data_18gtu282 _audit_creation_date 2018-10-17 _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. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C40 H44 N2 O2' _chemical_formula_sum 'C40 H44 N2 O2' _chemical_formula_weight 584.77 _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' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8605(8) _cell_length_b 11.7357(10) _cell_length_c 14.9221(12) _cell_angle_alpha 90 _cell_angle_beta 92.649(5) _cell_angle_gamma 90 _cell_volume 1724.9(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 3503 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 24.48 _cell_measurement_theta_min 2.21 _shelx_estimated_absorpt_T_max 0.991 _shelx_estimated_absorpt_T_min 0.974 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS)' _exptl_absorpt_special_details ? _exptl_crystal_colour 'green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier greenish _exptl_crystal_colour_primary ? _exptl_crystal_density_diffrn 1.126 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 628 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.381 _exptl_crystal_size_mid 0.168 _exptl_crystal_size_min 0.13 _exptl_transmission_factor_max 0.98 _exptl_transmission_factor_min 0.97 _diffrn_reflns_av_R_equivalents 0.0546 _diffrn_reflns_av_unetI/netI 0.0567 _diffrn_reflns_Laue_measured_fraction_full 0.991 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 11829 _diffrn_reflns_point_group_measured_fraction_full 0.991 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.026 _diffrn_reflns_theta_max 25.026 _diffrn_reflns_theta_min 2.068 _diffrn_ambient_temperature 172.99 _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker APEX II QUAZAR three-circle diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type 'Incoatec I\ms' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1644 _reflns_number_total 3012 _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 ? _computing_data_collection ? _computing_data_reduction ? _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 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.265 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.041 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 267 _refine_ls_number_reflns 3012 _refine_ls_number_restraints 164 _refine_ls_R_factor_all 0.1326 _refine_ls_R_factor_gt 0.0693 _refine_ls_restrained_S_all 1.033 _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^)+(0.0911P)^2^+0.6560P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1716 _refine_ls_wR_factor_ref 0.2066 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C20-C19 1.55 with sigma of 0.02 C19-C18 1.55 with sigma of 0.02 C18-C17 1.55 with sigma of 0.02 C17-C16 1.55 with sigma of 0.02 C16-C15 1.55 with sigma of 0.02 C15-C14 1.55 with sigma of 0.02 C21-C22 1.55 with sigma of 0.02 C22-C23 1.55 with sigma of 0.02 C23-C24 1.55 with sigma of 0.02 C24-C25 1.55 with sigma of 0.02 C25-C26 1.55 with sigma of 0.02 C26-C27 1.55 with sigma of 0.02 C13-C16 \\sim C13-C25 with sigma of 0.02 C16-C15 \\sim C25-C26 with sigma of 0.02 C16-C17 \\sim C25-C24 with sigma of 0.02 C15-C14 \\sim C26-C27 with sigma of 0.02 C17-C18 \\sim C24-C23 with sigma of 0.02 C19-C18 \\sim C22-C23 with sigma of 0.02 C19-C20 \\sim C22-C21 with sigma of 0.02 C13-C15 \\sim C13-C26 with sigma of 0.04 C13-C17 \\sim C13-C24 with sigma of 0.04 C16-C18 \\sim C25-C23 with sigma of 0.04 C16-C14 \\sim C25-C27 with sigma of 0.04 C15-C17 \\sim C26-C24 with sigma of 0.04 C17-C19 \\sim C24-C22 with sigma of 0.04 C18-C20 \\sim C23-C21 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints C19 \\sim C20: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C18 \\sim C19: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C17 \\sim C18: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C16 \\sim C17: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C15 \\sim C16: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C14 \\sim C15: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C26 \\sim C27: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C25 \\sim C26: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C24 \\sim C25: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C23 \\sim C24: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C22 \\sim C23: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 C21 \\sim C22: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.08 4. Rigid body (RIGU) restrains C14, C15, C16, C17, C18, C19, C20 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C21, C22, C23, C24, C25, C26, C27 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(H13C)=Sof(H13D)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=Sof(H22A)= Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)= Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=1- FVAR(1) Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)= Sof(H15B)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)= Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)= FVAR(1) 6.a Ternary CH refined with riding coordinates: C16(H16), C25(H25) 6.b Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C13(H13C,H13D), C15(H15A,H15B), C17(H17A,H17B), C18(H18A, H18B), C19(H19A,H19B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,H26B) 6.c Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C11(H11) 6.d Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C27(H27A,H27B, H27C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _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 0.4484(2) 0.5333(2) 0.67818(15) 0.0818(9) Uani 1 1 d . . . . . N1 N 0.8650(3) 0.8982(2) 0.52594(19) 0.0704(9) Uani 1 1 d . . . . . C1 C 0.8804(3) 0.8846(3) 0.4514(2) 0.0514(8) Uani 1 1 d . . . . . C2 C 0.8989(3) 0.8649(2) 0.35771(18) 0.0453(8) Uani 1 1 d . . . . . C3 C 0.9722(3) 0.9418(3) 0.3085(2) 0.0616(9) Uani 1 1 d . . . . . H3 H 1.010241 1.007879 0.336433 0.074 Uiso 1 1 calc R . . . . C4 C 0.9894(4) 0.9217(3) 0.2189(2) 0.0696(11) Uani 1 1 d . . . . . H4 H 1.039883 0.974001 0.185031 0.084 Uiso 1 1 calc R . . . . C5 C 0.9339(3) 0.8262(3) 0.1781(2) 0.0636(10) Uani 1 1 d . . . . . H5 H 0.946271 0.813080 0.116157 0.076 Uiso 1 1 calc R . . . . C6 C 0.8605(3) 0.7494(3) 0.22621(19) 0.0509(8) Uani 1 1 d . . . . . H6 H 0.822436 0.683921 0.197259 0.061 Uiso 1 1 calc R . . . . C7 C 0.8418(3) 0.7673(2) 0.31727(18) 0.0408(7) Uani 1 1 d . . . . . C8 C 0.7628(3) 0.6907(3) 0.36775(19) 0.0433(7) Uani 1 1 d . . . . . C9 C 0.6909(3) 0.6315(3) 0.40988(19) 0.0470(8) Uani 1 1 d . . . . . C10 C 0.5964(3) 0.5633(3) 0.45675(19) 0.0453(8) Uani 1 1 d . . . . . C11 C 0.5741(3) 0.5829(3) 0.5469(2) 0.0529(8) Uani 1 1 d . . . . . H11 H 0.625151 0.639808 0.578743 0.064 Uiso 1 1 calc R . . . . C12 C 0.4787(3) 0.5205(3) 0.5905(2) 0.0511(8) Uani 1 1 d . . . . . C13 C 0.5390(4) 0.5940(4) 0.7376(2) 0.0764(11) Uani 1 1 d D . . . . H13A H 0.532792 0.677008 0.726158 0.092 Uiso 0.480(9) 1 calc R . P A 1 H13B H 0.633794 0.569172 0.730375 0.092 Uiso 0.480(9) 1 calc R . P A 1 H13C H 0.560883 0.668879 0.711308 0.092 Uiso 0.520(9) 1 calc R . P A 2 H13D H 0.624553 0.550680 0.747250 0.092 Uiso 0.520(9) 1 calc R . P A 2 C14 C 0.6391(13) 0.3901(14) 0.8706(11) 0.137(6) Uani 0.480(9) 1 d D U P A 1 H14A H 0.675620 0.385852 0.810755 0.206 Uiso 0.480(9) 1 calc GR . P A 1 H14B H 0.635505 0.313484 0.896485 0.206 Uiso 0.480(9) 1 calc GR . P A 1 H14C H 0.697773 0.438682 0.909215 0.206 Uiso 0.480(9) 1 calc GR . P A 1 C15 C 0.4962(12) 0.4406(12) 0.8635(10) 0.088(4) Uani 0.480(9) 1 d D U P A 1 H15A H 0.440606 0.395792 0.819227 0.106 Uiso 0.480(9) 1 calc R . P A 1 H15B H 0.454608 0.432789 0.922321 0.106 Uiso 0.480(9) 1 calc R . P A 1 C16 C 0.4919(14) 0.5646(11) 0.8360(9) 0.107(4) Uani 0.480(9) 1 d D U P A 1 H16 H 0.552979 0.607290 0.879535 0.128 Uiso 0.480(9) 1 calc R . P A 1 C17 C 0.3506(11) 0.6126(10) 0.8433(9) 0.126(4) Uani 0.480(9) 1 d D U P A 1 H17A H 0.308856 0.579608 0.896468 0.151 Uiso 0.480(9) 1 calc R . P A 1 H17B H 0.294071 0.590533 0.789496 0.151 Uiso 0.480(9) 1 calc R . P A 1 C18 C 0.3524(16) 0.7416(10) 0.8514(14) 0.147(6) Uani 0.480(9) 1 d D U P A 1 H18A H 0.379034 0.774748 0.793785 0.177 Uiso 0.480(9) 1 calc R . P A 1 H18B H 0.421853 0.763891 0.898146 0.177 Uiso 0.480(9) 1 calc R . P A 1 C19 C 0.2145(19) 0.7914(18) 0.8754(13) 0.173(7) Uani 0.480(9) 1 d D U P A 1 H19A H 0.211606 0.870541 0.852484 0.208 Uiso 0.480(9) 1 calc R . P A 1 H19B H 0.144126 0.748391 0.840041 0.208 Uiso 0.480(9) 1 calc R . P A 1 C20 C 0.169(2) 0.796(2) 0.9716(14) 0.219(11) Uani 0.480(9) 1 d D U P A 1 H20A H 0.069690 0.787924 0.971481 0.329 Uiso 0.480(9) 1 calc GR . P A 1 H20B H 0.195515 0.868864 0.998802 0.329 Uiso 0.480(9) 1 calc GR . P A 1 H20C H 0.211277 0.733437 1.006309 0.329 Uiso 0.480(9) 1 calc GR . P A 1 C21 C 0.1247(12) 0.8647(10) 0.9728(7) 0.092(3) Uani 0.520(9) 1 d D U P A 2 H21A H 0.070444 0.933753 0.961957 0.137 Uiso 0.520(9) 1 calc GR . P A 2 H21B H 0.189016 0.877244 1.023893 0.137 Uiso 0.520(9) 1 calc GR . P A 2 H21C H 0.064544 0.801024 0.986067 0.137 Uiso 0.520(9) 1 calc GR . P A 2 C22 C 0.2028(10) 0.8369(9) 0.8893(6) 0.077(3) Uani 0.520(9) 1 d D U P A 2 H22A H 0.261751 0.902133 0.875230 0.092 Uiso 0.520(9) 1 calc R . P A 2 H22B H 0.137565 0.825284 0.837652 0.092 Uiso 0.520(9) 1 calc R . P A 2 C23 C 0.2915(9) 0.7282(7) 0.9028(4) 0.068(2) Uani 0.520(9) 1 d D U P A 2 H23A H 0.360712 0.741031 0.951959 0.082 Uiso 0.520(9) 1 calc R . P A 2 H23B H 0.233701 0.663455 0.919861 0.082 Uiso 0.520(9) 1 calc R . P A 2 C24 C 0.3616(9) 0.6997(9) 0.8159(5) 0.076(3) Uani 0.520(9) 1 d D U P A 2 H24A H 0.292408 0.671868 0.770974 0.091 Uiso 0.520(9) 1 calc R . P A 2 H24B H 0.401141 0.770387 0.792087 0.091 Uiso 0.520(9) 1 calc R . P A 2 C25 C 0.4722(11) 0.6113(9) 0.8273(6) 0.077(3) Uani 0.520(9) 1 d D U P A 2 H25 H 0.543497 0.645452 0.868928 0.093 Uiso 0.520(9) 1 calc R . P A 2 C26 C 0.4370(14) 0.5005(11) 0.8665(7) 0.107(4) Uani 0.520(9) 1 d D U P A 2 H26A H 0.367248 0.462560 0.827053 0.128 Uiso 0.520(9) 1 calc R . P A 2 H26B H 0.397923 0.513075 0.925616 0.128 Uiso 0.520(9) 1 calc R . P A 2 C27 C 0.563(2) 0.4220(13) 0.8782(14) 0.149(8) Uani 0.520(9) 1 d D U P A 2 H27A H 0.596721 0.403466 0.819178 0.223 Uiso 0.520(9) 1 calc GR . P A 2 H27B H 0.537779 0.351604 0.908615 0.223 Uiso 0.520(9) 1 calc GR . P A 2 H27C H 0.634331 0.461223 0.914252 0.223 Uiso 0.520(9) 1 calc GR . P A 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 O1 0.0794(16) 0.114(2) 0.0538(15) -0.0185(14) 0.0219(12) -0.0493(15) N1 0.102(2) 0.067(2) 0.0431(18) -0.0030(15) 0.0143(15) -0.0136(17) C1 0.066(2) 0.049(2) 0.039(2) 0.0009(15) 0.0062(15) -0.0098(16) C2 0.0541(17) 0.0448(18) 0.0377(17) 0.0045(14) 0.0090(13) -0.0053(14) C3 0.082(2) 0.059(2) 0.044(2) -0.0017(16) 0.0140(17) -0.0270(18) C4 0.092(3) 0.071(3) 0.048(2) 0.0098(18) 0.0175(19) -0.027(2) C5 0.080(2) 0.074(2) 0.0378(18) -0.0018(17) 0.0174(16) -0.011(2) C6 0.0540(18) 0.055(2) 0.0439(18) -0.0084(15) 0.0074(14) -0.0049(15) C7 0.0401(14) 0.0454(17) 0.0373(16) 0.0015(14) 0.0074(12) -0.0002(13) C8 0.0424(15) 0.0436(17) 0.0441(17) 0.0004(14) 0.0058(13) -0.0025(14) C9 0.0447(16) 0.0491(19) 0.0474(18) 0.0016(15) 0.0033(14) -0.0012(14) C10 0.0407(15) 0.0484(19) 0.0471(19) 0.0053(15) 0.0054(13) -0.0031(14) C11 0.0534(18) 0.054(2) 0.052(2) -0.0032(16) 0.0060(15) -0.0155(15) C12 0.0529(18) 0.057(2) 0.0440(18) -0.0004(16) 0.0110(14) -0.0085(16) C13 0.088(3) 0.087(3) 0.055(2) -0.014(2) 0.0099(19) -0.026(2) C14 0.124(9) 0.158(13) 0.125(11) -0.038(10) -0.037(9) -0.020(8) C15 0.101(8) 0.097(9) 0.070(7) -0.050(8) 0.029(6) -0.040(6) C16 0.120(8) 0.080(8) 0.123(10) -0.053(7) 0.055(7) -0.043(6) C17 0.127(7) 0.107(8) 0.146(9) -0.008(8) 0.044(7) -0.034(6) C18 0.129(9) 0.105(8) 0.209(14) -0.008(10) 0.023(10) -0.015(7) C19 0.125(11) 0.137(13) 0.258(17) 0.006(13) 0.023(12) -0.009(10) C20 0.116(14) 0.28(3) 0.263(19) -0.04(2) 0.026(13) -0.017(16) C21 0.078(7) 0.111(8) 0.087(6) -0.011(5) 0.021(5) -0.022(5) C22 0.076(6) 0.089(6) 0.067(5) 0.001(4) 0.012(4) -0.035(4) C23 0.074(5) 0.095(5) 0.037(4) -0.003(3) 0.016(3) -0.027(4) C24 0.086(5) 0.090(7) 0.054(4) -0.009(4) 0.031(4) -0.037(4) C25 0.102(7) 0.086(7) 0.046(5) -0.017(5) 0.028(4) -0.022(5) C26 0.166(10) 0.089(7) 0.069(6) -0.018(6) 0.045(6) -0.035(7) C27 0.25(2) 0.085(8) 0.115(12) 0.030(8) 0.077(16) 0.031(12) _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 C12 1.364(3) . ? O1 C13 1.421(4) . ? N1 C1 1.141(3) . ? C1 C2 1.436(4) . ? C2 C3 1.387(4) . ? C2 C7 1.401(4) . ? C3 C4 1.375(4) . ? C4 C5 1.378(5) . ? C5 C6 1.378(4) . ? C6 C7 1.396(4) . ? C7 C8 1.427(4) . ? C8 C9 1.193(4) . ? C9 C10 1.434(4) . ? C10 C11 1.393(4) . ? C10 C12 1.401(4) 3_666 ? C11 C12 1.379(4) . ? C13 C16 1.597(12) . ? C13 C25 1.531(9) . ? C14 C15 1.527(12) . ? C15 C16 1.513(12) . ? C16 C17 1.511(12) . ? C17 C18 1.518(11) . ? C18 C19 1.538(13) . ? C19 C20 1.526(13) . ? C21 C22 1.530(9) . ? C22 C23 1.554(10) . ? C23 C24 1.534(8) . ? C24 C25 1.509(11) . ? C25 C26 1.474(11) . ? C26 C27 1.551(12) . ? 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 C12 O1 C13 119.7(2) . . ? N1 C1 C2 178.8(3) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 C7 120.8(3) . . ? C7 C2 C1 118.9(2) . . ? C4 C3 C2 119.6(3) . . ? C3 C4 C5 120.3(3) . . ? C4 C5 C6 120.6(3) . . ? C5 C6 C7 120.3(3) . . ? C2 C7 C8 120.4(2) . . ? C6 C7 C2 118.3(2) . . ? C6 C7 C8 121.3(3) . . ? C9 C8 C7 176.1(3) . . ? C8 C9 C10 175.9(3) . . ? C11 C10 C9 120.9(3) . . ? C11 C10 C12 119.9(3) . 3_666 ? C12 C10 C9 119.1(3) 3_666 . ? C12 C11 C10 120.6(3) . . ? O1 C12 C10 115.2(2) . 3_666 ? O1 C12 C11 125.3(3) . . ? C11 C12 C10 119.5(3) . 3_666 ? O1 C13 C16 105.3(6) . . ? O1 C13 C25 109.2(5) . . ? C16 C15 C14 114.0(11) . . ? C15 C16 C13 116.8(9) . . ? C17 C16 C13 107.1(10) . . ? C17 C16 C15 110.7(10) . . ? C16 C17 C18 111.7(11) . . ? C17 C18 C19 113.0(14) . . ? C20 C19 C18 122.4(17) . . ? C21 C22 C23 111.8(7) . . ? C24 C23 C22 110.0(7) . . ? C25 C24 C23 114.0(7) . . ? C24 C25 C13 109.3(7) . . ? C26 C25 C13 110.4(7) . . ? C26 C25 C24 117.9(9) . . ? C25 C26 C27 111.5(11) . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma 1 0 0 754.72 18.6 2 0 0 2058.89 50.39 3 0 0 1053.49 26.9 -4 0 0 123.79 3.3 4 0 0 125.79 4.9 -4 0 0 122.59 3.4 5 0 0 18.1 2.3 -5 0 0 20.6 1.1 -5 0 0 22.2 1.4 6 0 0 37.6 3.2 -7 0 0 112.69 3.9 -7 0 0 102.49 4.6 7 0 0 90.09 5.3 -8 0 0 32.6 2.3 -8 0 0 25.2 3 -11 0 0 19.2 2.8 0 -1 0 0.8 0.2 0 -1 0 0.9 0.3 0 1 0 0.6 0.4 0 1 0 0.7 0.3 1 -1 0 257.57 6.6 1 -1 0 239.98 7.1 -1 1 0 260.57 7.2 1 1 0 253.77 7.3 -1 1 0 251.37 6.6 2 -1 0 2124.49 49.9 2 -1 0 2025.6 50.09 2 1 0 2089.59 50.79 -2 1 0 2015 50.39 -2 1 0 1997.9 49.7 3 -1 0 523.85 13.7 3 -1 0 503.35 13 -3 1 0 531.35 13.4 -3 1 0 521.05 14.1 3 1 0 522.55 14.6 -3 1 0 512.75 14.1 4 -1 0 0.5 0.9 -4 1 0 0.8 0.6 4 1 0 3.7 1.4 -4 1 0 0.2 0.9 5 -1 0 1.3 1.1 5 1 0 2.4 1.5 -5 1 0 1.1 1 -5 1 0 0.6 0.7 -5 1 0 2.2 1.1 6 -1 0 89.79 4.4 -6 1 0 90.29 3.7 -6 1 0 96.99 4.7 -6 1 0 102.49 5 6 1 0 89.59 5.1 7 -1 0 9.8 2 -7 1 0 3.8 1.8 -7 1 0 4.2 1.1 7 1 0 6.2 2 -8 -1 0 17.3 1.5 -8 -1 0 18.5 1.9 8 1 0 23.4 3.8 -8 1 0 14.1 2.1 -9 -1 0 0.3 0.9 -9 1 0 3.1 1.5 -10 -1 0 11.6 1.8 -10 1 0 12 2.2 -11 -1 0 4.6 1.7 -11 1 0 0.3 1.9 0 -2 0 173.18 5.5 0 -2 0 175.78 5.8 0 -2 0 171.88 5 0 2 0 183.28 5.5 0 2 0 177.68 5.7 0 2 0 178.18 5 1 -2 0 2551.74 61.49 -1 -2 0 2408.06 60.29 -1 -2 0 2460.15 61.59 1 -2 0 2565.34 60.59 1 -2 0 2507.95 60.79 -1 -2 0 2502.85 60.69 1 2 0 2521.85 61.59 -1 2 0 2420.36 61.39 -1 2 0 2498.75 60.59 2 -2 0 4866.21 116.79 2 -2 0 4867.71 117.99 -2 2 0 4840.42 118.09 2 2 0 4929.11 118.29 -2 2 0 4718.43 117.99 3 -2 0 2 0.8 3 2 0 4.5 1.6 -3 2 0 2.4 1.1 -3 2 0 1.3 0.7 4 -2 0 293.37 8.5 4 -2 0 291.37 8.5 4 2 0 284.97 10 -4 2 0 286.57 8.5 -4 2 0 288.17 9.8 5 -2 0 5.5 1.3 -5 2 0 1.6 1.5 -5 2 0 3.7 1 5 2 0 7.4 2.2 6 -2 0 4.5 1.3 6 2 0 7.3 2.2 -6 2 0 7.1 1.9 -6 2 0 2.4 1.1 7 2 0 4.5 2.2 -7 2 0 4.9 1.4 -7 2 0 3.4 2.4 -8 -2 0 1.6 2.6 8 2 0 2.7 2.3 -8 2 0 2.5 1.3 -9 -2 0 2 0.8 -9 -2 0 0.3 3.8 -9 -2 0 2 0.7 -9 2 0 2.6 1.4 -10 -2 0 15.6 1.8 -10 2 0 9.6 2.5 -11 -2 0 0.8 1.1 -11 2 0 -2.9 1.5 0 -3 0 1.3 0.7 0 -3 0 2.7 1.5 0 -3 0 0.6 1.2 0 3 0 3.4 1.6 0 3 0 2.5 0.9 1 -3 0 244.08 7.8 1 -3 0 250.07 8.4 -1 -3 0 245.18 7.2 -1 -3 0 250.87 6.7 1 -3 0 232.48 7.1 -1 -3 0 238.68 8.6 1 3 0 247.78 6.4 -1 3 0 237.98 7.2 1 3 0 250.67 8.5 -2 -3 0 79.49 4.3 2 -3 0 74.09 4.1 2 -3 0 73.59 3.3 2 3 0 73.39 4.2 -2 3 0 74.49 4.1 -2 3 0 73.99 3.3 3 -3 0 202.48 7.8 3 -3 0 205.68 6.5 3 3 0 197.48 8.1 -3 3 0 208.58 6.7 -3 3 0 219.28 8.2 4 -3 0 74.09 3.4 -4 3 0 80.09 4.9 4 3 0 87.19 5.2 -4 3 0 74.49 3.6 5 -3 0 8 1.5 5 -3 0 10.7 1.7 -5 3 0 8.1 1.5 5 3 0 6.4 2.2 -5 3 0 10.5 2.3 6 3 0 14.3 3 -7 -3 0 7.9 2.8 -7 3 0 9.7 1.9 7 3 0 10.4 3.1 -8 -3 0 3.2 2.8 -8 3 0 4.2 1.6 8 3 0 1 2.9 -9 -3 0 29.9 5.2 -9 3 0 25.4 3.3 9 3 0 28.7 4.6 -10 3 0 8.5 2.3 -11 -3 0 8.6 1.4 -11 3 0 6.6 2.6 0 -4 0 360.56 10.2 0 -4 0 357.36 11.6 0 -4 0 358.66 11.2 0 4 0 366.56 10.1 0 4 0 353.36 11.5 1 -4 0 117.79 5.6 -1 -4 0 120.09 5.8 -1 -4 0 121.39 4.8 1 -4 0 126.39 5.4 -1 -4 0 122.29 4.1 -1 4 0 123.79 4.6 1 4 0 113.09 5.6 -1 4 0 122.99 5.3 1 4 0 124.19 3.8 -2 -4 0 4 0.7 2 -4 0 3.5 1.3 -2 -4 0 7.6 1.2 2 -4 0 1.6 1.4 -2 -4 0 4.3 1.9 -2 4 0 3.5 1.1 2 4 0 7.3 1.9 -3 -4 0 25.9 3.8 3 -4 0 29.9 2.5 3 -4 0 42 3.7 -3 4 0 35 2.6 3 4 0 28.7 3.7 4 -4 0 97.29 5.3 -4 -4 0 81.29 5.8 4 -4 0 84.79 5.2 4 -4 0 85.69 4 -4 4 0 86.69 4.3 -4 4 0 96.49 6.6 4 4 0 83.99 5.8 -5 -4 0 66.79 5.4 5 -4 0 60.69 3.4 5 -4 0 56.49 4.2 5 4 0 62.29 5.2 -5 4 0 61.79 3.6 -5 4 0 51.99 4.7 6 -4 0 26.9 2.4 -6 -4 0 29.9 4.3 -6 4 0 33.1 3 6 4 0 27.5 3.9 -7 -4 0 -3.3 2.5 7 4 0 -4.2 2.2 -7 4 0 -1 1.1 -8 -4 0 3.9 3.4 8 4 0 5.4 3.2 -8 4 0 8.7 2.3 -9 -4 0 35.2 5.7 9 4 0 32.7 5.5 -9 4 0 32.7 4 -10 4 0 16.6 3.3 -11 4 0 0.3 2.3 0 -5 0 2.6 1.6 0 -5 0 -0.3 0.7 0 -5 0 1 1.5 0 5 0 0.8 0.8 0 5 0 2.3 1.7 -1 -5 0 5.8 1.6 -1 -5 0 7.8 2.5 1 -5 0 2.1 1.7 -1 -5 0 8.1 1.2 1 -5 0 5.6 2 -1 5 0 3.9 1.1 1 5 0 4.4 0.9 1 5 0 8.7 2.2 -1 5 0 5.6 1.9 2 -5 0 59.29 4 -2 -5 0 75.19 5.2 -2 -5 0 64.09 3.4 2 -5 0 71.09 4.8 -2 -5 0 71.59 2.9 -2 5 0 67.49 3.5 2 5 0 69.79 5 -3 -5 0 0.4 0.7 3 -5 0 4 1.6 -3 -5 0 1.7 1.9 -3 -5 0 0.9 0.5 3 -5 0 -0.4 1.4 -3 5 0 -0.3 0.9 3 5 0 2.6 1.9 4 -5 0 105.59 6.3 -4 -5 0 116.39 7.2 4 -5 0 116.09 5.2 4 5 0 122.69 7.2 -4 5 0 127.69 5.4 5 -5 0 65.19 3.8 -5 -5 0 65.89 6.1 5 -5 0 68.19 5.1 5 5 0 66.29 5.8 -5 5 0 59.59 4 -6 -5 0 44.7 5.3 6 5 0 34.2 4.6 -6 5 0 49.7 4 -7 -5 0 -2 2.2 -7 5 0 -1.2 1.7 7 5 0 1.9 3.1 -8 -5 0 79.49 8 -8 5 0 85.09 5.8 8 5 0 86.49 7.8 -9 -5 0 13 4.7 -9 5 0 12.1 3.1 9 5 0 10.2 4.1 -10 -5 0 -1.3 3.4 -10 5 0 0.7 2.4 10 5 0 5.9 3.8 0 -6 0 476.55 15.7 0 -6 0 497.25 15.5 0 6 0 432.66 15.3 0 6 0 457.85 13.3 -1 -6 0 5.9 2.7 1 -6 0 11.1 2.6 -1 -6 0 9.8 1.6 -1 -6 0 6.2 2 1 -6 0 6.1 2.1 1 6 0 9 2.7 1 6 0 8.3 1.3 -1 6 0 9.6 1.6 2 -6 0 53.19 4.2 -2 -6 0 61.89 5.2 -2 -6 0 53.59 3.6 2 -6 0 51.49 4.5 -2 -6 0 54.39 2.8 -2 6 0 53.69 3.4 2 6 0 62.39 5.1 -4 -6 0 74.89 3.4 4 -6 0 77.99 4.6 4 -6 0 68.79 5.5 -4 -6 0 73.89 2.9 -4 -6 0 74.79 6.2 -4 6 0 74.59 4.6 4 6 0 77.19 6.5 5 -6 0 47.3 4.7 -5 -6 0 43.4 5.8 5 -6 0 33.3 3.2 5 -6 0 35.6 4.7 5 6 0 46 5.6 -5 6 0 39.7 3.8 -7 -6 0 144.09 10.2 -7 6 0 138.59 7.5 7 6 0 132.49 9.3 -8 -6 0 8.9 4.1 -8 6 0 5.8 2.4 8 6 0 15 4.4 -9 -6 0 4 4.2 -9 6 0 0.2 2 9 6 0 3.4 3.6 -10 -6 0 5.8 4.4 -10 6 0 -4.8 2.6 10 6 0 0.1 3.6 0 -7 0 2.8 1.9 0 -7 0 2.2 1.7 0 7 0 2.2 1.9 -1 -7 0 66.69 3.6 1 -7 0 61.69 5.1 -1 -7 0 65.79 4.8 -1 -7 0 53.59 5.1 1 -7 0 62.09 5 1 7 0 59.29 3.1 1 7 0 63.89 5.3 -1 7 0 56.29 3.6 2 -7 0 83.79 6 -2 -7 0 56.09 5.6 2 -7 0 80.49 5.4 -2 -7 0 67.89 4.5 -2 -7 0 68.79 3.6 2 7 0 59.99 5.5 -2 7 0 71.09 4.1 3 -7 0 75.29 5.1 -3 -7 0 71.49 4.5 -3 -7 0 82.89 6.6 -3 -7 0 77.59 3.6 3 -7 0 74.59 6 -3 7 0 75.89 4.7 3 7 0 77.09 6.6 -4 -7 0 110.59 5.1 4 -7 0 99.09 7.1 -4 -7 0 104.29 8.1 -4 -7 0 106.79 4.3 -4 7 0 103.39 5.8 4 7 0 122.29 8.2 5 -7 0 54.99 4.2 -5 -7 0 47.9 2.5 -5 -7 0 37 5.7 -5 -7 0 44.7 3 -5 7 0 54.39 4.7 5 7 0 56.99 6.1 -6 -7 0 143.39 5 -6 -7 0 159.58 10.6 -6 -7 0 146.39 4.6 6 7 0 143.99 9.5 -6 7 0 147.59 7.8 7 7 0 52.19 7.2 -8 -7 0 1.8 3.3 8 7 0 1.4 3.6 -8 7 0 -3.7 2.3 -9 -7 0 -3.5 3.7 9 7 0 7.7 4.5 -9 7 0 -2.5 2.4 -10 -7 0 -3.9 4.1 -10 7 0 1.3 3 10 7 0 -1.5 3.9 0 -8 0 0.9 2.1 0 -8 0 2.4 2.1 0 8 0 2 2.2 -1 -8 0 10.9 1.9 -1 -8 0 12.3 2.7 1 -8 0 17.3 3.7 1 -8 0 13.5 3.3 -1 -8 0 11.3 3.3 1 8 0 13.1 3.2 -1 8 0 16.6 2.4 -2 -8 0 30.3 3.8 2 -8 0 25 4 2 -8 0 36.7 5.1 -2 -8 0 32.6 5.4 2 8 0 29.1 5 -2 8 0 25.7 2.9 -3 -8 0 59.09 6.8 3 -8 0 57.99 5.9 -3 -8 0 57.49 4.8 3 -8 0 57.89 5.4 -3 8 0 69.49 4.7 3 8 0 55.89 6.4 -4 -8 0 92.99 5.5 4 -8 0 84.89 7.2 -4 -8 0 99.89 8.2 4 8 0 87.99 7.4 -4 8 0 94.49 6.1 -5 -8 0 193.38 8.1 -5 -8 0 199.98 12.2 5 8 0 214.18 12.1 -5 8 0 227.48 9.8 -6 -8 0 29.9 3.1 -6 -8 0 40.5 6.7 6 8 0 31 6 -6 8 0 40 5.1 -7 -8 0 4 1.4 -7 -8 0 4.2 3.9 7 8 0 7.6 3.6 -7 8 0 2.2 2.3 -8 -8 0 9.7 4.4 8 8 0 12.1 4.3 -9 -8 0 5.2 5 9 8 0 -3.8 3.6 -9 8 0 0 3.1 0 -9 0 0.2 2.3 0 -9 0 3.8 2.7 0 9 0 3.3 2.4 1 -9 0 -0.8 2 -1 -9 0 -3 2.6 1 -9 0 0.3 2.7 -1 -9 0 -1.4 1.7 1 9 0 0.8 2.7 -2 -9 0 35.8 5.4 2 -9 0 33.9 5.6 -2 -9 0 38 4.8 2 -9 0 38.2 4.7 2 9 0 42.9 5.6 -3 -9 0 3.6 2.3 3 -9 0 2.9 2.7 -3 -9 0 0.6 2.6 3 -9 0 5.9 2.8 -3 9 0 3.8 2.2 3 9 0 2.5 2.6 4 -9 0 38.8 4.9 -4 -9 0 34.4 6.2 -4 -9 0 42.9 4.7 -4 9 0 48.7 4.8 4 9 0 43.1 6.8 -5 -9 0 56.19 7 -5 -9 0 62.79 5 -5 9 0 64.89 5.4 5 9 0 76.19 7.5 -6 -9 0 -2.4 2.9 -6 -9 0 1.9 1.9 6 9 0 -2.5 2.4 -6 9 0 2 2.2 -7 -9 0 1.3 4.5 -7 -9 0 1.1 1.8 -7 9 0 1.5 2.4 7 9 0 5.2 4.4 -8 -9 0 -1 4.6 -8 -9 0 1.1 1.6 -8 9 0 -0.1 2.7 8 9 0 1 3.4 0 -10 0 3.8 3.2 0 -10 0 4.1 3.1 1 -10 0 7.8 3.5 1 -10 0 12.4 3.7 -1 -10 0 4.1 3.6 -1 -10 0 13.1 3.4 1 10 0 6.9 4.2 2 -10 0 5.3 3.6 -2 -10 0 -1.6 2.8 -2 -10 0 1.9 2.5 2 -10 0 -2.5 2.6 2 10 0 1.3 2.8 3 -10 0 -1.4 3.6 -3 -10 0 4.2 4.1 3 -10 0 4 3.4 -3 -10 0 5.6 2.9 3 10 0 4.6 3.8 -4 -10 0 5.7 3.7 -4 -10 0 10.1 3.4 4 -10 0 13.7 4 4 10 0 6.8 3.4 -5 -10 0 -0.6 2.1 -5 -10 0 -1.3 3.4 5 10 0 0.6 3.5 -6 -10 0 0.1 2.1 -6 -10 0 0 4 6 10 0 1.6 3.6 -7 -10 0 1.5 2.3 -7 -10 0 -4.3 4.1 7 10 0 6.1 4.5 -8 -10 0 2.6 4.8 -8 -10 0 2.3 2.1 8 10 0 3.3 3.7 0 -11 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14 -3 2 -4 491.45 15.2 4 -2 4 29.9 2.4 -4 -2 -4 31.6 1.9 -4 -2 -4 23.4 2.9 -4 -2 -4 29.3 1.9 -4 2 -4 28.5 3.2 -4 2 -4 33.9 2.7 -5 -2 -4 134.39 4.6 -5 -2 -4 128.09 4.6 -5 -2 -4 127.59 6.3 -5 2 -4 137.09 5.7 -5 2 -4 133.99 6.7 -6 -2 -4 28.9 3.3 -6 -2 -4 24.3 1.9 -6 -2 -4 28.1 2 -6 2 -4 19.8 2.5 -6 2 -4 22.4 3.3 -7 -2 -4 0.4 0.9 -7 -2 -4 -1.7 1.8 -7 -2 -4 0 0.9 -7 2 -4 0.8 1.3 -8 -2 -4 8.7 1.6 -8 2 -4 7.8 2 -9 -2 -4 7.7 1.8 -9 2 -4 9.2 2.3 -10 -2 -4 1.8 1.6 -10 2 -4 3.4 2.2 -11 -2 -4 1.3 1.8 -11 2 -4 2.3 2.3 -11 -3 4 2.4 1.4 -11 3 4 8.8 2.8 -10 -3 4 0.9 1.1 -10 3 4 1 1.9 10 3 -4 -3.1 3.3 -9 -3 4 1.8 1.1 -9 3 4 -1 1.7 9 3 -4 5.7 3.8 -8 -3 4 -1.1 0.8 8 -3 -4 2.9 2.9 -8 -3 4 0.8 0.8 8 3 -4 -4.8 2.6 -8 3 4 -0.8 1.5 7 -3 -4 0 2.3 -7 3 4 1.1 1.5 7 3 -4 -0.1 2.7 6 -3 -4 2.3 2 6 3 -4 -0.7 2.7 -6 3 4 -1.9 0.9 -5 -3 4 12.6 1.1 5 -3 -4 17 3.1 5 -3 -4 9.6 2 -5 -3 4 12.6 1.3 -5 3 4 13.4 2.1 -5 3 4 12.7 2.4 5 3 -4 7.6 2.9 4 -3 -4 29.5 3.6 -4 -3 4 31.3 1.9 -4 -3 4 29.5 2 -4 3 4 31.4 3.2 -4 3 4 30 2.6 4 3 -4 32.2 3.9 -3 -3 4 79.59 3.4 -3 -3 4 80.29 3.7 3 -3 -4 80.99 4.7 3 -3 -4 82.89 4.9 -3 3 4 76.49 3.8 -3 3 4 77.59 5.5 3 3 -4 78.19 5.5 2 -3 -4 26.8 2.7 -2 -3 4 25.1 2.3 -2 -3 4 23.6 2.3 2 -3 -4 23.7 3 -2 -3 4 24.4 1.9 2 3 -4 28.2 3.2 -2 3 4 27.6 2.1 1 -3 -4 79.09 4.5 -1 -3 4 70.39 3.9 -1 -3 4 67.89 3.3 1 -3 -4 73.79 4.3 -1 3 4 71.99 3.3 1 3 -4 64.09 4.3 0 -3 4 33.9 2.8 0 -3 -4 27.7 2 0 -3 4 31.5 2.2 0 -3 -4 28.1 2.6 0 -3 -4 35.2 3.3 0 3 -4 26.1 2.6 0 3 4 33.5 2.1 0 3 -4 26.9 2.2 1 -3 4 27.2 2.9 -1 -3 -4 25.2 2.4 -1 -3 -4 21.6 1.8 -1 -3 -4 23.9 2.7 -1 3 -4 19.6 2.2 -1 3 -4 22.8 2.2 2 -3 4 217.58 8.4 -2 -3 -4 226.48 7 -2 -3 -4 231.98 7.5 -2 -3 -4 222.78 8.7 -2 3 -4 229.28 7.6 -2 3 -4 218.98 7.7 2 3 4 231.18 6.3 -3 -3 -4 176.18 5.5 -3 -3 -4 172.58 5.8 3 -3 4 161.78 6.9 -3 -3 -4 165.98 7.5 -3 3 -4 163.78 5.4 -3 3 -4 163.78 6.4 -4 -3 -4 279.17 8.2 -4 -3 -4 296.07 10.7 -4 -3 -4 278.57 8 -4 3 -4 274.87 9.4 -4 3 -4 283.57 11.2 -4 3 -4 258.47 10.6 -5 -3 -4 81.49 5.4 -5 -3 -4 82.09 3.4 5 -3 4 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1.2 1.7 -1 -4 4 0.5 0.8 -1 -4 4 0.3 1.2 1 -4 -4 4.1 1.6 1 4 -4 1.7 0.9 1 4 -4 -0.5 1.3 -1 4 4 1.2 1 0 -4 4 23 2.2 0 -4 -4 23.2 3 0 -4 4 22.1 3.1 0 -4 -4 26.2 2.2 0 -4 4 21.2 2.9 0 -4 -4 27.6 2.8 0 4 -4 22.7 2.9 0 4 -4 24.1 2.3 0 4 4 21.4 1.9 1 -4 4 164.88 7.2 -1 -4 -4 150.98 5.5 -1 -4 -4 154.68 6.4 -1 -4 -4 153.28 7.4 -1 4 -4 161.08 6 -1 4 -4 150.18 6.5 -2 -4 -4 112.09 4.4 -2 -4 -4 121.09 6.5 2 -4 4 107.69 5.9 -2 -4 -4 123.29 5.2 -2 4 -4 115.29 5.2 -2 4 -4 119.49 5.1 -3 -4 -4 34 2.4 -3 -4 -4 31.6 2 -3 -4 -4 33.7 3.9 3 -4 4 35.1 3.7 -3 4 -4 33 3 -3 4 -4 36.3 2.4 -4 -4 -4 33.7 2.3 4 -4 4 21.3 2.8 -4 -4 -4 27.9 3.8 4 -4 4 26.2 1.7 -4 -4 -4 30 2 -4 4 -4 28.5 2.8 -5 -4 -4 -0.3 2 -5 -4 -4 0.7 0.7 -5 -4 -4 1.3 0.8 -5 4 -4 1.8 1.7 -6 -4 -4 10.8 1.5 -6 -4 -4 12.4 1.4 -6 -4 -4 17.1 3.5 -6 4 -4 9.9 2.3 -7 -4 -4 7.7 1.2 -7 -4 -4 7.1 1.3 -7 -4 -4 6.8 3 -7 4 -4 7.9 2.4 -8 -4 -4 0.3 3 -8 -4 -4 1.7 1 -8 4 -4 0.2 1.9 -9 -4 -4 -0.1 1.1 -9 4 -4 1.6 2.2 -10 -4 -4 0.7 1.3 -10 4 -4 -3.7 2.1 10 5 -4 5.9 3.5 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6 -4 6.2 3 3 -6 -4 56.29 5.3 -3 -6 4 64.19 4.3 3 -6 -4 61.89 5.3 -3 -6 4 59.39 3.5 -3 6 4 66.69 4.2 3 6 -4 57.69 5.8 -2 -6 4 3.3 1.2 2 -6 -4 5.9 2.4 2 -6 -4 0 1.6 -2 -6 4 1.3 1.6 2 6 -4 5.6 2.3 -2 6 4 2.1 1.2 1 -6 -4 6.9 2.2 1 -6 -4 9.7 2.5 -1 -6 4 12.3 2.7 -1 -6 4 10.6 1.7 1 6 -4 8.8 1.5 -1 6 4 11.3 1.8 1 6 -4 10.6 2.9 0 -6 -4 361.36 13.7 0 -6 -4 366.76 13.1 0 -6 4 367.06 13.5 0 6 4 358.76 11 0 6 -4 360.76 11.5 0 6 -4 356.96 13.2 1 -6 4 66.39 5.3 -1 -6 -4 61.49 3.5 -1 -6 -4 60.89 4.4 1 -6 4 66.39 5.5 -1 -6 -4 59.89 5.5 1 6 4 58.79 3 -1 6 -4 64.99 4.8 -1 6 -4 61.19 3.9 -2 -6 -4 38.2 2.7 2 -6 4 53.49 5.2 2 -6 4 33.8 4.1 -2 -6 -4 34.9 3.6 -2 -6 -4 46.6 5.1 2 -6 4 36.7 3.8 -2 6 -4 45 3.7 -2 6 -4 38.1 3.5 -3 -6 -4 15.2 3.6 3 -6 4 10.4 3.1 3 -6 4 15.9 2.7 -3 -6 -4 10.5 1.6 -3 -6 -4 14.2 2.4 -3 6 -4 11.8 2.2 -3 6 -4 16.9 2.6 4 -6 4 2.7 1.4 -4 -6 -4 3.1 2.7 4 -6 4 -1.4 1.5 -4 -6 -4 0.6 1.1 -4 -6 -4 2.9 1 -4 6 -4 0.6 1.7 -5 -6 -4 2.7 3.1 -5 -6 -4 3.2 1 -5 -6 -4 2.5 1.3 -5 6 -4 5.3 2.3 -6 -6 -4 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24.2 3.7 -5 -3 -6 29.8 2.5 -5 -3 -6 25.9 2.6 -5 3 -6 30 3.5 -7 -3 -6 26.6 3 -7 -3 -6 32.6 4.3 -7 3 -6 35.6 4.1 -8 -3 -6 11.9 2.2 -8 3 -6 9.4 2.8 -9 -3 -6 0.4 1.6 -9 3 -6 -0.6 2.1 -10 -3 -6 -2.2 1.6 -10 3 -6 1.5 2.5 -10 -4 6 5 1.8 10 4 -6 0.2 4.2 -10 4 6 4.4 2.6 -9 -4 6 1.4 1.5 -9 4 6 -2.1 1.8 9 4 -6 3.4 3.4 8 -4 -6 18.5 4.6 -8 -4 6 22.6 2.9 -8 4 6 16.9 3.2 8 4 -6 10.3 4.9 -7 -4 6 16.5 2.7 7 -4 -6 11.2 3.9 7 4 -6 24.5 5.1 -7 4 6 16.6 2.8 -6 -4 6 0 1.3 -6 -4 6 0.7 1.2 6 -4 -6 2.2 2.7 -6 4 6 1.8 1.4 6 4 -6 1.9 3.1 5 -4 -6 75.39 6.3 -5 -4 6 77.39 4.2 -5 -4 6 77.59 4.5 5 4 -6 69.29 6.4 -5 4 6 73.49 4.7 4 -4 -6 0.5 1.6 -4 -4 6 0.4 1.1 -4 -4 6 -1.1 1.3 4 -4 -6 1.8 2.4 -4 4 6 1.2 1.2 4 4 -6 1.5 2.6 -3 -4 6 168.58 6.7 3 -4 -6 177.68 8.2 3 -4 -6 166.98 8.6 -3 -4 6 172.48 7.3 -3 4 6 167.58 6.8 3 4 -6 175.98 9 -2 -4 6 25.5 3.1 -2 -4 6 25.1 2.4 2 -4 -6 21.9 3.5 2 -4 -6 28.9 3.6 2 4 -6 28.1 2.3 2 4 -6 25.3 4.1 -2 4 6 22.8 2.4 -1 -4 6 3 1.4 -1 -4 6 3.6 1.3 1 -4 -6 3.5 2.3 1 -4 -6 9.6 2.4 -1 4 6 3.5 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3.8 0 6 -15 -6.7 3.5 -1 -6 -15 16.7 5.6 -1 6 -15 4.3 4.3 -2 -6 -15 11.6 5.3 -2 -6 -15 1.4 3.4 -3 -6 -15 -1.4 3.5 -3 -6 -15 -0.5 4.7 -2 -7 15 1.8 4.1 2 -7 -15 -1.5 4.2 2 7 -15 0.3 5.2 -1 -7 15 -2.9 4.4 1 -7 -15 3.3 4.3 1 7 -15 5.2 4.9 0 -7 -15 8.5 5.5 0 7 -15 -3.4 3.1 -1 -7 -15 -5 4.9 -1 7 -15 -5.4 4.5 -5 0 16 54.89 7.1 5 0 -16 54.49 9.2 -4 0 16 6.2 3.7 4 0 -16 15.1 5.7 3 0 -16 -7.2 3.6 -3 0 16 -0.4 2.9 2 0 -16 4 4.9 1 0 -16 -0.1 4.3 0 0 -16 5.2 4.3 -1 0 -16 8 4.9 -2 0 -16 4.2 4.5 -3 0 -16 -0.8 3.9 -5 -1 16 9.5 4.1 5 -1 -16 11.7 5.5 5 1 -16 12.8 6.2 -5 1 16 11.5 4.2 -4 -1 16 -2.1 2.3 4 -1 -16 1.5 3.7 4 1 -16 -3.3 3.5 -4 1 16 -1 3 3 -1 -16 -2 4.2 -3 -1 16 5.9 3.5 3 1 -16 10.9 4.8 2 -1 -16 -3.6 4.1 2 1 -16 -6.7 3.2 1 -1 -16 -0.2 3.9 1 1 -16 5.4 4.7 0 -1 -16 1.1 4.6 0 1 -16 5 3.8 -1 -1 -16 -2.2 4.4 -1 1 -16 -1.3 3.2 -2 -1 -16 6.7 5.1 -2 1 -16 0 3.9 -3 -1 -16 -3.1 3.8 -3 1 -16 5.1 4 -4 -1 -16 4 4 5 -2 -16 0.9 4.7 -5 -2 16 -4.1 2.9 5 2 -16 -0.7 4.9 -5 2 16 3.3 3.5 4 -2 -16 2.2 4.5 -4 -2 16 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-5 -16 1.5 3.8 3 5 -16 8 5.6 -2 -5 16 -0.5 2.7 2 -5 -16 0.4 3.9 2 5 -16 5.8 5.5 1 -5 -16 0.5 4.6 1 5 -16 -2.2 4.6 0 -5 -16 2.8 4.6 0 5 -16 4 4.5 -1 -5 -16 3.2 5.3 -1 5 -16 -0.4 4 -2 -5 -16 -5.4 3.7 1 -6 -16 8.2 4.8 1 6 -16 15.1 5.2 0 -6 -16 10.8 5.7 0 6 -16 6.6 5.4 3 0 -17 -4.4 3.6 2 0 -17 -0.8 4.2 1 0 -17 -3.6 3.6 0 0 -17 1.5 5.1 -1 0 -17 -4.8 4 -2 0 -17 -1.6 4.2 3 -1 -17 3.8 4.3 3 1 -17 10.9 5.4 2 -1 -17 4.3 5.3 2 1 -17 1.1 4.3 1 -1 -17 4.5 4.8 1 1 -17 4.3 5.2 0 -1 -17 -8.6 4.2 0 1 -17 4.4 5.4 -1 -1 -17 1 4.1 -1 1 -17 6.1 5.4 -2 -1 -17 6.6 5.4 -2 1 -17 -0.3 3.6 3 -2 -17 30 7.9 3 2 -17 28.4 7.1 2 -2 -17 9.3 5 2 2 -17 -6.4 4.4 1 -2 -17 8.6 4.9 1 2 -17 -5.8 4 0 -2 -17 6.4 4.8 0 2 -17 12.2 5.6 -1 -2 -17 0.5 5 -1 2 -17 2.5 4.4 -2 -2 -17 -7.4 4 -2 2 -17 3.5 4.2 2 -3 -17 4 5.5 2 3 -17 6.9 5.8 1 -3 -17 14.9 6.1 1 3 -17 13.2 5.3 0 -3 -17 2 5.4 0 3 -17 9.8 5.3 -1 -3 -17 -2.8 5 -1 3 -17 4.8 4.9 1 -4 -17 3.2 4.8 1 4 -17 -4.9 3.5 0 -4 -17 -5.1 3.8 0 4 -17 -1.5 4.3 _iucr_refine_instructions_details ; TITL 18gtu282_a.res in P2(1)/c 18gtu282.res created by SHELXL-2018/3 at 00:17:50 on 17-Oct-2018 REM Old TITL 18gtu282 in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.313, Rweak 0.029, Alpha 0.050 REM 0.954 for 169 systematic absences, Orientation as input REM Formula found by SHELXT: C17 N4 CELL 0.71073 9.8605 11.7357 14.9221 90 92.649 90 ZERR 2 0.0008 0.001 0.0012 0 0.005 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 80 88 4 4 DFIX 1.55 C20 C19 DFIX 1.55 C19 C18 DFIX 1.55 C18 C17 DFIX 1.55 C17 C16 DFIX 1.55 C16 C15 DFIX 1.55 C15 C14 DFIX 1.55 C21 C22 DFIX 1.55 C22 C23 DFIX 1.55 C23 C24 DFIX 1.55 C24 C25 DFIX 1.55 C25 C26 DFIX 1.55 C26 C27 SADI C13 C16 C13 C25 SADI C16 C15 C25 C26 SADI C16 C17 C25 C24 SADI C15 C14 C26 C27 SADI C17 C18 C24 C23 SADI C19 C18 C22 C23 SADI C19 C20 C22 C21 SADI 0.04 C13 C15 C13 C26 SADI 0.04 C13 C17 C13 C24 SADI 0.04 C16 C18 C25 C23 SADI 0.04 C16 C14 C25 C27 SADI 0.04 C15 C17 C26 C24 SADI 0.04 C17 C19 C24 C22 SADI 0.04 C18 C20 C23 C21 SIMU 0.02 0.08 1.7 C19 C20 SIMU 0.02 0.08 1.7 C18 C19 SIMU 0.02 0.08 1.7 C17 C18 SIMU 0.02 0.08 1.7 C16 C17 SIMU 0.02 0.08 1.7 C15 C16 SIMU 0.02 0.08 1.7 C14 C15 SIMU 0.02 0.08 1.7 C26 C27 SIMU 0.02 0.08 1.7 C25 C26 SIMU 0.02 0.08 1.7 C24 C25 SIMU 0.02 0.08 1.7 C23 C24 SIMU 0.02 0.08 1.7 C22 C23 SIMU 0.02 0.08 1.7 C21 C22 RIGU C14 > C20 RIGU C21 > C27 L.S. 20 PLAN 5 SIZE 0.13 0.168 0.381 TEMP -100.16 BOND list 4 fmap 2 acta OMIT 0 6 3 OMIT 7 7 0 OMIT 3 9 6 OMIT 6 6 3 OMIT 8 8 4 OMIT 4 9 7 OMIT 1 0 2 OMIT 8 0 0 OMIT -1 4 1 OMIT 1 2 2 OMIT 4 2 1 OMIT -1 0 8 OMIT 1 6 2 OMIT 6 3 0 OMIT 0 8 4 OMIT 9 2 4 OMIT 8 0 6 OMIT 1 1 8 OMIT -3 1 1 OMIT 6 0 0 OMIT 0 4 8 REM REM REM WGHT 0.091100 0.656000 FVAR 0.53762 0.47990 O1 4 0.448386 0.533297 0.678180 11.00000 0.07940 0.11381 = 0.05383 -0.01853 0.02193 -0.04929 N1 3 0.865022 0.898177 0.525942 11.00000 0.10204 0.06711 = 0.04309 -0.00304 0.01435 -0.01358 C1 1 0.880442 0.884557 0.451381 11.00000 0.06636 0.04944 = 0.03873 0.00094 0.00623 -0.00979 C2 1 0.898903 0.864925 0.357715 11.00000 0.05410 0.04477 = 0.03769 0.00455 0.00898 -0.00531 C3 1 0.972187 0.941773 0.308452 11.00000 0.08226 0.05929 = 0.04431 -0.00165 0.01399 -0.02701 AFIX 43 H3 2 1.010241 1.007879 0.336433 11.00000 -1.20000 AFIX 0 C4 1 0.989434 0.921722 0.218898 11.00000 0.09168 0.07057 = 0.04797 0.00976 0.01750 -0.02703 AFIX 43 H4 2 1.039883 0.974001 0.185031 11.00000 -1.20000 AFIX 0 C5 1 0.933884 0.826168 0.178071 11.00000 0.08029 0.07402 = 0.03777 -0.00177 0.01743 -0.01056 AFIX 43 H5 2 0.946271 0.813080 0.116157 11.00000 -1.20000 AFIX 0 C6 1 0.860499 0.749369 0.226213 11.00000 0.05404 0.05517 = 0.04387 -0.00838 0.00743 -0.00490 AFIX 43 H6 2 0.822436 0.683921 0.197259 11.00000 -1.20000 AFIX 0 C7 1 0.841838 0.767281 0.317271 11.00000 0.04012 0.04537 = 0.03735 0.00148 0.00744 -0.00017 C8 1 0.762815 0.690726 0.367751 11.00000 0.04238 0.04365 = 0.04410 0.00040 0.00585 -0.00254 C9 1 0.690863 0.631473 0.409883 11.00000 0.04472 0.04905 = 0.04740 0.00163 0.00333 -0.00115 C10 1 0.596358 0.563334 0.456746 11.00000 0.04071 0.04840 = 0.04710 0.00534 0.00544 -0.00312 C11 1 0.574114 0.582900 0.546935 11.00000 0.05337 0.05392 = 0.05186 -0.00320 0.00604 -0.01551 AFIX 43 H11 2 0.625151 0.639808 0.578743 11.00000 -1.20000 AFIX 0 C12 1 0.478715 0.520457 0.590501 11.00000 0.05293 0.05719 = 0.04400 -0.00036 0.01102 -0.00848 C13 1 0.538996 0.594044 0.737640 11.00000 0.08779 0.08722 = 0.05477 -0.01430 0.00992 -0.02640 PART 1 AFIX 23 H13A 2 0.532792 0.677008 0.726158 21.00000 -1.20000 H13B 2 0.633794 0.569172 0.730375 21.00000 -1.20000 AFIX 23 PART 0 PART 2 H13C 2 0.560883 0.668879 0.711308 -21.00000 -1.20000 H13D 2 0.624553 0.550680 0.747250 -21.00000 -1.20000 AFIX 0 PART 0 PART 1 C14 1 0.639074 0.390129 0.870629 21.00000 0.12429 0.15844 = 0.12498 -0.03752 -0.03676 -0.02021 AFIX 137 H14A 2 0.675620 0.385852 0.810755 21.00000 -1.50000 H14B 2 0.635505 0.313484 0.896485 21.00000 -1.50000 H14C 2 0.697773 0.438682 0.909215 21.00000 -1.50000 AFIX 0 C15 1 0.496231 0.440561 0.863514 21.00000 0.10077 0.09700 = 0.06997 -0.04986 0.02930 -0.04036 AFIX 23 H15A 2 0.440606 0.395792 0.819227 21.00000 -1.20000 H15B 2 0.454608 0.432789 0.922321 21.00000 -1.20000 AFIX 0 C16 1 0.491853 0.564632 0.835986 21.00000 0.12034 0.08045 = 0.12324 -0.05318 0.05451 -0.04280 AFIX 13 H16 2 0.552979 0.607290 0.879535 21.00000 -1.20000 AFIX 0 C17 1 0.350577 0.612643 0.843261 21.00000 0.12716 0.10746 = 0.14615 -0.00809 0.04436 -0.03372 AFIX 23 H17A 2 0.308856 0.579608 0.896468 21.00000 -1.20000 H17B 2 0.294071 0.590533 0.789496 21.00000 -1.20000 AFIX 0 C18 1 0.352424 0.741563 0.851384 21.00000 0.12906 0.10469 = 0.20898 -0.00844 0.02275 -0.01546 AFIX 23 H18A 2 0.379034 0.774748 0.793785 21.00000 -1.20000 H18B 2 0.421853 0.763891 0.898146 21.00000 -1.20000 AFIX 0 C19 1 0.214487 0.791366 0.875389 21.00000 0.12535 0.13713 = 0.25775 0.00584 0.02324 -0.00946 AFIX 23 H19A 2 0.211606 0.870541 0.852484 21.00000 -1.20000 H19B 2 0.144126 0.748391 0.840041 21.00000 -1.20000 AFIX 0 C20 1 0.168643 0.795794 0.971600 21.00000 0.11598 0.28075 = 0.26324 -0.03623 0.02550 -0.01662 AFIX 137 H20A 2 0.069690 0.787924 0.971481 21.00000 -1.50000 H20B 2 0.195515 0.868864 0.998802 21.00000 -1.50000 H20C 2 0.211277 0.733437 1.006309 21.00000 -1.50000 AFIX 0 PART 0 PART 2 C21 1 0.124675 0.864726 0.972812 -21.00000 0.07816 0.11111 = 0.08715 -0.01115 0.02063 -0.02161 AFIX 137 H21A 2 0.070444 0.933753 0.961957 -21.00000 -1.50000 H21B 2 0.189016 0.877244 1.023893 -21.00000 -1.50000 H21C 2 0.064544 0.801024 0.986067 -21.00000 -1.50000 AFIX 0 C22 1 0.202786 0.836864 0.889294 -21.00000 0.07636 0.08859 = 0.06695 0.00092 0.01221 -0.03503 AFIX 23 H22A 2 0.261751 0.902133 0.875230 -21.00000 -1.20000 H22B 2 0.137565 0.825284 0.837652 -21.00000 -1.20000 AFIX 0 C23 1 0.291458 0.728225 0.902829 -21.00000 0.07396 0.09472 = 0.03672 -0.00259 0.01574 -0.02660 AFIX 23 H23A 2 0.360712 0.741031 0.951959 -21.00000 -1.20000 H23B 2 0.233701 0.663455 0.919861 -21.00000 -1.20000 AFIX 0 C24 1 0.361598 0.699686 0.815948 -21.00000 0.08603 0.09033 = 0.05426 -0.00873 0.03119 -0.03748 AFIX 23 H24A 2 0.292408 0.671868 0.770974 -21.00000 -1.20000 H24B 2 0.401141 0.770387 0.792087 -21.00000 -1.20000 AFIX 0 C25 1 0.472247 0.611341 0.827264 -21.00000 0.10180 0.08648 = 0.04566 -0.01676 0.02799 -0.02219 AFIX 13 H25 2 0.543497 0.645452 0.868928 -21.00000 -1.20000 AFIX 0 C26 1 0.436992 0.500505 0.866487 -21.00000 0.16627 0.08896 = 0.06921 -0.01825 0.04502 -0.03508 AFIX 23 H26A 2 0.367248 0.462560 0.827053 -21.00000 -1.20000 H26B 2 0.397923 0.513075 0.925616 -21.00000 -1.20000 AFIX 0 C27 1 0.563056 0.421973 0.878212 -21.00000 0.25331 0.08463 = 0.11481 0.03040 0.07745 0.03128 AFIX 137 H27A 2 0.596721 0.403466 0.819178 -21.00000 -1.50000 H27B 2 0.537779 0.351604 0.908615 -21.00000 -1.50000 H27C 2 0.634331 0.461223 0.914252 -21.00000 -1.50000 AFIX 0 HKLF 4 REM 18gtu282_a.res in P2(1)/c REM wR2 = 0.2066, GooF = S = 1.033, Restrained GooF = 1.033 for all data REM R1 = 0.0693 for 1644 Fo > 4sig(Fo) and 0.1326 for all 3012 data REM 267 parameters refined using 164 restraints END WGHT 0.0920 0.6211 REM Highest difference peak 0.265, deepest hole -0.187, 1-sigma level 0.041 Q1 1 0.6426 0.3023 0.9247 11.00000 0.05 0.27 Q2 1 0.2130 0.7250 1.0739 11.00000 0.05 0.24 Q3 1 0.2578 0.7403 0.7786 11.00000 0.05 0.22 Q4 1 0.5049 0.5606 0.9067 11.00000 0.05 0.21 Q5 1 0.3861 0.5898 0.6423 11.00000 0.05 0.21 REM The information below was added by Olex2. REM REM R1 = 0.0693 for 1644 Fo > 4sig(Fo) and 0.1326 for all 12289 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.27, deepest hole -0.19 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1326 REM R1_gt = 0.0693 REM wR_ref = 0.2066 REM GOOF = 1.033 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 12289 REM Reflections_gt = 1644 REM Parameters = n/a REM Hole = -0.19 REM Peak = 0.27 REM Flack = n/a ; _olex2_submission_special_instructions 'No special instructions were received'