#------------------------------------------------------------------------------ #$Date: 2019-01-16 05:23:22 +0200 (Wed, 16 Jan 2019) $ #$Revision: 213110 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/28/2242813.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_2242813 loop_ _publ_author_name 'Kumar, Rajesh' 'Ogbeide, K. Osahon' Mujeeb-Ur-Rehman 'Owolabi, Bodunde' 'Falodun, Abiodun' 'Choudhary, M. Iqbal' 'Yousuf, Sammer' _publ_section_title ; Crystal structure, Hirshfeld surface analysis and electrostatic potential study of naturally occurring cassane-type diterpenoid Pulcherrimin C monohydrate at 100K ; _journal_issue 2 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 119 _journal_page_last 123 _journal_paper_doi 10.1107/S2056989018017498 _journal_volume 75 _journal_year 2019 _chemical_absolute_configuration rm _chemical_formula_iupac 'C34 H36 O8, H2 O' _chemical_formula_moiety 'C34 H36 O8, H2 O' _chemical_formula_sum 'C34 H38 O9' _chemical_formula_weight 590.64 _chemical_name_common 'Pulcherrimin C monohydrate' _chemical_name_systematic ;5,6-Bis(benzoyloxy)-4a-hydroxy-4,7,11b-trimethyl-1,2,3,4,4a,5,6,6a,7,11,11a,11b-dodecahydrophenanthro[3,2-b]furan-4-carboxylic acid monohydrate ; _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 _audit_creation_method SHELXL-2018/3 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8027(7) _cell_length_b 13.2843(8) _cell_length_c 19.0835(10) _cell_measurement_reflns_used 9847 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 68.22 _cell_measurement_theta_min 4.05 _cell_volume 2992.1(3) _computing_cell_refinement ; SAINT (Bruker, 2000) ; _computing_data_collection ; APEX2 (Bruker, 2000) ; _computing_data_reduction ; SAINT (Bruker, 2000) ; _computing_molecular_graphics ; SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2018 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2014 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_unetI/netI 0.0503 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 18780 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.213 _diffrn_reflns_theta_min 4.055 _exptl_absorpt_coefficient_mu 0.778 _exptl_absorpt_correction_T_max 0.9260 _exptl_absorpt_correction_T_min 0.7720 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2000) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.311 _exptl_crystal_description block _exptl_crystal_F_000 1256 _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.197 _refine_diff_density_min -0.234 _refine_ls_abs_structure_details ; Flack x determined using 1939 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013) ; _refine_ls_abs_structure_Flack 0.02(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 401 _refine_ls_number_reflns 5425 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0398 _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^)+(0.0537P)^2^+0.4392P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0947 _refine_ls_wR_factor_ref 0.0983 _reflns_number_gt 4931 _reflns_number_total 5425 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file rz5245sup1.cif _cod_data_source_block I _cod_database_code 2242813 _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 0.772 _shelx_estimated_absorpt_t_max 0.926 _shelx_hkl_file ; -1 0 0 1.20 1.10 1 0 0 0.60 1.60 2 0 0 64.59 3.40 -2 0 0 59.79 4.40 3 0 0 0.70 1.40 -4 0 0 132.39 8.60 4 0 0 135.39 7.10 5 0 0 5.00 2.60 -5 0 0 2.70 3.40 6 0 0 432.16 20.60 7 0 0 -3.50 5.60 8 0 0 1164.98 52.09 8 0 0 1065.19 58.09 9 0 0 10.30 13.90 9 0 0 -20.60 21.60 9 0 0 -25.00 20.20 10 0 0 702.73 48.40 10 0 0 720.43 46.20 11 0 0 -3.40 19.00 11 0 0 11.80 19.60 12 0 0 829.72 49.40 12 0 0 923.81 50.99 13 0 0 -4.40 19.10 13 0 0 -25.40 17.10 14 0 0 232.48 27.90 -3 1 0 196.88 9.00 3 1 0 199.88 9.10 3 -1 0 196.98 9.40 -4 1 0 4871.51 203.18 4 -1 0 4643.94 203.58 4 1 0 4733.93 203.38 5 1 0 22.40 3.10 5 -1 0 21.50 3.50 6 1 0 158.58 10.50 6 -1 0 173.08 10.60 7 1 0 194.48 13.50 7 -1 0 175.08 13.90 8 1 0 103.89 18.10 8 -1 0 113.29 19.80 8 1 0 84.19 17.60 8 -1 0 139.79 15.80 8 1 0 104.29 18.40 9 -1 0 863.41 41.40 9 -1 0 713.13 47.20 9 -1 0 676.63 59.29 9 1 0 794.82 51.69 9 1 0 766.72 43.70 10 1 0 175.08 27.80 10 1 0 155.98 24.50 10 -1 0 149.88 22.70 10 -1 0 137.79 29.60 11 1 0 23.90 16.70 11 -1 0 -5.30 25.10 11 -1 0 2.60 19.90 11 1 0 -27.00 19.30 12 1 0 3.80 19.70 12 1 0 8.00 15.40 12 -1 0 -11.20 23.30 12 -1 0 44.10 19.40 13 1 0 34.30 20.40 13 -1 0 32.20 16.60 13 -1 0 58.59 24.70 13 1 0 25.90 15.70 14 -1 0 94.29 22.10 -14 1 0 62.99 20.40 14 1 0 91.99 14.30 14 -1 0 45.30 16.70 0 2 0 378.96 16.40 -2 2 0 4533.25 193.78 -3 2 0 28.20 2.80 3 -2 0 34.00 3.60 -4 2 0 170.08 8.30 4 -2 0 168.18 9.00 -5 2 0 41.40 5.10 5 -2 0 41.40 5.60 6 -2 0 1155.38 51.39 7 -2 0 104.69 12.20 8 -2 0 1621.94 69.09 8 2 0 1477.45 70.49 8 2 0 1576.64 77.19 8 -2 0 1436.36 76.49 9 2 0 642.84 46.90 9 2 0 630.24 36.20 9 -2 0 700.93 35.50 9 -2 0 474.55 53.69 9 -2 0 596.44 44.60 10 -2 0 108.89 38.60 10 -2 0 149.39 23.10 10 2 0 164.68 25.40 10 2 0 105.79 16.20 11 -2 0 916.21 69.69 11 2 0 866.71 55.19 11 2 0 963.60 48.50 11 -2 0 1020.70 55.89 12 -2 0 427.36 66.99 12 2 0 368.26 28.20 12 -2 0 390.76 35.00 -13 2 0 304.87 25.90 13 -2 0 273.87 36.00 13 -2 0 240.58 27.50 13 2 0 283.07 25.30 -14 2 0 231.78 24.60 14 -2 0 239.78 45.40 14 -2 0 186.18 23.70 0 3 0 -0.60 1.10 1 3 0 59.39 3.30 -1 3 0 55.29 3.40 -2 3 0 2950.80 126.39 -3 3 0 3147.49 136.09 3 -3 0 3205.38 136.69 4 -3 0 992.50 44.00 -4 3 0 998.40 43.30 5 -3 0 1247.68 54.39 -5 3 0 1214.48 53.59 6 -3 0 1686.93 74.29 7 -3 0 98.19 13.00 8 3 0 244.88 43.20 8 3 0 234.48 20.70 8 -3 0 198.18 37.80 8 -3 0 227.98 19.60 9 -3 0 1.90 13.10 9 3 0 3.30 12.80 9 3 0 4.70 32.30 9 -3 0 29.20 25.80 10 3 0 465.95 30.20 10 3 0 467.85 46.20 10 -3 0 434.16 43.70 10 -3 0 532.85 44.00 11 3 0 1057.29 52.99 11 -3 0 1129.59 61.59 12 3 0 9.30 11.20 -12 3 0 -7.20 22.20 12 3 0 41.40 31.80 12 -3 0 18.20 19.50 13 3 0 45.10 11.90 13 -3 0 37.60 16.80 -13 3 0 81.69 16.30 0 4 0 2106.39 90.29 -1 4 0 1.30 1.60 1 4 0 3.10 1.60 2 -4 0 9317.37 395.96 -2 4 0 9186.58 395.46 3 -4 0 3085.79 135.29 -3 4 0 3190.18 134.59 -4 4 0 866.01 37.90 5 -4 0 98.19 9.60 -5 4 0 97.69 7.70 6 -4 0 6.00 6.10 7 4 0 70.69 11.90 7 -4 0 81.49 14.10 8 -4 0 -4.10 10.10 8 -4 0 33.90 28.00 8 4 0 12.40 9.80 9 -4 0 183.08 27.50 9 -4 0 192.58 39.40 9 4 0 54.79 57.59 10 4 0 34.00 11.20 -10 4 0 52.99 19.70 10 -4 0 35.90 24.50 10 -4 0 44.40 27.60 11 4 0 36.20 11.50 11 -4 0 48.70 24.60 -11 4 0 22.80 14.70 -12 4 0 18.20 15.60 13 -4 0 445.86 36.90 13 4 0 554.74 29.50 -13 4 0 575.34 33.40 0 -5 0 2.50 2.20 0 5 0 0.60 2.00 -1 5 0 2.70 2.10 1 5 0 -1.60 2.10 1 -5 0 8.80 2.70 2 -5 0 571.14 26.90 -2 5 0 610.44 26.20 3 -5 0 25.70 4.60 4 -5 0 518.45 26.00 -4 5 0 541.35 24.20 -5 5 0 323.97 16.20 5 -5 0 320.07 19.30 6 -5 0 207.38 17.10 7 -5 0 180.68 38.40 -7 5 0 151.28 21.60 7 -5 0 150.78 17.80 7 5 0 99.79 17.90 8 5 0 41.00 10.20 8 -5 0 33.30 40.40 8 -5 0 43.00 13.80 -8 5 0 34.50 18.90 9 5 0 249.58 19.70 -9 5 0 204.68 27.00 9 -5 0 248.78 39.90 9 -5 0 240.68 34.00 -10 5 0 29.60 15.70 10 5 0 33.10 11.10 10 -5 0 17.80 31.70 11 -5 0 814.32 55.29 11 5 0 699.63 37.80 -11 5 0 756.62 40.70 -12 5 0 -0.70 16.30 12 5 0 8.40 10.30 12 -5 0 -23.30 22.30 -13 5 0 9.10 14.20 13 -5 0 -10.50 17.70 13 5 0 -11.00 8.70 0 -6 0 1237.38 53.39 0 6 0 1210.38 53.09 1 -6 0 499.75 23.30 -1 6 0 500.85 22.50 2 -6 0 1385.46 64.29 -2 6 0 1536.85 63.49 -3 6 0 -1.70 3.40 3 -6 0 3.00 5.80 -4 6 0 1539.55 64.79 4 -6 0 1425.46 66.69 -5 6 0 1.50 5.40 -6 6 0 140.39 19.40 6 6 0 146.49 22.70 6 6 0 115.39 18.30 6 -6 0 148.09 18.70 7 6 0 194.58 18.30 7 -6 0 161.88 22.60 -7 6 0 240.18 28.20 7 -6 0 143.69 59.79 8 -6 0 99.29 50.09 8 6 0 126.59 18.40 8 -6 0 152.08 27.20 9 -6 0 -13.60 23.10 9 -6 0 59.19 42.00 9 6 0 15.80 10.20 -9 6 0 20.80 16.40 10 6 0 66.59 11.20 10 -6 0 94.29 36.80 -10 6 0 87.59 17.00 11 6 0 165.28 18.20 -11 6 0 185.78 22.80 11 -6 0 177.28 33.60 -12 6 0 89.19 16.60 12 6 0 127.59 17.00 -13 6 0 35.90 16.80 13 -6 0 -2.50 19.20 1 -7 0 306.97 17.60 -1 7 0 335.47 15.70 2 -7 0 3.00 7.10 -2 7 0 8.10 4.00 3 -7 0 265.87 20.20 -3 7 0 300.17 15.00 -4 7 0 60.59 8.50 4 -7 0 52.39 11.10 -5 7 0 20.80 17.20 -5 7 0 24.30 12.50 5 7 0 66.19 20.70 5 -7 0 17.70 11.70 -6 7 0 284.07 21.80 6 7 0 211.18 20.20 -6 7 0 255.17 28.20 6 -7 0 224.28 25.80 6 7 0 243.48 35.60 7 -7 0 38.20 17.00 7 7 0 16.20 10.90 -7 7 0 2.00 16.70 7 -7 0 100.59 66.09 -8 7 0 14.00 16.10 8 -7 0 1.90 22.90 8 -7 0 36.90 55.29 8 7 0 4.00 10.10 9 7 0 28.70 10.70 -9 7 0 9.30 15.20 9 -7 0 17.00 46.40 -10 7 0 11.20 15.30 10 -7 0 -9.50 38.10 10 7 0 5.70 9.90 11 -7 0 84.29 33.70 -11 7 0 136.69 24.00 11 7 0 124.49 18.20 12 7 0 70.99 10.70 -12 7 0 74.19 16.80 -12 7 0 72.59 16.00 12 -7 0 49.30 25.50 1 -8 0 253.07 20.30 2 -8 0 217.78 20.60 3 -8 0 302.67 25.40 4 -8 0 8.30 13.90 -4 8 0 32.30 12.90 -4 8 0 22.80 17.60 4 8 0 54.19 18.80 -4 8 0 53.09 20.30 5 8 0 400.56 30.50 -5 8 0 482.15 29.30 -5 8 0 563.44 40.50 -5 8 0 542.65 33.80 5 8 0 507.65 39.50 5 -8 0 398.66 34.40 6 8 0 160.28 20.90 -6 8 0 168.18 26.50 -6 8 0 213.28 36.10 -6 8 0 234.88 20.90 6 -8 0 223.38 32.70 6 8 0 203.68 34.50 7 8 0 1.50 11.10 7 -8 0 18.60 24.50 -7 8 0 9.20 16.10 8 -8 0 53.79 59.99 8 -8 0 37.90 30.90 9 8 0 372.96 24.60 9 -8 0 293.17 52.99 -9 8 0 373.66 28.10 -9 8 0 403.16 33.40 10 8 0 69.69 11.10 11 8 0 261.17 20.90 -11 8 0 242.28 26.70 -11 8 0 259.77 29.30 12 -8 0 49.99 24.60 -12 8 0 60.09 17.30 0 9 0 6.80 17.70 1 -9 0 152.88 16.00 1 9 0 88.89 18.80 1 9 0 121.69 20.00 -1 9 0 153.98 28.80 -1 9 0 116.29 21.30 -2 9 0 625.44 40.90 -2 9 0 587.74 40.30 2 9 0 548.65 39.10 2 -9 0 541.55 37.90 2 9 0 549.25 43.00 -3 9 0 63.79 18.10 -3 9 0 18.50 14.10 3 -9 0 -3.70 17.20 3 9 0 46.00 18.50 -3 9 0 23.60 20.30 3 9 0 57.29 20.50 4 9 0 42.40 17.90 -4 9 0 38.60 12.90 -4 9 0 -9.60 18.50 4 -9 0 4.20 20.20 -4 9 0 24.70 16.70 -5 9 0 384.66 37.00 -5 9 0 398.16 26.90 -5 9 0 411.06 32.40 5 9 0 357.26 37.60 -6 9 0 -7.10 19.60 6 9 0 0.90 18.00 6 -9 0 -14.60 30.00 -6 9 0 7.00 16.70 -7 9 0 25.70 16.40 -7 9 0 39.60 18.90 7 -9 0 10.70 37.00 -8 9 0 151.08 28.10 -8 9 0 157.98 24.80 8 9 0 156.78 21.80 -9 9 0 190.08 24.50 -9 9 0 146.09 27.40 -10 9 0 226.38 26.70 -10 9 0 241.18 29.80 -11 9 0 203.78 24.40 -11 9 0 170.68 27.30 0 10 0 403.86 34.20 0 10 0 392.86 32.80 -1 10 0 157.48 28.60 1 10 0 135.79 19.60 -1 10 0 87.09 19.20 2 10 0 186.98 32.40 -2 10 0 207.88 29.00 2 10 0 247.38 31.80 -2 10 0 212.58 32.80 -3 10 0 -24.00 19.10 3 -10 0 23.40 25.80 -3 10 0 -1.50 20.10 -3 10 0 14.90 14.20 3 10 0 -2.80 19.20 4 -10 0 307.77 53.79 -4 10 0 482.95 29.80 -5 10 0 79.69 14.00 -5 10 0 118.99 21.20 5 10 0 87.19 18.70 5 -10 0 86.09 38.70 6 -10 0 19.40 43.70 -6 10 0 117.19 19.60 6 10 0 130.69 18.50 -7 10 0 -6.80 17.40 -7 10 0 10.00 15.80 -8 10 0 136.69 24.40 -8 10 0 124.99 18.80 -9 10 0 8.60 18.60 -9 10 0 10.50 16.80 10 -10 0 38.70 54.69 -10 10 0 22.80 18.00 -10 10 0 14.40 16.20 -11 10 0 353.06 29.50 0 11 0 -5.50 23.60 1 11 0 179.78 34.10 -1 11 0 188.58 28.80 1 11 0 195.88 31.00 2 11 0 1248.78 62.99 2 11 0 1270.17 63.09 -2 11 0 1226.28 62.89 -2 11 0 1256.67 62.39 3 11 0 180.98 28.20 -3 11 0 134.69 21.80 -3 11 0 153.38 25.40 -3 11 0 132.89 18.60 -4 11 0 312.37 29.50 -4 11 0 306.97 32.00 -4 11 0 277.77 25.50 4 11 0 278.27 31.00 -5 11 0 210.28 28.60 -5 11 0 236.28 31.20 5 11 0 254.27 27.90 6 11 0 191.58 27.30 -6 11 0 155.28 26.60 -6 11 0 156.18 28.50 -7 11 0 14.10 16.20 -7 11 0 -6.00 17.40 -8 11 0 69.29 19.50 -8 11 0 81.49 18.60 -9 11 0 370.36 33.40 -9 11 0 422.96 31.00 -10 11 0 -8.90 12.40 0 12 0 177.58 26.90 0 12 0 219.38 28.40 1 12 0 1.00 17.20 -1 12 0 6.20 15.70 1 12 0 5.20 16.20 -1 12 0 13.00 17.10 2 12 0 1471.85 70.79 -2 12 0 1443.06 69.99 2 12 0 1442.96 69.59 -2 12 0 1484.25 69.59 -3 12 0 279.17 29.60 -3 12 0 297.07 28.30 3 12 0 319.57 29.50 4 12 0 111.99 16.90 -4 12 0 161.58 26.40 -4 12 0 94.69 17.40 5 12 0 68.89 16.40 -5 12 0 55.09 17.90 -5 12 0 83.49 16.00 -6 12 0 363.96 26.90 -6 12 0 309.57 35.80 6 12 0 390.56 30.50 -7 12 0 3.30 14.80 -7 12 0 -9.30 19.10 -8 12 0 183.88 24.10 -8 12 0 217.28 29.70 -9 12 0 95.89 14.50 0 13 0 10.20 15.00 0 13 0 6.90 16.40 1 13 0 369.46 31.10 -1 13 0 367.66 31.20 -1 13 0 391.06 29.80 1 13 0 394.56 28.50 -2 13 0 35.40 14.70 2 13 0 -0.70 15.30 -2 13 0 0.80 16.70 -3 13 0 268.07 27.50 -3 13 0 194.58 25.00 3 13 0 214.68 26.90 -4 13 0 705.13 42.60 -4 13 0 797.32 42.00 4 13 0 826.12 42.40 -5 13 0 226.18 29.80 -5 13 0 170.38 25.20 5 13 0 179.98 32.20 -6 13 0 36.00 15.80 -6 13 0 34.50 18.40 -7 13 0 166.48 28.60 -7 13 0 158.68 22.70 -8 13 0 62.79 13.30 0 14 0 853.21 43.70 -1 14 0 462.15 42.10 -1 14 0 396.36 38.60 -2 14 0 156.08 20.80 2 14 0 134.59 19.20 -2 14 0 121.99 20.30 -3 14 0 72.79 19.60 3 14 0 53.89 16.20 -3 14 0 71.19 15.50 4 14 0 237.88 26.30 -4 14 0 216.48 23.70 -4 14 0 232.58 30.40 -5 14 0 66.59 18.10 -5 14 0 40.40 14.10 -6 14 0 40.60 13.20 -6 14 0 71.49 26.90 0 15 0 -9.00 16.10 1 15 0 262.07 28.00 -1 15 0 219.08 29.70 -2 15 0 11.00 12.30 2 15 0 23.80 15.40 -2 15 0 22.80 18.20 3 15 0 186.38 24.50 -3 15 0 229.38 29.80 -3 15 0 211.98 21.50 -4 15 0 76.79 13.80 0 16 0 334.37 29.90 0 0 -1 0.20 0.70 -1 0 1 6527.65 307.47 1 0 -1 7550.94 307.27 -1 0 -1 7108.69 307.07 -1 0 1 7567.54 307.07 2 0 1 340.37 14.50 -2 0 1 313.57 15.40 -3 0 1 29.80 4.60 3 0 1 35.70 3.10 4 0 1 470.65 20.90 4 0 -1 477.25 20.80 -4 0 1 445.16 21.80 5 0 1 452.25 21.10 -5 0 1 463.35 22.00 5 0 -1 460.65 21.00 6 0 -1 844.92 37.90 -6 0 1 868.11 38.60 6 0 1 836.22 38.10 7 0 1 14.30 6.20 7 0 -1 25.20 6.20 8 0 1 9.10 18.60 8 0 1 -20.30 24.80 8 0 -1 40.20 17.70 8 0 -1 17.60 9.20 8 0 1 13.00 9.30 9 0 1 128.49 16.90 9 0 -1 132.19 20.00 9 0 1 110.29 22.10 9 0 -1 127.99 16.60 9 0 1 154.58 31.00 9 0 -1 104.79 22.30 10 0 1 736.73 48.10 10 0 1 676.43 47.40 10 0 -1 637.04 46.50 10 0 -1 690.53 46.80 11 0 -1 566.04 40.80 11 0 -1 549.15 39.70 11 0 1 593.14 41.30 11 0 1 553.64 42.00 12 0 -1 29.90 18.10 12 0 1 44.40 20.00 12 0 1 -1.80 18.50 12 0 -1 34.30 19.20 13 0 1 288.57 30.40 13 0 1 326.07 33.70 13 0 -1 262.47 28.10 13 0 -1 329.57 34.40 14 0 1 17.40 23.40 14 0 1 52.99 16.30 -14 0 1 23.40 13.40 14 0 -1 40.90 23.10 0 1 1 1656.73 69.39 0 -1 1 1688.13 69.39 0 -1 -1 1495.55 69.49 0 1 -1 1641.64 69.39 -1 -1 -1 1952.80 84.29 1 -1 1 1968.60 84.29 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9 3 9 539.55 33.90 9 -3 -9 550.54 36.60 10 3 -9 43.10 14.10 10 -3 9 31.60 25.30 10 -3 9 36.80 35.10 10 3 -9 38.40 10.30 10 3 9 67.39 14.10 10 -3 -9 44.40 15.50 11 3 -9 49.80 15.20 11 -3 9 26.00 35.50 -11 3 9 76.39 13.90 11 -3 9 60.39 26.30 11 3 -9 58.39 11.60 11 3 9 61.59 18.40 11 -3 -9 89.49 15.90 12 -3 9 93.49 23.60 -12 3 9 88.09 12.80 12 -3 9 66.19 28.80 12 3 -9 110.09 16.60 12 -3 -9 74.09 14.20 12 3 9 68.59 11.90 0 4 9 1647.24 73.19 0 -4 9 1602.04 76.89 0 -4 9 1702.23 73.89 1 -4 9 640.84 37.70 -1 4 9 682.73 32.10 1 -4 9 663.83 33.20 -1 -4 9 679.33 41.60 1 4 9 683.03 33.10 -1 -4 9 683.73 33.30 2 -4 9 288.97 19.10 2 -4 9 275.67 28.70 -2 4 9 302.37 16.90 2 4 9 303.27 19.90 -2 -4 9 289.97 33.30 3 -4 9 554.14 29.60 -3 4 9 577.44 27.30 -3 -4 9 545.55 46.80 3 4 9 580.94 29.90 -4 4 9 188.88 12.60 4 -4 9 167.38 17.30 -4 -4 9 224.08 41.20 -4 -4 9 196.88 21.40 4 4 9 182.28 19.90 5 4 -9 577.74 32.50 -5 4 9 594.84 28.40 -5 4 9 535.75 47.00 -5 4 9 575.54 30.20 5 -4 9 587.64 32.90 5 -4 9 664.73 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22.20 7.90 -1 -4 20 43.90 11.50 -1 4 -20 0.00 23.40 -1 4 -20 51.29 10.70 1 4 20 33.90 9.00 -1 -4 20 81.19 19.10 2 4 -20 133.89 19.30 -2 -4 -20 146.59 27.10 2 -4 20 154.58 31.10 2 -4 20 137.19 23.10 2 -4 -20 104.79 26.60 2 4 20 152.88 14.60 2 4 20 139.89 13.90 -2 4 -20 171.78 18.40 -3 -4 -20 81.69 22.70 3 4 -20 92.69 12.60 3 -4 20 109.49 22.40 3 4 -20 84.39 17.30 3 4 20 94.69 12.50 3 -4 -20 73.39 23.90 -3 4 -20 70.89 11.10 3 4 20 100.99 13.40 4 -4 20 317.67 28.30 -4 -4 -20 268.97 31.50 4 4 -20 261.77 25.80 4 4 -20 316.67 21.30 4 -4 20 306.47 33.90 4 -4 -20 254.17 33.30 -4 4 -20 319.37 20.90 4 4 20 318.27 18.70 4 4 20 309.77 17.40 5 -4 20 18.00 21.60 -5 -4 -20 28.70 16.40 5 -4 20 10.80 14.80 5 4 -20 24.70 9.00 5 4 20 20.70 6.60 -5 4 -20 22.90 8.50 5 -4 -20 47.40 15.00 6 -4 20 51.49 15.70 -6 -4 -20 59.09 15.20 -6 4 -20 36.60 8.10 6 -4 -20 37.60 11.60 6 4 20 53.39 7.20 0 -5 -20 10.80 33.00 0 5 20 7.20 8.20 0 5 -20 -1.20 8.60 0 -5 20 -4.50 17.10 0 -5 20 -0.50 13.10 1 -5 20 51.89 18.60 -1 -5 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27.70 -2 6 -20 183.38 15.30 2 6 20 197.68 12.70 3 6 -20 18.30 7.20 3 -6 20 23.70 22.30 -3 -6 -20 32.50 23.20 3 -6 20 43.10 17.10 3 6 20 18.70 5.60 3 -6 -20 23.30 18.70 -3 6 -20 20.60 7.20 4 6 -20 19.30 6.70 4 -6 20 21.60 17.80 -4 6 -20 20.40 6.60 4 -6 -20 14.40 15.70 4 6 20 21.10 5.00 0 -7 -20 15.80 26.60 0 7 20 15.00 6.30 0 -7 20 35.70 14.30 0 7 -20 29.70 6.70 -1 7 20 115.89 12.10 1 7 -20 117.89 12.30 -1 -7 -20 53.19 29.10 1 -7 20 174.18 23.10 -1 7 -20 140.79 12.20 1 7 20 121.09 10.40 2 -7 20 2.40 15.50 2 7 -20 12.50 6.30 -2 -7 -20 -8.80 30.80 -2 7 20 -6.90 7.80 3 -7 20 79.59 17.60 3 7 -20 67.49 9.90 3 7 20 79.19 8.30 -3 7 -20 87.29 10.50 0 0 -21 14.60 22.80 0 0 21 -0.90 7.60 -1 0 -21 195.28 24.60 1 0 21 232.28 16.50 1 0 -21 160.88 32.50 -2 0 -21 120.89 19.50 2 0 21 108.89 14.90 3 0 -21 63.09 17.80 3 0 21 105.99 14.00 -3 0 -21 68.99 16.60 -4 0 -21 10.10 14.30 4 0 21 16.70 8.10 4 0 -21 13.80 13.90 5 0 21 44.40 8.30 -5 0 -21 50.99 14.10 5 0 -21 34.20 11.80 0 -1 21 270.67 17.80 0 1 -21 228.88 34.20 0 1 -21 276.77 34.70 0 -1 -21 217.78 39.20 0 1 21 283.87 17.20 1 -1 21 341.57 20.40 -1 -1 -21 318.67 35.60 1 1 -21 314.77 36.50 -1 1 -21 303.37 33.90 -1 -1 21 322.47 19.30 -1 1 -21 223.68 37.00 1 1 21 369.56 20.00 2 1 -21 -4.50 17.50 2 -1 21 37.40 9.30 -2 -1 -21 32.90 17.60 2 1 -21 37.00 21.10 2 -1 -21 22.90 20.10 -2 1 -21 48.10 19.30 2 1 21 36.10 8.70 -2 1 -21 47.00 19.80 -3 -1 -21 126.59 24.90 3 -1 21 125.79 15.40 3 1 -21 112.59 21.30 3 1 21 166.18 14.60 -3 1 -21 161.18 28.50 3 -1 -21 93.79 19.90 -3 1 -21 143.39 19.80 4 1 -21 48.00 26.70 -4 -1 -21 60.49 14.40 4 1 -21 45.60 14.20 4 -1 21 36.30 9.10 -4 1 -21 58.69 16.60 4 1 21 42.60 8.40 4 -1 -21 32.00 15.40 -4 1 -21 31.90 24.50 5 -1 21 275.17 17.90 5 1 -21 233.58 20.30 -5 -1 -21 252.57 22.60 -5 1 -21 291.87 26.10 5 -1 -21 222.38 22.00 5 1 21 247.28 16.30 -5 1 -21 236.88 31.40 0 -2 -21 32.40 25.40 0 -2 21 -6.10 8.10 0 2 -21 -12.40 15.40 0 2 -21 8.30 19.90 1 2 -21 60.69 19.60 1 2 -21 89.09 16.80 -1 -2 -21 106.39 23.20 1 -2 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134.59 16.90 -2 3 -21 101.69 22.50 2 -3 -21 79.19 22.40 2 3 21 105.49 12.70 -2 3 -21 141.49 19.20 3 3 -21 -17.30 13.80 3 3 -21 23.30 11.90 3 -3 21 11.20 10.80 -3 -3 -21 17.70 18.30 3 -3 -21 10.10 18.60 -3 3 -21 11.10 10.30 3 3 21 10.10 7.30 -3 3 -21 -11.00 22.20 -4 -3 -21 38.80 16.10 4 3 -21 28.80 12.60 4 3 -21 44.30 11.50 4 3 21 44.00 7.40 4 3 21 82.09 12.70 -4 3 -21 10.80 29.90 -4 3 -21 57.99 11.10 4 -3 -21 63.09 16.30 5 -3 21 324.97 22.00 5 3 -21 255.67 20.40 -5 -3 -21 306.27 25.40 5 3 -21 237.98 22.40 5 3 21 275.57 18.40 5 3 21 282.47 17.90 5 -3 -21 287.17 23.40 -5 3 -21 270.17 22.00 0 -4 21 164.08 17.60 0 -4 -21 113.59 29.00 0 4 -21 207.28 17.80 1 -4 21 23.10 10.30 1 4 -21 42.50 10.80 1 -4 21 62.99 19.20 -1 -4 -21 14.20 27.10 1 4 -21 16.10 18.40 1 -4 -21 21.60 22.90 -1 4 -21 35.30 9.70 -1 4 -21 35.50 21.80 2 -4 21 43.00 11.80 -2 -4 -21 90.19 23.60 2 4 -21 51.39 10.80 2 -4 21 62.19 20.50 2 4 -21 17.90 16.80 2 -4 -21 -4.40 20.60 -2 4 -21 31.60 10.00 3 4 -21 114.49 15.80 3 -4 21 145.59 18.70 -3 -4 -21 121.39 22.20 3 -4 21 147.99 21.90 3 4 21 95.19 14.50 3 -4 -21 100.89 19.70 -3 4 -21 134.79 15.20 4 -4 21 186.28 22.60 4 4 -21 133.69 15.50 -4 -4 -21 158.58 28.10 4 4 21 142.69 12.70 4 -4 -21 127.49 24.20 -4 4 -21 176.98 15.00 0 -5 21 263.67 25.40 0 5 -21 233.18 17.60 1 5 -21 11.20 8.10 -1 -5 -21 13.40 26.00 1 -5 21 22.90 12.90 1 -5 21 1.10 16.00 1 -5 -21 2.90 21.40 1 5 21 -7.90 9.20 -1 5 -21 3.30 7.80 2 -5 21 94.89 14.40 -2 -5 -21 54.99 24.40 2 -5 21 136.29 19.00 2 5 -21 95.19 13.50 -2 5 -21 92.19 13.00 2 -5 -21 79.99 20.40 3 -5 21 32.00 15.20 3 5 -21 54.19 8.40 -3 -5 -21 73.09 21.10 3 -5 21 40.50 23.90 3 5 21 40.30 6.90 3 -5 -21 32.80 17.00 -3 5 -21 44.10 8.00 0 -6 -21 91.59 24.00 0 6 21 91.69 14.00 0 6 -21 136.09 12.60 -1 -6 -21 5.00 22.90 1 -6 21 57.19 15.00 1 6 -21 37.40 7.20 1 6 21 23.90 7.70 1 -6 -21 49.70 20.90 -1 6 -21 51.49 7.50 2 -6 21 33.30 16.90 2 6 -21 17.40 6.50 -2 -6 -21 7.30 25.10 2 6 21 29.60 6.70 2 -6 -21 27.40 18.00 -2 6 -21 39.10 6.80 0 0 -22 189.28 27.60 -1 0 -22 88.99 20.20 1 0 22 114.79 11.30 1 0 -22 97.79 18.00 2 0 22 12.50 7.00 2 0 -22 1.20 15.20 -2 0 -22 -6.50 18.90 -3 0 -22 158.78 25.10 3 0 22 150.98 12.80 4 0 -22 28.10 10.50 4 0 22 23.50 7.00 -4 0 -22 10.80 14.90 0 1 -22 -28.40 15.70 0 -1 -22 7.60 18.90 0 -1 22 -11.10 6.80 0 1 -22 -32.90 25.30 -1 -1 -22 121.49 21.80 1 -1 22 137.99 12.20 1 1 -22 135.39 25.60 1 1 -22 137.69 23.60 -1 1 -22 155.08 23.50 -1 1 -22 118.49 19.70 1 1 22 135.09 11.50 2 -1 22 157.38 13.30 2 1 22 129.19 12.40 -2 1 -22 144.59 25.00 2 -1 -22 125.69 25.30 3 -1 22 107.79 12.30 -3 -1 -22 86.79 17.60 3 1 22 115.79 11.20 3 -1 -22 90.19 15.10 -3 1 -22 66.89 29.70 4 1 -22 25.10 10.70 -4 -1 -22 17.10 14.80 4 -1 22 25.00 7.60 4 -1 -22 3.70 11.00 4 1 22 23.00 6.30 -4 1 -22 6.40 17.70 0 -2 -22 223.58 31.50 0 2 -22 343.07 25.30 1 -2 22 69.79 8.30 1 2 -22 49.40 16.20 1 2 -22 65.49 15.70 -1 -2 -22 56.79 21.30 -1 2 -22 64.49 17.30 1 -2 -22 29.90 18.20 -1 2 -22 79.99 14.70 2 2 -22 10.30 13.30 2 2 -22 -4.00 17.10 -2 -2 -22 47.90 19.10 2 -2 22 23.10 8.20 2 2 22 12.00 6.10 2 -2 -22 49.30 17.10 -2 2 -22 0.10 17.50 3 2 -22 46.50 14.50 -3 -2 -22 75.19 17.60 3 -2 22 76.49 12.40 3 2 -22 41.70 12.40 3 2 22 64.69 9.80 -3 2 -22 63.19 12.80 -3 2 -22 37.50 17.70 0 3 -22 -8.10 16.80 0 -3 -22 -12.20 19.70 0 3 -22 -12.20 10.60 -1 -3 -22 -4.80 20.80 1 3 -22 33.80 14.90 1 -3 22 33.50 7.90 1 3 -22 45.70 11.30 -1 3 -22 42.60 11.00 1 -3 -22 -5.70 18.60 -1 3 -22 16.40 17.80 -2 -3 -22 35.80 20.90 2 -3 22 5.70 7.80 2 3 -22 -3.80 14.50 -2 3 -22 13.90 25.40 2 -3 -22 1.70 17.00 -2 3 -22 17.90 11.40 3 -3 22 192.88 15.70 -3 -3 -22 181.78 26.90 3 3 -22 168.98 18.40 3 -3 -22 151.58 23.40 -3 3 -22 192.48 17.20 0 4 -22 -5.50 8.50 0 -4 -22 26.20 18.40 1 4 -22 31.50 9.10 -1 -4 -22 -7.80 19.50 1 -4 -22 21.20 17.90 -1 4 -22 45.10 8.90 2 -4 22 -5.10 11.90 -2 -4 -22 55.69 21.80 2 -4 -22 -3.40 16.30 ; _shelx_hkl_checksum 71450 _shelx_res_file ; TITL cp124135r_0m_a.res in P2(1)2(1)2(1) C:\CP1241~1\cp124135r_0m_a.res created by SHELXL-2018/3 at 08:42:41 on 02-Dec-2018 CELL 1.54178 11.8027 13.2843 19.0835 90.000 90.000 90.000 ZERR 4.000 0.0007 0.0008 0.0010 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H O UNIT 136 152 36 TEMP -173.140 SIZE 0.10 0.24 0.35 L.S. 20 ACTA CONF BOND $H EQIV $1 -x+1, y-1/2, -z+3/2 HTAB O1 O4_$1 HTAB O1W O1 HTAB O1W O8 EQIV $2 -x+1, y+1/2, -z+3/2 HTAB O3 O1W_$2 HTAB LIST 4 FMAP 2 DFIX 0.85 .001 O1W HWA O1W HWB DFIX 1.39 .001 HWA HWB PLAN 20 MPLA 5 O2 C12 C13 C15 C16 WGHT 0.053700 0.439200 FVAR 0.82216 O1 3 0.504383 0.476389 0.714028 11.00000 0.01870 0.01543 = 0.01667 0.00199 0.00265 0.00380 AFIX 148 H1 2 0.498287 0.423367 0.735593 11.00000 -1.50000 AFIX 0 O2 3 0.016383 0.251830 0.676356 11.00000 0.02277 0.02194 = 0.01772 0.00012 -0.00069 -0.00702 O1W 3 0.637484 0.417583 0.597169 11.00000 0.03057 0.02437 = 0.02435 0.00460 0.00888 0.00372 HWA 2 0.613618 0.442075 0.635582 11.00000 -1.50000 HWB 2 0.610207 0.450795 0.563036 11.00000 -1.50000 O3 3 0.394938 0.720181 0.881740 11.00000 0.03420 0.01966 = 0.01936 -0.00262 0.00368 0.00302 AFIX 148 H3 2 0.380820 0.779727 0.889607 11.00000 -1.50000 AFIX 0 O4 3 0.443453 0.782387 0.777971 11.00000 0.03070 0.01691 = 0.01896 0.00053 -0.00415 -0.00404 O5 3 0.316510 0.685722 0.681356 11.00000 0.01518 0.01423 = 0.01661 0.00067 0.00083 0.00184 O6 3 0.418563 0.787887 0.610264 11.00000 0.02033 0.02037 = 0.01805 0.00230 0.00151 -0.00148 O7 3 0.327858 0.595423 0.553595 11.00000 0.01702 0.01902 = 0.01312 0.00300 0.00249 -0.00026 O8 3 0.507114 0.577552 0.514480 11.00000 0.02160 0.03049 = 0.02073 0.00613 0.00401 0.00511 C1 1 0.344503 0.423908 0.829332 11.00000 0.01962 0.01665 = 0.01429 0.00265 0.00226 0.00032 AFIX 23 H1A 2 0.275590 0.389055 0.846246 11.00000 -1.20000 H1B 2 0.399822 0.371907 0.814829 11.00000 -1.20000 AFIX 0 C2 1 0.394692 0.485525 0.888950 11.00000 0.02450 0.02224 = 0.01332 0.00177 -0.00102 0.00307 AFIX 23 H2A 2 0.413298 0.440659 0.928742 11.00000 -1.20000 H2B 2 0.338465 0.535594 0.905294 11.00000 -1.20000 AFIX 0 C3 1 0.501338 0.539342 0.864345 11.00000 0.02231 0.01723 = 0.01775 0.00148 -0.00593 0.00235 AFIX 23 H3A 2 0.559558 0.487970 0.853582 11.00000 -1.20000 H3B 2 0.530399 0.580736 0.903561 11.00000 -1.20000 AFIX 0 C4 1 0.487377 0.608212 0.799285 11.00000 0.01786 0.01920 = 0.01476 -0.00122 -0.00187 -0.00206 C5 1 0.422397 0.547282 0.739698 11.00000 0.01632 0.01351 = 0.01316 -0.00066 -0.00119 0.00192 C6 1 0.398901 0.607093 0.671375 11.00000 0.01406 0.01410 = 0.01580 0.00251 0.00252 0.00014 AFIX 13 H6 2 0.471384 0.637824 0.654684 11.00000 -1.20000 AFIX 0 C7 1 0.354558 0.535016 0.615017 11.00000 0.01772 0.01521 = 0.01198 0.00197 0.00054 0.00360 AFIX 13 H7 2 0.415279 0.485543 0.602790 11.00000 -1.20000 AFIX 0 C8 1 0.247830 0.478529 0.635315 11.00000 0.01679 0.01525 = 0.01443 -0.00024 0.00167 0.00162 AFIX 13 H8 2 0.186764 0.528923 0.644741 11.00000 -1.20000 AFIX 0 C9 1 0.271325 0.419239 0.704507 11.00000 0.01711 0.01534 = 0.01403 0.00060 0.00202 0.00164 AFIX 13 H9 2 0.334191 0.370940 0.694319 11.00000 -1.20000 AFIX 0 C10 1 0.313478 0.489695 0.765006 11.00000 0.01511 0.01658 = 0.01274 -0.00075 -0.00012 0.00128 C11 1 0.168336 0.355865 0.728217 11.00000 0.01999 0.01805 = 0.01565 0.00130 0.00318 -0.00205 AFIX 23 H11A 2 0.194840 0.298367 0.756862 11.00000 -1.20000 H11B 2 0.117878 0.397728 0.757681 11.00000 -1.20000 AFIX 0 C12 1 0.104520 0.317884 0.667178 11.00000 0.01875 0.01502 = 0.01968 -0.00226 0.00375 0.00011 C13 1 0.117348 0.341236 0.598969 11.00000 0.02094 0.01810 = 0.01740 -0.00246 -0.00184 -0.00083 C14 1 0.208806 0.410142 0.573491 11.00000 0.02051 0.02000 = 0.01398 0.00040 0.00017 -0.00321 AFIX 13 H14 2 0.175084 0.454722 0.536778 11.00000 -1.20000 AFIX 0 C15 1 0.031111 0.285952 0.561917 11.00000 0.02598 0.02531 = 0.01833 -0.00226 -0.00137 -0.00609 AFIX 43 H15 2 0.017844 0.286084 0.512817 11.00000 -1.20000 AFIX 0 C16 1 -0.026553 0.234404 0.610418 11.00000 0.02345 0.02717 = 0.02096 -0.00473 -0.00380 -0.00875 AFIX 43 H16 2 -0.088919 0.191433 0.600640 11.00000 -1.20000 AFIX 0 C17 1 0.437741 0.710918 0.817187 11.00000 0.01557 0.02046 = 0.01685 -0.00221 -0.00523 -0.00349 C18 1 0.608284 0.635153 0.773945 11.00000 0.01722 0.02435 = 0.02141 -0.00020 -0.00400 -0.00264 AFIX 137 H18A 2 0.649574 0.573260 0.762598 11.00000 -1.50000 H18B 2 0.648405 0.671535 0.811094 11.00000 -1.50000 H18C 2 0.603385 0.677712 0.732109 11.00000 -1.50000 AFIX 0 C19 1 0.218851 0.562931 0.788202 11.00000 0.01631 0.01841 = 0.01474 0.00013 0.00223 0.00093 AFIX 137 H19A 2 0.178146 0.587521 0.746845 11.00000 -1.50000 H19B 2 0.252518 0.619990 0.813222 11.00000 -1.50000 H19C 2 0.165902 0.527710 0.819244 11.00000 -1.50000 REM ##### REM ##### REM ##### REM ##### AFIX 0 C20 1 0.304133 0.348576 0.538679 11.00000 0.03118 0.02773 = 0.01845 -0.00712 0.00619 -0.00706 AFIX 137 H20A 2 0.271281 0.302184 0.504307 11.00000 -1.50000 H20B 2 0.344815 0.310097 0.574548 11.00000 -1.50000 H20C 2 0.356908 0.394307 0.515049 11.00000 -1.50000 AFIX 0 C21 1 0.338207 0.774083 0.648157 11.00000 0.02022 0.01590 = 0.01513 -0.00020 -0.00553 -0.00164 C22 1 0.251203 0.851408 0.664029 11.00000 0.01611 0.01420 = 0.02148 -0.00177 -0.00511 -0.00216 C23 1 0.193207 0.853289 0.727454 11.00000 0.01995 0.01827 = 0.02724 -0.00011 -0.00248 -0.00274 AFIX 43 H23 2 0.203683 0.800542 0.760439 11.00000 -1.20000 AFIX 0 C24 1 0.120079 0.932090 0.742616 11.00000 0.01900 0.02233 = 0.03545 -0.00825 0.00132 -0.00376 AFIX 43 H24 2 0.081958 0.934114 0.786437 11.00000 -1.20000 AFIX 0 C25 1 0.102488 1.008320 0.693588 11.00000 0.01691 0.01806 = 0.04761 -0.00728 -0.00727 0.00214 AFIX 43 H25 2 0.052511 1.062358 0.703969 11.00000 -1.20000 AFIX 0 C26 1 0.158241 1.005038 0.629516 11.00000 0.02286 0.01724 = 0.03593 0.00260 -0.01259 0.00142 AFIX 43 H26 2 0.144897 1.056131 0.595677 11.00000 -1.20000 AFIX 0 C27 1 0.233132 0.927722 0.614719 11.00000 0.01992 0.01982 = 0.02492 -0.00016 -0.00724 -0.00160 AFIX 43 H27 2 0.272173 0.926462 0.571194 11.00000 -1.20000 AFIX 0 C28 1 0.415359 0.617172 0.510630 11.00000 0.01992 0.01813 = 0.01439 -0.00205 0.00023 -0.00086 C29 1 0.383913 0.696903 0.459158 11.00000 0.02567 0.01796 = 0.01293 -0.00129 0.00009 -0.00355 C30 1 0.278844 0.744227 0.460948 11.00000 0.02181 0.02044 = 0.01607 -0.00156 0.00202 -0.00297 AFIX 43 H30 2 0.223119 0.723328 0.493792 11.00000 -1.20000 AFIX 0 C31 1 0.255592 0.822208 0.414536 11.00000 0.02850 0.02363 = 0.02455 0.00082 -0.00376 0.00401 AFIX 43 H31 2 0.184156 0.855115 0.415744 11.00000 -1.20000 AFIX 0 C32 1 0.337334 0.851748 0.366398 11.00000 0.03957 0.02442 = 0.01966 0.00907 -0.00564 -0.00198 AFIX 43 H32 2 0.321630 0.905285 0.334856 11.00000 -1.20000 AFIX 0 C33 1 0.441100 0.804114 0.363939 11.00000 0.02954 0.03025 = 0.02030 0.00578 0.00307 -0.00715 AFIX 43 H33 2 0.496239 0.824739 0.330637 11.00000 -1.20000 AFIX 0 C34 1 0.465128 0.726241 0.409924 11.00000 0.02102 0.02645 = 0.01880 0.00245 0.00321 -0.00158 AFIX 43 H34 2 0.536337 0.693019 0.407994 11.00000 -1.20000 AFIX 0 HKLF 4 REM cp124135r_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.0983, GooF = S = 1.030, Restrained GooF = 1.029 for all data REM R1 = 0.0398 for 4931 Fo > 4sig(Fo) and 0.0469 for all 5425 data REM 401 parameters refined using 3 restraints END WGHT 0.0545 0.4425 REM Instructions for potential hydrogen bonds HTAB O1 O4_$1 HTAB O1W O1 HTAB O1W O8 HTAB O3 O1W_$2 REM Highest difference peak 0.197, deepest hole -0.234, 1-sigma level 0.046 Q1 1 0.0916 0.2970 0.5780 11.00000 0.05 0.20 Q2 1 0.4040 0.8407 0.7781 11.00000 0.05 0.19 Q3 1 0.3660 0.5198 0.7531 11.00000 0.05 0.19 Q4 1 0.1557 0.3767 0.5830 11.00000 0.05 0.19 Q5 1 0.4504 0.5848 0.7684 11.00000 0.05 0.19 Q6 1 0.4054 0.8595 0.3804 11.00000 0.05 0.18 Q7 1 0.4855 0.5815 0.8362 11.00000 0.05 0.18 Q8 1 0.3298 0.6951 0.4516 11.00000 0.05 0.17 Q9 1 0.2118 0.2947 0.7342 11.00000 0.05 0.17 Q10 1 0.1163 0.3744 0.6905 11.00000 0.05 0.17 Q11 1 0.6696 0.3482 0.5984 11.00000 0.05 0.17 Q12 1 0.4278 0.6445 0.8049 11.00000 0.05 0.17 Q13 1 0.3799 0.6399 0.4719 11.00000 0.05 0.16 Q14 1 0.3013 0.6676 0.5742 11.00000 0.05 0.16 Q15 1 0.4018 0.5737 0.7102 11.00000 0.05 0.16 Q16 1 0.1848 0.9372 0.3554 11.00000 0.05 0.15 Q17 1 0.0260 0.2234 0.5765 11.00000 0.05 0.15 Q18 1 0.5826 0.3667 0.5908 11.00000 0.05 0.15 Q19 1 0.2148 0.3407 0.8430 11.00000 0.05 0.15 Q20 1 -0.0295 0.3005 0.5806 11.00000 0.05 0.15 ; _shelx_res_checksum 20097 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_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 O O1 0.50438(17) 0.47639(16) 0.71403(10) 0.0169(4) Uani d 1 H H1 0.498(2) 0.423(3) 0.7356(16) 0.025 Uiso calc 1 O O2 0.01638(17) 0.25183(15) 0.67636(10) 0.0208(4) Uani d 1 O O1W 0.63748(19) 0.41758(16) 0.59717(11) 0.0264(5) Uani d 1 H HWA 0.614(3) 0.442(2) 0.6356(7) 0.040 Uiso d 1 H HWB 0.610(3) 0.451(2) 0.5630(8) 0.040 Uiso d 1 O O3 0.3949(2) 0.72018(17) 0.88174(10) 0.0244(5) Uani d 1 H H3 0.381(3) 0.780(3) 0.8896(9) 0.037 Uiso calc 1 O O4 0.44345(18) 0.78239(15) 0.77797(10) 0.0222(5) Uani d 1 O O5 0.31651(16) 0.68572(14) 0.68136(9) 0.0153(4) Uani d 1 O O6 0.41856(17) 0.78789(15) 0.61026(10) 0.0196(4) Uani d 1 O O7 0.32786(16) 0.59542(15) 0.55359(9) 0.0164(4) Uani d 1 O O8 0.50711(18) 0.57755(17) 0.51448(10) 0.0243(5) Uani d 1 C C1 0.3445(2) 0.4239(2) 0.82933(13) 0.0169(6) Uani d 1 H H1A 0.275590 0.389055 0.846246 0.020 Uiso calc 1 H H1B 0.399822 0.371907 0.814829 0.020 Uiso calc 1 C C2 0.3947(3) 0.4855(2) 0.88895(14) 0.0200(6) Uani d 1 H H2A 0.413298 0.440659 0.928742 0.024 Uiso calc 1 H H2B 0.338465 0.535594 0.905294 0.024 Uiso calc 1 C C3 0.5013(3) 0.5393(2) 0.86435(14) 0.0191(6) Uani d 1 H H3A 0.559558 0.487970 0.853582 0.023 Uiso calc 1 H H3B 0.530399 0.580736 0.903561 0.023 Uiso calc 1 C C4 0.4874(2) 0.6082(2) 0.79929(14) 0.0173(6) Uani d 1 C C5 0.4224(2) 0.5473(2) 0.73970(14) 0.0143(6) Uani d 1 C C6 0.3989(2) 0.6071(2) 0.67137(14) 0.0147(6) Uani d 1 H H6 0.471384 0.637824 0.654684 0.018 Uiso calc 1 C C7 0.3546(2) 0.5350(2) 0.61502(14) 0.0150(6) Uani d 1 H H7 0.415279 0.485543 0.602790 0.018 Uiso calc 1 C C8 0.2478(3) 0.4785(2) 0.63531(13) 0.0155(6) Uani d 1 H H8 0.186764 0.528923 0.644741 0.019 Uiso calc 1 C C9 0.2713(2) 0.4192(2) 0.70451(13) 0.0155(6) Uani d 1 H H9 0.334191 0.370940 0.694319 0.019 Uiso calc 1 C C10 0.3135(2) 0.4897(2) 0.76501(14) 0.0148(6) Uani d 1 C C11 0.1683(2) 0.3559(2) 0.72822(14) 0.0179(6) Uani d 1 H H11A 0.194840 0.298367 0.756862 0.021 Uiso calc 1 H H11B 0.117878 0.397728 0.757681 0.021 Uiso calc 1 C C12 0.1045(3) 0.3179(2) 0.66718(15) 0.0178(6) Uani d 1 C C13 0.1173(3) 0.3412(2) 0.59897(15) 0.0188(6) Uani d 1 C C14 0.2088(2) 0.4101(2) 0.57349(14) 0.0182(6) Uani d 1 H H14 0.175084 0.454722 0.536778 0.022 Uiso calc 1 C C15 0.0311(3) 0.2860(2) 0.56192(15) 0.0232(7) Uani d 1 H H15 0.017844 0.286084 0.512817 0.028 Uiso calc 1 C C16 -0.0266(3) 0.2344(2) 0.61042(15) 0.0239(7) Uani d 1 H H16 -0.088919 0.191433 0.600640 0.029 Uiso calc 1 C C17 0.4377(2) 0.7109(2) 0.81719(14) 0.0176(6) Uani d 1 C C18 0.6083(2) 0.6352(2) 0.77395(15) 0.0210(6) Uani d 1 H H18A 0.649574 0.573260 0.762598 0.031 Uiso calc 1 H H18B 0.648405 0.671535 0.811094 0.031 Uiso calc 1 H H18C 0.603385 0.677712 0.732109 0.031 Uiso calc 1 C C19 0.2189(2) 0.5629(2) 0.78820(14) 0.0165(6) Uani d 1 H H19A 0.178146 0.587521 0.746845 0.025 Uiso calc 1 H H19B 0.252518 0.619990 0.813222 0.025 Uiso calc 1 H H19C 0.165902 0.527710 0.819244 0.025 Uiso calc 1 C C20 0.3041(3) 0.3486(2) 0.53868(15) 0.0258(7) Uani d 1 H H20A 0.271281 0.302184 0.504307 0.039 Uiso calc 1 H H20B 0.344815 0.310097 0.574548 0.039 Uiso calc 1 H H20C 0.356908 0.394307 0.515049 0.039 Uiso calc 1 C C21 0.3382(2) 0.7741(2) 0.64816(14) 0.0171(6) Uani d 1 C C22 0.2512(2) 0.8514(2) 0.66403(14) 0.0173(6) Uani d 1 C C23 0.1932(3) 0.8533(2) 0.72745(16) 0.0218(6) Uani d 1 H H23 0.203683 0.800542 0.760439 0.026 Uiso calc 1 C C24 0.1201(3) 0.9321(2) 0.74262(17) 0.0256(7) Uani d 1 H H24 0.081958 0.934114 0.786437 0.031 Uiso calc 1 C C25 0.1025(3) 1.0083(2) 0.69359(18) 0.0275(7) Uani d 1 H H25 0.052511 1.062358 0.703969 0.033 Uiso calc 1 C C26 0.1582(3) 1.0050(2) 0.62952(17) 0.0253(7) Uani d 1 H H26 0.144897 1.056131 0.595677 0.030 Uiso calc 1 C C27 0.2331(3) 0.9277(2) 0.61472(15) 0.0216(6) Uani d 1 H H27 0.272173 0.926462 0.571194 0.026 Uiso calc 1 C C28 0.4154(2) 0.6172(2) 0.51063(14) 0.0175(6) Uani d 1 C C29 0.3839(3) 0.6969(2) 0.45916(14) 0.0189(6) Uani d 1 C C30 0.2788(2) 0.7442(2) 0.46095(14) 0.0194(6) Uani d 1 H H30 0.223119 0.723328 0.493792 0.023 Uiso calc 1 C C31 0.2556(3) 0.8222(2) 0.41454(16) 0.0256(7) Uani d 1 H H31 0.184156 0.855115 0.415744 0.031 Uiso calc 1 C C32 0.3373(3) 0.8517(3) 0.36640(16) 0.0279(7) Uani d 1 H H32 0.321630 0.905285 0.334856 0.033 Uiso calc 1 C C33 0.4411(3) 0.8041(3) 0.36394(16) 0.0267(7) Uani d 1 H H33 0.496239 0.824739 0.330637 0.032 Uiso calc 1 C C34 0.4651(3) 0.7262(2) 0.40992(15) 0.0221(6) Uani d 1 H H34 0.536337 0.693019 0.407994 0.027 Uiso calc 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 O1 0.0187(11) 0.0154(10) 0.0167(9) 0.0038(9) 0.0027(8) 0.0020(7) O2 0.0228(11) 0.0219(11) 0.0177(10) -0.0070(9) -0.0007(8) 0.0001(8) O1W 0.0306(13) 0.0244(12) 0.0243(10) 0.0037(10) 0.0089(9) 0.0046(9) O3 0.0342(13) 0.0197(11) 0.0194(10) 0.0030(10) 0.0037(9) -0.0026(8) O4 0.0307(12) 0.0169(10) 0.0190(10) -0.0040(9) -0.0041(9) 0.0005(8) O5 0.0152(10) 0.0142(10) 0.0166(9) 0.0018(8) 0.0008(8) 0.0007(7) O6 0.0203(11) 0.0204(11) 0.0180(9) -0.0015(9) 0.0015(8) 0.0023(8) O7 0.0170(10) 0.0190(10) 0.0131(9) -0.0003(9) 0.0025(8) 0.0030(7) O8 0.0216(11) 0.0305(12) 0.0207(10) 0.0051(10) 0.0040(9) 0.0061(9) C1 0.0196(14) 0.0167(14) 0.0143(12) 0.0003(12) 0.0023(11) 0.0027(10) C2 0.0245(16) 0.0222(15) 0.0133(13) 0.0031(13) -0.0010(11) 0.0018(11) C3 0.0223(16) 0.0172(15) 0.0178(13) 0.0023(13) -0.0059(12) 0.0015(11) C4 0.0179(15) 0.0192(15) 0.0148(13) -0.0021(13) -0.0019(11) -0.0012(10) C5 0.0163(14) 0.0135(14) 0.0132(12) 0.0019(12) -0.0012(11) -0.0007(10) C6 0.0141(13) 0.0141(13) 0.0158(12) 0.0001(12) 0.0025(11) 0.0025(10) C7 0.0177(15) 0.0152(14) 0.0120(12) 0.0036(12) 0.0005(11) 0.0020(10) C8 0.0168(14) 0.0152(14) 0.0144(12) 0.0016(12) 0.0017(11) -0.0002(10) C9 0.0171(14) 0.0153(14) 0.0140(12) 0.0016(12) 0.0020(10) 0.0006(10) C10 0.0151(14) 0.0166(14) 0.0127(12) 0.0013(12) -0.0001(11) -0.0008(10) C11 0.0200(15) 0.0180(14) 0.0156(13) -0.0021(12) 0.0032(12) 0.0013(11) C12 0.0187(15) 0.0150(13) 0.0197(13) 0.0001(12) 0.0038(12) -0.0023(11) C13 0.0209(16) 0.0181(15) 0.0174(13) -0.0008(13) -0.0018(12) -0.0025(11) C14 0.0205(15) 0.0200(15) 0.0140(12) -0.0032(13) 0.0002(11) 0.0004(11) C15 0.0260(16) 0.0253(17) 0.0183(14) -0.0061(14) -0.0014(12) -0.0023(12) C16 0.0235(16) 0.0272(17) 0.0210(15) -0.0087(14) -0.0038(12) -0.0047(12) C17 0.0156(14) 0.0205(15) 0.0169(13) -0.0035(12) -0.0052(11) -0.0022(11) C18 0.0172(15) 0.0243(16) 0.0214(14) -0.0026(13) -0.0040(12) -0.0002(12) C19 0.0163(14) 0.0184(14) 0.0147(12) 0.0009(12) 0.0022(11) 0.0001(10) C20 0.0312(18) 0.0277(17) 0.0184(14) -0.0071(15) 0.0062(13) -0.0071(12) C21 0.0202(15) 0.0159(14) 0.0151(12) -0.0016(12) -0.0055(11) -0.0002(10) C22 0.0161(14) 0.0142(14) 0.0215(13) -0.0022(12) -0.0051(11) -0.0018(11) C23 0.0199(15) 0.0183(14) 0.0272(15) -0.0027(13) -0.0025(12) -0.0001(12) C24 0.0190(15) 0.0223(16) 0.0355(17) -0.0038(14) 0.0013(13) -0.0082(13) C25 0.0169(15) 0.0181(16) 0.0476(19) 0.0021(14) -0.0073(15) -0.0073(14) C26 0.0229(16) 0.0172(16) 0.0359(17) 0.0014(14) -0.0126(14) 0.0026(12) C27 0.0199(15) 0.0198(15) 0.0249(14) -0.0016(13) -0.0072(12) -0.0002(12) C28 0.0199(15) 0.0181(15) 0.0144(12) -0.0009(13) 0.0002(11) -0.0020(10) C29 0.0257(16) 0.0180(15) 0.0129(12) -0.0036(13) 0.0001(11) -0.0013(11) C30 0.0218(15) 0.0204(15) 0.0161(13) -0.0030(13) 0.0020(11) -0.0016(11) C31 0.0285(17) 0.0236(16) 0.0245(15) 0.0040(14) -0.0038(13) 0.0008(12) C32 0.0396(19) 0.0244(16) 0.0197(14) -0.0020(16) -0.0056(14) 0.0091(12) C33 0.0295(17) 0.0302(18) 0.0203(15) -0.0072(15) 0.0031(13) 0.0058(12) C34 0.0210(15) 0.0265(17) 0.0188(14) -0.0016(14) 0.0032(11) 0.0025(12) 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_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C5 O1 H1 109.5 C12 O2 C16 105.7(2) HWA O1W HWB 109.7(3) C17 O3 H3 109.5 C21 O5 C6 116.0(2) C28 O7 C7 116.2(2) C2 C1 C10 112.4(2) C2 C1 H1A 109.1 C10 C1 H1A 109.1 C2 C1 H1B 109.1 C10 C1 H1B 109.1 H1A C1 H1B 107.9 C1 C2 C3 110.1(2) C1 C2 H2A 109.6 C3 C2 H2A 109.6 C1 C2 H2B 109.6 C3 C2 H2B 109.6 H2A C2 H2B 108.2 C2 C3 C4 115.9(2) C2 C3 H3A 108.3 C4 C3 H3A 108.3 C2 C3 H3B 108.3 C4 C3 H3B 108.3 H3A C3 H3B 107.4 C17 C4 C18 102.6(2) C17 C4 C3 112.9(2) C18 C4 C3 106.8(2) C17 C4 C5 115.5(2) C18 C4 C5 109.8(2) C3 C4 C5 108.8(2) O1 C5 C6 99.8(2) O1 C5 C10 109.7(2) C6 C5 C10 111.2(2) O1 C5 C4 104.6(2) C6 C5 C4 115.2(2) C10 C5 C4 114.9(2) O5 C6 C7 108.4(2) O5 C6 C5 112.4(2) C7 C6 C5 109.3(2) O5 C6 H6 108.9 C7 C6 H6 108.9 C5 C6 H6 108.9 O7 C7 C8 107.4(2) O7 C7 C6 107.1(2) C8 C7 C6 114.4(2) O7 C7 H7 109.3 C8 C7 H7 109.3 C6 C7 H7 109.3 C7 C8 C14 109.9(2) C7 C8 C9 108.5(2) C14 C8 C9 113.5(2) C7 C8 H8 108.3 C14 C8 H8 108.3 C9 C8 H8 108.3 C11 C9 C8 112.5(2) C11 C9 C10 111.0(2) C8 C9 C10 112.2(2) C11 C9 H9 106.9 C8 C9 H9 106.9 C10 C9 H9 106.9 C19 C10 C1 107.4(2) C19 C10 C9 110.9(2) C1 C10 C9 108.8(2) C19 C10 C5 111.9(2) C1 C10 C5 108.9(2) C9 C10 C5 108.9(2) C12 C11 C9 110.9(2) C12 C11 H11A 109.5 C9 C11 H11A 109.5 C12 C11 H11B 109.5 C9 C11 H11B 109.5 H11A C11 H11B 108.1 C13 C12 O2 110.9(3) C13 C12 C11 128.8(3) O2 C12 C11 120.3(2) C12 C13 C15 106.1(3) C12 C13 C14 122.4(3) C15 C13 C14 131.5(3) C13 C14 C20 110.0(2) C13 C14 C8 108.9(2) C20 C14 C8 114.8(2) C13 C14 H14 107.6 C20 C14 H14 107.6 C8 C14 H14 107.6 C16 C15 C13 106.3(3) C16 C15 H15 126.8 C13 C15 H15 126.8 C15 C16 O2 111.1(3) C15 C16 H16 124.5 O2 C16 H16 124.5 O4 C17 O3 121.2(3) O4 C17 C4 122.8(3) O3 C17 C4 115.7(2) C4 C18 H18A 109.5 C4 C18 H18B 109.5 H18A C18 H18B 109.5 C4 C18 H18C 109.5 H18A C18 H18C 109.5 H18B C18 H18C 109.5 C10 C19 H19A 109.5 C10 C19 H19B 109.5 H19A C19 H19B 109.5 C10 C19 H19C 109.5 H19A C19 H19C 109.5 H19B C19 H19C 109.5 C14 C20 H20A 109.5 C14 C20 H20B 109.5 H20A C20 H20B 109.5 C14 C20 H20C 109.5 H20A C20 H20C 109.5 H20B C20 H20C 109.5 O6 C21 O5 124.0(3) O6 C21 C22 124.1(3) O5 C21 C22 111.9(2) C23 C22 C27 119.8(3) C23 C22 C21 122.1(3) C27 C22 C21 118.0(3) C24 C23 C22 120.1(3) C24 C23 H23 120.0 C22 C23 H23 120.0 C23 C24 C25 120.1(3) C23 C24 H24 120.0 C25 C24 H24 120.0 C26 C25 C24 119.8(3) C26 C25 H25 120.1 C24 C25 H25 120.1 C27 C26 C25 120.4(3) C27 C26 H26 119.8 C25 C26 H26 119.8 C26 C27 C22 119.8(3) C26 C27 H27 120.1 C22 C27 H27 120.1 O8 C28 O7 123.8(3) O8 C28 C29 125.0(3) O7 C28 C29 111.2(2) C30 C29 C34 120.1(3) C30 C29 C28 121.8(3) C34 C29 C28 118.0(3) C31 C30 C29 119.8(3) C31 C30 H30 120.1 C29 C30 H30 120.1 C32 C31 C30 119.7(3) C32 C31 H31 120.2 C30 C31 H31 120.2 C33 C32 C31 120.6(3) C33 C32 H32 119.7 C31 C32 H32 119.7 C32 C33 C34 120.2(3) C32 C33 H33 119.9 C34 C33 H33 119.9 C33 C34 C29 119.6(3) C33 C34 H34 120.2 C29 C34 H34 120.2 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C5 1.436(3) O1 H1 0.82(4) O2 C12 1.372(4) O2 C16 1.376(3) O1W HWA 0.8501(14) O1W HWB 0.8501(14) O3 C17 1.337(3) O3 H3 0.82(4) O4 C17 1.211(3) O5 C21 1.358(3) O5 C6 1.440(3) O6 C21 1.207(4) O7 C28 1.350(3) O7 C7 1.455(3) O8 C28 1.206(4) C1 C2 1.522(4) C1 C10 1.551(4) C1 H1A 0.9900 C1 H1B 0.9900 C2 C3 1.522(4) C2 H2A 0.9900 C2 H2B 0.9900 C3 C4 1.551(4) C3 H3A 0.9900 C3 H3B 0.9900 C4 C17 1.524(4) C4 C18 1.549(4) C4 C5 1.593(4) C5 C6 1.552(4) C5 C10 1.572(4) C6 C7 1.532(4) C6 H6 1.0000 C7 C8 1.517(4) C7 H7 1.0000 C8 C14 1.559(4) C8 C9 1.562(3) C8 H8 1.0000 C9 C11 1.546(4) C9 C10 1.567(4) C9 H9 1.0000 C10 C19 1.546(4) C11 C12 1.476(4) C11 H11A 0.9900 C11 H11B 0.9900 C12 C13 1.347(4) C13 C15 1.441(4) C13 C14 1.496(4) C14 C20 1.541(4) C14 H14 1.0000 C15 C16 1.337(4) C15 H15 0.9500 C16 H16 0.9500 C18 H18A 0.9800 C18 H18B 0.9800 C18 H18C 0.9800 C19 H19A 0.9800 C19 H19B 0.9800 C19 H19C 0.9800 C20 H20A 0.9800 C20 H20B 0.9800 C20 H20C 0.9800 C21 C22 1.484(4) C22 C23 1.391(4) C22 C27 1.400(4) C23 C24 1.387(4) C23 H23 0.9500 C24 C25 1.394(5) C24 H24 0.9500 C25 C26 1.389(5) C25 H25 0.9500 C26 C27 1.384(4) C26 H26 0.9500 C27 H27 0.9500 C28 C29 1.491(4) C29 C30 1.391(4) C29 C34 1.398(4) C30 C31 1.390(4) C30 H30 0.9500 C31 C32 1.389(5) C31 H31 0.9500 C32 C33 1.379(5) C32 H32 0.9500 C33 C34 1.386(4) C33 H33 0.9500 C34 H34 0.9500 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O1 H1 O4 3_646 0.82(4) 2.01(4) 2.654(3) 134(4) O1W HWA O1 1_555 0.848(19) 2.03(3) 2.838(3) 158.6(15) O1W HWB O8 1_555 0.85(2) 2.27(3) 3.062(3) 154.2(19) O3 H3 O1W 3_656 0.83(4) 1.86(4) 2.680(3) 174(4) C19 H19B O3 1_555 0.98 2.51 3.445(3) 159 C1 H1A Cg1 2_565 0.99 2.98 3.910(3) 157 C34 H34 Cg2 4_566 0.95 2.85 3.655(3) 143 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 C10 C1 C2 C3 -59.2(3) C1 C2 C3 C4 56.0(3) C2 C3 C4 C17 80.5(3) C2 C3 C4 C18 -167.5(2) C2 C3 C4 C5 -49.1(3) C17 C4 C5 O1 158.7(2) C18 C4 C5 O1 43.5(3) C3 C4 C5 O1 -73.1(3) C17 C4 C5 C6 50.3(3) C18 C4 C5 C6 -65.0(3) C3 C4 C5 C6 178.5(2) C17 C4 C5 C10 -80.9(3) C18 C4 C5 C10 163.8(2) C3 C4 C5 C10 47.3(3) C21 O5 C6 C7 -99.4(2) C21 O5 C6 C5 139.7(2) O1 C5 C6 O5 179.7(2) C10 C5 C6 O5 64.0(3) C4 C5 C6 O5 -69.0(3) O1 C5 C6 C7 59.3(3) C10 C5 C6 C7 -56.4(3) C4 C5 C6 C7 170.6(2) C28 O7 C7 C8 -153.2(2) C28 O7 C7 C6 83.4(3) O5 C6 C7 O7 54.0(3) C5 C6 C7 O7 176.8(2) O5 C6 C7 C8 -64.9(3) C5 C6 C7 C8 57.9(3) O7 C7 C8 C14 59.6(3) C6 C7 C8 C14 178.4(2) O7 C7 C8 C9 -175.8(2) C6 C7 C8 C9 -57.0(3) C7 C8 C9 C11 -178.0(2) C14 C8 C9 C11 -55.5(3) C7 C8 C9 C10 56.0(3) C14 C8 C9 C10 178.5(2) C2 C1 C10 C19 -64.1(3) C2 C1 C10 C9 175.8(2) C2 C1 C10 C5 57.2(3) C11 C9 C10 C19 -59.9(3) C8 C9 C10 C19 67.0(3) C11 C9 C10 C1 58.0(3) C8 C9 C10 C1 -175.2(2) C11 C9 C10 C5 176.6(2) C8 C9 C10 C5 -56.6(3) O1 C5 C10 C19 -175.8(2) C6 C5 C10 C19 -66.5(3) C4 C5 C10 C19 66.6(3) O1 C5 C10 C1 65.6(3) C6 C5 C10 C1 175.0(2) C4 C5 C10 C1 -51.9(3) O1 C5 C10 C9 -52.9(3) C6 C5 C10 C9 56.5(3) C4 C5 C10 C9 -170.4(2) C8 C9 C11 C12 33.3(3) C10 C9 C11 C12 160.0(2) C16 O2 C12 C13 -0.1(3) C16 O2 C12 C11 178.0(3) C9 C11 C12 C13 -8.6(4) C9 C11 C12 O2 173.6(2) O2 C12 C13 C15 0.0(3) C11 C12 C13 C15 -178.0(3) O2 C12 C13 C14 -178.6(2) C11 C12 C13 C14 3.4(5) C12 C13 C14 C20 104.1(3) C15 C13 C14 C20 -74.1(4) C12 C13 C14 C8 -22.5(4) C15 C13 C14 C8 159.2(3) C7 C8 C14 C13 169.4(2) C9 C8 C14 C13 47.7(3) C7 C8 C14 C20 45.6(3) C9 C8 C14 C20 -76.1(3) C12 C13 C15 C16 0.2(4) C14 C13 C15 C16 178.6(3) C13 C15 C16 O2 -0.3(4) C12 O2 C16 C15 0.3(3) C18 C4 C17 O4 48.5(3) C3 C4 C17 O4 163.0(3) C5 C4 C17 O4 -70.8(4) C18 C4 C17 O3 -126.3(2) C3 C4 C17 O3 -11.8(4) C5 C4 C17 O3 114.4(3) C6 O5 C21 O6 2.4(4) C6 O5 C21 C22 -177.6(2) O6 C21 C22 C23 -150.1(3) O5 C21 C22 C23 30.0(4) O6 C21 C22 C27 26.0(4) O5 C21 C22 C27 -153.9(2) C27 C22 C23 C24 -1.8(4) C21 C22 C23 C24 174.2(3) C22 C23 C24 C25 1.5(4) C23 C24 C25 C26 0.1(5) C24 C25 C26 C27 -1.5(5) C25 C26 C27 C22 1.2(4) C23 C22 C27 C26 0.4(4) C21 C22 C27 C26 -175.7(3) C7 O7 C28 O8 11.8(4) C7 O7 C28 C29 -167.4(2) O8 C28 C29 C30 -175.4(3) O7 C28 C29 C30 3.7(4) O8 C28 C29 C34 2.2(4) O7 C28 C29 C34 -178.7(3) C34 C29 C30 C31 -1.3(4) C28 C29 C30 C31 176.3(3) C29 C30 C31 C32 0.4(4) C30 C31 C32 C33 0.4(5) C31 C32 C33 C34 -0.3(5) C32 C33 C34 C29 -0.5(5) C30 C29 C34 C33 1.3(4) C28 C29 C34 C33 -176.3(3) _cod_database_fobs_code 2242813