data_3 _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H13 N5 Ni O' _chemical_formula_weight 326.00 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' 'Ni' 'Ni' 0.3393 1.1124 '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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -y, -z' _cell_length_a 7.3030(11) _cell_length_b 9.0155(10) _cell_length_c 10.5740(12) _cell_angle_alpha 88.6220(10) _cell_angle_beta 77.0440(10) _cell_angle_gamma 85.6050(10) _cell_volume 676.46(15) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1501 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 25.8 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_F_000 336 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.130 _exptl_absorpt_coefficient_mu 1.440 _shelx_estimated_absorpt_T_min 0.813 _shelx_estimated_absorpt_T_max 0.835 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8112 _exptl_absorpt_correction_T_max 0.8273 _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'SMART CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3662 _diffrn_reflns_av_unetI/netI 0.0323 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.976 _diffrn_reflns_theta_max 25.493 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.987 _diffrn_measured_fraction_theta_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.987 _diffrn_reflns_point_group_measured_fraction_full 0.987 _reflns_number_total 2307 _reflns_number_gt 1937 _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 SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.0330P)^2^+0.4678P] 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 2307 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0820 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _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 Ni1 Ni 0.32096(5) 0.48820(4) 0.40978(4) 0.03254(15) Uani 1 1 d . . . . . O1 O 0.2235(3) 0.3174(2) 0.4839(2) 0.0394(5) Uani 1 1 d . . . . . N1 N 0.2358(3) 0.6012(3) 0.5570(2) 0.0298(5) Uani 1 1 d . . . . . N2 N 0.4172(3) 0.6678(3) 0.3321(2) 0.0339(6) Uani 1 1 d . . . . . N3 N 0.4203(4) 0.3786(4) 0.2541(3) 0.0521(8) Uani 1 1 d . . . . . N4 N 0.3205(4) 0.3013(3) 0.2146(3) 0.0455(7) Uani 1 1 d . . . . . N5 N 0.2298(5) 0.2248(4) 0.1726(4) 0.0710(10) Uani 1 1 d . . . . . C1 C 0.5135(4) 0.6846(4) 0.2079(3) 0.0455(8) Uani 1 1 d . . . . . H1 H 0.541852 0.602086 0.153989 0.055 Uiso 1 1 calc R U . . . C2 C 0.5706(5) 0.8208(4) 0.1597(3) 0.0524(10) Uani 1 1 d . . . . . H2 H 0.639002 0.829275 0.074684 0.063 Uiso 1 1 calc R U . . . C3 C 0.5267(4) 0.9431(4) 0.2367(4) 0.0514(10) Uani 1 1 d . . . . . H3 H 0.562808 1.035918 0.204489 0.062 Uiso 1 1 calc R U . . . C4 C 0.4283(4) 0.9275(4) 0.3626(3) 0.0428(8) Uani 1 1 d . . . . . H4 H 0.395776 1.009738 0.416564 0.051 Uiso 1 1 calc R U . . . C5 C 0.3781(4) 0.7879(4) 0.4082(3) 0.0356(7) Uani 1 1 d . . . . . C6 C 0.2788(5) 0.7580(3) 0.5449(3) 0.0404(8) Uani 1 1 d . . . . . H6A H 0.358151 0.779051 0.603595 0.048 Uiso 1 1 calc R U . . . H6B H 0.163268 0.821700 0.567387 0.048 Uiso 1 1 calc R U . . . C7 C 0.1408(4) 0.5586(3) 0.6681(3) 0.0336(7) Uani 1 1 d . . . . . H7 H 0.106946 0.628999 0.733611 0.040 Uiso 1 1 calc R U . . . C8 C 0.0839(4) 0.4120(3) 0.6980(3) 0.0324(7) Uani 1 1 d . . . . . C9 C 0.1282(4) 0.2993(3) 0.6039(3) 0.0332(7) Uani 1 1 d . . . . . C10 C 0.0645(4) 0.1582(3) 0.6424(3) 0.0422(8) Uani 1 1 d . . . . . H10 H 0.087826 0.081935 0.581961 0.051 Uiso 1 1 calc R U . . . C11 C -0.0310(4) 0.1303(4) 0.7666(3) 0.0463(9) Uani 1 1 d . . . . . H11 H -0.068819 0.035137 0.788487 0.056 Uiso 1 1 calc R U . . . C12 C -0.0732(4) 0.2405(4) 0.8614(3) 0.0437(8) Uani 1 1 d . . . . . C13 C -0.0159(4) 0.3798(4) 0.8249(3) 0.0402(8) Uani 1 1 d . . . . . H13 H -0.043850 0.455567 0.885964 0.048 Uiso 1 1 calc R U . . . C14 C -0.1747(5) 0.2065(5) 0.9991(3) 0.0644(11) Uani 1 1 d . . . . . H14A H -0.085640 0.163651 1.046530 0.097 Uiso 1 1 calc R U . . . H14B H -0.268027 0.137465 0.997777 0.097 Uiso 1 1 calc R U . . . H14C H -0.234765 0.296739 1.040390 0.097 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 Ni1 0.0317(2) 0.0346(2) 0.0295(2) -0.00215(17) -0.00343(15) -0.00064(15) O1 0.0463(12) 0.0328(12) 0.0365(12) -0.0049(10) -0.0024(10) -0.0042(9) N1 0.0309(12) 0.0291(13) 0.0297(13) 0.0004(11) -0.0077(10) -0.0018(10) N2 0.0268(12) 0.0451(16) 0.0299(13) 0.0038(13) -0.0076(10) -0.0007(11) N3 0.0512(18) 0.059(2) 0.0416(17) -0.0134(16) 0.0020(14) -0.0084(15) N4 0.0544(18) 0.0429(18) 0.0345(16) -0.0058(14) -0.0033(14) 0.0074(15) N5 0.078(2) 0.066(2) 0.072(2) -0.029(2) -0.0211(19) -0.0017(19) C1 0.0387(18) 0.060(2) 0.0363(18) 0.0022(17) -0.0047(14) -0.0061(16) C2 0.0416(19) 0.075(3) 0.039(2) 0.018(2) -0.0041(15) -0.0154(18) C3 0.0407(19) 0.057(2) 0.057(2) 0.021(2) -0.0111(16) -0.0141(17) C4 0.0370(17) 0.0427(19) 0.049(2) 0.0045(17) -0.0078(15) -0.0088(14) C5 0.0293(15) 0.0388(18) 0.0398(18) 0.0043(16) -0.0099(13) -0.0029(13) C6 0.0485(18) 0.0303(17) 0.0404(18) -0.0008(15) -0.0053(14) -0.0043(14) C7 0.0336(15) 0.0369(17) 0.0287(16) -0.0049(14) -0.0035(13) -0.0012(13) C8 0.0304(15) 0.0336(17) 0.0333(16) 0.0009(15) -0.0068(12) -0.0037(12) C9 0.0276(14) 0.0334(17) 0.0402(18) 0.0046(15) -0.0118(13) -0.0012(12) C10 0.0403(17) 0.0300(17) 0.058(2) -0.0011(16) -0.0145(16) -0.0009(14) C11 0.0393(18) 0.0404(19) 0.062(2) 0.0155(19) -0.0154(16) -0.0111(15) C12 0.0343(16) 0.055(2) 0.0433(19) 0.0156(18) -0.0107(14) -0.0112(15) C13 0.0376(17) 0.048(2) 0.0338(17) -0.0002(16) -0.0054(13) -0.0060(14) C14 0.065(2) 0.079(3) 0.049(2) 0.021(2) -0.0087(18) -0.024(2) _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 Ni1 O1 1.831(2) . ? Ni1 N1 1.842(2) . ? Ni1 N2 1.908(2) . ? Ni1 N3 1.909(3) . ? O1 C9 1.317(3) . ? N1 C7 1.289(3) . ? N1 C6 1.468(4) . ? N2 C5 1.339(4) . ? N2 C1 1.354(4) . ? N3 N4 1.192(4) . ? N4 N5 1.153(4) . ? C1 C2 1.377(5) . ? C1 H1 0.9300 . ? C2 C3 1.361(5) . ? C2 H2 0.9300 . ? C3 C4 1.374(5) . ? C3 H3 0.9300 . ? C4 C5 1.383(4) . ? C4 H4 0.9300 . ? C5 C6 1.492(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.423(4) . ? C7 H7 0.9300 . ? C8 C9 1.407(4) . ? C8 C13 1.411(4) . ? C9 C10 1.407(4) . ? C10 C11 1.369(5) . ? C10 H10 0.9300 . ? C11 C12 1.396(5) . ? C11 H11 0.9300 . ? C12 C13 1.374(4) . ? C12 C14 1.515(4) . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 Ni1 N1 94.84(10) . . ? O1 Ni1 N2 178.74(9) . . ? N1 Ni1 N2 84.92(10) . . ? O1 Ni1 N3 88.10(11) . . ? N1 Ni1 N3 176.74(11) . . ? N2 Ni1 N3 92.18(12) . . ? C9 O1 Ni1 127.2(2) . . ? C7 N1 C6 116.8(3) . . ? C7 N1 Ni1 127.3(2) . . ? C6 N1 Ni1 115.85(18) . . ? C5 N2 C1 118.3(3) . . ? C5 N2 Ni1 115.57(19) . . ? C1 N2 Ni1 126.1(3) . . ? N4 N3 Ni1 119.0(2) . . ? N5 N4 N3 177.4(4) . . ? N2 C1 C2 121.6(4) . . ? N2 C1 H1 119.2 . . ? C2 C1 H1 119.2 . . ? C3 C2 C1 119.9(3) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 119.2(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N2 C5 C4 122.0(3) . . ? N2 C5 C6 114.7(3) . . ? C4 C5 C6 123.3(3) . . ? N1 C6 C5 108.8(3) . . ? N1 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? N1 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N1 C7 C8 125.0(3) . . ? N1 C7 H7 117.5 . . ? C8 C7 H7 117.5 . . ? C9 C8 C13 120.0(3) . . ? C9 C8 C7 121.0(3) . . ? C13 C8 C7 119.0(3) . . ? O1 C9 C10 118.6(3) . . ? O1 C9 C8 124.6(3) . . ? C10 C9 C8 116.9(3) . . ? C11 C10 C9 121.7(3) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 122.0(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 117.2(3) . . ? C13 C12 C14 121.6(4) . . ? C11 C12 C14 121.2(3) . . ? C12 C13 C8 122.2(3) . . ? C12 C13 H13 118.9 . . ? C8 C13 H13 118.9 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _refine_diff_density_max 0.393 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.057 _shelx_res_file ; TITL 20181129a_0m_a.res in P-1 20181129a_0m.res created by SHELXL-2018/3 at 09:37:07 on 30-Mar-2022 CELL 0.71073 7.3030 9.0155 10.5740 88.622 77.044 85.605 ZERR 2 0.0011 0.0010 0.0012 0.001 0.001 0.001 LATT 1 SFAC C H N Ni O UNIT 28 26 10 2 2 OMIT -3.00 51.00 L.S. 8 ACTA BOND $H FMAP 2 PLAN 2 HTAB SIZE 0.15 0.13 0.13 TEMP 25 WGHT 0.033000 0.467800 FVAR 0.54244 NI1 4 0.320957 0.488204 0.409781 11.00000 0.03171 0.03461 = 0.02949 -0.00215 -0.00343 -0.00064 O1 5 0.223511 0.317406 0.483893 11.00000 0.04628 0.03276 = 0.03652 -0.00485 -0.00242 -0.00423 N1 3 0.235767 0.601233 0.557029 11.00000 0.03089 0.02909 = 0.02973 0.00042 -0.00772 -0.00179 N2 3 0.417156 0.667798 0.332072 11.00000 0.02675 0.04511 = 0.02992 0.00376 -0.00760 -0.00066 N3 3 0.420316 0.378604 0.254133 11.00000 0.05116 0.05921 = 0.04156 -0.01338 0.00198 -0.00845 N4 3 0.320501 0.301307 0.214623 11.00000 0.05436 0.04287 = 0.03455 -0.00584 -0.00326 0.00744 N5 3 0.229750 0.224846 0.172616 11.00000 0.07828 0.06609 = 0.07154 -0.02889 -0.02107 -0.00167 C1 1 0.513531 0.684554 0.207939 11.00000 0.03870 0.05991 = 0.03633 0.00219 -0.00473 -0.00611 AFIX 43 H1 2 0.541852 0.602086 0.153989 11.00000 -1.20000 AFIX 0 C2 1 0.570587 0.820817 0.159711 11.00000 0.04162 0.07496 = 0.03918 0.01797 -0.00410 -0.01539 AFIX 43 H2 2 0.639002 0.829275 0.074684 11.00000 -1.20000 AFIX 0 C3 1 0.526703 0.943137 0.236676 11.00000 0.04071 0.05743 = 0.05676 0.02122 -0.01109 -0.01408 AFIX 43 H3 2 0.562808 1.035918 0.204489 11.00000 -1.20000 AFIX 0 C4 1 0.428285 0.927451 0.362603 11.00000 0.03704 0.04267 = 0.04855 0.00445 -0.00780 -0.00878 AFIX 43 H4 2 0.395776 1.009738 0.416564 11.00000 -1.20000 AFIX 0 C5 1 0.378097 0.787850 0.408212 11.00000 0.02925 0.03883 = 0.03976 0.00429 -0.00994 -0.00286 C6 1 0.278841 0.758019 0.544862 11.00000 0.04849 0.03033 = 0.04040 -0.00084 -0.00525 -0.00431 AFIX 23 H6A 2 0.358151 0.779051 0.603595 11.00000 -1.20000 H6B 2 0.163268 0.821700 0.567387 11.00000 -1.20000 AFIX 0 C7 1 0.140824 0.558584 0.668056 11.00000 0.03359 0.03691 = 0.02872 -0.00493 -0.00353 -0.00117 AFIX 43 H7 2 0.106946 0.628999 0.733611 11.00000 -1.20000 AFIX 0 C8 1 0.083858 0.411976 0.698015 11.00000 0.03038 0.03362 = 0.03330 0.00088 -0.00682 -0.00370 C9 1 0.128155 0.299252 0.603948 11.00000 0.02758 0.03343 = 0.04024 0.00461 -0.01184 -0.00124 C10 1 0.064473 0.158188 0.642438 11.00000 0.04033 0.02997 = 0.05776 -0.00112 -0.01448 -0.00094 AFIX 43 H10 2 0.087826 0.081935 0.581961 11.00000 -1.20000 AFIX 0 C11 1 -0.030955 0.130345 0.766602 11.00000 0.03926 0.04037 = 0.06182 0.01545 -0.01539 -0.01107 AFIX 43 H11 2 -0.068819 0.035137 0.788487 11.00000 -1.20000 AFIX 0 C12 1 -0.073166 0.240487 0.861368 11.00000 0.03432 0.05500 = 0.04331 0.01562 -0.01067 -0.01116 C13 1 -0.015916 0.379847 0.824934 11.00000 0.03763 0.04838 = 0.03384 -0.00017 -0.00537 -0.00595 AFIX 43 H13 2 -0.043850 0.455567 0.885964 11.00000 -1.20000 AFIX 0 C14 1 -0.174697 0.206471 0.999131 11.00000 0.06503 0.07908 = 0.04890 0.02150 -0.00868 -0.02400 AFIX 137 H14A 2 -0.085640 0.163651 1.046530 11.00000 -1.50000 H14B 2 -0.268027 0.137465 0.997777 11.00000 -1.50000 H14C 2 -0.234765 0.296739 1.040390 11.00000 -1.50000 AFIX 0 HKLF 4 1 -1.0000 0.0000 0.0000 0.0000 0.0000 -0.5000 0.0000 -1.0000 0.0000 REM 20181129a_0m_a.res in P-1 REM wR2 = 0.0820, GooF = S = 1.055, Restrained GooF = 1.055 for all data REM R1 = 0.0346 for 1937 Fo > 4sig(Fo) and 0.0461 for all 2307 data REM 191 parameters refined using 0 restraints END WGHT 0.0353 0.4264 REM Instructions for potential hydrogen bonds HTAB C1 N3 EQIV $1 -x+1, -y+1, -z HTAB C2 N5_$1 EQIV $2 -x, -y+1, -z+1 HTAB C7 N5_$2 REM Highest difference peak 0.393, deepest hole -0.288, 1-sigma level 0.057 Q1 1 0.2502 0.4514 0.4948 11.00000 0.05 0.39 Q2 1 0.3324 0.4903 0.3091 11.00000 0.05 0.33 ; _shelx_res_checksum 17027 _shelx_hkl_file ; -1 0 0 195.58 2.50 1 0 0 188.38 2.10 -2 0 0 30.70 1.30 2 0 0 27.90 1.10 -3 0 0 226.18 4.20 3 0 0 226.08 3.50 -4 0 0 2.60 0.90 4 0 0 2.90 0.80 -5 0 0 56.09 2.80 5 0 0 58.19 2.50 -6 0 0 12.40 2.20 6 0 0 13.10 1.80 -7 0 0 0.30 1.50 7 0 0 -0.60 1.40 -8 0 0 31.00 3.80 -9 0 0 11.40 3.30 -9 1 0 39.10 5.20 -8 1 0 15.20 3.20 -7 1 0 20.60 3.20 6 -1 0 -0.50 1.10 -6 1 0 0.80 1.10 5 -1 0 25.20 2.00 -5 1 0 22.90 2.40 4 -1 0 188.08 3.60 -4 1 0 188.28 4.50 3 -1 0 289.97 4.10 -3 1 0 282.87 5.00 2 -1 0 15.60 0.90 -2 1 0 16.80 1.00 1 -1 0 1191.48 9.70 -1 1 0 1192.88 10.20 0 -1 0 2205.28 17.70 0 -1 0 2255.67 17.30 0 1 0 2163.78 16.90 0 1 0 2223.28 17.00 0 1 0 2241.08 17.60 -2 -1 0 3312.07 26.10 2 1 0 3275.17 25.40 -3 -1 0 192.18 3.80 3 1 0 202.28 3.30 -4 -1 0 22.70 1.70 4 1 0 24.30 1.60 -5 -1 0 99.19 3.60 5 1 0 101.69 3.10 -6 -1 0 37.10 2.70 6 1 0 37.90 2.50 -7 -1 0 23.50 3.00 -8 -1 0 1.00 1.90 -9 -1 0 -1.10 2.00 -9 2 0 19.30 3.90 -8 2 0 -1.80 1.90 7 -2 0 67.69 4.00 -7 2 0 56.49 4.10 6 -2 0 45.80 2.90 -6 2 0 48.80 3.30 5 -2 0 27.60 2.10 -5 2 0 26.70 2.30 4 -2 0 2.50 0.90 -4 2 0 2.40 0.80 3 -2 0 12.80 1.20 -3 2 0 12.80 1.50 2 -2 0 91.39 2.10 -2 2 0 91.59 2.40 1 -2 0 5.50 0.60 -1 2 0 7.20 0.70 -1 2 0 6.30 0.70 0 2 0 103.59 1.90 0 2 0 102.69 1.60 1 2 0 139.49 2.50 2 2 0 8381.56 63.29 -3 -2 0 49.50 1.90 -4 -2 0 1.20 0.70 4 2 0 -0.20 0.90 -5 -2 0 94.89 3.50 5 2 0 89.69 3.00 -6 -2 0 1.60 1.20 6 2 0 0.90 1.30 -7 -2 0 36.40 3.60 7 2 0 36.20 2.90 9 2 0 5.30 2.50 -8 3 0 28.60 4.10 -7 3 0 82.69 4.90 6 -3 0 11.30 1.90 -6 3 0 12.80 2.60 5 -3 0 83.39 3.20 -5 3 0 79.19 3.70 4 -3 0 6.30 1.30 -4 3 0 7.40 1.60 3 -3 0 3.80 1.00 -3 3 0 6.20 1.20 2 -3 0 169.58 3.20 -2 3 0 176.88 3.70 1 -3 0 136.09 2.70 -1 3 0 135.79 2.70 -1 3 0 135.59 2.70 0 -3 0 57.29 1.70 0 3 0 56.59 1.70 0 3 0 58.89 1.40 1 3 0 72.19 2.10 2 3 0 671.23 7.90 2 3 0 656.33 6.40 3 3 0 9.40 1.00 4 3 0 935.41 10.20 5 3 0 45.00 2.50 5 3 0 45.70 2.40 6 3 0 16.30 2.10 7 3 0 25.90 2.90 7 3 0 25.20 2.50 7 3 0 24.00 2.60 8 3 0 1.80 1.90 9 3 0 6.50 2.70 -8 4 0 26.00 4.20 -7 4 0 53.89 4.50 6 -4 0 5.40 1.80 -6 4 0 5.20 2.10 5 -4 0 155.78 4.30 -5 4 0 174.78 5.60 4 -4 0 64.89 2.70 -4 4 0 60.49 3.20 3 -4 0 103.29 3.00 -3 4 0 104.69 3.50 2 -4 0 10.80 1.20 -2 4 0 13.70 1.60 1 -4 0 273.37 4.60 -1 4 0 270.57 4.50 -1 4 0 272.57 4.40 0 -4 0 135.99 3.10 0 4 0 135.79 3.10 0 4 0 134.59 2.60 -1 -4 0 445.56 6.20 1 4 0 451.15 6.30 2 4 0 2.80 0.80 2 4 0 2.50 0.50 3 4 0 264.77 3.90 3 4 0 261.77 5.20 4 4 0 1131.59 13.30 4 4 0 1134.39 11.60 5 4 0 12.80 1.70 5 4 0 13.40 1.60 6 4 0 -0.70 1.10 6 4 0 0.50 1.40 6 4 0 1.40 1.10 7 4 0 32.20 3.00 7 4 0 28.40 2.80 7 4 0 29.70 2.90 8 4 0 4.80 2.00 9 4 0 8.30 2.70 -8 5 0 4.10 2.90 -7 5 0 11.00 3.10 6 -5 0 82.49 3.90 -6 5 0 86.69 4.90 5 -5 0 138.49 4.30 -5 5 0 135.49 5.20 4 -5 0 2.70 1.40 -4 5 0 1.80 1.40 3 -5 0 283.07 5.40 -3 5 0 272.07 5.90 2 -5 0 101.89 3.20 -2 5 0 103.79 3.30 -2 5 0 101.39 3.30 1 -5 0 107.49 3.10 -1 5 0 104.39 2.90 -1 5 0 107.59 3.10 0 -5 0 1049.09 11.60 0 5 0 1022.30 10.20 0 5 0 1037.80 11.50 -1 -5 0 218.68 4.50 1 5 0 226.78 4.70 2 5 0 28.10 1.90 3 5 0 154.38 4.30 3 5 0 154.48 2.90 4 5 0 55.29 2.80 4 5 0 60.49 2.20 5 5 0 4.30 1.10 5 5 0 3.00 1.20 6 5 0 181.88 4.70 6 5 0 188.68 5.10 6 5 0 180.18 5.70 7 5 0 9.30 2.00 7 5 0 8.10 1.80 7 5 0 7.10 2.00 8 5 0 11.70 3.30 8 5 0 12.30 2.40 8 5 0 8.80 2.30 9 5 0 9.70 2.60 -7 6 0 1.90 2.40 6 -6 0 53.69 3.70 -6 6 0 56.99 4.40 5 -6 0 48.40 3.40 -5 6 0 54.19 3.90 4 -6 0 47.10 3.00 -4 6 0 45.10 3.30 3 -6 0 284.47 5.90 -3 6 0 284.37 6.40 2 -6 0 1.30 1.20 -2 6 0 0.40 1.10 -2 6 0 -0.80 0.90 1 -6 0 381.06 6.60 -1 6 0 382.76 6.60 -1 6 0 387.46 6.20 0 -6 0 76.29 2.90 0 6 0 81.09 3.00 0 6 0 78.69 2.40 -1 -6 0 12.30 1.60 1 6 0 11.20 1.50 1 6 0 10.90 1.10 2 6 0 299.27 6.20 3 6 0 191.48 5.20 4 6 0 0.80 0.80 4 6 0 0.70 1.00 5 6 0 152.08 3.80 5 6 0 154.08 5.30 6 6 0 80.59 4.60 6 6 0 82.39 3.20 7 6 0 -0.90 1.50 7 6 0 2.20 1.40 7 6 0 0.90 1.60 8 6 0 4.70 2.30 8 6 0 4.80 1.90 8 6 0 4.20 2.10 9 6 0 3.90 2.10 -7 7 0 5.30 2.80 6 -7 0 12.10 2.60 -6 7 0 12.70 3.10 5 -7 0 -1.50 1.60 -5 7 0 1.90 1.80 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6 -10 84.79 3.10 -1 6 -10 87.79 4.00 1 -6 10 86.39 3.80 -2 6 -10 8.00 2.10 2 -6 10 9.70 2.00 -3 6 -10 59.79 4.00 3 -6 10 57.29 3.70 -4 6 -10 2.60 2.20 4 -6 10 5.10 2.20 -5 6 -10 34.70 4.50 5 -6 10 29.40 3.60 -6 6 -10 32.70 4.60 6 -6 10 22.20 3.70 8 5 -10 -1.30 2.20 7 5 -10 13.40 2.80 6 5 -10 32.50 3.40 5 5 -10 46.90 3.20 4 5 -10 179.98 5.10 3 5 -10 203.08 5.10 2 5 -10 2.00 1.20 -2 -5 10 4.20 1.20 1 5 -10 239.78 5.40 -1 -5 10 239.88 5.00 0 5 -10 182.38 5.00 0 -5 10 172.68 4.40 -1 5 -10 21.20 2.40 1 -5 10 23.70 2.20 -2 5 -10 0.30 1.30 2 -5 10 0.30 1.40 -3 5 -10 25.30 3.10 3 -5 10 22.70 2.60 -4 5 -10 21.50 3.10 4 -5 10 30.40 3.20 -5 5 -10 89.89 5.30 5 -5 10 91.99 4.90 -6 5 -10 21.40 3.80 6 -5 10 17.20 3.40 -7 5 -10 15.80 3.60 7 -5 10 11.40 3.30 8 4 -10 0.90 2.30 7 4 -10 8.10 2.50 6 4 -10 13.40 2.40 5 4 -10 15.30 2.20 4 4 -10 176.58 4.90 3 4 -10 175.58 4.60 2 4 -10 135.09 4.00 1 4 -10 188.98 4.60 -1 -4 10 188.98 4.10 0 4 -10 3.30 1.20 0 -4 10 3.40 1.00 -1 4 -10 113.59 3.90 1 -4 10 109.99 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-1.10 2.50 3 3 21 -1.40 2.00 4 3 21 -0.10 2.40 5 3 21 4.50 2.80 3 4 21 -7.70 3.00 4 4 21 0.30 2.30 5 4 21 3.00 2.60 4 5 21 -2.10 2.40 4 6 21 2.40 2.60 1 5 -22 8.30 2.70 0 5 -22 5.10 2.50 -1 5 -22 -2.00 2.10 2 4 -22 5.90 2.50 1 4 -22 9.90 2.90 0 4 -22 1.30 2.20 -1 4 -22 10.90 3.00 -2 4 -22 -0.70 2.20 2 3 -22 26.30 3.60 1 3 -22 0.70 2.20 0 3 -22 3.40 2.30 -1 3 -22 3.90 2.30 -2 3 -22 0.10 2.20 -3 3 -22 3.60 2.50 3 -3 22 -1.80 2.30 3 2 -22 9.80 2.50 2 2 -22 28.60 3.60 1 2 -22 0.90 1.90 0 2 -22 16.20 2.90 -1 2 -22 9.50 2.50 -2 2 -22 -3.90 1.80 -3 2 -22 21.40 3.80 3 -2 22 19.70 3.30 3 1 -22 14.20 2.90 2 1 -22 14.40 3.00 1 1 -22 19.60 3.00 0 1 -22 52.39 4.30 -1 1 -22 4.40 2.20 -2 1 -22 13.70 2.80 3 -1 22 14.00 3.10 4 -1 22 1.00 2.50 3 0 -22 10.50 2.60 2 0 -22 -3.80 1.40 1 0 -22 29.40 3.30 3 0 22 1.50 2.60 4 0 22 2.70 2.70 4 1 22 6.10 2.70 4 2 22 4.40 2.90 4 3 22 16.90 3.50 4 4 22 13.00 3.20 1 3 -23 -2.90 1.80 0 3 -23 0.70 2.20 -1 3 -23 -0.80 2.20 1 2 -23 -1.80 1.90 0 2 -23 0.40 2.10 -1 2 -23 6.00 2.30 -2 2 -23 1.60 2.30 2 1 -23 -0.70 1.90 1 1 -23 2.00 2.00 0 1 -23 -1.80 1.90 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 13429