# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2011-09-05 at 17:09:02 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : c:\wingx\files\archive.reqdat # CIF files read : fr36 #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_global #TrackingRef '- PdNeoc.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2011-09-05 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? # Insert blank lines between references _publ_section_references ; Bruker (2007) APEX2 (Version 2.1-4), SAINT (version 7.34A), SADABS (version 2007/4), BrukerAXS Inc, Madison, Wisconsin, USA. APEX, APEX2, SMART, SAINT, SAINT-Plus: Bruker (2007). Program name(s). Bruker AXS Inc., Madison, Wisconsin, USA. [Older versions (pre-1997) should refer to Siemens Analytical X-ray Instruments Inc. instead of Bruker AXS.] ORTEP-3: Farrugia, L. J. (1997). J. Appl. Cryst. 30, 565. SADABS, TWINABS: Bruker (2001). Program name. Bruker AXS Inc., Madison, Wisconsin, USA. or Sheldrick, G. M. (1996). Program name. University of Gottingen, Germany. SHELX Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122. SIR97: Altomare, A., Burla, M. C., Camalli, M., Cascarano, G. L., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polidori, G. & Spagna, R. (1999). J. Appl. Cryst. 32, 115-119. WinGX: Farrugia, L. J. (1999). J. Appl. Cryst. 32, 837-838. ; _publ_requested_category FM loop_ _publ_author_name M.Rimoldi F.Ragaini E.Gallo F.Ferretti P.Macchi N.Casati #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_2a _database_code_depnum_ccdc_archive 'CCDC 843108' #TrackingRef '- PdNeoc.cif' _audit_creation_date 2011-09-05T17:09:02-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C14 H12 Br2 N2 Pd' _chemical_formula_weight 474.48 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# 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 12.1525(7) _cell_length_b 7.8107(5) _cell_length_c 14.4621(8) _cell_angle_alpha 90 _cell_angle_beta 93.2980(10) _cell_angle_gamma 90 _cell_volume 1370.46(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 2.3 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.171 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.3 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_unetI/netI 0.0609 _diffrn_reflns_number 9451 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 29.3 _diffrn_measured_fraction_theta_max 0.672 _reflns_number_total 2520 _reflns_number_gt 1997 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 2520 _refine_ls_number_parameters 174 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0353 _refine_ls_R_factor_gt 0.025 _refine_ls_wR_factor_ref 0.0488 _refine_ls_wR_factor_gt 0.0475 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_restrained_S_all 0.834 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.478 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.089 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.07953(2) 0.23667(3) 0.265142(19) 0.01694(7) Uani 1 1 d . . . Br1 Br 0.19713(3) -0.00991(4) 0.25048(2) 0.02649(10) Uani 1 1 d . . . Br2 Br 0.02782(3) 0.19730(5) 0.10302(3) 0.03170(11) Uani 1 1 d . . . N11 N 0.0796(2) 0.2409(3) 0.4098(2) 0.0168(6) Uani 1 1 d . . . N21 N -0.0377(2) 0.4247(3) 0.28286(19) 0.0175(6) Uani 1 1 d . . . C22 C -0.0829(3) 0.5395(4) 0.2243(3) 0.0230(7) Uani 1 1 d . . . C16 C -0.0242(3) 0.2935(4) 0.4311(3) 0.0169(7) Uani 1 1 d . . . C12 C 0.1459(3) 0.1745(4) 0.4767(3) 0.0201(7) Uani 1 1 d . . . C15 C -0.0661(3) 0.2660(4) 0.5187(3) 0.0223(8) Uani 1 1 d . . . C13 C 0.1077(3) 0.1411(4) 0.5642(2) 0.0252(8) Uani 1 1 d . . . H13 H 0.1548 0.0896 0.6088 0.03 Uiso 1 1 calc R . . C23 C -0.1894(3) 0.6024(4) 0.2391(3) 0.0278(9) Uani 1 1 d . . . H23 H -0.2232 0.6759 0.1956 0.033 Uiso 1 1 calc R . . C14 C 0.0027(3) 0.1822(4) 0.5859(3) 0.0256(8) Uani 1 1 d . . . H14 H -0.0226 0.1553 0.6436 0.031 Uiso 1 1 calc R . . C26 C -0.0865(3) 0.3902(4) 0.3635(2) 0.0189(7) Uani 1 1 d . . . C25 C -0.1911(3) 0.4553(4) 0.3831(3) 0.0219(7) Uani 1 1 d . . . C17 C -0.1751(3) 0.3267(4) 0.5355(3) 0.0269(9) Uani 1 1 d . . . H17 H -0.2052 0.3039 0.5919 0.032 Uiso 1 1 calc R . . C27 C -0.2338(3) 0.4163(4) 0.4699(3) 0.0266(8) Uani 1 1 d . . . H27 H -0.3043 0.4536 0.482 0.032 Uiso 1 1 calc R . . C24 C -0.2440(3) 0.5586(4) 0.3150(3) 0.0267(8) Uani 1 1 d . . . H24 H -0.3156 0.5967 0.3216 0.032 Uiso 1 1 calc R . . C11 C 0.2647(3) 0.1421(4) 0.4594(3) 0.0265(8) Uani 1 1 d . . . H11A H 0.2748 0.0231 0.4455 0.04 Uiso 1 1 calc R . . H11B H 0.3099 0.172 0.5137 0.04 Uiso 1 1 calc R . . H11C H 0.2855 0.2104 0.4081 0.04 Uiso 1 1 calc R . . C21 C -0.0203(3) 0.6077(5) 0.1469(3) 0.0329(9) Uani 1 1 d . . . H21A H 0.0552 0.5714 0.1546 0.049 Uiso 1 1 calc R . . H21B H -0.0235 0.7305 0.147 0.049 Uiso 1 1 calc R . . H21C H -0.0521 0.5652 0.0891 0.049 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 0.01458(13) 0.02086(13) 0.01565(13) 0.00199(10) 0.00319(10) 0.00063(10) Br1 0.0294(2) 0.02591(19) 0.0249(2) 0.00139(15) 0.00804(16) 0.00649(15) Br2 0.0233(2) 0.0537(3) 0.0183(2) -0.00200(17) 0.00239(16) 0.00535(17) N11 0.0143(14) 0.0144(13) 0.0216(16) -0.0016(11) 0.0005(12) -0.0033(10) N21 0.0149(13) 0.0181(13) 0.0194(15) 0.0041(12) 0.0011(12) -0.0004(11) C22 0.0222(18) 0.0205(16) 0.0256(19) -0.0005(15) -0.0049(15) -0.0052(14) C16 0.0188(17) 0.0109(14) 0.0214(18) -0.0030(13) 0.0046(14) -0.0053(12) C12 0.0250(19) 0.0123(15) 0.0226(19) -0.0004(14) -0.0023(15) -0.0040(13) C15 0.030(2) 0.0158(16) 0.022(2) -0.0062(14) 0.0081(16) -0.0065(14) C13 0.036(2) 0.0200(17) 0.0188(18) 0.0007(14) -0.0090(16) -0.0038(16) C23 0.028(2) 0.0169(17) 0.037(2) -0.0003(17) -0.0101(18) 0.0052(15) C14 0.043(2) 0.0176(16) 0.0160(18) -0.0027(14) 0.0024(17) -0.0097(16) C26 0.0200(17) 0.0147(15) 0.0224(18) -0.0034(14) 0.0038(14) -0.0037(13) C25 0.0200(17) 0.0156(15) 0.030(2) -0.0082(15) 0.0032(15) -0.0010(13) C17 0.031(2) 0.0223(18) 0.029(2) -0.0080(16) 0.0145(18) -0.0067(15) C27 0.0221(18) 0.0219(17) 0.037(2) -0.0096(16) 0.0131(17) -0.0034(14) C24 0.0175(17) 0.0219(17) 0.040(2) -0.0079(17) -0.0010(16) 0.0018(14) C11 0.0226(18) 0.0275(19) 0.029(2) 0.0014(17) -0.0062(16) 0.0014(15) C21 0.034(2) 0.033(2) 0.031(2) 0.0110(18) 0.0011(19) -0.0016(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N21 2.073(3) . ? Pd1 N11 2.093(3) . ? Pd1 Br2 2.4119(5) . ? Pd1 Br1 2.4148(4) . ? N11 C12 1.328(4) . ? N11 C16 1.378(4) . ? N21 C22 1.330(4) . ? N21 C26 1.365(4) . ? C22 C23 1.412(5) . ? C22 C21 1.489(5) . ? C16 C15 1.408(5) . ? C16 C26 1.420(5) . ? C12 C13 1.397(5) . ? C12 C11 1.502(5) . ? C15 C14 1.406(6) . ? C15 C17 1.441(5) . ? C13 C14 1.370(6) . ? C13 H13 0.93 . ? C23 C24 1.358(5) . ? C23 H23 0.93 . ? C14 H14 0.93 . ? C26 C25 1.413(4) . ? C25 C24 1.400(5) . ? C25 C27 1.419(5) . ? C17 C27 1.350(5) . ? C17 H17 0.93 . ? C27 H27 0.93 . ? C24 H24 0.93 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? 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 N21 Pd1 N11 79.96(10) . . ? N21 Pd1 Br2 93.90(8) . . ? N11 Pd1 Br2 163.55(8) . . ? N21 Pd1 Br1 172.15(7) . . ? N11 Pd1 Br1 97.72(7) . . ? Br2 Pd1 Br1 86.295(16) . . ? C12 N11 C16 118.6(3) . . ? C12 N11 Pd1 133.4(2) . . ? C16 N11 Pd1 106.3(2) . . ? C22 N21 C26 119.5(3) . . ? C22 N21 Pd1 131.4(2) . . ? C26 N21 Pd1 107.5(2) . . ? N21 C22 C23 119.2(3) . . ? N21 C22 C21 120.6(3) . . ? C23 C22 C21 120.1(3) . . ? N11 C16 C15 122.6(3) . . ? N11 C16 C26 117.6(3) . . ? C15 C16 C26 119.6(3) . . ? N11 C12 C13 120.9(3) . . ? N11 C12 C11 119.6(3) . . ? C13 C12 C11 119.4(3) . . ? C14 C15 C16 117.4(3) . . ? C14 C15 C17 123.5(4) . . ? C16 C15 C17 119.1(4) . . ? C14 C13 C12 121.7(4) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C24 C23 C22 121.9(3) . . ? C24 C23 H23 119 . . ? C22 C23 H23 119 . . ? C13 C14 C15 118.4(4) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? N21 C26 C25 122.7(3) . . ? N21 C26 C16 116.9(3) . . ? C25 C26 C16 120.2(3) . . ? C24 C25 C26 116.6(3) . . ? C24 C25 C27 124.7(3) . . ? C26 C25 C27 118.7(3) . . ? C27 C17 C15 120.4(4) . . ? C27 C17 H17 119.8 . . ? C15 C17 H17 119.8 . . ? C17 C27 C25 121.9(3) . . ? C17 C27 H27 119.1 . . ? C25 C27 H27 119.1 . . ? C23 C24 C25 119.2(3) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_1a _database_code_depnum_ccdc_archive 'CCDC 843109' #TrackingRef '- PdNeoc.cif' _audit_creation_date 2011-09-05T17:14:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C29 H26 Cl6 N4 Pd2' _chemical_formula_weight 856.04 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# 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 9.897(4) _cell_length_b 21.440(8) _cell_length_c 15.012(6) _cell_angle_alpha 90 _cell_angle_beta 102.442(5) _cell_angle_gamma 90 _cell_volume 3111(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.828 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.699 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0226 _diffrn_reflns_av_unetI/netI 0.0215 _diffrn_reflns_number 34573 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 30.71 _diffrn_measured_fraction_theta_max 0.935 _reflns_number_total 9042 _reflns_number_gt 7434 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0316P)^2^+1.6121P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9042 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0366 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.04 _refine_ls_restrained_S_all 1.04 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.761 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 C12 C 0.5544(3) 0.08230(12) 0.91160(17) 0.0417(5) Uani 1 1 d . . . C13 C 0.5276(3) 0.02044(12) 0.87989(19) 0.0497(6) Uani 1 1 d . . . H13 H 0.4563 0.0129 0.8296 0.06 Uiso 1 1 calc R . . C14 C 0.6040(3) -0.02803(13) 0.9214(2) 0.0529(7) Uani 1 1 d . . . H14 H 0.581 -0.0687 0.9023 0.063 Uiso 1 1 calc R . . C15 C 0.7170(3) -0.01677(11) 0.99294(19) 0.0475(6) Uani 1 1 d . . . C16 C 0.7430(2) 0.04570(11) 1.02057(16) 0.0392(5) Uani 1 1 d . . . C17 C 0.8114(4) -0.06338(13) 1.0358(2) 0.0601(8) Uani 1 1 d . . . H17 H 0.7919 -0.1052 1.0222 0.072 Uiso 1 1 calc R . . C22 C 1.0195(3) 0.14309(14) 1.13943(17) 0.0479(6) Uani 1 1 d . . . C23 C 1.1200(3) 0.09816(18) 1.17665(19) 0.0604(8) Uani 1 1 d . . . H23 H 1.2073 0.1113 1.2071 0.073 Uiso 1 1 calc R . . C24 C 1.0919(3) 0.03630(17) 1.16891(18) 0.0611(8) Uani 1 1 d . . . H24 H 1.1575 0.0075 1.1973 0.073 Uiso 1 1 calc R . . C25 C 0.9639(3) 0.01567(14) 1.11805(18) 0.0517(7) Uani 1 1 d . . . C26 C 0.8673(3) 0.06215(12) 1.08234(16) 0.0413(5) Uani 1 1 d . . . C27 C 0.9278(4) -0.04816(14) 1.0955(2) 0.0642(9) Uani 1 1 d . . . H27 H 0.9869 -0.0797 1.123 0.077 Uiso 1 1 calc R . . C32 C 0.1256(3) 0.89749(11) 0.41275(16) 0.0390(5) Uani 1 1 d . . . C33 C -0.0091(3) 0.87172(12) 0.39052(18) 0.0478(6) Uani 1 1 d . . . H33 H -0.0204 0.8289 0.395 0.057 Uiso 1 1 calc R . . C34 C -0.1219(3) 0.90825(13) 0.36292(18) 0.0490(6) Uani 1 1 d . . . H34 H -0.2092 0.8903 0.3464 0.059 Uiso 1 1 calc R . . C35 C -0.1069(2) 0.97341(12) 0.35922(16) 0.0398(5) Uani 1 1 d . . . C36 C 0.0289(2) 0.99635(10) 0.38089(14) 0.0318(4) Uani 1 1 d . . . C37 C -0.2192(2) 1.01650(14) 0.33676(19) 0.0493(6) Uani 1 1 d . . . H37 H -0.3094 1.0015 0.3209 0.059 Uiso 1 1 calc R . . C42 C 0.2108(2) 1.14150(11) 0.43583(16) 0.0383(5) Uani 1 1 d . . . C43 C 0.1026(3) 1.18516(12) 0.41564(19) 0.0476(6) Uani 1 1 d . . . H43 H 0.1219 1.2272 0.4276 0.057 Uiso 1 1 calc R . . C44 C -0.0291(3) 1.16756(12) 0.37917(19) 0.0477(6) Uani 1 1 d . . . H44 H -0.0983 1.1974 0.3631 0.057 Uiso 1 1 calc R . . C45 C -0.0602(2) 1.10370(11) 0.36574(16) 0.0387(5) Uani 1 1 d . . . C46 C 0.0516(2) 1.06187(10) 0.38548(14) 0.0319(4) Uani 1 1 d . . . C47 C -0.1965(2) 1.07872(14) 0.33820(18) 0.0494(6) Uani 1 1 d . . . H47 H -0.2711 1.1057 0.3209 0.059 Uiso 1 1 calc R . . C11 C 0.4731(3) 0.13464(13) 0.86107(19) 0.0525(6) Uani 1 1 d . . . H11A H 0.5142 0.1736 0.8839 0.079 Uiso 1 1 calc R . . H11B H 0.3797 0.1329 0.8695 0.079 Uiso 1 1 calc R . . H11C H 0.4729 0.1311 0.7973 0.079 Uiso 1 1 calc R . . C21 C 1.0585(3) 0.21033(16) 1.1429(2) 0.0632(8) Uani 1 1 d . . . H21A H 0.9971 0.2324 1.0951 0.095 Uiso 1 1 calc R . . H21B H 1.1518 0.2145 1.1351 0.095 Uiso 1 1 calc R . . H21C H 1.0516 0.2274 1.2009 0.095 Uiso 1 1 calc R . . C31 C 0.2465(3) 0.85660(12) 0.4494(2) 0.0523(6) Uani 1 1 d . . . H31A H 0.2843 0.8411 0.3999 0.078 Uiso 1 1 calc R . . H31B H 0.2172 0.8222 0.4816 0.078 Uiso 1 1 calc R . . H31C H 0.3158 0.8801 0.4904 0.078 Uiso 1 1 calc R . . C41 C 0.3510(3) 1.16123(13) 0.4867(2) 0.0521(6) Uani 1 1 d . . . H41A H 0.4093 1.1252 0.5009 0.078 Uiso 1 1 calc R . . H41B H 0.3431 1.1817 0.5422 0.078 Uiso 1 1 calc R . . H41C H 0.3907 1.1894 0.4497 0.078 Uiso 1 1 calc R . . N11 N 0.6565(2) 0.09361(9) 0.98346(13) 0.0367(4) Uani 1 1 d . . . N21 N 0.8924(2) 0.12487(10) 1.09772(13) 0.0411(4) Uani 1 1 d . . . N31 N 0.14396(18) 0.95870(8) 0.40382(12) 0.0324(4) Uani 1 1 d . . . N41 N 0.18569(17) 1.08147(8) 0.41508(12) 0.0313(4) Uani 1 1 d . . . C9 C 0.9848(4) 0.24447(16) 0.8023(2) 0.0721(9) Uani 1 1 d . . . H9A H 0.9576 0.2878 0.8052 0.086 Uiso 1 1 calc R . . H9B H 1.0135 0.2383 0.7451 0.086 Uiso 1 1 calc R . . Cl91 Cl 1.12442(10) 0.22869(5) 0.89305(7) 0.0819(3) Uani 1 1 d . . . Cl92 Cl 0.84284(11) 0.19655(6) 0.80494(9) 0.0994(3) Uani 1 1 d . . . Cl11 Cl 0.47435(6) 0.19686(3) 1.05939(5) 0.04736(14) Uani 1 1 d . . . Cl12 Cl 0.75795(7) 0.24240(3) 1.18171(5) 0.05380(16) Uani 1 1 d . . . Cl21 Cl 0.42480(8) 0.93336(3) 0.33157(6) 0.06110(19) Uani 1 1 d . . . Cl22 Cl 0.45396(6) 1.08022(3) 0.33418(5) 0.04920(15) Uani 1 1 d . . . Pd1 Pd 0.700974(17) 0.167810(8) 1.071619(12) 0.03488(5) Uani 1 1 d . . . Pd2 Pd 0.310729(15) 1.011863(8) 0.386631(11) 0.03091(5) Uani 1 1 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 C12 0.0429(12) 0.0435(13) 0.0410(12) -0.0036(10) 0.0138(10) -0.0019(10) C13 0.0565(16) 0.0485(14) 0.0469(14) -0.0120(11) 0.0174(12) -0.0082(12) C14 0.0676(18) 0.0393(13) 0.0601(17) -0.0096(12) 0.0321(14) -0.0085(12) C15 0.0600(16) 0.0375(12) 0.0539(15) 0.0027(11) 0.0318(13) 0.0059(11) C16 0.0432(12) 0.0366(11) 0.0423(12) 0.0037(9) 0.0194(10) 0.0067(9) C17 0.084(2) 0.0402(14) 0.0656(19) 0.0112(13) 0.0381(17) 0.0164(14) C22 0.0380(12) 0.0701(17) 0.0356(12) 0.0031(12) 0.0077(10) 0.0034(12) C23 0.0397(14) 0.101(3) 0.0395(14) 0.0078(15) 0.0049(11) 0.0152(15) C24 0.0565(17) 0.089(2) 0.0397(14) 0.0187(15) 0.0145(12) 0.0350(16) C25 0.0554(16) 0.0624(17) 0.0420(13) 0.0154(12) 0.0207(12) 0.0244(13) C26 0.0435(12) 0.0451(13) 0.0395(12) 0.0088(10) 0.0183(10) 0.0115(10) C27 0.084(2) 0.0517(16) 0.0663(19) 0.0228(14) 0.0379(18) 0.0340(16) C32 0.0468(13) 0.0343(11) 0.0383(12) 0.0010(9) 0.0143(10) -0.0032(9) C33 0.0580(16) 0.0406(13) 0.0472(14) -0.0040(11) 0.0163(12) -0.0164(11) C34 0.0457(14) 0.0557(15) 0.0474(14) -0.0048(12) 0.0142(11) -0.0206(12) C35 0.0298(10) 0.0543(14) 0.0360(11) -0.0001(10) 0.0087(9) -0.0081(10) C36 0.0264(9) 0.0388(11) 0.0309(10) 0.0018(8) 0.0078(8) -0.0016(8) C37 0.0236(10) 0.0743(19) 0.0489(14) -0.0007(13) 0.0056(10) -0.0030(11) C42 0.0398(12) 0.0352(11) 0.0427(12) -0.0020(9) 0.0149(10) -0.0022(9) C43 0.0560(15) 0.0335(12) 0.0580(15) 0.0011(11) 0.0226(13) 0.0061(11) C44 0.0481(14) 0.0446(13) 0.0537(15) 0.0103(11) 0.0182(12) 0.0185(11) C45 0.0298(10) 0.0493(13) 0.0384(11) 0.0064(10) 0.0104(9) 0.0098(9) C46 0.0242(9) 0.0389(11) 0.0335(10) 0.0022(8) 0.0079(8) 0.0022(8) C47 0.0278(11) 0.0686(18) 0.0518(15) 0.0073(13) 0.0089(10) 0.0126(11) C11 0.0519(15) 0.0556(16) 0.0459(14) -0.0047(12) 0.0013(12) 0.0058(12) C21 0.0452(15) 0.079(2) 0.0618(18) -0.0015(16) 0.0040(13) -0.0121(14) C31 0.0609(16) 0.0367(12) 0.0620(17) 0.0105(12) 0.0194(13) 0.0082(12) C41 0.0475(14) 0.0464(14) 0.0624(17) -0.0138(12) 0.0120(12) -0.0117(11) N11 0.0378(10) 0.0328(9) 0.0416(10) -0.0015(8) 0.0131(8) 0.0014(7) N21 0.0368(10) 0.0502(12) 0.0364(10) 0.0053(9) 0.0080(8) 0.0065(9) N31 0.0300(8) 0.0328(9) 0.0352(9) 0.0008(7) 0.0089(7) 0.0003(7) N41 0.0259(8) 0.0324(9) 0.0366(9) 0.0009(7) 0.0093(7) 0.0009(7) C9 0.086(2) 0.068(2) 0.0608(19) 0.0017(16) 0.0121(17) 0.0111(18) Cl91 0.0848(6) 0.0782(6) 0.0738(6) 0.0037(5) -0.0024(5) -0.0071(5) Cl92 0.0667(6) 0.0983(8) 0.1267(9) 0.0067(7) 0.0062(6) 0.0043(5) Cl11 0.0394(3) 0.0394(3) 0.0628(4) -0.0068(3) 0.0099(3) 0.0052(2) Cl12 0.0559(4) 0.0504(4) 0.0508(4) -0.0121(3) 0.0020(3) 0.0031(3) Cl21 0.0702(4) 0.0459(3) 0.0809(5) 0.0068(3) 0.0467(4) 0.0176(3) Cl22 0.0298(3) 0.0491(3) 0.0731(4) 0.0017(3) 0.0208(3) -0.0046(2) Pd1 0.03512(9) 0.03169(9) 0.03714(9) 0.00132(7) 0.00623(7) 0.00290(6) Pd2 0.02271(7) 0.03366(8) 0.03670(9) 0.00201(6) 0.00721(6) 0.00346(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C12 N11 1.332(3) . ? C12 C13 1.415(4) . ? C12 C11 1.490(4) . ? C13 C14 1.355(4) . ? C13 H13 0.93 . ? C14 C15 1.395(4) . ? C14 H14 0.93 . ? C15 C16 1.409(3) . ? C15 C17 1.424(4) . ? C16 N11 1.376(3) . ? C16 C26 1.417(4) . ? C17 C27 1.338(5) . ? C17 H17 0.93 . ? C22 N21 1.337(3) . ? C22 C23 1.410(4) . ? C22 C21 1.490(4) . ? C23 C24 1.355(5) . ? C23 H23 0.93 . ? C24 C25 1.402(4) . ? C24 H24 0.93 . ? C25 C26 1.405(3) . ? C25 C27 1.436(5) . ? C26 N21 1.378(3) . ? C27 H27 0.93 . ? C32 N31 1.335(3) . ? C32 C33 1.416(4) . ? C32 C31 1.489(4) . ? C33 C34 1.353(4) . ? C33 H33 0.93 . ? C34 C35 1.407(4) . ? C34 H34 0.93 . ? C35 C36 1.402(3) . ? C35 C37 1.429(4) . ? C36 N31 1.378(3) . ? C36 C46 1.422(3) . ? C37 C47 1.352(4) . ? C37 H37 0.93 . ? C42 N41 1.335(3) . ? C42 C43 1.405(3) . ? C42 C41 1.494(3) . ? C43 C44 1.354(4) . ? C43 H43 0.93 . ? C44 C45 1.408(4) . ? C44 H44 0.93 . ? C45 C46 1.405(3) . ? C45 C47 1.427(3) . ? C46 N41 1.372(3) . ? C47 H47 0.93 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C41 H41A 0.96 . ? C41 H41B 0.96 . ? C41 H41C 0.96 . ? N11 Pd1 2.055(2) . ? N21 Pd1 2.067(2) . ? N31 Pd2 2.0673(18) . ? N41 Pd2 2.0418(18) . ? C9 Cl92 1.748(4) . ? C9 Cl91 1.752(3) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? Cl11 Pd1 2.2967(11) . ? Cl12 Pd1 2.2815(9) . ? Cl21 Pd2 2.2788(9) . ? Cl22 Pd2 2.2931(8) . ? 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 N11 C12 C13 119.9(2) . . ? N11 C12 C11 120.5(2) . . ? C13 C12 C11 119.5(2) . . ? C14 C13 C12 121.2(3) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 117.1(2) . . ? C14 C15 C17 124.5(3) . . ? C16 C15 C17 118.3(3) . . ? N11 C16 C15 122.2(2) . . ? N11 C16 C26 117.1(2) . . ? C15 C16 C26 120.4(2) . . ? C27 C17 C15 121.2(3) . . ? C27 C17 H17 119.4 . . ? C15 C17 H17 119.4 . . ? N21 C22 C23 119.9(3) . . ? N21 C22 C21 120.6(2) . . ? C23 C22 C21 119.5(3) . . ? C24 C23 C22 121.4(3) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 120.0(3) . . ? C23 C24 H24 120 . . ? C25 C24 H24 120 . . ? C24 C25 C26 116.4(3) . . ? C24 C25 C27 125.3(3) . . ? C26 C25 C27 118.1(3) . . ? N21 C26 C25 123.0(3) . . ? N21 C26 C16 116.9(2) . . ? C25 C26 C16 119.8(2) . . ? C17 C27 C25 121.6(3) . . ? C17 C27 H27 119.2 . . ? C25 C27 H27 119.2 . . ? N31 C32 C33 120.1(2) . . ? N31 C32 C31 120.0(2) . . ? C33 C32 C31 119.9(2) . . ? C34 C33 C32 121.3(2) . . ? C34 C33 H33 119.4 . . ? C32 C33 H33 119.4 . . ? C33 C34 C35 120.0(2) . . ? C33 C34 H34 120 . . ? C35 C34 H34 120 . . ? C36 C35 C34 116.3(2) . . ? C36 C35 C37 119.1(2) . . ? C34 C35 C37 124.6(2) . . ? N31 C36 C35 123.5(2) . . ? N31 C36 C46 116.96(18) . . ? C35 C36 C46 119.4(2) . . ? C47 C37 C35 121.0(2) . . ? C47 C37 H37 119.5 . . ? C35 C37 H37 119.5 . . ? N41 C42 C43 119.8(2) . . ? N41 C42 C41 119.9(2) . . ? C43 C42 C41 120.1(2) . . ? C44 C43 C42 121.6(2) . . ? C44 C43 H43 119.2 . . ? C42 C43 H43 119.2 . . ? C43 C44 C45 119.4(2) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? C46 C45 C44 116.9(2) . . ? C46 C45 C47 118.3(2) . . ? C44 C45 C47 124.8(2) . . ? N41 C46 C45 122.4(2) . . ? N41 C46 C36 116.75(18) . . ? C45 C46 C36 120.7(2) . . ? C37 C47 C45 121.2(2) . . ? C37 C47 H47 119.4 . . ? C45 C47 H47 119.4 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C12 N11 C16 119.3(2) . . ? C12 N11 Pd1 133.02(16) . . ? C16 N11 Pd1 106.80(15) . . ? C22 N21 C26 118.7(2) . . ? C22 N21 Pd1 133.66(19) . . ? C26 N21 Pd1 106.16(15) . . ? C32 N31 C36 118.56(19) . . ? C32 N31 Pd2 133.13(16) . . ? C36 N31 Pd2 106.55(14) . . ? C42 N41 C46 119.29(19) . . ? C42 N41 Pd2 131.52(15) . . ? C46 N41 Pd2 107.23(14) . . ? Cl92 C9 Cl91 111.8(2) . . ? Cl92 C9 H9A 109.3 . . ? Cl91 C9 H9A 109.3 . . ? Cl92 C9 H9B 109.3 . . ? Cl91 C9 H9B 109.3 . . ? H9A C9 H9B 107.9 . . ? N11 Pd1 N21 80.65(8) . . ? N11 Pd1 Cl12 173.78(6) . . ? N21 Pd1 Cl12 95.83(6) . . ? N11 Pd1 Cl11 95.08(6) . . ? N21 Pd1 Cl11 167.32(6) . . ? Cl12 Pd1 Cl11 87.28(3) . . ? N41 Pd2 N31 80.83(8) . . ? N41 Pd2 Cl21 170.30(5) . . ? N31 Pd2 Cl21 96.27(6) . . ? N41 Pd2 Cl22 92.98(6) . . ? N31 Pd2 Cl22 164.69(5) . . ? Cl21 Pd2 Cl22 87.50(4) . . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_2b _database_code_depnum_ccdc_archive 'CCDC 843110' #TrackingRef '- PdNeoc.cif' _audit_creation_date 2011-09-05T17:43:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C57 H50 Br8 Cl2 N8 Pd4' _chemical_formula_weight 1982.75 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.141(5) _cell_length_b 8.103(5) _cell_length_c 16.299(5) _cell_angle_alpha 90.181(5) _cell_angle_beta 109.819(5) _cell_angle_gamma 89.497(5) _cell_volume 1508.4(12) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) # Comment: A non-reduced unit cell is chosen in order to show the # metrix close to be monoclinic #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 2.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.605 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0298 _diffrn_reflns_av_unetI/netI 0.0469 _diffrn_reflns_number 10597 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 24.89 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 5098 _reflns_number_gt 3863 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0767P)^2^+0.7985P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5098 _refine_ls_number_parameters 351 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.073 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.058 _refine_diff_density_min -1.426 _refine_diff_density_rms 0.165 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cl Cl 0.1484 0.1585 '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' 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 C11 C 0.9041(7) 0.0275(10) 0.2169(5) 0.048(2) Uani 1 1 d . . . H11A H 0.8238 0.0498 0.1829 0.073 Uiso 1 1 calc R . . H11B H 0.917 -0.0896 0.222 0.073 Uiso 1 1 calc R . . H11C H 0.9541 0.075 0.1888 0.073 Uiso 1 1 calc R . . C12 C 0.9315(6) 0.1021(9) 0.3069(5) 0.0376(18) Uani 1 1 d . . . C13 C 1.0457(7) 0.0821(10) 0.3681(5) 0.047(2) Uani 1 1 d . . . H13 H 1.1032 0.0268 0.3526 0.057 Uiso 1 1 calc R . . C14 C 1.0702(7) 0.1447(10) 0.4497(5) 0.049(2) Uani 1 1 d . . . H14 H 1.1444 0.1295 0.4908 0.058 Uiso 1 1 calc R . . C15 C 0.9845(6) 0.2318(9) 0.4722(5) 0.0383(18) Uani 1 1 d . . . C16 C 0.8716(6) 0.2483(9) 0.4081(4) 0.0352(17) Uani 1 1 d . . . C17 C 1.0063(8) 0.2999(11) 0.5567(5) 0.052(2) Uani 1 1 d . . . H17 H 1.0796 0.2851 0.5991 0.063 Uiso 1 1 calc R . . C21 C 0.4870(7) 0.4967(12) 0.3078(6) 0.058(2) Uani 1 1 d . . . H21A H 0.4875 0.4379 0.2567 0.088 Uiso 1 1 calc R . . H21B H 0.4773 0.6127 0.2951 0.088 Uiso 1 1 calc R . . H21C H 0.4236 0.4585 0.3251 0.088 Uiso 1 1 calc R . . C22 C 0.6025(7) 0.4668(10) 0.3814(5) 0.0416(19) Uani 1 1 d . . . C23 C 0.6224(8) 0.5402(11) 0.4635(6) 0.055(2) Uani 1 1 d . . . H23 H 0.5656 0.6066 0.4737 0.066 Uiso 1 1 calc R . . C24 C 0.7265(9) 0.5118(12) 0.5271(5) 0.061(3) Uani 1 1 d . . . H24 H 0.7408 0.5582 0.5819 0.073 Uiso 1 1 calc R . . C25 C 0.8118(7) 0.4146(10) 0.5118(5) 0.046(2) Uani 1 1 d . . . C26 C 0.7849(7) 0.3452(9) 0.4282(4) 0.0355(17) Uani 1 1 d . . . C27 C 0.9246(8) 0.3841(12) 0.5765(5) 0.053(2) Uani 1 1 d . . . H27 H 0.9403 0.4238 0.6329 0.064 Uiso 1 1 calc R . . C31 C 0.8440(7) 0.5047(10) 0.2222(5) 0.046(2) Uani 1 1 d . . . H31A H 0.8316 0.4573 0.2722 0.069 Uiso 1 1 calc R . . H31B H 0.8342 0.6223 0.223 0.069 Uiso 1 1 calc R . . H31C H 0.9219 0.4788 0.2235 0.069 Uiso 1 1 calc R . . C32 C 0.7576(7) 0.4359(9) 0.1413(5) 0.0388(18) Uani 1 1 d . . . C33 C 0.7567(7) 0.4874(10) 0.0581(6) 0.048(2) Uani 1 1 d . . . H33 H 0.8134 0.5606 0.0543 0.058 Uiso 1 1 calc R . . C34 C 0.6746(8) 0.4319(10) -0.0165(5) 0.048(2) Uani 1 1 d . . . H34 H 0.6774 0.462 -0.0708 0.058 Uiso 1 1 calc R . . C35 C 0.5865(7) 0.3297(9) -0.0103(5) 0.0373(18) Uani 1 1 d . . . C36 C 0.5919(6) 0.2798(8) 0.0721(4) 0.0302(16) Uani 1 1 d . . . C37 C 0.4898(8) 0.2785(10) -0.0849(5) 0.045(2) Uani 1 1 d . . . H37 H 0.4889 0.3042 -0.1407 0.054 Uiso 1 1 calc R . . C41 C 0.4190(7) 0.0464(11) 0.2708(5) 0.047(2) Uani 1 1 d . . . H41A H 0.4946 0.0752 0.3111 0.071 Uiso 1 1 calc R . . H41B H 0.4046 -0.0682 0.2774 0.071 Uiso 1 1 calc R . . H41C H 0.3599 0.1124 0.2824 0.071 Uiso 1 1 calc R . . C42 C 0.4159(6) 0.0768(9) 0.1814(5) 0.0403(18) Uani 1 1 d . . . C43 C 0.3135(7) 0.0448(10) 0.1099(5) 0.046(2) Uani 1 1 d . . . H43 H 0.2485 0.0024 0.1204 0.055 Uiso 1 1 calc R . . C44 C 0.3068(7) 0.0737(10) 0.0266(5) 0.047(2) Uani 1 1 d . . . H44 H 0.2398 0.0445 -0.0193 0.056 Uiso 1 1 calc R . . C45 C 0.4011(6) 0.1481(9) 0.0091(5) 0.0373(18) Uani 1 1 d . . . C46 C 0.4994(6) 0.1869(8) 0.0828(4) 0.0293(15) Uani 1 1 d . . . C47 C 0.4005(8) 0.1939(10) -0.0746(5) 0.046(2) Uani 1 1 d . . . H47 H 0.3374 0.1651 -0.1235 0.055 Uiso 1 1 calc R . . N11 N 0.8481(5) 0.1785(7) 0.3265(4) 0.0325(14) Uani 1 1 d . . . N21 N 0.6795(5) 0.3728(8) 0.3642(4) 0.0388(15) Uani 1 1 d . . . N31 N 0.6781(5) 0.3284(7) 0.1475(4) 0.0314(13) Uani 1 1 d . . . N41 N 0.5089(5) 0.1417(7) 0.1662(4) 0.0296(13) Uani 1 1 d . . . Br1 Br 0.68485(7) -0.10761(10) 0.31599(5) 0.0426(2) Uani 1 1 d . . . Br21 Br 1.15566(9) 0.31232(12) 0.22845(6) 0.0622(3) Uani 1 1 d . . . Br22 Br 1.16432(10) 0.73209(13) 0.21527(7) 0.0691(3) Uani 1 1 d . . . Br23 Br 1.00079(8) 0.70864(11) -0.00681(6) 0.0571(3) Uani 1 1 d . . . Pd1 Pd 0.67655(5) 0.16547(7) 0.24802(3) 0.03031(18) Uani 1 1 d . . . Pd2 Pd 1.08361(5) 0.51205(8) 0.11392(4) 0.0454(2) Uani 1 1 d . . . C9 C 0.5497(17) -0.093(3) 0.505(3) 0.167(15) Uiso 0.5 1 d PD . . H9A H 0.5825 -0.162 0.5559 0.2 Uiso 0.5 1 calc PR . . H9B H 0.5721 -0.1407 0.458 0.2 Uiso 0.5 1 calc PR . . Cl9 Cl 0.6038(6) 0.0912(9) 0.5259(4) 0.208(3) 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 C11 0.041(5) 0.050(5) 0.052(5) -0.015(4) 0.014(4) 0.000(4) C12 0.034(4) 0.032(4) 0.043(4) 0.000(3) 0.008(3) -0.009(3) C13 0.029(4) 0.049(5) 0.058(5) 0.005(4) 0.007(4) 0.000(4) C14 0.035(4) 0.049(5) 0.045(5) 0.010(4) -0.009(4) -0.010(4) C15 0.036(4) 0.039(4) 0.030(4) 0.005(3) -0.002(3) -0.009(3) C16 0.042(4) 0.029(4) 0.029(4) 0.006(3) 0.006(3) -0.011(3) C17 0.046(5) 0.058(6) 0.035(5) 0.011(4) -0.010(4) -0.013(4) C21 0.041(5) 0.069(6) 0.062(6) 0.001(5) 0.012(4) 0.007(4) C22 0.036(4) 0.042(5) 0.050(5) -0.002(4) 0.020(4) -0.002(4) C23 0.058(6) 0.057(6) 0.058(6) -0.015(4) 0.028(5) -0.004(5) C24 0.070(7) 0.080(7) 0.034(5) -0.019(4) 0.019(5) -0.018(5) C25 0.049(5) 0.050(5) 0.037(4) -0.006(4) 0.011(4) -0.016(4) C26 0.043(4) 0.032(4) 0.028(4) -0.001(3) 0.008(3) -0.009(3) C27 0.061(6) 0.063(6) 0.029(4) 0.003(4) 0.006(4) -0.021(5) C31 0.041(5) 0.045(5) 0.049(5) 0.002(4) 0.012(4) -0.011(4) C32 0.041(4) 0.030(4) 0.048(5) 0.002(3) 0.019(4) 0.007(3) C33 0.044(5) 0.045(5) 0.066(6) 0.017(4) 0.033(5) 0.006(4) C34 0.058(5) 0.055(5) 0.041(5) 0.011(4) 0.030(4) 0.014(4) C35 0.043(4) 0.039(4) 0.030(4) 0.003(3) 0.014(3) 0.009(4) C36 0.030(4) 0.030(4) 0.026(4) -0.004(3) 0.005(3) 0.005(3) C37 0.066(6) 0.044(5) 0.021(4) 0.000(3) 0.012(4) 0.017(4) C41 0.039(5) 0.056(5) 0.047(5) 0.011(4) 0.015(4) -0.004(4) C42 0.031(4) 0.039(4) 0.047(5) -0.003(4) 0.008(4) 0.000(3) C43 0.030(4) 0.050(5) 0.054(5) -0.012(4) 0.009(4) -0.010(4) C44 0.036(4) 0.051(5) 0.042(5) -0.012(4) -0.001(4) -0.003(4) C45 0.037(4) 0.033(4) 0.034(4) -0.005(3) 0.002(3) 0.005(3) C46 0.026(4) 0.028(4) 0.031(4) -0.005(3) 0.006(3) 0.003(3) C47 0.054(5) 0.042(5) 0.036(4) -0.003(4) 0.007(4) 0.004(4) N11 0.029(3) 0.033(3) 0.032(3) 0.000(3) 0.006(3) -0.002(3) N21 0.036(4) 0.042(4) 0.036(4) 0.000(3) 0.009(3) -0.006(3) N31 0.033(3) 0.028(3) 0.033(3) -0.001(3) 0.011(3) -0.001(3) N41 0.027(3) 0.027(3) 0.030(3) -0.003(2) 0.003(3) 0.002(2) Br1 0.0400(4) 0.0410(5) 0.0392(4) 0.0088(3) 0.0033(3) -0.0042(3) Br21 0.0662(6) 0.0580(6) 0.0583(6) 0.0067(5) 0.0158(5) 0.0035(5) Br22 0.0785(7) 0.0579(6) 0.0730(7) -0.0121(5) 0.0283(6) -0.0153(5) Br23 0.0638(6) 0.0452(5) 0.0610(6) 0.0027(4) 0.0197(5) -0.0015(4) Pd1 0.0268(3) 0.0330(3) 0.0261(3) -0.0003(2) 0.0023(2) -0.0038(2) Pd2 0.0418(4) 0.0458(4) 0.0533(4) 0.0007(3) 0.0220(3) -0.0016(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C11 C12 1.514(10) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 N11 1.310(10) . ? C12 C13 1.415(10) . ? C13 C14 1.358(12) . ? C13 H13 0.93 . ? C14 C15 1.400(12) . ? C14 H14 0.93 . ? C15 C16 1.420(10) . ? C15 C17 1.423(11) . ? C16 N11 1.382(9) . ? C16 C26 1.432(11) . ? C17 C27 1.326(13) . ? C17 H17 0.93 . ? C21 C22 1.523(11) . ? C21 H21A 0.96 . ? C21 H21B 0.96 . ? C21 H21C 0.96 . ? C22 N21 1.303(10) . ? C22 C23 1.407(11) . ? C23 C24 1.353(12) . ? C23 H23 0.93 . ? C24 C25 1.384(13) . ? C24 H24 0.93 . ? C25 C26 1.405(10) . ? C25 C27 1.437(12) . ? C26 N21 1.366(9) . ? C27 H27 0.93 . ? C31 C32 1.490(10) . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C32 N31 1.335(9) . ? C32 C33 1.417(11) . ? C33 C34 1.363(12) . ? C33 H33 0.93 . ? C34 C35 1.389(11) . ? C34 H34 0.93 . ? C35 C36 1.384(10) . ? C35 C37 1.438(11) . ? C36 N31 1.376(8) . ? C36 C46 1.416(9) . ? C37 C47 1.344(11) . ? C37 H37 0.93 . ? C41 C42 1.467(11) . ? C41 H41A 0.96 . ? C41 H41B 0.96 . ? C41 H41C 0.96 . ? C42 N41 1.346(9) . ? C42 C43 1.412(10) . ? C43 C44 1.354(11) . ? C43 H43 0.93 . ? C44 C45 1.411(11) . ? C44 H44 0.93 . ? C45 C47 1.413(11) . ? C45 C46 1.414(9) . ? C46 N41 1.376(9) . ? C47 H47 0.93 . ? N11 Pd1 2.045(6) . ? N21 Pd1 2.518(6) . ? N31 Pd1 2.113(6) . ? N41 Pd1 2.031(5) . ? Br1 Pd1 2.4637(15) . ? Br21 Pd2 2.3993(14) . ? Br22 Pd2 2.4047(14) . ? Br23 Pd2 2.4639(13) . ? Br23 Pd2 2.4688(14) 2_765 ? Pd2 Br23 2.4688(14) 2_765 ? C9 Cl9 1.625(18) . ? C9 Cl9 1.758(18) 2_656 ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? Cl9 C9 1.758(18) 2_656 ? 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 C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 C13 122.1(7) . . ? N11 C12 C11 119.1(7) . . ? C13 C12 C11 118.7(7) . . ? C14 C13 C12 119.1(8) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.4(7) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C14 C15 C16 118.0(7) . . ? C14 C15 C17 122.3(7) . . ? C16 C15 C17 119.7(8) . . ? N11 C16 C15 120.3(7) . . ? N11 C16 C26 120.9(6) . . ? C15 C16 C26 118.7(7) . . ? C27 C17 C15 121.5(8) . . ? C27 C17 H17 119.2 . . ? C15 C17 H17 119.2 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N21 C22 C23 122.9(8) . . ? N21 C22 C21 117.1(7) . . ? C23 C22 C21 120.0(8) . . ? C24 C23 C22 118.3(8) . . ? C24 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? C23 C24 C25 121.0(8) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C24 C25 C26 117.1(7) . . ? C24 C25 C27 123.1(8) . . ? C26 C25 C27 119.8(8) . . ? N21 C26 C25 121.8(7) . . ? N21 C26 C16 118.8(6) . . ? C25 C26 C16 119.4(7) . . ? C17 C27 C25 120.7(8) . . ? C17 C27 H27 119.6 . . ? C25 C27 H27 119.6 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N31 C32 C33 119.8(7) . . ? N31 C32 C31 119.5(7) . . ? C33 C32 C31 120.7(7) . . ? C34 C33 C32 121.4(7) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C35 119.0(7) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? C36 C35 C34 117.7(7) . . ? C36 C35 C37 119.3(7) . . ? C34 C35 C37 122.9(7) . . ? N31 C36 C35 123.5(7) . . ? N31 C36 C46 116.2(6) . . ? C35 C36 C46 120.0(6) . . ? C47 C37 C35 120.6(7) . . ? C47 C37 H37 119.7 . . ? C35 C37 H37 119.7 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N41 C42 C43 118.9(7) . . ? N41 C42 C41 120.6(6) . . ? C43 C42 C41 120.4(7) . . ? C44 C43 C42 122.1(8) . . ? C44 C43 H43 119 . . ? C42 C43 H43 119 . . ? C43 C44 C45 120.2(7) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C47 124.9(7) . . ? C44 C45 C46 115.9(7) . . ? C47 C45 C46 119.1(7) . . ? N41 C46 C45 122.8(6) . . ? N41 C46 C36 117.5(6) . . ? C45 C46 C36 119.6(6) . . ? C37 C47 C45 121.1(7) . . ? C37 C47 H47 119.4 . . ? C45 C47 H47 119.4 . . ? C12 N11 C16 120.0(6) . . ? C12 N11 Pd1 121.8(5) . . ? C16 N11 Pd1 117.3(5) . . ? C22 N21 C26 118.8(7) . . ? C22 N21 Pd1 135.8(5) . . ? C26 N21 Pd1 103.9(5) . . ? C32 N31 C36 118.3(6) . . ? C32 N31 Pd1 132.0(5) . . ? C36 N31 Pd1 107.9(4) . . ? C42 N41 C46 119.6(6) . . ? C42 N41 Pd1 129.5(5) . . ? C46 N41 Pd1 110.5(4) . . ? Pd2 Br23 Pd2 93.18(5) . 2_765 ? N41 Pd1 N11 176.7(2) . . ? N41 Pd1 N31 79.9(2) . . ? N11 Pd1 N31 100.0(2) . . ? N41 Pd1 Br1 94.76(16) . . ? N11 Pd1 Br1 83.90(16) . . ? N31 Pd1 Br1 154.57(16) . . ? N41 Pd1 N21 108.5(2) . . ? N11 Pd1 N21 74.9(2) . . ? N31 Pd1 N21 99.5(2) . . ? Br1 Pd1 N21 105.77(15) . . ? Br21 Pd2 Br22 90.57(6) . . ? Br21 Pd2 Br23 177.13(4) . . ? Br22 Pd2 Br23 91.72(6) . . ? Br21 Pd2 Br23 90.89(5) . 2_765 ? Br22 Pd2 Br23 178.54(5) . 2_765 ? Br23 Pd2 Br23 86.82(5) . 2_765 ? Cl9 C9 Cl9 111.9(15) . 2_656 ? Cl9 C9 H9A 109.2 . . ? Cl9 C9 H9A 109.2 2_656 . ? Cl9 C9 H9B 109.2 . . ? Cl9 C9 H9B 109.2 2_656 . ? H9A C9 H9B 107.9 . . ? C9 Cl9 C9 68.1(15) . 2_656 ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_2c _database_code_depnum_ccdc_archive 'CCDC 843111' #TrackingRef '- PdNeoc.cif' _audit_creation_date 2011-09-05T17:50:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C16 H18 Br2 N2 O Pd S' _chemical_formula_weight 552.59 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.1737(7) _cell_length_b 7.8067(3) _cell_length_c 23.4069(8) _cell_angle_alpha 90 _cell_angle_beta 93.160(2) _cell_angle_gamma 90 _cell_volume 3680.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.994 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.468 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_unetI/netI 0.075 _diffrn_reflns_number 12802 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.77 _diffrn_measured_fraction_theta_max 0.894 _reflns_number_total 4291 _reflns_number_gt 2753 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0552P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4291 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.1185 _refine_ls_wR_factor_gt 0.1017 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.789 _refine_diff_density_min -1.02 _refine_diff_density_rms 0.145 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.88728(2) 0.17061(5) 0.149016(19) 0.03112(15) Uani 1 1 d . . . Br2 Br 0.98634(3) 0.35657(9) 0.15665(3) 0.0470(2) Uani 1 1 d . . . Br1 Br 0.80526(3) -0.05799(8) 0.15813(3) 0.0442(2) Uani 1 1 d . . . C12 C 0.9705(3) -0.1182(8) 0.1089(3) 0.0398(15) Uani 1 1 d . . . N21 N 0.8566(2) 0.2875(6) 0.0483(2) 0.0316(11) Uani 1 1 d . . . N11 N 0.9299(2) 0.0075(6) 0.0895(2) 0.0340(12) Uani 1 1 d . . . C15 C 0.9229(3) -0.1167(8) -0.0053(3) 0.0400(16) Uani 1 1 d . . . C25 C 0.8458(3) 0.1612(8) -0.0459(3) 0.0387(15) Uani 1 1 d . . . C22 C 0.8250(3) 0.4255(8) 0.0283(3) 0.0362(14) Uani 1 1 d . . . C26 C 0.8680(3) 0.1579(7) 0.0120(2) 0.0325(13) Uani 1 1 d . . . C24 C 0.8105(3) 0.3066(9) -0.0654(3) 0.0487(18) Uani 1 1 d . . . H24 H 0.7936 0.3128 -0.1031 0.058 Uiso 1 1 calc R . . C13 C 0.9890(3) -0.2469(8) 0.0702(3) 0.0486(18) Uani 1 1 d . . . H13 H 1.0179 -0.3332 0.0831 0.058 Uiso 1 1 calc R . . C11 C 0.9934(3) -0.1248(8) 0.1699(3) 0.0484(18) Uani 1 1 d . . . H11A H 0.9761 -0.028 0.1896 0.073 Uiso 1 1 calc R . . H11B H 1.041 -0.1221 0.1731 0.073 Uiso 1 1 calc R . . H11C H 0.9779 -0.2285 0.1867 0.073 Uiso 1 1 calc R . . C27 C 0.8603(3) 0.0199(9) -0.0820(3) 0.0458(17) Uani 1 1 d . . . H27 H 0.843 0.019 -0.1197 0.055 Uiso 1 1 calc R . . C16 C 0.9076(3) 0.0147(7) 0.0332(3) 0.0351(15) Uani 1 1 d . . . C23 C 0.8014(3) 0.4372(9) -0.0289(3) 0.0467(17) Uani 1 1 d . . . H23 H 0.7794 0.5356 -0.0419 0.056 Uiso 1 1 calc R . . C21 C 0.8139(4) 0.5680(8) 0.0691(3) 0.0475(17) Uani 1 1 d . . . H21A H 0.8333 0.5386 0.1062 0.071 Uiso 1 1 calc R . . H21B H 0.7671 0.5864 0.0716 0.071 Uiso 1 1 calc R . . H21C H 0.8342 0.6706 0.0558 0.071 Uiso 1 1 calc R . . C17 C 0.8976(4) -0.1091(9) -0.0632(3) 0.0508(19) Uani 1 1 d . . . H17 H 0.9075 -0.1968 -0.0882 0.061 Uiso 1 1 calc R . . C14 C 0.9657(3) -0.2470(8) 0.0149(3) 0.0473(17) Uani 1 1 d . . . H14 H 0.9781 -0.3335 -0.0096 0.057 Uiso 1 1 calc R . . S1 S 0.83120(8) 0.31588(19) 0.21315(6) 0.0355(4) Uani 1 1 d . . . O1 O 0.7615(2) 0.3478(6) 0.19506(19) 0.0502(12) Uani 1 1 d . . . C31 C 0.8360(3) 0.2038(9) 0.2786(3) 0.0447(16) Uani 1 1 d . . . H31A H 0.8178 0.091 0.2729 0.067 Uiso 1 1 calc R . . H31B H 0.8112 0.2641 0.3061 0.067 Uiso 1 1 calc R . . H31C H 0.8816 0.195 0.2924 0.067 Uiso 1 1 calc R . . C32 C 0.8664(4) 0.5132(8) 0.2361(3) 0.0523(19) Uani 1 1 d . . . H32A H 0.8671 0.5903 0.2041 0.078 Uiso 1 1 calc R . . H32B H 0.9109 0.4945 0.2514 0.078 Uiso 1 1 calc R . . H32C H 0.8403 0.562 0.265 0.078 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 0.0354(3) 0.0259(2) 0.0327(3) -0.0012(2) 0.0075(2) 0.0001(2) Br2 0.0431(4) 0.0401(4) 0.0584(4) -0.0060(3) 0.0074(3) -0.0076(3) Br1 0.0479(4) 0.0338(3) 0.0518(4) -0.0011(3) 0.0120(3) -0.0075(3) C12 0.035(4) 0.036(3) 0.050(4) 0.004(3) 0.012(3) 0.005(3) N21 0.031(3) 0.031(3) 0.033(3) -0.002(2) 0.008(2) -0.001(2) N11 0.037(3) 0.028(3) 0.038(3) -0.002(2) 0.010(2) -0.002(2) C15 0.042(4) 0.029(3) 0.051(4) -0.009(3) 0.016(3) -0.006(3) C25 0.034(4) 0.046(4) 0.037(3) -0.003(3) 0.007(3) 0.000(3) C22 0.037(4) 0.031(3) 0.041(4) -0.003(3) 0.005(3) -0.003(3) C26 0.032(3) 0.033(3) 0.033(3) -0.002(3) 0.008(3) -0.003(3) C24 0.049(4) 0.059(5) 0.037(4) -0.008(3) -0.001(3) 0.002(4) C13 0.053(5) 0.031(3) 0.064(5) 0.005(3) 0.021(4) 0.008(3) C11 0.052(5) 0.036(4) 0.057(4) 0.007(3) 0.002(4) 0.008(3) C27 0.048(4) 0.057(4) 0.032(3) -0.014(3) 0.000(3) -0.007(4) C16 0.026(3) 0.032(3) 0.049(4) -0.006(3) 0.017(3) -0.008(3) C23 0.047(4) 0.045(4) 0.047(4) 0.009(3) -0.003(3) 0.004(3) C21 0.064(5) 0.031(3) 0.048(4) -0.002(3) 0.008(4) 0.010(3) C17 0.057(5) 0.050(4) 0.047(4) -0.025(4) 0.018(4) -0.007(4) C14 0.050(4) 0.032(3) 0.062(5) -0.009(3) 0.019(4) -0.003(3) S1 0.0386(9) 0.0339(8) 0.0345(8) -0.0033(7) 0.0047(7) 0.0061(7) O1 0.044(3) 0.060(3) 0.046(3) -0.008(2) -0.002(2) 0.017(2) C31 0.048(4) 0.054(4) 0.033(3) 0.000(3) 0.003(3) 0.000(3) C32 0.074(5) 0.033(4) 0.050(4) -0.013(3) 0.008(4) -0.003(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N11 2.105(5) . ? Pd1 S1 2.2376(15) . ? Pd1 Br1 2.4510(8) . ? Pd1 Br2 2.4687(8) . ? Pd1 N21 2.571(5) . ? C12 N11 1.341(8) . ? C12 C13 1.417(9) . ? C12 C11 1.477(9) . ? N21 C22 1.325(8) . ? N21 C26 1.349(7) . ? N11 C16 1.370(8) . ? C15 C14 1.399(9) . ? C15 C16 1.411(8) . ? C15 C17 1.424(10) . ? C25 C24 1.403(9) . ? C25 C26 1.403(8) . ? C25 C27 1.430(8) . ? C22 C23 1.399(9) . ? C22 C21 1.491(8) . ? C26 C16 1.447(8) . ? C24 C23 1.349(9) . ? C13 C14 1.352(9) . ? C27 C17 1.319(10) . ? S1 O1 1.467(5) . ? S1 C31 1.762(6) . ? S1 C32 1.767(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 N11 Pd1 S1 172.04(13) . . ? N11 Pd1 Br1 85.37(13) . . ? S1 Pd1 Br1 86.67(5) . . ? N11 Pd1 Br2 92.59(13) . . ? S1 Pd1 Br2 95.20(5) . . ? Br1 Pd1 Br2 165.84(3) . . ? N11 Pd1 N21 72.22(17) . . ? S1 Pd1 N21 109.29(11) . . ? Br1 Pd1 N21 102.06(11) . . ? Br2 Pd1 N21 90.60(11) . . ? N11 C12 C13 118.7(6) . . ? N11 C12 C11 120.3(6) . . ? C13 C12 C11 121.0(6) . . ? C22 N21 C26 118.8(5) . . ? C22 N21 Pd1 134.4(4) . . ? C26 N21 Pd1 105.7(4) . . ? C12 N11 C16 121.2(5) . . ? C12 N11 Pd1 118.9(4) . . ? C16 N11 Pd1 119.2(4) . . ? C14 C15 C16 117.7(6) . . ? C14 C15 C17 122.3(6) . . ? C16 C15 C17 119.9(6) . . ? C24 C25 C26 117.3(6) . . ? C24 C25 C27 123.2(6) . . ? C26 C25 C27 119.5(6) . . ? N21 C22 C23 121.6(6) . . ? N21 C22 C21 117.8(6) . . ? C23 C22 C21 120.6(6) . . ? N21 C26 C25 122.6(6) . . ? N21 C26 C16 118.2(5) . . ? C25 C26 C16 119.1(5) . . ? C23 C24 C25 119.3(6) . . ? C14 C13 C12 121.5(6) . . ? C17 C27 C25 121.5(6) . . ? N11 C16 C15 120.9(6) . . ? N11 C16 C26 120.5(5) . . ? C15 C16 C26 118.6(6) . . ? C24 C23 C22 120.4(6) . . ? C27 C17 C15 121.2(6) . . ? C13 C14 C15 119.9(6) . . ? O1 S1 C31 109.9(3) . . ? O1 S1 C32 107.6(3) . . ? C31 S1 C32 99.6(3) . . ? O1 S1 Pd1 113.85(19) . . ? C31 S1 Pd1 109.0(2) . . ? C32 S1 Pd1 115.8(2) . . ? #===END #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_4 _database_code_depnum_ccdc_archive 'CCDC 843112' #TrackingRef '- PdNeoc.cif' _audit_creation_date 2011-09-05T18:40:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C29 H29 Br2 Cl3 N4 O2 Pd' _chemical_formula_weight 838.13 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# 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 17.348(5) _cell_length_b 7.517(5) _cell_length_c 24.825(5) _cell_angle_alpha 90.000 _cell_angle_beta 99.147(5) _cell_angle_gamma 90.000 _cell_volume 3196(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.742 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.365 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details sadabs _exptl_absorpt_correction_T_min 0.83 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.0772 _diffrn_reflns_av_unetI/netI 0.0671 _diffrn_reflns_number 32988 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 26.51 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 6580 _reflns_number_gt 4370 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1001P)^2^+29.0579P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6580 _refine_ls_number_parameters 357 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1183 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.2165 _refine_ls_wR_factor_gt 0.1904 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.572 _refine_diff_density_min -1.892 _refine_diff_density_rms 0.168 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Cl Cl 0.1484 0.1585 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C5 C 0.6408(9) 0.583(2) 0.7703(6) 0.080(4) Uiso 1 1 d . . . H5 H 0.6907 0.6462 0.7738 0.096 Uiso 1 1 calc R . . C11 C 0.7334(6) -0.0464(15) 1.0972(5) 0.052(3) Uani 1 1 d . . . H11A H 0.706 -0.0208 1.0613 0.077 Uiso 1 1 calc R . . H11B H 0.7106 0.0203 1.1236 0.077 Uiso 1 1 calc R . . H11C H 0.7296 -0.1712 1.1045 0.077 Uiso 1 1 calc R . . C12 C 0.8186(6) 0.0050(12) 1.1005(4) 0.036(2) Uani 1 1 d . . . C13 C 0.8736(7) -0.0600(14) 1.1425(4) 0.047(3) Uani 1 1 d . . . H13 H 0.857 -0.1293 1.1695 0.056 Uiso 1 1 calc R . . C14 C 0.9508(6) -0.0258(14) 1.1455(4) 0.046(3) Uani 1 1 d . . . H14 H 0.9866 -0.0642 1.1751 0.056 Uiso 1 1 calc R . . C15 C 0.9754(5) 0.0707(12) 1.1019(3) 0.034(2) Uani 1 1 d . . . C16 C 0.9176(5) 0.1356(11) 1.0618(4) 0.0302(19) Uani 1 1 d . . . C17 C 1.0552(6) 0.0986(14) 1.0962(4) 0.044(2) Uani 1 1 d . . . H17 H 1.0945 0.0607 1.1238 0.053 Uiso 1 1 calc R . . C21A C 0.8299(6) 0.4006(15) 0.8848(4) 0.047(3) Uani 1 1 d . . . H21A H 0.7807 0.3712 0.8955 0.07 Uiso 1 1 calc R . . H21B H 0.8358 0.3354 0.8524 0.07 Uiso 1 1 calc R . . H21C H 0.8317 0.5259 0.8775 0.07 Uiso 1 1 calc R . . C22 C 0.8945(5) 0.3530(12) 0.9295(4) 0.033(2) Uani 1 1 d . . . C23 C 0.9720(6) 0.3705(12) 0.9220(4) 0.038(2) Uani 1 1 d . . . H23 H 0.9827 0.4179 0.8894 0.046 Uiso 1 1 calc R . . C24 C 1.0326(5) 0.3203(12) 0.9608(4) 0.040(2) Uani 1 1 d . . . H24 H 1.0839 0.3373 0.9553 0.048 Uiso 1 1 calc R . . C25 C 1.0165(5) 0.2422(11) 1.0096(4) 0.032(2) Uani 1 1 d . . . C26 C 0.9379(5) 0.2256(11) 1.0152(4) 0.0295(19) Uani 1 1 d . . . C27 C 1.0747(5) 0.1780(13) 1.0521(4) 0.042(2) Uani 1 1 d . . . H27 H 1.1271 0.1916 1.0492 0.05 Uiso 1 1 calc R . . C31 C 0.7983(6) 0.4608(15) 1.1305(4) 0.047(3) Uani 1 1 d . . . H31A H 0.8018 0.5262 1.164 0.07 Uiso 1 1 calc R . . H31B H 0.8192 0.5314 1.104 0.07 Uiso 1 1 calc R . . H31C H 0.8276 0.3524 1.1368 0.07 Uiso 1 1 calc R . . C32 C 0.7139(5) 0.4176(12) 1.1095(4) 0.035(2) Uani 1 1 d . . . C33 C 0.6568(6) 0.4628(15) 1.1414(4) 0.048(3) Uani 1 1 d . . . H33 H 0.6711 0.5147 1.1756 0.058 Uiso 1 1 calc R . . C34 C 0.5800(6) 0.4296(14) 1.1217(4) 0.047(3) Uani 1 1 d . . . H34 H 0.542 0.4569 1.1429 0.056 Uiso 1 1 calc R . . C35 C 0.5583(5) 0.3558(12) 1.0706(4) 0.037(2) Uani 1 1 d . . . C36 C 0.6180(5) 0.3072(11) 1.0400(3) 0.0293(18) Uani 1 1 d . . . C37 C 0.4790(6) 0.3277(14) 1.0464(5) 0.048(3) Uani 1 1 d . . . H37 H 0.4398 0.358 1.0664 0.057 Uiso 1 1 calc R . . C41 C 0.7006(7) 0.0064(15) 0.8880(5) 0.053(3) Uani 1 1 d . . . H41A H 0.75 0.0396 0.9087 0.079 Uiso 1 1 calc R . . H41B H 0.6966 0.0532 0.8517 0.079 Uiso 1 1 calc R . . H41C H 0.6966 -0.121 0.8864 0.079 Uiso 1 1 calc R . . C42 C 0.6361(5) 0.0798(12) 0.9146(4) 0.037(2) Uani 1 1 d . . . C43 C 0.5584(7) 0.0668(14) 0.8894(4) 0.051(3) Uani 1 1 d . . . H43 H 0.5469 0.0168 0.8548 0.061 Uiso 1 1 calc R . . C44 C 0.4998(6) 0.1251(15) 0.9143(5) 0.050(3) Uani 1 1 d . . . H44 H 0.4483 0.1147 0.8973 0.06 Uiso 1 1 calc R . . C45 C 0.5175(5) 0.2020(12) 0.9663(4) 0.040(2) Uani 1 1 d . . . C46 C 0.5968(5) 0.2201(12) 0.9888(4) 0.0317(19) Uani 1 1 d . . . C47 C 0.4586(5) 0.2601(14) 0.9967(5) 0.044(2) Uani 1 1 d . . . H47 H 0.4061 0.2505 0.9817 0.052 Uiso 1 1 calc R . . N11 N 0.8395(4) 0.1074(9) 1.0617(3) 0.0284(15) Uani 1 1 d . . . N21 N 0.8781(4) 0.2907(9) 0.9766(3) 0.0300(16) Uani 1 1 d . . . N31 N 0.6947(4) 0.3411(9) 1.0608(3) 0.0271(15) Uani 1 1 d . . . N41 N 0.6552(4) 0.1567(9) 0.9630(3) 0.0320(17) Uani 1 1 d . . . Cl51 Cl 0.5596(4) 0.7274(10) 0.7463(3) 0.153(2) Uiso 1 1 d . . . Cl52 Cl 0.6250(3) 0.4963(6) 0.83210(18) 0.0948(12) Uiso 1 1 d . . . Cl53 Cl 0.6347(5) 0.4188(11) 0.7210(3) 0.168(3) Uiso 1 1 d . . . Br1 Br 0.74132(6) 0.60195(15) 0.97972(5) 0.0496(3) Uani 1 1 d . . . Br2 Br 0.80718(8) 0.8392(2) 0.76992(5) 0.0718(4) Uani 1 1 d . . . Pd1 Pd 0.77999(4) 0.30569(9) 1.01345(3) 0.0276(2) Uani 1 1 d . . . O8 O 0.9577(6) 0.5515(14) 0.7911(4) 0.082(3) Uiso 1 1 d D . . O9 O 0.9141(7) 1.2079(17) 0.7501(5) 0.098(3) Uiso 1 1 d D . . H81 H 0.922(8) 0.62(2) 0.767(6) 0.148 Uiso 1 1 d D . . H82 H 0.974(10) 0.432(9) 0.787(8) 0.148 Uiso 1 1 d D . . H91 H 0.874(8) 1.13(2) 0.757(8) 0.148 Uiso 1 1 d D . . H92 H 0.952(8) 1.18(2) 0.727(6) 0.148 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 C11 0.050(6) 0.050(6) 0.059(7) 0.015(5) 0.021(5) -0.005(5) C12 0.045(5) 0.031(5) 0.033(5) -0.005(4) 0.008(4) 0.000(4) C13 0.064(7) 0.040(6) 0.036(6) 0.003(4) 0.009(5) 0.006(5) C14 0.050(6) 0.051(6) 0.035(5) -0.005(5) -0.005(4) 0.013(5) C15 0.040(5) 0.035(5) 0.024(4) -0.009(4) -0.007(4) 0.006(4) C16 0.028(4) 0.025(4) 0.035(5) -0.008(4) -0.002(4) 0.006(3) C17 0.032(5) 0.047(6) 0.048(6) -0.010(5) -0.011(4) 0.009(4) C21A 0.044(6) 0.057(7) 0.039(6) 0.011(5) 0.009(5) 0.005(5) C22 0.040(5) 0.029(5) 0.034(5) -0.005(4) 0.014(4) 0.001(4) C23 0.043(6) 0.031(5) 0.045(6) -0.003(4) 0.017(5) -0.003(4) C24 0.029(5) 0.032(5) 0.063(6) -0.008(5) 0.018(4) -0.002(4) C25 0.024(4) 0.027(4) 0.046(6) -0.008(4) 0.009(4) 0.002(3) C26 0.027(4) 0.025(4) 0.037(5) -0.004(4) 0.008(4) 0.001(3) C27 0.021(4) 0.043(6) 0.060(7) -0.009(5) -0.001(4) 0.004(4) C31 0.045(6) 0.057(7) 0.037(5) -0.010(5) 0.003(4) 0.002(5) C32 0.035(5) 0.033(5) 0.038(5) 0.004(4) 0.008(4) 0.000(4) C33 0.061(7) 0.053(7) 0.032(5) -0.001(5) 0.016(5) 0.010(5) C34 0.045(6) 0.050(6) 0.054(7) -0.004(5) 0.032(5) 0.007(5) C35 0.033(5) 0.037(5) 0.044(6) 0.011(4) 0.014(4) 0.002(4) C36 0.031(4) 0.028(4) 0.031(4) 0.003(4) 0.011(3) 0.004(4) C37 0.031(5) 0.051(6) 0.066(7) 0.016(6) 0.025(5) 0.008(5) C41 0.064(7) 0.045(6) 0.049(6) -0.015(5) 0.009(5) -0.003(5) C42 0.039(5) 0.033(5) 0.038(5) 0.004(4) 0.003(4) -0.001(4) C43 0.057(7) 0.047(6) 0.044(6) -0.004(5) -0.004(5) -0.007(5) C44 0.041(6) 0.047(6) 0.056(7) 0.005(5) -0.007(5) -0.007(5) C45 0.029(5) 0.029(5) 0.061(6) 0.007(5) 0.002(4) 0.000(4) C46 0.030(4) 0.029(5) 0.036(5) 0.009(4) 0.005(4) -0.002(4) C47 0.020(4) 0.050(6) 0.061(7) 0.013(5) 0.006(4) 0.001(4) N11 0.028(4) 0.029(4) 0.029(4) 0.001(3) 0.005(3) 0.002(3) N21 0.030(4) 0.025(4) 0.036(4) 0.001(3) 0.008(3) 0.001(3) N31 0.024(3) 0.028(4) 0.031(4) 0.003(3) 0.008(3) 0.000(3) N41 0.028(4) 0.029(4) 0.038(4) -0.002(3) 0.005(3) -0.002(3) Br1 0.0395(6) 0.0471(6) 0.0648(7) 0.0153(5) 0.0161(5) 0.0085(5) Br2 0.0726(9) 0.0898(10) 0.0532(7) 0.0108(7) 0.0101(6) -0.0072(7) Pd1 0.0220(3) 0.0311(4) 0.0303(4) 0.0019(3) 0.0058(2) 0.0023(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C5 Cl53 1.727(16) . ? C5 Cl52 1.728(15) . ? C5 Cl51 1.805(16) . ? C5 H5 0.98 . ? C11 C12 1.518(14) . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 N11 1.327(11) . ? C12 C13 1.386(14) . ? C13 C14 1.353(15) . ? C13 H13 0.93 . ? C14 C15 1.422(14) . ? C14 H14 0.93 . ? C15 C16 1.386(12) . ? C15 C17 1.430(14) . ? C16 N11 1.371(11) . ? C16 C26 1.432(13) . ? C17 C27 1.335(15) . ? C17 H17 0.93 . ? C21A C22 1.490(13) . ? C21A H21A 0.96 . ? C21A H21B 0.96 . ? C21A H21C 0.96 . ? C22 N21 1.331(11) . ? C22 C23 1.393(13) . ? C23 C24 1.362(14) . ? C23 H23 0.93 . ? C24 C25 1.413(14) . ? C24 H24 0.93 . ? C25 C26 1.397(12) . ? C25 C27 1.424(13) . ? C26 N21 1.385(11) . ? C27 H27 0.93 . ? C31 C32 1.509(13) . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C32 N31 1.331(11) . ? C32 C33 1.406(13) . ? C33 C34 1.368(15) . ? C33 H33 0.93 . ? C34 C35 1.382(14) . ? C34 H34 0.93 . ? C35 C36 1.424(12) . ? C35 C37 1.427(14) . ? C36 N31 1.373(11) . ? C36 C46 1.427(12) . ? C37 C47 1.330(15) . ? C37 H37 0.93 . ? C41 C42 1.492(14) . ? C41 H41A 0.96 . ? C41 H41B 0.96 . ? C41 H41C 0.96 . ? C42 N41 1.327(12) . ? C42 C43 1.398(14) . ? C43 C44 1.343(16) . ? C43 H43 0.93 . ? C44 C45 1.402(15) . ? C44 H44 0.93 . ? C45 C46 1.407(12) . ? C45 C47 1.432(14) . ? C46 N41 1.367(11) . ? C47 H47 0.93 . ? N11 Pd1 2.081(7) . ? N21 Pd1 2.061(7) . ? N31 Pd1 2.048(7) . ? N41 Pd1 2.579(7) . ? Br1 Pd1 2.4356(18) . ? O8 H81 0.95(2) . ? O8 H82 0.95(2) . ? O9 H91 0.95(2) . ? O9 H92 0.95(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl53 C5 Cl52 111.2(9) . . ? Cl53 C5 Cl51 103.9(8) . . ? Cl52 C5 Cl51 107.1(9) . . ? Cl53 C5 H5 111.5 . . ? Cl52 C5 H5 111.5 . . ? Cl51 C5 H5 111.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 C13 121.0(9) . . ? N11 C12 C11 119.0(8) . . ? C13 C12 C11 120.0(9) . . ? C14 C13 C12 122.1(10) . . ? C14 C13 H13 119 . . ? C12 C13 H13 119 . . ? C13 C14 C15 118.0(9) . . ? C13 C14 H14 121 . . ? C15 C14 H14 121 . . ? C16 C15 C14 117.1(9) . . ? C16 C15 C17 118.6(9) . . ? C14 C15 C17 124.3(9) . . ? N11 C16 C15 123.2(9) . . ? N11 C16 C26 116.3(7) . . ? C15 C16 C26 120.3(8) . . ? C27 C17 C15 121.5(9) . . ? C27 C17 H17 119.3 . . ? C15 C17 H17 119.3 . . ? C22 C21A H21A 109.5 . . ? C22 C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C22 C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? N21 C22 C23 119.7(9) . . ? N21 C22 C21A 119.9(8) . . ? C23 C22 C21A 120.4(9) . . ? C24 C23 C22 122.2(9) . . ? C24 C23 H23 118.9 . . ? C22 C23 H23 118.9 . . ? C23 C24 C25 119.0(8) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 116.8(8) . . ? C26 C25 C27 118.9(9) . . ? C24 C25 C27 124.2(8) . . ? N21 C26 C25 122.3(8) . . ? N21 C26 C16 118.2(7) . . ? C25 C26 C16 119.4(8) . . ? C17 C27 C25 121.2(9) . . ? C17 C27 H27 119.4 . . ? C25 C27 H27 119.4 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N31 C32 C33 121.3(9) . . ? N31 C32 C31 119.7(8) . . ? C33 C32 C31 119.0(9) . . ? C34 C33 C32 119.2(9) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 120.7(9) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 118.5(9) . . ? C34 C35 C37 123.3(9) . . ? C36 C35 C37 118.2(9) . . ? N31 C36 C35 119.7(8) . . ? N31 C36 C46 121.2(7) . . ? C35 C36 C46 119.1(8) . . ? C47 C37 C35 122.9(9) . . ? C47 C37 H37 118.5 . . ? C35 C37 H37 118.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N41 C42 C43 121.3(9) . . ? N41 C42 C41 117.8(8) . . ? C43 C42 C41 120.9(9) . . ? C44 C43 C42 121.2(10) . . ? C44 C43 H43 119.4 . . ? C42 C43 H43 119.4 . . ? C43 C44 C45 119.2(10) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C44 C45 C46 117.5(9) . . ? C44 C45 C47 122.8(9) . . ? C46 C45 C47 119.7(10) . . ? N41 C46 C45 122.1(9) . . ? N41 C46 C36 118.2(8) . . ? C45 C46 C36 119.7(8) . . ? C37 C47 C45 119.9(9) . . ? C37 C47 H47 120 . . ? C45 C47 H47 120 . . ? C12 N11 C16 118.2(8) . . ? C12 N11 Pd1 131.7(6) . . ? C16 N11 Pd1 106.8(5) . . ? C22 N21 C26 119.4(7) . . ? C22 N21 Pd1 132.7(6) . . ? C26 N21 Pd1 107.0(5) . . ? C32 N31 C36 120.6(7) . . ? C32 N31 Pd1 118.5(6) . . ? C36 N31 Pd1 120.3(5) . . ? C42 N41 C46 118.6(8) . . ? C42 N41 Pd1 134.3(6) . . ? C46 N41 Pd1 104.4(5) . . ? N31 Pd1 N21 170.2(3) . . ? N31 Pd1 N11 95.7(3) . . ? N21 Pd1 N11 81.2(3) . . ? N31 Pd1 Br1 83.91(19) . . ? N21 Pd1 Br1 95.7(2) . . ? N11 Pd1 Br1 159.6(2) . . ? N31 Pd1 N41 73.0(3) . . ? N21 Pd1 N41 116.7(3) . . ? N11 Pd1 N41 105.7(3) . . ? Br1 Pd1 N41 93.79(17) . . ? H81 O8 H82 128(10) . . ? H91 O9 H92 124(10) . . ? # END of CIF