#------------------------------------------------------------------------------ #$Date: 2021-09-03 02:03:11 +0300 (Fri, 03 Sep 2021) $ #$Revision: 268372 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/81/7708165.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_7708165 loop_ _publ_author_name 'Matos, Cati\'ucia R. M. O.' 'Sarmiento, Charlie V.' 'C. Silva, Henrique' 'Ferreira, Glaucio B.' 'Guedes, Guilherme P.' 'Nunes, Wallace C.' 'Ronconi, C\'elia M.' _publ_section_title ; Field-induced single-ion magnets exhibiting tri-axial anisotropy in a 1D Co(ii) coordination polymer with a rigid ligand 4,4′-(buta-1,3-diyne-1,4-diyl)dibenzoate ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01961A _journal_year 2021 _chemical_formula_moiety 'C20 H14 O4' _chemical_formula_sum 'C20 H14 O4' _chemical_formula_weight 318.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary difmap _audit_creation_date 2021-04-11 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-04-13 deposited with the CCDC. 2021-08-16 downloaded from the CCDC. ; _cell_angle_alpha 75.773(3) _cell_angle_beta 73.159(2) _cell_angle_gamma 74.351(3) _cell_formula_units_Z 2 _cell_length_a 7.0604(4) _cell_length_b 10.6647(7) _cell_length_c 11.8334(7) _cell_measurement_reflns_used 9273 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 25.62 _cell_measurement_theta_min 2.46 _cell_volume 807.50(9) _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_collection 'Bruker Instrument Service vV6.2.6' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker D8-Venture' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_unetI/netI 0.0227 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _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 23446 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.024 _diffrn_reflns_theta_max 25.024 _diffrn_reflns_theta_min 2.464 _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6919 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.309 _exptl_crystal_description neddle _exptl_crystal_F_000 332 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.254 _exptl_crystal_size_min 0.164 _refine_diff_density_max 0.189 _refine_diff_density_min -0.199 _refine_diff_density_rms 0.041 _refine_ls_extinction_coef 0.127(18) _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 1.112 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 2839 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.112 _refine_ls_R_factor_all 0.0735 _refine_ls_R_factor_gt 0.0553 _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^)+(0.0565P)^2^+0.5678P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1416 _refine_ls_wR_factor_ref 0.1583 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2208 _reflns_number_total 2853 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01961a2.cif _cod_data_source_block 4 _cod_database_code 7708165 _shelx_shelxl_version_number 2014/7 _publcif_funding_html ; ; _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 0.985 _shelx_estimated_absorpt_t_min 0.975 _olex2_refinement_description ; 1.a Aromatic/amide H refined with riding coordinates: C4(H4), C5(H5), C12(H12), C13(H13), C17(H17), C18(H18), C19(H19), C20(H20) 1.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C16(H16A,H16B,H16C) ; _shelx_res_file ; mo_l1es_celia_0m.res created by SHELXL-2014/7 TITL mo_L1Es_Celia_0m_a.res in P-1 CELL 0.71073 7.0604 10.6647 11.8334 75.773 73.159 74.351 ZERR 2 0.0004 0.0007 0.0007 0.003 0.002 0.003 LATT 1 SFAC C H O UNIT 40 28 8 L.S. 50 PLAN 5 SIZE 0.164 0.254 0.28 TEMP 25(2) CONF BOND $H fmap 2 acta MORE -1 MERG 2 OMIT 3 8 3 REM REM REM WGHT 0.056500 0.567800 EXTI 0.127453 FVAR 1.84405 O1 3 1.598479 0.102124 0.310458 11.00000 0.03774 0.06176 = 0.06181 -0.03081 -0.01171 0.00011 O2 3 -0.465901 0.839095 1.167800 11.00000 0.04157 0.05857 = 0.05141 -0.01948 -0.00457 0.00106 O3 3 -0.591202 0.853796 1.011701 11.00000 0.04390 0.09793 = 0.07788 -0.03147 -0.02331 0.00469 O4 3 1.773378 0.153463 0.414055 11.00000 0.03468 0.11069 = 0.09295 -0.05487 -0.01925 -0.00213 C1 1 1.784909 0.033939 0.240865 11.00000 0.04343 0.05547 = 0.06211 -0.02623 -0.00580 0.00166 AFIX 137 H1A 2 1.884284 0.087539 0.217393 11.00000 -1.50000 H1B 2 1.760413 0.017946 0.170494 11.00000 -1.50000 H1C 2 1.833845 -0.048952 0.288487 11.00000 -1.50000 AFIX 0 C2 1 1.614473 0.157477 0.395349 11.00000 0.03933 0.04155 = 0.04439 -0.01006 -0.01371 -0.00657 C3 1 1.414438 0.223323 0.462398 11.00000 0.03572 0.03944 = 0.03787 -0.00759 -0.01236 -0.00446 C4 1 1.234160 0.206776 0.450521 11.00000 0.03791 0.05163 = 0.04534 -0.01874 -0.01163 -0.00808 AFIX 43 H4 2 1.235751 0.154530 0.397706 11.00000 -1.20000 AFIX 0 C5 1 1.052104 0.267238 0.516476 11.00000 0.03173 0.05797 = 0.04888 -0.01573 -0.01042 -0.01058 AFIX 43 H5 2 0.931485 0.255510 0.507908 11.00000 -1.20000 AFIX 0 C6 1 1.047165 0.345977 0.596078 11.00000 0.03508 0.04248 = 0.03563 -0.00511 -0.00720 -0.00349 C7 1 0.856306 0.406899 0.664150 11.00000 0.04300 0.04162 = 0.04050 -0.00643 -0.00860 -0.00739 C8 1 0.690985 0.455424 0.718188 11.00000 0.04442 0.04256 = 0.04204 -0.00729 -0.00559 -0.00819 C9 1 0.502470 0.512587 0.777929 11.00000 0.04596 0.04146 = 0.04335 -0.00844 -0.00491 -0.00942 C10 1 0.335172 0.563096 0.828567 11.00000 0.04673 0.03852 = 0.04470 -0.00664 -0.00398 -0.01070 C11 1 0.137606 0.625541 0.887385 11.00000 0.03844 0.03598 = 0.04258 -0.00769 -0.00118 -0.00830 C12 1 -0.027078 0.647851 0.837734 11.00000 0.05262 0.05028 = 0.04452 -0.01966 -0.01007 -0.00711 AFIX 43 H12 2 -0.009272 0.620772 0.765711 11.00000 -1.20000 AFIX 0 C13 1 -0.216485 0.709805 0.894505 11.00000 0.04398 0.04937 = 0.05163 -0.01234 -0.01845 -0.00687 AFIX 43 H13 2 -0.325755 0.724410 0.860552 11.00000 -1.20000 AFIX 0 C14 1 -0.245141 0.750532 1.002043 11.00000 0.03850 0.03591 = 0.04105 -0.00528 -0.00882 -0.00760 C15 1 -0.451652 0.819094 1.058509 11.00000 0.03955 0.04032 = 0.05100 -0.00617 -0.00929 -0.00982 C16 1 -0.660100 0.908984 1.226621 11.00000 0.04789 0.06224 = 0.06495 -0.01934 0.00226 0.00177 AFIX 137 H16A 2 -0.690335 0.996812 1.181354 11.00000 -1.50000 H16B 2 -0.656995 0.914014 1.305937 11.00000 -1.50000 H16C 2 -0.762529 0.862752 1.231813 11.00000 -1.50000 AFIX 0 C17 1 0.108598 0.666330 0.995337 11.00000 0.03644 0.05399 = 0.04810 -0.01176 -0.01131 -0.00720 AFIX 43 H17 2 0.217515 0.651578 1.029626 11.00000 -1.20000 AFIX 0 C18 1 -0.081862 0.728756 1.051723 11.00000 0.04323 0.05146 = 0.04001 -0.01515 -0.00739 -0.00918 AFIX 43 H18 2 -0.100205 0.756285 1.123604 11.00000 -1.20000 AFIX 0 C19 1 1.410128 0.302742 0.540705 11.00000 0.03583 0.05445 = 0.05256 -0.01637 -0.01703 -0.00833 AFIX 43 H19 2 1.530911 0.314874 0.548664 11.00000 -1.20000 AFIX 0 C20 1 1.228429 0.363525 0.606515 11.00000 0.04640 0.05047 = 0.04550 -0.01959 -0.01294 -0.00539 AFIX 43 H20 2 1.227253 0.416770 0.658375 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_L1Es_Celia_0m_a.res in P-1 REM R1 = 0.0553 for 2210 Fo > 4sig(Fo) and 0.0735 for all 2839 data REM 220 parameters refined using 0 restraints END WGHT 0.0563 0.5705 REM Highest difference peak 0.189, deepest hole -0.199, 1-sigma level 0.041 Q1 1 0.8123 0.4835 0.7046 11.00000 0.05 0.19 Q2 1 -0.7385 0.8332 1.3060 11.00000 0.05 0.19 Q3 1 -0.7435 0.9467 1.1602 11.00000 0.05 0.17 Q4 1 1.9616 0.0835 0.3544 11.00000 0.05 0.17 Q5 1 -0.1860 0.6983 1.0429 11.00000 0.05 0.17 ; _shelx_res_checksum 59382 _shelx_hkl_file ; -1 0 0 1919.21 61.69 -1 0 0 2034.50 61.69 -1 0 0 1732.83 62.19 -1 0 0 1894.11 61.69 1 0 0 1955.40 61.09 1 0 0 1909.91 61.69 1 0 0 1964.90 61.69 -2 0 0 12.50 2.90 -2 0 0 12.00 2.90 -2 0 0 9.20 3.10 -2 0 0 11.70 3.10 -2 0 0 13.30 2.20 2 0 0 13.70 3.30 2 0 0 11.80 2.90 2 0 0 19.60 2.90 2 0 0 14.40 3.00 -3 0 0 247.58 12.70 -3 0 0 225.98 12.60 -3 0 0 252.27 12.20 -3 0 0 256.47 10.60 -3 0 0 253.27 13.00 -3 0 0 255.07 12.60 3 0 0 249.68 12.00 3 0 0 247.98 12.50 3 0 0 243.28 10.70 3 0 0 233.18 12.50 -4 0 0 27.30 5.00 -4 0 0 23.60 5.60 -4 0 0 30.30 5.50 -4 0 0 39.60 5.30 -4 0 0 30.40 6.10 -4 0 0 30.70 6.00 4 0 0 21.70 5.70 4 0 0 27.00 5.80 4 0 0 24.00 5.20 4 0 0 35.10 4.70 -5 0 0 525.25 20.20 -5 0 0 482.75 24.30 -5 0 0 511.65 23.60 -5 0 0 508.05 24.60 -5 0 0 496.55 24.20 -5 0 0 491.05 23.70 5 0 0 501.25 23.50 5 0 0 492.05 24.20 5 0 0 515.45 23.80 5 0 0 490.35 20.40 -6 0 0 503.15 26.30 -6 0 0 484.55 26.50 -6 0 0 534.75 29.60 -6 0 0 470.55 26.00 -6 0 0 501.55 27.80 6 0 0 509.65 25.80 6 0 0 489.45 25.40 6 0 0 501.15 21.10 6 0 0 515.35 25.70 6 0 0 511.95 32.60 -7 0 0 75.39 12.60 -7 0 0 52.99 10.40 -7 0 0 51.49 10.80 -7 0 0 37.30 9.60 -7 0 0 50.79 10.20 7 0 0 57.59 8.30 7 0 0 55.89 9.60 7 0 0 102.49 21.10 7 0 0 59.59 11.90 7 0 0 44.30 10.00 7 -1 0 35.40 6.00 7 -1 0 25.50 8.20 7 -1 0 20.40 9.60 7 -1 0 27.90 9.00 -7 1 0 21.80 8.70 -7 1 0 32.60 10.00 -7 1 0 23.50 7.80 -7 1 0 27.90 9.00 -7 1 0 30.90 10.10 6 -1 0 51.59 9.00 6 -1 0 55.89 9.10 6 -1 0 69.09 8.00 6 -1 0 61.29 9.80 -6 1 0 57.19 10.20 -6 1 0 60.89 9.90 -6 1 0 62.19 9.60 -6 1 0 45.10 9.00 -6 1 0 49.60 9.90 5 -1 0 4618.54 152.48 5 -1 0 4575.34 151.68 5 -1 0 4698.03 152.58 5 -1 0 4479.15 149.29 5 -1 0 4618.24 151.68 -5 1 0 4579.14 152.38 -5 1 0 4357.56 152.68 -5 1 0 4552.44 151.68 -5 1 0 4740.23 152.08 -5 1 0 4640.84 151.98 4 -1 0 2.10 3.80 4 -1 0 9.10 4.80 4 -1 0 4.80 3.80 4 -1 0 9.20 3.00 4 -1 0 10.00 4.80 -4 1 0 13.00 4.50 -4 1 0 6.70 4.50 -4 1 0 9.60 3.40 -4 1 0 5.80 5.00 -4 1 0 5.60 3.80 -4 1 0 14.70 4.90 3 -1 0 1.70 2.90 3 -1 0 -1.90 2.90 3 -1 0 1.60 2.20 3 -1 0 -3.60 3.50 3 -1 0 -5.60 2.70 -3 1 0 -1.70 3.00 -3 1 0 4.10 2.90 -3 1 0 -0.70 3.10 -3 1 0 -2.80 3.40 -3 1 0 0.20 0.50 -3 1 0 -6.00 3.30 2 -1 0 49.60 5.20 2 -1 0 50.89 5.00 2 -1 0 53.49 4.30 2 -1 0 55.29 5.00 2 -1 0 51.99 5.20 -2 1 0 57.69 4.30 -2 1 0 47.20 5.10 -2 1 0 50.29 4.80 -2 1 0 47.10 5.50 -2 1 0 54.59 5.30 1 -1 0 3248.58 106.99 -1 1 0 3262.57 106.99 -1 1 0 3559.64 107.39 -2 -1 0 1124.29 36.90 -2 -1 0 1096.59 37.20 -2 -1 0 1120.29 37.50 -2 -1 0 1105.69 37.50 -2 -1 0 959.50 36.20 2 1 0 1087.19 37.30 2 1 0 1059.49 35.60 2 1 0 1090.89 37.20 2 1 0 1071.69 36.80 2 1 0 1112.59 39.50 -3 -1 0 8.20 2.70 -3 -1 0 14.00 3.50 -3 -1 0 7.60 4.20 -3 -1 0 12.70 4.00 3 1 0 10.10 4.10 3 1 0 9.80 3.30 3 1 0 5.00 4.70 3 1 0 9.80 3.70 -4 -1 0 4.90 3.70 -4 -1 0 5.70 4.90 -4 -1 0 1.10 4.60 -4 -1 0 9.20 2.80 -4 -1 0 -1.10 3.30 4 1 0 0.20 5.10 4 1 0 14.40 5.30 4 1 0 6.20 2.20 4 1 0 4.00 3.70 4 1 0 6.90 4.70 -5 -1 0 442.36 17.50 -5 -1 0 435.96 23.60 -5 -1 0 452.15 22.60 -5 -1 0 404.16 21.70 -5 -1 0 432.66 22.60 -5 -1 0 432.96 21.40 5 1 0 394.96 21.00 5 1 0 440.56 21.60 5 1 0 453.35 17.70 -6 -1 0 561.14 28.30 -6 -1 0 568.04 28.40 -6 -1 0 538.15 27.70 -6 -1 0 513.05 21.60 6 1 0 569.64 27.90 6 1 0 539.75 27.40 6 1 0 546.55 21.50 6 1 0 504.55 26.40 6 1 0 533.75 32.90 -7 -1 0 120.29 17.00 -7 -1 0 118.19 13.90 -7 -1 0 149.19 19.30 -7 -1 0 136.09 14.90 7 1 0 126.69 15.90 7 1 0 134.79 9.00 7 1 0 140.39 27.90 7 1 0 121.79 16.10 7 1 0 151.48 15.40 7 -2 0 97.09 11.40 7 -2 0 100.79 16.10 7 -2 0 104.79 15.10 7 -2 0 118.09 16.10 -7 2 0 101.99 15.90 -7 2 0 114.89 17.80 -7 2 0 103.19 14.10 -7 2 0 75.49 12.10 6 -2 0 50.89 7.30 6 -2 0 61.79 10.20 6 -2 0 52.89 8.70 6 -2 0 60.79 10.30 6 -2 0 79.49 13.50 -6 2 0 57.49 9.80 -6 2 0 62.09 10.20 -6 2 0 69.59 10.50 5 -2 0 829.62 33.50 5 -2 0 824.62 35.50 5 -2 0 909.71 35.70 5 -2 0 908.41 35.70 -5 2 0 873.51 35.50 -5 2 0 860.91 36.60 -5 2 0 838.22 36.10 -5 2 0 917.61 36.10 -5 2 0 866.11 35.50 4 -2 0 25.20 4.40 4 -2 0 25.00 5.60 4 -2 0 25.50 5.70 4 -2 0 22.70 5.50 4 -2 0 21.90 5.30 -4 2 0 30.90 5.20 -4 2 0 23.80 2.30 -4 2 0 26.20 6.00 -4 2 0 31.30 6.00 -4 2 0 22.50 5.30 -4 2 0 32.60 6.10 3 -2 0 14.90 4.00 3 -2 0 16.40 3.40 3 -2 0 16.50 3.80 3 -2 0 10.30 4.00 3 -2 0 19.30 4.20 -3 2 0 17.50 4.90 -3 2 0 14.90 4.60 -3 2 0 20.30 3.90 -3 2 0 20.90 4.40 2 -2 0 218.58 9.90 2 -2 0 216.18 10.40 2 -2 0 237.38 10.40 2 -2 0 216.18 10.30 2 -2 0 206.98 10.40 -2 2 0 211.88 10.50 -2 2 0 220.88 10.70 -2 2 0 218.78 10.60 -2 2 0 232.38 10.30 1 -2 0 4361.46 140.19 -1 2 0 4436.16 140.29 -1 -2 0 286.97 13.40 -1 -2 0 307.57 11.80 -1 -2 0 260.37 11.60 -1 -2 0 315.57 12.40 1 2 0 286.17 13.00 1 2 0 311.07 12.10 1 2 0 302.17 11.00 1 2 0 293.47 11.30 1 2 0 307.97 12.00 -2 -2 0 4737.43 152.58 -2 -2 0 4835.72 150.28 -2 -2 0 4608.04 150.48 -2 -2 0 4743.53 149.69 2 2 0 4529.05 150.08 2 2 0 4773.32 152.48 2 2 0 4589.24 149.79 2 2 0 4625.24 150.38 -3 -2 0 161.38 7.80 -3 -2 0 141.09 10.40 -3 -2 0 149.09 9.00 -3 -2 0 156.78 9.50 3 2 0 144.09 11.20 3 2 0 144.99 10.30 3 2 0 153.28 8.40 3 2 0 158.18 9.70 3 2 0 150.48 9.50 -4 -2 0 130.99 9.50 -4 -2 0 116.19 11.40 -4 -2 0 126.19 7.40 -4 -2 0 119.59 9.60 -4 -2 0 121.69 9.70 4 2 0 128.89 9.20 4 2 0 123.29 8.60 4 2 0 103.49 9.60 4 2 0 116.09 6.10 4 2 0 111.99 11.20 4 2 0 106.49 12.30 -5 -2 0 3.90 5.30 -5 -2 0 15.90 6.90 -5 -2 0 17.30 5.70 -5 -2 0 12.80 6.70 5 2 0 17.40 6.90 5 2 0 10.50 5.20 5 2 0 8.90 4.30 -6 -2 0 4390.16 158.88 -6 -2 0 4939.11 159.78 -6 -2 0 4547.25 152.18 -6 -2 0 4900.01 159.58 6 2 0 4816.02 173.98 6 2 0 4841.42 158.68 6 2 0 4675.63 157.98 6 2 0 4777.12 157.38 -7 -2 0 41.80 5.90 -7 -2 0 62.09 12.10 -7 -2 0 40.50 9.70 -7 -2 0 50.09 10.40 7 2 0 74.49 17.20 7 2 0 58.99 10.30 7 2 0 56.29 10.30 7 2 0 46.40 10.20 7 2 0 52.89 11.00 -8 -2 0 34.80 12.30 -8 -2 0 39.80 11.90 -8 -2 0 36.60 13.30 8 2 0 46.70 10.80 8 2 0 59.09 12.00 8 2 0 61.49 11.30 8 2 0 25.70 9.20 7 -3 0 36.90 9.40 7 -3 0 12.30 8.40 7 -3 0 23.00 7.60 7 -3 0 50.79 10.90 7 -3 0 24.60 9.30 -7 3 0 34.80 10.80 -7 3 0 40.00 10.30 6 -3 0 22.20 8.00 6 -3 0 12.90 7.60 6 -3 0 16.90 5.90 6 -3 0 21.60 8.20 -6 3 0 16.40 6.90 -6 3 0 22.10 8.40 -6 3 0 13.00 8.40 5 -3 0 -6.60 6.00 5 -3 0 7.60 6.10 5 -3 0 6.40 6.00 5 -3 0 0.00 5.20 -5 3 0 -6.80 6.10 -5 3 0 -6.40 5.90 -5 3 0 -3.00 5.20 -5 3 0 2.70 5.70 4 -3 0 -2.00 3.80 4 -3 0 3.10 3.70 4 -3 0 -1.80 4.30 4 -3 0 1.30 4.70 4 -3 0 -4.90 3.70 -4 3 0 0.20 2.30 -4 3 0 -7.10 4.30 -4 3 0 4.30 4.60 -4 3 0 3.10 4.50 3 -3 0 264.87 13.80 3 -3 0 273.27 14.20 3 -3 0 297.67 13.60 3 -3 0 274.37 13.30 3 -3 0 280.67 14.00 -3 3 0 280.77 13.40 -3 3 0 276.57 13.90 -3 3 0 264.77 14.20 -3 3 0 254.47 13.80 2 -3 0 143.19 9.10 2 -3 0 141.79 8.40 2 -3 0 155.78 8.70 2 -3 0 153.48 8.90 2 -3 0 150.18 8.70 -2 3 0 135.39 8.30 -2 3 0 152.18 9.10 -2 3 0 157.48 8.90 -2 3 0 146.09 8.80 1 -3 0 44.70 1.90 1 -3 0 41.50 4.40 1 -3 0 44.30 4.80 -1 3 0 43.60 3.60 -1 3 0 42.00 4.40 -1 3 0 46.30 4.80 -1 3 0 45.10 4.10 0 -3 0 603.44 21.90 0 -3 0 633.64 21.80 0 -3 0 617.74 23.00 0 3 0 583.54 21.70 0 3 0 597.04 21.70 0 3 0 662.93 21.40 -2 -3 0 1240.48 42.30 -2 -3 0 1248.68 42.10 -2 -3 0 1257.77 43.10 -2 -3 0 1271.17 43.70 -2 -3 0 1225.68 45.60 2 3 0 1291.17 45.40 2 3 0 1284.67 43.40 2 3 0 1236.08 41.90 2 3 0 1233.18 42.60 2 3 0 1283.17 43.70 -3 -3 0 1436.06 48.40 -3 -3 0 1445.56 49.10 -3 -3 0 1415.26 52.79 -3 -3 0 1403.66 46.90 -3 -3 0 1395.26 49.80 3 3 0 1366.86 51.99 3 3 0 1400.36 47.60 3 3 0 1384.76 49.10 3 3 0 1411.46 48.70 3 3 0 1396.16 49.70 -4 -3 0 192.18 13.50 -4 -3 0 178.68 11.60 -4 -3 0 178.28 11.10 -4 -3 0 196.88 12.40 -4 -3 0 182.78 9.40 4 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-12 45.50 12.60 -1 -6 -12 34.80 7.00 -1 -6 -12 29.00 10.00 -2 -6 -12 114.59 7.40 -2 -6 -12 134.19 18.20 -2 -6 -12 124.59 7.60 -2 -6 -12 98.69 11.50 -2 -6 -12 124.79 17.80 -2 -6 -12 117.39 15.20 2 6 12 117.99 14.60 -3 -6 -12 8.00 4.20 -3 -6 -12 4.90 4.90 -3 -6 -12 3.50 5.20 -3 -6 -12 9.70 11.60 -3 -6 -12 0.70 8.90 -3 -6 -12 11.60 3.40 3 6 12 2.60 3.90 -4 -6 -12 5.00 12.40 -4 -6 -12 1.30 4.30 -4 -6 -12 -8.90 7.10 -4 -6 -12 5.30 6.10 -4 -6 -12 -17.90 8.40 -4 -6 -12 0.10 5.30 4 6 12 -7.80 5.60 4 6 12 -1.50 6.20 4 6 12 -0.60 6.50 4 6 12 -13.00 9.60 -5 -6 -12 15.30 8.50 -5 -6 -12 -7.10 5.50 -5 -6 -12 4.80 8.90 -5 -6 -12 10.50 13.50 -5 -6 -12 -3.40 6.40 -5 -6 -12 0.10 9.00 5 6 12 3.60 6.50 5 6 12 7.80 7.70 5 6 12 -2.10 7.70 -6 -6 -12 51.59 18.40 -6 -6 -12 34.50 10.00 -6 -6 -12 45.20 11.60 -6 -6 -12 16.70 9.60 -6 -6 -12 23.30 8.40 -6 -6 -12 36.80 10.50 6 6 12 30.50 11.20 6 6 12 33.40 15.10 6 6 12 28.40 9.00 0 -7 -12 122.49 14.70 0 -7 -12 103.39 11.00 0 -7 -12 73.49 11.40 0 -7 -12 88.79 17.40 0 -7 -12 68.29 17.50 0 -7 -12 93.89 11.10 0 -7 -12 97.99 16.20 0 7 12 93.19 10.70 -1 -7 -12 -5.60 8.10 -1 -7 -12 3.40 6.40 -1 -7 -12 3.80 4.80 -1 -7 -12 19.80 5.80 -1 -7 -12 12.40 12.70 -1 -7 -12 1.60 7.60 -2 -7 -12 18.10 10.10 -2 -7 -12 28.70 4.30 -2 -7 -12 29.50 5.90 -2 -7 -12 46.20 9.80 -2 -7 -12 44.10 6.60 -2 -7 -12 35.40 5.40 -2 -7 -12 41.30 7.80 -2 -7 -12 59.79 14.00 -2 -7 -12 32.60 5.60 2 7 12 51.09 9.90 -3 -7 -12 243.58 15.00 -3 -7 -12 257.87 22.50 -3 -7 -12 221.58 11.50 -3 -7 -12 247.08 23.40 -3 -7 -12 202.78 18.00 -3 -7 -12 211.98 11.20 -3 -7 -12 244.08 16.20 3 7 12 198.78 11.70 3 7 12 226.58 10.70 -4 -7 -12 -9.60 12.30 -4 -7 -12 3.70 8.70 -4 -7 -12 -5.00 9.50 -4 -7 -12 -8.10 6.50 -4 -7 -12 0.40 4.30 -4 -7 -12 -7.60 4.30 4 7 12 -8.30 5.70 4 7 12 12.50 8.70 -5 -7 -12 9.70 9.80 -5 -7 -12 8.90 6.40 -5 -7 -12 15.00 11.00 -5 -7 -12 17.80 9.20 -5 -7 -12 24.20 6.10 5 7 12 1.60 7.70 5 7 12 27.30 9.20 5 7 12 10.50 7.20 5 7 12 6.70 13.00 -1 -8 -12 15.00 6.20 -1 -8 -12 12.10 3.90 -1 -8 -12 8.20 9.10 -1 -8 -12 12.10 10.20 -1 -8 -12 19.00 9.20 -2 -8 -12 -2.80 3.00 -2 -8 -12 4.20 3.50 -2 -8 -12 7.30 5.10 -2 -8 -12 -0.30 9.60 -2 -8 -12 6.70 4.20 -2 -8 -12 0.30 2.50 -2 -8 -12 11.20 14.20 -2 -8 -12 3.80 12.20 -2 -8 -12 4.00 7.40 2 8 12 -4.00 7.90 -3 -8 -12 3.90 12.00 -3 -8 -12 5.10 7.50 -3 -8 -12 13.70 9.70 -3 -8 -12 -4.50 5.90 -3 -8 -12 -0.10 3.00 3 8 12 3.00 3.40 3 8 12 -7.10 3.70 -4 -8 -12 3.00 4.70 -4 -8 -12 32.60 25.00 -4 -8 -12 -1.80 9.50 -4 -8 -12 14.30 4.00 4 8 12 5.90 6.70 4 8 12 -7.40 11.60 -5 -8 -12 38.20 12.40 -5 -8 -12 56.49 8.40 -5 -8 -12 63.39 17.80 -5 -8 -12 43.80 10.00 5 8 12 41.30 9.40 5 8 12 42.40 10.10 5 8 12 25.40 8.80 5 8 12 30.10 13.90 -3 -9 -12 0.60 13.20 -3 -9 -12 5.80 11.00 -3 -9 -12 10.60 6.40 3 9 12 12.30 4.10 3 9 12 7.50 8.00 0 1 -13 10.80 4.10 0 1 -13 7.40 6.00 0 1 -13 -0.60 7.30 0 -1 13 7.10 4.40 0 -1 13 24.10 11.70 -1 1 -13 -6.00 4.60 -1 1 -13 -12.80 7.70 1 -1 13 -1.10 9.50 -2 1 -13 -7.30 5.30 -2 1 -13 -7.10 8.00 2 -1 13 -1.50 9.10 2 -1 13 3.40 10.00 2 -1 13 11.70 7.00 2 -1 13 -2.50 6.90 -3 1 -13 9.50 6.90 -3 1 -13 7.70 9.40 3 -1 13 -5.60 9.60 3 -1 13 -5.50 7.80 3 -1 13 -13.10 9.60 3 -1 13 13.90 9.00 0 0 -13 125.89 11.00 0 0 -13 167.68 20.90 0 0 -13 132.59 15.30 0 0 13 117.59 6.30 0 0 13 140.49 19.00 -1 0 -13 0.40 6.40 -1 0 -13 -3.10 4.40 -1 0 -13 4.30 7.30 1 0 13 3.90 3.70 1 0 13 7.20 5.00 1 0 13 15.80 11.30 -2 0 -13 -1.50 6.50 -2 0 -13 -9.00 10.00 -2 0 -13 -5.50 5.10 2 0 13 -17.30 8.50 2 0 13 -12.40 9.60 -3 0 -13 17.70 13.40 -3 0 -13 1.50 6.50 -3 0 -13 -0.40 9.10 -3 0 -13 4.10 6.10 3 0 13 5.20 11.30 3 0 13 1.70 9.20 3 0 13 -13.40 8.10 3 0 13 -6.40 6.20 -4 0 -13 17.70 8.20 -4 0 -13 20.30 10.50 4 0 13 14.50 5.10 4 0 13 27.80 9.80 4 0 13 17.90 8.90 4 0 13 26.80 12.10 4 0 13 41.80 9.80 0 -1 -13 17.40 8.30 0 -1 -13 28.60 11.30 0 -1 -13 12.90 3.80 0 -1 -13 19.00 4.30 0 1 13 22.40 11.20 -1 -1 -13 11.70 6.80 -1 -1 -13 26.90 10.60 -1 -1 -13 11.90 4.40 -1 -1 -13 17.00 9.30 1 1 13 10.40 2.90 1 1 13 15.90 10.90 -2 -1 -13 -5.00 4.00 -2 -1 -13 -4.00 5.10 -2 -1 -13 2.10 8.80 -2 -1 -13 10.40 10.80 -2 -1 -13 -1.40 6.80 2 1 13 -6.10 9.20 2 1 13 10.60 5.60 -3 -1 -13 0.10 6.70 -3 -1 -13 -0.40 9.40 -3 -1 -13 17.80 10.00 3 1 13 -19.20 10.10 3 1 13 -1.70 5.80 3 1 13 1.30 8.40 3 1 13 11.50 10.20 -4 -1 -13 -6.10 8.30 -4 -1 -13 4.10 6.80 -4 -1 -13 12.60 10.80 4 1 13 13.40 6.00 4 1 13 -1.20 9.90 4 1 13 -4.00 6.90 4 1 13 0.80 9.30 4 1 13 -7.20 7.90 0 -2 -13 29.20 9.80 0 -2 -13 29.40 6.40 0 -2 -13 36.30 10.00 0 -2 -13 18.10 6.50 0 -2 -13 27.50 7.80 0 -2 -13 23.50 8.70 -1 -2 -13 60.89 12.50 -1 -2 -13 56.99 6.70 -1 -2 -13 45.30 7.10 -1 -2 -13 38.10 7.80 -1 -2 -13 42.10 8.00 -1 -2 -13 47.10 6.40 -1 -2 -13 32.10 9.30 1 2 13 55.99 12.60 -2 -2 -13 39.70 9.90 -2 -2 -13 15.90 9.50 -2 -2 -13 8.40 6.60 -2 -2 -13 14.70 4.50 2 2 13 13.30 7.50 2 2 13 7.50 3.10 2 2 13 12.40 4.60 2 2 13 23.50 9.90 -3 -2 -13 10.30 5.80 -3 -2 -13 15.70 5.90 -3 -2 -13 18.90 8.40 -3 -2 -13 10.70 7.30 -3 -2 -13 7.90 9.90 3 2 13 10.10 8.40 3 2 13 20.30 9.20 3 2 13 20.70 6.60 -4 -2 -13 10.60 9.80 -4 -2 -13 4.40 6.70 -4 -2 -13 14.80 10.80 -4 -2 -13 -9.20 6.10 -4 -2 -13 -7.20 7.20 4 2 13 -5.90 8.80 4 2 13 9.40 7.90 4 2 13 8.20 8.00 4 2 13 -1.60 6.40 4 2 13 -2.00 6.50 4 2 13 -0.20 10.10 -5 -2 -13 118.99 16.20 -5 -2 -13 76.49 15.10 -5 -2 -13 65.99 11.70 -5 -2 -13 122.49 16.70 -5 -2 -13 61.49 13.30 5 2 13 133.39 18.90 5 2 13 105.79 17.50 5 2 13 68.89 15.50 5 2 13 125.19 15.20 5 2 13 105.49 17.00 0 -3 -13 22.00 9.90 0 -3 -13 15.20 8.30 0 -3 -13 4.20 8.70 0 -3 -13 4.20 8.00 0 -3 -13 9.70 7.40 0 -3 -13 14.40 8.30 0 -3 -13 29.20 7.30 -1 -3 -13 33.30 7.90 -1 -3 -13 44.10 10.70 -1 -3 -13 36.10 9.40 -1 -3 -13 38.70 7.40 -1 -3 -13 36.40 9.00 -2 -3 -13 44.30 8.30 -2 -3 -13 55.89 11.60 -2 -3 -13 51.89 11.70 -2 -3 -13 57.79 8.30 -2 -3 -13 39.70 6.90 -2 -3 -13 47.30 10.20 2 3 13 45.30 10.30 2 3 13 47.60 10.90 2 3 13 40.00 5.30 -3 -3 -13 -10.80 8.80 -3 -3 -13 -0.40 9.10 -3 -3 -13 6.20 9.60 -3 -3 -13 6.30 4.90 -3 -3 -13 9.40 5.30 -3 -3 -13 6.90 3.50 3 3 13 5.80 5.20 3 3 13 1.10 7.70 3 3 13 6.70 7.60 -4 -3 -13 4.50 7.60 -4 -3 -13 1.00 6.80 -4 -3 -13 17.20 6.60 -4 -3 -13 16.00 9.20 -4 -3 -13 24.50 11.10 4 3 13 9.20 7.80 4 3 13 17.40 8.10 4 3 13 25.80 8.10 4 3 13 7.70 6.20 4 3 13 7.00 8.80 -5 -3 -13 14.10 8.10 -5 -3 -13 10.50 7.70 -5 -3 -13 23.80 10.80 -5 -3 -13 -4.10 7.90 5 3 13 13.60 7.20 5 3 13 11.20 8.80 5 3 13 7.70 10.00 5 3 13 14.30 8.50 5 3 13 17.10 8.80 0 -4 -13 -2.50 6.10 0 -4 -13 0.60 7.60 0 -4 -13 0.40 8.70 0 -4 -13 13.70 10.30 0 -4 -13 18.30 9.60 0 -4 -13 6.60 8.30 -1 -4 -13 13.30 6.70 -1 -4 -13 9.30 9.00 -1 -4 -13 2.30 6.90 -1 -4 -13 -7.50 6.70 -1 -4 -13 12.20 8.80 -1 -4 -13 18.90 10.10 -2 -4 -13 -2.00 8.90 -2 -4 -13 7.60 9.30 -2 -4 -13 4.50 5.70 -2 -4 -13 -4.60 6.70 -2 -4 -13 -3.00 2.80 -2 -4 -13 10.90 6.40 -2 -4 -13 2.00 4.30 2 4 13 4.20 7.30 -3 -4 -13 0.60 9.50 -3 -4 -13 2.70 4.30 -3 -4 -13 10.70 4.80 -3 -4 -13 7.10 7.20 -3 -4 -13 1.00 4.50 -3 -4 -13 12.30 10.00 3 4 13 -5.70 8.10 3 4 13 0.50 4.70 3 4 13 1.30 3.20 3 4 13 -2.50 7.20 -4 -4 -13 -4.50 6.20 -4 -4 -13 1.20 3.40 -4 -4 -13 -0.90 9.80 -4 -4 -13 0.60 7.70 -4 -4 -13 19.90 12.50 -4 -4 -13 -5.80 5.60 4 4 13 -4.20 8.70 4 4 13 15.20 8.10 4 4 13 -0.10 5.00 4 4 13 7.20 6.10 -5 -4 -13 3.80 10.90 -5 -4 -13 7.70 7.40 -5 -4 -13 12.00 8.10 -5 -4 -13 10.60 7.80 -5 -4 -13 9.00 10.50 -5 -4 -13 2.90 2.50 5 4 13 3.60 7.80 5 4 13 1.40 7.80 5 4 13 4.00 11.20 5 4 13 13.30 8.20 0 -5 -13 69.39 11.70 0 -5 -13 33.40 10.60 0 -5 -13 42.70 9.90 0 -5 -13 30.70 10.30 0 -5 -13 38.30 8.60 0 -5 -13 38.90 12.40 0 -5 -13 48.80 11.00 0 5 13 50.19 8.50 -1 -5 -13 56.79 9.10 -1 -5 -13 50.79 9.60 -1 -5 -13 65.69 11.70 -1 -5 -13 85.09 12.30 -1 -5 -13 68.59 13.80 -1 -5 -13 50.59 11.40 -1 -5 -13 57.29 9.00 -2 -5 -13 5.50 2.60 -2 -5 -13 5.80 2.90 -2 -5 -13 12.50 6.20 -2 -5 -13 21.90 9.90 -2 -5 -13 19.20 6.40 -2 -5 -13 2.70 10.60 -2 -5 -13 -8.70 12.90 2 5 13 8.70 8.70 -3 -5 -13 61.19 14.10 -3 -5 -13 46.80 11.50 -3 -5 -13 63.79 7.60 -3 -5 -13 64.79 9.00 -3 -5 -13 61.09 9.50 -3 -5 -13 50.09 12.00 3 5 13 52.39 7.90 3 5 13 58.59 10.70 3 5 13 48.60 5.50 -4 -5 -13 26.80 9.60 -4 -5 -13 26.90 7.90 -4 -5 -13 47.80 7.70 -4 -5 -13 32.00 11.40 -4 -5 -13 49.90 7.30 -4 -5 -13 41.10 6.30 -4 -5 -13 33.70 13.60 4 5 13 33.60 9.10 4 5 13 40.20 8.40 4 5 13 41.80 11.60 -5 -5 -13 72.39 14.20 -5 -5 -13 64.59 7.80 -5 -5 -13 49.80 14.40 -5 -5 -13 66.59 9.30 5 5 13 108.29 13.40 5 5 13 75.59 11.90 5 5 13 87.39 15.50 5 5 13 71.59 11.10 5 5 13 109.09 15.80 -1 -6 -13 7.30 6.40 -1 -6 -13 19.90 11.90 -1 -6 -13 -10.30 9.10 -1 -6 -13 10.10 7.90 -1 -6 -13 -5.60 6.60 -1 -6 -13 13.80 6.70 -1 -6 -13 12.60 9.30 -2 -6 -13 1.10 6.80 -2 -6 -13 2.00 9.90 -2 -6 -13 -0.40 9.60 -2 -6 -13 -2.10 1.50 -2 -6 -13 15.40 11.20 2 6 13 9.60 8.30 -3 -6 -13 -0.60 10.30 -3 -6 -13 15.80 5.00 -3 -6 -13 -0.30 9.90 -3 -6 -13 -0.10 3.50 -3 -6 -13 25.80 11.80 -3 -6 -13 2.40 5.20 -3 -6 -13 14.60 6.30 3 6 13 0.90 3.50 3 6 13 5.50 2.50 3 6 13 13.80 8.10 -4 -6 -13 1.70 13.10 -4 -6 -13 -11.70 8.80 -4 -6 -13 14.20 6.60 -4 -6 -13 -0.80 4.70 4 6 13 -9.10 10.40 4 6 13 5.50 4.40 4 6 13 -5.10 7.20 -2 -7 -13 58.09 10.20 -2 -7 -13 43.80 7.10 -2 -7 -13 62.99 13.30 -2 -7 -13 68.59 16.70 2 7 13 54.49 10.10 -3 -7 -13 13.90 12.60 -3 -7 -13 -6.90 3.40 -3 -7 -13 -11.30 6.20 -3 -7 -13 0.80 4.70 -3 -7 -13 5.30 10.70 -3 -7 -13 2.70 4.30 3 7 13 -1.30 2.40 3 7 13 0.70 7.30 -4 -7 -13 23.20 10.40 -4 -7 -13 57.09 16.10 -4 -7 -13 30.80 6.80 4 7 13 8.50 8.40 4 7 13 34.20 5.60 -2 -2 -14 88.69 10.50 -2 -2 -14 76.39 13.20 -2 -2 -14 59.79 8.70 2 2 14 66.39 8.20 2 2 14 70.69 14.20 -2 -3 -14 -7.70 9.40 -2 -3 -14 8.70 5.40 -2 -3 -14 -0.50 9.70 -2 -3 -14 -6.40 3.40 -2 -3 -14 12.20 8.00 2 3 14 6.40 16.20 -3 -3 -14 34.70 6.00 -3 -3 -14 44.50 11.30 -3 -3 -14 37.20 6.40 3 3 14 41.00 7.00 3 3 14 53.69 11.90 3 3 14 43.00 10.40 -2 -4 -14 8.50 10.60 -2 -4 -14 13.00 3.10 -2 -4 -14 18.20 10.10 -2 -4 -14 19.30 3.80 -2 -4 -14 27.00 6.90 -3 -4 -14 14.90 5.10 -3 -4 -14 -1.60 4.40 -3 -4 -14 25.00 10.80 -3 -4 -14 14.50 10.80 -3 -4 -14 1.40 5.20 3 4 14 3.30 4.50 3 4 14 2.70 8.60 3 4 14 2.60 9.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 74011 _olex2_submission_special_instructions 'No special instructions were received' 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 1.5985(2) 0.10212(18) 0.31046(16) 0.0524(5) Uani 1 1 d . . . . . O2 O -0.4659(2) 0.83910(18) 1.16780(15) 0.0526(5) Uani 1 1 d . . . . . O3 O -0.5912(3) 0.8538(2) 1.01170(19) 0.0725(7) Uani 1 1 d . . . . . O4 O 1.7734(3) 0.1535(2) 0.4141(2) 0.0746(7) Uani 1 1 d . . . . . C1 C 1.7849(4) 0.0339(3) 0.2409(2) 0.0548(7) Uani 1 1 d . . . . . H1A H 1.8843 0.0875 0.2174 0.082 Uiso 1 1 calc R U . . . H1B H 1.7604 0.0179 0.1705 0.082 Uiso 1 1 calc R U . . . H1C H 1.8338 -0.0490 0.2885 0.082 Uiso 1 1 calc R U . . . C2 C 1.6145(3) 0.1575(2) 0.3953(2) 0.0410(6) Uani 1 1 d . . . . . C3 C 1.4144(3) 0.2233(2) 0.46240(19) 0.0375(5) Uani 1 1 d . . . . . C4 C 1.2342(3) 0.2068(2) 0.4505(2) 0.0431(6) Uani 1 1 d . . . . . H4 H 1.2358 0.1545 0.3977 0.052 Uiso 1 1 calc R U . . . C5 C 1.0521(3) 0.2672(2) 0.5165(2) 0.0447(6) Uani 1 1 d . . . . . H5 H 0.9315 0.2555 0.5079 0.054 Uiso 1 1 calc R U . . . C6 C 1.0472(3) 0.3460(2) 0.59608(19) 0.0394(5) Uani 1 1 d . . . . . C7 C 0.8563(4) 0.4069(2) 0.6642(2) 0.0425(6) Uani 1 1 d . . . . . C8 C 0.6910(4) 0.4554(2) 0.7182(2) 0.0444(6) Uani 1 1 d . . . . . C9 C 0.5025(4) 0.5126(2) 0.7779(2) 0.0447(6) Uani 1 1 d . . . . . C10 C 0.3352(4) 0.5631(2) 0.8286(2) 0.0447(6) Uani 1 1 d . . . . . C11 C 0.1376(3) 0.6255(2) 0.8874(2) 0.0407(6) Uani 1 1 d . . . . . C12 C -0.0271(4) 0.6479(2) 0.8377(2) 0.0482(6) Uani 1 1 d . . . . . H12 H -0.0093 0.6208 0.7657 0.058 Uiso 1 1 calc R U . . . C13 C -0.2165(4) 0.7098(2) 0.8945(2) 0.0468(6) Uani 1 1 d . . . . . H13 H -0.3258 0.7244 0.8606 0.056 Uiso 1 1 calc R U . . . C14 C -0.2451(3) 0.7505(2) 1.0020(2) 0.0390(5) Uani 1 1 d . . . . . C15 C -0.4517(4) 0.8191(2) 1.0585(2) 0.0441(6) Uani 1 1 d . . . . . C16 C -0.6601(4) 0.9090(3) 1.2266(3) 0.0631(8) Uani 1 1 d . . . . . H16A H -0.6903 0.9968 1.1814 0.095 Uiso 1 1 calc R U . . . H16B H -0.6570 0.9140 1.3059 0.095 Uiso 1 1 calc R U . . . H16C H -0.7625 0.8628 1.2318 0.095 Uiso 1 1 calc R U . . . C17 C 0.1086(3) 0.6663(2) 0.9953(2) 0.0460(6) Uani 1 1 d . . . . . H17 H 0.2175 0.6516 1.0296 0.055 Uiso 1 1 calc R U . . . C18 C -0.0819(4) 0.7288(2) 1.0517(2) 0.0444(6) Uani 1 1 d . . . . . H18 H -0.1002 0.7563 1.1236 0.053 Uiso 1 1 calc R U . . . C19 C 1.4101(3) 0.3027(2) 0.5407(2) 0.0452(6) Uani 1 1 d . . . . . H19 H 1.5309 0.3149 0.5487 0.054 Uiso 1 1 calc R U . . . C20 C 1.2284(4) 0.3635(2) 0.6065(2) 0.0460(6) Uani 1 1 d . . . . . H20 H 1.2273 0.4168 0.6584 0.055 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 0.0377(9) 0.0618(11) 0.0618(11) -0.0308(9) -0.0117(8) 0.0001(8) O2 0.0416(10) 0.0586(11) 0.0514(10) -0.0195(8) -0.0046(8) 0.0011(8) O3 0.0439(11) 0.0979(17) 0.0779(14) -0.0315(12) -0.0233(10) 0.0047(10) O4 0.0347(10) 0.1107(18) 0.0930(16) -0.0549(13) -0.0192(10) -0.0021(10) C1 0.0434(14) 0.0555(16) 0.0621(16) -0.0262(13) -0.0058(12) 0.0017(11) C2 0.0393(13) 0.0415(13) 0.0444(13) -0.0101(10) -0.0137(10) -0.0066(10) C3 0.0357(12) 0.0394(12) 0.0379(12) -0.0076(9) -0.0124(9) -0.0045(9) C4 0.0379(12) 0.0516(14) 0.0453(13) -0.0187(11) -0.0116(10) -0.0081(10) C5 0.0317(11) 0.0580(15) 0.0489(13) -0.0157(11) -0.0104(10) -0.0106(10) C6 0.0351(12) 0.0425(12) 0.0356(11) -0.0051(10) -0.0072(9) -0.0035(10) C7 0.0430(13) 0.0416(13) 0.0405(12) -0.0064(10) -0.0086(10) -0.0074(10) C8 0.0444(14) 0.0426(13) 0.0420(13) -0.0073(10) -0.0056(11) -0.0082(11) C9 0.0460(14) 0.0415(13) 0.0434(13) -0.0084(10) -0.0049(11) -0.0094(11) C10 0.0467(14) 0.0385(13) 0.0447(13) -0.0066(10) -0.0040(11) -0.0107(10) C11 0.0384(12) 0.0360(12) 0.0426(12) -0.0077(9) -0.0012(10) -0.0083(9) C12 0.0526(15) 0.0503(14) 0.0445(13) -0.0197(11) -0.0101(11) -0.0071(11) C13 0.0440(14) 0.0494(14) 0.0516(14) -0.0123(11) -0.0185(11) -0.0069(11) C14 0.0385(12) 0.0359(12) 0.0411(12) -0.0053(9) -0.0088(10) -0.0076(9) C15 0.0395(13) 0.0403(13) 0.0510(14) -0.0062(10) -0.0093(11) -0.0098(10) C16 0.0479(15) 0.0622(17) 0.0649(17) -0.0193(14) 0.0023(13) 0.0018(13) C17 0.0364(12) 0.0540(15) 0.0481(13) -0.0118(11) -0.0113(10) -0.0072(10) C18 0.0432(13) 0.0515(14) 0.0400(12) -0.0152(11) -0.0074(10) -0.0092(11) C19 0.0358(12) 0.0545(14) 0.0526(14) -0.0164(11) -0.0170(10) -0.0083(10) C20 0.0464(13) 0.0505(14) 0.0455(13) -0.0196(11) -0.0129(11) -0.0054(11) 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_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 -1.00 -3.00 0.1030 -3.00 -2.00 0.00 0.0860 0.00 1.00 2.00 0.0830 2.00 3.00 3.00 0.0970 0.00 -3.00 1.00 0.0580 0.00 1.00 0.00 0.0670 0.00 -1.00 -3.00 0.1230 -3.00 -1.00 -3.00 0.1110 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 O1 C1 116.73(19) . . ? C15 O2 C16 115.9(2) . . ? O1 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 112.41(19) . . ? O4 C2 O1 122.7(2) . . ? O4 C2 C3 124.9(2) . . ? C4 C3 C2 122.2(2) . . ? C4 C3 C19 119.3(2) . . ? C19 C3 C2 118.44(19) . . ? C3 C4 H4 119.8 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.8 . . ? C4 C5 H5 119.7 . . ? C4 C5 C6 120.5(2) . . ? C6 C5 H5 119.7 . . ? C5 C6 C7 119.5(2) . . ? C20 C6 C5 118.9(2) . . ? C20 C6 C7 121.7(2) . . ? C8 C7 C6 176.5(3) . . ? C7 C8 C9 178.9(3) . . ? C10 C9 C8 178.7(3) . . ? C9 C10 C11 178.8(3) . . ? C12 C11 C10 121.0(2) . . ? C12 C11 C17 119.1(2) . . ? C17 C11 C10 119.9(2) . . ? C11 C12 H12 119.8 . . ? C13 C12 C11 120.4(2) . . ? C13 C12 H12 119.8 . . ? C12 C13 H13 119.8 . . ? C12 C13 C14 120.4(2) . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 118.2(2) . . ? C18 C14 C13 119.4(2) . . ? C18 C14 C15 122.3(2) . . ? O2 C15 C14 112.7(2) . . ? O3 C15 O2 123.0(2) . . ? O3 C15 C14 124.3(2) . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C17 H17 119.9 . . ? C18 C17 C11 120.1(2) . . ? C18 C17 H17 119.9 . . ? C14 C18 C17 120.5(2) . . ? C14 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C3 C19 H19 119.8 . . ? C20 C19 C3 120.5(2) . . ? C20 C19 H19 119.8 . . ? C6 C20 H20 119.8 . . ? C19 C20 C6 120.5(2) . . ? C19 C20 H20 119.8 . . ? 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 C1 1.445(3) . ? O1 C2 1.328(3) . ? O2 C15 1.333(3) . ? O2 C16 1.439(3) . ? O3 C15 1.197(3) . ? O4 C2 1.193(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.486(3) . ? C3 C4 1.381(3) . ? C3 C19 1.390(3) . ? C4 H4 0.9300 . ? C4 C5 1.377(3) . ? C5 H5 0.9300 . ? C5 C6 1.396(3) . ? C6 C7 1.429(3) . ? C6 C20 1.386(3) . ? C7 C8 1.201(3) . ? C8 C9 1.368(3) . ? C9 C10 1.204(3) . ? C10 C11 1.428(3) . ? C11 C12 1.390(3) . ? C11 C17 1.392(3) . ? C12 H12 0.9300 . ? C12 C13 1.377(3) . ? C13 H13 0.9300 . ? C13 C14 1.387(3) . ? C14 C15 1.486(3) . ? C14 C18 1.382(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17 0.9300 . ? C17 C18 1.383(3) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C19 C20 1.376(3) . ? C20 H20 0.9300 . ? 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 C2 C3 C4 10.8(3) . . . . ? O1 C2 C3 C19 -170.1(2) . . . . ? O4 C2 C3 C4 -169.2(3) . . . . ? O4 C2 C3 C19 10.0(4) . . . . ? C1 O1 C2 O4 0.7(4) . . . . ? C1 O1 C2 C3 -179.27(19) . . . . ? C2 C3 C4 C5 178.5(2) . . . . ? C2 C3 C19 C20 -178.7(2) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C3 C19 C20 C6 0.3(4) . . . . ? C4 C3 C19 C20 0.5(4) . . . . ? C4 C5 C6 C7 -179.6(2) . . . . ? C4 C5 C6 C20 0.8(4) . . . . ? C5 C6 C20 C19 -0.9(4) . . . . ? C7 C6 C20 C19 179.4(2) . . . . ? C10 C11 C12 C13 -179.1(2) . . . . ? C10 C11 C17 C18 179.0(2) . . . . ? C11 C12 C13 C14 -0.1(4) . . . . ? C11 C17 C18 C14 0.4(4) . . . . ? C12 C11 C17 C18 -0.3(4) . . . . ? C12 C13 C14 C15 178.9(2) . . . . ? C12 C13 C14 C18 0.2(4) . . . . ? C13 C14 C15 O2 172.4(2) . . . . ? C13 C14 C15 O3 -8.0(4) . . . . ? C13 C14 C18 C17 -0.3(4) . . . . ? C15 C14 C18 C17 -179.0(2) . . . . ? C16 O2 C15 O3 -1.6(4) . . . . ? C16 O2 C15 C14 178.0(2) . . . . ? C17 C11 C12 C13 0.1(4) . . . . ? C18 C14 C15 O2 -8.9(3) . . . . ? C18 C14 C15 O3 170.7(3) . . . . ? C19 C3 C4 C5 -0.7(4) . . . . ?