Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Davies, David' 'Davenport, Adam J.' 'Fawcett, John' 'Russell, David R.' _publ_contact_author_name 'Dr David Davies' _publ_contact_author_address ; Chemistry University of Leicester University Road Leicester LE1 7RH UNITED KINGDOM ; _publ_contact_author_email 'DLD3@LE.AC.UK' _publ_section_title ; Synthesis and structure of [2-{4(S)-isopropyl-2-oxazolinyl}phenyl]trimethyl tin and its reactivity as a carbometallating agent ; data_3d _database_code_CSD 181359 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H23 N O Sn' _chemical_formula_sum 'C15 H23 N O Sn' _chemical_formula_weight 352.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.7059(17) _cell_length_b 11.2951(18) _cell_length_c 18.111(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1576.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 190(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 5.33 _cell_measurement_theta_max 12.38 _exptl_crystal_description block _exptl_crystal_colour needle _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.611 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.514 _exptl_absorpt_correction_T_max 0.723 _exptl_absorpt_process_details ; 184 psi-scan data used for XEMP calculation ( SHELXL-97, Sheldrick, 1997), Rint before correction 0.0525 and 0.357 after correction ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 190(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens P4 diffractometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 2399 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 1 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 26.01 _reflns_number_total 2223 _reflns_number_gt 1939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Fait, 1991)' _computing_cell_refinement 'XSCANS (Fait, 1991)' _computing_data_reduction 'XSCANS (Fait, 1991)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0938P)^2^+2.0058P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(8) _refine_ls_number_reflns 2223 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1382 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn -0.02632(9) -0.59696(6) -0.93757(3) 0.0321(2) Uani 1 1 d . . . O1 O -0.0242(11) -0.2174(6) -1.0493(3) 0.0447(17) Uani 1 1 d . . . N1 N -0.0344(11) -0.3438(6) -0.9515(4) 0.0318(16) Uani 1 1 d . . . C1 C 0.0425(17) -0.0757(8) -0.8258(7) 0.055(3) Uani 1 1 d . . . H1B H 0.1101 -0.0646 -0.7818 0.083 Uiso 1 1 calc R . . H1C H -0.0758 -0.0539 -0.8163 0.083 Uiso 1 1 calc R . . H1D H 0.0883 -0.0271 -0.8646 0.083 Uiso 1 1 calc R . . C2 C -0.007(2) -0.2869(10) -0.7864(6) 0.065(4) Uani 1 1 d . . . H2A H 0.0643 -0.2732 -0.7438 0.097 Uiso 1 1 calc R . . H2B H 0.0041 -0.3679 -0.8017 0.097 Uiso 1 1 calc R . . H2C H -0.1261 -0.2708 -0.7742 0.097 Uiso 1 1 calc R . . C3 C 0.0503(13) -0.2055(8) -0.8490(5) 0.035(2) Uani 1 1 d . . . H3A H 0.1714 -0.2243 -0.8605 0.042 Uiso 1 1 calc R . . C4 C -0.0575(12) -0.2236(9) -0.9205(5) 0.034(2) Uani 1 1 d . . . H4A H -0.1804 -0.2131 -0.9083 0.041 Uiso 1 1 calc R . . C5 C -0.0134(14) -0.1408(7) -0.9826(5) 0.038(2) Uani 1 1 d . . . H5A H -0.0959 -0.0761 -0.9854 0.045 Uiso 1 1 calc R . . H5B H 0.1025 -0.1086 -0.9767 0.045 Uiso 1 1 calc R . . C6 C -0.0186(12) -0.3297(7) -1.0197(5) 0.0275(18) Uani 1 1 d . . . C7 C -0.0077(11) -0.4256(9) -1.0756(4) 0.034(2) Uani 1 1 d . . . C8 C 0.0086(11) -0.3981(11) -1.1512(5) 0.040(2) Uani 1 1 d . . . H8A H 0.0116 -0.3194 -1.1663 0.048 Uiso 1 1 calc R . . C9 C 0.0204(15) -0.4889(12) -1.2037(5) 0.050(3) Uani 1 1 d . . . H9A H 0.0343 -0.4709 -1.2535 0.059 Uiso 1 1 calc R . . C10 C 0.0111(14) -0.6051(12) -1.1808(5) 0.050(3) Uani 1 1 d . . . H10A H 0.0117 -0.6657 -1.2155 0.060 Uiso 1 1 calc R . . C11 C 0.0007(15) -0.6319(10) -1.1059(5) 0.049(3) Uani 1 1 d . . . H11A H 0.0016 -0.7108 -1.0913 0.058 Uiso 1 1 calc R . . C12 C -0.0110(13) -0.5434(9) -1.0517(5) 0.036(2) Uani 1 1 d . . . C13 C 0.2036(13) -0.5562(10) -0.8772(6) 0.044(3) Uani 1 1 d . . . H13A H 0.2315 -0.4740 -0.8835 0.067 Uiso 1 1 calc R . . H13B H 0.2978 -0.6039 -0.8951 0.067 Uiso 1 1 calc R . . H13C H 0.1852 -0.5725 -0.8257 0.067 Uiso 1 1 calc R . . C14 C -0.2637(12) -0.5556(9) -0.8820(5) 0.035(2) Uani 1 1 d . . . H14A H -0.2499 -0.4834 -0.8547 0.052 Uiso 1 1 calc R . . H14B H -0.2928 -0.6187 -0.8487 0.052 Uiso 1 1 calc R . . H14C H -0.3548 -0.5462 -0.9176 0.052 Uiso 1 1 calc R . . C15 C -0.0247(15) -0.7880(9) -0.9440(6) 0.047(2) Uani 1 1 d . . . H15A H -0.0293 -0.8206 -0.8951 0.071 Uiso 1 1 calc R . . H15B H 0.0796 -0.8139 -0.9681 0.071 Uiso 1 1 calc R . . H15C H -0.1237 -0.8143 -0.9717 0.071 Uiso 1 1 calc R . . 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 Sn1 0.0343(3) 0.0312(3) 0.0306(3) -0.0005(3) 0.0007(3) 0.0003(3) O1 0.064(5) 0.032(3) 0.038(4) 0.012(3) -0.006(4) 0.001(4) N1 0.034(4) 0.027(3) 0.035(4) -0.001(3) 0.002(4) -0.002(4) C1 0.067(7) 0.029(5) 0.070(7) -0.001(5) -0.002(7) -0.006(6) C2 0.108(12) 0.049(6) 0.037(5) -0.001(5) 0.014(7) -0.013(8) C3 0.035(5) 0.034(4) 0.034(4) -0.007(4) 0.000(4) 0.000(5) C4 0.022(5) 0.041(5) 0.039(5) -0.004(4) -0.012(4) -0.001(4) C5 0.045(6) 0.020(4) 0.047(5) 0.005(4) -0.007(5) -0.002(4) C6 0.024(4) 0.026(4) 0.033(4) 0.006(3) -0.003(4) 0.004(4) C7 0.022(4) 0.055(6) 0.024(4) -0.007(4) 0.000(3) 0.001(4) C8 0.030(5) 0.064(6) 0.026(4) 0.006(5) -0.003(4) -0.003(6) C9 0.041(6) 0.083(8) 0.024(4) -0.002(5) 0.001(4) 0.000(7) C10 0.052(7) 0.079(8) 0.020(4) -0.020(5) 0.013(4) -0.004(8) C11 0.056(7) 0.057(6) 0.033(5) -0.007(4) -0.001(5) 0.003(6) C12 0.034(5) 0.042(5) 0.032(5) -0.004(4) -0.007(4) 0.001(4) C13 0.042(6) 0.054(7) 0.037(5) -0.003(5) 0.000(4) 0.011(5) C14 0.037(5) 0.043(6) 0.026(4) -0.004(4) 0.007(4) -0.004(4) C15 0.058(6) 0.037(5) 0.047(5) 0.004(5) 0.016(7) 0.006(5) _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 Sn1 C13 2.133(10) . ? Sn1 C14 2.139(9) . ? Sn1 C12 2.157(9) . ? Sn1 C15 2.161(10) . ? O1 C6 1.378(10) . ? O1 C5 1.488(11) . ? N1 C6 1.250(11) . ? N1 C4 1.480(11) . ? C1 C3 1.526(13) . ? C2 C3 1.525(14) . ? C3 C4 1.552(12) . ? C4 C5 1.502(13) . ? C6 C7 1.485(12) . ? C7 C12 1.399(13) . ? C7 C8 1.409(11) . ? C8 C9 1.402(15) . ? C9 C10 1.378(17) . ? C10 C11 1.393(13) . ? C11 C12 1.404(14) . ? 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 C13 Sn1 C14 115.0(4) . . ? C13 Sn1 C12 112.7(4) . . ? C14 Sn1 C12 115.9(4) . . ? C13 Sn1 C15 103.8(4) . . ? C14 Sn1 C15 104.4(4) . . ? C12 Sn1 C15 103.2(4) . . ? C6 O1 C5 102.6(6) . . ? C6 N1 C4 105.6(7) . . ? C2 C3 C1 111.3(9) . . ? C2 C3 C4 112.7(9) . . ? C1 C3 C4 109.6(9) . . ? N1 C4 C5 105.1(7) . . ? N1 C4 C3 111.9(8) . . ? C5 C4 C3 115.0(8) . . ? O1 C5 C4 103.5(7) . . ? N1 C6 O1 119.9(8) . . ? N1 C6 C7 125.9(8) . . ? O1 C6 C7 114.0(7) . . ? C12 C7 C8 120.8(9) . . ? C12 C7 C6 118.7(7) . . ? C8 C7 C6 120.5(9) . . ? C9 C8 C7 120.3(11) . . ? C10 C9 C8 119.3(9) . . ? C9 C10 C11 120.2(10) . . ? C10 C11 C12 122.0(11) . . ? C7 C12 C11 117.4(9) . . ? C7 C12 Sn1 124.3(6) . . ? C11 C12 Sn1 118.3(7) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.413 _refine_diff_density_min -1.775 _refine_diff_density_rms 0.212 #===END data_5 _database_code_CSD 181360 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 Cl N O Sn' _chemical_formula_weight 372.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.570(2) _cell_length_b 13.984(5) _cell_length_c 14.563(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1541.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 38 _cell_measurement_theta_min 5.41 _cell_measurement_theta_max 12.44 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 744 _exptl_absorpt_coefficient_mu 1.820 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.465 _exptl_absorpt_correction_T_max 0.771 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 5721 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.01 _reflns_number_total 2797 _reflns_number_gt 2475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XSCANS (Fait, 1991)' _computing_cell_refinement 'XSCANS (Fait, 1991)' _computing_data_reduction 'XSCANS (Fait, 1991)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_number_reflns 2797 _refine_ls_number_parameters 163 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.72852(4) 0.28730(2) 0.23593(2) 0.02717(12) Uani 1 1 d . . . Cl1 Cl 0.7323(3) 0.16090(10) 0.35689(10) 0.0435(4) Uani 1 1 d . . . O1 O 0.7008(7) 0.3727(3) -0.0539(3) 0.0415(12) Uani 1 1 d . . . N1 N 0.7149(7) 0.3890(3) 0.0992(3) 0.0289(10) Uani 1 1 d . . . C1 C 0.7615(10) 0.5769(4) 0.2107(4) 0.0437(15) Uani 1 1 d . . . H1A H 0.7766 0.5174 0.2426 0.066 Uiso 1 1 calc R . . H1B H 0.6416 0.5982 0.2173 0.066 Uiso 1 1 calc R . . H1C H 0.8398 0.6239 0.2362 0.066 Uiso 1 1 calc R . . C2 C 0.7802(12) 0.6586(4) 0.0580(4) 0.0494(18) Uani 1 1 d . . . H2A H 0.8070 0.6501 -0.0059 0.074 Uiso 1 1 calc R . . H2B H 0.8587 0.7054 0.0838 0.074 Uiso 1 1 calc R . . H2C H 0.6604 0.6801 0.0645 0.074 Uiso 1 1 calc R . . C3 C 0.8036(8) 0.5629(4) 0.1088(4) 0.0335(13) Uani 1 1 d . . . H3A H 0.9270 0.5427 0.1030 0.040 Uiso 1 1 calc R . . C4 C 0.6869(8) 0.4873(4) 0.0655(4) 0.0301(13) Uani 1 1 d . . . H4A H 0.5634 0.5048 0.0766 0.036 Uiso 1 1 calc R . . C5 C 0.7135(11) 0.4756(4) -0.0384(4) 0.0402(15) Uani 1 1 d . . . H5A H 0.6227 0.5095 -0.0722 0.048 Uiso 1 1 calc R . . H5B H 0.8283 0.4995 -0.0570 0.048 Uiso 1 1 calc R . . C6 C 0.7155(8) 0.3336(4) 0.0296(4) 0.0318(13) Uani 1 1 d . . . C7 C 0.7234(8) 0.2279(4) 0.0350(4) 0.0327(12) Uani 1 1 d . . . C8 C 0.7255(9) 0.1720(4) -0.0436(4) 0.0431(15) Uani 1 1 d . . . H8A H 0.7234 0.1999 -0.1016 0.052 Uiso 1 1 calc R . . C9 C 0.7307(10) 0.0730(5) -0.0336(5) 0.0468(17) Uani 1 1 d . . . H9A H 0.7314 0.0342 -0.0854 0.056 Uiso 1 1 calc R . . C10 C 0.7349(9) 0.0324(4) 0.0518(5) 0.0448(16) Uani 1 1 d . . . H10A H 0.7388 -0.0338 0.0574 0.054 Uiso 1 1 calc R . . C11 C 0.7335(9) 0.0882(4) 0.1294(4) 0.0396(14) Uani 1 1 d . . . H11A H 0.7370 0.0592 0.1868 0.048 Uiso 1 1 calc R . . C12 C 0.7269(9) 0.1882(4) 0.1234(3) 0.0305(12) Uani 1 1 d . . . C13 C 0.4891(7) 0.3502(5) 0.2820(5) 0.0382(16) Uani 1 1 d . . . H13A H 0.4600 0.4036 0.2434 0.057 Uiso 1 1 calc R . . H13B H 0.5032 0.3718 0.3441 0.057 Uiso 1 1 calc R . . H13C H 0.3960 0.3037 0.2793 0.057 Uiso 1 1 calc R . . C14 C 0.9782(7) 0.3457(4) 0.2724(5) 0.0363(14) Uani 1 1 d . . . H14A H 1.0054 0.3983 0.2325 0.054 Uiso 1 1 calc R . . H14B H 1.0675 0.2974 0.2664 0.054 Uiso 1 1 calc R . . H14C H 0.9744 0.3677 0.3348 0.054 Uiso 1 1 calc R . . 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 Sn1 0.02974(18) 0.02344(18) 0.02832(19) -0.00042(14) 0.00026(15) 0.00050(16) Cl1 0.0514(10) 0.0338(7) 0.0451(8) 0.0121(6) 0.0005(9) 0.0023(9) O1 0.060(3) 0.039(2) 0.025(2) -0.0014(17) -0.003(2) 0.001(2) N1 0.033(3) 0.023(2) 0.030(2) 0.0013(18) 0.001(2) -0.001(2) C1 0.069(4) 0.030(3) 0.033(3) 0.002(2) -0.002(3) -0.001(3) C2 0.072(5) 0.029(3) 0.047(3) 0.009(3) 0.009(4) -0.003(4) C3 0.034(3) 0.030(3) 0.037(3) 0.002(2) -0.001(3) 0.003(3) C4 0.034(3) 0.029(3) 0.027(3) 0.006(2) 0.002(3) 0.000(3) C5 0.053(4) 0.038(3) 0.030(3) 0.005(2) -0.004(4) -0.001(3) C6 0.032(3) 0.035(3) 0.028(3) 0.000(2) -0.006(3) -0.003(3) C7 0.029(3) 0.034(3) 0.035(3) -0.008(2) 0.004(3) -0.004(3) C8 0.044(4) 0.046(3) 0.038(3) -0.014(3) -0.001(3) -0.002(3) C9 0.037(4) 0.047(4) 0.056(4) -0.027(3) 0.013(4) 0.000(4) C10 0.045(4) 0.027(3) 0.063(4) -0.010(3) 0.011(4) -0.007(3) C11 0.043(4) 0.026(3) 0.050(3) -0.002(2) 0.015(4) 0.004(3) C12 0.031(3) 0.028(3) 0.033(3) -0.003(2) 0.002(3) -0.006(3) C13 0.030(3) 0.042(4) 0.042(4) -0.001(3) 0.004(3) 0.005(3) C14 0.035(3) 0.036(3) 0.038(4) -0.002(3) -0.004(3) -0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C13 2.123(5) . ? Sn1 C14 2.126(5) . ? Sn1 C12 2.146(5) . ? Sn1 N1 2.449(4) . ? Sn1 Cl1 2.4957(15) . ? O1 C6 1.338(7) . ? O1 C5 1.460(7) . ? N1 C6 1.276(7) . ? N1 C4 1.475(7) . ? C1 C3 1.531(8) . ? C2 C3 1.539(8) . ? C3 C4 1.515(8) . ? C4 C5 1.535(8) . ? C6 C7 1.481(7) . ? C7 C8 1.386(7) . ? C7 C12 1.403(8) . ? C8 C9 1.393(9) . ? C9 C10 1.368(9) . ? C10 C11 1.373(8) . ? C11 C12 1.402(7) . ? 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 C13 Sn1 C14 121.4(2) . . ? C13 Sn1 C12 120.3(3) . . ? C14 Sn1 C12 116.3(3) . . ? C13 Sn1 N1 88.9(2) . . ? C14 Sn1 N1 91.0(2) . . ? C12 Sn1 N1 75.78(17) . . ? C13 Sn1 Cl1 94.61(19) . . ? C14 Sn1 Cl1 94.89(19) . . ? C12 Sn1 Cl1 94.67(15) . . ? N1 Sn1 Cl1 170.29(11) . . ? C6 O1 C5 104.9(4) . . ? C6 N1 C4 107.6(4) . . ? C6 N1 Sn1 107.0(3) . . ? C4 N1 Sn1 144.9(3) . . ? C4 C3 C1 111.8(5) . . ? C4 C3 C2 109.9(5) . . ? C1 C3 C2 109.3(5) . . ? N1 C4 C3 115.4(5) . . ? N1 C4 C5 102.1(4) . . ? C3 C4 C5 114.1(5) . . ? O1 C5 C4 104.4(4) . . ? N1 C6 O1 118.2(5) . . ? N1 C6 C7 124.4(5) . . ? O1 C6 C7 117.3(5) . . ? C8 C7 C12 122.3(5) . . ? C8 C7 C6 121.3(5) . . ? C12 C7 C6 116.4(5) . . ? C7 C8 C9 118.3(6) . . ? C10 C9 C8 120.6(6) . . ? C9 C10 C11 120.8(6) . . ? C10 C11 C12 121.1(6) . . ? C11 C12 C7 116.9(5) . . ? C11 C12 Sn1 126.6(4) . . ? C7 C12 Sn1 116.4(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.539 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.117 #===END data_2061 _database_code_CSD 181361 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H34 N2 O6 Pd2' _chemical_formula_weight 707.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.6973(15) _cell_length_b 15.045(3) _cell_length_c 21.616(3) _cell_angle_alpha 83.799(13) _cell_angle_beta 83.044(13) _cell_angle_gamma 73.291(13) _cell_volume 2989.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 40 _cell_measurement_theta_min 10.466 _cell_measurement_theta_max 24.984 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.572 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 1.244 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.56 _exptl_absorpt_correction_T_max 0.77 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <1 _diffrn_reflns_number 11177 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11177 _reflns_number_gt 9121 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1134P)^2^+6.1232P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(5) _refine_ls_number_reflns 11177 _refine_ls_number_parameters 1369 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0860 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1801 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.267 _refine_ls_shift/su_mean 0.029 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1A Pd 0.12837(14) 0.55334(9) 0.35620(7) 0.0556(4) Uani 1 1 d . . . Pd2A Pd 0.03398(13) 0.73181(9) 0.40632(6) 0.0481(3) Uani 1 1 d . . . O1A O -0.1191(13) 0.7436(9) 0.3418(7) 0.056(3) Uani 1 1 d . . . O2A O -0.0233(16) 0.6100(10) 0.2935(7) 0.065(3) Uani 1 1 d . . . O3A O -0.0868(14) 0.6767(10) 0.4757(6) 0.065(4) Uani 1 1 d . . . O4A O -0.0333(14) 0.5403(9) 0.4296(7) 0.066(4) Uani 1 1 d . . . O5A O 0.5204(13) 0.4859(9) 0.4224(9) 0.076(4) Uani 1 1 d . . . O6A O 0.3882(13) 0.8025(10) 0.3233(7) 0.064(4) Uani 1 1 d . . . N1A N 0.2889(15) 0.5008(9) 0.4112(7) 0.052(4) Uani 1 1 d . . . N2A N 0.1684(14) 0.7823(10) 0.3443(7) 0.048(3) Uani 1 1 d . . . C1A C -0.109(2) 0.6875(16) 0.3008(10) 0.065(6) Uani 1 1 d . . . C2A C -0.219(3) 0.724(2) 0.2513(14) 0.104(9) Uani 1 1 d . . . H2AA H -0.2061 0.6781 0.2221 0.156 Uiso 1 1 calc R . . H2AB H -0.2046 0.7804 0.2295 0.156 Uiso 1 1 calc R . . H2AC H -0.3158 0.7370 0.2718 0.156 Uiso 1 1 calc R . . C3A C -0.092(2) 0.5934(16) 0.4705(11) 0.072(7) Uani 1 1 d . . . C4A C -0.190(2) 0.5591(19) 0.5250(13) 0.100(10) Uani 1 1 d . . . H4AA H -0.1919 0.4971 0.5189 0.151 Uiso 1 1 calc R . . H4AB H -0.2868 0.6000 0.5255 0.151 Uiso 1 1 calc R . . H4AC H -0.1526 0.5590 0.5641 0.151 Uiso 1 1 calc R . . C5A C 0.304(2) 0.4689(16) 0.4755(12) 0.072(6) Uani 1 1 d . . . H5AA H 0.2326 0.5128 0.5018 0.086 Uiso 1 1 calc R . . C6A C 0.456(2) 0.4721(17) 0.4855(11) 0.074(6) Uani 1 1 d . . . H6AA H 0.4518 0.5233 0.5100 0.089 Uiso 1 1 calc R . . H6AB H 0.5093 0.4143 0.5063 0.089 Uiso 1 1 calc R . . C7A C 0.415(2) 0.5106(14) 0.3863(11) 0.066(5) Uani 1 1 d . . . C8A C 0.425(3) 0.5379(15) 0.3202(13) 0.085(8) Uani 1 1 d . . . C9A C 0.557(3) 0.5455(14) 0.2826(16) 0.104(11) Uani 1 1 d . . . H9AA H 0.6438 0.5353 0.2999 0.125 Uiso 1 1 calc R . . C10A C 0.544(4) 0.5692(18) 0.2187(18) 0.125(15) Uani 1 1 d . . . H10B H 0.6251 0.5720 0.1918 0.150 Uiso 1 1 calc R . . C11A C 0.418(4) 0.5874(19) 0.1962(14) 0.099(10) Uani 1 1 d . . . H11B H 0.4145 0.6057 0.1538 0.119 Uiso 1 1 calc R . . C12A C 0.289(3) 0.5820(13) 0.2300(9) 0.079(7) Uani 1 1 d . . . H12B H 0.2047 0.5942 0.2105 0.095 Uiso 1 1 calc R . . C13A C 0.290(3) 0.5574(13) 0.2948(11) 0.070(6) Uani 1 1 d . . . C14A C 0.275(2) 0.3700(15) 0.4881(11) 0.073(7) Uani 1 1 d . . . H14B H 0.1771 0.3771 0.4774 0.087 Uiso 1 1 calc R . . C15A C 0.278(3) 0.339(2) 0.5592(12) 0.099(8) Uani 1 1 d . . . H15D H 0.2596 0.2796 0.5671 0.149 Uiso 1 1 calc R . . H15E H 0.2047 0.3842 0.5824 0.149 Uiso 1 1 calc R . . H15F H 0.3711 0.3356 0.5720 0.149 Uiso 1 1 calc R . . C16A C 0.377(2) 0.3008(13) 0.4467(14) 0.088(8) Uani 1 1 d . . . H16D H 0.3664 0.3231 0.4037 0.132 Uiso 1 1 calc R . . H16E H 0.3543 0.2422 0.4544 0.132 Uiso 1 1 calc R . . H16F H 0.4745 0.2928 0.4555 0.132 Uiso 1 1 calc R . . C17A C 0.1677(19) 0.8194(12) 0.2806(8) 0.049(4) Uani 1 1 d . . . H17B H 0.1485 0.7743 0.2557 0.059 Uiso 1 1 calc R . . C18A C 0.3294(16) 0.8198(13) 0.2640(10) 0.054(5) Uani 1 1 d . . . H18C H 0.3800 0.7714 0.2365 0.064 Uiso 1 1 calc R . . H18D H 0.3357 0.8796 0.2439 0.064 Uiso 1 1 calc R . . C19A C 0.288(2) 0.7787(11) 0.3649(9) 0.052(4) Uani 1 1 d . . . C20A C 0.305(2) 0.7493(12) 0.4311(8) 0.051(4) Uani 1 1 d . . . C21A C 0.425(3) 0.7452(14) 0.4606(11) 0.078(6) Uani 1 1 d . . . H21C H 0.5045 0.7585 0.4374 0.093 Uiso 1 1 calc R . . C22A C 0.428(4) 0.7218(17) 0.5243(12) 0.099(10) Uani 1 1 d . . . H22B H 0.5049 0.7234 0.5459 0.119 Uiso 1 1 calc R . . C23A C 0.304(3) 0.6948(18) 0.5541(11) 0.082(7) Uani 1 1 d . . . H23B H 0.3058 0.6714 0.5958 0.098 Uiso 1 1 calc R . . C24A C 0.185(2) 0.7011(14) 0.5255(9) 0.064(5) Uani 1 1 d . . . H24B H 0.1043 0.6882 0.5484 0.077 Uiso 1 1 calc R . . C25A C 0.1820(19) 0.7276(12) 0.4607(9) 0.054(4) Uani 1 1 d . . . C26A C 0.0533(18) 0.9130(12) 0.2697(8) 0.050(4) Uani 1 1 d . . . H26B H -0.0412 0.9036 0.2850 0.060 Uiso 1 1 calc R . . C27A C 0.076(2) 0.9837(13) 0.3068(9) 0.064(5) Uani 1 1 d . . . H27D H 0.0031 1.0415 0.2998 0.095 Uiso 1 1 calc R . . H27E H 0.1697 0.9924 0.2945 0.095 Uiso 1 1 calc R . . H27F H 0.0690 0.9631 0.3504 0.095 Uiso 1 1 calc R . . C28A C 0.051(2) 0.9421(16) 0.2004(9) 0.066(5) Uani 1 1 d . . . H28D H -0.0216 1.0004 0.1942 0.099 Uiso 1 1 calc R . . H28E H 0.0283 0.8955 0.1795 0.099 Uiso 1 1 calc R . . H28F H 0.1437 0.9489 0.1835 0.099 Uiso 1 1 calc R . . Pd1B Pd 0.97265(12) 0.21796(8) 0.61737(6) 0.0436(3) Uani 1 1 d . . . Pd2B Pd 0.69397(13) 0.21618(11) 0.59114(7) 0.0602(4) Uani 1 1 d . . . O1B O 0.6505(16) 0.3349(9) 0.6433(8) 0.079(5) Uani 1 1 d . . . O2B O 0.8786(17) 0.3450(9) 0.6495(7) 0.074(4) Uani 1 1 d . . . O3B O 0.7384(14) 0.2952(12) 0.5132(8) 0.085(5) Uani 1 1 d . . . O4B O 0.9688(13) 0.2774(8) 0.5241(5) 0.052(3) Uani 1 1 d . . . O5B O 1.1192(16) -0.0639(10) 0.6250(8) 0.073(4) Uani 1 1 d . . . O6B O 0.6690(15) -0.0273(10) 0.6891(6) 0.064(3) Uani 1 1 d . . . N1B N 1.0632(12) 0.0883(9) 0.5933(6) 0.040(3) Uani 1 1 d . . . N2B N 0.6590(16) 0.1226(13) 0.6612(8) 0.064(5) Uani 1 1 d . . . C1B C 0.742(3) 0.3746(16) 0.6567(12) 0.085(8) Uani 1 1 d . . . C2B C 0.672(3) 0.4719(16) 0.6780(15) 0.111(10) Uani 1 1 d . . . H2BA H 0.7452 0.4984 0.6874 0.167 Uiso 1 1 calc R . . H2BB H 0.6066 0.4685 0.7148 0.167 Uiso 1 1 calc R . . H2BC H 0.6192 0.5103 0.6454 0.167 Uiso 1 1 calc R . . C3B C 0.8629(18) 0.3033(13) 0.4924(9) 0.055(5) Uani 1 1 d . . . C4B C 0.880(2) 0.3448(15) 0.4289(9) 0.067(5) Uani 1 1 d . . . H4BA H 0.9791 0.3453 0.4185 0.101 Uiso 1 1 calc R . . H4BB H 0.8186 0.4074 0.4260 0.101 Uiso 1 1 calc R . . H4BC H 0.8544 0.3090 0.4003 0.101 Uiso 1 1 calc R . . C5B C 1.1099(16) 0.0441(12) 0.5348(9) 0.051(4) Uani 1 1 d . . . H5BA H 1.0297 0.0643 0.5083 0.061 Uiso 1 1 calc R . . C6B C 1.132(2) -0.0614(13) 0.5560(11) 0.067(6) Uani 1 1 d . . . H6BA H 1.0579 -0.0842 0.5419 0.081 Uiso 1 1 calc R . . H6BB H 1.2262 -0.0986 0.5401 0.081 Uiso 1 1 calc R . . C7B C 1.0723(16) 0.0250(11) 0.6390(9) 0.048(4) Uani 1 1 d . . . C8B C 1.0316(18) 0.0557(13) 0.7019(8) 0.049(4) Uani 1 1 d . . . C9B C 1.043(2) -0.0020(15) 0.7560(11) 0.070(6) Uani 1 1 d . . . H9BA H 1.0736 -0.0664 0.7546 0.084 Uiso 1 1 calc R . . C10B C 1.007(2) 0.0379(15) 0.8123(9) 0.064(5) Uani 1 1 d . . . H10C H 1.0108 0.0007 0.8497 0.077 Uiso 1 1 calc R . . C11B C 0.965(2) 0.1332(19) 0.8127(10) 0.076(6) Uani 1 1 d . . . H11C H 0.9452 0.1604 0.8506 0.091 Uiso 1 1 calc R . . C12B C 0.951(2) 0.1895(16) 0.7570(8) 0.065(5) Uani 1 1 d . . . H12C H 0.9192 0.2538 0.7584 0.078 Uiso 1 1 calc R . . C13B C 0.9850(17) 0.1518(13) 0.7002(8) 0.047(4) Uani 1 1 d . . . C14B C 1.238(2) 0.0723(14) 0.5003(9) 0.057(4) Uani 1 1 d . . . H14C H 1.2103 0.1405 0.4964 0.068 Uiso 1 1 calc R . . C15B C 1.262(3) 0.041(2) 0.4346(11) 0.097(8) Uani 1 1 d . . . H15G H 1.1738 0.0639 0.4149 0.146 Uiso 1 1 calc R . . H15H H 1.2929 -0.0256 0.4362 0.146 Uiso 1 1 calc R . . H15I H 1.3356 0.0655 0.4109 0.146 Uiso 1 1 calc R . . C16B C 1.369(2) 0.0415(18) 0.5351(12) 0.080(7) Uani 1 1 d . . . H16G H 1.3462 0.0636 0.5762 0.119 Uiso 1 1 calc R . . H16H H 1.4439 0.0662 0.5131 0.119 Uiso 1 1 calc R . . H16I H 1.4026 -0.0253 0.5385 0.119 Uiso 1 1 calc R . . C17B C 0.610(2) 0.1250(14) 0.7292(8) 0.055(5) Uani 1 1 d . . . H17C H 0.6719 0.1497 0.7509 0.066 Uiso 1 1 calc R . . C18B C 0.637(2) 0.0192(14) 0.7464(9) 0.062(5) Uani 1 1 d . . . H18E H 0.7181 -0.0034 0.7718 0.074 Uiso 1 1 calc R . . H18F H 0.5525 0.0067 0.7702 0.074 Uiso 1 1 calc R . . C19B C 0.6823(19) 0.0390(15) 0.6439(9) 0.057(5) Uani 1 1 d . . . C20B C 0.7209(19) 0.0266(16) 0.5776(10) 0.065(5) Uani 1 1 d . . . C21B C 0.747(2) -0.058(2) 0.5530(12) 0.091(8) Uani 1 1 d . . . H21D H 0.7429 -0.1117 0.5782 0.109 Uiso 1 1 calc R . . C22B C 0.780(2) -0.060(2) 0.4852(11) 0.095(10) Uani 1 1 d . . . H22C H 0.8004 -0.1141 0.4648 0.114 Uiso 1 1 calc R . . C23B C 0.779(2) 0.028(2) 0.4525(13) 0.086(7) Uani 1 1 d . . . H23C H 0.8008 0.0287 0.4094 0.104 Uiso 1 1 calc R . . C24B C 0.751(2) 0.107(2) 0.4776(12) 0.080(7) Uani 1 1 d . . . H24C H 0.7515 0.1595 0.4506 0.095 Uiso 1 1 calc R . . C25B C 0.719(2) 0.121(3) 0.5451(10) 0.108(12) Uani 1 1 d . . . C26B C 0.453(2) 0.1811(15) 0.7410(8) 0.059(5) Uani 1 1 d . . . H26C H 0.4475 0.2451 0.7244 0.071 Uiso 1 1 calc R . . C27B C 0.355(2) 0.150(2) 0.7075(11) 0.083(7) Uani 1 1 d . . . H27G H 0.3875 0.1501 0.6638 0.124 Uiso 1 1 calc R . . H27H H 0.2591 0.1914 0.7133 0.124 Uiso 1 1 calc R . . H27I H 0.3537 0.0882 0.7236 0.124 Uiso 1 1 calc R . . C28B C 0.408(3) 0.184(2) 0.8113(10) 0.093(8) Uani 1 1 d . . . H28G H 0.3090 0.2203 0.8181 0.140 Uiso 1 1 calc R . . H28H H 0.4686 0.2125 0.8299 0.140 Uiso 1 1 calc R . . H28I H 0.4187 0.1222 0.8301 0.140 Uiso 1 1 calc R . . Pd1C Pd 0.04724(14) 0.78318(10) 0.85709(7) 0.0539(4) Uani 1 1 d . . . Pd2C Pd -0.06237(18) 0.62557(11) 0.85645(9) 0.0727(5) Uani 1 1 d . . . O1C O -0.2539(14) 0.7277(10) 0.8949(7) 0.068(4) Uani 1 1 d . . . O2C O -0.1661(14) 0.8530(9) 0.8767(7) 0.062(3) Uani 1 1 d . . . O3C O -0.1153(18) 0.6739(12) 0.7689(8) 0.084(5) Uani 1 1 d . . . O4C O 0.0142(16) 0.7777(11) 0.7631(7) 0.073(4) Uani 1 1 d . . . O5C O 0.4631(14) 0.6666(11) 0.8978(7) 0.071(4) Uani 1 1 d . . . O6C O 0.201(3) 0.4894(18) 0.9804(16) 0.145(10) Uani 1 1 d . . . N1C N 0.2617(16) 0.7225(11) 0.8469(9) 0.063(4) Uani 1 1 d . . . N2C N 0.007(3) 0.5690(13) 0.9370(11) 0.092(7) Uani 1 1 d . . . C1C C -0.263(2) 0.8092(15) 0.8947(8) 0.057(5) Uani 1 1 d . . . C2C C -0.408(2) 0.8722(17) 0.9151(10) 0.070(6) Uani 1 1 d . . . H2CA H -0.4753 0.8359 0.9275 0.105 Uiso 1 1 calc R . . H2CB H -0.4428 0.9164 0.8810 0.105 Uiso 1 1 calc R . . H2CC H -0.4004 0.9048 0.9497 0.105 Uiso 1 1 calc R . . C3C C -0.056(2) 0.7378(16) 0.7374(10) 0.063(5) Uani 1 1 d . . . C4C C -0.085(3) 0.756(2) 0.6723(12) 0.095(8) Uani 1 1 d . . . H4CA H -0.0415 0.8040 0.6533 0.142 Uiso 1 1 calc R . . H4CB H -0.1871 0.7770 0.6694 0.142 Uiso 1 1 calc R . . H4CC H -0.0437 0.7007 0.6510 0.142 Uiso 1 1 calc R . . C5C C 0.373(2) 0.6871(15) 0.7970(9) 0.057(5) Uani 1 1 d . . . H5CA H 0.3484 0.6374 0.7788 0.068 Uiso 1 1 calc R . . C6C C 0.507(2) 0.6445(16) 0.8312(12) 0.079(7) Uani 1 1 d . . . H6CA H 0.5403 0.5777 0.8281 0.095 Uiso 1 1 calc R . . H6CB H 0.5848 0.6713 0.8137 0.095 Uiso 1 1 calc R . . C7C C 0.316(2) 0.7091(16) 0.9003(10) 0.065(5) Uani 1 1 d . . . C8C C 0.231(2) 0.7448(15) 0.9560(9) 0.062(5) Uani 1 1 d . . . C9C C 0.283(3) 0.740(2) 1.0128(12) 0.090(7) Uani 1 1 d . . . H9CA H 0.3802 0.7131 1.0189 0.108 Uiso 1 1 calc R . . C10C C 0.185(3) 0.778(2) 1.0592(11) 0.099(9) Uani 1 1 d . . . H10D H 0.2142 0.7743 1.0991 0.118 Uiso 1 1 calc R . . C11C C 0.043(3) 0.821(2) 1.0495(10) 0.088(8) Uani 1 1 d . . . H11D H -0.0190 0.8494 1.0824 0.105 Uiso 1 1 calc R . . C12C C -0.009(2) 0.8253(13) 0.9935(9) 0.059(5) Uani 1 1 d . . . H12D H -0.1072 0.8507 0.9889 0.071 Uiso 1 1 calc R . . C13C C 0.089(2) 0.7895(13) 0.9424(10) 0.061(5) Uani 1 1 d . . . C14C C 0.387(2) 0.7633(14) 0.7446(9) 0.061(5) Uani 1 1 d . . . H14D H 0.2943 0.7872 0.7266 0.074 Uiso 1 1 calc R . . C15C C 0.500(3) 0.7200(18) 0.6941(10) 0.086(7) Uani 1 1 d . . . H15J H 0.5102 0.7668 0.6614 0.128 Uiso 1 1 calc R . . H15K H 0.4718 0.6721 0.6775 0.128 Uiso 1 1 calc R . . H15L H 0.5913 0.6934 0.7114 0.128 Uiso 1 1 calc R . . C16C C 0.423(2) 0.8446(14) 0.7697(10) 0.066(5) Uani 1 1 d . . . H16J H 0.3494 0.8701 0.8020 0.098 Uiso 1 1 calc R . . H16K H 0.4259 0.8918 0.7364 0.098 Uiso 1 1 calc R . . H16L H 0.5148 0.8230 0.7864 0.098 Uiso 1 1 calc R . . C17C C -0.042(3) 0.5741(19) 0.9993(17) 0.107(10) Uani 1 1 d . . . H17D H -0.0902 0.6387 1.0083 0.129 Uiso 1 1 calc R . . C18C C 0.121(4) 0.534(2) 1.0330(14) 0.119(12) Uani 1 1 d . . . H18G H 0.1568 0.5848 1.0430 0.142 Uiso 1 1 calc R . . H18H H 0.1169 0.4916 1.0696 0.142 Uiso 1 1 calc R . . C19C C 0.142(3) 0.5177(16) 0.9311(16) 0.102(10) Uani 1 1 d . . . C20C C 0.205(3) 0.494(2) 0.8696(15) 0.088(8) Uani 1 1 d . . . C21C C 0.358(4) 0.4369(19) 0.852(2) 0.134(15) Uani 1 1 d . . . H21E H 0.4229 0.4169 0.8824 0.161 Uiso 1 1 calc R . . C22C C 0.396(4) 0.417(2) 0.798(2) 0.122(12) Uani 1 1 d . . . H22E H 0.4868 0.3761 0.7895 0.147 Uiso 1 1 calc R . . C23C C 0.300(5) 0.457(3) 0.745(2) 0.148(17) Uani 1 1 d . . . H23D H 0.3289 0.4441 0.7037 0.177 Uiso 1 1 calc R . . C24C C 0.170(4) 0.512(2) 0.7640(18) 0.120(12) Uani 1 1 d . . . H24D H 0.1084 0.5376 0.7328 0.144 Uiso 1 1 calc R . . C25C C 0.116(4) 0.5364(17) 0.8228(19) 0.110(10) Uani 1 1 d . . . C26C C -0.142(5) 0.510(5) 1.024(2) 0.18(2) Uani 1 1 d . . . H26D H -0.1005 0.4443 1.0157 0.218 Uiso 1 1 calc R . . C27C C -0.288(7) 0.557(3) 0.998(2) 0.19(3) Uani 1 1 d . . . H27J H -0.3537 0.5203 1.0126 0.290 Uiso 1 1 calc R . . H27K H -0.2757 0.5617 0.9535 0.290 Uiso 1 1 calc R . . H27L H -0.3263 0.6179 1.0131 0.290 Uiso 1 1 calc R . . C28C C -0.196(5) 0.525(3) 1.082(3) 0.18(2) Uani 1 1 d . . . H28J H -0.2629 0.4890 1.0945 0.271 Uiso 1 1 calc R . . H28K H -0.2459 0.5902 1.0841 0.271 Uiso 1 1 calc R . . H28L H -0.1196 0.5080 1.1087 0.271 Uiso 1 1 calc R . . Pd1D Pd 0.66545(12) 0.05606(8) 0.13606(6) 0.0427(3) Uani 1 1 d . . . Pd2D Pd 0.36862(11) 0.06506(8) 0.17415(6) 0.0407(3) Uani 1 1 d . . . O1D O 0.4566(12) -0.0659(8) 0.1336(6) 0.052(3) Uani 1 1 d . . . O2D O 0.6858(14) -0.0727(9) 0.1078(7) 0.063(3) Uani 1 1 d . . . O3D O 0.4407(12) 0.0075(9) 0.2575(6) 0.052(3) Uani 1 1 d . . . O4D O 0.6746(12) -0.0033(9) 0.2293(6) 0.055(3) Uani 1 1 d . . . O5D O 0.5687(18) 0.3391(8) 0.1222(8) 0.075(4) Uani 1 1 d . . . O6D O 0.204(2) 0.2786(11) 0.0499(9) 0.094(5) Uani 1 1 d . . . N1D N 0.6330(14) 0.1894(8) 0.1556(6) 0.039(3) Uani 1 1 d . . . N2D N 0.2927(15) 0.1375(10) 0.0951(6) 0.046(3) Uani 1 1 d . . . C1D C 0.5866(18) -0.1066(11) 0.1130(7) 0.045(4) Uani 1 1 d . . . C2D C 0.609(2) -0.2027(12) 0.0951(9) 0.062(5) Uani 1 1 d . . . H2A H 0.7080 -0.2280 0.0797 0.093 Uiso 1 1 calc R . . H2B H 0.5475 -0.2014 0.0631 0.093 Uiso 1 1 calc R . . H2C H 0.5850 -0.2409 0.1310 0.093 Uiso 1 1 calc R . . C3D C 0.5712(19) -0.0140(11) 0.2698(8) 0.046(4) Uani 1 1 d . . . C4D C 0.606(2) -0.0553(12) 0.3332(7) 0.052(4) Uani 1 1 d . . . H4A H 0.5182 -0.0586 0.3582 0.079 Uiso 1 1 calc R . . H4B H 0.6510 -0.0174 0.3520 0.079 Uiso 1 1 calc R . . H4C H 0.6703 -0.1168 0.3305 0.079 Uiso 1 1 calc R . . C5D C 0.6068(19) 0.2342(13) 0.2143(9) 0.054(4) Uani 1 1 d . . . H5A H 0.5289 0.2160 0.2412 0.065 Uiso 1 1 calc R . . C6D C 0.553(3) 0.3367(14) 0.1888(13) 0.079(7) Uani 1 1 d . . . H6A H 0.4524 0.3626 0.2038 0.094 Uiso 1 1 calc R . . H6B H 0.6095 0.3732 0.2028 0.094 Uiso 1 1 calc R . . C7D C 0.6123(18) 0.2470(12) 0.1094(10) 0.054(5) Uani 1 1 d . . . C8D C 0.6317(19) 0.2147(14) 0.0488(9) 0.057(5) Uani 1 1 d . . . C9D C 0.629(3) 0.2677(19) -0.0097(12) 0.084(7) Uani 1 1 d . . . H9A H 0.6066 0.3322 -0.0111 0.101 Uiso 1 1 calc R . . C10D C 0.659(3) 0.225(2) -0.0629(11) 0.104(10) Uani 1 1 d . . . H10A H 0.6629 0.2592 -0.1011 0.124 Uiso 1 1 calc R . . C11D C 0.684(3) 0.130(2) -0.0613(10) 0.081(7) Uani 1 1 d . . . H11A H 0.6967 0.1018 -0.0987 0.097 Uiso 1 1 calc R . . C12D C 0.6922(19) 0.0743(15) -0.0059(9) 0.057(5) Uani 1 1 d . . . H12A H 0.7171 0.0099 -0.0068 0.068 Uiso 1 1 calc R . . C13D C 0.6637(18) 0.1131(13) 0.0507(8) 0.047(4) Uani 1 1 d . . . C14D C 0.742(2) 0.2088(16) 0.2480(10) 0.066(5) Uani 1 1 d . . . H14A H 0.7734 0.1408 0.2546 0.079 Uiso 1 1 calc R . . C15D C 0.709(3) 0.246(2) 0.3116(12) 0.103(9) Uani 1 1 d . . . H15A H 0.7956 0.2302 0.3324 0.155 Uiso 1 1 calc R . . H15B H 0.6387 0.2195 0.3358 0.155 Uiso 1 1 calc R . . H15C H 0.6705 0.3126 0.3071 0.155 Uiso 1 1 calc R . . C16D C 0.865(2) 0.238(2) 0.2114(14) 0.095(8) Uani 1 1 d . . . H16A H 0.8828 0.2135 0.1710 0.143 Uiso 1 1 calc R . . H16B H 0.9504 0.2141 0.2332 0.143 Uiso 1 1 calc R . . H16C H 0.8413 0.3045 0.2064 0.143 Uiso 1 1 calc R . . C17D C 0.2902(19) 0.1191(15) 0.0314(8) 0.056(5) Uani 1 1 d . . . H17A H 0.3894 0.0886 0.0151 0.068 Uiso 1 1 calc R . . C18D C 0.246(3) 0.2185(18) -0.0004(10) 0.083(7) Uani 1 1 d . . . H18A H 0.3273 0.2316 -0.0271 0.100 Uiso 1 1 calc R . . H18B H 0.1667 0.2264 -0.0255 0.100 Uiso 1 1 calc R . . C19D C 0.242(2) 0.2246(13) 0.1030(9) 0.057(5) Uani 1 1 d . . . C20D C 0.221(2) 0.2576(14) 0.1643(12) 0.067(6) Uani 1 1 d . . . C21D C 0.153(2) 0.3500(15) 0.1786(15) 0.084(7) Uani 1 1 d . . . H21A H 0.1199 0.3972 0.1480 0.101 Uiso 1 1 calc R . . C22D C 0.138(3) 0.3665(18) 0.2449(16) 0.089(8) Uani 1 1 d . . . H22A H 0.0920 0.4260 0.2571 0.106 Uiso 1 1 calc R . . C23D C 0.188(2) 0.3002(17) 0.2872(12) 0.070(6) Uani 1 1 d . . . H23A H 0.1788 0.3131 0.3289 0.084 Uiso 1 1 calc R . . C24D C 0.256(2) 0.2076(14) 0.2696(10) 0.059(5) Uani 1 1 d . . . H24A H 0.2912 0.1613 0.3005 0.071 Uiso 1 1 calc R . . C25D C 0.2723(18) 0.1852(11) 0.2113(9) 0.049(4) Uani 1 1 d . . . C26D C 0.199(2) 0.0570(16) 0.0247(9) 0.064(5) Uani 1 1 d . . . H26A H 0.2367 -0.0011 0.0500 0.076 Uiso 1 1 calc R . . C27D C 0.041(2) 0.0975(19) 0.0499(10) 0.075(6) Uani 1 1 d . . . H27A H 0.0376 0.1121 0.0923 0.112 Uiso 1 1 calc R . . H27B H -0.0113 0.0528 0.0484 0.112 Uiso 1 1 calc R . . H27C H -0.0010 0.1531 0.0247 0.112 Uiso 1 1 calc R . . C28D C 0.211(2) 0.032(2) -0.0437(10) 0.083(7) Uani 1 1 d . . . H28A H 0.3104 0.0039 -0.0574 0.124 Uiso 1 1 calc R . . H28B H 0.1740 0.0874 -0.0699 0.124 Uiso 1 1 calc R . . H28C H 0.1557 -0.0111 -0.0461 0.124 Uiso 1 1 calc R . . 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 Pd1A 0.0474(8) 0.0422(7) 0.0746(10) 0.0043(6) 0.0048(7) -0.0158(6) Pd2A 0.0449(7) 0.0450(7) 0.0522(8) 0.0061(6) -0.0007(6) -0.0145(6) O1A 0.044(7) 0.048(7) 0.078(8) 0.006(6) -0.012(6) -0.019(6) O2A 0.068(9) 0.054(8) 0.077(9) 0.003(7) -0.019(7) -0.021(7) O3A 0.055(8) 0.063(9) 0.066(8) 0.004(7) 0.013(6) -0.011(7) O4A 0.043(7) 0.049(7) 0.097(10) 0.002(7) 0.012(7) -0.008(6) O5A 0.030(6) 0.050(7) 0.142(14) -0.003(8) -0.001(8) -0.009(6) O6A 0.031(6) 0.072(9) 0.090(10) 0.015(7) -0.010(6) -0.024(6) N1A 0.039(8) 0.038(7) 0.072(10) -0.005(7) 0.002(7) -0.004(6) N2A 0.031(7) 0.059(9) 0.062(9) -0.008(7) -0.015(6) -0.021(6) C1A 0.057(12) 0.069(14) 0.076(14) 0.025(12) -0.014(10) -0.036(11) C2A 0.094(19) 0.13(2) 0.11(2) -0.003(17) -0.055(17) -0.042(18) C3A 0.033(9) 0.068(14) 0.095(16) 0.046(12) 0.006(10) -0.007(9) C4A 0.053(12) 0.101(18) 0.12(2) 0.049(16) 0.035(13) -0.015(12) C5A 0.034(9) 0.073(13) 0.102(17) -0.003(12) 0.003(10) -0.011(9) C6A 0.048(11) 0.082(15) 0.097(17) 0.004(13) -0.007(11) -0.027(11) C7A 0.050(11) 0.056(12) 0.092(15) -0.013(10) 0.005(11) -0.019(9) C8A 0.071(15) 0.056(12) 0.115(19) -0.004(12) 0.055(14) -0.023(11) C9A 0.087(17) 0.042(11) 0.17(3) -0.006(14) 0.066(18) -0.031(11) C10A 0.14(3) 0.062(14) 0.17(3) -0.035(17) 0.12(3) -0.064(18) C11A 0.11(2) 0.085(17) 0.098(19) -0.034(14) 0.071(18) -0.042(16) C12A 0.13(2) 0.043(10) 0.049(11) -0.016(8) 0.023(12) -0.016(12) C13A 0.067(14) 0.042(10) 0.095(16) -0.019(10) 0.010(12) -0.008(9) C14A 0.043(10) 0.070(13) 0.100(16) 0.043(12) -0.027(11) -0.018(10) C15A 0.09(2) 0.11(2) 0.088(18) 0.016(16) -0.002(15) -0.040(17) C16A 0.061(13) 0.036(10) 0.16(2) 0.026(12) -0.020(15) -0.015(10) C17A 0.052(10) 0.053(10) 0.053(10) 0.000(8) 0.002(8) -0.037(8) C18A 0.021(7) 0.055(10) 0.083(13) -0.003(9) 0.005(8) -0.012(7) C19A 0.059(11) 0.031(8) 0.067(11) 0.001(7) -0.001(9) -0.019(8) C20A 0.056(11) 0.046(9) 0.052(10) -0.005(8) -0.019(9) -0.009(8) C21A 0.082(15) 0.054(12) 0.086(16) -0.016(11) -0.022(13) 0.007(11) C22A 0.12(2) 0.067(14) 0.089(18) -0.033(13) -0.053(18) 0.029(15) C23A 0.067(14) 0.101(18) 0.066(14) 0.008(12) -0.023(12) -0.006(13) C24A 0.071(13) 0.060(11) 0.047(10) -0.003(9) -0.006(10) 0.003(10) C25A 0.045(10) 0.045(9) 0.073(12) -0.014(9) -0.014(9) -0.009(8) C26A 0.037(8) 0.059(10) 0.053(10) -0.010(8) 0.010(7) -0.018(8) C27A 0.059(12) 0.047(10) 0.070(12) 0.005(9) 0.013(10) -0.003(9) C28A 0.054(11) 0.086(14) 0.061(12) 0.014(10) -0.022(9) -0.024(10) Pd1B 0.0357(6) 0.0426(7) 0.0460(7) -0.0014(5) 0.0057(5) -0.0054(5) Pd2B 0.0292(6) 0.0765(10) 0.0641(9) 0.0220(8) 0.0062(6) -0.0120(6) O1B 0.048(8) 0.052(8) 0.115(12) 0.000(8) 0.041(8) 0.000(7) O2B 0.072(10) 0.049(7) 0.081(10) -0.013(7) 0.032(8) -0.001(7) O3B 0.036(7) 0.098(11) 0.107(12) 0.047(9) -0.001(7) -0.020(7) O4B 0.042(7) 0.058(7) 0.048(6) 0.014(5) 0.000(5) -0.013(6) O5B 0.063(9) 0.057(8) 0.098(11) 0.010(7) -0.005(8) -0.024(7) O6B 0.054(8) 0.069(8) 0.064(8) 0.005(7) -0.003(6) -0.014(7) N1B 0.017(6) 0.046(7) 0.056(8) -0.015(7) 0.007(5) -0.009(5) N2B 0.039(8) 0.077(12) 0.068(10) 0.026(9) 0.009(7) -0.020(8) C1B 0.075(16) 0.066(13) 0.088(16) 0.001(12) 0.048(13) -0.004(12) C2B 0.10(2) 0.058(13) 0.15(3) -0.031(15) 0.057(19) -0.012(14) C3B 0.034(9) 0.056(10) 0.065(11) 0.002(9) 0.019(8) -0.010(8) C4B 0.060(12) 0.084(14) 0.055(11) 0.013(10) -0.002(9) -0.022(11) C5B 0.021(7) 0.061(10) 0.076(12) -0.015(9) 0.010(7) -0.022(7) C6B 0.047(10) 0.051(11) 0.101(17) -0.037(11) 0.026(10) -0.011(8) C7B 0.027(7) 0.031(8) 0.079(12) 0.015(8) -0.005(8) -0.002(6) C8B 0.035(8) 0.060(11) 0.045(9) 0.009(8) -0.004(7) -0.008(8) C9B 0.040(10) 0.069(13) 0.098(17) 0.028(12) -0.007(10) -0.022(9) C10B 0.073(13) 0.069(13) 0.045(11) 0.014(9) 0.003(9) -0.024(11) C11B 0.063(13) 0.107(19) 0.061(13) -0.012(12) 0.008(10) -0.034(13) C12B 0.066(12) 0.086(14) 0.037(10) -0.002(9) 0.013(9) -0.020(11) C13B 0.028(8) 0.062(11) 0.054(10) 0.021(8) -0.013(7) -0.021(8) C14B 0.048(10) 0.066(11) 0.055(10) -0.006(9) 0.007(8) -0.020(9) C15B 0.082(16) 0.12(2) 0.082(16) -0.043(15) 0.038(14) -0.023(15) C16B 0.036(10) 0.096(17) 0.106(18) -0.010(14) 0.009(11) -0.022(10) C17B 0.052(10) 0.081(13) 0.036(9) -0.004(8) -0.001(8) -0.025(10) C18B 0.054(11) 0.072(12) 0.053(11) 0.014(9) -0.004(9) -0.016(10) C19B 0.037(9) 0.070(13) 0.066(12) 0.017(10) -0.014(8) -0.020(9) C20B 0.036(9) 0.083(14) 0.072(13) -0.035(12) -0.002(9) -0.001(9) C21B 0.043(11) 0.14(2) 0.092(17) -0.005(17) -0.014(11) -0.031(13) C22B 0.057(13) 0.16(3) 0.072(15) -0.077(18) -0.011(11) -0.004(15) C23B 0.049(12) 0.13(2) 0.081(16) -0.001(17) -0.001(11) -0.027(14) C24B 0.042(11) 0.11(2) 0.084(16) 0.017(14) -0.009(10) -0.025(12) C25B 0.022(9) 0.23(4) 0.066(13) 0.058(18) -0.016(9) -0.054(15) C26B 0.055(11) 0.073(13) 0.042(9) 0.005(9) 0.009(8) -0.016(10) C27B 0.040(10) 0.14(2) 0.071(14) 0.003(14) -0.001(10) -0.027(12) C28B 0.097(18) 0.12(2) 0.064(14) -0.012(14) 0.032(13) -0.053(17) Pd1C 0.0403(7) 0.0540(8) 0.0672(9) 0.0084(7) -0.0058(6) -0.0172(6) Pd2C 0.0578(9) 0.0501(8) 0.1074(13) 0.0012(8) 0.0037(9) -0.0180(7) O1C 0.043(7) 0.065(9) 0.094(11) 0.021(8) -0.008(7) -0.019(6) O2C 0.047(7) 0.048(7) 0.089(9) -0.011(6) -0.004(7) -0.007(6) O3C 0.077(10) 0.102(12) 0.081(10) -0.019(9) 0.010(8) -0.040(10) O4C 0.056(8) 0.094(11) 0.068(9) 0.013(8) -0.004(7) -0.025(8) O5C 0.043(7) 0.087(10) 0.069(9) -0.002(8) 0.013(7) -0.006(7) O6C 0.13(2) 0.118(18) 0.18(3) 0.056(19) -0.03(2) -0.046(16) N1C 0.040(8) 0.050(8) 0.099(13) 0.009(8) 0.003(8) -0.020(7) N2C 0.110(18) 0.052(11) 0.111(17) 0.045(11) -0.034(15) -0.028(12) C1C 0.063(12) 0.064(13) 0.046(10) 0.000(9) -0.004(9) -0.023(10) C2C 0.045(10) 0.096(16) 0.059(11) -0.008(11) 0.003(9) -0.007(10) C3C 0.041(10) 0.085(14) 0.066(12) -0.017(11) -0.003(9) -0.019(10) C4C 0.078(16) 0.12(2) 0.097(18) -0.015(16) -0.014(14) -0.036(16) C5C 0.043(9) 0.078(13) 0.054(10) -0.023(9) 0.005(8) -0.022(9) C6C 0.035(10) 0.069(13) 0.13(2) 0.019(13) -0.019(12) -0.019(10) C7C 0.046(10) 0.095(16) 0.063(12) 0.016(11) -0.015(9) -0.036(11) C8C 0.046(10) 0.087(14) 0.051(10) 0.013(10) -0.003(8) -0.020(10) C9C 0.058(13) 0.12(2) 0.093(18) -0.006(15) -0.008(13) -0.024(14) C10C 0.082(17) 0.16(3) 0.051(13) -0.019(14) -0.008(12) -0.022(17) C11C 0.065(15) 0.14(2) 0.059(14) -0.019(14) 0.010(11) -0.028(15) C12C 0.057(11) 0.052(10) 0.064(12) -0.015(9) 0.011(9) -0.010(9) C13C 0.047(10) 0.054(11) 0.083(14) 0.010(10) -0.014(10) -0.016(9) C14C 0.046(10) 0.072(13) 0.067(12) -0.007(10) -0.008(9) -0.017(9) C15C 0.11(2) 0.098(17) 0.052(12) -0.014(11) 0.023(13) -0.050(16) C16C 0.059(12) 0.063(12) 0.083(14) 0.015(10) -0.010(10) -0.035(10) C17C 0.11(2) 0.080(17) 0.14(3) 0.044(18) -0.04(2) -0.048(16) C18C 0.17(3) 0.12(2) 0.079(19) 0.042(18) -0.02(2) -0.07(2) C19C 0.11(2) 0.049(13) 0.14(3) 0.057(15) -0.05(2) -0.017(14) C20C 0.059(14) 0.089(18) 0.13(2) -0.029(17) 0.019(15) -0.039(13) C21C 0.11(3) 0.048(14) 0.22(5) -0.03(2) 0.02(3) 0.009(15) C22C 0.11(3) 0.08(2) 0.18(4) -0.06(2) 0.01(3) -0.026(19) C23C 0.17(4) 0.13(3) 0.16(3) -0.10(3) 0.08(3) -0.07(3) C24C 0.11(2) 0.13(3) 0.15(3) -0.09(2) 0.03(2) -0.06(2) C25C 0.09(2) 0.049(13) 0.18(3) -0.005(17) 0.01(2) -0.020(14) C26C 0.11(3) 0.32(7) 0.13(3) 0.01(4) 0.02(3) -0.10(4) C27C 0.28(7) 0.20(4) 0.16(4) 0.08(3) -0.06(4) -0.18(5) C28C 0.11(3) 0.14(4) 0.28(6) -0.06(4) 0.03(4) -0.02(3) Pd1D 0.0328(6) 0.0449(7) 0.0508(7) 0.0037(5) 0.0005(5) -0.0161(5) Pd2D 0.0288(6) 0.0461(7) 0.0486(7) 0.0068(5) -0.0063(5) -0.0155(5) O1D 0.036(6) 0.048(7) 0.073(8) -0.005(6) -0.008(6) -0.013(5) O2D 0.047(7) 0.052(7) 0.087(9) -0.008(6) 0.018(7) -0.018(6) O3D 0.028(6) 0.070(8) 0.060(7) 0.016(6) -0.017(5) -0.019(5) O4D 0.035(6) 0.078(9) 0.053(7) 0.016(6) 0.003(5) -0.029(6) O5D 0.086(10) 0.037(7) 0.098(11) 0.000(7) -0.020(9) -0.009(7) O6D 0.113(14) 0.067(10) 0.098(12) 0.033(9) -0.026(11) -0.027(10) N1D 0.036(7) 0.027(6) 0.056(8) -0.006(6) -0.006(6) -0.011(5) N2D 0.039(7) 0.051(9) 0.051(8) 0.015(6) -0.015(6) -0.017(7) C1D 0.044(9) 0.048(9) 0.039(8) 0.006(7) 0.002(7) -0.014(8) C2D 0.078(13) 0.046(10) 0.060(11) -0.009(8) 0.005(10) -0.016(9) C3D 0.054(10) 0.038(8) 0.050(9) 0.009(7) -0.012(8) -0.019(8) C4D 0.059(11) 0.057(10) 0.038(9) 0.002(8) -0.004(8) -0.012(9) C5D 0.041(9) 0.065(11) 0.065(11) -0.017(9) 0.004(8) -0.026(9) C6D 0.061(13) 0.050(12) 0.13(2) -0.029(12) -0.016(13) -0.008(10) C7D 0.039(9) 0.041(9) 0.086(14) 0.001(9) -0.003(9) -0.024(8) C8D 0.041(9) 0.070(12) 0.065(12) 0.015(10) -0.014(9) -0.027(9) C9D 0.073(15) 0.091(17) 0.087(18) 0.028(14) -0.011(13) -0.032(13) C10D 0.10(2) 0.15(3) 0.046(13) 0.028(15) 0.011(13) -0.032(19) C11D 0.072(14) 0.13(2) 0.048(12) -0.021(13) 0.000(10) -0.040(15) C12D 0.039(9) 0.079(13) 0.057(11) -0.001(10) -0.006(8) -0.027(9) C13D 0.036(8) 0.061(11) 0.039(9) 0.010(8) 0.005(7) -0.013(8) C14D 0.054(11) 0.076(13) 0.074(13) -0.018(11) -0.020(10) -0.019(10) C15D 0.092(19) 0.14(2) 0.096(19) -0.031(17) -0.020(15) -0.041(18) C16D 0.045(12) 0.13(2) 0.12(2) -0.015(17) -0.007(13) -0.029(14) C17D 0.036(9) 0.094(14) 0.044(10) 0.003(9) -0.016(7) -0.024(9) C18D 0.087(17) 0.099(18) 0.059(13) 0.011(12) -0.021(12) -0.020(14) C19D 0.065(12) 0.059(12) 0.053(10) 0.022(9) -0.015(9) -0.033(10) C20D 0.038(10) 0.057(12) 0.108(17) -0.012(11) -0.007(10) -0.017(9) C21D 0.059(13) 0.051(12) 0.14(2) 0.022(13) -0.021(14) -0.013(10) C22D 0.061(14) 0.067(14) 0.15(3) -0.019(16) -0.016(16) -0.027(12) C23D 0.037(9) 0.086(15) 0.091(15) -0.032(13) 0.007(10) -0.019(10) C24D 0.055(11) 0.061(11) 0.064(12) -0.025(9) 0.018(9) -0.023(9) C25D 0.032(8) 0.037(8) 0.073(12) 0.006(8) -0.008(8) -0.003(7) C26D 0.052(11) 0.082(14) 0.057(11) -0.001(10) -0.011(9) -0.017(10) C27D 0.049(11) 0.119(19) 0.059(12) -0.013(12) -0.003(9) -0.027(12) C28D 0.062(13) 0.13(2) 0.060(12) -0.025(13) -0.017(10) -0.024(14) _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 Pd1A C13A 1.94(2) . y Pd1A N1A 1.999(15) . y Pd1A O2A 2.059(14) . y Pd1A O4A 2.126(14) . y Pd1A Pd2A 2.863(2) . y Pd2A C25A 1.946(18) . y Pd2A N2A 2.000(14) . y Pd2A O3A 2.043(13) . y Pd2A O1A 2.115(13) . y O1A C1A 1.27(3) . ? O2A C1A 1.23(3) . ? O3A C3A 1.29(3) . ? O4A C3A 1.23(3) . ? O5A C7A 1.31(3) . ? O5A C6A 1.45(3) . ? O6A C19A 1.34(2) . ? O6A C18A 1.43(2) . ? N1A C7A 1.31(2) . ? N1A C5A 1.43(3) . ? N2A C19A 1.28(2) . ? N2A C17A 1.43(2) . ? C1A C2A 1.55(3) . ? C3A C4A 1.56(2) . ? C5A C6A 1.53(3) . ? C5A C14A 1.58(3) . ? C7A C8A 1.44(3) . ? C8A C13A 1.42(4) . ? C8A C9A 1.45(3) . ? C9A C10A 1.40(5) . ? C10A C11A 1.31(5) . ? C11A C12A 1.38(4) . ? C12A C13A 1.41(3) . ? C14A C16A 1.50(3) . ? C14A C15A 1.56(3) . ? C17A C26A 1.54(3) . ? C17A C18A 1.57(2) . ? C19A C20A 1.47(3) . ? C20A C21A 1.37(3) . ? C20A C25A 1.39(3) . ? C21A C22A 1.39(3) . ? C22A C23A 1.44(4) . ? C23A C24A 1.35(3) . ? C24A C25A 1.42(3) . ? C26A C27A 1.48(3) . ? C26A C28A 1.52(2) . ? Pd1B C13B 1.953(16) . y Pd1B N1B 1.993(13) . y Pd1B O2B 2.025(13) . y Pd1B O4B 2.116(11) . y Pd1B Pd2B 2.8358(19) . y Pd2B C25B 1.78(4) . y Pd2B N2B 2.020(15) . y Pd2B O3B 2.030(14) . y Pd2B O1B 2.128(16) . y O1B C1B 1.28(3) . ? O2B C1B 1.26(3) . ? O3B C3B 1.27(2) . ? O4B C3B 1.25(2) . ? O5B C7B 1.34(2) . ? O5B C6B 1.48(3) . ? O6B C19B 1.34(2) . ? O6B C18B 1.45(2) . ? N1B C7B 1.29(2) . ? N1B C5B 1.46(2) . ? N2B C19B 1.30(3) . ? N2B C17B 1.49(2) . ? C1B C2B 1.52(3) . ? C3B C4B 1.46(3) . ? C5B C14B 1.51(2) . ? C5B C6B 1.57(3) . ? C7B C8B 1.46(3) . ? C8B C9B 1.37(3) . ? C8B C13B 1.38(3) . ? C9B C10B 1.38(3) . ? C10B C11B 1.37(3) . ? C11B C12B 1.39(3) . ? C12B C13B 1.37(3) . ? C14B C16B 1.49(3) . ? C14B C15B 1.52(3) . ? C17B C26B 1.52(3) . ? C17B C18B 1.55(3) . ? C19B C20B 1.45(3) . ? C20B C21B 1.38(4) . ? C20B C25B 1.51(4) . ? C21B C22B 1.46(4) . ? C22B C23B 1.42(4) . ? C23B C24B 1.30(4) . ? C24B C25B 1.48(4) . ? C26B C27B 1.46(3) . ? C26B C28B 1.53(3) . ? Pd1C C13C 1.95(2) . y Pd1C N1C 2.012(15) . y Pd1C O2C 2.049(13) . y Pd1C O4C 2.109(15) . y Pd1C Pd2C 2.866(2) . y Pd2C N2C 1.96(2) . y Pd2C C25C 1.97(3) . y Pd2C O3C 2.024(17) . y Pd2C O1C 2.182(15) . y O1C C1C 1.20(2) . ? O2C C1C 1.29(2) . ? O3C C3C 1.34(3) . ? O4C C3C 1.24(2) . ? O5C C7C 1.38(2) . ? O5C C6C 1.50(3) . ? O6C C19C 1.25(4) . ? O6C C18C 1.41(4) . ? N1C C7C 1.30(3) . ? N1C C5C 1.46(2) . ? N2C C19C 1.31(4) . ? N2C C17C 1.37(4) . ? C1C C2C 1.50(3) . ? C3C C4C 1.45(3) . ? C5C C6C 1.52(3) . ? C5C C14C 1.55(3) . ? C7C C8C 1.44(3) . ? C8C C9C 1.37(3) . ? C8C C13C 1.40(3) . ? C9C C10C 1.35(4) . ? C10C C11C 1.37(4) . ? C11C C12C 1.36(3) . ? C12C C13C 1.41(3) . ? C14C C15C 1.51(3) . ? C14C C16C 1.53(3) . ? C17C C26C 1.56(5) . ? C17C C18C 1.74(5) . ? C19C C20C 1.43(4) . ? C20C C25C 1.39(4) . ? C20C C21C 1.51(4) . ? C21C C22C 1.22(5) . ? C22C C23C 1.53(6) . ? C23C C24C 1.34(5) . ? C24C C25C 1.36(4) . ? C26C C28C 1.32(6) . ? C26C C27C 1.53(7) . ? Pd1D C13D 1.950(16) . y Pd1D N1D 2.022(12) . y Pd1D O2D 2.042(13) . y Pd1D O4D 2.116(12) . y Pd1D Pd2D 2.8649(16) . y Pd2D C25D 1.987(18) . y Pd2D N2D 2.022(13) . y Pd2D O3D 2.026(11) . y Pd2D O1D 2.145(12) . y O1D C1D 1.28(2) . ? O2D C1D 1.20(2) . ? O3D C3D 1.27(2) . ? O4D C3D 1.28(2) . ? O5D C7D 1.37(2) . ? O5D C6D 1.43(3) . ? O6D C19D 1.36(2) . ? O6D C18D 1.44(3) . ? N1D C7D 1.24(2) . ? N1D C5D 1.46(2) . ? N2D C19D 1.28(2) . ? N2D C17D 1.44(2) . ? C1D C2D 1.49(2) . ? C3D C4D 1.48(2) . ? C5D C14D 1.51(3) . ? C5D C6D 1.54(3) . ? C7D C8D 1.42(3) . ? C8D C9D 1.42(3) . ? C8D C13D 1.47(3) . ? C9D C10D 1.34(4) . ? C10D C11D 1.38(4) . ? C11D C12D 1.38(3) . ? C12D C13D 1.38(3) . ? C14D C16D 1.49(3) . ? C14D C15D 1.50(3) . ? C17D C26D 1.49(3) . ? C17D C18D 1.54(3) . ? C19D C20D 1.44(3) . ? C20D C21D 1.41(3) . ? C20D C25D 1.43(3) . ? C21D C22D 1.46(4) . ? C22D C23D 1.30(3) . ? C23D C24D 1.43(3) . ? C24D C25D 1.32(3) . ? C26D C27D 1.53(3) . ? C26D C28D 1.55(3) . ? 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 C13A Pd1A N1A 81.3(9) . . y C13A Pd1A O2A 93.6(9) . . y N1A Pd1A O2A 174.9(6) . . y C13A Pd1A O4A 174.1(8) . . y N1A Pd1A O4A 93.0(6) . . y O2A Pd1A O4A 92.1(6) . . y C13A Pd1A Pd2A 106.1(6) . . y N1A Pd1A Pd2A 95.2(4) . . y O2A Pd1A Pd2A 85.4(4) . . y O4A Pd1A Pd2A 75.5(4) . . y C25A Pd2A N2A 81.2(7) . . y C25A Pd2A O3A 93.0(7) . . y N2A Pd2A O3A 174.1(6) . . y C25A Pd2A O1A 175.2(7) . . y N2A Pd2A O1A 94.2(5) . . y O3A Pd2A O1A 91.6(5) . . y C25A Pd2A Pd1A 103.5(5) . . y N2A Pd2A Pd1A 92.2(4) . . y O3A Pd2A Pd1A 88.1(4) . . y O1A Pd2A Pd1A 77.7(4) . . y C1A O1A Pd2A 125.4(12) . . ? C1A O2A Pd1A 119.5(14) . . ? C3A O3A Pd2A 116.6(13) . . ? C3A O4A Pd1A 129.1(13) . . ? C7A O5A C6A 106.7(15) . . ? C19A O6A C18A 106.4(13) . . ? C7A N1A C5A 107.2(16) . . ? C7A N1A Pd1A 114.1(14) . . ? C5A N1A Pd1A 137.5(12) . . ? C19A N2A C17A 110.0(14) . . ? C19A N2A Pd2A 113.8(12) . . ? C17A N2A Pd2A 136.1(10) . . ? O2A C1A O1A 130.3(19) . . ? O2A C1A C2A 116(2) . . ? O1A C1A C2A 114(2) . . ? O4A C3A O3A 129.5(17) . . ? O4A C3A C4A 118(2) . . ? O3A C3A C4A 112(2) . . ? N1A C5A C6A 104.2(18) . . ? N1A C5A C14A 109.4(19) . . ? C6A C5A C14A 115.7(18) . . ? O5A C6A C5A 103.2(18) . . ? O5A C7A N1A 117(2) . . ? O5A C7A C8A 127(2) . . ? N1A C7A C8A 116(2) . . ? C13A C8A C7A 112.2(18) . . ? C13A C8A C9A 123(3) . . ? C7A C8A C9A 125(3) . . ? C10A C9A C8A 116(3) . . ? C11A C10A C9A 121(2) . . ? C10A C11A C12A 126(3) . . ? C11A C12A C13A 118(3) . . ? C12A C13A C8A 117(2) . . ? C12A C13A Pd1A 129(2) . . ? C8A C13A Pd1A 114.4(17) . . ? C16A C14A C15A 114.2(18) . . ? C16A C14A C5A 111.6(17) . . ? C15A C14A C5A 109(2) . . ? N2A C17A C26A 114.1(15) . . ? N2A C17A C18A 101.7(14) . . ? C26A C17A C18A 116.2(14) . . ? O6A C18A C17A 104.1(14) . . ? N2A C19A O6A 116.3(16) . . ? N2A C19A C20A 118.3(17) . . ? O6A C19A C20A 125.4(17) . . ? C21A C20A C25A 124.2(19) . . ? C21A C20A C19A 125(2) . . ? C25A C20A C19A 110.6(16) . . ? C20A C21A C22A 121(3) . . ? C21A C22A C23A 114(3) . . ? C24A C23A C22A 124(2) . . ? C23A C24A C25A 120(2) . . ? C20A C25A C24A 115.6(17) . . ? C20A C25A Pd2A 115.4(14) . . ? C24A C25A Pd2A 129.0(16) . . ? C27A C26A C28A 113.7(16) . . ? C27A C26A C17A 110.6(15) . . ? C28A C26A C17A 110.3(15) . . ? C13B Pd1B N1B 80.2(7) . . y C13B Pd1B O2B 94.9(7) . . y N1B Pd1B O2B 175.0(6) . . y C13B Pd1B O4B 174.6(7) . . y N1B Pd1B O4B 94.4(5) . . y O2B Pd1B O4B 90.6(5) . . y C13B Pd1B Pd2B 101.2(4) . . y N1B Pd1B Pd2B 92.9(3) . . y O2B Pd1B Pd2B 87.4(5) . . y O4B Pd1B Pd2B 79.0(3) . . y C25B Pd2B N2B 82.4(9) . . y C25B Pd2B O3B 89.9(9) . . y N2B Pd2B O3B 172.1(8) . . y C25B Pd2B O1B 176.0(8) . . y N2B Pd2B O1B 99.0(7) . . y O3B Pd2B O1B 88.9(7) . . y C25B Pd2B Pd1B 106.8(6) . . y N2B Pd2B Pd1B 98.0(5) . . y O3B Pd2B Pd1B 82.9(4) . . y O1B Pd2B Pd1B 76.7(4) . . y C1B O1B Pd2B 127.0(12) . . ? C1B O2B Pd1B 119.5(17) . . ? C3B O3B Pd2B 125.6(13) . . ? C3B O4B Pd1B 127.4(10) . . ? C7B O5B C6B 106.0(14) . . ? C19B O6B C18B 104.9(16) . . ? C7B N1B C5B 109.3(14) . . ? C7B N1B Pd1B 114.8(11) . . ? C5B N1B Pd1B 135.6(12) . . ? C19B N2B C17B 110.1(15) . . ? C19B N2B Pd2B 114.0(13) . . ? C17B N2B Pd2B 135.9(15) . . ? O2B C1B O1B 127(2) . . ? O2B C1B C2B 119(3) . . ? O1B C1B C2B 113(2) . . ? O4B C3B O3B 122.7(17) . . ? O4B C3B C4B 119.6(15) . . ? O3B C3B C4B 117.7(18) . . ? N1B C5B C14B 111.5(14) . . ? N1B C5B C6B 102.6(15) . . ? C14B C5B C6B 117.6(15) . . ? O5B C6B C5B 103.7(14) . . ? N1B C7B O5B 117.4(17) . . ? N1B C7B C8B 117.5(15) . . ? O5B C7B C8B 125.1(15) . . ? C9B C8B C13B 124.2(19) . . ? C9B C8B C7B 125.1(18) . . ? C13B C8B C7B 110.6(14) . . ? C10B C9B C8B 118(2) . . ? C9B C10B C11B 119.3(18) . . ? C10B C11B C12B 121(2) . . ? C13B C12B C11B 121(2) . . ? C12B C13B C8B 116.2(16) . . ? C12B C13B Pd1B 127.5(15) . . ? C8B C13B Pd1B 116.3(14) . . ? C16B C14B C15B 114.0(19) . . ? C16B C14B C5B 113.1(16) . . ? C15B C14B C5B 109.2(18) . . ? N2B C17B C26B 112.0(15) . . ? N2B C17B C18B 98.9(15) . . ? C26B C17B C18B 114.4(16) . . ? O6B C18B C17B 108.2(14) . . ? N2B C19B O6B 116.7(18) . . ? N2B C19B C20B 116.8(17) . . ? O6B C19B C20B 126(2) . . ? C21B C20B C19B 123(2) . . ? C21B C20B C25B 130(2) . . ? C19B C20B C25B 107.5(19) . . ? C20B C21B C22B 117(3) . . ? C23B C22B C21B 115(2) . . ? C24B C23B C22B 126(2) . . ? C23B C24B C25B 126(3) . . ? C24B C25B C20B 106(3) . . ? C24B C25B Pd2B 135(2) . . ? C20B C25B Pd2B 118.8(15) . . ? C27B C26B C17B 112.9(18) . . ? C27B C26B C28B 113.2(18) . . ? C17B C26B C28B 110.3(18) . . ? C13C Pd1C N1C 81.7(8) . . y C13C Pd1C O2C 91.7(7) . . y N1C Pd1C O2C 172.7(7) . . y C13C Pd1C O4C 176.6(7) . . y N1C Pd1C O4C 95.5(7) . . y O2C Pd1C O4C 91.0(6) . . y C13C Pd1C Pd2C 107.7(6) . . y N1C Pd1C Pd2C 101.0(4) . . y O2C Pd1C Pd2C 83.8(4) . . y O4C Pd1C Pd2C 74.7(4) . . y N2C Pd2C C25C 82.9(14) . . y N2C Pd2C O3C 173.8(9) . . y C25C Pd2C O3C 90.9(13) . . y N2C Pd2C O1C 96.3(8) . . y C25C Pd2C O1C 177.5(11) . . y O3C Pd2C O1C 89.9(6) . . y N2C Pd2C Pd1C 94.2(6) . . y C25C Pd2C Pd1C 98.8(8) . . y O3C Pd2C Pd1C 87.1(5) . . y O1C Pd2C Pd1C 78.9(4) . . y C1C O1C Pd2C 123.5(13) . . ? C1C O2C Pd1C 121.5(12) . . ? C3C O3C Pd2C 119.4(14) . . ? C3C O4C Pd1C 133.4(14) . . ? C7C O5C C6C 105.1(15) . . ? C19C O6C C18C 113(3) . . ? C7C N1C C5C 110.7(16) . . ? C7C N1C Pd1C 111.0(14) . . ? C5C N1C Pd1C 138.3(14) . . ? C19C N2C C17C 110(2) . . ? C19C N2C Pd2C 112(2) . . ? C17C N2C Pd2C 138(2) . . ? O1C C1C O2C 129.7(19) . . ? O1C C1C C2C 116.7(19) . . ? O2C C1C C2C 113.4(18) . . ? O4C C3C O3C 122(2) . . ? O4C C3C C4C 124(2) . . ? O3C C3C C4C 114(2) . . ? N1C C5C C6C 103.5(16) . . ? N1C C5C C14C 112.3(16) . . ? C6C C5C C14C 114.9(16) . . ? O5C C6C C5C 105.6(16) . . ? N1C C7C O5C 115.0(19) . . ? N1C C7C C8C 121.6(18) . . ? O5C C7C C8C 123.2(17) . . ? C9C C8C C13C 125(2) . . ? C9C C8C C7C 125.2(19) . . ? C13C C8C C7C 109.5(18) . . ? C10C C9C C8C 116(2) . . ? C9C C10C C11C 122(2) . . ? C12C C11C C10C 123(2) . . ? C11C C12C C13C 118(2) . . ? C8C C13C C12C 116.1(19) . . ? C8C C13C Pd1C 115.7(16) . . ? C12C C13C Pd1C 127.9(15) . . ? C15C C14C C16C 111.5(18) . . ? C15C C14C C5C 108.7(17) . . ? C16C C14C C5C 111.8(16) . . ? N2C C17C C26C 114(3) . . ? N2C C17C C18C 101(3) . . ? C26C C17C C18C 110(3) . . ? O6C C18C C17C 95(2) . . ? O6C C19C N2C 116(3) . . ? O6C C19C C20C 126(3) . . ? N2C C19C C20C 118(3) . . ? C25C C20C C19C 114(3) . . ? C25C C20C C21C 120(3) . . ? C19C C20C C21C 126(3) . . ? C22C C21C C20C 120(4) . . ? C21C C22C C23C 122(4) . . ? C24C C23C C22C 113(3) . . ? C23C C24C C25C 128(4) . . ? C24C C25C C20C 115(3) . . ? C24C C25C Pd2C 133(3) . . ? C20C C25C Pd2C 111(3) . . ? C28C C26C C27C 92(4) . . ? C28C C26C C17C 111(5) . . ? C27C C26C C17C 106(4) . . ? C13D Pd1D N1D 81.7(7) . . y C13D Pd1D O2D 92.8(7) . . y N1D Pd1D O2D 173.6(6) . . y C13D Pd1D O4D 177.5(6) . . y N1D Pd1D O4D 96.9(5) . . y O2D Pd1D O4D 88.7(5) . . y C13D Pd1D Pd2D 104.3(5) . . y N1D Pd1D Pd2D 91.4(4) . . y O2D Pd1D Pd2D 86.8(3) . . y O4D Pd1D Pd2D 77.8(3) . . y C25D Pd2D N2D 83.0(7) . . y C25D Pd2D O3D 90.5(6) . . y N2D Pd2D O3D 173.1(6) . . y C25D Pd2D O1D 175.6(6) . . y N2D Pd2D O1D 95.7(5) . . y O3D Pd2D O1D 91.0(5) . . y C25D Pd2D Pd1D 109.1(5) . . y N2D Pd2D Pd1D 95.2(4) . . y O3D Pd2D Pd1D 85.0(3) . . y O1D Pd2D Pd1D 75.1(3) . . y C1D O1D Pd2D 130.4(11) . . ? C1D O2D Pd1D 122.6(12) . . ? C3D O3D Pd2D 125.1(11) . . ? C3D O4D Pd1D 129.2(11) . . ? C7D O5D C6D 104.5(15) . . ? C19D O6D C18D 106.7(17) . . ? C7D N1D C5D 112.2(15) . . ? C7D N1D Pd1D 114.4(12) . . ? C5D N1D Pd1D 132.7(11) . . ? C19D N2D C17D 111.4(14) . . ? C19D N2D Pd2D 111.1(12) . . ? C17D N2D Pd2D 137.3(12) . . ? O2D C1D O1D 124.9(16) . . ? O2D C1D C2D 120.6(16) . . ? O1D C1D C2D 114.5(16) . . ? O3D C3D O4D 122.9(15) . . ? O3D C3D C4D 118.3(15) . . ? O4D C3D C4D 118.8(15) . . ? N1D C5D C14D 111.1(15) . . ? N1D C5D C6D 99.4(16) . . ? C14D C5D C6D 116.1(17) . . ? O5D C6D C5D 107.7(16) . . ? N1D C7D O5D 115.8(18) . . ? N1D C7D C8D 119.2(16) . . ? O5D C7D C8D 124.9(17) . . ? C9D C8D C7D 128(2) . . ? C9D C8D C13D 120(2) . . ? C7D C8D C13D 112.2(15) . . ? C10D C9D C8D 120(3) . . ? C9D C10D C11D 120(2) . . ? C10D C11D C12D 122(2) . . ? C13D C12D C11D 121(2) . . ? C12D C13D C8D 116.8(16) . . ? C12D C13D Pd1D 131.2(15) . . ? C8D C13D Pd1D 112.0(13) . . ? C16D C14D C15D 112(2) . . ? C16D C14D C5D 113.6(19) . . ? C15D C14D C5D 110.1(19) . . ? N2D C17D C26D 113.4(15) . . ? N2D C17D C18D 101.4(17) . . ? C26D C17D C18D 117.5(16) . . ? O6D C18D C17D 105.1(16) . . ? N2D C19D O6D 114.1(18) . . ? N2D C19D C20D 120.8(16) . . ? O6D C19D C20D 125.1(19) . . ? C21D C20D C25D 122(2) . . ? C21D C20D C19D 125(2) . . ? C25D C20D C19D 112.8(17) . . ? C20D C21D C22D 115(2) . . ? C23D C22D C21D 122(2) . . ? C22D C23D C24D 120(2) . . ? C25D C24D C23D 123(2) . . ? C24D C25D C20D 117.8(18) . . ? C24D C25D Pd2D 130.8(14) . . ? C20D C25D Pd2D 111.2(15) . . ? C17D C26D C27D 112.3(18) . . ? C17D C26D C28D 111.4(18) . . ? C27D C26D C28D 111.5(17) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.670 _refine_diff_density_min -2.031 _refine_diff_density_rms 0.150 #===END