# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_p2121212121212 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H28 O4' _chemical_formula_weight 356.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 5.4244(18) _cell_length_b 11.419(4) _cell_length_c 15.941(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.108(13) _cell_angle_gamma 90.00 _cell_volume 975.0(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 513 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 17.75 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.990 _exptl_absorpt_correction_T_max 0.993 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3170 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 20.52 _reflns_number_total 1876 _reflns_number_gt 1418 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.046(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -4(3) _refine_ls_number_reflns 1876 _refine_ls_number_parameters 242 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1498 _refine_ls_wR_factor_gt 0.1355 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4522(15) 1.3911(7) 0.7312(6) 0.101(3) Uani 1 1 d . . . H1A H 0.3027 1.3579 0.7463 0.151 Uiso 1 1 calc R . . H1B H 0.4331 1.4000 0.6707 0.151 Uiso 1 1 calc R . . H1C H 0.4823 1.4663 0.7578 0.151 Uiso 1 1 calc R . . C2 C 0.6403(13) 1.2018(5) 0.7295(4) 0.0577(17) Uani 1 1 d . . . C3 C 0.4496(13) 1.1630(6) 0.6683(4) 0.0639(18) Uani 1 1 d . . . H3 H 0.3262 1.2149 0.6443 0.077 Uiso 1 1 calc R . . C4 C 0.4405(11) 1.0448(6) 0.6420(4) 0.0558(17) Uani 1 1 d . . . C5 C 0.2368(12) 1.0070(6) 0.5731(4) 0.0607(18) Uani 1 1 d . . . H5A H 0.2074 1.0683 0.5307 0.073 Uiso 1 1 calc R . . H5B H 0.0845 0.9967 0.5970 0.073 Uiso 1 1 calc R . . C6 C 0.2955(11) 0.8936(6) 0.5303(4) 0.0568(18) Uani 1 1 d . . . H6 H 0.4409 0.9079 0.5023 0.068 Uiso 1 1 calc R . . C7 C 0.0787(13) 0.8577(7) 0.4620(4) 0.084(2) Uani 1 1 d . . . H7A H -0.0599 0.8331 0.4885 0.126 Uiso 1 1 calc R . . H7B H 0.1301 0.7942 0.4293 0.126 Uiso 1 1 calc R . . H7C H 0.0295 0.9231 0.4254 0.126 Uiso 1 1 calc R . . C8 C 0.3857(15) 0.6788(6) 0.5655(4) 0.086(2) Uani 1 1 d . . . H8A H 0.4963 0.6777 0.5240 0.128 Uiso 1 1 calc R . . H8B H 0.2223 0.6540 0.5394 0.128 Uiso 1 1 calc R . . H8C H 0.4475 0.6266 0.6112 0.128 Uiso 1 1 calc R . . C9 C 0.3712(12) 0.8042(6) 0.6004(4) 0.0561(17) Uani 1 1 d . . . H9 H 0.2429 0.8047 0.6373 0.067 Uiso 1 1 calc R . . C10 C 0.6191(11) 0.8380(5) 0.6548(4) 0.0500(17) Uani 1 1 d . . . H10 H 0.7482 0.8284 0.6188 0.060 Uiso 1 1 calc R . . C11 C 0.6191(12) 0.9684(5) 0.6791(4) 0.0494(16) Uani 1 1 d . . . C12 C 0.8171(13) 1.0098(5) 0.7412(4) 0.0556(17) Uani 1 1 d . . . H12 H 0.9404 0.9582 0.7657 0.067 Uiso 1 1 calc R . . C13 C 0.8282(12) 1.1262(6) 0.7655(4) 0.0553(18) Uani 1 1 d . . . C14 C 1.2011(14) 1.0987(7) 0.8626(5) 0.084(2) Uani 1 1 d . . . H14A H 1.2808 1.0617 0.8200 0.126 Uiso 1 1 calc R . . H14B H 1.1302 1.0399 0.8947 0.126 Uiso 1 1 calc R . . H14C H 1.3219 1.1434 0.9000 0.126 Uiso 1 1 calc R . . C15 C 0.6907(11) 0.7582(5) 0.7308(4) 0.0485(16) Uani 1 1 d . . . C16 C 0.5733(11) 0.7649(5) 0.8023(4) 0.0545(17) Uani 1 1 d . . . H16 H 0.4503 0.8212 0.8041 0.065 Uiso 1 1 calc R . . C17 C 0.6344(12) 0.6905(6) 0.8703(4) 0.0568(16) Uani 1 1 d . . . C18 C 0.8175(12) 0.6049(6) 0.8677(5) 0.0582(18) Uani 1 1 d . . . C19 C 0.9360(12) 0.5990(6) 0.7986(5) 0.0643(19) Uani 1 1 d . . . H19 H 1.0601 0.5432 0.7971 0.077 Uiso 1 1 calc R . . C20 C 0.8747(12) 0.6749(6) 0.7305(4) 0.0609(18) Uani 1 1 d . . . H20 H 0.9587 0.6695 0.6841 0.073 Uiso 1 1 calc R . . C21 C 0.3588(13) 0.7833(7) 0.9535(4) 0.080(2) Uani 1 1 d . . . H21A H 0.2137 0.7778 0.9106 0.121 Uiso 1 1 calc R . . H21B H 0.4387 0.8575 0.9490 0.121 Uiso 1 1 calc R . . H21C H 0.3100 0.7764 1.0086 0.121 Uiso 1 1 calc R . . C22 C 1.0660(14) 0.4510(6) 0.9398(5) 0.090(3) Uani 1 1 d . . . H22A H 1.2180 0.4907 0.9335 0.135 Uiso 1 1 calc R . . H22B H 1.0238 0.3963 0.8940 0.135 Uiso 1 1 calc R . . H22C H 1.0884 0.4098 0.9929 0.135 Uiso 1 1 calc R . . O1 O 0.6574(9) 1.3158(4) 0.7591(3) 0.0859(16) Uani 1 1 d . . . O2 O 1.0106(9) 1.1735(4) 0.8234(3) 0.0745(13) Uani 1 1 d . . . O3 O 0.5285(8) 0.6911(4) 0.9421(3) 0.0746(14) Uani 1 1 d . . . O4 O 0.8695(8) 0.5345(4) 0.9381(3) 0.0764(14) Uani 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 C1 0.087(6) 0.049(5) 0.153(8) -0.008(5) -0.019(5) 0.013(5) C2 0.069(5) 0.040(4) 0.062(4) -0.011(4) 0.007(4) 0.000(4) C3 0.063(5) 0.055(5) 0.070(4) 0.002(4) -0.003(4) 0.004(4) C4 0.057(4) 0.052(5) 0.055(4) 0.006(4) -0.001(4) -0.003(4) C5 0.057(4) 0.061(5) 0.060(4) 0.001(4) -0.001(4) -0.003(4) C6 0.058(4) 0.062(4) 0.049(4) -0.007(4) 0.001(3) -0.005(4) C7 0.084(5) 0.095(6) 0.066(5) -0.026(4) -0.010(4) -0.004(4) C8 0.105(6) 0.063(5) 0.083(5) -0.016(5) -0.005(4) -0.007(5) C9 0.060(4) 0.055(4) 0.052(4) -0.008(4) 0.007(3) -0.009(3) C10 0.043(4) 0.043(4) 0.064(4) -0.011(4) 0.012(3) -0.004(3) C11 0.051(4) 0.051(4) 0.045(4) -0.004(3) 0.006(3) -0.004(4) C12 0.067(5) 0.043(5) 0.055(4) 0.003(3) 0.007(4) 0.000(3) C13 0.045(4) 0.052(5) 0.065(4) 0.000(4) -0.006(3) -0.004(4) C14 0.076(5) 0.087(6) 0.080(5) -0.001(5) -0.015(4) -0.011(5) C15 0.051(4) 0.038(4) 0.057(4) -0.004(3) 0.011(3) 0.000(3) C16 0.054(4) 0.053(4) 0.056(4) 0.000(4) 0.007(3) 0.009(3) C17 0.059(4) 0.053(4) 0.060(4) 0.004(4) 0.013(3) 0.008(4) C18 0.059(4) 0.054(5) 0.062(5) 0.005(4) 0.009(4) 0.003(4) C19 0.062(5) 0.054(4) 0.077(5) 0.000(4) 0.016(4) 0.008(4) C20 0.068(5) 0.050(4) 0.068(5) -0.003(4) 0.022(4) -0.002(4) C21 0.070(5) 0.098(6) 0.077(5) -0.001(4) 0.023(4) 0.025(5) C22 0.079(6) 0.070(5) 0.121(7) 0.034(5) 0.019(5) 0.031(5) O1 0.087(4) 0.056(3) 0.104(4) -0.016(3) -0.019(3) 0.003(3) O2 0.069(3) 0.061(3) 0.084(3) -0.012(3) -0.020(3) 0.002(3) O3 0.083(3) 0.083(3) 0.063(3) 0.012(3) 0.027(3) 0.026(3) O4 0.084(3) 0.066(3) 0.081(3) 0.020(3) 0.019(3) 0.021(3) _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 C1 O1 1.421(8) . ? C2 C3 1.378(8) . ? C2 O1 1.383(7) . ? C2 C13 1.389(8) . ? C3 C4 1.412(9) . ? C4 C11 1.367(8) . ? C4 C5 1.492(8) . ? C5 C6 1.520(8) . ? C6 C9 1.521(8) . ? C6 C7 1.527(8) . ? C8 C9 1.543(9) . ? C9 C10 1.530(8) . ? C10 C15 1.517(8) . ? C10 C11 1.538(8) . ? C11 C12 1.421(8) . ? C12 C13 1.383(9) . ? C13 O2 1.354(7) . ? C14 O2 1.408(8) . ? C15 C20 1.379(8) . ? C15 C16 1.393(8) . ? C16 C17 1.375(8) . ? C17 O3 1.359(7) . ? C17 C18 1.399(9) . ? C18 C19 1.362(8) . ? C18 O4 1.373(7) . ? C19 C20 1.388(9) . ? C21 O3 1.429(7) . ? C22 O4 1.428(7) . ? 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 C3 C2 O1 123.1(6) . . ? C3 C2 C13 120.9(6) . . ? O1 C2 C13 116.0(6) . . ? C2 C3 C4 120.3(6) . . ? C11 C4 C3 119.5(6) . . ? C11 C4 C5 121.7(6) . . ? C3 C4 C5 118.8(6) . . ? C4 C5 C6 113.2(5) . . ? C5 C6 C9 107.0(5) . . ? C5 C6 C7 110.9(5) . . ? C9 C6 C7 115.6(5) . . ? C6 C9 C10 111.0(5) . . ? C6 C9 C8 112.4(5) . . ? C10 C9 C8 110.4(6) . . ? C15 C10 C9 113.1(5) . . ? C15 C10 C11 113.0(5) . . ? C9 C10 C11 110.6(5) . . ? C4 C11 C12 119.6(5) . . ? C4 C11 C10 122.5(5) . . ? C12 C11 C10 117.9(6) . . ? C13 C12 C11 120.7(6) . . ? O2 C13 C12 124.7(6) . . ? O2 C13 C2 116.3(6) . . ? C12 C13 C2 119.0(6) . . ? C20 C15 C16 117.7(6) . . ? C20 C15 C10 120.4(6) . . ? C16 C15 C10 121.9(6) . . ? C17 C16 C15 121.8(6) . . ? O3 C17 C16 125.4(6) . . ? O3 C17 C18 115.1(6) . . ? C16 C17 C18 119.5(6) . . ? C19 C18 O4 124.8(6) . . ? C19 C18 C17 119.1(6) . . ? O4 C18 C17 116.1(6) . . ? C18 C19 C20 121.1(6) . . ? C15 C20 C19 120.8(6) . . ? C2 O1 C1 117.2(5) . . ? C13 O2 C14 117.8(5) . . ? C17 O3 C21 118.5(5) . . ? C18 O4 C22 117.5(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 20.52 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.175 _refine_diff_density_min -0.145 _refine_diff_density_rms 0.042 _database_code_depnum_ccdc_archive 'CCDC 953122' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_zhangjj0607_twin1_hklf4 _audit_creation_date 2013-06-14 _audit_creation_method ; Olex2 1.2 (compiled Apr 23 2013 17:54:37, GUI svn.r4466) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C22 H26 O6), O' _chemical_formula_sum 'C44 H52 O13' _chemical_formula_weight 788.85 _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' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.1666(8) _cell_length_b 12.3232(10) _cell_length_c 20.795(2) _cell_angle_alpha 85.685(8) _cell_angle_beta 80.440(8) _cell_angle_gamma 89.993(7) _cell_volume 2057.7(3) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1201 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 70.7470 _cell_measurement_theta_min 4.0660 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76996 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light colourless' _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 840 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.02 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0886 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 9890 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 68.251 _diffrn_reflns_theta_min 4.054 _diffrn_ambient_temperature 150.00(10) _diffrn_detector_area_resol_mean 16.0733 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -82.00 -36.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 178.0000 -30.0000 46 #__ type_ start__ end____ width___ exp.time_ 2 omega -78.00 -45.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 178.0000 -90.0000 33 #__ type_ start__ end____ width___ exp.time_ 3 omega -21.00 29.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -150.0000 50 #__ type_ start__ end____ width___ exp.time_ 4 omega 40.00 70.00 1.0000 6.0000 omega____ theta____ kappa____ phi______ frames - 0.0000 57.0000 -150.0000 30 #__ type_ start__ end____ width___ exp.time_ 5 omega -42.00 -11.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -42.5000 38.0000 0.0000 31 #__ type_ start__ end____ width___ exp.time_ 6 omega 32.00 125.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 77.0000 -180.0000 93 #__ type_ start__ end____ width___ exp.time_ 7 omega -17.00 69.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -38.0000 60.0000 86 #__ type_ start__ end____ width___ exp.time_ 8 omega 45.00 87.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -125.0000 150.0000 42 #__ type_ start__ end____ width___ exp.time_ 9 omega 5.00 101.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -99.0000 -120.0000 96 #__ type_ start__ end____ width___ exp.time_ 10 omega 9.00 79.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -57.0000 -30.0000 70 #__ type_ start__ end____ width___ exp.time_ 11 omega -20.00 110.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 56.0000 -19.0000 -150.0000 130 #__ type_ start__ end____ width___ exp.time_ 12 omega 73.00 109.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -63.0000 -60.0000 36 #__ type_ start__ end____ width___ exp.time_ 13 omega 94.00 124.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -63.0000 60.0000 30 #__ type_ start__ end____ width___ exp.time_ 14 omega 114.00 141.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -91.0000 -60.0000 27 #__ type_ start__ end____ width___ exp.time_ 15 omega 69.00 110.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -111.0000 -150.0000 41 #__ type_ start__ end____ width___ exp.time_ 16 omega 52.00 105.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -111.0000 0.0000 53 #__ type_ start__ end____ width___ exp.time_ 17 omega 49.00 74.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -63.0000 60.0000 25 #__ type_ start__ end____ width___ exp.time_ 18 omega 47.00 106.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 12.0000 -60.0000 59 #__ type_ start__ end____ width___ exp.time_ 19 omega 39.00 114.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -111.0000 150.0000 75 #__ type_ start__ end____ width___ exp.time_ 20 omega 152.00 177.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 38.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 21 omega 80.00 106.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 77.0000 120.0000 26 #__ type_ start__ end____ width___ exp.time_ 22 omega 95.00 144.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 38.0000 90.0000 49 #__ type_ start__ end____ width___ exp.time_ 23 omega 89.00 168.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 63.0000 -120.0000 79 #__ type_ start__ end____ width___ exp.time_ 24 omega 90.00 177.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 63.0000 0.0000 87 #__ type_ start__ end____ width___ exp.time_ 25 omega 106.00 135.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 178.0000 120.0000 29 #__ type_ start__ end____ width___ exp.time_ 26 omega 55.00 97.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 -180.0000 42 #__ type_ start__ end____ width___ exp.time_ 27 omega 67.00 114.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -111.0000 -90.0000 47 #__ type_ start__ end____ width___ exp.time_ 28 omega 104.00 148.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 25.0000 0.0000 44 #__ type_ start__ end____ width___ exp.time_ 29 omega 96.00 123.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -91.0000 30.0000 27 #__ type_ start__ end____ width___ exp.time_ 30 omega 43.00 93.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -38.0000 60.0000 50 #__ type_ start__ end____ width___ exp.time_ 31 omega 55.00 92.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -38.0000 -30.0000 37 #__ type_ start__ end____ width___ exp.time_ 32 omega 97.00 124.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 38.0000 -180.0000 27 #__ type_ start__ end____ width___ exp.time_ 33 omega 143.00 171.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 12.0000 -60.0000 28 #__ type_ start__ end____ width___ exp.time_ 34 omega 109.00 134.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 111.0000 -180.0000 25 #__ type_ start__ end____ width___ exp.time_ 35 omega 88.00 178.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 63.0000 -60.0000 90 #__ type_ start__ end____ width___ exp.time_ 36 omega 62.00 87.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -50.0000 -30.0000 25 #__ type_ start__ end____ width___ exp.time_ 37 omega 39.00 74.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -38.0000 150.0000 35 #__ type_ start__ end____ width___ exp.time_ 38 omega 133.00 168.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 111.0000 -150.0000 35 #__ type_ start__ end____ width___ exp.time_ 39 omega 61.00 86.00 1.0000 18.0000 omega____ theta____ kappa____ phi______ frames - 112.0000 -77.0000 -180.0000 25 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0485081000 _diffrn_orient_matrix_UB_12 -0.1184553000 _diffrn_orient_matrix_UB_13 0.0247871000 _diffrn_orient_matrix_UB_21 0.1052451000 _diffrn_orient_matrix_UB_22 -0.0402635000 _diffrn_orient_matrix_UB_23 -0.0619707000 _diffrn_orient_matrix_UB_31 0.1522226000 _diffrn_orient_matrix_UB_32 -0.0079244000 _diffrn_orient_matrix_UB_33 0.0349625000 loop_ _diffrn_oxdiff_twin_id _diffrn_oxdiff_twin_ratio _diffrn_oxdiff_twin_reflns_isolated _diffrn_oxdiff_twin_reflns_overlapped 1 0.5553 3821 10928 2 0.4447 3806 10927 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5543 _reflns_number_total 9890 _reflns_special_details ; _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, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 1.065 _refine_diff_density_min -0.451 _refine_diff_density_rms 0.112 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 538 _refine_ls_number_reflns 9890 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1727 _refine_ls_R_factor_gt 0.1125 _refine_ls_restrained_S_all 1.092 _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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2977 _refine_ls_wR_factor_ref 0.3393 _refine_special_details ; Refined as a 2-component twin. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups 2. Uiso/Uaniso restraints and constraints Uanis(O14) \\sim Ueq, Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 3. Others Fixed Sof: O14(0.5) O13(0.5) 4.a Ternary CH refined with riding coordinates: C4(H4), C24(H24), C25(H25), C3(H3) 4.b Aromatic/amide H refined with riding coordinates: C6(H6), C42(H42), C38(H38), C9(H9), C30(H30), C27(H27), C20(H20), C16(H16), C19(H19), C39(H39) 4.c Idealised Me refined as rotating group: C33(H33A,H33B,H33C), C36(H36A,H36B,H36C), C11(H11A,H11B,H11C), C14(H14A,H14B, H14C), C34(H34A,H34B,H34C), C43(H43A,H43B,H43C), C13(H13A,H13B,H13C), C12(H12A, H12B,H12C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C44(H44A,H44B,H44C), C35(H35A,H35B,H35C) 4.d Idealised tetrahedral OH refined as rotating group: O7(H7), O2(H2) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _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 O9 O 0.5438(7) 0.5865(4) 0.1728(2) 0.0352(13) Uani 1 1 d . . . . . O8 O 0.8464(7) 0.9190(4) 0.0388(3) 0.0362(13) Uani 1 1 d . . . . . O1 O 0.3475(6) 0.5719(4) 0.0403(3) 0.0349(13) Uani 1 1 d . . . . . O7 O 0.8607(6) 1.1343(4) 0.0496(3) 0.0359(13) Uani 1 1 d . . . . . H7 H 0.9191 1.0933 0.0266 0.054 Uiso 1 1 calc R U . . . O2 O 0.3606(6) 0.3549(4) 0.0502(3) 0.0366(13) Uani 1 1 d . . . . . H2 H 0.4283 0.4027 0.0341 0.055 Uiso 1 1 calc R U . . . O10 O 0.3619(6) 0.6650(4) 0.2713(2) 0.0352(12) Uani 1 1 d . . . . . O11 O 0.8624(7) 1.0063(5) 0.3863(3) 0.0429(14) Uani 1 1 d . . . . . O3 O 0.0434(6) 0.8691(4) 0.1731(2) 0.0345(12) Uani 1 1 d . . . . . O4 O -0.1390(7) 0.7680(4) 0.2717(2) 0.0356(13) Uani 1 1 d . . . . . O12 O 0.6316(7) 1.1041(5) 0.4628(3) 0.0414(13) Uani 1 1 d . . . . . O6 O 0.1368(8) 0.2668(5) 0.4601(3) 0.0454(14) Uani 1 1 d . . . . . O5 O 0.3659(7) 0.3877(5) 0.3857(3) 0.0409(13) Uani 1 1 d . . . . . C23 C 0.7172(9) 1.0758(6) 0.0843(4) 0.0295(16) Uani 1 1 d . . . . . C31 C 0.6441(8) 0.8816(5) 0.1338(4) 0.0267(16) Uani 1 1 d . . . . . C15 C 0.0656(9) 0.3719(6) 0.2728(4) 0.0310(17) Uani 1 1 d . . . . . C4 C 0.0531(9) 0.4066(5) 0.2021(3) 0.0267(15) Uani 1 1 d . . . . . H4 H -0.0524 0.3781 0.1934 0.032 Uiso 1 1 calc R U . . . C17 C 0.2284(9) 0.3664(6) 0.3597(4) 0.0326(17) Uani 1 1 d . . . . . C5 C 0.0506(8) 0.5308(6) 0.1905(4) 0.0273(16) Uani 1 1 d . . . . . C29 C 0.5516(8) 0.6975(5) 0.1736(4) 0.0281(16) Uani 1 1 d . . . . . C6 C -0.0463(8) 0.5899(6) 0.2375(4) 0.0279(15) Uani 1 1 d . . . . . H6 H -0.1080 0.5538 0.2745 0.033 Uiso 1 1 calc R U . . . C42 C 0.7076(9) 1.0209(5) 0.2971(4) 0.0306(17) Uani 1 1 d . . . . . H42 H 0.7898 0.9850 0.2706 0.037 Uiso 1 1 calc R U . . . C18 C 0.1044(10) 0.2991(6) 0.4004(4) 0.0356(18) Uani 1 1 d . . . . . C7 C -0.0499(9) 0.7028(6) 0.2284(4) 0.0303(16) Uani 1 1 d . . . . . C26 C 0.5525(8) 0.9217(5) 0.1892(3) 0.0249(15) Uani 1 1 d . . . . . C10 C 0.1426(9) 0.5857(6) 0.1348(3) 0.0282(16) Uani 1 1 d . . . . . C2 C 0.2187(9) 0.4031(5) 0.0861(4) 0.0274(16) Uani 1 1 d . . . . . C28 C 0.4540(9) 0.7414(6) 0.2282(3) 0.0286(16) Uani 1 1 d . . . . . C24 C 0.6942(9) 1.1061(6) 0.1548(3) 0.0290(16) Uani 1 1 d . . . . . H24 H 0.7980 1.0875 0.1707 0.035 Uiso 1 1 calc R U . . . C38 C 0.4445(9) 1.1094(6) 0.3128(4) 0.0341(17) Uani 1 1 d . . . . . H38 H 0.3510 1.1348 0.2966 0.041 Uiso 1 1 calc R U . . . C40 C 0.6007(10) 1.0893(6) 0.4010(4) 0.0347(17) Uani 1 1 d . . . . . C32 C 0.7445(9) 0.9536(6) 0.0827(4) 0.0293(16) Uani 1 1 d . . . . . C37 C 0.5677(9) 1.0574(5) 0.2723(4) 0.0286(16) Uani 1 1 d . . . . . C25 C 0.5550(9) 1.0431(6) 0.2017(4) 0.0293(16) Uani 1 1 d . . . . . H25 H 0.4490 1.0738 0.1935 0.035 Uiso 1 1 calc R U . . . C9 C 0.1424(8) 0.7001(5) 0.1279(4) 0.0283(16) Uani 1 1 d . . . . . H9 H 0.2062 0.7366 0.0915 0.034 Uiso 1 1 calc R U . . . C33 C 0.5699(9) 1.1052(6) 0.0508(4) 0.0323(17) Uani 1 1 d . . . . . H33A H 0.5578 1.1829 0.0476 0.048 Uiso 1 1 calc R U . . . H33B H 0.4709 1.0720 0.0759 0.048 Uiso 1 1 calc R U . . . H33C H 0.5877 1.0795 0.0078 0.048 Uiso 1 1 calc R U . . . C30 C 0.6443(9) 0.7681(6) 0.1261(4) 0.0297(17) Uani 1 1 d . . . . . H30 H 0.7065 0.7410 0.0893 0.036 Uiso 1 1 calc R U . . . C41 C 0.7257(9) 1.0367(6) 0.3590(4) 0.0311(16) Uani 1 1 d . . . . . C36 C 0.6570(10) 0.5404(6) 0.1217(4) 0.0375(19) Uani 1 1 d . . . . . H36A H 0.6334 0.5683 0.0799 0.056 Uiso 1 1 calc R U . . . H36B H 0.6443 0.4627 0.1259 0.056 Uiso 1 1 calc R U . . . H36C H 0.7689 0.5596 0.1253 0.056 Uiso 1 1 calc R U . . . C8 C 0.0500(9) 0.7579(6) 0.1737(4) 0.0297(16) Uani 1 1 d . . . . . C1 C 0.2458(8) 0.5262(5) 0.0842(4) 0.0271(16) Uani 1 1 d . . . . . C11 C 0.0695(9) 0.3831(6) 0.0512(4) 0.0307(17) Uani 1 1 d . . . . . H11A H 0.0889 0.4200 0.0083 0.046 Uiso 1 1 calc R U . . . H11B H -0.0297 0.4103 0.0760 0.046 Uiso 1 1 calc R U . . . H11C H 0.0566 0.3064 0.0478 0.046 Uiso 1 1 calc R U . . . C14 C 0.1565(9) 0.9284(6) 0.1225(4) 0.0330(18) Uani 1 1 d . . . . . H14A H 0.1375 0.9084 0.0806 0.050 Uiso 1 1 calc R U . . . H14B H 0.2686 0.9114 0.1276 0.050 Uiso 1 1 calc R U . . . H14C H 0.1392 1.0051 0.1254 0.050 Uiso 1 1 calc R U . . . C34 C 0.6721(9) 1.2300(6) 0.1597(4) 0.0335(18) Uani 1 1 d . . . . . H34A H 0.7584 1.2685 0.1296 0.050 Uiso 1 1 calc R U . . . H34B H 0.6783 1.2476 0.2035 0.050 Uiso 1 1 calc R U . . . H34C H 0.5659 1.2509 0.1492 0.050 Uiso 1 1 calc R U . . . C43 C 0.4988(13) 1.1534(8) 0.5045(4) 0.059(3) Uani 1 1 d . . . . . H43A H 0.4704 1.2212 0.4835 0.088 Uiso 1 1 calc R U . . . H43B H 0.5336 1.1664 0.5451 0.088 Uiso 1 1 calc R U . . . H43C H 0.4037 1.1055 0.5127 0.088 Uiso 1 1 calc R U . . . C3 C 0.1954(9) 0.3536(5) 0.1561(3) 0.0268(16) Uani 1 1 d . . . . . H3 H 0.2987 0.3667 0.1727 0.032 Uiso 1 1 calc R U . . . C27 C 0.4536(9) 0.8503(6) 0.2357(4) 0.0302(16) Uani 1 1 d . . . . . H27 H 0.3877 0.8774 0.2716 0.036 Uiso 1 1 calc R U . . . C20 C -0.0555(9) 0.3064(6) 0.3128(3) 0.0308(16) Uani 1 1 d . . . . . H20 H -0.1498 0.2853 0.2971 0.037 Uiso 1 1 calc R U . . . C13 C -0.2405(11) 0.7164(7) 0.3285(4) 0.044(2) Uani 1 1 d . . . . . H13A H -0.3267 0.6745 0.3154 0.067 Uiso 1 1 calc R U . . . H13B H -0.2893 0.7709 0.3561 0.067 Uiso 1 1 calc R U . . . H13C H -0.1735 0.6693 0.3520 0.067 Uiso 1 1 calc R U . . . C16 C 0.2065(10) 0.4012(6) 0.2968(4) 0.0334(17) Uani 1 1 d . . . . . H16 H 0.2875 0.4449 0.2703 0.040 Uiso 1 1 calc R U . . . C12 C 0.1685(10) 0.2306(6) 0.1601(4) 0.0360(18) Uani 1 1 d . . . . . H12A H 0.1750 0.2004 0.2035 0.054 Uiso 1 1 calc R U . . . H12B H 0.2525 0.1990 0.1294 0.054 Uiso 1 1 calc R U . . . H12C H 0.0610 0.2148 0.1499 0.054 Uiso 1 1 calc R U . . . C19 C -0.0347(10) 0.2728(6) 0.3764(4) 0.0368(18) Uani 1 1 d . . . . . H19 H -0.1179 0.2313 0.4031 0.044 Uiso 1 1 calc R U . . . C39 C 0.4592(10) 1.1238(6) 0.3773(4) 0.0372(18) Uani 1 1 d . . . . . H39 H 0.3742 1.1564 0.4044 0.045 Uiso 1 1 calc R U . . . C21 C 0.0223(13) 0.1863(8) 0.5004(4) 0.060(3) Uani 1 1 d . . . . . H21A H 0.0221 0.1207 0.4782 0.090 Uiso 1 1 calc R U . . . H21B H -0.0878 0.2153 0.5074 0.090 Uiso 1 1 calc R U . . . H21C H 0.0581 0.1704 0.5417 0.090 Uiso 1 1 calc R U . . . C22 C 0.5126(10) 0.4233(7) 0.3398(4) 0.046(2) Uani 1 1 d . . . . . H22A H 0.5223 0.3819 0.3021 0.068 Uiso 1 1 calc R U . . . H22B H 0.6091 0.4123 0.3602 0.068 Uiso 1 1 calc R U . . . H22C H 0.5036 0.4991 0.3268 0.068 Uiso 1 1 calc R U . . . C44 C 1.0096(10) 0.9862(7) 0.3421(4) 0.045(2) Uani 1 1 d . . . . . H44A H 1.0349 1.0479 0.3110 0.067 Uiso 1 1 calc R U . . . H44B H 0.9935 0.9229 0.3196 0.067 Uiso 1 1 calc R U . . . H44C H 1.0999 0.9743 0.3660 0.067 Uiso 1 1 calc R U . . . C35 C 0.2571(10) 0.7028(6) 0.3264(4) 0.0409(19) Uani 1 1 d . . . . . H35A H 0.1811 0.7550 0.3120 0.061 Uiso 1 1 calc R U . . . H35B H 0.3236 0.7365 0.3536 0.061 Uiso 1 1 calc R U . . . H35C H 0.1958 0.6426 0.3511 0.061 Uiso 1 1 calc R U . . . O14 O 0.765(3) 0.4883(16) 0.4784(9) 0.136(8) Uani 0.5 1 d . U P A 1 O13 O 0.924(2) 0.4555(16) 0.5229(10) 0.125(7) Uani 0.5 1 d . U P B 2 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 O9 0.044(3) 0.016(2) 0.044(3) -0.004(2) -0.001(2) 0.005(2) O8 0.038(3) 0.025(3) 0.043(3) -0.009(2) 0.002(2) 0.004(2) O1 0.031(3) 0.027(3) 0.043(3) 0.000(2) 0.004(2) 0.004(2) O7 0.033(3) 0.019(3) 0.052(4) -0.006(2) 0.005(2) 0.001(2) O2 0.031(3) 0.022(3) 0.053(4) 0.000(2) 0.004(2) 0.013(2) O10 0.041(3) 0.022(3) 0.042(3) -0.001(2) -0.004(2) 0.000(2) O11 0.040(3) 0.045(3) 0.046(3) 0.001(3) -0.015(3) 0.013(3) O3 0.038(3) 0.019(3) 0.045(3) -0.003(2) -0.003(2) 0.008(2) O4 0.042(3) 0.023(3) 0.039(3) -0.003(2) 0.004(2) 0.006(2) O12 0.042(3) 0.046(3) 0.038(3) -0.009(3) -0.010(2) 0.002(3) O6 0.067(4) 0.042(3) 0.028(3) 0.003(2) -0.011(3) -0.004(3) O5 0.041(3) 0.040(3) 0.044(3) -0.002(3) -0.014(2) 0.002(2) C23 0.022(4) 0.023(4) 0.042(5) -0.003(3) -0.001(3) 0.006(3) C31 0.026(4) 0.015(3) 0.040(4) -0.007(3) -0.006(3) 0.005(3) C15 0.033(4) 0.020(3) 0.040(5) -0.001(3) -0.006(3) 0.012(3) C4 0.028(4) 0.017(3) 0.035(4) 0.000(3) -0.006(3) 0.003(3) C17 0.034(4) 0.019(3) 0.047(5) -0.008(3) -0.010(3) 0.009(3) C5 0.021(3) 0.021(4) 0.041(4) -0.001(3) -0.010(3) 0.005(3) C29 0.023(4) 0.013(3) 0.051(5) -0.007(3) -0.009(3) 0.006(3) C6 0.025(4) 0.022(3) 0.036(4) -0.001(3) -0.003(3) 0.006(3) C42 0.032(4) 0.014(3) 0.046(5) -0.004(3) -0.007(3) 0.008(3) C18 0.055(5) 0.025(4) 0.029(4) -0.004(3) -0.010(3) 0.007(3) C7 0.030(4) 0.020(4) 0.042(5) -0.004(3) -0.009(3) 0.011(3) C26 0.029(4) 0.015(3) 0.034(4) -0.002(3) -0.011(3) 0.004(3) C10 0.027(4) 0.026(4) 0.032(4) -0.001(3) -0.004(3) 0.011(3) C2 0.030(4) 0.017(3) 0.036(4) -0.007(3) -0.007(3) 0.010(3) C28 0.027(4) 0.025(4) 0.035(4) -0.001(3) -0.008(3) 0.006(3) C24 0.024(4) 0.025(4) 0.037(4) -0.003(3) -0.003(3) 0.002(3) C38 0.031(4) 0.021(4) 0.049(5) 0.002(3) -0.004(3) 0.004(3) C40 0.042(4) 0.025(4) 0.036(4) -0.003(3) -0.003(3) 0.004(3) C32 0.028(4) 0.025(4) 0.035(4) -0.002(3) -0.007(3) 0.003(3) C37 0.032(4) 0.016(3) 0.038(4) -0.004(3) -0.007(3) 0.006(3) C25 0.025(4) 0.019(3) 0.045(5) -0.005(3) -0.009(3) 0.008(3) C9 0.023(4) 0.020(4) 0.041(4) 0.002(3) -0.005(3) 0.005(3) C33 0.039(4) 0.025(4) 0.034(4) -0.001(3) -0.010(3) 0.007(3) C30 0.026(4) 0.020(4) 0.042(5) 0.000(3) -0.006(3) 0.009(3) C41 0.030(4) 0.027(4) 0.036(4) 0.003(3) -0.009(3) 0.006(3) C36 0.039(4) 0.023(4) 0.051(5) -0.010(3) -0.005(4) 0.015(3) C8 0.034(4) 0.021(4) 0.037(4) -0.004(3) -0.013(3) 0.009(3) C1 0.024(4) 0.020(4) 0.038(4) -0.002(3) -0.008(3) 0.007(3) C11 0.033(4) 0.020(3) 0.036(4) 0.003(3) -0.001(3) 0.003(3) C14 0.036(4) 0.021(4) 0.040(5) 0.004(3) -0.003(3) 0.004(3) C34 0.035(4) 0.019(4) 0.047(5) -0.010(3) -0.006(3) 0.003(3) C43 0.092(8) 0.056(5) 0.032(5) -0.016(4) -0.017(5) 0.024(5) C3 0.027(4) 0.014(3) 0.041(4) -0.004(3) -0.008(3) 0.007(3) C27 0.024(4) 0.029(4) 0.038(4) -0.004(3) -0.006(3) 0.005(3) C20 0.032(4) 0.025(4) 0.034(4) -0.002(3) -0.005(3) 0.004(3) C13 0.053(5) 0.037(4) 0.039(5) -0.006(4) 0.007(4) 0.008(4) C16 0.041(4) 0.023(4) 0.034(4) 0.004(3) -0.001(3) 0.006(3) C12 0.038(5) 0.023(4) 0.047(5) -0.003(3) -0.008(3) 0.008(3) C19 0.041(4) 0.024(4) 0.042(5) 0.004(3) 0.000(3) 0.006(3) C39 0.045(5) 0.031(4) 0.036(5) -0.005(3) -0.008(3) 0.011(3) C21 0.075(7) 0.065(6) 0.035(5) 0.025(4) -0.009(4) -0.003(5) C22 0.029(4) 0.049(5) 0.059(6) -0.003(4) -0.012(4) -0.004(4) C44 0.043(5) 0.040(5) 0.053(6) 0.000(4) -0.016(4) 0.010(4) C35 0.050(5) 0.031(4) 0.038(5) 0.004(3) 0.001(4) -0.005(4) O14 0.231(19) 0.112(13) 0.096(12) -0.062(10) -0.098(12) 0.036(13) O13 0.089(12) 0.120(13) 0.172(15) -0.124(12) 0.009(11) -0.025(9) _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 O9 C29 1.371(8) . ? O9 C36 1.438(8) . ? O8 C32 1.230(8) . ? O1 C1 1.229(8) . ? O7 H7 0.8200 . ? O7 C23 1.433(8) . ? O2 H2 0.8200 . ? O2 C2 1.426(8) . ? O10 C28 1.381(8) . ? O10 C35 1.421(8) . ? O11 C41 1.373(8) . ? O11 C44 1.421(9) . ? O3 C8 1.370(8) . ? O3 C14 1.434(8) . ? O4 C7 1.371(8) . ? O4 C13 1.430(8) . ? O12 C40 1.376(9) . ? O12 C43 1.436(9) . ? O6 C18 1.343(9) . ? O6 C21 1.475(10) . ? O5 C17 1.359(9) . ? O5 C22 1.448(9) . ? C23 C24 1.523(10) . ? C23 C32 1.524(9) . ? C23 C33 1.517(9) . ? C31 C26 1.389(9) . ? C31 C32 1.470(10) . ? C31 C30 1.420(9) . ? C15 C4 1.518(10) . ? C15 C20 1.396(10) . ? C15 C16 1.386(10) . ? C4 H4 0.9800 . ? C4 C5 1.531(9) . ? C4 C3 1.555(9) . ? C17 C18 1.428(11) . ? C17 C16 1.385(10) . ? C5 C6 1.400(9) . ? C5 C10 1.399(10) . ? C29 C28 1.417(9) . ? C29 C30 1.389(10) . ? C6 H6 0.9300 . ? C6 C7 1.390(9) . ? C42 H42 0.9300 . ? C42 C37 1.390(9) . ? C42 C41 1.349(10) . ? C18 C19 1.363(11) . ? C7 C8 1.413(10) . ? C26 C25 1.538(9) . ? C26 C27 1.406(9) . ? C10 C9 1.406(9) . ? C10 C1 1.476(9) . ? C2 C1 1.529(9) . ? C2 C11 1.546(10) . ? C2 C3 1.517(10) . ? C28 C27 1.362(10) . ? C24 H24 0.9800 . ? C24 C25 1.537(9) . ? C24 C34 1.547(9) . ? C38 H38 0.9300 . ? C38 C37 1.389(9) . ? C38 C39 1.389(10) . ? C40 C41 1.419(10) . ? C40 C39 1.385(10) . ? C37 C25 1.512(10) . ? C25 H25 0.9800 . ? C9 H9 0.9300 . ? C9 C8 1.360(9) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C30 H30 0.9300 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C3 H3 0.9800 . ? C3 C12 1.527(9) . ? C27 H27 0.9300 . ? C20 H20 0.9300 . ? C20 C19 1.392(10) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C16 H16 0.9300 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C19 H19 0.9300 . ? C39 H39 0.9300 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? O13 O13 1.77(4) 2_766 ? 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 C29 O9 C36 115.7(6) . . ? C23 O7 H7 109.5 . . ? C2 O2 H2 109.5 . . ? C28 O10 C35 117.7(5) . . ? C41 O11 C44 116.5(6) . . ? C8 O3 C14 116.1(6) . . ? C7 O4 C13 117.9(6) . . ? C40 O12 C43 114.7(6) . . ? C18 O6 C21 117.5(7) . . ? C17 O5 C22 116.3(6) . . ? O7 C23 C24 107.1(6) . . ? O7 C23 C32 110.2(5) . . ? O7 C23 C33 108.7(6) . . ? C24 C23 C32 109.2(6) . . ? C33 C23 C24 113.2(6) . . ? C33 C23 C32 108.4(6) . . ? C26 C31 C32 121.7(6) . . ? C26 C31 C30 119.9(7) . . ? C30 C31 C32 118.3(6) . . ? C20 C15 C4 122.1(7) . . ? C16 C15 C4 118.7(7) . . ? C16 C15 C20 119.2(7) . . ? C15 C4 H4 107.6 . . ? C15 C4 C5 111.3(6) . . ? C15 C4 C3 109.3(5) . . ? C5 C4 H4 107.6 . . ? C5 C4 C3 113.1(6) . . ? C3 C4 H4 107.6 . . ? O5 C17 C18 115.9(7) . . ? O5 C17 C16 124.4(7) . . ? C16 C17 C18 119.6(7) . . ? C6 C5 C4 118.5(6) . . ? C10 C5 C4 121.8(6) . . ? C10 C5 C6 119.7(6) . . ? O9 C29 C28 115.5(6) . . ? O9 C29 C30 125.7(6) . . ? C30 C29 C28 118.8(6) . . ? C5 C6 H6 120.2 . . ? C7 C6 C5 119.7(7) . . ? C7 C6 H6 120.2 . . ? C37 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C41 C42 C37 121.0(7) . . ? O6 C18 C17 115.9(7) . . ? O6 C18 C19 125.5(8) . . ? C19 C18 C17 118.6(7) . . ? O4 C7 C6 124.2(7) . . ? O4 C7 C8 115.5(6) . . ? C6 C7 C8 120.2(6) . . ? C31 C26 C25 122.1(6) . . ? C31 C26 C27 119.7(6) . . ? C27 C26 C25 118.2(6) . . ? C5 C10 C9 119.6(6) . . ? C5 C10 C1 121.3(6) . . ? C9 C10 C1 119.0(6) . . ? O2 C2 C1 109.6(6) . . ? O2 C2 C11 107.6(6) . . ? O2 C2 C3 108.1(5) . . ? C1 C2 C11 107.6(6) . . ? C3 C2 C1 110.3(6) . . ? C3 C2 C11 113.6(6) . . ? O10 C28 C29 114.2(6) . . ? C27 C28 O10 124.4(6) . . ? C27 C28 C29 121.3(7) . . ? C23 C24 H24 106.4 . . ? C23 C24 C25 115.0(6) . . ? C23 C24 C34 111.9(6) . . ? C25 C24 H24 106.4 . . ? C25 C24 C34 110.2(6) . . ? C34 C24 H24 106.4 . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C39 C38 C37 120.9(7) . . ? O12 C40 C41 116.6(7) . . ? O12 C40 C39 124.6(7) . . ? C39 C40 C41 118.8(7) . . ? O8 C32 C23 119.5(7) . . ? O8 C32 C31 122.7(6) . . ? C31 C32 C23 117.8(6) . . ? C42 C37 C25 119.6(6) . . ? C38 C37 C42 118.9(7) . . ? C38 C37 C25 121.4(7) . . ? C26 C25 H25 107.5 . . ? C24 C25 C26 111.9(6) . . ? C24 C25 H25 107.5 . . ? C37 C25 C26 110.8(6) . . ? C37 C25 C24 111.3(6) . . ? C37 C25 H25 107.5 . . ? C10 C9 H9 119.6 . . ? C8 C9 C10 120.8(7) . . ? C8 C9 H9 119.6 . . ? C23 C33 H33A 109.5 . . ? C23 C33 H33B 109.5 . . ? C23 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C30 H30 120.0 . . ? C29 C30 C31 119.9(7) . . ? C29 C30 H30 120.0 . . ? O11 C41 C40 114.8(7) . . ? C42 C41 O11 124.5(7) . . ? C42 C41 C40 120.7(7) . . ? O9 C36 H36A 109.5 . . ? O9 C36 H36B 109.5 . . ? O9 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O3 C8 C7 114.2(6) . . ? C9 C8 O3 126.0(7) . . ? C9 C8 C7 119.8(7) . . ? O1 C1 C10 122.7(6) . . ? O1 C1 C2 119.7(6) . . ? C10 C1 C2 117.6(6) . . ? C2 C11 H11A 109.5 . . ? C2 C11 H11B 109.5 . . ? C2 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O3 C14 H14A 109.5 . . ? O3 C14 H14B 109.5 . . ? O3 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C24 C34 H34A 109.5 . . ? C24 C34 H34B 109.5 . . ? C24 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O12 C43 H43A 109.5 . . ? O12 C43 H43B 109.5 . . ? O12 C43 H43C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C4 C3 H3 107.1 . . ? C2 C3 C4 113.3(5) . . ? C2 C3 H3 107.1 . . ? C2 C3 C12 111.9(6) . . ? C12 C3 C4 110.0(6) . . ? C12 C3 H3 107.1 . . ? C26 C27 H27 119.9 . . ? C28 C27 C26 120.2(7) . . ? C28 C27 H27 119.9 . . ? C15 C20 H20 120.1 . . ? C19 C20 C15 119.9(7) . . ? C19 C20 H20 120.1 . . ? O4 C13 H13A 109.5 . . ? O4 C13 H13B 109.5 . . ? O4 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C16 H16 119.5 . . ? C17 C16 C15 121.0(7) . . ? C17 C16 H16 119.5 . . ? C3 C12 H12A 109.5 . . ? C3 C12 H12B 109.5 . . ? C3 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C19 C20 121.7(7) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C38 C39 H39 120.1 . . ? C40 C39 C38 119.8(7) . . ? C40 C39 H39 120.1 . . ? O6 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? O6 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O5 C22 H22A 109.5 . . ? O5 C22 H22B 109.5 . . ? O5 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O11 C44 H44A 109.5 . . ? O11 C44 H44B 109.5 . . ? O11 C44 H44C 109.5 . . ? H44A C44 H44B 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O10 C35 H35A 109.5 . . ? O10 C35 H35B 109.5 . . ? O10 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O9 C29 C28 O10 -1.8(9) . . . . ? O9 C29 C28 C27 178.6(6) . . . . ? O9 C29 C30 C31 -178.6(7) . . . . ? O7 C23 C24 C25 -174.6(5) . . . . ? O7 C23 C24 C34 58.7(7) . . . . ? O7 C23 C32 O8 -23.3(10) . . . . ? O7 C23 C32 C31 157.7(6) . . . . ? O2 C2 C1 O1 21.8(9) . . . . ? O2 C2 C1 C10 -160.1(6) . . . . ? O2 C2 C3 C4 175.0(6) . . . . ? O2 C2 C3 C12 -60.0(8) . . . . ? O10 C28 C27 C26 179.7(6) . . . . ? O4 C7 C8 O3 0.7(9) . . . . ? O4 C7 C8 C9 -179.7(7) . . . . ? O12 C40 C41 O11 0.5(10) . . . . ? O12 C40 C41 C42 -178.6(7) . . . . ? O12 C40 C39 C38 176.8(7) . . . . ? O6 C18 C19 C20 -177.4(7) . . . . ? O5 C17 C18 O6 1.3(9) . . . . ? O5 C17 C18 C19 -178.5(6) . . . . ? O5 C17 C16 C15 177.0(7) . . . . ? C23 C24 C25 C26 41.6(8) . . . . ? C23 C24 C25 C37 166.1(6) . . . . ? C31 C26 C25 C24 -11.9(9) . . . . ? C31 C26 C25 C37 -136.7(7) . . . . ? C31 C26 C27 C28 3.4(11) . . . . ? C15 C4 C5 C6 -42.6(9) . . . . ? C15 C4 C5 C10 137.1(7) . . . . ? C15 C4 C3 C2 -166.6(6) . . . . ? C15 C4 C3 C12 67.4(8) . . . . ? C15 C20 C19 C18 -2.2(11) . . . . ? C4 C15 C20 C19 177.2(6) . . . . ? C4 C15 C16 C17 -176.3(6) . . . . ? C4 C5 C6 C7 179.5(7) . . . . ? C4 C5 C10 C9 -177.0(7) . . . . ? C4 C5 C10 C1 0.5(11) . . . . ? C17 C18 C19 C20 2.4(11) . . . . ? C5 C4 C3 C2 -42.0(8) . . . . ? C5 C4 C3 C12 -168.0(6) . . . . ? C5 C6 C7 O4 -179.2(7) . . . . ? C5 C6 C7 C8 -3.1(11) . . . . ? C5 C10 C9 C8 -1.9(11) . . . . ? C5 C10 C1 O1 -168.2(7) . . . . ? C5 C10 C1 C2 13.8(10) . . . . ? C29 C28 C27 C26 -0.7(11) . . . . ? C6 C5 C10 C9 2.7(11) . . . . ? C6 C5 C10 C1 -179.8(7) . . . . ? C6 C7 C8 O3 -175.7(7) . . . . ? C6 C7 C8 C9 3.9(11) . . . . ? C42 C37 C25 C26 62.9(8) . . . . ? C42 C37 C25 C24 -62.2(8) . . . . ? C18 C17 C16 C15 0.1(10) . . . . ? C26 C31 C32 O8 168.1(7) . . . . ? C26 C31 C32 C23 -12.9(11) . . . . ? C26 C31 C30 C29 0.7(11) . . . . ? C10 C5 C6 C7 -0.2(11) . . . . ? C10 C9 C8 O3 178.2(7) . . . . ? C10 C9 C8 C7 -1.4(11) . . . . ? C28 C29 C30 C31 1.9(11) . . . . ? C24 C23 C32 O8 -140.7(7) . . . . ? C24 C23 C32 C31 40.3(9) . . . . ? C38 C37 C25 C26 -119.0(7) . . . . ? C38 C37 C25 C24 115.8(7) . . . . ? C32 C23 C24 C25 -55.3(8) . . . . ? C32 C23 C24 C34 178.0(6) . . . . ? C32 C31 C26 C25 -2.2(11) . . . . ? C32 C31 C26 C27 177.7(7) . . . . ? C32 C31 C30 C29 179.7(6) . . . . ? C37 C42 C41 O11 -177.8(7) . . . . ? C37 C42 C41 C40 1.2(11) . . . . ? C37 C38 C39 C40 2.2(11) . . . . ? C25 C26 C27 C28 -176.7(6) . . . . ? C9 C10 C1 O1 9.3(11) . . . . ? C9 C10 C1 C2 -168.7(6) . . . . ? C33 C23 C24 C25 65.7(8) . . . . ? C33 C23 C24 C34 -61.1(8) . . . . ? C33 C23 C32 O8 95.5(8) . . . . ? C33 C23 C32 C31 -83.5(8) . . . . ? C30 C31 C26 C25 176.8(6) . . . . ? C30 C31 C26 C27 -3.3(10) . . . . ? C30 C31 C32 O8 -10.8(11) . . . . ? C30 C31 C32 C23 168.1(7) . . . . ? C30 C29 C28 O10 177.7(6) . . . . ? C30 C29 C28 C27 -1.9(11) . . . . ? C41 C42 C37 C38 -1.0(11) . . . . ? C41 C42 C37 C25 177.1(7) . . . . ? C41 C40 C39 C38 -2.0(11) . . . . ? C36 O9 C29 C28 -173.0(6) . . . . ? C36 O9 C29 C30 7.6(10) . . . . ? C1 C10 C9 C8 -179.5(7) . . . . ? C1 C2 C3 C4 55.2(8) . . . . ? C1 C2 C3 C12 -179.8(6) . . . . ? C11 C2 C1 O1 -94.9(8) . . . . ? C11 C2 C1 C10 83.1(8) . . . . ? C11 C2 C3 C4 -65.7(7) . . . . ? C11 C2 C3 C12 59.3(8) . . . . ? C14 O3 C8 C7 173.3(6) . . . . ? C14 O3 C8 C9 -6.2(11) . . . . ? C34 C24 C25 C26 169.1(6) . . . . ? C34 C24 C25 C37 -66.3(8) . . . . ? C43 O12 C40 C41 -177.4(7) . . . . ? C43 O12 C40 C39 3.8(11) . . . . ? C3 C4 C5 C6 -166.1(6) . . . . ? C3 C4 C5 C10 13.5(10) . . . . ? C3 C2 C1 O1 140.7(7) . . . . ? C3 C2 C1 C10 -41.2(8) . . . . ? C27 C26 C25 C24 168.2(6) . . . . ? C27 C26 C25 C37 43.4(8) . . . . ? C20 C15 C4 C5 120.5(7) . . . . ? C20 C15 C4 C3 -113.9(7) . . . . ? C20 C15 C16 C17 0.1(10) . . . . ? C13 O4 C7 C6 -2.9(11) . . . . ? C13 O4 C7 C8 -179.1(7) . . . . ? C16 C15 C4 C5 -63.2(8) . . . . ? C16 C15 C4 C3 62.4(8) . . . . ? C16 C15 C20 C19 0.9(10) . . . . ? C16 C17 C18 O6 178.5(6) . . . . ? C16 C17 C18 C19 -1.3(10) . . . . ? C39 C38 C37 C42 -0.7(11) . . . . ? C39 C38 C37 C25 -178.8(7) . . . . ? C39 C40 C41 O11 179.4(7) . . . . ? C39 C40 C41 C42 0.3(11) . . . . ? C21 O6 C18 C17 -172.5(7) . . . . ? C21 O6 C18 C19 7.3(11) . . . . ? C22 O5 C17 C18 160.2(6) . . . . ? C22 O5 C17 C16 -16.8(10) . . . . ? C44 O11 C41 C42 18.6(11) . . . . ? C44 O11 C41 C40 -160.4(7) . . . . ? C35 O10 C28 C29 -178.3(6) . . . . ? C35 O10 C28 C27 1.3(10) . . . . ? _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _shelx_hkl_checksum 14225 _shelx_hkl_file ; 0 0 -2 53421.5 536.299 -2 0 0 2 53421.5 536.299 1 0 0 -3 62267.8 707.337 -2 0 0 3 62267.8 707.337 1 0 0 -4 41439.9 464.917 -2 0 0 4 41439.9 464.917 1 0 0 -5 45980.7 546.612 -2 0 0 5 45980.7 546.612 1 0 0 -6 95789.2 847.556 -2 0 0 6 95789.2 847.556 1 0 0 -7 25991.9 409.628 -2 0 0 7 25991.9 409.628 1 0 0 -8 1864.66 173.217 -2 0 0 8 1864.66 173.217 1 0 0 -9 205725. 1439.02 -2 0 0 9 205725. 1439.02 1 0 0 -10 13242.5 488.805 -2 0 0 10 13242.5 488.805 1 0 0 -11 1707.98 278.810 -2 0 0 11 1707.98 278.810 1 0 0 -12 16926.7 611.528 -2 0 0 12 16926.7 611.528 1 0 0 -13-182.899 290.429 -2 0 0 13-182.899 290.429 1 0 0 -14 12582.9 602.779 -2 0 0 14 12582.9 602.779 1 0 0 -15 251.023 344.453 -2 0 0 15 251.023 344.453 1 0 0 -16-177.698 555.606 -2 0 0 16-177.698 555.606 1 0 0 -17-36.6888 463.560 -2 0 0 17-36.6888 463.560 1 0 0 -18 4847.04 525.627 -2 0 0 18 4847.04 525.627 1 0 0 -19 3010.62 656.652 -2 0 0 19 3010.62 656.652 1 0 0 24 2946.32 477.601 -2 0 0 -24 2946.32 477.601 1 0 0 25 3287.29 383.170 -2 0 0 -25 3287.29 383.170 1 0 1 -24 780.325 390.816 1 0 1 -23 756.297 466.413 1 0 -1 17 1035.75 687.421 1 0 -1 -17 2518.20 867.972 -2 0 -1 17 2518.20 867.972 1 0 -1 16 320.541 548.468 1 0 -1 -16 1217.39 957.886 -2 0 -1 16 1217.39 957.886 1 0 -1 -15-42.6554 515.878 -2 0 -1 15-42.6554 515.878 1 0 -1 -14 6327.46 555.846 -2 0 -1 14 6327.46 555.846 1 0 -1 -13 9831.71 591.688 -2 0 -1 13 9831.71 591.688 1 0 -1 -12 24656.7 768.029 -2 0 -1 12 24656.7 768.029 1 0 -1 -11 6635.41 457.051 -2 0 -1 11 6635.41 457.051 1 0 -1 -10 37093.2 790.005 -2 0 -1 10 37093.2 790.005 1 0 -1 -9 5919.76 391.269 -2 0 -1 9 5919.76 391.269 1 0 -1 8 9454.42 614.958 1 0 -1 -8 16068.3 457.672 -2 0 -1 8 16068.3 457.672 1 0 -1 7 9480.98 294.524 1 0 -1 -7 16328.6 428.003 -2 0 -1 7 16328.6 428.003 1 0 -1 6 13594.9 330.354 1 0 -1 5 6854.56 265.806 1 0 -1 4 322.688 112.161 1 0 -1 3 159318. 682.568 1 0 1 -2 62651.3 428.076 1 0 1 -1 3267.72 158.684 1 0 1 0 268.725 93.0582 1 0 1 1 1629.58 152.545 1 0 1 -2 111738. 1102.76 -2 0 1 2 111738. 1102.76 1 0 1 -3 167810. 1480.51 -2 0 1 3 167810. 1480.51 1 0 -1 -4 22144.8 286.428 1 0 1 -4 26223.3 542.741 -2 0 1 4 26223.3 542.741 1 0 1 5 999.799 243.703 1 0 1 -5 5536.67 398.361 -2 0 1 5 5536.67 398.361 1 0 1 6 19515.6 641.625 1 0 1 -6 31658.6 777.622 -2 0 1 6 31658.6 777.622 1 0 1 7 7117.91 452.821 1 0 1 -7 15697.6 451.475 -2 0 1 7 15697.6 451.475 1 0 1 8 7326.49 301.769 1 0 1 -8 13643.6 461.784 -2 0 1 8 13643.6 461.784 1 0 1 9 32.7689 258.532 1 0 1 -9 3788.48 345.418 -2 0 1 9 3788.48 345.418 1 0 1 -10 40218.3 809.767 -2 0 1 10 40218.3 809.767 1 0 1 11 2445.75 422.900 1 0 1 -11 6656.84 624.741 -2 0 1 11 6656.84 624.741 1 0 1 -12 21302.9 712.311 -2 0 1 12 21302.9 712.311 1 0 1 -13 8625.93 782.642 -2 0 1 13 8625.93 782.642 1 0 1 -14 6464.62 740.801 -2 0 1 14 6464.62 740.801 1 0 1 -15-255.997 632.339 -2 0 1 15-255.997 632.339 1 0 1 16 1230.25 514.316 1 0 1 17 1303.72 648.782 1 0 1 -17 2593.48 938.220 -2 0 1 17 2593.48 938.220 1 0 1 18 891.899 750.046 1 0 1 -18 6821.39 918.050 -2 0 1 18 6821.39 918.050 1 0 1 -19 16180.7 1088.07 -2 0 1 19 16180.7 1088.07 1 0 1 20 3063.67 630.672 1 0 -1 -24 370.031 393.460 1 0 -1 -25 160.474 276.201 1 0 2 -24 15.8986 348.339 1 0 2 -23 1892.91 511.863 1 0 2 -22 426.825 497.790 1 0 2 -21 735.124 503.357 1 0 -2 17 822.567 729.504 1 0 -2 16 371.325 579.279 1 0 -2 15 307.258 388.378 1 0 -2 14 1108.84 328.447 1 0 -2 13 698.794 289.438 1 0 -2 12 5865.87 426.144 1 0 -2 11 994.414 258.289 1 0 -2 10 11510.3 699.916 1 0 -2 9 1802.27 260.509 1 0 -2 8 2035.82 228.031 1 0 -2 7 9171.59 413.769 1 0 -2 6 20699.0 473.431 1 0 2 -4 10436.6 389.413 1 0 2 -3 8435.82 347.919 1 0 -2 2 28529.2 361.366 1 0 -2 1 8374.36 358.176 1 0 2 0 9463.73 395.453 1 0 2 1 3207.66 284.197 1 0 2 2 31728.4 752.223 1 0 2 3 8556.94 452.991 1 0 2 4 786.719 272.745 1 0 2 5 7057.48 472.098 1 0 2 6 166.687 62.3643 1 0 2 7 31002.0 463.813 1 0 2 8 1443.47 173.957 1 0 2 9 1838.94 214.142 1 0 2 10 6707.60 525.960 1 0 2 11 7985.81 602.992 1 0 2 12 577.013 339.671 1 0 2 13 5190.09 576.798 1 0 2 14 260.756 401.617 1 0 2 15 957.592 439.813 1 0 2 16 419.158 546.389 1 0 2 17-96.1122 430.513 1 0 2 18 6144.38 535.160 1 0 2 19 3831.91 626.461 1 0 2 20 41.3248 507.113 1 0 2 21 4143.36 602.618 1 0 -2 -25 93.0305 286.758 1 0 3 -24-353.606 296.022 1 0 3 -23 610.112 373.139 1 0 3 -22 823.069 441.844 1 0 3 -21 376.662 498.847 1 0 3 21 27.1609 747.167 -2 0 3 -20 27.1609 747.167 1 0 3 20 1948.88 820.773 -2 0 3 -19 1948.88 820.773 1 0 -3 -17-548.666 1001.61 -2 0 -3 16-548.666 1001.61 1 0 -3 -16 10015.5 998.823 -2 0 -3 15 10015.5 998.823 1 0 -3 -15 719.826 534.987 -2 0 -3 14 719.826 534.987 1 0 -3 -14 853.950 454.524 -2 0 -3 13 853.950 454.524 1 0 -3 -13 8764.33 576.459 -2 0 -3 12 8764.33 576.459 1 0 -3 -12 4563.32 610.527 -2 0 -3 11 4563.32 610.527 1 0 -3 -11 8809.35 724.456 -2 0 -3 10 8809.35 724.456 1 0 -3 -10 8652.21 665.930 -2 0 -3 9 8652.21 665.930 1 0 -3 -9 14196.5 760.555 -2 0 -3 8 14196.5 760.555 1 0 -3 -8 1391.62 389.050 -2 0 -3 7 1391.62 389.050 1 0 -3 -7 4321.04 455.831 -2 0 -3 6 4321.04 455.831 1 0 3 6 28247.8 504.312 -2 0 3 -5 28247.8 504.312 1 0 3 -4 7349.99 419.927 1 0 -3 -5 7807.95 328.258 -2 0 -3 4 7807.95 328.258 1 0 -3 3 87691.4 911.366 1 0 -3 -4 204010. 1888.72 -2 0 -3 3 204010. 1888.72 1 0 3 3 452043. 2054.32 -2 0 3 -2 452043. 2054.32 1 0 -3 -2 35537.9 890.611 -2 0 -3 1 35537.9 890.611 1 0 -3 -1 79001.8 1326.92 -2 0 -3 0 79001.8 1326.92 1 0 3 0 84384.2 1428.04 -2 0 3 1 84384.2 1428.04 1 0 3 -1 19697.5 792.319 -2 0 3 2 19697.5 792.319 1 0 -3 2 470056. 1965.38 -2 0 -3 -3 470056. 1965.38 1 0 -3 3 252419. 1485.21 -2 0 -3 -4 252419. 1485.21 1 0 3 -4 4221.18 302.606 -2 0 3 5 4221.18 302.606 1 0 3 -5 34492.6 620.892 -2 0 3 6 34492.6 620.892 1 0 3 -6 6451.10 294.740 -2 0 3 7 6451.10 294.740 1 0 3 -7 712.661 250.087 -2 0 3 8 712.661 250.087 1 0 3 -8 13783.5 477.398 -2 0 3 9 13783.5 477.398 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-8 -15 349.590 238.125 2 -6 -8 -16-229.116 203.082 2 -6 -8 -17 44.5166 185.302 2 -6 -8 -18 266.179 188.242 2 6 9 -9 302.211 188.460 2 -6 -9 -17 50.1412 280.812 2 -7 8 -13-271.929 248.676 2 -7 7 10 115.341 277.426 2 -7 7 9 42.5044 282.317 2 -7 7 8 183.845 296.008 2 -7 7 7 1138.46 270.507 2 -7 7 6 1657.05 348.744 2 -7 7 5 14.1109 350.125 2 -7 7 4 1101.27 357.967 2 -7 7 3-87.3457 378.009 2 -7 7 2 259.241 372.143 2 -7 7 1 242.658 474.542 2 -7 7 0 275.047 398.603 2 -7 7 -1 1402.65 418.269 2 -7 7 -2-105.594 503.192 2 -7 7 -3 442.436 503.339 2 -7 7 -4 1369.48 534.431 2 -7 7 -5 289.273 546.523 2 -7 7 -6 128.254 546.786 2 -7 7 -7 429.065 561.857 2 -7 7 -10 7114.42 564.781 2 -7 7 -11 1008.60 265.541 2 -7 7 -12-24.8806 234.909 2 -7 7 -13 108.023 219.479 2 -7 7 -14 29.5330 198.626 2 -7 7 -15 32.1048 184.644 2 -7 4 13 28.7314 431.773 2 -7 4 12 346.302 223.020 2 -7 4 11 236.034 220.529 2 -7 4 10 467.733 191.744 2 -7 4 3 1090.75 646.450 2 -7 4 2 1349.31 642.081 2 -7 4 -6 205.366 726.347 2 -7 4 -7 930.123 754.490 2 -7 4 -15 973.144 227.316 2 -7 4 -16 654.140 206.631 2 -7 4 -17 8.72318 225.120 2 -7 4 -18 37.7661 199.139 2 -7 4 -19 251.113 305.047 2 -7 3 13 91.8665 159.496 2 -7 3 12 118.793 173.124 2 -7 3 11-46.4821 181.166 2 -7 3 10 590.881 200.029 2 -7 3 9 963.168 214.343 2 -7 3 8 18.9200 265.431 2 -7 3 7-493.974 574.072 2 -7 3 6 235.206 668.126 2 -7 3 5 288.285 478.448 2 -7 3 4 578.839 503.629 2 -7 3 3-80.1811 489.288 2 -7 3 2 921.126 499.557 2 -7 3 1 2831.99 713.843 2 -7 3 0 790.600 664.320 2 -7 3 -1 313.388 651.828 2 -7 3 -2 425.566 649.693 2 -7 3 -3 4706.52 741.945 2 -7 3 -4 3778.45 732.955 2 -7 3 -5 710.095 718.863 2 -7 3 -6 4197.54 747.841 2 -7 3 -7 698.228 746.684 2 -7 3 -8 940.491 778.368 2 -7 3 -13 686.106 576.305 2 -7 3 -14 38.5416 210.462 2 -7 3 -15 664.313 195.735 2 -7 3 -16 217.284 196.885 2 -7 3 -17 423.961 247.512 2 -7 3 -18 472.161 227.354 2 -7 3 -19 586.991 208.967 2 -7 3 -20-190.529 300.020 2 -7 0 14 268.214 403.502 2 -7 0 13 254.974 232.495 2 -7 0 12-30.7132 229.421 2 -7 0 11 1.97362 191.441 2 -7 0 10 6.48392 205.587 2 -7 0 9-123.292 259.696 2 -7 0 8-684.936 517.644 2 -7 0 7 23.0432 488.898 2 -7 0 3-59.7786 748.091 2 -7 0 2-861.280 735.216 2 -7 0 -4-5.38806 707.565 2 -7 0 -13 300.900 553.528 2 -7 0 -14-347.303 301.794 2 -7 0 -15 42.0636 236.926 2 -7 0 -16 219.461 209.411 2 -7 0 -17 242.919 191.220 2 -7 0 -18 269.605 271.138 2 -7 0 -19 154.069 414.745 2 -7 0 -20-288.657 378.161 2 -7 0 -21 72.3746 321.760 2 -7 -1 14 48.0742 392.525 2 -7 -1 13 285.604 229.616 2 -7 -1 12 385.212 231.934 2 -7 -1 11 449.957 186.805 2 -7 -1 9 336.328 451.189 2 -7 -1 -16 123.829 547.342 2 -7 -1 -17 101.620 313.078 2 -7 -1 -18 35.0840 314.146 2 -7 -1 -19 17.5408 295.725 2 -7 -1 -20-11.2199 364.989 2 -7 -1 -21 1373.86 373.678 2 -7 -4 12 214.929 259.629 2 -7 -4 11-25.9507 170.850 2 -7 -4 10 196.999 231.349 2 -7 -4 9 711.143 196.557 2 -7 -4 8 169.890 255.612 2 -7 -4 7 282.395 267.879 2 -7 -4 6 359.316 298.186 2 -7 -4 -6 612.448 524.793 2 -7 -4 -8 539.894 546.491 2 -7 -4 -9 721.316 379.425 2 -7 -4 -10 205.486 569.989 2 -7 -4 -11 4508.34 733.551 2 -7 -4 -12 830.828 615.694 2 -7 -4 -13 186.931 502.787 2 -7 -4 -14 1166.44 367.706 2 -7 -4 -15 102.741 276.382 2 -7 -4 -16 804.149 238.416 2 -7 -4 -17 642.750 309.264 2 -7 -4 -18-2.28424 337.093 2 -7 -4 -19 140.087 319.120 2 -7 -4 -20 19.7054 308.881 2 -7 -5 11 177.559 200.825 2 -7 -5 10-13.9998 312.368 2 -7 -8 7 1029.14 251.703 2 7 8 -6 146.251 211.459 2 -7 -8 5-35.8380 286.481 2 -7 -8 4 279.059 294.987 2 -7 -8 2 481.208 333.783 2 -7 -8 0-72.5484 370.918 2 -7 -8 -1 1268.40 412.459 2 -7 -8 -2 1192.27 421.998 2 -7 -8 -4 3213.58 512.721 2 -7 -8 -8 1209.81 403.813 2 -7 -8 -9 281.755 375.013 2 -7 -8 -10 350.504 281.088 2 -7 -8 -11 195.803 353.089 2 -7 -8 -13 461.451 234.678 2 -7 -8 -14 90.0190 217.880 2 -7 -8 -15 159.198 209.149 2 -7 -8 -16 323.780 287.487 2 -8 8 -6 306.828 420.023 2 -8 7 5 204.861 370.968 2 -8 7 4 1181.37 354.979 2 -8 7 3 435.526 380.490 2 -8 7 -6 858.271 451.131 2 -8 4 10 199.716 175.771 2 -8 4 9 234.043 189.392 2 -8 4 8-36.0671 163.623 2 -8 4 7 394.306 239.293 2 -8 4 6 271.451 226.234 2 -8 4 5 2542.29 498.302 2 -8 4 4 2162.62 520.079 2 -8 4 2 770.675 610.243 2 -8 4 1 2256.37 435.619 2 -8 4 0 677.479 522.970 2 -8 4 -1 754.279 534.646 2 -8 4 -2 867.253 527.100 2 -8 4 -3-489.747 515.254 2 -8 4 -4 391.507 523.898 2 -8 4 -5 99.7822 540.370 2 -8 4 -6 393.190 559.944 2 -8 4 -7 372.526 566.142 2 -8 4 -8 552.967 578.200 2 -8 4 -13-2.44484 282.578 2 -8 4 -14-17.6778 192.049 2 -8 4 -15-124.293 274.469 2 -8 4 -16-106.101 241.639 2 -8 3 10 53.4075 151.542 2 -8 3 9 160.296 198.486 2 8 -3 -8 55.7211 225.310 2 -8 3 3 451.429 499.401 2 -8 3 1 784.739 515.399 2 -8 3 -8 76.4370 589.233 2 -8 3 -9 1529.16 582.511 2 -8 3 -16 165.945 213.850 2 -8 3 -17 287.835 196.038 2 -8 0 11 163.422 177.331 2 -8 0 10 82.0814 143.437 2 -8 0 9 176.655 160.763 2 -8 0 8 209.907 192.117 2 -8 0 7 659.165 209.768 2 -8 0 6 2878.85 366.520 2 -8 0 5 17268.6 625.853 2 -8 0 4 14492.0 620.025 2 -8 0 3 2253.90 397.991 2 -8 0 2 26179.5 763.143 2 -8 0 1 1200.38 347.387 2 -8 0 0 1136.04 341.123 2 -8 0 -1 161.899 354.399 2 -8 0 -2 347.650 348.389 2 -8 0 -3 3627.33 491.089 2 -8 0 -4 3079.38 531.970 2 -8 0 -5 858.535 560.547 2 -8 0 -12 2420.14 497.055 2 -8 0 -13 808.871 229.841 2 -8 0 -14 680.799 211.671 2 -8 0 -15 3916.36 271.516 2 -8 0 -16 509.727 185.637 2 -8 0 -17 1641.15 413.619 2 -8 0 -18 319.928 320.618 2 -8 -1 11-60.1650 346.769 2 -8 -1 10 202.889 202.984 2 -8 -1 9-18.8479 196.772 2 -8 -1 -18 352.142 341.734 2 -8 -4 9 10.4485 349.839 2 -8 -4 8 22.7320 189.213 2 -8 -4 7-89.2029 214.840 2 -8 -4 6 400.559 213.194 2 -8 -4 5 280.216 225.077 2 -8 -4 4 864.284 246.410 2 -8 -4 3 1735.55 383.967 2 -8 -4 2 835.454 257.997 2 -8 -4 1 324.461 390.997 2 -8 -4 0 2042.21 419.897 2 -8 -4 -1 631.640 287.553 2 -8 -4 -2 1233.33 421.929 2 -8 -4 -3 366.403 455.655 2 -8 -4 -4-129.694 315.487 2 -8 -4 -6 836.425 410.943 2 -8 -4 -7 543.902 422.893 2 -8 -4 -14-77.2292 333.134 2 -8 -4 -15 27.1267 316.267 2 -8 -4 -16 461.781 305.497 2 -8 -4 -17 153.636 289.228 2 -9 4 4 278.977 327.561 2 -9 4 -3-631.851 395.368 2 -9 4 -4 995.863 394.257 2 -9 4 -5 449.584 419.556 2 -9 4 -12 13.1228 151.139 2 9 0 -6 13.4879 137.979 2 -9 0 5 59.1549 190.578 2 -9 0 4 322.870 485.479 2 -9 0 2-331.558 444.837 2 -9 0 1-160.420 248.520 2 -9 0 0 95.8706 257.780 2 -9 0 -1-102.078 250.335 2 -9 0 -2-392.632 397.934 2 -9 0 -3-130.785 420.179 2 -9 0 -4-201.888 425.095 2 -9 0 -5-213.559 379.453 2 -9 0 -6 47.9537 407.427 2 -9 0 -7-62.1732 384.701 2 -9 0 -8-100.012 389.225 2 -9 0 -9-91.3754 387.609 2 -9 0 -10 36.5739 398.632 2 -9 0 -11 196.913 424.129 2 -9 0 -13-0.57869 229.299 2 -9 0 -14 211.920 226.433 2 -9 -3 0 1933.87 427.329 2 -9 -3 -13-168.499 397.612 2 -9 -4 3 602.618 173.074 2 -9 -4 1 206.639 257.774 2 -9 -4 -1-113.629 407.478 2 -9 -4 -2 157.772 388.220 2 -9 -4 -3 642.826 253.045 2 -10 0 -4 102.324 293.138 2 -10 0 -5 246.941 282.980 2 -10 0 -6 240.009 284.836 2 ; _shelx_res_checksum 63615 _shelx_res_file ; TITL CF solution in P-1 CELL 1.54184 8.166595 12.323192 20.794783 85.6851 80.4403 89.9928 ZERR 2 0.00076 0.001003 0.002195 0.0076 0.0083 0.0071 LATT 1 SFAC C H O UNIT 88 104 26 ISOR 0.01 0.02 O14 O13 L.S. 10 PLAN 25 BOND $H HTAB CONF fmap 2 acta SHEL 999 0.83 OMIT 5 -8 3 OMIT 0 5 -17 OMIT 5 -8 2 OMIT -3 -1 -5 OMIT 1 0 3 OMIT 4 -6 -5 OMIT 2 -2 2 OMIT 0 2 0 OMIT 8 0 -3 OMIT -1 0 -2 OMIT 0 1 0 OMIT 1 0 0 OMIT -1 0 -4 OMIT -5 -1 15 OMIT -3 12 -11 OMIT 6 4 10 OMIT 9 0 -3 OMIT 0 1 -1 OMIT -2 -1 -3 OMIT -4 7 15 OMIT -2 -2 -4 OMIT 6 -8 12 OMIT 0 1 4 OMIT 0 2 1 OMIT 0 -1 -4 OMIT 1 7 -14 OMIT 0 2 5 OMIT 0 0 3 OMIT 0 2 2 OMIT 1 -1 0 OMIT -1 0 1 OMIT 4 0 3 OMIT 0 2 3 REM D:/olex2_zhangjj0607_twin1_hklf4/zhangjj0607_twin1_hklf5.hkl WGHT 0.200000 BASF 0.39597 FVAR 4.56437 O9 3 0.543777 0.586479 0.172773 11.00000 0.04421 0.01607 = 0.04353 -0.00398 -0.00097 0.00549 O8 3 0.846399 0.919028 0.038797 11.00000 0.03848 0.02505 = 0.04314 -0.00941 0.00180 0.00446 O1 3 0.347470 0.571940 0.040298 11.00000 0.03098 0.02706 = 0.04282 -0.00033 0.00419 0.00450 O7 3 0.860665 1.134273 0.049563 11.00000 0.03334 0.01891 = 0.05185 -0.00632 0.00484 0.00107 AFIX 147 H7 2 0.919104 1.093281 0.026550 11.00000 -1.50000 AFIX 0 O2 3 0.360623 0.354921 0.050182 11.00000 0.03128 0.02199 = 0.05256 -0.00019 0.00354 0.01287 AFIX 147 H2 2 0.428289 0.402659 0.034098 11.00000 -1.50000 AFIX 0 O10 3 0.361862 0.664951 0.271305 11.00000 0.04127 0.02187 = 0.04152 -0.00103 -0.00445 0.00046 O11 3 0.862380 1.006288 0.386333 11.00000 0.03976 0.04454 = 0.04649 0.00087 -0.01480 0.01289 O3 3 0.043373 0.869125 0.173089 11.00000 0.03816 0.01903 = 0.04507 -0.00261 -0.00315 0.00801 O4 3 -0.139009 0.768021 0.271723 11.00000 0.04162 0.02296 = 0.03866 -0.00294 0.00387 0.00574 O12 3 0.631611 1.104083 0.462795 11.00000 0.04229 0.04617 = 0.03809 -0.00925 -0.01048 0.00178 O6 3 0.136798 0.266801 0.460065 11.00000 0.06687 0.04174 = 0.02779 0.00332 -0.01087 -0.00417 O5 3 0.365867 0.387683 0.385725 11.00000 0.04073 0.04011 = 0.04429 -0.00245 -0.01434 0.00198 C23 1 0.717222 1.075825 0.084254 11.00000 0.02228 0.02281 = 0.04196 -0.00275 -0.00099 0.00628 C31 1 0.644090 0.881619 0.133808 11.00000 0.02563 0.01503 = 0.04014 -0.00703 -0.00564 0.00537 C15 1 0.065645 0.371868 0.272753 11.00000 0.03255 0.01995 = 0.04021 -0.00093 -0.00598 0.01228 C4 1 0.053145 0.406633 0.202139 11.00000 0.02842 0.01719 = 0.03457 -0.00023 -0.00590 0.00330 AFIX 13 H4 2 -0.052359 0.378150 0.193392 11.00000 -1.20000 AFIX 0 C17 1 0.228388 0.366364 0.359682 11.00000 0.03355 0.01937 = 0.04678 -0.00755 -0.00967 0.00897 C5 1 0.050610 0.530771 0.190508 11.00000 0.02100 0.02117 = 0.04128 -0.00143 -0.00999 0.00462 C29 1 0.551631 0.697500 0.173627 11.00000 0.02269 0.01257 = 0.05052 -0.00666 -0.00888 0.00562 C6 1 -0.046334 0.589903 0.237460 11.00000 0.02483 0.02183 = 0.03603 -0.00081 -0.00285 0.00619 AFIX 43 H6 2 -0.108027 0.553845 0.274526 11.00000 -1.20000 AFIX 0 C42 1 0.707569 1.020870 0.297101 11.00000 0.03167 0.01410 = 0.04647 -0.00427 -0.00676 0.00767 AFIX 43 H42 2 0.789847 0.984982 0.270574 11.00000 -1.20000 AFIX 0 C18 1 0.104412 0.299145 0.400392 11.00000 0.05450 0.02497 = 0.02871 -0.00373 -0.01001 0.00671 C7 1 -0.049923 0.702756 0.228408 11.00000 0.03048 0.02004 = 0.04178 -0.00420 -0.00940 0.01071 C26 1 0.552530 0.921721 0.189187 11.00000 0.02863 0.01458 = 0.03381 -0.00216 -0.01150 0.00437 C10 1 0.142601 0.585711 0.134806 11.00000 0.02677 0.02598 = 0.03150 -0.00148 -0.00416 0.01105 C2 1 0.218671 0.403147 0.086105 11.00000 0.03037 0.01737 = 0.03559 -0.00674 -0.00695 0.01009 C28 1 0.454039 0.741392 0.228223 11.00000 0.02730 0.02465 = 0.03472 -0.00112 -0.00816 0.00603 C24 1 0.694241 1.106084 0.154836 11.00000 0.02417 0.02498 = 0.03722 -0.00336 -0.00321 0.00224 AFIX 13 H24 2 0.797963 1.087544 0.170724 11.00000 -1.20000 AFIX 0 C38 1 0.444514 1.109351 0.312817 11.00000 0.03058 0.02141 = 0.04879 0.00191 -0.00409 0.00396 AFIX 43 H38 2 0.351045 1.134820 0.296573 11.00000 -1.20000 AFIX 0 C40 1 0.600709 1.089339 0.400965 11.00000 0.04202 0.02462 = 0.03614 -0.00346 -0.00255 0.00425 C32 1 0.744503 0.953639 0.082653 11.00000 0.02845 0.02503 = 0.03499 -0.00249 -0.00688 0.00335 C37 1 0.567693 1.057387 0.272332 11.00000 0.03233 0.01603 = 0.03790 -0.00366 -0.00672 0.00644 C25 1 0.555024 1.043103 0.201715 11.00000 0.02502 0.01928 = 0.04504 -0.00539 -0.00885 0.00825 AFIX 13 H25 2 0.449041 1.073824 0.193544 11.00000 -1.20000 AFIX 0 C9 1 0.142353 0.700090 0.127881 11.00000 0.02307 0.01991 = 0.04128 0.00173 -0.00544 0.00547 AFIX 43 H9 2 0.206151 0.736639 0.091486 11.00000 -1.20000 AFIX 0 C33 1 0.569878 1.105239 0.050819 11.00000 0.03879 0.02464 = 0.03450 -0.00068 -0.00990 0.00668 AFIX 137 H33A 2 0.557786 1.182854 0.047559 11.00000 -1.50000 H33B 2 0.470904 1.072004 0.075940 11.00000 -1.50000 H33C 2 0.587728 1.079469 0.007805 11.00000 -1.50000 AFIX 0 C30 1 0.644338 0.768067 0.126108 11.00000 0.02633 0.02033 = 0.04233 -0.00049 -0.00618 0.00852 AFIX 43 H30 2 0.706528 0.741005 0.089279 11.00000 -1.20000 AFIX 0 C41 1 0.725745 1.036707 0.359028 11.00000 0.03037 0.02660 = 0.03647 0.00311 -0.00861 0.00622 C36 1 0.656973 0.540437 0.121746 11.00000 0.03884 0.02319 = 0.05083 -0.01001 -0.00548 0.01482 AFIX 137 H36A 2 0.633384 0.568283 0.079933 11.00000 -1.50000 H36B 2 0.644255 0.462655 0.125920 11.00000 -1.50000 H36C 2 0.768863 0.559630 0.125312 11.00000 -1.50000 AFIX 0 C8 1 0.050019 0.757939 0.173721 11.00000 0.03429 0.02059 = 0.03698 -0.00386 -0.01302 0.00873 C1 1 0.245772 0.526236 0.084170 11.00000 0.02435 0.01995 = 0.03789 -0.00221 -0.00801 0.00705 C11 1 0.069494 0.383057 0.051248 11.00000 0.03338 0.01972 = 0.03649 0.00319 -0.00094 0.00266 AFIX 137 H11A 2 0.088907 0.419986 0.008302 11.00000 -1.50000 H11B 2 -0.029657 0.410314 0.076039 11.00000 -1.50000 H11C 2 0.056621 0.306397 0.047762 11.00000 -1.50000 AFIX 0 C14 1 0.156527 0.928420 0.122476 11.00000 0.03644 0.02072 = 0.03991 0.00400 -0.00344 0.00421 AFIX 137 H14A 2 0.137527 0.908439 0.080562 11.00000 -1.50000 H14B 2 0.268569 0.911434 0.127623 11.00000 -1.50000 H14C 2 0.139224 1.005075 0.125365 11.00000 -1.50000 AFIX 0 C34 1 0.672093 1.230018 0.159742 11.00000 0.03509 0.01872 = 0.04740 -0.01010 -0.00554 0.00292 AFIX 137 H34A 2 0.758368 1.268470 0.129647 11.00000 -1.50000 H34B 2 0.678279 1.247641 0.203471 11.00000 -1.50000 H34C 2 0.565887 1.250855 0.149151 11.00000 -1.50000 AFIX 0 C43 1 0.498823 1.153379 0.504487 11.00000 0.09204 0.05594 = 0.03181 -0.01592 -0.01690 0.02361 AFIX 137 H43A 2 0.470421 1.221172 0.483460 11.00000 -1.50000 H43B 2 0.533645 1.166373 0.545146 11.00000 -1.50000 H43C 2 0.403661 1.105537 0.512718 11.00000 -1.50000 AFIX 0 C3 1 0.195414 0.353638 0.156100 11.00000 0.02717 0.01364 = 0.04062 -0.00400 -0.00792 0.00719 AFIX 13 H3 2 0.298663 0.366707 0.172664 11.00000 -1.20000 AFIX 0 C27 1 0.453602 0.850252 0.235682 11.00000 0.02441 0.02902 = 0.03768 -0.00399 -0.00613 0.00513 AFIX 43 H27 2 0.387654 0.877383 0.271645 11.00000 -1.20000 AFIX 0 C20 1 -0.055464 0.306404 0.312816 11.00000 0.03250 0.02536 = 0.03440 -0.00220 -0.00546 0.00374 AFIX 43 H20 2 -0.149810 0.285273 0.297092 11.00000 -1.20000 AFIX 0 C13 1 -0.240495 0.716442 0.328451 11.00000 0.05276 0.03712 = 0.03869 -0.00639 0.00721 0.00773 AFIX 137 H13A 2 -0.326743 0.674550 0.315364 11.00000 -1.50000 H13B 2 -0.289340 0.770863 0.356116 11.00000 -1.50000 H13C 2 -0.173530 0.669289 0.351956 11.00000 -1.50000 AFIX 0 C16 1 0.206477 0.401185 0.296795 11.00000 0.04087 0.02275 = 0.03406 0.00412 -0.00144 0.00573 AFIX 43 H16 2 0.287456 0.444876 0.270319 11.00000 -1.20000 AFIX 0 C12 1 0.168493 0.230555 0.160093 11.00000 0.03806 0.02343 = 0.04694 -0.00295 -0.00815 0.00797 AFIX 137 H12A 2 0.175048 0.200437 0.203516 11.00000 -1.50000 H12B 2 0.252526 0.199025 0.129376 11.00000 -1.50000 H12C 2 0.060979 0.214808 0.149897 11.00000 -1.50000 AFIX 0 C19 1 -0.034716 0.272808 0.376366 11.00000 0.04058 0.02403 = 0.04240 0.00366 0.00048 0.00623 AFIX 43 H19 2 -0.117948 0.231311 0.403131 11.00000 -1.20000 AFIX 0 C39 1 0.459163 1.123757 0.377253 11.00000 0.04512 0.03106 = 0.03600 -0.00523 -0.00755 0.01101 AFIX 43 H39 2 0.374212 1.156397 0.404356 11.00000 -1.20000 AFIX 0 C21 1 0.022292 0.186268 0.500379 11.00000 0.07523 0.06478 = 0.03511 0.02498 -0.00922 -0.00260 AFIX 137 H21A 2 0.022094 0.120691 0.478223 11.00000 -1.50000 H21B 2 -0.087794 0.215283 0.507400 11.00000 -1.50000 H21C 2 0.058070 0.170429 0.541745 11.00000 -1.50000 AFIX 0 C22 1 0.512575 0.423256 0.339829 11.00000 0.02922 0.04930 = 0.05939 -0.00300 -0.01166 -0.00421 AFIX 137 H22A 2 0.522309 0.381943 0.302065 11.00000 -1.50000 H22B 2 0.609070 0.412292 0.360230 11.00000 -1.50000 H22C 2 0.503632 0.499121 0.326759 11.00000 -1.50000 AFIX 0 C44 1 1.009627 0.986221 0.342123 11.00000 0.04300 0.04042 = 0.05273 -0.00017 -0.01587 0.01032 AFIX 137 H44A 2 1.034914 1.047894 0.310964 11.00000 -1.50000 H44B 2 0.993508 0.922898 0.319579 11.00000 -1.50000 H44C 2 1.099935 0.974312 0.365960 11.00000 -1.50000 AFIX 0 C35 1 0.257109 0.702833 0.326442 11.00000 0.04979 0.03096 = 0.03823 0.00427 0.00069 -0.00500 AFIX 137 H35A 2 0.181142 0.754986 0.311951 11.00000 -1.50000 H35B 2 0.323569 0.736517 0.353552 11.00000 -1.50000 H35C 2 0.195844 0.642589 0.351074 11.00000 -1.50000 AFIX 0 PART 1 O14 3 0.764667 0.488296 0.478352 10.50000 0.23147 0.11186 = 0.09620 -0.06175 -0.09817 0.03551 PART 0 PART 2 O13 3 0.923562 0.455452 0.522913 10.50000 0.08946 0.11996 = 0.17216 -0.12398 0.00878 -0.02458 HKLF 5 REM CF solution in P-1 REM R1 = 0.1125 for 5543 Fo > 4sig(Fo) and 0.1727 for all 9890 data REM 538 parameters refined using 12 restraints END WGHT 0.2000 0.0000 REM Instructions for potential hydrogen bonds HTAB O7 O8 EQIV $1 -x+2, -y+2, -z HTAB O7 O8_$1 HTAB O2 O1 EQIV $2 -x+1, -y+1, -z HTAB O2 O1_$2 HTAB C36 O1 EQIV $3 x-1, y-1, z HTAB C11 O7_$3 EQIV $4 -x+1, -y+2, -z+1 HTAB C43 O12_$4 HTAB C19 O12_$3 EQIV $5 x, y+1, z HTAB C39 O6_$5 HTAB C22 O10 EQIV $6 x+1, y, z HTAB C44 O4_$6 REM Highest difference peak 1.065, deepest hole -0.451, 1-sigma level 0.112 Q1 1 0.6300 0.4150 0.5086 11.00000 0.05 1.06 Q2 1 0.5000 0.5000 0.5000 10.50000 0.05 0.99 Q3 1 0.5484 0.5128 0.4904 11.00000 0.05 0.96 Q4 1 0.9401 0.4075 0.5573 11.00000 0.05 0.80 Q5 1 0.8244 0.4961 0.4686 11.00000 0.05 0.69 Q6 1 0.9274 0.4766 0.5086 11.00000 0.05 0.68 Q7 1 -0.2065 0.2864 0.3072 11.00000 0.05 0.59 Q8 1 0.5691 0.3960 0.4649 11.00000 0.05 0.55 Q9 1 0.5095 0.4076 0.5568 11.00000 0.05 0.50 Q10 1 -0.1286 0.1746 0.5204 11.00000 0.05 0.48 Q11 1 -0.0127 0.1121 0.4907 11.00000 0.05 0.46 Q12 1 0.4311 0.8666 0.3023 11.00000 0.05 0.45 Q13 1 0.0596 0.4659 0.1891 11.00000 0.05 0.44 Q14 1 0.3554 0.4130 0.2691 11.00000 0.05 0.44 Q15 1 0.1269 0.0049 0.4592 11.00000 0.05 0.42 Q16 1 0.1432 0.4460 0.1328 11.00000 0.05 0.42 Q17 1 0.3052 1.1221 0.3076 11.00000 0.05 0.42 Q18 1 0.0430 0.1413 0.2013 11.00000 0.05 0.41 Q19 1 0.2229 0.2647 0.0959 11.00000 0.05 0.39 Q20 1 0.3597 1.0819 0.0507 11.00000 0.05 0.39 Q21 1 0.5195 1.3311 0.1881 11.00000 0.05 0.39 Q22 1 0.3088 0.6792 0.3795 11.00000 0.05 0.38 Q23 1 -0.1797 0.2841 0.3784 11.00000 0.05 0.37 Q24 1 0.6124 0.8251 0.1212 11.00000 0.05 0.37 Q25 1 0.2474 1.1252 0.2863 11.00000 0.05 0.36 ; _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. ; _shelxl_version_number 2013-2 _database_code_depnum_ccdc_archive 'CCDC 953123'