Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Stephen Loeb' _publ_contact_author_address ; Dept of Chemistry & Biochemistry University of Windsor Windsor Ontario N9B 3P4 CANADA ; _publ_contact_author_email LOEB@UWINDSOR.CA _publ_section_title ; 4,4'-Bipyridine-N-monoxide. A hybrid ligand for building networks using a combination of metal-ligand and hydrogen-bonding interactions ; loop_ _publ_author_name 'Stephen Loeb' 'Nicolle C. Habermehl' 'Dennis J. Hoffart' data_[Cu(H2O)2(BIPYMO)4][PF6]2 _database_code_depnum_ccdc_archive 'CCDC 639375' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H39 Cu F12 N8 O7.50 P2' _chemical_formula_weight 1105.27 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4nc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.183(8) _cell_length_b 17.183(8) _cell_length_c 8.128(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2400(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.5 _exptl_crystal_description blue _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.857200 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 100 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 18137 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2113 _reflns_number_gt 1777 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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. The PF6 anion is positionally disordered with two water molecules and needed to be restrained to attain a chemically reasonable geometry. The disordered PF6 was restrained (DFIX) to have P-F distances of 1.58 A and F-F distances of 2.22 A. The water molecules were restrained (anti-bumping) to have a minimum distance of 2.85 A. ; _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^)+(0.0707P)^2^+5.9652P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(4) _refine_ls_number_reflns 2113 _refine_ls_number_parameters 208 _refine_ls_number_restraints 145 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.1719 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.165 _refine_ls_shift/su_max 0.084 _refine_ls_shift/su_mean 0.008 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 Cu1 Cu 0.0000 0.0000 -0.0035(3) 0.0273(4) Uani 1 4 d S . . O1 O 0.4884(2) -0.3560(3) -0.0400(13) 0.104(4) Uani 1 1 d . . . O1W O 0.0000 0.0000 -0.2970(14) 0.041(3) Uani 1 4 d S . . H1W H -0.0012 -0.0461 -0.3314 0.049 Uiso 0.50 1 calc PR . . O2W O 0.0000 0.0000 0.2770(13) 0.040(3) Uani 1 4 d S . . H2W H -0.0004 -0.0461 0.3114 0.047 Uiso 0.50 1 calc PR . . N1 N 0.1003(2) -0.0641(2) -0.0034(9) 0.0298(10) Uani 1 1 d . . . N2 N 0.4284(3) -0.3090(3) -0.0290(12) 0.065(2) Uani 1 1 d . . . C1 C 0.1605(3) -0.0483(3) -0.1019(9) 0.0353(14) Uani 1 1 d . . . H1A H 0.1569 -0.0047 -0.1734 0.042 Uiso 1 1 calc R . . C2 C 0.2280(4) -0.0925(3) -0.1048(9) 0.0384(15) Uani 1 1 d . . . H2A H 0.2699 -0.0788 -0.1754 0.046 Uiso 1 1 calc R . . C3 C 0.2334(3) -0.1575(3) -0.0019(12) 0.0334(12) Uani 1 1 d . . . C4 C 0.1721(4) -0.1730(4) 0.1002(8) 0.0365(14) Uani 1 1 d . . . H4A H 0.1740 -0.2163 0.1727 0.044 Uiso 1 1 calc R . . C5 C 0.1073(4) -0.1255(3) 0.0976(8) 0.0352(15) Uani 1 1 d . . . H5A H 0.0657 -0.1368 0.1707 0.042 Uiso 1 1 calc R . . C6 C 0.3024(3) -0.2094(3) -0.0107(13) 0.0377(13) Uani 1 1 d . . . C7 C 0.3751(4) -0.1831(4) -0.0557(10) 0.051(2) Uani 1 1 d . . . H7A H 0.3824 -0.1297 -0.0820 0.062 Uiso 1 1 calc R . . C8 C 0.4381(4) -0.2342(4) -0.0631(13) 0.068(3) Uani 1 1 d . . . H8A H 0.4882 -0.2153 -0.0926 0.082 Uiso 1 1 calc R . . C9 C 0.3583(3) -0.3365(3) 0.0211(12) 0.047(2) Uani 1 1 d . . . H9A H 0.3529 -0.3894 0.0526 0.056 Uiso 1 1 calc R . . C10 C 0.2958(4) -0.2878(4) 0.0262(10) 0.044(2) Uani 1 1 d . . . H10A H 0.2463 -0.3082 0.0557 0.053 Uiso 1 1 calc R . . P1 P 0.0827(3) -0.3845(4) -0.2326(9) 0.100(2) Uani 0.50 1 d PDU A -1 F1 F 0.1098(13) -0.3932(14) -0.4150(17) 0.243(10) Uani 0.50 1 d PDU A -1 F2 F 0.1669(8) -0.3778(13) -0.175(3) 0.208(11) Uani 0.50 1 d PDU A -1 F3 F 0.0895(12) -0.4758(7) -0.217(4) 0.286(13) Uani 0.50 1 d PDU A -1 F4 F 0.0746(8) -0.2976(6) -0.254(2) 0.177(8) Uani 0.50 1 d PDU A -1 F5 F -0.0027(6) -0.3984(10) -0.289(3) 0.219(10) Uani 0.50 1 d PDU A -1 F6 F 0.0514(15) -0.3797(15) -0.0550(19) 0.325(13) Uani 0.50 1 d PDU A -1 O1S O 0.157(2) -0.390(3) -0.269(7) 0.27(3) Uani 0.50 1 d PD B -2 O2S O 0.028(2) -0.436(2) -0.465(8) 0.18(2) Uani 0.25 1 d PD C -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0171(4) 0.0171(4) 0.0476(7) 0.000 0.000 0.000 O1 0.023(2) 0.037(3) 0.252(12) -0.044(5) -0.020(4) 0.0150(19) O1W 0.029(4) 0.029(4) 0.063(8) 0.000 0.000 0.000 O2W 0.037(4) 0.037(4) 0.046(7) 0.000 0.000 0.000 N1 0.0204(19) 0.024(2) 0.045(2) 0.006(3) 0.004(4) 0.0019(16) N2 0.028(3) 0.036(3) 0.130(7) -0.033(4) -0.014(4) 0.007(2) C1 0.028(3) 0.029(3) 0.049(4) 0.005(3) 0.009(3) 0.002(2) C2 0.026(3) 0.031(3) 0.058(4) -0.001(3) 0.008(3) 0.000(2) C3 0.026(3) 0.026(2) 0.047(3) 0.000(4) -0.009(4) 0.005(2) C4 0.031(4) 0.031(4) 0.047(4) 0.003(3) 0.000(3) 0.006(3) C5 0.028(3) 0.028(3) 0.049(4) 0.004(3) 0.005(3) 0.007(3) C6 0.029(3) 0.031(3) 0.053(3) -0.006(4) -0.009(4) 0.006(2) C7 0.030(3) 0.033(3) 0.091(7) -0.018(3) 0.002(3) 0.008(3) C8 0.029(3) 0.037(4) 0.138(10) -0.025(4) -0.004(4) 0.010(3) C9 0.030(3) 0.026(3) 0.084(6) -0.012(4) -0.012(4) -0.002(2) C10 0.032(3) 0.034(3) 0.068(6) -0.011(4) -0.006(4) 0.002(2) P1 0.052(3) 0.117(5) 0.129(5) 0.055(5) -0.005(3) -0.003(3) F1 0.194(18) 0.37(2) 0.163(12) -0.075(16) 0.032(13) -0.01(3) F2 0.118(11) 0.24(2) 0.26(2) 0.08(2) -0.090(13) -0.042(13) F3 0.18(2) 0.111(8) 0.56(4) 0.088(18) -0.13(3) 0.016(12) F4 0.113(11) 0.105(7) 0.31(2) 0.046(11) 0.100(13) 0.007(8) F5 0.057(7) 0.133(14) 0.47(3) 0.01(2) -0.007(11) 0.024(7) F6 0.35(3) 0.43(3) 0.200(14) 0.134(19) 0.139(17) 0.06(3) O1S 0.18(3) 0.25(4) 0.38(7) 0.09(4) -0.11(3) -0.14(3) O2S 0.08(2) 0.13(3) 0.31(8) 0.01(4) -0.02(4) 0.06(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.046(4) 4 ? Cu1 N1 2.046(4) 3 ? Cu1 N1 2.046(4) . ? Cu1 N1 2.046(4) 2 ? Cu1 O2W 2.280(11) . ? Cu1 O1W 2.385(12) . ? O1 N2 1.312(7) . ? N1 C1 1.335(8) . ? N1 C5 1.342(8) . ? N2 C8 1.326(10) . ? N2 C9 1.355(9) . ? C1 C2 1.387(8) . ? C2 C3 1.399(9) . ? C3 C4 1.367(10) . ? C3 C6 1.485(7) . ? C4 C5 1.380(9) . ? C6 C7 1.378(9) . ? C6 C10 1.385(9) . ? C7 C8 1.396(9) . ? C9 C10 1.362(9) . ? P1 F2 1.525(11) . ? P1 F4 1.509(10) . ? P1 F6 1.543(11) . ? P1 F5 1.556(10) . ? P1 F1 1.560(10) . ? P1 F3 1.579(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 N1 Cu1 N1 179.9(4) 4 3 ? N1 Cu1 N1 90.0 4 . ? N1 Cu1 N1 90.0 3 . ? N1 Cu1 N1 90.0 4 2 ? N1 Cu1 N1 90.0 3 2 ? N1 Cu1 N1 179.9(4) . 2 ? N1 Cu1 O2W 90.0(2) 4 . ? N1 Cu1 O2W 90.0(2) 3 . ? N1 Cu1 O2W 90.0(2) . . ? N1 Cu1 O2W 90.0(2) 2 . ? N1 Cu1 O1W 90.0(2) 4 . ? N1 Cu1 O1W 90.0(2) 3 . ? N1 Cu1 O1W 90.0(2) . . ? N1 Cu1 O1W 90.0(2) 2 . ? O2W Cu1 O1W 180 . . ? C1 N1 C5 117.2(5) . . ? C1 N1 Cu1 122.9(4) . . ? C5 N1 Cu1 119.9(4) . . ? O1 N2 C8 118.9(6) . . ? O1 N2 C9 120.3(6) . . ? C8 N2 C9 120.8(6) . . ? N1 C1 C2 123.1(6) . . ? C1 C2 C3 118.8(6) . . ? C4 C3 C2 117.9(5) . . ? C4 C3 C6 121.8(6) . . ? C2 C3 C6 120.2(7) . . ? C3 C4 C5 119.8(6) . . ? N1 C5 C4 123.1(6) . . ? C7 C6 C10 116.8(5) . . ? C7 C6 C3 122.6(5) . . ? C10 C6 C3 120.6(6) . . ? C6 C7 C8 120.5(7) . . ? N2 C8 C7 120.2(7) . . ? N2 C9 C10 119.7(6) . . ? C9 C10 C6 121.7(6) . . ? F2 P1 F4 92.8(8) . . ? F2 P1 F6 92.2(8) . . ? F4 P1 F6 91.4(8) . . ? F2 P1 F5 175.5(9) . . ? F4 P1 F5 91.7(7) . . ? F6 P1 F5 87.4(7) . . ? F2 P1 F1 91.0(7) . . ? F4 P1 F1 90.7(8) . . ? F6 P1 F1 176.1(10) . . ? F5 P1 F1 89.2(8) . . ? F2 P1 F3 88.9(7) . . ? F4 P1 F3 177.6(9) . . ? F6 P1 F3 90.2(8) . . ? F5 P1 F3 86.6(7) . . ? F1 P1 F3 87.6(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.587 _refine_diff_density_min -0.269 _refine_diff_density_rms 0.079 # Attachment 'B703456C-Pd.cif' data_[Pd(BIPYMO)4][OTf]2 _database_code_depnum_ccdc_archive 'CCDC 639376' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41.33 H42 B0.67 F6.67 N8 O18 Pd S1.33' _chemical_formula_weight 1187.28 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' B B 0.0013 0.0007 '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' 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 20.6240(18) _cell_length_b 21.3105(19) _cell_length_c 22.366(2) _cell_angle_alpha 63.191(2) _cell_angle_beta 64.445(2) _cell_angle_gamma 82.821(2) _cell_volume 7885.5(12) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.5 _exptl_crystal_description pale-yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3724 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.863733 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 100 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 63630 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 27687 _reflns_number_gt 20306 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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. The two BF4 anions and one of the CF3SO3 anions needed to be restrained to attain chemically reasonable geometries. B-F, F-F, S-O, C-F, F...F and O...O distances were restrained to be equal using the SADI and SIMU commands. ; _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^)+(0.1474P)^2^+32.9059P] 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 27687 _refine_ls_number_parameters 2080 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2481 _refine_ls_wR_factor_gt 0.2219 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.136 _refine_ls_shift/su_mean 0.002 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 -0.68698(2) 0.25377(2) 0.39340(3) 0.02379(14) Uani 1 1 d . . . O1 O -1.1094(3) -0.1321(3) 0.6765(3) 0.0436(13) Uani 1 1 d . . . O2 O -0.2796(2) 0.6539(2) 0.1296(3) 0.0357(11) Uani 1 1 d . . . O3 O -0.3028(3) -0.1094(3) 0.3899(3) 0.0489(14) Uani 1 1 d . . . O4 O -1.0679(3) 0.6192(3) 0.3918(3) 0.0492(14) Uani 1 1 d . . . N1 N -0.7676(3) 0.1771(3) 0.4484(3) 0.0240(11) Uani 1 1 d . . . N2 N -1.0578(3) -0.0823(3) 0.6430(3) 0.0351(13) Uani 1 1 d . . . N3 N -0.6072(3) 0.3321(3) 0.3388(3) 0.0257(11) Uani 1 1 d . . . N4 N -0.3297(3) 0.6032(3) 0.1623(3) 0.0289(12) Uani 1 1 d . . . N5 N -0.6136(3) 0.1809(3) 0.3969(3) 0.0266(11) Uani 1 1 d . . . N6 N -0.3517(3) -0.0651(3) 0.3929(3) 0.0377(14) Uani 1 1 d . . . N7 N -0.7617(3) 0.3253(3) 0.3923(3) 0.0240(11) Uani 1 1 d . . . N8 N -1.0214(3) 0.5715(3) 0.3923(3) 0.0374(14) Uani 1 1 d . . . C1 C -0.7792(3) 0.1264(3) 0.5157(3) 0.0281(14) Uani 1 1 d . . . H1A H -0.7472 0.1256 0.5363 0.034 Uiso 1 1 calc R . . C2 C -0.8360(3) 0.0754(3) 0.5564(3) 0.0292(14) Uani 1 1 d . . . H2A H -0.8427 0.0399 0.6041 0.035 Uiso 1 1 calc R . . C3 C -0.8843(3) 0.0760(3) 0.5267(3) 0.0288(14) Uani 1 1 d . . . C4 C -0.8706(4) 0.1289(3) 0.4565(4) 0.0324(15) Uani 1 1 d . . . H4A H -0.9017 0.1313 0.4343 0.039 Uiso 1 1 calc R . . C5 C -0.8123(3) 0.1779(3) 0.4185(4) 0.0280(13) Uani 1 1 d . . . H5A H -0.8033 0.2132 0.3701 0.034 Uiso 1 1 calc R . . C6 C -0.9448(3) 0.0219(3) 0.5683(3) 0.0297(14) Uani 1 1 d . . . C7 C -0.9412(4) -0.0465(4) 0.6171(4) 0.0380(16) Uani 1 1 d . . . H7A H -0.8990 -0.0583 0.6256 0.046 Uiso 1 1 calc R . . C8 C -0.9962(4) -0.0966(4) 0.6528(4) 0.0392(17) Uani 1 1 d . . . H8A H -0.9917 -0.1430 0.6854 0.047 Uiso 1 1 calc R . . C9 C -1.0640(4) -0.0149(4) 0.5974(4) 0.0365(16) Uani 1 1 d . . . H9A H -1.1076 -0.0038 0.5917 0.044 Uiso 1 1 calc R . . C10 C -1.0099(4) 0.0363(4) 0.5604(4) 0.0331(15) Uani 1 1 d . . . H10A H -1.0157 0.0825 0.5286 0.040 Uiso 1 1 calc R . . C11 C -0.6133(3) 0.3822(3) 0.3609(4) 0.0308(14) Uani 1 1 d . . . H11A H -0.6563 0.3807 0.4017 0.037 Uiso 1 1 calc R . . C12 C -0.5606(3) 0.4353(3) 0.3278(4) 0.0317(15) Uani 1 1 d . . . H12A H -0.5683 0.4703 0.3450 0.038 Uiso 1 1 calc R . . C13 C -0.4952(3) 0.4386(3) 0.2686(3) 0.0279(14) Uani 1 1 d . . . C14 C -0.4894(3) 0.3858(3) 0.2456(4) 0.0301(14) Uani 1 1 d . . . H14A H -0.4468 0.3854 0.2055 0.036 Uiso 1 1 calc R . . C15 C -0.5451(3) 0.3350(3) 0.2810(3) 0.0277(13) Uani 1 1 d . . . H15A H -0.5399 0.3001 0.2643 0.033 Uiso 1 1 calc R . . C16 C -0.4372(3) 0.4947(3) 0.2319(3) 0.0282(14) Uani 1 1 d . . . C17 C -0.4474(4) 0.5516(4) 0.2488(4) 0.0382(16) Uani 1 1 d . . . H17A H -0.4925 0.5536 0.2854 0.046 Uiso 1 1 calc R . . C18 C -0.3946(4) 0.6047(4) 0.2142(4) 0.0357(16) Uani 1 1 d . . . H18A H -0.4035 0.6430 0.2267 0.043 Uiso 1 1 calc R . . C19 C -0.3177(4) 0.5490(4) 0.1450(4) 0.0371(16) Uani 1 1 d . . . H19A H -0.2719 0.5479 0.1086 0.044 Uiso 1 1 calc R . . C20 C -0.3702(4) 0.4949(4) 0.1785(4) 0.0353(15) Uani 1 1 d . . . H20A H -0.3602 0.4573 0.1649 0.042 Uiso 1 1 calc R . . C21 C -0.5640(3) 0.1816(3) 0.4193(4) 0.0303(14) Uani 1 1 d . . . H21A H -0.5646 0.2154 0.4363 0.036 Uiso 1 1 calc R . . C22 C -0.5117(3) 0.1348(3) 0.4188(4) 0.0304(14) Uani 1 1 d . . . H22A H -0.4760 0.1378 0.4338 0.036 Uiso 1 1 calc R . . C23 C -0.5104(4) 0.0830(3) 0.3965(4) 0.0316(14) Uani 1 1 d . . . C24 C -0.5643(4) 0.0825(4) 0.3748(4) 0.0383(16) Uani 1 1 d . . . H24A H -0.5664 0.0481 0.3595 0.046 Uiso 1 1 calc R . . C25 C -0.6136(4) 0.1311(4) 0.3752(4) 0.0362(16) Uani 1 1 d . . . H25A H -0.6496 0.1300 0.3598 0.043 Uiso 1 1 calc R . . C26 C -0.4556(4) 0.0312(3) 0.3961(4) 0.0314(14) Uani 1 1 d . . . C27 C -0.3878(4) 0.0470(4) 0.3871(4) 0.0438(18) Uani 1 1 d . . . H27A H -0.3765 0.0915 0.3822 0.053 Uiso 1 1 calc R . . C28 C -0.3374(4) -0.0003(4) 0.3852(5) 0.0455(18) Uani 1 1 d . . . H28A H -0.2911 0.0119 0.3784 0.055 Uiso 1 1 calc R . . C29 C -0.4183(4) -0.0822(4) 0.4042(4) 0.0371(16) Uani 1 1 d . . . H29A H -0.4298 -0.1279 0.4121 0.045 Uiso 1 1 calc R . . C30 C -0.4698(4) -0.0341(4) 0.4046(4) 0.0355(15) Uani 1 1 d . . . H30A H -0.5157 -0.0465 0.4107 0.043 Uiso 1 1 calc R . . C31 C -0.8154(3) 0.3198(3) 0.4553(3) 0.0300(14) Uani 1 1 d . . . H31A H -0.8174 0.2824 0.5004 0.036 Uiso 1 1 calc R . . C32 C -0.8685(4) 0.3662(3) 0.4578(3) 0.0315(14) Uani 1 1 d . . . H32A H -0.9068 0.3601 0.5037 0.038 Uiso 1 1 calc R . . C33 C -0.8649(3) 0.4220(3) 0.3919(3) 0.0260(13) Uani 1 1 d . . . C34 C -0.8084(3) 0.4273(3) 0.3265(3) 0.0290(14) Uani 1 1 d . . . H34A H -0.8043 0.4645 0.2804 0.035 Uiso 1 1 calc R . . C35 C -0.7581(3) 0.3780(3) 0.3288(3) 0.0276(13) Uani 1 1 d . . . H35A H -0.7197 0.3818 0.2837 0.033 Uiso 1 1 calc R . . C36 C -0.9200(4) 0.4736(4) 0.3922(3) 0.0308(14) Uani 1 1 d . . . C37 C -0.9910(4) 0.4538(4) 0.4443(4) 0.0346(15) Uani 1 1 d . . . H37A H -1.0051 0.4062 0.4809 0.041 Uiso 1 1 calc R . . C38 C -1.0409(4) 0.5030(4) 0.4433(4) 0.0362(16) Uani 1 1 d . . . H38A H -1.0897 0.4889 0.4787 0.043 Uiso 1 1 calc R . . C39 C -0.9528(4) 0.5912(4) 0.3412(4) 0.0458(19) Uani 1 1 d . . . H39A H -0.9396 0.6392 0.3054 0.055 Uiso 1 1 calc R . . C40 C -0.9020(4) 0.5441(4) 0.3394(4) 0.0388(16) Uani 1 1 d . . . H40A H -0.8540 0.5591 0.3022 0.047 Uiso 1 1 calc R . . Pd2 Pd -0.83411(2) -0.66155(2) 0.74871(3) 0.02490(14) Uani 1 1 d . . . O5 O -1.2289(3) -1.0679(2) 1.0014(3) 0.0474(13) Uani 1 1 d . . . O6 O -0.4339(3) -0.2539(3) 0.4778(3) 0.0493(14) Uani 1 1 d . . . O7 O -0.4473(4) -1.0188(4) 0.7322(4) 0.076(2) Uani 1 1 d . . . O8 O -1.2092(2) -0.2876(2) 0.7512(2) 0.0352(11) Uani 1 1 d . . . N9 N -0.9113(3) -0.7409(3) 0.7970(3) 0.0277(11) Uani 1 1 d . . . N10 N -1.1776(3) -1.0174(3) 0.9669(3) 0.0353(13) Uani 1 1 d . . . N11 N -0.7544(3) -0.5838(3) 0.6994(3) 0.0262(11) Uani 1 1 d . . . N12 N -0.4832(3) -0.3077(3) 0.5139(3) 0.0382(14) Uani 1 1 d . . . N13 N -0.7595(3) -0.7325(3) 0.7473(3) 0.0267(11) Uani 1 1 d . . . N14 N -0.4965(4) -0.9731(4) 0.7361(4) 0.0538(19) Uani 1 1 d . . . N15 N -0.9087(3) -0.5900(3) 0.7490(3) 0.0269(11) Uani 1 1 d . . . N16 N -1.1626(3) -0.3340(3) 0.7511(3) 0.0288(12) Uani 1 1 d . . . C41 C -0.9188(4) -0.7978(4) 0.8601(4) 0.0379(16) Uani 1 1 d . . . H41A H -0.8891 -0.7995 0.8834 0.045 Uiso 1 1 calc R . . C42 C -0.9678(4) -0.8531(4) 0.8915(4) 0.0399(17) Uani 1 1 d . . . H42A H -0.9704 -0.8933 0.9352 0.048 Uiso 1 1 calc R . . C43 C -1.0143(3) -0.8519(3) 0.8611(4) 0.0293(14) Uani 1 1 d . . . C44 C -1.0057(3) -0.7925(3) 0.7953(4) 0.0304(14) Uani 1 1 d . . . H44A H -1.0357 -0.7890 0.7716 0.036 Uiso 1 1 calc R . . C45 C -0.9532(3) -0.7388(3) 0.7650(4) 0.0308(14) Uani 1 1 d . . . H45A H -0.9471 -0.6991 0.7196 0.037 Uiso 1 1 calc R . . C46 C -1.0700(4) -0.9098(3) 0.8965(4) 0.0320(14) Uani 1 1 d . . . C47 C -1.0606(4) -0.9790(4) 0.9379(4) 0.0366(16) Uani 1 1 d . . . H47A H -1.0163 -0.9900 0.9422 0.044 Uiso 1 1 calc R . . C48 C -1.1141(4) -1.0318(4) 0.9727(4) 0.0385(17) Uani 1 1 d . . . H48A H -1.1068 -1.0789 1.0011 0.046 Uiso 1 1 calc R . . C49 C -1.1870(4) -0.9517(4) 0.9243(5) 0.0431(18) Uani 1 1 d . . . H49A H -1.2307 -0.9425 0.9183 0.052 Uiso 1 1 calc R . . C50 C -1.1350(4) -0.8982(4) 0.8895(4) 0.0414(17) Uani 1 1 d . . . H50A H -1.1430 -0.8520 0.8598 0.050 Uiso 1 1 calc R . . C51 C -0.7593(3) -0.5386(3) 0.7274(3) 0.0289(14) Uani 1 1 d . . . H51A H -0.7999 -0.5443 0.7719 0.035 Uiso 1 1 calc R . . C52 C -0.7070(3) -0.4840(3) 0.6934(3) 0.0297(14) Uani 1 1 d . . . H52A H -0.7128 -0.4517 0.7135 0.036 Uiso 1 1 calc R . . C53 C -0.6450(3) -0.4759(3) 0.6289(3) 0.0282(14) Uani 1 1 d . . . C54 C -0.6409(4) -0.5247(4) 0.6034(4) 0.0370(16) Uani 1 1 d . . . H54A H -0.5996 -0.5223 0.5608 0.044 Uiso 1 1 calc R . . C55 C -0.6954(4) -0.5766(4) 0.6385(4) 0.0356(16) Uani 1 1 d . . . H55A H -0.6911 -0.6090 0.6188 0.043 Uiso 1 1 calc R . . C56 C -0.5885(4) -0.4182(3) 0.5905(4) 0.0315(14) Uani 1 1 d . . . C57 C -0.6055(4) -0.3527(4) 0.5889(5) 0.0444(18) Uani 1 1 d . . . H57A H -0.6540 -0.3457 0.6150 0.053 Uiso 1 1 calc R . . C58 C -0.5529(4) -0.2977(4) 0.5499(5) 0.0447(19) Uani 1 1 d . . . H58A H -0.5655 -0.2526 0.5482 0.054 Uiso 1 1 calc R . . C59 C -0.4659(4) -0.3711(4) 0.5173(4) 0.0360(16) Uani 1 1 d . . . H59A H -0.4167 -0.3779 0.4932 0.043 Uiso 1 1 calc R . . C60 C -0.5164(3) -0.4265(4) 0.5540(4) 0.0338(15) Uani 1 1 d . . . H60A H -0.5023 -0.4709 0.5548 0.041 Uiso 1 1 calc R . . C61 C -0.7120(4) -0.7351(3) 0.7738(4) 0.0319(15) Uani 1 1 d . . . H61A H -0.7145 -0.7040 0.7944 0.038 Uiso 1 1 calc R . . C62 C -0.6599(4) -0.7814(4) 0.7722(4) 0.0344(15) Uani 1 1 d . . . H62A H -0.6255 -0.7810 0.7897 0.041 Uiso 1 1 calc R . . C63 C -0.6572(4) -0.8293(3) 0.7445(4) 0.0316(14) Uani 1 1 d . . . C64 C -0.7087(4) -0.8279(4) 0.7200(4) 0.0344(15) Uani 1 1 d . . . H64A H -0.7096 -0.8608 0.7026 0.041 Uiso 1 1 calc R . . C65 C -0.7586(4) -0.7785(3) 0.7209(4) 0.0320(15) Uani 1 1 d . . . H65A H -0.7930 -0.7768 0.7025 0.038 Uiso 1 1 calc R . . C66 C -0.6022(4) -0.8807(4) 0.7430(4) 0.0360(16) Uani 1 1 d . . . C67 C -0.5295(4) -0.8586(5) 0.7141(5) 0.050(2) Uani 1 1 d . . . H67A H -0.5160 -0.8103 0.6968 0.060 Uiso 1 1 calc R . . C68 C -0.4779(5) -0.9044(5) 0.7103(5) 0.058(2) Uani 1 1 d . . . H68A H -0.4286 -0.8882 0.6895 0.070 Uiso 1 1 calc R . . C69 C -0.5665(5) -0.9971(4) 0.7663(5) 0.052(2) Uani 1 1 d . . . H69A H -0.5788 -1.0459 0.7853 0.063 Uiso 1 1 calc R . . C70 C -0.6199(5) -0.9516(4) 0.7698(4) 0.0426(18) Uani 1 1 d . . . H70A H -0.6688 -0.9687 0.7905 0.051 Uiso 1 1 calc R . . C71 C -0.9712(3) -0.6026(3) 0.8094(3) 0.0286(14) Uani 1 1 d . . . H71A H -0.9807 -0.6465 0.8520 0.034 Uiso 1 1 calc R . . C72 C -1.0216(4) -0.5540(3) 0.8113(4) 0.0319(15) Uani 1 1 d . . . H72A H -1.0652 -0.5650 0.8549 0.038 Uiso 1 1 calc R . . C73 C -1.0096(3) -0.4890(3) 0.7506(3) 0.0259(13) Uani 1 1 d . . . C74 C -0.9444(3) -0.4772(3) 0.6885(3) 0.0299(14) Uani 1 1 d . . . H74A H -0.9331 -0.4336 0.6451 0.036 Uiso 1 1 calc R . . C75 C -0.8972(3) -0.5279(3) 0.6900(3) 0.0304(14) Uani 1 1 d . . . H75A H -0.8537 -0.5186 0.6467 0.037 Uiso 1 1 calc R . . C76 C -1.0625(3) -0.4349(3) 0.7509(3) 0.0274(13) Uani 1 1 d . . . C77 C -1.1315(3) -0.4505(4) 0.8094(4) 0.0324(15) Uani 1 1 d . . . H77A H -1.1448 -0.4962 0.8500 0.039 Uiso 1 1 calc R . . C78 C -1.1795(4) -0.4004(3) 0.8083(4) 0.0326(15) Uani 1 1 d . . . H78A H -1.2260 -0.4120 0.8484 0.039 Uiso 1 1 calc R . . C79 C -1.0961(4) -0.3180(4) 0.6948(4) 0.0344(15) Uani 1 1 d . . . H79A H -1.0834 -0.2720 0.6548 0.041 Uiso 1 1 calc R . . C80 C -1.0469(3) -0.3669(3) 0.6944(4) 0.0325(15) Uani 1 1 d . . . H80A H -1.0005 -0.3539 0.6541 0.039 Uiso 1 1 calc R . . Pd3 Pd 0.25025(2) 0.18823(2) 0.10291(2) 0.02307(14) Uani 1 1 d . . . O9 O -0.1575(2) -0.2139(2) 0.3713(3) 0.0353(11) Uani 1 1 d . . . O10 O 0.6374(3) 0.6067(2) -0.1745(2) 0.0387(12) Uani 1 1 d . . . O11 O -0.1251(3) 0.5579(3) 0.1151(3) 0.0461(13) Uani 1 1 d . . . O12 O 0.6227(3) -0.1867(3) 0.0960(3) 0.0438(12) Uani 1 1 d . . . N17 N 0.1707(3) 0.1088(3) 0.1579(3) 0.0253(11) Uani 1 1 d . . . N18 N -0.1063(3) -0.1636(3) 0.3376(3) 0.0291(12) Uani 1 1 d . . . N19 N 0.3269(3) 0.2691(3) 0.0477(3) 0.0226(10) Uani 1 1 d . . . N20 N 0.5880(3) 0.5553(3) -0.1415(3) 0.0310(12) Uani 1 1 d . . . N21 N 0.1753(3) 0.2593(3) 0.1055(3) 0.0233(11) Uani 1 1 d . . . N22 N -0.0779(3) 0.5116(3) 0.1127(3) 0.0361(13) Uani 1 1 d . . . N23 N 0.3271(3) 0.1185(3) 0.0993(3) 0.0260(11) Uani 1 1 d . . . N24 N 0.5774(3) -0.1389(3) 0.0985(3) 0.0339(13) Uani 1 1 d . . . C81 C 0.1699(3) 0.0477(3) 0.2142(3) 0.0299(14) Uani 1 1 d . . . H81A H 0.2071 0.0417 0.2301 0.036 Uiso 1 1 calc R . . C82 C 0.1178(3) -0.0065(3) 0.2497(3) 0.0277(13) Uani 1 1 d . . . H82A H 0.1203 -0.0496 0.2884 0.033 Uiso 1 1 calc R . . C83 C 0.0611(3) 0.0010(3) 0.2297(3) 0.0270(13) Uani 1 1 d . . . C84 C 0.0623(3) 0.0651(3) 0.1716(3) 0.0294(14) Uani 1 1 d . . . H84A H 0.0248 0.0731 0.1557 0.035 Uiso 1 1 calc R . . C85 C 0.1166(3) 0.1164(3) 0.1373(3) 0.0280(13) Uani 1 1 d . . . H85A H 0.1164 0.1593 0.0973 0.034 Uiso 1 1 calc R . . C86 C 0.0031(3) -0.0560(3) 0.2667(3) 0.0265(13) Uani 1 1 d . . . C87 C 0.0040(4) -0.1226(3) 0.3210(4) 0.0353(16) Uani 1 1 d . . . H87A H 0.0432 -0.1321 0.3345 0.042 Uiso 1 1 calc R . . C88 C -0.0500(4) -0.1746(4) 0.3551(4) 0.0371(16) Uani 1 1 d . . . H88A H -0.0476 -0.2193 0.3918 0.044 Uiso 1 1 calc R . . C89 C -0.1105(4) -0.0995(3) 0.2863(4) 0.0340(15) Uani 1 1 d . . . H89A H -0.1511 -0.0911 0.2749 0.041 Uiso 1 1 calc R . . C90 C -0.0570(4) -0.0467(3) 0.2507(4) 0.0331(15) Uani 1 1 d . . . H90A H -0.0606 -0.0025 0.2141 0.040 Uiso 1 1 calc R . . C91 C 0.3248(3) 0.3116(3) 0.0772(3) 0.0265(13) Uani 1 1 d . . . H91A H 0.2889 0.3015 0.1255 0.032 Uiso 1 1 calc R . . C92 C 0.3736(3) 0.3705(3) 0.0392(4) 0.0286(14) Uani 1 1 d . . . H92A H 0.3696 0.4011 0.0608 0.034 Uiso 1 1 calc R . . C93 C 0.4284(3) 0.3847(3) -0.0304(3) 0.0248(13) Uani 1 1 d . . . C94 C 0.4302(3) 0.3377(3) -0.0591(3) 0.0292(14) Uani 1 1 d . . . H94A H 0.4669 0.3447 -0.1061 0.035 Uiso 1 1 calc R . . C95 C 0.3790(3) 0.2819(3) -0.0193(4) 0.0290(14) Uani 1 1 d . . . H95A H 0.3805 0.2511 -0.0400 0.035 Uiso 1 1 calc R . . C96 C 0.4826(3) 0.4442(3) -0.0702(3) 0.0275(13) Uani 1 1 d . . . C97 C 0.4660(3) 0.5071(3) -0.0631(4) 0.0310(14) Uani 1 1 d . . . H97A H 0.4182 0.5124 -0.0331 0.037 Uiso 1 1 calc R . . C98 C 0.5196(4) 0.5613(3) -0.1001(3) 0.0304(14) Uani 1 1 d . . . H98A H 0.5076 0.6042 -0.0960 0.037 Uiso 1 1 calc R . . C99 C 0.6041(4) 0.4966(4) -0.1513(4) 0.0372(16) Uani 1 1 d . . . H99A H 0.6518 0.4932 -0.1831 0.045 Uiso 1 1 calc R . . C100 C 0.5527(4) 0.4415(4) -0.1159(4) 0.0367(16) Uani 1 1 d . . . H10B H 0.5659 0.4002 -0.1231 0.044 Uiso 1 1 calc R . . C101 C 0.1223(3) 0.2526(3) 0.1696(3) 0.0268(13) Uani 1 1 d . . . H10C H 0.1200 0.2139 0.2142 0.032 Uiso 1 1 calc R . . C102 C 0.0707(3) 0.3002(3) 0.1730(3) 0.0298(14) Uani 1 1 d . . . H10D H 0.0326 0.2934 0.2193 0.036 Uiso 1 1 calc R . . C103 C 0.0748(3) 0.3586(3) 0.1080(3) 0.0277(13) Uani 1 1 d . . . C104 C 0.1312(3) 0.3646(3) 0.0419(3) 0.0301(14) Uani 1 1 d . . . H10E H 0.1363 0.4035 -0.0036 0.036 Uiso 1 1 calc R . . C105 C 0.1793(3) 0.3138(3) 0.0428(3) 0.0267(13) Uani 1 1 d . . . H10F H 0.2167 0.3177 -0.0028 0.032 Uiso 1 1 calc R . . C106 C 0.0216(4) 0.4116(3) 0.1099(3) 0.0298(14) Uani 1 1 d . . . C107 C -0.0511(4) 0.3929(4) 0.1580(4) 0.0407(17) Uani 1 1 d . . . H10G H -0.0672 0.3447 0.1912 0.049 Uiso 1 1 calc R . . C108 C -0.0993(4) 0.4419(4) 0.1584(4) 0.0442(18) Uani 1 1 d . . . H10H H -0.1488 0.4275 0.1909 0.053 Uiso 1 1 calc R . . C109 C -0.0075(4) 0.5323(4) 0.0655(4) 0.0371(16) Uani 1 1 d . . . H10I H 0.0075 0.5810 0.0340 0.044 Uiso 1 1 calc R . . C110 C 0.0425(4) 0.4830(4) 0.0630(4) 0.0341(15) Uani 1 1 d . . . H11B H 0.0916 0.4980 0.0290 0.041 Uiso 1 1 calc R . . C111 C 0.3807(3) 0.1209(3) 0.1170(4) 0.0316(14) Uani 1 1 d . . . H11C H 0.3836 0.1571 0.1297 0.038 Uiso 1 1 calc R . . C112 C 0.4316(3) 0.0725(3) 0.1175(4) 0.0300(14) Uani 1 1 d . . . H11D H 0.4698 0.0765 0.1290 0.036 Uiso 1 1 calc R . . C113 C 0.4276(3) 0.0177(3) 0.1012(3) 0.0288(14) Uani 1 1 d . . . C114 C 0.3707(3) 0.0165(3) 0.0829(4) 0.0293(14) Uani 1 1 d . . . H11E H 0.3655 -0.0199 0.0714 0.035 Uiso 1 1 calc R . . C115 C 0.3230(3) 0.0672(3) 0.0815(3) 0.0287(14) Uani 1 1 d . . . H11F H 0.2858 0.0661 0.0675 0.034 Uiso 1 1 calc R . . C116 C 0.4792(4) -0.0364(3) 0.1019(4) 0.0319(15) Uani 1 1 d . . . C117 C 0.4610(4) -0.1015(4) 0.1104(4) 0.0388(16) Uani 1 1 d . . . H11G H 0.4138 -0.1118 0.1179 0.047 Uiso 1 1 calc R . . C118 C 0.5100(4) -0.1510(4) 0.1082(4) 0.0387(16) Uani 1 1 d . . . H11H H 0.4963 -0.1949 0.1136 0.046 Uiso 1 1 calc R . . C119 C 0.5962(4) -0.0761(4) 0.0909(4) 0.0344(15) Uani 1 1 d . . . H11I H 0.6435 -0.0673 0.0842 0.041 Uiso 1 1 calc R . . C120 C 0.5496(4) -0.0254(4) 0.0926(4) 0.0314(14) Uani 1 1 d . . . H12B H 0.5645 0.0179 0.0876 0.038 Uiso 1 1 calc R . . S1 S -0.43434(14) 0.35639(12) 0.60969(14) 0.0619(6) Uani 1 1 d . . . O13 O -0.3692(7) 0.3996(6) 0.5520(6) 0.156(5) Uani 1 1 d . . . O14 O -0.4897(7) 0.3995(6) 0.6197(6) 0.155(5) Uani 1 1 d . . . O15 O -0.4403(7) 0.3030(5) 0.5939(6) 0.132(4) Uani 1 1 d . . . C121 C -0.4168(8) 0.3177(6) 0.6877(7) 0.091(4) Uani 1 1 d . . . F1 F -0.3667(10) 0.2799(10) 0.6851(9) 0.298(12) Uani 1 1 d . . . F2 F -0.4783(7) 0.2821(7) 0.7456(6) 0.189(5) Uani 1 1 d . . . F3 F -0.4087(6) 0.3616(6) 0.7111(6) 0.160(4) Uani 1 1 d . . . S2 S -0.84580(14) -0.05859(14) 0.89252(14) 0.0673(7) Uani 1 1 d . . . O16 O -0.8288(9) 0.0125(5) 0.8521(7) 0.172(6) Uani 1 1 d . . . O17 O -0.8196(6) -0.0944(7) 0.9450(5) 0.141(5) Uani 1 1 d . . . O18 O -0.9198(5) -0.0752(6) 0.9142(6) 0.136(4) Uani 1 1 d . . . C122 C -0.8006(6) -0.0931(7) 0.8270(7) 0.084(3) Uani 1 1 d . . . F4 F -0.8211(6) -0.0696(7) 0.7736(6) 0.159(4) Uani 1 1 d . . . F5 F -0.7293(4) -0.0830(5) 0.7995(5) 0.130(3) Uani 1 1 d . . . F6 F -0.8129(5) -0.1628(5) 0.8573(6) 0.147(4) Uani 1 1 d . . . S3 S -0.45552(15) 0.22712(16) 0.0981(2) 0.0852(9) Uani 1 1 d U . . O19 O -0.5041(11) 0.2270(13) 0.1656(8) 0.385(16) Uani 1 1 d DU . . O20 O -0.4757(11) 0.2579(9) 0.0453(10) 0.257(9) Uani 1 1 d DU . . O21 O -0.4308(6) 0.1600(5) 0.1091(8) 0.196(7) Uani 1 1 d DU . . C123 C -0.3746(12) 0.2845(10) 0.0508(11) 0.177(7) Uani 1 1 d DU . . F7 F -0.3329(10) 0.2721(8) -0.0093(8) 0.244(7) Uani 1 1 d DU . . F8 F -0.3874(10) 0.3532(9) 0.0244(10) 0.277(9) Uani 1 1 d DU . . F9 F -0.3385(5) 0.2657(6) 0.0923(6) 0.164(4) Uani 1 1 d DU . . S4 S -0.2581(3) 0.2569(3) 0.2977(3) 0.1367(18) Uani 1 1 d . . . O22 O -0.2019(9) 0.2112(9) 0.2884(9) 0.203(7) Uani 1 1 d . . . O23 O -0.3303(8) 0.2169(7) 0.3659(8) 0.190(7) Uani 1 1 d . . . O24 O -0.2400(6) 0.3231(7) 0.2903(9) 0.198(8) Uani 1 1 d . . . C124 C -0.2937(12) 0.2738(10) 0.2358(13) 0.142(7) Uani 1 1 d . . . F10 F -0.2315(8) 0.3090(10) 0.1646(7) 0.256(9) Uani 1 1 d . . . F11 F -0.3136(7) 0.2170(9) 0.2375(8) 0.195(6) Uani 1 1 d . . . F12 F -0.3392(7) 0.3167(9) 0.2371(7) 0.246(8) Uani 1 1 d . . . B1 B -0.2635(5) 0.4573(5) 0.0030(5) 0.080(3) Uani 1 1 d DU . . F13 F -0.2383(4) 0.5179(4) -0.0060(4) 0.122(3) Uani 1 1 d DU . . F14 F -0.2954(4) 0.4795(4) -0.0472(4) 0.108(2) Uani 1 1 d DU . . F15 F -0.2080(3) 0.4180(3) -0.0174(3) 0.098(2) Uani 1 1 d DU . . F16 F -0.3143(3) 0.4191(3) 0.0731(3) 0.0719(15) Uani 1 1 d DU . . B2 B -0.0514(6) -0.7498(6) 0.5235(6) 0.111(4) Uani 1 1 d DU . . F17 F 0.0146(5) -0.7619(6) 0.4844(6) 0.309(10) Uani 1 1 d DU . . F18 F -0.0491(7) -0.7195(5) 0.5676(6) 0.194(5) Uani 1 1 d DU . . F19 F -0.0921(4) -0.8126(4) 0.5716(4) 0.111(2) Uani 1 1 d DU . . F20 F -0.0820(4) -0.7054(4) 0.4779(3) 0.106(2) Uani 1 1 d DU . . O1W O -0.2960(3) -0.2755(3) 0.4645(3) 0.0446(13) Uani 1 1 d . . . O2W O -0.2153(3) -0.3804(3) 0.4268(3) 0.0548(14) Uani 1 1 d . . . O3W O 0.2137(3) 0.2085(3) -0.0421(3) 0.0526(15) Uani 1 1 d . . . O4W O -0.2613(3) -1.1404(3) 0.7424(3) 0.0584(15) Uani 1 1 d . . . O5W O -0.3534(3) -1.2399(3) 0.7609(3) 0.0589(15) Uani 1 1 d . . . O6W O -0.1078(3) 0.7036(3) 0.0732(4) 0.0594(16) Uani 1 1 d . . . O7W O 0.2366(4) 0.5829(4) 0.1572(4) 0.0727(18) Uani 1 1 d . . . O8W O -0.3225(4) -0.4763(4) 0.5496(4) 0.080(2) Uani 1 1 d . . . O9W O -0.3021(4) -1.0082(4) 0.6867(5) 0.099(3) Uani 1 1 d . . . O10W O -0.0115(5) 0.8131(6) -0.0509(5) 0.133(4) Uani 1 1 d . . . O11W O 0.3304(5) 0.8611(5) 0.0775(6) 0.115(3) Uani 1 1 d . . . O12W O 0.1060(5) 0.6693(4) -0.0127(6) 0.123(4) Uani 1 1 d . . . O13W O 0.2543(6) 0.5484(5) 0.3540(6) 0.126(4) Uani 1 1 d . . . O14W O 0.3174(5) 0.9076(5) -0.0511(6) 0.113(3) Uani 1 1 d . . . O15W O 0.4163(5) -0.2538(5) 0.0950(6) 0.113(3) Uani 1 1 d . . . O16W O 0.3085(5) 0.6379(6) 0.2038(6) 0.116(3) Uani 1 1 d . . . O17W O -0.2234(6) 0.4048(5) 0.4605(5) 0.136(4) Uani 1 1 d . . . O18W O 0.0989(5) 0.7535(5) 0.0514(5) 0.124(3) Uani 1 1 d . . . O19W O 0.1436(6) 0.6873(6) 0.1626(6) 0.134(4) Uani 1 1 d . . . O20W O -0.3737(6) 0.1275(6) 0.5177(7) 0.152(5) Uani 1 1 d . . . O21W O -0.1696(6) 0.3862(7) 0.5629(8) 0.172(5) Uani 1 1 d . . . O22W O -0.3297(6) 0.2086(6) 0.5638(6) 0.132(4) Uani 1 1 d . . . O23W O -0.2175(12) -0.9504(7) 0.5363(7) 0.262(11) Uani 1 1 d . . . O24W O -0.2867(11) -0.8818(8) 0.6960(10) 0.227(8) Uani 1 1 d . . . O25W O -0.9369(8) -0.2439(15) 0.851(2) 0.47(3) Uani 1 1 d . . . O26W O 0.2111(13) 0.7504(10) 0.2022(12) 0.279(11) Uani 1 1 d . . . O27W O -0.2374(11) -0.9247(8) 0.4138(14) 0.280(12) Uani 1 1 d . . . O28W O 0.2196(13) 0.8522(11) 0.2359(16) 0.308(14) Uani 1 1 d . . . O29W O -0.9115(7) -0.2441(7) 0.6574(7) 0.178(6) Uani 1 1 d . . . O30W O -0.1972(11) 0.3152(14) 0.3987(17) 0.332(16) 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 Pd1 0.0179(2) 0.0210(2) 0.0253(3) -0.00679(19) -0.00591(19) -0.00143(18) O1 0.036(3) 0.047(3) 0.029(3) 0.001(2) -0.009(2) -0.027(2) O2 0.030(2) 0.031(2) 0.033(3) -0.011(2) -0.001(2) -0.013(2) O3 0.056(3) 0.055(3) 0.067(4) -0.043(3) -0.044(3) 0.036(3) O4 0.045(3) 0.053(3) 0.035(3) -0.017(2) -0.013(2) 0.026(3) N1 0.020(3) 0.024(3) 0.023(3) -0.009(2) -0.006(2) -0.001(2) N2 0.033(3) 0.040(3) 0.026(3) -0.009(3) -0.009(2) -0.012(3) N3 0.023(3) 0.024(3) 0.023(3) -0.007(2) -0.006(2) -0.002(2) N4 0.028(3) 0.028(3) 0.022(3) -0.007(2) -0.005(2) -0.008(2) N5 0.023(3) 0.025(3) 0.029(3) -0.010(2) -0.010(2) 0.002(2) N6 0.046(4) 0.044(4) 0.037(3) -0.024(3) -0.028(3) 0.021(3) N7 0.017(2) 0.023(3) 0.025(3) -0.006(2) -0.007(2) -0.001(2) N8 0.036(3) 0.046(4) 0.029(3) -0.020(3) -0.014(3) 0.021(3) C1 0.024(3) 0.028(3) 0.027(3) -0.010(3) -0.010(3) 0.002(3) C2 0.029(3) 0.031(3) 0.024(3) -0.008(3) -0.012(3) -0.003(3) C3 0.028(3) 0.027(3) 0.027(3) -0.012(3) -0.006(3) -0.002(3) C4 0.030(3) 0.034(4) 0.030(3) -0.010(3) -0.012(3) -0.004(3) C5 0.028(3) 0.023(3) 0.027(3) -0.006(3) -0.011(3) -0.001(3) C6 0.026(3) 0.033(4) 0.026(3) -0.011(3) -0.008(3) -0.005(3) C7 0.030(4) 0.032(4) 0.041(4) -0.006(3) -0.014(3) -0.007(3) C8 0.044(4) 0.028(4) 0.038(4) -0.004(3) -0.020(3) -0.004(3) C9 0.031(4) 0.046(4) 0.031(4) -0.014(3) -0.012(3) -0.005(3) C10 0.030(4) 0.034(4) 0.025(3) -0.008(3) -0.006(3) -0.007(3) C11 0.024(3) 0.031(3) 0.027(3) -0.010(3) -0.003(3) -0.002(3) C12 0.025(3) 0.029(3) 0.028(3) -0.010(3) -0.001(3) -0.005(3) C13 0.026(3) 0.029(3) 0.022(3) -0.006(3) -0.008(3) -0.004(3) C14 0.026(3) 0.031(3) 0.028(3) -0.013(3) -0.006(3) 0.000(3) C15 0.024(3) 0.029(3) 0.027(3) -0.012(3) -0.008(3) 0.001(3) C16 0.028(3) 0.030(3) 0.019(3) -0.006(3) -0.007(3) -0.005(3) C17 0.031(4) 0.043(4) 0.029(4) -0.019(3) 0.002(3) -0.004(3) C18 0.030(4) 0.037(4) 0.038(4) -0.023(3) -0.004(3) -0.007(3) C19 0.026(3) 0.037(4) 0.032(4) -0.014(3) 0.002(3) -0.004(3) C20 0.032(4) 0.029(3) 0.030(4) -0.011(3) -0.002(3) -0.001(3) C21 0.032(4) 0.027(3) 0.030(3) -0.012(3) -0.012(3) -0.002(3) C22 0.028(3) 0.031(3) 0.033(4) -0.015(3) -0.014(3) 0.005(3) C23 0.029(3) 0.032(3) 0.028(3) -0.010(3) -0.011(3) 0.005(3) C24 0.043(4) 0.035(4) 0.048(4) -0.023(3) -0.025(4) 0.010(3) C25 0.037(4) 0.034(4) 0.044(4) -0.018(3) -0.022(3) 0.005(3) C26 0.028(3) 0.031(3) 0.032(4) -0.014(3) -0.012(3) 0.008(3) C27 0.038(4) 0.039(4) 0.060(5) -0.026(4) -0.021(4) 0.007(3) C28 0.039(4) 0.050(5) 0.062(5) -0.032(4) -0.029(4) 0.013(4) C29 0.048(4) 0.037(4) 0.035(4) -0.022(3) -0.021(3) 0.010(3) C30 0.037(4) 0.037(4) 0.032(4) -0.014(3) -0.016(3) 0.007(3) C31 0.027(3) 0.030(3) 0.022(3) -0.008(3) -0.004(3) -0.001(3) C32 0.029(3) 0.032(3) 0.023(3) -0.009(3) -0.005(3) 0.002(3) C33 0.027(3) 0.027(3) 0.024(3) -0.010(3) -0.011(3) 0.001(3) C34 0.029(3) 0.024(3) 0.023(3) -0.005(3) -0.008(3) 0.000(3) C35 0.023(3) 0.025(3) 0.024(3) -0.008(3) -0.003(3) -0.004(2) C36 0.031(4) 0.036(4) 0.023(3) -0.013(3) -0.010(3) 0.005(3) C37 0.028(4) 0.044(4) 0.029(3) -0.016(3) -0.010(3) 0.006(3) C38 0.029(4) 0.044(4) 0.031(4) -0.017(3) -0.010(3) 0.008(3) C39 0.045(4) 0.036(4) 0.039(4) -0.013(3) -0.008(4) 0.012(3) C40 0.027(4) 0.042(4) 0.035(4) -0.015(3) -0.005(3) 0.003(3) Pd2 0.0203(2) 0.0225(2) 0.0249(3) -0.0079(2) -0.0053(2) -0.00251(18) O5 0.037(3) 0.028(3) 0.075(4) -0.015(3) -0.027(3) -0.008(2) O6 0.031(3) 0.039(3) 0.069(4) -0.027(3) -0.007(3) -0.012(2) O7 0.093(5) 0.096(5) 0.091(5) -0.073(4) -0.067(4) 0.070(4) O8 0.029(2) 0.033(3) 0.033(3) -0.012(2) -0.009(2) 0.008(2) N9 0.022(3) 0.027(3) 0.025(3) -0.008(2) -0.006(2) -0.002(2) N10 0.033(3) 0.024(3) 0.048(4) -0.013(3) -0.018(3) -0.004(2) N11 0.023(3) 0.025(3) 0.027(3) -0.011(2) -0.008(2) 0.000(2) N12 0.024(3) 0.037(3) 0.050(4) -0.020(3) -0.011(3) -0.003(2) N13 0.026(3) 0.023(3) 0.026(3) -0.009(2) -0.007(2) -0.003(2) N14 0.061(5) 0.076(5) 0.049(4) -0.042(4) -0.037(4) 0.038(4) N15 0.024(3) 0.024(3) 0.024(3) -0.005(2) -0.007(2) -0.005(2) N16 0.026(3) 0.027(3) 0.029(3) -0.010(2) -0.010(2) 0.003(2) C41 0.042(4) 0.034(4) 0.033(4) -0.006(3) -0.019(3) -0.009(3) C42 0.048(4) 0.029(4) 0.034(4) 0.001(3) -0.022(3) -0.012(3) C43 0.021(3) 0.031(3) 0.035(4) -0.014(3) -0.011(3) -0.001(3) C44 0.024(3) 0.031(3) 0.035(4) -0.012(3) -0.013(3) 0.003(3) C45 0.028(3) 0.030(3) 0.031(3) -0.011(3) -0.013(3) 0.004(3) C46 0.029(3) 0.033(4) 0.036(4) -0.016(3) -0.014(3) 0.003(3) C47 0.034(4) 0.032(4) 0.044(4) -0.012(3) -0.021(3) 0.000(3) C48 0.034(4) 0.026(3) 0.053(4) -0.009(3) -0.024(3) 0.001(3) C49 0.027(4) 0.039(4) 0.064(5) -0.017(4) -0.026(4) 0.002(3) C50 0.037(4) 0.032(4) 0.055(5) -0.012(3) -0.028(4) 0.005(3) C51 0.022(3) 0.030(3) 0.026(3) -0.012(3) -0.003(3) -0.002(3) C52 0.026(3) 0.032(3) 0.029(3) -0.019(3) -0.005(3) 0.002(3) C53 0.027(3) 0.028(3) 0.024(3) -0.010(3) -0.008(3) 0.001(3) C54 0.027(3) 0.044(4) 0.033(4) -0.021(3) 0.000(3) -0.004(3) C55 0.031(4) 0.038(4) 0.032(4) -0.019(3) -0.004(3) -0.003(3) C56 0.034(4) 0.027(3) 0.033(4) -0.012(3) -0.012(3) -0.003(3) C57 0.029(4) 0.043(4) 0.059(5) -0.031(4) -0.007(3) -0.002(3) C58 0.032(4) 0.033(4) 0.064(5) -0.028(4) -0.008(4) -0.003(3) C59 0.024(3) 0.032(4) 0.045(4) -0.020(3) -0.004(3) -0.002(3) C60 0.026(3) 0.033(4) 0.040(4) -0.021(3) -0.005(3) -0.002(3) C61 0.034(4) 0.031(3) 0.036(4) -0.017(3) -0.016(3) -0.002(3) C62 0.039(4) 0.036(4) 0.039(4) -0.019(3) -0.022(3) 0.005(3) C63 0.032(4) 0.027(3) 0.034(4) -0.011(3) -0.015(3) 0.001(3) C64 0.033(4) 0.033(4) 0.039(4) -0.021(3) -0.012(3) 0.002(3) C65 0.033(4) 0.034(4) 0.033(4) -0.016(3) -0.014(3) -0.001(3) C66 0.042(4) 0.045(4) 0.028(3) -0.016(3) -0.020(3) 0.003(3) C67 0.045(5) 0.055(5) 0.051(5) -0.025(4) -0.021(4) 0.007(4) C68 0.053(5) 0.064(6) 0.068(6) -0.037(5) -0.032(5) 0.024(4) C69 0.081(7) 0.038(4) 0.044(5) -0.020(4) -0.034(5) 0.013(4) C70 0.057(5) 0.036(4) 0.043(4) -0.021(3) -0.026(4) 0.014(4) C71 0.024(3) 0.027(3) 0.022(3) -0.006(3) -0.003(3) -0.002(3) C72 0.026(3) 0.034(4) 0.023(3) -0.008(3) -0.004(3) -0.003(3) C73 0.020(3) 0.032(3) 0.025(3) -0.013(3) -0.008(3) 0.000(3) C74 0.030(3) 0.028(3) 0.021(3) -0.005(3) -0.007(3) 0.001(3) C75 0.025(3) 0.035(4) 0.020(3) -0.009(3) -0.003(3) -0.003(3) C76 0.026(3) 0.031(3) 0.023(3) -0.009(3) -0.010(3) -0.003(3) C77 0.028(3) 0.030(3) 0.025(3) -0.004(3) -0.006(3) -0.003(3) C78 0.026(3) 0.034(4) 0.028(3) -0.011(3) -0.005(3) -0.001(3) C79 0.035(4) 0.027(3) 0.027(3) -0.005(3) -0.008(3) -0.001(3) C80 0.018(3) 0.035(4) 0.028(3) -0.008(3) -0.003(3) 0.002(3) Pd3 0.0185(2) 0.0194(2) 0.0244(3) -0.00701(19) -0.00508(19) -0.00205(18) O9 0.027(2) 0.030(2) 0.037(3) -0.005(2) -0.009(2) -0.0124(19) O10 0.036(3) 0.036(3) 0.027(2) -0.011(2) 0.004(2) -0.022(2) O11 0.049(3) 0.045(3) 0.036(3) -0.018(2) -0.016(2) 0.026(3) O12 0.045(3) 0.051(3) 0.056(3) -0.036(3) -0.032(3) 0.026(3) N17 0.022(3) 0.024(3) 0.024(3) -0.009(2) -0.005(2) -0.002(2) N18 0.024(3) 0.030(3) 0.026(3) -0.009(2) -0.005(2) -0.007(2) N19 0.021(3) 0.022(3) 0.024(3) -0.010(2) -0.009(2) 0.002(2) N20 0.031(3) 0.030(3) 0.020(3) -0.007(2) -0.002(2) -0.009(2) N21 0.018(2) 0.023(3) 0.025(3) -0.010(2) -0.005(2) -0.002(2) N22 0.036(3) 0.040(3) 0.030(3) -0.017(3) -0.014(3) 0.014(3) N23 0.022(3) 0.025(3) 0.024(3) -0.010(2) -0.003(2) -0.002(2) N24 0.037(3) 0.039(3) 0.033(3) -0.022(3) -0.017(3) 0.013(3) C81 0.026(3) 0.031(3) 0.029(3) -0.010(3) -0.011(3) 0.000(3) C82 0.027(3) 0.025(3) 0.025(3) -0.007(3) -0.008(3) -0.002(3) C83 0.021(3) 0.029(3) 0.025(3) -0.013(3) -0.003(3) -0.001(3) C84 0.023(3) 0.028(3) 0.028(3) -0.007(3) -0.008(3) -0.001(3) C85 0.028(3) 0.025(3) 0.025(3) -0.007(3) -0.010(3) 0.001(3) C86 0.021(3) 0.027(3) 0.024(3) -0.008(3) -0.005(3) -0.006(2) C87 0.029(4) 0.029(4) 0.036(4) -0.003(3) -0.015(3) -0.003(3) C88 0.037(4) 0.027(3) 0.036(4) -0.003(3) -0.016(3) -0.005(3) C89 0.027(3) 0.033(4) 0.036(4) -0.009(3) -0.013(3) -0.004(3) C90 0.031(4) 0.025(3) 0.035(4) -0.006(3) -0.014(3) -0.001(3) C91 0.021(3) 0.031(3) 0.022(3) -0.011(3) -0.004(3) -0.002(3) C92 0.023(3) 0.029(3) 0.032(3) -0.017(3) -0.006(3) -0.004(3) C93 0.023(3) 0.024(3) 0.024(3) -0.009(3) -0.007(3) -0.001(2) C94 0.026(3) 0.032(3) 0.023(3) -0.013(3) -0.004(3) 0.002(3) C95 0.028(3) 0.025(3) 0.034(4) -0.016(3) -0.011(3) 0.003(3) C96 0.030(3) 0.028(3) 0.024(3) -0.010(3) -0.011(3) -0.002(3) C97 0.024(3) 0.032(4) 0.030(3) -0.013(3) -0.006(3) -0.002(3) C98 0.035(4) 0.025(3) 0.026(3) -0.012(3) -0.006(3) -0.001(3) C99 0.026(3) 0.035(4) 0.036(4) -0.015(3) 0.000(3) -0.004(3) C100 0.029(4) 0.032(4) 0.040(4) -0.018(3) -0.003(3) -0.003(3) C101 0.023(3) 0.026(3) 0.024(3) -0.006(3) -0.008(3) -0.002(2) C102 0.023(3) 0.033(3) 0.025(3) -0.010(3) -0.004(3) -0.002(3) C103 0.024(3) 0.029(3) 0.028(3) -0.013(3) -0.008(3) -0.002(3) C104 0.030(3) 0.026(3) 0.022(3) -0.004(3) -0.007(3) -0.003(3) C105 0.027(3) 0.022(3) 0.025(3) -0.008(3) -0.007(3) -0.002(2) C106 0.031(4) 0.030(3) 0.024(3) -0.009(3) -0.012(3) 0.004(3) C107 0.035(4) 0.034(4) 0.038(4) -0.009(3) -0.010(3) 0.004(3) C108 0.034(4) 0.038(4) 0.035(4) -0.003(3) -0.006(3) 0.005(3) C109 0.044(4) 0.030(4) 0.031(4) -0.012(3) -0.013(3) 0.006(3) C110 0.033(4) 0.033(4) 0.035(4) -0.017(3) -0.013(3) 0.005(3) C111 0.030(3) 0.030(3) 0.035(4) -0.014(3) -0.013(3) -0.001(3) C112 0.026(3) 0.033(4) 0.035(4) -0.018(3) -0.014(3) 0.006(3) C113 0.028(3) 0.027(3) 0.024(3) -0.008(3) -0.009(3) 0.002(3) C114 0.032(3) 0.025(3) 0.032(3) -0.014(3) -0.013(3) 0.002(3) C115 0.021(3) 0.031(3) 0.030(3) -0.011(3) -0.009(3) -0.001(3) C116 0.034(4) 0.027(3) 0.030(3) -0.012(3) -0.012(3) 0.006(3) C117 0.036(4) 0.036(4) 0.051(4) -0.020(3) -0.025(4) 0.008(3) C118 0.042(4) 0.033(4) 0.045(4) -0.017(3) -0.022(3) 0.006(3) C119 0.033(4) 0.042(4) 0.032(4) -0.017(3) -0.016(3) 0.001(3) C120 0.031(4) 0.035(4) 0.027(3) -0.016(3) -0.009(3) 0.003(3) S1 0.0674(15) 0.0482(13) 0.0606(14) -0.0208(11) -0.0220(12) 0.0030(11) O13 0.167(11) 0.130(9) 0.102(8) 0.013(6) -0.045(7) -0.068(8) O14 0.226(13) 0.169(10) 0.143(9) -0.116(9) -0.120(10) 0.136(10) O15 0.254(13) 0.081(6) 0.116(7) -0.061(6) -0.119(9) 0.061(7) C121 0.127(11) 0.061(7) 0.064(7) -0.020(6) -0.023(7) -0.021(7) F1 0.39(2) 0.44(2) 0.283(17) -0.272(18) -0.290(18) 0.36(2) F2 0.199(12) 0.183(11) 0.109(8) -0.007(7) -0.041(8) -0.064(9) F3 0.173(9) 0.223(11) 0.197(10) -0.149(10) -0.128(9) 0.070(8) S2 0.0614(15) 0.0639(15) 0.0585(14) -0.0218(12) -0.0187(12) 0.0164(12) O16 0.310(18) 0.067(6) 0.134(9) -0.033(6) -0.107(11) 0.030(9) O17 0.128(8) 0.234(12) 0.100(7) -0.100(8) -0.079(6) 0.110(9) O18 0.078(6) 0.161(10) 0.139(9) -0.080(8) -0.014(6) 0.036(6) C122 0.065(7) 0.099(9) 0.067(7) -0.023(7) -0.022(6) 0.002(6) F4 0.160(9) 0.245(12) 0.151(8) -0.138(9) -0.100(7) 0.094(9) F5 0.067(5) 0.201(9) 0.114(6) -0.097(6) 0.003(4) -0.008(5) F6 0.154(8) 0.108(7) 0.140(8) -0.071(6) -0.009(6) 0.004(6) S3 0.0572(16) 0.0722(18) 0.112(2) -0.0318(17) -0.0328(16) 0.0010(13) O19 0.261(19) 0.47(3) 0.152(11) -0.087(16) 0.032(12) 0.24(2) O20 0.34(2) 0.261(17) 0.288(16) -0.148(15) -0.252(17) 0.204(17) O21 0.089(7) 0.060(5) 0.342(18) -0.033(8) -0.068(9) 0.011(5) C123 0.180(18) 0.218(16) 0.28(2) -0.186(18) -0.154(15) 0.092(15) F7 0.307(19) 0.259(15) 0.210(13) -0.152(13) -0.108(13) 0.068(14) F8 0.321(19) 0.244(16) 0.41(2) -0.211(16) -0.239(19) 0.164(15) F9 0.111(7) 0.239(11) 0.199(10) -0.115(9) -0.091(7) 0.006(7) S4 0.143(4) 0.165(4) 0.202(5) -0.144(4) -0.109(4) 0.083(4) O22 0.236(16) 0.264(17) 0.239(16) -0.187(15) -0.170(14) 0.175(14) O23 0.173(12) 0.139(10) 0.150(11) -0.070(9) 0.045(9) -0.050(9) O24 0.108(8) 0.203(13) 0.276(16) -0.206(13) 0.047(9) -0.047(8) C124 0.146(17) 0.117(14) 0.19(2) -0.073(14) -0.103(17) 0.071(13) F10 0.206(13) 0.34(2) 0.101(8) -0.073(11) 0.003(9) 0.036(14) F11 0.192(12) 0.253(15) 0.212(13) -0.159(13) -0.087(10) 0.018(11) F12 0.196(12) 0.288(17) 0.193(12) -0.072(12) -0.105(10) 0.163(13) B1 0.063(7) 0.072(7) 0.073(7) -0.030(6) -0.005(5) 0.006(5) F13 0.129(6) 0.105(5) 0.111(6) -0.061(5) -0.007(5) -0.036(5) F14 0.093(5) 0.128(6) 0.072(4) -0.029(4) -0.026(4) 0.011(4) F15 0.093(4) 0.097(4) 0.057(3) -0.026(3) -0.009(3) 0.042(4) F16 0.065(3) 0.083(4) 0.048(3) -0.028(3) -0.004(2) -0.012(3) B2 0.089(9) 0.098(10) 0.072(9) 0.009(6) -0.021(6) 0.008(7) F17 0.145(8) 0.248(13) 0.162(10) 0.067(8) 0.054(7) 0.117(8) F18 0.275(13) 0.114(7) 0.215(11) -0.007(7) -0.179(10) -0.035(8) F19 0.131(6) 0.090(5) 0.087(5) -0.011(4) -0.050(4) -0.007(4) F20 0.095(5) 0.103(5) 0.069(4) -0.011(3) -0.027(4) 0.032(4) O1W 0.030(3) 0.041(3) 0.038(3) -0.004(2) -0.004(2) -0.009(2) O2W 0.056(4) 0.054(3) 0.054(3) -0.022(3) -0.022(3) -0.006(3) O3W 0.038(3) 0.034(3) 0.049(3) -0.008(2) 0.002(2) -0.003(2) O4W 0.045(3) 0.065(4) 0.058(4) -0.031(3) -0.016(3) 0.019(3) O5W 0.065(4) 0.049(3) 0.056(4) -0.018(3) -0.028(3) 0.016(3) O6W 0.063(4) 0.052(3) 0.074(4) -0.024(3) -0.040(3) 0.001(3) O7W 0.074(5) 0.068(4) 0.065(4) -0.023(3) -0.026(4) 0.000(4) O8W 0.077(5) 0.077(5) 0.069(5) -0.038(4) -0.007(4) -0.004(4) O9W 0.079(5) 0.071(5) 0.086(5) -0.011(4) -0.013(4) 0.024(4) O10W 0.105(7) 0.134(8) 0.106(7) 0.017(6) -0.065(6) -0.023(6) O11W 0.118(7) 0.100(6) 0.196(10) -0.089(7) -0.112(8) 0.050(6) O12W 0.094(6) 0.062(5) 0.155(9) -0.009(5) -0.042(6) -0.001(4) O13W 0.149(9) 0.089(6) 0.163(10) -0.031(6) -0.102(8) -0.022(6) O14W 0.107(7) 0.115(7) 0.123(8) -0.054(6) -0.052(6) 0.005(6) O15W 0.128(8) 0.104(7) 0.169(9) -0.080(7) -0.105(7) 0.044(6) O16W 0.098(7) 0.152(9) 0.121(8) -0.078(7) -0.045(6) 0.005(6) O17W 0.154(10) 0.099(7) 0.091(7) -0.027(6) -0.007(6) -0.016(7) O18W 0.110(7) 0.109(7) 0.100(7) -0.028(6) -0.025(6) 0.028(6) O19W 0.116(8) 0.115(8) 0.129(8) -0.037(7) -0.043(7) 0.036(6) O20W 0.092(7) 0.131(9) 0.198(12) -0.097(9) -0.001(7) -0.012(6) O21W 0.108(9) 0.157(11) 0.208(14) -0.092(10) -0.012(9) -0.015(8) O22W 0.124(8) 0.124(8) 0.148(9) -0.078(8) -0.037(7) 0.004(7) O23W 0.40(3) 0.130(11) 0.095(9) -0.048(8) 0.015(12) 0.055(14) O24W 0.32(2) 0.170(13) 0.223(17) -0.084(13) -0.125(17) -0.043(14) O25W 0.117(11) 0.57(4) 0.96(7) -0.69(5) -0.04(2) -0.024(18) O26W 0.43(3) 0.248(19) 0.31(2) -0.170(18) -0.29(2) 0.21(2) O27W 0.32(2) 0.133(11) 0.54(4) -0.101(16) -0.35(3) 0.025(13) O28W 0.34(3) 0.26(2) 0.57(4) -0.28(3) -0.34(3) 0.20(2) O29W 0.145(10) 0.165(11) 0.122(9) -0.036(8) -0.005(8) 0.033(9) O30W 0.25(2) 0.46(3) 0.63(5) -0.46(4) -0.29(3) 0.21(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.012(5) . ? Pd1 N3 2.026(5) . ? Pd1 N7 2.028(5) . ? Pd1 N5 2.028(5) . ? O1 N2 1.303(7) . ? O2 N4 1.297(7) . ? O3 N6 1.294(7) . ? O4 N8 1.307(7) . ? N1 C1 1.334(8) . ? N1 C5 1.346(8) . ? N2 C8 1.354(9) . ? N2 C9 1.365(9) . ? N3 C11 1.338(8) . ? N3 C15 1.354(8) . ? N4 C19 1.341(9) . ? N4 C18 1.350(8) . ? N5 C21 1.324(8) . ? N5 C25 1.350(8) . ? N6 C29 1.351(9) . ? N6 C28 1.365(10) . ? N7 C31 1.328(8) . ? N7 C35 1.332(8) . ? N8 C39 1.343(9) . ? N8 C38 1.358(9) . ? C1 C2 1.374(9) . ? C2 C3 1.412(9) . ? C3 C4 1.384(9) . ? C3 C6 1.464(9) . ? C4 C5 1.376(9) . ? C6 C7 1.389(9) . ? C6 C10 1.408(9) . ? C7 C8 1.348(9) . ? C9 C10 1.347(9) . ? C11 C12 1.366(9) . ? C12 C13 1.407(9) . ? C13 C14 1.407(9) . ? C13 C16 1.469(9) . ? C14 C15 1.366(9) . ? C16 C20 1.382(9) . ? C16 C17 1.392(9) . ? C17 C18 1.362(9) . ? C19 C20 1.375(9) . ? C21 C22 1.375(9) . ? C22 C23 1.395(9) . ? C23 C24 1.395(10) . ? C23 C26 1.479(9) . ? C24 C25 1.359(10) . ? C26 C30 1.370(10) . ? C26 C27 1.386(10) . ? C27 C28 1.355(10) . ? C29 C30 1.381(10) . ? C31 C32 1.381(9) . ? C32 C33 1.393(9) . ? C33 C34 1.388(9) . ? C33 C36 1.478(9) . ? C34 C35 1.381(9) . ? C36 C37 1.385(9) . ? C36 C40 1.396(10) . ? C37 C38 1.375(10) . ? C39 C40 1.360(10) . ? Pd2 N13 2.018(5) . ? Pd2 N9 2.024(5) . ? Pd2 N15 2.027(5) . ? Pd2 N11 2.033(5) . ? O5 N10 1.305(7) . ? O6 N12 1.321(7) . ? O7 N14 1.318(8) . ? O8 N16 1.290(7) . ? N9 C45 1.328(8) . ? N9 C41 1.343(8) . ? N10 C49 1.340(9) . ? N10 C48 1.354(9) . ? N11 C55 1.337(8) . ? N11 C51 1.340(8) . ? N12 C59 1.331(9) . ? N12 C58 1.358(9) . ? N13 C61 1.331(8) . ? N13 C65 1.349(8) . ? N14 C68 1.345(12) . ? N14 C69 1.354(12) . ? N15 C75 1.335(8) . ? N15 C71 1.347(8) . ? N16 C79 1.351(8) . ? N16 C78 1.366(8) . ? C41 C42 1.356(9) . ? C42 C43 1.387(9) . ? C43 C44 1.396(9) . ? C43 C46 1.469(9) . ? C44 C45 1.385(9) . ? C46 C47 1.387(10) . ? C46 C50 1.396(9) . ? C47 C48 1.367(9) . ? C49 C50 1.356(10) . ? C51 C52 1.380(9) . ? C52 C53 1.409(9) . ? C53 C54 1.373(9) . ? C53 C56 1.466(9) . ? C54 C55 1.368(9) . ? C56 C57 1.383(10) . ? C56 C60 1.388(9) . ? C57 C58 1.375(10) . ? C59 C60 1.359(9) . ? C61 C62 1.366(10) . ? C62 C63 1.399(9) . ? C63 C64 1.381(9) . ? C63 C66 1.475(10) . ? C64 C65 1.378(9) . ? C66 C70 1.381(10) . ? C66 C67 1.398(11) . ? C67 C68 1.354(12) . ? C69 C70 1.374(11) . ? C71 C72 1.374(9) . ? C72 C73 1.387(9) . ? C73 C74 1.400(9) . ? C73 C76 1.485(9) . ? C74 C75 1.359(9) . ? C76 C80 1.384(9) . ? C76 C77 1.403(9) . ? C77 C78 1.361(9) . ? C79 C80 1.359(9) . ? Pd3 N19 2.018(5) . ? Pd3 N21 2.025(5) . ? Pd3 N23 2.034(5) . ? Pd3 N17 2.036(5) . ? O9 N18 1.303(7) . ? O10 N20 1.299(7) . ? O11 N22 1.298(7) . ? O12 N24 1.296(7) . ? N17 C81 1.338(8) . ? N17 C85 1.345(8) . ? N18 C88 1.342(9) . ? N18 C89 1.354(9) . ? N19 C91 1.327(8) . ? N19 C95 1.338(8) . ? N20 C98 1.342(8) . ? N20 C99 1.344(9) . ? N21 C101 1.332(8) . ? N21 C105 1.334(8) . ? N22 C109 1.354(9) . ? N22 C108 1.362(9) . ? N23 C111 1.339(8) . ? N23 C115 1.343(8) . ? N24 C118 1.352(9) . ? N24 C119 1.357(9) . ? C81 C82 1.366(9) . ? C82 C83 1.389(9) . ? C83 C84 1.392(9) . ? C83 C86 1.480(8) . ? C84 C85 1.359(9) . ? C86 C87 1.396(9) . ? C86 C90 1.402(9) . ? C87 C88 1.364(9) . ? C89 C90 1.363(9) . ? C91 C92 1.388(8) . ? C92 C93 1.390(9) . ? C93 C94 1.403(9) . ? C93 C96 1.459(8) . ? C94 C95 1.367(9) . ? C96 C100 1.378(9) . ? C96 C97 1.404(9) . ? C97 C98 1.381(9) . ? C99 C100 1.370(9) . ? C101 C102 1.377(9) . ? C102 C103 1.400(9) . ? C103 C104 1.393(9) . ? C103 C106 1.474(9) . ? C104 C105 1.373(9) . ? C106 C107 1.392(10) . ? C106 C110 1.392(9) . ? C107 C108 1.347(10) . ? C109 C110 1.380(10) . ? C111 C112 1.377(9) . ? C112 C113 1.393(9) . ? C113 C114 1.404(9) . ? C113 C116 1.467(9) . ? C114 C115 1.367(9) . ? C116 C117 1.390(10) . ? C116 C120 1.410(9) . ? C117 C118 1.369(10) . ? C119 C120 1.357(10) . ? S1 O15 1.368(9) . ? S1 O14 1.378(9) . ? S1 O13 1.435(10) . ? S1 C121 1.740(14) . ? C121 F1 1.225(16) . ? C121 F3 1.318(14) . ? C121 F2 1.341(15) . ? S2 O16 1.363(10) . ? S2 O17 1.375(9) . ? S2 O18 1.425(11) . ? S2 C122 1.783(14) . ? C122 F4 1.302(14) . ? C122 F6 1.330(14) . ? C122 F5 1.331(13) . ? S3 O20 1.286(13) . ? S3 O19 1.405(13) . ? S3 O21 1.406(10) . ? S3 C123 1.79(2) . ? C123 F9 1.326(14) . ? C123 F8 1.350(15) . ? C123 F7 1.371(16) . ? S4 O24 1.422(11) . ? S4 O22 1.424(12) . ? S4 O23 1.567(12) . ? S4 C124 1.72(2) . ? C124 F12 1.227(18) . ? C124 F11 1.31(2) . ? C124 F10 1.46(2) . ? B1 F13 1.350(10) . ? B1 F16 1.366(10) . ? B1 F15 1.369(10) . ? B1 F14 1.414(11) . ? B2 F17 1.331(11) . ? B2 F19 1.362(11) . ? B2 F20 1.369(11) . ? B2 F18 1.420(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N3 178.9(2) . . ? N1 Pd1 N7 88.5(2) . . ? N3 Pd1 N7 90.4(2) . . ? N1 Pd1 N5 90.6(2) . . ? N3 Pd1 N5 90.4(2) . . ? N7 Pd1 N5 178.8(2) . . ? C1 N1 C5 119.1(5) . . ? C1 N1 Pd1 120.8(4) . . ? C5 N1 Pd1 120.1(4) . . ? O1 N2 C8 120.3(6) . . ? O1 N2 C9 121.4(6) . . ? C8 N2 C9 118.3(6) . . ? C11 N3 C15 117.2(5) . . ? C11 N3 Pd1 120.3(4) . . ? C15 N3 Pd1 122.4(4) . . ? O2 N4 C19 120.6(5) . . ? O2 N4 C18 120.2(5) . . ? C19 N4 C18 119.3(5) . . ? C21 N5 C25 118.5(6) . . ? C21 N5 Pd1 120.9(4) . . ? C25 N5 Pd1 120.6(4) . . ? O3 N6 C29 120.6(6) . . ? O3 N6 C28 120.9(6) . . ? C29 N6 C28 118.5(6) . . ? C31 N7 C35 119.1(5) . . ? C31 N7 Pd1 120.1(4) . . ? C35 N7 Pd1 120.8(4) . . ? O4 N8 C39 118.9(6) . . ? O4 N8 C38 121.5(6) . . ? C39 N8 C38 119.7(6) . . ? N1 C1 C2 122.3(6) . . ? C1 C2 C3 119.6(6) . . ? C4 C3 C2 116.9(6) . . ? C4 C3 C6 122.3(6) . . ? C2 C3 C6 120.8(6) . . ? C5 C4 C3 120.5(6) . . ? N1 C5 C4 121.7(6) . . ? C7 C6 C10 116.2(6) . . ? C7 C6 C3 122.3(6) . . ? C10 C6 C3 121.5(6) . . ? C8 C7 C6 121.6(7) . . ? C7 C8 N2 121.4(6) . . ? C10 C9 N2 121.8(6) . . ? C9 C10 C6 120.5(6) . . ? N3 C11 C12 123.2(6) . . ? C11 C12 C13 120.4(6) . . ? C12 C13 C14 115.8(6) . . ? C12 C13 C16 122.0(6) . . ? C14 C13 C16 122.1(6) . . ? C15 C14 C13 120.1(6) . . ? N3 C15 C14 123.2(6) . . ? C20 C16 C17 116.1(6) . . ? C20 C16 C13 122.6(6) . . ? C17 C16 C13 121.3(6) . . ? C18 C17 C16 121.9(6) . . ? N4 C18 C17 120.5(6) . . ? N4 C19 C20 121.6(6) . . ? C19 C20 C16 120.7(6) . . ? N5 C21 C22 121.8(6) . . ? C21 C22 C23 120.8(6) . . ? C22 C23 C24 116.1(6) . . ? C22 C23 C26 122.3(6) . . ? C24 C23 C26 121.6(6) . . ? C25 C24 C23 120.2(6) . . ? N5 C25 C24 122.6(6) . . ? C30 C26 C27 117.6(6) . . ? C30 C26 C23 121.3(6) . . ? C27 C26 C23 121.2(6) . . ? C28 C27 C26 120.7(7) . . ? C27 C28 N6 121.5(7) . . ? N6 C29 C30 120.8(7) . . ? C26 C30 C29 120.9(7) . . ? N7 C31 C32 122.6(6) . . ? C31 C32 C33 118.9(6) . . ? C34 C33 C32 117.8(6) . . ? C34 C33 C36 121.5(5) . . ? C32 C33 C36 120.7(6) . . ? C35 C34 C33 119.6(6) . . ? N7 C35 C34 121.9(6) . . ? C37 C36 C40 117.8(6) . . ? C37 C36 C33 121.4(6) . . ? C40 C36 C33 120.8(6) . . ? C38 C37 C36 120.1(7) . . ? N8 C38 C37 120.8(6) . . ? N8 C39 C40 121.5(7) . . ? C39 C40 C36 120.2(7) . . ? N13 Pd2 N9 88.9(2) . . ? N13 Pd2 N15 179.4(2) . . ? N9 Pd2 N15 91.2(2) . . ? N13 Pd2 N11 89.4(2) . . ? N9 Pd2 N11 178.3(2) . . ? N15 Pd2 N11 90.4(2) . . ? C45 N9 C41 118.8(6) . . ? C45 N9 Pd2 120.4(4) . . ? C41 N9 Pd2 120.7(4) . . ? O5 N10 C49 120.0(6) . . ? O5 N10 C48 120.0(6) . . ? C49 N10 C48 120.0(6) . . ? C55 N11 C51 118.1(5) . . ? C55 N11 Pd2 121.0(4) . . ? C51 N11 Pd2 120.8(4) . . ? O6 N12 C59 121.8(6) . . ? O6 N12 C58 118.4(6) . . ? C59 N12 C58 119.7(6) . . ? C61 N13 C65 119.7(6) . . ? C61 N13 Pd2 120.2(4) . . ? C65 N13 Pd2 120.0(4) . . ? O7 N14 C68 121.1(8) . . ? O7 N14 C69 118.1(8) . . ? C68 N14 C69 120.8(7) . . ? C75 N15 C71 117.4(5) . . ? C75 N15 Pd2 121.4(4) . . ? C71 N15 Pd2 121.2(4) . . ? O8 N16 C79 120.8(5) . . ? O8 N16 C78 120.6(5) . . ? C79 N16 C78 118.6(5) . . ? N9 C41 C42 121.7(6) . . ? C41 C42 C43 121.2(6) . . ? C42 C43 C44 116.5(6) . . ? C42 C43 C46 121.8(6) . . ? C44 C43 C46 121.7(6) . . ? C45 C44 C43 119.4(6) . . ? N9 C45 C44 122.3(6) . . ? C47 C46 C50 116.2(6) . . ? C47 C46 C43 122.0(6) . . ? C50 C46 C43 121.8(6) . . ? C48 C47 C46 121.2(6) . . ? N10 C48 C47 120.4(6) . . ? N10 C49 C50 120.9(6) . . ? C49 C50 C46 121.3(7) . . ? N11 C51 C52 121.8(6) . . ? C51 C52 C53 120.2(6) . . ? C54 C53 C52 116.2(6) . . ? C54 C53 C56 121.7(6) . . ? C52 C53 C56 122.1(6) . . ? C55 C54 C53 120.8(6) . . ? N11 C55 C54 122.8(6) . . ? C57 C56 C60 117.3(6) . . ? C57 C56 C53 120.9(6) . . ? C60 C56 C53 121.8(6) . . ? C58 C57 C56 120.8(7) . . ? N12 C58 C57 119.9(7) . . ? N12 C59 C60 122.0(6) . . ? C59 C60 C56 120.1(6) . . ? N13 C61 C62 121.7(6) . . ? C61 C62 C63 119.8(6) . . ? C64 C63 C62 117.7(6) . . ? C64 C63 C66 121.2(6) . . ? C62 C63 C66 121.1(6) . . ? C65 C64 C63 119.9(6) . . ? N13 C65 C64 121.1(6) . . ? C70 C66 C67 117.7(7) . . ? C70 C66 C63 122.0(7) . . ? C67 C66 C63 120.4(7) . . ? C68 C67 C66 121.3(8) . . ? N14 C68 C67 119.8(9) . . ? N14 C69 C70 120.7(8) . . ? C69 C70 C66 119.7(8) . . ? N15 C71 C72 122.1(6) . . ? C71 C72 C73 120.8(6) . . ? C72 C73 C74 116.0(6) . . ? C72 C73 C76 122.3(6) . . ? C74 C73 C76 121.7(6) . . ? C75 C74 C73 120.1(6) . . ? N15 C75 C74 123.5(6) . . ? C80 C76 C77 116.3(6) . . ? C80 C76 C73 122.5(6) . . ? C77 C76 C73 121.2(6) . . ? C78 C77 C76 120.3(6) . . ? C77 C78 N16 121.8(6) . . ? N16 C79 C80 121.0(6) . . ? C79 C80 C76 122.0(6) . . ? N19 Pd3 N21 88.28(19) . . ? N19 Pd3 N23 90.59(19) . . ? N21 Pd3 N23 178.86(18) . . ? N19 Pd3 N17 178.3(2) . . ? N21 Pd3 N17 90.06(19) . . ? N23 Pd3 N17 91.1(2) . . ? C81 N17 C85 117.5(5) . . ? C81 N17 Pd3 122.6(4) . . ? C85 N17 Pd3 120.0(4) . . ? O9 N18 C88 120.0(5) . . ? O9 N18 C89 120.6(5) . . ? C88 N18 C89 119.5(5) . . ? C91 N19 C95 119.2(5) . . ? C91 N19 Pd3 119.7(4) . . ? C95 N19 Pd3 121.1(4) . . ? O10 N20 C98 120.6(5) . . ? O10 N20 C99 120.2(5) . . ? C98 N20 C99 119.2(5) . . ? C101 N21 C105 119.4(5) . . ? C101 N21 Pd3 120.5(4) . . ? C105 N21 Pd3 120.1(4) . . ? O11 N22 C109 120.5(6) . . ? O11 N22 C108 119.7(6) . . ? C109 N22 C108 119.7(6) . . ? C111 N23 C115 118.8(5) . . ? C111 N23 Pd3 121.3(4) . . ? C115 N23 Pd3 119.9(4) . . ? O12 N24 C118 119.9(6) . . ? O12 N24 C119 121.5(6) . . ? C118 N24 C119 118.5(6) . . ? N17 C81 C82 122.7(6) . . ? C81 C82 C83 120.4(6) . . ? C82 C83 C84 116.2(6) . . ? C82 C83 C86 122.5(6) . . ? C84 C83 C86 121.3(6) . . ? C85 C84 C83 120.6(6) . . ? N17 C85 C84 122.6(6) . . ? C87 C86 C90 115.1(6) . . ? C87 C86 C83 122.2(6) . . ? C90 C86 C83 122.6(6) . . ? C88 C87 C86 121.7(6) . . ? N18 C88 C87 121.2(6) . . ? N18 C89 C90 120.7(6) . . ? C89 C90 C86 121.8(6) . . ? N19 C91 C92 121.7(6) . . ? C91 C92 C93 120.2(6) . . ? C92 C93 C94 116.6(5) . . ? C92 C93 C96 121.5(5) . . ? C94 C93 C96 121.8(5) . . ? C95 C94 C93 120.0(6) . . ? N19 C95 C94 122.3(6) . . ? C100 C96 C97 116.5(6) . . ? C100 C96 C93 122.0(6) . . ? C97 C96 C93 121.5(6) . . ? C98 C97 C96 119.5(6) . . ? N20 C98 C97 122.0(6) . . ? N20 C99 C100 120.8(6) . . ? C99 C100 C96 121.9(6) . . ? N21 C101 C102 121.8(6) . . ? C101 C102 C103 119.7(6) . . ? C104 C103 C102 117.3(6) . . ? C104 C103 C106 121.6(6) . . ? C102 C103 C106 121.1(6) . . ? C105 C104 C103 119.6(6) . . ? N21 C105 C104 122.3(6) . . ? C107 C106 C110 117.1(6) . . ? C107 C106 C103 122.1(6) . . ? C110 C106 C103 120.8(6) . . ? C108 C107 C106 121.4(7) . . ? C107 C108 N22 120.9(7) . . ? N22 C109 C110 120.4(6) . . ? C109 C110 C106 120.5(7) . . ? N23 C111 C112 122.1(6) . . ? C111 C112 C113 120.3(6) . . ? C112 C113 C114 116.3(6) . . ? C112 C113 C116 123.3(6) . . ? C114 C113 C116 120.4(6) . . ? C115 C114 C113 120.5(6) . . ? N23 C115 C114 121.9(6) . . ? C117 C116 C120 116.4(6) . . ? C117 C116 C113 120.9(6) . . ? C120 C116 C113 122.7(6) . . ? C118 C117 C116 121.1(7) . . ? N24 C118 C117 121.5(7) . . ? C120 C119 N24 122.1(6) . . ? C119 C120 C116 120.4(6) . . ? O15 S1 O14 119.7(8) . . ? O15 S1 O13 107.3(8) . . ? O14 S1 O13 108.6(8) . . ? O15 S1 C121 106.4(6) . . ? O14 S1 C121 109.6(7) . . ? O13 S1 C121 104.1(7) . . ? F1 C121 F3 107.8(15) . . ? F1 C121 F2 111.0(14) . . ? F3 C121 F2 97.6(12) . . ? F1 C121 S1 116.5(10) . . ? F3 C121 S1 115.2(10) . . ? F2 C121 S1 107.2(11) . . ? O16 S2 O17 118.0(9) . . ? O16 S2 O18 110.2(9) . . ? O17 S2 O18 116.6(7) . . ? O16 S2 C122 104.3(7) . . ? O17 S2 C122 103.0(6) . . ? O18 S2 C122 102.3(6) . . ? F4 C122 F6 104.2(12) . . ? F4 C122 F5 110.3(11) . . ? F6 C122 F5 103.5(11) . . ? F4 C122 S2 113.8(9) . . ? F6 C122 S2 112.3(8) . . ? F5 C122 S2 112.0(9) . . ? O20 S3 O19 115.0(9) . . ? O20 S3 O21 116.0(10) . . ? O19 S3 O21 110.9(9) . . ? O20 S3 C123 94.9(11) . . ? O19 S3 C123 114.6(14) . . ? O21 S3 C123 104.1(7) . . ? F9 C123 F8 115.0(15) . . ? F9 C123 F7 106.7(14) . . ? F8 C123 F7 106.9(15) . . ? F9 C123 S3 110.5(14) . . ? F8 C123 S3 112.1(16) . . ? F7 C123 S3 105.0(14) . . ? O24 S4 O22 117.2(10) . . ? O24 S4 O23 114.6(7) . . ? O22 S4 O23 112.4(10) . . ? O24 S4 C124 107.3(11) . . ? O22 S4 C124 109.7(9) . . ? O23 S4 C124 92.7(11) . . ? F12 C124 F11 114(2) . . ? F12 C124 F10 105.9(17) . . ? F11 C124 F10 106.5(19) . . ? F12 C124 S4 113.4(17) . . ? F11 C124 S4 113.7(14) . . ? F10 C124 S4 102.2(14) . . ? F13 B1 F16 112.3(8) . . ? F13 B1 F15 110.9(8) . . ? F16 B1 F15 111.5(8) . . ? F13 B1 F14 104.3(8) . . ? F16 B1 F14 109.4(8) . . ? F15 B1 F14 108.1(8) . . ? F17 B2 F19 108.9(10) . . ? F17 B2 F20 110.7(9) . . ? F19 B2 F20 111.3(9) . . ? F17 B2 F18 110.7(11) . . ? F19 B2 F18 106.1(8) . . ? F20 B2 F18 109.1(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.440 _refine_diff_density_min -1.217 _refine_diff_density_rms 0.156 # Attachment 'B703456C-Pt.cif' data_[Pt(BIPYMO)4][OTf]2 _database_code_depnum_ccdc_archive 'CCDC 639377' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H40 F6 N10 O11 Pt S2' _chemical_formula_weight 1282.09 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n 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 17.559(4) _cell_length_b 14.088(4) _cell_length_c 19.738(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.894(4) _cell_angle_gamma 90.00 _cell_volume 4865(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.5 _exptl_crystal_description colourless _exptl_crystal_colour blocks _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.750 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 3.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.144803 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 100 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22714 _diffrn_reflns_av_R_equivalents 0.1838 _diffrn_reflns_av_sigmaI/netI 0.1914 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 20.81 _reflns_number_total 5092 _reflns_number_gt 3240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.0000P)^2^+105.4539P] 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 5092 _refine_ls_number_parameters 442 _refine_ls_number_restraints 37 _refine_ls_R_factor_all 0.1524 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.2369 _refine_ls_wR_factor_gt 0.2123 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.074 _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 Pt1 Pt 0.79214(5) 0.14902(7) 0.83827(4) 0.0247(4) Uani 1 1 d . . . O1 O 0.3401(10) 0.1178(13) 1.1472(9) 0.050(5) Uani 1 1 d . . . O2 O 1.1658(10) 0.1243(11) 1.2743(9) 0.053(5) Uani 1 1 d . . . O3 O 1.2357(17) 0.1820(19) 0.5284(15) 0.132(12) Uani 1 1 d . . . O4 O 0.4129(11) 0.1192(11) 0.4070(8) 0.052(5) Uani 1 1 d . . . N1 N 0.7018(11) 0.1391(14) 0.8960(9) 0.035(5) Uani 1 1 d U . . N2 N 0.3971(13) 0.1225(14) 1.1107(11) 0.044(6) Uani 1 1 d . . . N3 N 0.8682(10) 0.1532(15) 0.9250(9) 0.036(5) Uani 1 1 d . . . N4 N 1.1187(12) 0.1253(13) 1.2197(11) 0.040(6) Uani 1 1 d U . . N5 N 0.8804(11) 0.1616(13) 0.7786(8) 0.034(5) Uani 1 1 d . . . N6 N 1.1811(19) 0.179(2) 0.5669(18) 0.103(11) Uani 1 1 d . . . N7 N 0.7196(10) 0.1379(14) 0.7505(9) 0.029(5) Uani 1 1 d U . . N8 N 0.4642(14) 0.1204(13) 0.4581(9) 0.042(6) Uani 1 1 d . . . C1 C 0.6422(14) 0.2012(18) 0.8880(13) 0.040(7) Uiso 1 1 d . . . H1A H 0.6419 0.2477 0.8531 0.048 Uiso 1 1 calc R . . C2 C 0.5834(13) 0.1986(16) 0.9280(11) 0.028(6) Uiso 1 1 d . . . H2A H 0.5435 0.2440 0.9210 0.033 Uiso 1 1 calc R . . C3 C 0.5800(12) 0.1302(15) 0.9800(11) 0.026(6) Uiso 1 1 d . . . C4 C 0.6431(12) 0.0700(15) 0.9862(11) 0.024(6) Uiso 1 1 d . . . H4A H 0.6451 0.0227 1.0207 0.029 Uiso 1 1 calc R . . C5 C 0.7001(13) 0.0745(16) 0.9474(11) 0.030(6) Uiso 1 1 d . . . H5A H 0.7415 0.0314 0.9553 0.036 Uiso 1 1 calc R . . C6 C 0.5178(13) 0.1295(15) 1.0233(11) 0.030(6) Uiso 1 1 d . . . C7 C 0.4493(14) 0.1726(18) 1.0075(13) 0.045(7) Uiso 1 1 d . . . H7A H 0.4418 0.2056 0.9655 0.054 Uiso 1 1 calc R . . C8 C 0.3889(16) 0.1709(19) 1.0498(14) 0.054(8) Uiso 1 1 d . . . H8A H 0.3425 0.2032 1.0365 0.064 Uiso 1 1 calc R . . C9 C 0.4667(14) 0.0812(16) 1.1280(12) 0.032(6) Uiso 1 1 d . . . H9A H 0.4751 0.0506 1.1709 0.039 Uiso 1 1 calc R . . C10 C 0.5242(14) 0.0824(16) 1.0859(12) 0.032(6) Uiso 1 1 d . . . H10A H 0.5704 0.0500 1.0995 0.038 Uiso 1 1 calc R . . C11 C 0.8507(14) 0.1941(16) 0.9802(12) 0.033(7) Uiso 1 1 d . . . H11A H 0.8028 0.2253 0.9808 0.039 Uiso 1 1 calc R . . C12 C 0.8994(13) 0.1934(17) 1.0369(12) 0.033(7) Uiso 1 1 d . . . H12A H 0.8854 0.2263 1.0759 0.039 Uiso 1 1 calc R . . C13 C 0.9667(13) 0.1479(18) 1.0402(12) 0.037(6) Uiso 1 1 d . . . C14 C 0.9875(15) 0.1058(17) 0.9789(13) 0.042(7) Uiso 1 1 d . . . H14A H 1.0356 0.0753 0.9779 0.050 Uiso 1 1 calc R . . C15 C 0.9371(15) 0.1094(17) 0.9198(13) 0.041(7) Uiso 1 1 d . . . H15A H 0.9501 0.0827 0.8781 0.050 Uiso 1 1 calc R . . C16 C 1.0201(13) 0.1353(17) 1.1025(12) 0.037(7) Uiso 1 1 d . . . C17 C 0.9937(17) 0.155(2) 1.1648(14) 0.064(8) Uiso 1 1 d . . . H17A H 0.9417 0.1714 1.1682 0.076 Uiso 1 1 calc R . . C18 C 1.0463(14) 0.1501(18) 1.2241(13) 0.042(7) Uiso 1 1 d . . . H18A H 1.0293 0.1648 1.2673 0.050 Uiso 1 1 calc R . . C19 C 1.1485(19) 0.105(2) 1.1607(16) 0.066(9) Uiso 1 1 d . . . H19A H 1.2001 0.0854 1.1590 0.079 Uiso 1 1 calc R . . C20 C 1.0979(15) 0.1141(16) 1.1016(13) 0.041(7) Uiso 1 1 d . . . H20A H 1.1177 0.1056 1.0587 0.049 Uiso 1 1 calc R . . C21 C 0.9268(14) 0.2350(18) 0.7825(13) 0.039(7) Uiso 1 1 d . . . H21A H 0.9192 0.2831 0.8149 0.047 Uiso 1 1 calc R . . C22 C 0.9850(14) 0.2446(17) 0.7424(12) 0.036(7) Uiso 1 1 d . . . H22A H 1.0161 0.2998 0.7457 0.043 Uiso 1 1 calc R . . C23 C 0.9992(13) 0.1737(16) 0.6961(11) 0.030(6) Uiso 1 1 d . . . C24 C 0.9476(14) 0.0965(17) 0.6924(13) 0.037(7) Uiso 1 1 d . . . H24A H 0.9522 0.0477 0.6598 0.044 Uiso 1 1 calc R . . C25 C 0.8920(15) 0.0921(19) 0.7353(13) 0.040(7) Uiso 1 1 d . . . H25A H 0.8601 0.0375 0.7346 0.048 Uiso 1 1 calc R . . C26 C 1.0580(17) 0.176(2) 0.6506(15) 0.058(9) Uiso 1 1 d . . . C27 C 1.1257(16) 0.2284(19) 0.6663(14) 0.054(8) Uiso 1 1 d . . . H27A H 1.1318 0.2629 0.7077 0.065 Uiso 1 1 calc R . . C28 C 1.184(2) 0.231(2) 0.6223(18) 0.077(10) Uiso 1 1 d . . . H28A H 1.2276 0.2702 0.6330 0.092 Uiso 1 1 calc R . . C29 C 1.115(2) 0.133(3) 0.5463(19) 0.088(11) Uiso 1 1 d . . . H29A H 1.1106 0.1024 0.5032 0.105 Uiso 1 1 calc R . . C30 C 1.051(2) 0.128(2) 0.5871(17) 0.085(11) Uiso 1 1 d . . . H30A H 1.0055 0.0949 0.5721 0.102 Uiso 1 1 calc R . . C31 C 0.7310(14) 0.1930(17) 0.6975(12) 0.035(7) Uiso 1 1 d . . . H31A H 0.7723 0.2369 0.7012 0.042 Uiso 1 1 calc R . . C32 C 0.6851(13) 0.1883(16) 0.6379(12) 0.032(7) Uiso 1 1 d . . . H32A H 0.6942 0.2281 0.6005 0.038 Uiso 1 1 calc R . . C33 C 0.6244(12) 0.1231(14) 0.6335(11) 0.022(6) Uiso 1 1 d . . . C34 C 0.6157(13) 0.0641(16) 0.6888(11) 0.029(6) Uiso 1 1 d . . . H34A H 0.5763 0.0176 0.6869 0.034 Uiso 1 1 calc R . . C35 C 0.6645(11) 0.0741(14) 0.7453(10) 0.015(5) Uiso 1 1 d . . . H35A H 0.6587 0.0334 0.7829 0.019 Uiso 1 1 calc R . . C36 C 0.5689(13) 0.1205(15) 0.5718(12) 0.030(7) Uiso 1 1 d . . . C37 C 0.5904(14) 0.1438(18) 0.5083(12) 0.040(7) Uiso 1 1 d . . . H37A H 0.6423 0.1587 0.5027 0.048 Uiso 1 1 calc R . . C38 C 0.5366(18) 0.145(2) 0.4523(16) 0.066(9) Uiso 1 1 d . . . H38A H 0.5517 0.1646 0.4093 0.080 Uiso 1 1 calc R . . C39 C 0.4414(13) 0.0933(15) 0.5209(11) 0.024(6) Uiso 1 1 d . . . H39A H 0.3895 0.0767 0.5247 0.028 Uiso 1 1 calc R . . C40 C 0.4922(13) 0.0902(16) 0.5773(12) 0.034(7) Uiso 1 1 d . . . H40A H 0.4766 0.0682 0.6195 0.041 Uiso 1 1 calc R . . S1 S -0.3742(5) 1.0092(7) 0.2819(5) 0.080(3) Uani 1 1 d D . . O5 O -0.3283(13) 1.0616(18) 0.2379(13) 0.117(10) Uani 1 1 d D . . O6 O -0.3373(13) 0.988(2) 0.3473(11) 0.142(12) Uani 1 1 d D . . O7 O -0.4522(10) 1.0407(15) 0.2825(10) 0.082(7) Uani 1 1 d D . . C41 C -0.386(2) 0.893(3) 0.246(2) 0.088(12) Uiso 1 1 d D . . F1 F -0.4156(14) 0.8973(15) 0.1841(12) 0.126(8) Uani 1 1 d D . . F2 F -0.4257(15) 0.8385(14) 0.2809(13) 0.158(12) Uani 1 1 d D . . F3 F -0.3172(13) 0.8536(18) 0.2443(13) 0.169(12) Uani 1 1 d D . . S2 S 0.7082(6) 0.3880(7) 0.4294(5) 0.087(3) Uani 1 1 d D . . O8 O 0.7009(19) 0.311(2) 0.4774(15) 0.190(16) Uani 1 1 d D . . O9 O 0.6691(10) 0.4683(13) 0.4506(13) 0.101(9) Uani 1 1 d D . . O10 O 0.7846(10) 0.4003(18) 0.4109(10) 0.095(8) Uani 1 1 d D . . C42 C 0.658(3) 0.355(4) 0.351(2) 0.39(9) Uiso 1 1 d D . . F4 F 0.6830(18) 0.272(2) 0.3404(17) 0.28(2) Uani 1 1 d D . . F5 F 0.6659(14) 0.413(2) 0.3025(12) 0.176(12) Uani 1 1 d D . . F6 F 0.5844(14) 0.354(4) 0.3615(15) 0.60(7) Uani 1 1 d D . . N1S N 0.532(2) 0.610(2) 0.1182(16) 0.104(11) Uiso 1 1 d . . . C1S C 0.594(3) 0.620(3) 0.129(2) 0.118(15) Uiso 1 1 d . . . C2S C 0.677(3) 0.615(4) 0.136(3) 0.20(3) Uiso 1 1 d . . . H2SA H 0.6973 0.6731 0.1586 0.237 Uiso 1 1 calc R . . H2SB H 0.6961 0.6102 0.0910 0.237 Uiso 1 1 calc R . . H2SC H 0.6930 0.5598 0.1634 0.237 Uiso 1 1 calc R . . N2S N 0.832(2) 0.096(3) 0.535(2) 0.140(14) Uiso 1 1 d . . . C3S C 0.8016(19) 0.034(2) 0.5603(17) 0.073(10) Uiso 1 1 d . . . C4S C 0.763(2) -0.041(2) 0.5901(18) 0.094(12) Uiso 1 1 d . . . H4SA H 0.7077 -0.0273 0.5863 0.112 Uiso 1 1 calc R . . H4SB H 0.7812 -0.0465 0.6381 0.112 Uiso 1 1 calc R . . H4SC H 0.7721 -0.1003 0.5665 0.112 Uiso 1 1 calc R . . O1W O 0.6957(19) 0.590(2) 0.3411(17) 0.156(12) Uiso 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 Pt1 0.0204(6) 0.0372(6) 0.0141(5) -0.0012(6) -0.0133(4) -0.0025(6) O1 0.029(11) 0.086(16) 0.035(11) -0.014(10) 0.005(9) -0.009(10) O2 0.067(13) 0.044(12) 0.041(11) -0.008(9) -0.036(10) -0.006(10) O3 0.13(2) 0.13(2) 0.15(3) 0.037(19) 0.12(2) 0.022(19) O4 0.079(15) 0.044(13) 0.028(11) 0.004(9) -0.029(11) 0.002(10) N1 0.034(8) 0.040(9) 0.030(8) -0.003(8) -0.010(7) -0.008(8) N2 0.049(16) 0.040(15) 0.044(15) -0.014(11) 0.000(13) 0.008(12) N3 0.031(12) 0.058(14) 0.017(11) -0.004(11) -0.008(9) -0.017(12) N4 0.043(9) 0.031(9) 0.042(9) -0.004(7) -0.014(8) -0.008(7) N5 0.058(14) 0.027(12) 0.012(10) 0.013(10) -0.023(10) -0.025(12) N6 0.09(2) 0.10(3) 0.13(3) -0.02(2) 0.06(2) -0.02(2) N7 0.034(8) 0.031(8) 0.021(8) -0.016(7) -0.005(7) -0.002(7) N8 0.082(19) 0.035(15) 0.008(12) 0.007(9) -0.006(12) 0.014(12) S1 0.055(6) 0.101(8) 0.081(7) 0.034(6) -0.005(5) -0.002(5) O5 0.080(18) 0.14(2) 0.13(2) 0.056(19) 0.014(16) -0.038(17) O6 0.077(18) 0.24(4) 0.10(2) 0.05(2) -0.048(16) 0.00(2) O7 0.053(15) 0.108(18) 0.084(16) 0.026(14) -0.007(12) 0.003(14) F1 0.13(2) 0.120(18) 0.13(2) -0.024(15) 0.008(17) -0.007(15) F2 0.20(3) 0.081(16) 0.21(3) 0.015(17) 0.12(2) -0.036(17) F3 0.13(2) 0.21(3) 0.17(2) 0.08(2) 0.074(19) 0.11(2) S2 0.084(8) 0.086(8) 0.091(8) -0.003(6) 0.009(6) -0.033(6) O8 0.21(4) 0.19(3) 0.17(3) 0.09(3) 0.04(3) -0.07(3) O9 0.036(13) 0.053(14) 0.20(3) -0.058(16) -0.042(15) 0.028(11) O10 0.041(14) 0.19(3) 0.049(14) 0.013(15) -0.005(11) -0.019(15) F4 0.20(4) 0.38(6) 0.25(4) 0.08(4) -0.12(3) -0.13(4) F5 0.12(2) 0.28(4) 0.12(2) 0.05(2) -0.051(17) -0.01(2) F6 0.06(2) 1.6(2) 0.15(3) -0.30(7) 0.04(2) -0.12(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N5 2.03(2) . ? Pt1 N1 2.036(19) . ? Pt1 N7 2.066(17) . ? Pt1 N3 2.081(17) . ? O1 N2 1.29(2) . ? O2 N4 1.30(2) . ? O3 N6 1.27(3) . ? O4 N8 1.29(2) . ? N1 C1 1.36(3) . ? N1 C5 1.36(3) . ? N2 C9 1.37(3) . ? N2 C8 1.38(3) . ? N3 C11 1.29(3) . ? N3 C15 1.37(3) . ? N4 C18 1.33(3) . ? N4 C19 1.35(3) . ? N5 C21 1.31(3) . ? N5 C25 1.33(3) . ? N6 C28 1.31(4) . ? N6 C29 1.37(4) . ? N7 C35 1.32(2) . ? N7 C31 1.33(3) . ? N8 C38 1.33(3) . ? N8 C39 1.39(3) . ? C1 C2 1.35(3) . ? C2 C3 1.41(3) . ? C3 C4 1.39(3) . ? C3 C6 1.44(3) . ? C4 C5 1.31(3) . ? C6 C7 1.36(3) . ? C6 C10 1.40(3) . ? C7 C8 1.40(3) . ? C9 C10 1.36(3) . ? C11 C12 1.35(3) . ? C12 C13 1.34(3) . ? C13 C14 1.42(3) . ? C13 C16 1.49(3) . ? C14 C15 1.40(3) . ? C16 C17 1.38(3) . ? C16 C20 1.40(3) . ? C17 C18 1.43(4) . ? C19 C20 1.41(4) . ? C21 C22 1.35(3) . ? C22 C23 1.39(3) . ? C23 C24 1.41(3) . ? C23 C26 1.42(3) . ? C24 C25 1.35(3) . ? C26 C27 1.41(4) . ? C26 C30 1.42(4) . ? C27 C28 1.40(4) . ? C29 C30 1.44(4) . ? C31 C32 1.37(3) . ? C32 C33 1.40(3) . ? C33 C34 1.39(3) . ? C33 C36 1.49(3) . ? C34 C35 1.35(3) . ? C36 C37 1.38(3) . ? C36 C40 1.43(3) . ? C37 C38 1.39(4) . ? C39 C40 1.37(3) . ? S1 O6 1.425(18) . ? S1 O5 1.437(19) . ? S1 O7 1.441(17) . ? S1 C41 1.79(4) . ? C41 F1 1.28(4) . ? C41 F2 1.28(4) . ? C41 F3 1.33(4) . ? S2 O9 1.406(16) . ? S2 O10 1.431(17) . ? S2 O8 1.45(2) . ? S2 C42 1.77(4) . ? C42 F4 1.28(4) . ? C42 F5 1.28(4) . ? C42 F6 1.32(4) . ? N1S C1S 1.09(5) . ? C1S C2S 1.45(6) . ? N2S C3S 1.16(4) . ? C3S C4S 1.41(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Pt1 N1 178.3(7) . . ? N5 Pt1 N7 88.1(7) . . ? N1 Pt1 N7 90.6(7) . . ? N5 Pt1 N3 90.4(7) . . ? N1 Pt1 N3 91.0(7) . . ? N7 Pt1 N3 176.7(8) . . ? C1 N1 C5 117(2) . . ? C1 N1 Pt1 121.2(16) . . ? C5 N1 Pt1 122.0(16) . . ? O1 N2 C9 124(2) . . ? O1 N2 C8 119(2) . . ? C9 N2 C8 117(2) . . ? C11 N3 C15 123(2) . . ? C11 N3 Pt1 121.6(17) . . ? C15 N3 Pt1 115.8(16) . . ? O2 N4 C18 120(2) . . ? O2 N4 C19 117(2) . . ? C18 N4 C19 124(2) . . ? C21 N5 C25 119(2) . . ? C21 N5 Pt1 122.2(17) . . ? C25 N5 Pt1 118.3(16) . . ? O3 N6 C28 120(3) . . ? O3 N6 C29 120(3) . . ? C28 N6 C29 119(3) . . ? C35 N7 C31 119.6(19) . . ? C35 N7 Pt1 120.9(15) . . ? C31 N7 Pt1 119.4(16) . . ? O4 N8 C38 123(2) . . ? O4 N8 C39 117(2) . . ? C38 N8 C39 120(2) . . ? C2 C1 N1 122(2) . . ? C1 C2 C3 122(2) . . ? C4 C3 C2 113(2) . . ? C4 C3 C6 125(2) . . ? C2 C3 C6 121(2) . . ? C5 C4 C3 124(2) . . ? C4 C5 N1 122(2) . . ? C7 C6 C10 115(2) . . ? C7 C6 C3 124(2) . . ? C10 C6 C3 121(2) . . ? C6 C7 C8 124(3) . . ? N2 C8 C7 120(3) . . ? C10 C9 N2 122(2) . . ? C9 C10 C6 123(2) . . ? N3 C11 C12 121(2) . . ? C13 C12 C11 123(2) . . ? C12 C13 C14 116(2) . . ? C12 C13 C16 126(2) . . ? C14 C13 C16 118(2) . . ? C15 C14 C13 120(2) . . ? N3 C15 C14 117(2) . . ? C17 C16 C20 117(2) . . ? C17 C16 C13 118(2) . . ? C20 C16 C13 124(2) . . ? C16 C17 C18 119(3) . . ? N4 C18 C17 121(2) . . ? N4 C19 C20 116(3) . . ? C16 C20 C19 124(3) . . ? N5 C21 C22 123(2) . . ? C21 C22 C23 120(2) . . ? C22 C23 C24 116(2) . . ? C22 C23 C26 125(2) . . ? C24 C23 C26 119(2) . . ? C25 C24 C23 120(2) . . ? N5 C25 C24 122(3) . . ? C27 C26 C30 117(3) . . ? C27 C26 C23 121(3) . . ? C30 C26 C23 122(3) . . ? C28 C27 C26 122(3) . . ? N6 C28 C27 121(3) . . ? N6 C29 C30 123(3) . . ? C26 C30 C29 117(3) . . ? N7 C31 C32 122(2) . . ? C31 C32 C33 118(2) . . ? C34 C33 C32 119(2) . . ? C34 C33 C36 121(2) . . ? C32 C33 C36 120(2) . . ? C35 C34 C33 119(2) . . ? N7 C35 C34 123(2) . . ? C37 C36 C40 118(2) . . ? C37 C36 C33 122(2) . . ? C40 C36 C33 120(2) . . ? C36 C37 C38 120(3) . . ? N8 C38 C37 121(3) . . ? C40 C39 N8 121(2) . . ? C39 C40 C36 119(2) . . ? O6 S1 O5 114.7(15) . . ? O6 S1 O7 114.4(14) . . ? O5 S1 O7 115.5(14) . . ? O6 S1 C41 101.7(19) . . ? O5 S1 C41 106.3(18) . . ? O7 S1 C41 102.0(17) . . ? F1 C41 F2 110(4) . . ? F1 C41 F3 107(3) . . ? F2 C41 F3 107(3) . . ? F1 C41 S1 111(3) . . ? F2 C41 S1 112(3) . . ? F3 C41 S1 108(3) . . ? O9 S2 O10 118.2(14) . . ? O9 S2 O8 109.6(17) . . ? O10 S2 O8 113.2(17) . . ? O9 S2 C42 104.4(19) . . ? O10 S2 C42 102.6(18) . . ? O8 S2 C42 108(2) . . ? F4 C42 F5 114(4) . . ? F4 C42 F6 112(4) . . ? F5 C42 F6 107(4) . . ? F4 C42 S2 104(3) . . ? F5 C42 S2 114(3) . . ? F6 C42 S2 107(3) . . ? N1S C1S C2S 169(5) . . ? N2S C3S C4S 178(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.81 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.483 _refine_diff_density_min -1.654 _refine_diff_density_rms 0.201 # Attachment 'B703456C-Zn.cif' data_[Zn(H2O)2(BIPYMO)4][OTf]2 _database_code_depnum_ccdc_archive 'CCDC 639378' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H36 F6 N8 O12 S2 Zn' _chemical_formula_weight 1088.28 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4nc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 17.347(4) _cell_length_b 17.347(4) _cell_length_c 8.061(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2425.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.3 _exptl_crystal_description colourless _exptl_crystal_colour blocks _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.683 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.549499 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD' _diffrn_measurement_method 'hemisphere scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 100 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20987 _diffrn_reflns_av_R_equivalents 0.0895 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2141 _reflns_number_gt 1939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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. The two CF3SO3 anions and are disordered over two positions and needed to be restrained to attain chemically reasonable geometries. S-O, C-F, F...F and O...O distances were restrained to be equal using the SADI and SIMU commands; the S-c distance was restrained to be 1.84 A (DFIX). ; _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^)+(0.1224P)^2^+14.0521P] 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 SHELXL _refine_ls_extinction_coef 0.006(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.45(6) _refine_ls_number_reflns 2141 _refine_ls_number_parameters 200 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.1060 _refine_ls_R_factor_gt 0.0997 _refine_ls_wR_factor_ref 0.2704 _refine_ls_wR_factor_gt 0.2657 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.002 _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 Zn1 Zn 0.0000 0.0000 -0.4616(3) 0.0274(5) Uani 1 4 d S . . O1W O 0.0000 0.0000 -0.725(2) 0.034(4) Uani 1 4 d S . . H1WA H -0.0453 -0.0056 -0.7593 0.051 Uiso 0.50 1 calc PR . . O2W O 0.0000 0.0000 -0.199(2) 0.045(5) Uani 1 4 d S . . H2WA H 0.0453 0.0056 -0.1641 0.068 Uiso 0.50 1 calc PR . . N1 N -0.0675(3) 0.1042(3) -0.4559(13) 0.0285(14) Uani 1 1 d . . . C1 C -0.0520(6) 0.1669(6) -0.5543(15) 0.043(2) Uani 1 1 d . . . H1A H -0.0078 0.1655 -0.6237 0.052 Uiso 1 1 calc R . . C2 C -0.0971(6) 0.2305(5) -0.5567(15) 0.045(2) Uani 1 1 d . . . H2A H -0.0837 0.2731 -0.6251 0.054 Uiso 1 1 calc R . . C3 C -0.1639(4) 0.2335(4) -0.4574(17) 0.0357(19) Uani 1 1 d . . . C4 C -0.1782(6) 0.1735(6) -0.3583(13) 0.043(2) Uani 1 1 d . . . H4A H -0.2205 0.1760 -0.2837 0.052 Uiso 1 1 calc R . . C5 C -0.1318(5) 0.1062(5) -0.3613(12) 0.034(2) Uani 1 1 d . . . H5A H -0.1459 0.0626 -0.2969 0.041 Uiso 1 1 calc R . . C6 C -0.2156(5) 0.3026(5) -0.4630(19) 0.044(2) Uani 1 1 d . . . C7 C -0.1925(6) 0.3757(5) -0.5108(15) 0.051(3) Uani 1 1 d . . . H7A H -0.1400 0.3837 -0.5402 0.062 Uiso 1 1 calc R . . C8 C -0.2414(6) 0.4360(6) -0.5172(18) 0.068(5) Uani 1 1 d . . . H8A H -0.2233 0.4854 -0.5498 0.081 Uiso 1 1 calc R . . N2 N -0.3179(5) 0.4254(5) -0.476(3) 0.096(5) Uani 1 1 d . . . C9 C -0.3445(6) 0.3563(6) -0.426(2) 0.071(5) Uani 1 1 d . . . H9A H -0.3962 0.3505 -0.3892 0.086 Uiso 1 1 calc R . . C10 C -0.2948(6) 0.2940(6) -0.4290(15) 0.054(4) Uani 1 1 d . . . H10A H -0.3146 0.2439 -0.4076 0.065 Uiso 1 1 calc R . . O1 O -0.3666(5) 0.4837(4) -0.474(3) 0.171(9) Uani 1 1 d . . . S1 S -0.0893(3) -0.3618(4) -0.6365(8) 0.0626(16) Uani 0.50 1 d PDU . . O2 O -0.0738(14) -0.3561(15) -0.466(2) 0.128(8) Uani 0.50 1 d PDU . . O3 O -0.0609(12) -0.3025(13) -0.735(3) 0.120(10) Uani 0.50 1 d PDU . . O4 O -0.1659(7) -0.3832(9) -0.672(2) 0.075(5) Uani 0.50 1 d PDU . . C11 C -0.0289(11) -0.4377(10) -0.730(2) 0.088(7) Uani 0.50 1 d PDU . . F1 F 0.0441(11) -0.4195(12) -0.686(4) 0.129(7) Uani 0.50 1 d PDU . . F2 F -0.0356(18) -0.4298(12) -0.896(2) 0.160(10) Uani 0.50 1 d PDU . . F3 F -0.0442(11) -0.5099(13) -0.682(3) 0.134(9) Uani 0.50 1 d PDU . . 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 Zn1 0.0205(6) 0.0205(6) 0.0412(9) 0.000 0.000 0.000 O1W 0.030(6) 0.030(6) 0.042(10) 0.000 0.000 0.000 O2W 0.039(7) 0.039(7) 0.059(12) 0.000 0.000 0.000 N1 0.026(3) 0.018(3) 0.041(3) 0.002(4) 0.013(4) 0.006(2) C1 0.032(5) 0.042(5) 0.055(6) 0.005(5) 0.018(5) -0.004(4) C2 0.045(6) 0.032(5) 0.058(6) 0.016(5) 0.001(5) 0.005(4) C3 0.028(4) 0.030(4) 0.049(5) -0.017(6) 0.004(5) 0.012(3) C4 0.048(6) 0.036(5) 0.046(5) -0.005(4) 0.007(5) 0.016(4) C5 0.020(4) 0.033(5) 0.048(5) -0.001(4) 0.015(4) -0.005(4) C6 0.034(4) 0.028(4) 0.069(5) -0.015(6) -0.025(6) 0.011(3) C7 0.032(5) 0.026(4) 0.096(11) -0.003(5) -0.018(5) 0.007(4) C8 0.029(5) 0.033(5) 0.141(15) 0.000(6) -0.042(7) 0.002(4) N2 0.036(5) 0.032(5) 0.220(16) -0.020(9) -0.031(9) 0.018(4) C9 0.037(5) 0.039(6) 0.138(15) -0.029(7) -0.039(7) 0.013(4) C10 0.048(6) 0.035(5) 0.080(11) -0.034(5) -0.047(6) 0.017(4) O1 0.039(4) 0.023(4) 0.45(3) -0.068(11) -0.079(11) 0.022(3) S1 0.050(3) 0.069(4) 0.069(3) 0.011(3) 0.013(3) 0.015(3) O2 0.15(2) 0.13(2) 0.100(10) -0.022(16) -0.039(17) 0.003(17) O3 0.067(12) 0.104(17) 0.19(2) 0.084(17) -0.017(14) 0.015(11) O4 0.028(6) 0.065(9) 0.133(16) -0.032(10) 0.002(8) 0.039(6) C11 0.094(13) 0.053(10) 0.118(12) -0.041(13) 0.004(16) 0.043(12) F1 0.088(12) 0.087(13) 0.21(2) 0.006(15) 0.029(13) 0.002(11) F2 0.29(3) 0.091(14) 0.102(11) -0.048(10) 0.026(15) -0.011(19) F3 0.067(13) 0.115(14) 0.22(2) 0.040(16) -0.009(15) -0.006(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 Zn1 O1W 2.119(16) . ? Zn1 O2W 2.119(19) . ? Zn1 N1 2.154(6) 4 ? Zn1 N1 2.154(6) 2 ? Zn1 N1 2.154(6) . ? Zn1 N1 2.154(6) 3 ? N1 C5 1.351(11) . ? N1 C1 1.372(12) . ? C1 C2 1.353(14) . ? C2 C3 1.410(14) . ? C3 C4 1.335(15) . ? C3 C6 1.497(10) . ? C4 C5 1.418(14) . ? C6 C7 1.386(14) . ? C6 C10 1.407(15) . ? C7 C8 1.348(13) . ? C8 N2 1.380(16) . ? N2 O1 1.318(10) . ? N2 C9 1.347(18) . ? C9 C10 1.383(13) . ? S1 O3 1.387(16) . ? S1 O2 1.404(18) . ? S1 O4 1.410(14) . ? S1 C11 1.843(16) . ? C11 F3 1.338(19) . ? C11 F1 1.35(2) . ? C11 F2 1.35(2) . ? C11 F3 1.61(3) 2_545 ? F1 F3 1.23(3) 2_545 ? F3 F1 1.23(3) 2_545 ? F3 F3 1.57(4) 2_545 ? F3 C11 1.61(3) 2_545 ? 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 O1W Zn1 O2W 180 . . ? O1W Zn1 N1 91.2(3) . 4 ? O2W Zn1 N1 88.8(3) . 4 ? O1W Zn1 N1 91.2(3) . 2 ? O2W Zn1 N1 88.8(3) . 2 ? N1 Zn1 N1 89.975(13) 4 2 ? O1W Zn1 N1 91.2(3) . . ? O2W Zn1 N1 88.8(3) . . ? N1 Zn1 N1 89.974(13) 4 . ? N1 Zn1 N1 177.5(6) 2 . ? O1W Zn1 N1 91.2(3) . 3 ? O2W Zn1 N1 88.8(3) . 3 ? N1 Zn1 N1 177.5(6) 4 3 ? N1 Zn1 N1 89.972(13) 2 3 ? N1 Zn1 N1 89.973(13) . 3 ? C5 N1 C1 117.8(7) . . ? C5 N1 Zn1 118.8(6) . . ? C1 N1 Zn1 123.1(6) . . ? C2 C1 N1 122.8(9) . . ? C1 C2 C3 119.8(9) . . ? C4 C3 C2 117.6(8) . . ? C4 C3 C6 122.0(10) . . ? C2 C3 C6 120.4(10) . . ? C3 C4 C5 121.8(9) . . ? N1 C5 C4 120.0(8) . . ? C7 C6 C10 115.7(8) . . ? C7 C6 C3 124.5(9) . . ? C10 C6 C3 119.6(9) . . ? C8 C7 C6 122.6(10) . . ? C7 C8 N2 119.5(10) . . ? O1 N2 C9 117.3(12) . . ? O1 N2 C8 121.1(11) . . ? C9 N2 C8 121.4(9) . . ? N2 C9 C10 118.4(12) . . ? C9 C10 C6 122.0(10) . . ? O3 S1 O2 116.0(12) . . ? O3 S1 O4 114.4(10) . . ? O2 S1 O4 113.5(10) . . ? O3 S1 C11 95.5(14) . . ? O2 S1 C11 109.9(14) . . ? O4 S1 C11 105.3(9) . . ? F3 C11 F1 109.3(13) . . ? F3 C11 F2 111.3(14) . . ? F1 C11 F2 108.3(15) . . ? F3 C11 F3 63.7(14) . 2_545 ? F1 C11 F3 48.0(12) . 2_545 ? F2 C11 F3 111.3(19) . 2_545 ? F3 C11 S1 116.0(16) . . ? F1 C11 S1 105.1(15) . . ? F2 C11 S1 106.4(16) . . ? F3 C11 S1 139.0(13) 2_545 . ? F3 F1 C11 77.0(17) 2_545 . ? F1 F3 C11 158(2) 2_545 . ? F1 F3 F3 103(2) 2_545 2_545 ? C11 F3 F3 66.5(15) . 2_545 ? F1 F3 C11 55.0(15) 2_545 2_545 ? C11 F3 C11 107.7(17) . 2_545 ? F3 F3 C11 49.8(12) 2_545 2_545 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.707 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.133