 -1 4 8.70 0.80 12 0 -4 2.10 0.70 12 0 -4 4.10 0.50 -12 0 -4 3.40 0.60 12 0 4 2.30 0.70 12 0 4 2.30 0.90 12 0 4 2.70 1.10 -12 0 4 5.30 0.90 12 1 -4 6.70 0.90 -12 -1 -4 7.60 0.80 12 1 4 5.20 1.00 -12 -1 4 7.20 1.00 12 1 4 7.60 0.70 -12 -1 4 7.80 0.70 -12 -2 -4 91.79 3.00 -12 -2 4 91.79 3.10 -12 -2 4 88.19 2.90 12 2 4 77.49 3.00 -12 -3 -4 6.00 0.60 -12 -3 -4 4.50 0.60 -12 -3 4 5.80 0.70 -12 -3 4 6.30 0.80 12 -3 -5 3.80 0.50 12 -3 5 3.20 0.70 -12 3 5 3.00 0.60 12 -2 -5 -0.10 0.20 12 -2 -5 0.10 0.10 12 -2 5 -0.10 0.20 -12 2 5 -0.10 0.30 12 -2 5 -0.10 0.10 12 -1 -5 0.70 0.40 12 -1 -5 1.50 0.40 12 -1 -5 2.00 0.50 12 -1 5 1.70 0.50 -12 1 5 0.80 0.40 12 -1 5 0.70 0.30 12 0 -5 -0.10 0.10 12 0 -5 -0.10 0.20 -12 0 -5 -0.10 0.20 12 0 5 -0.10 0.10 -12 0 5 -0.10 0.30 -12 -1 -5 1.30 0.50 -12 -1 5 0.90 0.30 12 1 5 1.60 0.50 -12 -1 5 1.10 0.40 12 1 5 0.20 0.30 -12 -2 -5 0.00 0.20 12 2 5 -0.20 0.10 -12 -2 5 0.40 0.20 -12 -2 5 0.10 0.30 -12 -3 -5 2.90 0.40 -12 -3 -5 3.00 0.50 -12 -3 5 2.10 0.50 -12 -3 5 4.10 0.70 12 -2 -6 0.90 0.30 12 -2 6 1.30 0.40 -12 2 6 1.60 0.60 12 -2 6 1.80 0.50 12 -1 -6 0.10 0.10 -12 1 6 0.50 0.30 12 -1 6 0.20 0.10 12 -1 6 0.10 0.20 -12 0 -6 6.30 0.70 12 0 -6 6.40 0.70 12 0 6 4.80 0.80 -12 0 6 6.70 0.90 12 0 6 6.40 0.70 12 1 -6 0.30 0.10 -12 -1 -6 0.30 0.20 -12 -1 6 -0.40 0.20 -12 -1 6 0.10 0.30 12 1 6 0.20 0.10 -12 -2 -6 1.60 0.50 -12 -2 6 0.70 0.30 12 2 6 0.50 0.10 -12 -2 6 0.60 0.30 12 -2 -7 80.89 2.80 12 -2 -7 86.69 2.80 -12 2 7 88.19 3.00 12 -2 7 86.09 2.80 12 -2 7 85.09 2.90 12 -1 -7 19.10 1.30 12 -1 7 17.80 1.30 12 -1 7 18.10 1.10 -12 1 7 18.70 1.30 -12 0 -7 -0.10 0.20 12 0 -7 0.00 0.20 12 0 7 -0.10 0.20 12 0 7 0.00 0.10 -12 0 7 0.10 0.30 12 1 -7 18.30 1.30 -12 -1 -7 18.90 1.10 -12 -1 7 18.20 1.20 12 1 7 18.00 1.10 12 1 7 13.30 1.30 -12 -2 -7 84.39 2.80 -12 -2 7 87.99 3.00 12 2 7 87.09 2.90 12 -2 -8 55.79 2.20 12 -2 -8 50.09 2.10 12 -2 8 47.20 2.40 -12 2 8 51.69 2.00 12 -1 -8 10.20 0.80 12 -1 8 9.10 0.70 -12 1 8 10.20 0.90 12 -1 8 9.70 1.00 12 0 -8 2.50 0.50 -12 0 -8 1.60 0.50 12 0 8 2.50 0.60 12 0 8 2.50 0.50 -12 0 8 2.50 0.70 -12 -1 -8 9.70 0.80 12 1 -8 11.30 1.00 12 1 8 8.80 0.80 -12 -1 8 10.70 1.00 -12 -2 -8 52.59 2.40 -12 -2 8 54.19 2.40 12 -1 -9 0.20 0.10 12 -1 9 1.00 0.40 -12 1 9 0.20 0.30 12 -1 9 0.40 0.10 12 0 -9 -0.20 0.10 -12 0 -9 -0.10 0.10 12 0 9 0.10 0.20 -12 0 9 -0.10 0.30 12 0 9 0.00 0.10 -12 -1 -9 0.30 0.20 12 1 9 0.20 0.10 -12 -1 9 0.50 0.30 12 0 -10 -0.10 0.10 -12 0 -10 0.00 0.20 12 0 10 -0.10 0.10 -12 0 10 0.30 0.30 12 0 10 -0.10 0.20 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 72686 _olex2_submission_special_instructions 'No special instructions were received' 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' '-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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.54269(10) 0.14574(12) 0.59118(4) 0.0212(3) Uani 1 1 d . . . . . O2 O 0.49271(11) 0.00212(13) 0.61868(5) 0.0268(3) Uani 1 1 d . . . . . H2 H 0.450485 -0.040086 0.585427 0.040 Uiso 1 1 d R . . . . O3 O 0.34155(10) 0.25742(13) 0.58448(4) 0.0214(3) Uani 1 1 d . . . . . O4 O 0.34515(9) 0.25216(12) 0.52210(4) 0.0207(3) Uani 1 1 d . . . . . H4 H 0.343637 0.143085 0.517267 0.031 Uiso 1 1 d R . . . . C1 C 0.46640(13) 0.28069(17) 0.60512(6) 0.0169(3) Uani 1 1 d . . . . . C2 C 0.53621(14) 0.42188(18) 0.57843(6) 0.0192(4) Uani 1 1 d . . . . . H2A H 0.545072 0.404717 0.536687 0.023 Uiso 1 1 calc R . . . . C3 C 0.45823(15) 0.57430(18) 0.58971(7) 0.0222(4) Uani 1 1 d . . . . . H3A H 0.500683 0.666980 0.571997 0.027 Uiso 1 1 calc R . . . . H3B H 0.373057 0.563295 0.572583 0.027 Uiso 1 1 calc R . . . . C4 C 0.44556(16) 0.6018(2) 0.65342(7) 0.0261(4) Uani 1 1 d . . . . . H4A H 0.396442 0.701830 0.660424 0.031 Uiso 1 1 calc R . . . . C5 C 0.57713(15) 0.61628(19) 0.68030(7) 0.0246(4) Uani 1 1 d . . . . . H5A H 0.568570 0.634136 0.721585 0.030 Uiso 1 1 calc R . . . . H5B H 0.622391 0.708671 0.663824 0.030 Uiso 1 1 calc R . . . . C6 C 0.65329(15) 0.46331(19) 0.66954(7) 0.0236(4) Uani 1 1 d . . . . . H6 H 0.739013 0.473285 0.687236 0.028 Uiso 1 1 calc R . . . . C7 C 0.58363(16) 0.3208(2) 0.69525(6) 0.0242(4) Uani 1 1 d . . . . . H7B H 0.576371 0.334896 0.736775 0.029 Uiso 1 1 calc R . . . . H7A H 0.632333 0.222003 0.687997 0.029 Uiso 1 1 calc R . . . . C8 C 0.45008(15) 0.3058(2) 0.66899(6) 0.0232(4) Uani 1 1 d . . . . . H8 H 0.404595 0.212757 0.685956 0.028 Uiso 1 1 calc R . . . . C9 C 0.66745(14) 0.43963(18) 0.60541(6) 0.0206(4) Uani 1 1 d . . . . . H9A H 0.711807 0.532325 0.588670 0.025 Uiso 1 1 calc R . . . . H9B H 0.718590 0.343050 0.597804 0.025 Uiso 1 1 calc R . . . . C10 C 0.37517(15) 0.4591(2) 0.67983(7) 0.0262(4) Uani 1 1 d . . . . . H10A H 0.365408 0.475882 0.721122 0.031 Uiso 1 1 calc R . . . . H10B H 0.289627 0.449839 0.662939 0.031 Uiso 1 1 calc R . . . . O5 O 0.36753(10) -0.06335(12) 0.51630(4) 0.0216(3) Uani 1 1 d . . . . . H5C H 0.302955 -0.122042 0.517364 0.032 Uiso 1 1 d R . . . . H5D H 0.402365 -0.092342 0.485464 0.032 Uiso 1 1 d R . . . . 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 0.0227(6) 0.0157(6) 0.0253(6) 0.0020(4) 0.0007(4) 0.0004(4) O2 0.0344(7) 0.0151(6) 0.0309(6) 0.0065(5) -0.0041(5) -0.0033(5) O3 0.0192(6) 0.0270(6) 0.0181(5) -0.0018(4) 0.0003(4) -0.0011(4) O4 0.0233(6) 0.0210(5) 0.0177(5) -0.0020(4) -0.0035(4) 0.0025(4) C1 0.0154(7) 0.0166(8) 0.0189(8) -0.0008(6) -0.0004(6) 0.0016(6) C2 0.0221(8) 0.0195(8) 0.0160(7) 0.0009(6) 0.0012(6) 0.0006(6) C3 0.0251(8) 0.0169(8) 0.0245(8) 0.0006(6) -0.0031(6) 0.0019(6) C4 0.0272(9) 0.0235(8) 0.0277(9) -0.0066(7) 0.0016(7) 0.0045(7) C5 0.0286(9) 0.0242(8) 0.0211(8) -0.0062(6) 0.0004(6) -0.0033(7) C6 0.0219(8) 0.0269(9) 0.0219(8) -0.0015(6) -0.0047(6) -0.0018(7) C7 0.0290(9) 0.0257(8) 0.0178(7) 0.0020(6) -0.0033(6) -0.0004(7) C8 0.0254(8) 0.0271(9) 0.0170(8) 0.0021(6) 0.0024(6) -0.0037(7) C9 0.0181(8) 0.0208(8) 0.0229(8) -0.0011(6) 0.0030(6) -0.0019(6) C10 0.0228(8) 0.0337(9) 0.0222(8) -0.0089(7) 0.0054(6) -0.0013(7) O5 0.0202(5) 0.0200(5) 0.0245(6) -0.0046(4) 0.0038(4) -0.0042(4) 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 O2 110.27(10) . . ? O1 O2 H2 96.2 . . ? C1 O3 O4 108.87(10) . . ? O3 O4 H4 98.8 . . ? O1 C1 C2 104.32(11) . . ? O1 C1 C8 113.54(12) . . ? O3 C1 O1 109.61(11) . . ? O3 C1 C2 114.35(12) . . ? O3 C1 C8 104.62(11) . . ? C2 C1 C8 110.65(12) . . ? C1 C2 H2A 109.8 . . ? C1 C2 C3 108.26(12) . . ? C1 C2 C9 109.85(12) . . ? C3 C2 H2A 109.8 . . ? C9 C2 H2A 109.8 . . ? C9 C2 C3 109.27(12) . . ? C2 C3 H3A 109.7 . . ? C2 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C4 C3 C2 109.98(12) . . ? C4 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 . . ? C3 C4 H4A 109.6 . . ? C3 C4 C5 109.90(13) . . ? C3 C4 C10 108.84(13) . . ? C5 C4 H4A 109.6 . . ? C5 C4 C10 109.34(13) . . ? C10 C4 H4A 109.6 . . ? C4 C5 H5A 109.7 . . ? C4 C5 H5B 109.7 . . ? C4 C5 C6 109.88(12) . . ? H5A C5 H5B 108.2 . . ? C6 C5 H5A 109.7 . . ? C6 C5 H5B 109.7 . . ? C5 C6 H6 109.6 . . ? C7 C6 C5 109.66(13) . . ? C7 C6 H6 109.6 . . ? C7 C6 C9 109.70(12) . . ? C9 C6 C5 108.81(12) . . ? C9 C6 H6 109.6 . . ? C6 C7 H7B 109.6 . . ? C6 C7 H7A 109.6 . . ? C6 C7 C8 110.06(12) . . ? H7B C7 H7A 108.2 . . ? C8 C7 H7B 109.6 . . ? C8 C7 H7A 109.6 . . ? C1 C8 C7 107.66(12) . . ? C1 C8 H8 109.9 . . ? C7 C8 H8 109.9 . . ? C10 C8 C1 109.75(12) . . ? C10 C8 C7 109.62(13) . . ? C10 C8 H8 109.9 . . ? C2 C9 C6 109.55(12) . . ? C2 C9 H9A 109.8 . . ? C2 C9 H9B 109.8 . . ? C6 C9 H9A 109.8 . . ? C6 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C4 C10 H10A 109.7 . . ? C4 C10 H10B 109.7 . . ? C8 C10 C4 109.65(13) . . ? C8 C10 H10A 109.7 . . ? C8 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? H5C O5 H5D 102.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 O2 1.4668(15) . ? O1 C1 1.4278(18) . ? O2 H2 0.9694 . ? O3 O4 1.4733(14) . ? O3 C1 1.4184(18) . ? O4 H4 0.9224 . ? C1 C2 1.531(2) . ? C1 C8 1.5315(19) . ? C2 H2A 1.0000 . ? C2 C3 1.544(2) . ? C2 C9 1.532(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.527(2) . ? C4 H4A 1.0000 . ? C4 C5 1.531(2) . ? C4 C10 1.541(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.535(2) . ? C6 H6 1.0000 . ? C6 C7 1.529(2) . ? C6 C9 1.534(2) . ? C7 H7B 0.9900 . ? C7 H7A 0.9900 . ? C7 C8 1.545(2) . ? C8 H8 1.0000 . ? C8 C10 1.531(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? O5 H5C 0.8412 . ? O5 H5D 0.8509 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O2 H2 O5 0.97 1.86 2.8079(15) 164.5 . yes O4 H4 O5 0.92 1.75 2.6612(14) 168.8 . yes O5 H5C O3 0.84 2.42 3.1175(15) 140.8 8_655 yes O5 H5C O4 0.84 1.89 2.7300(14) 177.5 8_655 yes O5 H5D O1 0.85 1.95 2.7945(15) 170.7 5_656 yes 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 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 178.27(11) . . . . ? O1 C1 C2 C9 -62.48(14) . . . . ? O1 C1 C8 C7 56.77(16) . . . . ? O1 C1 C8 C10 176.02(12) . . . . ? O2 O1 C1 O3 -62.24(13) . . . . ? O2 O1 C1 C2 174.89(10) . . . . ? O2 O1 C1 C8 54.34(15) . . . . ? O3 C1 C2 C3 58.55(15) . . . . ? O3 C1 C2 C9 177.80(11) . . . . ? O3 C1 C8 C7 176.24(12) . . . . ? O3 C1 C8 C10 -64.50(15) . . . . ? O4 O3 C1 O1 -64.96(13) . . . . ? O4 O3 C1 C2 51.74(14) . . . . ? O4 O3 C1 C8 172.96(10) . . . . ? C1 C2 C3 C4 60.65(16) . . . . ? C1 C2 C9 C6 -58.26(16) . . . . ? C1 C8 C10 C4 -58.81(16) . . . . ? C2 C1 C8 C7 -60.13(16) . . . . ? C2 C1 C8 C10 59.13(16) . . . . ? C2 C3 C4 C5 58.42(17) . . . . ? C2 C3 C4 C10 -61.29(16) . . . . ? C3 C2 C9 C6 60.37(16) . . . . ? C3 C4 C5 C6 -59.35(17) . . . . ? C3 C4 C10 C8 60.02(16) . . . . ? C4 C5 C6 C7 -59.62(16) . . . . ? C4 C5 C6 C9 60.36(16) . . . . ? C5 C4 C10 C8 -60.04(16) . . . . ? C5 C6 C7 C8 58.76(16) . . . . ? C5 C6 C9 C2 -61.08(16) . . . . ? C6 C7 C8 C1 60.48(16) . . . . ? C6 C7 C8 C10 -58.87(16) . . . . ? C7 C6 C9 C2 58.88(16) . . . . ? C7 C8 C10 C4 59.24(16) . . . . ? C8 C1 C2 C3 -59.27(15) . . . . ? C8 C1 C2 C9 59.97(15) . . . . ? C9 C2 C3 C4 -58.96(16) . . . . ? C9 C6 C7 C8 -60.67(16) . . . . ? C10 C4 C5 C6 60.06(16) . . . . ?