#------------------------------------------------------------------------------ #$Date: 2020-06-05 14:35:57 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557952.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_1557952 loop_ _publ_author_name 'Dizon, Glenieliz C.' 'Atkinson, George' 'Argent, Stephen P.' 'Santu, Lea T.' 'Amabilino, David B.' _publ_section_title ; Sustainable sorbitol-derived compounds for gelation of the full range of ethanol-water mixtures. ; _journal_issue 19 _journal_name_full 'Soft matter' _journal_page_first 4640 _journal_page_last 4654 _journal_paper_doi 10.1039/d0sm00343c _journal_volume 16 _journal_year 2020 _chemical_absolute_configuration ad _chemical_formula_moiety 'C14 H20 O8' _chemical_formula_sum 'C14 H20 O8' _chemical_formula_weight 316.30 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _audit_creation_date 2019-08-05 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-08-06 deposited with the CCDC. 2020-04-28 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.9088(15) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.92283(14) _cell_length_b 4.60123(7) _cell_length_c 17.4539(3) _cell_measurement_reflns_used 7491 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 73.4150 _cell_measurement_theta_min 4.9530 _cell_volume 715.66(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment 'N2 gas' _diffrn_ambient_temperature 120(2) _diffrn_crystal_treatment 'flash frozen in gaseous N2' _diffrn_detector 'CCD area detector' _diffrn_detector_area_resol_mean 5.2349 _diffrn_detector_type 'Agilent Diffraction Atlas S2 detector' _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.990 _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 -50.00 34.00 1.00 6.00 -- -38.50 38.00 -60.00 84 2 \w -65.00 32.00 1.00 6.00 -- -38.50 57.00 60.00 97 3 \w 20.00 115.00 1.00 6.00 -- 42.83 38.00-120.00 95 4 \w 11.00 117.00 1.00 6.00 -- 42.83 77.00 120.00 106 5 \w 33.00 98.00 1.00 24.00 -- 104.50 -45.00 30.00 65 6 \w 81.00 178.00 1.00 24.00 -- 104.50 30.00 -90.00 97 7 \w 59.00 178.00 1.00 24.00 -- 104.50 15.00 0.00 119 8 \w 77.00 175.00 1.00 24.00 -- 104.50 61.00 90.00 98 9 \w 33.00 98.00 1.00 24.00 -- 104.50 -45.00 150.00 65 10 \w 33.00 98.00 1.00 24.00 -- 104.50 -45.00 -90.00 65 11 \w 30.00 91.00 1.00 24.00 -- 104.50 -30.00 90.00 61 12 \w 23.00 109.00 1.00 24.00 -- 104.50 -94.00 60.00 86 13 \w 30.00 91.00 1.00 24.00 -- 104.50 -30.00-180.00 61 14 \w 30.00 91.00 1.00 24.00 -- 104.50 -30.00 -30.00 61 15 \w 23.00 109.00 1.00 24.00 -- 104.50 -94.00 30.00 86 16 \w 23.00 109.00 1.00 24.00 -- 104.50 -94.00 -60.00 86 17 \w 23.00 109.00 1.00 24.00 -- 104.50 -94.00 150.00 86 18 \w -94.00 -2.00 1.00 6.00 -- -38.50 125.00 90.00 92 19 \w 11.00 117.00 1.00 6.00 -- 42.83 77.00-120.00 106 20 \w 16.00 113.00 1.00 6.00 -- 42.83 57.00 60.00 97 21 \w 16.00 113.00 1.00 6.00 -- 42.83 57.00-150.00 97 22 \w 11.00 117.00 1.00 6.00 -- 42.83 77.00 -30.00 106 23 \w 73.00 178.00 1.00 24.00 -- 104.50 77.00 30.00 105 24 \w 81.00 178.00 1.00 24.00 -- 104.50 30.00-180.00 97 25 \w 77.00 102.00 1.00 24.00 -- 104.50 61.00-150.00 25 ; _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'SuperNova, Atlas S2' _diffrn_measurement_method '\w scans' _diffrn_measurement_specimen_support 'MiTeGen micromount' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1706627000 _diffrn_orient_matrix_UB_12 0.0418094000 _diffrn_orient_matrix_UB_13 0.0041163000 _diffrn_orient_matrix_UB_21 0.0152040000 _diffrn_orient_matrix_UB_22 0.3158298000 _diffrn_orient_matrix_UB_23 -0.0279232000 _diffrn_orient_matrix_UB_31 -0.0228339000 _diffrn_orient_matrix_UB_32 -0.1031227000 _diffrn_orient_matrix_UB_33 -0.0837539000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0231 _diffrn_reflns_av_unetI/netI 0.0182 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 9752 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.977 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.532 _diffrn_reflns_theta_min 4.963 _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Agilent Diffraction microfocus tube' _exptl_absorpt_coefficient_mu 1.035 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.468 _exptl_crystal_description plank _exptl_crystal_F_000 336 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Water' _exptl_crystal_size_max 0.195 _exptl_crystal_size_mid 0.052 _exptl_crystal_size_min 0.026 _refine_diff_density_max 0.206 _refine_diff_density_min -0.177 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Flack x determined using 1179 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.07(5) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 201 _refine_ls_number_reflns 2828 _refine_ls_number_restraints 7 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0253 _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^)+(0.0352P)^2^+0.1508P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.0665 _reflns_Friedel_coverage 0.746 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.959 _reflns_number_gt 2777 _reflns_number_total 2828 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0sm00343c2.cif _cod_data_source_block MBS-Van _cod_depositor_comments 'Adding full bibliography for 1557951--1557952.cif.' _cod_database_code 1557952 _nottingham_internal_coll_name OGPALB _nottingham_internal_coll_number 17025 _nottingham_internal_coll_client GPA/DBA _nottingham_internal_coll_type custom _nottingham_internal_coll_frame_method '\w scans' _nottingham_internal_coll_frame_time '6.00, 24.00' _nottingham_internal_coll_frame_width 1.00 _nottingham_internal_coll_user pcxga2 _nottingham_internal_coll_date 15/05/2017 _nottingham_internal_coll_location NOTTS _nottingham_internal_coll_instrument 'GVB, PL13110001' _nottingham_internal_process_date 25/05/2017 _nottingham_internal_process_user pcxga2 _nottingham_internal_solution_date 25/05/2017 _nottingham_internal_solution_user pcxga2 _nottingham_internal_refinement_date 20/06/2019 _nottingham_internal_refinement_user pczspa _nottingham_internal_validation_date 2019 _nottingham_internal_validation_user pczspa _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C14 H20 O8' _chemical_oxdiff_usercomment 'OGPALB #17025 GVB-1352 IN FOMBLIM ON A MICROMOUNT FOR GPA/DBA' _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 0.974 _shelx_estimated_absorpt_t_min 0.824 _reflns_odcompleteness_completeness 99.93 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 67.13 _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, All O(H) groups 2. Restrained distances O22-H22 0.84 with sigma of 0.02 O4-H4 0.84 with sigma of 0.02 O2-H2 0.84 with sigma of 0.02 O8-H8 0.84 with sigma of 0.02 O12-H12 0.84 with sigma of 0.02 3. Restrained planarity C13, C14, C15, C19 with sigma of 0.01 4.a Ternary CH refined with riding coordinates: C3(H3), C5(H5), C7(H7), C9(H9), C13(H13) 4.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C11(H11A,H11B) 4.c Aromatic/amide H refined with riding coordinates: C18(H18), C19(H19), C15(H15) 4.d Fitted hexagon refined as free rotating group: C17(C18,C19,C14,C15,C16) 4.e Idealised Me refined as rotating group: C21(H21A,H21B,H21C) 4.f Idealised tetrahedral OH refined as rotating group: O2(H2) ; _shelx_res_file ; TITL OGPALB in P21 #4 ogpalb.res created by SHELXL-2018/3 at 09:49:48 on 05-Aug-2019 REM reset to P21 #4 CELL 1.54184 8.922827 4.601228 17.453883 90 92.9088 90 ZERR 2 0.000144 0.000067 0.000313 0 0.0015 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O UNIT 28 40 16 EQIV $1 -1+X,1+Y,+Z EQIV $2 +X,-1+Y,+Z EQIV $3 1+X,+Y,+Z EQIV $4 -X,0.5+Y,1-Z DFIX 0.84 O22 H22 DFIX 0.84 O4 H4 DFIX 0.84 O2 H2 DFIX 0.84 O8 H8 DFIX 0.84 O12 H12 FLAT 0.01 C13 C14 C15 C19 L.S. 10 PLAN 10 SIZE 0.026 0.052 0.195 TEMP -153(2) HTAB O2 O12_$1 HTAB O4 O8_$4 HTAB O8 O4_$2 HTAB O12 O2_$3 BOND fmap 2 acta OMIT 9 0 7 REM REM REM WGHT 0.035200 0.150800 FVAR 10.29852 C1 1 -0.187040 1.176717 0.710567 11.00000 0.01416 0.02401 = 0.01734 0.00157 0.00066 0.00294 AFIX 23 H1A 2 -0.175833 1.028610 0.751602 11.00000 -1.20000 H1B 2 -0.149762 1.364202 0.731836 11.00000 -1.20000 AFIX 0 O2 3 -0.342210 1.204741 0.686928 11.00000 0.01364 0.01960 = 0.02662 0.00511 0.00221 0.00255 AFIX 147 H2 2 -0.354700 1.355776 0.660333 11.00000 -1.50000 AFIX 0 C3 1 -0.093726 1.089099 0.644047 11.00000 0.01388 0.01186 = 0.01482 0.00167 -0.00134 -0.00057 AFIX 13 H3 2 -0.137670 0.911995 0.618424 11.00000 -1.20000 AFIX 0 O4 3 -0.097958 1.326748 0.591582 11.00000 0.01830 0.01398 = 0.01390 0.00127 -0.00063 0.00075 H4 2 -0.102371 1.263021 0.547323 11.00000 -1.50000 C5 1 0.069529 1.032282 0.670232 11.00000 0.01510 0.01114 = 0.01442 0.00201 -0.00200 0.00011 AFIX 13 H5 2 0.110961 1.211802 0.695707 11.00000 -1.20000 AFIX 0 O6 3 0.072125 0.800866 0.725956 11.00000 0.01415 0.01333 = 0.01463 0.00248 -0.00184 0.00120 C7 1 0.168543 0.952452 0.604710 11.00000 0.01321 0.01164 = 0.01547 0.00061 -0.00111 -0.00175 AFIX 13 H7 2 0.178564 1.127853 0.571529 11.00000 -1.20000 AFIX 0 O8 3 0.107064 0.721788 0.558050 11.00000 0.01887 0.01741 = 0.01436 -0.00224 0.00068 -0.00422 H8 2 0.049652 0.611569 0.581728 11.00000 -1.50000 C9 1 0.324622 0.871152 0.638162 11.00000 0.01505 0.01108 = 0.01813 0.00305 -0.00121 -0.00097 AFIX 13 H9 2 0.373612 1.048881 0.660921 11.00000 -1.20000 AFIX 0 O10 3 0.312799 0.655936 0.697513 11.00000 0.01635 0.01293 = 0.01710 0.00269 0.00041 0.00227 C11 1 0.423572 0.747572 0.578396 11.00000 0.01317 0.01733 = 0.02315 0.00280 0.00071 0.00188 AFIX 23 H11A 2 0.382528 0.557778 0.560756 11.00000 -1.20000 H11B 2 0.421767 0.879888 0.533631 11.00000 -1.20000 AFIX 0 O12 3 0.575159 0.708899 0.606662 11.00000 0.01419 0.01879 = 0.03586 -0.00050 0.00044 0.00284 H12 2 0.603564 0.860943 0.628885 11.00000 -1.50000 C13 1 0.222183 0.761762 0.755479 11.00000 0.01505 0.01376 = 0.01554 -0.00144 -0.00275 -0.00009 AFIX 13 H13 2 0.262647 0.953671 0.773742 11.00000 -1.20000 AFIX 66 C17 1 0.253771 0.173963 0.946346 11.00000 0.02479 0.01560 = 0.01399 0.00056 -0.00358 -0.00173 C18 1 0.117402 0.307967 0.927104 11.00000 0.02021 0.02186 = 0.01906 0.00038 0.00188 -0.00090 AFIX 43 H18 2 0.032710 0.270628 0.956464 11.00000 -1.20000 AFIX 65 C19 1 0.104950 0.496605 0.864903 11.00000 0.01915 0.01840 = 0.01824 -0.00031 -0.00267 0.00153 AFIX 43 H19 2 0.011748 0.588190 0.851752 11.00000 -1.20000 AFIX 65 C14 1 0.228867 0.551239 0.821944 11.00000 0.02069 0.01314 = 0.01390 -0.00205 -0.00352 -0.00092 C15 1 0.365237 0.417237 0.841186 11.00000 0.01928 0.01515 = 0.01511 0.00001 -0.00205 -0.00234 AFIX 43 H15 2 0.449928 0.454579 0.811825 11.00000 -1.20000 AFIX 65 C16 1 0.377690 0.228599 0.903386 11.00000 0.01978 0.01401 = 0.01571 -0.00186 -0.00409 0.00044 AFIX 0 O20 3 0.507307 0.086702 0.927862 11.00000 0.01910 0.02233 = 0.01784 0.00318 -0.00116 0.00453 C21 1 0.617949 0.046462 0.871800 11.00000 0.02281 0.02317 = 0.01892 0.00028 0.00111 0.00460 AFIX 137 H21A 2 0.569562 -0.030302 0.824363 11.00000 -1.50000 H21B 2 0.694355 -0.091085 0.891558 11.00000 -1.50000 H21C 2 0.665396 0.233329 0.861240 11.00000 -1.50000 AFIX 0 O22 3 0.263407 -0.016348 1.006850 11.00000 0.02456 0.02304 = 0.01990 0.00754 0.00045 0.00274 H22 2 0.345880 -0.108800 1.005134 11.00000 -1.50000 HKLF 4 REM OGPALB in P21 #4 REM wR2 = 0.0665, GooF = S = 1.064, Restrained GooF = 1.073 for all data REM R1 = 0.0253 for 2777 Fo > 4sig(Fo) and 0.0258 for all 2828 data REM 201 parameters refined using 7 restraints END WGHT 0.0352 0.1508 REM Highest difference peak 0.206, deepest hole -0.177, 1-sigma level 0.035 Q1 1 -0.1410 1.1333 0.6784 11.00000 0.05 0.21 Q2 1 0.3698 0.8041 0.6059 11.00000 0.05 0.20 Q3 1 0.1155 0.9877 0.6368 11.00000 0.05 0.18 Q4 1 0.2051 0.5152 0.8111 11.00000 0.05 0.17 Q5 1 0.2404 0.9063 0.6260 11.00000 0.05 0.16 Q6 1 -0.0156 1.0338 0.6546 11.00000 0.05 0.16 Q7 1 0.1782 0.1997 0.9211 11.00000 0.05 0.15 Q8 1 0.1631 0.5695 0.8588 11.00000 0.05 0.14 Q9 1 0.3029 0.1310 0.9105 11.00000 0.05 0.14 Q10 1 0.3566 0.2434 0.8619 11.00000 0.05 0.13 ; _shelx_res_checksum 4628 _shelx_hkl_file ; 0 -5 0 20.3022 61.2357 23 0 -5 0-98.6980 78.4504 13 0 -5 -1 405.689 97.6115 13 0 -5 -1 294.901 81.6495 23 0 -5 1 243.707 75.8471 23 0 -5 1 362.747 93.5463 13 0 -5 -2 3747.14 224.499 23 0 -5 -2 3829.66 249.641 13 0 -5 2 3973.29 252.285 13 0 -5 2 3619.65 216.228 23 0 -5 -2 3741.33 237.289 16 0 -5 -3 28848.2 744.652 13 0 -5 -3 28735.5 716.188 16 0 -5 3 29073.2 676.407 23 0 -5 -3 29503.5 713.642 23 0 -5 3 29382.3 739.142 13 0 -5 -4 21791.2 593.743 16 0 -5 -4 23592.0 645.487 13 0 -5 4 22508.4 616.801 13 0 -5 -4 22647.3 599.133 23 0 -5 4 22325.0 553.236 23 0 -5 5 15390.1 421.635 23 0 -5 -5 15260.1 465.751 23 0 -5 -5 15239.1 454.655 16 0 -5 -5 15620.1 489.639 13 0 -5 5 14972.9 471.343 13 0 -5 -6 12461.1 382.145 16 0 -5 6 12316.2 405.329 8 0 -5 -6 12820.8 420.118 13 0 -5 -6 12805.5 405.160 23 0 -5 -7 4095.43 193.366 16 0 -5 -7 4008.02 210.105 13 0 -5 -7 4490.07 218.680 23 0 -5 7 4039.83 218.991 8 0 -5 -8 10674.4 333.634 23 0 -5 8 10672.1 357.194 8 0 -5 9 1940.58 143.577 8 0 -4 0 18917.1 642.516 9 0 -4 0 20509.6 645.915 13 0 -4 0 20571.5 655.052 23 0 -4 -1 2609.16 233.014 23 0 -4 1 2708.30 224.558 23 0 -4 -1 2668.45 225.175 13 0 -4 -1 2506.72 223.999 9 0 -4 1 2568.46 224.720 9 0 -4 1 2706.34 222.334 13 0 -4 -2 1561.65 185.129 9 0 -4 2 1955.11 191.347 13 0 -4 2 1798.74 187.384 23 0 -4 -2 1867.86 188.771 13 0 -4 -2 1900.54 198.848 23 0 -4 2 1535.15 185.560 8 0 -4 -3 5506.13 332.890 9 0 -4 3 5957.16 345.093 8 0 -4 3 5786.83 316.898 13 0 -4 -3 6115.20 346.441 23 0 -4 -3 5910.98 333.484 13 0 -4 3 6171.57 335.697 23 0 -4 -4 1249.83 162.279 9 0 -4 -4 1233.35 154.082 13 0 -4 4 1406.61 156.734 23 0 -4 -4 1264.52 160.738 23 0 -4 4 1245.48 146.578 13 0 -4 4 1662.92 188.299 8 0 -4 -5 1466.14 165.454 13 0 -4 5 1562.71 195.621 8 0 -4 -5 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4900.44 450.206 2 4 2 -1 5085.62 510.340 22 -4 2 0 57741.9 1738.02 19 -4 2 0 61200.9 1942.67 3 -4 2 0 60932.1 1802.89 2 4 2 0 57412.3 1881.97 22 -4 2 0 61136.3 1922.45 21 -4 2 -1 25060.8 1053.51 19 -4 2 -1 24926.7 1190.65 3 -4 2 -1 24622.9 1143.21 2 4 2 1 23731.1 1179.31 22 -4 2 -1 25368.9 1197.00 21 -4 2 -2 42561.9 1378.84 19 -4 2 -2 42849.6 1603.59 3 -4 2 -2 45431.6 1643.33 21 4 2 2 41239.0 1609.51 22 -4 2 -2 44311.1 1608.76 2 4 2 3 8461.03 708.062 22 -4 2 -3 8163.79 676.997 2 -4 2 -3 8539.16 570.918 19 -4 2 -3 8068.63 674.867 3 -4 2 -3 8361.61 677.339 21 -4 2 -4 4791.29 509.981 3 -4 2 -4 4606.92 263.610 14 -4 2 -4 4214.17 506.472 2 -4 2 -4 4490.58 255.250 24 4 2 4 5059.48 555.868 22 -4 2 -4 4579.83 520.913 21 -4 2 -5 9963.51 749.696 3 -4 2 -5 10211.9 407.783 14 -4 2 -5 9859.40 393.044 24 4 2 5 9917.44 796.049 22 -4 2 -5 10189.4 826.208 2 -4 2 -5 11120.6 816.602 21 -4 2 -6 31361.3 1372.73 3 -4 2 -6 32290.2 803.834 14 -4 2 -6 31620.7 780.941 24 4 2 6 31055.0 1502.73 22 -4 2 -6 31343.6 1515.49 2 -4 2 -7 14249.8 1041.88 2 -4 2 -7 12898.2 838.198 3 -4 2 -7 13282.1 489.163 14 -4 2 -7 13826.6 486.803 24 4 2 7 13142.7 1002.58 22 -4 2 -8 61913.1 2343.91 2 4 2 8 61647.9 2313.67 22 -4 2 -8 64755.0 1249.42 15 -4 2 -8 59403.2 1239.89 24 -4 2 -8 64407.2 1297.04 14 -4 2 -9 105732. 3273.63 2 -4 2 -9 111410. 1896.98 15 -4 2 -9 112528. 1963.54 14 -4 2 -9 109493. 1895.29 24 4 2 9 107687. 3268.36 22 -4 2 -10 108406. 1991.84 12 -4 2 -10 108780. 1887.60 15 -4 2 -10 110428. 1956.07 14 -4 2 -10 108867. 1879.16 24 4 2 10 105988. 3287.89 22 -4 2 -11 5731.55 311.360 15 -4 2 -11 5777.49 339.295 14 -4 2 -11 6002.00 312.772 24 -4 2 -11 6105.38 352.283 12 -4 2 -12 6039.65 317.657 15 -4 2 -12 5859.55 338.954 14 -4 2 -12 6003.80 357.754 12 -4 2 -13 19680.3 600.937 15 -4 2 -13 19185.3 630.537 14 -4 2 -13 20570.8 663.761 12 -4 2 -14 1083.77 130.672 15 -4 2 -14 980.899 132.126 14 -4 2 -14 1013.55 159.918 12 -4 2 -15 1642.31 151.016 15 -4 2 -15 1467.79 147.815 5 -4 2 -15 1694.17 156.625 14 -4 2 -15 1741.07 183.430 12 -4 2 -16 346.053 77.8196 15 -4 2 -16 362.962 71.7472 5 -4 2 -16 271.841 89.3338 12 -4 2 -17 2599.11 147.517 15 -4 2 -17 2840.44 178.328 12 -4 2 -18 5125.99 207.630 12 4 3 -17 1454.24 109.805 5 4 3 -16 4946.04 238.810 5 4 3 -16 5131.11 201.333 17 4 3 -15 6725.42 312.316 5 4 3 -15 6673.37 269.092 17 4 3 -14 5449.29 298.280 5 4 3 -14 5584.41 265.436 17 4 3 -14 5668.92 251.600 6 4 3 -13 13032.4 488.552 5 4 3 -13 13029.9 437.477 6 4 3 -12 9649.27 425.315 5 -4 3 12 9246.18 390.599 25 4 3 -12 9514.44 392.972 6 4 3 -11 342.012 95.0500 6 4 3 -11 234.775 75.5706 5 -4 3 11 157.903 73.9318 25 4 3 -10 1950.34 204.808 5 -4 3 10 2439.01 225.464 25 4 3 -10 1842.24 196.463 6 4 3 -9 33831.6 879.914 5 4 3 -9 34913.0 820.422 7 -4 3 9 35579.4 908.793 25 4 3 -9 32743.5 869.556 6 4 3 -8 35538.4 891.644 5 -4 3 8 35049.8 900.479 25 4 3 -8 34989.0 840.678 7 4 3 -8 34050.4 886.667 6 -4 3 7 951.334 249.451 21 -4 3 7 1258.19 309.488 19 4 3 -7 1208.55 152.028 6 4 3 -7 1694.97 181.960 5 -4 3 7 1651.90 176.267 25 -4 3 7 1117.35 324.830 3 4 3 -7 1360.99 155.859 7 -4 3 6 1971.08 410.662 21 -4 3 6 1151.19 443.265 19 4 3 -6 1709.77 180.913 6 4 3 -6 1692.44 374.146 18 -4 3 6 1956.59 412.380 3 -4 3 6 1403.13 170.066 25 4 3 -5 21717.4 660.288 6 -4 3 5 21525.9 1348.52 19 4 3 -5 21183.9 1241.32 18 -4 3 5 22563.9 1363.08 3 -4 3 5 23771.2 709.335 25 -4 3 5 21755.6 1286.04 21 -4 3 4 18805.0 1243.26 19 4 3 -4 17829.4 1131.28 18 4 3 -4 20561.5 624.392 6 -4 3 4 20539.3 1288.53 3 -4 3 4 19525.5 642.678 25 -4 3 4 19684.8 1223.81 21 4 3 -3 7758.22 359.901 6 -4 3 3 6260.49 702.907 19 -4 3 3 7117.93 759.164 3 -4 3 3 7731.16 381.259 25 -4 3 3 7004.16 714.405 21 -4 3 2 1028.56 296.645 21 -4 3 2 827.878 388.368 19 4 3 -2 747.872 120.824 6 -4 3 2 720.525 142.630 25 -4 3 2 591.730 234.639 3 4 3 -1 2129.30 177.980 6 -4 3 1 1685.65 348.516 21 -4 3 1 1550.85 379.597 19 -4 3 1 2077.12 210.344 25 -4 3 1 1987.36 397.321 3 -4 3 1 2032.76 178.005 24 4 3 0 6473.87 314.523 6 -4 3 0 6506.23 665.460 19 -4 3 0 6630.54 722.669 3 -4 3 0 6849.95 361.625 25 -4 3 0 6547.67 328.360 24 -4 3 0 6959.05 670.043 2 4 3 0 6415.90 656.990 22 -4 3 0 6754.37 717.960 21 4 3 1 2062.79 175.270 6 -4 3 -1 2054.28 401.126 21 -4 3 -1 1976.17 349.185 19 4 3 1 2004.16 395.741 22 -4 3 -1 2043.17 182.902 24 -4 3 -1 2104.48 424.330 3 -4 3 -1 1880.17 163.639 14 -4 3 -1 1853.08 355.676 2 -4 3 -1 1961.33 196.945 25 -4 3 -2 1829.42 397.533 21 -4 3 -2 2196.60 405.078 19 -4 3 -2 2514.92 475.765 3 -4 3 -2 1915.63 180.254 14 -4 3 -2 2276.55 394.629 2 -4 3 -2 2051.34 183.458 24 4 3 2 1751.57 385.583 22 4 3 3 28872.6 741.168 7 -4 3 -3 28469.3 1528.00 3 -4 3 -3 27793.8 748.017 14 -4 3 -3 27279.2 739.730 24 -4 3 -3 27928.8 1471.98 2 4 3 3 26590.3 1457.97 22 -4 3 -3 26666.3 1459.37 21 4 3 4 38933.2 870.900 7 -4 3 -4 36774.6 1747.57 3 -4 3 -4 35719.4 896.117 14 -4 3 -4 34313.1 871.835 24 4 3 4 34403.0 1702.74 22 -4 3 -4 36398.0 1749.62 2 -4 3 -5 20028.6 1241.44 3 -4 3 -5 18475.1 616.775 6 -4 3 -5 20157.4 638.066 14 -4 3 -5 19347.0 619.515 24 4 3 5 20208.6 585.716 7 4 3 5 19625.4 1281.18 22 -4 3 -5 19762.7 1301.31 2 -4 3 -6 37249.0 1715.64 3 -4 3 -6 40106.7 919.724 6 -4 3 -6 38803.0 966.779 14 -4 3 -6 37767.7 935.289 24 4 3 6 36725.7 1826.23 22 -4 3 -7 18649.8 638.234 14 -4 3 -7 19519.6 627.915 24 -4 3 -8 3999.91 312.061 14 -4 3 -8 2479.11 213.617 24 -4 3 -9 3318.09 247.272 24 -4 3 -9 3153.40 251.789 12 -4 3 -10 9195.70 443.105 14 -4 3 -10 9382.40 419.906 12 -4 3 -11 8482.98 418.466 14 -4 3 -11 8169.75 379.849 12 -4 3 -12 4004.02 273.711 14 -4 3 -12 4099.88 252.322 12 -4 3 -13 9775.88 377.208 5 -4 3 -13 9097.09 402.425 14 -4 3 -13 9334.19 366.873 12 -4 3 -14 22780.9 566.370 5 -4 3 -14 21550.6 599.140 14 -4 3 -14 21590.7 552.877 12 -4 3 -15 6439.66 247.099 5 -4 3 -15 6191.01 263.144 14 -4 3 -15 6077.94 240.769 12 -4 3 -16 9107.99 260.034 5 4 4 -13 903.861 75.7235 17 4 4 -13 1030.77 81.7631 6 4 4 -12 2539.27 150.180 5 4 4 -12 2684.61 150.837 17 4 4 -12 2683.66 154.834 6 4 4 -11 5501.94 250.956 6 4 4 -10 139.449 63.5437 6 -4 4 9 2120.04 186.348 6 4 4 -9 2549.30 171.423 7 4 4 -9 2498.42 193.284 6 4 4 -8 8568.55 373.261 6 4 4 -8 8772.26 344.769 7 4 4 -7 380.832 98.4713 6 4 4 -7 422.138 89.2687 7 4 4 -6 8855.07 375.336 7 4 4 -6 8309.96 378.497 6 4 4 -5 14700.6 505.044 7 4 4 -5 13980.5 508.133 6 4 4 -4 14475.2 507.162 7 4 4 -4 13823.3 505.365 6 4 4 -3 1359.71 161.419 6 4 4 -2 7760.23 359.707 6 4 4 -1 1142.21 145.620 6 4 4 0 2576.65 200.696 6 -4 4 0 2228.98 227.806 6 -4 4 -1 3097.56 252.218 6 -4 4 -1 3024.26 207.508 24 4 4 1 3347.12 236.527 7 4 4 1 3134.08 210.058 6 -4 4 -2 982.003 156.312 6 -4 4 -2 798.638 117.478 24 4 4 2 1031.88 138.340 7 -4 4 -3 13344.7 510.767 6 -4 4 -3 12008.9 467.417 14 4 4 3 13508.8 467.724 7 -4 4 -4 3806.63 262.240 6 -4 4 -4 3732.55 256.710 14 4 4 4 3902.57 237.193 7 -4 4 -5 5191.68 285.035 6 -4 4 -5 4226.80 274.417 14 4 4 5 4794.60 250.283 7 -4 4 -6 5157.02 269.878 6 -4 4 -6 4846.68 296.745 14 -4 4 -7 289.814 69.1624 6 -4 4 -7 295.221 98.0085 14 -4 4 -8 10842.8 438.149 14 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419.397 7 -7 1 -3 10016.1 425.369 24 7 1 3 9666.84 900.039 22 -7 1 -4 260.618 82.4103 10 7 1 4-76.1243 151.752 20 -7 1 -4 225.233 82.9270 24 -7 1 -4 29.2392 137.887 2 7 1 4 143.751 66.6638 7 7 1 4-53.9115 141.254 22 -7 1 -5 9306.14 432.196 10 7 1 5 8355.08 764.924 20 7 1 5 9424.31 390.270 7 -7 1 -5 9439.26 412.470 24 7 1 5 8269.87 849.467 22 -7 1 -6 1690.28 190.002 10 -7 1 -6 1533.11 162.542 24 -7 1 -7 7395.01 391.344 10 -7 1 -7 7277.28 350.188 24 -7 1 -8 5082.66 316.159 10 -7 1 -8 5185.88 330.125 15 -7 1 -8 5335.29 285.575 24 -7 1 -9 845.787 130.709 10 -7 1 -9 846.599 147.432 15 -7 1 -9 802.218 125.537 14 -7 1 -9 1167.77 134.914 24 -7 1 -9 670.846 122.981 12 -7 1 -10 5081.11 314.194 10 -7 1 -10 5227.02 311.097 15 -7 1 -10 5180.81 298.095 14 -7 1 -10 4705.48 296.646 12 -7 1 -11 1879.60 182.006 15 -7 1 -11 1764.41 167.657 14 -7 1 -11 1870.05 180.990 12 -7 1 -12 2371.69 197.726 15 -7 1 -12 2340.73 173.391 14 -7 1 -12 2280.87 180.138 12 -7 1 -13 7902.78 328.747 15 -7 1 -13 7972.24 293.417 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-8 1 -4 14984.8 519.011 24 -8 1 -5 491.712 109.463 10 -8 1 -5 265.362 83.0955 24 8 1 5 345.351 88.6298 7 -8 1 -6 6405.77 347.453 10 -8 1 -6 5897.54 309.684 24 -8 1 -7 5795.18 327.943 10 -8 1 -7 5565.43 324.141 15 -8 1 -7 5656.52 290.910 24 -8 1 -8 3219.82 242.166 10 -8 1 -8 3076.75 236.470 15 -8 1 -8 3177.88 232.526 14 -8 1 -8 3146.09 201.099 24 -8 1 -8 2979.12 222.971 12 -8 1 -9 2761.36 213.980 15 -8 1 -9 3040.04 212.480 14 -8 1 -9 3053.01 209.402 12 -8 1 -10 2654.84 201.113 15 -8 1 -10 2503.31 181.575 14 -8 1 -10 2540.65 181.731 12 -8 1 -11 169.548 75.8926 15 -8 1 -11 200.644 69.1102 14 -8 1 -11 101.811 53.8491 12 -8 1 -12 4881.50 230.100 15 -8 1 -12 4819.41 205.195 14 -8 1 -12 5054.85 209.598 12 -8 1 -13 7508.38 256.948 15 8 2 -13 975.160 93.3104 11 -8 2 13 974.694 97.5049 25 8 2 -12 3980.41 177.937 17 -8 2 12 4199.40 213.145 25 8 2 -12 3937.46 204.650 11 8 2 -11 6939.78 255.999 17 -8 2 11 6966.61 298.728 25 8 2 -11 7051.76 296.813 11 8 2 -10 13456.3 398.029 17 -8 2 10 14220.0 458.230 25 8 2 -10 14414.5 457.931 11 8 2 -9 12964.5 390.233 17 8 2 -9 13578.2 412.850 7 -8 2 9 12663.5 449.215 25 8 2 -9 13167.9 448.808 11 8 2 -8 13960.9 420.217 17 8 2 -8 14976.8 467.979 7 -8 2 8 14393.3 496.456 25 -8 2 8 15290.3 438.645 24 8 2 -8 14008.5 473.544 11 8 2 -7 47010.4 920.878 17 8 2 -7 48657.6 1018.38 7 -8 2 7 48056.2 1042.79 25 -8 2 7 49362.4 970.492 24 8 2 -7 49632.9 1024.72 11 8 2 -6 2533.60 207.401 7 -8 2 6 2450.18 215.497 25 -8 2 6 2201.04 183.201 24 8 2 -6 2658.00 202.392 11 8 2 -5 4704.15 284.380 7 -8 2 5 4921.80 291.566 25 -8 2 5 4949.32 272.295 24 8 2 -5 5093.59 273.135 11 8 2 -4 13574.0 504.735 7 -8 2 4 14514.4 506.582 25 -8 2 4 13958.5 481.924 24 8 2 -4 14018.3 472.836 11 -8 2 3 593.163 108.123 25 -8 2 3 487.925 111.146 24 8 2 -3 385.531 104.593 7 -8 2 2 2194.77 194.709 25 -8 2 2 2000.59 182.507 24 8 2 -2 2040.49 195.463 7 -8 2 1 657.269 128.429 25 -8 2 1 532.301 115.162 24 8 2 -1 592.520 110.920 7 8 2 0 6159.46 334.175 7 -8 2 0 5893.87 306.647 25 -8 2 0 5970.12 322.424 24 -8 2 -1 4279.83 271.783 14 8 2 1 4724.96 291.828 7 -8 2 -1 5076.28 299.252 24 -8 2 -2 13116.5 484.956 14 8 2 2 14211.5 502.326 7 -8 2 -2 13711.4 503.069 24 -8 2 -3 2049.23 186.905 14 8 2 3 2297.19 195.126 7 -8 2 -3 2496.70 210.059 24 -8 2 -4 6539.23 333.156 14 8 2 4 6463.73 309.841 7 -8 2 -4 6858.53 329.908 24 -8 2 -5 10598.2 409.903 15 -8 2 -5 11384.7 441.842 14 8 2 5 11215.5 394.155 7 -8 2 -5 11748.3 437.491 24 -8 2 -6 8956.83 359.835 15 -8 2 -6 9608.03 400.563 14 -8 2 -6 9649.87 379.601 24 -8 2 -7 3560.07 214.540 15 -8 2 -7 3733.57 237.970 14 -8 2 -7 3166.95 215.958 24 -8 2 -8 1479.47 130.850 15 -8 2 -8 1571.44 149.923 14 -8 2 -8 1244.25 132.207 24 -8 2 -8 1260.92 149.800 12 -8 2 -9 2820.12 166.373 15 -8 2 -9 2874.17 191.504 14 -8 2 -9 2342.52 160.888 24 -8 2 -9 2834.92 198.077 12 -8 2 -10 11151.4 327.370 15 -8 2 -10 11960.8 380.997 14 -8 2 -10 12175.0 384.018 12 -8 2 -11 96.9615 39.3447 14 -8 2 -11 113.735 38.2038 12 -8 2 -12 372.566 56.6535 12 -8 3 10 1937.01 121.428 25 8 3 -10 1959.08 118.945 11 8 3 -9 1083.35 95.3636 11 -8 3 9 1245.05 107.389 25 8 3 -8 3433.68 170.574 7 -8 3 8 3437.63 189.527 25 8 3 -8 3616.36 178.202 11 8 3 -7 1980.81 142.198 7 -8 3 7 2004.19 152.989 25 8 3 -7 1994.25 135.987 11 8 3 -6 3553.66 202.021 7 -8 3 6 3457.05 206.609 25 8 3 -6 3594.23 182.331 11 8 3 -5 10985.4 382.363 7 -8 3 5 10929.8 384.993 25 8 3 -5 10953.5 332.413 11 8 3 -4 2109.25 174.011 7 -8 3 4 1889.18 162.914 25 -8 3 4 1874.19 137.042 24 8 3 -3 1826.41 166.594 7 -8 3 3 1815.14 140.041 24 8 3 -2 2352.84 188.778 7 -8 3 2 2185.33 161.201 24 -8 3 1 1015.79 117.526 24 8 3 -1 1148.15 141.410 7 8 3 0 4949.97 265.162 7 -8 3 0 4744.09 240.339 24 -8 3 -1 627.474 103.029 24 8 3 1 544.755 99.4801 7 -8 3 -2 49.1600 40.2170 14 -8 3 -2 36.9973 59.6085 24 8 3 2 59.8827 64.0546 7 -8 3 -3 174.624 49.0963 14 -8 3 -3 51.8801 63.2973 24 8 3 3 117.634 54.1372 7 -8 3 -4 766.974 94.7222 14 -8 3 -4 664.520 107.649 24 8 3 4 895.830 98.1324 7 -8 3 -5 2549.70 164.436 14 -8 3 -5 2390.26 174.579 24 -8 3 -6 2359.37 154.397 14 -8 3 -6 2595.74 161.114 24 -8 3 -7 16934.2 436.014 14 -8 3 -7 16539.9 417.362 24 -8 3 -7 16190.0 447.012 12 -8 3 -8 6023.30 231.740 14 -8 3 -8 5990.67 232.167 12 -8 3 -9 5717.65 208.459 14 -8 3 -9 6109.86 211.399 12 9 -3 -4 11095.1 315.292 7 -9 -3 3 1399.44 90.0344 8 9 -3 -3 1458.30 111.988 7 -9 -3 2 7339.45 228.860 8 9 -3 -2 7696.77 276.593 7 -9 -3 1 3572.83 156.470 8 9 -3 -1 3342.87 181.949 7 -9 -3 0 379.067 57.7491 10 -9 -3 0 394.354 59.0907 8 9 -3 0 357.218 70.6942 7 -9 -3 -1 207.279 45.2622 10 9 -3 1 187.599 55.8956 7 -9 -3 -2 2557.36 132.399 10 9 -3 2 2279.01 137.431 7 -9 -3 -3 535.065 65.6590 10 -9 -3 -4 1031.63 84.1997 10 9 -2 -11 12433.5 317.367 9 -9 -2 11 11879.6 303.072 24 9 -2 -10 6129.85 232.677 9 -9 -2 10 5730.39 222.723 24 9 -2 -9 5997.62 247.440 9 -9 -2 9 5749.20 232.399 24 9 -2 -8 582.106 82.5837 9 -9 -2 8 416.021 75.7583 24 9 -2 -7 11292.7 374.933 9 9 -2 -7 10957.4 343.058 7 -9 -2 7 10927.1 352.637 24 9 -2 -6 8130.71 313.495 9 9 -2 -6 8012.14 314.090 7 -9 -2 6 7866.22 300.312 24 9 -2 -5 2076.39 157.438 9 9 -2 -5 2184.91 173.455 7 -9 -2 5 2348.70 162.077 24 9 -2 -4 1378.43 126.557 9 -9 -2 4 1542.89 137.652 24 9 -2 -4 1399.51 148.019 7 9 -2 -3 25.4634 47.0365 9 -9 -2 3 121.041 49.2390 8 9 -2 -3-42.3360 72.5368 7 -9 -2 3 79.4508 52.8927 24 -9 -2 2 745.085 89.1817 8 9 -2 -2 657.075 128.364 7 -9 -2 2 608.461 86.6345 24 -9 -2 1 5709.83 244.993 10 -9 -2 1 5912.22 247.312 8 9 -2 -1 5970.16 308.416 7 -9 -2 0 17632.0 474.365 10 -9 -2 0 17414.8 465.329 8 9 -2 0 16887.1 541.375 7 -9 -2 -1 6241.17 267.494 10 -9 -2 -1 5993.61 257.749 8 9 -2 1 5864.41 303.646 7 -9 -2 -2 8964.91 331.516 10 9 -2 2 9350.40 368.214 7 -9 -2 -3 17090.9 480.036 10 9 -2 3 16105.4 485.554 7 -9 -2 -4 2742.73 177.620 10 9 -2 4 2805.38 182.752 7 -9 -2 -5 2788.22 177.924 10 9 -2 5 2750.13 164.788 7 -9 -2 -6 9773.01 333.996 10 9 -2 6 8746.66 278.912 7 9 -2 6 9339.50 311.093 23 -9 -2 -7 1152.04 108.074 10 9 -2 7 716.099 85.2830 23 -9 -2 -8 1973.63 128.350 10 9 -2 8 1724.98 119.536 23 -9 -2 -9 4928.63 191.618 10 9 -1 -12 3515.09 170.451 9 -9 -1 12 3335.80 163.398 24 9 -1 -12 3402.00 185.818 11 9 -1 -11 3390.01 186.033 9 -9 -1 11 3415.34 183.418 24 9 -1 -11 3359.74 204.667 11 9 -1 -10 713.364 102.495 9 -9 -1 10 722.871 99.3410 24 9 -1 -10 906.530 120.551 11 -9 -1 9 12695.9 411.879 24 9 -1 -9 12588.9 458.257 11 9 -1 -8 706.976 96.2779 7 -9 -1 8 622.508 102.120 24 9 -1 -8 555.528 114.384 11 9 -1 -7 6606.16 301.576 7 -9 -1 7 6810.68 316.123 24 9 -1 -7 6293.68 332.860 11 9 -1 -6 4071.89 252.223 7 -9 -1 6 4325.35 273.471 24 9 -1 -6 3792.57 265.005 11 9 -1 -5 5569.00 303.327 7 -9 -1 5 5316.60 287.438 24 9 -1 -5 5040.57 303.491 11 9 -1 -4 8033.20 376.553 7 -9 -1 4 7869.15 347.574 24 9 -1 -4 7408.79 370.017 11 -9 -1 3 613.317 115.113 24 9 -1 -3 460.963 118.012 7 9 -1 -3 526.950 109.317 11 9 -1 -2 2385.28 220.672 7 -9 -1 2 2433.92 193.585 24 9 -1 -2 2239.68 195.325 11 9 -1 -1 6864.08 352.876 7 -9 -1 1 6560.73 309.386 24 9 -1 -1 5974.38 315.991 11 -9 -1 0 16512.8 490.062 10 9 -1 0 15580.7 548.521 7 -9 -1 0 15691.7 490.490 24 -9 -1 -1 12999.1 436.426 10 9 -1 1 12466.5 476.883 7 -9 -1 -1 12616.2 416.713 24 -9 -1 -2 4749.25 258.635 10 9 -1 2 4251.57 261.929 7 -9 -1 -3 16126.5 509.914 10 9 -1 3 16007.4 521.450 7 -9 -1 -4 2873.74 208.760 10 9 -1 4 2933.42 204.138 7 -9 -1 -5 129.760 57.4312 10 -9 -1 -5 198.391 73.4422 15 9 -1 5 116.828 57.0110 7 9 -1 5 244.731 68.4609 23 -9 -1 -6 3647.94 225.148 10 -9 -1 -6 3054.86 210.324 15 9 -1 6 3255.56 189.583 7 9 -1 6 3249.83 204.616 23 -9 -1 -7 1554.22 145.802 10 -9 -1 -7 1744.68 151.627 15 9 -1 7 1539.59 141.591 23 -9 -1 -8 11067.4 382.945 10 -9 -1 -8 11098.4 355.498 15 9 -1 8 10358.6 357.296 23 -9 -1 -9 934.937 108.489 10 -9 -1 -9 909.301 92.6973 15 9 -1 9 1002.62 113.817 23 -9 -1 -10 197.630 48.5070 10 9 -1 10 368.238 70.0467 23 -9 -1 -11 345.888 58.0445 10 9 0 -13 122.948 39.5221 9 9 0 -13 203.007 55.9366 11 -9 0 12 508.950 71.2294 24 9 0 -12 372.689 73.5845 11 -9 0 11 681.933 89.6396 24 9 0 -11 478.363 88.1186 11 -9 0 10 557.656 94.2828 24 9 0 -10 612.933 107.374 11 -9 0 9 30.7618 61.8935 24 9 0 -9 113.887 55.9454 7 9 0 -9 131.764 80.7205 11 9 0 -8 6679.24 298.700 7 -9 0 8 6632.16 305.448 24 9 0 -8 6629.02 335.218 11 9 0 -7 2057.81 176.516 7 -9 0 7 2173.08 181.360 24 9 0 -7 2001.31 193.158 11 9 0 -6 8959.88 389.435 7 -9 0 6 9311.52 383.805 24 9 0 -6 8809.95 395.021 11 9 0 -5 5067.32 296.489 7 -9 0 5 5731.93 302.895 24 9 0 -5 5535.41 309.877 11 -9 0 4 146.678 85.9352 24 9 0 -4 275.849 95.1423 7 9 0 -4 370.854 89.1053 11 9 0 -3 7511.19 370.931 7 -9 0 3 7340.16 354.115 24 9 0 -3 6991.71 343.164 11 9 0 -2 7331.45 368.722 7 -9 0 2 7719.75 354.204 24 9 0 -2 6991.05 339.356 11 9 0 -1 9931.12 427.863 7 -9 0 1 9383.86 393.342 24 -9 0 0 6262.33 294.501 10 9 0 0 6769.07 353.622 7 -9 0 0 6616.54 325.324 24 -9 0 -1 15388.6 503.045 10 9 0 1 16207.0 549.454 7 -9 0 -1 17017.5 533.496 24 -9 0 -2 142.822 59.9392 10 -9 0 -2 150.299 79.7960 24 9 0 2 101.730 66.1498 7 -9 0 -3 2421.30 198.814 10 9 0 3 2364.20 197.545 7 -9 0 -3 2804.62 197.097 24 -9 0 -4 8182.96 366.624 10 9 0 4 8337.85 359.054 7 -9 0 -4 8927.43 342.866 24 -9 0 -5 1521.24 164.194 10 -9 0 -5 1618.30 138.045 24 9 0 5 1465.04 147.247 7 -9 0 -6 11934.5 440.864 10 -9 0 -6 11267.0 451.150 15 -9 0 -7 2229.16 182.845 10 -9 0 -7 2345.35 196.213 15 -9 0 -8 347.936 76.5887 10 -9 0 -8 568.812 102.577 15 -9 0 -8 522.868 87.3348 14 -9 0 -9 1208.35 128.473 10 -9 0 -9 1223.61 124.165 15 -9 0 -9 1234.65 106.810 14 -9 0 -10 19777.6 508.481 10 -9 0 -10 18770.6 483.465 15 -9 0 -11 788.731 82.0047 15 9 0 11 580.213 77.3179 23 9 1 -13 845.310 82.8136 11 -9 1 12 3444.95 165.606 25 9 1 -12 3820.00 190.577 11 -9 1 11 3246.31 172.084 25 9 1 -11 3501.60 197.637 11 -9 1 10 695.084 100.571 25 -9 1 10 734.423 86.9938 24 9 1 -10 842.396 112.233 11 9 1 -9 12345.8 368.538 7 -9 1 9 11227.4 373.844 25 -9 1 9 11966.7 371.728 24 9 1 -9 12566.6 420.809 11 -9 1 8 617.271 92.3588 25 -9 1 8 655.363 99.6849 24 9 1 -8 489.140 86.2936 7 9 1 -8 606.078 109.170 11 9 1 -7 6568.81 302.674 7 -9 1 7 6607.97 288.385 25 -9 1 7 7168.81 305.993 24 9 1 -7 6896.37 318.469 11 9 1 -6 3855.08 243.543 7 -9 1 6 3872.61 221.013 25 -9 1 6 3666.30 230.961 24 9 1 -6 4295.64 255.945 11 9 1 -5 5582.48 303.294 7 -9 1 5 5562.74 263.423 25 -9 1 5 5096.92 279.996 24 9 1 -5 5593.81 286.402 11 9 1 -4 7714.20 365.661 7 -9 1 4 7862.59 353.512 24 9 1 -4 8401.75 354.913 11 -9 1 3 758.277 128.818 24 9 1 -3 358.618 91.6939 7 9 1 -3 584.122 98.7981 11 9 1 -2 2353.93 206.324 7 -9 1 2 2367.36 200.998 24 9 1 -1 6468.81 336.041 7 -9 1 1 7219.52 342.755 24 9 1 0 15582.8 534.879 7 -9 1 0 16142.7 532.035 24 9 1 1 12590.0 468.889 7 -9 1 -1 12584.6 461.060 24 9 1 2 4608.61 271.245 7 -9 1 -2 4609.57 270.919 24 9 1 3 16280.5 517.772 7 -9 1 -3 16991.4 527.775 24 9 1 4 3230.63 212.809 7 -9 1 -4 3078.04 208.063 24 -9 1 -5 163.673 70.4979 15 -9 1 -5 139.027 68.0241 24 9 1 5 239.121 70.6615 7 -9 1 -6 3148.35 227.841 15 -9 1 -6 3232.73 219.894 14 -9 1 -6 3462.96 196.074 24 -9 1 -7 1731.06 158.319 15 -9 1 -7 1698.03 152.417 14 -9 1 -7 2036.26 149.468 24 -9 1 -7 1815.70 148.223 12 -9 1 -8 11648.9 395.923 15 -9 1 -8 11913.7 391.069 14 -9 1 -8 11633.6 351.393 12 -9 1 -9 909.251 103.250 15 -9 1 -9 924.193 103.050 14 -9 1 -10 283.297 59.3724 15 -9 1 -10 324.300 55.1488 14 -9 1 -11 463.275 61.5278 15 -9 2 10 5869.08 222.714 25 9 2 -10 6172.11 227.774 11 -9 2 9 5765.36 234.150 25 9 2 -9 5824.66 236.059 11 9 2 -8 393.523 66.3313 11 -9 2 8 505.915 77.4664 25 9 2 -8 484.609 70.6389 7 9 2 -7 10601.3 350.811 7 -9 2 7 10844.3 355.309 25 -9 2 7 10822.4 325.624 24 9 2 -7 11097.4 353.173 11 9 2 -6 7849.21 314.708 7 -9 2 6 7815.11 304.453 25 -9 2 6 7814.59 288.065 24 9 2 -6 7771.35 293.998 11 9 2 -5 2026.63 164.146 7 -9 2 5 2596.83 173.042 25 -9 2 5 2339.81 165.487 24 9 2 -5 2356.46 157.751 11 -9 2 4 1790.77 148.726 25 -9 2 4 1541.80 142.999 24 9 2 -4 1426.31 151.880 7 -9 2 3 139.859 55.7282 25 -9 2 3 137.222 56.6371 24 9 2 -3 45.3694 62.6765 7 -9 2 2 827.734 114.542 24 9 2 -2 563.761 100.427 7 -9 2 1 5890.23 255.736 14 9 2 -1 5393.28 287.143 7 -9 2 1 5792.43 279.823 24 -9 2 0 17698.4 490.410 14 9 2 0 17306.8 530.055 7 -9 2 0 18050.6 523.152 24 -9 2 -1 6177.17 279.187 14 9 2 1 6276.84 302.439 7 -9 2 -1 7068.47 309.059 24 -9 2 -2 9705.83 356.790 14 9 2 2 9791.94 368.604 7 -9 2 -2 9610.42 364.122 24 -9 2 -3 16006.9 463.526 15 -9 2 -3 17486.8 498.249 14 9 2 3 17873.8 494.426 7 -9 2 -3 17259.4 496.958 24 -9 2 -4 2914.36 176.746 15 -9 2 -4 3011.73 190.585 14 9 2 4 2944.45 174.853 7 -9 2 -4 3057.91 191.033 24 -9 2 -5 2784.08 167.906 15 -9 2 -5 2793.77 183.161 14 -9 2 -5 3139.87 181.801 24 -9 2 -6 9381.23 293.715 15 -9 2 -6 9568.37 329.533 14 -9 2 -7 818.363 79.4859 15 -9 2 -7 981.607 101.447 14 -9 2 -7 901.877 89.5514 24 -9 2 -7 929.899 104.798 12 -9 2 -8 1849.30 127.914 14 -9 2 -8 1693.70 101.732 24 -9 2 -8 1573.44 119.371 12 -9 2 -9 4938.55 192.150 14 9 3 -5 35087.3 658.579 7 9 3 -4 11075.8 323.995 7 9 3 -3 1692.80 123.568 7 9 3 -2 7723.66 264.683 7 -9 3 2 4420.67 205.870 24 9 3 -1 3301.14 170.619 7 -9 3 1 2026.25 139.288 24 -9 3 0 175.689 54.9340 24 9 3 0 326.190 62.7028 7 -9 3 -1 115.255 45.0402 24 9 3 1 235.457 49.0488 7 9 3 2 2447.51 128.579 7 -9 3 -2 1648.85 131.786 24 -9 3 -3 338.369 59.5858 24 -9 3 -4 1135.92 97.6454 24 10 -2 -5 1491.51 102.367 7 10 -2 -4 2246.27 136.562 7 10 -2 -3 2200.24 143.648 7 10 -2 -2 11540.7 350.490 7 10 -2 -1 3995.13 196.395 7 10 -2 0 2028.83 141.668 7 10 -2 1 3175.81 168.519 7 10 -2 2 1227.44 101.544 7 10 -2 3 613.794 70.2464 7 10 -1 -9 10250.3 286.192 9 -10 -1 9 9700.40 276.086 24 10 -1 -9 9445.07 303.656 11 10 -1 -8 2520.05 143.803 9 -10 -1 8 2467.38 138.950 24 10 -1 -8 2365.57 159.310 11 10 -1 -7 7261.05 259.161 9 10 -1 -7 7147.15 245.087 7 -10 -1 7 6957.70 254.248 24 10 -1 -7 6749.33 282.331 11 10 -1 -6 63.9263 41.3392 9 10 -1 -6 147.157 57.0637 7 -10 -1 6 51.4355 47.6440 24 10 -1 -6 202.896 71.5424 11 10 -1 -5 470.160 72.0784 9 10 -1 -5 496.831 83.0630 7 -10 -1 5 514.651 80.1231 24 10 -1 -5 524.285 92.4891 11 10 -1 -4 514.488 68.5369 9 10 -1 -4 746.065 99.4100 7 -10 -1 4 623.475 83.8662 24 10 -1 -4 605.911 95.7830 11 10 -1 -3 4490.33 244.952 7 -10 -1 3 4538.45 211.150 24 -10 -1 2 1588.42 128.166 24 10 -1 -2 1393.88 143.732 7 10 -1 -1-8.84342 69.2298 7 -10 -1 1-0.23328 39.3081 24 10 -1 0 2891.60 196.516 7 -10 -1 -1 616.308 78.7157 10 10 -1 1 436.814 85.2155 7 -10 -1 -2 630.047 80.4308 10 10 -1 2 677.091 93.2954 7 -10 -1 -3 1005.58 100.327 10 -10 -1 -3 923.049 106.859 15 10 -1 3 1009.30 107.706 7 -10 -1 -4 2169.85 145.578 10 10 -1 4 1731.22 127.150 7 -10 -1 -5 220.140 57.2572 10 -10 -1 -5 187.699 49.3354 15 -10 -1 -6 6310.41 236.969 10 -10 -1 -6 6500.95 218.254 15 -10 -1 -7 6783.48 235.297 10 10 0 -10 829.157 86.8074 11 -10 0 9 34.1336 37.9812 24 10 0 -9 67.2075 46.3995 11 -10 0 8 592.383 77.5956 24 10 0 -8 369.356 69.0834 11 -10 0 7 332.456 72.0896 24 10 0 -7 383.607 70.9692 7 10 0 -7 427.597 85.7787 11 10 0 -6 6804.23 282.427 7 -10 0 6 6617.41 269.624 24 10 0 -6 6554.60 281.020 11 10 0 -5 5088.16 252.260 7 -10 0 5 5172.00 241.514 24 10 0 -5 5125.12 249.746 11 10 0 -4 2772.44 195.015 7 -10 0 4 2695.66 177.350 24 10 0 -4 2598.91 174.334 11 -10 0 3 1268.80 128.848 24 10 0 -3 1437.81 144.082 7 -10 0 2 442.324 88.4045 24 10 0 -2 496.791 101.633 7 10 0 -1 4166.54 243.656 7 -10 0 1 4302.64 224.398 24 10 0 0 6475.05 302.850 7 -10 0 0 6941.37 283.974 24 -10 0 -1 188.386 58.6256 24 10 0 1 159.927 65.6148 7 -10 0 -2 2563.21 162.962 10 10 0 2 2575.16 182.455 7 -10 0 -2 3051.35 174.473 24 -10 0 -3 559.919 79.8655 10 -10 0 -3 756.100 91.6460 24 10 0 3 521.127 94.3816 7 -10 0 -4 5919.36 253.177 10 -10 0 -4 5644.86 273.035 15 10 0 4 5846.45 245.397 7 -10 0 -5-7.54179 40.0417 10 -10 0 -5-2.49807 54.9316 15 -10 0 -6 7149.73 270.203 10 -10 0 -6 7392.35 282.549 15 -10 0 -6 6889.86 259.880 14 -10 0 -7 2078.37 136.748 15 -10 0 -7 1979.22 122.290 14 -10 0 -8 1133.68 93.0549 15 -10 1 8 2491.79 131.409 24 10 1 -8 2309.24 139.915 11 10 1 -7 7153.92 253.809 7 -10 1 7 7319.05 253.216 24 10 1 -7 6930.56 255.192 11 -10 1 6 237.605 65.5531 24 10 1 -6 205.357 61.0814 7 -10 1 5 603.115 80.9130 24 10 1 -5 434.152 81.7686 7 -10 1 4 648.546 91.2042 24 10 1 -4 446.675 79.1673 7 10 1 -3 4547.21 240.399 7 -10 1 3 4677.63 235.370 24 -10 1 2 1504.11 135.396 24 10 1 -2 1323.76 138.443 7 -10 1 1 35.9265 54.9847 24 10 1 -1 29.3448 54.9970 7 10 1 0 3242.30 205.956 7 -10 1 0 3532.35 204.449 24 -10 1 -1 561.562 90.4082 24 10 1 1 496.756 88.7718 7 -10 1 -2 787.171 94.7055 24 10 1 2 668.696 100.029 7 -10 1 -3 825.778 104.333 15 -10 1 -3 945.629 107.501 14 -10 1 -3 973.310 97.7011 24 10 1 3 900.553 103.947 7 -10 1 -4 1927.60 147.809 15 10 1 4 2060.27 133.800 7 -10 1 -4 2095.53 152.572 14 -10 1 -4 2364.75 142.309 24 -10 1 -5 325.611 71.4063 15 -10 1 -5 291.167 70.3464 14 -10 1 -5 209.389 47.5267 24 -10 1 -6 6698.25 249.053 15 -10 1 -6 6739.91 245.879 14 -10 1 -7 7345.02 242.788 15 -10 1 -7 7414.50 241.902 14 10 2 -5 1630.65 113.432 7 10 2 -4 2267.60 136.963 7 -10 2 4 2012.73 117.282 24 10 2 -3 2392.75 146.588 7 -10 2 3 2451.05 135.347 24 10 2 -2 11619.5 345.642 7 -10 2 2 11530.2 323.964 24 10 2 -1 3769.89 189.054 7 -10 2 1 4081.00 185.362 24 10 2 0 1972.45 136.618 7 -10 2 0 2322.23 140.425 24 10 2 1 3445.20 173.923 7 -10 2 -1 3578.25 169.933 24 10 2 2 1107.13 90.2603 7 -10 2 -2 1194.87 89.7184 14 -10 2 -2 1144.60 95.7366 24 -10 2 -3 700.853 68.7788 14 -10 2 -3 456.921 72.1573 24 -10 2 -4 248.389 51.7343 24 -11 0 3 30.3108 35.4111 24 11 0 -3-15.9083 36.2491 7 11 0 -2 59.1849 39.2039 7 11 0 -1 239.324 53.3691 7 11 0 0 943.749 84.3767 7 -11 0 -1 212.620 53.1446 15 0 0 0 0.00 0.00 0 TITL OGPALB in P2(1) REM P2(1) (#4 in standard setting) CELL 1.54184 8.922827 4.601228 17.453883 90.0000 92.9088 90.0000 ZERR 2.00 0.000144 0.000067 0.000313 0.0000 0.0015 0.0000 LATT -1 SYMM -x, y+1/2,-z SFAC C H O UNIT 28.00 40.00 16.00 TREF HKLF 4 END ; _shelx_hkl_checksum 62799 _olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount' _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 1.439 _oxdiff_exptl_absorpt_empirical_full_min 0.782 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.18704(18) 1.1767(4) 0.71057(10) 0.0185(4) Uani 1 1 d . . . . . H1A H -0.175833 1.028610 0.751602 0.022 Uiso 1 1 calc R . . . . H1B H -0.149762 1.364202 0.731836 0.022 Uiso 1 1 calc R . . . . O2 O -0.34221(13) 1.2047(3) 0.68693(7) 0.0199(3) Uani 1 1 d D . . . . H2 H -0.354700 1.355776 0.660333 0.030 Uiso 1 1 calc DGR . . . . C3 C -0.09373(18) 1.0891(4) 0.64405(9) 0.0136(3) Uani 1 1 d . . . . . H3 H -0.137670 0.911995 0.618424 0.016 Uiso 1 1 calc R . . . . O4 O -0.09796(13) 1.3267(3) 0.59158(7) 0.0154(3) Uani 1 1 d D . . . . H4 H -0.102(2) 1.263(5) 0.5473(11) 0.023 Uiso 1 1 d DR . . . . C5 C 0.06953(18) 1.0323(4) 0.67023(10) 0.0136(3) Uani 1 1 d . . . . . H5 H 0.110961 1.211802 0.695707 0.016 Uiso 1 1 calc R . . . . O6 O 0.07212(12) 0.8009(2) 0.72596(6) 0.0141(3) Uani 1 1 d . . . . . C7 C 0.16854(18) 0.9525(4) 0.60471(10) 0.0135(3) Uani 1 1 d . . . . . H7 H 0.178564 1.127853 0.571529 0.016 Uiso 1 1 calc R . . . . O8 O 0.10706(13) 0.7218(3) 0.55805(7) 0.0169(3) Uani 1 1 d D . . . . H8 H 0.050(2) 0.612(5) 0.5817(13) 0.025 Uiso 1 1 d DR . . . . C9 C 0.32462(19) 0.8712(4) 0.63816(10) 0.0148(3) Uani 1 1 d . . . . . H9 H 0.373612 1.048881 0.660921 0.018 Uiso 1 1 calc R . . . . O10 O 0.31280(13) 0.6559(3) 0.69751(7) 0.0155(3) Uani 1 1 d . . . . . C11 C 0.42357(18) 0.7476(4) 0.57840(10) 0.0179(3) Uani 1 1 d . . . . . H11A H 0.382528 0.557778 0.560756 0.021 Uiso 1 1 calc R . . . . H11B H 0.421767 0.879888 0.533631 0.021 Uiso 1 1 calc R . . . . O12 O 0.57516(14) 0.7089(3) 0.60666(8) 0.0230(3) Uani 1 1 d D . . . . H12 H 0.604(3) 0.861(5) 0.6289(14) 0.034 Uiso 1 1 d DR . . . . C13 C 0.22218(18) 0.7618(4) 0.75548(9) 0.0149(3) Uani 1 1 d . . . . . H13 H 0.262647 0.953671 0.773742 0.018 Uiso 1 1 calc R . . . . C17 C 0.25377(13) 0.1740(2) 0.94635(6) 0.0183(4) Uani 1 1 d . . . . . C18 C 0.11740(11) 0.3080(3) 0.92710(6) 0.0203(4) Uani 1 1 d G . . . . H18 H 0.032710 0.270628 0.956464 0.024 Uiso 1 1 calc R . . . . C19 C 0.10495(10) 0.4966(3) 0.86490(7) 0.0187(4) Uani 1 1 d G . . . . H19 H 0.011748 0.588190 0.851752 0.022 Uiso 1 1 calc R . . . . C14 C 0.22887(12) 0.5512(2) 0.82194(6) 0.0161(3) Uani 1 1 d G . . . . C15 C 0.36524(10) 0.4172(3) 0.84119(6) 0.0166(3) Uani 1 1 d G . . . . H15 H 0.449928 0.454579 0.811825 0.020 Uiso 1 1 calc R . . . . C16 C 0.37769(10) 0.2286(2) 0.90339(6) 0.0167(3) Uani 1 1 d G . . . . O20 O 0.50731(14) 0.0867(3) 0.92786(7) 0.0198(3) Uani 1 1 d . . . . . C21 C 0.6179(2) 0.0465(4) 0.87180(10) 0.0216(4) Uani 1 1 d . . . . . H21A H 0.569562 -0.030302 0.824363 0.032 Uiso 1 1 calc GR . . . . H21B H 0.694355 -0.091085 0.891558 0.032 Uiso 1 1 calc GR . . . . H21C H 0.665396 0.233329 0.861240 0.032 Uiso 1 1 calc GR . . . . O22 O 0.26341(15) -0.0163(3) 1.00685(8) 0.0225(3) Uani 1 1 d D . . . . H22 H 0.346(2) -0.109(6) 1.0051(15) 0.034 Uiso 1 1 d DR . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0142(8) 0.0240(10) 0.0173(8) 0.0016(7) 0.0007(6) 0.0029(7) O2 0.0136(6) 0.0196(6) 0.0266(7) 0.0051(6) 0.0022(5) 0.0025(5) C3 0.0139(7) 0.0119(8) 0.0148(8) 0.0017(6) -0.0013(6) -0.0006(6) O4 0.0183(6) 0.0140(6) 0.0139(6) 0.0013(5) -0.0006(4) 0.0008(5) C5 0.0151(7) 0.0111(7) 0.0144(7) 0.0020(6) -0.0020(6) 0.0001(6) O6 0.0142(5) 0.0133(6) 0.0146(6) 0.0025(5) -0.0018(4) 0.0012(5) C7 0.0132(7) 0.0116(8) 0.0155(8) 0.0006(6) -0.0011(6) -0.0018(6) O8 0.0189(6) 0.0174(6) 0.0144(5) -0.0022(5) 0.0007(4) -0.0042(5) C9 0.0150(8) 0.0111(8) 0.0181(8) 0.0031(7) -0.0012(6) -0.0010(6) O10 0.0164(5) 0.0129(6) 0.0171(6) 0.0027(5) 0.0004(4) 0.0023(5) C11 0.0132(7) 0.0173(8) 0.0232(8) 0.0028(7) 0.0007(6) 0.0019(7) O12 0.0142(6) 0.0188(6) 0.0359(7) -0.0005(6) 0.0004(5) 0.0028(5) C13 0.0150(7) 0.0138(8) 0.0155(8) -0.0014(7) -0.0027(6) -0.0001(7) C17 0.0248(9) 0.0156(8) 0.0140(8) 0.0006(7) -0.0036(6) -0.0017(7) C18 0.0202(8) 0.0219(9) 0.0191(8) 0.0004(7) 0.0019(6) -0.0009(7) C19 0.0191(8) 0.0184(9) 0.0182(8) -0.0003(7) -0.0027(6) 0.0015(7) C14 0.0207(8) 0.0131(8) 0.0139(8) -0.0021(7) -0.0035(6) -0.0009(7) C15 0.0193(8) 0.0151(8) 0.0151(8) 0.0000(7) -0.0020(6) -0.0023(7) C16 0.0198(8) 0.0140(8) 0.0157(8) -0.0019(7) -0.0041(6) 0.0004(7) O20 0.0191(6) 0.0223(7) 0.0178(6) 0.0032(5) -0.0012(5) 0.0045(5) C21 0.0228(9) 0.0232(9) 0.0189(8) 0.0003(8) 0.0011(7) 0.0046(7) O22 0.0246(6) 0.0230(7) 0.0199(6) 0.0075(6) 0.0005(5) 0.0027(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 1 0.0410 5 0 -1 0.0040 -5 0 -3 0.0068 0 -3 -1 0.0936 0 3 2 0.0952 0 0 -1 0.0050 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 O2 C1 C3 111.35(13) . . ? C1 C3 C5 111.64(13) . . ? O4 C3 C1 106.86(14) . . ? O4 C3 C5 108.50(13) . . ? O6 C5 C3 108.11(13) . . ? O6 C5 C7 109.75(13) . . ? C7 C5 C3 113.39(13) . . ? C13 O6 C5 108.70(12) . . ? C5 C7 C9 108.89(13) . . ? O8 C7 C5 112.69(13) . . ? O8 C7 C9 110.58(13) . . ? O10 C9 C7 110.13(13) . . ? O10 C9 C11 107.72(14) . . ? C11 C9 C7 112.40(14) . . ? C13 O10 C9 110.08(12) . . ? O12 C11 C9 112.64(14) . . ? O6 C13 C14 111.06(12) . . ? O10 C13 O6 110.28(12) . . ? O10 C13 C14 109.10(12) . . ? C18 C17 C16 120.0 . . ? O22 C17 C18 119.29(9) . . ? O22 C17 C16 120.69(9) . . ? C17 C18 C19 120.0 . . ? C18 C19 C14 120.0 . . ? C19 C14 C13 121.93(9) . . ? C15 C14 C13 118.04(9) . . ? C15 C14 C19 120.0 . . ? C14 C15 C16 120.0 . . ? C15 C16 C17 120.0 . . ? O20 C16 C17 115.18(9) . . ? O20 C16 C15 124.82(9) . . ? C16 O20 C21 116.43(12) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.4303(19) . ? C1 C3 1.517(2) . ? C3 O4 1.426(2) . ? C3 C5 1.527(2) . ? C5 O6 1.4415(19) . ? C5 C7 1.525(2) . ? O6 C13 1.4215(19) . ? C7 O8 1.430(2) . ? C7 C9 1.529(2) . ? C9 O10 1.441(2) . ? C9 C11 1.511(2) . ? O10 C13 1.413(2) . ? C11 O12 1.427(2) . ? C13 C14 1.5102(18) . ? C17 C18 1.3900 . ? C17 C16 1.3900 . ? C17 O22 1.3712(15) . ? C18 C19 1.3900 . ? C19 C14 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 O20 1.3770(14) . ? O20 C21 1.437(2) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O2 H2 O12 0.84 1.96 2.7898(18) 168.3 1_465 yes O4 H4 O8 0.825(19) 1.847(19) 2.6531(17) 165(3) 2_556 yes O8 H8 O4 0.844(19) 1.87(2) 2.6649(17) 156(2) 1_545 yes O12 H12 O2 0.83(2) 1.93(2) 2.7580(19) 175(3) 1_655 yes loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0.0009 0.0002 0.9997 0.0040 -0.0278 -0.0838 4.9986 -0.0017 -1.0006 -0.8573 0.1034 -0.0302 -5.0023 0.0009 -2.9983 0.8414 0.0079 0.3653 -0.0078 -2.9994 -1.0059 -0.1282 -0.9193 0.3937 0.0087 2.9996 2.0056 0.1322 0.8915 -0.4775 -0.0009 -0.0002 -0.9997 -0.0040 0.0278 0.0838