#------------------------------------------------------------------------------ #$Date: 2017-07-25 11:18:07 +0300 (Tue, 25 Jul 2017) $ #$Revision: 199045 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/10/80/2108052.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2108052 loop_ _publ_author_name 'Ikemoto, Kazuto' 'Mori, Shigeki' 'Mukai, Kazuo' _publ_section_title ; Synthesis and crystal structure of pyrroloquinoline quinol (PQQH~2~) and pyrroloquinoline quinone (PQQ) ; _journal_coeditor_code XK5034 _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 489 _journal_page_last 497 _journal_paper_doi 10.1107/S2052520617002281 _journal_volume 73 _journal_year 2017 _chemical_formula_moiety 'C14 H6 N2 O8, 3(C2 H6 O S)' _chemical_formula_sum 'C20 H24 N2 O11 S3' _chemical_formula_weight 564.59 _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' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_space_group_name_H-M 'P 21 21 21' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2016/6 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.901(5) _cell_length_b 12.371(8) _cell_length_c 28.674(18) _cell_measurement_reflns_used 7223 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.28 _cell_measurement_theta_min 2.17 _cell_volume 2448(3) _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_molecular_graphics 'CrystalStructure 4.2.4 (Rigaku, 2016)' _computing_publication_material 'CrystalStructure 4.2.4 (Rigaku, 2016)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SIR2011 (Burla, et al., 2012)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.111 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_number 41911 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.998 _diffrn_reflns_theta_min 2.175 _exptl_absorpt_coefficient_mu 0.366 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_correction_T_min 0.910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1176 _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.020 _refine_diff_density_max 1.428 _refine_diff_density_min -0.781 _refine_ls_abs_structure_details ; Flack x determined using 1648 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.12(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 337 _refine_ls_number_reflns 5885 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0698 _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^)+(0.0801P)^2^+4.9734P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1701 _refine_ls_wR_factor_ref 0.1852 _reflns_number_gt 4968 _reflns_number_total 5885 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file xk5034sup1.cif _cod_data_source_block II _cod_database_code 2108052 _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_min 0.982 _shelx_estimated_absorpt_t_max 0.993 _shelx_hkl_file ; 0 0 3 0.39 0.41 0 0 -3 -0.52 1.69 0 0 -3 -0.05 1.13 0 0 3 -1.25 1.63 0 0 -4 1.40 1.53 0 0 4 1.60 1.08 0 0 4 2.70 1.23 0 0 -4 1.25 1.24 0 0 4 0.94 0.62 0 0 -4 4.03 1.21 0 0 -4 3.02 1.67 0 0 4 2.48 2.07 0 0 -5 1.73 1.23 0 0 5 0.71 0.93 0 0 5 5.40 2.06 0 0 -5 1.31 2.54 0 0 5 2.09 1.55 0 0 -5 1.48 1.16 0 0 -5 3.37 1.63 0 0 5 2.80 2.03 0 0 -6 1760.87 58.17 0 0 6 1753.81 57.52 0 0 6 1793.37 58.90 0 0 -6 1594.21 52.41 0 0 6 1682.43 55.19 0 0 -6 1607.78 52.72 0 0 -6 1782.81 58.53 0 0 6 1730.73 56.93 0 0 -7 0.84 1.08 0 0 7 1.79 0.76 0 0 7 -4.95 6.72 0 0 -7 1.01 1.25 0 0 7 0.68 1.10 0 0 -7 -0.84 2.18 0 0 -7 4.84 2.92 0 0 7 1.57 1.80 0 0 -8 3132.95 102.67 0 0 8 2563.38 84.01 0 0 8 2765.67 90.75 0 0 -8 2609.54 85.60 0 0 8 2745.50 89.98 0 0 -8 2636.28 86.40 0 0 -8 2877.20 94.40 0 0 8 2701.01 88.63 0 0 -9 -3.76 2.64 0 0 9 -0.35 1.48 0 0 9 2.88 1.50 0 0 -9 -2.05 2.42 0 0 9 0.87 1.52 0 0 -9 0.63 1.34 0 0 -9 -1.95 3.86 0 0 9 -5.81 2.52 0 0 -10 5.17 3.70 0 0 10 7.81 2.80 0 0 10 3.24 5.21 0 0 -10 8.53 2.77 0 0 10 8.87 3.86 0 0 -10 6.25 2.15 0 0 -10 9.27 4.09 0 0 10 6.02 3.19 0 0 -11 1.25 1.66 0 0 11 2.67 0.56 0 0 11 6.56 3.63 0 0 -11 2.71 1.20 0 0 11 1.51 1.00 0 0 -11 -2.53 1.57 0 0 -11 1.34 2.72 0 0 11 -1.21 2.78 0 0 -12 1.22 1.02 0 0 12 0.72 1.16 0 0 12 -6.28 3.48 0 0 -12 -4.56 2.59 0 0 12 -0.03 2.79 0 0 -12 -2.32 1.56 0 0 -12 -4.32 3.58 0 0 12 -1.92 2.75 0 0 -13 1.14 1.00 0 0 13 -1.62 1.65 0 0 13 -1.64 3.40 0 0 13 1.63 1.42 0 0 -13 -1.22 1.81 0 0 -14 1714.71 102.42 0 0 14 1587.44 94.61 0 0 14 1428.76 85.10 0 0 14 1618.79 96.47 0 0 -14 1572.57 93.53 0 0 -14 1463.96 87.22 0 0 15 2.68 1.39 0 0 15 -5.03 4.77 0 0 -15 -1.92 1.75 0 0 -15 -1.97 3.88 0 0 16 730.88 12.21 0 0 16 763.02 15.98 0 0 16 811.58 14.35 0 0 -16 765.79 12.83 0 0 -16 741.83 17.82 0 0 -16 804.23 14.21 0 0 17 0.10 1.46 0 0 17 2.42 1.60 0 0 17 3.20 2.10 0 0 -17 1.81 1.83 0 0 -17 6.57 3.34 0 0 -17 -1.09 3.75 0 0 18 7.40 3.67 0 0 18 10.60 6.32 0 0 18 8.16 5.90 0 0 -18 14.90 8.77 0 0 -18 8.35 4.42 0 0 19 5.82 4.62 0 0 19 21.12 13.50 0 0 -19 3.43 3.61 0 0 -19 16.53 13.46 0 0 20 92.68 16.34 0 0 20 84.89 28.72 0 0 -20 100.56 19.02 0 0 -20 82.32 26.93 0 0 21 6.43 4.17 0 0 21 -7.16 4.38 0 0 -21 -0.95 4.53 0 0 -21 -1.70 4.20 0 0 22 165.86 4.57 0 0 22 199.78 6.96 0 0 -22 155.48 6.70 0 0 -22 175.69 11.32 0 0 23 3.97 3.19 0 0 23 -1.41 3.83 0 0 -23 4.05 4.24 0 0 -23 4.84 3.89 0 0 24 81.12 23.87 0 0 24 102.71 29.59 0 0 -24 74.90 28.91 0 0 -24 96.25 31.92 0 0 25 9.52 5.69 0 0 -25 -4.61 4.10 0 0 -25 3.65 3.29 0 0 26 853.59 112.14 0 0 -26 827.66 108.86 0 0 -26 843.38 110.83 0 0 27 2.64 2.36 0 0 27 -2.20 4.64 0 0 -27 10.67 6.52 0 0 -27 -10.89 4.98 0 0 28 4.00 2.71 0 0 28 9.24 6.06 0 0 -28 4.80 4.13 0 0 -28 -0.43 3.71 0 0 29 2.22 2.94 0 0 29 7.71 6.50 0 0 -29 -3.11 4.29 0 0 -29 -4.22 5.45 0 0 30 192.73 28.58 0 0 30 227.57 37.82 0 0 -30 220.13 31.08 0 0 -30 206.52 29.05 0 0 31 5.15 4.13 0 0 31 0.12 1.80 0 0 -31 5.19 5.03 0 0 -31 2.94 3.32 0 0 32 176.44 32.52 0 0 32 202.76 40.70 0 0 -32 154.05 32.89 0 0 -32 193.29 35.96 0 0 33 2.11 2.58 0 0 33 6.97 5.15 0 0 -33 4.37 5.30 0 0 -33 -3.68 5.60 0 0 34 254.86 44.41 0 0 -34 236.49 38.38 0 0 -34 299.30 48.42 0 0 35 3.84 5.11 0 0 -35 -2.05 4.72 0 0 36 88.28 20.03 0 0 -36 56.14 19.90 0 0 37 9.43 7.29 0 0 -37 3.19 4.91 0 0 38 33.66 12.60 0 0 -38 43.49 18.11 0 0 39 6.00 5.42 0 0 -39 3.38 4.65 0 -1 2 151.26 3.29 0 -1 -2 151.86 2.89 0 -1 -2 148.76 3.09 0 1 -2 132.31 3.62 0 1 -2 163.47 3.28 0 1 2 152.50 4.91 0 1 2 147.71 5.97 0 -1 2 177.52 4.52 0 1 -3 641.09 21.17 0 -1 3 605.92 20.13 0 1 3 571.28 18.87 0 -1 -3 619.23 20.44 0 1 3 578.78 19.14 0 -1 -3 629.38 20.77 0 -1 3 640.87 21.32 0 1 -3 598.21 19.85 0 -1 3 659.71 21.71 0 1 -3 674.66 22.17 0 -1 -3 601.50 20.12 0 1 3 611.38 20.37 0 -1 -3 600.55 23.63 0 1 -3 620.02 20.52 0 1 3 670.34 22.20 0 -1 3 689.14 22.72 0 1 -4 1274.83 41.92 0 -1 4 1284.34 42.15 0 1 4 1321.39 43.47 0 -1 -4 1300.82 42.67 0 1 4 1285.01 42.22 0 -1 -4 1315.54 43.23 0 -1 4 1259.11 41.44 0 1 -4 1347.91 44.34 0 -1 4 1253.34 41.09 0 1 -4 1287.36 42.20 0 -1 -4 1285.31 42.57 0 1 4 1257.72 41.52 0 1 -4 1323.66 43.67 0 -1 -4 1227.75 40.64 0 -1 4 1346.61 44.35 0 1 -5 505.51 16.85 0 -1 5 485.73 16.13 0 1 5 522.22 18.08 0 -1 -5 490.86 16.22 0 1 5 460.42 15.45 0 -1 -5 522.55 17.51 0 -1 5 553.55 18.60 0 1 -5 495.48 16.81 0 -1 -5 516.88 17.21 0 -1 5 490.95 16.20 0 1 -5 507.24 16.86 0 -1 -5 499.18 16.84 0 1 -5 492.51 18.61 0 -1 -5 483.46 17.22 0 1 5 579.27 19.73 0 -1 5 520.89 19.51 0 1 -6 2866.33 93.93 0 -1 6 3031.15 99.36 0 1 6 2861.51 93.74 0 -1 -6 2994.54 98.16 0 1 6 2983.68 97.76 0 -1 -6 2947.55 96.63 0 -1 6 2852.80 93.83 0 1 -6 3065.52 100.53 0 -1 -6 2910.31 95.38 0 -1 6 3038.21 99.51 0 1 -6 2917.19 95.55 0 -1 -6 2801.92 92.02 0 -1 -6 3003.25 98.56 0 1 -6 3166.13 103.81 0 1 6 3442.71 113.49 0 -1 6 2926.86 95.98 0 1 -7 508.21 17.26 0 -1 7 438.88 14.89 0 1 7 440.62 14.74 0 1 7 437.35 14.93 0 -1 -7 408.28 13.87 0 -1 7 442.12 14.93 0 1 -7 415.47 13.97 0 -1 -7 417.61 13.92 0 -1 7 402.27 14.43 0 1 -7 443.62 14.75 0 -1 -7 426.01 15.65 0 -1 -7 395.93 14.18 0 1 -7 437.04 14.91 0 1 7 429.89 15.45 0 -1 7 357.61 12.34 0 1 8 710.70 24.15 0 1 -8 620.80 20.72 0 -1 8 615.69 20.78 0 1 8 662.59 22.01 0 1 8 682.27 23.06 0 -1 -8 631.98 21.03 0 -1 8 701.14 23.72 0 1 -8 628.97 20.88 0 -1 -8 636.53 21.09 0 -1 8 640.48 21.13 0 1 -8 734.07 24.46 0 -1 -8 657.85 22.96 0 1 -8 659.88 22.33 0 -1 -8 657.64 22.03 0 1 8 687.69 22.88 0 -1 8 643.71 21.73 0 1 9 982.30 32.28 0 1 -9 1026.68 33.95 0 -1 9 944.78 31.12 0 1 9 969.67 32.02 0 1 9 1075.86 35.76 0 -1 -9 932.97 30.82 0 -1 9 975.37 32.52 0 1 -9 953.82 31.49 0 -1 -9 957.16 31.52 0 -1 9 950.50 31.27 0 1 -9 928.11 30.58 0 -1 -9 916.81 31.53 0 1 -9 1006.12 33.54 0 -1 -9 968.85 32.45 0 -1 9 948.39 31.43 0 1 10 358.96 12.09 0 1 -10 345.04 12.11 0 -1 10 323.72 10.88 0 1 10 354.99 14.26 0 1 10 385.77 18.25 0 -1 -10 344.60 11.87 0 -1 10 333.26 14.33 0 1 -10 358.97 12.52 0 -1 -10 329.63 11.09 0 -1 10 355.70 12.02 0 1 -10 347.43 12.54 0 -1 -10 347.04 15.69 0 -1 -10 336.56 12.44 0 1 -10 322.91 11.26 0 1 10 360.36 12.43 0 -1 10 367.42 12.79 0 1 11 4.81 1.93 0 1 -11 2.11 2.21 0 -1 11 2.45 1.68 0 1 11 5.48 2.81 0 1 11 4.16 2.97 0 -1 -11 6.17 2.39 0 -1 11 4.91 3.73 0 1 -11 -0.70 2.94 0 -1 11 -0.09 1.91 0 -1 -11 1.80 1.43 0 1 -11 2.45 2.68 0 -1 -11 -1.79 4.31 0 -1 -11 -4.33 4.80 0 1 -11 0.80 1.25 0 -1 11 7.76 3.43 0 1 11 1.71 2.95 0 1 -12 330.20 20.13 0 1 12 324.79 19.52 0 -1 12 291.41 18.08 0 1 12 326.74 20.11 0 1 12 326.52 19.93 0 -1 -12 309.66 18.79 0 -1 12 337.37 21.34 0 1 -12 311.32 19.29 0 -1 12 312.59 18.84 0 -1 -12 296.84 18.03 0 1 -12 311.81 18.65 0 -1 -12 315.00 21.07 0 1 -12 312.03 18.86 0 -1 -12 348.44 21.42 0 1 12 337.24 20.47 0 -1 12 302.63 18.26 0 1 -13 225.93 14.00 0 1 13 225.18 13.56 0 -1 13 206.35 12.59 0 1 13 240.55 14.90 0 1 13 232.04 14.82 0 -1 13 227.68 14.21 0 -1 13 225.18 14.85 0 -1 -13 232.02 14.53 0 1 -13 233.24 14.12 0 -1 -13 214.59 14.96 0 1 -13 232.68 14.72 0 -1 -13 226.88 19.72 0 1 -14 556.66 33.31 0 1 14 629.71 37.77 0 -1 14 572.24 34.16 0 1 14 588.44 35.27 0 1 14 587.56 35.28 0 -1 14 610.81 36.70 0 -1 14 578.93 34.58 0 -1 -14 527.02 31.50 0 1 -14 554.66 33.05 0 -1 -14 593.36 36.12 0 -1 -14 523.34 31.39 0 1 -14 485.51 29.17 0 1 -15 39.93 17.27 0 1 15 45.86 18.22 0 -1 15 37.94 16.24 0 1 15 38.85 17.83 0 1 15 35.63 17.80 0 -1 15 32.91 17.11 0 -1 15 40.69 17.52 0 -1 -15 34.83 13.69 0 1 -15 33.22 13.03 0 -1 -15 34.74 17.94 0 -1 -15 22.45 11.01 0 1 -15 39.52 18.73 0 1 -16 19.41 8.82 0 1 16 18.09 7.67 0 -1 16 19.45 7.92 0 1 16 23.27 10.82 0 1 16 17.69 8.16 0 -1 16 19.30 9.73 0 -1 16 22.36 9.38 0 1 -16 18.35 8.60 0 -1 -16 20.39 10.29 0 -1 -16 22.25 10.31 0 1 -16 13.79 7.72 0 1 -17 96.12 5.27 0 1 17 122.36 7.85 0 1 17 92.72 5.50 0 1 17 94.52 7.64 0 -1 17 102.49 6.61 0 -1 17 90.79 5.11 0 1 -17 93.36 4.87 0 -1 -17 86.90 5.69 0 1 -17 101.89 19.00 0 -1 -17 96.81 7.04 0 1 -18 -10.00 6.06 0 1 18 -0.35 0.81 0 1 18 1.19 1.45 0 1 18 -12.29 5.78 0 -1 18 -11.27 5.88 0 -1 18 -6.29 3.81 0 1 -18 0.56 0.66 0 -1 -18 1.66 2.31 0 -1 -18 -16.39 6.40 0 1 -18 -13.90 5.81 0 1 -19 90.65 18.02 0 1 19 47.03 21.69 0 1 19 55.01 5.04 0 1 19 76.96 18.60 0 -1 19 83.49 14.33 0 -1 19 94.84 12.87 0 1 -19 48.69 22.54 0 -1 -19 56.53 6.87 0 -1 -19 106.94 25.43 0 1 -19 98.25 16.56 0 1 -20 175.96 21.29 0 1 20 205.52 22.09 0 1 20 186.30 20.65 0 -1 20 187.70 20.60 0 -1 -20 204.29 22.47 0 1 -20 174.71 23.40 0 -1 -20 164.00 19.74 0 1 -21 59.26 13.11 0 1 21 59.62 15.14 0 1 21 48.35 11.26 0 -1 21 55.77 11.63 0 -1 -21 49.06 13.54 0 1 -21 51.59 15.70 0 -1 -21 47.73 12.93 0 1 -21 56.98 14.27 0 1 22 21.46 12.18 0 1 22 17.85 10.77 0 -1 22 17.29 11.62 0 -1 -22 16.39 10.91 0 1 -22 19.09 13.23 0 1 -22 22.36 13.19 0 -1 -22 16.01 10.07 0 1 23 47.96 12.17 0 -1 23 24.61 17.56 0 1 23 43.03 12.09 0 -1 23 27.42 15.83 0 1 -23 38.69 12.53 0 1 -23 25.93 15.82 0 -1 -23 39.57 13.15 0 1 24 1071.83 112.21 0 -1 24 1122.45 117.62 0 -1 -24 1202.82 126.26 0 1 -24 1044.85 109.65 0 -1 -24 685.53 71.93 0 1 25 1246.64 529.57 0 1 25 1239.44 526.54 0 -1 25 1267.59 538.50 0 -1 -25 1128.85 118.38 0 1 -25 1213.35 515.47 0 1 -25 1176.14 123.19 0 -1 -25 1074.17 112.54 0 1 26 180.46 23.99 0 -1 26 162.93 21.84 0 1 26 159.95 24.20 0 -1 26 186.56 25.44 0 -1 -26 169.93 23.49 0 1 -26 162.48 22.04 0 1 -26 156.11 25.90 0 -1 -26 195.90 32.14 0 1 27 43.40 15.96 0 -1 27 42.55 16.05 0 1 27 38.33 15.68 0 -1 27 39.89 15.24 0 -1 -27 35.75 15.55 0 1 -27 38.72 14.75 0 -1 -27 39.35 17.30 0 1 -27 35.80 15.78 0 1 28 -0.58 2.17 0 -1 28 8.61 6.57 0 1 28 2.53 3.71 0 -1 28 -4.62 5.09 0 -1 -28 5.63 5.21 0 1 -28 4.27 3.56 0 -1 -28 9.08 6.98 0 1 -28 2.85 5.18 0 1 29 2.15 3.10 0 -1 29 5.90 5.57 0 1 29 6.07 5.67 0 -1 29 3.14 3.48 0 -1 -29 5.72 5.28 0 1 -29 4.15 4.36 0 1 -29 0.95 3.66 0 -1 -29 3.20 3.59 0 1 30 12.83 9.74 0 -1 30 12.20 10.12 0 1 30 17.18 12.48 0 -1 30 30.68 23.02 0 -1 -30 16.94 13.24 0 1 -30 10.90 8.76 0 1 -30 18.46 15.36 0 -1 -30 10.76 8.79 0 1 31 15.07 10.01 0 -1 31 5.26 4.60 0 1 31 6.94 7.05 0 -1 31 1.70 3.95 0 -1 -31 10.82 9.61 0 1 -31 13.34 9.13 0 -1 -31 9.72 10.84 0 1 -31 -1.99 4.87 0 1 32 153.06 28.18 0 -1 32 168.71 31.14 0 1 32 167.59 31.10 0 -1 32 135.75 27.37 0 -1 -32 144.10 31.11 0 1 -32 170.45 31.64 0 1 -32 159.26 29.67 0 -1 -32 232.55 43.47 0 -1 33 39.93 45.47 0 1 33 24.84 16.55 0 -1 33 45.49 14.54 0 -1 -33 21.12 13.71 0 1 -33 22.46 15.12 0 -1 -33 31.83 20.47 0 -1 34 -3.69 2.72 0 1 34 4.06 5.11 0 -1 34 2.10 5.16 0 -1 -34 2.99 4.43 0 -1 -34 2.89 4.57 0 1 -34 0.39 2.72 0 1 35 12.49 8.67 0 -1 35 6.16 7.73 0 -1 -35 4.91 6.04 0 -1 -35 2.68 4.54 0 1 -35 0.09 3.84 0 1 36 47.02 16.51 0 -1 36 40.63 15.71 0 -1 -36 49.59 21.86 0 1 -36 51.34 21.31 0 1 37 -0.69 5.05 0 -1 37 -1.36 3.25 0 -1 -37 5.47 6.90 0 1 -37 2.81 5.49 0 1 38 -0.13 4.66 0 -1 38 6.90 5.92 0 -1 -38 -0.05 4.92 0 1 -38 5.36 5.56 0 1 39 21.71 15.85 0 -1 39 25.30 18.89 0 1 -39 37.03 23.14 0 -1 -39 34.12 22.25 0 2 0 8.31 2.52 0 -2 0 5.14 2.09 0 2 0 11.49 3.29 0 -2 0 10.78 2.93 0 -2 0 18.30 5.85 0 2 0 5.50 2.44 0 2 -1 160.76 3.30 0 -2 1 162.05 3.71 0 2 1 175.66 3.72 0 -2 -1 169.27 3.71 0 2 -1 144.11 3.85 0 -2 1 159.90 5.88 0 2 1 172.07 4.30 0 -2 -1 170.08 4.32 0 -2 1 164.96 13.25 0 2 -1 185.59 6.96 0 -2 -1 156.23 4.73 0 2 1 168.01 9.89 0 -2 1 161.23 3.00 0 2 -2 172.40 4.03 0 -2 2 173.09 3.75 0 2 2 178.61 3.73 0 -2 -2 175.01 3.62 0 2 2 185.49 3.92 0 -2 -2 185.83 4.67 0 2 -2 169.31 4.99 0 -2 2 182.36 5.32 0 2 -2 182.10 6.14 0 -2 -2 187.69 5.75 0 2 2 184.82 6.66 0 -2 -2 176.21 3.42 0 2 -2 158.33 3.31 0 2 2 180.33 3.51 0 -2 2 173.52 3.34 0 2 -3 1961.05 64.32 0 -2 3 2279.38 74.73 0 2 3 2269.15 74.34 0 -2 -3 2259.79 74.05 0 2 3 2424.84 79.51 0 -2 -3 2330.13 76.41 0 -2 3 2078.77 68.23 0 2 -3 2495.26 81.94 0 -2 3 2242.41 73.51 0 2 -3 2555.02 83.74 0 -2 -3 2386.13 78.55 0 2 3 2280.97 75.12 0 -2 -3 2414.00 79.09 0 2 -3 2330.50 76.40 0 2 3 2416.03 79.15 0 -2 3 2519.23 82.55 0 2 -4 60.04 2.49 0 -2 4 63.68 2.43 0 2 4 65.22 2.17 0 -2 -4 63.25 1.90 0 2 4 73.80 4.02 0 -2 -4 69.03 5.13 0 -2 4 77.61 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63.45 23.94 0 10 28 91.21 21.23 0 -10 28 97.07 19.79 0 -10 -28 91.50 20.51 0 10 -28 84.75 19.16 0 10 -29 2.74 3.18 0 10 29 5.05 6.32 0 -10 29 5.86 8.14 0 -10 -29 1.52 7.55 0 10 -29 3.56 4.01 0 10 -30 2.32 3.59 0 10 30 19.94 15.93 0 -10 30 -0.39 5.43 0 -10 -30 -13.72 7.76 0 10 -30 1.49 2.50 0 10 -31 5.29 5.49 0 10 31 -3.34 4.48 0 -10 31 1.51 3.03 0 -10 -31 2.46 5.23 0 10 -31 -0.88 2.76 0 10 -32 44.54 20.02 0 10 -32 48.28 24.43 0 10 -33 5.10 5.67 0 10 -33 -0.78 2.58 0 10 -34 6.11 6.51 0 11 0 7.52 4.89 0 -11 0 -17.13 6.64 0 -11 0 6.42 3.76 0 11 -1 109.86 27.05 0 11 1 88.47 20.59 0 11 1 103.25 30.33 0 -11 1 82.34 28.06 0 -11 1 105.43 24.33 0 -11 -1 96.25 30.59 0 11 -2 785.20 103.07 0 11 2 749.32 98.73 0 11 2 799.73 105.06 0 -11 2 654.90 86.36 0 -11 2 742.42 97.59 0 -11 -2 719.17 95.68 0 11 -3 115.35 29.07 0 11 3 105.15 26.26 0 11 3 121.44 27.68 0 -11 3 96.03 22.55 0 -11 3 95.09 28.67 0 -11 -3 80.88 19.48 0 11 -4 4.67 2.65 0 11 4 3.15 1.90 0 11 4 -0.80 3.98 0 -11 4 13.50 8.12 0 -11 4 -0.61 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0 -12 3 100.14 14.87 0 -12 -3 84.90 24.13 0 12 -4 38.18 15.99 0 12 4 39.26 16.69 0 12 4 35.63 14.92 0 -12 4 20.82 11.42 0 -12 4 29.19 12.05 0 -12 -4 30.82 15.59 0 12 -5 10.67 7.79 0 12 5 4.06 3.92 0 12 5 5.80 6.08 0 -12 5 4.53 7.60 0 -12 5 6.15 4.57 0 -12 -5 -3.13 8.00 0 12 -6 -2.45 3.47 0 12 6 4.50 3.73 0 12 6 -1.84 4.83 0 -12 6 -3.12 3.91 0 -12 6 3.94 4.31 0 -12 -6 1.62 5.85 0 12 -7 277.87 37.27 0 12 7 281.43 37.56 0 12 7 285.13 38.42 0 -12 7 241.33 37.65 0 -12 7 264.62 35.74 0 -12 -7 281.24 52.37 0 12 -8 1.67 3.12 0 12 8 3.30 3.03 0 12 8 3.84 4.47 0 -12 8 9.62 10.20 0 -12 8 2.92 2.37 0 -12 -8 7.23 9.57 0 12 -9 41.22 20.61 0 12 9 47.24 17.26 0 12 9 46.15 22.78 0 -12 9 41.58 18.51 0 -12 9 43.24 18.60 0 -12 -9 40.29 21.25 0 12 -10 1.37 3.06 0 12 10 7.88 6.21 0 12 10 2.19 2.34 0 -12 10 8.34 7.49 0 -12 10 6.11 4.00 0 -12 -10 7.93 8.93 0 12 -11 4.32 4.09 0 12 11 -0.14 2.05 0 12 11 6.90 5.36 0 -12 11 8.53 8.04 0 -12 11 -3.27 3.14 0 -12 -11 9.60 8.90 0 12 -12 4.35 4.53 0 12 12 7.05 4.77 0 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24.39 0 -13 5 17.63 13.00 0 -13 -5 23.81 18.46 0 13 -6 160.98 33.40 0 13 6 170.58 32.63 0 13 6 186.92 40.78 0 -13 6 120.92 26.37 0 -13 6 170.48 34.11 0 -13 -6 167.07 33.59 0 13 -7 3.94 4.93 0 13 7 1.32 1.81 0 13 7 -6.22 5.41 0 -13 7 -0.56 4.59 0 -13 7 10.62 7.61 0 -13 -7 3.51 5.79 0 13 -8 10.24 7.88 0 13 8 6.83 5.19 0 13 8 12.63 9.34 0 -13 8 -3.28 7.13 0 -13 8 15.80 10.33 0 -13 -8 13.88 10.49 0 13 -9 10.58 9.59 0 13 9 2.97 2.76 0 13 9 5.07 5.57 0 -13 9 26.14 17.05 0 -13 9 6.90 5.99 0 -13 -9 19.20 15.66 0 13 -10 165.20 31.03 0 13 10 122.08 22.95 0 13 10 147.70 27.61 0 -13 10 161.82 37.17 0 -13 10 145.11 30.35 0 -13 -10 116.37 41.77 0 13 -11 209.25 40.27 0 13 11 172.40 31.67 0 13 11 193.83 35.89 0 -13 11 192.18 40.00 0 -13 11 187.24 34.44 0 -13 -11 158.98 43.38 0 13 -12 3.67 5.44 0 13 12 11.39 8.97 0 13 12 -1.54 3.45 0 -13 12 5.79 8.44 0 -13 12 7.33 8.24 0 -13 -12 10.38 8.51 0 13 -13 2.43 3.27 0 13 13 -5.91 2.23 0 13 13 3.77 5.91 0 -13 13 5.62 8.75 0 -13 -13 -10.96 8.08 0 13 -14 20.45 15.74 0 13 14 26.29 15.60 0 13 14 34.34 21.41 0 -13 14 30.89 21.08 0 -13 -14 30.62 20.79 0 13 -15 8.17 5.67 0 13 15 8.28 4.54 0 13 15 6.09 5.33 0 -13 15 3.69 4.83 0 -13 -15 -3.35 8.71 0 13 -16 24.71 16.35 0 13 16 31.09 17.91 0 -13 16 22.25 14.37 0 -13 -16 49.60 11.71 0 13 -17 -3.15 4.66 0 13 17 4.94 6.96 0 -13 17 11.15 8.87 0 -13 -17 9.05 9.80 0 13 -18 2.83 4.39 0 13 18 1.23 4.72 0 -13 18 4.18 7.94 0 -13 -18 6.77 9.64 0 13 -19 1.41 2.62 0 13 19 7.20 5.87 0 -13 19 12.56 9.19 0 -13 -19 6.34 8.70 0 13 -20 23.85 14.65 0 13 20 30.44 7.85 0 -13 20 26.11 16.25 0 -13 -20 27.91 17.33 0 13 -21 39.70 17.83 0 13 21 31.94 15.41 0 -13 21 26.78 15.75 0 -13 -21 35.59 14.74 0 13 -22 286.44 329.19 0 13 22 201.29 53.57 0 -13 22 226.82 61.78 0 -13 -22 86.52 47.00 0 13 -23 4.14 4.31 0 13 23 12.41 9.36 0 -13 23 6.98 8.81 0 -13 -23 2.90 10.93 0 13 -24 26.28 15.30 0 13 24 30.97 19.24 0 -13 24 21.96 12.76 0 -13 -24 23.85 15.27 0 13 -25 11.44 10.02 0 13 25 8.27 7.76 0 -13 -25 20.03 20.24 0 14 0 98.18 22.64 0 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-8 116.40 4.96 1 -3 8 102.59 2.72 -1 3 8 111.35 4.20 1 -3 8 117.91 3.51 1 -3 -9 218.52 13.41 -1 -3 9 232.90 14.25 -1 3 -9 221.87 15.03 -1 3 -9 235.97 14.71 1 3 9 221.68 13.24 1 -3 -9 237.66 14.51 1 -3 -9 213.11 12.88 -1 3 -9 233.81 14.19 1 -3 -9 246.52 16.32 1 3 9 237.87 14.67 -1 -3 9 215.54 13.16 1 3 9 227.05 13.86 -1 -3 9 226.16 14.03 -1 3 -9 223.54 13.74 1 3 -9 240.27 17.70 -1 3 9 227.44 14.00 -1 -3 -9 239.02 16.75 1 -3 9 245.97 15.47 1 -3 9 231.07 18.79 -1 3 9 239.51 17.98 1 3 -9 226.51 13.91 -1 -3 -9 228.46 19.53 -1 -3 -9 228.47 13.98 1 3 -9 251.72 15.48 -1 3 9 247.51 15.01 -1 3 9 246.68 21.49 1 -3 9 224.36 13.54 -1 -3 -9 228.69 14.40 1 -3 9 221.65 13.63 -1 -3 -9 224.60 13.45 -1 -3 10 1215.48 72.37 -1 -3 10 1253.63 74.63 -1 3 -10 1280.36 76.23 1 3 10 1374.35 81.81 1 3 10 1261.31 74.94 -1 3 -10 1276.66 76.13 1 -3 -10 1298.36 77.29 -1 -3 10 1384.63 82.51 -1 3 -10 1312.06 78.17 1 -3 -10 1312.57 78.18 1 -3 -10 1282.71 76.38 1 3 10 1293.17 77.03 1 -3 -10 1353.40 81.00 -1 3 -10 1270.28 75.70 1 -3 10 1338.36 79.64 1 -3 10 1311.30 78.25 1 -3 10 1315.59 78.39 -1 3 10 1320.68 78.64 -1 3 10 1217.13 73.95 1 3 -10 1223.96 72.98 -1 -3 -10 1269.67 75.59 1 3 -10 1283.37 76.97 -1 3 10 1290.75 77.14 1 3 -10 1342.05 79.98 -1 -3 -10 1362.02 81.41 -1 -3 -10 1309.98 78.48 1 -3 10 1278.82 76.12 -1 3 10 1328.01 79.04 -1 3 -11 2051.68 121.99 -1 3 -11 2086.63 124.42 1 -3 -11 2005.56 119.66 1 3 11 1828.04 108.61 -1 -3 11 1908.28 113.54 1 -3 -11 1878.20 111.72 1 -3 -11 2006.28 119.34 1 3 11 1989.24 118.33 -1 -3 11 2014.10 119.80 -1 3 -11 2072.96 123.34 1 3 11 1803.64 107.32 1 -3 11 2026.36 120.51 1 3 -11 1693.23 100.60 -1 3 11 1968.63 117.08 -1 3 11 1974.23 117.62 1 3 -11 1829.02 108.70 -1 -3 -11 1862.59 111.26 -1 3 11 1992.43 118.54 1 3 -11 1890.35 112.49 1 -3 11 1888.29 112.38 -1 3 11 1959.88 116.72 -1 -3 -11 2134.02 126.97 1 3 -11 1969.81 117.20 1 -3 11 1850.85 110.13 1 -3 11 1904.32 113.25 1 3 12 314.51 18.74 -1 3 -12 311.48 18.88 1 -3 -12 309.79 20.00 1 3 12 277.81 16.55 -1 -3 12 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26.25 -2 -2 0 920.65 30.24 2 -2 0 941.60 31.14 2 2 0 882.55 29.21 -2 -2 0 807.39 27.64 2 -2 0 871.73 29.14 -2 2 0 826.88 27.40 2 -2 0 868.24 29.07 2 2 0 838.89 27.76 -2 2 0 836.40 27.59 -2 -2 0 906.67 29.90 -2 -2 1 313.55 10.84 2 -2 -1 300.24 15.94 -2 2 -1 290.05 56.10 -2 -2 1 298.84 10.74 2 -2 -1 305.82 10.60 -2 -2 1 286.88 5.73 -2 -2 1 312.15 11.24 -2 -2 1 284.69 5.55 2 2 1 292.34 56.45 -2 2 -1 299.02 14.20 -2 -2 1 314.24 10.43 2 -2 -1 283.84 5.43 2 2 1 341.00 11.87 2 2 1 295.07 57.20 -2 2 -1 291.18 56.24 2 -2 1 300.54 12.56 2 2 -1 315.22 10.67 -2 -2 -1 335.51 11.43 -2 2 1 305.02 10.18 2 -2 1 316.26 11.70 2 -2 1 283.46 5.32 -2 2 1 286.45 6.71 -2 -2 -1 324.47 11.05 -2 -2 -1 298.10 9.92 2 2 -1 291.08 56.25 -2 2 1 316.69 11.00 -2 -2 -1 305.48 10.43 -2 2 1 281.24 5.39 -2 -2 -1 332.96 11.59 -2 -2 2 451.86 15.19 2 -2 -2 487.39 16.64 -2 -2 2 482.81 16.46 2 -2 -2 450.16 15.26 -2 2 -2 467.69 16.02 -2 -2 2 454.77 15.93 -2 -2 2 447.98 15.44 -2 -2 2 456.45 15.10 -2 2 -2 374.22 12.89 2 2 2 459.32 15.21 2 -2 -2 443.82 14.67 -2 2 -2 456.81 16.56 2 2 2 452.51 15.26 -2 -2 2 454.17 15.22 2 -2 -2 456.42 15.60 -2 2 2 480.11 19.20 2 -2 2 462.07 15.41 2 -2 2 460.02 15.25 -2 -2 -2 448.81 16.38 -2 2 2 463.68 15.37 2 -2 2 344.39 15.51 -2 2 2 435.50 14.90 -2 -2 -2 467.65 15.43 -2 -2 -2 454.10 15.15 2 -2 2 478.14 15.97 -2 2 2 463.83 15.45 2 2 -2 445.34 14.84 -2 -2 -2 472.01 16.19 -2 -2 -2 473.75 16.28 -2 2 -3 2001.94 65.71 -2 -2 3 1896.24 62.30 -2 2 -3 2027.02 66.61 -2 2 -3 1871.99 61.43 2 2 3 1895.01 62.29 2 -2 -3 1808.60 59.44 -2 2 -3 1819.35 59.84 -2 -2 3 1890.89 64.13 -2 -2 3 1927.54 63.25 2 2 3 1780.47 58.61 2 -2 -3 1829.08 59.96 2 -2 -3 1833.97 60.45 -2 -2 3 1846.25 60.60 -2 -2 3 1736.08 56.92 2 -2 -3 1832.46 60.27 -2 2 -3 1992.14 65.47 -2 -2 -3 1825.22 59.84 2 -2 3 1771.12 58.13 -2 2 3 1914.13 62.89 2 -2 3 1845.73 60.82 -2 2 3 1795.28 59.73 2 2 -3 1942.46 63.69 -2 2 3 1964.95 64.67 -2 -2 -3 2009.08 65.84 -2 -2 -3 1917.18 62.93 2 -2 3 1890.45 62.12 2 2 -3 1984.58 65.20 -2 2 3 1899.44 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26.01 13.52 -9 4 1 24.41 14.97 -9 4 -2 4.23 3.81 9 4 2 1.86 2.46 -9 -4 2 -2.14 2.66 9 -4 -2 -1.49 4.23 -9 -4 2 0.39 3.49 -9 4 -2 7.33 6.35 9 -4 2 -1.99 3.66 -9 4 2 8.06 6.54 -9 -4 -2 0.51 4.64 -9 4 2 -2.12 3.78 -9 4 -3 9.35 7.20 9 4 3 5.07 5.15 -9 -4 3 2.63 3.49 9 -4 -3 4.44 4.60 -9 -4 3 7.73 7.30 -9 4 -3 2.29 5.54 9 -4 3 3.09 4.94 -9 4 3 6.64 6.39 -9 -4 -3 6.92 6.88 -9 4 3 2.75 4.10 -9 4 -4 2.87 4.62 -9 4 -4 2.03 4.99 -9 -4 4 4.38 4.02 9 4 4 2.54 3.81 -9 -4 4 8.80 7.49 9 -4 -4 6.09 5.34 -9 4 4 4.14 4.93 -9 -4 -4 8.14 7.39 -9 4 4 35.28 23.74 9 -4 4 12.97 9.71 -9 4 -5 9.70 8.36 9 4 5 5.43 5.33 -9 -4 5 6.05 5.30 9 -4 -5 9.96 8.29 -9 -4 5 7.53 7.75 -9 4 -5 6.08 7.89 9 -4 5 12.59 9.45 -9 4 5 9.99 8.57 -9 -4 -5 6.51 6.76 -9 4 5 6.49 7.65 -9 4 -6 8.29 7.38 9 4 6 2.09 3.30 -9 -4 6 7.61 6.99 9 -4 -6 10.71 8.68 -9 -4 6 0.07 2.29 -9 4 -6 6.07 7.86 -9 -4 -6 19.98 14.57 -9 4 6 9.40 7.97 -9 4 6 8.43 7.28 9 -4 6 6.77 6.56 -9 4 -7 5.24 4.89 -9 4 -7 16.62 13.75 -9 -4 7 7.03 6.14 9 4 7 3.11 4.19 -9 -4 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5.49 -9 -5 2 3.31 4.84 9 -5 -2 6.85 6.99 -9 -5 -2 14.55 11.21 -9 5 2 9.17 8.52 -9 5 2 -4.10 4.66 9 -5 2 5.50 5.17 -9 5 -3 5.60 5.06 -9 -5 3 10.87 8.83 9 5 3 12.72 8.93 -9 5 -3 27.03 13.04 9 -5 -3 9.66 7.64 -9 5 3 8.09 7.67 -9 -5 -3 10.57 8.36 -9 5 3 8.04 7.57 9 -5 3 4.29 4.62 -9 5 -4 6.32 6.38 9 5 4 19.96 14.84 -9 -5 4 17.03 13.04 9 -5 -4 11.23 9.62 -9 -5 4 14.74 10.30 -9 5 -4 14.84 12.21 9 -5 4 17.12 13.51 -9 5 4 14.30 11.28 -9 -5 -4 10.58 7.98 -9 5 4 18.22 12.76 -9 5 -5 4.74 6.79 9 5 5 -1.55 2.72 -9 -5 5 3.28 2.36 9 -5 -5 -0.86 3.78 -9 -5 5 3.66 5.45 -9 5 -5 2.72 4.10 -9 -5 -5 -4.38 4.69 -9 5 5 1.19 2.92 -9 5 5 3.22 3.58 9 -5 5 3.52 3.37 -9 5 -6 3.77 4.83 9 5 6 0.58 1.87 -9 -5 6 0.85 1.61 9 -5 -6 -0.28 2.25 -9 -5 6 6.98 8.73 -9 5 -6 2.55 1.37 9 -5 6 -4.27 4.87 -9 5 6 4.75 6.44 -9 -5 -6 -0.90 4.55 -9 5 6 1.07 3.00 -9 5 -7 4.06 5.30 -9 5 -7 4.26 7.04 -9 -5 7 -1.62 3.13 9 5 7 1.80 1.96 9 -5 -7 6.48 6.72 -9 -5 7 6.14 6.39 -9 -5 -7 -6.16 4.57 -9 5 7 0.31 3.36 -9 5 7 2.79 2.06 -9 5 -8 10.58 8.34 -9 -5 8 -0.11 3.04 9 5 8 3.72 5.32 9 -5 -8 4.27 5.73 -9 5 -8 -0.29 5.16 -9 -5 8 6.17 6.41 -9 -5 -8 8.12 7.33 -9 5 8 6.58 6.94 -9 5 -9 56.57 25.49 -9 -5 9 21.17 18.73 9 5 9 20.02 17.31 9 -5 -9 22.84 19.13 9 5 -9 9.27 25.66 -9 -5 -9 34.45 22.81 -9 5 9 29.90 18.35 -9 5 -10 3.01 1.53 -9 -5 10 6.46 6.18 9 5 10 3.60 4.71 9 -5 -10 -4.16 3.11 -9 -5 -10 -2.97 4.20 -9 -5 11 3.22 3.74 9 5 11 1.83 1.81 9 -5 -11 -0.61 2.94 -9 -5 12 2.56 2.61 9 -5 -12 5.02 6.75 9 -5 -13 0.17 2.00 -9 6 0 1.47 2.37 9 -6 0 4.12 6.73 -9 -6 0 -9.05 3.75 -9 6 0 6.55 6.48 -9 6 -1 3.49 1.99 -9 -6 1 -0.31 3.84 9 -6 -1 9.26 8.41 -9 6 -1 5.37 5.80 -9 6 1 4.74 6.90 -9 -6 -1 2.07 3.48 -9 6 1 4.08 5.99 -9 6 -2 -2.51 2.93 -9 6 -2 1.51 3.62 9 -6 -2 -0.08 4.19 -9 -6 2 4.32 5.34 -9 -6 -2 1.00 3.50 -9 6 2 10.54 7.83 -9 6 2 -0.56 4.04 -9 6 -3 15.47 14.86 -9 -6 3 25.53 17.22 9 -6 -3 21.40 16.26 -9 6 -3 18.23 15.02 -9 -6 -3 31.23 14.59 -9 6 3 12.03 12.95 -9 6 3 25.76 20.54 -9 6 -4 -2.89 3.17 9 6 4 3.77 4.95 9 -6 -4 -0.96 4.03 -9 6 -4 -3.89 4.40 -9 -6 4 4.02 5.45 -9 6 4 7.92 7.19 -9 -6 -4 -5.28 3.84 -9 6 -5 12.78 9.91 9 6 5 5.33 5.84 9 -6 -5 7.19 6.90 -9 -6 5 7.98 8.05 -9 6 -5 10.71 7.59 -9 -6 -5 8.72 7.70 -9 6 5 9.19 8.81 -9 6 -6 10.77 9.28 -9 -6 6 4.74 6.15 9 6 6 2.10 2.51 9 -6 -6 1.99 3.09 -9 6 -6 18.67 12.01 -9 -6 6 4.48 5.65 -9 -6 -6 9.37 7.95 -9 6 6 5.86 6.11 -9 6 -7 19.43 14.47 -9 -6 7 9.44 9.81 9 6 7 20.12 13.50 9 -6 -7 24.09 16.73 -9 -6 7 22.50 14.36 -9 -6 -7 21.69 16.09 -9 6 7 28.32 16.61 -9 6 -8 1.12 2.23 -9 -6 8 1.52 2.34 9 6 8 1.25 1.75 9 -6 -8 -9.27 3.23 -9 -6 8 6.73 6.94 -9 -6 -8 8.11 7.10 -9 6 -9 -2.86 2.60 -9 -6 9 14.96 10.34 9 6 9 2.01 2.16 9 -6 -9 -0.61 3.24 -9 6 -10 8.67 8.29 -9 -6 10 10.23 7.08 9 6 10 9.46 8.39 9 -6 -10 2.05 2.79 -9 -6 11 1.58 1.50 9 6 11 -2.58 3.07 9 -6 -11 -2.01 2.94 9 -6 -12 7.25 6.13 -9 7 0 -7.42 3.64 -9 -7 0 -5.96 2.96 -9 7 -1 34.20 15.65 -9 -7 1 12.08 8.36 -9 -7 -1 22.27 14.97 -9 7 1 7.09 6.78 -9 7 -2 0.12 1.83 -9 -7 2 5.98 6.56 -9 -7 -2 13.66 9.34 -9 7 2 3.48 3.58 -9 7 -3 0.33 2.67 -9 -7 3 5.38 6.31 -9 -7 -3 6.40 6.18 -9 -7 4 5.67 7.82 -9 -7 -4 10.17 7.43 -9 -7 5 5.32 5.11 -9 -7 -5 -0.47 3.01 -9 -7 -6 11.84 9.06 9 7 7 -0.99 1.29 -9 -7 -7 8.77 7.98 9 7 8 -3.14 2.59 9 7 9 2.86 2.00 9 7 10 5.58 6.03 -9 -8 0 5.41 5.08 -9 -8 1 4.08 5.58 -9 -8 -1 3.22 1.84 -9 -8 2 -0.83 1.67 -9 -8 -2 7.08 6.06 -9 -8 -3 4.74 6.27 10 0 0 5.36 4.98 10 0 -1 1.28 1.97 10 0 1 3.79 4.81 -10 0 3 1.51 2.25 10 1 0 -1.71 2.85 10 -1 0 -0.99 3.35 10 -1 -1 67.70 30.46 10 1 1 93.03 40.26 -10 1 1 80.68 34.96 10 1 2 7.63 7.95 -10 1 2 13.74 11.06 10 -1 -3 7.36 6.28 10 1 3 3.47 4.58 -10 1 3 9.15 7.60 -10 -1 5 6.21 5.89 -10 2 0 -0.50 2.48 10 -2 -3 0.40 1.75 ; _shelx_hkl_checksum 29939 _shelx_res_file ; TITL ProfMukai shelxl.res created by SHELXL-2016/6 at 14:02:49 on 27-Apr-2017 CELL 0.71075 6.90090 12.37060 28.67350 90.000 90.000 90.000 ZERR 4 0.00450 0.00840 0.01820 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM 1/2+X, 1/2-Y, -Z SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O S UNIT 80 96 8 44 12 SHEL 99999.000000 0.756965 OMIT 3 0 25 OMIT -2 3 2 OMIT 2 1 6 OMIT -2 1 6 OMIT 2 3 2 OMIT 1 0 15 L.S. 20 FMAP 2 PLAN -5 WPDB -2 REM HTAB LIST 4 TEMP -173.0 ACTA BOND $H CONF SIZE 0.050 0.050 0.020 HTAB WGHT 0.080100 4.973400 FVAR 0.42007 N1 3 0.943978 0.846619 -0.059343 11.00000 0.02432 0.01745 = 0.02377 0.00318 0.00158 -0.00235 H1N 2 0.913936 0.906024 -0.039079 11.00000 -1.20000 C2 1 0.965259 0.849918 -0.107372 11.00000 0.02691 0.01667 = 0.02168 0.00062 -0.00218 0.00129 C3 1 0.986856 0.745900 -0.123473 11.00000 0.02364 0.01880 = 0.01932 0.00108 0.00102 0.00023 AFIX 43 H3 2 1.004371 0.724012 -0.154950 11.00000 -1.20000 AFIX 0 C3A 1 0.977738 0.677487 -0.083561 11.00000 0.01951 0.01939 = 0.01822 0.00048 -0.00410 0.00184 C4 1 0.982528 0.560493 -0.081015 11.00000 0.02417 0.01897 = 0.01782 -0.00149 -0.00174 0.00086 C5 1 0.945338 0.513428 -0.031232 11.00000 0.02543 0.01835 = 0.02210 -0.00229 -0.00059 0.00182 C5A 1 0.939909 0.589688 0.010078 11.00000 0.02037 0.01751 = 0.02027 0.00157 0.00076 -0.00034 N6 3 0.938704 0.539142 0.051505 11.00000 0.02389 0.01907 = 0.02254 0.00055 -0.00055 -0.00224 C7 1 0.949374 0.600951 0.089931 11.00000 0.02347 0.01789 = 0.01979 0.00227 -0.00026 0.00068 C8 1 0.959927 0.713969 0.087934 11.00000 0.02164 0.02051 = 0.02227 -0.00215 0.00487 -0.00195 AFIX 43 H8 2 0.972814 0.754651 0.115863 11.00000 -1.20000 AFIX 0 C9 1 0.951570 0.766728 0.045130 11.00000 0.02173 0.01843 = 0.02275 -0.00026 -0.00083 0.00126 C9A 1 0.944061 0.703118 0.003782 11.00000 0.01719 0.01687 = 0.02403 -0.00259 0.00148 0.00069 C1A 1 0.950138 0.743032 -0.043919 11.00000 0.02316 0.01405 = 0.02540 0.00024 -0.00201 -0.00227 C10 1 0.958755 0.956272 -0.130530 11.00000 0.03164 0.02275 = 0.02848 0.00377 0.00757 0.00418 C11 1 0.954380 0.543816 0.136689 11.00000 0.03067 0.02667 = 0.02190 0.00386 0.00031 -0.00145 C12 1 0.948384 0.889847 0.048025 11.00000 0.02919 0.01350 = 0.02206 0.00064 0.00309 0.00334 O1 4 0.924937 1.038399 -0.108784 11.00000 0.06664 0.02588 = 0.03689 0.00649 0.01615 0.01300 O2 4 0.990934 0.950563 -0.176097 11.00000 0.03772 0.02174 = 0.02477 0.00367 0.00184 -0.00170 AFIX 147 H2O 2 0.990325 1.013111 -0.187500 11.00000 -1.50000 AFIX 0 O3 4 1.008869 0.498927 -0.113518 11.00000 0.03816 0.02472 = 0.02364 -0.00711 0.00125 -0.00089 O4 4 0.919571 0.417346 -0.027317 11.00000 0.03730 0.01767 = 0.02723 -0.00253 -0.00216 -0.00190 O5 4 0.923375 0.446814 0.140376 11.00000 0.05236 0.01984 = 0.02731 0.00252 0.00010 -0.00010 O6 4 0.990505 0.609384 0.171409 11.00000 0.04306 0.02275 = 0.02137 0.00321 -0.00248 -0.00237 AFIX 147 H6O 2 0.990604 0.574423 0.196522 11.00000 -1.50000 AFIX 0 O7 4 0.850928 0.944890 0.020607 11.00000 0.02868 0.02110 = 0.02735 -0.00159 -0.00314 0.00318 O8 4 1.044940 0.927799 0.082210 11.00000 0.04614 0.01650 = 0.03278 -0.00471 -0.01254 0.00387 AFIX 147 H8O 2 1.001782 0.989128 0.089298 11.00000 -1.50000 AFIX 0 S1S 5 0.998523 1.237763 -0.178119 11.00000 0.04007 0.02978 = 0.02895 0.00326 -0.00170 -0.00685 C1SA 1 0.814623 1.328492 -0.195541 11.00000 0.08317 0.09788 = 0.14394 -0.08510 -0.06404 0.05198 AFIX 137 H1SA 2 0.688111 1.300080 -0.186011 11.00000 -1.20000 H1SB 2 0.817547 1.336838 -0.229521 11.00000 -1.20000 H1SC 2 0.836177 1.398896 -0.180755 11.00000 -1.20000 AFIX 0 C1SB 1 1.194215 1.316825 -0.196206 11.00000 0.07812 0.06992 = 0.12893 -0.05553 0.05696 -0.04504 AFIX 137 H1SD 2 1.175788 1.338065 -0.228833 11.00000 -1.20000 H1SE 2 1.314305 1.275098 -0.193257 11.00000 -1.20000 H1SF 2 1.202378 1.381684 -0.176680 11.00000 -1.20000 AFIX 0 O1S 4 0.990534 1.142620 -0.212346 11.00000 0.04849 0.02501 = 0.02507 0.00462 -0.00094 -0.00788 S2S 5 1.003891 0.402547 0.258918 11.00000 0.03405 0.04702 = 0.02353 0.01148 -0.00320 -0.00433 C2SA 1 0.809414 0.368676 0.296968 11.00000 0.03354 0.04721 = 0.03993 0.01296 -0.00703 -0.00512 AFIX 137 H2SA 2 0.821868 0.409741 0.326042 11.00000 -1.20000 H2SB 2 0.813356 0.291118 0.303868 11.00000 -1.20000 H2SC 2 0.685925 0.386517 0.281949 11.00000 -1.20000 AFIX 0 C2SB 1 1.193111 0.376663 0.299312 11.00000 0.03093 0.05514 = 0.02953 0.01230 0.00098 -0.00129 AFIX 137 H2SD 2 1.174405 0.421349 0.327172 11.00000 -1.20000 H2SE 2 1.318079 0.394221 0.284954 11.00000 -1.20000 H2SF 2 1.191343 0.300123 0.308118 11.00000 -1.20000 AFIX 0 O2S 4 0.996860 0.521351 0.251972 11.00000 0.05196 0.03984 = 0.02709 0.00090 -0.00383 -0.00347 S3S 5 0.989871 1.193529 0.053748 11.00000 0.03045 0.01862 = 0.02672 -0.00351 0.00010 -0.00232 C3SA 1 0.771053 1.265957 0.063988 11.00000 0.02689 0.02920 = 0.03515 0.00067 -0.00009 0.00083 AFIX 137 H3SA 2 0.780417 1.304637 0.093730 11.00000 -1.20000 H3SB 2 0.662183 1.215165 0.065177 11.00000 -1.20000 H3SC 2 0.750100 1.317939 0.038695 11.00000 -1.20000 AFIX 0 C3SB 1 1.162212 1.295504 0.064675 11.00000 0.02833 0.02279 = 0.04527 -0.00580 -0.00093 0.00060 AFIX 137 H3SD 2 1.292778 1.264513 0.063289 11.00000 -1.20000 H3SE 2 1.139876 1.326264 0.095709 11.00000 -1.20000 H3SF 2 1.149846 1.352457 0.041106 11.00000 -1.20000 AFIX 0 O3S 4 1.005075 1.119694 0.097754 11.00000 0.04227 0.01886 = 0.02654 -0.00040 -0.00422 0.00045 HKLF 4 REM ProfMukai REM R1 = 0.0698 for 4968 Fo > 4sig(Fo) and 0.0838 for all 5885 data REM 337 parameters refined using 0 restraints END WGHT 0.0802 4.9742 REM Instructions for potential hydrogen bonds HTAB N1 O7 HTAB O2 S1S HTAB O2 O1S HTAB O6 S2S HTAB O6 O2S HTAB O8 S3S HTAB O8 O3S EQIV $1 x, y+1, z HTAB C1SA O3_$1 EQIV $2 x-1/2, -y+3/2, -z HTAB C2SA O1S_$2 EQIV $3 x+1/2, -y+3/2, -z HTAB C2SB O1S_$3 HTAB C3SA O5_$1 HTAB C3SA O4_$2 HTAB C3SA O4_$1 HTAB C3SB O4_$3 HTAB C3SB O5_$1 HTAB C3SB O4_$1 REM Highest difference peak 1.428, deepest hole -0.781, 1-sigma level 0.105 Q1 1 0.9905 0.3682 0.2198 11.00000 0.05 1.43 Q2 1 0.9892 0.4555 0.2702 11.00000 0.05 0.92 Q3 1 1.1533 0.9456 0.0217 11.00000 0.05 0.74 Q4 1 1.0940 0.4188 -0.0292 11.00000 0.05 0.69 Q5 1 0.8172 1.2716 -0.1767 11.00000 0.05 0.53 ; _shelx_res_checksum 28943 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy N N1 0.9440(7) 0.8466(4) -0.05934(17) 0.0218(10) Uani d 1 H H1N 0.914(10) 0.906(6) -0.039(2) 0.026 Uiso d 1 C C2 0.9653(9) 0.8499(4) -0.10737(18) 0.0218(11) Uani d 1 C C3 0.9869(9) 0.7459(4) -0.12347(17) 0.0206(10) Uani d 1 H H3 1.004371 0.724012 -0.154950 0.025 Uiso calc 1 C C3A 0.9777(8) 0.6775(4) -0.08356(17) 0.0190(10) Uani d 1 C C4 0.9825(9) 0.5605(4) -0.08101(17) 0.0203(10) Uani d 1 C C5 0.9453(8) 0.5134(4) -0.03123(19) 0.0220(11) Uani d 1 C C5A 0.9399(8) 0.5897(4) 0.01008(18) 0.0194(10) Uani d 1 N N6 0.9387(7) 0.5391(4) 0.05150(16) 0.0218(9) Uani d 1 C C7 0.9494(8) 0.6010(4) 0.08993(18) 0.0204(11) Uani d 1 C C8 0.9599(8) 0.7140(4) 0.08793(19) 0.0215(11) Uani d 1 H H8 0.972814 0.754651 0.115863 0.026 Uiso calc 1 C C9 0.9516(8) 0.7667(4) 0.04513(19) 0.0210(11) Uani d 1 C C9A 0.9441(8) 0.7031(4) 0.00378(19) 0.0194(10) Uani d 1 C C1A 0.9501(8) 0.7430(4) -0.04392(19) 0.0209(11) Uani d 1 C C10 0.9588(9) 0.9563(5) -0.1305(2) 0.0276(13) Uani d 1 C C11 0.9544(9) 0.5438(5) 0.13669(19) 0.0264(13) Uani d 1 C C12 0.9484(8) 0.8898(4) 0.04803(19) 0.0216(11) Uani d 1 O O1 0.9249(9) 1.0384(4) -0.10878(17) 0.0431(13) Uani d 1 O O2 0.9909(8) 0.9506(3) -0.17610(13) 0.0281(8) Uani d 1 H H2O 0.990325 1.013111 -0.187500 0.042 Uiso calc 1 O O3 1.0089(8) 0.4989(3) -0.11352(13) 0.0288(9) Uani d 1 O O4 0.9196(7) 0.4173(3) -0.02732(15) 0.0274(9) Uani d 1 O O5 0.9234(8) 0.4468(3) 0.14038(15) 0.0332(11) Uani d 1 O O6 0.9905(8) 0.6094(3) 0.17141(13) 0.0291(9) Uani d 1 H H6O 0.990604 0.574423 0.196522 0.044 Uiso calc 1 O O7 0.8509(6) 0.9449(3) 0.02061(14) 0.0257(9) Uani d 1 O O8 1.0449(7) 0.9278(3) 0.08221(15) 0.0318(11) Uani d 1 H H8O 1.001782 0.989128 0.089298 0.048 Uiso calc 1 S S1S 0.9985(3) 1.23776(12) -0.17812(5) 0.0329(4) Uani d 1 C C1SA 0.8146(18) 1.3285(11) -0.1955(5) 0.108(6) Uani d 1 H H1SA 0.688111 1.300080 -0.186011 0.130 Uiso calc 1 H H1SB 0.817547 1.336838 -0.229521 0.130 Uiso calc 1 H H1SC 0.836177 1.398896 -0.180755 0.130 Uiso calc 1 C C1SB 1.1942(17) 1.3168(10) -0.1962(5) 0.092(5) Uani d 1 H H1SD 1.175788 1.338065 -0.228833 0.111 Uiso calc 1 H H1SE 1.314305 1.275098 -0.193257 0.111 Uiso calc 1 H H1SF 1.202378 1.381684 -0.176680 0.111 Uiso calc 1 O O1S 0.9905(8) 1.1426(3) -0.21235(13) 0.0329(10) Uani d 1 S S2S 1.0039(3) 0.40255(14) 0.25892(5) 0.0349(4) Uani d 1 C C2SA 0.8094(11) 0.3687(7) 0.2970(3) 0.0402(18) Uani d 1 H H2SA 0.821868 0.409741 0.326042 0.048 Uiso calc 1 H H2SB 0.813356 0.291118 0.303868 0.048 Uiso calc 1 H H2SC 0.685925 0.386517 0.281949 0.048 Uiso calc 1 C C2SB 1.1931(10) 0.3767(7) 0.2993(3) 0.0385(17) Uani d 1 H H2SD 1.174405 0.421349 0.327172 0.046 Uiso calc 1 H H2SE 1.318079 0.394221 0.284954 0.046 Uiso calc 1 H H2SF 1.191343 0.300123 0.308118 0.046 Uiso calc 1 O O2S 0.9969(9) 0.5214(4) 0.25197(15) 0.0396(11) Uani d 1 S S3S 0.9899(3) 1.19353(10) 0.05375(5) 0.0253(3) Uani d 1 C C3SA 0.7711(10) 1.2660(6) 0.0640(2) 0.0304(14) Uani d 1 H H3SA 0.780417 1.304637 0.093730 0.036 Uiso calc 1 H H3SB 0.662183 1.215165 0.065177 0.036 Uiso calc 1 H H3SC 0.750100 1.317939 0.038695 0.036 Uiso calc 1 C C3SB 1.1622(10) 1.2955(5) 0.0647(3) 0.0321(14) Uani d 1 H H3SD 1.292778 1.264513 0.063289 0.039 Uiso calc 1 H H3SE 1.139876 1.326264 0.095709 0.039 Uiso calc 1 H H3SF 1.149846 1.352457 0.041106 0.039 Uiso calc 1 O O3S 1.0051(8) 1.1197(3) 0.09775(13) 0.0292(9) Uani d 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.024(2) 0.017(2) 0.024(2) -0.0024(18) 0.0016(18) 0.0032(18) C2 0.027(3) 0.017(2) 0.022(2) 0.001(2) -0.002(2) 0.0006(19) C3 0.024(3) 0.019(2) 0.019(2) 0.000(2) 0.001(2) 0.0011(18) C3A 0.020(3) 0.019(2) 0.018(2) 0.002(2) -0.004(2) 0.0005(18) C4 0.024(3) 0.019(2) 0.018(2) 0.001(2) -0.002(2) -0.0015(18) C5 0.025(3) 0.018(2) 0.022(3) 0.002(2) -0.001(2) -0.002(2) C5A 0.020(2) 0.018(2) 0.020(2) -0.0003(19) 0.0008(19) 0.0016(19) N6 0.024(2) 0.019(2) 0.023(2) -0.0022(18) -0.0005(18) 0.0005(18) C7 0.023(3) 0.018(2) 0.020(2) 0.001(2) 0.000(2) 0.0023(19) C8 0.022(3) 0.021(2) 0.022(2) -0.002(2) 0.005(2) -0.002(2) C9 0.022(3) 0.018(2) 0.023(3) 0.001(2) -0.001(2) 0.000(2) C9A 0.017(2) 0.017(2) 0.024(2) 0.0007(19) 0.001(2) -0.003(2) C1A 0.023(3) 0.014(2) 0.025(3) -0.002(2) -0.002(2) 0.000(2) C10 0.032(3) 0.023(3) 0.028(3) 0.004(2) 0.008(2) 0.004(2) C11 0.031(3) 0.027(3) 0.022(2) -0.001(2) 0.000(2) 0.004(2) C12 0.029(3) 0.014(2) 0.022(2) 0.003(2) 0.003(2) 0.0006(19) O1 0.067(4) 0.026(2) 0.037(2) 0.013(2) 0.016(2) 0.006(2) O2 0.038(2) 0.0217(18) 0.0248(18) -0.002(2) 0.002(2) 0.0037(14) O3 0.038(2) 0.0247(19) 0.0236(18) -0.001(2) 0.001(2) -0.0071(14) O4 0.037(2) 0.0177(19) 0.027(2) -0.0019(17) -0.0022(18) -0.0025(16) O5 0.052(3) 0.020(2) 0.027(2) 0.000(2) 0.000(2) 0.0025(17) O6 0.043(3) 0.0227(19) 0.0214(17) -0.002(2) -0.002(2) 0.0032(14) O7 0.029(2) 0.021(2) 0.027(2) 0.0032(16) -0.0031(17) -0.0016(17) O8 0.046(3) 0.0165(19) 0.033(2) 0.0039(18) -0.013(2) -0.0047(16) S1S 0.0401(9) 0.0298(7) 0.0289(7) -0.0069(8) -0.0017(8) 0.0033(5) C1SA 0.083(9) 0.098(10) 0.144(12) 0.052(8) -0.064(8) -0.085(9) C1SB 0.078(8) 0.070(8) 0.129(11) -0.045(6) 0.057(7) -0.056(8) O1S 0.048(3) 0.0250(19) 0.0251(18) -0.008(2) -0.001(2) 0.0046(15) S2S 0.0341(8) 0.0470(9) 0.0235(6) -0.0043(8) -0.0032(7) 0.0115(6) C2SA 0.034(4) 0.047(4) 0.040(4) -0.005(3) -0.007(3) 0.013(4) C2SB 0.031(3) 0.055(5) 0.030(4) -0.001(3) 0.001(3) 0.012(3) O2S 0.052(3) 0.040(2) 0.027(2) -0.003(3) -0.004(2) 0.0009(17) S3S 0.0304(7) 0.0186(6) 0.0267(6) -0.0023(6) 0.0001(7) -0.0035(5) C3SA 0.027(3) 0.029(3) 0.035(3) 0.001(3) 0.000(3) 0.001(3) C3SB 0.028(3) 0.023(3) 0.045(4) 0.001(3) -0.001(3) -0.006(3) O3S 0.042(2) 0.0189(18) 0.0265(19) 0.000(2) -0.004(2) -0.0004(14) 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 C1A N1 C2 110.4(5) C1A N1 H1N 122(4) C2 N1 H1N 127(4) C3 C2 N1 108.5(5) C3 C2 C10 133.4(5) N1 C2 C10 118.1(5) C2 C3 C3A 106.3(4) C2 C3 H3 126.8 C3A C3 H3 126.8 C1A C3A C3 108.2(4) C1A C3A C4 122.5(5) C3 C3A C4 129.2(5) O3 C4 C3A 126.1(5) O3 C4 C5 119.4(5) C3A C4 C5 114.5(4) O4 C5 C5A 122.5(5) O4 C5 C4 118.4(5) C5A C5 C4 119.1(4) N6 C5A C9A 125.1(5) N6 C5A C5 113.7(5) C9A C5A C5 121.2(5) C5A N6 C7 117.4(5) N6 C7 C8 122.5(5) N6 C7 C11 117.5(5) C8 C7 C11 120.0(5) C9 C8 C7 120.1(5) C9 C8 H8 119.9 C7 C8 H8 119.9 C8 C9 C9A 118.5(5) C8 C9 C12 114.9(5) C9A C9 C12 126.6(5) C5A C9A C9 116.3(5) C5A C9A C1A 117.2(5) C9 C9A C1A 126.5(5) N1 C1A C3A 106.5(5) N1 C1A C9A 128.8(5) C3A C1A C9A 124.5(5) O1 C10 O2 125.6(5) O1 C10 C2 121.4(5) O2 C10 C2 113.0(5) O5 C11 O6 125.1(5) O5 C11 C7 122.0(5) O6 C11 C7 112.8(5) O7 C12 O8 124.7(5) O7 C12 C9 121.5(5) O8 C12 C9 113.7(5) C10 O2 H2O 109.5 C11 O6 H6O 109.5 C12 O8 H8O 109.5 O1S S1S C1SB 105.5(4) O1S S1S C1SA 106.3(4) C1SB S1S C1SA 96.6(7) S1S C1SA H1SA 109.5 S1S C1SA H1SB 109.5 H1SA C1SA H1SB 109.5 S1S C1SA H1SC 109.5 H1SA C1SA H1SC 109.5 H1SB C1SA H1SC 109.5 S1S C1SB H1SD 109.5 S1S C1SB H1SE 109.5 H1SD C1SB H1SE 109.5 S1S C1SB H1SF 109.5 H1SD C1SB H1SF 109.5 H1SE C1SB H1SF 109.5 O2S S2S C2SB 106.9(4) O2S S2S C2SA 106.9(4) C2SB S2S C2SA 96.4(3) S2S C2SA H2SA 109.5 S2S C2SA H2SB 109.5 H2SA C2SA H2SB 109.5 S2S C2SA H2SC 109.5 H2SA C2SA H2SC 109.5 H2SB C2SA H2SC 109.5 S2S C2SB H2SD 109.5 S2S C2SB H2SE 109.5 H2SD C2SB H2SE 109.5 S2S C2SB H2SF 109.5 H2SD C2SB H2SF 109.5 H2SE C2SB H2SF 109.5 O3S S3S C3SB 103.3(3) O3S S3S C3SA 102.6(3) C3SB S3S C3SA 100.5(3) S3S C3SA H3SA 109.5 S3S C3SA H3SB 109.5 H3SA C3SA H3SB 109.5 S3S C3SA H3SC 109.5 H3SA C3SA H3SC 109.5 H3SB C3SA H3SC 109.5 S3S C3SB H3SD 109.5 S3S C3SB H3SE 109.5 H3SD C3SB H3SE 109.5 S3S C3SB H3SF 109.5 H3SD C3SB H3SF 109.5 H3SE C3SB H3SF 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance N1 C1A 1.356(7) N1 C2 1.386(7) N1 H1N 0.96(7) C2 C3 1.375(7) C2 C10 1.474(8) C3 C3A 1.425(7) C3 H3 0.9500 C3A C1A 1.409(7) C3A C4 1.449(7) C4 O3 1.217(6) C4 C5 1.563(7) C5 O4 1.207(7) C5 C5A 1.515(7) C5A N6 1.342(7) C5A C9A 1.415(7) N6 C7 1.343(7) C7 C8 1.401(7) C7 C11 1.516(7) C8 C9 1.391(8) C8 H8 0.9500 C9 C9A 1.424(7) C9 C12 1.525(7) C9A C1A 1.455(8) C10 O1 1.215(8) C10 O2 1.327(7) C11 O5 1.223(7) C11 O6 1.308(7) C12 O7 1.239(7) C12 O8 1.275(7) O2 H2O 0.8400 O6 H6O 0.8400 O8 H8O 0.8400 S1S O1S 1.533(4) S1S C1SB 1.746(10) S1S C1SA 1.766(11) C1SA H1SA 0.9800 C1SA H1SB 0.9800 C1SA H1SC 0.9800 C1SB H1SD 0.9800 C1SB H1SE 0.9800 C1SB H1SF 0.9800 S2S O2S 1.484(5) S2S C2SB 1.775(7) S2S C2SA 1.780(8) C2SA H2SA 0.9800 C2SA H2SB 0.9800 C2SA H2SC 0.9800 C2SB H2SD 0.9800 C2SB H2SE 0.9800 C2SB H2SF 0.9800 S3S O3S 1.561(4) S3S C3SB 1.762(7) S3S C3SA 1.780(7) C3SA H3SA 0.9800 C3SA H3SB 0.9800 C3SA H3SC 0.9800 C3SB H3SD 0.9800 C3SB H3SE 0.9800 C3SB H3SF 0.9800 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 C1A N1 C2 C3 -0.3(7) C1A N1 C2 C10 178.9(5) N1 C2 C3 C3A 0.1(7) C10 C2 C3 C3A -179.0(6) C2 C3 C3A C1A 0.1(7) C2 C3 C3A C4 176.5(6) C1A C3A C4 O3 -178.7(6) C3 C3A C4 O3 5.3(11) C1A C3A C4 C5 2.6(8) C3 C3A C4 C5 -173.3(6) O3 C4 C5 O4 -9.2(9) C3A C4 C5 O4 169.6(5) O3 C4 C5 C5A 171.7(6) C3A C4 C5 C5A -9.5(8) O4 C5 C5A N6 11.2(8) C4 C5 C5A N6 -169.7(5) O4 C5 C5A C9A -171.2(5) C4 C5 C5A C9A 7.8(8) C9A C5A N6 C7 -2.6(8) C5 C5A N6 C7 174.9(5) C5A N6 C7 C8 0.5(8) C5A N6 C7 C11 -178.1(5) N6 C7 C8 C9 2.7(9) C11 C7 C8 C9 -178.7(5) C7 C8 C9 C9A -3.7(8) C7 C8 C9 C12 175.4(5) N6 C5A C9A C9 1.4(8) C5 C5A C9A C9 -175.9(5) N6 C5A C9A C1A 178.4(5) C5 C5A C9A C1A 1.1(8) C8 C9 C9A C5A 1.8(8) C12 C9 C9A C5A -177.2(5) C8 C9 C9A C1A -174.8(5) C12 C9 C9A C1A 6.2(9) C2 N1 C1A C3A 0.4(6) C2 N1 C1A C9A 176.4(5) C3 C3A C1A N1 -0.3(6) C4 C3A C1A N1 -177.0(5) C3 C3A C1A C9A -176.5(5) C4 C3A C1A C9A 6.8(9) C5A C9A C1A N1 175.9(5) C9 C9A C1A N1 -7.5(9) C5A C9A C1A C3A -8.8(8) C9 C9A C1A C3A 167.9(6) C3 C2 C10 O1 175.0(7) N1 C2 C10 O1 -4.1(9) C3 C2 C10 O2 -4.3(10) N1 C2 C10 O2 176.6(5) N6 C7 C11 O5 -9.9(9) C8 C7 C11 O5 171.5(6) N6 C7 C11 O6 171.5(5) C8 C7 C11 O6 -7.2(8) C8 C9 C12 O7 -143.3(6) C9A C9 C12 O7 35.7(9) C8 C9 C12 O8 33.0(7) C9A C9 C12 O8 -148.0(6) _cod_database_fobs_code 2108052