#------------------------------------------------------------------------------ #$Date: 2022-06-22 09:23:47 +0300 (Wed, 22 Jun 2022) $ #$Revision: 276143 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/43/1564313.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_1564313 loop_ _publ_author_name 'Zhu, Haiqian' 'Zheng, Hanliang' 'Zhang, Junhua' 'Feng, Jian' 'Kong, Lichun' 'Zhang, Fang' 'Xue, Xiao-Song' 'Zhu, Gangguo' _publ_section_title ; Solvent-controlled photocatalytic divergent cyclization of alkynyl aldehydes: access to cyclopentenones and dihydropyranols ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D1SC03416B _journal_year 2021 _chemical_formula_moiety 'C21 H19 N O3 S' _chemical_formula_sum 'C21 H19 N O3 S' _chemical_formula_weight 365.44 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2021-01-22 _audit_creation_method ; Olex2 1.2 (compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221) ; _audit_update_record ; 2021-02-03 deposited with the CCDC. 2021-07-26 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 91.831(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.8167(2) _cell_length_b 17.2043(6) _cell_length_c 19.0214(8) _cell_measurement_reflns_used 9554 _cell_measurement_temperature 250(2) _cell_measurement_theta_max 27.46 _cell_measurement_theta_min 3.43 _cell_volume 1902.54(12) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_temperature 250.0 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_unetI/netI 0.0195 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 19469 _diffrn_reflns_point_group_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.982 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.481 _diffrn_reflns_theta_min 2.368 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.6907 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0756 before and 0.0429 after correction. The Ratio of minimum to maximum transmission is 0.9264. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.276 _exptl_crystal_description block _exptl_crystal_F_000 768 _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _refine_diff_density_max 0.311 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.097 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.115 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 238 _refine_ls_number_reflns 4289 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.115 _refine_ls_R_factor_all 0.0565 _refine_ls_R_factor_gt 0.0456 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+0.3573P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1414 _refine_ls_wR_factor_ref 0.1580 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3717 _reflns_number_total 4289 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL a_a.res in P2(1)/n a_a.res created by SHELXL-2017/1 at 10:36:33 on 22-Jan-2021 REM Old TITL a in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.177, Rweak 0.010, Alpha 0.056, Orientation as input REM Formula found by SHELXT: C21 N O3 S CELL 0.71073 5.8167 17.2043 19.0214 90 91.831 90 ZERR 16 0.0002 0.0006 0.0008 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O S UNIT 84 76 4 12 4 L.S. 10 PLAN 20 TEMP -23.15 BOND $H LIST 6 MORE -1 CONF fmap 2 acta 52 REM REM REM WGHT 0.089900 0.357300 FVAR 1.83767 S001 5 0.735859 0.304893 0.804851 11.00000 0.05068 0.04913 = 0.05257 -0.00890 0.00861 -0.00973 O002 4 0.735225 0.362979 0.751122 11.00000 0.09389 0.05514 = 0.05954 -0.00187 0.02067 -0.02755 O003 4 0.949639 0.270216 0.827769 11.00000 0.04469 0.08477 = 0.08688 -0.02550 0.00344 -0.00055 C004 1 0.552629 0.227986 0.777768 11.00000 0.04665 0.03780 = 0.04286 -0.00079 0.00624 -0.00191 N005 3 0.241173 0.475511 0.443939 11.00000 0.09142 0.06606 = 0.05612 0.01400 -0.00720 0.00312 C006 1 0.595962 0.341546 0.878546 11.00000 0.05169 0.04333 = 0.04646 -0.00544 0.00003 0.00045 C007 1 0.424229 0.224661 0.718400 11.00000 0.04674 0.04117 = 0.04545 0.00367 0.00302 -0.00403 C008 1 0.525528 0.159480 0.825765 11.00000 0.06789 0.04703 = 0.04555 0.00631 -0.00203 -0.00447 AFIX 23 H00A 2 0.449926 0.174845 0.868928 11.00000 -1.20000 H00B 2 0.675320 0.136422 0.838336 11.00000 -1.20000 AFIX 0 C009 1 0.393068 0.279404 0.658904 11.00000 0.04829 0.04006 = 0.04240 0.00214 0.00171 -0.00356 C00A 1 0.375854 0.102357 0.782956 11.00000 0.05592 0.04063 = 0.05686 0.00797 0.00097 -0.00622 O00B 4 0.132244 0.134040 0.680553 11.00000 0.13792 0.09739 = 0.09506 0.03712 -0.06149 -0.06623 C00C 1 0.316929 0.379425 0.546370 11.00000 0.05951 0.04012 = 0.04172 0.00080 -0.00252 -0.00438 C00D 1 0.554826 0.286164 0.607259 11.00000 0.04942 0.06018 = 0.05660 0.01246 0.00918 0.00773 AFIX 43 H00D 2 0.690722 0.256637 0.610511 11.00000 -1.20000 AFIX 0 C00E 1 0.276708 0.432976 0.488936 11.00000 0.06789 0.04950 = 0.04754 0.00206 -0.00486 -0.00180 C00F 1 0.192156 0.322442 0.652963 11.00000 0.05471 0.05990 = 0.05463 0.00968 0.01457 0.00927 AFIX 43 H00F 2 0.080215 0.317385 0.687234 11.00000 -1.20000 AFIX 0 C00G 1 0.361289 0.397075 0.992921 11.00000 0.06494 0.06297 = 0.05452 -0.00948 0.00398 0.00664 C00H 1 0.154678 0.372793 0.597075 11.00000 0.05542 0.05146 = 0.06055 0.00718 0.00500 0.01032 AFIX 43 H00H 2 0.018871 0.402361 0.593758 11.00000 -1.20000 AFIX 0 C00I 1 0.287640 0.150809 0.721134 11.00000 0.07257 0.05152 = 0.05662 0.00991 -0.01208 -0.01980 C00J 1 0.517822 0.335872 0.551175 11.00000 0.05874 0.06491 = 0.05125 0.01169 0.01324 0.00335 AFIX 43 H00J 2 0.628119 0.340262 0.516337 11.00000 -1.20000 AFIX 0 C00K 1 0.664878 0.320127 0.945314 11.00000 0.06331 0.06478 = 0.05322 -0.00085 -0.00353 0.01811 AFIX 43 H00K 2 0.790876 0.286511 0.952431 11.00000 -1.20000 AFIX 0 C00L 1 0.409496 0.390011 0.867364 11.00000 0.08419 0.08206 = 0.04926 -0.00202 -0.00613 0.03400 AFIX 43 H00L 2 0.361433 0.404123 0.821470 11.00000 -1.20000 AFIX 0 C00M 1 0.178224 0.069950 0.824497 11.00000 0.06128 0.07463 = 0.09713 0.03492 0.00883 -0.00503 AFIX 137 H00C 2 0.239338 0.040643 0.864451 11.00000 -1.50000 H00E 2 0.084714 0.036093 0.794499 11.00000 -1.50000 H00G 2 0.084621 0.112452 0.841026 11.00000 -1.50000 AFIX 0 C00N 1 0.523399 0.036813 0.754115 11.00000 0.08725 0.05950 = 0.08234 -0.01405 0.00406 0.00081 AFIX 137 H00M 2 0.651368 0.058868 0.729427 11.00000 -1.50000 H00N 2 0.430728 0.005177 0.721913 11.00000 -1.50000 H00I 2 0.581676 0.004826 0.792713 11.00000 -1.50000 AFIX 0 C00O 1 0.548288 0.348179 1.002083 11.00000 0.07656 0.07318 = 0.04496 0.00004 -0.00232 0.01419 AFIX 43 H00O 2 0.597036 0.333744 1.047833 11.00000 -1.20000 AFIX 0 C00P 1 0.233428 0.427182 1.054687 11.00000 0.08750 0.10123 = 0.06743 -0.01711 0.01630 0.01781 AFIX 137 H00P 2 0.301485 0.406065 1.097814 11.00000 -1.50000 H00Q 2 0.073477 0.411456 1.050261 11.00000 -1.50000 H00R 2 0.242778 0.483462 1.055862 11.00000 -1.50000 AFIX 0 C00Q 1 0.294587 0.417458 0.924738 11.00000 0.08414 0.09543 = 0.06381 -0.00761 -0.00422 0.04415 AFIX 43 H00S 2 0.168024 0.450782 0.917392 11.00000 -1.20000 AFIX 0 HKLF 4 REM a_a.res in P2(1)/n REM R1 = 0.0456 for 3717 Fo > 4sig(Fo) and 0.0565 for all 4289 data REM 238 parameters refined using 0 restraints END WGHT 0.0899 0.3573 REM Highest difference peak 0.311, deepest hole -0.371, 1-sigma level 0.097 Q1 1 0.2749 0.1162 0.6619 11.00000 0.05 0.31 Q2 1 0.4502 0.0749 0.7732 11.00000 0.05 0.30 Q3 1 0.3153 0.1204 0.7566 11.00000 0.05 0.28 Q4 1 0.4361 0.1225 0.8043 11.00000 0.05 0.27 Q5 1 0.1166 0.4677 1.0422 11.00000 0.05 0.27 Q6 1 0.4808 0.0373 0.7163 11.00000 0.05 0.27 Q7 1 0.3033 0.0820 0.8005 11.00000 0.05 0.25 Q8 1 0.5550 0.0275 0.6990 11.00000 0.05 0.25 Q9 1 0.3933 0.0006 0.7463 11.00000 0.05 0.24 Q10 1 0.5813 0.0456 0.8607 11.00000 0.05 0.23 Q11 1 0.0109 0.5018 0.4748 11.00000 0.05 0.22 Q12 1 0.4779 0.0309 0.8751 11.00000 0.05 0.22 Q13 1 0.2627 0.4985 0.9252 11.00000 0.05 0.22 Q14 1 0.5163 0.0038 0.7623 11.00000 0.05 0.22 Q15 1 0.1120 0.5068 1.1049 11.00000 0.05 0.21 Q16 1 0.1150 0.4552 0.4562 11.00000 0.05 0.21 Q17 1 0.1097 0.1442 0.6988 11.00000 0.05 0.21 Q18 1 0.0169 0.5063 0.9343 11.00000 0.05 0.20 Q19 1 0.3858 0.4562 1.0951 11.00000 0.05 0.20 Q20 1 0.6607 0.0165 0.8048 11.00000 0.05 0.20 REM The information below was added by Olex2. REM REM R1 = 0.0456 for 3717 Fo > 4sig(Fo) and 0.0565 for all 19771 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.31, deepest hole -0.37 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0565 REM R1_gt = 0.0456 REM wR_ref = n/a REM GOOF = n/a REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 19771 REM Reflections_gt = 3717 REM Parameters = n/a REM Hole = -0.37 REM Peak = 0.31 REM Flack = n/a ; _cod_data_source_file d1sc03416b2.cif _cod_data_source_block a_a _cod_depositor_comments ; 2022-06-10 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C5.25 H4.75 N0.25 O0.75 S0.25' _cod_original_formula_weight 91.36 _cod_original_formula_moiety '0.25(C21 H19 N O3 S)' _cod_original_formula_units_Z 16 _cod_database_code 1564313 _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 Secondary CH2 refined with riding coordinates: C008(H00A,H00B) 2.b Aromatic/amide H refined with riding coordinates: C00D(H00D), C00F(H00F), C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L), C00O(H00O), C00Q(H00S) 2.c Idealised Me refined as rotating group: C00M(H00C,H00E,H00G), C00N(H00M,H00N,H00I), C00P(H00P,H00Q,H00R) ; _shelx_shelxl_version_number 2017/1 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 S001 S 0.73586(7) 0.30489(2) 0.80485(2) 0.05064(17) Uani 1 1 d . . . . . O002 O 0.7352(3) 0.36298(8) 0.75112(7) 0.0691(4) Uani 1 1 d . . . . . O003 O 0.9496(2) 0.27022(10) 0.82777(9) 0.0721(4) Uani 1 1 d . . . . . C004 C 0.5526(3) 0.22799(8) 0.77777(8) 0.0423(3) Uani 1 1 d . . . . . N005 N 0.2412(4) 0.47551(11) 0.44394(9) 0.0714(5) Uani 1 1 d . . . . . C006 C 0.5960(3) 0.34155(9) 0.87855(9) 0.0472(4) Uani 1 1 d . . . . . C007 C 0.4242(3) 0.22466(9) 0.71840(8) 0.0444(3) Uani 1 1 d . . . . . C008 C 0.5255(3) 0.15948(10) 0.82576(9) 0.0536(4) Uani 1 1 d . . . . . H00A H 0.449926 0.174845 0.868928 0.064 Uiso 1 1 calc R . . . . H00B H 0.675320 0.136422 0.838336 0.064 Uiso 1 1 calc R . . . . C009 C 0.3931(3) 0.27940(9) 0.65890(8) 0.0436(3) Uani 1 1 d . . . . . C00A C 0.3759(3) 0.10236(9) 0.78296(10) 0.0512(4) Uani 1 1 d . . . . . O00B O 0.1322(4) 0.13404(12) 0.68055(10) 0.1115(8) Uani 1 1 d . . . . . C00C C 0.3169(3) 0.37943(9) 0.54637(8) 0.0472(4) Uani 1 1 d . . . . . C00D C 0.5548(3) 0.28616(11) 0.60726(10) 0.0552(4) Uani 1 1 d . . . . . H00D H 0.690722 0.256637 0.610511 0.066 Uiso 1 1 calc R . . . . C00E C 0.2767(3) 0.43298(10) 0.48894(9) 0.0551(4) Uani 1 1 d . . . . . C00F C 0.1922(3) 0.32244(11) 0.65296(10) 0.0561(4) Uani 1 1 d . . . . . H00F H 0.080215 0.317385 0.687234 0.067 Uiso 1 1 calc R . . . . C00G C 0.3613(3) 0.39708(12) 0.99292(10) 0.0608(5) Uani 1 1 d . . . . . C00H C 0.1547(3) 0.37279(11) 0.59708(10) 0.0557(4) Uani 1 1 d . . . . . H00H H 0.018871 0.402361 0.593758 0.067 Uiso 1 1 calc R . . . . C00I C 0.2876(4) 0.15081(11) 0.72113(10) 0.0605(5) Uani 1 1 d . . . . . C00J C 0.5178(3) 0.33587(12) 0.55117(10) 0.0581(4) Uani 1 1 d . . . . . H00J H 0.628119 0.340262 0.516337 0.070 Uiso 1 1 calc R . . . . C00K C 0.6649(3) 0.32013(12) 0.94531(10) 0.0605(5) Uani 1 1 d . . . . . H00K H 0.790876 0.286511 0.952431 0.073 Uiso 1 1 calc R . . . . C00L C 0.4095(4) 0.39001(14) 0.86736(11) 0.0720(6) Uani 1 1 d . . . . . H00L H 0.361433 0.404123 0.821470 0.086 Uiso 1 1 calc R . . . . C00M C 0.1782(4) 0.06995(14) 0.82450(14) 0.0775(7) Uani 1 1 d . . . . . H00C H 0.239338 0.040643 0.864451 0.116 Uiso 1 1 calc GR . . . . H00E H 0.084714 0.036093 0.794499 0.116 Uiso 1 1 calc GR . . . . H00G H 0.084621 0.112452 0.841026 0.116 Uiso 1 1 calc GR . . . . C00N C 0.5234(4) 0.03681(13) 0.75411(13) 0.0763(6) Uani 1 1 d . . . . . H00M H 0.651368 0.058868 0.729427 0.114 Uiso 1 1 calc GR . . . . H00N H 0.430728 0.005177 0.721913 0.114 Uiso 1 1 calc GR . . . . H00I H 0.581676 0.004826 0.792713 0.114 Uiso 1 1 calc GR . . . . C00O C 0.5483(4) 0.34818(13) 1.00208(10) 0.0650(5) Uani 1 1 d . . . . . H00O H 0.597036 0.333744 1.047833 0.078 Uiso 1 1 calc R . . . . C00P C 0.2334(5) 0.42718(18) 1.05469(13) 0.0851(7) Uani 1 1 d . . . . . H00P H 0.301485 0.406065 1.097814 0.128 Uiso 1 1 calc GR . . . . H00Q H 0.073477 0.411456 1.050261 0.128 Uiso 1 1 calc GR . . . . H00R H 0.242778 0.483462 1.055862 0.128 Uiso 1 1 calc GR . . . . C00Q C 0.2946(4) 0.41746(16) 0.92474(12) 0.0813(7) Uani 1 1 d . . . . . H00S H 0.168024 0.450782 0.917392 0.098 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S001 0.0507(3) 0.0491(3) 0.0526(3) -0.00890(16) 0.00861(18) -0.00973(16) O002 0.0939(10) 0.0551(7) 0.0595(8) -0.0019(6) 0.0207(7) -0.0276(7) O003 0.0447(7) 0.0848(10) 0.0869(10) -0.0255(8) 0.0034(6) -0.0006(6) C004 0.0466(8) 0.0378(7) 0.0429(8) -0.0008(6) 0.0062(6) -0.0019(6) N005 0.0914(13) 0.0661(10) 0.0561(9) 0.0140(8) -0.0072(9) 0.0031(9) C006 0.0517(8) 0.0433(8) 0.0465(8) -0.0054(6) 0.0000(6) 0.0005(6) C007 0.0467(8) 0.0412(7) 0.0455(8) 0.0037(6) 0.0030(6) -0.0040(6) C008 0.0679(10) 0.0470(9) 0.0455(9) 0.0063(7) -0.0020(7) -0.0045(7) C009 0.0483(8) 0.0401(7) 0.0424(8) 0.0021(6) 0.0017(6) -0.0036(6) C00A 0.0559(9) 0.0406(8) 0.0569(9) 0.0080(7) 0.0010(7) -0.0062(7) O00B 0.1379(17) 0.0974(13) 0.0951(13) 0.0371(10) -0.0615(12) -0.0662(12) C00C 0.0595(9) 0.0401(7) 0.0417(8) 0.0008(6) -0.0025(7) -0.0044(6) C00D 0.0494(9) 0.0602(10) 0.0566(10) 0.0125(8) 0.0092(7) 0.0077(7) C00E 0.0679(10) 0.0495(9) 0.0475(9) 0.0021(7) -0.0049(8) -0.0018(8) C00F 0.0547(9) 0.0599(10) 0.0546(10) 0.0097(8) 0.0146(8) 0.0093(8) C00G 0.0649(11) 0.0630(11) 0.0545(10) -0.0095(8) 0.0040(8) 0.0066(9) C00H 0.0554(9) 0.0515(9) 0.0605(10) 0.0072(8) 0.0050(8) 0.0103(7) C00I 0.0726(11) 0.0515(9) 0.0566(10) 0.0099(8) -0.0121(9) -0.0198(8) C00J 0.0587(10) 0.0649(11) 0.0513(9) 0.0117(8) 0.0132(8) 0.0034(8) C00K 0.0633(11) 0.0648(11) 0.0532(10) -0.0008(8) -0.0035(8) 0.0181(9) C00L 0.0842(14) 0.0821(14) 0.0493(10) -0.0020(9) -0.0061(9) 0.0340(11) C00M 0.0613(11) 0.0746(13) 0.0971(16) 0.0349(13) 0.0088(11) -0.0050(10) C00N 0.0872(15) 0.0595(12) 0.0823(15) -0.0140(11) 0.0041(12) 0.0008(10) C00O 0.0766(12) 0.0732(12) 0.0450(9) 0.0000(8) -0.0023(8) 0.0142(10) C00P 0.0875(16) 0.1012(19) 0.0674(13) -0.0171(13) 0.0163(11) 0.0178(14) C00Q 0.0841(15) 0.0954(17) 0.0638(12) -0.0076(12) -0.0042(11) 0.0441(13) 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' N N 0.0061 0.0033 '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' S S 0.1246 0.1234 '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 O002 S001 O003 119.37(10) . . ? O002 S001 C004 109.12(8) . . ? O002 S001 C006 109.16(8) . . ? O003 S001 C004 106.64(8) . . ? O003 S001 C006 108.99(9) . . ? C006 S001 C004 102.17(8) . . ? C007 C004 S001 126.52(12) . . ? C007 C004 C008 114.44(14) . . ? C008 C004 S001 119.00(12) . . ? C00K C006 S001 120.86(13) . . ? C00K C006 C00L 120.73(17) . . ? C00L C006 S001 118.37(14) . . ? C004 C007 C009 132.18(14) . . ? C004 C007 C00I 106.83(14) . . ? C009 C007 C00I 120.91(14) . . ? C004 C008 H00A 110.9 . . ? C004 C008 H00B 110.9 . . ? C004 C008 C00A 104.44(13) . . ? H00A C008 H00B 108.9 . . ? C00A C008 H00A 110.9 . . ? C00A C008 H00B 110.9 . . ? C00D C009 C007 121.74(15) . . ? C00F C009 C007 119.03(15) . . ? C00F C009 C00D 119.16(15) . . ? C00I C00A C008 103.42(13) . . ? C00I C00A C00M 111.19(16) . . ? C00I C00A C00N 107.87(17) . . ? C00M C00A C008 112.67(17) . . ? C00M C00A C00N 110.98(17) . . ? C00N C00A C008 110.37(16) . . ? C00H C00C C00E 119.06(16) . . ? C00H C00C C00J 120.25(15) . . ? C00J C00C C00E 120.68(16) . . ? C009 C00D H00D 119.8 . . ? C00J C00D C009 120.49(16) . . ? C00J C00D H00D 119.8 . . ? N005 C00E C00C 178.8(2) . . ? C009 C00F H00F 119.7 . . ? C00H C00F C009 120.62(16) . . ? C00H C00F H00F 119.7 . . ? C00O C00G C00P 121.24(19) . . ? C00O C00G C00Q 117.87(18) . . ? C00Q C00G C00P 120.9(2) . . ? C00C C00H C00F 119.74(16) . . ? C00C C00H H00H 120.1 . . ? C00F C00H H00H 120.1 . . ? C007 C00I C00A 109.01(14) . . ? O00B C00I C007 124.60(17) . . ? O00B C00I C00A 126.38(17) . . ? C00C C00J H00J 120.1 . . ? C00D C00J C00C 119.72(16) . . ? C00D C00J H00J 120.1 . . ? C006 C00K H00K 120.2 . . ? C006 C00K C00O 119.64(17) . . ? C00O C00K H00K 120.2 . . ? C006 C00L H00L 120.6 . . ? C006 C00L C00Q 118.88(18) . . ? C00Q C00L H00L 120.6 . . ? C00A C00M H00C 109.5 . . ? C00A C00M H00E 109.5 . . ? C00A C00M H00G 109.5 . . ? H00C C00M H00E 109.5 . . ? H00C C00M H00G 109.5 . . ? H00E C00M H00G 109.5 . . ? C00A C00N H00M 109.5 . . ? C00A C00N H00N 109.5 . . ? C00A C00N H00I 109.5 . . ? H00M C00N H00N 109.5 . . ? H00M C00N H00I 109.5 . . ? H00N C00N H00I 109.5 . . ? C00G C00O H00O 119.4 . . ? C00K C00O C00G 121.24(18) . . ? C00K C00O H00O 119.4 . . ? C00G C00P H00P 109.5 . . ? C00G C00P H00Q 109.5 . . ? C00G C00P H00R 109.5 . . ? H00P C00P H00Q 109.5 . . ? H00P C00P H00R 109.5 . . ? H00Q C00P H00R 109.5 . . ? C00G C00Q H00S 119.2 . . ? C00L C00Q C00G 121.64(19) . . ? C00L C00Q H00S 119.2 . . ? 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 S001 O002 1.4293(15) . ? S001 O003 1.4344(15) . ? S001 C004 1.7655(16) . ? S001 C006 1.7600(17) . ? C004 C007 1.335(2) . ? C004 C008 1.502(2) . ? N005 C00E 1.140(2) . ? C006 C00K 1.370(2) . ? C006 C00L 1.379(3) . ? C007 C009 1.479(2) . ? C007 C00I 1.500(2) . ? C008 H00A 0.9800 . ? C008 H00B 0.9800 . ? C008 C00A 1.530(2) . ? C009 C00D 1.387(2) . ? C009 C00F 1.385(2) . ? C00A C00I 1.517(2) . ? C00A C00M 1.521(3) . ? C00A C00N 1.529(3) . ? O00B C00I 1.205(2) . ? C00C C00E 1.442(2) . ? C00C C00H 1.376(3) . ? C00C C00J 1.389(3) . ? C00D H00D 0.9400 . ? C00D C00J 1.379(2) . ? C00F H00F 0.9400 . ? C00F C00H 1.383(2) . ? C00G C00O 1.382(3) . ? C00G C00P 1.503(3) . ? C00G C00Q 1.387(3) . ? C00H H00H 0.9400 . ? C00J H00J 0.9400 . ? C00K H00K 0.9400 . ? C00K C00O 1.380(3) . ? C00L H00L 0.9400 . ? C00L C00Q 1.381(3) . ? C00M H00C 0.9700 . ? C00M H00E 0.9700 . ? C00M H00G 0.9700 . ? C00N H00M 0.9700 . ? C00N H00N 0.9700 . ? C00N H00I 0.9700 . ? C00O H00O 0.9400 . ? C00P H00P 0.9700 . ? C00P H00Q 0.9700 . ? C00P H00R 0.9700 . ? C00Q H00S 0.9400 . ? 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 S001 C004 C007 C009 0.4(3) . . . . ? S001 C004 C007 C00I -176.39(13) . . . . ? S001 C004 C008 C00A -174.85(12) . . . . ? S001 C006 C00K C00O -178.32(17) . . . . ? S001 C006 C00L C00Q 178.3(2) . . . . ? O002 S001 C004 C007 -2.78(18) . . . . ? O002 S001 C004 C008 179.81(13) . . . . ? O002 S001 C006 C00K -146.55(16) . . . . ? O002 S001 C006 C00L 35.93(19) . . . . ? O003 S001 C004 C007 -132.98(15) . . . . ? O003 S001 C004 C008 49.61(15) . . . . ? O003 S001 C006 C00K -14.58(19) . . . . ? O003 S001 C006 C00L 167.90(17) . . . . ? C004 S001 C006 C00K 98.00(17) . . . . ? C004 S001 C006 C00L -79.52(18) . . . . ? C004 C007 C009 C00D 77.9(2) . . . . ? C004 C007 C009 C00F -105.0(2) . . . . ? C004 C007 C00I C00A -9.5(2) . . . . ? C004 C007 C00I O00B 169.9(2) . . . . ? C004 C008 C00A C00I -12.26(19) . . . . ? C004 C008 C00A C00M -132.42(16) . . . . ? C004 C008 C00A C00N 102.90(18) . . . . ? C006 S001 C004 C007 112.70(15) . . . . ? C006 S001 C004 C008 -64.71(14) . . . . ? C006 C00K C00O C00G 0.6(3) . . . . ? C006 C00L C00Q C00G -0.4(4) . . . . ? C007 C004 C008 C00A 7.4(2) . . . . ? C007 C009 C00D C00J 177.91(17) . . . . ? C007 C009 C00F C00H -178.42(17) . . . . ? C008 C004 C007 C009 177.86(17) . . . . ? C008 C004 C007 C00I 1.1(2) . . . . ? C008 C00A C00I C007 13.6(2) . . . . ? C008 C00A C00I O00B -165.9(3) . . . . ? C009 C007 C00I C00A 173.29(15) . . . . ? C009 C007 C00I O00B -7.2(3) . . . . ? C009 C00D C00J C00C -0.1(3) . . . . ? C009 C00F C00H C00C 0.9(3) . . . . ? C00D C009 C00F C00H -1.3(3) . . . . ? C00E C00C C00H C00F -179.16(17) . . . . ? C00E C00C C00J C00D 178.72(18) . . . . ? C00F C009 C00D C00J 0.9(3) . . . . ? C00H C00C C00J C00D -0.4(3) . . . . ? C00I C007 C009 C00D -105.7(2) . . . . ? C00I C007 C009 C00F 71.3(2) . . . . ? C00J C00C C00H C00F -0.1(3) . . . . ? C00K C006 C00L C00Q 0.8(4) . . . . ? C00L C006 C00K C00O -0.9(3) . . . . ? C00M C00A C00I C007 134.73(19) . . . . ? C00M C00A C00I O00B -44.7(3) . . . . ? C00N C00A C00I C007 -103.38(18) . . . . ? C00N C00A C00I O00B 77.2(3) . . . . ? C00O C00G C00Q C00L 0.2(4) . . . . ? C00P C00G C00O C00K 179.6(2) . . . . ? C00P C00G C00Q C00L -179.7(3) . . . . ? C00Q C00G C00O C00K -0.3(4) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -1 0 0 -0.4 0.8 1 0 0 -0.1 0.9 -1 0 0 0.5 0.6 3 0 0 18.8 4.3 4 0 0 1845.42 47.4 -4 0 0 1891.11 41.8 -5 0 0 6.9 4.2 5 0 0 1.5 4.7 6 0 0 488.25 24.3 -6 0 0 464.05 18.4 7 0 0 -0.7 4.9 -7 0 0 -1.5 3.8 1 1 0 0.3 0.1 -2 -1 0 2661.23 52.29 2 -1 0 2661.63 51.69 -2 -1 0 2653.93 55.09 2 -1 0 2665.53 56.29 -2 1 0 2597.44 52.69 2 1 0 2560.04 55.19 3 -1 0 2857.71 55.99 -3 -1 0 2898.71 58.19 3 -1 0 2845.32 63.49 3 1 0 2820.52 62.59 -3 1 0 2837.82 58.59 -4 -1 0 207.78 9 4 -1 0 206.08 12.3 4 1 0 204.68 11.9 -4 1 0 213.18 9.3 5 -1 0 14.1 6.3 -5 -1 0 25 5 -5 1 0 21.4 4.8 5 1 0 30.2 7.3 6 -1 0 313.17 19.8 -6 -1 0 311.87 14.8 6 1 0 293.47 21.2 -6 1 0 329.37 15.1 7 -1 0 28.7 8.5 -7 -1 0 31.4 6.5 7 1 0 29.5 8.9 -7 1 0 29.7 7 0 -2 0 0.1 0.3 1 -2 0 2033.5 43.5 1 -2 0 2112.59 41.7 -1 -2 0 2077.99 41.3 -1 -2 0 2127.59 41.7 -1 2 0 2085.19 41.8 1 2 0 2186.38 42 1 2 0 2077.29 40.6 1 2 0 2084.19 40.8 3 -2 0 19.2 3.9 3 -2 0 23.4 2.5 -3 -2 0 28.9 3.3 -3 2 0 19 3 3 2 0 29 5.4 4 -2 0 187.98 11.9 -4 -2 0 170.98 8.2 -4 2 0 174.08 8.7 4 2 0 162.48 10.5 5 -2 0 614.24 25.4 -5 -2 0 614.94 19.4 5 2 0 585.34 23.7 -5 2 0 636.24 20.2 -6 -2 0 462.05 20.1 6 -2 0 402.66 23 6 2 0 453.25 23 -6 2 0 422.86 17.9 7 -2 0 55.59 11.9 -7 -2 0 61.19 8.2 7 2 0 59.39 10.8 -7 2 0 50.69 8.2 0 -3 0 1.5 1 0 -3 0 0.8 0.8 0 3 0 1.9 0.9 0 3 0 2 0.9 2 -3 0 10.4 2.7 -2 -3 0 19.3 2.8 2 -3 0 14.2 2.2 -2 3 0 14.5 2.5 2 3 0 16.6 1.4 2 3 0 19.2 1.4 2 3 0 16.1 2.6 -3 -3 0 133.19 6.2 3 -3 0 144.79 5.8 -3 -3 0 140.59 7.6 3 3 0 136.79 7.9 -3 3 0 134.39 6.7 4 -3 0 566.54 22 4 -3 0 575.44 14.5 -4 -3 0 592.74 17 -4 3 0 577.84 17.8 4 3 0 591.04 20.6 5 -3 0 2.3 4.9 -5 -3 0 5.6 3.6 -5 3 0 4.1 4 5 3 0 -0.3 3.8 6 -3 0 12.9 7.2 -6 -3 0 5.3 7.4 6 3 0 18 6.8 -6 3 0 14.2 5.2 7 -3 0 4.4 6 -7 -3 0 8 4.8 7 3 0 6.3 6.1 -7 3 0 28.1 6.6 3 -4 0 1944.91 48.8 3 -4 0 1902.91 42.5 -3 -4 0 1995.3 43.2 -3 -4 0 2024.2 45 3 4 0 2289.87 46.9 -3 4 0 2002.7 44.4 4 -4 0 711.83 25.6 4 -4 0 730.33 18.1 -4 -4 0 747.63 20.2 -4 4 0 724.53 21.3 5 -4 0 2266.87 60.59 -5 -4 0 2344.57 51.79 5 4 0 2184.38 56.59 -6 -4 0 275.37 15.6 6 -4 0 261.77 19 -6 4 0 300.97 15.2 6 4 0 283.07 17.4 7 -4 0 64.09 12.3 -7 -4 0 75.89 9.1 7 4 0 93.19 13 -7 4 0 85.39 10.2 0 5 0 38.2 3.1 -1 -5 0 3172.58 63.49 1 -5 0 3168.78 63.79 -1 -5 0 3162.38 62.99 1 5 0 3157.58 63.09 1 5 0 3128.19 62.39 -1 5 0 3146.89 63.79 -1 5 0 3116.89 63.79 -3 -5 0 25.6 3.8 -3 -5 0 30.6 3.8 3 -5 0 22.9 4.8 -3 5 0 21.3 3.8 3 5 0 20.4 3.6 4 -5 0 365.76 17.5 -4 -5 0 344.47 12.5 -4 5 0 339.07 13.5 4 5 0 325.67 14.3 -5 -5 0 28.2 5 5 -5 0 29.6 8.5 5 5 0 36.5 7 -5 5 0 35.9 6.2 -6 -5 0 8.6 4.2 6 -5 0 4.6 5.8 -6 5 0 10.8 5 6 5 0 -1.7 4.5 -7 -5 0 0.5 4 7 -5 0 1.6 5.3 -7 5 0 5.5 4.4 7 5 0 -3.7 4.5 0 -6 0 1649.54 35.2 0 -6 0 1600.24 34.9 0 6 0 1619.24 34.8 0 6 0 1594.84 35.1 1 -6 0 115.69 5.9 -1 -6 0 123.29 6 -1 -6 0 123.89 5.7 -1 6 0 118.39 6.1 1 6 0 120.69 5.8 1 6 0 121.69 5.4 -1 6 0 129.99 6.3 2 -6 0 185.68 7.9 -2 -6 0 165.28 6.2 2 -6 0 174.58 9.5 -2 -6 0 185.98 7.7 -2 6 0 169.58 8.1 2 6 0 178.28 6.1 2 6 0 187.38 6.6 -2 6 0 177.28 8 -3 -6 0 31.8 3.9 3 -6 0 32.3 3.9 3 -6 0 24.2 4.7 -3 -6 0 29.9 3.9 -3 6 0 32.4 4.4 3 6 0 32.5 4.3 -4 -6 0 861.51 23.8 4 -6 0 900.21 30.3 4 -6 0 897.51 22.8 4 6 0 929.81 26.5 -4 6 0 867.01 25.2 -5 -6 0 134.99 8.9 5 -6 0 114.59 12.3 -5 6 0 130.79 10 5 6 0 132.89 10.6 6 -6 0 0 5.5 -6 -6 0 3.6 3.6 6 6 0 8.9 5.2 -6 6 0 7.1 4.6 -7 -6 0 -5.2 3.5 7 -6 0 -5.9 9.1 7 6 0 -3.3 4.5 -7 6 0 -5.8 4 0 7 0 47.1 4 1 -7 0 1716.23 38.2 1 -7 0 1703.93 38.4 -1 -7 0 1753.92 38.3 -1 -7 0 1699.73 37.8 1 7 0 1742.63 37.1 -1 7 0 1709.53 38.5 1 7 0 1728.13 37.8 -1 7 0 1800.02 38.7 3 -7 0 1318.77 36.8 3 -7 0 1322.77 31.6 -3 -7 0 1342.77 30.3 -3 -7 0 1356.66 31.7 3 7 0 1282.17 26.3 3 7 0 1317.47 26.5 -3 7 0 1283.07 32.7 -4 -7 0 4.2 3.1 4 -7 0 2.4 4.3 4 -7 0 6.3 2.9 4 7 0 7.3 3.2 5 -7 0 304.27 18.9 -5 -7 0 319.27 13.8 5 7 0 348.57 16.1 -5 7 0 322.47 15.5 6 -7 0 101.19 13.3 -6 -7 0 82.59 8.4 6 7 0 101.19 10.4 -6 7 0 71.69 9.3 -7 -7 0 7.2 4.2 7 -7 0 4.9 7.3 7 7 0 4 5 -7 7 0 -3.1 4.7 0 -8 0 30.9 3.8 0 -8 0 42.1 4.2 0 8 0 33.9 4.1 0 8 0 37.2 4 -1 -8 0 787.72 20.6 1 -8 0 790.92 20.9 1 -8 0 782.22 21 -1 -8 0 789.62 20.8 1 -8 0 795.62 21.8 1 8 0 800.22 20.6 -1 8 0 789.82 21.1 -1 8 0 789.42 21.2 1 8 0 786.22 19.8 2 -8 0 2459.65 57.39 2 -8 0 2513.15 54.39 -2 -8 0 2522.95 54.09 -2 -8 0 2484.75 49.9 -2 8 0 2577.84 55.09 2 8 0 2460.75 51.39 -2 8 0 2500.25 54.89 2 8 0 2502.75 52.39 -3 -8 0 155.68 6.7 -3 -8 0 143.19 8.1 3 -8 0 170.88 11.3 3 -8 0 168.88 8.5 -3 8 0 160.08 9.3 3 8 0 157.28 5.5 -3 8 0 162.98 9 4 -8 0 1675.93 48.2 -4 -8 0 1753.22 41.3 4 -8 0 1750.12 40.5 -4 8 0 1704.53 43 -5 -8 0 99.19 8.4 5 -8 0 99.59 11.8 -5 8 0 107.99 10 -6 -8 0 48.8 7.2 6 -8 0 55.79 11.2 -6 8 0 56.49 8.5 7 -8 0 3.1 6.4 -7 -8 0 -4.5 3.7 0 -9 0 2.6 2.3 0 -9 0 3.2 2.1 0 9 0 7.7 2.5 0 9 0 2.6 2.2 1 -9 0 1100.69 27.9 -1 -9 0 1129.79 28.1 1 -9 0 1121.69 28.3 -1 -9 0 1107.29 27.7 1 -9 0 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13.7 -6 4 9 204.08 15.4 5 -4 -9 113.99 9.7 -5 -4 9 138.69 11.7 -5 4 9 138.59 12.1 5 4 -9 139.09 9.9 5 4 -9 118.69 10.2 4 -4 -9 113.69 9 -4 -4 9 121.89 10.4 -4 4 9 98.39 10 4 4 -9 100.69 8.4 -3 -4 9 4.8 3.8 3 -4 -9 3.2 3.6 -3 4 9 7.1 4 3 4 -9 3.7 3.6 2 -4 -9 70.59 6.8 -2 -4 9 69.19 7.2 -2 4 9 65.99 6.9 2 4 -9 71.99 6.9 1 -4 -9 535.65 17.1 -1 -4 9 550.84 17.6 -1 4 9 512.35 16.9 1 4 -9 546.15 17.8 0 -4 -9 -0.5 1.9 0 -4 9 1.7 2.1 0 4 -9 1.4 2.3 0 4 9 2.9 2.1 0 4 -9 1.5 2.5 -1 -4 -9 3713.23 76.79 1 -4 9 3834.22 76.69 -1 4 -9 3836.72 78.89 -1 4 -9 3851.21 83.39 -2 -4 -9 2710.13 65.09 -2 -4 -9 2744.73 54.69 2 -4 9 2697.23 65.69 -2 4 -9 2762.42 57.99 -2 4 -9 2728.63 64.69 -3 -4 -9 450.55 23.5 3 -4 9 526.35 22.9 -3 4 -9 508.85 15.1 -3 4 -9 509.65 21.7 4 -4 9 609.44 27.3 -4 -4 -9 574.94 24.9 -4 4 -9 603.94 17.4 -4 4 -9 573.54 17.3 5 -4 9 12.4 7.1 -5 -4 -9 18.7 7 -5 4 -9 14.3 3.8 -5 4 -9 14.8 4 -6 -4 -9 39.4 9.2 -6 -4 -9 52.59 4 6 -4 9 48.8 10.4 -6 4 -9 48.2 6.9 -6 4 -9 52.89 6.2 -6 -5 9 12.5 6.2 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