# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _publ_contact_author_email aklein@iac.uni-stuttgart.de _publ_contact_author_name 'Dr Axel Klein' _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_address ; Inorganic Chemistry University of Stuttgart Pfaffenwaldring 55 Stuttgart D-70569 GERMANY ; _publ_contact_author_phone '+49 711 685-4235' _publ_contact_author_fax '+49 711 685-4165' _publ_section_title ; Tri(allyl)- and tri(methylallyl)arsine complexes of palladium(II) and platinum(II): synthesis, spectroscopy, photochemistry and structures ; loop_ _publ_author_name 'Axel Klein' 'Vimal K. Jain' 'Wolfgang Kaim' 'Prasad P. Phadnis' 'Thilo Schurr' #======================================================================== data_jain09 _database_code_CSD 214025 _chemical_name_common trans-Dichlorobis(triallylarsine)palladium(ii) _audit_creation_method SHELXL-97 _chemical_name_systematic trans-Dichlorobis(triallylarsine)palladium(II) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 As2 Cl2 Pd' _chemical_formula_weight 573.56 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 P2(1)/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 8.0698(19) _cell_length_b 8.102(2) _cell_length_c 18.278(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.426(14) _cell_angle_gamma 90.00 _cell_volume 1182.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568 _exptl_absorpt_coefficient_mu 3.787 _exptl_absorpt_correction_type 'empirical - psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens-P4 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2749 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0704 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2568 _reflns_number_gt 1744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0502P)^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 2568 _refine_ls_number_parameters 129 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0902 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 0.5000 0.5000 0.5000 0.03052(18) Uani 1 2 d S . . As1 As 0.69999(8) 0.69359(7) 0.56065(3) 0.03663(19) Uani 1 1 d . B . Cl1 Cl 0.3332(2) 0.72213(18) 0.46049(9) 0.0475(4) Uani 1 1 d . . . C1 C 0.6126(9) 0.8223(8) 0.6371(3) 0.0472(17) Uani 1 1 d . . . H1A H 0.6996 0.9005 0.6598 0.057 Uiso 1 1 calc R . . H1B H 0.5147 0.8874 0.6143 0.057 Uiso 1 1 calc R . . C2 C 0.5618(10) 0.7136(9) 0.6956(4) 0.062(2) Uani 1 1 d . . . H2A H 0.4694 0.6419 0.6817 0.074 Uiso 1 1 calc R . . C3 C 0.6337(12) 0.7085(12) 0.7642(4) 0.081(3) Uani 1 1 d . . . H3A H 0.7266 0.7782 0.7803 0.097 Uiso 1 1 calc R . . H3B H 0.5932 0.6352 0.7981 0.097 Uiso 1 1 calc R . . C11 C 0.9144(9) 0.6071(9) 0.6117(4) 0.058(2) Uani 1 1 d D . . H11A H 0.8921 0.5065 0.6394 0.11(4) Uiso 1 1 calc R A 1 H11B H 0.9853 0.5749 0.5742 0.11(3) Uiso 1 1 calc R A 1 C12 C 1.0107(17) 0.7300(16) 0.6652(7) 0.054(4) Uani 0.60 1 d PD B 1 H12 H 0.9784 0.7521 0.7121 0.11(6) Uiso 0.60 1 calc PR B 1 C13 C 1.1378(18) 0.803(2) 0.6440(10) 0.066(4) Uani 0.60 1 d PD B 1 H13A H 1.1679 0.7787 0.5968 0.09(5) Uiso 0.60 1 calc PR B 1 H13B H 1.2013 0.8800 0.6756 0.10(5) Uiso 0.60 1 calc PR B 1 C12A C 1.040(2) 0.7483(19) 0.6255(10) 0.047(5) Uani 0.40 1 d PD B 2 H12A H 1.0790 0.7984 0.5842 0.057 Uiso 0.40 1 calc PR B 2 C13A C 1.096(3) 0.803(3) 0.6908(11) 0.073(7) Uani 0.40 1 d PD B 2 H13C H 1.0589 0.7542 0.7329 0.087 Uiso 0.40 1 calc PR B 2 H13D H 1.1743 0.8908 0.6968 0.087 Uiso 0.40 1 calc PR B 2 C21 C 0.7646(9) 0.8609(8) 0.4935(4) 0.0512(17) Uani 1 1 d . . . H21A H 0.6644 0.9250 0.4725 0.061 Uiso 1 1 calc R B . H21B H 0.8455 0.9380 0.5214 0.061 Uiso 1 1 calc R . . C22 C 0.8424(10) 0.7846(9) 0.4316(4) 0.061(2) Uani 1 1 d . B . H22A H 0.9608 0.7742 0.4373 0.073 Uiso 1 1 calc R . . C23 C 0.7556(13) 0.7326(12) 0.3710(5) 0.090(3) Uani 1 1 d . . . H23C H 0.6370 0.7417 0.3640 0.107 Uiso 1 1 calc R B . H23A H 0.8103 0.6852 0.3335 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0334(3) 0.0223(3) 0.0343(3) -0.0019(3) -0.0001(2) 0.0043(3) As1 0.0368(4) 0.0248(3) 0.0457(4) -0.0030(3) -0.0028(3) 0.0023(3) Cl1 0.0460(9) 0.0266(8) 0.0649(10) -0.0013(7) -0.0088(8) 0.0108(7) C1 0.054(4) 0.038(4) 0.043(3) -0.008(3) -0.013(3) 0.004(3) C2 0.067(5) 0.055(5) 0.061(5) -0.006(4) 0.004(4) 0.014(4) C3 0.088(7) 0.097(7) 0.060(5) 0.001(5) 0.015(5) 0.035(6) C11 0.046(4) 0.040(4) 0.080(5) -0.002(4) -0.019(4) 0.012(4) C12 0.057(9) 0.052(8) 0.053(8) 0.007(7) 0.013(8) 0.000(7) C13 0.053(9) 0.070(10) 0.076(11) 0.009(9) 0.004(8) 0.000(9) C12A 0.019(9) 0.052(12) 0.064(14) 0.001(10) -0.017(9) 0.002(9) C13A 0.034(10) 0.098(18) 0.085(16) -0.045(15) 0.000(11) -0.027(12) C21 0.051(4) 0.032(4) 0.070(4) 0.004(3) 0.007(3) 0.005(3) C22 0.053(5) 0.049(5) 0.084(6) 0.013(4) 0.023(4) -0.001(4) C23 0.084(7) 0.123(9) 0.067(6) -0.005(6) 0.026(5) 0.010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.2993(15) 3_666 ? Pd1 Cl1 2.2993(15) . ? Pd1 As1 2.4020(7) . ? Pd1 As1 2.4020(7) 3_666 ? As1 C21 1.951(7) . ? As1 C1 1.956(6) . ? As1 C11 1.970(6) . ? C1 C2 1.488(10) . ? C2 C3 1.303(10) . ? C11 C12A 1.526(12) . ? C11 C12 1.526(11) . ? C12 C13 1.290(12) . ? C12A C13A 1.290(12) . ? C21 C22 1.505(10) . ? C22 C23 1.290(10) . ? 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 Cl1 Pd1 Cl1 180.00(8) 3_666 . ? Cl1 Pd1 As1 92.49(5) 3_666 . ? Cl1 Pd1 As1 87.51(5) . . ? Cl1 Pd1 As1 87.51(5) 3_666 3_666 ? Cl1 Pd1 As1 92.49(5) . 3_666 ? As1 Pd1 As1 180.00(2) . 3_666 ? C21 As1 C1 103.7(3) . . ? C21 As1 C11 104.4(3) . . ? C1 As1 C11 103.6(3) . . ? C21 As1 Pd1 112.7(2) . . ? C1 As1 Pd1 112.9(2) . . ? C11 As1 Pd1 118.1(2) . . ? C2 C1 As1 111.3(5) . . ? C3 C2 C1 125.4(8) . . ? C12A C11 C12 30.7(8) . . ? C12A C11 As1 109.2(8) . . ? C12 C11 As1 113.6(7) . . ? C13 C12 C11 117.3(13) . . ? C13A C12A C11 122.9(18) . . ? C22 C21 As1 111.5(5) . . ? C23 C22 C21 123.0(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 As1 C21 124.9(2) 3_666 . . . ? Cl1 Pd1 As1 C21 -55.1(2) . . . . ? As1 Pd1 As1 C21 -42(100) 3_666 . . . ? Cl1 Pd1 As1 C1 -118.0(2) 3_666 . . . ? Cl1 Pd1 As1 C1 62.0(2) . . . . ? As1 Pd1 As1 C1 75(100) 3_666 . . . ? Cl1 Pd1 As1 C11 3.0(3) 3_666 . . . ? Cl1 Pd1 As1 C11 -177.0(3) . . . . ? As1 Pd1 As1 C11 -164(100) 3_666 . . . ? C21 As1 C1 C2 -178.0(5) . . . . ? C11 As1 C1 C2 -69.3(5) . . . . ? Pd1 As1 C1 C2 59.6(5) . . . . ? As1 C1 C2 C3 113.6(7) . . . . ? C21 As1 C11 C12A 37.0(9) . . . . ? C1 As1 C11 C12A -71.3(9) . . . . ? Pd1 As1 C11 C12A 163.0(9) . . . . ? C21 As1 C11 C12 69.7(8) . . . . ? C1 As1 C11 C12 -38.6(8) . . . . ? Pd1 As1 C11 C12 -164.2(6) . . . . ? C12A C11 C12 C13 -15.7(16) . . . . ? As1 C11 C12 C13 -103.7(14) . . . . ? C12 C11 C12A C13A 8.2(17) . . . . ? As1 C11 C12A C13A 112.4(19) . . . . ? C1 As1 C21 C22 177.7(5) . . . . ? C11 As1 C21 C22 69.5(6) . . . . ? Pd1 As1 C21 C22 -59.8(5) . . . . ? As1 C21 C22 C23 86.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.823 _refine_diff_density_min -0.835 _refine_diff_density_rms 0.129 #========================================================================= data_akfeb03 _database_code_CSD 214026 _chemical_name_common trans-Dibromobis(triallylarsine)palladium(ii) _audit_creation_method SHELXL-97 _chemical_name_systematic trans-Dibromobis(triallylarsine)palladium(II) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H30 As2 Br2 Pd' _chemical_formula_weight 662.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Pd Pd -0.9988 1.0072 '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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 8.21980(10) _cell_length_b 18.41340(10) _cell_length_c 49.8803(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.000(5) _cell_angle_gamma 90.00 _cell_volume 7549.61(13) _cell_formula_units_Z 12 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3840 _exptl_absorpt_coefficient_mu 6.521 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details '94 reflections' _exptl_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method CCD # Orientation matrix from 'scale_all.out' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_UB_11 -0.0035058 _diffrn_orient_matrix_UB_21 0.1130941 _diffrn_orient_matrix_UB_31 -0.0446987 _diffrn_orient_matrix_UB_12 0.0460827 _diffrn_orient_matrix_UB_22 0.0117867 _diffrn_orient_matrix_UB_32 0.0262078 _diffrn_orient_matrix_UB_13 0.0105923 _diffrn_orient_matrix_UB_23 -0.0059715 _diffrn_orient_matrix_UB_33 -0.0159394 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33313 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 24.12 _reflns_number_total 5797 _reflns_number_gt 4184 _reflns_threshold_expression >2sigma(I) loop_ _reflns_scale_group_code _reflns_scale_meas_F 1 1.0 _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, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0571P)^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 5797 _refine_ls_number_parameters 304 _refine_ls_number_restraints 17 _refine_ls_R_factor_all 0.0841 _refine_ls_R_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.301 _refine_ls_restrained_S_all 1.299 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.95734(6) 0.12462(3) 0.165550(10) 0.0759(2) Uani 1 1 d . . . As2 As 1.14173(8) 0.19815(4) 0.191032(15) 0.0868(3) Uani 1 1 d . D . As1 As 0.77406(8) 0.04658(4) 0.141767(15) 0.0883(3) Uani 1 1 d . B . Br1 Br 0.72048(9) 0.18229(5) 0.184849(18) 0.1119(3) Uani 1 1 d . . . Br2 Br 1.19407(10) 0.06664(5) 0.14652(2) 0.1197(3) Uani 1 1 d . . . Pd2 Pd 1.0000 0.0000 0.0000 0.0787(2) Uani 1 2 d S . . As3 As 1.18148(8) 0.07887(4) 0.023805(15) 0.0901(3) Uani 1 1 d . H . Br3 Br 0.76166(9) 0.05495(5) 0.01976(2) 0.1208(3) Uani 1 1 d . . . C11 C 0.6451(10) -0.0132(4) 0.16630(16) 0.110(2) Uani 1 1 d D . . H11A H 0.6081 0.0167 0.1811 0.133 Uiso 1 1 calc R A 1 H11B H 0.5497 -0.0310 0.1569 0.133 Uiso 1 1 calc R A 1 C12 C 0.736(3) -0.0753(11) 0.1770(5) 0.132(9) Uiso 0.40 1 d PD B 1 H12 H 0.7316 -0.1193 0.1679 0.158 Uiso 0.40 1 calc PR B 1 C13 C 0.825(4) -0.0717(19) 0.1990(5) 0.174(11) Uiso 0.40 1 d PD B 1 H13A H 0.8316 -0.0284 0.2085 0.209 Uiso 0.40 1 calc PR B 1 H13B H 0.8807 -0.1125 0.2050 0.209 Uiso 0.40 1 calc PR B 1 C12A C 0.7541(18) -0.0427(8) 0.1870(3) 0.111(5) Uiso 0.60 1 d PD B 2 H12A H 0.7910 -0.0122 0.2005 0.133 Uiso 0.60 1 calc PR B 2 C13A C 0.801(3) -0.1111(9) 0.1868(4) 0.159(7) Uiso 0.60 1 d PD B 2 H13C H 0.7650 -0.1422 0.1734 0.191 Uiso 0.60 1 calc PR B 2 H13D H 0.8700 -0.1282 0.2002 0.191 Uiso 0.60 1 calc PR B 2 C21 C 0.6111(9) 0.0973(4) 0.12005(16) 0.117(3) Uani 1 1 d D . . H21A H 0.5334 0.0625 0.1130 0.140 Uiso 1 1 calc R B 1 H21B H 0.5525 0.1317 0.1312 0.140 Uiso 1 1 calc R B 1 C22 C 0.6904(16) 0.1365(7) 0.0974(3) 0.117(4) Uiso 0.70 1 d PD B 1 H22 H 0.7066 0.1124 0.0812 0.140 Uiso 0.70 1 calc PR B 1 C23 C 0.737(2) 0.2029(9) 0.0996(4) 0.188(8) Uiso 0.70 1 d PD B 1 H23A H 0.7212 0.2276 0.1157 0.225 Uiso 0.70 1 calc PR B 1 H23B H 0.7859 0.2262 0.0852 0.225 Uiso 0.70 1 calc PR B 1 C22A C 0.665(5) 0.1706(10) 0.1109(7) 0.161(14) Uiso 0.30 1 d PD B 2 H22A H 0.6641 0.2102 0.1224 0.194 Uiso 0.30 1 calc PR B 2 C23A C 0.712(4) 0.177(2) 0.0864(6) 0.126(11) Uiso 0.30 1 d PD B 2 H23C H 0.7120 0.1369 0.0752 0.152 Uiso 0.30 1 calc PR B 2 H23D H 0.7463 0.2220 0.0800 0.152 Uiso 0.30 1 calc PR B 2 C31 C 0.8676(10) -0.0245(5) 0.11695(17) 0.129(3) Uani 1 1 d D . . H31A H 0.9567 -0.0023 0.1072 0.155 Uiso 1 1 calc R B 1 H31B H 0.9112 -0.0651 0.1271 0.155 Uiso 1 1 calc R B 1 C32 C 0.740(3) -0.0527(15) 0.0969(5) 0.154(11) Uiso 0.40 1 d PD B 1 H32 H 0.6995 -0.0240 0.0831 0.09(5) Uiso 0.40 1 calc PR B 1 C33 C 0.692(5) -0.1204(16) 0.1007(9) 0.210(15) Uiso 0.40 1 d PD B 1 H33A H 0.7358 -0.1474 0.1148 0.252 Uiso 0.40 1 calc PR B 1 H33B H 0.6155 -0.1410 0.0894 0.252 Uiso 0.40 1 calc PR B 1 C32A C 0.7447(19) -0.0833(10) 0.1086(3) 0.130(6) Uiso 0.60 1 d PD B 2 H32A H 0.7164 -0.1199 0.1206 0.11(4) Uiso 0.60 1 calc PR B 2 C33A C 0.679(3) -0.0816(13) 0.0845(3) 0.172(8) Uiso 0.60 1 d PD B 2 H33C H 0.7076 -0.0449 0.0725 0.206 Uiso 0.60 1 calc PR B 2 H33D H 0.6048 -0.1170 0.0794 0.206 Uiso 0.60 1 calc PR B 2 C41 C 1.2973(9) 0.2533(5) 0.16984(18) 0.114(3) Uani 1 1 d . D . H41A H 1.3575 0.2857 0.1815 0.13(3) Uiso 1 1 calc R . . H41B H 1.3744 0.2201 0.1617 0.14(3) Uiso 1 1 calc R . . C42 C 1.2164(13) 0.2967(6) 0.1485(2) 0.142(3) Uiso 1 1 d D . . H42 H 1.1590 0.2773 0.1341 0.170 Uiso 1 1 calc R C 1 C43 C 1.237(3) 0.3625(8) 0.1527(5) 0.153(9) Uiso 0.50 1 d PD D 1 H43A H 1.2027 0.3964 0.1401 0.184 Uiso 0.50 1 calc PR D 1 H43B H 1.2858 0.3779 0.1685 0.184 Uiso 0.50 1 calc PR D 1 C43A C 1.193(3) 0.3573(9) 0.1383(5) 0.152(9) Uiso 0.50 1 d PD D 2 H43C H 1.2248 0.3990 0.1473 0.182 Uiso 0.50 1 calc PR D 2 H43D H 1.1431 0.3608 0.1215 0.182 Uiso 0.50 1 calc PR D 2 C51 C 1.0482(9) 0.2684(4) 0.21562(17) 0.119(3) Uani 1 1 d D . . H51A H 1.0012 0.3076 0.2052 0.143 Uiso 1 1 calc R E 1 H51B H 0.9602 0.2451 0.2253 0.143 Uiso 1 1 calc R E 1 C52 C 1.1625(16) 0.3001(7) 0.2353(3) 0.103(4) Uiso 0.60 1 d PD F 1 H52 H 1.1994 0.2752 0.2504 0.09(3) Uiso 0.60 1 calc PR F 1 C53 C 1.208(3) 0.3680(9) 0.2294(5) 0.170(8) Uiso 0.60 1 d PD F 1 H53A H 1.1672 0.3905 0.2140 0.203 Uiso 0.60 1 calc PR F 1 H53B H 1.2793 0.3928 0.2405 0.203 Uiso 0.60 1 calc PR F 1 C52A C 1.174(4) 0.3241(17) 0.2207(7) 0.195(15) Uiso 0.40 1 d PD F 2 H52A H 1.2098 0.3482 0.2054 0.235 Uiso 0.40 1 calc PR F 2 C53A C 1.246(4) 0.346(2) 0.2433(6) 0.192(14) Uiso 0.40 1 d PD F 2 H53C H 1.2171 0.3246 0.2595 0.230 Uiso 0.40 1 calc PR F 2 H53D H 1.3240 0.3823 0.2428 0.230 Uiso 0.40 1 calc PR F 2 C61 C 1.2799(10) 0.1380(5) 0.2139(2) 0.114(3) Uani 1 1 d D . . H61A H 1.3711 0.1196 0.2036 0.17(4) Uiso 1 1 calc R F 1 H61B H 1.3224 0.1670 0.2286 0.14(3) Uiso 1 1 calc R F 1 C62 C 1.182(2) 0.0757(9) 0.2249(4) 0.124(6) Uiso 0.50 1 d PD F 1 H62 H 1.1500 0.0396 0.2130 0.10(4) Uiso 0.50 1 calc PR F 1 C63 C 1.140(3) 0.0684(13) 0.2503(4) 0.147(8) Uiso 0.50 1 d PD F 1 H63A H 1.1700 0.1033 0.2628 0.177 Uiso 0.50 1 calc PR F 1 H63B H 1.0793 0.0282 0.2557 0.177 Uiso 0.50 1 calc PR F 1 C62A C 1.194(2) 0.1092(9) 0.2383(3) 0.119(6) Uiso 0.50 1 d PD F 2 H62A H 1.1990 0.1323 0.2549 0.10(4) Uiso 0.50 1 calc PR F 2 C63A C 1.111(3) 0.0485(11) 0.2345(6) 0.158(9) Uiso 0.50 1 d PD F 2 H63C H 1.1087 0.0269 0.2177 0.189 Uiso 0.50 1 calc PR F 2 H63D H 1.0547 0.0275 0.2487 0.189 Uiso 0.50 1 calc PR F 2 C71 C 1.3196(10) 0.1367(4) 0.00020(19) 0.113(3) Uani 1 1 d D . . H71A H 1.4190 0.1483 0.0098 0.17(4) Uiso 1 1 calc R G 1 H71B H 1.3494 0.1070 -0.0151 0.12(3) Uiso 1 1 calc R G 1 C72 C 1.249(4) 0.2040(11) -0.0097(6) 0.191(15) Uiso 0.40 1 d PD H 1 H72 H 1.2687 0.2472 -0.0006 0.229 Uiso 0.40 1 calc PR H 1 C73 C 1.157(4) 0.2048(19) -0.0313(5) 0.170(12) Uiso 0.40 1 d PD H 1 H73A H 1.1371 0.1619 -0.0406 0.204 Uiso 0.40 1 calc PR H 1 H73B H 1.1132 0.2483 -0.0374 0.204 Uiso 0.40 1 calc PR H 1 C72A C 1.2190(18) 0.1714(7) -0.0201(3) 0.104(4) Uiso 0.60 1 d PD H 2 H72A H 1.1671 0.1430 -0.0330 0.125 Uiso 0.60 1 calc PR H 2 C73A C 1.200(2) 0.2424(8) -0.0206(4) 0.141(6) Uiso 0.60 1 d PD H 2 H73C H 1.2520 0.2711 -0.0078 0.170 Uiso 0.60 1 calc PR H 2 H73D H 1.1359 0.2639 -0.0337 0.170 Uiso 0.60 1 calc PR H 2 C81 C 1.3391(9) 0.0259(5) 0.04554(16) 0.122(3) Uani 1 1 d D . . H81A H 1.4345 0.0149 0.0348 0.146 Uiso 1 1 calc R H 1 H81B H 1.3729 0.0558 0.0606 0.146 Uiso 1 1 calc R H 1 C82 C 1.265(5) -0.0441(13) 0.0559(7) 0.178(18) Uiso 0.30 1 d PD H 1 H82 H 1.2379 -0.0815 0.0442 0.214 Uiso 0.30 1 calc PR H 1 C83 C 1.240(5) -0.050(2) 0.0807(6) 0.146(13) Uiso 0.30 1 d PD H 1 H83A H 1.2679 -0.0125 0.0922 0.175 Uiso 0.30 1 calc PR H 1 H83B H 1.1950 -0.0927 0.0876 0.175 Uiso 0.30 1 calc PR H 1 C82A C 1.2568(17) -0.0111(7) 0.0691(3) 0.126(4) Uiso 0.70 1 d PD H 2 H82A H 1.2429 0.0136 0.0852 0.151 Uiso 0.70 1 calc PR H 2 C83A C 1.207(2) -0.0756(9) 0.0666(4) 0.172(7) Uiso 0.70 1 d PD H 2 H83C H 1.2217 -0.1000 0.0504 0.207 Uiso 0.70 1 calc PR H 2 H83D H 1.1568 -0.0988 0.0809 0.207 Uiso 0.70 1 calc PR H 2 C91 C 1.0862(10) 0.1495(5) 0.04816(18) 0.131(3) Uani 1 1 d D . . H91A H 1.0415 0.1892 0.0378 0.157 Uiso 1 1 calc R H 1 H91B H 0.9971 0.1267 0.0577 0.157 Uiso 1 1 calc R H 1 C92 C 1.205(3) 0.1795(16) 0.0681(5) 0.158(12) Uiso 0.40 1 d PD H 1 H92 H 1.2445 0.1486 0.0814 0.13(7) Uiso 0.40 1 calc PR H 1 C93 C 1.256(4) 0.2470(15) 0.0679(7) 0.184(13) Uiso 0.40 1 d PD H 1 H93A H 1.2182 0.2790 0.0549 0.221 Uiso 0.40 1 calc PR H 1 H93B H 1.3297 0.2628 0.0808 0.221 Uiso 0.40 1 calc PR H 1 C92A C 1.203(2) 0.2078(10) 0.0564(3) 0.132(6) Uiso 0.60 1 d PD H 2 H92A H 1.2355 0.2446 0.0448 0.09(3) Uiso 0.60 1 calc PR H 2 C93A C 1.257(3) 0.2033(14) 0.0811(4) 0.177(8) Uiso 0.60 1 d PD H 2 H93C H 1.2228 0.1658 0.0921 0.212 Uiso 0.60 1 calc PR H 2 H93D H 1.3305 0.2378 0.0875 0.212 Uiso 0.60 1 calc PR H 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0466(3) 0.0840(4) 0.0971(4) -0.0004(3) 0.0073(3) 0.0057(2) As2 0.0528(4) 0.0946(5) 0.1129(6) -0.0082(4) -0.0014(4) 0.0078(3) As1 0.0563(4) 0.1036(5) 0.1050(6) -0.0106(4) 0.0085(4) -0.0037(4) Br1 0.0540(4) 0.1348(7) 0.1470(8) -0.0339(5) 0.0082(4) 0.0158(4) Br2 0.0580(5) 0.1330(7) 0.1680(9) -0.0439(6) 0.0201(5) 0.0091(4) Pd2 0.0474(4) 0.0887(5) 0.1001(6) -0.0045(4) 0.0103(4) 0.0022(3) As3 0.0560(4) 0.1037(5) 0.1107(6) -0.0130(4) 0.0061(4) -0.0022(4) Br3 0.0572(5) 0.1407(7) 0.1646(8) -0.0472(6) 0.0196(5) 0.0060(5) C11 0.086(5) 0.118(6) 0.126(6) -0.003(5) 0.011(5) -0.013(5) C21 0.066(5) 0.144(7) 0.139(7) 0.004(5) -0.011(5) 0.005(5) C31 0.100(6) 0.136(7) 0.151(8) -0.054(6) 0.020(6) -0.012(5) C41 0.067(5) 0.110(6) 0.163(8) 0.000(6) 0.010(5) -0.004(5) C51 0.072(5) 0.128(6) 0.157(7) -0.040(6) -0.009(5) 0.004(5) C61 0.073(5) 0.143(7) 0.127(7) 0.008(6) -0.017(5) 0.027(5) C71 0.077(5) 0.113(6) 0.149(7) -0.016(6) 0.019(6) -0.016(5) C81 0.062(5) 0.180(8) 0.123(7) 0.003(6) -0.004(5) 0.017(5) C91 0.084(6) 0.140(7) 0.168(8) -0.067(6) 0.005(6) -0.014(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 As1 2.3962(9) . ? Pd1 As2 2.3970(9) . ? Pd1 Br2 2.4140(8) . ? Pd1 Br1 2.4177(8) . ? As2 C51 1.941(7) . ? As2 C41 1.946(7) . ? As2 C61 1.954(7) . ? As1 C11 1.958(7) . ? As1 C21 1.959(7) . ? As1 C31 1.960(7) . ? Pd2 As3 2.3967(7) 5_755 ? Pd2 As3 2.3967(7) . ? Pd2 Br3 2.4153(7) 5_755 ? Pd2 Br3 2.4153(7) . ? As3 C91 1.944(7) . ? As3 C81 1.951(7) . ? As3 C71 1.951(7) . ? C11 C12 1.469(13) . ? C11 C12A 1.470(12) . ? C12 C13 1.318(15) . ? C12A C13A 1.316(15) . ? C21 C22 1.492(12) . ? C21 C22A 1.492(13) . ? C22 C23 1.285(16) . ? C22A C23A 1.284(16) . ? C31 C32A 1.537(14) . ? C31 C32 1.537(14) . ? C32 C33 1.321(17) . ? C32A C33A 1.321(16) . ? C41 C42 1.489(12) . ? C42 C43A 1.241(12) . ? C42 C43 1.242(12) . ? C51 C52A 1.479(13) . ? C51 C52 1.480(13) . ? C52 C53 1.338(16) . ? C52A C53A 1.334(17) . ? C61 C62A 1.502(13) . ? C61 C62 1.503(13) . ? C62 C63 1.321(14) . ? C62A C63A 1.322(14) . ? C71 C72 1.456(14) . ? C71 C72A 1.456(13) . ? C72 C73 1.316(16) . ? C72A C73A 1.316(15) . ? C81 C82A 1.516(13) . ? C81 C82 1.516(14) . ? C82 C83 1.262(17) . ? C82A C83A 1.262(16) . ? C91 C92 1.500(14) . ? C91 C92A 1.500(14) . ? C92 C93 1.311(17) . ? C92A C93A 1.312(17) . ? 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 As1 Pd1 As2 177.15(3) . . ? As1 Pd1 Br2 92.69(3) . . ? As2 Pd1 Br2 87.06(3) . . ? As1 Pd1 Br1 87.38(3) . . ? As2 Pd1 Br1 92.86(3) . . ? Br2 Pd1 Br1 179.67(4) . . ? C51 As2 C41 104.8(4) . . ? C51 As2 C61 103.8(4) . . ? C41 As2 C61 103.4(4) . . ? C51 As2 Pd1 117.4(2) . . ? C41 As2 Pd1 115.0(3) . . ? C61 As2 Pd1 110.9(3) . . ? C11 As1 C21 104.1(3) . . ? C11 As1 C31 103.4(4) . . ? C21 As1 C31 103.7(4) . . ? C11 As1 Pd1 111.6(2) . . ? C21 As1 Pd1 114.7(2) . . ? C31 As1 Pd1 117.8(3) . . ? As3 Pd2 As3 180.00(4) 5_755 . ? As3 Pd2 Br3 92.80(3) 5_755 . ? As3 Pd2 Br3 87.20(3) . 5_755 ? As3 Pd2 Br3 87.20(3) 5_755 . ? As3 Pd2 Br3 92.80(3) . . ? Br3 Pd2 Br3 180.00(5) 5_755 . ? C91 As3 C81 104.7(4) . . ? C91 As3 C71 104.3(4) . . ? C81 As3 C71 102.8(4) . . ? C91 As3 Pd2 117.6(2) . . ? C81 As3 Pd2 112.7(3) . . ? C71 As3 Pd2 113.2(3) . . ? C12 C11 C12A 31.3(11) . . ? C12 C11 As1 112.9(11) . . ? C12A C11 As1 108.4(7) . . ? C13 C12 C11 123(2) . . ? C13A C12A C11 121.9(15) . . ? C22 C21 C22A 36.8(14) . . ? C22 C21 As1 110.6(6) . . ? C22A C21 As1 113.5(16) . . ? C23 C22 C21 121.5(15) . . ? C23A C22A C21 118(3) . . ? C32A C31 C32 30.6(13) . . ? C32A C31 As1 112.5(8) . . ? C32 C31 As1 111.6(12) . . ? C33 C32 C31 115(3) . . ? C33A C32A C31 119.8(18) . . ? C42 C41 As2 112.0(6) . . ? C43A C42 C43 38.1(15) . . ? C43A C42 C41 147.7(17) . . ? C43 C42 C41 110.0(16) . . ? C52A C51 C52 33.8(15) . . ? C52A C51 As2 107.0(15) . . ? C52 C51 As2 115.5(7) . . ? C53 C52 C51 113.3(17) . . ? C53A C52A C51 131(3) . . ? C62A C61 C62 35.4(10) . . ? C62A C61 As2 113.6(8) . . ? C62 C61 As2 109.7(9) . . ? C63 C62 C61 124.7(18) . . ? C63A C62A C61 115.2(17) . . ? C72 C71 C72A 33.2(14) . . ? C72 C71 As3 115.9(15) . . ? C72A C71 As3 109.2(7) . . ? C73 C72 C71 121(3) . . ? C73A C72A C71 120.9(14) . . ? C82A C81 C82 34.5(15) . . ? C82A C81 As3 111.0(7) . . ? C82 C81 As3 110.3(17) . . ? C83 C82 C81 118(3) . . ? C83A C82A C81 119.3(15) . . ? C92 C91 C92A 30.3(14) . . ? C92 C91 As3 113.6(13) . . ? C92A C91 As3 113.0(8) . . ? C93 C92 C91 124(3) . . ? C93A C92A C91 115.4(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag As1 Pd1 As2 C51 -93.9(7) . . . . ? Br2 Pd1 As2 C51 -178.8(3) . . . . ? Br1 Pd1 As2 C51 0.9(3) . . . . ? As1 Pd1 As2 C41 142.1(7) . . . . ? Br2 Pd1 As2 C41 57.1(3) . . . . ? Br1 Pd1 As2 C41 -123.2(3) . . . . ? As1 Pd1 As2 C61 25.2(7) . . . . ? Br2 Pd1 As2 C61 -59.7(3) . . . . ? Br1 Pd1 As2 C61 120.0(3) . . . . ? As2 Pd1 As1 C11 31.9(7) . . . . ? Br2 Pd1 As1 C11 116.6(3) . . . . ? Br1 Pd1 As1 C11 -63.0(3) . . . . ? As2 Pd1 As1 C21 149.9(7) . . . . ? Br2 Pd1 As1 C21 -125.3(3) . . . . ? Br1 Pd1 As1 C21 55.0(3) . . . . ? As2 Pd1 As1 C31 -87.5(7) . . . . ? Br2 Pd1 As1 C31 -2.8(3) . . . . ? Br1 Pd1 As1 C31 177.6(3) . . . . ? As3 Pd2 As3 C91 -67(70) 5_755 . . . ? Br3 Pd2 As3 C91 -179.0(3) 5_755 . . . ? Br3 Pd2 As3 C91 1.0(3) . . . . ? As3 Pd2 As3 C81 55(69) 5_755 . . . ? Br3 Pd2 As3 C81 -57.0(3) 5_755 . . . ? Br3 Pd2 As3 C81 123.0(3) . . . . ? As3 Pd2 As3 C71 171(70) 5_755 . . . ? Br3 Pd2 As3 C71 59.2(3) 5_755 . . . ? Br3 Pd2 As3 C71 -120.8(3) . . . . ? C21 As1 C11 C12 157.7(12) . . . . ? C31 As1 C11 C12 49.6(12) . . . . ? Pd1 As1 C11 C12 -78.0(12) . . . . ? C21 As1 C11 C12A -169.1(8) . . . . ? C31 As1 C11 C12A 82.7(8) . . . . ? Pd1 As1 C11 C12A -44.9(8) . . . . ? C12A C11 C12 C13 0(2) . . . . ? As1 C11 C12 C13 89(2) . . . . ? C12 C11 C12A C13A -1(2) . . . . ? As1 C11 C12A C13A -105.1(14) . . . . ? C11 As1 C21 C22 -171.1(7) . . . . ? C31 As1 C21 C22 -63.2(8) . . . . ? Pd1 As1 C21 C22 66.7(7) . . . . ? C11 As1 C21 C22A 149.2(15) . . . . ? C31 As1 C21 C22A -102.9(15) . . . . ? Pd1 As1 C21 C22A 27.0(15) . . . . ? C22A C21 C22 C23 11(3) . . . . ? As1 C21 C22 C23 -91.3(14) . . . . ? C22 C21 C22A C23A 9(2) . . . . ? As1 C21 C22A C23A 103(3) . . . . ? C11 As1 C31 C32A 41.7(10) . . . . ? C21 As1 C31 C32A -66.7(10) . . . . ? Pd1 As1 C31 C32A 165.3(9) . . . . ? C11 As1 C31 C32 74.8(14) . . . . ? C21 As1 C31 C32 -33.6(14) . . . . ? Pd1 As1 C31 C32 -161.6(13) . . . . ? C32A C31 C32 C33 -10(2) . . . . ? As1 C31 C32 C33 -108(2) . . . . ? C32 C31 C32A C33A 11(3) . . . . ? As1 C31 C32A C33A 105.3(15) . . . . ? C51 As2 C41 C42 -78.5(8) . . . . ? C61 As2 C41 C42 173.0(7) . . . . ? Pd1 As2 C41 C42 52.0(8) . . . . ? As2 C41 C42 C43A 123(3) . . . . ? As2 C41 C42 C43 115.7(13) . . . . ? C41 As2 C51 C52A -29.5(17) . . . . ? C61 As2 C51 C52A 78.6(17) . . . . ? Pd1 As2 C51 C52A -158.6(17) . . . . ? C41 As2 C51 C52 -64.8(9) . . . . ? C61 As2 C51 C52 43.4(9) . . . . ? Pd1 As2 C51 C52 166.2(8) . . . . ? C52A C51 C52 C53 22(3) . . . . ? As2 C51 C52 C53 104.1(13) . . . . ? C52 C51 C52A C53A -10(3) . . . . ? As2 C51 C52A C53A -121(4) . . . . ? C51 As2 C61 C62A 51.3(10) . . . . ? C41 As2 C61 C62A 160.5(10) . . . . ? Pd1 As2 C61 C62A -75.8(10) . . . . ? C51 As2 C61 C62 89.2(10) . . . . ? C41 As2 C61 C62 -161.6(10) . . . . ? Pd1 As2 C61 C62 -37.8(10) . . . . ? C62A C61 C62 C63 -7.2(17) . . . . ? As2 C61 C62 C63 -110.5(18) . . . . ? C62 C61 C62A C63A -6.4(19) . . . . ? As2 C61 C62A C63A 84.8(17) . . . . ? C91 As3 C71 C72 -44.1(15) . . . . ? C81 As3 C71 C72 -153.2(15) . . . . ? Pd2 As3 C71 C72 85.0(15) . . . . ? C91 As3 C71 C72A -79.4(8) . . . . ? C81 As3 C71 C72A 171.5(8) . . . . ? Pd2 As3 C71 C72A 49.7(8) . . . . ? C72A C71 C72 C73 0(2) . . . . ? As3 C71 C72 C73 -86(3) . . . . ? C72 C71 C72A C73A 5(3) . . . . ? As3 C71 C72A C73A 112.9(12) . . . . ? C91 As3 C81 C82A 59.7(8) . . . . ? C71 As3 C81 C82A 168.5(8) . . . . ? Pd2 As3 C81 C82A -69.3(8) . . . . ? C91 As3 C81 C82 96.7(17) . . . . ? C71 As3 C81 C82 -154.6(16) . . . . ? Pd2 As3 C81 C82 -32.4(17) . . . . ? C82A C81 C82 C83 -15(2) . . . . ? As3 C81 C82 C83 -113(3) . . . . ? C82 C81 C82A C83A -4(3) . . . . ? As3 C81 C82A C83A 91.9(14) . . . . ? C81 As3 C91 C92 35.9(15) . . . . ? C71 As3 C91 C92 -71.8(15) . . . . ? Pd2 As3 C91 C92 161.9(14) . . . . ? C81 As3 C91 C92A 68.9(10) . . . . ? C71 As3 C91 C92A -38.7(11) . . . . ? Pd2 As3 C91 C92A -165.0(9) . . . . ? C92A C91 C92 C93 16(2) . . . . ? As3 C91 C92 C93 111(3) . . . . ? C92 C91 C92A C93A -9(3) . . . . ? As3 C91 C92A C93A -106.8(16) . . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 24.12 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.550 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.075 #======================================================================= data_jain02a _database_code_CSD 214027 _chemical_name_common trans-Dichlorobis(tri(methylallyl)arsine)palladium(ii) _audit_creation_method SHELXL-97 _chemical_name_systematic trans-Dichlorobis(tri(methylallyl)arsine)palladium(II) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 As2 Cl2 Pd' _chemical_formula_weight 657.72 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9820(9) _cell_length_b 9.366(2) _cell_length_c 10.1692(9) _cell_angle_alpha 68.166(12) _cell_angle_beta 82.138(9) _cell_angle_gamma 77.166(11) _cell_volume 686.81(18) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'orange red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 332 _exptl_absorpt_coefficient_mu 3.270 _exptl_absorpt_correction_type ; empirical - XABS2 (S. Parkin, B. Moezzi, H. Hope, J. Appl. Cryst. 1995, 28, 53.) ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens-P4 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3471 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3237 _reflns_number_gt 2675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^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 3237 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0992 _refine_ls_wR_factor_gt 0.0937 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 1.140 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.0000 0.5000 0.01927(11) Uani 1 2 d S . . As1 As 0.70185(4) -0.17932(4) 0.66853(3) 0.01986(11) Uani 1 1 d . . . Cl1 Cl 0.71804(12) 0.13496(12) 0.38945(11) 0.0370(2) Uani 1 1 d . . . C11 C 0.8869(4) -0.3005(4) 0.5841(4) 0.0253(7) Uani 1 1 d . . . H11A H 0.9833 -0.2426 0.5486 0.030 Uiso 1 1 calc R . . H11B H 0.9300 -0.4015 0.6584 0.030 Uiso 1 1 calc R . . C12 C 0.8301(4) -0.3318(4) 0.4642(4) 0.0262(7) Uani 1 1 d . . . C13 C 0.8848(6) -0.2633(5) 0.3317(4) 0.0384(9) Uani 1 1 d . . . H13A H 0.8470 -0.2847 0.2575 0.046 Uiso 1 1 calc R . . H13B H 0.9619 -0.1926 0.3105 0.046 Uiso 1 1 calc R . . C14 C 0.7085(6) -0.4441(5) 0.5028(5) 0.0409(10) Uani 1 1 d . . . H14A H 0.6827 -0.4572 0.4169 0.061 Uiso 1 1 calc R . . H14B H 0.6016 -0.4030 0.5475 0.061 Uiso 1 1 calc R . . H14C H 0.7615 -0.5456 0.5692 0.061 Uiso 1 1 calc R . . C21 C 0.8373(4) -0.0797(4) 0.7447(4) 0.0266(7) Uani 1 1 d . . . H21A H 0.9268 -0.1618 0.8023 0.032 Uiso 1 1 calc R . . H21B H 0.8968 -0.0071 0.6643 0.032 Uiso 1 1 calc R . . C22 C 0.7356(5) 0.0094(4) 0.8344(4) 0.0294(8) Uani 1 1 d . . . C23 C 0.7818(7) -0.0167(5) 0.9615(5) 0.0435(11) Uani 1 1 d . . . H23A H 0.8808 -0.0928 0.9978 0.052 Uiso 1 1 calc R . . H23B H 0.7164 0.0406 1.0172 0.052 Uiso 1 1 calc R . . C24 C 0.5855(6) 0.1334(5) 0.7681(5) 0.0459(11) Uani 1 1 d . . . H24A H 0.5316 0.1864 0.8344 0.069 Uiso 1 1 calc R . . H24B H 0.5013 0.0847 0.7464 0.069 Uiso 1 1 calc R . . H24C H 0.6259 0.2098 0.6804 0.069 Uiso 1 1 calc R . . C31 C 0.5990(5) -0.3280(4) 0.8354(4) 0.0296(8) Uani 1 1 d . . . H31A H 0.5271 -0.2679 0.8917 0.036 Uiso 1 1 calc R . . H31B H 0.5208 -0.3736 0.8013 0.036 Uiso 1 1 calc R . . C32 C 0.7167(5) -0.4595(4) 0.9328(4) 0.0296(8) Uani 1 1 d . . . C33 C 0.7680(6) -0.5988(5) 0.9123(5) 0.0401(10) Uani 1 1 d . . . H33A H 0.8374 -0.6837 0.9787 0.048 Uiso 1 1 calc R . . H33B H 0.7343 -0.6111 0.8316 0.048 Uiso 1 1 calc R . . C34 C 0.7670(6) -0.4386(5) 1.0557(5) 0.0409(10) Uani 1 1 d . . . H34A H 0.8327 -0.5376 1.1162 0.061 Uiso 1 1 calc R . . H34B H 0.6638 -0.4062 1.1097 0.061 Uiso 1 1 calc R . . H34C H 0.8385 -0.3579 1.0241 0.061 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 0.01440(17) 0.01915(18) 0.02215(19) -0.00576(13) 0.00150(13) -0.00318(13) As1 0.01618(18) 0.01933(18) 0.02182(19) -0.00600(13) 0.00131(13) -0.00256(13) Cl1 0.0218(4) 0.0390(5) 0.0396(5) 0.0019(4) -0.0007(4) -0.0127(4) C11 0.0213(16) 0.0266(17) 0.0283(18) -0.0135(14) 0.0032(13) -0.0010(13) C12 0.0218(16) 0.0264(17) 0.0327(19) -0.0149(15) -0.0009(14) -0.0013(13) C13 0.043(2) 0.043(2) 0.032(2) -0.0166(18) 0.0023(18) -0.0101(19) C14 0.042(2) 0.039(2) 0.049(3) -0.022(2) -0.001(2) -0.0116(19) C21 0.0195(16) 0.0296(18) 0.0316(19) -0.0113(15) -0.0015(14) -0.0054(14) C22 0.0320(19) 0.0255(17) 0.0342(19) -0.0125(15) 0.0038(15) -0.0125(15) C23 0.065(3) 0.031(2) 0.038(2) -0.0158(18) 0.001(2) -0.011(2) C24 0.041(2) 0.041(2) 0.066(3) -0.035(2) -0.004(2) 0.0019(19) C31 0.0217(17) 0.0317(19) 0.0270(18) -0.0028(15) 0.0044(14) -0.0052(14) C32 0.0259(18) 0.0304(18) 0.0259(18) -0.0018(14) 0.0017(14) -0.0084(15) C33 0.053(3) 0.0273(19) 0.036(2) -0.0084(17) -0.0007(19) -0.0048(18) C34 0.053(3) 0.033(2) 0.036(2) -0.0106(17) -0.0076(19) -0.0079(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.2968(10) . ? Pd1 Cl1 2.2968(10) 2_656 ? Pd1 As1 2.4012(5) 2_656 ? Pd1 As1 2.4012(5) . ? As1 C11 1.959(3) . ? As1 C21 1.963(3) . ? As1 C31 1.965(3) . ? C11 C12 1.501(5) . ? C12 C13 1.318(5) . ? C12 C14 1.499(5) . ? C21 C22 1.500(5) . ? C22 C23 1.312(6) . ? C22 C24 1.502(6) . ? C31 C32 1.487(5) . ? C32 C33 1.362(5) . ? C32 C34 1.455(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 Cl1 Pd1 Cl1 180.00(5) . 2_656 ? Cl1 Pd1 As1 92.35(3) . 2_656 ? Cl1 Pd1 As1 87.65(3) 2_656 2_656 ? Cl1 Pd1 As1 87.65(3) . . ? Cl1 Pd1 As1 92.35(3) 2_656 . ? As1 Pd1 As1 180.000(14) 2_656 . ? C11 As1 C21 100.31(15) . . ? C11 As1 C31 107.71(15) . . ? C21 As1 C31 105.41(16) . . ? C11 As1 Pd1 112.85(11) . . ? C21 As1 Pd1 114.68(11) . . ? C31 As1 Pd1 114.63(11) . . ? C12 C11 As1 112.9(2) . . ? C13 C12 C14 121.9(4) . . ? C13 C12 C11 121.4(3) . . ? C14 C12 C11 116.7(3) . . ? C22 C21 As1 115.0(2) . . ? C23 C22 C21 120.8(4) . . ? C23 C22 C24 122.6(4) . . ? C21 C22 C24 116.5(4) . . ? C32 C31 As1 118.1(2) . . ? C33 C32 C34 120.7(4) . . ? C33 C32 C31 121.0(4) . . ? C34 C32 C31 118.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 As1 C11 -66.60(12) . . . . ? Cl1 Pd1 As1 C11 113.40(12) 2_656 . . . ? As1 Pd1 As1 C11 101(100) 2_656 . . . ? Cl1 Pd1 As1 C21 47.43(12) . . . . ? Cl1 Pd1 As1 C21 -132.57(12) 2_656 . . . ? As1 Pd1 As1 C21 -145(100) 2_656 . . . ? Cl1 Pd1 As1 C31 169.59(13) . . . . ? Cl1 Pd1 As1 C31 -10.41(13) 2_656 . . . ? As1 Pd1 As1 C31 -23(100) 2_656 . . . ? C21 As1 C11 C12 -154.1(3) . . . . ? C31 As1 C11 C12 95.9(3) . . . . ? Pd1 As1 C11 C12 -31.6(3) . . . . ? As1 C11 C12 C13 109.9(4) . . . . ? As1 C11 C12 C14 -70.0(4) . . . . ? C11 As1 C21 C22 -172.9(3) . . . . ? C31 As1 C21 C22 -61.1(3) . . . . ? Pd1 As1 C21 C22 65.9(3) . . . . ? As1 C21 C22 C23 128.2(4) . . . . ? As1 C21 C22 C24 -54.6(4) . . . . ? C11 As1 C31 C32 43.6(3) . . . . ? C21 As1 C31 C32 -62.9(3) . . . . ? Pd1 As1 C31 C32 170.1(3) . . . . ? As1 C31 C32 C33 -89.8(4) . . . . ? As1 C31 C32 C34 94.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.699 _refine_diff_density_min -1.209 _refine_diff_density_rms 0.123 #=========================================================================== data_jain07 _database_code_CSD 214028 _chemical_name_common trans-Dibromobis(tri(methylallyl)arsine)palladium(ii) _audit_creation_method SHELXL-97 _chemical_name_systematic trans-Dibromobis(tri(methylallyl)arsine)palladium(II) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 As2 Br2 Pd' _chemical_formula_weight 746.64 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' As As 0.0499 2.0058 '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' _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 8.8295(17) _cell_length_b 9.4059(14) _cell_length_c 9.5258(19) _cell_angle_alpha 108.471(13) _cell_angle_beta 103.331(14) _cell_angle_gamma 96.937(12) _cell_volume 713.9(2) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 368 _exptl_absorpt_coefficient_mu 5.758 _exptl_absorpt_correction_type ; empirical - XABS2 (S. Parkin, B. Moezzi, H. Hope, J. Appl. Cryst. 1995, 28, 53.) ; _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens-P4 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3581 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3366 _reflns_number_gt 2744 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.1565P] 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 3366 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0835 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.5000 0.5000 0.0000 0.01694(11) Uani 1 2 d S . . As1 As 0.69805(4) 0.60612(4) -0.09741(4) 0.01783(11) Uani 1 1 d . . . Br1 Br 0.71076(5) 0.41935(6) 0.15294(6) 0.03245(13) Uani 1 1 d . . . C1 C 0.8242(5) 0.4568(5) -0.1764(5) 0.0234(8) Uani 1 1 d . . . H1A H 0.9270 0.5128 -0.1754 0.028 Uiso 1 1 calc R . . H1B H 0.8474 0.3987 -0.1064 0.028 Uiso 1 1 calc R . . C2 C 0.7415(5) 0.3454(5) -0.3378(5) 0.0314(10) Uani 1 1 d . . . C3 C 0.8081(7) 0.3305(6) -0.4498(6) 0.0470(13) Uani 1 1 d . . . H3A H 0.9105 0.3905 -0.4300 0.056 Uiso 1 1 calc R . . H3B H 0.7540 0.2596 -0.5508 0.056 Uiso 1 1 calc R . . C4 C 0.5804(6) 0.2514(6) -0.3607(7) 0.0440(12) Uani 1 1 d . . . H4A H 0.5369 0.1836 -0.4691 0.066 Uiso 1 1 calc R . . H4B H 0.5081 0.3200 -0.3333 0.066 Uiso 1 1 calc R . . H4C H 0.5916 0.1897 -0.2946 0.066 Uiso 1 1 calc R . . C11 C 0.8604(5) 0.7733(4) 0.0691(5) 0.0238(8) Uani 1 1 d . . . H11A H 0.9426 0.7289 0.1205 0.029 Uiso 1 1 calc R . . H11B H 0.9128 0.8393 0.0236 0.029 Uiso 1 1 calc R . . C12 C 0.7924(5) 0.8704(5) 0.1881(5) 0.0273(9) Uani 1 1 d . . . C13 C 0.8330(6) 0.8733(6) 0.3321(6) 0.0406(11) Uani 1 1 d . . . H13A H 0.7885 0.9338 0.4060 0.049 Uiso 1 1 calc R . . H13B H 0.9067 0.8148 0.3613 0.049 Uiso 1 1 calc R . . C14 C 0.6773(7) 0.9598(6) 0.1352(6) 0.0453(13) Uani 1 1 d . . . H14A H 0.6416 1.0182 0.2222 0.068 Uiso 1 1 calc R . . H14B H 0.5853 0.8893 0.0530 0.068 Uiso 1 1 calc R . . H14C H 0.7293 1.0306 0.0958 0.068 Uiso 1 1 calc R . . C21 C 0.6311(5) 0.6870(5) -0.2644(5) 0.0270(9) Uani 1 1 d . . . H21A H 0.5953 0.5998 -0.3641 0.032 Uiso 1 1 calc R . . H21B H 0.5382 0.7333 -0.2503 0.032 Uiso 1 1 calc R . . C22 C 0.7557(5) 0.8044(5) -0.2748(5) 0.0265(9) Uani 1 1 d . . . C23 C 0.7459(6) 0.9497(6) -0.2375(6) 0.0408(11) Uani 1 1 d . . . H23A H 0.8237 1.0211 -0.2487 0.049 Uiso 1 1 calc R . . H23B H 0.6610 0.9831 -0.1993 0.049 Uiso 1 1 calc R . . C24 C 0.8885(6) 0.7479(6) -0.3355(7) 0.0447(13) Uani 1 1 d . . . H24A H 0.9616 0.8345 -0.3364 0.067 Uiso 1 1 calc R . . H24B H 0.8441 0.6729 -0.4408 0.067 Uiso 1 1 calc R . . H24C H 0.9462 0.6994 -0.2690 0.067 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 0.01314(19) 0.0188(2) 0.0213(2) 0.01037(16) 0.00483(15) 0.00316(15) As1 0.01414(18) 0.0200(2) 0.0210(2) 0.01000(16) 0.00491(14) 0.00238(14) Br1 0.0187(2) 0.0486(3) 0.0431(3) 0.0332(2) 0.00813(17) 0.01023(18) C1 0.0169(18) 0.030(2) 0.025(2) 0.0112(17) 0.0061(15) 0.0084(16) C2 0.029(2) 0.028(2) 0.035(2) 0.0100(19) 0.0054(19) 0.0112(18) C3 0.060(4) 0.045(3) 0.035(3) 0.006(2) 0.019(3) 0.018(3) C4 0.039(3) 0.030(3) 0.048(3) 0.008(2) -0.001(2) -0.002(2) C11 0.0185(18) 0.023(2) 0.027(2) 0.0091(17) 0.0029(16) 0.0013(15) C12 0.026(2) 0.0170(19) 0.032(2) 0.0063(17) 0.0018(17) -0.0015(16) C13 0.048(3) 0.036(3) 0.032(3) 0.006(2) 0.011(2) 0.006(2) C14 0.049(3) 0.032(3) 0.046(3) 0.003(2) 0.006(2) 0.017(2) C21 0.0197(19) 0.035(2) 0.029(2) 0.0192(19) 0.0032(16) 0.0016(17) C22 0.023(2) 0.035(2) 0.025(2) 0.0193(18) 0.0051(16) 0.0013(17) C23 0.036(3) 0.040(3) 0.051(3) 0.026(2) 0.009(2) 0.001(2) C24 0.041(3) 0.054(3) 0.055(3) 0.034(3) 0.025(3) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 As1 2.4143(5) . ? Pd1 As1 2.4143(5) 2_665 ? Pd1 Br1 2.4397(6) 2_665 ? Pd1 Br1 2.4397(6) . ? As1 C11 1.967(4) . ? As1 C1 1.968(4) . ? As1 C21 1.975(4) . ? C1 C2 1.507(6) . ? C2 C3 1.311(7) . ? C2 C4 1.511(7) . ? C11 C12 1.507(6) . ? C12 C13 1.326(7) . ? C12 C14 1.494(6) . ? C21 C22 1.505(5) . ? C22 C23 1.318(6) . ? C22 C24 1.504(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 As1 Pd1 As1 180.0 . 2_665 ? As1 Pd1 Br1 92.02(2) . 2_665 ? As1 Pd1 Br1 87.98(2) 2_665 2_665 ? As1 Pd1 Br1 87.98(2) . . ? As1 Pd1 Br1 92.02(2) 2_665 . ? Br1 Pd1 Br1 180.00(2) 2_665 . ? C11 As1 C1 102.71(16) . . ? C11 As1 C21 105.55(17) . . ? C1 As1 C21 104.20(18) . . ? C11 As1 Pd1 111.32(12) . . ? C1 As1 Pd1 111.91(12) . . ? C21 As1 Pd1 119.58(12) . . ? C2 C1 As1 113.2(3) . . ? C3 C2 C1 121.3(5) . . ? C3 C2 C4 122.7(5) . . ? C1 C2 C4 116.0(4) . . ? C12 C11 As1 112.9(3) . . ? C13 C12 C14 122.5(4) . . ? C13 C12 C11 120.6(4) . . ? C14 C12 C11 116.9(4) . . ? C22 C21 As1 115.9(3) . . ? C23 C22 C24 121.3(4) . . ? C23 C22 C21 121.5(4) . . ? C24 C22 C21 117.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag As1 Pd1 As1 C11 -97(100) 2_665 . . . ? Br1 Pd1 As1 C11 116.52(13) 2_665 . . . ? Br1 Pd1 As1 C11 -63.48(13) . . . . ? As1 Pd1 As1 C1 17(100) 2_665 . . . ? Br1 Pd1 As1 C1 -129.18(13) 2_665 . . . ? Br1 Pd1 As1 C1 50.82(13) . . . . ? As1 Pd1 As1 C21 140(100) 2_665 . . . ? Br1 Pd1 As1 C21 -7.02(15) 2_665 . . . ? Br1 Pd1 As1 C21 172.98(15) . . . . ? C11 As1 C1 C2 -159.4(3) . . . . ? C21 As1 C1 C2 -49.4(3) . . . . ? Pd1 As1 C1 C2 81.1(3) . . . . ? As1 C1 C2 C3 123.4(4) . . . . ? As1 C1 C2 C4 -57.7(5) . . . . ? C1 As1 C11 C12 -156.7(3) . . . . ? C21 As1 C11 C12 94.4(3) . . . . ? Pd1 As1 C11 C12 -36.8(3) . . . . ? As1 C11 C12 C13 114.6(4) . . . . ? As1 C11 C12 C14 -64.5(4) . . . . ? C11 As1 C21 C22 29.8(4) . . . . ? C1 As1 C21 C22 -78.0(4) . . . . ? Pd1 As1 C21 C22 156.1(3) . . . . ? As1 C21 C22 C23 -109.2(4) . . . . ? As1 C21 C22 C24 73.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.511 _refine_diff_density_min -0.962 _refine_diff_density_rms 0.153 #============================================================================ data_jain03a _database_code_CSD 214029 _chemical_name_common trans-Dichlorobis(tri(methylallyl)arsine)platinum(ii) _audit_creation_method SHELXL-97 _chemical_name_systematic trans-Dichlorobis(tri(methylallyl)arsine)platinum(II) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 As2 Cl2 Pt' _chemical_formula_weight 746.41 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.6461(16) _cell_length_b 9.4107(17) _cell_length_c 9.532(3) _cell_angle_alpha 108.190(17) _cell_angle_beta 102.878(18) _cell_angle_gamma 97.604(14) _cell_volume 701.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 364 _exptl_absorpt_coefficient_mu 7.546 _exptl_absorpt_correction_type 'empirical - psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens-P4 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3522 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.00 _reflns_number_total 3307 _reflns_number_gt 3013 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0398P)^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 3307 _refine_ls_number_parameters 136 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0700 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Pt1 Pt 0.5000 0.5000 0.0000 0.02038(7) Uani 1 2 d S . . As1 As 0.69908(4) 0.60778(4) -0.09799(4) 0.02117(10) Uani 1 1 d . . . Cl1 Cl 0.70371(12) 0.42176(16) 0.13934(15) 0.0409(3) Uani 1 1 d . . . C11 C 0.8647(5) 0.7762(5) 0.0637(5) 0.0288(8) Uani 1 1 d . . . H11A H 0.9504 0.7335 0.1138 0.035 Uiso 1 1 calc R . . H11B H 0.9158 0.8426 0.0164 0.035 Uiso 1 1 calc R . . C12 C 0.7975(5) 0.8716(5) 0.1835(5) 0.0317(9) Uani 1 1 d . . . C13 C 0.8378(6) 0.8723(6) 0.3253(6) 0.0433(12) Uani 1 1 d . . . H13A H 0.7938 0.9330 0.4001 0.052 Uiso 1 1 calc R . . H13B H 0.9108 0.8121 0.3529 0.052 Uiso 1 1 calc R . . C14 C 0.6837(7) 0.9639(7) 0.1344(7) 0.0539(15) Uani 1 1 d . . . H14A H 0.6472 1.0202 0.2218 0.081 Uiso 1 1 calc R . . H14B H 0.5895 0.8956 0.0512 0.081 Uiso 1 1 calc R . . H14C H 0.7395 1.0368 0.0978 0.081 Uiso 1 1 calc R . . C21 C 0.6243(5) 0.6861(5) -0.2637(5) 0.0300(9) Uani 1 1 d . . . H21A H 0.5842 0.5980 -0.3620 0.036 Uiso 1 1 calc R . . H21B H 0.5309 0.7324 -0.2459 0.036 Uiso 1 1 calc R . . C22 C 0.7474(5) 0.8020(5) -0.2815(5) 0.0315(9) Uani 1 1 d . . . C23 C 0.7387(6) 0.9459(6) -0.2435(6) 0.0423(11) Uani 1 1 d . . . H23A H 0.6530 0.9789 -0.2037 0.051 Uiso 1 1 calc R . . H23B H 0.8181 1.0177 -0.2558 0.051 Uiso 1 1 calc R . . C24 C 0.8796(7) 0.7445(7) -0.3471(7) 0.0493(13) Uani 1 1 d . . . H24A H 0.9500 0.8295 -0.3567 0.074 Uiso 1 1 calc R . . H24B H 0.8308 0.6647 -0.4487 0.074 Uiso 1 1 calc R . . H24C H 0.9442 0.7018 -0.2786 0.074 Uiso 1 1 calc R . . C31 C 0.8261(5) 0.4588(5) -0.1773(5) 0.0284(8) Uani 1 1 d . . . H31A H 0.9314 0.5150 -0.1773 0.034 Uiso 1 1 calc R . . H31B H 0.8495 0.4010 -0.1071 0.034 Uiso 1 1 calc R . . C32 C 0.7421(6) 0.3479(6) -0.3362(6) 0.0363(10) Uani 1 1 d . . . C33 C 0.8109(8) 0.3343(7) -0.4479(6) 0.0527(14) Uani 1 1 d . . . H33A H 0.9154 0.3954 -0.4283 0.063 Uiso 1 1 calc R . . H33B H 0.7562 0.2633 -0.5484 0.063 Uiso 1 1 calc R . . C34 C 0.5787(7) 0.2524(6) -0.3587(7) 0.0489(13) Uani 1 1 d . . . H34A H 0.5454 0.1702 -0.4597 0.073 Uiso 1 1 calc R . . H34B H 0.4986 0.3171 -0.3531 0.073 Uiso 1 1 calc R . . H34C H 0.5855 0.2076 -0.2781 0.073 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 Pt1 0.01659(10) 0.02017(12) 0.02629(11) 0.01089(8) 0.00555(7) 0.00454(7) As1 0.01685(19) 0.0221(2) 0.0256(2) 0.01051(17) 0.00513(15) 0.00373(16) Cl1 0.0230(5) 0.0613(8) 0.0570(7) 0.0430(6) 0.0117(5) 0.0157(5) C11 0.0207(18) 0.027(2) 0.036(2) 0.0100(17) 0.0042(16) 0.0029(15) C12 0.026(2) 0.026(2) 0.032(2) 0.0018(17) 0.0029(16) -0.0019(16) C13 0.045(3) 0.038(3) 0.038(2) 0.007(2) 0.007(2) 0.003(2) C14 0.060(3) 0.041(3) 0.051(3) 0.005(3) 0.005(3) 0.026(3) C21 0.026(2) 0.036(2) 0.031(2) 0.0204(19) 0.0035(16) 0.0035(17) C22 0.028(2) 0.035(2) 0.034(2) 0.0190(19) 0.0062(17) 0.0032(17) C23 0.037(2) 0.039(3) 0.055(3) 0.027(2) 0.010(2) 0.007(2) C24 0.051(3) 0.055(3) 0.062(3) 0.033(3) 0.033(3) 0.016(3) C31 0.0229(18) 0.031(2) 0.033(2) 0.0111(18) 0.0093(16) 0.0109(16) C32 0.037(2) 0.030(2) 0.040(2) 0.0088(19) 0.008(2) 0.0123(19) C33 0.065(4) 0.047(3) 0.041(3) 0.002(2) 0.022(3) 0.015(3) C34 0.044(3) 0.032(3) 0.052(3) 0.004(2) -0.003(2) 0.001(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 Pt1 Cl1 2.3063(11) 2_665 ? Pt1 Cl1 2.3063(11) . ? Pt1 As1 2.3895(5) . ? Pt1 As1 2.3895(5) 2_665 ? As1 C11 1.957(4) . ? As1 C21 1.963(4) . ? As1 C31 1.964(4) . ? C11 C12 1.497(6) . ? C12 C13 1.316(7) . ? C12 C14 1.489(7) . ? C21 C22 1.497(6) . ? C22 C23 1.305(7) . ? C22 C24 1.504(7) . ? C31 C32 1.494(6) . ? C32 C33 1.312(8) . ? C32 C34 1.503(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 Cl1 Pt1 Cl1 180.00(6) 2_665 . ? Cl1 Pt1 As1 92.06(3) 2_665 . ? Cl1 Pt1 As1 87.94(3) . . ? Cl1 Pt1 As1 87.94(3) 2_665 2_665 ? Cl1 Pt1 As1 92.06(3) . 2_665 ? As1 Pt1 As1 180.0 . 2_665 ? C11 As1 C21 105.75(19) . . ? C11 As1 C31 103.03(17) . . ? C21 As1 C31 105.26(19) . . ? C11 As1 Pt1 112.12(13) . . ? C21 As1 Pt1 118.19(13) . . ? C31 As1 Pt1 111.18(13) . . ? C12 C11 As1 112.9(3) . . ? C13 C12 C14 122.1(5) . . ? C13 C12 C11 120.9(5) . . ? C14 C12 C11 117.0(4) . . ? C22 C21 As1 116.3(3) . . ? C23 C22 C21 121.3(5) . . ? C23 C22 C24 121.7(5) . . ? C21 C22 C24 116.9(4) . . ? C32 C31 As1 113.4(3) . . ? C33 C32 C31 120.8(5) . . ? C33 C32 C34 122.6(5) . . ? C31 C32 C34 116.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pt1 As1 C11 115.21(14) 2_665 . . . ? Cl1 Pt1 As1 C11 -64.79(14) . . . . ? As1 Pt1 As1 C11 -115(100) 2_665 . . . ? Cl1 Pt1 As1 C21 -8.18(16) 2_665 . . . ? Cl1 Pt1 As1 C21 171.82(16) . . . . ? As1 Pt1 As1 C21 122(100) 2_665 . . . ? Cl1 Pt1 As1 C31 -130.05(13) 2_665 . . . ? Cl1 Pt1 As1 C31 49.95(13) . . . . ? As1 Pt1 As1 C31 0(100) 2_665 . . . ? C21 As1 C11 C12 94.0(4) . . . . ? C31 As1 C11 C12 -155.7(3) . . . . ? Pt1 As1 C11 C12 -36.1(4) . . . . ? As1 C11 C12 C13 112.5(4) . . . . ? As1 C11 C12 C14 -67.2(5) . . . . ? C11 As1 C21 C22 31.2(4) . . . . ? C31 As1 C21 C22 -77.4(4) . . . . ? Pt1 As1 C21 C22 157.7(3) . . . . ? As1 C21 C22 C23 -108.4(5) . . . . ? As1 C21 C22 C24 72.5(5) . . . . ? C11 As1 C31 C32 -158.5(3) . . . . ? C21 As1 C31 C32 -47.9(4) . . . . ? Pt1 As1 C31 C32 81.2(3) . . . . ? As1 C31 C32 C33 123.0(5) . . . . ? As1 C31 C32 C34 -58.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.507 _refine_diff_density_min -1.836 _refine_diff_density_rms 0.141 #================================================================== data_jain06 _database_code_CSD 214030 _chemical_name_common ;trans-µ-Dichlorobis(chloro- tri(methylallyl)arsinepalladium(ii)) ; _audit_creation_method SHELXL-97 _chemical_name_systematic trans-µ-Dichlorobis(chloro-tri(methylallyl)arsinepalladium(II)) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H42 As2 Cl4 Pd2' _chemical_formula_weight 835.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.7802(15) _cell_length_b 10.0937(16) _cell_length_c 20.620(3) _cell_angle_alpha 94.326(12) _cell_angle_beta 98.760(13) _cell_angle_gamma 100.107(14) _cell_volume 1566.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'brown red' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.770 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 3.596 _exptl_absorpt_correction_type 'empirical - psi scans' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ? _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Siemens-P4 _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7514 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.00 _reflns_number_total 7514 _reflns_number_gt 5602 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0580P)^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 7514 _refine_ls_number_parameters 295 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0490 _refine_ls_wR_factor_ref 0.1270 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.189 _refine_ls_restrained_S_all 1.189 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.48595(6) 0.59894(4) 0.329046(19) 0.02848(11) Uani 1 1 d . . . Pd2 Pd 0.45849(6) 0.34760(4) 0.21116(2) 0.02954(11) Uani 1 1 d . . . Cl1 Cl 0.7178(2) 0.76320(15) 0.37731(8) 0.0432(4) Uani 1 1 d . . . Cl2 Cl 0.2388(2) 0.25196(16) 0.12554(7) 0.0429(3) Uani 1 1 d . . . Cl3 Cl 0.2550(2) 0.42699(15) 0.27815(8) 0.0408(3) Uani 1 1 d . . . Cl4 Cl 0.6842(2) 0.45557(15) 0.29520(7) 0.0404(3) Uani 1 1 d . . . As1 As 0.28223(8) 0.72740(6) 0.35965(3) 0.03105(14) Uani 1 1 d . . . As2 As 0.67447(8) 0.28401(5) 0.15478(3) 0.02982(14) Uani 1 1 d . . . C11 C 0.3924(9) 0.9048(6) 0.4077(4) 0.0536(18) Uani 1 1 d . . . H11A H 0.4285 0.8911 0.4545 0.064 Uiso 1 1 calc R . . H11B H 0.5019 0.9378 0.3902 0.064 Uiso 1 1 calc R . . C12 C 0.2860(10) 1.0144(7) 0.4061(4) 0.0526(18) Uani 1 1 d . . . C13 C 0.3204(14) 1.1135(8) 0.3679(5) 0.086(3) Uani 1 1 d . . . H13A H 0.2565 1.1855 0.3678 0.103 Uiso 1 1 calc R . . H13B H 0.4088 1.1120 0.3409 0.103 Uiso 1 1 calc R . . C14 C 0.1510(12) 1.0107(9) 0.4490(5) 0.071(2) Uani 1 1 d . . . H14A H 0.1057 1.0954 0.4489 0.107 Uiso 1 1 calc R . . H14B H 0.2038 0.9998 0.4941 0.107 Uiso 1 1 calc R . . H14C H 0.0533 0.9345 0.4327 0.107 Uiso 1 1 calc R . . C21 C 0.1050(8) 0.7551(7) 0.2858(3) 0.0423(14) Uani 1 1 d . . . H21A H 0.0262 0.6667 0.2701 0.051 Uiso 1 1 calc R . . H21B H 0.0314 0.8156 0.3030 0.051 Uiso 1 1 calc R . . C22 C 0.1709(9) 0.8127(7) 0.2275(3) 0.0454(15) Uani 1 1 d . . . C23 C 0.1462(12) 0.9353(9) 0.2131(4) 0.071(2) Uani 1 1 d . . . H23A H 0.0866 0.9861 0.2399 0.085 Uiso 1 1 calc R . . H23B H 0.1882 0.9717 0.1760 0.085 Uiso 1 1 calc R . . C24 C 0.2588(11) 0.7268(7) 0.1856(3) 0.0541(18) Uani 1 1 d . . . H24A H 0.2960 0.7766 0.1495 0.081 Uiso 1 1 calc R . . H24B H 0.1752 0.6433 0.1673 0.081 Uiso 1 1 calc R . . H24C H 0.3627 0.7044 0.2126 0.081 Uiso 1 1 calc R . . C31 C 0.1272(9) 0.6316(7) 0.4142(3) 0.0418(14) Uani 1 1 d . . . H31A H 0.0474 0.6914 0.4272 0.050 Uiso 1 1 calc R . . H31B H 0.0523 0.5510 0.3870 0.050 Uiso 1 1 calc R . . C32 C 0.2192(10) 0.5865(8) 0.4752(3) 0.0525(17) Uani 1 1 d . . . C33 C 0.2587(15) 0.6679(10) 0.5316(4) 0.093(3) Uani 1 1 d . . . H33A H 0.2283 0.7551 0.5331 0.112 Uiso 1 1 calc R . . H33B H 0.3173 0.6387 0.5702 0.112 Uiso 1 1 calc R . . C34 C 0.2615(13) 0.4470(8) 0.4685(4) 0.075(3) Uani 1 1 d . . . H34A H 0.2902 0.4177 0.5125 0.112 Uiso 1 1 calc R . . H34B H 0.3631 0.4484 0.4456 0.112 Uiso 1 1 calc R . . H34C H 0.1588 0.3840 0.4432 0.112 Uiso 1 1 calc R . . C41 C 0.5864(8) 0.1700(7) 0.0717(3) 0.0436(15) Uani 1 1 d . . . H41A H 0.4971 0.0931 0.0798 0.052 Uiso 1 1 calc R . . H41B H 0.5248 0.2233 0.0406 0.052 Uiso 1 1 calc R . . C42 C 0.7222(10) 0.1134(8) 0.0382(3) 0.0538(18) Uani 1 1 d . . . C43 C 0.7974(14) 0.1828(11) -0.0079(4) 0.088(3) Uani 1 1 d . . . H43A H 0.8822 0.1479 -0.0294 0.106 Uiso 1 1 calc R . . H43B H 0.7650 0.2661 -0.0185 0.106 Uiso 1 1 calc R . . C44 C 0.7705(13) -0.0151(9) 0.0551(4) 0.077(3) Uani 1 1 d . . . H44A H 0.8151 -0.0568 0.0182 0.116 Uiso 1 1 calc R . . H44B H 0.6660 -0.0760 0.0641 0.116 Uiso 1 1 calc R . . H44C H 0.8628 0.0015 0.0944 0.116 Uiso 1 1 calc R . . C51 C 0.8447(8) 0.2020(6) 0.2109(3) 0.0347(12) Uani 1 1 d . . . H51A H 0.9098 0.1541 0.1820 0.042 Uiso 1 1 calc R . . H51B H 0.9320 0.2758 0.2385 0.042 Uiso 1 1 calc R . . C52 C 0.7707(8) 0.1048(6) 0.2555(3) 0.0384(13) Uani 1 1 d . . . C53 C 0.8162(12) 0.1336(8) 0.3207(3) 0.061(2) Uani 1 1 d . . . H53A H 0.7694 0.0725 0.3492 0.073 Uiso 1 1 calc R . . H53B H 0.8954 0.2154 0.3385 0.073 Uiso 1 1 calc R . . C54 C 0.6491(12) -0.0197(8) 0.2253(4) 0.072(3) Uani 1 1 d . . . H54A H 0.5967 -0.0664 0.2596 0.109 Uiso 1 1 calc R . . H54B H 0.7142 -0.0787 0.2030 0.109 Uiso 1 1 calc R . . H54C H 0.5549 0.0028 0.1932 0.109 Uiso 1 1 calc R . . C61 C 0.8329(9) 0.4414(6) 0.1326(3) 0.0427(14) Uani 1 1 d . . . H61A H 0.8968 0.4952 0.1742 0.051 Uiso 1 1 calc R . . H61B H 0.9222 0.4089 0.1093 0.051 Uiso 1 1 calc R . . C62 C 0.7426(10) 0.5329(7) 0.0905(4) 0.0492(16) Uani 1 1 d . . . C63 C 0.7760(14) 0.5478(10) 0.0301(4) 0.087(3) Uani 1 1 d . . . H63A H 0.7254 0.6110 0.0051 0.105 Uiso 1 1 calc R . . H63B H 0.8505 0.4954 0.0117 0.105 Uiso 1 1 calc R . . C64 C 0.6263(14) 0.6132(8) 0.1211(5) 0.080(3) Uani 1 1 d . . . H64A H 0.5814 0.6721 0.0896 0.121 Uiso 1 1 calc R . . H64B H 0.6946 0.6686 0.1608 0.121 Uiso 1 1 calc R . . H64C H 0.5265 0.5516 0.1330 0.121 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 0.0339(2) 0.0252(2) 0.0250(2) 0.00219(15) 0.00462(16) 0.00252(16) Pd2 0.0349(2) 0.0246(2) 0.0279(2) 0.00228(16) 0.00575(17) 0.00219(16) Cl1 0.0372(8) 0.0333(7) 0.0534(9) -0.0024(6) 0.0003(7) 0.0008(6) Cl2 0.0369(8) 0.0504(9) 0.0377(7) 0.0000(6) 0.0043(6) 0.0020(7) Cl3 0.0386(8) 0.0343(7) 0.0462(8) -0.0067(6) 0.0122(6) -0.0015(6) Cl4 0.0405(8) 0.0406(8) 0.0370(7) -0.0080(6) 0.0009(6) 0.0096(6) As1 0.0366(3) 0.0292(3) 0.0265(3) 0.0021(2) 0.0041(2) 0.0054(2) As2 0.0339(3) 0.0272(3) 0.0266(3) 0.0019(2) 0.0049(2) 0.0016(2) C11 0.048(4) 0.035(3) 0.072(5) -0.015(3) 0.005(4) 0.003(3) C12 0.048(4) 0.041(4) 0.063(4) -0.014(3) 0.011(3) 0.002(3) C13 0.110(8) 0.039(4) 0.115(8) 0.009(5) 0.033(7) 0.016(5) C14 0.072(6) 0.060(5) 0.080(6) -0.017(4) 0.014(5) 0.018(4) C21 0.039(3) 0.052(4) 0.035(3) 0.011(3) 0.002(3) 0.008(3) C22 0.045(4) 0.054(4) 0.039(3) 0.020(3) 0.001(3) 0.013(3) C23 0.087(6) 0.069(5) 0.073(6) 0.034(4) 0.026(5) 0.036(5) C24 0.075(5) 0.053(4) 0.032(3) 0.011(3) 0.015(3) 0.000(4) C31 0.046(4) 0.054(4) 0.033(3) 0.010(3) 0.017(3) 0.017(3) C32 0.062(5) 0.063(4) 0.036(3) 0.015(3) 0.014(3) 0.012(4) C33 0.151(10) 0.104(8) 0.030(4) 0.012(4) 0.014(5) 0.037(7) C34 0.106(8) 0.069(6) 0.060(5) 0.029(4) 0.013(5) 0.039(5) C41 0.039(3) 0.050(4) 0.037(3) -0.012(3) 0.000(3) 0.007(3) C42 0.049(4) 0.069(5) 0.040(3) -0.015(3) 0.000(3) 0.017(4) C43 0.121(9) 0.101(8) 0.059(5) 0.009(5) 0.051(6) 0.033(7) C44 0.101(7) 0.078(6) 0.055(5) -0.014(4) 0.003(5) 0.039(6) C51 0.031(3) 0.035(3) 0.034(3) 0.003(2) 0.000(2) 0.000(2) C52 0.044(4) 0.032(3) 0.039(3) 0.006(2) 0.006(3) 0.007(3) C53 0.096(6) 0.051(4) 0.039(4) 0.014(3) 0.008(4) 0.022(4) C54 0.081(6) 0.056(5) 0.067(5) 0.024(4) -0.002(5) -0.020(4) C61 0.042(4) 0.038(3) 0.046(3) 0.009(3) 0.010(3) -0.003(3) C62 0.055(4) 0.041(4) 0.056(4) 0.020(3) 0.019(3) 0.007(3) C63 0.123(9) 0.096(7) 0.070(6) 0.052(5) 0.044(6) 0.054(7) C64 0.116(8) 0.050(5) 0.093(7) 0.033(5) 0.036(6) 0.038(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 Cl1 2.2686(16) . ? Pd1 Cl3 2.3236(15) . ? Pd1 As1 2.3439(8) . ? Pd1 Cl4 2.4329(16) . ? Pd2 Cl2 2.2835(16) . ? Pd2 Cl4 2.3218(15) . ? Pd2 As2 2.3341(8) . ? Pd2 Cl3 2.4498(16) . ? As1 C31 1.955(6) . ? As1 C11 1.964(6) . ? As1 C21 1.965(6) . ? As2 C41 1.949(6) . ? As2 C51 1.959(6) . ? As2 C61 1.961(6) . ? C11 C12 1.493(10) . ? C12 C13 1.334(12) . ? C12 C14 1.472(11) . ? C21 C22 1.494(9) . ? C22 C23 1.333(10) . ? C22 C24 1.497(10) . ? C31 C32 1.492(9) . ? C32 C33 1.334(10) . ? C32 C34 1.502(11) . ? C41 C42 1.514(9) . ? C42 C43 1.366(12) . ? C42 C44 1.465(11) . ? C51 C52 1.497(8) . ? C52 C53 1.333(9) . ? C52 C54 1.465(9) . ? C61 C62 1.504(9) . ? C62 C63 1.325(10) . ? C62 C64 1.493(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl3 178.13(6) . . ? Cl1 Pd1 As1 91.50(5) . . ? Cl3 Pd1 As1 90.35(4) . . ? Cl1 Pd1 Cl4 91.55(6) . . ? Cl3 Pd1 Cl4 86.60(5) . . ? As1 Pd1 Cl4 176.93(4) . . ? Cl2 Pd2 Cl4 176.82(6) . . ? Cl2 Pd2 As2 91.38(5) . . ? Cl4 Pd2 As2 88.31(4) . . ? Cl2 Pd2 Cl3 94.03(6) . . ? Cl4 Pd2 Cl3 86.24(5) . . ? As2 Pd2 Cl3 174.53(4) . . ? Pd1 Cl3 Pd2 88.54(5) . . ? Pd2 Cl4 Pd1 88.99(5) . . ? C31 As1 C11 107.7(3) . . ? C31 As1 C21 100.1(3) . . ? C11 As1 C21 108.3(3) . . ? C31 As1 Pd1 111.72(19) . . ? C11 As1 Pd1 113.9(2) . . ? C21 As1 Pd1 114.1(2) . . ? C41 As2 C51 110.0(3) . . ? C41 As2 C61 105.3(3) . . ? C51 As2 C61 100.4(3) . . ? C41 As2 Pd2 115.74(19) . . ? C51 As2 Pd2 112.19(18) . . ? C61 As2 Pd2 111.9(2) . . ? C12 C11 As1 118.1(5) . . ? C13 C12 C14 122.7(8) . . ? C13 C12 C11 119.3(8) . . ? C14 C12 C11 117.9(7) . . ? C22 C21 As1 117.6(4) . . ? C23 C22 C21 120.1(7) . . ? C23 C22 C24 122.0(7) . . ? C21 C22 C24 117.8(6) . . ? C32 C31 As1 115.5(5) . . ? C33 C32 C31 120.4(8) . . ? C33 C32 C34 123.5(8) . . ? C31 C32 C34 116.2(6) . . ? C42 C41 As2 116.8(4) . . ? C43 C42 C44 120.8(8) . . ? C43 C42 C41 119.3(8) . . ? C44 C42 C41 119.9(8) . . ? C52 C51 As2 116.7(4) . . ? C53 C52 C54 122.2(7) . . ? C53 C52 C51 119.6(6) . . ? C54 C52 C51 118.2(5) . . ? C62 C61 As2 114.9(5) . . ? C63 C62 C64 121.7(7) . . ? C63 C62 C61 120.6(7) . . ? C64 C62 C61 117.5(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 Cl3 Pd2 -13.9(19) . . . . ? As1 Pd1 Cl3 Pd2 157.85(4) . . . . ? Cl4 Pd1 Cl3 Pd2 -22.54(5) . . . . ? Cl2 Pd2 Cl3 Pd1 -153.13(6) . . . . ? Cl4 Pd2 Cl3 Pd1 23.69(6) . . . . ? As2 Pd2 Cl3 Pd1 18.1(5) . . . . ? Cl2 Pd2 Cl4 Pd1 72.4(11) . . . . ? As2 Pd2 Cl4 Pd1 156.90(4) . . . . ? Cl3 Pd2 Cl4 Pd1 -22.56(5) . . . . ? Cl1 Pd1 Cl4 Pd2 -155.87(6) . . . . ? Cl3 Pd1 Cl4 Pd2 23.85(6) . . . . ? As1 Pd1 Cl4 Pd2 31.2(8) . . . . ? Cl1 Pd1 As1 C31 -121.5(2) . . . . ? Cl3 Pd1 As1 C31 58.7(2) . . . . ? Cl4 Pd1 As1 C31 51.5(8) . . . . ? Cl1 Pd1 As1 C11 0.9(3) . . . . ? Cl3 Pd1 As1 C11 -178.9(3) . . . . ? Cl4 Pd1 As1 C11 173.8(8) . . . . ? Cl1 Pd1 As1 C21 125.9(2) . . . . ? Cl3 Pd1 As1 C21 -53.9(2) . . . . ? Cl4 Pd1 As1 C21 -61.2(8) . . . . ? Cl2 Pd2 As2 C41 -6.2(2) . . . . ? Cl4 Pd2 As2 C41 176.9(2) . . . . ? Cl3 Pd2 As2 C41 -177.4(5) . . . . ? Cl2 Pd2 As2 C51 -133.64(18) . . . . ? Cl4 Pd2 As2 C51 49.53(18) . . . . ? Cl3 Pd2 As2 C51 55.2(5) . . . . ? Cl2 Pd2 As2 C61 114.4(2) . . . . ? Cl4 Pd2 As2 C61 -62.4(2) . . . . ? Cl3 Pd2 As2 C61 -56.8(5) . . . . ? C31 As1 C11 C12 -79.6(7) . . . . ? C21 As1 C11 C12 27.8(7) . . . . ? Pd1 As1 C11 C12 155.8(5) . . . . ? As1 C11 C12 C13 -104.2(8) . . . . ? As1 C11 C12 C14 78.1(8) . . . . ? C31 As1 C21 C22 -173.0(5) . . . . ? C11 As1 C21 C22 74.4(6) . . . . ? Pd1 As1 C21 C22 -53.6(6) . . . . ? As1 C21 C22 C23 -113.6(7) . . . . ? As1 C21 C22 C24 68.3(7) . . . . ? C11 As1 C31 C32 -69.9(6) . . . . ? C21 As1 C31 C32 177.1(5) . . . . ? Pd1 As1 C31 C32 55.9(6) . . . . ? As1 C31 C32 C33 89.4(9) . . . . ? As1 C31 C32 C34 -91.0(8) . . . . ? C51 As2 C41 C42 -44.4(6) . . . . ? C61 As2 C41 C42 63.0(6) . . . . ? Pd2 As2 C41 C42 -172.8(5) . . . . ? As2 C41 C42 C43 -92.7(8) . . . . ? As2 C41 C42 C44 87.7(8) . . . . ? C41 As2 C51 C52 -88.6(5) . . . . ? C61 As2 C51 C52 160.7(5) . . . . ? Pd2 As2 C51 C52 41.8(5) . . . . ? As2 C51 C52 C53 -116.7(6) . . . . ? As2 C51 C52 C54 63.1(8) . . . . ? C41 As2 C61 C62 67.7(6) . . . . ? C51 As2 C61 C62 -178.0(5) . . . . ? Pd2 As2 C61 C62 -58.9(5) . . . . ? As2 C61 C62 C63 -115.5(8) . . . . ? As2 C61 C62 C64 69.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.158 _refine_diff_density_min -1.361 _refine_diff_density_rms 0.153 #========================================================================== #END