# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Garcia-Fernandez, E.' 'Garcia-Seijo, I.' 'Gould, Roberts O.' 'Habtemariam, A.' 'Parsons, S.' _publ_contact_author_name 'Dr E Garcia-Fernandez' _publ_contact_author_address ; Dept of Inorganic Chemistry Overseas University of Santiago de Compostel Santiago de Compostela E 15782 SPAIN ; _publ_contact_author_email 'QIEGQ@USC.ES' _publ_section_title ; Reactivity of a cationic aminophosphine palladium(II) complex : chloro substitutions and formation of neutral digold(I) compounds. The X-ray crystal structure of Au2(Ph2P(CH2)2N(NO)(CH2)2PPh2Cl2 ; #CIF file of [Pd(PNHP)(NO3)](NO3).H2O.CH3OH (4.H2O.CH3OH ) data_pdpni3 _database_code_CSD 181546 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Pd(NO3)(PNHP)]NO3.H2O.MeOH' _chemical_formula_sum 'C29 H35 N3 O8 P2 Pd' _chemical_formula_weight 721.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.044(5) _cell_length_b 12.719(5) _cell_length_c 15.492(7) _cell_angle_alpha 76.89(3) _cell_angle_beta 82.59(4) _cell_angle_gamma 89.47(4) _cell_volume 1530.6(13) _cell_formula_units_Z 2 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description tablet _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 6.343 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_correction_T_min 0.095 _exptl_absorpt_correction_T_max 0.407 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% -2 _diffrn_reflns_number 6923 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 70.25 _reflns_number_total 5034 _reflns_number_gt 3999 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _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^)+(0.1262P)^2^+4.9975P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric, not placed on H2O' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5034 _refine_ls_number_parameters 376 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0887 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.2161 _refine_ls_wR_factor_gt 0.1990 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.90718(7) 0.34830(4) 0.74508(4) 0.0387(2) Uani 1 1 d . . . N1 N 0.5900(13) 0.3861(7) 0.6864(8) 0.070(3) Uani 1 1 d . . . O1 O 0.7517(8) 0.3983(5) 0.6501(4) 0.0519(15) Uani 1 1 d . . . O2 O 0.5554(10) 0.3455(7) 0.7641(7) 0.076(2) Uani 1 1 d . . . O3 O 0.4890(13) 0.4191(9) 0.6338(8) 0.106(3) Uani 1 1 d . . . P1 P 0.9145(3) 0.51126(15) 0.78647(14) 0.0401(5) Uani 1 1 d . . . C11 C 0.7243(11) 0.5708(6) 0.8258(6) 0.0442(19) Uani 1 1 d . . . C12 C 0.6908(15) 0.5882(9) 0.9110(8) 0.068(3) Uani 1 1 d . . . H12 H 0.7682 0.5673 0.9520 0.081 Uiso 1 1 calc R . . C13 C 0.5418(16) 0.6368(11) 0.9361(9) 0.080(4) Uani 1 1 d . . . H13 H 0.5213 0.6520 0.9931 0.096 Uiso 1 1 calc R . . C14 C 0.4276(15) 0.6618(8) 0.8791(11) 0.086(4) Uani 1 1 d . . . H14 H 0.3250 0.6912 0.8973 0.103 Uiso 1 1 calc R . . C15 C 0.4605(15) 0.6445(8) 0.7936(10) 0.075(3) Uani 1 1 d . . . H15 H 0.3822 0.6649 0.7531 0.090 Uiso 1 1 calc R . . C16 C 0.6065(13) 0.5981(7) 0.7681(8) 0.060(3) Uani 1 1 d . . . H16 H 0.6267 0.5845 0.7106 0.073 Uiso 1 1 calc R . . C21 C 1.0285(11) 0.6176(7) 0.7018(6) 0.0438(18) Uani 1 1 d . . . C22 C 1.0402(12) 0.7204(7) 0.7170(6) 0.050(2) Uani 1 1 d . . . H22 H 0.9812 0.7372 0.7684 0.059 Uiso 1 1 calc R . . C23 C 1.1384(13) 0.7969(8) 0.6563(7) 0.059(2) Uani 1 1 d . . . H23 H 1.1556 0.8647 0.6687 0.071 Uiso 1 1 calc R . . C24 C 1.2127(14) 0.7752(9) 0.5769(8) 0.067(3) Uani 1 1 d . . . H24 H 1.2731 0.8299 0.5334 0.081 Uiso 1 1 calc R . . C25 C 1.1985(18) 0.6746(9) 0.5617(8) 0.083(4) Uani 1 1 d . . . H25 H 1.2520 0.6593 0.5085 0.099 Uiso 1 1 calc R . . C26 C 1.1058(16) 0.5953(9) 0.6242(7) 0.070(3) Uani 1 1 d . . . H26 H 1.0956 0.5260 0.6135 0.084 Uiso 1 1 calc R . . C2 C 1.0448(11) 0.4769(6) 0.8766(6) 0.0428(18) Uani 1 1 d . . . H2A H 1.1051 0.5411 0.8823 0.051 Uiso 1 1 calc R . . H2B H 0.9757 0.4466 0.9336 0.051 Uiso 1 1 calc R . . C3 C 1.1660(12) 0.3948(7) 0.8517(6) 0.049(2) Uani 1 1 d . . . H3A H 1.2419 0.4281 0.7979 0.059 Uiso 1 1 calc R . . H3B H 1.2335 0.3685 0.9003 0.059 Uiso 1 1 calc R . . N4 N 1.0705(8) 0.3025(5) 0.8347(5) 0.0398(14) Uani 1 1 d . . . H4 H 1.0055 0.2733 0.8881 0.048 Uiso 1 1 calc R . . C5 C 1.1866(12) 0.2148(7) 0.8168(6) 0.048(2) Uani 1 1 d . . . H5A H 1.2478 0.1885 0.8680 0.058 Uiso 1 1 calc R . . H5B H 1.2682 0.2427 0.7640 0.058 Uiso 1 1 calc R . . C6 C 1.0824(12) 0.1235(7) 0.8012(6) 0.0468(19) Uani 1 1 d . . . H6A H 1.0090 0.0903 0.8560 0.056 Uiso 1 1 calc R . . H6B H 1.1556 0.0679 0.7835 0.056 Uiso 1 1 calc R . . P7 P 0.9586(3) 0.18090(15) 0.71298(14) 0.0417(5) Uani 1 1 d . . . C31 C 0.7902(10) 0.0870(6) 0.7141(6) 0.0421(18) Uani 1 1 d . . . C32 C 0.6548(11) 0.1224(7) 0.6699(6) 0.047(2) Uani 1 1 d . . . H32 H 0.6517 0.1946 0.6381 0.057 Uiso 1 1 calc R . . C33 C 0.5251(13) 0.0528(8) 0.6725(7) 0.058(2) Uani 1 1 d . . . H33 H 0.4349 0.0770 0.6406 0.069 Uiso 1 1 calc R . . C34 C 0.5243(14) -0.0512(8) 0.7203(8) 0.066(3) Uani 1 1 d . . . H34 H 0.4318 -0.0972 0.7236 0.079 Uiso 1 1 calc R . . C35 C 0.6580(17) -0.0886(8) 0.7635(8) 0.074(3) Uani 1 1 d . . . H35 H 0.6584 -0.1609 0.7953 0.088 Uiso 1 1 calc R . . C36 C 0.7943(12) -0.0202(7) 0.7609(7) 0.054(2) Uani 1 1 d . . . H36 H 0.8870 -0.0460 0.7901 0.065 Uiso 1 1 calc R . . C41 C 1.0931(11) 0.1899(6) 0.6092(6) 0.0442(19) Uani 1 1 d . . . C42 C 1.1981(13) 0.2815(7) 0.5739(6) 0.054(2) Uani 1 1 d . . . H42 H 1.1946 0.3386 0.6033 0.065 Uiso 1 1 calc R . . C43 C 1.3059(16) 0.2874(9) 0.4965(8) 0.072(3) Uani 1 1 d . . . H43 H 1.3758 0.3488 0.4734 0.086 Uiso 1 1 calc R . . C44 C 1.3131(14) 0.2053(9) 0.4524(7) 0.062(3) Uani 1 1 d . . . H44 H 1.3869 0.2111 0.3992 0.074 Uiso 1 1 calc R . . C45 C 1.2121(12) 0.1134(8) 0.4858(6) 0.054(2) Uani 1 1 d . . . H45 H 1.2183 0.0562 0.4564 0.065 Uiso 1 1 calc R . . C46 C 1.1011(12) 0.1076(7) 0.5639(7) 0.054(2) Uani 1 1 d . . . H46 H 1.0303 0.0465 0.5862 0.065 Uiso 1 1 calc R . . O1W O 0.4053(10) 0.8379(7) 0.0950(5) 0.071(2) Uani 1 1 d . . . O1A O 0.1152(11) 0.8554(6) 0.8629(5) 0.072(2) Uani 1 1 d D A . N1A N 0.0566(11) 0.8101(6) 0.9365(6) 0.061(2) Uani 1 1 d D . . O2A O 0.072(3) 0.7200(12) 0.9807(12) 0.073(5) Uiso 0.40 1 d PD A 1 O3A O -0.044(4) 0.868(2) 0.9763(19) 0.140(11) Uiso 0.40 1 d PD A 1 O2B O 0.134(2) 0.7751(17) 1.0015(10) 0.072(5) Uiso 0.40 1 d PD A 2 O3B O -0.092(3) 0.775(3) 0.948(2) 0.165(14) Uiso 0.40 1 d PD A 2 O2C O 0.078(4) 0.840(2) 1.0054(13) 0.051(7) Uiso 0.20 1 d PD A 3 O3C O -0.008(3) 0.7181(14) 0.9479(15) 0.035(5) Uiso 0.20 1 d PD A 3 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 0.0444(4) 0.0294(3) 0.0444(3) -0.0105(2) -0.0098(2) -0.0027(2) N1 0.068(6) 0.048(5) 0.117(8) -0.044(5) -0.049(6) 0.013(4) O1 0.050(4) 0.049(3) 0.061(4) -0.016(3) -0.018(3) 0.003(3) O2 0.060(5) 0.063(5) 0.105(7) -0.020(5) -0.008(4) -0.003(4) O3 0.079(6) 0.111(8) 0.150(9) -0.050(7) -0.060(6) 0.006(5) P1 0.0466(12) 0.0307(9) 0.0451(11) -0.0112(8) -0.0091(9) -0.0012(8) C11 0.041(5) 0.036(4) 0.059(5) -0.017(4) -0.004(4) 0.007(3) C12 0.073(7) 0.067(7) 0.067(7) -0.024(5) -0.006(5) 0.013(5) C13 0.068(8) 0.088(9) 0.085(8) -0.024(7) -0.003(6) 0.026(7) C14 0.049(7) 0.042(5) 0.156(13) -0.018(7) 0.014(7) 0.011(4) C15 0.060(7) 0.036(5) 0.131(11) -0.018(6) -0.024(7) 0.005(4) C16 0.064(6) 0.034(4) 0.085(7) -0.016(4) -0.015(5) 0.000(4) C21 0.046(5) 0.040(4) 0.047(5) -0.011(3) -0.011(4) 0.000(3) C22 0.052(5) 0.043(4) 0.056(5) -0.012(4) -0.014(4) 0.003(4) C23 0.057(6) 0.041(5) 0.079(7) -0.004(4) -0.023(5) -0.010(4) C24 0.063(7) 0.056(6) 0.070(7) 0.013(5) -0.008(5) -0.007(5) C25 0.114(11) 0.057(6) 0.065(7) -0.005(5) 0.015(7) -0.002(6) C26 0.100(9) 0.056(6) 0.051(6) -0.013(5) 0.003(5) -0.013(6) C2 0.049(5) 0.036(4) 0.046(4) -0.010(3) -0.014(4) -0.004(3) C3 0.059(6) 0.038(4) 0.055(5) -0.013(4) -0.016(4) -0.005(4) N4 0.037(4) 0.033(3) 0.050(4) -0.010(3) -0.007(3) 0.002(3) C5 0.059(6) 0.034(4) 0.056(5) -0.017(4) -0.009(4) -0.005(4) C6 0.049(5) 0.035(4) 0.058(5) -0.012(4) -0.012(4) 0.001(3) P7 0.0485(12) 0.0264(9) 0.0518(12) -0.0099(8) -0.0105(9) -0.0015(8) C31 0.040(5) 0.035(4) 0.054(5) -0.017(3) -0.004(3) -0.002(3) C32 0.040(5) 0.039(4) 0.068(6) -0.016(4) -0.016(4) -0.001(3) C33 0.057(6) 0.050(5) 0.072(6) -0.023(5) -0.015(5) 0.000(4) C34 0.051(6) 0.056(6) 0.093(8) -0.018(5) -0.016(5) -0.014(5) C35 0.095(9) 0.037(5) 0.088(8) -0.007(5) -0.022(6) -0.018(5) C36 0.050(5) 0.033(4) 0.077(6) -0.010(4) -0.007(4) -0.013(4) C41 0.047(5) 0.035(4) 0.053(5) -0.016(3) -0.007(4) -0.001(3) C42 0.067(6) 0.044(5) 0.052(5) -0.017(4) 0.005(4) -0.007(4) C43 0.082(8) 0.051(6) 0.079(7) -0.014(5) 0.006(6) -0.019(5) C44 0.060(6) 0.065(6) 0.062(6) -0.019(5) -0.003(5) -0.003(5) C45 0.052(6) 0.060(6) 0.058(6) -0.024(5) -0.014(4) 0.006(4) C46 0.055(6) 0.044(5) 0.068(6) -0.019(4) -0.012(4) -0.009(4) O1W 0.066(5) 0.089(5) 0.057(4) -0.008(4) -0.015(3) 0.005(4) O1A 0.099(6) 0.056(4) 0.053(4) 0.002(3) -0.004(4) 0.006(4) N1A 0.072(6) 0.047(4) 0.065(5) -0.014(4) -0.014(4) 0.008(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 N4 2.021(7) . ? Pd1 O1 2.041(6) . ? Pd1 P1 2.308(2) . ? Pd1 P7 2.316(2) . ? N1 O2 1.195(13) . ? N1 O3 1.228(12) . ? N1 O1 1.344(13) . ? P1 C11 1.798(8) . ? P1 C21 1.816(9) . ? P1 C2 1.826(9) . ? C11 C16 1.374(14) . ? C11 C12 1.379(13) . ? C12 C13 1.395(16) . ? C13 C14 1.343(19) . ? C14 C15 1.38(2) . ? C15 C16 1.363(16) . ? C21 C26 1.368(13) . ? C21 C22 1.387(12) . ? C22 C23 1.364(13) . ? C23 C24 1.381(16) . ? C24 C25 1.361(17) . ? C25 C26 1.377(15) . ? C2 C3 1.502(12) . ? C3 N4 1.499(10) . ? N4 C5 1.500(11) . ? C5 C6 1.519(11) . ? C6 P7 1.810(9) . ? P7 C41 1.800(9) . ? P7 C31 1.810(8) . ? C31 C32 1.379(12) . ? C31 C36 1.394(12) . ? C32 C33 1.366(12) . ? C33 C34 1.361(15) . ? C34 C35 1.365(16) . ? C35 C36 1.396(14) . ? C41 C46 1.383(12) . ? C41 C42 1.407(12) . ? C42 C43 1.374(14) . ? C43 C44 1.368(15) . ? C44 C45 1.388(14) . ? C45 C46 1.396(14) . ? O1A N1A 1.193(11) . ? N1A O2A 1.209(14) . ? N1A O2C 1.243(15) . ? N1A O2B 1.244(14) . ? N1A O3C 1.250(15) . ? N1A O3B 1.256(16) . ? N1A O3A 1.281(16) . ? 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 N4 Pd1 O1 177.2(3) . . ? N4 Pd1 P1 84.17(19) . . ? O1 Pd1 P1 95.31(18) . . ? N4 Pd1 P7 84.51(19) . . ? O1 Pd1 P7 95.73(18) . . ? P1 Pd1 P7 167.34(8) . . ? O2 N1 O3 125.6(12) . . ? O2 N1 O1 119.7(9) . . ? O3 N1 O1 114.7(12) . . ? N1 O1 Pd1 111.0(6) . . ? C11 P1 C21 106.0(4) . . ? C11 P1 C2 109.3(4) . . ? C21 P1 C2 105.9(4) . . ? C11 P1 Pd1 120.7(3) . . ? C21 P1 Pd1 113.6(3) . . ? C2 P1 Pd1 100.4(3) . . ? C16 C11 C12 119.1(9) . . ? C16 C11 P1 117.8(7) . . ? C12 C11 P1 123.1(8) . . ? C11 C12 C13 119.8(11) . . ? C14 C13 C12 120.1(12) . . ? C13 C14 C15 120.2(10) . . ? C16 C15 C14 120.0(12) . . ? C15 C16 C11 120.7(11) . . ? C26 C21 C22 120.2(9) . . ? C26 C21 P1 119.9(7) . . ? C22 C21 P1 119.9(7) . . ? C23 C22 C21 119.2(9) . . ? C22 C23 C24 120.4(9) . . ? C25 C24 C23 120.0(9) . . ? C24 C25 C26 120.1(11) . . ? C21 C26 C25 119.9(10) . . ? C3 C2 P1 106.0(6) . . ? N4 C3 C2 109.3(7) . . ? C3 N4 C5 110.8(7) . . ? C3 N4 Pd1 113.7(5) . . ? C5 N4 Pd1 114.9(5) . . ? N4 C5 C6 108.3(7) . . ? C5 C6 P7 107.4(6) . . ? C41 P7 C6 106.5(4) . . ? C41 P7 C31 106.5(4) . . ? C6 P7 C31 109.0(4) . . ? C41 P7 Pd1 112.4(3) . . ? C6 P7 Pd1 99.6(3) . . ? C31 P7 Pd1 121.9(3) . . ? C32 C31 C36 119.7(8) . . ? C32 C31 P7 119.7(6) . . ? C36 C31 P7 120.6(7) . . ? C33 C32 C31 120.0(9) . . ? C34 C33 C32 121.1(10) . . ? C33 C34 C35 119.9(9) . . ? C34 C35 C36 120.5(10) . . ? C31 C36 C35 118.7(10) . . ? C46 C41 C42 118.4(8) . . ? C46 C41 P7 122.0(7) . . ? C42 C41 P7 119.6(6) . . ? C43 C42 C41 120.1(8) . . ? C44 C43 C42 121.0(10) . . ? C43 C44 C45 120.4(10) . . ? C44 C45 C46 118.8(9) . . ? C41 C46 C45 121.3(9) . . ? O1A N1A O2A 132.7(12) . . ? O1A N1A O2C 124.2(15) . . ? O2A N1A O2C 85.0(17) . . ? O1A N1A O2B 127.1(12) . . ? O2A N1A O2B 47.8(12) . . ? O2C N1A O2B 44.6(15) . . ? O1A N1A O3C 118.6(12) . . ? O2A N1A O3C 41.5(13) . . ? O2C N1A O3C 116.1(17) . . ? O2B N1A O3C 88.7(16) . . ? O1A N1A O3B 118.3(16) . . ? O2A N1A O3B 80(2) . . ? O2C N1A O3B 106(2) . . ? O2B N1A O3B 113.3(18) . . ? O3C N1A O3B 47(2) . . ? O1A N1A O3A 113.8(15) . . ? O2A N1A O3A 113.6(17) . . ? O2C N1A O3A 54.4(18) . . ? O2B N1A O3A 95.5(18) . . ? O3C N1A O3A 109(2) . . ? O3B N1A O3A 68(2) . . ? _diffrn_measured_fraction_theta_max 0.863 _diffrn_reflns_theta_full 70.25 _diffrn_measured_fraction_theta_full 0.863 _refine_diff_density_max 1.865 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.144 #CIF file of [Pd(PNHP)Cl]Cl.H2O (1.H2O) data_pdgshi _database_code_CSD 181547 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Pd Cl NH(C2H4PPh2)2 .Cl.H2O' _chemical_formula_sum 'C28 H31 Cl2 N O P2 Pd' _chemical_formula_weight 636.78 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 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 20.245(3) _cell_length_b 15.725(2) _cell_length_c 17.788(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.492(2) _cell_angle_gamma 90.00 _cell_volume 5482.8(12) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1763 _cell_measurement_theta_min 4 _cell_measurement_theta_max 44 _exptl_crystal_description plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.756 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'SMART APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36346 _diffrn_reflns_av_R_equivalents 0.1300 _diffrn_reflns_av_sigmaI/netI 0.1567 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.39 _reflns_number_total 11191 _reflns_number_gt 5662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric, except water hydrogens' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 11191 _refine_ls_number_parameters 647 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1447 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _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 0.08860(3) 0.06186(3) 0.30014(3) 0.02081(14) Uani 1 1 d . . . Cl1 Cl 0.05268(8) -0.06840(10) 0.24507(10) 0.0275(4) Uani 1 1 d . . . P1A P 0.02321(9) 0.14079(11) 0.20016(10) 0.0217(4) Uani 1 1 d . . . C1A1 C 0.0322(3) 0.1211(4) 0.1033(4) 0.0213(15) Uani 1 1 d . . . C1A2 C 0.0865(3) 0.0714(5) 0.0939(4) 0.0326(18) Uani 1 1 d . . . H1A2 H 0.1171 0.0474 0.1381 0.039 Uiso 1 1 calc R . . C1A3 C 0.0964(4) 0.0565(5) 0.0210(4) 0.0353(18) Uani 1 1 d . . . H1A3 H 0.1335 0.0223 0.0152 0.042 Uiso 1 1 calc R . . C1A4 C 0.0523(3) 0.0914(4) -0.0430(4) 0.0275(17) Uani 1 1 d . . . H1A4 H 0.0594 0.0819 -0.0932 0.033 Uiso 1 1 calc R . . C1A5 C -0.0021(4) 0.1401(5) -0.0348(4) 0.041(2) Uani 1 1 d . . . H1A5 H -0.0325 0.1641 -0.0792 0.049 Uiso 1 1 calc R . . C1A6 C -0.0122(3) 0.1540(5) 0.0395(4) 0.0314(18) Uani 1 1 d . . . H1A6 H -0.0502 0.1865 0.0453 0.038 Uiso 1 1 calc R . . C1B1 C -0.0670(3) 0.1403(4) 0.1947(4) 0.0240(16) Uani 1 1 d . . . C1B2 C -0.1005(3) 0.0621(4) 0.1866(4) 0.0280(17) Uani 1 1 d . . . H1B2 H -0.0754 0.0114 0.1844 0.034 Uiso 1 1 calc R . . C1B3 C -0.1703(3) 0.0572(5) 0.1816(4) 0.0313(17) Uani 1 1 d . . . H1B3 H -0.1932 0.0039 0.1741 0.038 Uiso 1 1 calc R . . C1B4 C -0.2058(4) 0.1312(5) 0.1878(4) 0.0326(18) Uani 1 1 d . . . H1B4 H -0.2533 0.1283 0.1848 0.039 Uiso 1 1 calc R . . C1B5 C -0.1736(4) 0.2079(5) 0.1980(4) 0.0373(19) Uani 1 1 d . . . H1B5 H -0.1984 0.2580 0.2029 0.045 Uiso 1 1 calc R . . C1B6 C -0.1042(3) 0.2125(4) 0.2012(4) 0.0273(17) Uani 1 1 d . . . H1B6 H -0.0820 0.2662 0.2081 0.033 Uiso 1 1 calc R . . C2A C 0.0564(3) 0.2466(4) 0.2266(4) 0.0247(16) Uani 1 1 d . . . H2A1 H 0.0948 0.2583 0.2029 0.030 Uiso 1 1 calc R . . H2A2 H 0.0203 0.2894 0.2069 0.030 Uiso 1 1 calc R . . C3A C 0.0808(3) 0.2531(4) 0.3149(4) 0.0284(17) Uani 1 1 d . . . H3A1 H 0.1063 0.3068 0.3295 0.034 Uiso 1 1 calc R . . H3A2 H 0.0412 0.2531 0.3381 0.034 Uiso 1 1 calc R . . N4A N 0.1261(3) 0.1785(3) 0.3447(3) 0.0227(13) Uani 1 1 d . . . H4A H 0.1644 0.1871 0.3258 0.027 Uiso 1 1 calc R . . C5A C 0.1525(4) 0.1815(4) 0.4309(3) 0.0300(17) Uani 1 1 d . . . H5A1 H 0.1140 0.1786 0.4560 0.036 Uiso 1 1 calc R . . H5A2 H 0.1774 0.2354 0.4465 0.036 Uiso 1 1 calc R . . C6A C 0.2001(3) 0.1061(4) 0.4563(4) 0.0290(17) Uani 1 1 d . . . H6A1 H 0.2125 0.1017 0.5136 0.035 Uiso 1 1 calc R . . H6A2 H 0.2425 0.1145 0.4390 0.035 Uiso 1 1 calc R . . P7A P 0.15751(9) 0.00858(11) 0.41369(10) 0.0239(4) Uani 1 1 d . . . C7A1 C 0.1105(3) -0.0365(4) 0.4800(4) 0.0250(16) Uani 1 1 d . . . C7A2 C 0.0526(4) -0.0814(4) 0.4490(4) 0.0347(18) Uani 1 1 d . . . H7A2 H 0.0367 -0.0856 0.3942 0.042 Uiso 1 1 calc R . . C7A3 C 0.0164(4) -0.1209(5) 0.4955(4) 0.042(2) Uani 1 1 d . . . H7A3 H -0.0238 -0.1523 0.4732 0.050 Uiso 1 1 calc R . . C7A4 C 0.0405(4) -0.1136(5) 0.5765(4) 0.041(2) Uani 1 1 d . . . H7A4 H 0.0162 -0.1397 0.6096 0.049 Uiso 1 1 calc R . . C7A5 C 0.0990(4) -0.0689(5) 0.6076(4) 0.046(2) Uani 1 1 d . . . H7A5 H 0.1150 -0.0643 0.6624 0.055 Uiso 1 1 calc R . . C7A6 C 0.1351(4) -0.0304(5) 0.5606(4) 0.042(2) Uani 1 1 d . . . H7A6 H 0.1760 -0.0003 0.5827 0.050 Uiso 1 1 calc R . . C7B1 C 0.2243(3) -0.0674(4) 0.4113(4) 0.0249(16) Uani 1 1 d . . . C7B2 C 0.2546(3) -0.0625(4) 0.3476(4) 0.0272(16) Uani 1 1 d . . . H7B2 H 0.2385 -0.0218 0.3077 0.033 Uiso 1 1 calc R . . C7B3 C 0.3070(3) -0.1163(4) 0.3432(4) 0.0292(17) Uani 1 1 d . . . H7B3 H 0.3283 -0.1117 0.3014 0.035 Uiso 1 1 calc R . . C7B4 C 0.3286(3) -0.1775(4) 0.4005(4) 0.0307(18) Uani 1 1 d . . . H7B4 H 0.3639 -0.2159 0.3969 0.037 Uiso 1 1 calc R . . C7B5 C 0.2992(3) -0.1830(5) 0.4627(4) 0.0311(18) Uani 1 1 d . . . H7B5 H 0.3150 -0.2244 0.5020 0.037 Uiso 1 1 calc R . . C7B6 C 0.2472(3) -0.1289(4) 0.4676(4) 0.0303(17) Uani 1 1 d . . . H7B6 H 0.2267 -0.1336 0.5101 0.036 Uiso 1 1 calc R . . Pd2 Pd -0.59910(3) 0.08832(3) 0.19765(3) 0.02329(15) Uani 1 1 d . . . Cl2 Cl -0.55480(9) -0.04198(10) 0.24338(10) 0.0288(4) Uani 1 1 d . . . P1C P -0.53994(9) 0.16092(11) 0.30604(10) 0.0241(4) Uani 1 1 d . . . C1C1 C -0.5465(3) 0.1276(4) 0.4017(4) 0.0227(15) Uani 1 1 d . . . C1C2 C -0.6041(4) 0.0840(4) 0.4085(4) 0.0331(18) Uani 1 1 d . . . H1C2 H -0.6396 0.0722 0.3636 0.040 Uiso 1 1 calc R . . C1C3 C -0.6099(4) 0.0577(5) 0.4809(4) 0.0333(18) Uani 1 1 d . . . H1C3 H -0.6490 0.0267 0.4854 0.040 Uiso 1 1 calc R . . C1C4 C -0.5594(4) 0.0761(4) 0.5458(4) 0.0328(18) Uani 1 1 d . . . H1C4 H -0.5639 0.0585 0.5954 0.039 Uiso 1 1 calc R . . C1C5 C -0.5032(4) 0.1192(5) 0.5401(4) 0.040(2) Uani 1 1 d . . . H1C5 H -0.4685 0.1317 0.5856 0.048 Uiso 1 1 calc R . . C1C6 C -0.4960(4) 0.1450(5) 0.4685(4) 0.0358(19) Uani 1 1 d . . . H1C6 H -0.4562 0.1750 0.4649 0.043 Uiso 1 1 calc R . . C1D1 C -0.4504(3) 0.1717(4) 0.3127(4) 0.0264(17) Uani 1 1 d . . . C1D2 C -0.4107(4) 0.0986(5) 0.3127(4) 0.0307(18) Uani 1 1 d . . . H1D2 H -0.4317 0.0442 0.3089 0.037 Uiso 1 1 calc R . . C1D3 C -0.3409(4) 0.1047(5) 0.3183(4) 0.039(2) Uani 1 1 d . . . H1D3 H -0.3145 0.0548 0.3176 0.046 Uiso 1 1 calc R . . C1D4 C -0.3103(4) 0.1839(5) 0.3247(4) 0.0330(18) Uani 1 1 d . . . H1D4 H -0.2626 0.1884 0.3301 0.040 Uiso 1 1 calc R . . C1D5 C -0.3485(4) 0.2557(5) 0.3235(4) 0.0356(19) Uani 1 1 d . . . H1D5 H -0.3273 0.3099 0.3262 0.043 Uiso 1 1 calc R . . C1D6 C -0.4186(3) 0.2507(5) 0.3183(4) 0.0298(17) Uani 1 1 d . . . H1D6 H -0.4444 0.3011 0.3186 0.036 Uiso 1 1 calc R . . C2C C -0.5786(4) 0.2660(4) 0.2863(4) 0.0291(17) Uani 1 1 d . . . H2C1 H -0.6203 0.2697 0.3056 0.035 Uiso 1 1 calc R . . H2C2 H -0.5462 0.3104 0.3124 0.035 Uiso 1 1 calc R . . C3C C -0.5962(4) 0.2782(4) 0.1982(4) 0.0318(17) Uani 1 1 d . . . H3C1 H -0.6209 0.3325 0.1840 0.038 Uiso 1 1 calc R . . H3C2 H -0.5539 0.2799 0.1798 0.038 Uiso 1 1 calc R . . N4C N -0.6399(3) 0.2055(3) 0.1615(3) 0.0270(14) Uani 1 1 d . . . H4C H -0.6787 0.2093 0.1803 0.032 Uiso 1 1 calc R . . C5C C -0.6654(4) 0.2150(5) 0.0756(4) 0.0338(18) Uani 1 1 d . . . H5C1 H -0.6263 0.2185 0.0515 0.041 Uiso 1 1 calc R . . H5C2 H -0.6923 0.2680 0.0634 0.041 Uiso 1 1 calc R . . C6C C -0.7095(3) 0.1390(4) 0.0435(4) 0.0308(18) Uani 1 1 d . . . H6C1 H -0.7211 0.1403 -0.0139 0.037 Uiso 1 1 calc R . . H6C2 H -0.7525 0.1413 0.0604 0.037 Uiso 1 1 calc R . . P7C P -0.66385(9) 0.04134(12) 0.07843(10) 0.0256(4) Uani 1 1 d . . . C7C1 C -0.7265(3) -0.0395(4) 0.0790(4) 0.0292(17) Uani 1 1 d . . . C7C2 C -0.7552(3) -0.0468(4) 0.1426(4) 0.0277(17) Uani 1 1 d . . . H7C2 H -0.7417 -0.0084 0.1850 0.033 Uiso 1 1 calc R . . C7C3 C -0.8022(3) -0.1083(4) 0.1444(4) 0.0260(16) Uani 1 1 d . . . H7C3 H -0.8216 -0.1116 0.1877 0.031 Uiso 1 1 calc R . . C7C4 C -0.8220(3) -0.1659(5) 0.0843(4) 0.0330(18) Uani 1 1 d . . . H7C4 H -0.8536 -0.2095 0.0873 0.040 Uiso 1 1 calc R . . C7C5 C -0.7958(3) -0.1601(5) 0.0196(4) 0.0341(19) Uani 1 1 d . . . H7C5 H -0.8104 -0.1984 -0.0226 0.041 Uiso 1 1 calc R . . C7C6 C -0.7481(3) -0.0978(5) 0.0173(4) 0.0335(18) Uani 1 1 d . . . H7C6 H -0.7296 -0.0942 -0.0267 0.040 Uiso 1 1 calc R . . C7D1 C -0.6207(3) 0.0034(4) 0.0073(4) 0.0264(16) Uani 1 1 d . . . C7D2 C -0.5751(3) -0.0631(5) 0.0285(4) 0.0323(18) Uani 1 1 d . . . H7D2 H -0.5637 -0.0827 0.0806 0.039 Uiso 1 1 calc R . . C7D3 C -0.5457(4) -0.1013(5) -0.0252(4) 0.0372(19) Uani 1 1 d . . . H7D3 H -0.5150 -0.1474 -0.0099 0.045 Uiso 1 1 calc R . . C7D4 C -0.5612(4) -0.0721(4) -0.1024(4) 0.0347(18) Uani 1 1 d . . . H7D4 H -0.5418 -0.0992 -0.1396 0.042 Uiso 1 1 calc R . . C7D5 C -0.6043(4) -0.0047(5) -0.1235(4) 0.0369(19) Uani 1 1 d . . . H7D5 H -0.6137 0.0165 -0.1752 0.044 Uiso 1 1 calc R . . C7D6 C -0.6349(4) 0.0339(5) -0.0689(4) 0.0322(18) Uani 1 1 d . . . H7D6 H -0.6652 0.0805 -0.0839 0.039 Uiso 1 1 calc R . . Cl1S Cl 0.26392(11) 0.40667(14) 0.19272(14) 0.0587(6) Uani 1 1 d . . . Cl2S Cl -0.75615(9) 0.14794(12) 0.25213(10) 0.0335(4) Uani 1 1 d . . . O1W O 0.2464(3) 0.3213(4) 0.3448(4) 0.0577(17) Uani 1 1 d D . . H1W1 H 0.259(4) 0.269(2) 0.332(4) 0.04(2) Uiso 1 1 d D . . H1W2 H 0.240(11) 0.351(6) 0.300(4) 0.40(15) Uiso 1 1 d D . . O2W O 0.1682(3) 0.2335(4) 0.6026(3) 0.0524(16) Uani 1 1 d D . . H2W1 H 0.197(2) 0.189(3) 0.618(3) 0.019(19) Uiso 1 1 d D . . H2W2 H 0.174(12) 0.265(10) 0.646(5) 0.55(19) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0227(3) 0.0233(3) 0.0167(3) 0.0000(2) 0.0054(2) -0.0015(2) Cl1 0.0336(10) 0.0233(9) 0.0236(9) -0.0004(8) 0.0032(7) -0.0025(8) P1A 0.0240(10) 0.0238(10) 0.0183(9) -0.0021(8) 0.0072(8) -0.0020(8) C1A1 0.024(4) 0.017(3) 0.023(4) 0.004(3) 0.006(3) -0.001(3) C1A2 0.030(4) 0.047(5) 0.021(4) 0.006(4) 0.008(3) 0.005(4) C1A3 0.040(5) 0.036(4) 0.032(4) 0.005(4) 0.011(4) 0.016(4) C1A4 0.027(4) 0.038(4) 0.019(4) 0.001(3) 0.009(3) 0.000(3) C1A5 0.037(5) 0.069(6) 0.018(4) 0.001(4) 0.010(3) 0.012(4) C1A6 0.023(4) 0.049(5) 0.024(4) 0.003(4) 0.011(3) 0.012(4) C1B1 0.019(4) 0.034(4) 0.021(4) 0.001(3) 0.007(3) 0.000(3) C1B2 0.030(4) 0.027(4) 0.025(4) 0.002(3) 0.005(3) -0.003(4) C1B3 0.031(4) 0.045(5) 0.018(4) 0.001(4) 0.007(3) -0.001(4) C1B4 0.026(4) 0.055(5) 0.021(4) 0.002(4) 0.013(3) -0.007(4) C1B5 0.039(5) 0.044(5) 0.028(4) -0.003(4) 0.006(4) 0.012(4) C1B6 0.020(4) 0.029(4) 0.029(4) 0.000(3) 0.000(3) -0.005(3) C2A 0.026(4) 0.026(4) 0.024(4) 0.004(3) 0.012(3) -0.003(3) C3A 0.030(4) 0.023(4) 0.032(4) -0.004(3) 0.006(3) 0.000(3) N4A 0.027(3) 0.026(3) 0.016(3) 0.000(3) 0.006(2) 0.000(3) C5A 0.037(4) 0.039(4) 0.012(4) -0.004(3) 0.002(3) -0.007(4) C6A 0.017(4) 0.045(5) 0.026(4) -0.002(3) 0.007(3) -0.006(3) P7A 0.0235(10) 0.0287(10) 0.0187(9) 0.0014(8) 0.0038(8) -0.0015(8) C7A1 0.021(4) 0.034(4) 0.022(4) 0.007(3) 0.010(3) 0.000(3) C7A2 0.042(5) 0.036(4) 0.027(4) -0.002(4) 0.011(4) -0.006(4) C7A3 0.050(5) 0.042(5) 0.039(5) 0.007(4) 0.020(4) -0.011(4) C7A4 0.042(5) 0.058(5) 0.027(4) 0.013(4) 0.017(4) -0.001(4) C7A5 0.044(5) 0.066(6) 0.026(4) 0.003(4) 0.009(4) -0.010(5) C7A6 0.036(5) 0.070(6) 0.020(4) 0.001(4) 0.006(3) -0.005(4) C7B1 0.027(4) 0.031(4) 0.017(4) 0.002(3) 0.006(3) -0.008(3) C7B2 0.024(4) 0.029(4) 0.028(4) 0.003(3) 0.005(3) -0.011(3) C7B3 0.023(4) 0.034(4) 0.028(4) 0.000(3) 0.002(3) -0.009(3) C7B4 0.018(4) 0.031(4) 0.039(5) 0.000(4) -0.001(3) -0.007(3) C7B5 0.030(4) 0.041(5) 0.020(4) 0.003(3) 0.002(3) 0.001(4) C7B6 0.029(4) 0.041(5) 0.021(4) 0.011(3) 0.005(3) -0.006(4) Pd2 0.0243(3) 0.0262(3) 0.0193(3) 0.0018(3) 0.0053(2) 0.0001(3) Cl2 0.0352(10) 0.0239(9) 0.0264(10) 0.0026(8) 0.0058(8) -0.0004(8) P1C 0.0224(10) 0.0259(10) 0.0241(10) -0.0005(8) 0.0062(8) -0.0015(8) C1C1 0.027(4) 0.022(4) 0.021(4) -0.001(3) 0.009(3) -0.001(3) C1C2 0.032(4) 0.039(5) 0.028(4) -0.001(4) 0.006(3) -0.002(4) C1C3 0.036(4) 0.039(5) 0.025(4) 0.004(4) 0.008(3) -0.013(4) C1C4 0.035(4) 0.036(5) 0.027(4) 0.003(3) 0.006(3) -0.002(4) C1C5 0.040(5) 0.061(6) 0.021(4) -0.002(4) 0.012(3) -0.008(4) C1C6 0.030(4) 0.051(5) 0.030(4) 0.002(4) 0.012(3) -0.016(4) C1D1 0.029(4) 0.030(4) 0.019(4) -0.011(3) 0.005(3) -0.003(3) C1D2 0.044(5) 0.032(4) 0.020(4) -0.003(3) 0.016(3) -0.004(4) C1D3 0.026(4) 0.046(5) 0.045(5) -0.003(4) 0.011(4) 0.005(4) C1D4 0.026(4) 0.054(5) 0.022(4) -0.006(4) 0.011(3) -0.001(4) C1D5 0.027(4) 0.042(5) 0.038(5) 0.008(4) 0.008(3) -0.009(4) C1D6 0.032(4) 0.032(4) 0.026(4) 0.005(3) 0.009(3) -0.008(4) C2C 0.041(4) 0.021(4) 0.026(4) -0.004(3) 0.011(3) 0.000(3) C3C 0.046(5) 0.022(4) 0.035(4) -0.002(4) 0.024(4) -0.009(4) N4C 0.028(3) 0.031(3) 0.024(3) 0.002(3) 0.010(3) -0.001(3) C5C 0.032(4) 0.038(5) 0.034(4) 0.008(4) 0.013(4) 0.009(4) C6C 0.028(4) 0.044(5) 0.019(4) -0.001(3) 0.003(3) 0.007(4) P7C 0.0248(10) 0.0338(11) 0.0174(10) 0.0014(8) 0.0040(8) 0.0047(9) C7C1 0.025(4) 0.041(5) 0.019(4) -0.002(3) 0.003(3) 0.014(3) C7C2 0.039(4) 0.024(4) 0.020(4) 0.002(3) 0.006(3) 0.013(4) C7C3 0.020(4) 0.027(4) 0.031(4) 0.000(3) 0.006(3) 0.004(3) C7C4 0.023(4) 0.042(5) 0.032(4) -0.005(4) 0.004(3) -0.001(4) C7C5 0.019(4) 0.046(5) 0.034(4) -0.015(4) 0.001(3) 0.005(4) C7C6 0.028(4) 0.054(5) 0.016(4) -0.011(4) 0.003(3) -0.002(4) C7D1 0.016(4) 0.039(4) 0.022(4) -0.002(3) 0.002(3) 0.000(3) C7D2 0.031(4) 0.041(5) 0.025(4) 0.007(4) 0.007(3) 0.001(4) C7D3 0.038(5) 0.035(5) 0.037(5) -0.007(4) 0.006(4) 0.005(4) C7D4 0.043(5) 0.031(4) 0.036(5) -0.001(4) 0.022(4) 0.005(4) C7D5 0.047(5) 0.044(5) 0.020(4) 0.001(4) 0.010(4) -0.005(4) C7D6 0.034(4) 0.043(5) 0.019(4) 0.004(3) 0.004(3) 0.007(4) Cl1S 0.0490(14) 0.0452(13) 0.0731(17) 0.0101(12) -0.0014(12) -0.0022(11) Cl2S 0.0358(11) 0.0337(11) 0.0346(10) 0.0015(8) 0.0157(8) 0.0007(8) O1W 0.060(4) 0.068(5) 0.055(4) -0.030(4) 0.033(3) -0.024(4) O2W 0.064(4) 0.059(4) 0.038(3) 0.001(3) 0.021(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N4A 2.065(5) . ? Pd1 P1A 2.2973(18) . ? Pd1 P7A 2.3060(18) . ? Pd1 Cl1 2.3082(17) . ? P1A C1A1 1.803(6) . ? P1A C1B1 1.804(6) . ? P1A C2A 1.812(6) . ? C1A1 C1A6 1.362(9) . ? C1A1 C1A2 1.394(9) . ? C1A2 C1A3 1.380(9) . ? C1A3 C1A4 1.373(9) . ? C1A4 C1A5 1.379(9) . ? C1A5 C1A6 1.405(9) . ? C1B1 C1B6 1.383(9) . ? C1B1 C1B2 1.395(9) . ? C1B2 C1B3 1.397(9) . ? C1B3 C1B4 1.386(10) . ? C1B4 C1B5 1.361(10) . ? C1B5 C1B6 1.395(9) . ? C2A C3A 1.528(9) . ? C3A N4A 1.502(8) . ? N4A C5A 1.493(7) . ? C5A C6A 1.523(9) . ? C6A P7A 1.829(7) . ? P7A C7B1 1.813(7) . ? P7A C7A1 1.833(6) . ? C7A1 C7A2 1.361(9) . ? C7A1 C7A6 1.399(9) . ? C7A2 C7A3 1.381(9) . ? C7A3 C7A4 1.405(10) . ? C7A4 C7A5 1.371(10) . ? C7A5 C7A6 1.379(10) . ? C7B1 C7B6 1.386(9) . ? C7B1 C7B2 1.418(9) . ? C7B2 C7B3 1.375(9) . ? C7B3 C7B4 1.391(9) . ? C7B4 C7B5 1.383(9) . ? C7B5 C7B6 1.374(9) . ? Pd2 N4C 2.056(5) . ? Pd2 Cl2 2.3019(17) . ? Pd2 P1C 2.3021(19) . ? Pd2 P7C 2.3172(18) . ? P1C C1D1 1.794(7) . ? P1C C1C1 1.817(6) . ? P1C C2C 1.824(7) . ? C1C1 C1C2 1.383(9) . ? C1C1 C1C6 1.387(9) . ? C1C2 C1C3 1.385(9) . ? C1C3 C1C4 1.369(9) . ? C1C4 C1C5 1.349(9) . ? C1C5 C1C6 1.379(9) . ? C1D1 C1D6 1.391(9) . ? C1D1 C1D2 1.403(9) . ? C1D2 C1D3 1.396(9) . ? C1D3 C1D4 1.382(10) . ? C1D4 C1D5 1.366(10) . ? C1D5 C1D6 1.401(9) . ? C2C C3C 1.530(9) . ? C3C N4C 1.493(8) . ? N4C C5C 1.492(8) . ? C5C C6C 1.516(9) . ? C6C P7C 1.820(7) . ? P7C C7C1 1.798(7) . ? P7C C7D1 1.809(7) . ? C7C1 C7C2 1.400(9) . ? C7C1 C7C6 1.413(9) . ? C7C2 C7C3 1.362(9) . ? C7C3 C7C4 1.382(9) . ? C7C4 C7C5 1.384(9) . ? C7C5 C7C6 1.382(10) . ? C7D1 C7D2 1.382(9) . ? C7D1 C7D6 1.399(9) . ? C7D2 C7D3 1.382(9) . ? C7D3 C7D4 1.406(10) . ? C7D4 C7D5 1.365(9) . ? C7D5 C7D6 1.414(9) . ? 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 N4A Pd1 P1A 84.41(15) . . ? N4A Pd1 P7A 84.43(15) . . ? P1A Pd1 P7A 168.37(7) . . ? N4A Pd1 Cl1 175.76(15) . . ? P1A Pd1 Cl1 95.26(6) . . ? P7A Pd1 Cl1 96.12(6) . . ? C1A1 P1A C1B1 106.9(3) . . ? C1A1 P1A C2A 106.6(3) . . ? C1B1 P1A C2A 108.8(3) . . ? C1A1 P1A Pd1 118.1(2) . . ? C1B1 P1A Pd1 114.8(2) . . ? C2A P1A Pd1 101.0(2) . . ? C1A6 C1A1 C1A2 119.3(6) . . ? C1A6 C1A1 P1A 121.9(5) . . ? C1A2 C1A1 P1A 118.9(5) . . ? C1A3 C1A2 C1A1 120.9(6) . . ? C1A4 C1A3 C1A2 119.7(7) . . ? C1A3 C1A4 C1A5 120.2(7) . . ? C1A4 C1A5 C1A6 119.7(7) . . ? C1A1 C1A6 C1A5 120.2(6) . . ? C1B6 C1B1 C1B2 118.2(6) . . ? C1B6 C1B1 P1A 123.9(5) . . ? C1B2 C1B1 P1A 117.9(5) . . ? C1B1 C1B2 C1B3 120.9(7) . . ? C1B4 C1B3 C1B2 119.0(7) . . ? C1B5 C1B4 C1B3 121.0(7) . . ? C1B4 C1B5 C1B6 119.7(7) . . ? C1B1 C1B6 C1B5 121.2(7) . . ? C3A C2A P1A 109.4(4) . . ? N4A C3A C2A 108.8(5) . . ? C5A N4A C3A 111.6(5) . . ? C5A N4A Pd1 115.1(4) . . ? C3A N4A Pd1 115.2(4) . . ? N4A C5A C6A 108.5(5) . . ? C5A C6A P7A 109.3(4) . . ? C7B1 P7A C6A 106.6(3) . . ? C7B1 P7A C7A1 105.7(3) . . ? C6A P7A C7A1 109.0(3) . . ? C7B1 P7A Pd1 120.7(2) . . ? C6A P7A Pd1 100.2(2) . . ? C7A1 P7A Pd1 114.0(2) . . ? C7A2 C7A1 C7A6 120.0(6) . . ? C7A2 C7A1 P7A 118.3(5) . . ? C7A6 C7A1 P7A 121.6(5) . . ? C7A1 C7A2 C7A3 121.5(7) . . ? C7A2 C7A3 C7A4 118.5(7) . . ? C7A5 C7A4 C7A3 119.9(7) . . ? C7A4 C7A5 C7A6 121.0(7) . . ? C7A5 C7A6 C7A1 119.0(7) . . ? C7B6 C7B1 C7B2 118.9(6) . . ? C7B6 C7B1 P7A 124.0(5) . . ? C7B2 C7B1 P7A 117.2(5) . . ? C7B3 C7B2 C7B1 120.4(6) . . ? C7B2 C7B3 C7B4 119.3(7) . . ? C7B5 C7B4 C7B3 120.7(7) . . ? C7B6 C7B5 C7B4 120.2(7) . . ? C7B5 C7B6 C7B1 120.5(6) . . ? N4C Pd2 Cl2 177.40(16) . . ? N4C Pd2 P1C 84.37(16) . . ? Cl2 Pd2 P1C 94.04(6) . . ? N4C Pd2 P7C 84.73(16) . . ? Cl2 Pd2 P7C 96.94(7) . . ? P1C Pd2 P7C 168.86(7) . . ? C1D1 P1C C1C1 106.0(3) . . ? C1D1 P1C C2C 107.7(3) . . ? C1C1 P1C C2C 108.2(3) . . ? C1D1 P1C Pd2 114.0(2) . . ? C1C1 P1C Pd2 119.8(2) . . ? C2C P1C Pd2 100.4(2) . . ? C1C2 C1C1 C1C6 118.7(6) . . ? C1C2 C1C1 P1C 119.0(5) . . ? C1C6 C1C1 P1C 122.3(5) . . ? C1C1 C1C2 C1C3 119.9(7) . . ? C1C4 C1C3 C1C2 120.1(7) . . ? C1C5 C1C4 C1C3 120.6(7) . . ? C1C4 C1C5 C1C6 120.2(7) . . ? C1C5 C1C6 C1C1 120.5(6) . . ? C1D6 C1D1 C1D2 118.5(6) . . ? C1D6 C1D1 P1C 122.1(5) . . ? C1D2 C1D1 P1C 119.5(5) . . ? C1D3 C1D2 C1D1 121.0(7) . . ? C1D4 C1D3 C1D2 119.4(7) . . ? C1D5 C1D4 C1D3 120.3(7) . . ? C1D4 C1D5 C1D6 121.0(7) . . ? C1D1 C1D6 C1D5 119.9(7) . . ? C3C C2C P1C 106.8(4) . . ? N4C C3C C2C 108.2(5) . . ? C5C N4C C3C 112.7(5) . . ? C5C N4C Pd2 114.8(4) . . ? C3C N4C Pd2 113.7(4) . . ? N4C C5C C6C 109.0(6) . . ? C5C C6C P7C 109.6(5) . . ? C7C1 P7C C7D1 103.6(3) . . ? C7C1 P7C C6C 107.4(3) . . ? C7D1 P7C C6C 109.5(3) . . ? C7C1 P7C Pd2 117.3(2) . . ? C7D1 P7C Pd2 118.9(2) . . ? C6C P7C Pd2 99.5(2) . . ? C7C2 C7C1 C7C6 117.7(7) . . ? C7C2 C7C1 P7C 119.9(5) . . ? C7C6 C7C1 P7C 122.5(5) . . ? C7C3 C7C2 C7C1 120.7(7) . . ? C7C2 C7C3 C7C4 121.1(7) . . ? C7C3 C7C4 C7C5 120.1(7) . . ? C7C6 C7C5 C7C4 119.2(7) . . ? C7C5 C7C6 C7C1 121.3(7) . . ? C7D2 C7D1 C7D6 119.0(6) . . ? C7D2 C7D1 P7C 117.8(5) . . ? C7D6 C7D1 P7C 123.0(5) . . ? C7D3 C7D2 C7D1 120.9(7) . . ? C7D2 C7D3 C7D4 120.3(7) . . ? C7D5 C7D4 C7D3 119.5(7) . . ? C7D4 C7D5 C7D6 120.3(7) . . ? C7D1 C7D6 C7D5 120.0(7) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.640 _refine_diff_density_min -1.107 _refine_diff_density_rms 0.132 #CIF file of [Pd(PNHP)Br]Br.(CH3)2CO (2.(CH3)2CO) data_pdinbr _database_code_CSD 181548 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[PdBr(Ph2PCH2CH2NHCH2CH2PPh2)]+Br-.Me2CO' _chemical_formula_sum 'C31 H35 Br2 N O P2 Pd' _chemical_formula_weight 765.76 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.722(4) _cell_length_b 12.209(4) _cell_length_c 12.640(4) _cell_angle_alpha 114.823(13) _cell_angle_beta 101.696(19) _cell_angle_gamma 98.816(17) _cell_volume 1548.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _exptl_crystal_description block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 3.307 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_correction_T_min 0.532 _exptl_absorpt_correction_T_max 0.819 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6158 _diffrn_reflns_av_R_equivalents 0.0833 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 25.09 _reflns_number_total 5495 _reflns_number_gt 3865 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _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^)+(0.0585P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5495 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0832 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0970 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.23820(4) 0.10499(4) 0.27978(4) 0.01735(14) Uani 1 1 d . . . Br1 Br 0.02782(5) 0.08496(6) 0.19232(6) 0.02324(17) Uani 1 1 d . . . P1 P 0.20927(16) -0.08957(16) 0.27129(15) 0.0253(4) Uani 1 1 d . . . C11 C 0.1633(7) -0.2242(6) 0.1205(6) 0.0319(17) Uani 1 1 d . . . C12 C 0.1886(9) -0.3364(7) 0.1074(7) 0.053(3) Uani 1 1 d . . . H12 H 0.2329 -0.3419 0.1760 0.064 Uiso 1 1 calc R . . C13 C 0.1475(10) -0.4413(7) -0.0090(7) 0.063(3) Uani 1 1 d . . . H13 H 0.1632 -0.5185 -0.0188 0.076 Uiso 1 1 calc R . . C14 C 0.0850(8) -0.4332(7) -0.1080(7) 0.047(2) Uani 1 1 d . . . H14 H 0.0580 -0.5047 -0.1861 0.057 Uiso 1 1 calc R . . C15 C 0.0609(7) -0.3218(6) -0.0954(6) 0.0350(17) Uani 1 1 d . . . H15 H 0.0176 -0.3169 -0.1647 0.042 Uiso 1 1 calc R . . C16 C 0.1003(6) -0.2164(6) 0.0195(6) 0.0268(15) Uani 1 1 d . . . H16 H 0.0840 -0.1397 0.0284 0.032 Uiso 1 1 calc R . . C21 C 0.1130(6) -0.1289(6) 0.3522(6) 0.0257(15) Uani 1 1 d . . . C22 C -0.0020(7) -0.2111(6) 0.2890(6) 0.0329(17) Uani 1 1 d . . . H22 H -0.0283 -0.2499 0.2023 0.040 Uiso 1 1 calc R . . C23 C -0.0788(8) -0.2374(6) 0.3507(7) 0.0381(18) Uani 1 1 d . . . H23 H -0.1567 -0.2945 0.3066 0.046 Uiso 1 1 calc R . . C24 C -0.0405(7) -0.1791(6) 0.4780(6) 0.0334(17) Uani 1 1 d . . . H24 H -0.0924 -0.1959 0.5213 0.040 Uiso 1 1 calc R . . C25 C 0.0736(7) -0.0966(6) 0.5411(6) 0.0348(18) Uani 1 1 d . . . H25 H 0.1001 -0.0582 0.6277 0.042 Uiso 1 1 calc R . . C26 C 0.1492(7) -0.0694(6) 0.4796(6) 0.0310(17) Uani 1 1 d . . . H26 H 0.2259 -0.0100 0.5240 0.037 Uiso 1 1 calc R . . C2 C 0.3628(7) -0.0796(7) 0.3496(6) 0.0362(19) Uani 1 1 d . . . H2A H 0.3740 -0.0464 0.4383 0.043 Uiso 1 1 calc R . . H2B H 0.3771 -0.1638 0.3179 0.043 Uiso 1 1 calc R . . C3 C 0.4502(7) 0.0062(7) 0.3275(6) 0.040(2) Uani 1 1 d . . . H3A H 0.5336 0.0209 0.3766 0.048 Uiso 1 1 calc R . . H3B H 0.4467 -0.0328 0.2402 0.048 Uiso 1 1 calc R . . N4 N 0.4177(5) 0.1274(5) 0.3624(5) 0.0280(13) Uani 1 1 d . . . H4 H 0.4259 0.1602 0.4454 0.034 Uiso 1 1 calc R . . C5 C 0.5032(6) 0.2210(7) 0.3513(6) 0.0359(19) Uani 1 1 d . . . H5A H 0.5033 0.1900 0.2653 0.043 Uiso 1 1 calc R . . H5B H 0.5860 0.2363 0.4020 0.043 Uiso 1 1 calc R . . C6 C 0.4642(6) 0.3421(6) 0.3940(6) 0.0320(17) Uani 1 1 d . . . H6A H 0.5161 0.4045 0.3810 0.038 Uiso 1 1 calc R . . H6B H 0.4714 0.3778 0.4821 0.038 Uiso 1 1 calc R . . P7 P 0.30647(14) 0.30353(15) 0.30432(14) 0.0218(4) Uani 1 1 d . . . C31 C 0.3120(6) 0.3171(6) 0.1684(6) 0.0283(15) Uani 1 1 d . . . C32 C 0.3881(7) 0.4204(7) 0.1757(6) 0.0394(19) Uani 1 1 d . . . H32 H 0.4346 0.4873 0.2536 0.047 Uiso 1 1 calc R . . C33 C 0.3973(7) 0.4274(8) 0.0724(7) 0.051(2) Uani 1 1 d . . . H33 H 0.4492 0.4991 0.0786 0.061 Uiso 1 1 calc R . . C34 C 0.3297(7) 0.3282(8) -0.0432(7) 0.048(2) Uani 1 1 d . . . H34 H 0.3373 0.3315 -0.1152 0.058 Uiso 1 1 calc R . . C35 C 0.2529(7) 0.2268(7) -0.0510(6) 0.0366(18) Uani 1 1 d . . . H35 H 0.2055 0.1611 -0.1290 0.044 Uiso 1 1 calc R . . C36 C 0.2432(6) 0.2184(6) 0.0532(6) 0.0299(16) Uani 1 1 d . . . H36 H 0.1907 0.1468 0.0467 0.036 Uiso 1 1 calc R . . C41 C 0.2460(5) 0.4257(5) 0.3953(5) 0.0199(13) Uani 1 1 d . . . C42 C 0.2384(6) 0.4374(6) 0.5080(6) 0.0282(15) Uani 1 1 d . . . H42 H 0.2683 0.3844 0.5376 0.034 Uiso 1 1 calc R . . C43 C 0.1875(6) 0.5257(6) 0.5763(6) 0.0334(17) Uani 1 1 d . . . H43 H 0.1809 0.5315 0.6520 0.040 Uiso 1 1 calc R . . C44 C 0.1459(6) 0.6059(6) 0.5374(6) 0.0313(16) Uani 1 1 d . . . H44 H 0.1123 0.6672 0.5868 0.038 Uiso 1 1 calc R . . C45 C 0.1529(7) 0.5973(6) 0.4262(6) 0.0361(18) Uani 1 1 d . . . H45 H 0.1234 0.6519 0.3987 0.043 Uiso 1 1 calc R . . C46 C 0.2036(7) 0.5081(6) 0.3548(6) 0.0335(17) Uani 1 1 d . . . H46 H 0.2097 0.5026 0.2790 0.040 Uiso 1 1 calc R . . Br2 Br -0.41031(7) -0.25405(7) 0.35338(6) 0.0340(2) Uani 1 1 d . . . C1S C 0.5955(8) 0.2123(9) 0.0427(8) 0.065(3) Uani 1 1 d . . . H1S1 H 0.5612 0.2016 -0.0396 0.098 Uiso 1 1 calc R . . H1S2 H 0.6649 0.2865 0.0877 0.098 Uiso 1 1 calc R . . H1S3 H 0.5340 0.2228 0.0857 0.098 Uiso 1 1 calc R . . O1S O 0.6125(5) 0.0058(6) -0.0632(5) 0.0546(16) Uani 1 1 d . . . C2S C 0.6357(6) 0.0995(8) 0.0339(7) 0.045(2) Uani 1 1 d . . . C3S C 0.7067(7) 0.1039(9) 0.1496(7) 0.059(3) Uani 1 1 d . . . H3S1 H 0.6793 0.0234 0.1486 0.089 Uiso 1 1 calc R . . H3S2 H 0.6941 0.1708 0.2199 0.089 Uiso 1 1 calc R . . H3S3 H 0.7928 0.1204 0.1556 0.089 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 0.0178(3) 0.0203(3) 0.0116(2) 0.0049(2) 0.00275(19) 0.0086(2) Br1 0.0198(3) 0.0273(4) 0.0225(3) 0.0124(3) 0.0035(3) 0.0077(3) P1 0.0382(10) 0.0275(9) 0.0169(9) 0.0120(7) 0.0084(8) 0.0216(8) C11 0.054(5) 0.019(3) 0.029(4) 0.010(3) 0.018(3) 0.021(3) C12 0.112(8) 0.040(5) 0.024(4) 0.019(4) 0.023(5) 0.051(5) C13 0.130(9) 0.031(5) 0.041(5) 0.014(4) 0.035(6) 0.050(5) C14 0.099(7) 0.023(4) 0.023(4) 0.006(3) 0.027(4) 0.024(4) C15 0.053(5) 0.024(4) 0.023(4) 0.008(3) 0.007(3) 0.010(3) C16 0.044(4) 0.022(3) 0.021(3) 0.012(3) 0.014(3) 0.018(3) C21 0.049(4) 0.018(3) 0.016(3) 0.010(3) 0.008(3) 0.018(3) C22 0.063(5) 0.028(4) 0.018(4) 0.014(3) 0.013(3) 0.025(4) C23 0.060(5) 0.023(4) 0.034(4) 0.012(3) 0.020(4) 0.017(4) C24 0.058(5) 0.022(4) 0.032(4) 0.017(3) 0.021(4) 0.020(4) C25 0.063(5) 0.023(4) 0.022(4) 0.012(3) 0.015(4) 0.014(4) C26 0.061(5) 0.019(3) 0.021(4) 0.011(3) 0.018(3) 0.016(3) C2 0.050(5) 0.050(5) 0.021(4) 0.018(3) 0.013(3) 0.038(4) C3 0.038(4) 0.067(5) 0.020(4) 0.017(4) 0.008(3) 0.042(4) N4 0.019(3) 0.045(4) 0.014(3) 0.007(3) 0.001(2) 0.014(3) C5 0.015(3) 0.052(5) 0.020(4) 0.000(3) 0.002(3) 0.009(3) C6 0.020(4) 0.036(4) 0.026(4) 0.004(3) 0.006(3) 0.000(3) P7 0.0182(8) 0.0242(9) 0.0151(8) 0.0041(7) 0.0042(7) 0.0002(7) C31 0.029(4) 0.031(4) 0.017(3) 0.008(3) 0.006(3) -0.002(3) C32 0.042(5) 0.042(4) 0.023(4) 0.011(3) 0.009(3) -0.007(4) C33 0.047(5) 0.059(6) 0.043(5) 0.024(4) 0.022(4) -0.008(4) C34 0.048(5) 0.063(6) 0.031(4) 0.020(4) 0.019(4) 0.002(4) C35 0.037(4) 0.044(5) 0.021(4) 0.011(3) 0.006(3) 0.006(4) C36 0.029(4) 0.030(4) 0.022(4) 0.007(3) 0.006(3) 0.004(3) C41 0.017(3) 0.014(3) 0.019(3) 0.003(3) 0.002(3) -0.005(2) C42 0.031(4) 0.034(4) 0.028(4) 0.018(3) 0.013(3) 0.015(3) C43 0.034(4) 0.041(4) 0.030(4) 0.018(3) 0.016(3) 0.012(3) C44 0.030(4) 0.026(4) 0.030(4) 0.004(3) 0.010(3) 0.009(3) C45 0.049(5) 0.023(4) 0.032(4) 0.011(3) 0.003(4) 0.013(3) C46 0.048(5) 0.021(4) 0.023(4) 0.009(3) 0.003(3) -0.001(3) Br2 0.0451(4) 0.0375(4) 0.0195(4) 0.0092(3) 0.0097(3) 0.0230(3) C1S 0.047(5) 0.080(7) 0.055(6) 0.013(5) 0.022(5) 0.026(5) O1S 0.055(4) 0.065(4) 0.026(3) 0.006(3) 0.012(3) 0.013(3) C2S 0.026(4) 0.068(6) 0.025(4) 0.007(4) 0.013(3) 0.010(4) C3S 0.030(5) 0.090(7) 0.026(4) 0.004(4) -0.004(3) 0.017(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 N4 2.070(5) . ? Pd1 P7 2.2991(19) . ? Pd1 P1 2.3008(19) . ? Pd1 Br1 2.4179(11) . ? P1 C21 1.807(7) . ? P1 C11 1.819(7) . ? P1 C2 1.828(7) . ? C11 C16 1.386(9) . ? C11 C12 1.396(9) . ? C12 C13 1.406(10) . ? C13 C14 1.366(11) . ? C14 C15 1.381(9) . ? C15 C16 1.398(9) . ? C21 C22 1.392(10) . ? C21 C26 1.394(9) . ? C22 C23 1.388(10) . ? C23 C24 1.394(10) . ? C24 C25 1.386(10) . ? C25 C26 1.381(10) . ? C2 C3 1.502(11) . ? C3 N4 1.491(8) . ? N4 C5 1.474(9) . ? C5 C6 1.524(9) . ? C6 P7 1.834(6) . ? P7 C41 1.807(6) . ? P7 C31 1.807(7) . ? C31 C32 1.385(9) . ? C31 C36 1.405(9) . ? C32 C33 1.369(10) . ? C33 C34 1.407(11) . ? C34 C35 1.368(10) . ? C35 C36 1.389(9) . ? C41 C42 1.393(9) . ? C41 C46 1.415(9) . ? C42 C43 1.374(9) . ? C43 C44 1.375(9) . ? C44 C45 1.386(10) . ? C45 C46 1.394(10) . ? C1S C2S 1.491(12) . ? O1S C2S 1.216(8) . ? C2S C3S 1.503(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 N4 Pd1 P7 84.51(17) . . ? N4 Pd1 P1 84.27(17) . . ? P7 Pd1 P1 168.76(6) . . ? N4 Pd1 Br1 177.39(14) . . ? P7 Pd1 Br1 94.87(5) . . ? P1 Pd1 Br1 96.37(5) . . ? C21 P1 C11 105.5(3) . . ? C21 P1 C2 106.2(3) . . ? C11 P1 C2 107.7(3) . . ? C21 P1 Pd1 119.1(2) . . ? C11 P1 Pd1 116.9(2) . . ? C2 P1 Pd1 100.3(3) . . ? C16 C11 C12 120.2(6) . . ? C16 C11 P1 120.2(5) . . ? C12 C11 P1 119.6(5) . . ? C11 C12 C13 118.9(7) . . ? C14 C13 C12 120.6(7) . . ? C13 C14 C15 120.5(7) . . ? C14 C15 C16 119.9(7) . . ? C11 C16 C15 119.8(6) . . ? C22 C21 C26 119.0(7) . . ? C22 C21 P1 120.6(5) . . ? C26 C21 P1 120.2(6) . . ? C23 C22 C21 121.0(6) . . ? C22 C23 C24 119.3(7) . . ? C25 C24 C23 119.7(7) . . ? C26 C25 C24 120.8(7) . . ? C25 C26 C21 120.0(7) . . ? C3 C2 P1 108.3(5) . . ? N4 C3 C2 109.1(5) . . ? C5 N4 C3 113.1(5) . . ? C5 N4 Pd1 113.7(4) . . ? C3 N4 Pd1 112.9(4) . . ? N4 C5 C6 108.6(5) . . ? C5 C6 P7 107.3(4) . . ? C41 P7 C31 108.5(3) . . ? C41 P7 C6 105.4(3) . . ? C31 P7 C6 106.0(3) . . ? C41 P7 Pd1 118.5(2) . . ? C31 P7 Pd1 116.9(2) . . ? C6 P7 Pd1 99.7(2) . . ? C32 C31 C36 119.5(6) . . ? C32 C31 P7 120.9(5) . . ? C36 C31 P7 119.5(5) . . ? C33 C32 C31 120.8(7) . . ? C32 C33 C34 119.9(7) . . ? C35 C34 C33 119.5(7) . . ? C34 C35 C36 121.1(7) . . ? C35 C36 C31 119.1(7) . . ? C42 C41 C46 118.9(6) . . ? C42 C41 P7 118.9(5) . . ? C46 C41 P7 122.2(5) . . ? C43 C42 C41 120.0(6) . . ? C42 C43 C44 121.5(7) . . ? C43 C44 C45 120.0(6) . . ? C44 C45 C46 119.7(7) . . ? C45 C46 C41 119.9(6) . . ? O1S C2S C1S 121.9(8) . . ? O1S C2S C3S 120.1(8) . . ? C1S C2S C3S 118.0(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.09 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.237 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.135 #CIF file of Au2(PN(NO)P)Cl2 (5a) data_aupni6 _database_code_CSD 181549 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 Au2 Cl2 N2 O P2' _chemical_formula_weight 935.30 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' 'Au' 'Au' -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.120(3) _cell_length_b 12.871(3) _cell_length_c 16.849(3) _cell_angle_alpha 90.00 _cell_angle_beta 109.72(3) _cell_angle_gamma 90.00 _cell_volume 2882.5(10) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 46 _cell_measurement_theta_min 12 _cell_measurement_theta_max 13 _exptl_crystal_description chip _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1760 _exptl_absorpt_coefficient_mu 10.489 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_correction_T_min 0.3013 _exptl_absorpt_correction_T_max 0.4544 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _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 'Stoe Stadi-4' _diffrn_measurement_method '\q\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 2 _diffrn_reflns_number 5066 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5066 _reflns_number_gt 3323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material CIFTAB _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^)+(0.0455P)^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 5066 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.0963 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _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_multiplicit _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.05673(4) -0.54013(4) 0.16141(3) 0.03030(16) Uani 1 1 d . . . Cl1 Cl 0.2055(3) -0.6289(3) 0.1838(2) 0.0363(9) Uani 1 1 d . . . P1 P -0.0805(3) -0.4399(3) 0.1272(2) 0.0242(8) Uani 1 1 d . . . C11 C -0.1617(10) -0.4606(11) 0.0207(8) 0.033(3) Uani 1 1 d . . . H11A H -0.2127 -0.4067 0.0052 0.039 Uiso 1 1 calc R . . H11B H -0.1226 -0.4551 -0.0167 0.039 Uiso 1 1 calc R . . C12 C -0.2137(10) -0.5678(10) 0.0083(8) 0.030(3) Uani 1 1 d . . . H12A H -0.1643 -0.6211 0.0341 0.036 Uiso 1 1 calc R . . H12B H -0.2639 -0.5684 0.0358 0.036 Uiso 1 1 calc R . . C1A1 C -0.1589(10) -0.4592(10) 0.1918(8) 0.027(3) Uani 1 1 d . . . C1A2 C -0.2440(11) -0.3946(15) 0.1795(9) 0.052(5) Uani 1 1 d . . . H1A2 H -0.2599 -0.3417 0.1395 0.062 Uiso 1 1 calc R . . C1A3 C -0.3024(11) -0.4133(16) 0.2290(10) 0.055(5) Uani 1 1 d . . . H1A3 H -0.3601 -0.3734 0.2196 0.066 Uiso 1 1 calc R . . C1A4 C -0.2814(12) -0.4851(14) 0.2896(10) 0.049(5) Uani 1 1 d . . . H1A4 H -0.3215 -0.4934 0.3231 0.059 Uiso 1 1 calc R . . C1A5 C -0.1984(14) -0.5463(13) 0.3005(10) 0.055(5) Uani 1 1 d . . . H1A5 H -0.1835 -0.5992 0.3405 0.066 Uiso 1 1 calc R . . C1A6 C -0.1365(12) -0.5307(12) 0.2532(9) 0.042(4) Uani 1 1 d . . . H1A6 H -0.0785 -0.5704 0.2641 0.050 Uiso 1 1 calc R . . C1B1 C -0.0492(9) -0.3040(10) 0.1317(8) 0.022(3) Uani 1 1 d . . . C1B2 C -0.0072(11) -0.2586(12) 0.2070(9) 0.040(4) Uani 1 1 d . . . H1B2 H 0.0030 -0.2978 0.2555 0.048 Uiso 1 1 calc R . . C1B3 C 0.0221(10) -0.1527(13) 0.2150(10) 0.040(4) Uani 1 1 d . . . H1B3 H 0.0509 -0.1220 0.2677 0.049 Uiso 1 1 calc R . . C1B4 C 0.0066(11) -0.0977(12) 0.1431(11) 0.045(4) Uani 1 1 d . . . H1B4 H 0.0247 -0.0279 0.1468 0.055 Uiso 1 1 calc R . . C1B5 C -0.0346(12) -0.1419(13) 0.0659(11) 0.053(5) Uani 1 1 d . . . H1B5 H -0.0436 -0.1031 0.0173 0.063 Uiso 1 1 calc R . . C1B6 C -0.0629(11) -0.2442(12) 0.0604(9) 0.042(4) Uani 1 1 d . . . H1B6 H -0.0919 -0.2741 0.0075 0.050 Uiso 1 1 calc R . . N1 N -0.2616(8) -0.5905(8) -0.0813(6) 0.024(2) Uani 1 1 d . . . N2 N -0.3447(10) -0.5438(10) -0.1319(9) 0.045(3) Uani 1 1 d . . . O3 O -0.3767(7) -0.4822(8) -0.0945(6) 0.042(3) Uani 1 1 d . . . Au2 Au -0.45716(4) -0.76175(4) -0.24478(3) 0.02791(16) Uani 1 1 d . . . Cl2 Cl -0.5561(3) -0.6955(3) -0.3722(2) 0.0401(9) Uani 1 1 d . . . P2 P -0.3550(3) -0.8165(3) -0.1186(2) 0.0243(8) Uani 1 1 d . . . C21 C -0.2280(10) -0.7736(10) -0.1013(8) 0.028(3) Uani 1 1 d . . . H21A H -0.1887 -0.7830 -0.0422 0.034 Uiso 1 1 calc R . . H21B H -0.1988 -0.8175 -0.1338 0.034 Uiso 1 1 calc R . . C22 C -0.2193(9) -0.6626(9) -0.1246(8) 0.020(3) Uani 1 1 d . . . H22A H -0.1488 -0.6461 -0.1124 0.024 Uiso 1 1 calc R . . H22B H -0.2529 -0.6545 -0.1849 0.024 Uiso 1 1 calc R . . C2A1 C -0.3466(9) -0.9554(11) -0.1022(7) 0.026(3) Uani 1 1 d . . . C2A2 C -0.4079(11) -1.0051(12) -0.0656(9) 0.039(4) Uani 1 1 d . . . H2A2 H -0.4527 -0.9670 -0.0475 0.046 Uiso 1 1 calc R . . C2A3 C -0.4023(12) -1.1118(13) -0.0560(10) 0.045(4) Uani 1 1 d . . . H2A3 H -0.4440 -1.1448 -0.0313 0.054 Uiso 1 1 calc R . . C2A4 C -0.3384(11) -1.1693(12) -0.0813(10) 0.043(4) Uani 1 1 d . . . H2A4 H -0.3361 -1.2411 -0.0743 0.051 Uiso 1 1 calc R . . C2A5 C -0.2765(14) -1.1210(12) -0.1177(10) 0.051(5) Uani 1 1 d . . . H2A5 H -0.2332 -1.1603 -0.1367 0.062 Uiso 1 1 calc R . . C2A6 C -0.2785(11) -1.0157(11) -0.1259(9) 0.040(4) Uani 1 1 d . . . H2A6 H -0.2336 -0.9834 -0.1476 0.048 Uiso 1 1 calc R . . C2B1 C -0.3888(9) -0.7628(10) -0.0325(8) 0.025(3) Uani 1 1 d . . . C2B2 C -0.3319(10) -0.7832(11) 0.0503(8) 0.031(3) Uani 1 1 d . . . H2B2 H -0.2790 -0.8304 0.0625 0.038 Uiso 1 1 calc R . . C2B4 C -0.4308(12) -0.6632(12) 0.0973(9) 0.040(4) Uani 1 1 d . . . H2B4 H -0.4443 -0.6290 0.1410 0.047 Uiso 1 1 calc R . . C2B3 C -0.3534(10) -0.7333(13) 0.1156(8) 0.039(4) Uani 1 1 d . . . H2B3 H -0.3154 -0.7475 0.1713 0.047 Uiso 1 1 calc R . . C2B5 C -0.4894(11) -0.6425(11) 0.0143(9) 0.037(4) Uani 1 1 d . . . H2B5 H -0.5425 -0.5956 0.0021 0.044 Uiso 1 1 calc R . . C2B6 C -0.4675(10) -0.6925(11) -0.0496(9) 0.033(3) Uani 1 1 d . . . H2B6 H -0.5062 -0.6789 -0.1053 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 Au1 0.0347(3) 0.0290(3) 0.0283(3) 0.0055(3) 0.0121(2) 0.0022(3) Cl1 0.036(2) 0.039(2) 0.034(2) 0.0088(17) 0.0125(17) 0.0067(17) P1 0.0280(19) 0.022(2) 0.0199(18) -0.0016(15) 0.0047(15) 0.0046(16) C11 0.044(8) 0.037(9) 0.021(7) -0.009(7) 0.016(6) 0.001(8) C12 0.039(8) 0.024(8) 0.022(7) -0.007(6) 0.004(6) -0.009(7) C1A1 0.032(7) 0.021(7) 0.027(7) -0.009(6) 0.008(6) -0.004(7) C1A2 0.043(10) 0.086(14) 0.027(9) 0.015(9) 0.012(8) 0.029(10) C1A3 0.021(8) 0.114(17) 0.030(9) -0.004(10) 0.009(7) 0.007(9) C1A4 0.042(10) 0.076(13) 0.041(10) -0.034(10) 0.030(8) -0.031(10) C1A5 0.084(14) 0.042(11) 0.049(11) 0.012(9) 0.036(10) -0.007(10) C1A6 0.058(10) 0.038(9) 0.037(9) 0.004(8) 0.026(8) 0.013(8) C1B1 0.021(7) 0.027(7) 0.022(7) 0.003(6) 0.014(6) 0.005(6) C1B2 0.050(9) 0.045(10) 0.028(8) -0.002(8) 0.017(7) -0.002(8) C1B3 0.030(8) 0.047(10) 0.044(10) -0.020(9) 0.011(7) -0.011(8) C1B4 0.046(10) 0.030(9) 0.064(12) -0.028(9) 0.024(9) -0.019(8) C1B5 0.060(11) 0.037(10) 0.052(11) 0.022(9) 0.006(9) 0.006(9) C1B6 0.053(10) 0.032(9) 0.029(8) 0.000(7) -0.001(7) -0.011(8) N1 0.021(6) 0.019(6) 0.026(6) -0.003(5) -0.001(5) -0.004(5) N2 0.064(9) 0.024(7) 0.059(9) 0.002(7) 0.036(8) 0.001(7) O3 0.039(6) 0.050(7) 0.038(6) 0.008(5) 0.014(5) 0.006(5) Au2 0.0308(3) 0.0251(3) 0.0242(3) -0.0046(3) 0.0045(2) 0.0001(3) Cl2 0.045(2) 0.039(2) 0.0264(19) -0.0019(17) -0.0017(17) 0.0011(18) P2 0.0249(19) 0.023(2) 0.0212(18) -0.0044(15) 0.0030(15) -0.0005(16) C21 0.030(7) 0.034(8) 0.023(7) -0.008(6) 0.012(6) 0.005(7) C22 0.018(6) 0.023(7) 0.019(7) -0.005(6) 0.006(5) -0.003(6) C2A1 0.028(7) 0.027(8) 0.014(6) -0.004(6) -0.003(6) -0.007(7) C2A2 0.034(9) 0.040(10) 0.043(9) -0.011(8) 0.013(7) 0.004(7) C2A3 0.045(10) 0.049(11) 0.043(10) 0.010(8) 0.016(8) -0.012(9) C2A4 0.047(10) 0.019(8) 0.049(10) 0.000(8) 0.000(8) 0.007(8) C2A5 0.075(13) 0.030(9) 0.044(10) 0.006(8) 0.013(9) 0.015(9) C2A6 0.049(10) 0.030(9) 0.046(10) 0.004(7) 0.021(8) 0.006(8) C2B1 0.031(7) 0.025(7) 0.020(7) 0.003(6) 0.009(6) -0.006(6) C2B2 0.037(8) 0.032(8) 0.033(8) 0.007(7) 0.021(7) 0.004(7) C2B4 0.066(11) 0.035(9) 0.035(9) -0.002(7) 0.041(9) -0.005(8) C2B3 0.030(8) 0.063(11) 0.018(7) -0.002(8) 0.001(6) -0.018(8) C2B5 0.045(9) 0.022(8) 0.049(10) 0.006(7) 0.025(8) 0.010(7) C2B6 0.041(9) 0.035(9) 0.025(8) -0.002(7) 0.013(7) 0.013(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 Au1 P1 2.236(3) . ? Au1 Cl1 2.308(4) . ? Au1 Au2 3.0412(9) 4_646 ? P1 C11 1.794(13) . ? P1 C1B1 1.799(13) . ? P1 C1A1 1.812(13) . ? C11 C12 1.544(18) . ? C12 N1 1.460(15) . ? C1A1 C1A6 1.339(19) . ? C1A1 C1A2 1.418(19) . ? C1A2 C1A3 1.38(2) . ? C1A3 C1A4 1.33(2) . ? C1A4 C1A5 1.37(2) . ? C1A5 C1A6 1.38(2) . ? C1B1 C1B2 1.339(18) . ? C1B1 C1B6 1.386(18) . ? C1B2 C1B3 1.42(2) . ? C1B3 C1B4 1.36(2) . ? C1B4 C1B5 1.36(2) . ? C1B5 C1B6 1.37(2) . ? N1 N2 1.338(16) . ? N1 C22 1.431(15) . ? N2 O3 1.193(14) . ? Au2 P2 2.243(4) . ? Au2 Cl2 2.295(4) . ? Au2 Au1 3.0412(9) 4_545 ? P2 C21 1.804(13) . ? P2 C2A1 1.808(14) . ? P2 C2B1 1.809(13) . ? C21 C22 1.497(17) . ? C2A1 C2A2 1.378(18) . ? C2A1 C2A6 1.394(18) . ? C2A2 C2A3 1.38(2) . ? C2A3 C2A4 1.34(2) . ? C2A4 C2A5 1.37(2) . ? C2A5 C2A6 1.36(2) . ? C2B1 C2B2 1.380(17) . ? C2B1 C2B6 1.386(18) . ? C2B2 C2B3 1.394(18) . ? C2B4 C2B3 1.37(2) . ? C2B4 C2B5 1.39(2) . ? C2B5 C2B6 1.376(18) . ? 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 Au1 Cl1 171.82(13) . . ? P1 Au1 Au2 114.56(9) . 4_646 ? Cl1 Au1 Au2 73.44(9) . 4_646 ? C11 P1 C1B1 104.6(6) . . ? C11 P1 C1A1 105.5(6) . . ? C1B1 P1 C1A1 107.4(6) . . ? C11 P1 Au1 112.2(5) . . ? C1B1 P1 Au1 111.7(4) . . ? C1A1 P1 Au1 114.7(5) . . ? C12 C11 P1 112.5(9) . . ? N1 C12 C11 110.6(10) . . ? C1A6 C1A1 C1A2 118.9(13) . . ? C1A6 C1A1 P1 121.7(11) . . ? C1A2 C1A1 P1 119.4(11) . . ? C1A3 C1A2 C1A1 117.4(15) . . ? C1A4 C1A3 C1A2 124.1(16) . . ? C1A3 C1A4 C1A5 117.4(14) . . ? C1A4 C1A5 C1A6 121.1(16) . . ? C1A1 C1A6 C1A5 121.0(15) . . ? C1B2 C1B1 C1B6 117.8(13) . . ? C1B2 C1B1 P1 119.2(11) . . ? C1B6 C1B1 P1 122.9(10) . . ? C1B1 C1B2 C1B3 122.1(14) . . ? C1B4 C1B3 C1B2 117.6(14) . . ? C1B3 C1B4 C1B5 121.7(15) . . ? C1B4 C1B5 C1B6 119.2(15) . . ? C1B5 C1B6 C1B1 121.5(14) . . ? N2 N1 C22 113.1(10) . . ? N2 N1 C12 124.8(11) . . ? C22 N1 C12 122.0(11) . . ? O3 N2 N1 111.6(13) . . ? P2 Au2 Cl2 176.20(13) . . ? P2 Au2 Au1 95.50(9) . 4_545 ? Cl2 Au2 Au1 87.20(10) . 4_545 ? C21 P2 C2A1 105.5(6) . . ? C21 P2 C2B1 105.7(6) . . ? C2A1 P2 C2B1 106.1(6) . . ? C21 P2 Au2 110.1(5) . . ? C2A1 P2 Au2 116.3(4) . . ? C2B1 P2 Au2 112.4(4) . . ? C22 C21 P2 114.5(9) . . ? N1 C22 C21 113.6(10) . . ? C2A2 C2A1 C2A6 117.9(13) . . ? C2A2 C2A1 P2 120.6(11) . . ? C2A6 C2A1 P2 121.5(11) . . ? C2A1 C2A2 C2A3 119.6(14) . . ? C2A4 C2A3 C2A2 121.9(15) . . ? C2A3 C2A4 C2A5 119.3(15) . . ? C2A6 C2A5 C2A4 120.1(16) . . ? C2A5 C2A6 C2A1 121.1(15) . . ? C2B2 C2B1 C2B6 119.1(12) . . ? C2B2 C2B1 P2 121.1(10) . . ? C2B6 C2B1 P2 119.5(10) . . ? C2B1 C2B2 C2B3 120.2(13) . . ? C2B3 C2B4 C2B5 120.7(13) . . ? C2B4 C2B3 C2B2 119.8(13) . . ? C2B6 C2B5 C2B4 118.9(13) . . ? C2B5 C2B6 C2B1 121.3(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.866 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.230