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 ; Dr Ramon Vilar Imperial College London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email R.VILAR@IMPERIAL.AC.UK #------------------------------------------------------------------------- #3 Publication details _publ_section_title ; Synthesis, structural characterization and anion binding studies of palladium macrocycles with hydrogen-bonding ligands ; loop_ _publ_author_name _publ_author_address P.Diaz ;Department of Chemistry Imperial College London London SW7 2AZ, UK ; J.A.Tovilla ;Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; P.Ballester ;Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; J.Benet-Buchholz ;X-ray Diffraction Unit Institute of Chemical Research of Catalonia (ICIQ) Avd. Paisos Catalans 16 E-43007 Tarragona, Spain ; R.Vilar ;Department of Chemistry Imperial College London South Kensington London SW7 2AZ, UK ; _publ_contact_author_name 'Dr Ramon Vilar' data_L1aJTC306Pccn _database_code_depnum_ccdc_archive 'CCDC 624779' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H14 N4 O' _chemical_formula_weight 242.28 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 16.291(2) _cell_length_b 16.300(2) _cell_length_c 9.1949(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2441.7(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8524 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 36.29 _exptl_crystal_description Block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.088 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.866473 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16300 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.79 _diffrn_reflns_theta_max 36.45 _reflns_number_total 4673 _reflns_number_gt 4197 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.1258P)^2^+0.5313P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4673 _refine_ls_number_parameters 166 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0700 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 N1A N 0.18257(8) 0.72843(10) 0.80330(10) 0.0161(3) Uani 1 1 d . . . H1AA H 0.1831 0.7328 0.8987 0.019 Uiso 1 1 calc R . . O1A O 0.2500 0.7500 0.58992(13) 0.0154(3) Uani 1 2 d S . . C1A C 0.2500 0.7500 0.72582(17) 0.0120(3) Uani 1 2 d S . . N2A N -0.03680(9) 0.87728(11) 0.49928(14) 0.0229(3) Uani 1 1 d . . . C2A C 0.10963(10) 0.69819(10) 0.73039(13) 0.0165(3) Uani 1 1 d . . . H2AA H 0.0739 0.6715 0.8035 0.020 Uiso 1 1 calc R . . H6AB H 0.1264 0.6556 0.6596 0.020 Uiso 1 1 calc R . . C3A C 0.05982(9) 0.76241(11) 0.65121(13) 0.0163(3) Uani 1 1 d . . . C4A C 0.07496(11) 0.84524(12) 0.66317(14) 0.0207(3) Uani 1 1 d . . . H4AB H 0.1181 0.8647 0.7235 0.025 Uiso 1 1 calc R . . C5A C 0.02606(12) 0.90010(13) 0.58555(16) 0.0230(3) Uani 1 1 d . . . H5AB H 0.0378 0.9570 0.5940 0.028 Uiso 1 1 calc R . . C6A C -0.05098(11) 0.79766(14) 0.48977(17) 0.0248(4) Uani 1 1 d . . . H6AA H -0.0953 0.7800 0.4303 0.030 Uiso 1 1 calc R . . C7A C -0.00508(11) 0.73791(13) 0.56132(16) 0.0225(3) Uani 1 1 d . . . H7AA H -0.0176 0.6814 0.5493 0.027 Uiso 1 1 calc R . . N1B N 0.76925(9) 0.81742(9) 0.84273(11) 0.0161(3) Uani 1 1 d . . . H1BA H 0.7605 0.8182 0.9371 0.019 Uiso 1 1 calc R . . O1B O 0.7500 0.7500 0.62859(14) 0.0174(3) Uani 1 2 d S . . C1B C 0.7500 0.7500 0.76411(17) 0.0129(3) Uani 1 2 d S . . N2B N 0.63758(12) 1.04401(11) 0.52973(14) 0.0269(3) Uani 1 1 d . . . C2B C 0.80422(10) 0.88810(11) 0.77162(14) 0.0183(3) Uani 1 1 d . . . H2BA H 0.8470 0.8691 0.7030 0.022 Uiso 1 1 calc R . . H2BB H 0.8316 0.9224 0.8460 0.022 Uiso 1 1 calc R . . C3B C 0.74396(11) 0.94108(11) 0.68915(13) 0.0177(3) Uani 1 1 d . . . C4B C 0.77410(14) 1.00357(13) 0.60113(17) 0.0251(4) Uani 1 1 d . . . H4BB H 0.8315 1.0125 0.5928 0.030 Uiso 1 1 calc R . . C5B C 0.71916(15) 1.05283(14) 0.52562(18) 0.0298(4) Uani 1 1 d . . . H5BA H 0.7410 1.0956 0.4671 0.036 Uiso 1 1 calc R . . C6B C 0.60873(12) 0.98351(13) 0.61455(16) 0.0243(3) Uani 1 1 d . . . H6BA H 0.5510 0.9757 0.6196 0.029 Uiso 1 1 calc R . . C7B C 0.65920(11) 0.93146(12) 0.69583(15) 0.0211(3) Uani 1 1 d . . . H7BA H 0.6358 0.8899 0.7551 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1A 0.0146(6) 0.0303(8) 0.0035(4) 0.0008(3) 0.0006(3) 0.0014(4) O1A 0.0188(8) 0.0255(9) 0.0020(4) 0.000 0.000 0.0012(6) C1A 0.0147(9) 0.0173(10) 0.0039(5) 0.000 0.000 0.0022(6) N2A 0.0157(7) 0.0394(9) 0.0135(4) 0.0032(5) -0.0014(4) 0.0058(5) C2A 0.0167(7) 0.0236(8) 0.0092(4) 0.0008(4) -0.0005(4) 0.0000(5) C3A 0.0141(7) 0.0282(8) 0.0065(4) -0.0005(4) 0.0004(3) 0.0003(5) C4A 0.0217(8) 0.0275(9) 0.0129(5) -0.0033(4) -0.0061(4) 0.0048(6) C5A 0.0243(8) 0.0290(10) 0.0156(5) -0.0021(5) -0.0041(5) 0.0071(6) C6A 0.0149(8) 0.0426(12) 0.0170(5) 0.0049(6) -0.0052(4) -0.0031(6) C7A 0.0176(8) 0.0343(10) 0.0157(5) 0.0039(5) -0.0046(4) -0.0058(6) N1B 0.0270(7) 0.0183(7) 0.0029(4) -0.0002(3) 0.0003(3) -0.0015(5) O1B 0.0279(9) 0.0224(9) 0.0020(4) 0.000 0.000 0.0003(6) C1B 0.0162(9) 0.0188(11) 0.0036(5) 0.000 0.000 0.0017(6) N2B 0.0444(10) 0.0220(9) 0.0143(5) 0.0013(4) -0.0008(5) 0.0053(6) C2B 0.0224(8) 0.0229(9) 0.0096(4) 0.0009(4) -0.0005(4) -0.0025(5) C3B 0.0296(8) 0.0168(8) 0.0066(4) 0.0003(4) 0.0015(4) -0.0026(5) C4B 0.0344(10) 0.0262(10) 0.0147(5) 0.0059(5) -0.0007(5) -0.0078(7) C5B 0.0487(12) 0.0239(10) 0.0167(6) 0.0059(5) -0.0019(6) -0.0044(8) C6B 0.0301(9) 0.0282(10) 0.0145(5) 0.0020(5) 0.0038(5) 0.0073(7) C7B 0.0272(9) 0.0242(9) 0.0118(5) 0.0042(4) 0.0047(4) 0.0021(6) _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 N1A C1A 1.3556(15) . ? N1A C2A 1.451(2) . ? O1A C1A 1.2497(19) . ? C1A N1A 1.3557(15) 2_565 ? N2A C6A 1.321(3) . ? N2A C5A 1.348(2) . ? C2A C3A 1.511(2) . ? C3A C4A 1.377(3) . ? C3A C7A 1.400(2) . ? C4A C5A 1.394(2) . ? C6A C7A 1.393(3) . ? N1B C1B 1.3523(16) . ? N1B C2B 1.442(2) . ? O1B C1B 1.2461(19) . ? C1B N1B 1.3523(16) 2_665 ? N2B C5B 1.337(3) . ? N2B C6B 1.342(3) . ? C2B C3B 1.511(2) . ? C3B C4B 1.391(2) . ? C3B C7B 1.391(3) . ? C4B C5B 1.389(3) . ? C6B C7B 1.398(2) . ? 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 C1A N1A C2A 120.60(10) . . ? O1A C1A N1A 121.70(7) . . ? O1A C1A N1A 121.70(7) . 2_565 ? N1A C1A N1A 116.60(14) . 2_565 ? C6A N2A C5A 116.29(15) . . ? N1A C2A C3A 115.29(14) . . ? C4A C3A C7A 117.52(15) . . ? C4A C3A C2A 122.99(13) . . ? C7A C3A C2A 119.49(16) . . ? C3A C4A C5A 119.06(15) . . ? N2A C5A C4A 123.95(19) . . ? N2A C6A C7A 124.18(16) . . ? C6A C7A C3A 118.99(19) . . ? C1B N1B C2B 119.91(10) . . ? O1B C1B N1B 122.31(7) . . ? O1B C1B N1B 122.31(7) . 2_665 ? N1B C1B N1B 115.37(15) . 2_665 ? C5B N2B C6B 116.32(17) . . ? N1B C2B C3B 115.31(14) . . ? C4B C3B C7B 117.31(16) . . ? C4B C3B C2B 118.76(16) . . ? C7B C3B C2B 123.93(14) . . ? C5B C4B C3B 119.1(2) . . ? N2B C5B C4B 124.36(18) . . ? N2B C6B C7B 123.41(19) . . ? C3B C7B C6B 119.46(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2A N1A C1A O1A 4.92(17) . . . . ? C2A N1A C1A N1A -175.08(17) . . . 2_565 ? C1A N1A C2A C3A -73.95(17) . . . . ? N1A C2A C3A C4A -8.87(19) . . . . ? N1A C2A C3A C7A 171.30(13) . . . . ? C7A C3A C4A C5A -0.5(2) . . . . ? C2A C3A C4A C5A 179.71(14) . . . . ? C6A N2A C5A C4A -0.3(2) . . . . ? C3A C4A C5A N2A 0.8(3) . . . . ? C5A N2A C6A C7A -0.6(3) . . . . ? N2A C6A C7A C3A 0.9(3) . . . . ? C4A C3A C7A C6A -0.3(2) . . . . ? C2A C3A C7A C6A 179.50(14) . . . . ? C2B N1B C1B O1B -10.67(16) . . . . ? C2B N1B C1B N1B 169.33(16) . . . 2_665 ? C1B N1B C2B C3B 77.65(17) . . . . ? N1B C2B C3B C4B -171.10(14) . . . . ? N1B C2B C3B C7B 9.1(2) . . . . ? C7B C3B C4B C5B 0.2(2) . . . . ? C2B C3B C4B C5B -179.64(16) . . . . ? C6B N2B C5B C4B 0.7(3) . . . . ? C3B C4B C5B N2B -0.8(3) . . . . ? C5B N2B C6B C7B 0.1(3) . . . . ? C4B C3B C7B C6B 0.5(2) . . . . ? C2B C3B C7B C6B -179.66(15) . . . . ? N2B C6B C7B C3B -0.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.781 _diffrn_reflns_theta_full 36.45 _diffrn_measured_fraction_theta_full 0.781 _refine_diff_density_max 0.488 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.081 #===END data_L1bjtc307p21212 _database_code_depnum_ccdc_archive 'CCDC 624780' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H16 N4 O2' _chemical_formula_weight 260.30 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 10.5821(18) _cell_length_b 13.149(3) _cell_length_c 4.5942(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 639.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6863 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 37.12 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 276 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.792707 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11047 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 3.65 _diffrn_reflns_theta_max 37.24 _reflns_number_total 3252 _reflns_number_gt 2989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.0898P)^2^+0.4018P] 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 noref _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(2) _refine_ls_number_reflns 3252 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0712 _refine_ls_wR_factor_ref 0.2063 _refine_ls_wR_factor_gt 0.2021 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 O1 O 0.0000 0.5000 0.1967(3) 0.0211(3) Uani 1 2 d S . . C1 C 0.0000 0.5000 0.4695(4) 0.0166(3) Uani 1 2 d S . . N1 N 0.10070(13) 0.53473(13) 0.6263(3) 0.0225(3) Uani 1 1 d . . . H1A H 0.0975 0.5342 0.8177 0.027 Uiso 1 1 calc R . . C2 C 0.21325(14) 0.57254(14) 0.4803(3) 0.0206(3) Uani 1 1 d . . . H2A H 0.2356 0.5257 0.3255 0.025 Uiso 1 1 d R . . H2B H 0.2824 0.5732 0.6188 0.025 Uiso 1 1 d R . . N2 N 0.1761(2) 0.87487(16) 0.1121(5) 0.0372(4) Uani 1 1 d . . . C3 C 0.19911(13) 0.67833(13) 0.3525(3) 0.0193(3) Uani 1 1 d . . . C4 C 0.28963(15) 0.71628(12) 0.1593(4) 0.0212(3) Uani 1 1 d . . . H4 H 0.3606 0.6761 0.1063 0.025 Uiso 1 1 calc R . . C5 C 0.2743(2) 0.81413(16) 0.0449(5) 0.0298(4) Uani 1 1 d . . . H5 H 0.3363 0.8390 -0.0867 0.036 Uiso 1 1 calc R . . C6 C 0.0915(2) 0.83848(19) 0.3032(6) 0.0396(5) Uani 1 1 d . . . H6 H 0.0233 0.8813 0.3583 0.048 Uiso 1 1 calc R . . C7 C 0.09757(18) 0.74207(17) 0.4251(5) 0.0317(4) Uani 1 1 d . . . H7 H 0.0339 0.7195 0.5559 0.038 Uiso 1 1 calc R . . O1W O 0.0000 1.0000 -0.2136(8) 0.0566(8) Uani 1 2 d S . . H1W H 0.0582 0.9624 -0.1105 0.085 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0237(7) 0.0332(9) 0.0063(5) 0.000 0.000 -0.0041(6) C1 0.0168(7) 0.0255(9) 0.0076(6) 0.000 0.000 -0.0037(6) N1 0.0195(5) 0.0401(8) 0.0079(4) -0.0002(4) 0.0000(4) -0.0101(5) C2 0.0170(5) 0.0284(7) 0.0164(5) 0.0003(5) 0.0009(4) -0.0038(5) N2 0.0405(9) 0.0305(8) 0.0406(10) -0.0100(7) -0.0177(8) 0.0075(7) C3 0.0154(5) 0.0270(7) 0.0153(5) -0.0054(5) -0.0004(4) -0.0009(4) C4 0.0207(5) 0.0232(6) 0.0198(6) -0.0012(5) 0.0008(5) -0.0002(5) C5 0.0344(9) 0.0274(8) 0.0278(8) 0.0005(7) -0.0017(7) 0.0005(7) C6 0.0273(8) 0.0392(11) 0.0524(13) -0.0215(10) -0.0094(9) 0.0109(8) C7 0.0197(6) 0.0401(10) 0.0353(9) -0.0136(8) 0.0028(6) 0.0020(6) O1W 0.0554(17) 0.0591(19) 0.0552(18) 0.000 0.000 0.0188(15) _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 O1 C1 1.253(2) . ? C1 N1 1.3649(16) . ? C1 N1 1.3650(15) 2_565 ? N1 C2 1.455(2) . ? C2 C3 1.517(2) . ? N2 C6 1.342(4) . ? N2 C5 1.347(3) . ? C3 C4 1.398(2) . ? C3 C7 1.403(2) . ? C4 C5 1.399(3) . ? C6 C7 1.387(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 O1 C1 N1 121.85(8) . . ? O1 C1 N1 121.85(8) . 2_565 ? N1 C1 N1 116.29(15) . 2_565 ? C1 N1 C2 120.68(12) . . ? N1 C2 C3 114.28(14) . . ? C6 N2 C5 117.0(2) . . ? C4 C3 C7 117.55(16) . . ? C4 C3 C2 120.35(13) . . ? C7 C3 C2 122.09(15) . . ? C3 C4 C5 119.16(16) . . ? N2 C5 C4 123.3(2) . . ? N2 C6 C7 123.97(18) . . ? C6 C7 C3 119.05(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 N1 C2 -0.55(19) . . . . ? N1 C1 N1 C2 179.45(19) 2_565 . . . ? C1 N1 C2 C3 76.40(18) . . . . ? N1 C2 C3 C4 -167.55(13) . . . . ? N1 C2 C3 C7 13.5(2) . . . . ? C7 C3 C4 C5 -1.0(2) . . . . ? C2 C3 C4 C5 -179.93(16) . . . . ? C6 N2 C5 C4 1.3(3) . . . . ? C3 C4 C5 N2 0.2(3) . . . . ? C5 N2 C6 C7 -2.2(3) . . . . ? N2 C6 C7 C3 1.5(3) . . . . ? C4 C3 C7 C6 0.1(3) . . . . ? C2 C3 C7 C6 179.10(17) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 37.24 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.419 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.088 #===END data_pd221_0m _database_code_depnum_ccdc_archive 'CCDC 624781' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H90 F12 N8 O15.25 P4 Pd2 S4' _chemical_formula_weight 2196.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 18.6063(11) _cell_length_b 21.5364(13) _cell_length_c 27.1103(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10863.4(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8397 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 32.09 _exptl_crystal_description Needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 0.546 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.616631 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 160178 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.0481 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 33.18 _reflns_number_total 41344 _reflns_number_gt 32844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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 triflate anions refined are partially disordered. Also the isopropanol molecules localized are disordered or have a partial occupation. Distances and thermical displacement parameters for these anions/solvent molecules are in some cases restrained. After final refinement there are residual voids which probably contain highly disordered isopropanol molecules. The detected highest peak and deepest hole of the electron densities are localized close to one of the disordered sulfur atoms belonging to a triflate anion and could not be improved. The structure refined as a racemic twin 53:47. ; _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^)+(0.1383P)^2^+22.3850P] 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 noref _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 0.48(3) _refine_ls_number_reflns 41344 _refine_ls_number_parameters 1229 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.1067 _refine_ls_R_factor_gt 0.0854 _refine_ls_wR_factor_ref 0.2552 _refine_ls_wR_factor_gt 0.2381 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.123 _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 Pd1 Pd 0.50052(2) 0.165924(16) 0.204547(14) 0.03097(8) Uani 1 1 d . . . P1 P 0.54896(7) 0.16053(6) 0.12778(5) 0.0305(2) Uani 1 1 d . . . N1 N 0.4534(3) 0.25267(19) 0.18876(17) 0.0308(8) Uani 1 1 d . . . C1 C 0.3852(3) 0.2555(2) 0.1728(2) 0.0351(11) Uani 1 1 d . . . H1 H 0.3598 0.2178 0.1673 0.042 Uiso 1 1 calc R . . O1 O 0.2084(3) 0.4217(2) 0.20254(19) 0.0447(10) Uani 1 1 d . . . Pd2 Pd -0.02246(2) 0.157089(16) 0.215207(14) 0.02966(8) Uani 1 1 d . . . C2 C 0.3505(3) 0.3111(2) 0.1641(2) 0.0361(11) Uani 1 1 d . . . H2 H 0.3025 0.3111 0.1522 0.043 Uiso 1 1 calc R . . N2 N 0.2866(3) 0.4283(2) 0.1376(2) 0.0379(10) Uani 1 1 d . . . H2A H 0.2907 0.4308 0.1053 0.046 Uiso 1 1 calc R . . P2 P 0.55035(8) 0.07300(6) 0.22574(5) 0.0326(3) Uani 1 1 d . . . O2 O 0.2651(5) 0.2593(3) 0.4213(3) 0.080(2) Uani 1 1 d . . . C3 C 0.3855(3) 0.3667(2) 0.1727(2) 0.0293(9) Uani 1 1 d . . . N3 N 0.1651(3) 0.4203(2) 0.1241(2) 0.0375(10) Uani 1 1 d . . . H3A H 0.1748 0.4183 0.0924 0.045 Uiso 1 1 calc R . . P3 P -0.07908(8) 0.13623(6) 0.14272(5) 0.0292(2) Uani 1 1 d . . . C4 C 0.4570(3) 0.3630(3) 0.1898(2) 0.0377(11) Uani 1 1 d . . . H4 H 0.4835 0.3999 0.1960 0.045 Uiso 1 1 calc R . . N4 N 0.0132(3) 0.24255(19) 0.18814(16) 0.0324(9) Uani 1 1 d . . . P4 P -0.06007(8) 0.06517(6) 0.24741(5) 0.0313(3) Uani 1 1 d . . . N5 N 0.0294(3) 0.18186(18) 0.28156(18) 0.0343(9) Uani 1 1 d . . . C5 C 0.4884(3) 0.3061(2) 0.1973(2) 0.0377(11) Uani 1 1 d . . . H5 H 0.5366 0.3044 0.2089 0.045 Uiso 1 1 calc R . . C6 C 0.3507(3) 0.4289(2) 0.1667(3) 0.0379(12) Uani 1 1 d . . . H6A H 0.3389 0.4455 0.1998 0.045 Uiso 1 1 calc R . . H6B H 0.3856 0.4576 0.1513 0.045 Uiso 1 1 calc R . . N6 N 0.1942(4) 0.1753(3) 0.4300(2) 0.0493(13) Uani 1 1 d . . . H6C H 0.1919 0.1352 0.4360 0.059 Uiso 1 1 calc R . . C7 C 0.2202(3) 0.4242(2) 0.1573(2) 0.0360(11) Uani 1 1 d . . . N7 N 0.3151(4) 0.1636(4) 0.4351(2) 0.0577(15) Uani 1 1 d . . . H7A H 0.3076 0.1254 0.4455 0.069 Uiso 1 1 calc R . . C8 C 0.0910(3) 0.4196(2) 0.1405(3) 0.0373(12) Uani 1 1 d . . . H8A H 0.0601 0.4349 0.1134 0.045 Uiso 1 1 calc R . . H8B H 0.0857 0.4485 0.1686 0.045 Uiso 1 1 calc R . . N8 N 0.4592(3) 0.1780(2) 0.27625(19) 0.0398(10) Uani 1 1 d . . . C9 C 0.0651(3) 0.3570(2) 0.1559(2) 0.0299(9) Uani 1 1 d . . . C10 C 0.1079(3) 0.3032(2) 0.1546(2) 0.0351(11) Uani 1 1 d . . . H10 H 0.1555 0.3050 0.1420 0.042 Uiso 1 1 calc R . . C11 C 0.0801(3) 0.2479(2) 0.1718(2) 0.0345(10) Uani 1 1 d . . . H11 H 0.1101 0.2122 0.1719 0.041 Uiso 1 1 calc R . . C12 C -0.0296(3) 0.2935(3) 0.1892(2) 0.0348(10) Uani 1 1 d . . . H12 H -0.0774 0.2898 0.2013 0.042 Uiso 1 1 calc R . . C13 C -0.0054(3) 0.3506(2) 0.1732(2) 0.0336(9) Uani 1 1 d . . . H13 H -0.0365 0.3855 0.1739 0.040 Uiso 1 1 calc R . . C14 C 0.0994(3) 0.1709(2) 0.2880(2) 0.0370(10) Uani 1 1 d . . . H14 H 0.1266 0.1562 0.2608 0.044 Uiso 1 1 calc R . . C15 C 0.1339(4) 0.1799(3) 0.3322(2) 0.0399(12) Uani 1 1 d . . . H15 H 0.1838 0.1712 0.3353 0.048 Uiso 1 1 calc R . . C16 C 0.0942(4) 0.2022(3) 0.3729(2) 0.0417(13) Uani 1 1 d . . . C17 C 0.0231(4) 0.2157(3) 0.3650(2) 0.0413(12) Uani 1 1 d . . . H17 H -0.0047 0.2326 0.3912 0.050 Uiso 1 1 calc R . . C18 C -0.0091(4) 0.2051(2) 0.3191(2) 0.0384(12) Uani 1 1 d . . . H18 H -0.0586 0.2144 0.3145 0.046 Uiso 1 1 calc R . . C19 C 0.1281(5) 0.2092(4) 0.4226(3) 0.0547(19) Uani 1 1 d . . . H19A H 0.1378 0.2539 0.4283 0.066 Uiso 1 1 calc R . . H19B H 0.0931 0.1956 0.4478 0.066 Uiso 1 1 calc R . . C20 C 0.2586(5) 0.2025(3) 0.4279(2) 0.0512(17) Uani 1 1 d . . . C21 C 0.3870(6) 0.1845(7) 0.4259(3) 0.081(3) Uani 1 1 d . . . H21A H 0.4205 0.1574 0.4444 0.097 Uiso 1 1 calc R . . H21B H 0.3920 0.2270 0.4393 0.097 Uiso 1 1 calc R . . C22 C 0.4100(4) 0.1854(4) 0.3726(3) 0.0545(17) Uani 1 1 d . . . C23 C 0.3673(4) 0.1608(4) 0.3352(2) 0.0493(15) Uani 1 1 d . . . H23 H 0.3207 0.1454 0.3426 0.059 Uiso 1 1 calc R . . C24 C 0.3925(3) 0.1590(3) 0.2876(2) 0.0418(11) Uani 1 1 d . . . H24 H 0.3620 0.1439 0.2622 0.050 Uiso 1 1 calc R . . C25 C 0.5009(4) 0.2030(3) 0.3118(2) 0.0444(13) Uani 1 1 d . . . H25 H 0.5475 0.2178 0.3036 0.053 Uiso 1 1 calc R . . C26 C 0.4771(5) 0.2073(4) 0.3599(3) 0.0528(16) Uani 1 1 d . . . H26 H 0.5071 0.2254 0.3843 0.063 Uiso 1 1 calc R . . C27 C 0.6393(3) 0.1296(3) 0.1269(3) 0.0398(12) Uani 1 1 d . . . H27A H 0.6579 0.1309 0.0927 0.048 Uiso 1 1 calc R . . H27B H 0.6707 0.1563 0.1474 0.048 Uiso 1 1 calc R . . C28 C 0.6434(3) 0.0635(3) 0.1458(2) 0.0381(11) Uani 1 1 d . . . H28A H 0.6887 0.0443 0.1342 0.046 Uiso 1 1 calc R . . H28B H 0.6030 0.0393 0.1318 0.046 Uiso 1 1 calc R . . C29 C 0.6403(3) 0.0599(2) 0.2028(2) 0.0372(11) Uani 1 1 d . . . H29A H 0.6731 0.0913 0.2170 0.045 Uiso 1 1 calc R . . H29B H 0.6570 0.0184 0.2136 0.045 Uiso 1 1 calc R . . C30 C 0.4993(4) 0.1131(2) 0.0839(2) 0.0349(10) Uani 1 1 d . . . C31 C 0.5309(5) 0.0946(3) 0.0401(3) 0.0471(14) Uani 1 1 d . . . H31 H 0.5786 0.1075 0.0329 0.056 Uiso 1 1 calc R . . C32 C 0.4955(5) 0.0584(3) 0.0070(3) 0.0530(16) Uani 1 1 d . . . H32 H 0.5190 0.0461 -0.0226 0.064 Uiso 1 1 calc R . . C33 C 0.4272(6) 0.0397(4) 0.0156(3) 0.061(2) Uani 1 1 d . . . H33 H 0.4022 0.0156 -0.0082 0.073 Uiso 1 1 calc R . . C34 C 0.3934(5) 0.0566(5) 0.0608(4) 0.075(3) Uani 1 1 d . . . H34 H 0.3462 0.0425 0.0681 0.089 Uiso 1 1 calc R . . C35 C 0.4299(5) 0.0938(4) 0.0939(3) 0.060(2) Uani 1 1 d . . . H35 H 0.4073 0.1061 0.1237 0.073 Uiso 1 1 calc R . . C36 C 0.5566(4) 0.2378(2) 0.1016(2) 0.0360(11) Uani 1 1 d . . . C37 C 0.5017(4) 0.2605(3) 0.0719(2) 0.0444(13) Uani 1 1 d . . . H37 H 0.4622 0.2346 0.0635 0.053 Uiso 1 1 calc R . . C38 C 0.5050(6) 0.3216(3) 0.0544(3) 0.059(2) Uani 1 1 d . . . H38 H 0.4665 0.3381 0.0355 0.071 Uiso 1 1 calc R . . C39 C 0.5649(5) 0.3581(4) 0.0648(4) 0.065(2) Uani 1 1 d . . . H39 H 0.5689 0.3985 0.0510 0.078 Uiso 1 1 calc R . . C40 C 0.6195(5) 0.3352(3) 0.0960(5) 0.073(3) Uani 1 1 d . . . H40 H 0.6589 0.3609 0.1051 0.088 Uiso 1 1 calc R . . C41 C 0.6149(4) 0.2741(3) 0.1133(3) 0.0497(16) Uani 1 1 d . . . H41 H 0.6522 0.2577 0.1333 0.060 Uiso 1 1 calc R . . C42 C 0.5578(3) 0.0670(2) 0.2920(2) 0.0373(11) Uani 1 1 d . . . C43 C 0.5010(4) 0.0421(3) 0.3199(2) 0.0400(11) Uani 1 1 d . . . H43 H 0.4604 0.0250 0.3036 0.048 Uiso 1 1 calc R . . C44 C 0.5035(5) 0.0421(3) 0.3714(3) 0.0544(17) Uani 1 1 d . . . H44 H 0.4643 0.0266 0.3901 0.065 Uiso 1 1 calc R . . C45 C 0.5656(5) 0.0655(3) 0.3951(3) 0.0527(18) Uani 1 1 d . . . H45 H 0.5686 0.0650 0.4301 0.063 Uiso 1 1 calc R . . C46 C 0.6218(5) 0.0889(3) 0.3678(3) 0.0497(16) Uani 1 1 d . . . H46 H 0.6635 0.1039 0.3842 0.060 Uiso 1 1 calc R . . C47 C 0.6181(4) 0.0908(3) 0.3167(3) 0.0421(13) Uani 1 1 d . . . H47 H 0.6566 0.1084 0.2983 0.050 Uiso 1 1 calc R . . C48 C 0.4975(4) 0.0067(2) 0.2063(2) 0.0391(11) Uani 1 1 d . . . C49 C 0.5305(4) -0.0516(3) 0.1994(3) 0.0500(16) Uani 1 1 d . . . H49 H 0.5808 -0.0566 0.2042 0.060 Uiso 1 1 calc R . . C50 C 0.4874(6) -0.1022(4) 0.1854(4) 0.073(3) Uani 1 1 d . . . H50 H 0.5093 -0.1415 0.1802 0.088 Uiso 1 1 calc R . . C51 C 0.4158(6) -0.0965(4) 0.1791(4) 0.075(3) Uani 1 1 d . . . H51 H 0.3881 -0.1314 0.1691 0.089 Uiso 1 1 calc R . . C52 C 0.3838(6) -0.0414(4) 0.1870(5) 0.078(3) Uani 1 1 d . . . H52 H 0.3329 -0.0381 0.1847 0.094 Uiso 1 1 calc R . . C53 C 0.4248(5) 0.0108(3) 0.1984(4) 0.068(3) Uani 1 1 d . . . H53 H 0.4019 0.0501 0.2007 0.081 Uiso 1 1 calc R . . C54 C -0.1660(3) 0.1005(2) 0.1499(2) 0.0331(10) Uani 1 1 d . . . H54A H -0.1977 0.1294 0.1682 0.040 Uiso 1 1 calc R . . H54B H -0.1873 0.0942 0.1168 0.040 Uiso 1 1 calc R . . C55 C -0.1646(3) 0.0378(2) 0.1770(2) 0.0337(10) Uani 1 1 d . . . H55A H -0.1256 0.0117 0.1634 0.040 Uiso 1 1 calc R . . H55B H -0.2107 0.0159 0.1716 0.040 Uiso 1 1 calc R . . C56 C -0.1526(3) 0.0470(3) 0.2327(2) 0.0365(11) Uani 1 1 d . . . H56A H -0.1667 0.0086 0.2503 0.044 Uiso 1 1 calc R . . H56B H -0.1839 0.0810 0.2446 0.044 Uiso 1 1 calc R . . C57 C -0.0297(3) 0.0882(2) 0.1003(2) 0.0326(10) Uani 1 1 d . . . C58 C -0.0631(4) 0.0692(3) 0.0569(2) 0.0399(12) Uani 1 1 d . . . H58 H -0.1118 0.0803 0.0511 0.048 Uiso 1 1 calc R . . C59 C -0.0260(4) 0.0342(3) 0.0218(3) 0.0489(15) Uani 1 1 d . . . H59 H -0.0489 0.0215 -0.0079 0.059 Uiso 1 1 calc R . . C60 C 0.0455(5) 0.0185(3) 0.0313(3) 0.0536(18) Uani 1 1 d . . . H60 H 0.0721 -0.0038 0.0072 0.064 Uiso 1 1 calc R . . C61 C 0.0783(5) 0.0349(4) 0.0755(3) 0.060(2) Uani 1 1 d . . . H61 H 0.1257 0.0211 0.0827 0.072 Uiso 1 1 calc R . . C62 C 0.0409(4) 0.0719(3) 0.1092(3) 0.0461(14) Uani 1 1 d . . . H62 H 0.0641 0.0859 0.1384 0.055 Uiso 1 1 calc R . . C63 C -0.0962(3) 0.2074(2) 0.1085(2) 0.0337(10) Uani 1 1 d . . . C64 C -0.0457(4) 0.2296(3) 0.0760(2) 0.0410(13) Uani 1 1 d . . . H64 H -0.0037 0.2058 0.0695 0.049 Uiso 1 1 calc R . . C65 C -0.0553(5) 0.2866(3) 0.0527(2) 0.0507(17) Uani 1 1 d . . . H65 H -0.0197 0.3023 0.0309 0.061 Uiso 1 1 calc R . . C66 C -0.1182(5) 0.3204(3) 0.0617(3) 0.0537(18) Uani 1 1 d . . . H66 H -0.1261 0.3584 0.0448 0.064 Uiso 1 1 calc R . . C67 C -0.1701(5) 0.2987(3) 0.0957(3) 0.0530(17) Uani 1 1 d . . . H67 H -0.2119 0.3225 0.1027 0.064 Uiso 1 1 calc R . . C68 C -0.1584(4) 0.2413(3) 0.1186(3) 0.0432(13) Uani 1 1 d . . . H68 H -0.1930 0.2254 0.1411 0.052 Uiso 1 1 calc R . . C69 C -0.0072(4) -0.0019(2) 0.2293(2) 0.0409(13) Uani 1 1 d . . . C70 C -0.0411(4) -0.0607(3) 0.2247(2) 0.0432(14) Uani 1 1 d . . . H70 H -0.0906 -0.0656 0.2323 0.052 Uiso 1 1 calc R . . C71 C -0.0001(6) -0.1109(3) 0.2089(3) 0.064(2) Uani 1 1 d . . . H71 H -0.0224 -0.1501 0.2044 0.076 Uiso 1 1 calc R . . C72 C 0.0740(6) -0.1043(4) 0.1995(4) 0.070(3) Uani 1 1 d . . . H72 H 0.1014 -0.1388 0.1883 0.084 Uiso 1 1 calc R . . C73 C 0.1070(6) -0.0464(5) 0.2068(5) 0.078(3) Uani 1 1 d . . . H73 H 0.1574 -0.0418 0.2030 0.093 Uiso 1 1 calc R . . C74 C 0.0650(5) 0.0034(3) 0.2195(4) 0.064(2) Uani 1 1 d . . . H74 H 0.0867 0.0433 0.2215 0.077 Uiso 1 1 calc R . . C75 C -0.0556(4) 0.0666(3) 0.3137(2) 0.0393(12) Uani 1 1 d . . . C76 C -0.1159(4) 0.0855(3) 0.3428(3) 0.0475(14) Uani 1 1 d . . . H76 H -0.1598 0.0967 0.3273 0.057 Uiso 1 1 calc R . . C77 C -0.1101(5) 0.0873(4) 0.3937(3) 0.059(2) Uani 1 1 d . . . H77 H -0.1508 0.0985 0.4129 0.071 Uiso 1 1 calc R . . C78 C -0.0473(6) 0.0734(4) 0.4167(3) 0.060(2) Uani 1 1 d . . . H78 H -0.0447 0.0757 0.4516 0.072 Uiso 1 1 calc R . . C79 C 0.0136(5) 0.0558(3) 0.3901(3) 0.0513(17) Uani 1 1 d . . . H79 H 0.0575 0.0467 0.4065 0.062 Uiso 1 1 calc R . . C80 C 0.0086(4) 0.0519(2) 0.3378(2) 0.0425(13) Uani 1 1 d . . . H80 H 0.0492 0.0392 0.3192 0.051 Uiso 1 1 calc R . . S1B S -0.23582(12) 0.22401(9) 0.26318(8) 0.0558(5) Uani 1 1 d . A 1 F1B F -0.2457(4) 0.3451(3) 0.2821(4) 0.118(3) Uani 1 1 d . A 1 O1B O -0.1603(3) 0.2307(3) 0.2572(3) 0.0719(19) Uani 1 1 d . A 1 C1B C -0.2686(6) 0.3045(6) 0.2498(5) 0.087(4) Uani 1 1 d . A 1 F2B F -0.2472(6) 0.3223(4) 0.2089(4) 0.132(4) Uani 1 1 d . A 1 O2B O -0.2716(4) 0.1928(3) 0.2235(3) 0.084(2) Uani 1 1 d . A 1 O3B O -0.2597(7) 0.2108(6) 0.3125(3) 0.134(5) Uani 1 1 d . A 1 F3B F -0.3402(4) 0.3016(6) 0.2544(5) 0.194(7) Uani 1 1 d . A 1 S1A S 0.23870(13) 0.10411(10) 0.16063(11) 0.0646(6) Uani 1 1 d . B 1 O1A O 0.1736(3) 0.1170(3) 0.1874(2) 0.0507(11) Uani 1 1 d . B 1 F1A F 0.1714(4) 0.1560(4) 0.0851(3) 0.092(2) Uani 1 1 d . B 1 C1A C 0.2316(5) 0.1572(4) 0.1091(4) 0.0623(19) Uani 1 1 d . B 1 F2A F 0.2870(4) 0.1575(4) 0.0792(3) 0.104(3) Uani 1 1 d . B 1 O2A O 0.2400(5) 0.0430(4) 0.1381(4) 0.090(3) Uani 1 1 d . B 1 O3A O 0.3055(3) 0.1210(2) 0.1831(2) 0.0534(12) Uani 1 1 d . B 1 F3A F 0.2348(4) 0.2172(3) 0.1224(3) 0.092(2) Uani 1 1 d . B 1 S1C S 0.25087(15) -0.00126(10) 0.41799(15) 0.0853(10) Uani 1 1 d . . . O1C O 0.1921(4) 0.0396(3) 0.4332(4) 0.094(3) Uani 1 1 d . . . F1C F 0.2362(6) 0.0453(4) 0.3317(5) 0.151(5) Uani 1 1 d . . . C1C C 0.2352(11) -0.0108(6) 0.3529(7) 0.116(6) Uani 1 1 d . . . O2C O 0.3197(4) 0.0309(4) 0.4217(4) 0.099(3) Uani 1 1 d . . . F2C F 0.2859(7) -0.0450(4) 0.3327(4) 0.143(4) Uani 1 1 d . . . O3C O 0.2481(5) -0.0641(4) 0.4384(6) 0.136(5) Uani 1 1 d . . . F3C F 0.1721(6) -0.0377(4) 0.3435(5) 0.139(4) Uani 1 1 d . . . S1D S 0.24677(18) 0.4208(3) 0.00360(11) 0.1522(17) Uani 1 1 d DU C 1 O1D O 0.2520(4) 0.4265(5) -0.04896(16) 0.091(2) Uani 1 1 d DU C 1 F1D F 0.2101(7) 0.2983(7) -0.0152(4) 0.178(5) Uani 1 1 d DU C 1 C1D C 0.2529(7) 0.3345(4) 0.0114(4) 0.158(8) Uani 1 1 d DU C 1 O2D O 0.3042(3) 0.4474(4) 0.0325(2) 0.084(2) Uani 1 1 d DU C 1 F2D F 0.2442(6) 0.3141(6) 0.0571(4) 0.150(4) Uani 1 1 d DU C 1 O3D O 0.1757(3) 0.4341(5) 0.0233(3) 0.093(2) Uani 1 1 d DU C 1 F3D F 0.3193(7) 0.3186(9) 0.0002(6) 0.234(8) Uani 1 1 d DU C 1 O1L2 O 0.0050(11) 0.2910(7) 0.4773(7) 0.045(4) Uani 0.25 1 d PDU . . H1LD H -0.0209 0.2813 0.5015 0.067 Uiso 0.25 1 calc PR . . C2L2 C -0.0805(14) 0.3470(16) 0.4400(12) 0.056(6) Uani 0.25 1 d PDU . . H2LD H -0.1154 0.3315 0.4641 0.083 Uiso 0.25 1 calc PR . . H2LE H -0.0764 0.3173 0.4127 0.083 Uiso 0.25 1 calc PR . . H2LF H -0.0967 0.3872 0.4272 0.083 Uiso 0.25 1 calc PR . . C3L2 C 0.0401(12) 0.3787(11) 0.4224(8) 0.075(5) Uani 0.50 1 d PDU . . H3LD H 0.0902 0.3817 0.4333 0.112 Uiso 0.25 1 calc PR . . H3LE H 0.0231 0.4198 0.4121 0.112 Uiso 0.25 1 calc PR . . H3LF H 0.0369 0.3499 0.3945 0.112 Uiso 0.25 1 calc PR . . C1L2 C -0.0068(12) 0.3547(8) 0.4650(9) 0.056(7) Uani 0.25 1 d PDU . . H1LC H -0.0077 0.3830 0.4943 0.067 Uiso 0.25 1 calc PR . . O1L O 0.2869(3) 0.4202(2) 0.2885(2) 0.0537(12) Uani 1 1 d . . . H1LF H 0.3086 0.4088 0.2629 0.081 Uiso 1 1 calc R . . C1L C 0.2733(5) 0.3691(4) 0.3182(4) 0.062(2) Uani 1 1 d . . . H1LE H 0.2973 0.3748 0.3509 0.075 Uiso 1 1 calc R . . C2L C 0.1926(7) 0.3543(5) 0.3261(6) 0.098(5) Uani 1 1 d . . . H2LG H 0.1664 0.3929 0.3327 0.148 Uiso 1 1 calc R . . H2LH H 0.1873 0.3261 0.3542 0.148 Uiso 1 1 calc R . . H2LI H 0.1732 0.3346 0.2964 0.148 Uiso 1 1 calc R . . C3L C 0.3041(8) 0.3097(5) 0.2921(6) 0.103(4) Uani 1 1 d U . . H3LG H 0.3539 0.3173 0.2820 0.155 Uiso 1 1 calc R . . H3LH H 0.2750 0.3001 0.2630 0.155 Uiso 1 1 calc R . . H3LI H 0.3026 0.2746 0.3151 0.155 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.03379(17) 0.02579(14) 0.03332(17) 0.00537(11) -0.00380(14) 0.00073(13) P1 0.0322(6) 0.0242(5) 0.0350(6) 0.0048(5) -0.0038(5) 0.0001(5) N1 0.033(2) 0.0243(16) 0.035(2) 0.0010(15) -0.0048(16) 0.0016(15) C1 0.035(3) 0.0202(18) 0.050(3) 0.0020(18) -0.002(2) -0.0024(17) O1 0.042(2) 0.042(2) 0.050(3) -0.0038(19) -0.001(2) 0.0014(17) Pd2 0.03489(17) 0.02518(14) 0.02890(15) 0.00161(12) 0.00011(13) -0.00418(12) C2 0.029(2) 0.024(2) 0.055(3) 0.000(2) -0.007(2) -0.0051(17) N2 0.032(2) 0.0274(19) 0.054(3) 0.0022(18) -0.004(2) 0.0028(16) P2 0.0378(7) 0.0239(5) 0.0361(7) 0.0067(4) -0.0069(5) -0.0002(4) O2 0.110(6) 0.047(3) 0.083(5) 0.003(3) -0.024(4) -0.013(4) C3 0.028(2) 0.0259(19) 0.034(2) -0.0016(16) -0.0030(18) 0.0022(16) N3 0.036(2) 0.0283(19) 0.048(3) 0.0063(18) -0.003(2) -0.0027(16) P3 0.0375(7) 0.0208(5) 0.0293(6) -0.0003(4) 0.0000(5) -0.0011(4) C4 0.035(3) 0.028(2) 0.050(3) -0.009(2) -0.009(2) -0.0041(18) N4 0.041(3) 0.0248(16) 0.0314(19) -0.0005(14) 0.0009(17) 0.0013(15) P4 0.0375(7) 0.0246(5) 0.0319(6) 0.0036(4) -0.0012(5) -0.0043(5) N5 0.044(2) 0.0221(15) 0.037(2) 0.0029(15) 0.002(2) -0.0082(15) C5 0.033(3) 0.029(2) 0.051(3) -0.0017(19) -0.010(2) 0.0019(17) C6 0.029(2) 0.0219(19) 0.063(4) -0.003(2) -0.007(2) -0.0001(16) N6 0.064(4) 0.039(3) 0.045(3) 0.004(2) -0.014(3) 0.001(2) C7 0.036(3) 0.0151(16) 0.057(3) 0.0027(18) -0.003(2) 0.0000(16) N7 0.067(4) 0.067(4) 0.039(3) 0.005(3) 0.004(3) -0.004(4) C8 0.032(2) 0.0192(18) 0.061(4) 0.002(2) -0.003(2) 0.0000(16) N8 0.046(3) 0.038(2) 0.036(2) 0.0036(18) -0.0005(19) 0.0056(19) C9 0.033(2) 0.0216(17) 0.035(2) -0.0014(15) -0.0039(19) 0.0017(15) C10 0.031(2) 0.0235(19) 0.050(3) 0.0060(19) 0.005(2) 0.0064(17) C11 0.037(3) 0.0191(17) 0.048(3) 0.0035(18) -0.004(2) 0.0031(17) C12 0.032(2) 0.035(2) 0.038(2) -0.0074(19) 0.002(2) 0.0029(19) C13 0.030(2) 0.0247(18) 0.046(3) -0.0039(17) -0.001(2) 0.0006(16) C14 0.045(3) 0.032(2) 0.034(2) -0.0043(19) 0.001(2) -0.0047(19) C15 0.048(3) 0.032(2) 0.040(3) -0.004(2) -0.004(2) 0.000(2) C16 0.060(4) 0.027(2) 0.039(3) -0.002(2) -0.009(3) -0.003(2) C17 0.053(3) 0.036(2) 0.034(3) -0.0005(19) 0.004(2) -0.004(2) C18 0.049(3) 0.028(2) 0.038(3) -0.0006(18) -0.003(2) -0.005(2) C19 0.080(5) 0.045(3) 0.040(3) -0.009(3) -0.018(3) 0.011(3) C20 0.078(5) 0.047(3) 0.029(3) -0.005(2) -0.011(3) -0.008(3) C21 0.070(6) 0.131(10) 0.041(4) -0.003(5) -0.004(4) -0.023(6) C22 0.050(4) 0.074(5) 0.039(3) -0.002(3) -0.007(3) -0.001(3) C23 0.046(3) 0.068(4) 0.034(3) 0.007(3) -0.003(2) -0.005(3) C24 0.046(3) 0.041(3) 0.038(3) 0.004(2) 0.001(2) 0.004(2) C25 0.049(3) 0.037(2) 0.047(3) -0.001(2) -0.012(3) 0.006(3) C26 0.054(4) 0.064(4) 0.040(3) 0.006(3) -0.007(3) -0.001(3) C27 0.031(3) 0.039(3) 0.049(3) 0.015(2) -0.001(2) 0.004(2) C28 0.040(3) 0.033(2) 0.040(3) 0.011(2) -0.002(2) 0.008(2) C29 0.038(3) 0.0253(19) 0.049(3) 0.008(2) -0.003(2) 0.0021(17) C30 0.044(3) 0.0261(18) 0.035(2) 0.0010(16) -0.001(2) 0.003(2) C31 0.060(4) 0.035(3) 0.046(3) 0.001(2) 0.006(3) -0.001(3) C32 0.069(5) 0.043(3) 0.048(3) -0.007(2) 0.003(3) 0.003(3) C33 0.078(6) 0.046(4) 0.057(4) -0.011(3) -0.006(4) -0.010(4) C34 0.055(5) 0.077(6) 0.092(7) -0.039(5) 0.006(5) -0.027(4) C35 0.055(4) 0.072(5) 0.054(4) -0.025(4) 0.010(3) -0.025(4) C36 0.045(3) 0.026(2) 0.036(3) 0.0042(18) -0.003(2) -0.0017(19) C37 0.064(4) 0.031(2) 0.038(3) 0.0026(19) -0.014(3) 0.002(3) C38 0.097(6) 0.038(3) 0.043(3) 0.011(2) -0.010(4) 0.008(4) C39 0.071(5) 0.040(3) 0.083(6) 0.024(4) 0.009(5) -0.002(3) C40 0.053(4) 0.030(3) 0.138(9) 0.009(4) 0.006(5) -0.007(3) C41 0.037(3) 0.032(3) 0.081(5) 0.007(3) -0.003(3) -0.003(2) C42 0.047(3) 0.0235(18) 0.041(3) 0.0073(19) -0.010(2) 0.0032(18) C43 0.046(3) 0.033(2) 0.041(3) 0.0093(19) 0.000(3) 0.004(2) C44 0.071(5) 0.048(3) 0.044(3) 0.015(3) 0.009(3) 0.013(3) C45 0.083(6) 0.039(3) 0.037(3) 0.002(2) -0.004(3) 0.006(3) C46 0.063(4) 0.028(2) 0.058(4) 0.005(2) -0.018(3) -0.002(3) C47 0.051(4) 0.029(2) 0.046(3) 0.004(2) -0.009(3) -0.004(2) C48 0.050(3) 0.0235(18) 0.044(3) 0.0026(17) -0.009(3) -0.0029(19) C49 0.061(4) 0.025(2) 0.064(4) -0.004(2) -0.016(3) 0.001(2) C50 0.099(8) 0.038(3) 0.084(6) -0.007(3) -0.030(6) -0.014(4) C51 0.096(8) 0.054(4) 0.074(6) 0.000(4) -0.021(5) -0.031(5) C52 0.062(5) 0.051(4) 0.123(9) 0.000(5) -0.033(6) -0.020(4) C53 0.056(4) 0.031(3) 0.116(8) 0.006(4) -0.033(5) -0.007(3) C54 0.041(3) 0.028(2) 0.030(2) 0.0036(17) -0.004(2) -0.0001(18) C55 0.037(3) 0.026(2) 0.038(3) 0.0011(18) -0.005(2) -0.0057(18) C56 0.039(3) 0.033(2) 0.038(3) 0.0043(19) -0.001(2) -0.008(2) C57 0.042(3) 0.0216(18) 0.035(2) -0.0008(16) 0.001(2) -0.0002(18) C58 0.045(3) 0.036(3) 0.039(3) -0.007(2) 0.004(2) 0.001(2) C59 0.056(4) 0.044(3) 0.047(3) -0.014(3) 0.005(3) -0.004(3) C60 0.073(5) 0.038(3) 0.050(4) -0.011(3) 0.004(3) 0.014(3) C61 0.059(5) 0.056(4) 0.065(5) -0.013(4) -0.003(4) 0.019(4) C62 0.050(4) 0.043(3) 0.045(3) -0.008(2) -0.001(3) 0.004(3) C63 0.045(3) 0.027(2) 0.030(2) 0.0004(17) -0.002(2) 0.0007(19) C64 0.062(4) 0.026(2) 0.034(3) -0.0004(18) 0.005(3) -0.004(2) C65 0.083(5) 0.031(2) 0.037(3) 0.004(2) 0.003(3) -0.008(3) C66 0.074(5) 0.031(3) 0.056(4) 0.014(3) -0.009(4) -0.007(3) C67 0.057(4) 0.031(3) 0.071(5) 0.008(3) -0.008(4) 0.004(3) C68 0.045(3) 0.030(2) 0.055(4) 0.003(2) -0.006(3) 0.001(2) C69 0.060(4) 0.0256(19) 0.037(2) 0.0044(17) 0.002(3) 0.007(2) C70 0.066(4) 0.027(2) 0.037(3) -0.0002(19) -0.003(3) -0.003(2) C71 0.099(6) 0.033(3) 0.059(4) 0.002(3) -0.023(5) 0.018(3) C72 0.088(7) 0.057(4) 0.065(5) 0.019(4) 0.024(5) 0.027(4) C73 0.070(6) 0.067(5) 0.096(8) 0.026(5) 0.020(6) 0.020(4) C74 0.062(5) 0.038(3) 0.092(6) 0.017(4) 0.021(5) 0.017(3) C75 0.056(4) 0.030(2) 0.032(2) 0.0034(19) -0.005(2) -0.009(2) C76 0.052(4) 0.051(3) 0.040(3) 0.007(3) -0.002(3) -0.006(3) C77 0.071(5) 0.073(5) 0.034(3) -0.002(3) 0.008(3) -0.014(4) C78 0.088(6) 0.057(4) 0.034(3) 0.007(3) -0.006(3) -0.017(4) C79 0.067(5) 0.040(3) 0.047(3) 0.010(2) -0.011(3) -0.014(3) C80 0.049(4) 0.026(2) 0.053(3) 0.009(2) -0.008(3) -0.008(2) S1B 0.0632(11) 0.0471(9) 0.0571(10) -0.0106(8) 0.0169(9) -0.0170(8) F1B 0.089(5) 0.082(4) 0.184(9) -0.080(5) -0.019(5) 0.007(3) O1B 0.050(3) 0.054(3) 0.111(6) 0.018(3) -0.003(3) 0.009(3) C1B 0.056(5) 0.102(8) 0.105(8) -0.070(7) -0.029(5) 0.031(5) F2B 0.190(10) 0.064(4) 0.142(8) 0.013(5) -0.049(8) 0.031(5) O2B 0.088(5) 0.073(4) 0.092(5) -0.037(4) 0.020(4) -0.029(4) O3B 0.181(11) 0.144(9) 0.075(5) -0.025(5) 0.056(6) -0.103(9) F3B 0.049(4) 0.251(13) 0.281(14) -0.196(12) -0.052(6) 0.055(6) S1A 0.0577(11) 0.0494(10) 0.0868(16) -0.0118(10) 0.0033(11) -0.0045(8) O1A 0.037(2) 0.053(3) 0.062(3) -0.004(2) 0.001(2) 0.005(2) F1A 0.084(4) 0.104(5) 0.089(4) 0.021(4) -0.026(3) -0.019(4) C1A 0.058(5) 0.054(4) 0.076(5) -0.004(4) 0.006(4) 0.004(4) F2A 0.098(5) 0.120(6) 0.094(5) 0.034(4) 0.037(4) 0.037(5) O2A 0.077(5) 0.084(5) 0.108(6) -0.037(5) -0.006(5) -0.007(4) O3A 0.038(2) 0.045(2) 0.076(4) 0.003(2) 0.002(2) -0.0018(19) F3A 0.072(4) 0.046(3) 0.159(7) 0.001(3) -0.016(4) 0.002(3) S1C 0.0598(13) 0.0384(9) 0.158(3) 0.0122(13) 0.0251(16) 0.0040(8) O1C 0.069(4) 0.042(3) 0.171(9) 0.003(4) 0.039(5) 0.000(3) F1C 0.149(9) 0.054(4) 0.250(14) 0.007(6) -0.003(9) 0.026(5) C1C 0.146(15) 0.061(7) 0.140(14) -0.006(8) -0.031(12) 0.025(8) O2C 0.056(4) 0.081(5) 0.160(9) 0.026(6) 0.021(5) -0.003(4) F2C 0.178(10) 0.083(5) 0.167(9) -0.022(6) 0.005(8) 0.066(6) O3C 0.079(6) 0.046(4) 0.281(16) 0.012(6) 0.050(8) 0.007(4) F3C 0.133(8) 0.085(6) 0.198(11) 0.002(6) -0.031(8) -0.007(6) S1D 0.0737(19) 0.334(5) 0.0491(14) -0.037(2) 0.0130(13) -0.049(3) O1D 0.093(4) 0.115(4) 0.066(3) -0.009(3) 0.007(3) -0.007(4) F1D 0.180(7) 0.183(7) 0.173(6) -0.019(5) -0.008(5) -0.009(5) C1D 0.156(9) 0.164(9) 0.154(9) -0.009(5) -0.004(5) 0.001(5) O2D 0.074(4) 0.111(4) 0.067(3) -0.007(3) 0.003(3) -0.015(3) F2D 0.161(6) 0.151(6) 0.138(5) 0.000(4) -0.005(4) -0.007(4) O3D 0.082(4) 0.132(5) 0.066(3) -0.002(3) 0.002(3) -0.015(4) F3D 0.228(9) 0.239(9) 0.235(9) -0.012(5) 0.002(5) 0.001(5) O1L2 0.045(4) 0.044(4) 0.045(4) 0.000(2) 0.001(2) 0.003(2) C2L2 0.056(7) 0.056(7) 0.055(7) -0.0001(10) 0.0002(10) 0.0000(10) C3L2 0.075(5) 0.074(5) 0.074(5) -0.001(2) 0.000(2) 0.000(2) C1L2 0.056(7) 0.056(7) 0.055(7) -0.001(2) 0.001(2) 0.001(2) O1L 0.060(3) 0.0320(19) 0.069(3) 0.003(2) -0.010(3) -0.0080(19) C1L 0.067(5) 0.053(4) 0.067(5) 0.018(4) 0.027(4) 0.008(4) C2L 0.102(9) 0.055(5) 0.138(11) 0.026(6) 0.048(9) 0.001(5) C3L 0.119(9) 0.055(5) 0.136(10) 0.037(6) 0.041(8) 0.020(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 Pd1 N8 2.106(5) . ? Pd1 N1 2.108(4) . ? Pd1 P1 2.2710(14) . ? Pd1 P2 2.2791(13) . ? P1 C27 1.809(6) . ? P1 C36 1.815(5) . ? P1 C30 1.819(6) . ? N1 C5 1.342(7) . ? N1 C1 1.342(7) . ? C1 C2 1.379(7) . ? O1 C7 1.246(8) . ? Pd2 N4 2.089(4) . ? Pd2 N5 2.110(5) . ? Pd2 P4 2.2740(13) . ? Pd2 P3 2.2745(14) . ? C2 C3 1.384(7) . ? N2 C7 1.350(8) . ? N2 C6 1.429(8) . ? P2 C42 1.805(6) . ? P2 C29 1.807(6) . ? P2 C48 1.812(6) . ? O2 C20 1.243(10) . ? C3 C4 1.411(8) . ? C3 C6 1.497(7) . ? N3 C7 1.366(8) . ? N3 C8 1.450(8) . ? P3 C57 1.800(5) . ? P3 C54 1.802(6) . ? P3 C63 1.820(5) . ? C4 C5 1.375(8) . ? N4 C11 1.327(8) . ? N4 C12 1.356(7) . ? P4 C75 1.800(6) . ? P4 C56 1.810(6) . ? P4 C69 1.816(6) . ? N5 C14 1.335(8) . ? N5 C18 1.342(8) . ? N6 C20 1.335(11) . ? N6 C19 1.444(10) . ? N7 C20 1.359(12) . ? N7 C21 1.433(13) . ? C8 C9 1.491(7) . ? N8 C24 1.343(9) . ? N8 C25 1.350(8) . ? C9 C13 1.399(8) . ? C9 C10 1.405(7) . ? C10 C11 1.380(7) . ? C12 C13 1.380(7) . ? C14 C15 1.372(8) . ? C15 C16 1.412(9) . ? C16 C17 1.371(10) . ? C16 C19 1.496(9) . ? C17 C18 1.401(9) . ? C21 C22 1.505(12) . ? C22 C26 1.380(12) . ? C22 C23 1.393(10) . ? C23 C24 1.373(9) . ? C25 C26 1.379(10) . ? C27 C28 1.515(8) . ? C28 C29 1.549(9) . ? C30 C35 1.382(10) . ? C30 C31 1.386(9) . ? C31 C32 1.359(10) . ? C32 C33 1.353(13) . ? C33 C34 1.426(14) . ? C34 C35 1.380(11) . ? C36 C41 1.375(9) . ? C36 C37 1.389(9) . ? C37 C38 1.400(8) . ? C38 C39 1.393(13) . ? C39 C40 1.411(14) . ? C40 C41 1.399(10) . ? C42 C47 1.405(9) . ? C42 C43 1.406(9) . ? C43 C44 1.396(9) . ? C44 C45 1.416(13) . ? C45 C46 1.375(12) . ? C46 C47 1.389(10) . ? C48 C53 1.372(11) . ? C48 C49 1.410(8) . ? C49 C50 1.406(10) . ? C50 C51 1.349(16) . ? C51 C52 1.345(16) . ? C52 C53 1.394(10) . ? C54 C55 1.538(7) . ? C55 C56 1.539(8) . ? C57 C62 1.380(10) . ? C57 C58 1.392(8) . ? C58 C59 1.396(9) . ? C59 C60 1.397(12) . ? C60 C61 1.390(12) . ? C61 C62 1.399(10) . ? C63 C64 1.374(9) . ? C63 C68 1.396(9) . ? C64 C65 1.393(9) . ? C65 C66 1.401(12) . ? C66 C67 1.412(12) . ? C67 C68 1.400(9) . ? C69 C74 1.374(11) . ? C69 C70 1.419(8) . ? C70 C71 1.390(10) . ? C71 C72 1.409(15) . ? C72 C73 1.405(16) . ? C73 C74 1.371(12) . ? C75 C80 1.398(9) . ? C75 C76 1.432(11) . ? C76 C77 1.383(10) . ? C77 C78 1.359(13) . ? C78 C79 1.395(13) . ? C79 C80 1.422(10) . ? S1B O1B 1.421(7) . ? S1B O2B 1.433(7) . ? S1B O3B 1.439(9) . ? S1B C1B 1.873(14) . ? F1B C1B 1.308(10) . ? C1B F2B 1.242(17) . ? C1B F3B 1.337(14) . ? S1A O3A 1.431(6) . ? S1A O1A 1.439(6) . ? S1A O2A 1.452(8) . ? S1A C1A 1.810(10) . ? F1A C1A 1.296(11) . ? C1A F2A 1.310(11) . ? C1A F3A 1.343(11) . ? S1C O2C 1.459(9) . ? S1C O1C 1.462(8) . ? S1C O3C 1.463(9) . ? S1C C1C 1.802(19) . ? F1C C1C 1.339(18) . ? C1C F2C 1.32(2) . ? C1C F3C 1.33(2) . ? S1D O1D 1.434(4) . ? S1D O2D 1.444(4) . ? S1D O3D 1.455(4) . ? S1D C1D 1.873(5) . ? F1D C1D 1.327(5) . ? C1D F3D 1.318(5) . ? C1D F2D 1.325(5) . ? O1L2 C1L2 1.428(5) . ? C2L2 C1L2 1.540(5) . ? C3L2 C1L2 1.539(5) . ? O1L C1L 1.386(9) . ? C1L C2L 1.550(15) . ? C1L C3L 1.570(15) . ? 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 N8 Pd1 N1 85.78(19) . . ? N8 Pd1 P1 175.47(16) . . ? N1 Pd1 P1 91.39(13) . . ? N8 Pd1 P2 91.37(14) . . ? N1 Pd1 P2 177.10(14) . . ? P1 Pd1 P2 91.42(5) . . ? C27 P1 C36 105.0(3) . . ? C27 P1 C30 104.9(3) . . ? C36 P1 C30 107.4(3) . . ? C27 P1 Pd1 113.6(2) . . ? C36 P1 Pd1 110.0(2) . . ? C30 P1 Pd1 115.2(2) . . ? C5 N1 C1 118.5(4) . . ? C5 N1 Pd1 121.5(4) . . ? C1 N1 Pd1 119.9(3) . . ? N1 C1 C2 122.4(5) . . ? N4 Pd2 N5 86.07(17) . . ? N4 Pd2 P4 177.96(13) . . ? N5 Pd2 P4 91.92(11) . . ? N4 Pd2 P3 91.01(13) . . ? N5 Pd2 P3 176.74(12) . . ? P4 Pd2 P3 90.99(5) . . ? C1 C2 C3 120.2(5) . . ? C7 N2 C6 123.0(6) . . ? C42 P2 C29 105.1(3) . . ? C42 P2 C48 105.9(3) . . ? C29 P2 C48 106.2(3) . . ? C42 P2 Pd1 110.18(17) . . ? C29 P2 Pd1 115.30(17) . . ? C48 P2 Pd1 113.5(2) . . ? C2 C3 C4 116.7(5) . . ? C2 C3 C6 123.6(5) . . ? C4 C3 C6 119.6(5) . . ? C7 N3 C8 120.9(6) . . ? C57 P3 C54 106.4(3) . . ? C57 P3 C63 104.4(3) . . ? C54 P3 C63 104.9(3) . . ? C57 P3 Pd2 115.4(2) . . ? C54 P3 Pd2 114.04(19) . . ? C63 P3 Pd2 110.77(18) . . ? C5 C4 C3 120.0(5) . . ? C11 N4 C12 119.2(5) . . ? C11 N4 Pd2 119.4(3) . . ? C12 N4 Pd2 121.3(4) . . ? C75 P4 C56 105.5(3) . . ? C75 P4 C69 105.0(3) . . ? C56 P4 C69 106.4(3) . . ? C75 P4 Pd2 110.74(19) . . ? C56 P4 Pd2 113.38(19) . . ? C69 P4 Pd2 115.0(2) . . ? C14 N5 C18 119.2(5) . . ? C14 N5 Pd2 120.9(4) . . ? C18 N5 Pd2 119.8(4) . . ? N1 C5 C4 122.2(5) . . ? N2 C6 C3 114.4(4) . . ? C20 N6 C19 122.5(7) . . ? O1 C7 N2 123.6(6) . . ? O1 C7 N3 120.9(6) . . ? N2 C7 N3 115.5(6) . . ? C20 N7 C21 120.2(9) . . ? N3 C8 C9 113.8(4) . . ? C24 N8 C25 119.3(6) . . ? C24 N8 Pd1 120.8(4) . . ? C25 N8 Pd1 119.9(5) . . ? C13 C9 C10 117.3(5) . . ? C13 C9 C8 119.0(4) . . ? C10 C9 C8 123.7(5) . . ? C11 C10 C9 119.4(5) . . ? N4 C11 C10 122.6(5) . . ? N4 C12 C13 121.5(5) . . ? C12 C13 C9 120.0(5) . . ? N5 C14 C15 123.2(6) . . ? C14 C15 C16 118.9(6) . . ? C17 C16 C15 117.2(6) . . ? C17 C16 C19 121.7(7) . . ? C15 C16 C19 121.1(7) . . ? C16 C17 C18 121.1(6) . . ? N5 C18 C17 120.4(6) . . ? N6 C19 C16 115.7(6) . . ? O2 C20 N6 121.6(9) . . ? O2 C20 N7 123.6(9) . . ? N6 C20 N7 114.8(7) . . ? N7 C21 C22 115.9(7) . . ? C26 C22 C23 117.6(7) . . ? C26 C22 C21 120.1(7) . . ? C23 C22 C21 122.1(8) . . ? C24 C23 C22 120.1(7) . . ? N8 C24 C23 121.5(6) . . ? N8 C25 C26 121.2(7) . . ? C25 C26 C22 120.3(7) . . ? C28 C27 P1 112.8(4) . . ? C27 C28 C29 112.5(5) . . ? C28 C29 P2 111.7(4) . . ? C35 C30 C31 118.5(6) . . ? C35 C30 P1 121.1(5) . . ? C31 C30 P1 120.4(5) . . ? C32 C31 C30 121.7(7) . . ? C33 C32 C31 120.8(7) . . ? C32 C33 C34 119.1(7) . . ? C35 C34 C33 119.3(8) . . ? C34 C35 C30 120.5(8) . . ? C41 C36 C37 120.9(5) . . ? C41 C36 P1 119.6(5) . . ? C37 C36 P1 119.4(5) . . ? C36 C37 C38 119.6(7) . . ? C39 C38 C37 119.9(8) . . ? C38 C39 C40 119.9(6) . . ? C41 C40 C39 119.0(8) . . ? C36 C41 C40 120.4(7) . . ? C47 C42 C43 118.9(6) . . ? C47 C42 P2 120.6(5) . . ? C43 C42 P2 120.4(5) . . ? C44 C43 C42 120.9(7) . . ? C43 C44 C45 118.7(8) . . ? C46 C45 C44 120.4(7) . . ? C45 C46 C47 120.7(7) . . ? C46 C47 C42 120.2(7) . . ? C53 C48 C49 117.8(6) . . ? C53 C48 P2 122.0(5) . . ? C49 C48 P2 120.2(5) . . ? C50 C49 C48 118.5(8) . . ? C51 C50 C49 121.9(9) . . ? C52 C51 C50 119.9(8) . . ? C51 C52 C53 120.2(10) . . ? C48 C53 C52 121.5(8) . . ? C55 C54 P3 114.2(4) . . ? C54 C55 C56 111.1(4) . . ? C55 C56 P4 112.4(4) . . ? C62 C57 C58 119.9(6) . . ? C62 C57 P3 121.3(5) . . ? C58 C57 P3 118.7(5) . . ? C57 C58 C59 120.9(6) . . ? C58 C59 C60 118.4(7) . . ? C61 C60 C59 121.1(7) . . ? C60 C61 C62 119.3(8) . . ? C57 C62 C61 120.2(7) . . ? C64 C63 C68 120.8(5) . . ? C64 C63 P3 119.9(5) . . ? C68 C63 P3 119.1(5) . . ? C63 C64 C65 120.6(7) . . ? C64 C65 C66 119.1(7) . . ? C65 C66 C67 120.9(6) . . ? C68 C67 C66 118.3(7) . . ? C63 C68 C67 120.2(7) . . ? C74 C69 C70 119.5(6) . . ? C74 C69 P4 121.0(5) . . ? C70 C69 P4 119.5(6) . . ? C71 C70 C69 118.5(7) . . ? C70 C71 C72 121.0(8) . . ? C73 C72 C71 119.4(8) . . ? C74 C73 C72 118.8(10) . . ? C73 C74 C69 122.7(8) . . ? C80 C75 C76 118.4(6) . . ? C80 C75 P4 120.2(6) . . ? C76 C75 P4 121.3(5) . . ? C77 C76 C75 119.8(8) . . ? C78 C77 C76 121.2(8) . . ? C77 C78 C79 121.5(7) . . ? C78 C79 C80 118.5(7) . . ? C75 C80 C79 120.6(7) . . ? O1B S1B O2B 114.8(5) . . ? O1B S1B O3B 115.6(7) . . ? O2B S1B O3B 117.6(5) . . ? O1B S1B C1B 101.9(5) . . ? O2B S1B C1B 97.9(5) . . ? O3B S1B C1B 105.2(7) . . ? F2B C1B F1B 106.6(14) . . ? F2B C1B F3B 114.6(13) . . ? F1B C1B F3B 107.2(8) . . ? F2B C1B S1B 110.8(7) . . ? F1B C1B S1B 112.5(9) . . ? F3B C1B S1B 105.3(12) . . ? O3A S1A O1A 117.9(4) . . ? O3A S1A O2A 113.3(5) . . ? O1A S1A O2A 113.7(5) . . ? O3A S1A C1A 103.4(4) . . ? O1A S1A C1A 101.9(4) . . ? O2A S1A C1A 104.4(5) . . ? F1A C1A F2A 111.8(9) . . ? F1A C1A F3A 101.0(8) . . ? F2A C1A F3A 97.3(8) . . ? F1A C1A S1A 115.9(7) . . ? F2A C1A S1A 115.1(7) . . ? F3A C1A S1A 113.4(7) . . ? O2C S1C O1C 110.6(5) . . ? O2C S1C O3C 116.4(6) . . ? O1C S1C O3C 115.0(5) . . ? O2C S1C C1C 105.3(8) . . ? O1C S1C C1C 102.9(7) . . ? O3C S1C C1C 105.0(8) . . ? F2C C1C F3C 108.0(13) . . ? F2C C1C F1C 108.6(17) . . ? F3C C1C F1C 108.9(14) . . ? F2C C1C S1C 110.8(12) . . ? F3C C1C S1C 112.3(15) . . ? F1C C1C S1C 108.3(11) . . ? O1D S1D O2D 117.0(5) . . ? O1D S1D O3D 114.2(5) . . ? O2D S1D O3D 113.2(5) . . ? O1D S1D C1D 101.2(6) . . ? O2D S1D C1D 106.7(6) . . ? O3D S1D C1D 102.1(6) . . ? F3D C1D F2D 104.1(7) . . ? F3D C1D F1D 106.5(7) . . ? F2D C1D F1D 103.8(7) . . ? F3D C1D S1D 106.8(11) . . ? F2D C1D S1D 115.3(9) . . ? F1D C1D S1D 119.0(10) . . ? O1L2 C1L2 C3L2 114.3(18) . . ? O1L2 C1L2 C2L2 98(2) . . ? C3L2 C1L2 C2L2 102(2) . . ? O1L C1L C2L 114.9(8) . . ? O1L C1L C3L 108.6(7) . . ? C2L C1L C3L 104.3(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Pd1 P1 C27 88.5(19) . . . . ? N1 Pd1 P1 C27 139.9(3) . . . . ? P2 Pd1 P1 C27 -39.4(2) . . . . ? N8 Pd1 P1 C36 -29(2) . . . . ? N1 Pd1 P1 C36 22.4(3) . . . . ? P2 Pd1 P1 C36 -156.8(2) . . . . ? N8 Pd1 P1 C30 -150.4(19) . . . . ? N1 Pd1 P1 C30 -99.1(2) . . . . ? P2 Pd1 P1 C30 81.6(2) . . . . ? N8 Pd1 N1 C5 86.7(5) . . . . ? P1 Pd1 N1 C5 -89.7(5) . . . . ? P2 Pd1 N1 C5 76(3) . . . . ? N8 Pd1 N1 C1 -88.9(5) . . . . ? P1 Pd1 N1 C1 94.7(4) . . . . ? P2 Pd1 N1 C1 -99(3) . . . . ? C5 N1 C1 C2 1.2(9) . . . . ? Pd1 N1 C1 C2 176.9(5) . . . . ? N1 C1 C2 C3 -1.3(10) . . . . ? N8 Pd1 P2 C42 -18.6(3) . . . . ? N1 Pd1 P2 C42 -8(3) . . . . ? P1 Pd1 P2 C42 157.8(2) . . . . ? N8 Pd1 P2 C29 -137.3(3) . . . . ? N1 Pd1 P2 C29 -127(3) . . . . ? P1 Pd1 P2 C29 39.1(2) . . . . ? N8 Pd1 P2 C48 99.9(3) . . . . ? N1 Pd1 P2 C48 110(3) . . . . ? P1 Pd1 P2 C48 -83.7(2) . . . . ? C1 C2 C3 C4 0.9(9) . . . . ? C1 C2 C3 C6 -176.8(6) . . . . ? N4 Pd2 P3 C57 97.2(2) . . . . ? N5 Pd2 P3 C57 123(3) . . . . ? P4 Pd2 P3 C57 -83.28(19) . . . . ? N4 Pd2 P3 C54 -139.2(2) . . . . ? N5 Pd2 P3 C54 -113(3) . . . . ? P4 Pd2 P3 C54 40.3(2) . . . . ? N4 Pd2 P3 C63 -21.2(3) . . . . ? N5 Pd2 P3 C63 5(3) . . . . ? P4 Pd2 P3 C63 158.4(2) . . . . ? C2 C3 C4 C5 -0.4(9) . . . . ? C6 C3 C4 C5 177.4(6) . . . . ? N5 Pd2 N4 C11 81.2(4) . . . . ? P4 Pd2 N4 C11 93(4) . . . . ? P3 Pd2 N4 C11 -100.2(4) . . . . ? N5 Pd2 N4 C12 -95.4(4) . . . . ? P4 Pd2 N4 C12 -84(4) . . . . ? P3 Pd2 N4 C12 83.1(4) . . . . ? N4 Pd2 P4 C75 7(4) . . . . ? N5 Pd2 P4 C75 18.0(3) . . . . ? P3 Pd2 P4 C75 -160.6(3) . . . . ? N4 Pd2 P4 C56 125(4) . . . . ? N5 Pd2 P4 C56 136.4(3) . . . . ? P3 Pd2 P4 C56 -42.2(2) . . . . ? N4 Pd2 P4 C69 -112(4) . . . . ? N5 Pd2 P4 C69 -100.8(3) . . . . ? P3 Pd2 P4 C69 80.6(2) . . . . ? N4 Pd2 N5 C14 -85.1(4) . . . . ? P4 Pd2 N5 C14 95.3(4) . . . . ? P3 Pd2 N5 C14 -111(2) . . . . ? N4 Pd2 N5 C18 99.4(4) . . . . ? P4 Pd2 N5 C18 -80.2(4) . . . . ? P3 Pd2 N5 C18 73(3) . . . . ? C1 N1 C5 C4 -0.7(9) . . . . ? Pd1 N1 C5 C4 -176.3(5) . . . . ? C3 C4 C5 N1 0.3(10) . . . . ? C7 N2 C6 C3 95.2(7) . . . . ? C2 C3 C6 N2 -18.0(9) . . . . ? C4 C3 C6 N2 164.3(6) . . . . ? C6 N2 C7 O1 1.4(8) . . . . ? C6 N2 C7 N3 -176.1(4) . . . . ? C8 N3 C7 O1 6.3(7) . . . . ? C8 N3 C7 N2 -176.2(4) . . . . ? C7 N3 C8 C9 -83.1(6) . . . . ? N1 Pd1 N8 C24 88.0(5) . . . . ? P1 Pd1 N8 C24 139.5(17) . . . . ? P2 Pd1 N8 C24 -92.6(4) . . . . ? N1 Pd1 N8 C25 -94.5(5) . . . . ? P1 Pd1 N8 C25 -43(2) . . . . ? P2 Pd1 N8 C25 85.0(4) . . . . ? N3 C8 C9 C13 178.9(5) . . . . ? N3 C8 C9 C10 -0.3(8) . . . . ? C13 C9 C10 C11 -2.3(8) . . . . ? C8 C9 C10 C11 177.0(6) . . . . ? C12 N4 C11 C10 -1.5(9) . . . . ? Pd2 N4 C11 C10 -178.3(5) . . . . ? C9 C10 C11 N4 2.3(9) . . . . ? C11 N4 C12 C13 0.8(8) . . . . ? Pd2 N4 C12 C13 177.4(4) . . . . ? N4 C12 C13 C9 -0.8(8) . . . . ? C10 C9 C13 C12 1.6(8) . . . . ? C8 C9 C13 C12 -177.7(5) . . . . ? C18 N5 C14 C15 2.8(8) . . . . ? Pd2 N5 C14 C15 -172.7(4) . . . . ? N5 C14 C15 C16 -0.5(9) . . . . ? C14 C15 C16 C17 -2.2(8) . . . . ? C14 C15 C16 C19 176.4(6) . . . . ? C15 C16 C17 C18 2.8(8) . . . . ? C19 C16 C17 C18 -175.8(6) . . . . ? C14 N5 C18 C17 -2.2(8) . . . . ? Pd2 N5 C18 C17 173.4(4) . . . . ? C16 C17 C18 N5 -0.6(8) . . . . ? C20 N6 C19 C16 101.6(8) . . . . ? C17 C16 C19 N6 160.5(6) . . . . ? C15 C16 C19 N6 -18.0(10) . . . . ? C19 N6 C20 O2 2.7(11) . . . . ? C19 N6 C20 N7 -179.2(6) . . . . ? C21 N7 C20 O2 -12.3(12) . . . . ? C21 N7 C20 N6 169.7(7) . . . . ? C20 N7 C21 C22 -79.2(13) . . . . ? N7 C21 C22 C26 177.3(9) . . . . ? N7 C21 C22 C23 -7.1(17) . . . . ? C26 C22 C23 C24 0.1(13) . . . . ? C21 C22 C23 C24 -175.7(10) . . . . ? C25 N8 C24 C23 -4.1(9) . . . . ? Pd1 N8 C24 C23 173.5(6) . . . . ? C22 C23 C24 N8 2.9(12) . . . . ? C24 N8 C25 C26 2.3(9) . . . . ? Pd1 N8 C25 C26 -175.3(5) . . . . ? N8 C25 C26 C22 0.6(11) . . . . ? C23 C22 C26 C25 -1.8(13) . . . . ? C21 C22 C26 C25 174.1(9) . . . . ? C36 P1 C27 C28 -177.7(5) . . . . ? C30 P1 C27 C28 -64.7(5) . . . . ? Pd1 P1 C27 C28 62.0(5) . . . . ? P1 C27 C28 C29 -77.9(6) . . . . ? C27 C28 C29 P2 75.2(6) . . . . ? C42 P2 C29 C28 -180.0(4) . . . . ? C48 P2 C29 C28 68.1(4) . . . . ? Pd1 P2 C29 C28 -58.5(4) . . . . ? C27 P1 C30 C35 139.2(6) . . . . ? C36 P1 C30 C35 -109.5(7) . . . . ? Pd1 P1 C30 C35 13.5(7) . . . . ? C27 P1 C30 C31 -39.5(5) . . . . ? C36 P1 C30 C31 71.9(5) . . . . ? Pd1 P1 C30 C31 -165.1(4) . . . . ? C35 C30 C31 C32 0.3(10) . . . . ? P1 C30 C31 C32 178.9(5) . . . . ? C30 C31 C32 C33 0.8(11) . . . . ? C31 C32 C33 C34 -2.2(13) . . . . ? C32 C33 C34 C35 2.7(16) . . . . ? C33 C34 C35 C30 -1.7(17) . . . . ? C31 C30 C35 C34 0.2(14) . . . . ? P1 C30 C35 C34 -178.5(8) . . . . ? C27 P1 C36 C41 -39.4(7) . . . . ? C30 P1 C36 C41 -150.7(6) . . . . ? Pd1 P1 C36 C41 83.2(6) . . . . ? C27 P1 C36 C37 143.7(6) . . . . ? C30 P1 C36 C37 32.4(6) . . . . ? Pd1 P1 C36 C37 -93.7(5) . . . . ? C41 C36 C37 C38 -1.3(11) . . . . ? P1 C36 C37 C38 175.6(6) . . . . ? C36 C37 C38 C39 3.2(12) . . . . ? C37 C38 C39 C40 -4.8(14) . . . . ? C38 C39 C40 C41 4.3(16) . . . . ? C37 C36 C41 C40 0.9(12) . . . . ? P1 C36 C41 C40 -176.0(7) . . . . ? C39 C40 C41 C36 -2.4(15) . . . . ? C29 P2 C42 C47 38.4(5) . . . . ? C48 P2 C42 C47 150.6(5) . . . . ? Pd1 P2 C42 C47 -86.4(5) . . . . ? C29 P2 C42 C43 -145.9(4) . . . . ? C48 P2 C42 C43 -33.7(5) . . . . ? Pd1 P2 C42 C43 89.3(4) . . . . ? C47 C42 C43 C44 1.3(8) . . . . ? P2 C42 C43 C44 -174.5(5) . . . . ? C42 C43 C44 C45 -2.4(10) . . . . ? C43 C44 C45 C46 1.3(10) . . . . ? C44 C45 C46 C47 0.9(11) . . . . ? C45 C46 C47 C42 -2.1(10) . . . . ? C43 C42 C47 C46 0.9(9) . . . . ? P2 C42 C47 C46 176.7(5) . . . . ? C42 P2 C48 C53 96.4(7) . . . . ? C29 P2 C48 C53 -152.2(7) . . . . ? Pd1 P2 C48 C53 -24.6(8) . . . . ? C42 P2 C48 C49 -82.8(6) . . . . ? C29 P2 C48 C49 28.5(6) . . . . ? Pd1 P2 C48 C49 156.2(5) . . . . ? C53 C48 C49 C50 -0.7(12) . . . . ? P2 C48 C49 C50 178.6(7) . . . . ? C48 C49 C50 C51 -0.9(15) . . . . ? C49 C50 C51 C52 -1.0(18) . . . . ? C50 C51 C52 C53 4.3(19) . . . . ? C49 C48 C53 C52 4.0(15) . . . . ? P2 C48 C53 C52 -175.3(9) . . . . ? C51 C52 C53 C48 -5.9(19) . . . . ? C57 P3 C54 C55 68.3(4) . . . . ? C63 P3 C54 C55 178.6(4) . . . . ? Pd2 P3 C54 C55 -60.1(4) . . . . ? P3 C54 C55 C56 74.5(6) . . . . ? C54 C55 C56 P4 -76.2(6) . . . . ? C75 P4 C56 C55 -174.7(4) . . . . ? C69 P4 C56 C55 -63.4(4) . . . . ? Pd2 P4 C56 C55 64.0(4) . . . . ? C54 P3 C57 C62 -135.1(5) . . . . ? C63 P3 C57 C62 114.3(5) . . . . ? Pd2 P3 C57 C62 -7.5(5) . . . . ? C54 P3 C57 C58 47.3(5) . . . . ? C63 P3 C57 C58 -63.3(5) . . . . ? Pd2 P3 C57 C58 174.9(4) . . . . ? C62 C57 C58 C59 -0.5(9) . . . . ? P3 C57 C58 C59 177.1(5) . . . . ? C57 C58 C59 C60 0.2(10) . . . . ? C58 C59 C60 C61 2.6(12) . . . . ? C59 C60 C61 C62 -5.0(13) . . . . ? C58 C57 C62 C61 -1.9(10) . . . . ? P3 C57 C62 C61 -179.5(6) . . . . ? C60 C61 C62 C57 4.6(13) . . . . ? C57 P3 C63 C64 -35.4(5) . . . . ? C54 P3 C63 C64 -147.1(5) . . . . ? Pd2 P3 C63 C64 89.4(5) . . . . ? C57 P3 C63 C68 149.4(5) . . . . ? C54 P3 C63 C68 37.7(5) . . . . ? Pd2 P3 C63 C68 -85.7(5) . . . . ? C68 C63 C64 C65 0.4(10) . . . . ? P3 C63 C64 C65 -174.7(5) . . . . ? C63 C64 C65 C66 -1.7(10) . . . . ? C64 C65 C66 C67 2.7(11) . . . . ? C65 C66 C67 C68 -2.4(12) . . . . ? C64 C63 C68 C67 -0.1(10) . . . . ? P3 C63 C68 C67 175.0(6) . . . . ? C66 C67 C68 C63 1.1(11) . . . . ? C75 P4 C69 C74 -90.9(7) . . . . ? C56 P4 C69 C74 157.5(7) . . . . ? Pd2 P4 C69 C74 31.1(7) . . . . ? C75 P4 C69 C70 89.7(5) . . . . ? C56 P4 C69 C70 -21.9(5) . . . . ? Pd2 P4 C69 C70 -148.4(4) . . . . ? C74 C69 C70 C71 -1.9(10) . . . . ? P4 C69 C70 C71 177.5(5) . . . . ? C69 C70 C71 C72 2.5(11) . . . . ? C70 C71 C72 C73 0.8(13) . . . . ? C71 C72 C73 C74 -4.7(16) . . . . ? C72 C73 C74 C69 5.4(17) . . . . ? C70 C69 C74 C73 -2.1(14) . . . . ? P4 C69 C74 C73 178.4(9) . . . . ? C56 P4 C75 C80 151.5(4) . . . . ? C69 P4 C75 C80 39.3(5) . . . . ? Pd2 P4 C75 C80 -85.4(5) . . . . ? C56 P4 C75 C76 -31.5(6) . . . . ? C69 P4 C75 C76 -143.7(5) . . . . ? Pd2 P4 C75 C76 91.6(5) . . . . ? C80 C75 C76 C77 -1.5(10) . . . . ? P4 C75 C76 C77 -178.6(6) . . . . ? C75 C76 C77 C78 2.1(13) . . . . ? C76 C77 C78 C79 -1.0(13) . . . . ? C77 C78 C79 C80 -0.8(11) . . . . ? C76 C75 C80 C79 -0.2(8) . . . . ? P4 C75 C80 C79 176.9(4) . . . . ? C78 C79 C80 C75 1.3(9) . . . . ? O1B S1B C1B F2B 55.0(9) . . . . ? O2B S1B C1B F2B -62.6(9) . . . . ? O3B S1B C1B F2B 176.0(9) . . . . ? O1B S1B C1B F1B -64.2(11) . . . . ? O2B S1B C1B F1B 178.2(10) . . . . ? O3B S1B C1B F1B 56.8(12) . . . . ? O1B S1B C1B F3B 179.4(9) . . . . ? O2B S1B C1B F3B 61.8(9) . . . . ? O3B S1B C1B F3B -59.6(10) . . . . ? O3A S1A C1A F1A -173.0(7) . . . . ? O1A S1A C1A F1A -50.2(8) . . . . ? O2A S1A C1A F1A 68.3(8) . . . . ? O3A S1A C1A F2A 54.0(9) . . . . ? O1A S1A C1A F2A 176.7(8) . . . . ? O2A S1A C1A F2A -64.8(9) . . . . ? O3A S1A C1A F3A -56.8(7) . . . . ? O1A S1A C1A F3A 66.0(7) . . . . ? O2A S1A C1A F3A -175.5(7) . . . . ? O2C S1C C1C F2C 61.6(13) . . . . ? O1C S1C C1C F2C 177.5(12) . . . . ? O3C S1C C1C F2C -61.8(14) . . . . ? O2C S1C C1C F3C -177.5(9) . . . . ? O1C S1C C1C F3C -61.6(10) . . . . ? O3C S1C C1C F3C 59.1(11) . . . . ? O2C S1C C1C F1C -57.3(14) . . . . ? O1C S1C C1C F1C 58.6(14) . . . . ? O3C S1C C1C F1C 179.3(12) . . . . ? O1D S1D C1D F3D 69.6(8) . . . . ? O2D S1D C1D F3D -53.3(8) . . . . ? O3D S1D C1D F3D -172.3(8) . . . . ? O1D S1D C1D F2D -175.2(9) . . . . ? O2D S1D C1D F2D 61.8(10) . . . . ? O3D S1D C1D F2D -57.2(10) . . . . ? O1D S1D C1D F1D -50.8(10) . . . . ? O2D S1D C1D F1D -173.7(8) . . . . ? O3D S1D C1D F1D 67.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.18 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.535 _refine_diff_density_min -2.093 _refine_diff_density_rms 0.181 #===END data_pd210isg _database_code_depnum_ccdc_archive 'CCDC 624783' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C100.25 H94.50 F12 N8 O18.75 P4 Pd2 S4' _chemical_formula_weight 2404.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.8443(7) _cell_length_b 18.8383(9) _cell_length_c 20.6983(8) _cell_angle_alpha 95.680(2) _cell_angle_beta 94.482(2) _cell_angle_gamma 104.570(2) _cell_volume 5915.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2452 _exptl_absorpt_coefficient_mu 0.510 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.873952 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'MACScience Co. M18X-HF' _diffrn_source_power 40 _diffrn_source_current 240 _diffrn_source_size '10 mm x 0.5 mm fine focus' _diffrn_radiation_monochromator Graphite _diffrn_detector_type 'Smart 1000 CCD area detector' _diffrn_measurement_device_type 'four-circle diffractometer Bruker P4' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 74819 _diffrn_reflns_av_R_equivalents 0.1251 _diffrn_reflns_av_sigmaI/netI 0.1867 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 28.00 _reflns_number_total 28010 _reflns_number_gt 12427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart CCDC area detector system' _computing_cell_refinement 'Bruker SAINT program vers. 5.0' _computing_data_reduction 'Bruker SAINT program vers. 5.0' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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 triflate anions refined are partly disordered with large thermical ellipsoids. Also the isopropanol and the water molecules are disordered and in some cases have partial assigned occupancies. Distances and thermical displacement parameters for these anions/solvent molecules are in some cases restrained. After final refinement there are residual voids which probably contain highly disordered isopropanol molecules. The detected highest peak and deepest hole of the electron densities are localized close to one of the disordere solvent molecules but could not be identified and refined as disordered solvent. Applying Squeeze (Platon) did not give significant data improvements resulting to similar R-values as modeling disordered solvent molecules. ; _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^)+(0.1356P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28010 _refine_ls_number_parameters 1404 _refine_ls_number_restraints 196 _refine_ls_R_factor_all 0.1796 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_ref 0.2690 _refine_ls_wR_factor_gt 0.2237 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.988 _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 Pd1 Pd 0.12997(4) 0.19899(3) 0.16932(3) 0.02689(16) Uani 1 1 d . . . P1 P -0.00923(13) 0.20395(11) 0.13889(10) 0.0304(4) Uani 1 1 d . . . N1 N 0.2588(4) 0.1970(3) 0.1987(3) 0.0267(13) Uani 1 1 d . . . O1 O 0.5948(4) 0.3388(3) 0.3170(3) 0.0448(14) Uani 1 1 d . . . C1 C -0.0708(5) 0.1295(4) 0.0786(4) 0.0371(19) Uani 1 1 d . . . H1A H -0.0757 0.0822 0.0968 0.045 Uiso 1 1 calc R . . H1B H -0.1309 0.1353 0.0698 0.045 Uiso 1 1 calc R . . Pd2 Pd 0.39464(4) 0.77512(3) 0.27529(3) 0.03165(17) Uani 1 1 d . . . P2 P 0.14661(12) 0.17347(10) 0.06256(10) 0.0272(4) Uani 1 1 d . . . N2 N 0.5905(4) 0.2564(3) 0.2300(3) 0.0380(16) Uani 1 1 d . . . H2C H 0.6091 0.2481 0.1917 0.046 Uiso 1 1 calc R . . C2 C -0.0306(5) 0.1253(4) 0.0138(4) 0.0378(19) Uani 1 1 d . . . H2A H -0.0733 0.0894 -0.0189 0.045 Uiso 1 1 calc R . . H2B H -0.0198 0.1742 -0.0022 0.045 Uiso 1 1 calc R . . O2 O 0.8084(6) 0.6279(4) 0.2150(4) 0.098(3) Uani 1 1 d . . . P3 P 0.42516(14) 0.79542(10) 0.17236(10) 0.0332(5) Uani 1 1 d . . . O3 O 0.1314(4) 0.6841(3) 0.5487(3) 0.0485(15) Uani 1 1 d . . . N3 N 0.7497(5) 0.6059(4) 0.3082(4) 0.050(2) Uani 1 1 d . . . H3C H 0.7294 0.5724 0.3338 0.060 Uiso 1 1 calc R . . C3 C 0.0545(5) 0.1026(4) 0.0192(4) 0.0342(18) Uani 1 1 d . . . H3A H 0.0690 0.0893 -0.0253 0.041 Uiso 1 1 calc R . . H3B H 0.0459 0.0578 0.0419 0.041 Uiso 1 1 calc R . . P4 P 0.27003(16) 0.81247(11) 0.25844(12) 0.0424(6) Uani 1 1 d . . . N4 N 0.5087(4) 0.7406(3) 0.2928(3) 0.0377(16) Uani 1 1 d . . . O4 O 0.1823(4) 0.3593(3) 0.5250(3) 0.0528(16) Uani 1 1 d . . . C4 C -0.0740(6) 0.1974(5) 0.2072(4) 0.044(2) Uani 1 1 d . . . N5 N 0.3704(5) 0.7529(4) 0.3704(3) 0.0396(16) Uani 1 1 d . . . C5 C -0.0972(6) 0.2575(5) 0.2366(4) 0.050(2) Uani 1 1 d . . . H5A H -0.0807 0.3035 0.2197 0.060 Uiso 1 1 calc R . . N6 N 0.2516(5) 0.6449(4) 0.5711(3) 0.0417(17) Uani 1 1 d . . . H6B H 0.2730 0.6080 0.5809 0.050 Uiso 1 1 calc R . . C6 C -0.1432(7) 0.2520(7) 0.2890(6) 0.073(3) Uani 1 1 d . . . H6A H -0.1630 0.2928 0.3063 0.087 Uiso 1 1 calc R . . N7 N 0.0384(5) 0.3033(3) 0.4934(3) 0.0390(16) Uani 1 1 d . . . H7B H -0.0156 0.3081 0.4897 0.047 Uiso 1 1 calc R . . C7 C -0.1614(7) 0.1879(8) 0.3171(5) 0.076(4) Uani 1 1 d . . . H7A H -0.1903 0.1853 0.3556 0.092 Uiso 1 1 calc R . . N8 N 0.1166(4) 0.2178(3) 0.2700(3) 0.0313(14) Uani 1 1 d . . . C8 C -0.1378(8) 0.1273(8) 0.2895(6) 0.087(4) Uani 1 1 d . . . H8A H -0.1497 0.0828 0.3091 0.104 Uiso 1 1 calc R . . C9 C -0.0960(7) 0.1317(7) 0.2322(5) 0.063(3) Uani 1 1 d . . . H9A H -0.0831 0.0892 0.2109 0.076 Uiso 1 1 calc R . . C10 C -0.0106(5) 0.2899(4) 0.1080(4) 0.0383(19) Uani 1 1 d . . . C11 C -0.0712(6) 0.2947(5) 0.0575(4) 0.047(2) Uani 1 1 d . . . H11A H -0.1159 0.2521 0.0392 0.056 Uiso 1 1 calc R . . C12 C -0.0662(8) 0.3625(7) 0.0338(5) 0.065(3) Uani 1 1 d . . . H12A H -0.1060 0.3662 -0.0018 0.078 Uiso 1 1 calc R . . C13 C -0.0020(9) 0.4243(6) 0.0632(6) 0.071(3) Uani 1 1 d . . . H13A H 0.0008 0.4708 0.0481 0.086 Uiso 1 1 calc R . . C14 C 0.0548(8) 0.4202(5) 0.1113(6) 0.071(3) Uani 1 1 d . . . H14A H 0.0976 0.4636 0.1308 0.085 Uiso 1 1 calc R . . C16 C 0.0528(7) 0.3533(5) 0.1339(5) 0.058(3) Uani 1 1 d . . . H16A H 0.0957 0.3509 0.1677 0.069 Uiso 1 1 calc R . . C17 C 0.2408(5) 0.1380(4) 0.0491(3) 0.0285(16) Uani 1 1 d . . . C18 C 0.2313(6) 0.0613(4) 0.0444(4) 0.0379(19) Uani 1 1 d . . . H18A H 0.1763 0.0281 0.0480 0.045 Uiso 1 1 calc R . . C19 C 0.3049(7) 0.0350(5) 0.0344(5) 0.055(3) Uani 1 1 d . . . H19A H 0.2988 -0.0168 0.0299 0.066 Uiso 1 1 calc R . . C20 C 0.3858(7) 0.0822(6) 0.0308(5) 0.057(3) Uani 1 1 d . . . H20A H 0.4350 0.0634 0.0235 0.068 Uiso 1 1 calc R . . C21 C 0.3943(6) 0.1567(6) 0.0381(5) 0.057(3) Uani 1 1 d . . . H21A H 0.4503 0.1898 0.0374 0.068 Uiso 1 1 calc R . . C22 C 0.3223(5) 0.1848(5) 0.0465(4) 0.043(2) Uani 1 1 d . . . H22A H 0.3294 0.2367 0.0504 0.051 Uiso 1 1 calc R . . C23 C 0.1634(5) 0.2527(4) 0.0183(4) 0.0303(16) Uani 1 1 d . . . C24 C 0.1401(5) 0.2444(5) -0.0485(4) 0.0393(19) Uani 1 1 d . . . H24A H 0.1090 0.1974 -0.0707 0.047 Uiso 1 1 calc R . . C25 C 0.1624(6) 0.3049(5) -0.0828(5) 0.050(2) Uani 1 1 d . . . H25A H 0.1459 0.2997 -0.1285 0.060 Uiso 1 1 calc R . . C26 C 0.2097(6) 0.3740(5) -0.0495(6) 0.061(3) Uani 1 1 d . . . H26A H 0.2256 0.4155 -0.0728 0.073 Uiso 1 1 calc R . . C27 C 0.2328(7) 0.3814(5) 0.0162(5) 0.060(3) Uani 1 1 d . . . H27A H 0.2652 0.4280 0.0384 0.072 Uiso 1 1 calc R . . C28 C 0.2095(6) 0.3217(4) 0.0506(5) 0.048(2) Uani 1 1 d . . . H28A H 0.2249 0.3275 0.0965 0.058 Uiso 1 1 calc R . . C29 C 0.2811(5) 0.1340(4) 0.2045(4) 0.0340(18) Uani 1 1 d . . . H29A H 0.2367 0.0887 0.1969 0.041 Uiso 1 1 calc R . . C30 C 0.3649(5) 0.1326(4) 0.2209(4) 0.0292(16) Uani 1 1 d . . . H30A H 0.3784 0.0866 0.2240 0.035 Uiso 1 1 calc R . . C31 C 0.4319(5) 0.1982(4) 0.2334(4) 0.0274(16) Uani 1 1 d . . . C32 C 0.4072(5) 0.2635(4) 0.2280(4) 0.0340(18) Uani 1 1 d . . . H32A H 0.4498 0.3099 0.2358 0.041 Uiso 1 1 calc R . . C33 C 0.3214(5) 0.2602(4) 0.2114(4) 0.0332(18) Uani 1 1 d . . . H33A H 0.3054 0.3052 0.2088 0.040 Uiso 1 1 calc R . . C34 C 0.5245(5) 0.1971(4) 0.2527(4) 0.0375(19) Uani 1 1 d . . . H34A H 0.5343 0.2013 0.3010 0.045 Uiso 1 1 calc R . . H34B H 0.5330 0.1489 0.2350 0.045 Uiso 1 1 calc R . . C35 C 0.6232(5) 0.3221(4) 0.2652(4) 0.0348(18) Uani 1 1 d . . . C36 C 0.6922(5) 0.3755(4) 0.2375(4) 0.0381(19) Uani 1 1 d . . . C37 C 0.7034(5) 0.4503(4) 0.2581(4) 0.040(2) Uani 1 1 d . . . H37A H 0.6675 0.4646 0.2889 0.048 Uiso 1 1 calc R . . C38 C 0.7661(5) 0.5041(5) 0.2345(5) 0.045(2) Uani 1 1 d . . . C39 C 0.8164(7) 0.4814(6) 0.1899(7) 0.076(3) Uani 1 1 d . . . H39A H 0.8593 0.5176 0.1730 0.092 Uiso 1 1 calc R . . C40 C 0.8071(7) 0.4092(7) 0.1692(6) 0.081(4) Uani 1 1 d . . . H40A H 0.8425 0.3955 0.1377 0.097 Uiso 1 1 calc R . . C41 C 0.7451(6) 0.3543(6) 0.1945(6) 0.063(3) Uani 1 1 d . . . H41A H 0.7401 0.3035 0.1818 0.076 Uiso 1 1 calc R . . C42 C 0.7775(7) 0.5843(5) 0.2522(6) 0.063(3) Uani 1 1 d . . . C43 C 0.7515(6) 0.6811(5) 0.3286(5) 0.056(3) Uani 1 1 d . . . H43A H 0.7965 0.7135 0.3064 0.068 Uiso 1 1 calc R . . H43B H 0.7700 0.6919 0.3761 0.068 Uiso 1 1 calc R . . C44 C 0.6653(6) 0.7010(5) 0.3151(5) 0.046(2) Uani 1 1 d . . . C45 C 0.6604(6) 0.7734(5) 0.3285(5) 0.058(3) Uani 1 1 d . . . H45A H 0.7112 0.8108 0.3468 0.069 Uiso 1 1 calc R . . C46 C 0.5828(6) 0.7910(5) 0.3156(5) 0.060(3) Uani 1 1 d . . . H46A H 0.5818 0.8413 0.3233 0.072 Uiso 1 1 calc R . . C49 C 0.5118(6) 0.6709(5) 0.2787(5) 0.060(3) Uani 1 1 d . . . H49A H 0.4595 0.6346 0.2614 0.072 Uiso 1 1 calc R . . C50 C 0.5882(6) 0.6500(5) 0.2886(6) 0.068(3) Uani 1 1 d . . . H50A H 0.5883 0.6000 0.2771 0.082 Uiso 1 1 calc R . . C51 C 0.3679(5) 0.7178(4) 0.1133(4) 0.0330(18) Uani 1 1 d . . . C52 C 0.3294(5) 0.6506(4) 0.1331(4) 0.0379(19) Uani 1 1 d . . . H52A H 0.3307 0.6453 0.1783 0.045 Uiso 1 1 calc R . . C53 C 0.2885(6) 0.5904(5) 0.0870(5) 0.051(2) Uani 1 1 d . . . H53A H 0.2622 0.5441 0.1010 0.061 Uiso 1 1 calc R . . C54 C 0.2860(7) 0.5970(5) 0.0228(5) 0.058(3) Uani 1 1 d . . . H54A H 0.2562 0.5558 -0.0081 0.069 Uiso 1 1 calc R . . C55 C 0.3261(8) 0.6626(5) 0.0015(5) 0.064(3) Uani 1 1 d . . . H55A H 0.3263 0.6665 -0.0439 0.076 Uiso 1 1 calc R . . C56 C 0.3663(7) 0.7235(5) 0.0470(4) 0.053(2) Uani 1 1 d . . . H56A H 0.3930 0.7693 0.0325 0.064 Uiso 1 1 calc R . . C57 C 0.5396(6) 0.8071(4) 0.1626(4) 0.0388(19) Uani 1 1 d . . . C58 C 0.5997(7) 0.8755(5) 0.1816(6) 0.066(3) Uani 1 1 d . . . H58A H 0.5795 0.9165 0.1979 0.079 Uiso 1 1 calc R . . C59 C 0.6871(7) 0.8843(6) 0.1770(6) 0.069(3) Uani 1 1 d . . . H59A H 0.7269 0.9316 0.1893 0.082 Uiso 1 1 calc R . . C60 C 0.7177(7) 0.8261(6) 0.1551(6) 0.073(3) Uani 1 1 d . . . H60A H 0.7786 0.8323 0.1522 0.088 Uiso 1 1 calc R . . C61 C 0.6591(7) 0.7581(7) 0.1371(7) 0.087(4) Uani 1 1 d . . . H61A H 0.6803 0.7170 0.1224 0.104 Uiso 1 1 calc R . . C62 C 0.5715(7) 0.7484(5) 0.1399(5) 0.062(3) Uani 1 1 d . . . H62A H 0.5321 0.7012 0.1262 0.074 Uiso 1 1 calc R . . C63 C 0.3928(6) 0.8075(5) 0.4194(5) 0.054(3) Uani 1 1 d . . . H63A H 0.4211 0.8558 0.4107 0.065 Uiso 1 1 calc R . . C64 C 0.3761(6) 0.7961(5) 0.4837(4) 0.056(3) Uani 1 1 d . . . H64A H 0.3953 0.8355 0.5182 0.067 Uiso 1 1 calc R . . C65 C 0.3312(6) 0.7266(5) 0.4962(4) 0.043(2) Uani 1 1 d . . . C66 C 0.3091(5) 0.6706(4) 0.4443(4) 0.0392(19) Uani 1 1 d . . . H66A H 0.2802 0.6218 0.4513 0.047 Uiso 1 1 calc R . . C67 C 0.3287(5) 0.6854(4) 0.3832(4) 0.0378(19) Uani 1 1 d . . . H67A H 0.3121 0.6462 0.3483 0.045 Uiso 1 1 calc R . . C68 C 0.3119(6) 0.7155(5) 0.5649(4) 0.055(3) Uani 1 1 d . . . H68A H 0.3677 0.7198 0.5919 0.066 Uiso 1 1 calc R . . H68B H 0.2869 0.7556 0.5826 0.066 Uiso 1 1 calc R . . C69 C 0.1645(5) 0.6344(4) 0.5623(4) 0.0369(19) Uani 1 1 d . . . C70 C 0.1101(5) 0.5597(4) 0.5711(4) 0.0351(18) Uani 1 1 d . . . C71 C 0.1316(6) 0.4969(4) 0.5455(4) 0.0386(19) Uani 1 1 d . . . H71A H 0.1827 0.5011 0.5234 0.046 Uiso 1 1 calc R . . C72 C 0.0785(6) 0.4276(5) 0.5519(4) 0.041(2) Uani 1 1 d . . . C73 C 0.0048(6) 0.4217(5) 0.5852(4) 0.046(2) Uani 1 1 d . . . H73A H -0.0323 0.3744 0.5891 0.055 Uiso 1 1 calc R . . C74 C -0.0145(6) 0.4849(5) 0.6125(4) 0.050(2) Uani 1 1 d . . . H74A H -0.0636 0.4809 0.6368 0.060 Uiso 1 1 calc R . . C75 C 0.0362(6) 0.5532(5) 0.6049(4) 0.043(2) Uani 1 1 d . . . H75A H 0.0212 0.5963 0.6226 0.052 Uiso 1 1 calc R . . C76 C 0.1058(7) 0.3611(5) 0.5234(4) 0.045(2) Uani 1 1 d . . . C77 C 0.0554(6) 0.2349(4) 0.4682(4) 0.045(2) Uani 1 1 d . . . H77A H 0.0022 0.1943 0.4693 0.054 Uiso 1 1 calc R . . H77B H 0.1029 0.2256 0.4975 0.054 Uiso 1 1 calc R . . C78 C 0.0813(5) 0.2320(4) 0.3997(4) 0.0369(19) Uani 1 1 d . . . C79 C 0.1017(6) 0.2913(4) 0.3663(4) 0.042(2) Uani 1 1 d . . . H79A H 0.1054 0.3393 0.3875 0.051 Uiso 1 1 calc R . . C80 C 0.1171(5) 0.2824(4) 0.3017(4) 0.0359(18) Uani 1 1 d . . . H80A H 0.1287 0.3247 0.2789 0.043 Uiso 1 1 calc R . . C81 C 0.1016(7) 0.1603(5) 0.3036(5) 0.057(3) Uani 1 1 d . . . H81A H 0.1047 0.1138 0.2829 0.068 Uiso 1 1 calc R . . C82 C 0.0817(7) 0.1651(5) 0.3671(4) 0.058(3) Uani 1 1 d . . . H82A H 0.0682 0.1219 0.3885 0.070 Uiso 1 1 calc R . . C83 C 0.2342(7) 0.8416(5) 0.3362(5) 0.061(3) Uani 1 1 d . . . C84 C 0.2703(8) 0.9122(6) 0.3673(5) 0.070(3) Uani 1 1 d . . . H84A H 0.3122 0.9467 0.3478 0.084 Uiso 1 1 calc R . . C85 C 0.2445(10) 0.9317(7) 0.4271(6) 0.091(4) Uani 1 1 d . . . H85A H 0.2665 0.9809 0.4480 0.110 Uiso 1 1 calc R . . C86 C 0.1885(10) 0.8818(7) 0.4558(7) 0.102(5) Uani 1 1 d . . . H86A H 0.1720 0.8960 0.4973 0.122 Uiso 1 1 calc R . . C87 C 0.1554(9) 0.8122(8) 0.4271(7) 0.093(4) Uani 1 1 d U . . H87A H 0.1183 0.7772 0.4494 0.111 Uiso 1 1 calc R . . C88 C 0.1746(9) 0.7911(6) 0.3660(6) 0.084(4) Uani 1 1 d . . . H88A H 0.1477 0.7429 0.3443 0.101 Uiso 1 1 calc R . . C89 C 0.1797(6) 0.7394(5) 0.2160(5) 0.046(2) Uani 1 1 d . . . C90 C 0.1701(6) 0.6662(5) 0.2307(5) 0.050(2) Uani 1 1 d . . . H90A H 0.2123 0.6555 0.2608 0.059 Uiso 1 1 calc R . . C91 C 0.1003(7) 0.6111(6) 0.2018(7) 0.076(4) Uani 1 1 d . . . H91A H 0.0926 0.5631 0.2149 0.092 Uiso 1 1 calc R . . C92 C 0.0419(8) 0.6214(9) 0.1556(7) 0.089(4) Uani 1 1 d . . . H92A H -0.0042 0.5815 0.1342 0.107 Uiso 1 1 calc R . . C93 C 0.0520(8) 0.6966(9) 0.1396(7) 0.094(4) Uani 1 1 d . . . H93A H 0.0113 0.7060 0.1075 0.112 Uiso 1 1 calc R . . C94 C 0.1188(7) 0.7535(7) 0.1700(6) 0.074(3) Uani 1 1 d . . . H94A H 0.1239 0.8024 0.1599 0.089 Uiso 1 1 calc R . . C95 C 0.4006(6) 0.8779(4) 0.1440(5) 0.048(2) Uani 1 1 d . . . H95A H 0.4380 0.9220 0.1719 0.057 Uiso 1 1 calc R . . H95B H 0.4168 0.8810 0.0989 0.057 Uiso 1 1 calc R . . C96 C 0.3085(7) 0.8802(5) 0.1444(5) 0.053(3) Uani 1 1 d . . . H96A H 0.2705 0.8335 0.1207 0.064 Uiso 1 1 calc R . . H96B H 0.2995 0.9210 0.1203 0.064 Uiso 1 1 calc R . . C97 C 0.2790(7) 0.8913(5) 0.2138(5) 0.058(3) Uani 1 1 d . . . H97A H 0.2214 0.9028 0.2096 0.069 Uiso 1 1 calc R . . H97B H 0.3216 0.9345 0.2394 0.069 Uiso 1 1 calc R . . S1SA S 0.03256(19) -0.03879(12) 0.16956(12) 0.0536(6) Uani 1 1 d . . . C1SA C 0.0103(13) -0.0642(10) 0.2466(9) 0.121(5) Uani 1 1 d U . . O1SA O 0.0814(6) -0.0821(5) 0.1410(4) 0.098(3) Uani 1 1 d U . . F1SA F -0.0353(9) -0.1372(7) 0.2434(6) 0.185(5) Uani 1 1 d U . . O2SA O 0.0678(5) 0.0370(4) 0.1765(4) 0.073(2) Uani 1 1 d U . . F2SA F -0.0341(6) -0.0254(4) 0.2790(4) 0.108(2) Uani 1 1 d U . . O3SA O -0.0623(7) -0.0553(6) 0.1372(5) 0.118(3) Uani 1 1 d U . . F3SA F 0.0855(9) -0.0513(7) 0.2821(6) 0.177(4) Uani 1 1 d U . . S1SB S 0.5107(2) 1.00403(13) 0.3388(2) 0.0839(11) Uani 1 1 d . . . C1SB C 0.6206(9) 1.0416(8) 0.3472(7) 0.085(4) Uani 1 1 d U . . O1SB O 0.4894(9) 1.0202(7) 0.2760(7) 0.154(5) Uani 1 1 d U . . F1SB F 0.6453(5) 1.1138(4) 0.3497(4) 0.116(3) Uani 1 1 d U . . O2SB O 0.4919(6) 0.9273(4) 0.3318(4) 0.086(2) Uani 1 1 d U . . F2SB F 0.6624(6) 1.0145(5) 0.3029(5) 0.135(3) Uani 1 1 d U . . O3SB O 0.4724(11) 1.0497(9) 0.3653(9) 0.201(6) Uani 1 1 d U . . F3SB F 0.6606(10) 1.0329(8) 0.3991(8) 0.217(6) Uani 1 1 d U . . S1SC S 0.26973(18) 0.48053(12) 0.26555(15) 0.0587(7) Uani 1 1 d . . . C1SC C 0.3266(11) 0.4625(6) 0.3329(7) 0.098(5) Uani 1 1 d . . . O1SC O 0.3036(5) 0.5533(3) 0.2577(4) 0.075(2) Uani 1 1 d . . . F1SC F 0.3092(7) 0.3966(4) 0.3501(5) 0.143(4) Uani 1 1 d . . . O2SC O 0.2588(6) 0.4227(5) 0.2184(4) 0.095(3) Uani 1 1 d U . . F2SC F 0.4145(7) 0.4691(8) 0.3202(7) 0.205(7) Uani 1 1 d . . . O3SC O 0.1848(9) 0.4714(7) 0.2892(7) 0.156(5) Uani 1 1 d U . . F3SC F 0.3505(8) 0.5109(6) 0.3823(5) 0.146(3) Uani 1 1 d U . . S1SD S -0.34160(15) 0.15309(12) 0.07378(12) 0.0447(5) Uani 1 1 d . . . O1SD O -0.3945(4) 0.1983(3) 0.0991(3) 0.0473(15) Uani 1 1 d . . . F1SD F -0.2947(4) 0.0415(3) 0.1155(3) 0.0787(18) Uani 1 1 d U . . C1SD C -0.3456(7) 0.0857(5) 0.1271(5) 0.055(2) Uani 1 1 d . . . O2SD O -0.2526(6) 0.1894(5) 0.0804(5) 0.095(3) Uani 1 1 d U . . F2SD F -0.4277(5) 0.0456(4) 0.1293(4) 0.105(2) Uani 1 1 d U . . F3SD F -0.3219(5) 0.1169(4) 0.1897(3) 0.088(2) Uani 1 1 d U . . O3SD O -0.3816(6) 0.1102(4) 0.0121(4) 0.081(2) Uani 1 1 d U . . C1IS C 0.3915(9) 0.4801(8) 0.5838(13) 0.034(7) Uani 0.25 1 d PDU A -2 H1IB H 0.4156 0.4899 0.6309 0.041 Uiso 0.25 1 d PR A -2 O1IS O 0.3034(8) 0.4811(7) 0.5935(7) 0.010(3) Uani 0.25 1 d PDU A -2 H1IC H 0.2973 0.4848 0.5534 0.015 Uiso 0.25 1 d PR A -2 C2IS C 0.4450(14) 0.5496(13) 0.5590(15) 0.032(7) Uani 0.25 1 d PDU A -2 H2ID H 0.4349 0.5935 0.5834 0.049 Uiso 0.25 1 calc PR A -2 H2IE H 0.4269 0.5485 0.5125 0.049 Uiso 0.25 1 calc PR A -2 H2IF H 0.5075 0.5513 0.5652 0.049 Uiso 0.25 1 calc PR A -2 C3IS C 0.4005(16) 0.4077(13) 0.5481(18) 0.048(9) Uani 0.25 1 d PD A -2 H3ID H 0.4613 0.4086 0.5622 0.072 Uiso 0.25 1 d PR A -2 H3IE H 0.3607 0.3662 0.5644 0.072 Uiso 0.25 1 d PR A -2 H3IF H 0.3914 0.4019 0.5003 0.072 Uiso 0.25 1 d PR A -2 O1IT O 0.565(2) 0.5365(15) 0.1018(16) 0.263(18) Uani 0.50 1 d PDU B -3 H1IF H 0.5645 0.5364 0.0612 0.395 Uiso 0.50 1 calc PR B -3 C1IT C 0.4937(17) 0.4792(16) 0.1161(13) 0.181(18) Uani 0.50 1 d PDU B -3 H1IA H 0.4364 0.4858 0.0976 0.217 Uiso 0.50 1 d PR B -3 C2IT C 0.502(2) 0.4007(14) 0.0964(18) 0.143(13) Uani 0.50 1 d PDU B -3 H2IA H 0.5034 0.3928 0.0491 0.215 Uiso 0.50 1 calc PR B -3 H2IB H 0.4509 0.3648 0.1087 0.215 Uiso 0.50 1 calc PR B -3 H2IC H 0.5555 0.3944 0.1189 0.215 Uiso 0.50 1 calc PR B -3 C3IT C 0.493(2) 0.4678(18) 0.1881(15) 0.131(12) Uani 0.50 1 d PDU B -3 H3IA H 0.4975 0.5153 0.2141 0.197 Uiso 0.50 1 d PR B -3 H3IB H 0.5422 0.4486 0.2019 0.197 Uiso 0.50 1 d PR B -3 H3IC H 0.4376 0.4327 0.1945 0.197 Uiso 0.50 1 d PR B -3 O1W O 0.5954(10) 0.4177(8) 0.4405(7) 0.069(4) Uani 0.50 1 d P C 1 O2W O 0.6415(11) 0.5581(9) 0.4231(8) 0.078(4) Uani 0.50 1 d PU D 1 O3W O 0.4269(11) 1.0653(9) 0.4959(7) 0.079(5) Uani 0.50 1 d P . . O4W O 0.4021(19) 0.4219(16) 0.1399(15) 0.071(8) Uiso 0.25 1 d P B 3 O5W O 0.120(3) 0.066(3) 0.558(2) 0.137(16) Uiso 0.25 1 d P E 3 H5WA H 0.1722 0.0671 0.5524 0.205 Uiso 0.25 1 d PR E 3 H5WB H 0.1133 0.1044 0.5846 0.205 Uiso 0.25 1 d PR E 3 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 0.0288(3) 0.0211(3) 0.0301(3) -0.0027(2) -0.0013(2) 0.0089(2) P1 0.0298(11) 0.0307(10) 0.0323(11) 0.0022(8) 0.0035(8) 0.0113(8) N1 0.030(3) 0.023(3) 0.026(3) 0.000(2) -0.001(3) 0.007(3) O1 0.048(4) 0.042(3) 0.041(4) 0.006(3) 0.008(3) 0.003(3) C1 0.022(4) 0.044(5) 0.045(5) 0.005(4) 0.009(3) 0.005(3) Pd2 0.0373(4) 0.0239(3) 0.0336(4) 0.0043(2) 0.0102(3) 0.0056(2) P2 0.0274(10) 0.0193(9) 0.0333(11) -0.0033(8) -0.0001(8) 0.0067(7) N2 0.037(4) 0.028(3) 0.052(4) 0.007(3) 0.014(3) 0.010(3) C2 0.035(5) 0.036(4) 0.036(5) -0.008(4) -0.001(4) 0.003(3) O2 0.143(8) 0.053(5) 0.100(7) 0.031(5) 0.053(6) 0.006(5) P3 0.0441(12) 0.0212(9) 0.0348(12) 0.0060(8) 0.0111(9) 0.0066(8) O3 0.055(4) 0.030(3) 0.059(4) -0.001(3) 0.004(3) 0.011(3) N3 0.046(5) 0.039(4) 0.065(6) 0.020(4) -0.009(4) 0.008(3) C3 0.039(5) 0.026(4) 0.032(4) -0.006(3) 0.000(3) 0.004(3) P4 0.0494(14) 0.0261(10) 0.0591(15) 0.0122(10) 0.0214(11) 0.0160(10) N4 0.042(4) 0.029(3) 0.039(4) 0.001(3) 0.001(3) 0.007(3) O4 0.054(4) 0.051(4) 0.052(4) -0.005(3) 0.000(3) 0.016(3) C4 0.043(5) 0.061(6) 0.031(5) 0.002(4) 0.004(4) 0.020(4) N5 0.046(4) 0.032(4) 0.037(4) 0.009(3) 0.008(3) 0.000(3) C5 0.037(5) 0.062(6) 0.044(5) -0.013(4) 0.012(4) 0.007(4) N6 0.046(4) 0.048(4) 0.029(4) 0.006(3) 0.005(3) 0.009(3) C6 0.057(7) 0.091(9) 0.059(7) -0.027(6) 0.017(6) 0.009(6) N7 0.049(4) 0.030(3) 0.036(4) -0.002(3) 0.010(3) 0.008(3) C7 0.050(7) 0.140(12) 0.036(6) -0.007(7) 0.015(5) 0.023(7) N8 0.040(4) 0.026(3) 0.026(3) -0.005(3) -0.004(3) 0.009(3) C8 0.073(8) 0.131(11) 0.086(9) 0.062(9) 0.044(7) 0.049(8) C9 0.069(7) 0.095(8) 0.047(6) 0.031(6) 0.027(5) 0.046(6) C10 0.038(5) 0.039(5) 0.044(5) 0.001(4) 0.005(4) 0.022(4) C11 0.053(6) 0.056(6) 0.041(5) 0.009(4) 0.008(4) 0.031(5) C12 0.082(8) 0.086(8) 0.055(7) 0.027(6) 0.019(6) 0.061(7) C13 0.104(10) 0.051(7) 0.076(8) 0.021(6) 0.023(7) 0.041(7) C14 0.081(8) 0.038(5) 0.093(9) 0.007(6) 0.000(7) 0.017(5) C16 0.066(7) 0.030(5) 0.073(7) -0.002(5) -0.017(5) 0.016(4) C17 0.038(4) 0.024(4) 0.027(4) 0.001(3) 0.007(3) 0.014(3) C18 0.047(5) 0.025(4) 0.044(5) -0.003(3) 0.013(4) 0.015(4) C19 0.077(7) 0.052(6) 0.057(6) 0.007(5) 0.022(5) 0.050(5) C20 0.052(6) 0.083(8) 0.054(6) 0.016(5) 0.025(5) 0.042(6) C21 0.041(5) 0.065(7) 0.070(7) 0.026(5) 0.017(5) 0.016(5) C22 0.027(4) 0.041(5) 0.063(6) 0.017(4) 0.013(4) 0.010(4) C23 0.029(4) 0.028(4) 0.035(4) 0.004(3) 0.001(3) 0.009(3) C24 0.033(5) 0.038(4) 0.045(5) 0.005(4) 0.000(4) 0.008(4) C25 0.052(6) 0.058(6) 0.046(6) 0.018(5) 0.002(4) 0.023(5) C26 0.051(6) 0.047(6) 0.095(9) 0.036(6) 0.013(6) 0.022(5) C27 0.079(7) 0.028(5) 0.066(7) 0.009(5) -0.006(6) 0.003(5) C28 0.071(7) 0.023(4) 0.048(5) 0.004(4) 0.000(5) 0.011(4) C29 0.038(5) 0.022(4) 0.039(5) 0.000(3) 0.002(4) 0.003(3) C30 0.033(4) 0.024(4) 0.032(4) 0.004(3) -0.001(3) 0.012(3) C31 0.028(4) 0.021(3) 0.033(4) 0.002(3) 0.001(3) 0.008(3) C32 0.035(4) 0.019(3) 0.045(5) -0.003(3) -0.005(4) 0.007(3) C33 0.034(4) 0.022(4) 0.044(5) 0.001(3) -0.001(4) 0.012(3) C34 0.031(4) 0.022(4) 0.059(6) 0.006(4) 0.004(4) 0.007(3) C35 0.031(4) 0.031(4) 0.046(5) 0.007(4) 0.002(4) 0.013(3) C36 0.024(4) 0.037(4) 0.055(6) 0.008(4) 0.005(4) 0.011(3) C37 0.035(5) 0.041(5) 0.051(5) 0.013(4) 0.004(4) 0.019(4) C38 0.028(4) 0.044(5) 0.063(6) 0.020(4) 0.003(4) 0.006(4) C39 0.050(7) 0.057(7) 0.119(11) 0.025(7) 0.027(7) -0.002(5) C40 0.059(7) 0.073(8) 0.108(10) 0.012(7) 0.050(7) 0.001(6) C41 0.036(5) 0.053(6) 0.100(9) -0.004(6) 0.021(5) 0.012(4) C42 0.053(6) 0.044(6) 0.087(9) 0.036(6) -0.008(6) -0.004(5) C43 0.050(6) 0.043(5) 0.072(7) 0.014(5) -0.020(5) 0.011(4) C44 0.038(5) 0.040(5) 0.056(6) 0.010(4) -0.005(4) 0.004(4) C45 0.042(6) 0.048(6) 0.071(7) -0.026(5) -0.005(5) 0.007(4) C46 0.051(6) 0.042(5) 0.082(8) -0.016(5) 0.006(5) 0.011(5) C49 0.052(6) 0.024(4) 0.098(8) 0.009(5) -0.021(6) 0.007(4) C50 0.055(6) 0.025(4) 0.115(10) 0.011(5) -0.030(6) 0.006(4) C51 0.037(4) 0.021(4) 0.044(5) 0.010(3) 0.012(4) 0.010(3) C52 0.038(5) 0.029(4) 0.045(5) 0.006(4) 0.008(4) 0.004(3) C53 0.056(6) 0.029(4) 0.063(7) 0.006(4) 0.009(5) 0.004(4) C54 0.074(7) 0.032(5) 0.060(7) -0.003(4) -0.011(5) 0.009(5) C55 0.102(9) 0.043(5) 0.042(6) 0.003(4) -0.007(6) 0.018(6) C56 0.086(7) 0.033(5) 0.040(5) 0.009(4) 0.004(5) 0.012(5) C57 0.054(5) 0.034(4) 0.029(4) 0.005(3) 0.017(4) 0.009(4) C58 0.061(7) 0.040(5) 0.089(8) 0.000(5) 0.034(6) -0.003(5) C59 0.053(7) 0.051(6) 0.091(9) 0.003(6) 0.025(6) -0.009(5) C60 0.047(6) 0.069(7) 0.097(9) -0.004(6) 0.029(6) 0.002(5) C61 0.047(7) 0.076(8) 0.136(12) -0.023(8) 0.026(7) 0.024(6) C62 0.055(6) 0.043(5) 0.083(8) -0.006(5) 0.013(6) 0.008(5) C63 0.063(6) 0.037(5) 0.049(6) -0.003(4) 0.019(5) -0.013(4) C64 0.063(6) 0.050(6) 0.036(5) -0.008(4) 0.016(5) -0.017(5) C65 0.040(5) 0.049(5) 0.034(5) 0.000(4) 0.005(4) 0.002(4) C66 0.048(5) 0.032(4) 0.037(5) 0.012(4) 0.007(4) 0.006(4) C67 0.041(5) 0.031(4) 0.037(5) 0.002(3) 0.004(4) 0.004(4) C68 0.051(6) 0.061(6) 0.036(5) -0.001(4) 0.012(4) -0.018(5) C69 0.039(5) 0.041(5) 0.027(4) -0.002(4) 0.005(4) 0.006(4) C70 0.043(5) 0.031(4) 0.030(4) 0.003(3) 0.008(4) 0.006(3) C71 0.049(5) 0.040(5) 0.028(4) 0.006(4) 0.016(4) 0.010(4) C72 0.058(6) 0.041(5) 0.025(4) 0.002(4) 0.003(4) 0.015(4) C73 0.055(6) 0.038(5) 0.040(5) 0.003(4) 0.010(4) 0.002(4) C74 0.052(6) 0.051(5) 0.050(6) 0.005(4) 0.031(5) 0.013(4) C75 0.048(5) 0.036(5) 0.044(5) 0.001(4) 0.018(4) 0.007(4) C76 0.065(7) 0.039(5) 0.034(5) 0.006(4) 0.009(4) 0.019(4) C77 0.074(6) 0.028(4) 0.033(5) 0.005(3) 0.007(4) 0.010(4) C78 0.043(5) 0.031(4) 0.035(5) -0.003(3) -0.001(4) 0.012(4) C79 0.068(6) 0.021(4) 0.037(5) -0.005(3) 0.009(4) 0.012(4) C80 0.048(5) 0.022(4) 0.038(5) 0.004(3) -0.002(4) 0.011(3) C81 0.102(8) 0.024(4) 0.045(6) -0.003(4) 0.006(5) 0.019(5) C82 0.112(9) 0.023(4) 0.042(6) 0.009(4) 0.013(6) 0.017(5) C83 0.082(8) 0.038(5) 0.077(7) 0.021(5) 0.048(6) 0.026(5) C84 0.092(9) 0.053(6) 0.068(7) -0.003(5) 0.037(6) 0.019(6) C85 0.151(13) 0.059(7) 0.075(9) 0.000(6) 0.055(9) 0.037(8) C86 0.167(14) 0.070(8) 0.084(9) 0.010(7) 0.087(10) 0.036(9) C87 0.099(6) 0.091(6) 0.092(6) 0.012(4) 0.037(4) 0.023(4) C88 0.118(10) 0.040(6) 0.102(10) 0.012(6) 0.074(8) 0.018(6) C89 0.044(5) 0.043(5) 0.059(6) 0.013(4) 0.011(4) 0.020(4) C90 0.040(5) 0.043(5) 0.069(7) 0.015(5) 0.014(5) 0.012(4) C91 0.047(7) 0.054(6) 0.120(11) 0.018(7) 0.013(7) -0.005(5) C92 0.040(7) 0.117(12) 0.097(10) 0.004(9) 0.006(7) 0.001(7) C93 0.049(7) 0.137(13) 0.099(11) 0.005(10) -0.011(7) 0.042(8) C94 0.050(7) 0.079(8) 0.109(10) 0.028(7) 0.008(7) 0.038(6) C95 0.069(6) 0.022(4) 0.057(6) 0.013(4) 0.026(5) 0.013(4) C96 0.079(7) 0.033(5) 0.062(6) 0.026(4) 0.018(5) 0.028(5) C97 0.081(7) 0.033(5) 0.071(7) 0.019(5) 0.028(6) 0.028(5) S1SA 0.091(2) 0.0281(11) 0.0463(14) 0.0035(10) 0.0124(13) 0.0237(12) C1SA 0.122(7) 0.117(7) 0.121(7) 0.013(5) 0.016(5) 0.029(5) O1SA 0.127(5) 0.096(4) 0.090(4) 0.013(4) 0.016(4) 0.061(4) F1SA 0.210(6) 0.165(6) 0.182(6) 0.039(4) 0.039(5) 0.038(4) O2SA 0.078(4) 0.055(3) 0.079(4) -0.002(3) 0.017(3) 0.007(3) F2SA 0.126(4) 0.111(4) 0.100(4) 0.018(3) 0.045(4) 0.044(4) O3SA 0.116(5) 0.121(5) 0.106(5) 0.010(4) 0.001(4) 0.019(4) F3SA 0.169(6) 0.208(6) 0.167(6) 0.022(4) 0.004(4) 0.076(5) S1SB 0.0688(19) 0.0268(12) 0.159(4) 0.0029(16) 0.048(2) 0.0105(12) C1SB 0.090(5) 0.082(5) 0.086(5) 0.006(4) 0.009(4) 0.028(4) O1SB 0.149(6) 0.141(6) 0.167(6) 0.030(5) -0.018(4) 0.034(4) F1SB 0.103(4) 0.084(4) 0.145(5) -0.006(4) 0.001(4) 0.008(3) O2SB 0.094(4) 0.061(4) 0.103(4) 0.017(3) 0.032(4) 0.010(3) F2SB 0.116(5) 0.130(5) 0.146(5) -0.018(4) 0.031(4) 0.019(4) O3SB 0.195(7) 0.194(7) 0.217(8) 0.011(5) 0.050(5) 0.054(5) F3SB 0.221(7) 0.227(7) 0.204(7) 0.049(5) -0.002(5) 0.057(5) S1SC 0.0611(16) 0.0250(11) 0.086(2) 0.0116(12) -0.0070(14) 0.0065(10) C1SC 0.151(14) 0.039(6) 0.079(9) 0.000(6) -0.046(9) 0.000(7) O1SC 0.103(6) 0.032(3) 0.081(5) 0.016(3) -0.011(4) 0.000(4) F1SC 0.177(9) 0.060(5) 0.181(9) 0.057(5) -0.052(7) 0.012(5) O2SC 0.117(5) 0.074(4) 0.097(4) -0.002(3) -0.014(4) 0.044(4) F2SC 0.074(7) 0.306(17) 0.236(15) 0.107(12) -0.030(8) 0.038(8) O3SC 0.139(6) 0.164(6) 0.176(6) 0.035(5) 0.026(4) 0.054(5) F3SC 0.173(5) 0.132(5) 0.137(5) 0.021(4) -0.007(4) 0.053(4) S1SD 0.0465(13) 0.0379(11) 0.0578(15) 0.0128(10) 0.0202(11) 0.0188(10) O1SD 0.049(4) 0.043(3) 0.057(4) 0.006(3) 0.010(3) 0.023(3) F1SD 0.101(4) 0.073(3) 0.081(4) 0.017(3) 0.014(3) 0.052(3) C1SD 0.056(6) 0.054(6) 0.063(7) 0.012(5) 0.007(5) 0.023(5) O2SD 0.072(4) 0.101(4) 0.123(5) 0.034(4) 0.026(4) 0.031(3) F2SD 0.101(4) 0.088(4) 0.128(4) 0.051(3) 0.014(3) 0.012(3) F3SD 0.100(4) 0.102(4) 0.073(4) 0.015(3) 0.001(3) 0.045(3) O3SD 0.111(4) 0.070(4) 0.071(4) 0.005(3) 0.007(3) 0.044(3) C1IS 0.034(7) 0.034(7) 0.034(8) 0.003(2) 0.004(2) 0.009(3) O1IS 0.010(4) 0.011(4) 0.009(4) 0.000(2) 0.002(2) 0.002(2) C2IS 0.032(8) 0.033(8) 0.034(8) 0.003(5) 0.003(5) 0.012(5) C3IS 0.024(17) 0.035(18) 0.07(3) -0.013(17) 0.014(17) -0.012(14) O1IT 0.263(19) 0.263(19) 0.262(19) 0.033(6) 0.025(5) 0.067(7) C1IT 0.178(18) 0.183(18) 0.180(18) 0.022(6) 0.019(5) 0.046(7) C2IT 0.146(14) 0.142(14) 0.143(14) 0.023(5) 0.016(5) 0.037(6) C3IT 0.126(13) 0.133(13) 0.132(13) 0.014(5) 0.017(5) 0.029(6) O1W 0.065(9) 0.092(11) 0.048(9) -0.008(8) -0.006(7) 0.024(8) O2W 0.079(6) 0.077(6) 0.077(6) 0.016(5) 0.004(4) 0.018(5) O3W 0.091(12) 0.089(11) 0.040(8) 0.014(8) -0.002(8) -0.003(9) _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 2.094(6) . ? Pd1 N8 2.115(6) . ? Pd1 P2 2.264(2) . ? Pd1 P1 2.273(2) . ? P1 C1 1.804(8) . ? P1 C10 1.804(8) . ? P1 C4 1.808(9) . ? N1 C33 1.332(9) . ? N1 C29 1.335(9) . ? O1 C35 1.237(9) . ? C1 C2 1.532(11) . ? Pd2 N4 2.087(7) . ? Pd2 N5 2.097(7) . ? Pd2 P3 2.269(2) . ? Pd2 P4 2.270(2) . ? P2 C23 1.802(8) . ? P2 C17 1.811(7) . ? P2 C3 1.816(7) . ? N2 C35 1.331(10) . ? N2 C34 1.467(10) . ? C2 C3 1.514(11) . ? O2 C42 1.221(11) . ? P3 C57 1.801(9) . ? P3 C51 1.806(8) . ? P3 C95 1.833(8) . ? O3 C69 1.228(9) . ? N3 C42 1.335(14) . ? N3 C43 1.429(11) . ? P4 C97 1.807(9) . ? P4 C89 1.813(10) . ? P4 C83 1.828(10) . ? N4 C46 1.329(11) . ? N4 C49 1.331(10) . ? O4 C76 1.220(11) . ? C4 C9 1.363(13) . ? C4 C5 1.377(12) . ? N5 C63 1.330(11) . ? N5 C67 1.340(10) . ? C5 C6 1.351(14) . ? N6 C69 1.339(10) . ? N6 C68 1.453(10) . ? C6 C7 1.366(16) . ? N7 C76 1.375(11) . ? N7 C77 1.439(10) . ? C7 C8 1.374(17) . ? N8 C80 1.323(9) . ? N8 C81 1.326(10) . ? C8 C9 1.403(14) . ? C10 C16 1.382(12) . ? C10 C11 1.388(11) . ? C11 C12 1.400(13) . ? C12 C13 1.389(16) . ? C13 C14 1.310(15) . ? C14 C16 1.381(13) . ? C17 C22 1.378(11) . ? C17 C18 1.407(10) . ? C18 C19 1.397(11) . ? C19 C20 1.376(14) . ? C20 C21 1.368(13) . ? C21 C22 1.387(12) . ? C23 C24 1.384(11) . ? C23 C28 1.394(11) . ? C24 C25 1.388(12) . ? C25 C26 1.407(14) . ? C26 C27 1.365(14) . ? C27 C28 1.377(12) . ? C29 C30 1.351(10) . ? C30 C31 1.399(10) . ? C31 C32 1.394(9) . ? C31 C34 1.496(10) . ? C32 C33 1.359(10) . ? C35 C36 1.481(11) . ? C36 C41 1.367(12) . ? C36 C37 1.394(11) . ? C37 C38 1.386(11) . ? C38 C39 1.370(14) . ? C38 C42 1.480(13) . ? C39 C40 1.352(15) . ? C40 C41 1.408(14) . ? C43 C44 1.517(12) . ? C44 C50 1.383(12) . ? C44 C45 1.388(12) . ? C45 C46 1.365(13) . ? C49 C50 1.371(13) . ? C51 C52 1.377(10) . ? C51 C56 1.386(11) . ? C52 C53 1.392(12) . ? C53 C54 1.346(13) . ? C54 C55 1.372(13) . ? C55 C56 1.389(13) . ? C57 C62 1.384(12) . ? C57 C58 1.394(12) . ? C58 C59 1.365(14) . ? C59 C60 1.359(14) . ? C60 C61 1.378(15) . ? C61 C62 1.361(14) . ? C63 C64 1.403(12) . ? C64 C65 1.383(12) . ? C65 C66 1.385(11) . ? C65 C68 1.502(12) . ? C66 C67 1.364(11) . ? C69 C70 1.489(11) . ? C70 C71 1.380(11) . ? C70 C75 1.396(11) . ? C71 C72 1.389(11) . ? C72 C73 1.388(12) . ? C72 C76 1.508(11) . ? C73 C74 1.381(12) . ? C74 C75 1.365(11) . ? C77 C78 1.506(11) . ? C78 C79 1.356(11) . ? C78 C82 1.370(11) . ? C79 C80 1.379(11) . ? C81 C82 1.376(13) . ? C83 C84 1.378(14) . ? C83 C88 1.388(13) . ? C84 C85 1.378(14) . ? C85 C86 1.341(16) . ? C86 C87 1.341(17) . ? C87 C88 1.368(16) . ? C89 C94 1.393(13) . ? C89 C90 1.415(11) . ? C90 C91 1.362(14) . ? C91 C92 1.341(16) . ? C92 C93 1.458(18) . ? C93 C94 1.364(17) . ? C95 C96 1.471(13) . ? C96 C97 1.555(13) . ? S1SA O1SA 1.381(8) . ? S1SA O2SA 1.385(7) . ? S1SA O3SA 1.540(10) . ? S1SA C1SA 1.746(19) . ? C1SA F3SA 1.305(19) . ? C1SA F2SA 1.310(18) . ? C1SA F1SA 1.377(19) . ? S1SB O3SB 1.276(16) . ? S1SB O2SB 1.390(8) . ? S1SB O1SB 1.399(13) . ? S1SB C1SB 1.696(15) . ? C1SB F3SB 1.250(17) . ? C1SB F2SB 1.308(15) . ? C1SB F1SB 1.312(14) . ? S1SC O2SC 1.356(8) . ? S1SC O1SC 1.371(6) . ? S1SC O3SC 1.443(13) . ? S1SC C1SC 1.710(13) . ? C1SC F3SC 1.266(14) . ? C1SC F1SC 1.293(12) . ? C1SC F2SC 1.414(19) . ? S1SD O2SD 1.393(9) . ? S1SD O1SD 1.428(6) . ? S1SD O3SD 1.448(8) . ? S1SD C1SD 1.756(10) . ? F1SD C1SD 1.314(10) . ? C1SD F2SD 1.337(12) . ? C1SD F3SD 1.354(11) . ? C1IS O1IS 1.431(5) . ? C1IS C2IS 1.529(5) . ? C1IS C3IS 1.531(5) . ? O1IT C1IT 1.428(5) . ? C1IT C3IT 1.527(5) . ? C1IT C2IT 1.532(5) . ? C1IT O4W 1.71(4) . ? C3IT O4W 1.67(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 N1 Pd1 N8 86.1(2) . . ? N1 Pd1 P2 92.13(17) . . ? N8 Pd1 P2 176.99(17) . . ? N1 Pd1 P1 178.59(17) . . ? N8 Pd1 P1 93.07(18) . . ? P2 Pd1 P1 88.72(7) . . ? C1 P1 C10 107.9(4) . . ? C1 P1 C4 104.1(4) . . ? C10 P1 C4 107.0(4) . . ? C1 P1 Pd1 114.7(3) . . ? C10 P1 Pd1 111.4(3) . . ? C4 P1 Pd1 111.2(3) . . ? C33 N1 C29 118.2(6) . . ? C33 N1 Pd1 119.6(5) . . ? C29 N1 Pd1 122.2(5) . . ? C2 C1 P1 114.2(5) . . ? N4 Pd2 N5 86.1(3) . . ? N4 Pd2 P3 91.29(19) . . ? N5 Pd2 P3 177.2(2) . . ? N4 Pd2 P4 178.8(2) . . ? N5 Pd2 P4 92.7(2) . . ? P3 Pd2 P4 89.91(8) . . ? C23 P2 C17 103.6(3) . . ? C23 P2 C3 107.7(4) . . ? C17 P2 C3 104.1(3) . . ? C23 P2 Pd1 114.0(3) . . ? C17 P2 Pd1 113.9(2) . . ? C3 P2 Pd1 112.7(3) . . ? C35 N2 C34 122.4(7) . . ? C3 C2 C1 113.3(7) . . ? C57 P3 C51 105.1(4) . . ? C57 P3 C95 104.2(4) . . ? C51 P3 C95 107.0(4) . . ? C57 P3 Pd2 112.3(3) . . ? C51 P3 Pd2 111.5(3) . . ? C95 P3 Pd2 115.9(3) . . ? C42 N3 C43 123.0(8) . . ? C2 C3 P2 114.0(5) . . ? C97 P4 C89 106.7(5) . . ? C97 P4 C83 104.2(4) . . ? C89 P4 C83 106.6(5) . . ? C97 P4 Pd2 115.6(3) . . ? C89 P4 Pd2 112.4(3) . . ? C83 P4 Pd2 110.6(4) . . ? C46 N4 C49 118.2(8) . . ? C46 N4 Pd2 118.8(6) . . ? C49 N4 Pd2 122.9(6) . . ? C9 C4 C5 119.7(9) . . ? C9 C4 P1 118.4(7) . . ? C5 C4 P1 121.9(7) . . ? C63 N5 C67 118.2(7) . . ? C63 N5 Pd2 119.8(6) . . ? C67 N5 Pd2 121.9(5) . . ? C6 C5 C4 121.0(10) . . ? C69 N6 C68 121.9(8) . . ? C5 C6 C7 120.2(11) . . ? C76 N7 C77 120.4(8) . . ? C6 C7 C8 120.0(10) . . ? C80 N8 C81 116.8(7) . . ? C80 N8 Pd1 124.8(5) . . ? C81 N8 Pd1 118.3(5) . . ? C7 C8 C9 119.4(11) . . ? C4 C9 C8 119.4(11) . . ? C16 C10 C11 118.4(8) . . ? C16 C10 P1 119.0(7) . . ? C11 C10 P1 122.6(7) . . ? C10 C11 C12 119.8(10) . . ? C13 C12 C11 118.7(10) . . ? C14 C13 C12 121.7(10) . . ? C13 C14 C16 120.4(11) . . ? C14 C16 C10 121.0(9) . . ? C22 C17 C18 119.3(7) . . ? C22 C17 P2 121.2(5) . . ? C18 C17 P2 119.4(6) . . ? C19 C18 C17 118.5(8) . . ? C20 C19 C18 121.7(8) . . ? C21 C20 C19 118.8(8) . . ? C20 C21 C22 121.1(9) . . ? C17 C22 C21 120.5(8) . . ? C24 C23 C28 119.9(7) . . ? C24 C23 P2 120.7(6) . . ? C28 C23 P2 118.9(6) . . ? C23 C24 C25 119.8(8) . . ? C24 C25 C26 119.6(9) . . ? C27 C26 C25 120.1(9) . . ? C26 C27 C28 120.5(9) . . ? C27 C28 C23 120.2(9) . . ? N1 C29 C30 122.1(7) . . ? C29 C30 C31 120.7(6) . . ? C32 C31 C30 116.4(7) . . ? C32 C31 C34 122.7(6) . . ? C30 C31 C34 120.9(6) . . ? C33 C32 C31 119.3(7) . . ? N1 C33 C32 123.3(7) . . ? N2 C34 C31 114.0(6) . . ? O1 C35 N2 121.7(7) . . ? O1 C35 C36 121.7(7) . . ? N2 C35 C36 116.6(7) . . ? C41 C36 C37 119.8(8) . . ? C41 C36 C35 123.0(8) . . ? C37 C36 C35 117.2(7) . . ? C38 C37 C36 121.2(8) . . ? C39 C38 C37 117.8(9) . . ? C39 C38 C42 118.9(9) . . ? C37 C38 C42 123.3(9) . . ? C40 C39 C38 122.4(10) . . ? C39 C40 C41 119.9(10) . . ? C36 C41 C40 118.9(9) . . ? O2 C42 N3 122.1(10) . . ? O2 C42 C38 120.2(12) . . ? N3 C42 C38 117.7(9) . . ? N3 C43 C44 115.3(7) . . ? C50 C44 C45 116.1(8) . . ? C50 C44 C43 123.4(8) . . ? C45 C44 C43 120.5(8) . . ? C46 C45 C44 120.2(8) . . ? N4 C46 C45 122.7(9) . . ? N4 C49 C50 121.8(8) . . ? C49 C50 C44 120.9(9) . . ? C52 C51 C56 118.7(8) . . ? C52 C51 P3 120.6(6) . . ? C56 C51 P3 120.6(6) . . ? C51 C52 C53 120.1(8) . . ? C54 C53 C52 120.7(8) . . ? C53 C54 C55 120.6(9) . . ? C54 C55 C56 119.4(9) . . ? C51 C56 C55 120.6(8) . . ? C62 C57 C58 117.9(9) . . ? C62 C57 P3 121.6(7) . . ? C58 C57 P3 120.3(7) . . ? C59 C58 C57 121.0(9) . . ? C60 C59 C58 120.6(10) . . ? C59 C60 C61 119.0(10) . . ? C62 C61 C60 121.3(10) . . ? C61 C62 C57 120.2(9) . . ? N5 C63 C64 122.2(8) . . ? C65 C64 C63 119.1(8) . . ? C64 C65 C66 117.4(8) . . ? C64 C65 C68 118.6(8) . . ? C66 C65 C68 123.9(8) . . ? C67 C66 C65 120.3(8) . . ? N5 C67 C66 122.7(8) . . ? N6 C68 C65 114.3(7) . . ? O3 C69 N6 121.6(8) . . ? O3 C69 C70 121.9(8) . . ? N6 C69 C70 116.5(7) . . ? C71 C70 C75 119.6(7) . . ? C71 C70 C69 120.6(7) . . ? C75 C70 C69 119.7(7) . . ? C70 C71 C72 120.0(8) . . ? C73 C72 C71 119.9(8) . . ? C73 C72 C76 122.6(8) . . ? C71 C72 C76 117.5(8) . . ? C74 C73 C72 119.6(8) . . ? C75 C74 C73 120.7(8) . . ? C74 C75 C70 120.1(8) . . ? O4 C76 N7 122.2(8) . . ? O4 C76 C72 122.5(8) . . ? N7 C76 C72 115.2(8) . . ? N7 C77 C78 115.2(7) . . ? C79 C78 C82 116.6(8) . . ? C79 C78 C77 124.4(7) . . ? C82 C78 C77 118.9(7) . . ? C78 C79 C80 120.4(7) . . ? N8 C80 C79 123.0(7) . . ? N8 C81 C82 122.7(8) . . ? C78 C82 C81 120.3(8) . . ? C84 C83 C88 120.0(10) . . ? C84 C83 P4 120.0(7) . . ? C88 C83 P4 119.9(8) . . ? C85 C84 C83 118.7(11) . . ? C86 C85 C84 120.4(12) . . ? C87 C86 C85 121.3(12) . . ? C86 C87 C88 120.6(13) . . ? C87 C88 C83 118.7(11) . . ? C94 C89 C90 119.2(9) . . ? C94 C89 P4 121.8(8) . . ? C90 C89 P4 119.0(7) . . ? C91 C90 C89 119.9(10) . . ? C92 C91 C90 123.0(12) . . ? C91 C92 C93 117.2(12) . . ? C94 C93 C92 121.0(11) . . ? C93 C94 C89 119.5(11) . . ? C96 C95 P3 115.0(6) . . ? C95 C96 C97 114.3(8) . . ? C96 C97 P4 114.4(6) . . ? O1SA S1SA O2SA 117.0(5) . . ? O1SA S1SA O3SA 114.0(6) . . ? O2SA S1SA O3SA 107.8(5) . . ? O1SA S1SA C1SA 109.8(7) . . ? O2SA S1SA C1SA 107.8(7) . . ? O3SA S1SA C1SA 98.8(8) . . ? F3SA C1SA F2SA 104.8(15) . . ? F3SA C1SA F1SA 110.7(16) . . ? F2SA C1SA F1SA 106.8(15) . . ? F3SA C1SA S1SA 107.1(14) . . ? F2SA C1SA S1SA 115.2(13) . . ? F1SA C1SA S1SA 112.0(13) . . ? O3SB S1SB O2SB 132.7(9) . . ? O3SB S1SB O1SB 92.5(10) . . ? O2SB S1SB O1SB 103.8(7) . . ? O3SB S1SB C1SB 110.0(9) . . ? O2SB S1SB C1SB 110.4(6) . . ? O1SB S1SB C1SB 99.7(8) . . ? F3SB C1SB F2SB 102.1(14) . . ? F3SB C1SB F1SB 100.5(13) . . ? F2SB C1SB F1SB 107.3(12) . . ? F3SB C1SB S1SB 115.3(13) . . ? F2SB C1SB S1SB 114.7(11) . . ? F1SB C1SB S1SB 115.2(10) . . ? O2SC S1SC O1SC 125.0(6) . . ? O2SC S1SC O3SC 104.6(7) . . ? O1SC S1SC O3SC 109.4(7) . . ? O2SC S1SC C1SC 107.8(6) . . ? O1SC S1SC C1SC 107.8(5) . . ? O3SC S1SC C1SC 99.2(9) . . ? F3SC C1SC F1SC 111.0(12) . . ? F3SC C1SC F2SC 91.7(12) . . ? F1SC C1SC F2SC 98.5(13) . . ? F3SC C1SC S1SC 119.8(10) . . ? F1SC C1SC S1SC 120.3(9) . . ? F2SC C1SC S1SC 108.8(11) . . ? O2SD S1SD O1SD 113.1(5) . . ? O2SD S1SD O3SD 119.1(5) . . ? O1SD S1SD O3SD 111.8(4) . . ? O2SD S1SD C1SD 102.3(5) . . ? O1SD S1SD C1SD 105.2(4) . . ? O3SD S1SD C1SD 103.3(5) . . ? F1SD C1SD F2SD 109.8(9) . . ? F1SD C1SD F3SD 106.1(8) . . ? F2SD C1SD F3SD 102.2(9) . . ? F1SD C1SD S1SD 115.0(7) . . ? F2SD C1SD S1SD 111.7(7) . . ? F3SD C1SD S1SD 111.2(7) . . ? O1IS C1IS C2IS 114.4(8) . . ? O1IS C1IS C3IS 114.4(8) . . ? C2IS C1IS C3IS 114(2) . . ? O1IT C1IT C3IT 115.1(9) . . ? O1IT C1IT C2IT 114.4(9) . . ? C3IT C1IT C2IT 92(3) . . ? O1IT C1IT O4W 171(2) . . ? C3IT C1IT O4W 61.6(18) . . ? C2IT C1IT O4W 75(2) . . ? C1IT C3IT O4W 64.8(18) . . ? C3IT O4W C1IT 53.7(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pd1 P1 C1 172(41) . . . . ? N8 Pd1 P1 C1 -132.1(3) . . . . ? P2 Pd1 P1 C1 45.4(3) . . . . ? N1 Pd1 P1 C10 49(7) . . . . ? N8 Pd1 P1 C10 104.9(3) . . . . ? P2 Pd1 P1 C10 -77.5(3) . . . . ? N1 Pd1 P1 C4 -70(7) . . . . ? N8 Pd1 P1 C4 -14.3(4) . . . . ? P2 Pd1 P1 C4 163.2(3) . . . . ? N8 Pd1 N1 C33 -84.6(6) . . . . ? P2 Pd1 N1 C33 97.9(6) . . . . ? P1 Pd1 N1 C33 -29(8) . . . . ? N8 Pd1 N1 C29 96.1(6) . . . . ? P2 Pd1 N1 C29 -81.4(6) . . . . ? P1 Pd1 N1 C29 152(7) . . . . ? C10 P1 C1 C2 64.2(7) . . . . ? C4 P1 C1 C2 177.6(6) . . . . ? Pd1 P1 C1 C2 -60.6(6) . . . . ? N1 Pd1 P2 C23 -102.4(3) . . . . ? N8 Pd1 P2 C23 -157(3) . . . . ? P1 Pd1 P2 C23 76.5(3) . . . . ? N1 Pd1 P2 C17 16.2(3) . . . . ? N8 Pd1 P2 C17 -39(3) . . . . ? P1 Pd1 P2 C17 -164.9(3) . . . . ? N1 Pd1 P2 C3 134.5(3) . . . . ? N8 Pd1 P2 C3 80(3) . . . . ? P1 Pd1 P2 C3 -46.6(3) . . . . ? P1 C1 C2 C3 68.9(8) . . . . ? N4 Pd2 P3 C57 -21.0(3) . . . . ? N5 Pd2 P3 C57 -43(4) . . . . ? P4 Pd2 P3 C57 158.9(3) . . . . ? N4 Pd2 P3 C51 96.8(3) . . . . ? N5 Pd2 P3 C51 75(4) . . . . ? P4 Pd2 P3 C51 -83.3(3) . . . . ? N4 Pd2 P3 C95 -140.6(4) . . . . ? N5 Pd2 P3 C95 -162(4) . . . . ? P4 Pd2 P3 C95 39.3(4) . . . . ? C1 C2 C3 P2 -72.1(8) . . . . ? C23 P2 C3 C2 -60.8(7) . . . . ? C17 P2 C3 C2 -170.3(6) . . . . ? Pd1 P2 C3 C2 65.8(6) . . . . ? N4 Pd2 P4 C97 134(9) . . . . ? N5 Pd2 P4 C97 140.7(4) . . . . ? P3 Pd2 P4 C97 -40.4(4) . . . . ? N4 Pd2 P4 C89 -103(9) . . . . ? N5 Pd2 P4 C89 -96.5(4) . . . . ? P3 Pd2 P4 C89 82.5(3) . . . . ? N4 Pd2 P4 C83 16(9) . . . . ? N5 Pd2 P4 C83 22.6(4) . . . . ? P3 Pd2 P4 C83 -158.4(3) . . . . ? N5 Pd2 N4 C46 -93.0(7) . . . . ? P3 Pd2 N4 C46 88.1(7) . . . . ? P4 Pd2 N4 C46 -87(9) . . . . ? N5 Pd2 N4 C49 90.9(8) . . . . ? P3 Pd2 N4 C49 -88.0(8) . . . . ? P4 Pd2 N4 C49 97(9) . . . . ? C1 P1 C4 C9 54.7(8) . . . . ? C10 P1 C4 C9 168.8(8) . . . . ? Pd1 P1 C4 C9 -69.4(8) . . . . ? C1 P1 C4 C5 -128.9(8) . . . . ? C10 P1 C4 C5 -14.8(9) . . . . ? Pd1 P1 C4 C5 107.0(7) . . . . ? N4 Pd2 N5 C63 96.8(7) . . . . ? P3 Pd2 N5 C63 119(4) . . . . ? P4 Pd2 N5 C63 -83.0(7) . . . . ? N4 Pd2 N5 C67 -86.5(7) . . . . ? P3 Pd2 N5 C67 -65(4) . . . . ? P4 Pd2 N5 C67 93.6(6) . . . . ? C9 C4 C5 C6 -1.4(14) . . . . ? P1 C4 C5 C6 -177.8(8) . . . . ? C4 C5 C6 C7 5.3(16) . . . . ? C5 C6 C7 C8 -4.2(18) . . . . ? N1 Pd1 N8 C80 103.7(6) . . . . ? P2 Pd1 N8 C80 159(3) . . . . ? P1 Pd1 N8 C80 -75.2(6) . . . . ? N1 Pd1 N8 C81 -80.3(7) . . . . ? P2 Pd1 N8 C81 -25(4) . . . . ? P1 Pd1 N8 C81 100.9(7) . . . . ? C6 C7 C8 C9 -0.7(19) . . . . ? C5 C4 C9 C8 -3.5(15) . . . . ? P1 C4 C9 C8 173.0(9) . . . . ? C7 C8 C9 C4 4.5(18) . . . . ? C1 P1 C10 C16 -159.7(7) . . . . ? C4 P1 C10 C16 88.8(8) . . . . ? Pd1 P1 C10 C16 -33.0(8) . . . . ? C1 P1 C10 C11 18.2(8) . . . . ? C4 P1 C10 C11 -93.4(8) . . . . ? Pd1 P1 C10 C11 144.9(6) . . . . ? C16 C10 C11 C12 0.8(13) . . . . ? P1 C10 C11 C12 -177.1(7) . . . . ? C10 C11 C12 C13 -2.3(14) . . . . ? C11 C12 C13 C14 1.6(17) . . . . ? C12 C13 C14 C16 0.6(19) . . . . ? C13 C14 C16 C10 -2.2(18) . . . . ? C11 C10 C16 C14 1.5(15) . . . . ? P1 C10 C16 C14 179.4(8) . . . . ? C23 P2 C17 C22 36.9(8) . . . . ? C3 P2 C17 C22 149.4(7) . . . . ? Pd1 P2 C17 C22 -87.5(7) . . . . ? C23 P2 C17 C18 -146.3(6) . . . . ? C3 P2 C17 C18 -33.7(7) . . . . ? Pd1 P2 C17 C18 89.3(6) . . . . ? C22 C17 C18 C19 -2.7(12) . . . . ? P2 C17 C18 C19 -179.6(7) . . . . ? C17 C18 C19 C20 1.8(14) . . . . ? C18 C19 C20 C21 0.7(15) . . . . ? C19 C20 C21 C22 -2.3(15) . . . . ? C18 C17 C22 C21 1.2(13) . . . . ? P2 C17 C22 C21 178.0(7) . . . . ? C20 C21 C22 C17 1.4(15) . . . . ? C17 P2 C23 C24 81.9(7) . . . . ? C3 P2 C23 C24 -28.0(7) . . . . ? Pd1 P2 C23 C24 -153.8(6) . . . . ? C17 P2 C23 C28 -90.6(7) . . . . ? C3 P2 C23 C28 159.5(6) . . . . ? Pd1 P2 C23 C28 33.7(7) . . . . ? C28 C23 C24 C25 -0.4(12) . . . . ? P2 C23 C24 C25 -172.8(6) . . . . ? C23 C24 C25 C26 1.0(13) . . . . ? C24 C25 C26 C27 -0.5(14) . . . . ? C25 C26 C27 C28 -0.5(16) . . . . ? C26 C27 C28 C23 1.2(15) . . . . ? C24 C23 C28 C27 -0.7(13) . . . . ? P2 C23 C28 C27 171.9(7) . . . . ? C33 N1 C29 C30 -2.0(11) . . . . ? Pd1 N1 C29 C30 177.3(6) . . . . ? N1 C29 C30 C31 0.9(12) . . . . ? C29 C30 C31 C32 0.0(11) . . . . ? C29 C30 C31 C34 178.9(7) . . . . ? C30 C31 C32 C33 0.1(11) . . . . ? C34 C31 C32 C33 -178.7(7) . . . . ? C29 N1 C33 C32 2.2(12) . . . . ? Pd1 N1 C33 C32 -177.1(6) . . . . ? C31 C32 C33 N1 -1.3(12) . . . . ? C35 N2 C34 C31 89.7(9) . . . . ? C32 C31 C34 N2 -33.3(11) . . . . ? C30 C31 C34 N2 147.9(7) . . . . ? C34 N2 C35 O1 -5.6(12) . . . . ? C34 N2 C35 C36 177.3(7) . . . . ? O1 C35 C36 C41 157.7(9) . . . . ? N2 C35 C36 C41 -25.2(12) . . . . ? O1 C35 C36 C37 -21.1(12) . . . . ? N2 C35 C36 C37 156.0(7) . . . . ? C41 C36 C37 C38 1.6(13) . . . . ? C35 C36 C37 C38 -179.6(7) . . . . ? C36 C37 C38 C39 0.3(13) . . . . ? C36 C37 C38 C42 176.8(8) . . . . ? C37 C38 C39 C40 -0.5(17) . . . . ? C42 C38 C39 C40 -177.1(11) . . . . ? C38 C39 C40 C41 -1(2) . . . . ? C37 C36 C41 C40 -3.2(15) . . . . ? C35 C36 C41 C40 178.0(10) . . . . ? C39 C40 C41 C36 3.0(19) . . . . ? C43 N3 C42 O2 1.8(16) . . . . ? C43 N3 C42 C38 -175.5(8) . . . . ? C39 C38 C42 O2 22.8(15) . . . . ? C37 C38 C42 O2 -153.6(10) . . . . ? C39 C38 C42 N3 -159.8(10) . . . . ? C37 C38 C42 N3 23.7(14) . . . . ? C42 N3 C43 C44 98.3(11) . . . . ? N3 C43 C44 C50 3.7(15) . . . . ? N3 C43 C44 C45 -175.6(10) . . . . ? C50 C44 C45 C46 0.0(16) . . . . ? C43 C44 C45 C46 179.3(10) . . . . ? C49 N4 C46 C45 -3.8(15) . . . . ? Pd2 N4 C46 C45 179.9(8) . . . . ? C44 C45 C46 N4 3.0(17) . . . . ? C46 N4 C49 C50 1.6(15) . . . . ? Pd2 N4 C49 C50 177.7(8) . . . . ? N4 C49 C50 C44 1.4(18) . . . . ? C45 C44 C50 C49 -2.1(16) . . . . ? C43 C44 C50 C49 178.6(10) . . . . ? C57 P3 C51 C52 107.8(7) . . . . ? C95 P3 C51 C52 -141.8(7) . . . . ? Pd2 P3 C51 C52 -14.2(7) . . . . ? C57 P3 C51 C56 -68.4(8) . . . . ? C95 P3 C51 C56 42.0(8) . . . . ? Pd2 P3 C51 C56 169.7(6) . . . . ? C56 C51 C52 C53 -1.1(12) . . . . ? P3 C51 C52 C53 -177.4(6) . . . . ? C51 C52 C53 C54 -0.1(14) . . . . ? C52 C53 C54 C55 2.1(15) . . . . ? C53 C54 C55 C56 -2.7(17) . . . . ? C52 C51 C56 C55 0.5(14) . . . . ? P3 C51 C56 C55 176.7(8) . . . . ? C54 C55 C56 C51 1.5(16) . . . . ? C51 P3 C57 C62 -27.5(9) . . . . ? C95 P3 C57 C62 -139.8(8) . . . . ? Pd2 P3 C57 C62 94.0(8) . . . . ? C51 P3 C57 C58 156.2(8) . . . . ? C95 P3 C57 C58 43.9(9) . . . . ? Pd2 P3 C57 C58 -82.3(8) . . . . ? C62 C57 C58 C59 0.8(16) . . . . ? P3 C57 C58 C59 177.2(9) . . . . ? C57 C58 C59 C60 -1.3(19) . . . . ? C58 C59 C60 C61 0(2) . . . . ? C59 C60 C61 C62 1(2) . . . . ? C60 C61 C62 C57 -2(2) . . . . ? C58 C57 C62 C61 0.6(16) . . . . ? P3 C57 C62 C61 -175.8(10) . . . . ? C67 N5 C63 C64 1.5(14) . . . . ? Pd2 N5 C63 C64 178.3(8) . . . . ? N5 C63 C64 C65 -3.0(16) . . . . ? C63 C64 C65 C66 3.3(14) . . . . ? C63 C64 C65 C68 -178.6(9) . . . . ? C64 C65 C66 C67 -2.3(13) . . . . ? C68 C65 C66 C67 179.7(9) . . . . ? C63 N5 C67 C66 -0.5(13) . . . . ? Pd2 N5 C67 C66 -177.2(6) . . . . ? C65 C66 C67 N5 0.9(13) . . . . ? C69 N6 C68 C65 -84.6(10) . . . . ? C64 C65 C68 N6 169.6(9) . . . . ? C66 C65 C68 N6 -12.4(14) . . . . ? C68 N6 C69 O3 -0.1(12) . . . . ? C68 N6 C69 C70 -179.1(7) . . . . ? O3 C69 C70 C71 137.7(8) . . . . ? N6 C69 C70 C71 -43.3(11) . . . . ? O3 C69 C70 C75 -41.6(11) . . . . ? N6 C69 C70 C75 137.4(8) . . . . ? C75 C70 C71 C72 1.6(12) . . . . ? C69 C70 C71 C72 -177.7(7) . . . . ? C70 C71 C72 C73 -1.1(13) . . . . ? C70 C71 C72 C76 -179.6(8) . . . . ? C71 C72 C73 C74 -1.0(13) . . . . ? C76 C72 C73 C74 177.3(8) . . . . ? C72 C73 C74 C75 2.7(14) . . . . ? C73 C74 C75 C70 -2.1(14) . . . . ? C71 C70 C75 C74 0.0(13) . . . . ? C69 C70 C75 C74 179.3(8) . . . . ? C77 N7 C76 O4 6.2(12) . . . . ? C77 N7 C76 C72 -175.8(7) . . . . ? C73 C72 C76 O4 -141.1(9) . . . . ? C71 C72 C76 O4 37.3(12) . . . . ? C73 C72 C76 N7 40.9(11) . . . . ? C71 C72 C76 N7 -140.7(8) . . . . ? C76 N7 C77 C78 -86.4(10) . . . . ? N7 C77 C78 C79 10.5(13) . . . . ? N7 C77 C78 C82 -167.1(9) . . . . ? C82 C78 C79 C80 3.4(13) . . . . ? C77 C78 C79 C80 -174.2(8) . . . . ? C81 N8 C80 C79 -1.1(12) . . . . ? Pd1 N8 C80 C79 175.1(6) . . . . ? C78 C79 C80 N8 -2.8(13) . . . . ? C80 N8 C81 C82 4.2(14) . . . . ? Pd1 N8 C81 C82 -172.2(8) . . . . ? C79 C78 C82 C81 -0.4(15) . . . . ? C77 C78 C82 C81 177.4(9) . . . . ? N8 C81 C82 C78 -3.5(17) . . . . ? C97 P4 C83 C84 -41.5(11) . . . . ? C89 P4 C83 C84 -154.1(9) . . . . ? Pd2 P4 C83 C84 83.4(9) . . . . ? C97 P4 C83 C88 142.5(10) . . . . ? C89 P4 C83 C88 29.9(11) . . . . ? Pd2 P4 C83 C88 -92.6(10) . . . . ? C88 C83 C84 C85 -1.5(18) . . . . ? P4 C83 C84 C85 -177.6(10) . . . . ? C83 C84 C85 C86 3(2) . . . . ? C84 C85 C86 C87 -1(2) . . . . ? C85 C86 C87 C88 -3(2) . . . . ? C86 C87 C88 C83 5(2) . . . . ? C84 C83 C88 C87 -2.4(19) . . . . ? P4 C83 C88 C87 173.6(10) . . . . ? C97 P4 C89 C94 -15.5(10) . . . . ? C83 P4 C89 C94 95.4(9) . . . . ? Pd2 P4 C89 C94 -143.3(8) . . . . ? C97 P4 C89 C90 165.5(7) . . . . ? C83 P4 C89 C90 -83.6(8) . . . . ? Pd2 P4 C89 C90 37.7(8) . . . . ? C94 C89 C90 C91 -2.3(15) . . . . ? P4 C89 C90 C91 176.8(8) . . . . ? C89 C90 C91 C92 4.8(18) . . . . ? C90 C91 C92 C93 -4(2) . . . . ? C91 C92 C93 C94 1(2) . . . . ? C92 C93 C94 C89 1.5(19) . . . . ? C90 C89 C94 C93 -0.8(16) . . . . ? P4 C89 C94 C93 -179.8(9) . . . . ? C57 P3 C95 C96 177.5(7) . . . . ? C51 P3 C95 C96 66.5(8) . . . . ? Pd2 P3 C95 C96 -58.5(8) . . . . ? P3 C95 C96 C97 69.7(9) . . . . ? C95 C96 C97 P4 -70.3(10) . . . . ? C89 P4 C97 C96 -67.0(8) . . . . ? C83 P4 C97 C96 -179.6(8) . . . . ? Pd2 P4 C97 C96 58.8(9) . . . . ? O1SA S1SA C1SA F3SA 62.4(14) . . . . ? O2SA S1SA C1SA F3SA -66.2(14) . . . . ? O3SA S1SA C1SA F3SA -178.1(12) . . . . ? O1SA S1SA C1SA F2SA 178.4(12) . . . . ? O2SA S1SA C1SA F2SA 49.9(15) . . . . ? O3SA S1SA C1SA F2SA -62.1(14) . . . . ? O1SA S1SA C1SA F1SA -59.2(15) . . . . ? O2SA S1SA C1SA F1SA 172.2(12) . . . . ? O3SA S1SA C1SA F1SA 60.2(14) . . . . ? O3SB S1SB C1SB F3SB 86.8(16) . . . . ? O2SB S1SB C1SB F3SB -68.1(15) . . . . ? O1SB S1SB C1SB F3SB -176.9(14) . . . . ? O3SB S1SB C1SB F2SB -154.9(13) . . . . ? O2SB S1SB C1SB F2SB 50.2(13) . . . . ? O1SB S1SB C1SB F2SB -58.6(13) . . . . ? O3SB S1SB C1SB F1SB -29.6(15) . . . . ? O2SB S1SB C1SB F1SB 175.5(10) . . . . ? O1SB S1SB C1SB F1SB 66.7(13) . . . . ? O2SC S1SC C1SC F3SC 175.0(14) . . . . ? O1SC S1SC C1SC F3SC 37.7(17) . . . . ? O3SC S1SC C1SC F3SC -76.2(16) . . . . ? O2SC S1SC C1SC F1SC -40.6(17) . . . . ? O1SC S1SC C1SC F1SC -178.0(14) . . . . ? O3SC S1SC C1SC F1SC 68.1(16) . . . . ? O2SC S1SC C1SC F2SC 71.7(11) . . . . ? O1SC S1SC C1SC F2SC -65.7(11) . . . . ? O3SC S1SC C1SC F2SC -179.6(11) . . . . ? O2SD S1SD C1SD F1SD -56.1(9) . . . . ? O1SD S1SD C1SD F1SD -174.5(7) . . . . ? O3SD S1SD C1SD F1SD 68.1(9) . . . . ? O2SD S1SD C1SD F2SD 178.0(8) . . . . ? O1SD S1SD C1SD F2SD 59.6(8) . . . . ? O3SD S1SD C1SD F2SD -57.8(9) . . . . ? O2SD S1SD C1SD F3SD 64.5(8) . . . . ? O1SD S1SD C1SD F3SD -53.9(8) . . . . ? O3SD S1SD C1SD F3SD -171.3(7) . . . . ? O1IT C1IT C3IT O4W 170(2) . . . . ? C2IT C1IT C3IT O4W -71(2) . . . . ? O1IT C1IT O4W C3IT -71(13) . . . . ? C2IT C1IT O4W C3IT 101(3) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 2.423 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.177 #===END data_pd324b_0m _database_code_depnum_ccdc_archive 'CCDC 624784' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H86 Cl2 F12 Fe2 N8 O17 P4 Pd2 S4' _chemical_formula_weight 2535.28 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' Cl Cl 0.1484 0.1585 '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 15.828(3) _cell_length_b 16.901(3) _cell_length_c 20.704(4) _cell_angle_alpha 71.936(4) _cell_angle_beta 86.141(4) _cell_angle_gamma 87.923(4) _cell_volume 5252.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7942 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 30.51 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.603 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.866473 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55822 _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_sigmaI/netI 0.1111 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 29.00 _reflns_number_total 25830 _reflns_number_gt 17616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.1259P)^2^+51.2008P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 25830 _refine_ls_number_parameters 1371 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.1402 _refine_ls_R_factor_gt 0.0973 _refine_ls_wR_factor_ref 0.2967 _refine_ls_wR_factor_gt 0.2504 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8492(4) 0.9682(5) 0.6949(4) 0.0295(15) Uani 1 1 d . . . H1A H 0.8315 0.9696 0.7393 0.035 Uiso 1 1 calc R . . Fe1 Fe 0.69593(6) 1.31241(7) 0.72405(7) 0.0300(3) Uani 1 1 d . . . N1 N 0.8101(3) 1.0186(4) 0.6414(3) 0.0229(12) Uani 1 1 d . . . O1 O 0.9838(4) 0.7056(5) 0.7115(4) 0.0504(17) Uani 1 1 d . . . P1 P 0.81661(10) 1.19919(12) 0.64626(10) 0.0217(3) Uani 1 1 d . . . Pd1 Pd 0.71477(3) 1.10179(4) 0.65455(3) 0.02193(14) Uani 1 1 d . . . C2 C 0.9136(4) 0.9150(5) 0.6877(4) 0.0285(15) Uani 1 1 d . . . H2A H 0.9402 0.8806 0.7266 0.034 Uiso 1 1 calc R . . Fe2 Fe 0.81603(6) 0.69020(7) 1.28615(6) 0.0281(2) Uani 1 1 d . . . N2 N 1.0620(3) 0.8221(4) 0.6681(3) 0.0281(13) Uani 1 1 d . . . H2B H 1.1083 0.8477 0.6710 0.034 Uiso 1 1 calc R . . O2 O 0.5693(4) 0.6702(5) 0.7701(5) 0.0551(19) Uani 1 1 d . . . P2 P 0.59633(10) 1.18336(12) 0.66158(10) 0.0229(4) Uani 1 1 d . . . Pd2 Pd 0.81496(3) 0.65211(3) 1.08939(3) 0.02322(14) Uani 1 1 d . . . C3 C 0.9401(4) 0.9113(5) 0.6231(4) 0.0261(14) Uani 1 1 d . . . N3 N 1.0796(4) 0.7358(5) 0.7767(4) 0.0340(15) Uani 1 1 d . . . H3A H 1.1151 0.7724 0.7812 0.041 Uiso 1 1 calc R . . P3 P 0.92705(10) 0.66757(13) 1.14927(10) 0.0249(4) Uani 1 1 d . . . C4 C 0.8960(4) 0.9615(5) 0.5669(4) 0.0249(14) Uani 1 1 d . . . H4A H 0.9094 0.9592 0.5221 0.030 Uiso 1 1 calc R . . N4 N 0.8998(4) 0.6622(4) 1.0045(3) 0.0245(12) Uani 1 1 d . . . P4 P 0.70733(10) 0.64241(12) 1.17194(11) 0.0249(4) Uani 1 1 d . . . C5 C 0.8329(4) 1.0137(5) 0.5799(4) 0.0264(15) Uani 1 1 d . . . H5A H 0.8039 1.0484 0.5425 0.032 Uiso 1 1 calc R . . N5 N 0.7245(4) 0.6274(4) 1.0285(4) 0.0271(13) Uani 1 1 d . . . C6 C 1.0119(4) 0.8545(5) 0.6102(4) 0.0288(15) Uani 1 1 d . . . H6A H 0.9878 0.8076 0.5987 0.035 Uiso 1 1 calc R . . H6B H 1.0487 0.8860 0.5707 0.035 Uiso 1 1 calc R . . N6 N 0.4906(5) 0.6354(5) 0.8701(5) 0.048(2) Uani 1 1 d . . . H6C H 0.4439 0.6445 0.8925 0.058 Uiso 1 1 calc R . . C7 C 1.0382(5) 0.7519(5) 0.7184(5) 0.0340(17) Uani 1 1 d . . . N7 N 0.4546(5) 0.7496(5) 0.7824(5) 0.0427(18) Uani 1 1 d . . . H7A H 0.4143 0.7608 0.8099 0.051 Uiso 1 1 calc R . . C8 C 1.0659(5) 0.6602(6) 0.8305(5) 0.0380(19) Uani 1 1 d . . . H8A H 1.1212 0.6395 0.8493 0.046 Uiso 1 1 calc R . . H8B H 1.0450 0.6186 0.8109 0.046 Uiso 1 1 calc R . . N8 N 0.6321(3) 1.0026(4) 0.6704(4) 0.0279(13) Uani 1 1 d . . . C9 C 1.0042(4) 0.6643(5) 0.8891(4) 0.0287(15) Uani 1 1 d . . . C10 C 0.9728(5) 0.5911(5) 0.9338(4) 0.0316(16) Uani 1 1 d . . . H10A H 0.9872 0.5397 0.9259 0.038 Uiso 1 1 calc R . . C11 C 0.9213(5) 0.5918(5) 0.9892(5) 0.0318(16) Uani 1 1 d . . . H11A H 0.8997 0.5405 1.0183 0.038 Uiso 1 1 calc R . . C12 C 0.9270(5) 0.7335(5) 0.9592(4) 0.0300(15) Uani 1 1 d . . . H12A H 0.9093 0.7845 0.9666 0.036 Uiso 1 1 calc R . . C13 C 0.9791(5) 0.7368(5) 0.9026(4) 0.0322(16) Uani 1 1 d . . . H13A H 0.9978 0.7889 0.8728 0.039 Uiso 1 1 calc R . . C14 C 0.7082(4) 0.5493(5) 1.0329(5) 0.0301(16) Uani 1 1 d . . . H14A H 0.7356 0.5051 1.0655 0.036 Uiso 1 1 calc R . . C15 C 0.6521(5) 0.5305(5) 0.9910(5) 0.0338(18) Uani 1 1 d . . . H15A H 0.6418 0.4741 0.9953 0.041 Uiso 1 1 calc R . . C16 C 0.6115(5) 0.5928(5) 0.9437(5) 0.0343(18) Uani 1 1 d . . . C17 C 0.6300(5) 0.6740(5) 0.9395(5) 0.0333(17) Uani 1 1 d . . . H17A H 0.6029 0.7191 0.9076 0.040 Uiso 1 1 calc R . . C18 C 0.6874(5) 0.6899(5) 0.9814(4) 0.0292(15) Uani 1 1 d . . . H18A H 0.7007 0.7458 0.9768 0.035 Uiso 1 1 calc R . . C19 C 0.5486(6) 0.5698(6) 0.9007(6) 0.043(2) Uani 1 1 d . . . H19A H 0.5803 0.5524 0.8644 0.051 Uiso 1 1 calc R . . H19B H 0.5160 0.5214 0.9297 0.051 Uiso 1 1 calc R . . C20 C 0.5097(5) 0.6820(6) 0.8066(6) 0.042(2) Uani 1 1 d . . . C21 C 0.4633(5) 0.7999(5) 0.7142(6) 0.042(2) Uani 1 1 d . . . H21A H 0.4068 0.8228 0.6996 0.051 Uiso 1 1 calc R . . H21B H 0.4830 0.7644 0.6859 0.051 Uiso 1 1 calc R . . C22 C 0.5237(5) 0.8714(5) 0.7003(6) 0.041(2) Uani 1 1 d . . . C23 C 0.5391(5) 0.9194(6) 0.6350(5) 0.039(2) Uani 1 1 d . . . H23A H 0.5123 0.9078 0.5993 0.047 Uiso 1 1 calc R . . C24 C 0.5935(4) 0.9845(6) 0.6206(5) 0.0327(18) Uani 1 1 d . . . H24A H 0.6043 1.0176 0.5746 0.039 Uiso 1 1 calc R . . C25 C 0.6192(4) 0.9541(5) 0.7351(5) 0.0292(16) Uani 1 1 d . . . H25A H 0.6482 0.9659 0.7696 0.035 Uiso 1 1 calc R . . C26 C 0.5652(4) 0.8880(5) 0.7529(5) 0.0324(17) Uani 1 1 d . . . H26A H 0.5561 0.8546 0.7989 0.039 Uiso 1 1 calc R . . C27 C 0.8024(4) 1.2501(5) 0.7104(4) 0.0279(16) Uani 1 1 d . . . C28 C 0.7588(4) 1.2091(5) 0.7754(4) 0.0304(16) Uani 1 1 d . . . H28A H 0.7367 1.1511 0.7906 0.036 Uiso 1 1 calc R . . C29 C 0.7532(5) 1.2667(7) 0.8140(5) 0.045(2) Uani 1 1 d . . . H29A H 0.7247 1.2563 0.8605 0.054 Uiso 1 1 calc R . . C30 C 0.7928(5) 1.3402(7) 0.7753(6) 0.046(2) Uani 1 1 d . . . H30A H 0.7960 1.3917 0.7891 0.055 Uiso 1 1 calc R . . C31 C 0.8231(4) 1.3318(6) 0.7108(5) 0.038(2) Uani 1 1 d . . . H31A H 0.8526 1.3755 0.6727 0.045 Uiso 1 1 calc R . . C32 C 0.6414(4) 1.3523(5) 0.6333(5) 0.0338(18) Uani 1 1 d . . . H32A H 0.6696 1.3566 0.5877 0.041 Uiso 1 1 calc R . . C33 C 0.5994(4) 1.2801(5) 0.6795(4) 0.0257(14) Uani 1 1 d . . . C34 C 0.5673(4) 1.3016(5) 0.7386(5) 0.0330(18) Uani 1 1 d . . . H34A H 0.5358 1.2639 0.7794 0.040 Uiso 1 1 calc R . . C35 C 0.5899(5) 1.3862(6) 0.7293(5) 0.039(2) Uani 1 1 d . . . H35A H 0.5778 1.4176 0.7627 0.047 Uiso 1 1 calc R . . C36 C 0.6349(5) 1.4160(6) 0.6651(6) 0.043(2) Uani 1 1 d . . . H36A H 0.6601 1.4725 0.6459 0.052 Uiso 1 1 calc R . . C37 C 0.9207(4) 1.1495(4) 0.6617(4) 0.0232(13) Uani 1 1 d . . . C38 C 0.9420(4) 1.1104(5) 0.7274(4) 0.0320(16) Uani 1 1 d . . . H38A H 0.9037 1.1116 0.7644 0.038 Uiso 1 1 calc R . . C39 C 1.0200(5) 1.0690(5) 0.7396(5) 0.0342(17) Uani 1 1 d . . . H39A H 1.0351 1.0423 0.7850 0.041 Uiso 1 1 calc R . . C40 C 1.0753(4) 1.0670(5) 0.6855(5) 0.0349(18) Uani 1 1 d . . . H40A H 1.1277 1.0376 0.6941 0.042 Uiso 1 1 calc R . . C41 C 1.0555(4) 1.1070(5) 0.6191(5) 0.0347(18) Uani 1 1 d . . . H41A H 1.0948 1.1064 0.5825 0.042 Uiso 1 1 calc R . . C42 C 0.9776(4) 1.1482(5) 0.6062(4) 0.0284(15) Uani 1 1 d . . . H42A H 0.9629 1.1751 0.5608 0.034 Uiso 1 1 calc R . . C43 C 0.8313(4) 1.2714(5) 0.5622(4) 0.0290(15) Uani 1 1 d . . . C44 C 0.8856(7) 1.3400(7) 0.5469(6) 0.049(2) Uani 1 1 d . . . H44A H 0.9060 1.3566 0.5828 0.059 Uiso 1 1 calc R . . C45 C 0.9095(9) 1.3836(8) 0.4796(7) 0.066(3) Uani 1 1 d . . . H45A H 0.9473 1.4288 0.4695 0.079 Uiso 1 1 calc R . . C46 C 0.8779(9) 1.3607(9) 0.4283(7) 0.071(4) Uani 1 1 d . . . H46A H 0.8925 1.3926 0.3826 0.085 Uiso 1 1 calc R . . C47 C 0.8252(8) 1.2926(7) 0.4398(6) 0.056(3) Uani 1 1 d . . . H47A H 0.8066 1.2764 0.4031 0.067 Uiso 1 1 calc R . . C48 C 0.8007(6) 1.2486(7) 0.5079(5) 0.043(2) Uani 1 1 d . . . H48A H 0.7632 1.2032 0.5174 0.052 Uiso 1 1 calc R . . C49 C 0.5460(4) 1.2150(5) 0.5811(4) 0.0252(14) Uani 1 1 d . . . C50 C 0.5796(4) 1.1928(5) 0.5251(4) 0.0302(16) Uani 1 1 d . . . H50A H 0.6295 1.1590 0.5291 0.036 Uiso 1 1 calc R . . C51 C 0.5415(5) 1.2193(6) 0.4641(5) 0.0387(19) Uani 1 1 d . . . H51A H 0.5653 1.2035 0.4265 0.046 Uiso 1 1 calc R . . C52 C 0.4688(5) 1.2687(6) 0.4568(5) 0.041(2) Uani 1 1 d . . . H52A H 0.4423 1.2869 0.4147 0.049 Uiso 1 1 calc R . . C53 C 0.4358(5) 1.2909(6) 0.5128(5) 0.041(2) Uani 1 1 d . . . H53A H 0.3855 1.3241 0.5086 0.049 Uiso 1 1 calc R . . C54 C 0.4730(4) 1.2669(5) 0.5732(4) 0.0314(16) Uani 1 1 d . . . H54A H 0.4500 1.2849 0.6100 0.038 Uiso 1 1 calc R . . C55 C 0.5197(4) 1.1212(5) 0.7249(4) 0.0249(14) Uani 1 1 d . . . C56 C 0.5360(4) 1.0974(5) 0.7932(4) 0.0310(16) Uani 1 1 d . . . H56A H 0.5850 1.1174 0.8067 0.037 Uiso 1 1 calc R . . C57 C 0.4819(5) 1.0447(5) 0.8426(5) 0.0348(17) Uani 1 1 d . . . H57A H 0.4928 1.0295 0.8895 0.042 Uiso 1 1 calc R . . C58 C 0.4107(5) 1.0146(5) 0.8208(5) 0.0345(18) Uani 1 1 d . . . H58A H 0.3731 0.9783 0.8535 0.041 Uiso 1 1 calc R . . C59 C 0.3949(4) 1.0368(5) 0.7536(5) 0.0351(18) Uani 1 1 d . . . H59A H 0.3462 1.0161 0.7402 0.042 Uiso 1 1 calc R . . C60 C 0.4485(4) 1.0890(5) 0.7045(4) 0.0287(15) Uani 1 1 d . . . H60A H 0.4376 1.1030 0.6577 0.034 Uiso 1 1 calc R . . C61 C 0.9167(4) 0.6519(5) 1.2395(4) 0.0272(15) Uani 1 1 d . . . C62 C 0.9433(4) 0.7101(6) 1.2712(5) 0.0329(17) Uani 1 1 d . . . H62A H 0.9711 0.7646 1.2478 0.039 Uiso 1 1 calc R . . C63 C 0.9220(4) 0.6765(6) 1.3429(5) 0.0363(19) Uani 1 1 d . . . H63A H 0.9308 0.7042 1.3781 0.044 Uiso 1 1 calc R . . C64 C 0.8823(5) 0.5986(6) 1.3546(5) 0.0401(19) Uani 1 1 d . . . H64A H 0.8591 0.5620 1.3997 0.048 Uiso 1 1 calc R . . C65 C 0.8786(5) 0.5832(5) 1.2916(5) 0.0321(17) Uani 1 1 d . . . H65A H 0.8545 0.5328 1.2846 0.039 Uiso 1 1 calc R . . C66 C 0.7491(4) 0.7795(6) 1.2188(5) 0.037(2) Uani 1 1 d . . . H66A H 0.7712 0.8155 1.1732 0.044 Uiso 1 1 calc R . . C67 C 0.7489(5) 0.7988(7) 1.2803(6) 0.049(3) Uani 1 1 d . . . H67A H 0.7718 0.8503 1.2863 0.059 Uiso 1 1 calc R . . C68 C 0.7126(5) 0.7306(8) 1.3328(7) 0.059(3) Uani 1 1 d . . . H68A H 0.7056 0.7261 1.3822 0.070 Uiso 1 1 calc R . . C69 C 0.6901(5) 0.6689(7) 1.3038(6) 0.046(2) Uani 1 1 d . . . H69A H 0.6634 0.6144 1.3288 0.055 Uiso 1 1 calc R . . C70 C 0.7140(4) 0.6978(5) 1.2332(5) 0.0341(19) Uani 1 1 d . . . C71 C 1.0171(4) 0.5983(6) 1.1428(5) 0.0341(18) Uani 1 1 d . . . C72 C 1.0747(5) 0.6181(7) 1.0862(5) 0.041(2) Uani 1 1 d . . . H72A H 1.0654 0.6655 1.0480 0.049 Uiso 1 1 calc R . . C73 C 1.1469(5) 0.5664(8) 1.0868(7) 0.054(3) Uani 1 1 d . . . H73A H 1.1869 0.5800 1.0488 0.065 Uiso 1 1 calc R . . C74 C 1.1608(5) 0.4974(7) 1.1406(7) 0.050(3) Uani 1 1 d . . . H74A H 1.2094 0.4631 1.1397 0.061 Uiso 1 1 calc R . . C75 C 1.1049(6) 0.4778(7) 1.1956(7) 0.052(3) Uani 1 1 d . . . H75A H 1.1147 0.4304 1.2336 0.062 Uiso 1 1 calc R . . C76 C 1.0324(5) 0.5284(6) 1.1958(6) 0.040(2) Uani 1 1 d . . . H76A H 0.9928 0.5135 1.2340 0.048 Uiso 1 1 calc R . . C77 C 0.9641(5) 0.7721(5) 1.1151(4) 0.0316(16) Uani 1 1 d . . . C78 C 1.0468(5) 0.7907(6) 1.1268(4) 0.0361(18) Uani 1 1 d . . . H78A H 1.0852 0.7470 1.1472 0.043 Uiso 1 1 calc R . . C79 C 1.0719(6) 0.8722(6) 1.1086(5) 0.044(2) Uani 1 1 d . . . H79A H 1.1281 0.8849 1.1150 0.052 Uiso 1 1 calc R . . C80 C 1.0146(7) 0.9352(6) 1.0811(5) 0.050(3) Uani 1 1 d . . . H80A H 1.0312 0.9914 1.0705 0.060 Uiso 1 1 calc R . . C81 C 0.9327(8) 0.9182(6) 1.0683(6) 0.053(3) Uani 1 1 d . . . H81A H 0.8942 0.9624 1.0489 0.064 Uiso 1 1 calc R . . C82 C 0.9083(6) 0.8364(6) 1.0844(5) 0.0384(19) Uani 1 1 d . . . H82A H 0.8536 0.8240 1.0744 0.046 Uiso 1 1 calc R . . C83 C 0.6888(4) 0.5345(5) 1.2183(4) 0.0295(16) Uani 1 1 d . . . C84 C 0.7489(5) 0.4738(5) 1.2143(5) 0.0323(17) Uani 1 1 d . . . H84A H 0.7991 0.4891 1.1858 0.039 Uiso 1 1 calc R . . C85 C 0.7359(5) 0.3904(5) 1.2519(5) 0.0357(18) Uani 1 1 d . . . H85A H 0.7772 0.3491 1.2491 0.043 Uiso 1 1 calc R . . C86 C 0.6628(6) 0.3682(6) 1.2932(6) 0.045(2) Uani 1 1 d . . . H86A H 0.6542 0.3114 1.3183 0.054 Uiso 1 1 calc R . . C87 C 0.6028(5) 0.4260(7) 1.2988(6) 0.052(3) Uani 1 1 d . . . H87A H 0.5530 0.4096 1.3276 0.062 Uiso 1 1 calc R . . C88 C 0.6155(5) 0.5108(6) 1.2612(6) 0.041(2) Uani 1 1 d . . . H88A H 0.5744 0.5516 1.2651 0.049 Uiso 1 1 calc R . . C89 C 0.6095(4) 0.6821(5) 1.1299(5) 0.0303(16) Uani 1 1 d . . . C90 C 0.5506(5) 0.6283(6) 1.1197(5) 0.0358(19) Uani 1 1 d . . . H90A H 0.5576 0.5696 1.1376 0.043 Uiso 1 1 calc R . . C91 C 0.4805(5) 0.6638(6) 1.0822(5) 0.039(2) Uani 1 1 d . . . H91A H 0.4398 0.6282 1.0744 0.047 Uiso 1 1 calc R . . C92 C 0.4691(5) 0.7478(6) 1.0565(5) 0.040(2) Uani 1 1 d . . . H92A H 0.4212 0.7704 1.0313 0.049 Uiso 1 1 calc R . . C93 C 0.5287(5) 0.8002(5) 1.0676(5) 0.0345(18) Uani 1 1 d . . . H93A H 0.5217 0.8589 1.0497 0.041 Uiso 1 1 calc R . . C94 C 0.5975(4) 0.7672(5) 1.1046(5) 0.0314(16) Uani 1 1 d . . . H94A H 0.6372 0.8032 1.1128 0.038 Uiso 1 1 calc R . . S1A S 0.72633(11) 1.04374(13) 0.41348(10) 0.0305(4) Uani 1 1 d . . . O1A O 0.6908(4) 1.0709(5) 0.3480(4) 0.0503(17) Uani 1 1 d . . . F1A F 0.7136(4) 0.8919(4) 0.4073(4) 0.0535(15) Uani 1 1 d . . . C1A C 0.6882(5) 0.9379(6) 0.4479(5) 0.0363(18) Uani 1 1 d . . . O2A O 0.6907(4) 1.0827(5) 0.4612(4) 0.0498(17) Uani 1 1 d . . . F2A F 0.7167(4) 0.9009(4) 0.5092(3) 0.0521(14) Uani 1 1 d . . . O3A O 0.8175(3) 1.0341(4) 0.4122(3) 0.0341(13) Uani 1 1 d . . . F3A F 0.6040(3) 0.9354(4) 0.4540(4) 0.0547(15) Uani 1 1 d . . . S1B S 0.73260(14) 0.93656(13) 0.90812(12) 0.0350(4) Uani 1 1 d . . . O1B O 0.7611(5) 0.9966(5) 0.8460(4) 0.0540(19) Uani 1 1 d . . . F1B F 0.7635(4) 1.0407(4) 0.9741(4) 0.0586(17) Uani 1 1 d . . . C1B C 0.6987(5) 1.0005(6) 0.9627(5) 0.0350(17) Uani 1 1 d . . . O2B O 0.6548(5) 0.8972(5) 0.9030(4) 0.0514(17) Uani 1 1 d . . . F2B F 0.6653(6) 0.9590(5) 1.0218(4) 0.079(2) Uani 1 1 d . . . F3B F 0.6436(5) 1.0594(5) 0.9336(5) 0.085(3) Uani 1 1 d . . . O3B O 0.7915(6) 0.8806(5) 0.9491(5) 0.070(3) Uani 1 1 d . . . Cl1L Cl 0.73379(16) 0.80670(18) 0.66308(15) 0.0535(6) Uani 1 1 d . . . C1L C 0.7766(9) 0.7331(9) 0.7313(8) 0.072(3) Uani 1 1 d U . . H1LA H 0.8355 0.7199 0.7185 0.087 Uiso 1 1 calc R . . H1LB H 0.7436 0.6814 0.7433 0.087 Uiso 1 1 calc R . . Cl2L Cl 0.7756(2) 0.7713(3) 0.80570(18) 0.0773(9) Uani 1 1 d . . . S1T S 0.8085(3) 0.5713(3) 0.5768(3) 0.0990(14) Uani 1 1 d U . . O1T O 0.8891(7) 0.5303(7) 0.5676(7) 0.089(3) Uani 1 1 d U . . F1T F 0.8948(9) 0.6925(9) 0.4969(8) 0.151(5) Uani 1 1 d DU . . C1T C 0.8366(7) 0.6706(9) 0.5478(7) 0.084(4) Uani 1 1 d DU . . F2T F 0.8834(6) 0.7036(6) 0.5833(6) 0.099(3) Uani 1 1 d DU . . O2T O 0.7759(14) 0.5700(14) 0.6538(14) 0.192(9) Uani 1 1 d U . . F3T F 0.7749(9) 0.7272(9) 0.5309(10) 0.163(6) Uani 1 1 d DU . . O3T O 0.7459(13) 0.5627(13) 0.5282(13) 0.171(7) Uani 1 1 d U . . F1D F 0.2245(5) 0.7622(6) 1.0256(4) 0.075(2) Uani 1 1 d . . . O1D O 0.3481(5) 0.6799(5) 0.9543(5) 0.062(2) Uani 1 1 d . . . C1D C 0.2368(7) 0.7961(9) 0.9563(8) 0.070(4) Uani 1 1 d . . . S2D S 0.27394(16) 0.71371(19) 0.92037(14) 0.0519(6) Uani 1 1 d . . . O2D O 0.2885(5) 0.7612(7) 0.8483(5) 0.073(3) Uani 1 1 d . . . F2D F 0.2966(6) 0.8519(5) 0.9475(5) 0.093(3) Uani 1 1 d . . . O3D O 0.2082(7) 0.6537(8) 0.9359(6) 0.096(4) Uani 1 1 d . . . F3D F 0.1672(6) 0.8274(7) 0.9339(6) 0.107(3) Uani 1 1 d U . . O1W O 1.1885(5) 0.8832(5) 0.7627(5) 0.0598(19) Uani 1 1 d U . . O2W O 0.6779(8) 0.5420(8) 0.7629(7) 0.052(3) Uani 0.604(16) 1 d PU A 1 O2W' O 0.6721(5) 0.6391(6) 0.6970(5) 0.006(2) Uani 0.396(16) 1 d PU A 2 O3W O 0.5376(9) 0.5073(8) 1.4355(9) 0.096(4) Uani 0.840(18) 1 d PU B 1 O3W' O 0.6782(15) 0.4396(17) 1.4432(14) 0.015(7) Uani 0.160(18) 1 d PU B 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 C1 0.027(3) 0.042(4) 0.023(4) -0.015(3) 0.000(3) 0.001(3) Fe1 0.0186(4) 0.0419(6) 0.0402(7) -0.0289(5) 0.0011(4) -0.0002(4) N1 0.019(2) 0.037(3) 0.020(3) -0.019(3) 0.000(2) 0.001(2) O1 0.054(4) 0.061(4) 0.032(4) -0.003(3) -0.013(3) -0.029(3) P1 0.0136(6) 0.0333(10) 0.0235(9) -0.0169(7) -0.0008(6) 0.0024(6) Pd1 0.0132(2) 0.0363(3) 0.0239(3) -0.0203(2) -0.00306(16) 0.00183(18) C2 0.021(3) 0.042(4) 0.024(4) -0.013(3) -0.002(2) 0.008(3) Fe2 0.0159(4) 0.0422(6) 0.0352(6) -0.0254(5) 0.0020(4) -0.0014(4) N2 0.017(2) 0.040(4) 0.027(4) -0.011(3) -0.002(2) 0.002(2) O2 0.043(4) 0.065(5) 0.061(5) -0.024(4) -0.006(3) 0.000(3) P2 0.0134(6) 0.0373(10) 0.0253(9) -0.0209(8) -0.0011(6) 0.0021(6) Pd2 0.0143(2) 0.0311(3) 0.0294(3) -0.0160(2) -0.00435(17) -0.00103(17) C3 0.021(3) 0.033(4) 0.028(4) -0.015(3) 0.001(2) -0.001(3) N3 0.029(3) 0.046(4) 0.032(4) -0.018(3) -0.006(3) 0.002(3) P3 0.0115(6) 0.0419(11) 0.0279(10) -0.0202(8) -0.0012(6) -0.0009(6) C4 0.022(3) 0.033(4) 0.027(4) -0.019(3) 0.000(2) 0.001(3) N4 0.027(3) 0.028(3) 0.021(3) -0.012(2) -0.002(2) -0.003(2) P4 0.0122(6) 0.0311(10) 0.0374(11) -0.0194(8) -0.0020(6) -0.0003(6) C5 0.021(3) 0.044(4) 0.022(4) -0.021(3) -0.006(2) 0.005(3) N5 0.022(3) 0.029(3) 0.033(4) -0.013(3) -0.007(2) -0.001(2) C6 0.024(3) 0.037(4) 0.024(4) -0.010(3) 0.003(3) 0.010(3) N6 0.043(4) 0.054(5) 0.051(6) -0.017(4) -0.030(4) 0.012(3) C7 0.024(3) 0.042(5) 0.034(5) -0.009(4) -0.001(3) 0.001(3) N7 0.035(4) 0.057(5) 0.043(5) -0.022(4) -0.007(3) -0.006(3) C8 0.041(4) 0.053(5) 0.028(5) -0.024(4) -0.010(3) 0.014(4) N8 0.018(2) 0.039(4) 0.036(4) -0.026(3) 0.000(2) 0.001(2) C9 0.028(3) 0.039(4) 0.024(4) -0.016(3) -0.010(3) 0.007(3) C10 0.030(3) 0.039(4) 0.034(5) -0.022(4) -0.008(3) 0.003(3) C11 0.030(3) 0.037(4) 0.034(5) -0.018(3) -0.002(3) -0.006(3) C12 0.034(4) 0.035(4) 0.026(4) -0.017(3) -0.007(3) 0.007(3) C13 0.036(4) 0.035(4) 0.027(4) -0.014(3) -0.003(3) 0.006(3) C14 0.025(3) 0.028(4) 0.039(5) -0.012(3) -0.011(3) -0.002(3) C15 0.029(3) 0.033(4) 0.049(5) -0.025(4) -0.016(3) 0.001(3) C16 0.030(3) 0.035(4) 0.044(5) -0.018(4) -0.017(3) -0.001(3) C17 0.036(4) 0.031(4) 0.033(5) -0.009(3) -0.015(3) 0.000(3) C18 0.030(3) 0.029(4) 0.033(4) -0.014(3) -0.007(3) -0.002(3) C19 0.045(5) 0.038(5) 0.053(6) -0.022(4) -0.026(4) 0.005(4) C20 0.029(4) 0.046(5) 0.060(7) -0.032(5) 0.002(4) -0.010(3) C21 0.034(4) 0.035(5) 0.062(7) -0.018(4) -0.027(4) 0.000(3) C22 0.022(3) 0.035(4) 0.079(8) -0.035(5) -0.018(4) 0.006(3) C23 0.024(3) 0.048(5) 0.057(6) -0.032(5) -0.015(3) 0.006(3) C24 0.024(3) 0.050(5) 0.039(5) -0.033(4) -0.012(3) 0.008(3) C25 0.017(3) 0.034(4) 0.047(5) -0.025(4) -0.011(3) 0.002(3) C26 0.022(3) 0.033(4) 0.046(5) -0.017(4) -0.009(3) 0.006(3) C27 0.015(3) 0.042(4) 0.038(4) -0.028(4) -0.003(2) 0.002(3) C28 0.019(3) 0.047(5) 0.030(4) -0.018(3) -0.003(3) -0.002(3) C29 0.025(3) 0.086(7) 0.041(5) -0.045(5) -0.003(3) 0.002(4) C30 0.026(4) 0.064(6) 0.065(7) -0.045(5) -0.003(4) -0.005(4) C31 0.020(3) 0.044(5) 0.061(6) -0.033(4) -0.003(3) -0.001(3) C32 0.020(3) 0.041(5) 0.046(5) -0.024(4) -0.002(3) 0.007(3) C33 0.017(3) 0.039(4) 0.027(4) -0.020(3) 0.001(2) 0.004(3) C34 0.022(3) 0.047(5) 0.044(5) -0.037(4) 0.003(3) 0.002(3) C35 0.025(3) 0.046(5) 0.059(6) -0.034(4) -0.001(3) 0.006(3) C36 0.032(4) 0.039(5) 0.068(7) -0.031(5) -0.001(4) 0.009(3) C37 0.017(3) 0.031(4) 0.027(4) -0.016(3) -0.002(2) 0.001(2) C38 0.019(3) 0.046(5) 0.035(5) -0.019(4) -0.002(3) 0.002(3) C39 0.028(3) 0.047(5) 0.031(5) -0.014(4) -0.015(3) 0.004(3) C40 0.018(3) 0.038(4) 0.055(6) -0.024(4) -0.012(3) 0.007(3) C41 0.018(3) 0.046(5) 0.046(5) -0.024(4) -0.004(3) 0.010(3) C42 0.016(3) 0.040(4) 0.031(4) -0.015(3) 0.001(2) 0.002(3) C43 0.027(3) 0.035(4) 0.024(4) -0.010(3) -0.003(3) 0.011(3) C44 0.057(6) 0.050(6) 0.038(6) -0.007(4) -0.013(4) -0.010(4) C45 0.092(9) 0.057(7) 0.042(7) -0.003(5) -0.004(6) -0.014(6) C46 0.094(9) 0.073(9) 0.029(6) 0.009(5) -0.003(6) -0.007(7) C47 0.078(7) 0.061(7) 0.027(5) -0.010(5) -0.010(5) 0.008(5) C48 0.038(4) 0.059(6) 0.036(5) -0.017(4) -0.009(3) 0.001(4) C49 0.015(3) 0.039(4) 0.026(4) -0.017(3) -0.001(2) 0.000(2) C50 0.024(3) 0.048(5) 0.025(4) -0.019(3) -0.010(3) 0.006(3) C51 0.030(4) 0.058(6) 0.034(5) -0.023(4) -0.001(3) -0.001(3) C52 0.029(4) 0.052(5) 0.040(5) -0.010(4) -0.009(3) -0.001(3) C53 0.027(4) 0.051(5) 0.041(5) -0.009(4) -0.004(3) 0.009(3) C54 0.019(3) 0.045(5) 0.032(4) -0.015(3) 0.001(3) 0.007(3) C55 0.015(3) 0.031(4) 0.034(4) -0.020(3) 0.003(2) -0.002(2) C56 0.024(3) 0.041(4) 0.032(4) -0.016(3) 0.000(3) -0.007(3) C57 0.037(4) 0.042(5) 0.030(5) -0.016(4) -0.002(3) -0.002(3) C58 0.028(3) 0.032(4) 0.044(5) -0.014(4) 0.008(3) -0.006(3) C59 0.019(3) 0.044(5) 0.047(5) -0.022(4) -0.002(3) 0.000(3) C60 0.020(3) 0.045(4) 0.028(4) -0.022(3) -0.006(3) 0.002(3) C61 0.013(3) 0.045(4) 0.031(4) -0.022(3) -0.005(2) 0.009(3) C62 0.015(3) 0.048(5) 0.044(5) -0.026(4) -0.002(3) 0.000(3) C63 0.023(3) 0.062(6) 0.034(5) -0.030(4) -0.006(3) 0.004(3) C64 0.041(4) 0.054(6) 0.029(5) -0.018(4) -0.006(3) 0.002(4) C65 0.028(3) 0.037(4) 0.038(5) -0.021(4) -0.003(3) 0.002(3) C66 0.019(3) 0.047(5) 0.062(6) -0.039(4) -0.013(3) 0.009(3) C67 0.016(3) 0.066(6) 0.088(8) -0.057(6) -0.007(4) 0.009(3) C68 0.021(3) 0.106(9) 0.080(8) -0.077(8) 0.009(4) 0.001(4) C69 0.018(3) 0.077(7) 0.056(6) -0.041(5) 0.010(3) -0.006(4) C70 0.008(2) 0.046(5) 0.060(6) -0.034(4) 0.000(3) 0.004(3) C71 0.018(3) 0.052(5) 0.045(5) -0.033(4) -0.001(3) -0.002(3) C72 0.021(3) 0.068(6) 0.045(6) -0.034(5) 0.000(3) -0.001(3) C73 0.020(3) 0.088(8) 0.078(8) -0.064(7) 0.009(4) -0.005(4) C74 0.024(4) 0.062(6) 0.085(9) -0.050(6) -0.007(4) 0.010(4) C75 0.033(4) 0.055(6) 0.084(9) -0.044(6) -0.020(4) 0.014(4) C76 0.022(3) 0.050(5) 0.063(6) -0.038(5) -0.010(3) 0.011(3) C77 0.029(3) 0.035(4) 0.033(5) -0.014(3) 0.003(3) -0.010(3) C78 0.031(4) 0.057(5) 0.025(4) -0.017(4) -0.003(3) -0.013(3) C79 0.051(5) 0.062(6) 0.020(4) -0.013(4) -0.005(3) -0.027(4) C80 0.074(7) 0.042(5) 0.033(5) -0.007(4) 0.000(5) -0.034(5) C81 0.082(7) 0.039(5) 0.038(6) -0.008(4) -0.016(5) -0.016(5) C82 0.049(5) 0.039(5) 0.031(5) -0.014(4) -0.007(3) -0.013(4) C83 0.020(3) 0.033(4) 0.038(5) -0.014(3) 0.001(3) -0.005(3) C84 0.024(3) 0.041(4) 0.039(5) -0.022(4) 0.001(3) -0.002(3) C85 0.038(4) 0.035(4) 0.039(5) -0.017(4) -0.006(3) 0.003(3) C86 0.044(5) 0.042(5) 0.049(6) -0.009(4) -0.005(4) -0.013(4) C87 0.024(4) 0.062(6) 0.068(8) -0.019(5) 0.004(4) -0.014(4) C88 0.020(3) 0.044(5) 0.062(7) -0.022(4) 0.005(3) -0.007(3) C89 0.014(3) 0.033(4) 0.049(5) -0.020(4) -0.002(3) 0.003(2) C90 0.023(3) 0.040(5) 0.054(6) -0.027(4) -0.011(3) 0.002(3) C91 0.020(3) 0.043(5) 0.061(6) -0.023(4) -0.015(3) 0.002(3) C92 0.023(3) 0.049(5) 0.059(6) -0.029(5) -0.017(3) 0.007(3) C93 0.031(4) 0.024(4) 0.050(6) -0.014(4) -0.005(3) 0.004(3) C94 0.018(3) 0.040(4) 0.041(5) -0.020(4) -0.005(3) 0.002(3) S1A 0.0219(7) 0.0488(12) 0.0264(10) -0.0200(8) -0.0059(6) 0.0113(7) O1A 0.036(3) 0.075(5) 0.037(4) -0.012(3) -0.017(3) 0.009(3) F1A 0.047(3) 0.067(4) 0.064(4) -0.045(3) -0.004(3) -0.004(3) C1A 0.024(3) 0.059(5) 0.036(5) -0.028(4) -0.006(3) -0.001(3) O2A 0.054(4) 0.056(4) 0.049(5) -0.033(3) 0.008(3) 0.004(3) F2A 0.057(3) 0.056(4) 0.046(4) -0.015(3) -0.018(3) -0.001(3) O3A 0.021(2) 0.049(4) 0.038(3) -0.023(3) -0.003(2) 0.006(2) F3A 0.028(2) 0.085(4) 0.059(4) -0.034(3) -0.003(2) -0.002(2) S1B 0.0444(10) 0.0338(11) 0.0312(11) -0.0159(8) -0.0070(8) 0.0032(8) O1B 0.068(4) 0.057(4) 0.043(4) -0.028(3) 0.022(4) -0.019(3) F1B 0.045(3) 0.070(4) 0.078(5) -0.047(4) 0.006(3) -0.016(3) C1B 0.036(4) 0.046(5) 0.027(4) -0.015(4) -0.002(3) -0.007(3) O2B 0.071(5) 0.059(4) 0.031(4) -0.019(3) -0.008(3) -0.021(3) F2B 0.120(6) 0.086(5) 0.034(4) -0.026(3) 0.026(4) -0.044(5) F3B 0.088(5) 0.105(6) 0.083(6) -0.061(5) -0.037(4) 0.057(5) O3B 0.074(5) 0.066(5) 0.087(7) -0.045(5) -0.038(5) 0.033(4) Cl1L 0.0466(12) 0.0606(16) 0.0519(16) -0.0166(12) -0.0001(10) 0.0080(10) C1L 0.072(5) 0.069(5) 0.073(5) -0.016(4) -0.010(4) -0.003(4) Cl2L 0.0712(19) 0.103(3) 0.0489(19) -0.0105(17) 0.0000(14) -0.0153(17) S1T 0.085(2) 0.094(3) 0.129(3) -0.055(2) 0.029(2) -0.030(2) O1T 0.091(5) 0.076(4) 0.109(5) -0.041(4) -0.005(4) 0.004(4) F1T 0.141(6) 0.153(6) 0.143(7) -0.019(4) -0.005(5) -0.018(4) C1T 0.088(6) 0.089(6) 0.082(6) -0.036(4) -0.006(4) 0.004(4) F2T 0.097(4) 0.099(4) 0.111(5) -0.042(4) -0.014(4) -0.013(4) O2T 0.191(9) 0.192(9) 0.188(10) -0.055(5) -0.004(5) -0.009(5) F3T 0.166(7) 0.161(7) 0.169(7) -0.055(5) -0.031(5) 0.002(5) O3T 0.173(8) 0.172(8) 0.176(9) -0.062(5) -0.017(5) -0.010(5) F1D 0.074(4) 0.116(6) 0.041(4) -0.033(4) 0.006(3) -0.009(4) O1D 0.065(5) 0.061(5) 0.063(6) -0.025(4) -0.013(4) 0.009(4) C1D 0.033(5) 0.085(9) 0.098(11) -0.045(8) 0.025(6) 0.003(5) S2D 0.0464(12) 0.0743(18) 0.0369(14) -0.0199(12) -0.0011(10) -0.0042(11) O2D 0.059(5) 0.115(7) 0.041(5) -0.022(5) -0.002(4) 0.030(5) F2D 0.122(7) 0.051(4) 0.098(7) -0.022(4) 0.031(6) 0.001(4) O3D 0.102(8) 0.127(9) 0.061(7) -0.021(6) -0.026(5) -0.058(7) F3D 0.091(4) 0.127(5) 0.102(5) -0.038(4) -0.005(4) 0.034(4) O1W 0.057(3) 0.061(4) 0.061(4) -0.016(3) -0.013(3) 0.003(3) O2W 0.055(5) 0.053(5) 0.055(5) -0.027(4) -0.009(4) 0.021(4) O2W' 0.005(3) 0.007(3) 0.006(3) -0.0016(12) -0.0011(10) -0.0002(10) O3W 0.101(6) 0.089(6) 0.108(6) -0.044(4) 0.003(4) -0.015(4) O3W' 0.013(8) 0.021(9) 0.014(9) -0.009(5) -0.002(4) 0.001(4) _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 C1 N1 1.343(10) . ? C1 C2 1.365(10) . ? Fe1 C27 2.004(6) . ? Fe1 C28 2.009(9) . ? Fe1 C33 2.011(7) . ? Fe1 C32 2.029(9) . ? Fe1 C31 2.037(7) . ? Fe1 C29 2.043(10) . ? Fe1 C34 2.045(7) . ? Fe1 C36 2.049(10) . ? Fe1 C30 2.068(9) . ? Fe1 C35 2.072(7) . ? N1 C5 1.326(9) . ? N1 Pd1 2.088(5) . ? O1 C7 1.228(11) . ? P1 C27 1.792(7) . ? P1 C43 1.794(8) . ? P1 C37 1.824(7) . ? P1 Pd1 2.3059(18) . ? Pd1 N8 2.095(6) . ? Pd1 P2 2.3101(17) . ? C2 C3 1.395(10) . ? Fe2 C70 1.991(8) . ? Fe2 C61 2.000(6) . ? Fe2 C65 2.006(8) . ? Fe2 C69 2.027(8) . ? Fe2 C66 2.030(9) . ? Fe2 C62 2.041(7) . ? Fe2 C68 2.048(7) . ? Fe2 C64 2.057(10) . ? Fe2 C67 2.061(9) . ? Fe2 C63 2.078(8) . ? N2 C7 1.359(11) . ? N2 C6 1.432(10) . ? O2 C20 1.219(11) . ? P2 C33 1.789(7) . ? P2 C49 1.814(8) . ? P2 C55 1.822(7) . ? Pd2 N5 2.103(6) . ? Pd2 N4 2.106(6) . ? Pd2 P3 2.2985(18) . ? Pd2 P4 2.3032(19) . ? C3 C4 1.420(11) . ? C3 C6 1.524(9) . ? N3 C7 1.360(11) . ? N3 C8 1.423(12) . ? P3 C77 1.792(8) . ? P3 C61 1.800(8) . ? P3 C71 1.835(8) . ? C4 C5 1.375(9) . ? N4 C12 1.341(11) . ? N4 C11 1.350(10) . ? P4 C83 1.803(8) . ? P4 C70 1.805(8) . ? P4 C89 1.830(8) . ? N5 C14 1.328(10) . ? N5 C18 1.344(10) . ? N6 C20 1.328(14) . ? N6 C19 1.430(11) . ? N7 C20 1.396(13) . ? N7 C21 1.404(14) . ? C8 C9 1.523(11) . ? N8 C25 1.342(11) . ? N8 C24 1.351(9) . ? C9 C13 1.377(11) . ? C9 C10 1.381(12) . ? C10 C11 1.364(11) . ? C12 C13 1.373(11) . ? C14 C15 1.392(10) . ? C15 C16 1.369(12) . ? C16 C17 1.389(11) . ? C16 C19 1.515(11) . ? C17 C18 1.384(10) . ? C21 C22 1.513(11) . ? C22 C23 1.355(15) . ? C22 C26 1.412(12) . ? C23 C24 1.367(12) . ? C25 C26 1.373(11) . ? C27 C31 1.433(11) . ? C27 C28 1.448(11) . ? C28 C29 1.437(11) . ? C29 C30 1.396(15) . ? C30 C31 1.435(13) . ? C32 C36 1.424(11) . ? C32 C33 1.447(12) . ? C33 C34 1.437(9) . ? C34 C35 1.438(12) . ? C35 C36 1.418(15) . ? C37 C38 1.374(12) . ? C37 C42 1.417(9) . ? C38 C39 1.396(10) . ? C39 C40 1.383(12) . ? C40 C41 1.382(13) . ? C41 C42 1.394(9) . ? C43 C44 1.410(13) . ? C43 C48 1.417(13) . ? C44 C45 1.393(16) . ? C45 C46 1.37(2) . ? C46 C47 1.397(19) . ? C47 C48 1.409(15) . ? C49 C50 1.394(10) . ? C49 C54 1.412(9) . ? C50 C51 1.376(12) . ? C51 C52 1.385(12) . ? C52 C53 1.390(14) . ? C53 C54 1.358(13) . ? C55 C56 1.384(12) . ? C55 C60 1.413(9) . ? C56 C57 1.394(12) . ? C57 C58 1.409(12) . ? C58 C59 1.363(13) . ? C59 C60 1.383(12) . ? C61 C62 1.430(10) . ? C61 C65 1.437(12) . ? C62 C63 1.436(13) . ? C63 C64 1.423(13) . ? C64 C65 1.414(12) . ? C66 C67 1.409(13) . ? C66 C70 1.443(12) . ? C67 C68 1.424(18) . ? C68 C69 1.421(13) . ? C69 C70 1.419(14) . ? C71 C76 1.368(14) . ? C71 C72 1.397(12) . ? C72 C73 1.413(12) . ? C73 C74 1.363(18) . ? C74 C75 1.355(17) . ? C75 C76 1.407(11) . ? C77 C82 1.394(13) . ? C77 C78 1.410(10) . ? C78 C79 1.376(13) . ? C79 C80 1.380(16) . ? C80 C81 1.397(15) . ? C81 C82 1.381(13) . ? C83 C84 1.391(10) . ? C83 C88 1.403(11) . ? C84 C85 1.399(13) . ? C85 C86 1.381(13) . ? C86 C87 1.363(14) . ? C87 C88 1.417(15) . ? C89 C94 1.380(11) . ? C89 C90 1.396(10) . ? C90 C91 1.405(11) . ? C91 C92 1.364(13) . ? C92 C93 1.395(11) . ? C93 C94 1.373(11) . ? S1A O2A 1.424(6) . ? S1A O1A 1.437(7) . ? S1A O3A 1.446(5) . ? S1A C1A 1.817(10) . ? F1A C1A 1.345(10) . ? C1A F3A 1.331(9) . ? C1A F2A 1.332(11) . ? S1B O3B 1.424(8) . ? S1B O1B 1.426(8) . ? S1B O2B 1.446(7) . ? S1B C1B 1.835(9) . ? F1B C1B 1.322(10) . ? C1B F2B 1.294(11) . ? C1B F3B 1.323(11) . ? Cl1L C1L 1.726(15) . ? C1L Cl2L 1.845(17) . ? S1T O1T 1.459(11) . ? S1T O3T 1.50(2) . ? S1T O2T 1.64(3) . ? S1T C1T 1.664(14) . ? F1T C1T 1.321(5) . ? C1T F2T 1.327(5) . ? C1T F3T 1.328(5) . ? F1D C1D 1.373(17) . ? O1D S2D 1.419(9) . ? C1D F3D 1.259(16) . ? C1D F2D 1.324(15) . ? C1D S2D 1.834(12) . ? S2D O3D 1.429(10) . ? S2D O2D 1.465(9) . ? 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 C1 C2 122.3(7) . . ? C27 Fe1 C28 42.3(3) . . ? C27 Fe1 C33 111.0(3) . . ? C28 Fe1 C33 109.1(3) . . ? C27 Fe1 C32 107.2(3) . . ? C28 Fe1 C32 135.4(3) . . ? C33 Fe1 C32 42.0(3) . . ? C27 Fe1 C31 41.5(3) . . ? C28 Fe1 C31 69.9(4) . . ? C33 Fe1 C31 141.4(3) . . ? C32 Fe1 C31 110.5(4) . . ? C27 Fe1 C29 70.2(3) . . ? C28 Fe1 C29 41.5(3) . . ? C33 Fe1 C29 136.8(4) . . ? C32 Fe1 C29 176.9(3) . . ? C31 Fe1 C29 68.8(4) . . ? C27 Fe1 C34 142.8(3) . . ? C28 Fe1 C34 113.1(3) . . ? C33 Fe1 C34 41.5(3) . . ? C32 Fe1 C34 69.8(3) . . ? C31 Fe1 C34 175.6(3) . . ? C29 Fe1 C34 111.1(4) . . ? C27 Fe1 C36 134.1(4) . . ? C28 Fe1 C36 175.7(4) . . ? C33 Fe1 C36 69.3(3) . . ? C32 Fe1 C36 40.9(3) . . ? C31 Fe1 C36 108.7(4) . . ? C29 Fe1 C36 142.2(4) . . ? C34 Fe1 C36 68.5(4) . . ? C27 Fe1 C30 69.3(3) . . ? C28 Fe1 C30 68.6(4) . . ? C33 Fe1 C30 176.5(4) . . ? C32 Fe1 C30 141.5(4) . . ? C31 Fe1 C30 40.9(4) . . ? C29 Fe1 C30 39.7(4) . . ? C34 Fe1 C30 136.4(3) . . ? C36 Fe1 C30 113.2(4) . . ? C27 Fe1 C35 174.2(4) . . ? C28 Fe1 C35 143.4(4) . . ? C33 Fe1 C35 69.4(3) . . ? C32 Fe1 C35 69.0(3) . . ? C31 Fe1 C35 134.9(3) . . ? C29 Fe1 C35 113.7(4) . . ? C34 Fe1 C35 40.9(3) . . ? C36 Fe1 C35 40.2(4) . . ? C30 Fe1 C35 110.7(3) . . ? C5 N1 C1 118.4(6) . . ? C5 N1 Pd1 120.6(5) . . ? C1 N1 Pd1 121.0(5) . . ? C27 P1 C43 112.5(4) . . ? C27 P1 C37 102.9(3) . . ? C43 P1 C37 103.2(3) . . ? C27 P1 Pd1 113.4(2) . . ? C43 P1 Pd1 113.1(3) . . ? C37 P1 Pd1 110.8(2) . . ? N1 Pd1 N8 85.8(2) . . ? N1 Pd1 P1 89.27(16) . . ? N8 Pd1 P1 172.8(2) . . ? N1 Pd1 P2 171.34(16) . . ? N8 Pd1 P2 87.06(16) . . ? P1 Pd1 P2 98.31(6) . . ? C1 C2 C3 119.8(7) . . ? C70 Fe2 C61 110.4(3) . . ? C70 Fe2 C65 109.2(3) . . ? C61 Fe2 C65 42.0(3) . . ? C70 Fe2 C69 41.3(4) . . ? C61 Fe2 C69 139.2(3) . . ? C65 Fe2 C69 109.7(4) . . ? C70 Fe2 C66 42.0(3) . . ? C61 Fe2 C66 111.1(3) . . ? C65 Fe2 C66 139.1(3) . . ? C69 Fe2 C66 69.3(4) . . ? C70 Fe2 C62 140.2(4) . . ? C61 Fe2 C62 41.4(3) . . ? C65 Fe2 C62 69.9(3) . . ? C69 Fe2 C62 178.4(4) . . ? C66 Fe2 C62 112.0(4) . . ? C70 Fe2 C68 69.2(4) . . ? C61 Fe2 C68 179.3(5) . . ? C65 Fe2 C68 138.6(5) . . ? C69 Fe2 C68 40.8(4) . . ? C66 Fe2 C68 68.2(5) . . ? C62 Fe2 C68 138.6(3) . . ? C70 Fe2 C64 137.2(4) . . ? C61 Fe2 C64 69.3(3) . . ? C65 Fe2 C64 40.7(3) . . ? C69 Fe2 C64 109.9(4) . . ? C66 Fe2 C64 179.1(3) . . ? C62 Fe2 C64 68.8(4) . . ? C68 Fe2 C64 111.4(5) . . ? C70 Fe2 C67 69.5(3) . . ? C61 Fe2 C67 138.8(4) . . ? C65 Fe2 C67 178.6(3) . . ? C69 Fe2 C67 68.9(4) . . ? C66 Fe2 C67 40.3(4) . . ? C62 Fe2 C67 111.5(3) . . ? C68 Fe2 C67 40.5(5) . . ? C64 Fe2 C67 139.9(4) . . ? C70 Fe2 C63 177.4(4) . . ? C61 Fe2 C63 69.0(3) . . ? C65 Fe2 C63 68.6(3) . . ? C69 Fe2 C63 137.6(4) . . ? C66 Fe2 C63 140.5(4) . . ? C62 Fe2 C63 40.8(4) . . ? C68 Fe2 C63 111.4(4) . . ? C64 Fe2 C63 40.3(4) . . ? C67 Fe2 C63 112.6(3) . . ? C7 N2 C6 120.3(7) . . ? C33 P2 C49 101.4(4) . . ? C33 P2 C55 105.0(3) . . ? C49 P2 C55 106.6(3) . . ? C33 P2 Pd1 123.7(2) . . ? C49 P2 Pd1 109.9(2) . . ? C55 P2 Pd1 108.9(2) . . ? N5 Pd2 N4 84.7(2) . . ? N5 Pd2 P3 171.68(17) . . ? N4 Pd2 P3 88.86(17) . . ? N5 Pd2 P4 87.53(18) . . ? N4 Pd2 P4 171.94(18) . . ? P3 Pd2 P4 99.08(7) . . ? C2 C3 C4 117.8(6) . . ? C2 C3 C6 123.4(7) . . ? C4 C3 C6 118.7(6) . . ? C7 N3 C8 120.4(7) . . ? C77 P3 C61 103.2(4) . . ? C77 P3 C71 107.0(4) . . ? C61 P3 C71 101.7(4) . . ? C77 P3 Pd2 108.9(3) . . ? C61 P3 Pd2 122.1(2) . . ? C71 P3 Pd2 112.8(2) . . ? C5 C4 C3 117.4(6) . . ? C12 N4 C11 116.1(7) . . ? C12 N4 Pd2 125.8(5) . . ? C11 N4 Pd2 117.6(5) . . ? C83 P4 C70 107.8(4) . . ? C83 P4 C89 105.8(4) . . ? C70 P4 C89 104.3(3) . . ? C83 P4 Pd2 109.6(2) . . ? C70 P4 Pd2 120.0(2) . . ? C89 P4 Pd2 108.4(3) . . ? N1 C5 C4 124.2(7) . . ? C14 N5 C18 119.2(7) . . ? C14 N5 Pd2 120.0(5) . . ? C18 N5 Pd2 120.7(5) . . ? N2 C6 C3 112.2(6) . . ? C20 N6 C19 117.6(9) . . ? O1 C7 N2 122.4(9) . . ? O1 C7 N3 122.2(8) . . ? N2 C7 N3 115.4(7) . . ? C20 N7 C21 120.0(8) . . ? N3 C8 C9 116.7(7) . . ? C25 N8 C24 119.4(7) . . ? C25 N8 Pd1 116.0(5) . . ? C24 N8 Pd1 124.7(6) . . ? C13 C9 C10 116.7(7) . . ? C13 C9 C8 124.3(8) . . ? C10 C9 C8 118.9(7) . . ? C11 C10 C9 120.7(7) . . ? N4 C11 C10 122.9(8) . . ? N4 C12 C13 123.5(7) . . ? C12 C13 C9 119.9(8) . . ? N5 C14 C15 121.7(8) . . ? C16 C15 C14 120.6(7) . . ? C15 C16 C17 116.9(7) . . ? C15 C16 C19 118.9(7) . . ? C17 C16 C19 124.1(8) . . ? C18 C17 C16 120.6(8) . . ? N5 C18 C17 121.0(7) . . ? N6 C19 C16 114.2(7) . . ? O2 C20 N6 125.6(10) . . ? O2 C20 N7 120.1(10) . . ? N6 C20 N7 114.3(8) . . ? N7 C21 C22 115.2(8) . . ? C23 C22 C26 119.7(8) . . ? C23 C22 C21 118.3(8) . . ? C26 C22 C21 122.0(10) . . ? C22 C23 C24 119.8(8) . . ? N8 C24 C23 121.3(9) . . ? N8 C25 C26 122.1(7) . . ? C25 C26 C22 117.7(9) . . ? C31 C27 C28 107.2(7) . . ? C31 C27 P1 132.1(7) . . ? C28 C27 P1 120.6(6) . . ? C31 C27 Fe1 70.5(4) . . ? C28 C27 Fe1 69.0(4) . . ? P1 C27 Fe1 122.9(4) . . ? C29 C28 C27 107.6(8) . . ? C29 C28 Fe1 70.5(6) . . ? C27 C28 Fe1 68.7(5) . . ? C30 C29 C28 108.4(8) . . ? C30 C29 Fe1 71.1(6) . . ? C28 C29 Fe1 68.0(5) . . ? C29 C30 C31 109.0(7) . . ? C29 C30 Fe1 69.2(5) . . ? C31 C30 Fe1 68.4(5) . . ? C27 C31 C30 107.8(8) . . ? C27 C31 Fe1 68.0(4) . . ? C30 C31 Fe1 70.7(5) . . ? C36 C32 C33 107.0(8) . . ? C36 C32 Fe1 70.3(6) . . ? C33 C32 Fe1 68.3(5) . . ? C34 C33 C32 107.8(7) . . ? C34 C33 P2 129.9(6) . . ? C32 C33 P2 122.3(5) . . ? C34 C33 Fe1 70.5(4) . . ? C32 C33 Fe1 69.7(4) . . ? P2 C33 Fe1 123.3(4) . . ? C33 C34 C35 107.9(8) . . ? C33 C34 Fe1 68.0(4) . . ? C35 C34 Fe1 70.6(4) . . ? C36 C35 C34 107.6(7) . . ? C36 C35 Fe1 69.0(5) . . ? C34 C35 Fe1 68.6(4) . . ? C35 C36 C32 109.7(8) . . ? C35 C36 Fe1 70.7(6) . . ? C32 C36 Fe1 68.8(5) . . ? C38 C37 C42 120.4(6) . . ? C38 C37 P1 119.5(5) . . ? C42 C37 P1 120.1(6) . . ? C37 C38 C39 119.9(7) . . ? C40 C39 C38 119.8(8) . . ? C41 C40 C39 121.1(7) . . ? C40 C41 C42 119.6(7) . . ? C41 C42 C37 119.1(8) . . ? C44 C43 C48 118.7(8) . . ? C44 C43 P1 122.6(7) . . ? C48 C43 P1 117.4(7) . . ? C45 C44 C43 120.6(11) . . ? C46 C45 C44 119.3(12) . . ? C45 C46 C47 123.1(11) . . ? C46 C47 C48 117.6(11) . . ? C47 C48 C43 120.7(10) . . ? C50 C49 C54 118.4(7) . . ? C50 C49 P2 121.8(5) . . ? C54 C49 P2 119.8(6) . . ? C51 C50 C49 120.7(7) . . ? C50 C51 C52 120.9(8) . . ? C51 C52 C53 118.0(9) . . ? C54 C53 C52 122.3(8) . . ? C53 C54 C49 119.6(7) . . ? C56 C55 C60 119.3(7) . . ? C56 C55 P2 119.9(5) . . ? C60 C55 P2 120.4(6) . . ? C55 C56 C57 121.4(7) . . ? C56 C57 C58 118.0(8) . . ? C59 C58 C57 120.9(8) . . ? C58 C59 C60 121.2(7) . . ? C59 C60 C55 119.1(8) . . ? C62 C61 C65 107.9(7) . . ? C62 C61 P3 124.3(7) . . ? C65 C61 P3 127.8(6) . . ? C62 C61 Fe2 70.8(4) . . ? C65 C61 Fe2 69.2(4) . . ? P3 C61 Fe2 123.6(4) . . ? C61 C62 C63 107.5(7) . . ? C61 C62 Fe2 67.7(4) . . ? C63 C62 Fe2 71.0(4) . . ? C64 C63 C62 108.0(7) . . ? C64 C63 Fe2 69.1(5) . . ? C62 C63 Fe2 68.2(4) . . ? C65 C64 C63 108.5(8) . . ? C65 C64 Fe2 67.7(5) . . ? C63 C64 Fe2 70.7(5) . . ? C64 C65 C61 108.1(7) . . ? C64 C65 Fe2 71.6(5) . . ? C61 C65 Fe2 68.7(4) . . ? C67 C66 C70 108.3(9) . . ? C67 C66 Fe2 71.0(6) . . ? C70 C66 Fe2 67.5(5) . . ? C66 C67 C68 107.6(8) . . ? C66 C67 Fe2 68.7(5) . . ? C68 C67 Fe2 69.3(5) . . ? C69 C68 C67 108.7(10) . . ? C69 C68 Fe2 68.8(4) . . ? C67 C68 Fe2 70.2(5) . . ? C70 C69 C68 107.8(10) . . ? C70 C69 Fe2 68.0(4) . . ? C68 C69 Fe2 70.4(5) . . ? C69 C70 C66 107.5(8) . . ? C69 C70 P4 127.3(7) . . ? C66 C70 P4 125.1(7) . . ? C69 C70 Fe2 70.7(5) . . ? C66 C70 Fe2 70.4(4) . . ? P4 C70 Fe2 122.1(3) . . ? C76 C71 C72 118.3(8) . . ? C76 C71 P3 120.2(6) . . ? C72 C71 P3 121.3(8) . . ? C71 C72 C73 118.7(10) . . ? C74 C73 C72 121.6(9) . . ? C75 C74 C73 119.9(8) . . ? C74 C75 C76 119.4(12) . . ? C71 C76 C75 122.0(10) . . ? C82 C77 C78 119.8(8) . . ? C82 C77 P3 120.0(6) . . ? C78 C77 P3 119.7(7) . . ? C79 C78 C77 120.0(9) . . ? C78 C79 C80 119.3(8) . . ? C79 C80 C81 121.6(9) . . ? C82 C81 C80 119.1(11) . . ? C81 C82 C77 120.0(9) . . ? C84 C83 C88 119.0(8) . . ? C84 C83 P4 120.3(6) . . ? C88 C83 P4 120.7(6) . . ? C83 C84 C85 120.4(7) . . ? C86 C85 C84 119.7(8) . . ? C87 C86 C85 121.6(9) . . ? C86 C87 C88 119.2(9) . . ? C83 C88 C87 120.1(8) . . ? C94 C89 C90 120.3(7) . . ? C94 C89 P4 118.3(5) . . ? C90 C89 P4 121.2(6) . . ? C89 C90 C91 117.8(8) . . ? C92 C91 C90 121.9(7) . . ? C91 C92 C93 119.2(7) . . ? C94 C93 C92 120.1(8) . . ? C93 C94 C89 120.7(7) . . ? O2A S1A O1A 115.0(5) . . ? O2A S1A O3A 114.9(4) . . ? O1A S1A O3A 115.3(4) . . ? O2A S1A C1A 103.0(4) . . ? O1A S1A C1A 101.9(4) . . ? O3A S1A C1A 104.1(4) . . ? F3A C1A F2A 107.6(8) . . ? F3A C1A F1A 106.7(6) . . ? F2A C1A F1A 108.0(8) . . ? F3A C1A S1A 112.1(6) . . ? F2A C1A S1A 110.9(5) . . ? F1A C1A S1A 111.3(6) . . ? O3B S1B O1B 120.2(6) . . ? O3B S1B O2B 113.2(5) . . ? O1B S1B O2B 113.3(5) . . ? O3B S1B C1B 101.3(5) . . ? O1B S1B C1B 103.2(4) . . ? O2B S1B C1B 102.5(4) . . ? F2B C1B F1B 106.6(8) . . ? F2B C1B F3B 107.5(8) . . ? F1B C1B F3B 105.0(8) . . ? F2B C1B S1B 114.4(7) . . ? F1B C1B S1B 110.8(6) . . ? F3B C1B S1B 112.0(7) . . ? Cl1L C1L Cl2L 110.9(8) . . ? O1T S1T O3T 111.5(10) . . ? O1T S1T O2T 118.4(11) . . ? O3T S1T O2T 119.8(12) . . ? O1T S1T C1T 100.5(6) . . ? O3T S1T C1T 104.6(10) . . ? O2T S1T C1T 97.5(9) . . ? F1T C1T F2T 88.7(11) . . ? F1T C1T F3T 105.3(14) . . ? F2T C1T F3T 101.4(12) . . ? F1T C1T S1T 118.3(11) . . ? F2T C1T S1T 121.4(11) . . ? F3T C1T S1T 117.1(10) . . ? F3D C1D F2D 113.3(13) . . ? F3D C1D F1D 107.4(9) . . ? F2D C1D F1D 104.9(12) . . ? F3D C1D S2D 111.8(12) . . ? F2D C1D S2D 110.3(7) . . ? F1D C1D S2D 108.7(10) . . ? O1D S2D O3D 111.4(6) . . ? O1D S2D O2D 114.9(5) . . ? O3D S2D O2D 115.8(6) . . ? O1D S2D C1D 105.4(6) . . ? O3D S2D C1D 106.7(7) . . ? O2D S2D C1D 101.2(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 N1 C5 2.8(11) . . . . ? C2 C1 N1 Pd1 -177.9(6) . . . . ? C5 N1 Pd1 N8 92.4(6) . . . . ? C1 N1 Pd1 N8 -86.9(6) . . . . ? C5 N1 Pd1 P1 -92.8(5) . . . . ? C1 N1 Pd1 P1 87.9(5) . . . . ? C5 N1 Pd1 P2 58.5(15) . . . . ? C1 N1 Pd1 P2 -120.8(11) . . . . ? C27 P1 Pd1 N1 -134.0(3) . . . . ? C43 P1 Pd1 N1 96.4(3) . . . . ? C37 P1 Pd1 N1 -18.9(3) . . . . ? C27 P1 Pd1 N8 -88.0(14) . . . . ? C43 P1 Pd1 N8 142.4(14) . . . . ? C37 P1 Pd1 N8 27.1(14) . . . . ? C27 P1 Pd1 P2 50.2(3) . . . . ? C43 P1 Pd1 P2 -79.4(2) . . . . ? C37 P1 Pd1 P2 165.3(3) . . . . ? N1 C1 C2 C3 -0.6(12) . . . . ? N1 Pd1 P2 C33 -165.9(12) . . . . ? N8 Pd1 P2 C33 160.2(4) . . . . ? P1 Pd1 P2 C33 -15.0(3) . . . . ? N1 Pd1 P2 C49 -46.3(13) . . . . ? N8 Pd1 P2 C49 -80.2(3) . . . . ? P1 Pd1 P2 C49 104.6(3) . . . . ? N1 Pd1 P2 C55 70.2(13) . . . . ? N8 Pd1 P2 C55 36.3(3) . . . . ? P1 Pd1 P2 C55 -138.9(3) . . . . ? C1 C2 C3 C4 -2.5(11) . . . . ? C1 C2 C3 C6 179.4(7) . . . . ? N5 Pd2 P3 C77 108.3(14) . . . . ? N4 Pd2 P3 C77 69.3(3) . . . . ? P4 Pd2 P3 C77 -109.4(3) . . . . ? N5 Pd2 P3 C61 -131.8(14) . . . . ? N4 Pd2 P3 C61 -170.8(3) . . . . ? P4 Pd2 P3 C61 10.6(3) . . . . ? N5 Pd2 P3 C71 -10.3(14) . . . . ? N4 Pd2 P3 C71 -49.3(4) . . . . ? P4 Pd2 P3 C71 132.0(3) . . . . ? C2 C3 C4 C5 3.4(10) . . . . ? C6 C3 C4 C5 -178.4(7) . . . . ? N5 Pd2 N4 C12 101.5(6) . . . . ? P3 Pd2 N4 C12 -83.8(6) . . . . ? P4 Pd2 N4 C12 86.5(14) . . . . ? N5 Pd2 N4 C11 -70.2(6) . . . . ? P3 Pd2 N4 C11 104.6(6) . . . . ? P4 Pd2 N4 C11 -85.1(14) . . . . ? N5 Pd2 P4 C83 81.3(3) . . . . ? N4 Pd2 P4 C83 96.3(13) . . . . ? P3 Pd2 P4 C83 -93.6(3) . . . . ? N5 Pd2 P4 C70 -153.2(4) . . . . ? N4 Pd2 P4 C70 -138.3(13) . . . . ? P3 Pd2 P4 C70 31.9(4) . . . . ? N5 Pd2 P4 C89 -33.7(3) . . . . ? N4 Pd2 P4 C89 -18.8(13) . . . . ? P3 Pd2 P4 C89 151.3(3) . . . . ? C1 N1 C5 C4 -1.8(11) . . . . ? Pd1 N1 C5 C4 178.9(6) . . . . ? C3 C4 C5 N1 -1.3(11) . . . . ? N4 Pd2 N5 C14 93.9(6) . . . . ? P3 Pd2 N5 C14 54.7(17) . . . . ? P4 Pd2 N5 C14 -88.2(6) . . . . ? N4 Pd2 N5 C18 -81.1(6) . . . . ? P3 Pd2 N5 C18 -120.4(12) . . . . ? P4 Pd2 N5 C18 96.8(6) . . . . ? C7 N2 C6 C3 85.8(9) . . . . ? C2 C3 C6 N2 -14.7(10) . . . . ? C4 C3 C6 N2 167.2(6) . . . . ? C6 N2 C7 O1 13.5(12) . . . . ? C6 N2 C7 N3 -167.3(6) . . . . ? C8 N3 C7 O1 5.2(12) . . . . ? C8 N3 C7 N2 -174.1(7) . . . . ? C7 N3 C8 C9 -98.9(9) . . . . ? N1 Pd1 N8 C25 90.5(5) . . . . ? P1 Pd1 N8 C25 44.3(16) . . . . ? P2 Pd1 N8 C25 -94.3(5) . . . . ? N1 Pd1 N8 C24 -88.3(6) . . . . ? P1 Pd1 N8 C24 -134.6(12) . . . . ? P2 Pd1 N8 C24 86.8(5) . . . . ? N3 C8 C9 C13 -17.9(12) . . . . ? N3 C8 C9 C10 164.5(7) . . . . ? C13 C9 C10 C11 -1.7(11) . . . . ? C8 C9 C10 C11 176.2(7) . . . . ? C12 N4 C11 C10 4.6(11) . . . . ? Pd2 N4 C11 C10 177.1(6) . . . . ? C9 C10 C11 N4 -1.5(13) . . . . ? C11 N4 C12 C13 -4.8(11) . . . . ? Pd2 N4 C12 C13 -176.6(6) . . . . ? N4 C12 C13 C9 1.8(13) . . . . ? C10 C9 C13 C12 1.5(12) . . . . ? C8 C9 C13 C12 -176.2(8) . . . . ? C18 N5 C14 C15 -1.5(12) . . . . ? Pd2 N5 C14 C15 -176.6(6) . . . . ? N5 C14 C15 C16 -0.2(13) . . . . ? C14 C15 C16 C17 0.7(13) . . . . ? C14 C15 C16 C19 -177.9(9) . . . . ? C15 C16 C17 C18 0.5(13) . . . . ? C19 C16 C17 C18 179.0(9) . . . . ? C14 N5 C18 C17 2.7(12) . . . . ? Pd2 N5 C18 C17 177.8(6) . . . . ? C16 C17 C18 N5 -2.2(13) . . . . ? C20 N6 C19 C16 95.6(11) . . . . ? C15 C16 C19 N6 160.5(9) . . . . ? C17 C16 C19 N6 -18.0(15) . . . . ? C19 N6 C20 O2 5.7(14) . . . . ? C19 N6 C20 N7 -174.0(7) . . . . ? C21 N7 C20 O2 5.6(12) . . . . ? C21 N7 C20 N6 -174.6(7) . . . . ? C20 N7 C21 C22 -87.9(10) . . . . ? N7 C21 C22 C23 176.1(8) . . . . ? N7 C21 C22 C26 -2.5(12) . . . . ? C26 C22 C23 C24 -1.3(11) . . . . ? C21 C22 C23 C24 -179.9(7) . . . . ? C25 N8 C24 C23 2.3(10) . . . . ? Pd1 N8 C24 C23 -178.9(5) . . . . ? C22 C23 C24 N8 -0.4(11) . . . . ? C24 N8 C25 C26 -2.4(10) . . . . ? Pd1 N8 C25 C26 178.6(5) . . . . ? N8 C25 C26 C22 0.8(10) . . . . ? C23 C22 C26 C25 1.1(11) . . . . ? C21 C22 C26 C25 179.7(7) . . . . ? C43 P1 C27 C31 -20.0(8) . . . . ? C37 P1 C27 C31 90.3(8) . . . . ? Pd1 P1 C27 C31 -150.0(6) . . . . ? C43 P1 C27 C28 156.3(6) . . . . ? C37 P1 C27 C28 -93.3(6) . . . . ? Pd1 P1 C27 C28 26.4(7) . . . . ? C43 P1 C27 Fe1 72.8(6) . . . . ? C37 P1 C27 Fe1 -176.9(5) . . . . ? Pd1 P1 C27 Fe1 -57.2(6) . . . . ? C28 Fe1 C27 C31 -118.2(7) . . . . ? C33 Fe1 C27 C31 146.1(6) . . . . ? C32 Fe1 C27 C31 101.8(6) . . . . ? C29 Fe1 C27 C31 -80.0(6) . . . . ? C34 Fe1 C27 C31 -179.2(6) . . . . ? C36 Fe1 C27 C31 65.1(7) . . . . ? C30 Fe1 C27 C31 -37.6(6) . . . . ? C35 Fe1 C27 C31 54(3) . . . . ? C33 Fe1 C27 C28 -95.7(5) . . . . ? C32 Fe1 C27 C28 -140.1(4) . . . . ? C31 Fe1 C27 C28 118.2(7) . . . . ? C29 Fe1 C27 C28 38.1(5) . . . . ? C34 Fe1 C27 C28 -61.0(7) . . . . ? C36 Fe1 C27 C28 -176.7(5) . . . . ? C30 Fe1 C27 C28 80.5(5) . . . . ? C35 Fe1 C27 C28 172(3) . . . . ? C28 Fe1 C27 P1 113.6(7) . . . . ? C33 Fe1 C27 P1 17.9(6) . . . . ? C32 Fe1 C27 P1 -26.5(6) . . . . ? C31 Fe1 C27 P1 -128.2(8) . . . . ? C29 Fe1 C27 P1 151.8(6) . . . . ? C34 Fe1 C27 P1 52.6(9) . . . . ? C36 Fe1 C27 P1 -63.1(7) . . . . ? C30 Fe1 C27 P1 -165.8(7) . . . . ? C35 Fe1 C27 P1 -75(3) . . . . ? C31 C27 C28 C29 0.4(8) . . . . ? P1 C27 C28 C29 -176.7(6) . . . . ? Fe1 C27 C28 C29 -60.0(6) . . . . ? C31 C27 C28 Fe1 60.4(5) . . . . ? P1 C27 C28 Fe1 -116.7(5) . . . . ? C27 Fe1 C28 C29 118.8(6) . . . . ? C33 Fe1 C28 C29 -140.7(5) . . . . ? C32 Fe1 C28 C29 179.6(5) . . . . ? C31 Fe1 C28 C29 80.4(5) . . . . ? C34 Fe1 C28 C29 -96.2(5) . . . . ? C36 Fe1 C28 C29 152(4) . . . . ? C30 Fe1 C28 C29 36.5(5) . . . . ? C35 Fe1 C28 C29 -59.8(7) . . . . ? C33 Fe1 C28 C27 100.5(4) . . . . ? C32 Fe1 C28 C27 60.8(6) . . . . ? C31 Fe1 C28 C27 -38.5(4) . . . . ? C29 Fe1 C28 C27 -118.8(6) . . . . ? C34 Fe1 C28 C27 144.9(4) . . . . ? C36 Fe1 C28 C27 34(5) . . . . ? C30 Fe1 C28 C27 -82.4(5) . . . . ? C35 Fe1 C28 C27 -178.6(5) . . . . ? C27 C28 C29 C30 -1.0(9) . . . . ? Fe1 C28 C29 C30 -59.8(7) . . . . ? C27 C28 C29 Fe1 58.9(5) . . . . ? C27 Fe1 C29 C30 81.1(5) . . . . ? C28 Fe1 C29 C30 119.9(7) . . . . ? C33 Fe1 C29 C30 -179.0(5) . . . . ? C32 Fe1 C29 C30 115(6) . . . . ? C31 Fe1 C29 C30 36.7(5) . . . . ? C34 Fe1 C29 C30 -138.6(5) . . . . ? C36 Fe1 C29 C30 -56.9(7) . . . . ? C35 Fe1 C29 C30 -94.3(5) . . . . ? C27 Fe1 C29 C28 -38.8(4) . . . . ? C33 Fe1 C29 C28 61.1(6) . . . . ? C32 Fe1 C29 C28 -5(7) . . . . ? C31 Fe1 C29 C28 -83.2(5) . . . . ? C34 Fe1 C29 C28 101.5(5) . . . . ? C36 Fe1 C29 C28 -176.8(5) . . . . ? C30 Fe1 C29 C28 -119.9(7) . . . . ? C35 Fe1 C29 C28 145.8(5) . . . . ? C28 C29 C30 C31 1.1(10) . . . . ? Fe1 C29 C30 C31 -56.8(6) . . . . ? C28 C29 C30 Fe1 57.9(6) . . . . ? C27 Fe1 C30 C29 -83.6(5) . . . . ? C28 Fe1 C30 C29 -38.1(5) . . . . ? C33 Fe1 C30 C29 12(5) . . . . ? C32 Fe1 C30 C29 -175.5(5) . . . . ? C31 Fe1 C30 C29 -121.7(8) . . . . ? C34 Fe1 C30 C29 63.4(7) . . . . ? C36 Fe1 C30 C29 146.1(5) . . . . ? C35 Fe1 C30 C29 102.6(6) . . . . ? C27 Fe1 C30 C31 38.2(6) . . . . ? C28 Fe1 C30 C31 83.6(6) . . . . ? C33 Fe1 C30 C31 133(5) . . . . ? C32 Fe1 C30 C31 -53.7(8) . . . . ? C29 Fe1 C30 C31 121.7(8) . . . . ? C34 Fe1 C30 C31 -174.8(6) . . . . ? C36 Fe1 C30 C31 -92.2(6) . . . . ? C35 Fe1 C30 C31 -135.7(6) . . . . ? C28 C27 C31 C30 0.3(9) . . . . ? P1 C27 C31 C30 177.0(6) . . . . ? Fe1 C27 C31 C30 59.8(6) . . . . ? C28 C27 C31 Fe1 -59.5(5) . . . . ? P1 C27 C31 Fe1 117.2(7) . . . . ? C29 C30 C31 C27 -0.9(10) . . . . ? Fe1 C30 C31 C27 -58.1(5) . . . . ? C29 C30 C31 Fe1 57.2(6) . . . . ? C28 Fe1 C31 C27 39.2(5) . . . . ? C33 Fe1 C31 C27 -56.6(8) . . . . ? C32 Fe1 C31 C27 -93.1(6) . . . . ? C29 Fe1 C31 C27 83.7(6) . . . . ? C34 Fe1 C31 C27 174(5) . . . . ? C36 Fe1 C31 C27 -136.5(6) . . . . ? C30 Fe1 C31 C27 119.3(9) . . . . ? C35 Fe1 C31 C27 -173.4(6) . . . . ? C27 Fe1 C31 C30 -119.3(9) . . . . ? C28 Fe1 C31 C30 -80.2(6) . . . . ? C33 Fe1 C31 C30 -175.9(6) . . . . ? C32 Fe1 C31 C30 147.6(6) . . . . ? C29 Fe1 C31 C30 -35.6(6) . . . . ? C34 Fe1 C31 C30 54(6) . . . . ? C36 Fe1 C31 C30 104.1(7) . . . . ? C35 Fe1 C31 C30 67.2(8) . . . . ? C27 Fe1 C32 C36 -139.1(5) . . . . ? C28 Fe1 C32 C36 -177.0(5) . . . . ? C33 Fe1 C32 C36 118.4(6) . . . . ? C31 Fe1 C32 C36 -95.2(5) . . . . ? C29 Fe1 C32 C36 -172(6) . . . . ? C34 Fe1 C32 C36 80.1(5) . . . . ? C30 Fe1 C32 C36 -60.9(7) . . . . ? C35 Fe1 C32 C36 36.3(5) . . . . ? C27 Fe1 C32 C33 102.5(4) . . . . ? C28 Fe1 C32 C33 64.5(5) . . . . ? C31 Fe1 C32 C33 146.3(4) . . . . ? C29 Fe1 C32 C33 70(7) . . . . ? C34 Fe1 C32 C33 -38.3(4) . . . . ? C36 Fe1 C32 C33 -118.4(6) . . . . ? C30 Fe1 C32 C33 -179.4(5) . . . . ? C35 Fe1 C32 C33 -82.1(4) . . . . ? C36 C32 C33 C34 0.5(9) . . . . ? Fe1 C32 C33 C34 60.5(5) . . . . ? C36 C32 C33 P2 -177.2(6) . . . . ? Fe1 C32 C33 P2 -117.3(5) . . . . ? C36 C32 C33 Fe1 -60.0(6) . . . . ? C49 P2 C33 C34 124.9(7) . . . . ? C55 P2 C33 C34 14.0(8) . . . . ? Pd1 P2 C33 C34 -111.6(6) . . . . ? C49 P2 C33 C32 -57.9(6) . . . . ? C55 P2 C33 C32 -168.8(6) . . . . ? Pd1 P2 C33 C32 65.6(7) . . . . ? C49 P2 C33 Fe1 -143.5(4) . . . . ? C55 P2 C33 Fe1 105.7(5) . . . . ? Pd1 P2 C33 Fe1 -20.0(6) . . . . ? C27 Fe1 C33 C34 148.8(5) . . . . ? C28 Fe1 C33 C34 103.7(5) . . . . ? C32 Fe1 C33 C34 -118.5(6) . . . . ? C31 Fe1 C33 C34 -174.9(6) . . . . ? C29 Fe1 C33 C34 65.7(6) . . . . ? C36 Fe1 C33 C34 -80.5(6) . . . . ? C30 Fe1 C33 C34 55(5) . . . . ? C35 Fe1 C33 C34 -37.4(5) . . . . ? C27 Fe1 C33 C32 -92.7(5) . . . . ? C28 Fe1 C33 C32 -137.8(4) . . . . ? C31 Fe1 C33 C32 -56.4(7) . . . . ? C29 Fe1 C33 C32 -175.8(4) . . . . ? C34 Fe1 C33 C32 118.5(6) . . . . ? C36 Fe1 C33 C32 38.0(4) . . . . ? C30 Fe1 C33 C32 173(5) . . . . ? C35 Fe1 C33 C32 81.1(5) . . . . ? C27 Fe1 C33 P2 23.2(6) . . . . ? C28 Fe1 C33 P2 -21.9(5) . . . . ? C32 Fe1 C33 P2 116.0(6) . . . . ? C31 Fe1 C33 P2 59.6(8) . . . . ? C29 Fe1 C33 P2 -59.8(6) . . . . ? C34 Fe1 C33 P2 -125.5(8) . . . . ? C36 Fe1 C33 P2 153.9(6) . . . . ? C30 Fe1 C33 P2 -71(5) . . . . ? C35 Fe1 C33 P2 -162.9(6) . . . . ? C32 C33 C34 C35 -0.5(9) . . . . ? P2 C33 C34 C35 177.0(6) . . . . ? Fe1 C33 C34 C35 59.5(6) . . . . ? C32 C33 C34 Fe1 -60.0(5) . . . . ? P2 C33 C34 Fe1 117.6(6) . . . . ? C27 Fe1 C34 C33 -53.3(8) . . . . ? C28 Fe1 C34 C33 -93.1(5) . . . . ? C32 Fe1 C34 C33 38.8(5) . . . . ? C31 Fe1 C34 C33 134(5) . . . . ? C29 Fe1 C34 C33 -138.1(5) . . . . ? C36 Fe1 C34 C33 82.6(6) . . . . ? C30 Fe1 C34 C33 -175.8(6) . . . . ? C35 Fe1 C34 C33 119.7(8) . . . . ? C27 Fe1 C34 C35 -173.0(6) . . . . ? C28 Fe1 C34 C35 147.2(6) . . . . ? C33 Fe1 C34 C35 -119.7(8) . . . . ? C32 Fe1 C34 C35 -80.9(6) . . . . ? C31 Fe1 C34 C35 14(6) . . . . ? C29 Fe1 C34 C35 102.3(6) . . . . ? C36 Fe1 C34 C35 -37.0(6) . . . . ? C30 Fe1 C34 C35 64.5(8) . . . . ? C33 C34 C35 C36 0.3(9) . . . . ? Fe1 C34 C35 C36 58.2(6) . . . . ? C33 C34 C35 Fe1 -57.9(5) . . . . ? C27 Fe1 C35 C36 13(3) . . . . ? C28 Fe1 C35 C36 -176.5(6) . . . . ? C33 Fe1 C35 C36 -81.9(6) . . . . ? C32 Fe1 C35 C36 -36.8(5) . . . . ? C31 Fe1 C35 C36 61.7(8) . . . . ? C29 Fe1 C35 C36 144.8(6) . . . . ? C34 Fe1 C35 C36 -119.9(8) . . . . ? C30 Fe1 C35 C36 101.9(6) . . . . ? C27 Fe1 C35 C34 133(3) . . . . ? C28 Fe1 C35 C34 -56.6(8) . . . . ? C33 Fe1 C35 C34 38.0(5) . . . . ? C32 Fe1 C35 C34 83.0(6) . . . . ? C31 Fe1 C35 C34 -178.5(6) . . . . ? C29 Fe1 C35 C34 -95.4(6) . . . . ? C36 Fe1 C35 C34 119.9(8) . . . . ? C30 Fe1 C35 C34 -138.3(6) . . . . ? C34 C35 C36 C32 0.0(10) . . . . ? Fe1 C35 C36 C32 57.9(6) . . . . ? C34 C35 C36 Fe1 -57.9(6) . . . . ? C33 C32 C36 C35 -0.3(10) . . . . ? Fe1 C32 C36 C35 -59.0(7) . . . . ? C33 C32 C36 Fe1 58.7(5) . . . . ? C27 Fe1 C36 C35 -178.2(5) . . . . ? C28 Fe1 C36 C35 151(4) . . . . ? C33 Fe1 C36 C35 82.2(5) . . . . ? C32 Fe1 C36 C35 121.2(7) . . . . ? C31 Fe1 C36 C35 -138.8(5) . . . . ? C29 Fe1 C36 C35 -59.5(8) . . . . ? C34 Fe1 C36 C35 37.6(5) . . . . ? C30 Fe1 C36 C35 -95.1(6) . . . . ? C27 Fe1 C36 C32 60.6(6) . . . . ? C28 Fe1 C36 C32 29(5) . . . . ? C33 Fe1 C36 C32 -39.0(5) . . . . ? C31 Fe1 C36 C32 100.0(5) . . . . ? C29 Fe1 C36 C32 179.3(5) . . . . ? C34 Fe1 C36 C32 -83.6(5) . . . . ? C30 Fe1 C36 C32 143.7(5) . . . . ? C35 Fe1 C36 C32 -121.2(7) . . . . ? C27 P1 C37 C38 42.1(7) . . . . ? C43 P1 C37 C38 159.3(6) . . . . ? Pd1 P1 C37 C38 -79.4(6) . . . . ? C27 P1 C37 C42 -140.6(6) . . . . ? C43 P1 C37 C42 -23.4(7) . . . . ? Pd1 P1 C37 C42 97.9(6) . . . . ? C42 C37 C38 C39 -0.2(12) . . . . ? P1 C37 C38 C39 177.1(6) . . . . ? C37 C38 C39 C40 -0.5(12) . . . . ? C38 C39 C40 C41 1.5(13) . . . . ? C39 C40 C41 C42 -1.8(13) . . . . ? C40 C41 C42 C37 1.1(12) . . . . ? C38 C37 C42 C41 -0.1(11) . . . . ? P1 C37 C42 C41 -177.4(6) . . . . ? C27 P1 C43 C44 44.8(8) . . . . ? C37 P1 C43 C44 -65.3(8) . . . . ? Pd1 P1 C43 C44 174.9(7) . . . . ? C27 P1 C43 C48 -148.1(6) . . . . ? C37 P1 C43 C48 101.7(6) . . . . ? Pd1 P1 C43 C48 -18.0(7) . . . . ? C48 C43 C44 C45 -0.9(15) . . . . ? P1 C43 C44 C45 165.9(9) . . . . ? C43 C44 C45 C46 1.8(19) . . . . ? C44 C45 C46 C47 -3(2) . . . . ? C45 C46 C47 C48 3(2) . . . . ? C46 C47 C48 C43 -2.3(16) . . . . ? C44 C43 C48 C47 1.2(13) . . . . ? P1 C43 C48 C47 -166.3(8) . . . . ? C33 P2 C49 C50 130.6(7) . . . . ? C55 P2 C49 C50 -119.8(7) . . . . ? Pd1 P2 C49 C50 -1.9(7) . . . . ? C33 P2 C49 C54 -46.2(7) . . . . ? C55 P2 C49 C54 63.4(7) . . . . ? Pd1 P2 C49 C54 -178.7(5) . . . . ? C54 C49 C50 C51 -1.4(12) . . . . ? P2 C49 C50 C51 -178.3(7) . . . . ? C49 C50 C51 C52 0.0(13) . . . . ? C50 C51 C52 C53 0.3(14) . . . . ? C51 C52 C53 C54 1.0(14) . . . . ? C52 C53 C54 C49 -2.4(14) . . . . ? C50 C49 C54 C53 2.6(12) . . . . ? P2 C49 C54 C53 179.5(7) . . . . ? C33 P2 C55 C56 -64.4(7) . . . . ? C49 P2 C55 C56 -171.5(6) . . . . ? Pd1 P2 C55 C56 70.0(6) . . . . ? C33 P2 C55 C60 123.0(6) . . . . ? C49 P2 C55 C60 16.0(7) . . . . ? Pd1 P2 C55 C60 -102.6(6) . . . . ? C60 C55 C56 C57 -2.4(11) . . . . ? P2 C55 C56 C57 -175.1(6) . . . . ? C55 C56 C57 C58 1.4(12) . . . . ? C56 C57 C58 C59 -0.4(12) . . . . ? C57 C58 C59 C60 0.5(12) . . . . ? C58 C59 C60 C55 -1.5(11) . . . . ? C56 C55 C60 C59 2.5(10) . . . . ? P2 C55 C60 C59 175.1(6) . . . . ? C77 P3 C61 C62 -6.3(6) . . . . ? C71 P3 C61 C62 104.5(6) . . . . ? Pd2 P3 C61 C62 -128.9(5) . . . . ? C77 P3 C61 C65 170.9(6) . . . . ? C71 P3 C61 C65 -78.3(7) . . . . ? Pd2 P3 C61 C65 48.3(7) . . . . ? C77 P3 C61 Fe2 82.3(5) . . . . ? C71 P3 C61 Fe2 -166.9(5) . . . . ? Pd2 P3 C61 Fe2 -40.3(6) . . . . ? C70 Fe2 C61 C62 145.0(5) . . . . ? C65 Fe2 C61 C62 -118.6(7) . . . . ? C69 Fe2 C61 C62 -177.8(7) . . . . ? C66 Fe2 C61 C62 99.9(5) . . . . ? C68 Fe2 C61 C62 91(28) . . . . ? C64 Fe2 C61 C62 -80.9(6) . . . . ? C67 Fe2 C61 C62 63.1(7) . . . . ? C63 Fe2 C61 C62 -37.7(5) . . . . ? C70 Fe2 C61 C65 -96.4(5) . . . . ? C69 Fe2 C61 C65 -59.1(8) . . . . ? C66 Fe2 C61 C65 -141.5(5) . . . . ? C62 Fe2 C61 C65 118.6(7) . . . . ? C68 Fe2 C61 C65 -150(27) . . . . ? C64 Fe2 C61 C65 37.7(5) . . . . ? C67 Fe2 C61 C65 -178.3(5) . . . . ? C63 Fe2 C61 C65 80.9(5) . . . . ? C70 Fe2 C61 P3 25.9(6) . . . . ? C65 Fe2 C61 P3 122.3(7) . . . . ? C69 Fe2 C61 P3 63.2(9) . . . . ? C66 Fe2 C61 P3 -19.2(6) . . . . ? C62 Fe2 C61 P3 -119.1(8) . . . . ? C68 Fe2 C61 P3 -28(28) . . . . ? C64 Fe2 C61 P3 160.0(6) . . . . ? C67 Fe2 C61 P3 -55.9(7) . . . . ? C63 Fe2 C61 P3 -156.8(6) . . . . ? C65 C61 C62 C63 0.5(8) . . . . ? P3 C61 C62 C63 178.2(5) . . . . ? Fe2 C61 C62 C63 60.1(5) . . . . ? C65 C61 C62 Fe2 -59.6(5) . . . . ? P3 C61 C62 Fe2 118.1(5) . . . . ? C70 Fe2 C62 C61 -57.3(7) . . . . ? C65 Fe2 C62 C61 38.8(5) . . . . ? C69 Fe2 C62 C61 115(13) . . . . ? C66 Fe2 C62 C61 -97.3(5) . . . . ? C68 Fe2 C62 C61 -178.9(7) . . . . ? C64 Fe2 C62 C61 82.4(5) . . . . ? C67 Fe2 C62 C61 -140.8(6) . . . . ? C63 Fe2 C62 C61 119.0(7) . . . . ? C70 Fe2 C62 C63 -176.3(5) . . . . ? C61 Fe2 C62 C63 -119.0(7) . . . . ? C65 Fe2 C62 C63 -80.3(5) . . . . ? C69 Fe2 C62 C63 -4(13) . . . . ? C66 Fe2 C62 C63 143.7(5) . . . . ? C68 Fe2 C62 C63 62.1(9) . . . . ? C64 Fe2 C62 C63 -36.6(5) . . . . ? C67 Fe2 C62 C63 100.1(6) . . . . ? C61 C62 C63 C64 -0.4(8) . . . . ? Fe2 C62 C63 C64 57.7(6) . . . . ? C61 C62 C63 Fe2 -58.1(5) . . . . ? C70 Fe2 C63 C64 -5(7) . . . . ? C61 Fe2 C63 C64 -82.4(5) . . . . ? C65 Fe2 C63 C64 -37.1(5) . . . . ? C69 Fe2 C63 C64 59.2(7) . . . . ? C66 Fe2 C63 C64 179.6(5) . . . . ? C62 Fe2 C63 C64 -120.7(7) . . . . ? C68 Fe2 C63 C64 98.3(6) . . . . ? C67 Fe2 C63 C64 142.1(6) . . . . ? C70 Fe2 C63 C62 115(7) . . . . ? C61 Fe2 C63 C62 38.3(5) . . . . ? C65 Fe2 C63 C62 83.5(5) . . . . ? C69 Fe2 C63 C62 179.8(6) . . . . ? C66 Fe2 C63 C62 -59.8(7) . . . . ? C68 Fe2 C63 C62 -141.1(6) . . . . ? C64 Fe2 C63 C62 120.7(7) . . . . ? C67 Fe2 C63 C62 -97.2(6) . . . . ? C62 C63 C64 C65 0.1(9) . . . . ? Fe2 C63 C64 C65 57.2(6) . . . . ? C62 C63 C64 Fe2 -57.2(5) . . . . ? C70 Fe2 C64 C65 59.1(7) . . . . ? C61 Fe2 C64 C65 -38.9(5) . . . . ? C69 Fe2 C64 C65 97.5(5) . . . . ? C66 Fe2 C64 C65 77(23) . . . . ? C62 Fe2 C64 C65 -83.4(5) . . . . ? C68 Fe2 C64 C65 141.2(5) . . . . ? C67 Fe2 C64 C65 178.0(5) . . . . ? C63 Fe2 C64 C65 -120.5(7) . . . . ? C70 Fe2 C64 C63 179.6(5) . . . . ? C61 Fe2 C64 C63 81.6(5) . . . . ? C65 Fe2 C64 C63 120.5(7) . . . . ? C69 Fe2 C64 C63 -142.0(5) . . . . ? C66 Fe2 C64 C63 -162(23) . . . . ? C62 Fe2 C64 C63 37.1(5) . . . . ? C68 Fe2 C64 C63 -98.3(5) . . . . ? C67 Fe2 C64 C63 -61.5(7) . . . . ? C63 C64 C65 C61 0.3(9) . . . . ? Fe2 C64 C65 C61 59.3(5) . . . . ? C63 C64 C65 Fe2 -59.0(6) . . . . ? C62 C61 C65 C64 -0.5(8) . . . . ? P3 C61 C65 C64 -178.1(6) . . . . ? Fe2 C61 C65 C64 -61.1(6) . . . . ? C62 C61 C65 Fe2 60.6(5) . . . . ? P3 C61 C65 Fe2 -117.0(5) . . . . ? C70 Fe2 C65 C64 -141.8(5) . . . . ? C61 Fe2 C65 C64 118.7(7) . . . . ? C69 Fe2 C65 C64 -97.9(6) . . . . ? C66 Fe2 C65 C64 -178.7(5) . . . . ? C62 Fe2 C65 C64 80.5(5) . . . . ? C68 Fe2 C65 C64 -61.8(7) . . . . ? C67 Fe2 C65 C64 -114(18) . . . . ? C63 Fe2 C65 C64 36.7(5) . . . . ? C70 Fe2 C65 C61 99.5(5) . . . . ? C69 Fe2 C65 C61 143.4(5) . . . . ? C66 Fe2 C65 C61 62.6(7) . . . . ? C62 Fe2 C65 C61 -38.2(5) . . . . ? C68 Fe2 C65 C61 179.4(5) . . . . ? C64 Fe2 C65 C61 -118.7(7) . . . . ? C67 Fe2 C65 C61 127(18) . . . . ? C63 Fe2 C65 C61 -82.0(5) . . . . ? C70 Fe2 C66 C67 120.1(7) . . . . ? C61 Fe2 C66 C67 -142.4(5) . . . . ? C65 Fe2 C66 C67 178.0(5) . . . . ? C69 Fe2 C66 C67 81.3(6) . . . . ? C62 Fe2 C66 C67 -97.8(6) . . . . ? C68 Fe2 C66 C67 37.4(5) . . . . ? C64 Fe2 C66 C67 102(23) . . . . ? C63 Fe2 C66 C67 -60.2(8) . . . . ? C61 Fe2 C66 C70 97.5(5) . . . . ? C65 Fe2 C66 C70 57.9(7) . . . . ? C69 Fe2 C66 C70 -38.8(5) . . . . ? C62 Fe2 C66 C70 142.1(5) . . . . ? C68 Fe2 C66 C70 -82.7(5) . . . . ? C64 Fe2 C66 C70 -18(24) . . . . ? C67 Fe2 C66 C70 -120.1(7) . . . . ? C63 Fe2 C66 C70 179.7(5) . . . . ? C70 C66 C67 C68 -1.1(9) . . . . ? Fe2 C66 C67 C68 -58.4(6) . . . . ? C70 C66 C67 Fe2 57.4(5) . . . . ? C70 Fe2 C67 C66 -38.2(5) . . . . ? C61 Fe2 C67 C66 59.7(7) . . . . ? C65 Fe2 C67 C66 -66(18) . . . . ? C69 Fe2 C67 C66 -82.6(6) . . . . ? C62 Fe2 C67 C66 99.1(5) . . . . ? C68 Fe2 C67 C66 -119.7(7) . . . . ? C64 Fe2 C67 C66 -178.7(6) . . . . ? C63 Fe2 C67 C66 143.3(5) . . . . ? C70 Fe2 C67 C68 81.5(6) . . . . ? C61 Fe2 C67 C68 179.5(5) . . . . ? C65 Fe2 C67 C68 54(18) . . . . ? C69 Fe2 C67 C68 37.2(6) . . . . ? C66 Fe2 C67 C68 119.7(7) . . . . ? C62 Fe2 C67 C68 -141.2(6) . . . . ? C64 Fe2 C67 C68 -59.0(8) . . . . ? C63 Fe2 C67 C68 -97.0(6) . . . . ? C66 C67 C68 C69 0.0(10) . . . . ? Fe2 C67 C68 C69 -58.1(6) . . . . ? C66 C67 C68 Fe2 58.1(5) . . . . ? C70 Fe2 C68 C69 37.9(7) . . . . ? C61 Fe2 C68 C69 92(28) . . . . ? C65 Fe2 C68 C69 -57.9(10) . . . . ? C66 Fe2 C68 C69 83.2(7) . . . . ? C62 Fe2 C68 C69 -177.7(7) . . . . ? C64 Fe2 C68 C69 -96.0(8) . . . . ? C67 Fe2 C68 C69 120.4(10) . . . . ? C63 Fe2 C68 C69 -139.4(7) . . . . ? C70 Fe2 C68 C67 -82.5(6) . . . . ? C61 Fe2 C68 C67 -28(28) . . . . ? C65 Fe2 C68 C67 -178.2(5) . . . . ? C69 Fe2 C68 C67 -120.4(10) . . . . ? C66 Fe2 C68 C67 -37.2(5) . . . . ? C62 Fe2 C68 C67 61.9(9) . . . . ? C64 Fe2 C68 C67 143.6(6) . . . . ? C63 Fe2 C68 C67 100.2(6) . . . . ? C67 C68 C69 C70 1.1(10) . . . . ? Fe2 C68 C69 C70 -57.8(6) . . . . ? C67 C68 C69 Fe2 59.0(6) . . . . ? C61 Fe2 C69 C70 -59.3(8) . . . . ? C65 Fe2 C69 C70 -96.9(6) . . . . ? C66 Fe2 C69 C70 39.4(5) . . . . ? C62 Fe2 C69 C70 -172(100) . . . . ? C68 Fe2 C69 C70 119.6(10) . . . . ? C64 Fe2 C69 C70 -140.3(5) . . . . ? C67 Fe2 C69 C70 82.7(6) . . . . ? C63 Fe2 C69 C70 -176.5(5) . . . . ? C70 Fe2 C69 C68 -119.6(10) . . . . ? C61 Fe2 C69 C68 -178.9(7) . . . . ? C65 Fe2 C69 C68 143.5(8) . . . . ? C66 Fe2 C69 C68 -80.2(8) . . . . ? C62 Fe2 C69 C68 68(13) . . . . ? C64 Fe2 C69 C68 100.1(8) . . . . ? C67 Fe2 C69 C68 -36.9(8) . . . . ? C63 Fe2 C69 C68 63.9(10) . . . . ? C68 C69 C70 C66 -1.8(9) . . . . ? Fe2 C69 C70 C66 -61.2(5) . . . . ? C68 C69 C70 P4 175.5(6) . . . . ? Fe2 C69 C70 P4 116.1(6) . . . . ? C68 C69 C70 Fe2 59.4(6) . . . . ? C67 C66 C70 C69 1.8(8) . . . . ? Fe2 C66 C70 C69 61.3(6) . . . . ? C67 C66 C70 P4 -175.5(5) . . . . ? Fe2 C66 C70 P4 -116.0(5) . . . . ? C67 C66 C70 Fe2 -59.5(5) . . . . ? C83 P4 C70 C69 -13.5(8) . . . . ? C89 P4 C70 C69 98.7(7) . . . . ? Pd2 P4 C70 C69 -139.8(6) . . . . ? C83 P4 C70 C66 163.3(6) . . . . ? C89 P4 C70 C66 -84.5(6) . . . . ? Pd2 P4 C70 C66 37.0(7) . . . . ? C83 P4 C70 Fe2 75.8(6) . . . . ? C89 P4 C70 Fe2 -172.1(5) . . . . ? Pd2 P4 C70 Fe2 -50.6(7) . . . . ? C61 Fe2 C70 C69 143.2(6) . . . . ? C65 Fe2 C70 C69 98.4(6) . . . . ? C66 Fe2 C70 C69 -117.5(7) . . . . ? C62 Fe2 C70 C69 179.7(6) . . . . ? C68 Fe2 C70 C69 -37.4(6) . . . . ? C64 Fe2 C70 C69 62.1(7) . . . . ? C67 Fe2 C70 C69 -80.9(6) . . . . ? C63 Fe2 C70 C69 67(7) . . . . ? C61 Fe2 C70 C66 -99.2(5) . . . . ? C65 Fe2 C70 C66 -144.0(5) . . . . ? C69 Fe2 C70 C66 117.5(7) . . . . ? C62 Fe2 C70 C66 -62.8(7) . . . . ? C68 Fe2 C70 C66 80.1(6) . . . . ? C64 Fe2 C70 C66 179.6(5) . . . . ? C67 Fe2 C70 C66 36.7(5) . . . . ? C63 Fe2 C70 C66 -175(91) . . . . ? C61 Fe2 C70 P4 20.6(7) . . . . ? C65 Fe2 C70 P4 -24.2(7) . . . . ? C69 Fe2 C70 P4 -122.6(8) . . . . ? C66 Fe2 C70 P4 119.8(8) . . . . ? C62 Fe2 C70 P4 57.1(8) . . . . ? C68 Fe2 C70 P4 -160.0(7) . . . . ? C64 Fe2 C70 P4 -60.5(8) . . . . ? C67 Fe2 C70 P4 156.5(7) . . . . ? C63 Fe2 C70 P4 -55(7) . . . . ? C77 P3 C71 C76 136.9(7) . . . . ? C61 P3 C71 C76 29.0(7) . . . . ? Pd2 P3 C71 C76 -103.4(6) . . . . ? C77 P3 C71 C72 -38.7(8) . . . . ? C61 P3 C71 C72 -146.6(7) . . . . ? Pd2 P3 C71 C72 81.0(7) . . . . ? C76 C71 C72 C73 -1.5(12) . . . . ? P3 C71 C72 C73 174.2(6) . . . . ? C71 C72 C73 C74 1.1(13) . . . . ? C72 C73 C74 C75 -0.9(15) . . . . ? C73 C74 C75 C76 1.1(14) . . . . ? C72 C71 C76 C75 1.8(12) . . . . ? P3 C71 C76 C75 -174.0(6) . . . . ? C74 C75 C76 C71 -1.6(14) . . . . ? C61 P3 C77 C82 -102.7(7) . . . . ? C71 P3 C77 C82 150.5(7) . . . . ? Pd2 P3 C77 C82 28.3(8) . . . . ? C61 P3 C77 C78 69.5(7) . . . . ? C71 P3 C77 C78 -37.3(8) . . . . ? Pd2 P3 C77 C78 -159.5(6) . . . . ? C82 C77 C78 C79 0.8(13) . . . . ? P3 C77 C78 C79 -171.4(6) . . . . ? C77 C78 C79 C80 2.1(13) . . . . ? C78 C79 C80 C81 -2.9(16) . . . . ? C79 C80 C81 C82 0.6(17) . . . . ? C80 C81 C82 C77 2.3(16) . . . . ? C78 C77 C82 C81 -3.0(14) . . . . ? P3 C77 C82 C81 169.1(8) . . . . ? C70 P4 C83 C84 -115.7(7) . . . . ? C89 P4 C83 C84 133.1(7) . . . . ? Pd2 P4 C83 C84 16.4(7) . . . . ? C70 P4 C83 C88 61.4(8) . . . . ? C89 P4 C83 C88 -49.7(8) . . . . ? Pd2 P4 C83 C88 -166.4(7) . . . . ? C88 C83 C84 C85 0.7(13) . . . . ? P4 C83 C84 C85 177.9(7) . . . . ? C83 C84 C85 C86 0.1(13) . . . . ? C84 C85 C86 C87 -0.6(15) . . . . ? C85 C86 C87 C88 0.2(16) . . . . ? C84 C83 C88 C87 -1.1(14) . . . . ? P4 C83 C88 C87 -178.3(8) . . . . ? C86 C87 C88 C83 0.6(16) . . . . ? C83 P4 C89 C94 164.3(7) . . . . ? C70 P4 C89 C94 50.7(8) . . . . ? Pd2 P4 C89 C94 -78.2(7) . . . . ? C83 P4 C89 C90 -19.6(8) . . . . ? C70 P4 C89 C90 -133.2(8) . . . . ? Pd2 P4 C89 C90 97.9(7) . . . . ? C94 C89 C90 C91 1.2(13) . . . . ? P4 C89 C90 C91 -174.9(7) . . . . ? C89 C90 C91 C92 -0.4(14) . . . . ? C90 C91 C92 C93 0.1(15) . . . . ? C91 C92 C93 C94 -0.5(14) . . . . ? C92 C93 C94 C89 1.3(13) . . . . ? C90 C89 C94 C93 -1.6(13) . . . . ? P4 C89 C94 C93 174.5(7) . . . . ? O2A S1A C1A F3A 58.4(7) . . . . ? O1A S1A C1A F3A -61.1(7) . . . . ? O3A S1A C1A F3A 178.6(6) . . . . ? O2A S1A C1A F2A -61.9(7) . . . . ? O1A S1A C1A F2A 178.6(6) . . . . ? O3A S1A C1A F2A 58.4(6) . . . . ? O2A S1A C1A F1A 177.8(6) . . . . ? O1A S1A C1A F1A 58.3(7) . . . . ? O3A S1A C1A F1A -62.0(7) . . . . ? O3B S1B C1B F2B -58.7(9) . . . . ? O1B S1B C1B F2B 176.3(8) . . . . ? O2B S1B C1B F2B 58.4(8) . . . . ? O3B S1B C1B F1B 61.8(8) . . . . ? O1B S1B C1B F1B -63.2(8) . . . . ? O2B S1B C1B F1B 178.9(7) . . . . ? O3B S1B C1B F3B 178.7(8) . . . . ? O1B S1B C1B F3B 53.7(8) . . . . ? O2B S1B C1B F3B -64.2(8) . . . . ? O1T S1T C1T F1T 34.2(13) . . . . ? O3T S1T C1T F1T -81.5(15) . . . . ? O2T S1T C1T F1T 155.0(14) . . . . ? O1T S1T C1T F2T -73.2(12) . . . . ? O3T S1T C1T F2T 171.1(13) . . . . ? O2T S1T C1T F2T 47.5(14) . . . . ? O1T S1T C1T F3T 161.9(13) . . . . ? O3T S1T C1T F3T 46.2(16) . . . . ? O2T S1T C1T F3T -77.3(16) . . . . ? F3D C1D S2D O1D -175.2(10) . . . . ? F2D C1D S2D O1D 57.8(12) . . . . ? F1D C1D S2D O1D -56.7(9) . . . . ? F3D C1D S2D O3D -56.6(13) . . . . ? F2D C1D S2D O3D 176.3(11) . . . . ? F1D C1D S2D O3D 61.8(10) . . . . ? F3D C1D S2D O2D 64.9(11) . . . . ? F2D C1D S2D O2D -62.1(12) . . . . ? F1D C1D S2D O2D -176.7(8) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 2.889 _refine_diff_density_min -2.727 _refine_diff_density_rms 0.194 #===END