#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 9 _journal_issue 4 _journal_year 2018 _journal_page_first 281 _journal_page_last 286 #=============================================================================== data_e4220a_a _audit_update_record ; 2018-05-29 # Formatted by publCIF ; _audit_creation_method SHELXL-2014/6 _publ_contact_author_name ; 'Mohamed Gaye' ; _publ_contact_author_address ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar S\'en\'egal ; _publ_contact_author_phone '00221338247804' _publ_contact_author_fax '00221338246318' _publ_contact_author_email 'mlgayeastou@yahoo.fr' loop_ _publ_author_name _publ_author_address 'Gueye, Amadou' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; 'Tamboura, Farba Bouyagui' ; D\'epartement de Chimie Facult\'e des Sciences Universit\'e Alioune Diop Bambey, S\'en\'egal ; 'Gruber, Nathalie' ; Laboratoire de Tectonique Mol\'eculaire UMR 7140 Chimie de Mati\`ere Condens\'e Institue Le Bel, 4 rue Blaise Pascal CS 90032 F-67081 Strasbourg France ; 'Planeix, Jean-Marc' ; Laboratoire de Tectonique Mol\'eculaire UMR 7140 Chimie de Mati\`ere Condens\'e Institue Le Bel, 4 rue Blaise Pascal CS 90032 F-67081 Strasbourg France ; 'Gaye, Mohamed' ; D\'epartement de Chimie Facult\'e des Sciences et Techniques Universit\'e Cheikh Anta Diop Dakar, S\'en\'egal ; _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H34 N2 O8 S2 Zn2' _chemical_formula_sum 'C32 H34 N2 O8 S2 Zn2' _chemical_formula_weight 769.47 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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.3176(7) _cell_length_b 9.1247(3) _cell_length_c 21.8274(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3250.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28000 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25. _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_F_000 1584 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.090 _exptl_absorpt_coefficient_mu 1.658 _shelx_estimated_absorpt_T_min 0.839 _shelx_estimated_absorpt_T_max 0.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.831 _exptl_absorpt_correction_T_max 0.867 _exptl_absorpt_process_details sadabs _exptl_absorpt_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28116 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.245 _diffrn_reflns_theta_max 30.146 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.926 _diffrn_measured_fraction_theta_full 0.979 _diffrn_reflns_Laue_measured_fraction_max 0.926 _diffrn_reflns_Laue_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.926 _diffrn_reflns_point_group_measured_fraction_full 0.979 _reflns_number_total 4457 _reflns_number_gt 3516 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ? _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^)+(0.0275P)^2^+1.7715P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4457 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 Zn1 Zn 0.55379(2) 0.61524(2) 0.46731(2) 0.01708(7) Uani 1 1 d . . . . . O1 O 0.57702(8) 0.72803(12) 0.39246(5) 0.0255(3) Uani 1 1 d . . . . . C1 C 0.61881(10) 0.68111(16) 0.34601(7) 0.0191(3) Uani 1 1 d . . . . . C2 C 0.60806(11) 0.75175(17) 0.28792(7) 0.0228(4) Uani 1 1 d . . . . . C3 C 0.65033(11) 0.70896(19) 0.23695(8) 0.0284(4) Uani 1 1 d . . . . . H3 H 0.6419 0.7587 0.1992 0.034 Uiso 1 1 calc R U . . . C4 C 0.70605(12) 0.5921(2) 0.23993(9) 0.0365(5) Uani 1 1 d . . . . . H4 H 0.7350 0.5623 0.2043 0.044 Uiso 1 1 calc R U . . . C5 C 0.71850(12) 0.5218(2) 0.29400(8) 0.0356(5) Uani 1 1 d . . . . . H5 H 0.7567 0.4434 0.2958 0.043 Uiso 1 1 calc R U . . . C6 C 0.67565(10) 0.56309(18) 0.34782(8) 0.0238(4) Uani 1 1 d . . . . . O2 O 0.55230(8) 0.86402(14) 0.28902(6) 0.0362(3) Uani 1 1 d . . . . . C7 C 0.53771(19) 0.9382(3) 0.23292(10) 0.0731(9) Uani 1 1 d . . . . . H7A H 0.5894 0.9785 0.2174 0.110 Uiso 1 1 calc R U . . . H7B H 0.4986 1.0180 0.2397 0.110 Uiso 1 1 calc R U . . . H7C H 0.5151 0.8692 0.2029 0.110 Uiso 1 1 calc R U . . . C8 C 0.69346(10) 0.47983(18) 0.40192(8) 0.0244(4) Uani 1 1 d . . . . . H8 H 0.7353 0.4079 0.3987 0.029 Uiso 1 1 calc R U . . . N1 N 0.65814(8) 0.49314(14) 0.45465(6) 0.0195(3) Uani 1 1 d . . . . . C9 C 0.68020(10) 0.40541(16) 0.50570(8) 0.0189(3) Uani 1 1 d . . . . . C10 C 0.62172(10) 0.40535(16) 0.55348(8) 0.0185(3) Uani 1 1 d . . . . . C11 C 0.63677(11) 0.32061(17) 0.60522(8) 0.0232(4) Uani 1 1 d . . . . . H11 H 0.5977 0.3182 0.6375 0.028 Uiso 1 1 calc R U . . . C12 C 0.70817(11) 0.23994(18) 0.61000(8) 0.0270(4) Uani 1 1 d . . . . . H12 H 0.7175 0.1816 0.6454 0.032 Uiso 1 1 calc R U . . . C13 C 0.76616(11) 0.24328(18) 0.56376(8) 0.0278(4) Uani 1 1 d . . . . . H13 H 0.8155 0.1887 0.5678 0.033 Uiso 1 1 calc R U . . . C14 C 0.75237(11) 0.32573(18) 0.51188(8) 0.0245(4) Uani 1 1 d . . . . . H14 H 0.7923 0.3281 0.4802 0.029 Uiso 1 1 calc R U . . . O3 O 0.55361(6) 0.48655(12) 0.54770(5) 0.0193(2) Uani 1 1 d . . . . . O4 O 0.52393(8) 0.80177(12) 0.51179(5) 0.0252(3) Uani 1 1 d . . . . . S1 S 0.50278(3) 0.82363(4) 0.57923(2) 0.02714(12) Uani 1 1 d . . . . . C15 C 0.55951(11) 0.9818(2) 0.60049(9) 0.0323(4) Uani 1 1 d . . . . . H15A H 0.6180 0.9576 0.6019 0.048 Uiso 1 1 calc R U . . . H15B H 0.5415 1.0153 0.6410 0.048 Uiso 1 1 calc R U . . . H15C H 0.5503 1.0596 0.5703 0.048 Uiso 1 1 calc R U . . . C16 C 0.40354(12) 0.9059(2) 0.57902(11) 0.0416(5) Uani 1 1 d . . . . . H16A H 0.4052 0.9972 0.5554 0.062 Uiso 1 1 calc R U . . . H16B H 0.3868 0.9271 0.6212 0.062 Uiso 1 1 calc R U . . . H16C H 0.3641 0.8384 0.5603 0.062 Uiso 1 1 calc R U . . . 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 Zn1 0.01773(12) 0.01486(10) 0.01864(12) 0.00020(7) 0.00241(7) 0.00230(7) O1 0.0338(7) 0.0214(6) 0.0212(6) 0.0025(5) 0.0101(5) 0.0075(5) C1 0.0189(8) 0.0177(7) 0.0206(9) -0.0023(6) 0.0039(7) -0.0038(6) C2 0.0251(9) 0.0202(8) 0.0230(9) -0.0011(7) 0.0019(7) -0.0017(7) C3 0.0349(11) 0.0301(9) 0.0202(9) -0.0004(7) 0.0046(8) -0.0020(8) C4 0.0428(12) 0.0413(11) 0.0254(10) -0.0036(8) 0.0142(9) 0.0072(9) C5 0.0383(11) 0.0359(10) 0.0327(11) -0.0007(8) 0.0131(9) 0.0136(9) C6 0.0225(9) 0.0249(8) 0.0239(9) -0.0008(7) 0.0049(7) 0.0012(7) O2 0.0490(9) 0.0362(7) 0.0234(7) 0.0084(6) 0.0069(6) 0.0193(6) C7 0.108(2) 0.0808(18) 0.0307(13) 0.0174(13) 0.0080(14) 0.0607(18) C8 0.0200(9) 0.0224(8) 0.0308(10) -0.0012(7) 0.0038(8) 0.0051(7) N1 0.0183(7) 0.0172(6) 0.0229(8) -0.0005(5) 0.0009(6) 0.0003(5) C9 0.0200(9) 0.0145(7) 0.0224(9) -0.0019(6) -0.0037(7) -0.0011(6) C10 0.0195(9) 0.0133(7) 0.0228(9) -0.0026(6) -0.0047(7) 0.0000(6) C11 0.0256(9) 0.0213(8) 0.0227(9) 0.0009(7) -0.0039(7) -0.0025(7) C12 0.0312(10) 0.0199(8) 0.0298(10) 0.0030(7) -0.0123(8) -0.0007(7) C13 0.0225(9) 0.0197(8) 0.0411(11) -0.0020(8) -0.0095(9) 0.0040(7) C14 0.0209(9) 0.0217(8) 0.0308(10) -0.0026(7) -0.0007(8) 0.0015(7) O3 0.0192(6) 0.0172(5) 0.0214(6) 0.0005(5) -0.0003(5) 0.0025(4) O4 0.0383(7) 0.0175(6) 0.0197(6) -0.0029(5) 0.0022(5) 0.0046(5) S1 0.0403(3) 0.0187(2) 0.0224(2) -0.00116(16) 0.00638(19) 0.00400(19) C15 0.0339(11) 0.0319(10) 0.0311(11) -0.0118(8) -0.0046(8) 0.0039(8) C16 0.0296(12) 0.0370(11) 0.0583(14) -0.0174(10) 0.0123(10) -0.0031(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.9679(11) . ? Zn1 O3 2.0104(11) 5_666 ? Zn1 O4 2.0192(11) . ? Zn1 N1 2.0534(13) . ? Zn1 O3 2.1112(11) . ? Zn1 Zn1 3.0887(4) 5_666 ? O1 C1 1.2948(19) . ? C1 C6 1.422(2) . ? C1 C2 1.433(2) . ? C2 C3 1.366(2) . ? C2 O2 1.370(2) . ? C3 C4 1.403(3) . ? C3 H3 0.9500 . ? C4 C5 1.359(3) . ? C4 H4 0.9500 . ? C5 C6 1.418(2) . ? C5 H5 0.9500 . ? C6 C8 1.434(2) . ? O2 C7 1.419(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N1 1.293(2) . ? C8 H8 0.9500 . ? N1 C9 1.418(2) . ? C9 C14 1.391(2) . ? C9 C10 1.414(2) . ? C10 O3 1.3417(19) . ? C10 C11 1.391(2) . ? C11 C12 1.382(2) . ? C11 H11 0.9500 . ? C12 C13 1.384(3) . ? C12 H12 0.9500 . ? C13 C14 1.378(2) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? O3 Zn1 2.0103(11) 5_666 ? O4 S1 1.5250(12) . ? S1 C15 1.7760(19) . ? S1 C16 1.785(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 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 O1 Zn1 O3 105.92(5) . 5_666 ? O1 Zn1 O4 90.27(5) . . ? O3 Zn1 O4 104.91(5) 5_666 . ? O1 Zn1 N1 90.70(5) . . ? O3 Zn1 N1 116.76(5) 5_666 . ? O4 Zn1 N1 136.24(5) . . ? O1 Zn1 O3 168.87(5) . . ? O3 Zn1 O3 82.95(5) 5_666 . ? O4 Zn1 O3 93.95(4) . . ? N1 Zn1 O3 79.13(5) . . ? O1 Zn1 Zn1 148.12(4) . 5_666 ? O3 Zn1 Zn1 42.71(3) 5_666 5_666 ? O4 Zn1 Zn1 102.40(4) . 5_666 ? N1 Zn1 Zn1 99.44(4) . 5_666 ? O3 Zn1 Zn1 40.24(3) . 5_666 ? C1 O1 Zn1 125.36(10) . . ? O1 C1 C6 124.91(15) . . ? O1 C1 C2 118.66(14) . . ? C6 C1 C2 116.43(14) . . ? C3 C2 O2 124.29(15) . . ? C3 C2 C1 122.02(15) . . ? O2 C2 C1 113.70(14) . . ? C2 C3 C4 120.45(16) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.74(17) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.38(17) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C5 C6 C1 119.98(16) . . ? C5 C6 C8 116.21(15) . . ? C1 C6 C8 123.81(15) . . ? C2 O2 C7 116.91(15) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C6 126.36(15) . . ? N1 C8 H8 116.8 . . ? C6 C8 H8 116.8 . . ? C8 N1 C9 122.21(14) . . ? C8 N1 Zn1 122.72(11) . . ? C9 N1 Zn1 114.26(10) . . ? C14 C9 C10 119.99(15) . . ? C14 C9 N1 125.89(15) . . ? C10 C9 N1 114.11(14) . . ? O3 C10 C11 121.99(15) . . ? O3 C10 C9 119.32(14) . . ? C11 C10 C9 118.70(15) . . ? C12 C11 C10 120.42(16) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.65(16) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C14 C13 C12 119.97(16) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C9 120.23(17) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? C10 O3 Zn1 118.84(9) . 5_666 ? C10 O3 Zn1 112.59(10) . . ? Zn1 O3 Zn1 97.05(5) 5_666 . ? S1 O4 Zn1 128.97(7) . . ? O4 S1 C15 103.92(8) . . ? O4 S1 C16 104.94(9) . . ? C15 S1 C16 97.59(9) . . ? S1 C15 H15A 109.5 . . ? S1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? S1 C16 H16A 109.5 . . ? S1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? _refine_diff_density_max 0.352 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.072 _shelxl_version_number 2014/6 _shelx_res_file ; TITL e4220a_a.res in Pbca CELL 0.71073 16.3176 9.1247 21.8274 90.000 90.000 90.000 ZERR 4.000 0.0007 0.0003 0.0010 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H N O Zn S UNIT 128 136 8 32 8 8 L.S. 10 ACTA BOND $H FMAP 2 PLAN 20 SIZE 0.09 0.09 0.11 TEMP -100.000 WGHT 0.027500 1.771500 FVAR 0.30212 ZN1 5 0.553794 0.615236 0.467315 11.00000 0.01773 0.01486 = 0.01864 0.00020 0.00241 0.00230 O1 4 0.577023 0.728034 0.392462 11.00000 0.03375 0.02140 = 0.02124 0.00246 0.01008 0.00747 C1 1 0.618814 0.681109 0.346010 11.00000 0.01887 0.01774 = 0.02064 -0.00226 0.00390 -0.00378 C2 1 0.608057 0.751748 0.287915 11.00000 0.02509 0.02024 = 0.02295 -0.00113 0.00186 -0.00172 C3 1 0.650327 0.708961 0.236949 11.00000 0.03487 0.03010 = 0.02017 -0.00041 0.00463 -0.00198 AFIX 43 H3 2 0.641924 0.758663 0.199224 11.00000 -1.20000 AFIX 0 C4 1 0.706050 0.592148 0.239932 11.00000 0.04279 0.04132 = 0.02541 -0.00358 0.01419 0.00719 AFIX 43 H4 2 0.734976 0.562303 0.204281 11.00000 -1.20000 AFIX 0 C5 1 0.718501 0.521843 0.294003 11.00000 0.03828 0.03585 = 0.03271 -0.00067 0.01310 0.01364 AFIX 43 H5 2 0.756712 0.443410 0.295791 11.00000 -1.20000 AFIX 0 C6 1 0.675652 0.563089 0.347821 11.00000 0.02248 0.02489 = 0.02390 -0.00081 0.00492 0.00122 O2 4 0.552299 0.864018 0.289023 11.00000 0.04903 0.03618 = 0.02344 0.00844 0.00687 0.01932 C7 1 0.537708 0.938161 0.232923 11.00000 0.10772 0.08081 = 0.03071 0.01743 0.00799 0.06067 AFIX 137 H7A 2 0.589350 0.978456 0.217380 11.00000 -1.50000 H7B 2 0.498595 1.018029 0.239711 11.00000 -1.50000 H7C 2 0.515103 0.869200 0.202938 11.00000 -1.50000 AFIX 0 C8 1 0.693465 0.479834 0.401921 11.00000 0.01997 0.02241 = 0.03078 -0.00120 0.00382 0.00515 AFIX 43 H8 2 0.735315 0.407866 0.398708 11.00000 -1.20000 AFIX 0 N1 3 0.658136 0.493141 0.454646 11.00000 0.01826 0.01724 = 0.02290 -0.00045 0.00087 0.00027 C9 1 0.680203 0.405412 0.505696 11.00000 0.01999 0.01448 = 0.02238 -0.00192 -0.00373 -0.00105 C10 1 0.621724 0.405351 0.553475 11.00000 0.01950 0.01327 = 0.02279 -0.00263 -0.00465 -0.00003 C11 1 0.636773 0.320609 0.605216 11.00000 0.02564 0.02127 = 0.02266 0.00089 -0.00386 -0.00246 AFIX 43 H11 2 0.597728 0.318151 0.637483 11.00000 -1.20000 AFIX 0 C12 1 0.708168 0.239944 0.609997 11.00000 0.03117 0.01985 = 0.02983 0.00304 -0.01231 -0.00073 AFIX 43 H12 2 0.717523 0.181636 0.645369 11.00000 -1.20000 AFIX 0 C13 1 0.766164 0.243275 0.563762 11.00000 0.02251 0.01965 = 0.04113 -0.00202 -0.00946 0.00402 AFIX 43 H13 2 0.815466 0.188743 0.567785 11.00000 -1.20000 AFIX 0 C14 1 0.752372 0.325732 0.511880 11.00000 0.02088 0.02165 = 0.03084 -0.00264 -0.00069 0.00153 AFIX 43 H14 2 0.792310 0.328147 0.480229 11.00000 -1.20000 AFIX 0 O3 4 0.553608 0.486551 0.547697 11.00000 0.01917 0.01716 = 0.02143 0.00052 -0.00033 0.00250 O4 4 0.523927 0.801772 0.511793 11.00000 0.03833 0.01746 = 0.01969 -0.00294 0.00216 0.00464 S1 6 0.502784 0.823633 0.579231 11.00000 0.04030 0.01866 = 0.02244 -0.00116 0.00638 0.00400 C15 1 0.559509 0.981763 0.600489 11.00000 0.03391 0.03192 = 0.03115 -0.01177 -0.00464 0.00392 AFIX 137 H15A 2 0.618000 0.957628 0.601919 11.00000 -1.50000 H15B 2 0.541515 1.015337 0.640960 11.00000 -1.50000 H15C 2 0.550314 1.059584 0.570319 11.00000 -1.50000 AFIX 0 C16 1 0.403542 0.905862 0.579017 11.00000 0.02956 0.03695 = 0.05828 -0.01740 0.01234 -0.00312 AFIX 137 H16A 2 0.405234 0.997201 0.555432 11.00000 -1.50000 H16B 2 0.386820 0.927108 0.621215 11.00000 -1.50000 H16C 2 0.364079 0.838430 0.560287 11.00000 -1.50000 AFIX 0 HKLF 4 REM e4220a_a.res in Pbca REM R1 = 0.0307 for 3516 Fo > 4sig(Fo) and 0.0466 for all 4457 data REM 211 parameters refined using 0 restraints END WGHT 0.0282 1.4820 REM Highest difference peak 0.352, deepest hole -0.354, 1-sigma level 0.072 Q1 1 0.6894 0.6736 0.2484 11.00000 0.05 0.35 Q2 1 0.6751 0.6225 0.3498 11.00000 0.05 0.31 Q3 1 0.6363 0.3580 0.5818 11.00000 0.05 0.31 Q4 1 0.6152 0.3276 0.6223 11.00000 0.05 0.30 Q5 1 0.6424 0.5580 0.4592 11.00000 0.05 0.30 Q6 1 0.5125 0.7363 0.5944 11.00000 0.05 0.30 Q7 1 0.6853 0.5379 0.3721 11.00000 0.05 0.29 Q8 1 0.4452 0.8792 0.5859 11.00000 0.05 0.28 Q9 1 0.5933 0.4469 0.5501 11.00000 0.05 0.28 Q10 1 0.6831 0.5465 0.3230 11.00000 0.05 0.28 Q11 1 0.7624 0.3239 0.4929 11.00000 0.05 0.27 Q12 1 0.8023 0.4412 0.3100 11.00000 0.05 0.27 Q13 1 0.6597 0.4773 0.4291 11.00000 0.05 0.26 Q14 1 0.6727 0.4354 0.4793 11.00000 0.05 0.26 Q15 1 0.5362 0.8287 0.5305 11.00000 0.05 0.24 Q16 1 0.6044 0.7013 0.3120 11.00000 0.05 0.24 Q17 1 0.5870 0.7982 0.3901 11.00000 0.05 0.24 Q18 1 0.5064 0.7941 0.5357 11.00000 0.05 0.24 Q19 1 0.5504 0.8843 0.4991 11.00000 0.05 0.24 Q20 1 0.5283 0.4788 0.5561 11.00000 0.05 0.23 ; _shelx_res_checksum 67331 _shelx_hkl_file ; 2 0 0 5432.96 259.77 2 0 0 5280.37 259.07 -2 0 0 5596.44 259.97 -2 0 0 5653.63 259.17 3 0 0 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2 -5 0 26.10 2.90 -3 5 0 -1.90 0.90 -3 5 0 -1.90 0.90 3 5 0 0.20 0.50 3 5 0 -0.60 0.40 3 -5 0 -2.20 1.30 -3 -5 0 -0.10 0.50 3 -5 0 -0.40 0.90 -3 -5 0 0.80 0.40 4 5 0 493.65 23.90 4 5 0 504.25 24.00 -4 5 0 528.75 25.00 -4 5 0 521.35 24.80 -4 -5 0 505.65 23.90 4 -5 0 499.15 24.70 4 -5 0 494.45 25.50 -4 -5 0 491.25 24.00 -4 -5 0 507.75 24.10 -5 5 0 0.20 1.20 -5 5 0 -0.10 1.10 5 5 0 -0.30 0.50 5 5 0 0.00 0.50 5 -5 0 -0.10 1.80 -5 -5 0 -0.70 0.60 -5 -5 0 0.30 0.50 5 -5 0 0.40 1.00 6 5 0 707.73 33.70 -6 5 0 735.83 34.70 6 5 0 722.83 33.60 -6 5 0 664.33 34.80 -6 -5 0 728.63 33.90 6 -5 0 683.73 34.60 6 -5 0 679.73 35.40 -6 -5 0 730.73 33.70 -7 5 0 -0.90 1.40 7 5 0 -0.50 0.60 7 5 0 -0.10 0.70 7 -5 0 0.20 1.20 7 -5 0 -0.90 2.10 -7 -5 0 -0.20 0.80 -7 -5 0 0.10 0.60 8 5 0 241.48 11.30 -8 5 0 210.28 12.20 8 5 0 219.08 11.20 -8 -5 0 228.88 11.30 8 -5 0 222.68 13.20 8 -5 0 228.88 12.30 9 5 0 -0.80 0.80 9 5 0 -0.10 0.90 -9 5 0 -2.80 1.40 -9 -5 0 0.40 0.80 9 -5 0 -0.90 2.40 9 -5 0 -0.80 1.50 10 5 0 5.50 1.30 10 5 0 8.20 1.50 -10 5 0 8.70 2.30 10 -5 0 4.60 2.80 -10 -5 0 6.60 1.30 10 -5 0 6.10 2.20 11 5 0 0.10 1.10 11 5 0 0.40 1.10 -11 5 0 -1.40 1.60 -11 -5 0 -0.70 0.90 11 -5 0 -1.60 1.70 11 -5 0 -1.20 2.70 12 5 0 33.60 3.00 12 5 0 32.20 2.90 12 5 0 29.60 2.80 12 -5 0 26.40 5.00 -12 -5 0 27.10 2.70 13 5 0 -1.50 1.20 13 5 0 0.60 1.40 13 -5 0 -1.30 3.20 -13 -5 0 -0.20 1.20 13 -5 0 2.40 2.70 14 5 0 337.37 17.00 14 5 0 323.17 17.10 14 -5 0 321.37 19.50 14 -5 0 331.47 19.00 15 5 0 -0.30 1.70 15 -5 0 -1.20 3.20 16 5 0 13.90 2.70 16 -5 0 18.60 4.80 17 5 0 2.20 2.10 17 -5 0 5.20 3.90 0 6 0 6.30 1.10 0 6 0 7.50 1.10 0 -6 0 7.40 1.70 0 -6 0 4.30 1.00 -1 6 0 0.20 0.80 -1 6 0 0.80 0.90 1 6 0 0.20 0.60 1 6 0 0.20 0.70 -1 -6 0 0.40 0.60 1 -6 0 1.40 1.40 -1 -6 0 0.30 1.10 1 -6 0 0.10 0.80 2 6 0 221.98 10.70 -2 6 0 218.78 11.30 -2 6 0 217.18 11.30 2 6 0 225.98 10.80 -2 -6 0 226.18 11.40 2 -6 0 210.78 12.00 2 -6 0 197.68 11.10 -2 -6 0 228.68 10.70 3 6 0 0.60 0.50 -3 6 0 -1.30 1.00 3 6 0 0.50 0.60 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628.94 31.20 -6 -7 0 613.14 30.10 6 -7 0 660.53 32.50 -7 7 0 -1.40 1.70 -7 7 0 -0.80 1.60 -7 -7 0 1.30 0.90 7 -7 0 0.40 1.60 7 -7 0 1.70 2.30 -8 7 0 94.79 6.40 -8 7 0 85.79 6.50 8 -7 0 92.89 7.60 8 -7 0 83.09 6.20 -9 7 0 -0.50 1.80 -9 7 0 1.20 2.00 9 -7 0 -2.60 1.40 9 -7 0 2.80 2.80 -10 7 0 146.49 9.40 10 -7 0 119.49 9.60 11 -7 0 0.40 3.00 12 -7 0 625.84 33.60 13 -7 0 0.10 3.20 13 -7 0 -3.30 3.50 14 -7 0 410.06 23.80 15 -7 0 -1.20 3.60 16 -7 0 129.09 12.10 17 -7 0 -2.90 4.10 0 8 0 556.14 26.60 0 8 0 533.05 26.50 0 -8 0 543.25 27.50 0 -8 0 563.14 26.50 1 8 0 -0.30 0.90 -1 8 0 -0.30 1.00 1 8 0 0.30 0.80 -1 8 0 0.10 1.00 -1 -8 0 0.20 0.80 1 -8 0 1.60 1.90 1 -8 0 0.40 1.00 -1 -8 0 -1.00 1.50 2 8 0 93.69 5.00 -2 8 0 91.29 5.60 -2 8 0 95.09 5.70 2 -8 0 93.99 6.80 2 -8 0 95.29 5.60 -2 -8 0 89.89 6.00 -2 -8 0 100.29 4.90 -3 8 0 1.00 1.30 -3 8 0 0.60 1.30 3 -8 0 0.10 1.20 3 -8 0 0.30 2.10 -3 -8 0 0.40 0.50 -3 -8 0 1.60 1.40 -4 8 0 22.70 2.80 -4 8 0 20.80 2.70 -4 -8 0 24.50 1.80 4 -8 0 19.60 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6.10 9 -9 0 -0.30 3.50 10 -9 0 5.20 3.80 11 -9 0 0.60 3.70 12 -9 0 82.69 8.80 13 -9 0 -2.00 3.90 14 -9 0 3.00 3.90 15 -9 0 4.70 4.30 16 -9 0 59.09 8.90 0 -10 0 675.43 33.80 1 -10 0 0.10 2.30 -1 -10 0 -0.80 2.00 -2 -10 0 220.88 11.70 2 -10 0 189.78 12.20 3 -10 0 0.50 2.60 4 -10 0 2.60 2.80 5 -10 0 2.70 3.00 6 -10 0 11.60 3.90 7 -10 0 -3.80 2.80 8 -10 0 92.59 9.00 9 -10 0 -1.60 3.50 10 -10 0 113.29 10.50 11 -10 0 1.90 3.70 12 -10 0 48.30 7.10 13 -10 0 1.90 4.40 14 -10 0 -0.20 4.50 0 -11 0 -0.60 2.30 1 -11 0 -1.20 2.40 2 -11 0 59.39 6.10 3 -11 0 -0.70 2.90 4 -11 0 421.46 23.00 5 -11 0 -1.00 3.20 6 -11 0 247.18 15.50 7 -11 0 -3.00 3.10 8 -11 0 61.49 7.40 9 -11 0 -3.50 3.60 10 -11 0 0.50 3.80 11 -11 0 -0.80 4.00 3 -12 0 5.60 3.10 4 -12 0 -1.00 3.10 5 -12 0 1.40 3.40 6 -12 0 66.29 7.40 7 -12 0 -1.60 3.60 8 -12 0 280.67 17.50 16 0 1 4.60 2.90 15 0 1 1.20 2.10 -15 0 -1 -0.70 1.70 15 0 1 -1.10 2.20 14 0 1 2.10 1.80 14 0 1 2.10 2.50 -14 0 -1 -0.80 1.80 14 0 1 -0.10 1.80 -13 0 -1 -0.30 1.60 13 0 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-30 25.30 7.30 3 -2 -30 9.80 6.80 4 -2 -30 33.80 8.20 0 -3 -30 3.00 5.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 91940 loop_ _publcif_info_datablock.id _publcif_info_datablock.publ_exptl _publcif_info_datablock.publ_geom _publcif_info_datablock.structure '{15d5521e-3311-48a7-8237-d1267630e480}' y y y loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? _publcif_info_exptl_table_max_cols 4 _publcif_info_exptl_table_use_headnotes n loop_ _publcif_info_tables.block_id _publcif_info_tables.reference_item "{15d5521e-3311-48a7-8237-d1267630e480}" "_publcif_info_datablock.publ_exptl" loop_ _publcif_info_cif.paper_type EE _publcif_funding_html ; ;