data_s _audit_creation_date 2019-01-14 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C22 H20 I N O5' _chemical_formula_sum 'C22 H20 I N O5' _chemical_formula_weight 505.29 _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' 'I' 'I' -0.3257 6.8362 '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' _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 10.7031(14) _cell_length_b 10.0960(13) _cell_length_c 19.634(3) _cell_angle_alpha 90 _cell_angle_beta 101.314(3) _cell_angle_gamma 90 _cell_volume 2080.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9832 _cell_measurement_temperature 153 _cell_measurement_theta_max 68.324 _cell_measurement_theta_min 4.380 _shelx_estimated_absorpt_T_max 0.119 _shelx_estimated_absorpt_T_min 0.063 _exptl_absorpt_coefficient_mu 12.379 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.3867 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1421 before and 0.0826 after correction. The Ratio of minimum to maximum transmission is 0.5135. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1008 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0581 _diffrn_reflns_av_unetI/netI 0.0306 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 34900 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.342 _diffrn_reflns_theta_min 4.212 _diffrn_ambient_temperature 152.99 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3795 _reflns_number_total 3796 _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 'SAINT V8.38A (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'XT (Sheldrick, 2015)' _refine_diff_density_max 0.816 _refine_diff_density_min -1.788 _refine_diff_density_rms 0.146 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 266 _refine_ls_number_reflns 3796 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0366 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0601P)^2^+3.3045P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.0952 _refine_special_details ? _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 2.a Aromatic/amide H refined with riding coordinates: C00B(H00B), C00E(H00E), C00I(H00I), C00L(H00L), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q) 2.b Idealised Me refined as rotating group: C00H(H00A,H00C,H00D), C00R(H00F,H00G,H00H), C00S(H00J,H00K,H00M), C00T(H00R, H00S,H00T) ; _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 I001 I 0.91196(2) 0.55391(2) 0.59483(2) 0.01875(11) Uani 1 1 d . . . . . O002 O 0.67276(18) 0.2991(2) 0.34703(11) 0.0148(4) Uani 1 1 d . . . . . O003 O 0.19896(18) 0.7995(2) 0.36906(10) 0.0147(4) Uani 1 1 d . . . . . O004 O 0.7817(2) 0.4745(2) 0.31785(13) 0.0199(5) Uani 1 1 d . . . . . O005 O 0.3129(2) 0.6404(2) 0.29378(11) 0.0242(5) Uani 1 1 d . . . . . N006 N 0.3833(2) 0.6956(2) 0.41107(11) 0.0078(4) Uani 1 1 d . . . . . O007 O 0.3012(2) 0.8445(3) 0.47805(14) 0.0376(7) Uani 1 1 d . . . . . C008 C 0.7312(2) 0.5991(3) 0.53640(14) 0.0101(5) Uani 1 1 d . . . . . C009 C 0.4958(2) 0.6680(2) 0.46069(13) 0.0069(5) Uani 1 1 d . . . . . C00A C 0.5556(2) 0.4879(3) 0.30968(13) 0.0078(5) Uani 1 1 d . . . . . C00B C 0.6475(3) 0.6738(3) 0.56665(14) 0.0117(5) Uani 1 1 d . . . . . H00B H 0.6726 0.7017 0.6135 0.014 Uiso 1 1 calc R . . . . C00C C 0.5780(2) 0.5894(3) 0.43031(13) 0.0064(5) Uani 1 1 d . . . . . C00D C 0.6844(3) 0.4216(3) 0.32526(14) 0.0083(5) Uani 1 1 d . . . . . C00E C 0.6974(3) 0.5545(2) 0.46829(16) 0.0097(6) Uani 1 1 d . . . . . H00E H 0.7541 0.5017 0.4482 0.012 Uiso 1 1 calc R . . . . C00F C 0.2910(3) 0.7872(3) 0.42354(15) 0.0130(6) Uani 1 1 d . . . . . C00G C 0.5159(3) 0.5615(2) 0.35870(15) 0.0076(6) Uani 1 1 d . . . . . C00H C 0.7886(3) 0.2195(3) 0.36041(18) 0.0195(6) Uani 1 1 d . . . . . H00A H 0.8328 0.2284 0.3214 0.029 Uiso 1 1 calc GR . . . . H00C H 0.7665 0.1264 0.3657 0.029 Uiso 1 1 calc GR . . . . H00D H 0.8444 0.2504 0.4031 0.029 Uiso 1 1 calc GR . . . . C00I C 0.5286(3) 0.7079(3) 0.52960(14) 0.0108(5) Uani 1 1 d . . . . . H00I H 0.4708 0.7573 0.5506 0.013 Uiso 1 1 calc R . . . . C00J C 0.3910(3) 0.6337(3) 0.34635(14) 0.0097(5) Uani 1 1 d . . . . . C00K C 0.4833(3) 0.4592(3) 0.23852(15) 0.0092(5) Uani 1 1 d . . . . . C00L C 0.5255(3) 0.5079(3) 0.18101(15) 0.0161(6) Uani 1 1 d . . . . . H00L H 0.5987 0.5632 0.1872 0.019 Uiso 1 1 calc R . . . . C00M C 0.0915(3) 0.8925(3) 0.37000(17) 0.0192(6) Uani 1 1 d . . . . . C00N C 0.3782(3) 0.3746(3) 0.22872(15) 0.0157(6) Uani 1 1 d . . . . . H00N H 0.3490 0.3396 0.2677 0.019 Uiso 1 1 calc R . . . . C00O C 0.4615(3) 0.4763(3) 0.11431(16) 0.0211(7) Uani 1 1 d . . . . . H00O H 0.4901 0.5114 0.0752 0.025 Uiso 1 1 calc R . . . . C00P C 0.3162(3) 0.3416(3) 0.16205(17) 0.0206(7) Uani 1 1 d . . . . . H00P H 0.2457 0.2826 0.1556 0.025 Uiso 1 1 calc R . . . . C00Q C 0.3564(3) 0.3940(3) 0.10487(15) 0.0204(7) Uani 1 1 d . . . . . H00Q H 0.3119 0.3735 0.0593 0.024 Uiso 1 1 calc R . . . . C00R C 0.0230(3) 0.8582(4) 0.42830(18) 0.0271(7) Uani 1 1 d . . . . . H00F H -0.0009 0.7643 0.4252 0.041 Uiso 1 1 calc GR . . . . H00G H -0.0539 0.9127 0.4243 0.041 Uiso 1 1 calc GR . . . . H00H H 0.0794 0.8753 0.4731 0.041 Uiso 1 1 calc GR . . . . C00S C 0.0090(3) 0.8673(5) 0.29966(18) 0.0362(9) Uani 1 1 d . . . . . H00J H 0.0581 0.8849 0.2634 0.054 Uiso 1 1 calc GR . . . . H00K H -0.0655 0.9258 0.2931 0.054 Uiso 1 1 calc GR . . . . H00M H -0.0192 0.7748 0.2967 0.054 Uiso 1 1 calc GR . . . . C00T C 0.1419(4) 1.0336(4) 0.3750(4) 0.0530(15) Uani 1 1 d . . . . . H00R H 0.1974 1.0470 0.4205 0.079 Uiso 1 1 calc GR . . . . H00S H 0.0704 1.0958 0.3695 0.079 Uiso 1 1 calc GR . . . . H00T H 0.1906 1.0489 0.3383 0.079 Uiso 1 1 calc GR . . . . 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 I001 0.01333(15) 0.01823(15) 0.01919(15) -0.00041(6) -0.01030(9) -0.00035(6) O002 0.0070(9) 0.0084(9) 0.0281(11) 0.0029(8) 0.0012(8) 0.0024(7) O003 0.0095(9) 0.0161(10) 0.0174(10) -0.0041(8) 0.0000(8) 0.0085(8) O004 0.0079(10) 0.0181(10) 0.0346(13) 0.0034(9) 0.0068(9) -0.0018(8) O005 0.0202(11) 0.0346(13) 0.0135(10) -0.0094(9) -0.0073(9) 0.0184(10) N006 0.0071(10) 0.0052(10) 0.0103(10) -0.0024(8) -0.0003(8) 0.0004(8) O007 0.0243(13) 0.0507(17) 0.0317(13) -0.0303(12) -0.0093(10) 0.0223(12) C008 0.0082(12) 0.0060(12) 0.0132(12) 0.0027(10) -0.0047(10) -0.0046(10) C009 0.0069(12) 0.0022(11) 0.0110(12) 0.0009(9) 0.0006(10) -0.0024(9) C00A 0.0064(12) 0.0066(12) 0.0102(12) -0.0003(10) 0.0012(10) -0.0001(10) C00B 0.0148(14) 0.0092(12) 0.0095(12) -0.0013(10) -0.0016(11) -0.0067(10) C00C 0.0084(12) 0.0020(10) 0.0082(12) 0.0012(10) 0.0004(10) -0.0020(10) C00D 0.0070(13) 0.0094(11) 0.0081(12) -0.0026(10) 0.0004(10) 0.0016(10) C00E 0.0072(14) 0.0070(14) 0.0137(15) 0.0010(9) -0.0012(11) 0.0005(8) C00F 0.0068(12) 0.0127(13) 0.0186(14) -0.0046(11) -0.0002(11) 0.0032(10) C00G 0.0059(13) 0.0063(13) 0.0097(14) 0.0007(9) -0.0009(11) 0.0000(9) C00H 0.0103(14) 0.0099(13) 0.0353(18) 0.0025(12) -0.0031(12) 0.0063(11) C00I 0.0136(13) 0.0084(12) 0.0105(12) -0.0016(10) 0.0026(10) -0.0015(10) C00J 0.0093(13) 0.0093(12) 0.0100(13) -0.0020(10) 0.0002(10) 0.0016(10) C00K 0.0094(14) 0.0079(13) 0.0095(13) -0.0028(9) 0.0000(11) 0.0052(9) C00L 0.0224(15) 0.0115(14) 0.0143(14) 0.0004(11) 0.0034(12) 0.0014(11) C00M 0.0106(14) 0.0202(16) 0.0272(16) 0.0003(12) 0.0047(12) 0.0110(12) C00N 0.0119(13) 0.0214(15) 0.0139(13) -0.0052(11) 0.0025(11) -0.0018(11) C00O 0.0372(19) 0.0159(13) 0.0099(14) 0.0031(12) 0.0037(14) 0.0093(14) C00P 0.0137(14) 0.0250(17) 0.0205(15) -0.0125(13) -0.0031(12) 0.0034(12) C00Q 0.0253(16) 0.0189(16) 0.0125(13) -0.0077(12) -0.0068(12) 0.0180(13) C00R 0.0166(16) 0.042(2) 0.0236(16) -0.0025(15) 0.0060(13) 0.0122(14) C00S 0.0182(17) 0.068(3) 0.0221(17) 0.0060(17) 0.0023(14) 0.0242(17) C00T 0.026(2) 0.0150(17) 0.117(5) 0.005(2) 0.010(3) 0.0097(16) _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 I001 C008 2.097(3) . ? O002 C00D 1.323(4) . ? O002 C00H 1.457(3) . ? O003 C00F 1.310(4) . ? O003 C00M 1.488(3) . ? O004 C00D 1.204(4) . ? O005 C00J 1.196(4) . ? N006 C009 1.420(3) . ? N006 C00F 1.410(3) . ? N006 C00J 1.433(3) . ? O007 C00F 1.202(4) . ? C008 C00B 1.390(4) . ? C008 C00E 1.390(4) . ? C009 C00C 1.401(4) . ? C009 C00I 1.389(4) . ? C00A C00D 1.509(4) . ? C00A C00G 1.349(4) . ? C00A C00K 1.487(4) . ? C00B H00B 0.9500 . ? C00B C00I 1.380(4) . ? C00C C00E 1.393(4) . ? C00C C00G 1.460(4) . ? C00E H00E 0.9500 . ? C00G C00J 1.500(4) . ? C00H H00A 0.9800 . ? C00H H00C 0.9800 . ? C00H H00D 0.9800 . ? C00I H00I 0.9500 . ? C00K C00L 1.386(4) . ? C00K C00N 1.395(4) . ? C00L H00L 0.9500 . ? C00L C00O 1.391(4) . ? C00M C00R 1.515(4) . ? C00M C00S 1.508(5) . ? C00M C00T 1.519(5) . ? C00N H00N 0.9500 . ? C00N C00P 1.387(4) . ? C00O H00O 0.9500 . ? C00O C00Q 1.381(5) . ? C00P H00P 0.9500 . ? C00P C00Q 1.384(5) . ? C00Q H00Q 0.9500 . ? C00R H00F 0.9800 . ? C00R H00G 0.9800 . ? C00R H00H 0.9800 . ? C00S H00J 0.9800 . ? C00S H00K 0.9800 . ? C00S H00M 0.9800 . ? C00T H00R 0.9800 . ? C00T H00S 0.9800 . ? C00T H00T 0.9800 . ? 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 C00D O002 C00H 116.3(2) . . ? C00F O003 C00M 120.6(2) . . ? C009 N006 C00J 109.5(2) . . ? C00F N006 C009 122.6(2) . . ? C00F N006 C00J 127.2(2) . . ? C00B C008 I001 119.13(19) . . ? C00E C008 I001 119.6(2) . . ? C00E C008 C00B 121.2(3) . . ? C00C C009 N006 109.7(2) . . ? C00I C009 N006 129.0(2) . . ? C00I C009 C00C 121.2(2) . . ? C00G C00A C00D 120.2(2) . . ? C00G C00A C00K 126.8(2) . . ? C00K C00A C00D 113.0(2) . . ? C008 C00B H00B 119.5 . . ? C00I C00B C008 121.0(2) . . ? C00I C00B H00B 119.5 . . ? C009 C00C C00G 108.3(2) . . ? C00E C00C C009 120.1(2) . . ? C00E C00C C00G 131.6(2) . . ? O002 C00D C00A 109.9(2) . . ? O004 C00D O002 126.3(3) . . ? O004 C00D C00A 123.8(3) . . ? C008 C00E C00C 118.1(3) . . ? C008 C00E H00E 120.9 . . ? C00C C00E H00E 120.9 . . ? O003 C00F N006 111.2(2) . . ? O007 C00F O003 127.1(3) . . ? O007 C00F N006 121.7(3) . . ? C00A C00G C00C 130.2(3) . . ? C00A C00G C00J 123.2(3) . . ? C00C C00G C00J 106.5(2) . . ? O002 C00H H00A 109.5 . . ? O002 C00H H00C 109.5 . . ? O002 C00H H00D 109.5 . . ? H00A C00H H00C 109.5 . . ? H00A C00H H00D 109.5 . . ? H00C C00H H00D 109.5 . . ? C009 C00I H00I 120.9 . . ? C00B C00I C009 118.1(3) . . ? C00B C00I H00I 120.9 . . ? O005 C00J N006 126.1(2) . . ? O005 C00J C00G 128.1(3) . . ? N006 C00J C00G 105.8(2) . . ? C00L C00K C00A 120.2(3) . . ? C00L C00K C00N 119.2(3) . . ? C00N C00K C00A 120.4(3) . . ? C00K C00L H00L 119.8 . . ? C00K C00L C00O 120.4(3) . . ? C00O C00L H00L 119.8 . . ? O003 C00M C00R 110.8(2) . . ? O003 C00M C00S 101.4(2) . . ? O003 C00M C00T 109.0(3) . . ? C00R C00M C00T 112.6(4) . . ? C00S C00M C00R 111.7(3) . . ? C00S C00M C00T 110.8(4) . . ? C00K C00N H00N 120.0 . . ? C00P C00N C00K 120.1(3) . . ? C00P C00N H00N 120.0 . . ? C00L C00O H00O 119.9 . . ? C00Q C00O C00L 120.1(3) . . ? C00Q C00O H00O 119.9 . . ? C00N C00P H00P 119.8 . . ? C00Q C00P C00N 120.4(3) . . ? C00Q C00P H00P 119.8 . . ? C00O C00Q C00P 119.7(3) . . ? C00O C00Q H00Q 120.1 . . ? C00P C00Q H00Q 120.1 . . ? C00M C00R H00F 109.5 . . ? C00M C00R H00G 109.5 . . ? C00M C00R H00H 109.5 . . ? H00F C00R H00G 109.5 . . ? H00F C00R H00H 109.5 . . ? H00G C00R H00H 109.5 . . ? C00M C00S H00J 109.5 . . ? C00M C00S H00K 109.5 . . ? C00M C00S H00M 109.5 . . ? H00J C00S H00K 109.5 . . ? H00J C00S H00M 109.5 . . ? H00K C00S H00M 109.5 . . ? C00M C00T H00R 109.5 . . ? C00M C00T H00S 109.5 . . ? C00M C00T H00T 109.5 . . ? H00R C00T H00S 109.5 . . ? H00R C00T H00T 109.5 . . ? H00S C00T H00T 109.5 . . ? _shelx_res_file ; s.res created by SHELXL-2014/7 TITL s_a.res in P2(1)/c REM Old TITL s in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.133, Rweak 0.005, Alpha 0.048, Orientation as input REM Formula found by SHELXT: C22 N O5 I CELL 1.54178 10.7031 10.096 19.6338 90 101.314 90 ZERR 4 0.0014 0.0013 0.0025 0 0.003 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H I N O UNIT 88 80 4 4 20 L.S. 4 PLAN 20 SIZE 0.5 0.4 0.3 TEMP -120.16 BOND $H list 4 fmap 2 ACTA OMIT 0 1 1 OMIT -1 5 5 OMIT 3 1 1 REM REM REM WGHT 0.060100 3.304500 FVAR 0.43460 I001 3 0.911964 0.553913 0.594831 11.00000 0.01333 0.01823 = 0.01919 -0.00041 -0.01030 -0.00035 O002 5 0.672757 0.299064 0.347033 11.00000 0.00696 0.00842 = 0.02814 0.00289 0.00120 0.00237 O003 5 0.198959 0.799523 0.369062 11.00000 0.00947 0.01611 = 0.01743 -0.00414 0.00004 0.00848 O004 5 0.781675 0.474522 0.317853 11.00000 0.00790 0.01814 = 0.03462 0.00342 0.00675 -0.00184 O005 5 0.312880 0.640400 0.293781 11.00000 0.02019 0.03458 = 0.01349 -0.00944 -0.00734 0.01836 N006 4 0.383323 0.695617 0.411067 11.00000 0.00709 0.00523 = 0.01027 -0.00244 -0.00034 0.00044 O007 5 0.301230 0.844456 0.478052 11.00000 0.02431 0.05072 = 0.03172 -0.03034 -0.00926 0.02233 C008 1 0.731217 0.599062 0.536398 11.00000 0.00816 0.00602 = 0.01323 0.00274 -0.00475 -0.00460 C009 1 0.495803 0.667956 0.460686 11.00000 0.00693 0.00217 = 0.01099 0.00091 0.00059 -0.00243 C00A 1 0.555588 0.487871 0.309679 11.00000 0.00643 0.00663 = 0.01024 -0.00033 0.00120 -0.00013 C00B 1 0.647535 0.673752 0.566652 11.00000 0.01477 0.00915 = 0.00953 -0.00125 -0.00160 -0.00670 AFIX 43 H00B 2 0.672584 0.701713 0.613549 11.00000 -1.20000 AFIX 0 C00C 1 0.577983 0.589437 0.430314 11.00000 0.00844 0.00200 = 0.00819 0.00123 0.00039 -0.00205 C00D 1 0.684390 0.421581 0.325263 11.00000 0.00696 0.00942 = 0.00811 -0.00262 0.00038 0.00157 C00E 1 0.697383 0.554510 0.468287 11.00000 0.00717 0.00703 = 0.01370 0.00097 -0.00117 0.00055 AFIX 43 H00E 2 0.754120 0.501709 0.448197 11.00000 -1.20000 AFIX 0 C00F 1 0.290969 0.787195 0.423535 11.00000 0.00680 0.01265 = 0.01857 -0.00460 -0.00018 0.00315 C00G 1 0.515857 0.561496 0.358697 11.00000 0.00592 0.00634 = 0.00966 0.00068 -0.00089 0.00004 C00H 1 0.788581 0.219544 0.360409 11.00000 0.01029 0.00987 = 0.03525 0.00253 -0.00307 0.00631 AFIX 137 H00A 2 0.832791 0.228355 0.321407 11.00000 -1.50000 H00C 2 0.766487 0.126411 0.365693 11.00000 -1.50000 H00D 2 0.844375 0.250374 0.403127 11.00000 -1.50000 AFIX 0 C00I 1 0.528636 0.707899 0.529604 11.00000 0.01365 0.00840 = 0.01047 -0.00164 0.00265 -0.00153 AFIX 43 H00I 2 0.470842 0.757339 0.550634 11.00000 -1.20000 AFIX 0 C00J 1 0.390995 0.633685 0.346349 11.00000 0.00927 0.00926 = 0.00997 -0.00195 0.00017 0.00158 C00K 1 0.483263 0.459193 0.238519 11.00000 0.00935 0.00791 = 0.00950 -0.00282 0.00005 0.00522 C00L 1 0.525527 0.507887 0.181006 11.00000 0.02237 0.01148 = 0.01435 0.00041 0.00338 0.00144 AFIX 43 H00L 2 0.598701 0.563185 0.187194 11.00000 -1.20000 AFIX 0 C00M 1 0.091456 0.892515 0.370001 11.00000 0.01058 0.02016 = 0.02725 0.00026 0.00474 0.01100 C00N 1 0.378172 0.374630 0.228715 11.00000 0.01190 0.02139 = 0.01391 -0.00522 0.00248 -0.00184 AFIX 43 H00N 2 0.349037 0.339650 0.267731 11.00000 -1.20000 AFIX 0 C00O 1 0.461493 0.476307 0.114309 11.00000 0.03718 0.01585 = 0.00992 0.00307 0.00369 0.00933 AFIX 43 H00O 2 0.490094 0.511396 0.075155 11.00000 -1.20000 AFIX 0 C00P 1 0.316184 0.341582 0.162054 11.00000 0.01368 0.02500 = 0.02049 -0.01255 -0.00314 0.00338 AFIX 43 H00P 2 0.245696 0.282586 0.155604 11.00000 -1.20000 AFIX 0 C00Q 1 0.356398 0.394031 0.104875 11.00000 0.02529 0.01895 = 0.01254 -0.00770 -0.00677 0.01800 AFIX 43 H00Q 2 0.311896 0.373527 0.059321 11.00000 -1.20000 AFIX 0 C00R 1 0.022990 0.858179 0.428305 11.00000 0.01661 0.04194 = 0.02358 -0.00249 0.00602 0.01220 AFIX 137 H00F 2 -0.000864 0.764337 0.425230 11.00000 -1.50000 H00G 2 -0.053884 0.912675 0.424275 11.00000 -1.50000 H00H 2 0.079443 0.875322 0.473112 11.00000 -1.50000 AFIX 0 C00S 1 0.009007 0.867310 0.299660 11.00000 0.01821 0.06775 = 0.02208 0.00604 0.00231 0.02420 AFIX 137 H00J 2 0.058111 0.884935 0.263435 11.00000 -1.50000 H00K 2 -0.065451 0.925821 0.293106 11.00000 -1.50000 H00M 2 -0.019235 0.774788 0.296713 11.00000 -1.50000 AFIX 0 C00T 1 0.141934 1.033570 0.375009 11.00000 0.02581 0.01495 = 0.11650 0.00532 0.00991 0.00971 AFIX 137 H00R 2 0.197439 1.047042 0.420482 11.00000 -1.50000 H00S 2 0.070370 1.095789 0.369451 11.00000 -1.50000 H00T 2 0.190551 1.048853 0.338324 11.00000 -1.50000 AFIX 0 HKLF 4 REM s_a.res in P2(1)/c REM R1 = 0.0366 for 3795 Fo > 4sig(Fo) and 0.0366 for all 3796 data REM 266 parameters refined using 0 restraints END WGHT 0.0601 3.3045 REM Highest difference peak 0.816, deepest hole -1.788, 1-sigma level 0.146 Q1 1 0.8045 0.5556 0.5767 11.00000 0.05 0.82 Q2 1 1.0260 0.5544 0.6089 11.00000 0.05 0.78 Q3 1 0.9651 0.6644 0.6370 11.00000 0.05 0.60 Q4 1 0.8616 0.6628 0.5520 11.00000 0.05 0.55 Q5 1 0.9061 0.5010 0.4368 11.00000 0.05 0.49 Q6 1 0.2800 0.5563 0.3866 11.00000 0.05 0.46 Q7 1 0.8696 0.4382 0.5507 11.00000 0.05 0.45 Q8 1 -0.0001 0.6656 0.3693 11.00000 0.05 0.45 Q9 1 0.9561 0.4396 0.6370 11.00000 0.05 0.43 Q10 1 0.9196 0.4189 0.5146 11.00000 0.05 0.40 Q11 1 0.9217 0.6777 0.5171 11.00000 0.05 0.38 Q12 1 0.1438 1.2162 0.4353 11.00000 0.05 0.37 Q13 1 0.8672 0.3857 0.3762 11.00000 0.05 0.37 Q14 1 0.1305 0.5810 0.3215 11.00000 0.05 0.37 Q15 1 0.1810 0.6415 0.4575 11.00000 0.05 0.37 Q16 1 0.6135 0.4606 0.3156 11.00000 0.05 0.36 Q17 1 0.1278 0.6882 0.4435 11.00000 0.05 0.35 Q18 1 0.9179 0.3680 0.4376 11.00000 0.05 0.34 Q19 1 0.5338 0.6252 0.4470 11.00000 0.05 0.32 Q20 1 -0.1054 0.9930 0.3812 11.00000 0.05 0.32 ; _shelx_res_checksum 24731 _shelx_hkl_file ; 1 0 0 360.86 26.10 -2 0 0 589.84 46.50 2 0 0 651.93 47.70 3 0 0 398.06 34.70 -3 0 0 402.06 33.40 -3 0 0 443.76 30.80 -4 0 0 349.87 31.60 -4 0 0 409.96 27.40 -4 0 0 359.06 28.10 5 0 0 7666.33 547.05 -6 0 0 636.04 48.80 6 0 0 666.73 47.10 -6 0 0 724.43 46.70 6 0 0 583.64 56.59 7 0 0 2726.13 183.08 7 0 0 2526.65 181.48 7 0 0 2451.15 181.68 -7 0 0 2511.65 184.08 -7 0 0 2717.13 181.28 8 0 0 391.26 36.30 8 0 0 387.96 30.40 -8 0 0 464.85 30.00 -8 0 0 424.76 33.30 9 0 0 313.27 23.40 9 0 0 334.77 30.50 9 0 0 315.67 23.60 9 0 0 295.87 24.10 -9 0 0 307.47 26.30 -9 0 0 319.27 23.30 -9 0 0 355.06 23.20 -9 0 0 321.17 23.00 10 0 0 2760.32 187.88 -10 0 0 2386.16 190.78 10 0 0 2519.45 188.58 10 0 0 2782.62 188.18 10 0 0 2943.61 198.08 -11 0 0 884.41 63.49 11 0 0 860.91 62.19 11 0 0 905.81 62.59 -11 0 0 860.51 62.19 -12 0 0 455.35 37.00 12 0 0 563.04 36.70 12 0 0 493.85 36.70 12 0 0 533.75 36.40 0 -1 0 4.40 0.70 0 1 0 5.40 0.70 1 -1 0 542.95 40.00 1 -1 0 495.25 40.20 1 -1 0 644.64 40.70 -1 1 0 614.84 40.10 -1 1 0 500.35 40.60 1 1 0 555.54 40.20 1 1 0 625.94 40.90 -2 -1 0 182.58 13.20 2 -1 0 153.78 13.70 -2 -1 0 143.89 15.00 -2 1 0 153.28 13.80 -2 1 0 184.48 12.40 3 -1 0 1361.66 115.59 -3 -1 0 1601.64 117.59 3 1 0 1664.93 112.69 -3 1 0 1762.32 115.99 -4 -1 0 75.99 6.90 -4 -1 0 78.49 6.40 4 -1 0 55.39 8.90 -4 1 0 65.49 6.10 4 1 0 77.59 12.00 4 1 0 56.59 5.80 -4 1 0 70.89 8.70 5 -1 0 117.89 9.50 -5 -1 0 129.89 9.30 -5 -1 0 143.39 10.80 5 1 0 136.99 18.10 5 1 0 104.39 15.50 -5 1 0 130.79 14.20 -5 1 0 115.79 10.30 5 1 0 118.79 12.50 5 1 0 113.09 9.40 -6 -1 0 167.38 15.60 -6 -1 0 203.78 13.30 -6 -1 0 172.88 13.00 -6 -1 0 200.48 13.30 6 -1 0 185.08 13.70 6 1 0 167.78 17.30 6 1 0 152.88 14.10 6 1 0 182.68 24.60 -6 1 0 192.28 13.10 6 1 0 191.78 13.60 6 1 0 169.88 13.10 6 1 0 166.28 13.30 -6 1 0 155.08 14.50 -7 -1 0 395.76 27.70 7 -1 0 379.76 28.00 7 -1 0 350.36 28.00 -7 -1 0 323.67 30.50 7 -1 0 387.16 28.70 -7 -1 0 434.56 28.00 7 1 0 371.36 27.80 -7 1 0 445.96 27.90 7 1 0 394.26 28.10 7 1 0 388.46 33.60 7 1 0 381.76 28.40 7 1 0 388.46 33.60 -7 1 0 394.86 29.90 -7 1 0 382.76 27.60 7 1 0 389.46 29.20 -8 -1 0 405.36 27.30 8 -1 0 355.96 27.60 8 -1 0 363.26 27.60 8 -1 0 333.67 29.10 8 -1 0 402.36 28.40 -8 -1 0 405.96 27.60 8 1 0 327.57 27.60 -8 1 0 367.76 29.60 8 1 0 367.36 27.40 8 1 0 388.96 27.70 -8 1 0 392.26 27.30 -8 1 0 398.46 27.10 -8 1 0 430.86 27.40 8 1 0 374.16 28.10 9 -1 0 35.30 3.70 -9 -1 0 35.20 3.40 9 -1 0 38.50 8.20 -9 -1 0 37.40 3.20 9 -1 0 30.30 4.00 -9 -1 0 35.30 5.80 9 -1 0 34.00 3.50 9 1 0 37.50 3.80 9 1 0 29.80 3.40 -9 1 0 38.90 3.30 9 1 0 18.60 6.90 -9 1 0 31.30 5.20 9 1 0 34.80 3.90 9 1 0 34.80 3.30 -10 -1 0 340.87 22.70 10 -1 0 320.37 23.20 -10 -1 0 282.67 26.60 10 -1 0 281.77 23.90 10 -1 0 328.57 23.40 -10 -1 0 345.27 23.20 -10 1 0 320.67 22.90 10 1 0 299.07 22.90 10 1 0 343.67 23.50 10 1 0 311.07 31.10 -10 1 0 331.47 24.10 10 1 0 273.77 23.50 -11 -1 0 247.28 17.80 11 -1 0 246.68 17.80 11 -1 0 247.88 18.00 11 1 0 204.28 17.80 -11 1 0 246.48 18.60 11 1 0 232.78 17.60 -11 1 0 241.68 17.60 11 1 0 260.37 18.10 12 -1 0 45.30 4.50 12 -1 0 46.80 4.20 -12 -1 0 42.30 4.60 12 -1 0 52.09 4.20 -12 1 0 43.90 4.50 12 1 0 52.69 4.40 12 1 0 46.80 3.80 0 -2 0 3944.01 277.17 1 2 0 1293.57 82.49 1 2 0 1083.69 84.29 1 2 0 1101.49 81.99 2 -2 0 3218.98 199.38 2 2 0 2421.26 202.28 3 -2 0 1643.34 116.79 -3 -2 0 1785.42 116.59 -3 2 0 1678.83 117.29 3 2 0 1393.16 120.59 -4 -2 0 339.47 24.10 -4 -2 0 348.37 25.90 -4 2 0 374.76 24.60 4 2 0 316.67 24.00 4 2 0 306.67 31.90 4 2 0 290.37 24.70 4 2 0 312.17 26.90 -4 2 0 376.16 27.90 -5 -2 0 3371.16 224.08 5 -2 0 3237.48 222.08 -5 -2 0 3170.48 221.78 5 2 0 3366.56 235.48 5 2 0 2987.50 233.48 5 2 0 2846.92 222.68 -6 -2 0 3195.38 214.78 6 -2 0 3040.30 215.48 -6 -2 0 3400.16 214.98 -6 -2 0 3085.59 214.58 -6 -2 0 3275.57 218.68 6 2 0 2783.52 219.68 -6 2 0 3367.56 214.68 6 2 0 3005.20 214.88 6 2 0 3042.10 231.08 6 2 0 2964.50 216.18 6 2 0 2815.32 214.68 6 2 0 2776.62 219.68 7 -2 0 635.64 48.90 -7 -2 0 718.63 48.40 7 -2 0 638.74 49.50 -7 -2 0 755.32 49.00 -7 -2 0 688.73 48.70 7 2 0 596.44 53.89 7 2 0 620.34 48.60 -7 2 0 738.93 49.20 -7 2 0 733.03 48.60 7 2 0 647.14 50.09 7 2 0 669.63 48.90 -7 2 0 774.22 50.29 8 -2 0 61.59 5.90 -8 -2 0 52.49 7.80 8 -2 0 49.60 4.80 -8 -2 0 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-3 0 0.20 1.00 0 3 0 2.40 0.70 1 -3 0 4188.98 302.97 1 3 0 4255.07 305.07 -1 3 0 4511.85 303.37 -1 3 0 4298.57 302.87 -2 -3 0 1212.48 93.69 -2 -3 0 1087.69 92.49 2 -3 0 1400.46 92.09 2 -3 0 1335.37 91.99 2 3 0 1133.69 91.49 2 3 0 1283.37 96.39 2 3 0 1469.25 96.49 -2 3 0 1412.26 91.79 -2 3 0 1266.27 91.99 3 -3 0 3277.27 210.78 3 3 0 2852.61 216.58 3 3 0 2668.13 209.38 3 3 0 3235.98 216.88 -3 3 0 2837.72 210.58 -4 -3 0 862.91 56.79 4 -3 0 803.92 57.19 -4 -3 0 711.63 53.69 4 3 0 656.33 54.69 -4 3 0 826.42 56.89 4 3 0 674.13 62.89 5 -3 0 229.38 15.60 -5 -3 0 238.28 18.90 -5 -3 0 178.98 14.70 -5 -3 0 197.48 15.30 -5 -3 0 215.18 15.00 -5 -3 0 215.08 18.10 5 3 0 178.98 16.30 5 3 0 207.18 25.10 5 3 0 177.78 18.30 5 3 0 207.38 15.10 -6 -3 0 100.69 8.20 -6 -3 0 113.09 11.10 -6 -3 0 108.09 7.70 -6 -3 0 102.99 7.80 -6 -3 0 102.69 8.00 -6 -3 0 93.29 10.90 6 -3 0 111.09 8.60 -6 3 0 105.59 8.50 6 3 0 98.79 8.00 6 3 0 98.09 11.70 6 3 0 80.39 9.00 6 3 0 93.19 8.10 -6 3 0 106.09 8.20 6 3 0 90.29 7.60 6 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875.91 65.89 -10 3 0 914.31 64.29 -10 3 0 897.01 65.49 -10 3 0 881.91 64.79 10 3 0 912.71 64.29 10 3 0 837.42 64.99 10 3 0 957.20 64.89 11 -3 0 16.90 2.10 11 -3 0 15.70 2.80 -11 -3 0 21.30 2.10 11 -3 0 18.30 2.40 -11 3 0 17.00 2.50 11 3 0 14.20 2.30 11 3 0 22.50 2.70 -12 -3 0 85.29 7.90 12 -3 0 96.89 7.30 12 -3 0 97.69 7.90 12 -3 0 91.59 7.10 12 3 0 104.09 7.30 -12 3 0 91.79 7.50 12 3 0 89.49 7.30 0 -4 0 7.30 2.50 0 4 0 8.00 1.00 0 4 0 12.80 2.90 0 4 0 8.00 2.60 0 4 0 8.00 2.30 1 -4 0 14.90 2.70 1 -4 0 13.80 3.00 -1 -4 0 17.40 3.10 -1 4 0 25.10 3.20 -1 4 0 23.40 3.40 1 4 0 23.00 4.40 1 4 0 19.10 2.90 2 -4 0 119.59 10.20 2 -4 0 113.59 9.40 -2 -4 0 97.29 11.80 -2 -4 0 99.79 10.40 2 4 0 123.49 13.60 -2 4 0 110.89 9.50 2 4 0 104.09 9.80 2 4 0 112.29 13.40 -3 -4 0 2604.44 192.98 3 4 0 2942.11 194.78 3 4 0 3060.89 203.08 -3 4 0 2409.66 194.18 -4 -4 0 153.28 14.80 -4 -4 0 139.89 11.60 -4 -4 0 159.48 15.60 4 4 0 176.08 14.90 4 4 0 135.09 12.80 -5 -4 0 41.80 3.60 5 -4 0 45.00 4.10 -5 -4 0 36.00 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57.59 1 8 0 753.12 56.89 -1 8 0 789.02 58.09 2 -8 0 133.39 15.60 2 -8 0 138.59 10.90 -2 -8 0 123.29 10.10 -2 -8 0 123.49 10.30 -2 -8 0 136.09 11.40 2 8 0 140.39 9.80 -2 8 0 145.59 11.30 -2 8 0 123.69 10.50 2 8 0 128.19 14.20 2 8 0 127.19 10.30 -2 8 0 126.79 10.60 2 8 0 128.59 9.90 -2 8 0 129.39 10.00 -2 8 0 133.29 10.30 -3 -8 0 25.40 8.70 -3 -8 0 40.00 3.50 3 -8 0 36.40 3.90 -3 -8 0 36.00 4.40 -3 -8 0 29.00 3.30 3 8 0 30.90 7.70 -3 8 0 31.20 3.20 3 8 0 29.50 3.10 3 8 0 36.40 3.20 -3 8 0 32.00 3.40 -3 8 0 34.70 3.80 3 8 0 31.30 3.40 -4 -8 0 482.85 34.30 4 -8 0 547.25 35.20 -4 -8 0 509.75 35.60 -4 -8 0 402.96 34.20 -4 8 0 428.56 34.50 4 8 0 469.95 38.80 -4 8 0 443.36 34.70 -4 8 0 471.45 34.10 4 8 0 531.45 34.20 4 8 0 453.55 34.20 4 8 0 469.85 34.00 -4 8 0 491.15 34.20 -5 -8 0 1389.06 107.69 -5 -8 0 1437.66 114.99 -5 -8 0 1561.64 107.79 -5 -8 0 1617.64 117.49 5 8 0 1562.24 112.39 5 8 0 1763.82 107.89 5 8 0 1374.46 107.49 -5 8 0 1378.96 107.99 5 8 0 1626.54 107.59 -5 8 0 1563.14 107.69 -6 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134.59 10 -1 9 1596.44 105.59 -10 -1 -9 1439.86 105.29 10 -1 9 1522.35 106.39 -10 1 -9 1456.95 105.29 10 1 9 1476.95 105.39 -12 -2 9 208.18 13.60 -12 -2 9 176.38 13.70 -12 -2 9 192.98 14.00 12 -2 -9 189.28 13.90 12 -2 -9 196.98 13.50 12 2 -9 184.28 13.60 -12 2 9 162.08 13.60 12 2 -9 188.38 13.90 11 -2 -9 118.09 8.90 11 -2 -9 108.19 9.30 -11 -2 9 123.89 9.00 -11 -2 9 120.89 8.90 11 -2 -9 123.69 9.30 11 2 -9 117.39 8.90 -11 2 9 109.69 8.90 -11 2 9 110.59 9.00 10 -2 -9 173.88 13.00 10 -2 -9 159.28 13.50 -10 -2 9 180.88 13.00 10 -2 -9 187.68 13.40 -10 -2 9 175.68 13.00 10 2 -9 175.78 12.90 -10 2 9 166.28 13.10 -10 2 9 170.08 13.30 -10 2 9 167.28 12.40 -9 -2 9 749.33 50.29 -9 -2 9 760.22 50.99 9 -2 -9 688.13 50.59 -9 -2 9 723.43 50.59 9 -2 -9 709.83 50.99 -9 -2 9 705.03 50.59 9 2 -9 716.33 50.49 9 2 -9 726.73 56.49 -9 2 9 700.13 50.19 -9 2 9 643.44 53.89 -9 2 9 686.63 51.09 -8 -2 9 468.25 33.60 8 -2 -9 503.95 34.20 -8 -2 9 461.55 33.60 -8 -2 9 461.95 33.50 8 -2 -9 443.36 33.60 8 -2 -9 416.56 34.30 8 2 -9 475.05 33.30 8 2 -9 470.55 33.50 8 2 -9 517.15 37.30 -7 -2 9 102.19 7.80 -7 -2 9 95.69 7.70 -7 -2 9 90.29 11.40 -7 -2 9 105.39 8.50 -7 -2 9 90.29 11.40 7 -2 -9 96.69 8.20 7 -2 -9 100.69 7.90 7 -2 -9 97.49 8.60 7 2 -9 103.69 7.50 -7 2 9 102.89 8.10 7 2 -9 97.99 7.30 7 2 -9 101.79 10.60 7 2 -9 108.49 7.80 -7 2 9 76.09 10.60 -6 -2 9 45.70 4.80 -6 -2 9 50.99 4.20 -6 -2 9 62.39 7.80 -6 -2 9 51.09 4.30 6 -2 -9 47.90 4.50 6 -2 -9 54.39 4.50 6 -2 -9 45.30 4.80 6 2 -9 51.89 4.20 -6 2 9 46.40 7.10 -6 2 9 44.00 3.80 6 2 -9 51.99 4.30 -6 2 9 60.09 4.60 -5 -2 9 362.26 28.00 5 -2 -9 392.06 27.60 5 -2 -9 400.06 28.30 5 -2 -9 386.06 27.70 -5 2 9 402.26 27.70 -5 2 9 382.06 27.50 5 2 -9 421.76 27.50 -5 2 9 352.86 27.10 5 2 -9 345.17 29.80 -4 -2 9 623.44 55.69 -4 -2 9 630.84 55.79 4 -2 -9 682.23 47.40 4 -2 -9 594.54 56.99 4 -2 -9 729.43 48.00 4 -2 -9 696.73 47.30 -4 2 9 580.84 56.39 -4 2 9 688.73 47.40 4 2 -9 689.33 49.60 -4 2 9 691.83 47.40 -3 -2 9 248.98 24.50 -3 -2 9 233.88 19.30 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80.29 7.70 3 2 9 76.19 7.00 4 -2 9 126.09 10.50 4 -2 9 149.69 14.10 -4 -2 -9 132.09 9.70 4 -2 9 122.89 13.50 4 2 9 106.39 9.80 4 2 9 117.09 16.00 4 2 9 116.99 10.50 4 2 9 116.69 10.10 -4 2 -9 140.39 9.40 4 2 9 108.49 9.70 -4 2 -9 130.59 10.50 -4 2 -9 118.49 9.40 -4 2 -9 139.69 10.50 5 -2 9 94.49 12.10 5 -2 9 99.59 7.80 -5 -2 -9 106.09 7.50 -5 -2 -9 70.99 10.20 5 -2 9 75.79 7.30 5 2 9 85.09 7.60 5 2 9 84.79 8.10 -5 2 -9 104.59 7.60 -5 2 -9 93.19 8.30 5 2 9 80.39 13.60 -5 2 -9 99.79 8.20 5 2 9 87.69 8.50 -5 2 -9 106.89 7.20 -6 -2 -9 720.53 45.00 6 -2 9 719.63 45.50 -6 -2 -9 569.54 45.70 6 2 9 555.64 54.99 -6 2 -9 674.03 45.20 6 2 9 603.54 45.90 -6 2 -9 611.04 46.10 -6 2 -9 665.43 44.70 -6 2 -9 578.14 45.50 6 2 9 583.14 45.30 -7 -2 -9 970.50 68.99 -7 -2 -9 885.21 70.19 7 -2 9 1043.70 69.69 7 -2 9 1070.49 70.89 -7 -2 -9 997.10 69.09 -7 2 -9 900.41 68.89 -7 2 -9 997.10 70.79 7 2 9 1031.30 70.39 -7 2 -9 980.30 69.49 7 2 9 959.70 80.89 7 2 9 935.61 69.69 8 -2 9 304.77 21.50 8 -2 9 303.37 20.40 8 -2 9 232.78 20.00 -8 -2 -9 235.68 20.70 8 2 9 275.47 20.40 -8 2 -9 270.87 20.10 8 2 9 305.67 21.00 -9 -2 -9 360.46 25.80 9 -2 9 351.46 26.80 9 -2 9 398.26 25.90 -9 -2 -9 308.57 26.20 -9 2 -9 315.57 25.50 9 2 9 361.96 25.80 -9 2 -9 400.66 27.30 -9 2 -9 352.36 25.60 10 -2 9 83.59 6.80 10 -2 9 84.79 6.10 -10 -2 -9 71.79 5.90 -10 -2 -9 65.59 6.20 10 2 9 77.19 5.80 -10 2 -9 72.49 6.80 -10 2 -9 74.79 5.70 10 2 9 70.19 6.10 -12 -3 9 149.99 11.50 12 -3 -9 165.48 11.50 -12 -3 9 170.88 11.50 12 -3 -9 151.58 11.70 12 3 -9 156.38 11.30 -12 3 9 151.98 11.40 -11 -3 9 164.38 11.90 -11 -3 9 154.88 11.90 11 -3 -9 166.08 12.30 11 -3 -9 150.78 12.50 11 -3 -9 158.78 12.00 -11 3 9 151.48 11.90 11 3 -9 163.18 11.80 -11 3 9 164.88 12.20 11 3 -9 168.88 12.20 -10 -3 9 16.20 1.90 10 -3 -9 11.40 2.40 10 -3 -9 11.10 2.10 -10 -3 9 15.90 2.20 10 -3 -9 16.50 2.60 -10 -3 9 15.00 1.60 -10 3 9 14.80 2.20 -10 3 9 13.90 2.00 10 3 -9 14.20 1.90 -9 -3 9 82.59 7.10 -9 -3 9 87.29 6.50 -9 -3 9 80.09 6.50 9 -3 -9 72.99 7.40 9 -3 -9 72.89 7.00 -9 -3 9 82.09 10.40 -9 -3 9 88.59 6.70 9 -3 -9 76.09 6.80 9 3 -9 79.29 6.40 9 3 -9 72.99 9.90 -9 3 9 90.59 6.90 -9 3 9 84.99 7.20 9 3 -9 60.09 9.10 -8 -3 9 16.70 2.20 -8 -3 9 15.40 2.60 8 -3 -9 14.80 2.30 8 -3 -9 19.20 2.70 -8 -3 9 17.90 2.30 8 -3 -9 15.00 2.80 -8 3 9 13.50 4.20 -8 3 9 16.20 1.80 8 3 -9 18.50 1.80 8 3 -9 16.80 5.30 -8 3 9 13.40 4.20 8 3 -9 19.80 2.10 -7 -3 9 1091.19 78.09 7 -3 -9 1020.10 78.59 -7 -3 9 1069.89 78.09 -7 -3 9 1194.48 83.19 7 -3 -9 1036.10 78.39 -7 3 9 1131.89 78.49 7 3 -9 1236.48 78.09 7 3 -9 1181.48 77.79 -7 3 9 957.10 81.59 7 3 -9 1140.99 81.59 6 -3 -9 288.27 21.60 6 -3 -9 277.87 22.20 6 -3 -9 296.67 21.40 -6 -3 9 255.17 21.70 -6 -3 9 264.87 21.00 -6 -3 9 292.47 21.20 -6 -3 9 301.97 25.30 6 3 -9 293.27 24.10 6 3 -9 264.87 21.50 -6 3 9 314.57 21.50 6 3 -9 327.37 21.10 6 3 -9 312.77 21.00 6 3 -9 296.87 20.90 5 -3 -9 2.80 1.00 -5 -3 9 2.30 1.00 5 -3 -9 5.20 1.20 5 3 -9 2.80 1.00 5 3 -9 2.00 1.60 5 3 -9 3.00 0.80 -5 3 9 6.70 2.90 5 3 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418.96 30.40 2 4 -21 423.16 30.90 2 4 -21 405.16 30.40 1 -4 -21 199.68 14.30 -1 -4 21 205.58 14.80 1 -4 -21 167.48 14.30 -1 -4 21 209.78 14.20 1 4 -21 197.98 14.00 1 4 -21 196.38 14.10 -1 4 21 210.08 16.40 1 4 -21 182.48 14.50 0 -4 -21 18.20 1.80 0 -4 21 22.60 2.00 0 -4 -21 19.10 2.10 0 -4 21 19.10 2.30 0 4 21 20.20 2.20 0 4 -21 18.20 1.90 0 4 -21 16.20 2.10 0 4 -21 19.60 1.60 0 4 -21 20.00 1.80 1 -4 21 223.58 15.80 1 -4 21 236.38 16.40 -1 -4 -21 210.68 15.90 -1 4 -21 209.48 15.70 -1 4 -21 201.18 15.80 1 4 21 210.98 16.00 -1 4 -21 244.58 16.00 -4 -5 21 26.20 2.70 4 -5 -21 32.10 2.70 -4 -5 21 25.60 2.30 -4 5 21 26.80 2.70 4 5 -21 27.70 2.30 4 5 -21 23.70 2.30 4 5 -21 22.70 2.30 -3 -5 21 69.39 5.60 3 -5 -21 77.09 5.40 -3 -5 21 67.19 5.10 3 5 -21 55.39 5.20 3 5 -21 59.79 5.00 -3 5 21 76.49 5.60 3 5 -21 63.09 5.30 2 -5 -21 46.20 3.60 2 -5 -21 48.90 3.70 -2 -5 21 41.50 3.50 -2 -5 21 44.80 4.00 2 5 -21 42.30 3.40 2 5 -21 40.30 3.30 2 5 -21 48.00 4.00 -2 5 21 47.80 4.00 2 5 -21 38.00 3.70 -1 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-1 22 2.40 1.00 -5 -1 22 2.80 0.80 5 -1 -22 3.20 1.10 5 1 -22 1.60 0.70 5 1 -22 1.90 0.80 -5 1 22 2.70 0.80 -4 -1 22 81.79 6.50 -4 -1 22 80.99 5.90 4 -1 -22 69.89 6.10 -4 1 22 69.99 5.60 4 1 -22 70.39 5.70 4 1 -22 73.79 6.00 -3 -1 22 29.90 3.20 3 -1 -22 22.80 2.70 3 -1 -22 28.20 2.30 -3 -1 22 29.90 2.70 -3 1 22 25.50 2.50 3 1 -22 23.50 2.60 -3 1 22 23.20 2.90 3 1 -22 24.60 2.40 3 1 -22 29.00 2.30 2 -1 -22 16.80 2.20 -2 -1 22 23.20 2.30 -2 -1 22 23.30 2.80 2 -1 -22 20.50 2.00 2 1 -22 22.70 2.00 -2 1 22 19.60 2.60 -2 1 22 24.80 2.30 2 1 -22 22.80 2.20 2 1 -22 19.50 2.00 2 1 -22 18.50 2.20 -1 -1 22 65.09 5.00 -1 -1 22 65.99 5.80 1 -1 -22 53.59 4.80 -1 1 22 65.69 5.70 -1 1 22 65.69 5.10 1 1 -22 62.29 5.80 1 1 -22 57.19 4.70 1 1 -22 56.79 4.60 0 -1 -22 42.60 3.50 0 -1 -22 42.20 3.80 0 -1 -22 39.70 3.70 0 -1 -22 49.99 4.10 0 -1 22 52.89 4.80 0 -1 22 51.89 4.00 0 1 -22 44.50 3.80 0 1 -22 40.90 3.80 0 1 22 56.19 4.80 0 1 22 55.79 4.20 0 1 -22 43.70 3.50 0 1 -22 50.19 4.20 -1 -1 -22 19.50 2.00 1 -1 22 21.90 2.60 -1 -1 -22 20.50 2.10 1 -1 22 20.60 2.10 -1 1 -22 17.40 1.90 -1 1 -22 17.10 2.10 1 1 22 19.60 2.60 -1 1 -22 16.00 1.70 1 1 22 23.00 2.20 2 -1 22 79.09 6.50 2 -1 22 83.19 6.00 -2 -1 -22 67.69 5.70 -2 -1 -22 65.59 6.00 2 1 22 78.59 6.40 -2 1 -22 75.19 5.70 2 1 22 87.79 6.00 -6 -2 22 58.49 5.00 6 -2 -22 59.29 5.00 -6 -2 22 68.59 4.70 6 2 -22 63.09 4.70 6 2 -22 60.69 4.80 -6 2 22 57.29 4.80 -5 -2 22 403.36 26.20 5 -2 -22 349.96 26.00 -5 -2 22 385.96 25.60 5 2 -22 359.96 25.50 -5 2 22 314.17 25.70 5 2 -22 340.27 25.70 -4 -2 22 286.87 18.40 -4 2 22 228.58 18.40 4 2 -22 253.37 18.20 4 2 -22 247.08 18.50 -3 -2 22 31.90 3.20 3 -2 -22 22.70 2.80 3 -2 -22 28.60 2.30 -3 -2 22 28.50 2.60 3 2 -22 23.60 2.40 3 2 -22 29.40 2.50 3 2 -22 30.00 2.20 3 2 -22 22.00 2.70 -2 -2 22 1.80 1.00 2 -2 -22 0.80 0.70 -2 -2 22 3.20 0.90 2 2 -22 3.50 1.00 2 2 -22 2.40 0.70 2 2 -22 1.60 0.80 -1 -2 22 15.40 1.70 1 -2 -22 12.90 1.60 1 -2 -22 14.60 1.70 -1 -2 22 16.70 2.20 1 2 -22 12.60 1.80 1 2 -22 14.90 1.40 -1 2 22 16.80 1.70 1 2 -22 11.30 1.60 1 2 -22 15.60 1.60 0 -2 -22 441.66 32.30 0 -2 -22 420.26 32.20 0 -2 22 508.35 32.40 0 -2 -22 437.16 32.00 0 2 -22 413.66 32.30 0 2 -22 451.35 32.20 0 2 -22 446.26 32.00 0 2 22 523.65 32.40 1 -2 22 605.64 38.70 1 -2 22 572.34 38.00 -1 -2 -22 531.55 38.00 -1 -2 -22 503.15 37.80 -1 2 -22 481.45 38.10 1 2 22 595.44 37.90 -1 2 -22 488.05 37.80 -1 2 -22 506.25 37.80 -5 -3 22 7.70 1.40 -5 -3 22 9.20 1.20 5 -3 -22 6.70 1.50 5 3 -22 8.70 1.10 5 3 -22 7.30 1.10 -5 3 22 6.70 1.20 -4 -3 22 20.30 2.30 -4 -3 22 20.10 1.90 4 -3 -22 17.50 2.20 4 3 -22 17.70 1.80 4 3 -22 16.40 1.90 -4 3 22 19.00 2.00 3 -3 -22 158.38 13.20 -3 -3 22 188.18 13.60 -3 -3 22 181.28 13.00 3 -3 -22 188.58 12.80 3 3 -22 173.28 12.80 3 3 -22 184.38 13.10 -3 3 22 171.48 13.20 3 3 -22 181.38 12.60 3 3 -22 170.98 13.20 2 -3 -22 546.35 37.30 -2 -3 22 536.95 37.30 2 -3 -22 443.26 37.40 -2 -3 22 603.54 38.10 2 3 -22 524.25 37.10 2 3 -22 538.45 37.10 -2 3 22 491.85 37.50 1 -3 -22 482.25 38.20 -1 -3 22 596.54 38.20 1 -3 -22 568.64 38.20 -1 3 22 496.45 38.30 1 3 -22 562.64 38.50 1 3 -22 581.14 38.00 1 3 -22 561.34 37.90 1 3 -22 462.65 38.20 0 -3 22 24.30 2.50 0 -3 -22 16.20 1.70 0 -3 -22 19.70 2.00 0 -3 22 24.50 2.00 0 3 -22 16.90 1.90 0 3 -22 21.50 1.90 0 3 -22 20.10 2.10 -1 -3 -22 9.40 1.30 1 -3 22 10.50 1.60 1 -3 22 10.90 1.20 -1 3 -22 7.00 1.30 -1 3 -22 10.10 1.10 -1 3 -22 8.40 1.00 -4 -4 22 73.89 5.60 -4 -4 22 80.19 6.10 4 4 -22 62.59 5.60 -4 4 22 80.79 5.90 4 4 -22 74.59 5.50 -3 -4 22 11.30 1.40 -3 -4 22 10.40 1.60 3 4 -22 9.30 1.30 3 4 -22 12.30 1.30 -3 4 22 13.50 1.60 3 4 -22 12.70 1.40 2 -4 -22 20.10 1.70 2 -4 -22 14.20 1.80 -2 -4 22 17.20 1.70 -2 -4 22 17.80 2.10 2 4 -22 16.90 1.50 2 4 -22 13.80 1.70 -2 4 22 17.30 1.90 2 4 -22 16.30 1.80 2 4 -22 17.60 1.60 1 -4 -22 4.10 0.90 -1 -4 22 4.30 0.90 1 -4 -22 3.90 0.80 -1 -4 22 4.90 1.10 1 4 -22 5.40 0.80 -1 4 22 4.90 1.00 1 4 -22 3.50 0.80 1 4 -22 3.70 1.00 1 4 -22 3.80 0.60 5 0 -23 1.00 0.60 5 0 -23 0.70 0.60 4 0 -23 0.60 0.60 4 0 -23 0.60 0.70 -4 0 23 1.00 0.60 3 0 -23 1.20 0.60 -3 0 23 -0.10 0.90 3 0 -23 0.50 0.70 -3 0 23 0.70 0.70 2 0 -23 1.70 0.50 -2 0 23 1.00 0.90 2 0 -23 0.80 0.60 2 0 -23 0.50 0.50 -2 0 23 0.40 0.70 -1 0 23 0.70 0.60 1 0 -23 0.40 0.50 1 0 -23 2.00 0.60 -1 0 23 0.30 0.80 0 0 -23 2.10 1.30 0 0 23 1.70 0.90 0 0 23 1.60 0.70 0 0 -23 0.40 0.40 0 0 -23 1.40 0.60 -5 -1 23 152.58 9.70 5 -1 -23 128.29 10.00 5 1 -23 133.09 9.70 5 1 -23 121.09 9.90 -4 -1 23 340.07 23.30 -4 -1 23 361.56 22.80 4 -1 -23 295.67 23.00 4 1 -23 285.07 22.90 4 1 -23 313.47 22.70 3 -1 -23 279.37 22.90 -3 -1 23 366.86 22.90 3 1 -23 318.87 22.70 3 1 -23 273.47 22.90 -3 1 23 355.66 22.70 -2 -1 23 237.68 16.10 2 -1 -23 182.18 16.10 -2 -1 23 246.68 16.80 2 -1 -23 228.98 17.30 2 1 -23 201.98 15.90 -2 1 23 244.18 16.10 2 1 -23 222.58 15.90 -1 -1 23 6.90 1.20 1 -1 -23 3.80 0.80 1 -1 -23 4.50 0.80 1 -1 -23 5.20 0.70 -1 -1 23 4.70 1.30 1 1 -23 4.10 0.90 1 1 -23 6.90 0.90 1 1 -23 4.50 0.90 1 1 -23 3.70 0.60 0 -1 -23 152.98 11.40 0 -1 -23 134.49 11.30 0 -1 23 175.68 12.20 0 -1 23 187.78 11.60 0 1 -23 161.48 11.60 0 1 -23 148.29 11.30 0 1 -23 142.69 11.30 -4 -2 23 140.19 9.50 -4 -2 23 142.99 10.00 4 -2 -23 119.89 9.70 4 2 -23 114.59 9.50 4 2 -23 127.69 9.40 -3 -2 23 38.90 3.60 3 -2 -23 33.90 3.30 -3 -2 23 41.40 3.20 3 2 -23 35.60 3.00 3 2 -23 37.50 3.20 2 -2 -23 104.29 9.10 -2 -2 23 130.89 9.10 2 -2 -23 127.79 9.00 -2 -2 23 136.99 9.80 2 2 -23 124.39 8.90 2 2 -23 117.89 8.90 -1 -2 23 168.08 10.90 1 -2 -23 155.98 10.80 1 -2 -23 127.19 10.80 1 -2 -23 139.19 10.60 1 2 -23 138.99 10.90 1 2 -23 161.38 11.00 1 2 -23 146.39 10.60 1 2 -23 155.58 10.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 47219 _olex2_submission_special_instructions 'No special instructions were received'