#------------------------------------------------------------------------------ #$Date: 2024-06-15 01:10:55 +0300 (Sat, 15 Jun 2024) $ #$Revision: 292399 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/18/1571887.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_1571887 loop_ _publ_author_name 'Zhao, Yankun' 'Yan, Hongya' 'Zhang, Yulian' 'Zhou, Tao' 'Tian, Mengxing' 'Zhang, Chongzhou' 'Yuan, Shan' 'Qiu, Hanyue' 'He, Ling' 'Zhang, Min' _publ_section_title ; Catalytic Asymmetric Intramolecular Propargylation of Cyclopropanols to Access the Cuparane Core ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC02504K _journal_year 2024 _chemical_absolute_configuration unk _chemical_formula_moiety 'C23 H24 O2' _chemical_formula_sum 'C23 H24 O2' _chemical_formula_weight 332.42 _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 _atom_sites_solution_primary dual _audit_creation_date 2022-10-24 _audit_creation_method ; Olex2 1.5 (compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410) ; _audit_update_record ; 2023-12-22 deposited with the CCDC. 2024-06-10 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.6478(3) _cell_length_b 10.5086(5) _cell_length_c 26.9042(15) _cell_measurement_reflns_used 2657 _cell_measurement_temperature 293 _cell_measurement_theta_max 26.3720 _cell_measurement_theta_min 3.9280 _cell_volume 1879.50(16) _computing_cell_refinement 'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)' _computing_data_collection 'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)' _computing_data_reduction 'CrysAlisPro 1.171.41.117a (Rigaku OD, 2021)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0892 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.888 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -40.00 42.00 1.00 18.00 -- 18.74 -38.00-150.00 82 2 \w -24.00 51.00 1.00 18.00 -- 18.74 19.00 90.00 75 3 \w -27.00 -2.00 1.00 18.00 -- -18.85 -77.00 120.00 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset/far, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0779480000 _diffrn_orient_matrix_UB_12 -0.0416942000 _diffrn_orient_matrix_UB_13 -0.0076626000 _diffrn_orient_matrix_UB_21 -0.0092972000 _diffrn_orient_matrix_UB_22 -0.0340855000 _diffrn_orient_matrix_UB_23 0.0226483000 _diffrn_orient_matrix_UB_31 -0.0721812000 _diffrn_orient_matrix_UB_32 -0.0406674000 _diffrn_orient_matrix_UB_33 -0.0111527000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_unetI/netI 0.0591 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.888 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 6986 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.860 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.866 _diffrn_reflns_theta_min 3.418 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91462 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.117a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.175 _exptl_crystal_description block _exptl_crystal_F_000 712 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.22 _refine_diff_density_max 0.180 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.042 _refine_ls_abs_structure_details ; Flack x determined using 902 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -1.3(10) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 229 _refine_ls_number_reflns 4231 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0556 _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^)+(0.0456P)^2^+0.3098P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1219 _refine_ls_wR_factor_ref 0.1392 _reflns_Friedel_coverage 0.684 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.823 _reflns_number_gt 3112 _reflns_number_total 4231 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc02504k2.cif _cod_data_source_block 20221024-zyk10066-1-1 _cod_database_code 1571887 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C23 H24 O2' _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. ; _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 C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C00F(H00F) 2.b Secondary CH2 refined with riding coordinates: C00B(H00B,H00C), C00H(H00H,H00I) 2.c Aromatic/amide H refined with riding coordinates: C009(H009), C00A(H00A), C00C(H00D), C00D(H00E), C00G(H00G), C00I(H00J), C00L(H00Q), C00M(H00R), C00N(H00S) 2.d Idealised Me refined as rotating group: C00J(H00K,H00L,H00M), C00K(H00N,H00O,H00P), C00O(H00T,H00U,H00V) 2.e : C00P(H00W) ; _shelx_res_file ; TITL 20221024-zyk10066-1-1_a.res in P2(1)2(1)2(1) 20221024-zyk10066-1-1.res created by SHELXL-2018/3 at 16:19:22 on 24-Oct-2022 REM Old TITL 20221024-Zhang Min-ZYK10066-1-1_auto in P2(1)2(1)2 REM SHELXT solution in P2(1)2(1)2(1): R1 0.156, Rweak 0.242, Alpha 0.003 REM 4.080 for 23 systematic absences, Orientation as input REM Flack x = -2.412 ( 0.982 ) from 985 Parsons' quotients REM Formula found by SHELXT: C22 O3 CELL 0.71073 6.6478 10.5086 26.9042 90 90 90 ZERR 4 0.0003 0.0005 0.0015 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 92 96 8 L.S. 10 PLAN 4 CONF BOND list 4 fmap 2 53 MORE -1 BOND $H ACTA REM REM REM WGHT 0.045600 0.309800 FVAR 0.76208 O001 3 -0.083580 0.070048 0.337845 11.00000 0.07432 0.05259 = 0.05947 -0.00337 -0.00528 -0.02452 O002 3 0.725963 0.356308 0.123936 11.00000 0.05208 0.07531 = 0.06292 0.02022 0.01373 0.00801 C003 1 0.416155 0.222781 0.248500 11.00000 0.05070 0.03556 = 0.03609 -0.00535 -0.00306 0.00050 C004 1 0.634657 0.309335 0.165779 11.00000 0.04311 0.04468 = 0.04527 0.00206 0.00015 -0.00225 C005 1 0.036664 0.377265 0.384671 11.00000 0.03124 0.03779 = 0.03739 0.00192 0.00020 -0.00133 C006 1 -0.024796 0.236811 0.398599 11.00000 0.04431 0.03861 = 0.03756 0.00720 -0.00280 -0.00719 C007 1 0.097015 0.459408 0.429620 11.00000 0.04070 0.03761 = 0.04066 0.00073 0.00022 0.00103 C008 1 -0.131636 0.441109 0.359039 11.00000 0.03994 0.04499 = 0.04410 0.00987 0.00156 -0.00164 C009 1 0.292790 0.500214 0.437754 11.00000 0.04478 0.04986 = 0.05473 -0.00781 -0.00646 0.00270 AFIX 43 H009 2 0.394189 0.476240 0.415857 11.00000 -1.20000 AFIX 0 C00A 1 0.608436 0.180616 0.239000 11.00000 0.05294 0.04202 = 0.04562 0.00214 -0.01030 0.00461 AFIX 43 H00A 2 0.666333 0.122172 0.260660 11.00000 -1.20000 AFIX 0 C00B 1 0.206104 0.356065 0.345546 11.00000 0.03657 0.03999 = 0.04442 0.00101 0.00446 -0.00342 AFIX 23 H00B 2 0.225852 0.431878 0.325566 11.00000 -1.20000 H00C 2 0.332037 0.334504 0.361691 11.00000 -1.20000 AFIX 0 C00C 1 0.337568 0.313743 0.216378 11.00000 0.04635 0.04234 = 0.04923 0.00209 0.00467 0.00839 AFIX 43 H00D 2 0.210237 0.346877 0.222503 11.00000 -1.20000 AFIX 0 C00D 1 0.719472 0.222004 0.198281 11.00000 0.03929 0.05068 = 0.05506 -0.00148 -0.00598 0.00389 AFIX 43 H00E 2 0.848988 0.191513 0.192905 11.00000 -1.20000 AFIX 0 C00E 1 -0.002651 0.170076 0.348304 11.00000 0.04477 0.03940 = 0.04339 0.00641 -0.00659 -0.00451 C00F 1 0.131614 0.245595 0.313485 11.00000 0.05003 0.03879 = 0.03562 -0.00063 -0.00172 -0.00437 AFIX 13 H00F 2 0.047741 0.280515 0.286815 11.00000 -1.20000 AFIX 0 C00G 1 0.444449 0.355913 0.175606 11.00000 0.05107 0.04648 = 0.05099 0.00888 -0.00078 0.00929 AFIX 43 H00G 2 0.387878 0.416271 0.154542 11.00000 -1.20000 AFIX 0 C00H 1 0.294558 0.162139 0.289873 11.00000 0.06683 0.04242 = 0.04432 -0.00196 0.00625 0.00257 AFIX 23 H00H 2 0.386684 0.135516 0.315826 11.00000 -1.20000 H00I 2 0.230873 0.086110 0.276819 11.00000 -1.20000 AFIX 0 C00I 1 -0.048816 0.497730 0.463219 11.00000 0.04899 0.05601 = 0.05715 -0.00793 0.00754 -0.00138 AFIX 43 H00J 2 -0.181468 0.472594 0.458305 11.00000 -1.20000 AFIX 0 C00J 1 0.918380 0.308085 0.110999 11.00000 0.05712 0.06401 = 0.06774 0.00238 0.01477 0.00324 AFIX 137 H00K 2 0.956106 0.339609 0.078832 11.00000 -1.50000 H00L 2 0.913755 0.216801 0.110213 11.00000 -1.50000 H00M 2 1.015435 0.335227 0.135200 11.00000 -1.50000 AFIX 0 C00K 1 0.130912 0.174882 0.433179 11.00000 0.08811 0.04922 = 0.04879 0.00902 -0.02304 0.00328 AFIX 137 H00N 2 0.262972 0.185084 0.419302 11.00000 -1.50000 H00O 2 0.101384 0.085895 0.436625 11.00000 -1.50000 H00P 2 0.125672 0.214973 0.465215 11.00000 -1.50000 AFIX 0 C00L 1 -0.001579 0.572797 0.504064 11.00000 0.08192 0.06259 = 0.04989 -0.00912 0.00529 0.00862 AFIX 43 H00Q 2 -0.101442 0.596103 0.526495 11.00000 -1.20000 AFIX 0 C00M 1 0.338645 0.576901 0.478514 11.00000 0.05495 0.06346 = 0.07209 -0.01755 -0.01743 0.00130 AFIX 43 H00R 2 0.470358 0.604004 0.483375 11.00000 -1.20000 AFIX 0 C00N 1 0.193394 0.612561 0.511234 11.00000 0.08251 0.05838 = 0.05355 -0.01375 -0.02024 0.01001 AFIX 43 H00S 2 0.225684 0.663583 0.538327 11.00000 -1.20000 AFIX 0 C00O 1 -0.235416 0.217563 0.419675 11.00000 0.06414 0.06258 = 0.07194 0.00844 0.02382 -0.01732 AFIX 137 H00T 2 -0.241042 0.250935 0.452862 11.00000 -1.50000 H00U 2 -0.266502 0.128363 0.420249 11.00000 -1.50000 H00V 2 -0.331369 0.261267 0.399188 11.00000 -1.50000 AFIX 0 C00P 1 -0.262259 0.492049 0.338093 11.00000 0.04972 0.08435 = 0.07178 0.03272 -0.00388 0.00992 AFIX 163 H00W 2 -0.366497 0.532700 0.321378 11.00000 -1.20000 AFIX 0 HKLF 4 REM 20221024-zyk10066-1-1_a.res in P2(1)2(1)2(1) REM wR2 = 0.1392, GooF = S = 1.065, Restrained GooF = 1.065 for all data REM R1 = 0.0556 for 3112 Fo > 4sig(Fo) and 0.0800 for all 4231 data REM 229 parameters refined using 0 restraints END WGHT 0.0455 0.3091 REM Highest difference peak 0.180, deepest hole -0.169, 1-sigma level 0.042 Q1 1 -0.0050 0.5776 0.3583 11.00000 0.05 0.18 Q2 1 0.3220 0.3853 0.1372 11.00000 0.05 0.15 Q3 1 0.9967 0.3812 0.1386 11.00000 0.05 0.15 Q4 1 0.0952 0.1883 0.5044 11.00000 0.05 0.13 ; _shelx_res_checksum 2473 _shelx_hkl_file ; 0 0 5 6.75 1.51 0 0 -5 9.88 2.21 0 0 6 1815.09 34.19 0 0 -6 1678.46 34.02 0 0 7 13.47 2.09 0 0 -7 15.46 2.66 0 0 -8 16.87 2.86 0 0 8 10.89 1.86 0 0 -9 6.59 2.08 0 0 9 2.96 1.34 0 0 -10 254.31 10.41 0 0 10 252.22 10.34 0 0 -11 26.31 4.24 0 0 -12 984.22 26.66 0 0 -13 67.55 7.04 0 0 -14 76.71 6.99 0 0 -15 45.71 5.65 0 0 -16 44.74 5.95 0 0 -17 28.26 5.49 0 0 -18 212.95 12.66 0 0 -19 38.36 6.02 0 0 -20 30.97 5.48 0 0 -21 38.70 6.49 0 0 -22 584.00 25.11 0 0 -23 30.45 6.15 0 0 -24 29.04 5.80 0 0 -25 12.30 4.12 0 0 -26 11.31 3.84 0 0 -27 8.43 3.93 0 0 -28 52.63 7.84 0 0 -29 2.09 1.81 0 0 -30 0.95 1.62 0 0 -31 2.58 2.56 0 0 -32 20.64 5.96 0 0 -33 3.57 2.60 0 1 -4 2295.51 41.25 0 -1 4 2272.32 41.31 0 1 4 2319.10 41.77 0 1 5 3218.86 56.99 0 1 -5 3165.81 56.52 0 -1 -5 3201.92 57.05 0 -1 5 3151.65 56.52 0 1 6 136.18 6.01 0 1 -6 125.43 5.62 0 -1 -6 125.61 5.94 0 -1 6 126.48 5.66 0 1 7 687.30 17.33 0 -1 7 658.42 17.04 0 1 -7 669.49 16.78 0 -1 -7 705.71 17.50 0 -1 -8 359.97 12.03 0 -1 8 336.54 11.36 0 1 -8 335.07 11.12 0 1 8 343.37 11.52 0 -1 9 2089.59 42.12 0 -1 -9 1935.27 42.78 0 1 9 2184.50 42.99 0 1 -9 2009.24 41.83 0 -1 10 4.36 1.57 0 1 -10 6.68 2.10 0 1 -11 33.56 3.72 0 -1 -11 34.66 4.14 0 -1 -12 137.28 8.41 0 1 -12 130.02 7.89 0 -1 -13 245.66 11.88 0 1 -13 253.53 11.71 0 1 -14 82.88 6.90 0 -1 -14 96.74 7.48 0 -1 -15 16.32 3.21 0 1 -15 15.31 3.23 0 -1 -16 12.36 3.89 0 1 -16 10.33 3.64 0 1 -17 425.47 17.74 0 -1 -17 419.14 18.13 0 1 -18 2.06 2.37 0 -1 -18 4.48 2.96 0 1 -19 45.15 6.20 0 -1 -19 52.99 6.51 0 -1 -20 120.84 10.02 0 1 -20 114.04 9.86 0 -1 -21 12.76 3.74 0 1 -21 16.46 4.36 0 -1 -22 21.89 4.94 0 1 -22 25.53 4.99 0 -1 -23 59.25 7.71 0 1 -23 61.57 7.77 0 1 -24 93.71 9.81 0 -1 -24 96.10 10.08 0 1 -25 25.25 5.27 0 -1 -25 22.63 4.92 0 -1 -26 56.71 8.08 0 1 -26 55.67 7.95 0 -1 -27 105.85 11.66 0 1 -27 111.26 11.79 0 1 -28 9.51 3.66 0 -1 -28 8.26 3.40 0 1 -29 7.17 3.68 0 -1 -29 6.21 3.43 0 1 -30 -1.13 2.64 0 -1 -30 -1.90 2.54 0 1 -31 -0.69 1.89 0 -1 -31 -0.10 1.91 0 1 -32 -1.67 2.47 0 1 -33 13.08 4.44 0 2 0 2738.52 48.93 0 -2 0 2717.08 49.16 0 2 1 273.27 8.22 0 2 -1 287.17 8.55 0 -2 -1 296.07 8.51 0 -2 1 299.11 8.69 0 2 -2 6510.54 113.75 0 2 2 6791.27 113.24 0 -2 -2 6785.86 113.35 0 -2 -3 2027.69 37.95 0 -2 3 2046.19 38.36 0 2 3 1957.00 37.68 0 2 -3 1977.60 37.03 0 2 4 102.79 5.17 0 2 -4 104.63 4.77 0 -2 4 106.42 4.88 0 -2 5 3688.88 64.51 0 2 -5 3645.44 64.58 0 2 5 3471.15 65.29 0 2 -6 2400.23 45.03 0 -2 6 2407.18 45.12 0 2 6 2292.25 45.63 0 -2 7 105.21 5.78 0 2 7 111.34 6.06 0 2 -7 109.51 5.82 0 2 -8 26.52 2.99 0 -2 8 26.41 2.93 0 2 8 25.45 2.96 0 -2 9 404.24 13.32 0 2 9 372.45 13.58 0 2 -9 393.28 13.07 0 2 -10 1484.24 33.45 0 2 -11 699.85 20.22 0 2 -12 19.16 3.12 0 -2 -12 23.92 4.23 0 2 -13 29.57 3.97 0 -2 -13 30.86 5.06 0 2 -14 359.18 15.08 0 -2 -14 378.95 15.81 0 -2 -15 110.44 8.57 0 2 -15 105.08 8.08 0 2 -16 30.46 4.44 0 -2 -16 27.02 4.39 0 -2 -17 0.81 1.47 0 2 -17 1.36 1.29 0 -2 -18 46.03 6.26 0 2 -18 52.11 6.63 0 2 -19 391.37 18.35 0 -2 -19 375.92 18.29 0 2 -20 75.40 8.20 0 -2 -20 99.54 9.29 0 2 -21 33.39 5.39 0 -2 -21 37.65 6.25 0 2 -22 12.03 3.47 0 -2 -22 8.99 3.25 0 2 -23 10.94 3.75 0 -2 -23 10.61 3.71 0 -2 -24 -0.53 2.68 0 2 -24 0.91 1.88 0 2 -25 7.39 3.14 0 2 -26 3.09 2.55 0 2 -27 11.35 4.04 0 2 -28 3.31 2.93 0 2 -29 35.14 6.80 0 2 -30 33.80 6.99 0 2 -31 5.71 3.51 0 2 -32 1.39 2.54 0 2 -33 0.24 2.41 0 -3 0 -0.66 0.85 0 3 0 -0.21 0.99 0 -3 1 524.21 14.29 0 -3 -1 497.10 10.84 0 3 1 476.79 13.72 0 3 -1 501.54 14.19 0 -3 -1 522.23 14.26 0 -3 -2 9999.00 162.07 0 -3 2 9597.56 162.33 0 -3 -2 9746.42 156.85 0 3 -2 9832.56 162.57 0 3 -3 4164.82 78.15 0 3 3 4279.26 77.44 0 -3 3 4404.01 78.23 0 -3 -3 4437.27 77.87 0 3 4 407.08 12.67 0 -3 4 425.23 13.34 0 -3 -4 428.09 13.28 0 3 -4 403.74 12.08 0 3 5 155.43 7.38 0 3 -5 148.35 6.86 0 -3 5 162.54 7.78 0 -3 -5 152.22 7.49 0 3 -6 728.33 18.89 0 3 6 755.53 19.99 0 -3 6 752.41 20.52 0 3 -7 63.10 4.74 0 -3 7 64.68 4.65 0 3 7 62.89 5.02 0 3 -8 51.13 4.38 0 3 8 57.40 4.98 0 -3 8 54.04 4.46 0 3 8 56.29 4.74 0 3 -9 691.36 19.56 0 3 -10 155.99 8.41 0 3 -11 866.03 23.96 0 3 -12 204.64 10.54 0 3 -13 64.57 5.85 0 3 -14 3.34 1.53 0 3 -15 91.74 7.86 0 3 -16 23.45 4.95 0 3 -17 3.59 1.95 0 3 -18 15.04 3.66 0 3 -19 81.36 8.25 0 3 -20 260.85 15.22 0 3 -21 99.39 9.70 0 3 -22 215.64 14.54 0 3 -23 49.08 7.21 0 3 -24 21.97 4.93 0 3 -25 83.40 9.62 0 3 -26 72.94 9.49 0 3 -27 24.37 5.71 0 3 -28 20.45 5.20 0 3 -29 10.12 3.92 0 3 -30 11.71 4.57 0 3 -31 1.06 1.69 0 3 -32 7.23 3.68 0 3 -33 -1.78 2.00 0 -4 0 0.32 0.69 0 4 0 0.05 1.07 0 4 -1 103.08 6.31 0 -4 1 113.50 6.59 0 -4 -1 103.86 4.38 0 4 1 106.57 6.38 0 -4 -1 104.06 6.29 0 4 2 11.85 2.07 0 4 -2 11.77 2.47 0 -4 2 10.28 1.98 0 -4 -2 9.78 1.20 0 -4 -2 9.91 1.94 0 -4 -3 11.49 2.08 0 4 -3 10.94 2.30 0 -4 3 6.46 1.57 0 4 3 7.19 1.88 0 4 4 132.52 7.41 0 -4 -4 122.75 7.14 0 4 5 1660.09 35.87 0 4 5 1575.74 28.08 0 -4 -5 1716.36 36.89 0 4 -5 1603.79 34.71 0 4 6 1174.71 28.60 0 4 -6 1235.45 27.96 0 4 6 1144.19 21.47 0 -4 -6 1179.45 29.21 0 4 7 213.31 10.04 0 4 -7 204.53 9.40 0 4 -8 1569.68 35.15 0 4 8 1481.47 35.70 0 4 -9 73.77 5.81 0 4 9 80.77 6.60 0 4 -10 7.34 2.05 0 4 10 8.89 2.24 0 4 -11 224.37 10.96 0 4 11 226.03 11.81 0 4 12 32.49 4.43 0 4 -12 34.48 4.36 0 4 13 123.86 9.03 0 4 -13 114.11 8.19 0 4 -14 161.54 9.94 0 4 -15 12.83 3.05 0 4 -16 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6.34 0 8 -3 49.79 6.49 0 8 -4 18.22 4.27 0 8 4 12.94 3.15 0 8 5 2.47 3.37 0 8 -6 1.59 1.25 0 8 6 4.54 2.31 0 8 -7 -0.46 1.26 0 8 7 -1.01 1.95 0 8 8 64.95 7.66 0 8 -8 57.43 6.61 0 8 9 -1.77 2.32 0 8 -9 -0.84 1.42 0 8 10 51.55 6.55 0 8 -10 43.57 5.73 0 8 11 18.72 4.17 0 8 -11 18.95 3.96 0 8 -12 57.91 6.75 0 8 12 53.95 6.96 0 8 -13 50.46 6.37 0 8 13 49.10 6.90 0 8 14 174.23 12.87 0 8 -14 165.80 11.93 0 8 -15 49.06 6.58 0 8 15 36.46 6.03 0 8 16 46.67 6.85 0 8 -16 42.96 6.19 0 8 17 11.42 3.43 0 8 -17 20.39 4.51 0 8 -18 3.82 1.78 0 8 18 6.71 2.91 0 8 -19 -0.61 1.64 0 8 19 -0.74 1.66 0 8 20 13.83 4.20 0 8 -20 13.46 3.85 0 8 -21 0.75 1.53 0 8 21 5.14 2.87 0 8 22 15.98 4.44 0 8 -22 12.13 3.65 0 8 23 12.00 3.92 0 8 -23 12.54 4.24 0 8 -24 11.25 3.93 0 8 24 7.63 3.56 0 8 -25 0.20 1.80 0 8 25 -3.33 2.40 0 8 -26 5.45 2.78 0 8 26 2.46 2.20 0 8 -27 4.43 2.97 0 8 27 -1.84 1.91 0 8 28 2.59 2.25 0 8 -28 1.34 2.15 0 8 -29 1.78 2.14 0 8 29 4.42 3.17 0 9 0 4.21 2.69 0 9 1 100.64 9.56 0 9 -1 105.59 9.82 0 9 2 96.16 9.27 0 9 -2 94.81 9.61 0 9 -3 6.97 3.13 0 9 3 5.59 2.60 0 9 4 52.65 6.92 0 9 5 18.37 4.03 0 9 -6 116.66 9.58 0 9 6 144.01 11.98 0 9 7 6.39 2.72 0 9 -7 8.60 2.69 0 9 8 1.58 1.45 0 9 -8 6.23 2.40 0 9 -9 96.13 8.77 0 9 9 92.43 9.44 0 9 -10 -0.12 1.30 0 9 10 -0.80 1.97 0 9 -11 4.88 2.13 0 9 11 14.89 3.96 0 9 12 11.18 3.42 0 9 -12 7.56 2.74 0 9 -13 -0.49 1.42 0 9 13 -1.39 1.39 0 9 -14 22.50 4.52 0 9 14 20.94 4.76 0 9 15 15.50 4.12 0 9 -15 18.78 4.36 0 9 16 13.29 4.10 0 9 -16 15.85 3.96 0 9 17 -2.27 1.77 0 9 -17 6.89 3.09 0 9 -18 48.81 7.06 0 9 18 33.95 6.16 0 9 19 14.01 4.40 0 9 -19 14.95 4.34 0 9 -20 80.55 9.26 0 9 20 89.67 10.32 0 9 -21 1.28 2.10 0 9 21 1.71 1.94 0 9 22 22.43 5.44 0 9 -22 16.88 4.46 0 9 23 14.77 4.51 0 9 -23 14.75 4.29 0 9 -24 24.19 5.58 0 9 24 28.30 6.28 0 9 -25 -4.74 2.76 0 9 25 -1.47 2.23 0 9 -26 5.45 3.28 0 9 26 4.94 3.31 0 9 -27 10.46 4.12 0 9 -28 1.48 1.98 0 10 0 14.51 4.01 0 10 1 7.59 2.48 0 10 -1 7.81 3.23 0 10 2 29.07 5.69 0 10 -2 27.77 5.47 0 10 3 29.71 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4.85 7 3 -3 28.20 6.13 -7 3 3 21.62 4.43 7 3 -2 22.86 5.85 -7 3 2 14.01 3.75 7 3 -1 33.22 6.71 -7 3 1 29.90 5.17 7 3 0 35.09 6.98 -7 3 0 31.59 5.14 7 3 1 31.32 7.06 7 -3 -2 22.37 5.55 7 3 2 16.89 5.18 7 3 3 23.42 5.72 7 -3 -3 26.03 5.85 7 3 4 -0.48 3.32 7 -3 -4 6.32 2.88 -7 3 -4 4.78 2.68 7 -3 -5 30.76 5.92 -7 3 -5 28.46 5.75 7 -3 -6 5.31 2.81 -7 3 -6 1.54 1.35 -7 3 -7 16.98 5.00 7 -3 -7 19.72 4.53 7 -3 -8 2.07 1.68 -7 3 -8 -1.91 1.60 7 -3 -9 9.26 3.23 -7 3 -9 12.75 4.15 7 -3 -10 13.70 3.82 -7 3 -10 6.22 2.86 -7 3 -11 7.60 3.21 7 -3 -11 13.95 3.85 -7 3 -12 9.00 3.57 -7 3 -13 16.20 4.71 -7 3 -14 2.11 1.55 -7 3 -15 10.10 3.89 -7 3 -16 16.69 4.86 -7 3 -17 3.91 3.29 -7 3 -18 3.99 3.12 -7 3 -19 0.57 1.90 -7 3 -20 3.75 2.89 -7 4 18 10.43 4.40 -7 4 17 2.08 1.77 -7 4 16 21.11 5.74 -7 4 15 -2.56 2.22 -7 4 14 5.08 2.95 -7 4 13 3.13 2.45 -7 4 12 10.03 3.78 -7 4 11 -0.70 2.12 -7 4 10 11.10 3.67 -7 4 9 5.33 2.93 -7 4 8 3.58 2.59 -7 4 7 0.71 1.31 7 4 -7 4.45 3.41 -7 4 6 17.57 4.61 7 4 -6 38.59 7.22 -7 4 5 -2.59 2.40 7 4 -5 3.05 3.49 7 4 -4 13.88 4.36 -7 4 4 7.28 2.73 7 4 -3 10.41 3.73 -7 4 3 6.30 2.96 7 4 -2 42.86 7.92 -7 4 2 39.68 6.21 7 4 -1 11.32 4.28 -7 4 1 12.90 3.61 7 4 0 115.23 12.78 -7 4 0 97.95 9.75 7 4 1 4.26 3.35 -7 4 -1 21.91 4.57 7 -4 -2 34.28 6.59 7 4 2 47.46 8.11 -7 4 -2 35.13 5.77 7 -4 -3 11.00 3.78 7 4 3 15.74 4.98 -7 4 -3 9.57 2.98 7 4 4 5.40 2.89 7 -4 -4 9.27 3.64 7 4 5 -4.01 3.55 -7 4 -5 0.74 1.29 7 -4 -5 -3.65 3.02 7 4 6 8.12 4.20 7 -4 -6 14.80 4.15 7 -4 -7 4.15 2.68 -7 4 -7 3.83 2.19 -7 4 -8 2.74 2.62 7 -4 -8 3.11 1.95 7 -4 -9 5.94 2.45 -7 4 -9 2.89 1.60 -7 4 -10 10.62 3.74 -7 4 -11 5.91 3.24 -7 4 -12 13.43 4.49 -7 4 -13 5.29 2.99 -7 4 -14 0.80 2.01 -7 4 -15 0.06 1.52 -7 4 -16 18.15 5.49 -7 4 -17 5.17 3.35 -7 4 -18 9.05 3.96 -7 5 16 1.96 1.64 -7 5 15 5.61 2.80 -7 5 14 1.23 2.09 -7 5 13 3.19 2.35 -7 5 12 13.72 4.40 -7 5 11 0.61 1.88 -7 5 10 3.27 2.26 -7 5 9 -4.18 3.28 -7 5 8 14.94 4.59 -7 5 7 5.04 2.74 -7 5 6 7.75 3.01 7 5 -6 19.87 5.22 7 5 -5 1.33 2.47 -7 5 5 1.72 1.27 7 5 -4 11.16 4.41 -7 5 4 2.18 1.88 7 5 -3 5.88 3.39 -7 5 3 2.52 2.12 7 5 -2 11.56 4.30 -7 5 2 13.71 4.04 7 5 -1 53.59 8.75 -7 5 1 34.73 6.24 7 5 0 7.45 3.52 -7 5 0 1.90 1.95 7 5 1 34.37 7.25 -7 5 -1 32.63 5.95 7 -5 -2 10.40 3.54 7 5 2 14.72 5.06 -7 5 -2 14.55 3.92 7 -5 -3 7.18 2.82 7 5 3 0.94 2.61 -7 5 -3 5.26 2.41 7 -5 -4 2.21 1.87 -7 5 -4 -0.45 1.24 7 5 5 -1.42 2.87 -7 5 -5 3.41 2.53 -7 5 -5 5.81 2.70 7 5 6 11.46 4.90 -7 5 -6 9.86 3.71 -7 5 -7 9.22 3.84 7 5 7 0.61 2.26 7 5 8 15.90 5.16 -7 5 -8 21.56 5.37 -7 5 -9 -0.64 2.23 7 5 9 -7.08 4.46 -7 5 -10 4.35 2.63 -7 5 -11 2.77 2.03 -7 5 -12 13.81 4.64 -7 5 -13 10.68 4.34 -7 5 -14 1.99 2.42 -7 5 -15 3.17 2.52 -7 6 13 -0.60 1.85 -7 6 12 4.22 2.54 -7 6 11 7.66 3.52 -7 6 10 16.66 5.08 -7 6 9 0.12 2.27 -7 6 8 -2.89 2.34 -7 6 7 10.03 3.70 -7 6 6 4.71 3.05 -7 6 5 8.98 3.62 7 6 -4 4.42 3.06 -7 6 4 3.05 2.40 7 6 -3 9.43 3.87 -7 6 3 9.00 3.56 7 6 -2 2.46 3.05 -7 6 2 3.57 2.43 7 6 -1 12.93 4.51 -7 6 1 7.50 3.30 7 6 0 16.93 5.08 -7 6 0 10.83 3.64 7 6 1 13.82 4.69 -7 6 -1 11.37 3.90 7 6 2 2.04 2.27 -7 6 -2 2.86 2.25 7 6 3 3.54 2.68 -7 6 -3 4.77 2.48 7 6 4 -1.29 2.24 -7 6 -4 4.52 2.57 7 6 5 7.15 3.64 -7 6 -5 5.62 2.54 -7 6 -5 7.10 3.16 7 6 6 1.03 3.15 -7 6 -6 -0.67 1.89 -7 6 -6 -1.20 1.63 7 6 7 5.99 3.25 -7 6 -7 8.52 3.85 -7 6 -7 15.61 4.30 7 6 8 -2.26 3.22 -7 6 -8 2.43 2.73 7 6 9 -1.99 3.24 -7 6 -9 -1.80 2.49 -7 6 -10 25.22 6.26 7 6 10 15.34 5.24 7 6 11 -0.22 2.88 -7 6 -11 0.80 1.75 7 6 12 -8.24 4.14 -7 6 -12 6.39 3.66 -7 7 10 2.21 1.93 -7 7 9 -2.56 2.29 -7 7 8 3.05 2.34 -7 7 7 13.57 4.82 -7 7 6 1.78 2.11 -7 7 5 5.10 2.98 -7 7 4 19.61 5.28 -7 7 3 62.90 9.37 7 7 -2 13.97 5.18 -7 7 2 3.49 2.48 7 7 -1 15.49 4.82 -7 7 1 9.00 3.92 7 7 0 9.92 4.16 -7 7 0 4.66 2.92 7 7 1 21.98 5.90 -7 7 -1 25.32 5.83 7 7 2 13.13 5.11 -7 7 -2 5.00 2.56 7 7 3 57.45 9.28 -7 7 -3 45.44 7.61 7 7 4 29.53 6.50 -7 7 -4 11.91 3.86 7 7 5 1.74 2.31 -7 7 -5 7.28 3.34 7 7 6 -1.59 2.44 -7 7 -6 0.05 1.75 -7 7 -6 5.09 3.14 7 7 7 19.01 5.52 -7 7 -7 17.66 5.53 -7 7 -7 16.96 4.90 7 7 8 4.60 3.38 -7 7 -8 5.73 3.12 7 7 9 -1.34 2.10 7 7 10 -1.75 2.16 7 7 11 0.42 1.65 -7 8 4 3.86 2.86 -7 8 3 1.46 1.70 -7 8 2 1.34 2.01 -7 8 1 9.07 3.89 -7 8 0 -7.95 3.62 -7 8 -1 8.47 3.87 -7 8 -2 3.00 2.69 -7 8 -3 -0.83 1.80 -7 8 -4 0.22 1.46 -7 8 -5 0.70 1.46 -7 8 -6 1.08 1.74 -7 8 -7 3.75 2.87 -7 8 -8 3.93 2.72 8 0 0 3.54 3.02 8 0 1 3.56 3.13 8 0 -1 -3.73 3.19 8 0 2 -2.11 3.65 8 0 -2 -0.26 2.85 8 0 -3 8.50 3.88 8 0 -4 13.65 4.74 8 0 -5 5.49 2.95 8 0 -6 7.30 3.88 8 0 -7 18.20 5.39 8 0 -8 7.11 3.57 8 0 -9 10.67 4.03 8 0 -10 4.54 3.36 8 1 -9 5.20 3.06 8 1 -8 5.41 3.35 8 1 -7 7.86 3.55 8 1 -6 4.21 3.07 8 1 -5 -1.74 2.32 8 1 -4 7.91 3.85 8 1 -3 1.03 2.60 8 1 -2 3.72 2.33 8 -1 1 16.63 5.68 8 1 -1 11.30 4.75 8 -1 0 4.10 3.04 8 1 0 -3.24 3.13 8 1 1 10.02 4.11 8 -1 -1 8.45 3.86 8 1 2 2.17 2.18 8 -1 -2 0.24 2.19 8 1 3 -8.01 4.29 8 -1 -3 0.16 1.92 8 1 4 3.67 2.87 8 -1 -4 9.37 3.67 8 -1 -5 2.66 2.82 8 -1 -6 6.17 3.60 8 -1 -7 6.90 3.25 8 -1 -8 4.81 3.05 8 -1 -9 4.19 2.92 8 -1 -10 2.00 2.26 8 2 -8 18.83 5.31 8 2 -7 10.58 4.48 8 2 -6 7.57 3.97 8 2 -5 22.18 5.87 8 2 -4 0.34 2.09 8 2 -3 0.15 2.26 8 2 -2 5.83 3.78 8 -2 1 -0.75 2.15 8 2 -1 5.63 3.34 8 -2 0 11.69 4.49 8 2 0 6.59 3.88 8 -2 -1 0.70 1.77 8 2 1 5.08 2.38 8 2 2 1.16 2.75 8 -2 -2 -1.74 2.58 8 2 3 -11.82 4.91 8 -2 -3 -2.70 2.64 8 2 4 3.75 3.03 8 -2 -4 2.60 2.42 8 2 5 9.58 4.04 8 -2 -5 18.56 5.30 8 -2 -6 7.51 3.29 8 -2 -7 5.51 3.13 8 -2 -8 12.28 4.36 8 -2 -9 1.79 2.40 8 -2 -10 23.72 5.63 -8 3 15 0.10 1.04 -8 3 14 9.08 3.87 8 3 -6 23.85 6.09 8 3 -5 -1.73 2.83 8 3 -4 6.64 3.89 8 3 -3 7.91 4.25 8 3 -2 5.53 3.49 8 3 -1 -2.09 1.95 8 -3 0 0.69 2.10 8 3 0 3.73 3.80 8 -3 -1 -1.60 2.04 8 3 1 -1.91 2.69 8 -3 -2 12.37 4.43 8 3 2 4.88 3.61 -8 3 -2 6.17 3.16 8 3 3 -1.44 2.40 8 -3 -3 0.80 1.57 -8 3 -3 0.38 1.40 8 3 4 9.73 4.64 8 -3 -4 2.58 2.02 -8 3 -4 7.11 3.36 8 -3 -5 -3.13 2.94 -8 3 -5 -1.14 2.46 -8 3 -6 21.77 5.69 8 -3 -6 26.09 6.18 8 -3 -7 6.87 3.26 -8 3 -7 -1.21 1.85 8 -3 -8 11.03 3.98 -8 3 -8 11.83 4.17 8 -3 -9 0.55 1.41 -8 3 -9 0.55 1.46 -8 3 -10 23.54 6.13 -8 3 -11 4.55 3.10 -8 3 -12 9.80 4.25 -8 3 -13 5.98 3.50 -8 3 -14 9.11 4.11 -8 3 -15 0.01 2.13 -8 4 13 1.94 1.87 -8 4 12 6.04 3.49 -8 4 11 0.76 2.10 -8 4 10 4.73 2.81 8 -4 0 -5.41 3.33 8 -4 -1 15.04 5.06 8 -4 -2 2.67 2.68 -8 4 -2 2.21 2.18 8 -4 -3 -0.87 2.24 -8 4 -3 5.03 2.82 8 -4 -4 0.97 1.76 -8 4 -4 -0.01 1.25 8 -4 -5 10.77 3.92 -8 4 -5 9.94 4.04 -8 4 -6 7.71 3.86 -8 4 -7 0.82 1.88 -8 4 -8 0.35 1.64 -8 4 -9 13.82 4.98 -8 4 -10 4.59 3.33 -8 4 -11 -0.58 1.54 -8 4 -12 6.24 3.71 -8 5 10 15.30 5.08 -8 5 9 0.01 1.81 -8 5 8 9.31 3.99 -8 5 -3 3.23 2.35 -8 5 -4 0.62 1.74 -8 5 -5 10.56 4.31 -8 5 -6 6.68 3.83 -8 5 -7 4.42 3.00 -8 6 7 12.08 4.51 -8 6 6 -0.40 2.38 -8 6 5 7.17 3.63 0 0 0 0.00 0.00 TITL 20221024-Zhang Min-ZYK10066-1-1_auto in P2(1)2(1)2 REM P2(1)2(1)2 (#18 in standard setting) CELL 0.71073 6.647780 10.508620 26.904215 90.0000 90.0000 90.0000 ZERR 4.00 0.000294 0.000544 0.001456 0.0000 0.0000 0.0000 LATT -1 SYMM -x,-y, z SYMM -x+1/2, y+1/2,-z SYMM x+1/2,-y+1/2,-z SFAC C H O UNIT 92.00 96.00 8.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 68416 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.202 _oxdiff_exptl_absorpt_empirical_full_min 0.870 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 O001 O -0.0836(4) 0.0700(2) 0.33784(10) 0.0621(8) Uani 1 1 d . . . . . O002 O 0.7260(4) 0.3563(3) 0.12394(10) 0.0634(8) Uani 1 1 d . . . . . C003 C 0.4162(5) 0.2228(3) 0.24850(12) 0.0408(8) Uani 1 1 d . . . . . C004 C 0.6347(5) 0.3093(3) 0.16578(13) 0.0444(8) Uani 1 1 d . . . . . C005 C 0.0367(4) 0.3773(3) 0.38467(11) 0.0355(7) Uani 1 1 d . . . . . C006 C -0.0248(5) 0.2368(3) 0.39860(12) 0.0402(8) Uani 1 1 d . . . . . C007 C 0.0970(5) 0.4594(3) 0.42962(13) 0.0397(8) Uani 1 1 d . . . . . C008 C -0.1316(5) 0.4411(3) 0.35904(13) 0.0430(8) Uani 1 1 d . . . . . C009 C 0.2928(5) 0.5002(3) 0.43775(14) 0.0498(9) Uani 1 1 d . . . . . H009 H 0.394189 0.476240 0.415857 0.060 Uiso 1 1 calc R U . . . C00A C 0.6084(5) 0.1806(3) 0.23900(13) 0.0469(8) Uani 1 1 d . . . . . H00A H 0.666333 0.122172 0.260660 0.056 Uiso 1 1 calc R U . . . C00B C 0.2061(5) 0.3561(3) 0.34555(12) 0.0403(8) Uani 1 1 d . . . . . H00B H 0.225852 0.431878 0.325566 0.048 Uiso 1 1 calc R U . . . H00C H 0.332037 0.334504 0.361691 0.048 Uiso 1 1 calc R U . . . C00C C 0.3376(5) 0.3137(3) 0.21638(13) 0.0460(8) Uani 1 1 d . . . . . H00D H 0.210237 0.346877 0.222503 0.055 Uiso 1 1 calc R U . . . C00D C 0.7195(5) 0.2220(3) 0.19828(14) 0.0483(9) Uani 1 1 d . . . . . H00E H 0.848988 0.191513 0.192905 0.058 Uiso 1 1 calc R U . . . C00E C -0.0027(5) 0.1701(3) 0.34830(12) 0.0425(8) Uani 1 1 d . . . . . C00F C 0.1316(5) 0.2456(3) 0.31349(13) 0.0415(8) Uani 1 1 d . . . . . H00F H 0.047741 0.280515 0.286815 0.050 Uiso 1 1 calc R U . . . C00G C 0.4444(5) 0.3559(3) 0.17561(14) 0.0495(9) Uani 1 1 d . . . . . H00G H 0.387878 0.416271 0.154542 0.059 Uiso 1 1 calc R U . . . C00H C 0.2946(6) 0.1621(3) 0.28987(14) 0.0512(9) Uani 1 1 d . . . . . H00H H 0.386684 0.135516 0.315826 0.061 Uiso 1 1 calc R U . . . H00I H 0.230873 0.086110 0.276819 0.061 Uiso 1 1 calc R U . . . C00I C -0.0488(6) 0.4977(4) 0.46322(15) 0.0541(10) Uani 1 1 d . . . . . H00J H -0.181468 0.472594 0.458305 0.065 Uiso 1 1 calc R U . . . C00J C 0.9184(5) 0.3081(4) 0.11100(16) 0.0630(11) Uani 1 1 d . . . . . H00K H 0.956106 0.339609 0.078832 0.094 Uiso 1 1 calc R U . . . H00L H 0.913755 0.216801 0.110213 0.094 Uiso 1 1 calc R U . . . H00M H 1.015435 0.335227 0.135200 0.094 Uiso 1 1 calc R U . . . C00K C 0.1309(7) 0.1749(4) 0.43318(14) 0.0620(11) Uani 1 1 d . . . . . H00N H 0.262972 0.185084 0.419302 0.093 Uiso 1 1 calc R U . . . H00O H 0.101384 0.085895 0.436625 0.093 Uiso 1 1 calc R U . . . H00P H 0.125672 0.214973 0.465215 0.093 Uiso 1 1 calc R U . . . C00L C -0.0016(7) 0.5728(4) 0.50406(15) 0.0648(11) Uani 1 1 d . . . . . H00Q H -0.101442 0.596103 0.526495 0.078 Uiso 1 1 calc R U . . . C00M C 0.3386(6) 0.5769(4) 0.47851(16) 0.0635(12) Uani 1 1 d . . . . . H00R H 0.470358 0.604004 0.483375 0.076 Uiso 1 1 calc R U . . . C00N C 0.1934(7) 0.6126(4) 0.51123(16) 0.0648(11) Uani 1 1 d . . . . . H00S H 0.225684 0.663583 0.538327 0.078 Uiso 1 1 calc R U . . . C00O C -0.2354(6) 0.2176(4) 0.41967(17) 0.0662(12) Uani 1 1 d . . . . . H00T H -0.241042 0.250935 0.452862 0.099 Uiso 1 1 calc R U . . . H00U H -0.266502 0.128363 0.420249 0.099 Uiso 1 1 calc R U . . . H00V H -0.331369 0.261267 0.399188 0.099 Uiso 1 1 calc R U . . . C00P C -0.2623(6) 0.4920(5) 0.33809(17) 0.0686(12) Uani 1 1 d . . . . . H00W H -0.366497 0.532700 0.321378 0.082 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 O001 0.0743(18) 0.0526(15) 0.0595(17) -0.0034(13) -0.0053(15) -0.0245(15) O002 0.0521(14) 0.0753(19) 0.0629(18) 0.0202(15) 0.0137(14) 0.0080(14) C003 0.0507(18) 0.0356(17) 0.0361(18) -0.0054(13) -0.0031(16) 0.0005(16) C004 0.0431(17) 0.0447(18) 0.045(2) 0.0021(16) 0.0001(16) -0.0022(16) C005 0.0312(15) 0.0378(16) 0.0374(18) 0.0019(13) 0.0002(14) -0.0013(14) C006 0.0443(17) 0.0386(17) 0.0376(18) 0.0072(14) -0.0028(15) -0.0072(15) C007 0.0407(17) 0.0376(17) 0.0407(19) 0.0007(13) 0.0002(16) 0.0010(15) C008 0.0399(17) 0.0450(18) 0.044(2) 0.0099(16) 0.0016(16) -0.0016(16) C009 0.0448(18) 0.050(2) 0.055(2) -0.0078(18) -0.0065(18) 0.0027(18) C00A 0.053(2) 0.0420(18) 0.046(2) 0.0021(15) -0.0103(17) 0.0046(17) C00B 0.0366(16) 0.0400(17) 0.0444(19) 0.0010(15) 0.0045(15) -0.0034(15) C00C 0.0463(18) 0.0423(18) 0.049(2) 0.0021(16) 0.0047(17) 0.0084(16) C00D 0.0393(17) 0.051(2) 0.055(2) -0.0015(17) -0.0060(17) 0.0039(17) C00E 0.0448(17) 0.0394(18) 0.0434(19) 0.0064(15) -0.0066(16) -0.0045(16) C00F 0.0500(19) 0.0388(17) 0.0356(18) -0.0006(14) -0.0017(16) -0.0044(17) C00G 0.051(2) 0.046(2) 0.051(2) 0.0089(16) -0.0008(18) 0.0093(18) C00H 0.067(2) 0.0424(19) 0.044(2) -0.0020(16) 0.0062(19) 0.0026(18) C00I 0.049(2) 0.056(2) 0.057(2) -0.0079(19) 0.0075(19) -0.0014(18) C00J 0.057(2) 0.064(2) 0.068(3) 0.002(2) 0.015(2) 0.003(2) C00K 0.088(3) 0.049(2) 0.049(2) 0.0090(18) -0.023(2) 0.003(2) C00L 0.082(3) 0.063(3) 0.050(2) -0.009(2) 0.005(2) 0.009(2) C00M 0.055(2) 0.063(2) 0.072(3) -0.018(2) -0.017(2) 0.001(2) C00N 0.083(3) 0.058(2) 0.054(2) -0.0137(19) -0.020(2) 0.010(2) C00O 0.064(2) 0.063(3) 0.072(3) 0.008(2) 0.024(2) -0.017(2) C00P 0.050(2) 0.084(3) 0.072(3) 0.033(2) -0.004(2) 0.010(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C004 O002 C00J 118.2(3) . . ? C00A C003 C00C 117.0(3) . . ? C00A C003 C00H 119.7(3) . . ? C00C C003 C00H 123.0(3) . . ? O002 C004 C00D 125.2(3) . . ? O002 C004 C00G 115.8(3) . . ? C00G C004 C00D 119.1(3) . . ? C007 C005 C006 113.9(3) . . ? C007 C005 C00B 115.0(2) . . ? C008 C005 C006 109.9(3) . . ? C008 C005 C007 108.1(3) . . ? C008 C005 C00B 107.3(3) . . ? C00B C005 C006 102.4(2) . . ? C00E C006 C005 101.2(2) . . ? C00E C006 C00K 106.0(3) . . ? C00K C006 C005 111.5(3) . . ? C00O C006 C005 116.8(3) . . ? C00O C006 C00E 110.9(3) . . ? C00O C006 C00K 109.7(3) . . ? C009 C007 C005 122.8(3) . . ? C00I C007 C005 119.6(3) . . ? C00I C007 C009 117.6(3) . . ? C00P C008 C005 178.8(4) . . ? C007 C009 H009 119.7 . . ? C007 C009 C00M 120.5(4) . . ? C00M C009 H009 119.7 . . ? C003 C00A H00A 118.7 . . ? C003 C00A C00D 122.6(3) . . ? C00D C00A H00A 118.7 . . ? C005 C00B H00B 110.8 . . ? C005 C00B H00C 110.8 . . ? H00B C00B H00C 108.9 . . ? C00F C00B C005 104.8(2) . . ? C00F C00B H00B 110.8 . . ? C00F C00B H00C 110.8 . . ? C003 C00C H00D 119.3 . . ? C00G C00C C003 121.4(3) . . ? C00G C00C H00D 119.3 . . ? C004 C00D C00A 119.2(3) . . ? C004 C00D H00E 120.4 . . ? C00A C00D H00E 120.4 . . ? O001 C00E C006 124.0(3) . . ? O001 C00E C00F 124.8(3) . . ? C00F C00E C006 111.3(3) . . ? C00B C00F H00F 108.2 . . ? C00B C00F C00H 116.1(3) . . ? C00E C00F C00B 103.8(3) . . ? C00E C00F H00F 108.2 . . ? C00E C00F C00H 111.9(3) . . ? C00H C00F H00F 108.2 . . ? C004 C00G H00G 119.7 . . ? C00C C00G C004 120.6(3) . . ? C00C C00G H00G 119.7 . . ? C003 C00H C00F 116.2(3) . . ? C003 C00H H00H 108.2 . . ? C003 C00H H00I 108.2 . . ? C00F C00H H00H 108.2 . . ? C00F C00H H00I 108.2 . . ? H00H C00H H00I 107.4 . . ? C007 C00I H00J 119.2 . . ? C007 C00I C00L 121.5(4) . . ? C00L C00I H00J 119.2 . . ? O002 C00J H00K 109.5 . . ? O002 C00J H00L 109.5 . . ? O002 C00J H00M 109.5 . . ? H00K C00J H00L 109.5 . . ? H00K C00J H00M 109.5 . . ? H00L C00J H00M 109.5 . . ? C006 C00K H00N 109.5 . . ? C006 C00K H00O 109.5 . . ? C006 C00K H00P 109.5 . . ? H00N C00K H00O 109.5 . . ? H00N C00K H00P 109.5 . . ? H00O C00K H00P 109.5 . . ? C00I C00L H00Q 120.1 . . ? C00N C00L C00I 119.8(4) . . ? C00N C00L H00Q 120.1 . . ? C009 C00M H00R 119.6 . . ? C00N C00M C009 120.9(4) . . ? C00N C00M H00R 119.6 . . ? C00L C00N H00S 120.2 . . ? C00M C00N C00L 119.7(4) . . ? C00M C00N H00S 120.2 . . ? C006 C00O H00T 109.5 . . ? C006 C00O H00U 109.5 . . ? C006 C00O H00V 109.5 . . ? H00T C00O H00U 109.5 . . ? H00T C00O H00V 109.5 . . ? H00U C00O H00V 109.5 . . ? C008 C00P H00W 180.0 . . ? 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 O001 C00E 1.214(4) . ? O002 C004 1.371(4) . ? O002 C00J 1.419(4) . ? C003 C00A 1.377(5) . ? C003 C00C 1.391(4) . ? C003 C00H 1.516(5) . ? C004 C00D 1.387(5) . ? C004 C00G 1.381(5) . ? C005 C006 1.577(4) . ? C005 C007 1.539(4) . ? C005 C008 1.476(4) . ? C005 C00B 1.558(4) . ? C006 C00E 1.531(4) . ? C006 C00K 1.536(5) . ? C006 C00O 1.524(5) . ? C007 C009 1.388(5) . ? C007 C00I 1.385(5) . ? C008 C00P 1.165(5) . ? C009 H009 0.9300 . ? C009 C00M 1.395(5) . ? C00A H00A 0.9300 . ? C00A C00D 1.391(5) . ? C00B H00B 0.9700 . ? C00B H00C 0.9700 . ? C00B C00F 1.529(4) . ? C00C H00D 0.9300 . ? C00C C00G 1.380(5) . ? C00D H00E 0.9300 . ? C00E C00F 1.518(4) . ? C00F H00F 0.9800 . ? C00F C00H 1.532(5) . ? C00G H00G 0.9300 . ? C00H H00H 0.9700 . ? C00H H00I 0.9700 . ? C00I H00J 0.9300 . ? C00I C00L 1.389(5) . ? C00J H00K 0.9600 . ? C00J H00L 0.9600 . ? C00J H00M 0.9600 . ? C00K H00N 0.9600 . ? C00K H00O 0.9600 . ? C00K H00P 0.9600 . ? C00L H00Q 0.9300 . ? C00L C00N 1.375(6) . ? C00M H00R 0.9300 . ? C00M C00N 1.359(6) . ? C00N H00S 0.9300 . ? C00O H00T 0.9600 . ? C00O H00U 0.9600 . ? C00O H00V 0.9600 . ? C00P H00W 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 O001 C00E C00F C00B -175.9(3) . . . . ? O001 C00E C00F C00H -49.9(5) . . . . ? O002 C004 C00D C00A -178.9(3) . . . . ? O002 C004 C00G C00C 179.1(3) . . . . ? C003 C00A C00D C004 0.1(5) . . . . ? C003 C00C C00G C004 -0.6(5) . . . . ? C005 C006 C00E O001 -159.5(3) . . . . ? C005 C006 C00E C00F 20.1(3) . . . . ? C005 C007 C009 C00M 178.6(3) . . . . ? C005 C007 C00I C00L -179.4(3) . . . . ? C005 C00B C00F C00E -28.0(3) . . . . ? C005 C00B C00F C00H -151.2(3) . . . . ? C006 C005 C007 C009 111.0(4) . . . . ? C006 C005 C007 C00I -70.6(4) . . . . ? C006 C005 C00B C00F 40.7(3) . . . . ? C006 C00E C00F C00B 4.6(4) . . . . ? C006 C00E C00F C00H 130.5(3) . . . . ? C007 C005 C006 C00E -161.0(3) . . . . ? C007 C005 C006 C00K -48.6(4) . . . . ? C007 C005 C006 C00O 78.6(4) . . . . ? C007 C005 C00B C00F 164.8(3) . . . . ? C007 C009 C00M C00N 0.4(6) . . . . ? C007 C00I C00L C00N 1.2(6) . . . . ? C008 C005 C006 C00E 77.6(3) . . . . ? C008 C005 C006 C00K -170.0(3) . . . . ? C008 C005 C006 C00O -42.8(4) . . . . ? C008 C005 C007 C009 -126.6(3) . . . . ? C008 C005 C007 C00I 51.9(4) . . . . ? C008 C005 C00B C00F -74.9(3) . . . . ? C009 C007 C00I C00L -0.9(6) . . . . ? C009 C00M C00N C00L -0.1(7) . . . . ? C00A C003 C00C C00G 2.6(5) . . . . ? C00A C003 C00H C00F 153.8(3) . . . . ? C00B C005 C006 C00E -36.2(3) . . . . ? C00B C005 C006 C00K 76.2(3) . . . . ? C00B C005 C006 C00O -156.6(3) . . . . ? C00B C005 C007 C009 -6.8(4) . . . . ? C00B C005 C007 C00I 171.7(3) . . . . ? C00B C00F C00H C003 -70.3(4) . . . . ? C00C C003 C00A C00D -2.4(5) . . . . ? C00C C003 C00H C00F -31.5(5) . . . . ? C00D C004 C00G C00C -1.8(5) . . . . ? C00E C00F C00H C003 170.8(3) . . . . ? C00G C004 C00D C00A 2.0(5) . . . . ? C00H C003 C00A C00D 172.7(3) . . . . ? C00H C003 C00C C00G -172.2(3) . . . . ? C00I C007 C009 C00M 0.1(5) . . . . ? C00I C00L C00N C00M -0.7(7) . . . . ? C00J O002 C004 C00D 3.3(5) . . . . ? C00J O002 C004 C00G -177.6(3) . . . . ? C00K C006 C00E O001 84.1(4) . . . . ? C00K C006 C00E C00F -96.3(3) . . . . ? C00O C006 C00E O001 -35.0(5) . . . . ? C00O C006 C00E C00F 144.6(3) . . . . ?