data_compound_2 _audit_creation_method 'SHELXL-2018/1' _shelx_SHELXL_version_number '2018/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H11 Cl4 N10 O2 Ru, O3' _chemical_formula_sum 'C10 H11 Cl4 N10 O5 Ru' _chemical_formula_weight 594.16 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'Ru' 'Ru' -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 7 _space_group_name_H-M_alt 'P c' _space_group_name_Hall 'P -2yc' _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+1/2' _cell_length_a 7.3191(6) _cell_length_b 11.4326(8) _cell_length_c 11.4016(10) _cell_angle_alpha 90 _cell_angle_beta 91.643(3) _cell_angle_gamma 90 _cell_volume 953.65(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7542 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 27.10 _exptl_crystal_description 'cube' _exptl_crystal_colour 'orange' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.069 _exptl_crystal_F_000 586 _exptl_transmission_factor_min 0.62 _exptl_transmission_factor_max 0.75 _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_absorpt_coefficient_mu 1.433 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'Multi-Scan' _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details 'SADABS' _exptl_absorpt_special_details 'SADABS (version 2.03) was used for absorption correction. The ratio of minimum to maximum apparent transmission was 0.8357' _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'D8 VENTURE_PHOTON II' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7542 _diffrn_reflns_av_unetI/netI 0.0782 _diffrn_reflns_av_R_equivalents 0.0673 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.523 _diffrn_reflns_theta_max 27.100 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.955 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.955 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.955 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 3302 _reflns_number_gt 3106 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.994 _reflns_Friedel_fraction_max 0.955 _reflns_Friedel_fraction_full 0.999 _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 APEX' _computing_cell_refinement 'Bruker APEX' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_molecular_graphics 'DIAMOND' _computing_publication_material 'DIAMOND' _refine_special_details ; Refined as a 4-component inversion twin. ; _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^)+(0.0847P)^2^+5.4914P] 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_abs_structure_details ; Twinning involves inversion, so Flack parameter cannot be determined ; _refine_ls_abs_structure_Flack ? _chemical_absolute_configuration ? _refine_ls_number_reflns 3302 _refine_ls_number_parameters 276 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0591 _refine_ls_wR_factor_ref 0.1594 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.079 _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 Ru1 Ru 0.63189(14) 0.67737(7) 0.41364(11) 0.0142(3) Uani 1 1 d . . . . . O6 O 0.1177(15) 0.2512(8) 0.6123(9) 0.027(2) Uani 1 1 d . . . . . O66 O 0.8933(15) 1.2316(8) 0.3918(9) 0.028(2) Uani 1 1 d . . . . . O1W O 0.3747(13) 0.8193(7) 0.5958(8) 0.0192(14) Uani 1 1 d . U . . . O2W O 0.3089(11) 0.8719(6) 0.7621(7) 0.0118(13) Uani 1 1 d . U . . . O3W O 0.1759(12) 0.8905(7) 0.6376(8) 0.0151(12) Uani 1 1 d . U . . . N1 N 0.1020(17) 0.4389(10) 0.6709(10) 0.020(3) Uani 1 1 d . . . . . H1 H 0.024151 0.416837 0.723970 0.024 Uiso 1 1 calc R U . . . N2 N 0.0723(17) 0.6279(12) 0.7350(11) 0.026(3) Uani 1 1 d . . . . . H2A H 0.101762 0.702290 0.730050 0.040 Uiso 1 1 calc R U . . . H2B H -0.009578 0.605148 0.785264 0.040 Uiso 1 1 calc R U . . . N3 N 0.2734(15) 0.5857(9) 0.5922(9) 0.018(2) Uani 1 1 d . . . . . H3 H 0.305942 0.659777 0.590234 0.021 Uiso 1 1 calc R U . . . N7 N 0.3990(17) 0.3410(10) 0.4337(10) 0.023(3) Uani 1 1 d . . . . . H7 H 0.394644 0.266531 0.414470 0.027 Uiso 1 1 calc R U . . . N9 N 0.4819(15) 0.5271(8) 0.4416(9) 0.015(2) Uani 1 1 d . . . . . N11 N 0.7108(19) 1.1531(9) 0.5256(11) 0.028(3) Uani 1 1 d . . . . . N22 N 0.496(3) 1.0925(11) 0.6573(19) 0.074(8) Uani 1 1 d . . . . . H22A H 0.431957 1.036106 0.688958 0.089 Uiso 1 1 calc R U . . . H22B H 0.488866 1.164253 0.684848 0.089 Uiso 1 1 calc R U . . . N33 N 0.613(2) 0.9621(10) 0.5267(13) 0.039(4) Uani 1 1 d . . . . . H33 H 0.546563 0.905962 0.556168 0.047 Uiso 1 1 calc R U . . . N77 N 0.939(2) 0.9724(11) 0.3132(15) 0.052(5) Uani 1 1 d . . . . . H77 H 1.019676 1.006064 0.268794 0.062 Uiso 1 1 calc R U . . . N99 N 0.7693(16) 0.8359(8) 0.3903(10) 0.019(2) Uani 1 1 d . . . . . Cl1 Cl 0.3548(4) 0.7783(3) 0.3943(3) 0.0225(7) Uani 1 1 d . . . . . Cl2 Cl 0.6538(4) 0.7097(3) 0.6169(3) 0.0196(6) Uani 1 1 d . . . . . Cl3 Cl 0.9058(4) 0.5709(3) 0.4232(3) 0.0220(7) Uani 1 1 d . . . . . Cl4 Cl 0.6276(5) 0.6374(3) 0.2099(3) 0.0241(7) Uani 1 1 d . . . . . C2 C 0.148(2) 0.5527(12) 0.6692(14) 0.023(3) Uani 1 1 d . . . . . C4 C 0.3518(17) 0.5099(10) 0.5172(12) 0.016(3) Uani 1 1 d . . . . . C5 C 0.2913(19) 0.3961(12) 0.5158(12) 0.023(3) Uani 1 1 d . . . . . C6 C 0.1664(19) 0.3526(11) 0.5956(11) 0.016(3) Uani 1 1 d . . . . . C8 C 0.510(2) 0.4211(10) 0.3892(13) 0.020(3) Uani 1 1 d . . . . . H8 H 0.595876 0.406785 0.329883 0.023 Uiso 1 1 calc R U . . . C66 C 0.823(2) 1.1442(11) 0.4308(12) 0.022(3) Uani 1 1 d . . . . . C22 C 0.602(3) 1.0696(13) 0.5688(16) 0.047(5) Uani 1 1 d . . . . . C44 C 0.7291(19) 0.9379(12) 0.4376(13) 0.022(3) Uani 1 1 d . . . . . C55 C 0.830(2) 1.0282(11) 0.3942(14) 0.027(3) Uani 1 1 d . . . . . C88 C 0.899(2) 0.8613(12) 0.3149(16) 0.037(4) Uani 1 1 d . . . . . H88 H 0.956403 0.804653 0.267459 0.045 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 Ru1 0.0148(4) 0.0134(4) 0.0146(4) -0.0011(4) 0.0058(3) -0.0005(4) O6 0.036(6) 0.023(4) 0.024(5) 0.006(4) 0.003(4) -0.012(4) O66 0.036(6) 0.017(4) 0.031(5) 0.006(4) 0.018(5) -0.004(4) O1W 0.018(3) 0.017(3) 0.022(3) -0.002(2) 0.003(2) 0.001(2) O2W 0.0120(16) 0.0103(15) 0.0135(16) 0.0009(11) 0.0052(11) -0.0001(11) O3W 0.015(2) 0.0135(19) 0.017(2) -0.0011(17) 0.0057(18) -0.0018(17) N1 0.023(6) 0.021(5) 0.018(6) 0.008(4) 0.010(5) -0.001(5) N2 0.020(6) 0.037(7) 0.023(6) -0.012(5) 0.008(5) -0.001(5) N3 0.017(5) 0.021(5) 0.015(5) 0.000(4) 0.013(4) -0.006(4) N7 0.028(6) 0.015(5) 0.024(6) -0.002(4) 0.005(5) 0.003(4) N9 0.022(6) 0.011(4) 0.014(5) 0.001(4) 0.008(4) -0.002(4) N11 0.040(7) 0.014(5) 0.032(7) -0.004(5) 0.013(6) -0.010(5) N22 0.104(16) 0.019(6) 0.104(15) -0.026(8) 0.082(14) -0.020(8) N33 0.042(8) 0.022(6) 0.054(9) -0.012(6) 0.035(7) 0.000(6) N77 0.070(11) 0.023(6) 0.066(11) 0.002(7) 0.058(10) -0.005(7) N99 0.024(6) 0.009(4) 0.025(6) -0.004(4) 0.019(5) -0.004(4) Cl1 0.0162(15) 0.0194(13) 0.0323(18) 0.0097(13) 0.0063(13) 0.0032(12) Cl2 0.0224(17) 0.0239(14) 0.0128(15) -0.0019(13) 0.0053(12) -0.0057(14) Cl3 0.0153(15) 0.0287(15) 0.0221(16) -0.0027(12) 0.0034(13) 0.0060(12) Cl4 0.0370(19) 0.0191(16) 0.0163(15) 0.0018(13) 0.0001(14) -0.0033(15) C2 0.019(7) 0.023(7) 0.028(8) -0.008(6) -0.001(6) 0.003(5) C4 0.015(6) 0.016(5) 0.018(6) -0.002(5) -0.001(5) 0.005(5) C5 0.017(6) 0.030(6) 0.021(7) -0.002(6) 0.007(5) -0.004(6) C6 0.023(7) 0.011(5) 0.013(6) -0.001(5) -0.001(5) 0.002(5) C8 0.024(7) 0.012(5) 0.022(6) 0.004(5) 0.005(5) -0.003(5) C66 0.028(7) 0.019(6) 0.020(6) -0.008(5) 0.011(6) -0.010(5) C22 0.083(15) 0.023(7) 0.039(9) 0.001(7) 0.031(10) -0.010(8) C44 0.015(7) 0.026(7) 0.025(7) -0.004(5) 0.008(6) -0.001(5) C55 0.029(8) 0.018(6) 0.034(8) 0.004(6) 0.021(7) 0.002(6) C88 0.047(10) 0.020(6) 0.047(10) -0.002(7) 0.035(9) 0.004(6) _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 Ru1 N9 2.069(10) . ? Ru1 N99 2.094(10) . ? Ru1 Cl1 2.338(3) . ? Ru1 Cl3 2.346(3) . ? Ru1 Cl2 2.348(3) . ? Ru1 Cl4 2.367(3) . ? O6 C6 1.229(16) . ? O66 C66 1.213(15) . ? O1W O3W 1.745(12) . ? O2W O3W 1.711(13) . ? N1 C2 1.345(15) . ? N1 C6 1.399(17) . ? N1 H1 0.8800 . ? N2 C2 1.279(18) . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? N3 C2 1.340(18) . ? N3 C4 1.357(15) . ? N3 H3 0.8800 . ? N7 C8 1.334(17) . ? N7 C5 1.392(17) . ? N7 H7 0.8800 . ? N9 C4 1.317(16) . ? N9 C8 1.369(16) . ? N11 C22 1.345(19) . ? N11 C66 1.381(17) . ? N22 C22 1.32(2) . ? N22 H22A 0.8800 . ? N22 H22B 0.8800 . ? N33 C22 1.322(19) . ? N33 C44 1.369(17) . ? N33 H33 0.8800 . ? N77 C88 1.302(19) . ? N77 C55 1.391(17) . ? N77 H77 0.8800 . ? N99 C44 1.322(16) . ? N99 C88 1.330(17) . ? C4 C5 1.375(18) . ? C5 C6 1.399(18) . ? C8 H8 0.9500 . ? C66 C55 1.392(18) . ? C44 C55 1.369(18) . ? C88 H88 0.9500 . ? 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 N9 Ru1 N99 176.1(4) . . ? N9 Ru1 Cl1 87.8(3) . . ? N99 Ru1 Cl1 88.8(3) . . ? N9 Ru1 Cl3 91.0(3) . . ? N99 Ru1 Cl3 92.4(3) . . ? Cl1 Ru1 Cl3 176.84(14) . . ? N9 Ru1 Cl2 90.0(3) . . ? N99 Ru1 Cl2 88.3(3) . . ? Cl1 Ru1 Cl2 92.85(12) . . ? Cl3 Ru1 Cl2 90.10(12) . . ? N9 Ru1 Cl4 89.9(3) . . ? N99 Ru1 Cl4 92.0(3) . . ? Cl1 Ru1 Cl4 90.91(13) . . ? Cl3 Ru1 Cl4 86.14(12) . . ? Cl2 Ru1 Cl4 176.23(15) . . ? O2W O3W O1W 73.1(5) . . ? C2 N1 C6 125.7(10) . . ? C2 N1 H1 117.1 . . ? C6 N1 H1 117.1 . . ? C2 N2 H2A 120.0 . . ? C2 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C2 N3 C4 122.8(11) . . ? C2 N3 H3 118.6 . . ? C4 N3 H3 118.6 . . ? C8 N7 C5 108.0(11) . . ? C8 N7 H7 126.0 . . ? C5 N7 H7 126.0 . . ? C4 N9 C8 105.9(10) . . ? C4 N9 Ru1 128.4(8) . . ? C8 N9 Ru1 125.5(8) . . ? C22 N11 C66 127.4(12) . . ? C22 N22 H22A 120.0 . . ? C22 N22 H22B 120.0 . . ? H22A N22 H22B 120.0 . . ? C22 N33 C44 120.3(13) . . ? C22 N33 H33 119.9 . . ? C44 N33 H33 119.9 . . ? C88 N77 C55 107.8(12) . . ? C88 N77 H77 126.1 . . ? C55 N77 H77 126.1 . . ? C44 N99 C88 104.0(10) . . ? C44 N99 Ru1 126.7(8) . . ? C88 N99 Ru1 128.7(9) . . ? N2 C2 N3 120.8(13) . . ? N2 C2 N1 121.8(13) . . ? N3 C2 N1 117.4(11) . . ? N9 C4 N3 130.1(11) . . ? N9 C4 C5 111.9(11) . . ? N3 C4 C5 118.0(11) . . ? C4 C5 N7 104.3(11) . . ? C4 C5 C6 123.1(12) . . ? N7 C5 C6 132.1(12) . . ? O6 C6 N1 117.7(12) . . ? O6 C6 C5 129.4(12) . . ? N1 C6 C5 112.7(11) . . ? N7 C8 N9 109.9(11) . . ? N7 C8 H8 125.1 . . ? N9 C8 H8 125.1 . . ? O66 C66 N11 119.6(11) . . ? O66 C66 C55 131.0(12) . . ? N11 C66 C55 109.3(11) . . ? N22 C22 N33 120.5(14) . . ? N22 C22 N11 120.5(14) . . ? N33 C22 N11 118.8(14) . . ? N99 C44 C55 112.9(11) . . ? N99 C44 N33 129.1(12) . . ? C55 C44 N33 117.8(12) . . ? C44 C55 N77 102.6(11) . . ? C44 C55 C66 125.9(12) . . ? N77 C55 C66 131.4(12) . . ? N77 C88 N99 112.7(12) . . ? N77 C88 H88 123.7 . . ? N99 C88 H88 123.7 . . ? _refine_diff_density_max 2.867 _refine_diff_density_min -0.915 _refine_diff_density_rms 0.208 _shelx_res_file ; TITL compound_2.res in Pc compound_2.res created by SHELXL-2018/1 at 09:43:09 on 18-Jul-2022 REM SHELXT solution in Pc REM R1 0.084, Rweak 0.034, Alpha 0.015, Orientation as input REM Flack x = 0.172 ( 0.042 ) from Parsons' quotients REM Formula found by SHELXT: C18 Cl4 N5 O4 Ru CELL 0.71073 7.3191 11.4326 11.4016 90.000 91.643 90.000 ZERR 2.000 0.0006 0.0008 0.0010 0.000 0.003 0.000 LATT -1 SYMM X, -Y, 1/2+Z SFAC C H CL N O RU UNIT 20 22 8 20 10 2 ACTA TEMP -153.160 L.S. 4 BOND $H LIST 4 FMAP 2 PLAN 5 OMIT -1 0 0 OMIT -7 7 7 OMIT 0 1 -1 OMIT -1 3 2 OMIT 1 3 -2 ISOR 0.00045 O2w ISOR 0.003 O3w SIMU 0.001 O3w O2w O1w TWIN -1 0 0 0 -1 0 0 0 1 -4 WGHT 0.084700 5.491400 SWAT 0.382532 3.1238 BASF 0.00210 0.06998 0.00422 FVAR 0.61864 RU1 6 0.631889 0.677374 0.413639 11.00000 0.01481 0.01335 = 0.01460 -0.00105 0.00577 -0.00048 O6 5 0.117653 0.251184 0.612350 11.00000 0.03566 0.02261 = 0.02377 0.00553 0.00349 -0.01181 O66 5 0.893315 1.231613 0.391764 11.00000 0.03563 0.01715 = 0.03103 0.00627 0.01775 -0.00440 O1W 5 0.374689 0.819331 0.595816 11.00000 0.01845 0.01701 = 0.02213 -0.00177 0.00291 0.00064 O2W 5 0.308946 0.871930 0.762074 11.00000 0.01200 0.01026 = 0.01348 0.00090 0.00524 -0.00010 O3W 5 0.175898 0.890540 0.637581 11.00000 0.01481 0.01353 = 0.01739 -0.00110 0.00571 -0.00175 N1 4 0.101966 0.438907 0.670866 11.00000 0.02282 0.02104 = 0.01786 0.00770 0.01029 -0.00141 AFIX 43 H1 2 0.024151 0.416837 0.723970 11.00000 -1.20000 AFIX 0 N2 4 0.072293 0.627865 0.735019 11.00000 0.01955 0.03691 = 0.02336 -0.01170 0.00766 -0.00072 AFIX 93 H2A 2 0.101762 0.702290 0.730050 11.00000 -1.50000 H2B 2 -0.009578 0.605148 0.785264 11.00000 -1.50000 AFIX 0 N3 4 0.273376 0.585724 0.592224 11.00000 0.01734 0.02096 = 0.01527 0.00035 0.01279 -0.00551 AFIX 43 H3 2 0.305942 0.659777 0.590234 11.00000 -1.20000 AFIX 0 N7 4 0.399006 0.341050 0.433681 11.00000 0.02837 0.01538 = 0.02428 -0.00249 0.00547 0.00315 AFIX 43 H7 2 0.394644 0.266531 0.414470 11.00000 -1.20000 AFIX 0 N9 4 0.481907 0.527059 0.441594 11.00000 0.02247 0.01059 = 0.01362 0.00112 0.00833 -0.00155 N11 4 0.710807 1.153069 0.525611 11.00000 0.03981 0.01390 = 0.03157 -0.00356 0.01330 -0.00953 N22 4 0.495842 1.092526 0.657331 11.00000 0.10435 0.01868 = 0.10450 -0.02577 0.08190 -0.01963 AFIX 93 H22A 2 0.431957 1.036106 0.688958 11.00000 -1.20000 H22B 2 0.488866 1.164253 0.684848 11.00000 -1.20000 AFIX 0 N33 4 0.613459 0.962147 0.526731 11.00000 0.04229 0.02200 = 0.05420 -0.01160 0.03452 0.00045 AFIX 43 H33 2 0.546563 0.905962 0.556168 11.00000 -1.20000 AFIX 0 N77 4 0.938593 0.972369 0.313221 11.00000 0.07026 0.02311 = 0.06575 0.00172 0.05813 -0.00522 AFIX 43 H77 2 1.019676 1.006064 0.268794 11.00000 -1.20000 AFIX 0 N99 4 0.769346 0.835926 0.390255 11.00000 0.02422 0.00883 = 0.02487 -0.00380 0.01940 -0.00369 CL1 3 0.354841 0.778296 0.394324 11.00000 0.01622 0.01943 = 0.03227 0.00974 0.00628 0.00325 CL2 3 0.653770 0.709691 0.616883 11.00000 0.02236 0.02387 = 0.01284 -0.00195 0.00526 -0.00573 CL3 3 0.905835 0.570881 0.423220 11.00000 0.01530 0.02874 = 0.02211 -0.00273 0.00336 0.00597 CL4 3 0.627592 0.637352 0.209913 11.00000 0.03702 0.01909 = 0.01630 0.00177 0.00015 -0.00327 C2 1 0.148480 0.552691 0.669194 11.00000 0.01867 0.02317 = 0.02796 -0.00800 -0.00146 0.00331 C4 1 0.351835 0.509895 0.517188 11.00000 0.01549 0.01550 = 0.01820 -0.00223 -0.00067 0.00517 C5 1 0.291296 0.396052 0.515833 11.00000 0.01739 0.03011 = 0.02126 -0.00153 0.00663 -0.00401 C6 1 0.166436 0.352565 0.595593 11.00000 0.02295 0.01072 = 0.01277 -0.00080 -0.00083 0.00224 C8 1 0.510057 0.421141 0.389154 11.00000 0.02407 0.01235 = 0.02250 0.00403 0.00456 -0.00315 AFIX 43 H8 2 0.595876 0.406785 0.329883 11.00000 -1.20000 AFIX 0 C66 1 0.823251 1.144244 0.430781 11.00000 0.02837 0.01860 = 0.02039 -0.00840 0.01075 -0.00989 C22 1 0.601924 1.069612 0.568790 11.00000 0.08251 0.02258 = 0.03898 0.00120 0.03137 -0.01038 C44 1 0.729054 0.937922 0.437569 11.00000 0.01455 0.02608 = 0.02463 -0.00374 0.00800 -0.00076 C55 1 0.829835 1.028198 0.394212 11.00000 0.02894 0.01829 = 0.03386 0.00422 0.02052 0.00194 C88 1 0.898964 0.861345 0.314905 11.00000 0.04728 0.02014 = 0.04660 -0.00222 0.03479 0.00450 AFIX 43 H88 2 0.956403 0.804653 0.267459 11.00000 -1.20000 AFIX 0 HKLF 4 REM compound_2.res in Pc REM R1 = 0.0591 for 3106 Fo > 4sig(Fo) and 0.0634 for all 3302 data REM 276 parameters refined using 26 restraints END WGHT 0.0847 5.4914 REM Highest difference peak 2.867, deepest hole -0.915, 1-sigma level 0.208 Q1 1 0.3656 0.8758 0.8152 11.00000 0.05 2.87 Q2 1 0.1500 1.0228 0.5310 11.00000 0.05 2.18 Q3 1 0.1005 0.9192 0.5711 11.00000 0.05 1.92 Q4 1 0.2698 0.8647 0.7296 11.00000 0.05 1.77 Q5 1 0.8376 0.5888 0.3592 11.00000 0.05 1.01 ; _shelx_res_checksum 10016 _shelx_hkl_file ; -1 0 0 292.67 21.70 2 0 0 1970.90 132.09 -2 0 0 1897.21 131.79 3 0 0 3798.92 252.97 -3 0 0 3674.73 252.37 4 0 0 8028.80 521.65 -4 0 0 7539.65 520.35 5 0 0 291.47 30.70 -5 0 0 255.17 27.10 6 0 0 1018.40 80.39 7 0 0 1829.92 136.59 8 0 0 977.20 82.39 9 0 0 181.78 30.30 1 -1 0 243.18 21.90 -1 -1 0 312.47 21.50 -1 1 0 284.67 22.60 1 1 0 292.67 19.70 1 1 0 263.77 21.40 -2 -1 0 1168.78 82.79 2 -1 0 1274.67 86.59 2 1 0 1252.77 84.69 -2 1 0 1240.68 87.39 2 1 0 1207.98 84.49 3 -1 0 562.44 44.60 -3 -1 0 534.75 40.70 3 1 0 573.74 40.30 3 1 0 517.05 41.60 -3 1 0 554.44 44.60 -4 -1 0 519.95 43.30 4 -1 0 633.84 49.00 -4 1 0 596.64 46.70 4 1 0 528.95 43.40 4 1 0 513.95 39.80 5 -1 0 592.74 51.39 -5 1 0 490.35 47.50 5 1 0 637.74 48.00 6 -1 0 300.37 33.80 -6 1 0 309.57 34.90 6 1 0 280.37 30.90 7 -1 0 404.46 43.70 7 1 0 284.57 32.20 8 -1 0 309.67 39.90 8 1 0 299.57 36.10 9 -1 0 37.60 18.70 0 -2 0 504.55 33.60 0 -2 0 506.75 37.40 0 -2 0 468.65 35.20 0 2 0 505.55 36.90 0 2 0 467.15 35.20 0 2 0 486.45 33.10 1 -2 0 1621.54 106.89 1 -2 0 1473.05 106.99 -1 -2 0 1556.54 107.29 1 2 0 1449.85 98.69 1 2 0 1507.45 102.29 -1 2 0 1437.16 102.49 1 2 0 1507.65 97.99 2 -2 0 1179.28 90.89 2 -2 0 1293.07 88.49 -2 -2 0 1347.07 89.69 2 2 0 1399.76 85.79 -2 2 0 1067.39 89.89 2 2 0 1314.07 89.09 3 -2 0 2456.05 180.08 3 -2 0 2709.43 175.48 -3 -2 0 2616.94 176.98 -3 2 0 2237.98 165.48 3 2 0 2391.26 160.48 3 2 0 2482.55 162.48 4 -2 0 1684.43 113.69 4 -2 0 1640.94 121.49 4 2 0 1544.35 109.99 -4 2 0 1534.75 115.29 4 2 0 1637.24 110.29 5 -2 0 518.25 47.90 5 2 0 855.81 60.59 5 2 0 700.83 56.89 6 -2 0 258.47 32.20 -6 2 0 242.88 31.10 6 2 0 257.37 27.40 7 -2 0 410.46 45.40 -7 2 0 379.06 42.30 7 2 0 425.76 40.00 8 -2 0 176.68 30.50 8 2 0 210.88 29.70 9 -2 0 82.49 25.20 9 2 0 159.98 28.20 0 -3 0 1409.56 98.09 0 -3 0 1558.54 100.59 0 -3 0 1428.96 103.59 0 3 0 1457.15 95.59 0 3 0 1324.77 92.09 0 3 0 1339.57 97.19 1 -3 0 3861.61 275.17 1 -3 0 4239.48 276.37 -1 -3 0 4172.08 276.87 1 3 0 4009.50 252.57 1 3 0 3852.81 245.98 -1 3 0 3364.96 251.07 1 3 0 3650.43 247.68 -2 -3 0 8954.80 574.94 2 -3 0 7839.82 574.74 2 -3 0 9049.59 574.04 -2 3 0 7267.17 535.45 2 3 0 8165.78 528.85 2 3 0 8598.14 535.45 3 -3 0 3192.68 217.48 3 -3 0 3086.39 212.98 -3 -3 0 3120.49 214.48 -3 3 0 2722.63 197.58 3 3 0 2867.71 189.88 3 3 0 2903.21 195.08 4 -3 0 1714.63 123.19 4 -3 0 1616.64 115.79 4 3 0 1621.54 122.39 4 3 0 1835.32 119.89 5 -3 0 2708.33 188.68 5 -3 0 2870.91 199.48 5 3 0 2461.05 170.68 5 3 0 2559.54 172.18 -5 3 0 2405.56 178.58 6 -3 0 1193.08 95.99 -6 3 0 1106.09 90.29 7 -3 0 247.48 34.50 -7 3 0 329.07 39.00 7 3 0 368.96 35.20 8 -3 0 314.87 49.50 8 3 0 357.56 43.90 9 -3 0 605.04 63.39 9 3 0 664.83 60.79 0 -4 0 1190.48 87.09 0 -4 0 1320.27 92.69 0 -4 0 1257.57 84.59 0 4 0 1154.58 86.59 0 4 0 1218.08 80.29 0 4 0 1165.98 84.39 -1 -4 0 249.97 24.40 -1 -4 0 211.28 14.90 1 -4 0 196.98 17.10 1 -4 0 194.38 21.50 1 -4 0 232.68 23.60 1 4 0 216.88 19.60 1 4 0 217.78 23.30 -1 4 0 193.48 22.20 1 4 0 222.18 16.20 2 -4 0 565.04 46.70 2 -4 0 564.74 47.40 -2 -4 0 571.34 47.70 2 4 0 565.04 37.20 -2 4 0 513.85 45.60 2 4 0 501.85 44.30 3 -4 0 256.07 24.60 -3 -4 0 198.88 24.30 3 -4 0 232.48 27.20 3 4 0 165.58 21.80 -3 4 0 238.88 28.10 3 4 0 215.88 16.90 4 -4 0 14.90 7.00 -4 -4 0 16.20 8.00 4 -4 0 12.30 10.20 4 4 0 18.60 5.50 -4 4 0 10.80 10.10 4 4 0 18.50 9.10 5 -4 0 180.68 26.30 5 -4 0 152.18 18.50 5 4 0 183.58 21.60 -5 4 0 140.29 24.80 5 4 0 178.38 18.00 6 -4 0 228.38 31.90 -6 4 0 197.08 28.40 6 4 0 153.18 19.00 7 -4 0 62.59 19.80 7 4 0 65.29 14.50 -7 4 0 64.89 19.50 8 -4 0 89.29 26.10 8 4 0 128.09 21.20 9 -4 0 203.18 36.90 9 4 0 202.28 29.80 0 -5 0 173.78 14.60 0 -5 0 175.18 22.90 0 -5 0 186.98 17.90 0 5 0 165.68 20.30 0 5 0 167.28 18.90 0 5 0 158.08 13.90 1 -5 0 1878.21 132.79 -1 -5 0 1869.41 125.69 1 -5 0 1827.92 127.79 1 -5 0 1897.91 136.29 -1 -5 0 1894.61 125.49 -1 -5 0 1962.70 137.19 1 5 0 1866.01 123.49 -1 5 0 1746.63 130.99 1 5 0 1886.11 133.09 1 5 0 1856.21 127.89 -2 -5 0 2722.73 186.68 2 -5 0 2717.03 185.68 2 -5 0 2587.64 178.18 2 -5 0 2520.75 184.08 2 5 0 2454.75 166.78 2 5 0 2305.07 155.98 -2 5 0 2260.17 165.98 -3 -5 0 310.77 32.60 3 -5 0 309.17 31.70 3 -5 0 333.97 34.20 -3 5 0 260.47 31.90 3 5 0 327.27 23.20 3 5 0 298.87 31.40 4 -5 0 397.66 41.80 4 -5 0 388.46 37.80 -4 -5 0 473.55 41.40 4 5 0 456.65 43.80 4 5 0 509.95 36.70 5 -5 0 759.22 67.39 5 -5 0 746.63 59.99 -5 5 0 602.44 62.39 5 5 0 769.92 53.19 5 5 0 733.63 60.89 6 -5 0 596.44 58.29 6 -5 0 569.74 49.40 6 5 0 666.43 49.50 -6 5 0 554.64 58.39 7 -5 0 74.89 23.40 7 5 0 170.88 25.60 8 -5 0 33.20 18.30 8 5 0 114.59 19.40 0 -6 0 339.17 27.90 0 -6 0 292.87 34.00 0 -6 0 321.97 24.50 0 6 0 316.27 30.50 0 6 0 306.47 24.30 0 6 0 314.17 32.60 1 -6 0 2269.37 150.48 -1 -6 0 2216.08 161.28 -1 -6 0 2177.28 147.69 -1 -6 0 2104.59 148.19 1 -6 0 2288.97 161.48 1 -6 0 2287.07 155.88 -1 6 0 1976.90 145.59 1 6 0 1983.80 142.19 1 6 0 2094.29 136.69 1 6 0 2062.19 153.78 -2 -6 0 822.72 78.19 2 -6 0 938.11 73.19 -2 6 0 881.81 72.59 2 6 0 929.61 61.79 2 6 0 849.72 76.89 3 -6 0 878.11 72.09 -3 -6 0 791.22 74.49 3 -6 0 919.31 72.39 3 -6 0 906.71 64.69 3 6 0 790.62 53.59 -3 6 0 728.53 65.19 3 6 0 761.02 64.39 -4 -6 0 430.06 43.60 4 -6 0 465.95 45.40 4 -6 0 409.36 41.60 -4 6 0 394.06 42.50 4 6 0 412.76 40.70 4 6 0 411.26 30.90 -5 -6 0 1579.84 112.49 5 -6 0 1333.67 107.09 5 -6 0 1395.76 113.29 -5 6 0 1178.18 108.29 5 6 0 1513.25 96.79 5 6 0 1403.56 107.09 6 -6 0 471.55 51.59 6 6 0 436.66 36.10 -6 6 0 395.16 46.90 7 -6 0 198.98 21.90 7 -6 0 188.88 33.00 7 6 0 250.07 25.70 8 -6 0 77.99 24.00 8 6 0 164.48 22.50 0 -7 0 24.60 10.60 0 -7 0 38.60 6.50 0 -7 0 42.40 9.60 0 7 0 26.10 10.20 0 7 0 48.20 8.90 0 7 0 70.69 16.50 -1 -7 0 617.74 58.89 1 -7 0 665.73 53.19 -1 -7 0 640.94 45.20 1 -7 0 670.93 59.99 -1 -7 0 657.33 44.70 1 -7 0 647.34 47.70 1 7 0 600.64 49.80 1 7 0 607.04 42.90 -1 7 0 582.24 52.29 1 7 0 570.64 53.59 2 -7 0 67.89 16.70 -2 -7 0 83.99 21.40 2 -7 0 57.49 17.60 2 -7 0 51.79 9.90 2 7 0 73.69 8.50 -2 7 0 50.39 15.60 2 7 0 73.49 20.60 3 -7 0 178.48 19.30 3 -7 0 190.38 26.70 -3 -7 0 212.88 28.40 3 -7 0 170.78 26.20 3 7 0 183.68 25.50 3 7 0 161.98 14.30 -3 7 0 160.38 24.90 -4 -7 0 144.19 24.30 4 -7 0 113.59 19.90 4 -7 0 88.59 13.90 4 -7 0 67.49 20.10 4 7 0 182.18 15.60 4 7 0 129.89 24.40 5 -7 0 367.36 40.50 5 -7 0 430.56 45.40 -5 -7 0 372.16 42.70 -5 7 0 347.57 41.10 5 7 0 358.96 29.00 6 -7 0 39.40 16.70 6 7 0 57.29 11.30 7 -7 0 20.50 11.80 7 -7 0 24.00 17.60 7 7 0 67.09 13.20 8 -7 0 138.59 32.90 8 7 0 275.07 28.50 0 -8 0 343.37 27.20 0 -8 0 372.66 41.90 0 -8 0 347.47 30.40 0 8 0 318.57 34.30 1 -8 0 1218.28 96.39 -1 -8 0 1102.79 77.99 1 -8 0 1166.88 81.39 -1 -8 0 1187.38 96.39 -1 -8 0 1130.19 77.69 1 8 0 1127.19 76.29 1 8 0 1006.50 88.19 1 8 0 1161.48 85.29 -1 8 0 1029.60 86.69 2 -8 0 535.55 47.00 2 -8 0 471.25 39.40 2 -8 0 469.45 50.79 -2 -8 0 542.05 52.79 -2 8 0 456.15 47.30 2 8 0 501.05 35.70 2 8 0 447.36 48.00 3 -8 0 359.96 39.00 3 -8 0 371.96 41.20 3 -8 0 351.66 30.90 -3 -8 0 315.37 40.60 3 8 0 322.17 24.40 3 8 0 284.67 35.80 -3 8 0 291.57 36.50 4 -8 0 415.56 46.60 -4 -8 0 487.75 50.39 4 -8 0 426.56 38.30 4 -8 0 460.25 47.80 4 8 0 439.36 33.80 4 8 0 466.05 47.70 5 -8 0 168.58 28.50 -5 -8 0 255.77 34.20 5 -8 0 189.08 31.30 5 8 0 328.87 33.30 6 -8 0 100.49 26.50 6 -8 0 79.79 20.70 6 8 0 152.58 19.30 7 -8 0 116.09 24.40 7 8 0 231.48 23.80 0 -9 0 810.92 58.39 0 -9 0 767.02 75.09 0 -9 0 857.41 61.79 0 9 0 772.72 67.29 0 9 0 776.22 57.19 1 -9 0 66.09 21.40 1 -9 0 78.59 17.00 1 -9 0 74.09 16.80 -1 -9 0 102.89 24.90 1 9 0 100.29 22.70 -1 9 0 80.49 20.80 -2 -9 0 42.70 19.30 2 -9 0 19.20 7.40 2 -9 0 15.20 10.30 2 -9 0 23.40 15.00 -2 9 0 18.10 11.20 2 9 0 26.20 6.70 2 9 0 11.50 9.80 -3 -9 0 305.57 38.40 3 -9 0 198.38 29.30 3 -9 0 235.58 23.90 3 -9 0 221.88 33.90 3 9 0 233.18 33.80 3 9 0 271.17 22.10 4 -9 0 718.53 58.19 -4 -9 0 712.43 71.99 4 -9 0 816.82 69.19 4 -9 0 693.23 68.69 4 9 0 771.12 55.79 5 -9 0 22.60 13.90 -5 -9 0 11.40 14.50 5 -9 0 29.30 16.60 5 9 0 22.90 6.90 6 -9 0 36.10 20.20 6 -9 0 48.10 19.50 6 9 0 90.19 12.80 7 -9 0 117.09 29.30 7 -9 0 146.69 29.90 7 9 0 272.97 25.70 0 -10 0 63.09 25.80 0 -10 0 63.69 12.50 0 -10 0 46.00 8.40 0 10 0 79.29 21.10 1 -10 0 168.88 17.60 1 -10 0 183.38 22.60 1 -10 0 165.48 37.10 -1 -10 0 141.09 34.60 1 10 0 115.19 14.40 -1 10 0 176.68 26.70 1 10 0 119.39 23.40 -2 -10 0 4.60 12.20 2 -10 0 2.10 5.20 2 -10 0 1.10 9.30 2 -10 0 4.80 13.20 2 10 0 -0.10 4.40 -3 -10 0 141.79 33.40 3 -10 0 88.09 15.80 3 -10 0 111.99 32.60 3 -10 0 93.19 23.20 -3 10 0 68.59 21.70 4 -10 0 23.00 15.50 4 -10 0 12.90 16.20 -4 -10 0 9.90 14.00 -5 -10 0 23.40 16.10 5 -10 0 26.00 16.50 5 -10 0 20.00 15.90 5 10 0 7.70 6.90 -6 -10 0 65.29 25.80 6 -10 0 36.70 18.80 6 -10 0 35.60 17.90 6 10 0 81.19 12.30 0 -11 0 665.13 72.19 0 -11 0 710.93 52.39 0 -11 0 679.93 50.29 0 11 0 687.53 64.69 1 -11 0 213.48 39.10 1 -11 0 218.58 21.60 -1 -11 0 250.37 39.30 1 -11 0 228.58 25.80 1 11 0 182.18 19.50 -1 11 0 217.08 34.10 2 -11 0 91.49 20.80 2 -11 0 65.19 22.90 -2 -11 0 64.79 23.40 2 -11 0 84.19 13.90 -2 11 0 70.99 23.20 2 11 0 102.79 13.30 3 -11 0 595.94 58.09 3 -11 0 534.35 64.89 3 -11 0 638.44 55.69 -3 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