# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a1 _database_code_depnum_ccdc_archive 'CCDC 894034' #TrackingRef 'web_deposit_cif_file_0_DrAndreiV.Churakov_1354804993.1_07str03.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H18 N2 O14 Pd4, C7 H8' _chemical_formula_sum 'C19 H26 N2 O14 Pd4' _chemical_formula_weight 932.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2/c' _symmetry_space_group_name_Hall '-P 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.788(3) _cell_length_b 8.531(2) _cell_length_c 13.945(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.170(4) _cell_angle_gamma 90.00 _cell_volume 1375.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2042 _cell_measurement_theta_min 2.814 _cell_measurement_theta_max 25.427 _exptl_crystal_description block _exptl_crystal_colour dark-orange _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 2.641 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8576 _exptl_absorpt_correction_T_max 0.9491 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8630 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2677 _reflns_number_gt 1949 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+9.7251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2677 _refine_ls_number_parameters 164 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0819 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1378 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.04966(6) 0.07694(8) 0.61142(5) 0.0361(2) Uani 1 1 d . . . Pd2 Pd 0.19521(6) 0.09190(8) 0.80555(5) 0.0346(2) Uani 1 1 d . . . N1 N 0.0955(7) 0.1755(8) 0.8863(5) 0.0354(17) Uani 1 1 d . . . O1 O 0.1251(7) 0.2863(7) 0.9352(5) 0.0517(19) Uani 1 1 d . . . O11 O 0.1868(6) -0.1297(7) 0.8527(5) 0.0435(16) Uani 1 1 d . . . O12 O 0.0082(6) -0.1449(7) 0.8814(5) 0.0436(16) Uani 1 1 d . . . C11 C 0.1023(9) -0.2007(11) 0.8705(7) 0.040(2) Uani 1 1 d . . . C12 C 0.1131(10) -0.3770(11) 0.8823(8) 0.050(3) Uani 1 1 d . . . H12A H 0.1928 -0.4041 0.9123 0.075 Uiso 1 1 calc R . . H12B H 0.0926 -0.4271 0.8180 0.075 Uiso 1 1 calc R . . H12C H 0.0607 -0.4138 0.9242 0.075 Uiso 1 1 calc R . . O21 O 0.1988(7) -0.0274(10) 0.5874(6) 0.061(2) Uani 1 1 d . . . O22 O 0.3158(6) 0.0076(9) 0.7310(6) 0.0554(19) Uani 1 1 d . . . C21 C 0.2942(10) -0.0377(11) 0.6457(10) 0.050(3) Uani 1 1 d . . . C22 C 0.3920(12) -0.1105(15) 0.6058(12) 0.081(5) Uani 1 1 d . . . H22A H 0.4646 -0.0967 0.6530 0.122 Uiso 1 1 calc R . . H22B H 0.3981 -0.0596 0.5440 0.122 Uiso 1 1 calc R . . H22C H 0.3769 -0.2226 0.5945 0.122 Uiso 1 1 calc R . . O31 O 0.1210(7) 0.2924(9) 0.6035(5) 0.057(2) Uani 1 1 d . . . O32 O 0.2188(6) 0.3153(8) 0.7562(5) 0.0471(17) Uani 1 1 d . . . C31 C 0.1837(8) 0.3629(10) 0.6711(7) 0.036(2) Uani 1 1 d . . . C32 C 0.2231(9) 0.5261(11) 0.6503(8) 0.045(2) Uani 1 1 d . . . H32A H 0.2606 0.5757 0.7117 0.067 Uiso 1 1 calc R . . H32B H 0.1560 0.5887 0.6198 0.067 Uiso 1 1 calc R . . H32C H 0.2781 0.5196 0.6060 0.067 Uiso 1 1 calc R . . C1 C 0.501(2) 0.562(2) 0.4674(13) 0.071(7) Uiso 0.50 1 d PGD A -1 C2 C 0.4271(18) 0.438(3) 0.4338(12) 0.14(3) Uiso 0.50 1 d PG A -1 H2A H 0.3860 0.4370 0.3681 0.167 Uiso 0.50 1 calc PR A -1 C3 C 0.4139(19) 0.315(2) 0.4964(16) 0.080(8) Uiso 0.50 1 d PG A -1 H3A H 0.3637 0.2307 0.4734 0.096 Uiso 0.50 1 calc PR A -1 C4 C 0.474(2) 0.317(2) 0.5925(15) 0.087(19) Uiso 0.50 1 d PG A -1 H4A H 0.4650 0.2331 0.6352 0.104 Uiso 0.50 1 calc PR A -1 C5 C 0.5475(19) 0.441(3) 0.6260(11) 0.109(12) Uiso 0.50 1 d PG A -1 H5A H 0.5887 0.4420 0.6917 0.130 Uiso 0.50 1 calc PR A -1 C6 C 0.5608(16) 0.564(2) 0.5635(13) 0.058(10) Uiso 0.50 1 d PG A -1 H6A H 0.6110 0.6483 0.5864 0.069 Uiso 0.50 1 calc PR A -1 C7 C 0.526(5) 0.697(5) 0.409(4) 0.16(4) Uiso 0.50 1 d PD A -1 H7A H 0.5525 0.6595 0.3508 0.234 Uiso 0.50 1 calc PR A -1 H7B H 0.5873 0.7609 0.4486 0.234 Uiso 0.50 1 calc PR A -1 H7C H 0.4565 0.7607 0.3898 0.234 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0530(5) 0.0252(4) 0.0338(4) -0.0053(3) 0.0175(3) -0.0114(3) Pd2 0.0457(4) 0.0178(4) 0.0416(4) 0.0026(3) 0.0118(3) 0.0007(3) N1 0.063(5) 0.014(3) 0.029(4) 0.000(3) 0.007(3) -0.001(3) O1 0.096(6) 0.019(3) 0.040(4) -0.002(3) 0.013(4) -0.004(3) O11 0.064(5) 0.025(3) 0.046(4) 0.004(3) 0.023(3) 0.008(3) O12 0.057(4) 0.023(3) 0.055(4) 0.009(3) 0.021(3) 0.009(3) C11 0.053(6) 0.028(5) 0.041(5) -0.002(4) 0.012(5) -0.001(4) C12 0.078(8) 0.023(5) 0.050(6) -0.002(4) 0.018(6) 0.004(5) O21 0.057(5) 0.063(5) 0.072(5) -0.031(4) 0.037(4) -0.023(4) O22 0.054(5) 0.048(5) 0.069(5) 0.004(4) 0.026(4) 0.006(4) C21 0.051(7) 0.014(4) 0.092(9) -0.013(5) 0.034(7) -0.009(4) C22 0.075(9) 0.050(7) 0.135(13) -0.025(8) 0.060(9) 0.000(7) O31 0.077(5) 0.046(5) 0.048(4) 0.005(3) 0.015(4) -0.031(4) O32 0.067(5) 0.029(3) 0.047(4) -0.001(3) 0.015(4) -0.010(3) C31 0.044(5) 0.021(4) 0.045(6) 0.000(4) 0.015(4) -0.004(4) C32 0.062(6) 0.023(5) 0.051(6) 0.002(4) 0.019(5) -0.011(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 Pd1 N1 1.913(8) 2_556 ? Pd1 O12 2.021(6) 2_556 ? Pd1 O31 2.033(7) . ? Pd1 O21 2.055(8) . ? Pd1 Pd2 2.9136(12) . ? Pd1 Pd2 3.3142(12) 2_556 ? Pd1 Pd1 3.3679(15) 3_556 ? Pd2 N1 1.915(8) . ? Pd2 O11 2.010(6) . ? Pd2 O22 2.047(7) . ? Pd2 O32 2.063(7) . ? N1 O1 1.179(9) . ? O11 C11 1.232(11) . ? O12 C11 1.242(11) . ? C11 C12 1.515(13) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? O21 C21 1.257(14) . ? O22 C21 1.230(13) . ? C21 C22 1.508(15) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O31 C31 1.235(11) . ? O32 C31 1.246(11) . ? C31 C32 1.513(12) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C1 C7 1.473(19) . ? C2 C3 1.3900 . ? C2 H2A 0.9500 . ? C3 C4 1.3900 . ? C3 H3A 0.9500 . ? C4 C5 1.3900 . ? C4 H4A 0.9500 . ? C5 C6 1.3900 . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? 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 O12 95.7(3) 2_556 2_556 ? N1 Pd1 O31 89.1(3) 2_556 . ? O12 Pd1 O31 175.2(3) 2_556 . ? N1 Pd1 O21 171.7(3) 2_556 . ? O12 Pd1 O21 84.9(3) 2_556 . ? O31 Pd1 O21 90.4(3) . . ? N1 Pd1 Pd2 109.4(2) 2_556 . ? O12 Pd1 Pd2 98.0(2) 2_556 . ? O31 Pd1 Pd2 80.5(2) . . ? O21 Pd1 Pd2 78.6(2) . . ? N1 Pd1 Pd2 30.1(2) 2_556 2_556 ? O12 Pd1 Pd2 72.14(19) 2_556 2_556 ? O31 Pd1 Pd2 112.4(2) . 2_556 ? O21 Pd1 Pd2 154.7(2) . 2_556 ? Pd2 Pd1 Pd2 93.99(3) . 2_556 ? N1 Pd1 Pd1 92.0(2) 2_556 3_556 ? O12 Pd1 Pd1 67.7(2) 2_556 3_556 ? O31 Pd1 Pd1 112.1(2) . 3_556 ? O21 Pd1 Pd1 80.6(2) . 3_556 ? Pd2 Pd1 Pd1 155.69(4) . 3_556 ? Pd2 Pd1 Pd1 99.60(4) 2_556 3_556 ? N1 Pd2 O11 94.8(3) . . ? N1 Pd2 O22 174.0(3) . . ? O11 Pd2 O22 85.3(3) . . ? N1 Pd2 O32 89.4(3) . . ? O11 Pd2 O32 174.9(3) . . ? O22 Pd2 O32 90.2(3) . . ? N1 Pd2 Pd1 104.2(2) . . ? O11 Pd2 Pd1 101.8(2) . . ? O22 Pd2 Pd1 81.6(2) . . ? O32 Pd2 Pd1 79.8(2) . . ? O1 N1 Pd1 120.5(7) . 2_556 ? O1 N1 Pd2 119.5(7) . . ? Pd1 N1 Pd2 119.9(4) 2_556 . ? C11 O11 Pd2 128.4(6) . . ? C11 O12 Pd1 133.1(6) . 2_556 ? O11 C11 O12 127.7(9) . . ? O11 C11 C12 117.1(9) . . ? O12 C11 C12 115.2(9) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 O21 Pd1 127.7(7) . . ? C21 O22 Pd2 124.6(7) . . ? O22 C21 O21 126.5(10) . . ? O22 C21 C22 117.2(12) . . ? O21 C21 C22 116.3(12) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C31 O31 Pd1 126.2(6) . . ? C31 O32 Pd2 125.3(6) . . ? O31 C31 O32 127.4(8) . . ? O31 C31 C32 117.5(9) . . ? O32 C31 C32 115.1(8) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C2 C1 C6 120.0 . . ? C2 C1 C7 126(2) . . ? C6 C1 C7 114(2) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2A 120.0 . . ? C3 C2 H2A 120.0 . . ? C4 C3 C2 120.0 . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.0 . . ? C4 C5 H5A 120.0 . . ? C6 C5 H5A 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C1 C7 H7A 109.5 . . ? C1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.479 _refine_diff_density_min -1.154 _refine_diff_density_rms 0.187 data_z1 _database_code_depnum_ccdc_archive 'CCDC 894035' #TrackingRef 'web_deposit_cif_file_1_DrAndreiV.Churakov_1354804993.3_12str04.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H66 N2 O14 Pd4' _chemical_formula_sum 'C42 H66 N2 O14 Pd4' _chemical_formula_weight 1248.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.2473(11) _cell_length_b 13.4637(11) _cell_length_c 27.762(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.7640(10) _cell_angle_gamma 90.00 _cell_volume 4829.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 9851 _cell_measurement_theta_min 2.194 _cell_measurement_theta_max 30.554 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 1.529 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7704 _exptl_absorpt_correction_T_max 0.9414 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45151 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.00 _reflns_number_total 10532 _reflns_number_gt 9163 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered cyclohexyl ring was refined with restrained C-C distances (SADI). ; _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^)+(0.0162P)^2^+4.4785P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10532 _refine_ls_number_parameters 555 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0718 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.023 _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 Pd1 Pd 0.283672(16) 0.398139(16) 0.278457(8) 0.01818(6) Uani 1 1 d . . . Pd2 Pd 0.175190(16) 0.211110(16) 0.288895(8) 0.01835(6) Uani 1 1 d . . . Pd3 Pd -0.008299(17) 0.264648(16) 0.193546(8) 0.02057(6) Uani 1 1 d . . . Pd4 Pd 0.062223(16) 0.472373(16) 0.209108(8) 0.01876(6) Uani 1 1 d . . . N1 N 0.20972(18) 0.46167(17) 0.21994(9) 0.0210(5) Uani 1 1 d . . . O1 O 0.25501(17) 0.49298(18) 0.19038(8) 0.0330(5) Uani 1 1 d . . . N2 N 0.10589(18) 0.18083(17) 0.22280(9) 0.0205(5) Uani 1 1 d . . . O2 O 0.13516(16) 0.11690(16) 0.19993(8) 0.0277(5) Uani 1 1 d . . . O11 O 0.22324(15) 0.48583(15) 0.32335(7) 0.0237(4) Uani 1 1 d . . . O12 O 0.05789(15) 0.50347(15) 0.28052(7) 0.0230(4) Uani 1 1 d . . . O21 O 0.37341(15) 0.34189(15) 0.34236(7) 0.0233(4) Uani 1 1 d . . . O22 O 0.25390(15) 0.23842(16) 0.36071(7) 0.0247(4) Uani 1 1 d . . . O31 O 0.35719(16) 0.30936(15) 0.23809(8) 0.0262(5) Uani 1 1 d . . . O32 O 0.30993(15) 0.16787(15) 0.27058(7) 0.0223(4) Uani 1 1 d . . . O41 O 0.04385(16) 0.23982(16) 0.31376(8) 0.0260(5) Uani 1 1 d . . . O42 O -0.08656(16) 0.23272(16) 0.24592(8) 0.0276(5) Uani 1 1 d . . . O51 O -0.13724(16) 0.34415(15) 0.15963(8) 0.0278(5) Uani 1 1 d . . . O52 O -0.09589(15) 0.49292(15) 0.19474(7) 0.0249(4) Uani 1 1 d . . . O61 O 0.05901(18) 0.28640(16) 0.13507(8) 0.0294(5) Uani 1 1 d . . . O62 O 0.05565(17) 0.45380(16) 0.13534(7) 0.0260(5) Uani 1 1 d . . . C11 C 0.1298(2) 0.5105(2) 0.31872(10) 0.0194(6) Uani 1 1 d . . . C12 C 0.1018(2) 0.5484(2) 0.36542(10) 0.0216(6) Uani 1 1 d . . . H12 H 0.0353 0.5861 0.3560 0.026 Uiso 1 1 calc R . . C13 C 0.0847(3) 0.4591(3) 0.39675(12) 0.0321(7) Uani 1 1 d . . . H13A H 0.1490 0.4193 0.4054 0.038 Uiso 1 1 calc R . . H13B H 0.0293 0.4164 0.3775 0.038 Uiso 1 1 calc R . . C14 C 0.0540(3) 0.4938(3) 0.44411(13) 0.0466(10) Uani 1 1 d . . . H14A H -0.0148 0.5261 0.4355 0.056 Uiso 1 1 calc R . . H14B H 0.0486 0.4354 0.4651 0.056 Uiso 1 1 calc R . . C15 C 0.1317(3) 0.5658(3) 0.47277(12) 0.0475(10) Uani 1 1 d . . . H15A H 0.1979 0.5307 0.4855 0.057 Uiso 1 1 calc R . . H15B H 0.1063 0.5908 0.5015 0.057 Uiso 1 1 calc R . . C16 C 0.1505(3) 0.6529(3) 0.44133(12) 0.0372(8) Uani 1 1 d . . . H16A H 0.2048 0.6963 0.4609 0.045 Uiso 1 1 calc R . . H16B H 0.0862 0.6924 0.4316 0.045 Uiso 1 1 calc R . . C17 C 0.1843(2) 0.6174(2) 0.39516(11) 0.0249(6) Uani 1 1 d . . . H17A H 0.2510 0.5815 0.4047 0.030 Uiso 1 1 calc R . . H17B H 0.1943 0.6752 0.3747 0.030 Uiso 1 1 calc R . . C21 C 0.3381(2) 0.2853(2) 0.37126(11) 0.0225(6) Uani 1 1 d . . . C22 C 0.4033(2) 0.2753(2) 0.42286(11) 0.0253(6) Uani 1 1 d . . . H22 H 0.3756 0.2185 0.4393 0.030 Uiso 1 1 calc R . . C23 C 0.3961(3) 0.3693(3) 0.45291(12) 0.0343(7) Uani 1 1 d . . . H23A H 0.4219 0.4270 0.4370 0.041 Uiso 1 1 calc R . . H23B H 0.3229 0.3821 0.4538 0.041 Uiso 1 1 calc R . . C24 C 0.4602(3) 0.3572(3) 0.50544(13) 0.0436(9) Uani 1 1 d . . . H24A H 0.4582 0.4198 0.5238 0.052 Uiso 1 1 calc R . . H24B H 0.4292 0.3043 0.5223 0.052 Uiso 1 1 calc R . . C25 C 0.5718(3) 0.3308(3) 0.50639(13) 0.0450(9) Uani 1 1 d . . . H25A H 0.6059 0.3879 0.4940 0.054 Uiso 1 1 calc R . . H25B H 0.6088 0.3177 0.5409 0.054 Uiso 1 1 calc R . . C26 C 0.5799(3) 0.2403(3) 0.47510(14) 0.0422(9) Uani 1 1 d . . . H26A H 0.5550 0.1812 0.4902 0.051 Uiso 1 1 calc R . . H26B H 0.6533 0.2291 0.4742 0.051 Uiso 1 1 calc R . . C27 C 0.5163(2) 0.2531(3) 0.42253(12) 0.0311(7) Uani 1 1 d . . . H27A H 0.5203 0.1917 0.4034 0.037 Uiso 1 1 calc R . . H27B H 0.5452 0.3083 0.4062 0.037 Uiso 1 1 calc R . . C31 C 0.3625(2) 0.2168(2) 0.24610(11) 0.0227(6) Uani 1 1 d . . . C32 C 0.4357(2) 0.1576(2) 0.22231(11) 0.0253(6) Uani 1 1 d . . . H32 H 0.4513 0.0935 0.2407 0.030 Uiso 1 1 calc R . . C33 C 0.3818(3) 0.1339(3) 0.16922(14) 0.0465(10) Uani 1 1 d . . . H33A H 0.3643 0.1963 0.1504 0.056 Uiso 1 1 calc R . . H33B H 0.3167 0.0974 0.1688 0.056 Uiso 1 1 calc R . . C34 C 0.4533(3) 0.0703(4) 0.14502(15) 0.0523(11) Uani 1 1 d . . . H34A H 0.4658 0.0057 0.1623 0.063 Uiso 1 1 calc R . . H34B H 0.4188 0.0570 0.1102 0.063 Uiso 1 1 calc R . . C35 C 0.5551(3) 0.1210(3) 0.14676(13) 0.0379(8) Uani 1 1 d . . . H35A H 0.6006 0.0764 0.1327 0.046 Uiso 1 1 calc R . . H35B H 0.5433 0.1820 0.1263 0.046 Uiso 1 1 calc R . . C36 C 0.6076(3) 0.1479(3) 0.19868(15) 0.0420(9) Uani 1 1 d . . . H36A H 0.6715 0.1857 0.1983 0.050 Uiso 1 1 calc R . . H36B H 0.6275 0.0864 0.2180 0.050 Uiso 1 1 calc R . . C37 C 0.5369(3) 0.2106(3) 0.22369(15) 0.0408(9) Uani 1 1 d . . . H37A H 0.5723 0.2235 0.2584 0.049 Uiso 1 1 calc R . . H37B H 0.5231 0.2753 0.2066 0.049 Uiso 1 1 calc R . . C41 C -0.0498(2) 0.2355(2) 0.29188(11) 0.0238(6) Uani 1 1 d . . . C42 C -0.1309(2) 0.2387(2) 0.32312(12) 0.0276(7) Uani 1 1 d . . . H42 H -0.1830 0.1856 0.3107 0.033 Uiso 1 1 calc R . . C43 C -0.1863(3) 0.3388(3) 0.31385(13) 0.0421(9) Uani 1 1 d . . . H43A H -0.1348 0.3930 0.3219 0.050 Uiso 1 1 calc R . . H43B H -0.2203 0.3444 0.2784 0.050 Uiso 1 1 calc R . . C44 C -0.2674(3) 0.3506(4) 0.34488(14) 0.0533(11) Uani 1 1 d . . . H44A H -0.2978 0.4180 0.3400 0.064 Uiso 1 1 calc R . . H44B H -0.3237 0.3018 0.3339 0.064 Uiso 1 1 calc R . . C45 C -0.2195(3) 0.3348(3) 0.39927(13) 0.0446(9) Uani 1 1 d . . . H45A H -0.1667 0.3866 0.4108 0.054 Uiso 1 1 calc R . . H45B H -0.2737 0.3411 0.4186 0.054 Uiso 1 1 calc R . . C46 C -0.1701(3) 0.2339(3) 0.40796(15) 0.0460(9) Uani 1 1 d . . . H46A H -0.2240 0.1821 0.3987 0.055 Uiso 1 1 calc R . . H46B H -0.1382 0.2260 0.4435 0.055 Uiso 1 1 calc R . . C47 C -0.0875(3) 0.2194(3) 0.37789(12) 0.0327(7) Uani 1 1 d . . . H47A H -0.0291 0.2654 0.3902 0.039 Uiso 1 1 calc R . . H47B H -0.0605 0.1507 0.3824 0.039 Uiso 1 1 calc R . . C51 C -0.1585(2) 0.4327(2) 0.16889(10) 0.0228(6) Uani 1 1 d . . . C52 C -0.2676(2) 0.4689(2) 0.14796(11) 0.0245(6) Uani 1 1 d . . . H52 H -0.2654 0.5429 0.1455 0.029 Uiso 1 1 calc R . . C53 C -0.3125(3) 0.4281(3) 0.09642(12) 0.0381(8) Uani 1 1 d . . . H53A H -0.3152 0.3547 0.0977 0.046 Uiso 1 1 calc R . . H53B H -0.2673 0.4470 0.0739 0.046 Uiso 1 1 calc R . . C54 C -0.4212(3) 0.4691(3) 0.07678(14) 0.0472(10) Uani 1 1 d . . . H54A H -0.4174 0.5420 0.0730 0.057 Uiso 1 1 calc R . . H54B H -0.4502 0.4403 0.0438 0.057 Uiso 1 1 calc R . . C55 C -0.4923(3) 0.4451(3) 0.11127(16) 0.0507(11) Uani 1 1 d . . . H55A H -0.5603 0.4771 0.0988 0.061 Uiso 1 1 calc R . . H55B H -0.5033 0.3724 0.1117 0.061 Uiso 1 1 calc R . . C56 C -0.4472(3) 0.4809(3) 0.16329(15) 0.0427(9) Uani 1 1 d . . . H56A H -0.4921 0.4585 0.1854 0.051 Uiso 1 1 calc R . . H56B H -0.4461 0.5544 0.1636 0.051 Uiso 1 1 calc R . . C57 C -0.3379(2) 0.4423(3) 0.18290(12) 0.0329(7) Uani 1 1 d . . . H57A H -0.3399 0.3692 0.1867 0.040 Uiso 1 1 calc R . . H57B H -0.3095 0.4714 0.2158 0.040 Uiso 1 1 calc R . . C61 C 0.0663(2) 0.3706(2) 0.11600(11) 0.0253(6) Uani 1 1 d . B . C62 C 0.0889(3) 0.3711(2) 0.06481(12) 0.0374(8) Uani 1 1 d D . . H62B H 0.0239 0.3825 0.0392 0.045 Uiso 0.48 1 calc PR A 2 H62A H 0.0211 0.3647 0.0438 0.045 Uiso 0.52 1 d PR A 1 C63A C 0.1265(6) 0.4699(3) 0.0479(2) 0.0418(17) Uiso 0.52 1 d PD B 1 H63A H 0.1925 0.4897 0.0703 0.050 Uiso 0.52 1 calc PR B 1 H63B H 0.0747 0.5226 0.0486 0.050 Uiso 0.52 1 calc PR B 1 C64A C 0.1421(6) 0.4564(6) -0.0048(2) 0.0490(19) Uiso 0.52 1 d PD B 1 H64A H 0.1602 0.5210 -0.0178 0.059 Uiso 0.52 1 calc PR B 1 H64B H 0.0771 0.4325 -0.0265 0.059 Uiso 0.52 1 calc PR B 1 C65A C 0.2292(6) 0.3811(5) -0.0050(4) 0.053(3) Uiso 0.52 1 d PD B 1 H65A H 0.2513 0.3810 -0.0368 0.063 Uiso 0.52 1 calc PR B 1 H65B H 0.2899 0.3931 0.0224 0.063 Uiso 0.52 1 calc PR B 1 C66A C 0.1723(7) 0.2851(6) 0.00263(19) 0.040(2) Uiso 0.52 1 d PD B 1 H66A H 0.2165 0.2278 -0.0015 0.048 Uiso 0.52 1 calc PR B 1 H66B H 0.1081 0.2806 -0.0235 0.048 Uiso 0.52 1 calc PR B 1 C63B C 0.1677(6) 0.4539(5) 0.0630(3) 0.0432(19) Uiso 0.48 1 d PD B 2 H63C H 0.1395 0.5176 0.0720 0.052 Uiso 0.48 1 calc PR B 2 H63D H 0.2319 0.4398 0.0880 0.052 Uiso 0.48 1 calc PR B 2 C64B C 0.1950(8) 0.4657(5) 0.0123(3) 0.052(2) Uiso 0.48 1 d PD B 2 H64C H 0.2610 0.5025 0.0165 0.062 Uiso 0.48 1 calc PR B 2 H64D H 0.1406 0.5058 -0.0093 0.062 Uiso 0.48 1 calc PR B 2 C65B C 0.2053(8) 0.3662(5) -0.0132(4) 0.044(3) Uiso 0.48 1 d PD B 2 H65C H 0.1850 0.3778 -0.0493 0.053 Uiso 0.48 1 calc PR B 2 H65D H 0.2797 0.3485 -0.0056 0.053 Uiso 0.48 1 calc PR B 2 C66B C 0.1457(9) 0.2745(7) -0.00193(18) 0.052(3) Uiso 0.48 1 d PD B 2 H66C H 0.1802 0.2132 -0.0097 0.062 Uiso 0.48 1 calc PR B 2 H66D H 0.0742 0.2755 -0.0223 0.062 Uiso 0.48 1 calc PR B 2 C67 C 0.1436(3) 0.2767(3) 0.05311(13) 0.0488(10) Uani 1 1 d D B . H67C H 0.1067 0.2174 0.0615 0.059 Uiso 0.48 1 calc PR C 2 H67D H 0.2153 0.2751 0.0733 0.059 Uiso 0.48 1 calc PR C 2 H67A H 0.1000 0.2203 0.0544 0.059 Uiso 0.52 1 d PR C 1 H67B H 0.2064 0.2681 0.0777 0.059 Uiso 0.52 1 d PR C 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01882(11) 0.01835(11) 0.01906(11) 0.00044(8) 0.00780(8) 0.00116(8) Pd2 0.01744(11) 0.01920(11) 0.01932(11) -0.00055(8) 0.00606(8) -0.00057(8) Pd3 0.02150(11) 0.01848(11) 0.02172(12) -0.00255(8) 0.00474(9) 0.00188(8) Pd4 0.02102(11) 0.01867(11) 0.01711(11) -0.00112(8) 0.00535(8) 0.00048(8) N1 0.0242(12) 0.0187(12) 0.0212(12) -0.0002(10) 0.0073(10) -0.0012(10) O1 0.0297(12) 0.0436(14) 0.0288(12) 0.0111(10) 0.0134(10) -0.0006(10) N2 0.0193(12) 0.0190(12) 0.0248(12) -0.0013(10) 0.0087(10) -0.0035(9) O2 0.0237(11) 0.0279(12) 0.0313(12) -0.0097(9) 0.0055(9) 0.0024(9) O11 0.0197(10) 0.0284(11) 0.0233(10) -0.0059(9) 0.0058(8) 0.0024(8) O12 0.0206(10) 0.0308(11) 0.0178(10) -0.0033(8) 0.0051(8) 0.0010(8) O21 0.0224(10) 0.0253(11) 0.0225(10) 0.0037(8) 0.0055(8) 0.0002(8) O22 0.0213(10) 0.0328(12) 0.0207(10) -0.0018(9) 0.0060(8) -0.0036(9) O31 0.0306(11) 0.0232(11) 0.0293(11) 0.0021(9) 0.0161(9) 0.0053(9) O32 0.0194(10) 0.0229(11) 0.0263(11) 0.0006(8) 0.0084(8) 0.0028(8) O41 0.0213(10) 0.0316(12) 0.0273(11) -0.0020(9) 0.0099(9) 0.0005(9) O42 0.0219(11) 0.0335(12) 0.0287(12) -0.0027(9) 0.0083(9) -0.0004(9) O51 0.0256(11) 0.0226(11) 0.0323(12) -0.0024(9) -0.0001(9) 0.0047(9) O52 0.0222(10) 0.0274(11) 0.0244(11) -0.0056(9) 0.0036(8) 0.0029(9) O61 0.0391(13) 0.0290(12) 0.0224(11) -0.0007(9) 0.0117(9) 0.0051(10) O62 0.0343(12) 0.0270(11) 0.0182(10) 0.0002(9) 0.0091(9) 0.0011(9) C11 0.0221(14) 0.0163(13) 0.0208(14) -0.0004(11) 0.0069(11) -0.0020(11) C12 0.0172(13) 0.0272(15) 0.0200(14) -0.0022(12) 0.0032(11) 0.0028(11) C13 0.0350(18) 0.0351(18) 0.0293(17) 0.0001(14) 0.0142(14) -0.0078(14) C14 0.047(2) 0.066(3) 0.0326(19) -0.0003(18) 0.0231(17) -0.008(2) C15 0.038(2) 0.086(3) 0.0209(17) -0.0094(18) 0.0119(15) 0.001(2) C16 0.0245(16) 0.052(2) 0.0348(18) -0.0210(16) 0.0055(14) 0.0027(15) C17 0.0253(15) 0.0265(16) 0.0233(15) -0.0051(12) 0.0063(12) -0.0006(12) C21 0.0214(14) 0.0243(15) 0.0230(15) -0.0017(12) 0.0078(12) 0.0040(12) C22 0.0232(15) 0.0303(16) 0.0216(15) 0.0043(12) 0.0035(12) -0.0018(12) C23 0.0319(17) 0.045(2) 0.0254(16) -0.0044(15) 0.0042(13) 0.0017(15) C24 0.042(2) 0.062(3) 0.0258(17) -0.0075(17) 0.0052(15) -0.0028(18) C25 0.038(2) 0.065(3) 0.0276(18) 0.0033(18) -0.0022(15) -0.0085(18) C26 0.0278(18) 0.057(2) 0.037(2) 0.0096(18) -0.0028(15) 0.0017(16) C27 0.0229(16) 0.0379(19) 0.0301(17) 0.0029(14) 0.0005(13) 0.0026(13) C31 0.0204(14) 0.0266(16) 0.0213(14) -0.0017(12) 0.0047(11) 0.0032(12) C32 0.0269(15) 0.0237(15) 0.0281(16) 0.0012(12) 0.0121(13) 0.0056(12) C33 0.0266(18) 0.069(3) 0.046(2) -0.028(2) 0.0141(16) -0.0015(18) C34 0.035(2) 0.076(3) 0.050(2) -0.035(2) 0.0190(18) -0.0056(19) C35 0.0366(19) 0.042(2) 0.042(2) 0.0000(16) 0.0247(16) 0.0089(16) C36 0.0258(17) 0.041(2) 0.063(2) -0.0134(18) 0.0174(17) 0.0054(15) C37 0.0210(16) 0.048(2) 0.055(2) -0.0210(18) 0.0099(15) 0.0002(15) C41 0.0243(15) 0.0180(14) 0.0308(17) -0.0028(12) 0.0100(13) -0.0007(11) C42 0.0226(15) 0.0289(17) 0.0339(17) -0.0062(13) 0.0122(13) -0.0045(12) C43 0.0357(19) 0.060(3) 0.0305(18) -0.0009(17) 0.0070(15) 0.0173(18) C44 0.032(2) 0.082(3) 0.047(2) -0.016(2) 0.0101(17) 0.018(2) C45 0.0314(18) 0.067(3) 0.040(2) -0.0183(19) 0.0184(16) -0.0007(18) C46 0.048(2) 0.054(2) 0.043(2) -0.0001(18) 0.0252(18) -0.0094(19) C47 0.0360(18) 0.0326(18) 0.0339(18) 0.0051(14) 0.0173(15) 0.0024(14) C51 0.0250(15) 0.0226(15) 0.0210(14) 0.0004(12) 0.0056(12) 0.0028(12) C52 0.0239(15) 0.0212(15) 0.0265(15) 0.0003(12) 0.0013(12) 0.0027(12) C53 0.042(2) 0.043(2) 0.0256(17) -0.0059(15) -0.0020(14) 0.0125(16) C54 0.051(2) 0.047(2) 0.0332(19) -0.0141(17) -0.0141(17) 0.0195(18) C55 0.0307(19) 0.040(2) 0.071(3) -0.008(2) -0.0114(19) 0.0028(16) C56 0.0271(18) 0.047(2) 0.053(2) 0.0038(18) 0.0079(16) 0.0072(16) C57 0.0277(17) 0.0377(19) 0.0339(18) 0.0022(15) 0.0077(14) 0.0058(14) C61 0.0242(15) 0.0315(17) 0.0202(14) 0.0008(12) 0.0052(12) 0.0051(13) C62 0.043(2) 0.047(2) 0.0236(16) 0.0012(15) 0.0113(14) 0.0127(17) C67 0.069(3) 0.039(2) 0.047(2) -0.0029(18) 0.034(2) 0.0065(19) _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 1.905(2) . ? Pd1 O11 2.0074(19) . ? Pd1 O31 2.029(2) . ? Pd1 O21 2.050(2) . ? Pd1 Pd2 2.9452(3) . ? Pd1 Pd4 3.2888(4) . ? Pd2 N2 1.906(2) . ? Pd2 O41 2.045(2) . ? Pd2 O32 2.0457(19) . ? Pd2 O22 2.069(2) . ? Pd2 Pd3 3.2545(4) . ? Pd3 N2 1.918(2) . ? Pd3 O42 2.010(2) . ? Pd3 O61 2.038(2) . ? Pd3 O51 2.059(2) . ? Pd3 Pd4 2.9501(4) . ? Pd4 N1 1.916(2) . ? Pd4 O12 2.0394(19) . ? Pd4 O62 2.0458(19) . ? Pd4 O52 2.062(2) . ? N1 O1 1.195(3) . ? N2 O2 1.185(3) . ? O11 C11 1.261(3) . ? O12 C11 1.263(3) . ? O21 C21 1.268(3) . ? O22 C21 1.259(4) . ? O31 C31 1.265(4) . ? O32 C31 1.261(3) . ? O41 C41 1.257(4) . ? O42 C41 1.262(4) . ? O51 C51 1.265(3) . ? O52 C51 1.264(4) . ? O61 C61 1.265(4) . ? O62 C61 1.263(4) . ? C11 C12 1.514(4) . ? C12 C13 1.529(4) . ? C12 C17 1.530(4) . ? C12 H12 1.0000 . ? C13 C14 1.532(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.506(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.515(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.525(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C21 C22 1.506(4) . ? C22 C27 1.528(4) . ? C22 C23 1.531(5) . ? C22 H22 1.0000 . ? C23 C24 1.526(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.515(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.513(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.525(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C31 C32 1.515(4) . ? C32 C37 1.512(4) . ? C32 C33 1.523(5) . ? C32 H32 1.0000 . ? C33 C34 1.537(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.504(5) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.500(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.535(4) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C41 C42 1.523(4) . ? C42 C47 1.524(5) . ? C42 C43 1.529(5) . ? C42 H42 1.0000 . ? C43 C44 1.527(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.518(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.504(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.529(5) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C51 C52 1.514(4) . ? C52 C53 1.525(4) . ? C52 C57 1.529(4) . ? C52 H52 1.0000 . ? C53 C54 1.526(5) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.519(6) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.514(5) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.521(4) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C61 C62 1.515(4) . ? C62 C63A 1.531(3) . ? C62 C67 1.533(2) . ? C62 C63B 1.537(3) . ? C62 H62B 1.0000 . ? C62 H62A 0.9601 . ? C63A C64A 1.535(3) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A C65A 1.537(3) . ? C64A H64A 0.9900 . ? C64A H64B 0.9900 . ? C65A C66A 1.534(3) . ? C65A H65A 0.9900 . ? C65A H65B 0.9900 . ? C66A C67 1.535(3) . ? C66A H66A 0.9900 . ? C66A H66B 0.9900 . ? C63B C64B 1.535(3) . ? C63B H63C 0.9900 . ? C63B H63D 0.9900 . ? C64B C65B 1.536(3) . ? C64B H64C 0.9900 . ? C64B H64D 0.9900 . ? C65B C66B 1.534(3) . ? C65B H65C 0.9900 . ? C65B H65D 0.9900 . ? C66B C67 1.535(3) . ? C66B H66C 0.9900 . ? C66B H66D 0.9900 . ? C67 H67C 0.9900 . ? C67 H67D 0.9900 . ? C67 H67A 0.9598 . ? C67 H67B 0.9599 . ? 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 O11 93.72(9) . . ? N1 Pd1 O31 90.73(9) . . ? O11 Pd1 O31 174.61(8) . . ? N1 Pd1 O21 174.14(9) . . ? O11 Pd1 O21 85.09(8) . . ? O31 Pd1 O21 90.17(8) . . ? N1 Pd1 Pd2 107.32(7) . . ? O11 Pd1 Pd2 99.88(6) . . ? O31 Pd1 Pd2 81.65(6) . . ? O21 Pd1 Pd2 78.54(6) . . ? N1 Pd1 Pd4 30.68(7) . . ? O11 Pd1 Pd4 76.01(6) . . ? O31 Pd1 Pd4 109.31(6) . . ? O21 Pd1 Pd4 152.95(5) . . ? Pd2 Pd1 Pd4 85.750(9) . . ? N2 Pd2 O41 95.77(9) . . ? N2 Pd2 O32 87.76(9) . . ? O41 Pd2 O32 172.60(8) . . ? N2 Pd2 O22 177.57(9) . . ? O41 Pd2 O22 85.78(8) . . ? O32 Pd2 O22 90.49(8) . . ? N2 Pd2 Pd1 103.29(7) . . ? O41 Pd2 Pd1 109.97(6) . . ? O32 Pd2 Pd1 75.37(6) . . ? O22 Pd2 Pd1 77.87(6) . . ? N2 Pd2 Pd3 31.77(7) . . ? O41 Pd2 Pd3 72.21(6) . . ? O32 Pd2 Pd3 113.38(6) . . ? O22 Pd2 Pd3 150.63(6) . . ? Pd1 Pd2 Pd3 91.352(9) . . ? N2 Pd3 O42 93.00(9) . . ? N2 Pd3 O61 88.79(9) . . ? O42 Pd3 O61 173.25(9) . . ? N2 Pd3 O51 175.24(9) . . ? O42 Pd3 O51 86.19(9) . . ? O61 Pd3 O51 91.48(9) . . ? N2 Pd3 Pd4 107.53(7) . . ? O42 Pd3 Pd4 107.10(6) . . ? O61 Pd3 Pd4 78.48(6) . . ? O51 Pd3 Pd4 77.17(6) . . ? N2 Pd3 Pd2 31.55(7) . . ? O42 Pd3 Pd2 77.06(6) . . ? O61 Pd3 Pd2 107.46(6) . . ? O51 Pd3 Pd2 151.91(6) . . ? Pd4 Pd3 Pd2 86.296(8) . . ? N1 Pd4 O12 96.30(9) . . ? N1 Pd4 O62 87.95(9) . . ? O12 Pd4 O62 173.76(8) . . ? N1 Pd4 O52 175.99(9) . . ? O12 Pd4 O52 85.12(8) . . ? O62 Pd4 O52 90.35(8) . . ? N1 Pd4 Pd3 103.34(7) . . ? O12 Pd4 Pd3 105.13(6) . . ? O62 Pd4 Pd3 78.20(6) . . ? O52 Pd4 Pd3 79.84(6) . . ? N1 Pd4 Pd1 30.49(7) . . ? O12 Pd4 Pd1 72.92(6) . . ? O62 Pd4 Pd1 112.59(6) . . ? O52 Pd4 Pd1 152.92(6) . . ? Pd3 Pd4 Pd1 90.589(9) . . ? O1 N1 Pd1 120.2(2) . . ? O1 N1 Pd4 121.0(2) . . ? Pd1 N1 Pd4 118.83(12) . . ? O2 N2 Pd2 121.8(2) . . ? O2 N2 Pd3 121.4(2) . . ? Pd2 N2 Pd3 116.68(12) . . ? C11 O11 Pd1 127.50(18) . . ? C11 O12 Pd4 130.83(18) . . ? C21 O21 Pd1 123.03(19) . . ? C21 O22 Pd2 123.05(18) . . ? C31 O31 Pd1 119.89(18) . . ? C31 O32 Pd2 126.97(18) . . ? C41 O41 Pd2 130.6(2) . . ? C41 O42 Pd3 125.43(19) . . ? C51 O51 Pd3 126.65(19) . . ? C51 O52 Pd4 122.35(18) . . ? C61 O61 Pd3 123.36(19) . . ? C61 O62 Pd4 123.36(19) . . ? O11 C11 O12 127.4(3) . . ? O11 C11 C12 115.0(2) . . ? O12 C11 C12 117.5(2) . . ? C11 C12 C13 108.5(2) . . ? C11 C12 C17 112.7(2) . . ? C13 C12 C17 110.4(2) . . ? C11 C12 H12 108.4 . . ? C13 C12 H12 108.4 . . ? C17 C12 H12 108.4 . . ? C12 C13 C14 110.5(3) . . ? C12 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? C12 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C13 111.7(3) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 107.9 . . ? C14 C15 C16 112.0(3) . . ? C14 C15 H15A 109.2 . . ? C16 C15 H15A 109.2 . . ? C14 C15 H15B 109.2 . . ? C16 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C15 C16 C17 110.9(3) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.4 . . ? C17 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 C17 C12 109.7(2) . . ? C16 C17 H17A 109.7 . . ? C12 C17 H17A 109.7 . . ? C16 C17 H17B 109.7 . . ? C12 C17 H17B 109.7 . . ? H17A C17 H17B 108.2 . . ? O22 C21 O21 125.9(3) . . ? O22 C21 C22 117.9(3) . . ? O21 C21 C22 116.2(3) . . ? C21 C22 C27 111.6(2) . . ? C21 C22 C23 110.7(3) . . ? C27 C22 C23 110.1(3) . . ? C21 C22 H22 108.1 . . ? C27 C22 H22 108.1 . . ? C23 C22 H22 108.1 . . ? C24 C23 C22 110.1(3) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.2 . . ? C25 C24 C23 112.1(3) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C26 C25 C24 111.7(3) . . ? C26 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? C26 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? C25 C26 C27 111.4(3) . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? C27 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C26 C27 C22 110.6(3) . . ? C26 C27 H27A 109.5 . . ? C22 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? O32 C31 O31 126.4(3) . . ? O32 C31 C32 116.3(3) . . ? O31 C31 C32 117.3(3) . . ? C37 C32 C31 113.0(3) . . ? C37 C32 C33 110.3(3) . . ? C31 C32 C33 108.9(2) . . ? C37 C32 H32 108.2 . . ? C31 C32 H32 108.2 . . ? C33 C32 H32 108.2 . . ? C32 C33 C34 109.7(3) . . ? C32 C33 H33A 109.7 . . ? C34 C33 H33A 109.7 . . ? C32 C33 H33B 109.7 . . ? C34 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? C35 C34 C33 111.6(3) . . ? C35 C34 H34A 109.3 . . ? C33 C34 H34A 109.3 . . ? C35 C34 H34B 109.3 . . ? C33 C34 H34B 109.3 . . ? H34A C34 H34B 108.0 . . ? C36 C35 C34 111.2(3) . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C34 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C37 111.6(3) . . ? C35 C36 H36A 109.3 . . ? C37 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C37 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C32 C37 C36 110.8(3) . . ? C32 C37 H37A 109.5 . . ? C36 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 108.1 . . ? O41 C41 O42 127.5(3) . . ? O41 C41 C42 118.0(3) . . ? O42 C41 C42 114.4(3) . . ? C41 C42 C47 113.9(3) . . ? C41 C42 C43 107.5(3) . . ? C47 C42 C43 112.3(3) . . ? C41 C42 H42 107.6 . . ? C47 C42 H42 107.6 . . ? C43 C42 H42 107.6 . . ? C44 C43 C42 111.6(3) . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C45 C44 C43 110.8(3) . . ? C45 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? C45 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? C46 C45 C44 111.0(3) . . ? C46 C45 H45A 109.4 . . ? C44 C45 H45A 109.4 . . ? C46 C45 H45B 109.4 . . ? C44 C45 H45B 109.4 . . ? H45A C45 H45B 108.0 . . ? C45 C46 C47 111.5(3) . . ? C45 C46 H46A 109.3 . . ? C47 C46 H46A 109.3 . . ? C45 C46 H46B 109.3 . . ? C47 C46 H46B 109.3 . . ? H46A C46 H46B 108.0 . . ? C42 C47 C46 111.4(3) . . ? C42 C47 H47A 109.3 . . ? C46 C47 H47A 109.3 . . ? C42 C47 H47B 109.3 . . ? C46 C47 H47B 109.3 . . ? H47A C47 H47B 108.0 . . ? O52 C51 O51 124.9(3) . . ? O52 C51 C52 117.6(3) . . ? O51 C51 C52 117.5(3) . . ? C51 C52 C53 112.7(3) . . ? C51 C52 C57 110.2(2) . . ? C53 C52 C57 110.2(3) . . ? C51 C52 H52 107.9 . . ? C53 C52 H52 107.9 . . ? C57 C52 H52 107.9 . . ? C52 C53 C54 110.3(3) . . ? C52 C53 H53A 109.6 . . ? C54 C53 H53A 109.6 . . ? C52 C53 H53B 109.6 . . ? C54 C53 H53B 109.6 . . ? H53A C53 H53B 108.1 . . ? C55 C54 C53 111.4(3) . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54B 109.3 . . ? C53 C54 H54B 109.3 . . ? H54A C54 H54B 108.0 . . ? C56 C55 C54 111.4(3) . . ? C56 C55 H55A 109.4 . . ? C54 C55 H55A 109.4 . . ? C56 C55 H55B 109.4 . . ? C54 C55 H55B 109.4 . . ? H55A C55 H55B 108.0 . . ? C55 C56 C57 112.1(3) . . ? C55 C56 H56A 109.2 . . ? C57 C56 H56A 109.2 . . ? C55 C56 H56B 109.2 . . ? C57 C56 H56B 109.2 . . ? H56A C56 H56B 107.9 . . ? C56 C57 C52 111.0(3) . . ? C56 C57 H57A 109.4 . . ? C52 C57 H57A 109.4 . . ? C56 C57 H57B 109.4 . . ? C52 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? O62 C61 O61 126.2(3) . . ? O62 C61 C62 117.3(3) . . ? O61 C61 C62 116.4(3) . . ? C61 C62 C63A 115.8(3) . . ? C61 C62 C67 113.3(2) . . ? C63A C62 C67 117.0(4) . . ? C61 C62 C63B 108.0(3) . . ? C67 C62 C63B 103.8(4) . . ? C61 C62 H62B 110.5 . . ? C67 C62 H62B 110.5 . . ? C63B C62 H62B 110.5 . . ? C61 C62 H62A 102.6 . . ? C63A C62 H62A 102.4 . . ? C67 C62 H62A 102.7 . . ? C62 C63A C64A 108.1(5) . . ? C62 C63A H63A 110.1 . . ? C64A C63A H63A 110.1 . . ? C62 C63A H63B 110.1 . . ? C64A C63A H63B 110.1 . . ? H63A C63A H63B 108.4 . . ? C63A C64A C65A 109.9(7) . . ? C63A C64A H64A 109.7 . . ? C65A C64A H64A 109.7 . . ? C63A C64A H64B 109.7 . . ? C65A C64A H64B 109.7 . . ? H64A C64A H64B 108.2 . . ? C66A C65A C64A 99.4(7) . . ? C66A C65A H65A 111.9 . . ? C64A C65A H65A 111.9 . . ? C66A C65A H65B 111.9 . . ? C64A C65A H65B 111.9 . . ? H65A C65A H65B 109.6 . . ? C65A C66A C67 114.6(6) . . ? C65A C66A H66A 108.6 . . ? C67 C66A H66A 108.6 . . ? C65A C66A H66B 108.6 . . ? C67 C66A H66B 108.6 . . ? H66A C66A H66B 107.6 . . ? C64B C63B C62 113.8(5) . . ? C64B C63B H63C 108.8 . . ? C62 C63B H63C 108.8 . . ? C64B C63B H63D 108.8 . . ? C62 C63B H63D 108.8 . . ? H63C C63B H63D 107.7 . . ? C63B C64B C65B 113.3(7) . . ? C63B C64B H64C 108.9 . . ? C65B C64B H64C 108.9 . . ? C63B C64B H64D 108.9 . . ? C65B C64B H64D 108.9 . . ? H64C C64B H64D 107.7 . . ? C66B C65B C64B 120.3(8) . . ? C66B C65B H65C 107.2 . . ? C64B C65B H65C 107.2 . . ? C66B C65B H65D 107.2 . . ? C64B C65B H65D 107.2 . . ? H65C C65B H65D 106.9 . . ? C65B C66B C67 108.1(6) . . ? C65B C66B H66C 110.1 . . ? C67 C66B H66C 110.1 . . ? C65B C66B H66D 110.1 . . ? C67 C66B H66D 110.1 . . ? H66C C66B H66D 108.4 . . ? C62 C67 C66B 109.9(5) . . ? C62 C67 C66A 110.9(4) . . ? C62 C67 H67C 109.7 . . ? C62 C67 H67D 109.7 . . ? H67C C67 H67D 108.2 . . ? C62 C67 H67A 109.4 . . ? C66B C67 H67A 99.5 . . ? C66A C67 H67A 111.3 . . ? C62 C67 H67B 109.0 . . ? H67A C67 H67B 108.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.831 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.097 data_a2 _database_code_depnum_ccdc_archive 'CCDC 894036' #TrackingRef 'web_deposit_cif_file_2_DrAndreiV.Churakov_1354804993.4_10str07.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 N2 O4 Pd2' _chemical_formula_sum 'C20 H22 N2 O4 Pd2' _chemical_formula_weight 567.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' _symmetry_space_group_name_Hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 13.1912(19) _cell_length_b 20.076(3) _cell_length_c 32.596(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8632(2) _cell_formula_units_Z 16 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9965 _cell_measurement_theta_min 2.383 _cell_measurement_theta_max 29.860 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.746 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4480 _exptl_absorpt_coefficient_mu 1.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8490 _exptl_absorpt_correction_T_max 0.9052 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21325 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 28.00 _reflns_number_total 2609 _reflns_number_gt 2337 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2609 _refine_ls_number_parameters 129 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0243 _refine_ls_R_factor_gt 0.0204 _refine_ls_wR_factor_ref 0.0821 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.684356(11) 0.392217(8) 0.087747(5) 0.02352(9) Uani 1 1 d . . . N1 N 0.77220(15) 0.31152(10) 0.09197(6) 0.0285(4) Uani 1 1 d . . . H1 H 0.8265 0.3111 0.1076 0.034 Uiso 1 1 calc R . . O1 O 0.59410(14) 0.47313(8) 0.07525(5) 0.0337(4) Uani 1 1 d . . . O2 O 0.47481(12) 0.45333(8) 0.12229(5) 0.0333(4) Uani 1 1 d . . . C1 C 0.65423(19) 0.26976(12) 0.04647(8) 0.0354(5) Uani 1 1 d . . . C2 C 0.61007(17) 0.33337(11) 0.05009(6) 0.0277(4) Uani 1 1 d . . . C3 C 0.5219(2) 0.34731(14) 0.02804(8) 0.0421(6) Uani 1 1 d . . . H3 H 0.4912 0.3900 0.0300 0.051 Uiso 1 1 calc R . . C4 C 0.4788(2) 0.29852(18) 0.00304(9) 0.0538(8) Uani 1 1 d . . . H4 H 0.4187 0.3084 -0.0118 0.065 Uiso 1 1 calc R . . C5 C 0.5222(2) 0.23596(18) -0.00043(10) 0.0587(8) Uani 1 1 d . . . H5 H 0.4915 0.2030 -0.0173 0.070 Uiso 1 1 calc R . . C6 C 0.6108(2) 0.22164(15) 0.02085(10) 0.0513(7) Uani 1 1 d . . . H6 H 0.6419 0.1792 0.0180 0.062 Uiso 1 1 calc R . . C7 C 0.74627(19) 0.26010(12) 0.07085(7) 0.0335(5) Uani 1 1 d . . . C8 C 0.8052(2) 0.19615(14) 0.07138(11) 0.0500(7) Uani 1 1 d . . . H8A H 0.8671 0.2021 0.0876 0.075 Uiso 1 1 calc R . . H8B H 0.8234 0.1837 0.0432 0.075 Uiso 1 1 calc R . . H8C H 0.7637 0.1609 0.0836 0.075 Uiso 1 1 calc R . . C9 C 0.51039(19) 0.48446(12) 0.09223(7) 0.0316(5) Uani 1 1 d . . . C10 C 0.4506(2) 0.54078(16) 0.07442(10) 0.0528(8) Uani 1 1 d . . . H10A H 0.3790 0.5357 0.0818 0.079 Uiso 1 1 calc R . . H10B H 0.4575 0.5405 0.0445 0.079 Uiso 1 1 calc R . . H10C H 0.4761 0.5831 0.0853 0.079 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 0.02065(13) 0.02619(13) 0.02370(13) -0.00176(5) 0.00279(5) 0.00045(5) N1 0.0253(9) 0.0302(10) 0.0299(9) -0.0013(7) -0.0034(7) 0.0017(8) O1 0.0346(9) 0.0326(8) 0.0339(8) 0.0058(7) 0.0099(7) 0.0083(7) O2 0.0246(8) 0.0370(8) 0.0382(9) 0.0109(7) 0.0067(7) 0.0085(6) C1 0.0356(12) 0.0373(12) 0.0332(12) -0.0078(9) -0.0054(10) -0.0006(10) C2 0.0264(10) 0.0331(11) 0.0237(9) -0.0028(8) -0.0011(8) 0.0001(9) C3 0.0347(13) 0.0537(16) 0.0379(13) -0.0088(11) -0.0054(11) 0.0078(12) C4 0.0407(15) 0.073(2) 0.0481(16) -0.0151(15) -0.0190(13) 0.0063(15) C5 0.0531(18) 0.068(2) 0.0551(17) -0.0234(16) -0.0194(15) -0.0077(16) C6 0.0609(18) 0.0412(14) 0.0518(17) -0.0155(12) -0.0162(14) 0.0011(14) C7 0.0355(12) 0.0294(11) 0.0355(12) -0.0018(9) -0.0038(9) 0.0011(9) C8 0.0558(18) 0.0336(14) 0.0605(18) -0.0060(13) -0.0130(14) 0.0123(12) C9 0.0307(12) 0.0304(11) 0.0338(11) 0.0032(9) 0.0039(9) 0.0070(9) C10 0.0552(18) 0.0521(17) 0.0511(16) 0.0183(14) 0.0098(14) 0.0275(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C2 1.965(2) . ? Pd1 N1 1.997(2) . ? Pd1 O1 2.0548(16) . ? Pd1 O2 2.1535(15) 11_554 ? Pd1 Pd1 2.8895(4) 11_554 ? N1 C7 1.287(3) . ? N1 H1 0.8800 . ? O1 C9 1.256(3) . ? O2 C9 1.253(3) . ? O2 Pd1 2.1534(15) 11_554 ? C1 C6 1.399(3) . ? C1 C2 1.409(3) . ? C1 C7 1.464(3) . ? C2 C3 1.396(3) . ? C3 C4 1.395(4) . ? C3 H3 0.9500 . ? C4 C5 1.385(5) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.501(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.496(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pd1 N1 81.06(8) . . ? C2 Pd1 O1 93.59(8) . . ? N1 Pd1 O1 172.49(7) . . ? C2 Pd1 O2 176.07(8) . 11_554 ? N1 Pd1 O2 95.60(7) . 11_554 ? O1 Pd1 O2 89.53(7) . 11_554 ? C2 Pd1 Pd1 104.75(7) . 11_554 ? N1 Pd1 Pd1 104.87(5) . 11_554 ? O1 Pd1 Pd1 81.52(5) . 11_554 ? O2 Pd1 Pd1 78.06(4) 11_554 11_554 ? C7 N1 Pd1 117.37(16) . . ? C7 N1 H1 121.3 . . ? Pd1 N1 H1 121.3 . . ? C9 O1 Pd1 124.42(15) . . ? C9 O2 Pd1 123.27(15) . 11_554 ? C6 C1 C2 120.4(2) . . ? C6 C1 C7 124.9(2) . . ? C2 C1 C7 114.7(2) . . ? C3 C2 C1 118.9(2) . . ? C3 C2 Pd1 128.07(18) . . ? C1 C2 Pd1 113.03(16) . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 121.1(3) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C6 C5 C4 119.6(3) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C1 120.0(3) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? N1 C7 C1 113.9(2) . . ? N1 C7 C8 122.8(2) . . ? C1 C7 C8 123.3(2) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C9 O1 125.7(2) . . ? O2 C9 C10 118.9(2) . . ? O1 C9 C10 115.4(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.88 2.08 2.931(2) 161.5 12_554 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.494 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.073 data_z2 _database_code_depnum_ccdc_archive 'CCDC 894037' #TrackingRef 'web_deposit_cif_file_3_DrAndreiV.Churakov_1354804993.5_10str12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H60 N4 O16 Pd5' _chemical_formula_sum 'C34 H60 N4 O16 Pd5' _chemical_formula_weight 1312.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 40.832(6) _cell_length_b 40.832(6) _cell_length_c 15.260(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 22034(8) _cell_formula_units_Z 18 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2874 _cell_measurement_theta_min 2.468 _cell_measurement_theta_max 18.204 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.781 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 11700 _exptl_absorpt_coefficient_mu 1.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5868 _exptl_absorpt_correction_T_max 0.9816 _exptl_absorpt_process_details 'SADABS (Bruker, 2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 50001 _diffrn_reflns_av_R_equivalents 0.2306 _diffrn_reflns_av_sigmaI/netI 0.1597 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8859 _reflns_number_gt 4153 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four disordered t-Bu droups were refined with restrained C-C distances (SADI). ; _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^)+(0.0601P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8859 _refine_ls_number_parameters 522 _refine_ls_number_restraints 120 _refine_ls_R_factor_all 0.1610 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1213 _refine_ls_goodness_of_fit_ref 0.857 _refine_ls_restrained_S_all 0.863 _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 Pd1 Pd 0.38076(2) 0.48895(2) 0.64832(6) 0.0458(2) Uani 1 1 d . . . Pd2 Pd 0.36868(2) 0.52106(2) 0.45415(6) 0.0470(3) Uani 1 1 d . . . Pd3 Pd 0.45866(2) 0.50703(2) 0.65238(6) 0.0471(3) Uani 1 1 d . . . Pd4 Pd 0.42973(2) 0.57184(2) 0.33851(6) 0.0470(3) Uani 1 1 d . . . Pd5 Pd 0.46086(2) 0.52589(2) 0.44659(5) 0.0442(2) Uani 1 1 d . . . N1 N 0.3890(3) 0.5285(3) 0.5695(6) 0.051(2) Uani 1 1 d . . . O1 O 0.4109(2) 0.5605(2) 0.5918(5) 0.057(2) Uani 1 1 d . . . N4 N 0.4539(2) 0.4679(3) 0.5671(7) 0.049(2) Uani 1 1 d . . . O3 O 0.4525(2) 0.4741(2) 0.4837(5) 0.053(2) Uani 1 1 d . . . O4 O 0.4503(2) 0.4387(2) 0.5887(5) 0.066(2) Uani 1 1 d . . . C1 C 0.5109(3) 0.6445(3) 0.4122(8) 0.068(4) Uani 1 1 d . . . H1A H 0.4940 0.6437 0.3656 0.102 Uiso 1 1 calc R . . H1B H 0.5367 0.6557 0.3894 0.102 Uiso 1 1 calc R . . H1C H 0.5104 0.6597 0.4611 0.102 Uiso 1 1 calc R . . C2 C 0.4983(3) 0.6060(3) 0.4427(8) 0.048(3) Uani 1 1 d . . . C3 C 0.5100(3) 0.5797(3) 0.5690(8) 0.047(3) Uani 1 1 d . . . C4 C 0.5357(3) 0.5950(3) 0.6442(7) 0.055(3) Uani 1 1 d . . . H4A H 0.5272 0.5759 0.6907 0.083 Uiso 1 1 calc R . . H4B H 0.5357 0.6175 0.6663 0.083 Uiso 1 1 calc R . . H4C H 0.5613 0.6018 0.6260 0.083 Uiso 1 1 calc R . . O2 O 0.52178(19) 0.6070(2) 0.5070(5) 0.0457(18) Uani 1 1 d . . . N2 N 0.4714(3) 0.5765(3) 0.4120(5) 0.046(2) Uani 1 1 d . . . N3 N 0.4823(2) 0.5466(2) 0.5617(5) 0.041(2) Uani 1 1 d . . . O11 O 0.3530(2) 0.4457(2) 0.5659(5) 0.058(2) Uani 1 1 d . . . O12 O 0.3661(2) 0.4717(2) 0.4314(5) 0.052(2) Uani 1 1 d . . . C11 C 0.3546(3) 0.4443(4) 0.4836(9) 0.054(3) Uani 1 1 d . A . C12 C 0.3414(3) 0.4048(3) 0.4439(7) 0.056(3) Uani 1 1 d D . . C13 C 0.3585(8) 0.4078(9) 0.3543(14) 0.070(9) Uiso 0.41 1 d PD A 1 H13A H 0.3861 0.4239 0.3578 0.105 Uiso 0.41 1 calc PR A 1 H13B H 0.3484 0.4189 0.3130 0.105 Uiso 0.41 1 calc PR A 1 H13C H 0.3522 0.3826 0.3340 0.105 Uiso 0.41 1 calc PR A 1 C14 C 0.3001(5) 0.3803(9) 0.445(2) 0.082(10) Uiso 0.41 1 d PD A 1 H14A H 0.2908 0.3764 0.5050 0.124 Uiso 0.41 1 calc PR A 1 H14B H 0.2933 0.3558 0.4182 0.124 Uiso 0.41 1 calc PR A 1 H14C H 0.2884 0.3922 0.4107 0.124 Uiso 0.41 1 calc PR A 1 C15 C 0.3586(8) 0.3863(9) 0.5033(18) 0.087(11) Uiso 0.41 1 d PD A 1 H15A H 0.3861 0.4028 0.5067 0.131 Uiso 0.41 1 calc PR A 1 H15B H 0.3528 0.3618 0.4783 0.131 Uiso 0.41 1 calc PR A 1 H15C H 0.3477 0.3824 0.5622 0.131 Uiso 0.41 1 calc PR A 1 C16 C 0.3175(6) 0.4019(7) 0.3626(13) 0.099(8) Uiso 0.59 1 d PD A 2 H16A H 0.3149 0.3814 0.3247 0.149 Uiso 0.59 1 calc PR A 2 H16B H 0.3300 0.4258 0.3302 0.149 Uiso 0.59 1 calc PR A 2 H16C H 0.2923 0.3967 0.3814 0.149 Uiso 0.59 1 calc PR A 2 C17 C 0.3747(5) 0.4027(7) 0.4176(16) 0.091(8) Uiso 0.59 1 d PD A 2 H17A H 0.3882 0.4019 0.4699 0.136 Uiso 0.59 1 calc PR A 2 H17B H 0.3914 0.4250 0.3824 0.136 Uiso 0.59 1 calc PR A 2 H17C H 0.3668 0.3798 0.3828 0.136 Uiso 0.59 1 calc PR A 2 C18 C 0.3144(6) 0.3726(6) 0.5021(14) 0.096(8) Uiso 0.59 1 d PD A 2 H18A H 0.3278 0.3718 0.5546 0.144 Uiso 0.59 1 calc PR A 2 H18B H 0.3045 0.3487 0.4701 0.144 Uiso 0.59 1 calc PR A 2 H18C H 0.2934 0.3764 0.5192 0.144 Uiso 0.59 1 calc PR A 2 O21 O 0.3739(2) 0.4466(2) 0.7309(5) 0.062(2) Uani 1 1 d . . . O22 O 0.4354(2) 0.4662(2) 0.7459(5) 0.057(2) Uani 1 1 d . . . C21 C 0.4012(4) 0.4453(3) 0.7632(7) 0.053(3) Uani 1 1 d . B . C22 C 0.3927(3) 0.4127(4) 0.8261(9) 0.080(4) Uani 1 1 d D . . C23 C 0.3822(6) 0.3790(6) 0.7651(14) 0.076(8) Uiso 0.55 1 d PD B 3 H23A H 0.3583 0.3720 0.7355 0.114 Uiso 0.55 1 calc PR B 3 H23B H 0.3795 0.3575 0.7995 0.114 Uiso 0.55 1 calc PR B 3 H23C H 0.4022 0.3860 0.7213 0.114 Uiso 0.55 1 calc PR B 3 C24 C 0.3605(6) 0.4044(8) 0.8861(15) 0.086(9) Uiso 0.55 1 d PD B 3 H24A H 0.3390 0.4016 0.8517 0.129 Uiso 0.55 1 calc PR B 3 H24B H 0.3683 0.4253 0.9277 0.129 Uiso 0.55 1 calc PR B 3 H24C H 0.3531 0.3810 0.9183 0.129 Uiso 0.55 1 calc PR B 3 C25 C 0.4284(6) 0.4208(8) 0.8752(18) 0.119(11) Uiso 0.55 1 d PD B 3 H25A H 0.4471 0.4218 0.8336 0.178 Uiso 0.55 1 calc PR B 3 H25B H 0.4223 0.4008 0.9182 0.178 Uiso 0.55 1 calc PR B 3 H25C H 0.4387 0.4452 0.9054 0.178 Uiso 0.55 1 calc PR B 3 C26 C 0.4091(8) 0.3904(8) 0.7941(19) 0.085(10) Uiso 0.45 1 d PD B 4 H26A H 0.4041 0.3857 0.7311 0.127 Uiso 0.45 1 calc PR B 4 H26B H 0.3977 0.3662 0.8253 0.127 Uiso 0.45 1 calc PR B 4 H26C H 0.4365 0.4042 0.8042 0.127 Uiso 0.45 1 calc PR B 4 C27 C 0.4108(7) 0.4320(8) 0.9141(15) 0.082(10) Uiso 0.45 1 d PD B 4 H27A H 0.4064 0.4532 0.9242 0.123 Uiso 0.45 1 calc PR B 4 H27B H 0.4381 0.4415 0.9121 0.123 Uiso 0.45 1 calc PR B 4 H27C H 0.3995 0.4136 0.9618 0.123 Uiso 0.45 1 calc PR B 4 C28 C 0.3502(5) 0.3896(8) 0.841(2) 0.088(11) Uiso 0.45 1 d PD B 4 H28A H 0.3376 0.3761 0.7876 0.132 Uiso 0.45 1 calc PR B 4 H28B H 0.3407 0.4065 0.8581 0.132 Uiso 0.45 1 calc PR B 4 H28C H 0.3449 0.3713 0.8886 0.132 Uiso 0.45 1 calc PR B 4 O31 O 0.4001(2) 0.5256(2) 0.7490(4) 0.050(2) Uani 1 1 d . . . O32 O 0.4623(2) 0.5455(2) 0.7399(5) 0.054(2) Uani 1 1 d . . . C31 C 0.4340(4) 0.5456(3) 0.7720(7) 0.048(3) Uani 1 1 d . . . C32 C 0.4417(3) 0.5756(3) 0.8423(8) 0.059(3) Uani 1 1 d . . . C33 C 0.4120(4) 0.5581(4) 0.9118(10) 0.092(5) Uiso 1 1 d . . . H33A H 0.3869 0.5467 0.8847 0.138 Uiso 1 1 calc R . . H33B H 0.4150 0.5776 0.9535 0.138 Uiso 1 1 calc R . . H33C H 0.4148 0.5386 0.9426 0.138 Uiso 1 1 calc R . . C34 C 0.4386(4) 0.6071(4) 0.7976(9) 0.086(4) Uiso 1 1 d . . . H34A H 0.4149 0.5964 0.7644 0.129 Uiso 1 1 calc R . . H34B H 0.4600 0.6208 0.7576 0.129 Uiso 1 1 calc R . . H34C H 0.4389 0.6246 0.8420 0.129 Uiso 1 1 calc R . . C35 C 0.4814(3) 0.5918(3) 0.8789(8) 0.069(4) Uiso 1 1 d . . . H35A H 0.4851 0.6094 0.9266 0.104 Uiso 1 1 calc R . . H35B H 0.4999 0.6053 0.8324 0.104 Uiso 1 1 calc R . . H35C H 0.4848 0.5713 0.9014 0.104 Uiso 1 1 calc R . . O41 O 0.3424(2) 0.5118(2) 0.3351(6) 0.074(3) Uani 1 1 d . . . O42 O 0.3852(2) 0.5643(2) 0.2652(5) 0.050(2) Uani 1 1 d . . . C41 C 0.3532(4) 0.5351(4) 0.2728(8) 0.056(3) Uani 1 1 d . . . C42 C 0.3244(4) 0.5276(4) 0.2008(8) 0.071(4) Uani 1 1 d . . . C43 C 0.2954(5) 0.4891(5) 0.1991(11) 0.118(6) Uiso 1 1 d . . . H43A H 0.3063 0.4731 0.1863 0.177 Uiso 1 1 calc R . . H43B H 0.2769 0.4856 0.1536 0.177 Uiso 1 1 calc R . . H43C H 0.2827 0.4822 0.2562 0.177 Uiso 1 1 calc R . . C44 C 0.3101(5) 0.5551(5) 0.2201(12) 0.142(7) Uiso 1 1 d . . . H44A H 0.2879 0.5487 0.1834 0.214 Uiso 1 1 calc R . . H44B H 0.3301 0.5810 0.2072 0.214 Uiso 1 1 calc R . . H44C H 0.3030 0.5532 0.2821 0.214 Uiso 1 1 calc R . . C45 C 0.3428(4) 0.5382(4) 0.1140(9) 0.084(4) Uiso 1 1 d . . . H45A H 0.3558 0.5239 0.1024 0.126 Uiso 1 1 calc R . . H45B H 0.3613 0.5653 0.1131 0.126 Uiso 1 1 calc R . . H45C H 0.3237 0.5324 0.0687 0.126 Uiso 1 1 calc R . . O51 O 0.3659(2) 0.5685(2) 0.4670(5) 0.058(2) Uani 1 1 d . . . O52 O 0.4242(2) 0.6082(2) 0.4154(5) 0.0483(19) Uani 1 1 d . . . C51 C 0.3941(4) 0.6006(4) 0.4557(7) 0.052(3) Uani 1 1 d . C . C52 C 0.3931(4) 0.6353(4) 0.4916(9) 0.086(5) Uani 1 1 d D . . C53 C 0.4053(7) 0.6663(7) 0.4261(14) 0.103(9) Uiso 0.59 1 d PD C 7 H53A H 0.3904 0.6563 0.3724 0.154 Uiso 0.59 1 calc PR C 7 H53B H 0.4322 0.6767 0.4127 0.154 Uiso 0.59 1 calc PR C 7 H53C H 0.4014 0.6863 0.4501 0.154 Uiso 0.59 1 calc PR C 7 C54 C 0.4257(5) 0.6524(6) 0.5648(14) 0.076(7) Uiso 0.59 1 d PD C 7 H54A H 0.4198 0.6335 0.6108 0.114 Uiso 0.59 1 calc PR C 7 H54B H 0.4271 0.6751 0.5905 0.114 Uiso 0.59 1 calc PR C 7 H54C H 0.4500 0.6590 0.5378 0.114 Uiso 0.59 1 calc PR C 7 C55 C 0.3567(6) 0.6264(8) 0.5370(16) 0.102(11) Uiso 0.59 1 d PD C 7 H55A H 0.3362 0.6171 0.4939 0.153 Uiso 0.59 1 calc PR C 7 H55B H 0.3596 0.6493 0.5650 0.153 Uiso 0.59 1 calc PR C 7 H55C H 0.3506 0.6069 0.5817 0.153 Uiso 0.59 1 calc PR C 7 C56 C 0.3740(8) 0.6417(9) 0.4091(15) 0.079(10) Uiso 0.41 1 d PD C 8 H56A H 0.3478 0.6210 0.4043 0.118 Uiso 0.41 1 calc PR C 8 H56B H 0.3880 0.6424 0.3563 0.118 Uiso 0.41 1 calc PR C 8 H56C H 0.3743 0.6658 0.4151 0.118 Uiso 0.41 1 calc PR C 8 C57 C 0.4296(8) 0.6691(10) 0.510(3) 0.16(2) Uiso 0.41 1 d PD C 8 H57A H 0.4429 0.6797 0.4542 0.236 Uiso 0.41 1 calc PR C 8 H57B H 0.4448 0.6624 0.5468 0.236 Uiso 0.41 1 calc PR C 8 H57C H 0.4254 0.6880 0.5395 0.236 Uiso 0.41 1 calc PR C 8 C58 C 0.3644(7) 0.6217(8) 0.5648(15) 0.049(8) Uiso 0.41 1 d PD C 8 H58A H 0.3394 0.6037 0.5415 0.073 Uiso 0.41 1 calc PR C 8 H58B H 0.3637 0.6433 0.5907 0.073 Uiso 0.41 1 calc PR C 8 H58C H 0.3715 0.6093 0.6098 0.073 Uiso 0.41 1 calc PR C 8 O71 O 0.4380(2) 0.5430(2) 0.2457(5) 0.055(2) Uani 1 1 d . . . O72 O 0.4458(2) 0.5014(2) 0.3264(5) 0.055(2) Uani 1 1 d . . . C71 C 0.4422(3) 0.5148(4) 0.2549(8) 0.058(3) Uani 1 1 d . D . C72 C 0.4418(3) 0.4943(3) 0.1690(8) 0.061(3) Uani 1 1 d D . . C73 C 0.4494(7) 0.4626(6) 0.1798(18) 0.074(9) Uiso 0.50 1 d PD D 5 H73A H 0.4291 0.4424 0.2144 0.111 Uiso 0.50 1 calc PR D 5 H73B H 0.4736 0.4717 0.2102 0.111 Uiso 0.50 1 calc PR D 5 H73C H 0.4506 0.4527 0.1221 0.111 Uiso 0.50 1 calc PR D 5 C74 C 0.4707(7) 0.5239(7) 0.1068(19) 0.104(12) Uiso 0.50 1 d PD D 5 H74A H 0.4960 0.5351 0.1329 0.157 Uiso 0.50 1 calc PR D 5 H74B H 0.4643 0.5438 0.0966 0.157 Uiso 0.50 1 calc PR D 5 H74C H 0.4704 0.5119 0.0509 0.157 Uiso 0.50 1 calc PR D 5 C75 C 0.4030(6) 0.4795(8) 0.1269(19) 0.095(10) Uiso 0.50 1 d PD D 5 H75A H 0.3836 0.4602 0.1648 0.143 Uiso 0.50 1 calc PR D 5 H75B H 0.4026 0.4683 0.0698 0.143 Uiso 0.50 1 calc PR D 5 H75C H 0.3980 0.5004 0.1189 0.143 Uiso 0.50 1 calc PR D 5 C76 C 0.4022(5) 0.4609(7) 0.161(2) 0.102(11) Uiso 0.50 1 d PD D 6 H76A H 0.3969 0.4439 0.2110 0.153 Uiso 0.50 1 calc PR D 6 H76B H 0.4001 0.4472 0.1065 0.153 Uiso 0.50 1 calc PR D 6 H76C H 0.3839 0.4698 0.1599 0.153 Uiso 0.50 1 calc PR D 6 C77 C 0.4691(6) 0.4798(7) 0.1767(16) 0.060(7) Uiso 0.50 1 d PD D 6 H77A H 0.4612 0.4614 0.2247 0.089 Uiso 0.50 1 calc PR D 6 H77B H 0.4945 0.5010 0.1887 0.089 Uiso 0.50 1 calc PR D 6 H77C H 0.4694 0.4675 0.1217 0.089 Uiso 0.50 1 calc PR D 6 C78 C 0.4508(7) 0.5193(6) 0.0910(14) 0.062(7) Uiso 0.50 1 d PD D 6 H78A H 0.4320 0.5274 0.0853 0.093 Uiso 0.50 1 calc PR D 6 H78B H 0.4505 0.5054 0.0383 0.093 Uiso 0.50 1 calc PR D 6 H78C H 0.4760 0.5415 0.0981 0.093 Uiso 0.50 1 calc PR D 6 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 0.0490(6) 0.0457(5) 0.0375(5) 0.0006(4) -0.0044(4) 0.0198(5) Pd2 0.0439(5) 0.0516(6) 0.0392(5) 0.0046(4) -0.0051(4) 0.0191(5) Pd3 0.0517(6) 0.0506(6) 0.0418(6) -0.0012(4) -0.0019(4) 0.0277(5) Pd4 0.0451(6) 0.0524(6) 0.0423(5) 0.0059(4) -0.0004(4) 0.0233(5) Pd5 0.0449(5) 0.0472(5) 0.0397(5) -0.0021(4) -0.0030(4) 0.0225(5) N1 0.051(6) 0.047(6) 0.047(6) -0.003(5) -0.016(5) 0.019(5) O1 0.065(6) 0.048(5) 0.051(5) -0.001(4) -0.010(4) 0.023(5) N4 0.048(6) 0.048(6) 0.056(7) 0.001(5) 0.000(5) 0.028(5) O3 0.069(5) 0.057(5) 0.041(5) -0.002(4) -0.011(4) 0.038(4) O4 0.092(7) 0.059(6) 0.062(6) 0.011(5) 0.010(5) 0.050(5) C1 0.067(9) 0.061(9) 0.078(10) 0.003(7) -0.014(7) 0.034(7) C2 0.049(8) 0.042(7) 0.054(8) -0.006(6) -0.001(6) 0.025(6) C3 0.042(7) 0.052(8) 0.052(8) -0.014(6) -0.010(6) 0.026(6) C4 0.048(7) 0.046(7) 0.064(9) -0.016(6) -0.007(6) 0.018(6) O2 0.048(5) 0.047(5) 0.037(5) 0.001(4) -0.003(4) 0.020(4) N2 0.056(6) 0.054(6) 0.038(6) 0.000(5) 0.002(5) 0.035(6) N3 0.055(6) 0.041(6) 0.031(5) -0.008(4) -0.009(4) 0.027(5) O11 0.076(6) 0.051(5) 0.038(5) 0.000(4) 0.003(4) 0.026(4) O12 0.064(5) 0.046(5) 0.040(5) 0.003(4) -0.002(4) 0.023(4) C11 0.051(8) 0.066(9) 0.053(9) -0.005(7) -0.001(6) 0.035(7) C12 0.066(8) 0.042(7) 0.057(8) -0.008(6) -0.004(6) 0.024(6) O21 0.061(6) 0.050(5) 0.056(6) 0.006(4) -0.021(4) 0.013(4) O22 0.079(6) 0.057(5) 0.038(5) 0.009(4) 0.012(4) 0.035(5) C21 0.063(9) 0.041(7) 0.035(7) 0.004(6) 0.004(7) 0.010(7) C22 0.079(10) 0.061(9) 0.087(11) 0.003(8) -0.028(8) 0.027(8) O31 0.040(5) 0.066(5) 0.042(5) -0.003(4) -0.008(4) 0.024(4) O32 0.051(5) 0.052(5) 0.055(5) 0.001(4) -0.003(4) 0.022(4) C31 0.053(8) 0.051(8) 0.041(7) 0.006(6) 0.003(6) 0.028(7) C32 0.056(8) 0.074(9) 0.044(8) -0.011(7) -0.018(6) 0.032(7) O41 0.063(6) 0.077(6) 0.061(6) 0.016(5) -0.022(5) 0.020(5) O42 0.037(5) 0.068(5) 0.042(5) 0.011(4) 0.002(4) 0.023(4) C41 0.055(9) 0.057(8) 0.050(8) 0.004(7) -0.009(7) 0.024(7) C42 0.067(9) 0.069(9) 0.048(8) 0.006(7) -0.007(7) 0.013(8) O51 0.042(5) 0.055(5) 0.076(6) 0.021(4) 0.014(4) 0.024(4) O52 0.048(5) 0.051(5) 0.051(5) 0.002(4) -0.006(4) 0.028(4) C51 0.056(9) 0.068(9) 0.046(8) 0.013(7) 0.007(6) 0.041(8) C52 0.092(11) 0.068(10) 0.110(13) 0.023(9) 0.024(9) 0.049(9) O71 0.061(5) 0.061(6) 0.046(5) -0.003(4) -0.011(4) 0.033(5) O72 0.073(6) 0.064(5) 0.032(5) -0.005(4) -0.007(4) 0.036(5) C71 0.045(8) 0.069(9) 0.044(8) 0.000(7) -0.002(6) 0.017(7) C72 0.075(9) 0.059(8) 0.055(8) 0.001(7) -0.004(7) 0.037(7) _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 1.906(9) . ? Pd1 O11 1.996(8) . ? Pd1 O31 2.011(7) . ? Pd1 O21 2.043(8) . ? Pd1 Pd3 2.8841(13) . ? Pd2 N1 1.904(9) . ? Pd2 O12 1.996(7) . ? Pd2 O51 2.004(8) . ? Pd2 O41 2.047(8) . ? Pd2 Pd4 2.9082(13) . ? Pd3 N3 1.973(9) . ? Pd3 N4 1.993(9) . ? Pd3 O32 2.011(8) . ? Pd3 O22 2.032(7) . ? Pd3 Pd5 3.2240(15) . ? Pd4 N2 1.964(9) . ? Pd4 O71 1.976(8) . ? Pd4 O52 1.994(7) . ? Pd4 O42 2.021(7) . ? Pd4 Pd5 3.2003(13) . ? Pd5 N3 1.955(8) . ? Pd5 N2 1.963(9) . ? Pd5 O72 2.032(7) . ? Pd5 O3 2.044(7) . ? N1 O1 1.205(10) . ? N4 O4 1.175(10) . ? N4 O3 1.306(11) . ? C1 C2 1.464(15) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N2 1.246(13) . ? C2 O2 1.357(13) . ? C3 N3 1.261(13) . ? C3 O2 1.352(13) . ? C3 C4 1.469(14) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O11 C11 1.261(13) . ? O12 C11 1.257(13) . ? C11 C12 1.543(15) . ? C12 C17 1.462(17) . ? C12 C14 1.470(18) . ? C12 C18 1.512(17) . ? C12 C13 1.513(18) . ? C12 C16 1.547(17) . ? C12 C15 1.556(19) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O21 C21 1.245(14) . ? O22 C21 1.248(13) . ? C21 C22 1.533(17) . ? C22 C26 1.457(18) . ? C22 C24 1.497(17) . ? C22 C25 1.520(18) . ? C22 C28 1.524(18) . ? C22 C23 1.533(17) . ? C22 C27 1.546(18) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O31 C31 1.254(13) . ? O32 C31 1.258(12) . ? C31 C32 1.535(15) . ? C32 C33 1.495(17) . ? C32 C35 1.517(15) . ? C32 C34 1.519(16) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? O41 C41 1.259(13) . ? O42 C41 1.259(13) . ? C41 C42 1.524(16) . ? C42 C43 1.417(18) . ? C42 C45 1.478(17) . ? C42 C44 1.54(2) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? O51 C51 1.253(13) . ? O52 C51 1.264(12) . ? C51 C52 1.539(17) . ? C52 C57 1.46(2) . ? C52 C53 1.490(17) . ? C52 C58 1.510(18) . ? C52 C55 1.511(18) . ? C52 C56 1.571(19) . ? C52 C54 1.604(17) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? O71 C71 1.254(14) . ? O72 C71 1.262(13) . ? C71 C72 1.551(17) . ? C72 C73 1.484(17) . ? C72 C78 1.489(17) . ? C72 C77 1.507(17) . ? C72 C76 1.511(18) . ? C72 C75 1.524(18) . ? C72 C74 1.528(18) . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? 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 O11 97.7(4) . . ? N1 Pd1 O31 90.8(3) . . ? O11 Pd1 O31 168.0(3) . . ? N1 Pd1 O21 177.6(4) . . ? O11 Pd1 O21 82.1(3) . . ? O31 Pd1 O21 89.7(3) . . ? N1 Pd1 Pd3 95.3(3) . . ? O11 Pd1 Pd3 107.8(2) . . ? O31 Pd1 Pd3 79.7(2) . . ? O21 Pd1 Pd3 82.5(2) . . ? N1 Pd2 O12 97.0(3) . . ? N1 Pd2 O51 89.2(4) . . ? O12 Pd2 O51 173.0(3) . . ? N1 Pd2 O41 175.0(4) . . ? O12 Pd2 O41 84.3(3) . . ? O51 Pd2 O41 89.3(3) . . ? N1 Pd2 Pd4 107.3(3) . . ? O12 Pd2 Pd4 102.0(2) . . ? O51 Pd2 Pd4 79.2(2) . . ? O41 Pd2 Pd4 77.1(2) . . ? N3 Pd3 N4 90.5(4) . . ? N3 Pd3 O32 90.7(3) . . ? N4 Pd3 O32 178.6(4) . . ? N3 Pd3 O22 178.7(3) . . ? N4 Pd3 O22 89.0(4) . . ? O32 Pd3 O22 89.8(3) . . ? N3 Pd3 Pd1 102.7(2) . . ? N4 Pd3 Pd1 97.4(3) . . ? O32 Pd3 Pd1 81.7(2) . . ? O22 Pd3 Pd1 78.6(2) . . ? N3 Pd3 Pd5 34.7(2) . . ? N4 Pd3 Pd5 62.3(3) . . ? O32 Pd3 Pd5 118.5(2) . . ? O22 Pd3 Pd5 145.6(2) . . ? Pd1 Pd3 Pd5 86.31(3) . . ? N2 Pd4 O71 94.0(3) . . ? N2 Pd4 O52 90.4(3) . . ? O71 Pd4 O52 169.5(3) . . ? N2 Pd4 O42 177.1(4) . . ? O71 Pd4 O42 85.5(3) . . ? O52 Pd4 O42 90.6(3) . . ? N2 Pd4 Pd2 96.6(3) . . ? O71 Pd4 Pd2 110.6(2) . . ? O52 Pd4 Pd2 78.3(2) . . ? O42 Pd4 Pd2 80.9(2) . . ? N2 Pd4 Pd5 35.4(3) . . ? O71 Pd4 Pd5 77.5(2) . . ? O52 Pd4 Pd5 111.1(2) . . ? O42 Pd4 Pd5 141.8(2) . . ? Pd2 Pd4 Pd5 73.71(3) . . ? N3 Pd5 N2 88.4(4) . . ? N3 Pd5 O72 169.5(3) . . ? N2 Pd5 O72 97.4(3) . . ? N3 Pd5 O3 90.3(3) . . ? N2 Pd5 O3 177.4(3) . . ? O72 Pd5 O3 83.5(3) . . ? N3 Pd5 Pd4 115.7(2) . . ? N2 Pd5 Pd4 35.4(3) . . ? O72 Pd5 Pd4 73.3(2) . . ? O3 Pd5 Pd4 147.0(2) . . ? N3 Pd5 Pd3 35.0(3) . . ? N2 Pd5 Pd3 118.6(3) . . ? O72 Pd5 Pd3 142.8(2) . . ? O3 Pd5 Pd3 60.9(2) . . ? Pd4 Pd5 Pd3 132.08(4) . . ? O1 N1 Pd2 117.6(7) . . ? O1 N1 Pd1 117.4(7) . . ? Pd2 N1 Pd1 124.7(5) . . ? O4 N4 O3 118.5(9) . . ? O4 N4 Pd3 122.9(8) . . ? O3 N4 Pd3 118.5(7) . . ? N4 O3 Pd5 118.1(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 O2 124.8(10) . . ? N2 C2 C1 125.6(11) . . ? O2 C2 C1 109.5(10) . . ? N3 C3 O2 125.5(10) . . ? N3 C3 C4 126.3(11) . . ? O2 C3 C4 108.2(10) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 O2 C2 121.7(9) . . ? C2 N2 Pd5 122.5(8) . . ? C2 N2 Pd4 127.8(8) . . ? Pd5 N2 Pd4 109.2(5) . . ? C3 N3 Pd5 120.6(8) . . ? C3 N3 Pd3 128.7(8) . . ? Pd5 N3 Pd3 110.3(4) . . ? C11 O11 Pd1 130.4(8) . . ? C11 O12 Pd2 126.7(8) . . ? O12 C11 O11 126.5(11) . . ? O12 C11 C12 117.4(11) . . ? O11 C11 C12 116.1(11) . . ? C17 C12 C18 113.9(13) . . ? C14 C12 C13 112.8(14) . . ? C17 C12 C11 108.7(13) . . ? C14 C12 C11 113.1(15) . . ? C18 C12 C11 113.6(13) . . ? C13 C12 C11 111.4(14) . . ? C17 C12 C16 110.2(12) . . ? C18 C12 C16 104.2(12) . . ? C11 C12 C16 105.8(12) . . ? C14 C12 C15 107.9(14) . . ? C13 C12 C15 105.2(13) . . ? C11 C12 C15 105.8(15) . . ? C16 C12 C15 148.3(18) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 O21 Pd1 122.2(7) . . ? C21 O22 Pd3 127.9(8) . . ? O21 C21 O22 127.4(11) . . ? O21 C21 C22 117.7(11) . . ? O22 C21 C22 114.6(12) . . ? C26 C22 C24 133.7(19) . . ? C26 C22 C25 67.2(13) . . ? C24 C22 C25 112.7(14) . . ? C26 C22 C28 113.7(15) . . ? C24 C22 C23 110.4(13) . . ? C25 C22 C23 107.7(13) . . ? C26 C22 C21 111.0(16) . . ? C24 C22 C21 111.7(14) . . ? C25 C22 C21 110.0(15) . . ? C28 C22 C21 109.1(16) . . ? C23 C22 C21 103.9(13) . . ? C26 C22 C27 111.0(14) . . ? C28 C22 C27 106.8(14) . . ? C21 C22 C27 104.9(14) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? C22 C28 H28A 109.5 . . ? C22 C28 H28B 109.5 . . ? C22 C28 H28C 109.5 . . ? C31 O31 Pd1 126.5(7) . . ? C31 O32 Pd3 123.6(7) . . ? O31 C31 O32 127.2(11) . . ? O31 C31 C32 115.8(10) . . ? O32 C31 C32 116.9(11) . . ? C33 C32 C35 112.4(11) . . ? C33 C32 C34 109.4(11) . . ? C35 C32 C34 108.6(10) . . ? C33 C32 C31 108.7(11) . . ? C35 C32 C31 110.8(10) . . ? C34 C32 C31 106.9(10) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C41 O41 Pd2 125.2(8) . . ? C41 O42 Pd4 121.5(7) . . ? O42 C41 O41 126.2(11) . . ? O42 C41 C42 117.1(11) . . ? O41 C41 C42 116.6(11) . . ? C43 C42 C45 109.2(12) . . ? C43 C42 C41 111.8(12) . . ? C45 C42 C41 111.1(11) . . ? C43 C42 C44 113.6(14) . . ? C45 C42 C44 106.4(12) . . ? C41 C42 C44 104.6(12) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C51 O51 Pd2 122.1(7) . . ? C51 O52 Pd4 124.1(8) . . ? O51 C51 O52 126.6(11) . . ? O51 C51 C52 118.8(11) . . ? O52 C51 C52 114.6(11) . . ? C57 C52 C58 116.5(17) . . ? C53 C52 C55 112.6(14) . . ? C53 C52 C51 113.0(14) . . ? C58 C52 C51 107.4(14) . . ? C55 C52 C51 114.7(15) . . ? C57 C52 C56 110.3(16) . . ? C58 C52 C56 107.2(14) . . ? C53 C52 C54 104.2(13) . . ? C55 C52 C54 106.7(13) . . ? C51 C52 C54 104.5(12) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? C52 C56 H56A 109.5 . . ? C52 C56 H56B 109.5 . . ? C52 C56 H56C 109.5 . . ? C52 C57 H57A 109.5 . . ? C52 C57 H57B 109.5 . . ? C52 C57 H57C 109.5 . . ? C52 C58 H58A 109.5 . . ? C52 C58 H58B 109.5 . . ? C52 C58 H58C 109.5 . . ? C71 O71 Pd4 127.6(8) . . ? C71 O72 Pd5 129.7(8) . . ? O71 C71 O72 126.5(12) . . ? O71 C71 C72 115.6(11) . . ? O72 C71 C72 117.9(12) . . ? C78 C72 C77 110.6(13) . . ? C78 C72 C76 110.0(14) . . ? C77 C72 C76 108.6(13) . . ? C73 C72 C75 109.3(14) . . ? C73 C72 C74 110.1(14) . . ? C75 C72 C74 106.9(14) . . ? C73 C72 C71 115.2(14) . . ? C78 C72 C71 111.9(13) . . ? C77 C72 C71 109.5(13) . . ? C76 C72 C71 106.0(15) . . ? C75 C72 C71 107.5(15) . . ? C74 C72 C71 107.5(15) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? C72 C75 H75A 109.5 . . ? C72 C75 H75B 109.5 . . ? C72 C75 H75C 109.5 . . ? C72 C76 H76A 109.5 . . ? C72 C76 H76B 109.5 . . ? C72 C76 H76C 109.5 . . ? C72 C77 H77A 109.5 . . ? C72 C77 H77B 109.5 . . ? C72 C77 H77C 109.5 . . ? C72 C78 H78A 109.5 . . ? C72 C78 H78B 109.5 . . ? C72 C78 H78C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.308 _refine_diff_density_min -0.845 _refine_diff_density_rms 0.152 data_z3 _database_code_depnum_ccdc_archive 'CCDC 894038' #TrackingRef 'web_deposit_cif_file_4_DrAndreiV.Churakov_1354804993.6_10str02.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H82 N3 O16 Pd5' _chemical_formula_sum 'C53 H82 N3 O16 Pd5' _chemical_formula_weight 1549.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 43.61(4) _cell_length_b 9.370(9) _cell_length_c 30.03(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.504(16) _cell_angle_gamma 90.00 _cell_volume 12166(20) _cell_formula_units_Z 8 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 7372 _cell_measurement_theta_min 2.469 _cell_measurement_theta_max 26.299 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.692 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6232 _exptl_absorpt_coefficient_mu 1.515 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5967 _exptl_absorpt_correction_T_max 0.9850 _exptl_absorpt_process_details 'SADABS (Bruker, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX II' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41209 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -52 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.50 _reflns_number_total 11257 _reflns_number_gt 8541 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 (Bruker, 2008)' _computing_cell_refinement 'SAINT (Bruker, 2008)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Disordered cyclohexyl ring C32 > C37 was refined with restrained C-C distances. Two cyclohexyl rings (namely C32 > C37 and C62 > C67) were refined with restrained anisotropic displacement parameters due to high thermal motion. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11257 _refine_ls_number_parameters 720 _refine_ls_number_restraints 129 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.957 _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 Pd1 Pd 0.178985(11) 0.27861(5) 0.599239(15) 0.03249(14) Uani 1 1 d . . . Pd2 Pd 0.129686(11) 0.27821(5) 0.498852(15) 0.03346(14) Uani 1 1 d . . . Pd3 Pd 0.181423(12) 0.02046(5) 0.654240(16) 0.03672(14) Uani 1 1 d . . . Pd4 Pd 0.093716(11) 0.02134(5) 0.477751(16) 0.03606(14) Uani 1 1 d . . . Pd5 Pd 0.114508(12) 0.00063(5) 0.588149(17) 0.03624(14) Uani 1 1 d . . . N1 N 0.16408(12) 0.2034(5) 0.53983(16) 0.0333(11) Uani 1 1 d . . . O1 O 0.17625(10) 0.0979(5) 0.52799(14) 0.0407(10) Uani 1 1 d . . . C1 C 0.11905(16) -0.3103(7) 0.4836(2) 0.0440(16) Uani 1 1 d . . . H1A H 0.1083 -0.2539 0.4588 0.066 Uiso 1 1 calc R . . H1B H 0.1062 -0.3920 0.4897 0.066 Uiso 1 1 calc R . . H1C H 0.1388 -0.3446 0.4752 0.066 Uiso 1 1 calc R . . C2 C 0.12508(14) -0.2189(7) 0.5249(2) 0.0354(14) Uani 1 1 d . . . C3 C 0.16121(16) -0.2188(7) 0.5949(2) 0.0392(15) Uani 1 1 d . . . C4 C 0.18800(18) -0.3089(8) 0.6144(3) 0.054(2) Uani 1 1 d . . . H4A H 0.1976 -0.2665 0.6427 0.081 Uiso 1 1 calc R . . H4B H 0.2032 -0.3139 0.5932 0.081 Uiso 1 1 calc R . . H4C H 0.1807 -0.4053 0.6201 0.081 Uiso 1 1 calc R . . N2 N 0.11331(11) -0.0947(5) 0.52995(16) 0.0322(11) Uani 1 1 d . . . N3 N 0.15392(12) -0.0972(6) 0.60969(17) 0.0366(12) Uani 1 1 d . . . O2 O 0.14407(10) -0.2879(4) 0.55885(14) 0.0380(10) Uani 1 1 d . . . O11 O 0.13980(11) 0.3745(5) 0.61119(14) 0.0444(11) Uani 1 1 d . . . O12 O 0.10726(10) 0.3746(5) 0.54505(14) 0.0443(11) Uani 1 1 d . . . C11 C 0.11411(16) 0.4001(7) 0.5868(2) 0.0418(16) Uani 1 1 d . . . C12 C 0.08885(16) 0.4721(7) 0.6106(2) 0.0435(16) Uani 1 1 d . . . H12A H 0.0744 0.3959 0.6184 0.052 Uiso 1 1 calc R . . C13 C 0.1028(2) 0.5459(11) 0.6549(3) 0.076(3) Uani 1 1 d . . . H13A H 0.1143 0.4751 0.6752 0.091 Uiso 1 1 calc R . . H13B H 0.1175 0.6213 0.6484 0.091 Uiso 1 1 calc R . . C14 C 0.0766(2) 0.6116(13) 0.6778(3) 0.089(3) Uani 1 1 d . . . H14A H 0.0628 0.5350 0.6862 0.107 Uiso 1 1 calc R . . H14B H 0.0855 0.6613 0.7056 0.107 Uiso 1 1 calc R . . C15 C 0.0580(2) 0.7177(10) 0.6463(3) 0.077(3) Uani 1 1 d . . . H15A H 0.0409 0.7569 0.6613 0.092 Uiso 1 1 calc R . . H15B H 0.0715 0.7981 0.6399 0.092 Uiso 1 1 calc R . . C16 C 0.0447(2) 0.6478(10) 0.6025(3) 0.070(2) Uani 1 1 d . . . H16A H 0.0336 0.7204 0.5825 0.083 Uiso 1 1 calc R . . H16B H 0.0296 0.5740 0.6086 0.083 Uiso 1 1 calc R . . C17 C 0.06982(17) 0.5795(8) 0.5789(3) 0.0526(19) Uani 1 1 d . . . H17A H 0.0837 0.6545 0.5697 0.063 Uiso 1 1 calc R . . H17B H 0.0602 0.5293 0.5516 0.063 Uiso 1 1 calc R . . O21 O 0.19610(10) 0.3589(5) 0.66227(14) 0.0402(10) Uani 1 1 d . . . O22 O 0.20785(10) 0.1509(5) 0.69877(14) 0.0403(10) Uani 1 1 d . . . C21 C 0.20730(15) 0.2860(7) 0.6963(2) 0.0391(15) Uani 1 1 d . . . C22 C 0.22268(16) 0.3692(7) 0.7380(2) 0.0413(15) Uani 1 1 d . . . H22A H 0.2455 0.3529 0.7402 0.050 Uiso 1 1 calc R . . C23 C 0.2119(2) 0.3089(9) 0.7816(2) 0.061(2) Uani 1 1 d . . . H23A H 0.2140 0.2037 0.7819 0.073 Uiso 1 1 calc R . . H23B H 0.2253 0.3472 0.8080 0.073 Uiso 1 1 calc R . . C24 C 0.1795(2) 0.3477(11) 0.7844(3) 0.087(3) Uani 1 1 d . . . H24A H 0.1736 0.3112 0.8131 0.104 Uiso 1 1 calc R . . H24B H 0.1660 0.3010 0.7596 0.104 Uiso 1 1 calc R . . C25 C 0.1739(3) 0.5088(11) 0.7820(4) 0.090(3) Uani 1 1 d . . . H25A H 0.1857 0.5555 0.8085 0.108 Uiso 1 1 calc R . . H25B H 0.1517 0.5288 0.7825 0.108 Uiso 1 1 calc R . . C26 C 0.1842(2) 0.5700(10) 0.7387(3) 0.069(2) Uani 1 1 d . . . H26A H 0.1704 0.5334 0.7123 0.083 Uiso 1 1 calc R . . H26B H 0.1823 0.6753 0.7389 0.083 Uiso 1 1 calc R . . C27 C 0.21733(18) 0.5287(7) 0.7346(3) 0.0507(18) Uani 1 1 d . . . H27A H 0.2227 0.5627 0.7053 0.061 Uiso 1 1 calc R . . H27B H 0.2313 0.5769 0.7586 0.061 Uiso 1 1 calc R . . O31 O 0.22223(10) 0.2094(5) 0.59157(15) 0.0444(11) Uani 1 1 d . A . O32 O 0.21766(12) -0.0132(5) 0.61898(17) 0.0488(12) Uani 1 1 d . A . C31 C 0.23107(15) 0.0826(10) 0.5981(2) 0.0471(18) Uani 1 1 d U . . C32A C 0.2599(2) 0.0548(10) 0.5754(3) 0.0346(18) Uani 0.71 1 d PDU A 1 H32A H 0.2755 0.1292 0.5864 0.042 Uiso 0.71 1 calc PR A 1 C33A C 0.2743(3) -0.0892(13) 0.5876(4) 0.076(4) Uani 0.71 1 d PDU A 1 H33A H 0.2589 -0.1651 0.5792 0.092 Uiso 0.71 1 calc PR A 1 H33B H 0.2804 -0.0940 0.6205 0.092 Uiso 0.71 1 calc PR A 1 C34A C 0.3028(3) -0.1156(19) 0.5637(3) 0.089(5) Uani 0.71 1 d PDU A 1 H34A H 0.3189 -0.0440 0.5739 0.107 Uiso 0.71 1 calc PR A 1 H34B H 0.3113 -0.2114 0.5719 0.107 Uiso 0.71 1 calc PR A 1 C35A C 0.2945(3) -0.1061(14) 0.5130(3) 0.067(3) Uani 0.71 1 d PDU A 1 H35A H 0.3132 -0.1229 0.4982 0.081 Uiso 0.71 1 calc PR A 1 H35B H 0.2789 -0.1795 0.5025 0.081 Uiso 0.71 1 calc PR A 1 C36A C 0.2816(3) 0.0419(14) 0.5013(4) 0.080(4) Uani 0.71 1 d PDU A 1 H36A H 0.2976 0.1146 0.5107 0.095 Uiso 0.71 1 calc PR A 1 H36B H 0.2760 0.0496 0.4684 0.095 Uiso 0.71 1 calc PR A 1 C37A C 0.2533(3) 0.0698(17) 0.5246(3) 0.077(4) Uani 0.71 1 d PDU A 1 H37A H 0.2368 0.0018 0.5130 0.093 Uiso 0.71 1 calc PR A 1 H37B H 0.2456 0.1674 0.5171 0.093 Uiso 0.71 1 calc PR A 1 C32B C 0.2551(5) -0.018(3) 0.5790(7) 0.040(6) Uiso 0.29 1 d PD A 2 H32B H 0.2555 -0.1147 0.5929 0.048 Uiso 0.29 1 calc PR A 2 C33B C 0.2859(5) 0.058(4) 0.5899(11) 0.082(10) Uiso 0.29 1 d PD A 2 H33C H 0.2925 0.0526 0.6227 0.098 Uiso 0.29 1 calc PR A 2 H33D H 0.2834 0.1597 0.5816 0.098 Uiso 0.29 1 calc PR A 2 C34B C 0.3110(7) -0.007(3) 0.5653(8) 0.069(9) Uiso 0.29 1 d PD A 2 H34C H 0.3302 0.0504 0.5716 0.083 Uiso 0.29 1 calc PR A 2 H34D H 0.3157 -0.1050 0.5766 0.083 Uiso 0.29 1 calc PR A 2 C35B C 0.3010(6) -0.012(4) 0.5149(8) 0.063(8) Uiso 0.29 1 d PD A 2 H35C H 0.2988 0.0865 0.5031 0.075 Uiso 0.29 1 calc PR A 2 H35D H 0.3171 -0.0606 0.5002 0.075 Uiso 0.29 1 calc PR A 2 C36B C 0.2705(5) -0.090(3) 0.5034(11) 0.075(9) Uiso 0.29 1 d PD A 2 H36C H 0.2732 -0.1921 0.5116 0.091 Uiso 0.29 1 calc PR A 2 H36D H 0.2639 -0.0844 0.4706 0.091 Uiso 0.29 1 calc PR A 2 C37B C 0.2457(6) -0.025(3) 0.5283(7) 0.062(8) Uiso 0.29 1 d PD A 2 H37C H 0.2265 -0.0823 0.5220 0.075 Uiso 0.29 1 calc PR A 2 H37D H 0.2411 0.0726 0.5168 0.075 Uiso 0.29 1 calc PR A 2 O41 O 0.09371(12) 0.3571(5) 0.45352(15) 0.0503(12) Uani 1 1 d . . . O42 O 0.07490(11) 0.1444(5) 0.42505(16) 0.0492(12) Uani 1 1 d . . . C41 C 0.07777(18) 0.2812(8) 0.4245(2) 0.0494(18) Uani 1 1 d . . . C42 C 0.06047(18) 0.3579(8) 0.3833(2) 0.0536(19) Uani 1 1 d . . . H42A H 0.0505 0.4454 0.3941 0.064 Uiso 1 1 calc R . . C43 C 0.0848(2) 0.4056(12) 0.3531(3) 0.088(3) Uani 1 1 d . . . H43A H 0.1003 0.4681 0.3705 0.105 Uiso 1 1 calc R . . H43B H 0.0957 0.3208 0.3433 0.105 Uiso 1 1 calc R . . C44 C 0.0690(3) 0.4869(13) 0.3115(4) 0.099(4) Uani 1 1 d . . . H44A H 0.0601 0.5770 0.3215 0.118 Uiso 1 1 calc R . . H44B H 0.0847 0.5117 0.2918 0.118 Uiso 1 1 calc R . . C45 C 0.0436(2) 0.4004(11) 0.2851(3) 0.071(2) Uani 1 1 d . . . H45A H 0.0525 0.3150 0.2723 0.086 Uiso 1 1 calc R . . H45B H 0.0332 0.4583 0.2599 0.086 Uiso 1 1 calc R . . C46 C 0.0199(2) 0.3545(12) 0.3156(3) 0.080(3) Uani 1 1 d . . . H46A H 0.0038 0.2951 0.2982 0.096 Uiso 1 1 calc R . . H46B H 0.0098 0.4402 0.3263 0.096 Uiso 1 1 calc R . . C47 C 0.03544(18) 0.2689(10) 0.3563(3) 0.062(2) Uani 1 1 d . . . H47A H 0.0197 0.2412 0.3756 0.075 Uiso 1 1 calc R . . H47B H 0.0447 0.1806 0.3458 0.075 Uiso 1 1 calc R . . O51 O 0.14981(11) 0.2043(5) 0.44472(14) 0.0430(11) Uani 1 1 d . . . O52 O 0.12980(11) -0.0175(5) 0.44341(15) 0.0416(11) Uani 1 1 d . . . C51 C 0.14721(15) 0.0762(7) 0.4305(2) 0.0367(14) Uani 1 1 d . . . C52 C 0.16786(16) 0.0332(7) 0.3953(2) 0.0408(15) Uani 1 1 d . . . H52A H 0.1613 -0.0641 0.3842 0.049 Uiso 1 1 calc R . . C53 C 0.1636(2) 0.1342(9) 0.3552(3) 0.067(2) Uani 1 1 d . . . H53A H 0.1684 0.2332 0.3654 0.081 Uiso 1 1 calc R . . H53B H 0.1418 0.1311 0.3408 0.081 Uiso 1 1 calc R . . C54 C 0.1856(3) 0.0884(11) 0.3209(3) 0.084(3) Uani 1 1 d . . . H54A H 0.1786 -0.0045 0.3074 0.101 Uiso 1 1 calc R . . H54B H 0.1844 0.1597 0.2964 0.101 Uiso 1 1 calc R . . C55 C 0.2183(3) 0.0754(13) 0.3422(4) 0.100(3) Uani 1 1 d U . . H55A H 0.2310 0.0387 0.3197 0.120 Uiso 1 1 calc R . . H55B H 0.2262 0.1714 0.3515 0.120 Uiso 1 1 calc R . . C56 C 0.2222(3) -0.0180(14) 0.3810(4) 0.101(4) Uani 1 1 d U . . H56A H 0.2441 -0.0158 0.3946 0.121 Uiso 1 1 calc R . . H56B H 0.2173 -0.1170 0.3709 0.121 Uiso 1 1 calc R . . C57 C 0.2015(2) 0.0230(11) 0.4171(3) 0.079(3) Uani 1 1 d . . . H57A H 0.2034 -0.0500 0.4411 0.094 Uiso 1 1 calc R . . H57B H 0.2083 0.1159 0.4307 0.094 Uiso 1 1 calc R . . O61 O 0.14993(12) 0.0361(6) 0.69777(18) 0.0550(13) Uani 1 1 d . . . O62 O 0.10978(13) 0.0993(6) 0.64757(19) 0.0667(15) Uani 1 1 d . . . C61 C 0.1226(2) 0.0805(9) 0.6867(3) 0.063(2) Uani 1 1 d . . . C62 C 0.1038(3) 0.1229(19) 0.7239(4) 0.132(3) Uani 1 1 d U . . H62A H 0.1119 0.2153 0.7374 0.158 Uiso 1 1 calc R . . C63 C 0.1055(4) 0.0128(17) 0.7599(5) 0.146(3) Uani 1 1 d U . . H63A H 0.1274 -0.0024 0.7727 0.175 Uiso 1 1 calc R . . H63B H 0.0972 -0.0787 0.7470 0.175 Uiso 1 1 calc R . . C64 C 0.0863(3) 0.063(2) 0.7980(5) 0.154(3) Uani 1 1 d U . . H64A H 0.0889 -0.0049 0.8235 0.184 Uiso 1 1 calc R . . H64B H 0.0930 0.1588 0.8091 0.184 Uiso 1 1 calc R . . C65 C 0.0524(3) 0.065(2) 0.7757(5) 0.152(3) Uani 1 1 d U . . H65A H 0.0467 -0.0292 0.7623 0.182 Uiso 1 1 calc R . . H65B H 0.0386 0.0856 0.7986 0.182 Uiso 1 1 calc R . . C66 C 0.0484(3) 0.1750(18) 0.7406(5) 0.145(3) Uani 1 1 d U . . H66A H 0.0545 0.2692 0.7539 0.175 Uiso 1 1 calc R . . H66B H 0.0263 0.1803 0.7277 0.175 Uiso 1 1 calc R . . C67 C 0.0673(3) 0.1413(19) 0.7053(4) 0.138(3) Uani 1 1 d U . . H67A H 0.0649 0.2183 0.6826 0.166 Uiso 1 1 calc R . . H67B H 0.0596 0.0517 0.6903 0.166 Uiso 1 1 calc R . . O71 O 0.05358(11) 0.0447(6) 0.50271(19) 0.0580(14) Uani 1 1 d . . . O72 O 0.07196(12) 0.0976(6) 0.57378(19) 0.0592(14) Uani 1 1 d . . . C71 C 0.05123(19) 0.0857(10) 0.5423(3) 0.061(2) Uani 1 1 d . . . C72 C 0.0178(2) 0.1224(11) 0.5493(3) 0.079(3) Uani 1 1 d . . . H72A H 0.0042 0.0524 0.5309 0.095 Uiso 1 1 calc R . . C73 C 0.0112(2) 0.1055(13) 0.5964(4) 0.098(4) Uani 1 1 d . . . H73A H 0.0149 0.0046 0.6054 0.118 Uiso 1 1 calc R . . H73B H 0.0262 0.1646 0.6162 0.118 Uiso 1 1 calc R . . C74 C -0.0205(2) 0.1454(15) 0.6043(5) 0.113(4) Uani 1 1 d . . . H74A H -0.0353 0.0747 0.5895 0.136 Uiso 1 1 calc R . . H74B H -0.0219 0.1427 0.6370 0.136 Uiso 1 1 calc R . . C75 C -0.0288(3) 0.2831(13) 0.5876(5) 0.112(4) Uani 1 1 d . . . H75A H -0.0365 0.3540 0.6058 0.134 Uiso 1 1 calc R . . C76 C -0.0245(3) 0.3111(15) 0.5390(5) 0.114(4) Uani 1 1 d . . . H76A H -0.0280 0.4136 0.5321 0.137 Uiso 1 1 calc R . . H76B H -0.0400 0.2555 0.5190 0.137 Uiso 1 1 calc R . . C77 C 0.0094(2) 0.2674(10) 0.5299(4) 0.089(3) Uani 1 1 d . . . H77A H 0.0104 0.2661 0.4971 0.107 Uiso 1 1 calc R . . H77B H 0.0245 0.3389 0.5436 0.107 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 0.0427(3) 0.0276(3) 0.0265(2) -0.00125(19) 0.0022(2) 0.0015(2) Pd2 0.0470(3) 0.0261(3) 0.0266(2) -0.00154(19) 0.0022(2) 0.0039(2) Pd3 0.0484(3) 0.0270(3) 0.0333(3) 0.0004(2) -0.0002(2) 0.0038(2) Pd4 0.0393(3) 0.0317(3) 0.0363(3) 0.0019(2) 0.0012(2) 0.0020(2) Pd5 0.0419(3) 0.0286(3) 0.0396(3) -0.0004(2) 0.0102(2) 0.0019(2) N1 0.042(3) 0.028(3) 0.030(3) -0.003(2) 0.003(2) -0.003(2) O1 0.047(3) 0.034(3) 0.040(2) -0.008(2) 0.004(2) 0.007(2) C1 0.050(4) 0.038(4) 0.041(4) -0.003(3) -0.003(3) 0.002(3) C2 0.032(3) 0.036(4) 0.039(3) 0.002(3) 0.007(3) -0.005(3) C3 0.050(4) 0.027(3) 0.040(4) 0.003(3) 0.003(3) -0.006(3) C4 0.066(5) 0.034(4) 0.053(4) -0.001(3) -0.026(4) 0.007(4) N2 0.036(3) 0.027(3) 0.034(3) 0.002(2) 0.006(2) 0.000(2) N3 0.047(3) 0.029(3) 0.033(3) 0.000(2) 0.001(2) 0.004(2) O2 0.047(2) 0.024(2) 0.040(2) -0.0001(19) -0.004(2) 0.003(2) O11 0.055(3) 0.043(3) 0.034(2) -0.010(2) 0.001(2) 0.009(2) O12 0.050(3) 0.050(3) 0.032(2) -0.006(2) 0.004(2) 0.018(2) C11 0.056(4) 0.024(3) 0.048(4) -0.005(3) 0.015(3) 0.002(3) C12 0.051(4) 0.040(4) 0.042(4) -0.007(3) 0.014(3) 0.004(3) C13 0.077(6) 0.098(7) 0.053(5) -0.026(5) 0.011(4) 0.021(5) C14 0.084(7) 0.128(10) 0.060(6) -0.033(6) 0.026(5) 0.018(7) C15 0.080(6) 0.064(6) 0.093(7) -0.023(5) 0.038(5) 0.003(5) C16 0.070(5) 0.064(6) 0.078(6) -0.004(5) 0.021(5) 0.016(5) C17 0.051(4) 0.048(5) 0.062(5) -0.004(4) 0.019(4) 0.010(4) O21 0.055(3) 0.031(2) 0.032(2) -0.0010(19) -0.006(2) 0.008(2) O22 0.052(3) 0.029(3) 0.037(2) -0.0013(19) -0.004(2) 0.006(2) C21 0.040(3) 0.043(4) 0.032(3) -0.007(3) -0.002(3) 0.004(3) C22 0.048(4) 0.041(4) 0.033(3) -0.003(3) -0.002(3) -0.007(3) C23 0.102(7) 0.049(5) 0.032(4) -0.003(3) 0.012(4) -0.014(5) C24 0.111(8) 0.085(8) 0.075(6) -0.027(5) 0.056(6) -0.027(6) C25 0.098(8) 0.095(8) 0.082(7) -0.037(6) 0.032(6) 0.006(6) C26 0.082(6) 0.058(5) 0.064(5) -0.024(4) -0.003(5) 0.024(5) C27 0.069(5) 0.036(4) 0.045(4) -0.008(3) -0.004(4) -0.010(4) O31 0.042(3) 0.046(3) 0.045(3) -0.002(2) 0.003(2) 0.000(2) O32 0.050(3) 0.042(3) 0.051(3) -0.009(2) -0.003(2) 0.013(2) C31 0.035(3) 0.073(6) 0.032(3) -0.021(4) -0.001(3) 0.005(3) C32A 0.031(4) 0.036(5) 0.038(4) -0.014(4) 0.004(3) -0.007(4) C33A 0.077(7) 0.102(9) 0.056(6) 0.038(7) 0.030(6) 0.056(7) C34A 0.080(9) 0.131(14) 0.062(6) 0.031(7) 0.034(6) 0.065(9) C35A 0.042(6) 0.105(9) 0.058(5) -0.022(6) 0.017(5) 0.010(6) C36A 0.075(8) 0.132(11) 0.036(5) 0.020(6) 0.022(5) 0.029(8) C37A 0.076(8) 0.110(11) 0.051(5) 0.043(7) 0.029(5) 0.049(8) O41 0.075(3) 0.042(3) 0.030(2) -0.008(2) -0.010(2) 0.012(3) O42 0.058(3) 0.038(3) 0.048(3) 0.004(2) -0.008(2) 0.003(2) C41 0.060(4) 0.050(5) 0.036(4) 0.003(3) -0.003(3) 0.020(4) C42 0.074(5) 0.044(4) 0.040(4) 0.003(3) -0.003(4) 0.020(4) C43 0.093(7) 0.095(8) 0.065(6) 0.039(6) -0.028(5) -0.020(6) C44 0.091(8) 0.124(10) 0.075(7) 0.042(6) -0.009(6) -0.022(7) C45 0.080(6) 0.088(7) 0.043(4) 0.016(4) 0.001(4) -0.003(5) C46 0.069(6) 0.115(9) 0.051(5) 0.026(5) -0.006(4) 0.018(6) C47 0.047(4) 0.095(7) 0.043(4) 0.014(4) -0.001(3) 0.002(4) O51 0.059(3) 0.037(3) 0.034(2) -0.002(2) 0.011(2) 0.000(2) O52 0.051(3) 0.032(3) 0.043(3) -0.001(2) 0.011(2) 0.000(2) C51 0.049(4) 0.033(4) 0.027(3) 0.000(3) 0.002(3) 0.005(3) C52 0.057(4) 0.033(4) 0.034(3) -0.008(3) 0.009(3) -0.004(3) C53 0.103(7) 0.053(5) 0.051(5) -0.001(4) 0.034(5) 0.019(5) C54 0.146(10) 0.066(6) 0.049(5) 0.010(4) 0.046(6) 0.019(6) C55 0.106(7) 0.090(6) 0.114(7) -0.044(6) 0.052(6) -0.024(6) C56 0.075(6) 0.131(8) 0.097(7) -0.039(6) 0.012(5) 0.027(5) C57 0.069(6) 0.106(8) 0.059(5) -0.032(5) 0.002(4) 0.023(5) O61 0.056(3) 0.053(3) 0.056(3) 0.000(3) 0.011(3) -0.008(3) O62 0.080(4) 0.070(4) 0.054(3) -0.018(3) 0.022(3) 0.007(3) C61 0.073(6) 0.053(5) 0.066(6) -0.001(4) 0.022(5) -0.015(4) C62 0.119(5) 0.191(8) 0.101(5) 0.032(5) 0.067(5) 0.025(6) C63 0.134(5) 0.204(8) 0.113(6) 0.036(5) 0.062(5) 0.031(6) C64 0.139(6) 0.212(8) 0.122(6) 0.037(6) 0.060(5) 0.030(6) C65 0.134(6) 0.209(8) 0.124(6) 0.035(5) 0.060(5) 0.029(6) C66 0.129(5) 0.200(8) 0.119(6) 0.032(5) 0.060(5) 0.028(6) C67 0.123(5) 0.194(8) 0.111(6) 0.030(5) 0.062(5) 0.029(6) O71 0.045(3) 0.066(4) 0.064(4) 0.010(3) 0.014(3) 0.008(3) O72 0.049(3) 0.055(3) 0.074(4) -0.005(3) 0.010(3) 0.010(3) C71 0.055(5) 0.061(5) 0.071(6) 0.006(5) 0.016(4) 0.015(4) C72 0.056(5) 0.088(7) 0.095(7) 0.003(6) 0.019(5) 0.026(5) C73 0.084(7) 0.088(8) 0.133(10) 0.009(7) 0.057(7) 0.021(6) C74 0.077(7) 0.130(12) 0.141(11) -0.022(9) 0.046(7) 0.014(7) C75 0.083(8) 0.086(9) 0.166(14) -0.036(9) 0.013(8) 0.018(7) C76 0.082(7) 0.135(11) 0.120(11) 0.004(9) -0.002(7) 0.060(7) C77 0.061(5) 0.063(6) 0.136(10) 0.003(6) -0.014(6) 0.018(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 N1 1.949(5) . ? Pd1 O11 2.004(5) . ? Pd1 O31 2.036(5) . ? Pd1 O21 2.083(4) . ? Pd1 Pd3 2.923(2) . ? Pd2 N1 1.943(5) . ? Pd2 O12 2.013(4) . ? Pd2 O51 2.065(5) . ? Pd2 O41 2.074(5) . ? Pd2 Pd4 2.897(2) . ? Pd3 N3 2.006(5) . ? Pd3 O61 2.021(5) . ? Pd3 O32 2.038(5) . ? Pd3 O22 2.051(4) . ? Pd4 O71 2.004(5) . ? Pd4 N2 2.005(5) . ? Pd4 O52 2.024(5) . ? Pd4 O42 2.042(5) . ? Pd5 N2 1.958(5) . ? Pd5 N3 1.981(5) . ? Pd5 O62 2.044(5) . ? Pd5 O72 2.060(5) . ? N1 O1 1.197(6) . ? C1 C2 1.501(9) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N2 1.289(8) . ? C2 O2 1.388(7) . ? C3 N3 1.278(8) . ? C3 O2 1.393(8) . ? C3 C4 1.497(9) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O11 C11 1.279(8) . ? O12 C11 1.272(8) . ? C11 C12 1.545(9) . ? C12 C17 1.548(10) . ? C12 C13 1.553(10) . ? C12 H12A 1.0000 . ? C13 C14 1.536(11) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.532(14) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.513(12) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.521(10) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O21 C21 1.272(8) . ? O22 C21 1.268(8) . ? C21 C22 1.553(9) . ? C22 C27 1.514(10) . ? C22 C23 1.554(9) . ? C22 H22A 1.0000 . ? C23 C24 1.473(13) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.528(14) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.541(14) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.518(11) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? O31 C31 1.256(9) . ? O32 C31 1.280(9) . ? C31 C32A 1.529(11) . ? C31 C32B 1.57(3) . ? C32A C33A 1.513(8) . ? C32A C37A 1.522(7) . ? C32A H32A 1.0000 . ? C33A C34A 1.532(8) . ? C33A H33A 0.9900 . ? C33A H33B 0.9900 . ? C34A C35A 1.521(8) . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C35A C36A 1.520(8) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C36A C37A 1.520(8) . ? C36A H36A 0.9900 . ? C36A H36B 0.9900 . ? C37A H37A 0.9900 . ? C37A H37B 0.9900 . ? C32B C33B 1.518(9) . ? C32B C37B 1.524(9) . ? C32B H32B 1.0000 . ? C33B C34B 1.524(9) . ? C33B H33C 0.9900 . ? C33B H33D 0.9900 . ? C34B C35B 1.521(9) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? C35B C36B 1.517(9) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36B C37B 1.521(9) . ? C36B H36C 0.9900 . ? C36B H36D 0.9900 . ? C37B H37C 0.9900 . ? C37B H37D 0.9900 . ? O41 C41 1.262(9) . ? O42 C41 1.288(9) . ? C41 C42 1.539(9) . ? C42 C47 1.521(11) . ? C42 C43 1.549(12) . ? C42 H42A 1.0000 . ? C43 C44 1.547(12) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.512(13) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.526(11) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.544(10) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? O51 C51 1.274(8) . ? O52 C51 1.255(8) . ? C51 C52 1.530(9) . ? C52 C53 1.522(10) . ? C52 C57 1.529(11) . ? C52 H52A 1.0000 . ? C53 C54 1.559(11) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.493(14) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.449(16) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C57 1.546(13) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? O61 C61 1.264(10) . ? O62 C61 1.248(10) . ? C61 C62 1.522(14) . ? C62 C63 1.488(18) . ? C62 C67 1.626(17) . ? C62 H62A 1.0000 . ? C63 C64 1.576(18) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.542(19) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.465(18) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.462(16) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? O71 C71 1.266(10) . ? O72 C71 1.225(10) . ? C71 C72 1.541(11) . ? C72 C73 1.489(14) . ? C72 C77 1.504(13) . ? C72 H72A 1.0000 . ? C73 C74 1.482(13) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.414(17) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.518(18) . ? C75 H75A 0.9500 . ? C76 C77 1.592(14) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? 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 O11 97.8(2) . . ? N1 Pd1 O31 89.1(2) . . ? O11 Pd1 O31 170.87(19) . . ? N1 Pd1 O21 178.5(2) . . ? O11 Pd1 O21 83.57(18) . . ? O31 Pd1 O21 89.46(18) . . ? N1 Pd1 Pd3 101.60(16) . . ? O11 Pd1 Pd3 103.82(14) . . ? O31 Pd1 Pd3 80.46(14) . . ? O21 Pd1 Pd3 78.64(13) . . ? N1 Pd2 O12 97.5(2) . . ? N1 Pd2 O51 90.3(2) . . ? O12 Pd2 O51 171.00(18) . . ? N1 Pd2 O41 178.3(2) . . ? O12 Pd2 O41 84.18(19) . . ? O51 Pd2 O41 88.03(19) . . ? N1 Pd2 Pd4 100.95(16) . . ? O12 Pd2 Pd4 103.04(15) . . ? O51 Pd2 Pd4 79.81(13) . . ? O41 Pd2 Pd4 79.11(15) . . ? N3 Pd3 O61 94.2(2) . . ? N3 Pd3 O32 90.3(2) . . ? O61 Pd3 O32 170.2(2) . . ? N3 Pd3 O22 176.61(19) . . ? O61 Pd3 O22 84.6(2) . . ? O32 Pd3 O22 91.3(2) . . ? N3 Pd3 Pd1 95.94(16) . . ? O61 Pd3 Pd1 109.14(16) . . ? O32 Pd3 Pd1 78.94(15) . . ? O22 Pd3 Pd1 81.45(14) . . ? O71 Pd4 N2 94.0(2) . . ? O71 Pd4 O52 170.2(2) . . ? N2 Pd4 O52 91.2(2) . . ? O71 Pd4 O42 86.9(2) . . ? N2 Pd4 O42 178.1(2) . . ? O52 Pd4 O42 88.1(2) . . ? O71 Pd4 Pd2 107.57(18) . . ? N2 Pd4 Pd2 96.68(15) . . ? O52 Pd4 Pd2 79.99(14) . . ? O42 Pd4 Pd2 81.48(15) . . ? N2 Pd5 N3 90.1(2) . . ? N2 Pd5 O62 172.7(2) . . ? N3 Pd5 O62 96.1(2) . . ? N2 Pd5 O72 95.5(2) . . ? N3 Pd5 O72 172.7(2) . . ? O62 Pd5 O72 78.0(2) . . ? O1 N1 Pd2 116.4(4) . . ? O1 N1 Pd1 117.6(4) . . ? Pd2 N1 Pd1 125.9(3) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N2 C2 O2 122.8(6) . . ? N2 C2 C1 125.7(6) . . ? O2 C2 C1 111.4(5) . . ? N3 C3 O2 123.5(6) . . ? N3 C3 C4 125.7(6) . . ? O2 C3 C4 110.7(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 N2 Pd5 123.6(4) . . ? C2 N2 Pd4 122.2(4) . . ? Pd5 N2 Pd4 114.2(3) . . ? C3 N3 Pd5 123.0(5) . . ? C3 N3 Pd3 124.6(5) . . ? Pd5 N3 Pd3 112.4(3) . . ? C2 O2 C3 124.3(5) . . ? C11 O11 Pd1 133.2(4) . . ? C11 O12 Pd2 133.7(4) . . ? O12 C11 O11 127.2(6) . . ? O12 C11 C12 116.6(6) . . ? O11 C11 C12 116.1(6) . . ? C11 C12 C17 110.9(6) . . ? C11 C12 C13 111.6(6) . . ? C17 C12 C13 110.9(6) . . ? C11 C12 H12A 107.8 . . ? C17 C12 H12A 107.8 . . ? C13 C12 H12A 107.8 . . ? C14 C13 C12 109.3(7) . . ? C14 C13 H13A 109.8 . . ? C12 C13 H13A 109.8 . . ? C14 C13 H13B 109.8 . . ? C12 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? C15 C14 C13 110.5(8) . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 111.6(8) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 108.0 . . ? C15 C16 C17 111.7(7) . . ? C15 C16 H16A 109.3 . . ? C17 C16 H16A 109.3 . . ? C15 C16 H16B 109.3 . . ? C17 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? C16 C17 C12 110.4(6) . . ? C16 C17 H17A 109.6 . . ? C12 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? C12 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? C21 O21 Pd1 126.2(4) . . ? C21 O22 Pd3 123.5(4) . . ? O22 C21 O21 125.9(6) . . ? O22 C21 C22 116.8(5) . . ? O21 C21 C22 117.3(6) . . ? C27 C22 C23 110.8(6) . . ? C27 C22 C21 113.2(5) . . ? C23 C22 C21 110.5(6) . . ? C27 C22 H22A 107.3 . . ? C23 C22 H22A 107.3 . . ? C21 C22 H22A 107.3 . . ? C24 C23 C22 111.0(7) . . ? C24 C23 H23A 109.4 . . ? C22 C23 H23A 109.4 . . ? C24 C23 H23B 109.4 . . ? C22 C23 H23B 109.4 . . ? H23A C23 H23B 108.0 . . ? C23 C24 C25 112.8(8) . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24A 109.0 . . ? C23 C24 H24B 109.0 . . ? C25 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 110.3(7) . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C27 C26 C25 111.0(7) . . ? C27 C26 H26A 109.4 . . ? C25 C26 H26A 109.4 . . ? C27 C26 H26B 109.4 . . ? C25 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C22 C27 C26 112.7(6) . . ? C22 C27 H27A 109.0 . . ? C26 C27 H27A 109.0 . . ? C22 C27 H27B 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C31 O31 Pd1 123.6(5) . . ? C31 O32 Pd3 125.5(4) . . ? O31 C31 O32 126.1(6) . . ? O31 C31 C32A 110.2(7) . . ? O32 C31 C32A 123.7(7) . . ? O31 C31 C32B 135.7(11) . . ? O32 C31 C32B 97.4(11) . . ? C32A C31 C32B 27.0(8) . . ? C33A C32A C37A 110.1(8) . . ? C33A C32A C31 112.6(8) . . ? C37A C32A C31 111.8(7) . . ? C33A C32A H32A 107.4 . . ? C37A C32A H32A 107.4 . . ? C31 C32A H32A 107.4 . . ? C32A C33A C34A 111.5(9) . . ? C32A C33A H33A 109.3 . . ? C34A C33A H33A 109.3 . . ? C32A C33A H33B 109.3 . . ? C34A C33A H33B 109.3 . . ? H33A C33A H33B 108.0 . . ? C35A C34A C33A 111.0(9) . . ? C35A C34A H34A 109.4 . . ? C33A C34A H34A 109.4 . . ? C35A C34A H34B 109.4 . . ? C33A C34A H34B 109.4 . . ? H34A C34A H34B 108.0 . . ? C36A C35A C34A 108.5(10) . . ? C36A C35A H35A 110.0 . . ? C34A C35A H35A 110.0 . . ? C36A C35A H35B 110.0 . . ? C34A C35A H35B 110.0 . . ? H35A C35A H35B 108.4 . . ? C37A C36A C35A 110.4(10) . . ? C37A C36A H36A 109.6 . . ? C35A C36A H36A 109.6 . . ? C37A C36A H36B 109.6 . . ? C35A C36A H36B 109.6 . . ? H36A C36A H36B 108.1 . . ? C36A C37A C32A 112.8(8) . . ? C36A C37A H37A 109.0 . . ? C32A C37A H37A 109.0 . . ? C36A C37A H37B 109.0 . . ? C32A C37A H37B 109.0 . . ? H37A C37A H37B 107.8 . . ? C33B C32B C37B 111(2) . . ? C33B C32B C31 104.9(18) . . ? C37B C32B C31 106.7(17) . . ? C33B C32B H32B 111.5 . . ? C37B C32B H32B 111.5 . . ? C31 C32B H32B 111.5 . . ? C32B C33B C34B 112(2) . . ? C32B C33B H33C 109.1 . . ? C34B C33B H33C 109.1 . . ? C32B C33B H33D 109.1 . . ? C34B C33B H33D 109.1 . . ? H33C C33B H33D 107.8 . . ? C35B C34B C33B 111(3) . . ? C35B C34B H34C 109.4 . . ? C33B C34B H34C 109.4 . . ? C35B C34B H34D 109.4 . . ? C33B C34B H34D 109.4 . . ? H34C C34B H34D 108.0 . . ? C36B C35B C34B 112(2) . . ? C36B C35B H35C 109.2 . . ? C34B C35B H35C 109.2 . . ? C36B C35B H35D 109.2 . . ? C34B C35B H35D 109.2 . . ? H35C C35B H35D 107.9 . . ? C35B C36B C37B 111(2) . . ? C35B C36B H36C 109.5 . . ? C37B C36B H36C 109.5 . . ? C35B C36B H36D 109.5 . . ? C37B C36B H36D 109.5 . . ? H36C C36B H36D 108.1 . . ? C36B C37B C32B 113(2) . . ? C36B C37B H37C 108.9 . . ? C32B C37B H37C 108.9 . . ? C36B C37B H37D 108.9 . . ? C32B C37B H37D 108.9 . . ? H37C C37B H37D 107.7 . . ? C41 O41 Pd2 123.6(4) . . ? C41 O42 Pd4 122.9(4) . . ? O41 C41 O42 126.7(6) . . ? O41 C41 C42 117.4(7) . . ? O42 C41 C42 116.0(6) . . ? C47 C42 C41 114.5(7) . . ? C47 C42 C43 110.1(7) . . ? C41 C42 C43 107.6(6) . . ? C47 C42 H42A 108.1 . . ? C41 C42 H42A 108.1 . . ? C43 C42 H42A 108.1 . . ? C44 C43 C42 110.3(8) . . ? C44 C43 H43A 109.6 . . ? C42 C43 H43A 109.6 . . ? C44 C43 H43B 109.6 . . ? C42 C43 H43B 109.6 . . ? H43A C43 H43B 108.1 . . ? C45 C44 C43 112.3(9) . . ? C45 C44 H44A 109.1 . . ? C43 C44 H44A 109.1 . . ? C45 C44 H44B 109.1 . . ? C43 C44 H44B 109.1 . . ? H44A C44 H44B 107.9 . . ? C44 C45 C46 110.0(8) . . ? C44 C45 H45A 109.7 . . ? C46 C45 H45A 109.7 . . ? C44 C45 H45B 109.7 . . ? C46 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? C45 C46 C47 111.2(7) . . ? C45 C46 H46A 109.4 . . ? C47 C46 H46A 109.4 . . ? C45 C46 H46B 109.4 . . ? C47 C46 H46B 109.4 . . ? H46A C46 H46B 108.0 . . ? C42 C47 C46 110.3(8) . . ? C42 C47 H47A 109.6 . . ? C46 C47 H47A 109.6 . . ? C42 C47 H47B 109.6 . . ? C46 C47 H47B 109.6 . . ? H47A C47 H47B 108.1 . . ? C51 O51 Pd2 123.4(4) . . ? C51 O52 Pd4 125.0(4) . . ? O52 C51 O51 125.9(6) . . ? O52 C51 C52 117.6(6) . . ? O51 C51 C52 116.4(6) . . ? C53 C52 C57 112.9(7) . . ? C53 C52 C51 111.1(6) . . ? C57 C52 C51 109.8(6) . . ? C53 C52 H52A 107.6 . . ? C57 C52 H52A 107.6 . . ? C51 C52 H52A 107.6 . . ? C52 C53 C54 109.2(7) . . ? C52 C53 H53A 109.8 . . ? C54 C53 H53A 109.8 . . ? C52 C53 H53B 109.8 . . ? C54 C53 H53B 109.8 . . ? H53A C53 H53B 108.3 . . ? C55 C54 C53 112.0(8) . . ? C55 C54 H54A 109.2 . . ? C53 C54 H54A 109.2 . . ? C55 C54 H54B 109.2 . . ? C53 C54 H54B 109.2 . . ? H54A C54 H54B 107.9 . . ? C56 C55 C54 113.4(9) . . ? C56 C55 H55A 108.9 . . ? C54 C55 H55A 108.9 . . ? C56 C55 H55B 108.9 . . ? C54 C55 H55B 108.9 . . ? H55A C55 H55B 107.7 . . ? C55 C56 C57 113.4(9) . . ? C55 C56 H56A 108.9 . . ? C57 C56 H56A 108.9 . . ? C55 C56 H56B 108.9 . . ? C57 C56 H56B 108.9 . . ? H56A C56 H56B 107.7 . . ? C52 C57 C56 109.3(7) . . ? C52 C57 H57A 109.8 . . ? C56 C57 H57A 109.8 . . ? C52 C57 H57B 109.8 . . ? C56 C57 H57B 109.8 . . ? H57A C57 H57B 108.3 . . ? C61 O61 Pd3 123.4(5) . . ? C61 O62 Pd5 132.5(6) . . ? O62 C61 O61 125.8(8) . . ? O62 C61 C62 115.9(9) . . ? O61 C61 C62 118.2(9) . . ? C63 C62 C61 111.7(12) . . ? C63 C62 C67 106.1(11) . . ? C61 C62 C67 111.8(11) . . ? C63 C62 H62A 109.0 . . ? C61 C62 H62A 109.0 . . ? C67 C62 H62A 109.0 . . ? C62 C63 C64 109.9(12) . . ? C62 C63 H63A 109.7 . . ? C64 C63 H63A 109.7 . . ? C62 C63 H63B 109.7 . . ? C64 C63 H63B 109.7 . . ? H63A C63 H63B 108.2 . . ? C65 C64 C63 105.0(13) . . ? C65 C64 H64A 110.7 . . ? C63 C64 H64A 110.7 . . ? C65 C64 H64B 110.7 . . ? C63 C64 H64B 110.7 . . ? H64A C64 H64B 108.8 . . ? C66 C65 C64 109.9(14) . . ? C66 C65 H65A 109.7 . . ? C64 C65 H65A 109.7 . . ? C66 C65 H65B 109.7 . . ? C64 C65 H65B 109.7 . . ? H65A C65 H65B 108.2 . . ? C65 C66 C67 110.1(13) . . ? C65 C66 H66A 109.6 . . ? C67 C66 H66A 109.6 . . ? C65 C66 H66B 109.6 . . ? C67 C66 H66B 109.6 . . ? H66A C66 H66B 108.2 . . ? C66 C67 C62 113.2(12) . . ? C66 C67 H67A 108.9 . . ? C62 C67 H67A 108.9 . . ? C66 C67 H67B 108.9 . . ? C62 C67 H67B 108.9 . . ? H67A C67 H67B 107.8 . . ? C71 O71 Pd4 124.5(5) . . ? C71 O72 Pd5 132.4(5) . . ? O72 C71 O71 127.6(7) . . ? O72 C71 C72 119.4(8) . . ? O71 C71 C72 113.0(8) . . ? C73 C72 C77 113.5(9) . . ? C73 C72 C71 114.1(8) . . ? C77 C72 C71 109.5(8) . . ? C73 C72 H72A 106.4 . . ? C77 C72 H72A 106.4 . . ? C71 C72 H72A 106.4 . . ? C74 C73 C72 115.0(10) . . ? C74 C73 H73A 108.5 . . ? C72 C73 H73A 108.5 . . ? C74 C73 H73B 108.5 . . ? C72 C73 H73B 108.5 . . ? H73A C73 H73B 107.5 . . ? C75 C74 C73 112.0(11) . . ? C75 C74 H74A 109.2 . . ? C73 C74 H74A 109.2 . . ? C75 C74 H74B 109.2 . . ? C73 C74 H74B 109.2 . . ? H74A C74 H74B 107.9 . . ? C74 C75 C76 116.2(11) . . ? C74 C75 H75A 121.9 . . ? C76 C75 H75A 121.9 . . ? C75 C76 C77 110.7(9) . . ? C75 C76 H76A 109.5 . . ? C77 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 108.1 . . ? C72 C77 C76 110.4(9) . . ? C72 C77 H77A 109.6 . . ? C76 C77 H77A 109.6 . . ? C72 C77 H77B 109.6 . . ? C76 C77 H77B 109.6 . . ? H77A C77 H77B 108.1 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.195 _refine_diff_density_min -0.861 _refine_diff_density_rms 0.119