#------------------------------------------------------------------------------ #$Date: 2021-09-24 01:49:09 +0300 (Fri, 24 Sep 2021) $ #$Revision: 269268 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/35/7243573.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_7243573 loop_ _publ_author_name 'Gamidi, Rama Krishna' 'Dandawate, Monica' 'Choudhury, Rahul' 'Tothadi, Srinu' 'Nangia, Ashwini' 'Reddy, D. Srinivasa' _publ_section_title ; Separation of a diastereomeric diol pair using mechanical properties of crystals ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D1CE01055G _journal_year 2021 _chemical_absolute_configuration S,S _chemical_formula_sum 'C14 H20 O2' _chemical_formula_weight 220.30 _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' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2020-12-03 deposited with the CCDC. 2021-09-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.0851(17) _cell_length_b 13.6181(18) _cell_length_c 18.784(2) _cell_measurement_reflns_used 9881 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 72.64 _cell_measurement_theta_min 5.73 _cell_volume 1300.8(5) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 VENTURE Kappa Duo PHOTON II CPAD' _diffrn_measurement_method '\ f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_unetI/netI 0.0216 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 53763 _diffrn_reflns_point_group_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 72.483 _diffrn_reflns_theta_min 5.722 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_correction_T_min 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS; Bruker, 2016' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.125 _exptl_crystal_description needle _exptl_crystal_F_000 480 _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.096 _refine_diff_density_max 0.185 _refine_diff_density_min -0.159 _refine_diff_density_rms 0.034 _refine_ls_abs_structure_details ; Flack x determined using 986 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(7) _refine_ls_extinction_coef 0.0059(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 149 _refine_ls_number_reflns 2552 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.069 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0338 _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^)+(0.0364P)^2^+0.3375P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.0814 _reflns_Friedel_coverage 0.681 _reflns_Friedel_fraction_full 0.992 _reflns_Friedel_fraction_max 0.990 _reflns_number_gt 2446 _reflns_number_total 2552 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1ce01055g4.cif _cod_data_source_block Peak1 _cod_database_code 7243573 _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 ; Peak1.res created by SHELXL-2014/7 TITL Peak1_a.res in P2(1)2(1)2(1) CELL 1.54178 5.0851 13.6181 18.7837 90.000 90.000 90.000 ZERR 4.000 0.0017 0.0018 0.0022 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H O UNIT 56 80 8 REM Old TITL Peak1 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.116, Rweak 0.033, Alpha 0.001, Orientation as input REM Flack x= 0.133 ( 0.059 ) from Parsons' quotients REM Formula found by SHELXT: C13 O3 L.S. 10 ACTA BOND $H FMAP 2 PLAN 10 TEMP -173.150 WGHT 0.036400 0.337500 EXTI 0.005938 FVAR 1.29393 C1 1 0.250182 0.181575 0.797892 11.00000 0.05682 0.03530 = 0.02821 0.00646 -0.00332 -0.00850 AFIX 93 H1A 2 0.414221 0.206019 0.814377 11.00000 -1.20000 H1B 2 0.135840 0.148178 0.829727 11.00000 -1.20000 AFIX 0 C2 1 0.181167 0.194009 0.730789 11.00000 0.02740 0.02195 = 0.02587 0.00117 -0.00075 -0.00185 AFIX 43 H2A 2 0.015613 0.168488 0.716405 11.00000 -1.20000 AFIX 0 C3 1 0.342934 0.245098 0.675582 11.00000 0.01690 0.02116 = 0.02472 0.00133 -0.00354 -0.00066 AFIX 23 H3A 2 0.410124 0.195825 0.641364 11.00000 -1.20000 H3B 2 0.496402 0.276118 0.698947 11.00000 -1.20000 AFIX 0 C4 1 0.188214 0.324538 0.634349 11.00000 0.01156 0.02057 = 0.01947 -0.00174 -0.00225 -0.00043 C5 1 0.371313 0.377224 0.581286 11.00000 0.01206 0.02006 = 0.01926 -0.00246 -0.00112 0.00202 AFIX 13 H5 2 0.507154 0.414048 0.609020 11.00000 -1.20000 AFIX 0 C6 1 0.233142 0.449742 0.530979 11.00000 0.01585 0.02438 = 0.02441 0.00299 -0.00113 0.00223 AFIX 23 H6A 2 0.124433 0.413004 0.496304 11.00000 -1.20000 H6B 2 0.115401 0.493091 0.558802 11.00000 -1.20000 AFIX 0 C7 1 0.433425 0.511225 0.491689 11.00000 0.01792 0.02138 = 0.02519 0.00444 -0.00254 0.00376 C8 1 0.526737 0.484324 0.424781 11.00000 0.02776 0.02661 = 0.02439 0.00211 -0.00184 -0.00091 AFIX 43 H8 2 0.452850 0.429047 0.401291 11.00000 -1.20000 AFIX 0 C9 1 0.726255 0.537145 0.391906 11.00000 0.03342 0.03616 = 0.02714 0.00696 0.00502 -0.00031 AFIX 43 H9 2 0.788896 0.517451 0.346447 11.00000 -1.20000 AFIX 0 C10 1 0.834630 0.618767 0.425313 11.00000 0.02487 0.03326 = 0.04000 0.01681 0.00076 -0.00416 AFIX 43 H10 2 0.971854 0.654707 0.402977 11.00000 -1.20000 AFIX 0 C11 1 0.740732 0.647386 0.491622 11.00000 0.03042 0.02319 = 0.04181 0.00379 -0.00620 -0.00430 AFIX 43 H11 2 0.812605 0.703363 0.514695 11.00000 -1.20000 AFIX 0 C12 1 0.541691 0.593934 0.524002 11.00000 0.02753 0.02393 = 0.02819 0.00055 -0.00190 0.00218 AFIX 43 H12 2 0.477821 0.614181 0.569207 11.00000 -1.20000 AFIX 0 C13 1 0.053552 0.397046 0.685421 11.00000 0.01770 0.02237 = 0.02100 -0.00232 0.00124 -0.00001 AFIX 23 H13A 2 -0.054017 0.443306 0.657049 11.00000 -1.20000 H13B 2 -0.067404 0.359877 0.716718 11.00000 -1.20000 AFIX 0 C14 1 0.241926 0.456313 0.732075 11.00000 0.02821 0.03164 = 0.02777 -0.01040 0.00071 -0.00380 AFIX 137 H14A 2 0.353247 0.411358 0.759488 11.00000 -1.50000 H14B 2 0.140576 0.497671 0.764788 11.00000 -1.50000 H14C 2 0.352714 0.497905 0.701855 11.00000 -1.50000 AFIX 0 O1 3 -0.020628 0.276102 0.596407 11.00000 0.01237 0.02385 = 0.02029 -0.00468 -0.00127 -0.00020 AFIX 147 H1 2 0.041715 0.246638 0.560929 11.00000 -1.50000 AFIX 0 O2 3 0.502843 0.306302 0.537600 11.00000 0.01429 0.02492 = 0.02080 -0.00257 -0.00039 0.00438 AFIX 147 H2 2 0.653214 0.295160 0.554256 11.00000 -1.50000 AFIX 0 HKLF 4 REM Peak1_a.res in P2(1)2(1)2(1) REM R1 = 0.0338 for 2446 Fo > 4sig(Fo) and 0.0361 for all 2552 data REM 149 parameters refined using 0 restraints END WGHT 0.0364 0.3375 REM Highest difference peak 0.185, deepest hole -0.159, 1-sigma level 0.034 Q1 1 0.3179 0.3350 0.6182 11.00000 0.05 0.19 Q2 1 0.2322 0.3567 0.6037 11.00000 0.05 0.15 Q3 1 0.4567 0.4985 0.4609 11.00000 0.05 0.13 Q4 1 -0.1633 0.3052 0.5841 11.00000 0.05 0.13 Q5 1 0.0806 0.4497 0.5159 11.00000 0.05 0.13 Q6 1 0.5223 0.3836 0.6187 11.00000 0.05 0.12 Q7 1 0.3082 0.4109 0.5548 11.00000 0.05 0.11 Q8 1 0.3740 0.4721 0.5141 11.00000 0.05 0.11 Q9 1 -0.0099 0.3267 0.5383 11.00000 0.05 0.11 Q10 1 0.5020 0.2467 0.6787 11.00000 0.05 0.11 ; _shelx_res_checksum 43979 _shelx_hkl_file ; 1 0 0 0.00 1.20 1 0 0 -0.20 0.80 1 0 0 -1.20 0.70 -1 0 0 6.00 3.90 -1 0 0 0.60 1.10 -1 0 0 5.70 3.20 -1 0 0 -0.30 1.60 1 0 0 -0.50 1.10 1 0 0 -0.60 4.30 -1 0 0 0.90 2.40 -1 0 0 -0.70 3.20 -1 0 0 1.80 1.40 -2 0 0 30.70 8.30 -2 0 0 29.20 5.30 2 0 0 23.90 2.90 2 0 0 33.20 3.30 -2 0 0 23.00 5.70 -2 0 0 32.20 3.80 -2 0 0 29.00 6.50 2 0 0 27.30 2.80 2 0 0 29.10 3.30 2 0 0 31.90 3.00 -2 0 0 37.10 4.40 2 0 0 30.50 3.00 2 0 0 33.90 3.10 2 0 0 18.40 8.00 3 0 0 0.90 1.30 -3 0 0 1.90 2.90 3 0 0 2.60 6.70 3 0 0 -0.60 4.10 -3 0 0 0.80 5.30 -3 0 0 0.80 3.10 3 0 0 -0.70 1.20 3 0 0 -2.30 1.80 3 0 0 0.80 1.30 -3 0 0 -1.00 0.90 -3 0 0 1.80 5.50 3 0 0 0.30 1.30 3 0 0 2.30 2.20 -3 0 0 -4.60 5.40 -4 0 0 2604.34 170.98 4 0 0 2403.66 163.28 -4 0 0 2026.30 164.88 -4 0 0 2754.82 185.38 -4 0 0 2458.45 169.78 -4 0 0 2529.05 190.48 -4 0 0 2391.36 166.48 -4 0 0 2487.75 176.68 -4 0 0 2385.66 164.38 -4 0 0 2616.44 170.38 4 0 0 2090.49 161.08 5 0 0 -3.10 5.30 -5 0 0 -6.70 6.90 -5 0 0 -5.80 3.50 5 0 0 -1.90 2.50 -5 0 0 -2.20 7.30 -5 0 0 -3.20 11.80 -5 0 0 3.40 5.80 -5 0 0 0.50 8.10 -5 0 0 -6.50 6.40 -5 0 0 1.70 7.70 -5 0 0 9.40 9.80 -6 0 0 176.98 26.20 -6 0 0 118.89 18.80 -6 0 0 155.78 24.20 -6 0 0 125.39 17.40 -6 0 0 151.58 22.20 0 -1 0 0.10 0.20 0 -1 0 0.00 0.70 0 -1 0 0.10 0.40 0 1 0 0.10 0.50 0 1 0 0.60 0.30 0 1 0 2.70 0.70 0 -1 0 0.30 0.30 0 1 0 0.00 0.70 0 -1 0 -0.70 0.30 0 1 0 0.00 0.30 0 1 0 2.10 0.60 0 -1 0 -0.20 0.30 0 1 0 0.10 0.40 0 1 0 0.30 0.30 0 -1 0 0.30 1.10 0 1 0 0.00 0.40 -1 -1 0 55.49 7.20 1 1 0 53.99 5.00 1 1 0 41.70 6.40 1 1 0 59.99 4.60 1 -1 0 58.49 4.00 -1 1 0 52.49 6.70 1 -1 0 41.90 8.20 1 1 0 57.29 4.80 -1 1 0 43.80 7.90 -1 -1 0 57.29 6.60 -1 -1 0 52.69 5.20 1 1 0 56.39 4.30 -1 -1 0 56.09 7.10 1 1 0 54.89 4.10 1 1 0 58.99 4.40 1 1 0 55.29 4.10 -1 -1 0 57.59 5.80 -1 1 0 54.39 6.90 -1 -1 0 56.89 4.70 -1 -1 0 59.29 4.80 1 -1 0 56.29 3.90 -1 1 0 55.99 5.20 1 -1 0 50.09 4.30 1 -1 0 61.29 4.90 -1 1 0 56.29 7.20 1 -1 0 62.69 4.90 1 -1 0 54.59 4.40 1 -1 0 58.79 5.00 -1 1 0 55.39 4.80 -2 1 0 3.20 3.60 -2 1 0 0.60 2.00 2 1 0 4.10 0.90 2 1 0 2.80 1.70 -2 -1 0 5.80 1.70 2 1 0 4.90 1.30 2 -1 0 3.90 1.20 -2 -1 0 5.20 4.50 2 1 0 4.50 1.20 2 1 0 6.30 1.00 2 1 0 4.40 1.20 -2 1 0 7.40 2.10 -2 1 0 5.00 1.90 -2 1 0 8.90 3.50 2 -1 0 5.40 1.10 -2 1 0 1.10 3.80 2 -1 0 3.90 1.30 -2 -1 0 5.70 3.70 2 -1 0 1.80 5.00 2 -1 0 8.00 1.80 -2 -1 0 5.70 2.80 2 1 0 6.10 1.90 2 1 0 2.30 3.90 -2 -1 0 7.00 2.20 2 -1 0 5.20 1.20 2 -1 0 4.60 4.20 -2 -1 0 4.50 3.10 -3 1 0 106.09 13.00 -3 1 0 92.59 12.20 3 1 0 95.19 8.90 3 -1 0 88.99 16.40 -3 1 0 103.69 9.50 -3 -1 0 118.69 16.30 3 -1 0 112.59 8.20 -3 1 0 104.09 9.00 -3 1 0 114.79 14.60 3 -1 0 106.09 8.40 3 1 0 103.49 8.90 -3 -1 0 78.49 10.90 3 -1 0 112.89 7.80 -3 -1 0 97.89 13.10 3 1 0 102.89 8.50 3 -1 0 81.19 19.10 -3 1 0 89.69 15.80 3 -1 0 98.99 8.40 -3 -1 0 101.29 8.80 -3 -1 0 109.39 14.20 3 -1 0 95.89 9.00 3 1 0 116.39 9.10 3 1 0 99.29 8.20 3 1 0 100.99 8.70 -4 -1 0 237.18 34.30 -4 1 0 218.38 33.50 4 1 0 200.38 18.60 -4 1 0 288.77 26.20 -4 -1 0 283.57 27.20 4 -1 0 262.17 20.70 -4 1 0 280.17 31.40 -4 1 0 236.28 31.20 4 1 0 235.68 18.50 -4 1 0 226.48 35.30 -4 -1 0 266.07 26.40 -4 1 0 293.67 25.00 4 -1 0 187.08 31.30 -4 -1 0 267.07 23.90 -4 -1 0 294.77 30.80 -4 -1 0 248.48 25.90 -4 -1 0 247.78 36.20 4 -1 0 233.68 18.40 4 -1 0 254.87 17.80 -4 -1 0 196.38 22.70 -4 1 0 288.27 29.00 -4 1 0 237.78 21.30 -4 1 0 238.08 30.90 5 -1 0 6.70 2.90 -5 1 0 5.40 11.00 -5 -1 0 1.20 12.40 -5 -1 0 9.10 7.50 -5 -1 0 5.20 6.10 -5 -1 0 3.60 11.90 -5 1 0 5.30 7.60 -5 -1 0 6.80 5.70 -5 -1 0 7.50 8.90 -5 1 0 8.70 8.80 5 1 0 5.00 3.70 -5 1 0 0.30 7.50 -5 -1 0 5.20 5.60 5 -1 0 0.10 6.70 -5 -1 0 1.50 7.50 -5 -1 0 -0.40 5.60 -5 1 0 0.60 3.90 -5 1 0 6.20 5.00 -5 1 0 7.90 10.00 5 -1 0 6.90 5.80 -5 1 0 4.50 8.70 -6 1 0 86.89 11.30 -6 1 0 80.59 16.50 -6 1 0 93.89 18.80 -6 1 0 64.59 12.70 -6 1 0 70.99 10.50 -6 -1 0 82.89 17.30 -6 -1 0 88.09 17.80 -6 -1 0 63.09 14.00 -6 -1 0 93.29 15.40 0 2 0 96.39 6.50 0 2 0 101.59 9.80 0 -2 0 97.09 9.30 0 2 0 76.89 6.90 0 -2 0 80.39 6.70 0 -2 0 77.09 7.20 0 2 0 105.29 8.90 0 -2 0 91.99 7.00 0 2 0 76.79 6.80 0 2 0 88.89 6.90 0 -2 0 73.89 6.60 0 -2 0 81.19 6.50 0 -2 0 87.69 6.50 0 -2 0 99.09 8.50 0 -2 0 106.59 9.00 1 2 0 9.10 2.80 -1 2 0 17.60 2.10 1 2 0 8.80 1.80 -1 -2 0 10.30 1.50 -1 -2 0 12.90 1.70 1 -2 0 9.70 4.50 -1 2 0 9.40 1.60 1 2 0 7.80 2.80 1 -2 0 14.60 3.10 -1 -2 0 12.20 2.50 1 -2 0 13.40 2.00 -1 -2 0 12.10 3.60 1 2 0 8.00 2.00 -1 2 0 17.00 2.50 -1 2 0 11.60 3.50 -1 2 0 10.40 6.30 -1 -2 0 10.00 3.70 -1 -2 0 11.60 3.30 1 2 0 12.60 2.50 -1 2 0 7.40 5.20 -1 2 0 12.60 3.40 -1 -2 0 15.30 3.30 1 -2 0 6.50 2.30 1 2 0 10.50 2.70 1 2 0 12.30 1.90 1 -2 0 7.30 1.80 -1 -2 0 12.90 1.70 1 -2 0 6.00 4.00 1 2 0 12.10 1.70 -2 2 0 360.26 28.90 -2 2 0 390.06 37.10 -2 -2 0 305.07 27.90 2 2 0 316.87 31.20 -2 -2 0 380.56 30.70 -2 -2 0 381.56 27.20 -2 2 0 387.66 26.70 2 2 0 399.86 25.30 -2 2 0 393.16 26.20 2 2 0 388.66 26.60 -2 -2 0 367.16 26.80 -2 2 0 345.97 27.70 -2 -2 0 410.16 30.70 2 -2 0 438.86 27.00 2 -2 0 374.26 26.00 -2 -2 0 412.86 26.30 2 -2 0 396.96 26.00 2 2 0 332.97 25.20 2 2 0 411.66 26.30 2 2 0 393.16 26.00 -2 2 0 347.27 31.70 2 -2 0 320.77 34.00 2 2 0 409.06 26.00 -2 -2 0 348.07 29.60 3 2 0 188.38 14.00 -3 2 0 190.78 19.60 3 -2 0 148.89 22.00 3 2 0 197.68 14.60 -3 -2 0 204.58 21.20 3 -2 0 200.98 16.40 -3 2 0 186.98 15.20 -3 -2 0 189.28 21.50 -3 2 0 201.38 21.10 -3 -2 0 185.48 27.70 -3 2 0 147.29 27.00 -3 -2 0 173.98 28.50 3 -2 0 195.18 14.50 3 -2 0 186.18 14.20 -3 2 0 173.98 23.40 -3 2 0 189.48 26.90 -3 2 0 200.18 14.80 -3 2 0 190.48 17.90 3 2 0 202.18 15.10 -3 -2 0 192.38 20.60 -3 -2 0 184.08 18.10 3 2 0 192.28 14.60 -4 -2 0 -1.70 8.50 -4 -2 0 4.90 9.40 -4 2 0 6.50 6.60 -4 2 0 -0.20 6.60 -4 2 0 10.00 6.60 -4 -2 0 -6.70 7.30 -4 -2 0 1.40 4.90 4 -2 0 -0.30 9.30 -4 2 0 -1.30 6.30 -4 2 0 6.10 8.90 -4 2 0 -6.50 3.90 -4 -2 0 -5.10 6.40 -4 -2 0 -2.10 7.60 -4 -2 0 -1.80 10.00 4 2 0 -2.50 4.50 4 2 0 0.20 2.00 -4 2 0 2.20 7.60 4 -2 0 4.00 2.30 4 2 0 3.00 2.30 -4 2 0 -6.20 6.10 -4 2 0 1.90 9.90 -4 2 0 0.80 8.10 4 2 0 -3.80 5.90 -4 -2 0 3.90 4.70 -4 -2 0 7.10 5.60 4 -2 0 -1.20 2.30 4 -2 0 5.50 3.10 4 -2 0 2.50 4.50 -5 2 0 17.50 9.10 -5 -2 0 27.10 12.30 -5 -2 0 16.50 9.60 -5 2 0 13.80 9.80 -5 2 0 15.90 9.90 5 2 0 16.10 4.50 -5 2 0 18.30 9.10 -5 -2 0 11.10 7.10 -5 -2 0 22.00 10.10 5 2 0 17.50 4.50 -5 -2 0 16.00 6.50 5 -2 0 8.60 5.40 -5 2 0 15.20 7.70 -5 -2 0 7.50 7.70 -5 -2 0 15.80 10.80 -5 2 0 20.40 12.00 -5 2 0 17.20 5.00 -5 -2 0 23.00 13.20 -6 2 0 965.70 78.89 -6 -2 0 1212.48 85.19 -6 2 0 997.10 82.29 -6 2 0 1039.80 82.79 -6 2 0 1254.17 76.99 -6 -2 0 1001.90 82.89 -6 -2 0 1029.20 78.89 0 -3 0 0.00 1.30 0 3 0 0.30 1.60 0 -3 0 -1.10 3.00 0 -3 0 0.60 1.30 0 -3 0 -0.30 3.40 0 3 0 0.10 4.20 0 3 0 1.30 2.20 0 3 0 -1.00 2.30 0 -3 0 1.00 1.80 0 -3 0 -0.20 1.20 0 -3 0 1.10 1.60 0 -3 0 0.50 3.00 0 3 0 -0.20 1.90 0 -3 0 -0.10 2.30 0 3 0 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-5 20 32.90 5.20 2 -5 20 44.30 7.10 -2 -5 -20 32.40 6.60 2 -5 20 30.10 5.00 -2 -5 -20 33.30 6.60 -2 5 -20 46.30 8.40 2 -5 -20 31.70 5.70 -2 5 -20 22.10 4.90 -2 5 -20 43.70 11.30 2 5 20 23.40 5.40 2 5 20 27.70 5.00 2 5 20 26.10 6.30 -2 -5 20 37.20 5.90 0 -6 -20 40.80 6.00 0 -6 20 41.70 7.10 0 6 20 25.60 4.80 0 -6 20 52.09 6.00 0 6 -20 37.40 8.10 0 6 20 30.30 6.80 0 6 -20 47.40 6.50 0 6 20 23.90 7.90 0 6 -20 49.80 10.60 0 6 -20 34.40 8.10 0 6 20 46.30 7.50 0 -6 20 43.70 6.70 -1 6 20 27.60 5.10 -1 -6 -20 37.50 7.50 -1 6 20 26.80 6.80 1 -6 20 21.90 5.30 -1 6 20 19.50 5.20 1 6 -20 28.90 5.50 1 6 -20 24.00 5.90 1 -6 20 30.80 5.50 1 -6 20 29.40 5.50 -1 6 -20 35.20 8.10 1 6 20 20.70 5.20 1 6 20 26.20 5.40 -1 -6 20 31.40 6.00 -1 6 -20 33.20 10.60 1 6 20 26.70 5.40 -1 -6 20 21.60 5.70 -1 6 -20 24.20 4.20 1 6 20 28.50 4.90 -1 6 -20 33.30 7.20 -1 -6 20 26.70 4.70 1 -6 -20 36.30 6.20 2 -6 20 32.20 6.20 2 -6 20 14.90 3.50 -2 -6 -20 22.70 8.60 2 -6 20 16.50 5.50 -2 6 20 22.10 4.30 -2 -6 -20 26.50 5.40 2 6 -20 27.10 8.10 2 6 -20 38.90 5.60 2 6 20 25.40 5.30 -2 6 -20 28.40 6.40 -2 -6 20 31.80 5.50 -2 -6 20 22.20 4.30 2 -6 -20 15.70 4.20 -2 6 -20 29.20 7.30 2 6 20 17.50 4.20 2 6 20 16.40 5.40 0 7 20 7.90 3.70 0 7 -20 0.10 3.90 0 7 20 -5.30 3.80 0 7 -20 -2.70 5.30 0 -7 -20 0.40 2.50 0 7 -20 4.20 3.50 0 -7 20 -0.70 3.30 0 7 20 -3.80 3.90 1 7 -20 3.10 4.50 -1 7 20 6.80 3.70 1 7 -20 3.60 5.20 -1 -7 -20 2.40 6.10 1 -7 20 3.30 2.60 1 7 -20 3.70 3.40 1 -7 20 3.00 3.10 1 7 20 -1.00 3.70 1 7 20 8.00 4.50 -1 7 -20 -3.60 5.90 -1 7 -20 8.50 8.00 -1 -7 20 2.10 3.70 1 7 20 0.60 2.80 1 -7 -20 4.20 3.70 -1 -7 20 1.50 3.40 -1 -7 20 2.10 3.00 1 7 20 1.70 5.30 -1 7 -20 1.40 4.20 0 8 -20 32.80 7.80 0 8 20 48.10 8.90 0 -8 20 22.90 4.90 0 8 -20 27.60 4.20 0 -8 -20 35.60 4.60 1 -8 20 49.20 6.40 1 8 -20 55.09 9.50 1 -8 20 40.60 5.10 -1 -8 -20 57.59 7.40 1 8 -20 46.20 6.00 -1 8 -20 38.50 8.80 1 8 20 43.10 5.10 1 8 20 30.90 5.80 -1 -8 20 40.80 6.10 1 -8 -20 49.70 5.60 -1 8 -20 67.39 9.60 0 0 21 -13.00 5.50 0 0 -21 1.10 4.20 0 0 -21 -7.00 9.60 0 0 -21 3.10 3.70 0 0 21 -4.80 3.60 0 0 21 -0.70 2.70 0 0 21 1.90 8.50 1 0 21 99.19 11.30 1 0 21 52.89 15.00 -1 0 -21 78.49 6.90 -1 0 21 90.69 10.40 -1 0 -21 63.29 8.30 1 0 -21 92.89 10.20 -1 0 -21 86.99 10.30 1 0 21 70.49 9.80 -1 0 21 87.99 11.20 1 0 21 92.19 10.20 -1 0 21 86.59 10.30 1 0 -21 88.89 11.10 -1 0 21 79.09 11.00 1 0 21 76.29 11.30 2 0 21 18.30 4.70 -2 0 21 11.30 3.50 -2 0 21 18.70 4.80 2 0 -21 23.60 8.10 -2 0 -21 19.20 5.30 -2 0 21 11.40 5.00 2 0 21 12.40 4.30 2 0 -21 17.80 4.20 2 0 21 13.80 4.10 -2 0 -21 18.60 3.40 -2 0 -21 23.60 8.80 0 1 -21 163.68 17.10 0 1 21 221.08 19.20 0 -1 21 207.68 18.20 0 -1 21 202.98 17.50 0 1 21 202.28 17.20 0 -1 21 204.18 18.00 0 1 -21 167.28 16.30 0 -1 21 203.58 16.50 0 1 21 176.48 18.60 0 1 21 193.58 15.80 0 -1 -21 204.68 16.70 0 -1 -21 196.28 17.00 0 1 21 157.28 18.00 0 -1 21 198.98 18.10 1 -1 21 264.87 23.00 1 1 -21 253.77 21.90 -1 -1 -21 255.37 21.80 -1 -1 -21 297.37 26.00 1 1 -21 266.57 21.50 -1 1 21 251.87 21.50 1 -1 21 266.07 21.40 -1 1 21 316.97 22.80 -1 1 21 286.47 22.40 1 -1 21 266.87 21.90 -1 1 21 239.18 21.50 -1 -1 -21 227.48 18.30 1 -1 21 232.68 21.30 1 -1 21 290.17 21.10 -1 -1 21 289.67 22.10 -1 1 -21 261.87 22.00 1 1 21 279.27 24.00 -1 1 -21 243.58 18.70 -1 -1 21 245.88 22.10 1 1 21 234.68 21.40 1 1 21 352.26 28.00 -1 1 -21 220.88 20.10 -1 -1 21 232.88 21.50 1 1 21 282.97 21.10 -1 -1 21 297.07 25.40 1 1 21 262.17 21.60 1 -1 -21 259.97 21.30 -1 1 -21 268.47 26.40 2 -1 21 75.79 7.20 2 -1 21 75.69 9.40 -2 -1 -21 78.89 12.90 2 -1 21 71.59 8.50 -2 -1 -21 61.99 7.10 -2 -1 -21 73.49 12.00 2 1 -21 66.29 8.00 -2 1 21 63.09 9.30 -2 -1 -21 62.79 9.60 2 -1 -21 64.19 8.00 -2 1 -21 68.79 7.40 -2 -1 21 64.59 6.40 -2 -1 21 67.89 9.00 -2 1 -21 72.39 12.20 2 1 21 61.39 7.90 2 1 21 73.99 10.10 2 1 21 70.79 8.60 0 2 21 222.18 18.80 0 -2 -21 223.58 18.70 0 2 21 233.68 18.60 0 2 -21 177.98 19.10 0 -2 21 253.57 20.40 0 2 21 222.28 19.60 0 2 -21 237.88 19.00 0 -2 -21 214.18 19.40 0 -2 21 231.18 18.30 0 -2 21 251.37 21.00 0 2 21 245.08 20.40 0 -2 21 242.98 19.50 1 -2 21 22.00 5.30 1 -2 21 21.60 5.40 -1 2 21 20.40 5.10 -1 -2 -21 17.10 2.80 -1 -2 -21 35.10 9.80 -1 2 21 27.30 12.70 1 -2 21 21.80 8.30 1 2 -21 30.10 6.60 1 2 -21 17.10 5.10 -1 -2 -21 33.30 6.90 -1 2 21 39.30 10.50 1 -2 21 16.50 5.50 1 -2 21 23.10 4.90 -1 2 21 13.20 6.20 -1 2 -21 26.50 6.20 -1 2 -21 19.60 2.90 -1 2 -21 45.70 12.90 1 2 21 19.60 5.10 1 2 21 69.69 15.50 1 2 21 20.80 5.00 -1 -2 21 35.50 6.60 -1 -2 21 23.70 4.80 1 -2 -21 21.80 5.30 -1 -2 21 28.90 5.80 1 2 21 17.30 6.10 -1 2 -21 22.50 8.30 1 -2 -21 12.10 3.70 1 2 21 24.40 10.30 -1 -2 21 21.10 8.60 -1 2 -21 19.80 4.20 -2 -2 -21 33.00 6.90 -2 2 21 23.80 4.00 -2 2 21 24.20 5.10 2 2 -21 18.20 4.90 2 -2 21 29.70 4.60 -2 -2 -21 15.90 4.20 2 2 -21 25.20 5.60 2 -2 21 25.40 4.70 -2 -2 -21 24.70 6.20 -2 2 21 27.50 6.40 2 -2 21 18.90 4.60 -2 -2 -21 32.60 7.20 2 2 21 9.40 4.70 -2 -2 21 23.60 3.50 -2 2 -21 36.90 10.30 -2 -2 21 14.50 6.20 -2 2 -21 37.10 6.80 2 2 21 19.90 5.10 -2 -2 21 26.20 4.30 -2 2 -21 38.70 5.30 2 2 21 30.50 6.00 2 -2 -21 26.70 5.70 2 2 21 23.70 4.80 0 3 21 1.00 3.50 0 -3 21 -2.20 4.80 0 3 21 0.70 4.20 0 3 21 -2.80 3.10 0 3 21 -3.40 5.50 0 -3 21 -7.40 6.10 0 -3 -21 -0.10 3.20 0 3 -21 -0.30 2.50 0 -3 21 -10.00 4.10 0 -3 21 -0.60 3.60 0 -3 -21 0.30 3.10 0 3 -21 2.60 3.50 0 3 21 0.70 3.10 0 -3 21 7.50 6.60 -1 3 21 28.80 6.10 -1 3 21 15.10 7.00 1 -3 21 29.00 6.10 1 3 -21 27.40 6.50 -1 3 21 24.70 5.80 -1 3 21 22.70 6.70 1 -3 21 33.10 7.50 -1 -3 -21 33.20 6.70 1 -3 21 22.20 5.80 1 3 -21 30.40 5.90 1 -3 21 27.50 6.10 -1 -3 -21 36.80 12.40 -1 3 -21 25.90 8.00 -1 -3 21 31.30 7.50 1 3 21 33.90 6.00 1 3 21 23.90 6.30 1 3 21 31.70 6.60 1 -3 -21 36.50 6.10 1 3 21 21.70 6.20 -1 -3 21 38.40 7.40 -1 -3 21 31.60 5.80 -1 3 -21 21.10 3.20 -1 -3 21 21.80 5.40 1 3 21 29.00 6.20 -1 3 -21 40.40 11.90 -2 -3 -21 6.50 5.20 2 -3 21 10.70 4.80 2 3 -21 2.10 3.90 2 -3 21 3.60 3.30 2 -3 21 7.20 3.30 2 3 -21 10.40 3.80 -2 3 21 5.10 5.10 -2 3 21 1.30 3.10 -2 -3 -21 5.10 5.00 -2 3 -21 5.30 7.90 -2 -3 21 0.90 5.00 -2 3 -21 1.30 3.90 2 3 21 1.90 3.30 -2 -3 21 -1.30 3.30 2 3 21 7.70 3.90 2 -3 -21 10.30 6.00 2 3 21 6.00 4.00 0 4 21 18.60 6.00 0 4 21 30.80 5.20 0 -4 21 41.50 6.70 0 -4 -21 25.30 6.00 0 4 -21 35.40 6.10 0 4 21 28.20 6.00 0 -4 21 27.50 4.70 0 4 21 30.90 6.50 0 -4 -21 31.80 5.20 0 4 -21 38.10 5.70 0 -4 21 26.10 5.50 1 -4 21 18.70 5.20 1 -4 21 15.10 5.20 -1 -4 -21 16.70 6.30 1 4 -21 16.80 4.60 -1 4 21 15.30 5.20 -1 4 21 20.70 4.80 1 -4 21 19.00 4.90 1 4 -21 17.60 4.90 -1 -4 21 20.40 5.50 1 4 21 16.50 4.40 1 4 21 16.00 4.20 -1 -4 21 13.70 4.20 1 -4 -21 18.50 4.70 1 -4 -21 13.30 4.40 -1 4 -21 11.60 2.10 1 4 21 14.00 5.50 -1 4 -21 18.70 6.50 -1 -4 21 10.50 4.50 -1 4 -21 18.40 8.00 1 4 21 10.00 4.20 2 4 -21 60.29 9.00 -2 -4 -21 56.69 9.00 2 -4 21 87.79 9.10 -2 4 21 66.49 7.90 2 -4 21 81.29 8.70 -2 -4 -21 76.99 9.40 2 4 -21 73.89 8.00 -2 -4 21 78.19 8.80 2 4 21 71.39 7.80 -2 4 -21 70.39 7.30 -2 4 -21 99.69 13.80 0 -5 21 -2.40 2.30 0 5 -21 -6.50 4.30 0 5 21 -1.90 4.10 0 5 21 -2.30 2.40 0 5 -21 0.30 5.40 0 5 -21 -0.60 3.30 0 -5 21 6.50 3.70 0 -5 -21 1.80 5.40 0 -5 21 0.70 3.80 0 -5 -21 0.40 3.30 0 5 21 0.80 4.00 -1 5 21 29.00 7.00 -1 -5 -21 40.10 7.50 1 5 -21 63.39 7.20 1 -5 21 46.80 5.80 -1 5 21 33.40 6.90 1 5 -21 42.20 7.20 1 -5 21 55.79 7.20 -1 -5 21 54.19 6.60 -1 -5 21 32.90 5.20 1 -5 -21 54.49 7.00 1 5 21 47.50 7.30 -1 -5 21 53.49 7.20 1 5 21 36.70 6.20 1 -5 -21 50.79 6.80 -1 5 -21 51.19 10.00 -1 5 -21 52.89 11.70 0 -6 -21 4.20 2.30 0 -6 21 1.80 3.30 0 6 -21 4.80 2.80 0 6 21 -0.30 6.80 0 -6 -21 4.50 6.10 0 6 21 2.10 3.60 0 6 -21 10.60 6.00 0 6 21 4.30 3.90 0 6 -21 -1.70 3.90 -1 6 21 -1.90 3.10 1 -6 21 4.70 2.60 1 6 -21 3.00 6.50 1 -6 21 -1.50 2.60 1 6 -21 -5.50 6.00 -1 -6 -21 7.00 8.50 1 6 -21 3.20 3.20 1 -6 -21 -4.90 3.60 1 -6 -21 3.10 3.30 1 6 21 4.20 2.70 1 6 21 -2.10 7.40 -1 6 -21 -1.00 4.20 -1 -6 21 3.30 2.50 -1 6 -21 -2.50 3.70 1 6 21 3.50 3.50 0 7 -21 34.40 7.50 0 -7 -21 35.80 4.00 0 -7 21 42.20 5.70 0 7 21 19.30 4.90 0 7 -21 39.40 5.00 0 -7 -21 35.00 6.30 0 0 22 211.48 17.20 0 0 -22 163.88 15.20 0 0 22 223.18 17.60 -1 0 22 39.70 6.80 -1 0 -22 57.69 11.50 1 0 22 69.39 8.90 1 0 22 36.50 7.00 -1 0 22 47.90 7.50 1 0 22 60.19 7.80 1 0 -22 61.09 7.30 -2 0 22 1.70 5.20 2 0 -22 6.20 3.60 2 0 22 12.00 3.20 0 1 -22 76.39 7.90 0 -1 -22 50.59 6.70 0 -1 22 71.49 9.00 0 1 22 54.19 9.50 0 -1 22 69.29 9.00 0 -1 22 75.79 7.60 0 -1 -22 62.29 7.40 0 1 22 68.19 8.90 -1 1 22 238.48 20.80 -1 1 22 278.97 21.40 1 1 -22 284.67 20.70 -1 -1 -22 271.07 25.20 1 -1 22 315.47 21.40 1 -1 22 244.78 21.10 -1 1 -22 305.67 24.20 -1 -1 22 209.78 20.10 -1 -1 22 250.37 21.10 1 -1 -22 270.77 20.70 1 1 22 242.78 20.30 1 1 22 246.68 20.60 1 1 22 329.27 26.80 -1 1 -22 269.67 25.70 0 2 22 184.08 17.50 0 -2 -22 193.68 16.70 0 -2 22 205.08 17.90 0 2 -22 197.58 16.20 0 2 22 240.38 18.40 0 2 -22 269.37 23.70 0 2 22 206.48 15.90 0 -2 22 210.28 16.20 1 -2 22 5.60 8.00 -1 -2 -22 2.50 3.50 1 -2 22 11.50 5.50 -1 2 22 7.30 5.70 -1 -2 -22 4.50 5.50 1 -2 22 1.20 4.00 1 2 -22 8.60 4.50 -1 2 22 7.00 3.40 -1 -2 22 2.00 2.80 -1 -2 22 -0.20 3.50 1 -2 -22 4.00 4.20 1 2 22 -0.60 2.80 1 2 22 -1.50 3.30 -1 2 -22 6.20 6.70 1 2 22 5.00 3.20 1 2 22 3.90 5.70 0 -3 -22 17.10 3.70 0 3 22 11.80 6.00 0 3 22 11.20 3.30 0 -3 -22 7.90 3.80 0 3 -22 9.50 6.60 0 -3 22 16.00 5.40 0 -3 22 19.80 4.60 0 3 -22 15.60 4.00 0 -3 22 14.30 2.90 0 3 22 13.90 4.60 -1 -3 -22 43.90 9.00 1 3 -22 60.79 7.10 1 -3 22 49.30 6.60 -1 3 22 52.99 6.80 -1 3 22 41.80 6.70 1 -3 22 54.19 6.10 1 3 22 52.59 6.30 -1 3 -22 79.19 13.00 1 -3 -22 83.39 8.40 1 3 22 52.49 7.20 1 3 22 53.39 7.20 1 3 22 50.59 9.20 -1 -3 22 59.79 7.90 -1 -3 22 33.90 6.00 0 -4 -22 12.70 2.90 0 4 22 9.30 6.60 0 4 -22 19.90 4.40 0 4 22 14.30 3.50 0 -4 22 16.00 4.40 0 4 -22 13.90 7.60 0 4 -22 24.70 6.50 0 -4 -22 18.70 4.70 0 4 22 13.80 4.70 1 -4 22 0.70 2.40 1 -4 22 -0.60 2.50 -1 -4 -22 -0.40 3.50 -1 4 22 1.10 3.20 1 4 -22 -1.30 2.90 -1 -4 22 -0.50 3.00 1 4 22 -0.70 3.20 1 4 22 0.80 2.50 -1 -4 22 3.20 2.50 1 -4 -22 1.20 2.30 -1 4 -22 1.90 5.60 1 4 22 1.80 4.00 0 -5 -22 7.00 3.60 0 5 22 9.60 4.00 0 5 -22 2.90 4.10 0 5 -22 5.50 4.80 0 -5 -22 7.20 1.70 0 5 -22 9.40 2.20 0 -5 22 7.00 3.30 0 0 -23 -0.50 1.40 0 0 23 0.40 5.60 0 0 23 1.10 4.30 0 -1 -23 259.87 21.10 0 1 23 272.37 19.20 0 -1 -23 205.98 16.80 0 1 -23 245.78 21.50 0 2 23 8.90 3.40 0 2 -23 3.40 4.80 0 -2 -23 4.60 1.90 0 -2 -23 9.40 5.30 0 -2 23 -2.70 3.00 0 2 -23 6.90 2.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 88006 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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2502(5) 0.18157(15) 0.79789(10) 0.0401(5) Uani 1 1 d . . . . . H1A H 0.4142 0.2060 0.8144 0.048 Uiso 1 1 calc R U . . . H1B H 0.1358 0.1482 0.8297 0.048 Uiso 1 1 calc R U . . . C2 C 0.1812(4) 0.19401(12) 0.73079(9) 0.0251(4) Uani 1 1 d . . . . . H2A H 0.0156 0.1685 0.7164 0.030 Uiso 1 1 calc R U . . . C3 C 0.3429(3) 0.24510(12) 0.67558(9) 0.0209(4) Uani 1 1 d . . . . . H3A H 0.4101 0.1958 0.6414 0.025 Uiso 1 1 calc R U . . . H3B H 0.4964 0.2761 0.6989 0.025 Uiso 1 1 calc R U . . . C4 C 0.1882(3) 0.32454(12) 0.63435(8) 0.0172(3) Uani 1 1 d . . . . . C5 C 0.3713(3) 0.37722(12) 0.58129(8) 0.0171(3) Uani 1 1 d . . . . . H5 H 0.5072 0.4140 0.6090 0.021 Uiso 1 1 calc R U . . . C6 C 0.2331(3) 0.44974(12) 0.53098(9) 0.0215(4) Uani 1 1 d . . . . . H6A H 0.1244 0.4130 0.4963 0.026 Uiso 1 1 calc R U . . . H6B H 0.1154 0.4931 0.5588 0.026 Uiso 1 1 calc R U . . . C7 C 0.4334(3) 0.51122(12) 0.49169(9) 0.0215(4) Uani 1 1 d . . . . . C8 C 0.5267(4) 0.48432(13) 0.42478(9) 0.0263(4) Uani 1 1 d . . . . . H8 H 0.4529 0.4290 0.4013 0.032 Uiso 1 1 calc R U . . . C9 C 0.7263(4) 0.53715(14) 0.39191(10) 0.0322(4) Uani 1 1 d . . . . . H9 H 0.7889 0.5175 0.3464 0.039 Uiso 1 1 calc R U . . . C10 C 0.8346(4) 0.61877(14) 0.42531(10) 0.0327(5) Uani 1 1 d . . . . . H10 H 0.9719 0.6547 0.4030 0.039 Uiso 1 1 calc R U . . . C11 C 0.7407(4) 0.64739(13) 0.49162(11) 0.0318(4) Uani 1 1 d . . . . . H11 H 0.8126 0.7034 0.5147 0.038 Uiso 1 1 calc R U . . . C12 C 0.5417(4) 0.59393(13) 0.52400(9) 0.0265(4) Uani 1 1 d . . . . . H12 H 0.4778 0.6142 0.5692 0.032 Uiso 1 1 calc R U . . . C13 C 0.0536(3) 0.39705(13) 0.68542(8) 0.0204(4) Uani 1 1 d . . . . . H13A H -0.0540 0.4433 0.6570 0.024 Uiso 1 1 calc R U . . . H13B H -0.0674 0.3599 0.7167 0.024 Uiso 1 1 calc R U . . . C14 C 0.2419(4) 0.45631(14) 0.73207(10) 0.0292(4) Uani 1 1 d . . . . . H14A H 0.3532 0.4114 0.7595 0.044 Uiso 1 1 calc R U . . . H14B H 0.1406 0.4977 0.7648 0.044 Uiso 1 1 calc R U . . . H14C H 0.3527 0.4979 0.7019 0.044 Uiso 1 1 calc R U . . . O1 O -0.0206(2) 0.27610(8) 0.59641(6) 0.0188(3) Uani 1 1 d . . . . . H1 H 0.0417 0.2466 0.5609 0.028 Uiso 1 1 calc R U . . . O2 O 0.5028(2) 0.30630(8) 0.53760(6) 0.0200(3) Uani 1 1 d . . . . . H2 H 0.6532 0.2952 0.5543 0.030 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 C1 0.0568(14) 0.0353(10) 0.0282(9) 0.0065(8) -0.0033(10) -0.0085(11) C2 0.0274(9) 0.0219(8) 0.0259(9) 0.0012(7) -0.0007(7) -0.0019(7) C3 0.0169(8) 0.0212(8) 0.0247(8) 0.0013(6) -0.0035(7) -0.0007(7) C4 0.0116(7) 0.0206(8) 0.0195(7) -0.0017(6) -0.0022(6) -0.0004(6) C5 0.0121(8) 0.0201(8) 0.0193(7) -0.0025(6) -0.0011(6) 0.0020(6) C6 0.0159(8) 0.0244(8) 0.0244(8) 0.0030(7) -0.0011(7) 0.0022(7) C7 0.0179(8) 0.0214(8) 0.0252(8) 0.0044(7) -0.0025(7) 0.0038(6) C8 0.0278(10) 0.0266(9) 0.0244(8) 0.0021(7) -0.0018(8) -0.0009(8) C9 0.0334(11) 0.0362(10) 0.0271(9) 0.0070(8) 0.0050(8) -0.0003(9) C10 0.0249(10) 0.0333(10) 0.0400(11) 0.0168(8) 0.0008(8) -0.0042(8) C11 0.0304(10) 0.0232(8) 0.0418(10) 0.0038(8) -0.0062(9) -0.0043(8) C12 0.0275(10) 0.0239(8) 0.0282(9) 0.0006(7) -0.0019(8) 0.0022(8) C13 0.0177(8) 0.0224(8) 0.0210(7) -0.0023(6) 0.0012(6) 0.0000(7) C14 0.0282(10) 0.0316(9) 0.0278(9) -0.0104(8) 0.0007(8) -0.0038(8) O1 0.0124(5) 0.0238(6) 0.0203(5) -0.0047(4) -0.0013(5) -0.0002(5) O2 0.0143(6) 0.0249(6) 0.0208(5) -0.0026(4) -0.0004(4) 0.0044(5) 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 C2 C1 H1A 120.0 . . ? C2 C1 H1B 120.0 . . ? H1A C1 H1B 120.0 . . ? C1 C2 C3 125.16(19) . . ? C1 C2 H2A 117.4 . . ? C3 C2 H2A 117.4 . . ? C2 C3 C4 113.15(14) . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.8 . . ? O1 C4 C13 105.94(12) . . ? O1 C4 C5 109.81(12) . . ? C13 C4 C5 111.94(13) . . ? O1 C4 C3 107.64(12) . . ? C13 C4 C3 111.32(13) . . ? C5 C4 C3 110.02(13) . . ? O2 C5 C6 107.12(12) . . ? O2 C5 C4 109.79(13) . . ? C6 C5 C4 114.87(13) . . ? O2 C5 H5 108.3 . . ? C6 C5 H5 108.3 . . ? C4 C5 H5 108.3 . . ? C7 C6 C5 110.38(14) . . ? C7 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? C7 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 118.12(17) . . ? C8 C7 C6 121.65(16) . . ? C12 C7 C6 120.11(16) . . ? C9 C8 C7 120.94(17) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 120.20(17) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 119.51(18) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C12 C11 C10 119.77(18) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C7 121.44(17) . . ? C11 C12 H12 119.3 . . ? C7 C12 H12 119.3 . . ? C14 C13 C4 114.69(14) . . ? C14 C13 H13A 108.6 . . ? C4 C13 H13A 108.6 . . ? C14 C13 H13B 108.6 . . ? C4 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 O1 H1 109.5 . . ? C5 O2 H2 109.5 . . ? 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 C1 C2 1.319(3) . ? C1 H1A 0.9500 . ? C1 H1B 0.9500 . ? C2 C3 1.495(2) . ? C2 H2A 0.9500 . ? C3 C4 1.546(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 O1 1.4390(19) . ? C4 C13 1.538(2) . ? C4 C5 1.541(2) . ? C5 O2 1.4330(19) . ? C5 C6 1.537(2) . ? C5 H5 1.0000 . ? C6 C7 1.511(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.392(2) . ? C7 C12 1.393(2) . ? C8 C9 1.389(3) . ? C8 H8 0.9500 . ? C9 C10 1.390(3) . ? C9 H9 0.9500 . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.529(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O1 H1 0.8400 . ? O2 H2 0.8400 . ?