# Copyright The Royal Society of Chemistry, 1998 #============================================================================== data_8/00602D #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. C.J. McKenzie Department of Chemistry Odense University Campusvej 55 DK-5230 Odense M Denmark ; _publ_contact_author_phone '+45 6557 2518' _publ_contact_author_fax '+45 6615 8780' _publ_contact_author_email chk@chem.ou.dk _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Mono-, di- and poly-nuclear transition metal complexes of a bis-tridentate ligand: Towards p-phenylenediamine-bridged co-ordination polymers. ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Alan Hazell ' ; Department of Chemistry Aarhus University DK-8000 \%Arhus C Denmark ; 'Christine J. McKenzie ' ; Department of Chemistry Odense University DK-5230 Odense M Denmark ; 'Lars Preuss Nielsen ' ; Department of Chemistry Odense University DK-5230 Odense M Denmark ; #============================================================================== data_1 #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; Dichloro(tetrakis-N,N,N',N'-(2-pyridylmethyl)-1,4-benzenediamine)zinc(II) ; _chemical_name_common ? _chemical_formula_sum C30H28N6Cl2Zn _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety ? _chemical_formula_weight 608.88 _chemical_melting_point ? _chemical_compound_source 'synthesized by authors' #================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2y1' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '-x,1/2+y,-z' _cell_length_a 8.369(2) _cell_length_b 13.448(3) _cell_length_c 13.330(4) _cell_angle_alpha 90.0 _cell_angle_beta 111.19(1) _cell_angle_gamma 90.0 _cell_volume 1399(1) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 30 _cell_measurement_theta_min 7.7 _cell_measurement_theta_max 12.5 _exptl_crystal_description tabular _exptl_crystal_colour pink _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 628 _exptl_absorpt_correction_type integration _exptl_absorpt_coefficient_mu 1.100 _exptl_absorpt_correction_T_min 0.727 _exptl_absorpt_correction_T_max 0.851 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Huber four-circle diffractometer' _diffrn_measurement_method \q/2\q _diffrn_standards_number 2 _diffrn_standards_interval_count 50 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 0 0 0 0 2 _diffrn_reflns_number 5288 _diffrn_reflns_av_R_equivalents 0.170 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.6 _diffrn_reflns_theta_max 27.6 _diffrn_reflns_reduction_process 5075 _reflns_number_total 3352 _reflns_number_observed 1976 _reflns_observed_criterion I>2\s(I) _computing_data_collection 'MAD (Allibon, 1995)' _computing_cell_refinement MAD _computing_data_reduction 'KRYSTAL (Hazell, 1995)' _computing_structure_solution ; SIR92 (Altomare et al., 1994), KRYSTAL ; _computing_structure_refinement 'modified ORFLS' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix The crystal was twinned on (001), reflections hkl with l = 2,9 and 13 were not included in the refinement, reflections with l = 0,11 were almost totally overlapped and could be unscrambled, the remaining reflections were used unaltered. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|} ; _refine_ls_hydrogen_treatment ; Hydrogen atoms fixed in calculated positions, C-H = 0.95\%A, with Uiso 20% larger than Ueq for the atoms to which they are attached. ; _refine_ls_abs_structure_Rogers no _refine_ls_extinction_method none _refine_ls_number_reflns 1976 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_obs 0.065 _refine_ls_wR_factor_obs 0.073 _refine_ls_goodness_of_fit_obs 1.395 _refine_ls_shift/esd_max 0.028 _refine_ls_shift/esd_mean 0.005 _refine_diff_density_max 1.2(1) _refine_diff_density_min -1.1(1) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type Zn 0.4922(2) 0.1120 0.5772(1) 0.031(1) Uij Cl1 0.5123(5) 0.1000(5) 0.4118(3) 0.058(3) Uij Cl2 0.4134(5) 0.2663(3) 0.6178(3) 0.055(3) Uij N1 0.5643(14) -0.0346(7) 0.6650(9) 0.036(7) Uij C1 0.5383(15) -0.0334(8) 0.7697(10) 0.031(7) Uij C2 0.5737(14) 0.0551(7) 0.8308(9) 0.025(6) Uij C3 0.5585(16) 0.0580(7) 0.9317(9) 0.028(7) Uij C4 0.5065(14) -0.0259(9) 0.9744(9) 0.027(6) Uij C5 0.4592(18) -0.1109(10) 0.9065(12) 0.042(9) Uij C6 0.4798(16) -0.1163(9) 0.8080(11) 0.036(8) Uij N2 0.4914(18) -0.0241(10) 1.0735(8) 0.050(8) Uij N11 0.7649(11) 0.1284(10) 0.6694(7) 0.036(6) Uij C12 0.8499(18) 0.2113(13) 0.6807(10) 0.044(9) Uij C13 1.0258(27) 0.2191(18) 0.7308(19) 0.078(17) Uij C14 1.1154(20) 0.1389(17) 0.7692(15) 0.070(14) Uij C15 1.0337(25) 0.0452(19) 0.7596(17) 0.075(15) Uij C16 0.8490(20) 0.0423(12) 0.7094(9) 0.040(8) Uij C17 0.7447(20) -0.0510(11) 0.6800(13) 0.055(11) Uij N21 0.2560(14) 0.0383(9) 0.5462(8) 0.042(7) Uij C22 0.1020(19) 0.0795(12) 0.5115(11) 0.053(11) Uij C23 -0.0500(19) 0.0250(23) 0.4803(13) 0.077(16) Uij C24 -0.0320(32) -0.0750(27) 0.4840(18) 0.109(24) Uij C25 0.1275(29) -0.1202(14) 0.5240(15) 0.078(15) Uij C26 0.2698(22) -0.0628(11) 0.5505(11) 0.051(10) Uij C27 0.4437(23) -0.1020(10) 0.5841(12) 0.055(11) Uij N31 0.2282(15) -0.2413(9) 1.0651(11) 0.052(8) Uij C32 0.0654(26) -0.2678(14) 1.0257(16) 0.067(14) Uij C33 -0.0688(22) -0.2016(15) 0.9852(17) 0.058(13) Uij C34 -0.0330(29) -0.1038(17) 0.9912(17) 0.075(16) Uij C35 0.1363(21) -0.0711(13) 1.0280(16) 0.061(12) Uij C36 0.2618(17) -0.1418(11) 1.0682(9) 0.041(7) Uij C37 0.4464(19) -0.1148(10) 1.1146(10) 0.040(8) Uij N41 0.7617(18) 0.1829(10) 1.2106(11) 0.055(9) Uij C42 0.9240(32) 0.2131(14) 1.2486(18) 0.081(17) Uij C43 1.0533(27) 0.1504(17) 1.2610(16) 0.067(14) Uij C44 1.0264(33) 0.0532(18) 1.2371(15) 0.076(17) Uij C45 0.8500(28) 0.0200(12) 1.1912(13) 0.064(13) Uij C46 0.7218(19) 0.0905(10) 1.1826(11) 0.045(9) Uij C47 0.5355(21) 0.0626(12) 1.1381(11) 0.048(10) Uij H2 0.6081 0.1130 0.8032 0.030 Uiso H3 0.5838 0.1179 0.9722 0.034 Uiso H5 0.4114 -0.1664 0.9297 0.050 Uiso H6 0.4542 -0.1760 0.7673 0.043 Uiso H12 0.7870 0.2703 0.6528 0.053 Uiso H13 1.0807 0.2819 0.7372 0.094 Uiso H14 1.2363 0.1434 0.8039 0.083 Uiso H15 1.0981 -0.0137 0.7852 0.090 Uiso H17a 0.7507 -0.0762 0.6149 0.066 Uiso H17b 0.7916 -0.0984 0.7358 0.066 Uiso H22 0.0946 0.1500 0.5077 0.063 Uiso H23 -0.1592 0.0562 0.4578 0.092 Uiso H24 -0.1317 -0.1155 0.4584 0.130 Uiso H25 0.1369 -0.1903 0.5326 0.093 Uiso H27a 0.4470 -0.1660 0.6150 0.066 Uiso H27b 0.4769 -0.1071 0.5233 0.066 Uiso H32 0.0390 -0.3366 1.0251 0.080 Uiso H33 -0.1836 -0.2246 0.9539 0.070 Uiso H34 -0.1238 -0.0567 0.9701 0.090 Uiso H35 0.1638 -0.0029 1.0255 0.073 Uiso H37a 0.4774 -0.1078 1.1902 0.048 Uiso H37b 0.5104 -0.1676 1.1000 0.048 Uiso H42 0.9485 0.2810 1.2675 0.097 Uiso H43 1.1674 0.1750 1.2874 0.081 Uiso H44 1.1191 0.0081 1.2497 0.092 Uiso H45 0.8221 -0.0467 1.1680 0.077 Uiso H47a 0.4993 0.0531 1.1972 0.057 Uiso H47b 0.4744 0.1167 1.0956 0.057 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zn 0.030(1) 0.029(1) 0.033(1) 0.003(1) 0.011 0.003(1) Cl1 0.051(2) 0.089(4) 0.038(2) 0.014(3) 0.021(1) 0.005(2) Cl2 0.064(2) 0.034(2) 0.065(2) 0.019(2) 0.021(2) 0.001(2) N1 0.048(6) 0.022(5) 0.051(6) 0.008(5) 0.032(5) -0.001(5) C1 0.032(6) 0.015(5) 0.045(7) 0.003(4) 0.013(5) -0.003(5) C2 0.028(5) 0.009(5) 0.038(6) 0.000(4) 0.011(4) 0.008(4) C3 0.043(6) 0.009(5) 0.033(6) 0.000(4) 0.013(5) -0.006(4) C4 0.027(5) 0.020(5) 0.033(6) 0.007(4) 0.008(5) 0.004(4) C5 0.040(7) 0.032(7) 0.051(9) -0.002(5) 0.012(6) 0.007(6) C6 0.034(6) 0.025(7) 0.048(8) -0.001(5) 0.016(6) -0.006(5) N2 0.071(8) 0.056(7) 0.020(5) -0.022(7) 0.012(5) -0.009(6) N11 0.027(4) 0.053(8) 0.023(4) 0.003(5) 0.004(3) 0.007(5) C12 0.036(7) 0.079(11) 0.022(7) -0.009(8) 0.017(6) 0.008(7) C13 0.052(12) 0.089(17) 0.098(17) -0.019(12) 0.031(11) -0.006(13) C14 0.029(7) 0.102(18) 0.072(11) -0.022(10) 0.010(7) -0.010(10) C15 0.036(10) 0.112(18) 0.068(12) 0.050(11) 0.008(9) 0.019(13) C16 0.049(8) 0.066(9) 0.007(5) 0.020(7) 0.012(5) 0.011(5) C17 0.054(9) 0.050(9) 0.079(11) 0.019(8) 0.046(8) -0.001(8) N21 0.039(6) 0.058(7) 0.034(5) -0.004(5) 0.019(5) -0.012(5) C22 0.045(8) 0.074(13) 0.044(8) -0.014(7) 0.022(6) -0.007(7) C23 0.018(6) 0.166(24) 0.047(9) -0.028(11) 0.012(6) -0.045(12) C24 0.082(18) 0.185(30) 0.079(15) -0.082(20) 0.053(14) -0.066(19) C25 0.101(15) 0.073(14) 0.075(12) -0.056(12) 0.052(11) -0.044(10) C26 0.074(11) 0.045(8) 0.036(7) -0.030(8) 0.023(7) -0.021(6) C27 0.078(12) 0.016(6) 0.056(10) -0.025(7) 0.008(9) -0.018(6) N31 0.030(6) 0.034(6) 0.080(9) 0.011(5) 0.006(6) 0.013(6) C32 0.065(11) 0.046(10) 0.084(14) -0.006(9) 0.021(10) 0.002(9) C33 0.025(8) 0.072(12) 0.083(13) -0.007(8) 0.027(8) 0.005(10) C34 0.063(14) 0.084(15) 0.086(14) 0.038(11) 0.035(12) 0.023(11) C35 0.036(10) 0.045(9) 0.097(13) 0.014(7) 0.020(9) 0.021(9) C36 0.056(8) 0.030(6) 0.037(6) -0.002(7) 0.019(5) 0.003(6) C37 0.052(8) 0.033(7) 0.022(6) -0.006(6) -0.002(5) 0.011(5) N41 0.055(8) 0.041(7) 0.062(9) -0.003(6) 0.012(7) 0.006(6) C42 0.095(17) 0.045(11) 0.076(14) -0.001(11) -0.002(12) 0.010(10) C43 0.053(10) 0.098(16) 0.047(10) -0.025(10) 0.013(9) 0.004(10) C44 0.091(18) 0.085(16) 0.036(9) 0.019(14) 0.001(11) -0.002(10) C45 0.081(14) 0.045(10) 0.050(9) 0.000(9) 0.005(9) -0.016(8) C46 0.059(8) 0.030(8) 0.040(6) 0.022(6) 0.010(6) 0.006(5) C47 0.059(10) 0.047(9) 0.035(7) -0.003(8) 0.015(7) -0.005(6) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Zn N21 2.115(11) Zn N11 2.177(9) Zn N1 2.261(10) Zn Cl1 2.277(4) Zn Cl2 2.300(4) N1 C17 1.466(16) N1 C1 1.488(14) N1 C27 1.489(16) C1 C6 1.387(16) C1 C2 1.411(15) C2 C3 1.397(15) C3 C4 1.401(15) C4 N2 1.372(14) C4 C5 1.422(18) C5 C6 1.386(18) N2 C47 1.417(19) N2 C37 1.442(17) N11 C12 1.301(20) N11 C16 1.360(18) C12 C13 1.383(24) C13 C14 1.309(29) C14 C15 1.417(30) C15 C16 1.446(24) C16 C17 1.497(22) N21 C22 1.323(19) N21 C26 1.363(18) C22 C23 1.395(23) C23 C24 1.353(36) C24 C25 1.386(36) C25 C26 1.355(21) C26 C27 1.458(24) N31 C32 1.320(21) N31 C36 1.365(18) C32 C33 1.381(26) C33 C34 1.345(27) C34 C35 1.393(27) C35 C36 1.373(20) C36 C37 1.487(19) N41 C46 1.306(19) N41 C42 1.330(26) C42 C43 1.334(31) C43 C44 1.345(27) C44 C45 1.449(32) C45 C46 1.405(23) C46 C47 1.502(22) C2 H2 0.950 C3 H3 0.950 C5 H5 0.950 C6 H6 0.950 C12 H12 0.950 C13 H13 0.950 C14 H14 0.950 C15 H15 0.950 C17 H17a 0.950 C17 H17b 0.950 C22 H22 0.950 C23 H23 0.950 C24 H24 0.950 C25 H25 0.950 C27 H27a 0.950 C27 H27b 0.950 C32 H32 0.950 C33 H33 0.950 C34 H34 0.950 C35 H35 0.950 C37 H37a 0.950 C37 H37b 0.950 C42 H42 0.950 C43 H43 0.950 C44 H44 0.950 C45 H45 0.950 C47 H47a 0.950 C47 H47b 0.950 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N11 Zn N21 150.8(4) N1 Zn N21 75.4(4) Cl1 Zn N21 99.7(3) Cl2 Zn N21 98.1(3) N1 Zn N11 76.5(4) Cl1 Zn N11 97.2(3) Cl2 Zn N11 96.1(3) Cl1 Zn N1 109.9(3) Cl2 Zn N1 135.3(3) Cl1 Zn Cl2 114.8(2) Zn N1 C17 105.7(8) Zn N1 C1 111.9(7) Zn N1 C27 99.9(8) Zn N1 C26 77.8(5) Zn N1 C16 79.2(4) Zn N1 C2 87.4(4) Zn N11 C12 124.7(10) Zn N11 C16 115.0(10) Zn N11 C13 153.2(8) Zn N11 C15 146.5(9) Zn N11 C17 81.4(6) Zn N21 C22 126.6(10) Zn N21 C26 113.6(10) Zn N21 C25 143.1(8) Zn N21 C27 80.3(5) Zn N21 C23 155.1(9) C1 N1 C17 111.5(10) C17 N1 C27 113.7(12) C1 N1 C27 113.3(11) C2 C1 C6 119.6(11) N1 C1 C6 121.8(11) N1 C1 C2 118.6(10) C1 C2 C3 120.4(10) C2 C3 C4 121.2(9) C3 C4 N2 121.8(11) C5 C4 N2 121.7(11) C3 C4 C5 116.4(10) C4 C5 C6 122.9(12) C1 C6 C5 119.2(11) C4 N2 C47 120.4(12) C4 N2 C37 118.6(11) C37 N2 C47 120.8(11) C12 N11 C16 120.0(11) N11 C12 C13 124.2(18) C12 C13 C14 119.1(20) C13 C14 C15 120.6(14) C14 C15 C16 117.8(16) N11 C16 C15 118.3(16) N11 C16 C17 116.2(12) C15 C16 C17 124.6(16) N1 C17 C16 112.6(11) C22 N21 C26 119.3(14) N21 C22 C23 123.5(18) C22 C23 C24 115.7(20) C23 C24 C25 121.9(18) C24 C25 C26 118.9(21) N21 C26 C25 120.3(18) C25 C26 C27 124.0(16) N21 C26 C27 115.7(13) N1 C27 C26 110.0(12) C32 N31 C36 116.7(13) N31 C32 C33 123.9(17) C32 C33 C34 118.4(18) C33 C34 C35 120.4(17) C34 C35 C36 117.2(16) N31 C36 C35 123.1(14) N31 C36 C37 115.1(12) C35 C36 C37 121.8(13) N2 C37 C36 115.0(11) C42 N41 C46 121.3(16) N41 C42 C43 121.7(18) C42 C43 C44 121.7(24) C43 C44 C45 117.2(23) C44 C45 C46 117.3(15) N41 C46 C45 120.7(16) N41 C46 C47 118.2(13) C45 C46 C47 121.1(13) N2 C47 C46 116.8(13) C3 C2 H2 119.8 C1 C2 H2 119.8 C2 C3 H3 119.4 C4 C3 H3 119.4 C6 C5 H5 118.6 C4 C5 H5 118.6 C5 C6 H6 120.4 C1 C6 H6 120.4 N11 C12 H12 117.9 C13 C12 H12 117.9 C14 C13 H13 120.5 C12 C13 H13 120.5 C13 C14 H14 119.7 C15 C14 H14 119.7 C14 C15 H15 121.1 C16 C15 H15 121.1 H17a C17 H17b 109.5 N1 C17 H17a 108.7 C16 C17 H17a 108.7 N1 C17 H17b 108.7 C16 C17 H17b 108.7 N21 C22 H22 118.2 C23 C22 H22 118.2 C24 C23 H23 122.1 C22 C23 H23 122.1 C23 C24 H24 119.0 C25 C24 H24 119.0 C26 C25 H25 120.5 C24 C25 H25 120.5 H27a C27 H27b 109.5 C26 C27 H27a 109.3 N1 C27 H27a 109.3 C26 C27 H27b 109.3 N1 C27 H27b 109.3 N31 C32 H32 118.0 C33 C32 H32 118.0 C34 C33 H33 120.8 C32 C33 H33 120.8 C33 C34 H34 119.8 C35 C34 H34 119.8 C36 C35 H35 121.4 C34 C35 H35 121.4 H37a C37 H37b 109.5 N2 C37 H37a 108.1 C36 C37 H37a 108.1 N2 C37 H37b 108.1 C36 C37 H37b 108.1 N41 C42 H42 119.2 C43 C42 H42 119.1 C42 C43 H43 119.1 C44 C43 H43 119.1 C43 C44 H44 121.4 C45 C44 H44 121.4 C46 C45 H45 121.4 C44 C45 H45 121.3 H47a C47 H47b 109.5 N2 C47 H47a 107.6 C46 C47 H47a 107.6 N2 C47 H47b 107.6 C46 C47 H47b 107.6 #=END #============================================================================== data_2 #============================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; [Dichloro(tetrakis-N,N,N',N'-(2-pyridylmethyl)-1,4-benzenediamine) dipalladium(II)]bis[trichloro(dimethylsulphoxide)palladium]0.53hydrate ; _chemical_name_common ? _chemical_formula_sum C34H41.06N6O2.53S2Cl8Pd4 _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_moiety [C30H28N6Cl2Pd2][(CH3)2SOPdCl3]2,0.53H2O _chemical_formula_weight 1347.62 _chemical_melting_point ? _chemical_compound_source ? #================================== # 6. CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M '1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' '1/2+x,1/2-y,1/2+z' '-x,-y,-z' '1/2-x,1/2+y,1/2-z' _cell_length_a 8.822(1) _cell_length_b 36.340(5) _cell_length_c 14.125(1) _cell_angle_alpha 90.0 _cell_angle_beta 92.086(6) _cell_angle_gamma 90.0 _cell_volume 4525(1) _cell_formula_units_Z 4 _cell_measurement_temperature 294 _cell_measurement_reflns_used 30 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 11.9 _exptl_crystal_description 'lath shaped' _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.978 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2637.20 _exptl_absorpt_coefficient_mu 2.170 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 1.210 #================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 294 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Huber four-circle diffractometer' _diffrn_measurement_method \q/2\q _diffrn_standards_number 2 _diffrn_standards_interval_count 2 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 8 0 0 0 4 _diffrn_reflns_number 8892 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.1 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_reduction_process 8547 _reflns_number_total 7996 _reflns_number_observed 5575 _reflns_observed_criterion I>3\s(I) _computing_data_collection 'MAD (Allibon, 1995)' _computing_cell_refinement MAD _computing_data_reduction 'KRYSTAL (Hazell, 1995)' _computing_structure_solution ; SIR92 (Altomare et al., 1994) KRYSTAL ; _computing_structure_refinement 'modified ORFLS' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #================================== # 8. REFINEMENT DATA _refine_special_details ; sfls: F calc weight full matrix ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme ; 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^-|F|} ; _refine_ls_hydrogen_treatment ; Hydrogen atoms in fixed positions, C-H = 0.95\%A, with Uiso 20% larger than Ueq of the atoms to which they are attached. Hydrogen atoms of water molecule kept at positions determined from difference map and with fixes Ueq. ; _refine_ls_extinction_method none _refine_ls_abs_structure_Rogers no _refine_ls_number_reflns 5575 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_number_constraints 2 _refine_ls_R_factor_obs 0.036 _refine_ls_wR_factor_obs 0.046 _refine_ls_goodness_of_fit_obs 1.094 _refine_ls_shift/esd_max 0.035 _refine_ls_shift/esd_mean 0.001 _refine_diff_density_max 0.7(1) _refine_diff_density_min -0.8(1) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy Pd1 -0.59274(6) 0.28279(1) 0.85119(3) 0.0285(3) Uij 1. Pd2 -0.27378(6) 0.47244(1) 0.80392(3) 0.0300(3) Uij 1. Pd3 -0.28385(6) 0.34501(2) 1.09770(3) 0.0362(3) Uij 1. Pd4 0.20899(7) 0.40164(2) 0.40690(4) 0.0439(3) Uij 1. Cl1 -0.6666(2) 0.25818(5) 0.9918(1) 0.049(1) Uij 1. Cl2 -0.2321(2) 0.50620(6) 0.9389(1) 0.056(1) Uij 1. Cl3 -0.0366(2) 0.32393(7) 1.1020(1) 0.060(1) Uij 1. Cl4 -0.3454(2) 0.29507(5) 1.1867(2) 0.056(1) Uij 1. Cl5 -0.2168(3) 0.39652(6) 1.0150(2) 0.066(1) Uij 1. Cl6 0.4396(3) 0.43152(6) 0.3991(1) 0.061(1) Uij 1. Cl7 0.0893(3) 0.45733(5) 0.4301(2) 0.064(1) Uij 1. Cl8 0.3291(3) 0.34601(6) 0.4052(2) 0.081(2) Uij 1. S1 -0.5235(2) 0.36566(5) 1.0843(1) 0.040(1) Uij 1. S2 -0.0189(3) 0.37360(5) 0.4101(1) 0.048(1) Uij 1. O1 -0.5861(7) 0.3682(2) 0.9869(4) 0.070(4) Uij 1. O2 -0.0819(7) 0.3717(2) 0.5050(4) 0.066(4) Uij 1. N1 -0.5375(5) 0.2979(1) 0.7168(3) 0.025(3) Uij 1. N2 -0.3069(6) 0.4445(1) 0.6794(3) 0.030(3) Uij 1. C1 -0.4773(6) 0.3357(2) 0.7089(4) 0.023(3) Uij 1. C2 -0.4529(8) 0.3502(2) 0.6190(4) 0.034(4) Uij 1. C3 -0.3993(8) 0.3857(2) 0.6109(4) 0.036(4) Uij 1. C4 -0.3677(7) 0.4068(2) 0.6898(4) 0.026(3) Uij 1. C5 -0.3883(7) 0.3923(2) 0.7790(4) 0.029(3) Uij 1. C6 -0.4441(7) 0.3566(2) 0.7881(4) 0.027(3) Uij 1. C7 -0.6536(9) 0.3406(3) 1.1504(7) 0.067(6) Uij 1. C8 -0.5349(12) 0.4088(2) 1.1397(7) 0.080(7) Uij 1. C9 -0.0230(12) 0.3288(2) 0.3623(7) 0.073(6) Uij 1. C10 -0.1529(11) 0.3952(3) 0.3320(7) 0.076(7) Uij 1. N11 -0.7924(6) 0.3061(1) 0.8145(4) 0.033(3) Uij 1. C12 -0.8960(8) 0.3196(2) 0.8708(5) 0.043(4) Uij 1. C13 -1.0270(8) 0.3361(2) 0.8348(6) 0.049(5) Uij 1. C14 -1.0510(9) 0.3382(2) 0.7388(6) 0.054(5) Uij 1. C15 -0.9406(9) 0.3249(2) 0.6794(5) 0.046(4) Uij 1. C16 -0.8120(7) 0.3090(2) 0.7198(5) 0.034(4) Uij 1. C17 -0.6877(7) 0.2936(2) 0.6630(4) 0.031(3) Uij 1. N21 -0.3784(6) 0.2645(1) 0.8584(4) 0.031(3) Uij 1. C22 -0.2913(8) 0.2591(2) 0.9369(4) 0.038(4) Uij 1. C23 -0.1413(9) 0.2485(2) 0.9312(5) 0.046(4) Uij 1. C24 -0.0804(8) 0.2431(2) 0.8438(5) 0.043(4) Uij 1. C25 -0.1708(8) 0.2499(2) 0.7628(5) 0.037(4) Uij 1. C26 -0.3183(8) 0.2612(2) 0.7722(4) 0.032(4) Uij 1. C27 -0.4239(8) 0.2692(2) 0.6892(4) 0.033(4) Uij 1. N31 -0.0668(6) 0.4493(1) 0.8020(4) 0.034(3) Uij 1. C32 0.0302(8) 0.4439(2) 0.8750(5) 0.046(4) Uij 1. C33 0.1674(9) 0.4247(2) 0.8611(7) 0.062(6) Uij 1. C34 0.1998(9) 0.4119(2) 0.7737(8) 0.066(6) Uij 1. C35 0.0973(9) 0.4175(2) 0.6984(6) 0.053(5) Uij 1. C36 -0.0362(7) 0.4362(2) 0.7154(5) 0.038(4) Uij 1. C37 -0.1516(8) 0.4440(2) 0.6390(5) 0.040(4) Uij 1. N41 -0.4891(6) 0.4893(1) 0.7783(4) 0.037(3) Uij 1. C42 -0.5859(8) 0.5036(2) 0.8392(5) 0.046(4) Uij 1. C43 -0.7324(9) 0.5136(2) 0.8123(7) 0.060(6) Uij 1. C44 -0.7789(9) 0.5073(2) 0.7184(7) 0.060(6) Uij 1. C45 -0.6806(9) 0.4915(2) 0.6564(6) 0.053(5) Uij 1. C46 -0.5356(8) 0.4830(2) 0.6872(5) 0.038(4) Uij 1. C47 -0.4153(8) 0.4690(2) 0.6240(5) 0.039(4) Uij 1. O3 0.5733(17) 0.0810(5) 0.6544(12) 0.119(14) Uij 0.53(2) H2 -0.4730 0.3358 0.5639 0.041 Uiso 1. H3 -0.3841 0.3957 0.5498 0.044 Uiso 1. H5 -0.3645 0.4066 0.8338 0.035 Uiso 1. H6 -0.4592 0.3467 0.8493 0.032 Uiso 1. H7a -0.6131 0.3390 1.2135 0.081 Uiso 1. H7b -0.6667 0.3167 1.1245 0.081 Uiso 1. H7c -0.7485 0.3530 1.1497 0.081 Uiso 1. H8a -0.4944 0.4072 1.2028 0.096 Uiso 1. H8b -0.6380 0.4163 1.1406 0.096 Uiso 1. H8c -0.4786 0.4263 1.1055 0.096 Uiso 1. H9a 0.0177 0.3300 0.3010 0.088 Uiso 1. H9b -0.1245 0.3200 0.3577 0.088 Uiso 1. H9c 0.0365 0.3127 0.4015 0.088 Uiso 1. H10a -0.1122 0.3964 0.2707 0.091 Uiso 1. H10b -0.1733 0.4193 0.3538 0.091 Uiso 1. H10c -0.2442 0.3813 0.3293 0.091 Uiso 1. H12 -0.8797 0.3179 0.9375 0.052 Uiso 1. H13 -1.0992 0.3459 0.8762 0.059 Uiso 1. H14 -1.1421 0.3487 0.7128 0.065 Uiso 1. H15 -0.9538 0.3267 0.6125 0.055 Uiso 1. H17a -0.7065 0.2682 0.6511 0.038 Uiso 1. H17b -0.6842 0.3064 0.6044 0.038 Uiso 1. H22 -0.3331 0.2626 0.9973 0.045 Uiso 1. H23 -0.0804 0.2450 0.9873 0.055 Uiso 1. H24 0.0212 0.2349 0.8390 0.052 Uiso 1. H25 -0.1311 0.2467 0.7017 0.045 Uiso 1. H27a -0.3675 0.2780 0.6379 0.040 Uiso 1. H27b -0.4757 0.2472 0.6706 0.040 Uiso 1. H32 0.0076 0.4529 0.9360 0.055 Uiso 1. H33 0.2369 0.4207 0.9130 0.074 Uiso 1. H34 0.2922 0.3993 0.7643 0.079 Uiso 1. H35 0.1178 0.4088 0.6368 0.064 Uiso 1. H37a -0.1312 0.4673 0.6115 0.048 Uiso 1. H37b -0.1477 0.4254 0.5918 0.048 Uiso 1. H42 -0.5526 0.5071 0.9033 0.055 Uiso 1. H43 -0.7987 0.5242 0.8561 0.071 Uiso 1. H44 -0.8785 0.5140 0.6969 0.073 Uiso 1. H45 -0.7132 0.4865 0.5929 0.064 Uiso 1. H47a -0.4616 0.4554 0.5734 0.047 Uiso 1. H47b -0.3613 0.4892 0.5992 0.047 Uiso 1. OH1 0.5671 0.0912 0.7051 0.150 Uiso 1. OH2 0.5139 0.0635 0.6474 0.150 Uiso 1. loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Pd1 0.0295(3) 0.0292(2) 0.0271(2) -0.0017(2) 0.0079(2) 0.0021(2) Pd2 0.0260(3) 0.0283(2) 0.0351(3) -0.0029(2) -0.0045(2) -0.0025(2) Pd3 0.0302(3) 0.0431(3) 0.0356(3) -0.0026(2) 0.0052(2) -0.0005(2) Pd4 0.0569(4) 0.0375(3) 0.0368(3) 0.0052(3) -0.0061(3) -0.0003(2) Cl1 0.057(1) 0.055(1) 0.038(1) -0.002(1) 0.018(1) 0.013(1) Cl2 0.056(1) 0.057(1) 0.054(1) 0.001(1) -0.013(1) -0.024(1) Cl3 0.032(1) 0.090(2) 0.058(1) 0.006(1) 0.007(1) 0.006(1) Cl4 0.047(1) 0.047(1) 0.073(1) 0.003(1) 0.016(1) 0.016(1) Cl5 0.070(2) 0.065(1) 0.064(1) -0.017(1) 0.010(1) 0.019(1) Cl6 0.055(1) 0.074(1) 0.054(1) -0.004(1) -0.007(1) 0.004(1) Cl7 0.065(1) 0.037(1) 0.090(2) 0.004(1) -0.009(1) -0.001(1) Cl8 0.105(2) 0.056(1) 0.080(2) 0.037(1) -0.031(1) -0.018(1) S1 0.038(1) 0.045(1) 0.039(1) 0.008(1) 0.002(1) -0.005(1) S2 0.066(1) 0.037(1) 0.040(1) -0.001(1) -0.003(1) -0.001(1) O1 0.056(4) 0.113(5) 0.040(3) 0.019(4) -0.005(3) -0.001(3) O2 0.082(4) 0.065(4) 0.050(3) -0.011(3) 0.011(3) -0.006(3) N1 0.023(3) 0.027(2) 0.025(2) -0.002(2) 0.002(2) 0.002(2) N2 0.030(3) 0.027(3) 0.032(3) -0.008(2) -0.003(2) 0.001(2) C1 0.015(3) 0.028(3) 0.027(3) 0.001(2) 0.004(2) 0.004(2) C2 0.038(4) 0.037(4) 0.028(3) -0.008(3) 0.002(3) -0.005(3) C3 0.046(4) 0.040(4) 0.023(3) -0.011(3) 0.005(3) 0.006(3) C4 0.019(3) 0.025(3) 0.032(3) -0.001(2) -0.003(3) 0.003(2) C5 0.026(3) 0.032(3) 0.029(3) 0.003(3) -0.003(3) -0.005(3) C6 0.022(3) 0.034(3) 0.024(3) -0.001(3) 0.000(3) 0.000(2) C7 0.032(5) 0.090(7) 0.081(6) 0.005(4) 0.014(4) -0.004(5) C8 0.097(8) 0.049(5) 0.096(7) 0.013(5) 0.018(6) -0.023(5) C9 0.094(8) 0.052(5) 0.074(6) -0.012(5) 0.000(6) -0.021(4) C10 0.066(7) 0.072(6) 0.089(7) -0.008(5) -0.034(5) 0.016(5) N11 0.029(3) 0.036(3) 0.033(3) -0.002(2) 0.011(2) 0.001(2) C12 0.038(4) 0.047(4) 0.045(4) -0.010(3) 0.016(3) 0.003(3) C13 0.029(4) 0.043(4) 0.075(6) -0.001(3) 0.015(4) 0.002(4) C14 0.035(4) 0.048(4) 0.080(6) 0.001(4) 0.008(4) 0.012(4) C15 0.044(5) 0.040(4) 0.054(4) -0.007(4) -0.005(4) -0.001(3) C16 0.027(4) 0.034(3) 0.042(4) -0.007(3) 0.000(3) -0.002(3) C17 0.031(4) 0.037(3) 0.027(3) -0.004(3) 0.003(3) 0.003(3) N21 0.031(3) 0.030(3) 0.032(3) 0.003(2) 0.004(2) 0.004(2) C22 0.039(4) 0.042(4) 0.032(3) 0.000(3) 0.006(3) 0.002(3) C23 0.047(5) 0.045(4) 0.044(4) -0.001(4) -0.001(4) 0.009(3) C24 0.036(4) 0.045(4) 0.049(4) 0.008(3) 0.003(3) 0.005(3) C25 0.042(4) 0.030(3) 0.041(4) 0.002(3) 0.007(3) -0.003(3) C26 0.038(4) 0.020(3) 0.038(4) 0.002(3) 0.009(3) -0.002(3) C27 0.042(4) 0.031(3) 0.027(3) 0.005(3) 0.003(3) -0.002(3) N31 0.027(3) 0.032(3) 0.044(3) -0.008(2) -0.002(3) 0.001(2) C32 0.029(4) 0.052(4) 0.057(5) -0.014(3) -0.008(4) 0.007(3) C33 0.030(5) 0.054(5) 0.100(7) -0.007(4) -0.023(5) 0.025(5) C34 0.034(5) 0.046(5) 0.118(8) -0.003(4) 0.011(5) 0.000(5) C35 0.036(4) 0.040(4) 0.084(6) -0.007(4) 0.009(4) -0.003(4) C36 0.028(4) 0.028(3) 0.059(4) -0.012(3) 0.009(3) 0.001(3) C37 0.037(4) 0.039(4) 0.045(4) -0.011(3) 0.009(3) 0.000(3) N41 0.029(3) 0.029(3) 0.053(4) -0.002(2) -0.007(3) 0.000(3) C42 0.035(4) 0.040(4) 0.064(5) 0.002(3) 0.003(4) -0.006(3) C43 0.030(4) 0.039(4) 0.110(8) 0.008(3) 0.005(5) 0.000(4) C44 0.030(5) 0.048(5) 0.103(7) -0.001(4) -0.010(5) 0.029(5) C45 0.046(5) 0.045(4) 0.067(5) -0.008(4) -0.015(4) 0.019(4) C46 0.033(4) 0.026(3) 0.053(4) -0.009(3) -0.012(3) 0.012(3) C47 0.047(4) 0.033(3) 0.036(4) -0.011(3) -0.008(3) 0.009(3) O3 0.083(11) 0.138(15) 0.135(15) 0.030(10) -0.012(10) -0.013(11) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Pd1 N11 2.005(5) Pd1 N21 2.004(5) Pd1 N1 2.051(5) Pd1 Cl1 2.294(2) Pd2 N31 2.011(5) Pd2 N41 2.016(5) Pd2 N2 2.042(5) Pd2 Cl2 2.286(2) Pd3 S1 2.245(2) Pd3 Cl3 2.311(2) Pd3 Cl4 2.284(2) Pd3 Cl5 2.296(2) Pd4 S2 2.256(2) Pd4 Cl6 2.312(2) Pd4 Cl7 2.312(2) Pd4 Cl8 2.283(2) S1 O1 1.467(5) S1 C7 1.759(9) S1 C8 1.757(8) S2 O2 1.470(6) S2 C9 1.763(8) S2 C10 1.770(9) N1 C1 1.480(7) N1 C17 1.511(8) N1 C27 1.508(8) N2 C4 1.480(7) N2 C37 1.503(9) N2 C47 1.504(8) C1 C2 1.399(8) C1 C6 1.376(8) C2 H2 0.950 C2 C3 1.378(9) C3 H3 0.950 C3 C4 1.374(9) C4 C5 1.383(8) C5 H5 0.950 C5 C6 1.395(8) C6 H6 0.950 C7 H7a 0.950 C7 H7b 0.950 C7 H7c 0.950 C8 H8a 0.950 C8 H8b 0.950 C8 H8c 0.950 C9 H9a 0.950 C9 H9b 0.950 C9 H9c 0.950 C10 H10a 0.950 C10 H10b 0.950 C10 H10c 0.950 N11 C12 1.327(8) N11 C16 1.347(8) C12 H12 0.950 C12 C13 1.383(10) C13 H13 0.950 C13 C14 1.367(11) C14 H14 0.950 C14 C15 1.396(11) C15 H15 0.950 C15 C16 1.378(10) C16 C17 1.491(9) C17 H17a 0.950 C17 H17b 0.950 N21 C22 1.339(8) N21 C26 1.352(8) C22 H22 0.950 C22 C23 1.383(10) C23 H23 0.950 C23 C24 1.377(10) C24 H24 0.950 C24 C25 1.393(9) C25 H25 0.950 C25 C26 1.376(9) C26 C27 1.498(9) C27 H27a 0.950 C27 H27b 0.950 N31 C32 1.330(9) N31 C36 1.350(8) C32 H32 0.950 C32 C33 1.418(11) C33 H33 0.950 C33 C34 1.358(13) C34 H34 0.950 C34 C35 1.385(12) C35 H35 0.950 C35 C36 1.387(10) C36 C37 1.484(10) C37 H37a 0.950 C37 H37b 0.950 N41 C42 1.339(9) N41 C46 1.355(8) C42 H42 0.950 C42 C43 1.382(11) C43 H43 0.950 C43 C44 1.393(12) C44 H44 0.950 C44 C45 1.381(12) C45 H45 0.950 C45 C46 1.371(10) C46 C47 1.500(10) C47 H47a 0.950 C47 H47b 0.950 O3 OH1 0.811 O3 OH2 0.826 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N11 Pd1 N21 166.4(2) N1 Pd1 N21 83.2(2) Cl1 Pd1 N21 97.1(1) N1 Pd1 N11 83.3(2) Cl1 Pd1 N11 96.5(1) Cl1 Pd1 N1 171.8(1) N31 Pd2 N41 167.1(2) N2 Pd2 N31 83.3(2) Cl2 Pd2 N31 96.7(2) N2 Pd2 N41 83.8(2) Cl2 Pd2 N41 96.2(2) Cl2 Pd2 N2 177.0(2) Cl4 Pd3 S1 94.01(7) Cl5 Pd3 S1 86.79(8) Cl3 Pd3 S1 176.66(6) Cl4 Pd3 Cl5 177.13(9) Cl3 Pd3 Cl4 88.01(8) Cl3 Pd3 Cl5 91.32(8) Cl8 Pd4 S2 90.8(1) Cl7 Pd4 S2 88.89(8) Cl6 Pd4 S2 178.02(9) Cl7 Pd4 Cl8 172.44(9) Cl6 Pd4 Cl8 90.3(1) Cl6 Pd4 Cl7 90.15(8) Pd1 N1 C1 114.6(3) Pd1 N1 C17 101.8(3) Pd1 N1 C27 103.7(3) Pd1 N11 C12 128.2(5) Pd1 N11 C16 111.7(4) Pd1 N21 C22 127.1(4) Pd1 N21 C26 112.5(4) Pd2 N2 C4 114.5(4) Pd2 N2 C37 103.3(4) Pd2 N2 C47 102.9(4) Pd2 N31 C32 127.6(5) Pd2 N31 C36 111.8(4) Pd2 N41 C42 128.4(5) Pd2 N41 C46 111.7(5) Pd3 S1 O1 114.9(2) Pd3 S1 C7 114.4(3) Pd3 S1 C8 109.3(4) Pd4 S2 O2 113.9(3) Pd4 S2 C9 114.5(4) Pd4 S2 C10 111.3(3) O1 S1 C8 109.7(5) O1 S1 C7 107.5(4) C7 S1 C8 100.1(5) O2 S2 C9 107.7(4) O2 S2 C10 108.8(5) C9 S2 C10 99.5(5) C1 N1 C17 111.6(4) C1 N1 C27 112.3(5) C17 N1 C27 112.2(5) C4 N2 C37 111.4(5) C4 N2 C47 111.9(5) C37 N2 C47 112.4(5) C2 C1 C6 119.6(5) N1 C1 C6 121.2(5) N1 C1 C2 119.2(5) C3 C2 H2 120.2 C1 C2 H2 120.2 C1 C2 C3 119.5(6) C4 C3 H3 119.5 C2 C3 H3 119.5 C2 C3 C4 121.0(6) C3 C4 C5 119.7(5) N2 C4 C3 120.0(5) N2 C4 C5 120.3(5) C4 C5 H5 120.1 C6 C5 H5 120.1 C4 C5 C6 119.9(5) C1 C6 H6 119.9 C5 C6 H6 119.9 C1 C6 C5 120.2(5) H7a C7 H7b 110.0 H7a C7 H7c 110.0 S1 C7 H7a 107.5 H7b C7 H7c 109.5 S1 C7 H7b 110.0 S1 C7 H7c 110.0 H8a C8 H8b 109.4 H8a C8 H8c 109.4 S1 C8 H8a 109.7 H8b C8 H8c 109.5 S1 C8 H8b 109.4 S1 C8 H8c 109.4 H9a C9 H9b 109.9 H9a C9 H9c 109.9 S2 C9 H9a 107.7 H9b C9 H9c 109.5 S2 C9 H9b 109.9 S2 C9 H9c 109.9 H10a C10 H10b 109.6 H10a C10 H10c 109.6 S2 C10 H10a 108.8 H10b C10 H10c 109.5 S2 C10 H10b 109.6 S2 C10 H10c 109.6 C12 N11 C16 120.0(6) N11 C12 H12 119.2 C13 C12 H12 119.2 N11 C12 C13 121.7(7) C14 C13 H13 120.4 C12 C13 H13 120.4 C12 C13 C14 119.1(7) C13 C14 H14 120.3 C15 C14 H14 120.3 C13 C14 C15 119.4(7) C16 C15 H15 120.7 C14 C15 H15 120.7 C14 C15 C16 118.6(7) N11 C16 C15 121.2(6) N11 C16 C17 115.8(6) C15 C16 C17 123.0(6) H17a C17 H17b 109.5 C16 C17 H17a 109.4 N1 C17 H17a 109.4 C16 C17 H17b 109.4 N1 C17 H17b 109.4 N1 C17 C16 109.8(5) C22 N21 C26 120.1(6) N21 C22 H22 119.6 C23 C22 H22 119.6 N21 C22 C23 120.9(6) C24 C23 H23 120.1 C22 C23 H23 120.1 C22 C23 C24 119.8(7) C23 C24 H24 120.6 C25 C24 H24 120.6 C23 C24 C25 118.7(7) C26 C25 H25 120.4 C24 C25 H25 120.4 C24 C25 C26 119.3(6) N21 C26 C25 121.0(6) N21 C26 C27 115.8(6) C25 C26 C27 123.1(6) H27a C27 H27b 109.5 C26 C27 H27a 109.5 N1 C27 H27a 109.5 C26 C27 H27b 109.5 N1 C27 H27b 109.5 N1 C27 C26 109.3(5) C32 N31 C36 120.4(6) N31 C32 H32 120.2 C33 C32 H32 120.2 N31 C32 C33 119.6(7) C34 C33 H33 119.9 C32 C33 H33 119.9 C32 C33 C34 120.2(8) C33 C34 H34 120.2 C35 C34 H34 120.2 C33 C34 C35 119.7(8) C34 C35 H35 120.9 C36 C35 H35 120.9 C34 C35 C36 118.3(8) N31 C36 C35 121.9(7) N31 C36 C37 115.9(6) C35 C36 C37 122.2(7) H37a C37 H37b 109.5 C36 C37 H37a 109.4 N2 C37 H37a 109.4 C36 C37 H37b 109.4 N2 C37 H37b 109.4 N2 C37 C36 109.7(5) C42 N41 C46 119.8(6) N41 C42 H42 118.8 C43 C42 H42 118.8 N41 C42 C43 122.5(8) C42 C43 H43 121.3 C44 C43 H43 121.3 C42 C43 C44 117.4(8) C45 C44 H44 120.0 C43 C44 H44 120.0 C43 C44 C45 120.1(7) C46 C45 H45 120.2 C44 C45 H45 120.2 C44 C45 C46 119.5(8) N41 C46 C45 120.6(7) N41 C46 C47 115.2(6) C45 C46 C47 124.0(7) H47a C47 H47b 109.5 C46 C47 H47a 109.3 N2 C47 H47a 109.3 C46 C47 H47b 109.3 N2 C47 H47b 109.3 N2 C47 C46 110.0 OH1 O3 OH2 113.2