Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 ####################################################################### # # 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_cmpd2 _database_code_depnum_ccdc_archive 'CCDC 262707' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Pd3(OAc)5NO2 _chemical_melting_point ? _chemical_formula_moiety Pd3O12C10NH15 _chemical_formula_sum 'C10 H15 N O12 Pd3' _chemical_formula_weight 660.43 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 Pna2(1) 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' _cell_length_a 15.854(4) _cell_length_b 11.608(3) _cell_length_c 10.109(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1860.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6893 _cell_measurement_theta_min 2.5693 _cell_measurement_theta_max 25.1753 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 2.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6679 _exptl_absorpt_correction_T_max 0.8213 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 ' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10208 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.27 _reflns_number_total 3284 _reflns_number_gt 3104 _reflns_threshold_expression I>2sigma(I) _computing_data_collection SAINT _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+2.2947P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(5) _refine_ls_number_reflns 3284 _refine_ls_number_parameters 235 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0717 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 -0.48266(3) -0.16629(4) -0.10402(6) 0.03078(13) Uani 1 1 d . . . Pd2 Pd -0.43659(3) -0.09237(4) 0.18108(5) 0.03080(13) Uani 1 1 d . . . Pd3 Pd -0.44343(3) -0.35336(4) 0.10340(4) 0.02744(12) Uani 1 1 d . . . O6 O -0.5584(3) -0.3960(4) 0.0342(5) 0.0424(12) Uani 1 1 d . . . O1 O -0.3265(3) -0.3363(4) 0.1776(5) 0.0383(11) Uani 1 1 d . . . O9 O -0.5479(3) -0.0118(4) 0.1549(5) 0.0377(12) Uani 1 1 d . . . O5 O -0.5635(3) -0.2913(4) -0.1547(5) 0.0423(12) Uani 1 1 d . . . O10 O -0.5849(3) -0.0772(4) -0.0476(5) 0.0361(11) Uani 1 1 d . . . O12 O -0.4807(4) -0.1632(4) 0.3506(5) 0.0476(14) Uani 1 1 d . . . O3 O -0.3860(3) -0.4066(4) -0.0637(5) 0.0397(12) Uani 1 1 d . . . O11 O -0.4940(4) -0.3485(4) 0.2857(5) 0.0409(12) Uani 1 1 d . . . O2 O -0.3187(3) -0.1480(4) 0.2233(6) 0.0505(15) Uani 1 1 d . . . C9 C -0.4982(4) -0.2692(6) 0.3703(7) 0.0361(17) Uani 1 1 d . . . C7 C -0.5961(4) -0.0177(5) 0.0550(6) 0.0302(14) Uani 1 1 d . . . O4 O -0.3863(4) -0.2478(4) -0.1924(5) 0.0462(13) Uani 1 1 d . . . C5 C -0.5913(5) -0.3689(6) -0.0749(7) 0.0352(16) Uani 1 1 d . . . C3 C -0.3624(5) -0.3479(6) -0.1641(8) 0.0436(18) Uani 1 1 d . . . O8 O -0.3401(5) 0.0761(7) 0.0484(9) 0.094(3) Uani 1 1 d . . . O7 O -0.4021(4) -0.0368(5) -0.0765(8) 0.0650(18) Uani 1 1 d . . . C2 C -0.1991(5) -0.2625(8) 0.2634(9) 0.053(2) Uani 1 1 d . . . H2A H -0.1827 -0.3417 0.2540 0.079 Uiso 1 1 calc R . . H2B H -0.1949 -0.2403 0.3546 0.079 Uiso 1 1 calc R . . H2C H -0.1626 -0.2149 0.2109 0.079 Uiso 1 1 calc R . . N1 N -0.3870(4) -0.0081(6) 0.0336(9) 0.0566(19) Uani 1 1 d . . . C1 C -0.2891(4) -0.2478(5) 0.2171(6) 0.0285(14) Uani 1 1 d . . . C4 C -0.3023(7) -0.4048(9) -0.2594(9) 0.077(3) Uani 1 1 d . . . H4A H -0.2886 -0.3520 -0.3292 0.115 Uiso 1 1 calc R . . H4B H -0.3284 -0.4723 -0.2961 0.115 Uiso 1 1 calc R . . H4C H -0.2518 -0.4265 -0.2134 0.115 Uiso 1 1 calc R . . C8 C -0.6768(4) 0.0520(6) 0.0648(7) 0.0375(16) Uani 1 1 d . . . H8A H -0.7092 0.0422 -0.0146 0.056 Uiso 1 1 calc R . . H8B H -0.6632 0.1320 0.0759 0.056 Uiso 1 1 calc R . . H8C H -0.7091 0.0260 0.1394 0.056 Uiso 1 1 calc R . . C6 C -0.6692(5) -0.4312(7) -0.1164(9) 0.054(2) Uani 1 1 d . . . H6A H -0.6844 -0.4862 -0.0496 0.081 Uiso 1 1 calc R . . H6B H -0.6591 -0.4704 -0.1984 0.081 Uiso 1 1 calc R . . H6C H -0.7144 -0.3770 -0.1277 0.081 Uiso 1 1 calc R . . C10 C -0.5253(6) -0.3016(8) 0.5098(8) 0.055(2) Uani 1 1 d . . . H10A H -0.5367 -0.3828 0.5135 0.083 Uiso 1 1 calc R . . H10B H -0.5753 -0.2596 0.5329 0.083 Uiso 1 1 calc R . . H10C H -0.4810 -0.2830 0.5708 0.083 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 0.0398(3) 0.0291(2) 0.0234(2) 0.0013(2) 0.0005(2) 0.0065(2) Pd2 0.0331(2) 0.0252(3) 0.0341(3) -0.0005(2) -0.0066(2) 0.00014(19) Pd3 0.0328(3) 0.0258(2) 0.0237(2) -0.0008(2) -0.0027(2) -0.00145(18) O6 0.045(3) 0.049(3) 0.033(3) -0.001(2) -0.010(2) -0.011(2) O1 0.035(2) 0.038(2) 0.042(3) -0.003(2) -0.009(2) 0.002(2) O9 0.035(3) 0.040(3) 0.039(3) -0.002(2) -0.009(2) 0.013(2) O5 0.055(3) 0.041(3) 0.031(3) -0.008(2) -0.011(2) 0.005(2) O10 0.040(3) 0.038(2) 0.031(2) -0.005(2) -0.002(2) 0.007(2) O12 0.076(4) 0.040(3) 0.027(3) 0.002(2) -0.004(2) 0.003(3) O3 0.058(3) 0.032(2) 0.029(3) -0.0028(18) 0.006(2) 0.007(2) O11 0.050(3) 0.043(3) 0.029(3) -0.002(2) 0.004(2) -0.012(2) O2 0.038(3) 0.037(3) 0.076(4) -0.004(2) -0.019(3) -0.002(2) C9 0.037(4) 0.040(4) 0.032(4) -0.001(3) -0.005(3) 0.006(3) C7 0.040(4) 0.022(3) 0.029(3) 0.005(2) 0.001(3) 0.001(3) O4 0.060(3) 0.050(3) 0.029(3) 0.008(2) 0.018(2) 0.018(3) C5 0.039(4) 0.031(3) 0.035(4) -0.013(3) -0.008(3) 0.008(3) C3 0.055(5) 0.038(4) 0.038(4) -0.001(3) 0.004(4) 0.012(3) O8 0.078(5) 0.098(6) 0.106(6) 0.022(5) -0.016(5) -0.023(4) O7 0.057(4) 0.056(3) 0.083(5) -0.006(3) -0.024(4) 0.008(3) C2 0.031(4) 0.071(5) 0.056(5) -0.002(4) -0.007(4) 0.005(4) N1 0.043(4) 0.050(4) 0.078(6) 0.017(4) 0.007(4) 0.003(3) C1 0.022(3) 0.034(3) 0.030(4) -0.001(2) -0.003(2) 0.002(2) C4 0.107(8) 0.079(6) 0.045(5) 0.008(5) 0.022(5) 0.052(6) C8 0.037(4) 0.049(4) 0.027(4) -0.004(3) -0.001(3) 0.010(3) C6 0.044(4) 0.064(5) 0.055(5) -0.010(4) -0.015(4) -0.011(4) C10 0.068(6) 0.062(5) 0.036(4) 0.012(4) 0.005(4) 0.000(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 O7 1.992(6) . ? Pd1 O5 2.003(5) . ? Pd1 O10 2.005(5) . ? Pd1 O4 2.006(5) . ? Pd1 Pd3 3.0821(9) . ? Pd1 Pd2 3.0945(10) . ? Pd2 N1 1.949(7) . ? Pd2 O9 2.015(4) . ? Pd2 O2 2.023(5) . ? Pd2 O12 2.026(5) . ? Pd2 Pd3 3.1315(10) . ? Pd3 O1 2.009(5) . ? Pd3 O11 2.011(5) . ? Pd3 O6 2.014(5) . ? Pd3 O3 2.017(5) . ? O6 C5 1.261(9) . ? O1 C1 1.252(7) . ? O9 C7 1.268(8) . ? O5 C5 1.286(9) . ? O10 C7 1.259(8) . ? O12 C9 1.276(9) . ? O3 C3 1.278(9) . ? O11 C9 1.258(8) . ? O2 C1 1.252(7) . ? C9 C10 1.522(11) . ? C7 C8 1.517(9) . ? O4 C3 1.256(9) . ? C5 C6 1.492(10) . ? C3 C4 1.507(11) . ? O8 N1 1.237(10) . ? O7 N1 1.187(10) . ? C2 C1 1.511(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 Pd1 O5 173.1(3) . . ? O7 Pd1 O10 95.1(2) . . ? O5 Pd1 O10 85.9(2) . . ? O7 Pd1 O4 86.0(3) . . ? O5 Pd1 O4 91.8(2) . . ? O10 Pd1 O4 170.0(2) . . ? O7 Pd1 Pd3 107.89(19) . . ? O5 Pd1 Pd3 78.04(15) . . ? O10 Pd1 Pd3 109.45(14) . . ? O4 Pd1 Pd3 79.47(13) . . ? O7 Pd1 Pd2 60.6(2) . . ? O5 Pd1 Pd2 126.17(15) . . ? O10 Pd1 Pd2 77.47(14) . . ? O4 Pd1 Pd2 111.46(16) . . ? Pd3 Pd1 Pd2 60.93(2) . . ? N1 Pd2 O9 91.2(2) . . ? N1 Pd2 O2 87.1(3) . . ? O9 Pd2 O2 170.2(2) . . ? N1 Pd2 O12 172.1(3) . . ? O9 Pd2 O12 89.8(2) . . ? O2 Pd2 O12 90.6(3) . . ? N1 Pd2 Pd1 61.5(3) . . ? O9 Pd2 Pd1 78.43(14) . . ? O2 Pd2 Pd1 109.03(17) . . ? O12 Pd2 Pd1 126.43(16) . . ? N1 Pd2 Pd3 107.9(2) . . ? O9 Pd2 Pd3 112.68(14) . . ? O2 Pd2 Pd3 77.04(13) . . ? O12 Pd2 Pd3 78.90(14) . . ? Pd1 Pd2 Pd3 59.339(14) . . ? O1 Pd3 O11 91.3(2) . . ? O1 Pd3 O6 171.38(19) . . ? O11 Pd3 O6 87.9(2) . . ? O1 Pd3 O3 85.8(2) . . ? O11 Pd3 O3 163.1(2) . . ? O6 Pd3 O3 92.4(2) . . ? O1 Pd3 Pd1 111.76(14) . . ? O11 Pd3 Pd1 121.55(16) . . ? O6 Pd3 Pd1 75.77(15) . . ? O3 Pd3 Pd1 74.76(13) . . ? O1 Pd3 Pd2 77.24(12) . . ? O11 Pd3 Pd2 75.93(14) . . ? O6 Pd3 Pd2 110.85(15) . . ? O3 Pd3 Pd2 119.41(13) . . ? Pd1 Pd3 Pd2 59.73(2) . . ? C5 O6 Pd3 128.1(5) . . ? C1 O1 Pd3 129.6(4) . . ? C7 O9 Pd2 127.4(4) . . ? C5 O5 Pd1 124.5(4) . . ? C7 O10 Pd1 129.2(5) . . ? C9 O12 Pd2 126.7(5) . . ? C3 O3 Pd3 129.3(4) . . ? C9 O11 Pd3 131.6(5) . . ? C1 O2 Pd2 129.2(4) . . ? O11 C9 O12 126.0(7) . . ? O11 C9 C10 117.6(7) . . ? O12 C9 C10 116.4(7) . . ? O10 C7 O9 126.9(6) . . ? O10 C7 C8 117.8(6) . . ? O9 C7 C8 115.3(6) . . ? C3 O4 Pd1 124.4(5) . . ? O6 C5 O5 125.6(7) . . ? O6 C5 C6 117.8(7) . . ? O5 C5 C6 116.5(7) . . ? O4 C3 O3 125.9(7) . . ? O4 C3 C4 116.8(7) . . ? O3 C3 C4 117.3(7) . . ? N1 O7 Pd1 118.2(6) . . ? O7 N1 O8 117.2(8) . . ? O7 N1 Pd2 119.7(6) . . ? O8 N1 Pd2 123.2(8) . . ? O2 C1 O1 126.6(6) . . ? O2 C1 C2 116.4(6) . . ? O1 C1 C2 117.0(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.522 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.111 data_cmpd1 _database_code_depnum_ccdc_archive 'CCDC 262708' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Pd3(OAc)6CH2Cl2 _chemical_melting_point ? _chemical_formula_moiety Pd3(CH3CO2)6,CH2Cl2 _chemical_formula_sum 'C13 H20 Cl2 O12 Pd3' _chemical_formula_weight 758.39 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y-1/2, z' _cell_length_a 8.139(2) _cell_length_b 15.891(4) _cell_length_c 17.500(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2263.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 8579 _cell_measurement_theta_min 2.323 _cell_measurement_theta_max 27.509 _exptl_crystal_description orange _exptl_crystal_colour block _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 2.649 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5242 _exptl_absorpt_correction_T_max 0.6921 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Brucker SMART 1000' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13267 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0155 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.55 _reflns_number_total 2691 _reflns_number_gt 2467 _reflns_threshold_expression >2sigma(I) _computing_data_collection SAINT _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+3.1263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2691 _refine_ls_number_parameters 147 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0214 _refine_ls_wR_factor_ref 0.0583 _refine_ls_wR_factor_gt 0.0563 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.004 _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 0.64438(2) 0.098457(12) 0.158584(11) 0.02535(7) Uani 1 1 d . . . Pd2 Pd 0.79515(4) -0.054011(17) 0.2500 0.02745(8) Uani 1 2 d S . . O1 O 0.6541(3) -0.11048(14) 0.32830(14) 0.0487(6) Uani 1 1 d . . . O2 O 0.5517(3) -0.00253(13) 0.10590(12) 0.0460(5) Uani 1 1 d . . . O3 O 0.8620(3) 0.08226(15) 0.10789(13) 0.0457(6) Uani 1 1 d . . . O4 O 0.9665(3) -0.02383(15) 0.32615(14) 0.0509(6) Uani 1 1 d . . . O5 O 0.7219(3) 0.21323(13) 0.18654(12) 0.0453(5) Uani 1 1 d . . . O6 O 0.4154(3) 0.13070(17) 0.18660(12) 0.0474(5) Uani 1 1 d . . . C1 C 0.5738(4) -0.07925(18) 0.38152(16) 0.0324(6) Uani 1 1 d . . . C2 C 0.9731(3) 0.03073(17) 0.12316(14) 0.0292(5) Uani 1 1 d . . . C3 C 0.3514(5) 0.1441(2) 0.2500 0.0301(8) Uani 1 2 d S . . C4 C 0.7382(5) 0.2479(2) 0.2500 0.0303(8) Uani 1 2 d S . . C10 C 0.4951(5) -0.1402(2) 0.43638(19) 0.0472(8) Uani 1 1 d . . . H10A H 0.4356 -0.1093 0.4753 0.071 Uiso 1 1 calc R . . H10B H 0.5795 -0.1743 0.4603 0.071 Uiso 1 1 calc R . . H10C H 0.4196 -0.1764 0.4088 0.071 Uiso 1 1 calc R . . C20 C 1.1284(3) 0.0335(2) 0.07680(18) 0.0408(7) Uani 1 1 d . . . H20A H 1.2035 -0.0095 0.0948 0.061 Uiso 1 1 calc R . . H20B H 1.1794 0.0884 0.0822 0.061 Uiso 1 1 calc R . . H20C H 1.1027 0.0236 0.0234 0.061 Uiso 1 1 calc R . . C30 C 0.1817(5) 0.1818(3) 0.2500 0.0444(10) Uani 1 2 d S . . H30A H 0.1446 0.1891 0.3023 0.067 Uiso 0.50 1 calc PR . . H30B H 0.1069 0.1446 0.2232 0.067 Uiso 0.50 1 calc PR . . H30C H 0.1843 0.2360 0.2245 0.067 Uiso 0.50 1 calc PR . . C40 C 0.7770(6) 0.3402(3) 0.2500 0.0425(10) Uani 1 2 d S . . H40A H 0.7872 0.3599 0.3023 0.064 Uiso 0.50 1 calc PR . . H40B H 0.6894 0.3707 0.2246 0.064 Uiso 0.50 1 calc PR . . H40C H 0.8796 0.3497 0.2231 0.064 Uiso 0.50 1 calc PR . . Cl1 Cl 0.04147(18) 0.29972(7) 0.43098(5) 0.0784(4) Uani 1 1 d . . . C1S C -0.0764(7) 0.2500 0.5000 0.0471(11) Uani 1 2 d SD . . H1SA H -0.143(4) 0.2925(19) 0.5257(19) 0.056 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.02587(11) 0.02414(11) 0.02603(11) -0.00085(7) -0.00063(7) 0.00126(7) Pd2 0.03326(16) 0.02398(14) 0.02510(14) 0.000 0.000 0.00308(11) O1 0.0686(17) 0.0288(10) 0.0487(13) 0.0068(9) 0.0206(12) 0.0005(10) O2 0.0631(15) 0.0326(10) 0.0424(11) -0.0041(9) -0.0196(11) -0.0053(10) O3 0.0360(12) 0.0559(13) 0.0452(12) 0.0204(11) 0.0118(10) 0.0134(10) O4 0.0459(14) 0.0505(13) 0.0562(13) -0.0215(11) -0.0199(11) 0.0183(11) O5 0.0695(16) 0.0279(10) 0.0384(11) 0.0019(8) -0.0068(11) -0.0124(10) O6 0.0317(11) 0.0745(16) 0.0361(11) -0.0020(11) -0.0012(9) 0.0141(11) C1 0.0302(14) 0.0339(13) 0.0330(13) 0.0063(11) -0.0020(11) -0.0050(11) C2 0.0288(13) 0.0322(12) 0.0267(12) -0.0046(10) -0.0006(10) -0.0022(11) C3 0.0238(18) 0.0256(17) 0.041(2) 0.000 0.000 -0.0013(14) C4 0.0271(18) 0.0270(17) 0.0369(19) 0.000 0.000 -0.0018(15) C10 0.054(2) 0.0423(16) 0.0457(17) 0.0143(14) 0.0075(15) -0.0127(15) C20 0.0292(15) 0.0526(18) 0.0405(16) 0.0021(14) 0.0048(12) 0.0008(13) C30 0.030(2) 0.054(3) 0.048(2) 0.000 0.000 0.012(2) C40 0.051(3) 0.0277(19) 0.049(2) 0.000 0.000 -0.0126(19) Cl1 0.1283(11) 0.0670(6) 0.0399(4) 0.0038(4) -0.0009(6) -0.0388(7) C1S 0.056(3) 0.041(2) 0.044(2) -0.0095(19) 0.000 0.000 _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 O5 1.991(2) . ? Pd1 O6 1.994(2) . ? Pd1 O3 1.998(2) . ? Pd1 O2 1.999(2) . ? Pd1 Pd2 3.1520(6) . ? Pd1 Pd1 3.1995(9) 6_556 ? Pd2 O4 1.988(2) . ? Pd2 O4 1.988(2) 6_556 ? Pd2 O1 2.000(2) . ? Pd2 O1 2.000(2) 6_556 ? Pd2 Pd1 3.1521(6) 6_556 ? O1 C1 1.241(4) . ? O2 C1 1.252(3) 6_556 ? O3 C2 1.249(3) . ? O4 C2 1.242(3) 6_556 ? O5 C4 1.247(3) . ? O6 C3 1.244(3) . ? C1 O2 1.252(3) 6_556 ? C1 C10 1.507(4) . ? C2 O4 1.242(3) 6_556 ? C2 C20 1.503(4) . ? C3 O6 1.244(3) 6_556 ? C3 C30 1.506(5) . ? C4 O5 1.247(3) 6_556 ? C4 C40 1.501(5) . ? Cl1 C1S 1.733(3) . ? C1S Cl1 1.733(3) 4_556 ? 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 O5 Pd1 O6 90.01(11) . . ? O5 Pd1 O3 86.92(11) . . ? O6 Pd1 O3 166.17(9) . . ? O5 Pd1 O2 165.59(9) . . ? O6 Pd1 O2 88.12(10) . . ? O3 Pd1 O2 91.50(11) . . ? O5 Pd1 Pd2 117.14(7) . . ? O6 Pd1 Pd2 115.89(7) . . ? O3 Pd1 Pd2 77.36(6) . . ? O2 Pd1 Pd2 76.34(6) . . ? O5 Pd1 Pd1 75.77(6) . 6_556 ? O6 Pd1 Pd1 75.76(6) . 6_556 ? O3 Pd1 Pd1 116.36(7) . 6_556 ? O2 Pd1 Pd1 117.47(6) . 6_556 ? Pd2 Pd1 Pd1 59.501(10) . 6_556 ? O4 Pd2 O4 84.19(16) . 6_556 ? O4 Pd2 O1 92.97(12) . . ? O4 Pd2 O1 165.99(9) 6_556 . ? O4 Pd2 O1 165.99(9) . 6_556 ? O4 Pd2 O1 92.97(12) 6_556 6_556 ? O1 Pd2 O1 86.48(15) . 6_556 ? O4 Pd2 Pd1 115.34(7) . . ? O4 Pd2 Pd1 75.37(6) 6_556 . ? O1 Pd2 Pd1 117.97(7) . . ? O1 Pd2 Pd1 76.92(7) 6_556 . ? O4 Pd2 Pd1 75.38(6) . 6_556 ? O4 Pd2 Pd1 115.34(7) 6_556 6_556 ? O1 Pd2 Pd1 76.92(7) . 6_556 ? O1 Pd2 Pd1 117.97(7) 6_556 6_556 ? Pd1 Pd2 Pd1 61.00(2) . 6_556 ? C1 O1 Pd2 129.55(19) . . ? C1 O2 Pd1 130.3(2) 6_556 . ? C2 O3 Pd1 129.15(19) . . ? C2 O4 Pd2 132.6(2) 6_556 . ? C4 O5 Pd1 131.1(2) . . ? C3 O6 Pd1 130.9(2) . . ? O1 C1 O2 126.6(3) . 6_556 ? O1 C1 C10 116.4(3) . . ? O2 C1 C10 117.0(3) 6_556 . ? O4 C2 O3 125.4(3) 6_556 . ? O4 C2 C20 116.3(3) 6_556 . ? O3 C2 C20 118.3(2) . . ? O6 C3 O6 126.2(4) . 6_556 ? O6 C3 C30 116.91(18) . . ? O6 C3 C30 116.91(18) 6_556 . ? O5 C4 O5 125.9(4) 6_556 . ? O5 C4 C40 117.03(18) 6_556 . ? O5 C4 C40 117.03(18) . . ? Cl1 C1S Cl1 112.8(3) 4_556 . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.564 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.080 # === end of compound 1 ===