Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_page_first ? _journal_volume ? _journal_year ? _publ_contact_author_address ; School of Chemistry University of Birmingham Edgbaston Birmingham B15 2TT UK ; _publ_contact_author_email L.CRONIN@BHAM.AC.UK _publ_contact_author_name 'Dr L Cronin' _publ_section_title ; Self-assembly of a twelve-component hexanuclear metallomacrocycle constructured with a novel tri-amino ligand ; loop_ _publ_author_name G.Seeber D.-L.Long B.Kariuki L.Cronin data_6 _database_code_CSD 184117 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 7 [Pd{Pd(L)Cl2}Cl2] ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C12 H30 Cl6 N6 Pd3)' _chemical_formula_sum 'C12 H30 Cl6 N6 Pd3' _chemical_formula_weight 790.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 15.5544(9) _cell_length_b 9.6173(5) _cell_length_c 17.1240(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(4) _cell_angle_gamma 90.00 _cell_volume 2561.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2140 _cell_measurement_theta_min 5.2 _cell_measurement_theta_max 70.7 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.049 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 22.670 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART AXS' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5038 _diffrn_reflns_av_R_equivalents 0.1149 _diffrn_reflns_av_sigmaI/netI 0.2165 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 5.17 _diffrn_reflns_theta_max 70.69 _reflns_number_total 2140 _reflns_number_gt 1650 _reflns_threshold_expression >2sigma(I) _computing_data_collection texray _computing_cell_refinement texray _computing_data_reduction texray _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2140 _refine_ls_number_parameters 123 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1031 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2351 _refine_ls_wR_factor_gt 0.2145 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5774(8) -0.0158(13) 0.2327(7) 0.032(3) Uani 1 1 d . . . H1 H 0.5381 -0.0285 0.2768 0.038 Uiso 1 1 calc R . . C2 C 0.5340(9) 0.0852(15) 0.1741(8) 0.042(3) Uani 1 1 d . . . H2C H 0.4758 0.0539 0.1637 0.050 Uiso 1 1 calc R . . H2D H 0.5307 0.1771 0.1972 0.050 Uiso 1 1 calc R . . C3 C 0.5833(9) 0.0932(13) 0.0982(8) 0.035(3) Uani 1 1 d . . . H3 H 0.5466 0.1436 0.0613 0.042 Uiso 1 1 calc R . . C4 C 0.6016(10) -0.0490(14) 0.0616(7) 0.040(3) Uani 1 1 d . . . H4A H 0.6389 -0.0369 0.0167 0.048 Uiso 1 1 calc R . . H4B H 0.5480 -0.0892 0.0434 0.048 Uiso 1 1 calc R . . C5 C 0.6445(9) -0.1499(13) 0.1198(7) 0.033(3) Uani 1 1 d . . . H5 H 0.7018 -0.1144 0.1328 0.040 Uiso 1 1 calc R . . C6 C 0.5913(10) -0.1582(15) 0.1946(7) 0.041(3) Uani 1 1 d . . . H6A H 0.6202 -0.2189 0.2314 0.049 Uiso 1 1 calc R . . H6B H 0.5358 -0.1990 0.1826 0.049 Uiso 1 1 calc R . . N1 N 0.6561(7) 0.0470(12) 0.2625(6) 0.035(2) Uani 1 1 d . . . H1A H 0.6798 -0.0145 0.2958 0.042 Uiso 1 1 calc R . . H1B H 0.6405 0.1214 0.2910 0.042 Uiso 1 1 calc R . . N2 N 0.6623(7) 0.1759(10) 0.1071(6) 0.030(2) Uani 1 1 d . . . H2A H 0.6468 0.2634 0.1193 0.036 Uiso 1 1 calc R . . H2B H 0.6886 0.1792 0.0604 0.036 Uiso 1 1 calc R . . N3 N 0.6538(8) -0.2891(11) 0.0830(6) 0.037(3) Uani 1 1 d . . . H3A H 0.6037 -0.3130 0.0604 0.045 Uiso 1 1 calc R . . H3B H 0.6656 -0.3523 0.1202 0.045 Uiso 1 1 calc R . . Cl1 Cl 0.8505(2) 0.0428(3) 0.28256(19) 0.0385(8) Uani 1 1 d . . . Cl2 Cl 0.8554(2) 0.1898(4) 0.10256(19) 0.0446(8) Uani 1 1 d . . . Cl3 Cl 0.8527(3) -0.2989(4) 0.09670(19) 0.0530(10) Uani 1 1 d . . . Pd1 Pd 0.75122(6) 0.11076(8) 0.18853(5) 0.0281(4) Uani 1 1 d . . . Pd2 Pd 0.7500 -0.29323(13) 0.0000 0.0330(5) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(7) 0.045(7) 0.027(5) 0.001(5) 0.001(5) -0.002(5) C2 0.028(8) 0.053(8) 0.045(7) -0.005(7) -0.010(6) 0.012(6) C3 0.025(7) 0.038(7) 0.043(7) 0.017(6) -0.007(6) -0.001(5) C4 0.048(9) 0.048(8) 0.023(5) -0.009(5) -0.009(6) -0.004(6) C5 0.037(8) 0.037(6) 0.026(5) -0.009(5) -0.013(6) -0.009(5) C6 0.042(8) 0.052(8) 0.028(6) -0.001(6) -0.007(6) -0.010(7) N1 0.021(6) 0.053(7) 0.031(5) 0.007(5) -0.005(5) -0.005(5) N2 0.029(6) 0.034(5) 0.026(4) 0.003(4) 0.005(4) -0.006(4) N3 0.039(7) 0.041(6) 0.031(5) 0.004(4) -0.008(5) -0.010(5) Cl1 0.0269(17) 0.0451(17) 0.0436(16) 0.0011(13) -0.0094(14) 0.0038(12) Cl2 0.0322(19) 0.062(2) 0.0401(16) -0.0019(15) 0.0095(15) -0.0057(14) Cl3 0.047(2) 0.080(3) 0.0316(16) 0.0122(16) -0.0169(16) -0.0060(17) Pd1 0.0214(6) 0.0360(6) 0.0268(5) -0.0039(3) -0.0039(4) -0.0007(3) Pd2 0.0361(9) 0.0388(8) 0.0241(6) 0.000 -0.0070(6) 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 C1 N1 1.457(16) . ? C1 C6 1.53(2) . ? C1 C2 1.551(18) . ? C2 C3 1.51(2) . ? C3 N2 1.471(16) . ? C3 C4 1.531(19) . ? C4 C5 1.544(18) . ? C5 N3 1.487(17) . ? C5 C6 1.526(18) . ? N1 Pd1 2.042(11) . ? N2 Pd1 2.061(10) . ? N3 Pd2 2.063(12) . ? Cl1 Pd1 2.325(3) . ? Cl2 Pd1 2.318(3) . ? Cl3 Pd2 2.302(3) . ? Pd2 N3 2.063(12) 2_655 ? Pd2 Cl3 2.302(3) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C6 113.7(11) . . ? N1 C1 C2 109.4(11) . . ? C6 C1 C2 110.2(10) . . ? C3 C2 C1 111.5(11) . . ? N2 C3 C2 111.2(11) . . ? N2 C3 C4 111.7(11) . . ? C2 C3 C4 113.6(11) . . ? C3 C4 C5 112.2(10) . . ? N3 C5 C6 111.2(11) . . ? N3 C5 C4 109.5(9) . . ? C6 C5 C4 109.9(12) . . ? C5 C6 C1 112.8(12) . . ? C1 N1 Pd1 121.0(8) . . ? C3 N2 Pd1 117.8(7) . . ? C5 N3 Pd2 112.3(8) . . ? N1 Pd1 N2 91.4(4) . . ? N1 Pd1 Cl2 177.7(3) . . ? N2 Pd1 Cl2 86.6(3) . . ? N1 Pd1 Cl1 88.1(3) . . ? N2 Pd1 Cl1 178.3(3) . . ? Cl2 Pd1 Cl1 93.87(13) . . ? N3 Pd2 N3 177.8(6) 2_655 . ? N3 Pd2 Cl3 89.6(3) 2_655 . ? N3 Pd2 Cl3 90.5(3) . . ? N3 Pd2 Cl3 90.5(3) 2_655 2_655 ? N3 Pd2 Cl3 89.6(3) . 2_655 ? Cl3 Pd2 Cl3 177.3(2) . 2_655 ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 70.69 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 1.839 _refine_diff_density_min -1.688 _refine_diff_density_rms 0.293 data_1 _database_code_CSD 214307 _chemical_name_common 'Complex 1 (Pd(LH)Cl2)Cl' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 1 [Pd(LH)Cl2]Cl ; _chemical_melting_point ? _chemical_formula_moiety '(C6 H16 Cl2 N3 Pd +), (Cl -), (H2 O)' _chemical_formula_sum 'C6 H18 Cl3 N3 O Pd' _chemical_formula_weight 360.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbc21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y+1/2, z' 'x, -y+1/2, z+1/2' _cell_length_a 12.44450(10) _cell_length_b 12.20510(10) _cell_length_c 8.32130(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1263.89(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1904 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 70.7 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 17.500 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART AXS' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5508 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0579 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 70.71 _reflns_number_total 1904 _reflns_number_gt 1735 _reflns_threshold_expression >2sigma(I) _computing_data_collection texray _computing_cell_refinement texray _computing_data_reduction texray _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0728P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.14(2) _refine_ls_number_reflns 1904 _refine_ls_number_parameters 134 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0459 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.1082 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8184(5) 0.0829(5) 0.9445(9) 0.0252(17) Uani 1 1 d . . . H1 H 0.8356 0.1547 0.8985 0.030 Uiso 1 1 calc R . . C2 C 0.7187(6) 0.0410(6) 0.8614(9) 0.0293(15) Uani 1 1 d . . . H2C H 0.7357 0.0252 0.7501 0.035 Uiso 1 1 calc R . . H2D H 0.6644 0.0981 0.8626 0.035 Uiso 1 1 calc R . . C3 C 0.6721(5) -0.0628(5) 0.9400(8) 0.0234(17) Uani 1 1 d . . . H3 H 0.6019 -0.0772 0.8911 0.028 Uiso 1 1 calc R . . C4 C 0.6554(6) -0.0489(6) 1.1199(9) 0.0258(15) Uani 1 1 d . . . H4A H 0.6371 -0.1195 1.1659 0.031 Uiso 1 1 calc R . . H4B H 0.5949 -0.0002 1.1373 0.031 Uiso 1 1 calc R . . C5 C 0.7535(6) -0.0030(6) 1.2086(9) 0.0257(14) Uani 1 1 d . . . H5 H 0.8086 -0.0601 1.2151 0.031 Uiso 1 1 calc R . . C6 C 0.8016(6) 0.0983(6) 1.1248(9) 0.0267(15) Uani 1 1 d . . . H6A H 0.7541 0.1603 1.1419 0.032 Uiso 1 1 calc R . . H6B H 0.8701 0.1155 1.1742 0.032 Uiso 1 1 calc R . . Cl1 Cl 0.88543(15) -0.33766(13) 1.0447(3) 0.0299(4) Uani 1 1 d . . . Cl2 Cl 1.07758(15) -0.14499(13) 1.0586(3) 0.0280(4) Uani 1 1 d . . . Cl3 Cl 0.57734(17) -0.34742(13) 1.0483(3) 0.0339(4) Uani 1 1 d . . . Pd1 Pd 0.90026(3) -0.15382(3) 0.97580(4) 0.02075(18) Uani 1 1 d . . . N1 N 0.9116(4) 0.0074(5) 0.9107(10) 0.0263(13) Uani 1 1 d . . . H1A H 0.9698 0.0355 0.9598 0.032 Uiso 1 1 calc R . . H1B H 0.9245 0.0097 0.8043 0.032 Uiso 1 1 calc R . . N2 N 0.7426(5) -0.1581(4) 0.9059(9) 0.0251(12) Uani 1 1 d . . . H2A H 0.7415 -0.1694 0.7990 0.030 Uiso 1 1 calc R . . H2B H 0.7124 -0.2173 0.9520 0.030 Uiso 1 1 calc R . . N3 N 0.7214(5) 0.0285(5) 1.3733(7) 0.0284(13) Uani 1 1 d . . . H3A H 0.7783 0.0542 1.4260 0.043 Uiso 1 1 calc R . . H3B H 0.6955 -0.0298 1.4245 0.043 Uiso 1 1 calc R . . H3C H 0.6710 0.0802 1.3685 0.043 Uiso 1 1 calc R . . O1 O 0.5790(5) 0.2034(6) 1.3349(10) 0.0486(16) Uani 1 1 d D . . H20 H 0.547(8) 0.203(9) 1.243(6) 0.073 Uiso 1 1 d D . . H21 H 0.540(7) 0.250(7) 1.387(10) 0.073 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 C1 0.031(3) 0.018(3) 0.027(5) 0.004(3) -0.002(3) 0.000(2) C2 0.029(4) 0.032(4) 0.026(4) 0.003(3) -0.001(3) 0.002(3) C3 0.020(3) 0.022(3) 0.028(5) -0.001(3) -0.007(3) 0.000(2) C4 0.023(3) 0.022(3) 0.033(4) -0.005(3) 0.005(3) -0.001(3) C5 0.026(3) 0.027(4) 0.024(3) 0.001(2) -0.002(3) -0.003(3) C6 0.028(3) 0.024(3) 0.028(4) -0.004(3) 0.005(3) -0.005(3) Cl1 0.0289(8) 0.0174(8) 0.0434(11) 0.0044(7) 0.0035(8) 0.0016(5) Cl2 0.0216(7) 0.0275(8) 0.0349(10) 0.0011(7) -0.0024(8) 0.0000(6) Cl3 0.0314(8) 0.0338(10) 0.0364(11) 0.0012(8) 0.0050(9) 0.0002(6) Pd1 0.0204(3) 0.0182(3) 0.0236(3) 0.0001(3) 0.0010(2) -0.00009(13) N1 0.025(3) 0.023(3) 0.031(4) 0.001(3) 0.001(2) -0.002(2) N2 0.028(3) 0.025(3) 0.022(3) -0.003(2) 0.002(3) -0.003(2) N3 0.033(3) 0.029(3) 0.023(3) -0.001(3) 0.001(2) -0.002(2) O1 0.035(3) 0.050(4) 0.061(4) -0.014(3) -0.003(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.508(8) . ? C1 C2 1.510(10) . ? C1 C6 1.526(10) . ? C2 C3 1.539(9) . ? C3 N2 1.485(8) . ? C3 C4 1.520(10) . ? C4 C5 1.533(10) . ? C5 N3 1.478(10) . ? C5 C6 1.540(10) . ? Cl1 Pd1 2.3232(16) . ? Cl2 Pd1 2.3142(19) . ? Pd1 N1 2.046(6) . ? Pd1 N2 2.047(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 109.9(5) . . ? N1 C1 C6 111.3(6) . . ? C2 C1 C6 112.3(6) . . ? C1 C2 C3 113.2(6) . . ? N2 C3 C4 110.9(6) . . ? N2 C3 C2 110.0(5) . . ? C4 C3 C2 112.2(5) . . ? C3 C4 C5 114.0(6) . . ? N3 C5 C4 109.1(6) . . ? N3 C5 C6 108.4(6) . . ? C4 C5 C6 112.6(6) . . ? C1 C6 C5 113.6(6) . . ? N1 Pd1 N2 90.9(2) . . ? N1 Pd1 Cl2 88.18(16) . . ? N2 Pd1 Cl2 178.55(18) . . ? N1 Pd1 Cl1 178.8(2) . . ? N2 Pd1 Cl1 88.24(16) . . ? Cl2 Pd1 Cl1 92.70(6) . . ? C1 N1 Pd1 119.0(4) . . ? C3 N2 Pd1 119.5(4) . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 70.71 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 2.710 _refine_diff_density_min -1.893 _refine_diff_density_rms 0.161 data_2 _database_code_CSD 214308 _chemical_name_common 'Complex 2 (Pd(LH)Br2)Br' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 2 [Pd(LH)Br2]Br ; _chemical_melting_point ? _chemical_formula_moiety '2(C6 H16 Br2 N3 Pd +), (Pd Br4 2-), 2(H2 O)' _chemical_formula_sum 'C12 H36 Br8 N6 O2 Pd3' _chemical_formula_weight 1254.95 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8314(4) _cell_length_b 8.8782(3) _cell_length_c 11.5103(6) _cell_angle_alpha 69.095(2) _cell_angle_beta 76.249(2) _cell_angle_gamma 60.895(2) _cell_volume 734.35(6) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3371 _cell_measurement_theta_min 1.9 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.838 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 12.722 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.174 _exptl_absorpt_correction_T_max 0.492 _exptl_absorpt_process_details ; P. Coppens, L. Leiserowitz, D Rabinovich, Acta Cryst. (1965), 18, 1035-1038 ; _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 'Nonius Kappa-CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18770 _diffrn_reflns_av_R_equivalents 0.1237 _diffrn_reflns_av_sigmaI/netI 0.0474 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3371 _reflns_number_gt 2978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0641P)^2^+4.4332P] 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 SHELXL _refine_ls_extinction_coef 0.0023(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3371 _refine_ls_number_parameters 149 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0513 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1189 _refine_ls_wR_factor_gt 0.1155 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6256(9) 0.0521(9) 0.6147(6) 0.0179(13) Uani 1 1 d . . . H1 H 0.5788 0.1065 0.5327 0.022 Uiso 1 1 calc R . . C2 C 0.8192(9) 0.0065(9) 0.5932(6) 0.0185(13) Uani 1 1 d . . . H2A H 0.8714 -0.0528 0.5276 0.022 Uiso 1 1 calc R . . H2B H 0.8310 0.1174 0.5646 0.022 Uiso 1 1 calc R . . C3 C 0.9186(8) -0.1141(9) 0.7090(7) 0.0176(13) Uani 1 1 d . . . H3 H 1.0427 -0.1515 0.6837 0.021 Uiso 1 1 calc R . . C4 C 0.8910(9) -0.2833(9) 0.7668(6) 0.0178(13) Uani 1 1 d . . . H4A H 0.9436 -0.3578 0.7104 0.021 Uiso 1 1 calc R . . H4B H 0.9480 -0.3514 0.8440 0.021 Uiso 1 1 calc R . . C5 C 0.6988(9) -0.2376(9) 0.7934(6) 0.0168(13) Uani 1 1 d . . . H5 H 0.6492 -0.1764 0.8590 0.020 Uiso 1 1 calc R . . C6 C 0.5992(8) -0.1174(9) 0.6772(7) 0.0183(13) Uani 1 1 d . . . H6A H 0.6361 -0.1856 0.6177 0.022 Uiso 1 1 calc R . . H6B H 0.4762 -0.0829 0.7001 0.022 Uiso 1 1 calc R . . N1 N 0.5294(8) 0.1868(8) 0.6859(5) 0.0181(11) Uani 1 1 d . . . H1A H 0.4239 0.1890 0.7105 0.022 Uiso 1 1 calc R . . H1B H 0.5122 0.2947 0.6314 0.022 Uiso 1 1 calc R . . N2 N 0.8706(7) -0.0158(8) 0.8037(6) 0.0180(11) Uani 1 1 d . . . H2C H 0.9387 0.0406 0.7834 0.022 Uiso 1 1 calc R . . H2D H 0.9032 -0.1002 0.8770 0.022 Uiso 1 1 calc R . . N3 N 0.6802(8) -0.4093(8) 0.8375(6) 0.0209(12) Uani 1 1 d . . . H3A H 0.5681 -0.3842 0.8537 0.031 Uiso 1 1 calc R . . H3B H 0.7355 -0.4797 0.9065 0.031 Uiso 1 1 calc R . . H3C H 0.7261 -0.4657 0.7784 0.031 Uiso 1 1 calc R . . Br1 Br 0.71892(9) 0.15701(10) 1.02419(6) 0.02136(19) Uani 1 1 d . . . Br2 Br 0.34297(9) 0.42625(10) 0.86097(7) 0.02332(19) Uani 1 1 d . . . Br3 Br 0.12691(9) 0.21639(9) 0.66162(6) 0.02051(18) Uani 1 1 d . . . Br4 Br -0.28048(8) 0.49273(9) 0.56051(6) 0.01940(18) Uani 1 1 d . . . Pd1 Pd 0.62152(6) 0.17058(6) 0.83847(5) 0.01448(16) Uani 1 1 d . . . Pd2 Pd 0.0000 0.5000 0.5000 0.01414(18) Uani 1 2 d S . . O1 O 0.9802(7) -0.3036(7) 1.0498(5) 0.0278(12) Uani 1 1 d D . . H11 H 0.901(9) -0.336(13) 1.087(7) 0.042 Uiso 1 1 d D . . H12 H 0.991(12) -0.256(13) 1.098(7) 0.042 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 C1 0.019(3) 0.014(3) 0.019(3) -0.003(2) -0.003(3) -0.007(3) C2 0.024(3) 0.023(3) 0.012(3) -0.009(3) 0.009(2) -0.015(3) C3 0.007(3) 0.020(3) 0.025(3) -0.008(3) 0.002(2) -0.006(2) C4 0.018(3) 0.015(3) 0.018(3) -0.001(3) -0.005(2) -0.006(3) C5 0.022(3) 0.012(3) 0.018(3) -0.004(2) -0.002(3) -0.009(3) C6 0.013(3) 0.014(3) 0.025(3) -0.002(3) -0.004(3) -0.005(2) N1 0.021(3) 0.017(3) 0.016(3) -0.002(2) -0.002(2) -0.009(2) N2 0.014(3) 0.015(3) 0.026(3) -0.007(2) -0.003(2) -0.007(2) N3 0.023(3) 0.019(3) 0.022(3) -0.001(2) -0.004(2) -0.012(2) Br1 0.0195(3) 0.0250(4) 0.0206(3) -0.0072(3) -0.0026(3) -0.0097(3) Br2 0.0174(3) 0.0227(4) 0.0262(4) -0.0097(3) -0.0022(3) -0.0040(3) Br3 0.0196(3) 0.0187(3) 0.0203(3) 0.0032(3) -0.0047(3) -0.0109(3) Br4 0.0178(3) 0.0171(3) 0.0230(4) -0.0008(3) -0.0017(2) -0.0108(3) Pd1 0.0142(3) 0.0137(3) 0.0155(3) -0.00238(19) -0.00096(18) -0.00750(19) Pd2 0.0157(3) 0.0133(3) 0.0134(3) -0.0012(3) -0.0010(2) -0.0082(3) O1 0.032(3) 0.022(3) 0.029(3) -0.003(2) -0.003(2) -0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.485(9) . ? C1 C6 1.525(9) . ? C1 C2 1.532(9) . ? C2 C3 1.522(10) . ? C3 N2 1.493(9) . ? C3 C4 1.524(9) . ? C4 C5 1.520(9) . ? C5 N3 1.503(8) . ? C5 C6 1.527(9) . ? N1 Pd1 2.037(6) . ? N2 Pd1 2.061(6) . ? Br1 Pd1 2.4319(8) . ? Br2 Pd1 2.4404(8) . ? Br3 Pd2 2.4413(7) . ? Br4 Pd2 2.4348(6) . ? Pd2 Br4 2.4348(6) 2_566 ? Pd2 Br3 2.4413(7) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C6 112.0(6) . . ? N1 C1 C2 111.1(5) . . ? C6 C1 C2 111.0(5) . . ? C3 C2 C1 113.6(5) . . ? N2 C3 C2 111.5(5) . . ? N2 C3 C4 110.1(6) . . ? C2 C3 C4 111.8(5) . . ? C5 C4 C3 111.4(5) . . ? N3 C5 C4 108.7(5) . . ? N3 C5 C6 108.5(5) . . ? C4 C5 C6 111.8(5) . . ? C1 C6 C5 113.4(5) . . ? C1 N1 Pd1 122.4(4) . . ? C3 N2 Pd1 123.4(4) . . ? N1 Pd1 N2 94.7(2) . . ? N1 Pd1 Br1 177.59(17) . . ? N2 Pd1 Br1 87.64(16) . . ? N1 Pd1 Br2 85.73(16) . . ? N2 Pd1 Br2 171.06(16) . . ? Br1 Pd1 Br2 92.11(3) . . ? Br4 Pd2 Br4 180.00(3) 2_566 . ? Br4 Pd2 Br3 90.98(2) 2_566 . ? Br4 Pd2 Br3 89.02(2) . . ? Br4 Pd2 Br3 89.02(2) 2_566 2_566 ? Br4 Pd2 Br3 90.98(2) . 2_566 ? Br3 Pd2 Br3 180.00(3) . 2_566 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.833 _refine_diff_density_min -1.866 _refine_diff_density_rms 0.276 data_3 _database_code_CSD 214309 _chemical_name_common 'Complex 3 (Pd(LH)2)(NO3)4' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 3 [Pd(LH)2](NO3)4 ; _chemical_melting_point ? _chemical_formula_moiety '(C12 H32 N6 Pd 4+), 4(N O3 -)' _chemical_formula_sum 'C12 H32 N10 O12 Pd' _chemical_formula_weight 614.88 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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3934(11) _cell_length_b 16.649(2) _cell_length_c 8.6914(11) _cell_angle_alpha 90.00 _cell_angle_beta 109.419(4) _cell_angle_gamma 90.00 _cell_volume 1145.5(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2026 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25.5 _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.783 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis Diffractometer' _diffrn_measurement_method 'Image plate detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6093 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0611 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 25.47 _reflns_number_total 2026 _reflns_number_gt 1796 _reflns_threshold_expression >2sigma(I) _computing_data_collection texray _computing_cell_refinement texray _computing_data_reduction texray _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+5.1164P] 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 SHELXL _refine_ls_extinction_coef 0.0021(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2026 _refine_ls_number_parameters 161 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0857 _refine_ls_wR_factor_ref 0.1240 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.333 _refine_ls_restrained_S_all 1.333 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1195(9) -0.0522(4) 0.3583(9) 0.0392(18) Uani 1 1 d . . . H1 H 0.1270 -0.0356 0.4686 0.047 Uiso 1 1 calc R . . C2 C 0.0097(10) -0.1264(5) 0.3157(10) 0.047(2) Uani 1 1 d . . . H2C H -0.1047 -0.1121 0.3077 0.057 Uiso 1 1 calc R . . H2D H 0.0507 -0.1653 0.4032 0.057 Uiso 1 1 calc R . . C3 C 0.0070(9) -0.1653(4) 0.1563(10) 0.0405(19) Uani 1 1 d . . . H3 H -0.0528 -0.2166 0.1458 0.049 Uiso 1 1 calc R . . C4 C 0.1859(9) -0.1826(4) 0.1562(9) 0.0384(18) Uani 1 1 d . . . H4A H 0.2336 -0.2261 0.2317 0.046 Uiso 1 1 calc R . . H4B H 0.1802 -0.2002 0.0481 0.046 Uiso 1 1 calc R . . C5 C 0.3018(8) -0.1103(4) 0.2037(9) 0.0351(17) Uani 1 1 d . . . H5 H 0.2664 -0.0713 0.1143 0.042 Uiso 1 1 calc R . . C6 C 0.2983(9) -0.0691(5) 0.3590(9) 0.0406(18) Uani 1 1 d . . . H6A H 0.3598 -0.0188 0.3720 0.049 Uiso 1 1 calc R . . H6B H 0.3556 -0.1029 0.4518 0.049 Uiso 1 1 calc R . . N1 N 0.0420(7) 0.0155(3) 0.2448(7) 0.0334(15) Uani 1 1 d . . . H1A H 0.1089 0.0588 0.2778 0.040 Uiso 1 1 calc R . . H1B H -0.0577 0.0273 0.2571 0.040 Uiso 1 1 calc R . . N2 N -0.0877(7) -0.1139(4) 0.0150(8) 0.0438(17) Uani 1 1 d . . . H2A H -0.1945 -0.1095 0.0152 0.053 Uiso 1 1 calc R . . H2B H -0.0921 -0.1402 -0.0767 0.053 Uiso 1 1 calc R . . N3 N 0.4790(7) -0.1355(4) 0.2255(8) 0.0408(16) Uani 1 1 d . . . H3A H 0.5470 -0.0930 0.2525 0.061 Uiso 1 1 calc R . . H3B H 0.4834 -0.1564 0.1327 0.061 Uiso 1 1 calc R . . H3C H 0.5122 -0.1722 0.3043 0.061 Uiso 1 1 calc R . . N4 N 0.6098(8) 0.0632(4) 0.1791(8) 0.0434(16) Uani 1 1 d . . . N5 N 0.6673(8) 0.7004(4) 0.1256(8) 0.0425(16) Uani 1 1 d . . . O1 O 0.6958(9) 0.1198(4) 0.1644(9) 0.073(2) Uani 1 1 d . . . O2 O 0.6844(6) 0.0025(4) 0.2550(7) 0.0559(14) Uani 1 1 d . . . O3 O 0.4558(7) 0.0636(4) 0.1225(9) 0.076(2) Uani 1 1 d . . . O4 O 0.7238(8) 0.6388(4) 0.0798(8) 0.0672(19) Uani 1 1 d . . . O5 O 0.5377(7) 0.7322(3) 0.0313(7) 0.0582(17) Uani 1 1 d . . . O6 O 0.7387(7) 0.7293(4) 0.2631(7) 0.0576(16) Uani 1 1 d . . . Pd Pd 0.0000 0.0000 0.0000 0.0322(3) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(4) 0.046(5) 0.027(4) -0.006(4) 0.007(3) 0.008(4) C2 0.042(5) 0.051(5) 0.050(5) 0.009(4) 0.016(4) 0.007(4) C3 0.036(4) 0.034(4) 0.049(5) 0.001(4) 0.012(4) -0.008(3) C4 0.039(4) 0.037(4) 0.038(4) -0.001(4) 0.010(4) 0.004(3) C5 0.024(3) 0.038(4) 0.038(4) -0.005(3) 0.003(3) 0.008(3) C6 0.033(4) 0.045(5) 0.038(4) -0.003(4) 0.005(3) 0.005(3) N1 0.029(3) 0.020(3) 0.045(3) -0.002(3) 0.005(3) 0.001(2) N2 0.028(3) 0.038(4) 0.055(4) -0.003(3) -0.001(3) -0.004(3) N3 0.036(3) 0.039(4) 0.046(4) -0.002(3) 0.012(3) 0.006(3) N4 0.040(4) 0.047(4) 0.043(4) -0.002(3) 0.014(3) 0.003(3) N5 0.042(4) 0.034(4) 0.049(4) 0.008(3) 0.012(3) 0.000(3) O1 0.077(5) 0.055(4) 0.095(6) 0.004(4) 0.040(4) -0.009(4) O2 0.043(3) 0.054(3) 0.061(3) 0.014(4) 0.005(3) 0.005(3) O3 0.039(4) 0.080(5) 0.100(5) 0.010(4) 0.011(4) 0.018(3) O4 0.078(4) 0.048(4) 0.072(4) 0.005(3) 0.021(4) 0.030(3) O5 0.055(4) 0.052(3) 0.048(4) -0.005(3) -0.009(3) 0.022(3) O6 0.054(4) 0.061(4) 0.045(4) -0.003(3) -0.001(3) -0.007(3) Pd 0.0260(4) 0.0314(4) 0.0343(4) -0.0034(5) 0.0033(3) -0.0002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.496(9) . ? C1 C2 1.513(10) . ? C1 C6 1.524(10) . ? C2 C3 1.522(11) . ? C3 N2 1.491(9) . ? C3 C4 1.530(10) . ? C4 C5 1.515(10) . ? C5 N3 1.496(8) . ? C5 C6 1.523(10) . ? N1 Pd 2.054(6) . ? N2 Pd 2.053(6) . ? N4 O1 1.220(8) . ? N4 O3 1.220(8) . ? N4 O2 1.254(8) . ? N5 O6 1.242(8) . ? N5 O5 1.242(7) . ? N5 O4 1.248(8) . ? Pd N2 2.053(6) 3 ? Pd N1 2.054(6) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.0(6) . . ? N1 C1 C6 110.7(6) . . ? C2 C1 C6 111.6(6) . . ? C1 C2 C3 113.2(7) . . ? N2 C3 C2 110.4(6) . . ? N2 C3 C4 111.2(6) . . ? C2 C3 C4 111.3(6) . . ? C5 C4 C3 113.1(6) . . ? N3 C5 C4 109.4(6) . . ? N3 C5 C6 109.0(6) . . ? C4 C5 C6 113.5(6) . . ? C5 C6 C1 112.9(6) . . ? C1 N1 Pd 118.4(4) . . ? C3 N2 Pd 118.5(4) . . ? O1 N4 O3 122.5(8) . . ? O1 N4 O2 117.9(7) . . ? O3 N4 O2 119.6(7) . . ? O6 N5 O5 120.4(7) . . ? O6 N5 O4 120.8(7) . . ? O5 N5 O4 118.8(7) . . ? N2 Pd N2 180.0(4) . 3 ? N2 Pd N1 90.5(2) . 3 ? N2 Pd N1 89.5(2) 3 3 ? N2 Pd N1 89.5(2) . . ? N2 Pd N1 90.5(2) 3 . ? N1 Pd N1 180.0(3) 3 . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.47 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.504 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.111 data_4 _database_code_CSD 214310 _chemical_name_common 'Complex 4 (Pd(LH)2)(SO4)2' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 4 [Pd(LH)2](SO4)2 ; _chemical_melting_point ? _chemical_formula_moiety '(C12 H32 N6 Pd 4+), 2(S O4 2-), 6(H2 O)' _chemical_formula_sum 'C12 H44 N6 O14 Pd S2' _chemical_formula_weight 667.05 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.2588(2) _cell_length_b 17.3414(4) _cell_length_c 9.1518(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.1200(10) _cell_angle_gamma 90.00 _cell_volume 1294.14(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 5618 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 35.0 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Kappa CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23350 _diffrn_reflns_av_R_equivalents 0.0527 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 35.05 _reflns_number_total 5618 _reflns_number_gt 4538 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor, 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX (Farrugia, 1999)' _computing_publication_material 'WinGX (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0279P)^2^+1.1423P] 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 5618 _refine_ls_number_parameters 178 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.03784(19) -0.13643(9) 0.21478(17) 0.0148(3) Uani 1 1 d . . . H1 H 0.0115 -0.1550 0.3129 0.018 Uiso 1 1 calc R . . C2 C 0.0263(2) -0.18733(10) 0.09991(18) 0.0177(3) Uani 1 1 d . . . H2C H 0.1419 -0.1766 0.1020 0.021 Uiso 1 1 calc R . . H2D H 0.0161 -0.2410 0.1272 0.021 Uiso 1 1 calc R . . C3 C -0.06366(19) -0.17545(10) -0.05745(17) 0.0152(3) Uani 1 1 d . . . H3 H -0.0304 -0.2170 -0.1191 0.018 Uiso 1 1 calc R . . C4 C -0.2495(2) -0.18066(10) -0.06408(17) 0.0166(3) Uani 1 1 d . . . H4A H -0.3029 -0.1673 -0.1630 0.020 Uiso 1 1 calc R . . H4B H -0.2790 -0.2334 -0.0445 0.020 Uiso 1 1 calc R . . C5 C -0.31156(19) -0.12716(10) 0.04768(17) 0.0145(3) Uani 1 1 d . . . H5 H -0.2908 -0.0736 0.0219 0.017 Uiso 1 1 calc R . . C6 C -0.22417(19) -0.14322(10) 0.20408(17) 0.0157(3) Uani 1 1 d . . . H6A H -0.2517 -0.1947 0.2333 0.019 Uiso 1 1 calc R . . H6B H -0.2619 -0.1069 0.2720 0.019 Uiso 1 1 calc R . . N1 N 0.01349(17) -0.05435(8) 0.20215(15) 0.0148(2) Uani 1 1 d . . . H1A H 0.1185 -0.0510 0.2469 0.018 Uiso 1 1 calc R . . H1B H -0.0462 -0.0260 0.2565 0.018 Uiso 1 1 calc R . . N2 N -0.01767(17) -0.10048(8) -0.12051(15) 0.0151(2) Uani 1 1 d . . . H2A H -0.0908 -0.0919 -0.2028 0.018 Uiso 1 1 calc R . . H2B H 0.0801 -0.1077 -0.1501 0.018 Uiso 1 1 calc R . . N3 N -0.49242(16) -0.13857(9) 0.03916(16) 0.0168(3) Uani 1 1 d . . . H3A H -0.5423 -0.1288 -0.0525 0.025 Uiso 1 1 calc R . . H3B H -0.5302 -0.1066 0.1020 0.025 Uiso 1 1 calc R . . H3C H -0.5123 -0.1871 0.0628 0.025 Uiso 1 1 calc R . . O1 O -0.92996(17) -0.54268(8) -0.28896(14) 0.0246(3) Uani 1 1 d . . . O2 O -0.92567(16) -0.61171(8) -0.05950(14) 0.0230(3) Uani 1 1 d . . . O3 O -0.75669(15) -0.65305(8) -0.23849(15) 0.0212(2) Uani 1 1 d . . . O4 O -0.68954(15) -0.53605(8) -0.09921(14) 0.0217(3) Uani 1 1 d . . . S1 S -0.82468(5) -0.58560(2) -0.17001(4) 0.01508(8) Uani 1 1 d . . . Pd1 Pd 0.0000 0.0000 0.0000 0.01150(4) Uani 1 2 d S . . O5 O -0.73930(16) -0.41618(8) 0.08848(14) 0.0205(2) Uani 1 1 d D . . H51 H -0.726(3) -0.4552(12) 0.038(3) 0.031 Uiso 1 1 d D . . H52 H -0.840(2) -0.4112(14) 0.084(3) 0.031 Uiso 1 1 d D . . O6 O -0.53335(18) -0.29366(8) 0.07203(16) 0.0257(3) Uani 1 1 d D . . H61 H -0.604(2) -0.3305(13) 0.069(3) 0.039 Uiso 1 1 d D . . H62 H -0.446(2) -0.3133(15) 0.113(3) 0.039 Uiso 1 1 d D . . O7 O -0.86755(16) -0.57201(8) 0.23034(14) 0.0205(2) Uani 1 1 d D . . H71 H -0.880(3) -0.5861(14) 0.1408(19) 0.031 Uiso 1 1 d D . . H72 H -0.920(3) -0.5312(11) 0.233(3) 0.031 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 C1 0.0163(7) 0.0153(7) 0.0125(6) 0.0031(5) 0.0013(5) -0.0011(5) C2 0.0164(7) 0.0159(7) 0.0206(7) 0.0026(6) 0.0020(6) 0.0020(6) C3 0.0170(7) 0.0135(7) 0.0161(7) -0.0013(5) 0.0052(5) -0.0007(5) C4 0.0169(7) 0.0190(8) 0.0148(6) -0.0026(6) 0.0050(5) -0.0045(6) C5 0.0144(6) 0.0157(7) 0.0140(6) 0.0008(5) 0.0037(5) -0.0014(5) C6 0.0168(7) 0.0177(7) 0.0130(6) 0.0007(5) 0.0040(5) -0.0018(6) N1 0.0147(6) 0.0154(6) 0.0141(6) 0.0008(5) 0.0018(5) -0.0017(5) N2 0.0159(6) 0.0155(6) 0.0146(6) -0.0005(5) 0.0051(5) -0.0017(5) N3 0.0155(6) 0.0200(7) 0.0151(5) 0.0005(5) 0.0025(5) 0.0003(5) O1 0.0291(7) 0.0249(7) 0.0182(6) -0.0015(5) -0.0014(5) 0.0053(5) O2 0.0197(6) 0.0313(7) 0.0191(6) -0.0027(5) 0.0071(5) -0.0052(5) O3 0.0200(6) 0.0187(6) 0.0261(6) -0.0067(5) 0.0075(5) 0.0007(5) O4 0.0191(6) 0.0223(7) 0.0239(6) -0.0071(5) 0.0038(5) -0.0056(5) S1 0.01386(16) 0.01677(18) 0.01502(16) -0.00303(13) 0.00355(13) -0.00108(13) Pd1 0.01162(7) 0.01225(7) 0.01076(7) 0.00020(6) 0.00223(5) -0.00133(6) O5 0.0184(6) 0.0228(6) 0.0207(6) -0.0038(5) 0.0040(5) -0.0038(5) O6 0.0233(6) 0.0217(7) 0.0310(7) 0.0048(5) 0.0008(5) -0.0049(5) O7 0.0196(6) 0.0243(7) 0.0174(5) 0.0015(5) 0.0025(4) 0.0024(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 C1 N1 1.495(2) . ? C1 C2 1.530(2) . ? C1 C6 1.531(2) . ? C2 C3 1.526(2) . ? C3 N2 1.496(2) . ? C3 C4 1.529(2) . ? C4 C5 1.528(2) . ? C5 N3 1.496(2) . ? C5 C6 1.523(2) . ? N1 Pd1 2.0635(13) . ? N2 Pd1 2.0550(14) . ? O1 S1 1.4816(14) . ? O2 S1 1.4802(13) . ? O3 S1 1.4790(13) . ? O4 S1 1.4746(13) . ? Pd1 N2 2.0550(14) 3 ? Pd1 N1 2.0635(13) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.27(12) . . ? N1 C1 C6 111.27(13) . . ? C2 C1 C6 111.45(13) . . ? C3 C2 C1 113.62(13) . . ? N2 C3 C2 111.47(13) . . ? N2 C3 C4 110.53(13) . . ? C2 C3 C4 111.41(13) . . ? C5 C4 C3 112.25(13) . . ? N3 C5 C6 110.19(12) . . ? N3 C5 C4 108.83(13) . . ? C6 C5 C4 111.01(14) . . ? C5 C6 C1 111.58(12) . . ? C1 N1 Pd1 121.91(10) . . ? C3 N2 Pd1 122.06(10) . . ? O4 S1 O3 109.59(8) . . ? O4 S1 O2 110.32(8) . . ? O3 S1 O2 109.91(8) . . ? O4 S1 O1 110.19(9) . . ? O3 S1 O1 107.69(8) . . ? O2 S1 O1 109.09(8) . . ? N2 Pd1 N2 180.00(10) . 3 ? N2 Pd1 N1 85.24(5) . 3 ? N2 Pd1 N1 94.76(5) 3 3 ? N2 Pd1 N1 94.76(5) . . ? N2 Pd1 N1 85.24(5) 3 . ? N1 Pd1 N1 180.00(10) 3 . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 35.05 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.712 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.112 data_5 _database_code_CSD 214311 _chemical_name_common 'Complex 6 (Pd(L)Br)6Br6' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Complex 6 [Pd(L)Br]6Br6 ; _chemical_melting_point ? _chemical_formula_moiety '(C36 H90 Br6 N18 Pd6 6+), 6(Br -), 20(H2 O)' _chemical_formula_sum 'C36 H130 Br12 N18 O20 Pd6' _chemical_formula_weight 2732.90 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4054(2) _cell_length_b 26.6675(5) _cell_length_c 12.8312(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.7010(10) _cell_angle_gamma 90.00 _cell_volume 4244.51(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8317 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2656 _exptl_absorpt_coefficient_mu 6.958 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 1.196 _exptl_absorpt_process_details ; R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Nonius Kappa-CCD' _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26763 _diffrn_reflns_av_R_equivalents 0.1146 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8317 _reflns_number_gt 6573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0415P)^2^+7.1163P] 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 8317 _refine_ls_number_parameters 475 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0919 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3127(4) 0.7866(2) 0.4626(4) 0.0138(12) Uani 1 1 d . . . H1 H 0.2522 0.7685 0.4934 0.017 Uiso 1 1 calc R . . C2 C 0.3617(4) 0.7534(2) 0.3806(4) 0.0158(12) Uani 1 1 d . . . H2A H 0.3103 0.7496 0.3236 0.019 Uiso 1 1 calc R . . H2B H 0.3743 0.7204 0.4104 0.019 Uiso 1 1 calc R . . C3 C 0.4670(4) 0.7732(2) 0.3375(4) 0.0154(12) Uani 1 1 d . . . H3 H 0.4986 0.7468 0.2942 0.019 Uiso 1 1 calc R . . C4 C 0.5472(4) 0.7852(2) 0.4260(4) 0.0167(13) Uani 1 1 d . . . H4A H 0.5699 0.7542 0.4591 0.020 Uiso 1 1 calc R . . H4B H 0.6105 0.8010 0.3970 0.020 Uiso 1 1 calc R . . C5 C 0.4991(4) 0.8197(2) 0.5078(4) 0.0148(12) Uani 1 1 d . . . H5 H 0.4828 0.8519 0.4744 0.018 Uiso 1 1 calc R . . C6 C 0.3940(4) 0.7983(2) 0.5494(4) 0.0145(12) Uani 1 1 d . . . H6A H 0.3625 0.8222 0.5972 0.017 Uiso 1 1 calc R . . H6B H 0.4095 0.7678 0.5881 0.017 Uiso 1 1 calc R . . C7 C 0.4861(4) 0.9326(2) 0.9138(4) 0.0154(12) Uani 1 1 d . . . H7 H 0.4402 0.9574 0.9481 0.018 Uiso 1 1 calc R . . C8 C 0.4587(5) 0.8808(2) 0.9586(4) 0.0183(13) Uani 1 1 d . . . H8A H 0.4599 0.8826 1.0341 0.022 Uiso 1 1 calc R . . H8B H 0.3863 0.8716 0.9366 0.022 Uiso 1 1 calc R . . C9 C 0.5373(4) 0.8406(2) 0.9234(4) 0.0161(13) Uani 1 1 d . . . H9 H 0.5245 0.8107 0.9661 0.019 Uiso 1 1 calc R . . C10 C 0.6545(5) 0.8551(2) 0.9389(4) 0.0196(13) Uani 1 1 d . . . H10A H 0.6989 0.8309 0.9030 0.024 Uiso 1 1 calc R . . H10B H 0.6721 0.8529 1.0127 0.024 Uiso 1 1 calc R . . C11 C 0.6843(4) 0.9079(2) 0.9004(4) 0.0150(12) Uani 1 1 d . . . H11 H 0.6877 0.9078 0.8241 0.018 Uiso 1 1 calc R . . C12 C 0.6029(4) 0.9471(2) 0.9353(4) 0.0153(12) Uani 1 1 d . . . H12A H 0.6124 0.9528 1.0095 0.018 Uiso 1 1 calc R . . H12B H 0.6179 0.9785 0.8999 0.018 Uiso 1 1 calc R . . C13 C 0.0509(4) 1.0269(2) 0.3269(4) 0.0155(12) Uani 1 1 d . . . H13 H 0.0181 1.0505 0.3757 0.019 Uiso 1 1 calc R . . C14 C -0.0268(5) 0.9834(2) 0.3123(4) 0.0190(13) Uani 1 1 d . . . H14A H -0.0488 0.9715 0.3802 0.023 Uiso 1 1 calc R . . H14B H -0.0908 0.9953 0.2758 0.023 Uiso 1 1 calc R . . C15 C 0.0206(4) 0.9400(2) 0.2519(4) 0.0175(13) Uani 1 1 d . . . H15 H -0.0308 0.9121 0.2547 0.021 Uiso 1 1 calc R . . C16 C 0.1271(4) 0.9220(2) 0.3009(4) 0.0169(13) Uani 1 1 d . . . H16A H 0.1121 0.9058 0.3668 0.020 Uiso 1 1 calc R . . H16B H 0.1590 0.8971 0.2555 0.020 Uiso 1 1 calc R . . C17 C 0.2088(4) 0.9640(2) 0.3199(4) 0.0145(12) Uani 1 1 d . . . H17 H 0.2376 0.9748 0.2527 0.017 Uiso 1 1 calc R . . C18 C 0.1585(4) 1.0097(2) 0.3747(4) 0.0150(12) Uani 1 1 d . . . H18A H 0.1474 1.0014 0.4474 0.018 Uiso 1 1 calc R . . H18B H 0.2091 1.0374 0.3723 0.018 Uiso 1 1 calc R . . N1 N 0.2701(4) 0.83396(18) 0.4159(3) 0.0155(10) Uani 1 1 d . . . H1A H 0.2440 0.8527 0.4682 0.019 Uiso 1 1 calc R . . H1B H 0.2138 0.8257 0.3745 0.019 Uiso 1 1 calc R . . N2 N 0.4472(4) 0.81788(17) 0.2704(3) 0.0144(10) Uani 1 1 d . . . H2C H 0.4084 0.8076 0.2147 0.017 Uiso 1 1 calc R . . H2D H 0.5116 0.8281 0.2466 0.017 Uiso 1 1 calc R . . N3 N 0.5757(4) 0.82908(18) 0.5955(3) 0.0147(10) Uani 1 1 d . . . H3A H 0.6388 0.8396 0.5693 0.018 Uiso 1 1 calc R . . H3B H 0.5880 0.8000 0.6291 0.018 Uiso 1 1 calc R . . N4 N 0.4610(4) 0.93427(18) 0.7994(3) 0.0148(10) Uani 1 1 d . . . H4C H 0.4824 0.9644 0.7759 0.018 Uiso 1 1 calc R . . H4D H 0.3887 0.9333 0.7922 0.018 Uiso 1 1 calc R . . N5 N 0.5126(4) 0.82670(19) 0.8122(3) 0.0165(11) Uani 1 1 d . . . H5A H 0.4453 0.8142 0.8096 0.020 Uiso 1 1 calc R . . H5B H 0.5576 0.8018 0.7942 0.020 Uiso 1 1 calc R . . N6 N 0.7933(4) 0.92123(19) 0.9450(3) 0.0165(11) Uani 1 1 d . . . H6C H 0.8372 0.8951 0.9325 0.020 Uiso 1 1 calc R . . H6D H 0.7861 0.9231 1.0146 0.020 Uiso 1 1 calc R . . N7 N 0.9351(4) 0.94630(19) 0.7740(3) 0.0185(11) Uani 1 1 d . . . H7A H 0.9999 0.9341 0.7935 0.022 Uiso 1 1 calc R . . H7B H 0.8918 0.9198 0.7619 0.022 Uiso 1 1 calc R . . N8 N 0.9667(4) 1.04577(19) 0.8592(3) 0.0187(11) Uani 1 1 d . . . H8C H 0.9397 1.0726 0.8925 0.022 Uiso 1 1 calc R . . H8D H 1.0331 1.0404 0.8858 0.022 Uiso 1 1 calc R . . N9 N 0.2994(3) 0.94337(18) 0.3859(3) 0.0143(10) Uani 1 1 d . . . H9A H 0.2739 0.9367 0.4497 0.017 Uiso 1 1 calc R . . H9B H 0.3502 0.9673 0.3931 0.017 Uiso 1 1 calc R . . Br1 Br 0.81128(5) 1.03166(2) 1.05063(4) 0.02093(14) Uani 1 1 d . . . Br2 Br 0.48559(5) 0.93305(2) 0.22529(4) 0.01864(14) Uani 1 1 d . . . Br3 Br 0.53801(5) 0.94626(2) 0.56979(4) 0.01922(14) Uani 1 1 d . . . Br4 Br 0.16479(5) 0.15940(2) 0.33124(5) 0.02390(15) Uani 1 1 d . . . Br5 Br 0.41088(5) 0.29109(2) 0.28537(4) 0.02323(15) Uani 1 1 d . . . Br6 Br 0.78573(5) 0.08981(3) 0.36169(4) 0.02510(15) Uani 1 1 d . . . Pd1 Pd 0.87376(3) 0.985123(17) 0.89887(3) 0.01443(11) Uani 1 1 d . . . Pd2 Pd 0.37170(3) 0.879444(17) 0.32960(3) 0.01238(11) Uani 1 1 d . . . Pd3 Pd 0.52278(3) 0.881309(17) 0.70118(3) 0.01293(11) Uani 1 1 d . . . O1 O 0.1832(4) 0.27500(18) 0.4108(3) 0.0273(11) Uani 1 1 d D . . H21 H 0.239(4) 0.285(2) 0.378(4) 0.041 Uiso 1 1 d D . . H22 H 0.179(5) 0.293(2) 0.463(3) 0.041 Uiso 1 1 d D . . O2 O 0.6938(4) 0.21938(17) 0.1277(3) 0.0283(10) Uani 1 1 d D . . H23 H 0.680(6) 0.218(2) 0.0624(19) 0.042 Uiso 1 1 d D . . H24 H 0.691(6) 0.2514(9) 0.140(4) 0.042 Uiso 1 1 d D . . O3 O 0.2246(4) 0.08732(19) 0.8301(3) 0.0301(11) Uani 1 1 d D . . H31 H 0.259(5) 0.0697(19) 0.785(4) 0.045 Uiso 1 1 d D . . H32 H 0.226(6) 0.1168(11) 0.803(5) 0.045 Uiso 1 1 d D . . O5 O 0.0098(4) 0.14004(19) 0.9975(4) 0.0348(11) Uani 1 1 d D . . H51 H -0.039(4) 0.148(3) 1.040(4) 0.052 Uiso 1 1 d D . . H52 H -0.001(6) 0.160(2) 0.946(4) 0.052 Uiso 1 1 d D . . O4 O 0.7098(3) 0.97001(18) 0.3547(3) 0.0289(11) Uani 1 1 d D . . H41 H 0.6424(18) 0.969(2) 0.364(5) 0.043 Uiso 1 1 d D . . H42 H 0.727(5) 1.0003(11) 0.366(6) 0.043 Uiso 1 1 d D . . O6 O 0.8752(4) 0.1619(2) 0.1630(4) 0.0432(13) Uani 1 1 d D . . H61 H 0.854(6) 0.139(2) 0.206(5) 0.065 Uiso 1 1 d D . . H62 H 0.820(4) 0.182(2) 0.163(6) 0.065 Uiso 1 1 d D . . O7 O 0.8387(4) 0.8140(2) 0.2905(4) 0.0400(12) Uani 1 1 d D . . H71 H 0.902(3) 0.808(3) 0.268(6) 0.060 Uiso 1 1 d D . . H72 H 0.848(5) 0.8412(18) 0.323(6) 0.060 Uiso 1 1 d D . . O8 O 0.8462(5) 0.2972(2) 0.3339(4) 0.0485(15) Uani 1 1 d D . . H81 H 0.856(7) 0.2662(10) 0.348(7) 0.073 Uiso 1 1 d D . . H82 H 0.783(6) 0.294(3) 0.297(6) 0.073 Uiso 1 1 d D . . O9 O 0.9192(4) 0.2026(2) 0.4057(5) 0.0564(16) Uani 1 1 d D . . H91 H 0.986(2) 0.196(3) 0.402(7) 0.085 Uiso 1 1 d D . . H92 H 0.887(5) 0.178(2) 0.378(7) 0.085 Uiso 1 1 d D . . O10 O 0.1781(6) 0.1120(2) 0.5691(4) 0.0679(19) Uani 1 1 d D . . H101 H 0.238(5) 0.128(4) 0.557(7) 0.102 Uiso 1 1 d D . . H102 H 0.145(6) 0.116(4) 0.510(4) 0.102 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 C1 0.016(3) 0.006(3) 0.019(3) 0.003(2) -0.001(2) -0.003(2) C2 0.014(3) 0.015(3) 0.018(3) 0.004(2) -0.004(2) -0.001(2) C3 0.019(3) 0.012(3) 0.015(3) -0.006(2) -0.002(2) 0.000(2) C4 0.017(3) 0.015(3) 0.019(3) 0.001(2) -0.003(2) 0.003(2) C5 0.012(3) 0.019(3) 0.013(3) 0.002(2) -0.006(2) 0.003(2) C6 0.017(3) 0.012(3) 0.014(3) 0.003(2) 0.001(2) 0.003(2) C7 0.018(3) 0.018(3) 0.010(2) -0.007(2) 0.001(2) 0.003(3) C8 0.024(3) 0.016(3) 0.015(3) -0.005(2) 0.003(2) -0.005(3) C9 0.024(3) 0.012(3) 0.012(3) 0.000(2) -0.002(2) -0.003(3) C10 0.025(3) 0.015(3) 0.018(3) 0.000(3) -0.003(2) -0.004(3) C11 0.013(3) 0.018(3) 0.014(3) 0.003(2) -0.003(2) 0.001(2) C12 0.019(3) 0.015(3) 0.012(3) 0.000(2) -0.002(2) -0.001(2) C13 0.011(3) 0.019(3) 0.017(3) -0.002(2) 0.008(2) 0.001(2) C14 0.014(3) 0.020(4) 0.024(3) 0.004(3) -0.002(2) 0.002(3) C15 0.014(3) 0.014(3) 0.025(3) 0.000(3) -0.001(2) -0.005(2) C16 0.019(3) 0.014(3) 0.018(3) 0.000(2) -0.003(2) 0.000(3) C17 0.013(3) 0.014(3) 0.017(3) 0.002(2) -0.004(2) 0.001(2) C18 0.013(3) 0.018(3) 0.014(3) -0.003(2) -0.002(2) -0.003(2) N1 0.014(2) 0.014(3) 0.018(2) -0.002(2) -0.0030(19) 0.000(2) N2 0.018(3) 0.012(3) 0.012(2) -0.001(2) -0.0038(18) -0.001(2) N3 0.014(2) 0.015(3) 0.015(2) 0.001(2) -0.0030(18) 0.002(2) N4 0.016(2) 0.008(3) 0.021(2) -0.004(2) -0.0026(19) 0.000(2) N5 0.017(3) 0.019(3) 0.014(2) 0.000(2) -0.0012(18) 0.003(2) N6 0.014(2) 0.018(3) 0.017(2) 0.002(2) -0.0026(19) 0.001(2) N7 0.013(2) 0.019(3) 0.024(2) -0.003(2) -0.0045(19) 0.001(2) N8 0.014(2) 0.019(3) 0.023(2) 0.000(2) -0.0053(19) 0.001(2) N9 0.009(2) 0.019(3) 0.015(2) 0.002(2) 0.0014(18) -0.001(2) Br1 0.0194(3) 0.0228(4) 0.0206(3) -0.0039(3) -0.0013(2) 0.0017(3) Br2 0.0227(3) 0.0169(3) 0.0164(3) -0.0002(2) 0.0033(2) -0.0029(3) Br3 0.0256(3) 0.0157(3) 0.0163(3) 0.0031(2) -0.0031(2) -0.0032(3) Br4 0.0235(3) 0.0198(4) 0.0283(3) 0.0003(3) -0.0039(2) -0.0008(3) Br5 0.0246(3) 0.0180(4) 0.0270(3) 0.0034(3) -0.0039(2) 0.0032(3) Br6 0.0248(3) 0.0261(4) 0.0245(3) 0.0018(3) 0.0054(2) 0.0057(3) Pd1 0.0133(2) 0.0144(3) 0.0155(2) 0.00016(18) -0.00331(16) 0.00059(18) Pd2 0.0125(2) 0.0121(2) 0.01251(19) 0.00048(17) -0.00156(16) 0.00041(18) Pd3 0.0149(2) 0.0121(2) 0.0117(2) -0.00043(17) -0.00232(16) 0.00035(18) O1 0.027(3) 0.033(3) 0.021(2) -0.001(2) 0.0000(18) 0.002(2) O2 0.033(3) 0.022(3) 0.029(2) 0.002(2) -0.001(2) -0.005(2) O3 0.039(3) 0.029(3) 0.022(2) 0.003(2) -0.003(2) 0.003(2) O5 0.034(3) 0.028(3) 0.042(3) 0.002(2) 0.004(2) 0.008(2) O4 0.022(2) 0.030(3) 0.034(2) -0.002(2) 0.003(2) -0.002(2) O6 0.037(3) 0.041(4) 0.052(3) 0.009(3) 0.008(2) 0.004(3) O7 0.034(3) 0.034(3) 0.052(3) -0.010(3) 0.006(2) -0.007(2) O8 0.046(3) 0.056(4) 0.044(3) -0.021(3) 0.019(2) -0.019(3) O9 0.035(3) 0.070(5) 0.065(4) -0.024(3) 0.015(3) -0.014(3) O10 0.123(6) 0.047(4) 0.034(3) -0.002(3) -0.003(3) 0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.492(7) . ? C1 C2 1.508(8) . ? C1 C6 1.525(7) . ? C2 C3 1.520(8) . ? C3 N2 1.490(7) . ? C3 C4 1.534(7) . ? C4 C5 1.522(8) . ? C5 N3 1.485(6) . ? C5 C6 1.526(8) . ? C7 N4 1.497(6) . ? C7 C12 1.521(8) . ? C7 C8 1.536(8) . ? C8 C9 1.523(8) . ? C9 N5 1.503(6) . ? C9 C10 1.515(8) . ? C10 C11 1.538(8) . ? C11 N6 1.504(7) . ? C11 C12 1.526(8) . ? C13 N7 1.490(7) 3_676 ? C13 C14 1.519(8) . ? C13 C18 1.532(7) . ? C14 C15 1.516(8) . ? C15 N8 1.487(7) 3_676 ? C15 C16 1.534(8) . ? C16 C17 1.529(8) . ? C17 N9 1.504(6) . ? C17 C18 1.542(8) . ? N1 Pd2 2.078(5) . ? N2 Pd2 2.041(5) . ? N3 Pd3 2.057(4) . ? N4 Pd3 2.048(4) . ? N5 Pd3 2.042(5) . ? N6 Pd1 2.065(5) . ? N7 C13 1.490(7) 3_676 ? N7 Pd1 2.061(5) . ? N8 C15 1.487(7) 3_676 ? N8 Pd1 2.053(5) . ? N9 Pd2 2.061(5) . ? Br1 Pd1 2.4433(7) . ? Br2 Pd2 2.4243(7) . ? Br3 Pd3 2.4260(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 111.1(4) . . ? N1 C1 C6 110.4(4) . . ? C2 C1 C6 111.2(4) . . ? C1 C2 C3 113.9(5) . . ? N2 C3 C2 110.6(5) . . ? N2 C3 C4 111.2(5) . . ? C2 C3 C4 110.8(4) . . ? C5 C4 C3 112.3(4) . . ? N3 C5 C6 109.8(4) . . ? N3 C5 C4 111.8(4) . . ? C6 C5 C4 111.1(5) . . ? C5 C6 C1 112.3(4) . . ? N4 C7 C12 110.9(4) . . ? N4 C7 C8 110.4(4) . . ? C12 C7 C8 112.1(5) . . ? C9 C8 C7 112.1(5) . . ? N5 C9 C10 111.8(4) . . ? N5 C9 C8 109.3(4) . . ? C10 C9 C8 113.4(5) . . ? C9 C10 C11 115.3(5) . . ? N6 C11 C12 108.7(4) . . ? N6 C11 C10 108.2(4) . . ? C12 C11 C10 111.7(5) . . ? C7 C12 C11 113.9(5) . . ? N7 C13 C14 109.9(4) 3_676 . ? N7 C13 C18 112.4(4) 3_676 . ? C14 C13 C18 111.7(5) . . ? C15 C14 C13 113.4(5) . . ? N8 C15 C14 110.0(5) 3_676 . ? N8 C15 C16 111.8(5) 3_676 . ? C14 C15 C16 111.6(5) . . ? C17 C16 C15 113.7(5) . . ? N9 C17 C16 108.1(4) . . ? N9 C17 C18 109.7(4) . . ? C16 C17 C18 112.4(5) . . ? C13 C18 C17 114.2(4) . . ? C1 N1 Pd2 119.6(3) . . ? C3 N2 Pd2 120.1(3) . . ? C5 N3 Pd3 114.0(3) . . ? C7 N4 Pd3 120.5(3) . . ? C9 N5 Pd3 118.3(4) . . ? C11 N6 Pd1 121.4(3) . . ? C13 N7 Pd1 118.8(4) 3_676 . ? C15 N8 Pd1 120.4(4) 3_676 . ? C17 N9 Pd2 115.5(3) . . ? N8 Pd1 N7 89.39(19) . . ? N8 Pd1 N6 174.59(18) . . ? N7 Pd1 N6 89.59(19) . . ? N8 Pd1 Br1 88.96(14) . . ? N7 Pd1 Br1 176.81(13) . . ? N6 Pd1 Br1 91.80(13) . . ? N2 Pd2 N9 177.72(19) . . ? N2 Pd2 N1 90.74(18) . . ? N9 Pd2 N1 91.54(18) . . ? N2 Pd2 Br2 89.75(13) . . ? N9 Pd2 Br2 87.97(13) . . ? N1 Pd2 Br2 178.23(12) . . ? N5 Pd3 N4 92.04(19) . . ? N5 Pd3 N3 90.00(18) . . ? N4 Pd3 N3 175.91(17) . . ? N5 Pd3 Br3 179.07(13) . . ? N4 Pd3 Br3 88.19(13) . . ? N3 Pd3 Br3 89.83(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.891 _refine_diff_density_min -0.913 _refine_diff_density_rms 0.206