data_csj-cy-2 _audit_creation_date 2019-08-19 _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 'C24 H36 O6' _chemical_formula_sum 'C24 H36 O6' _chemical_formula_weight 420.53 _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 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' 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' _cell_length_a 8.08181(13) _cell_length_b 10.73068(14) _cell_length_c 24.3476(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2111.51(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8739 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.2910 _cell_measurement_theta_min 3.6210 _shelx_estimated_absorpt_T_max 0.942 _shelx_estimated_absorpt_T_min 0.908 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.72782 _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 1.323 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_unetI/netI 0.0210 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.980 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 9823 _diffrn_reflns_point_group_measured_fraction_full 0.978 _diffrn_reflns_point_group_measured_fraction_max 0.946 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.416 _diffrn_reflns_theta_min 3.631 _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 0.999 _diffrn_measured_fraction_theta_max 0.980 _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 -115.00 -17.00 1.00 1.00 -- -41.11 -38.00-120.00 98 2 \w -115.00 -17.00 1.00 1.00 -- -41.11 -38.00 -60.00 98 3 \w -69.00 32.00 1.00 1.00 -- -41.11 57.00 150.00 101 4 \w 23.00 97.00 1.00 1.00 -- 41.11-125.00 0.00 74 5 \w 34.00 133.00 1.00 1.00 -- 106.95 -45.00 30.00 99 6 \w 94.00 178.00 1.00 1.00 -- 106.95 125.00 -60.00 84 7 \w 94.00 178.00 1.00 1.00 -- 106.95 125.00 150.00 84 8 \w 81.00 178.00 1.00 1.00 -- 106.95 45.00 -90.00 97 9 \w 35.00 112.00 1.00 1.00 -- 106.95 -61.00-180.00 77 ; _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 -0.0795058000 _diffrn_orient_matrix_UB_12 -0.1303399000 _diffrn_orient_matrix_UB_13 -0.0029856000 _diffrn_orient_matrix_UB_21 -0.0741248000 _diffrn_orient_matrix_UB_22 0.0188578000 _diffrn_orient_matrix_UB_23 0.0577105000 _diffrn_orient_matrix_UB_31 -0.1565011000 _diffrn_orient_matrix_UB_32 0.0571649000 _diffrn_orient_matrix_UB_33 -0.0258283000 _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 0.679 _reflns_Friedel_fraction_full 0.950 _reflns_Friedel_fraction_max 0.900 _reflns_number_gt 3978 _reflns_number_total 4020 _reflns_odcompleteness_completeness 99.86 _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 0.230 _refine_diff_density_min -0.139 _refine_diff_density_rms 0.036 _refine_ls_abs_structure_details ; Flack x determined using 1589 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.04(5) _refine_ls_extinction_coef 0.0072(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 277 _refine_ls_number_reflns 4020 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0281 _refine_ls_restrained_S_all 1.055 _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^)+(0.0417P)^2^+0.4438P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0731 _refine_ls_wR_factor_ref 0.0734 _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 2.a Ternary CH refined with riding coordinates: C17(H17), C1(H1A) 2.b Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C5(H5A,H5B), C18(H18A,H18B), C9(H9A,H9B), C14(H14A,H14B), C19(H19A,H19B), C2(H2A,H2B), C20(H20A,H20B), C6(H6A,H6B), C12(H12A,H12B), C4(H4A,H4B), C13(H13A,H13B), C3(H3A,H3B), C22(H22A,H22B), C23(H23A,H23B) 2.c Idealised Me refined as rotating group: C24(H24A,H24B,H24C) ; _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 O1 O 0.27442(16) 0.26740(11) 0.38577(5) 0.0167(3) Uani 1 1 d . . . . . O2 O 0.35158(17) 0.20157(11) 0.26510(5) 0.0208(3) Uani 1 1 d . . . . . O4 O 0.12355(15) 0.56793(11) 0.27942(5) 0.0173(3) Uani 1 1 d . . . . . O5 O 0.33615(16) 0.86172(11) 0.36394(5) 0.0182(3) Uani 1 1 d . . . . . O6 O 0.29610(17) 0.84195(11) 0.45693(5) 0.0205(3) Uani 1 1 d . . . . . O3 O 0.08241(15) 0.36643(11) 0.30641(5) 0.0179(3) Uani 1 1 d . . . . . C8 C 0.3827(2) 0.29644(15) 0.28948(7) 0.0153(3) Uani 1 1 d . . . . . C15 C 0.1311(2) 0.65467(15) 0.39204(7) 0.0164(3) Uani 1 1 d . . . . . H15A H 0.072852 0.682076 0.424712 0.020 Uiso 1 1 calc R . . . . H15B H 0.108642 0.714100 0.362958 0.020 Uiso 1 1 calc R . . . . C17 C 0.4131(2) 0.59630(14) 0.35322(6) 0.0132(3) Uani 1 1 d . . . . . H17 H 0.392432 0.656204 0.323621 0.016 Uiso 1 1 calc R . . . . C11 C 0.1545(2) 0.48375(15) 0.32349(7) 0.0150(3) Uani 1 1 d . . . . . C10 C 0.3456(2) 0.47071(15) 0.33018(6) 0.0133(3) Uani 1 1 d . . . . . C5 C 0.7536(2) 0.27808(16) 0.45505(7) 0.0193(4) Uani 1 1 d . . . . . H5A H 0.828866 0.341417 0.441487 0.023 Uiso 1 1 calc R . . . . H5B H 0.755691 0.280668 0.494866 0.023 Uiso 1 1 calc R . . . . C18 C 0.6012(2) 0.60265(15) 0.36211(7) 0.0146(3) Uani 1 1 d . . . . . H18A H 0.630847 0.553226 0.393981 0.017 Uiso 1 1 calc R . . . . H18B H 0.657248 0.567737 0.330422 0.017 Uiso 1 1 calc R . . . . C9 C 0.4152(2) 0.43041(15) 0.27283(6) 0.0147(3) Uani 1 1 d . . . . . H9A H 0.349245 0.458585 0.241955 0.018 Uiso 1 1 calc R . . . . H9B H 0.531362 0.449842 0.267526 0.018 Uiso 1 1 calc R . . . . C7 C 0.3872(2) 0.32939(14) 0.35092(7) 0.0136(3) Uani 1 1 d . . . . . C1 C 0.5652(2) 0.29995(15) 0.37207(7) 0.0136(3) Uani 1 1 d . . . . . H1A H 0.640776 0.362135 0.356567 0.016 Uiso 1 1 calc R . . . . C24 C 0.3463(2) 0.58031(15) 0.45736(7) 0.0169(3) Uani 1 1 d . . . . . H24A H 0.284351 0.618876 0.486398 0.025 Uiso 1 1 calc GR . . . . H24B H 0.461921 0.581542 0.466377 0.025 Uiso 1 1 calc GR . . . . H24C H 0.310353 0.495644 0.452910 0.025 Uiso 1 1 calc GR . . . . C14 C 0.0672(2) 0.52681(16) 0.37508(7) 0.0164(3) Uani 1 1 d . . . . . H14A H 0.086652 0.467509 0.404451 0.020 Uiso 1 1 calc R . . . . H14B H -0.050997 0.531044 0.368504 0.020 Uiso 1 1 calc R . . . . C19 C 0.6579(2) 0.73713(15) 0.37067(7) 0.0175(4) Uani 1 1 d . . . . . H19A H 0.776046 0.738389 0.377717 0.021 Uiso 1 1 calc R . . . . H19B H 0.637236 0.784788 0.337522 0.021 Uiso 1 1 calc R . . . . C2 C 0.6230(2) 0.16986(15) 0.35275(7) 0.0168(3) Uani 1 1 d . . . . . H2A H 0.546592 0.107238 0.366223 0.020 Uiso 1 1 calc R . . . . H2B H 0.621662 0.166905 0.312930 0.020 Uiso 1 1 calc R . . . . C20 C 0.5669(2) 0.79728(16) 0.41879(7) 0.0177(4) Uani 1 1 d . . . . . H20A H 0.598587 0.756194 0.452683 0.021 Uiso 1 1 calc R . . . . H20B H 0.598325 0.884301 0.421522 0.021 Uiso 1 1 calc R . . . . C6 C 0.5787(2) 0.30625(16) 0.43486(7) 0.0164(3) Uani 1 1 d . . . . . H6A H 0.546729 0.388807 0.447133 0.020 Uiso 1 1 calc R . . . . H6B H 0.502407 0.246784 0.450947 0.020 Uiso 1 1 calc R . . . . C16 C 0.3179(2) 0.65200(15) 0.40370(7) 0.0137(3) Uani 1 1 d . . . . . C21 C 0.3801(2) 0.78752(15) 0.41117(6) 0.0157(4) Uani 1 1 d . . . . . C12 C -0.0012(3) 0.38339(18) 0.25493(8) 0.0225(4) Uani 1 1 d . . . . . H12A H -0.107352 0.341237 0.254689 0.027 Uiso 1 1 calc R . . . . H12B H 0.065235 0.352989 0.224568 0.027 Uiso 1 1 calc R . . . . C4 C 0.8113(2) 0.15019(18) 0.43550(8) 0.0224(4) Uani 1 1 d . . . . . H4A H 0.925470 0.137234 0.446431 0.027 Uiso 1 1 calc R . . . . H4B H 0.744430 0.085995 0.452629 0.027 Uiso 1 1 calc R . . . . C13 C -0.0225(2) 0.52397(17) 0.25212(8) 0.0208(4) Uani 1 1 d . . . . . H13A H -0.026840 0.552830 0.214389 0.025 Uiso 1 1 calc R . . . . H13B H -0.121894 0.550490 0.271151 0.025 Uiso 1 1 calc R . . . . C3 C 0.7972(2) 0.13986(17) 0.37325(7) 0.0203(4) Uani 1 1 d . . . . . H3A H 0.826328 0.055924 0.362076 0.024 Uiso 1 1 calc R . . . . H3B H 0.875255 0.196737 0.356312 0.024 Uiso 1 1 calc R . . . . C22 C 0.2634(3) 0.96886(16) 0.44210(8) 0.0241(4) Uani 1 1 d . . . . . H22A H 0.358996 1.021429 0.448735 0.029 Uiso 1 1 calc R . . . . H22B H 0.169278 1.001766 0.462096 0.029 Uiso 1 1 calc R . . . . C23 C 0.2267(2) 0.95817(16) 0.38152(9) 0.0239(4) Uani 1 1 d . . . . . H23A H 0.112103 0.935266 0.375264 0.029 Uiso 1 1 calc R . . . . H23B H 0.249811 1.035801 0.362611 0.029 Uiso 1 1 calc R . . . . H1 H 0.180(4) 0.268(3) 0.3673(11) 0.041(7) 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 O1 0.0157(6) 0.0147(6) 0.0197(6) 0.0035(5) 0.0006(5) -0.0016(5) O2 0.0245(7) 0.0161(6) 0.0219(6) -0.0057(5) -0.0054(5) 0.0013(5) O4 0.0164(6) 0.0171(6) 0.0183(6) 0.0051(5) -0.0043(5) -0.0002(5) O5 0.0220(6) 0.0126(5) 0.0199(6) 0.0033(5) -0.0018(5) 0.0034(5) O6 0.0262(7) 0.0141(6) 0.0212(6) -0.0051(5) 0.0038(5) 0.0034(5) O3 0.0182(6) 0.0143(5) 0.0213(6) -0.0006(5) -0.0062(5) -0.0033(5) C8 0.0131(8) 0.0154(7) 0.0175(8) -0.0009(6) -0.0020(6) 0.0027(6) C15 0.0141(8) 0.0142(7) 0.0209(8) -0.0005(6) 0.0022(7) 0.0021(7) C17 0.0151(8) 0.0105(7) 0.0140(7) 0.0006(6) 0.0005(6) 0.0002(6) C11 0.0162(8) 0.0115(7) 0.0173(7) 0.0026(6) -0.0021(7) -0.0012(7) C10 0.0153(8) 0.0110(7) 0.0138(7) 0.0003(6) -0.0003(6) -0.0004(6) C5 0.0209(9) 0.0191(8) 0.0178(8) -0.0001(7) -0.0035(7) 0.0019(7) C18 0.0140(8) 0.0138(7) 0.0159(7) -0.0012(6) 0.0009(6) -0.0001(6) C9 0.0161(8) 0.0151(7) 0.0130(7) -0.0011(6) -0.0003(7) 0.0014(6) C7 0.0148(8) 0.0114(7) 0.0145(7) 0.0002(6) 0.0006(6) -0.0001(6) C1 0.0138(8) 0.0123(7) 0.0148(7) 0.0006(6) 0.0004(6) 0.0005(6) C24 0.0200(8) 0.0156(7) 0.0150(7) 0.0011(6) 0.0029(7) 0.0028(7) C14 0.0116(7) 0.0170(8) 0.0207(8) 0.0011(6) 0.0019(7) -0.0008(6) C19 0.0159(8) 0.0154(8) 0.0211(8) -0.0004(6) -0.0007(7) -0.0023(7) C2 0.0190(9) 0.0147(7) 0.0167(7) -0.0012(6) 0.0000(7) 0.0029(7) C20 0.0206(9) 0.0136(7) 0.0190(8) -0.0013(6) -0.0036(7) -0.0017(7) C6 0.0194(8) 0.0153(7) 0.0146(8) -0.0007(6) 0.0003(7) 0.0034(7) C16 0.0154(8) 0.0118(7) 0.0137(7) 0.0001(6) 0.0005(6) 0.0007(6) C21 0.0210(9) 0.0126(7) 0.0137(7) -0.0001(6) 0.0002(7) 0.0027(7) C12 0.0207(8) 0.0258(9) 0.0209(8) -0.0018(7) -0.0060(7) -0.0028(7) C4 0.0230(9) 0.0218(9) 0.0224(9) 0.0010(7) -0.0041(7) 0.0074(8) C13 0.0155(9) 0.0270(9) 0.0198(8) 0.0026(7) -0.0053(7) 0.0006(7) C3 0.0212(9) 0.0182(8) 0.0214(8) -0.0010(7) 0.0009(7) 0.0070(7) C22 0.0249(9) 0.0125(8) 0.0350(10) -0.0060(7) 0.0038(9) 0.0035(7) C23 0.0230(9) 0.0120(7) 0.0366(10) 0.0004(7) -0.0030(9) 0.0042(7) _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 O1 C7 1.412(2) . ? O2 C8 1.205(2) . ? O4 C11 1.4248(19) . ? O4 C13 1.434(2) . ? O5 C21 1.4432(19) . ? O5 C23 1.427(2) . ? O6 C21 1.429(2) . ? O6 C22 1.433(2) . ? O3 C11 1.4482(19) . ? O3 C12 1.436(2) . ? C8 C9 1.517(2) . ? C8 C7 1.538(2) . ? C15 C14 1.523(2) . ? C15 C16 1.537(2) . ? C17 C10 1.558(2) . ? C17 C18 1.537(2) . ? C17 C16 1.568(2) . ? C11 C10 1.559(2) . ? C11 C14 1.513(2) . ? C10 C9 1.566(2) . ? C10 C7 1.633(2) . ? C5 C6 1.527(2) . ? C5 C4 1.526(2) . ? C18 C19 1.528(2) . ? C7 C1 1.560(2) . ? C1 C2 1.545(2) . ? C1 C6 1.534(2) . ? C24 C16 1.533(2) . ? C19 C20 1.527(2) . ? C2 C3 1.527(3) . ? C20 C21 1.524(3) . ? C16 C21 1.549(2) . ? C12 C13 1.520(3) . ? C4 C3 1.524(2) . ? C22 C23 1.509(3) . ? 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 C11 O4 C13 106.55(13) . . ? C23 O5 C21 108.29(13) . . ? C21 O6 C22 106.22(13) . . ? C12 O3 C11 109.25(13) . . ? O2 C8 C9 134.87(15) . . ? O2 C8 C7 132.72(15) . . ? C9 C8 C7 92.17(12) . . ? C14 C15 C16 111.48(14) . . ? C10 C17 C16 116.11(13) . . ? C18 C17 C10 115.80(13) . . ? C18 C17 C16 110.96(13) . . ? O4 C11 O3 105.33(13) . . ? O4 C11 C10 108.03(13) . . ? O4 C11 C14 110.48(14) . . ? O3 C11 C10 110.51(13) . . ? O3 C11 C14 108.45(13) . . ? C14 C11 C10 113.72(14) . . ? C17 C10 C11 107.86(14) . . ? C17 C10 C9 115.70(13) . . ? C17 C10 C7 128.27(13) . . ? C11 C10 C9 106.72(13) . . ? C11 C10 C7 108.66(13) . . ? C9 C10 C7 86.86(12) . . ? C4 C5 C6 111.15(15) . . ? C19 C18 C17 110.97(13) . . ? C8 C9 C10 87.77(12) . . ? O1 C7 C8 117.44(14) . . ? O1 C7 C10 119.34(14) . . ? O1 C7 C1 107.56(13) . . ? C8 C7 C10 84.71(11) . . ? C8 C7 C1 107.25(13) . . ? C1 C7 C10 118.69(13) . . ? C2 C1 C7 111.17(13) . . ? C6 C1 C7 112.67(13) . . ? C6 C1 C2 108.76(14) . . ? C11 C14 C15 110.02(14) . . ? C20 C19 C18 111.06(14) . . ? C3 C2 C1 111.68(14) . . ? C21 C20 C19 110.78(14) . . ? C5 C6 C1 112.20(14) . . ? C15 C16 C17 110.13(14) . . ? C15 C16 C21 108.84(13) . . ? C24 C16 C15 108.28(14) . . ? C24 C16 C17 113.79(13) . . ? C24 C16 C21 108.80(13) . . ? C21 C16 C17 106.90(13) . . ? O5 C21 C20 107.64(14) . . ? O5 C21 C16 110.14(13) . . ? O6 C21 O5 106.17(13) . . ? O6 C21 C20 110.34(14) . . ? O6 C21 C16 108.71(13) . . ? C20 C21 C16 113.57(13) . . ? O3 C12 C13 102.62(14) . . ? C3 C4 C5 110.65(15) . . ? O4 C13 C12 102.25(14) . . ? C4 C3 C2 112.27(15) . . ? O6 C22 C23 102.14(14) . . ? O5 C23 C22 103.07(15) . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code 0 0 2 258588 3711.71 1 0 0 2 259966 3673.23 3 0 0 2 255511 3702.29 2 0 0 3 51.3214 17.4644 2 0 0 3 138.438 15.8035 3 0 0 5 28.1246 26.9104 1 0 0 5 79.5576 21.2683 3 0 0 6 579836 8184.94 3 0 0 6 569880 8280.59 2 0 0 6 564124 8304.93 1 0 0 7 14.7122 21.2985 3 0 0 7 16.9655 32.2951 2 0 0 8 501002 7266.65 1 0 0 8 485943 7225.83 2 0 0 8 494001 7088.96 3 0 0 9 151.796 59.8396 1 0 0 9 52.5622 25.9163 3 0 0 10 954598 13606.7 2 0 0 10 960186 13650.8 1 0 0 10 925757 13384.1 3 0 0 11 339.654 90.1741 1 0 0 11 50.9006 58.6475 2 0 0 12 607056 8964.13 1 0 0 12 590121 8894.68 2 0 0 13 58.7861 72.2505 2 0 0 13 257.422 95.0153 1 0 0 14 6913.65 369.524 2 0 0 14 7178.84 398.53 1 0 0 15 60.9407 77.3871 2 0 0 15 53.2363 91.7825 1 0 0 -16 99523 2091.28 4 0 0 16 96321.3 2000.13 2 0 0 16 98624.7 2099.33 1 0 0 17 50.3263 82.8573 1 0 0 -17 151.65 118.534 4 0 0 18 1242.76 213.441 1 0 0 -18 1013.53 195.262 9 0 0 18 793.644 178.087 8 0 0 -19 90.3403 121.398 9 0 0 19 -49.12 98.3876 8 0 0 19 -69.6113 138.77 1 0 0 20 37.0569 112.46 1 0 0 -20 174.941 125.467 9 0 0 20 158.021 111.385 8 0 0 -21 88.2198 128.168 9 0 0 21 208.62 135.357 8 0 0 -22 103712 2352.03 9 0 0 22 99370.9 2294.31 8 0 0 23 182.056 138.002 8 0 0 -23 85.5214 120.637 9 0 0 -24 8788.42 551.986 9 0 0 24 8704.58 542.15 8 0 0 25 424.63 154.567 8 0 0 -25 1.30896 104.878 9 0 0 -26 3435.83 311.456 9 0 0 26 3303.61 312.274 8 0 0 27 77.7348 88.2653 8 0 0 -27 44.1172 88.6395 9 0 0 28 1708.86 195.572 8 0 0 29 136.04 82.61 8 0 1 0 50.4996 11.9874 2 0 1 -1 5952.71 121.775 4 0 -1 1 5360.22 139.218 1 0 -1 2 439699 6424.68 1 0 1 2 429344 6397.16 2 0 1 -3 137172 1988.99 4 0 -1 3 132849 2030.18 1 0 1 3 131401 2006.48 2 0 1 4 808719 11477.6 3 0 -1 4 793868 11540.1 1 0 1 4 818500 11515.1 2 0 1 -4 802462 11497 4 0 -1 5 457497 6649.21 1 0 1 5 468332 6621.72 2 0 -1 5 450778 6588.29 2 0 1 -5 452840 6605.96 4 0 1 5 467323 6624.39 1 0 1 5 448542 6566.18 3 0 -1 6 76286.4 1291.61 1 0 1 6 72642.1 1254.46 2 0 1 6 77265.1 1269.42 1 0 -1 6 74021.2 1231.55 2 0 1 6 73213.6 1191.03 3 0 1 -6 76924.7 1251.99 4 0 1 7 50215.3 963.899 1 0 -1 7 51733.5 991.785 1 0 -1 7 50664.7 932.443 2 0 1 -7 50621.1 945.475 4 0 1 7 51065.7 890.203 3 0 1 -8 30912.4 668.478 4 0 -1 8 30606.4 650.31 2 0 1 8 32183 684.102 1 0 -1 8 30761 705.26 1 0 1 8 30000.2 662.34 2 0 1 8 30090.4 591.843 3 0 -1 9 2366.2 180.759 1 0 1 -9 2295.78 159.41 4 0 1 9 2305.13 158.34 2 0 1 9 2228.22 124.779 3 0 -1 9 2163.99 151.651 2 0 1 10 14681.1 466.133 1 0 1 10 15603.9 386.481 3 0 -1 10 14678.4 446.752 2 0 -1 10 15401.4 499.005 1 0 1 -10 15188.5 468.751 4 0 1 10 14390.7 456.161 2 0 1 11 100544 1836.73 2 0 1 -11 104677 1868.44 4 0 1 11 105511 1701.51 3 0 1 11 102665 1859.95 1 0 -1 11 102465 1910.63 1 0 -1 11 101003 1820.64 2 0 1 12 14435.3 509.522 2 0 1 -12 15236.3 531.874 4 0 -1 12 15867.6 563.435 1 0 1 12 15915.1 415.622 3 0 1 12 15149.4 520.23 1 0 -1 12 14233.8 489.054 2 0 1 -13 1248.39 162.047 4 0 1 13 2278.76 217.589 2 0 1 13 2029.46 219.745 1 0 -1 13 1300.65 177.096 1 0 1 14 83813.6 1715.16 2 0 1 -14 86173.6 1750.23 4 0 1 14 81372.3 1718.59 1 0 -1 14 84506.9 1796.69 1 0 -1 15 35300.7 1074.9 1 0 1 15 38801.3 1055.08 1 0 1 15 34988.1 996.215 2 0 1 -15 40119.3 1065.59 4 0 1 16 33853.5 1002.17 2 0 -1 16 36361.9 1104.9 1 0 1 16 33581.1 1026.95 1 0 1 17 153449 2936.83 2 0 1 17 156524 3007.04 1 0 -1 17 157903 3087.12 1 0 -1 -18 1242.45 221.728 9 0 -1 18 1358.22 228.813 1 0 1 18 824.583 177.878 2 0 1 18 906.179 180.89 8 0 1 -18 986.565 191.544 9 0 1 19 3298.23 350.262 1 0 -1 -19 3948.44 370.104 9 0 -1 -19 3408.93 364.884 4 0 1 -19 3931.89 369.654 9 0 -1 19 3479.35 368.306 1 0 1 19 3876.97 355.819 8 0 1 19 3157.28 324.635 2 0 -1 19 3303.18 338.439 8 0 1 20 670.365 190.238 1 0 -1 20 709.854 176.64 8 0 -1 20 875.712 214.33 1 0 1 20 703.479 178.966 8 0 1 -20 919.774 197.707 9 0 -1 -20 1196.57 224.976 9 0 -1 -21 9514.04 589.195 9 0 -1 21 7805.84 531.314 8 0 1 21 7934.79 528.835 8 0 1 -21 8524.67 552.13 9 0 1 -22 498.475 172.07 9 0 1 22 680.8 175.805 8 0 -1 22 522.139 169.687 8 0 -1 -22 659.103 191.655 9 0 -1 23 133157 2787.18 8 0 1 23 131381 2781.8 8 0 1 -23 132903 2809.64 9 0 -1 -23 136629 2844.06 9 0 1 24 4770.16 406.296 8 0 -1 -24 5111.86 424.867 9 0 -1 24 4858.28 406.359 8 0 1 -24 4957.28 412.937 9 0 -1 -25 5551.67 423.776 9 0 -1 25 4951.88 393.39 8 0 1 -25 5121.3 397.546 9 0 1 25 5324.48 412.251 8 0 1 -26 8497.46 485.43 9 0 -1 -26 8749.66 495.094 9 0 -1 26 8641.09 494.17 8 0 1 26 8267.99 490.669 8 0 1 -27 445.896 122.722 9 0 1 27 357.529 120.287 8 0 -1 27 419.497 124.028 8 0 1 -28 320.192 105.11 9 0 -1 28 288.486 101.531 8 0 1 28 197.491 92.1487 8 0 1 29 84.7971 80.8133 8 0 -1 29 153.042 77.8603 8 0 2 0 261712 3793.16 2 0 2 -1 18751.1 354.523 2 0 -2 1 18097.2 396.962 1 0 2 2 348815 4953.26 2 0 -2 2 331532 4997.38 1 0 2 -3 50202.4 805.838 4 0 -2 3 48515.7 884.367 1 0 2 3 48619.9 840.32 2 0 -2 4 318148 4692.84 1 0 2 -4 301073 4591.41 4 0 2 5 100721 1722.16 2 0 2 5 101852 1704.19 3 0 -2 5 105503 1780.61 1 0 2 6 140014 2224.88 2 0 2 -6 143684 2172.77 4 0 -2 6 135548 2267.64 1 0 2 6 139990 2180.52 3 0 2 -7 133175 2086.12 4 0 2 7 135343 2154.17 2 0 2 7 132628 2091.67 3 0 -2 7 130932 2194.31 1 0 2 7 130819 2131.28 1 0 2 8 8399.74 312.365 2 0 -2 8 8525 347.914 1 0 2 8 8672.9 312.627 1 0 2 8 8272.48 272.979 3 0 2 -8 8852.97 289.787 4 0 2 9 56412.3 1111.69 1 0 -2 9 57837 1180.09 1 0 2 9 55660.2 1041.41 3 0 2 -9 58218.3 1074.15 4 0 2 9 55100.5 1114.37 2 0 -2 10 28417.8 768.599 1 0 2 10 29250.4 650.893 3 0 2 10 27522.3 706.011 2 0 2 -10 28742.9 679.652 4 0 2 -11 5607.6 269.268 4 0 2 11 5164.82 280.282 2 0 -2 11 5362 309.961 1 0 2 11 5296.52 236.815 3 0 2 11 5573.44 288.084 1 0 2 12 31161.5 816.919 1 0 2 12 32130.4 721.837 3 0 -2 12 30440 872.1 1 0 2 12 29942.9 813.365 2 0 2 -12 33038.5 792.433 4 0 -2 13 234.993 106.731 1 0 2 13 352.846 77.9252 3 0 -2 14 42230.2 1150.33 1 0 2 14 43265.3 1114.61 2 0 2 14 41403.7 1074.18 1 0 -2 15 39169.8 1147.98 1 0 2 15 40139.2 1078.18 1 0 2 15 40146.8 1088.59 2 0 2 16 1294.77 195.333 2 0 2 16 856.256 165.547 1 0 -2 -17 26884.5 963.318 9 0 -2 17 26808.7 1011.8 1 0 2 17 27281.7 937.404 1 0 2 17 26583.8 935.994 8 0 2 17 26612.3 915.973 2 0 2 -17 27660.6 962.109 9 0 2 18 31711 1063.95 8 0 2 18 30753.4 1039.26 2 0 -2 18 31456.2 1153.04 1 0 2 18 31984.8 1077.59 1 0 2 -18 33883.3 1104.09 9 0 -2 -18 33183.7 1114.12 9 0 2 19 7907.5 512.673 8 0 2 -19 8148.73 526.442 9 0 2 19 7876.12 516.452 2 0 -2 -19 8485.73 546.035 9 0 -2 19 8377.3 580.585 1 0 2 19 7668.85 522.939 1 0 2 20 15224.5 742.8 2 0 -2 20 16046.2 835.559 1 0 2 20 17127.3 807.301 1 0 -2 -20 14834.6 796.871 4 0 2 20 16660.5 768.541 8 0 2 -20 16928.9 783.023 9 0 -2 -20 17550.8 807.883 9 0 -2 21 1130.77 217.819 8 0 2 -21 1106.7 217.631 9 0 -2 -21 1211.48 231.267 9 0 2 21 1158.47 219.634 8 0 -2 -22 123.058 146.632 9 0 2 -22 346.801 149.521 9 0 2 22 198.811 125.343 8 0 -2 22 167.184 126.343 8 0 -2 -23 15587.4 759.866 9 0 2 -23 15012.9 730.325 9 0 -2 23 14783.7 726.338 8 0 2 23 14819.6 733.294 8 0 2 24 84.5467 112.572 8 0 -2 -24 34.7066 114.985 9 0 -2 24 115.012 114.549 8 0 2 -24 5.03774 116.187 9 0 2 -25 6950.32 453.461 9 0 -2 25 7046.46 461.251 8 0 2 25 6584.93 455.547 8 0 2 26 11986.3 591.335 8 0 2 -26 12536.4 579.598 9 0 -2 26 12636.4 594.076 8 0 2 27 14227.2 607.08 8 0 2 -27 14467.3 578.633 9 0 -2 27 14257.5 591.431 8 0 2 28 3413.64 268.76 8 0 2 -28 3487.42 248.244 9 0 -2 28 4009.36 276.701 8 0 -2 29 70.9388 62.7908 8 0 2 29 14.2935 59.7082 8 0 3 0 41.9712 30.9128 2 0 3 1 446353 6500.13 2 0 3 -1 451151 6470.83 2 0 3 -2 3027.35 122.03 2 0 3 2 2605.85 126.965 2 0 3 3 14465 366.438 2 0 -3 3 16271.1 427.599 1 0 3 4 18540.6 441.661 2 0 -3 4 18088.8 489.071 1 0 -3 5 27875.6 664.126 1 0 3 5 27493.4 606.205 3 0 3 -5 27105.5 524.801 4 0 3 5 28165.5 608.683 2 0 3 -6 20686.8 436.906 4 0 3 6 19531.6 493.4 3 0 -3 6 20706.1 564.503 1 0 3 6 19746.3 502.391 2 0 -3 7 46733.1 1028.87 1 0 3 7 48056.4 945.006 3 0 3 -7 49672.4 876.654 4 0 3 7 48643.7 971.716 2 0 3 8 66027.5 1231.15 1 0 3 -8 68805.2 1145.06 4 0 3 8 62483.3 1195.19 3 0 -3 8 61369.3 1299.06 1 0 3 8 64976.5 1250.52 2 0 -3 9 77287.1 1569.21 1 0 3 -9 84553.9 1393.75 4 0 3 9 77082.4 1433.59 3 0 3 9 81141.8 1493.57 1 0 3 9 81438.9 1512.81 2 0 3 10 209.729 81.8372 2 0 -3 10 72.3968 80.2864 1 0 3 10 19.5968 46.4104 3 0 -3 11 505123 7708.47 1 0 3 11 484507 7563.34 2 0 3 11 511583 7482.6 3 0 3 11 501655 7547.68 1 0 3 12 111234 1916.64 3 0 3 12 105435 1991.8 1 0 3 12 105972 2016.32 2 0 -3 12 105796 2122.56 1 0 3 13 28799.1 834.747 1 0 -3 13 30118.9 947.409 1 0 3 13 29935.9 862.438 2 0 3 13 31674.7 780.277 3 0 -3 14 85179.1 1914.48 1 0 3 14 84247.3 1763.74 1 0 3 14 89331.2 1823.46 2 0 3 15 753.033 163.749 2 0 -3 15 577.376 156.665 1 0 3 15 552.535 128.913 1 0 3 16 15871.4 660.285 1 0 3 16 15934.5 682.306 2 0 3 -16 16517.9 724.044 9 0 -3 16 15052.8 716.175 1 0 3 16 15948.9 705.855 8 0 3 -17 4487.14 384.015 9 0 -3 -17 4406.26 384.4 9 0 3 17 4174.04 354.943 2 0 -3 17 4125.18 384.641 1 0 3 17 4298.7 371.425 8 0 3 17 4098.47 345.639 1 0 3 18 36284.2 1187.74 8 0 3 18 36555.5 1157.01 1 0 3 18 36976.3 1171.99 2 0 -3 -18 37218.5 1218.29 9 0 -3 18 35810.4 1247.09 1 0 3 -18 37426.3 1194.27 9 0 3 -19 45135.9 1359.03 9 0 3 19 47498.5 1392.24 1 0 3 19 45243.5 1355.62 2 0 3 19 42241.9 1338.85 8 0 -3 19 45939.2 1478.02 1 0 -3 -19 47303.5 1420.51 9 0 3 -20 70251.3 1801.79 9 0 3 20 67978.5 1801.72 8 0 -3 -20 70708.6 1848.82 9 0 -3 -21 650.352 185.827 9 0 3 -21 669.259 200.965 9 0 3 21 863.154 206.069 8 0 3 22 65318.4 1752.36 8 0 -3 22 68747.6 1762.78 8 0 3 -22 67108.3 1744.56 9 0 3 -23 54.282 122.767 9 0 -3 23 161.944 144.076 8 0 3 23 38.5058 125.734 8 0 -3 24 14317.9 683.538 8 0 3 24 13655.5 687.623 8 0 3 -24 14552.8 677.695 9 0 3 -25 1694.34 227.068 9 0 -3 25 1598.63 226.624 8 0 3 25 1590.57 228.705 8 0 3 -26 12058.5 544.16 9 0 3 26 11607 568.249 8 0 -3 26 12541.1 570.799 8 0 -3 27 17325.1 631.295 8 0 3 27 15879.7 625.327 8 0 3 -27 16685.2 598.862 9 0 3 28 181.325 84.7448 8 0 -3 28 198.04 84.3573 8 0 3 -28 229.48 86.7132 9 0 -3 29 3180.4 202.365 8 0 4 0 29692.9 589.747 2 0 4 1 110181 1760.81 2 0 4 -1 109823 1734.79 2 0 4 2 4640.35 190.382 2 0 4 -2 4178.3 158.341 2 0 4 3 182825 2804.39 2 0 4 -3 178987 2709.11 2 0 -4 4 954.678 114.614 1 0 4 4 1028.71 113.751 3 0 4 5 24988.5 595.695 2 0 -4 5 24579.2 665.433 1 0 4 -5 24122.6 494.558 2 0 4 5 25563.5 620.566 3 0 4 6 41887.5 887.999 3 0 -4 6 42720.3 983.463 1 0 4 6 41044.5 873.689 2 0 4 7 78468.1 1439.72 2 0 4 7 74564.2 1423.02 3 0 -4 7 78318.8 1547.64 1 0 4 8 1143.56 134.427 2 0 -4 8 1278.88 159.729 1 0 4 8 1418.05 139.418 3 0 4 9 22099.3 614.868 1 0 4 9 22311.8 643.37 2 0 -4 9 22297.6 715.231 1 0 4 9 22169.9 609.002 3 0 -4 10 23961.8 776.66 1 0 4 10 24394.4 667.971 3 0 4 10 25011.6 714.031 2 0 4 10 24552.3 682.146 1 0 4 11 23878.8 719.83 2 0 4 11 24029.1 700.192 1 0 -4 11 23787.6 802.539 1 0 4 11 25429.2 702.119 3 0 4 12 20428.7 678.565 2 0 -4 12 20008.1 754.67 1 0 4 12 20218.3 649.729 1 0 4 12 20602.4 636.969 3 0 -4 13 174583 3245.78 1 0 4 13 174203 2970.01 3 0 4 13 176618 3098.31 2 0 4 13 169729 3029.87 1 0 4 14 80073.4 1738.14 1 0 4 14 82282.9 1799.54 2 0 -4 14 82251.5 1940.68 1 0 -4 15 34409.5 1144.77 1 0 4 15 33735.7 998.824 1 0 4 15 34133.5 1120.27 8 0 4 15 35685.7 1066.42 2 0 4 -15 35920.9 1130.32 9 0 -4 16 12240.3 671.406 1 0 4 16 12494.9 587.443 1 0 4 16 13533.2 644.282 2 0 4 16 12904.3 662.096 8 0 4 -16 12774 651.423 9 0 4 17 100.403 112.436 2 0 -4 17 369.141 165.975 1 0 4 17 153.784 126.635 8 0 4 17 88.9143 95.6049 1 0 4 -17 -16.1701 105.372 9 0 4 -18 89907.6 2118.02 9 0 4 18 89031.7 2049.83 1 0 -4 18 91263.8 2264.21 1 0 4 18 88621.5 2157.08 8 0 4 18 91621.9 2117.05 2 0 4 19 69905.9 1849.91 8 0 4 -19 70460.5 1810.51 9 0 4 -20 87664.8 2073.43 9 0 4 20 84142.5 2104.42 8 0 4 -21 10626.6 607.861 9 0 4 21 10074.4 618.122 8 0 4 22 13406.4 705.638 8 0 4 -22 13324.5 670.627 9 0 4 23 14757.3 729.392 8 0 4 -23 16019.4 715.742 9 0 -4 23 15639.7 725.566 8 0 -4 24 75299.1 1760.97 8 0 4 24 70568.4 1766.86 8 0 4 -24 72179.1 1714.48 9 0 -4 25 21284.3 782.089 8 0 4 25 20460.9 797.651 8 0 4 -25 20777.6 753.402 9 0 4 26 1597.35 205.621 8 0 4 -26 1635.67 193.016 9 0 -4 26 1725.91 210.648 8 0 4 -27 952.737 137.93 9 0 4 27 864.59 145.76 8 0 -4 27 956.423 148.308 8 0 4 -28 7357.29 305.471 9 0 -4 28 8361.96 352.792 8 0 5 0 147.723 46.4894 2 0 5 1 6015.54 244.189 2 0 5 -1 9862.6 279.478 2 0 5 2 8333.91 295.772 2 0 5 -2 8646.16 264.653 2 0 5 3 57397.8 1117.3 2 0 5 -3 59481.5 1021.38 2 0 5 3 61413.6 1202.03 3 0 5 4 1451.38 132.41 2 0 5 4 1629.33 157.541 3 0 5 5 3047.71 197.308 2 0 5 5 3716.89 229.957 3 0 5 6 156588 2636.29 2 0 5 6 158095 2674.19 3 0 -5 6 162727 2784.15 1 0 5 -7 4396.8 215.757 3 0 5 7 3806.86 240.116 2 0 -5 7 4206.26 283.172 1 0 5 7 3552.63 236.594 3 0 5 8 27673.5 757.874 3 0 -5 8 28794.5 854.308 1 0 5 8 28432 764.64 2 0 5 9 1181.2 145.493 3 0 5 9 1129.89 134.563 1 0 5 9 928.726 136.804 2 0 -5 9 1143.7 170.485 1 0 5 10 1399.07 162.471 3 0 -5 10 1341.49 199.177 1 0 5 10 1772.13 174.008 1 0 5 10 1463.7 173.567 2 0 5 11 44738.1 1077.05 1 0 5 11 44425 1118.68 2 0 -5 11 48377.1 1289.35 1 0 5 11 45524.5 1102.33 3 0 5 12 61909.3 1447.9 2 0 5 12 64934.3 1419.13 3 0 5 12 61165.1 1376.74 1 0 -5 12 64629.4 1606.06 1 0 5 -13 22302.7 864.631 9 0 5 13 21669.1 779.032 2 0 5 13 22277 739.291 1 0 -5 13 23522.5 901.586 1 0 5 13 23098.6 743.381 3 0 5 14 164208 3064.96 2 0 -5 14 168471 3275.18 1 0 5 -14 164745 3215.17 9 0 5 14 159696 2968.76 1 0 5 14 167139 2964.17 3 0 5 14 162901 3256.62 8 0 5 15 181808 3387.22 2 0 5 15 172960 3228.89 1 0 -5 15 187750 3580.95 1 0 5 -15 185177 3489.71 9 0 5 15 177570 3521.7 8 0 5 16 3427.74 362.844 8 0 5 16 2864.56 287.209 1 0 5 -16 3351.17 343.1 9 0 5 16 3215.8 330.725 2 0 -5 16 3066.41 360 1 0 5 -17 306.621 158.478 9 0 -5 17 421.635 192.06 1 0 5 17 437.635 148.986 1 0 5 17 489.337 150.999 2 0 5 17 329.515 157.113 8 0 5 -18 23109.4 934.04 9 0 5 18 23914.9 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9059.99 399.15 7 -9 -2 6 8479.53 353.305 7 -9 -2 7 12105.7 426.988 5 -9 2 -7 13592.9 486.087 7 -9 -2 7 12699.6 415.405 7 -9 -2 8 33107.1 784.672 5 -9 -2 9 5051.66 258.498 5 -9 -2 10 12490.6 414.503 5 -9 -2 11 11621.7 380.626 5 -9 -2 12 3616.55 191.126 5 -9 -3 -9 1343.31 121.02 7 -9 3 9 1169.98 120.952 5 -9 -3 -8 13425.6 428.583 7 -9 -3 -7 1585.85 153.098 7 -9 -3 -6 14152.9 484.496 7 -9 -3 -5 14157.8 500.393 7 -9 -3 -4 893.555 136.392 7 -9 -3 -3 11185 456.196 7 -9 -3 -2 6396.87 346.034 7 -9 3 1 7121.18 317.86 7 -9 -3 -1 7549.92 377.69 7 -9 3 0 435.395 94.7748 7 -9 -3 0 379.385 104.218 7 -9 3 -1 7389.19 342.056 7 -9 -3 1 7696.27 378.366 7 -9 3 -2 5787.22 304.849 7 -9 -3 2 6144.55 336.592 7 -9 3 -3 10506.2 420.872 7 -9 -3 3 10166.1 430.628 7 -9 -3 4 910.81 132.034 7 -9 -3 5 13581.4 471.344 7 -9 -3 6 12591.5 418.098 5 -9 -3 6 13187 442.245 7 -9 -3 7 1569.83 143.646 5 -9 -3 7 1454.12 137.016 7 -9 -3 8 12603.4 410.893 5 -9 -3 8 12575.6 377.25 7 -9 -3 9 1083.02 117.321 5 -9 -3 10 7826.55 297.224 5 -9 -4 -7 14789.7 433.047 7 -9 -4 -6 9744.92 359.36 7 -9 -4 -5 2616.77 192.628 7 -9 -4 -4 20807.2 604.965 7 -9 -4 -3 743.766 122.449 7 -9 -4 -2 3101.64 226.031 7 -9 -4 -1 2912.78 222.272 7 -9 -4 0 5200.39 296.582 7 -9 -4 1 2944.01 225.029 7 -9 -4 2 3266.66 232.537 7 -9 -4 3 861.906 128.461 7 -9 -4 4 18721.9 570.252 7 -9 -4 5 2331.88 181.148 7 -9 -4 6 7930.26 294.953 5 -9 -4 6 8734.1 336.096 7 -9 -4 7 13122.1 394.036 5 -9 -4 7 13900.6 412.878 7 -9 -5 -5 49319.1 960.973 7 -9 -5 -4 8674.65 325.111 7 -9 -5 -3 8329.72 329.97 7 -9 -5 -2 4702.79 249.552 7 -9 -5 -1 2258.99 178.063 7 -9 -5 0 683.291 108.051 7 -9 -5 1 2256.78 179.084 7 -9 -5 2 4571.61 252.25 7 -9 -5 3 8482.82 342.754 7 -9 -5 4 8189.12 326.617 7 -9 -5 5 44559.4 918.14 7 -10 0 -2 2258.79 148.026 7 _iucr_refine_instructions_details ; TITL csj-cy-2_a.res in P2(1)2(1)2(1) csj-cy-2.res created by SHELXL-2018/3 at 11:10:05 on 19-Aug-2019 REM Old TITL csj-cy-2 in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.093, Rweak 0.032, Alpha 0.003 REM 2.150 for 26 systematic absences, Orientation as input REM Flack x = -0.050 ( 0.060 ) from 1502 Parsons' quotients REM Formula found by SHELXT: C24 O6 CELL 1.54184 8.081808 10.730685 24.347647 90 90 90 ZERR 4 0.000131 0.000139 0.000358 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H O UNIT 96 144 24 L.S. 20 PLAN 20 SIZE 0.08 0.11 0.13 BOND list 4 fmap 2 53 acta REM REM REM WGHT 0.041700 0.443800 EXTI 0.007221 FVAR 9.13756 O1 3 0.274420 0.267400 0.385765 11.00000 0.01570 0.01469 = 0.01967 0.00348 0.00055 -0.00165 O2 3 0.351582 0.201565 0.265103 11.00000 0.02448 0.01609 = 0.02192 -0.00565 -0.00542 0.00127 O4 3 0.123551 0.567933 0.279417 11.00000 0.01640 0.01707 = 0.01834 0.00511 -0.00433 -0.00017 O5 3 0.336145 0.861719 0.363941 11.00000 0.02201 0.01265 = 0.01992 0.00325 -0.00184 0.00344 O6 3 0.296100 0.841947 0.456927 11.00000 0.02621 0.01410 = 0.02117 -0.00510 0.00375 0.00339 O3 3 0.082409 0.366428 0.306414 11.00000 0.01817 0.01428 = 0.02125 -0.00064 -0.00615 -0.00331 C8 1 0.382685 0.296437 0.289476 11.00000 0.01307 0.01542 = 0.01751 -0.00095 -0.00203 0.00274 C15 1 0.131098 0.654674 0.392038 11.00000 0.01409 0.01424 = 0.02086 -0.00052 0.00221 0.00213 AFIX 23 H15A 2 0.072852 0.682076 0.424712 11.00000 -1.20000 H15B 2 0.108642 0.714100 0.362958 11.00000 -1.20000 AFIX 0 C17 1 0.413079 0.596301 0.353220 11.00000 0.01506 0.01045 = 0.01401 0.00061 0.00055 0.00018 AFIX 13 H17 2 0.392432 0.656204 0.323621 11.00000 -1.20000 AFIX 0 C11 1 0.154491 0.483750 0.323488 11.00000 0.01625 0.01149 = 0.01734 0.00261 -0.00207 -0.00117 C10 1 0.345563 0.470706 0.330179 11.00000 0.01525 0.01097 = 0.01382 0.00027 -0.00026 -0.00035 C5 1 0.753604 0.278083 0.455049 11.00000 0.02087 0.01908 = 0.01781 -0.00015 -0.00347 0.00192 AFIX 23 H5A 2 0.828866 0.341417 0.441487 11.00000 -1.20000 H5B 2 0.755691 0.280668 0.494866 11.00000 -1.20000 AFIX 0 C18 1 0.601179 0.602647 0.362110 11.00000 0.01401 0.01379 = 0.01594 -0.00120 0.00093 -0.00006 AFIX 23 H18A 2 0.630847 0.553226 0.393981 11.00000 -1.20000 H18B 2 0.657248 0.567737 0.330422 11.00000 -1.20000 AFIX 0 C9 1 0.415238 0.430414 0.272829 11.00000 0.01609 0.01513 = 0.01302 -0.00108 -0.00030 0.00141 AFIX 23 H9A 2 0.349245 0.458585 0.241955 11.00000 -1.20000 H9B 2 0.531362 0.449842 0.267526 11.00000 -1.20000 AFIX 0 C7 1 0.387240 0.329391 0.350917 11.00000 0.01477 0.01142 = 0.01449 0.00016 0.00060 -0.00012 C1 1 0.565228 0.299954 0.372066 11.00000 0.01384 0.01227 = 0.01480 0.00059 0.00041 0.00049 AFIX 13 H1A 2 0.640776 0.362135 0.356567 11.00000 -1.20000 AFIX 0 C24 1 0.346293 0.580314 0.457363 11.00000 0.02002 0.01563 = 0.01502 0.00110 0.00288 0.00282 AFIX 137 H24A 2 0.284351 0.618876 0.486398 11.00000 -1.50000 H24B 2 0.461921 0.581542 0.466377 11.00000 -1.50000 H24C 2 0.310353 0.495644 0.452910 11.00000 -1.50000 AFIX 0 C14 1 0.067245 0.526811 0.375081 11.00000 0.01157 0.01696 = 0.02070 0.00108 0.00186 -0.00076 AFIX 23 H14A 2 0.086652 0.467509 0.404451 11.00000 -1.20000 H14B 2 -0.050997 0.531044 0.368504 11.00000 -1.20000 AFIX 0 C19 1 0.657928 0.737128 0.370671 11.00000 0.01591 0.01545 = 0.02109 -0.00040 -0.00069 -0.00225 AFIX 23 H19A 2 0.776046 0.738389 0.377717 11.00000 -1.20000 H19B 2 0.637236 0.784788 0.337522 11.00000 -1.20000 AFIX 0 C2 1 0.623037 0.169860 0.352746 11.00000 0.01898 0.01475 = 0.01672 -0.00122 -0.00002 0.00291 AFIX 23 H2A 2 0.546592 0.107238 0.366223 11.00000 -1.20000 H2B 2 0.621662 0.166905 0.312930 11.00000 -1.20000 AFIX 0 C20 1 0.566912 0.797278 0.418789 11.00000 0.02062 0.01361 = 0.01900 -0.00134 -0.00359 -0.00172 AFIX 23 H20A 2 0.598587 0.756194 0.452683 11.00000 -1.20000 H20B 2 0.598325 0.884301 0.421522 11.00000 -1.20000 AFIX 0 C6 1 0.578709 0.306251 0.434859 11.00000 0.01937 0.01525 = 0.01459 -0.00065 0.00031 0.00340 AFIX 23 H6A 2 0.546729 0.388807 0.447133 11.00000 -1.20000 H6B 2 0.502407 0.246784 0.450947 11.00000 -1.20000 AFIX 0 C16 1 0.317948 0.651998 0.403700 11.00000 0.01538 0.01184 = 0.01373 0.00009 0.00050 0.00065 C21 1 0.380137 0.787523 0.411172 11.00000 0.02096 0.01262 = 0.01367 -0.00013 0.00022 0.00270 C12 1 -0.001183 0.383394 0.254926 11.00000 0.02075 0.02582 = 0.02090 -0.00176 -0.00604 -0.00280 AFIX 23 H12A 2 -0.107352 0.341237 0.254689 11.00000 -1.20000 H12B 2 0.065235 0.352989 0.224568 11.00000 -1.20000 AFIX 0 C4 1 0.811344 0.150186 0.435497 11.00000 0.02303 0.02180 = 0.02242 0.00100 -0.00412 0.00743 AFIX 23 H4A 2 0.925470 0.137234 0.446431 11.00000 -1.20000 H4B 2 0.744430 0.085995 0.452629 11.00000 -1.20000 AFIX 0 C13 1 -0.022509 0.523974 0.252116 11.00000 0.01546 0.02705 = 0.01980 0.00260 -0.00528 0.00063 AFIX 23 H13A 2 -0.026840 0.552830 0.214389 11.00000 -1.20000 H13B 2 -0.121894 0.550490 0.271151 11.00000 -1.20000 AFIX 0 C3 1 0.797151 0.139864 0.373246 11.00000 0.02122 0.01824 = 0.02135 -0.00097 0.00088 0.00701 AFIX 23 H3A 2 0.826328 0.055924 0.362076 11.00000 -1.20000 H3B 2 0.875255 0.196737 0.356312 11.00000 -1.20000 AFIX 0 C22 1 0.263432 0.968855 0.442095 11.00000 0.02487 0.01254 = 0.03500 -0.00597 0.00382 0.00352 AFIX 23 H22A 2 0.358996 1.021429 0.448735 11.00000 -1.20000 H22B 2 0.169278 1.001766 0.462096 11.00000 -1.20000 AFIX 0 C23 1 0.226666 0.958174 0.381523 11.00000 0.02298 0.01199 = 0.03663 0.00040 -0.00299 0.00420 AFIX 23 H23A 2 0.112103 0.935266 0.375264 11.00000 -1.20000 H23B 2 0.249811 1.035801 0.362611 11.00000 -1.20000 AFIX 0 H1 2 0.180384 0.268086 0.367332 11.00000 0.04093 HKLF 4 REM csj-cy-2_a.res in P2(1)2(1)2(1) REM wR2 = 0.0734, GooF = S = 1.055, Restrained GooF = 1.055 for all data REM R1 = 0.0281 for 3978 Fo > 4sig(Fo) and 0.0283 for all 4020 data REM 277 parameters refined using 0 restraints END WGHT 0.0413 0.4464 REM Highest difference peak 0.230, deepest hole -0.139, 1-sigma level 0.036 Q1 1 0.2536 0.4784 0.3228 11.00000 0.05 0.23 Q2 1 0.3555 0.7160 0.4027 11.00000 0.05 0.23 Q3 1 0.2272 0.6544 0.3976 11.00000 0.05 0.23 Q4 1 0.3656 0.6173 0.3800 11.00000 0.05 0.23 Q5 1 0.4754 0.3111 0.3597 11.00000 0.05 0.23 Q6 1 0.5049 0.5965 0.3601 11.00000 0.05 0.21 Q7 1 0.5730 0.3031 0.3998 11.00000 0.05 0.21 Q8 1 0.3851 0.3019 0.3217 11.00000 0.05 0.20 Q9 1 0.4756 0.7837 0.4163 11.00000 0.05 0.18 Q10 1 0.3819 0.4564 0.3007 11.00000 0.05 0.18 Q11 1 0.6684 0.2956 0.4437 11.00000 0.05 0.18 Q12 1 0.1317 0.5018 0.3573 11.00000 0.05 0.17 Q13 1 0.7098 0.1599 0.3631 11.00000 0.05 0.16 Q14 1 0.3778 0.5266 0.3454 11.00000 0.05 0.15 Q15 1 0.8041 0.1409 0.4013 11.00000 0.05 0.15 Q16 1 0.5919 0.2351 0.3607 11.00000 0.05 0.15 Q17 1 0.4549 0.8781 0.3629 11.00000 0.05 0.14 Q18 1 0.3996 0.3617 0.2765 11.00000 0.05 0.13 Q19 1 0.1891 0.8188 0.4558 11.00000 0.05 0.13 Q20 1 0.3294 0.6217 0.4256 11.00000 0.05 0.13 REM The information below was added by Olex2. REM REM R1 = 0.0281 for 3978 Fo > 4sig(Fo) and 0.0283 for all 9868 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.23, deepest hole -0.14 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0283 REM R1_gt = 0.0281 REM wR_ref = 0.0734 REM GOOF = 1.055 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 9868 REM Reflections_gt = 3978 REM Parameters = n/a REM Hole = -0.14 REM Peak = 0.23 REM Flack = -0.04(5) ; _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 1.478 _oxdiff_exptl_absorpt_empirical_full_min 0.658