# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound1 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common 'diperchlorato-(2,6-bis([(2-pyridylmethyl)amino]methyl)pyridine) mercury(ii)' _chemical_melting_point ? _chemical_formula_moiety 'C19 H21 Cl2 Hg N5 O8' _chemical_formula_sum 'C19 H21 Cl2 Hg N5 O8' _chemical_formula_weight 718.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -4.2923 7.6849 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1045(3) _cell_length_b 27.3639(9) _cell_length_c 9.5438(3) _cell_angle_alpha 90 _cell_angle_beta 94.719(2) _cell_angle_gamma 90 _cell_volume 2369.63(13) _cell_formula_units_Z 4 _cell_measurement_temperature 297(2) _cell_measurement_reflns_used 7451 _cell_measurement_theta_min 5.14 _cell_measurement_theta_max 58.86 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.015 _exptl_crystal_F_000 1392 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.090 _exptl_absorpt_coefficient_mu 14.230 _shelx_estimated_absorpt_T_min 0.241 _shelx_estimated_absorpt_T_max 0.361 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2406 _exptl_absorpt_correction_T_max 0.3608 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 297(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\w and \y' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 34367 _diffrn_reflns_av_unetI/netI 0.0155 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.230 _diffrn_reflns_theta_max 58.938 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.776 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_Laue_measured_fraction_full 0.776 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_point_group_measured_fraction_full 0.776 _reflns_number_total 3327 _reflns_number_gt 3128 _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 'APEX2 (Bruker AXS, 2004)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2004)' _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXLE (Hubschle, 2011)' _computing_publication_material 'Mercury 3.1 (CCDC, 2013)' _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^)+(0.0340P)^2^+6.2649P] 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 3327 _refine_ls_number_parameters 376 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.044 _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 Hg1 Hg 0.23039(2) 0.12368(2) 0.13922(2) 0.05090(11) Uani 1 1 d . . . . . N1 N 0.3174(5) 0.20634(15) 0.1340(5) 0.0534(11) Uani 1 1 d . . . . . N2 N 0.3931(5) 0.12986(16) -0.0442(5) 0.0577(12) Uani 1 1 d . . . . . H2N H 0.3505 0.1108 -0.1246 0.069 Uiso 1 1 calc R U . . . N3 N 0.4030(5) 0.06222(15) 0.1683(5) 0.0527(11) Uani 1 1 d . . . . . N4 N 0.1303(6) 0.05576(19) 0.2674(6) 0.0743(14) Uani 1 1 d . . . . . H4N H 0.0822 0.0343 0.1954 0.089 Uiso 1 1 calc R U . . . N5 N 0.0051(5) 0.14689(17) 0.2048(5) 0.0541(11) Uani 1 1 d . . . . . C1 C 0.3047(7) 0.2385(2) 0.2372(6) 0.0658(16) Uani 1 1 d . . . . . H1 H 0.2461 0.2306 0.3093 0.079 Uiso 1 1 calc R U . . . C2 C 0.3745(7) 0.2825(2) 0.2407(7) 0.0698(17) Uani 1 1 d . . . . . H2 H 0.3611 0.3049 0.3120 0.084 Uiso 1 1 calc R U . . . C3 C 0.4653(7) 0.2933(2) 0.1369(7) 0.0661(16) Uani 1 1 d . . . . . H3 H 0.5166 0.3227 0.1378 0.079 Uiso 1 1 calc R U . . . C4 C 0.4786(6) 0.2599(2) 0.0319(6) 0.0592(14) Uani 1 1 d . . . . . H4 H 0.5398 0.2664 -0.0392 0.071 Uiso 1 1 calc R U . . . C5 C 0.4015(6) 0.21665(19) 0.0315(5) 0.0484(12) Uani 1 1 d . . . . . C6 C 0.4028(7) 0.1809(2) -0.0891(6) 0.0648(15) Uani 1 1 d . . . . . H6A H 0.3204 0.1880 -0.1571 0.078 Uiso 1 1 calc R U . . . H6B H 0.4928 0.1853 -0.1354 0.078 Uiso 1 1 calc R U . . . C7 C 0.5359(7) 0.1080(2) 0.0030(7) 0.0677(16) Uani 1 1 d . . . . . H7A H 0.5978 0.1328 0.0504 0.081 Uiso 1 1 calc R U . . . H7B H 0.5839 0.0972 -0.0786 0.081 Uiso 1 1 calc R U . . . C8 C 0.5239(6) 0.0654(2) 0.1004(6) 0.0571(14) Uani 1 1 d . . . . . C9 C 0.6361(7) 0.0307(2) 0.1251(7) 0.0732(18) Uani 1 1 d . . . . . H9 H 0.7215 0.0324 0.0780 0.088 Uiso 1 1 calc R U . . . C10 C 0.6172(8) -0.0057(2) 0.2202(8) 0.080(2) Uani 1 1 d . . . . . H10 H 0.6910 -0.0289 0.2388 0.096 Uiso 1 1 calc R U . . . C11 C 0.4904(8) -0.0085(2) 0.2883(7) 0.0736(18) Uani 1 1 d . . . . . H11 H 0.4770 -0.0336 0.3517 0.088 Uiso 1 1 calc R U . . . C12 C 0.3833(7) 0.02657(19) 0.2611(6) 0.0593(15) Uani 1 1 d . . . . . C13 C 0.2452(7) 0.0273(2) 0.3371(7) 0.0686(17) Uani 1 1 d . . . . . H13A H 0.2105 -0.0059 0.3467 0.082 Uiso 1 1 calc R U . . . H13B H 0.2681 0.0403 0.4309 0.082 Uiso 1 1 calc R U . . . C14 C 0.0143(7) 0.0726(2) 0.3496(7) 0.0731(17) Uani 1 1 d . . . . . H14A H 0.0554 0.0783 0.4452 0.088 Uiso 1 1 calc R U . . . H14B H -0.0590 0.0470 0.3525 0.088 Uiso 1 1 calc R U . . . C15 C -0.0615(7) 0.1190(2) 0.2946(6) 0.0586(15) Uani 1 1 d . . . . . C16 C -0.1957(7) 0.1335(3) 0.3394(7) 0.0719(18) Uani 1 1 d . . . . . H16 H -0.2427 0.1140 0.4019 0.086 Uiso 1 1 calc R U . . . C17 C -0.2591(7) 0.1762(3) 0.2921(8) 0.0773(19) Uani 1 1 d . . . . . H17 H -0.3491 0.1859 0.3225 0.093 Uiso 1 1 calc R U . . . C18 C -0.1906(7) 0.2045(2) 0.2007(7) 0.0706(17) Uani 1 1 d . . . . . H18 H -0.2319 0.2339 0.1678 0.085 Uiso 1 1 calc R U . . . C19 C -0.0592(6) 0.1887(2) 0.1585(6) 0.0610(15) Uani 1 1 d . . . . . H19 H -0.0121 0.2076 0.0949 0.073 Uiso 1 1 calc R U . . . Cl1A Cl 0.39942(18) 0.15006(5) 0.53352(15) 0.0652(4) Uani 0.72(2) 1 d D . P A 1 O1A O 0.4381(8) 0.1314(2) 0.4092(6) 0.139(3) Uani 0.72(2) 1 d D . P A 1 O2A O 0.2506(9) 0.1603(5) 0.5006(16) 0.222(10) Uani 0.72(2) 1 d D . P A 1 O3A O 0.413(2) 0.1176(4) 0.6377(12) 0.193(11) Uani 0.72(2) 1 d D . P A 1 O4A O 0.4675(15) 0.1936(3) 0.5621(11) 0.119(5) Uani 0.72(2) 1 d D . P A 1 Cl1B Cl 0.39942(18) 0.15006(5) 0.53352(15) 0.0652(4) Uani 0.28(2) 1 d D . P A 2 O1B O 0.4381(8) 0.1314(2) 0.4092(6) 0.139(3) Uani 0.28(2) 1 d D . P A 2 O2B O 0.322(7) 0.1926(13) 0.539(4) 0.24(3) Uani 0.28(2) 1 d D . P A 2 O3B O 0.537(3) 0.164(3) 0.597(3) 0.30(4) Uani 0.28(2) 1 d D . P A 2 O4B O 0.344(4) 0.1206(9) 0.634(2) 0.104(12) Uani 0.28(2) 1 d D . P A 2 Cl2A Cl -0.01220(17) 0.07947(5) -0.16350(16) 0.0662(4) Uani 0.56(3) 1 d D . P A 1 O5A O 0.0657(7) 0.12181(19) -0.1268(6) 0.111(2) Uani 0.56(3) 1 d D . P A 1 O6A O -0.020(3) 0.0728(7) -0.3028(11) 0.164(12) Uani 0.56(3) 1 d D . P A 1 O7A O 0.071(2) 0.0429(6) -0.094(2) 0.172(10) Uani 0.56(3) 1 d D . P A 1 O8A O -0.1423(19) 0.0796(9) -0.110(3) 0.202(12) Uani 0.56(3) 1 d D . P A 1 Cl2B Cl -0.01220(17) 0.07947(5) -0.16350(16) 0.0662(4) Uani 0.44(3) 1 d D . P A 2 O5B O 0.0657(7) 0.12181(19) -0.1268(6) 0.111(2) Uani 0.44(3) 1 d D . P A 2 O6B O 0.046(3) 0.0592(10) -0.276(3) 0.201(16) Uani 0.44(3) 1 d D . P A 2 O7B O -0.015(4) 0.0480(9) -0.057(2) 0.180(15) Uani 0.44(3) 1 d D . P A 2 O8B O -0.1567(16) 0.0933(6) -0.213(4) 0.152(14) Uani 0.44(3) 1 d D . P A 2 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 Hg1 0.05682(17) 0.04524(16) 0.05166(16) 0.00478(9) 0.01059(10) 0.00109(9) N1 0.068(3) 0.044(2) 0.050(3) 0.001(2) 0.017(2) -0.006(2) N2 0.073(3) 0.055(3) 0.046(3) -0.012(2) 0.008(2) -0.005(2) N3 0.059(3) 0.042(2) 0.056(3) -0.010(2) -0.004(2) 0.003(2) N4 0.078(4) 0.064(3) 0.081(4) 0.019(3) 0.012(3) -0.001(3) N5 0.053(3) 0.057(3) 0.054(3) 0.000(2) 0.011(2) 0.000(2) C1 0.087(4) 0.057(4) 0.057(4) -0.008(3) 0.027(3) -0.005(3) C2 0.098(5) 0.053(4) 0.059(4) -0.009(3) 0.013(3) 0.002(3) C3 0.077(4) 0.053(4) 0.068(4) 0.000(3) 0.007(3) -0.009(3) C4 0.062(3) 0.061(4) 0.055(3) 0.011(3) 0.011(3) -0.006(3) C5 0.059(3) 0.047(3) 0.039(3) 0.008(2) 0.008(2) 0.001(2) C6 0.089(4) 0.063(4) 0.046(3) 0.000(3) 0.019(3) -0.006(3) C7 0.069(4) 0.067(4) 0.068(4) -0.013(3) 0.014(3) -0.004(3) C8 0.057(3) 0.052(3) 0.062(3) -0.019(3) -0.004(3) -0.002(3) C9 0.062(4) 0.068(4) 0.088(5) -0.031(4) -0.004(3) 0.005(3) C10 0.080(5) 0.054(4) 0.101(5) -0.020(4) -0.018(4) 0.017(3) C11 0.090(5) 0.047(3) 0.082(4) -0.006(3) -0.012(4) 0.008(3) C12 0.073(4) 0.040(3) 0.061(4) -0.009(3) -0.012(3) 0.001(3) C13 0.087(5) 0.046(3) 0.072(4) 0.009(3) 0.002(3) -0.008(3) C14 0.086(4) 0.067(4) 0.070(4) 0.011(3) 0.027(3) -0.006(3) C15 0.063(4) 0.059(4) 0.055(3) -0.005(3) 0.013(3) -0.011(3) C16 0.064(4) 0.078(5) 0.077(4) -0.012(4) 0.022(3) -0.018(3) C17 0.050(4) 0.085(5) 0.098(5) -0.020(4) 0.013(3) -0.001(3) C18 0.056(4) 0.069(4) 0.085(4) -0.011(4) -0.002(3) 0.007(3) C19 0.057(4) 0.063(4) 0.062(4) 0.000(3) 0.003(3) 0.000(3) Cl1A 0.0841(10) 0.0622(9) 0.0511(8) -0.0045(7) 0.0173(7) 0.0067(8) O1A 0.183(7) 0.146(6) 0.097(4) -0.067(4) 0.065(4) -0.063(5) O2A 0.085(7) 0.171(14) 0.41(3) 0.155(15) 0.036(9) 0.024(7) O3A 0.40(3) 0.093(9) 0.084(9) 0.026(7) 0.004(12) 0.100(13) O4A 0.208(14) 0.048(5) 0.099(7) -0.023(4) -0.004(8) -0.022(6) Cl1B 0.0841(10) 0.0622(9) 0.0511(8) -0.0045(7) 0.0173(7) 0.0067(8) O1B 0.183(7) 0.146(6) 0.097(4) -0.067(4) 0.065(4) -0.063(5) O2B 0.44(8) 0.12(3) 0.18(3) 0.08(2) 0.19(4) 0.20(4) O3B 0.12(3) 0.70(11) 0.08(2) -0.14(4) 0.053(19) -0.17(5) O4B 0.20(3) 0.086(19) 0.033(11) 0.013(10) 0.028(11) -0.089(19) Cl2A 0.0705(10) 0.0580(9) 0.0705(10) 0.0033(7) 0.0083(8) -0.0016(7) O5A 0.129(5) 0.101(4) 0.100(4) 0.011(3) -0.017(4) -0.032(3) O6A 0.26(3) 0.179(15) 0.049(7) -0.016(8) 0.000(10) -0.138(17) O7A 0.212(18) 0.115(11) 0.20(2) 0.073(11) 0.079(14) 0.099(12) O8A 0.090(12) 0.30(3) 0.23(3) 0.02(2) 0.087(14) -0.004(15) Cl2B 0.0705(10) 0.0580(9) 0.0705(10) 0.0033(7) 0.0083(8) -0.0016(7) O5B 0.129(5) 0.101(4) 0.100(4) 0.011(3) -0.017(4) -0.032(3) O6B 0.129(16) 0.33(4) 0.15(3) -0.08(2) 0.062(15) 0.070(19) O7B 0.28(4) 0.15(2) 0.118(14) 0.066(14) 0.05(2) -0.03(2) O8B 0.052(9) 0.097(12) 0.30(4) 0.034(16) -0.015(15) -0.016(7) _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 Hg1 N5 2.283(4) . ? Hg1 N3 2.303(4) . ? Hg1 N2 2.391(5) . ? Hg1 N1 2.398(4) . ? Hg1 N4 2.442(5) . ? Hg1 O5A 2.841(6) . ? Hg1 O1A 3.075(7) . ? N1 C5 1.322(6) . ? N1 C1 1.333(7) . ? N2 C6 1.465(7) . ? N2 C7 1.469(8) . ? N2 H2N 0.9800 . ? N3 C8 1.325(7) . ? N3 C12 1.340(7) . ? N4 C13 1.424(8) . ? N4 C14 1.442(8) . ? N4 H4N 0.9800 . ? N5 C15 1.331(7) . ? N5 C19 1.343(7) . ? C1 C2 1.361(8) . ? C1 H1 0.9300 . ? C2 C3 1.374(9) . ? C2 H2 0.9300 . ? C3 C4 1.369(8) . ? C3 H3 0.9300 . ? C4 C5 1.376(8) . ? C4 H4 0.9300 . ? C5 C6 1.512(8) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.499(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.401(8) . ? C9 C10 1.369(10) . ? C9 H9 0.9300 . ? C10 C11 1.373(10) . ? C10 H10 0.9300 . ? C11 C12 1.377(8) . ? C11 H11 0.9300 . ? C12 C13 1.503(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.517(8) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.385(9) . ? C16 C17 1.365(9) . ? C16 H16 0.9300 . ? C17 C18 1.356(9) . ? C17 H17 0.9300 . ? C18 C19 1.364(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? Cl1A O3A 1.331(9) . ? Cl1A O4A 1.359(7) . ? Cl1A O1A 1.365(5) . ? Cl1A O2A 1.394(8) . ? Cl2A O8A 1.328(12) . ? Cl2A O6A 1.338(11) . ? Cl2A O5A 1.388(5) . ? Cl2A O7A 1.394(12) . ? 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 N5 Hg1 N3 142.15(17) . . ? N5 Hg1 N2 143.70(17) . . ? N3 Hg1 N2 71.46(16) . . ? N5 Hg1 N1 92.81(16) . . ? N3 Hg1 N1 117.89(15) . . ? N2 Hg1 N1 72.09(14) . . ? N5 Hg1 N4 72.15(17) . . ? N3 Hg1 N4 70.32(17) . . ? N2 Hg1 N4 134.43(17) . . ? N1 Hg1 N4 149.93(17) . . ? N5 Hg1 O5A 80.21(18) . . ? N3 Hg1 O5A 113.55(17) . . ? N2 Hg1 O5A 70.14(18) . . ? N1 Hg1 O5A 98.60(15) . . ? N4 Hg1 O5A 104.04(17) . . ? N5 Hg1 O1A 104.80(16) . . ? N3 Hg1 O1A 65.33(16) . . ? N2 Hg1 O1A 103.48(16) . . ? N1 Hg1 O1A 76.76(16) . . ? N4 Hg1 O1A 82.06(18) . . ? O5A Hg1 O1A 173.19(16) . . ? C5 N1 C1 119.8(5) . . ? C5 N1 Hg1 115.4(3) . . ? C1 N1 Hg1 124.0(4) . . ? C6 N2 C7 113.9(5) . . ? C6 N2 Hg1 109.7(3) . . ? C7 N2 Hg1 109.4(3) . . ? C6 N2 H2N 107.9 . . ? C7 N2 H2N 107.9 . . ? Hg1 N2 H2N 107.9 . . ? C8 N3 C12 122.2(5) . . ? C8 N3 Hg1 118.6(4) . . ? C12 N3 Hg1 119.0(4) . . ? C13 N4 C14 117.6(5) . . ? C13 N4 Hg1 111.1(4) . . ? C14 N4 Hg1 110.4(4) . . ? C13 N4 H4N 105.6 . . ? C14 N4 H4N 105.6 . . ? Hg1 N4 H4N 105.6 . . ? C15 N5 C19 119.4(5) . . ? C15 N5 Hg1 118.9(4) . . ? C19 N5 Hg1 121.6(4) . . ? N1 C1 C2 122.3(5) . . ? N1 C1 H1 118.9 . . ? C2 C1 H1 118.9 . . ? C1 C2 C3 118.7(6) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 118.7(6) . . ? C4 C3 H3 120.7 . . ? C2 C3 H3 120.7 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C5 C4 120.6(5) . . ? N1 C5 C6 117.8(5) . . ? C4 C5 C6 121.5(5) . . ? N2 C6 C5 113.0(4) . . ? N2 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? N2 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N2 C7 C8 113.5(5) . . ? N2 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N2 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? N3 C8 C9 119.8(6) . . ? N3 C8 C7 117.4(5) . . ? C9 C8 C7 122.8(6) . . ? C10 C9 C8 118.4(6) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C9 C10 C11 120.7(6) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 118.9(7) . . ? C10 C11 H11 120.6 . . ? C12 C11 H11 120.6 . . ? N3 C12 C11 120.0(6) . . ? N3 C12 C13 118.2(5) . . ? C11 C12 C13 121.8(6) . . ? N4 C13 C12 113.2(5) . . ? N4 C13 H13A 108.9 . . ? C12 C13 H13A 108.9 . . ? N4 C13 H13B 108.9 . . ? C12 C13 H13B 108.9 . . ? H13A C13 H13B 107.8 . . ? N4 C14 C15 114.3(5) . . ? N4 C14 H14A 108.7 . . ? C15 C14 H14A 108.7 . . ? N4 C14 H14B 108.7 . . ? C15 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? N5 C15 C16 119.6(6) . . ? N5 C15 C14 119.0(5) . . ? C16 C15 C14 121.3(6) . . ? C17 C16 C15 120.2(6) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 119.9(6) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C17 C18 C19 118.0(6) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? N5 C19 C18 122.9(6) . . ? N5 C19 H19 118.6 . . ? C18 C19 H19 118.6 . . ? O3A Cl1A O4A 115.0(7) . . ? O3A Cl1A O1A 112.7(6) . . ? O4A Cl1A O1A 110.8(5) . . ? O3A Cl1A O2A 109.3(8) . . ? O4A Cl1A O2A 106.7(6) . . ? O1A Cl1A O2A 101.2(7) . . ? Cl1A O1A Hg1 124.7(5) . . ? O8A Cl2A O6A 113.9(10) . . ? O8A Cl2A O5A 110.7(9) . . ? O6A Cl2A O5A 110.5(6) . . ? O8A Cl2A O7A 106.6(10) . . ? O6A Cl2A O7A 111.1(10) . . ? O5A Cl2A O7A 103.4(9) . . ? Cl2A O5A Hg1 117.5(3) . . ? 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 C5 N1 C1 C2 0.8(9) . . . . ? Hg1 N1 C1 C2 169.8(5) . . . . ? N1 C1 C2 C3 -2.3(10) . . . . ? C1 C2 C3 C4 1.8(10) . . . . ? C2 C3 C4 C5 0.3(9) . . . . ? C1 N1 C5 C4 1.4(8) . . . . ? Hg1 N1 C5 C4 -168.5(4) . . . . ? C1 N1 C5 C6 -175.1(5) . . . . ? Hg1 N1 C5 C6 15.0(6) . . . . ? C3 C4 C5 N1 -1.9(8) . . . . ? C3 C4 C5 C6 174.5(5) . . . . ? C7 N2 C6 C5 -85.5(6) . . . . ? Hg1 N2 C6 C5 37.6(6) . . . . ? N1 C5 C6 N2 -36.6(7) . . . . ? C4 C5 C6 N2 147.0(5) . . . . ? C6 N2 C7 C8 156.5(5) . . . . ? Hg1 N2 C7 C8 33.2(6) . . . . ? C12 N3 C8 C9 0.0(8) . . . . ? Hg1 N3 C8 C9 174.8(4) . . . . ? C12 N3 C8 C7 -177.8(5) . . . . ? Hg1 N3 C8 C7 -3.0(6) . . . . ? N2 C7 C8 N3 -21.6(7) . . . . ? N2 C7 C8 C9 160.7(5) . . . . ? N3 C8 C9 C10 -0.2(8) . . . . ? C7 C8 C9 C10 177.4(6) . . . . ? C8 C9 C10 C11 0.8(9) . . . . ? C9 C10 C11 C12 -1.0(10) . . . . ? C8 N3 C12 C11 -0.3(8) . . . . ? Hg1 N3 C12 C11 -175.0(4) . . . . ? C8 N3 C12 C13 177.5(5) . . . . ? Hg1 N3 C12 C13 2.8(6) . . . . ? C10 C11 C12 N3 0.8(9) . . . . ? C10 C11 C12 C13 -176.9(6) . . . . ? C14 N4 C13 C12 -159.7(5) . . . . ? Hg1 N4 C13 C12 -31.0(6) . . . . ? N3 C12 C13 N4 20.4(8) . . . . ? C11 C12 C13 N4 -161.9(5) . . . . ? C13 N4 C14 C15 153.6(5) . . . . ? Hg1 N4 C14 C15 24.7(7) . . . . ? C19 N5 C15 C16 -0.2(8) . . . . ? Hg1 N5 C15 C16 177.7(4) . . . . ? C19 N5 C15 C14 -178.2(5) . . . . ? Hg1 N5 C15 C14 -0.3(7) . . . . ? N4 C14 C15 N5 -17.8(8) . . . . ? N4 C14 C15 C16 164.3(6) . . . . ? N5 C15 C16 C17 -0.2(9) . . . . ? C14 C15 C16 C17 177.7(6) . . . . ? C15 C16 C17 C18 0.1(10) . . . . ? C16 C17 C18 C19 0.4(10) . . . . ? C15 N5 C19 C18 0.8(9) . . . . ? Hg1 N5 C19 C18 -177.0(4) . . . . ? C17 C18 C19 N5 -0.9(9) . . . . ? O3A Cl1A O1A Hg1 119.4(9) . . . . ? O4A Cl1A O1A Hg1 -110.1(6) . . . . ? O2A Cl1A O1A Hg1 2.8(7) . . . . ? O8A Cl2A O5A Hg1 84.1(15) . . . . ? O6A Cl2A O5A Hg1 -148.8(14) . . . . ? O7A Cl2A O5A Hg1 -29.8(10) . . . . ? 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 N2 H2N O3A 0.98 2.39 3.074(13) 126.3 1_554 N2 H2N O4B 0.98 2.32 3.08(2) 133.9 1_554 N4 H4N O7B 0.98 2.53 3.27(2) 132.9 . N4 H4N O7B 0.98 2.66 3.58(2) 158.2 3 _refine_diff_density_max 0.636 _refine_diff_density_min -0.938 _refine_diff_density_rms 0.077 _shelxl_version_number 2013-2 _shelx_res_file ; TITL DCB002 in P2(1)/n CELL 1.54178 9.1045 27.3639 9.5438 90.000 94.719 90.000 ZERR 4.00 0.0003 0.0009 0.0003 0.000 0.002 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O Cl Hg UNIT 76 84 20 32 8 4 LIST 4 OMIT -2 134 OMIT 1 2 2 L.S. 20 ACTA BOND $H CONF SIZE 0.14 0.13 0.09 FMAP 2 PLAN 10 TEMP 24 EQIV $1 x, y, z-1 BIND Hg1 O1A BIND Hg1 O5A EXYZ Cl1A Cl1B EADP Cl1A Cl1B EXYZ O1A O1B EADP O1A O1B EXYZ Cl2A Cl2B EADP Cl2A Cl2B EXYZ O5A O5B EADP O5A O5B EQIV $1 x, y, z-1 EQIV $2 -x, -y, -z HTAB N2 O3A_$1 HTAB N2 O4B_$1 HTAB N4 O7B HTAB N4 O7B_$2 WGHT 0.034000 6.264900 FVAR 0.25662 1.35263 0.71751 1.35263 1.35368 0.56113 1.36359 MOLE 1 HG1 6 0.230388 0.123677 0.139221 11.00000 0.05682 0.04524 = 0.05166 0.00478 0.01059 0.00109 N1 3 0.317416 0.206336 0.134037 11.00000 0.06786 0.04382 = 0.05039 0.00133 0.01677 -0.00635 N2 3 0.393088 0.129858 -0.044219 11.00000 0.07261 0.05507 = 0.04586 -0.01190 0.00844 -0.00478 AFIX 13 H2N 2 0.350521 0.110843 -0.124592 11.00000 -1.20000 AFIX 0 N3 3 0.403027 0.062224 0.168298 11.00000 0.05924 0.04165 = 0.05581 -0.01010 -0.00434 0.00338 N4 3 0.130265 0.055761 0.267431 11.00000 0.07840 0.06398 = 0.08145 0.01948 0.01159 -0.00142 AFIX 13 H4N 2 0.082166 0.034281 0.195392 11.00000 -1.20000 AFIX 0 N5 3 0.005112 0.146887 0.204840 11.00000 0.05254 0.05657 = 0.05429 -0.00045 0.01057 0.00009 C1 1 0.304687 0.238517 0.237218 11.00000 0.08664 0.05730 = 0.05707 -0.00792 0.02744 -0.00495 AFIX 43 H1 2 0.246055 0.230622 0.309270 11.00000 -1.20000 AFIX 0 C2 1 0.374550 0.282533 0.240745 11.00000 0.09775 0.05337 = 0.05931 -0.00945 0.01297 0.00176 AFIX 43 H2 2 0.361117 0.304859 0.312044 11.00000 -1.20000 AFIX 0 C3 1 0.465300 0.293315 0.136867 11.00000 0.07697 0.05318 = 0.06833 -0.00016 0.00665 -0.00850 AFIX 43 H3 2 0.516628 0.322713 0.137834 11.00000 -1.20000 AFIX 0 C4 1 0.478644 0.259903 0.031891 11.00000 0.06189 0.06139 = 0.05531 0.01105 0.01096 -0.00551 AFIX 43 H4 2 0.539832 0.266444 -0.039201 11.00000 -1.20000 AFIX 0 C5 1 0.401546 0.216648 0.031547 11.00000 0.05931 0.04738 = 0.03936 0.00841 0.00840 0.00098 C6 1 0.402760 0.180882 -0.089073 11.00000 0.08855 0.06259 = 0.04550 0.00034 0.01857 -0.00640 AFIX 23 H6A 2 0.320429 0.188013 -0.157056 11.00000 -1.20000 H6B 2 0.492756 0.185309 -0.135376 11.00000 -1.20000 AFIX 0 C7 1 0.535930 0.107951 0.003016 11.00000 0.06879 0.06734 = 0.06819 -0.01274 0.01381 -0.00380 AFIX 23 H7A 2 0.597824 0.132752 0.050425 11.00000 -1.20000 H7B 2 0.583930 0.097193 -0.078634 11.00000 -1.20000 AFIX 0 C8 1 0.523866 0.065430 0.100384 11.00000 0.05651 0.05169 = 0.06173 -0.01897 -0.00364 -0.00172 C9 1 0.636139 0.030697 0.125074 11.00000 0.06165 0.06808 = 0.08837 -0.03091 -0.00370 0.00499 AFIX 43 H9 2 0.721465 0.032368 0.077995 11.00000 -1.20000 AFIX 0 C10 1 0.617167 -0.005744 0.220153 11.00000 0.08006 0.05445 = 0.10063 -0.01958 -0.01831 0.01736 AFIX 43 H10 2 0.690954 -0.028903 0.238790 11.00000 -1.20000 AFIX 0 C11 1 0.490390 -0.008472 0.288294 11.00000 0.08952 0.04665 = 0.08165 -0.00607 -0.01170 0.00780 AFIX 43 H11 2 0.477047 -0.033567 0.351725 11.00000 -1.20000 AFIX 0 C12 1 0.383334 0.026572 0.261141 11.00000 0.07348 0.04034 = 0.06111 -0.00936 -0.01246 0.00117 C13 1 0.245157 0.027311 0.337147 11.00000 0.08745 0.04583 = 0.07164 0.00934 0.00204 -0.00773 AFIX 23 H13A 2 0.210485 -0.005946 0.346720 11.00000 -1.20000 H13B 2 0.268140 0.040333 0.430920 11.00000 -1.20000 AFIX 0 C14 1 0.014302 0.072613 0.349621 11.00000 0.08575 0.06663 = 0.07044 0.01111 0.02703 -0.00571 AFIX 23 H14A 2 0.055390 0.078314 0.445240 11.00000 -1.20000 H14B 2 -0.058974 0.046979 0.352506 11.00000 -1.20000 AFIX 0 C15 1 -0.061477 0.118972 0.294621 11.00000 0.06322 0.05900 = 0.05489 -0.00503 0.01261 -0.01136 C16 1 -0.195698 0.133467 0.339414 11.00000 0.06369 0.07820 = 0.07656 -0.01166 0.02247 -0.01804 AFIX 43 H16 2 -0.242735 0.114004 0.401915 11.00000 -1.20000 AFIX 0 C17 1 -0.259128 0.176221 0.292115 11.00000 0.05014 0.08457 = 0.09833 -0.02003 0.01287 -0.00083 AFIX 43 H17 2 -0.349130 0.185916 0.322481 11.00000 -1.20000 AFIX 0 C18 1 -0.190604 0.204537 0.200726 11.00000 0.05646 0.06937 = 0.08461 -0.01137 -0.00175 0.00743 AFIX 43 H18 2 -0.231938 0.233868 0.167836 11.00000 -1.20000 AFIX 0 C19 1 -0.059197 0.188675 0.158529 11.00000 0.05744 0.06326 = 0.06184 -0.00017 0.00259 0.00028 AFIX 43 H19 2 -0.012088 0.207638 0.094894 11.00000 -1.20000 AFIX 0 MOLE 2 PART 1 DFIX 21 Cl1A O1A Cl1A O2A Cl1A O3A Cl1A O4A DFIX 21.6440 O1A O2A O1A O3A O1A O4A O2A O3A O2A O4A O3A O4A CL1A 5 0.399425 0.150064 0.533525 31.00000 0.08414 0.06218 = 0.05110 -0.00447 0.01733 0.00675 O1A 4 0.438130 0.131411 0.409162 31.00000 0.18337 0.14638 = 0.09718 -0.06724 0.06503 -0.06307 O2A 4 0.250640 0.160295 0.500619 31.00000 0.08482 0.17136 = 0.41281 0.15477 0.03636 0.02427 O3A 4 0.412786 0.117602 0.637687 31.00000 0.39947 0.09299 = 0.08446 0.02554 0.00435 0.09969 O4A 4 0.467498 0.193565 0.562073 31.00000 0.20807 0.04793 = 0.09891 -0.02348 -0.00370 -0.02157 PART 2 DFIX 41 Cl1A O1A Cl1A O2A Cl1A O3A Cl1A O4A DFIX 41.6440 O1A O2A O1A O3A O1A O4A O2A O3A O2A O4A O3A O4A SAME Cl1A O1A O2A O3A O4A CL1B 5 0.399425 0.150064 0.533525 -31.00000 0.08414 0.06218 = 0.05110 -0.00447 0.01733 0.00675 O1B 4 0.438130 0.131411 0.409162 -31.00000 0.18337 0.14638 = 0.09718 -0.06724 0.06503 -0.06307 O2B 4 0.321780 0.192627 0.538890 -31.00000 0.44412 0.11938 = 0.17656 0.07865 0.18740 0.20038 O3B 4 0.537262 0.163995 0.596941 -31.00000 0.12280 0.70107 = 0.08214 -0.13572 0.05255 -0.17244 O4B 4 0.343713 0.120643 0.633804 -31.00000 0.19533 0.08570 = 0.03327 0.01250 0.02774 -0.08931 PART 0 MOLE 3 PART 1 DFIX 51 Cl2A O5A Cl2A O6A Cl2A O7A Cl2A O8A DFIX 51.6440 O5A O6A O5A O7A O5A O8A O6A O7A O6A O8A O7A O8A SAME Cl2A O5A O6A O7A O8A CL2A 5 -0.012195 0.079470 -0.163500 61.00000 0.07047 0.05800 = 0.07050 0.00334 0.00825 -0.00161 O5A 4 0.065662 0.121812 -0.126767 61.00000 0.12910 0.10061 = 0.09963 0.01127 -0.01698 -0.03202 O6A 4 -0.020309 0.072806 -0.302841 61.00000 0.26229 0.17916 = 0.04864 -0.01589 0.00048 -0.13770 O7A 4 0.071392 0.042857 -0.093629 61.00000 0.21214 0.11510 = 0.20010 0.07346 0.07950 0.09922 O8A 4 -0.142267 0.079598 -0.109845 61.00000 0.08980 0.29711 = 0.23236 0.02394 0.08660 -0.00353 PART 2 DFIX 71 Cl2B O5B Cl2B O6B Cl2B O7B Cl2B O8B DFIX 71.6440 O5B O6B O5B O7B O5B O8B O6B O7B O6B O8B O7B O8B CL2B 5 -0.012195 0.079470 -0.163500 -61.00000 0.07047 0.05800 = 0.07050 0.00334 0.00825 -0.00161 O5B 4 0.065662 0.121812 -0.126767 -61.00000 0.12910 0.10061 = 0.09963 0.01127 -0.01698 -0.03202 O6B 4 0.045776 0.059154 -0.275883 -61.00000 0.12914 0.32976 = 0.15159 -0.08404 0.06168 0.07026 O7B 4 -0.014648 0.047974 -0.057167 -61.00000 0.28011 0.14690 = 0.11836 0.06559 0.04996 -0.02905 O8B 4 -0.156674 0.093262 -0.213266 -61.00000 0.05235 0.09736 = 0.30234 0.03425 -0.01465 -0.01611 PART 0 HKLF 4 REM DCB002 in P2(1)/n REM R1 = 0.0273 for 3128 Fo > 4sig(Fo) and 0.0299 for all 3327 data REM 376 parameters refined using 50 restraints END WGHT 0.0280 5.5196 REM Highest difference peak 0.636, deepest hole -0.938, 1-sigma level 0.077 Q1 1 0.5059 0.1155 0.5073 11.00000 0.05 0.64 Q2 1 0.1589 0.0769 0.3549 11.00000 0.05 0.53 Q3 1 0.2717 0.1500 0.4182 11.00000 0.05 0.52 Q4 1 -0.0403 0.1191 -0.0700 11.00000 0.05 0.45 Q5 1 0.3130 0.1272 0.1956 11.00000 0.05 0.40 Q6 1 0.2961 0.1397 0.0805 11.00000 0.05 0.36 Q7 1 -0.1143 0.1030 -0.2716 11.00000 0.05 0.33 Q8 1 0.2248 0.1329 0.2353 11.00000 0.05 0.31 Q9 1 0.2908 0.1070 0.0629 11.00000 0.05 0.28 Q10 1 -0.1273 0.0503 -0.1288 11.00000 0.05 0.28 ; _shelx_res_checksum 83995 _shelx_hkl_file ; 1 0 0 0.97 0.34 -2 0 0 108.53 4.03 -2 0 0 106.72 5.12 2 0 0 111.39 5.50 2 0 0 108.83 4.50 -2 0 0 106.94 4.45 3 0 0 1.98 1.08 -3 0 0 1.08 0.72 -3 0 0 4.56 1.11 -3 0 0 0.27 0.39 3 0 0 3.32 0.98 -3 0 0 0.85 0.35 -3 0 0 0.83 0.62 -3 0 0 1.40 0.85 -4 0 0 2418.61 87.53 4 0 0 2550.17 86.70 -4 0 0 2567.10 86.42 -4 0 0 2625.43 86.25 4 0 0 2667.65 100.64 -4 0 0 2575.92 82.90 4 0 0 2380.08 87.79 -4 0 0 2629.70 90.68 -4 0 0 2538.85 86.10 -4 0 0 2613.05 86.70 -4 0 0 2616.50 100.29 5 0 0 5.33 0.95 -5 0 0 1.93 0.60 -5 0 0 2.18 0.85 5 0 0 0.59 1.76 -5 0 0 2.06 0.75 -5 0 0 0.34 1.30 -5 0 0 1.63 1.19 -5 0 0 0.84 0.73 -5 0 0 1.39 1.14 -6 0 0 570.70 19.34 -6 0 0 566.62 20.37 -6 0 0 570.27 20.40 -6 0 0 595.17 19.67 -6 0 0 566.21 25.38 -6 0 0 573.86 20.46 6 0 0 581.64 20.67 6 0 0 579.39 26.36 -6 0 0 570.75 21.90 -6 0 0 587.15 21.82 -6 0 0 534.01 19.25 -7 0 0 0.95 1.03 -7 0 0 -0.35 0.97 7 0 0 -1.19 1.32 -7 0 0 0.34 1.54 -7 0 0 1.60 1.64 -7 0 0 1.21 1.91 -7 0 0 1.64 1.70 -7 0 0 0.67 1.67 -7 0 0 1.28 1.82 -7 0 0 0.53 1.05 -8 0 0 249.75 12.66 -8 0 0 300.75 13.48 8 0 0 268.09 12.14 -8 0 0 282.40 12.14 -9 0 0 0.60 2.05 0 1 0 0.98 0.23 1 1 0 65.32 3.33 -1 -1 0 67.35 3.10 1 1 0 66.52 3.13 1 -1 0 70.75 3.17 2 -1 0 1880.35 77.69 -2 -1 0 1856.87 62.68 -2 -1 0 1797.74 63.44 -2 1 0 1982.31 72.46 2 1 0 1864.42 77.91 -2 -1 0 1964.75 72.52 -2 1 0 1734.03 63.30 -2 1 0 1926.14 62.76 2 1 0 1777.59 63.49 -3 -1 0 8.52 1.19 -3 -1 0 15.25 1.02 -3 1 0 14.80 1.62 3 -1 0 8.87 1.47 -3 1 0 10.39 1.22 -3 -1 0 16.54 1.24 -3 -1 0 10.19 1.44 -3 1 0 12.57 0.79 -3 1 0 12.38 1.34 -3 1 0 14.73 1.60 3 -1 0 8.72 1.22 -3 -1 0 10.28 1.09 -3 -1 0 11.53 0.88 3 1 0 10.09 1.39 -4 -1 0 382.62 14.39 -4 1 0 361.93 14.05 -4 -1 0 375.11 13.44 -4 1 0 370.22 14.38 -4 -1 0 394.82 14.55 -4 1 0 385.68 14.37 4 1 0 402.66 17.04 -4 1 0 366.36 14.24 4 1 0 386.19 13.58 -4 1 0 378.74 13.33 4 1 0 377.60 14.71 -4 -1 0 395.03 13.58 -4 -1 0 398.76 16.72 -4 1 0 394.66 13.41 -4 -1 0 408.78 13.68 -4 1 0 381.03 16.58 -4 -1 0 390.99 14.43 4 1 0 375.61 11.78 -4 -1 0 384.72 13.09 -4 1 0 385.80 12.89 -5 1 0 1095.36 38.52 -5 -1 0 1092.44 44.66 -5 1 0 1127.11 37.53 -5 -1 0 1082.89 39.40 -5 -1 0 1114.12 34.22 -5 -1 0 1122.81 38.49 5 -1 0 1113.23 45.17 -5 1 0 1083.01 44.57 -5 -1 0 1088.46 38.53 5 1 0 1073.49 37.79 5 1 0 1095.40 45.21 -5 1 0 1094.38 38.36 -5 -1 0 1099.89 36.18 5 -1 0 1087.16 37.54 -5 -1 0 1088.48 37.74 -5 -1 0 1060.77 37.82 6 1 0 219.73 8.75 -6 1 0 215.34 9.75 6 -1 0 215.16 12.20 -6 -1 0 216.58 11.53 -6 1 0 210.71 9.81 -6 1 0 208.40 8.19 -6 1 0 206.10 11.25 -6 1 0 208.98 9.01 -6 1 0 218.40 7.97 -6 -1 0 217.98 9.91 -6 -1 0 220.85 8.33 -6 -1 0 212.45 9.72 -6 -1 0 201.43 9.89 -6 1 0 211.93 8.60 -6 -1 0 212.01 8.48 -6 -1 0 208.26 9.00 -6 -1 0 214.37 8.22 -6 -1 0 214.33 8.67 6 1 0 216.34 12.34 -6 1 0 210.51 8.04 -6 -1 0 195.77 8.57 6 -1 0 216.62 8.42 -6 1 0 203.55 8.58 -7 1 0 131.04 6.84 -7 -1 0 117.75 7.13 -7 1 0 117.49 5.46 -7 1 0 111.81 5.09 -7 1 0 123.86 5.37 -7 1 0 128.22 7.22 -7 -1 0 125.34 6.40 -7 -1 0 111.41 7.07 -7 -1 0 121.38 6.74 -7 1 0 120.66 7.10 -7 1 0 117.69 7.09 -7 -1 0 116.05 7.00 7 1 0 119.16 6.37 -7 -1 0 127.33 5.64 7 -1 0 124.05 6.02 -7 1 0 123.79 6.35 -7 -1 0 111.17 5.66 -7 -1 0 118.37 6.30 -8 1 0 85.08 6.04 -8 1 0 85.52 6.11 8 1 0 77.98 5.56 -8 -1 0 84.12 5.88 -8 -1 0 93.38 6.34 -8 -1 0 80.02 6.07 -8 -1 0 88.11 5.58 -8 1 0 75.94 5.99 8 -1 0 76.94 5.33 -9 -1 0 75.99 6.14 0 2 0 76.24 4.18 0 -2 0 75.67 4.18 1 2 0 6991.71 286.07 -1 -2 0 7630.35 286.82 1 2 0 7446.83 308.40 -1 2 0 7346.43 287.12 -1 -2 0 7728.58 308.41 -2 -2 0 276.25 9.73 -2 -2 0 283.47 11.58 2 -2 0 269.90 12.08 -2 2 0 252.50 9.84 2 2 0 263.31 10.18 -2 2 0 268.36 9.45 2 2 0 291.92 11.73 2 2 0 271.17 12.51 -2 2 0 287.56 11.48 -2 -2 0 262.78 12.30 -3 2 0 1278.13 39.36 -3 2 0 1329.97 43.77 -3 2 0 1331.61 51.20 -3 -2 0 1299.67 44.80 -3 -2 0 1349.55 51.33 -3 -2 0 1318.83 44.09 3 -2 0 1258.60 54.78 3 -2 0 1256.23 44.70 -3 -2 0 1375.79 44.10 -3 -2 0 1220.48 44.42 -3 -2 0 1254.12 54.86 3 2 0 1305.22 44.23 3 2 0 1360.48 51.54 -3 -2 0 1294.08 35.88 -3 -2 0 1301.49 44.22 3 2 0 1253.43 36.00 -3 2 0 1233.90 44.61 -3 2 0 1353.42 44.19 -3 -2 0 1328.06 44.23 3 2 0 1289.21 45.06 -3 2 0 1302.57 44.80 3 2 0 1259.79 55.23 -4 -2 0 3.24 0.81 -4 -2 0 1.27 0.95 -4 -2 0 0.80 0.60 -4 2 0 -0.10 0.91 -4 2 0 0.86 0.42 -4 -2 0 0.73 0.98 -4 2 0 0.90 0.48 -4 -2 0 5.65 1.34 4 2 0 2.98 1.14 -4 2 0 1.27 0.92 4 2 0 4.75 1.41 -4 -2 0 1.50 0.53 4 2 0 1.39 0.68 4 2 0 1.07 1.13 -4 -2 0 2.10 0.88 -4 2 0 0.95 0.88 -5 -2 0 987.40 30.86 -5 -2 0 972.24 40.34 -5 2 0 998.40 32.20 5 -2 0 989.81 40.78 -5 -2 0 972.50 34.04 -5 -2 0 992.70 34.81 5 2 0 985.15 34.18 -5 -2 0 942.29 34.08 -5 2 0 986.08 33.58 -5 -2 0 1009.02 35.64 -5 -2 0 977.88 34.67 -5 2 0 955.05 40.14 -5 2 0 984.76 34.72 -5 -2 0 995.72 32.67 -5 2 0 979.43 34.56 5 -2 0 963.31 33.60 5 2 0 972.97 40.89 -6 -2 0 10.34 2.65 -6 -2 0 11.15 1.99 -6 -2 0 7.04 1.92 6 -2 0 12.13 1.50 6 2 0 10.13 1.81 -6 2 0 12.82 1.35 -6 2 0 13.15 2.76 -6 2 0 11.68 2.27 6 2 0 11.62 3.40 -6 -2 0 10.13 2.31 -6 -2 0 10.18 1.42 -6 2 0 11.23 1.34 -6 -2 0 9.74 1.58 -6 -2 0 8.86 1.44 -6 -2 0 7.92 2.03 -6 2 0 12.57 2.45 6 -2 0 16.51 3.73 -6 2 0 14.32 2.12 -6 -2 0 7.85 1.93 -6 2 0 9.37 2.03 -6 -2 0 13.32 2.35 -6 -2 0 10.40 1.39 -7 2 0 728.72 25.82 -7 2 0 706.41 25.72 -7 2 0 703.20 24.40 -7 -2 0 717.76 27.74 -7 -2 0 716.87 28.67 -7 2 0 728.58 24.47 -7 2 0 687.73 27.44 -7 -2 0 738.35 24.56 7 -2 0 746.19 26.25 -7 -2 0 762.69 26.05 7 2 0 757.59 27.06 -7 -2 0 723.85 24.57 -7 2 0 722.22 27.45 -7 -2 0 731.94 27.61 -7 2 0 741.74 25.80 -7 2 0 672.79 28.24 -7 -2 0 745.22 26.31 -8 -2 0 28.00 3.96 -8 -2 0 27.48 3.56 -8 -2 0 22.11 3.70 8 -2 0 21.88 2.95 -8 2 0 24.15 3.66 8 2 0 28.38 3.65 -8 2 0 22.61 3.60 -8 -2 0 21.39 3.57 -9 -2 0 17.15 3.10 -9 -2 0 14.81 3.29 9 2 0 8.64 4.62 0 3 0 0.71 0.51 0 -3 0 4.07 0.75 1 3 0 6.54 1.12 -1 3 0 3.74 0.69 1 3 0 6.26 0.88 -1 -3 0 2.72 0.80 1 -3 0 5.61 0.82 1 3 0 2.50 0.91 -2 3 0 299.76 9.75 -2 3 0 304.53 10.49 -2 3 0 293.06 10.83 -2 -3 0 303.60 12.82 2 3 0 305.76 13.97 -2 -3 0 300.84 10.81 2 3 0 310.62 12.96 2 -3 0 311.93 13.35 -2 3 0 315.58 12.61 -2 -3 0 305.64 13.74 2 3 0 291.97 11.29 -3 -3 0 64.80 2.88 -3 -3 0 61.38 3.07 -3 -3 0 67.74 4.07 -3 3 0 60.98 2.46 -3 3 0 62.26 3.67 -3 -3 0 69.01 4.00 -3 3 0 71.26 2.90 -3 -3 0 62.32 3.37 -3 -3 0 61.97 2.75 3 -3 0 62.15 3.82 -3 -3 0 66.61 3.37 3 3 0 66.32 4.46 -3 3 0 57.97 2.98 -3 -3 0 68.79 3.01 3 3 0 64.90 2.92 -3 3 0 60.59 3.05 3 3 0 67.60 4.16 3 3 0 66.00 2.93 4 3 0 327.23 14.48 -4 3 0 308.94 10.46 -4 3 0 317.08 11.99 4 3 0 313.36 11.49 -4 -3 0 317.07 11.43 4 3 0 297.55 9.98 -4 -3 0 310.17 11.02 -4 -3 0 317.36 14.05 -4 -3 0 317.14 12.09 -4 -3 0 305.37 11.32 -4 -3 0 306.90 12.12 -4 3 0 317.02 13.83 -4 -3 0 315.78 12.16 4 3 0 312.77 12.56 -4 3 0 302.68 10.79 -4 3 0 308.43 11.89 -5 3 0 622.06 26.82 -5 3 0 617.02 23.13 -5 3 0 617.18 23.03 5 3 0 610.84 24.08 -5 -3 0 651.47 20.68 -5 -3 0 640.14 23.23 -5 -3 0 633.54 22.53 -5 3 0 623.37 21.85 -5 -3 0 643.57 23.64 -5 -3 0 624.95 22.48 -5 -3 0 661.72 23.43 -5 -3 0 639.70 21.65 5 3 0 639.04 22.74 5 3 0 630.78 27.71 -5 3 0 637.93 20.99 -5 -3 0 630.45 27.11 -6 -3 0 421.04 16.02 -6 -3 0 427.59 16.09 -6 3 0 418.65 16.98 -6 3 0 417.85 19.72 -6 -3 0 432.59 17.12 -6 -3 0 444.88 15.98 -6 -3 0 431.21 16.43 -6 3 0 427.12 15.91 6 -3 0 429.07 15.47 -6 3 0 424.77 15.30 6 3 0 421.04 21.00 -6 -3 0 431.64 15.32 6 -3 0 443.89 20.88 6 3 0 441.40 16.54 -6 3 0 426.30 15.05 -6 -3 0 442.34 15.32 -6 -3 0 438.16 15.48 -6 3 0 422.88 16.89 -6 -3 0 403.96 17.63 -6 -3 0 419.36 17.17 -7 -3 0 112.04 7.01 -7 -3 0 126.35 7.12 -7 -3 0 120.68 6.26 -7 3 0 104.97 4.63 -7 3 0 109.54 6.77 -7 3 0 107.13 5.05 -7 -3 0 122.51 6.57 7 -3 0 106.79 5.46 -7 -3 0 115.04 6.88 -7 -3 0 117.95 6.26 7 3 0 113.46 6.46 -7 3 0 104.03 6.35 -7 3 0 118.25 6.21 -7 -3 0 122.00 5.65 -8 -3 0 111.99 7.18 -8 3 0 104.72 6.68 -8 -3 0 102.09 6.87 8 3 0 90.84 6.43 -8 -3 0 101.48 6.67 -8 -3 0 110.91 6.35 8 3 0 109.75 10.28 9 3 0 61.61 7.42 -9 -3 0 68.95 5.81 -9 -3 0 62.36 5.11 0 4 0 8677.78 361.14 0 -4 0 8643.63 360.13 -1 4 0 5.03 1.26 1 4 0 10.21 1.76 -1 -4 0 10.16 1.58 1 4 0 15.09 2.04 -1 4 0 5.87 1.05 1 -4 0 6.66 1.32 1 4 0 6.79 1.38 -1 4 0 5.66 0.91 2 -4 0 1857.29 78.23 2 4 0 1873.61 78.92 -2 -4 0 1843.57 78.62 2 4 0 1948.36 73.44 2 -4 0 1922.14 64.40 2 4 0 1813.62 64.20 -2 4 0 1756.02 63.64 -2 4 0 1875.28 56.42 -2 4 0 1874.47 63.01 -2 4 0 1921.81 72.92 -2 -4 0 1890.93 63.73 -3 -4 0 49.22 3.38 -3 4 0 48.18 2.03 3 -4 0 47.06 3.16 3 4 0 44.97 3.13 -3 -4 0 43.96 2.32 -3 -4 0 45.26 3.43 3 4 0 50.11 4.03 -3 -4 0 50.12 2.52 -3 4 0 45.97 2.47 3 4 0 50.01 3.68 3 4 0 49.29 2.63 -3 -4 0 44.73 2.78 -3 4 0 43.08 2.51 3 -4 0 50.22 2.88 -3 -4 0 48.66 2.49 3 4 0 48.46 2.66 -3 4 0 49.55 3.17 -3 -4 0 47.38 2.92 -4 -4 0 2012.45 66.58 -4 4 0 1969.26 63.38 -4 -4 0 1956.48 66.31 -4 -4 0 1979.20 77.40 -4 4 0 1935.51 66.06 -4 -4 0 1977.24 63.99 -4 4 0 1988.01 66.34 -4 4 0 1924.03 76.17 4 4 0 1981.49 77.83 -4 -4 0 1991.12 70.02 -4 4 0 1946.73 77.06 -4 -4 0 1917.47 67.23 -4 -4 0 1980.71 66.89 -4 -4 0 1993.27 59.08 4 4 0 1997.85 67.05 -4 4 0 1914.16 65.79 4 4 0 1847.59 54.37 4 4 0 1904.02 68.06 -5 -4 0 5.22 1.51 5 4 0 6.17 2.37 5 4 0 3.90 2.05 -5 -4 0 5.76 1.08 -5 4 0 4.10 1.57 5 4 0 9.90 1.59 -5 -4 0 4.70 1.80 -5 4 0 4.22 1.52 -5 4 0 3.02 0.75 -5 4 0 3.79 1.43 -5 -4 0 7.45 1.30 -5 -4 0 3.40 1.34 -5 -4 0 4.12 1.26 -5 -4 0 8.01 1.57 -5 4 0 2.67 0.72 -5 -4 0 3.77 1.46 -5 -4 0 4.13 1.20 -5 -4 0 4.88 0.71 -6 4 0 754.98 28.12 -6 4 0 757.87 27.98 -6 -4 0 767.53 25.32 6 -4 0 757.47 33.75 6 4 0 781.60 27.97 -6 -4 0 790.03 28.33 -6 -4 0 817.29 28.52 -6 4 0 732.79 26.42 6 4 0 759.55 34.22 -6 -4 0 769.66 26.71 -6 4 0 745.39 24.89 -6 4 0 739.59 32.61 -6 -4 0 772.07 25.18 -6 4 0 787.50 26.57 -6 -4 0 695.50 29.34 6 -4 0 770.72 26.72 -6 -4 0 770.28 28.39 -6 -4 0 763.75 27.45 7 -4 0 4.64 1.49 -7 -4 0 9.13 2.30 -7 4 0 4.42 1.93 -7 -4 0 4.87 2.24 -7 -4 0 6.29 1.55 7 4 0 8.11 2.26 -7 -4 0 4.60 2.16 -7 -4 0 7.34 2.15 -7 -4 0 6.11 2.12 -7 4 0 4.01 1.12 -7 -4 0 8.52 2.18 -8 -4 0 99.44 6.90 -8 -4 0 106.64 6.37 -8 -4 0 106.00 7.13 8 4 0 112.90 10.32 -8 -4 0 104.46 6.70 9 4 0 2.42 4.22 -9 -4 0 0.13 2.21 -9 -4 0 3.61 2.40 0 -5 0 4.72 1.12 0 5 0 4.42 1.49 0 5 0 -0.05 0.71 0 5 0 0.96 0.58 0 5 0 2.28 0.70 0 -5 0 1.02 0.76 -1 -5 0 962.14 41.17 -1 5 0 941.98 37.99 -1 5 0 934.71 29.41 1 5 0 909.63 33.53 1 -5 0 1030.11 33.79 -1 -5 0 963.14 33.79 1 5 0 1008.48 41.45 1 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405.86 17.89 4 5 0 415.45 13.44 -4 5 0 397.87 14.24 4 5 0 437.51 15.80 -4 -5 0 427.07 14.98 -5 5 0 457.96 17.16 -5 -5 0 449.40 17.48 5 5 0 457.56 17.14 -5 5 0 447.86 19.97 -5 -5 0 458.67 17.38 -5 -5 0 465.31 16.24 5 5 0 454.98 21.19 -5 -5 0 479.57 15.56 5 5 0 455.87 18.54 -5 -5 0 460.65 17.75 -5 -5 0 425.92 16.33 -5 -5 0 465.33 16.74 -5 -5 0 416.69 15.44 -5 5 0 458.55 15.27 -5 -5 0 470.18 16.90 -5 5 0 420.63 16.18 -5 5 0 458.62 15.97 -5 -5 0 463.07 17.51 -6 -5 0 341.94 12.27 -6 5 0 299.77 15.52 -6 -5 0 310.34 14.11 -6 5 0 313.29 12.65 6 5 0 331.49 13.36 -6 -5 0 339.57 13.87 -6 -5 0 339.85 13.79 -6 -5 0 318.31 13.20 6 -5 0 316.80 12.03 -6 5 0 314.92 11.17 6 5 0 322.93 17.36 -6 -5 0 334.35 12.69 -6 -5 0 328.85 12.31 -6 -5 0 330.07 12.93 6 -5 0 323.21 16.81 -6 5 0 317.32 11.74 7 -5 0 104.49 5.07 -7 -5 0 97.26 4.99 -7 -5 0 110.94 6.07 -7 -5 0 102.46 6.69 -7 -5 0 108.75 6.68 -7 -5 0 107.72 6.74 -7 -5 0 108.69 5.50 -7 5 0 91.06 4.45 -7 5 0 100.36 6.17 -7 -5 0 105.28 5.91 7 5 0 102.67 6.39 -7 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4 1645.02 51.28 2 12 -4 1615.70 57.49 -2 12 4 1638.85 65.89 1 12 -4 142.10 7.47 -1 12 4 146.17 6.87 -1 12 4 135.40 7.85 -1 12 4 147.26 7.20 -1 12 4 140.29 9.13 -1 12 4 143.89 9.10 1 -12 -4 133.53 7.42 1 12 -4 142.20 6.11 -1 -12 4 141.70 6.07 0 12 -4 1935.53 67.04 0 12 4 1979.63 60.67 0 12 -4 1877.26 72.83 0 -12 -4 1878.90 68.15 0 -12 4 1870.21 69.01 0 12 -4 1888.03 59.43 0 12 -4 1985.18 67.55 0 12 -4 1859.01 64.13 0 -12 4 1785.52 55.24 0 12 4 2062.81 78.14 0 -12 4 1931.06 67.94 0 12 -4 1924.38 67.66 0 12 -4 1888.68 70.18 0 12 4 1999.16 77.30 0 12 -4 1933.49 54.20 -1 12 -4 57.16 3.61 1 12 4 70.61 6.04 1 12 4 57.94 5.92 -1 12 -4 58.36 4.37 -1 12 -4 60.40 3.98 -1 -12 -4 62.11 4.67 -1 12 -4 60.31 4.44 1 12 4 64.89 5.81 -1 12 -4 57.72 3.82 1 -12 4 55.47 5.01 -1 12 -4 60.75 3.04 -1 12 -4 56.33 3.80 1 12 4 55.62 3.47 -1 12 -4 59.39 4.00 1 -12 4 58.45 4.58 -1 12 -4 56.59 4.32 -1 12 -4 63.48 4.05 1 12 4 61.42 4.62 2 12 4 1252.12 52.38 -2 -12 -4 1198.51 45.39 2 -12 4 1268.74 44.79 -2 -12 -4 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0.39 2.45 1 -2 -9 0.45 1.97 1 2 -9 1.93 2.02 -1 2 9 2.49 2.54 1 -2 -9 7.75 2.73 1 2 -9 4.69 2.28 0 -2 -9 197.81 11.10 0 2 -9 201.83 9.65 0 -2 9 206.52 10.77 0 -2 -9 202.32 9.44 0 2 -9 204.57 10.93 0 -2 -9 226.81 11.38 -1 -2 -9 -0.11 1.56 -1 -2 -9 2.14 1.92 -1 2 -9 0.84 1.53 -1 2 -9 2.16 2.09 -1 -2 -9 0.51 1.95 1 -2 9 2.39 2.01 -2 2 -9 269.98 11.09 -2 -2 -9 249.81 10.96 -2 2 -9 254.05 8.93 -2 -2 -9 248.61 11.49 -2 2 -9 258.87 11.16 2 2 9 245.05 9.79 2 -2 9 247.44 9.89 3 2 9 -0.60 1.70 -3 2 -9 0.94 1.15 -3 -2 -9 1.99 1.90 -3 2 -9 3.77 2.29 -3 -2 -9 -0.48 1.11 3 -2 9 2.07 1.79 4 2 9 157.28 6.85 4 -2 9 160.90 7.05 5 3 -9 30.19 4.53 -5 3 9 33.17 3.68 -5 -3 9 28.49 3.74 5 -3 -9 36.85 4.67 5 3 -9 27.33 3.62 4 3 -9 15.60 3.19 -4 -3 9 23.62 3.52 4 -3 -9 9.71 3.21 4 3 -9 16.50 3.83 3 3 -9 30.60 4.04 -3 -3 9 32.51 3.94 -3 3 9 37.95 4.71 3 -3 -9 32.21 4.74 -3 -3 9 39.14 5.08 3 -3 -9 30.30 3.69 2 3 -9 41.77 4.51 2 -3 -9 40.99 5.06 -2 -3 9 46.03 5.37 2 -3 -9 39.04 4.15 -2 3 9 38.64 4.86 -1 3 9 61.36 5.41 1 -3 -9 59.77 4.78 1 -3 -9 60.75 5.53 -1 -3 9 55.19 6.00 1 3 -9 52.26 5.08 1 3 -9 54.56 4.78 0 -3 -9 2.16 2.00 0 -3 -9 3.83 2.17 0 3 -9 2.90 2.17 0 -3 -9 1.79 2.16 0 -3 9 -1.79 2.40 0 3 -9 3.57 1.99 1 -3 9 16.25 2.76 -1 3 -9 21.03 3.34 -1 3 -9 17.12 2.82 1 -3 9 21.65 3.89 -1 -3 -9 17.68 3.37 -1 -3 -9 20.92 3.22 -1 -3 -9 13.42 2.80 -2 3 -9 12.75 1.78 -2 3 -9 13.27 1.95 -2 -3 -9 12.85 2.82 2 -3 9 9.65 2.39 -2 3 -9 16.41 3.11 -2 -3 -9 14.39 3.27 -2 -3 -9 13.00 2.25 2 3 9 9.17 2.30 -3 3 -9 33.80 2.60 3 3 9 29.21 3.15 3 -3 9 30.23 3.24 -3 -3 -9 29.65 2.53 -3 -3 -9 34.74 3.90 -3 3 -9 35.30 4.03 4 3 9 8.58 2.04 4 -3 9 4.13 1.95 5 -4 -9 178.58 9.80 5 4 -9 169.60 8.43 -5 -4 9 164.77 8.50 4 -4 -9 -2.33 2.21 4 4 -9 1.25 2.27 -4 -4 9 -1.02 1.90 -3 -4 9 500.99 19.68 -3 4 9 508.07 21.13 3 -4 -9 571.58 23.30 3 4 -9 554.21 19.95 2 -4 -9 2.99 2.45 -2 4 9 3.63 2.59 -2 -4 9 2.67 2.75 2 -4 -9 2.95 2.14 2 4 -9 6.88 2.43 -1 4 9 175.15 9.55 1 4 -9 195.52 9.20 1 4 -9 182.44 10.39 1 -4 -9 178.41 8.62 -1 -4 9 176.24 10.17 1 -4 -9 210.95 10.75 0 -4 -9 8.04 2.80 0 -4 -9 7.13 2.43 0 4 -9 8.05 2.34 0 -4 9 5.33 2.93 0 -4 -9 5.70 2.34 0 4 -9 9.98 2.78 1 -4 9 176.08 9.82 -1 -4 -9 188.93 8.90 1 -4 9 187.50 8.02 -1 4 -9 183.73 9.00 -1 -4 -9 187.73 10.21 -1 4 -9 187.28 9.45 -1 -4 -9 181.53 9.87 2 -4 9 5.12 2.03 -2 4 -9 3.26 1.40 2 4 9 -0.61 1.71 -2 -4 -9 3.05 1.96 -2 -4 -9 1.48 2.05 -2 -4 -9 2.37 1.48 -2 4 -9 1.86 2.17 3 4 9 188.61 7.86 -3 -4 -9 186.82 8.70 -3 -4 -9 189.39 10.04 -3 4 -9 194.94 9.07 3 -4 9 176.79 7.90 -3 4 -9 199.51 7.09 4 -4 9 -0.87 1.62 -5 -5 9 24.34 3.48 5 -5 -9 17.96 3.63 4 -5 -9 36.01 4.75 4 5 -9 30.13 4.01 -4 -5 9 33.84 4.09 -3 -5 9 115.86 6.83 3 -5 -9 105.39 7.50 3 5 -9 103.43 6.66 -2 5 9 28.28 3.99 2 5 -9 22.78 3.72 -2 -5 9 27.10 4.49 2 -5 -9 28.24 4.32 1 5 -9 17.99 3.24 1 5 -9 17.05 3.25 -1 5 9 18.25 3.54 1 -5 -9 16.68 3.43 -1 -5 9 19.30 4.07 1 -5 -9 15.62 2.86 0 -5 -9 1.35 2.02 0 5 -9 4.48 1.87 0 -5 -9 1.82 1.89 0 5 -9 7.85 2.58 0 -5 9 3.49 2.65 0 -5 -9 2.58 2.01 1 -5 9 13.79 2.58 -1 -5 -9 20.43 3.08 -1 -5 -9 14.01 3.14 -1 5 -9 19.08 3.26 1 -5 9 9.44 3.11 -1 -5 -9 13.74 2.67 -1 5 -9 17.18 2.64 -2 -5 -9 28.27 3.60 -2 5 -9 36.30 2.86 2 -5 9 31.50 3.47 -2 -5 -9 30.74 3.19 -2 -5 -9 33.78 4.33 -2 5 -9 29.95 3.85 -3 5 -9 11.26 1.76 -3 -5 -9 9.08 2.41 3 -5 9 5.87 2.21 -3 5 -9 9.94 2.79 -3 -5 -9 11.66 2.90 3 5 9 8.09 2.07 -5 -6 9 4.08 2.20 5 -6 -9 2.56 2.56 4 -6 -9 294.02 14.45 4 6 -9 299.25 12.60 3 -6 -9 -0.70 2.09 -3 -6 9 1.64 2.04 3 6 -9 1.18 2.33 2 -6 -9 411.84 18.04 -2 6 9 370.64 16.24 -2 -6 9 372.32 16.98 2 6 -9 409.26 15.65 1 6 -9 1.83 2.02 1 6 -9 4.20 2.16 -1 -6 9 -1.46 2.49 1 -6 -9 -0.77 1.94 0 -6 9 120.14 8.06 0 -6 -9 143.09 8.40 0 -6 -9 131.96 7.00 0 6 -9 126.67 7.64 0 -6 -9 122.05 8.10 0 6 -9 134.94 7.45 -1 -6 -9 17.84 3.01 1 -6 9 17.80 2.80 1 -6 9 14.35 3.45 -1 6 -9 18.83 3.39 -1 -6 -9 22.92 3.79 -1 6 -9 19.85 2.77 -1 -6 -9 20.79 3.16 2 -6 9 241.74 9.94 -2 6 -9 260.17 8.96 -2 -6 -9 264.44 12.60 -2 -6 -9 255.46 11.81 -2 6 -9 266.26 11.15 -2 -6 -9 234.56 10.66 -3 -6 -9 14.03 3.05 -3 6 -9 13.39 1.80 3 -6 9 15.80 2.62 -3 6 -9 14.40 2.94 -3 -6 -9 9.05 2.29 -5 -7 9 42.89 4.41 5 -7 -9 49.19 4.98 -4 -7 9 16.80 3.13 4 7 -9 16.12 3.26 4 -7 -9 14.65 3.35 -3 -7 9 29.26 3.90 3 -7 -9 35.75 4.67 3 7 -9 30.93 4.15 -2 -7 9 85.49 5.97 2 -7 -9 84.50 6.58 2 7 -9 78.48 5.78 1 -7 -9 3.22 2.20 1 7 -9 2.16 1.94 1 7 -9 2.22 2.22 -1 -7 9 1.70 2.58 0 -7 -9 8.63 2.68 0 7 -9 4.81 2.51 0 -7 -9 4.70 2.29 0 -7 9 5.80 2.82 0 7 -9 6.96 2.10 -1 -7 -9 3.55 2.22 -1 7 -9 3.34 2.34 -1 -7 -9 2.89 1.79 -1 7 -9 2.28 1.46 -1 -7 -9 3.66 2.02 1 -7 9 -0.90 1.82 -2 -7 -9 13.87 3.00 -2 7 -9 11.68 1.81 -2 7 -9 14.24 2.87 -2 -7 -9 11.92 2.56 -2 -7 -9 11.51 2.24 2 -7 9 7.88 2.29 -3 7 -9 18.11 1.95 -3 -7 -9 24.10 3.56 3 7 9 14.49 2.38 3 -7 9 15.93 2.65 -3 -7 -9 16.28 2.57 -5 -8 9 152.70 7.98 5 -8 -9 163.51 8.93 -4 -8 9 2.85 2.05 4 -8 -9 2.73 2.36 4 8 -9 2.56 2.37 3 -8 -9 276.20 13.46 -3 -8 9 258.92 11.82 3 8 -9 290.78 12.15 2 -8 -9 7.47 2.69 -2 -8 9 6.97 2.49 2 8 -9 7.80 2.77 -1 -8 9 291.74 14.21 1 8 -9 309.07 12.77 1 8 -9 304.08 14.88 1 -8 -9 319.54 14.75 0 -8 -9 13.37 3.01 0 8 -9 12.23 3.01 0 -8 -9 12.54 2.81 0 8 -9 10.10 2.37 -1 -8 -9 122.40 7.63 -1 8 -9 118.27 6.83 -1 -8 -9 107.71 7.03 1 -8 9 116.86 6.07 -1 -8 -9 107.22 6.18 -1 8 -9 118.90 6.29 2 -8 9 0.53 1.83 -2 -8 -9 1.00 1.85 -2 -8 -9 1.86 2.00 -2 8 -9 -0.18 2.19 -2 8 -9 1.09 1.24 3 -8 9 214.71 8.71 -5 -9 9 12.46 2.57 5 -9 -9 12.11 2.76 4 -9 -9 20.26 3.51 4 9 -9 20.47 3.48 -4 -9 9 20.22 3.21 3 -9 -9 31.13 4.36 -3 -9 9 40.56 4.40 3 9 -9 32.55 4.20 -2 -9 9 3.59 2.25 2 9 -9 3.95 2.44 2 -9 -9 1.87 2.14 1 9 -9 22.35 3.54 1 9 -9 19.02 3.25 1 -9 -9 19.79 3.62 0 9 -9 3.72 2.56 0 -9 -9 3.29 2.14 0 9 -9 2.40 1.62 -1 -9 -9 3.08 1.79 -1 -9 -9 1.85 2.15 -1 9 -9 3.73 2.43 -1 9 -9 5.38 1.56 1 -9 9 2.13 2.03 -2 9 -9 8.24 1.66 -2 -9 -9 11.33 2.72 2 -9 9 4.91 2.11 3 -9 9 22.77 2.88 -3 -9 -9 30.28 3.83 4 -10 -9 172.03 9.16 -4 -10 9 159.01 8.19 3 10 -9 -0.02 2.18 -3 -10 9 1.59 2.14 3 -10 -9 0.97 2.28 2 10 -9 369.28 14.26 -2 -10 9 337.80 14.10 2 -10 -9 349.13 16.10 1 10 -9 6.40 2.53 1 -10 -9 9.65 2.78 1 10 -9 4.31 1.96 0 10 -9 203.00 9.55 0 -10 -9 221.06 11.06 0 10 -9 204.64 10.29 -1 -10 -9 21.85 3.63 1 -10 9 20.17 2.88 -2 10 -9 205.64 7.40 2 -10 9 202.38 8.38 -2 -10 -9 194.92 10.28 -3 -10 -9 4.64 2.18 4 -11 -9 -0.50 2.12 -4 -11 9 2.28 1.97 3 -11 -9 6.04 2.47 3 11 -9 9.24 2.81 -3 -11 9 7.58 2.55 2 11 -9 57.19 4.87 -2 -11 9 55.80 4.69 2 -11 -9 43.43 4.64 -1 -11 9 6.15 2.53 1 -11 -9 9.75 2.77 1 11 -9 9.81 2.80 0 -11 -9 0.42 1.91 1 -11 9 -0.79 1.81 -1 -11 -9 0.47 1.89 -2 -11 -9 6.81 2.36 2 -11 9 6.88 2.09 -3 -11 -9 9.79 2.31 4 -12 -9 3.06 1.98 -4 -12 9 0.65 1.77 -3 -12 9 154.09 7.84 3 -12 -9 145.88 8.36 -2 -12 9 2.58 2.15 2 -12 -9 3.27 2.16 2 12 -9 0.46 2.16 1 -12 -9 302.87 14.05 1 12 -9 297.23 12.24 -1 -12 9 300.42 12.49 0 -12 -9 30.55 4.12 -1 -12 -9 176.85 9.48 2 -12 9 -0.23 1.73 -2 -12 -9 1.78 1.81 -3 -13 9 14.06 2.75 3 -13 -9 9.87 2.65 -2 -13 9 4.17 2.22 2 -13 -9 5.95 2.31 -1 -13 9 30.15 3.69 1 -13 -9 25.48 3.65 0 -13 -9 1.31 2.06 -1 -13 -9 0.65 1.77 -2 -13 -9 3.89 1.94 -3 -14 9 1.79 1.74 2 -14 -9 184.72 9.63 -2 -14 9 195.55 8.98 1 -14 -9 3.71 2.16 -1 -14 9 5.87 2.27 0 -14 -9 182.86 9.51 -1 -14 -9 0.65 1.79 2 -15 -9 10.11 2.40 -2 -15 9 9.98 2.43 1 -15 -9 0.60 1.88 -1 -15 9 1.77 1.91 0 -15 -9 2.30 2.01 -1 -15 -9 0.88 1.58 2 0 -10 99.80 5.92 1 0 -10 0.94 1.89 0 0 -10 205.53 9.21 -1 0 -10 0.58 1.58 2 -1 -10 40.46 4.70 2 1 -10 35.36 3.83 2 -1 -10 32.30 3.69 1 -1 -10 34.78 4.36 1 1 -10 29.21 3.63 1 -1 -10 32.46 3.69 0 1 -10 115.56 6.44 0 -1 -10 117.13 6.44 -1 1 -10 62.15 4.46 -1 -1 -10 64.51 4.48 3 -2 -10 104.68 7.08 2 2 -10 11.21 2.64 1 2 -10 161.91 7.81 1 -2 -10 154.73 7.65 0 2 -10 1.31 1.87 0 -2 -10 1.95 1.82 3 -3 -10 3.93 2.48 2 -3 -10 18.05 3.41 2 3 -10 16.50 2.93 1 3 -10 81.66 5.30 0 3 -10 39.10 4.04 0 -3 -10 41.04 4.01 0 -3 -10 38.32 4.38 3 -4 -10 2.10 2.20 2 -4 -10 141.50 8.16 2 4 -10 126.47 6.90 1 -4 -10 10.64 2.80 1 4 -10 8.60 2.50 0 4 -10 100.05 6.00 -1 -4 -10 6.62 2.44 3 -5 -10 21.21 3.44 2 -5 -10 23.59 3.59 1 5 -10 25.86 3.47 1 -5 -10 28.07 3.87 0 5 -10 39.76 4.06 0 -5 -10 45.35 4.45 3 -6 -10 144.45 8.23 2 -6 -10 0.47 1.87 0 -6 -10 0.44 1.93 -1 -6 -10 93.60 6.24 3 -7 -10 0.77 1.88 2 -7 -10 29.44 3.87 1 -7 -10 68.94 5.36 0 -7 -10 46.95 4.49 -1 -7 -10 9.71 2.45 2 -8 -10 177.17 9.34 1 -8 -10 5.12 2.25 0 -8 -10 92.80 6.16 -1 -8 -10 4.09 1.92 2 -9 -10 29.16 3.65 1 -9 -10 38.56 3.96 0 -9 -10 33.60 3.95 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 33117 _database_code_depnum_ccdc_archive 'CCDC 931870' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common diperchlorato-(2,6-bis([(2-pyridylmethyl)amino]methyl)pyridine)-cadmium(ii) _chemical_melting_point ? _chemical_formula_moiety 'C19 H21 Cd Cl2 N5 O8' _chemical_formula_sum 'C19 H21 Cd Cl2 N5 O8' _chemical_formula_weight 630.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 '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 9.1253(3) _cell_length_b 9.1478(3) _cell_length_c 15.9271(5) _cell_angle_alpha 74.250(2) _cell_angle_beta 81.541(2) _cell_angle_gamma 65.904(2) _cell_volume 1167.12(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 6939 _cell_measurement_theta_min 2.89 _cell_measurement_theta_max 72.04 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.795 _exptl_crystal_F_000 632 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.440 _exptl_crystal_size_mid 0.320 _exptl_crystal_size_min 0.240 _exptl_absorpt_coefficient_mu 10.110 _shelx_estimated_absorpt_T_min 0.095 _shelx_estimated_absorpt_T_max 0.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.0950 _exptl_absorpt_correction_T_max 0.1952 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method '\w and \y' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 19926 _diffrn_reflns_av_unetI/netI 0.0293 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.885 _diffrn_reflns_theta_max 62.489 _diffrn_reflns_theta_full 67.679 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measured_fraction_theta_full 0.864 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_Laue_measured_fraction_full 0.864 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_point_group_measured_fraction_full 0.864 _reflns_number_total 3643 _reflns_number_gt 3532 _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 'APEX2 (Bruker AXS, 2004)' _computing_cell_refinement 'SAINTPLUS (Bruker AXS, 2004)' _computing_data_reduction SAINTPLUS _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'SHELXLE (Hubschle, 2011)' _computing_publication_material 'Mercury 3.1 (CCDC, 2013)' _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^)+(0.0499P)^2^+1.0004P] 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 3643 _refine_ls_number_parameters 366 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0873 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.055 _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 Cd1 Cd 0.33165(3) 0.30914(3) 0.24876(2) 0.05412(12) Uani 1 1 d . . . . . N1 N 0.1960(4) 0.3205(4) 0.3852(2) 0.0624(8) Uani 1 1 d . . . . . N2 N 0.4715(5) 0.3906(5) 0.3330(3) 0.0721(9) Uani 1 1 d . . . . . H2 H 0.4962 0.4824 0.2950 0.087 Uiso 1 1 calc R U . . . N3 N 0.6042(4) 0.1649(4) 0.2327(2) 0.0593(7) Uani 1 1 d . . . . . N4 N 0.3910(4) 0.2203(4) 0.1140(2) 0.0656(8) Uani 1 1 d . . . . . H4 H 0.4056 0.3105 0.0686 0.079 Uiso 1 1 calc R U . . . N5 N 0.0910(4) 0.3910(4) 0.1809(2) 0.0651(8) Uani 1 1 d . . . . . C1 C 0.0861(7) 0.2558(6) 0.4149(4) 0.0833(13) Uani 1 1 d . . . . . H1 H 0.0439 0.2255 0.3758 0.100 Uiso 1 1 calc R U . . . C2 C 0.0326(8) 0.2320(7) 0.5006(5) 0.108(2) Uani 1 1 d . . . . . H2A H -0.0436 0.1853 0.5188 0.130 Uiso 1 1 calc R U . . . C3 C 0.0907(9) 0.2765(7) 0.5583(4) 0.104(2) Uani 1 1 d . . . . . H3 H 0.0535 0.2636 0.6164 0.125 Uiso 1 1 calc R U . . . C4 C 0.2047(7) 0.3406(7) 0.5300(3) 0.0875(15) Uani 1 1 d . . . . . H4A H 0.2487 0.3694 0.5690 0.105 Uiso 1 1 calc R U . . . C5 C 0.2552(5) 0.3629(5) 0.4429(3) 0.0656(10) Uani 1 1 d . . . . . C6 C 0.3703(6) 0.4484(7) 0.4064(4) 0.0897(15) Uani 1 1 d . . . . . H6A H 0.3089 0.5659 0.3879 0.108 Uiso 1 1 calc R U . . . H6B H 0.4385 0.4311 0.4525 0.108 Uiso 1 1 calc R U . . . C7 C 0.6232(5) 0.2535(7) 0.3582(3) 0.0784(12) Uani 1 1 d . . . . . H7A H 0.6038 0.1763 0.4093 0.094 Uiso 1 1 calc R U . . . H7B H 0.6952 0.2948 0.3740 0.094 Uiso 1 1 calc R U . . . C8 C 0.7030(5) 0.1646(5) 0.2870(3) 0.0626(9) Uani 1 1 d . . . . . C9 C 0.8677(5) 0.0806(5) 0.2792(3) 0.0715(11) Uani 1 1 d . . . . . H9 H 0.9357 0.0820 0.3169 0.086 Uiso 1 1 calc R U . . . C10 C 0.9282(5) -0.0042(6) 0.2152(3) 0.0762(12) Uani 1 1 d . . . . . H10 H 1.0384 -0.0612 0.2087 0.091 Uiso 1 1 calc R U . . . C11 C 0.8262(5) -0.0052(5) 0.1606(3) 0.0735(12) Uani 1 1 d . . . . . H11 H 0.8667 -0.0636 0.1172 0.088 Uiso 1 1 calc R U . . . C12 C 0.6624(5) 0.0814(5) 0.1704(2) 0.0594(9) Uani 1 1 d . . . . . C13 C 0.5424(5) 0.0781(5) 0.1167(3) 0.0672(10) Uani 1 1 d . . . . . H13A H 0.5869 0.0759 0.0577 0.081 Uiso 1 1 calc R U . . . H13B H 0.5224 -0.0217 0.1410 0.081 Uiso 1 1 calc R U . . . C14 C 0.2530(6) 0.2000(5) 0.0908(3) 0.0686(11) Uani 1 1 d . . . . . H14A H 0.2606 0.0887 0.1179 0.082 Uiso 1 1 calc R U . . . H14B H 0.2570 0.2136 0.0280 0.082 Uiso 1 1 calc R U . . . C15 C 0.0945(5) 0.3189(5) 0.1177(2) 0.0604(9) Uani 1 1 d . . . . . C16 C -0.0467(6) 0.3516(6) 0.0795(3) 0.0753(12) Uani 1 1 d . . . . . H16 H -0.0441 0.3006 0.0358 0.090 Uiso 1 1 calc R U . . . C17 C -0.1910(6) 0.4605(7) 0.1069(3) 0.0832(14) Uani 1 1 d . . . . . H17 H -0.2864 0.4817 0.0826 0.100 Uiso 1 1 calc R U . . . C18 C -0.1924(6) 0.5360(6) 0.1697(4) 0.0830(13) Uani 1 1 d . . . . . H18 H -0.2879 0.6115 0.1880 0.100 Uiso 1 1 calc R U . . . C19 C -0.0506(6) 0.4988(6) 0.2053(3) 0.0772(12) Uani 1 1 d . . . . . H19 H -0.0518 0.5504 0.2485 0.093 Uiso 1 1 calc R U . . . Cl1 Cl 0.38761(12) -0.11411(13) 0.35580(7) 0.0686(3) Uani 1 1 d D . . . . O1A O 0.3041(5) 0.0257(5) 0.2872(3) 0.0770(14) Uani 0.801(9) 1 d . . P A 1 O2A O 0.4587(6) -0.0458(6) 0.4058(4) 0.0968(17) Uani 0.801(9) 1 d D . P A 1 O3A O 0.2783(10) -0.1639(8) 0.4130(5) 0.124(3) Uani 0.801(9) 1 d D . P A 1 O1B O 0.448(3) -0.005(3) 0.336(2) 0.127(9) Uiso 0.199(9) 1 d . . P A 2 O2B O 0.371(4) -0.205(3) 0.4396(12) 0.109(8) Uiso 0.199(9) 1 d D . P A 2 O3B O 0.251(3) -0.081(3) 0.3060(16) 0.127(9) Uiso 0.199(9) 1 d D . P A 2 O4 O 0.5093(5) -0.2419(5) 0.3210(3) 0.1001(11) Uani 1 1 d D . . . . Cl2 Cl 0.31027(12) 0.69290(12) 0.10860(7) 0.0663(3) Uani 1 1 d . . . . . O5A O 0.234(2) 0.646(2) 0.1867(13) 0.154(8) Uani 0.53(3) 1 d . . P A 1 O6A O 0.4282(16) 0.736(3) 0.1197(15) 0.151(7) Uani 0.53(3) 1 d . . P A 1 O7A O 0.1844(17) 0.8436(17) 0.0645(9) 0.104(5) Uani 0.53(3) 1 d . . P A 1 O8A O 0.372(3) 0.594(2) 0.0463(8) 0.124(5) Uani 0.53(3) 1 d . . P A 1 O5B O 0.280(3) 0.609(2) 0.1937(10) 0.118(7) Uani 0.47(3) 1 d . . P A 2 O6B O 0.405(3) 0.786(3) 0.1090(13) 0.139(7) Uani 0.47(3) 1 d . . P A 2 O7B O 0.179(2) 0.782(4) 0.0649(13) 0.151(9) Uani 0.47(3) 1 d . . P A 2 O8B O 0.402(2) 0.543(3) 0.091(3) 0.164(11) Uani 0.47(3) 1 d . . P A 2 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 Cd1 0.05200(17) 0.05411(17) 0.06201(18) -0.02271(12) -0.00279(11) -0.02035(12) N1 0.066(2) 0.0598(18) 0.0665(19) -0.0231(15) 0.0023(15) -0.0256(16) N2 0.070(2) 0.068(2) 0.092(2) -0.0323(19) -0.0025(18) -0.0320(18) N3 0.0530(17) 0.0620(18) 0.0644(18) -0.0199(15) 0.0037(14) -0.0225(15) N4 0.075(2) 0.064(2) 0.0646(19) -0.0191(16) -0.0031(16) -0.0311(17) N5 0.064(2) 0.0601(19) 0.074(2) -0.0178(16) -0.0157(16) -0.0208(16) C1 0.090(3) 0.079(3) 0.096(3) -0.032(3) 0.016(3) -0.047(3) C2 0.113(5) 0.072(3) 0.127(5) -0.021(3) 0.045(4) -0.042(3) C3 0.131(5) 0.069(3) 0.073(3) -0.003(3) 0.008(3) -0.010(3) C4 0.086(3) 0.077(3) 0.073(3) -0.025(2) -0.020(3) 0.005(3) C5 0.059(2) 0.062(2) 0.070(2) -0.0279(19) -0.0105(18) -0.0071(18) C6 0.076(3) 0.107(4) 0.116(4) -0.072(3) 0.004(3) -0.039(3) C7 0.062(3) 0.094(3) 0.089(3) -0.039(3) -0.010(2) -0.026(2) C8 0.054(2) 0.067(2) 0.068(2) -0.0150(18) -0.0010(18) -0.0267(19) C9 0.059(2) 0.066(2) 0.086(3) -0.010(2) -0.006(2) -0.025(2) C10 0.054(2) 0.067(3) 0.095(3) -0.016(2) 0.006(2) -0.015(2) C11 0.066(3) 0.064(2) 0.083(3) -0.023(2) 0.015(2) -0.019(2) C12 0.063(2) 0.053(2) 0.060(2) -0.0151(17) 0.0106(17) -0.0235(17) C13 0.073(3) 0.066(2) 0.065(2) -0.0284(19) 0.0115(19) -0.027(2) C14 0.090(3) 0.066(2) 0.060(2) -0.0174(19) -0.012(2) -0.036(2) C15 0.074(2) 0.055(2) 0.055(2) 0.0010(16) -0.0135(18) -0.0331(19) C16 0.091(3) 0.083(3) 0.064(2) 0.001(2) -0.022(2) -0.050(3) C17 0.072(3) 0.090(3) 0.081(3) 0.012(3) -0.025(2) -0.038(3) C18 0.065(3) 0.076(3) 0.095(3) -0.003(3) -0.016(2) -0.020(2) C19 0.065(3) 0.068(3) 0.093(3) -0.022(2) -0.014(2) -0.015(2) Cl1 0.0625(5) 0.0651(6) 0.0668(5) -0.0027(4) 0.0007(4) -0.0225(5) O1A 0.091(3) 0.059(2) 0.075(2) -0.0021(17) -0.020(2) -0.0273(19) O2A 0.108(4) 0.087(3) 0.106(4) -0.033(3) -0.034(3) -0.032(3) O3A 0.128(5) 0.099(4) 0.141(5) -0.015(4) 0.050(5) -0.065(4) O4 0.084(2) 0.091(2) 0.106(3) -0.036(2) -0.0059(19) -0.0062(19) Cl2 0.0609(5) 0.0538(5) 0.0853(6) -0.0214(5) -0.0110(5) -0.0173(4) O5A 0.103(8) 0.105(9) 0.161(13) 0.049(8) -0.004(7) 0.001(7) O6A 0.089(7) 0.112(11) 0.281(19) -0.023(10) -0.083(9) -0.057(7) O7A 0.080(6) 0.079(7) 0.098(7) 0.000(5) 0.013(6) 0.006(4) O8A 0.191(14) 0.088(9) 0.095(7) -0.053(6) 0.003(6) -0.040(8) O5B 0.219(19) 0.073(8) 0.090(7) 0.000(6) -0.047(9) -0.084(10) O6B 0.24(2) 0.086(9) 0.135(11) -0.031(7) -0.024(10) -0.103(11) O7B 0.101(9) 0.18(2) 0.140(12) -0.046(12) -0.077(9) 0.011(10) O8B 0.100(9) 0.097(12) 0.31(3) -0.113(18) 0.026(15) -0.025(8) _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 Cd1 N3 2.304(3) . ? Cd1 N5 2.339(3) . ? Cd1 N1 2.343(3) . ? Cd1 N4 2.409(3) . ? Cd1 N2 2.409(4) . ? Cd1 O5B 2.506(15) . ? Cd1 O1A 2.605(4) . ? Cd1 O1B 2.66(3) . ? Cd1 O5A 2.761(17) . ? N1 C1 1.331(6) . ? N1 C5 1.341(5) . ? N2 C6 1.456(6) . ? N2 C7 1.457(6) . ? N2 H2 0.9800 . ? N3 C12 1.333(5) . ? N3 C8 1.337(6) . ? N4 C13 1.457(6) . ? N4 C14 1.457(6) . ? N4 H4 0.9800 . ? N5 C15 1.335(5) . ? N5 C19 1.347(6) . ? C1 C2 1.370(8) . ? C1 H1 0.9300 . ? C2 C3 1.348(10) . ? C2 H2A 0.9300 . ? C3 C4 1.360(9) . ? C3 H3 0.9300 . ? C4 C5 1.383(7) . ? C4 H4A 0.9300 . ? C5 C6 1.515(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.500(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.385(6) . ? C9 C10 1.364(7) . ? C9 H9 0.9300 . ? C10 C11 1.368(7) . ? C10 H10 0.9300 . ? C11 C12 1.385(6) . ? C11 H11 0.9300 . ? C12 C13 1.499(6) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.498(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.392(6) . ? C16 C17 1.383(8) . ? C16 H16 0.9300 . ? C17 C18 1.356(8) . ? C17 H17 0.9300 . ? C18 C19 1.366(7) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? Cl1 O1B 1.28(3) . ? Cl1 O3A 1.382(5) . ? Cl1 O2B 1.390(17) . ? Cl1 O4 1.421(4) . ? Cl1 O1A 1.450(4) . ? Cl1 O3B 1.459(17) . ? Cl1 O2A 1.482(5) . ? Cl2 O7B 1.311(15) . ? Cl2 O6A 1.336(12) . ? Cl2 O8B 1.362(16) . ? Cl2 O5A 1.386(19) . ? Cl2 O5B 1.414(16) . ? Cl2 O8A 1.426(13) . ? Cl2 O6B 1.438(17) . ? Cl2 O7A 1.460(13) . ? 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 N3 Cd1 N5 141.35(12) . . ? N3 Cd1 N1 123.02(12) . . ? N5 Cd1 N1 91.24(12) . . ? N3 Cd1 N4 70.31(12) . . ? N5 Cd1 N4 71.10(12) . . ? N1 Cd1 N4 151.47(12) . . ? N3 Cd1 N2 70.77(12) . . ? N5 Cd1 N2 143.95(12) . . ? N1 Cd1 N2 72.15(12) . . ? N4 Cd1 N2 134.62(13) . . ? N3 Cd1 O5B 107.2(6) . . ? N5 Cd1 O5B 82.1(5) . . ? N1 Cd1 O5B 98.3(5) . . ? N4 Cd1 O5B 101.2(3) . . ? N2 Cd1 O5B 69.4(4) . . ? N3 Cd1 O1A 86.78(13) . . ? N5 Cd1 O1A 81.26(13) . . ? N1 Cd1 O1A 80.88(12) . . ? N4 Cd1 O1A 74.54(12) . . ? N2 Cd1 O1A 125.16(13) . . ? N3 Cd1 O1B 63.2(6) . . ? N5 Cd1 O1B 114.5(7) . . ? N1 Cd1 O1B 77.8(7) . . ? N4 Cd1 O1B 89.1(7) . . ? N2 Cd1 O1B 93.5(7) . . ? O5B Cd1 O1B 162.8(8) . . ? N3 Cd1 O5A 114.2(4) . . ? N5 Cd1 O5A 75.1(4) . . ? N1 Cd1 O5A 95.6(4) . . ? N4 Cd1 O5A 101.0(4) . . ? N2 Cd1 O5A 75.0(4) . . ? O1A Cd1 O5A 156.1(4) . . ? C1 N1 C5 117.4(4) . . ? C1 N1 Cd1 123.5(3) . . ? C5 N1 Cd1 117.6(3) . . ? C6 N2 C7 113.8(4) . . ? C6 N2 Cd1 110.8(3) . . ? C7 N2 Cd1 108.5(3) . . ? C6 N2 H2 107.9 . . ? C7 N2 H2 107.9 . . ? Cd1 N2 H2 107.9 . . ? C12 N3 C8 120.4(4) . . ? C12 N3 Cd1 120.3(3) . . ? C8 N3 Cd1 119.4(3) . . ? C13 N4 C14 115.3(3) . . ? C13 N4 Cd1 111.4(3) . . ? C14 N4 Cd1 110.0(3) . . ? C13 N4 H4 106.5 . . ? C14 N4 H4 106.5 . . ? Cd1 N4 H4 106.5 . . ? C15 N5 C19 119.0(4) . . ? C15 N5 Cd1 117.3(3) . . ? C19 N5 Cd1 123.6(3) . . ? N1 C1 C2 122.8(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.7(6) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 118.6(5) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? N1 C5 C4 121.6(5) . . ? N1 C5 C6 116.5(4) . . ? C4 C5 C6 121.8(4) . . ? N2 C6 C5 113.5(4) . . ? N2 C6 H6A 108.9 . . ? C5 C6 H6A 108.9 . . ? N2 C6 H6B 108.9 . . ? C5 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? N2 C7 C8 112.9(4) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 121.2(4) . . ? N3 C8 C7 115.7(4) . . ? C9 C8 C7 123.0(4) . . ? C10 C9 C8 118.7(5) . . ? C10 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? C9 C10 C11 119.8(4) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 119.6(4) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? N3 C12 C11 120.3(4) . . ? N3 C12 C13 116.9(3) . . ? C11 C12 C13 122.7(4) . . ? N4 C13 C12 112.2(3) . . ? N4 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? N4 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N4 C14 C15 113.8(3) . . ? N4 C14 H14A 108.8 . . ? C15 C14 H14A 108.8 . . ? N4 C14 H14B 108.8 . . ? C15 C14 H14B 108.8 . . ? H14A C14 H14B 107.7 . . ? N5 C15 C16 120.3(4) . . ? N5 C15 C14 118.4(4) . . ? C16 C15 C14 121.3(4) . . ? C17 C16 C15 119.6(5) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 118.6(5) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? N5 C19 C18 123.0(5) . . ? N5 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? O1B Cl1 O2B 125.8(18) . . ? O1B Cl1 O4 100.5(13) . . ? O3A Cl1 O4 114.1(3) . . ? O2B Cl1 O4 99.1(12) . . ? O3A Cl1 O1A 110.1(4) . . ? O4 Cl1 O1A 111.5(2) . . ? O1B Cl1 O3B 116.1(17) . . ? O2B Cl1 O3B 108.9(16) . . ? O4 Cl1 O3B 100.8(11) . . ? O3A Cl1 O2A 105.7(4) . . ? O4 Cl1 O2A 110.8(3) . . ? O1A Cl1 O2A 104.1(3) . . ? Cl1 O1A Cd1 125.0(2) . . ? Cl1 O1B Cd1 131.4(18) . . ? O7B Cl2 O8B 116.9(13) . . ? O6A Cl2 O5A 112.5(13) . . ? O7B Cl2 O5B 112.9(13) . . ? O8B Cl2 O5B 88(2) . . ? O6A Cl2 O8A 106.2(12) . . ? O5A Cl2 O8A 122.5(11) . . ? O7B Cl2 O6B 112.7(16) . . ? O8B Cl2 O6B 112.1(12) . . ? O5B Cl2 O6B 112.0(9) . . ? O6A Cl2 O7A 106.3(10) . . ? O5A Cl2 O7A 102.7(8) . . ? O8A Cl2 O7A 105.2(8) . . ? Cl2 O5A Cd1 114.0(9) . . ? Cl2 O5B Cd1 128.2(10) . . ? 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 N4 H4 O8A 0.98 2.41 3.228(18) 140.7 . N4 H4 O8B 0.98 2.24 2.92(2) 125.4 . _refine_diff_density_max 0.618 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.066 _shelxl_version_number 2013-2 _shelx_res_file ; TITL P1bar in P-1 CELL 1.54178 9.1253 9.1478 15.9271 74.250 81.541 65.904 ZERR 2.00 0.0003 0.0003 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H N O Cl Cd UNIT 38 42 10 16 4 2 LIST 4 OMIT -2 125 OMIT -1 -2 2 L.S. 20 ACTA HTAB N4 O8A HTAB N4 O8B BOND $H BIND O5A Cd1 BIND O5B Cd1 BIND O1A Cd1 BIND O1B Cd1 FMAP 2 PLAN 5 SIZE 0.240 0.320 0.440 TEMP 23 DFIX 1.44 Cl1 O2A DFIX 1.44 Cl1 O2B DFIX 1.44 Cl1 O3A DFIX 1.44 Cl1 O3B DFIX 1.44 Cl1 O4 WGHT 0.049900 1.000400 FVAR 0.53902 0.80090 0.53109 MOLE 1 CD1 6 0.331652 0.309142 0.248757 11.00000 0.05200 0.05411 = 0.06201 -0.02271 -0.00279 -0.02035 N1 3 0.196005 0.320473 0.385199 11.00000 0.06593 0.05983 = 0.06650 -0.02312 0.00229 -0.02564 N2 3 0.471514 0.390576 0.332960 11.00000 0.07044 0.06784 = 0.09183 -0.03226 -0.00254 -0.03205 AFIX 13 H2 2 0.496153 0.482440 0.295031 11.00000 -1.20000 AFIX 0 N3 3 0.604165 0.164919 0.232714 11.00000 0.05303 0.06199 = 0.06444 -0.01986 0.00371 -0.02251 N4 3 0.391007 0.220266 0.114046 11.00000 0.07454 0.06438 = 0.06464 -0.01909 -0.00314 -0.03106 AFIX 13 H4 2 0.405596 0.310512 0.068585 11.00000 -1.20000 AFIX 0 N5 3 0.090956 0.390970 0.180887 11.00000 0.06380 0.06010 = 0.07401 -0.01781 -0.01571 -0.02082 C1 1 0.086124 0.255820 0.414885 11.00000 0.09011 0.07902 = 0.09601 -0.03200 0.01637 -0.04735 AFIX 43 H1 2 0.043868 0.225518 0.375788 11.00000 -1.20000 AFIX 0 C2 1 0.032570 0.231975 0.500564 11.00000 0.11348 0.07165 = 0.12748 -0.02127 0.04496 -0.04202 AFIX 43 H2A 2 -0.043553 0.185276 0.518772 11.00000 -1.20000 AFIX 0 C3 1 0.090666 0.276476 0.558341 11.00000 0.13053 0.06887 = 0.07305 -0.00316 0.00777 -0.01042 AFIX 43 H3 2 0.053502 0.263569 0.616389 11.00000 -1.20000 AFIX 0 C4 1 0.204738 0.340632 0.529984 11.00000 0.08626 0.07685 = 0.07252 -0.02483 -0.02009 0.00540 AFIX 43 H4A 2 0.248671 0.369425 0.569011 11.00000 -1.20000 AFIX 0 C5 1 0.255211 0.362921 0.442902 11.00000 0.05857 0.06230 = 0.07013 -0.02791 -0.01052 -0.00706 C6 1 0.370329 0.448373 0.406438 11.00000 0.07618 0.10748 = 0.11551 -0.07189 0.00419 -0.03918 AFIX 23 H6A 2 0.308940 0.565866 0.387917 11.00000 -1.20000 H6B 2 0.438488 0.431109 0.452490 11.00000 -1.20000 AFIX 0 C7 1 0.623182 0.253540 0.358161 11.00000 0.06174 0.09444 = 0.08865 -0.03933 -0.00980 -0.02632 AFIX 23 H7A 2 0.603789 0.176292 0.409278 11.00000 -1.20000 H7B 2 0.695225 0.294783 0.373981 11.00000 -1.20000 AFIX 0 C8 1 0.702991 0.164648 0.286991 11.00000 0.05424 0.06742 = 0.06823 -0.01496 -0.00095 -0.02668 C9 1 0.867685 0.080602 0.279217 11.00000 0.05942 0.06627 = 0.08607 -0.01029 -0.00552 -0.02538 AFIX 43 H9 2 0.935667 0.081975 0.316886 11.00000 -1.20000 AFIX 0 C10 1 0.928152 -0.004218 0.215197 11.00000 0.05368 0.06742 = 0.09485 -0.01639 0.00550 -0.01528 AFIX 43 H10 2 1.038386 -0.061229 0.208697 11.00000 -1.20000 AFIX 0 C11 1 0.826220 -0.005199 0.160586 11.00000 0.06559 0.06357 = 0.08297 -0.02274 0.01467 -0.01921 AFIX 43 H11 2 0.866657 -0.063625 0.117154 11.00000 -1.20000 AFIX 0 C12 1 0.662429 0.081367 0.170387 11.00000 0.06266 0.05308 = 0.06026 -0.01512 0.01056 -0.02345 C13 1 0.542429 0.078149 0.116724 11.00000 0.07348 0.06649 = 0.06544 -0.02841 0.01147 -0.02733 AFIX 23 H13A 2 0.586912 0.075871 0.057683 11.00000 -1.20000 H13B 2 0.522405 -0.021703 0.140970 11.00000 -1.20000 AFIX 0 C14 1 0.253019 0.200002 0.090769 11.00000 0.09027 0.06634 = 0.05994 -0.01742 -0.01225 -0.03626 AFIX 23 H14A 2 0.260643 0.088684 0.117950 11.00000 -1.20000 H14B 2 0.256996 0.213642 0.028024 11.00000 -1.20000 AFIX 0 C15 1 0.094546 0.318853 0.117695 11.00000 0.07420 0.05483 = 0.05527 0.00103 -0.01352 -0.03310 C16 1 -0.046743 0.351624 0.079491 11.00000 0.09137 0.08283 = 0.06359 0.00084 -0.02232 -0.05037 AFIX 43 H16 2 -0.044110 0.300625 0.035789 11.00000 -1.20000 AFIX 0 C17 1 -0.191045 0.460502 0.106940 11.00000 0.07224 0.09020 = 0.08107 0.01166 -0.02539 -0.03790 AFIX 43 H17 2 -0.286354 0.481746 0.082590 11.00000 -1.20000 AFIX 0 C18 1 -0.192393 0.536025 0.169664 11.00000 0.06489 0.07552 = 0.09534 -0.00294 -0.01628 -0.02037 AFIX 43 H18 2 -0.287884 0.611539 0.187998 11.00000 -1.20000 AFIX 0 C19 1 -0.050564 0.498849 0.205339 11.00000 0.06488 0.06816 = 0.09305 -0.02154 -0.01442 -0.01476 AFIX 43 H19 2 -0.051788 0.550418 0.248508 11.00000 -1.20000 AFIX 0 MOLE 2 CL1 5 0.387611 -0.114115 0.355798 11.00000 0.06246 0.06506 = 0.06683 -0.00269 0.00072 -0.02255 PART 1 O1A 4 0.304120 0.025712 0.287166 21.00000 0.09146 0.05901 = 0.07547 -0.00213 -0.02001 -0.02730 O2A 4 0.458666 -0.045796 0.405751 21.00000 0.10833 0.08687 = 0.10561 -0.03270 -0.03389 -0.03196 O3A 4 0.278298 -0.163938 0.412984 21.00000 0.12754 0.09850 = 0.14080 -0.01533 0.05044 -0.06512 PART 2 O1B 4 0.448481 -0.004715 0.335532 -21.00000 0.12748 O2B 4 0.371091 -0.204518 0.439600 -21.00000 0.10925 O3B 4 0.250943 -0.080972 0.306022 -21.00000 0.12690 PART 0 O4 4 0.509332 -0.241864 0.320964 11.00000 0.08405 0.09107 = 0.10633 -0.03639 -0.00589 -0.00622 MOLE 3 CL2 5 0.310275 0.692903 0.108597 11.00000 0.06090 0.05377 = 0.08530 -0.02139 -0.01102 -0.01727 PART 1 O5A 4 0.233826 0.645899 0.186744 31.00000 0.10327 0.10516 = 0.16126 0.04926 -0.00447 0.00140 O6A 4 0.428233 0.735853 0.119739 31.00000 0.08936 0.11190 = 0.28079 -0.02313 -0.08256 -0.05720 O7A 4 0.184351 0.843609 0.064523 31.00000 0.07980 0.07862 = 0.09762 -0.00005 0.01302 0.00630 O8A 4 0.371556 0.593585 0.046313 31.00000 0.19064 0.08843 = 0.09524 -0.05323 0.00329 -0.03991 PART 2 O5B 4 0.280267 0.609064 0.193715 -31.00000 0.21883 0.07278 = 0.09028 -0.00031 -0.04703 -0.08355 O6B 4 0.404986 0.785500 0.109028 -31.00000 0.24381 0.08579 = 0.13488 -0.03107 -0.02365 -0.10285 O7B 4 0.179215 0.781540 0.064906 -31.00000 0.10103 0.17731 = 0.14036 -0.04600 -0.07731 0.01062 O8B 4 0.401642 0.543188 0.091065 -31.00000 0.09967 0.09688 = 0.31168 -0.11292 0.02623 -0.02536 PART 0 HKLF 4 REM P1bar in P-1 REM R1 = 0.0332 for 3532 Fo > 4sig(Fo) and 0.0341 for all 3643 data REM 366 parameters refined using 5 restraints END WGHT 0.0482 1.0318 REM Highest difference peak 0.618, deepest hole -0.677, 1-sigma level 0.066 Q1 1 0.3266 0.2433 0.2992 11.00000 0.05 0.62 Q2 1 0.3658 0.1378 0.1570 11.00000 0.05 0.58 Q3 1 0.2334 -0.1696 0.3380 11.00000 0.05 0.50 Q4 1 0.3840 -0.1153 0.4285 11.00000 0.05 0.48 Q5 1 0.4804 0.2719 0.3807 11.00000 0.05 0.45 ; _shelx_res_checksum 90128 _shelx_hkl_file ; 1 0 0 2728.27 148.41 1 0 0 2903.99 180.24 -1 0 0 3049.81 180.37 -1 0 0 2899.57 161.61 2 0 0 1201.12 61.93 2 0 0 1229.05 75.66 -2 0 0 1161.07 53.32 -2 0 0 1225.21 67.34 -3 0 0 2489.38 136.30 3 0 0 2506.09 125.40 -3 0 0 2145.10 107.83 -3 0 0 2562.55 108.00 3 0 0 2507.48 152.82 4 0 0 511.85 34.79 4 0 0 546.82 28.18 -4 0 0 537.47 30.35 5 0 0 146.95 8.93 -5 0 0 143.22 9.16 -5 0 0 147.88 6.81 -5 0 0 146.45 6.89 -5 0 0 153.17 7.63 -6 0 0 268.81 10.85 -6 0 0 270.47 9.83 -6 0 0 296.16 12.53 -6 0 0 275.53 12.54 -7 0 0 100.72 4.48 -7 0 0 99.75 6.29 -7 0 0 103.23 5.00 -7 0 0 115.05 5.57 -7 0 0 105.03 5.00 -7 0 0 108.88 6.24 -7 0 0 109.51 4.42 -7 0 0 101.51 5.71 -7 0 0 105.92 4.60 -7 0 0 105.35 5.77 -7 0 0 103.81 4.59 -8 0 0 76.37 4.94 -8 0 0 78.86 4.16 -8 0 0 67.45 5.04 -8 0 0 70.91 3.55 -8 0 0 83.37 4.46 -8 0 0 72.15 3.52 -8 0 0 76.33 3.37 -8 0 0 72.74 4.14 -9 0 0 18.57 1.44 -9 0 0 19.13 2.26 -9 0 0 18.03 1.47 -9 0 0 17.83 1.60 -9 0 0 18.02 1.85 -9 0 0 17.10 1.28 -9 0 0 19.10 2.10 -9 0 0 20.22 2.22 -10 0 0 -0.03 0.45 -10 0 0 1.81 0.74 -10 0 0 0.95 0.46 -9 1 0 14.43 1.72 9 -1 0 9.37 1.53 -9 1 0 10.09 0.97 -9 1 0 9.41 0.91 -9 1 0 10.10 1.01 -9 1 0 12.58 1.55 -9 1 0 10.85 1.28 -8 1 0 47.16 3.20 -8 1 0 45.75 3.65 -8 1 0 48.75 3.20 -8 1 0 48.53 2.60 -8 1 0 48.31 2.42 -8 1 0 51.55 3.80 -8 1 0 44.71 2.95 -8 1 0 53.86 3.72 -8 1 0 49.88 2.66 -8 1 0 47.90 3.22 -7 1 0 175.86 8.64 -7 1 0 162.24 7.45 -7 1 0 177.58 7.52 -7 1 0 173.99 8.67 -7 1 0 175.35 6.51 -7 1 0 154.75 8.82 -7 1 0 171.82 6.83 -7 1 0 176.38 7.33 -7 1 0 169.18 6.89 -7 1 0 156.02 7.76 -7 1 0 172.36 8.11 -6 1 0 47.86 3.05 -6 1 0 45.20 2.87 -6 1 0 45.12 2.79 -6 1 0 40.40 3.79 -6 1 0 49.08 3.31 -6 1 0 48.30 2.55 -5 1 0 12.60 1.50 -5 1 0 10.90 1.53 -4 1 0 270.68 13.22 -4 1 0 296.57 12.53 -4 1 0 267.44 12.04 4 -1 0 274.08 18.71 4 -1 0 253.42 15.19 -4 1 0 277.34 16.25 3 -1 0 122.53 7.79 -3 1 0 135.49 6.49 -3 1 0 145.42 8.40 3 -1 0 135.38 9.65 2 -1 0 548.79 31.18 -2 1 0 638.79 33.97 -2 1 0 624.45 37.95 -2 1 0 580.56 26.86 1 -1 0 30.93 2.08 -1 1 0 24.76 1.84 -1 1 0 23.93 2.24 1 -1 0 25.74 2.44 -1 1 0 23.96 2.26 0 1 0 244.69 14.50 0 -1 0 257.99 16.07 0 1 0 245.09 15.99 1 1 0 877.25 55.15 -1 -1 0 885.00 55.16 -2 -1 0 21.04 1.27 -2 -1 0 27.12 1.64 2 1 0 21.10 2.47 2 1 0 26.07 2.51 -3 -1 0 112.23 6.38 3 1 0 104.53 5.86 3 1 0 101.01 8.26 4 1 0 862.34 42.72 4 1 0 791.32 53.02 -4 -1 0 811.36 46.33 5 1 0 313.17 16.64 -5 -1 0 324.78 17.80 -5 -1 0 291.41 14.43 5 1 0 284.44 21.27 -6 -1 0 72.60 4.00 6 1 0 68.79 5.18 -6 -1 0 70.80 3.70 -7 -1 0 28.70 2.87 -7 -1 0 29.00 1.76 -7 -1 0 25.53 2.08 -7 -1 0 31.53 2.34 -7 -1 0 21.36 2.64 -7 -1 0 25.96 2.17 -8 -1 0 398.46 14.26 -8 -1 0 393.01 17.47 -8 -1 0 397.54 17.07 -8 -1 0 388.48 16.34 -8 -1 0 375.49 14.28 -8 -1 0 367.74 17.71 -8 -1 0 382.78 15.14 -8 -1 0 401.07 13.64 -9 -1 0 35.23 3.22 -9 -1 0 33.96 2.09 -9 -1 0 39.72 2.08 -9 -1 0 35.13 3.01 -9 -1 0 31.39 1.87 -9 -1 0 28.81 2.98 -9 -1 0 31.68 2.61 -9 -1 0 30.16 2.25 -10 -1 0 19.66 1.20 -10 -1 0 18.48 1.23 -10 -1 0 16.68 1.09 -10 -1 0 15.62 1.67 -10 -1 0 16.54 1.76 -10 -1 0 16.10 1.52 -9 2 0 23.60 1.25 9 -2 0 22.04 1.61 -8 2 0 66.03 3.00 -8 2 0 62.31 3.56 -8 2 0 68.41 3.44 -8 2 0 70.51 3.91 -8 2 0 66.35 3.67 8 -2 0 65.18 3.96 -8 2 0 66.42 2.91 -8 2 0 65.81 3.50 -8 2 0 55.90 4.10 -7 2 0 2.48 1.11 -7 2 0 3.89 0.99 -7 2 0 7.04 1.46 -7 2 0 9.85 2.04 -7 2 0 2.19 1.18 -7 2 0 3.29 1.14 -6 2 0 181.21 7.24 -6 2 0 171.96 7.21 -6 2 0 185.26 8.12 -6 2 0 174.83 9.27 -6 2 0 184.18 8.57 -6 2 0 166.92 8.01 -6 2 0 177.82 7.80 -6 2 0 188.36 9.08 -6 2 0 190.77 7.87 -6 2 0 185.05 6.82 -6 2 0 179.68 8.88 -5 2 0 478.73 19.94 -5 2 0 455.07 15.88 -5 2 0 470.29 20.22 -5 2 0 429.04 17.40 -4 2 0 5.83 1.14 -4 2 0 6.37 1.18 -4 2 0 10.78 1.99 -4 2 0 10.71 1.34 3 -2 0 1765.86 119.00 -3 2 0 1896.83 107.00 3 -2 0 1887.31 98.28 -3 2 0 2051.88 84.77 2 -2 0 1530.07 71.11 -2 2 0 1650.37 90.25 2 -2 0 1609.67 82.63 -2 2 0 1646.70 71.31 -2 2 0 1562.09 100.06 -1 2 0 1251.28 64.28 1 -2 0 1116.70 58.21 1 -2 0 1091.53 50.13 -1 2 0 1173.59 70.52 -1 2 0 1010.39 50.33 0 2 0 3143.13 179.86 0 -2 0 3132.86 142.23 0 -2 0 3027.64 158.27 0 -2 0 3394.95 200.34 0 2 0 3394.60 200.14 1 2 0 5414.47 373.54 -1 -2 0 6050.92 265.59 -1 -2 0 6124.79 295.62 -1 -2 0 6450.47 373.60 -2 -2 0 78.64 5.83 -2 -2 0 78.74 4.13 2 2 0 84.10 5.85 3 2 0 365.82 24.69 -3 -2 0 385.00 18.65 4 2 0 199.59 10.11 4 2 0 166.74 13.37 5 2 0 4.95 1.01 5 2 0 1.16 1.77 -5 -2 0 3.20 0.87 -6 -2 0 125.65 5.65 6 2 0 124.55 7.56 -6 -2 0 118.99 6.05 -7 -2 0 61.47 2.68 -7 -2 0 56.39 4.41 -7 -2 0 71.00 3.52 -8 -2 0 12.37 2.27 -8 -2 0 17.61 1.81 -8 -2 0 12.98 2.38 -8 -2 0 17.75 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28.65 -1 3 0 622.87 40.08 0 3 0 1943.64 90.91 0 3 0 1842.03 115.10 0 3 0 2136.06 127.48 0 -3 0 2054.49 90.76 0 -3 0 2260.37 127.81 0 -3 0 2044.07 101.04 -1 -3 0 632.54 29.41 1 3 0 648.86 41.29 -1 -3 0 626.69 32.75 1 3 0 684.70 37.45 -1 -3 0 700.35 41.51 -2 -3 0 1333.16 57.23 -2 -3 0 1400.01 63.70 2 3 0 1288.35 80.87 -2 -3 0 1141.69 57.17 -3 -3 0 1712.98 81.34 3 3 0 1587.22 103.52 4 3 0 25.36 3.33 -4 -3 0 26.39 1.65 -5 -3 0 1451.09 65.76 5 3 0 1357.96 92.65 5 3 0 1552.13 75.29 -6 -3 0 742.17 35.54 6 3 0 818.35 41.27 -6 -3 0 793.25 32.65 -7 -3 0 17.81 2.40 -7 -3 0 19.83 1.58 7 3 0 18.33 2.65 -7 -3 0 21.72 1.24 -8 -3 0 270.02 11.89 -8 -3 0 271.27 9.44 -8 -3 0 259.46 12.58 -8 -3 0 275.04 10.07 -8 -3 0 278.57 12.72 -8 -3 0 254.63 11.58 -9 -3 0 211.69 9.20 -9 -3 0 199.36 9.19 -9 -3 0 200.60 7.26 -9 -3 0 184.17 7.56 -9 -3 0 197.26 9.84 -9 -3 0 206.50 7.63 -9 -3 0 204.30 9.81 -10 -3 0 1.31 1.55 -10 -3 0 1.34 0.49 -10 -3 0 1.65 0.65 -10 -3 0 -1.18 0.64 -10 -3 0 1.21 1.55 -10 -3 0 1.58 1.32 -10 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32.33 -1 -5 0 175.22 9.41 1 5 0 167.31 11.76 -1 -5 0 163.50 8.60 -1 -5 0 179.57 8.31 -2 -5 0 174.02 7.70 2 5 0 156.38 10.68 -2 -5 0 155.23 8.03 -2 -5 0 163.69 8.79 -3 -5 0 947.90 43.29 -3 -5 0 910.01 39.62 -3 -5 0 996.97 47.39 -4 -5 0 187.40 8.35 -4 -5 0 187.71 9.14 -4 -5 0 199.16 10.02 -5 -5 0 33.97 2.19 -5 -5 0 34.68 1.87 -5 -5 0 29.17 1.84 -5 -5 0 34.15 2.25 -5 -5 0 30.87 1.84 -6 -5 0 615.41 20.58 -6 -5 0 611.23 21.77 -6 -5 0 644.93 25.78 -6 -5 0 560.39 26.57 -6 -5 0 599.66 21.55 6 5 0 613.78 32.90 -6 -5 0 652.39 28.09 -7 -5 0 131.39 5.90 -7 -5 0 126.60 6.55 -7 -5 0 130.68 5.05 -7 -5 0 122.15 7.26 -7 -5 0 134.94 4.68 -7 -5 0 122.27 6.84 -8 -5 0 2.40 0.77 -8 -5 0 2.61 0.52 -8 -5 0 3.43 2.00 -8 -5 0 2.98 0.73 -8 -5 0 1.52 1.56 -8 -5 0 4.96 1.34 -9 -5 0 73.73 3.04 -9 -5 0 64.91 2.94 -9 -5 0 72.11 3.66 -9 -5 0 72.73 4.91 -9 -5 0 72.04 2.92 -9 -5 0 74.59 4.61 -10 -5 0 12.26 1.00 -10 -5 0 12.60 0.97 -10 -5 0 12.02 2.13 -10 -5 0 17.28 2.07 -6 6 0 8.44 0.74 5 -6 0 3.21 0.90 -5 6 0 4.23 0.88 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92.39 5.47 -6 -6 0 98.72 4.17 -6 -6 0 100.66 4.56 -7 -6 0 81.00 3.14 -7 -6 0 76.50 3.61 -7 -6 0 86.00 5.54 -7 -6 0 76.80 3.63 -7 -6 0 78.79 3.38 -7 -6 0 87.11 5.05 -7 -6 0 82.43 3.97 -7 -6 0 79.47 4.70 -8 -6 0 331.72 15.56 -8 -6 0 351.69 11.82 -8 -6 0 348.62 15.77 -8 -6 0 348.90 15.89 -8 -6 0 336.79 12.47 -8 -6 0 347.59 14.84 -9 -6 0 21.97 1.30 -9 -6 0 24.30 1.28 -9 -6 0 26.10 2.29 -9 -6 0 21.75 1.32 -9 -6 0 20.10 2.65 -9 -6 0 23.97 2.49 -9 -6 0 22.26 1.66 -10 -6 0 24.69 1.31 -10 -6 0 23.61 1.33 -10 -6 0 28.63 2.73 -10 -6 0 26.02 2.54 -4 7 0 2.16 0.87 4 -7 0 1.20 0.73 3 -7 0 44.41 2.72 2 -7 0 145.58 7.03 1 -7 0 32.56 2.46 -1 7 0 28.53 2.54 0 -7 0 50.01 3.15 0 -7 0 52.79 3.09 0 -7 0 53.84 3.47 -1 -7 0 264.30 11.11 -1 -7 0 255.18 11.17 -1 -7 0 256.69 9.16 -1 -7 0 267.46 13.00 -1 -7 0 257.44 12.11 -1 -7 0 256.40 12.00 -2 -7 0 31.33 2.69 -2 -7 0 31.72 2.10 -2 -7 0 32.01 2.36 -2 -7 0 29.41 2.77 -2 -7 0 32.41 2.09 -2 -7 0 32.23 1.94 -3 -7 0 97.20 5.37 -3 -7 0 89.39 3.93 -3 -7 0 92.77 3.82 -3 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0.61 -8 -7 0 3.86 1.52 -8 -7 0 0.22 0.73 -8 -7 0 1.31 1.11 -8 -7 0 1.21 1.54 -8 -7 0 0.47 0.75 -8 -7 0 2.29 0.53 -8 -7 0 1.42 0.60 -8 -7 0 2.24 0.52 -9 -7 0 3.29 1.46 -9 -7 0 4.08 0.63 -9 -7 0 4.38 0.82 -9 -7 0 4.92 1.56 -9 -7 0 4.49 0.59 -9 -7 0 4.53 1.31 -10 -7 0 7.35 1.44 -10 -7 0 6.01 0.61 -10 -7 0 7.02 0.66 3 -8 0 19.43 1.39 2 -8 0 37.63 2.33 1 -8 0 24.89 2.00 0 -8 0 79.76 4.35 0 8 0 83.16 4.29 -1 -8 0 33.95 2.58 -1 -8 0 29.81 2.34 -1 -8 0 33.44 2.34 -2 -8 0 131.11 6.69 -2 -8 0 135.78 7.13 -2 -8 0 130.73 5.05 -2 -8 0 138.77 6.19 -2 -8 0 124.12 5.15 -2 -8 0 130.65 6.05 -3 -8 0 293.84 12.42 -3 -8 0 301.92 10.36 -3 -8 0 283.59 13.47 -3 -8 0 292.23 12.29 -3 -8 0 294.52 13.59 -3 -8 0 297.09 10.90 -3 -8 0 291.12 10.69 -3 -8 0 299.15 10.87 -3 -8 0 297.14 10.96 -3 -8 0 295.72 14.37 -3 -8 0 294.50 11.11 -4 -8 0 8.72 1.16 -4 -8 0 4.81 0.98 -4 -8 0 6.24 1.12 -4 -8 0 6.18 1.09 -4 -8 0 8.63 0.93 -4 -8 0 7.16 1.14 -4 -8 0 7.35 0.91 -4 -8 0 5.71 1.13 -4 -8 0 4.98 1.64 -4 -8 0 8.26 1.34 -4 -8 0 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