# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name R.Troff R.Hovorka T.Weilandt A.Lutzen M.Cetina M.Nieger D.Lentz K.Rissanen C.Schalley _publ_contact_author_name 'Christoph Schalley' _publ_contact_author_email christoph@schalley-lab.de data_10 _database_code_depnum_ccdc_archive 'CCDC 864202' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound10.cif' _audit_creation_date 2008-11-14T08:15:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C13 H14 N4 O' _chemical_formula_sum 'C13 H14 N4 O' _chemical_formula_weight 242.28 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.0896(2) _cell_length_b 4.59310(10) _cell_length_c 21.5276(5) _cell_angle_alpha 90 _cell_angle_beta 96.9200(10) _cell_angle_gamma 90 _cell_volume 1186.69(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 11446 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.312597E-1 _diffrn_orient_matrix_ub_12 0.197034 _diffrn_orient_matrix_ub_13 -0.114323E-1 _diffrn_orient_matrix_ub_21 0.772219E-1 _diffrn_orient_matrix_ub_22 0.806491E-1 _diffrn_orient_matrix_ub_23 0.23397E-2 _diffrn_orient_matrix_ub_31 0.15076E-2 _diffrn_orient_matrix_ub_32 -0.455454E-1 _diffrn_orient_matrix_ub_33 -0.453144E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_unetI/netI 0.027 _diffrn_reflns_number 3886 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.4 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 2093 _reflns_number_gt 1769 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0399P)^2^+0.4318P] 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_number_reflns 2093 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.093 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.1 _refine_ls_restrained_S_all 1.1 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.152 _refine_diff_density_min -0.198 _refine_diff_density_rms 0.04 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O8 O 0.72862(8) 0.2927(2) 0.48997(5) 0.0212(3) Uani 1 1 d . . . N1 N 0.59391(10) -0.0200(3) 0.69036(5) 0.0226(3) Uani 1 1 d . . . N1' N 0.97536(10) 0.0283(3) 0.33288(6) 0.0237(3) Uani 1 1 d . . . N7' N 0.78939(10) -0.1344(3) 0.45160(5) 0.0185(3) Uani 1 1 d . . . H7' H 0.799 -0.3222 0.4583 0.022 Uiso 1 1 calc R . . N7 N 0.69658(9) -0.1367(3) 0.53828(5) 0.0182(3) Uani 1 1 d . . . H7 H 0.7104 -0.3248 0.5395 0.022 Uiso 1 1 calc R . . C2 C 0.65435(11) -0.1167(3) 0.64586(6) 0.0182(3) Uani 1 1 d . . . C2' C 0.93581(11) -0.0808(3) 0.38387(6) 0.0186(3) Uani 1 1 d . . . C3 C 0.63345(11) -0.0190(3) 0.58380(6) 0.0167(3) Uani 1 1 d . . . C3' C 0.82926(11) -0.0088(3) 0.39810(6) 0.0163(3) Uani 1 1 d . . . C4' C 0.76328(12) 0.1776(3) 0.35913(7) 0.0198(3) Uani 1 1 d . . . H4' H 0.69 0.2246 0.3676 0.024 Uiso 1 1 calc R . . C4 C 0.54942(11) 0.1825(3) 0.56810(7) 0.0191(3) Uani 1 1 d . . . H4 H 0.5336 0.2501 0.5263 0.023 Uiso 1 1 calc R . . C5 C 0.48892(12) 0.2836(3) 0.61424(7) 0.0231(3) Uani 1 1 d . . . H5 H 0.4315 0.4235 0.6048 0.028 Uiso 1 1 calc R . . C5' C 0.80537(13) 0.2948(3) 0.30763(7) 0.0253(4) Uani 1 1 d . . . H5' H 0.7626 0.4273 0.2806 0.03 Uiso 1 1 calc R . . C6 C 0.51379(12) 0.1767(4) 0.67435(7) 0.0250(4) Uani 1 1 d . . . H6 H 0.4719 0.2463 0.7059 0.03 Uiso 1 1 calc R . . C6' C 0.91135(13) 0.2137(4) 0.29650(7) 0.0267(4) Uani 1 1 d . . . H6' H 0.9403 0.294 0.2611 0.032 Uiso 1 1 calc R . . C8 C 0.73696(11) 0.0243(3) 0.49291(6) 0.0158(3) Uani 1 1 d . . . C9 C 0.74558(12) -0.3282(3) 0.66602(7) 0.0229(3) Uani 1 1 d . . . H9A H 0.7438 -0.3786 0.7101 0.034 Uiso 1 1 calc R . . H9B H 0.8177 -0.24 0.6608 0.034 Uiso 1 1 calc R . . H9C H 0.7351 -0.5047 0.6404 0.034 Uiso 1 1 calc R . . C9' C 1.01030(12) -0.2853(4) 0.42366(7) 0.0264(4) Uani 1 1 d . . . H9'1 H 0.9786 -0.4818 0.4204 0.04 Uiso 1 1 calc R . . H9'2 H 1.0169 -0.2209 0.4673 0.04 Uiso 1 1 calc R . . H9'3 H 1.0842 -0.287 0.4093 0.04 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 O8 0.0287(5) 0.0128(5) 0.0235(5) -0.0005(4) 0.0091(4) -0.0003(4) N1 0.0244(6) 0.0245(7) 0.0200(6) -0.0035(6) 0.0071(5) -0.0047(6) N1' 0.0270(7) 0.0239(7) 0.0216(6) -0.0037(6) 0.0081(5) -0.0059(6) N7' 0.0250(6) 0.0116(6) 0.0209(6) 0.0016(5) 0.0105(5) 0.0018(5) N7 0.0245(6) 0.0119(6) 0.0194(6) 0.0002(5) 0.0082(5) 0.0023(5) C2 0.0188(7) 0.0175(8) 0.0185(7) -0.0014(6) 0.0034(6) -0.0051(6) C2' 0.0213(7) 0.0171(7) 0.0178(7) -0.0048(6) 0.0042(6) -0.0028(6) C3 0.0182(7) 0.0149(7) 0.0181(7) -0.0040(6) 0.0060(6) -0.0036(6) C3' 0.0211(7) 0.0131(7) 0.0155(7) -0.0041(6) 0.0046(6) -0.0035(6) C4' 0.0212(7) 0.0178(8) 0.0207(7) -0.0029(6) 0.0036(6) 0.0004(6) C4 0.0190(7) 0.0178(7) 0.0205(7) -0.0015(6) 0.0021(6) -0.0017(6) C5 0.0179(7) 0.0210(8) 0.0310(8) -0.0054(7) 0.0048(6) 0.0020(6) C5' 0.0365(9) 0.0194(8) 0.0195(7) 0.0018(7) 0.0005(6) -0.0003(7) C6 0.0229(7) 0.0260(9) 0.0278(8) -0.0093(7) 0.0105(6) -0.0043(7) C6' 0.0368(9) 0.0259(9) 0.0186(7) 0.0000(7) 0.0087(7) -0.0072(7) C8 0.0168(7) 0.0144(8) 0.0164(7) -0.0010(6) 0.0021(6) -0.0001(6) C9 0.0267(8) 0.0221(8) 0.0195(7) 0.0013(6) 0.0018(6) -0.0008(7) C9' 0.0245(8) 0.0273(9) 0.0273(8) -0.0030(7) 0.0031(6) 0.0040(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O8 C8 1.2380(18) . ? N1 C6 1.339(2) . ? N1 C2 1.3480(18) . ? N1' C6' 1.339(2) . ? N1' C2' 1.3458(18) . ? N7' C8 1.3638(18) . ? N7' C3' 1.4231(17) . ? N7' H7' 0.88 . ? N7 C8 1.3617(18) . ? N7 C3 1.4195(17) . ? N7 H7 0.88 . ? C2 C3 1.403(2) . ? C2 C9 1.494(2) . ? C2' C3' 1.399(2) . ? C2' C9' 1.497(2) . ? C3 C4 1.386(2) . ? C3' C4' 1.383(2) . ? C4' C5' 1.383(2) . ? C4' H4' 0.95 . ? C4 C5 1.383(2) . ? C4 H4 0.95 . ? C5 C6 1.383(2) . ? C5 H5 0.95 . ? C5' C6' 1.383(2) . ? C5' H5' 0.95 . ? C6 H6 0.95 . ? C6' H6' 0.95 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C9' H9'1 0.98 . ? C9' H9'2 0.98 . ? C9' H9'3 0.98 . ? 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 C6 N1 C2 118.47(13) . . ? C6' N1' C2' 118.49(13) . . ? C8 N7' C3' 122.72(12) . . ? C8 N7' H7' 118.6 . . ? C3' N7' H7' 118.6 . . ? C8 N7 C3 123.87(12) . . ? C8 N7 H7 118.1 . . ? C3 N7 H7 118.1 . . ? N1 C2 C3 121.36(13) . . ? N1 C2 C9 116.87(13) . . ? C3 C2 C9 121.76(13) . . ? N1' C2' C3' 121.17(13) . . ? N1' C2' C9' 116.87(13) . . ? C3' C2' C9' 121.96(13) . . ? C4 C3 C2 119.24(13) . . ? C4 C3 N7 121.70(12) . . ? C2 C3 N7 119.03(13) . . ? C4' C3' C2' 119.51(13) . . ? C4' C3' N7' 121.00(12) . . ? C2' C3' N7' 119.47(12) . . ? C5' C4' C3' 119.08(13) . . ? C5' C4' H4' 120.5 . . ? C3' C4' H4' 120.5 . . ? C5 C4 C3 119.00(14) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C4 C5 C6 118.60(14) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C6' C5' C4' 118.18(14) . . ? C6' C5' H5' 120.9 . . ? C4' C5' H5' 120.9 . . ? N1 C6 C5 123.33(14) . . ? N1 C6 H6 118.3 . . ? C5 C6 H6 118.3 . . ? N1' C6' C5' 123.53(14) . . ? N1' C6' H6' 118.2 . . ? C5' C6' H6' 118.2 . . ? O8 C8 N7 122.92(13) . . ? O8 C8 N7' 122.71(13) . . ? N7 C8 N7' 114.36(13) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C2' C9' H9'1 109.5 . . ? C2' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C2' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 C3 -1.1(2) . . . . ? C6 N1 C2 C9 177.92(13) . . . . ? C6' N1' C2' C3' 1.5(2) . . . . ? C6' N1' C2' C9' -179.47(14) . . . . ? N1 C2 C3 C4 0.4(2) . . . . ? C9 C2 C3 C4 -178.49(13) . . . . ? N1 C2 C3 N7 -177.47(13) . . . . ? C9 C2 C3 N7 3.6(2) . . . . ? C8 N7 C3 C4 43.2(2) . . . . ? C8 N7 C3 C2 -138.92(14) . . . . ? N1' C2' C3' C4' 0.0(2) . . . . ? C9' C2' C3' C4' -178.94(14) . . . . ? N1' C2' C3' N7' 178.45(13) . . . . ? C9' C2' C3' N7' -0.5(2) . . . . ? C8 N7' C3' C4' -46.85(19) . . . . ? C8 N7' C3' C2' 134.75(14) . . . . ? C2' C3' C4' C5' -1.6(2) . . . . ? N7' C3' C4' C5' 180.00(13) . . . . ? C2 C3 C4 C5 0.5(2) . . . . ? N7 C3 C4 C5 178.35(13) . . . . ? C3 C4 C5 C6 -0.8(2) . . . . ? C3' C4' C5' C6' 1.6(2) . . . . ? C2 N1 C6 C5 0.8(2) . . . . ? C4 C5 C6 N1 0.2(2) . . . . ? C2' N1' C6' C5' -1.5(2) . . . . ? C4' C5' C6' N1' -0.1(2) . . . . ? C3 N7 C8 O8 5.1(2) . . . . ? C3 N7 C8 N7' -176.08(12) . . . . ? C3' N7' C8 O8 -6.4(2) . . . . ? C3' N7' C8 N7 174.86(11) . . . . ? # Attachment '- Schalley_DT-ART-01-2012-030190_Compound11.cif' data_11 _database_code_depnum_ccdc_archive 'CCDC 864203' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound11.cif' _audit_creation_date 2008-11-14T08:13:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C13 H14 N4 O, C3 H4 N2, H2 O' _chemical_formula_sum 'C16 H20 N6 O2' _chemical_formula_weight 328.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.4693(4) _cell_length_b 13.3280(6) _cell_length_c 15.0145(8) _cell_angle_alpha 90 _cell_angle_beta 103.537(4) _cell_angle_gamma 90 _cell_volume 1647.74(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4269 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 26.733 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.092 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.143758E-1 _diffrn_orient_matrix_ub_12 -0.36168E-1 _diffrn_orient_matrix_ub_13 -0.597057E-1 _diffrn_orient_matrix_ub_21 0.113146 _diffrn_orient_matrix_ub_22 -0.267753E-1 _diffrn_orient_matrix_ub_23 0.196701E-1 _diffrn_orient_matrix_ub_31 -0.41825E-1 _diffrn_orient_matrix_ub_32 -0.60002E-1 _diffrn_orient_matrix_ub_33 0.272118E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.1406 _diffrn_reflns_av_unetI/netI 0.0877 _diffrn_reflns_number 21314 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.47 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 2890 _reflns_number_gt 1808 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0430P)^2^+0.6487P] 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_number_reflns 2890 _refine_ls_number_parameters 227 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1085 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.262 _refine_diff_density_min -0.205 _refine_diff_density_rms 0.052 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O8 O 0.1304(2) 0.07821(14) 0.39105(13) 0.0258(5) Uani 1 1 d . . . O15 O 0.4316(3) -0.57886(15) 0.59596(15) 0.0324(5) Uani 1 1 d D . . N1 N -0.2569(3) -0.00547(18) 0.18655(16) 0.0264(6) Uani 1 1 d . . . N1' N 0.4432(3) 0.21265(17) 0.60813(18) 0.0275(6) Uani 1 1 d . . . N7 N 0.0474(3) -0.08527(16) 0.39382(16) 0.0221(6) Uani 1 1 d . . . H7 H 0.0622 -0.1405 0.4269 0.027 Uiso 1 1 calc R . . N7' N 0.2450(3) -0.02414(16) 0.51218(16) 0.0208(6) Uani 1 1 d . . . H7' H 0.2442 -0.0857 0.5332 0.025 Uiso 1 1 calc R . . N10 N 0.1909(3) -0.24571(17) 0.53022(17) 0.0283(6) Uani 1 1 d . . . N12 N 0.2366(3) -0.40725(17) 0.55636(16) 0.0267(6) Uani 1 1 d . . . H12 H 0.2809 -0.467 0.5565 0.032 Uiso 1 1 calc R . . C2' C 0.3411(3) 0.1474(2) 0.5547(2) 0.0236(7) Uani 1 1 d . . . H2' H 0.2571 0.1732 0.5068 0.028 Uiso 1 1 calc R . . C2 C -0.1456(3) -0.0033(2) 0.26675(19) 0.0231(7) Uani 1 1 d . . . H2 H -0.118 0.0597 0.2957 0.028 Uiso 1 1 calc R . . C3' C 0.3536(3) 0.0439(2) 0.56658(19) 0.0195(6) Uani 1 1 d . . . C3 C -0.0686(3) -0.08898(19) 0.30962(19) 0.0201(6) Uani 1 1 d . . . C4' C 0.4762(3) 0.0055(2) 0.63825(19) 0.0221(7) Uani 1 1 d . . . C4 C -0.1124(3) -0.1825(2) 0.2689(2) 0.0224(7) Uani 1 1 d . . . C5' C 0.5802(4) 0.0735(2) 0.6915(2) 0.0280(7) Uani 1 1 d . . . H5' H 0.6657 0.0502 0.7398 0.034 Uiso 1 1 calc R . . C5 C -0.2256(3) -0.1832(2) 0.1857(2) 0.0255(7) Uani 1 1 d . . . H5 H -0.2576 -0.2451 0.1555 0.031 Uiso 1 1 calc R . . C6 C -0.2924(3) -0.0945(2) 0.1463(2) 0.0273(7) Uani 1 1 d . . . H6 H -0.3666 -0.0971 0.0881 0.033 Uiso 1 1 calc R . . C6' C 0.5607(4) 0.1750(2) 0.6749(2) 0.0292(7) Uani 1 1 d . . . H6' H 0.6341 0.2201 0.7126 0.035 Uiso 1 1 calc R . . C9 C -0.0419(4) -0.2794(2) 0.3130(2) 0.0319(8) Uani 1 1 d . . . H9A H -0.0839 -0.3357 0.2725 0.048 Uiso 1 1 calc R . . H9B H -0.0728 -0.288 0.3715 0.048 Uiso 1 1 calc R . . H9C H 0.0767 -0.2773 0.3238 0.048 Uiso 1 1 calc R . . C9' C 0.4933(4) -0.1050(2) 0.6569(2) 0.0290(7) Uani 1 1 d . . . H9'1 H 0.5847 -0.1169 0.7094 0.044 Uiso 1 1 calc R . . H9'2 H 0.5132 -0.1394 0.6029 0.044 Uiso 1 1 calc R . . H9'3 H 0.3933 -0.1308 0.6706 0.044 Uiso 1 1 calc R . . C11 C 0.2816(4) -0.3236(2) 0.5194(2) 0.0273(7) Uani 1 1 d . . . H11 H 0.3682 -0.3205 0.4891 0.033 Uiso 1 1 calc R . . C13 C 0.1094(4) -0.3828(2) 0.5937(2) 0.0299(8) Uani 1 1 d . . . H13 H 0.0516 -0.4264 0.6249 0.036 Uiso 1 1 calc R . . C14 C 0.0826(4) -0.2840(2) 0.5773(2) 0.0265(7) Uani 1 1 d . . . H14 H 0.0006 -0.2461 0.5957 0.032 Uiso 1 1 calc R . . C18 C 0.1395(3) -0.0035(2) 0.42897(19) 0.0200(6) Uani 1 1 d . . . H15A H 0.426(5) -0.6510(14) 0.599(3) 0.076(13) Uiso 1 1 d D . . H15B H 0.534(3) -0.562(3) 0.633(2) 0.074(13) Uiso 1 1 d D . . 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 O8 0.0313(12) 0.0160(11) 0.0269(12) 0.0051(9) 0.0001(9) -0.0009(8) O15 0.0304(13) 0.0215(11) 0.0398(14) 0.0001(10) -0.0027(10) 0.0003(9) N1 0.0215(13) 0.0296(14) 0.0264(14) 0.0007(12) 0.0022(11) -0.0013(11) N1' 0.0319(15) 0.0205(13) 0.0306(15) -0.0010(12) 0.0083(12) -0.0028(11) N7 0.0256(13) 0.0141(12) 0.0246(14) 0.0024(11) 0.0018(11) -0.0003(10) N7' 0.0243(13) 0.0136(12) 0.0229(14) 0.0026(10) 0.0022(10) 0.0013(9) N10 0.0266(14) 0.0227(13) 0.0358(16) 0.0052(12) 0.0078(12) 0.0036(11) N12 0.0286(14) 0.0184(13) 0.0321(15) 0.0027(12) 0.0054(12) 0.0060(11) C2' 0.0272(17) 0.0209(16) 0.0222(17) 0.0021(13) 0.0047(13) -0.0008(12) C2 0.0219(16) 0.0213(15) 0.0256(16) -0.0013(14) 0.0046(13) 0.0000(12) C3' 0.0190(15) 0.0203(15) 0.0202(16) -0.0014(12) 0.0066(12) -0.0010(12) C3 0.0198(15) 0.0186(15) 0.0220(16) -0.0020(13) 0.0048(12) -0.0012(12) C4' 0.0232(16) 0.0235(15) 0.0210(16) 0.0018(13) 0.0079(13) 0.0047(13) C4 0.0230(16) 0.0206(15) 0.0257(17) -0.0026(13) 0.0102(13) -0.0019(12) C5' 0.0256(16) 0.0305(17) 0.0249(17) 0.0007(14) -0.0001(13) 0.0008(13) C5 0.0236(16) 0.0274(17) 0.0256(17) -0.0064(14) 0.0062(13) -0.0068(13) C6 0.0222(16) 0.0352(18) 0.0239(17) -0.0017(15) 0.0045(13) -0.0035(14) C6' 0.0271(17) 0.0287(17) 0.0294(18) -0.0065(15) 0.0021(13) -0.0052(14) C9 0.0365(19) 0.0207(16) 0.037(2) -0.0060(14) 0.0047(15) 0.0006(13) C9' 0.0301(17) 0.0275(17) 0.0262(17) 0.0020(14) -0.0002(13) 0.0111(14) C11 0.0264(16) 0.0258(16) 0.0309(18) 0.0046(15) 0.0095(13) 0.0009(14) C13 0.0272(17) 0.0284(18) 0.0349(19) 0.0104(14) 0.0088(15) 0.0019(13) C14 0.0246(17) 0.0274(16) 0.0289(18) 0.0031(14) 0.0092(14) 0.0061(13) C18 0.0217(16) 0.0184(15) 0.0213(15) 0.0013(13) 0.0079(12) 0.0039(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O8 C18 1.223(3) . ? O15 H15A 0.964(19) . ? O15 H15B 0.943(19) . ? N1 C6 1.334(4) . ? N1 C2 1.345(4) . ? N1' C6' 1.335(4) . ? N1' C2' 1.351(4) . ? N7 C18 1.372(3) . ? N7 C3 1.409(3) . ? N7 H7 0.88 . ? N7' C18 1.383(3) . ? N7' C3' 1.409(3) . ? N7' H7' 0.88 . ? N10 C11 1.324(4) . ? N10 C14 1.381(4) . ? N12 C11 1.340(4) . ? N12 C13 1.366(4) . ? N12 H12 0.88 . ? C2' C3' 1.391(4) . ? C2' H2' 0.95 . ? C2 C3 1.395(4) . ? C2 H2 0.95 . ? C3' C4' 1.405(4) . ? C3 C4 1.400(4) . ? C4' C5' 1.381(4) . ? C4' C9' 1.500(4) . ? C4 C5 1.385(4) . ? C4 C9 1.509(4) . ? C5' C6' 1.378(4) . ? C5' H5' 0.95 . ? C5 C6 1.382(4) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C6' H6' 0.95 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C9' H9'1 0.98 . ? C9' H9'2 0.98 . ? C9' H9'3 0.98 . ? C11 H11 0.95 . ? C13 C14 1.349(4) . ? C13 H13 0.95 . ? C14 H14 0.95 . ? 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 H15A O15 H15B 106(3) . . ? C6 N1 C2 117.4(2) . . ? C6' N1' C2' 117.7(2) . . ? C18 N7 C3 126.0(2) . . ? C18 N7 H7 117 . . ? C3 N7 H7 117 . . ? C18 N7' C3' 126.3(2) . . ? C18 N7' H7' 116.9 . . ? C3' N7' H7' 116.9 . . ? C11 N10 C14 104.3(2) . . ? C11 N12 C13 107.5(2) . . ? C11 N12 H12 126.3 . . ? C13 N12 H12 126.3 . . ? N1' C2' C3' 122.9(3) . . ? N1' C2' H2' 118.5 . . ? C3' C2' H2' 118.5 . . ? N1 C2 C3 123.4(3) . . ? N1 C2 H2 118.3 . . ? C3 C2 H2 118.3 . . ? C2' C3' C4' 118.7(3) . . ? C2' C3' N7' 123.0(3) . . ? C4' C3' N7' 118.3(2) . . ? C2 C3 C4 118.7(3) . . ? C2 C3 N7 122.5(2) . . ? C4 C3 N7 118.8(2) . . ? C5' C4' C3' 117.4(3) . . ? C5' C4' C9' 121.0(3) . . ? C3' C4' C9' 121.5(3) . . ? C5 C4 C3 117.2(3) . . ? C5 C4 C9 120.6(3) . . ? C3 C4 C9 122.2(3) . . ? C6' C5' C4' 120.4(3) . . ? C6' C5' H5' 119.8 . . ? C4' C5' H5' 119.8 . . ? C6 C5 C4 120.5(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? N1 C6 C5 122.7(3) . . ? N1 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? N1' C6' C5' 122.8(3) . . ? N1' C6' H6' 118.6 . . ? C5' C6' H6' 118.6 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4' C9' H9'1 109.5 . . ? C4' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C4' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? N10 C11 N12 111.8(3) . . ? N10 C11 H11 124.1 . . ? N12 C11 H11 124.1 . . ? C14 C13 N12 105.8(3) . . ? C14 C13 H13 127.1 . . ? N12 C13 H13 127.1 . . ? C13 C14 N10 110.6(3) . . ? C13 C14 H14 124.7 . . ? N10 C14 H14 124.7 . . ? O8 C18 N7 124.1(3) . . ? O8 C18 N7' 123.7(2) . . ? N7 C18 N7' 112.2(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6' N1' C2' C3' 0.2(4) . . . . ? C6 N1 C2 C3 -0.9(4) . . . . ? N1' C2' C3' C4' 1.0(4) . . . . ? N1' C2' C3' N7' 178.5(3) . . . . ? C18 N7' C3' C2' 16.4(4) . . . . ? C18 N7' C3' C4' -166.1(3) . . . . ? N1 C2 C3 C4 -2.0(4) . . . . ? N1 C2 C3 N7 -179.8(3) . . . . ? C18 N7 C3 C2 -23.4(4) . . . . ? C18 N7 C3 C4 158.8(3) . . . . ? C2' C3' C4' C5' -1.6(4) . . . . ? N7' C3' C4' C5' -179.2(3) . . . . ? C2' C3' C4' C9' 178.0(3) . . . . ? N7' C3' C4' C9' 0.4(4) . . . . ? C2 C3 C4 C5 2.7(4) . . . . ? N7 C3 C4 C5 -179.4(2) . . . . ? C2 C3 C4 C9 -176.6(3) . . . . ? N7 C3 C4 C9 1.2(4) . . . . ? C3' C4' C5' C6' 1.1(4) . . . . ? C9' C4' C5' C6' -178.5(3) . . . . ? C3 C4 C5 C6 -0.7(4) . . . . ? C9 C4 C5 C6 178.7(3) . . . . ? C2 N1 C6 C5 3.1(4) . . . . ? C4 C5 C6 N1 -2.4(4) . . . . ? C2' N1' C6' C5' -0.7(4) . . . . ? C4' C5' C6' N1' 0.0(5) . . . . ? C14 N10 C11 N12 0.1(3) . . . . ? C13 N12 C11 N10 -0.1(3) . . . . ? C11 N12 C13 C14 0.1(3) . . . . ? N12 C13 C14 N10 0.0(3) . . . . ? C11 N10 C14 C13 -0.1(3) . . . . ? C3 N7 C18 O8 0.9(4) . . . . ? C3 N7 C18 N7' -178.7(2) . . . . ? C3' N7' C18 O8 1.5(4) . . . . ? C3' N7' C18 N7 -178.9(2) . . . . ? # Attachment '- Schalley_DT-ART-01-2012-030190_Compound12.cif' data_12 _database_code_depnum_ccdc_archive 'CCDC 864204' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound12.cif' _audit_creation_date 2008-11-14T08:10:21-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 12' _chemical_formula_moiety 'C13 H14 N4 O1' _chemical_formula_sum 'C13 H14 N4 O' _chemical_formula_weight 242.28 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pc21b _symmetry_space_group_name_Hall 'P -2bc -2c' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, y, z+1/2' 'x, y+1/2, -z+1/2' _cell_length_a 8.3851(7) _cell_length_b 11.5345(6) _cell_length_c 12.4214(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1201.37(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123.0(1) _cell_measurement_reflns_used 23483 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.34 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.09 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 123.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.999296E-1 _diffrn_orient_matrix_ub_12 -0.243703E-1 _diffrn_orient_matrix_ub_13 0.376832E-1 _diffrn_orient_matrix_ub_21 0.446935E-1 _diffrn_orient_matrix_ub_22 0.283836E-1 _diffrn_orient_matrix_ub_23 0.698391E-1 _diffrn_orient_matrix_ub_31 -0.473609E-1 _diffrn_orient_matrix_ub_32 0.782054E-1 _diffrn_orient_matrix_ub_33 -0.136043E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0869 _diffrn_reflns_av_unetI/netI 0.057 _diffrn_reflns_number 7448 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 1112 _reflns_number_gt 950 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0347P)^2^+0.3216P] 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_number_reflns 1112 _refine_ls_number_parameters 165 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.088 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.176 _refine_diff_density_min -0.18 _refine_diff_density_rms 0.041 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O8 O 0.3148(3) 0.55996(19) 0.69314(19) 0.0305(6) Uani 1 1 d . . . N1 N 0.5636(4) 0.3267(2) 0.4988(2) 0.0316(8) Uani 1 1 d . . . N1' N 0.1362(5) 0.7392(3) 1.0655(2) 0.0403(8) Uani 1 1 d . . . N7' N 0.2864(4) 0.5265(2) 0.8745(2) 0.0280(7) Uani 1 1 d . . . H7' H 0.303 0.4736 0.9243 0.034 Uiso 1 1 calc R . . N7 N 0.4179(4) 0.3962(2) 0.7717(2) 0.0266(7) Uani 1 1 d . . . H7 H 0.4224 0.3597 0.8338 0.032 Uiso 1 1 calc R . . C2' C 0.2088(5) 0.6497(3) 1.0194(3) 0.0356(10) Uani 1 1 d . . . H2' H 0.2635 0.5965 1.0647 0.043 Uiso 1 1 calc R . . C2 C 0.4880(5) 0.3814(3) 0.5791(3) 0.0307(9) Uani 1 1 d . . . H2 H 0.429 0.4497 0.5634 0.037 Uiso 1 1 calc R . . C3 C 0.4932(5) 0.3414(3) 0.6848(3) 0.0250(8) Uani 1 1 d . . . C3' C 0.2100(5) 0.6286(3) 0.9084(3) 0.0258(8) Uani 1 1 d . . . C4 C 0.5792(4) 0.2413(3) 0.7058(3) 0.0258(8) Uani 1 1 d . . . H4 H 0.5847 0.2125 0.7774 0.031 Uiso 1 1 calc R . . C4' C 0.1329(5) 0.7077(3) 0.8426(3) 0.0271(9) Uani 1 1 d . . . H4' H 0.1324 0.6974 0.7668 0.033 Uiso 1 1 calc R . . C5' C 0.0568(5) 0.8015(3) 0.8883(3) 0.0297(9) Uani 1 1 d . . . C5 C 0.6572(5) 0.1827(3) 0.6239(3) 0.0247(8) Uani 1 1 d . . . C6' C 0.0619(5) 0.8128(3) 1.0000(3) 0.0375(10) Uani 1 1 d . . . H6' H 0.009 0.8773 1.0314 0.045 Uiso 1 1 calc R . . C6 C 0.6460(5) 0.2291(3) 0.5212(3) 0.0300(9) Uani 1 1 d . . . H6 H 0.6988 0.1903 0.4639 0.036 Uiso 1 1 calc R . . C8 C 0.3386(4) 0.4994(3) 0.7717(3) 0.0246(8) Uani 1 1 d . . . C9 C 0.7511(5) 0.0739(3) 0.6448(3) 0.0348(10) Uani 1 1 d . . . H9A H 0.8255 0.0607 0.5852 0.052 Uiso 1 1 calc R . . H9B H 0.678 0.0079 0.6506 0.052 Uiso 1 1 calc R . . H9C H 0.811 0.0822 0.7121 0.052 Uiso 1 1 calc R . . C9' C -0.0302(5) 0.8901(3) 0.8208(3) 0.0365(10) Uani 1 1 d . . . H9'1 H 0.0253 0.9647 0.8253 0.055 Uiso 1 1 calc R . . H9'2 H -0.1395 0.8989 0.8476 0.055 Uiso 1 1 calc R . . H9'3 H -0.033 0.8641 0.7457 0.055 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 O8 0.0420(17) 0.0305(13) 0.0191(13) 0.0050(10) -0.0006(12) 0.0040(12) N1 0.042(2) 0.0346(17) 0.0183(15) 0.0010(12) 0.0043(16) -0.0004(17) N1' 0.052(2) 0.0419(19) 0.0271(17) -0.0082(16) -0.0006(17) 0.0084(17) N7' 0.039(2) 0.0287(16) 0.0157(15) 0.0033(12) 0.0011(15) 0.0025(15) N7 0.038(2) 0.0275(15) 0.0138(15) 0.0024(12) 0.0021(13) 0.0020(15) C2' 0.045(3) 0.037(2) 0.026(2) -0.0018(15) -0.004(2) 0.0006(19) C2 0.042(3) 0.0286(19) 0.0217(19) 0.0030(15) -0.0029(18) -0.0006(18) C3 0.030(2) 0.0272(17) 0.0182(19) -0.0031(13) 0.0006(16) -0.0074(17) C3' 0.024(2) 0.0299(19) 0.0237(19) -0.0029(15) 0.0018(17) -0.0037(16) C4 0.030(2) 0.0268(18) 0.0206(17) 0.0026(15) -0.0013(16) -0.0035(17) C4' 0.033(2) 0.0274(18) 0.0214(19) 0.0014(14) 0.0004(16) -0.0053(17) C5' 0.029(2) 0.0288(18) 0.031(2) -0.0012(16) -0.0020(18) -0.0010(17) C5 0.025(2) 0.0224(18) 0.027(2) -0.0007(15) -0.0018(15) -0.0052(16) C6' 0.040(3) 0.036(2) 0.036(2) -0.0084(18) -0.001(2) 0.004(2) C6 0.037(2) 0.0291(19) 0.024(2) -0.0075(16) 0.0068(18) -0.0055(17) C8 0.029(2) 0.0276(19) 0.0174(19) -0.0011(15) -0.0001(16) -0.0009(16) C9 0.036(3) 0.033(2) 0.036(2) 0.0033(18) 0.0017(19) 0.0042(18) C9' 0.038(3) 0.034(2) 0.038(2) -0.0003(17) -0.003(2) 0.0053(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O8 C8 1.216(4) . ? N1 C2 1.339(5) . ? N1 C6 1.350(5) . ? N1' C2' 1.328(5) . ? N1' C6' 1.331(5) . ? N7' C8 1.386(4) . ? N7' C3' 1.405(5) . ? N7' H7' 0.88 . ? N7 C8 1.363(4) . ? N7 C3 1.402(4) . ? N7 H7 0.88 . ? C2' C3' 1.401(5) . ? C2' H2' 0.95 . ? C2 C3 1.393(5) . ? C2 H2 0.95 . ? C3 C4 1.386(5) . ? C3' C4' 1.385(5) . ? C4 C5 1.385(5) . ? C4 H4 0.95 . ? C4' C5' 1.378(5) . ? C4' H4' 0.95 . ? C5' C6' 1.394(5) . ? C5' C9' 1.509(5) . ? C5 C6 1.387(5) . ? C5 C9 1.504(5) . ? C6' H6' 0.95 . ? C6 H6 0.95 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C9' H9'1 0.98 . ? C9' H9'2 0.98 . ? C9' H9'3 0.98 . ? 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 C2 N1 C6 118.8(3) . . ? C2' N1' C6' 116.5(3) . . ? C8 N7' C3' 127.5(3) . . ? C8 N7' H7' 116.2 . . ? C3' N7' H7' 116.2 . . ? C8 N7 C3 127.9(3) . . ? C8 N7 H7 116.1 . . ? C3 N7 H7 116.1 . . ? N1' C2' C3' 124.2(4) . . ? N1' C2' H2' 117.9 . . ? C3' C2' H2' 117.9 . . ? N1 C2 C3 122.1(3) . . ? N1 C2 H2 119 . . ? C3 C2 H2 119 . . ? C4 C3 C2 118.0(3) . . ? C4 C3 N7 117.7(3) . . ? C2 C3 N7 124.2(3) . . ? C4' C3' C2' 117.6(3) . . ? C4' C3' N7' 126.1(3) . . ? C2' C3' N7' 116.4(3) . . ? C5 C4 C3 120.9(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C5' C4' C3' 119.4(3) . . ? C5' C4' H4' 120.3 . . ? C3' C4' H4' 120.3 . . ? C4' C5' C6' 118.0(3) . . ? C4' C5' C9' 121.8(3) . . ? C6' C5' C9' 120.3(3) . . ? C4 C5 C6 117.1(3) . . ? C4 C5 C9 121.9(3) . . ? C6 C5 C9 121.0(3) . . ? N1' C6' C5' 124.3(4) . . ? N1' C6' H6' 117.9 . . ? C5' C6' H6' 117.9 . . ? N1 C6 C5 123.1(3) . . ? N1 C6 H6 118.5 . . ? C5 C6 H6 118.5 . . ? O8 C8 N7 125.6(3) . . ? O8 C8 N7' 123.9(3) . . ? N7 C8 N7' 110.5(3) . . ? C5 C9 H9A 109.5 . . ? C5 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C5 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5' C9' H9'1 109.5 . . ? C5' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C5' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6' N1' C2' C3' -0.7(6) . . . . ? C6 N1 C2 C3 0.7(5) . . . . ? N1 C2 C3 C4 -0.4(5) . . . . ? N1 C2 C3 N7 179.1(3) . . . . ? C8 N7 C3 C4 174.3(3) . . . . ? C8 N7 C3 C2 -5.2(6) . . . . ? N1' C2' C3' C4' 1.3(6) . . . . ? N1' C2' C3' N7' -177.0(4) . . . . ? C8 N7' C3' C4' 19.2(6) . . . . ? C8 N7' C3' C2' -162.7(4) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? N7 C3 C4 C5 -179.8(3) . . . . ? C2' C3' C4' C5' -1.1(6) . . . . ? N7' C3' C4' C5' 177.0(3) . . . . ? C3' C4' C5' C6' 0.4(6) . . . . ? C3' C4' C5' C9' -179.6(3) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C3 C4 C5 C9 -180.0(3) . . . . ? C2' N1' C6' C5' -0.2(6) . . . . ? C4' C5' C6' N1' 0.3(6) . . . . ? C9' C5' C6' N1' -179.8(4) . . . . ? C2 N1 C6 C5 -0.4(6) . . . . ? C4 C5 C6 N1 -0.1(5) . . . . ? C9 C5 C6 N1 -179.7(3) . . . . ? C3 N7 C8 O8 2.9(6) . . . . ? C3 N7 C8 N7' -177.6(3) . . . . ? C3' N7' C8 O8 -5.1(6) . . . . ? C3' N7' C8 N7 175.4(3) . . . . ? # Attachment '- Schalley_DT-ART-01-2012-030190_Compound13.cif' data_13 _database_code_depnum_ccdc_archive 'CCDC 864205' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound13.cif' _audit_creation_date 2008-11-14T08:06:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C13 H14 N4 O' _chemical_formula_sum 'C13 H14 N4 O' _chemical_formula_weight 242.28 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.3327(3) _cell_length_b 8.3914(3) _cell_length_c 19.4356(9) _cell_angle_alpha 90 _cell_angle_beta 91.255(2) _cell_angle_gamma 90 _cell_volume 1195.62(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 17212 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.103 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.09 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.178173E-1 _diffrn_orient_matrix_ub_12 0.698221E-1 _diffrn_orient_matrix_ub_13 0.410069E-1 _diffrn_orient_matrix_ub_21 -0.131868 _diffrn_orient_matrix_ub_22 0.302975E-1 _diffrn_orient_matrix_ub_23 -0.3968E-3 _diffrn_orient_matrix_ub_31 -0.300034E-1 _diffrn_orient_matrix_ub_32 -0.91697E-1 _diffrn_orient_matrix_ub_33 0.310933E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_av_unetI/netI 0.0441 _diffrn_reflns_number 15175 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 12.5 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 2094 _reflns_number_gt 1568 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0529P)^2^+0.7548P] 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_number_reflns 2094 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1288 _refine_ls_wR_factor_gt 0.1163 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.206 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O O 0.0106 0.006 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O8 O 0.2423(2) -0.0022(2) 0.42603(8) 0.0364(5) Uani 1 1 d . . . N1' N 0.7934(3) 0.3067(2) 0.31394(9) 0.0295(5) Uani 1 1 d . . . N1 N -0.3011(3) -0.3129(2) 0.31608(10) 0.0302(5) Uani 1 1 d . . . N7 N 0.1122(3) -0.0734(2) 0.32441(9) 0.0276(5) Uani 1 1 d . . . H7 H 0.1234 -0.0693 0.2805 0.033 Uiso 1 1 calc R . . N7' N 0.3803(3) 0.0653(2) 0.32343(9) 0.0275(5) Uani 1 1 d . . . H7' H 0.366 0.0586 0.2795 0.033 Uiso 1 1 calc R . . C2 C -0.1485(3) -0.2331(3) 0.30117(12) 0.0308(6) Uani 1 1 d . . . H2 H -0.1115 -0.2319 0.2557 0.037 Uiso 1 1 calc R . . C2' C 0.6417(3) 0.2275(3) 0.29964(12) 0.0304(6) Uani 1 1 d . . . H2' H 0.601 0.2267 0.254 0.036 Uiso 1 1 calc R . . C3' C 0.5353(3) 0.1435(3) 0.34755(11) 0.0246(5) Uani 1 1 d . . . C3 C -0.0439(3) -0.1529(3) 0.34941(11) 0.0256(5) Uani 1 1 d . . . C4 C -0.1046(3) -0.1590(3) 0.41757(11) 0.0282(6) Uani 1 1 d . . . H4 H -0.0386 -0.1077 0.4524 0.034 Uiso 1 1 calc R . . C4' C 0.5947(3) 0.1437(3) 0.41504(12) 0.0288(6) Uani 1 1 d . . . H4' H 0.531 0.0907 0.449 0.035 Uiso 1 1 calc R . . C5' C 0.7527(3) 0.2258(3) 0.43000(12) 0.0308(6) Uani 1 1 d . . . H5' H 0.7961 0.2282 0.4753 0.037 Uiso 1 1 calc R . . C5 C -0.2638(3) -0.2422(3) 0.43295(12) 0.0296(6) Uani 1 1 d . . . H5 H -0.3036 -0.2458 0.478 0.035 Uiso 1 1 calc R . . C6 C -0.3608(3) -0.3181(3) 0.38190(11) 0.0273(6) Uani 1 1 d . . . C6' C 0.8508(3) 0.3060(3) 0.37954(12) 0.0272(6) Uani 1 1 d . . . C8 C 0.2446(3) -0.0038(3) 0.36316(11) 0.0248(5) Uani 1 1 d . . . C9' C 1.0236(3) 0.3946(3) 0.39404(13) 0.0346(6) Uani 1 1 d . . . H9'1 H 1.1256 0.33 0.3813 0.052 Uiso 1 1 calc R . . H9'2 H 1.0329 0.4191 0.4422 0.052 Uiso 1 1 calc R . . H9'3 H 1.0237 0.4916 0.3679 0.052 Uiso 1 1 calc R . . C9 C -0.5351(3) -0.4059(3) 0.39664(13) 0.0357(6) Uani 1 1 d . . . H9A H -0.6376 -0.3422 0.3821 0.054 Uiso 1 1 calc R . . H9B H -0.5415 -0.4262 0.4451 0.054 Uiso 1 1 calc R . . H9C H -0.537 -0.5052 0.3721 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 O8 0.0414(10) 0.0471(12) 0.0207(9) -0.0007(8) -0.0020(7) -0.0128(9) N1' 0.0318(11) 0.0325(12) 0.0243(11) 0.0020(9) -0.0017(8) -0.0039(9) N1 0.0312(11) 0.0308(12) 0.0283(11) -0.0012(9) -0.0041(8) -0.0040(9) N7 0.0302(11) 0.0332(12) 0.0194(10) -0.0009(8) -0.0027(8) -0.0031(9) N7' 0.0309(11) 0.0316(12) 0.0197(10) 0.0008(8) -0.0045(8) -0.0036(9) C2 0.0344(14) 0.0364(15) 0.0216(12) -0.0027(10) -0.0020(10) -0.0023(11) C2' 0.0357(14) 0.0343(15) 0.0210(12) 0.0018(10) -0.0033(10) -0.0024(11) C3' 0.0281(12) 0.0216(13) 0.0240(12) 0.0009(9) -0.0004(9) 0.0009(10) C3 0.0270(12) 0.0237(13) 0.0261(12) -0.0012(10) -0.0025(10) 0.0013(10) C4 0.0308(13) 0.0292(14) 0.0244(12) -0.0063(10) -0.0016(10) 0.0011(10) C4' 0.0296(13) 0.0311(15) 0.0257(12) 0.0049(10) -0.0002(10) 0.0000(11) C5' 0.0346(14) 0.0342(15) 0.0233(13) 0.0024(11) -0.0044(10) 0.0033(11) C5 0.0329(13) 0.0337(15) 0.0223(13) 0.0004(10) 0.0041(10) 0.0011(11) C6 0.0277(12) 0.0269(14) 0.0272(12) 0.0000(10) -0.0023(10) 0.0033(10) C6' 0.0281(12) 0.0269(14) 0.0266(12) -0.0002(10) -0.0012(10) 0.0036(10) C8 0.0283(12) 0.0222(13) 0.0237(12) 0.0006(10) -0.0008(9) 0.0009(10) C9' 0.0344(14) 0.0360(15) 0.0333(14) -0.0027(12) -0.0035(11) -0.0012(12) C9 0.0340(14) 0.0394(16) 0.0337(14) 0.0002(12) -0.0025(11) -0.0045(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 O8 C8 1.223(3) . ? N1' C2' 1.321(3) . ? N1' C6' 1.334(3) . ? N1 C2 1.341(3) . ? N1 C6 1.362(3) . ? N7 C8 1.348(3) . ? N7 C3 1.420(3) . ? N7 H7 0.86 . ? N7' C3' 1.385(3) . ? N7' C8 1.399(3) . ? N7' H7' 0.86 . ? C2 C3 1.374(3) . ? C2 H2 0.93 . ? C2' C3' 1.415(3) . ? C2' H2' 0.93 . ? C3' C4' 1.373(3) . ? C3 C4 1.408(3) . ? C4 C5 1.398(3) . ? C4 H4 0.93 . ? C4' C5' 1.373(3) . ? C4' H4' 0.93 . ? C5' C6' 1.401(3) . ? C5' H5' 0.93 . ? C5 C6 1.366(3) . ? C5 H5 0.93 . ? C6 C9 1.508(3) . ? C6' C9' 1.491(3) . ? C9' H9'1 0.96 . ? C9' H9'2 0.96 . ? C9' H9'3 0.96 . ? C9 H9A 0.96 . ? C9 H9B 0.96 . ? C9 H9C 0.96 . ? 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 C2' N1' C6' 116.5(2) . . ? C2 N1 C6 120.4(2) . . ? C8 N7 C3 126.03(19) . . ? C8 N7 H7 117 . . ? C3 N7 H7 117 . . ? C3' N7' C8 126.74(19) . . ? C3' N7' H7' 116.6 . . ? C8 N7' H7' 116.6 . . ? N1 C2 C3 123.6(2) . . ? N1 C2 H2 118.2 . . ? C3 C2 H2 118.2 . . ? N1' C2' C3' 125.9(2) . . ? N1' C2' H2' 117.1 . . ? C3' C2' H2' 117.1 . . ? C4' C3' N7' 124.4(2) . . ? C4' C3' C2' 117.4(2) . . ? N7' C3' C2' 118.23(19) . . ? C2 C3 C4 116.1(2) . . ? C2 C3 N7 116.0(2) . . ? C4 C3 N7 127.8(2) . . ? C5 C4 C3 120.2(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C3' C4' C5' 116.8(2) . . ? C3' C4' H4' 121.6 . . ? C5' C4' H4' 121.6 . . ? C4' C5' C6' 122.4(2) . . ? C4' C5' H5' 118.8 . . ? C6' C5' H5' 118.8 . . ? C6 C5 C4 120.1(2) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? N1 C6 C5 119.6(2) . . ? N1 C6 C9 119.0(2) . . ? C5 C6 C9 121.3(2) . . ? N1' C6' C5' 121.0(2) . . ? N1' C6' C9' 115.3(2) . . ? C5' C6' C9' 123.7(2) . . ? O8 C8 N7 122.5(2) . . ? O8 C8 N7' 124.9(2) . . ? N7 C8 N7' 112.55(19) . . ? C6' C9' H9'1 109.5 . . ? C6' C9' H9'2 109.5 . . ? H9'1 C9' H9'2 109.5 . . ? C6' C9' H9'3 109.5 . . ? H9'1 C9' H9'3 109.5 . . ? H9'2 C9' H9'3 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 C3 0.0(4) . . . . ? C6' N1' C2' C3' 0.4(4) . . . . ? C8 N7' C3' C4' 10.8(4) . . . . ? C8 N7' C3' C2' -170.1(2) . . . . ? N1' C2' C3' C4' -0.2(4) . . . . ? N1' C2' C3' N7' -179.4(2) . . . . ? N1 C2 C3 C4 0.5(4) . . . . ? N1 C2 C3 N7 -179.3(2) . . . . ? C8 N7 C3 C2 -171.8(2) . . . . ? C8 N7 C3 C4 8.5(4) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? N7 C3 C4 C5 179.3(2) . . . . ? N7' C3' C4' C5' 179.2(2) . . . . ? C2' C3' C4' C5' 0.1(3) . . . . ? C3' C4' C5' C6' -0.2(4) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C2 N1 C6 C5 -0.3(4) . . . . ? C2 N1 C6 C9 178.7(2) . . . . ? C4 C5 C6 N1 0.3(4) . . . . ? C4 C5 C6 C9 -178.7(2) . . . . ? C2' N1' C6' C5' -0.5(4) . . . . ? C2' N1' C6' C9' 179.2(2) . . . . ? C4' C5' C6' N1' 0.4(4) . . . . ? C4' C5' C6' C9' -179.3(2) . . . . ? C3 N7 C8 O8 -0.2(4) . . . . ? C3 N7 C8 N7' -179.8(2) . . . . ? C3' N7' C8 O8 1.4(4) . . . . ? C3' N7' C8 N7 -179.0(2) . . . . ? # Attachment '- Schalley_DT-ART-01-2012-030190_Compound23a.CIF' data_squeeze _database_code_depnum_ccdc_archive 'CCDC 864206' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound23a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H52 N16 O18 Pd2' _chemical_formula_weight 1137.68 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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.577(4) _cell_length_b 15.891(5) _cell_length_c 20.526(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.995(7) _cell_angle_gamma 90.00 _cell_volume 4426(2) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 1013 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.0 _exptl_crystal_description platelett _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2320 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.865 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'SADABS (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-AXS SMART CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65917 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0338 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 30.05 _reflns_number_total 12812 _reflns_number_gt 10995 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-AXS)' _computing_cell_refinement 'SAINT (Bruker-AXS)' _computing_data_reduction 'SAINT (Bruker-AXS)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Refinement with the listed atoms show resudual electron density due to a heavily disordered nitrate anion which could not be refined with split atoms. Therefore the option "SQUEEZE" of the program package PLATON (Spek, A.L. (2009). Acta Cryst. D65, 148-155.) was used to create a hkl file taking into account the residual electron density in the void areas. Therefore the atoms list and unit card do not agree. The hydrogen atoms at the hydrate water molecules were not included. ; _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^)+(0.0079P)^2^+40.8987P] 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_number_reflns 12812 _refine_ls_number_parameters 554 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1347 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C21 C 0.1885(3) 0.0061(3) 0.3099(2) 0.0186(9) Uani 1 1 d . . . H21 H 0.2005 0.0507 0.3400 0.022 Uiso 1 1 calc R . . C22 C 0.4370(3) 0.0229(3) 0.3556(2) 0.0183(9) Uani 1 1 d . . . H22 H 0.3870 0.0638 0.3614 0.022 Uiso 1 1 calc R . . C31 C 0.1413(3) 0.0234(3) 0.2490(2) 0.0164(8) Uani 1 1 d . . . C32 C 0.5256(3) 0.0471(3) 0.3302(2) 0.0163(8) Uani 1 1 d . . . C41 C 0.1242(3) -0.0423(3) 0.2066(2) 0.0188(9) Uani 1 1 d . . . H41 H 0.0918 -0.0320 0.1656 0.023 Uiso 1 1 calc R . . C42 C 0.5971(4) -0.0143(3) 0.3204(2) 0.0195(9) Uani 1 1 d . . . H42 H 0.6581 0.0010 0.3023 0.023 Uiso 1 1 calc R . . C51 C 0.1537(3) -0.1236(3) 0.2228(2) 0.0194(9) Uani 1 1 d . . . C52 C 0.5794(4) -0.0973(3) 0.3368(2) 0.0209(9) Uani 1 1 d . . . C61 C 0.1991(3) -0.1359(3) 0.2841(2) 0.0183(9) Uani 1 1 d . . . H61 H 0.2182 -0.1912 0.2967 0.022 Uiso 1 1 calc R . . C62 C 0.4889(4) -0.1162(3) 0.3633(2) 0.0190(9) Uani 1 1 d . . . H62 H 0.4756 -0.1727 0.3754 0.023 Uiso 1 1 calc R . . C71 C 0.1389(5) -0.1965(4) 0.1770(3) 0.0327(13) Uani 1 1 d . . . H71A H 0.1109 -0.2441 0.2005 0.049 Uiso 1 1 calc R . . H71B H 0.2024 -0.2130 0.1596 0.049 Uiso 1 1 calc R . . H71C H 0.0936 -0.1801 0.1410 0.049 Uiso 1 1 calc R . . C72 C 0.6544(4) -0.1655(3) 0.3283(3) 0.0316(12) Uani 1 1 d . . . H72A H 0.6750 -0.1660 0.2830 0.047 Uiso 1 1 calc R . . H72B H 0.6255 -0.2200 0.3390 0.047 Uiso 1 1 calc R . . H72C H 0.7119 -0.1548 0.3574 0.047 Uiso 1 1 calc R . . C91 C 0.1447(4) 0.1791(3) 0.2602(3) 0.0223(10) Uani 1 1 d . . . C92 C 0.4993(4) 0.2003(3) 0.3348(2) 0.0195(9) Uani 1 1 d . . . C102 C 0.1513(4) 0.4940(4) 0.5263(2) 0.0260(11) Uani 1 1 d . . . H10A H 0.1565 0.4390 0.5488 0.031 Uiso 1 1 calc R . . H10B H 0.0974 0.5265 0.5456 0.031 Uiso 1 1 calc R . . C103 C 0.2467(4) 0.5412(4) 0.5346(2) 0.0251(10) Uani 1 1 d . . . H10C H 0.2384 0.5997 0.5188 0.030 Uiso 1 1 calc R . . H10D H 0.2678 0.5429 0.5812 0.030 Uiso 1 1 calc R . . C112 C 0.1984(4) -0.1636(3) 0.5231(2) 0.0236(10) Uani 1 1 d . . . C113 C 0.2817(4) -0.1104(3) 0.5509(2) 0.0215(9) Uani 1 1 d . . . H11A H 0.2576 -0.0532 0.5610 0.026 Uiso 1 1 calc R . . H11B H 0.3090 -0.1359 0.5917 0.026 Uiso 1 1 calc R . . C21' C 0.1628(3) 0.3541(3) 0.3110(2) 0.0188(9) Uani 1 1 d . . . H21' H 0.1802 0.3122 0.3423 0.023 Uiso 1 1 calc R . . C22' C 0.4139(4) 0.3721(3) 0.3491(3) 0.0222(10) Uani 1 1 d . . . H22' H 0.3676 0.3281 0.3548 0.027 Uiso 1 1 calc R . . C31' C 0.1163(3) 0.3311(3) 0.2530(2) 0.0175(9) Uani 1 1 d . . . C32' C 0.5044(4) 0.3537(3) 0.3222(2) 0.0196(9) Uani 1 1 d . . . C41' C 0.0898(3) 0.3927(3) 0.2071(3) 0.0210(9) Uani 1 1 d . . . H41' H 0.0574 0.3773 0.1671 0.025 Uiso 1 1 calc R . . C42' C 0.5689(3) 0.4199(3) 0.3121(2) 0.0177(9) Uani 1 1 d . . . H42' H 0.6304 0.4094 0.2930 0.021 Uiso 1 1 calc R . . C51' C 0.1111(3) 0.4763(3) 0.2204(3) 0.0207(9) Uani 1 1 d . . . C52' C 0.5445(3) 0.5011(3) 0.3297(2) 0.0152(8) Uani 1 1 d . . . C61' C 0.1577(4) 0.4947(3) 0.2800(3) 0.0213(10) Uani 1 1 d . . . H61' H 0.1714 0.5518 0.2904 0.026 Uiso 1 1 calc R . . C62' C 0.4537(3) 0.5137(3) 0.3584(2) 0.0170(8) Uani 1 1 d . . . H62' H 0.4363 0.5688 0.3719 0.020 Uiso 1 1 calc R . . C71' C 0.0883(4) 0.5460(3) 0.1719(3) 0.0283(11) Uani 1 1 d . . . H71D H 0.0888 0.5233 0.1276 0.042 Uiso 1 1 calc R . . H71E H 0.1383 0.5903 0.1768 0.042 Uiso 1 1 calc R . . H71F H 0.0232 0.5697 0.1801 0.042 Uiso 1 1 calc R . . C72' C 0.6118(4) 0.5754(3) 0.3204(3) 0.0209(9) Uani 1 1 d . . . H72D H 0.6665 0.5731 0.3528 0.031 Uiso 1 1 calc R . . H72E H 0.5748 0.6277 0.3260 0.031 Uiso 1 1 calc R . . H72F H 0.6378 0.5736 0.2765 0.031 Uiso 1 1 calc R . . N1 N 0.1676(3) -0.1268(3) 0.4584(2) 0.0196(8) Uani 1 1 d . . . H11C H 0.1272 -0.0812 0.4642 0.024 Uiso 1 1 calc R . . H11D H 0.1335 -0.1662 0.4337 0.024 Uiso 1 1 calc R . . N2 N 0.3592(3) -0.1057(3) 0.5016(2) 0.0210(8) Uani 1 1 d . . . H11E H 0.3962 -0.1542 0.5025 0.025 Uiso 1 1 calc R . . H11F H 0.4005 -0.0609 0.5106 0.025 Uiso 1 1 calc R . . N3 N 0.1298(3) 0.4810(3) 0.4553(2) 0.0211(8) Uani 1 1 d . . . H10E H 0.0957 0.5265 0.4384 0.025 Uiso 1 1 calc R . . H10F H 0.0913 0.4338 0.4492 0.025 Uiso 1 1 calc R . . N4 N 0.3213(3) 0.4970(3) 0.4964(2) 0.0204(8) Uani 1 1 d . . . H10G H 0.3422 0.4490 0.5179 0.025 Uiso 1 1 calc R . . H10H H 0.3750 0.5312 0.4910 0.025 Uiso 1 1 calc R . . N11 N 0.2166(3) -0.0722(2) 0.3259(2) 0.0169(7) Uani 1 1 d . . . N12 N 0.4202(3) -0.0573(2) 0.37231(19) 0.0153(7) Uani 1 1 d . . . N71 N 0.1101(3) 0.1044(3) 0.2326(2) 0.0213(8) Uani 1 1 d . . . H81 H 0.0639 0.1088 0.2017 0.026 Uiso 1 1 calc R . . N72 N 0.5455(3) 0.1303(3) 0.3118(2) 0.0198(8) Uani 1 1 d . . . H82 H 0.5915 0.1381 0.2833 0.024 Uiso 1 1 calc R . . N11' N 0.1841(3) 0.4351(3) 0.3237(2) 0.0186(8) Uani 1 1 d . . . N12' N 0.3909(3) 0.4504(3) 0.3673(2) 0.0184(8) Uani 1 1 d . . . N71' N 0.0934(3) 0.2469(3) 0.2369(2) 0.0240(9) Uani 1 1 d . . . H81' H 0.0427 0.2376 0.2099 0.029 Uiso 1 1 calc R . . N72' N 0.5303(3) 0.2719(3) 0.3043(2) 0.0218(8) Uani 1 1 d . . . H82' H 0.5692 0.2660 0.2712 0.026 Uiso 1 1 calc R . . N1N N 0.4577(4) 0.6896(3) 0.5050(2) 0.0299(10) Uani 1 1 d . . . N2N N 0.3147(3) 0.6778(3) 0.3159(2) 0.0239(9) Uani 1 1 d . . . N3N N 0.9393(3) 0.1802(3) 0.1016(2) 0.0213(8) Uani 1 1 d . . . O81 O 0.2141(3) 0.1817(2) 0.2998(2) 0.0312(9) Uani 1 1 d . . . O82 O 0.4386(3) 0.1991(2) 0.37715(19) 0.0300(9) Uani 1 1 d . . . O1N O 0.3852(3) 0.7044(3) 0.5382(2) 0.0415(11) Uani 1 1 d . . . O2N O 0.4885(3) 0.6155(3) 0.4969(2) 0.0339(9) Uani 1 1 d . . . O3N O 0.5027(3) 0.7492(3) 0.4790(2) 0.0341(9) Uani 1 1 d . . . O4N O 0.2707(3) 0.6550(3) 0.3645(2) 0.0362(10) Uani 1 1 d . . . O5N O 0.2829(3) 0.6568(3) 0.2599(2) 0.0287(8) Uani 1 1 d . . . O6N O 0.3911(3) 0.7217(3) 0.3211(2) 0.0368(10) Uani 1 1 d . . . O7N O 0.9396(3) 0.2439(3) 0.1368(2) 0.0317(9) Uani 1 1 d . . . O8N O 0.9786(3) 0.1131(2) 0.1222(2) 0.0301(9) Uani 1 1 d . . . O9N O 0.8995(3) 0.1825(3) 0.04604(18) 0.0265(8) Uani 1 1 d . . . O1W O 0.3865(3) 0.0825(3) 0.5005(2) 0.0354(9) Uani 1 1 d . . . O2W O 0.3077(4) 0.3195(3) 0.5408(3) 0.0488(12) Uani 1 1 d . . . O3W O 0.0352(3) 0.3210(3) 0.4446(2) 0.0408(11) Uani 1 1 d . . . Pd1 Pd 0.29125(2) -0.09088(2) 0.412489(17) 0.01420(8) Uani 1 1 d . . . Pd2 Pd 0.25805(2) 0.46692(2) 0.408717(17) 0.01496(8) Uani 1 1 d . . . 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 C21 0.020(2) 0.018(2) 0.018(2) -0.0017(17) -0.0038(17) -0.0007(17) C22 0.020(2) 0.013(2) 0.021(2) 0.0034(17) 0.0006(17) -0.0005(16) C31 0.019(2) 0.020(2) 0.0103(19) -0.0008(16) -0.0077(15) -0.0034(17) C32 0.022(2) 0.012(2) 0.014(2) 0.0008(15) 0.0001(16) -0.0012(16) C41 0.019(2) 0.020(2) 0.017(2) 0.0013(17) -0.0010(16) -0.0013(17) C42 0.019(2) 0.018(2) 0.022(2) 0.0015(17) 0.0031(17) 0.0014(17) C51 0.019(2) 0.019(2) 0.020(2) -0.0052(18) -0.0003(17) -0.0010(17) C52 0.024(2) 0.018(2) 0.021(2) 0.0006(18) -0.0001(18) 0.0019(18) C61 0.018(2) 0.013(2) 0.024(2) 0.0025(17) -0.0005(17) -0.0006(16) C62 0.024(2) 0.014(2) 0.019(2) -0.0002(17) 0.0005(17) -0.0019(17) C71 0.044(3) 0.022(3) 0.032(3) -0.011(2) -0.013(2) 0.006(2) C72 0.029(3) 0.019(2) 0.048(3) 0.006(2) 0.015(2) 0.006(2) C91 0.027(2) 0.010(2) 0.029(3) 0.0027(18) -0.004(2) 0.0016(17) C92 0.022(2) 0.017(2) 0.020(2) -0.0022(17) 0.0011(18) -0.0032(17) C102 0.021(2) 0.039(3) 0.019(2) 0.002(2) 0.0033(18) 0.002(2) C103 0.023(2) 0.033(3) 0.019(2) -0.006(2) 0.0012(18) 0.004(2) C112 0.030(3) 0.026(3) 0.014(2) 0.0043(18) -0.0024(18) -0.008(2) C113 0.024(2) 0.023(2) 0.017(2) -0.0003(18) -0.0014(18) -0.0051(18) C21' 0.020(2) 0.015(2) 0.021(2) -0.0013(17) -0.0005(17) 0.0007(17) C22' 0.024(2) 0.017(2) 0.026(3) -0.0023(18) 0.0061(19) -0.0032(18) C31' 0.015(2) 0.013(2) 0.024(2) -0.0021(17) 0.0009(17) 0.0023(16) C32' 0.025(2) 0.017(2) 0.017(2) -0.0013(17) 0.0035(17) 0.0004(17) C41' 0.018(2) 0.017(2) 0.028(3) 0.0014(18) 0.0029(18) 0.0013(17) C42' 0.017(2) 0.019(2) 0.018(2) 0.0010(17) 0.0034(16) 0.0024(16) C51' 0.017(2) 0.017(2) 0.028(2) 0.0024(18) 0.0060(18) 0.0014(17) C52' 0.0145(19) 0.015(2) 0.016(2) 0.0001(16) 0.0008(15) -0.0033(16) C61' 0.020(2) 0.014(2) 0.030(3) 0.0017(18) 0.0149(19) 0.0034(17) C62' 0.021(2) 0.012(2) 0.018(2) -0.0007(16) 0.0004(17) -0.0007(16) C71' 0.031(3) 0.019(2) 0.035(3) 0.007(2) 0.001(2) 0.002(2) C72' 0.021(2) 0.016(2) 0.027(2) 0.0002(18) 0.0041(18) -0.0045(17) N1 0.0163(18) 0.021(2) 0.021(2) 0.0033(16) 0.0010(15) -0.0029(15) N2 0.0210(19) 0.018(2) 0.023(2) -0.0007(16) -0.0017(16) -0.0038(15) N3 0.0170(18) 0.023(2) 0.024(2) 0.0023(16) 0.0045(15) 0.0000(15) N4 0.0145(18) 0.020(2) 0.027(2) -0.0023(16) 0.0045(15) 0.0006(15) N11 0.0165(17) 0.0136(18) 0.0205(19) 0.0030(14) -0.0001(14) -0.0006(14) N12 0.0151(17) 0.0150(18) 0.0157(18) 0.0015(14) -0.0016(14) -0.0002(14) N71 0.027(2) 0.0141(19) 0.022(2) 0.0006(15) -0.0111(16) 0.0010(15) N72 0.0176(18) 0.0171(19) 0.025(2) 0.0015(16) 0.0073(15) 0.0000(15) N11' 0.0205(19) 0.0173(19) 0.0183(19) -0.0007(15) 0.0052(15) -0.0008(15) N12' 0.0201(18) 0.0156(19) 0.0195(19) -0.0016(15) 0.0043(15) -0.0023(14) N71' 0.028(2) 0.0145(19) 0.029(2) -0.0030(16) -0.0123(18) 0.0009(16) N72' 0.024(2) 0.0152(19) 0.027(2) -0.0032(16) 0.0116(17) -0.0029(15) N1N 0.026(2) 0.028(2) 0.035(3) 0.003(2) -0.0106(19) 0.0021(18) N2N 0.024(2) 0.0123(19) 0.036(2) 0.0000(17) 0.0073(18) 0.0027(15) N3N 0.0143(18) 0.022(2) 0.027(2) -0.0003(17) -0.0054(16) 0.0012(15) O81 0.032(2) 0.0170(18) 0.044(2) 0.0003(16) -0.0179(18) 0.0019(15) O82 0.042(2) 0.0179(18) 0.031(2) -0.0035(15) 0.0194(17) -0.0044(16) O1N 0.031(2) 0.036(2) 0.057(3) 0.002(2) 0.002(2) 0.0069(19) O2N 0.027(2) 0.0206(19) 0.054(3) -0.0007(18) -0.0043(18) 0.0011(15) O3N 0.042(2) 0.025(2) 0.034(2) 0.0040(17) -0.0079(18) -0.0029(17) O4N 0.037(2) 0.033(2) 0.039(2) 0.0029(19) 0.0200(18) -0.0007(18) O5N 0.0233(18) 0.028(2) 0.035(2) -0.0005(17) 0.0021(15) -0.0025(15) O6N 0.037(2) 0.034(2) 0.039(2) -0.0017(19) 0.0042(18) -0.0176(18) O7N 0.034(2) 0.024(2) 0.036(2) -0.0071(17) -0.0115(17) 0.0055(16) O8N 0.036(2) 0.0221(19) 0.031(2) -0.0027(15) -0.0172(17) 0.0091(16) O9N 0.0215(18) 0.036(2) 0.0214(18) 0.0018(16) -0.0048(14) 0.0036(15) O1W 0.041(2) 0.022(2) 0.043(2) -0.0023(17) -0.0020(19) -0.0006(17) O2W 0.050(3) 0.037(3) 0.060(3) 0.015(2) 0.002(2) -0.003(2) O3W 0.043(3) 0.050(3) 0.029(2) 0.000(2) 0.0012(19) -0.018(2) Pd1 0.01566(15) 0.01233(15) 0.01444(15) 0.00190(12) -0.00195(11) -0.00079(12) Pd2 0.01493(15) 0.01366(15) 0.01656(16) -0.00147(12) 0.00422(11) -0.00126(12) _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 C21 N11 1.339(6) . ? C21 C31 1.411(6) . ? C21 H21 0.9500 . ? C22 N12 1.341(6) . ? C22 C32 1.383(6) . ? C22 H22 0.9500 . ? C31 C41 1.374(6) . ? C31 N71 1.393(6) . ? C32 C42 1.396(6) . ? C32 N72 1.404(6) . ? C41 C51 1.389(7) . ? C41 H41 0.9500 . ? C42 C52 1.385(7) . ? C42 H42 0.9500 . ? C51 C61 1.396(7) . ? C51 C71 1.501(7) . ? C52 C62 1.395(7) . ? C52 C72 1.501(7) . ? C61 N11 1.343(6) . ? C61 H61 0.9500 . ? C62 N12 1.339(6) . ? C62 H62 0.9500 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C91 O81 1.224(6) . ? C91 N71' 1.362(6) . ? C91 N71 1.388(6) . ? C92 O82 1.220(6) . ? C92 N72 1.369(6) . ? C92 N72' 1.371(6) . ? C102 N3 1.490(7) . ? C102 C103 1.500(7) . ? C102 H10A 0.9900 . ? C102 H10B 0.9900 . ? C103 N4 1.479(6) . ? C103 H10C 0.9900 . ? C103 H10D 0.9900 . ? C112 N1 1.496(6) . ? C112 C113 1.508(7) . ? C113 N2 1.487(6) . ? C113 H11A 0.9900 . ? C113 H11B 0.9900 . ? C21' N11' 1.342(6) . ? C21' C31' 1.377(7) . ? C21' H21' 0.9500 . ? C22' N12' 1.337(6) . ? C22' C32' 1.396(7) . ? C22' H22' 0.9500 . ? C31' C41' 1.396(7) . ? C31' N71' 1.410(6) . ? C32' C42' 1.390(7) . ? C32' N72' 1.399(6) . ? C41' C51' 1.385(7) . ? C41' H41' 0.9500 . ? C42' C52' 1.383(6) . ? C42' H42' 0.9500 . ? C51' C61' 1.388(7) . ? C51' C71' 1.514(7) . ? C52' C62' 1.398(6) . ? C52' C72' 1.509(6) . ? C61' N11' 1.344(6) . ? C61' H61' 0.9500 . ? C62' N12' 1.336(6) . ? C62' H62' 0.9500 . ? C71' H71D 0.9800 . ? C71' H71E 0.9800 . ? C71' H71F 0.9800 . ? C72' H72D 0.9800 . ? C72' H72E 0.9800 . ? C72' H72F 0.9800 . ? N1 Pd1 2.036(4) . ? N1 H11C 0.9200 . ? N1 H11D 0.9200 . ? N2 Pd1 2.034(4) . ? N2 H11E 0.9200 . ? N2 H11F 0.9200 . ? N3 Pd2 2.028(4) . ? N3 H10E 0.9200 . ? N3 H10F 0.9200 . ? N4 Pd2 2.025(4) . ? N4 H10G 0.9200 . ? N4 H10H 0.9200 . ? N11 Pd1 2.036(4) . ? N12 Pd1 2.032(4) . ? N71 H81 0.8800 . ? N72 H82 0.8800 . ? N11' Pd2 2.047(4) . ? N12' Pd2 2.038(4) . ? N71' H81' 0.8800 . ? N72' H82' 0.8800 . ? N1N O1N 1.238(7) . ? N1N O3N 1.256(6) . ? N1N O2N 1.263(6) . ? N2N O4N 1.234(6) . ? N2N O6N 1.251(6) . ? N2N O5N 1.260(6) . ? N3N O7N 1.244(6) . ? N3N O9N 1.246(5) . ? N3N O8N 1.258(5) . ? 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 N11 C21 C31 121.0(4) . . ? N11 C21 H21 119.5 . . ? C31 C21 H21 119.5 . . ? N12 C22 C32 121.3(4) . . ? N12 C22 H22 119.4 . . ? C32 C22 H22 119.4 . . ? C41 C31 N71 120.4(4) . . ? C41 C31 C21 118.3(4) . . ? N71 C31 C21 121.3(4) . . ? C22 C32 C42 118.6(4) . . ? C22 C32 N72 122.8(4) . . ? C42 C32 N72 118.5(4) . . ? C31 C41 C51 121.0(4) . . ? C31 C41 H41 119.5 . . ? C51 C41 H41 119.5 . . ? C52 C42 C32 120.2(4) . . ? C52 C42 H42 119.9 . . ? C32 C42 H42 119.9 . . ? C41 C51 C61 117.4(4) . . ? C41 C51 C71 122.5(5) . . ? C61 C51 C71 120.1(5) . . ? C42 C52 C62 117.6(4) . . ? C42 C52 C72 122.3(5) . . ? C62 C52 C72 120.1(5) . . ? N11 C61 C51 122.3(4) . . ? N11 C61 H61 118.9 . . ? C51 C61 H61 118.9 . . ? N12 C62 C52 122.1(4) . . ? N12 C62 H62 119.0 . . ? C52 C62 H62 119.0 . . ? C51 C71 H71A 109.5 . . ? C51 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C51 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C52 C72 H72A 109.5 . . ? C52 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C52 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? O81 C91 N71' 125.4(5) . . ? O81 C91 N71 122.8(4) . . ? N71' C91 N71 111.8(4) . . ? O82 C92 N72 124.2(5) . . ? O82 C92 N72' 124.4(5) . . ? N72 C92 N72' 111.5(4) . . ? N3 C102 C103 108.7(4) . . ? N3 C102 H10A 110.0 . . ? C103 C102 H10A 110.0 . . ? N3 C102 H10B 110.0 . . ? C103 C102 H10B 110.0 . . ? H10A C102 H10B 108.3 . . ? N4 C103 C102 107.9(4) . . ? N4 C103 H10C 110.1 . . ? C102 C103 H10C 110.1 . . ? N4 C103 H10D 110.1 . . ? C102 C103 H10D 110.1 . . ? H10C C103 H10D 108.4 . . ? N1 C112 C113 107.5(4) . . ? N2 C113 C112 108.1(4) . . ? N2 C113 H11A 110.1 . . ? C112 C113 H11A 110.1 . . ? N2 C113 H11B 110.1 . . ? C112 C113 H11B 110.1 . . ? H11A C113 H11B 108.4 . . ? N11' C21' C31' 120.7(4) . . ? N11' C21' H21' 119.6 . . ? C31' C21' H21' 119.6 . . ? N12' C22' C32' 121.5(4) . . ? N12' C22' H22' 119.2 . . ? C32' C22' H22' 119.2 . . ? C21' C31' C41' 119.8(4) . . ? C21' C31' N71' 123.1(4) . . ? C41' C31' N71' 117.2(4) . . ? C42' C32' C22' 117.9(4) . . ? C42' C32' N72' 120.0(4) . . ? C22' C32' N72' 122.1(4) . . ? C51' C41' C31' 119.5(5) . . ? C51' C41' H41' 120.3 . . ? C31' C41' H41' 120.3 . . ? C52' C42' C32' 120.6(4) . . ? C52' C42' H42' 119.7 . . ? C32' C42' H42' 119.7 . . ? C41' C51' C61' 117.5(5) . . ? C41' C51' C71' 122.4(5) . . ? C61' C51' C71' 120.0(5) . . ? C42' C52' C62' 117.8(4) . . ? C42' C52' C72' 123.0(4) . . ? C62' C52' C72' 119.2(4) . . ? N11' C61' C51' 122.8(5) . . ? N11' C61' H61' 118.6 . . ? C51' C61' H61' 118.6 . . ? N12' C62' C52' 121.7(4) . . ? N12' C62' H62' 119.2 . . ? C52' C62' H62' 119.2 . . ? C51' C71' H71D 109.5 . . ? C51' C71' H71E 109.5 . . ? H71D C71' H71E 109.5 . . ? C51' C71' H71F 109.5 . . ? H71D C71' H71F 109.5 . . ? H71E C71' H71F 109.5 . . ? C52' C72' H72D 109.5 . . ? C52' C72' H72E 109.5 . . ? H72D C72' H72E 109.5 . . ? C52' C72' H72F 109.5 . . ? H72D C72' H72F 109.5 . . ? H72E C72' H72F 109.5 . . ? C112 N1 Pd1 108.1(3) . . ? C112 N1 H11C 110.1 . . ? Pd1 N1 H11C 110.1 . . ? C112 N1 H11D 110.1 . . ? Pd1 N1 H11D 110.1 . . ? H11C N1 H11D 108.4 . . ? C113 N2 Pd1 108.0(3) . . ? C113 N2 H11E 110.1 . . ? Pd1 N2 H11E 110.1 . . ? C113 N2 H11F 110.1 . . ? Pd1 N2 H11F 110.1 . . ? H11E N2 H11F 108.4 . . ? C102 N3 Pd2 109.5(3) . . ? C102 N3 H10E 109.8 . . ? Pd2 N3 H10E 109.8 . . ? C102 N3 H10F 109.8 . . ? Pd2 N3 H10F 109.8 . . ? H10E N3 H10F 108.2 . . ? C103 N4 Pd2 107.8(3) . . ? C103 N4 H10G 110.2 . . ? Pd2 N4 H10G 110.2 . . ? C103 N4 H10H 110.2 . . ? Pd2 N4 H10H 110.2 . . ? H10G N4 H10H 108.5 . . ? C21 N11 C61 120.0(4) . . ? C21 N11 Pd1 118.6(3) . . ? C61 N11 Pd1 121.3(3) . . ? C62 N12 C22 120.2(4) . . ? C62 N12 Pd1 119.1(3) . . ? C22 N12 Pd1 120.6(3) . . ? C91 N71 C31 126.6(4) . . ? C91 N71 H81 116.7 . . ? C31 N71 H81 116.7 . . ? C92 N72 C32 125.4(4) . . ? C92 N72 H82 117.3 . . ? C32 N72 H82 117.3 . . ? C21' N11' C61' 119.7(4) . . ? C21' N11' Pd2 119.9(3) . . ? C61' N11' Pd2 120.4(3) . . ? C62' N12' C22' 120.4(4) . . ? C62' N12' Pd2 122.5(3) . . ? C22' N12' Pd2 117.1(3) . . ? C91 N71' C31' 124.2(4) . . ? C91 N71' H81' 117.9 . . ? C31' N71' H81' 117.9 . . ? C92 N72' C32' 124.6(4) . . ? C92 N72' H82' 117.7 . . ? C32' N72' H82' 117.7 . . ? O1N N1N O3N 119.9(5) . . ? O1N N1N O2N 121.5(5) . . ? O3N N1N O2N 118.5(5) . . ? O4N N2N O6N 121.2(5) . . ? O4N N2N O5N 120.1(5) . . ? O6N N2N O5N 118.7(4) . . ? O7N N3N O9N 120.0(4) . . ? O7N N3N O8N 120.2(4) . . ? O9N N3N O8N 119.8(4) . . ? N12 Pd1 N2 91.45(16) . . ? N12 Pd1 N1 176.02(16) . . ? N2 Pd1 N1 84.63(17) . . ? N12 Pd1 N11 90.99(15) . . ? N2 Pd1 N11 176.53(17) . . ? N1 Pd1 N11 92.95(16) . . ? N4 Pd2 N3 84.22(17) . . ? N4 Pd2 N12' 92.73(16) . . ? N3 Pd2 N12' 176.43(17) . . ? N4 Pd2 N11' 175.54(16) . . ? N3 Pd2 N11' 91.46(17) . . ? N12' Pd2 N11' 91.56(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.05 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.705 _refine_diff_density_min -1.745 _refine_diff_density_rms 0.157 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.124 0.146 0.497 96 42 ' ' 2 0.124 0.354 0.997 94 41 ' ' 3 0.873 0.649 0.004 93 40 ' ' 4 0.873 0.851 0.504 92 39 ' ' _platon_squeeze_details ; ; # Attachment '- Schalley_DT-ART-01-2012-030190_Compound24a.cif' data_24a _database_code_depnum_ccdc_archive 'CCDC 864207' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound24a.cif' _audit_creation_method 'WinGX routine-INITIALISE' _audit_creation_date 2010-03-29T11:04:34-00:00 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION - Compound (??????????????????)# #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C76 H72 N8 O2 P4 Pd2 4+, 4(C F3 S O3 1-)' _chemical_formula_sum 'C80 H72 F12 N8 O14 P4 Pd2 S4' _chemical_formula_weight 2062.38 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.7089(3) _cell_length_b 16.7004(3) _cell_length_c 34.7739(6) _cell_angle_alpha 85.1940(10) _cell_angle_beta 82.8360(10) _cell_angle_gamma 88.7500(10) _cell_volume 9019.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123.0(1) _cell_measurement_reflns_used 26677 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.103 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4176 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5891 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ; Sheldrick, G. M. SADABS 2008/2; University of G\"ottingen: G\"ottingen, Germany, 2008. ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 123.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Bruker-Nonius Kappa Apex II Diffractometer' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.222835E-1 _diffrn_orient_matrix_UB_12 -0.92149E-2 _diffrn_orient_matrix_UB_13 0.257383E-1 _diffrn_orient_matrix_UB_21 -0.590767E-1 _diffrn_orient_matrix_UB_22 -0.138772E-1 _diffrn_orient_matrix_UB_23 0.126988E-1 _diffrn_orient_matrix_UB_31 0.114108E-1 _diffrn_orient_matrix_UB_32 -0.577384E-1 _diffrn_orient_matrix_UB_33 -0.46865E-2 _diffrn_reflns_number 75806 _diffrn_reflns_av_R_equivalents 0.0543 _diffrn_reflns_av_sigmaI/netI 0.0920 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 0.59 _diffrn_reflns_theta_max 25.00 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 31694 _reflns_number_gt 19752 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. Although data were collected at 123 K, the phenyl ring atoms C117, C139, 140, C141 and C199 have high anisotropic thermal parameters (due to disorder). ISOR restraint was therefore used in their refinement. The same case is with triflate atoms O11, O21, O31, F11, C11, O32, C13, O13, O23, F23, F33, O24, S17, C17, O17, O27, O37, F27, S18, O28, O38, F18, F28 and C18 (due to disorder These restraints were used in order to avoid Alerts in CHECKCIF. As bond length and angles were not in accord with expected for triflates DFIX command in SHELXL was used for S -- O, S -- C, C --F, O -- O, F -- F and O -- F distances in triflates #1, 3, 7 and 8. In addition, the same command was used for one S -- O distance in triflates #4 and 7. ; _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^)+(0.2088P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31694 _refine_ls_number_parameters 2233 _refine_ls_number_restraints 269 _refine_ls_R_factor_all 0.1532 _refine_ls_R_factor_gt 0.1103 _refine_ls_wR_factor_ref 0.3438 _refine_ls_wR_factor_gt 0.3137 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.208 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 4.215 _refine_diff_density_min -2.411 _refine_diff_density_rms 0.199 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pd1 Pd 0.61714(4) 0.32362(4) 0.630490(19) 0.0316(2) Uani 1 1 d . . . Pd2 Pd 0.63586(6) 0.29557(5) 0.88342(2) 0.0521(3) Uani 1 1 d . . . P1 P 0.62667(15) 0.18917(14) 0.62405(7) 0.0327(5) Uani 1 1 d . . . P2 P 0.47256(15) 0.32122(15) 0.62862(7) 0.0355(5) Uani 1 1 d . . . P3 P 0.6465(2) 0.15960(18) 0.89349(8) 0.0572(8) Uani 1 1 d . . . P4 P 0.4931(2) 0.28910(18) 0.90289(8) 0.0570(8) Uani 1 1 d . . . N11 N 0.7504(5) 0.3284(5) 0.6325(2) 0.0354(17) Uani 1 1 d . . . N71 N 0.9016(5) 0.3016(5) 0.7044(2) 0.0400(19) Uani 1 1 d . . . H71 H 0.9554 0.2854 0.7035 0.048 Uiso 1 1 calc R . . N11' N 0.7658(6) 0.3040(5) 0.8632(2) 0.052(2) Uani 1 1 d . . . N71' N 0.9060(5) 0.2972(5) 0.7701(2) 0.049(2) Uani 1 1 d . . . H71' H 0.9600 0.2831 0.7641 0.059 Uiso 1 1 calc R . . O81 O 0.7812(4) 0.3315(5) 0.74498(19) 0.0509(18) Uani 1 1 d . . . C21 C 0.7792(6) 0.3150(5) 0.6663(2) 0.0313(19) Uani 1 1 d . . . H21 H 0.7398 0.3042 0.6891 0.038 Uiso 1 1 calc R . . C31 C 0.8666(5) 0.3162(5) 0.6692(2) 0.034(2) Uani 1 1 d . . . C41 C 0.9250(6) 0.3313(6) 0.6347(3) 0.046(3) Uani 1 1 d . . . H41 H 0.9852 0.3326 0.6355 0.056 Uiso 1 1 calc R . . C51 C 0.8907(7) 0.3441(7) 0.6001(3) 0.055(3) Uani 1 1 d . . . H51 H 0.9281 0.3530 0.5765 0.066 Uiso 1 1 calc R . . C61 C 0.8052(6) 0.3442(6) 0.5989(3) 0.038(2) Uani 1 1 d . . . H61 H 0.7829 0.3552 0.5748 0.046 Uiso 1 1 calc R . . C81 C 0.8567(6) 0.3113(6) 0.7401(3) 0.040(2) Uani 1 1 d . . . C21' C 0.7922(7) 0.3022(7) 0.8253(3) 0.054(3) Uani 1 1 d . . . H21' H 0.7498 0.3000 0.8082 0.065 Uiso 1 1 calc R . . C31' C 0.8770(7) 0.3035(7) 0.8094(3) 0.054(3) Uani 1 1 d . . . C41' C 0.9385(8) 0.3010(7) 0.8352(3) 0.059(3) Uani 1 1 d . . . H41' H 0.9976 0.2956 0.8258 0.071 Uiso 1 1 calc R . . C51' C 0.9134(9) 0.3064(7) 0.8744(3) 0.061(3) Uani 1 1 d . . . H51' H 0.9546 0.3090 0.8921 0.074 Uiso 1 1 calc R . . C61' C 0.8265(9) 0.3078(7) 0.8872(3) 0.063(3) Uani 1 1 d . . . H61' H 0.8088 0.3116 0.9142 0.076 Uiso 1 1 calc R . . N12 N 0.6162(4) 0.4469(4) 0.6384(2) 0.0303(16) Uani 1 1 d . . . N72 N 0.6018(5) 0.5732(5) 0.7207(2) 0.046(2) Uani 1 1 d . . . H72 H 0.5970 0.6252 0.7232 0.055 Uiso 1 1 calc R . . N12' N 0.6302(7) 0.4215(5) 0.8709(3) 0.062(3) Uani 1 1 d . . . N72' N 0.6120(7) 0.5645(5) 0.7858(2) 0.063(3) Uani 1 1 d . . . H72' H 0.6150 0.6171 0.7817 0.076 Uiso 1 1 calc R . . O82 O 0.5969(5) 0.4525(4) 0.7555(2) 0.060(2) Uani 1 1 d . . . C22 C 0.6072(6) 0.4677(5) 0.6748(3) 0.041(2) Uani 1 1 d . . . H22 H 0.5997 0.4270 0.6957 0.050 Uiso 1 1 calc R . . C32 C 0.6086(5) 0.5488(5) 0.6830(3) 0.036(2) Uani 1 1 d . . . C42 C 0.6249(6) 0.6077(6) 0.6519(3) 0.044(2) Uani 1 1 d . . . H42 H 0.6292 0.6627 0.6565 0.053 Uiso 1 1 calc R . . C52 C 0.6345(6) 0.5840(6) 0.6143(3) 0.047(2) Uani 1 1 d . . . H52 H 0.6449 0.6226 0.5926 0.056 Uiso 1 1 calc R . . C62 C 0.6288(6) 0.5031(6) 0.6089(3) 0.043(2) Uani 1 1 d . . . H62 H 0.6341 0.4872 0.5831 0.051 Uiso 1 1 calc R . . C82 C 0.6018(7) 0.5237(6) 0.7540(3) 0.047(2) Uani 1 1 d . . . C22' C 0.6208(8) 0.4501(6) 0.8342(3) 0.057(3) Uani 1 1 d . . . H22' H 0.6159 0.4132 0.8152 0.069 Uiso 1 1 calc R . . C32' C 0.6179(8) 0.5334(6) 0.8231(3) 0.060(3) Uani 1 1 d . . . C42' C 0.6265(8) 0.5849(7) 0.8527(3) 0.061(3) Uani 1 1 d . . . H42' H 0.6228 0.6415 0.8474 0.074 Uiso 1 1 calc R . . C52' C 0.6401(8) 0.5529(7) 0.8885(3) 0.063(3) Uani 1 1 d . . . H52' H 0.6482 0.5875 0.9080 0.075 Uiso 1 1 calc R . . C62' C 0.6422(7) 0.4726(7) 0.8968(3) 0.055(3) Uani 1 1 d . . . H62' H 0.6526 0.4521 0.9222 0.067 Uiso 1 1 calc R . . C100 C 0.5416(6) 0.1288(5) 0.6516(3) 0.042(2) Uani 1 1 d . . . H10A H 0.5527 0.0717 0.6467 0.050 Uiso 1 1 calc R . . H10B H 0.5432 0.1338 0.6796 0.050 Uiso 1 1 calc R . . C101 C 0.4516(6) 0.1525(6) 0.6416(3) 0.046(2) Uani 1 1 d . . . H10C H 0.4519 0.1525 0.6131 0.055 Uiso 1 1 calc R . . H10D H 0.4109 0.1108 0.6540 0.055 Uiso 1 1 calc R . . C102 C 0.4183(6) 0.2344(5) 0.6540(3) 0.047(2) Uani 1 1 d . . . H10E H 0.4225 0.2357 0.6821 0.056 Uiso 1 1 calc R . . H10F H 0.3568 0.2390 0.6506 0.056 Uiso 1 1 calc R . . C103 C 0.7232(6) 0.1461(5) 0.6411(3) 0.036(2) Uani 1 1 d . . . C104 C 0.7266(7) 0.1258(6) 0.6799(3) 0.045(2) Uani 1 1 d . . . H104 H 0.6762 0.1277 0.6981 0.054 Uiso 1 1 calc R . . C105 C 0.8075(8) 0.1016(7) 0.6928(3) 0.060(3) Uani 1 1 d . . . H105 H 0.8100 0.0851 0.7194 0.072 Uiso 1 1 calc R . . C106 C 0.8806(8) 0.1021(6) 0.6671(4) 0.059(3) Uani 1 1 d . . . H106 H 0.9343 0.0890 0.6761 0.070 Uiso 1 1 calc R . . C107 C 0.8761(7) 0.1217(7) 0.6284(3) 0.056(3) Uani 1 1 d . . . H107 H 0.9268 0.1203 0.6104 0.067 Uiso 1 1 calc R . . C108 C 0.7976(6) 0.1438(6) 0.6149(3) 0.048(3) Uani 1 1 d . . . H108 H 0.7953 0.1571 0.5879 0.057 Uiso 1 1 calc R . . C109 C 0.6273(6) 0.1660(5) 0.5744(3) 0.037(2) Uani 1 1 d . . . C110 C 0.6129(7) 0.0901(7) 0.5650(3) 0.051(3) Uani 1 1 d . . . H110 H 0.6067 0.0470 0.5848 0.061 Uiso 1 1 calc R . . C111 C 0.6072(8) 0.0754(8) 0.5260(3) 0.065(3) Uani 1 1 d . . . H111 H 0.5968 0.0227 0.5194 0.078 Uiso 1 1 calc R . . C112 C 0.6171(8) 0.1392(9) 0.4974(3) 0.067(3) Uani 1 1 d . . . H112 H 0.6134 0.1303 0.4710 0.080 Uiso 1 1 calc R . . C113 C 0.6315(8) 0.2114(8) 0.5069(3) 0.061(3) Uani 1 1 d . . . H113 H 0.6368 0.2543 0.4871 0.074 Uiso 1 1 calc R . . C114 C 0.6395(6) 0.2281(6) 0.5452(3) 0.044(2) Uani 1 1 d . . . H114 H 0.6529 0.2806 0.5510 0.053 Uiso 1 1 calc R . . C115 C 0.4469(6) 0.3311(6) 0.5785(3) 0.048(3) Uani 1 1 d . . . C116 C 0.3733(9) 0.2966(10) 0.5698(4) 0.094(5) Uani 1 1 d . . . H116 H 0.3385 0.2646 0.5893 0.113 Uiso 1 1 calc R . . C117 C 0.3510(10) 0.3085(11) 0.5334(5) 0.100(5) Uani 1 1 d U . . H117 H 0.2985 0.2878 0.5277 0.120 Uiso 1 1 calc R . . C118 C 0.4057(10) 0.3519(10) 0.5036(4) 0.093(5) Uani 1 1 d . . . H118 H 0.3925 0.3571 0.4776 0.112 Uiso 1 1 calc R . . C119 C 0.4771(7) 0.3858(7) 0.5131(4) 0.060(3) Uani 1 1 d . . . H119 H 0.5140 0.4170 0.4941 0.072 Uiso 1 1 calc R . . C120 C 0.4947(6) 0.3738(6) 0.5511(3) 0.042(2) Uani 1 1 d . . . H120 H 0.5445 0.3980 0.5577 0.050 Uiso 1 1 calc R . . C121 C 0.4155(6) 0.4019(6) 0.6536(3) 0.041(2) Uani 1 1 d . . . C122 C 0.3650(6) 0.4586(6) 0.6331(3) 0.046(2) Uani 1 1 d . . . H122 H 0.3630 0.4573 0.6059 0.056 Uiso 1 1 calc R . . C123 C 0.3187(6) 0.5161(7) 0.6542(4) 0.053(3) Uani 1 1 d . . . H123 H 0.2845 0.5544 0.6411 0.064 Uiso 1 1 calc R . . C124 C 0.3214(7) 0.5189(6) 0.6934(3) 0.055(3) Uani 1 1 d . . . H124 H 0.2891 0.5585 0.7072 0.066 Uiso 1 1 calc R . . C125 C 0.3710(8) 0.4639(7) 0.7126(4) 0.064(3) Uani 1 1 d . . . H125 H 0.3741 0.4661 0.7396 0.077 Uiso 1 1 calc R . . C126 C 0.4175(7) 0.4040(6) 0.6919(3) 0.046(2) Uani 1 1 d . . . H126 H 0.4504 0.3650 0.7054 0.055 Uiso 1 1 calc R . . C127 C 0.5641(7) 0.1072(7) 0.8738(3) 0.059(3) Uani 1 1 d . . . H12A H 0.5638 0.1261 0.8461 0.070 Uiso 1 1 calc R . . H12B H 0.5778 0.0489 0.8752 0.070 Uiso 1 1 calc R . . C128 C 0.4711(9) 0.1210(7) 0.8966(4) 0.082(5) Uani 1 1 d . . . H12C H 0.4312 0.0805 0.8902 0.099 Uiso 1 1 calc R . . H12D H 0.4740 0.1142 0.9250 0.099 Uiso 1 1 calc R . . C129 C 0.4364(8) 0.2076(7) 0.8853(4) 0.063(3) Uani 1 1 d . . . H12E H 0.3750 0.2110 0.8958 0.075 Uiso 1 1 calc R . . H12F H 0.4403 0.2158 0.8566 0.075 Uiso 1 1 calc R . . C130 C 0.7469(9) 0.1241(8) 0.8685(3) 0.070(4) Uani 1 1 d . . . C131 C 0.8226(9) 0.1144(7) 0.8880(4) 0.069(4) Uani 1 1 d . . . H131 H 0.8189 0.1226 0.9149 0.082 Uiso 1 1 calc R . . C132 C 0.8985(10) 0.0938(8) 0.8687(4) 0.078(4) Uani 1 1 d . . . H132 H 0.9477 0.0879 0.8821 0.093 Uiso 1 1 calc R . . C133 C 0.9053(9) 0.0817(9) 0.8315(4) 0.080(4) Uani 1 1 d . . . H133 H 0.9597 0.0693 0.8180 0.096 Uiso 1 1 calc R . . C134 C 0.8347(11) 0.0869(11) 0.8121(4) 0.104(6) Uani 1 1 d . . . H134 H 0.8412 0.0745 0.7857 0.125 Uiso 1 1 calc R . . C135 C 0.7534(9) 0.1095(10) 0.8290(4) 0.091(5) Uani 1 1 d . . . H135 H 0.7056 0.1148 0.8147 0.110 Uiso 1 1 calc R . . C136 C 0.6428(11) 0.1204(8) 0.9436(3) 0.081(4) Uani 1 1 d . . . C137 C 0.6513(9) 0.1745(8) 0.9722(3) 0.071(4) Uani 1 1 d . . . H137 H 0.6602 0.2301 0.9650 0.085 Uiso 1 1 calc R . . C138 C 0.6463(11) 0.1439(8) 1.0116(4) 0.092(5) Uani 1 1 d . . . H138 H 0.6529 0.1795 1.0309 0.111 Uiso 1 1 calc R . . C139 C 0.6316(11) 0.0616(10) 1.0227(5) 0.099(5) Uani 1 1 d U . . H139 H 0.6275 0.0415 1.0492 0.119 Uiso 1 1 calc R . . C140 C 0.6232(11) 0.0099(10) 0.9930(4) 0.097(5) Uani 1 1 d U . . H140 H 0.6145 -0.0458 0.9999 0.117 Uiso 1 1 calc R . . C141 C 0.6273(10) 0.0388(9) 0.9530(4) 0.087(4) Uani 1 1 d U . . H141 H 0.6199 0.0037 0.9335 0.105 Uiso 1 1 calc R . . C142 C 0.4662(8) 0.2842(7) 0.9548(3) 0.061(3) Uani 1 1 d . . . C143 C 0.5128(10) 0.3258(8) 0.9759(4) 0.077(4) Uani 1 1 d . . . H143 H 0.5598 0.3569 0.9635 0.092 Uiso 1 1 calc R . . C144 C 0.4917(10) 0.3235(9) 1.0176(4) 0.084(4) Uani 1 1 d . . . H144 H 0.5237 0.3545 1.0323 0.101 Uiso 1 1 calc R . . C145 C 0.4303(11) 0.2800(12) 1.0349(4) 0.095(5) Uani 1 1 d . . . H145 H 0.4193 0.2766 1.0625 0.114 Uiso 1 1 calc R . . C146 C 0.3792(11) 0.2374(10) 1.0137(4) 0.099(5) Uani 1 1 d . . . H146 H 0.3314 0.2081 1.0268 0.119 Uiso 1 1 calc R . . C147 C 0.3974(10) 0.2379(9) 0.9751(4) 0.087(5) Uani 1 1 d . . . H147 H 0.3639 0.2069 0.9610 0.105 Uiso 1 1 calc R . . C148 C 0.4380(7) 0.3778(7) 0.8833(3) 0.055(3) Uani 1 1 d . . . C149 C 0.4223(10) 0.3858(8) 0.8450(3) 0.079(4) Uani 1 1 d . . . H149 H 0.4388 0.3436 0.8288 0.095 Uiso 1 1 calc R . . C150 C 0.3837(10) 0.4529(10) 0.8298(4) 0.088(5) Uani 1 1 d . . . H150 H 0.3743 0.4564 0.8033 0.106 Uiso 1 1 calc R . . C151 C 0.3575(9) 0.5165(8) 0.8521(4) 0.072(4) Uani 1 1 d . . . H151 H 0.3300 0.5632 0.8417 0.086 Uiso 1 1 calc R . . C152 C 0.3741(9) 0.5071(8) 0.8904(3) 0.075(4) Uani 1 1 d . . . H152 H 0.3600 0.5503 0.9062 0.090 Uiso 1 1 calc R . . C153 C 0.4099(8) 0.4389(7) 0.9067(4) 0.063(3) Uani 1 1 d . . . H153 H 0.4154 0.4336 0.9337 0.076 Uiso 1 1 calc R . . Pd3 Pd 0.10056(4) 0.72964(4) 0.62569(2) 0.0350(2) Uani 1 1 d . . . Pd4 Pd 0.13073(6) 0.72045(6) 0.87733(2) 0.0585(3) Uani 1 1 d . . . P5 P -0.04280(15) 0.73639(15) 0.62342(8) 0.0431(6) Uani 1 1 d . . . P6 P 0.11024(15) 0.86501(15) 0.61169(8) 0.0378(6) Uani 1 1 d . . . P7 P -0.0130(2) 0.7226(2) 0.89569(9) 0.0662(9) Uani 1 1 d . . . P8 P 0.1342(2) 0.8552(2) 0.88207(9) 0.0607(8) Uani 1 1 d . . . N13 N 0.0975(5) 0.6047(5) 0.6403(2) 0.0405(19) Uani 1 1 d . . . N73 N 0.0927(6) 0.4676(5) 0.7290(3) 0.057(2) Uani 1 1 d . . . H73 H 0.0875 0.4152 0.7337 0.069 Uiso 1 1 calc R . . N13' N 0.1316(7) 0.5973(6) 0.8705(3) 0.060(3) Uani 1 1 d . . . N73' N 0.1070(7) 0.4642(5) 0.7934(3) 0.065(3) Uani 1 1 d . . . H73' H 0.1060 0.4118 0.7922 0.078 Uiso 1 1 calc R . . O83 O 0.0894(6) 0.5829(4) 0.7581(2) 0.067(2) Uani 1 1 d . . . C23 C 0.0910(6) 0.5773(5) 0.6778(3) 0.044(2) Uani 1 1 d . . . H23 H 0.0818 0.6152 0.6968 0.053 Uiso 1 1 calc R . . C33 C 0.0968(7) 0.4978(6) 0.6903(3) 0.048(3) Uani 1 1 d . . . C43 C 0.1088(7) 0.4433(7) 0.6611(3) 0.052(3) Uani 1 1 d . . . H43 H 0.1118 0.3871 0.6677 0.063 Uiso 1 1 calc R . . C53 C 0.1157(7) 0.4727(6) 0.6236(3) 0.050(3) Uani 1 1 d . . . H53 H 0.1242 0.4365 0.6037 0.060 Uiso 1 1 calc R . . C63 C 0.1108(6) 0.5541(6) 0.6134(3) 0.046(2) Uani 1 1 d . . . H63 H 0.1170 0.5735 0.5867 0.056 Uiso 1 1 calc R . . C83 C 0.0958(8) 0.5108(7) 0.7601(4) 0.062(3) Uani 1 1 d . . . C23' C 0.1199(8) 0.5744(7) 0.8362(3) 0.061(3) Uani 1 1 d . . . H23' H 0.1112 0.6137 0.8157 0.073 Uiso 1 1 calc R . . C33' C 0.1200(8) 0.4917(7) 0.8297(3) 0.063(3) Uani 1 1 d . . . C43' C 0.1321(9) 0.4374(8) 0.8595(4) 0.072(4) Uani 1 1 d . . . H43' H 0.1323 0.3817 0.8557 0.086 Uiso 1 1 calc R . . C53' C 0.1440(9) 0.4616(8) 0.8954(4) 0.072(4) Uani 1 1 d . . . H53' H 0.1514 0.4226 0.9163 0.086 Uiso 1 1 calc R . . C63' C 0.1453(8) 0.5388(10) 0.9008(4) 0.079(4) Uani 1 1 d . . . H63' H 0.1556 0.5551 0.9254 0.095 Uiso 1 1 calc R . . N14 N 0.2338(4) 0.7184(5) 0.6269(2) 0.0332(17) Uani 1 1 d . . . N74 N 0.3905(5) 0.7313(5) 0.6963(2) 0.0402(19) Uani 1 1 d . . . H74 H 0.4446 0.7454 0.6943 0.048 Uiso 1 1 calc R . . N14' N 0.2630(6) 0.7171(5) 0.8559(2) 0.052(2) Uani 1 1 d . . . N74' N 0.3980(5) 0.7346(5) 0.7614(2) 0.043(2) Uani 1 1 d . . . H74' H 0.4512 0.7497 0.7539 0.052 Uiso 1 1 calc R . . O84 O 0.2721(4) 0.7004(5) 0.73980(19) 0.0537(19) Uani 1 1 d . . . C24 C 0.2664(6) 0.7259(5) 0.6598(3) 0.036(2) Uani 1 1 d . . . H24 H 0.2288 0.7349 0.6827 0.043 Uiso 1 1 calc R . . C34 C 0.3546(6) 0.7209(6) 0.6616(3) 0.038(2) Uani 1 1 d . . . C44 C 0.4081(6) 0.7053(6) 0.6286(3) 0.037(2) Uani 1 1 d . . . H44 H 0.4685 0.7015 0.6290 0.044 Uiso 1 1 calc R . . C54 C 0.3728(6) 0.6954(6) 0.5951(3) 0.041(2) Uani 1 1 d . . . H54 H 0.4089 0.6832 0.5723 0.049 Uiso 1 1 calc R . . C64 C 0.2871(6) 0.7028(6) 0.5943(3) 0.040(2) Uani 1 1 d . . . H64 H 0.2638 0.6970 0.5707 0.048 Uiso 1 1 calc R . . C84 C 0.3457(6) 0.7206(6) 0.7327(3) 0.044(2) Uani 1 1 d . . . C24' C 0.2841(7) 0.7256(6) 0.8173(3) 0.047(2) Uani 1 1 d . . . H24' H 0.2406 0.7315 0.8006 0.056 Uiso 1 1 calc R . . C34' C 0.3695(7) 0.7259(6) 0.8019(3) 0.046(2) Uani 1 1 d . . . C44' C 0.4309(7) 0.7218(7) 0.8273(3) 0.052(3) Uani 1 1 d . . . H44' H 0.4899 0.7239 0.8172 0.062 Uiso 1 1 calc R . . C54' C 0.4080(10) 0.7148(8) 0.8659(3) 0.070(4) Uani 1 1 d . . . H54' H 0.4509 0.7113 0.8830 0.083 Uiso 1 1 calc R . . C64' C 0.3222(8) 0.7129(7) 0.8808(3) 0.061(3) Uani 1 1 d . . . H64' H 0.3054 0.7086 0.9081 0.073 Uiso 1 1 calc R . . C154 C -0.0965(6) 0.8216(6) 0.6452(3) 0.048(3) Uani 1 1 d . . . H15A H -0.1590 0.8175 0.6441 0.057 Uiso 1 1 calc R . . H15B H -0.0873 0.8191 0.6729 0.057 Uiso 1 1 calc R . . C155 C -0.0657(6) 0.9037(7) 0.6253(4) 0.055(3) Uani 1 1 d . . . H15C H -0.0641 0.9028 0.5968 0.066 Uiso 1 1 calc R . . H15D H -0.1070 0.9461 0.6339 0.066 Uiso 1 1 calc R . . C156 C 0.0247(6) 0.9243(6) 0.6350(3) 0.044(2) Uani 1 1 d . . . H15E H 0.0252 0.9163 0.6635 0.053 Uiso 1 1 calc R . . H15F H 0.0359 0.9818 0.6270 0.053 Uiso 1 1 calc R . . C157 C -0.0988(6) 0.6519(6) 0.6505(3) 0.043(2) Uani 1 1 d . . . C158 C -0.1109(8) 0.6471(7) 0.6911(3) 0.062(3) Uani 1 1 d . . . H158 H -0.0910 0.6886 0.7047 0.074 Uiso 1 1 calc R . . C159 C -0.1522(8) 0.5813(8) 0.7113(4) 0.067(3) Uani 1 1 d . . . H159 H -0.1623 0.5796 0.7388 0.080 Uiso 1 1 calc R . . C160 C -0.1790(6) 0.5185(6) 0.6931(3) 0.050(3) Uani 1 1 d . . . H160 H -0.2052 0.4728 0.7076 0.060 Uiso 1 1 calc R . . C161 C -0.1670(7) 0.5239(7) 0.6538(4) 0.057(3) Uani 1 1 d . . . H161 H -0.1865 0.4814 0.6407 0.068 Uiso 1 1 calc R . . C162 C -0.1272(6) 0.5893(6) 0.6319(3) 0.047(2) Uani 1 1 d . . . H162 H -0.1195 0.5910 0.6043 0.056 Uiso 1 1 calc R . . C163 C -0.0676(6) 0.7382(6) 0.5745(3) 0.043(2) Uani 1 1 d . . . C164 C -0.1434(7) 0.7702(7) 0.5620(4) 0.064(3) Uani 1 1 d . . . H164 H -0.1851 0.7918 0.5806 0.076 Uiso 1 1 calc R . . C165 C -0.1607(8) 0.7723(8) 0.5241(4) 0.075(4) Uani 1 1 d . . . H165 H -0.2109 0.7989 0.5166 0.090 Uiso 1 1 calc R . . C166 C -0.1053(7) 0.7358(8) 0.4974(4) 0.064(3) Uani 1 1 d . . . H166 H -0.1178 0.7358 0.4713 0.077 Uiso 1 1 calc R . . C167 C -0.0311(7) 0.6989(8) 0.5080(3) 0.063(3) Uani 1 1 d . . . H167 H 0.0077 0.6741 0.4893 0.076 Uiso 1 1 calc R . . C168 C -0.0128(7) 0.6982(7) 0.5471(3) 0.057(3) Uani 1 1 d . . . H168 H 0.0366 0.6705 0.5547 0.068 Uiso 1 1 calc R . . C169 C 0.1178(6) 0.8968(6) 0.5601(3) 0.045(2) Uani 1 1 d . . . C170 C 0.1368(7) 0.8386(8) 0.5325(3) 0.058(3) Uani 1 1 d . . . H170 H 0.1441 0.7837 0.5411 0.070 Uiso 1 1 calc R . . C171 C 0.1444(8) 0.8612(8) 0.4943(3) 0.065(3) Uani 1 1 d . . . H171 H 0.1580 0.8215 0.4764 0.078 Uiso 1 1 calc R . . C172 C 0.1336(9) 0.9373(10) 0.4803(4) 0.088(5) Uani 1 1 d . . . H172 H 0.1389 0.9512 0.4530 0.105 Uiso 1 1 calc R . . C173 C 0.1140(10) 0.9967(9) 0.5070(5) 0.097(5) Uani 1 1 d . . . H173 H 0.1063 1.0511 0.4977 0.116 Uiso 1 1 calc R . . C174 C 0.1062(10) 0.9758(8) 0.5461(4) 0.083(4) Uani 1 1 d . . . H174 H 0.0928 1.0159 0.5639 0.100 Uiso 1 1 calc R . . C175 C 0.2059(7) 0.9029(6) 0.6281(3) 0.049(3) Uani 1 1 d . . . C176 C 0.2774(7) 0.9247(6) 0.6015(4) 0.060(3) Uani 1 1 d . . . H176 H 0.2746 0.9256 0.5743 0.071 Uiso 1 1 calc R . . C177 C 0.3515(8) 0.9449(7) 0.6150(5) 0.069(4) Uani 1 1 d . . . H177 H 0.4002 0.9595 0.5969 0.083 Uiso 1 1 calc R . . C178 C 0.3569(8) 0.9446(7) 0.6541(6) 0.080(5) Uani 1 1 d . . . H178 H 0.4093 0.9577 0.6629 0.096 Uiso 1 1 calc R . . C179 C 0.2874(9) 0.9255(7) 0.6799(4) 0.071(4) Uani 1 1 d . . . H179 H 0.2911 0.9263 0.7069 0.086 Uiso 1 1 calc R . . C180 C 0.2096(8) 0.9043(7) 0.6674(4) 0.062(3) Uani 1 1 d . . . H180 H 0.1608 0.8914 0.6856 0.075 Uiso 1 1 calc R . . C181 C -0.0696(9) 0.8067(8) 0.8741(4) 0.077(4) Uani 1 1 d . . . H18A H -0.0641 0.8026 0.8457 0.092 Uiso 1 1 calc R . . H18B H -0.1312 0.8022 0.8841 0.092 Uiso 1 1 calc R . . C182 C -0.0396(8) 0.8899(7) 0.8814(4) 0.067(3) Uani 1 1 d . . . H18C H -0.0389 0.8926 0.9096 0.081 Uiso 1 1 calc R . . H18D H -0.0814 0.9307 0.8727 0.081 Uiso 1 1 calc R . . C183 C 0.0502(8) 0.9109(8) 0.8602(3) 0.068(3) Uani 1 1 d . . . H18E H 0.0598 0.9691 0.8607 0.081 Uiso 1 1 calc R . . H18F H 0.0528 0.8989 0.8326 0.081 Uiso 1 1 calc R . . C184 C -0.0637(8) 0.6377(7) 0.8796(3) 0.063(3) Uani 1 1 d . . . C185 C -0.0934(8) 0.5721(9) 0.9045(3) 0.072(4) Uani 1 1 d . . . H185 H -0.0893 0.5718 0.9315 0.087 Uiso 1 1 calc R . . C186 C -0.1282(10) 0.5082(8) 0.8906(4) 0.080(4) Uani 1 1 d . . . H186 H -0.1455 0.4626 0.9078 0.096 Uiso 1 1 calc R . . C187 C -0.1383(9) 0.5090(8) 0.8533(4) 0.076(4) Uani 1 1 d . . . H187 H -0.1668 0.4658 0.8444 0.091 Uiso 1 1 calc R . . C188 C -0.1082(9) 0.5712(9) 0.8273(4) 0.074(4) Uani 1 1 d . . . H188 H -0.1115 0.5692 0.8003 0.089 Uiso 1 1 calc R . . C189 C -0.0735(9) 0.6362(8) 0.8407(4) 0.074(4) Uani 1 1 d . . . H189 H -0.0558 0.6810 0.8231 0.089 Uiso 1 1 calc R . . C190 C -0.0421(8) 0.7209(9) 0.9478(4) 0.071(4) Uani 1 1 d . . . C191 C 0.0013(10) 0.6739(11) 0.9738(5) 0.101(5) Uani 1 1 d . . . H191 H 0.0476 0.6411 0.9637 0.121 Uiso 1 1 calc R . . C192 C -0.0185(12) 0.6724(11) 1.0124(4) 0.098(5) Uani 1 1 d . . . H192 H 0.0152 0.6412 1.0291 0.118 Uiso 1 1 calc R . . C193 C -0.0840(13) 0.7136(14) 1.0271(5) 0.115(7) Uani 1 1 d . . . H193 H -0.0990 0.7114 1.0544 0.138 Uiso 1 1 calc R . . C194 C -0.1310(13) 0.7601(12) 1.0032(5) 0.116(7) Uani 1 1 d . . . H194 H -0.1784 0.7902 1.0144 0.140 Uiso 1 1 calc R . . C195 C -0.1121(12) 0.7648(9) 0.9633(4) 0.100(5) Uani 1 1 d . . . H195 H -0.1458 0.7971 0.9470 0.120 Uiso 1 1 calc R . . C196 C 0.1272(8) 0.8836(9) 0.9319(3) 0.067(3) Uani 1 1 d . . . C197 C 0.1422(9) 0.8245(10) 0.9615(4) 0.082(4) Uani 1 1 d . . . H197 H 0.1606 0.7718 0.9557 0.098 Uiso 1 1 calc R . . C198 C 0.1286(10) 0.8468(12) 1.0010(5) 0.102(5) Uani 1 1 d . . . H198 H 0.1310 0.8077 1.0223 0.122 Uiso 1 1 calc R . . C199 C 0.1118(11) 0.9272(11) 1.0070(5) 0.097(5) Uani 1 1 d U . . H199 H 0.1029 0.9431 1.0328 0.116 Uiso 1 1 calc R . . C200 C 0.1080(11) 0.9816(9) 0.9778(5) 0.093(5) Uani 1 1 d . . . H200 H 0.1010 1.0366 0.9828 0.111 Uiso 1 1 calc R . . C201 C 0.1141(9) 0.9604(9) 0.9393(4) 0.082(4) Uani 1 1 d . . . H201 H 0.1089 1.0005 0.9186 0.098 Uiso 1 1 calc R . . C202 C 0.2344(8) 0.8982(7) 0.8565(3) 0.063(3) Uani 1 1 d . . . C203 C 0.2404(10) 0.9194(8) 0.8171(4) 0.079(4) Uani 1 1 d . . . H203 H 0.1927 0.9152 0.8031 0.095 Uiso 1 1 calc R . . C204 C 0.3209(11) 0.9476(9) 0.7984(5) 0.089(5) Uani 1 1 d . . . H204 H 0.3269 0.9648 0.7714 0.107 Uiso 1 1 calc R . . C205 C 0.3897(11) 0.9506(8) 0.8184(5) 0.084(5) Uani 1 1 d . . . H205 H 0.4449 0.9650 0.8056 0.101 Uiso 1 1 calc R . . C206 C 0.3765(11) 0.9326(9) 0.8565(5) 0.091(5) Uani 1 1 d . . . H206 H 0.4230 0.9402 0.8708 0.109 Uiso 1 1 calc R . . C207 C 0.3026(8) 0.9041(7) 0.8768(4) 0.067(3) Uani 1 1 d . . . H207 H 0.2984 0.8890 0.9039 0.080 Uiso 1 1 calc R . . S11 S 0.7601(3) 0.4054(2) 0.99848(10) 0.1027(14) Uani 1 1 d D . . O11 O 0.7240(5) 0.3721(4) 0.96707(17) 0.116(4) Uani 1 1 d DU . . O21 O 0.8515(3) 0.4203(4) 0.9905(3) 0.201(7) Uani 1 1 d DU . . O31 O 0.7332(6) 0.3682(3) 1.03707(13) 0.141(5) Uani 1 1 d DU . . F11 F 0.6284(3) 0.5021(4) 1.0064(2) 0.163(5) Uani 1 1 d DU . . F21 F 0.7344(5) 0.5491(3) 0.96580(15) 0.110(3) Uani 1 1 d D . . F31 F 0.7421(5) 0.5451(3) 1.02742(16) 0.113(3) Uani 1 1 d D . . C11 C 0.7136(3) 0.5063(2) 0.99966(13) 0.128(7) Uani 1 1 d DU . . S12 S 0.0100(3) 0.7987(2) 0.75204(9) 0.0750(10) Uani 1 1 d . . . O12 O 0.0527(6) 0.7901(5) 0.7142(2) 0.072(2) Uani 1 1 d . . . O22 O 0.0631(5) 0.7868(5) 0.7835(3) 0.072(2) Uani 1 1 d . . . O32 O -0.0751(7) 0.7618(7) 0.7617(3) 0.103(3) Uani 1 1 d U . . F12 F -0.0724(5) 0.9247(5) 0.7255(2) 0.081(2) Uani 1 1 d . . . F22 F 0.0473(6) 0.9495(5) 0.7443(3) 0.103(3) Uani 1 1 d . . . F32 F -0.0615(5) 0.9193(5) 0.7871(2) 0.089(2) Uani 1 1 d . . . C12 C -0.0217(10) 0.9047(9) 0.7503(4) 0.079(4) Uani 1 1 d . . . S13 S 0.1215(3) 0.1703(3) 0.86236(15) 0.1308(19) Uani 1 1 d D . . O13 O 0.1164(5) 0.2468(4) 0.8398(3) 0.162(6) Uani 1 1 d DU . . O23 O 0.0702(4) 0.1644(6) 0.90009(19) 0.133(4) Uani 1 1 d DU . . O33 O 0.1193(5) 0.1001(5) 0.8407(3) 0.182(7) Uani 1 1 d D . . F13 F 0.2875(3) 0.1722(6) 0.8427(2) 0.153(5) Uani 1 1 d D . . F23 F 0.2437(5) 0.2306(5) 0.8952(2) 0.152(4) Uani 1 1 d DU . . F33 F 0.2473(5) 0.1013(5) 0.8960(3) 0.196(6) Uani 1 1 d DU . . C13 C 0.2309(3) 0.1687(4) 0.87473(18) 0.164(9) Uani 1 1 d DU . . S14 S 0.5390(3) 0.2416(2) 0.76197(9) 0.0923(14) Uani 1 1 d D . . O14 O 0.5809(5) 0.2557(4) 0.72363(19) 0.0565(19) Uani 1 1 d . . . O24 O 0.4548(5) 0.2821(7) 0.7678(3) 0.111(4) Uani 1 1 d DU . . O34 O 0.5868(6) 0.2502(5) 0.7940(2) 0.067(2) Uani 1 1 d . . . F14 F 0.5696(7) 0.0900(7) 0.7648(3) 0.125(4) Uani 1 1 d . . . F24 F 0.4512(4) 0.1285(4) 0.74085(19) 0.0716(19) Uani 1 1 d . . . F34 F 0.4525(5) 0.1263(4) 0.80176(18) 0.0712(19) Uani 1 1 d . . . C14 C 0.4989(10) 0.1467(11) 0.7671(3) 0.096(6) Uani 1 1 d . . . S15 S 0.75589(16) 0.42920(15) 0.49069(7) 0.0429(6) Uani 1 1 d . . . O15 O 0.7178(5) 0.4631(5) 0.4580(2) 0.0574(19) Uani 1 1 d . . . O25 O 0.6992(4) 0.4172(4) 0.52657(19) 0.0504(17) Uani 1 1 d . . . O35 O 0.8133(4) 0.3635(5) 0.4825(2) 0.060(2) Uani 1 1 d . . . F15 F 0.8828(5) 0.5300(5) 0.4716(2) 0.092(3) Uani 1 1 d . . . F25 F 0.7806(6) 0.5721(4) 0.5115(2) 0.091(2) Uani 1 1 d . . . F35 F 0.8690(5) 0.4837(5) 0.5307(2) 0.086(2) Uani 1 1 d . . . C15 C 0.8244(8) 0.5080(8) 0.5013(3) 0.061(3) Uani 1 1 d . . . S16 S 0.61516(17) 0.85564(17) 0.63397(10) 0.0600(8) Uani 1 1 d . . . O16 O 0.6051(7) 0.9358(5) 0.6381(3) 0.094(3) Uani 1 1 d . . . O26 O 0.6963(5) 0.8201(6) 0.6383(3) 0.093(3) Uani 1 1 d . . . O36 O 0.5451(5) 0.8084(6) 0.6557(3) 0.081(3) Uani 1 1 d . . . F16 F 0.5309(5) 0.8772(6) 0.5730(3) 0.110(3) Uani 1 1 d . . . F26 F 0.6679(5) 0.8856(5) 0.5596(2) 0.091(2) Uani 1 1 d . . . F36 F 0.6092(6) 0.7713(4) 0.5737(2) 0.102(3) Uani 1 1 d . . . C16 C 0.6046(8) 0.8481(7) 0.5825(4) 0.072(4) Uani 1 1 d . . . S17 S 0.6121(3) 0.8629(3) 0.85434(16) 0.178(3) Uani 1 1 d DU . . O17 O 0.5654(4) 0.8796(6) 0.89143(19) 0.122(4) Uani 1 1 d DU . . O27 O 0.5971(5) 0.7854(4) 0.8407(3) 0.162(6) Uani 1 1 d DU . . O37 O 0.6150(6) 0.9293(5) 0.8245(2) 0.196(7) Uani 1 1 d DU . . F17 F 0.7315(5) 0.7948(6) 0.8919(3) 0.168(6) Uani 1 1 d D . . F27 F 0.7482(5) 0.9223(6) 0.8774(3) 0.193(6) Uani 1 1 d DU . . F37 F 0.7761(4) 0.8405(7) 0.8328(3) 0.247(9) Uani 1 1 d D . . C17 C 0.7231(3) 0.8546(4) 0.86460(19) 0.178(10) Uani 1 1 d DU . . S18 S 0.8602(2) 0.7660(3) 0.36072(13) 0.143(2) Uani 1 1 d DU . . O18 O 0.9348(3) 0.7768(4) 0.33194(16) 0.071(2) Uani 1 1 d D . . O28 O 0.8732(5) 0.7164(4) 0.39582(18) 0.108(4) Uani 1 1 d DU . . O38 O 0.7819(4) 0.7505(5) 0.3447(2) 0.165(6) Uani 1 1 d DU . . F18 F 0.8276(7) 0.9196(4) 0.3490(3) 0.278(10) Uani 1 1 d DU . . F28 F 0.7722(5) 0.8652(5) 0.4049(3) 0.181(5) Uani 1 1 d DU . . F38 F 0.9081(6) 0.8890(5) 0.3940(3) 0.203(6) Uani 1 1 d DU . . C18 C 0.8408(4) 0.8655(3) 0.3781(2) 0.35(3) Uani 1 1 d DU . . 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 Pd1 0.0333(4) 0.0273(4) 0.0344(4) -0.0034(3) -0.0044(3) 0.0011(3) Pd2 0.0759(6) 0.0439(5) 0.0309(5) -0.0038(3) 0.0155(4) -0.0016(4) P1 0.0386(13) 0.0265(12) 0.0329(13) -0.0026(9) -0.0044(10) 0.0032(10) P2 0.0315(12) 0.0335(13) 0.0420(14) -0.0057(10) -0.0050(10) 0.0022(10) P3 0.088(2) 0.0460(17) 0.0326(15) -0.0022(12) 0.0080(14) 0.0056(15) P4 0.081(2) 0.0443(16) 0.0390(16) -0.0096(12) 0.0221(14) -0.0031(15) N11 0.032(4) 0.038(4) 0.034(4) 0.001(3) 0.003(3) -0.004(3) N71 0.029(4) 0.050(5) 0.040(5) -0.001(4) -0.003(3) 0.005(4) N11' 0.070(6) 0.054(6) 0.028(5) 0.006(4) 0.005(4) -0.002(5) N71' 0.052(5) 0.065(6) 0.027(5) 0.007(4) 0.003(4) 0.006(4) O81 0.041(4) 0.074(5) 0.036(4) 0.001(3) 0.000(3) -0.004(4) C21 0.039(5) 0.027(5) 0.025(5) -0.001(3) 0.003(4) 0.004(4) C31 0.031(5) 0.041(5) 0.029(5) 0.002(4) -0.009(4) 0.001(4) C41 0.029(5) 0.061(7) 0.047(6) 0.009(5) -0.004(4) -0.009(5) C51 0.051(6) 0.074(8) 0.034(6) 0.005(5) 0.011(5) -0.012(6) C61 0.032(5) 0.045(6) 0.034(5) 0.006(4) 0.001(4) 0.003(4) C81 0.049(6) 0.038(5) 0.032(5) 0.005(4) -0.003(4) -0.006(5) C21' 0.063(7) 0.059(7) 0.037(6) 0.005(5) 0.000(5) 0.005(6) C31' 0.060(7) 0.057(7) 0.042(6) -0.005(5) 0.002(5) -0.002(6) C41' 0.066(7) 0.064(8) 0.042(7) 0.012(5) 0.002(5) -0.004(6) C51' 0.091(9) 0.053(7) 0.037(7) 0.011(5) -0.008(6) -0.014(6) C61' 0.100(10) 0.058(7) 0.025(6) -0.008(5) 0.020(6) -0.004(7) N12 0.034(4) 0.026(4) 0.032(4) -0.008(3) -0.002(3) 0.007(3) N72 0.060(5) 0.026(4) 0.048(5) -0.002(4) 0.007(4) 0.003(4) N12' 0.089(7) 0.036(5) 0.057(6) -0.006(4) 0.015(5) -0.009(5) N72' 0.116(8) 0.033(5) 0.037(5) -0.002(4) 0.007(5) -0.018(5) O82 0.094(6) 0.033(4) 0.056(5) -0.007(3) -0.011(4) -0.006(4) C22 0.044(5) 0.025(5) 0.052(6) 0.006(4) -0.002(4) -0.004(4) C32 0.031(5) 0.032(5) 0.044(6) -0.006(4) -0.001(4) 0.001(4) C42 0.043(6) 0.034(5) 0.054(7) 0.000(5) -0.008(5) 0.000(4) C52 0.052(6) 0.043(6) 0.040(6) 0.003(4) 0.007(5) 0.012(5) C62 0.044(6) 0.038(6) 0.047(6) -0.012(5) -0.002(4) 0.006(4) C82 0.053(6) 0.037(6) 0.049(7) 0.001(5) 0.004(5) -0.002(5) C22' 0.083(8) 0.044(6) 0.041(7) -0.007(5) 0.013(5) -0.009(6) C32' 0.096(9) 0.043(6) 0.037(6) -0.017(5) 0.021(6) -0.020(6) C42' 0.079(8) 0.050(7) 0.055(8) -0.014(5) 0.004(6) -0.021(6) C52' 0.080(8) 0.063(8) 0.046(7) -0.020(6) 0.001(6) -0.009(6) C62' 0.077(8) 0.060(8) 0.032(6) -0.009(5) -0.009(5) -0.007(6) C100 0.066(7) 0.026(5) 0.033(5) -0.007(4) 0.000(4) 0.003(5) C101 0.048(6) 0.028(5) 0.060(7) -0.003(4) 0.001(5) -0.006(4) C102 0.043(6) 0.026(5) 0.073(7) -0.002(5) -0.012(5) 0.003(4) C103 0.048(5) 0.033(5) 0.027(5) -0.005(4) -0.007(4) 0.010(4) C104 0.057(6) 0.041(6) 0.035(6) 0.003(4) -0.005(5) 0.004(5) C105 0.086(9) 0.053(7) 0.047(7) -0.003(5) -0.028(6) -0.003(6) C106 0.061(7) 0.039(6) 0.081(9) -0.011(6) -0.032(6) 0.019(5) C107 0.048(6) 0.069(8) 0.049(7) -0.002(6) -0.006(5) 0.022(6) C108 0.047(6) 0.049(6) 0.050(6) -0.011(5) -0.013(5) 0.011(5) C109 0.045(5) 0.030(5) 0.034(5) -0.002(4) -0.001(4) 0.008(4) C110 0.063(7) 0.051(7) 0.041(6) -0.014(5) -0.012(5) 0.005(5) C111 0.089(9) 0.071(8) 0.036(7) -0.016(6) -0.003(6) 0.002(7) C112 0.069(8) 0.092(10) 0.042(7) -0.009(7) -0.021(6) 0.020(7) C113 0.078(8) 0.065(8) 0.039(7) 0.012(6) -0.009(6) 0.012(7) C114 0.049(6) 0.044(6) 0.035(6) 0.010(4) -0.003(4) 0.005(5) C115 0.045(6) 0.041(6) 0.060(7) -0.016(5) -0.012(5) 0.008(5) C116 0.088(10) 0.139(14) 0.062(9) 0.016(8) -0.046(7) -0.053(9) C117 0.089(8) 0.120(9) 0.096(8) 0.001(7) -0.032(7) -0.039(7) C118 0.110(12) 0.118(13) 0.062(9) 0.010(8) -0.061(9) -0.017(10) C119 0.062(7) 0.053(7) 0.067(8) -0.006(6) -0.017(6) 0.008(6) C120 0.038(5) 0.048(6) 0.041(6) -0.007(4) -0.010(4) 0.002(5) C121 0.045(6) 0.035(5) 0.042(6) 0.001(4) -0.006(4) -0.001(4) C122 0.048(6) 0.039(6) 0.050(6) 0.000(5) -0.004(5) 0.005(5) C123 0.033(5) 0.045(6) 0.077(9) 0.004(5) 0.001(5) 0.007(5) C124 0.058(7) 0.036(6) 0.066(8) -0.004(5) 0.012(6) 0.005(5) C125 0.072(8) 0.053(7) 0.062(8) -0.005(6) 0.013(6) 0.010(6) C126 0.063(7) 0.034(5) 0.038(6) 0.005(4) -0.005(5) 0.012(5) C127 0.076(8) 0.055(7) 0.043(7) -0.014(5) 0.009(5) -0.002(6) C128 0.107(11) 0.042(7) 0.090(10) -0.028(6) 0.038(8) -0.022(7) C129 0.067(8) 0.058(8) 0.062(8) -0.009(6) 0.005(6) -0.008(6) C130 0.112(11) 0.066(8) 0.033(6) -0.015(5) -0.003(6) 0.012(7) C131 0.096(10) 0.051(7) 0.065(8) -0.014(6) -0.029(8) -0.002(7) C132 0.102(11) 0.061(9) 0.071(10) -0.011(7) -0.014(8) 0.008(8) C133 0.080(9) 0.092(11) 0.066(9) -0.027(8) 0.006(7) 0.023(8) C134 0.119(13) 0.141(16) 0.054(9) -0.045(9) -0.003(9) 0.052(12) C135 0.079(9) 0.151(15) 0.044(8) -0.037(8) 0.008(6) 0.038(9) C136 0.157(14) 0.052(8) 0.028(6) 0.005(5) 0.008(7) 0.011(8) C137 0.099(10) 0.080(9) 0.029(6) -0.004(6) 0.009(6) -0.025(7) C138 0.178(17) 0.052(8) 0.046(8) 0.004(6) -0.012(9) -0.029(9) C139 0.131(9) 0.093(8) 0.073(8) -0.010(7) 0.000(7) -0.017(7) C140 0.140(9) 0.081(8) 0.068(7) 0.009(6) -0.009(7) -0.011(7) C141 0.117(8) 0.078(8) 0.064(7) 0.004(6) -0.005(6) -0.014(7) C142 0.084(8) 0.054(7) 0.037(6) 0.000(5) 0.022(6) -0.001(6) C143 0.098(10) 0.073(9) 0.056(8) -0.009(7) 0.008(7) -0.007(8) C144 0.108(11) 0.098(11) 0.041(8) -0.011(7) 0.018(7) -0.005(9) C145 0.096(11) 0.134(15) 0.049(9) -0.016(9) 0.020(8) 0.021(11) C146 0.111(12) 0.110(13) 0.062(10) -0.003(8) 0.050(9) -0.029(10) C147 0.114(12) 0.078(10) 0.059(9) -0.010(7) 0.038(8) -0.023(8) C148 0.066(7) 0.049(7) 0.047(7) -0.011(5) 0.017(5) -0.003(5) C149 0.130(13) 0.066(9) 0.041(7) -0.021(6) 0.005(7) -0.001(8) C150 0.120(12) 0.093(12) 0.055(9) -0.019(8) -0.018(8) 0.029(10) C151 0.088(9) 0.059(8) 0.060(8) 0.012(6) 0.009(7) 0.017(7) C152 0.113(11) 0.071(9) 0.039(7) -0.010(6) -0.005(7) 0.023(8) C153 0.084(9) 0.052(7) 0.053(7) -0.011(6) -0.010(6) 0.020(6) Pd3 0.0288(4) 0.0337(4) 0.0406(4) -0.0017(3) 0.0029(3) 0.0010(3) Pd4 0.0758(6) 0.0577(6) 0.0353(5) 0.0020(4) 0.0165(4) -0.0032(5) P5 0.0299(12) 0.0347(14) 0.0630(18) -0.0091(12) 0.0044(11) 0.0005(11) P6 0.0287(12) 0.0345(13) 0.0478(15) 0.0015(11) 0.0012(10) 0.0012(10) P7 0.080(2) 0.063(2) 0.0470(18) -0.0001(15) 0.0227(16) -0.0057(17) P8 0.075(2) 0.061(2) 0.0408(17) -0.0021(14) 0.0133(14) -0.0020(16) N13 0.034(4) 0.036(5) 0.048(5) -0.006(4) 0.010(3) -0.004(3) N73 0.075(6) 0.034(5) 0.053(6) 0.009(4) 0.015(5) 0.012(4) N13' 0.090(7) 0.053(6) 0.031(5) 0.013(4) 0.006(5) -0.004(5) N73' 0.097(8) 0.033(5) 0.059(7) 0.008(4) 0.000(5) 0.007(5) O83 0.113(7) 0.031(4) 0.052(5) 0.006(3) -0.003(4) 0.005(4) C23 0.044(6) 0.027(5) 0.055(7) -0.005(4) 0.019(5) -0.001(4) C33 0.053(6) 0.043(6) 0.043(6) 0.000(5) 0.016(5) 0.010(5) C43 0.052(6) 0.044(6) 0.055(7) 0.010(5) 0.007(5) 0.004(5) C53 0.055(6) 0.033(6) 0.061(7) 0.000(5) -0.007(5) 0.007(5) C63 0.044(6) 0.041(6) 0.052(7) 0.002(5) -0.002(5) -0.004(5) C83 0.065(7) 0.052(8) 0.060(8) 0.001(6) 0.027(6) -0.007(6) C23' 0.072(8) 0.050(7) 0.052(8) 0.014(5) 0.016(6) 0.007(6) C33' 0.075(8) 0.053(7) 0.052(7) 0.015(6) 0.018(6) 0.009(6) C43' 0.092(10) 0.060(8) 0.056(8) 0.015(6) -0.001(7) 0.013(7) C53' 0.081(9) 0.059(9) 0.064(9) 0.014(6) 0.015(7) 0.021(7) C63' 0.072(9) 0.112(13) 0.047(8) 0.007(7) 0.013(6) -0.007(8) N14 0.028(4) 0.041(4) 0.030(4) 0.003(3) -0.005(3) 0.006(3) N74 0.031(4) 0.055(5) 0.035(5) -0.002(4) -0.007(3) 0.000(4) N14' 0.064(6) 0.052(6) 0.038(5) -0.009(4) 0.006(4) 0.009(4) N74' 0.041(4) 0.060(6) 0.029(4) -0.002(4) -0.005(3) -0.004(4) O84 0.038(4) 0.088(6) 0.033(4) 0.004(4) 0.000(3) -0.010(4) C24 0.032(5) 0.037(5) 0.035(5) 0.007(4) 0.002(4) 0.003(4) C34 0.034(5) 0.037(5) 0.041(6) 0.004(4) 0.002(4) 0.000(4) C44 0.030(5) 0.038(5) 0.042(6) 0.003(4) -0.004(4) 0.006(4) C54 0.034(5) 0.052(6) 0.033(5) 0.001(4) 0.005(4) 0.012(4) C64 0.036(5) 0.049(6) 0.035(5) 0.003(4) -0.002(4) -0.003(4) C84 0.044(6) 0.055(6) 0.031(5) -0.002(4) 0.003(4) 0.003(5) C24' 0.055(6) 0.057(7) 0.025(5) 0.001(4) 0.008(4) 0.009(5) C34' 0.067(7) 0.035(5) 0.034(6) 0.001(4) -0.006(5) 0.002(5) C44' 0.059(7) 0.057(7) 0.041(6) -0.013(5) -0.009(5) 0.011(5) C54' 0.108(11) 0.069(8) 0.035(7) 0.000(6) -0.023(7) -0.001(8) C64' 0.080(9) 0.072(8) 0.027(6) -0.005(5) -0.001(6) 0.014(7) C154 0.029(5) 0.039(6) 0.073(7) -0.025(5) 0.016(5) -0.002(4) C155 0.041(6) 0.048(7) 0.078(8) -0.023(6) -0.002(5) 0.002(5) C156 0.033(5) 0.040(6) 0.059(7) -0.009(5) -0.004(4) 0.007(4) C157 0.030(5) 0.040(6) 0.058(7) -0.014(5) 0.007(4) -0.005(4) C158 0.077(8) 0.050(7) 0.057(8) -0.006(5) 0.004(6) -0.019(6) C159 0.061(7) 0.079(9) 0.057(8) -0.005(6) 0.007(6) -0.011(7) C160 0.044(6) 0.035(6) 0.068(8) 0.006(5) 0.003(5) -0.002(5) C161 0.046(6) 0.044(6) 0.082(9) 0.007(6) -0.017(6) -0.013(5) C162 0.029(5) 0.058(7) 0.054(7) -0.007(5) -0.006(4) -0.004(5) C163 0.032(5) 0.033(5) 0.062(7) -0.003(5) -0.003(4) 0.009(4) C164 0.039(6) 0.058(8) 0.095(10) -0.014(7) -0.011(6) 0.014(5) C165 0.056(7) 0.073(9) 0.108(11) -0.038(8) -0.041(7) 0.016(7) C166 0.057(7) 0.075(9) 0.068(8) -0.017(7) -0.029(6) -0.009(6) C167 0.052(7) 0.075(8) 0.063(8) -0.034(6) 0.007(6) 0.010(6) C168 0.043(6) 0.071(8) 0.061(7) -0.022(6) -0.019(5) 0.012(5) C169 0.040(5) 0.049(6) 0.042(6) 0.009(5) 0.003(4) 0.013(5) C170 0.062(7) 0.069(8) 0.040(7) 0.000(5) 0.004(5) 0.005(6) C171 0.072(8) 0.075(9) 0.041(7) 0.009(6) 0.004(5) 0.022(7) C172 0.094(10) 0.102(12) 0.058(9) 0.014(8) 0.005(7) 0.047(9) C173 0.109(12) 0.067(10) 0.099(12) 0.037(9) 0.011(9) 0.026(9) C174 0.111(11) 0.059(8) 0.068(9) 0.009(7) 0.017(8) 0.035(8) C175 0.051(6) 0.033(6) 0.062(7) -0.002(5) -0.004(5) -0.001(5) C176 0.051(7) 0.039(6) 0.087(9) -0.019(6) 0.010(6) -0.006(5) C177 0.044(7) 0.052(8) 0.114(12) -0.023(7) -0.004(7) -0.005(6) C178 0.048(8) 0.040(7) 0.162(16) -0.018(8) -0.044(9) 0.003(6) C179 0.082(10) 0.040(7) 0.101(11) -0.010(6) -0.049(8) 0.011(7) C180 0.069(8) 0.053(7) 0.068(8) -0.002(6) -0.024(6) 0.003(6) C181 0.076(9) 0.083(10) 0.070(9) -0.024(7) 0.010(7) -0.001(7) C182 0.067(8) 0.058(8) 0.070(8) -0.002(6) 0.017(6) 0.002(6) C183 0.081(9) 0.067(8) 0.052(7) -0.001(6) 0.002(6) 0.000(7) C184 0.080(8) 0.060(8) 0.040(7) 0.005(5) 0.021(6) 0.002(6) C185 0.077(9) 0.095(11) 0.038(7) 0.005(6) 0.013(6) -0.008(8) C186 0.112(12) 0.068(9) 0.052(8) 0.012(6) 0.017(7) -0.013(8) C187 0.078(9) 0.068(9) 0.078(10) -0.001(7) 0.004(7) -0.027(7) C188 0.091(10) 0.078(10) 0.051(8) 0.013(7) -0.010(7) 0.002(8) C189 0.083(9) 0.069(9) 0.064(9) 0.016(7) 0.005(7) -0.017(7) C190 0.056(7) 0.079(9) 0.068(9) 0.000(7) 0.030(6) -0.005(7) C191 0.083(11) 0.114(14) 0.096(13) -0.012(10) 0.027(9) -0.002(10) C192 0.113(13) 0.135(15) 0.041(8) 0.001(8) 0.012(8) -0.007(11) C193 0.129(16) 0.160(19) 0.049(10) -0.022(11) 0.036(10) -0.060(14) C194 0.136(16) 0.130(16) 0.064(11) -0.009(10) 0.065(11) -0.011(13) C195 0.147(15) 0.075(10) 0.067(10) -0.006(7) 0.036(9) 0.011(10) C196 0.070(8) 0.087(10) 0.041(7) -0.010(6) 0.015(6) 0.001(7) C197 0.088(10) 0.112(12) 0.042(8) -0.003(7) 0.005(6) 0.004(9) C198 0.102(12) 0.124(15) 0.076(11) -0.013(10) 0.010(9) -0.007(11) C199 0.112(9) 0.105(9) 0.075(8) -0.018(7) -0.013(7) 0.025(7) C200 0.123(13) 0.066(10) 0.095(12) -0.030(9) -0.025(10) 0.031(9) C201 0.109(11) 0.075(10) 0.055(8) -0.014(7) 0.018(7) -0.002(8) C202 0.073(8) 0.065(8) 0.045(7) -0.001(6) 0.019(6) 0.002(6) C203 0.107(11) 0.068(9) 0.053(8) 0.004(6) 0.022(7) 0.015(8) C204 0.110(12) 0.068(10) 0.074(10) 0.009(7) 0.039(9) 0.000(9) C205 0.095(11) 0.044(8) 0.098(12) 0.009(7) 0.035(10) 0.002(8) C206 0.098(12) 0.071(10) 0.106(13) -0.032(9) -0.007(10) -0.004(9) C207 0.062(8) 0.060(8) 0.077(9) -0.025(7) 0.011(7) -0.002(6) S11 0.148(4) 0.095(3) 0.071(3) 0.015(2) -0.047(3) -0.027(3) O11 0.160(8) 0.115(7) 0.073(6) -0.030(5) -0.005(6) 0.007(6) O21 0.163(10) 0.224(11) 0.210(11) 0.008(9) -0.022(8) 0.006(9) O31 0.197(9) 0.111(8) 0.111(7) -0.014(6) -0.002(7) -0.014(7) F11 0.148(8) 0.181(9) 0.158(8) -0.047(7) 0.011(6) -0.030(7) F21 0.170(9) 0.105(7) 0.043(4) 0.008(4) 0.022(5) 0.012(6) F31 0.175(9) 0.104(7) 0.059(5) -0.013(5) 0.003(5) -0.028(6) C11 0.151(11) 0.131(10) 0.106(10) -0.034(8) -0.014(8) -0.011(9) S12 0.103(3) 0.071(2) 0.0466(19) -0.0048(15) 0.0092(17) 0.003(2) O12 0.107(7) 0.062(5) 0.039(4) -0.014(4) 0.033(4) -0.007(5) O22 0.069(5) 0.077(6) 0.074(6) -0.032(5) -0.002(4) 0.006(5) O32 0.113(7) 0.113(7) 0.081(6) -0.009(5) 0.004(5) -0.055(6) F12 0.075(5) 0.108(6) 0.062(5) -0.021(4) -0.009(4) 0.020(4) F22 0.105(7) 0.075(6) 0.126(8) -0.022(5) 0.012(5) -0.013(5) F32 0.088(5) 0.113(7) 0.069(5) -0.052(5) -0.003(4) 0.018(5) C12 0.073(9) 0.081(10) 0.081(10) -0.028(8) 0.017(8) -0.002(8) S13 0.121(4) 0.122(4) 0.151(5) -0.036(4) -0.014(4) 0.022(3) O13 0.159(9) 0.142(9) 0.188(10) -0.009(8) -0.042(8) -0.001(7) O23 0.111(7) 0.168(9) 0.118(7) -0.044(7) 0.012(6) 0.006(7) O33 0.239(18) 0.146(13) 0.180(15) -0.105(12) -0.021(13) -0.063(12) F13 0.100(7) 0.216(14) 0.136(9) -0.032(9) 0.027(7) 0.009(8) F23 0.155(8) 0.165(8) 0.154(8) -0.084(7) -0.039(6) -0.006(6) F33 0.157(8) 0.189(9) 0.238(10) 0.044(8) -0.053(8) -0.014(7) C13 0.163(12) 0.159(12) 0.173(12) -0.006(9) -0.034(9) -0.037(9) S14 0.146(4) 0.094(3) 0.0352(18) 0.0005(16) 0.0028(19) -0.059(3) O14 0.074(5) 0.061(5) 0.030(4) 0.001(3) 0.011(3) -0.013(4) O24 0.112(7) 0.120(7) 0.100(7) -0.029(6) -0.004(5) 0.068(6) O34 0.094(6) 0.070(5) 0.037(4) 0.003(4) -0.010(4) -0.017(5) F14 0.141(9) 0.136(9) 0.094(7) -0.015(6) -0.008(6) 0.067(7) F24 0.076(5) 0.085(5) 0.054(4) -0.005(3) -0.003(3) -0.026(4) F34 0.088(5) 0.079(5) 0.041(4) 0.004(3) 0.012(3) -0.025(4) C14 0.103(11) 0.153(16) 0.029(7) 0.005(8) 0.007(7) -0.059(11) S15 0.0466(14) 0.0406(14) 0.0400(14) -0.0031(11) -0.0003(11) 0.0016(11) O15 0.072(5) 0.055(5) 0.045(4) 0.004(3) -0.014(4) 0.010(4) O25 0.050(4) 0.054(5) 0.044(4) -0.003(3) 0.006(3) -0.002(3) O35 0.044(4) 0.056(5) 0.079(6) -0.012(4) -0.003(4) 0.000(4) F15 0.097(6) 0.111(6) 0.065(5) 0.012(4) -0.005(4) -0.059(5) F25 0.125(7) 0.050(4) 0.101(6) -0.020(4) -0.013(5) -0.002(4) F35 0.102(6) 0.091(6) 0.071(5) 0.023(4) -0.040(4) -0.042(5) C15 0.081(8) 0.063(8) 0.037(6) 0.009(5) -0.006(6) -0.031(7) S16 0.0396(15) 0.0394(16) 0.101(2) -0.0150(15) -0.0015(14) 0.0017(12) O16 0.121(8) 0.042(5) 0.116(8) -0.004(5) -0.007(6) -0.001(5) O26 0.039(5) 0.111(8) 0.125(8) 0.003(6) -0.006(5) 0.004(5) O36 0.060(5) 0.084(6) 0.094(7) -0.006(5) 0.012(5) -0.030(5) F16 0.061(5) 0.147(9) 0.124(7) -0.025(6) -0.020(5) 0.037(5) F26 0.082(5) 0.067(5) 0.110(6) 0.006(4) 0.028(5) -0.002(4) F36 0.163(8) 0.047(4) 0.094(6) -0.024(4) 0.008(5) 0.001(5) C16 0.053(7) 0.047(7) 0.110(11) -0.018(7) 0.018(7) -0.005(6) S17 0.189(6) 0.138(5) 0.195(6) -0.069(4) 0.076(5) -0.082(4) O17 0.100(7) 0.156(8) 0.100(7) 0.013(6) 0.006(6) 0.018(6) O27 0.169(9) 0.125(8) 0.204(10) -0.035(8) -0.056(8) -0.026(7) O37 0.227(11) 0.189(11) 0.167(10) 0.027(8) -0.031(8) 0.020(9) F17 0.135(9) 0.197(13) 0.147(10) 0.103(9) -0.005(7) -0.007(8) F27 0.178(9) 0.193(9) 0.228(10) -0.081(8) -0.060(8) -0.010(7) F37 0.125(11) 0.35(3) 0.251(18) -0.132(17) 0.087(11) -0.002(12) C17 0.192(13) 0.170(13) 0.180(13) -0.047(10) -0.036(10) 0.021(10) S18 0.059(2) 0.235(6) 0.145(4) -0.074(4) -0.017(3) 0.016(3) O18 0.062(5) 0.080(6) 0.063(5) 0.000(4) 0.012(4) 0.024(4) O28 0.143(8) 0.092(6) 0.096(6) 0.015(5) -0.061(6) -0.010(6) O38 0.117(8) 0.211(10) 0.177(9) -0.010(8) -0.052(7) -0.018(7) F18 0.299(13) 0.267(13) 0.269(13) -0.012(9) -0.043(9) -0.019(9) F28 0.168(8) 0.147(8) 0.218(9) -0.060(7) 0.046(7) -0.019(7) F38 0.195(10) 0.199(10) 0.216(10) -0.047(8) -0.006(8) -0.042(8) C18 0.35(3) 0.34(3) 0.36(3) -0.031(11) -0.046(11) -0.005(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pd1 N12 2.100(7) . ? Pd1 N11 2.106(7) . ? Pd1 P1 2.275(2) . ? Pd1 P2 2.281(2) . ? Pd2 N11' 2.078(9) . ? Pd2 N12' 2.113(9) . ? Pd2 P4 2.262(3) . ? Pd2 P3 2.274(3) . ? P1 C109 1.801(9) . ? P1 C103 1.809(9) . ? P1 C100 1.815(10) . ? P2 C102 1.806(10) . ? P2 C115 1.829(11) . ? P2 C121 1.823(10) . ? P3 C130 1.817(14) . ? P3 C136 1.803(12) . ? P3 C127 1.812(12) . ? P4 C142 1.797(11) . ? P4 C148 1.824(13) . ? P4 C129 1.829(12) . ? N11 C21 1.312(11) . ? N11 C61 1.371(11) . ? N71 C81 1.368(12) . ? N71 C31 1.404(11) . ? N71 H71 0.8800 . ? N11' C21' 1.334(13) . ? N11' C61' 1.350(15) . ? N71' C81 1.379(12) . ? N71' C31' 1.399(13) . ? N71' H71' 0.8800 . ? O81 C81 1.221(11) . ? C21 C31 1.390(12) . ? C21 H21 0.9500 . ? C31 C41 1.425(13) . ? C41 C51 1.377(14) . ? C41 H41 0.9500 . ? C51 C61 1.349(14) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C21' C31' 1.378(15) . ? C21' H21' 0.9500 . ? C31' C41' 1.394(16) . ? C41' C51' 1.383(15) . ? C41' H41' 0.9500 . ? C51' C61' 1.381(17) . ? C51' H51' 0.9500 . ? C61' H61' 0.9500 . ? N12 C62 1.331(12) . ? N12 C22 1.332(12) . ? N72 C82 1.365(13) . ? N72 C32 1.395(12) . ? N72 H72 0.8800 . ? N12' C62' 1.326(13) . ? N12' C22' 1.351(14) . ? N72' C82 1.374(13) . ? N72' C32' 1.369(14) . ? N72' H72' 0.8800 . ? O82 C82 1.189(12) . ? C22 C32 1.408(12) . ? C22 H22 0.9500 . ? C32 C42 1.402(13) . ? C42 C52 1.387(14) . ? C42 H42 0.9500 . ? C52 C62 1.386(14) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C22' C32' 1.414(15) . ? C22' H22' 0.9500 . ? C32' C42' 1.415(14) . ? C42' C52' 1.354(17) . ? C42' H42' 0.9500 . ? C52' C62' 1.348(16) . ? C52' H52' 0.9500 . ? C62' H62' 0.9500 . ? C100 C101 1.533(14) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.530(13) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? C103 C104 1.373(13) . ? C103 C108 1.391(14) . ? C104 C105 1.437(15) . ? C104 H104 0.9500 . ? C105 C106 1.364(17) . ? C105 H105 0.9500 . ? C106 C107 1.370(16) . ? C106 H106 0.9500 . ? C107 C108 1.405(14) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C110 1.365(13) . ? C109 C114 1.388(13) . ? C110 C111 1.412(14) . ? C110 H110 0.9500 . ? C111 C112 1.394(17) . ? C111 H111 0.9500 . ? C112 C113 1.309(17) . ? C112 H112 0.9500 . ? C113 C114 1.404(15) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C115 C120 1.308(14) . ? C115 C116 1.383(15) . ? C116 C117 1.353(19) . ? C116 H116 0.9500 . ? C117 C118 1.42(2) . ? C117 H117 0.9500 . ? C118 C119 1.355(17) . ? C118 H118 0.9500 . ? C119 C120 1.380(14) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? C121 C126 1.340(13) . ? C121 C122 1.426(14) . ? C122 C123 1.395(14) . ? C122 H122 0.9500 . ? C123 C124 1.375(16) . ? C123 H123 0.9500 . ? C124 C125 1.374(16) . ? C124 H124 0.9500 . ? C125 C126 1.418(14) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C127 C128 1.595(16) . ? C127 H12A 0.9900 . ? C127 H12B 0.9900 . ? C128 C129 1.571(18) . ? C128 H12C 0.9900 . ? C128 H12D 0.9900 . ? C129 H12E 0.9900 . ? C129 H12F 0.9900 . ? C130 C135 1.404(16) . ? C130 C131 1.441(18) . ? C131 C132 1.346(19) . ? C131 H131 0.9500 . ? C132 C133 1.317(18) . ? C132 H132 0.9500 . ? C133 C134 1.37(2) . ? C133 H133 0.9500 . ? C134 C135 1.395(18) . ? C134 H134 0.9500 . ? C135 H135 0.9500 . ? C136 C137 1.418(17) . ? C136 C141 1.395(19) . ? C137 C138 1.414(16) . ? C137 H137 0.9500 . ? C138 C139 1.41(2) . ? C138 H138 0.9500 . ? C139 C140 1.42(2) . ? C139 H139 0.9500 . ? C140 C141 1.426(19) . ? C140 H140 0.9500 . ? C141 H141 0.9500 . ? C142 C143 1.342(18) . ? C142 C147 1.421(17) . ? C143 C144 1.443(17) . ? C143 H143 0.9500 . ? C144 C145 1.28(2) . ? C144 H144 0.9500 . ? C145 C146 1.40(2) . ? C145 H145 0.9500 . ? C146 C147 1.338(19) . ? C146 H146 0.9500 . ? C147 H147 0.9500 . ? C148 C149 1.382(17) . ? C148 C153 1.388(15) . ? C149 C150 1.360(19) . ? C149 H149 0.9500 . ? C150 C151 1.391(18) . ? C150 H150 0.9500 . ? C151 C152 1.384(17) . ? C151 H151 0.9500 . ? C152 C153 1.370(17) . ? C152 H152 0.9500 . ? C153 H153 0.9500 . ? Pd3 N14 2.102(7) . ? Pd3 N13 2.106(8) . ? Pd3 P5 2.263(3) . ? Pd3 P6 2.277(3) . ? Pd4 N13' 2.088(10) . ? Pd4 N14' 2.119(9) . ? Pd4 P7 2.269(4) . ? Pd4 P8 2.273(3) . ? P5 C163 1.789(11) . ? P5 C154 1.811(9) . ? P5 C157 1.810(10) . ? P6 C156 1.801(9) . ? P6 C169 1.816(10) . ? P6 C175 1.816(11) . ? P7 C184 1.803(13) . ? P7 C190 1.811(13) . ? P7 C181 1.806(15) . ? P8 C183 1.807(13) . ? P8 C196 1.825(12) . ? P8 C202 1.838(12) . ? N13 C63 1.306(12) . ? N13 C23 1.338(13) . ? N73 C83 1.357(15) . ? N73 C33 1.388(13) . ? N73 H73 0.8800 . ? N13' C23' 1.318(15) . ? N13' C63' 1.409(16) . ? N73' C83 1.368(15) . ? N73' C33' 1.419(16) . ? N73' H73' 0.8800 . ? O83 C83 1.202(13) . ? C23 C33 1.368(14) . ? C23 H23 0.9500 . ? C33 C43 1.414(15) . ? C43 C53 1.346(15) . ? C43 H43 0.9500 . ? C53 C63 1.379(14) . ? C53 H53 0.9500 . ? C63 H63 0.9500 . ? C23' C33' 1.418(17) . ? C23' H23' 0.9500 . ? C33' C43' 1.348(16) . ? C43' C53' 1.380(19) . ? C43' H43' 0.9500 . ? C53' C63' 1.320(19) . ? C53' H53' 0.9500 . ? C63' H63' 0.9500 . ? N14 C24 1.325(11) . ? N14 C64 1.365(11) . ? N74 C84 1.370(12) . ? N74 C34 1.419(12) . ? N74 H74 0.8800 . ? N14' C24' 1.337(12) . ? N14' C64' 1.345(14) . ? N74' C84 1.407(12) . ? N74' C34' 1.419(12) . ? N74' H74' 0.8800 . ? O84 C84 1.202(11) . ? C24 C34 1.396(12) . ? C24 H24 0.9500 . ? C34 C44 1.373(13) . ? C44 C54 1.377(13) . ? C44 H44 0.9500 . ? C54 C64 1.353(13) . ? C54 H54 0.9500 . ? C64 H64 0.9500 . ? C24' C34' 1.382(14) . ? C24' H24' 0.9500 . ? C34' C44' 1.381(14) . ? C44' C54' 1.342(15) . ? C44' H44' 0.9500 . ? C54' C64' 1.384(17) . ? C54' H54' 0.9500 . ? C64' H64' 0.9500 . ? C154 C155 1.543(15) . ? C154 H15A 0.9900 . ? C154 H15B 0.9900 . ? C155 C156 1.552(13) . ? C155 H15C 0.9900 . ? C155 H15D 0.9900 . ? C156 H15E 0.9900 . ? C156 H15F 0.9900 . ? C157 C162 1.386(14) . ? C157 C158 1.396(15) . ? C158 C159 1.381(16) . ? C158 H158 0.9500 . ? C159 C160 1.369(16) . ? C159 H159 0.9500 . ? C160 C161 1.350(16) . ? C160 H160 0.9500 . ? C161 C162 1.393(15) . ? C161 H161 0.9500 . ? C162 H162 0.9500 . ? C163 C164 1.398(14) . ? C163 C168 1.405(14) . ? C164 C165 1.375(17) . ? C164 H164 0.9500 . ? C165 C166 1.364(17) . ? C165 H165 0.9500 . ? C166 C167 1.384(16) . ? C166 H166 0.9500 . ? C167 C168 1.422(15) . ? C167 H167 0.9500 . ? C168 H168 0.9500 . ? C169 C174 1.384(16) . ? C169 C170 1.425(15) . ? C170 C171 1.342(15) . ? C170 H170 0.9500 . ? C171 C172 1.336(18) . ? C171 H171 0.9500 . ? C172 C173 1.42(2) . ? C172 H172 0.9500 . ? C173 C174 1.367(19) . ? C173 H173 0.9500 . ? C174 H174 0.9500 . ? C175 C180 1.374(16) . ? C175 C176 1.399(15) . ? C176 C177 1.366(16) . ? C176 H176 0.9500 . ? C177 C178 1.37(2) . ? C177 H177 0.9500 . ? C178 C179 1.35(2) . ? C178 H178 0.9500 . ? C179 C180 1.409(16) . ? C179 H179 0.9500 . ? C180 H180 0.9500 . ? C181 C182 1.528(18) . ? C181 H18A 0.9900 . ? C181 H18B 0.9900 . ? C182 C183 1.540(16) . ? C182 H18C 0.9900 . ? C182 H18D 0.9900 . ? C183 H18E 0.9900 . ? C183 H18F 0.9900 . ? C184 C185 1.388(16) . ? C184 C189 1.383(17) . ? C185 C186 1.359(19) . ? C185 H185 0.9500 . ? C186 C187 1.326(18) . ? C186 H186 0.9500 . ? C187 C188 1.370(17) . ? C187 H187 0.9500 . ? C188 C189 1.366(18) . ? C188 H188 0.9500 . ? C189 H189 0.9500 . ? C190 C191 1.38(2) . ? C190 C195 1.386(19) . ? C191 C192 1.34(2) . ? C191 H191 0.9500 . ? C192 C193 1.30(2) . ? C192 H192 0.9500 . ? C193 C194 1.36(3) . ? C193 H193 0.9500 . ? C194 C195 1.38(2) . ? C194 H194 0.9500 . ? C195 H195 0.9500 . ? C196 C201 1.335(18) . ? C196 C197 1.401(19) . ? C197 C198 1.444(19) . ? C197 H197 0.9500 . ? C198 C199 1.39(2) . ? C198 H198 0.9500 . ? C199 C200 1.31(2) . ? C199 H199 0.9500 . ? C200 C201 1.405(19) . ? C200 H200 0.9500 . ? C201 H201 0.9500 . ? C202 C207 1.365(18) . ? C202 C203 1.377(17) . ? C203 C204 1.42(2) . ? C203 H203 0.9500 . ? C204 C205 1.36(2) . ? C204 H204 0.9500 . ? C205 C206 1.32(2) . ? C205 H205 0.9500 . ? C206 C207 1.36(2) . ? C206 H206 0.9500 . ? C207 H207 0.9500 . ? S11 O31 1.448(6) . ? S11 O11 1.447(8) . ? S11 O21 1.451(7) . ? S11 C11 1.824(5) . ? F11 C11 1.332(7) . ? F21 C11 1.333(7) . ? F31 C11 1.333(7) . ? S12 O12 1.417(7) . ? S12 O22 1.453(9) . ? S12 O32 1.473(10) . ? S12 C12 1.826(15) . ? F12 C12 1.267(17) . ? F22 C12 1.317(16) . ? F32 C12 1.391(14) . ? S13 O23 1.449(8) . ? S13 O13 1.448(9) . ? S13 O33 1.449(8) . ? S13 C13 1.822(7) . ? F13 C13 1.334(9) . ? F23 C13 1.336(10) . ? F33 C13 1.333(11) . ? S14 O14 1.416(7) . ? S14 O34 1.438(8) . ? S14 O24 1.471(10) . ? S14 C14 1.706(17) . ? F14 C14 1.44(2) . ? F24 C14 1.308(15) . ? F34 C14 1.351(13) . ? S15 O15 1.420(7) . ? S15 O35 1.430(8) . ? S15 O25 1.442(7) . ? S15 C15 1.808(11) . ? F15 C15 1.326(13) . ? F25 C15 1.310(14) . ? F35 C15 1.340(13) . ? S16 O16 1.362(9) . ? S16 O26 1.414(9) . ? S16 O36 1.462(8) . ? S16 C16 1.832(15) . ? F16 C16 1.315(15) . ? F26 C16 1.328(14) . ? F36 C16 1.340(13) . ? S17 O27 1.449(9) . ? S17 O17 1.447(9) . ? S17 O37 1.451(9) . ? S17 C17 1.823(7) . ? F17 C17 1.335(12) . ? F27 C17 1.334(12) . ? F37 C17 1.333(11) . ? S18 O18 1.447(6) . ? S18 O28 1.450(8) . ? S18 O38 1.449(7) . ? S18 C18 1.822(7) . ? F18 C18 1.332(11) . ? F28 C18 1.334(11) . ? F38 C18 1.333(11) . ? 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 N12 Pd1 N11 85.7(3) . . ? N12 Pd1 P1 176.0(2) . . ? N11 Pd1 P1 90.7(2) . . ? N12 Pd1 P2 93.1(2) . . ? N11 Pd1 P2 178.8(2) . . ? P1 Pd1 P2 90.54(9) . . ? N11' Pd2 N12' 86.3(4) . . ? N11' Pd2 P4 177.5(3) . . ? N12' Pd2 P4 92.3(3) . . ? N11' Pd2 P3 91.4(3) . . ? N12' Pd2 P3 176.7(3) . . ? P4 Pd2 P3 89.97(12) . . ? C109 P1 C103 107.5(4) . . ? C109 P1 C100 105.3(4) . . ? C103 P1 C100 103.6(4) . . ? C109 P1 Pd1 112.3(3) . . ? C103 P1 Pd1 111.5(3) . . ? C100 P1 Pd1 115.9(3) . . ? C102 P2 C115 108.8(5) . . ? C102 P2 C121 100.8(5) . . ? C115 P2 C121 107.1(4) . . ? C102 P2 Pd1 115.4(3) . . ? C115 P2 Pd1 111.3(3) . . ? C121 P2 Pd1 112.8(3) . . ? C130 P3 C136 106.5(7) . . ? C130 P3 C127 104.7(6) . . ? C136 P3 C127 105.8(7) . . ? C130 P3 Pd2 110.2(5) . . ? C136 P3 Pd2 115.6(4) . . ? C127 P3 Pd2 113.3(4) . . ? C142 P4 C148 106.4(5) . . ? C142 P4 C129 107.2(6) . . ? C148 P4 C129 101.9(6) . . ? C142 P4 Pd2 113.5(5) . . ? C148 P4 Pd2 110.7(4) . . ? C129 P4 Pd2 116.2(4) . . ? C21 N11 C61 121.3(8) . . ? C21 N11 Pd1 118.5(6) . . ? C61 N11 Pd1 120.2(6) . . ? C81 N71 C31 123.7(8) . . ? C81 N71 H71 118.1 . . ? C31 N71 H71 118.1 . . ? C21' N11' C61' 117.4(10) . . ? C21' N11' Pd2 119.9(8) . . ? C61' N11' Pd2 122.6(7) . . ? C81 N71' C31' 125.2(9) . . ? C81 N71' H71' 117.4 . . ? C31' N71' H71' 117.4 . . ? N11 C21 C31 120.9(8) . . ? N11 C21 H21 119.5 . . ? C31 C21 H21 119.6 . . ? C21 C31 C41 118.9(8) . . ? C21 C31 N71 123.7(8) . . ? C41 C31 N71 117.4(8) . . ? C51 C41 C31 117.3(8) . . ? C51 C41 H41 121.3 . . ? C31 C41 H41 121.3 . . ? C61 C51 C41 121.4(9) . . ? C61 C51 H51 119.3 . . ? C41 C51 H51 119.3 . . ? C51 C61 N11 120.1(9) . . ? C51 C61 H61 120.0 . . ? N11 C61 H61 120.0 . . ? O81 C81 N71' 123.1(9) . . ? O81 C81 N71 123.9(9) . . ? N71' C81 N71 113.0(9) . . ? N11' C21' C31' 124.1(11) . . ? N11' C21' H21' 118.0 . . ? C31' C21' H21' 118.0 . . ? C21' C31' N71' 124.8(10) . . ? C21' C31' C41' 117.2(10) . . ? N71' C31' C41' 117.5(10) . . ? C51' C41' C31' 119.9(11) . . ? C51' C41' H41' 120.1 . . ? C31' C41' H41' 120.1 . . ? C61' C51' C41' 118.0(12) . . ? C61' C51' H51' 121.0 . . ? C41' C51' H51' 121.0 . . ? N11' C61' C51' 123.0(10) . . ? N11' C61' H61' 118.5 . . ? C51' C61' H61' 118.5 . . ? C62 N12 C22 120.0(8) . . ? C62 N12 Pd1 122.7(6) . . ? C22 N12 Pd1 117.2(6) . . ? C82 N72 C32 125.8(8) . . ? C82 N72 H72 117.1 . . ? C32 N72 H72 117.1 . . ? C62' N12' C22' 119.2(10) . . ? C62' N12' Pd2 122.4(8) . . ? C22' N12' Pd2 118.1(7) . . ? C82 N72' C32' 128.1(9) . . ? C82 N72' H72' 115.9 . . ? C32' N72' H72' 115.9 . . ? N12 C22 C32 121.2(8) . . ? N12 C22 H22 119.4 . . ? C32 C22 H22 119.4 . . ? C22 C32 C42 118.7(9) . . ? C22 C32 N72 123.2(9) . . ? C42 C32 N72 117.9(8) . . ? C32 C42 C52 118.6(9) . . ? C32 C42 H42 120.7 . . ? C52 C42 H42 120.7 . . ? C62 C52 C42 118.9(9) . . ? C62 C52 H52 120.5 . . ? C42 C52 H52 120.5 . . ? N12 C62 C52 122.5(9) . . ? N12 C62 H62 118.8 . . ? C52 C62 H62 118.8 . . ? O82 C82 N72 124.3(10) . . ? O82 C82 N72' 122.8(10) . . ? N72 C82 N72' 112.8(9) . . ? N12' C22' C32' 122.0(10) . . ? N12' C22' H22' 119.0 . . ? C32' C22' H22' 119.0 . . ? N72' C32' C22' 123.4(9) . . ? N72' C32' C42' 120.5(10) . . ? C22' C32' C42' 115.9(11) . . ? C52' C42' C32' 119.6(11) . . ? C52' C42' H42' 120.2 . . ? C32' C42' H42' 120.2 . . ? C62' C52' C42' 120.9(10) . . ? C62' C52' H52' 119.5 . . ? C42' C52' H52' 119.5 . . ? N12' C62' C52' 122.2(11) . . ? N12' C62' H62' 118.9 . . ? C52' C62' H62' 118.9 . . ? C101 C100 P1 113.9(7) . . ? C101 C100 H10A 108.8 . . ? P1 C100 H10A 108.8 . . ? C101 C100 H10B 108.8 . . ? P1 C100 H10B 108.8 . . ? H10A C100 H10B 107.7 . . ? C102 C101 C100 115.3(8) . . ? C102 C101 H10C 108.4 . . ? C100 C101 H10C 108.4 . . ? C102 C101 H10D 108.4 . . ? C100 C101 H10D 108.4 . . ? H10C C101 H10D 107.5 . . ? C101 C102 P2 116.2(7) . . ? C101 C102 H10E 108.2 . . ? P2 C102 H10E 108.2 . . ? C101 C102 H10F 108.2 . . ? P2 C102 H10F 108.2 . . ? H10E C102 H10F 107.4 . . ? C104 C103 C108 119.9(9) . . ? C104 C103 P1 120.9(7) . . ? C108 C103 P1 118.7(7) . . ? C103 C104 C105 119.0(10) . . ? C103 C104 H104 120.5 . . ? C105 C104 H104 120.5 . . ? C106 C105 C104 120.7(10) . . ? C106 C105 H105 119.7 . . ? C104 C105 H105 119.7 . . ? C105 C106 C107 119.6(10) . . ? C105 C106 H106 120.2 . . ? C107 C106 H106 120.2 . . ? C106 C107 C108 120.9(10) . . ? C106 C107 H107 119.6 . . ? C108 C107 H107 119.6 . . ? C107 C108 C103 119.9(10) . . ? C107 C108 H108 120.1 . . ? C103 C108 H108 120.1 . . ? C110 C109 C114 119.7(9) . . ? C110 C109 P1 121.7(8) . . ? C114 C109 P1 118.5(7) . . ? C109 C110 C111 120.1(11) . . ? C109 C110 H110 119.9 . . ? C111 C110 H110 119.9 . . ? C112 C111 C110 119.1(12) . . ? C112 C111 H111 120.4 . . ? C110 C111 H111 120.4 . . ? C113 C112 C111 119.8(11) . . ? C113 C112 H112 120.1 . . ? C111 C112 H112 120.1 . . ? C112 C113 C114 122.8(11) . . ? C112 C113 H113 118.6 . . ? C114 C113 H113 118.6 . . ? C113 C114 C109 118.3(10) . . ? C113 C114 H114 120.8 . . ? C109 C114 H114 120.8 . . ? C120 C115 C116 119.1(11) . . ? C120 C115 P2 121.3(8) . . ? C116 C115 P2 119.5(9) . . ? C115 C116 C117 119.7(14) . . ? C115 C116 H116 120.2 . . ? C117 C116 H116 120.2 . . ? C116 C117 C118 120.3(13) . . ? C116 C117 H117 119.9 . . ? C118 C117 H117 119.9 . . ? C119 C118 C117 118.6(12) . . ? C119 C118 H118 120.7 . . ? C117 C118 H118 120.7 . . ? C118 C119 C120 118.2(12) . . ? C118 C119 H119 120.9 . . ? C120 C119 H119 120.9 . . ? C115 C120 C119 124.0(10) . . ? C115 C120 H120 118.0 . . ? C119 C120 H120 118.0 . . ? C126 C121 C122 120.7(9) . . ? C126 C121 P2 119.0(7) . . ? C122 C121 P2 120.1(7) . . ? C123 C122 C121 117.6(10) . . ? C123 C122 H122 121.2 . . ? C121 C122 H122 121.2 . . ? C124 C123 C122 121.8(10) . . ? C124 C123 H123 119.1 . . ? C122 C123 H123 119.1 . . ? C125 C124 C123 119.6(10) . . ? C125 C124 H124 120.2 . . ? C123 C124 H124 120.2 . . ? C124 C125 C126 119.8(11) . . ? C124 C125 H125 120.1 . . ? C126 C125 H125 120.1 . . ? C121 C126 C125 120.5(10) . . ? C121 C126 H126 119.7 . . ? C125 C126 H126 119.7 . . ? C128 C127 P3 112.2(8) . . ? C128 C127 H12A 109.2 . . ? P3 C127 H12A 109.2 . . ? C128 C127 H12B 109.2 . . ? P3 C127 H12B 109.2 . . ? H12A C127 H12B 107.9 . . ? C129 C128 C127 110.5(10) . . ? C129 C128 H12C 109.6 . . ? C127 C128 H12C 109.6 . . ? C129 C128 H12D 109.6 . . ? C127 C128 H12D 109.6 . . ? H12C C128 H12D 108.1 . . ? C128 C129 P4 114.7(9) . . ? C128 C129 H12E 108.6 . . ? P4 C129 H12E 108.6 . . ? C128 C129 H12F 108.6 . . ? P4 C129 H12F 108.6 . . ? H12E C129 H12F 107.6 . . ? C135 C130 C131 118.6(12) . . ? C135 C130 P3 120.5(11) . . ? C131 C130 P3 120.8(9) . . ? C132 C131 C130 120.9(12) . . ? C132 C131 H131 119.6 . . ? C130 C131 H131 119.6 . . ? C133 C132 C131 120.7(14) . . ? C133 C132 H132 119.6 . . ? C131 C132 H132 119.6 . . ? C132 C133 C134 120.5(14) . . ? C132 C133 H133 119.7 . . ? C134 C133 H133 119.7 . . ? C133 C134 C135 123.5(13) . . ? C133 C134 H134 118.3 . . ? C135 C134 H134 118.3 . . ? C134 C135 C130 115.7(13) . . ? C134 C135 H135 122.1 . . ? C130 C135 H135 122.1 . . ? C137 C136 C141 122.5(11) . . ? C137 C136 P3 118.7(9) . . ? C141 C136 P3 118.7(10) . . ? C138 C137 C136 118.6(12) . . ? C138 C137 H137 120.7 . . ? C136 C137 H137 120.7 . . ? C139 C138 C137 121.3(13) . . ? C139 C138 H138 119.3 . . ? C137 C138 H138 119.3 . . ? C138 C139 C140 117.9(14) . . ? C138 C139 H139 121.0 . . ? C140 C139 H139 121.0 . . ? C139 C140 C141 122.3(15) . . ? C139 C140 H140 118.9 . . ? C141 C140 H140 118.9 . . ? C136 C141 C140 117.4(14) . . ? C136 C141 H141 121.3 . . ? C140 C141 H141 121.3 . . ? C143 C142 C147 117.4(12) . . ? C143 C142 P4 119.3(9) . . ? C147 C142 P4 123.3(11) . . ? C142 C143 C144 120.2(13) . . ? C142 C143 H143 119.9 . . ? C144 C143 H143 119.9 . . ? C145 C144 C143 120.6(15) . . ? C145 C144 H144 119.7 . . ? C143 C144 H144 119.7 . . ? C144 C145 C146 120.7(14) . . ? C144 C145 H145 119.6 . . ? C146 C145 H145 119.6 . . ? C147 C146 C145 120.0(14) . . ? C147 C146 H146 120.0 . . ? C145 C146 H146 120.0 . . ? C146 C147 C142 120.9(15) . . ? C146 C147 H147 119.6 . . ? C142 C147 H147 119.6 . . ? C149 C148 C153 118.0(12) . . ? C149 C148 P4 121.1(9) . . ? C153 C148 P4 120.9(9) . . ? C150 C149 C148 121.4(12) . . ? C150 C149 H149 119.3 . . ? C148 C149 H149 119.3 . . ? C149 C150 C151 122.0(13) . . ? C149 C150 H150 119.0 . . ? C151 C150 H150 119.0 . . ? C150 C151 C152 115.5(12) . . ? C150 C151 H151 122.2 . . ? C152 C151 H151 122.2 . . ? C153 C152 C151 123.6(12) . . ? C153 C152 H152 118.2 . . ? C151 C152 H152 118.2 . . ? C152 C153 C148 119.2(11) . . ? C152 C153 H153 120.4 . . ? C148 C153 H153 120.4 . . ? N14 Pd3 N13 85.7(3) . . ? N14 Pd3 P5 177.5(2) . . ? N13 Pd3 P5 92.3(2) . . ? N14 Pd3 P6 91.6(2) . . ? N13 Pd3 P6 176.9(2) . . ? P5 Pd3 P6 90.49(9) . . ? N13' Pd4 N14' 86.2(4) . . ? N13' Pd4 P7 92.4(3) . . ? N14' Pd4 P7 175.7(3) . . ? N13' Pd4 P8 177.3(3) . . ? N14' Pd4 P8 91.6(3) . . ? P7 Pd4 P8 89.62(13) . . ? C163 P5 C154 107.7(5) . . ? C163 P5 C157 107.0(5) . . ? C154 P5 C157 102.5(5) . . ? C163 P5 Pd3 111.4(3) . . ? C154 P5 Pd3 114.9(3) . . ? C157 P5 Pd3 112.7(3) . . ? C156 P6 C169 105.9(5) . . ? C156 P6 C175 103.6(5) . . ? C169 P6 C175 105.7(5) . . ? C156 P6 Pd3 115.8(4) . . ? C169 P6 Pd3 114.2(4) . . ? C175 P6 Pd3 110.6(3) . . ? C184 P7 C190 107.0(6) . . ? C184 P7 C181 102.5(6) . . ? C190 P7 C181 106.9(6) . . ? C184 P7 Pd4 111.2(4) . . ? C190 P7 Pd4 113.6(5) . . ? C181 P7 Pd4 114.9(5) . . ? C183 P8 C196 106.2(6) . . ? C183 P8 C202 104.6(6) . . ? C196 P8 C202 106.3(6) . . ? C183 P8 Pd4 114.0(5) . . ? C196 P8 Pd4 114.0(5) . . ? C202 P8 Pd4 111.0(4) . . ? C63 N13 C23 119.6(9) . . ? C63 N13 Pd3 121.0(7) . . ? C23 N13 Pd3 119.0(6) . . ? C83 N73 C33 126.5(10) . . ? C83 N73 H73 116.7 . . ? C33 N73 H73 116.7 . . ? C23' N13' C63' 119.4(11) . . ? C23' N13' Pd4 118.0(7) . . ? C63' N13' Pd4 122.6(9) . . ? C83 N73' C33' 126.6(10) . . ? C83 N73' H73' 116.7 . . ? C33' N73' H73' 116.7 . . ? N13 C23 C33 123.8(9) . . ? N13 C23 H23 118.1 . . ? C33 C23 H23 118.1 . . ? C23 C33 N73 125.2(10) . . ? C23 C33 C43 116.1(10) . . ? N73 C33 C43 118.7(9) . . ? C53 C43 C33 118.8(10) . . ? C53 C43 H43 120.6 . . ? C33 C43 H43 120.6 . . ? C43 C53 C63 121.4(11) . . ? C43 C53 H53 119.3 . . ? C63 C53 H53 119.3 . . ? N13 C63 C53 120.3(10) . . ? N13 C63 H63 119.9 . . ? C53 C63 H63 119.9 . . ? O83 C83 N73 122.6(12) . . ? O83 C83 N73' 124.2(12) . . ? N73 C83 N73' 113.2(10) . . ? N13' C23' C33' 120.7(11) . . ? N13' C23' H23' 119.6 . . ? C33' C23' H23' 119.6 . . ? C43' C33' C23' 118.2(13) . . ? C43' C33' N73' 119.0(12) . . ? C23' C33' N73' 122.7(10) . . ? C33' C43' C53' 120.8(13) . . ? C33' C43' H43' 119.6 . . ? C53' C43' H43' 119.6 . . ? C63' C53' C43' 120.2(13) . . ? C63' C53' H53' 119.9 . . ? C43' C53' H53' 119.9 . . ? C53' C63' N13' 120.6(13) . . ? C53' C63' H63' 119.7 . . ? N13' C63' H63' 119.7 . . ? C24 N14 C64 119.5(8) . . ? C24 N14 Pd3 119.8(6) . . ? C64 N14 Pd3 120.6(6) . . ? C84 N74 C34 123.8(8) . . ? C84 N74 H74 118.1 . . ? C34 N74 H74 118.1 . . ? C24' N14' C64' 122.4(10) . . ? C24' N14' Pd4 117.5(7) . . ? C64' N14' Pd4 120.0(7) . . ? C84 N74' C34' 123.5(8) . . ? C84 N74' H74' 118.2 . . ? C34' N74' H74' 118.2 . . ? N14 C24 C34 121.5(8) . . ? N14 C24 H24 119.2 . . ? C34 C24 H24 119.2 . . ? C44 C34 C24 118.8(9) . . ? C44 C34 N74 119.2(8) . . ? C24 C34 N74 122.0(8) . . ? C34 C44 C54 118.8(8) . . ? C34 C44 H44 120.6 . . ? C54 C44 H44 120.6 . . ? C64 C54 C44 120.7(9) . . ? C64 C54 H54 119.6 . . ? C44 C54 H54 119.6 . . ? C54 C64 N14 120.6(9) . . ? C54 C64 H64 119.7 . . ? N14 C64 H64 119.7 . . ? O84 C84 N74 125.3(9) . . ? O84 C84 N74' 123.7(9) . . ? N74 C84 N74' 111.0(8) . . ? N14' C24' C34' 119.7(10) . . ? N14' C24' H24' 120.1 . . ? C34' C24' H24' 120.1 . . ? C24' C34' C44' 118.3(9) . . ? C24' C34' N74' 123.7(9) . . ? C44' C34' N74' 117.9(10) . . ? C54' C44' C34' 120.8(11) . . ? C54' C44' H44' 119.6 . . ? C34' C44' H44' 119.6 . . ? C44' C54' C64' 120.1(12) . . ? C44' C54' H54' 119.9 . . ? C64' C54' H54' 119.9 . . ? N14' C64' C54' 118.6(10) . . ? N14' C64' H64' 120.7 . . ? C54' C64' H64' 120.7 . . ? C155 C154 P5 113.9(7) . . ? C155 C154 H15A 108.8 . . ? P5 C154 H15A 108.8 . . ? C155 C154 H15B 108.8 . . ? P5 C154 H15B 108.8 . . ? H15A C154 H15B 107.7 . . ? C156 C155 C154 111.8(9) . . ? C156 C155 H15C 109.3 . . ? C154 C155 H15C 109.3 . . ? C156 C155 H15D 109.3 . . ? C154 C155 H15D 109.3 . . ? H15C C155 H15D 107.9 . . ? C155 C156 P6 114.0(7) . . ? C155 C156 H15E 108.8 . . ? P6 C156 H15E 108.8 . . ? C155 C156 H15F 108.8 . . ? P6 C156 H15F 108.8 . . ? H15E C156 H15F 107.6 . . ? C162 C157 C158 118.5(10) . . ? C162 C157 P5 121.3(8) . . ? C158 C157 P5 120.1(8) . . ? C159 C158 C157 119.2(11) . . ? C159 C158 H158 120.4 . . ? C157 C158 H158 120.4 . . ? C158 C159 C160 122.6(12) . . ? C158 C159 H159 118.7 . . ? C160 C159 H159 118.7 . . ? C161 C160 C159 117.6(10) . . ? C161 C160 H160 121.2 . . ? C159 C160 H160 121.2 . . ? C160 C161 C162 122.5(11) . . ? C160 C161 H161 118.8 . . ? C162 C161 H161 118.8 . . ? C157 C162 C161 119.5(10) . . ? C157 C162 H162 120.2 . . ? C161 C162 H162 120.2 . . ? C164 C163 C168 116.0(10) . . ? C164 C163 P5 124.4(8) . . ? C168 C163 P5 119.3(7) . . ? C165 C164 C163 123.6(11) . . ? C165 C164 H164 118.2 . . ? C163 C164 H164 118.2 . . ? C166 C165 C164 119.4(11) . . ? C166 C165 H165 120.3 . . ? C164 C165 H165 120.3 . . ? C165 C166 C167 120.3(11) . . ? C165 C166 H166 119.8 . . ? C167 C166 H166 119.8 . . ? C166 C167 C168 119.9(10) . . ? C166 C167 H167 120.1 . . ? C168 C167 H167 120.1 . . ? C163 C168 C167 120.4(10) . . ? C163 C168 H168 119.8 . . ? C167 C168 H168 119.8 . . ? C174 C169 C170 117.7(10) . . ? C174 C169 P6 122.9(9) . . ? C170 C169 P6 119.3(8) . . ? C171 C170 C169 120.2(12) . . ? C171 C170 H170 119.9 . . ? C169 C170 H170 119.9 . . ? C172 C171 C170 122.8(13) . . ? C172 C171 H171 118.6 . . ? C170 C171 H171 118.6 . . ? C171 C172 C173 118.5(13) . . ? C171 C172 H172 120.7 . . ? C173 C172 H172 120.7 . . ? C174 C173 C172 120.2(13) . . ? C174 C173 H173 119.9 . . ? C172 C173 H173 119.9 . . ? C173 C174 C169 120.5(13) . . ? C173 C174 H174 119.7 . . ? C169 C174 H174 119.7 . . ? C180 C175 C176 120.0(11) . . ? C180 C175 P6 119.2(9) . . ? C176 C175 P6 120.6(9) . . ? C177 C176 C175 119.2(13) . . ? C177 C176 H176 120.4 . . ? C175 C176 H176 120.4 . . ? C176 C177 C178 121.4(13) . . ? C176 C177 H177 119.3 . . ? C178 C177 H177 119.3 . . ? C179 C178 C177 119.7(12) . . ? C179 C178 H178 120.2 . . ? C177 C178 H178 120.2 . . ? C178 C179 C180 121.0(14) . . ? C178 C179 H179 119.5 . . ? C180 C179 H179 119.5 . . ? C175 C180 C179 118.7(13) . . ? C175 C180 H180 120.7 . . ? C179 C180 H180 120.7 . . ? C182 C181 P7 115.8(10) . . ? C182 C181 H18A 108.3 . . ? P7 C181 H18A 108.3 . . ? C182 C181 H18B 108.3 . . ? P7 C181 H18B 108.3 . . ? H18A C181 H18B 107.4 . . ? C181 C182 C183 113.4(10) . . ? C181 C182 H18C 108.9 . . ? C183 C182 H18C 108.9 . . ? C181 C182 H18D 108.9 . . ? C183 C182 H18D 108.9 . . ? H18C C182 H18D 107.7 . . ? C182 C183 P8 112.1(9) . . ? C182 C183 H18E 109.2 . . ? P8 C183 H18E 109.2 . . ? C182 C183 H18F 109.2 . . ? P8 C183 H18F 109.2 . . ? H18E C183 H18F 107.9 . . ? C185 C184 C189 117.3(12) . . ? C185 C184 P7 123.3(10) . . ? C189 C184 P7 119.4(9) . . ? C184 C185 C186 120.9(12) . . ? C184 C185 H185 119.5 . . ? C186 C185 H185 119.5 . . ? C187 C186 C185 120.5(12) . . ? C187 C186 H186 119.7 . . ? C185 C186 H186 119.7 . . ? C186 C187 C188 121.0(13) . . ? C186 C187 H187 119.5 . . ? C188 C187 H187 119.5 . . ? C189 C188 C187 119.1(13) . . ? C189 C188 H188 120.4 . . ? C187 C188 H188 120.4 . . ? C188 C189 C184 120.9(12) . . ? C188 C189 H189 119.5 . . ? C184 C189 H189 119.5 . . ? C191 C190 C195 116.9(13) . . ? C191 C190 P7 122.3(11) . . ? C195 C190 P7 120.8(12) . . ? C192 C191 C190 123.3(16) . . ? C192 C191 H191 118.4 . . ? C190 C191 H191 118.4 . . ? C191 C192 C193 119.9(18) . . ? C191 C192 H192 120.0 . . ? C193 C192 H192 120.0 . . ? C194 C193 C192 120.1(16) . . ? C194 C193 H193 120.0 . . ? C192 C193 H193 120.0 . . ? C193 C194 C195 122.1(18) . . ? C193 C194 H194 119.0 . . ? C195 C194 H194 119.0 . . ? C194 C195 C190 117.7(17) . . ? C194 C195 H195 121.2 . . ? C190 C195 H195 121.2 . . ? C201 C196 C197 121.2(13) . . ? C201 C196 P8 120.0(11) . . ? C197 C196 P8 118.6(11) . . ? C196 C197 C198 117.5(15) . . ? C196 C197 H197 121.3 . . ? C198 C197 H197 121.3 . . ? C199 C198 C197 118.0(16) . . ? C199 C198 H198 121.0 . . ? C197 C198 H198 121.0 . . ? C200 C199 C198 121.5(16) . . ? C200 C199 H199 119.3 . . ? C198 C199 H199 119.3 . . ? C199 C200 C201 121.4(15) . . ? C199 C200 H200 119.3 . . ? C201 C200 H200 119.3 . . ? C196 C201 C200 119.6(14) . . ? C196 C201 H201 120.2 . . ? C200 C201 H201 120.2 . . ? C207 C202 C203 121.7(13) . . ? C207 C202 P8 118.7(10) . . ? C203 C202 P8 119.5(11) . . ? C202 C203 C204 117.1(15) . . ? C202 C203 H203 121.4 . . ? C204 C203 H203 121.4 . . ? C205 C204 C203 121.0(15) . . ? C205 C204 H204 119.5 . . ? C203 C204 H204 119.5 . . ? C206 C205 C204 117.2(15) . . ? C206 C205 H205 121.4 . . ? C204 C205 H205 121.4 . . ? C205 C206 C207 125.7(16) . . ? C205 C206 H206 117.1 . . ? C207 C206 H206 117.1 . . ? C206 C207 C202 116.9(14) . . ? C206 C207 H207 121.6 . . ? C202 C207 H207 121.6 . . ? O31 S11 O11 115.7(3) . . ? O31 S11 O21 114.2(3) . . ? O11 S11 O21 114.0(3) . . ? O31 S11 C11 103.7(2) . . ? O11 S11 C11 104.0(2) . . ? O21 S11 C11 103.1(2) . . ? F21 C11 F11 108.2(3) . . ? F21 C11 F31 108.0(3) . . ? F11 C11 F31 109.0(3) . . ? F21 C11 S11 110.8(2) . . ? F11 C11 S11 109.9(3) . . ? F31 C11 S11 110.9(3) . . ? O12 S12 O22 115.6(6) . . ? O12 S12 O32 117.0(6) . . ? O22 S12 O32 113.1(6) . . ? O12 S12 C12 103.4(6) . . ? O22 S12 C12 105.5(6) . . ? O32 S12 C12 99.6(7) . . ? F12 C12 F22 110.8(14) . . ? F12 C12 F32 109.2(11) . . ? F22 C12 F32 105.9(11) . . ? F12 C12 S12 113.9(10) . . ? F22 C12 S12 109.5(10) . . ? F32 C12 S12 107.3(10) . . ? O23 S13 O13 115.4(3) . . ? O23 S13 O33 114.8(3) . . ? O13 S13 O33 115.2(3) . . ? O23 S13 C13 102.9(2) . . ? O13 S13 C13 102.8(5) . . ? O33 S13 C13 103.1(5) . . ? F23 C13 F13 108.9(3) . . ? F23 C13 F33 107.9(7) . . ? F13 C13 F33 107.3(7) . . ? F23 C13 S13 110.8(3) . . ? F13 C13 S13 110.7(3) . . ? F33 C13 S13 111.2(3) . . ? O14 S14 O34 118.7(5) . . ? O14 S14 O24 113.1(6) . . ? O34 S14 O24 111.1(6) . . ? O14 S14 C14 108.1(6) . . ? O34 S14 C14 107.8(6) . . ? O24 S14 C14 95.2(8) . . ? F24 C14 F34 105.6(11) . . ? F24 C14 F14 105.8(13) . . ? F34 C14 F14 104.7(13) . . ? F24 C14 S14 116.5(12) . . ? F34 C14 S14 114.7(11) . . ? F14 C14 S14 108.7(10) . . ? O15 S15 O35 114.0(5) . . ? O15 S15 O25 115.9(5) . . ? O35 S15 O25 114.7(5) . . ? O15 S15 C15 103.8(5) . . ? O35 S15 C15 104.3(6) . . ? O25 S15 C15 101.8(5) . . ? F25 C15 F15 108.2(10) . . ? F25 C15 F35 106.8(10) . . ? F15 C15 F35 105.4(10) . . ? F25 C15 S15 112.1(9) . . ? F15 C15 S15 112.7(8) . . ? F35 C15 S15 111.2(8) . . ? O16 S16 O26 118.0(7) . . ? O16 S16 O36 112.6(6) . . ? O26 S16 O36 112.1(6) . . ? O16 S16 C16 103.2(6) . . ? O26 S16 C16 103.6(6) . . ? O36 S16 C16 105.7(6) . . ? F16 C16 F36 106.8(11) . . ? F16 C16 F26 108.8(12) . . ? F36 C16 F26 106.0(10) . . ? F16 C16 S16 112.4(9) . . ? F36 C16 S16 111.2(10) . . ? F26 C16 S16 111.4(9) . . ? O27 S17 O17 116.2(3) . . ? O27 S17 O37 114.3(3) . . ? O17 S17 O37 114.8(3) . . ? O27 S17 C17 103.0(5) . . ? O17 S17 C17 103.2(2) . . ? O37 S17 C17 102.7(5) . . ? F17 C17 F27 108.1(7) . . ? F17 C17 F37 108.7(4) . . ? F27 C17 F37 107.5(7) . . ? F17 C17 S17 110.2(3) . . ? F27 C17 S17 111.0(3) . . ? F37 C17 S17 111.2(3) . . ? O18 S18 O28 115.7(3) . . ? O18 S18 O38 114.1(3) . . ? O28 S18 O38 115.0(3) . . ? O18 S18 C18 103.6(2) . . ? O28 S18 C18 102.9(2) . . ? O38 S18 C18 103.1(2) . . ? F28 C18 F38 108.2(7) . . ? F28 C18 F18 108.5(7) . . ? F38 C18 F18 107.8(7) . . ? F28 C18 S18 110.6(3) . . ? F38 C18 S18 110.6(3) . . ? F18 C18 S18 110.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Pd1 P1 C109 -99.8(4) . . . . ? P2 Pd1 P1 C109 80.4(3) . . . . ? N11 Pd1 P1 C103 21.0(4) . . . . ? P2 Pd1 P1 C103 -158.9(3) . . . . ? N11 Pd1 P1 C100 139.1(4) . . . . ? P2 Pd1 P1 C100 -40.7(4) . . . . ? N12 Pd1 P2 C102 -139.3(4) . . . . ? P1 Pd1 P2 C102 38.9(4) . . . . ? N12 Pd1 P2 C115 96.1(4) . . . . ? P1 Pd1 P2 C115 -85.6(4) . . . . ? N12 Pd1 P2 C121 -24.2(4) . . . . ? P1 Pd1 P2 C121 154.0(3) . . . . ? N11' Pd2 P3 C130 -15.0(5) . . . . ? P4 Pd2 P3 C130 162.9(4) . . . . ? N11' Pd2 P3 C136 105.7(7) . . . . ? P4 Pd2 P3 C136 -76.4(6) . . . . ? N11' Pd2 P3 C127 -131.9(5) . . . . ? P4 Pd2 P3 C127 46.0(4) . . . . ? N12' Pd2 P4 C142 -99.2(5) . . . . ? P3 Pd2 P4 C142 83.3(4) . . . . ? N12' Pd2 P4 C148 20.4(5) . . . . ? P3 Pd2 P4 C148 -157.2(4) . . . . ? N12' Pd2 P4 C129 135.9(6) . . . . ? P3 Pd2 P4 C129 -41.7(5) . . . . ? N12 Pd1 N11 C21 90.3(7) . . . . ? P1 Pd1 N11 C21 -87.9(6) . . . . ? N12 Pd1 N11 C61 -90.6(7) . . . . ? P1 Pd1 N11 C61 91.2(7) . . . . ? N12' Pd2 N11' C21' -86.1(8) . . . . ? P3 Pd2 N11' C21' 91.5(8) . . . . ? N12' Pd2 N11' C61' 96.8(9) . . . . ? P3 Pd2 N11' C61' -85.5(9) . . . . ? C61 N11 C21 C31 -0.1(13) . . . . ? Pd1 N11 C21 C31 179.0(6) . . . . ? N11 C21 C31 C41 -0.8(13) . . . . ? N11 C21 C31 N71 -179.5(8) . . . . ? C81 N71 C31 C21 -22.7(14) . . . . ? C81 N71 C31 C41 158.5(9) . . . . ? C21 C31 C41 C51 0.0(15) . . . . ? N71 C31 C41 C51 178.8(9) . . . . ? C31 C41 C51 C61 1.6(17) . . . . ? C41 C51 C61 N11 -2.5(16) . . . . ? C21 N11 C61 C51 1.7(14) . . . . ? Pd1 N11 C61 C51 -177.4(8) . . . . ? C31' N71' C81 O81 0.4(16) . . . . ? C31' N71' C81 N71 179.3(9) . . . . ? C31 N71 C81 O81 1.9(15) . . . . ? C31 N71 C81 N71' -177.0(8) . . . . ? C61' N11' C21' C31' 0.5(17) . . . . ? Pd2 N11' C21' C31' -176.7(9) . . . . ? N11' C21' C31' N71' 176.2(10) . . . . ? N11' C21' C31' C41' 4.5(17) . . . . ? C81 N71' C31' C21' 19.2(17) . . . . ? C81 N71' C31' C41' -169.0(10) . . . . ? C21' C31' C41' C51' -7.1(17) . . . . ? N71' C31' C41' C51' -179.5(10) . . . . ? C31' C41' C51' C61' 5.0(17) . . . . ? C21' N11' C61' C51' -2.9(17) . . . . ? Pd2 N11' C61' C51' 174.2(9) . . . . ? C41' C51' C61' N11' 0.2(18) . . . . ? N11 Pd1 N12 C62 88.1(7) . . . . ? P2 Pd1 N12 C62 -92.0(7) . . . . ? N11 Pd1 N12 C22 -88.2(6) . . . . ? P2 Pd1 N12 C22 91.7(6) . . . . ? N11' Pd2 N12' C62' -90.3(10) . . . . ? P4 Pd2 N12' C62' 91.8(9) . . . . ? N11' Pd2 N12' C22' 84.4(9) . . . . ? P4 Pd2 N12' C22' -93.6(9) . . . . ? C62 N12 C22 C32 1.6(13) . . . . ? Pd1 N12 C22 C32 177.9(7) . . . . ? N12 C22 C32 C42 -3.8(13) . . . . ? N12 C22 C32 N72 -178.2(8) . . . . ? C82 N72 C32 C22 7.1(15) . . . . ? C82 N72 C32 C42 -167.3(9) . . . . ? C22 C32 C42 C52 3.3(13) . . . . ? N72 C32 C42 C52 178.0(8) . . . . ? C32 C42 C52 C62 -0.8(14) . . . . ? C22 N12 C62 C52 1.1(14) . . . . ? Pd1 N12 C62 C52 -175.0(7) . . . . ? C42 C52 C62 N12 -1.5(15) . . . . ? C32 N72 C82 O82 -9.8(17) . . . . ? C32 N72 C82 N72' 167.4(9) . . . . ? C32' N72' C82 O82 -0.2(19) . . . . ? C32' N72' C82 N72 -177.4(11) . . . . ? C62' N12' C22' C32' -4.0(18) . . . . ? Pd2 N12' C22' C32' -178.9(9) . . . . ? C82 N72' C32' C22' 5(2) . . . . ? C82 N72' C32' C42' -178.6(11) . . . . ? N12' C22' C32' N72' 177.3(11) . . . . ? N12' C22' C32' C42' 0.7(18) . . . . ? N72' C32' C42' C52' -174.1(12) . . . . ? C22' C32' C42' C52' 2.6(18) . . . . ? C32' C42' C52' C62' -2.6(19) . . . . ? C22' N12' C62' C52' 4.1(18) . . . . ? Pd2 N12' C62' C52' 178.8(9) . . . . ? C42' C52' C62' N12' -0.8(19) . . . . ? C109 P1 C100 C101 -65.8(7) . . . . ? C103 P1 C100 C101 -178.6(7) . . . . ? Pd1 P1 C100 C101 59.0(7) . . . . ? P1 C100 C101 C102 -68.7(10) . . . . ? C100 C101 C102 P2 68.2(11) . . . . ? C115 P2 C102 C101 69.6(9) . . . . ? C121 P2 C102 C101 -178.1(8) . . . . ? Pd1 P2 C102 C101 -56.3(9) . . . . ? C109 P1 C103 C104 -154.5(8) . . . . ? C100 P1 C103 C104 -43.3(9) . . . . ? Pd1 P1 C103 C104 82.0(8) . . . . ? C109 P1 C103 C108 34.1(9) . . . . ? C100 P1 C103 C108 145.3(8) . . . . ? Pd1 P1 C103 C108 -89.4(8) . . . . ? C108 C103 C104 C105 -0.6(15) . . . . ? P1 C103 C104 C105 -171.9(8) . . . . ? C103 C104 C105 C106 2.9(16) . . . . ? C104 C105 C106 C107 -3.6(17) . . . . ? C105 C106 C107 C108 2.1(18) . . . . ? C106 C107 C108 C103 0.1(17) . . . . ? C104 C103 C108 C107 -0.8(15) . . . . ? P1 C103 C108 C107 170.7(8) . . . . ? C103 P1 C109 C110 72.3(9) . . . . ? C100 P1 C109 C110 -37.7(9) . . . . ? Pd1 P1 C109 C110 -164.7(7) . . . . ? C103 P1 C109 C114 -110.3(8) . . . . ? C100 P1 C109 C114 139.7(8) . . . . ? Pd1 P1 C109 C114 12.7(8) . . . . ? C114 C109 C110 C111 -2.4(15) . . . . ? P1 C109 C110 C111 175.0(9) . . . . ? C109 C110 C111 C112 0.5(17) . . . . ? C110 C111 C112 C113 0.1(19) . . . . ? C111 C112 C113 C114 1(2) . . . . ? C112 C113 C114 C109 -3.3(17) . . . . ? C110 C109 C114 C113 3.7(15) . . . . ? P1 C109 C114 C113 -173.8(8) . . . . ? C102 P2 C115 C120 -160.8(8) . . . . ? C121 P2 C115 C120 91.1(9) . . . . ? Pd1 P2 C115 C120 -32.5(10) . . . . ? C102 P2 C115 C116 22.7(12) . . . . ? C121 P2 C115 C116 -85.4(11) . . . . ? Pd1 P2 C115 C116 151.0(10) . . . . ? C120 C115 C116 C117 -1(2) . . . . ? P2 C115 C116 C117 175.4(13) . . . . ? C115 C116 C117 C118 4(3) . . . . ? C116 C117 C118 C119 -5(3) . . . . ? C117 C118 C119 C120 2(2) . . . . ? C116 C115 C120 C119 -1.2(18) . . . . ? P2 C115 C120 C119 -177.7(8) . . . . ? C118 C119 C120 C115 0.5(18) . . . . ? C102 P2 C121 C126 60.6(9) . . . . ? C115 P2 C121 C126 174.2(8) . . . . ? Pd1 P2 C121 C126 -63.1(9) . . . . ? C102 P2 C121 C122 -115.3(8) . . . . ? C115 P2 C121 C122 -1.7(9) . . . . ? Pd1 P2 C121 C122 121.1(7) . . . . ? C126 C121 C122 C123 0.4(15) . . . . ? P2 C121 C122 C123 176.3(8) . . . . ? C121 C122 C123 C124 0.2(15) . . . . ? C122 C123 C124 C125 0.2(16) . . . . ? C123 C124 C125 C126 -1.3(17) . . . . ? C122 C121 C126 C125 -1.5(16) . . . . ? P2 C121 C126 C125 -177.4(8) . . . . ? C124 C125 C126 C121 2.0(17) . . . . ? C130 P3 C127 C128 171.9(9) . . . . ? C136 P3 C127 C128 59.5(10) . . . . ? Pd2 P3 C127 C128 -68.1(9) . . . . ? P3 C127 C128 C129 74.9(13) . . . . ? C127 C128 C129 P4 -69.1(12) . . . . ? C142 P4 C129 C128 -70.0(10) . . . . ? C148 P4 C129 C128 178.5(8) . . . . ? Pd2 P4 C129 C128 58.1(10) . . . . ? C136 P3 C130 C135 149.4(13) . . . . ? C127 P3 C130 C135 37.6(14) . . . . ? Pd2 P3 C130 C135 -84.5(13) . . . . ? C136 P3 C130 C131 -33.9(13) . . . . ? C127 P3 C130 C131 -145.7(11) . . . . ? Pd2 P3 C130 C131 92.2(11) . . . . ? C135 C130 C131 C132 2(2) . . . . ? P3 C130 C131 C132 -175.1(11) . . . . ? C130 C131 C132 C133 0(2) . . . . ? C131 C132 C133 C134 -2(2) . . . . ? C132 C133 C134 C135 4(3) . . . . ? C133 C134 C135 C130 -2(3) . . . . ? C131 C130 C135 C134 0(2) . . . . ? P3 C130 C135 C134 176.4(13) . . . . ? C130 P3 C136 C137 110.1(13) . . . . ? C127 P3 C136 C137 -138.8(12) . . . . ? Pd2 P3 C136 C137 -12.6(15) . . . . ? C130 P3 C136 C141 -73.2(15) . . . . ? C127 P3 C136 C141 37.9(15) . . . . ? Pd2 P3 C136 C141 164.1(11) . . . . ? C141 C136 C137 C138 2(2) . . . . ? P3 C136 C137 C138 178.5(12) . . . . ? C136 C137 C138 C139 -1(2) . . . . ? C137 C138 C139 C140 1(3) . . . . ? C138 C139 C140 C141 -1(3) . . . . ? C137 C136 C141 C140 -2(2) . . . . ? P3 C136 C141 C140 -178.8(12) . . . . ? C139 C140 C141 C136 2(3) . . . . ? C148 P4 C142 C143 -85.7(12) . . . . ? C129 P4 C142 C143 165.9(11) . . . . ? Pd2 P4 C142 C143 36.3(12) . . . . ? C148 P4 C142 C147 94.4(12) . . . . ? C129 P4 C142 C147 -14.0(14) . . . . ? Pd2 P4 C142 C147 -143.6(11) . . . . ? C147 C142 C143 C144 -1(2) . . . . ? P4 C142 C143 C144 179.3(11) . . . . ? C142 C143 C144 C145 2(2) . . . . ? C143 C144 C145 C146 -4(3) . . . . ? C144 C145 C146 C147 4(3) . . . . ? C145 C146 C147 C142 -3(3) . . . . ? C143 C142 C147 C146 1(2) . . . . ? P4 C142 C147 C146 -178.9(13) . . . . ? C142 P4 C148 C149 -159.4(11) . . . . ? C129 P4 C148 C149 -47.3(12) . . . . ? Pd2 P4 C148 C149 76.8(11) . . . . ? C142 P4 C148 C153 20.1(12) . . . . ? C129 P4 C148 C153 132.2(10) . . . . ? Pd2 P4 C148 C153 -103.7(10) . . . . ? C153 C148 C149 C150 3(2) . . . . ? P4 C148 C149 C150 -177.9(12) . . . . ? C148 C149 C150 C151 0(3) . . . . ? C149 C150 C151 C152 1(2) . . . . ? C150 C151 C152 C153 -3(2) . . . . ? C151 C152 C153 C148 6(2) . . . . ? C149 C148 C153 C152 -5.1(19) . . . . ? P4 C148 C153 C152 175.5(11) . . . . ? N13 Pd3 P5 C163 -99.0(4) . . . . ? P6 Pd3 P5 C163 82.4(4) . . . . ? N13 Pd3 P5 C154 138.2(5) . . . . ? P6 Pd3 P5 C154 -40.4(4) . . . . ? N13 Pd3 P5 C157 21.2(4) . . . . ? P6 Pd3 P5 C157 -157.3(4) . . . . ? N14 Pd3 P6 C156 -141.6(4) . . . . ? P5 Pd3 P6 C156 39.7(4) . . . . ? N14 Pd3 P6 C169 94.9(4) . . . . ? P5 Pd3 P6 C169 -83.8(4) . . . . ? N14 Pd3 P6 C175 -24.1(4) . . . . ? P5 Pd3 P6 C175 157.2(4) . . . . ? N13' Pd4 P7 C184 -21.0(5) . . . . ? P8 Pd4 P7 C184 157.2(4) . . . . ? N13' Pd4 P7 C190 99.7(6) . . . . ? P8 Pd4 P7 C190 -82.1(5) . . . . ? N13' Pd4 P7 C181 -136.7(5) . . . . ? P8 Pd4 P7 C181 41.5(5) . . . . ? N14' Pd4 P8 C183 130.4(5) . . . . ? P7 Pd4 P8 C183 -45.5(4) . . . . ? N14' Pd4 P8 C196 -107.4(5) . . . . ? P7 Pd4 P8 C196 76.7(5) . . . . ? N14' Pd4 P8 C202 12.5(5) . . . . ? P7 Pd4 P8 C202 -163.3(5) . . . . ? N14 Pd3 N13 C63 -85.7(7) . . . . ? P5 Pd3 N13 C63 93.0(7) . . . . ? N14 Pd3 N13 C23 87.1(7) . . . . ? P5 Pd3 N13 C23 -94.2(7) . . . . ? N14' Pd4 N13' C23' -86.2(9) . . . . ? P7 Pd4 N13' C23' 89.7(9) . . . . ? N14' Pd4 N13' C63' 92.8(9) . . . . ? P7 Pd4 N13' C63' -91.2(9) . . . . ? C63 N13 C23 C33 -0.4(15) . . . . ? Pd3 N13 C23 C33 -173.4(8) . . . . ? N13 C23 C33 N73 178.2(9) . . . . ? N13 C23 C33 C43 -1.3(15) . . . . ? C83 N73 C33 C23 -11.2(18) . . . . ? C83 N73 C33 C43 168.3(11) . . . . ? C23 C33 C43 C53 1.7(15) . . . . ? N73 C33 C43 C53 -177.8(10) . . . . ? C33 C43 C53 C63 -0.5(16) . . . . ? C23 N13 C63 C53 1.8(14) . . . . ? Pd3 N13 C63 C53 174.5(7) . . . . ? C43 C53 C63 N13 -1.3(16) . . . . ? C33 N73 C83 O83 11.9(18) . . . . ? C33 N73 C83 N73' -168.1(10) . . . . ? C33' N73' C83 O83 -6(2) . . . . ? C33' N73' C83 N73 174.3(11) . . . . ? C63' N13' C23' C33' 0.7(17) . . . . ? Pd4 N13' C23' C33' 179.8(9) . . . . ? N13' C23' C33' C43' 0.3(18) . . . . ? N13' C23' C33' N73' 179.5(11) . . . . ? C83 N73' C33' C43' -178.4(12) . . . . ? C83 N73' C33' C23' 2.4(19) . . . . ? C23' C33' C43' C53' -0.1(19) . . . . ? N73' C33' C43' C53' -179.3(12) . . . . ? C33' C43' C53' C63' -1(2) . . . . ? C43' C53' C63' N13' 2(2) . . . . ? C23' N13' C63' C53' -2.0(18) . . . . ? Pd4 N13' C63' C53' 179.0(10) . . . . ? N13 Pd3 N14 C24 -90.1(7) . . . . ? P6 Pd3 N14 C24 88.4(7) . . . . ? N13 Pd3 N14 C64 89.3(7) . . . . ? P6 Pd3 N14 C64 -92.2(7) . . . . ? N13' Pd4 N14' C24' 86.6(8) . . . . ? P8 Pd4 N14' C24' -91.7(8) . . . . ? N13' Pd4 N14' C64' -98.4(9) . . . . ? P8 Pd4 N14' C64' 83.3(9) . . . . ? C64 N14 C24 C34 2.3(13) . . . . ? Pd3 N14 C24 C34 -178.3(7) . . . . ? N14 C24 C34 C44 -2.1(14) . . . . ? N14 C24 C34 N74 178.0(8) . . . . ? C84 N74 C34 C44 -157.6(9) . . . . ? C84 N74 C34 C24 22.4(14) . . . . ? C24 C34 C44 C54 0.1(14) . . . . ? N74 C34 C44 C54 -180.0(8) . . . . ? C34 C44 C54 C64 1.6(15) . . . . ? C44 C54 C64 N14 -1.5(15) . . . . ? C24 N14 C64 C54 -0.5(14) . . . . ? Pd3 N14 C64 C54 -179.9(7) . . . . ? C34 N74 C84 O84 1.0(16) . . . . ? C34 N74 C84 N74' 179.6(8) . . . . ? C34' N74' C84 O84 0.5(16) . . . . ? C34' N74' C84 N74 -178.2(9) . . . . ? C64' N14' C24' C34' 3.5(16) . . . . ? Pd4 N14' C24' C34' 178.4(7) . . . . ? N14' C24' C34' C44' -3.6(15) . . . . ? N14' C24' C34' N74' -179.9(9) . . . . ? C84 N74' C34' C24' -19.4(15) . . . . ? C84 N74' C34' C44' 164.3(9) . . . . ? C24' C34' C44' C54' 2.4(16) . . . . ? N74' C34' C44' C54' 178.9(10) . . . . ? C34' C44' C54' C64' -0.9(18) . . . . ? C24' N14' C64' C54' -2.1(17) . . . . ? Pd4 N14' C64' C54' -176.8(9) . . . . ? C44' C54' C64' N14' 0.7(19) . . . . ? C163 P5 C154 C155 -63.0(9) . . . . ? C157 P5 C154 C155 -175.7(8) . . . . ? Pd3 P5 C154 C155 61.8(9) . . . . ? P5 C154 C155 C156 -73.4(10) . . . . ? C154 C155 C156 P6 71.8(10) . . . . ? C169 P6 C156 C155 68.7(9) . . . . ? C175 P6 C156 C155 179.7(8) . . . . ? Pd3 P6 C156 C155 -59.0(9) . . . . ? C163 P5 C157 C162 20.0(9) . . . . ? C154 P5 C157 C162 133.2(9) . . . . ? Pd3 P5 C157 C162 -102.8(8) . . . . ? C163 P5 C157 C158 -162.9(9) . . . . ? C154 P5 C157 C158 -49.7(10) . . . . ? Pd3 P5 C157 C158 74.3(9) . . . . ? C162 C157 C158 C159 -1.4(17) . . . . ? P5 C157 C158 C159 -178.6(9) . . . . ? C157 C158 C159 C160 2.6(19) . . . . ? C158 C159 C160 C161 -2.6(18) . . . . ? C159 C160 C161 C162 1.4(16) . . . . ? C158 C157 C162 C161 0.3(15) . . . . ? P5 C157 C162 C161 177.4(8) . . . . ? C160 C161 C162 C157 -0.3(16) . . . . ? C154 P5 C163 C164 -29.1(11) . . . . ? C157 P5 C163 C164 80.6(10) . . . . ? Pd3 P5 C163 C164 -155.9(9) . . . . ? C154 P5 C163 C168 157.7(8) . . . . ? C157 P5 C163 C168 -92.7(9) . . . . ? Pd3 P5 C163 C168 30.9(10) . . . . ? C168 C163 C164 C165 -7.7(18) . . . . ? P5 C163 C164 C165 178.9(10) . . . . ? C163 C164 C165 C166 5(2) . . . . ? C164 C165 C166 C167 -2(2) . . . . ? C165 C166 C167 C168 1(2) . . . . ? C164 C163 C168 C167 6.4(16) . . . . ? P5 C163 C168 C167 -179.8(9) . . . . ? C166 C167 C168 C163 -3.2(18) . . . . ? C156 P6 C169 C174 37.5(11) . . . . ? C175 P6 C169 C174 -72.0(11) . . . . ? Pd3 P6 C169 C174 166.1(10) . . . . ? C156 P6 C169 C170 -142.9(8) . . . . ? C175 P6 C169 C170 107.6(9) . . . . ? Pd3 P6 C169 C170 -14.2(9) . . . . ? C174 C169 C170 C171 1.1(17) . . . . ? P6 C169 C170 C171 -178.6(9) . . . . ? C169 C170 C171 C172 -1(2) . . . . ? C170 C171 C172 C173 1(2) . . . . ? C171 C172 C173 C174 0(2) . . . . ? C172 C173 C174 C169 0(2) . . . . ? C170 C169 C174 C173 -1(2) . . . . ? P6 C169 C174 C173 178.9(12) . . . . ? C156 P6 C175 C180 54.3(10) . . . . ? C169 P6 C175 C180 165.5(9) . . . . ? Pd3 P6 C175 C180 -70.4(9) . . . . ? C156 P6 C175 C176 -130.4(9) . . . . ? C169 P6 C175 C176 -19.2(10) . . . . ? Pd3 P6 C175 C176 104.9(8) . . . . ? C180 C175 C176 C177 2.1(16) . . . . ? P6 C175 C176 C177 -173.2(9) . . . . ? C175 C176 C177 C178 -0.3(18) . . . . ? C176 C177 C178 C179 -1.3(19) . . . . ? C177 C178 C179 C180 1.2(18) . . . . ? C176 C175 C180 C179 -2.2(16) . . . . ? P6 C175 C180 C179 173.1(8) . . . . ? C178 C179 C180 C175 0.5(17) . . . . ? C184 P7 C181 C182 -178.3(9) . . . . ? C190 P7 C181 C182 69.4(11) . . . . ? Pd4 P7 C181 C182 -57.7(10) . . . . ? P7 C181 C182 C183 69.3(14) . . . . ? C181 C182 C183 P8 -72.5(13) . . . . ? C196 P8 C183 C182 -61.0(10) . . . . ? C202 P8 C183 C182 -173.2(9) . . . . ? Pd4 P8 C183 C182 65.3(10) . . . . ? C190 P7 C184 C185 -19.0(13) . . . . ? C181 P7 C184 C185 -131.3(12) . . . . ? Pd4 P7 C184 C185 105.5(11) . . . . ? C190 P7 C184 C189 161.6(11) . . . . ? C181 P7 C184 C189 49.3(12) . . . . ? Pd4 P7 C184 C189 -73.9(11) . . . . ? C189 C184 C185 C186 2(2) . . . . ? P7 C184 C185 C186 -177.5(11) . . . . ? C184 C185 C186 C187 -3(2) . . . . ? C185 C186 C187 C188 5(2) . . . . ? C186 C187 C188 C189 -5(2) . . . . ? C187 C188 C189 C184 4(2) . . . . ? C185 C184 C189 C188 -2(2) . . . . ? P7 C184 C189 C188 177.1(11) . . . . ? C184 P7 C190 C191 83.2(14) . . . . ? C181 P7 C190 C191 -167.6(13) . . . . ? Pd4 P7 C190 C191 -39.8(14) . . . . ? C184 P7 C190 C195 -94.1(13) . . . . ? C181 P7 C190 C195 15.0(14) . . . . ? Pd4 P7 C190 C195 142.8(11) . . . . ? C195 C190 C191 C192 -3(3) . . . . ? P7 C190 C191 C192 179.2(14) . . . . ? C190 C191 C192 C193 3(3) . . . . ? C191 C192 C193 C194 -2(3) . . . . ? C192 C193 C194 C195 0(3) . . . . ? C193 C194 C195 C190 -1(3) . . . . ? C191 C190 C195 C194 2(2) . . . . ? P7 C190 C195 C194 179.4(13) . . . . ? C183 P8 C196 C201 -42.5(13) . . . . ? C202 P8 C196 C201 68.6(13) . . . . ? Pd4 P8 C196 C201 -168.8(10) . . . . ? C183 P8 C196 C197 142.2(11) . . . . ? C202 P8 C196 C197 -106.7(11) . . . . ? Pd4 P8 C196 C197 15.9(12) . . . . ? C201 C196 C197 C198 10(2) . . . . ? P8 C196 C197 C198 -174.5(11) . . . . ? C196 C197 C198 C199 -8(2) . . . . ? C197 C198 C199 C200 0(3) . . . . ? C198 C199 C200 C201 5(3) . . . . ? C197 C196 C201 C200 -5(2) . . . . ? P8 C196 C201 C200 179.4(12) . . . . ? C199 C200 C201 C196 -3(3) . . . . ? C183 P8 C202 C207 144.9(10) . . . . ? C196 P8 C202 C207 32.7(12) . . . . ? Pd4 P8 C202 C207 -91.7(10) . . . . ? C183 P8 C202 C203 -38.6(12) . . . . ? C196 P8 C202 C203 -150.8(11) . . . . ? Pd4 P8 C202 C203 84.8(11) . . . . ? C207 C202 C203 C204 0.1(19) . . . . ? P8 C202 C203 C204 -176.2(10) . . . . ? C202 C203 C204 C205 2(2) . . . . ? C203 C204 C205 C206 -6(2) . . . . ? C204 C205 C206 C207 7(2) . . . . ? C205 C206 C207 C202 -4(2) . . . . ? C203 C202 C207 C206 0.6(19) . . . . ? P8 C202 C207 C206 177.0(10) . . . . ? O31 S11 C11 F21 179.0(4) . . . . ? O11 S11 C11 F21 -59.6(4) . . . . ? O21 S11 C11 F21 59.7(4) . . . . ? O31 S11 C11 F11 -61.5(4) . . . . ? O11 S11 C11 F11 60.0(4) . . . . ? O21 S11 C11 F11 179.2(4) . . . . ? O31 S11 C11 F31 59.1(4) . . . . ? O11 S11 C11 F31 -179.5(3) . . . . ? O21 S11 C11 F31 -60.2(4) . . . . ? O12 S12 C12 F12 61.5(11) . . . . ? O22 S12 C12 F12 -176.7(9) . . . . ? O32 S12 C12 F12 -59.3(11) . . . . ? O12 S12 C12 F22 -63.1(12) . . . . ? O22 S12 C12 F22 58.7(11) . . . . ? O32 S12 C12 F22 176.0(10) . . . . ? O12 S12 C12 F32 -177.6(9) . . . . ? O22 S12 C12 F32 -55.8(11) . . . . ? O32 S12 C12 F32 61.6(11) . . . . ? O23 S13 C13 F23 -60.3(4) . . . . ? O13 S13 C13 F23 59.9(4) . . . . ? O33 S13 C13 F23 -179.9(4) . . . . ? O23 S13 C13 F13 178.9(4) . . . . ? O13 S13 C13 F13 -60.9(4) . . . . ? O33 S13 C13 F13 59.2(4) . . . . ? O23 S13 C13 F33 59.6(4) . . . . ? O13 S13 C13 F33 179.8(4) . . . . ? O33 S13 C13 F33 -60.0(4) . . . . ? O14 S14 C14 F24 -52.3(14) . . . . ? O34 S14 C14 F24 178.2(11) . . . . ? O24 S14 C14 F24 64.1(13) . . . . ? O14 S14 C14 F34 -176.3(11) . . . . ? O34 S14 C14 F34 54.2(14) . . . . ? O24 S14 C14 F34 -60.0(13) . . . . ? O14 S14 C14 F14 66.9(10) . . . . ? O34 S14 C14 F14 -62.5(9) . . . . ? O24 S14 C14 F14 -176.7(9) . . . . ? O15 S15 C15 F25 63.6(9) . . . . ? O35 S15 C15 F25 -176.7(8) . . . . ? O25 S15 C15 F25 -57.1(9) . . . . ? O15 S15 C15 F15 -58.7(11) . . . . ? O35 S15 C15 F15 60.9(10) . . . . ? O25 S15 C15 F15 -179.5(9) . . . . ? O15 S15 C15 F35 -176.8(9) . . . . ? O35 S15 C15 F35 -57.2(10) . . . . ? O25 S15 C15 F35 62.4(10) . . . . ? O16 S16 C16 F16 -57.6(11) . . . . ? O26 S16 C16 F16 178.8(9) . . . . ? O36 S16 C16 F16 60.8(10) . . . . ? O16 S16 C16 F36 -177.3(9) . . . . ? O26 S16 C16 F36 59.1(10) . . . . ? O36 S16 C16 F36 -58.9(10) . . . . ? O16 S16 C16 F26 64.8(10) . . . . ? O26 S16 C16 F26 -58.8(10) . . . . ? O36 S16 C16 F26 -176.8(8) . . . . ? O27 S17 C17 F17 -60.7(4) . . . . ? O17 S17 C17 F17 60.6(4) . . . . ? O37 S17 C17 F17 -179.8(4) . . . . ? O27 S17 C17 F27 179.5(4) . . . . ? O17 S17 C17 F27 -59.2(4) . . . . ? O37 S17 C17 F27 60.4(4) . . . . ? O27 S17 C17 F37 59.9(4) . . . . ? O17 S17 C17 F37 -178.8(4) . . . . ? O37 S17 C17 F37 -59.2(4) . . . . ? O18 S18 C18 F28 179.2(4) . . . . ? O28 S18 C18 F28 -59.8(4) . . . . ? O38 S18 C18 F28 60.0(4) . . . . ? O18 S18 C18 F38 -60.7(4) . . . . ? O28 S18 C18 F38 60.2(4) . . . . ? O38 S18 C18 F38 -180.0(4) . . . . ? O18 S18 C18 F18 58.8(4) . . . . ? O28 S18 C18 F18 179.8(4) . . . . ? O38 S18 C18 F18 -60.4(4) . . . . ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 7 1 ' ' 2 -0.189 0.803 0.250 140 52 ' ' 3 0.189 0.197 0.750 140 53 ' ' 4 0.204 0.062 0.045 19 4 ' ' 5 0.340 0.147 0.261 149 58 ' ' 6 0.364 0.098 0.528 45 9 ' ' 7 0.660 0.853 0.739 149 58 ' ' 8 0.636 0.902 0.472 45 8 ' ' 9 0.796 0.938 0.955 19 4 ' ' _platon_squeeze_details ; ; #============================================================================= # END of CIF #============================================================================= # Attachment '- Schalley_DT-ART-01-2012-030190_Compound25a.cif' data_25a _database_code_depnum_ccdc_archive 'CCDC 864208' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound25a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C80 H80 N8 O2 P4 Pd2 4+, 4(C F3 O3 S 1-), 3(C3 H7 N O), 1/2(C4 H10 O), H2 O' _chemical_formula_sum 'C95 H108 F12 N11 O18.50 P4 Pd2 S4' _chemical_formula_weight 2392.84 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.3896(2) _cell_length_b 18.3213(2) _cell_length_c 21.5285(3) _cell_angle_alpha 87.680(1) _cell_angle_beta 78.927(1) _cell_angle_gamma 71.110(1) _cell_volume 6000.9(1) _cell_formula_units_Z 2 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 21254 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 27.103 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2454 _exptl_absorpt_coefficient_mu 0.503 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6050 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ; Sheldrick, G. M. SADABS 2008/2; University of G\"ottingen: G\"ottingen, Germany, 2008. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Bruker-Nonius Kappa Apex II Diffractometer' _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_UB_11 0.579874E-1 _diffrn_orient_matrix_UB_12 -0.126827E-1 _diffrn_orient_matrix_UB_13 -0.296163E-1 _diffrn_orient_matrix_UB_21 0.300837E-1 _diffrn_orient_matrix_UB_22 -0.35301E-2 _diffrn_orient_matrix_UB_23 0.367946E-1 _diffrn_orient_matrix_UB_31 0.67559E-2 _diffrn_orient_matrix_UB_32 -0.56182E-1 _diffrn_orient_matrix_UB_33 0.32375E-2 _diffrn_reflns_number 71355 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21076 _reflns_number_gt 16013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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. Although data were collected at 173 K, some atoms of solvent molecules and triflates had high anisotropic thermal parameters. Therefore, ISOR restraint was used in the refinement of O1, C1, C3, C5 and C8 atoms in N,N-dimethylformamide molecules and O11, O31, O22, O32, F12, F32, F13 and F23 atoms in triflates #1-3. In addition, EADP constraint was used in the refinement of O24, O14, F24, F14 and C14' atoms in triflate #4, so that displacement parameters are taken from O34, F34 and C14 atoms, respectively. These restraints and constraints were used in order to avoid Alerts in CHECKCIF. As bond length and angles were not in accord with expected DFIX command in SHELXL was used for S -- O distance in triflate #1, C -- F and S12 -- O32 distances in triflate #2, S14 -- O14, S14 -- O24 and C14 -- F24 distances in triflate #4, N1 -- C1 distance in N,N-dimethylformamide molecule, O -- C and C -- C distances in diethyl ether molecule and O -- H distances in water molecule. ; _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^)+(0.2000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21076 _refine_ls_number_parameters 1317 _refine_ls_number_restraints 107 _refine_ls_R_factor_all 0.1000 _refine_ls_R_factor_gt 0.0780 _refine_ls_wR_factor_ref 0.2707 _refine_ls_wR_factor_gt 0.2499 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.001 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 Pd1 Pd 0.90797(3) 0.34896(2) 0.29006(2) 0.02828(16) Uani 1 1 d . . . Pd2 Pd 0.70710(3) 0.25902(2) 0.68644(2) 0.02883(16) Uani 1 1 d . . . P1 P 1.01741(10) 0.23499(9) 0.26503(8) 0.0336(4) Uani 1 1 d . . . P2 P 1.01020(10) 0.40554(9) 0.29928(7) 0.0320(4) Uani 1 1 d . . . P3 P 0.81493(10) 0.14748(9) 0.70060(7) 0.0332(4) Uani 1 1 d . . . P4 P 0.76830(10) 0.33160(9) 0.73333(7) 0.0314(3) Uani 1 1 d . . . N11 N 0.8121(3) 0.2982(3) 0.2824(2) 0.0299(11) Uani 1 1 d . . . N71 N 0.7075(3) 0.1684(3) 0.3739(2) 0.0328(11) Uani 1 1 d . . . H71 H 0.7007 0.1249 0.3641 0.039 Uiso 1 1 calc R . . N11' N 0.6496(3) 0.1963(3) 0.6390(2) 0.0313(11) Uani 1 1 d . . . N71' N 0.6777(4) 0.1317(3) 0.4752(2) 0.0367(12) Uani 1 1 d . . . H71' H 0.6848 0.0870 0.4576 0.044 Uiso 1 1 calc R . . O81 O 0.6965(3) 0.2493(2) 0.4549(2) 0.0415(11) Uani 1 1 d . . . C21 C 0.7861(4) 0.2571(3) 0.3305(3) 0.0295(12) Uani 1 1 d . . . H21 H 0.8054 0.2568 0.3694 0.035 Uiso 1 1 calc R . . C31 C 0.7310(4) 0.2146(3) 0.3239(3) 0.0318(13) Uani 1 1 d . . . C41 C 0.7014(4) 0.2157(4) 0.2682(3) 0.0364(14) Uani 1 1 d . . . C51 C 0.7270(4) 0.2626(4) 0.2195(3) 0.0389(14) Uani 1 1 d . . . H51 H 0.7062 0.2668 0.1808 0.047 Uiso 1 1 calc R . . C61 C 0.7816(4) 0.3014(4) 0.2287(3) 0.0383(14) Uani 1 1 d . . . H61 H 0.7989 0.3322 0.1956 0.046 Uiso 1 1 calc R . . C81 C 0.6947(4) 0.1875(3) 0.4368(3) 0.0312(13) Uani 1 1 d . . . C4A C 0.6445(5) 0.1691(5) 0.2584(3) 0.0498(17) Uani 1 1 d . . . H4A1 H 0.6237 0.1832 0.2185 0.075 Uiso 1 1 calc R . . H4A2 H 0.5941 0.1795 0.2935 0.075 Uiso 1 1 calc R . . H4A3 H 0.6786 0.1141 0.2569 0.075 Uiso 1 1 calc R . . C21' C 0.6745(4) 0.1875(3) 0.5766(3) 0.0321(13) Uani 1 1 d . . . H21' H 0.7111 0.2151 0.5550 0.039 Uiso 1 1 calc R . . C31' C 0.6492(4) 0.1402(3) 0.5423(3) 0.0350(13) Uani 1 1 d . . . C41' C 0.5972(4) 0.0970(4) 0.5727(3) 0.0397(15) Uani 1 1 d . . . C51' C 0.5734(4) 0.1074(4) 0.6388(3) 0.0406(15) Uani 1 1 d . . . H51' H 0.5390 0.0790 0.6620 0.049 Uiso 1 1 calc R . . C61' C 0.5982(4) 0.1569(4) 0.6703(3) 0.0392(15) Uani 1 1 d . . . H61' H 0.5791 0.1639 0.7149 0.047 Uiso 1 1 calc R . . C4A' C 0.5751(6) 0.0390(4) 0.5373(4) 0.055(2) Uani 1 1 d . . . H4A4 H 0.6291 -0.0022 0.5195 0.083 Uiso 1 1 calc R . . H4A5 H 0.5456 0.0645 0.5030 0.083 Uiso 1 1 calc R . . H4A6 H 0.5361 0.0168 0.5664 0.083 Uiso 1 1 calc R . . N12 N 0.8039(3) 0.4522(3) 0.3140(2) 0.0317(11) Uani 1 1 d . . . N72 N 0.6325(3) 0.5385(3) 0.4520(2) 0.0354(12) Uani 1 1 d . . . H72 H 0.5925 0.5841 0.4612 0.042 Uiso 1 1 calc R . . N12' N 0.6066(3) 0.3603(3) 0.6712(2) 0.0332(11) Uani 1 1 d . . . N72' N 0.5739(3) 0.5122(3) 0.5525(2) 0.0339(11) Uani 1 1 d . . . H72' H 0.5388 0.5601 0.5523 0.041 Uiso 1 1 calc R . . O82 O 0.6848(4) 0.4190(3) 0.4916(2) 0.0692(18) Uani 1 1 d . . . C22 C 0.7552(4) 0.4616(3) 0.3723(3) 0.0337(13) Uani 1 1 d . . . H22 H 0.7682 0.4208 0.4012 0.040 Uiso 1 1 calc R . . C32 C 0.6853(4) 0.5294(3) 0.3924(3) 0.0304(12) Uani 1 1 d . . . C42 C 0.6675(4) 0.5897(3) 0.3492(3) 0.0316(13) Uani 1 1 d . . . C52 C 0.7192(4) 0.5760(4) 0.2892(3) 0.0386(14) Uani 1 1 d . . . H52 H 0.7090 0.6153 0.2587 0.046 Uiso 1 1 calc R . . C62 C 0.7839(4) 0.5082(3) 0.2728(3) 0.0363(14) Uani 1 1 d . . . H62 H 0.8160 0.5003 0.2305 0.044 Uiso 1 1 calc R . . C82 C 0.6356(4) 0.4846(3) 0.4984(3) 0.0347(14) Uani 1 1 d . . . C4B C 0.5974(4) 0.6644(3) 0.3682(3) 0.0385(14) Uani 1 1 d . . . H4B1 H 0.5903 0.6971 0.3312 0.058 Uiso 1 1 calc R . . H4B2 H 0.6138 0.6904 0.4004 0.058 Uiso 1 1 calc R . . H4B3 H 0.5420 0.6549 0.3856 0.058 Uiso 1 1 calc R . . C22' C 0.6204(4) 0.3976(3) 0.6170(3) 0.0332(13) Uani 1 1 d . . . H22' H 0.6699 0.3740 0.5850 0.040 Uiso 1 1 calc R . . C32' C 0.5623(4) 0.4717(3) 0.6069(3) 0.0304(12) Uani 1 1 d . . . C42' C 0.4906(4) 0.5068(4) 0.6561(3) 0.0343(13) Uani 1 1 d . . . C52' C 0.4783(4) 0.4637(4) 0.7106(3) 0.0361(14) Uani 1 1 d . . . H52' H 0.4298 0.4848 0.7439 0.043 Uiso 1 1 calc R . . C62' C 0.5357(4) 0.3916(4) 0.7157(3) 0.0355(14) Uani 1 1 d . . . H62' H 0.5249 0.3627 0.7522 0.043 Uiso 1 1 calc R . . C4B' C 0.4310(4) 0.5881(4) 0.6524(3) 0.0425(15) Uani 1 1 d . . . H4B4 H 0.3902 0.6036 0.6929 0.064 Uiso 1 1 calc R . . H4B5 H 0.3977 0.5910 0.6186 0.064 Uiso 1 1 calc R . . H4B6 H 0.4662 0.6229 0.6433 0.064 Uiso 1 1 calc R . . C100 C 1.0980(5) 0.2130(4) 0.3166(4) 0.0466(17) Uani 1 1 d . . . H10A H 1.0676 0.2089 0.3604 0.056 Uiso 1 1 calc R . . H10B H 1.1417 0.1618 0.3037 0.056 Uiso 1 1 calc R . . C101 C 1.1474(5) 0.2713(4) 0.3171(4) 0.0484(17) Uani 1 1 d . . . H10C H 1.1952 0.2496 0.3413 0.058 Uiso 1 1 calc R . . H10D H 1.1748 0.2782 0.2731 0.058 Uiso 1 1 calc R . . C102 C 1.0897(5) 0.3506(4) 0.3460(3) 0.0436(16) Uani 1 1 d . . . H10E H 1.1282 0.3810 0.3514 0.052 Uiso 1 1 calc R . . H10F H 1.0580 0.3434 0.3886 0.052 Uiso 1 1 calc R . . C103 C 0.9760(4) 0.1534(3) 0.2723(3) 0.0390(15) Uani 1 1 d . . . C104 C 0.9473(4) 0.1315(4) 0.2205(3) 0.0434(16) Uani 1 1 d . . . H104 H 0.9539 0.1562 0.1811 0.052 Uiso 1 1 calc R . . C105 C 0.9088(5) 0.0729(4) 0.2277(4) 0.0499(17) Uani 1 1 d . . . H105 H 0.8899 0.0577 0.1927 0.060 Uiso 1 1 calc R . . C106 C 0.8982(5) 0.0371(4) 0.2841(4) 0.0502(18) Uani 1 1 d . . . H106 H 0.8712 -0.0020 0.2883 0.060 Uiso 1 1 calc R . . C107 C 0.9269(5) 0.0578(4) 0.3355(4) 0.0510(19) Uani 1 1 d . . . H107 H 0.9202 0.0319 0.3744 0.061 Uiso 1 1 calc R . . C108 C 0.9657(4) 0.1168(3) 0.3306(3) 0.0412(15) Uani 1 1 d . . . H108 H 0.9845 0.1313 0.3659 0.049 Uiso 1 1 calc R . . C109 C 1.0747(4) 0.2300(4) 0.1846(3) 0.0410(15) Uani 1 1 d . . . C110 C 1.1649(5) 0.1918(5) 0.1669(4) 0.061(2) Uani 1 1 d . . . H110 H 1.1984 0.1678 0.1980 0.073 Uiso 1 1 calc R . . C111 C 1.2051(7) 0.1891(6) 0.1039(5) 0.078(3) Uani 1 1 d . . . H111 H 1.2666 0.1635 0.0926 0.093 Uiso 1 1 calc R . . C112 C 1.1599(7) 0.2216(7) 0.0582(5) 0.086(3) Uani 1 1 d . . . H112 H 1.1891 0.2194 0.0153 0.103 Uiso 1 1 calc R . . C113 C 1.0692(7) 0.2588(5) 0.0747(4) 0.070(2) Uani 1 1 d . . . H113 H 1.0363 0.2803 0.0428 0.084 Uiso 1 1 calc R . . C114 C 1.0274(5) 0.2642(4) 0.1376(3) 0.0507(18) Uani 1 1 d . . . H114 H 0.9663 0.2912 0.1488 0.061 Uiso 1 1 calc R . . C115 C 1.0731(4) 0.4233(3) 0.2254(3) 0.0330(13) Uani 1 1 d . . . C116 C 1.1551(5) 0.4303(4) 0.2216(3) 0.0459(16) Uani 1 1 d . . . H116 H 1.1802 0.4259 0.2584 0.055 Uiso 1 1 calc R . . C117 C 1.2010(5) 0.4442(5) 0.1626(4) 0.0541(19) Uani 1 1 d . . . H117 H 1.2572 0.4497 0.1601 0.065 Uiso 1 1 calc R . . C118 C 1.1688(5) 0.4496(5) 0.1112(4) 0.056(2) Uani 1 1 d . . . H118 H 1.2030 0.4562 0.0718 0.067 Uiso 1 1 calc R . . C119 C 1.0839(5) 0.4459(4) 0.1132(3) 0.0521(18) Uani 1 1 d . . . H119 H 1.0592 0.4532 0.0760 0.063 Uiso 1 1 calc R . . C120 C 1.0369(4) 0.4312(4) 0.1707(3) 0.0403(15) Uani 1 1 d . . . H120 H 0.9803 0.4266 0.1728 0.048 Uiso 1 1 calc R . . C121 C 0.9617(4) 0.4982(4) 0.3401(3) 0.0400(15) Uani 1 1 d . . . C122 C 0.9201(6) 0.5034(5) 0.4034(4) 0.060(2) Uani 1 1 d . . . H122 H 0.9213 0.4573 0.4255 0.072 Uiso 1 1 calc R . . C123 C 0.8772(8) 0.5738(6) 0.4349(5) 0.093(4) Uani 1 1 d . . . H123 H 0.8515 0.5765 0.4786 0.112 Uiso 1 1 calc R . . C124 C 0.8728(7) 0.6413(5) 0.4001(5) 0.082(3) Uani 1 1 d . . . H124 H 0.8414 0.6902 0.4202 0.098 Uiso 1 1 calc R . . C125 C 0.9119(6) 0.6381(5) 0.3390(5) 0.066(2) Uani 1 1 d . . . H125 H 0.9095 0.6844 0.3169 0.079 Uiso 1 1 calc R . . C126 C 0.9563(5) 0.5667(4) 0.3080(4) 0.0478(17) Uani 1 1 d . . . H126 H 0.9830 0.5648 0.2646 0.057 Uiso 1 1 calc R . . C127 C 0.9238(4) 0.1547(4) 0.6964(4) 0.0425(15) Uani 1 1 d . . . H12A H 0.9639 0.1038 0.7056 0.051 Uiso 1 1 calc R . . H12B H 0.9459 0.1677 0.6526 0.051 Uiso 1 1 calc R . . C128 C 0.9267(4) 0.2153(4) 0.7423(4) 0.0465(16) Uani 1 1 d . . . H12C H 0.8936 0.2090 0.7846 0.056 Uiso 1 1 calc R . . H12D H 0.9885 0.2060 0.7461 0.056 Uiso 1 1 calc R . . C129 C 0.8883(4) 0.2980(4) 0.7215(3) 0.0384(14) Uani 1 1 d . . . H12E H 0.9125 0.3015 0.6761 0.046 Uiso 1 1 calc R . . H12F H 0.9071 0.3327 0.7456 0.046 Uiso 1 1 calc R . . C130 C 0.8335(4) 0.0752(4) 0.6392(3) 0.0381(14) Uani 1 1 d . . . C131 C 0.8759(5) 0.0859(5) 0.5789(4) 0.059(2) Uani 1 1 d . . . H131 H 0.8990 0.1273 0.5701 0.071 Uiso 1 1 calc R . . C132 C 0.8828(6) 0.0329(6) 0.5317(4) 0.072(3) Uani 1 1 d . . . H132 H 0.9132 0.0380 0.4903 0.086 Uiso 1 1 calc R . . C133 C 0.8490(7) -0.0242(6) 0.5419(5) 0.080(3) Uani 1 1 d . . . H133 H 0.8546 -0.0581 0.5080 0.096 Uiso 1 1 calc R . . C134 C 0.8058(6) -0.0344(5) 0.6016(4) 0.067(2) Uani 1 1 d . . . H134 H 0.7815 -0.0753 0.6091 0.080 Uiso 1 1 calc R . . C135 C 0.7983(5) 0.0151(4) 0.6502(3) 0.0467(17) Uani 1 1 d . . . H135 H 0.7689 0.0084 0.6915 0.056 Uiso 1 1 calc R . . C136 C 0.7916(4) 0.1027(4) 0.7761(3) 0.0360(14) Uani 1 1 d . . . C137 C 0.8549(5) 0.0390(4) 0.7938(3) 0.0458(16) Uani 1 1 d . . . H137 H 0.9108 0.0192 0.7670 0.055 Uiso 1 1 calc R . . C138 C 0.8361(6) 0.0039(4) 0.8510(4) 0.057(2) Uani 1 1 d . . . H138 H 0.8788 -0.0406 0.8628 0.069 Uiso 1 1 calc R . . C139 C 0.7571(6) 0.0332(5) 0.8899(4) 0.065(2) Uani 1 1 d . . . H139 H 0.7450 0.0101 0.9294 0.078 Uiso 1 1 calc R . . C140 C 0.6953(6) 0.0956(5) 0.8723(4) 0.067(3) Uani 1 1 d . . . H140 H 0.6403 0.1165 0.8999 0.081 Uiso 1 1 calc R . . C141 C 0.7119(5) 0.1292(4) 0.8141(3) 0.0492(17) Uani 1 1 d . . . H141 H 0.6670 0.1710 0.8012 0.059 Uiso 1 1 calc R . . C142 C 0.7297(4) 0.3412(4) 0.8182(3) 0.0364(14) Uani 1 1 d . . . C143 C 0.6554(4) 0.3246(4) 0.8458(3) 0.0452(16) Uani 1 1 d . . . H143 H 0.6244 0.3068 0.8201 0.054 Uiso 1 1 calc R . . C144 C 0.6247(6) 0.3331(5) 0.9103(4) 0.059(2) Uani 1 1 d . . . H144 H 0.5717 0.3235 0.9284 0.071 Uiso 1 1 calc R . . C145 C 0.6713(6) 0.3556(6) 0.9482(4) 0.067(2) Uani 1 1 d . . . H145 H 0.6525 0.3584 0.9928 0.081 Uiso 1 1 calc R . . C146 C 0.7472(6) 0.3745(6) 0.9208(4) 0.065(2) Uani 1 1 d . . . H146 H 0.7780 0.3924 0.9466 0.079 Uiso 1 1 calc R . . C147 C 0.7765(5) 0.3664(5) 0.8557(3) 0.0499(17) Uani 1 1 d . . . H147 H 0.8280 0.3781 0.8367 0.060 Uiso 1 1 calc R . . C148 C 0.7427(4) 0.4289(4) 0.7032(3) 0.0383(14) Uani 1 1 d . . . C149 C 0.6765(4) 0.4902(4) 0.7371(4) 0.0434(16) Uani 1 1 d . . . H149 H 0.6472 0.4814 0.7779 0.052 Uiso 1 1 calc R . . C150 C 0.6526(6) 0.5630(4) 0.7128(4) 0.059(2) Uani 1 1 d . . . H150 H 0.6071 0.6043 0.7362 0.071 Uiso 1 1 calc R . . C151 C 0.6975(6) 0.5749(5) 0.6520(5) 0.065(2) Uani 1 1 d . . . H151 H 0.6815 0.6246 0.6341 0.078 Uiso 1 1 calc R . . C152 C 0.7632(7) 0.5156(5) 0.6193(5) 0.067(2) Uani 1 1 d . . . H152 H 0.7941 0.5246 0.5792 0.081 Uiso 1 1 calc R . . C153 C 0.7860(5) 0.4412(4) 0.6441(3) 0.0500(17) Uani 1 1 d . . . H153 H 0.8308 0.3997 0.6204 0.060 Uiso 1 1 calc R . . S11 S 0.44658(17) 0.19681(12) 0.41655(15) 0.0873(9) Uani 1 1 d D . . O11 O 0.4826(7) 0.2148(7) 0.4683(4) 0.152(4) Uani 1 1 d DU . . O21 O 0.4852(4) 0.11621(17) 0.3971(3) 0.084(2) Uani 1 1 d D . . O31 O 0.4367(6) 0.2535(5) 0.3673(4) 0.144(4) Uani 1 1 d DU . . F11 F 0.2951(6) 0.1782(6) 0.4234(7) 0.193(5) Uani 1 1 d . . . F21 F 0.2924(5) 0.2783(4) 0.4725(4) 0.127(3) Uani 1 1 d . . . F31 F 0.3373(7) 0.1644(5) 0.5049(4) 0.165(4) Uani 1 1 d . . . C11 C 0.3391(7) 0.2064(6) 0.4568(5) 0.076(3) Uani 1 1 d . . . S12 S 0.43194(12) 0.22712(13) 0.82560(10) 0.0576(5) Uani 1 1 d D . . O12 O 0.5099(4) 0.2453(4) 0.8138(3) 0.0819(19) Uani 1 1 d . . . O22 O 0.4445(8) 0.1488(6) 0.8105(5) 0.139(3) Uani 1 1 d U . . O32 O 0.3590(4) 0.2805(6) 0.8014(4) 0.127(3) Uani 1 1 d DU . . F12 F 0.4602(5) 0.1837(5) 0.9383(3) 0.153(3) Uani 1 1 d DU . . F22 F 0.3967(10) 0.3020(6) 0.9341(4) 0.222(7) Uani 1 1 d D . . F32 F 0.3267(6) 0.2231(8) 0.9302(5) 0.186(4) Uani 1 1 d DU . . C12 C 0.4032(4) 0.2348(5) 0.9083(4) 0.115(5) Uani 1 1 d D . . S13 S 0.81807(12) 0.41901(11) 0.07670(8) 0.0451(4) Uani 1 1 d . . . O13 O 0.8603(4) 0.4383(5) 0.0171(3) 0.080(2) Uani 1 1 d . . . O23 O 0.7928(6) 0.3510(4) 0.0741(3) 0.092(2) Uani 1 1 d . . . O33 O 0.8569(3) 0.4248(3) 0.1300(2) 0.0531(13) Uani 1 1 d . . . F13 F 0.6665(5) 0.4882(6) 0.1445(4) 0.135(3) Uani 1 1 d U . . F23 F 0.7271(6) 0.5601(5) 0.0990(5) 0.143(3) Uani 1 1 d U . . F33 F 0.6682(4) 0.5018(4) 0.0472(3) 0.097(2) Uani 1 1 d . . . C13 C 0.7151(6) 0.4959(7) 0.0910(5) 0.075(3) Uani 1 1 d . . . S14 S 0.9122(2) 0.2604(2) 0.48977(16) 0.0448(8) Uani 0.60 1 d PD A 1 S14' S 0.9041(3) 0.3024(4) 0.5007(2) 0.0456(12) Uani 0.40 1 d P A 2 O14 O 0.8991(4) 0.3092(4) 0.4355(2) 0.0797(11) Uani 1 1 d D . . O24 O 0.9458(4) 0.1801(2) 0.4691(3) 0.0797(11) Uani 1 1 d D . . O34 O 0.8444(4) 0.2784(4) 0.5466(3) 0.0797(11) Uani 1 1 d . . . F14 F 1.0202(4) 0.2339(4) 0.5692(3) 0.1010(12) Uani 1 1 d . . . F24 F 0.9869(4) 0.3455(4) 0.5333(3) 0.1010(12) Uani 1 1 d D . . F34 F 1.0780(4) 0.2517(4) 0.4750(3) 0.1010(12) Uani 1 1 d . . . C14 C 1.0041(8) 0.2714(5) 0.5178(5) 0.038(3) Uani 0.60 1 d PD A 1 C14' C 1.0137(14) 0.2308(10) 0.5112(9) 0.038(3) Uani 0.40 1 d P A 2 N1 N 0.4367(6) 0.0495(7) 0.2285(5) 0.108(3) Uani 1 1 d D . . O1 O 0.2943(5) 0.0950(5) 0.2638(5) 0.122(3) Uani 1 1 d U . . C1 C 0.3698(8) 0.0838(7) 0.2715(6) 0.120(4) Uani 1 1 d DU . . H1 H 0.3791 0.1008 0.3098 0.144 Uiso 1 1 calc R . . C2 C 0.5281(6) 0.0339(6) 0.2317(6) 0.086(3) Uani 1 1 d . . . H2A H 0.5652 0.0045 0.1937 0.129 Uiso 1 1 calc R . . H2B H 0.5412 0.0038 0.2693 0.129 Uiso 1 1 calc R . . H2C H 0.5399 0.0828 0.2341 0.129 Uiso 1 1 calc R . . C3 C 0.4129(13) 0.0132(12) 0.1759(10) 0.174(7) Uani 1 1 d U . . H3A H 0.4663 -0.0138 0.1457 0.260 Uiso 1 1 calc R . . H3B H 0.3735 0.0534 0.1540 0.260 Uiso 1 1 calc R . . H3C H 0.3832 -0.0238 0.1937 0.260 Uiso 1 1 calc R . . N2 N 0.7224(4) -0.1058(3) 0.3517(3) 0.0526(15) Uani 1 1 d . . . O2 O 0.7090(4) 0.0120(3) 0.3834(3) 0.0606(14) Uani 1 1 d . . . C4 C 0.6824(5) -0.0343(4) 0.3636(4) 0.0521(18) Uani 1 1 d . . . H4 H 0.6241 -0.0153 0.3558 0.062 Uiso 1 1 calc R . . C5 C 0.8099(8) -0.1403(6) 0.3631(7) 0.098(3) Uani 1 1 d U . . H5A H 0.8302 -0.1955 0.3521 0.147 Uiso 1 1 calc R . . H5B H 0.8105 -0.1334 0.4079 0.147 Uiso 1 1 calc R . . H5C H 0.8490 -0.1156 0.3369 0.147 Uiso 1 1 calc R . . C6 C 0.6872(9) -0.1589(7) 0.3240(7) 0.106(4) Uani 1 1 d . . . H6A H 0.7299 -0.2110 0.3206 0.160 Uiso 1 1 calc R . . H6B H 0.6763 -0.1415 0.2818 0.160 Uiso 1 1 calc R . . H6C H 0.6321 -0.1593 0.3512 0.160 Uiso 1 1 calc R . . N3 N 0.9241(4) 0.6432(4) 0.1154(3) 0.0608(18) Uani 1 1 d . . . O3 O 1.0055(5) 0.6774(5) 0.1732(4) 0.099(2) Uani 1 1 d . . . C7 C 0.9972(5) 0.6509(5) 0.1238(4) 0.059(2) Uani 1 1 d . . . H7 H 1.0468 0.6353 0.0903 0.071 Uiso 1 1 calc R . . C8 C 0.8490(8) 0.6593(8) 0.1635(6) 0.106(4) Uani 1 1 d U . . H8A H 0.8009 0.6511 0.1470 0.159 Uiso 1 1 calc R . . H8B H 0.8318 0.7131 0.1781 0.159 Uiso 1 1 calc R . . H8C H 0.8620 0.6250 0.1990 0.159 Uiso 1 1 calc R . . C9 C 0.9216(6) 0.6049(6) 0.0587(5) 0.076(3) Uani 1 1 d . . . H9A H 0.8618 0.6040 0.0599 0.115 Uiso 1 1 calc R . . H9B H 0.9621 0.5519 0.0563 0.115 Uiso 1 1 calc R . . H9C H 0.9391 0.6328 0.0214 0.115 Uiso 1 1 calc R . . O4 O 0.5627(8) 0.6587(7) 0.8591(6) 0.075(3) Uiso 0.50 1 d PD . . C16 C 0.580(2) 0.7239(12) 0.8711(10) 0.138(11) Uiso 0.50 1 d PD . . H16A H 0.5254 0.7633 0.8919 0.166 Uiso 0.50 1 calc PR . . H16B H 0.6223 0.7122 0.9003 0.166 Uiso 0.50 1 calc PR . . C17 C 0.6177(15) 0.7551(13) 0.8114(10) 0.092(6) Uiso 0.50 1 d PD . . H17A H 0.6299 0.8019 0.8212 0.138 Uiso 0.50 1 calc PR . . H17B H 0.5756 0.7675 0.7827 0.138 Uiso 0.50 1 calc PR . . H17C H 0.6724 0.7164 0.7911 0.138 Uiso 0.50 1 calc PR . . C18 C 0.5256(13) 0.6258(10) 0.9097(7) 0.082(6) Uiso 0.50 1 d PD . . H18A H 0.4646 0.6604 0.9233 0.098 Uiso 0.50 1 calc PR . . H18B H 0.5571 0.6267 0.9444 0.098 Uiso 0.50 1 calc PR . . C19 C 0.5211(16) 0.5462(10) 0.9062(11) 0.095(7) Uiso 0.50 1 d PD . . H19A H 0.4881 0.5347 0.9463 0.142 Uiso 0.50 1 calc PR . . H19B H 0.5806 0.5091 0.8984 0.142 Uiso 0.50 1 calc PR . . H19C H 0.4914 0.5424 0.8716 0.142 Uiso 0.50 1 calc PR . . O1W O 0.4771(4) 0.6576(3) 0.5085(3) 0.0625(15) Uani 1 1 d D . . H1W H 0.424(2) 0.665(6) 0.524(5) 0.09(3) Uiso 1 1 d D . . H2W H 0.492(9) 0.688(6) 0.529(6) 0.13(5) Uiso 1 1 d D . . 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 Pd1 0.0259(3) 0.0248(3) 0.0318(3) -0.00064(18) 0.00067(19) -0.00840(19) Pd2 0.0289(3) 0.0289(3) 0.0275(3) 0.00184(18) -0.00502(19) -0.00802(19) P1 0.0296(8) 0.0258(7) 0.0405(9) -0.0003(6) 0.0012(7) -0.0066(6) P2 0.0327(8) 0.0319(8) 0.0330(8) 0.0005(6) -0.0029(6) -0.0142(7) P3 0.0305(8) 0.0322(8) 0.0318(8) 0.0040(6) -0.0036(6) -0.0051(6) P4 0.0326(8) 0.0331(8) 0.0292(8) 0.0024(6) -0.0059(6) -0.0116(7) N11 0.025(2) 0.022(2) 0.039(3) 0.002(2) -0.003(2) -0.0044(19) N71 0.045(3) 0.023(2) 0.032(3) -0.007(2) -0.001(2) -0.016(2) N11' 0.027(2) 0.030(3) 0.036(3) 0.000(2) -0.005(2) -0.007(2) N71' 0.054(3) 0.026(2) 0.033(3) 0.001(2) -0.004(2) -0.019(2) O81 0.062(3) 0.034(2) 0.034(2) -0.0027(18) -0.004(2) -0.025(2) C21 0.028(3) 0.026(3) 0.032(3) 0.000(2) -0.005(2) -0.006(2) C31 0.032(3) 0.025(3) 0.036(3) -0.004(2) -0.001(3) -0.008(2) C41 0.039(3) 0.037(3) 0.033(3) -0.002(3) 0.001(3) -0.016(3) C51 0.044(4) 0.039(3) 0.032(3) 0.000(3) -0.002(3) -0.013(3) C61 0.038(3) 0.034(3) 0.039(3) 0.000(3) 0.002(3) -0.011(3) C81 0.030(3) 0.030(3) 0.034(3) -0.002(2) -0.004(2) -0.011(2) C4A 0.049(4) 0.069(5) 0.042(4) -0.005(3) -0.008(3) -0.032(4) C21' 0.036(3) 0.027(3) 0.037(3) 0.005(2) -0.012(3) -0.013(3) C31' 0.039(3) 0.033(3) 0.034(3) 0.003(3) -0.008(3) -0.014(3) C41' 0.043(4) 0.038(3) 0.040(4) 0.005(3) -0.011(3) -0.016(3) C51' 0.044(4) 0.043(4) 0.039(3) 0.001(3) 0.001(3) -0.025(3) C61' 0.037(3) 0.045(4) 0.033(3) 0.002(3) 0.000(3) -0.014(3) C4A' 0.079(5) 0.057(4) 0.047(4) 0.003(3) -0.004(4) -0.050(4) N12 0.031(3) 0.030(3) 0.032(3) -0.001(2) -0.001(2) -0.010(2) N72 0.037(3) 0.023(2) 0.036(3) -0.001(2) 0.000(2) 0.001(2) N12' 0.031(3) 0.032(3) 0.033(3) 0.000(2) -0.007(2) -0.005(2) N72' 0.031(3) 0.028(2) 0.034(3) -0.001(2) -0.006(2) 0.001(2) O82 0.079(4) 0.034(3) 0.050(3) 0.009(2) 0.020(3) 0.024(3) C22 0.029(3) 0.024(3) 0.041(3) 0.000(2) 0.001(3) -0.003(2) C32 0.027(3) 0.025(3) 0.039(3) 0.001(2) -0.005(3) -0.009(2) C42 0.028(3) 0.032(3) 0.038(3) 0.005(2) -0.009(3) -0.013(2) C52 0.039(4) 0.036(3) 0.038(3) 0.009(3) -0.008(3) -0.008(3) C62 0.032(3) 0.035(3) 0.040(3) 0.002(3) 0.003(3) -0.013(3) C82 0.033(3) 0.033(3) 0.034(3) -0.003(3) -0.005(3) -0.006(3) C4B 0.043(4) 0.026(3) 0.045(4) 0.006(3) -0.009(3) -0.009(3) C22' 0.030(3) 0.033(3) 0.032(3) -0.007(2) -0.002(3) -0.006(3) C32' 0.029(3) 0.027(3) 0.032(3) 0.001(2) -0.007(2) -0.005(2) C42' 0.025(3) 0.039(3) 0.039(3) -0.010(3) -0.001(3) -0.010(3) C52' 0.027(3) 0.039(3) 0.038(3) -0.006(3) 0.000(3) -0.007(3) C62' 0.032(3) 0.041(3) 0.036(3) 0.005(3) -0.007(3) -0.016(3) C4B' 0.034(3) 0.037(3) 0.047(4) -0.003(3) -0.002(3) -0.002(3) C100 0.042(4) 0.035(3) 0.060(4) 0.012(3) -0.012(3) -0.009(3) C101 0.038(4) 0.050(4) 0.063(5) 0.015(3) -0.020(3) -0.016(3) C102 0.048(4) 0.051(4) 0.041(4) 0.009(3) -0.010(3) -0.028(3) C103 0.032(3) 0.026(3) 0.052(4) -0.005(3) 0.006(3) -0.008(3) C104 0.041(4) 0.034(3) 0.052(4) -0.008(3) -0.008(3) -0.006(3) C105 0.042(4) 0.044(4) 0.061(5) -0.007(3) 0.001(3) -0.015(3) C106 0.045(4) 0.026(3) 0.075(5) -0.008(3) 0.005(4) -0.013(3) C107 0.041(4) 0.033(3) 0.069(5) 0.011(3) 0.007(4) -0.009(3) C108 0.041(4) 0.029(3) 0.045(4) -0.005(3) 0.005(3) -0.007(3) C109 0.039(4) 0.029(3) 0.050(4) -0.005(3) 0.007(3) -0.013(3) C110 0.048(4) 0.050(4) 0.073(5) -0.012(4) 0.018(4) -0.015(4) C111 0.071(6) 0.073(6) 0.071(6) -0.026(5) 0.029(5) -0.020(5) C112 0.076(7) 0.104(8) 0.069(6) -0.036(6) 0.034(6) -0.040(6) C113 0.101(7) 0.073(6) 0.040(4) -0.008(4) 0.001(4) -0.040(5) C114 0.057(4) 0.044(4) 0.044(4) -0.007(3) 0.007(3) -0.015(3) C115 0.033(3) 0.036(3) 0.032(3) 0.001(2) -0.005(3) -0.016(3) C116 0.047(4) 0.059(4) 0.042(4) 0.000(3) -0.010(3) -0.030(3) C117 0.050(4) 0.075(5) 0.047(4) 0.009(4) 0.003(3) -0.042(4) C118 0.058(5) 0.078(5) 0.040(4) 0.002(4) 0.010(4) -0.043(4) C119 0.069(5) 0.061(5) 0.037(4) 0.009(3) -0.019(4) -0.031(4) C120 0.037(3) 0.042(4) 0.042(4) 0.006(3) -0.009(3) -0.012(3) C121 0.041(4) 0.042(4) 0.040(4) -0.008(3) 0.002(3) -0.022(3) C122 0.081(6) 0.049(4) 0.044(4) -0.007(3) 0.012(4) -0.025(4) C123 0.139(10) 0.077(6) 0.061(6) -0.034(5) 0.035(6) -0.057(7) C124 0.097(7) 0.061(5) 0.080(6) -0.038(5) 0.027(6) -0.035(5) C125 0.058(5) 0.041(4) 0.090(7) -0.010(4) 0.012(5) -0.018(4) C126 0.052(4) 0.038(4) 0.054(4) -0.010(3) -0.002(3) -0.019(3) C127 0.026(3) 0.041(4) 0.057(4) 0.002(3) -0.006(3) -0.008(3) C128 0.033(3) 0.048(4) 0.058(4) 0.007(3) -0.016(3) -0.009(3) C129 0.036(3) 0.044(4) 0.038(3) -0.006(3) -0.004(3) -0.017(3) C130 0.038(3) 0.039(3) 0.032(3) 0.009(3) -0.006(3) -0.006(3) C131 0.049(4) 0.079(6) 0.046(4) -0.008(4) -0.003(3) -0.017(4) C132 0.064(5) 0.099(7) 0.036(4) -0.011(4) 0.004(4) -0.009(5) C133 0.094(7) 0.073(6) 0.062(6) -0.036(5) -0.017(5) -0.007(6) C134 0.081(6) 0.045(4) 0.070(6) -0.009(4) -0.027(5) -0.005(4) C135 0.058(4) 0.040(4) 0.041(4) -0.001(3) -0.019(3) -0.009(3) C136 0.039(3) 0.040(3) 0.029(3) 0.002(3) -0.001(3) -0.016(3) C137 0.041(4) 0.045(4) 0.040(4) 0.006(3) -0.005(3) 0.000(3) C138 0.066(5) 0.046(4) 0.051(4) 0.016(3) -0.018(4) -0.003(4) C139 0.073(6) 0.074(6) 0.041(4) 0.009(4) -0.003(4) -0.019(5) C140 0.065(5) 0.058(5) 0.047(4) 0.015(4) 0.016(4) 0.007(4) C141 0.053(4) 0.043(4) 0.042(4) 0.007(3) -0.002(3) -0.008(3) C142 0.047(4) 0.036(3) 0.031(3) 0.004(3) -0.010(3) -0.019(3) C143 0.038(4) 0.065(4) 0.035(3) 0.000(3) -0.001(3) -0.022(3) C144 0.062(5) 0.076(5) 0.046(4) -0.006(4) 0.006(4) -0.040(4) C145 0.074(6) 0.090(6) 0.035(4) -0.012(4) 0.004(4) -0.029(5) C146 0.071(5) 0.101(7) 0.035(4) -0.015(4) -0.009(4) -0.042(5) C147 0.048(4) 0.070(5) 0.039(4) -0.006(3) -0.011(3) -0.026(4) C148 0.042(4) 0.041(3) 0.039(3) 0.001(3) -0.016(3) -0.019(3) C149 0.042(4) 0.041(4) 0.052(4) -0.004(3) -0.012(3) -0.018(3) C150 0.059(5) 0.046(4) 0.083(6) 0.001(4) -0.037(5) -0.018(4) C151 0.076(6) 0.046(5) 0.091(7) 0.028(5) -0.044(5) -0.032(4) C152 0.083(6) 0.065(6) 0.074(6) 0.028(5) -0.033(5) -0.044(5) C153 0.055(4) 0.048(4) 0.048(4) 0.017(3) -0.014(3) -0.017(3) S11 0.0617(14) 0.0473(12) 0.126(2) 0.0091(13) 0.0199(15) -0.0034(11) O11 0.143(7) 0.149(7) 0.200(8) -0.029(6) -0.069(6) -0.071(6) O21 0.081(4) 0.054(4) 0.099(5) 0.002(3) -0.001(4) -0.006(3) O31 0.125(6) 0.101(5) 0.145(7) 0.035(5) 0.045(5) 0.001(5) F11 0.097(6) 0.166(9) 0.330(17) -0.050(10) -0.067(8) -0.036(6) F21 0.101(5) 0.080(4) 0.142(6) -0.001(4) 0.038(4) 0.015(4) F31 0.188(9) 0.141(7) 0.107(6) 0.031(5) 0.060(6) -0.028(7) C11 0.070(6) 0.078(6) 0.070(6) 0.004(5) -0.008(5) -0.012(5) S12 0.0394(10) 0.0691(13) 0.0594(12) 0.0158(10) -0.0042(9) -0.0153(9) O12 0.057(4) 0.116(5) 0.078(4) -0.001(4) 0.003(3) -0.043(4) O22 0.184(8) 0.121(6) 0.141(7) -0.006(5) -0.024(6) -0.093(6) O32 0.073(4) 0.169(7) 0.102(5) 0.053(5) -0.013(4) 0.003(5) F12 0.148(6) 0.180(7) 0.091(4) 0.061(5) -0.036(4) 0.001(5) F22 0.335(17) 0.138(8) 0.095(6) -0.026(6) 0.007(8) 0.033(10) F32 0.122(6) 0.270(9) 0.137(6) 0.045(6) 0.025(5) -0.060(6) C12 0.062(6) 0.116(10) 0.104(9) 0.056(8) 0.029(6) 0.026(6) S13 0.0545(10) 0.0544(10) 0.0296(8) 0.0021(7) -0.0113(7) -0.0202(9) O13 0.071(4) 0.136(6) 0.035(3) 0.012(3) -0.003(3) -0.042(4) O23 0.144(7) 0.080(4) 0.087(5) 0.022(4) -0.064(5) -0.062(5) O33 0.058(3) 0.073(3) 0.038(3) 0.005(2) -0.023(2) -0.026(3) F13 0.091(4) 0.201(6) 0.099(4) -0.025(4) -0.011(4) -0.029(4) F23 0.129(5) 0.103(4) 0.185(6) -0.033(4) -0.070(5) 0.005(4) F33 0.067(3) 0.126(5) 0.093(4) -0.017(4) -0.045(3) -0.004(3) C13 0.052(5) 0.101(8) 0.070(6) -0.035(5) -0.006(5) -0.021(5) S14 0.0475(19) 0.046(2) 0.0393(17) 0.0067(16) -0.0064(13) -0.0147(18) S14' 0.038(2) 0.056(3) 0.040(3) 0.010(3) -0.0041(19) -0.014(3) O14 0.072(2) 0.092(3) 0.071(2) 0.003(2) -0.0009(19) -0.028(2) O24 0.072(2) 0.092(3) 0.071(2) 0.003(2) -0.0009(19) -0.028(2) O34 0.072(2) 0.092(3) 0.071(2) 0.003(2) -0.0009(19) -0.028(2) F14 0.072(2) 0.155(4) 0.079(2) 0.032(2) -0.0147(18) -0.044(2) F24 0.072(2) 0.155(4) 0.079(2) 0.032(2) -0.0147(18) -0.044(2) F34 0.072(2) 0.155(4) 0.079(2) 0.032(2) -0.0147(18) -0.044(2) C14 0.039(5) 0.035(7) 0.031(5) 0.020(6) 0.004(4) -0.009(7) C14' 0.039(5) 0.035(7) 0.031(5) 0.020(6) 0.004(4) -0.009(7) N1 0.078(6) 0.152(10) 0.093(7) 0.002(7) -0.024(5) -0.031(6) O1 0.061(4) 0.101(5) 0.194(7) 0.049(5) -0.016(5) -0.024(4) C1 0.089(7) 0.113(8) 0.150(9) 0.048(7) -0.004(7) -0.037(6) C2 0.049(5) 0.082(7) 0.127(9) -0.001(6) -0.024(6) -0.016(5) C3 0.168(11) 0.175(11) 0.179(11) -0.003(8) -0.066(9) -0.037(8) N2 0.057(4) 0.033(3) 0.071(4) -0.003(3) -0.010(3) -0.020(3) O2 0.072(4) 0.037(3) 0.068(4) -0.009(2) 0.004(3) -0.020(3) C4 0.047(4) 0.037(4) 0.069(5) -0.009(3) -0.004(4) -0.012(3) C5 0.089(6) 0.062(5) 0.141(8) 0.004(5) -0.029(6) -0.017(5) C6 0.111(9) 0.080(7) 0.143(11) -0.029(7) -0.041(8) -0.038(7) N3 0.046(4) 0.083(5) 0.057(4) 0.019(4) -0.011(3) -0.027(3) O3 0.067(4) 0.134(7) 0.105(6) -0.031(5) -0.025(4) -0.036(4) C7 0.047(4) 0.065(5) 0.072(5) -0.012(4) -0.017(4) -0.020(4) C8 0.078(6) 0.135(8) 0.102(7) 0.012(6) -0.012(6) -0.034(6) C9 0.056(5) 0.103(7) 0.081(7) 0.003(6) -0.024(5) -0.035(5) O1W 0.054(4) 0.042(3) 0.068(4) -0.001(3) 0.009(3) 0.005(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pd1 N11 2.102(5) . ? Pd1 N12 2.099(5) . ? Pd1 P1 2.2720(15) . ? Pd1 P2 2.2781(16) . ? Pd2 N11' 2.102(5) . ? Pd2 N12' 2.108(5) . ? Pd2 P4 2.2705(16) . ? Pd2 P3 2.2826(15) . ? P1 C109 1.796(7) . ? P1 C100 1.823(7) . ? P1 C103 1.821(6) . ? P2 C115 1.802(6) . ? P2 C121 1.807(7) . ? P2 C102 1.815(7) . ? P3 C130 1.821(7) . ? P3 C136 1.821(6) . ? P3 C127 1.817(6) . ? P4 C148 1.818(7) . ? P4 C142 1.812(6) . ? P4 C129 1.830(6) . ? N11 C61 1.336(8) . ? N11 C21 1.340(8) . ? N71 C81 1.370(8) . ? N71 C31 1.415(8) . ? N71 H71 0.8800 . ? N11' C21' 1.328(8) . ? N11' C61' 1.350(8) . ? N71' C81 1.354(8) . ? N71' C31' 1.428(8) . ? N71' H71' 0.8800 . ? O81 C81 1.224(7) . ? C21 C31 1.399(8) . ? C21 H21 0.9500 . ? C31 C41 1.373(9) . ? C41 C51 1.416(9) . ? C41 C4A 1.500(9) . ? C51 C61 1.356(10) . ? C51 H51 0.9500 . ? C61 H61 0.9500 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C21' C31' 1.367(9) . ? C21' H21' 0.9500 . ? C31' C41' 1.400(9) . ? C41' C51' 1.405(9) . ? C41' C4A' 1.505(10) . ? C51' C61' 1.357(9) . ? C51' H51' 0.9500 . ? C61' H61' 0.9500 . ? C4A' H4A4 0.9800 . ? C4A' H4A5 0.9800 . ? C4A' H4A6 0.9800 . ? N12 C62 1.329(8) . ? N12 C22 1.337(8) . ? N72 C82 1.372(8) . ? N72 C32 1.385(8) . ? N72 H72 0.8800 . ? N12' C62' 1.335(8) . ? N12' C22' 1.347(8) . ? N72' C82 1.379(8) . ? N72' C32' 1.377(8) . ? N72' H72' 0.8800 . ? O82 C82 1.207(8) . ? C22 C32 1.404(8) . ? C22 H22 0.9500 . ? C32 C42 1.410(8) . ? C42 C52 1.384(9) . ? C42 C4B 1.485(8) . ? C52 C62 1.354(9) . ? C52 H52 0.9500 . ? C62 H62 0.9500 . ? C4B H4B1 0.9800 . ? C4B H4B2 0.9800 . ? C4B H4B3 0.9800 . ? C22' C32' 1.419(8) . ? C22' H22' 0.9500 . ? C32' C42' 1.415(8) . ? C42' C52' 1.406(9) . ? C42' C4B' 1.504(9) . ? C52' C62' 1.366(9) . ? C52' H52' 0.9500 . ? C62' H62' 0.9500 . ? C4B' H4B4 0.9800 . ? C4B' H4B5 0.9800 . ? C4B' H4B6 0.9800 . ? C100 C101 1.536(10) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? C101 C102 1.533(10) . ? C101 H10C 0.9900 . ? C101 H10D 0.9900 . ? C102 H10E 0.9900 . ? C102 H10F 0.9900 . ? C103 C108 1.407(9) . ? C103 C104 1.411(10) . ? C104 C105 1.400(10) . ? C104 H104 0.9500 . ? C105 C106 1.365(11) . ? C105 H105 0.9500 . ? C106 C107 1.392(12) . ? C106 H106 0.9500 . ? C107 C108 1.412(10) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C114 1.396(11) . ? C109 C110 1.398(10) . ? C110 C111 1.385(12) . ? C110 H110 0.9500 . ? C111 C112 1.351(15) . ? C111 H111 0.9500 . ? C112 C113 1.399(14) . ? C112 H112 0.9500 . ? C113 C114 1.387(11) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C115 C116 1.377(9) . ? C115 C120 1.400(9) . ? C116 C117 1.406(10) . ? C116 H116 0.9500 . ? C117 C118 1.302(11) . ? C117 H117 0.9500 . ? C118 C119 1.407(11) . ? C118 H118 0.9500 . ? C119 C120 1.393(10) . ? C119 H119 0.9500 . ? C120 H120 0.9500 . ? C121 C126 1.392(10) . ? C121 C122 1.394(10) . ? C122 C123 1.386(12) . ? C122 H122 0.9500 . ? C123 C124 1.410(14) . ? C123 H123 0.9500 . ? C124 C125 1.341(13) . ? C124 H124 0.9500 . ? C125 C126 1.399(10) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C127 C128 1.533(10) . ? C127 H12A 0.9900 . ? C127 H12B 0.9900 . ? C128 C129 1.526(9) . ? C128 H12C 0.9900 . ? C128 H12D 0.9900 . ? C129 H12E 0.9900 . ? C129 H12F 0.9900 . ? C130 C135 1.393(10) . ? C130 C131 1.389(10) . ? C131 C132 1.396(12) . ? C131 H131 0.9500 . ? C132 C133 1.326(14) . ? C132 H132 0.9500 . ? C133 C134 1.382(14) . ? C133 H133 0.9500 . ? C134 C135 1.373(11) . ? C134 H134 0.9500 . ? C135 H135 0.9500 . ? C136 C141 1.351(10) . ? C136 C137 1.384(9) . ? C137 C138 1.395(10) . ? C137 H137 0.9500 . ? C138 C139 1.355(12) . ? C138 H138 0.9500 . ? C139 C140 1.355(12) . ? C139 H139 0.9500 . ? C140 C141 1.393(10) . ? C140 H140 0.9500 . ? C141 H141 0.9500 . ? C142 C143 1.369(9) . ? C142 C147 1.396(9) . ? C143 C144 1.379(10) . ? C143 H143 0.9500 . ? C144 C145 1.374(12) . ? C144 H144 0.9500 . ? C145 C146 1.412(12) . ? C145 H145 0.9500 . ? C146 C147 1.389(10) . ? C146 H146 0.9500 . ? C147 H147 0.9500 . ? C148 C149 1.394(10) . ? C148 C153 1.381(10) . ? C149 C150 1.375(10) . ? C149 H149 0.9500 . ? C150 C151 1.419(13) . ? C150 H150 0.9500 . ? C151 C152 1.361(14) . ? C151 H151 0.9500 . ? C152 C153 1.404(11) . ? C152 H152 0.9500 . ? C153 H153 0.9500 . ? S11 O31 1.4485(11) . ? S11 O21 1.4488(10) . ? S11 O11 1.4505(11) . ? S11 C11 1.764(11) . ? F11 C11 1.332(14) . ? F21 C11 1.311(11) . ? F31 C11 1.267(12) . ? S12 O12 1.397(6) . ? S12 O22 1.424(10) . ? S12 O32 1.4488(10) . ? S12 C12 1.752(10) . ? F12 C12 1.3345(11) . ? F22 C12 1.3346(11) . ? F32 C12 1.3344(11) . ? S13 O13 1.424(6) . ? S13 O33 1.437(5) . ? S13 O23 1.441(7) . ? S13 C13 1.796(10) . ? F13 C13 1.299(12) . ? F23 C13 1.277(13) . ? F33 C13 1.306(10) . ? S14 O14 1.4486(11) . ? S14 O34 1.453(7) . ? S14 O24 1.4498(11) . ? S14 C14 1.798(14) . ? S14' O14 1.421(8) . ? S14' O34 1.411(8) . ? S14' C14' 1.90(2) . ? S14' F24 2.016(9) . ? S14' O24 2.214(6) . ? O24 C14' 2.01(2) . ? F14 C14' 1.28(2) . ? F14 C14 1.303(13) . ? F24 C14 1.3355(11) . ? F34 C14' 1.34(2) . ? F34 C14 1.328(13) . ? N1 C1 1.2897(11) . ? N1 C2 1.446(13) . ? N1 C3 1.51(2) . ? O1 C1 1.229(15) . ? C1 H1 0.9500 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? N2 C4 1.273(9) . ? N2 C5 1.432(12) . ? N2 C6 1.474(12) . ? O2 C4 1.196(9) . ? C4 H4 0.9500 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? N3 C7 1.297(10) . ? N3 C8 1.406(13) . ? N3 C9 1.447(12) . ? O3 C7 1.234(10) . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O4 C18 1.3597(11) . ? O4 C16 1.3600(11) . ? C16 C17 1.4899(11) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.4899(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? O1W H1W 0.846(11) . ? O1W H2W 0.840(11) . ? 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 N11 Pd1 N12 86.71(18) . . ? N11 Pd1 P1 91.52(13) . . ? N12 Pd1 P1 178.11(14) . . ? N11 Pd1 P2 179.08(14) . . ? N12 Pd1 P2 92.42(14) . . ? P1 Pd1 P2 89.35(6) . . ? N11' Pd2 N12' 88.41(19) . . ? N11' Pd2 P4 176.84(14) . . ? N12' Pd2 P4 89.39(15) . . ? N11' Pd2 P3 89.91(13) . . ? N12' Pd2 P3 178.24(14) . . ? P4 Pd2 P3 92.27(6) . . ? C109 P1 C100 108.2(3) . . ? C109 P1 C103 105.0(3) . . ? C100 P1 C103 104.8(3) . . ? C109 P1 Pd1 112.7(2) . . ? C100 P1 Pd1 113.4(2) . . ? C103 P1 Pd1 112.0(2) . . ? C115 P2 C121 105.3(3) . . ? C115 P2 C102 106.0(3) . . ? C121 P2 C102 103.8(3) . . ? C115 P2 Pd1 115.0(2) . . ? C121 P2 Pd1 112.3(2) . . ? C102 P2 Pd1 113.4(2) . . ? C130 P3 C136 106.6(3) . . ? C130 P3 C127 102.6(3) . . ? C136 P3 C127 105.0(3) . . ? C130 P3 Pd2 111.8(2) . . ? C136 P3 Pd2 113.6(2) . . ? C127 P3 Pd2 116.2(2) . . ? C148 P4 C142 106.6(3) . . ? C148 P4 C129 103.3(3) . . ? C142 P4 C129 105.9(3) . . ? C148 P4 Pd2 111.7(2) . . ? C142 P4 Pd2 112.3(2) . . ? C129 P4 Pd2 116.3(2) . . ? C61 N11 C21 119.4(5) . . ? C61 N11 Pd1 121.1(4) . . ? C21 N11 Pd1 119.2(4) . . ? C81 N71 C31 123.9(5) . . ? C81 N71 H71 118.0 . . ? C31 N71 H71 118.0 . . ? C21' N11' C61' 119.4(5) . . ? C21' N11' Pd2 117.8(4) . . ? C61' N11' Pd2 122.2(4) . . ? C81 N71' C31' 124.7(5) . . ? C81 N71' H71' 117.7 . . ? C31' N71' H71' 117.7 . . ? N11 C21 C31 120.6(5) . . ? N11 C21 H21 119.7 . . ? C31 C21 H21 119.7 . . ? C41 C31 C21 120.3(6) . . ? C41 C31 N71 119.6(5) . . ? C21 C31 N71 120.1(5) . . ? C31 C41 C51 117.5(6) . . ? C31 C41 C4A 122.0(6) . . ? C51 C41 C4A 120.5(6) . . ? C61 C51 C41 119.1(6) . . ? C61 C51 H51 120.4 . . ? C41 C51 H51 120.4 . . ? N11 C61 C51 123.0(6) . . ? N11 C61 H61 118.5 . . ? C51 C61 H61 118.5 . . ? O81 C81 N71' 124.9(6) . . ? O81 C81 N71 122.6(5) . . ? N71' C81 N71 112.5(5) . . ? C41 C4A H4A1 109.5 . . ? C41 C4A H4A2 109.5 . . ? H4A1 C4A H4A2 109.5 . . ? C41 C4A H4A3 109.5 . . ? H4A1 C4A H4A3 109.5 . . ? H4A2 C4A H4A3 109.5 . . ? N11' C21' C31' 122.3(6) . . ? N11' C21' H21' 118.8 . . ? C31' C21' H21' 118.8 . . ? C21' C31' C41' 120.5(6) . . ? C21' C31' N71' 120.9(5) . . ? C41' C31' N71' 118.6(6) . . ? C51' C41' C31' 115.2(6) . . ? C51' C41' C4A' 122.7(6) . . ? C31' C41' C4A' 122.0(6) . . ? C61' C51' C41' 122.0(6) . . ? C61' C51' H51' 119.0 . . ? C41' C51' H51' 119.0 . . ? N11' C61' C51' 120.6(6) . . ? N11' C61' H61' 119.7 . . ? C51' C61' H61' 119.7 . . ? C41' C4A' H4A4 109.5 . . ? C41' C4A' H4A5 109.5 . . ? H4A4 C4A' H4A5 109.5 . . ? C41' C4A' H4A6 109.5 . . ? H4A4 C4A' H4A6 109.5 . . ? H4A5 C4A' H4A6 109.5 . . ? C62 N12 C22 118.8(5) . . ? C62 N12 Pd1 122.2(4) . . ? C22 N12 Pd1 119.0(4) . . ? C82 N72 C32 127.3(5) . . ? C82 N72 H72 116.3 . . ? C32 N72 H72 116.3 . . ? C62' N12' C22' 120.1(5) . . ? C62' N12' Pd2 122.1(4) . . ? C22' N12' Pd2 117.4(4) . . ? C82 N72' C32' 125.9(5) . . ? C82 N72' H72' 117.1 . . ? C32' N72' H72' 117.1 . . ? N12 C22 C32 122.6(5) . . ? N12 C22 H22 118.7 . . ? C32 C22 H22 118.7 . . ? N72 C32 C22 123.0(5) . . ? N72 C32 C42 119.0(5) . . ? C22 C32 C42 118.0(5) . . ? C52 C42 C32 116.7(5) . . ? C52 C42 C4B 122.4(5) . . ? C32 C42 C4B 120.9(5) . . ? C62 C52 C42 121.8(6) . . ? C62 C52 H52 119.1 . . ? C42 C52 H52 119.1 . . ? N12 C62 C52 122.0(6) . . ? N12 C62 H62 119.0 . . ? C52 C62 H62 119.0 . . ? O82 C82 N72 123.6(6) . . ? O82 C82 N72' 123.5(6) . . ? N72 C82 N72' 112.9(5) . . ? C42 C4B H4B1 109.5 . . ? C42 C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C42 C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? N12' C22' C32' 121.1(5) . . ? N12' C22' H22' 119.4 . . ? C32' C22' H22' 119.4 . . ? N72' C32' C22' 123.2(5) . . ? N72' C32' C42' 118.3(5) . . ? C22' C32' C42' 118.4(5) . . ? C52' C42' C32' 117.5(5) . . ? C52' C42' C4B' 120.3(5) . . ? C32' C42' C4B' 122.2(6) . . ? C62' C52' C42' 120.3(6) . . ? C62' C52' H52' 119.8 . . ? C42' C52' H52' 119.8 . . ? N12' C62' C52' 122.3(6) . . ? N12' C62' H62' 118.9 . . ? C52' C62' H62' 118.9 . . ? C42' C4B' H4B4 109.5 . . ? C42' C4B' H4B5 109.5 . . ? H4B4 C4B' H4B5 109.5 . . ? C42' C4B' H4B6 109.5 . . ? H4B4 C4B' H4B6 109.5 . . ? H4B5 C4B' H4B6 109.5 . . ? C101 C100 P1 116.0(5) . . ? C101 C100 H10A 108.3 . . ? P1 C100 H10A 108.3 . . ? C101 C100 H10B 108.3 . . ? P1 C100 H10B 108.3 . . ? H10A C100 H10B 107.4 . . ? C102 C101 C100 114.4(6) . . ? C102 C101 H10C 108.7 . . ? C100 C101 H10C 108.7 . . ? C102 C101 H10D 108.7 . . ? C100 C101 H10D 108.7 . . ? H10C C101 H10D 107.6 . . ? C101 C102 P2 114.2(5) . . ? C101 C102 H10E 108.7 . . ? P2 C102 H10E 108.7 . . ? C101 C102 H10F 108.7 . . ? P2 C102 H10F 108.7 . . ? H10E C102 H10F 107.6 . . ? C108 C103 C104 120.1(6) . . ? C108 C103 P1 120.4(5) . . ? C104 C103 P1 119.3(5) . . ? C105 C104 C103 119.3(7) . . ? C105 C104 H104 120.3 . . ? C103 C104 H104 120.3 . . ? C106 C105 C104 121.1(7) . . ? C106 C105 H105 119.4 . . ? C104 C105 H105 119.4 . . ? C105 C106 C107 120.1(7) . . ? C105 C106 H106 120.0 . . ? C107 C106 H106 120.0 . . ? C106 C107 C108 120.9(7) . . ? C106 C107 H107 119.6 . . ? C108 C107 H107 119.6 . . ? C103 C108 C107 118.5(7) . . ? C103 C108 H108 120.8 . . ? C107 C108 H108 120.8 . . ? C114 C109 C110 118.7(7) . . ? C114 C109 P1 119.0(5) . . ? C110 C109 P1 122.3(6) . . ? C111 C110 C109 119.6(9) . . ? C111 C110 H110 120.2 . . ? C109 C110 H110 120.2 . . ? C110 C111 C112 122.1(9) . . ? C110 C111 H111 118.9 . . ? C112 C111 H111 118.9 . . ? C111 C112 C113 119.1(9) . . ? C111 C112 H112 120.5 . . ? C113 C112 H112 120.5 . . ? C114 C113 C112 120.1(9) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C109 C114 C113 120.3(8) . . ? C109 C114 H114 119.8 . . ? C113 C114 H114 119.8 . . ? C116 C115 C120 119.4(6) . . ? C116 C115 P2 121.7(5) . . ? C120 C115 P2 118.8(5) . . ? C117 C116 C115 119.1(6) . . ? C117 C116 H116 120.4 . . ? C115 C116 H116 120.4 . . ? C118 C117 C116 121.8(7) . . ? C118 C117 H117 119.1 . . ? C116 C117 H117 119.1 . . ? C119 C118 C117 121.0(7) . . ? C119 C118 H118 119.5 . . ? C117 C118 H118 119.5 . . ? C118 C119 C120 118.7(7) . . ? C118 C119 H119 120.6 . . ? C120 C119 H119 120.6 . . ? C115 C120 C119 119.8(6) . . ? C115 C120 H120 120.1 . . ? C119 C120 H120 120.1 . . ? C126 C121 C122 117.9(6) . . ? C126 C121 P2 121.4(5) . . ? C122 C121 P2 120.4(5) . . ? C123 C122 C121 122.0(8) . . ? C123 C122 H122 119.0 . . ? C121 C122 H122 119.0 . . ? C124 C123 C122 117.8(8) . . ? C124 C123 H123 121.1 . . ? C122 C123 H123 121.1 . . ? C125 C124 C123 121.5(8) . . ? C125 C124 H124 119.3 . . ? C123 C124 H124 119.3 . . ? C124 C125 C126 120.1(8) . . ? C124 C125 H125 119.9 . . ? C126 C125 H125 119.9 . . ? C121 C126 C125 120.7(7) . . ? C121 C126 H126 119.6 . . ? C125 C126 H126 119.6 . . ? C128 C127 P3 113.8(5) . . ? C128 C127 H12A 108.8 . . ? P3 C127 H12A 108.8 . . ? C128 C127 H12B 108.8 . . ? P3 C127 H12B 108.8 . . ? H12A C127 H12B 107.7 . . ? C129 C128 C127 113.3(6) . . ? C129 C128 H12C 108.9 . . ? C127 C128 H12C 108.9 . . ? C129 C128 H12D 108.9 . . ? C127 C128 H12D 108.9 . . ? H12C C128 H12D 107.7 . . ? C128 C129 P4 113.4(5) . . ? C128 C129 H12E 108.9 . . ? P4 C129 H12E 108.9 . . ? C128 C129 H12F 108.9 . . ? P4 C129 H12F 108.9 . . ? H12E C129 H12F 107.7 . . ? C135 C130 C131 120.1(7) . . ? C135 C130 P3 121.2(5) . . ? C131 C130 P3 118.3(6) . . ? C130 C131 C132 116.9(9) . . ? C130 C131 H131 121.5 . . ? C132 C131 H131 121.5 . . ? C133 C132 C131 123.1(8) . . ? C133 C132 H132 118.5 . . ? C131 C132 H132 118.5 . . ? C132 C133 C134 120.2(8) . . ? C132 C133 H133 119.9 . . ? C134 C133 H133 119.9 . . ? C133 C134 C135 119.2(9) . . ? C133 C134 H134 120.4 . . ? C135 C134 H134 120.4 . . ? C130 C135 C134 120.4(7) . . ? C130 C135 H135 119.8 . . ? C134 C135 H135 119.8 . . ? C141 C136 C137 119.4(6) . . ? C141 C136 P3 120.7(5) . . ? C137 C136 P3 119.9(5) . . ? C138 C137 C136 119.7(6) . . ? C138 C137 H137 120.2 . . ? C136 C137 H137 120.2 . . ? C139 C138 C137 120.2(7) . . ? C139 C138 H138 119.9 . . ? C137 C138 H138 119.9 . . ? C138 C139 C140 119.9(7) . . ? C138 C139 H139 120.1 . . ? C140 C139 H139 120.1 . . ? C139 C140 C141 120.5(7) . . ? C139 C140 H140 119.7 . . ? C141 C140 H140 119.7 . . ? C136 C141 C140 120.3(7) . . ? C136 C141 H141 119.9 . . ? C140 C141 H141 119.9 . . ? C143 C142 C147 119.9(6) . . ? C143 C142 P4 121.0(5) . . ? C147 C142 P4 119.1(5) . . ? C144 C143 C142 121.3(7) . . ? C144 C143 H143 119.3 . . ? C142 C143 H143 119.3 . . ? C145 C144 C143 119.6(7) . . ? C145 C144 H144 120.2 . . ? C143 C144 H144 120.2 . . ? C144 C145 C146 120.1(7) . . ? C144 C145 H145 120.0 . . ? C146 C145 H145 120.0 . . ? C147 C146 C145 119.3(7) . . ? C147 C146 H146 120.3 . . ? C145 C146 H146 120.3 . . ? C146 C147 C142 119.6(7) . . ? C146 C147 H147 120.2 . . ? C142 C147 H147 120.2 . . ? C149 C148 C153 119.8(6) . . ? C149 C148 P4 121.0(5) . . ? C153 C148 P4 119.2(5) . . ? C148 C149 C150 121.4(7) . . ? C148 C149 H149 119.3 . . ? C150 C149 H149 119.3 . . ? C149 C150 C151 118.4(8) . . ? C149 C150 H150 120.8 . . ? C151 C150 H150 120.8 . . ? C152 C151 C150 120.4(7) . . ? C152 C151 H151 119.8 . . ? C150 C151 H151 119.8 . . ? C151 C152 C153 120.7(9) . . ? C151 C152 H152 119.7 . . ? C153 C152 H152 119.7 . . ? C148 C153 C152 119.3(8) . . ? C148 C153 H153 120.3 . . ? C152 C153 H153 120.3 . . ? O31 S11 O21 117.6(5) . . ? O31 S11 O11 114.7(7) . . ? O21 S11 O11 111.7(6) . . ? O31 S11 C11 105.7(5) . . ? O21 S11 C11 105.1(5) . . ? O11 S11 C11 99.7(6) . . ? F31 C11 F21 110.2(9) . . ? F31 C11 F11 99.6(11) . . ? F21 C11 F11 108.0(10) . . ? F31 C11 S11 113.0(8) . . ? F21 C11 S11 112.4(8) . . ? F11 C11 S11 112.8(9) . . ? O12 S12 O22 113.1(6) . . ? O12 S12 O32 115.8(5) . . ? O22 S12 O32 112.5(7) . . ? O12 S12 C12 102.2(4) . . ? O22 S12 C12 105.2(5) . . ? O32 S12 C12 106.6(4) . . ? F32 C12 F12 104.5(8) . . ? F32 C12 F22 105.8(11) . . ? F12 C12 F22 102.7(9) . . ? F32 C12 S12 112.4(7) . . ? F12 C12 S12 114.2(7) . . ? F22 C12 S12 116.0(6) . . ? O13 S13 O33 115.7(4) . . ? O13 S13 O23 113.6(4) . . ? O33 S13 O23 115.3(3) . . ? O13 S13 C13 102.5(5) . . ? O33 S13 C13 103.6(4) . . ? O23 S13 C13 103.6(5) . . ? F23 C13 F13 102.7(9) . . ? F23 C13 F33 110.3(10) . . ? F13 C13 F33 107.0(8) . . ? F23 C13 S13 110.5(7) . . ? F13 C13 S13 111.6(9) . . ? F33 C13 S13 114.0(6) . . ? O14 S14 O34 118.8(4) . . ? O14 S14 O24 109.5(5) . . ? O34 S14 O24 115.5(4) . . ? O14 S14 C14 107.4(5) . . ? O34 S14 C14 101.9(5) . . ? O24 S14 C14 101.5(4) . . ? O14 S14' O34 123.6(6) . . ? O14 S14' C14' 110.2(7) . . ? O34 S14' C14' 102.0(7) . . ? O14 S14' F24 118.8(5) . . ? O34 S14' F24 116.7(5) . . ? C14' S14' F24 63.3(7) . . ? O14 S14' O24 77.9(4) . . ? O34 S14' O24 82.0(4) . . ? C14' S14' O24 58.0(7) . . ? F24 S14' O24 121.0(4) . . ? S14' O14 S14 31.3(2) . . ? S14 O24 C14' 56.9(6) . . ? S14 O24 S14' 4.0(3) . . ? C14' O24 S14' 53.1(5) . . ? S14' O34 S14 31.3(3) . . ? C14' F14 C14 32.5(8) . . ? C14 F24 S14' 55.0(6) . . ? C14' F34 C14 31.5(8) . . ? F34 C14 F14 108.0(9) . . ? F34 C14 F24 106.5(8) . . ? F14 C14 F24 105.0(9) . . ? F34 C14 S14 113.6(8) . . ? F14 C14 S14 113.9(7) . . ? F24 C14 S14 109.2(8) . . ? F14 C14' F34 109.0(17) . . ? F14 C14' O24 131.0(12) . . ? F34 C14' O24 118.3(14) . . ? F14 C14' S14' 108.1(12) . . ? F34 C14' S14' 108.7(10) . . ? O24 C14' S14' 68.9(8) . . ? C1 N1 C2 126.6(12) . . ? C1 N1 C3 113.1(14) . . ? C2 N1 C3 119.6(12) . . ? N1 C1 O1 121.5(15) . . ? N1 C1 H1 119.2 . . ? O1 C1 H1 119.2 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 N2 C5 120.2(8) . . ? C4 N2 C6 125.2(8) . . ? C5 N2 C6 114.6(8) . . ? O2 C4 N2 128.1(8) . . ? O2 C4 H4 116.0 . . ? N2 C4 H4 116.0 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C7 N3 C8 122.7(9) . . ? C7 N3 C9 120.0(8) . . ? C8 N3 C9 116.5(8) . . ? O3 C7 N3 123.2(9) . . ? O3 C7 H7 118.4 . . ? N3 C7 H7 118.4 . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C18 O4 C16 116.7(14) . . ? C17 C16 O4 110.9(17) . . ? C17 C16 H16A 109.5 . . ? O4 C16 H16A 109.4 . . ? C17 C16 H16B 109.5 . . ? O4 C16 H16B 109.5 . . ? H16A C16 H16B 108.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O4 C18 C19 122.0(17) . . ? O4 C18 H18A 106.8 . . ? C19 C18 H18A 106.8 . . ? O4 C18 H18B 106.8 . . ? C19 C18 H18B 106.8 . . ? H18A C18 H18B 106.7 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? H1W O1W H2W 106(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Pd1 P1 C109 102.3(3) . . . . ? N12 Pd1 P1 C109 123(4) . . . . ? P2 Pd1 P1 C109 -78.0(3) . . . . ? N11 Pd1 P1 C100 -134.3(3) . . . . ? N12 Pd1 P1 C100 -114(4) . . . . ? P2 Pd1 P1 C100 45.4(3) . . . . ? N11 Pd1 P1 C103 -15.9(3) . . . . ? N12 Pd1 P1 C103 4(4) . . . . ? P2 Pd1 P1 C103 163.8(3) . . . . ? N11 Pd1 P2 C115 -123(9) . . . . ? N12 Pd1 P2 C115 -105.9(3) . . . . ? P1 Pd1 P2 C115 74.8(2) . . . . ? N11 Pd1 P2 C121 -3(9) . . . . ? N12 Pd1 P2 C121 14.6(3) . . . . ? P1 Pd1 P2 C121 -164.7(3) . . . . ? N11 Pd1 P2 C102 115(9) . . . . ? N12 Pd1 P2 C102 131.9(3) . . . . ? P1 Pd1 P2 C102 -47.4(3) . . . . ? N11' Pd2 P3 C130 27.0(3) . . . . ? N12' Pd2 P3 C130 10(5) . . . . ? P4 Pd2 P3 C130 -150.8(2) . . . . ? N11' Pd2 P3 C136 -93.7(3) . . . . ? N12' Pd2 P3 C136 -111(5) . . . . ? P4 Pd2 P3 C136 88.6(2) . . . . ? N11' Pd2 P3 C127 144.3(3) . . . . ? N12' Pd2 P3 C127 127(5) . . . . ? P4 Pd2 P3 C127 -33.4(3) . . . . ? N11' Pd2 P4 C148 18(2) . . . . ? N12' Pd2 P4 C148 -27.6(3) . . . . ? P3 Pd2 P4 C148 151.8(2) . . . . ? N11' Pd2 P4 C142 138(2) . . . . ? N12' Pd2 P4 C142 92.0(3) . . . . ? P3 Pd2 P4 C142 -88.6(2) . . . . ? N11' Pd2 P4 C129 -100(2) . . . . ? N12' Pd2 P4 C129 -145.8(3) . . . . ? P3 Pd2 P4 C129 33.6(2) . . . . ? N12 Pd1 N11 C61 85.5(4) . . . . ? P1 Pd1 N11 C61 -95.1(4) . . . . ? P2 Pd1 N11 C61 103(9) . . . . ? N12 Pd1 N11 C21 -99.6(4) . . . . ? P1 Pd1 N11 C21 79.8(4) . . . . ? P2 Pd1 N11 C21 -82(9) . . . . ? N12' Pd2 N11' C21' 88.4(4) . . . . ? P4 Pd2 N11' C21' 43(3) . . . . ? P3 Pd2 N11' C21' -91.1(4) . . . . ? N12' Pd2 N11' C61' -100.4(5) . . . . ? P4 Pd2 N11' C61' -146(2) . . . . ? P3 Pd2 N11' C61' 80.1(4) . . . . ? C61 N11 C21 C31 3.1(8) . . . . ? Pd1 N11 C21 C31 -171.9(4) . . . . ? N11 C21 C31 C41 -1.1(8) . . . . ? N11 C21 C31 N71 176.9(5) . . . . ? C81 N71 C31 C41 -147.4(6) . . . . ? C81 N71 C31 C21 34.6(8) . . . . ? C21 C31 C41 C51 -1.7(9) . . . . ? N71 C31 C41 C51 -179.7(5) . . . . ? C21 C31 C41 C4A 178.0(6) . . . . ? N71 C31 C41 C4A 0.0(9) . . . . ? C31 C41 C51 C61 2.6(9) . . . . ? C4A C41 C51 C61 -177.2(6) . . . . ? C21 N11 C61 C51 -2.2(9) . . . . ? Pd1 N11 C61 C51 172.7(5) . . . . ? C41 C51 C61 N11 -0.7(10) . . . . ? C31' N71' C81 O81 7.8(10) . . . . ? C31' N71' C81 N71 -170.3(5) . . . . ? C31 N71 C81 O81 5.4(9) . . . . ? C31 N71 C81 N71' -176.4(5) . . . . ? C61' N11' C21' C31' 0.5(9) . . . . ? Pd2 N11' C21' C31' 172.0(5) . . . . ? N11' C21' C31' C41' -1.7(9) . . . . ? N11' C21' C31' N71' -179.5(5) . . . . ? C81 N71' C31' C21' -31.0(9) . . . . ? C81 N71' C31' C41' 151.2(6) . . . . ? C21' C31' C41' C51' 0.9(9) . . . . ? N71' C31' C41' C51' 178.7(6) . . . . ? C21' C31' C41' C4A' -174.3(7) . . . . ? N71' C31' C41' C4A' 3.5(10) . . . . ? C31' C41' C51' C61' 1.0(10) . . . . ? C4A' C41' C51' C61' 176.2(7) . . . . ? C21' N11' C61' C51' 1.5(9) . . . . ? Pd2 N11' C61' C51' -169.6(5) . . . . ? C41' C51' C61' N11' -2.3(10) . . . . ? N11 Pd1 N12 C62 -102.1(5) . . . . ? P1 Pd1 N12 C62 -122(4) . . . . ? P2 Pd1 N12 C62 78.2(5) . . . . ? N11 Pd1 N12 C22 76.7(5) . . . . ? P1 Pd1 N12 C22 56(5) . . . . ? P2 Pd1 N12 C22 -103.0(4) . . . . ? N11' Pd2 N12' C62' 98.3(5) . . . . ? P4 Pd2 N12' C62' -84.0(5) . . . . ? P3 Pd2 N12' C62' 115(5) . . . . ? N11' Pd2 N12' C22' -88.8(5) . . . . ? P4 Pd2 N12' C22' 89.0(4) . . . . ? P3 Pd2 N12' C22' -72(5) . . . . ? C62 N12 C22 C32 -2.2(9) . . . . ? Pd1 N12 C22 C32 178.9(5) . . . . ? C82 N72 C32 C22 -3.7(10) . . . . ? C82 N72 C32 C42 174.8(6) . . . . ? N12 C22 C32 N72 177.7(6) . . . . ? N12 C22 C32 C42 -0.8(9) . . . . ? N72 C32 C42 C52 -176.6(6) . . . . ? C22 C32 C42 C52 1.9(8) . . . . ? N72 C32 C42 C4B 4.4(9) . . . . ? C22 C32 C42 C4B -177.1(6) . . . . ? C32 C42 C52 C62 -0.2(9) . . . . ? C4B C42 C52 C62 178.8(6) . . . . ? C22 N12 C62 C52 4.1(9) . . . . ? Pd1 N12 C62 C52 -177.1(5) . . . . ? C42 C52 C62 N12 -2.9(10) . . . . ? C32 N72 C82 O82 -2.8(11) . . . . ? C32 N72 C82 N72' 179.8(6) . . . . ? C32' N72' C82 O82 3.5(11) . . . . ? C32' N72' C82 N72 -179.1(6) . . . . ? C62' N12' C22' C32' 2.2(9) . . . . ? Pd2 N12' C22' C32' -170.8(4) . . . . ? C82 N72' C32' C22' 7.9(10) . . . . ? C82 N72' C32' C42' -174.5(6) . . . . ? N12' C22' C32' N72' 179.7(6) . . . . ? N12' C22' C32' C42' 2.1(9) . . . . ? N72' C32' C42' C52' 178.2(6) . . . . ? C22' C32' C42' C52' -4.1(9) . . . . ? N72' C32' C42' C4B' -4.0(9) . . . . ? C22' C32' C42' C4B' 173.8(6) . . . . ? C32' C42' C52' C62' 2.1(9) . . . . ? C4B' C42' C52' C62' -175.9(6) . . . . ? C22' N12' C62' C52' -4.5(9) . . . . ? Pd2 N12' C62' C52' 168.2(5) . . . . ? C42' C52' C62' N12' 2.3(10) . . . . ? C109 P1 C100 C101 65.5(6) . . . . ? C103 P1 C100 C101 177.1(5) . . . . ? Pd1 P1 C100 C101 -60.4(6) . . . . ? P1 C100 C101 C102 67.1(8) . . . . ? C100 C101 C102 P2 -68.4(7) . . . . ? C115 P2 C102 C101 -63.2(5) . . . . ? C121 P2 C102 C101 -174.0(5) . . . . ? Pd1 P2 C102 C101 63.9(5) . . . . ? C109 P1 C103 C108 149.5(5) . . . . ? C100 P1 C103 C108 35.6(6) . . . . ? Pd1 P1 C103 C108 -87.8(5) . . . . ? C109 P1 C103 C104 -35.8(6) . . . . ? C100 P1 C103 C104 -149.7(5) . . . . ? Pd1 P1 C103 C104 86.9(5) . . . . ? C108 C103 C104 C105 -0.2(9) . . . . ? P1 C103 C104 C105 -174.9(5) . . . . ? C103 C104 C105 C106 0.5(10) . . . . ? C104 C105 C106 C107 -1.0(11) . . . . ? C105 C106 C107 C108 1.2(10) . . . . ? C104 C103 C108 C107 0.4(9) . . . . ? P1 C103 C108 C107 175.0(5) . . . . ? C106 C107 C108 C103 -0.9(10) . . . . ? C100 P1 C109 C114 -162.8(5) . . . . ? C103 P1 C109 C114 85.7(6) . . . . ? Pd1 P1 C109 C114 -36.6(6) . . . . ? C100 P1 C109 C110 18.3(7) . . . . ? C103 P1 C109 C110 -93.1(6) . . . . ? Pd1 P1 C109 C110 144.6(5) . . . . ? C114 C109 C110 C111 0.4(11) . . . . ? P1 C109 C110 C111 179.2(6) . . . . ? C109 C110 C111 C112 -0.7(14) . . . . ? C110 C111 C112 C113 -0.5(16) . . . . ? C111 C112 C113 C114 2.2(15) . . . . ? C110 C109 C114 C113 1.3(11) . . . . ? P1 C109 C114 C113 -177.6(6) . . . . ? C112 C113 C114 C109 -2.6(13) . . . . ? C121 P2 C115 C116 79.5(6) . . . . ? C102 P2 C115 C116 -30.1(6) . . . . ? Pd1 P2 C115 C116 -156.3(5) . . . . ? C121 P2 C115 C120 -99.5(5) . . . . ? C102 P2 C115 C120 150.8(5) . . . . ? Pd1 P2 C115 C120 24.7(6) . . . . ? C120 C115 C116 C117 -1.0(10) . . . . ? P2 C115 C116 C117 180.0(6) . . . . ? C115 C116 C117 C118 -0.8(12) . . . . ? C116 C117 C118 C119 3.4(13) . . . . ? C117 C118 C119 C120 -4.1(12) . . . . ? C116 C115 C120 C119 0.1(10) . . . . ? P2 C115 C120 C119 179.2(5) . . . . ? C118 C119 C120 C115 2.3(11) . . . . ? C115 P2 C121 C126 17.5(7) . . . . ? C102 P2 C121 C126 128.7(6) . . . . ? Pd1 P2 C121 C126 -108.5(6) . . . . ? C115 P2 C121 C122 -169.5(6) . . . . ? C102 P2 C121 C122 -58.3(7) . . . . ? Pd1 P2 C121 C122 64.5(7) . . . . ? C126 C121 C122 C123 -2.4(14) . . . . ? P2 C121 C122 C123 -175.6(9) . . . . ? C121 C122 C123 C124 3.1(17) . . . . ? C122 C123 C124 C125 -2.8(18) . . . . ? C123 C124 C125 C126 1.9(16) . . . . ? C122 C121 C126 C125 1.3(11) . . . . ? P2 C121 C126 C125 174.5(6) . . . . ? C124 C125 C126 C121 -1.1(13) . . . . ? C130 P3 C127 C128 177.7(5) . . . . ? C136 P3 C127 C128 -71.1(5) . . . . ? Pd2 P3 C127 C128 55.3(6) . . . . ? P3 C127 C128 C129 -74.5(7) . . . . ? C127 C128 C129 P4 74.5(7) . . . . ? C148 P4 C129 C128 -178.7(5) . . . . ? C142 P4 C129 C128 69.4(5) . . . . ? Pd2 P4 C129 C128 -56.1(5) . . . . ? C136 P3 C130 C135 24.3(6) . . . . ? C127 P3 C130 C135 134.4(6) . . . . ? Pd2 P3 C130 C135 -100.4(5) . . . . ? C136 P3 C130 C131 -162.5(5) . . . . ? C127 P3 C130 C131 -52.4(6) . . . . ? Pd2 P3 C130 C131 72.8(6) . . . . ? C135 C130 C131 C132 -1.7(11) . . . . ? P3 C130 C131 C132 -175.0(6) . . . . ? C130 C131 C132 C133 2.0(13) . . . . ? C131 C132 C133 C134 -1.2(16) . . . . ? C132 C133 C134 C135 0.0(14) . . . . ? C131 C130 C135 C134 0.6(10) . . . . ? P3 C130 C135 C134 173.7(6) . . . . ? C133 C134 C135 C130 0.3(12) . . . . ? C130 P3 C136 C141 -114.8(6) . . . . ? C127 P3 C136 C141 136.8(6) . . . . ? Pd2 P3 C136 C141 8.8(7) . . . . ? C130 P3 C136 C137 62.8(6) . . . . ? C127 P3 C136 C137 -45.6(6) . . . . ? Pd2 P3 C136 C137 -173.7(5) . . . . ? C141 C136 C137 C138 -1.1(11) . . . . ? P3 C136 C137 C138 -178.7(6) . . . . ? C136 C137 C138 C139 -1.6(13) . . . . ? C137 C138 C139 C140 1.7(14) . . . . ? C138 C139 C140 C141 0.9(15) . . . . ? C137 C136 C141 C140 3.7(12) . . . . ? P3 C136 C141 C140 -178.7(7) . . . . ? C139 C140 C141 C136 -3.7(14) . . . . ? C148 P4 C142 C143 105.8(6) . . . . ? C129 P4 C142 C143 -144.6(6) . . . . ? Pd2 P4 C142 C143 -16.8(6) . . . . ? C148 P4 C142 C147 -73.7(6) . . . . ? C129 P4 C142 C147 35.8(6) . . . . ? Pd2 P4 C142 C147 163.7(5) . . . . ? C147 C142 C143 C144 0.8(11) . . . . ? P4 C142 C143 C144 -178.7(6) . . . . ? C142 C143 C144 C145 -2.8(13) . . . . ? C143 C144 C145 C146 3.9(14) . . . . ? C144 C145 C146 C147 -3.1(14) . . . . ? C145 C146 C147 C142 1.1(13) . . . . ? C143 C142 C147 C146 0.1(11) . . . . ? P4 C142 C147 C146 179.6(6) . . . . ? C142 P4 C148 C149 -22.7(6) . . . . ? C129 P4 C148 C149 -134.0(5) . . . . ? Pd2 P4 C148 C149 100.3(5) . . . . ? C142 P4 C148 C153 161.2(6) . . . . ? C129 P4 C148 C153 49.9(6) . . . . ? Pd2 P4 C148 C153 -75.7(6) . . . . ? C153 C148 C149 C150 0.5(10) . . . . ? P4 C148 C149 C150 -175.6(5) . . . . ? C148 C149 C150 C151 -0.4(11) . . . . ? C149 C150 C151 C152 -0.8(12) . . . . ? C150 C151 C152 C153 2.0(13) . . . . ? C149 C148 C153 C152 0.7(11) . . . . ? P4 C148 C153 C152 176.8(6) . . . . ? C151 C152 C153 C148 -1.9(12) . . . . ? O31 S11 C11 F31 -174.6(10) . . . . ? O21 S11 C11 F31 60.3(10) . . . . ? O11 S11 C11 F31 -55.5(11) . . . . ? O31 S11 C11 F21 -49.1(10) . . . . ? O21 S11 C11 F21 -174.2(8) . . . . ? O11 S11 C11 F21 70.1(9) . . . . ? O31 S11 C11 F11 73.3(10) . . . . ? O21 S11 C11 F11 -51.8(10) . . . . ? O11 S11 C11 F11 -167.5(10) . . . . ? O12 S12 C12 F32 177.0(8) . . . . ? O22 S12 C12 F32 -64.6(9) . . . . ? O32 S12 C12 F32 55.0(9) . . . . ? O12 S12 C12 F12 -64.2(9) . . . . ? O22 S12 C12 F12 54.2(10) . . . . ? O32 S12 C12 F12 173.9(9) . . . . ? O12 S12 C12 F22 55.1(9) . . . . ? O22 S12 C12 F22 173.4(9) . . . . ? O32 S12 C12 F22 -66.9(9) . . . . ? O13 S13 C13 F23 -66.2(9) . . . . ? O33 S13 C13 F23 54.6(9) . . . . ? O23 S13 C13 F23 175.4(8) . . . . ? O13 S13 C13 F13 -179.8(7) . . . . ? O33 S13 C13 F13 -59.0(8) . . . . ? O23 S13 C13 F13 61.7(8) . . . . ? O13 S13 C13 F33 58.7(9) . . . . ? O33 S13 C13 F33 179.5(8) . . . . ? O23 S13 C13 F33 -59.7(9) . . . . ? O34 S14' O14 S14 -64.2(7) . . . . ? C14' S14' O14 S14 56.5(8) . . . . ? F24 S14' O14 S14 126.5(8) . . . . ? O24 S14' O14 S14 7.6(5) . . . . ? O34 S14 O14 S14' 56.2(6) . . . . ? O24 S14 O14 S14' -168.0(8) . . . . ? C14 S14 O14 S14' -58.5(6) . . . . ? O14 S14 O24 C14' 116.9(7) . . . . ? O34 S14 O24 C14' -105.7(7) . . . . ? C14 S14 O24 C14' 3.6(8) . . . . ? O14 S14 O24 S14' 98(3) . . . . ? O34 S14 O24 S14' -125(3) . . . . ? C14 S14 O24 S14' -16(3) . . . . ? O14 S14' O24 S14 -77(3) . . . . ? O34 S14' O24 S14 50(3) . . . . ? C14' S14' O24 S14 160(3) . . . . ? F24 S14' O24 S14 167(3) . . . . ? O14 S14' O24 C14' 123.4(7) . . . . ? O34 S14' O24 C14' -109.6(7) . . . . ? F24 S14' O24 C14' 6.9(7) . . . . ? O14 S14' O34 S14 63.8(7) . . . . ? C14' S14' O34 S14 -60.7(9) . . . . ? F24 S14' O34 S14 -126.7(8) . . . . ? O24 S14' O34 S14 -5.9(5) . . . . ? O14 S14 O34 S14' -56.7(6) . . . . ? O24 S14 O34 S14' 170.0(8) . . . . ? C14 S14 O34 S14' 60.9(6) . . . . ? O14 S14' F24 C14 -98.3(8) . . . . ? O34 S14' F24 C14 91.6(8) . . . . ? C14' S14' F24 C14 1.2(10) . . . . ? O24 S14' F24 C14 -5.4(7) . . . . ? C14' F34 C14 F14 65(2) . . . . ? C14' F34 C14 F24 177(3) . . . . ? C14' F34 C14 S14 -63(2) . . . . ? C14' F14 C14 F34 -67(2) . . . . ? C14' F14 C14 F24 180(3) . . . . ? C14' F14 C14 S14 60(2) . . . . ? S14' F24 C14 F34 124.1(10) . . . . ? S14' F24 C14 F14 -121.5(10) . . . . ? S14' F24 C14 S14 1.1(3) . . . . ? O14 S14 C14 F34 -59.6(7) . . . . ? O34 S14 C14 F34 174.9(7) . . . . ? O24 S14 C14 F34 55.4(7) . . . . ? O14 S14 C14 F14 176.2(7) . . . . ? O34 S14 C14 F14 50.6(8) . . . . ? O24 S14 C14 F14 -68.9(8) . . . . ? O14 S14 C14 F24 59.1(8) . . . . ? O34 S14 C14 F24 -66.5(8) . . . . ? O24 S14 C14 F24 174.0(7) . . . . ? C14 F14 C14' F34 67(2) . . . . ? C14 F14 C14' O24 -129(3) . . . . ? C14 F14 C14' S14' -51.3(17) . . . . ? C14 F34 C14' F14 -68(2) . . . . ? C14 F34 C14' O24 125(3) . . . . ? C14 F34 C14' S14' 49.6(17) . . . . ? S14 O24 C14' F14 94.4(17) . . . . ? S14' O24 C14' F14 96.1(17) . . . . ? S14 O24 C14' F34 -102.1(13) . . . . ? S14' O24 C14' F34 -100.5(13) . . . . ? S14 O24 C14' S14' -1.6(3) . . . . ? O14 S14' C14' F14 171.7(10) . . . . ? O34 S14' C14' F14 -55.4(13) . . . . ? F24 S14' C14' F14 58.7(11) . . . . ? O24 S14' C14' F14 -127.9(13) . . . . ? O14 S14' C14' F34 53.5(15) . . . . ? O34 S14' C14' F34 -173.5(12) . . . . ? F24 S14' C14' F34 -59.4(12) . . . . ? O24 S14' C14' F34 114.0(15) . . . . ? O14 S14' C14' O24 -60.5(6) . . . . ? O34 S14' C14' O24 72.5(6) . . . . ? F24 S14' C14' O24 -173.4(7) . . . . ? C2 N1 C1 O1 179.2(12) . . . . ? C3 N1 C1 O1 -11(2) . . . . ? C5 N2 C4 O2 1.2(15) . . . . ? C6 N2 C4 O2 -176.5(10) . . . . ? C8 N3 C7 O3 -4.7(15) . . . . ? C9 N3 C7 O3 -174.0(9) . . . . ? C18 O4 C16 C17 -178(2) . . . . ? C16 O4 C18 C19 -166(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.761 _refine_diff_density_min -2.813 _refine_diff_density_rms 0.130 #============================================================================= # END of CIF #============================================================================= # Attachment '- Schalley_DT-ART-01-2012-030190_Compound28a.cif' data_28a _database_code_depnum_ccdc_archive 'CCDC 864209' #TrackingRef '- Schalley_DT-ART-01-2012-030190_Compound28a.cif' _audit_creation_date 2012-04-26T10:43:04-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C85.50 H81 Cl3 F12 N8 O16 P4 Pd2 S4' _chemical_formula_sum 'C85.50 H81 Cl3 F12 N8 O16 P4 Pd2 S4' _chemical_formula_weight 2275.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 23.0442(5) _cell_length_b 19.7734(4) _cell_length_c 25.6540(5) _cell_angle_alpha 90 _cell_angle_beta 106.8410(10) _cell_angle_gamma 90 _cell_volume 11188.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173.0(1) _cell_measurement_reflns_used 319977 _cell_measurement_theta_min 0.407 _cell_measurement_theta_max 28.283 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4612 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.602 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5814 _exptl_absorpt_correction_T_max 0.7457 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Bruker AXS Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.450476E-1 _diffrn_orient_matrix_ub_12 0.21986E-2 _diffrn_orient_matrix_ub_13 -0.157993E-1 _diffrn_orient_matrix_ub_21 0.47048E-2 _diffrn_orient_matrix_ub_22 0.363766E-1 _diffrn_orient_matrix_ub_23 -0.255519E-1 _diffrn_orient_matrix_ub_31 0.20563E-2 _diffrn_orient_matrix_ub_32 -0.350647E-1 _diffrn_orient_matrix_ub_33 -0.274984E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.058 _diffrn_reflns_av_unetI/netI 0.0712 _diffrn_reflns_number 77842 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 19696 _reflns_number_gt 13377 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. Although data were collected at 173 K, some atoms of solvent molecules and triflates had high anisotropic thermal parameters. Some of the triflates are very badly disorder and many restrains (listed below) had to be used in order to make the S1C, S1CB, S1D, S1d' triflates and some solvent molecules chemically reasonable. DFIX 1.750 0.002 CL6 C1G DFIX 1.750 0.002 C1G CL5 DFIX 1.750 0.002 CL1 C1E DFIX 1.750 0.002 C1E CL2 DFIX 2.200 0.002 F2D' F1D' DFIX 1.775 0.002 s1C c1C DFIX 1.335 0.002 C1C F1C DFIX 1.335 0.002 C1C F2C DFIX 1.335 0.002 C1C F3C DFIX 1.430 0.002 S1c O1c DFIX 1.430 0.002 S1c O2c DFIX 1.430 0.002 S1c O3c DFIX 2.200 0.002 F1C F2C DFIX 2.200 0.002 F2C F3C DFIX 2.200 0.002 F1C F3C DFIX 2.350 0.002 o1C o2C DFIX 2.350 0.002 o2C o3C DFIX 2.350 0.002 o1C o3C DFIX 3.150 0.002 F2C O2C DFIX 3.150 0.002 F3C O1C DFIX 3.150 0.002 F1C O3C DFIX 1.775 0.002 S1Cb C1CB DFIX 1.335 0.002 C1CB F1CB DFIX 1.335 0.002 C1CB F2CB DFIX 1.335 0.002 C1CB F3CB dfix 1.430 0.002 S1cB O1cB dfix 1.430 0.002 S1cB O2cB dfix 1.430 0.002 S1cB O3cB DFIX 2.200 0.002 F1CB F2CB DFIX 2.200 0.002 F2CB F3CB DFIX 2.200 0.002 F1CB F3CB DFIX 2.350 0.002 o1CB o2CB DFIX 2.350 0.002 o2CB o3CB DFIX 2.350 0.002 o1CB o3CB DFIX 3.150 0.002 F2CB O3CB DFIX 3.150 0.002 F3CB O1CB DFIX 3.150 0.002 F1CB O2CB DFIX 1.775 0.002 S1D C1D DFIX 1.335 0.002 C1D F1D DFIX 1.335 0.002 C1D F2D DFIX 1.335 0.002 C1D F3D dfix 1.430 0.002 S1D O1D dfix 1.430 0.002 S1D O2D dfix 1.430 0.002 S1D O3D DFIX 2.200 0.002 F1D F2D DFIX 2.200 0.002 F2D F3D DFIX 2.200 0.002 F1D F3D DFIX 2.350 0.002 o1D o2D DFIX 2.350 0.002 o2D o3D DFIX 2.350 0.002 o1D o3D DFIX 3.150 0.002 F3D O1D DFIX 3.150 0.002 F2D O2D DFIX 3.150 0.002 F1D O3D DFIX 1.775 0.002 S1D' C1D' DFIX 1.335 0.002 C1D' F1D' DFIX 1.335 0.002 C1D' F2D' DFIX 1.335 0.002 C1D' F3D' dfix 1.430 0.002 S1D' O1D' dfix 1.430 0.002 S1D' O2D' dfix 1.430 0.002 S1D' O3D' DFIX 2.200 0.002 F1D' F2D' DFIX 2.200 0.002 F2D' F3D' DFIX 2.200 0.002 F1D' F3D' DFIX 2.350 0.002 o1D' o2D' DFIX 2.350 0.002 o2D' o3D' DFIX 2.350 0.002 o1D' o3D' DFIX 3.150 0.002 F2D' O3D' DFIX 3.150 0.002 F3D' O1D' DFIX 3.150 0.002 F1D' O2D' ISOR 0.10 0.20 O1W DFIX 1.000 0.030 H1w O3W DFIX 1.000 0.030 H2w O3W DFIX 1.900 0.020 O82 H1w DFIX 1.700 0.020 H2w H1w DFIX 2.200 0.002 F1D F3D DFIX 2.200 0.002 F1D F2D DFIX 2.200 0.002 F2D F3D EADP O1D O2D O3D F1D F2D F3D EADP O1D' O2D' O3D' F1D' F2D' F3D' EADP O1C O2C O3C F1C F2C F3C EADP O1CB O2CB O3CB F1CB F2CB F3CB EADP S1CB C1CB EADP S1C C1C EADP S1D C1D EADP S1D' C1D' eadp C124 C125 isor 0.2 S1CB C1CB S1C C1C S1D C1D S1D' C1D' ; _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^)+(0.1814P)^2^+73.8362P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 19696 _refine_ls_number_parameters 1256 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.147 _refine_ls_R_factor_gt 0.1129 _refine_ls_wR_factor_ref 0.3338 _refine_ls_wR_factor_gt 0.3102 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.12 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 3.039 _refine_diff_density_min -2.629 _refine_diff_density_rms 0.181 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pd1 Pd 0.49615(3) 0.88313(4) 0.18429(3) 0.0323(2) Uani 1 1 d . . . Pd2 Pd 0.46365(3) 1.39704(4) 0.19768(3) 0.0351(2) Uani 1 1 d . . . P1 P 0.45088(13) 0.82582(13) 0.23881(10) 0.0402(6) Uani 1 1 d . . . P2 P 0.58764(13) 0.83884(14) 0.23080(10) 0.0410(6) Uani 1 1 d . . . P3 P 0.40386(12) 1.43566(15) 0.24840(10) 0.0432(6) Uani 1 1 d . . . P4 P 0.54397(12) 1.45583(13) 0.25072(10) 0.0366(6) Uani 1 1 d . . . S1A S 0.42566(15) 1.58415(16) 0.10307(12) 0.0563(8) Uani 1 1 d . . . S1B S 0.80837(16) 1.13833(17) 0.10604(16) 0.0732(10) Uani 1 1 d . . . S1C S 0.5218(3) 1.1375(4) 0.2714(2) 0.080(2) Uani 0.6 1 d PDU A 1 O1C O 0.4811(6) 1.1864(6) 0.2388(5) 0.118(3) Uani 0.6 1 d PD A 1 O2C O 0.5011(7) 1.0705(4) 0.2543(5) 0.118(3) Uani 0.6 1 d PD A 1 O3C O 0.5248(7) 1.1466(7) 0.3277(3) 0.118(3) Uani 0.6 1 d PD A 1 C1C C 0.5926(3) 1.1482(5) 0.2571(4) 0.080(2) Uani 0.6 1 d PDU A 1 F1C F 0.6236(7) 1.0914(5) 0.2759(5) 0.118(3) Uani 0.6 1 d PD A 1 F2C F 0.5871(6) 1.1550(7) 0.2037(3) 0.118(3) Uani 0.6 1 d PD A 1 F3C F 0.6228(6) 1.2018(6) 0.2842(4) 0.118(3) Uani 0.6 1 d PD A 1 S1CB S 0.4925(3) 1.1368(3) 0.2670(4) 0.139(8) Uani 0.4 1 d PDU B 2 O1CB O 0.5231(6) 1.1255(6) 0.3239(4) 0.058(2) Uani 0.4 1 d PD B 2 O2CB O 0.5148(6) 1.0890(5) 0.2351(5) 0.058(2) Uani 0.4 1 d PD B 2 O3CB O 0.5050(6) 1.2044(4) 0.2526(5) 0.058(2) Uani 0.4 1 d PD B 2 C1CB C 0.4124(3) 1.1275(4) 0.2527(4) 0.139(8) Uani 0.4 1 d PDU B 2 F1CB F 0.4002(6) 1.0711(4) 0.2769(4) 0.058(2) Uani 0.4 1 d PD B 2 F2CB F 0.3850(6) 1.1236(5) 0.1988(3) 0.058(2) Uani 0.4 1 d PD B 2 F3CB F 0.3910(6) 1.1816(4) 0.2731(4) 0.058(2) Uani 0.4 1 d PD B 2 S1D S 0.1608(3) 1.1529(3) 0.1641(2) 0.0604(16) Uani 0.5 1 d PDU C 3 O1D O 0.1633(7) 1.1973(6) 0.1203(4) 0.105(3) Uani 0.5 1 d PD C 3 O2D O 0.1436(6) 1.0863(4) 0.1425(6) 0.105(3) Uani 0.5 1 d PD C 3 O3D O 0.1163(6) 1.1777(6) 0.1888(6) 0.105(3) Uani 0.5 1 d PD C 3 C1D C 0.2336(3) 1.1506(5) 0.2134(4) 0.0604(16) Uani 0.5 1 d PDU C 3 F1D F 0.2357(6) 1.0982(6) 0.2473(6) 0.105(3) Uani 0.5 1 d PD C 3 F2D F 0.2764(6) 1.1426(7) 0.1877(5) 0.105(3) Uani 0.5 1 d PD C 3 F3D F 0.2439(7) 1.2085(6) 0.2422(5) 0.105(3) Uani 0.5 1 d PD C 3 S1D' S 0.1113(2) 1.1533(3) 0.1173(2) 0.0542(14) Uani 0.5 1 d PDU D 4 O1D' O 0.1424(5) 1.2150(4) 0.1121(5) 0.078(2) Uani 0.5 1 d PD D 4 O2D' O 0.1533(4) 1.0976(4) 0.1237(5) 0.078(2) Uani 0.5 1 d PD D 4 O3D' O 0.0908(5) 1.1574(6) 0.1653(3) 0.078(2) Uani 0.5 1 d PD D 4 C1D' C 0.0472(3) 1.1390(5) 0.0593(3) 0.0542(14) Uani 0.5 1 d PDU D 4 F1D' F 0.0126(4) 1.0880(5) 0.0686(5) 0.078(2) Uani 0.5 1 d PD D 4 F2D' F 0.0130(5) 1.1953(5) 0.0465(4) 0.078(2) Uani 0.5 1 d PD D 4 F3D' F 0.0675(5) 1.1222(6) 0.0167(4) 0.078(2) Uani 0.5 1 d PD D 4 Cl1 Cl 0.7115(8) 1.0905(9) 0.1989(5) 0.200(9) Uani 0.5 1 d PD . . Cl2 Cl 0.7345(4) 1.2324(5) 0.2268(4) 0.099(3) Uani 0.5 1 d PD . . Cl3 Cl 0.5701(5) 0.8880(5) 0.5505(4) 0.107(3) Uani 0.5 1 d P . . Cl4 Cl 0.6800(4) 0.8449(9) 0.5318(4) 0.151(6) Uani 0.5 1 d P . . Cl5 Cl 0.3816(5) 0.9468(6) 0.5047(3) 0.118(4) Uani 0.5 1 d PD . . Cl6 Cl 0.4133(6) 0.8091(5) 0.5203(4) 0.131(4) Uani 0.5 1 d PD . . F1A F 0.3164(6) 1.5608(9) 0.0446(7) 0.211(9) Uani 1 1 d . . . F1BB F 0.8230(8) 1.1704(9) 0.0117(5) 0.183(7) Uani 1 1 d . . . F2A F 0.3220(5) 1.6086(6) 0.1205(5) 0.118(4) Uani 1 1 d . . . F2B F 0.8892(7) 1.0992(8) 0.0636(7) 0.173(6) Uani 1 1 d . . . F3A F 0.3375(5) 1.6669(6) 0.0569(4) 0.123(4) Uani 1 1 d . . . F3B F 0.8885(6) 1.2066(7) 0.0793(5) 0.141(5) Uani 1 1 d . . . O1A O 0.4271(5) 1.5194(4) 0.1282(4) 0.073(3) Uani 1 1 d . . . O1B O 0.7742(4) 1.1975(4) 0.1112(6) 0.103(4) Uani 1 1 d . . . O1W O 0.5747(10) 1.6424(10) 0.0446(9) 0.085(6) Uiso 0.5 1 d P . . O2A O 0.4467(6) 1.5880(8) 0.0581(4) 0.120(5) Uani 1 1 d . . . O2B O 0.7699(4) 1.0815(5) 0.0811(5) 0.090(3) Uani 1 1 d . . . O2W O 0.4343(13) 1.1427(11) 0.0788(10) 0.132(13) Uani 0.5 1 d P . . O3A O 0.4506(6) 1.6379(5) 0.1404(5) 0.099(4) Uani 1 1 d . . . O3B O 0.8515(5) 1.1216(5) 0.1584(5) 0.102(4) Uani 1 1 d . . . O3W O 0.5188(4) 1.2341(4) -0.1053(4) 0.066(2) Uani 1 1 d D E 1 O81 O 0.2847(4) 1.1077(5) 0.0085(3) 0.067(3) Uani 1 1 d . . . O82 O 0.5595(3) 1.1799(5) 0.0044(3) 0.060(2) Uani 1 1 d D . . N11 N 0.4133(4) 0.9222(4) 0.1386(3) 0.0339(17) Uani 1 1 d . . . N11' N 0.3917(4) 1.3440(4) 0.1448(3) 0.0393(19) Uani 1 1 d . . . N12 N 0.5336(4) 0.9392(4) 0.1325(3) 0.0348(17) Uani 1 1 d . . . N12' N 0.5163(4) 1.3611(4) 0.1492(3) 0.0388(19) Uani 1 1 d . . . N71' N 0.2286(5) 1.1782(5) 0.0465(4) 0.054(2) Uani 1 1 d . . . N71 N 0.2230(4) 1.0645(5) 0.0551(3) 0.046(2) Uani 1 1 d . . . N72 N 0.6395(4) 1.1117(5) 0.0444(3) 0.047(2) Uani 1 1 d . . . N72' N 0.6481(4) 1.2266(5) 0.0568(4) 0.048(2) Uani 1 1 d . . . C1A C 0.3470(8) 1.6074(10) 0.0795(7) 0.088(5) Uani 1 1 d . . . C1B C 0.8542(9) 1.1547(12) 0.0642(9) 0.119(8) Uani 1 1 d . . . C1E C 0.7629(7) 1.1499(5) 0.2368(8) 0.079(9) Uani 0.5 1 d PD . . H1E1 H 0.7724 1.1386 0.2752 0.095 Uiso 0.5 1 calc PR . . H1E2 H 0.8002 1.1475 0.2266 0.095 Uiso 0.5 1 calc PR . . C1F C 0.6098(14) 0.8685(19) 0.5055(13) 0.088(10) Uani 0.5 1 d P . . H1F1 H 0.5884 0.8326 0.4818 0.105 Uiso 0.5 1 calc PR . . H1F2 H 0.6095 0.9079 0.4828 0.105 Uiso 0.5 1 calc PR . . C1G C 0.3951(19) 0.8809(7) 0.5523(7) 0.119(15) Uani 0.5 1 d PD . . H1G1 H 0.3594 0.8725 0.564 0.143 Uiso 0.5 1 calc PR . . H1G2 H 0.4284 0.8925 0.584 0.143 Uiso 0.5 1 calc PR . . C4A C 0.2378(5) 0.9941(6) 0.0441(5) 0.055(3) Uani 1 1 d . . . H4A1 H 0.2358 0.9902 0.0059 0.066 Uiso 1 1 calc R . . H4A2 H 0.2073 0.9642 0.0506 0.066 Uiso 1 1 calc R . . C4A' C 0.2482(7) 1.2394(7) 0.0267(5) 0.070(4) Uani 1 1 d . . . H4A3 H 0.2137 1.2695 0.014 0.084 Uiso 1 1 calc R . . H4A4 H 0.2629 1.2287 -0.0042 0.084 Uiso 1 1 calc R . . C4B C 0.6080(5) 1.0498(6) 0.0213(4) 0.051(3) Uani 1 1 d . . . H4B1 H 0.6361 1.0202 0.0106 0.061 Uiso 1 1 calc R . . H4B2 H 0.5756 1.0611 -0.0112 0.061 Uiso 1 1 calc R . . C4B' C 0.6247(5) 1.2931(5) 0.0481(4) 0.049(3) Uani 1 1 d . . . H4B3 H 0.6005 1.2969 0.0103 0.058 Uiso 1 1 calc R . . H4B4 H 0.6585 1.3241 0.0535 0.058 Uiso 1 1 calc R . . C21' C 0.3829(5) 1.2785(5) 0.1513(4) 0.046(3) Uani 1 1 d . . . H21' H 0.4087 1.2556 0.1806 0.055 Uiso 1 1 calc R . . C21 C 0.3944(5) 0.9845(5) 0.1465(4) 0.040(2) Uani 1 1 d . . . H21 H 0.42 1.0119 0.1727 0.048 Uiso 1 1 calc R . . C22' C 0.5433(5) 1.2999(5) 0.1577(4) 0.039(2) Uani 1 1 d . . . H22' H 0.5375 1.2725 0.1853 0.046 Uiso 1 1 calc R . . C22 C 0.5472(5) 1.0034(5) 0.1408(4) 0.047(3) Uani 1 1 d . . . H22 H 0.5402 1.0246 0.1708 0.057 Uiso 1 1 calc R . . C31 C 0.3393(5) 1.0092(5) 0.1179(4) 0.045(2) Uani 1 1 d . . . H31 H 0.3281 1.0527 0.125 0.054 Uiso 1 1 calc R . . C31' C 0.3355(5) 1.2433(5) 0.1147(4) 0.047(3) Uani 1 1 d . . . H31' H 0.3289 1.1979 0.1205 0.057 Uiso 1 1 calc R . . C32' C 0.5795(5) 1.2768(5) 0.1266(4) 0.043(2) Uani 1 1 d . . . H32' H 0.599 1.2353 0.1346 0.051 Uiso 1 1 calc R . . C32 C 0.5718(6) 1.0413(6) 0.1065(5) 0.060(3) Uani 1 1 d . . . H32 H 0.5818 1.0865 0.1144 0.072 Uiso 1 1 calc R . . C41 C 0.2996(4) 0.9703(5) 0.0781(4) 0.039(2) Uani 1 1 d . . . C41' C 0.2990(5) 1.2762(6) 0.0707(4) 0.051(3) Uani 1 1 d . . . C42 C 0.5812(5) 1.0122(5) 0.0609(4) 0.041(2) Uani 1 1 d . . . C42' C 0.5865(5) 1.3155(6) 0.0835(4) 0.048(3) Uani 1 1 d . . . C51 C 0.3182(4) 0.9067(5) 0.0691(4) 0.038(2) Uani 1 1 d . . . H51 H 0.293 0.8793 0.0425 0.045 Uiso 1 1 calc R . . C51' C 0.3075(5) 1.3440(6) 0.0641(4) 0.053(3) Uani 1 1 d . . . H51' H 0.2825 1.3676 0.0348 0.063 Uiso 1 1 calc R . . C52' C 0.5574(5) 1.3777(6) 0.0752(4) 0.052(3) Uani 1 1 d . . . H52' H 0.5607 1.405 0.0467 0.062 Uiso 1 1 calc R . . C52 C 0.5684(6) 0.9443(6) 0.0535(4) 0.054(3) Uani 1 1 d . . . H52 H 0.5762 0.9218 0.0244 0.065 Uiso 1 1 calc R . . C61 C 0.3747(5) 0.8833(5) 0.0996(4) 0.037(2) Uani 1 1 d . . . H61 H 0.3866 0.8399 0.0934 0.045 Uiso 1 1 calc R . . C61' C 0.3545(5) 1.3765(6) 0.1024(4) 0.047(3) Uani 1 1 d . . . H61' H 0.3602 1.4225 0.0984 0.056 Uiso 1 1 calc R . . C62 C 0.5439(6) 0.9091(6) 0.0891(4) 0.050(3) Uani 1 1 d . . . H62 H 0.5344 0.8636 0.0826 0.06 Uiso 1 1 calc R . . C62' C 0.5244(5) 1.3995(5) 0.1078(4) 0.046(3) Uani 1 1 d . . . H62' H 0.5066 1.4421 0.1017 0.055 Uiso 1 1 calc R . . C81 C 0.2483(5) 1.1173(7) 0.0350(4) 0.054(3) Uani 1 1 d . . . C82 C 0.6127(5) 1.1734(6) 0.0336(4) 0.044(3) Uani 1 1 d . . . C100 C 0.4756(5) 0.7396(5) 0.2518(5) 0.052(3) Uani 1 1 d . . . H10A H 0.4528 0.7184 0.2737 0.063 Uiso 1 1 calc R . . H10B H 0.4663 0.7156 0.2174 0.063 Uiso 1 1 calc R . . C101 C 0.5449(6) 0.7316(5) 0.2816(5) 0.055(3) Uani 1 1 d . . . H10C H 0.5557 0.7611 0.3131 0.066 Uiso 1 1 calc R . . H10D H 0.5528 0.6854 0.2944 0.066 Uiso 1 1 calc R . . C102 C 0.5843(6) 0.7485(6) 0.2452(5) 0.061(3) Uani 1 1 d . . . H10E H 0.569 0.7244 0.211 0.073 Uiso 1 1 calc R . . H10F H 0.6251 0.7324 0.2625 0.073 Uiso 1 1 calc R . . C103 C 0.3689(5) 0.8195(6) 0.2091(5) 0.051(3) Uani 1 1 d . . . C104 C 0.3446(7) 0.7651(7) 0.1775(6) 0.076(4) Uani 1 1 d . . . H104 H 0.369 0.7298 0.1724 0.091 Uiso 1 1 calc R . . C105 C 0.2804(7) 0.7640(9) 0.1525(7) 0.092(5) Uani 1 1 d . . . H105 H 0.2621 0.7265 0.1325 0.111 Uiso 1 1 calc R . . C106 C 0.2455(7) 0.8192(10) 0.1581(7) 0.088(5) Uani 1 1 d . . . H106 H 0.2041 0.8197 0.1404 0.105 Uiso 1 1 calc R . . C107 C 0.2715(7) 0.8721(9) 0.1892(6) 0.074(4) Uani 1 1 d . . . H107 H 0.2475 0.9083 0.1933 0.089 Uiso 1 1 calc R . . C108 C 0.3326(5) 0.8738(7) 0.2150(5) 0.060(3) Uani 1 1 d . . . H108 H 0.3497 0.9109 0.2363 0.072 Uiso 1 1 calc R . . C109 C 0.4610(5) 0.8654(6) 0.3041(4) 0.048(3) Uani 1 1 d . . . C110 C 0.4740(6) 0.9343(6) 0.3106(5) 0.059(3) Uani 1 1 d . . . H110 H 0.4792 0.9589 0.2814 0.071 Uiso 1 1 calc R . . C111 C 0.4791(7) 0.9662(7) 0.3583(5) 0.071(4) Uani 1 1 d . . . H111 H 0.4861 1.0126 0.3607 0.085 Uiso 1 1 calc R . . C112 C 0.4741(7) 0.9310(9) 0.4038(6) 0.077(4) Uani 1 1 d . . . H112 H 0.4781 0.9529 0.4367 0.092 Uiso 1 1 calc R . . C113 C 0.4633(6) 0.8640(9) 0.3984(5) 0.073(4) Uani 1 1 d . . . H113 H 0.4606 0.8397 0.4286 0.087 Uiso 1 1 calc R . . C114 C 0.4560(6) 0.8291(7) 0.3489(5) 0.058(3) Uani 1 1 d . . . H114 H 0.4479 0.783 0.3464 0.07 Uiso 1 1 calc R . . C115 C 0.6239(5) 0.8787(5) 0.2961(4) 0.041(2) Uani 1 1 d . . . C116 C 0.6123(5) 0.9455(6) 0.3037(5) 0.055(3) Uani 1 1 d . . . H116 H 0.586 0.97 0.2758 0.066 Uiso 1 1 calc R . . C117 C 0.6402(7) 0.9765(8) 0.3536(5) 0.074(4) Uani 1 1 d . . . H117 H 0.6331 1.022 0.3586 0.089 Uiso 1 1 calc R . . C118 C 0.6788(6) 0.9394(8) 0.3962(5) 0.068(4) Uani 1 1 d . . . H118 H 0.6964 0.9596 0.4297 0.082 Uiso 1 1 calc R . . C119 C 0.6901(6) 0.8737(7) 0.3879(5) 0.062(3) Uani 1 1 d . . . H119 H 0.7167 0.8493 0.4158 0.075 Uiso 1 1 calc R . . C120 C 0.6628(5) 0.8420(6) 0.3385(4) 0.046(2) Uani 1 1 d . . . H120 H 0.6704 0.7966 0.3337 0.055 Uiso 1 1 calc R . . C121 C 0.6411(6) 0.8469(7) 0.1922(5) 0.062(3) Uani 1 1 d . . . C122 C 0.6764(6) 0.9038(9) 0.1963(5) 0.076(4) Uani 1 1 d . . . H122 H 0.6749 0.9376 0.2211 0.091 Uiso 1 1 calc R . . C123 C 0.7148(6) 0.9108(12) 0.1626(7) 0.109(7) Uani 1 1 d . . . H123 H 0.7385 0.9496 0.1664 0.131 Uiso 1 1 calc R . . C124 C 0.7193(13) 0.8655(15) 0.1260(11) 0.150(9) Uani 1 1 d . . . H124 H 0.7453 0.8718 0.1046 0.18 Uiso 1 1 calc R . . C125 C 0.6845(13) 0.8097(15) 0.1212(10) 0.150(9) Uani 1 1 d . . . H125 H 0.6876 0.7773 0.0959 0.18 Uiso 1 1 calc R . . C126 C 0.6431(9) 0.7966(8) 0.1522(7) 0.097(6) Uani 1 1 d . . . H126 H 0.619 0.758 0.1469 0.117 Uiso 1 1 calc R . . C127 C 0.4145(5) 1.5229(6) 0.2660(4) 0.053(3) Uani 1 1 d . . . H12A H 0.4047 1.5492 0.2327 0.063 Uiso 1 1 calc R . . H12B H 0.3861 1.5355 0.2858 0.063 Uiso 1 1 calc R . . C128 C 0.4784(5) 1.5420(5) 0.3005(5) 0.053(3) Uani 1 1 d . . . H12C H 0.4909 1.5111 0.3312 0.063 Uiso 1 1 calc R . . H12D H 0.4775 1.5872 0.3149 0.063 Uiso 1 1 calc R . . C129 C 0.5257(5) 1.5399(5) 0.2684(4) 0.043(2) Uani 1 1 d . . . H12E H 0.5626 1.5615 0.29 0.052 Uiso 1 1 calc R . . H12F H 0.5103 1.5659 0.2352 0.052 Uiso 1 1 calc R . . C130 C 0.4131(5) 1.3906(6) 0.3116(4) 0.047(3) Uani 1 1 d . . . C131 C 0.4291(6) 1.3220(7) 0.3151(5) 0.061(3) Uani 1 1 d . . . H131 H 0.4355 1.2997 0.2853 0.073 Uiso 1 1 calc R . . C132 C 0.4354(6) 1.2880(8) 0.3633(5) 0.072(4) Uani 1 1 d . . . H132 H 0.445 1.2423 0.365 0.086 Uiso 1 1 calc R . . C133 C 0.4280(7) 1.3185(9) 0.4085(5) 0.077(4) Uani 1 1 d . . . H133 H 0.4344 1.2948 0.441 0.093 Uiso 1 1 calc R . . C134 C 0.4106(7) 1.3860(9) 0.4045(5) 0.078(5) Uani 1 1 d . . . H134 H 0.4032 1.4072 0.4343 0.093 Uiso 1 1 calc R . . C135 C 0.4040(6) 1.4231(7) 0.3565(4) 0.060(3) Uani 1 1 d . . . H135 H 0.3938 1.4687 0.3548 0.072 Uiso 1 1 calc R . . C136 C 0.3244(5) 1.4274(7) 0.2121(5) 0.055(3) Uani 1 1 d . . . C137 C 0.2942(6) 1.3665(7) 0.2093(5) 0.060(3) Uani 1 1 d . . . H137 H 0.3148 1.3296 0.2286 0.072 Uiso 1 1 calc R . . C138 C 0.2339(6) 1.3583(8) 0.1785(5) 0.069(4) Uani 1 1 d . . . H138 H 0.2147 1.3168 0.1777 0.083 Uiso 1 1 calc R . . C139 C 0.2026(6) 1.4130(11) 0.1488(6) 0.088(5) Uani 1 1 d . . . H139 H 0.1623 1.4085 0.1281 0.105 Uiso 1 1 calc R . . C140 C 0.2311(8) 1.4710(12) 0.1507(7) 0.105(6) Uani 1 1 d . . . H140 H 0.2104 1.5062 0.1291 0.126 Uiso 1 1 calc R . . C141 C 0.2920(6) 1.4837(9) 0.1839(5) 0.077(4) Uani 1 1 d . . . H141 H 0.3093 1.5265 0.1867 0.092 Uiso 1 1 calc R . . C142 C 0.6031(5) 1.4689(6) 0.2177(4) 0.051(3) Uani 1 1 d . . . C143 C 0.6009(7) 1.5278(7) 0.1856(6) 0.075(4) Uani 1 1 d . . . H143 H 0.5714 1.5608 0.1832 0.09 Uiso 1 1 calc R . . C144 C 0.6445(8) 1.5343(10) 0.1580(8) 0.109(7) Uani 1 1 d . . . H144 H 0.6433 1.5715 0.1354 0.131 Uiso 1 1 calc R . . C145 C 0.6891(8) 1.4867(11) 0.1635(7) 0.104(6) Uani 1 1 d . . . H145 H 0.7195 1.4934 0.1468 0.125 Uiso 1 1 calc R . . C146 C 0.6891(6) 1.4296(9) 0.1935(6) 0.076(4) Uani 1 1 d . . . H146 H 0.718 1.3962 0.1951 0.092 Uiso 1 1 calc R . . C147 C 0.6467(5) 1.4209(7) 0.2213(4) 0.056(3) Uani 1 1 d . . . H147 H 0.6478 1.3825 0.2425 0.067 Uiso 1 1 calc R . . C148 C 0.5797(4) 1.4123(5) 0.3140(4) 0.036(2) Uani 1 1 d . . . C149 C 0.6159(6) 1.4477(6) 0.3580(4) 0.056(3) Uani 1 1 d . . . H149 H 0.6222 1.4939 0.3552 0.067 Uiso 1 1 calc R . . C150 C 0.6429(6) 1.4135(6) 0.4068(5) 0.066(4) Uani 1 1 d . . . H150 H 0.6687 1.4364 0.4361 0.079 Uiso 1 1 calc R . . C151 C 0.6311(5) 1.3462(6) 0.4111(4) 0.056(3) Uani 1 1 d . . . H151 H 0.6468 1.3242 0.4442 0.067 Uiso 1 1 calc R . . C152 C 0.5965(6) 1.3110(6) 0.3670(5) 0.058(3) Uani 1 1 d . . . H152 H 0.5903 1.2649 0.3698 0.07 Uiso 1 1 calc R . . C153 C 0.5710(5) 1.3441(5) 0.3188(4) 0.051(3) Uani 1 1 d . . . H153 H 0.5475 1.3201 0.289 0.061 Uiso 1 1 calc R . . H1W H 0.543(3) 1.214(6) -0.068(2) 0.077 Uiso 1 1 d D F 1 H2W H 0.477(3) 1.249(6) -0.106(4) 0.077 Uiso 1 1 d D G 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0298(4) 0.0387(4) 0.0277(4) 0.0037(3) 0.0073(3) -0.0006(3) Pd2 0.0305(4) 0.0479(4) 0.0232(4) 0.0003(3) 0.0021(3) -0.0040(3) P1 0.0402(15) 0.0447(14) 0.0346(13) 0.0082(11) 0.0090(12) -0.0034(11) P2 0.0369(15) 0.0500(15) 0.0335(13) 0.0037(11) 0.0059(11) 0.0071(12) P3 0.0325(15) 0.0669(18) 0.0266(12) -0.0002(12) 0.0028(11) -0.0001(13) P4 0.0324(14) 0.0462(14) 0.0272(12) 0.0015(10) 0.0023(11) -0.0045(11) S1A 0.067(2) 0.0577(17) 0.0434(15) 0.0164(13) 0.0156(15) 0.0115(15) S1B 0.057(2) 0.0595(19) 0.082(2) -0.0254(17) -0.0131(18) 0.0109(16) S1C 0.093(6) 0.085(5) 0.052(3) 0.003(3) 0.004(3) -0.017(4) O1C 0.157(8) 0.129(6) 0.071(4) 0.002(4) 0.038(5) 0.006(6) O2C 0.157(8) 0.129(6) 0.071(4) 0.002(4) 0.038(5) 0.006(6) O3C 0.157(8) 0.129(6) 0.071(4) 0.002(4) 0.038(5) 0.006(6) C1C 0.093(6) 0.085(5) 0.052(3) 0.003(3) 0.004(3) -0.017(4) F1C 0.157(8) 0.129(6) 0.071(4) 0.002(4) 0.038(5) 0.006(6) F2C 0.157(8) 0.129(6) 0.071(4) 0.002(4) 0.038(5) 0.006(6) F3C 0.157(8) 0.129(6) 0.071(4) 0.002(4) 0.038(5) 0.006(6) S1CB 0.060(7) 0.004(3) 0.36(2) 0.013(6) 0.063(10) 0.002(4) O1CB 0.080(6) 0.037(4) 0.043(4) -0.003(3) -0.006(4) 0.008(3) O2CB 0.080(6) 0.037(4) 0.043(4) -0.003(3) -0.006(4) 0.008(3) O3CB 0.080(6) 0.037(4) 0.043(4) -0.003(3) -0.006(4) 0.008(3) C1CB 0.060(7) 0.004(3) 0.36(2) 0.013(6) 0.063(10) 0.002(4) F1CB 0.080(6) 0.037(4) 0.043(4) -0.003(3) -0.006(4) 0.008(3) F2CB 0.080(6) 0.037(4) 0.043(4) -0.003(3) -0.006(4) 0.008(3) F3CB 0.080(6) 0.037(4) 0.043(4) -0.003(3) -0.006(4) 0.008(3) S1D 0.079(4) 0.045(3) 0.071(4) 0.004(3) 0.044(4) 0.004(3) O1D 0.099(7) 0.105(6) 0.119(7) -0.020(5) 0.045(6) -0.007(5) O2D 0.099(7) 0.105(6) 0.119(7) -0.020(5) 0.045(6) -0.007(5) O3D 0.099(7) 0.105(6) 0.119(7) -0.020(5) 0.045(6) -0.007(5) C1D 0.079(4) 0.045(3) 0.071(4) 0.004(3) 0.044(4) 0.004(3) F1D 0.099(7) 0.105(6) 0.119(7) -0.020(5) 0.045(6) -0.007(5) F2D 0.099(7) 0.105(6) 0.119(7) -0.020(5) 0.045(6) -0.007(5) F3D 0.099(7) 0.105(6) 0.119(7) -0.020(5) 0.045(6) -0.007(5) S1D' 0.068(4) 0.046(3) 0.055(3) -0.003(2) 0.030(3) 0.003(3) O1D' 0.057(4) 0.104(5) 0.081(5) -0.023(4) 0.034(4) -0.006(4) O2D' 0.057(4) 0.104(5) 0.081(5) -0.023(4) 0.034(4) -0.006(4) O3D' 0.057(4) 0.104(5) 0.081(5) -0.023(4) 0.034(4) -0.006(4) C1D' 0.068(4) 0.046(3) 0.055(3) -0.003(2) 0.030(3) 0.003(3) F1D' 0.057(4) 0.104(5) 0.081(5) -0.023(4) 0.034(4) -0.006(4) F2D' 0.057(4) 0.104(5) 0.081(5) -0.023(4) 0.034(4) -0.006(4) F3D' 0.057(4) 0.104(5) 0.081(5) -0.023(4) 0.034(4) -0.006(4) Cl1 0.263(19) 0.229(15) 0.114(9) -0.052(9) 0.066(11) -0.189(15) Cl2 0.065(5) 0.128(7) 0.108(6) 0.002(5) 0.030(5) -0.045(5) Cl3 0.113(7) 0.140(8) 0.078(5) 0.037(5) 0.046(5) 0.051(6) Cl4 0.056(5) 0.309(17) 0.074(6) 0.065(8) -0.001(4) 0.043(8) Cl5 0.158(10) 0.147(8) 0.050(4) 0.011(5) 0.032(5) 0.073(7) Cl6 0.202(12) 0.110(7) 0.121(8) 0.004(6) 0.108(9) -0.043(7) F1A 0.090(9) 0.229(17) 0.227(17) -0.077(14) -0.090(10) 0.039(10) F1BB 0.205(15) 0.241(17) 0.082(8) -0.039(9) 0.008(9) -0.124(14) F2A 0.107(8) 0.144(9) 0.124(8) 0.053(7) 0.066(7) 0.032(7) F2B 0.142(12) 0.170(13) 0.230(17) -0.076(12) 0.088(12) -0.003(10) F3A 0.122(8) 0.168(10) 0.099(7) 0.081(7) 0.063(7) 0.083(8) F3B 0.144(11) 0.160(11) 0.123(9) -0.064(8) 0.044(8) -0.057(9) O1A 0.081(7) 0.050(5) 0.083(6) 0.014(4) 0.015(5) 0.001(4) O1B 0.055(6) 0.048(5) 0.184(12) -0.036(6) -0.001(7) 0.013(4) O2A 0.111(10) 0.197(13) 0.069(7) 0.064(8) 0.054(7) 0.072(9) O2B 0.061(6) 0.064(6) 0.116(8) -0.038(6) -0.018(6) 0.004(5) O2W 0.20(3) 0.114(16) 0.142(19) 0.093(15) 0.15(2) 0.139(18) O3A 0.126(10) 0.049(5) 0.101(8) -0.003(5) 0.000(7) 0.012(6) O3B 0.061(6) 0.083(7) 0.114(9) -0.025(6) -0.051(6) 0.018(5) O3W 0.074(6) 0.057(5) 0.067(5) -0.008(4) 0.019(5) -0.007(4) O81 0.037(5) 0.125(8) 0.038(4) -0.017(5) 0.010(4) -0.011(5) O82 0.028(4) 0.100(6) 0.050(5) -0.004(4) 0.007(4) 0.005(4) N11 0.033(4) 0.045(5) 0.024(4) 0.002(3) 0.010(3) -0.002(4) N11' 0.037(5) 0.054(5) 0.024(4) 0.003(3) 0.003(4) -0.003(4) N12 0.033(4) 0.040(4) 0.034(4) 0.002(3) 0.013(4) -0.004(3) N12' 0.037(5) 0.050(5) 0.029(4) 0.002(4) 0.008(4) 0.001(4) N71' 0.060(6) 0.053(6) 0.045(5) -0.016(4) 0.007(5) -0.027(5) N71 0.032(5) 0.057(5) 0.043(5) 0.003(4) 0.000(4) 0.001(4) N72 0.046(5) 0.058(6) 0.038(5) 0.003(4) 0.015(4) -0.012(4) N72' 0.047(6) 0.053(5) 0.047(5) -0.003(4) 0.019(5) -0.003(4) C1A 0.070(11) 0.118(14) 0.084(11) 0.035(10) 0.033(9) 0.025(10) C1B 0.084(13) 0.152(19) 0.113(16) -0.080(14) 0.014(12) -0.014(13) C1E 0.09(2) 0.11(2) 0.037(13) -0.014(14) 0.027(14) -0.041(19) C1F 0.07(2) 0.12(3) 0.08(2) 0.020(18) 0.030(17) 0.036(18) C1G 0.14(4) 0.12(3) 0.07(2) -0.06(2) -0.01(2) 0.02(2) C4A 0.034(6) 0.064(7) 0.057(7) -0.011(6) 0.000(5) 0.000(5) C4A' 0.076(9) 0.077(9) 0.038(6) 0.011(6) -0.011(6) -0.036(7) C4B 0.055(7) 0.061(7) 0.042(6) -0.012(5) 0.025(6) -0.016(6) C4B' 0.048(7) 0.054(6) 0.046(6) 0.013(5) 0.016(5) 0.002(5) C21' 0.056(7) 0.043(6) 0.031(5) 0.006(4) 0.001(5) -0.005(5) C21 0.040(6) 0.044(6) 0.033(5) -0.005(4) 0.005(5) 0.003(5) C22' 0.040(6) 0.048(6) 0.029(5) 0.005(4) 0.011(4) -0.009(5) C22 0.059(7) 0.054(6) 0.036(5) -0.001(5) 0.028(5) -0.007(5) C31 0.045(7) 0.046(6) 0.040(6) -0.010(5) 0.004(5) 0.001(5) C31' 0.055(7) 0.044(6) 0.037(5) 0.002(4) 0.002(5) -0.017(5) C32' 0.036(6) 0.049(6) 0.039(5) 0.004(4) 0.006(5) 0.001(5) C32 0.095(10) 0.044(6) 0.054(7) -0.004(5) 0.042(7) -0.020(6) C41 0.029(5) 0.053(6) 0.033(5) -0.009(4) 0.007(4) -0.001(4) C41' 0.057(7) 0.058(7) 0.029(5) -0.003(5) 0.000(5) -0.023(6) C42 0.037(6) 0.058(6) 0.027(5) 0.000(4) 0.008(4) -0.009(5) C42' 0.037(6) 0.068(7) 0.037(5) 0.005(5) 0.008(5) -0.003(5) C51 0.033(6) 0.052(6) 0.028(5) -0.005(4) 0.009(4) -0.011(4) C51' 0.055(7) 0.060(7) 0.029(5) 0.006(5) -0.011(5) -0.019(6) C52' 0.053(7) 0.061(7) 0.042(6) 0.010(5) 0.013(5) 0.007(6) C52 0.069(8) 0.066(7) 0.031(5) -0.014(5) 0.021(6) -0.016(6) C61 0.043(6) 0.036(5) 0.034(5) -0.002(4) 0.015(5) -0.004(4) C61' 0.047(7) 0.056(6) 0.028(5) 0.010(4) -0.004(5) -0.005(5) C62 0.069(8) 0.046(6) 0.036(6) -0.003(5) 0.018(6) -0.012(5) C62' 0.060(7) 0.049(6) 0.027(5) 0.008(4) 0.009(5) 0.012(5) C81 0.036(6) 0.083(9) 0.030(5) -0.009(5) -0.010(5) -0.009(6) C82 0.041(6) 0.067(7) 0.031(5) 0.008(5) 0.021(5) 0.003(5) C100 0.058(8) 0.039(6) 0.051(6) 0.005(5) 0.002(6) -0.005(5) C101 0.067(8) 0.036(6) 0.055(7) 0.013(5) 0.007(6) 0.003(5) C102 0.057(8) 0.052(7) 0.061(7) 0.001(6) -0.005(6) 0.014(6) C103 0.042(7) 0.058(7) 0.051(6) 0.013(5) 0.011(5) -0.008(5) C104 0.060(9) 0.069(9) 0.088(10) 0.024(8) 0.005(8) -0.011(7) C105 0.062(10) 0.093(12) 0.112(13) 0.013(10) 0.010(9) -0.044(9) C106 0.049(9) 0.120(14) 0.098(12) 0.046(11) 0.027(9) 0.000(9) C107 0.059(9) 0.110(12) 0.064(9) 0.009(8) 0.033(8) 0.001(8) C108 0.041(7) 0.102(10) 0.044(6) 0.008(6) 0.022(6) 0.003(7) C109 0.048(7) 0.062(7) 0.033(5) 0.008(5) 0.010(5) -0.004(5) C110 0.074(9) 0.059(7) 0.052(7) 0.000(6) 0.031(7) -0.016(6) C111 0.084(10) 0.078(9) 0.053(7) -0.009(6) 0.024(7) -0.025(8) C112 0.083(11) 0.101(12) 0.056(8) -0.017(8) 0.035(8) -0.014(9) C113 0.064(9) 0.115(12) 0.041(7) 0.020(7) 0.020(6) 0.010(8) C114 0.055(8) 0.073(8) 0.047(6) 0.017(6) 0.015(6) -0.007(6) C115 0.033(5) 0.053(6) 0.038(5) 0.004(5) 0.011(5) 0.008(5) C116 0.047(7) 0.064(7) 0.049(7) -0.004(5) 0.006(6) 0.008(6) C117 0.082(10) 0.082(9) 0.050(7) -0.015(7) 0.006(7) 0.016(8) C118 0.070(9) 0.095(10) 0.034(6) -0.018(6) 0.006(6) -0.016(8) C119 0.056(8) 0.088(10) 0.036(6) 0.012(6) 0.003(6) -0.001(7) C120 0.036(6) 0.057(6) 0.042(6) 0.010(5) 0.004(5) 0.009(5) C121 0.045(7) 0.093(10) 0.043(6) 0.014(6) 0.007(6) 0.018(7) C122 0.037(7) 0.151(14) 0.038(6) -0.001(8) 0.011(6) -0.009(8) C123 0.033(8) 0.21(2) 0.080(11) 0.035(13) 0.014(8) -0.014(10) C124 0.17(2) 0.20(2) 0.122(11) 0.022(16) 0.109(15) 0.067(17) C125 0.17(2) 0.20(2) 0.122(11) 0.022(16) 0.109(15) 0.067(17) C126 0.135(16) 0.079(10) 0.106(12) 0.008(9) 0.079(12) 0.037(10) C127 0.050(7) 0.065(7) 0.038(6) -0.007(5) 0.003(5) 0.018(6) C128 0.056(7) 0.040(6) 0.062(7) -0.010(5) 0.016(6) 0.002(5) C129 0.041(6) 0.041(5) 0.040(5) 0.004(4) -0.001(5) -0.002(5) C130 0.031(6) 0.071(7) 0.035(5) -0.002(5) 0.005(5) -0.005(5) C131 0.065(8) 0.085(9) 0.034(6) 0.011(6) 0.016(6) 0.010(7) C132 0.068(9) 0.100(10) 0.044(7) 0.023(7) 0.011(6) 0.012(8) C133 0.068(10) 0.126(14) 0.034(6) 0.023(8) 0.007(6) -0.002(9) C134 0.060(9) 0.139(15) 0.032(6) -0.004(8) 0.011(6) -0.026(9) C135 0.060(8) 0.086(9) 0.035(6) -0.002(6) 0.017(6) -0.009(7) C136 0.036(6) 0.089(9) 0.042(6) 0.004(6) 0.014(5) -0.001(6) C137 0.046(7) 0.097(10) 0.035(6) -0.001(6) 0.011(5) -0.001(7) C138 0.039(7) 0.118(12) 0.050(7) -0.005(7) 0.012(6) -0.023(7) C139 0.035(8) 0.170(18) 0.050(8) 0.006(10) -0.001(6) -0.006(10) C140 0.060(11) 0.157(18) 0.084(12) 0.038(12) -0.002(9) 0.020(12) C141 0.050(8) 0.117(12) 0.056(8) 0.023(8) 0.004(7) 0.014(8) C142 0.041(7) 0.072(7) 0.038(6) 0.001(5) 0.007(5) -0.017(6) C143 0.068(9) 0.085(10) 0.084(10) 0.017(8) 0.041(8) -0.018(7) C144 0.088(13) 0.122(14) 0.143(17) 0.048(13) 0.074(13) 0.003(11) C145 0.071(12) 0.164(18) 0.094(12) 0.020(12) 0.051(10) -0.024(12) C146 0.032(7) 0.122(13) 0.071(9) 0.000(9) 0.008(6) -0.004(7) C147 0.026(6) 0.098(9) 0.039(6) 0.000(6) 0.002(5) -0.006(6) C148 0.030(5) 0.049(6) 0.024(5) -0.003(4) 0.000(4) -0.005(4) C149 0.066(8) 0.042(6) 0.039(6) -0.002(5) -0.019(6) 0.001(5) C150 0.072(9) 0.062(8) 0.038(6) -0.011(5) -0.026(6) 0.004(7) C151 0.050(7) 0.074(8) 0.034(6) 0.011(5) -0.004(5) 0.010(6) C152 0.053(8) 0.057(7) 0.051(7) 0.009(6) -0.007(6) 0.006(6) C153 0.046(7) 0.047(6) 0.041(6) -0.006(5) -0.019(5) -0.001(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Pd1 N11 2.078(8) . ? Pd1 N12 2.100(7) . ? Pd1 P1 2.275(3) . ? Pd1 P2 2.275(3) . ? Pd2 N11' 2.094(8) . ? Pd2 N12' 2.099(8) . ? Pd2 P4 2.274(3) . ? Pd2 P3 2.283(3) . ? P1 C100 1.798(11) . ? P1 C109 1.802(11) . ? P1 C103 1.826(12) . ? P2 C121 1.796(12) . ? P2 C115 1.821(11) . ? P2 C102 1.830(12) . ? P3 C127 1.781(12) . ? P3 C136 1.805(12) . ? P3 C130 1.808(11) . ? P4 C129 1.805(10) . ? P4 C148 1.811(10) . ? P4 C142 1.820(11) . ? S1A O2A 1.377(10) . ? S1A O1A 1.429(9) . ? S1A O3A 1.435(11) . ? S1A C1A 1.796(17) . ? S1B O1B 1.438(9) . ? S1B O2B 1.459(9) . ? S1B O3B 1.459(11) . ? S1B C1B 1.74(2) . ? S1C O2C 1.434(2) . ? S1C O1C 1.435(2) . ? S1C O3C 1.437(2) . ? S1C C1C 1.785(2) . ? C1C F1C 1.345(2) . ? C1C F3C 1.345(2) . ? C1C F2C 1.346(2) . ? S1CB O3CB 1.438(2) . ? S1CB O2CB 1.438(2) . ? S1CB O1CB 1.443(2) . ? S1CB C1CB 1.785(2) . ? C1CB F3CB 1.345(2) . ? C1CB F1CB 1.345(2) . ? C1CB F2CB 1.346(2) . ? S1D O3D 1.438(2) . ? S1D O1D 1.439(2) . ? S1D O2D 1.440(2) . ? S1D C1D 1.786(2) . ? C1D F3D 1.346(2) . ? C1D F1D 1.346(2) . ? C1D F2D 1.346(2) . ? S1D' O1D' 1.441(2) . ? S1D' O3D' 1.442(2) . ? S1D' O2D' 1.443(2) . ? S1D' C1D' 1.789(2) . ? C1D' F2D' 1.348(2) . ? C1D' F3D' 1.348(2) . ? C1D' F1D' 1.349(2) . ? Cl1 C1E 1.750(2) . ? Cl2 C1E 1.750(2) . ? Cl3 C1F 1.71(3) . ? Cl4 C1F 1.63(3) . ? Cl5 C1G 1.749(2) . ? Cl6 C1G 1.750(2) . ? F1A C1A 1.34(2) . ? F1BB C1B 1.36(3) . ? F2A C1A 1.340(18) . ? F2B C1B 1.36(2) . ? F3A C1A 1.300(18) . ? F3B C1B 1.29(2) . ? O3W H1W 1.03(2) . ? O3W H2W 1.01(3) . ? O81 C81 1.239(14) . ? O82 C82 1.246(13) . ? N11 C21 1.341(12) . ? N11 C61 1.367(12) . ? N11' C21' 1.329(13) . ? N11' C61' 1.338(13) . ? N12 C22 1.311(13) . ? N12 C62 1.343(13) . ? N12' C22' 1.349(13) . ? N12' C62' 1.360(12) . ? N71' C81 1.349(16) . ? N71' C4A' 1.434(14) . ? N71 C81 1.367(15) . ? N71 C4A 1.481(14) . ? N72 C82 1.358(14) . ? N72 C4B 1.458(13) . ? N72' C82 1.359(14) . ? N72' C4B' 1.413(14) . ? C1E H1E1 0.97 . ? C1E H1E2 0.97 . ? C1F H1F1 0.97 . ? C1F H1F2 0.97 . ? C1G H1G1 0.97 . ? C1G H1G2 0.97 . ? C4A C41 1.514(15) . ? C4A H4A1 0.97 . ? C4A H4A2 0.97 . ? C4A' C41' 1.553(15) . ? C4A' H4A3 0.97 . ? C4A' H4A4 0.97 . ? C4B C42 1.526(13) . ? C4B H4B1 0.97 . ? C4B H4B2 0.97 . ? C4B' C42' 1.504(15) . ? C4B' H4B3 0.97 . ? C4B' H4B4 0.97 . ? C21' C31' 1.402(14) . ? C21' H21' 0.93 . ? C21 C31 1.359(14) . ? C21 H21 0.93 . ? C22' C32' 1.388(14) . ? C22' H22' 0.93 . ? C22 C32 1.397(14) . ? C22 H22 0.93 . ? C31 C41 1.389(14) . ? C31 H31 0.93 . ? C31' C41' 1.363(15) . ? C31' H31' 0.93 . ? C32' C42' 1.394(14) . ? C32' H32' 0.93 . ? C32 C42 1.375(14) . ? C32 H32 0.93 . ? C41 C51 1.368(14) . ? C41' C51' 1.371(15) . ? C42 C52 1.376(15) . ? C42' C52' 1.387(16) . ? C51 C61 1.392(14) . ? C51 H51 0.93 . ? C51' C61' 1.391(15) . ? C51' H51' 0.93 . ? C52' C62' 1.354(15) . ? C52' H52' 0.93 . ? C52 C62 1.391(15) . ? C52 H52 0.93 . ? C61 H61 0.93 . ? C61' H61' 0.93 . ? C62 H62 0.93 . ? C62' H62' 0.93 . ? C100 C101 1.566(16) . ? C100 H10A 0.97 . ? C100 H10B 0.97 . ? C101 C102 1.516(18) . ? C101 H10C 0.97 . ? C101 H10D 0.97 . ? C102 H10E 0.97 . ? C102 H10F 0.97 . ? C103 C104 1.366(18) . ? C103 C108 1.397(17) . ? C104 C105 1.43(2) . ? C104 H104 0.93 . ? C105 C106 1.39(2) . ? C105 H105 0.93 . ? C106 C107 1.35(2) . ? C106 H106 0.93 . ? C107 C108 1.371(19) . ? C107 H107 0.93 . ? C108 H108 0.93 . ? C109 C114 1.387(14) . ? C109 C110 1.395(16) . ? C110 C111 1.350(17) . ? C110 H110 0.93 . ? C111 C112 1.392(19) . ? C111 H111 0.93 . ? C112 C113 1.35(2) . ? C112 H112 0.93 . ? C113 C114 1.412(18) . ? C113 H113 0.93 . ? C114 H114 0.93 . ? C115 C116 1.373(15) . ? C115 C120 1.396(14) . ? C116 C117 1.397(17) . ? C116 H116 0.93 . ? C117 C118 1.399(19) . ? C117 H117 0.93 . ? C118 C119 1.353(19) . ? C118 H118 0.93 . ? C119 C120 1.390(16) . ? C119 H119 0.93 . ? C120 H120 0.93 . ? C121 C122 1.38(2) . ? C121 C126 1.44(2) . ? C122 C123 1.411(19) . ? C122 H122 0.93 . ? C123 C124 1.32(3) . ? C123 H123 0.93 . ? C124 C125 1.35(4) . ? C124 H124 0.93 . ? C125 C126 1.43(2) . ? C125 H125 0.93 . ? C126 H126 0.93 . ? C127 C128 1.529(16) . ? C127 H12A 0.97 . ? C127 H12B 0.97 . ? C128 C129 1.545(15) . ? C128 H12C 0.97 . ? C128 H12D 0.97 . ? C129 H12E 0.97 . ? C129 H12F 0.97 . ? C130 C135 1.388(15) . ? C130 C131 1.401(17) . ? C131 C132 1.379(16) . ? C131 H131 0.93 . ? C132 C133 1.359(19) . ? C132 H132 0.93 . ? C133 C134 1.39(2) . ? C133 H133 0.93 . ? C134 C135 1.404(18) . ? C134 H134 0.93 . ? C135 H135 0.93 . ? C136 C137 1.382(18) . ? C136 C141 1.418(19) . ? C137 C138 1.394(17) . ? C137 H137 0.93 . ? C138 C139 1.40(2) . ? C138 H138 0.93 . ? C139 C140 1.32(2) . ? C139 H139 0.93 . ? C140 C141 1.44(2) . ? C140 H140 0.93 . ? C141 H141 0.93 . ? C142 C147 1.367(17) . ? C142 C143 1.417(17) . ? C143 C144 1.396(19) . ? C143 H143 0.93 . ? C144 C145 1.37(2) . ? C144 H144 0.93 . ? C145 C146 1.37(2) . ? C145 H145 0.93 . ? C146 C147 1.377(17) . ? C146 H146 0.93 . ? C147 H147 0.93 . ? C148 C153 1.373(14) . ? C148 C149 1.384(14) . ? C149 C150 1.399(15) . ? C149 H149 0.93 . ? C150 C151 1.369(18) . ? C150 H150 0.93 . ? C151 C152 1.370(16) . ? C151 H151 0.93 . ? C152 C153 1.372(15) . ? C152 H152 0.93 . ? C153 H153 0.93 . ? 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 N11 Pd1 N12 85.7(3) . . ? N11 Pd1 P1 91.3(2) . . ? N12 Pd1 P1 176.9(2) . . ? N11 Pd1 P2 177.5(2) . . ? N12 Pd1 P2 92.7(2) . . ? P1 Pd1 P2 90.35(10) . . ? N11' Pd2 N12' 86.1(3) . . ? N11' Pd2 P4 176.5(2) . . ? N12' Pd2 P4 91.0(2) . . ? N11' Pd2 P3 92.4(2) . . ? N12' Pd2 P3 178.3(2) . . ? P4 Pd2 P3 90.52(10) . . ? C100 P1 C109 106.9(5) . . ? C100 P1 C103 104.2(5) . . ? C109 P1 C103 104.9(5) . . ? C100 P1 Pd1 114.1(4) . . ? C109 P1 Pd1 113.4(4) . . ? C103 P1 Pd1 112.4(3) . . ? C121 P2 C115 105.3(6) . . ? C121 P2 C102 105.9(6) . . ? C115 P2 C102 105.7(5) . . ? C121 P2 Pd1 110.8(4) . . ? C115 P2 Pd1 115.1(3) . . ? C102 P2 Pd1 113.3(4) . . ? C127 P3 C136 105.3(6) . . ? C127 P3 C130 106.1(5) . . ? C136 P3 C130 104.8(5) . . ? C127 P3 Pd2 114.0(4) . . ? C136 P3 Pd2 111.4(4) . . ? C130 P3 Pd2 114.3(4) . . ? C129 P4 C148 106.9(5) . . ? C129 P4 C142 104.3(5) . . ? C148 P4 C142 106.1(5) . . ? C129 P4 Pd2 114.3(4) . . ? C148 P4 Pd2 111.9(3) . . ? C142 P4 Pd2 112.5(4) . . ? O2A S1A O1A 117.4(7) . . ? O2A S1A O3A 110.4(9) . . ? O1A S1A O3A 114.1(6) . . ? O2A S1A C1A 105.6(7) . . ? O1A S1A C1A 105.7(7) . . ? O3A S1A C1A 101.8(8) . . ? O1B S1B O2B 112.8(6) . . ? O1B S1B O3B 110.2(7) . . ? O2B S1B O3B 113.2(7) . . ? O1B S1B C1B 110.6(10) . . ? O2B S1B C1B 105.9(8) . . ? O3B S1B C1B 103.7(10) . . ? O2C S1C O1C 109.9(2) . . ? O2C S1C O3C 109.7(2) . . ? O1C S1C O3C 109.7(2) . . ? O2C S1C C1C 106.8(7) . . ? O1C S1C C1C 106.3(7) . . ? O3C S1C C1C 114.3(7) . . ? F1C C1C F3C 109.4(2) . . ? F1C C1C F2C 109.4(2) . . ? F3C C1C F2C 109.3(2) . . ? F1C C1C S1C 104.5(7) . . ? F3C C1C S1C 110.7(7) . . ? F2C C1C S1C 113.5(7) . . ? O3CB S1CB O2CB 109.5(2) . . ? O3CB S1CB O1CB 109.1(2) . . ? O2CB S1CB O1CB 108.9(2) . . ? O3CB S1CB C1CB 108.4(7) . . ? O2CB S1CB C1CB 109.6(7) . . ? O1CB S1CB C1CB 111.4(8) . . ? F3CB C1CB F1CB 109.4(2) . . ? F3CB C1CB F2CB 109.2(2) . . ? F1CB C1CB F2CB 109.2(2) . . ? F3CB C1CB S1CB 108.2(8) . . ? F1CB C1CB S1CB 109.4(7) . . ? F2CB C1CB S1CB 111.4(8) . . ? O3D S1D O1D 109.3(2) . . ? O3D S1D O2D 109.2(2) . . ? O1D S1D O2D 109.1(2) . . ? O3D S1D C1D 109.9(7) . . ? O1D S1D C1D 109.0(7) . . ? O2D S1D C1D 110.3(7) . . ? F3D C1D F1D 109.4(2) . . ? F3D C1D F2D 109.5(2) . . ? F1D C1D F2D 109.5(2) . . ? F3D C1D S1D 110.3(8) . . ? F1D C1D S1D 109.1(8) . . ? F2D C1D S1D 109.1(7) . . ? O1D' S1D' O3D' 108.9(2) . . ? O1D' S1D' O2D' 108.8(2) . . ? O3D' S1D' O2D' 108.7(2) . . ? O1D' S1D' C1D' 111.7(6) . . ? O3D' S1D' C1D' 108.9(6) . . ? O2D' S1D' C1D' 109.8(6) . . ? F2D' C1D' F3D' 108.8(2) . . ? F2D' C1D' F1D' 109.03(19) . . ? F3D' C1D' F1D' 108.8(2) . . ? F2D' C1D' S1D' 110.7(6) . . ? F3D' C1D' S1D' 108.4(6) . . ? F1D' C1D' S1D' 111.0(6) . . ? H1W O3W H2W 113(3) . . ? C21 N11 C61 117.1(9) . . ? C21 N11 Pd1 122.9(7) . . ? C61 N11 Pd1 120.0(6) . . ? C21' N11' C61' 119.0(9) . . ? C21' N11' Pd2 121.8(7) . . ? C61' N11' Pd2 119.2(7) . . ? C22 N12 C62 118.3(8) . . ? C22 N12 Pd1 122.0(6) . . ? C62 N12 Pd1 119.7(7) . . ? C22' N12' C62' 117.8(8) . . ? C22' N12' Pd2 121.7(6) . . ? C62' N12' Pd2 120.5(7) . . ? C81 N71' C4A' 121.0(11) . . ? C81 N71 C4A 119.9(10) . . ? C82 N72 C4B 121.8(10) . . ? C82 N72' C4B' 119.9(10) . . ? F3A C1A F1A 109.7(16) . . ? F3A C1A F2A 106.1(14) . . ? F1A C1A F2A 105.9(17) . . ? F3A C1A S1A 113.9(13) . . ? F1A C1A S1A 109.5(12) . . ? F2A C1A S1A 111.2(12) . . ? F3B C1B F2B 109.4(17) . . ? F3B C1B F1BB 103(2) . . ? F2B C1B F1BB 108.4(16) . . ? F3B C1B S1B 113.1(13) . . ? F2B C1B S1B 108.8(19) . . ? F1BB C1B S1B 114.2(15) . . ? Cl2 C1E Cl1 112.2(10) . . ? Cl2 C1E H1E1 109.2 . . ? Cl1 C1E H1E1 109.2 . . ? Cl2 C1E H1E2 109.2 . . ? Cl1 C1E H1E2 109.2 . . ? H1E1 C1E H1E2 107.9 . . ? Cl4 C1F Cl3 116.3(19) . . ? Cl4 C1F H1F1 108.2 . . ? Cl3 C1F H1F1 108.2 . . ? Cl4 C1F H1F2 108.2 . . ? Cl3 C1F H1F2 108.2 . . ? H1F1 C1F H1F2 107.4 . . ? Cl5 C1G Cl6 107.2(8) . . ? Cl5 C1G H1G1 110.3 . . ? Cl6 C1G H1G1 110.3 . . ? Cl5 C1G H1G2 110.3 . . ? Cl6 C1G H1G2 110.3 . . ? H1G1 C1G H1G2 108.5 . . ? N71 C4A C41 114.3(9) . . ? N71 C4A H4A1 108.7 . . ? C41 C4A H4A1 108.7 . . ? N71 C4A H4A2 108.7 . . ? C41 C4A H4A2 108.7 . . ? H4A1 C4A H4A2 107.6 . . ? N71' C4A' C41' 112.8(9) . . ? N71' C4A' H4A3 109 . . ? C41' C4A' H4A3 109 . . ? N71' C4A' H4A4 109 . . ? C41' C4A' H4A4 109 . . ? H4A3 C4A' H4A4 107.8 . . ? N72 C4B C42 112.9(8) . . ? N72 C4B H4B1 109 . . ? C42 C4B H4B1 109 . . ? N72 C4B H4B2 109 . . ? C42 C4B H4B2 109 . . ? H4B1 C4B H4B2 107.8 . . ? N72' C4B' C42' 116.2(9) . . ? N72' C4B' H4B3 108.2 . . ? C42' C4B' H4B3 108.2 . . ? N72' C4B' H4B4 108.2 . . ? C42' C4B' H4B4 108.2 . . ? H4B3 C4B' H4B4 107.4 . . ? N11' C21' C31' 121.2(10) . . ? N11' C21' H21' 119.4 . . ? C31' C21' H21' 119.4 . . ? N11 C21 C31 122.9(9) . . ? N11 C21 H21 118.6 . . ? C31 C21 H21 118.6 . . ? N12' C22' C32' 121.8(8) . . ? N12' C22' H22' 119.1 . . ? C32' C22' H22' 119.1 . . ? N12 C22 C32 122.5(9) . . ? N12 C22 H22 118.7 . . ? C32 C22 H22 118.7 . . ? C21 C31 C41 120.6(10) . . ? C21 C31 H31 119.7 . . ? C41 C31 H31 119.7 . . ? C41' C31' C21' 119.5(10) . . ? C41' C31' H31' 120.3 . . ? C21' C31' H31' 120.3 . . ? C22' C32' C42' 120.2(10) . . ? C22' C32' H32' 119.9 . . ? C42' C32' H32' 119.9 . . ? C42 C32 C22 120.3(10) . . ? C42 C32 H32 119.8 . . ? C22 C32 H32 119.8 . . ? C51 C41 C31 117.6(10) . . ? C51 C41 C4A 118.4(9) . . ? C31 C41 C4A 124.1(9) . . ? C31' C41' C51' 119.5(10) . . ? C31' C41' C4A' 122.2(10) . . ? C51' C41' C4A' 118.3(10) . . ? C32 C42 C52 116.5(9) . . ? C32 C42 C4B 123.7(9) . . ? C52 C42 C4B 119.7(9) . . ? C52' C42' C32' 116.6(10) . . ? C52' C42' C4B' 120.7(9) . . ? C32' C42' C4B' 122.7(10) . . ? C41 C51 C61 119.8(9) . . ? C41 C51 H51 120.1 . . ? C61 C51 H51 120.1 . . ? C41' C51' C61' 118.4(10) . . ? C41' C51' H51' 120.8 . . ? C61' C51' H51' 120.8 . . ? C62' C52' C42' 121.3(10) . . ? C62' C52' H52' 119.3 . . ? C42' C52' H52' 119.3 . . ? C42 C52 C62 120.6(9) . . ? C42 C52 H52 119.7 . . ? C62 C52 H52 119.7 . . ? N11 C61 C51 122.0(9) . . ? N11 C61 H61 119 . . ? C51 C61 H61 119 . . ? N11' C61' C51' 122.5(10) . . ? N11' C61' H61' 118.8 . . ? C51' C61' H61' 118.8 . . ? N12 C62 C52 121.6(10) . . ? N12 C62 H62 119.2 . . ? C52 C62 H62 119.2 . . ? C52' C62' N12' 122.2(10) . . ? C52' C62' H62' 118.9 . . ? N12' C62' H62' 118.9 . . ? O81 C81 N71' 125.5(12) . . ? O81 C81 N71 121.4(12) . . ? N71' C81 N71 113.1(10) . . ? O82 C82 N72 121.7(11) . . ? O82 C82 N72' 123.0(11) . . ? N72 C82 N72' 115.2(10) . . ? C101 C100 P1 114.2(8) . . ? C101 C100 H10A 108.7 . . ? P1 C100 H10A 108.7 . . ? C101 C100 H10B 108.7 . . ? P1 C100 H10B 108.7 . . ? H10A C100 H10B 107.6 . . ? C102 C101 C100 112.7(9) . . ? C102 C101 H10C 109.1 . . ? C100 C101 H10C 109.1 . . ? C102 C101 H10D 109.1 . . ? C100 C101 H10D 109.1 . . ? H10C C101 H10D 107.8 . . ? C101 C102 P2 114.0(8) . . ? C101 C102 H10E 108.8 . . ? P2 C102 H10E 108.8 . . ? C101 C102 H10F 108.8 . . ? P2 C102 H10F 108.8 . . ? H10E C102 H10F 107.7 . . ? C104 C103 C108 121.0(12) . . ? C104 C103 P1 119.9(10) . . ? C108 C103 P1 118.8(9) . . ? C103 C104 C105 118.0(15) . . ? C103 C104 H104 121 . . ? C105 C104 H104 121 . . ? C106 C105 C104 119.8(16) . . ? C106 C105 H105 120.1 . . ? C104 C105 H105 120.1 . . ? C107 C106 C105 120.0(15) . . ? C107 C106 H106 120 . . ? C105 C106 H106 120 . . ? C106 C107 C108 121.6(16) . . ? C106 C107 H107 119.2 . . ? C108 C107 H107 119.2 . . ? C107 C108 C103 119.5(14) . . ? C107 C108 H108 120.3 . . ? C103 C108 H108 120.3 . . ? C114 C109 C110 118.2(11) . . ? C114 C109 P1 121.8(9) . . ? C110 C109 P1 120.0(8) . . ? C111 C110 C109 121.5(11) . . ? C111 C110 H110 119.2 . . ? C109 C110 H110 119.2 . . ? C110 C111 C112 121.3(13) . . ? C110 C111 H111 119.4 . . ? C112 C111 H111 119.4 . . ? C113 C112 C111 117.6(12) . . ? C113 C112 H112 121.2 . . ? C111 C112 H112 121.2 . . ? C112 C113 C114 122.9(12) . . ? C112 C113 H113 118.6 . . ? C114 C113 H113 118.6 . . ? C109 C114 C113 118.4(12) . . ? C109 C114 H114 120.8 . . ? C113 C114 H114 120.8 . . ? C116 C115 C120 119.8(10) . . ? C116 C115 P2 119.4(8) . . ? C120 C115 P2 120.8(8) . . ? C115 C116 C117 119.7(12) . . ? C115 C116 H116 120.1 . . ? C117 C116 H116 120.1 . . ? C116 C117 C118 120.3(13) . . ? C116 C117 H117 119.8 . . ? C118 C117 H117 119.8 . . ? C119 C118 C117 119.3(11) . . ? C119 C118 H118 120.4 . . ? C117 C118 H118 120.4 . . ? C118 C119 C120 121.3(12) . . ? C118 C119 H119 119.4 . . ? C120 C119 H119 119.4 . . ? C119 C120 C115 119.6(11) . . ? C119 C120 H120 120.2 . . ? C115 C120 H120 120.2 . . ? C122 C121 C126 118.6(13) . . ? C122 C121 P2 121.1(10) . . ? C126 C121 P2 120.0(12) . . ? C121 C122 C123 119.8(16) . . ? C121 C122 H122 120.1 . . ? C123 C122 H122 120.1 . . ? C124 C123 C122 124(2) . . ? C124 C123 H123 118 . . ? C122 C123 H123 118 . . ? C123 C124 C125 117(2) . . ? C123 C124 H124 121.6 . . ? C125 C124 H124 121.6 . . ? C124 C125 C126 125(2) . . ? C124 C125 H125 117.6 . . ? C126 C125 H125 117.6 . . ? C121 C126 C125 115.9(19) . . ? C121 C126 H126 122.1 . . ? C125 C126 H126 122.1 . . ? C128 C127 P3 115.2(8) . . ? C128 C127 H12A 108.5 . . ? P3 C127 H12A 108.5 . . ? C128 C127 H12B 108.5 . . ? P3 C127 H12B 108.5 . . ? H12A C127 H12B 107.5 . . ? C127 C128 C129 113.2(9) . . ? C127 C128 H12C 108.9 . . ? C129 C128 H12C 108.9 . . ? C127 C128 H12D 108.9 . . ? C129 C128 H12D 108.9 . . ? H12C C128 H12D 107.8 . . ? C128 C129 P4 114.3(7) . . ? C128 C129 H12E 108.7 . . ? P4 C129 H12E 108.7 . . ? C128 C129 H12F 108.7 . . ? P4 C129 H12F 108.7 . . ? H12E C129 H12F 107.6 . . ? C135 C130 C131 119.7(11) . . ? C135 C130 P3 120.6(9) . . ? C131 C130 P3 119.7(8) . . ? C132 C131 C130 119.1(12) . . ? C132 C131 H131 120.5 . . ? C130 C131 H131 120.5 . . ? C133 C132 C131 122.9(15) . . ? C133 C132 H132 118.5 . . ? C131 C132 H132 118.5 . . ? C132 C133 C134 117.8(12) . . ? C132 C133 H133 121.1 . . ? C134 C133 H133 121.1 . . ? C133 C134 C135 121.5(13) . . ? C133 C134 H134 119.3 . . ? C135 C134 H134 119.3 . . ? C130 C135 C134 118.8(13) . . ? C130 C135 H135 120.6 . . ? C134 C135 H135 120.6 . . ? C137 C136 C141 118.4(12) . . ? C137 C136 P3 121.8(10) . . ? C141 C136 P3 119.8(11) . . ? C136 C137 C138 122.4(13) . . ? C136 C137 H137 118.8 . . ? C138 C137 H137 118.8 . . ? C137 C138 C139 119.5(14) . . ? C137 C138 H138 120.3 . . ? C139 C138 H138 120.3 . . ? C140 C139 C138 118.8(14) . . ? C140 C139 H139 120.6 . . ? C138 C139 H139 120.6 . . ? C139 C140 C141 124.4(17) . . ? C139 C140 H140 117.8 . . ? C141 C140 H140 117.8 . . ? C136 C141 C140 116.4(16) . . ? C136 C141 H141 121.8 . . ? C140 C141 H141 121.8 . . ? C147 C142 C143 120.9(11) . . ? C147 C142 P4 120.3(9) . . ? C143 C142 P4 118.7(10) . . ? C144 C143 C142 117.4(15) . . ? C144 C143 H143 121.3 . . ? C142 C143 H143 121.3 . . ? C145 C144 C143 120.9(16) . . ? C145 C144 H144 119.6 . . ? C143 C144 H144 119.6 . . ? C146 C145 C144 120.3(14) . . ? C146 C145 H145 119.9 . . ? C144 C145 H145 119.9 . . ? C145 C146 C147 120.7(15) . . ? C145 C146 H146 119.6 . . ? C147 C146 H146 119.6 . . ? C142 C147 C146 119.7(13) . . ? C142 C147 H147 120.1 . . ? C146 C147 H147 120.1 . . ? C153 C148 C149 119.5(9) . . ? C153 C148 P4 120.5(7) . . ? C149 C148 P4 120.0(8) . . ? C148 C149 C150 119.4(10) . . ? C148 C149 H149 120.3 . . ? C150 C149 H149 120.3 . . ? C151 C150 C149 119.7(10) . . ? C151 C150 H150 120.2 . . ? C149 C150 H150 120.2 . . ? C150 C151 C152 120.6(10) . . ? C150 C151 H151 119.7 . . ? C152 C151 H151 119.7 . . ? C151 C152 C153 119.7(11) . . ? C151 C152 H152 120.1 . . ? C153 C152 H152 120.1 . . ? C152 C153 C148 120.9(10) . . ? C152 C153 H153 119.5 . . ? C148 C153 H153 119.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 Pd1 P1 C100 134.4(5) . . . . ? N12 Pd1 P1 C100 150(4) . . . . ? P2 Pd1 P1 C100 -43.6(4) . . . . ? N11 Pd1 P1 C109 -102.9(5) . . . . ? N12 Pd1 P1 C109 -87(4) . . . . ? P2 Pd1 P1 C109 79.1(4) . . . . ? N11 Pd1 P1 C103 15.9(5) . . . . ? N12 Pd1 P1 C103 32(4) . . . . ? P2 Pd1 P1 C103 -162.1(4) . . . . ? N11 Pd1 P2 C121 33(5) . . . . ? N12 Pd1 P2 C121 -18.4(6) . . . . ? P1 Pd1 P2 C121 162.3(5) . . . . ? N11 Pd1 P2 C115 152(5) . . . . ? N12 Pd1 P2 C115 100.9(4) . . . . ? P1 Pd1 P2 C115 -78.3(4) . . . . ? N11 Pd1 P2 C102 -86(5) . . . . ? N12 Pd1 P2 C102 -137.2(5) . . . . ? P1 Pd1 P2 C102 43.5(5) . . . . ? N11' Pd2 P3 C127 -136.1(5) . . . . ? N12' Pd2 P3 C127 -113(8) . . . . ? P4 Pd2 P3 C127 42.0(4) . . . . ? N11' Pd2 P3 C136 -17.1(5) . . . . ? N12' Pd2 P3 C136 6(8) . . . . ? P4 Pd2 P3 C136 161.0(5) . . . . ? N11' Pd2 P3 C130 101.6(5) . . . . ? N12' Pd2 P3 C130 124(8) . . . . ? P4 Pd2 P3 C130 -80.4(4) . . . . ? N11' Pd2 P4 C129 104(4) . . . . ? N12' Pd2 P4 C129 137.5(4) . . . . ? P3 Pd2 P4 C129 -41.8(4) . . . . ? N11' Pd2 P4 C148 -134(4) . . . . ? N12' Pd2 P4 C148 -100.8(4) . . . . ? P3 Pd2 P4 C148 79.9(4) . . . . ? N11' Pd2 P4 C142 -15(4) . . . . ? N12' Pd2 P4 C142 18.7(5) . . . . ? P3 Pd2 P4 C142 -160.6(5) . . . . ? O2C S1C C1C F1C -46.3(5) . . . . ? O1C S1C C1C F1C -163.6(5) . . . . ? O3C S1C C1C F1C 75.2(7) . . . . ? O2C S1C C1C F3C -164.0(5) . . . . ? O1C S1C C1C F3C 78.7(7) . . . . ? O3C S1C C1C F3C -42.4(7) . . . . ? O2C S1C C1C F2C 72.7(7) . . . . ? O1C S1C C1C F2C -44.6(6) . . . . ? O3C S1C C1C F2C -165.7(5) . . . . ? O3CB S1CB C1CB F3CB -46.9(5) . . . . ? O2CB S1CB C1CB F3CB -166.4(5) . . . . ? O1CB S1CB C1CB F3CB 73.1(6) . . . . ? O3CB S1CB C1CB F1CB -166.0(5) . . . . ? O2CB S1CB C1CB F1CB 74.6(7) . . . . ? O1CB S1CB C1CB F1CB -46.0(6) . . . . ? O3CB S1CB C1CB F2CB 73.2(7) . . . . ? O2CB S1CB C1CB F2CB -46.3(6) . . . . ? O1CB S1CB C1CB F2CB -166.8(5) . . . . ? O3D S1D C1D F3D -45.7(6) . . . . ? O1D S1D C1D F3D 74.0(7) . . . . ? O2D S1D C1D F3D -166.2(5) . . . . ? O3D S1D C1D F1D 74.5(7) . . . . ? O1D S1D C1D F1D -165.8(5) . . . . ? O2D S1D C1D F1D -46.0(6) . . . . ? O3D S1D C1D F2D -166.0(5) . . . . ? O1D S1D C1D F2D -46.2(6) . . . . ? O2D S1D C1D F2D 73.5(7) . . . . ? O1D' S1D' C1D' F2D' -47.9(5) . . . . ? O3D' S1D' C1D' F2D' 72.4(6) . . . . ? O2D' S1D' C1D' F2D' -168.7(5) . . . . ? O1D' S1D' C1D' F3D' 71.4(6) . . . . ? O3D' S1D' C1D' F3D' -168.3(5) . . . . ? O2D' S1D' C1D' F3D' -49.4(5) . . . . ? O1D' S1D' C1D' F1D' -169.2(5) . . . . ? O3D' S1D' C1D' F1D' -48.9(5) . . . . ? O2D' S1D' C1D' F1D' 70.0(6) . . . . ? N12 Pd1 N11 C21 -80.6(7) . . . . ? P1 Pd1 N11 C21 98.6(7) . . . . ? P2 Pd1 N11 C21 -132(5) . . . . ? N12 Pd1 N11 C61 101.4(7) . . . . ? P1 Pd1 N11 C61 -79.4(6) . . . . ? P2 Pd1 N11 C61 50(5) . . . . ? N12' Pd2 N11' C21' 84.3(8) . . . . ? P4 Pd2 N11' C21' 118(4) . . . . ? P3 Pd2 N11' C21' -96.3(8) . . . . ? N12' Pd2 N11' C61' -93.9(8) . . . . ? P4 Pd2 N11' C61' -61(4) . . . . ? P3 Pd2 N11' C61' 85.5(8) . . . . ? N11 Pd1 N12 C22 83.7(9) . . . . ? P1 Pd1 N12 C22 68(5) . . . . ? P2 Pd1 N12 C22 -98.3(8) . . . . ? N11 Pd1 N12 C62 -95.8(8) . . . . ? P1 Pd1 N12 C62 -112(4) . . . . ? P2 Pd1 N12 C62 82.2(8) . . . . ? N11' Pd2 N12' C22' -85.5(8) . . . . ? P4 Pd2 N12' C22' 96.4(7) . . . . ? P3 Pd2 N12' C22' -108(8) . . . . ? N11' Pd2 N12' C62' 94.6(8) . . . . ? P4 Pd2 N12' C62' -83.5(8) . . . . ? P3 Pd2 N12' C62' 72(8) . . . . ? O2A S1A C1A F3A -57.2(16) . . . . ? O1A S1A C1A F3A 177.7(12) . . . . ? O3A S1A C1A F3A 58.2(15) . . . . ? O2A S1A C1A F1A 66.1(16) . . . . ? O1A S1A C1A F1A -59.0(15) . . . . ? O3A S1A C1A F1A -178.5(14) . . . . ? O2A S1A C1A F2A -177.1(14) . . . . ? O1A S1A C1A F2A 57.8(15) . . . . ? O3A S1A C1A F2A -61.8(14) . . . . ? O1B S1B C1B F3B 54(2) . . . . ? O2B S1B C1B F3B 176.1(16) . . . . ? O3B S1B C1B F3B -64.5(19) . . . . ? O1B S1B C1B F2B 175.5(12) . . . . ? O2B S1B C1B F2B -62.0(15) . . . . ? O3B S1B C1B F2B 57.4(14) . . . . ? O1B S1B C1B F1BB -63.2(17) . . . . ? O2B S1B C1B F1BB 59.3(18) . . . . ? O3B S1B C1B F1BB 178.7(15) . . . . ? C81 N71 C4A C41 76.6(13) . . . . ? C81 N71' C4A' C41' -100.7(13) . . . . ? C82 N72 C4B C42 -98.7(12) . . . . ? C82 N72' C4B' C42' 81.9(12) . . . . ? C61' N11' C21' C31' -0.2(16) . . . . ? Pd2 N11' C21' C31' -178.4(8) . . . . ? C61 N11 C21 C31 0.3(14) . . . . ? Pd1 N11 C21 C31 -177.7(8) . . . . ? C62' N12' C22' C32' 1.5(15) . . . . ? Pd2 N12' C22' C32' -178.3(7) . . . . ? C62 N12 C22 C32 0.0(17) . . . . ? Pd1 N12 C22 C32 -179.6(10) . . . . ? N11 C21 C31 C41 -0.3(16) . . . . ? N11' C21' C31' C41' 2.3(17) . . . . ? N12' C22' C32' C42' -3.0(16) . . . . ? N12 C22 C32 C42 2(2) . . . . ? C21 C31 C41 C51 -0.2(15) . . . . ? C21 C31 C41 C4A -179.5(10) . . . . ? N71 C4A C41 C51 -177.3(9) . . . . ? N71 C4A C41 C31 2.0(16) . . . . ? C21' C31' C41' C51' -2.9(18) . . . . ? C21' C31' C41' C4A' 176.1(11) . . . . ? N71' C4A' C41' C31' 22.5(19) . . . . ? N71' C4A' C41' C51' -158.4(12) . . . . ? C22 C32 C42 C52 -3.5(19) . . . . ? C22 C32 C42 C4B -179.8(11) . . . . ? N72 C4B C42 C32 17.9(17) . . . . ? N72 C4B C42 C52 -158.3(11) . . . . ? C22' C32' C42' C52' 2.0(16) . . . . ? C22' C32' C42' C4B' -179.6(10) . . . . ? N72' C4B' C42' C52' -174.8(11) . . . . ? N72' C4B' C42' C32' 6.9(16) . . . . ? C31 C41 C51 C61 0.6(14) . . . . ? C4A C41 C51 C61 180.0(9) . . . . ? C31' C41' C51' C61' 1.5(18) . . . . ? C4A' C41' C51' C61' -177.6(11) . . . . ? C32' C42' C52' C62' 0.4(17) . . . . ? C4B' C42' C52' C62' -178.0(11) . . . . ? C32 C42 C52 C62 3.6(18) . . . . ? C4B C42 C52 C62 -179.9(11) . . . . ? C21 N11 C61 C51 0.2(13) . . . . ? Pd1 N11 C61 C51 178.3(6) . . . . ? C41 C51 C61 N11 -0.7(13) . . . . ? C21' N11' C61' C51' -1.3(16) . . . . ? Pd2 N11' C61' C51' 176.9(9) . . . . ? C41' C51' C61' N11' 0.7(18) . . . . ? C22 N12 C62 C52 0.2(17) . . . . ? Pd1 N12 C62 C52 179.7(9) . . . . ? C42 C52 C62 N12 -2.1(19) . . . . ? C42' C52' C62' N12' -2.0(18) . . . . ? C22' N12' C62' C52' 0.9(16) . . . . ? Pd2 N12' C62' C52' -179.2(9) . . . . ? C4A' N71' C81 O81 1.5(16) . . . . ? C4A' N71' C81 N71 -177.3(9) . . . . ? C4A N71 C81 O81 -1.6(15) . . . . ? C4A N71 C81 N71' 177.3(9) . . . . ? C4B N72 C82 O82 1.3(14) . . . . ? C4B N72 C82 N72' -178.4(8) . . . . ? C4B' N72' C82 O82 0.2(14) . . . . ? C4B' N72' C82 N72 179.8(8) . . . . ? C109 P1 C100 C101 -65.0(10) . . . . ? C103 P1 C100 C101 -175.8(8) . . . . ? Pd1 P1 C100 C101 61.2(9) . . . . ? P1 C100 C101 C102 -71.6(12) . . . . ? C100 C101 C102 P2 72.2(11) . . . . ? C121 P2 C102 C101 175.5(9) . . . . ? C115 P2 C102 C101 64.1(10) . . . . ? Pd1 P2 C102 C101 -62.8(9) . . . . ? C100 P1 C103 C104 -32.8(11) . . . . ? C109 P1 C103 C104 -145.0(10) . . . . ? Pd1 P1 C103 C104 91.3(10) . . . . ? C100 P1 C103 C108 153.3(9) . . . . ? C109 P1 C103 C108 41.1(10) . . . . ? Pd1 P1 C103 C108 -82.5(9) . . . . ? C108 C103 C104 C105 -2.7(19) . . . . ? P1 C103 C104 C105 -176.4(10) . . . . ? C103 C104 C105 C106 4(2) . . . . ? C104 C105 C106 C107 -3(2) . . . . ? C105 C106 C107 C108 1(2) . . . . ? C106 C107 C108 C103 -0.2(19) . . . . ? C104 C103 C108 C107 0.9(17) . . . . ? P1 C103 C108 C107 174.7(9) . . . . ? C100 P1 C109 C114 -30.9(12) . . . . ? C103 P1 C109 C114 79.4(11) . . . . ? Pd1 P1 C109 C114 -157.6(9) . . . . ? C100 P1 C109 C110 149.5(10) . . . . ? C103 P1 C109 C110 -100.2(11) . . . . ? Pd1 P1 C109 C110 22.9(11) . . . . ? C114 C109 C110 C111 -3(2) . . . . ? P1 C109 C110 C111 176.9(11) . . . . ? C109 C110 C111 C112 3(2) . . . . ? C110 C111 C112 C113 -1(2) . . . . ? C111 C112 C113 C114 -1(2) . . . . ? C110 C109 C114 C113 0.9(18) . . . . ? P1 C109 C114 C113 -178.7(10) . . . . ? C112 C113 C114 C109 1(2) . . . . ? C121 P2 C115 C116 93.8(10) . . . . ? C102 P2 C115 C116 -154.4(9) . . . . ? Pd1 P2 C115 C116 -28.6(10) . . . . ? C121 P2 C115 C120 -86.7(10) . . . . ? C102 P2 C115 C120 25.1(10) . . . . ? Pd1 P2 C115 C120 151.0(7) . . . . ? C120 C115 C116 C117 0.8(18) . . . . ? P2 C115 C116 C117 -179.6(10) . . . . ? C115 C116 C117 C118 -1(2) . . . . ? C116 C117 C118 C119 2(2) . . . . ? C117 C118 C119 C120 -2(2) . . . . ? C118 C119 C120 C115 1.3(18) . . . . ? C116 C115 C120 C119 -0.8(16) . . . . ? P2 C115 C120 C119 179.7(9) . . . . ? C115 P2 C121 C122 -36.6(12) . . . . ? C102 P2 C121 C122 -148.3(11) . . . . ? Pd1 P2 C121 C122 88.5(11) . . . . ? C115 P2 C121 C126 149.8(11) . . . . ? C102 P2 C121 C126 38.1(12) . . . . ? Pd1 P2 C121 C126 -85.1(11) . . . . ? C126 C121 C122 C123 -2(2) . . . . ? P2 C121 C122 C123 -175.5(11) . . . . ? C121 C122 C123 C124 1(3) . . . . ? C122 C123 C124 C125 0(4) . . . . ? C123 C124 C125 C126 1(5) . . . . ? C122 C121 C126 C125 2(2) . . . . ? P2 C121 C126 C125 176.2(15) . . . . ? C124 C125 C126 C121 -2(4) . . . . ? C136 P3 C127 C128 176.4(8) . . . . ? C130 P3 C127 C128 65.6(9) . . . . ? Pd2 P3 C127 C128 -61.2(9) . . . . ? P3 C127 C128 C129 71.6(11) . . . . ? C127 C128 C129 P4 -70.5(11) . . . . ? C148 P4 C129 C128 -64.4(9) . . . . ? C142 P4 C129 C128 -176.6(8) . . . . ? Pd2 P4 C129 C128 60.1(8) . . . . ? C127 P3 C130 C135 23.5(11) . . . . ? C136 P3 C130 C135 -87.7(10) . . . . ? Pd2 P3 C130 C135 150.0(8) . . . . ? C127 P3 C130 C131 -157.0(10) . . . . ? C136 P3 C130 C131 91.9(10) . . . . ? Pd2 P3 C130 C131 -30.4(11) . . . . ? C135 C130 C131 C132 0.3(19) . . . . ? P3 C130 C131 C132 -179.3(10) . . . . ? C130 C131 C132 C133 -2(2) . . . . ? C131 C132 C133 C134 3(2) . . . . ? C132 C133 C134 C135 -3(2) . . . . ? C131 C130 C135 C134 -0.7(18) . . . . ? P3 C130 C135 C134 178.9(10) . . . . ? C133 C134 C135 C130 2(2) . . . . ? C127 P3 C136 C137 -155.8(9) . . . . ? C130 P3 C136 C137 -44.1(11) . . . . ? Pd2 P3 C136 C137 80.1(9) . . . . ? C127 P3 C136 C141 26.6(11) . . . . ? C130 P3 C136 C141 138.4(10) . . . . ? Pd2 P3 C136 C141 -97.5(10) . . . . ? C141 C136 C137 C138 1.8(17) . . . . ? P3 C136 C137 C138 -175.7(9) . . . . ? C136 C137 C138 C139 0.7(18) . . . . ? C137 C138 C139 C140 0(2) . . . . ? C138 C139 C140 C141 -4(3) . . . . ? C137 C136 C141 C140 -4.9(18) . . . . ? P3 C136 C141 C140 172.7(11) . . . . ? C139 C140 C141 C136 6(3) . . . . ? C129 P4 C142 C147 149.3(9) . . . . ? C148 P4 C142 C147 36.5(11) . . . . ? Pd2 P4 C142 C147 -86.2(10) . . . . ? C129 P4 C142 C143 -34.4(11) . . . . ? C148 P4 C142 C143 -147.1(10) . . . . ? Pd2 P4 C142 C143 90.2(10) . . . . ? C147 C142 C143 C144 0(2) . . . . ? P4 C142 C143 C144 -176.0(13) . . . . ? C142 C143 C144 C145 -3(3) . . . . ? C143 C144 C145 C146 4(3) . . . . ? C144 C145 C146 C147 -4(3) . . . . ? C143 C142 C147 C146 -0.1(18) . . . . ? P4 C142 C147 C146 176.2(10) . . . . ? C145 C146 C147 C142 2(2) . . . . ? C129 P4 C148 C153 145.8(9) . . . . ? C142 P4 C148 C153 -103.2(10) . . . . ? Pd2 P4 C148 C153 19.9(10) . . . . ? C129 P4 C148 C149 -33.9(11) . . . . ? C142 P4 C148 C149 77.0(10) . . . . ? Pd2 P4 C148 C149 -159.8(8) . . . . ? C153 C148 C149 C150 -0.2(19) . . . . ? P4 C148 C149 C150 179.6(10) . . . . ? C148 C149 C150 C151 -3(2) . . . . ? C149 C150 C151 C152 4(2) . . . . ? C150 C151 C152 C153 -3(2) . . . . ? C151 C152 C153 C148 0.1(19) . . . . ? C149 C148 C153 C152 1.5(18) . . . . ? P4 C148 C153 C152 -178.2(10) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 192 58 ' ' 2 0.083 0.000 0.996 9 4 ' ' 3 0.917 0.000 0.004 8 3 ' ' 4 0.028 0.041 0.927 9 3 ' ' 5 0.329 0.172 0.352 10 2 ' ' 6 0.399 0.222 0.987 17 7 ' ' 7 0.944 0.224 0.545 16 7 ' ' 8 0.448 0.282 0.051 14 5 ' ' 9 0.894 0.283 0.482 15 5 ' ' 10 0.500 0.500 1.000 192 58 ' ' 11 0.829 0.328 0.852 10 2 ' ' 12 0.532 0.463 0.433 10 3 ' ' 13 0.417 0.500 0.504 8 3 ' ' 14 0.588 0.503 0.502 8 3 ' ' 15 0.472 0.541 0.573 9 2 ' ' 16 0.171 0.672 0.148 10 1 ' ' 17 0.101 0.722 0.513 18 8 ' ' 18 0.556 0.724 0.955 15 6 ' ' 19 0.052 0.782 0.448 13 5 ' ' 20 0.606 0.783 0.018 16 6 ' ' 21 0.671 0.828 0.648 10 1 ' ' 22 0.972 0.959 0.073 9 2 ' ' _platon_squeeze_details ; ; # END of CIF