# CIF-file generated for cu_ModSa3_P 21/no R = 0.03 #============================================================================== data_global #============================================================================== # 0. AUDIT DETAILS _audit_creation_date 'Wednesday, 7 November 20' _audit_creation_method 'PLATON option' _audit_update_record ; ; #=============================================================================== # 1. SUBMISSION DETAILS # Name and address of author for X-ray correspondence _publ_contact_author_name # Name of author for correspondence ; Dr. Alexander P\"othig ; _publ_contact_author_address # address of author for correspondence ; Catalysis Research Center Technische Universit\"at M\"unchen Ernst-Otto-Fischer-Str. 1 85747 Garching bei M\"unchen Germany ; _publ_contact_author_email alexander.poethig@tum.de _publ_contact_author_fax '+49(0)89 289 54128' _publ_contact_author_phone '+49(0)89 289 54149' _publ_requested_journal 'J. Organ. Chem.' _publ_contact_letter # Include date of submission ; Date of submission: November 2018 ; #=============================================================================== # 2. PROCESSING SUMMARY (JOURNAL OFFICE ONLY) #=============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; [6 pi] Photocyclization to cis-Hexahydrocarbazol-4-ones: Substrate Modification Mechanism and Scope ; _publ_section_title_footnote ; ; # The loop structure below should contain the names and adresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Modha, S. G.' ; # author related footnote ? ; ; Catalysis Research Center & Department Chemie Technische Universit\"at M\"unchen Lichtenbergstr. 4 85747 Garching bei M\"unchen Germany ; 'P\"othig, A.' ; # author related footnote ? ; ; Catalysis Research Center & Department Chemie Technische Universit\"at M\"unchen Lichtenbergstr. 4 85747 Garching bei M\"unchen Germany ; 'Dreuw, A.' ; # author related footnote ? ; ; Interdisciplinary Center for Scientific Computing Ruprecht-Karls University Im Neuenheimer Feld 205A 69120 Heidelberg Germany ; 'Bach, Th.' ; # author related footnote ? ; ; Catalysis Research Center & Department Chemie Technische Universit\"at M\"unchen Lichtenbergstr. 4 85747 Garching bei M\"unchen Germany ; #=============================================================================== # 4. TEXT _publ_section_synopsis ; ? ; _publ_section_abstract ; Upon irradiation at 366 nm, tertiary N-alkoxycarbonyl-N-aryl-beta-enaminones furnished exclusively the trans-hexahydrocarbazol-4-ones via conrotatory [6 pi] photocyclization, but epimerized on silica to cis-hexahydrocarbazol-4 -ones. Acceptor substitution on the nitrogen atom enhanced the stability of the cyclized products compared to N-alkyl-N-aryl-beta-enaminones reported previously. The mechanism of this [6 pi] photocyclization was investigated by quenching experiments, deuterium labelling experiments and DFT calculations suggesting a triplet pathway for the conrotatory ring closure followed by a suprafacial [1,4]-hydrogen migration. ; # Insert blank lines between paragraphs _publ_section_comment ; ; _publ_section_exptl_prep ; The crystal was fixed on the top of a microsampler with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Solution and refinements with the program APEX (Bruker 2013) and SHELXL2014 (Sheldrick, 2014)in conjunction with SHELXLE (Huebschle, 2011). Hydrogen atoms could not be located in the difference Fourier maps and were calculated in ideal positions (riding model). Hydroxy hydrogen atoms could be located in the difference Fourier maps and were allowed to refine freely. ; # Insert blank lines between references _publ_section_references ; Allen, F. H.(2004). ENCIFER. J. Applied Cryst. 37, 335-338. Bruker (2013). APEX suite of crystallographic software. APEX 2 Version 2013.4. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2012). SAINT, Version 8.27b and SADABS Version 2012/1. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2008b). SAINT, Version 7.56a and TWINABS Version 2008/1. Bruker AXS Inc., Madison, Wisconsin, USA. Flack, H.D. (1983). Acta Cryst. A39, 876-881. Huebschle, C. B.; Sheldrick, G. M.; Dittrich, B. (2011). SHELXLE. J. Appl. Cryst., 44, (2011) 1281 - 1284. Sheldrick, G. M. (1997). SHELXS97. University of G\"ottingen, Germany. Sheldrick, G. M. (2014). SHELXL2014. University of G\"ottingen, Germany. Spek, A. L. (2011). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13. Wilson, A.J.C. (1992). Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_acknowledgements ; ; _publ_section_figure_captions ; View of the title compound with the atom numbering scheme. Displacement ellipsoids for non-H atoms are drawn at the 50% probability level. ; #=============================================================================== data_cu_modsa3_0m-auto #=============================================================================== # 5. CHEMICAL DATA _chemical_formula_moiety 'C14 H15 N O4' _chemical_formula_sum 'C14 H15 N O4' _chemical_formula_weight 261.27 _chemical_compound_source 'see text' 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' N N 0.0311 0.0180 ' 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' #=============================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' _symmetry_Int_Tables_number 14 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 1/2-x,1/2+y,1/2-z 3 -x,-y,-z 4 1/2+x,1/2-y,1/2+z _cell_length_a 7.1881(19) _cell_length_b 16.816(6) _cell_length_c 10.435(4) _cell_angle_alpha 90 _cell_angle_beta 99.549(12) _cell_angle_gamma 90 _cell_volume 1243.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100 _cell_measurement_reflns_used 9846 _cell_measurement_theta_min 5.0380 _cell_measurement_theta_max 68.1556 _exptl_crystal_description 'fragment' _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.343 _exptl_crystal_size_mid 0.209 _exptl_crystal_size_min 0.091 _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'Not Measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 0.855 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'SADABS 2014/5, Bruker, 2014' _exptl_absorpt_correction_T_min 0.6742 _exptl_absorpt_correction_T_max 0.7531 #=============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; Diffractometer operator A. Poethig scanspeed 30 s per frame dx 34 mm 1791 frames measured in 24 data sets phi-scans with delta_phi = 0.5 omega-scans with delta_omega = 0.5 ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_probe 'x-ray' _diffrn_radiation_type 'CuK\a' _diffrn_radiation_source 'IMS microsource' _diffrn_radiation_monochromator 'HELIOS optic' _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Bruker Photon CMOS ' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CMOS plate ' _diffrn_detector_area_resol_mean 16 # number of measured reflections (redundant set) _diffrn_reflns_number 28372 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_unetI/netI 0.0152 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 5.04 _diffrn_reflns_theta_max 68.45 _diffrn_reflns_theta_full 67.68 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_reduction_process ; ; # number of unique reflections _reflns_number_total 2281 # number of observed reflections (> n sig(I)) _reflns_number_gt 2141 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX III Control Software (Bruker, 2015)' _computing_cell_refinement 'SAINT (Bruker, 2015)' _computing_data_reduction 'SAINT (Bruker, 2015)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL2014 (Sheldrick, 2014), SHELXLE (Huebschle, 2011)' _computing_molecular_graphics 'PLATON (Spek, 2011)' _computing_publication_material 'PLATON (Spek, 2011), enCIFer (Allen, 2014)' #=============================================================================== # 8. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except those flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating -R-factor-obs 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 'W=1/[\S^2^(FO^2^)+(0.0381P)^2^+0.6700P] WHERE P=(FO^2^+2FC^2^)/3' _atom_sites_solution_primary '?' _atom_sites_solution_secondary '?' _atom_sites_solution_hydrogens 'mixed' _refine_ls_hydrogen_treatment 'mixed' _refine_ls_extinction_method 'none' _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack . _refine_ls_number_reflns 2281 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0832 _refine_ls_wR_factor_gt 0.0815 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.264 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.046 #=============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O4A O Uani 0.07456(12) 0.36134(5) 0.67699(9) 1.000 0.0175(3) d . . . O10 O Uani 0.24653(14) 0.42044(6) 0.90702(9) 1.000 0.0237(3) d . . . O12 O Uani 0.36552(13) 0.20670(5) 0.35344(8) 1.000 0.0171(3) d . . . O13 O Uani 0.36130(12) 0.34090(5) 0.33270(8) 1.000 0.0158(3) d . . . N9 N Uani 0.34836(15) 0.28769(6) 0.52610(10) 1.000 0.0137(3) d . . . C1 C Uani 0.56122(18) 0.39746(8) 0.61028(12) 1.000 0.0160(3) d . . . C2 C Uani 0.58815(19) 0.46611(8) 0.70683(12) 1.000 0.0200(4) d . . . C3 C Uani 0.54609(19) 0.43785(8) 0.83862(12) 1.000 0.0195(4) d . . . C4 C Uani 0.34835(19) 0.40696(7) 0.82743(12) 1.000 0.0163(4) d . . . C4A C Uani 0.27377(17) 0.35324(7) 0.71102(11) 1.000 0.0140(3) d . . . C4B C Uani 0.32912(17) 0.26691(7) 0.74027(12) 1.000 0.0138(3) d . . . C5 C Uani 0.34208(17) 0.22419(8) 0.85477(12) 1.000 0.0159(4) d . . . C6 C Uani 0.37987(17) 0.14295(8) 0.85274(12) 1.000 0.0173(4) d . . . C7 C Uani 0.40212(17) 0.10608(8) 0.73671(12) 1.000 0.0173(3) d . . . C8 C Uani 0.39195(17) 0.14858(7) 0.62073(12) 1.000 0.0157(3) d . . . C8A C Uani 0.35747(17) 0.22973(7) 0.62510(11) 1.000 0.0133(3) d . . . C9A C Uani 0.35705(17) 0.36811(7) 0.58570(11) 1.000 0.0135(3) d . . . C11 C Uani 0.35961(17) 0.27299(7) 0.39956(11) 1.000 0.0131(3) d . . . C14 C Uani 0.36996(18) 0.33219(8) 0.19568(11) 1.000 0.0171(4) d . . . H1A H Uiso 0.64560 0.35310 0.64440 1.000 0.0190 c RU . . H1B H Uiso 0.59690 0.41500 0.52710 1.000 0.0190 c RU . . H2A H Uiso 0.50230 0.51030 0.67420 1.000 0.0240 c RU . . H2B H Uiso 0.71950 0.48590 0.71670 1.000 0.0240 c RU . . H3A H Uiso 0.63600 0.39530 0.87260 1.000 0.0230 c RU . . H3B H Uiso 0.56380 0.48260 0.90100 1.000 0.0230 c RU . . H4A H Uiso 0.024(3) 0.3448(12) 0.7418(19) 1.000 0.043(5) d . . . H5 H Uiso 0.32550 0.24980 0.93330 1.000 0.0190 c RU . . H6 H Uiso 0.39050 0.11270 0.93050 1.000 0.0210 c RU . . H7 H Uiso 0.42490 0.05040 0.73640 1.000 0.0210 c RU . . H8 H Uiso 0.40800 0.12300 0.54210 1.000 0.0190 c RU . . H9A H Uiso 0.27550 0.40600 0.52750 1.000 0.0160 c RU . . H14A H Uiso 0.28480 0.28940 0.15900 1.000 0.0260 c RU . . H14B H Uiso 0.49930 0.31910 0.18490 1.000 0.0260 c RU . . H14C H Uiso 0.33160 0.38210 0.15050 1.000 0.0260 c RU . . 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 O4A 0.0146(5) 0.0252(5) 0.0133(4) 0.0034(4) 0.0040(4) 0.0029(4) O10 0.0334(6) 0.0249(5) 0.0150(5) -0.0033(4) 0.0101(4) 0.0014(4) O12 0.0210(5) 0.0177(5) 0.0135(4) -0.0042(3) 0.0054(4) -0.0029(3) O13 0.0217(5) 0.0178(4) 0.0083(4) -0.0003(3) 0.0033(3) -0.0004(3) N9 0.0175(5) 0.0136(5) 0.0101(5) -0.0008(4) 0.0028(4) -0.0011(4) C1 0.0168(6) 0.0179(6) 0.0135(6) -0.0014(5) 0.0033(5) -0.0011(5) C2 0.0228(7) 0.0187(6) 0.0181(6) -0.0032(5) 0.0025(5) -0.0038(5) C3 0.0232(7) 0.0199(6) 0.0141(6) -0.0049(5) -0.0009(5) 0.0010(5) C4 0.0248(7) 0.0134(6) 0.0104(6) 0.0017(5) 0.0024(5) 0.0048(5) C4A 0.0147(6) 0.0172(6) 0.0102(6) 0.0005(5) 0.0022(5) 0.0009(5) C4B 0.0110(6) 0.0171(6) 0.0127(6) -0.0009(5) 0.0005(5) -0.0012(5) C5 0.0140(6) 0.0220(7) 0.0117(6) 0.0001(5) 0.0019(5) -0.0011(5) C6 0.0132(6) 0.0220(7) 0.0159(6) 0.0050(5) 0.0001(5) -0.0018(5) C7 0.0134(6) 0.0159(6) 0.0216(6) 0.0011(5) 0.0000(5) -0.0012(5) C8 0.0134(6) 0.0174(6) 0.0160(6) -0.0021(5) 0.0016(5) -0.0019(5) C8A 0.0104(6) 0.0177(6) 0.0113(6) 0.0002(5) 0.0007(4) -0.0020(5) C9A 0.0174(6) 0.0139(6) 0.0093(6) -0.0013(4) 0.0027(5) 0.0005(5) C11 0.0102(6) 0.0176(6) 0.0114(6) -0.0013(5) 0.0017(4) -0.0020(5) C14 0.0192(7) 0.0245(7) 0.0081(6) -0.0006(5) 0.0037(5) 0.0000(5) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O4A C4A 1.4235(16) . . yes O10 C4 1.2159(17) . . yes O12 C11 1.2177(15) . . yes O13 C11 1.3393(15) . . yes O13 C14 1.4489(15) . . yes O4A H4A 0.87(2) . . no N9 C8A 1.4139(16) . . yes N9 C11 1.3589(16) . . yes N9 C9A 1.4855(16) . . yes C1 C9A 1.5292(19) . . no C1 C2 1.5233(19) . . no C2 C3 1.5318(19) . . no C3 C4 1.500(2) . . no C4 C4A 1.5372(18) . . no C4A C4B 1.5227(18) . . no C4A C9A 1.5462(17) . . no C4B C8A 1.3993(18) . . no C4B C5 1.3840(18) . . no C5 C6 1.394(2) . . no C6 C7 1.3929(19) . . no C7 C8 1.3970(18) . . no C8 C8A 1.3890(18) . . no C1 H1A 0.9900 . . no C1 H1B 0.9900 . . no C2 H2A 0.9900 . . no C2 H2B 0.9900 . . no C3 H3A 0.9900 . . no C3 H3B 0.9900 . . no C5 H5 0.9500 . . no C6 H6 0.9500 . . no C7 H7 0.9500 . . no C8 H8 0.9500 . . no C9A H9A 1.0000 . . no C14 H14A 0.9800 . . no C14 H14B 0.9800 . . no C14 H14C 0.9800 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 O13 C14 115.69(9) . . . yes C4A O4A H4A 108.1(14) . . . no C8A N9 C11 125.56(10) . . . yes C9A N9 C11 124.56(10) . . . yes C8A N9 C9A 109.15(9) . . . yes C2 C1 C9A 111.63(11) . . . no C1 C2 C3 109.65(11) . . . no C2 C3 C4 111.30(11) . . . no O10 C4 C4A 118.61(12) . . . yes C3 C4 C4A 117.83(11) . . . no O10 C4 C3 123.53(11) . . . yes O4A C4A C4B 111.09(10) . . . yes O4A C4A C9A 106.75(9) . . . yes C4 C4A C4B 110.89(10) . . . no C4 C4A C9A 116.11(10) . . . no C4B C4A C9A 101.47(9) . . . no O4A C4A C4 110.21(10) . . . yes C4A C4B C5 130.23(11) . . . no C5 C4B C8A 120.73(11) . . . no C4A C4B C8A 108.92(10) . . . no C4B C5 C6 118.75(11) . . . no C5 C6 C7 120.02(12) . . . no C6 C7 C8 121.89(12) . . . no C7 C8 C8A 117.27(11) . . . no N9 C8A C4B 108.90(10) . . . yes N9 C8A C8 129.80(11) . . . yes C4B C8A C8 121.29(11) . . . no N9 C9A C4A 102.22(9) . . . yes C1 C9A C4A 113.94(10) . . . no N9 C9A C1 109.67(10) . . . yes O12 C11 N9 124.21(11) . . . yes O13 C11 N9 110.99(10) . . . yes O12 C11 O13 124.80(11) . . . yes C2 C1 H1A 109.00 . . . no C2 C1 H1B 109.00 . . . no C9A C1 H1A 109.00 . . . no C9A C1 H1B 109.00 . . . no H1A C1 H1B 108.00 . . . no C1 C2 H2A 110.00 . . . no C1 C2 H2B 110.00 . . . no C3 C2 H2A 110.00 . . . no C3 C2 H2B 110.00 . . . no H2A C2 H2B 108.00 . . . no C2 C3 H3A 109.00 . . . no C2 C3 H3B 109.00 . . . no C4 C3 H3A 109.00 . . . no C4 C3 H3B 109.00 . . . no H3A C3 H3B 108.00 . . . no C4B C5 H5 121.00 . . . no C6 C5 H5 121.00 . . . no C5 C6 H6 120.00 . . . no C7 C6 H6 120.00 . . . no C6 C7 H7 119.00 . . . no C8 C7 H7 119.00 . . . no C7 C8 H8 121.00 . . . no C8A C8 H8 121.00 . . . no N9 C9A H9A 110.00 . . . no C1 C9A H9A 110.00 . . . no C4A C9A H9A 110.00 . . . no O13 C14 H14A 109.00 . . . no O13 C14 H14B 109.00 . . . no O13 C14 H14C 109.00 . . . no H14A C14 H14B 109.00 . . . no H14A C14 H14C 109.00 . . . no H14B C14 H14C 110.00 . . . no 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 C14 O13 C11 O12 0.31(18) . . . . no C14 O13 C11 N9 -179.04(10) . . . . no C9A N9 C8A C4B 13.08(14) . . . . no C9A N9 C8A C8 -165.55(13) . . . . no C11 N9 C8A C4B -176.37(12) . . . . no C11 N9 C8A C8 5.0(2) . . . . no C8A N9 C9A C1 94.04(11) . . . . no C8A N9 C9A C4A -27.18(12) . . . . no C11 N9 C9A C1 -76.62(14) . . . . no C11 N9 C9A C4A 162.16(11) . . . . no C8A N9 C11 O12 5.5(2) . . . . no C8A N9 C11 O13 -175.10(11) . . . . no C9A N9 C11 O12 174.69(12) . . . . no C9A N9 C11 O13 -5.96(17) . . . . no C9A C1 C2 C3 62.78(14) . . . . no C2 C1 C9A N9 -162.46(10) . . . . no C2 C1 C9A C4A -48.60(14) . . . . no C1 C2 C3 C4 -59.07(14) . . . . no C2 C3 C4 O10 -138.93(13) . . . . no C2 C3 C4 C4A 43.07(15) . . . . no O10 C4 C4A O4A 30.84(15) . . . . no O10 C4 C4A C4B -92.58(14) . . . . no O10 C4 C4A C9A 152.33(11) . . . . no C3 C4 C4A O4A -151.06(10) . . . . no C3 C4 C4A C4B 85.51(13) . . . . no C3 C4 C4A C9A -29.57(15) . . . . no O4A C4A C4B C5 -86.26(16) . . . . no O4A C4A C4B C8A 89.72(12) . . . . no C4 C4A C4B C5 36.66(18) . . . . no C4 C4A C4B C8A -147.37(11) . . . . no C9A C4A C4B C5 160.58(13) . . . . no C9A C4A C4B C8A -23.44(13) . . . . no O4A C4A C9A N9 -87.00(10) . . . . no O4A C4A C9A C1 154.78(10) . . . . no C4 C4A C9A N9 149.69(10) . . . . no C4 C4A C9A C1 31.47(15) . . . . no C4B C4A C9A N9 29.39(11) . . . . no C4B C4A C9A C1 -88.84(12) . . . . no C4A C4B C5 C6 174.18(12) . . . . no C8A C4B C5 C6 -1.39(19) . . . . no C4A C4B C8A N9 7.38(14) . . . . no C4A C4B C8A C8 -173.85(11) . . . . no C5 C4B C8A N9 -176.19(11) . . . . no C5 C4B C8A C8 2.57(19) . . . . no C4B C5 C6 C7 -0.59(18) . . . . no C5 C6 C7 C8 1.48(19) . . . . no C6 C7 C8 C8A -0.34(18) . . . . no C7 C8 C8A N9 176.82(12) . . . . no C7 C8 C8A C4B -1.66(18) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag # #D H A D - H H...A D...A D - H...A symm(A) # O4A H4A O12 0.87(2) 1.96(2) 2.8063(17) 165(2) 4_455 yes C3 H3A O12 0.9900 2.4100 3.330(2) 154.00 4_555 yes C8 H8 O12 0.9500 2.4000 2.9317(19) 115.00 . yes C14 H14C O10 0.9800 2.5900 3.343(2) 133.00 1_554 yes # Loop Mechanism for Extra Tables(s) #loop_ #_publ_manuscript_incl_extra_item #'_geom_extra_tableA_col_1' #'_geom_extra_tableA_col_2' #'_geom_extra_tableA_col_3' #'_geom_extra_table_head_A' #'_geom_table_footnote_A' #'_geom_extra_tableB_col_1' #'_geom_extra_tableB_col_2' #'_geom_extra_tableB_col_3' #'_geom_extra_table_head_B' #'_geom_table_footnote_B' # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 # ? ? ? # #loop_ #_geom_extra_tableB_col_1 #_geom_extra_tableB_col_2 #_geom_extra_tableB_col_3 # ? ? ? # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; # #_geom_table_footnote_A #; # ? #; # #_geom_table_footnote_B #; # ? #; _shelx_res_file ; cu_ModSa3_0m-auto.res created by SHELXL-2014/7 TITL cu_ModSa3_0m_a.res in P2(1)/n CELL 1.54178 7.1881 16.8165 10.4352 90.000 99.549 90.000 ZERR 4.00 0.0019 0.0060 0.0035 0.000 0.012 0.000 LATT 1 SYMM -x+1/2, y+1/2, -z+1/2 SFAC C H N O UNIT 56 60 4 16 LIST 4 TEMP -173 ACTA SIZE 0.091 0.209 0.343 L.S. 4 FMAP -2 PLAN 20 REM Instructions for potential hydrogen bonds EQIV $2 x-1/2, -y+1/2, z+1/2 HTAB O4A O12_$2 HTAB C8 O12 CONF WGHT 0.038100 0.670000 FVAR 0.58213 O4A 4 0.074563 0.361336 0.676985 11.00000 0.01457 0.02520 = 0.01326 0.00344 0.00404 0.00287 O10 4 0.246533 0.420443 0.907021 11.00000 0.03337 0.02492 = 0.01503 -0.00330 0.01007 0.00138 O12 4 0.365524 0.206703 0.353442 11.00000 0.02096 0.01772 = 0.01353 -0.00415 0.00535 -0.00293 O13 4 0.361303 0.340897 0.332698 11.00000 0.02168 0.01780 = 0.00827 -0.00031 0.00333 -0.00037 N9 3 0.348364 0.287691 0.526101 11.00000 0.01747 0.01362 = 0.01013 -0.00082 0.00279 -0.00110 C1 1 0.561216 0.397462 0.610276 11.00000 0.01675 0.01793 = 0.01347 -0.00135 0.00329 -0.00110 AFIX 23 H1A 2 0.645575 0.353073 0.644405 11.00000 -1.20000 H1B 2 0.596899 0.415045 0.527118 11.00000 -1.20000 AFIX 0 C2 1 0.588145 0.466114 0.706833 11.00000 0.02278 0.01873 = 0.01807 -0.00324 0.00245 -0.00378 AFIX 23 H2A 2 0.502296 0.510327 0.674150 11.00000 -1.20000 H2B 2 0.719468 0.485896 0.716693 11.00000 -1.20000 AFIX 0 C3 1 0.546088 0.437850 0.838621 11.00000 0.02316 0.01987 = 0.01412 -0.00492 -0.00088 0.00097 AFIX 23 H3A 2 0.636034 0.395287 0.872622 11.00000 -1.20000 H3B 2 0.563823 0.482629 0.901046 11.00000 -1.20000 AFIX 0 C4 1 0.348354 0.406959 0.827433 11.00000 0.02482 0.01336 = 0.01039 0.00167 0.00237 0.00481 H4A 2 0.024470 0.344831 0.741819 11.00000 0.04307 C5 1 0.342081 0.224188 0.854775 11.00000 0.01396 0.02204 = 0.01171 0.00014 0.00187 -0.00106 AFIX 43 H5 2 0.325526 0.249755 0.933281 11.00000 -1.20000 AFIX 0 C4A 1 0.273767 0.353236 0.711023 11.00000 0.01469 0.01719 = 0.01019 0.00052 0.00225 0.00088 C4B 1 0.329123 0.266914 0.740269 11.00000 0.01097 0.01711 = 0.01272 -0.00093 0.00049 -0.00117 C6 1 0.379874 0.142950 0.852737 11.00000 0.01324 0.02203 = 0.01589 0.00498 0.00007 -0.00175 AFIX 43 H6 2 0.390462 0.112711 0.930508 11.00000 -1.20000 AFIX 0 C7 1 0.402124 0.106084 0.736706 11.00000 0.01343 0.01591 = 0.02159 0.00111 0.00001 -0.00120 AFIX 43 H7 2 0.424870 0.050440 0.736434 11.00000 -1.20000 AFIX 0 C8 1 0.391952 0.148581 0.620735 11.00000 0.01344 0.01742 = 0.01596 -0.00210 0.00160 -0.00189 AFIX 43 H8 2 0.407965 0.123031 0.542102 11.00000 -1.20000 AFIX 0 C8A 1 0.357467 0.229725 0.625096 11.00000 0.01037 0.01770 = 0.01125 0.00025 0.00070 -0.00200 C9A 1 0.357054 0.368107 0.585705 11.00000 0.01736 0.01392 = 0.00928 -0.00134 0.00268 0.00050 AFIX 13 H9A 2 0.275467 0.405985 0.527536 11.00000 -1.20000 AFIX 0 C11 1 0.359608 0.272990 0.399556 11.00000 0.01022 0.01764 = 0.01141 -0.00126 0.00168 -0.00196 C14 1 0.369961 0.332188 0.195684 11.00000 0.01921 0.02448 = 0.00810 -0.00061 0.00371 0.00001 AFIX 137 H14A 2 0.284791 0.289439 0.158998 11.00000 -1.50000 H14B 2 0.499300 0.319100 0.184859 11.00000 -1.50000 H14C 2 0.331647 0.382135 0.150518 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM cu_ModSa3_0m_a.res in P2(1)/n REM R1 = 0.0333 for 2141 Fo > 4sig(Fo) and 0.0356 for all 2281 data REM 177 parameters refined using 0 restraints END WGHT 0.0381 0.6700 REM Highest difference peak 0.264, deepest hole -0.254, 1-sigma level 0.046 Q1 1 0.3154 0.3823 0.7634 11.00000 0.05 0.26 Q2 1 0.3479 0.3181 0.4402 11.00000 0.05 -0.25 Q3 1 0.3142 0.3649 0.6499 11.00000 0.05 0.25 Q4 1 0.3490 0.2810 0.6227 11.00000 0.05 -0.23 Q5 1 0.3611 0.2398 0.4534 11.00000 0.05 -0.23 Q6 1 0.3537 0.1967 0.6890 11.00000 0.05 -0.22 Q7 1 0.2523 0.3970 0.6876 11.00000 0.05 -0.21 Q8 1 0.3512 0.2958 0.2414 11.00000 0.05 -0.20 Q9 1 0.3670 0.2162 0.5581 11.00000 0.05 -0.20 Q10 1 0.4613 0.3812 0.5988 11.00000 0.05 0.19 Q11 1 0.3457 0.1607 0.7269 11.00000 0.05 -0.19 Q12 1 0.3424 0.2178 0.7360 11.00000 0.05 -0.19 Q13 1 0.5763 0.4318 0.6573 11.00000 0.05 0.19 Q14 1 0.5801 0.4473 0.7782 11.00000 0.05 0.18 Q15 1 0.3384 0.3805 0.1074 11.00000 0.05 -0.18 Q16 1 0.3688 0.2663 0.3413 11.00000 0.05 -0.18 Q17 1 0.3831 0.3563 0.7257 11.00000 0.05 -0.18 Q18 1 0.3799 0.1637 0.9167 11.00000 0.05 -0.18 Q19 1 0.2526 0.3958 0.8188 11.00000 0.05 -0.17 Q20 1 0.3035 0.2436 0.6796 11.00000 0.05 0.17 ; _shelx_res_checksum 6086 _shelx_hkl_file ; -1 0 0 0.77369 0.17149 14 -1 0 0 0.59774 0.52426 1 1 0 0 -0.0364 0.48042 1 1 0 0 1.32665 0.20969 14 -2 0 0 238.692 9.05541 18 2 0 0 248.297 9.02384 5 2 0 0 244.602 9.96358 1 2 0 0 251.408 9.89554 1 -3 0 0 -0.2169 0.33999 18 3 0 0 -0.2140 0.32185 5 3 0 0 -0.1448 0.24838 9 4 0 0 3505.72 131.009 5 -4 0 0 3697.05 132.571 18 -4 0 0 3415.03 131.165 10 4 0 0 3867.31 131.983 9 -5 0 0 -1.0024 0.82057 18 5 0 0 -0.0359 0.61319 6 -5 0 0 2.40929 1.33542 3 -5 0 0 0.03700 1.00251 10 -5 0 0 -1.4335 1.14209 2 6 0 0 3.03843 1.20561 6 -6 0 0 2.06757 1.37809 3 -6 0 0 4.24937 1.40177 2 -6 0 0 3.12020 1.18412 10 -7 0 0 -0.5132 1.97466 3 -7 0 0 -0.9564 1.04460 10 -8 0 0 127.852 5.31342 10 -1 -1 0 665.564 22.7081 18 -1 -1 0 614.468 22.5619 22 1 -1 0 601.200 23.1555 1 1 -1 0 574.538 22.3936 14 -1 -1 0 630.492 22.6142 14 1 -1 0 626.574 22.6734 5 -1 1 0 584.375 22.4991 5 -1 1 0 647.689 22.6995 18 -1 1 0 582.852 23.1086 1 1 1 0 659.139 23.7850 1 1 1 0 644.270 22.7038 9 1 1 0 573.747 22.3885 14 1 1 0 633.414 23.7414 1 -2 -1 0 8825.29 341.870 18 2 1 0 9333.71 343.163 1 -2 1 0 9666.55 342.185 18 2 1 0 9398.48 341.119 21 2 1 0 9999.99 343.412 1 3 -1 0 95.9748 3.73498 5 -3 -1 0 99.2635 3.80999 18 -3 1 0 95.6689 3.83042 18 3 1 0 92.8358 3.70091 9 3 1 0 97.7099 3.77650 5 4 -1 0 1462.04 52.2517 5 -4 -1 0 1414.58 52.3045 18 -4 -1 0 1470.92 52.5976 3 4 -1 0 1383.97 52.0518 9 4 1 0 1575.46 52.3340 5 -4 1 0 1392.59 52.3334 18 -4 1 0 1360.84 52.4233 10 -5 -1 0 68.9174 3.38157 10 5 -1 0 69.0527 2.94342 6 -5 -1 0 64.6551 3.26969 18 -5 -1 0 69.1550 3.69015 2 -5 -1 0 71.0686 3.66299 3 -5 1 0 71.3149 3.45224 10 -5 1 0 69.9410 3.65096 2 -5 1 0 64.9517 3.89474 3 5 1 0 64.2016 2.73286 16 -5 1 0 66.6049 3.30873 18 -6 -1 0 883.809 32.7753 10 -6 -1 0 865.253 32.6754 2 -6 -1 0 914.119 32.9124 3 6 1 0 877.161 32.1819 16 -6 1 0 881.817 32.7851 3 -6 1 0 868.234 32.7094 2 -6 1 0 892.158 32.7459 10 -7 -1 0 8.03005 1.44401 10 -7 1 0 5.82120 1.61184 3 -7 1 0 9.82072 1.71610 10 -8 -1 0 161.510 6.08911 10 -8 1 0 122.801 6.47935 2 -8 1 0 161.421 6.08996 10 0 -2 0 3452.48 115.513 8 0 -2 0 2809.45 115.106 18 0 -2 0 3095.74 115.451 9 0 -2 0 2960.26 116.702 1 0 -2 0 3321.39 115.210 24 0 -2 0 3257.05 115.405 22 0 2 0 3288.82 115.204 6 0 2 0 3221.78 116.850 1 0 2 0 3257.15 115.475 9 -1 -2 0 1212.82 42.3790 22 -1 -2 0 1232.20 42.3320 14 1 -2 0 1161.10 42.1569 24 1 -2 0 1146.50 42.4044 5 1 -2 0 1130.51 42.2488 9 1 -2 0 1142.32 42.0878 6 -1 -2 0 1148.24 42.3037 8 1 -2 0 1148.06 43.6419 1 1 2 0 1149.52 44.3127 1 -1 2 0 1137.92 42.4456 5 -1 2 0 1138.52 43.6046 1 -1 2 0 1101.89 42.2799 18 1 2 0 1241.12 42.5668 9 1 2 0 1173.08 44.3324 1 1 2 0 1150.94 42.1336 14 -2 -2 0 574.164 22.3732 18 2 -2 0 670.796 24.0323 1 2 -2 0 603.079 22.3688 5 2 -2 0 637.535 22.4053 6 -2 2 0 633.279 23.8382 1 2 2 0 587.809 22.3900 9 2 2 0 623.965 25.3225 1 2 2 0 612.746 26.3014 1 -2 2 0 613.738 22.4375 18 -2 2 0 604.399 22.3799 5 -3 -2 0 916.951 32.5757 18 3 -2 0 863.362 32.4261 6 3 -2 0 887.124 32.5207 5 3 2 0 935.747 35.5701 1 -3 2 0 908.215 32.6365 18 3 2 0 881.329 35.7058 1 3 2 0 871.115 32.5265 9 4 -2 0 1336.05 47.9125 5 -4 -2 0 1337.14 48.1447 10 -4 -2 0 1306.71 47.9574 18 4 -2 0 1297.50 47.7522 6 4 2 0 1366.35 48.0152 5 -4 2 0 1299.76 48.0266 18 4 2 0 1275.59 47.8488 9 -5 -2 0 30.1175 2.02322 18 -5 -2 0 31.2407 2.42532 3 -5 -2 0 31.8597 2.69114 2 5 -2 0 28.6565 1.68597 6 -5 2 0 28.7580 2.53871 2 -5 2 0 26.9412 1.94567 18 -5 2 0 29.6913 3.13330 3 5 2 0 30.4236 1.50977 16 -5 2 0 23.8813 2.70325 11 -6 -2 0 465.801 17.9471 2 -6 -2 0 480.324 18.1986 3 -6 -2 0 485.307 18.0281 10 -6 2 0 458.263 18.0493 3 -6 2 0 470.348 17.9680 10 -6 2 0 475.677 18.0318 2 6 2 0 478.926 17.4449 16 -7 -2 0 9.18833 1.59546 10 -7 -2 0 10.5484 1.66800 2 7 2 0 7.34406 2.70670 24 -7 2 0 7.03583 2.18334 2 7 2 0 8.98619 1.13153 16 -8 -2 0 69.4189 3.46285 3 -8 -2 0 70.0680 3.35918 10 -8 2 0 67.8260 3.41225 2 -8 2 0 73.0717 3.41465 10 0 -3 0 -1.0691 1.49426 1 0 -3 0 0.07128 0.14444 22 0 -3 0 0.19609 0.20495 8 0 3 0 0.55701 0.20090 9 0 3 0 0.33958 1.80516 1 1 -3 0 350.558 13.2803 24 1 -3 0 408.697 17.6321 1 -1 -3 0 397.316 13.4579 18 -1 -3 0 369.175 13.3031 14 1 -3 0 386.401 13.3637 6 -1 -3 0 355.238 13.3603 22 -1 -3 0 371.322 13.3714 8 -1 -3 0 353.237 13.2637 21 -1 3 0 364.784 13.3518 5 -1 3 0 352.051 13.3288 9 -1 3 0 395.406 16.0257 1 1 3 0 357.057 13.3822 9 -1 3 0 349.492 13.3559 18 -1 3 0 341.966 13.2703 6 1 3 0 338.597 13.3173 14 1 3 0 385.211 16.7169 1 2 -3 0 1670.63 59.9863 5 -2 -3 0 1613.46 59.8564 14 -2 -3 0 1669.76 59.9540 18 2 -3 0 1674.85 61.9519 1 2 -3 0 1624.91 59.6451 24 2 -3 0 1609.50 59.5825 6 -2 -3 0 1671.97 59.9656 22 -2 3 0 1616.88 60.0034 5 2 3 0 1655.82 63.2473 1 2 3 0 1603.95 63.3265 1 2 3 0 1553.79 59.5415 16 2 3 0 1638.36 60.2122 9 -2 3 0 1683.84 61.7563 1 -2 3 0 1663.36 60.1704 18 3 -3 0 316.145 12.6076 5 3 -3 0 345.066 12.3961 6 -3 -3 0 359.296 12.5460 18 3 3 0 319.806 17.5282 1 3 3 0 357.231 12.5628 9 -3 3 0 335.937 12.6155 18 3 3 0 338.114 12.3994 16 4 -3 0 -0.4380 0.66028 5 -4 -3 0 0.44158 0.91684 10 4 -3 0 0.77156 0.39980 6 -4 -3 0 1.13374 1.13595 3 4 -3 0 0.32159 0.49172 24 -4 -3 0 -0.1081 0.57979 18 -4 3 0 1.24110 0.65350 18 4 3 0 0.56816 0.56222 9 4 3 0 1.65529 0.41878 16 4 3 0 -1.0273 0.90682 5 -4 3 0 1.27771 1.12045 2 -5 -3 0 264.681 9.76443 18 -5 -3 0 248.269 9.99156 2 5 -3 0 235.575 9.38477 6 -5 -3 0 251.957 9.92681 10 5 -3 0 257.423 9.47554 24 -5 -3 0 252.048 11.0211 3 5 3 0 247.884 9.34150 16 -5 3 0 247.709 9.88018 11 -5 3 0 248.333 9.82961 18 -6 -3 0 4.65404 1.21699 10 -6 -3 0 3.85780 1.41997 3 -6 -3 0 0.13914 1.54430 2 -6 3 0 2.81109 1.32867 10 6 3 0 6.19884 1.00959 16 -6 3 0 0.66292 1.63083 11 -6 3 0 3.34107 1.30002 2 6 3 0 2.96496 1.21413 6 7 3 0 77.4735 3.53230 16 -7 3 0 86.0427 5.23425 10 -8 -3 0 102.373 4.39698 3 -8 -3 0 105.882 4.37984 10 -8 3 0 102.954 4.40379 10 -8 3 0 87.6950 4.15082 2 0 -4 0 2166.97 78.3585 18 0 -4 0 2173.46 78.8263 22 0 -4 0 2189.72 78.8494 8 0 -4 0 2098.27 78.3942 16 0 -4 0 2093.02 81.8187 1 0 4 0 2216.60 78.9080 9 0 4 0 2182.15 82.0539 1 -1 -4 0 87.0603 3.23979 8 -1 -4 0 86.1350 3.09374 18 1 -4 0 85.7902 3.25226 8 -1 -4 0 83.9528 3.23162 22 1 -4 0 83.5642 3.12519 24 -1 -4 0 84.1639 3.13080 14 1 -4 0 85.4906 6.89155 1 1 -4 0 82.8514 3.10597 6 1 4 0 82.9388 3.26512 9 1 4 0 80.7926 3.19857 16 -1 4 0 86.1929 3.13344 6 -1 4 0 86.9850 3.21866 18 -1 4 0 83.8534 3.20478 9 -1 4 0 73.9131 6.59534 1 1 4 0 87.0412 7.36875 1 -1 4 0 85.8234 3.22337 5 2 -4 0 88.7827 3.39557 6 -2 -4 0 94.6769 3.55966 22 -2 -4 0 94.0527 3.46576 18 2 -4 0 91.1110 3.52435 16 2 -4 0 91.4922 3.42267 24 -2 -4 0 90.7526 3.54995 8 2 -4 0 88.0278 7.39815 1 -2 4 0 84.4040 6.89346 1 -2 4 0 93.5955 3.54509 5 2 4 0 88.8675 9.43934 1 2 4 0 92.5566 3.59206 9 2 4 0 91.0289 3.47993 16 -2 4 0 93.7096 3.59164 18 2 4 0 96.0977 8.34604 1 -3 -4 0 567.568 21.0473 18 3 -4 0 566.735 20.8953 16 3 -4 0 584.999 20.9255 6 3 4 0 577.639 21.1365 9 -3 4 0 597.745 21.1144 5 3 4 0 570.134 27.5094 1 -3 4 0 594.304 21.1933 18 -3 4 0 547.181 23.6363 1 4 -4 0 10.9469 0.92199 24 -4 -4 0 10.5592 1.52014 10 -4 -4 0 11.5534 1.91806 3 4 -4 0 9.91218 0.79389 6 4 4 0 9.11322 1.09471 9 4 4 0 10.2644 0.80304 16 -4 4 0 10.1624 1.13670 18 -4 4 0 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185.089 7.05695 22 1 -6 0 197.797 7.08497 8 1 -6 0 190.708 6.97836 16 -1 -6 0 192.997 7.06494 8 -1 -6 0 169.378 6.98140 16 -1 -6 0 193.464 6.86387 14 -1 6 0 186.294 7.16350 5 1 6 0 175.788 14.4058 1 1 6 0 190.318 6.99497 16 -1 6 0 164.553 12.8439 1 1 6 0 190.034 7.09976 9 -1 6 0 190.694 7.03922 9 2 -6 0 129.321 12.1450 1 -2 -6 0 133.169 5.06805 22 2 -6 0 136.444 5.11898 8 2 -6 0 128.193 4.85694 24 -2 -6 0 134.868 5.08179 8 2 6 0 127.575 4.98599 16 -2 6 0 133.452 5.09047 5 2 6 0 121.843 13.1342 1 2 6 0 128.947 5.07416 20 2 6 0 112.555 13.7288 1 -2 6 0 137.083 5.08661 18 2 6 0 135.812 5.14971 9 -3 -6 0 42.7875 1.98064 22 -3 -6 0 41.5517 1.83943 18 -3 -6 0 40.8906 2.51213 10 3 -6 0 41.6595 1.80664 16 3 -6 0 43.3719 2.04027 8 3 -6 0 41.7397 1.68632 6 -3 -6 0 49.2200 2.99264 3 -3 6 0 40.7281 2.66533 2 3 6 0 42.1042 2.22863 16 -3 6 0 43.3550 2.09957 5 3 6 0 44.5577 2.07436 20 -3 6 0 40.1433 2.51074 11 3 6 0 43.7735 2.07214 9 4 -6 0 55.1003 2.33099 16 -4 -6 0 57.7776 2.91797 10 -4 -6 0 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27.5133 2.30263 3 -4 -7 0 29.4653 2.76076 12 -4 -7 0 26.4976 1.97141 10 -4 7 0 19.9917 2.32843 7 4 7 0 28.4616 1.48022 16 -4 7 0 26.0821 2.03730 11 -4 7 0 26.4986 2.33475 10 -4 7 0 23.5485 2.03261 17 -4 7 0 25.2852 2.17851 2 4 7 0 29.9202 2.52782 13 4 7 0 26.5883 1.90386 9 -5 -7 0 51.5400 2.90675 10 -5 -7 0 55.8982 3.34473 3 -5 -7 0 48.3313 3.11322 4 5 -7 0 52.1214 2.37240 16 5 -7 0 51.2934 2.91339 8 5 7 0 50.7912 2.59091 20 -5 7 0 47.8997 3.23581 7 -5 7 0 50.1138 2.94839 11 5 7 0 49.2382 3.18226 9 -5 7 0 47.9099 3.12087 2 5 7 0 53.2743 2.40119 16 -6 -7 0 3.26306 1.59249 3 6 -7 0 3.39322 0.92044 16 6 -7 0 2.28394 2.16410 8 -6 -7 0 4.48709 1.32519 10 6 -7 0 4.33820 2.03764 22 6 7 0 4.12447 0.83198 16 6 7 0 4.19583 0.95963 20 -6 7 0 1.96746 1.15958 11 -6 7 0 3.93285 1.52724 2 -6 7 0 4.55996 1.44790 10 -7 -7 0 39.5548 2.69216 3 -7 -7 0 39.5092 2.43394 10 -7 7 0 43.6160 2.75423 11 -7 7 0 36.5761 2.61428 10 7 7 0 38.7832 2.21611 16 -7 7 0 43.7036 2.66155 2 7 7 0 42.6038 2.26729 20 -8 -7 0 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122.884 5.71950 20 -3 -8 0 145.652 6.07997 12 -3 -8 0 141.657 6.16392 3 -3 -8 0 150.899 5.70127 22 -3 -8 0 144.378 5.88711 4 3 -8 0 143.502 5.49875 16 3 8 0 139.030 5.59768 20 3 8 0 147.895 5.55869 16 -3 8 0 144.094 5.74777 4 -3 8 0 135.339 5.98397 7 -3 8 0 144.252 5.98220 17 -3 8 0 138.819 6.12589 2 3 8 0 151.111 5.88632 9 -3 8 0 149.347 5.93284 5 3 8 0 138.781 6.01540 13 -3 8 0 150.390 5.98401 11 -4 -8 0 158.283 6.66327 10 -4 -8 0 163.214 6.83203 12 -4 -8 0 164.763 6.83814 3 4 -8 0 159.621 6.17353 16 4 -8 0 164.755 6.54629 8 -4 8 0 156.658 6.81395 10 -4 8 0 162.582 6.62017 17 -4 8 0 153.222 6.30073 4 -4 8 0 166.683 6.66321 11 4 8 0 158.212 6.23357 16 4 8 0 156.644 6.29461 20 -4 8 0 162.911 6.82107 2 4 8 0 155.450 6.69913 13 4 8 0 159.793 6.55823 9 -4 8 0 162.193 6.71060 7 5 -8 0 0.55627 0.95011 20 -5 -8 0 0.03783 1.03163 10 5 -8 0 -1.6540 0.90431 22 -5 -8 0 2.06448 1.65862 12 -5 -8 0 -0.5320 0.99582 4 -5 -8 0 0.30586 1.25623 3 5 -8 0 0.01920 0.65356 16 -5 8 0 0.12017 1.25502 10 5 8 0 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3.01323 15 -3 7 11 53.2984 2.88076 4 3 7 -11 50.0722 2.77588 4 -3 7 11 52.9314 2.98419 13 -2 -7 11 29.0899 1.92436 13 -2 -7 11 36.6254 4.04052 4 2 -7 -11 31.8670 2.16410 4 2 -7 -11 28.4032 2.09504 19 2 7 -11 32.7272 2.02140 4 2 7 -11 27.6917 2.21378 15 -2 7 11 28.9984 2.22123 4 -2 7 11 30.8036 1.92013 13 1 -7 -11 24.3535 1.83903 4 -1 -7 11 29.8965 1.95693 13 1 -7 -11 24.9725 2.07454 19 -1 7 11 27.0893 1.81166 13 1 7 -11 25.3520 2.03873 19 1 7 -11 30.8594 2.19407 15 1 7 -11 25.6021 1.70877 4 0 -7 11 44.3461 2.32550 20 0 -7 11 48.0250 2.51289 13 0 -7 -11 48.6988 2.69725 19 0 -7 -11 43.9805 2.37790 4 0 7 -11 44.3862 2.24006 4 0 7 11 49.9341 2.47310 13 0 7 -11 43.1991 2.63900 15 -1 -7 -11 1.79136 0.89283 4 -1 -7 -11 1.17967 0.83326 11 1 -7 11 2.25045 0.84369 13 1 -7 11 1.03251 0.77936 20 1 7 11 1.19194 0.85979 20 1 7 11 0.80449 0.79867 13 -1 7 -11 -1.6509 1.35559 15 -3 -8 11 0.09618 1.00306 13 3 -8 -11 3.78263 1.15355 13 3 -8 -11 3.58694 0.95015 19 -3 -8 11 3.25999 0.94481 4 3 -8 -11 0.51603 1.14018 4 3 8 -11 1.34395 0.87922 15 3 8 -11 1.86689 0.78931 4 -3 8 11 2.99243 1.04307 4 2 -8 -11 33.7702 2.34213 4 -2 -8 11 39.3565 2.17407 13 2 -8 -11 38.5656 2.36949 19 -2 8 11 35.5598 2.74318 4 2 8 -11 36.3288 2.41623 15 -2 8 11 39.6479 2.13950 13 2 8 -11 35.4772 2.10298 4 1 -8 -11 31.2415 2.24415 19 1 -8 -11 31.5119 2.21919 4 -1 -8 11 37.5987 2.14660 13 -1 8 11 34.2248 2.11202 13 1 8 -11 36.0719 2.05322 4 1 8 -11 32.4162 2.26441 15 0 -8 -11 17.7479 2.34812 19 0 -8 11 13.1710 1.49864 20 0 8 -11 17.0541 1.30949 4 0 8 -11 21.9875 2.16036 15 0 8 11 17.2587 1.44037 13 1 -8 11 6.61199 1.12533 20 -1 -8 -11 8.31675 1.27308 11 1 -8 11 5.56793 0.87615 13 1 8 11 7.30200 1.26566 13 -1 8 -11 8.79007 1.84285 15 2 -9 -11 38.8780 2.22066 4 -2 -9 11 39.5014 2.07430 13 2 -9 -11 37.1020 2.14287 19 2 9 -11 41.4512 2.07122 4 -2 9 11 31.3059 2.16722 13 2 9 -11 39.8820 2.30158 15 -2 9 11 37.7411 2.28392 4 1 -9 -11 178.063 6.61406 19 1 -9 -11 157.735 6.36171 4 -1 -9 11 146.588 6.19785 13 -1 9 11 154.376 6.22595 13 1 9 -11 154.745 6.41623 15 1 9 -11 165.298 6.22970 4 0 -9 -11 23.4864 1.50033 4 0 -9 -11 21.2152 1.72704 19 0 -9 11 22.7935 1.58057 13 0 9 -11 25.7844 1.56090 4 0 9 11 23.2785 1.59854 13 0 9 -11 25.8308 2.82608 15 -3 0 12 0.19410 1.59630 4 3 0 -12 -0.4842 0.81041 4 3 0 -12 1.05963 1.26157 15 3 0 -12 -0.4660 0.83295 19 -2 0 12 16.1969 2.23926 4 -2 0 12 13.8212 1.52634 13 2 0 -12 11.7093 1.44494 4 2 0 -12 15.4274 1.77245 19 1 0 -12 -0.1983 0.83417 19 1 0 -12 0.37004 0.82508 4 1 0 -12 -1.9788 1.65174 11 0 0 -12 39.9803 2.82864 11 0 0 -12 43.5656 2.07544 4 0 0 12 42.3445 2.21954 13 0 0 12 35.6477 2.10129 20 0 0 -12 39.3539 2.24741 19 -1 0 -12 -0.9002 0.85222 11 1 0 12 1.39110 0.73275 20 -1 0 -12 0.51868 1.00501 19 1 0 12 -0.1505 1.09333 13 -3 -1 12 20.4051 2.20563 13 3 -1 -12 13.7349 2.49202 15 3 -1 -12 20.3561 1.58877 4 3 -1 -12 17.2941 1.63408 19 3 1 -12 22.1315 2.01038 15 -3 1 12 18.2541 2.07091 13 3 1 -12 22.9946 1.56179 4 -3 1 12 16.6913 2.15217 4 3 1 -12 18.2681 1.90938 19 2 -1 -12 13.9384 1.75356 19 -2 -1 12 13.9581 1.57548 13 2 -1 -12 17.2759 1.71474 4 2 -1 -12 22.9192 3.44420 15 -2 -1 12 21.3277 2.30104 4 -2 1 12 17.5280 1.58721 13 2 1 -12 15.3514 1.65209 19 2 1 -12 17.6388 2.34479 15 -2 1 12 13.5245 2.02867 4 2 1 -12 16.1425 1.60926 4 1 -1 -12 30.2278 2.05539 19 1 -1 -12 28.5034 1.81144 4 -1 -1 12 28.0185 1.87715 13 1 1 -12 28.1542 2.07947 19 -1 1 12 29.0021 1.87919 13 0 -1 -12 91.8388 3.89863 4 0 -1 -12 94.9457 4.12941 19 0 -1 12 101.244 4.12056 13 0 -1 12 87.4246 3.90892 20 0 -1 -12 90.4672 4.12702 11 0 1 -12 107.467 4.79077 11 0 1 -12 93.9945 4.10572 19 0 1 12 102.851 4.13701 13 0 1 -12 92.6706 3.92779 4 1 -1 12 5.97602 0.91596 20 1 -1 12 4.27123 1.11946 13 -1 -1 -12 7.14637 1.38866 19 1 1 12 7.63992 1.37692 13 -1 1 -12 8.93817 1.64280 19 1 1 12 6.73110 1.11946 20 3 -2 -12 118.958 5.08590 4 3 -2 -12 129.323 5.49934 15 -3 -2 12 128.898 5.53385 4 3 -2 -12 120.587 5.10031 19 -3 -2 12 119.176 5.23541 13 3 2 -12 123.662 5.30619 15 -3 2 12 134.416 5.26272 13 3 2 -12 124.558 5.09443 4 2 -2 -12 34.9287 2.21227 19 2 -2 -12 39.9255 2.27048 4 -2 -2 12 34.9494 2.12504 13 -2 2 12 34.5772 2.81660 4 2 2 -12 35.4128 2.52556 15 2 2 -12 39.9838 2.14096 4 -2 2 12 35.6455 2.08301 13 2 2 -12 33.8664 2.27634 19 -1 -2 12 58.0386 2.82505 13 1 -2 -12 47.5321 3.32190 11 1 -2 -12 58.2880 2.75413 4 1 -2 -12 56.8740 2.86547 19 -1 2 12 62.9346 2.81019 13 1 2 -12 54.2103 2.79300 19 1 2 -12 53.3998 2.60887 4 1 2 -12 50.7971 3.13839 15 0 -2 -12 8.99427 1.42652 11 0 -2 -12 9.36296 1.23472 4 0 -2 -12 10.2978 1.46295 19 0 -2 12 11.7736 1.48284 13 0 2 -12 10.5934 1.44844 19 0 2 12 11.8326 1.37556 13 0 2 12 8.32773 1.81790 20 0 2 -12 8.48513 1.54659 11 1 -2 12 58.8267 2.59984 20 -1 -2 -12 53.6115 2.68515 19 1 -2 12 63.0337 2.79307 13 -1 2 -12 61.3355 2.77433 11 -1 2 -12 67.8019 3.19144 19 1 2 12 58.5844 2.72263 20 3 -3 -12 38.5603 2.81028 15 -3 -3 12 45.2285 2.57561 4 3 -3 -12 46.0017 2.39056 19 3 -3 -12 49.2059 2.41381 4 -3 -3 12 53.8020 2.91098 13 3 3 -12 47.0176 2.44581 19 3 3 -12 44.3417 2.52693 15 -3 3 12 55.9701 2.98454 4 3 3 -12 48.2507 2.39698 4 -3 3 12 42.1709 2.37008 13 2 -3 -12 132.564 5.65918 19 -2 -3 12 133.516 5.49356 13 2 -3 -12 154.203 6.41688 11 2 -3 -12 139.002 5.63398 4 2 3 -12 139.534 5.64946 19 2 3 -12 144.606 5.83465 15 2 3 -12 135.143 5.54233 4 -2 3 12 138.590 5.50762 13 -2 3 12 130.600 5.81741 4 1 -3 -12 23.4015 1.72383 4 1 -3 -12 21.2034 1.78409 19 -1 -3 12 23.3348 1.83805 13 1 -3 -12 27.6431 2.47992 11 -1 3 12 24.9874 1.75145 13 1 3 -12 23.5666 1.93347 19 1 3 -12 24.2512 1.52958 4 1 3 -12 23.8468 2.67516 15 0 -3 -12 2.52891 0.97532 19 0 -3 12 4.03416 0.94195 13 0 -3 12 3.69240 1.03589 20 0 -3 -12 3.51815 0.79315 4 0 3 -12 4.28313 0.71348 4 0 3 12 3.60948 0.81743 13 0 3 -12 3.36338 0.81807 19 -3 -4 12 59.7267 2.79929 13 3 -4 -12 54.3726 2.75715 19 -3 4 12 61.2071 2.88658 4 3 4 -12 61.3904 2.97585 4 3 4 -12 58.9126 3.29797 15 -3 4 12 56.3225 2.91526 13 3 4 -12 62.9466 2.95063 19 2 -4 -12 13.3775 1.50210 4 -2 -4 12 14.0135 1.41524 13 2 -4 -12 14.7570 1.64971 19 2 4 -12 14.5957 2.07715 15 -2 4 12 15.2201 1.42694 13 -2 4 12 14.0088 1.64144 4 2 4 -12 15.0023 1.38264 4 2 4 -12 12.5983 1.52118 19 1 -4 -12 50.8579 2.51546 4 1 -4 -12 51.1474 3.32581 11 1 -4 -12 53.5049 2.70087 19 -1 -4 12 51.1193 2.52571 13 1 4 -12 49.9705 2.38993 4 -1 4 12 48.4283 2.40822 13 1 4 -12 52.2210 2.63222 19 0 -4 12 54.6208 2.62033 13 0 -4 -12 54.1382 2.50992 4 0 -4 -12 53.0744 2.91102 19 0 -4 -12 58.1293 2.97435 11 0 4 -12 54.6500 2.68656 19 0 4 12 58.4114 2.60370 13 2 -5 -12 1.06354 0.77045 4 -2 -5 12 -0.2079 0.78191 13 2 -5 -12 0.69387 0.68371 19 -2 5 12 0.42712 0.92476 13 -2 5 12 -0.9817 0.97000 4 2 5 -12 0.09068 0.63491 4 2 5 -12 0.42784 1.18095 15 2 5 -12 -0.1868 0.94529 19 1 -5 -12 0.42567 0.96033 19 1 -5 -12 0.72582 0.66688 4 1 -5 -12 -0.0862 2.12390 11 -1 -5 12 0.51024 0.77547 13 1 5 -12 0.46484 1.03064 15 -1 5 12 1.83735 0.86437 13 1 5 -12 0.71264 0.84138 19 1 5 -12 0.97086 0.69080 4 0 -5 -12 54.7477 2.73097 19 0 5 -12 48.7340 2.25183 4 0 5 12 48.6511 2.39707 13 -1 -6 12 4.99831 0.87507 13 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.6742 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54179 7.173 16.838 10.432 89.998 99.480 89.994 ) ; _shelx_hkl_checksum 61363 #===END