data_me _audit_creation_date 2019-06-27 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C19 H28 O6' _chemical_formula_sum 'C19 H28 O6' _chemical_formula_weight 352.41 _chemical_absolute_configuration ad _chemical_melting_point ? 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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.17106(13) _cell_length_b 34.8703(6) _cell_length_c 9.23924(15) _cell_angle_alpha 90 _cell_angle_beta 91.1734(15) _cell_angle_gamma 90 _cell_volume 2631.96(8) _cell_formula_units_Z 6 _cell_measurement_reflns_used 8254 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.4250 _cell_measurement_theta_min 4.7730 _shelx_estimated_absorpt_T_max 0.916 _shelx_estimated_absorpt_T_min 0.895 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.80801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1140 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_unetI/netI 0.0307 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 10571 _diffrn_reflns_point_group_measured_fraction_full 0.752 _diffrn_reflns_point_group_measured_fraction_max 0.717 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.551 _diffrn_reflns_theta_min 2.534 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2684 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.969 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w 18.00 45.00 1.00 1.00 -- 41.11 -99.00 90.00 27 2 \w 32.00 81.00 1.00 1.00 -- 41.11-125.00 60.00 49 3 \w 43.00 120.00 1.00 1.00 -- 106.95-125.00 -30.00 77 4 \w 79.00 139.00 1.00 1.00 -- 106.95 -77.00 0.00 60 5 \w 108.00 133.00 1.00 1.00 -- 106.95 -30.00 150.00 25 6 \w 81.00 149.00 1.00 1.00 -- 106.95 45.00 150.00 68 7 \w 101.00 136.00 1.00 1.00 -- 106.95 112.00 70.00 35 8 \w 80.00 164.00 1.00 1.00 -- 106.95 30.00 30.00 84 9 \w 109.00 134.00 1.00 1.00 -- 106.95 125.00-150.00 25 10 \w 42.00 68.00 1.00 1.00 -- 106.95 -77.00 0.00 26 11 \w 39.00 96.00 1.00 1.00 -- 106.95 -95.00-180.00 57 12 \w -129.00 -4.00 1.00 1.00 -- -41.11 0.00 120.00 125 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0781545000 _diffrn_orient_matrix_UB_12 0.0393506000 _diffrn_orient_matrix_UB_13 -0.0328234000 _diffrn_orient_matrix_UB_21 0.1715187000 _diffrn_orient_matrix_UB_22 0.0182025000 _diffrn_orient_matrix_UB_23 -0.0056063000 _diffrn_orient_matrix_UB_31 0.0060532000 _diffrn_orient_matrix_UB_32 -0.0085092000 _diffrn_orient_matrix_UB_33 -0.1634472000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.456 _reflns_Friedel_fraction_full 0.496 _reflns_Friedel_fraction_max 0.457 _reflns_number_gt 7556 _reflns_number_total 7622 _reflns_odcompleteness_completeness 99.85 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 0.258 _refine_diff_density_min -0.430 _refine_diff_density_rms 0.069 _refine_ls_abs_structure_details ; Flack x determined using 2296 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 691 _refine_ls_number_reflns 7622 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0346 _refine_ls_restrained_S_all 1.043 _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^)+(0.0530P)^2^+0.6700P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.0908 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2.a Ternary CH refined with riding coordinates: C7D(H7D), C7B(H7BA), C5(H5) 2.b Secondary CH2 refined with riding coordinates: C11B(H11C,H11D), C1AA(H1AA,H1AB), C15B(H15C,H15D), C1B(H1BA,H1BB), C4B(H4BA, H4BB), C2(H2A,H2B), C14(H14A,H14B), C8(H8A,H8B), C7(H7A,H7B), C9D(H9DA,H9DB), C13(H13A,H13B), C2D(H2DA,H2DB), C1(H1A,H1B), C15D(H15E,H15F), C4D(H4DA,H4DB), C16D(H16F,H16G), C15(H15A,H15B), C2B(H2BA,H2BB), C11(H11A,H11B), C5B(H5BA, H5BB), C16B(H16D,H16E), C1D(H1DA,H1DB), C14D(H14C,H14D), C5D(H5DA,H5DB), C18B(H18C,H18D), C19B(H19C,H19D), C18(H18A,H18B), C18D(H18E,H18F), C19D(H19E, H19F), C19(H19A,H19B) 2.c Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C12B(H12D,H12E,H12F), C13B(H13C, H13D,H13E), C13D(H13F,H13G,H13H), C12D(H12G,H12H,H12I) 2.d Idealised tetrahedral OH refined as rotating group: O4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O2 O 0.2890(2) 0.52639(5) 0.55744(17) 0.0165(3) Uani 1 1 d . . . . . O3B O -0.4018(2) 0.60673(5) 0.86006(17) 0.0174(3) Uani 1 1 d . . . . . O1 O 0.44099(19) 0.54717(5) 0.36774(17) 0.0161(3) Uani 1 1 d . . . . . O4B O -0.2860(2) 0.63687(5) 1.05584(17) 0.0182(4) Uani 1 1 d . . . . . O5 O 0.4779(2) 0.49466(5) -0.04896(19) 0.0202(4) Uani 1 1 d . . . . . O3 O -0.0697(2) 0.56205(6) 0.56111(19) 0.0215(4) Uani 1 1 d . . . . . O2B O -0.4860(2) 0.65363(5) 0.43776(19) 0.0206(4) Uani 1 1 d . . . . . O4 O 0.0339(2) 0.47835(5) 0.50304(17) 0.0165(3) Uani 1 1 d . . . . . H4 H 0.090898 0.485927 0.571327 0.025 Uiso 1 1 calc GR . . . . O1D O 0.7908(2) 0.39250(5) -0.34480(18) 0.0192(4) Uani 1 1 d . . . . . O1B O -0.5098(2) 0.71907(6) 0.4489(2) 0.0234(4) Uani 1 1 d . . . . . O5B O -0.1027(2) 0.69983(5) 1.0141(2) 0.0217(4) Uani 1 1 d . . . . . O2D O 0.8976(2) 0.36013(5) -0.53516(19) 0.0212(4) Uani 1 1 d . . . . . O6 O 0.4103(2) 0.43092(5) -0.04073(19) 0.0210(4) Uani 1 1 d . . . . . O6D O 0.7008(2) 0.35113(6) 0.0744(2) 0.0229(4) Uani 1 1 d . . . . . O3D O 1.2984(3) 0.36569(8) -0.5435(2) 0.0365(5) Uani 1 1 d . . . . . O4D O 1.0696(2) 0.29528(6) -0.4817(2) 0.0274(4) Uani 1 1 d . . . . . O6B O 0.1105(2) 0.62685(6) 1.0747(2) 0.0272(4) Uani 1 1 d . . . . . O5D O 0.6564(3) 0.28633(6) 0.0697(2) 0.0309(5) Uani 1 1 d . . . . . C12 C -0.1404(3) 0.49863(7) 0.3122(3) 0.0164(5) Uani 1 1 d . . . . . H12A H -0.123400 0.475555 0.257847 0.025 Uiso 1 1 calc GR . . . . H12B H -0.165149 0.519354 0.246980 0.025 Uiso 1 1 calc GR . . . . H12C H -0.230014 0.495003 0.376397 0.025 Uiso 1 1 calc GR . . . . C7D C 0.9666(3) 0.34422(7) -0.1334(3) 0.0157(5) Uani 1 1 d . . . . . H7D H 0.912037 0.368207 -0.107445 0.019 Uiso 1 1 calc R . . . . C10 C -0.0026(3) 0.54916(7) 0.4574(2) 0.0158(5) Uani 1 1 d . . . . . C3 C 0.3261(3) 0.51875(7) 0.4077(2) 0.0132(4) Uani 1 1 d . . . . . C8B C -0.1687(3) 0.64765(7) 0.8180(2) 0.0135(4) Uani 1 1 d . . . . . C10B C 0.0264(3) 0.63506(8) 0.9702(3) 0.0189(5) Uani 1 1 d . . . . . C7B C -0.2161(3) 0.65524(7) 0.6569(2) 0.0137(4) Uani 1 1 d . . . . . H7BA H -0.274703 0.632078 0.625389 0.016 Uiso 1 1 calc R . . . . C11B C -0.0554(3) 0.61259(7) 0.8487(2) 0.0166(5) Uani 1 1 d . . . . . H11C H -0.113205 0.589943 0.880917 0.020 Uiso 1 1 calc R . . . . H11D H 0.016784 0.606497 0.769906 0.020 Uiso 1 1 calc R . . . . C3B C -0.3284(3) 0.64182(7) 0.9036(2) 0.0150(4) Uani 1 1 d . . . . . C17B C -0.3972(3) 0.68830(7) 0.4726(3) 0.0171(5) Uani 1 1 d . . . . . C9B C -0.0431(3) 0.67323(7) 0.9136(3) 0.0167(5) Uani 1 1 d . . . . . C6 C 0.2897(3) 0.47294(7) 0.1378(2) 0.0135(4) Uani 1 1 d . . . . . C16 C 0.1715(3) 0.43987(7) 0.1718(3) 0.0167(4) Uani 1 1 d . . . . . H16A H 0.137017 0.441955 0.270138 0.025 Uiso 1 1 calc GR . . . . H16B H 0.226209 0.415792 0.158527 0.025 Uiso 1 1 calc GR . . . . H16C H 0.077694 0.441248 0.107721 0.025 Uiso 1 1 calc GR . . . . C1AA C -0.0723(3) 0.65883(7) 0.5523(2) 0.0157(4) Uani 1 1 d . . . . . H1AA H -0.013968 0.682589 0.571237 0.019 Uiso 1 1 calc R . . . . H1AB H 0.003308 0.637743 0.568253 0.019 Uiso 1 1 calc R . . . . C15B C -0.1347(3) 0.65832(8) 0.3952(2) 0.0183(5) Uani 1 1 d . . . . . H15C H -0.043091 0.660908 0.330739 0.022 Uiso 1 1 calc R . . . . H15D H -0.188147 0.634032 0.374689 0.022 Uiso 1 1 calc R . . . . C1B C -0.4794(3) 0.59153(8) 0.9860(3) 0.0214(5) Uani 1 1 d . . . . . H1BA H -0.492188 0.563931 0.979281 0.026 Uiso 1 1 calc R . . . . H1BB H -0.585800 0.603179 0.999695 0.026 Uiso 1 1 calc R . . . . C5 C 0.2100(3) 0.51318(7) 0.1543(2) 0.0130(4) Uani 1 1 d . . . . . H5 H 0.295603 0.531312 0.126871 0.016 Uiso 1 1 calc R . . . . C6D C 0.8346(3) 0.31256(7) -0.1120(3) 0.0186(5) Uani 1 1 d . . . . . C4B C -0.4476(3) 0.67492(7) 0.8865(3) 0.0182(5) Uani 1 1 d . . . . . H4BA H -0.398421 0.698090 0.925952 0.022 Uiso 1 1 calc R . . . . H4BB H -0.545745 0.669505 0.940169 0.022 Uiso 1 1 calc R . . . . C2 C 0.5258(3) 0.55896(8) 0.4983(3) 0.0194(5) Uani 1 1 d . . . . . H2A H 0.567982 0.584847 0.489750 0.023 Uiso 1 1 calc R . . . . H2B H 0.615303 0.541686 0.522454 0.023 Uiso 1 1 calc R . . . . C12B C 0.0938(3) 0.69371(8) 0.8345(3) 0.0198(5) Uani 1 1 d . . . . . H12D H 0.049498 0.715342 0.782728 0.030 Uiso 1 1 calc GR . . . . H12E H 0.142906 0.676327 0.767499 0.030 Uiso 1 1 calc GR . . . . H12F H 0.175183 0.702349 0.903473 0.030 Uiso 1 1 calc GR . . . . C14 C 0.1347(3) 0.51587(7) -0.1118(3) 0.0194(5) Uani 1 1 d . . . . . H14A H 0.045547 0.519596 -0.181296 0.023 Uiso 1 1 calc R . . . . H14B H 0.216523 0.535456 -0.128426 0.023 Uiso 1 1 calc R . . . . C4 C 0.1696(3) 0.52398(7) 0.3128(2) 0.0129(4) Uani 1 1 d . . . . . C8 C 0.3994(3) 0.47900(7) 0.3966(2) 0.0152(4) Uani 1 1 d . . . . . H8A H 0.322363 0.460206 0.431890 0.018 Uiso 1 1 calc R . . . . H8B H 0.498161 0.477543 0.456391 0.018 Uiso 1 1 calc R . . . . C7 C 0.4403(3) 0.46988(7) 0.2391(3) 0.0159(5) Uani 1 1 d . . . . . H7A H 0.484536 0.444107 0.233881 0.019 Uiso 1 1 calc R . . . . H7B H 0.523822 0.487516 0.206869 0.019 Uiso 1 1 calc R . . . . C3D C 0.8575(3) 0.35652(7) -0.3856(3) 0.0167(5) Uani 1 1 d . . . . . C9D C 1.1362(3) 0.38347(8) -0.3250(3) 0.0213(5) Uani 1 1 d . . . . . H9DA H 1.083011 0.406451 -0.361907 0.026 Uiso 1 1 calc R . . . . H9DB H 1.209900 0.389409 -0.244478 0.026 Uiso 1 1 calc R . . . . C13 C 0.0705(3) 0.51965(7) 0.0423(2) 0.0167(5) Uani 1 1 d . . . . . H13A H -0.015400 0.500947 0.057001 0.020 Uiso 1 1 calc R . . . . H13B H 0.024309 0.545012 0.055260 0.020 Uiso 1 1 calc R . . . . C10D C 1.2127(3) 0.35893(9) -0.4413(3) 0.0256(6) Uani 1 1 d . . . . . C17D C 0.7779(3) 0.31485(8) 0.0474(3) 0.0218(5) Uani 1 1 d . . . . . C8D C 1.0156(3) 0.34979(7) -0.2943(3) 0.0168(5) Uani 1 1 d . . . . . C2D C 0.8335(3) 0.39549(8) -0.5903(3) 0.0234(5) Uani 1 1 d . . . . . H2DA H 0.774681 0.391578 -0.681340 0.028 Uiso 1 1 calc R . . . . H2DB H 0.920316 0.413992 -0.604622 0.028 Uiso 1 1 calc R . . . . C6B C -0.3419(3) 0.68845(7) 0.6338(3) 0.0157(4) Uani 1 1 d . . . . . C17 C 0.3458(3) 0.46852(7) -0.0210(3) 0.0165(5) Uani 1 1 d . . . . . C1 C 0.3917(3) 0.55678(8) 0.6095(3) 0.0207(5) Uani 1 1 d . . . . . H1A H 0.436785 0.550903 0.704886 0.025 Uiso 1 1 calc R . . . . H1B H 0.331558 0.580722 0.614069 0.025 Uiso 1 1 calc R . . . . C15D C 1.0466(3) 0.34167(8) 0.1325(3) 0.0226(5) Uani 1 1 d . . . . . H15E H 1.137765 0.338000 0.199906 0.027 Uiso 1 1 calc R . . . . H15F H 0.999012 0.366633 0.150998 0.027 Uiso 1 1 calc R . . . . C4D C 0.7308(3) 0.32484(8) -0.3697(3) 0.0201(5) Uani 1 1 d . . . . . H4DA H 0.774771 0.300892 -0.405572 0.024 Uiso 1 1 calc R . . . . H4DB H 0.633733 0.331076 -0.427170 0.024 Uiso 1 1 calc R . . . . C16D C 0.9189(3) 0.31067(8) 0.1562(3) 0.0239(5) Uani 1 1 d . . . . . H16F H 0.968795 0.285609 0.145642 0.029 Uiso 1 1 calc R . . . . H16G H 0.877818 0.312634 0.253636 0.029 Uiso 1 1 calc R . . . . C9 C 0.0147(3) 0.50812(7) 0.4005(2) 0.0133(4) Uani 1 1 d . . . . . C15 C 0.2100(3) 0.47627(7) -0.1329(3) 0.0186(5) Uani 1 1 d . . . . . H15A H 0.254246 0.474559 -0.229272 0.022 Uiso 1 1 calc R . . . . H15B H 0.125592 0.456883 -0.124535 0.022 Uiso 1 1 calc R . . . . C13B C -0.2699(3) 0.72809(7) 0.6719(3) 0.0193(5) Uani 1 1 d . . . . . H13C H -0.242016 0.728958 0.773250 0.029 Uiso 1 1 calc GR . . . . H13D H -0.349319 0.747598 0.649494 0.029 Uiso 1 1 calc GR . . . . H13E H -0.173384 0.732408 0.616577 0.029 Uiso 1 1 calc GR . . . . C13D C 0.9007(3) 0.27211(8) -0.1420(3) 0.0255(6) Uani 1 1 d . . . . . H13F H 0.926405 0.269895 -0.242614 0.038 Uiso 1 1 calc GR . . . . H13G H 0.819176 0.253429 -0.118308 0.038 Uiso 1 1 calc GR . . . . H13H H 0.997649 0.267748 -0.083983 0.038 Uiso 1 1 calc GR . . . . C2B C -0.3603(3) 0.60243(8) 1.1069(3) 0.0217(5) Uani 1 1 d . . . . . H2BA H -0.417144 0.606965 1.196467 0.026 Uiso 1 1 calc R . . . . H2BB H -0.279186 0.582482 1.122791 0.026 Uiso 1 1 calc R . . . . C11 C 0.1033(3) 0.56535(7) 0.3392(2) 0.0154(4) Uani 1 1 d . . . . . H11A H 0.185912 0.583276 0.373950 0.019 Uiso 1 1 calc R . . . . H11B H 0.041524 0.575892 0.257715 0.019 Uiso 1 1 calc R . . . . C5B C -0.4927(3) 0.68111(7) 0.7271(3) 0.0188(5) Uani 1 1 d . . . . . H5BA H -0.566435 0.702836 0.718521 0.023 Uiso 1 1 calc R . . . . H5BB H -0.550234 0.658661 0.690636 0.023 Uiso 1 1 calc R . . . . C16B C -0.2552(3) 0.69107(8) 0.3688(2) 0.0192(5) Uani 1 1 d . . . . . H16D H -0.296702 0.689998 0.269755 0.023 Uiso 1 1 calc R . . . . H16E H -0.199466 0.715404 0.382463 0.023 Uiso 1 1 calc R . . . . C11D C 1.1360(3) 0.32205(8) -0.3829(3) 0.0227(5) Uani 1 1 d . . . . . C1D C 0.7184(3) 0.40882(8) -0.4728(3) 0.0230(5) Uani 1 1 d . . . . . H1DA H 0.714991 0.436577 -0.466952 0.028 Uiso 1 1 calc R . . . . H1DB H 0.608303 0.399157 -0.489823 0.028 Uiso 1 1 calc R . . . . C14D C 1.1086(3) 0.34033(8) -0.0231(3) 0.0202(5) Uani 1 1 d . . . . . H14C H 1.164949 0.316252 -0.038740 0.024 Uiso 1 1 calc R . . . . H14D H 1.186135 0.360993 -0.037230 0.024 Uiso 1 1 calc R . . . . C12D C 1.2687(3) 0.30097(9) -0.2970(3) 0.0285(6) Uani 1 1 d . . . . . H12G H 1.220050 0.280766 -0.241888 0.043 Uiso 1 1 calc GR . . . . H12H H 1.323533 0.318575 -0.232562 0.043 Uiso 1 1 calc GR . . . . H12I H 1.346239 0.290237 -0.362334 0.043 Uiso 1 1 calc GR . . . . C5D C 0.6850(3) 0.32014(8) -0.2114(3) 0.0198(5) Uani 1 1 d . . . . . H5DA H 0.608745 0.298967 -0.203268 0.024 Uiso 1 1 calc R . . . . H5DB H 0.630175 0.343214 -0.179436 0.024 Uiso 1 1 calc R . . . . C18B C -0.6451(3) 0.66372(10) 0.3836(3) 0.0314(6) Uani 1 1 d . . . . . H18C H -0.727032 0.659836 0.456665 0.038 Uiso 1 1 calc R . . . . H18D H -0.674403 0.648654 0.298665 0.038 Uiso 1 1 calc R . . . . C19B C -0.6299(4) 0.70533(10) 0.3461(3) 0.0340(7) Uani 1 1 d . . . . . H19C H -0.593180 0.708621 0.247698 0.041 Uiso 1 1 calc R . . . . H19D H -0.733463 0.718541 0.356778 0.041 Uiso 1 1 calc R . . . . C18 C 0.6106(4) 0.47321(11) -0.1031(5) 0.0452(9) Uani 1 1 d . . . . . H18A H 0.703804 0.474534 -0.036543 0.054 Uiso 1 1 calc R . . . . H18B H 0.643110 0.483240 -0.196100 0.054 Uiso 1 1 calc R . . . . C18D C 0.5383(4) 0.34432(11) 0.1217(4) 0.0384(7) Uani 1 1 d . . . . . H18E H 0.459031 0.349238 0.044322 0.046 Uiso 1 1 calc R . . . . H18F H 0.513082 0.360476 0.203766 0.046 Uiso 1 1 calc R . . . . C19D C 0.5379(4) 0.30310(12) 0.1635(4) 0.0424(8) Uani 1 1 d . . . . . H19E H 0.569991 0.299852 0.264365 0.051 Uiso 1 1 calc R . . . . H19F H 0.430596 0.291784 0.147295 0.051 Uiso 1 1 calc R . . . . C19 C 0.5547(6) 0.43397(11) -0.1181(6) 0.0667(15) Uani 1 1 d . . . . . H19A H 0.534469 0.427836 -0.219260 0.080 Uiso 1 1 calc R . . . . H19B H 0.636594 0.416401 -0.079393 0.080 Uiso 1 1 calc R . . . . H5B H -0.154(5) 0.6880(13) 1.073(4) 0.036(10) Uiso 1 1 d . . . . . H4D H 1.027(6) 0.3080(14) -0.546(5) 0.046(12) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O2 0.0167(7) 0.0209(9) 0.0119(7) -0.0031(6) -0.0003(6) -0.0036(7) O3B 0.0227(8) 0.0147(8) 0.0150(8) 0.0015(7) 0.0003(6) -0.0085(7) O1 0.0152(7) 0.0177(9) 0.0155(8) -0.0012(7) 0.0002(6) -0.0064(6) O4B 0.0232(8) 0.0199(9) 0.0116(7) 0.0013(7) 0.0003(6) -0.0066(7) O5 0.0201(8) 0.0194(9) 0.0214(8) -0.0008(7) 0.0082(7) -0.0020(7) O3 0.0210(8) 0.0240(9) 0.0197(8) -0.0070(7) 0.0037(6) 0.0012(7) O2B 0.0178(8) 0.0224(9) 0.0215(8) 0.0030(7) -0.0040(6) -0.0002(7) O4 0.0189(8) 0.0165(8) 0.0142(7) 0.0036(6) -0.0002(6) -0.0027(7) O1D 0.0220(8) 0.0158(9) 0.0198(8) 0.0024(7) 0.0036(6) 0.0071(7) O1B 0.0227(9) 0.0222(10) 0.0252(9) 0.0065(7) 0.0000(7) 0.0071(7) O5B 0.0247(9) 0.0195(9) 0.0214(9) -0.0081(7) 0.0068(7) -0.0081(7) O2D 0.0219(8) 0.0220(9) 0.0196(9) -0.0021(7) 0.0020(7) 0.0060(7) O6 0.0263(9) 0.0157(9) 0.0210(8) -0.0047(7) 0.0042(7) 0.0042(7) O6D 0.0178(8) 0.0239(10) 0.0272(9) 0.0041(7) 0.0040(7) -0.0002(7) O3D 0.0268(10) 0.0530(14) 0.0299(11) -0.0088(10) 0.0096(8) -0.0011(10) O4D 0.0260(9) 0.0245(10) 0.0312(10) -0.0160(8) -0.0091(8) 0.0099(8) O6B 0.0267(9) 0.0347(11) 0.0200(9) 0.0038(8) -0.0071(7) -0.0034(8) O5D 0.0324(10) 0.0292(11) 0.0309(10) 0.0102(9) -0.0063(8) -0.0162(9) C12 0.0118(10) 0.0192(12) 0.0181(11) -0.0010(9) 0.0005(8) -0.0009(9) C7D 0.0154(10) 0.0114(11) 0.0203(11) -0.0023(9) -0.0024(8) 0.0011(9) C10 0.0138(10) 0.0156(12) 0.0178(11) -0.0022(9) -0.0031(8) 0.0004(9) C3 0.0133(10) 0.0153(12) 0.0110(10) -0.0002(9) 0.0008(8) -0.0030(9) C8B 0.0141(10) 0.0097(11) 0.0167(11) -0.0017(8) 0.0007(8) -0.0009(8) C10B 0.0165(10) 0.0236(13) 0.0165(11) -0.0011(10) 0.0004(9) -0.0018(9) C7B 0.0137(10) 0.0116(11) 0.0157(10) -0.0007(9) 0.0017(8) 0.0014(8) C11B 0.0197(11) 0.0160(12) 0.0140(11) -0.0008(9) -0.0021(8) 0.0004(9) C3B 0.0176(10) 0.0154(11) 0.0120(10) 0.0001(9) -0.0003(8) -0.0030(9) C17B 0.0172(10) 0.0139(11) 0.0203(11) 0.0037(9) 0.0026(9) 0.0024(9) C9B 0.0169(10) 0.0181(12) 0.0152(11) -0.0041(9) 0.0015(8) -0.0037(9) C6 0.0164(10) 0.0118(11) 0.0121(10) -0.0008(8) 0.0007(8) -0.0005(9) C16 0.0185(10) 0.0136(11) 0.0182(11) 0.0000(9) 0.0016(8) -0.0019(9) C1AA 0.0175(10) 0.0160(12) 0.0137(10) -0.0012(9) 0.0017(8) 0.0021(9) C15B 0.0188(11) 0.0216(13) 0.0146(11) 0.0000(10) 0.0017(8) 0.0026(10) C1B 0.0253(12) 0.0198(12) 0.0192(11) 0.0039(10) 0.0021(9) -0.0090(10) C5 0.0129(10) 0.0120(11) 0.0142(10) -0.0010(8) 0.0011(8) -0.0010(8) C6D 0.0195(11) 0.0123(12) 0.0237(12) 0.0005(9) -0.0074(9) -0.0016(9) C4B 0.0193(11) 0.0179(12) 0.0175(11) 0.0003(9) 0.0065(8) -0.0005(9) C2 0.0178(11) 0.0223(13) 0.0180(11) -0.0053(10) -0.0027(9) -0.0055(9) C12B 0.0156(10) 0.0229(13) 0.0209(11) -0.0039(10) 0.0015(9) -0.0060(9) C14 0.0240(12) 0.0192(13) 0.0150(11) 0.0001(9) -0.0005(9) 0.0031(10) C4 0.0136(10) 0.0113(11) 0.0138(10) -0.0001(8) -0.0002(8) -0.0007(8) C8 0.0127(10) 0.0172(12) 0.0155(11) 0.0011(9) -0.0021(8) 0.0006(8) C7 0.0136(10) 0.0147(11) 0.0193(11) -0.0008(9) 0.0012(8) 0.0025(9) C3D 0.0151(10) 0.0140(11) 0.0210(12) -0.0011(9) 0.0012(9) 0.0033(9) C9D 0.0192(11) 0.0205(13) 0.0244(12) -0.0051(10) 0.0025(9) -0.0031(10) C13 0.0177(11) 0.0178(12) 0.0146(11) -0.0003(9) 0.0004(8) 0.0021(9) C10D 0.0179(11) 0.0341(15) 0.0247(13) -0.0083(11) -0.0006(10) 0.0026(11) C17D 0.0209(11) 0.0165(12) 0.0277(13) 0.0064(10) -0.0057(10) -0.0055(10) C8D 0.0133(10) 0.0138(12) 0.0231(12) -0.0068(9) -0.0017(9) 0.0018(9) C2D 0.0294(13) 0.0195(13) 0.0215(12) 0.0045(10) 0.0047(10) 0.0034(11) C6B 0.0158(10) 0.0115(11) 0.0199(11) 0.0016(9) 0.0045(8) 0.0020(9) C17 0.0199(11) 0.0103(11) 0.0194(11) -0.0018(9) 0.0037(9) 0.0003(9) C1 0.0218(11) 0.0223(13) 0.0180(11) -0.0069(10) -0.0001(9) -0.0043(10) C15D 0.0207(11) 0.0214(13) 0.0254(13) -0.0024(11) -0.0068(9) -0.0030(10) C4D 0.0172(10) 0.0185(12) 0.0245(12) 0.0013(10) -0.0063(9) -0.0003(9) C16D 0.0280(13) 0.0198(13) 0.0237(12) 0.0035(10) -0.0084(10) -0.0055(10) C9 0.0133(10) 0.0135(11) 0.0129(10) 0.0009(8) 0.0007(8) 0.0000(8) C15 0.0240(12) 0.0197(13) 0.0121(10) -0.0027(9) 0.0023(9) 0.0004(10) C13B 0.0248(12) 0.0123(11) 0.0210(11) -0.0004(9) 0.0073(9) 0.0022(9) C13D 0.0309(13) 0.0140(12) 0.0309(14) -0.0005(10) -0.0141(11) -0.0009(10) C2B 0.0273(12) 0.0206(13) 0.0173(11) 0.0053(10) -0.0001(10) -0.0060(10) C11 0.0177(10) 0.0115(11) 0.0171(10) -0.0021(9) 0.0007(8) 0.0000(9) C5B 0.0145(10) 0.0185(12) 0.0236(12) 0.0034(10) 0.0035(9) 0.0026(9) C16B 0.0204(11) 0.0220(13) 0.0154(11) 0.0033(10) 0.0031(9) 0.0023(10) C11D 0.0169(11) 0.0246(14) 0.0264(13) -0.0126(11) -0.0035(9) 0.0057(10) C1D 0.0244(12) 0.0214(13) 0.0233(12) 0.0065(10) 0.0032(10) 0.0058(10) C14D 0.0177(11) 0.0197(13) 0.0231(12) -0.0067(10) -0.0038(9) -0.0014(9) C12D 0.0181(11) 0.0327(15) 0.0343(14) -0.0164(12) -0.0077(10) 0.0105(11) C5D 0.0157(11) 0.0178(12) 0.0256(12) 0.0046(10) -0.0052(9) -0.0029(9) C18B 0.0181(12) 0.0378(17) 0.0378(15) 0.0032(13) -0.0081(11) 0.0000(11) C19B 0.0267(13) 0.0406(18) 0.0341(15) 0.0098(14) -0.0096(11) 0.0064(13) C18 0.0241(14) 0.0402(19) 0.072(2) -0.0243(18) 0.0237(15) -0.0050(13) C18D 0.0211(13) 0.051(2) 0.0440(17) 0.0065(16) 0.0093(12) -0.0048(13) C19D 0.0327(15) 0.056(2) 0.0386(17) 0.0178(16) 0.0025(13) -0.0143(15) C19 0.069(3) 0.0303(19) 0.103(4) 0.011(2) 0.068(3) 0.0144(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O2 C3 1.447(3) . ? O2 C1 1.429(3) . ? O3B C3B 1.417(3) . ? O3B C1B 1.438(3) . ? O1 C3 1.419(3) . ? O1 C2 1.438(3) . ? O4B C3B 1.452(3) . ? O4B C2B 1.430(3) . ? O5 C17 1.440(3) . ? O5 C18 1.417(3) . ? O3 C10 1.201(3) . ? O2B C17B 1.443(3) . ? O2B C18B 1.428(3) . ? O4 H4 0.8200 . ? O4 C9 1.412(3) . ? O1D C3D 1.422(3) . ? O1D C1D 1.430(3) . ? O1B C17B 1.427(3) . ? O1B C19B 1.435(4) . ? O5B C9B 1.407(3) . ? O5B H5B 0.81(4) . ? O2D C3D 1.432(3) . ? O2D C2D 1.429(3) . ? O6 C17 1.426(3) . ? O6 C19 1.396(4) . ? O6D C17D 1.437(3) . ? O6D C18D 1.426(3) . ? O3D C10D 1.210(4) . ? O4D C11D 1.407(3) . ? O4D H4D 0.81(5) . ? O6B C10B 1.208(3) . ? O5D C17D 1.423(3) . ? O5D C19D 1.437(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 C9 1.529(3) . ? C7D H7D 0.9800 . ? C7D C6D 1.559(3) . ? C7D C8D 1.559(3) . ? C7D C14D 1.535(3) . ? C10 C9 1.532(3) . ? C10 C11 1.516(3) . ? C3 C4 1.546(3) . ? C3 C8 1.514(3) . ? C8B C7B 1.553(3) . ? C8B C11B 1.556(3) . ? C8B C3B 1.553(3) . ? C8B C9B 1.610(3) . ? C10B C11B 1.513(3) . ? C10B C9B 1.535(4) . ? C7B H7BA 0.9800 . ? C7B C1AA 1.542(3) . ? C7B C6B 1.560(3) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C3B C4B 1.516(3) . ? C17B C6B 1.547(3) . ? C17B C16B 1.524(3) . ? C9B C12B 1.527(3) . ? C6 C16 1.541(3) . ? C6 C5 1.556(3) . ? C6 C7 1.534(3) . ? C6 C17 1.554(3) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C1AA H1AA 0.9700 . ? C1AA H1AB 0.9700 . ? C1AA C15B 1.528(3) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C15B C16B 1.524(3) . ? C1B H1BA 0.9700 . ? C1B H1BB 0.9700 . ? C1B C2B 1.515(3) . ? C5 H5 0.9800 . ? C5 C4 1.554(3) . ? C5 C13 1.540(3) . ? C6D C17D 1.555(4) . ? C6D C13D 1.538(4) . ? C6D C5D 1.537(3) . ? C4B H4BA 0.9700 . ? C4B H4BB 0.9700 . ? C4B C5B 1.526(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C2 C1 1.520(3) . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C13 1.533(3) . ? C14 C15 1.526(4) . ? C4 C9 1.615(3) . ? C4 C11 1.562(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C8 C7 1.532(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C3D C8D 1.546(3) . ? C3D C4D 1.523(3) . ? C9D H9DA 0.9700 . ? C9D H9DB 0.9700 . ? C9D C10D 1.518(4) . ? C9D C8D 1.563(3) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C10D C11D 1.534(4) . ? C17D C16D 1.520(3) . ? C8D C11D 1.615(3) . ? C2D H2DA 0.9700 . ? C2D H2DB 0.9700 . ? C2D C1D 1.523(3) . ? C6B C13B 1.540(3) . ? C6B C5B 1.540(3) . ? C17 C15 1.525(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C15D H15E 0.9700 . ? C15D H15F 0.9700 . ? C15D C16D 1.521(4) . ? C15D C14D 1.535(4) . ? C4D H4DA 0.9700 . ? C4D H4DB 0.9700 . ? C4D C5D 1.526(4) . ? C16D H16F 0.9700 . ? C16D H16G 0.9700 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C13B H13C 0.9600 . ? C13B H13D 0.9600 . ? C13B H13E 0.9600 . ? C13D H13F 0.9600 . ? C13D H13G 0.9600 . ? C13D H13H 0.9600 . ? C2B H2BA 0.9700 . ? C2B H2BB 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C5B H5BA 0.9700 . ? C5B H5BB 0.9700 . ? C16B H16D 0.9700 . ? C16B H16E 0.9700 . ? C11D C12D 1.520(4) . ? C1D H1DA 0.9700 . ? C1D H1DB 0.9700 . ? C14D H14C 0.9700 . ? C14D H14D 0.9700 . ? C12D H12G 0.9600 . ? C12D H12H 0.9600 . ? C12D H12I 0.9600 . ? C5D H5DA 0.9700 . ? C5D H5DB 0.9700 . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C18B C19B 1.497(5) . ? C19B H19C 0.9700 . ? C19B H19D 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 C19 1.448(6) . ? C18D H18E 0.9700 . ? C18D H18F 0.9700 . ? C18D C19D 1.488(6) . ? C19D H19E 0.9700 . ? C19D H19F 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O2 C3 109.01(17) . . ? C3B O3B C1B 106.23(17) . . ? C3 O1 C2 106.94(17) . . ? C2B O4B C3B 108.96(18) . . ? C18 O5 C17 108.1(2) . . ? C18B O2B C17B 108.8(2) . . ? C9 O4 H4 109.5 . . ? C3D O1D C1D 106.63(19) . . ? C17B O1B C19B 106.3(2) . . ? C9B O5B H5B 108(3) . . ? C2D O2D C3D 109.28(18) . . ? C19 O6 C17 108.3(2) . . ? C18D O6D C17D 108.7(2) . . ? C11D O4D H4D 105(3) . . ? C17D O5D C19D 106.5(2) . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? C6D C7D H7D 104.7 . . ? C6D C7D C8D 113.66(19) . . ? C8D C7D H7D 104.7 . . ? C14D C7D H7D 104.7 . . ? C14D C7D C6D 111.7(2) . . ? C14D C7D C8D 116.01(19) . . ? O3 C10 C9 132.1(2) . . ? O3 C10 C11 135.4(2) . . ? C11 C10 C9 92.43(17) . . ? O2 C3 C4 109.51(17) . . ? O2 C3 C8 108.92(18) . . ? O1 C3 O2 105.82(17) . . ? O1 C3 C4 108.29(18) . . ? O1 C3 C8 110.89(18) . . ? C8 C3 C4 113.15(19) . . ? C7B C8B C11B 116.37(19) . . ? C7B C8B C3B 108.37(17) . . ? C7B C8B C9B 125.10(19) . . ? C11B C8B C9B 88.00(17) . . ? C3B C8B C11B 107.89(18) . . ? C3B C8B C9B 109.01(18) . . ? O6B C10B C11B 134.9(3) . . ? O6B C10B C9B 132.7(2) . . ? C11B C10B C9B 92.37(18) . . ? C8B C7B H7BA 104.8 . . ? C8B C7B C6B 114.10(18) . . ? C1AA C7B C8B 115.88(18) . . ? C1AA C7B H7BA 104.8 . . ? C1AA C7B C6B 111.23(18) . . ? C6B C7B H7BA 104.8 . . ? C8B C11B H11C 113.8 . . ? C8B C11B H11D 113.8 . . ? C10B C11B C8B 88.88(18) . . ? C10B C11B H11C 113.8 . . ? C10B C11B H11D 113.8 . . ? H11C C11B H11D 111.1 . . ? O3B C3B O4B 105.29(18) . . ? O3B C3B C8B 108.86(18) . . ? O3B C3B C4B 111.11(19) . . ? O4B C3B C8B 108.83(18) . . ? O4B C3B C4B 109.37(19) . . ? C4B C3B C8B 113.06(19) . . ? O2B C17B C6B 110.68(19) . . ? O2B C17B C16B 107.4(2) . . ? O1B C17B O2B 106.05(18) . . ? O1B C17B C6B 108.64(19) . . ? O1B C17B C16B 110.66(19) . . ? C16B C17B C6B 113.20(19) . . ? O5B C9B C8B 120.14(19) . . ? O5B C9B C10B 118.5(2) . . ? O5B C9B C12B 105.9(2) . . ? C10B C9B C8B 86.20(18) . . ? C12B C9B C8B 117.50(19) . . ? C12B C9B C10B 107.4(2) . . ? C16 C6 C5 112.94(18) . . ? C16 C6 C17 108.43(18) . . ? C7 C6 C16 108.80(19) . . ? C7 C6 C5 109.59(18) . . ? C7 C6 C17 108.71(18) . . ? C17 C6 C5 108.29(18) . . ? C6 C16 H16A 109.5 . . ? C6 C16 H16B 109.5 . . ? C6 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C7B C1AA H1AA 109.5 . . ? C7B C1AA H1AB 109.5 . . ? H1AA C1AA H1AB 108.1 . . ? C15B C1AA C7B 110.55(18) . . ? C15B C1AA H1AA 109.5 . . ? C15B C1AA H1AB 109.5 . . ? C1AA C15B H15C 109.6 . . ? C1AA C15B H15D 109.6 . . ? H15C C15B H15D 108.1 . . ? C16B C15B C1AA 110.2(2) . . ? C16B C15B H15C 109.6 . . ? C16B C15B H15D 109.6 . . ? O3B C1B H1BA 111.3 . . ? O3B C1B H1BB 111.3 . . ? O3B C1B C2B 102.53(19) . . ? H1BA C1B H1BB 109.2 . . ? C2B C1B H1BA 111.3 . . ? C2B C1B H1BB 111.3 . . ? C6 C5 H5 104.7 . . ? C4 C5 C6 114.08(19) . . ? C4 C5 H5 104.7 . . ? C13 C5 C6 111.83(19) . . ? C13 C5 H5 104.7 . . ? C13 C5 C4 115.43(18) . . ? C17D C6D C7D 107.72(19) . . ? C13D C6D C7D 112.3(2) . . ? C13D C6D C17D 109.3(2) . . ? C5D C6D C7D 110.3(2) . . ? C5D C6D C17D 108.0(2) . . ? C5D C6D C13D 109.1(2) . . ? C3B C4B H4BA 109.5 . . ? C3B C4B H4BB 109.5 . . ? C3B C4B C5B 110.51(19) . . ? H4BA C4B H4BB 108.1 . . ? C5B C4B H4BA 109.5 . . ? C5B C4B H4BB 109.5 . . ? O1 C2 H2A 111.3 . . ? O1 C2 H2B 111.3 . . ? O1 C2 C1 102.18(18) . . ? H2A C2 H2B 109.2 . . ? C1 C2 H2A 111.3 . . ? C1 C2 H2B 111.3 . . ? C9B C12B H12D 109.5 . . ? C9B C12B H12E 109.5 . . ? C9B C12B H12F 109.5 . . ? H12D C12B H12E 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? H14A C14 H14B 108.2 . . ? C13 C14 H14A 109.7 . . ? C13 C14 H14B 109.7 . . ? C15 C14 H14A 109.7 . . ? C15 C14 H14B 109.7 . . ? C15 C14 C13 110.0(2) . . ? C3 C4 C5 108.48(17) . . ? C3 C4 C9 108.83(17) . . ? C3 C4 C11 107.81(18) . . ? C5 C4 C9 125.01(18) . . ? C5 C4 C11 116.88(19) . . ? C11 C4 C9 87.67(16) . . ? C3 C8 H8A 109.6 . . ? C3 C8 H8B 109.6 . . ? C3 C8 C7 110.42(19) . . ? H8A C8 H8B 108.1 . . ? C7 C8 H8A 109.6 . . ? C7 C8 H8B 109.6 . . ? C6 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? C8 C7 C6 112.12(18) . . ? C8 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? O1D C3D O2D 105.94(19) . . ? O1D C3D C8D 108.03(19) . . ? O1D C3D C4D 110.48(19) . . ? O2D C3D C8D 109.56(18) . . ? O2D C3D C4D 109.0(2) . . ? C4D C3D C8D 113.5(2) . . ? H9DA C9D H9DB 111.1 . . ? C10D C9D H9DA 113.9 . . ? C10D C9D H9DB 113.9 . . ? C10D C9D C8D 88.6(2) . . ? C8D C9D H9DA 113.9 . . ? C8D C9D H9DB 113.9 . . ? C5 C13 H13A 109.6 . . ? C5 C13 H13B 109.6 . . ? C14 C13 C5 110.42(19) . . ? C14 C13 H13A 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? O3D C10D C9D 134.1(3) . . ? O3D C10D C11D 133.2(3) . . ? C9D C10D C11D 92.7(2) . . ? O6D C17D C6D 110.5(2) . . ? O6D C17D C16D 107.4(2) . . ? O5D C17D O6D 106.3(2) . . ? O5D C17D C6D 108.9(2) . . ? O5D C17D C16D 111.0(2) . . ? C16D C17D C6D 112.6(2) . . ? C7D C8D C9D 116.2(2) . . ? C7D C8D C11D 125.4(2) . . ? C3D C8D C7D 108.13(18) . . ? C3D C8D C9D 108.0(2) . . ? C3D C8D C11D 108.98(19) . . ? C9D C8D C11D 87.99(18) . . ? O2D C2D H2DA 111.0 . . ? O2D C2D H2DB 111.0 . . ? O2D C2D C1D 103.67(19) . . ? H2DA C2D H2DB 109.0 . . ? C1D C2D H2DA 111.0 . . ? C1D C2D H2DB 111.0 . . ? C17B C6B C7B 107.94(19) . . ? C13B C6B C7B 112.79(19) . . ? C13B C6B C17B 109.0(2) . . ? C5B C6B C7B 109.41(19) . . ? C5B C6B C17B 108.47(18) . . ? C5B C6B C13B 109.1(2) . . ? O5 C17 C6 110.08(19) . . ? O5 C17 C15 107.70(19) . . ? O6 C17 O5 106.20(18) . . ? O6 C17 C6 109.18(19) . . ? O6 C17 C15 110.0(2) . . ? C15 C17 C6 113.44(19) . . ? O2 C1 C2 103.64(19) . . ? O2 C1 H1A 111.0 . . ? O2 C1 H1B 111.0 . . ? C2 C1 H1A 111.0 . . ? C2 C1 H1B 111.0 . . ? H1A C1 H1B 109.0 . . ? H15E C15D H15F 108.1 . . ? C16D C15D H15E 109.5 . . ? C16D C15D H15F 109.5 . . ? C16D C15D C14D 110.7(2) . . ? C14D C15D H15E 109.5 . . ? C14D C15D H15F 109.5 . . ? C3D C4D H4DA 109.5 . . ? C3D C4D H4DB 109.5 . . ? C3D C4D C5D 110.5(2) . . ? H4DA C4D H4DB 108.1 . . ? C5D C4D H4DA 109.5 . . ? C5D C4D H4DB 109.5 . . ? C17D C16D C15D 110.5(2) . . ? C17D C16D H16F 109.6 . . ? C17D C16D H16G 109.6 . . ? C15D C16D H16F 109.6 . . ? C15D C16D H16G 109.6 . . ? H16F C16D H16G 108.1 . . ? O4 C9 C12 106.17(19) . . ? O4 C9 C10 117.75(19) . . ? O4 C9 C4 120.69(18) . . ? C12 C9 C10 107.73(19) . . ? C12 C9 C4 117.16(18) . . ? C10 C9 C4 86.06(17) . . ? C14 C15 C17 111.3(2) . . ? C14 C15 H15A 109.4 . . ? C14 C15 H15B 109.4 . . ? C17 C15 H15A 109.4 . . ? C17 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C6B C13B H13C 109.5 . . ? C6B C13B H13D 109.5 . . ? C6B C13B H13E 109.5 . . ? H13C C13B H13D 109.5 . . ? H13C C13B H13E 109.5 . . ? H13D C13B H13E 109.5 . . ? C6D C13D H13F 109.5 . . ? C6D C13D H13G 109.5 . . ? C6D C13D H13H 109.5 . . ? H13F C13D H13G 109.5 . . ? H13F C13D H13H 109.5 . . ? H13G C13D H13H 109.5 . . ? O4B C2B C1B 103.77(19) . . ? O4B C2B H2BA 111.0 . . ? O4B C2B H2BB 111.0 . . ? C1B C2B H2BA 111.0 . . ? C1B C2B H2BB 111.0 . . ? H2BA C2B H2BB 109.0 . . ? C10 C11 C4 88.49(17) . . ? C10 C11 H11A 113.9 . . ? C10 C11 H11B 113.9 . . ? C4 C11 H11A 113.9 . . ? C4 C11 H11B 113.9 . . ? H11A C11 H11B 111.1 . . ? C4B C5B C6B 112.56(19) . . ? C4B C5B H5BA 109.1 . . ? C4B C5B H5BB 109.1 . . ? C6B C5B H5BA 109.1 . . ? C6B C5B H5BB 109.1 . . ? H5BA C5B H5BB 107.8 . . ? C17B C16B H16D 109.6 . . ? C17B C16B H16E 109.6 . . ? C15B C16B C17B 110.5(2) . . ? C15B C16B H16D 109.6 . . ? C15B C16B H16E 109.6 . . ? H16D C16B H16E 108.1 . . ? O4D C11D C10D 118.9(2) . . ? O4D C11D C8D 119.7(2) . . ? O4D C11D C12D 106.2(2) . . ? C10D C11D C8D 86.20(19) . . ? C12D C11D C10D 107.3(2) . . ? C12D C11D C8D 117.4(2) . . ? O1D C1D C2D 102.52(19) . . ? O1D C1D H1DA 111.3 . . ? O1D C1D H1DB 111.3 . . ? C2D C1D H1DA 111.3 . . ? C2D C1D H1DB 111.3 . . ? H1DA C1D H1DB 109.2 . . ? C7D C14D H14C 109.4 . . ? C7D C14D H14D 109.4 . . ? C15D C14D C7D 111.08(19) . . ? C15D C14D H14C 109.4 . . ? C15D C14D H14D 109.4 . . ? H14C C14D H14D 108.0 . . ? C11D C12D H12G 109.5 . . ? C11D C12D H12H 109.5 . . ? C11D C12D H12I 109.5 . . ? H12G C12D H12H 109.5 . . ? H12G C12D H12I 109.5 . . ? H12H C12D H12I 109.5 . . ? C6D C5D H5DA 109.1 . . ? C6D C5D H5DB 109.1 . . ? C4D C5D C6D 112.6(2) . . ? C4D C5D H5DA 109.1 . . ? C4D C5D H5DB 109.1 . . ? H5DA C5D H5DB 107.8 . . ? O2B C18B H18C 111.0 . . ? O2B C18B H18D 111.0 . . ? O2B C18B C19B 103.9(2) . . ? H18C C18B H18D 109.0 . . ? C19B C18B H18C 111.0 . . ? C19B C18B H18D 111.0 . . ? O1B C19B C18B 103.3(2) . . ? O1B C19B H19C 111.1 . . ? O1B C19B H19D 111.1 . . ? C18B C19B H19C 111.1 . . ? C18B C19B H19D 111.1 . . ? H19C C19B H19D 109.1 . . ? O5 C18 H18A 110.3 . . ? O5 C18 H18B 110.3 . . ? O5 C18 C19 106.9(2) . . ? H18A C18 H18B 108.6 . . ? C19 C18 H18A 110.3 . . ? C19 C18 H18B 110.3 . . ? O6D C18D H18E 110.9 . . ? O6D C18D H18F 110.9 . . ? O6D C18D C19D 104.3(3) . . ? H18E C18D H18F 108.9 . . ? C19D C18D H18E 110.9 . . ? C19D C18D H18F 110.9 . . ? O5D C19D C18D 103.4(2) . . ? O5D C19D H19E 111.1 . . ? O5D C19D H19F 111.1 . . ? C18D C19D H19E 111.1 . . ? C18D C19D H19F 111.1 . . ? H19E C19D H19F 109.0 . . ? O6 C19 C18 106.9(3) . . ? O6 C19 H19A 110.3 . . ? O6 C19 H19B 110.3 . . ? C18 C19 H19A 110.3 . . ? C18 C19 H19B 110.3 . . ? H19A C19 H19B 108.6 . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 -42 1 690.883 103.59 8 0 -42 2 5327.43 282.444 8 0 -41 0 -17.7012 48.6978 8 0 -41 1 2194.91 196.357 8 0 -41 2 5974.25 328.739 8 0 -41 3 190.946 65.5352 8 0 -40 0 3450.34 259.168 8 0 -40 1 14906.1 590.21 8 0 -40 2 4184.84 291.882 8 0 -40 3 1117.12 145.19 8 0 -40 4 90.4358 47.1186 8 0 -39 0 67.8269 44.6106 8 0 -39 1 7309.3 416.825 8 0 -39 2 2852.76 252.006 8 0 -39 3 1995.15 201.154 8 0 -39 4 2217.32 196.517 8 0 -38 0 12456.5 572.875 8 0 -38 -1 10133.5 485.083 8 0 -38 1 9122.04 491.245 8 0 -38 2 1196.18 175.103 8 0 -38 3 5130.05 342.316 8 0 -38 4 1478.27 170.888 8 0 -38 5 543.234 92.4322 8 0 -37 0 45.4817 67.665 8 0 -37 1 14727.2 664.589 8 0 -37 -1 15919.6 652.997 8 0 -37 2 5546.12 381.136 8 0 -37 3 191.632 79.9421 8 0 -37 4 3887.45 290.803 8 0 -37 5 1558.44 162.42 8 0 -36 0 11686.7 588.959 8 0 -36 1 14856.3 678.884 8 0 -36 -1 15696.6 671.173 8 0 -36 2 688.031 148.486 8 0 -36 3 3321.69 294.009 8 0 -36 4 116.43 69.6024 8 0 -36 5 198.04 72.2055 8 0 -35 0 -17.4669 67.8387 8 0 -35 -1 10404.3 548.172 8 0 -35 1 10776.9 572.353 8 0 -35 2 1354.14 207.078 8 0 -35 3 35605.8 1126.49 8 0 -35 4 5951.55 386.762 8 0 -35 5 610.132 113.618 8 0 -35 6 117.066 57.3203 8 0 -34 0 5335.45 401.47 8 0 -34 -1 89689.5 2137.07 8 0 -34 1 87623.5 2154.57 8 0 -34 2 5273.77 394.304 8 0 -34 3 2925.64 291.188 8 0 -34 4 7068.37 437.13 8 0 -34 5 3498.24 279.673 8 0 -34 6 376.301 87.0082 8 0 -33 0 37.5219 75.0596 8 0 -33 -1 383.485 119.791 8 0 -33 1 448.626 130.362 8 0 -33 2 31899.1 1082.27 8 0 -33 3 16882 733.879 8 0 -33 4 6513.48 423.065 8 0 -33 -5 11314.9 480.693 11 0 -33 5 10434.7 519.537 8 0 -33 -6 2733.46 207.284 11 0 -33 6 2511.35 214.694 8 0 -32 0 16677.4 741.325 8 0 -32 -1 702.158 160.756 8 0 -32 1 723.989 158.544 8 0 -32 2 995.281 178.708 8 0 -32 3 391.47 124.065 8 0 -32 4 8639.22 499.97 8 0 -32 -5 512.169 106.55 11 0 -32 5 553.882 128.808 8 0 -32 6 138.548 72.5867 8 0 -32 -6 29.9931 42.4213 11 0 -32 -7 8249.19 353.188 11 0 -31 0 34.2841 65.3247 8 0 -31 -1 15395.1 700.892 8 0 -31 1 15591 709.323 8 0 -31 2 139.638 78.1902 8 0 -31 3 5573.87 406.544 8 0 -31 4 4344.85 351.615 8 0 -31 5 13293.2 610.675 8 0 -31 -5 13662.2 592.81 11 0 -31 -6 29061.8 898.256 11 0 -31 6 28554.8 888.405 8 0 -31 -7 8399.72 385.79 11 0 -30 0 7732.55 478.722 8 0 -30 -1 138677 3008.73 8 0 -30 1 139157 3014.36 8 0 -30 2 23304 882.611 8 0 -30 3 51981.9 1468.04 8 0 -30 -4 20019.1 762.254 11 0 -30 4 19599.9 794.742 8 0 -30 -5 11590.5 561.464 11 0 -30 5 11401.3 565.503 8 0 -30 6 3415.57 275.29 8 0 -30 -6 3528.83 286.657 11 0 -30 -7 12946.1 526.491 11 0 -30 -8 14798.6 478.121 11 0 -29 0 73.5378 66.3268 8 0 -29 1 2876.67 283.299 8 0 -29 -1 2239.63 252.605 8 0 -29 2 47396.7 1369.76 8 0 -29 3 28681.3 997.456 8 0 -29 4 43523.2 1286.15 8 0 -29 -4 41853.1 1240.85 11 0 -29 -5 9179.36 505.566 11 0 -29 5 9011.83 499.879 8 0 -29 -6 5745.99 383.472 11 0 -29 6 6008.52 374.491 8 0 -29 -7 253.624 85.4382 11 0 -29 -8 4461.8 259.928 11 0 -28 0 5944.07 401.385 8 0 -28 1 78962.5 1920.85 8 0 -28 -1 78539.9 1920.09 8 0 -28 2 2591.68 266.295 8 0 -28 3 32173.2 1055.76 8 0 -28 4 233.571 105.236 8 0 -28 -4 138.616 52.0898 11 0 -28 -5 6528.62 435.873 11 0 -28 5 6762.62 430.749 8 0 -28 -6 14906.6 668.142 11 0 -28 6 15542.5 640.147 8 0 -28 -7 5889.25 372.222 11 0 -28 -8 11481.3 469.809 11 0 -27 0 20.7008 63.2934 8 0 -27 -1 29852.2 984.777 8 0 -27 1 30597.1 993.598 8 0 -27 2 1354.28 189.886 8 0 -27 3 12860.8 605.138 8 0 -27 -4 13894.8 645.125 11 0 -27 4 13879.4 642.061 8 0 -27 5 40501.5 1214.17 8 0 -27 -5 40294.4 1245.62 11 0 -27 6 14298.7 612.872 8 0 -27 -6 13719.5 654.071 11 0 -27 -7 2484.21 249.359 11 0 -27 -8 8263.49 410.499 11 0 -26 0 59234.4 1517.45 8 0 -26 1 12900.2 576.721 8 0 -26 -1 11516.9 550.775 8 0 -26 2 53420.8 1423.64 8 0 -26 3 25850.8 906.575 8 0 -26 -3 27852.7 921.584 11 0 -26 -4 11690.6 590.9 11 0 -26 4 12262.1 587.732 8 0 -26 -5 20063.5 828.015 11 0 -26 5 21482.4 807.452 8 0 -26 6 18129.4 705.5 8 0 -26 -6 17260.9 757.029 11 0 -26 -7 7271.81 444.118 11 0 -26 -8 6842.79 385.901 11 0 -25 0 439.984 118.892 8 0 -25 1 15298.8 622.552 8 0 -25 -1 14803.3 620.641 8 0 -25 2 1279.32 174.698 8 0 -25 3 3637.75 298.86 8 0 -25 -3 4277.2 325.794 11 0 -25 -4 29324.5 1008.43 11 0 -25 4 30672.4 995.304 8 0 -25 -5 11652.8 610.141 11 0 -25 5 11837.4 571.268 8 0 -25 -6 1940.63 244.944 11 0 -25 6 2418.83 240.916 8 0 -25 -7 31393.2 1052.91 11 0 -25 -8 1428.09 182.366 11 0 -25 -9 787.991 108.86 11 0 -24 2 388.528 98.6008 8 0 -24 3 33762.7 1018.43 8 0 -24 -3 31843.2 1008.73 11 0 -24 4 26128.8 882.642 8 0 -24 -4 24894.5 906.323 11 0 -24 -5 16493 745.546 11 0 -24 5 16798.2 689.711 8 0 -24 6 4024.44 312.424 8 0 -24 -6 4151.69 361.343 11 0 -24 -7 6874.95 455.035 11 0 -24 -8 10604.5 523.981 11 0 -24 -9 701.236 108.72 11 0 -23 3 3449.75 273.955 8 0 -23 -3 3247.14 275.362 11 0 -23 -4 8354 485.036 11 0 -23 4 9220.85 474.422 8 0 -23 -5 419.933 117.203 11 0 -23 5 664.827 132.415 8 0 -23 -6 15115.2 722.268 11 0 -23 6 15445.6 640.33 8 0 -23 -7 13216.7 658.328 11 0 -23 -8 4789.08 357.38 11 0 -23 -9 1002.53 135.585 11 0 -22 3 5330.9 335.563 8 0 -22 -4 8627.46 487.42 11 0 -22 4 9101.57 464.685 8 0 -22 5 16239.9 653.491 8 0 -22 -5 14806.2 700.689 11 0 -22 6 12484.1 563.876 8 0 -22 -6 12428.5 650.372 11 0 -22 -7 19626.5 829.297 11 0 -22 -8 13292.9 624.3 11 0 -22 -9 851.004 130.128 11 0 -21 -4 17976.7 726.172 11 0 -21 4 18596.9 682.465 8 0 -21 5 13114 574.426 8 0 -21 -5 13376.7 652.097 11 0 -21 6 7503.7 422.245 8 0 -21 -6 6595.25 467.481 11 0 -21 -7 11311.4 616.99 11 0 -21 -8 4197.45 346.355 11 0 -21 -9 7365.31 402.182 11 0 -20 4 7083.95 384.017 8 0 -20 -4 6528.28 407.965 11 0 -20 -5 6249.49 433.473 11 0 -20 5 6875.67 394.116 8 0 -20 6 17248.9 658.641 8 0 -20 -6 15172.6 736.008 11 0 -20 -7 15945.7 750.808 11 0 -20 -8 43.6066 77.3535 11 0 -20 -9 6166.93 377.396 11 0 -19 5 2790.62 244.119 8 0 -19 -5 2529.69 269.32 11 0 -19 -6 11279.3 613.012 11 0 -19 -7 26279 1005.5 11 0 -19 -8 2413.33 193.39 3 0 -19 -8 2408.52 272.804 11 0 -19 -9 3656.55 298.584 11 0 -19 -9 4275.55 229.672 3 0 -18 5 39162.2 1063.25 8 0 -18 -5 36442.8 1166.82 11 0 -18 -6 7251.4 481.429 11 0 -18 -7 391.161 130.499 11 0 -18 -7 130.513 59.8553 3 0 -18 -8 435.089 82.2133 3 0 -18 -8 643.268 157.921 11 0 -18 -9 2453.94 185.01 3 0 -18 -9 2480.42 249.832 11 0 -17 -5 1046.41 170.724 11 0 -17 -6 8296.05 516.754 11 0 -17 -7 11662.1 493.293 3 0 -17 -7 11140 624.067 11 0 -17 -8 2157.45 196.328 3 0 -17 -8 2308.88 274.766 11 0 -17 -9 2550.46 258.606 11 0 -17 -9 2265.59 185.446 3 0 -17 -10 5218.09 225.999 3 0 -16 -5 56844.8 1518 11 0 -16 -6 2381.04 207.141 3 0 -16 -6 2640.49 281.349 11 0 -16 -7 20002.3 685.543 3 0 -16 -7 19082.4 840.425 11 0 -16 -8 7349.02 383.576 3 0 -16 -8 7471.99 497.038 11 0 -16 -9 20798.1 651.798 3 0 -16 -9 20391.4 797.483 11 0 -16 -10 1216.2 124.57 3 0 -15 -6 8387.1 406.539 3 0 -15 -6 8192.07 499.863 11 0 -15 -7 24149.9 781.839 3 0 -15 -7 23883.4 949.85 11 0 -15 -8 83344.4 1861.08 3 0 -15 -8 82509.3 2113.72 11 0 -15 -9 6022.48 325.355 3 0 -15 -9 5829.47 404.088 11 0 -15 -10 1248.86 133.854 3 0 -14 -6 5302.74 318.245 3 0 -14 -6 5493.43 399.576 11 0 -14 -7 9710.56 572.575 11 0 -14 -7 9770.12 460.701 3 0 -14 -8 85718.7 1906.9 3 0 -14 -8 82609.1 2125.59 11 0 -14 -9 9520.15 425.406 3 0 -14 -9 8611.54 503.547 11 0 -14 -10 2172.07 168.13 3 0 -13 -6 17785.4 631.225 3 0 -13 -6 17791.6 753.521 11 0 -13 -7 7331.12 492.841 11 0 -13 -7 8072.71 417.689 3 0 -13 -8 362.065 91.3299 3 0 -13 -8 693.783 165.692 11 0 -13 -9 3846.54 334.481 11 0 -13 -9 3737.68 261.94 3 0 -13 -10 1320.29 140.709 3 0 -12 -6 6806.12 362.928 3 0 -12 -6 7164.74 446.99 11 0 -12 -7 37118.1 1052.7 3 0 -12 -7 36450.6 1210.68 11 0 -12 -8 2401.2 231.227 3 0 -12 -8 2754.74 301.06 11 0 -12 -9 673.778 149.925 11 0 -12 -9 746.352 124.376 3 0 -12 -10 7065.73 327.239 3 0 -11 -6 993.045 166.719 11 0 -11 -6 1566.9 172.607 3 0 -11 -7 10060.8 476.735 3 0 -11 -7 9723.5 558.293 11 0 -11 -8 44480.2 1214.9 3 0 -11 -8 45358.5 1396.95 11 0 -11 -9 7458.8 395.804 3 0 -11 -9 7696.67 480.539 11 0 -11 -10 9454.19 395.479 3 0 -10 -6 31828.1 1031.78 11 0 -10 -6 31920.6 918.198 3 0 -10 -7 1201.72 190.24 11 0 -10 -7 1131.83 157.619 3 0 -10 -8 24602 959.972 11 0 -10 -8 24504.3 827.641 3 0 -10 -9 3679.19 330.059 11 0 -10 -9 3565.26 270.873 3 0 -10 -10 2394.38 197.267 3 0 -9 -7 8909.84 522.675 11 0 -9 -7 8326.05 433.728 3 0 -9 -8 67461.4 1835.21 11 0 -9 -8 70132.8 1678.28 3 0 -9 -9 24626 914.859 11 0 -9 -9 22999.2 780.511 3 0 -9 -10 190.436 81.6204 3 0 -9 -11 8317.08 304.475 3 0 -8 -7 11736.1 603.404 11 0 -8 -7 11650.2 526.437 3 0 -8 -8 58392.4 1636.36 11 0 -8 -8 58180.7 1485.95 3 0 -8 -9 2881.97 291.83 11 0 -8 -9 3153.53 258.7 3 0 -8 -10 302.764 87.3601 3 0 -8 -11 18226.8 506.977 3 0 -7 -7 2189.13 214.838 3 0 -7 -7 2394.5 260.633 11 0 -7 -8 16567.7 750.453 11 0 -7 -8 16816.4 668.368 3 0 -7 -9 8955.77 453.827 3 0 -7 -9 8466.08 499.873 11 0 -7 -10 2303.69 201.789 3 0 -7 -11 18788.3 526.506 3 0 -6 -7 1522.57 209.48 11 0 -6 -7 1770.5 193.245 3 0 -6 -8 2507.93 245.258 3 0 -6 -8 2381.24 269.676 11 0 -6 -9 26340.8 865.723 3 0 -6 -9 27769.5 966.676 11 0 -6 -10 2278.05 204.653 3 0 -6 -11 14218.7 443.658 3 0 -5 -3 25134.7 638.31 2 0 -5 -4 17060.8 546.535 2 0 -5 -5 13914.9 539.021 2 0 -5 -7 33904.5 1081.64 11 0 -5 -7 32198.5 978.618 3 0 -5 -8 29078.2 1014.97 11 0 -5 -8 27279.3 907.636 3 0 -5 -9 20554.1 745.157 3 0 -5 -9 21473.8 820.602 11 0 -5 -10 2317.09 206.177 3 0 -5 -11 3751.94 215.48 3 0 -4 -2 40433.5 837.978 2 0 -4 -3 39789.5 897.936 2 0 -4 -4 29952 796.973 2 0 -4 -5 4982.41 305.444 2 0 -4 -6 1979.28 213.989 2 0 -4 -7 3609.21 311.125 11 0 -4 -7 3599.67 279.998 3 0 -4 -8 3125.56 274.969 3 0 -4 -8 3050.27 296.311 11 0 -4 -9 3023.63 258.01 3 0 -4 -10 1643.82 174.676 3 0 -4 -11 17481.5 514.106 3 0 -3 -3 182199 3303.99 2 0 -3 -4 277990 5009.38 2 0 -3 -5 167927 3277.02 2 0 -3 -6 32821.3 1008.93 2 0 -3 -7 8789.34 446.24 3 0 -3 -7 8623.38 483.471 11 0 -3 -8 7902.71 477.545 11 0 -3 -8 7418.53 425.624 3 0 -3 -9 1324 168.831 3 0 -3 -10 1270.9 158.726 3 0 -3 -11 5374.98 264.202 3 0 -2 -3 48899.6 1059.37 2 0 -2 -4 16796.3 548.54 2 0 -2 -5 11771.1 497.96 2 0 -2 -6 6488.49 396.012 2 0 -2 -7 5292.21 394.561 2 0 -2 -7 4869.62 355.676 11 0 -2 -7 5445.13 343.981 3 0 -2 -8 806.186 135.445 3 0 -2 -8 1004.87 171.145 11 0 -2 -9 1411.83 179.073 3 0 -2 -10 467.535 105.296 3 0 -2 -11 30343 756.089 3 0 -1 -3 12442.7 404.354 2 0 -1 -4 13613.2 483.269 2 0 -1 -5 3399.72 255.557 2 0 -1 -6 21685.8 791.749 2 0 -1 -7 2870.2 244.841 10 0 -1 -7 2372.51 265.273 2 0 -1 -7 2943.28 251.042 3 0 -1 -7 3012.13 270.615 11 0 -1 -8 1800 201.054 10 0 -1 -8 1655.7 189.171 3 0 -1 -8 1639.1 210.843 11 0 -1 -9 10568 505 3 0 -1 -10 7526.82 380.236 3 0 -1 -11 15199.2 473.807 3 0 0 -1 3856.67 120.163 1 0 0 -2 868632 14640.7 1 0 0 -3 16488.3 491.486 2 0 0 -4 347808 6200.81 2 0 0 -5 16572.3 615.081 2 0 0 -6 5926.27 389.049 2 0 0 -7 3848.82 337.967 2 0 0 -7 3294.31 264.272 3 0 0 -7 3669.06 282.302 10 0 0 -8 1248.43 167.864 3 0 0 -8 1554.08 193.24 10 0 0 -9 236.99 78.5318 3 0 0 -10 16814.3 599.272 3 0 0 -11 3387.57 206.347 3 0 1 -1 2486.53 63.7661 12 0 1 -2 518105 8702.37 1 0 1 -2 510988 8588.68 12 0 1 -3 12861 374.339 1 0 1 -3 12278.7 399.631 2 0 1 -4 14112.3 507.88 2 0 1 -5 3554.02 265.539 2 0 1 -6 21136.1 794.365 2 0 1 -7 2747.81 246.599 10 0 1 -7 2723.16 240.215 3 0 1 -7 3113.97 308.322 2 0 1 -8 1530.88 186.707 3 0 1 -8 1667.1 205.136 10 0 1 -9 9958.69 485.178 3 0 1 -10 7585.77 377.791 3 0 2 0 21026.8 380.5 12 0 2 1 9024.86 159.748 12 0 2 -1 7282.98 173.803 12 0 2 -2 68364.7 1288.75 1 0 2 -2 67932 1193.26 12 0 2 -3 48423 878.732 12 0 2 -3 48270.9 1022.39 1 0 2 -3 48121.1 1078.23 2 0 2 -4 17632.9 585.69 2 0 2 -4 17474.4 537.037 1 0 2 -5 10719.4 492.498 2 0 2 -6 6390.32 405.359 2 0 2 -7 5259.77 405.388 2 0 2 -7 4887.38 322.594 3 0 2 -7 4967.61 340.032 10 0 2 -8 1011.96 158.241 10 0 2 -8 712.587 124.008 3 0 2 -9 1546.17 186.399 3 0 2 -10 782.462 130.02 3 0 3 0 43.173 9.8099 12 0 3 1 328733 5528.41 12 0 3 -1 330546 5549.96 12 0 3 -2 132693 2288.48 12 0 3 -3 169723 3154.06 1 0 3 -3 175713 3014.57 12 0 3 -3 180395 3238.26 2 0 3 -4 280705 5090.99 2 0 3 -4 279016 4994.8 1 0 3 -5 173253 3436.52 2 0 3 -6 32152 1047.67 2 0 3 -7 8240.72 452.703 10 0 3 -7 8017.14 419.417 3 0 3 -7 8384.1 520.759 2 0 3 -8 6343.96 392.454 3 0 3 -8 8068.22 454.641 10 0 3 -9 785.609 129.103 3 0 3 -10 1877.78 187.362 3 0 4 0 127820 2192.78 12 0 4 1 7135.39 165.368 12 0 4 -1 7562.99 183.037 12 0 4 -2 34669.8 666.574 12 0 4 2 34735.4 616.636 12 0 4 -3 39911.8 943.259 2 0 4 -3 39033.2 762.982 12 0 4 -3 39632.1 879.831 1 0 4 -4 29686.2 769.365 1 0 4 -4 29420.3 837.36 2 0 4 -5 5410.47 346.29 2 0 4 -6 1943.88 231.246 2 0 4 -7 3248.58 258.416 3 0 4 -7 3443.12 338.529 2 0 4 -7 4052.49 312.264 10 0 4 -8 2917.72 272.935 10 0 4 -8 2819.33 249.514 3 0 4 -9 3144.55 276.812 10 0 4 -9 2893.56 252.225 3 0 4 -10 2039.01 199.199 3 0 5 0 39.6715 15.0246 12 0 5 1 22142.2 445.081 12 0 5 -1 24545.3 471.218 12 0 5 2 298102 5010.44 12 0 5 -2 295177 5061.37 12 0 5 -3 22571.6 499.107 12 0 5 -3 23860 602.302 1 0 5 -3 23566.9 659.97 2 0 5 -4 16182.5 584.514 2 0 5 -4 15397.2 515.864 1 0 5 -5 12657.9 559.135 2 0 5 -5 13781.7 513.359 1 0 5 -6 25963.3 933.588 2 0 5 -7 33264.9 957.376 3 0 5 -7 31886.9 1133.91 2 0 5 -7 31728 1020.95 10 0 5 -8 27537.1 952.345 10 0 5 -8 28382.5 900.623 3 0 5 -9 20703.9 766.396 10 0 5 -9 19214.6 701.021 3 0 5 -10 3065.8 240.082 3 0 6 -1 854441 14385.3 12 0 6 1 857885 14363.2 12 0 6 -2 42278.1 809.611 12 0 6 2 40886.6 762.61 12 0 6 -3 121914 2182.65 12 0 6 -4 47263.9 938.559 12 0 6 -4 46551.6 1167.54 2 0 6 -4 44701.8 1074.78 1 0 6 -5 8417.14 388.059 1 0 6 -5 7852 432.907 2 0 6 -6 23912.2 903.749 2 0 6 -7 1363.93 186.987 10 0 6 -7 1253.53 153.201 3 0 6 -7 1435.36 231.903 2 0 6 -8 2680.95 268.566 10 0 6 -8 2358.08 227.361 3 0 6 -9 28259.6 932.099 10 0 6 -9 26486.9 840.366 3 0 6 -10 2830.21 222.738 3 0 7 0 63.3344 19.9906 12 0 7 1 5190.35 157.885 12 0 7 -1 4716.49 163.358 12 0 7 2 106799 1905.08 12 0 7 -2 111593 1952.63 12 0 7 -3 30703 650.221 12 0 7 3 29362.9 558.856 12 0 7 -4 5709.17 291.387 1 0 7 -4 6555.57 234.846 12 0 7 -4 6165.17 345.571 2 0 7 -5 28256 817.344 1 0 7 -5 27740.2 912.992 2 0 7 -6 19698.9 818.855 2 0 7 -7 1856.99 187.405 3 0 7 -7 2439.3 286.143 2 0 7 -7 1851.49 223.492 10 0 7 -8 15456.8 613.955 3 0 7 -8 15937.2 697.64 10 0 7 -9 8946.87 485.074 10 0 7 -9 8010.81 412.338 3 0 7 -10 3558.46 235.902 3 0 8 0 79850.4 1452.24 12 0 8 -1 207176 3557.79 12 0 8 1 203365 3534.36 12 0 8 2 6215.01 184.569 12 0 8 -2 6242.77 210.927 12 0 8 3 16964.3 362.25 12 0 8 -3 16334.2 428.885 12 0 8 -4 14643.7 410.852 12 0 8 -4 13052.7 474.456 1 0 8 -4 13739.5 553.195 2 0 8 -5 14915.1 634.736 2 0 8 -5 14528.8 546.18 1 0 8 -6 24025.8 919.564 2 0 8 -7 12859.6 691.915 2 0 8 -7 12940.8 525.446 3 0 8 -7 12306.5 596.01 10 0 8 -8 57214.5 1417.56 3 0 8 -8 55970.9 1547.47 10 0 8 -9 3180.24 293.125 10 0 8 -9 3465.64 261.002 3 0 8 -10 1588.83 176.924 3 0 9 0 38.4644 22.1274 12 0 9 1 2943.94 127.313 12 0 9 -1 3110.01 138.947 12 0 9 -2 55971.4 1108.04 12 0 9 2 56424.2 1061.98 12 0 9 3 44395 846.612 12 0 9 -3 44096.3 925.504 12 0 9 -4 18966.1 506.802 12 0 9 -4 19625 687.367 2 0 9 -5 57939.6 1524.96 2 0 9 -5 58893.9 1389.47 1 0 9 -6 15765.7 731.982 2 0 9 -7 8535.43 492.1 10 0 9 -7 9267.75 429.274 3 0 9 -8 69839.6 1621.94 3 0 9 -8 67279.3 1770.8 10 0 9 -9 23259.2 848.258 10 0 9 -9 23383.7 736.982 3 0 10 0 5917.25 206.993 12 0 10 -1 228288 3907.26 12 0 10 1 220041 3886.77 12 0 10 -2 38327.8 813.639 12 0 10 2 37741.5 774.343 12 0 10 3 13140.8 328.945 12 0 10 -3 13144.7 390.559 12 0 10 -4 9778.53 407.276 1 0 10 -4 10316.2 351.072 12 0 10 -5 16607.6 691.488 2 0 10 -5 15316.7 575.776 1 0 10 -6 32379.4 973.619 1 0 10 -6 30646.6 1098.5 2 0 10 -7 1111.61 198.505 2 0 10 -7 1028.75 175.785 10 0 10 -7 1084.93 136.43 3 0 10 -8 23074.6 754.679 3 0 10 -8 24337.4 910.345 10 0 10 -9 3969.47 270.57 3 0 10 -9 3693.96 311.405 10 0 11 0 27.206 19.1948 12 0 11 -1 24011.1 555.174 12 0 11 1 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19 -1 5426.74 298.326 6 -8 19 -2 15661.7 523.818 6 -8 19 -3 1011.73 106.249 6 8 20 -4 6782.31 322.591 9 -8 20 4 6660.72 274.673 6 8 20 -3 4235.55 276.636 9 -8 20 3 4209.7 239.32 6 -8 20 2 11018.8 433.775 6 -8 20 1 240.904 70.9057 6 -8 20 0 2216.86 190.11 6 -8 20 -1 803.631 112.836 6 -8 20 -2 8774.82 363.154 6 -8 20 -3 2913.92 175.672 6 8 21 -4 2507.17 180.34 9 -8 21 4 2418.51 147.372 6 8 21 -3 6492.81 333.514 9 -8 21 3 6279.51 287.294 6 8 21 -2 13874.1 550.068 9 -8 21 2 14234.4 490.238 6 -8 21 1 6837.45 331.097 6 -8 21 0 1856.61 169.793 6 -8 21 -1 3361.09 222.171 6 -8 21 -2 3769.43 221.915 6 8 22 -4 2371.15 164.502 9 8 22 -3 1358.25 144.655 9 -8 22 3 1543.66 130.682 6 8 22 -2 11277.5 472.221 9 -8 22 2 11874.6 425.154 6 -8 22 1 2010.64 168.794 6 -8 22 0 6038.97 302.982 6 -8 22 -1 748.402 106.939 6 -8 22 -2 20632.4 587.035 6 8 23 -3 914.445 113.177 9 -8 23 3 881.013 92.8426 6 8 23 -2 8887.07 388.671 9 -8 23 2 8014.97 330.749 6 -8 23 1 5490.94 275.657 6 -8 23 0 6729.26 311.216 6 -8 23 -1 15155.9 492.083 6 -8 23 -2 2655.83 171.729 6 8 24 -3 2239.61 158.909 9 8 24 -2 1266.57 134.727 9 -8 24 2 1325.39 120.926 6 -8 24 1 3396.34 205.287 6 -8 24 0 3721.42 216.57 6 -8 24 -1 7248.62 305.158 6 -8 24 -2 3018.55 174.871 6 8 25 -2 847.034 101.882 9 -8 25 2 899.957 92.9106 6 -8 25 1 4668.02 232.911 6 -8 25 0 4686.16 235.27 6 -8 25 -1 2309.91 158.48 6 8 26 -1 2648.92 174.953 9 -8 26 1 2532.06 156.954 6 -8 26 0 2912.02 172.323 6 -8 26 -1 1003.86 97.98 6 -9 -18 -1 524.285 85.7098 5 -9 -18 -2 250.755 57.0837 5 -9 -17 0 1460.15 132.075 5 -9 -17 -1 1368.28 136.197 5 -9 -17 -2 301.885 58.569 3 -9 -17 -2 492.953 79.2072 5 -9 -16 0 2777.84 193.249 5 -9 -16 -1 6141.98 306.898 5 -9 -16 -2 102.178 44.4131 3 -9 -16 -2 239.184 64.7205 5 -9 -16 -3 2526.75 166.087 5 -9 -15 0 3251.84 218.482 5 -9 -15 -1 6824.16 334.998 5 -9 -15 -2 219.453 60.4702 5 -9 -15 -3 1773.16 143.841 5 -9 -15 -3 1348.44 111.312 3 -9 -14 0 2363.36 191.214 5 -9 -14 -1 279.927 79.6546 5 -9 -14 -2 1567.38 156.881 5 -9 -14 -3 2481.79 178.971 5 -9 -14 -3 1981.9 145.028 3 -9 -13 2 12157.7 380.313 7 -9 -13 1 696.66 101.647 5 -9 -13 1 707.955 88.7342 7 -9 -13 0 10388.3 440.207 5 -9 -13 0 11667 386.789 7 -9 -13 -1 1027.98 136.246 5 -9 -13 -1 994.702 100.97 7 -9 -13 -2 3601.34 245.427 5 -9 -13 -2 3906.8 190.323 7 -9 -13 -3 2251.21 176.667 5 -9 -13 -3 1812.67 141.37 3 -9 -12 2 91.1245 41.0974 7 -9 -12 1 412.651 88.4666 5 -9 -12 1 402.927 74.4653 7 -9 -12 0 1975.97 188.521 5 -9 -12 0 2095.98 158.589 7 -9 -12 -1 11055.7 479.639 5 -9 -12 -1 12763.1 419.236 7 -9 -12 -2 18586.4 622.955 5 -9 -12 -2 18323.5 516.211 7 -9 -12 -3 8984.52 372.738 5 -9 -12 -3 7452.24 315.731 3 -9 -12 -4 2414.28 145.118 3 -9 -11 1 5532.53 291.463 5 -9 -11 1 5622.12 273.183 7 -9 -11 0 941.581 135.287 5 -9 -11 0 1178.21 124.526 7 -9 -11 -1 4454.56 294.358 5 -9 -11 -1 4486.57 242.757 7 -9 -11 -2 4556.58 289.929 5 -9 -11 -2 4389.12 228.976 7 -9 -11 -3 1479.42 152.568 5 -9 -11 -3 1414.25 114.305 7 -9 -11 -3 1172.27 121.948 3 -9 -11 -4 2251.51 156.819 5 -9 -11 -4 2049.48 136.774 3 -9 -10 1 609.645 105.195 5 -9 -10 1 525.783 89.7335 7 -9 -10 0 4833.79 304.843 5 -9 -10 0 5472.95 279.254 7 -9 -10 -1 6213.58 356.478 5 -9 -10 -1 6723.52 310.779 7 -9 -10 -2 8634.52 414.424 5 -9 -10 -2 9157.84 357.963 7 -9 -10 -3 1334.1 148.063 5 -9 -10 -3 1189.07 111.257 7 -9 -10 -3 1140.07 121.664 3 -9 -10 -4 2343.52 169.799 5 -9 -10 -4 2152.75 143.525 3 -9 -9 1 523.768 108.254 5 -9 -9 1 607.26 96.4865 7 -9 -9 0 3203.35 251.204 5 -9 -9 0 3274.32 220.394 7 -9 -9 -1 4753.81 317.137 5 -9 -9 -1 4603.94 262.277 7 -9 -9 -2 19562.7 678.518 5 -9 -9 -2 20617 605.277 7 -9 -9 -3 7720.49 363.732 5 -9 -9 -3 8226.84 319.863 7 -9 -9 -3 7031.87 322.78 3 -9 -9 -4 14929.1 447.873 3 -9 -8 0 586.98 125.47 5 -9 -8 0 543.915 97.9589 7 -9 -8 -1 2508.47 230.045 5 -9 -8 -1 2684.22 203.589 7 -9 -8 -2 5351.76 336.969 5 -9 -8 -2 4605 260.874 7 -9 -8 -3 2397.91 214.967 5 -9 -8 -3 1938.58 155.055 7 -9 -8 -4 24303.7 629.804 3 -9 -7 2 472.688 80.6624 6 -9 -7 0 2909.95 247.501 5 -9 -7 0 2610.08 204.918 7 -9 -7 -1 2103.54 223.392 5 -9 -7 -1 1716.88 164.509 7 -9 -7 -2 8277.01 414.225 5 -9 -7 -2 8571.5 372.036 7 -9 -7 -3 1641.63 168.263 5 -9 -7 -3 1028.99 118.298 7 -9 -7 -4 12585.2 408.412 3 -9 -6 2 1680.2 147.875 6 -9 -6 0 3257.31 263.121 5 -9 -6 0 3336.06 235.651 7 -9 -6 -1 4919.57 325.769 5 -9 -6 -1 4560.81 276.479 7 -9 -6 -2 2156.32 268.254 5 -9 -6 -2 743.944 113.654 7 -9 -6 -3 6586.25 344.671 5 -9 -6 -3 5707.28 286.923 7 -9 -6 -4 1065.7 108.572 3 -9 -5 2 5643.8 282.286 6 -9 -5 0 1131.73 183.142 5 -9 -5 0 1019.95 135.249 7 -9 -5 -1 4677.9 319.844 5 -9 -5 -1 4092.69 265.288 7 -9 -5 -2 14454 572.9 5 -9 -5 -2 14168.5 514.857 7 -9 -5 -3 10115 440.423 5 -9 -5 -3 10086.5 398.465 7 -9 -5 -4 9161.04 334.123 7 -9 -5 -4 7424.91 303.011 3 -9 -4 2 5146.84 273.072 6 -9 -4 0 2246.86 227.735 5 -9 -4 0 1718.57 171.883 7 -9 -4 -1 6680.66 388.622 5 -9 -4 -1 2872.43 227.581 7 -9 -4 -2 6908.06 381.513 5 -9 -4 -2 6127.01 322.941 7 -9 -4 -3 4174.33 275.545 5 -9 -4 -3 4075.77 243.74 7 -9 -4 -4 5120.49 245.757 7 -9 -4 -4 4109.3 215.484 3 -9 -3 5 6233.24 268.069 6 -9 -3 2 14745.8 506.9 6 -9 -3 0 1912.21 182.946 7 -9 -3 -1 16450.7 642.084 5 -9 -3 -1 17517.7 602.066 7 -9 -3 -2 6916.74 385.494 5 -9 -3 -2 7064.08 349.637 7 -9 -3 -3 5061.1 275.505 7 -9 -3 -4 13897.9 442.597 7 -9 -3 -4 11914.3 398.261 3 -9 -2 5 962.877 105.461 6 -9 -2 3 4570.04 264.474 6 -9 -2 2 3362.83 223.615 6 -9 -2 1 15691.4 518.71 6 -9 -2 0 932.785 127.151 7 -9 -2 -1 283.093 83.1486 7 -9 -2 -2 917.787 125.421 7 -9 -2 -3 10274.5 406.864 7 -9 -2 -3 8974.61 370.718 3 -9 -2 -4 13089.4 431.938 7 -9 -2 -4 11807.6 387.719 3 -9 -1 5 3893.7 209.718 6 -9 -1 4 10659.2 406.137 6 -9 -1 3 402.306 86.5449 6 -9 -1 2 5305.61 287.293 6 -9 -1 1 846.323 115.477 6 -9 -1 0 1569.83 168.016 7 -9 -1 -1 2034.4 189.483 7 -9 -1 -2 6387.16 336.14 7 -9 -1 -3 7021.37 330.838 7 -9 -1 -3 6389.19 299.015 3 -9 -1 -4 679.249 81.5964 3 -9 -1 -4 746.811 97.7639 7 -9 0 5 3401.05 195.211 6 -9 0 4 1865.85 163.395 6 -9 0 3 5641.4 295.452 6 -9 0 2 38.0155 46.5794 6 -9 0 1 361.33 78.5152 6 -9 0 0 1624.93 169.253 7 -9 0 -1 19074.8 639.857 7 -9 0 -2 1297.7 150.093 7 -9 0 -3 7272.76 338.272 7 -9 0 -3 6932.2 306.139 3 -9 0 -4 225.92 50.1318 3 -9 0 -4 253.363 62.4451 7 -9 1 5 3890.28 209.981 6 -9 1 4 11094.8 417.359 6 -9 1 3 388.989 82.9153 6 -9 1 2 5468.74 296.31 6 -9 1 1 623.333 100.717 6 -9 1 0 1596.9 168.345 7 -9 1 -1 1996.84 189.558 7 -9 1 -2 6072.15 325.559 7 -9 1 -3 6656.96 321.232 7 -9 1 -3 6276.06 280.667 3 -9 1 -4 809.735 100.976 7 -9 2 5 949.866 105.401 6 -9 2 4 3286.9 214.264 6 -9 2 3 4721.8 271.164 6 -9 2 2 3817.55 247.581 6 -9 2 1 15875.1 539.716 6 -9 2 0 909.254 131.591 7 -9 2 -1 169.472 77.4205 7 -9 2 -2 881.104 127.116 7 -9 2 -3 9417.39 388.98 7 -9 2 -3 9250.02 339.268 3 -9 2 -4 13432.3 442.789 7 -9 3 5 6858.12 284.374 6 -9 3 4 1104.17 124.97 6 -9 3 3 22992.9 685.2 6 -9 3 2 15345.4 535.511 6 -9 3 1 3286.75 226.682 6 -9 3 0 1877.6 179.952 7 -9 3 0 2022.9 166.304 6 -9 3 -1 16780.2 586.795 7 -9 3 -2 6468.76 330.755 7 -9 3 -3 4198.95 247.579 7 -9 3 -4 13258.4 436.2 7 -9 4 5 4695.71 227.775 6 -9 4 4 3962.84 233.386 6 -9 4 3 7510.95 349.75 6 -9 4 2 5403.2 296.842 6 -9 4 1 7874.77 361.406 6 -9 4 0 1887.62 178.574 7 -9 4 0 1685.48 151.638 6 -9 4 -1 2639.89 211.162 7 -9 4 -2 6025.59 315.944 7 -9 4 -3 3733.69 230.095 7 -9 4 -4 5015.19 243.308 7 -9 5 5 5425.74 243.651 6 -9 5 4 1127.32 126.603 6 -9 5 3 7902.48 356.302 6 -9 5 2 5850.44 308.154 6 -9 5 1 411.268 84.8816 6 -9 5 0 1056.16 134.207 7 -9 5 0 935.621 117.382 6 -9 5 -1 3916.43 254.654 7 -9 5 -2 12798.5 475.635 7 -9 5 -3 8863.06 365.44 7 -9 6 5 2193.73 148.472 6 -9 6 4 5938.56 286.298 6 -9 6 3 356.247 82.5409 6 9 6 -3 370.684 82.921 9 -9 6 2 2031.53 178.097 6 -9 6 1 1286.94 140.502 6 -9 6 0 3033.08 218.937 7 -9 6 0 2973.49 204.693 6 -9 6 -1 4039.85 254.329 7 -9 6 -2 626.465 99.7821 7 -9 6 -3 4933.27 256.723 7 -9 7 5 7275.35 278.078 6 -9 7 4 24629 675.353 6 9 7 -3 4223.7 245.046 9 -9 7 3 4508.87 258.728 6 -9 7 2 471.751 89.3648 6 9 7 -2 338.249 76.3937 9 -9 7 1 10785.1 428.562 6 -9 7 0 2448.62 192.4 7 -9 7 0 2618.65 191.093 6 -9 7 -1 1424.16 149.559 7 -9 7 -2 7596.84 341.169 7 -9 7 -3 914.82 107.723 7 -9 8 5 1543.19 117.557 6 -9 8 4 28580.8 741.471 6 9 8 -3 5490.37 284.691 9 -9 8 3 5744.61 292.206 6 9 8 -2 2952.33 214.311 9 -9 8 2 3102.67 215.491 6 9 8 -1 10038.9 418.137 9 -9 8 1 9001.5 377.539 7 -9 8 1 9310.22 392.278 6 -9 8 0 447.388 82.8667 6 -9 8 0 438.819 82.2341 7 -9 8 -1 2450.68 187.324 7 -9 8 -2 3988.57 233.678 7 -9 8 -3 1607.37 136.224 7 -9 9 4 1352.33 132.744 6 9 9 -3 4958.15 272.367 9 -9 9 3 5405.14 278.474 6 9 9 -2 6623.5 332.166 9 -9 9 2 6642.15 323.168 6 -9 9 1 658.677 103.166 6 9 9 -1 651.389 106.566 9 -9 9 1 656.073 94.8942 7 -9 9 0 3489.45 219.698 7 -9 9 0 3621.09 223.317 6 -9 9 -1 4473.79 248.914 7 -9 9 -2 18236.5 547.78 7 -9 9 -3 7417.02 294.296 7 -9 10 4 12268.7 412.331 6 9 10 -3 1357.94 140.208 9 -9 10 3 1395.88 138.999 6 9 10 -2 4879.67 282.435 9 -9 10 2 5254.69 279.112 6 -9 10 1 528.996 91.8741 6 9 10 -1 542.217 105.777 9 -9 10 1 445.979 77.2497 7 -9 10 0 4869.34 255.639 7 -9 10 0 5288.57 272.419 6 -9 10 -1 6234.81 290.18 7 -9 10 -1 6444.86 284.747 6 -9 10 -2 8777.81 337.509 7 -9 10 -3 1070.1 101.331 7 -9 11 4 2365.61 161.095 6 9 11 -3 7486.55 340.119 9 -9 11 3 8044.09 336.714 6 9 11 -2 2786.49 209.314 9 -9 11 2 2769.72 171.547 7 -9 11 2 2840.05 199.472 6 9 11 -1 5626.63 308.932 9 -9 11 1 5338.01 255.214 7 -9 11 1 5606.27 286.356 6 -9 11 0 1002.66 109.103 7 -9 11 0 1182.04 127.472 6 -9 11 -1 4845.89 241.66 7 -9 11 -1 4851.41 242.583 6 -9 11 -2 4020.54 207.154 7 9 12 -4 4201.21 220.827 9 -9 12 4 4371.17 215.398 6 -9 12 3 261.232 60.4324 6 9 12 -3 258.396 68.1628 9 -9 12 2 90.6682 49.3636 6 9 12 -2 85.0144 50.6951 9 -9 12 2 107.94 45.9182 7 -9 12 1 454.775 85.4395 6 9 12 -1 323.375 81.7575 9 -9 12 1 388.938 71.1034 7 -9 12 0 2159.47 152.73 7 -9 12 0 1770.59 153.87 6 -9 12 -1 12100.8 391.5 7 -9 12 -1 11911.9 404.437 6 -9 12 -2 18222.4 492.161 7 -9 13 4 882.675 91.0887 6 9 13 -3 2088.86 167.686 9 -9 13 3 2228.59 160.713 6 9 13 -2 12393.3 470.837 9 -9 13 2 12993.2 448.274 6 -9 13 1 697.75 96.5528 6 9 13 -1 729.829 110.046 9 -9 13 0 11671.7 418.445 6 -9 13 -1 1207.07 117.155 6 -9 14 4 5620.52 229.202 6 9 14 -3 2114.71 166.608 9 -9 14 3 2096.28 153.92 6 9 14 -2 651.668 102.521 9 -9 14 2 736.199 97.9327 6 9 14 -1 4091.42 258.017 9 -9 14 1 4755.91 250.104 6 -9 14 0 2906.28 189.24 6 -9 14 -1 348.539 66.8976 6 -9 15 3 559.185 78.6939 6 9 15 -3 311.399 66.4989 9 9 15 -2 5180.18 276.427 9 -9 15 2 4923.58 246.552 6 9 15 -1 3288.61 225.669 9 -9 15 1 3303 202.385 6 -9 15 0 4137.01 222.58 6 -9 15 -1 6972.2 280.037 6 9 16 -3 1837.02 146.211 9 -9 16 3 1907.93 135.269 6 9 16 -2 1561.98 147.445 9 -9 16 2 1923.88 146.197 6 9 16 -1 2027.42 174.502 9 -9 16 1 1965.75 152.389 6 -9 16 0 3272.69 191.364 6 -9 16 -1 5754.84 244.744 6 -9 17 3 11983.6 367.06 6 9 17 -2 5349.26 267.075 9 -9 17 2 5436.6 244.5 6 9 17 -1 5859.88 293.144 9 -9 17 1 5861 262.496 6 -9 17 0 1243.33 113.249 6 -9 17 -1 1664.1 122.126 6 9 18 -2 1023.4 111.012 9 -9 18 2 1075.41 100.505 6 9 18 -1 5456.69 270.962 9 -9 18 1 5258.94 239.036 6 -9 18 0 265.312 53.9306 6 -9 19 2 1372.98 108.471 6 9 19 -1 5910.09 272.199 9 -9 19 1 5828.63 243.733 6 -9 19 0 714.629 81.134 6 -10 -6 0 3767.46 182.142 7 -10 -5 1 1945.74 128.78 7 -10 -5 0 4428.36 203.896 7 -10 -5 -1 1388.17 106.17 7 -10 -4 1 121.781 39.5388 7 -10 -4 0 305.06 57.1424 7 -10 -4 -1 3105.92 165.597 7 -10 -3 2 189.289 45.3878 7 -10 -3 1 1438.9 115.705 7 -10 -3 0 849.458 91.6012 7 -10 -3 -1 2400.63 147.87 7 -10 -2 2 4338.28 197.103 7 -10 -2 1 448.448 67.5927 7 -10 -2 0 1072.64 102.025 7 -10 -2 -1 125.537 40.4718 7 -10 -1 2 3120.7 166.857 7 -10 -1 1 445.336 67.7356 7 -10 -1 0 6468.59 267.139 7 -10 -1 -1 2594.35 156.446 7 -10 0 2 9334.59 311.727 7 -10 0 1 825.302 89.1664 7 -10 0 0 3490.2 188.336 7 -10 0 -1 81.4874 33.7346 7 -10 1 2 3226.11 166.859 7 -10 1 1 373.033 62.8197 7 -10 1 0 6661.55 267.722 7 -10 1 -1 2680.69 157.987 7 -10 2 2 4270.28 193.787 7 -10 2 1 507.296 70.3595 7 -10 2 0 1162.84 105.684 7 -10 2 -1 96.7914 35.7889 7 -10 3 1 1293.34 108.027 7 -10 3 0 757.089 83.7494 7 -10 3 -1 2220.33 138.662 7 -10 4 1 116.465 36.8797 7 -10 4 0 186.69 44.0142 7 -10 4 -1 3025.97 160.08 7 -10 5 1 1922.37 124.011 7 -10 5 0 4146.13 190.452 7 _iucr_refine_instructions_details ; TITL me_a.res in P2(1) me.res created by SHELXL-2018/3 at 12:19:33 on 27-Jun-2019 REM Old TITL ME in P2(1) REM SHELXT solution in P2(1): R1 0.087, Rweak 0.042, Alpha 0.004 REM 0.892 for 9 systematic absences, Orientation as input REM Flack x = 0.121 ( 0.062 ) from 2246 Parsons' quotients REM Formula found by SHELXT: C55 N2 O18 CELL 1.54184 8.171059 34.870304 9.23924 90 91.1734 90 ZERR 6 0.000128 0.000643 0.000153 0 0.0015 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O UNIT 114 168 36 L.S. 20 PLAN 20 SIZE 0.11 0.12 0.14 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.053000 0.670000 FVAR 6.00824 O2 3 0.289032 0.526386 0.557437 11.00000 0.01669 0.02087 = 0.01189 -0.00310 -0.00027 -0.00357 O3B 3 -0.401791 0.606733 0.860061 11.00000 0.02268 0.01469 = 0.01495 0.00149 0.00034 -0.00848 O1 3 0.440992 0.547175 0.367738 11.00000 0.01516 0.01773 = 0.01555 -0.00123 0.00022 -0.00641 O4B 3 -0.285979 0.636872 1.055838 11.00000 0.02321 0.01991 = 0.01157 0.00134 0.00031 -0.00665 O5 3 0.477881 0.494657 -0.048956 11.00000 0.02006 0.01942 = 0.02138 -0.00083 0.00816 -0.00204 O3 3 -0.069655 0.562047 0.561114 11.00000 0.02104 0.02399 = 0.01966 -0.00696 0.00375 0.00120 O2B 3 -0.485977 0.653625 0.437761 11.00000 0.01777 0.02242 = 0.02154 0.00295 -0.00398 -0.00025 O4 3 0.033947 0.478351 0.503038 11.00000 0.01892 0.01646 = 0.01421 0.00363 -0.00018 -0.00269 AFIX 147 H4 2 0.090898 0.485927 0.571327 11.00000 -1.50000 AFIX 0 O1D 3 0.790800 0.392501 -0.344805 11.00000 0.02200 0.01579 = 0.01984 0.00237 0.00358 0.00708 O1B 3 -0.509797 0.719069 0.448919 11.00000 0.02268 0.02224 = 0.02523 0.00649 0.00004 0.00711 O5B 3 -0.102750 0.699834 1.014093 11.00000 0.02467 0.01945 = 0.02136 -0.00809 0.00676 -0.00807 O2D 3 0.897554 0.360127 -0.535162 11.00000 0.02186 0.02202 = 0.01965 -0.00214 0.00198 0.00597 O6 3 0.410287 0.430920 -0.040734 11.00000 0.02635 0.01572 = 0.02103 -0.00474 0.00422 0.00421 O6D 3 0.700826 0.351132 0.074426 11.00000 0.01777 0.02392 = 0.02724 0.00410 0.00403 -0.00017 O3D 3 1.298416 0.365686 -0.543451 11.00000 0.02677 0.05305 = 0.02991 -0.00883 0.00961 -0.00106 O4D 3 1.069632 0.295281 -0.481742 11.00000 0.02597 0.02451 = 0.03122 -0.01604 -0.00909 0.00989 O6B 3 0.110517 0.626845 1.074671 11.00000 0.02666 0.03474 = 0.01997 0.00382 -0.00707 -0.00344 O5D 3 0.656387 0.286328 0.069669 11.00000 0.03236 0.02921 = 0.03094 0.01023 -0.00634 -0.01617 C12 1 -0.140400 0.498625 0.312212 11.00000 0.01177 0.01923 = 0.01810 -0.00098 0.00055 -0.00094 AFIX 137 H12A 2 -0.123400 0.475555 0.257847 11.00000 -1.50000 H12B 2 -0.165149 0.519354 0.246980 11.00000 -1.50000 H12C 2 -0.230014 0.495003 0.376397 11.00000 -1.50000 AFIX 0 C7D 1 0.966567 0.344216 -0.133429 11.00000 0.01541 0.01143 = 0.02029 -0.00227 -0.00237 0.00111 AFIX 13 H7D 2 0.912037 0.368207 -0.107445 11.00000 -1.20000 AFIX 0 C10 1 -0.002584 0.549155 0.457443 11.00000 0.01383 0.01562 = 0.01784 -0.00219 -0.00305 0.00043 C3 1 0.326067 0.518749 0.407690 11.00000 0.01330 0.01532 = 0.01095 -0.00017 0.00076 -0.00300 C8B 1 -0.168731 0.647651 0.818003 11.00000 0.01410 0.00971 = 0.01667 -0.00173 0.00070 -0.00093 C10B 1 0.026354 0.635061 0.970234 11.00000 0.01650 0.02356 = 0.01649 -0.00106 0.00044 -0.00177 C7B 1 -0.216118 0.655240 0.656878 11.00000 0.01367 0.01163 = 0.01571 -0.00070 0.00165 0.00143 AFIX 13 H7BA 2 -0.274703 0.632078 0.625389 11.00000 -1.20000 AFIX 0 C11B 1 -0.055429 0.612591 0.848701 11.00000 0.01967 0.01597 = 0.01400 -0.00077 -0.00213 0.00038 AFIX 23 H11C 2 -0.113205 0.589943 0.880917 11.00000 -1.20000 H11D 2 0.016784 0.606497 0.769906 11.00000 -1.20000 AFIX 0 C3B 1 -0.328390 0.641823 0.903644 11.00000 0.01757 0.01539 = 0.01200 0.00006 -0.00032 -0.00296 C17B 1 -0.397232 0.688300 0.472576 11.00000 0.01717 0.01392 = 0.02031 0.00375 0.00259 0.00238 C9B 1 -0.043141 0.673231 0.913605 11.00000 0.01688 0.01807 = 0.01518 -0.00408 0.00148 -0.00372 C6 1 0.289739 0.472937 0.137849 11.00000 0.01642 0.01184 = 0.01210 -0.00077 0.00068 -0.00047 C16 1 0.171528 0.439867 0.171753 11.00000 0.01849 0.01360 = 0.01820 0.00004 0.00164 -0.00190 AFIX 137 H16A 2 0.137017 0.441955 0.270138 11.00000 -1.50000 H16B 2 0.226209 0.415792 0.158527 11.00000 -1.50000 H16C 2 0.077694 0.441248 0.107721 11.00000 -1.50000 AFIX 0 C1AA 1 -0.072336 0.658833 0.552284 11.00000 0.01755 0.01596 = 0.01373 -0.00118 0.00167 0.00213 AFIX 23 H1AA 2 -0.013968 0.682589 0.571237 11.00000 -1.20000 H1AB 2 0.003308 0.637743 0.568253 11.00000 -1.20000 AFIX 0 C15B 1 -0.134656 0.658320 0.395203 11.00000 0.01884 0.02161 = 0.01462 -0.00001 0.00173 0.00261 AFIX 23 H15C 2 -0.043091 0.660908 0.330739 11.00000 -1.20000 H15D 2 -0.188147 0.634032 0.374689 11.00000 -1.20000 AFIX 0 C1B 1 -0.479427 0.591534 0.985998 11.00000 0.02531 0.01981 = 0.01923 0.00393 0.00209 -0.00897 AFIX 23 H1BA 2 -0.492188 0.563931 0.979281 11.00000 -1.20000 H1BB 2 -0.585800 0.603179 0.999695 11.00000 -1.20000 AFIX 0 C5 1 0.209993 0.513184 0.154305 11.00000 0.01293 0.01200 = 0.01416 -0.00096 0.00107 -0.00098 AFIX 13 H5 2 0.295603 0.531312 0.126871 11.00000 -1.20000 AFIX 0 C6D 1 0.834552 0.312565 -0.111978 11.00000 0.01953 0.01234 = 0.02371 0.00051 -0.00740 -0.00158 C4B 1 -0.447587 0.674920 0.886522 11.00000 0.01931 0.01785 = 0.01754 0.00031 0.00648 -0.00050 AFIX 23 H4BA 2 -0.398421 0.698090 0.925952 11.00000 -1.20000 H4BB 2 -0.545745 0.669505 0.940169 11.00000 -1.20000 AFIX 0 C2 1 0.525803 0.558960 0.498260 11.00000 0.01781 0.02229 = 0.01803 -0.00525 -0.00265 -0.00553 AFIX 23 H2A 2 0.567982 0.584847 0.489750 11.00000 -1.20000 H2B 2 0.615303 0.541686 0.522454 11.00000 -1.20000 AFIX 0 C12B 1 0.093819 0.693713 0.834485 11.00000 0.01562 0.02288 = 0.02089 -0.00392 0.00152 -0.00600 AFIX 137 H12D 2 0.049498 0.715342 0.782728 11.00000 -1.50000 H12E 2 0.142906 0.676327 0.767499 11.00000 -1.50000 H12F 2 0.175183 0.702349 0.903473 11.00000 -1.50000 AFIX 0 C14 1 0.134735 0.515869 -0.111818 11.00000 0.02396 0.01918 = 0.01500 0.00011 -0.00045 0.00310 AFIX 23 H14A 2 0.045547 0.519596 -0.181296 11.00000 -1.20000 H14B 2 0.216523 0.535456 -0.128426 11.00000 -1.20000 AFIX 0 C4 1 0.169635 0.523977 0.312764 11.00000 0.01357 0.01127 = 0.01378 -0.00008 -0.00021 -0.00073 C8 1 0.399420 0.478999 0.396555 11.00000 0.01271 0.01717 = 0.01554 0.00106 -0.00208 0.00063 AFIX 23 H8A 2 0.322363 0.460206 0.431890 11.00000 -1.20000 H8B 2 0.498161 0.477543 0.456391 11.00000 -1.20000 AFIX 0 C7 1 0.440343 0.469876 0.239144 11.00000 0.01362 0.01472 = 0.01928 -0.00085 0.00124 0.00253 AFIX 23 H7A 2 0.484536 0.444107 0.233881 11.00000 -1.20000 H7B 2 0.523822 0.487516 0.206869 11.00000 -1.20000 AFIX 0 C3D 1 0.857464 0.356517 -0.385599 11.00000 0.01512 0.01404 = 0.02097 -0.00109 0.00121 0.00330 C9D 1 1.136191 0.383474 -0.325014 11.00000 0.01917 0.02051 = 0.02443 -0.00512 0.00251 -0.00313 AFIX 23 H9DA 2 1.083011 0.406451 -0.361907 11.00000 -1.20000 H9DB 2 1.209900 0.389409 -0.244478 11.00000 -1.20000 AFIX 0 C13 1 0.070531 0.519653 0.042269 11.00000 0.01771 0.01778 = 0.01455 -0.00026 0.00039 0.00214 AFIX 23 H13A 2 -0.015400 0.500947 0.057001 11.00000 -1.20000 H13B 2 0.024309 0.545012 0.055260 11.00000 -1.20000 AFIX 0 C10D 1 1.212696 0.358934 -0.441293 11.00000 0.01791 0.03412 = 0.02470 -0.00834 -0.00065 0.00255 C17D 1 0.777866 0.314854 0.047419 11.00000 0.02089 0.01655 = 0.02774 0.00645 -0.00569 -0.00549 C8D 1 1.015556 0.349789 -0.294278 11.00000 0.01331 0.01382 = 0.02311 -0.00676 -0.00174 0.00181 C2D 1 0.833481 0.395495 -0.590271 11.00000 0.02944 0.01951 = 0.02146 0.00446 0.00466 0.00336 AFIX 23 H2DA 2 0.774681 0.391578 -0.681340 11.00000 -1.20000 H2DB 2 0.920316 0.413992 -0.604622 11.00000 -1.20000 AFIX 0 C6B 1 -0.341872 0.688453 0.633750 11.00000 0.01577 0.01147 = 0.01990 0.00163 0.00447 0.00201 C17 1 0.345836 0.468524 -0.021014 11.00000 0.01991 0.01031 = 0.01936 -0.00180 0.00368 0.00026 C1 1 0.391656 0.556777 0.609525 11.00000 0.02183 0.02233 = 0.01801 -0.00691 -0.00010 -0.00430 AFIX 23 H1A 2 0.436785 0.550903 0.704886 11.00000 -1.20000 H1B 2 0.331558 0.580722 0.614069 11.00000 -1.20000 AFIX 0 C15D 1 1.046577 0.341669 0.132455 11.00000 0.02069 0.02144 = 0.02535 -0.00243 -0.00678 -0.00301 AFIX 23 H15E 2 1.137765 0.338000 0.199906 11.00000 -1.20000 H15F 2 0.999012 0.366633 0.150998 11.00000 -1.20000 AFIX 0 C4D 1 0.730814 0.324841 -0.369734 11.00000 0.01718 0.01851 = 0.02447 0.00131 -0.00628 -0.00032 AFIX 23 H4DA 2 0.774771 0.300892 -0.405572 11.00000 -1.20000 H4DB 2 0.633733 0.331076 -0.427170 11.00000 -1.20000 AFIX 0 C16D 1 0.918894 0.310669 0.156155 11.00000 0.02799 0.01977 = 0.02372 0.00355 -0.00836 -0.00553 AFIX 23 H16F 2 0.968795 0.285609 0.145642 11.00000 -1.20000 H16G 2 0.877818 0.312634 0.253636 11.00000 -1.20000 AFIX 0 C9 1 0.014655 0.508122 0.400456 11.00000 0.01332 0.01353 = 0.01292 0.00088 0.00073 0.00002 C15 1 0.210001 0.476272 -0.132862 11.00000 0.02405 0.01970 = 0.01215 -0.00273 0.00234 0.00039 AFIX 23 H15A 2 0.254246 0.474559 -0.229272 11.00000 -1.20000 H15B 2 0.125592 0.456883 -0.124535 11.00000 -1.20000 AFIX 0 C13B 1 -0.269868 0.728086 0.671856 11.00000 0.02477 0.01235 = 0.02104 -0.00042 0.00732 0.00221 AFIX 137 H13C 2 -0.242016 0.728958 0.773250 11.00000 -1.50000 H13D 2 -0.349319 0.747598 0.649494 11.00000 -1.50000 H13E 2 -0.173384 0.732408 0.616577 11.00000 -1.50000 AFIX 0 C13D 1 0.900656 0.272108 -0.142045 11.00000 0.03090 0.01395 = 0.03093 -0.00053 -0.01415 -0.00085 AFIX 137 H13F 2 0.926405 0.269895 -0.242614 11.00000 -1.50000 H13G 2 0.819176 0.253429 -0.118308 11.00000 -1.50000 H13H 2 0.997649 0.267748 -0.083983 11.00000 -1.50000 AFIX 0 C2B 1 -0.360323 0.602429 1.106914 11.00000 0.02728 0.02056 = 0.01729 0.00534 -0.00010 -0.00599 AFIX 23 H2BA 2 -0.417144 0.606965 1.196467 11.00000 -1.20000 H2BB 2 -0.279186 0.582482 1.122791 11.00000 -1.20000 AFIX 0 C11 1 0.103257 0.565352 0.339211 11.00000 0.01772 0.01152 = 0.01706 -0.00212 0.00066 0.00001 AFIX 23 H11A 2 0.185912 0.583276 0.373950 11.00000 -1.20000 H11B 2 0.041524 0.575892 0.257715 11.00000 -1.20000 AFIX 0 C5B 1 -0.492727 0.681113 0.727126 11.00000 0.01446 0.01850 = 0.02363 0.00343 0.00348 0.00257 AFIX 23 H5BA 2 -0.566435 0.702836 0.718521 11.00000 -1.20000 H5BB 2 -0.550234 0.658661 0.690636 11.00000 -1.20000 AFIX 0 C16B 1 -0.255159 0.691067 0.368776 11.00000 0.02040 0.02205 = 0.01540 0.00332 0.00306 0.00235 AFIX 23 H16D 2 -0.296702 0.689998 0.269755 11.00000 -1.20000 H16E 2 -0.199466 0.715404 0.382463 11.00000 -1.20000 AFIX 0 C11D 1 1.135999 0.322051 -0.382884 11.00000 0.01690 0.02460 = 0.02640 -0.01261 -0.00350 0.00570 C1D 1 0.718350 0.408815 -0.472810 11.00000 0.02444 0.02143 = 0.02327 0.00645 0.00324 0.00578 AFIX 23 H1DA 2 0.714991 0.436577 -0.466952 11.00000 -1.20000 H1DB 2 0.608303 0.399157 -0.489823 11.00000 -1.20000 AFIX 0 C14D 1 1.108578 0.340335 -0.023123 11.00000 0.01767 0.01966 = 0.02311 -0.00675 -0.00384 -0.00137 AFIX 23 H14C 2 1.164949 0.316252 -0.038740 11.00000 -1.20000 H14D 2 1.186135 0.360993 -0.037230 11.00000 -1.20000 AFIX 0 C12D 1 1.268674 0.300965 -0.297008 11.00000 0.01807 0.03270 = 0.03434 -0.01642 -0.00770 0.01050 AFIX 137 H12G 2 1.220050 0.280766 -0.241888 11.00000 -1.50000 H12H 2 1.323533 0.318575 -0.232562 11.00000 -1.50000 H12I 2 1.346239 0.290237 -0.362334 11.00000 -1.50000 AFIX 0 C5D 1 0.685000 0.320139 -0.211434 11.00000 0.01571 0.01777 = 0.02563 0.00456 -0.00523 -0.00290 AFIX 23 H5DA 2 0.608745 0.298967 -0.203268 11.00000 -1.20000 H5DB 2 0.630175 0.343214 -0.179436 11.00000 -1.20000 AFIX 0 C18B 1 -0.645120 0.663719 0.383571 11.00000 0.01814 0.03778 = 0.03783 0.00318 -0.00812 -0.00001 AFIX 23 H18C 2 -0.727032 0.659836 0.456665 11.00000 -1.20000 H18D 2 -0.674403 0.648654 0.298665 11.00000 -1.20000 AFIX 0 C19B 1 -0.629949 0.705327 0.346081 11.00000 0.02669 0.04063 = 0.03414 0.00979 -0.00963 0.00640 AFIX 23 H19C 2 -0.593180 0.708621 0.247698 11.00000 -1.20000 H19D 2 -0.733463 0.718541 0.356778 11.00000 -1.20000 AFIX 0 C18 1 0.610602 0.473205 -0.103084 11.00000 0.02406 0.04021 = 0.07222 -0.02428 0.02366 -0.00501 AFIX 23 H18A 2 0.703804 0.474534 -0.036543 11.00000 -1.20000 H18B 2 0.643110 0.483240 -0.196100 11.00000 -1.20000 AFIX 0 C18D 1 0.538284 0.344324 0.121704 11.00000 0.02113 0.05055 = 0.04402 0.00645 0.00933 -0.00484 AFIX 23 H18E 2 0.459031 0.349238 0.044322 11.00000 -1.20000 H18F 2 0.513082 0.360476 0.203766 11.00000 -1.20000 AFIX 0 C19D 1 0.537872 0.303096 0.163455 11.00000 0.03270 0.05595 = 0.03861 0.01781 0.00253 -0.01429 AFIX 23 H19E 2 0.569991 0.299852 0.264365 11.00000 -1.20000 H19F 2 0.430596 0.291784 0.147295 11.00000 -1.20000 AFIX 0 C19 1 0.554691 0.433967 -0.118061 11.00000 0.06909 0.03031 = 0.10344 0.01146 0.06780 0.01444 AFIX 23 H19A 2 0.534469 0.427836 -0.219260 11.00000 -1.20000 H19B 2 0.636594 0.416401 -0.079393 11.00000 -1.20000 AFIX 0 H5B 2 -0.154046 0.688027 1.073419 11.00000 0.03597 H4D 2 1.027081 0.308035 -0.546064 11.00000 0.04647 HKLF 4 REM me_a.res in P2(1) REM wR2 = 0.0908, GooF = S = 1.043, Restrained GooF = 1.043 for all data REM R1 = 0.0346 for 7556 Fo > 4sig(Fo) and 0.0350 for all 7622 data REM 691 parameters refined using 1 restraints END WGHT 0.0485 0.6036 REM Highest difference peak 0.258, deepest hole -0.430, 1-sigma level 0.069 Q1 1 0.6074 0.4380 -0.0418 11.00000 0.05 0.26 Q2 1 0.7005 0.4885 -0.1319 11.00000 0.05 0.25 Q3 1 0.6122 0.4105 -0.1387 11.00000 0.05 0.25 Q4 1 0.1675 0.6959 0.9981 11.00000 0.05 0.21 Q5 1 1.2170 0.3675 0.1798 11.00000 0.05 0.21 Q6 1 -0.6924 0.6909 0.1339 11.00000 0.05 0.20 Q7 1 1.3380 0.3614 -0.0864 11.00000 0.05 0.19 Q8 1 1.3329 0.2990 -0.4882 11.00000 0.05 0.19 Q9 1 1.1418 0.3090 -0.5876 11.00000 0.05 0.19 Q10 1 -0.6859 0.6282 0.4695 11.00000 0.05 0.19 Q11 1 0.1164 0.6418 0.3029 11.00000 0.05 0.19 Q12 1 0.7282 0.4643 -0.4107 11.00000 0.05 0.19 Q13 1 -0.6807 0.7098 0.4353 11.00000 0.05 0.19 Q14 1 0.6960 0.4702 -0.4484 11.00000 0.05 0.19 Q15 1 0.2144 0.6707 1.0636 11.00000 0.05 0.18 Q16 1 1.2957 0.3070 0.3323 11.00000 0.05 0.18 Q17 1 -0.7936 0.6882 0.2113 11.00000 0.05 0.18 Q18 1 0.8444 0.4725 -0.3202 11.00000 0.05 0.18 Q19 1 0.0735 0.6513 1.1753 11.00000 0.05 0.18 Q20 1 0.2881 0.6832 1.0439 11.00000 0.05 0.18 REM The information below was added by Olex2. REM REM R1 = 0.0346 for 7556 Fo > 4sig(Fo) and 0.0350 for all 10594 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.26, deepest hole -0.43 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0350 REM R1_gt = 0.0346 REM wR_ref = 0.0908 REM GOOF = 1.043 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 10594 REM Reflections_gt = 7556 REM Parameters = n/a REM Hole = -0.43 REM Peak = 0.26 REM Flack = 0.01(6) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.497 _oxdiff_exptl_absorpt_empirical_full_min 0.695