data_shelx _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H16 N2 O2' _chemical_formula_sum 'C19 H16 N2 O2' _chemical_formula_weight 304.34 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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _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' _cell_length_a 6.1227(4) _cell_length_b 12.5222(3) _cell_length_c 20.3948(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1563.66(12) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3664 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 23.41 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.293 _exptl_crystal_F_000 640 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.130 _exptl_absorpt_coefficient_mu 0.085 _shelx_estimated_absorpt_T_min 0.985 _shelx_estimated_absorpt_T_max 0.989 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.9848 _exptl_absorpt_correction_T_max 0.9890 _exptl_absorpt_process_details 'SADABS; Bruker, 2012' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX II QUAZAR three-circle diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 16168 _diffrn_reflns_av_unetI/netI 0.0673 _diffrn_reflns_av_R_equivalents 0.0535 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.576 _diffrn_reflns_theta_max 26.294 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 3162 _reflns_number_gt 1782 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.706 _reflns_Friedel_fraction_max 0.988 _reflns_Friedel_fraction_full 0.998 _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 'APEX2 (Bruker, 2012)' _computing_cell_refinement 'SAINT (Bruker, 2012)' _computing_data_reduction 'SAINT' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2015a)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2015b)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'WinGX publication routines (Farrugia, 2012) and PLATON (Spek, 2009)' _refine_special_details ; The NH and OH hydrogens were located in a difference Fourier map and refined isotropically. The aromatic and methyl hydrogens were positioned geometrically at distances of 0.93 and 0.96 \%A, respectively, and refined using a riding model by applying the contraints of U~iso~ = k \\times U~eq~(C), where k = 1.2 for aromatic and k = 1.5 for methyl hydrogen atoms. ; _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^)+(0.0463P)^2^+0.0818P] 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_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 554 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.8(9) _chemical_absolute_configuration ? _refine_ls_number_reflns 3162 _refine_ls_number_parameters 217 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1243 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6063(5) 0.79672(19) 0.64698(12) 0.0607(7) Uani 1 1 d . . . . . O2 O 0.1161(5) 1.1759(2) 0.79030(16) 0.0869(10) Uani 1 1 d D . . . . N1 N 0.3255(5) 0.6598(2) 0.58999(15) 0.0565(8) Uani 1 1 d . . . . . N2 N 0.2567(6) 0.7501(3) 0.62343(17) 0.0571(9) Uani 1 1 d D . . . . C1 C 0.3223(6) 0.9069(3) 0.68863(15) 0.0438(9) Uani 1 1 d . . . . . C2 C 0.1133(6) 0.9490(3) 0.68074(17) 0.0532(10) Uani 1 1 d . . . . . H2 H 0.016369 0.916333 0.651924 0.064 Uiso 1 1 calc R U . . . C3 C 0.0480(6) 1.0382(3) 0.71488(18) 0.0597(10) Uani 1 1 d . . . . . H3 H -0.091192 1.065846 0.708263 0.072 Uiso 1 1 calc R U . . . C4 C 0.1871(7) 1.0870(3) 0.75885(18) 0.0559(11) Uani 1 1 d . . . . . C5 C 0.3959(6) 1.0452(3) 0.76827(16) 0.0527(10) Uani 1 1 d . . . . . H5 H 0.490571 1.076513 0.798307 0.063 Uiso 1 1 calc R U . . . C6 C 0.4606(6) 0.9576(3) 0.73294(15) 0.0470(9) Uani 1 1 d . . . . . H6 H 0.601321 0.931226 0.738766 0.056 Uiso 1 1 calc R U . . . C7 C 0.4074(7) 0.8138(3) 0.65256(16) 0.0475(9) Uani 1 1 d . . . . . C8 C 0.1829(6) 0.6168(3) 0.55102(16) 0.0465(9) Uani 1 1 d . . . . . C9 C -0.0402(6) 0.6624(3) 0.53920(19) 0.0799(13) Uani 1 1 d . . . . . H9A H -0.034213 0.738799 0.542571 0.120 Uiso 1 1 calc R U . . . H9B H -0.140035 0.634861 0.571321 0.120 Uiso 1 1 calc R U . . . H9C H -0.089133 0.642706 0.496143 0.120 Uiso 1 1 calc R U . . . C10 C 0.2561(5) 0.5205(3) 0.51569(16) 0.0437(9) Uani 1 1 d . . . . . C11 C 0.4613(5) 0.4727(3) 0.53068(17) 0.0558(10) Uani 1 1 d . . . . . H11 H 0.546811 0.501198 0.564070 0.067 Uiso 1 1 calc R U . . . C12 C 0.5343(6) 0.3859(3) 0.49685(18) 0.0571(10) Uani 1 1 d . . . . . H12 H 0.669307 0.356723 0.507611 0.069 Uiso 1 1 calc R U . . . C13 C 0.4108(6) 0.3389(3) 0.44589(17) 0.0496(10) Uani 1 1 d . . . . . C14 C 0.4818(7) 0.2493(3) 0.4096(2) 0.0613(11) Uani 1 1 d . . . . . H14 H 0.617633 0.219218 0.418253 0.074 Uiso 1 1 calc R U . . . C15 C 0.3523(8) 0.2066(3) 0.3617(2) 0.0721(13) Uani 1 1 d . . . . . H15 H 0.400239 0.147573 0.338075 0.087 Uiso 1 1 calc R U . . . C16 C 0.1484(8) 0.2512(3) 0.3483(2) 0.0715(12) Uani 1 1 d . . . . . H16 H 0.061327 0.221400 0.315745 0.086 Uiso 1 1 calc R U . . . C17 C 0.0753(6) 0.3374(3) 0.38212(17) 0.0585(10) Uani 1 1 d . . . . . H17 H -0.061230 0.365852 0.372474 0.070 Uiso 1 1 calc R U . . . C18 C 0.2039(6) 0.3842(3) 0.43166(15) 0.0451(9) Uani 1 1 d . . . . . C19 C 0.1325(6) 0.4747(2) 0.46697(15) 0.0462(9) Uani 1 1 d . . . . . H19 H -0.002692 0.504358 0.456907 0.055 Uiso 1 1 calc R U . . . H2A H 0.116(4) 0.753(4) 0.630(2) 0.13(2) Uiso 1 1 d D . . . . H2B H 0.228(7) 1.219(4) 0.813(2) 0.14(2) Uiso 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0555(18) 0.0487(14) 0.0778(19) -0.0052(13) -0.0066(15) 0.0039(14) O2 0.062(2) 0.089(2) 0.109(2) -0.050(2) 0.0138(18) -0.0025(17) N1 0.064(2) 0.0482(19) 0.0578(19) -0.0105(17) 0.0017(18) -0.0035(17) N2 0.056(2) 0.0473(19) 0.068(2) -0.0163(17) 0.0015(18) -0.0075(17) C1 0.047(2) 0.037(2) 0.047(2) 0.0020(17) -0.0037(18) -0.0052(19) C2 0.047(2) 0.052(2) 0.061(2) -0.007(2) -0.0101(19) -0.008(2) C3 0.044(2) 0.060(3) 0.075(3) -0.007(2) -0.002(2) 0.000(2) C4 0.050(3) 0.061(3) 0.056(2) -0.011(2) 0.005(2) -0.012(2) C5 0.053(3) 0.059(3) 0.046(2) -0.0075(19) -0.0048(19) -0.013(2) C6 0.044(2) 0.046(2) 0.050(2) 0.0029(19) -0.0045(18) -0.008(2) C7 0.057(3) 0.041(2) 0.045(2) 0.0049(17) -0.003(2) -0.005(2) C8 0.051(2) 0.047(2) 0.041(2) 0.0013(18) -0.0005(18) -0.007(2) C9 0.079(3) 0.081(3) 0.080(3) -0.029(3) -0.020(2) 0.018(2) C10 0.051(2) 0.039(2) 0.041(2) 0.0043(18) -0.0023(17) -0.0040(18) C11 0.057(2) 0.050(2) 0.060(2) -0.002(2) -0.016(2) -0.004(2) C12 0.053(2) 0.046(2) 0.072(3) 0.004(2) -0.008(2) 0.001(2) C13 0.054(3) 0.043(2) 0.052(2) 0.0029(18) 0.001(2) -0.006(2) C14 0.067(3) 0.044(2) 0.073(3) -0.001(2) 0.015(3) 0.003(2) C15 0.097(4) 0.051(2) 0.068(3) -0.012(2) 0.016(3) -0.001(3) C16 0.094(4) 0.062(3) 0.059(3) -0.013(2) -0.005(3) -0.008(3) C17 0.066(3) 0.058(2) 0.051(2) -0.006(2) -0.007(2) -0.002(2) C18 0.053(2) 0.040(2) 0.042(2) 0.0023(18) 0.0021(18) -0.0055(19) C19 0.052(2) 0.043(2) 0.043(2) 0.0028(18) -0.0032(19) -0.0005(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C7 1.241(4) . ? O2 C4 1.357(5) . ? O2 H2B 0.99(3) . ? N1 C8 1.298(4) . ? N1 N2 1.386(4) . ? N2 C7 1.357(5) . ? N2 H2A 0.87(2) . ? C1 C6 1.392(4) . ? C1 C2 1.394(4) . ? C1 C7 1.474(5) . ? C2 C3 1.375(5) . ? C2 H2 0.9300 . ? C3 C4 1.379(5) . ? C3 H3 0.9300 . ? C4 C5 1.395(5) . ? C5 C6 1.371(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C8 C10 1.474(4) . ? C8 C9 1.500(5) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C19 1.374(4) . ? C10 C11 1.425(4) . ? C11 C12 1.363(5) . ? C11 H11 0.9300 . ? C12 C13 1.414(4) . ? C12 H12 0.9300 . ? C13 C14 1.413(5) . ? C13 C18 1.418(4) . ? C14 C15 1.366(5) . ? C14 H14 0.9300 . ? C15 C16 1.395(6) . ? C15 H15 0.9300 . ? C16 C17 1.356(5) . ? C16 H16 0.9300 . ? C17 C18 1.409(4) . ? C17 H17 0.9300 . ? C18 C19 1.413(4) . ? C19 H19 0.9300 . ? 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 C4 O2 H2B 117(3) . . ? C8 N1 N2 115.8(3) . . ? C7 N2 N1 119.2(3) . . ? C7 N2 H2A 125(4) . . ? N1 N2 H2A 114(4) . . ? C6 C1 C2 117.5(3) . . ? C6 C1 C7 118.0(3) . . ? C2 C1 C7 124.5(3) . . ? C3 C2 C1 121.0(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.6(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? O2 C4 C3 118.2(4) . . ? O2 C4 C5 122.5(4) . . ? C3 C4 C5 119.3(4) . . ? C6 C5 C4 119.5(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 122.0(3) . . ? C5 C6 H6 119.0 . . ? C1 C6 H6 119.0 . . ? O1 C7 N2 121.7(4) . . ? O1 C7 C1 121.9(3) . . ? N2 C7 C1 116.3(4) . . ? N1 C8 C10 115.7(3) . . ? N1 C8 C9 123.6(3) . . ? C10 C8 C9 120.7(3) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C19 C10 C11 117.8(3) . . ? C19 C10 C8 121.8(3) . . ? C11 C10 C8 120.4(3) . . ? C12 C11 C10 121.0(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 121.9(3) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C14 C13 C12 123.5(4) . . ? C14 C13 C18 119.0(3) . . ? C12 C13 C18 117.5(3) . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 120.9(4) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C19 121.8(3) . . ? C17 C18 C13 118.7(3) . . ? C19 C18 C13 119.5(3) . . ? C10 C19 C18 122.2(3) . . ? C10 C19 H19 118.9 . . ? C18 C19 H19 118.9 . . ? 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 C8 N1 N2 C7 -164.5(3) . . . . ? C6 C1 C2 C3 0.9(5) . . . . ? C7 C1 C2 C3 -178.1(3) . . . . ? C1 C2 C3 C4 -1.3(6) . . . . ? C2 C3 C4 O2 178.7(3) . . . . ? C2 C3 C4 C5 0.3(6) . . . . ? O2 C4 C5 C6 -177.3(3) . . . . ? C3 C4 C5 C6 1.1(5) . . . . ? C4 C5 C6 C1 -1.5(5) . . . . ? C2 C1 C6 C5 0.5(5) . . . . ? C7 C1 C6 C5 179.5(3) . . . . ? N1 N2 C7 O1 4.1(5) . . . . ? N1 N2 C7 C1 -178.5(3) . . . . ? C6 C1 C7 O1 -19.3(4) . . . . ? C2 C1 C7 O1 159.6(3) . . . . ? C6 C1 C7 N2 163.3(3) . . . . ? C2 C1 C7 N2 -17.7(4) . . . . ? N2 N1 C8 C10 -179.8(3) . . . . ? N2 N1 C8 C9 2.8(5) . . . . ? N1 C8 C10 C19 -171.7(3) . . . . ? C9 C8 C10 C19 5.8(5) . . . . ? N1 C8 C10 C11 7.3(4) . . . . ? C9 C8 C10 C11 -175.2(3) . . . . ? C19 C10 C11 C12 1.3(5) . . . . ? C8 C10 C11 C12 -177.7(3) . . . . ? C10 C11 C12 C13 -0.3(5) . . . . ? C11 C12 C13 C14 179.6(3) . . . . ? C11 C12 C13 C18 -1.2(5) . . . . ? C12 C13 C14 C15 178.7(3) . . . . ? C18 C13 C14 C15 -0.4(5) . . . . ? C13 C14 C15 C16 0.0(6) . . . . ? C14 C15 C16 C17 0.1(6) . . . . ? C15 C16 C17 C18 0.1(6) . . . . ? C16 C17 C18 C19 179.2(3) . . . . ? C16 C17 C18 C13 -0.5(5) . . . . ? C14 C13 C18 C17 0.6(5) . . . . ? C12 C13 C18 C17 -178.5(3) . . . . ? C14 C13 C18 C19 -179.1(3) . . . . ? C12 C13 C18 C19 1.7(5) . . . . ? C11 C10 C19 C18 -0.8(5) . . . . ? C8 C10 C19 C18 178.3(3) . . . . ? C17 C18 C19 C10 179.5(3) . . . . ? C13 C18 C19 C10 -0.8(5) . . . . ? 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) # N2 H2A O2 0.871(19) 2.37(3) 3.028(3) 132(3) 3_546 yes O2 H2B O1 0.99(3) 1.62(3) 2.610(3) 175(3) 3_656 yes C3 H3 Cg3 0.93 2.87 3.502(3) 129 3_656 yes C12 H12 Cg3 0.93 2.80 3.475(3) 130 3_465 yes C17 H17 Cg1 0.93 2.84 3.582(3) 137 3_656 yes _iucr_geom_hbonds_special_details ; Cg1 and Cg3 are the centroids of the (C1---C6)and (C13---C18)rings. ; loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O1 N1 2.692(3) . . yes O2 O1 2.610(3) . 3_656 yes N2 O2 3.028(3) . 3_546 yes H2B O1 1.62(3) . 3_656 yes O1 H6 2.52 . . yes H2A O2 2.37(3) . 3_546 yes N1 H11 2.46 . . yes H5 N1 2.75 . 3_656 yes N2 H9A 2.43 . . yes N2 H2 2.61 . . yes C2 H2A 2.67(4) . . yes C6 H16 2.81 . 2_565 yes H2B C7 2.62(3) . 3_656 yes C9 H2A 2.37(3) . . yes C9 H19 2.61 . . yes C19 H9C 2.57 . . yes H2 H2A 2.18 . . yes H2A H9A 2.01 . . yes H2A H2B 2.44(4) . 3_546 yes H9C H19 1.98 . . yes _refine_diff_density_max 0.179 _refine_diff_density_min -0.153 _refine_diff_density_rms 0.037 _shelx_res_file ; TITL topkaya10_0m_a.res in P2(1)2(1)2(1) shelx.res created by SHELXL-2018/3 at 16:29:10 on 23-Feb-2024 CELL 0.71073 6.1227 12.5222 20.3948 90.000 90.000 90.000 ZERR 4.00 0.0004 0.0003 0.0005 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 UNIT 76 64 8 8 MERG 2 OMIT 0 0 2 OMIT 0 1 1 DFIX 0.860 0.020 H2A N2 DFIX 1.000 0.020 H2B O2 FMAP 2 PLAN 20 SIZE 0.130 0.140 0.180 ACTA BOND $H CONF LIST 4 L.S. 10 TEMP 0.00 WGHT 0.046300 0.081800 FVAR 0.58591 O1 4 0.606288 0.796725 0.646978 11.00000 0.05551 0.04867 = 0.07779 -0.00517 -0.00655 0.00393 O2 4 0.116120 1.175934 0.790303 11.00000 0.06234 0.08931 = 0.10909 -0.04977 0.01378 -0.00252 N1 3 0.325514 0.659802 0.589992 11.00000 0.06357 0.04820 = 0.05782 -0.01047 0.00171 -0.00351 N2 3 0.256735 0.750053 0.623432 11.00000 0.05565 0.04734 = 0.06837 -0.01626 0.00150 -0.00752 C1 1 0.322342 0.906887 0.688631 11.00000 0.04679 0.03740 = 0.04735 0.00205 -0.00366 -0.00519 C2 1 0.113263 0.949029 0.680737 11.00000 0.04695 0.05206 = 0.06063 -0.00719 -0.01012 -0.00762 AFIX 43 H2 2 0.016369 0.916333 0.651924 11.00000 -1.20000 AFIX 0 C3 1 0.048032 1.038174 0.714879 11.00000 0.04401 0.06040 = 0.07465 -0.00741 -0.00197 -0.00021 AFIX 43 H3 2 -0.091192 1.065846 0.708263 11.00000 -1.20000 AFIX 0 C4 1 0.187145 1.086954 0.758854 11.00000 0.05048 0.06104 = 0.05605 -0.01104 0.00543 -0.01210 C5 1 0.395928 1.045179 0.768275 11.00000 0.05296 0.05899 = 0.04611 -0.00754 -0.00484 -0.01268 AFIX 43 H5 2 0.490571 1.076513 0.798307 11.00000 -1.20000 AFIX 0 C6 1 0.460646 0.957585 0.732943 11.00000 0.04423 0.04641 = 0.05027 0.00287 -0.00452 -0.00785 AFIX 43 H6 2 0.601321 0.931226 0.738766 11.00000 -1.20000 AFIX 0 C7 1 0.407425 0.813753 0.652558 11.00000 0.05730 0.04066 = 0.04453 0.00494 -0.00320 -0.00459 C8 1 0.182919 0.616752 0.551020 11.00000 0.05149 0.04660 = 0.04133 0.00131 -0.00048 -0.00708 C9 1 -0.040204 0.662388 0.539200 11.00000 0.07870 0.08108 = 0.08001 -0.02941 -0.02048 0.01849 AFIX 37 H9A 2 -0.034213 0.738799 0.542571 11.00000 -1.50000 H9B 2 -0.140035 0.634861 0.571321 11.00000 -1.50000 H9C 2 -0.089133 0.642706 0.496143 11.00000 -1.50000 AFIX 0 C10 1 0.256135 0.520490 0.515691 11.00000 0.05111 0.03924 = 0.04071 0.00433 -0.00233 -0.00400 C11 1 0.461336 0.472706 0.530680 11.00000 0.05735 0.04990 = 0.06014 -0.00193 -0.01551 -0.00410 AFIX 43 H11 2 0.546811 0.501198 0.564070 11.00000 -1.20000 AFIX 0 C12 1 0.534305 0.385903 0.496851 11.00000 0.05279 0.04602 = 0.07250 0.00418 -0.00756 0.00138 AFIX 43 H12 2 0.669307 0.356723 0.507611 11.00000 -1.20000 AFIX 0 C13 1 0.410836 0.338912 0.445889 11.00000 0.05444 0.04278 = 0.05158 0.00292 0.00082 -0.00588 C14 1 0.481816 0.249301 0.409553 11.00000 0.06735 0.04356 = 0.07299 -0.00112 0.01519 0.00258 AFIX 43 H14 2 0.617633 0.219218 0.418253 11.00000 -1.20000 AFIX 0 C15 1 0.352322 0.206570 0.361745 11.00000 0.09687 0.05145 = 0.06795 -0.01234 0.01556 -0.00139 AFIX 43 H15 2 0.400239 0.147573 0.338075 11.00000 -1.20000 AFIX 0 C16 1 0.148414 0.251175 0.348327 11.00000 0.09365 0.06241 = 0.05856 -0.01307 -0.00535 -0.00759 AFIX 43 H16 2 0.061327 0.221400 0.315745 11.00000 -1.20000 AFIX 0 C17 1 0.075311 0.337358 0.382119 11.00000 0.06629 0.05800 = 0.05127 -0.00650 -0.00684 -0.00199 AFIX 43 H17 2 -0.061230 0.365852 0.372474 11.00000 -1.20000 AFIX 0 C18 1 0.203905 0.384182 0.431657 11.00000 0.05327 0.04002 = 0.04199 0.00229 0.00207 -0.00551 C19 1 0.132496 0.474724 0.466966 11.00000 0.05210 0.04320 = 0.04329 0.00276 -0.00322 -0.00051 AFIX 43 H19 2 -0.002692 0.504358 0.456907 11.00000 -1.20000 AFIX 0 H2A 2 0.116147 0.753497 0.629525 11.00000 0.13475 H2B 2 0.227712 1.218816 0.813489 11.00000 0.14448 HKLF 4 REM topkaya10_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.1137, GooF = S = 1.027, Restrained GooF = 1.027 for all data REM R1 = 0.0503 for 1782 Fo > 4sig(Fo) and 0.1243 for all 3162 data REM 217 parameters refined using 2 restraints END WGHT 0.0463 0.0818 REM Highest difference peak 0.179, deepest hole -0.153, 1-sigma level 0.037 Q1 1 -0.1830 0.5949 0.5117 11.00000 0.05 0.18 Q2 1 0.1729 1.1194 0.8239 11.00000 0.05 0.14 Q3 1 0.5423 1.0763 0.8212 11.00000 0.05 0.13 Q4 1 0.7631 0.3469 0.5100 11.00000 0.05 0.12 Q5 1 -0.1547 0.5120 0.5451 11.00000 0.05 0.12 Q6 1 -0.1300 0.5139 0.4645 11.00000 0.05 0.12 Q7 1 0.2242 0.0531 0.3665 11.00000 0.05 0.12 Q8 1 0.6209 0.4530 0.4191 11.00000 0.05 0.12 Q9 1 -0.1180 1.0341 0.8006 11.00000 0.05 0.12 Q10 1 -0.1180 0.7523 0.4957 11.00000 0.05 0.11 Q11 1 -0.0002 0.6772 0.5349 11.00000 0.05 0.11 Q12 1 0.6120 0.3202 0.5394 11.00000 0.05 0.11 Q13 1 -0.1606 0.9767 0.7120 11.00000 0.05 0.11 Q14 1 -0.2370 0.9551 0.6305 11.00000 0.05 0.11 Q15 1 0.5779 0.4183 0.5889 11.00000 0.05 0.11 Q16 1 -0.1460 0.8766 0.5495 11.00000 0.05 0.11 Q17 1 -0.0786 0.7028 0.4786 11.00000 0.05 0.11 Q18 1 0.3617 0.0260 0.4007 11.00000 0.05 0.11 Q19 1 -0.1555 0.4061 0.3719 11.00000 0.05 0.11 Q20 1 0.0299 0.8744 0.6822 11.00000 0.05 0.10 ; _shelx_res_checksum 94223 _shelx_hkl_file ; 1 0 0 0.20 0.60 2 0 0 341.67 10.00 2 0 0 339.17 10.90 -2 0 0 343.27 10.80 3 0 0 9.40 3.20 -3 0 0 3.00 1.90 -4 0 0 141.29 8.60 4 0 0 135.89 7.80 4 0 0 116.29 8.40 5 0 0 3.30 2.30 -5 0 0 -3.50 2.40 -6 0 0 10.30 5.10 6 0 0 4.30 4.00 -7 0 0 -3.20 4.00 0 -1 0 -0.20 0.30 0 1 0 0.00 0.30 -1 1 0 0.10 0.50 1 -1 0 0.10 0.40 1 -1 0 -0.60 0.40 -1 1 0 -0.10 0.10 1 -1 0 0.30 0.30 1 -1 0 0.30 0.60 -1 1 0 0.20 0.20 1 1 0 -0.20 0.60 1 1 0 0.60 0.30 -2 1 0 493.15 12.40 -2 -1 0 499.75 14.20 -2 1 0 496.55 13.50 2 -1 0 500.15 12.60 2 1 0 490.35 13.20 2 -1 0 504.85 13.70 2 1 0 495.35 14.30 3 1 0 422.56 15.10 3 1 0 487.45 14.70 -3 -1 0 421.86 14.70 3 -1 0 412.36 14.40 3 -1 0 425.36 13.20 -3 1 0 423.66 14.10 4 -1 0 19.80 4.30 -4 1 0 29.40 4.60 4 1 0 22.90 6.40 4 -1 0 27.60 4.00 -4 -1 0 23.60 4.60 -5 -1 0 -2.60 2.60 5 1 0 3.80 2.40 -5 1 0 1.90 3.10 5 -1 0 2.80 2.20 -6 1 0 16.40 5.60 6 1 0 16.10 5.00 -6 -1 0 16.40 5.00 6 -1 0 12.50 3.90 -7 -1 0 5.60 4.90 -7 1 0 2.30 4.90 0 -2 0 230.88 6.40 0 2 0 225.48 6.50 0 -2 0 231.58 4.90 0 2 0 219.08 4.90 -1 2 0 1857.31 34.70 -1 2 0 1879.21 34.50 1 -2 0 1892.11 34.80 -1 -2 0 1865.91 36.20 1 -2 0 1837.12 34.10 1 2 0 1833.92 34.50 -1 -2 0 1835.32 34.20 -1 2 0 1848.81 35.10 1 2 0 1875.61 36.20 1 -2 0 1844.82 35.40 2 -2 0 52.19 2.60 2 2 0 49.90 2.40 2 -2 0 52.39 3.00 2 -2 0 47.90 3.20 -2 2 0 54.89 3.20 2 -2 0 49.70 3.50 2 2 0 50.89 2.30 -2 2 0 47.30 3.30 2 2 0 47.30 3.90 -2 -2 0 46.00 3.80 3 2 0 12.80 1.30 3 2 0 8.10 2.40 3 2 0 18.80 3.80 3 -2 0 13.00 2.50 3 -2 0 11.70 1.40 3 -2 0 10.50 1.50 -3 2 0 12.50 2.70 3 -2 0 12.10 2.80 -3 -2 0 14.80 3.10 -3 2 0 13.40 2.40 -4 -2 0 53.39 5.40 4 -2 0 44.30 4.50 4 -2 0 42.10 2.50 -4 2 0 45.00 4.90 4 2 0 44.70 2.50 4 2 0 47.80 5.00 4 -2 0 50.69 2.70 4 -2 0 47.10 2.90 4 -2 0 37.80 5.40 4 -2 0 48.10 2.80 -5 2 0 -1.30 2.50 5 2 0 -1.60 2.30 5 -2 0 2.10 2.10 -5 -2 0 -1.20 2.80 -6 2 0 3.70 4.50 -6 -2 0 -0.90 2.90 6 2 0 2.90 3.50 -7 -2 0 3.90 5.30 -7 2 0 -2.30 3.40 7 2 0 7.80 4.80 0 -3 0 -0.70 0.40 0 -3 0 0.10 0.60 0 -3 0 -0.70 0.60 0 3 0 -0.30 0.80 0 3 0 -0.60 0.60 0 3 0 0.40 0.30 -1 -3 0 3.50 1.10 1 3 0 1.70 0.90 1 3 0 3.10 1.40 -1 -3 0 2.40 1.20 1 -3 0 3.20 1.10 1 -3 0 2.20 1.10 -1 3 0 0.60 1.00 -1 3 0 4.30 0.70 -1 -3 0 2.90 1.10 -1 3 0 4.70 1.30 -2 3 0 68.59 3.70 -2 3 0 62.49 3.30 2 3 0 67.29 4.90 -2 -3 0 64.89 2.60 2 3 0 60.19 3.40 2 -3 0 58.39 3.40 2 3 0 64.59 3.50 -2 -3 0 67.19 4.90 -2 3 0 65.69 3.60 2 -3 0 67.39 4.10 3 3 0 24.80 5.40 -3 3 0 22.50 3.10 3 -3 0 21.20 2.40 3 -3 0 24.70 2.70 -3 3 0 24.70 3.40 3 3 0 24.30 2.20 -3 -3 0 28.20 4.70 3 -3 0 23.60 3.20 3 -3 0 21.00 3.30 3 3 0 25.30 2.30 4 -3 0 5.30 2.20 4 -3 0 5.20 2.20 4 3 0 4.70 1.40 4 -3 0 5.40 1.50 -4 -3 0 6.60 1.80 -4 -3 0 5.80 1.70 -4 -3 0 8.90 2.90 4 3 0 2.80 1.90 4 -3 0 4.90 1.60 -4 3 0 6.70 2.90 4 -3 0 7.70 2.90 4 3 0 4.00 1.40 -5 -3 0 -3.90 2.60 5 3 0 0.60 2.70 -5 3 0 0.20 3.20 -6 -3 0 27.90 6.40 -6 3 0 31.80 6.20 -7 -3 0 0.20 5.00 7 3 0 0.70 5.10 -7 3 0 -0.90 5.20 0 -4 0 126.99 5.80 0 4 0 138.79 4.00 0 4 0 127.59 5.70 0 -4 0 129.79 3.70 0 4 0 112.49 5.80 0 -4 0 117.29 5.50 1 -4 0 137.29 6.40 -1 -4 0 138.39 5.80 1 4 0 149.59 6.30 -1 4 0 134.99 5.90 1 4 0 144.39 6.30 -1 -4 0 137.59 5.80 -1 4 0 142.09 6.60 1 4 0 139.19 5.90 -1 -4 0 136.69 5.80 1 -4 0 133.79 6.10 2 -4 0 58.89 3.60 -2 4 0 66.79 3.70 -2 4 0 66.39 4.30 -2 -4 0 61.49 3.40 -2 -4 0 63.79 4.80 2 4 0 65.59 5.10 -2 4 0 67.39 3.40 2 -4 0 63.29 4.20 2 -4 0 57.39 4.30 2 4 0 67.09 4.20 2 4 0 61.89 3.90 -3 4 0 19.20 2.90 -3 4 0 25.50 3.40 3 4 0 21.00 2.70 3 -4 0 21.10 3.10 -3 4 0 22.40 1.30 -3 4 0 20.50 1.40 3 4 0 20.50 4.10 3 -4 0 27.10 2.90 -3 -4 0 20.10 4.80 3 4 0 19.00 2.70 3 -4 0 23.40 3.40 4 -4 0 26.30 5.40 -4 4 0 29.20 4.20 -4 -4 0 24.00 4.80 4 -4 0 18.70 2.90 4 -4 0 20.10 3.70 4 -4 0 21.70 3.40 4 4 0 30.10 4.00 4 4 0 26.10 4.60 4 4 0 27.50 2.90 -4 4 0 24.40 4.20 5 -4 0 230.48 11.60 5 -4 0 228.08 9.20 -5 4 0 244.78 12.20 -5 -4 0 226.58 7.40 -5 -4 0 223.38 13.50 5 -4 0 180.08 9.30 -5 -4 0 239.78 7.50 5 4 0 235.78 13.30 -6 4 0 22.80 5.10 6 4 0 15.40 5.60 -6 -4 0 21.90 5.60 -7 -4 0 -5.50 4.20 7 4 0 -1.90 4.50 0 5 0 0.30 0.50 0 5 0 -0.30 0.90 0 5 0 -1.60 1.00 0 -5 0 1.00 1.20 0 -5 0 -0.20 1.00 -1 -5 0 57.89 4.20 -1 -5 0 69.99 4.40 1 5 0 65.19 4.30 -1 5 0 66.39 5.00 1 -5 0 66.19 5.00 -1 5 0 69.39 4.50 1 -5 0 63.89 4.50 1 5 0 60.89 4.60 -1 -5 0 66.19 4.00 1 5 0 69.89 4.80 2 -5 0 187.98 8.60 -2 5 0 174.28 7.30 -2 -5 0 186.78 7.10 2 5 0 179.58 8.00 2 -5 0 181.18 7.80 -2 -5 0 181.78 7.10 -2 -5 0 181.08 8.50 -2 5 0 164.28 7.80 -2 5 0 184.28 7.30 2 5 0 174.68 8.60 2 5 0 163.08 7.60 -2 5 0 187.78 6.30 -3 -5 0 -0.20 2.30 -3 5 0 -0.60 1.60 3 5 0 -0.20 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