Electronic Supplementary Material for CrystEngComm this journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Martin Smith' _publ_contact_author_address ; Department of Chemistry Loughborough University Loughborough LEICESTERSHIRE LE11 3TU UNITED KINGDOM ; _publ_contact_author_email M.B.SMITH@LBORO.AC.UK _publ_section_title ; Hydrogen bonded supramolecular assemblies based on neutral square-planar palladium(II) complexes ; loop_ _publ_author_name 'Martin Smith' 'Simon J. Coles' 'Sophie H. Dale' 'Thomas Gelbrich' 'Peter N. Horton' M.Hursthouse ; M.E.Light ; data_2a.MeOH _database_code_depnum_ccdc_archive 'CCDC 626743' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr. M. Smith ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H33 Cl2 N O4 P2 Pd' _chemical_formula_sum 'C34 H33 Cl2 N O4 P2 Pd' _chemical_formula_weight 758.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8750(1) _cell_length_b 11.4418(1) _cell_length_c 14.8044(2) _cell_angle_alpha 107.154(1) _cell_angle_beta 98.373(1) _cell_angle_gamma 108.360(1) _cell_volume 1611.75(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6947 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.881 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8164 _exptl_absorpt_correction_T_max 0.9656 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28221 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7359 _reflns_number_gt 6605 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0208P)^2^+1.6227P] 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 7359 _refine_ls_number_parameters 401 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0705 _refine_ls_wR_factor_gt 0.0671 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7317(2) 0.9860(2) 0.65854(14) 0.0142(4) Uani 1 1 d . . . C2 C 0.6046(2) 0.8856(2) 0.62690(17) 0.0215(5) Uani 1 1 d . . . H2 H 0.5685 0.8486 0.6714 0.026 Uiso 1 1 calc R . . C3 C 0.5307(2) 0.8396(2) 0.52977(18) 0.0298(6) Uani 1 1 d . . . H3 H 0.4442 0.7710 0.5082 0.036 Uiso 1 1 calc R . . C4 C 0.5818(3) 0.8927(3) 0.46480(17) 0.0297(6) Uani 1 1 d . . . H4 H 0.5316 0.8593 0.3983 0.036 Uiso 1 1 calc R . . C5 C 0.7061(2) 0.9944(3) 0.49603(16) 0.0262(5) Uani 1 1 d . . . H5 H 0.7403 1.0324 0.4514 0.031 Uiso 1 1 calc R . . C6 C 0.7814(2) 1.0415(2) 0.59261(16) 0.0193(4) Uani 1 1 d . . . H6 H 0.8669 1.1116 0.6138 0.023 Uiso 1 1 calc R . . C7 C 0.80282(19) 1.17771(19) 0.85844(14) 0.0127(4) Uani 1 1 d . . . C8 C 0.6782(2) 1.1870(2) 0.83264(16) 0.0183(4) Uani 1 1 d . . . H8 H 0.6134 1.1245 0.7738 0.022 Uiso 1 1 calc R . . C9 C 0.6496(2) 1.2878(2) 0.89327(18) 0.0254(5) Uani 1 1 d . . . H9 H 0.5651 1.2943 0.8758 0.030 Uiso 1 1 calc R . . C10 C 0.7438(2) 1.3789(2) 0.97913(18) 0.0245(5) Uani 1 1 d . . . H10 H 0.7243 1.4484 1.0198 0.029 Uiso 1 1 calc R . . C11 C 0.8671(2) 1.3688(2) 1.00591(16) 0.0215(5) Uani 1 1 d . . . H11 H 0.9310 1.4305 1.0654 0.026 Uiso 1 1 calc R . . C12 C 0.8968(2) 1.2685(2) 0.94564(15) 0.0168(4) Uani 1 1 d . . . H12 H 0.9811 1.2618 0.9638 0.020 Uiso 1 1 calc R . . C13 C 0.96769(19) 0.77785(19) 0.61931(14) 0.0124(4) Uani 1 1 d . . . C14 C 0.9310(2) 0.6402(2) 0.58697(15) 0.0160(4) Uani 1 1 d . . . H14 H 0.9410 0.5986 0.6329 0.019 Uiso 1 1 calc R . . C15 C 0.8798(2) 0.5653(2) 0.48744(16) 0.0190(4) Uani 1 1 d . . . H15 H 0.8548 0.4721 0.4653 0.023 Uiso 1 1 calc R . . C16 C 0.8651(2) 0.6258(2) 0.42019(16) 0.0197(4) Uani 1 1 d . . . H16 H 0.8308 0.5739 0.3522 0.024 Uiso 1 1 calc R . . C17 C 0.9000(2) 0.7608(2) 0.45159(15) 0.0195(4) Uani 1 1 d . . . H17 H 0.8885 0.8016 0.4053 0.023 Uiso 1 1 calc R . . C18 C 0.9521(2) 0.8373(2) 0.55096(15) 0.0161(4) Uani 1 1 d . . . H18 H 0.9770 0.9304 0.5723 0.019 Uiso 1 1 calc R . . C19 C 1.17980(19) 0.85286(19) 0.79614(15) 0.0128(4) Uani 1 1 d . . . C20 C 1.2352(2) 0.7749(2) 0.73757(17) 0.0203(5) Uani 1 1 d . . . H20 H 1.1994 0.7381 0.6684 0.024 Uiso 1 1 calc R . . C21 C 1.3431(2) 0.7511(2) 0.78059(19) 0.0254(5) Uani 1 1 d . . . H21 H 1.3802 0.6972 0.7408 0.031 Uiso 1 1 calc R . . C22 C 1.3963(2) 0.8058(2) 0.88131(18) 0.0251(5) Uani 1 1 d . . . H22 H 1.4691 0.7887 0.9106 0.030 Uiso 1 1 calc R . . C23 C 1.3432(2) 0.8856(2) 0.93914(17) 0.0216(5) Uani 1 1 d . . . H23 H 1.3802 0.9235 1.0081 0.026 Uiso 1 1 calc R . . C24 C 1.2366(2) 0.9104(2) 0.89712(15) 0.0165(4) Uani 1 1 d . . . H24 H 1.2019 0.9668 0.9372 0.020 Uiso 1 1 calc R . . C25 C 0.67055(19) 0.67254(19) 0.77402(15) 0.0128(4) Uani 1 1 d . . . C26 C 0.5980(2) 0.5883(2) 0.67715(15) 0.0147(4) Uani 1 1 d . . . C27 C 0.4868(2) 0.4738(2) 0.65757(16) 0.0183(4) Uani 1 1 d . . . H27 H 0.4385 0.4182 0.5918 0.022 Uiso 1 1 calc R . . C28 C 0.4471(2) 0.4417(2) 0.73467(16) 0.0185(4) Uani 1 1 d . . . H28 H 0.3713 0.3637 0.7217 0.022 Uiso 1 1 calc R . . C29 C 0.5170(2) 0.5223(2) 0.83060(16) 0.0180(4) Uani 1 1 d . . . H29 H 0.4884 0.4992 0.8828 0.022 Uiso 1 1 calc R . . C30 C 0.62965(19) 0.63803(19) 0.85172(15) 0.0135(4) Uani 1 1 d . . . C31 C 0.7022(2) 0.7194(2) 0.95678(15) 0.0153(4) Uani 1 1 d . . . C32 C 0.77120(19) 0.91605(19) 0.83275(14) 0.0120(4) Uani 1 1 d . . . H32A H 0.8206 0.9487 0.9026 0.014 Uiso 1 1 calc R . . H32B H 0.6758 0.9017 0.8299 0.014 Uiso 1 1 calc R . . C33 C 0.91475(19) 0.78772(19) 0.80778(14) 0.0118(4) Uani 1 1 d . . . H33A H 0.9082 0.6949 0.7875 0.014 Uiso 1 1 calc R . . H33B H 0.9518 0.8291 0.8798 0.014 Uiso 1 1 calc R . . N1 N 0.78014(16) 0.78958(16) 0.78170(12) 0.0109(3) Uani 1 1 d . . . O1 O 0.63478(15) 0.61585(15) 0.59953(10) 0.0210(3) Uani 1 1 d . . . H1 H 0.7038 0.6856 0.6199 0.031 Uiso 1 1 calc R . . O2 O 0.81362(14) 0.80487(14) 0.98620(10) 0.0166(3) Uani 1 1 d . . . O3 O 0.62897(16) 0.68778(18) 1.01725(12) 0.0314(4) Uani 1 1 d . . . H3A H 0.6740 0.7328 1.0756 0.047 Uiso 1 1 calc R . . P1 P 0.83927(5) 1.04354(5) 0.78153(4) 0.01011(10) Uani 1 1 d . . . P2 P 1.02971(5) 0.87640(5) 0.74882(4) 0.00985(10) Uani 1 1 d . . . Cl1 Cl 1.09027(5) 1.30984(5) 0.79785(4) 0.01580(11) Uani 1 1 d . . . Cl2 Cl 1.27548(5) 1.12727(5) 0.76031(4) 0.01589(11) Uani 1 1 d . . . Pd1 Pd 1.054906(14) 1.088060(13) 0.777075(10) 0.00946(5) Uani 1 1 d . . . C41 C 0.7936(3) 1.3786(3) 0.6756(3) 0.0606(10) Uani 1 1 d . . . H41A H 0.7467 1.3301 0.7130 0.091 Uiso 1 1 calc R . . H41B H 0.8074 1.3169 0.6200 0.091 Uiso 1 1 calc R . . H41C H 0.7394 1.4226 0.6514 0.091 Uiso 1 1 calc R . . O41 O 0.9175(2) 1.47301(18) 0.73590(14) 0.0388(5) Uani 1 1 d . . . H41 H 0.9646 1.4352 0.7557 0.058 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 C1 0.0164(10) 0.0131(10) 0.0121(9) 0.0017(8) 0.0008(8) 0.0084(8) C2 0.0178(11) 0.0190(11) 0.0228(11) 0.0055(9) -0.0010(9) 0.0054(9) C3 0.0246(12) 0.0216(12) 0.0297(13) 0.0014(10) -0.0099(10) 0.0063(10) C4 0.0352(14) 0.0334(14) 0.0160(11) 0.0012(10) -0.0061(10) 0.0201(11) C5 0.0347(13) 0.0369(14) 0.0157(11) 0.0110(10) 0.0066(10) 0.0232(11) C6 0.0197(11) 0.0252(12) 0.0160(10) 0.0078(9) 0.0047(8) 0.0119(9) C7 0.0146(9) 0.0108(9) 0.0141(9) 0.0045(8) 0.0059(8) 0.0058(8) C8 0.0179(10) 0.0184(11) 0.0189(11) 0.0051(9) 0.0033(8) 0.0097(9) C9 0.0255(12) 0.0280(13) 0.0309(13) 0.0114(10) 0.0106(10) 0.0186(10) C10 0.0317(13) 0.0165(11) 0.0290(13) 0.0052(10) 0.0150(10) 0.0133(10) C11 0.0223(11) 0.0157(11) 0.0182(11) -0.0014(9) 0.0064(9) 0.0028(9) C12 0.0161(10) 0.0153(10) 0.0162(10) 0.0032(8) 0.0045(8) 0.0046(8) C13 0.0097(9) 0.0152(10) 0.0111(9) 0.0017(8) 0.0037(7) 0.0054(8) C14 0.0159(10) 0.0141(10) 0.0172(10) 0.0038(8) 0.0035(8) 0.0069(8) C15 0.0183(10) 0.0164(10) 0.0174(10) -0.0001(8) 0.0029(8) 0.0070(8) C16 0.0152(10) 0.0243(11) 0.0131(10) -0.0001(9) 0.0025(8) 0.0061(9) C17 0.0200(11) 0.0247(11) 0.0130(10) 0.0073(9) 0.0039(8) 0.0074(9) C18 0.0161(10) 0.0159(10) 0.0156(10) 0.0054(8) 0.0049(8) 0.0052(8) C19 0.0105(9) 0.0107(9) 0.0173(10) 0.0055(8) 0.0038(7) 0.0036(7) C20 0.0157(10) 0.0190(11) 0.0213(11) 0.0005(9) 0.0040(8) 0.0069(9) C21 0.0159(11) 0.0227(12) 0.0376(14) 0.0053(10) 0.0075(10) 0.0122(9) C22 0.0152(11) 0.0312(13) 0.0357(14) 0.0175(11) 0.0049(9) 0.0134(10) C23 0.0155(10) 0.0318(13) 0.0190(11) 0.0125(10) 0.0026(8) 0.0087(9) C24 0.0142(10) 0.0195(11) 0.0180(10) 0.0076(8) 0.0061(8) 0.0078(8) C25 0.0094(9) 0.0110(9) 0.0177(10) 0.0051(8) 0.0029(7) 0.0038(7) C26 0.0159(10) 0.0144(10) 0.0149(10) 0.0044(8) 0.0045(8) 0.0079(8) C27 0.0163(10) 0.0138(10) 0.0179(10) -0.0003(8) -0.0004(8) 0.0045(8) C28 0.0161(10) 0.0133(10) 0.0267(12) 0.0091(9) 0.0051(9) 0.0047(8) C29 0.0160(10) 0.0165(10) 0.0244(11) 0.0102(9) 0.0062(8) 0.0070(8) C30 0.0117(9) 0.0132(10) 0.0166(10) 0.0046(8) 0.0029(8) 0.0070(8) C31 0.0151(10) 0.0174(10) 0.0185(10) 0.0096(8) 0.0060(8) 0.0091(8) C32 0.0116(9) 0.0119(9) 0.0136(9) 0.0048(8) 0.0046(7) 0.0051(7) C33 0.0115(9) 0.0126(9) 0.0128(9) 0.0058(8) 0.0023(7) 0.0058(8) N1 0.0096(8) 0.0095(8) 0.0129(8) 0.0033(6) 0.0031(6) 0.0036(6) O1 0.0182(8) 0.0232(8) 0.0122(7) 0.0031(6) 0.0016(6) 0.0000(6) O2 0.0153(7) 0.0173(7) 0.0137(7) 0.0054(6) 0.0021(6) 0.0026(6) O3 0.0217(8) 0.0431(11) 0.0144(8) 0.0068(8) 0.0050(6) -0.0037(8) P1 0.0097(2) 0.0098(2) 0.0101(2) 0.00260(19) 0.00169(18) 0.00405(19) P2 0.0095(2) 0.0095(2) 0.0098(2) 0.00232(19) 0.00216(18) 0.00393(19) Cl1 0.0195(2) 0.0106(2) 0.0178(2) 0.00521(19) 0.00620(19) 0.00567(19) Cl2 0.0126(2) 0.0161(2) 0.0196(2) 0.0073(2) 0.00658(19) 0.00436(19) Pd1 0.00950(8) 0.00847(8) 0.00914(8) 0.00227(6) 0.00195(6) 0.00286(6) C41 0.0401(18) 0.0351(17) 0.102(3) 0.0380(19) -0.0031(18) 0.0063(14) O41 0.0450(11) 0.0285(10) 0.0427(11) 0.0139(9) -0.0049(9) 0.0198(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.394(3) . ? C1 C6 1.397(3) . ? C1 P1 1.818(2) . ? C2 H2 0.9500 . ? C2 C3 1.393(3) . ? C3 H3 0.9500 . ? C3 C4 1.376(4) . ? C4 H4 0.9500 . ? C4 C5 1.380(4) . ? C5 H5 0.9500 . ? C5 C6 1.390(3) . ? C6 H6 0.9500 . ? C7 C8 1.399(3) . ? C7 C12 1.395(3) . ? C7 P1 1.815(2) . ? C8 H8 0.9500 . ? C8 C9 1.389(3) . ? C9 H9 0.9500 . ? C9 C10 1.385(3) . ? C10 H10 0.9500 . ? C10 C11 1.392(3) . ? C11 H11 0.9500 . ? C11 C12 1.390(3) . ? C12 H12 0.9500 . ? C13 C14 1.404(3) . ? C13 C18 1.395(3) . ? C13 P2 1.809(2) . ? C14 H14 0.9500 . ? C14 C15 1.390(3) . ? C15 H15 0.9500 . ? C15 C16 1.388(3) . ? C16 H16 0.9500 . ? C16 C17 1.379(3) . ? C17 H17 0.9500 . ? C17 C18 1.392(3) . ? C18 H18 0.9500 . ? C19 C20 1.394(3) . ? C19 C24 1.394(3) . ? C19 P2 1.812(2) . ? C20 H20 0.9500 . ? C20 C21 1.394(3) . ? C21 H21 0.9500 . ? C21 C22 1.386(3) . ? C22 H22 0.9500 . ? C22 C23 1.383(3) . ? C23 H23 0.9500 . ? C23 C24 1.383(3) . ? C24 H24 0.9500 . ? C25 C26 1.409(3) . ? C25 C30 1.408(3) . ? C25 N1 1.446(2) . ? C26 C27 1.392(3) . ? C26 O1 1.360(2) . ? C27 H27 0.9500 . ? C27 C28 1.384(3) . ? C28 H28 0.9500 . ? C28 C29 1.384(3) . ? C29 H29 0.9500 . ? C29 C30 1.405(3) . ? C30 C31 1.495(3) . ? C31 O2 1.209(2) . ? C31 O3 1.336(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 N1 1.463(2) . ? C32 P1 1.8403(19) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 N1 1.467(2) . ? C33 P2 1.8427(19) . ? O1 H1 0.8400 . ? O3 H3A 0.8400 . ? P1 Pd1 2.2529(5) . ? P2 Pd1 2.2508(5) . ? Cl1 Pd1 2.3605(5) . ? Cl2 Pd1 2.3618(5) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C41 O41 1.394(4) . ? O41 H41 0.8400 . ? 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 C2 C1 C6 119.22(19) . . ? C2 C1 P1 122.49(16) . . ? C6 C1 P1 118.23(16) . . ? C1 C2 H2 120.1 . . ? C1 C2 C3 119.8(2) . . ? H2 C2 C3 120.1 . . ? C2 C3 H3 119.7 . . ? C2 C3 C4 120.6(2) . . ? H3 C3 C4 119.7 . . ? C3 C4 H4 120.0 . . ? C3 C4 C5 120.1(2) . . ? H4 C4 C5 120.0 . . ? C4 C5 H5 119.9 . . ? C4 C5 C6 120.2(2) . . ? H5 C5 C6 119.9 . . ? C1 C6 C5 120.1(2) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 C12 119.83(18) . . ? C8 C7 P1 120.11(15) . . ? C12 C7 P1 120.01(15) . . ? C7 C8 H8 120.1 . . ? C7 C8 C9 119.8(2) . . ? H8 C8 C9 120.1 . . ? C8 C9 H9 119.9 . . ? C8 C9 C10 120.3(2) . . ? H9 C9 C10 119.9 . . ? C9 C10 H10 119.9 . . ? C9 C10 C11 120.2(2) . . ? H10 C10 C11 119.9 . . ? C10 C11 H11 120.0 . . ? C10 C11 C12 120.0(2) . . ? H11 C11 C12 120.0 . . ? C7 C12 C11 119.9(2) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C18 119.44(18) . . ? C14 C13 P2 120.22(15) . . ? C18 C13 P2 120.31(15) . . ? C13 C14 H14 120.2 . . ? C13 C14 C15 119.6(2) . . ? H14 C14 C15 120.2 . . ? C14 C15 H15 119.8 . . ? C14 C15 C16 120.4(2) . . ? H15 C15 C16 119.8 . . ? C15 C16 H16 119.9 . . ? C15 C16 C17 120.29(19) . . ? H16 C16 C17 119.9 . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.1(2) . . ? H17 C17 C18 120.0 . . ? C13 C18 C17 120.2(2) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C20 C19 C24 119.41(19) . . ? C20 C19 P2 123.25(16) . . ? C24 C19 P2 117.23(15) . . ? C19 C20 H20 120.0 . . ? C19 C20 C21 119.9(2) . . ? H20 C20 C21 120.0 . . ? C20 C21 H21 119.9 . . ? C20 C21 C22 120.1(2) . . ? H21 C21 C22 119.9 . . ? C21 C22 H22 120.0 . . ? C21 C22 C23 119.9(2) . . ? H22 C22 C23 120.0 . . ? C22 C23 H23 119.8 . . ? C22 C23 C24 120.4(2) . . ? H23 C23 C24 119.8 . . ? C19 C24 C23 120.2(2) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C30 118.67(18) . . ? C26 C25 N1 114.33(17) . . ? C30 C25 N1 126.99(18) . . ? C25 C26 C27 121.27(19) . . ? C25 C26 O1 120.98(18) . . ? C27 C26 O1 117.76(18) . . ? C26 C27 H27 120.3 . . ? C26 C27 C28 119.42(19) . . ? H27 C27 C28 120.3 . . ? C27 C28 H28 119.7 . . ? C27 C28 C29 120.6(2) . . ? H28 C28 C29 119.7 . . ? C28 C29 H29 119.6 . . ? C28 C29 C30 120.8(2) . . ? H29 C29 C30 119.6 . . ? C25 C30 C29 119.29(19) . . ? C25 C30 C31 122.56(18) . . ? C29 C30 C31 118.15(18) . . ? C30 C31 O2 125.62(18) . . ? C30 C31 O3 112.01(17) . . ? O2 C31 O3 122.36(19) . . ? H32A C32 H32B 107.7 . . ? H32A C32 N1 108.8 . . ? H32A C32 P1 108.8 . . ? H32B C32 N1 108.8 . . ? H32B C32 P1 108.8 . . ? N1 C32 P1 113.64(13) . . ? H33A C33 H33B 107.9 . . ? H33A C33 N1 109.2 . . ? H33A C33 P2 109.2 . . ? H33B C33 N1 109.2 . . ? H33B C33 P2 109.2 . . ? N1 C33 P2 111.87(13) . . ? C25 N1 C32 116.05(15) . . ? C25 N1 C33 115.32(15) . . ? C32 N1 C33 113.77(15) . . ? C26 O1 H1 109.5 . . ? C31 O3 H3A 109.5 . . ? C1 P1 C7 107.66(9) . . ? C1 P1 C32 106.48(9) . . ? C1 P1 Pd1 110.19(7) . . ? C7 P1 C32 100.24(9) . . ? C7 P1 Pd1 116.54(7) . . ? C32 P1 Pd1 114.83(6) . . ? C13 P2 C19 108.00(9) . . ? C13 P2 C33 105.53(9) . . ? C13 P2 Pd1 111.31(7) . . ? C19 P2 C33 99.33(9) . . ? C19 P2 Pd1 115.08(7) . . ? C33 P2 Pd1 116.50(7) . . ? P1 Pd1 P2 91.586(18) . . ? P1 Pd1 Cl1 91.507(18) . . ? P1 Pd1 Cl2 175.974(18) . . ? P2 Pd1 Cl1 175.772(18) . . ? P2 Pd1 Cl2 87.378(18) . . ? Cl1 Pd1 Cl2 89.339(18) . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41A C41 O41 109.5 . . ? H41B C41 H41C 109.5 . . ? H41B C41 O41 109.5 . . ? H41C C41 O41 109.5 . . ? C41 O41 H41 109.5 . . ? 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 H1 N1 0.84 2.23 2.709(2) 116.6 . O3 H3A Cl2 0.84 2.35 3.1479(17) 158.3 2_777 O41 H41 Cl1 0.84 2.41 3.2518(18) 174.7 . _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.472 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.116 # End of data for 2a.MeOH data_2b.0.5Et2O _database_code_depnum_ccdc_archive 'CCDC 626744' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C107 H107 Cl6 N3 O11 P6 Pd3' _chemical_formula_sum 'C107 H107 Cl6 N3 O11 P6 Pd3' _chemical_formula_weight 2328.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 28.5307(4) _cell_length_b 31.9677(6) _cell_length_c 12.6120(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11502.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4752 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9295 _exptl_absorpt_correction_T_max 0.9709 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26761 _diffrn_reflns_av_R_equivalents 0.0610 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 25.03 _reflns_number_total 10137 _reflns_number_gt 6799 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10137 _refine_ls_number_parameters 633 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1114 _refine_ls_wR_factor_gt 0.1022 _refine_ls_goodness_of_fit_ref 0.980 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 0.005 _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 0.199316(10) 1.037946(10) 0.50614(2) 0.01954(10) Uani 1 1 d . . . Cl1 Cl 0.20490(4) 0.99997(3) 0.66472(8) 0.0275(3) Uani 1 1 d . . . Cl2 Cl 0.21766(4) 1.10003(3) 0.59594(9) 0.0313(3) Uani 1 1 d . . . P1 P 0.17740(4) 0.97834(3) 0.42574(8) 0.0192(2) Uani 1 1 d . . . P2 P 0.19138(4) 1.07731(3) 0.36170(9) 0.0215(3) Uani 1 1 d . . . N1 N 0.15191(10) 1.01624(10) 0.2350(3) 0.0183(7) Uani 1 1 d . . . O1 O 0.08668(9) 0.98235(9) -0.1762(2) 0.0246(7) Uani 1 1 d . . . H1 H 0.0574 0.9794 -0.1770 0.037 Uiso 1 1 calc R . . O2 O 0.00857(9) 0.99926(10) 0.1776(2) 0.0321(8) Uani 1 1 d . . . O3 O 0.06315(9) 1.02099(9) 0.2889(2) 0.0263(7) Uani 1 1 d . . . H3 H 0.0922 1.0250 0.2887 0.039 Uiso 1 1 calc R . . C1 C 0.17277(14) 0.97738(13) 0.2793(3) 0.0218(9) Uani 1 1 d . . . H1A H 0.2044 0.9734 0.2487 0.026 Uiso 1 1 calc R . . H1B H 0.1533 0.9532 0.2578 0.026 Uiso 1 1 calc R . . C2 C 0.18718(14) 1.05065(13) 0.2334(3) 0.0244(10) Uani 1 1 d . . . H2A H 0.1784 1.0712 0.1782 0.029 Uiso 1 1 calc R . . H2B H 0.2182 1.0390 0.2145 0.029 Uiso 1 1 calc R . . C3 C 0.13443(13) 1.00751(12) 0.1276(3) 0.0181(9) Uani 1 1 d . . . C4 C 0.16462(14) 1.00479(13) 0.0423(3) 0.0238(10) Uani 1 1 d . . . H4 H 0.1973 1.0082 0.0537 0.029 Uiso 1 1 calc R . . C5 C 0.14857(14) 0.99733(13) -0.0586(3) 0.0247(10) Uani 1 1 d . . . H5 H 0.1698 0.9971 -0.1167 0.030 Uiso 1 1 calc R . . C6 C 0.10115(15) 0.99018(12) -0.0752(3) 0.0226(10) Uani 1 1 d . . . C7 C 0.07050(14) 0.99180(13) 0.0092(3) 0.0228(9) Uani 1 1 d . . . H7 H 0.0381 0.9865 -0.0020 0.027 Uiso 1 1 calc R . . C8 C 0.08664(13) 1.00120(12) 0.1114(3) 0.0184(9) Uani 1 1 d . . . C9 C 0.04989(14) 1.00683(13) 0.1953(3) 0.0216(9) Uani 1 1 d . . . C10 C 0.11965(14) 0.96340(12) 0.4701(3) 0.0200(9) Uani 1 1 d . . . C11 C 0.09932(15) 0.92604(13) 0.4364(4) 0.0297(11) Uani 1 1 d . . . H11 H 0.1162 0.9078 0.3908 0.036 Uiso 1 1 calc R . . C12 C 0.05483(16) 0.91547(14) 0.4693(4) 0.0341(11) Uani 1 1 d . . . H12 H 0.0414 0.8898 0.4468 0.041 Uiso 1 1 calc R . . C13 C 0.02964(16) 0.94178(14) 0.5343(4) 0.0340(12) Uani 1 1 d . . . H13 H -0.0013 0.9345 0.5553 0.041 Uiso 1 1 calc R . . C14 C 0.04917(14) 0.97850(13) 0.5687(3) 0.0265(10) Uani 1 1 d . . . H14 H 0.0319 0.9965 0.6141 0.032 Uiso 1 1 calc R . . C15 C 0.09440(14) 0.98941(13) 0.5372(3) 0.0213(9) Uani 1 1 d . . . H15 H 0.1080 1.0147 0.5618 0.026 Uiso 1 1 calc R . . C20 C 0.21556(15) 0.93379(13) 0.4487(3) 0.0249(10) Uani 1 1 d . . . C21 C 0.25467(14) 0.92629(15) 0.3842(4) 0.0319(11) Uani 1 1 d . . . H21 H 0.2615 0.9446 0.3269 0.038 Uiso 1 1 calc R . . C22 C 0.28288(17) 0.89269(17) 0.4039(4) 0.0456(14) Uani 1 1 d . . . H22 H 0.3093 0.8877 0.3597 0.055 Uiso 1 1 calc R . . C23 C 0.27360(19) 0.86577(16) 0.4873(4) 0.0463(14) Uani 1 1 d . . . H23 H 0.2933 0.8423 0.4993 0.056 Uiso 1 1 calc R . . C24 C 0.23614(17) 0.87301(15) 0.5523(4) 0.0416(13) Uani 1 1 d . . . H24 H 0.2302 0.8550 0.6107 0.050 Uiso 1 1 calc R . . C25 C 0.20676(16) 0.90671(14) 0.5328(3) 0.0337(12) Uani 1 1 d . . . H25 H 0.1804 0.9113 0.5773 0.040 Uiso 1 1 calc R . . C30 C 0.24233(14) 1.11024(13) 0.3412(3) 0.0257(10) Uani 1 1 d . . . C31 C 0.28433(14) 1.09024(13) 0.3202(3) 0.0261(10) Uani 1 1 d . . . H31 H 0.2852 1.0606 0.3145 0.031 Uiso 1 1 calc R . . C32 C 0.32526(16) 1.11315(15) 0.3075(4) 0.0356(12) Uani 1 1 d . . . H32 H 0.3541 1.0994 0.2934 0.043 Uiso 1 1 calc R . . C33 C 0.32348(18) 1.15561(16) 0.3154(4) 0.0486(14) Uani 1 1 d . . . H33 H 0.3511 1.1716 0.3047 0.058 Uiso 1 1 calc R . . C34 C 0.28180(19) 1.17553(16) 0.3390(5) 0.0542(16) Uani 1 1 d . . . H34 H 0.2812 1.2051 0.3466 0.065 Uiso 1 1 calc R . . C35 C 0.24125(17) 1.15309(14) 0.3514(4) 0.0388(12) Uani 1 1 d . . . H35 H 0.2126 1.1670 0.3670 0.047 Uiso 1 1 calc R . . C40 C 0.13992(15) 1.11004(13) 0.3647(3) 0.0266(10) Uani 1 1 d . . . C41 C 0.12912(18) 1.13497(16) 0.2791(4) 0.0443(13) Uani 1 1 d . . . H41 H 0.1491 1.1352 0.2189 0.053 Uiso 1 1 calc R . . C42 C 0.0895(2) 1.15956(18) 0.2802(4) 0.0562(16) Uani 1 1 d . . . H42 H 0.0821 1.1764 0.2205 0.067 Uiso 1 1 calc R . . C43 C 0.06087(18) 1.15982(17) 0.3670(4) 0.0472(14) Uani 1 1 d . . . H43 H 0.0340 1.1773 0.3680 0.057 Uiso 1 1 calc R . . C44 C 0.07093(16) 1.13458(15) 0.4535(4) 0.0371(12) Uani 1 1 d . . . H44 H 0.0507 1.1342 0.5133 0.045 Uiso 1 1 calc R . . C45 C 0.11053(15) 1.11014(13) 0.4515(4) 0.0295(11) Uani 1 1 d . . . H45 H 0.1178 1.0930 0.5108 0.035 Uiso 1 1 calc R . . Pd2 Pd -0.023347(17) 1.2500 0.66380(4) 0.03040(14) Uani 1 2 d S . . Cl3 Cl -0.03105(5) 1.19796(4) 0.53448(10) 0.0439(3) Uani 1 1 d . . . P3 P -0.01869(4) 1.19742(3) 0.78200(10) 0.0308(3) Uani 1 1 d . . . N2 N -0.0216(2) 1.2500 0.9505(4) 0.0382(14) Uani 1 2 d S . . O4 O 0.0646(3) 1.2500 1.0768(7) 0.099(2) Uani 1 2 d S . . H4A H 0.0477 1.2500 1.0223 0.119 Uiso 1 2 calc SR . . O5 O 0.0589(3) 1.2500 1.2513(7) 0.124(3) Uani 1 2 d S . . O6 O -0.1007(3) 1.2500 1.3582(6) 0.124(3) Uani 1 2 d S . . H6 H -0.0808 1.2500 1.4072 0.186 Uiso 1 2 calc SR . . C48 C -0.0872(3) 1.2500 1.0725(7) 0.055(2) Uani 1 2 d S . . H48 H -0.1074 1.2500 1.0126 0.066 Uiso 1 2 calc SR . . C49 C -0.1061(3) 1.2500 1.1776(7) 0.049(2) Uani 1 2 d S . . H49 H -0.1392 1.2500 1.1872 0.059 Uiso 1 2 calc SR . . C50 C -0.0782(4) 1.2500 1.2618(7) 0.059(2) Uani 1 2 d S . . C51 C -0.0321(4) 1.2500 1.2521(7) 0.068(3) Uani 1 2 d S . . H51 H -0.0130 1.2500 1.3137 0.082 Uiso 1 2 calc SR . . C52 C -0.0111(3) 1.2500 1.1503(7) 0.050(2) Uani 1 2 d S . . C53 C 0.0385(5) 1.2500 1.1597(10) 0.088(4) Uani 1 2 d S . . C60 C -0.07402(16) 1.17106(13) 0.8050(4) 0.0354(12) Uani 1 1 d . . . C61 C -0.11207(17) 1.17817(15) 0.7380(5) 0.0500(15) Uani 1 1 d . . . H61 H -0.1090 1.1967 0.6795 0.060 Uiso 1 1 calc R . . C62 C -0.15468(18) 1.15806(18) 0.7567(6) 0.0629(18) Uani 1 1 d . . . H62 H -0.1807 1.1627 0.7111 0.075 Uiso 1 1 calc R . . C63 C -0.1586(2) 1.13096(18) 0.8434(6) 0.069(2) Uani 1 1 d . . . H63 H -0.1879 1.1183 0.8583 0.083 Uiso 1 1 calc R . . C64 C -0.1216(2) 1.12246(17) 0.9065(5) 0.0535(15) Uani 1 1 d . . . H64 H -0.1244 1.1027 0.9624 0.064 Uiso 1 1 calc R . . C65 C -0.07876(18) 1.14296(15) 0.8887(4) 0.0475(14) Uani 1 1 d . . . H65 H -0.0529 1.1376 0.9340 0.057 Uiso 1 1 calc R . . C74 C 0.05346(17) 1.08739(13) 0.7415(3) 0.0357(12) Uani 1 1 d . . . H74 H 0.0474 1.0582 0.7457 0.043 Uiso 1 1 calc R . . C46 C 0.00179(16) 1.21213(13) 0.9145(4) 0.0337(11) Uani 1 1 d . . . H46A H -0.0047 1.1891 0.9648 0.040 Uiso 1 1 calc R . . H46B H 0.0361 1.2168 0.9127 0.040 Uiso 1 1 calc R . . C47 C -0.0391(3) 1.2500 1.0590(6) 0.0396(18) Uani 1 2 d S . . C70 C 0.02512(15) 1.15792(13) 0.7496(4) 0.0289(10) Uani 1 1 d . . . C71 C 0.07029(15) 1.17211(14) 0.7270(4) 0.0354(12) Uani 1 1 d . . . H71 H 0.0761 1.2012 0.7202 0.042 Uiso 1 1 calc R . . C72 C 0.10682(17) 1.14376(15) 0.7144(4) 0.0358(12) Uani 1 1 d . . . H72 H 0.1377 1.1535 0.7004 0.043 Uiso 1 1 calc R . . C73 C 0.09788(17) 1.10102(14) 0.7224(3) 0.0341(12) Uani 1 1 d . . . H73 H 0.1227 1.0815 0.7146 0.041 Uiso 1 1 calc R . . C75 C 0.01703(16) 1.11539(13) 0.7549(4) 0.0315(11) Uani 1 1 d . . . H75 H -0.0138 1.1053 0.7679 0.038 Uiso 1 1 calc R . . C100 C -0.0480(2) 1.1393(2) 0.2062(7) 0.097(3) Uani 1 1 d . . . H10A H -0.0296 1.1616 0.2396 0.146 Uiso 1 1 calc R . . H10B H -0.0660 1.1244 0.2606 0.146 Uiso 1 1 calc R . . H10C H -0.0695 1.1515 0.1542 0.146 Uiso 1 1 calc R . . C101 C -0.0176(3) 1.1111(2) 0.1550(6) 0.087(2) Uani 1 1 d . . . H10D H 0.0001 1.0950 0.2090 0.105 Uiso 1 1 calc R . . H10E H -0.0363 1.0910 0.1129 0.105 Uiso 1 1 calc R . . C102 C 0.0512(3) 1.10338(18) 0.0573(5) 0.073(2) Uani 1 1 d . . . H10F H 0.0644 1.0896 0.1209 0.088 Uiso 1 1 calc R . . H10G H 0.0384 1.0814 0.0102 0.088 Uiso 1 1 calc R . . C103 C 0.0877(2) 1.1258(2) 0.0026(5) 0.0659(18) Uani 1 1 d . . . H10H H 0.0751 1.1380 -0.0627 0.099 Uiso 1 1 calc R . . H10I H 0.1133 1.1066 -0.0149 0.099 Uiso 1 1 calc R . . H10J H 0.0996 1.1482 0.0484 0.099 Uiso 1 1 calc R . . O8 O 0.01391(14) 1.13143(11) 0.0886(3) 0.0575(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 Pd1 0.01446(17) 0.02926(18) 0.01490(18) -0.00317(15) -0.00149(14) -0.00215(14) Cl1 0.0250(6) 0.0413(6) 0.0163(5) 0.0011(5) -0.0026(5) -0.0005(5) Cl2 0.0291(6) 0.0390(6) 0.0259(6) -0.0105(5) -0.0026(5) -0.0064(5) P1 0.0158(5) 0.0264(6) 0.0154(6) -0.0012(5) -0.0011(5) 0.0002(5) P2 0.0171(6) 0.0290(6) 0.0185(6) -0.0026(5) -0.0012(5) -0.0027(5) N1 0.0131(17) 0.0243(18) 0.0173(19) -0.0016(15) -0.0017(15) -0.0037(14) O1 0.0198(15) 0.0402(17) 0.0139(15) -0.0050(13) -0.0032(13) -0.0014(13) O2 0.0146(16) 0.062(2) 0.0194(16) -0.0002(15) 0.0005(13) -0.0066(15) O3 0.0152(15) 0.0448(18) 0.0188(16) -0.0043(14) 0.0004(13) -0.0015(13) C1 0.016(2) 0.032(2) 0.017(2) -0.0019(19) -0.0013(18) 0.0022(18) C2 0.016(2) 0.036(2) 0.022(2) 0.000(2) 0.0006(19) -0.0066(19) C3 0.015(2) 0.022(2) 0.017(2) -0.0014(18) -0.0032(19) -0.0010(17) C4 0.011(2) 0.038(3) 0.023(2) -0.003(2) -0.0022(19) 0.0016(19) C5 0.020(2) 0.035(2) 0.020(2) -0.003(2) 0.003(2) -0.0005(19) C6 0.030(3) 0.024(2) 0.014(2) -0.0016(19) -0.001(2) 0.0008(19) C7 0.017(2) 0.030(2) 0.021(2) 0.000(2) -0.005(2) -0.0014(18) C8 0.013(2) 0.023(2) 0.019(2) 0.0010(18) 0.0025(18) -0.0008(17) C9 0.019(2) 0.030(2) 0.017(2) 0.0057(19) 0.0006(19) 0.0005(18) C10 0.019(2) 0.022(2) 0.019(2) 0.0046(19) -0.0009(18) -0.0032(18) C11 0.028(3) 0.030(2) 0.032(3) -0.007(2) 0.003(2) 0.000(2) C12 0.032(3) 0.028(2) 0.042(3) -0.005(2) -0.002(2) -0.011(2) C13 0.023(3) 0.041(3) 0.038(3) 0.004(2) 0.005(2) -0.008(2) C14 0.019(2) 0.033(2) 0.027(3) -0.004(2) 0.003(2) 0.0022(19) C15 0.021(2) 0.025(2) 0.018(2) -0.0048(18) -0.0036(19) -0.0021(18) C20 0.024(2) 0.031(2) 0.019(2) -0.006(2) -0.003(2) 0.0043(19) C21 0.021(2) 0.050(3) 0.026(3) 0.002(2) -0.001(2) 0.003(2) C22 0.034(3) 0.070(4) 0.033(3) -0.004(3) 0.007(2) 0.023(3) C23 0.049(3) 0.052(3) 0.038(3) 0.008(3) 0.003(3) 0.027(3) C24 0.048(3) 0.039(3) 0.038(3) 0.014(2) 0.007(3) 0.012(2) C25 0.036(3) 0.045(3) 0.020(2) 0.008(2) 0.008(2) 0.014(2) C30 0.025(2) 0.036(3) 0.016(2) -0.002(2) 0.000(2) -0.005(2) C31 0.025(2) 0.030(2) 0.023(2) -0.004(2) -0.002(2) -0.002(2) C32 0.021(2) 0.048(3) 0.038(3) 0.002(2) -0.002(2) -0.008(2) C33 0.032(3) 0.042(3) 0.072(4) 0.003(3) -0.005(3) -0.019(2) C34 0.043(3) 0.030(3) 0.090(5) 0.005(3) -0.007(3) -0.015(3) C35 0.034(3) 0.030(3) 0.052(3) -0.009(2) -0.002(2) 0.001(2) C40 0.024(2) 0.033(2) 0.023(3) -0.004(2) -0.004(2) 0.002(2) C41 0.048(3) 0.061(3) 0.023(3) 0.000(3) 0.007(2) 0.025(3) C42 0.065(4) 0.074(4) 0.030(3) 0.009(3) -0.004(3) 0.038(3) C43 0.038(3) 0.067(4) 0.037(3) -0.009(3) -0.012(3) 0.030(3) C44 0.028(3) 0.045(3) 0.039(3) -0.009(2) 0.001(2) 0.005(2) C45 0.025(3) 0.032(2) 0.031(3) -0.002(2) -0.002(2) -0.002(2) Pd2 0.0273(3) 0.0207(2) 0.0432(3) 0.000 0.0072(2) 0.000 Cl3 0.0526(8) 0.0300(6) 0.0491(8) -0.0080(6) 0.0043(6) 0.0048(6) P3 0.0273(6) 0.0192(6) 0.0460(8) -0.0011(6) 0.0096(6) 0.0011(5) N2 0.050(4) 0.022(3) 0.043(4) 0.000 0.016(3) 0.000 O4 0.097(6) 0.113(6) 0.089(6) 0.000 -0.010(5) 0.000 O5 0.186(9) 0.091(6) 0.095(6) 0.000 -0.045(6) 0.000 O6 0.123(7) 0.175(8) 0.073(5) 0.000 0.038(5) 0.000 C48 0.061(6) 0.022(4) 0.082(7) 0.000 0.006(5) 0.000 C49 0.051(5) 0.032(4) 0.064(6) 0.000 0.019(5) 0.000 C50 0.066(6) 0.058(5) 0.053(6) 0.000 -0.009(5) 0.000 C51 0.107(9) 0.048(5) 0.049(6) 0.000 -0.004(6) 0.000 C52 0.052(5) 0.035(4) 0.063(6) 0.000 0.004(5) 0.000 C53 0.152(13) 0.045(5) 0.068(8) 0.000 0.007(9) 0.000 C60 0.024(3) 0.024(2) 0.058(3) -0.006(2) 0.012(3) 0.000(2) C61 0.032(3) 0.037(3) 0.081(4) -0.004(3) 0.015(3) 0.001(2) C62 0.030(3) 0.053(4) 0.106(5) -0.025(4) 0.009(3) -0.003(3) C63 0.051(4) 0.044(3) 0.113(6) -0.017(4) 0.050(4) -0.015(3) C64 0.046(4) 0.048(3) 0.067(4) -0.006(3) 0.024(3) -0.010(3) C65 0.039(3) 0.040(3) 0.063(4) -0.002(3) 0.022(3) -0.010(2) C74 0.054(3) 0.022(2) 0.030(3) -0.005(2) 0.000(2) 0.008(2) C46 0.038(3) 0.021(2) 0.041(3) -0.001(2) 0.008(2) 0.000(2) C47 0.046(5) 0.013(3) 0.059(5) 0.000 0.014(4) 0.000 C70 0.026(2) 0.030(2) 0.030(3) -0.002(2) 0.002(2) 0.003(2) C71 0.030(3) 0.033(3) 0.044(3) 0.000(2) 0.006(2) 0.000(2) C72 0.032(3) 0.044(3) 0.032(3) 0.002(2) -0.001(2) 0.005(2) C73 0.036(3) 0.039(3) 0.027(3) -0.002(2) 0.005(2) 0.016(2) C75 0.033(3) 0.022(2) 0.040(3) -0.004(2) 0.005(2) 0.001(2) C100 0.033(3) 0.079(5) 0.179(8) -0.023(5) 0.030(5) -0.022(3) C101 0.104(6) 0.064(4) 0.095(6) -0.010(4) 0.010(5) -0.043(4) C102 0.109(6) 0.043(3) 0.068(5) -0.012(3) -0.034(4) 0.026(4) C103 0.068(4) 0.086(5) 0.044(4) 0.001(4) -0.003(3) 0.034(4) O8 0.072(3) 0.051(2) 0.050(2) 0.0030(19) 0.018(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3451(11) . ? Pd1 Cl2 2.3443(11) . ? Pd1 P1 2.2472(11) . ? Pd1 P2 2.2255(11) . ? P1 C1 1.852(4) . ? P1 C10 1.804(4) . ? P1 C20 1.816(4) . ? P2 C2 1.833(4) . ? P2 C30 1.814(4) . ? P2 C40 1.803(4) . ? N1 C1 1.486(5) . ? N1 C2 1.491(5) . ? N1 C3 1.470(5) . ? O1 C6 1.362(4) . ? O2 C9 1.224(5) . ? O3 C9 1.319(5) . ? C3 C4 1.381(5) . ? C3 C8 1.393(5) . ? C4 C5 1.374(6) . ? C5 C6 1.388(6) . ? C6 C7 1.378(6) . ? C7 C8 1.402(5) . ? C8 C9 1.500(5) . ? C10 C11 1.394(6) . ? C10 C15 1.388(5) . ? C11 C12 1.377(6) . ? C12 C13 1.377(6) . ? C13 C14 1.370(6) . ? C14 C15 1.395(6) . ? C20 C21 1.402(6) . ? C20 C25 1.392(6) . ? C21 C22 1.365(6) . ? C22 C23 1.385(7) . ? C23 C24 1.367(7) . ? C24 C25 1.387(6) . ? C30 C31 1.384(6) . ? C30 C35 1.376(6) . ? C31 C32 1.388(6) . ? C32 C33 1.362(7) . ? C33 C34 1.381(7) . ? C34 C35 1.370(7) . ? C40 C41 1.376(6) . ? C40 C45 1.379(6) . ? C41 C42 1.376(7) . ? C42 C43 1.366(7) . ? C43 C44 1.387(7) . ? C44 C45 1.374(6) . ? Pd2 Cl3 2.3400(12) . ? Pd2 Cl3 2.3400(12) 7_585 ? Pd2 P3 2.2506(12) . ? Pd2 P3 2.2507(12) 7_585 ? P3 C60 1.813(5) . ? P3 C46 1.831(5) . ? P3 C70 1.823(4) . ? N2 C46 1.455(5) . ? N2 C46 1.455(5) 7_585 ? N2 C47 1.458(9) . ? O4 C53 1.284(12) . ? O5 C53 1.294(12) . ? O6 C50 1.376(11) . ? C48 C49 1.432(11) . ? C48 C47 1.381(10) . ? C49 C50 1.329(11) . ? C50 C51 1.319(12) . ? C51 C52 1.416(11) . ? C52 C53 1.420(15) . ? C52 C47 1.402(11) . ? C60 C61 1.395(7) . ? C60 C65 1.392(7) . ? C61 C62 1.395(7) . ? C62 C63 1.400(9) . ? C63 C64 1.349(8) . ? C64 C65 1.404(7) . ? C74 C73 1.362(6) . ? C74 C75 1.382(6) . ? C70 C71 1.396(6) . ? C70 C75 1.381(6) . ? C71 C72 1.390(6) . ? C72 C73 1.394(6) . ? C100 C101 1.408(9) . ? C101 O8 1.390(7) . ? C102 C103 1.441(9) . ? C102 O8 1.446(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl2 90.63(4) . . ? Cl1 Pd1 P1 87.98(4) . . ? Cl1 Pd1 P2 176.11(4) . . ? Cl2 Pd1 P1 176.36(4) . . ? Cl2 Pd1 P2 86.53(4) . . ? P1 Pd1 P2 94.69(4) . . ? Pd1 P1 C1 118.95(14) . . ? Pd1 P1 C10 109.80(14) . . ? Pd1 P1 C20 115.22(14) . . ? C1 P1 C10 103.87(18) . . ? C1 P1 C20 100.89(19) . . ? C10 P1 C20 106.88(19) . . ? Pd1 P2 C2 117.80(14) . . ? Pd1 P2 C30 111.32(14) . . ? Pd1 P2 C40 113.20(15) . . ? C2 P2 C30 101.31(18) . . ? C2 P2 C40 103.59(19) . . ? C30 P2 C40 108.6(2) . . ? C1 N1 C2 110.6(3) . . ? C1 N1 C3 108.8(3) . . ? C2 N1 C3 110.9(3) . . ? P1 C1 N1 112.9(3) . . ? P2 C2 N1 112.0(3) . . ? N1 C3 C4 121.2(3) . . ? N1 C3 C8 119.6(3) . . ? C4 C3 C8 119.2(4) . . ? C3 C4 C5 121.7(4) . . ? C4 C5 C6 119.5(4) . . ? O1 C6 C5 117.8(4) . . ? O1 C6 C7 122.5(4) . . ? C5 C6 C7 119.8(4) . . ? C6 C7 C8 120.7(4) . . ? C3 C8 C7 119.1(4) . . ? C3 C8 C9 124.3(4) . . ? C7 C8 C9 116.4(3) . . ? O2 C9 O3 120.5(4) . . ? O2 C9 C8 121.4(4) . . ? O3 C9 C8 118.1(3) . . ? P1 C10 C11 120.8(3) . . ? P1 C10 C15 120.3(3) . . ? C11 C10 C15 118.9(4) . . ? C10 C11 C12 120.1(4) . . ? C11 C12 C13 120.7(4) . . ? C12 C13 C14 120.0(4) . . ? C13 C14 C15 120.0(4) . . ? C10 C15 C14 120.3(4) . . ? P1 C20 C21 121.3(3) . . ? P1 C20 C25 120.1(3) . . ? C21 C20 C25 118.6(4) . . ? C20 C21 C22 119.9(4) . . ? C21 C22 C23 120.9(5) . . ? C22 C23 C24 120.0(4) . . ? C23 C24 C25 119.9(4) . . ? C20 C25 C24 120.6(4) . . ? P2 C30 C31 117.0(3) . . ? P2 C30 C35 123.1(4) . . ? C31 C30 C35 119.8(4) . . ? C30 C31 C32 120.5(4) . . ? C31 C32 C33 119.1(5) . . ? C32 C33 C34 120.5(4) . . ? C33 C34 C35 120.7(5) . . ? C30 C35 C34 119.4(5) . . ? P2 C40 C41 120.1(3) . . ? P2 C40 C45 120.9(3) . . ? C41 C40 C45 119.0(4) . . ? C40 C41 C42 120.4(5) . . ? C41 C42 C43 120.2(5) . . ? C42 C43 C44 120.2(4) . . ? C43 C44 C45 119.1(5) . . ? C40 C45 C44 121.1(4) . . ? Cl3 Pd2 Cl3 90.62(6) . 7_585 ? Cl3 Pd2 P3 86.35(4) . . ? Cl3 Pd2 P3 176.51(5) . 7_585 ? Cl3 Pd2 P3 176.52(5) 7_585 . ? Cl3 Pd2 P3 86.34(4) 7_585 7_585 ? P3 Pd2 P3 96.64(6) . 7_585 ? Pd2 P3 C60 113.69(17) . . ? Pd2 P3 C46 115.55(14) . . ? Pd2 P3 C70 114.16(15) . . ? C60 P3 C46 104.5(2) . . ? C60 P3 C70 108.1(2) . . ? C46 P3 C70 99.4(2) . . ? C46 N2 C46 112.7(5) . 7_585 ? C46 N2 C47 116.8(3) . . ? C46 N2 C47 116.8(3) 7_585 . ? C49 C48 C47 119.3(8) . . ? C48 C49 C50 120.8(8) . . ? O6 C50 C49 115.1(9) . . ? O6 C50 C51 123.2(9) . . ? C49 C50 C51 121.6(9) . . ? C50 C51 C52 120.3(9) . . ? C51 C52 C53 110.2(9) . . ? C51 C52 C47 120.2(8) . . ? C53 C52 C47 129.6(9) . . ? O4 C53 O5 117.8(13) . . ? O4 C53 C52 120.6(11) . . ? O5 C53 C52 121.6(11) . . ? P3 C60 C61 120.3(4) . . ? P3 C60 C65 120.4(4) . . ? C61 C60 C65 119.3(5) . . ? C60 C61 C62 120.0(5) . . ? C61 C62 C63 119.1(6) . . ? C62 C63 C64 121.5(5) . . ? C63 C64 C65 119.5(6) . . ? C60 C65 C64 120.5(6) . . ? C73 C74 C75 120.9(4) . . ? P3 C46 N2 110.7(4) . . ? N2 C47 C48 117.2(7) . . ? N2 C47 C52 125.1(7) . . ? C48 C47 C52 117.7(7) . . ? P3 C70 C71 117.0(3) . . ? P3 C70 C75 123.8(3) . . ? C71 C70 C75 119.0(4) . . ? C70 C71 C72 120.2(4) . . ? C71 C72 C73 119.6(4) . . ? C74 C73 C72 119.8(4) . . ? C74 C75 C70 120.4(4) . . ? C100 C101 O8 112.0(6) . . ? C103 C102 O8 110.7(5) . . ? C101 O8 C102 110.5(5) . . ? 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 O3 H3 N1 0.84 1.85 2.626(4) 152.3 . O1 H1 O2 0.84 2.00 2.781(4) 153.6 5_575 O4 H4A N2 0.84 2.17 2.928(9) 149.7 . O6 H6 Cl3 0.84 2.71 3.415(8) 142.2 7_586 O6 H6 Cl3 0.84 2.71 3.415(8) 142.2 1_556 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 1.071 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.093 # End of data for 2b.0.5Et2O data_2c.MeOH _database_code_depnum_ccdc_archive 'CCDC 223301' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Cl2 N O4 P2 Pd' _chemical_formula_weight 758.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4716(3) _cell_length_b 16.8605(4) _cell_length_c 16.8411(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.148(1) _cell_angle_gamma 90.00 _cell_volume 3365.14(14) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.844 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7027 _exptl_absorpt_correction_T_max 0.9204 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18916 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6578 _reflns_number_gt 5193 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0698P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6578 _refine_ls_number_parameters 430 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1139 _refine_ls_wR_factor_gt 0.1067 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.258152(15) 0.253940(10) 0.039163(12) 0.01489(10) Uani 1 1 d . . . P1 P 0.27832(6) 0.15160(4) 0.12767(4) 0.01725(16) Uani 1 1 d . . . P2 P 0.30157(6) 0.34729(4) 0.13834(4) 0.01755(16) Uani 1 1 d . . . Cl1 Cl 0.22012(6) 0.15950(4) -0.06963(4) 0.02465(17) Uani 1 1 d . . . Cl2 Cl 0.23330(5) 0.35807(4) -0.05774(4) 0.02438(17) Uani 1 1 d . . . N1 N 0.40913(18) 0.23900(11) 0.25816(14) 0.0172(5) Uani 1 1 d . . . O1 O 0.7648(2) 0.22797(16) 0.55844(14) 0.0467(6) Uani 1 1 d . . . H1 H 0.8269 0.2228 0.5493 0.071(14) Uiso 1 1 calc R . . O2 O 0.89895(17) 0.21915(17) 0.46657(15) 0.0525(6) Uani 1 1 d . . . O3 O 0.82380(19) 0.22539(18) 0.32807(15) 0.0560(7) Uani 1 1 d . . . H3 H 0.8921 0.2263 0.3305 0.085(15) Uiso 1 1 calc R . . C1 C 0.3318(2) 0.17150(15) 0.24133(16) 0.0210(6) Uani 1 1 d . . . H1A H 0.2677 0.1830 0.2624 0.006(6) Uiso 1 1 calc R . . H1B H 0.3715 0.1240 0.2709 0.024(7) Uiso 1 1 calc R . . C2 C 0.3460(2) 0.31368(14) 0.24819(16) 0.0191(6) Uani 1 1 d . . . H2A H 0.3939 0.3549 0.2841 0.037(8) Uiso 1 1 calc R . . H2B H 0.2786 0.3062 0.2665 0.011(6) Uiso 1 1 calc R . . C3 C 0.4990(2) 0.23407(15) 0.33630(18) 0.0196(6) Uani 1 1 d . . . C4 C 0.4801(2) 0.23894(15) 0.41360(19) 0.0238(6) Uani 1 1 d . . . H4 H 0.4053 0.2444 0.4160 0.014(7) Uiso 1 1 calc R . . C5 C 0.5700(3) 0.23585(16) 0.48697(19) 0.0297(7) Uani 1 1 d . . . H5 H 0.5563 0.2384 0.5393 0.045(10) Uiso 1 1 calc R . . C6 C 0.6799(2) 0.22904(18) 0.48458(18) 0.0299(7) Uani 1 1 d . . . C7 C 0.7000(2) 0.22458(18) 0.40765(18) 0.0287(6) Uani 1 1 d . . . C8 C 0.6082(2) 0.22641(16) 0.33432(18) 0.0253(6) Uani 1 1 d . . . H8 H 0.6214 0.2223 0.2819 0.022(7) Uiso 1 1 calc R . . C9 C 0.8162(2) 0.2227(2) 0.4036(2) 0.0396(8) Uani 1 1 d . . . C10 C 0.1472(2) 0.09954(16) 0.11522(17) 0.0264(6) Uani 1 1 d . . . C11 C 0.1433(3) 0.03534(18) 0.16622(19) 0.0368(8) Uani 1 1 d . . . H11 H 0.2106 0.0174 0.2066 0.039(9) Uiso 1 1 calc R . . C12 C 0.0416(3) -0.0028(2) 0.1585(2) 0.0483(9) Uani 1 1 d . . . H12 H 0.0396 -0.0473 0.1926 0.041(9) Uiso 1 1 calc R . . C13 C -0.0572(3) 0.0246(2) 0.1004(2) 0.0494(9) Uani 1 1 d . . . H13 H -0.1269 -0.0011 0.0949 0.095(14) Uiso 1 1 calc R . . C14 C -0.0539(3) 0.08822(19) 0.0516(2) 0.0420(8) Uani 1 1 d . . . H14 H -0.1219 0.1072 0.0129 0.083(13) Uiso 1 1 calc R . . C15 C 0.0476(2) 0.12586(17) 0.05755(18) 0.0297(7) Uani 1 1 d . . . H15 H 0.0488 0.1695 0.0222 0.038(8) Uiso 1 1 calc R . . C20 C 0.3818(2) 0.08191(15) 0.11400(16) 0.0241(6) Uani 1 1 d . . . C21 C 0.4911(2) 0.10984(18) 0.12682(18) 0.0327(7) Uani 1 1 d . . . H21 H 0.5082 0.1641 0.1400 0.053(10) Uiso 1 1 calc R . . C22 C 0.5744(3) 0.0588(2) 0.12036(19) 0.0444(9) Uani 1 1 d . . . H22 H 0.6487 0.0781 0.1290 0.056(11) Uiso 1 1 calc R . . C23 C 0.5508(3) -0.0198(2) 0.1015(2) 0.0488(10) Uani 1 1 d . . . H23 H 0.6085 -0.0546 0.0970 0.056(10) Uiso 1 1 calc R . . C24 C 0.4433(3) -0.0480(2) 0.0891(2) 0.0471(9) Uani 1 1 d . . . H24 H 0.4271 -0.1025 0.0765 0.080(13) Uiso 1 1 calc R . . C25 C 0.3588(3) 0.00249(16) 0.09500(19) 0.0349(7) Uani 1 1 d . . . H25 H 0.2847 -0.0173 0.0860 0.044(9) Uiso 1 1 calc R . . C30 C 0.4226(2) 0.40461(15) 0.13326(17) 0.0239(6) Uani 1 1 d . . . C32 C 0.6246(3) 0.41093(19) 0.1614(2) 0.0409(8) Uani 1 1 d . . . H32 H 0.6971 0.3873 0.1831 0.063(11) Uiso 1 1 calc R . . C31 C 0.5292(2) 0.37052(17) 0.16461(19) 0.0315(7) Uani 1 1 d . . . H31 H 0.5366 0.3190 0.1885 0.062(11) Uiso 1 1 calc R . . C33 C 0.6137(3) 0.4853(2) 0.1265(2) 0.0469(9) Uani 1 1 d . . . H33 H 0.6785 0.5131 0.1234 0.066(11) Uiso 1 1 calc R . . C34 C 0.5085(3) 0.51967(19) 0.0959(2) 0.0468(10) Uani 1 1 d . . . H34 H 0.5017 0.5714 0.0724 0.053(10) Uiso 1 1 calc R . . C35 C 0.4134(3) 0.48031(17) 0.09896(18) 0.0358(7) Uani 1 1 d . . . H35 H 0.3415 0.5048 0.0777 0.031(8) Uiso 1 1 calc R . . C40 C 0.1899(2) 0.41564(16) 0.13601(17) 0.0266(6) Uani 1 1 d . . . C41 C 0.2105(3) 0.47901(18) 0.1911(2) 0.0415(8) Uani 1 1 d . . . H41 H 0.2850 0.4889 0.2266 0.060(11) Uiso 1 1 calc R . . C42 C 0.1233(3) 0.5279(2) 0.1948(2) 0.0560(10) Uani 1 1 d . . . H42 H 0.1378 0.5711 0.2330 0.064(11) Uiso 1 1 calc R . . C43 C 0.0159(3) 0.5141(2) 0.1434(2) 0.0537(10) Uani 1 1 d . . . H43 H -0.0436 0.5485 0.1454 0.070(11) Uiso 1 1 calc R . . C44 C -0.0066(3) 0.4512(2) 0.0890(2) 0.0470(9) Uani 1 1 d . . . H44 H -0.0818 0.4413 0.0548 0.073(13) Uiso 1 1 calc R . . C45 C 0.0804(2) 0.40191(18) 0.08390(19) 0.0328(7) Uani 1 1 d . . . H45 H 0.0653 0.3592 0.0452 0.038(9) Uiso 1 1 calc R . . C1S C 1.0156(4) 0.2669(3) 0.2376(3) 0.0661(13) Uani 1 1 d . . . H1S1 H 1.0455 0.3196 0.2573 0.099 Uiso 1 1 calc R . . H1S2 H 0.9383 0.2721 0.1997 0.099 Uiso 1 1 calc R . . H1S3 H 1.0630 0.2422 0.2078 0.099 Uiso 1 1 calc R . . O1S O 1.0155(2) 0.2220(2) 0.30251(17) 0.0736(9) Uani 1 1 d . . . H1S H 1.0723 0.2330 0.3434 0.088 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 0.01088(14) 0.01686(14) 0.01448(15) 0.00115(7) 0.00041(10) -0.00037(6) P1 0.0164(3) 0.0158(3) 0.0169(3) 0.0010(3) 0.0012(3) -0.0028(3) P2 0.0165(3) 0.0160(3) 0.0174(3) 0.0006(3) 0.0014(3) 0.0024(3) Cl1 0.0260(4) 0.0260(4) 0.0198(4) -0.0053(3) 0.0040(3) -0.0050(3) Cl2 0.0229(4) 0.0244(3) 0.0236(3) 0.0087(3) 0.0039(3) 0.0036(3) N1 0.0119(11) 0.0191(10) 0.0162(12) 0.0014(9) -0.0018(9) -0.0017(8) O1 0.0313(14) 0.0728(16) 0.0225(11) 0.0045(12) -0.0114(10) -0.0037(12) O2 0.0186(12) 0.0810(17) 0.0442(14) 0.0016(14) -0.0102(11) -0.0005(12) O3 0.0151(13) 0.110(2) 0.0400(15) 0.0028(15) 0.0040(10) 0.0000(13) C1 0.0189(13) 0.0216(13) 0.0195(13) 0.0030(11) 0.0018(11) -0.0035(10) C2 0.0148(13) 0.0180(13) 0.0209(13) -0.0010(11) 0.0001(11) 0.0007(10) C3 0.0157(14) 0.0199(12) 0.0198(15) 0.0004(11) 0.0006(11) -0.0019(10) C4 0.0191(15) 0.0285(14) 0.0228(16) 0.0027(12) 0.0050(12) -0.0006(10) C5 0.0350(18) 0.0351(16) 0.0167(15) 0.0023(12) 0.0047(13) -0.0002(13) C6 0.0243(16) 0.0346(15) 0.0212(15) 0.0031(13) -0.0071(12) -0.0025(12) C7 0.0181(14) 0.0346(15) 0.0271(16) 0.0007(14) -0.0020(12) -0.0008(12) C8 0.0189(14) 0.0336(15) 0.0199(14) -0.0001(13) 0.0009(11) 0.0003(12) C9 0.0174(16) 0.057(2) 0.0370(19) 0.0005(17) -0.0029(14) -0.0006(14) C10 0.0257(15) 0.0301(15) 0.0237(15) -0.0052(13) 0.0081(12) -0.0112(12) C11 0.0419(19) 0.0333(16) 0.0328(17) 0.0012(14) 0.0084(15) -0.0156(14) C12 0.061(2) 0.0383(19) 0.052(2) 0.0016(18) 0.027(2) -0.0236(17) C13 0.041(2) 0.055(2) 0.058(2) -0.019(2) 0.0240(19) -0.0271(17) C14 0.0237(17) 0.045(2) 0.057(2) -0.0137(18) 0.0126(16) -0.0115(14) C15 0.0214(15) 0.0346(16) 0.0325(16) -0.0050(14) 0.0078(13) -0.0059(12) C20 0.0273(15) 0.0238(14) 0.0182(14) 0.0040(12) 0.0024(12) 0.0063(11) C21 0.0305(17) 0.0362(17) 0.0315(17) 0.0002(14) 0.0098(13) 0.0062(13) C22 0.0333(19) 0.065(2) 0.0356(18) 0.0093(17) 0.0114(15) 0.0200(17) C23 0.067(3) 0.050(2) 0.0322(19) 0.0166(17) 0.0195(18) 0.0401(19) C24 0.070(3) 0.0333(19) 0.0380(19) 0.0060(16) 0.0171(18) 0.0182(17) C25 0.046(2) 0.0213(14) 0.0351(17) 0.0013(13) 0.0095(15) 0.0034(13) C30 0.0285(15) 0.0173(13) 0.0255(15) -0.0054(12) 0.0076(12) -0.0051(11) C32 0.0302(18) 0.048(2) 0.047(2) -0.0077(17) 0.0154(15) -0.0165(15) C31 0.0273(16) 0.0269(16) 0.0406(18) -0.0018(14) 0.0108(14) -0.0070(12) C33 0.054(2) 0.053(2) 0.0371(19) -0.0123(17) 0.0184(17) -0.0372(18) C34 0.081(3) 0.0282(17) 0.0284(17) -0.0045(15) 0.0127(18) -0.0255(18) C35 0.048(2) 0.0267(15) 0.0284(16) -0.0013(14) 0.0052(15) -0.0110(14) C40 0.0268(15) 0.0273(15) 0.0238(15) 0.0052(13) 0.0050(12) 0.0111(12) C41 0.047(2) 0.0376(18) 0.0320(17) -0.0039(15) 0.0006(16) 0.0189(15) C42 0.070(3) 0.048(2) 0.043(2) -0.0075(18) 0.0086(19) 0.0343(19) C43 0.055(2) 0.061(2) 0.047(2) 0.012(2) 0.0194(19) 0.0410(19) C44 0.0283(18) 0.071(3) 0.0398(19) 0.0126(19) 0.0075(15) 0.0238(17) C45 0.0232(16) 0.0455(18) 0.0291(16) 0.0012(15) 0.0072(13) 0.0067(13) C1S 0.033(2) 0.121(4) 0.038(2) 0.006(2) 0.0014(18) 0.001(2) O1S 0.0204(14) 0.144(3) 0.0487(18) 0.0126(19) -0.0004(12) -0.0091(16) _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 2.2354(7) . ? Pd1 P1 2.2424(7) . ? Pd1 Cl2 2.3510(7) . ? Pd1 Cl1 2.3614(7) . ? P1 C10 1.809(3) . ? P1 C20 1.812(3) . ? P1 C1 1.851(3) . ? P2 C40 1.799(3) . ? P2 C30 1.817(3) . ? P2 C2 1.847(3) . ? N1 C3 1.441(3) . ? N1 C1 1.461(3) . ? N1 C2 1.467(3) . ? O1 C6 1.360(3) . ? O1 H1 0.8400 . ? O2 C9 1.230(3) . ? O3 C9 1.305(4) . ? O3 H3 0.8400 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C8 1.378(4) . ? C3 C4 1.396(4) . ? C4 C5 1.387(4) . ? C4 H4 0.9500 . ? C5 C6 1.388(4) . ? C5 H5 0.9500 . ? C6 C7 1.397(4) . ? C7 C8 1.399(4) . ? C7 C9 1.472(4) . ? C8 H8 0.9500 . ? C10 C15 1.390(4) . ? C10 C11 1.392(4) . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.360(5) . ? C13 H13 0.9500 . ? C14 C15 1.392(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C20 C25 1.386(4) . ? C20 C21 1.394(4) . ? C21 C22 1.379(4) . ? C21 H21 0.9500 . ? C22 C23 1.372(5) . ? C22 H22 0.9500 . ? C23 C24 1.376(5) . ? C23 H23 0.9500 . ? C24 C25 1.382(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C30 C35 1.391(4) . ? C30 C31 1.392(4) . ? C32 C33 1.373(5) . ? C32 C31 1.388(4) . ? C32 H32 0.9500 . ? C31 H31 0.9500 . ? C33 C34 1.379(5) . ? C33 H33 0.9500 . ? C34 C35 1.373(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C40 C41 1.386(4) . ? C40 C45 1.393(4) . ? C41 C42 1.382(4) . ? C41 H41 0.9500 . ? C42 C43 1.369(5) . ? C42 H42 0.9500 . ? C43 C44 1.373(5) . ? C43 H43 0.9500 . ? C44 C45 1.391(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C1S O1S 1.330(5) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? O1S H1S 0.8400 . ? 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 95.41(3) . . ? P2 Pd1 Cl2 86.66(3) . . ? P1 Pd1 Cl2 177.85(2) . . ? P2 Pd1 Cl1 176.30(2) . . ? P1 Pd1 Cl1 87.17(2) . . ? Cl2 Pd1 Cl1 90.79(3) . . ? C10 P1 C20 108.92(13) . . ? C10 P1 C1 103.25(12) . . ? C20 P1 C1 101.97(12) . . ? C10 P1 Pd1 112.71(10) . . ? C20 P1 Pd1 110.57(9) . . ? C1 P1 Pd1 118.53(8) . . ? C40 P2 C30 107.89(13) . . ? C40 P2 C2 101.96(12) . . ? C30 P2 C2 102.47(12) . . ? C40 P2 Pd1 115.41(9) . . ? C30 P2 Pd1 110.54(9) . . ? C2 P2 Pd1 117.36(8) . . ? C3 N1 C1 114.3(2) . . ? C3 N1 C2 113.0(2) . . ? C1 N1 C2 110.4(2) . . ? C6 O1 H1 109.5 . . ? C9 O3 H3 109.5 . . ? N1 C1 P1 110.19(18) . . ? N1 C1 H1A 109.6 . . ? P1 C1 H1A 109.6 . . ? N1 C1 H1B 109.6 . . ? P1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? N1 C2 P2 111.17(18) . . ? N1 C2 H2A 109.4 . . ? P2 C2 H2A 109.4 . . ? N1 C2 H2B 109.4 . . ? P2 C2 H2B 109.4 . . ? H2A C2 H2B 108.0 . . ? C8 C3 C4 118.9(3) . . ? C8 C3 N1 118.5(3) . . ? C4 C3 N1 122.6(2) . . ? C5 C4 C3 120.2(3) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? O1 C6 C5 118.0(3) . . ? O1 C6 C7 122.3(3) . . ? C5 C6 C7 119.7(3) . . ? C6 C7 C8 118.9(3) . . ? C6 C7 C9 120.6(3) . . ? C8 C7 C9 120.4(3) . . ? C3 C8 C7 121.6(3) . . ? C3 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? O2 C9 O3 123.1(3) . . ? O2 C9 C7 122.3(3) . . ? O3 C9 C7 114.6(3) . . ? C15 C10 C11 119.0(3) . . ? C15 C10 P1 120.3(2) . . ? C11 C10 P1 120.6(2) . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C14 C13 C12 120.0(3) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.9(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C10 C15 C14 120.0(3) . . ? C10 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C25 C20 C21 118.9(3) . . ? C25 C20 P1 123.5(2) . . ? C21 C20 P1 117.5(2) . . ? C22 C21 C20 120.1(3) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 119.9(3) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C23 C24 C25 120.3(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? C24 C25 C20 120.3(3) . . ? C24 C25 H25 119.9 . . ? C20 C25 H25 119.9 . . ? C35 C30 C31 118.8(3) . . ? C35 C30 P2 123.1(2) . . ? C31 C30 P2 118.1(2) . . ? C33 C32 C31 119.5(3) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C31 C30 120.8(3) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C32 C33 C34 120.0(3) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 121.0(3) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C30 119.9(3) . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C41 C40 C45 119.4(3) . . ? C41 C40 P2 119.9(2) . . ? C45 C40 P2 120.5(2) . . ? C42 C41 C40 120.4(3) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C43 C42 C41 119.9(3) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.7(3) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C43 C44 C45 120.1(3) . . ? C43 C44 H44 119.9 . . ? C45 C44 H44 119.9 . . ? C44 C45 C40 119.5(3) . . ? C44 C45 H45 120.3 . . ? C40 C45 H45 120.3 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? C1S O1S H1S 109.5 . . ? 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 O3 H3 O1S 0.84 1.75 2.559(4) 162.1 . O1 H1 O2 0.84 1.88 2.613(4) 145.2 . O1S H1S Cl2 0.84 2.66 3.280(3) 131.7 4_666 O1S H1S Cl1 0.84 2.67 3.422(3) 149.2 4_666 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.126 _refine_diff_density_min -1.635 _refine_diff_density_rms 0.112 # End of data for 2c.MeOH data_2d.CHCl3 _database_code_depnum_ccdc_archive 'CCDC 626745' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cl5 N O3 P2 Pd' _chemical_formula_weight 846.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.0640(5) _cell_length_b 24.7367(17) _cell_length_c 15.9091(10) _cell_angle_alpha 90.00 _cell_angle_beta 97.144(2) _cell_angle_gamma 90.00 _cell_volume 3539.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 1.028 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8208 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40756 _diffrn_reflns_av_R_equivalents 0.2408 _diffrn_reflns_av_sigmaI/netI 0.1856 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6006 _reflns_number_gt 3112 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0639P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6006 _refine_ls_number_parameters 417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1674 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1531 _refine_ls_wR_factor_gt 0.1227 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 0.98013(7) 0.28270(3) 0.08582(4) 0.0197(2) Uani 1 1 d . . . Cl1 Cl 0.9845(2) 0.19270(8) 0.13511(13) 0.0268(5) Uani 1 1 d . . . Cl2 Cl 1.0986(2) 0.25770(9) -0.03188(12) 0.0263(5) Uani 1 1 d . . . P2 P 0.9985(2) 0.36844(9) 0.04281(12) 0.0195(5) Uani 1 1 d . . . P1 P 0.8590(2) 0.30265(9) 0.19636(13) 0.0202(5) Uani 1 1 d . . . Cl3 Cl 0.4900(4) 0.38374(18) 0.3323(2) 0.0998(13) Uani 1 1 d . . . Cl5 Cl 0.7294(4) 0.41667(16) 0.4525(3) 0.0998(13) Uani 1 1 d . . . Cl4 Cl 0.4282(4) 0.42735(16) 0.4910(2) 0.0995(13) Uani 1 1 d . . . O3 O 0.7840(7) 0.6163(3) 0.3697(3) 0.0362(16) Uani 1 1 d . . . H3 H 0.7149 0.6392 0.3656 0.054 Uiso 1 1 calc R . . O2 O 0.6674(7) 0.5896(2) 0.2440(4) 0.0376(16) Uani 1 1 d . . . O1 O 0.7415(6) 0.4986(2) 0.1823(3) 0.0298(15) Uani 1 1 d . . . H1 H 0.6838 0.5245 0.1887 0.045 Uiso 1 1 calc R . . N1 N 0.9255(7) 0.4083(3) 0.1936(4) 0.0190(16) Uani 1 1 d . . . C28 C 1.1898(8) 0.3895(3) 0.0401(5) 0.0167(19) Uani 1 1 d . . . C1 C 0.8666(9) 0.5372(3) 0.3117(5) 0.020(2) Uani 1 1 d . . . C13 C 0.4120(10) 0.2146(4) 0.1915(5) 0.030(2) Uani 1 1 d . . . H13 H 0.3188 0.1968 0.1895 0.036 Uiso 1 1 calc R . . C25 C 0.7162(9) 0.4037(4) -0.2115(5) 0.028(2) Uani 1 1 d . . . H25 H 0.6556 0.4111 -0.2633 0.033 Uiso 1 1 calc R . . C10 C 0.6877(9) 0.2657(3) 0.1964(5) 0.023(2) Uani 1 1 d . . . C15 C 0.6647(10) 0.2247(4) 0.2529(5) 0.031(2) Uani 1 1 d . . . H15 H 0.7447 0.2140 0.2938 0.038 Uiso 1 1 calc R . . C3 C 0.9444(9) 0.4520(3) 0.2554(5) 0.022(2) Uani 1 1 d . . . C24 C 0.6871(9) 0.3583(4) -0.1636(5) 0.026(2) Uani 1 1 d . . . H24 H 0.6049 0.3355 -0.1820 0.031 Uiso 1 1 calc R . . C8 C 0.7994(9) 0.3724(3) 0.2050(5) 0.0188(19) Uani 1 1 d . . . H8A H 0.7147 0.3801 0.1611 0.023 Uiso 1 1 calc R . . H8B H 0.7666 0.3786 0.2613 0.023 Uiso 1 1 calc R . . C2 C 0.8501(9) 0.4965(3) 0.2496(5) 0.021(2) Uani 1 1 d . . . C23 C 0.7788(9) 0.3466(4) -0.0892(5) 0.026(2) Uani 1 1 d . . . H23 H 0.7609 0.3151 -0.0578 0.031 Uiso 1 1 calc R . . C22 C 0.8970(9) 0.3806(3) -0.0603(5) 0.021(2) Uani 1 1 d . . . C18 C 1.0101(11) 0.3037(4) 0.4472(5) 0.038(3) Uani 1 1 d . . . H18 H 0.9695 0.3095 0.4987 0.045 Uiso 1 1 calc R . . C32 C 1.4080(10) 0.4349(4) 0.1104(6) 0.033(2) Uani 1 1 d . . . H32 H 1.4595 0.4519 0.1590 0.040 Uiso 1 1 calc R . . C16 C 0.9761(9) 0.2944(3) 0.2957(5) 0.022(2) Uani 1 1 d . . . C21 C 1.1288(9) 0.2879(3) 0.2972(6) 0.031(2) Uani 1 1 d . . . H21 H 1.1701 0.2826 0.2458 0.038 Uiso 1 1 calc R . . C31 C 1.4747(10) 0.4302(4) 0.0361(6) 0.037(3) Uani 1 1 d . . . H31 H 1.5700 0.4456 0.0334 0.045 Uiso 1 1 calc R . . C4 C 1.0541(9) 0.4469(3) 0.3228(5) 0.025(2) Uani 1 1 d . . . H4 H 1.1177 0.4163 0.3271 0.030 Uiso 1 1 calc R . . C6 C 0.9806(9) 0.5313(4) 0.3787(5) 0.027(2) Uani 1 1 d . . . H6 H 0.9953 0.5586 0.4209 0.032 Uiso 1 1 calc R . . C20 C 1.2210(10) 0.2890(4) 0.3739(6) 0.040(3) Uani 1 1 d . . . H20 H 1.3252 0.2841 0.3751 0.048 Uiso 1 1 calc R . . C7 C 0.7637(10) 0.5827(4) 0.3047(6) 0.027(2) Uani 1 1 d . . . C5 C 1.0717(10) 0.4870(4) 0.3847(5) 0.032(2) Uani 1 1 d . . . H5 H 1.1473 0.4835 0.4313 0.038 Uiso 1 1 calc R . . C11 C 0.5657(9) 0.2811(3) 0.1372(5) 0.025(2) Uani 1 1 d . . . H11 H 0.5777 0.3093 0.0982 0.030 Uiso 1 1 calc R . . C27 C 0.9245(9) 0.4260(3) -0.1092(5) 0.024(2) Uani 1 1 d . . . H27 H 1.0065 0.4489 -0.0914 0.029 Uiso 1 1 calc R . . C26 C 0.8324(10) 0.4373(4) -0.1835(5) 0.030(2) Uani 1 1 d . . . H26 H 0.8499 0.4687 -0.2152 0.036 Uiso 1 1 calc R . . C12 C 0.4310(10) 0.2561(4) 0.1349(5) 0.031(2) Uani 1 1 d . . . H12 H 0.3503 0.2671 0.0947 0.038 Uiso 1 1 calc R . . C33 C 1.2680(9) 0.4148(3) 0.1128(5) 0.028(2) Uani 1 1 d . . . H33 H 1.2226 0.4177 0.1633 0.034 Uiso 1 1 calc R . . C29 C 1.2608(10) 0.3832(4) -0.0311(5) 0.029(2) Uani 1 1 d . . . H29 H 1.2117 0.3649 -0.0791 0.035 Uiso 1 1 calc R . . C30 C 1.4034(10) 0.4034(4) -0.0333(6) 0.037(2) Uani 1 1 d . . . H30 H 1.4515 0.3987 -0.0825 0.045 Uiso 1 1 calc R . . C17 C 0.9174(10) 0.3017(3) 0.3712(5) 0.033(2) Uani 1 1 d . . . H17 H 0.8130 0.3054 0.3708 0.040 Uiso 1 1 calc R . . C19 C 1.1609(12) 0.2972(3) 0.4479(6) 0.038(3) Uani 1 1 d . . . H19 H 1.2242 0.2985 0.5002 0.046 Uiso 1 1 calc R . . C9 C 0.9238(9) 0.4227(3) 0.1060(4) 0.020(2) Uani 1 1 d . . . H9A H 0.9836 0.4559 0.1021 0.024 Uiso 1 1 calc R . . H9B H 0.8203 0.4309 0.0816 0.024 Uiso 1 1 calc R . . C34 C 0.5523(11) 0.3887(4) 0.4415(7) 0.056(3) Uani 1 1 d . . . H34 H 0.5578 0.3516 0.4667 0.067 Uiso 1 1 calc R . . C14 C 0.5310(10) 0.1991(4) 0.2516(5) 0.033(2) Uani 1 1 d . . . H14 H 0.5186 0.1711 0.2909 0.040 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 0.0193(4) 0.0210(4) 0.0187(3) 0.0006(3) 0.0022(3) -0.0005(3) Cl1 0.0287(13) 0.0205(13) 0.0304(12) 0.0047(9) 0.0008(9) -0.0019(10) Cl2 0.0254(13) 0.0276(13) 0.0267(12) -0.0002(9) 0.0057(9) 0.0017(10) P2 0.0170(13) 0.0215(14) 0.0200(12) 0.0002(9) 0.0023(9) -0.0009(10) P1 0.0181(13) 0.0211(14) 0.0218(12) 0.0013(9) 0.0034(9) -0.0024(10) Cl3 0.069(2) 0.152(4) 0.079(2) 0.034(2) 0.0139(18) -0.020(2) Cl5 0.059(2) 0.101(3) 0.141(3) -0.057(2) 0.015(2) -0.018(2) Cl4 0.102(3) 0.098(3) 0.108(3) 0.037(2) 0.052(2) 0.047(2) O3 0.036(4) 0.043(5) 0.028(4) -0.013(3) -0.001(3) 0.008(3) O2 0.031(4) 0.046(4) 0.033(4) -0.009(3) -0.008(3) 0.014(3) O1 0.024(4) 0.033(4) 0.029(3) -0.007(3) -0.009(3) 0.007(3) N1 0.016(4) 0.023(4) 0.017(4) 0.001(3) 0.000(3) 0.002(3) C28 0.017(5) 0.013(5) 0.019(5) 0.007(3) -0.003(4) -0.002(4) C1 0.014(5) 0.023(5) 0.025(5) -0.008(4) 0.007(4) 0.003(4) C13 0.025(5) 0.032(6) 0.034(5) -0.004(5) 0.011(4) -0.004(5) C25 0.021(5) 0.043(6) 0.020(5) 0.001(4) 0.005(4) 0.005(5) C10 0.024(5) 0.028(6) 0.017(5) -0.003(4) 0.004(4) -0.005(4) C15 0.028(6) 0.051(7) 0.015(5) 0.004(4) 0.000(4) 0.002(5) C3 0.029(6) 0.020(5) 0.019(5) 0.003(4) 0.011(4) -0.008(4) C24 0.005(5) 0.035(6) 0.037(6) -0.004(4) 0.003(4) -0.003(4) C8 0.017(5) 0.014(5) 0.025(5) 0.001(3) 0.000(4) 0.004(4) C2 0.025(5) 0.020(5) 0.018(5) 0.002(4) 0.007(4) -0.003(4) C23 0.018(5) 0.027(6) 0.032(5) -0.001(4) 0.004(4) 0.006(4) C22 0.017(5) 0.026(5) 0.021(5) 0.003(4) 0.001(4) 0.003(4) C18 0.049(7) 0.043(7) 0.022(5) 0.001(4) 0.008(5) 0.003(5) C32 0.022(6) 0.041(7) 0.036(6) 0.006(4) -0.003(4) -0.010(5) C16 0.026(6) 0.017(5) 0.021(5) -0.004(3) -0.002(4) -0.006(4) C21 0.025(6) 0.021(6) 0.049(6) 0.007(4) 0.007(4) 0.004(5) C31 0.025(6) 0.020(6) 0.063(7) 0.009(5) -0.010(5) -0.002(4) C4 0.026(5) 0.025(5) 0.024(5) 0.001(4) 0.002(4) 0.009(4) C6 0.027(6) 0.031(6) 0.022(5) -0.011(4) 0.003(4) -0.003(5) C20 0.027(6) 0.033(6) 0.053(7) -0.002(5) -0.026(5) -0.001(5) C7 0.021(6) 0.026(6) 0.036(6) 0.002(4) 0.007(4) -0.005(4) C5 0.042(6) 0.036(6) 0.014(5) -0.008(4) -0.008(4) 0.012(5) C11 0.034(6) 0.013(5) 0.028(5) 0.006(4) 0.004(4) -0.001(5) C27 0.017(5) 0.026(6) 0.032(5) 0.002(4) 0.008(4) -0.006(4) C26 0.027(6) 0.021(6) 0.042(6) 0.007(4) 0.002(4) 0.002(4) C12 0.025(6) 0.031(6) 0.035(5) -0.006(4) -0.005(4) -0.003(5) C33 0.020(6) 0.032(6) 0.032(5) 0.001(4) 0.001(4) -0.003(4) C29 0.033(6) 0.034(6) 0.021(5) -0.003(4) 0.001(4) 0.008(5) C30 0.029(6) 0.046(7) 0.040(6) 0.015(5) 0.015(5) 0.005(5) C17 0.029(6) 0.037(6) 0.033(6) 0.013(4) 0.006(4) 0.000(5) C19 0.056(8) 0.028(6) 0.026(6) 0.002(4) -0.012(5) 0.011(5) C9 0.031(5) 0.013(5) 0.017(4) -0.003(3) 0.003(4) -0.009(4) C34 0.045(7) 0.042(7) 0.080(8) 0.005(6) 0.006(6) 0.004(6) C14 0.026(6) 0.048(7) 0.028(5) 0.006(4) 0.013(4) -0.016(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.241(2) . ? Pd1 P2 2.241(2) . ? Pd1 Cl2 2.354(2) . ? Pd1 Cl1 2.359(2) . ? P2 C22 1.804(8) . ? P2 C28 1.817(8) . ? P2 C9 1.855(8) . ? P1 C16 1.802(8) . ? P1 C10 1.802(8) . ? P1 C8 1.818(8) . ? Cl3 C34 1.762(11) . ? Cl5 C34 1.737(11) . ? Cl4 C34 1.738(11) . ? O3 C7 1.323(9) . ? O3 H3 0.8400 . ? O2 C7 1.230(9) . ? O1 C2 1.363(9) . ? O1 H1 0.8400 . ? N1 C9 1.438(9) . ? N1 C3 1.457(10) . ? N1 C8 1.476(9) . ? C28 C29 1.378(10) . ? C28 C33 1.424(10) . ? C1 C6 1.397(11) . ? C1 C2 1.405(10) . ? C1 C7 1.457(11) . ? C13 C12 1.390(12) . ? C13 C14 1.402(12) . ? C13 H13 0.9500 . ? C25 C26 1.374(11) . ? C25 C24 1.400(11) . ? C25 H25 0.9500 . ? C10 C15 1.389(11) . ? C10 C11 1.412(11) . ? C15 C14 1.365(11) . ? C15 H15 0.9500 . ? C3 C4 1.374(11) . ? C3 C2 1.390(11) . ? C24 C23 1.390(10) . ? C24 H24 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C23 C22 1.395(11) . ? C23 H23 0.9500 . ? C22 C27 1.405(11) . ? C18 C19 1.375(12) . ? C18 C17 1.385(12) . ? C18 H18 0.9500 . ? C32 C33 1.367(11) . ? C32 C31 1.399(12) . ? C32 H32 0.9500 . ? C16 C17 1.385(11) . ? C16 C21 1.390(11) . ? C21 C20 1.392(11) . ? C21 H21 0.9500 . ? C31 C30 1.377(12) . ? C31 H31 0.9500 . ? C4 C5 1.391(11) . ? C4 H4 0.9500 . ? C6 C5 1.368(11) . ? C6 H6 0.9500 . ? C20 C19 1.372(12) . ? C20 H20 0.9500 . ? C5 H5 0.9500 . ? C11 C12 1.364(11) . ? C11 H11 0.9500 . ? C27 C26 1.388(11) . ? C27 H27 0.9500 . ? C26 H26 0.9500 . ? C12 H12 0.9500 . ? C33 H33 0.9500 . ? C29 C30 1.390(12) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C17 H17 0.9500 . ? C19 H19 0.9500 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C34 H34 1.0000 . ? C14 H14 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 P1 Pd1 P2 95.36(8) . . ? P1 Pd1 Cl2 176.89(8) . . ? P2 Pd1 Cl2 86.97(8) . . ? P1 Pd1 Cl1 86.37(8) . . ? P2 Pd1 Cl1 174.74(8) . . ? Cl2 Pd1 Cl1 91.49(8) . . ? C22 P2 C28 108.1(4) . . ? C22 P2 C9 101.1(4) . . ? C28 P2 C9 102.7(4) . . ? C22 P2 Pd1 112.8(3) . . ? C28 P2 Pd1 112.7(3) . . ? C9 P2 Pd1 118.3(3) . . ? C16 P1 C10 110.9(4) . . ? C16 P1 C8 100.9(4) . . ? C10 P1 C8 102.5(4) . . ? C16 P1 Pd1 111.8(3) . . ? C10 P1 Pd1 113.2(3) . . ? C8 P1 Pd1 116.6(3) . . ? C7 O3 H3 109.5 . . ? C2 O1 H1 109.5 . . ? C9 N1 C3 117.2(6) . . ? C9 N1 C8 110.7(6) . . ? C3 N1 C8 113.0(6) . . ? C29 C28 C33 118.7(8) . . ? C29 C28 P2 122.1(6) . . ? C33 C28 P2 119.1(6) . . ? C6 C1 C2 117.7(7) . . ? C6 C1 C7 123.0(7) . . ? C2 C1 C7 119.2(7) . . ? C12 C13 C14 119.8(8) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C26 C25 C24 119.8(8) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C15 C10 C11 117.4(8) . . ? C15 C10 P1 124.7(6) . . ? C11 C10 P1 117.8(6) . . ? C14 C15 C10 122.2(8) . . ? C14 C15 H15 118.9 . . ? C10 C15 H15 118.9 . . ? C4 C3 C2 120.2(7) . . ? C4 C3 N1 118.2(7) . . ? C2 C3 N1 121.6(7) . . ? C23 C24 C25 119.9(8) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? N1 C8 P1 108.6(5) . . ? N1 C8 H8A 110.0 . . ? P1 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? P1 C8 H8B 110.0 . . ? H8A C8 H8B 108.3 . . ? O1 C2 C3 117.5(7) . . ? O1 C2 C1 121.9(7) . . ? C3 C2 C1 120.7(7) . . ? C24 C23 C22 120.6(8) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C22 C27 118.8(7) . . ? C23 C22 P2 118.9(6) . . ? C27 C22 P2 122.1(6) . . ? C19 C18 C17 119.9(8) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C33 C32 C31 119.5(8) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C17 C16 C21 119.3(7) . . ? C17 C16 P1 119.8(7) . . ? C21 C16 P1 120.3(6) . . ? C16 C21 C20 120.1(8) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C30 C31 C32 120.5(9) . . ? C30 C31 H31 119.7 . . ? C32 C31 H31 119.7 . . ? C3 C4 C5 119.7(8) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C5 C6 C1 121.3(7) . . ? C5 C6 H6 119.4 . . ? C1 C6 H6 119.4 . . ? C19 C20 C21 119.8(9) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? O2 C7 O3 122.9(8) . . ? O2 C7 C1 123.5(8) . . ? O3 C7 C1 113.6(7) . . ? C6 C5 C4 120.5(8) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C12 C11 C10 121.3(8) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C26 C27 C22 120.2(8) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C25 C26 C27 120.7(8) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C11 C12 C13 120.0(8) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C32 C33 C28 120.5(8) . . ? C32 C33 H33 119.8 . . ? C28 C33 H33 119.8 . . ? C28 C29 C30 120.7(8) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C31 C30 C29 119.9(8) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C16 C17 C18 120.3(9) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C20 C19 C18 120.7(8) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? N1 C9 P2 112.6(5) . . ? N1 C9 H9A 109.1 . . ? P2 C9 H9A 109.1 . . ? N1 C9 H9B 109.1 . . ? P2 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? Cl5 C34 Cl4 112.1(6) . . ? Cl5 C34 Cl3 107.8(6) . . ? Cl4 C34 Cl3 109.8(6) . . ? Cl5 C34 H34 109.0 . . ? Cl4 C34 H34 109.0 . . ? Cl3 C34 H34 109.0 . . ? C15 C14 C13 119.3(8) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? 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 O3 H3 Cl1 0.84 2.24 3.075(6) 172.5 2_655 O1 H1 O2 0.84 1.85 2.577(8) 144.0 . _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 1.016 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.145 # End of data for 2d.CHCl3 data_2e.CHCl3 _database_code_depnum_ccdc_archive 'CCDC 626746' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H30 Cl5 N O3 P2 Pd' _chemical_formula_weight 846.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.657(5) _cell_length_b 9.830(5) _cell_length_c 21.630(5) _cell_angle_alpha 86.346(5) _cell_angle_beta 82.333(5) _cell_angle_gamma 69.590(5) _cell_volume 1906.9(15) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8701 _exptl_absorpt_correction_T_max 0.9628 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14762 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.02 _reflns_number_total 6063 _reflns_number_gt 4229 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0514P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6063 _refine_ls_number_parameters 420 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1106 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.58580(4) 0.08411(4) 0.197381(17) 0.01996(13) Uani 1 1 d . . . Cl1 Cl 0.74788(13) -0.12426(12) 0.14702(6) 0.0283(3) Uani 1 1 d . . . Cl2 Cl 0.38417(13) 0.00187(12) 0.19433(6) 0.0285(3) Uani 1 1 d . . . P1 P 0.78310(13) 0.15248(12) 0.19853(6) 0.0198(3) Uani 1 1 d . . . P2 P 0.43059(13) 0.27148(12) 0.25308(6) 0.0209(3) Uani 1 1 d . . . O1 O 0.5274(4) 0.6857(3) 0.23658(15) 0.0280(8) Uani 1 1 d . . . H1 H 0.4903 0.7760 0.2314 0.042 Uiso 1 1 calc R . . O2 O 0.9394(5) 0.4108(4) 0.4465(2) 0.0644(14) Uani 1 1 d . . . H2 H 1.0063 0.3988 0.4695 0.097 Uiso 1 1 calc R . . O3 O 0.9101(4) 0.6427(4) 0.45741(17) 0.0436(10) Uani 1 1 d . . . N1 N 0.6415(4) 0.3914(4) 0.27622(17) 0.0194(9) Uani 1 1 d . . . C1 C 0.8894(5) 0.1531(5) 0.1242(2) 0.0254(12) Uani 1 1 d . . . C2 C 0.8223(6) 0.1706(5) 0.0692(2) 0.0332(13) Uani 1 1 d . . . H2A H 0.7227 0.1727 0.0714 0.040 Uiso 1 1 calc R . . C3 C 0.8989(7) 0.1849(5) 0.0122(3) 0.0439(15) Uani 1 1 d . . . H3 H 0.8519 0.1981 -0.0247 0.053 Uiso 1 1 calc R . . C4 C 1.0448(8) 0.1797(6) 0.0089(3) 0.0533(18) Uani 1 1 d . . . H4 H 1.0983 0.1883 -0.0304 0.064 Uiso 1 1 calc R . . C5 C 1.1121(7) 0.1626(6) 0.0618(3) 0.0515(17) Uani 1 1 d . . . H5 H 1.2123 0.1591 0.0589 0.062 Uiso 1 1 calc R . . C6 C 1.0364(6) 0.1502(6) 0.1196(3) 0.0384(14) Uani 1 1 d . . . H6 H 1.0841 0.1398 0.1562 0.046 Uiso 1 1 calc R . . C7 C 0.9049(5) 0.0318(5) 0.2512(2) 0.0270(12) Uani 1 1 d . . . C8 C 1.0270(6) -0.0869(5) 0.2289(3) 0.0392(14) Uani 1 1 d . . . H8 H 1.0501 -0.1035 0.1853 0.047 Uiso 1 1 calc R . . C9 C 1.1144(6) -0.1806(6) 0.2703(4) 0.0529(19) Uani 1 1 d . . . H9 H 1.1985 -0.2607 0.2551 0.064 Uiso 1 1 calc R . . C10 C 1.0796(7) -0.1577(7) 0.3333(4) 0.058(2) Uani 1 1 d . . . H10 H 1.1405 -0.2217 0.3615 0.069 Uiso 1 1 calc R . . C11 C 0.9584(7) -0.0439(7) 0.3559(3) 0.0487(16) Uani 1 1 d . . . H11 H 0.9334 -0.0303 0.3996 0.058 Uiso 1 1 calc R . . C12 C 0.8720(6) 0.0520(6) 0.3145(3) 0.0373(14) Uani 1 1 d . . . H12 H 0.7890 0.1325 0.3302 0.045 Uiso 1 1 calc R . . C13 C 0.3807(5) 0.2124(5) 0.3314(2) 0.0284(12) Uani 1 1 d . . . C14 C 0.4508(6) 0.2332(6) 0.3811(3) 0.0452(15) Uani 1 1 d . . . H14 H 0.5189 0.2843 0.3745 0.054 Uiso 1 1 calc R . . C15 C 0.4200(8) 0.1790(8) 0.4392(3) 0.0616(19) Uani 1 1 d . . . H15 H 0.4694 0.1909 0.4725 0.074 Uiso 1 1 calc R . . C16 C 0.3193(8) 0.1080(7) 0.4502(3) 0.0614(19) Uani 1 1 d . . . H16 H 0.2985 0.0718 0.4909 0.074 Uiso 1 1 calc R . . C17 C 0.2498(7) 0.0899(7) 0.4026(3) 0.0518(17) Uani 1 1 d . . . H17 H 0.1787 0.0423 0.4103 0.062 Uiso 1 1 calc R . . C18 C 0.2805(6) 0.1398(6) 0.3429(3) 0.0405(14) Uani 1 1 d . . . H18 H 0.2326 0.1239 0.3098 0.049 Uiso 1 1 calc R . . C19 C 0.2615(5) 0.3661(5) 0.2186(2) 0.0208(11) Uani 1 1 d . . . C20 C 0.1329(5) 0.4523(5) 0.2540(2) 0.0283(12) Uani 1 1 d . . . H20 H 0.1269 0.4515 0.2982 0.034 Uiso 1 1 calc R . . C21 C 0.0141(6) 0.5389(5) 0.2240(3) 0.0343(13) Uani 1 1 d . . . H21 H -0.0737 0.5982 0.2480 0.041 Uiso 1 1 calc R . . C22 C 0.0207(6) 0.5409(5) 0.1603(3) 0.0368(14) Uani 1 1 d . . . H22 H -0.0627 0.6005 0.1407 0.044 Uiso 1 1 calc R . . C23 C 0.1481(6) 0.4568(5) 0.1242(3) 0.0345(13) Uani 1 1 d . . . H23 H 0.1533 0.4594 0.0800 0.041 Uiso 1 1 calc R . . C24 C 0.2684(5) 0.3684(5) 0.1539(2) 0.0287(12) Uani 1 1 d . . . H24 H 0.3559 0.3092 0.1298 0.034 Uiso 1 1 calc R . . C25 C 0.6654(5) 0.5100(5) 0.3054(2) 0.0215(11) Uani 1 1 d . . . C26 C 0.7546(5) 0.4770(5) 0.3535(2) 0.0246(11) Uani 1 1 d . . . H26 H 0.7945 0.3789 0.3673 0.030 Uiso 1 1 calc R . . C27 C 0.7869(5) 0.5818(5) 0.3818(2) 0.0267(12) Uani 1 1 d . . . C28 C 0.7198(5) 0.7285(5) 0.3640(2) 0.0309(12) Uani 1 1 d . . . H28 H 0.7367 0.8023 0.3849 0.037 Uiso 1 1 calc R . . C29 C 0.6303(5) 0.7658(5) 0.3169(2) 0.0256(12) Uani 1 1 d . . . H29 H 0.5847 0.8649 0.3056 0.031 Uiso 1 1 calc R . . C30 C 0.6068(5) 0.6561(5) 0.2856(2) 0.0207(11) Uani 1 1 d . . . C31 C 0.8843(6) 0.5457(6) 0.4315(2) 0.0320(13) Uani 1 1 d . . . C32 C 0.7517(5) 0.3395(5) 0.2221(2) 0.0216(11) Uani 1 1 d . . . H32A H 0.8476 0.3445 0.2312 0.026 Uiso 1 1 calc R . . H32B H 0.7199 0.4061 0.1864 0.026 Uiso 1 1 calc R . . C33 C 0.4882(5) 0.4278(4) 0.2614(2) 0.0216(11) Uani 1 1 d . . . H33A H 0.4777 0.4856 0.2220 0.026 Uiso 1 1 calc R . . H33B H 0.4194 0.4899 0.2948 0.026 Uiso 1 1 calc R . . C34 C 0.5408(6) 0.7085(6) 0.0772(3) 0.0399(14) Uani 1 1 d . . . Cl3 Cl 0.3902(2) 0.6520(2) 0.10398(8) 0.0715(6) Uani 1 1 d . . . Cl4 Cl 0.7035(2) 0.55856(17) 0.05843(8) 0.0658(5) Uani 1 1 d . . . Cl5 Cl 0.50108(16) 0.82438(15) 0.01141(7) 0.0462(4) Uani 1 1 d . . . H34 H 0.557(6) 0.761(6) 0.112(3) 0.055 Uiso 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 Pd1 0.0165(2) 0.0142(2) 0.0302(2) -0.00171(15) -0.00876(16) -0.00408(14) Cl1 0.0228(7) 0.0183(6) 0.0427(8) -0.0108(5) -0.0041(6) -0.0038(5) Cl2 0.0205(7) 0.0178(6) 0.0505(8) -0.0016(5) -0.0128(6) -0.0073(5) P1 0.0163(7) 0.0156(7) 0.0282(7) -0.0031(5) -0.0082(6) -0.0040(5) P2 0.0174(7) 0.0159(7) 0.0291(7) -0.0010(5) -0.0072(6) -0.0037(5) O1 0.035(2) 0.0192(18) 0.035(2) 0.0012(15) -0.0203(17) -0.0104(15) O2 0.078(3) 0.043(3) 0.073(3) -0.011(2) -0.059(3) -0.001(2) O3 0.057(3) 0.041(2) 0.044(2) -0.0045(18) -0.028(2) -0.0220(19) N1 0.024(2) 0.012(2) 0.026(2) -0.0001(16) -0.0127(18) -0.0069(16) C1 0.028(3) 0.016(3) 0.036(3) -0.007(2) -0.005(2) -0.010(2) C2 0.037(3) 0.027(3) 0.034(3) 0.000(2) -0.008(3) -0.007(2) C3 0.059(4) 0.028(3) 0.041(4) -0.001(3) -0.004(3) -0.010(3) C4 0.075(5) 0.041(4) 0.044(4) -0.016(3) 0.024(4) -0.028(3) C5 0.043(4) 0.051(4) 0.066(5) -0.023(3) 0.016(4) -0.028(3) C6 0.040(4) 0.040(3) 0.040(4) -0.013(3) 0.003(3) -0.021(3) C7 0.020(3) 0.027(3) 0.039(3) 0.002(2) -0.013(2) -0.012(2) C8 0.031(3) 0.032(3) 0.060(4) -0.002(3) -0.017(3) -0.014(3) C9 0.033(4) 0.020(3) 0.112(6) 0.012(3) -0.040(4) -0.008(2) C10 0.052(5) 0.049(4) 0.089(6) 0.037(4) -0.048(4) -0.029(3) C11 0.059(4) 0.050(4) 0.043(4) 0.021(3) -0.028(3) -0.023(3) C12 0.036(3) 0.038(3) 0.044(4) 0.010(3) -0.018(3) -0.017(3) C13 0.021(3) 0.024(3) 0.038(3) 0.004(2) -0.006(2) -0.005(2) C14 0.037(4) 0.066(4) 0.040(4) 0.007(3) -0.005(3) -0.028(3) C15 0.062(5) 0.096(6) 0.034(4) 0.014(4) -0.014(3) -0.037(4) C16 0.073(5) 0.069(5) 0.037(4) 0.016(3) -0.001(4) -0.023(4) C17 0.048(4) 0.058(4) 0.054(4) 0.004(3) 0.004(3) -0.028(3) C18 0.046(4) 0.040(3) 0.042(4) -0.002(3) -0.004(3) -0.022(3) C19 0.020(3) 0.013(2) 0.032(3) 0.002(2) -0.012(2) -0.0062(19) C20 0.024(3) 0.022(3) 0.038(3) -0.005(2) -0.004(2) -0.006(2) C21 0.020(3) 0.020(3) 0.064(4) -0.008(3) -0.008(3) -0.005(2) C22 0.030(3) 0.015(3) 0.068(4) 0.002(3) -0.026(3) -0.004(2) C23 0.036(3) 0.028(3) 0.045(3) 0.001(3) -0.021(3) -0.012(2) C24 0.022(3) 0.019(3) 0.043(3) -0.004(2) -0.008(2) -0.002(2) C25 0.016(3) 0.023(3) 0.027(3) -0.005(2) -0.008(2) -0.006(2) C26 0.028(3) 0.022(3) 0.025(3) -0.001(2) -0.012(2) -0.007(2) C27 0.031(3) 0.020(3) 0.031(3) -0.004(2) -0.018(2) -0.005(2) C28 0.032(3) 0.029(3) 0.031(3) -0.010(2) -0.006(2) -0.008(2) C29 0.023(3) 0.015(3) 0.039(3) -0.003(2) -0.011(2) -0.005(2) C30 0.018(3) 0.019(3) 0.024(3) -0.004(2) -0.005(2) -0.003(2) C31 0.031(3) 0.030(3) 0.034(3) -0.004(2) -0.013(3) -0.005(2) C32 0.018(3) 0.017(3) 0.033(3) -0.001(2) -0.007(2) -0.009(2) C33 0.021(3) 0.012(2) 0.033(3) -0.002(2) -0.009(2) -0.0035(19) C34 0.051(4) 0.037(3) 0.040(4) 0.005(3) -0.011(3) -0.025(3) Cl3 0.0914(14) 0.1092(15) 0.0547(11) 0.0346(10) -0.0367(10) -0.0815(12) Cl4 0.0883(14) 0.0412(9) 0.0544(11) -0.0010(8) -0.0235(9) 0.0001(8) Cl5 0.0475(9) 0.0409(9) 0.0544(10) 0.0165(7) -0.0141(7) -0.0203(7) _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 2.2285(14) . ? Pd1 P1 2.2340(16) . ? Pd1 Cl1 2.3292(14) . ? Pd1 Cl2 2.3640(16) . ? P1 C1 1.789(5) . ? P1 C7 1.817(5) . ? P1 C32 1.849(4) . ? P2 C19 1.807(4) . ? P2 C13 1.815(5) . ? P2 C33 1.834(4) . ? O1 C30 1.348(5) . ? O2 C31 1.282(6) . ? O3 C31 1.248(6) . ? N1 C32 1.459(6) . ? N1 C25 1.459(5) . ? N1 C33 1.472(5) . ? C1 C6 1.400(7) . ? C1 C2 1.402(7) . ? C2 C3 1.377(7) . ? C3 C4 1.385(8) . ? C4 C5 1.363(8) . ? C5 C6 1.382(8) . ? C7 C12 1.375(7) . ? C7 C8 1.395(7) . ? C8 C9 1.386(8) . ? C9 C10 1.372(9) . ? C10 C11 1.365(9) . ? C11 C12 1.388(7) . ? C13 C18 1.379(7) . ? C13 C14 1.406(7) . ? C14 C15 1.369(8) . ? C15 C16 1.372(9) . ? C16 C17 1.354(8) . ? C17 C18 1.384(8) . ? C19 C24 1.390(7) . ? C19 C20 1.394(6) . ? C20 C21 1.382(7) . ? C21 C22 1.370(7) . ? C22 C23 1.388(7) . ? C23 C24 1.394(6) . ? C25 C26 1.389(6) . ? C25 C30 1.410(6) . ? C26 C27 1.374(6) . ? C27 C28 1.411(7) . ? C27 C31 1.469(6) . ? C28 C29 1.373(6) . ? C29 C30 1.406(6) . ? C34 Cl3 1.748(6) . ? C34 Cl4 1.760(6) . ? C34 Cl5 1.762(5) . ? 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 94.15(6) . . ? P2 Pd1 Cl1 174.99(5) . . ? P1 Pd1 Cl1 87.10(6) . . ? P2 Pd1 Cl2 88.34(6) . . ? P1 Pd1 Cl2 177.47(4) . . ? Cl1 Pd1 Cl2 90.38(5) . . ? C1 P1 C7 108.4(2) . . ? C1 P1 C32 99.0(2) . . ? C7 P1 C32 106.4(2) . . ? C1 P1 Pd1 115.02(16) . . ? C7 P1 Pd1 108.66(16) . . ? C32 P1 Pd1 118.53(15) . . ? C19 P2 C13 108.4(2) . . ? C19 P2 C33 98.1(2) . . ? C13 P2 C33 106.7(2) . . ? C19 P2 Pd1 113.36(16) . . ? C13 P2 Pd1 110.65(16) . . ? C33 P2 Pd1 118.67(16) . . ? C32 N1 C25 110.7(3) . . ? C32 N1 C33 112.4(3) . . ? C25 N1 C33 113.1(3) . . ? C6 C1 C2 118.3(5) . . ? C6 C1 P1 121.1(4) . . ? C2 C1 P1 120.3(4) . . ? C3 C2 C1 120.9(5) . . ? C2 C3 C4 119.6(6) . . ? C5 C4 C3 120.5(6) . . ? C4 C5 C6 120.8(6) . . ? C5 C6 C1 119.9(5) . . ? C12 C7 C8 119.0(5) . . ? C12 C7 P1 119.8(4) . . ? C8 C7 P1 121.1(4) . . ? C9 C8 C7 119.9(6) . . ? C10 C9 C8 120.0(6) . . ? C11 C10 C9 120.8(5) . . ? C10 C11 C12 119.5(6) . . ? C7 C12 C11 120.9(5) . . ? C18 C13 C14 118.8(5) . . ? C18 C13 P2 121.2(4) . . ? C14 C13 P2 119.9(4) . . ? C15 C14 C13 119.4(6) . . ? C14 C15 C16 121.3(6) . . ? C17 C16 C15 119.4(6) . . ? C16 C17 C18 121.2(6) . . ? C13 C18 C17 119.9(5) . . ? C24 C19 C20 119.8(4) . . ? C24 C19 P2 118.0(4) . . ? C20 C19 P2 121.6(4) . . ? C21 C20 C19 119.1(5) . . ? C22 C21 C20 121.1(5) . . ? C21 C22 C23 120.7(5) . . ? C22 C23 C24 118.7(5) . . ? C19 C24 C23 120.6(5) . . ? C26 C25 C30 118.3(4) . . ? C26 C25 N1 118.6(4) . . ? C30 C25 N1 123.1(4) . . ? C27 C26 C25 122.1(4) . . ? C26 C27 C28 118.8(4) . . ? C26 C27 C31 121.8(4) . . ? C28 C27 C31 119.3(4) . . ? C29 C28 C27 120.8(4) . . ? C28 C29 C30 119.5(4) . . ? O1 C30 C29 122.1(4) . . ? O1 C30 C25 117.7(4) . . ? C29 C30 C25 120.3(4) . . ? O3 C31 O2 122.8(5) . . ? O3 C31 C27 120.8(5) . . ? O2 C31 C27 116.4(4) . . ? N1 C32 P1 115.4(3) . . ? N1 C33 P2 115.1(3) . . ? Cl3 C34 Cl4 110.9(3) . . ? Cl3 C34 Cl5 110.2(3) . . ? Cl4 C34 Cl5 109.9(3) . . ? 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 H1 Cl2 0.84 2.24 3.064(3) 165.8 1_565 O2 H2 O3 0.84 1.83 2.616(5) 155.5 2_766 _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.899 _refine_diff_density_max 0.931 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.094 #END of data for 2e.CHCl3 data_2a.CHCl3 _database_code_depnum_ccdc_archive 'CCDC 626747' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H30 Cl5 N O3 P2 Pd' _chemical_formula_sum 'C34 H30 Cl5 N O3 P2 Pd' _chemical_formula_weight 846.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4008(2) _cell_length_b 10.9060(2) _cell_length_c 17.6929(5) _cell_angle_alpha 91.922(1) _cell_angle_beta 102.160(1) _cell_angle_gamma 117.036(1) _cell_volume 1728.13(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.626 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8171 _exptl_absorpt_correction_T_max 0.9020 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11581 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0446 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6005 _reflns_number_gt 5318 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0178P)^2^+1.8332P] 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 SHELXL _refine_ls_extinction_coef 0.0023(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6005 _refine_ls_number_parameters 417 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.07705(2) 0.131213(18) 0.231813(10) 0.01440(8) Uani 1 1 d . . . Cl1 Cl -0.14138(7) -0.01760(6) 0.26762(4) 0.02217(15) Uani 1 1 d . . . Cl2 Cl -0.04467(7) 0.24679(7) 0.16369(4) 0.02286(16) Uani 1 1 d . . . P1 P 0.18365(7) 0.02085(6) 0.30392(4) 0.01528(15) Uani 1 1 d . . . P2 P 0.28185(7) 0.27365(6) 0.19462(4) 0.01475(15) Uani 1 1 d . . . N1 N 0.4640(2) 0.2057(2) 0.30243(12) 0.0164(5) Uani 1 1 d . . . O1 O 0.6586(2) 0.1364(2) 0.25263(12) 0.0303(5) Uani 1 1 d . . . H1 H 0.7233 0.1159 0.2438 0.045 Uiso 1 1 calc R . . O2 O 0.5048(2) 0.4376(2) 0.40311(11) 0.0373(5) Uani 1 1 d . . . H2 H 0.4625 0.4719 0.4257 0.056 Uiso 1 1 calc R . . O3 O 0.5914(3) 0.4138(2) 0.52530(12) 0.0386(5) Uani 1 1 d . . . C1 C 0.0780(3) -0.1678(3) 0.28498(15) 0.0182(6) Uani 1 1 d . . . C2 C -0.0106(3) -0.2422(3) 0.33347(17) 0.0288(7) Uani 1 1 d . . . H2A H -0.0153 -0.1943 0.3778 0.035 Uiso 1 1 calc R . . C3 C -0.0920(4) -0.3864(3) 0.31690(18) 0.0354(7) Uani 1 1 d . . . H3 H -0.1532 -0.4368 0.3497 0.043 Uiso 1 1 calc R . . C4 C -0.0846(3) -0.4570(3) 0.25317(17) 0.0291(7) Uani 1 1 d . . . H4 H -0.1392 -0.5558 0.2427 0.035 Uiso 1 1 calc R . . C5 C 0.0020(3) -0.3845(3) 0.20484(16) 0.0257(6) Uani 1 1 d . . . H5 H 0.0070 -0.4331 0.1609 0.031 Uiso 1 1 calc R . . C6 C 0.0821(3) -0.2400(3) 0.22026(15) 0.0221(6) Uani 1 1 d . . . H6 H 0.1403 -0.1902 0.1861 0.027 Uiso 1 1 calc R . . C7 C 0.2141(3) 0.0740(3) 0.40717(15) 0.0203(6) Uani 1 1 d U . . C8 C 0.2720(4) 0.0147(3) 0.46407(17) 0.0331(7) Uani 1 1 d U . . H8 H 0.2937 -0.0570 0.4492 0.040 Uiso 1 1 calc R . . C9 C 0.2979(4) 0.0605(3) 0.54247(18) 0.0401(8) Uani 1 1 d U . . H9 H 0.3366 0.0192 0.5811 0.048 Uiso 1 1 calc R . . C10 C 0.2685(3) 0.1649(3) 0.56513(17) 0.0354(7) Uani 1 1 d U . . H10 H 0.2869 0.1955 0.6191 0.043 Uiso 1 1 calc R . . C11 C 0.2122(3) 0.2249(3) 0.50936(17) 0.0342(7) Uani 1 1 d U . . H11 H 0.1915 0.2970 0.5248 0.041 Uiso 1 1 calc R . . C12 C 0.1856(3) 0.1801(3) 0.43060(16) 0.0275(6) Uani 1 1 d U . . H12 H 0.1475 0.2224 0.3923 0.033 Uiso 1 1 calc R . . C13 C 0.3488(3) 0.4578(3) 0.22189(14) 0.0189(6) Uani 1 1 d . . . C14 C 0.2900(3) 0.5074(3) 0.27109(15) 0.0216(6) Uani 1 1 d . . . H14 H 0.2113 0.4440 0.2913 0.026 Uiso 1 1 calc R . . C15 C 0.3462(3) 0.6501(3) 0.29087(16) 0.0284(7) Uani 1 1 d . . . H15 H 0.3080 0.6842 0.3259 0.034 Uiso 1 1 calc R . . C16 C 0.4573(3) 0.7418(3) 0.25959(17) 0.0311(7) Uani 1 1 d . . . H16 H 0.4932 0.8391 0.2720 0.037 Uiso 1 1 calc R . . C17 C 0.5168(3) 0.6938(3) 0.21047(17) 0.0316(7) Uani 1 1 d . . . H17 H 0.5936 0.7576 0.1892 0.038 Uiso 1 1 calc R . . C18 C 0.4640(3) 0.5522(3) 0.19247(16) 0.0252(6) Uani 1 1 d . . . H18 H 0.5065 0.5189 0.1597 0.030 Uiso 1 1 calc R . . C19 C 0.2415(3) 0.2413(3) 0.08898(15) 0.0183(5) Uani 1 1 d . . . C20 C 0.2319(3) 0.3377(3) 0.04208(16) 0.0289(7) Uani 1 1 d . . . H20 H 0.2475 0.4249 0.0651 0.035 Uiso 1 1 calc R . . C21 C 0.1995(4) 0.3064(3) -0.03874(17) 0.0392(8) Uani 1 1 d . . . H21 H 0.1944 0.3732 -0.0707 0.047 Uiso 1 1 calc R . . C22 C 0.1747(3) 0.1801(3) -0.07270(17) 0.0351(8) Uani 1 1 d . . . H22 H 0.1542 0.1602 -0.1279 0.042 Uiso 1 1 calc R . . C23 C 0.1795(3) 0.0820(3) -0.02674(17) 0.0341(7) Uani 1 1 d . . . H23 H 0.1600 -0.0063 -0.0503 0.041 Uiso 1 1 calc R . . C24 C 0.2127(3) 0.1123(3) 0.05385(16) 0.0269(6) Uani 1 1 d . . . H24 H 0.2158 0.0444 0.0854 0.032 Uiso 1 1 calc R . . C25 C 0.6124(3) 0.2534(3) 0.34981(16) 0.0213(6) Uani 1 1 d . . . C26 C 0.7096(3) 0.2130(3) 0.32436(16) 0.0234(6) Uani 1 1 d . . . C27 C 0.8498(3) 0.2496(3) 0.37187(17) 0.0296(7) Uani 1 1 d . . . H27 H 0.9171 0.2277 0.3531 0.036 Uiso 1 1 calc R . . C28 C 0.8907(3) 0.3188(3) 0.44717(18) 0.0323(7) Uani 1 1 d . . . H28 H 0.9844 0.3395 0.4809 0.039 Uiso 1 1 calc R . . C29 C 0.7978(3) 0.3578(3) 0.47374(16) 0.0245(6) Uani 1 1 d . . . H29 H 0.8268 0.4040 0.5256 0.029 Uiso 1 1 calc R . . C30 C 0.6604(3) 0.3293(3) 0.42410(16) 0.0239(6) Uani 1 1 d . . . C31 C 0.5784(3) 0.3936(3) 0.45428(17) 0.0243(6) Uani 1 1 d . . . C32 C 0.3699(3) 0.0556(3) 0.29622(15) 0.0188(6) Uani 1 1 d . . . H32A H 0.4146 0.0189 0.3385 0.023 Uiso 1 1 calc R . . H32B H 0.3624 0.0086 0.2454 0.023 Uiso 1 1 calc R . . C33 C 0.4521(3) 0.2534(3) 0.22649(15) 0.0190(6) Uani 1 1 d . . . H33A H 0.4504 0.1857 0.1871 0.023 Uiso 1 1 calc R . . H33B H 0.5411 0.3439 0.2294 0.023 Uiso 1 1 calc R . . Cl3 Cl 0.41169(10) 0.70488(9) -0.02806(5) 0.0463(2) Uani 1 1 d . . . Cl4 Cl 0.44074(10) 0.92043(8) 0.08405(5) 0.0425(2) Uani 1 1 d . . . Cl5 Cl 0.16364(10) 0.66377(11) 0.03437(5) 0.0535(2) Uani 1 1 d . . . C34 C 0.3188(3) 0.7861(3) 0.00533(17) 0.0322(7) Uani 1 1 d . . . H34 H 0.2830 0.8278 -0.0384 0.039 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 0.01239(12) 0.01443(12) 0.01621(12) 0.00117(8) 0.00342(8) 0.00637(9) Cl1 0.0158(3) 0.0210(3) 0.0285(4) 0.0021(3) 0.0094(3) 0.0061(3) Cl2 0.0211(3) 0.0230(3) 0.0256(4) 0.0019(3) 0.0000(3) 0.0140(3) P1 0.0144(3) 0.0134(3) 0.0173(3) 0.0023(3) 0.0038(3) 0.0060(3) P2 0.0139(3) 0.0152(3) 0.0144(3) 0.0018(3) 0.0027(3) 0.0066(3) N1 0.0143(11) 0.0164(11) 0.0170(11) 0.0033(8) 0.0025(9) 0.0064(9) O1 0.0230(11) 0.0318(11) 0.0384(12) -0.0077(9) 0.0059(9) 0.0165(10) O2 0.0512(14) 0.0559(14) 0.0237(11) 0.0038(10) 0.0087(10) 0.0414(13) O3 0.0503(14) 0.0501(14) 0.0234(12) -0.0001(10) 0.0016(10) 0.0341(12) C1 0.0156(13) 0.0159(13) 0.0227(14) 0.0046(10) 0.0025(11) 0.0080(11) C2 0.0280(16) 0.0208(14) 0.0330(17) 0.0028(12) 0.0150(13) 0.0047(13) C3 0.0373(18) 0.0246(15) 0.0342(18) 0.0056(13) 0.0171(14) 0.0027(14) C4 0.0288(16) 0.0148(13) 0.0355(17) 0.0023(12) 0.0055(13) 0.0047(13) C5 0.0242(15) 0.0197(14) 0.0287(16) -0.0007(12) 0.0054(13) 0.0074(12) C6 0.0209(14) 0.0196(14) 0.0243(15) 0.0045(11) 0.0067(12) 0.0077(12) C7 0.0191(14) 0.0204(13) 0.0161(13) 0.0032(10) 0.0039(11) 0.0051(12) C8 0.0417(19) 0.0230(15) 0.0280(16) 0.0074(12) 0.0044(14) 0.0113(14) C9 0.047(2) 0.0346(17) 0.0233(16) 0.0134(13) 0.0022(14) 0.0085(16) C10 0.0297(17) 0.0442(19) 0.0189(15) 0.0019(13) 0.0096(13) 0.0049(15) C11 0.0276(17) 0.050(2) 0.0239(16) -0.0061(14) 0.0059(13) 0.0184(15) C12 0.0221(15) 0.0379(17) 0.0239(15) 0.0002(12) 0.0040(12) 0.0165(14) C13 0.0175(13) 0.0193(13) 0.0159(13) 0.0006(10) -0.0020(11) 0.0083(12) C14 0.0227(14) 0.0210(14) 0.0190(14) 0.0017(11) 0.0011(11) 0.0104(12) C15 0.0347(17) 0.0272(15) 0.0222(15) -0.0054(12) -0.0057(13) 0.0196(14) C16 0.0324(17) 0.0158(14) 0.0322(17) -0.0008(12) -0.0086(14) 0.0080(13) C17 0.0262(16) 0.0209(15) 0.0335(17) 0.0022(12) -0.0011(13) 0.0030(13) C18 0.0216(15) 0.0211(14) 0.0267(16) 0.0031(11) 0.0031(12) 0.0063(12) C19 0.0138(13) 0.0210(13) 0.0186(14) 0.0008(10) 0.0042(11) 0.0070(11) C20 0.0341(17) 0.0238(15) 0.0226(15) 0.0019(12) -0.0004(13) 0.0119(14) C21 0.043(2) 0.0407(19) 0.0228(16) 0.0061(14) -0.0005(14) 0.0143(16) C22 0.0269(17) 0.055(2) 0.0166(15) -0.0036(14) 0.0031(13) 0.0151(16) C23 0.0291(17) 0.0412(18) 0.0299(17) -0.0127(14) 0.0026(13) 0.0180(15) C24 0.0267(16) 0.0271(15) 0.0282(16) -0.0012(12) 0.0057(13) 0.0146(13) C25 0.0147(13) 0.0178(13) 0.0256(15) 0.0069(11) 0.0019(11) 0.0039(11) C26 0.0213(15) 0.0190(14) 0.0274(15) 0.0040(11) 0.0073(12) 0.0068(12) C27 0.0341(17) 0.0214(14) 0.0346(17) -0.0006(12) 0.0064(14) 0.0153(14) C28 0.0229(16) 0.0272(16) 0.0409(19) 0.0017(13) -0.0028(13) 0.0118(14) C29 0.0215(15) 0.0245(14) 0.0226(15) 0.0007(11) -0.0007(12) 0.0096(12) C30 0.0233(15) 0.0195(14) 0.0267(16) 0.0067(11) 0.0072(12) 0.0077(12) C31 0.0216(15) 0.0194(14) 0.0324(17) 0.0080(12) 0.0096(12) 0.0086(12) C32 0.0167(13) 0.0157(13) 0.0227(14) 0.0019(10) 0.0023(11) 0.0079(11) C33 0.0161(13) 0.0220(14) 0.0212(14) 0.0074(11) 0.0072(11) 0.0095(12) Cl3 0.0423(5) 0.0401(5) 0.0585(6) 0.0024(4) 0.0237(4) 0.0168(4) Cl4 0.0554(5) 0.0341(4) 0.0344(4) 0.0046(3) 0.0041(4) 0.0214(4) Cl5 0.0328(5) 0.0701(6) 0.0502(6) 0.0140(5) 0.0198(4) 0.0139(5) C34 0.0309(17) 0.0362(17) 0.0287(16) 0.0070(13) 0.0065(13) 0.0153(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3495(6) . ? Pd1 Cl2 2.3566(6) . ? Pd1 P1 2.2419(7) . ? Pd1 P2 2.2437(7) . ? P1 C1 1.815(3) . ? P1 C7 1.815(3) . ? P1 C32 1.833(3) . ? P2 C13 1.809(3) . ? P2 C19 1.812(3) . ? P2 C33 1.856(3) . ? N1 C25 1.432(3) . ? N1 C32 1.462(3) . ? N1 C33 1.458(3) . ? O1 C26 1.354(3) . ? O2 C31 1.306(3) . ? O3 C31 1.236(3) . ? C1 C2 1.394(4) . ? C1 C6 1.387(4) . ? C2 C3 1.390(4) . ? C3 C4 1.379(4) . ? C4 C5 1.374(4) . ? C5 C6 1.391(4) . ? C7 C8 1.392(4) . ? C7 C12 1.389(4) . ? C8 C9 1.386(4) . ? C9 C10 1.374(5) . ? C10 C11 1.376(5) . ? C11 C12 1.388(4) . ? C13 C14 1.385(4) . ? C13 C18 1.394(4) . ? C14 C15 1.391(4) . ? C15 C16 1.377(4) . ? C16 C17 1.380(4) . ? C17 C18 1.381(4) . ? C19 C20 1.386(4) . ? C19 C24 1.392(4) . ? C20 C21 1.391(4) . ? C21 C22 1.372(4) . ? C22 C23 1.377(5) . ? C23 C24 1.385(4) . ? C25 C26 1.415(4) . ? C25 C30 1.392(4) . ? C26 C27 1.387(4) . ? C27 C28 1.388(4) . ? C28 C29 1.373(4) . ? C29 C30 1.400(4) . ? C30 C31 1.489(4) . ? Cl3 C34 1.747(3) . ? Cl4 C34 1.768(3) . ? Cl5 C34 1.756(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl2 90.68(2) . . ? Cl1 Pd1 P1 85.91(2) . . ? Cl1 Pd1 P2 178.46(2) . . ? Cl2 Pd1 P1 175.52(2) . . ? Cl2 Pd1 P2 88.01(2) . . ? P1 Pd1 P2 95.44(2) . . ? Pd1 P1 C1 114.90(8) . . ? Pd1 P1 C7 110.15(9) . . ? Pd1 P1 C32 117.14(9) . . ? C1 P1 C7 107.49(12) . . ? C1 P1 C32 103.25(12) . . ? C7 P1 C32 102.82(12) . . ? Pd1 P2 C13 115.51(9) . . ? Pd1 P2 C19 108.58(8) . . ? Pd1 P2 C33 118.37(8) . . ? C13 P2 C19 107.01(12) . . ? C13 P2 C33 103.46(12) . . ? C19 P2 C33 102.69(12) . . ? C25 N1 C32 113.0(2) . . ? C25 N1 C33 116.0(2) . . ? C32 N1 C33 111.9(2) . . ? P1 C1 C2 121.2(2) . . ? P1 C1 C6 119.8(2) . . ? C2 C1 C6 118.9(2) . . ? C1 C2 C3 120.0(3) . . ? C2 C3 C4 120.5(3) . . ? C3 C4 C5 120.0(3) . . ? C4 C5 C6 120.0(3) . . ? C1 C6 C5 120.6(3) . . ? P1 C7 C8 121.2(2) . . ? P1 C7 C12 119.8(2) . . ? C8 C7 C12 118.9(3) . . ? C7 C8 C9 119.7(3) . . ? C8 C9 C10 121.0(3) . . ? C9 C10 C11 119.7(3) . . ? C10 C11 C12 120.0(3) . . ? C7 C12 C11 120.7(3) . . ? P2 C13 C14 122.2(2) . . ? P2 C13 C18 118.5(2) . . ? C14 C13 C18 119.3(2) . . ? C13 C14 C15 120.0(3) . . ? C14 C15 C16 119.9(3) . . ? C15 C16 C17 120.6(3) . . ? C16 C17 C18 119.5(3) . . ? C13 C18 C17 120.6(3) . . ? P2 C19 C20 122.5(2) . . ? P2 C19 C24 118.4(2) . . ? C20 C19 C24 119.1(2) . . ? C19 C20 C21 119.8(3) . . ? C20 C21 C22 120.6(3) . . ? C21 C22 C23 120.0(3) . . ? C22 C23 C24 119.9(3) . . ? C19 C24 C23 120.5(3) . . ? N1 C25 C26 120.0(2) . . ? N1 C25 C30 121.5(2) . . ? C26 C25 C30 118.3(2) . . ? O1 C26 C25 117.0(2) . . ? O1 C26 C27 122.2(3) . . ? C25 C26 C27 120.8(3) . . ? C26 C27 C28 119.2(3) . . ? C27 C28 C29 121.1(3) . . ? C28 C29 C30 119.8(3) . . ? C25 C30 C29 120.6(3) . . ? C25 C30 C31 123.8(2) . . ? C29 C30 C31 115.5(2) . . ? O2 C31 O3 122.8(3) . . ? O2 C31 C30 116.7(2) . . ? O3 C31 C30 120.3(2) . . ? P1 C32 N1 109.21(17) . . ? P2 C33 N1 112.30(17) . . ? Cl3 C34 Cl4 110.53(17) . . ? Cl3 C34 Cl5 110.25(17) . . ? Cl4 C34 Cl5 110.13(17) . . ? 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 H1 Cl1 0.84 2.44 3.192(2) 150.3 1_655 O1 H1 Cl2 0.84 2.88 3.499(2) 131.7 1_655 O2 H2 O3 0.84 1.84 2.665(3) 166.4 2_666 _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.626 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.073 # End of data for 2a.CHCl3 data_4.2.5MeOH _database_code_depnum_ccdc_archive 'CCDC 626748' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36.50 H39 Cl2 N O6.50 P2 Pd' _chemical_formula_sum 'C36.50 H39 Cl2 N O6.50 P2 Pd' _chemical_formula_weight 834.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.1097(10) _cell_length_b 8.0163(2) _cell_length_c 19.7326(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.948(1) _cell_angle_gamma 90.00 _cell_volume 3912.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1708 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8091 _exptl_absorpt_correction_T_max 0.9299 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15853 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0756 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6657 _reflns_number_gt 4940 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0511P)^2^+5.4877P] 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 6657 _refine_ls_number_parameters 445 _refine_ls_number_restraints 111 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.002 _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 0.160466(14) 0.14382(4) 0.084216(17) 0.01695(12) Uani 1 1 d . . . Cl1 Cl 0.16100(6) 0.33238(14) 0.17533(6) 0.0303(3) Uani 1 1 d . . . Cl2 Cl 0.12063(5) 0.34357(13) 0.00490(6) 0.0236(3) Uani 1 1 d . . . P1 P 0.20189(5) -0.03757(14) 0.16303(6) 0.0174(3) Uani 1 1 d . . . P2 P 0.15713(5) -0.02223(14) -0.00822(6) 0.0171(3) Uani 1 1 d . . . N1 N 0.21928(15) -0.2673(4) 0.06363(19) 0.0184(9) Uani 1 1 d . . . O1 O 0.43737(16) -0.1886(5) 0.1572(2) 0.0449(10) Uani 1 1 d . . . H1 H 0.4606 -0.1902 0.1934 0.067 Uiso 1 1 calc R . . O2 O 0.41808(15) -0.4387(5) 0.19434(18) 0.0389(9) Uani 1 1 d . . . O3 O 0.46814(14) -0.4404(5) 0.05989(18) 0.0366(9) Uani 1 1 d . . . O4 O 0.43226(15) -0.4662(6) -0.05177(18) 0.0435(10) Uani 1 1 d . . . H4 H 0.4641 -0.4940 -0.0546 0.065 Uiso 1 1 calc R . . C1 C 0.16835(19) -0.0604(5) 0.2364(2) 0.0192(10) Uani 1 1 d . . . C2 C 0.12230(19) -0.1609(6) 0.2322(2) 0.0214(11) Uani 1 1 d . . . H2A H 0.1103 -0.2262 0.1923 0.026 Uiso 1 1 calc R . . C3 C 0.0941(2) -0.1637(6) 0.2875(3) 0.0274(12) Uani 1 1 d . . . H3A H 0.0632 -0.2330 0.2852 0.033 Uiso 1 1 calc R . . C4 C 0.1106(2) -0.0676(6) 0.3453(2) 0.0279(12) Uani 1 1 d . . . H4A H 0.0906 -0.0689 0.3819 0.033 Uiso 1 1 calc R . . C5 C 0.1564(2) 0.0307(6) 0.3499(3) 0.0271(12) Uani 1 1 d . . . H5A H 0.1683 0.0949 0.3902 0.032 Uiso 1 1 calc R . . C6 C 0.1849(2) 0.0355(6) 0.2958(2) 0.0232(11) Uani 1 1 d . . . H6A H 0.2160 0.1044 0.2989 0.028 Uiso 1 1 calc R . . C7 C 0.27061(19) 0.0244(6) 0.1990(2) 0.0214(11) Uani 1 1 d . . . C8 C 0.3004(2) -0.0680(6) 0.2517(2) 0.0263(12) Uani 1 1 d . . . H8 H 0.2843 -0.1608 0.2702 0.032 Uiso 1 1 calc R . . C9 C 0.3534(2) -0.0267(7) 0.2776(3) 0.0364(14) Uani 1 1 d . . . H9 H 0.3739 -0.0921 0.3130 0.044 Uiso 1 1 calc R . . C10 C 0.3764(2) 0.1115(8) 0.2516(3) 0.0407(15) Uani 1 1 d . . . H10 H 0.4127 0.1414 0.2697 0.049 Uiso 1 1 calc R . . C11 C 0.3476(2) 0.2044(8) 0.2003(3) 0.0391(14) Uani 1 1 d . . . H11 H 0.3637 0.2983 0.1825 0.047 Uiso 1 1 calc R . . C12 C 0.2939(2) 0.1609(6) 0.1737(3) 0.0299(12) Uani 1 1 d . . . H12 H 0.2736 0.2260 0.1380 0.036 Uiso 1 1 calc R . . C13 C 0.20562(19) 0.0358(6) -0.0620(2) 0.0206(10) Uani 1 1 d U . . C14 C 0.2459(2) 0.1532(6) -0.0392(3) 0.0316(11) Uani 1 1 d U . . H14 H 0.2472 0.2059 0.0042 0.038 Uiso 1 1 calc R . . C15 C 0.2838(2) 0.1927(7) -0.0798(3) 0.0405(13) Uani 1 1 d U . . H15 H 0.3114 0.2715 -0.0637 0.049 Uiso 1 1 calc R . . C16 C 0.2822(2) 0.1194(7) -0.1429(3) 0.0389(12) Uani 1 1 d U . . H16 H 0.3086 0.1469 -0.1702 0.047 Uiso 1 1 calc R . . C17 C 0.2419(2) 0.0052(6) -0.1669(3) 0.0297(11) Uani 1 1 d U . . H17 H 0.2403 -0.0436 -0.2110 0.036 Uiso 1 1 calc R . . C18 C 0.2040(2) -0.0379(6) -0.1266(2) 0.0262(10) Uani 1 1 d U . . H18 H 0.1768 -0.1177 -0.1429 0.031 Uiso 1 1 calc R . . C19 C 0.09119(19) -0.0313(6) -0.0626(2) 0.0206(10) Uani 1 1 d U . . C20 C 0.0793(2) 0.0500(6) -0.1261(2) 0.0264(10) Uani 1 1 d U . . H20 H 0.1061 0.1154 -0.1422 0.032 Uiso 1 1 calc R . . C21 C 0.0283(2) 0.0345(7) -0.1653(3) 0.0339(11) Uani 1 1 d U . . H21 H 0.0203 0.0889 -0.2087 0.041 Uiso 1 1 calc R . . C22 C -0.0110(2) -0.0590(7) -0.1422(3) 0.0362(12) Uani 1 1 d U . . H22 H -0.0456 -0.0704 -0.1701 0.043 Uiso 1 1 calc R . . C23 C -0.0003(2) -0.1356(6) -0.0793(3) 0.0324(11) Uani 1 1 d U . . H23 H -0.0279 -0.1975 -0.0631 0.039 Uiso 1 1 calc R . . C24 C 0.04989(19) -0.1230(6) -0.0395(3) 0.0255(10) Uani 1 1 d U . . H24 H 0.0570 -0.1767 0.0041 0.031 Uiso 1 1 calc R . . C25 C 0.27021(18) -0.3002(5) 0.0494(2) 0.0191(10) Uani 1 1 d . . . C26 C 0.31564(19) -0.2990(6) 0.1020(2) 0.0207(11) Uani 1 1 d . . . H26 H 0.3111 -0.2704 0.1474 0.025 Uiso 1 1 calc R . . C27 C 0.36646(19) -0.3380(6) 0.0900(2) 0.0216(11) Uani 1 1 d . . . C28 C 0.37503(19) -0.3803(6) 0.0242(2) 0.0235(11) Uani 1 1 d . . . C29 C 0.3304(2) -0.3777(6) -0.0284(2) 0.0268(12) Uani 1 1 d . . . H29 H 0.3354 -0.4043 -0.0738 0.032 Uiso 1 1 calc R . . C30 C 0.2795(2) -0.3381(6) -0.0173(2) 0.0237(11) Uani 1 1 d . . . H30 H 0.2502 -0.3364 -0.0549 0.028 Uiso 1 1 calc R . . C31 C 0.4109(2) -0.3285(6) 0.1512(3) 0.0275(12) Uani 1 1 d . . . C32 C 0.20701(19) -0.2554(5) 0.1329(2) 0.0207(11) Uani 1 1 d . . . H32A H 0.2356 -0.3139 0.1651 0.025 Uiso 1 1 calc R . . H32B H 0.1724 -0.3133 0.1342 0.025 Uiso 1 1 calc R . . C33 C 0.17202(18) -0.2463(5) 0.0103(2) 0.0180(10) Uani 1 1 d . . . H33A H 0.1404 -0.2996 0.0252 0.022 Uiso 1 1 calc R . . H33B H 0.1783 -0.3026 -0.0323 0.022 Uiso 1 1 calc R . . C34 C 0.4294(2) -0.4289(6) 0.0127(3) 0.0280(12) Uani 1 1 d . . . O5 O 0.07152(14) 0.6165(4) 0.0971(2) 0.0340(9) Uani 1 1 d U . . H5 H 0.0888 0.5290 0.0917 0.051 Uiso 1 1 calc R . . C35 C 0.0193(3) 0.5752(8) 0.1049(4) 0.067(2) Uani 1 1 d U . . H35A H 0.0202 0.5178 0.1490 0.101 Uiso 1 1 calc R . . H35B H 0.0031 0.5017 0.0673 0.101 Uiso 1 1 calc R . . H35C H -0.0024 0.6771 0.1042 0.101 Uiso 1 1 calc R . . O6 O 0.5045(2) -0.1736(7) 0.2695(3) 0.0878(18) Uani 1 1 d U . . H6 H 0.5245 -0.0908 0.2807 0.132 Uiso 1 1 calc R . . C36 C 0.5021(3) -0.2695(11) 0.3268(4) 0.078(2) Uani 1 1 d U . . H36A H 0.5350 -0.3370 0.3376 0.117 Uiso 1 1 calc R . . H36B H 0.4705 -0.3429 0.3177 0.117 Uiso 1 1 calc R . . H36C H 0.4991 -0.1966 0.3658 0.117 Uiso 1 1 calc R . . O7 O 0.4900(9) -0.546(2) 0.5199(10) 0.170(7) Uiso 0.50 1 d PU . . C37 C 0.4299(11) -0.563(3) 0.4844(13) 0.135(8) Uiso 0.50 1 d PU . . 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 0.0221(2) 0.01340(19) 0.0164(2) 0.00029(14) 0.00611(15) 0.00048(15) Cl1 0.0511(9) 0.0196(6) 0.0199(7) -0.0028(5) 0.0055(6) 0.0049(6) Cl2 0.0353(7) 0.0171(6) 0.0191(6) 0.0039(4) 0.0071(5) 0.0039(5) P1 0.0196(7) 0.0169(6) 0.0167(6) 0.0014(5) 0.0062(5) -0.0001(5) P2 0.0175(7) 0.0158(6) 0.0189(7) -0.0009(5) 0.0053(5) 0.0013(5) N1 0.017(2) 0.018(2) 0.021(2) -0.0016(16) 0.0065(17) 0.0012(16) O1 0.040(3) 0.032(2) 0.056(3) -0.0018(18) -0.011(2) -0.0036(19) O2 0.034(2) 0.044(2) 0.036(2) 0.0078(19) -0.0027(17) -0.0042(18) O3 0.025(2) 0.054(2) 0.032(2) -0.0032(18) 0.0067(18) 0.0105(18) O4 0.024(2) 0.077(3) 0.031(2) -0.004(2) 0.0110(17) 0.016(2) C1 0.023(3) 0.019(2) 0.017(3) 0.0091(19) 0.009(2) 0.007(2) C2 0.022(3) 0.025(3) 0.017(3) 0.0062(19) 0.002(2) 0.005(2) C3 0.022(3) 0.027(3) 0.034(3) 0.015(2) 0.009(2) 0.002(2) C4 0.031(3) 0.035(3) 0.021(3) 0.009(2) 0.015(2) 0.016(2) C5 0.033(3) 0.027(3) 0.021(3) -0.001(2) 0.004(2) 0.006(2) C6 0.031(3) 0.019(3) 0.021(3) 0.002(2) 0.007(2) 0.005(2) C7 0.022(3) 0.024(3) 0.020(3) -0.006(2) 0.009(2) 0.001(2) C8 0.024(3) 0.035(3) 0.020(3) -0.004(2) 0.003(2) 0.002(2) C9 0.029(3) 0.053(4) 0.027(3) -0.005(3) 0.002(2) 0.004(3) C10 0.023(3) 0.066(4) 0.033(3) -0.014(3) 0.004(3) -0.008(3) C11 0.030(3) 0.051(4) 0.039(4) -0.006(3) 0.013(3) -0.013(3) C12 0.030(3) 0.030(3) 0.030(3) 0.000(2) 0.008(2) -0.005(2) C13 0.025(2) 0.017(2) 0.021(2) 0.0004(18) 0.0071(19) 0.0027(18) C14 0.034(3) 0.031(3) 0.033(3) -0.008(2) 0.015(2) -0.007(2) C15 0.035(3) 0.042(3) 0.048(3) -0.006(2) 0.020(2) -0.014(2) C16 0.043(3) 0.040(3) 0.040(3) 0.003(2) 0.027(2) 0.002(2) C17 0.040(3) 0.033(3) 0.019(2) 0.0043(19) 0.013(2) 0.008(2) C18 0.032(3) 0.026(3) 0.022(2) -0.0016(18) 0.008(2) 0.003(2) C19 0.019(2) 0.016(2) 0.026(2) -0.0061(17) 0.0008(19) 0.0031(18) C20 0.029(2) 0.021(2) 0.028(3) -0.0013(19) 0.000(2) 0.003(2) C21 0.033(3) 0.033(3) 0.031(3) -0.002(2) -0.007(2) 0.013(2) C22 0.024(3) 0.035(3) 0.045(3) -0.012(2) -0.006(2) 0.008(2) C23 0.023(2) 0.025(3) 0.049(3) -0.008(2) 0.005(2) 0.001(2) C24 0.022(2) 0.021(2) 0.034(3) -0.0044(19) 0.0075(19) 0.0047(19) C25 0.014(3) 0.016(2) 0.027(3) 0.0008(19) 0.004(2) 0.0011(19) C26 0.026(3) 0.020(2) 0.017(3) -0.0015(19) 0.006(2) 0.001(2) C27 0.020(3) 0.019(3) 0.026(3) 0.001(2) 0.003(2) 0.001(2) C28 0.020(3) 0.026(3) 0.027(3) 0.001(2) 0.011(2) 0.004(2) C29 0.030(3) 0.034(3) 0.019(3) -0.001(2) 0.014(2) 0.005(2) C30 0.021(3) 0.032(3) 0.017(3) -0.003(2) 0.002(2) 0.004(2) C31 0.025(3) 0.022(3) 0.038(3) -0.004(2) 0.012(2) 0.003(2) C32 0.022(3) 0.016(2) 0.025(3) 0.0048(19) 0.005(2) 0.003(2) C33 0.015(3) 0.018(2) 0.022(3) -0.0031(19) 0.006(2) 0.0029(19) C34 0.026(3) 0.030(3) 0.032(3) 0.003(2) 0.014(3) 0.007(2) O5 0.029(2) 0.0208(18) 0.055(2) -0.0032(17) 0.0163(18) 0.0043(15) C35 0.043(4) 0.039(4) 0.129(6) -0.020(4) 0.040(4) -0.004(3) O6 0.092(4) 0.063(4) 0.089(4) 0.008(3) -0.040(3) -0.023(3) C36 0.069(5) 0.089(6) 0.069(5) -0.009(4) -0.009(4) -0.004(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3471(12) . ? Pd1 Cl2 2.3395(11) . ? Pd1 P1 2.2485(12) . ? Pd1 P2 2.2479(12) . ? P1 C1 1.806(4) . ? P1 C7 1.818(5) . ? P1 C32 1.856(4) . ? P2 C13 1.809(5) . ? P2 C19 1.812(5) . ? P2 C33 1.858(4) . ? N1 C25 1.381(6) . ? N1 C32 1.456(6) . ? N1 C33 1.454(6) . ? O1 C31 1.299(6) . ? O2 C31 1.218(6) . ? O3 C34 1.228(6) . ? O4 C34 1.321(6) . ? C1 C2 1.399(7) . ? C1 C6 1.403(6) . ? C2 C3 1.400(7) . ? C3 C4 1.379(7) . ? C4 C5 1.384(7) . ? C5 C6 1.385(7) . ? C7 C8 1.387(7) . ? C7 C12 1.375(7) . ? C8 C9 1.379(7) . ? C9 C10 1.389(8) . ? C10 C11 1.360(8) . ? C11 C12 1.403(7) . ? C13 C14 1.398(7) . ? C13 C18 1.399(6) . ? C14 C15 1.383(7) . ? C15 C16 1.371(8) . ? C16 C17 1.385(8) . ? C17 C18 1.385(7) . ? C19 C20 1.398(7) . ? C19 C24 1.410(7) . ? C20 C21 1.383(7) . ? C21 C22 1.378(8) . ? C22 C23 1.370(8) . ? C23 C24 1.369(7) . ? C25 C26 1.404(6) . ? C25 C30 1.409(6) . ? C26 C27 1.373(6) . ? C27 C28 1.394(6) . ? C27 C31 1.497(7) . ? C28 C29 1.389(7) . ? C28 C34 1.475(7) . ? C29 C30 1.372(7) . ? O5 C35 1.388(7) . ? O6 C36 1.377(9) . ? O7 C37 1.56(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl2 90.97(4) . . ? Cl1 Pd1 P1 86.90(4) . . ? Cl1 Pd1 P2 175.84(4) . . ? Cl2 Pd1 P1 176.92(4) . . ? Cl2 Pd1 P2 84.88(4) . . ? P1 Pd1 P2 97.25(4) . . ? Pd1 P1 C1 113.34(15) . . ? Pd1 P1 C7 112.81(16) . . ? Pd1 P1 C32 115.87(15) . . ? C1 P1 C7 104.9(2) . . ? C1 P1 C32 103.2(2) . . ? C7 P1 C32 105.6(2) . . ? Pd1 P2 C13 112.91(15) . . ? Pd1 P2 C19 113.97(15) . . ? Pd1 P2 C33 115.79(15) . . ? C13 P2 C19 107.6(2) . . ? C13 P2 C33 103.3(2) . . ? C19 P2 C33 102.1(2) . . ? C25 N1 C32 123.9(4) . . ? C25 N1 C33 122.9(4) . . ? C32 N1 C33 113.2(3) . . ? P1 C1 C2 120.3(4) . . ? P1 C1 C6 120.1(4) . . ? C2 C1 C6 119.2(4) . . ? C1 C2 C3 119.1(4) . . ? C2 C3 C4 121.0(5) . . ? C3 C4 C5 120.1(5) . . ? C4 C5 C6 119.8(5) . . ? C1 C6 C5 120.7(5) . . ? P1 C7 C8 120.0(4) . . ? P1 C7 C12 120.7(4) . . ? C8 C7 C12 119.3(5) . . ? C7 C8 C9 120.7(5) . . ? C8 C9 C10 119.4(5) . . ? C9 C10 C11 120.6(5) . . ? C10 C11 C12 119.8(5) . . ? C7 C12 C11 120.2(5) . . ? P2 C13 C14 120.5(4) . . ? P2 C13 C18 120.6(4) . . ? C14 C13 C18 119.0(4) . . ? C13 C14 C15 120.0(5) . . ? C14 C15 C16 120.8(5) . . ? C15 C16 C17 119.9(5) . . ? C16 C17 C18 120.2(5) . . ? C13 C18 C17 120.1(5) . . ? P2 C19 C20 122.9(4) . . ? P2 C19 C24 118.5(4) . . ? C20 C19 C24 118.6(4) . . ? C19 C20 C21 119.6(5) . . ? C20 C21 C22 120.7(5) . . ? C21 C22 C23 120.3(5) . . ? C22 C23 C24 120.2(5) . . ? C19 C24 C23 120.6(5) . . ? N1 C25 C26 120.7(4) . . ? N1 C25 C30 122.6(4) . . ? C26 C25 C30 116.7(4) . . ? C25 C26 C27 122.1(4) . . ? C26 C27 C28 120.9(4) . . ? C26 C27 C31 115.7(4) . . ? C28 C27 C31 123.4(4) . . ? C27 C28 C29 117.3(4) . . ? C27 C28 C34 120.2(4) . . ? C29 C28 C34 122.5(4) . . ? C28 C29 C30 122.6(4) . . ? C25 C30 C29 120.5(4) . . ? O1 C31 O2 123.4(5) . . ? O1 C31 C27 114.6(4) . . ? O2 C31 C27 121.8(4) . . ? P1 C32 N1 113.6(3) . . ? P2 C33 N1 111.5(3) . . ? O3 C34 O4 123.1(4) . . ? O3 C34 C28 122.4(5) . . ? O4 C34 C28 114.4(4) . . ? 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 O5 H5 Cl2 0.84 2.50 3.223(4) 144.5 . O5 H5 Cl1 0.84 2.73 3.379(4) 135.2 . O1 H1 O6 0.84 1.71 2.543(6) 173.6 . O4 H4 O3 0.84 1.80 2.642(5) 178.4 3_645 O6 H6 O2 0.84 1.89 2.713(6) 167.4 2_655 _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.024 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.105 # End of data for 4.2.5MeOH data_4.3DMSO _database_code_depnum_ccdc_archive 'CCDC 626749' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H47 Cl2 N O7 P2 Pd S3' _chemical_formula_sum 'C40 H47 Cl2 N O7 P2 Pd S3' _chemical_formula_weight 989.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3355(2) _cell_length_b 13.5157(3) _cell_length_c 14.6704(2) _cell_angle_alpha 67.561(1) _cell_angle_beta 86.733(1) _cell_angle_gamma 80.258(1) _cell_volume 2228.03(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8258 _exptl_absorpt_correction_T_max 0.9613 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28952 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7779 _reflns_number_gt 6342 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0655P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0008(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7779 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1137 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.15136(2) 0.029632(19) 0.221184(16) 0.01183(11) Uani 1 1 d . . . Cl1 Cl 0.04512(7) -0.11052(7) 0.26709(6) 0.0172(2) Uani 1 1 d . . . Cl2 Cl 0.31628(7) -0.09496(7) 0.24778(6) 0.0208(2) Uani 1 1 d . . . P1 P -0.00884(7) 0.13975(7) 0.21133(6) 0.0109(2) Uani 1 1 d . . . P2 P 0.25688(7) 0.16067(7) 0.16227(6) 0.0132(2) Uani 1 1 d . . . N1 N 0.0777(2) 0.3215(2) 0.09463(19) 0.0146(6) Uani 1 1 d . . . O1 O 0.2098(2) 0.6042(2) -0.25549(19) 0.0272(6) Uani 1 1 d . . . O2 O 0.2442(2) 0.4494(2) -0.28139(18) 0.0260(6) Uani 1 1 d . . . H2 H 0.2943 0.4789 -0.3174 0.039 Uiso 1 1 calc R . . O3 O 0.0169(2) 0.5931(2) -0.37365(17) 0.0240(6) Uani 1 1 d . . . O4 O -0.1531(2) 0.5710(3) -0.32278(19) 0.0448(9) Uani 1 1 d . . . H4 H -0.1681 0.6092 -0.3823 0.067 Uiso 1 1 calc R . . C1 C -0.1054(3) 0.1415(3) 0.1223(2) 0.0126(7) Uani 1 1 d . . . C2 C -0.0676(3) 0.1150(3) 0.0425(2) 0.0173(8) Uani 1 1 d . . . H2A H 0.0073 0.0845 0.0402 0.021 Uiso 1 1 calc R . . C3 C -0.1386(3) 0.1328(3) -0.0341(3) 0.0236(9) Uani 1 1 d . . . H3 H -0.1119 0.1158 -0.0893 0.028 Uiso 1 1 calc R . . C4 C -0.2475(3) 0.1751(3) -0.0305(3) 0.0230(8) Uani 1 1 d . . . H4A H -0.2958 0.1867 -0.0831 0.028 Uiso 1 1 calc R . . C5 C -0.2874(3) 0.2008(3) 0.0494(3) 0.0211(8) Uani 1 1 d . . . H5 H -0.3630 0.2289 0.0520 0.025 Uiso 1 1 calc R . . C6 C -0.2166(3) 0.1855(3) 0.1256(2) 0.0160(7) Uani 1 1 d . . . H6 H -0.2432 0.2046 0.1797 0.019 Uiso 1 1 calc R . . C7 C -0.0769(3) 0.1072(3) 0.3297(2) 0.0130(7) Uani 1 1 d . . . C8 C -0.1503(3) 0.0337(3) 0.3569(2) 0.0163(7) Uani 1 1 d . . . H8 H -0.1665 0.0023 0.3124 0.020 Uiso 1 1 calc R . . C9 C -0.1999(3) 0.0059(3) 0.4481(2) 0.0194(8) Uani 1 1 d . . . H9 H -0.2504 -0.0442 0.4659 0.023 Uiso 1 1 calc R . . C10 C -0.1761(3) 0.0511(3) 0.5136(2) 0.0222(8) Uani 1 1 d . . . H10 H -0.2117 0.0335 0.5757 0.027 Uiso 1 1 calc R . . C11 C -0.1012(3) 0.1212(3) 0.4887(2) 0.0216(8) Uani 1 1 d . . . H11 H -0.0835 0.1504 0.5344 0.026 Uiso 1 1 calc R . . C12 C -0.0510(3) 0.1499(3) 0.3970(2) 0.0189(8) Uani 1 1 d . . . H12 H 0.0008 0.1985 0.3802 0.023 Uiso 1 1 calc R . . C13 C 0.3247(3) 0.1600(3) 0.0492(2) 0.0163(7) Uani 1 1 d . . . C14 C 0.3939(3) 0.2364(3) -0.0002(2) 0.0190(8) Uani 1 1 d . . . H14 H 0.4052 0.2888 0.0252 0.023 Uiso 1 1 calc R . . C15 C 0.4452(3) 0.2348(3) -0.0858(3) 0.0249(9) Uani 1 1 d . . . H15 H 0.4921 0.2862 -0.1193 0.030 Uiso 1 1 calc R . . C16 C 0.4285(3) 0.1583(3) -0.1234(3) 0.0254(9) Uani 1 1 d . . . H16 H 0.4650 0.1570 -0.1818 0.030 Uiso 1 1 calc R . . C17 C 0.3592(3) 0.0842(3) -0.0763(3) 0.0264(9) Uani 1 1 d . . . H17 H 0.3474 0.0325 -0.1025 0.032 Uiso 1 1 calc R . . C18 C 0.3064(3) 0.0856(3) 0.0102(2) 0.0193(8) Uani 1 1 d . . . H18 H 0.2578 0.0354 0.0423 0.023 Uiso 1 1 calc R . . C19 C 0.3636(3) 0.1469(3) 0.2486(2) 0.0158(7) Uani 1 1 d . . . C20 C 0.4723(3) 0.1027(3) 0.2387(3) 0.0207(8) Uani 1 1 d . . . H20 H 0.4923 0.0803 0.1852 0.025 Uiso 1 1 calc R . . C21 C 0.5510(3) 0.0915(3) 0.3074(3) 0.0234(8) Uani 1 1 d . . . H21 H 0.6250 0.0617 0.3004 0.028 Uiso 1 1 calc R . . C22 C 0.5231(3) 0.1231(3) 0.3857(3) 0.0266(9) Uani 1 1 d . . . H22 H 0.5778 0.1156 0.4320 0.032 Uiso 1 1 calc R . . C23 C 0.4149(3) 0.1661(3) 0.3967(3) 0.0223(8) Uani 1 1 d . . . H23 H 0.3953 0.1879 0.4506 0.027 Uiso 1 1 calc R . . C24 C 0.3358(3) 0.1770(3) 0.3290(2) 0.0198(8) Uani 1 1 d . . . H24 H 0.2617 0.2053 0.3373 0.024 Uiso 1 1 calc R . . C25 C 0.1892(3) 0.3020(3) 0.1316(2) 0.0141(7) Uani 1 1 d . . . H25A H 0.1874 0.3197 0.1913 0.017 Uiso 1 1 calc R . . H25B H 0.2331 0.3510 0.0812 0.017 Uiso 1 1 calc R . . C26 C -0.0009(3) 0.2851(3) 0.1728(2) 0.0132(7) Uani 1 1 d . . . H26A H -0.0746 0.3279 0.1498 0.016 Uiso 1 1 calc R . . H26B H 0.0199 0.2991 0.2304 0.016 Uiso 1 1 calc R . . C27 C 0.0489(3) 0.3730(3) -0.0043(2) 0.0136(7) Uani 1 1 d . . . C28 C 0.1279(3) 0.4121(3) -0.0764(2) 0.0159(7) Uani 1 1 d . . . H28 H 0.2030 0.3996 -0.0575 0.019 Uiso 1 1 calc R . . C29 C 0.0978(3) 0.4686(3) -0.1748(2) 0.0137(7) Uani 1 1 d . . . C30 C -0.0121(3) 0.4881(3) -0.2053(2) 0.0146(7) Uani 1 1 d . . . C31 C -0.0885(3) 0.4464(3) -0.1329(2) 0.0178(8) Uani 1 1 d . . . H31 H -0.1633 0.4573 -0.1518 0.021 Uiso 1 1 calc R . . C32 C -0.0605(3) 0.3909(3) -0.0362(2) 0.0158(7) Uani 1 1 d . . . H32 H -0.1156 0.3638 0.0104 0.019 Uiso 1 1 calc R . . C33 C 0.1882(3) 0.5166(3) -0.2433(2) 0.0163(8) Uani 1 1 d . . . C34 C -0.0455(3) 0.5548(3) -0.3088(2) 0.0175(8) Uani 1 1 d . . . S1 S 0.44548(8) 0.50737(8) 0.12004(7) 0.0271(2) Uani 1 1 d . . . O5 O 0.3631(2) 0.4751(2) 0.0698(2) 0.0371(7) Uani 1 1 d . . . C35 C 0.3890(4) 0.5014(4) 0.2359(3) 0.0425(12) Uani 1 1 d . . . H35A H 0.3293 0.5625 0.2258 0.064 Uiso 1 1 calc R . . H35B H 0.4464 0.5051 0.2775 0.064 Uiso 1 1 calc R . . H35C H 0.3601 0.4331 0.2684 0.064 Uiso 1 1 calc R . . C36 C 0.5519(4) 0.3936(4) 0.1658(3) 0.0386(11) Uani 1 1 d . . . H36A H 0.5193 0.3282 0.2016 0.058 Uiso 1 1 calc R . . H36B H 0.5999 0.4054 0.2104 0.058 Uiso 1 1 calc R . . H36C H 0.5950 0.3846 0.1105 0.058 Uiso 1 1 calc R . . S2 S -0.14560(8) 0.74299(7) -0.57729(6) 0.0232(2) Uani 1 1 d . . . O6 O -0.2230(2) 0.6822(2) -0.49923(18) 0.0314(7) Uani 1 1 d . . . C37 C -0.0540(3) 0.6421(3) -0.6055(3) 0.0271(9) Uani 1 1 d . . . H37A H -0.0960 0.5915 -0.6152 0.041 Uiso 1 1 calc R . . H37B H -0.0016 0.6026 -0.5509 0.041 Uiso 1 1 calc R . . H37C H -0.0140 0.6767 -0.6659 0.041 Uiso 1 1 calc R . . C38 C -0.2255(4) 0.7978(3) -0.6886(3) 0.0320(10) Uani 1 1 d . . . H38A H -0.2899 0.8479 -0.6818 0.048 Uiso 1 1 calc R . . H38B H -0.2497 0.7387 -0.7012 0.048 Uiso 1 1 calc R . . H38C H -0.1806 0.8367 -0.7437 0.048 Uiso 1 1 calc R . . S3 S 0.36916(9) 0.65665(8) -0.46513(7) 0.0322(3) Uani 1 1 d . . . O7 O 0.4010(2) 0.5404(2) -0.39117(19) 0.0342(7) Uani 1 1 d . . . C39 C 0.4757(4) 0.6739(4) -0.5546(3) 0.0408(11) Uani 1 1 d . . . H39A H 0.4823 0.6165 -0.5809 0.061 Uiso 1 1 calc R . . H39B H 0.5455 0.6700 -0.5237 0.061 Uiso 1 1 calc R . . H39C H 0.4578 0.7448 -0.6085 0.061 Uiso 1 1 calc R . . C40 C 0.2599(4) 0.6492(4) -0.5363(3) 0.0458(12) Uani 1 1 d . . . H40A H 0.1961 0.6307 -0.4940 0.069 Uiso 1 1 calc R . . H40B H 0.2843 0.5934 -0.5636 0.069 Uiso 1 1 calc R . . H40C H 0.2396 0.7195 -0.5902 0.069 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 0.01261(17) 0.01187(16) 0.00962(16) -0.00295(11) 0.00085(10) -0.00118(11) Cl1 0.0219(5) 0.0154(4) 0.0150(4) -0.0056(3) 0.0043(3) -0.0065(4) Cl2 0.0175(5) 0.0182(5) 0.0206(5) -0.0034(4) 0.0008(3) 0.0037(4) P1 0.0128(5) 0.0121(4) 0.0075(4) -0.0034(3) 0.0006(3) -0.0020(3) P2 0.0118(5) 0.0145(5) 0.0115(4) -0.0030(3) -0.0004(3) -0.0019(4) N1 0.0110(15) 0.0175(15) 0.0134(15) -0.0034(12) 0.0000(11) -0.0029(12) O1 0.0256(15) 0.0236(15) 0.0330(16) -0.0110(12) 0.0136(11) -0.0098(12) O2 0.0311(16) 0.0218(14) 0.0229(15) -0.0086(11) 0.0123(11) -0.0020(12) O3 0.0255(15) 0.0265(15) 0.0135(13) -0.0003(11) -0.0002(11) -0.0049(12) O4 0.0247(17) 0.077(2) 0.0118(14) 0.0060(14) -0.0049(11) -0.0050(15) C1 0.0163(18) 0.0105(17) 0.0096(16) -0.0026(13) -0.0005(12) -0.0013(14) C2 0.020(2) 0.0146(18) 0.0144(18) -0.0038(14) -0.0003(14) -0.0001(15) C3 0.037(2) 0.023(2) 0.0152(19) -0.0106(15) -0.0044(15) -0.0038(18) C4 0.029(2) 0.022(2) 0.0175(19) -0.0071(15) -0.0087(15) 0.0006(17) C5 0.0166(19) 0.025(2) 0.0210(19) -0.0088(16) -0.0041(14) 0.0003(16) C6 0.0180(19) 0.0170(18) 0.0122(17) -0.0048(14) 0.0007(13) -0.0029(15) C7 0.0143(18) 0.0150(18) 0.0075(16) -0.0037(13) -0.0007(12) 0.0024(14) C8 0.0149(19) 0.0178(19) 0.0150(18) -0.0060(14) -0.0044(13) 0.0014(15) C9 0.0169(19) 0.023(2) 0.0116(18) 0.0007(14) 0.0008(13) -0.0030(15) C10 0.025(2) 0.028(2) 0.0074(17) -0.0038(15) 0.0013(14) 0.0035(17) C11 0.030(2) 0.023(2) 0.0129(18) -0.0096(15) -0.0030(15) 0.0018(17) C12 0.024(2) 0.0191(19) 0.0128(18) -0.0057(14) -0.0024(14) -0.0010(16) C13 0.0121(18) 0.0185(19) 0.0145(18) -0.0043(14) -0.0010(13) 0.0032(15) C14 0.0170(19) 0.022(2) 0.0166(19) -0.0052(15) -0.0031(14) -0.0035(15) C15 0.019(2) 0.031(2) 0.020(2) -0.0035(16) 0.0026(15) -0.0052(17) C16 0.023(2) 0.034(2) 0.0167(19) -0.0083(16) 0.0037(15) -0.0022(17) C17 0.035(2) 0.030(2) 0.019(2) -0.0145(17) 0.0015(16) -0.0046(18) C18 0.019(2) 0.021(2) 0.0166(19) -0.0054(15) 0.0017(14) -0.0045(16) C19 0.0161(19) 0.0148(18) 0.0130(18) -0.0007(14) -0.0019(13) -0.0038(15) C20 0.017(2) 0.022(2) 0.0209(19) -0.0064(15) -0.0013(14) -0.0028(16) C21 0.0120(19) 0.030(2) 0.023(2) -0.0057(16) -0.0013(14) -0.0004(16) C22 0.027(2) 0.032(2) 0.019(2) -0.0061(16) -0.0101(15) -0.0054(18) C23 0.026(2) 0.026(2) 0.0144(19) -0.0070(15) -0.0063(14) -0.0008(17) C24 0.0169(19) 0.023(2) 0.0173(19) -0.0064(15) -0.0004(14) -0.0014(16) C25 0.0146(18) 0.0140(18) 0.0129(17) -0.0034(13) 0.0002(13) -0.0039(14) C26 0.0145(18) 0.0147(17) 0.0081(16) -0.0023(13) 0.0016(12) -0.0010(14) C27 0.0169(19) 0.0103(17) 0.0132(17) -0.0041(13) -0.0010(13) -0.0015(14) C28 0.0142(18) 0.0132(18) 0.0194(19) -0.0053(14) -0.0006(13) -0.0014(14) C29 0.0186(19) 0.0109(17) 0.0131(18) -0.0052(13) 0.0029(13) -0.0055(14) C30 0.0213(19) 0.0135(17) 0.0091(17) -0.0045(13) -0.0006(13) -0.0024(14) C31 0.0163(19) 0.0191(19) 0.0183(19) -0.0067(15) -0.0032(14) -0.0029(15) C32 0.0171(19) 0.0140(18) 0.0182(19) -0.0067(14) 0.0025(13) -0.0067(14) C33 0.0170(19) 0.017(2) 0.0102(17) -0.0026(14) -0.0024(13) 0.0041(15) C34 0.020(2) 0.0160(18) 0.0168(19) -0.0072(15) -0.0023(15) 0.0003(15) S1 0.0231(5) 0.0286(5) 0.0291(5) -0.0085(4) 0.0002(4) -0.0090(4) O5 0.0299(16) 0.0467(18) 0.0392(17) -0.0173(14) -0.0057(13) -0.0135(14) C35 0.032(3) 0.073(3) 0.033(3) -0.028(2) 0.0015(18) -0.015(2) C36 0.037(3) 0.035(3) 0.038(3) -0.009(2) -0.0077(19) 0.000(2) S2 0.0317(6) 0.0199(5) 0.0163(5) -0.0054(4) -0.0032(4) -0.0019(4) O6 0.0291(16) 0.0404(17) 0.0141(14) 0.0002(11) -0.0024(11) -0.0020(13) C37 0.037(2) 0.021(2) 0.023(2) -0.0089(16) -0.0007(17) -0.0029(18) C38 0.045(3) 0.026(2) 0.020(2) -0.0039(17) -0.0071(17) -0.0040(19) S3 0.0310(6) 0.0311(6) 0.0317(6) -0.0103(5) 0.0039(4) -0.0024(5) O7 0.0285(16) 0.0386(17) 0.0222(15) -0.0004(12) 0.0071(11) 0.0010(13) C39 0.039(3) 0.030(2) 0.039(3) 0.0014(19) 0.0062(19) -0.004(2) C40 0.044(3) 0.040(3) 0.043(3) -0.005(2) -0.012(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 Cl1 2.3505(8) . ? Pd1 Cl2 2.3571(8) . ? Pd1 P1 2.2392(9) . ? Pd1 P2 2.2497(9) . ? P1 C1 1.808(3) . ? P1 C7 1.814(3) . ? P1 C26 1.844(3) . ? P2 C13 1.816(3) . ? P2 C19 1.817(3) . ? P2 C25 1.843(3) . ? N1 C25 1.451(4) . ? N1 C26 1.450(4) . ? N1 C27 1.386(4) . ? O1 C33 1.202(4) . ? O2 H2 0.8400 . ? O2 C33 1.321(4) . ? O3 C34 1.201(4) . ? O4 H4 0.8400 . ? O4 C34 1.323(4) . ? C1 C2 1.385(5) . ? C1 C6 1.405(5) . ? C2 H2A 0.9500 . ? C2 C3 1.387(5) . ? C3 H3 0.9500 . ? C3 C4 1.374(5) . ? C4 H4A 0.9500 . ? C4 C5 1.388(5) . ? C5 H5 0.9500 . ? C5 C6 1.388(5) . ? C6 H6 0.9500 . ? C7 C8 1.388(5) . ? C7 C12 1.393(5) . ? C8 H8 0.9500 . ? C8 C9 1.380(5) . ? C9 H9 0.9500 . ? C9 C10 1.388(5) . ? C10 H10 0.9500 . ? C10 C11 1.371(5) . ? C11 H11 0.9500 . ? C11 C12 1.390(5) . ? C12 H12 0.9500 . ? C13 C14 1.406(5) . ? C13 C18 1.386(5) . ? C14 H14 0.9500 . ? C14 C15 1.380(5) . ? C15 H15 0.9500 . ? C15 C16 1.391(5) . ? C16 H16 0.9500 . ? C16 C17 1.380(5) . ? C17 H17 0.9500 . ? C17 C18 1.398(5) . ? C18 H18 0.9500 . ? C19 C20 1.396(5) . ? C19 C24 1.394(5) . ? C20 H20 0.9500 . ? C20 C21 1.388(5) . ? C21 H21 0.9500 . ? C21 C22 1.378(5) . ? C22 H22 0.9500 . ? C22 C23 1.389(5) . ? C23 H23 0.9500 . ? C23 C24 1.382(5) . ? C24 H24 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.407(5) . ? C27 C32 1.405(5) . ? C28 H28 0.9500 . ? C28 C29 1.389(5) . ? C29 C30 1.402(5) . ? C29 C33 1.514(5) . ? C30 C31 1.394(5) . ? C30 C34 1.479(5) . ? C31 H31 0.9500 . ? C31 C32 1.360(5) . ? C32 H32 0.9500 . ? S1 O5 1.499(3) . ? S1 C35 1.778(4) . ? S1 C36 1.780(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? S2 O6 1.523(3) . ? S2 C37 1.778(4) . ? S2 C38 1.789(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? S3 O7 1.529(3) . ? S3 C39 1.783(4) . ? S3 C40 1.789(5) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Pd1 Cl2 91.64(3) . . ? Cl1 Pd1 P1 85.66(3) . . ? Cl1 Pd1 P2 173.89(3) . . ? Cl2 Pd1 P1 174.47(3) . . ? Cl2 Pd1 P2 86.59(3) . . ? P1 Pd1 P2 96.59(3) . . ? Pd1 P1 C1 114.58(11) . . ? Pd1 P1 C7 111.82(11) . . ? Pd1 P1 C26 116.07(11) . . ? C1 P1 C7 108.02(15) . . ? C1 P1 C26 101.76(15) . . ? C7 P1 C26 103.51(15) . . ? Pd1 P2 C13 111.12(12) . . ? Pd1 P2 C19 112.88(11) . . ? Pd1 P2 C25 117.73(11) . . ? C13 P2 C19 107.24(15) . . ? C13 P2 C25 104.67(15) . . ? C19 P2 C25 102.26(15) . . ? C25 N1 C26 112.7(2) . . ? C25 N1 C27 123.7(3) . . ? C26 N1 C27 123.6(3) . . ? H2 O2 C33 109.5 . . ? H4 O4 C34 109.5 . . ? P1 C1 C2 120.0(3) . . ? P1 C1 C6 119.8(2) . . ? C2 C1 C6 119.5(3) . . ? C1 C2 H2A 119.9 . . ? C1 C2 C3 120.3(3) . . ? H2A C2 C3 119.9 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.2(3) . . ? H3 C3 C4 119.9 . . ? C3 C4 H4A 119.8 . . ? C3 C4 C5 120.5(3) . . ? H4A C4 C5 119.8 . . ? C4 C5 H5 120.1 . . ? C4 C5 C6 119.9(3) . . ? H5 C5 C6 120.1 . . ? C1 C6 C5 119.7(3) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.2 . . ? P1 C7 C8 120.1(2) . . ? P1 C7 C12 120.7(3) . . ? C8 C7 C12 119.1(3) . . ? C7 C8 H8 119.7 . . ? C7 C8 C9 120.6(3) . . ? H8 C8 C9 119.7 . . ? C8 C9 H9 120.0 . . ? C8 C9 C10 120.0(3) . . ? H9 C9 C10 120.0 . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 119.9(3) . . ? H10 C10 C11 120.0 . . ? C10 C11 H11 119.7 . . ? C10 C11 C12 120.5(3) . . ? H11 C11 C12 119.7 . . ? C7 C12 C11 119.9(3) . . ? C7 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? P2 C13 C14 120.3(3) . . ? P2 C13 C18 120.1(3) . . ? C14 C13 C18 119.7(3) . . ? C13 C14 H14 120.1 . . ? C13 C14 C15 119.7(3) . . ? H14 C14 C15 120.1 . . ? C14 C15 H15 119.9 . . ? C14 C15 C16 120.3(4) . . ? H15 C15 C16 119.9 . . ? C15 C16 H16 119.8 . . ? C15 C16 C17 120.4(3) . . ? H16 C16 C17 119.8 . . ? C16 C17 H17 120.2 . . ? C16 C17 C18 119.6(4) . . ? H17 C17 C18 120.2 . . ? C13 C18 C17 120.2(3) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? P2 C19 C20 121.5(3) . . ? P2 C19 C24 119.4(3) . . ? C20 C19 C24 119.0(3) . . ? C19 C20 H20 120.1 . . ? C19 C20 C21 119.7(3) . . ? H20 C20 C21 120.1 . . ? C20 C21 H21 119.6 . . ? C20 C21 C22 120.8(3) . . ? H21 C21 C22 119.6 . . ? C21 C22 H22 120.1 . . ? C21 C22 C23 119.8(3) . . ? H22 C22 C23 120.1 . . ? C22 C23 H23 120.1 . . ? C22 C23 C24 119.8(3) . . ? H23 C23 C24 120.1 . . ? C19 C24 C23 120.8(3) . . ? C19 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? P2 C25 N1 112.8(2) . . ? P2 C25 H25A 109.0 . . ? P2 C25 H25B 109.0 . . ? N1 C25 H25A 109.0 . . ? N1 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? P1 C26 N1 112.8(2) . . ? P1 C26 H26A 109.0 . . ? P1 C26 H26B 109.0 . . ? N1 C26 H26A 109.0 . . ? N1 C26 H26B 109.0 . . ? H26A C26 H26B 107.8 . . ? N1 C27 C28 121.1(3) . . ? N1 C27 C32 121.5(3) . . ? C28 C27 C32 117.5(3) . . ? C27 C28 H28 119.6 . . ? C27 C28 C29 120.9(3) . . ? H28 C28 C29 119.6 . . ? C28 C29 C30 121.1(3) . . ? C28 C29 C33 115.7(3) . . ? C30 C29 C33 122.9(3) . . ? C29 C30 C31 117.0(3) . . ? C29 C30 C34 121.1(3) . . ? C31 C30 C34 121.9(3) . . ? C30 C31 H31 118.6 . . ? C30 C31 C32 122.8(3) . . ? H31 C31 C32 118.6 . . ? C27 C32 C31 120.8(3) . . ? C27 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? O1 C33 O2 124.5(3) . . ? O1 C33 C29 122.3(3) . . ? O2 C33 C29 113.0(3) . . ? O3 C34 O4 122.6(3) . . ? O3 C34 C30 124.5(3) . . ? O4 C34 C30 112.8(3) . . ? O5 S1 C35 106.88(19) . . ? O5 S1 C36 106.6(2) . . ? C35 S1 C36 97.3(2) . . ? S1 C35 H35A 109.5 . . ? S1 C35 H35B 109.5 . . ? S1 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? S1 C36 H36A 109.5 . . ? S1 C36 H36B 109.5 . . ? S1 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O6 S2 C37 105.81(17) . . ? O6 S2 C38 104.02(18) . . ? C37 S2 C38 97.71(19) . . ? S2 C37 H37A 109.5 . . ? S2 C37 H37B 109.5 . . ? S2 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? S2 C38 H38A 109.5 . . ? S2 C38 H38B 109.5 . . ? S2 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O7 S3 C39 104.30(18) . . ? O7 S3 C40 104.26(19) . . ? C39 S3 C40 99.4(2) . . ? S3 C39 H39A 109.5 . . ? S3 C39 H39B 109.5 . . ? S3 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? S3 C40 H40A 109.5 . . ? S3 C40 H40B 109.5 . . ? S3 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Pd1 P1 C1 -60.77(12) . . . . ? Cl1 Pd1 P1 C7 62.56(12) . . . . ? Cl1 Pd1 P1 C26 -179.01(12) . . . . ? Cl2 Pd1 P1 C1 -121.7(3) . . . . ? Cl2 Pd1 P1 C7 1.7(4) . . . . ? Cl2 Pd1 P1 C26 120.1(3) . . . . ? P2 Pd1 P1 C1 113.52(12) . . . . ? P2 Pd1 P1 C7 -123.15(12) . . . . ? P2 Pd1 P1 C26 -4.72(12) . . . . ? Cl1 Pd1 P2 C13 -7.4(3) . . . . ? Cl1 Pd1 P2 C19 -127.9(3) . . . . ? Cl1 Pd1 P2 C25 113.3(3) . . . . ? Cl2 Pd1 P2 C13 65.92(11) . . . . ? Cl2 Pd1 P2 C19 -54.60(13) . . . . ? Cl2 Pd1 P2 C25 -173.43(12) . . . . ? P1 Pd1 P2 C13 -118.62(11) . . . . ? P1 Pd1 P2 C19 120.85(13) . . . . ? P1 Pd1 P2 C25 2.02(12) . . . . ? Pd1 P1 C1 C2 -25.2(3) . . . . ? Pd1 P1 C1 C6 164.6(2) . . . . ? C7 P1 C1 C2 -150.6(3) . . . . ? C7 P1 C1 C6 39.2(3) . . . . ? C26 P1 C1 C2 100.9(3) . . . . ? C26 P1 C1 C6 -69.4(3) . . . . ? P1 C1 C2 C3 -169.6(3) . . . . ? C6 C1 C2 C3 0.7(5) . . . . ? C1 C2 C3 C4 -1.2(5) . . . . ? C2 C3 C4 C5 0.3(6) . . . . ? C3 C4 C5 C6 1.0(5) . . . . ? C4 C5 C6 C1 -1.5(5) . . . . ? P1 C1 C6 C5 170.9(3) . . . . ? C2 C1 C6 C5 0.6(5) . . . . ? Pd1 P1 C7 C8 -90.5(3) . . . . ? Pd1 P1 C7 C12 85.3(3) . . . . ? C1 P1 C7 C8 36.5(3) . . . . ? C1 P1 C7 C12 -147.7(3) . . . . ? C26 P1 C7 C8 143.8(3) . . . . ? C26 P1 C7 C12 -40.3(3) . . . . ? P1 C7 C8 C9 178.0(3) . . . . ? C12 C7 C8 C9 2.1(5) . . . . ? C7 C8 C9 C10 -0.3(5) . . . . ? C8 C9 C10 C11 -1.7(5) . . . . ? C9 C10 C11 C12 1.8(5) . . . . ? C10 C11 C12 C7 0.0(5) . . . . ? P1 C7 C12 C11 -177.9(3) . . . . ? C8 C7 C12 C11 -2.0(5) . . . . ? Pd1 P2 C13 C14 179.4(2) . . . . ? Pd1 P2 C13 C18 0.9(3) . . . . ? C19 P2 C13 C14 -56.8(3) . . . . ? C19 P2 C13 C18 124.7(3) . . . . ? C25 P2 C13 C14 51.4(3) . . . . ? C25 P2 C13 C18 -127.2(3) . . . . ? P2 C13 C14 C15 179.8(3) . . . . ? C18 C13 C14 C15 -1.6(5) . . . . ? C13 C14 C15 C16 0.2(5) . . . . ? C14 C15 C16 C17 1.0(6) . . . . ? C15 C16 C17 C18 -0.6(6) . . . . ? P2 C13 C18 C17 -179.4(3) . . . . ? C14 C13 C18 C17 2.0(5) . . . . ? C16 C17 C18 C13 -0.9(5) . . . . ? Pd1 P2 C19 C20 100.9(3) . . . . ? Pd1 P2 C19 C24 -76.4(3) . . . . ? C13 P2 C19 C20 -21.8(3) . . . . ? C13 P2 C19 C24 160.9(3) . . . . ? C25 P2 C19 C20 -131.6(3) . . . . ? C25 P2 C19 C24 51.0(3) . . . . ? P2 C19 C20 C21 -178.7(3) . . . . ? C24 C19 C20 C21 -1.4(5) . . . . ? C19 C20 C21 C22 0.3(5) . . . . ? C20 C21 C22 C23 0.4(6) . . . . ? C21 C22 C23 C24 -0.1(6) . . . . ? C22 C23 C24 C19 -1.0(5) . . . . ? P2 C19 C24 C23 179.1(3) . . . . ? C20 C19 C24 C23 1.7(5) . . . . ? C26 N1 C25 P2 80.0(3) . . . . ? C27 N1 C25 P2 -102.3(3) . . . . ? Pd1 P2 C25 N1 -33.6(3) . . . . ? C13 P2 C25 N1 90.4(2) . . . . ? C19 P2 C25 N1 -157.9(2) . . . . ? C25 N1 C26 P1 -84.5(3) . . . . ? C27 N1 C26 P1 97.7(3) . . . . ? Pd1 P1 C26 N1 40.3(2) . . . . ? C1 P1 C26 N1 -84.8(2) . . . . ? C7 P1 C26 N1 163.2(2) . . . . ? C25 N1 C27 C28 -1.1(5) . . . . ? C25 N1 C27 C32 -179.4(3) . . . . ? C26 N1 C27 C28 176.4(3) . . . . ? C26 N1 C27 C32 -1.9(5) . . . . ? N1 C27 C28 C29 -176.6(3) . . . . ? C32 C27 C28 C29 1.7(5) . . . . ? C27 C28 C29 C30 -0.3(5) . . . . ? C27 C28 C29 C33 173.8(3) . . . . ? C28 C29 C30 C31 -1.2(5) . . . . ? C28 C29 C30 C34 175.7(3) . . . . ? C33 C29 C30 C31 -174.8(3) . . . . ? C33 C29 C30 C34 2.2(5) . . . . ? C29 C30 C31 C32 1.2(5) . . . . ? C34 C30 C31 C32 -175.7(3) . . . . ? C30 C31 C32 C27 0.3(5) . . . . ? N1 C27 C32 C31 176.6(3) . . . . ? C28 C27 C32 C31 -1.7(5) . . . . ? C28 C29 C33 O1 -86.1(4) . . . . ? C28 C29 C33 O2 89.4(4) . . . . ? C30 C29 C33 O1 87.7(4) . . . . ? C30 C29 C33 O2 -96.8(4) . . . . ? C29 C30 C34 O3 2.7(5) . . . . ? C29 C30 C34 O4 -175.5(3) . . . . ? C31 C30 C34 O3 179.5(3) . . . . ? C31 C30 C34 O4 1.2(5) . . . . ? 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 O2 H2 O7 0.84 1.76 2.604(4) 178.9 . O4 H4 O6 0.84 1.73 2.559(3) 169.5 . _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.649 _refine_diff_density_min -1.022 _refine_diff_density_rms 0.108 # End of data for 4.3DMSO data_2e.2DMSO _database_code_depnum_ccdc_archive 'CCDC 223229' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H41 Cl2 N O5 P2 Pd S2' _chemical_formula_sum 'C37 H41 Cl2 N O5 P2 Pd S2' _chemical_formula_weight 883.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6157(4) _cell_length_b 31.5085(8) _cell_length_c 9.9021(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.629(1) _cell_angle_gamma 90.00 _cell_volume 3928.21(18) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 16510 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.493 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.838 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8502 _exptl_absorpt_correction_T_max 0.9672 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22977 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.1001 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6640 _reflns_number_gt 4372 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6640 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0894 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0188(3) 0.09473(13) 0.5774(4) 0.0204(10) Uani 1 1 d . . . C2 C -0.0757(4) 0.06373(14) 0.5050(5) 0.0282(12) Uani 1 1 d . . . H92 H -0.0623 0.0584 0.4131 0.034 Uiso 1 1 calc R . . C3 C -0.1522(4) 0.04044(15) 0.5669(5) 0.0376(13) Uani 1 1 d . . . H3 H -0.1920 0.0195 0.5169 0.045 Uiso 1 1 calc R . . C4 C -0.1712(4) 0.04767(15) 0.7020(5) 0.0376(13) Uani 1 1 d . . . H4 H -0.2213 0.0308 0.7457 0.045 Uiso 1 1 calc R . . C5 C -0.1170(4) 0.07922(17) 0.7708(5) 0.0449(14) Uani 1 1 d . . . H5 H -0.1313 0.0849 0.8620 0.054 Uiso 1 1 calc R . . C6 C -0.0412(4) 0.10314(15) 0.7094(4) 0.0326(12) Uani 1 1 d . . . H6 H -0.0048 0.1253 0.7582 0.039 Uiso 1 1 calc R . . C7 C 0.1244(3) 0.16896(12) 0.5852(4) 0.0157(10) Uani 1 1 d . . . C8 C 0.0966(4) 0.20680(14) 0.5195(4) 0.0280(12) Uani 1 1 d . . . H8 H 0.0610 0.2060 0.4321 0.034 Uiso 1 1 calc R . . C9 C 0.1200(4) 0.24515(15) 0.5792(5) 0.0335(12) Uani 1 1 d . . . H9 H 0.0998 0.2706 0.5333 0.040 Uiso 1 1 calc R . . C10 C 0.1723(4) 0.24712(14) 0.7043(5) 0.0311(12) Uani 1 1 d . . . H10 H 0.1899 0.2738 0.7442 0.037 Uiso 1 1 calc R . . C11 C 0.1992(4) 0.21021(15) 0.7717(5) 0.0375(13) Uani 1 1 d . . . H11 H 0.2336 0.2113 0.8598 0.045 Uiso 1 1 calc R . . C12 C 0.1760(4) 0.17151(14) 0.7114(4) 0.0314(12) Uani 1 1 d . . . H12 H 0.1962 0.1461 0.7580 0.038 Uiso 1 1 calc R . . C13 C 0.3251(3) 0.14615(12) 0.2026(4) 0.0174(10) Uani 1 1 d . . . C14 C 0.3701(3) 0.17067(13) 0.3077(4) 0.0223(11) Uani 1 1 d . . . H14 H 0.3568 0.1637 0.3984 0.027 Uiso 1 1 calc R . . C15 C 0.4336(3) 0.20472(14) 0.2825(5) 0.0262(11) Uani 1 1 d . . . H15 H 0.4639 0.2212 0.3555 0.031 Uiso 1 1 calc R . . C16 C 0.4533(3) 0.21512(14) 0.1514(5) 0.0307(12) Uani 1 1 d . . . H16 H 0.4973 0.2387 0.1341 0.037 Uiso 1 1 calc R . . C17 C 0.4096(3) 0.19145(14) 0.0456(5) 0.0274(11) Uani 1 1 d . . . H17 H 0.4235 0.1987 -0.0447 0.033 Uiso 1 1 calc R . . C18 C 0.3448(3) 0.15688(13) 0.0703(4) 0.0229(11) Uani 1 1 d . . . H18 H 0.3142 0.1407 -0.0031 0.028 Uiso 1 1 calc R . . C19 C 0.2405(4) 0.06364(13) 0.1076(4) 0.0202(10) Uani 1 1 d . . . C20 C 0.3373(4) 0.04878(14) 0.0647(4) 0.0269(11) Uani 1 1 d . . . H20 H 0.4020 0.0607 0.1014 0.032 Uiso 1 1 calc R . . C21 C 0.3396(4) 0.01684(14) -0.0306(4) 0.0324(12) Uani 1 1 d . . . H21 H 0.4057 0.0067 -0.0587 0.039 Uiso 1 1 calc R . . C22 C 0.2457(4) -0.00037(15) -0.0849(5) 0.0375(13) Uani 1 1 d . . . H22 H 0.2472 -0.0220 -0.1514 0.045 Uiso 1 1 calc R . . C23 C 0.1499(4) 0.01365(15) -0.0432(5) 0.0409(14) Uani 1 1 d . . . H23 H 0.0856 0.0015 -0.0803 0.049 Uiso 1 1 calc R . . C24 C 0.1470(4) 0.04557(13) 0.0529(4) 0.0285(12) Uani 1 1 d . . . H24 H 0.0806 0.0551 0.0815 0.034 Uiso 1 1 calc R . . C25 C 0.3914(3) 0.08604(13) 0.6046(4) 0.0154(10) Uani 1 1 d . . . C26 C 0.4433(3) 0.12095(13) 0.6619(4) 0.0179(10) Uani 1 1 d . . . H26 H 0.4178 0.1487 0.6408 0.021 Uiso 1 1 calc R . . C27 C 0.5326(3) 0.11580(13) 0.7503(4) 0.0211(11) Uani 1 1 d . . . C28 C 0.5690(3) 0.07503(14) 0.7793(4) 0.0226(11) Uani 1 1 d . . . H28 H 0.6300 0.0712 0.8394 0.027 Uiso 1 1 calc R . . C29 C 0.5183(3) 0.04006(14) 0.7224(4) 0.0236(11) Uani 1 1 d . . . H29 H 0.5447 0.0124 0.7423 0.028 Uiso 1 1 calc R . . C30 C 0.4278(3) 0.04551(13) 0.6354(4) 0.0197(10) Uani 1 1 d . . . C31 C 0.5957(4) 0.15196(14) 0.8085(4) 0.0216(11) Uani 1 1 d . . . C32 C 0.1984(3) 0.08287(13) 0.5652(4) 0.0191(10) Uani 1 1 d . . . H32A H 0.2055 0.0845 0.6652 0.023 Uiso 1 1 calc R . . H32B H 0.1782 0.0534 0.5400 0.023 Uiso 1 1 calc R . . C33 C 0.3112(3) 0.07362(13) 0.3783(4) 0.0182(10) Uani 1 1 d . . . H33A H 0.2848 0.0440 0.3800 0.022 Uiso 1 1 calc R . . H33B H 0.3873 0.0727 0.3596 0.022 Uiso 1 1 calc R . . C34 C 0.3610(4) -0.12164(15) 0.8287(5) 0.0392(13) Uani 1 1 d . . . H34A H 0.3587 -0.1052 0.9125 0.059 Uiso 1 1 calc R . . H34B H 0.4317 -0.1342 0.8236 0.059 Uiso 1 1 calc R . . H34C H 0.3076 -0.1442 0.8278 0.059 Uiso 1 1 calc R . . C35 C 0.3402(4) -0.12594(15) 0.5581(5) 0.0419(14) Uani 1 1 d . . . H35A H 0.4104 -0.1394 0.5631 0.063 Uiso 1 1 calc R . . H35B H 0.3280 -0.1117 0.4705 0.063 Uiso 1 1 calc R . . H35C H 0.2855 -0.1476 0.5679 0.063 Uiso 1 1 calc R . . C36 C 0.7914(4) 0.27930(15) 1.0953(4) 0.0388(13) Uani 1 1 d . . . H36A H 0.8252 0.2962 1.0267 0.058 Uiso 1 1 calc R . . H36B H 0.8444 0.2719 1.1682 0.058 Uiso 1 1 calc R . . H36C H 0.7343 0.2958 1.1324 0.058 Uiso 1 1 calc R . . C37 C 0.8588(4) 0.21275(15) 0.9621(5) 0.0346(13) Uani 1 1 d . . . H37A H 0.8443 0.1877 0.9053 0.052 Uiso 1 1 calc R . . H37B H 0.9069 0.2050 1.0397 0.052 Uiso 1 1 calc R . . H37C H 0.8919 0.2348 0.9089 0.052 Uiso 1 1 calc R . . N1 N 0.3004(3) 0.09296(10) 0.5108(3) 0.0159(8) Uani 1 1 d . . . O1 O 0.3733(2) 0.01235(9) 0.5795(3) 0.0266(8) Uani 1 1 d . . . H1 H 0.3965 -0.0103 0.6147 0.040 Uiso 1 1 calc R . . O2 O 0.5566(2) 0.18979(9) 0.7725(3) 0.0263(7) Uani 1 1 d . . . H2 H 0.5902 0.2088 0.8166 0.039 Uiso 1 1 calc R . . O3 O 0.6755(2) 0.14749(9) 0.8807(3) 0.0309(8) Uani 1 1 d . . . O4 O 0.4328(2) -0.06046(9) 0.6827(3) 0.0308(8) Uani 1 1 d . . . O5 O 0.6714(2) 0.24744(9) 0.8970(3) 0.0322(8) Uani 1 1 d . . . P1 P 0.09351(9) 0.11909(3) 0.50156(11) 0.0174(3) Uani 1 1 d . . . P2 P 0.23766(9) 0.10268(3) 0.24114(11) 0.0165(3) Uani 1 1 d . . . Cl1 Cl -0.09311(8) 0.15715(4) 0.30143(11) 0.0282(3) Uani 1 1 d . . . Cl2 Cl 0.06640(9) 0.14247(3) 0.04354(10) 0.0248(3) Uani 1 1 d . . . Pd1 Pd 0.07622(3) 0.127886(10) 0.27627(3) 0.01691(11) Uani 1 1 d . . . S1 S 0.33439(9) -0.08818(4) 0.68984(11) 0.0254(3) Uani 1 1 d . . . S2 S 0.73810(10) 0.23226(4) 1.02029(12) 0.0302(3) 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 C1 0.012(2) 0.020(3) 0.029(3) 0.003(2) 0.003(2) 0.000(2) C2 0.027(3) 0.025(3) 0.034(3) 0.003(2) 0.007(2) -0.003(2) C3 0.023(3) 0.027(3) 0.062(4) 0.001(3) 0.003(3) -0.005(2) C4 0.026(3) 0.030(3) 0.059(4) 0.005(3) 0.022(3) 0.000(2) C5 0.041(3) 0.055(4) 0.042(3) -0.001(3) 0.030(3) -0.009(3) C6 0.030(3) 0.039(3) 0.030(3) -0.004(2) 0.009(2) -0.010(2) C7 0.012(2) 0.022(3) 0.014(2) 0.0016(18) 0.004(2) 0.003(2) C8 0.032(3) 0.027(3) 0.025(3) 0.000(2) -0.004(2) -0.001(2) C9 0.035(3) 0.024(3) 0.042(3) 0.002(2) 0.001(3) 0.003(2) C10 0.030(3) 0.023(3) 0.040(3) -0.015(2) -0.001(3) -0.001(2) C11 0.042(3) 0.033(3) 0.034(3) -0.007(2) -0.018(3) 0.000(3) C12 0.039(3) 0.021(3) 0.032(3) 0.001(2) -0.010(3) 0.003(2) C13 0.015(3) 0.016(2) 0.021(2) 0.0012(19) -0.002(2) 0.005(2) C14 0.021(3) 0.022(3) 0.023(3) 0.005(2) 0.001(2) 0.002(2) C15 0.023(3) 0.022(3) 0.033(3) -0.004(2) 0.002(2) -0.003(2) C16 0.016(3) 0.026(3) 0.051(3) 0.007(2) 0.005(3) -0.005(2) C17 0.023(3) 0.030(3) 0.030(3) 0.009(2) 0.009(2) 0.001(2) C18 0.019(3) 0.025(3) 0.024(3) -0.001(2) -0.002(2) 0.006(2) C19 0.023(3) 0.020(3) 0.018(2) 0.0064(18) 0.007(2) 0.002(2) C20 0.023(3) 0.032(3) 0.026(3) 0.004(2) 0.002(2) 0.001(2) C21 0.033(3) 0.035(3) 0.031(3) -0.001(2) 0.013(3) 0.016(3) C22 0.045(4) 0.031(3) 0.037(3) -0.019(2) 0.007(3) 0.003(3) C23 0.036(3) 0.042(3) 0.044(3) -0.017(3) -0.005(3) -0.001(3) C24 0.021(3) 0.030(3) 0.036(3) -0.013(2) 0.006(2) 0.000(2) C25 0.007(2) 0.023(3) 0.016(2) 0.0048(19) 0.006(2) 0.002(2) C26 0.012(2) 0.025(3) 0.016(2) 0.0033(19) 0.004(2) 0.005(2) C27 0.017(3) 0.026(3) 0.021(2) 0.000(2) 0.008(2) 0.000(2) C28 0.012(2) 0.038(3) 0.018(2) 0.002(2) 0.001(2) 0.003(2) C29 0.021(3) 0.020(3) 0.030(3) 0.006(2) 0.005(2) 0.009(2) C30 0.014(3) 0.023(3) 0.022(3) 0.002(2) 0.003(2) -0.001(2) C31 0.022(3) 0.027(3) 0.018(3) 0.003(2) 0.012(2) 0.001(2) C32 0.017(3) 0.025(3) 0.015(2) -0.0035(18) 0.000(2) 0.000(2) C33 0.013(2) 0.020(3) 0.021(2) 0.0025(19) 0.002(2) 0.003(2) C34 0.037(3) 0.040(3) 0.039(3) 0.012(2) -0.003(3) 0.000(3) C35 0.039(3) 0.045(3) 0.043(3) -0.013(3) 0.018(3) -0.010(3) C36 0.042(3) 0.045(3) 0.030(3) -0.003(2) 0.003(3) 0.000(3) C37 0.026(3) 0.041(3) 0.035(3) -0.002(2) -0.002(2) 0.009(2) N1 0.010(2) 0.023(2) 0.0149(19) 0.0015(15) 0.0005(17) 0.0022(16) O1 0.0281(19) 0.0164(18) 0.0339(19) 0.0022(14) -0.0079(16) 0.0008(15) O2 0.0223(19) 0.0252(19) 0.0312(19) -0.0034(14) -0.0003(15) -0.0003(15) O3 0.026(2) 0.0325(19) 0.0331(19) 0.0010(15) -0.0113(17) 0.0016(16) O4 0.0237(19) 0.0209(18) 0.048(2) 0.0054(15) 0.0009(16) -0.0042(15) O5 0.0233(19) 0.0298(19) 0.042(2) 0.0013(14) -0.0107(16) 0.0054(15) P1 0.0119(6) 0.0215(7) 0.0191(6) -0.0005(5) 0.0025(5) 0.0005(5) P2 0.0129(6) 0.0183(6) 0.0184(6) 0.0006(5) 0.0022(5) 0.0008(5) Cl1 0.0149(6) 0.0411(8) 0.0287(6) 0.0020(5) 0.0024(5) 0.0080(5) Cl2 0.0248(7) 0.0308(7) 0.0186(6) 0.0007(5) -0.0005(5) 0.0046(5) Pd1 0.01223(19) 0.0207(2) 0.01773(18) -0.00057(14) 0.00071(15) 0.00157(16) S1 0.0203(7) 0.0276(7) 0.0284(7) 0.0011(5) 0.0028(6) 0.0012(5) S2 0.0257(7) 0.0335(8) 0.0314(7) 0.0023(5) 0.0029(6) -0.0022(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.385(6) . ? C1 C6 1.381(6) . ? C1 P1 1.815(4) . ? C2 H92 0.9500 . ? C2 C3 1.387(6) . ? C3 H3 0.9500 . ? C3 C4 1.392(7) . ? C4 H4 0.9500 . ? C4 C5 1.364(7) . ? C5 H5 0.9500 . ? C5 C6 1.387(6) . ? C6 H6 0.9500 . ? C7 C8 1.393(5) . ? C7 C12 1.374(5) . ? C7 P1 1.807(4) . ? C8 H8 0.9500 . ? C8 C9 1.369(6) . ? C9 H9 0.9500 . ? C9 C10 1.367(6) . ? C10 H10 0.9500 . ? C10 C11 1.373(6) . ? C11 H11 0.9500 . ? C11 C12 1.381(6) . ? C12 H12 0.9500 . ? C13 C14 1.388(5) . ? C13 C18 1.391(6) . ? C13 P2 1.814(4) . ? C14 H14 0.9500 . ? C14 C15 1.371(6) . ? C15 H15 0.9500 . ? C15 C16 1.377(6) . ? C16 H16 0.9500 . ? C16 C17 1.373(6) . ? C17 H17 0.9500 . ? C17 C18 1.392(6) . ? C18 H18 0.9500 . ? C19 C20 1.399(6) . ? C19 C24 1.388(6) . ? C19 P2 1.808(4) . ? C20 H20 0.9500 . ? C20 C21 1.381(6) . ? C21 H21 0.9500 . ? C21 C22 1.381(6) . ? C22 H22 0.9500 . ? C22 C23 1.373(6) . ? C23 H23 0.9500 . ? C23 C24 1.387(6) . ? C24 H24 0.9500 . ? C25 C26 1.383(5) . ? C25 C30 1.384(5) . ? C25 N1 1.447(5) . ? C26 H26 0.9500 . ? C26 C27 1.391(5) . ? C27 C28 1.388(6) . ? C27 C31 1.485(6) . ? C28 H28 0.9500 . ? C28 C29 1.377(6) . ? C29 H29 0.9500 . ? C29 C30 1.397(5) . ? C30 O1 1.350(5) . ? C31 O2 1.330(5) . ? C31 O3 1.206(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 N1 1.461(5) . ? C32 P1 1.829(4) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 N1 1.461(5) . ? C33 P2 1.840(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34 S1 1.748(4) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C35 S1 1.770(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C36 S2 1.771(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C37 S2 1.772(4) . ? O1 H1 0.8400 . ? O2 H2 0.8400 . ? O4 S1 1.523(3) . ? O5 S2 1.516(3) . ? P1 Pd1 2.2449(11) . ? P2 Pd1 2.2337(12) . ? Cl1 Pd1 2.3544(11) . ? Cl2 Pd1 2.3454(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.7(4) . . ? C2 C1 P1 118.4(3) . . ? C6 C1 P1 121.5(3) . . ? C1 C2 H92 120.1 . . ? C1 C2 C3 119.8(4) . . ? H92 C2 C3 120.1 . . ? C2 C3 H3 119.8 . . ? C2 C3 C4 120.4(4) . . ? H3 C3 C4 119.8 . . ? C3 C4 H4 120.4 . . ? C3 C4 C5 119.2(5) . . ? H4 C4 C5 120.4 . . ? C4 C5 H5 119.5 . . ? C4 C5 C6 121.0(5) . . ? H5 C5 C6 119.5 . . ? C1 C6 C5 119.9(4) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C8 C7 C12 117.7(4) . . ? C8 C7 P1 119.3(3) . . ? C12 C7 P1 122.9(3) . . ? C7 C8 H8 119.6 . . ? C7 C8 C9 120.8(4) . . ? H8 C8 C9 119.6 . . ? C8 C9 H9 119.7 . . ? C8 C9 C10 120.7(4) . . ? H9 C9 C10 119.7 . . ? C9 C10 H10 120.2 . . ? C9 C10 C11 119.5(4) . . ? H10 C10 C11 120.2 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.9(4) . . ? H11 C11 C12 120.1 . . ? C7 C12 C11 121.3(4) . . ? C7 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C14 C13 C18 118.8(4) . . ? C14 C13 P2 119.2(3) . . ? C18 C13 P2 121.9(3) . . ? C13 C14 H14 119.5 . . ? C13 C14 C15 121.0(4) . . ? H14 C14 C15 119.5 . . ? C14 C15 H15 120.0 . . ? C14 C15 C16 120.0(4) . . ? H15 C15 C16 120.0 . . ? C15 C16 H16 119.9 . . ? C15 C16 C17 120.1(4) . . ? H16 C16 C17 119.9 . . ? C16 C17 H17 119.9 . . ? C16 C17 C18 120.2(4) . . ? H17 C17 C18 119.9 . . ? C13 C18 C17 119.8(4) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C20 C19 C24 118.7(4) . . ? C20 C19 P2 120.5(3) . . ? C24 C19 P2 120.6(3) . . ? C19 C20 H20 119.7 . . ? C19 C20 C21 120.5(4) . . ? H20 C20 C21 119.7 . . ? C20 C21 H21 120.1 . . ? C20 C21 C22 119.8(4) . . ? H21 C21 C22 120.1 . . ? C21 C22 H22 119.8 . . ? C21 C22 C23 120.4(4) . . ? H22 C22 C23 119.8 . . ? C22 C23 H23 120.0 . . ? C22 C23 C24 120.1(5) . . ? H23 C23 C24 120.0 . . ? C19 C24 C23 120.4(4) . . ? C19 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C30 120.1(4) . . ? C26 C25 N1 118.6(4) . . ? C30 C25 N1 121.3(4) . . ? C25 C26 H26 119.7 . . ? C25 C26 C27 120.6(4) . . ? H26 C26 C27 119.7 . . ? C26 C27 C28 118.8(4) . . ? C26 C27 C31 123.2(4) . . ? C28 C27 C31 117.8(4) . . ? C27 C28 H28 119.4 . . ? C27 C28 C29 121.1(4) . . ? H28 C28 C29 119.4 . . ? C28 C29 H29 120.2 . . ? C28 C29 C30 119.6(4) . . ? H29 C29 C30 120.2 . . ? C25 C30 C29 119.7(4) . . ? C25 C30 O1 118.1(4) . . ? C29 C30 O1 122.2(4) . . ? C27 C31 O2 113.7(4) . . ? C27 C31 O3 123.2(4) . . ? O2 C31 O3 123.1(4) . . ? H32A C32 H32B 107.9 . . ? H32A C32 N1 109.2 . . ? H32A C32 P1 109.2 . . ? H32B C32 N1 109.2 . . ? H32B C32 P1 109.2 . . ? N1 C32 P1 111.8(3) . . ? H33A C33 H33B 107.8 . . ? H33A C33 N1 109.1 . . ? H33A C33 P2 109.1 . . ? H33B C33 N1 109.1 . . ? H33B C33 P2 109.1 . . ? N1 C33 P2 112.6(3) . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34A C34 S1 109.5 . . ? H34B C34 H34C 109.5 . . ? H34B C34 S1 109.5 . . ? H34C C34 S1 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35A C35 S1 109.5 . . ? H35B C35 H35C 109.5 . . ? H35B C35 S1 109.5 . . ? H35C C35 S1 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36A C36 S2 109.5 . . ? H36B C36 H36C 109.5 . . ? H36B C36 S2 109.5 . . ? H36C C36 S2 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37A C37 S2 109.5 . . ? H37B C37 H37C 109.5 . . ? H37B C37 S2 109.5 . . ? H37C C37 S2 109.5 . . ? C25 N1 C32 114.4(3) . . ? C25 N1 C33 113.5(3) . . ? C32 N1 C33 112.0(3) . . ? C30 O1 H1 109.5 . . ? C31 O2 H2 109.5 . . ? C1 P1 C7 109.24(19) . . ? C1 P1 C32 99.21(19) . . ? C1 P1 Pd1 115.72(14) . . ? C7 P1 C32 104.74(18) . . ? C7 P1 Pd1 110.65(13) . . ? C32 P1 Pd1 116.23(14) . . ? C13 P2 C19 108.63(19) . . ? C13 P2 C33 104.26(19) . . ? C13 P2 Pd1 109.69(13) . . ? C19 P2 C33 99.73(18) . . ? C19 P2 Pd1 114.60(15) . . ? C33 P2 Pd1 118.94(14) . . ? P1 Pd1 P2 94.51(4) . . ? P1 Pd1 Cl1 88.56(4) . . ? P1 Pd1 Cl2 175.11(4) . . ? P2 Pd1 Cl1 176.45(4) . . ? P2 Pd1 Cl2 84.76(4) . . ? Cl1 Pd1 Cl2 92.03(4) . . ? C34 S1 C35 99.2(2) . . ? C34 S1 O4 105.4(2) . . ? C35 S1 O4 106.2(2) . . ? C36 S2 C37 96.6(2) . . ? C36 S2 O5 104.5(2) . . ? C37 S2 O5 107.0(2) . . ? 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 O2 H2 O5 0.84 1.75 2.586(4) 173.8 . O1 H1 O4 0.84 1.77 2.603(4) 174.1 . _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.508 _refine_diff_density_min -0.619 _refine_diff_density_rms 0.099 # End of data for 2e.2DMSO data_2a.DMSO _database_code_depnum_ccdc_archive 'CCDC 617764' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H35 Cl2 N O4 P2 Pd S' _chemical_formula_sum 'C35 H35 Cl2 N O4 P2 Pd S' _chemical_formula_weight 804.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n m a' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 19.631(4) _cell_length_b 17.047(3) _cell_length_c 10.506(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3515.7(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.869 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8592 _exptl_absorpt_correction_T_max 0.9661 _exptl_absorpt_process_details 'SORTAV Blessing (1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21715 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3563 _reflns_number_gt 2572 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL and local programs' _computing_publication_material Diamond _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^)+(0.1222P)^2^+22.4164P] 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 3563 _refine_ls_number_parameters 212 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2292 _refine_ls_wR_factor_gt 0.2041 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2954(4) 0.1783(4) 0.6801(7) 0.0404(18) Uani 1 1 d . . . H1A H 0.3389 0.1853 0.6338 0.048 Uiso 1 1 calc R . . H1B H 0.2702 0.1347 0.6393 0.048 Uiso 1 1 calc R . . N1 N 0.2554(4) 0.2500 0.6699(8) 0.0303(18) Uani 1 2 d S . . C2 C 0.1965(7) 0.2500 0.5888(10) 0.0648(19) Uani 1 2 d SDU . . C3 C 0.1281(6) 0.2500 0.6620(13) 0.069(2) Uani 1 2 d SDU . . C4 C 0.0697(6) 0.2500 0.5922(14) 0.072(2) Uani 1 2 d SDU . . H4 H 0.0265 0.2500 0.6331 0.086 Uiso 1 2 calc SR . . C5 C 0.0741(7) 0.2500 0.4616(11) 0.072(2) Uani 1 2 d SDU . . H5 H 0.0318 0.2500 0.4177 0.086 Uiso 1 2 calc SR . . C6 C 0.1311(6) 0.2500 0.3857(13) 0.072(2) Uani 1 2 d SDU . . H6 H 0.1269 0.2500 0.2957 0.086 Uiso 1 2 calc SR . . C7 C 0.1936(6) 0.2500 0.4417(13) 0.0708(19) Uani 1 2 d SDU . . O1 O 0.1337(6) 0.2500 0.7859(12) 0.101(3) Uani 1 2 d SU . . H1 H 0.0946 0.2500 0.8185 0.152 Uiso 1 2 d SR . . C8 C 0.2570(6) 0.2500 0.4089(10) 0.070(2) Uani 1 2 d SDU . . O2 O 0.3148(5) 0.2627(7) 0.4256(9) 0.043(3) Uani 0.50 1 d PDU . . O3 O 0.2493(8) 0.2098(7) 0.2997(13) 0.097(4) Uani 0.50 1 d PDU . . H3 H 0.2822 0.1927 0.2565 0.145 Uiso 0.50 1 d PRD . . C9 C 0.2406(2) 0.0973(3) 0.9006(5) 0.0393(17) Uani 1 1 d G . . C10 C 0.2204(3) 0.0297(3) 0.8369(5) 0.055(2) Uani 1 1 d G . . H10 H 0.2434 0.0140 0.7615 0.066 Uiso 1 1 calc R . . C11 C 0.1666(3) -0.0149(3) 0.8835(6) 0.064(3) Uani 1 1 d G . . H11 H 0.1529 -0.0611 0.8400 0.077 Uiso 1 1 calc R . . C12 C 0.1330(3) 0.0080(3) 0.9939(6) 0.066(3) Uani 1 1 d G . . H12 H 0.0963 -0.0224 1.0257 0.079 Uiso 1 1 calc R . . C13 C 0.1532(3) 0.0756(3) 1.0576(5) 0.057(2) Uani 1 1 d G . . H13 H 0.1302 0.0914 1.1330 0.068 Uiso 1 1 calc R . . C14 C 0.2069(3) 0.1203(3) 1.0109(5) 0.0459(19) Uani 1 1 d G . . H14 H 0.2207 0.1664 1.0545 0.055 Uiso 1 1 calc R . . C15 C 0.3862(2) 0.0862(3) 0.8295(6) 0.047(2) Uani 1 1 d G . . C16 C 0.3883(3) 0.0120(3) 0.8842(5) 0.057(2) Uani 1 1 d G . . H16 H 0.3495 -0.0079 0.9276 0.069 Uiso 1 1 calc R . . C17 C 0.4471(3) -0.0331(3) 0.8752(6) 0.066(3) Uani 1 1 d G . . H17 H 0.4486 -0.0838 0.9126 0.079 Uiso 1 1 calc R . . C18 C 0.5038(3) -0.0039(4) 0.8116(6) 0.069(3) Uani 1 1 d G . . H18 H 0.5440 -0.0347 0.8055 0.083 Uiso 1 1 calc R . . C19 C 0.5017(2) 0.0703(4) 0.7570(6) 0.070(3) Uani 1 1 d G . . H19 H 0.5404 0.0902 0.7135 0.084 Uiso 1 1 calc R . . C20 C 0.4429(3) 0.1154(3) 0.7659(6) 0.057(2) Uani 1 1 d G . . H20 H 0.4414 0.1661 0.7286 0.069 Uiso 1 1 calc R . . P1 P 0.31338(10) 0.15279(11) 0.84566(19) 0.0347(5) Uani 1 1 d . . . Cl1 Cl 0.37061(13) 0.15288(12) 1.1261(2) 0.0607(7) Uani 1 1 d . . . Pd1 Pd 0.34158(4) 0.2500 0.97860(8) 0.0348(3) Uani 1 2 d S . . S1 S 0.02497(17) 0.2500 1.0408(3) 0.0534(8) Uani 1 2 d S . . O4 O 0.0136(6) 0.2500 0.9046(10) 0.087(3) Uani 1 2 d S . . C21 C -0.0224(5) 0.1726(6) 1.1028(12) 0.072(3) Uani 1 1 d . . . H21A H -0.0093 0.1237 1.0601 0.107 Uiso 1 1 calc R . . H21B H -0.0710 0.1825 1.0891 0.107 Uiso 1 1 calc R . . H21C H -0.0134 0.1679 1.1943 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.050(4) 0.038(4) 0.033(4) -0.003(3) -0.009(3) 0.010(3) N1 0.036(4) 0.025(4) 0.030(4) 0.000 -0.005(3) 0.000 C2 0.059(3) 0.062(5) 0.074(4) 0.000 -0.014(3) 0.000 C3 0.057(3) 0.074(5) 0.077(4) 0.000 -0.015(3) 0.000 C4 0.058(3) 0.077(5) 0.081(4) 0.000 -0.014(3) 0.000 C5 0.061(3) 0.078(5) 0.078(4) 0.000 -0.016(3) 0.000 C6 0.059(3) 0.078(5) 0.079(4) 0.000 -0.017(3) 0.000 C7 0.059(3) 0.076(5) 0.078(4) 0.000 -0.015(3) 0.000 O1 0.065(5) 0.164(8) 0.075(4) 0.000 -0.008(3) 0.000 C8 0.060(3) 0.077(5) 0.074(4) 0.000 -0.015(3) 0.000 O2 0.055(3) 0.025(9) 0.049(5) 0.007(4) 0.004(4) 0.006(4) O3 0.081(6) 0.114(9) 0.094(7) -0.029(5) -0.006(5) -0.016(6) C9 0.047(4) 0.031(4) 0.040(4) -0.002(3) -0.006(3) -0.001(3) C10 0.065(6) 0.036(4) 0.065(6) -0.010(4) -0.003(5) -0.006(4) C11 0.080(7) 0.046(5) 0.065(7) -0.008(5) -0.007(5) -0.020(5) C12 0.061(6) 0.054(6) 0.081(7) 0.019(5) -0.016(5) -0.022(5) C13 0.060(5) 0.052(5) 0.058(6) 0.005(5) -0.001(4) -0.004(4) C14 0.056(5) 0.031(4) 0.051(5) -0.004(3) -0.002(4) -0.001(4) C15 0.055(5) 0.039(4) 0.046(5) -0.009(4) -0.015(4) 0.017(4) C16 0.077(6) 0.040(5) 0.056(6) -0.001(4) -0.021(5) 0.016(4) C17 0.101(8) 0.041(5) 0.056(6) -0.010(4) -0.029(6) 0.020(5) C18 0.072(7) 0.073(7) 0.062(7) -0.023(5) -0.021(5) 0.025(6) C19 0.057(6) 0.089(8) 0.063(6) -0.016(6) -0.004(5) 0.028(5) C20 0.051(5) 0.058(5) 0.063(6) -0.008(5) -0.008(4) 0.016(4) P1 0.0417(11) 0.0269(9) 0.0356(10) -0.0020(8) -0.0084(8) 0.0073(8) Cl1 0.0878(17) 0.0422(12) 0.0522(13) 0.0060(10) -0.0281(12) 0.0175(11) Pd1 0.0407(5) 0.0269(4) 0.0369(5) 0.000 -0.0127(3) 0.000 S1 0.0518(18) 0.0450(17) 0.063(2) 0.000 0.0154(15) 0.000 O4 0.086(8) 0.126(10) 0.049(6) 0.000 0.016(5) 0.000 C21 0.057(6) 0.052(5) 0.106(9) 0.028(6) 0.003(6) -0.002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.456(8) . ? C1 P1 1.828(7) . ? N1 C1 1.456(8) 7_565 ? N1 C2 1.437(16) . ? C2 C3 1.547(13) . ? C2 C7 1.546(13) . ? C3 C4 1.361(14) . ? C3 O1 1.306(17) . ? C4 C5 1.374(13) . ? C5 C6 1.374(13) . ? C6 C7 1.362(14) . ? C7 C8 1.290(17) . ? C8 O2 1.170(9) . ? C8 O2 1.170(9) 7_565 ? C8 O3 1.345(9) . ? C8 O3 1.345(9) 7_565 ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C9 P1 1.809(4) . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C13 C14 1.3900 . ? C15 C16 1.3900 . ? C15 C20 1.3900 . ? C15 P1 1.833(4) . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C19 C20 1.3900 . ? P1 Pd1 2.2368(19) . ? Cl1 Pd1 2.338(2) . ? Pd1 P1 2.2368(19) 7_565 ? Pd1 Cl1 2.338(2) 7_565 ? S1 O4 1.448(11) . ? S1 C21 1.741(9) . ? S1 C21 1.741(9) 7_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 P1 112.0(5) . . ? C1 N1 C1 114.1(8) . 7_565 ? C1 N1 C2 118.5(4) . . ? C1 N1 C2 118.5(4) 7_565 . ? N1 C2 C3 113.8(8) . . ? N1 C2 C7 128.5(9) . . ? C3 C2 C7 117.8(12) . . ? C2 C3 C4 117.6(11) . . ? C2 C3 O1 115.0(11) . . ? C4 C3 O1 127.4(13) . . ? C3 C4 C5 119.0(12) . . ? C4 C5 C6 129.1(15) . . ? C5 C6 C7 119.0(12) . . ? C2 C7 C6 117.6(11) . . ? C2 C7 C8 103.4(10) . . ? C6 C7 C8 138.9(12) . . ? C7 C8 O2 153.6(12) . . ? C7 C8 O2 153.6(12) . 7_565 ? C7 C8 O3 96.9(10) . . ? C7 C8 O3 96.9(10) . 7_565 ? O2 C8 O2 21.4(13) . 7_565 ? O2 C8 O3 109.3(13) . . ? O2 C8 O3 98.1(11) 7_565 . ? O2 C8 O3 98.1(11) . 7_565 ? O2 C8 O3 109.3(13) 7_565 7_565 ? O3 C8 O3 61.3(12) . 7_565 ? C10 C9 C14 120.0 . . ? C10 C9 P1 120.3(3) . . ? C14 C9 P1 119.6(3) . . ? C9 C10 C11 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C13 C14 120.0 . . ? C9 C14 C13 120.0 . . ? C16 C15 C20 120.0 . . ? C16 C15 P1 123.3(3) . . ? C20 C15 P1 116.6(3) . . ? C15 C16 C17 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C19 120.0 . . ? C18 C19 C20 120.0 . . ? C15 C20 C19 120.0 . . ? C1 P1 C9 106.0(3) . . ? C1 P1 C15 102.1(3) . . ? C1 P1 Pd1 117.7(3) . . ? C9 P1 C15 108.8(3) . . ? C9 P1 Pd1 112.57(18) . . ? C15 P1 Pd1 108.9(2) . . ? P1 Pd1 P1 95.61(10) . 7_565 ? P1 Pd1 Cl1 87.11(8) . . ? P1 Pd1 Cl1 177.10(8) . 7_565 ? P1 Pd1 Cl1 87.11(8) 7_565 7_565 ? P1 Pd1 Cl1 177.10(8) 7_565 . ? Cl1 Pd1 Cl1 90.16(11) . 7_565 ? O4 S1 C21 106.8(5) . . ? O4 S1 C21 106.8(5) . 7_565 ? C21 S1 C21 98.6(7) . 7_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C1 N1 C1 81.4(9) . . . 7_565 ? P1 C1 N1 C2 -131.7(7) . . . . ? C1 N1 C2 C3 107.3(7) . . . . ? C1 N1 C2 C3 -107.3(7) 7_565 . . . ? C1 N1 C2 C7 -72.7(7) . . . . ? C1 N1 C2 C7 72.7(7) 7_565 . . . ? N1 C2 C3 C4 180.000(2) . . . . ? N1 C2 C3 O1 0.000(2) . . . . ? C7 C2 C3 C4 0.000(2) . . . . ? C7 C2 C3 O1 180.000(2) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? O1 C3 C4 C5 180.000(2) . . . . ? C3 C4 C5 C6 0.000(3) . . . . ? C4 C5 C6 C7 0.000(2) . . . . ? C5 C6 C7 C2 0.000(2) . . . . ? C5 C6 C7 C8 180.000(1) . . . . ? N1 C2 C7 C6 180.000(2) . . . . ? N1 C2 C7 C8 0.000(2) . . . . ? C3 C2 C7 C6 0.000(2) . . . . ? C3 C2 C7 C8 180.000(2) . . . . ? C2 C7 C8 O2 -24.7(9) . . . . ? C2 C7 C8 O2 24.7(9) . . . 7_565 ? C2 C7 C8 O3 149.1(6) . . . . ? C2 C7 C8 O3 -149.1(6) . . . 7_565 ? C6 C7 C8 O2 155.3(9) . . . . ? C6 C7 C8 O2 -155.3(9) . . . 7_565 ? C6 C7 C8 O3 -30.9(6) . . . . ? C6 C7 C8 O3 30.9(6) . . . 7_565 ? C14 C9 C10 C11 0.0 . . . . ? P1 C9 C10 C11 176.6(4) . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C14 0.0 . . . . ? C12 C13 C14 C9 0.0 . . . . ? C10 C9 C14 C13 0.0 . . . . ? P1 C9 C14 C13 -176.7(4) . . . . ? C20 C15 C16 C17 0.0 . . . . ? P1 C15 C16 C17 -175.5(4) . . . . ? C15 C16 C17 C18 0.0 . . . . ? C16 C17 C18 C19 0.0 . . . . ? C17 C18 C19 C20 0.0 . . . . ? C18 C19 C20 C15 0.0 . . . . ? C16 C15 C20 C19 0.0 . . . . ? P1 C15 C20 C19 175.8(4) . . . . ? C10 C9 P1 C1 56.8(4) . . . . ? C10 C9 P1 C15 -52.4(4) . . . . ? C10 C9 P1 Pd1 -173.2(3) . . . . ? C14 C9 P1 C1 -126.6(4) . . . . ? C14 C9 P1 C15 124.2(4) . . . . ? C14 C9 P1 Pd1 3.5(4) . . . . ? N1 C1 P1 C9 85.7(6) . . . . ? N1 C1 P1 C15 -160.5(5) . . . . ? N1 C1 P1 Pd1 -41.3(7) . . . . ? C16 C15 P1 C1 -127.8(4) . . . . ? C16 C15 P1 C9 -16.0(4) . . . . ? C16 C15 P1 Pd1 107.0(3) . . . . ? C20 C15 P1 C1 56.6(4) . . . . ? C20 C15 P1 C9 168.3(3) . . . . ? C20 C15 P1 Pd1 -68.7(3) . . . . ? C1 P1 Pd1 P1 11.1(3) . . . 7_565 ? C1 P1 Pd1 Cl1 -169.9(3) . . . . ? C1 P1 Pd1 Cl1 170.8(17) . . . 7_565 ? C9 P1 Pd1 P1 -112.6(2) . . . 7_565 ? C9 P1 Pd1 Cl1 66.3(2) . . . . ? C9 P1 Pd1 Cl1 47.0(18) . . . 7_565 ? C15 P1 Pd1 P1 126.7(2) . . . 7_565 ? C15 P1 Pd1 Cl1 -54.3(2) . . . . ? C15 P1 Pd1 Cl1 -73.7(18) . . . 7_565 ? 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 H1 O4 0.84 1.83 2.666(16) 174.4 . O3 H3 Cl1 0.84 2.31 3.152(16) 175.7 1_554 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.098 _refine_diff_density_min -2.056 _refine_diff_density_rms 0.159 # End of data for 2a.DMSO # End of cif