# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Rhett Smith' 'Gabriela A. Galdamez' R.J.Gilliard.Junior. 'Brad P. Morgan' _publ_contact_author_name 'Rhett Smith' _publ_contact_author_email RHETT@CLEMSON.EDU _publ_section_title ; Canopied trans-chelating bis(N-heterocyclic carbene) ligand: synthesis, structure and catalysis ; # Attachment '_Morgan_DT_2008_Publication.cif' data_{{Ag{1}}AgBr2}2 _database_code_depnum_ccdc_archive 'CCDC 701814' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C68 H76 Ag4 Br4 N8' _chemical_formula_sum 'C68 H76 Ag4 Br4 N8' _chemical_formula_weight 1756.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_hall '-P 2yn' 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 15.262(3) _cell_length_b 10.348(2) _cell_length_c 21.561(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.12(3) _cell_angle_gamma 90.00 _cell_volume 3316.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9441 _cell_measurement_theta_min 2.7408 _cell_measurement_theta_max 26.3839 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 3.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.6504 _exptl_absorpt_correction_T_min 0.2781 _exptl_absorpt_process_details 'REQAB, Rigaku/MSC, The Woodlands, TX, USA, 1999.' _exptl_special_details ? _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method omega _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 260 Slice: -40.0000 - 90.0000 Image width: 0.5000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 27.7046 2theta: -0.1887 scan: Number of images: 220 Slice: -40.0000 - 70.0000 Image width: 0.5000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 27.7046 2theta: -0.1887 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3 circle ; _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21729 _diffrn_reflns_av_R_equivalents 0.0282 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.74 _diffrn_reflns_theta_max 25.10 _reflns_number_total 5901 _reflns_number_gt 5123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC,2001)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC,2001)' _computing_data_reduction 'CrystalClear (Rigaku/MSC,2001)' _computing_structure_solution 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_structure_refinement 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_publication_material 'SHELXTL 6.10 (Bruker AXS,2000)' _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^)+(0.0010P)^2^+25.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5901 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0779 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Ag1 Ag 0.53335(2) 0.70725(4) 0.167621(17) 0.02445(10) Uani 1 1 d . . . Ag2 Ag 0.55775(3) 0.63621(4) 0.03654(2) 0.03415(11) Uani 1 1 d . . . Br1 Br 0.69310(4) 0.78491(5) 0.07140(3) 0.03835(14) Uani 1 1 d . . . Br2 Br 0.44487(3) 0.61145(5) -0.07878(2) 0.02938(12) Uani 1 1 d . . . N1 N 0.3587(2) 0.7033(4) 0.05862(18) 0.0198(8) Uani 1 1 d . . . N2 N 0.4225(3) 0.8892(4) 0.06332(18) 0.0239(9) Uani 1 1 d . . . N3 N 0.6088(3) 0.5579(4) 0.2939(2) 0.0272(9) Uani 1 1 d . . . N4 N 0.6972(3) 0.7136(4) 0.28431(19) 0.0259(9) Uani 1 1 d . . . C1 C 0.3218(3) 0.5893(4) 0.2260(2) 0.0217(10) Uani 1 1 d . . . H1 H 0.3192 0.4977 0.2239 0.026 Uiso 1 1 calc R . . C2 C 0.2715(3) 0.6614(5) 0.1754(2) 0.0219(10) Uani 1 1 d . . . C3 C 0.2768(3) 0.7950(5) 0.1786(2) 0.0255(10) Uani 1 1 d . . . H3 H 0.2427 0.8457 0.1449 0.031 Uiso 1 1 calc R . . C4 C 0.3314(4) 0.8548(5) 0.2303(2) 0.0317(12) Uani 1 1 d . . . H4 H 0.3351 0.9465 0.2317 0.038 Uiso 1 1 calc R . . C5 C 0.3805(3) 0.7831(5) 0.2800(2) 0.0280(11) Uani 1 1 d . . . H5 H 0.4182 0.8257 0.3152 0.034 Uiso 1 1 calc R . . C6 C 0.3755(3) 0.6480(5) 0.2791(2) 0.0242(10) Uani 1 1 d . . . C7 C 0.4148(3) 0.5661(5) 0.3355(2) 0.0264(11) Uani 1 1 d . . . C8 C 0.3761(4) 0.5740(5) 0.3884(2) 0.0331(12) Uani 1 1 d . . . H8 H 0.3332 0.6397 0.3900 0.040 Uiso 1 1 calc R . . C9 C 0.3996(4) 0.4869(6) 0.4383(3) 0.0400(14) Uani 1 1 d . . . H9 H 0.3727 0.4930 0.4738 0.048 Uiso 1 1 calc R . . C10 C 0.4617(4) 0.3922(6) 0.4365(3) 0.0418(15) Uani 1 1 d . . . H10 H 0.4761 0.3305 0.4700 0.050 Uiso 1 1 calc R . . C11 C 0.5036(4) 0.3863(5) 0.3860(3) 0.0366(13) Uani 1 1 d . . . H11 H 0.5483 0.3224 0.3860 0.044 Uiso 1 1 calc R . . C12 C 0.4814(3) 0.4723(5) 0.3351(2) 0.0288(11) Uani 1 1 d . . . C13 C 0.5332(3) 0.4671(5) 0.2825(3) 0.0306(12) Uani 1 1 d . . . H13A H 0.5562 0.3783 0.2797 0.037 Uiso 1 1 calc R . . H13B H 0.4920 0.4878 0.2412 0.037 Uiso 1 1 calc R . . C14 C 0.6194(3) 0.6546(5) 0.2545(2) 0.0257(11) Uani 1 1 d . . . C15 C 0.6787(4) 0.5565(5) 0.3485(3) 0.0339(12) Uani 1 1 d . . . H15 H 0.6859 0.4980 0.3832 0.041 Uiso 1 1 calc R . . C16 C 0.7333(3) 0.6535(5) 0.3421(2) 0.0333(12) Uani 1 1 d . . . H16 H 0.7871 0.6772 0.3716 0.040 Uiso 1 1 calc R . . C17 C 0.7342(4) 0.8298(5) 0.2613(3) 0.0332(12) Uani 1 1 d . . . H17A H 0.7357 0.8180 0.2159 0.040 Uiso 1 1 calc R . . H17B H 0.7968 0.8429 0.2858 0.040 Uiso 1 1 calc R . . C18 C 0.6784(4) 0.9487(6) 0.2679(3) 0.0443(15) Uani 1 1 d . . . H18A H 0.7067 1.0250 0.2527 0.053 Uiso 1 1 calc R . . H18B H 0.6178 0.9382 0.2398 0.053 Uiso 1 1 calc R . . C19 C 0.6682(5) 0.9749(6) 0.3342(3) 0.0507(16) Uani 1 1 d . . . H19A H 0.7282 0.9898 0.3625 0.061 Uiso 1 1 calc R . . H19B H 0.6408 0.8989 0.3503 0.061 Uiso 1 1 calc R . . C20 C 0.6093(4) 1.0928(6) 0.3349(3) 0.0517(17) Uani 1 1 d . . . H20A H 0.6393 1.1694 0.3229 0.078 Uiso 1 1 calc R . . H20B H 0.5988 1.1046 0.3777 0.078 Uiso 1 1 calc R . . H20C H 0.5515 1.0804 0.3045 0.078 Uiso 1 1 calc R . . C21 C 0.3626(4) 1.2330(6) 0.1764(3) 0.0434(15) Uani 1 1 d . . . H21A H 0.3661 1.1836 0.2157 0.065 Uiso 1 1 calc R . . H21B H 0.3037 1.2751 0.1641 0.065 Uiso 1 1 calc R . . H21C H 0.4100 1.2987 0.1835 0.065 Uiso 1 1 calc R . . C22 C 0.3749(3) 1.1424(5) 0.1238(2) 0.0289(11) Uani 1 1 d . . . H22A H 0.3261 1.0772 0.1164 0.035 Uiso 1 1 calc R . . H22B H 0.3694 1.1926 0.0839 0.035 Uiso 1 1 calc R . . C23 C 0.4645(3) 1.0738(5) 0.1386(2) 0.0286(11) Uani 1 1 d . . . H23A H 0.4661 1.0141 0.1747 0.034 Uiso 1 1 calc R . . H23B H 0.5127 1.1386 0.1523 0.034 Uiso 1 1 calc R . . C24 C 0.4842(3) 0.9976(5) 0.0833(3) 0.0279(11) Uani 1 1 d . . . H24A H 0.4807 1.0566 0.0467 0.033 Uiso 1 1 calc R . . H24B H 0.5465 0.9640 0.0956 0.033 Uiso 1 1 calc R . . C25 C 0.3424(3) 0.8980(5) 0.0176(2) 0.0264(11) Uani 1 1 d . . . H25 H 0.3198 0.9720 -0.0069 0.032 Uiso 1 1 calc R . . C26 C 0.3031(3) 0.7812(5) 0.0149(2) 0.0257(11) Uani 1 1 d . . . H26 H 0.2473 0.7570 -0.0122 0.031 Uiso 1 1 calc R . . C27 C 0.4336(3) 0.7698(5) 0.0892(2) 0.0218(10) Uani 1 1 d . . . C28 C 0.3442(3) 0.5651(5) 0.0687(2) 0.0263(11) Uani 1 1 d . . . H28A H 0.3857 0.5367 0.1086 0.032 Uiso 1 1 calc R . . H28B H 0.3584 0.5149 0.0332 0.032 Uiso 1 1 calc R . . C29 C 0.2488(3) 0.5368(5) 0.0728(2) 0.0238(10) Uani 1 1 d . . . C30 C 0.1968(4) 0.4541(5) 0.0279(3) 0.0329(12) Uani 1 1 d . . . H30 H 0.2210 0.4177 -0.0051 0.039 Uiso 1 1 calc R . . C31 C 0.1091(4) 0.4253(6) 0.0319(3) 0.0394(14) Uani 1 1 d . . . H31 H 0.0742 0.3671 0.0022 0.047 Uiso 1 1 calc R . . C32 C 0.0727(4) 0.4798(6) 0.0782(3) 0.0392(14) Uani 1 1 d . . . H32 H 0.0120 0.4619 0.0794 0.047 Uiso 1 1 calc R . . C33 C 0.1243(3) 0.5611(5) 0.1233(2) 0.0313(12) Uani 1 1 d . . . H33 H 0.0990 0.5980 0.1556 0.038 Uiso 1 1 calc R . . C34 C 0.2130(3) 0.5890(4) 0.1214(2) 0.0222(10) 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 Ag1 0.02346(18) 0.02549(19) 0.02172(19) 0.00010(15) -0.00047(14) 0.00119(15) Ag2 0.0303(2) 0.0340(2) 0.0395(2) -0.00978(18) 0.01066(17) -0.00541(17) Br1 0.0371(3) 0.0327(3) 0.0420(3) -0.0031(2) 0.0022(2) -0.0050(2) Br2 0.0290(3) 0.0288(3) 0.0292(3) 0.0020(2) 0.0042(2) 0.0022(2) N1 0.0172(18) 0.023(2) 0.019(2) -0.0017(16) 0.0036(15) 0.0017(16) N2 0.026(2) 0.027(2) 0.020(2) 0.0007(17) 0.0062(16) 0.0025(17) N3 0.030(2) 0.024(2) 0.024(2) 0.0012(17) -0.0018(18) 0.0051(18) N4 0.025(2) 0.027(2) 0.024(2) -0.0049(18) 0.0023(17) 0.0041(17) C1 0.024(2) 0.016(2) 0.024(3) -0.0001(19) 0.0057(19) 0.0028(18) C2 0.021(2) 0.028(3) 0.019(2) 0.0005(19) 0.0085(19) 0.0014(19) C3 0.030(3) 0.023(2) 0.025(3) 0.003(2) 0.010(2) 0.007(2) C4 0.047(3) 0.016(2) 0.034(3) 0.001(2) 0.014(2) 0.006(2) C5 0.032(3) 0.021(2) 0.032(3) -0.006(2) 0.011(2) -0.002(2) C6 0.025(2) 0.022(2) 0.024(3) -0.001(2) 0.005(2) 0.001(2) C7 0.030(3) 0.022(2) 0.023(3) -0.001(2) -0.002(2) -0.007(2) C8 0.032(3) 0.039(3) 0.026(3) -0.005(2) 0.002(2) -0.009(2) C9 0.044(3) 0.049(4) 0.023(3) 0.000(2) -0.001(2) -0.017(3) C10 0.056(4) 0.036(3) 0.025(3) 0.006(2) -0.007(3) -0.015(3) C11 0.047(3) 0.021(3) 0.035(3) 0.002(2) -0.005(3) -0.001(2) C12 0.037(3) 0.019(2) 0.027(3) -0.004(2) 0.000(2) -0.006(2) C13 0.035(3) 0.020(2) 0.034(3) -0.005(2) 0.003(2) 0.001(2) C14 0.023(2) 0.025(3) 0.029(3) -0.003(2) 0.007(2) 0.007(2) C15 0.033(3) 0.038(3) 0.027(3) 0.002(2) -0.003(2) 0.012(2) C16 0.026(3) 0.043(3) 0.027(3) -0.003(2) -0.002(2) 0.007(2) C17 0.030(3) 0.041(3) 0.029(3) -0.004(2) 0.009(2) -0.002(2) C18 0.052(4) 0.032(3) 0.052(4) 0.001(3) 0.019(3) -0.004(3) C19 0.052(4) 0.048(4) 0.053(4) 0.000(3) 0.014(3) 0.009(3) C20 0.045(4) 0.043(4) 0.069(5) -0.006(3) 0.019(3) 0.004(3) C21 0.050(4) 0.032(3) 0.053(4) -0.015(3) 0.022(3) -0.005(3) C22 0.030(3) 0.027(3) 0.030(3) -0.005(2) 0.008(2) -0.001(2) C23 0.029(3) 0.027(3) 0.029(3) 0.000(2) 0.003(2) -0.004(2) C24 0.025(2) 0.024(3) 0.035(3) 0.000(2) 0.008(2) -0.004(2) C25 0.028(3) 0.029(3) 0.022(2) 0.002(2) 0.005(2) 0.010(2) C26 0.021(2) 0.030(3) 0.023(3) 0.000(2) -0.0009(19) 0.009(2) C27 0.023(2) 0.026(2) 0.018(2) -0.0005(19) 0.0085(19) 0.0028(19) C28 0.027(3) 0.023(2) 0.029(3) -0.003(2) 0.006(2) 0.003(2) C29 0.021(2) 0.023(2) 0.026(3) 0.002(2) 0.0009(19) 0.0019(19) C30 0.035(3) 0.030(3) 0.030(3) -0.002(2) 0.000(2) 0.000(2) C31 0.035(3) 0.038(3) 0.037(3) 0.007(3) -0.010(2) -0.013(3) C32 0.025(3) 0.055(4) 0.032(3) 0.018(3) -0.004(2) -0.010(3) C33 0.025(3) 0.044(3) 0.024(3) 0.015(2) 0.004(2) 0.003(2) C34 0.020(2) 0.022(2) 0.023(2) 0.0067(19) 0.0012(19) 0.0027(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 Ag1 C14 2.100(5) . ? Ag1 C27 2.104(5) . ? Ag1 Ag2 3.0241(8) . ? Ag2 Br1 2.5486(8) . ? Ag2 Br2 2.6965(11) . ? Ag2 Br2 2.7231(8) 3_665 ? Br2 Ag2 2.7231(8) 3_665 ? N1 C27 1.368(6) . ? N1 C26 1.377(6) . ? N1 C28 1.471(6) . ? N2 C27 1.350(6) . ? N2 C25 1.388(6) . ? N2 C24 1.465(6) . ? N3 C14 1.347(6) . ? N3 C15 1.396(6) . ? N3 C13 1.464(6) . ? N4 C14 1.360(6) . ? N4 C16 1.389(6) . ? N4 C17 1.463(7) . ? C1 C6 1.389(6) . ? C1 C2 1.397(6) . ? C1 H1 0.9500 . ? C2 C3 1.386(7) . ? C2 C34 1.497(6) . ? C3 C4 1.378(7) . ? C3 H3 0.9500 . ? C4 C5 1.377(7) . ? C4 H4 0.9500 . ? C5 C6 1.400(7) . ? C5 H5 0.9500 . ? C6 C7 1.493(7) . ? C7 C8 1.399(7) . ? C7 C12 1.407(7) . ? C8 C9 1.388(8) . ? C8 H8 0.9500 . ? C9 C10 1.370(9) . ? C9 H9 0.9500 . ? C10 C11 1.383(8) . ? C10 H10 0.9500 . ? C11 C12 1.395(7) . ? C11 H11 0.9500 . ? C12 C13 1.524(7) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C15 C16 1.332(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.522(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.497(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.518(8) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.516(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.509(7) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.515(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.344(7) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C28 C29 1.506(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.396(7) . ? C29 C34 1.397(7) . ? C30 C31 1.393(8) . ? C30 H30 0.9500 . ? C31 C32 1.369(9) . ? C31 H31 0.9500 . ? C32 C33 1.388(8) . ? C32 H32 0.9500 . ? C33 C34 1.394(7) . ? C33 H33 0.9500 . ? 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 C14 Ag1 C27 171.16(18) . . ? C14 Ag1 Ag2 125.84(13) . . ? C27 Ag1 Ag2 62.88(12) . . ? Br1 Ag2 Br2 129.40(3) . . ? Br1 Ag2 Br2 122.82(3) . 3_665 ? Br2 Ag2 Br2 99.45(2) . 3_665 ? Br1 Ag2 Ag1 80.86(3) . . ? Br2 Ag2 Ag1 134.14(2) . . ? Br2 Ag2 Ag1 84.37(2) 3_665 . ? Ag2 Br2 Ag2 80.55(2) . 3_665 ? C27 N1 C26 110.7(4) . . ? C27 N1 C28 123.8(4) . . ? C26 N1 C28 125.4(4) . . ? C27 N2 C25 111.2(4) . . ? C27 N2 C24 124.6(4) . . ? C25 N2 C24 124.2(4) . . ? C14 N3 C15 111.2(4) . . ? C14 N3 C13 124.9(4) . . ? C15 N3 C13 123.9(4) . . ? C14 N4 C16 110.5(4) . . ? C14 N4 C17 124.8(4) . . ? C16 N4 C17 124.6(4) . . ? C6 C1 C2 121.8(4) . . ? C6 C1 H1 119.1 . . ? C2 C1 H1 119.1 . . ? C3 C2 C1 118.6(4) . . ? C3 C2 C34 123.7(4) . . ? C1 C2 C34 117.7(4) . . ? C4 C3 C2 120.4(5) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.7(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.6(5) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 117.9(5) . . ? C1 C6 C7 118.5(4) . . ? C5 C6 C7 123.0(4) . . ? C8 C7 C12 119.0(5) . . ? C8 C7 C6 117.7(5) . . ? C12 C7 C6 122.9(5) . . ? C9 C8 C7 120.7(6) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C10 C9 C8 120.1(6) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.0(5) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 121.2(5) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 118.8(5) . . ? C11 C12 C13 119.3(5) . . ? C7 C12 C13 121.8(4) . . ? N3 C13 C12 112.0(4) . . ? N3 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? N3 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? N3 C14 N4 104.6(4) . . ? N3 C14 Ag1 128.0(4) . . ? N4 C14 Ag1 127.4(4) . . ? C16 C15 N3 106.4(5) . . ? C16 C15 H15 126.8 . . ? N3 C15 H15 126.8 . . ? C15 C16 N4 107.4(4) . . ? C15 C16 H16 126.3 . . ? N4 C16 H16 126.3 . . ? N4 C17 C18 111.4(4) . . ? N4 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N4 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C19 C18 C17 114.7(5) . . ? C19 C18 H18A 108.6 . . ? C17 C18 H18A 108.6 . . ? C19 C18 H18B 108.6 . . ? C17 C18 H18B 108.6 . . ? H18A C18 H18B 107.6 . . ? C18 C19 C20 110.2(6) . . ? C18 C19 H19A 109.6 . . ? C20 C19 H19A 109.6 . . ? C18 C19 H19B 109.6 . . ? C20 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 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 . . ? C23 C22 C21 113.1(4) . . ? C23 C22 H22A 109.0 . . ? C21 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C21 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C22 C23 C24 114.2(4) . . ? C22 C23 H23A 108.7 . . ? C24 C23 H23A 108.7 . . ? C22 C23 H23B 108.7 . . ? C24 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? N2 C24 C23 113.6(4) . . ? N2 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? N2 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C26 C25 N2 106.5(4) . . ? C26 C25 H25 126.7 . . ? N2 C25 H25 126.7 . . ? C25 C26 N1 107.2(4) . . ? C25 C26 H26 126.4 . . ? N1 C26 H26 126.4 . . ? N2 C27 N1 104.4(4) . . ? N2 C27 Ag1 127.9(3) . . ? N1 C27 Ag1 127.3(3) . . ? N1 C28 C29 112.2(4) . . ? N1 C28 H28A 109.2 . . ? C29 C28 H28A 109.2 . . ? N1 C28 H28B 109.2 . . ? C29 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? C30 C29 C34 119.9(5) . . ? C30 C29 C28 119.0(5) . . ? C34 C29 C28 121.1(4) . . ? C31 C30 C29 119.4(5) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C32 C31 C30 120.8(5) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 120.0(5) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 120.4(5) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C29 119.3(5) . . ? C33 C34 C2 119.5(4) . . ? C29 C34 C2 120.8(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.863 _refine_diff_density_min -1.118 _refine_diff_density_rms 0.117 #===END data_{u-ClPd{PPh2OH}{PPh2O}}2 _database_code_depnum_ccdc_archive 'CCDC 701815' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H42 Cl2 O4 P4 Pd2' _chemical_formula_sum 'C48 H42 Cl2 O4 P4 Pd2' _chemical_formula_weight 1090.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' _symmetry_space_group_name_hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.855(2) _cell_length_b 13.167(3) _cell_length_c 17.352(4) _cell_angle_alpha 68.76(3) _cell_angle_beta 78.84(3) _cell_angle_gamma 63.27(3) _cell_volume 2253.2(8) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6963 _cell_measurement_theta_min 3.3777 _cell_measurement_theta_max 26.3856 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 1.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5748 _exptl_absorpt_correction_T_max 0.6715 _exptl_absorpt_process_details 'REQAB, Rigaku/MSC, The Woodlands, TX, USA, 1999.' _exptl_special_details ? _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method omega _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 260 Slice: -40.0000 - 90.0000 Image width: 0.5000 Exp time: 5.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 27.5694 2theta: -0.1332 scan: Number of images: 220 Slice: -30.0000 - 80.0000 Image width: 0.5000 Exp time: 5.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 27.5694 2theta: -0.1332 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3 circle ; _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16023 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0369 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 25.10 _reflns_number_total 7784 _reflns_number_gt 6880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC,2001)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC,2001)' _computing_data_reduction 'CrystalClear (Rigaku/MSC,2001)' _computing_structure_solution 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_structure_refinement 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_publication_material 'SHELXTL 6.10 (Bruker AXS,2000)' _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^)+(0.0010P)^2^+8.5864P] 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 7784 _refine_ls_number_parameters 567 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0436 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.10520(2) 0.35300(2) 0.493556(16) 0.01650(8) Uani 1 1 d . . . Pd2 Pd 0.08377(2) 0.85646(2) 0.983106(16) 0.01982(8) Uani 1 1 d . . . Cl1 Cl 0.11584(7) 0.54091(7) 0.47124(5) 0.02045(18) Uani 1 1 d . . . Cl2 Cl -0.11189(8) 0.96021(8) 1.05074(6) 0.02400(19) Uani 1 1 d . . . P1 P 0.06855(8) 0.19364(8) 0.50580(6) 0.02003(19) Uani 1 1 d . . . P2 P 0.31268(8) 0.25892(8) 0.46470(5) 0.01771(19) Uani 1 1 d . . . P3 P 0.28338(8) 0.76160(8) 0.94121(6) 0.0205(2) Uani 1 1 d . . . P4 P 0.04358(9) 0.69626(8) 1.00716(6) 0.0226(2) Uani 1 1 d . . . O1 O 0.1756(2) 0.0901(2) 0.47902(18) 0.0287(6) Uani 1 1 d . . . H49 H 0.264(4) 0.085(4) 0.462(3) 0.034 Uiso 1 1 d . . . O2 O 0.3584(2) 0.1338(2) 0.45630(16) 0.0233(5) Uani 1 1 d . . . O3 O 0.3262(2) 0.6354(2) 0.93508(17) 0.0277(6) Uani 1 1 d . . . H50 H 0.269(4) 0.588(4) 0.965(3) 0.033 Uiso 1 1 d . . . O4 O 0.1503(3) 0.5838(2) 0.99052(18) 0.0322(6) Uani 1 1 d . . . C1 C 0.0134(3) 0.1346(3) 0.6090(2) 0.0254(8) Uani 1 1 d . . . C2 C 0.0164(4) 0.1728(4) 0.6720(3) 0.0351(10) Uani 1 1 d . . . H2 H 0.0452 0.2336 0.6609 0.042 Uiso 1 1 calc R . . C3 C -0.0225(5) 0.1231(4) 0.7525(3) 0.0476(12) Uani 1 1 d . . . H3 H -0.0198 0.1499 0.7959 0.057 Uiso 1 1 calc R . . C4 C -0.0644(4) 0.0356(4) 0.7690(3) 0.0442(11) Uani 1 1 d . . . H4 H -0.0918 0.0025 0.8236 0.053 Uiso 1 1 calc R . . C5 C -0.0669(4) -0.0044(4) 0.7063(3) 0.0405(11) Uani 1 1 d . . . H5 H -0.0951 -0.0657 0.7181 0.049 Uiso 1 1 calc R . . C6 C -0.0286(4) 0.0442(4) 0.6267(3) 0.0345(9) Uani 1 1 d . . . H6 H -0.0307 0.0165 0.5837 0.041 Uiso 1 1 calc R . . C7 C -0.0606(3) 0.2516(3) 0.4385(2) 0.0242(8) Uani 1 1 d . . . C8 C -0.0329(4) 0.2709(4) 0.3541(3) 0.0402(10) Uani 1 1 d . . . H8 H 0.0521 0.2511 0.3335 0.048 Uiso 1 1 calc R . . C9 C -0.1298(5) 0.3193(5) 0.2996(3) 0.0540(13) Uani 1 1 d . . . H9 H -0.1105 0.3313 0.2421 0.065 Uiso 1 1 calc R . . C10 C -0.2526(4) 0.3495(4) 0.3286(3) 0.0481(12) Uani 1 1 d . . . H10 H -0.3184 0.3831 0.2913 0.058 Uiso 1 1 calc R . . C11 C -0.2807(4) 0.3315(4) 0.4118(3) 0.0384(10) Uani 1 1 d . . . H11 H -0.3661 0.3525 0.4316 0.046 Uiso 1 1 calc R . . C12 C -0.1856(4) 0.2827(4) 0.4670(3) 0.0325(9) Uani 1 1 d . . . H12 H -0.2061 0.2707 0.5244 0.039 Uiso 1 1 calc R . . C13 C 0.4139(3) 0.2434(3) 0.5382(2) 0.0215(7) Uani 1 1 d . . . C14 C 0.5331(3) 0.1502(3) 0.5464(2) 0.0279(8) Uani 1 1 d . . . H14 H 0.5565 0.0960 0.5160 0.033 Uiso 1 1 calc R . . C15 C 0.6190(4) 0.1347(4) 0.5983(3) 0.0317(9) Uani 1 1 d . . . H15 H 0.6999 0.0694 0.6039 0.038 Uiso 1 1 calc R . . C16 C 0.5874(4) 0.2134(4) 0.6416(2) 0.0328(9) Uani 1 1 d . . . H16 H 0.6462 0.2030 0.6770 0.039 Uiso 1 1 calc R . . C17 C 0.4691(4) 0.3079(4) 0.6332(3) 0.0450(12) Uani 1 1 d . . . H17 H 0.4473 0.3636 0.6621 0.054 Uiso 1 1 calc R . . C18 C 0.3827(4) 0.3217(4) 0.5830(3) 0.0356(10) Uani 1 1 d . . . H18 H 0.3009 0.3855 0.5791 0.043 Uiso 1 1 calc R . . C19 C 0.3564(3) 0.3485(3) 0.3670(2) 0.0213(8) Uani 1 1 d . . . C20 C 0.3770(3) 0.4475(3) 0.3590(2) 0.0256(8) Uani 1 1 d . . . H20 H 0.3702 0.4707 0.4062 0.031 Uiso 1 1 calc R . . C21 C 0.4076(4) 0.5122(4) 0.2820(3) 0.0353(10) Uani 1 1 d . . . H21 H 0.4196 0.5813 0.2763 0.042 Uiso 1 1 calc R . . C22 C 0.4210(4) 0.4782(4) 0.2136(3) 0.0369(10) Uani 1 1 d . . . H22 H 0.4437 0.5225 0.1612 0.044 Uiso 1 1 calc R . . C23 C 0.4012(4) 0.3792(4) 0.2212(2) 0.0373(10) Uani 1 1 d . . . H23 H 0.4101 0.3554 0.1740 0.045 Uiso 1 1 calc R . . C24 C 0.3685(4) 0.3150(4) 0.2976(2) 0.0294(9) Uani 1 1 d . . . H24 H 0.3542 0.2474 0.3027 0.035 Uiso 1 1 calc R . . C25 C 0.3150(3) 0.8498(3) 0.8394(2) 0.0234(8) Uani 1 1 d . . . C26 C 0.3698(4) 0.9287(4) 0.8258(3) 0.0316(9) Uani 1 1 d . . . H26 H 0.3916 0.9399 0.8712 0.038 Uiso 1 1 calc R . . C27 C 0.3927(4) 0.9914(4) 0.7446(3) 0.0400(11) Uani 1 1 d . . . H27 H 0.4299 1.0458 0.7345 0.048 Uiso 1 1 calc R . . C28 C 0.3614(4) 0.9748(4) 0.6790(3) 0.0384(10) Uani 1 1 d . . . H28 H 0.3794 1.0163 0.6241 0.046 Uiso 1 1 calc R . . C29 C 0.3043(4) 0.8985(4) 0.6921(2) 0.0363(10) Uani 1 1 d . . . H29 H 0.2815 0.8889 0.6465 0.044 Uiso 1 1 calc R . . C30 C 0.2808(4) 0.8364(4) 0.7719(2) 0.0306(9) Uani 1 1 d . . . H30 H 0.2411 0.7842 0.7812 0.037 Uiso 1 1 calc R . . C31 C 0.3879(3) 0.7481(3) 1.0112(2) 0.0240(8) Uani 1 1 d . . . C32 C 0.5155(4) 0.6743(4) 1.0062(2) 0.0319(9) Uani 1 1 d . . . H32 H 0.5459 0.6342 0.9657 0.038 Uiso 1 1 calc R . . C33 C 0.5991(4) 0.6587(4) 1.0599(3) 0.0366(10) Uani 1 1 d . . . H33 H 0.6862 0.6080 1.0561 0.044 Uiso 1 1 calc R . . C34 C 0.5560(4) 0.7164(4) 1.1184(3) 0.0387(10) Uani 1 1 d . . . H34 H 0.6136 0.7066 1.1545 0.046 Uiso 1 1 calc R . . C35 C 0.4290(4) 0.7888(4) 1.1252(3) 0.0406(11) Uani 1 1 d . . . H35 H 0.3993 0.8276 1.1664 0.049 Uiso 1 1 calc R . . C36 C 0.3452(4) 0.8048(4) 1.0718(3) 0.0332(9) Uani 1 1 d . . . H36 H 0.2580 0.8547 1.0765 0.040 Uiso 1 1 calc R . . C37 C -0.0876(4) 0.7381(3) 0.9457(2) 0.0248(8) Uani 1 1 d . . . C38 C -0.1999(4) 0.8408(4) 0.9392(3) 0.0359(10) Uani 1 1 d . . . H38 H -0.2124 0.8920 0.9700 0.043 Uiso 1 1 calc R . . C39 C -0.2936(4) 0.8692(4) 0.8883(3) 0.0420(11) Uani 1 1 d . . . H39 H -0.3698 0.9394 0.8844 0.050 Uiso 1 1 calc R . . C40 C -0.2763(4) 0.7962(4) 0.8434(3) 0.0397(10) Uani 1 1 d . . . H40 H -0.3395 0.8169 0.8074 0.048 Uiso 1 1 calc R . . C41 C -0.1680(5) 0.6933(4) 0.8505(3) 0.0445(11) Uani 1 1 d . . . H41 H -0.1577 0.6418 0.8205 0.053 Uiso 1 1 calc R . . C42 C -0.0739(4) 0.6637(4) 0.9010(3) 0.0372(10) Uani 1 1 d . . . H42 H 0.0009 0.5922 0.9053 0.045 Uiso 1 1 calc R . . C43 C -0.0047(4) 0.6537(3) 1.1150(2) 0.0248(8) Uani 1 1 d . . . C44 C 0.0842(4) 0.6135(5) 1.1725(3) 0.0465(12) Uani 1 1 d . . . H44 H 0.1657 0.6121 1.1542 0.056 Uiso 1 1 calc R . . C45 C 0.0564(5) 0.5757(4) 1.2560(3) 0.0461(12) Uani 1 1 d . . . H45 H 0.1199 0.5464 1.2943 0.055 Uiso 1 1 calc R . . C46 C -0.0590(5) 0.5794(5) 1.2845(3) 0.0512(13) Uani 1 1 d . . . C47A C -0.165(3) 0.660(6) 1.2282(8) 0.061(12) Uani 0.50(7) 1 d P . . C47B C -0.1355(13) 0.590(3) 1.2289(8) 0.039(6) Uani 0.50(7) 1 d P . . C48A C -0.139(4) 0.695(7) 1.1443(10) 0.040(12) Uani 0.42(10) 1 d P . . C48B C -0.1100(19) 0.635(4) 1.1417(7) 0.037(6) Uani 0.58(10) 1 d P . . 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 0.01474(14) 0.01444(13) 0.01957(14) -0.00661(10) 0.00050(10) -0.00490(10) Pd2 0.01935(15) 0.01878(14) 0.02194(15) -0.00702(11) 0.00130(10) -0.00876(11) Cl1 0.0153(4) 0.0159(4) 0.0311(5) -0.0095(3) 0.0031(3) -0.0073(3) Cl2 0.0213(4) 0.0216(4) 0.0328(5) -0.0120(4) 0.0053(4) -0.0118(4) P1 0.0188(4) 0.0162(4) 0.0283(5) -0.0105(4) 0.0007(4) -0.0078(4) P2 0.0139(4) 0.0173(4) 0.0205(4) -0.0079(4) 0.0009(3) -0.0044(3) P3 0.0185(4) 0.0205(5) 0.0224(5) -0.0078(4) 0.0015(4) -0.0080(4) P4 0.0256(5) 0.0210(5) 0.0243(5) -0.0064(4) -0.0005(4) -0.0128(4) O1 0.0212(14) 0.0203(13) 0.0496(17) -0.0197(12) 0.0035(12) -0.0080(11) O2 0.0181(12) 0.0180(12) 0.0316(14) -0.0126(11) 0.0005(10) -0.0025(10) O3 0.0259(14) 0.0229(14) 0.0347(15) -0.0118(12) 0.0052(11) -0.0107(12) O4 0.0312(15) 0.0191(13) 0.0457(17) -0.0118(12) 0.0005(13) -0.0094(12) C1 0.0204(18) 0.0185(18) 0.031(2) -0.0022(16) -0.0044(15) -0.0055(15) C2 0.046(3) 0.030(2) 0.032(2) -0.0037(18) -0.0057(19) -0.021(2) C3 0.069(3) 0.045(3) 0.027(2) -0.003(2) -0.007(2) -0.025(3) C4 0.046(3) 0.040(3) 0.035(2) 0.002(2) 0.001(2) -0.019(2) C5 0.036(2) 0.030(2) 0.050(3) -0.001(2) 0.004(2) -0.020(2) C6 0.032(2) 0.028(2) 0.044(3) -0.0104(19) -0.0029(18) -0.0131(18) C7 0.0248(19) 0.0201(18) 0.033(2) -0.0117(16) -0.0045(16) -0.0094(15) C8 0.031(2) 0.054(3) 0.040(2) -0.023(2) -0.0002(19) -0.015(2) C9 0.048(3) 0.075(4) 0.037(3) -0.024(3) -0.006(2) -0.018(3) C10 0.040(3) 0.054(3) 0.055(3) -0.022(2) -0.021(2) -0.012(2) C11 0.024(2) 0.043(3) 0.051(3) -0.020(2) -0.0058(19) -0.0117(19) C12 0.024(2) 0.039(2) 0.040(2) -0.0149(19) -0.0010(17) -0.0146(18) C13 0.0192(18) 0.0222(18) 0.0207(18) -0.0054(15) 0.0008(14) -0.0082(15) C14 0.0212(19) 0.028(2) 0.035(2) -0.0138(17) -0.0043(16) -0.0058(16) C15 0.0207(19) 0.031(2) 0.039(2) -0.0104(18) -0.0082(17) -0.0039(17) C16 0.023(2) 0.045(2) 0.029(2) -0.0112(19) -0.0084(16) -0.0109(18) C17 0.036(2) 0.053(3) 0.050(3) -0.033(2) -0.011(2) -0.005(2) C18 0.022(2) 0.043(2) 0.039(2) -0.024(2) -0.0100(17) 0.0000(18) C19 0.0124(16) 0.0254(19) 0.0211(18) -0.0076(15) -0.0007(13) -0.0033(14) C20 0.0188(18) 0.030(2) 0.0256(19) -0.0077(16) 0.0016(15) -0.0103(16) C21 0.027(2) 0.039(2) 0.037(2) -0.0028(19) -0.0012(17) -0.0185(19) C22 0.031(2) 0.044(3) 0.025(2) 0.0013(19) 0.0003(17) -0.016(2) C23 0.037(2) 0.049(3) 0.021(2) -0.0127(19) 0.0011(17) -0.013(2) C24 0.030(2) 0.031(2) 0.024(2) -0.0099(17) -0.0013(16) -0.0088(17) C25 0.0181(18) 0.0231(19) 0.0244(19) -0.0079(15) 0.0019(14) -0.0054(15) C26 0.032(2) 0.034(2) 0.031(2) -0.0072(18) -0.0022(17) -0.0169(18) C27 0.041(3) 0.036(2) 0.040(2) -0.002(2) 0.004(2) -0.022(2) C28 0.036(2) 0.040(2) 0.024(2) -0.0012(18) 0.0016(17) -0.012(2) C29 0.034(2) 0.045(3) 0.024(2) -0.0095(19) -0.0055(17) -0.011(2) C30 0.028(2) 0.036(2) 0.028(2) -0.0114(17) 0.0000(16) -0.0127(18) C31 0.0220(19) 0.0254(19) 0.0223(18) -0.0046(15) 0.0024(14) -0.0113(16) C32 0.026(2) 0.036(2) 0.029(2) -0.0114(18) 0.0061(16) -0.0112(18) C33 0.024(2) 0.042(2) 0.038(2) -0.012(2) -0.0020(17) -0.0098(19) C34 0.034(2) 0.053(3) 0.034(2) -0.012(2) -0.0077(18) -0.021(2) C35 0.043(3) 0.048(3) 0.033(2) -0.019(2) -0.0070(19) -0.013(2) C36 0.027(2) 0.035(2) 0.032(2) -0.0125(18) -0.0053(17) -0.0048(18) C37 0.031(2) 0.028(2) 0.0213(18) -0.0058(15) 0.0000(15) -0.0187(17) C38 0.034(2) 0.043(3) 0.042(2) -0.024(2) -0.0019(19) -0.017(2) C39 0.033(2) 0.040(3) 0.060(3) -0.019(2) -0.013(2) -0.014(2) C40 0.046(3) 0.048(3) 0.037(2) -0.014(2) -0.010(2) -0.025(2) C41 0.054(3) 0.055(3) 0.043(3) -0.028(2) -0.006(2) -0.027(3) C42 0.044(3) 0.034(2) 0.040(2) -0.018(2) -0.002(2) -0.016(2) C43 0.030(2) 0.0232(19) 0.0238(19) -0.0047(15) -0.0033(15) -0.0145(16) C44 0.029(2) 0.064(3) 0.032(2) -0.014(2) -0.0074(18) -0.007(2) C45 0.044(3) 0.047(3) 0.029(2) -0.008(2) -0.015(2) -0.002(2) C46 0.069(4) 0.068(3) 0.024(2) -0.002(2) -0.007(2) -0.043(3) C47A 0.059(12) 0.10(3) 0.033(6) 0.013(8) -0.005(6) -0.062(18) C47B 0.036(6) 0.044(14) 0.029(5) 0.006(6) -0.003(4) -0.023(7) C48A 0.036(12) 0.07(3) 0.026(6) -0.003(8) 0.002(6) -0.037(16) C48B 0.034(6) 0.049(16) 0.023(4) -0.003(5) -0.002(3) -0.020(8) _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 P2 2.2510(12) . ? Pd1 P1 2.2578(10) . ? Pd1 Cl1 2.4198(10) . ? Pd1 Cl1 2.4284(12) 2_566 ? Pd2 P3 2.2410(13) . ? Pd2 P4 2.2449(11) . ? Pd2 Cl2 2.4251(13) . ? Pd2 Cl2 2.4297(10) 2_577 ? Cl1 Pd1 2.4284(12) 2_566 ? Cl2 Pd2 2.4297(10) 2_577 ? P1 O1 1.537(3) . ? P1 C1 1.798(4) . ? P1 C7 1.812(4) . ? P2 O2 1.539(3) . ? P2 C13 1.814(4) . ? P2 C19 1.815(4) . ? P3 O3 1.542(3) . ? P3 C25 1.805(4) . ? P3 C31 1.808(4) . ? P4 O4 1.536(3) . ? P4 C43 1.805(4) . ? P4 C37 1.818(4) . ? O1 H49 1.01(4) . ? O3 H50 1.06(4) . ? O4 H50 1.41(4) . ? C1 C2 1.371(6) . ? C1 C6 1.402(5) . ? C2 C3 1.397(6) . ? C2 H2 0.9500 . ? C3 C4 1.370(7) . ? C3 H3 0.9500 . ? C4 C5 1.379(7) . ? C4 H4 0.9500 . ? C5 C6 1.380(6) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.388(5) . ? C7 C8 1.392(6) . ? C8 C9 1.394(6) . ? C8 H8 0.9500 . ? C9 C10 1.368(7) . ? C9 H9 0.9500 . ? C10 C11 1.373(7) . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.384(5) . ? C13 C18 1.389(5) . ? C14 C15 1.387(5) . ? C14 H14 0.9500 . ? C15 C16 1.373(6) . ? C15 H15 0.9500 . ? C16 C17 1.383(6) . ? C16 H16 0.9500 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C20 1.387(5) . ? C19 C24 1.387(5) . ? C20 C21 1.382(5) . ? C20 H20 0.9500 . ? C21 C22 1.372(6) . ? C21 H21 0.9500 . ? C22 C23 1.381(6) . ? C22 H22 0.9500 . ? C23 C24 1.380(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.389(5) . ? C25 C30 1.401(5) . ? C26 C27 1.397(6) . ? C26 H26 0.9500 . ? C27 C28 1.376(6) . ? C27 H27 0.9500 . ? C28 C29 1.380(6) . ? C28 H28 0.9500 . ? C29 C30 1.378(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.389(5) . ? C31 C36 1.393(6) . ? C32 C33 1.389(6) . ? C32 H32 0.9500 . ? C33 C34 1.370(6) . ? C33 H33 0.9500 . ? C34 C35 1.382(6) . ? C34 H34 0.9500 . ? C35 C36 1.385(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C38 1.394(6) . ? C37 C42 1.395(6) . ? C38 C39 1.386(6) . ? C38 H38 0.9500 . ? C39 C40 1.369(6) . ? C39 H39 0.9500 . ? C40 C41 1.369(7) . ? C40 H40 0.9500 . ? C41 C42 1.380(6) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C48B 1.344(15) . ? C43 C44 1.382(6) . ? C43 C48A 1.48(5) . ? C44 C45 1.377(6) . ? C44 H44 0.9500 . ? C45 C46 1.347(7) . ? C45 H45 0.9500 . ? C46 C47B 1.377(16) . ? C46 C47A 1.48(3) . ? C47A C47B 0.82(3) . ? C47A C48A 1.38(2) . ? C47A C48B 1.61(5) . ? C47B C48B 1.436(18) . ? C47B C48A 1.60(5) . ? C48A C48B 0.73(4) . ? 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 P2 Pd1 P1 92.56(4) . . ? P2 Pd1 Cl1 93.85(4) . . ? P1 Pd1 Cl1 171.87(3) . . ? P2 Pd1 Cl1 177.06(3) . 2_566 ? P1 Pd1 Cl1 89.77(4) . 2_566 ? Cl1 Pd1 Cl1 83.99(4) . 2_566 ? P3 Pd2 P4 91.69(5) . . ? P3 Pd2 Cl2 168.14(4) . . ? P4 Pd2 Cl2 93.84(4) . . ? P3 Pd2 Cl2 91.09(4) . 2_577 ? P4 Pd2 Cl2 175.05(3) . 2_577 ? Cl2 Pd2 Cl2 84.19(4) . 2_577 ? Pd1 Cl1 Pd1 96.01(4) . 2_566 ? Pd2 Cl2 Pd2 95.81(4) . 2_577 ? O1 P1 C1 108.99(17) . . ? O1 P1 C7 105.99(17) . . ? C1 P1 C7 106.61(18) . . ? O1 P1 Pd1 117.83(11) . . ? C1 P1 Pd1 111.19(13) . . ? C7 P1 Pd1 105.49(12) . . ? O2 P2 C13 106.40(16) . . ? O2 P2 C19 105.65(16) . . ? C13 P2 C19 103.87(16) . . ? O2 P2 Pd1 116.85(11) . . ? C13 P2 Pd1 113.46(12) . . ? C19 P2 Pd1 109.56(12) . . ? O3 P3 C25 105.17(17) . . ? O3 P3 C31 106.71(17) . . ? C25 P3 C31 107.53(17) . . ? O3 P3 Pd2 118.80(11) . . ? C25 P3 Pd2 109.91(12) . . ? C31 P3 Pd2 108.18(13) . . ? O4 P4 C43 107.36(17) . . ? O4 P4 C37 106.33(17) . . ? C43 P4 C37 108.07(17) . . ? O4 P4 Pd2 118.45(11) . . ? C43 P4 Pd2 106.73(13) . . ? C37 P4 Pd2 109.52(13) . . ? P1 O1 H49 124(2) . . ? P3 O3 H50 118(2) . . ? P4 O4 H50 116.4(17) . . ? C2 C1 C6 119.0(4) . . ? C2 C1 P1 121.1(3) . . ? C6 C1 P1 119.8(3) . . ? C1 C2 C3 120.6(4) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C4 C3 C2 120.0(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 120.0(4) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 118.9(4) . . ? C12 C7 P1 122.9(3) . . ? C8 C7 P1 118.1(3) . . ? C7 C8 C9 120.1(4) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.3(5) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.6(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C7 120.1(4) . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? C14 C13 C18 118.2(3) . . ? C14 C13 P2 117.0(3) . . ? C18 C13 P2 124.7(3) . . ? C13 C14 C15 121.0(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C16 C15 C14 120.2(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.4(4) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 120.3(4) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C13 120.8(4) . . ? C17 C18 H18 119.6 . . ? C13 C18 H18 119.6 . . ? C20 C19 C24 119.4(3) . . ? C20 C19 P2 123.2(3) . . ? C24 C19 P2 117.4(3) . . ? C21 C20 C19 119.5(4) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C22 C21 C20 121.0(4) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 119.7(4) . . ? C24 C23 H23 120.1 . . ? C22 C23 H23 120.1 . . ? C23 C24 C19 120.5(4) . . ? C23 C24 H24 119.7 . . ? C19 C24 H24 119.7 . . ? C26 C25 C30 119.8(4) . . ? C26 C25 P3 123.3(3) . . ? C30 C25 P3 116.9(3) . . ? C25 C26 C27 119.0(4) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C28 C27 C26 120.4(4) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 120.8(4) . . ? C27 C28 H28 119.6 . . ? C29 C28 H28 119.6 . . ? C30 C29 C28 119.5(4) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C25 120.5(4) . . ? C29 C30 H30 119.7 . . ? C25 C30 H30 119.7 . . ? C32 C31 C36 118.8(4) . . ? C32 C31 P3 118.3(3) . . ? C36 C31 P3 122.9(3) . . ? C33 C32 C31 120.5(4) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.1(4) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.3(4) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 120.0(4) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 120.4(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C38 C37 C42 118.0(4) . . ? C38 C37 P4 124.2(3) . . ? C42 C37 P4 117.8(3) . . ? C39 C38 C37 120.8(4) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 120.0(4) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C41 C40 C39 120.1(4) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.5(4) . . ? C40 C41 H41 119.7 . . ? C42 C41 H41 119.7 . . ? C41 C42 C37 120.5(4) . . ? C41 C42 H42 119.7 . . ? C37 C42 H42 119.7 . . ? C48B C43 C44 117.9(6) . . ? C48B C43 C48A 29.4(9) . . ? C44 C43 C48A 116.8(8) . . ? C48B C43 P4 123.4(7) . . ? C44 C43 P4 117.2(3) . . ? C48A C43 P4 122.9(9) . . ? C45 C44 C43 120.9(4) . . ? C45 C44 H44 119.5 . . ? C43 C44 H44 119.5 . . ? C46 C45 C44 121.3(4) . . ? C46 C45 H45 119.3 . . ? C44 C45 H45 119.3 . . ? C45 C46 C47B 117.0(7) . . ? C45 C46 C47A 117.6(6) . . ? C47B C46 C47A 33.2(9) . . ? C47B C47A C48A 90(5) . . ? C47B C47A C46 66(3) . . ? C48A C47A C46 118(3) . . ? C47B C47A C48B 63(3) . . ? C48A C47A C48B 27(2) . . ? C46 C47A C48B 104(3) . . ? C47A C47B C46 80(3) . . ? C47A C47B C48B 86(3) . . ? C46 C47B C48B 119.5(17) . . ? C47A C47B C48A 59(4) . . ? C46 C47B C48A 111(2) . . ? C48B C47B C48A 27.0(10) . . ? C48B C48A C47A 94(5) . . ? C48B C48A C43 65(4) . . ? C47A C48A C43 118(3) . . ? C48B C48A C47B 64(3) . . ? C47A C48A C47B 30.9(19) . . ? C43 C48A C47B 102(4) . . ? C48A C48B C43 86(4) . . ? C48A C48B C47B 89(3) . . ? C43 C48B C47B 119.8(12) . . ? C48A C48B C47A 59(3) . . ? C43 C48B C47A 112(2) . . ? C47B C48B C47A 30.7(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H49 O2 1.01(4) 1.49(4) 2.411(4) 148(4) . O3 H50 O4 1.06(4) 1.41(4) 2.400(4) 152(4) . _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.924 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.093 # start Validation Reply Form _vrf_PLAT772_{u-ClPd{PPh2OH}{PPh2O}}2 ; PROBLEM: Suspect O-H Bond in CIF: O4 -- H50 .. 1.41 Ang. RESPONSE: Hydrogen Bond from O4..H50 demonstrates a O..H..O bridge which is an exception to PLAT772 alert level A ; # end Validation Reply Form #===END data_{X2Pd{1}}CH3Ph _database_code_depnum_ccdc_archive 'CCDC 701816' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H38 Br0.57 Cl1.43 N4 Pd, C7 H8' _chemical_formula_sum 'C41 H46 Br0.57 Cl1.43 N4 Pd' _chemical_formula_weight 797.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 _symmetry_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.392(2) _cell_length_b 13.675(3) _cell_length_c 15.092(3) _cell_angle_alpha 109.66(3) _cell_angle_beta 91.31(3) _cell_angle_gamma 111.21(3) _cell_volume 1857.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4694 _cell_measurement_theta_min 2.1313 _cell_measurement_theta_max 26.3732 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 821 _exptl_absorpt_coefficient_mu 1.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7705 _exptl_absorpt_correction_T_max 0.8852 _exptl_absorpt_process_details 'REQAB, Rigaku/MSC, The Woodlands, TX, USA, 1999.' _exptl_special_details ? _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Sealed Tube' _diffrn_radiation_monochromator 'Graphite Monochromator' _diffrn_radiation_detector CCD _diffrn_measurement_device ; Mercury CCD (2x2 bin mode) ; _diffrn_detector_area_resol_mean 14.6306 _diffrn_measurement_method omega _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_measurement_details ; scan: Number of images: 260 Slice: -40.0000 - 90.0000 Image width: 0.5000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 0.0000 XTD: 27.6329 2theta: -0.3627 scan: Number of images: 220 Slice: -40.0000 - 90.0000 Image width: 0.5000 Exp time: 15.0000 Rotation axis: Omega Omega: 0.0000 Chi: 45.0000 Phi: 90.0000 XTD: 27.6329 2theta: -0.3627 ; _diffrn_measurement_device_details ; AFC8: Eulerian 3 circle ; _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13822 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 25.10 _reflns_number_total 6539 _reflns_number_gt 4343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku/MSC,2001)' _computing_cell_refinement 'CrystalClear (Rigaku/MSC,2001)' _computing_data_reduction 'CrystalClear (Rigaku/MSC,2001)' _computing_structure_solution 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_structure_refinement 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_molecular_graphics 'SHELXTL 6.10 (Bruker AXS,2000)' _computing_publication_material 'SHELXTL 6.10 (Bruker AXS,2000)' # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 1.000 1.000 48.7 7.5 _platon_squeeze_details ; ; _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. Platon squeeze function was used to account for disordered solvent in void. ; _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^)+(0.0010P)^2^+9.5800P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6539 _refine_ls_number_parameters 473 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.1196 _refine_ls_wR_factor_gt 0.1073 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.025 _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 0.75099(6) 0.68261(5) 0.30786(3) 0.03243(16) Uani 1 1 d . . . Br1 Br 0.50269(12) 0.61274(12) 0.28809(8) 0.0510(5) Uani 0.384(6) 1 d P . . Br2 Br 0.99613(13) 0.76445(10) 0.32777(8) 0.0337(5) Uani 0.188(5) 1 d P . . Cl1 Cl 0.50269(12) 0.61274(12) 0.28809(8) 0.0510(5) Uani 0.616(6) 1 d P . . Cl2 Cl 0.99613(13) 0.76445(10) 0.32777(8) 0.0337(5) Uani 0.812(5) 1 d P . . N1 N 0.7090(5) 0.5873(5) 0.0918(3) 0.0314(12) Uani 1 1 d . . . N2 N 0.7849(6) 0.7684(5) 0.1453(4) 0.0408(14) Uani 1 1 d . . . N3 N 0.8057(6) 0.7687(4) 0.5251(3) 0.0318(12) Uani 1 1 d . . . N4 N 0.7162(5) 0.5880(4) 0.4656(3) 0.0258(11) Uani 1 1 d . . . C1 C 0.8171(6) 0.3799(5) 0.2162(4) 0.0294(13) Uani 1 1 d . . . H1 H 0.7215 0.3294 0.1992 0.035 Uiso 1 1 calc R . . C2 C 0.8839(6) 0.4157(5) 0.3087(4) 0.0257(12) Uani 1 1 d . . . C3 C 1.0238(6) 0.4891(5) 0.3325(4) 0.0322(14) Uani 1 1 d . . . H3 H 1.0720 0.5137 0.3952 0.039 Uiso 1 1 calc R . . C4 C 1.0944(7) 0.5272(5) 0.2656(4) 0.0332(14) Uani 1 1 d . . . H4 H 1.1895 0.5787 0.2831 0.040 Uiso 1 1 calc R . . C5 C 1.0262(6) 0.4900(5) 0.1742(4) 0.0302(13) Uani 1 1 d . . . H5 H 1.0753 0.5153 0.1286 0.036 Uiso 1 1 calc R . . C6 C 0.8853(6) 0.4156(5) 0.1471(4) 0.0267(13) Uani 1 1 d . . . C7 C 0.8153(6) 0.3708(5) 0.0454(4) 0.0308(14) Uani 1 1 d . . . C8 C 0.8677(8) 0.3071(6) -0.0240(5) 0.0424(17) Uani 1 1 d . . . H8 H 0.9460 0.2931 -0.0067 0.051 Uiso 1 1 calc R . . C9 C 0.8061(9) 0.2631(6) -0.1194(5) 0.052(2) Uani 1 1 d . . . H9 H 0.8439 0.2208 -0.1670 0.063 Uiso 1 1 calc R . . C10 C 0.6909(8) 0.2807(6) -0.1448(5) 0.051(2) Uani 1 1 d . . . H10 H 0.6471 0.2485 -0.2096 0.062 Uiso 1 1 calc R . . C11 C 0.6393(7) 0.3450(6) -0.0762(5) 0.0453(18) Uani 1 1 d . . . H11 H 0.5596 0.3569 -0.0941 0.054 Uiso 1 1 calc R . . C12 C 0.7020(6) 0.3931(6) 0.0193(4) 0.0340(15) Uani 1 1 d . . . C13 C 0.6488(7) 0.4714(6) 0.0897(4) 0.0376(16) Uani 1 1 d . . . H13A H 0.5457 0.4419 0.0731 0.045 Uiso 1 1 calc R . . H13B H 0.6710 0.4724 0.1542 0.045 Uiso 1 1 calc R . . C14 C 0.7257(7) 0.6181(7) 0.0127(4) 0.0395(17) Uani 1 1 d . . . H14 H 0.7078 0.5688 -0.0521 0.047 Uiso 1 1 calc R . . C15 C 0.7715(7) 0.7297(7) 0.0454(5) 0.0434(18) Uani 1 1 d . . . H15 H 0.7917 0.7754 0.0079 0.052 Uiso 1 1 calc R . . C16 C 0.7461(6) 0.6783(6) 0.1730(4) 0.0321(15) Uani 1 1 d . . . C17 C 0.8303(9) 0.8871(7) 0.2103(5) 0.057(2) Uani 1 1 d D . . C18A C 0.7056(19) 0.9159(13) 0.1709(19) 0.049(6) Uani 0.479(17) 1 d PD . . C18 C 0.726(2) 0.9393(16) 0.2384(19) 0.063(5) Uani 0.521(17) 1 d PD . . C19 C 0.659(2) 0.9478(15) 0.1534(17) 0.075(7) Uani 0.479(17) 1 d PD . . C19A C 0.7306(16) 1.0335(12) 0.2402(10) 0.050(5) Uani 0.521(17) 1 d PD . . C20 C 0.626(2) 1.0691(18) 0.1927(17) 0.091(8) Uani 0.521(17) 1 d PD . . C20A C 0.722(3) 1.047(3) 0.140(2) 0.167(19) Uani 0.479(17) 1 d PD . . C21 C 0.5981(9) 1.0186(7) 0.6288(6) 0.063(2) Uani 1 1 d . . . H21A H 0.6528 1.0905 0.6224 0.095 Uiso 1 1 calc R . . H21B H 0.5646 1.0334 0.6902 0.095 Uiso 1 1 calc R . . H21C H 0.5179 0.9748 0.5769 0.095 Uiso 1 1 calc R . . C22 C 0.6879(8) 0.9535(6) 0.6241(5) 0.0467(18) Uani 1 1 d . . . H22A H 0.6303 0.8789 0.6260 0.056 Uiso 1 1 calc R . . H22B H 0.7626 0.9942 0.6807 0.056 Uiso 1 1 calc R . . C23 C 0.7537(8) 0.9367(6) 0.5359(5) 0.0472(18) Uani 1 1 d . . . H23A H 0.7972 1.0104 0.5286 0.057 Uiso 1 1 calc R . . H23B H 0.6790 0.8859 0.4801 0.057 Uiso 1 1 calc R . . C24 C 0.8639(8) 0.8875(5) 0.5341(5) 0.0414(17) Uani 1 1 d . . . H24A H 0.9139 0.8938 0.4799 0.050 Uiso 1 1 calc R . . H24B H 0.9331 0.9328 0.5935 0.050 Uiso 1 1 calc R . . C25 C 0.7589(6) 0.6793(5) 0.4413(4) 0.0269(13) Uani 1 1 d . . . C26 C 0.7887(7) 0.7310(6) 0.6017(4) 0.0324(14) Uani 1 1 d . . . H26 H 0.8129 0.7770 0.6677 0.039 Uiso 1 1 calc R . . C27 C 0.7324(6) 0.6188(6) 0.5644(4) 0.0323(14) Uani 1 1 d . . . H27 H 0.7081 0.5692 0.5984 0.039 Uiso 1 1 calc R . . C28 C 0.6477(7) 0.4717(5) 0.3956(4) 0.0338(14) Uani 1 1 d . . . H28A H 0.6647 0.4713 0.3312 0.041 Uiso 1 1 calc R . . H28B H 0.5454 0.4453 0.3951 0.041 Uiso 1 1 calc R . . C29 C 0.6995(6) 0.3910(5) 0.4165(4) 0.0299(13) Uani 1 1 d . . . C30 C 0.6344(7) 0.3386(5) 0.4779(4) 0.0354(15) Uani 1 1 d . . . H30 H 0.5550 0.3506 0.5012 0.042 Uiso 1 1 calc R . . C31 C 0.6833(8) 0.2695(6) 0.5055(5) 0.0440(17) Uani 1 1 d . . . H31 H 0.6370 0.2338 0.5467 0.053 Uiso 1 1 calc R . . C32 C 0.7991(8) 0.2529(5) 0.4731(5) 0.0422(17) Uani 1 1 d . . . H32 H 0.8359 0.2089 0.4943 0.051 Uiso 1 1 calc R . . C33 C 0.8624(7) 0.3007(5) 0.4088(5) 0.0398(16) Uani 1 1 d . . . H33 H 0.9402 0.2867 0.3847 0.048 Uiso 1 1 calc R . . C34 C 0.8127(6) 0.3694(5) 0.3793(4) 0.0283(13) Uani 1 1 d . . . C35 C 0.6631(16) 0.8205(14) 0.8466(7) 0.099(4) Uani 1 1 d . . . C36 C 0.6472(11) 0.7108(9) 0.8143(5) 0.069(3) Uani 1 1 d . . . H36 H 0.5559 0.6526 0.7949 0.083 Uiso 1 1 calc R . . C37 C 0.7608(10) 0.6837(7) 0.8095(5) 0.0493(19) Uani 1 1 d . . . H37 H 0.7485 0.6066 0.7848 0.059 Uiso 1 1 calc R . . C38 C 0.8961(10) 0.7682(7) 0.8406(5) 0.055(2) Uani 1 1 d . . . H38 H 0.9756 0.7490 0.8378 0.066 Uiso 1 1 calc R . . C39 C 0.9124(11) 0.8810(7) 0.8759(5) 0.067(3) Uani 1 1 d . . . H39 H 1.0037 0.9390 0.8968 0.080 Uiso 1 1 calc R . . C40 C 0.797(2) 0.9096(11) 0.8807(7) 0.105(5) Uani 1 1 d . . . C41 C 0.7916(15) 1.0256(9) 0.9152(7) 0.050(4) Uani 0.60 1 d P . . C41A C 0.580(2) 0.894(3) 0.8594(16) 0.090(9) Uani 0.40 1 d P . . 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 0.0397(3) 0.0520(3) 0.0212(3) 0.0211(2) 0.0127(2) 0.0278(2) Br1 0.0353(7) 0.1045(11) 0.0325(7) 0.0364(7) 0.0142(5) 0.0377(7) Br2 0.0365(8) 0.0431(8) 0.0267(7) 0.0165(6) 0.0111(5) 0.0174(6) Cl1 0.0353(7) 0.1045(11) 0.0325(7) 0.0364(7) 0.0142(5) 0.0377(7) Cl2 0.0365(8) 0.0431(8) 0.0267(7) 0.0165(6) 0.0111(5) 0.0174(6) N1 0.033(3) 0.060(4) 0.014(3) 0.019(3) 0.008(2) 0.027(3) N2 0.057(4) 0.069(4) 0.027(3) 0.034(3) 0.024(3) 0.043(3) N3 0.045(3) 0.042(3) 0.017(3) 0.015(2) 0.010(2) 0.023(3) N4 0.031(3) 0.040(3) 0.016(2) 0.015(2) 0.007(2) 0.019(2) C1 0.019(3) 0.040(3) 0.030(3) 0.014(3) 0.003(2) 0.012(3) C2 0.021(3) 0.033(3) 0.028(3) 0.012(3) 0.004(2) 0.014(2) C3 0.034(4) 0.035(3) 0.025(3) 0.008(3) -0.001(3) 0.014(3) C4 0.026(3) 0.039(4) 0.034(4) 0.014(3) 0.003(3) 0.011(3) C5 0.023(3) 0.035(3) 0.036(3) 0.017(3) 0.010(3) 0.012(3) C6 0.027(3) 0.030(3) 0.023(3) 0.009(3) 0.006(2) 0.011(2) C7 0.025(3) 0.033(3) 0.032(3) 0.015(3) 0.008(3) 0.005(3) C8 0.054(5) 0.043(4) 0.034(4) 0.015(3) 0.020(3) 0.021(3) C9 0.077(6) 0.047(4) 0.038(4) 0.021(4) 0.032(4) 0.023(4) C10 0.053(5) 0.052(4) 0.030(4) 0.017(3) 0.003(3) -0.001(4) C11 0.034(4) 0.066(5) 0.032(4) 0.022(4) 0.005(3) 0.012(3) C12 0.022(3) 0.050(4) 0.024(3) 0.017(3) 0.004(3) 0.006(3) C13 0.028(4) 0.072(5) 0.023(3) 0.026(3) 0.009(3) 0.022(3) C14 0.041(4) 0.076(5) 0.021(3) 0.028(4) 0.013(3) 0.035(4) C15 0.050(4) 0.084(6) 0.031(4) 0.042(4) 0.021(3) 0.045(4) C16 0.033(4) 0.062(4) 0.025(3) 0.026(3) 0.016(3) 0.034(3) C17 0.098(7) 0.058(5) 0.044(4) 0.028(4) 0.035(4) 0.055(5) C18A 0.050(11) 0.023(9) 0.080(17) 0.016(10) -0.001(10) 0.024(7) C18 0.082(14) 0.047(10) 0.071(15) 0.019(10) 0.029(12) 0.036(9) C19 0.074(15) 0.031(11) 0.111(19) 0.017(11) -0.002(13) 0.022(10) C19A 0.058(10) 0.045(9) 0.049(9) 0.005(7) 0.009(7) 0.034(8) C20 0.087(15) 0.138(18) 0.16(2) 0.123(18) 0.075(15) 0.096(15) C20A 0.11(3) 0.20(3) 0.16(3) 0.14(3) -0.05(2) -0.03(2) C21 0.069(6) 0.057(5) 0.072(6) 0.023(5) 0.016(5) 0.033(4) C22 0.057(5) 0.036(4) 0.043(4) 0.010(3) 0.016(4) 0.017(3) C23 0.079(6) 0.040(4) 0.032(4) 0.014(3) 0.008(4) 0.033(4) C24 0.054(5) 0.038(4) 0.036(4) 0.018(3) 0.019(3) 0.018(3) C25 0.031(3) 0.044(4) 0.015(3) 0.013(3) 0.006(2) 0.023(3) C26 0.042(4) 0.054(4) 0.012(3) 0.016(3) 0.008(3) 0.026(3) C27 0.039(4) 0.052(4) 0.018(3) 0.018(3) 0.010(3) 0.026(3) C28 0.031(4) 0.049(4) 0.028(3) 0.020(3) 0.010(3) 0.018(3) C29 0.028(3) 0.037(3) 0.020(3) 0.010(3) 0.002(2) 0.008(3) C30 0.037(4) 0.041(4) 0.027(3) 0.015(3) 0.007(3) 0.013(3) C31 0.051(5) 0.044(4) 0.034(4) 0.022(3) 0.003(3) 0.010(3) C32 0.055(5) 0.039(4) 0.033(4) 0.019(3) -0.007(3) 0.014(3) C33 0.044(4) 0.039(4) 0.037(4) 0.014(3) 0.005(3) 0.018(3) C34 0.028(3) 0.034(3) 0.023(3) 0.012(3) 0.002(2) 0.011(3) C35 0.155(12) 0.171(13) 0.041(6) 0.044(8) 0.031(7) 0.136(11) C36 0.093(7) 0.124(8) 0.030(4) 0.039(5) 0.022(4) 0.074(7) C37 0.081(6) 0.069(5) 0.022(3) 0.027(3) 0.017(4) 0.044(5) C38 0.096(7) 0.073(6) 0.025(4) 0.029(4) 0.022(4) 0.055(5) C39 0.115(8) 0.060(5) 0.034(4) 0.023(4) 0.003(5) 0.041(5) C40 0.253(17) 0.100(9) 0.029(5) 0.031(6) 0.038(8) 0.135(11) C41 0.112(11) 0.022(5) 0.016(5) -0.005(4) -0.017(6) 0.039(6) C41A 0.053(14) 0.21(3) 0.066(15) 0.072(18) 0.035(12) 0.093(18) _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 C16 2.015(6) . ? Pd1 C25 2.031(5) . ? Pd1 Br2 2.3470(16) . ? Pd1 Br1 2.3768(15) . ? N1 C16 1.343(8) . ? N1 C14 1.389(7) . ? N1 C13 1.467(8) . ? N2 C16 1.360(8) . ? N2 C15 1.405(8) . ? N2 C17 1.474(9) . ? N3 C25 1.353(7) . ? N3 C26 1.407(7) . ? N3 C24 1.469(8) . ? N4 C25 1.343(7) . ? N4 C27 1.394(7) . ? N4 C28 1.473(8) . ? C1 C2 1.386(8) . ? C1 C6 1.397(7) . ? C1 H1 0.9500 . ? C2 C3 1.389(8) . ? C2 C34 1.495(7) . ? C3 C4 1.392(8) . ? C3 H3 0.9500 . ? C4 C5 1.373(8) . ? C4 H4 0.9500 . ? C5 C6 1.400(8) . ? C5 H5 0.9500 . ? C6 C7 1.501(8) . ? C7 C8 1.382(8) . ? C7 C12 1.399(9) . ? C8 C9 1.393(10) . ? C8 H8 0.9500 . ? C9 C10 1.373(11) . ? C9 H9 0.9500 . ? C10 C11 1.374(10) . ? C10 H10 0.9500 . ? C11 C12 1.394(9) . ? C11 H11 0.9500 . ? C12 C13 1.508(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.325(10) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C17 C18 1.499(18) . ? C17 C18A 1.64(2) . ? C18A C19 0.85(2) . ? C18A C18 0.95(2) . ? C18A C19A 1.52(2) . ? C18A C20A 1.95(4) . ? C18 C19A 1.26(2) . ? C18 C19 1.50(3) . ? C19 C20A 1.37(3) . ? C19 C19A 1.39(2) . ? C19 C20 1.73(2) . ? C19A C20 1.58(2) . ? C19A C20A 1.59(3) . ? C20 C20A 1.35(4) . ? C21 C22 1.494(10) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.497(9) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.520(10) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C26 C27 1.330(9) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.504(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.397(8) . ? C29 C34 1.399(8) . ? C30 C31 1.390(9) . ? C30 H30 0.9500 . ? C31 C32 1.374(10) . ? C31 H31 0.9500 . ? C32 C33 1.395(9) . ? C32 H32 0.9500 . ? C33 C34 1.402(8) . ? C33 H33 0.9500 . ? C35 C36 1.356(15) . ? C35 C40 1.419(18) . ? C35 C41A 1.51(2) . ? C36 C37 1.356(11) . ? C36 H36 0.9500 . ? C37 C38 1.401(12) . ? C37 H37 0.9500 . ? C38 C39 1.396(11) . ? C38 H38 0.9500 . ? C39 C40 1.381(16) . ? C39 H39 0.9500 . ? C40 C41 1.519(13) . ? 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 C16 Pd1 C25 176.8(3) . . ? C16 Pd1 Br2 88.08(18) . . ? C25 Pd1 Br2 91.19(17) . . ? C16 Pd1 Br1 90.69(18) . . ? C25 Pd1 Br1 90.26(17) . . ? Br2 Pd1 Br1 175.75(6) . . ? C16 N1 C14 111.3(5) . . ? C16 N1 C13 122.8(4) . . ? C14 N1 C13 125.8(5) . . ? C16 N2 C15 109.1(6) . . ? C16 N2 C17 125.0(5) . . ? C15 N2 C17 125.9(6) . . ? C25 N3 C26 110.0(5) . . ? C25 N3 C24 124.8(5) . . ? C26 N3 C24 125.3(5) . . ? C25 N4 C27 111.2(5) . . ? C25 N4 C28 123.3(5) . . ? C27 N4 C28 125.2(5) . . ? C2 C1 C6 122.3(5) . . ? C2 C1 H1 118.8 . . ? C6 C1 H1 118.8 . . ? C1 C2 C3 118.2(5) . . ? C1 C2 C34 121.5(5) . . ? C3 C2 C34 120.1(5) . . ? C2 C3 C4 120.9(6) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C5 C4 C3 119.8(6) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 121.1(5) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C1 C6 C5 117.6(5) . . ? C1 C6 C7 122.1(5) . . ? C5 C6 C7 120.1(5) . . ? C8 C7 C12 119.7(6) . . ? C8 C7 C6 118.0(6) . . ? C12 C7 C6 122.3(6) . . ? C7 C8 C9 120.2(7) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.2(7) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.8(7) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 121.0(7) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C11 C12 C7 118.9(6) . . ? C11 C12 C13 118.5(6) . . ? C7 C12 C13 122.5(5) . . ? N1 C13 C12 113.1(5) . . ? N1 C13 H13A 109.0 . . ? C12 C13 H13A 109.0 . . ? N1 C13 H13B 109.0 . . ? C12 C13 H13B 109.0 . . ? H13A C13 H13B 107.8 . . ? C15 C14 N1 106.4(6) . . ? C15 C14 H14 126.8 . . ? N1 C14 H14 126.8 . . ? C14 C15 N2 107.9(5) . . ? C14 C15 H15 126.1 . . ? N2 C15 H15 126.1 . . ? N1 C16 N2 105.3(5) . . ? N1 C16 Pd1 127.8(4) . . ? N2 C16 Pd1 126.8(5) . . ? N2 C17 C18 120.8(11) . . ? N2 C17 C18A 98.8(9) . . ? C18 C17 C18A 34.9(9) . . ? C19 C18A C18 113(3) . . ? C19 C18A C19A 65.0(19) . . ? C18 C18A C19A 56.0(15) . . ? C19 C18A C17 164(2) . . ? C18 C18A C17 64.6(16) . . ? C19A C18A C17 104.3(14) . . ? C19 C18A C20A 36(2) . . ? C18 C18A C20A 109(2) . . ? C19A C18A C20A 52.8(13) . . ? C17 C18A C20A 128.4(14) . . ? C18A C18 C19A 85.3(18) . . ? C18A C18 C17 80.5(18) . . ? C19A C18 C17 128.7(15) . . ? C18A C18 C19 31.2(14) . . ? C19A C18 C19 59.7(13) . . ? C17 C18 C19 110.3(17) . . ? C18A C19 C20A 122(3) . . ? C18A C19 C19A 81(2) . . ? C20A C19 C19A 70.6(16) . . ? C18A C19 C18 35.6(19) . . ? C20A C19 C18 115.7(19) . . ? C19A C19 C18 51.6(11) . . ? C18A C19 C20 141(3) . . ? C20A C19 C20 50(2) . . ? C19A C19 C20 59.9(12) . . ? C18 C19 C20 107.7(15) . . ? C18 C19A C19 68.7(13) . . ? C18 C19A C18A 38.7(10) . . ? C19 C19A C18A 33.5(10) . . ? C18 C19A C20 132.8(18) . . ? C19 C19A C20 70.6(14) . . ? C18A C19A C20 104.1(15) . . ? C18 C19A C20A 116(2) . . ? C19 C19A C20A 54.0(15) . . ? C18A C19A C20A 78(2) . . ? C20 C19A C20A 50.3(17) . . ? C20A C20 C19A 65.3(12) . . ? C20A C20 C19 51.0(16) . . ? C19A C20 C19 49.5(10) . . ? C20 C20A C19 78.9(19) . . ? C20 C20A C19A 64.5(17) . . ? C19 C20A C19A 55.5(13) . . ? C20 C20A C18A 93.7(15) . . ? C19 C20A C18A 21.5(13) . . ? C19A C20A C18A 49.4(11) . . ? 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 . . ? C21 C22 C23 112.7(6) . . ? C21 C22 H22A 109.1 . . ? C23 C22 H22A 109.1 . . ? C21 C22 H22B 109.1 . . ? C23 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? C22 C23 C24 115.2(6) . . ? C22 C23 H23A 108.5 . . ? C24 C23 H23A 108.5 . . ? C22 C23 H23B 108.5 . . ? C24 C23 H23B 108.5 . . ? H23A C23 H23B 107.5 . . ? N3 C24 C23 113.4(6) . . ? N3 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? N3 C24 H24B 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? N4 C25 N3 105.2(4) . . ? N4 C25 Pd1 127.5(4) . . ? N3 C25 Pd1 127.4(4) . . ? C27 C26 N3 107.0(5) . . ? C27 C26 H26 126.5 . . ? N3 C26 H26 126.5 . . ? C26 C27 N4 106.7(5) . . ? C26 C27 H27 126.7 . . ? N4 C27 H27 126.7 . . ? N4 C28 C29 112.8(5) . . ? N4 C28 H28A 109.0 . . ? C29 C28 H28A 109.0 . . ? N4 C28 H28B 109.0 . . ? C29 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C30 C29 C34 119.0(6) . . ? C30 C29 C28 118.5(6) . . ? C34 C29 C28 122.5(5) . . ? C31 C30 C29 121.4(6) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C30 119.7(6) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? C31 C32 C33 119.9(6) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C32 C33 C34 120.9(6) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C29 C34 C33 119.0(5) . . ? C29 C34 C2 123.1(5) . . ? C33 C34 C2 117.9(5) . . ? C36 C35 C40 121.4(11) . . ? C36 C35 C41A 141.6(18) . . ? C40 C35 C41A 96.9(16) . . ? C37 C36 C35 120.4(11) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 120.7(9) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C39 C38 C37 118.9(9) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C40 C39 C38 120.9(11) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C35 117.6(10) . . ? C39 C40 C41 129.4(15) . . ? C35 C40 C41 112.9(14) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.10 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.086 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.114 #===END