Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Orla M. Ni Dhubhghaill' _publ_contact_author_address ; Department of Chemistry University College Cork Cork REPUBLIC OF IRELAND ; _publ_contact_author_email O.NIDHUBHGHAILL@UCC.IE _publ_section_title ; Palladium(II) and Platinum(II) Complexes with Tridentate Iminophosphine Ligands; Synthesis and Structural Studies ; _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; loop_ _publ_author_name 'Orla M. Ni Dhubhghaill' 'M. Drew' 'Joanne Lennon' data_3 _database_code_depnum_ccdc_archive 'CCDC 249207' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H18 Br Cl N O P Pd' _chemical_formula_weight 601.13 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' Pd Pd -0.9988 1.0072 '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' Cl Cl 0.1484 0.1585 '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 12.193(14) _cell_length_b 12.369(14) _cell_length_c 15.176(16) _cell_angle_alpha 90.00 _cell_angle_beta 99.035(10) _cell_angle_gamma 90.00 _cell_volume 2260(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 25.98 _exptl_crystal_description parallelopiped _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 2.796 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.158 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_interval_count ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12226 _diffrn_reflns_av_R_equivalents 0.1328 _diffrn_reflns_av_sigmaI/netI 0.1066 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 25.94 _reflns_number_total 4346 _reflns_number_observed 3667 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.0763P)^2^+4.9394P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0067(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4346 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_obs 0.0718 _refine_ls_wR_factor_all 0.1748 _refine_ls_wR_factor_obs 0.1658 _refine_ls_goodness_of_fit_all 1.117 _refine_ls_goodness_of_fit_obs 1.157 _refine_ls_restrained_S_all 1.117 _refine_ls_restrained_S_obs 1.157 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly #_atom_site_disorder_group Pd1 Pd 0.14588(4) 0.73822(4) 0.37841(3) 0.0183(2) Uani 1 d . . Br45 Br -0.41371(7) 0.96576(9) 0.23423(7) 0.0554(3) Uani 1 d . . P1 P 0.23379(14) 0.59112(15) 0.34731(11) 0.0215(4) Uani 1 d . . Cl1 Cl 0.2515(2) 0.7515(2) 0.51853(12) 0.0368(5) Uani 1 d . . N41 N 0.0568(5) 0.7174(5) 0.2558(4) 0.0236(12) Uani 1 d . . N42 C -0.0420(6) 0.7561(6) 0.2367(5) 0.026(2) Uani 1 d . . O49 O 0.0555(4) 0.8721(4) 0.4020(3) 0.0290(11) Uani 1 d . . C11 C 0.3829(6) 0.5909(6) 0.3642(5) 0.029(2) Uani 1 d . . C12 C 0.4454(7) 0.4982(8) 0.3850(6) 0.042(2) Uani 1 d . . C13 C 0.5601(7) 0.5022(10) 0.3901(6) 0.052(3) Uani 1 d . . C14 C 0.6110(8) 0.5972(12) 0.3728(7) 0.065(3) Uani 1 d . . C15 C 0.5502(9) 0.6876(11) 0.3548(8) 0.068(3) Uani 1 d . . C16 C 0.4369(7) 0.6884(9) 0.3498(7) 0.051(2) Uani 1 d . . C21 C 0.1864(6) 0.4689(6) 0.3945(5) 0.0256(15) Uani 1 d . . C22 C 0.1861(7) 0.3689(7) 0.3497(6) 0.039(2) Uani 1 d . . C23 C 0.1434(10) 0.2785(7) 0.3844(7) 0.053(3) Uani 1 d . . C24 C 0.0979(9) 0.2833(8) 0.4633(6) 0.052(3) Uani 1 d . . C25 C 0.1009(8) 0.3797(8) 0.5071(6) 0.045(2) Uani 1 d . . C26 C 0.1438(6) 0.4730(7) 0.4739(5) 0.031(2) Uani 1 d . . C31 C 0.1912(6) 0.5835(5) 0.2271(4) 0.0218(14) Uani 1 d . . C32 C 0.2402(7) 0.5190(7) 0.1698(5) 0.032(2) Uani 1 d . . C33 C 0.2028(8) 0.5204(7) 0.0795(5) 0.040(2) Uani 1 d . . C34 C 0.1160(8) 0.5862(7) 0.0456(5) 0.039(2) Uani 1 d . . C35 C 0.0650(7) 0.6536(7) 0.1025(5) 0.033(2) Uani 1 d . . C36 C 0.1028(6) 0.6512(6) 0.1930(4) 0.0227(14) Uani 1 d . . C43 C -0.0979(5) 0.8318(5) 0.2845(4) 0.0205(14) Uani 1 d . . C44 C -0.2090(6) 0.8556(6) 0.2495(5) 0.027(2) Uani 1 d . . C45 C -0.2632(6) 0.9373(7) 0.2827(5) 0.032(2) Uani 1 d . . C46 C -0.2098(7) 1.0014(7) 0.3515(5) 0.037(2) Uani 1 d . . C47 C -0.1030(7) 0.9799(7) 0.3882(5) 0.037(2) Uani 1 d . . C48 C -0.0431(6) 0.8929(6) 0.3592(4) 0.0217(14) Uani 1 d . . H12 H 0.4107(7) 0.4336(8) 0.3955(6) 0.050 Uiso 1 calc R . H13 H 0.6024(7) 0.4405(10) 0.4053(6) 0.062 Uiso 1 calc R . H14 H 0.6873(8) 0.5990(12) 0.3734(7) 0.078 Uiso 1 calc R . H15 H 0.5863(9) 0.7519(11) 0.3455(8) 0.082 Uiso 1 calc R . H16 H 0.3967(7) 0.7519(9) 0.3373(7) 0.062 Uiso 1 calc R . H22 H 0.2149(7) 0.3642(7) 0.2967(6) 0.047 Uiso 1 calc R . H23 H 0.1447(10) 0.2128(7) 0.3549(7) 0.063 Uiso 1 calc R . H24 H 0.0665(9) 0.2225(8) 0.4853(6) 0.063 Uiso 1 calc R . H25 H 0.0735(8) 0.3833(8) 0.5609(6) 0.055 Uiso 1 calc R . H26 H 0.1438(6) 0.5378(7) 0.5049(5) 0.037 Uiso 1 calc R . H32 H 0.2992(7) 0.4743(7) 0.1926(5) 0.038 Uiso 1 calc R . H33 H 0.2363(8) 0.4767(7) 0.0415(5) 0.048 Uiso 1 calc R . H34 H 0.0904(8) 0.5865(7) -0.0155(5) 0.047 Uiso 1 calc R . H35 H 0.0068(7) 0.6989(7) 0.0792(5) 0.040 Uiso 1 calc R . H42 H -0.0829(6) 0.7309(6) 0.1838(5) 0.031 Uiso 1 calc R . H44 H -0.2456(6) 0.8143(6) 0.2028(5) 0.033 Uiso 1 calc R . H46 H -0.2472(7) 1.0592(7) 0.3725(5) 0.045 Uiso 1 calc R . H47 H -0.0684(7) 1.0239(7) 0.4340(5) 0.044 Uiso 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(3) 0.0149(3) 0.0186(3) -0.0009(2) -0.0036(2) 0.0023(2) Br45 0.0292(5) 0.0582(7) 0.0739(7) -0.0047(5) -0.0068(4) 0.0226(5) Cl1 0.0458(12) 0.0324(10) 0.0254(9) -0.0024(7) -0.0156(8) 0.0035(9) P1 0.0186(8) 0.0212(9) 0.0234(8) 0.0020(7) -0.0006(6) 0.0055(7) N41 0.025(3) 0.020(3) 0.025(3) 0.003(2) 0.004(2) 0.000(3) N42 0.027(4) 0.028(4) 0.022(3) -0.007(3) -0.002(3) 0.001(3) O49 0.032(3) 0.020(2) 0.031(3) -0.010(2) -0.006(2) 0.004(2) C11 0.022(3) 0.030(4) 0.033(4) -0.002(3) -0.002(3) 0.003(3) C12 0.032(4) 0.044(5) 0.048(5) -0.003(4) 0.004(4) 0.009(4) C13 0.027(4) 0.071(7) 0.054(5) -0.017(5) -0.003(4) 0.023(5) C14 0.024(4) 0.108(11) 0.064(7) -0.009(7) 0.006(4) -0.002(6) C15 0.035(5) 0.071(8) 0.096(9) 0.011(7) 0.001(5) -0.004(6) C16 0.027(4) 0.056(6) 0.069(6) 0.020(5) -0.003(4) -0.002(5) C21 0.019(3) 0.022(4) 0.035(4) 0.006(3) 0.000(3) 0.003(3) C22 0.045(5) 0.029(4) 0.045(5) 0.005(4) 0.016(4) 0.004(4) C23 0.080(8) 0.020(4) 0.063(6) 0.001(4) 0.027(6) -0.001(5) C24 0.071(7) 0.035(5) 0.054(6) 0.017(4) 0.017(5) -0.001(5) C25 0.045(5) 0.045(5) 0.049(5) 0.006(4) 0.017(4) -0.011(5) C26 0.029(4) 0.032(4) 0.032(4) -0.002(3) 0.006(3) -0.001(4) C31 0.023(3) 0.018(3) 0.024(3) -0.002(3) 0.005(3) 0.001(3) C32 0.030(4) 0.034(4) 0.032(4) -0.002(3) 0.010(3) 0.003(4) C33 0.056(5) 0.040(5) 0.027(4) -0.008(3) 0.016(4) 0.012(4) C34 0.053(5) 0.044(5) 0.019(3) -0.006(3) 0.004(3) 0.011(4) C35 0.036(4) 0.040(4) 0.020(3) -0.005(3) -0.007(3) 0.015(4) C36 0.024(3) 0.022(3) 0.024(3) -0.003(3) 0.008(3) -0.001(3) C43 0.019(3) 0.019(3) 0.023(3) 0.000(3) 0.002(3) 0.009(3) C44 0.023(4) 0.025(4) 0.030(4) -0.001(3) -0.007(3) 0.004(3) C45 0.024(4) 0.042(5) 0.031(4) 0.001(3) 0.008(3) 0.013(4) C46 0.047(5) 0.033(4) 0.033(4) 0.003(3) 0.009(3) 0.025(4) C47 0.046(5) 0.030(4) 0.031(4) -0.010(3) -0.006(3) 0.018(4) C48 0.023(3) 0.022(3) 0.017(3) -0.001(3) -0.005(2) 0.002(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 N41 2.018(6) . ? Pd1 O49 2.051(5) . ? Pd1 P1 2.200(3) . ? Pd1 Cl1 2.312(3) . ? N42 N41 1.287(10) . ? N42 C43 1.423(9) . ? C43 C44 1.406(9) . ? C43 C48 1.436(9) . ? C44 C45 1.347(10) . ? C45 C46 1.389(12) . ? C45 Br45 1.900(8) . ? C46 C47 1.360(12) . ? C47 C48 1.410(10) . ? C48 O49 1.300(8) . ? N41 C36 1.435(9) . ? P1 C11 1.796(8) . ? P1 C21 1.806(7) . ? P1 C31 1.819(7) . ? C31 C32 1.383(10) . ? C31 C36 1.399(10) . ? C36 C35 1.379(10) . ? C35 C34 1.413(10) . ? C34 C33 1.370(12) . ? C33 C32 1.375(11) . ? C11 C12 1.385(12) . ? C11 C16 1.407(13) . ? C12 C13 1.389(12) . ? C13 C14 1.37(2) . ? C14 C15 1.35(2) . ? C15 C16 1.372(13) . ? C21 C26 1.386(10) . ? C21 C22 1.411(11) . ? C22 C23 1.373(12) . ? C23 C24 1.398(12) . ? C24 C25 1.362(13) . ? C25 C26 1.394(12) . ? 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 N41 Pd1 O49 92.2(2) . . ? N41 Pd1 P1 84.6(2) . . ? O49 Pd1 P1 176.45(14) . . ? N41 Pd1 Cl1 176.6(2) . . ? O49 Pd1 Cl1 91.08(15) . . ? P1 Pd1 Cl1 92.08(8) . . ? N41 N42 C43 129.5(6) . . ? C44 C43 N42 117.1(6) . . ? C44 C43 C48 119.3(6) . . ? N42 C43 C48 123.2(6) . . ? C45 C44 C43 121.1(7) . . ? C44 C45 C46 120.6(7) . . ? C44 C45 Br45 119.7(6) . . ? C46 C45 Br45 119.7(6) . . ? C47 C46 C45 120.1(7) . . ? C46 C47 C48 122.1(7) . . ? O49 C48 C47 118.6(6) . . ? O49 C48 C43 124.7(6) . . ? C47 C48 C43 116.7(6) . . ? N42 N41 C36 120.8(6) . . ? N42 N41 Pd1 120.7(5) . . ? C36 N41 Pd1 118.3(5) . . ? C48 O49 Pd1 123.5(4) . . ? C11 P1 C21 108.8(3) . . ? C11 P1 C31 105.4(3) . . ? C21 P1 C31 107.2(3) . . ? C11 P1 Pd1 119.2(3) . . ? C21 P1 Pd1 114.2(3) . . ? C31 P1 Pd1 100.7(2) . . ? C32 C31 C36 119.8(6) . . ? C32 C31 P1 125.2(6) . . ? C36 C31 P1 115.0(5) . . ? C35 C36 C31 119.9(6) . . ? C35 C36 N41 123.0(7) . . ? C31 C36 N41 117.0(6) . . ? C36 C35 C34 119.1(7) . . ? C33 C34 C35 120.6(7) . . ? C32 C33 C34 119.9(7) . . ? C31 C32 C33 120.7(7) . . ? C12 C11 C16 119.4(7) . . ? C12 C11 P1 122.8(6) . . ? C16 C11 P1 117.7(6) . . ? C13 C12 C11 119.7(9) . . ? C14 C13 C12 120.1(10) . . ? C15 C14 C13 120.0(9) . . ? C14 C15 C16 122.3(12) . . ? C15 C16 C11 118.5(10) . . ? C26 C21 C22 118.5(7) . . ? C26 C21 P1 120.1(6) . . ? C22 C21 P1 121.3(6) . . ? C23 C22 C21 120.1(8) . . ? C22 C23 C24 121.3(9) . . ? C25 C24 C23 118.1(8) . . ? C24 C25 C26 122.0(8) . . ? C21 C26 C25 119.8(8) . . ? _refine_diff_density_max 1.649 _refine_diff_density_min -1.452 _refine_diff_density_rms 0.177 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_15 _database_code_depnum_ccdc_archive 'CCDC 249208' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H33 Br Cl N O5 P2 Pd' _chemical_formula_weight 927.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Pd Pd -0.9988 1.0072 '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' Cl Cl 0.1484 0.1585 '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 16.035(17) _cell_length_b 15.835(17) _cell_length_c 16.354(17) _cell_angle_alpha 90.00 _cell_angle_beta 107.699(10) _cell_angle_gamma 90.00 _cell_volume 3956(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 25.89 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.674 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11095 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.89 _reflns_number_total 6963 _reflns_number_gt 4079 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.2000P)^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 0.0003(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6963 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1344 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2448 _refine_ls_wR_factor_gt 0.1970 _refine_ls_goodness_of_fit_ref 0.856 _refine_ls_restrained_S_all 0.856 _refine_ls_shift/su_max 0.011 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.59330(3) 0.17113(3) 0.88454(4) 0.0441(3) Uani 1 d . . . Br45 Br 0.33655(10) -0.20818(8) 0.68044(10) 0.1153(6) Uani 1 d . . . P1 P 0.59489(12) 0.26703(12) 0.98365(13) 0.0469(5) Uani 1 d . . . P2 P 0.69930(12) 0.22805(12) 0.83258(13) 0.0470(5) Uani 1 d . . . Cl1 Cl 0.19449(16) 0.02104(17) 0.89860(19) 0.0810(7) Uani 1 d . . . N41 N 0.4949(3) 0.1153(3) 0.9238(4) 0.0414(13) Uani 1 d . . . O11 O 0.1249(5) -0.0390(6) 0.8823(7) 0.117(3) Uani 1 d . . . O12 O 0.2108(14) 0.0445(15) 0.8268(10) 0.277(11) Uani 1 d . . . O13 O 0.2706(7) -0.0208(7) 0.9379(16) 0.260(12) Uani 1 d . . . O14 O 0.1885(8) 0.0836(7) 0.9521(10) 0.175(6) Uani 1 d . . . O49 O 0.5799(4) 0.0861(3) 0.7886(4) 0.0622(14) Uani 1 d . . . C16 C 0.7047(6) 0.3608(6) 1.1177(7) 0.072(3) Uani 1 d . . . C11 C 0.6911(5) 0.2856(5) 1.0716(5) 0.055(2) Uani 1 d . . . C12 C 0.7500(5) 0.2210(5) 1.0984(6) 0.060(2) Uani 1 d . . . C13 C 0.8216(6) 0.2309(7) 1.1690(6) 0.077(3) Uani 1 d . . . C14 C 0.8391(7) 0.3041(9) 1.2122(8) 0.100(4) Uani 1 d . . . C15 C 0.7791(7) 0.3661(8) 1.1904(8) 0.102(4) Uani 1 d . . . C21 C 0.5460(6) 0.3646(5) 0.9341(6) 0.061(2) Uani 1 d . . . C22 C 0.5930(6) 0.4357(5) 0.9300(7) 0.075(3) Uani 1 d . . . C23 C 0.5580(10) 0.5055(6) 0.8819(9) 0.101(4) Uani 1 d . . . C24 C 0.4674(8) 0.5034(6) 0.8370(8) 0.090(3) Uani 1 d . . . C25 C 0.4183(7) 0.4344(7) 0.8432(7) 0.085(3) Uani 1 d . . . C26 C 0.4574(6) 0.3650(6) 0.8926(6) 0.071(3) Uani 1 d . . . C31 C 0.5157(4) 0.2241(4) 1.0303(5) 0.0486(18) Uani 1 d . . . C32 C 0.4968(6) 0.2616(6) 1.0982(7) 0.080(3) Uani 1 d . . . C33 C 0.4331(6) 0.2296(7) 1.1307(7) 0.079(3) Uani 1 d . . . C34 C 0.3865(6) 0.1604(6) 1.0926(7) 0.075(3) Uani 1 d . . . C35 C 0.4077(5) 0.1197(6) 1.0256(6) 0.064(2) Uani 1 d . . . C36 C 0.4720(5) 0.1515(4) 0.9928(5) 0.0483(18) Uani 1 d . . . C42 C 0.4534(5) 0.0477(4) 0.8839(5) 0.0490(17) Uani 1 d . . . C43 C 0.4623(5) 0.0061(5) 0.8123(5) 0.0489(17) Uani 1 d . . . C44 C 0.4056(5) -0.0655(5) 0.7839(6) 0.063(2) Uani 1 d . . . C45 C 0.4094(6) -0.1108(5) 0.7163(6) 0.071(2) Uani 1 d . . . C46 C 0.4668(6) -0.0922(6) 0.6710(6) 0.074(3) Uani 1 d . . . C47 C 0.5230(7) -0.0241(6) 0.6966(7) 0.076(3) Uani 1 d . . . C48 C 0.5232(5) 0.0254(5) 0.7678(6) 0.056(2) Uani 1 d . . . C51 C 0.7913(5) 0.1569(5) 0.8468(5) 0.0541(19) Uani 1 d . . . C52 C 0.8656(5) 0.1829(6) 0.8278(5) 0.060(2) Uani 1 d . . . C53 C 0.9358(6) 0.1302(7) 0.8377(7) 0.077(3) Uani 1 d . . . C54 C 0.9310(7) 0.0488(8) 0.8644(8) 0.088(3) Uani 1 d . . . C55 C 0.8586(6) 0.0210(6) 0.8844(7) 0.079(3) Uani 1 d . . . C56 C 0.7880(6) 0.0757(5) 0.8745(6) 0.065(2) Uani 1 d . . . C61 C 0.6490(5) 0.2460(5) 0.7192(5) 0.0520(18) Uani 1 d . . . C62 C 0.6895(6) 0.2254(6) 0.6589(6) 0.071(2) Uani 1 d . . . C63 C 0.5677(5) 0.2828(6) 0.6906(6) 0.072(3) Uani 1 d . . . C64 C 0.5293(7) 0.3007(7) 0.6058(7) 0.088(3) Uani 1 d . . . C65 C 0.5709(8) 0.2807(7) 0.5454(7) 0.091(3) Uani 1 d . . . C66 C 0.6519(8) 0.2441(8) 0.5725(7) 0.096(3) Uani 1 d . . . C71 C 0.7506(6) 0.3274(5) 0.8704(6) 0.0558(19) Uani 1 d . . . C72 C 0.7313(6) 0.4020(5) 0.8257(6) 0.070(2) Uani 1 d . . . C73 C 0.7703(8) 0.4779(6) 0.8571(8) 0.088(3) Uani 1 d . . . C74 C 0.8325(9) 0.4810(8) 0.9362(10) 0.103(4) Uani 1 d . . . C75 C 0.8551(7) 0.4076(8) 0.9853(8) 0.092(4) Uani 1 d . . . C76 C 0.8169(5) 0.3306(6) 0.9512(6) 0.066(2) Uani 1 d . . . H12 H 0.7412 0.1702 1.0685 0.072 Uiso 1 calc R . . H13 H 0.8594 0.1855 1.1875 0.092 Uiso 1 calc R . . H14 H 0.8913 0.3117 1.2561 0.120 Uiso 1 calc R . . H15 H 0.7870 0.4141 1.2246 0.122 Uiso 1 calc R . . H16 H 0.6660 0.4059 1.1011 0.086 Uiso 1 calc R . . H22 H 0.6520 0.4369 0.9615 0.090 Uiso 1 calc R . . H23 H 0.5923 0.5521 0.8790 0.121 Uiso 1 calc R . . H24 H 0.4412 0.5491 0.8032 0.108 Uiso 1 calc R . . H25 H 0.3586 0.4338 0.8144 0.102 Uiso 1 calc R . . H26 H 0.4234 0.3189 0.8976 0.086 Uiso 1 calc R . . H32 H 0.5276 0.3096 1.1230 0.096 Uiso 1 calc R . . H33 H 0.4222 0.2548 1.1778 0.095 Uiso 1 calc R . . H34 H 0.3408 0.1404 1.1111 0.090 Uiso 1 calc R . . H35 H 0.3782 0.0705 1.0025 0.077 Uiso 1 calc R . . H42 H 0.4124 0.0246 0.9073 0.059 Uiso 1 calc R . . H44 H 0.3660 -0.0803 0.8129 0.075 Uiso 1 calc R . . H46 H 0.4679 -0.1249 0.6241 0.088 Uiso 1 calc R . . H47 H 0.5614 -0.0108 0.6658 0.092 Uiso 1 calc R . . H52 H 0.8680 0.2376 0.8079 0.072 Uiso 1 calc R . . H53 H 0.9860 0.1494 0.8264 0.093 Uiso 1 calc R . . H54 H 0.9774 0.0121 0.8691 0.106 Uiso 1 calc R . . H55 H 0.8565 -0.0338 0.9042 0.095 Uiso 1 calc R . . H56 H 0.7383 0.0568 0.8869 0.078 Uiso 1 calc R . . H62 H 0.7435 0.1984 0.6765 0.085 Uiso 1 calc R . . H63 H 0.5382 0.2959 0.7299 0.086 Uiso 1 calc R . . H64 H 0.4746 0.3265 0.5884 0.105 Uiso 1 calc R . . H65 H 0.5442 0.2921 0.4875 0.109 Uiso 1 calc R . . H66 H 0.6817 0.2317 0.5332 0.115 Uiso 1 calc R . . H72 H 0.6900 0.4012 0.7717 0.084 Uiso 1 calc R . . H73 H 0.7544 0.5269 0.8248 0.105 Uiso 1 calc R . . H74 H 0.8596 0.5319 0.9570 0.124 Uiso 1 calc R . . H75 H 0.8950 0.4097 1.0400 0.110 Uiso 1 calc R . . H76 H 0.8352 0.2810 0.9818 0.079 Uiso 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 0.0424(3) 0.0486(4) 0.0417(4) -0.0032(2) 0.0132(2) -0.0011(2) Br45 0.1376(11) 0.1032(9) 0.1114(11) -0.0501(8) 0.0471(9) -0.0609(8) P1 0.0474(10) 0.0481(10) 0.0457(12) -0.0071(8) 0.0147(8) -0.0015(8) P2 0.0447(9) 0.0536(10) 0.0436(11) 0.0011(8) 0.0148(8) -0.0028(8) Cl1 0.0698(14) 0.0938(17) 0.0823(18) -0.0138(14) 0.0275(12) -0.0114(12) N41 0.039(3) 0.046(3) 0.036(3) -0.004(3) 0.006(2) 0.000(2) O11 0.062(4) 0.135(7) 0.159(9) -0.021(6) 0.039(5) -0.027(4) O12 0.34(2) 0.35(2) 0.118(12) 0.015(13) 0.045(14) -0.17(2) O13 0.098(7) 0.100(8) 0.57(4) -0.073(13) 0.083(13) -0.034(6) O14 0.177(10) 0.147(9) 0.246(16) -0.096(10) 0.132(11) -0.045(8) O49 0.064(3) 0.069(3) 0.059(4) -0.016(3) 0.028(3) -0.016(3) C11 0.048(4) 0.066(5) 0.050(5) -0.012(4) 0.011(4) -0.005(3) C12 0.062(5) 0.066(5) 0.055(5) -0.004(4) 0.020(4) -0.002(4) C13 0.065(5) 0.095(7) 0.060(6) 0.003(5) 0.006(5) -0.001(5) C14 0.064(6) 0.145(10) 0.069(7) -0.035(7) -0.012(5) -0.018(7) C15 0.077(7) 0.127(9) 0.095(9) -0.068(8) 0.016(6) -0.020(7) C16 0.061(5) 0.079(6) 0.073(7) -0.025(5) 0.018(5) -0.006(4) C21 0.072(5) 0.059(5) 0.053(5) -0.010(4) 0.021(4) 0.006(4) C22 0.076(6) 0.058(5) 0.102(8) 0.019(5) 0.043(5) 0.007(4) C23 0.145(10) 0.051(6) 0.118(10) 0.013(6) 0.055(8) -0.023(6) C24 0.107(8) 0.069(6) 0.093(8) 0.002(6) 0.029(7) 0.029(6) C25 0.081(6) 0.087(7) 0.074(7) -0.012(6) 0.001(5) 0.016(6) C26 0.077(6) 0.062(5) 0.066(6) -0.006(4) 0.006(5) 0.010(4) C31 0.046(4) 0.051(4) 0.049(5) 0.000(3) 0.013(3) 0.006(3) C32 0.083(6) 0.080(6) 0.084(7) -0.040(5) 0.036(5) -0.017(5) C33 0.075(6) 0.111(8) 0.073(7) -0.023(6) 0.052(5) -0.013(5) C34 0.068(5) 0.093(7) 0.077(7) -0.019(5) 0.041(5) -0.011(5) C35 0.058(4) 0.069(5) 0.067(6) -0.003(4) 0.023(4) -0.009(4) C36 0.050(4) 0.042(4) 0.052(5) -0.006(3) 0.016(4) 0.001(3) C42 0.047(4) 0.051(4) 0.051(5) 0.000(3) 0.018(3) -0.004(3) C43 0.049(4) 0.055(4) 0.041(4) -0.008(3) 0.012(3) -0.003(3) C44 0.066(5) 0.051(4) 0.073(6) -0.016(4) 0.024(4) -0.021(4) C45 0.085(6) 0.056(5) 0.071(6) -0.020(4) 0.023(5) -0.027(4) C46 0.087(6) 0.075(6) 0.060(6) -0.020(5) 0.024(5) -0.020(5) C47 0.087(6) 0.076(6) 0.079(7) -0.016(5) 0.045(5) -0.019(5) C48 0.064(5) 0.048(4) 0.053(5) -0.001(4) 0.013(4) -0.005(4) C51 0.052(4) 0.064(5) 0.045(5) -0.003(4) 0.014(4) 0.003(3) C52 0.049(4) 0.085(6) 0.045(5) 0.005(4) 0.014(4) 0.001(4) C53 0.053(5) 0.112(8) 0.068(7) -0.006(6) 0.019(4) 0.016(5) C54 0.069(6) 0.110(8) 0.083(8) 0.003(6) 0.018(5) 0.031(6) C55 0.082(6) 0.078(6) 0.079(7) 0.009(5) 0.027(5) 0.030(5) C56 0.061(5) 0.067(5) 0.068(6) 0.007(4) 0.021(4) 0.007(4) C61 0.052(4) 0.053(4) 0.048(5) 0.001(3) 0.011(4) -0.009(3) C62 0.070(5) 0.089(6) 0.052(6) 0.011(5) 0.016(5) 0.003(5) C63 0.052(5) 0.092(7) 0.067(6) 0.011(5) 0.011(4) 0.001(4) C64 0.070(6) 0.101(7) 0.066(7) 0.015(6) -0.018(6) 0.003(5) C65 0.100(8) 0.099(8) 0.058(7) 0.023(6) 0.001(6) -0.020(6) C66 0.130(10) 0.117(9) 0.047(6) 0.011(6) 0.038(6) 0.017(8) C71 0.069(5) 0.049(4) 0.062(5) -0.001(4) 0.038(4) -0.007(3) C72 0.084(6) 0.063(5) 0.065(6) -0.002(4) 0.026(5) -0.014(4) C73 0.122(8) 0.061(6) 0.087(8) -0.011(5) 0.040(7) -0.028(6) C74 0.122(10) 0.091(8) 0.117(11) -0.031(8) 0.066(9) -0.041(7) C75 0.073(6) 0.130(10) 0.078(8) -0.032(7) 0.032(5) -0.039(6) C76 0.054(4) 0.091(6) 0.056(5) -0.014(5) 0.022(4) -0.010(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 O49 2.028(6) . ? Pd1 N41 2.074(6) . ? Pd1 P1 2.215(3) . ? Pd1 P2 2.303(3) . ? P1 C11 1.785(8) . ? P1 C31 1.802(8) . ? P1 C21 1.808(9) . ? C11 C12 1.371(11) . ? C11 C16 1.390(12) . ? C12 C13 1.367(12) . ? C13 C14 1.342(15) . ? C14 C15 1.344(16) . ? C15 C16 1.409(14) . ? C21 C22 1.369(12) . ? C21 C26 1.377(12) . ? C22 C23 1.373(15) . ? C23 C24 1.414(17) . ? C24 C25 1.369(15) . ? C25 C26 1.395(13) . ? C31 C32 1.372(12) . ? C31 C36 1.389(10) . ? C36 C35 1.393(12) . ? C36 N41 1.409(10) . ? C35 C34 1.398(13) . ? C34 C33 1.365(14) . ? C33 C32 1.383(14) . ? N41 C42 1.323(9) . ? C42 C43 1.388(11) . ? C43 C48 1.418(12) . ? C43 C44 1.439(10) . ? C44 C45 1.335(13) . ? C48 O49 1.295(9) . ? C48 C47 1.403(13) . ? C47 C46 1.386(12) . ? Br45 C45 1.916(8) . ? C46 C45 1.377(14) . ? P2 C71 1.796(8) . ? P2 C61 1.805(8) . ? P2 C51 1.813(8) . ? C51 C56 1.370(11) . ? C51 C52 1.382(12) . ? C52 C53 1.371(12) . ? C53 C54 1.370(15) . ? C54 C55 1.371(16) . ? C55 C56 1.394(12) . ? C61 C63 1.373(11) . ? C61 C62 1.375(13) . ? C62 C66 1.390(14) . ? C63 C64 1.364(14) . ? C64 C65 1.387(17) . ? C65 C66 1.367(16) . ? C71 C72 1.373(12) . ? C71 C76 1.424(13) . ? C72 C73 1.380(12) . ? C73 C74 1.373(17) . ? C74 C75 1.397(17) . ? C75 C76 1.401(14) . ? Cl1 O12 1.331(17) . ? Cl1 O14 1.345(10) . ? Cl1 O13 1.365(14) . ? Cl1 O11 1.428(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O49 Pd1 N41 92.6(2) . . ? O49 Pd1 P1 174.63(17) . . ? N41 Pd1 P1 84.61(17) . . ? O49 Pd1 P2 83.74(17) . . ? N41 Pd1 P2 176.19(16) . . ? P1 Pd1 P2 98.98(9) . . ? C11 P1 C31 105.6(4) . . ? C11 P1 C21 111.8(4) . . ? C31 P1 C21 104.3(4) . . ? C11 P1 Pd1 121.2(3) . . ? C31 P1 Pd1 101.4(3) . . ? C21 P1 Pd1 110.5(3) . . ? C12 C11 C16 119.1(7) . . ? C12 C11 P1 118.5(6) . . ? C16 C11 P1 122.2(6) . . ? C13 C12 C11 120.3(8) . . ? C14 C13 C12 122.1(10) . . ? C13 C14 C15 118.2(9) . . ? C14 C15 C16 122.3(10) . . ? C11 C16 C15 117.5(9) . . ? C22 C21 C26 118.2(8) . . ? C22 C21 P1 123.8(7) . . ? C26 C21 P1 117.9(7) . . ? C21 C22 C23 123.8(10) . . ? C22 C23 C24 117.1(10) . . ? C25 C24 C23 120.2(9) . . ? C24 C25 C26 120.3(10) . . ? C21 C26 C25 120.3(10) . . ? C32 C31 C36 120.7(8) . . ? C32 C31 P1 122.5(6) . . ? C36 C31 P1 116.9(6) . . ? C31 C36 C35 117.5(7) . . ? C31 C36 N41 118.1(7) . . ? C35 C36 N41 124.4(7) . . ? C36 C35 C34 121.3(8) . . ? C33 C34 C35 119.9(9) . . ? C34 C33 C32 119.0(9) . . ? C31 C32 C33 121.5(9) . . ? C42 N41 C36 120.6(6) . . ? C42 N41 Pd1 120.5(5) . . ? C36 N41 Pd1 118.9(4) . . ? N41 C42 C43 129.4(7) . . ? C42 C43 C48 126.4(7) . . ? C42 C43 C44 115.4(7) . . ? C48 C43 C44 118.1(7) . . ? C45 C44 C43 120.5(8) . . ? O49 C48 C47 117.2(8) . . ? O49 C48 C43 124.3(7) . . ? C47 C48 C43 118.5(7) . . ? C46 C47 C48 121.5(9) . . ? C45 C46 C47 118.9(9) . . ? C48 O49 Pd1 126.6(5) . . ? C44 C45 C46 122.5(8) . . ? C44 C45 Br45 120.5(7) . . ? C46 C45 Br45 116.9(7) . . ? C71 P2 C61 103.3(4) . . ? C71 P2 C51 103.3(4) . . ? C61 P2 C51 108.8(4) . . ? C71 P2 Pd1 121.9(3) . . ? C61 P2 Pd1 106.9(3) . . ? C51 P2 Pd1 111.9(3) . . ? C56 C51 C52 118.4(8) . . ? C56 C51 P2 121.0(7) . . ? C52 C51 P2 120.6(6) . . ? C53 C52 C51 121.7(9) . . ? C54 C53 C52 119.1(10) . . ? C53 C54 C55 120.8(9) . . ? C54 C55 C56 119.2(10) . . ? C51 C56 C55 120.7(9) . . ? C63 C61 C62 117.5(8) . . ? C63 C61 P2 119.9(7) . . ? C62 C61 P2 122.5(6) . . ? C61 C62 C66 121.7(9) . . ? C64 C63 C61 121.6(10) . . ? C63 C64 C65 120.6(10) . . ? C66 C65 C64 118.8(10) . . ? C65 C66 C62 119.7(11) . . ? C72 C71 C76 116.6(8) . . ? C72 C71 P2 124.4(7) . . ? C76 C71 P2 119.0(6) . . ? C71 C72 C73 123.2(9) . . ? C74 C73 C72 119.9(10) . . ? C73 C74 C75 119.9(10) . . ? C74 C75 C76 119.4(10) . . ? C75 C76 C71 120.8(9) . . ? O12 Cl1 O14 116.2(12) . . ? O12 Cl1 O13 99.4(13) . . ? O14 Cl1 O13 106.4(10) . . ? O12 Cl1 O11 111.9(9) . . ? O14 Cl1 O11 113.9(6) . . ? O13 Cl1 O11 107.5(6) . . ? _refine_diff_density_max 1.662 _refine_diff_density_min -1.068 _refine_diff_density_rms 0.119 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 249209' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H21 Cl N O2 PPt' _chemical_formula_weight 640.95 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' Pt Pt -1.7033 8.3905 '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' Cl Cl 0.1484 0.1585 '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 12.350(14) _cell_length_b 12.138(14) _cell_length_c 15.550(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.700(10) _cell_angle_gamma 90.00 _cell_volume 2310(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 25.84 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.843 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 6.283 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.456 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4051 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1006 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.84 _reflns_number_total 4051 _reflns_number_gt 2563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.1463P)^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 0.0014(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4051 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1418 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.2087 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.14428(5) 0.72770(4) 0.38075(3) 0.0334(3) Uani 1 d . . . P1 P 0.2349(4) 0.5814(3) 0.3479(2) 0.0384(9) Uani 1 d . . . Cl1 Cl 0.2429(4) 0.7442(3) 0.5167(2) 0.0502(11) Uani 1 d . . . N41 N 0.0568(12) 0.7110(9) 0.2632(7) 0.044(3) Uani 1 d . . . O450 O -0.3546(14) 0.9843(13) 0.2603(9) 0.091(6) Uani 1 d . . . O49 O 0.0572(11) 0.8670(9) 0.4085(6) 0.057(3) Uani 1 d . . . C11 C 0.1903(14) 0.4527(13) 0.3936(8) 0.041(4) Uani 1 d . . . C12 C 0.1928(16) 0.3538(14) 0.3529(10) 0.057(5) Uani 1 d . . . C13 C 0.149(2) 0.2629(15) 0.3870(12) 0.075(7) Uani 1 d . . . C14 C 0.108(2) 0.2647(15) 0.4610(12) 0.071(6) Uani 1 d . . . C15 C 0.1021(18) 0.3662(14) 0.5040(10) 0.061(5) Uani 1 d . . . C16 C 0.1476(16) 0.4588(13) 0.4705(9) 0.052(4) Uani 1 d . . . C21 C 0.3824(15) 0.5885(14) 0.3618(9) 0.048(4) Uani 1 d . . . C22 C 0.4467(19) 0.4945(15) 0.3832(11) 0.060(5) Uani 1 d . . . C23 C 0.5577(19) 0.512(2) 0.3927(13) 0.081(7) Uani 1 d . . . C24 C 0.606(3) 0.609(3) 0.3790(14) 0.114(11) Uani 1 d . . . C25 C 0.538(2) 0.696(3) 0.3605(14) 0.093(8) Uani 1 d . . . C26 C 0.429(2) 0.6858(19) 0.3560(13) 0.076(6) Uani 1 d . . . C31 C 0.1907(15) 0.5733(11) 0.2314(8) 0.042(4) Uani 1 d . . . C32 C 0.2399(14) 0.5068(12) 0.1735(8) 0.042(4) Uani 1 d . . . C33 C 0.1997(17) 0.5101(15) 0.0876(10) 0.057(5) Uani 1 d . . . C34 C 0.1094(18) 0.5762(15) 0.0565(11) 0.062(5) Uani 1 d . . . C35 C 0.0609(15) 0.6421(13) 0.1140(8) 0.050(4) Uani 1 d . . . C36 C 0.0976(12) 0.6414(12) 0.2006(8) 0.037(3) Uani 1 d . . . C42 C -0.0383(14) 0.7502(11) 0.2427(9) 0.037(4) Uani 1 d . . . C43 C -0.0908(13) 0.8294(12) 0.2929(8) 0.038(3) Uani 1 d . . . C44 C -0.1994(15) 0.8621(13) 0.2562(8) 0.048(4) Uani 1 d . . . C45 C -0.2534(17) 0.9455(15) 0.2886(10) 0.056(4) Uani 1 d . . . C451 C -0.409(2) 0.929(2) 0.1944(14) 0.093(8) Uani 1 d . . . C46 C -0.194(2) 1.0104(16) 0.3575(11) 0.073(7) Uani 1 d . . . C47 C -0.0932(15) 0.9833(12) 0.3929(10) 0.047(4) Uani 1 d . . . C48 C -0.0329(15) 0.8901(12) 0.3651(8) 0.042(4) Uani 1 d . . . H12 H 0.2241 0.3481 0.3019 0.069 Uiso 1 calc R . . H13 H 0.1491 0.1967 0.3568 0.090 Uiso 1 calc R . . H14 H 0.0827 0.2003 0.4841 0.085 Uiso 1 calc R . . H15 H 0.0686 0.3712 0.5539 0.073 Uiso 1 calc R . . H16 H 0.1491 0.5253 0.5004 0.062 Uiso 1 calc R . . H22 H 0.4163 0.4256 0.3904 0.072 Uiso 1 calc R . . H23 H 0.6027 0.4519 0.4098 0.097 Uiso 1 calc R . . H24 H 0.6815 0.6158 0.3822 0.137 Uiso 1 calc R . . H25 H 0.5681 0.7642 0.3505 0.111 Uiso 1 calc R . . H26 H 0.3854 0.7485 0.3486 0.092 Uiso 1 calc R . . H32 H 0.2986 0.4615 0.1935 0.051 Uiso 1 calc R . . H33 H 0.2327 0.4677 0.0486 0.068 Uiso 1 calc R . . H34 H 0.0821 0.5759 -0.0022 0.074 Uiso 1 calc R . . H35 H 0.0026 0.6874 0.0930 0.060 Uiso 1 calc R . . H42 H -0.0777 0.7259 0.1910 0.045 Uiso 1 calc R . . H44 H -0.2336 0.8240 0.2082 0.057 Uiso 1 calc R . . H45A H -0.3677 0.9280 0.1465 0.112 Uiso 1 calc R . . H45B H -0.4783 0.9644 0.1768 0.112 Uiso 1 calc R . . H45C H -0.4216 0.8549 0.2123 0.112 Uiso 1 calc R . . H46 H -0.2272 1.0724 0.3776 0.088 Uiso 1 calc R . . H47 H -0.0595 1.0267 0.4380 0.056 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0330(4) 0.0336(4) 0.0336(3) -0.0007(2) 0.0040(2) 0.0009(2) Cl1 0.053(3) 0.060(2) 0.0343(17) 0.0032(15) -0.0062(17) 0.0034(19) P1 0.042(3) 0.0374(19) 0.0378(18) 0.0044(15) 0.0134(16) 0.0045(18) N41 0.042(9) 0.045(8) 0.040(6) -0.015(5) -0.005(6) 0.011(6) O450 0.068(13) 0.113(12) 0.084(9) -0.033(8) -0.015(8) 0.050(10) O49 0.080(11) 0.047(6) 0.041(5) 0.003(5) 0.001(6) 0.024(6) C11 0.034(10) 0.046(9) 0.042(7) 0.018(6) 0.004(6) -0.003(7) C12 0.068(16) 0.049(9) 0.057(9) 0.000(8) 0.018(9) 0.003(9) C13 0.09(2) 0.031(9) 0.114(19) 0.002(9) 0.048(16) -0.004(9) C14 0.10(2) 0.057(11) 0.063(11) 0.019(9) 0.029(12) 0.003(11) C15 0.077(17) 0.049(10) 0.062(9) 0.003(8) 0.029(9) -0.005(10) C16 0.053(13) 0.050(9) 0.052(8) -0.005(7) 0.005(8) 0.000(8) C21 0.029(11) 0.060(10) 0.053(9) -0.007(7) 0.002(7) -0.001(8) C22 0.064(16) 0.051(10) 0.065(10) 0.010(8) 0.011(9) 0.012(9) C23 0.026(14) 0.13(2) 0.083(14) 0.001(13) 0.005(10) 0.027(12) C24 0.05(2) 0.21(4) 0.082(16) -0.020(18) 0.023(14) -0.01(2) C25 0.037(17) 0.14(2) 0.101(17) 0.009(16) 0.018(13) -0.026(15) C26 0.057(17) 0.082(14) 0.091(14) 0.022(12) 0.016(11) 0.002(12) C31 0.049(12) 0.037(8) 0.039(7) -0.005(6) 0.008(7) -0.001(7) C32 0.049(11) 0.043(8) 0.034(7) 0.001(6) 0.002(7) -0.002(7) C33 0.054(14) 0.069(12) 0.052(9) -0.010(8) 0.022(9) -0.005(9) C34 0.054(15) 0.069(12) 0.065(10) -0.024(9) 0.017(9) 0.004(10) C35 0.050(12) 0.056(9) 0.043(7) -0.013(7) 0.001(7) 0.018(8) C36 0.023(9) 0.047(8) 0.040(7) -0.004(6) 0.005(6) -0.002(6) C42 0.033(10) 0.038(8) 0.038(7) 0.001(6) -0.006(6) -0.005(6) C43 0.026(9) 0.044(8) 0.042(7) -0.017(6) 0.003(6) 0.009(7) C44 0.047(12) 0.056(9) 0.041(7) -0.016(7) 0.011(7) 0.015(8) C45 0.042(13) 0.067(11) 0.060(9) -0.003(8) 0.007(8) 0.017(9) C451 0.08(2) 0.108(19) 0.089(15) 0.009(13) -0.007(14) 0.021(15) C46 0.10(2) 0.063(11) 0.053(9) -0.006(8) 0.004(10) 0.041(12) C47 0.038(11) 0.040(8) 0.060(9) -0.022(7) -0.004(8) 0.022(7) C48 0.056(12) 0.039(8) 0.033(6) 0.008(6) 0.006(7) 0.006(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 Pt1 N41 2.005(12) . ? Pt1 O49 2.080(11) . ? Pt1 P1 2.196(4) . ? Pt1 Cl1 2.303(4) . ? C42 N41 1.27(2) . ? C42 C43 1.45(2) . ? C43 C44 1.44(2) . ? C43 C48 1.449(19) . ? C44 C45 1.35(2) . ? C45 O450 1.35(2) . ? C45 C46 1.45(3) . ? O450 C451 1.33(2) . ? C46 C47 1.33(3) . ? C47 C48 1.45(2) . ? C48 O49 1.25(2) . ? N41 C36 1.430(18) . ? P1 C21 1.808(19) . ? P1 C31 1.824(13) . ? P1 C11 1.831(15) . ? C31 C32 1.41(2) . ? C31 C36 1.44(2) . ? C36 C35 1.362(18) . ? C35 C34 1.39(2) . ? C34 C33 1.41(3) . ? C33 C32 1.36(2) . ? C21 C26 1.32(3) . ? C21 C22 1.40(2) . ? C22 C23 1.37(3) . ? C23 C24 1.36(4) . ? C24 C25 1.35(4) . ? C25 C26 1.35(3) . ? C11 C12 1.36(2) . ? C11 C16 1.37(2) . ? C12 C13 1.36(2) . ? C13 C14 1.32(2) . ? C14 C15 1.41(2) . ? C15 C16 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Pt1 O49 92.3(5) . . ? N41 Pt1 P1 86.3(4) . . ? O49 Pt1 P1 178.5(3) . . ? N41 Pt1 Cl1 179.0(4) . . ? O49 Pt1 Cl1 87.9(3) . . ? P1 Pt1 Cl1 93.48(16) . . ? N41 C42 C43 125.6(13) . . ? C44 C43 C48 120.2(13) . . ? C44 C43 C42 115.5(12) . . ? C48 C43 C42 123.1(14) . . ? C45 C44 C43 122.7(15) . . ? O450 C45 C44 128.5(17) . . ? O450 C45 C46 113.9(16) . . ? C44 C45 C46 117.3(19) . . ? C451 O450 C45 115.3(17) . . ? C47 C46 C45 121.5(17) . . ? C46 C47 C48 123.9(15) . . ? O49 C48 C43 127.8(14) . . ? O49 C48 C47 117.9(13) . . ? C43 C48 C47 114.1(15) . . ? C42 N41 C36 116.7(12) . . ? C42 N41 Pt1 124.0(10) . . ? C36 N41 Pt1 118.9(10) . . ? C48 O49 Pt1 121.1(9) . . ? C21 P1 C31 106.5(8) . . ? C21 P1 C11 110.2(8) . . ? C31 P1 C11 105.9(7) . . ? C21 P1 Pt1 118.1(6) . . ? C31 P1 Pt1 100.4(5) . . ? C11 P1 Pt1 114.2(6) . . ? C32 C31 C36 120.7(13) . . ? C32 C31 P1 124.7(13) . . ? C36 C31 P1 114.6(10) . . ? C35 C36 N41 124.6(14) . . ? C35 C36 C31 118.4(13) . . ? N41 C36 C31 116.8(11) . . ? C36 C35 C34 121.1(16) . . ? C35 C34 C33 119.7(16) . . ? C32 C33 C34 121.5(17) . . ? C33 C32 C31 118.6(16) . . ? C26 C21 C22 120(2) . . ? C26 C21 P1 118.3(16) . . ? C22 C21 P1 121.2(15) . . ? C23 C22 C21 115.3(19) . . ? C22 C23 C24 125(3) . . ? C25 C24 C23 116(3) . . ? C26 C25 C24 122(3) . . ? C21 C26 C25 121(2) . . ? C12 C11 C16 119.3(14) . . ? C12 C11 P1 123.1(11) . . ? C16 C11 P1 117.6(12) . . ? C13 C12 C11 119.9(16) . . ? C14 C13 C12 122.9(18) . . ? C13 C14 C15 118.5(17) . . ? C16 C15 C14 118.9(15) . . ? C11 C16 C15 120.3(15) . . ? _refine_diff_density_max 2.582 _refine_diff_density_min -2.405 _refine_diff_density_rms 0.383 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_10 _database_code_depnum_ccdc_archive 'CCDC 249210' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C27 H23 Cl2 I N O2 P Pt' _chemical_formula_weight 817.32 _chemical_melting_point ? _chemical_compound_source ? 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _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 10.446(11) _cell_length_b 16.389(17) _cell_length_c 16.507(17) _cell_angle_alpha 90.00 _cell_angle_beta 100.238(10) _cell_angle_gamma 90.00 _cell_volume 2781.0(50) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.77 _cell_measurement_theta_max 25.80 _exptl_crystal_description needle _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.931 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 6.353 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.353 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_standards_interval_count ? _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12685 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0896 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.80 _reflns_number_total 5189 _reflns_number_observed 4021 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0777P)^2^+33.9767P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5189 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1019 _refine_ls_R_factor_obs 0.0725 _refine_ls_wR_factor_all 0.1758 _refine_ls_wR_factor_obs 0.1566 _refine_ls_goodness_of_fit_all 1.128 _refine_ls_goodness_of_fit_obs 1.148 _refine_ls_restrained_S_all 1.128 _refine_ls_restrained_S_obs 1.148 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.79265(5) 0.80750(3) 0.03026(3) 0.0215(2) Uani 1 d . . I1 I 0.75155(11) 0.89881(6) 0.15324(6) 0.0355(3) Uani 1 d . . P1 P 0.9899(4) 0.7680(2) 0.0879(2) 0.0240(8) Uani 1 d . . N41 N 0.8244(12) 0.7409(6) -0.0666(7) 0.028(3) Uani 1 d . . O450 O 0.4313(12) 0.8563(7) -0.3650(7) 0.048(3) Uani 1 d . . O49 O 0.6126(11) 0.8424(7) -0.0298(6) 0.040(3) Uani 1 d . . C11 C 1.1225(14) 0.8421(8) 0.0853(8) 0.025(3) Uani 1 d . . C12 C 1.2467(17) 0.8175(10) 0.0814(11) 0.045(4) Uani 1 d . . C13 C 1.3419(19) 0.8726(11) 0.0709(14) 0.060(6) Uani 1 d . . C14 C 1.3137(20) 0.9547(11) 0.0659(12) 0.055(5) Uani 1 d . . C15 C 1.1851(21) 0.9801(10) 0.0707(11) 0.053(5) Uani 1 d . . C16 C 1.0912(17) 0.9256(8) 0.0785(9) 0.034(3) Uani 1 d . . C21 C 1.0176(16) 0.7219(8) 0.1897(9) 0.031(3) Uani 1 d . . C22 C 1.1089(19) 0.7546(10) 0.2549(9) 0.046(5) Uani 1 d . . C23 C 1.1285(22) 0.7162(12) 0.3316(9) 0.055(5) Uani 1 d . . C24 C 1.0613(24) 0.6448(12) 0.3445(10) 0.060(6) Uani 1 d . . C25 C 0.9688(25) 0.6120(11) 0.2783(11) 0.060(6) Uani 1 d . . C26 C 0.9486(19) 0.6510(9) 0.2021(10) 0.045(4) Uani 1 d . . C31 C 1.0195(13) 0.6861(7) 0.0188(8) 0.021(3) Uani 1 d . . C32 C 1.1192(16) 0.6282(9) 0.0356(10) 0.035(4) Uani 1 d . . C33 C 1.1332(17) 0.5681(9) -0.0234(10) 0.041(4) Uani 1 d . . C34 C 1.0455(17) 0.5649(9) -0.0962(10) 0.038(4) Uani 1 d . . C35 C 0.9426(17) 0.6188(8) -0.1122(8) 0.033(4) Uani 1 d . . C36 C 0.9290(15) 0.6805(8) -0.0549(8) 0.029(3) Uani 1 d . . C42 C 0.7607(15) 0.7535(8) -0.1433(8) 0.028(3) Uani 1 d . . C43 C 0.6466(15) 0.8015(8) -0.1653(9) 0.030(3) Uani 1 d . . C44 C 0.5964(15) 0.8072(8) -0.2537(8) 0.030(3) Uani 1 d . . C45 C 0.4841(17) 0.8463(9) -0.2831(9) 0.038(4) Uani 1 d . . C451 C 0.5138(21) 0.8406(13) -0.4248(11) 0.059(5) Uani 1 d . . C46 C 0.4119(16) 0.8798(10) -0.2283(10) 0.042(4) Uani 1 d . . C47 C 0.4530(16) 0.8767(10) -0.1437(10) 0.038(4) Uani 1 d . . C48 C 0.5748(16) 0.8398(7) -0.1104(9) 0.033(4) Uani 1 d . . H12 H 1.2672(17) 0.7623(10) 0.0860(11) 0.054 Uiso 1 calc R . H13 H 1.4250(19) 0.8544(11) 0.0673(14) 0.072 Uiso 1 calc R . H14 H 1.3773(20) 0.9927(11) 0.0596(12) 0.066 Uiso 1 calc R . H15 H 1.1653(21) 1.0354(10) 0.0683(11) 0.063 Uiso 1 calc R . H16 H 1.0067(17) 0.9431(8) 0.0795(9) 0.041 Uiso 1 calc R . H22 H 1.1556(19) 0.8013(10) 0.2468(9) 0.055 Uiso 1 calc R . H23 H 1.1873(22) 0.7384(12) 0.3749(9) 0.066 Uiso 1 calc R . H24 H 1.0767(24) 0.6191(12) 0.3956(10) 0.072 Uiso 1 calc R . H25 H 0.9224(25) 0.5650(11) 0.2860(11) 0.072 Uiso 1 calc R . H26 H 0.8886(19) 0.6297(9) 0.1589(10) 0.055 Uiso 1 calc R . H32 H 1.1763(16) 0.6293(9) 0.0857(10) 0.042 Uiso 1 calc R . H33 H 1.2012(17) 0.5308(9) -0.0131(10) 0.049 Uiso 1 calc R . H34 H 1.0559(17) 0.5258(9) -0.1353(10) 0.046 Uiso 1 calc R . H35 H 0.8823(17) 0.6144(8) -0.1608(8) 0.040 Uiso 1 calc R . H42 H 0.7940(15) 0.7288(8) -0.1859(8) 0.034 Uiso 1 calc R . H44 H 0.6430(15) 0.7832(8) -0.2905(8) 0.037 Uiso 1 calc R . H45A H 0.5933(51) 0.8709(55) -0.4104(40) 0.071 Uiso 1 calc R . H45B H 0.4699(49) 0.8571(66) -0.4783(16) 0.071 Uiso 1 calc R . H45C H 0.5332(92) 0.7833(16) -0.4253(51) 0.071 Uiso 1 calc R . H46 H 0.3333(16) 0.9052(10) -0.2490(10) 0.051 Uiso 1 calc R . H47 H 0.4013(16) 0.8986(10) -0.1087(10) 0.046 Uiso 1 calc R . C100 C 0.4679(27) 0.5852(20) -0.2064(18) 0.101(10) Uani 1 d . . Cl1 Cl 0.6002(8) 0.5694(5) -0.1269(5) 0.100(2) Uani 1 d . . Cl2 Cl 0.3226(10) 0.5577(8) -0.1874(8) 0.166(5) Uani 1 d . . H10A H 0.4646(27) 0.6428(20) -0.2204(18) 0.121 Uiso 1 calc R . H10B H 0.4838(27) 0.5555(20) -0.2545(18) 0.121 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0206(3) 0.0213(3) 0.0220(3) 0.0005(2) 0.0020(2) -0.0001(2) I1 0.0405(6) 0.0388(5) 0.0275(5) -0.0031(4) 0.0074(4) 0.0070(4) P1 0.026(2) 0.023(2) 0.021(2) -0.0009(13) -0.0011(15) -0.0018(14) N41 0.030(7) 0.018(5) 0.030(6) 0.002(5) -0.010(5) 0.007(5) O450 0.042(8) 0.057(7) 0.037(6) -0.002(5) -0.013(6) 0.011(6) O49 0.038(7) 0.048(6) 0.026(5) -0.003(5) -0.013(5) 0.006(5) C11 0.025(8) 0.026(6) 0.025(6) 0.002(5) 0.002(6) 0.002(6) C12 0.036(10) 0.034(8) 0.063(11) -0.001(8) 0.005(9) 0.000(7) C13 0.027(10) 0.057(11) 0.096(16) 0.018(11) 0.010(11) -0.014(8) C14 0.054(13) 0.045(9) 0.063(11) -0.007(9) -0.003(10) -0.027(9) C15 0.066(14) 0.027(8) 0.063(11) 0.001(8) 0.008(10) -0.003(8) C16 0.031(9) 0.030(7) 0.042(8) -0.001(6) 0.005(7) -0.001(6) C21 0.035(9) 0.023(6) 0.032(7) -0.004(6) -0.001(7) 0.009(6) C22 0.063(13) 0.041(8) 0.027(7) -0.007(7) -0.009(8) -0.001(8) C23 0.074(15) 0.069(12) 0.017(7) -0.001(8) -0.002(8) 0.013(11) C24 0.096(18) 0.065(12) 0.024(8) 0.012(8) 0.025(10) 0.023(12) C25 0.104(19) 0.042(9) 0.040(9) 0.010(8) 0.029(11) -0.002(10) C26 0.059(13) 0.037(8) 0.038(9) 0.003(7) 0.002(8) -0.007(8) C31 0.022(7) 0.015(5) 0.024(6) 0.005(5) -0.001(5) -0.001(5) C32 0.030(9) 0.034(7) 0.040(8) 0.000(7) 0.004(7) 0.000(7) C33 0.039(10) 0.032(8) 0.051(9) -0.002(7) 0.010(8) 0.015(7) C34 0.039(10) 0.029(7) 0.044(9) -0.007(7) -0.001(8) 0.004(7) C35 0.048(10) 0.027(7) 0.025(7) -0.007(6) 0.004(7) 0.007(7) C36 0.030(8) 0.026(7) 0.027(7) -0.001(5) -0.007(6) -0.010(6) C42 0.031(8) 0.021(6) 0.030(7) -0.008(5) -0.002(6) 0.003(6) C43 0.029(8) 0.021(6) 0.037(7) 0.000(6) -0.006(6) -0.002(6) C44 0.038(9) 0.032(7) 0.019(6) -0.005(6) 0.001(6) -0.003(7) C45 0.040(10) 0.035(8) 0.033(8) 0.010(7) -0.016(8) 0.001(7) C451 0.049(13) 0.079(13) 0.046(10) 0.009(10) 0.002(9) 0.016(10) C46 0.023(9) 0.056(10) 0.042(9) 0.011(8) -0.012(7) 0.001(7) C47 0.026(9) 0.050(9) 0.038(8) -0.004(7) 0.007(7) 0.008(7) C48 0.044(10) 0.012(6) 0.042(8) 0.008(6) 0.002(7) 0.015(6) C100 0.065(19) 0.136(24) 0.093(19) 0.010(18) -0.006(16) -0.023(17) Cl1 0.084(5) 0.103(5) 0.104(5) 0.012(4) -0.009(4) -0.020(4) Cl2 0.067(6) 0.220(11) 0.215(12) 0.100(10) 0.039(7) 0.014(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 Pt1 N41 2.011(12) . ? Pt1 O49 2.045(10) . ? Pt1 P1 2.207(4) . ? Pt1 I1 2.618(2) . ? P1 C21 1.818(15) . ? P1 C31 1.824(13) . ? P1 C11 1.849(15) . ? N41 C42 1.34(2) . ? N41 C36 1.46(2) . ? C31 C32 1.40(2) . ? C31 C36 1.40(2) . ? C36 C35 1.41(2) . ? C35 C34 1.38(2) . ? C34 C33 1.38(2) . ? C33 C32 1.41(2) . ? C42 C43 1.42(2) . ? C43 C48 1.42(2) . ? C43 C44 1.46(2) . ? C44 C45 1.35(2) . ? C45 O450 1.38(2) . ? C45 C46 1.39(3) . ? O450 C451 1.44(2) . ? C46 C47 1.39(2) . ? C47 C48 1.43(2) . ? C48 O49 1.32(2) . ? C22 C23 1.40(2) . ? C22 C21 1.41(2) . ? C23 C24 1.40(3) . ? C24 C25 1.43(3) . ? C25 C26 1.39(2) . ? C26 C21 1.40(2) . ? C12 C13 1.38(2) . ? C12 C11 1.37(2) . ? C13 C14 1.38(3) . ? C14 C15 1.42(3) . ? C15 C16 1.35(2) . ? C16 C11 1.41(2) . ? C100 Cl2 1.67(3) . ? C100 Cl1 1.75(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 Pt1 O49 92.0(4) . . ? N41 Pt1 P1 84.8(3) . . ? O49 Pt1 P1 176.6(3) . . ? N41 Pt1 I1 178.0(3) . . ? O49 Pt1 I1 87.3(3) . . ? P1 Pt1 I1 95.89(10) . . ? C21 P1 C31 104.8(6) . . ? C21 P1 C11 107.3(6) . . ? C31 P1 C11 104.9(7) . . ? C21 P1 Pt1 120.2(6) . . ? C31 P1 Pt1 101.3(4) . . ? C11 P1 Pt1 116.3(4) . . ? C42 N41 C36 117.7(12) . . ? C42 N41 Pt1 122.9(9) . . ? C36 N41 Pt1 119.2(8) . . ? C32 C31 C36 119.3(12) . . ? C32 C31 P1 125.4(10) . . ? C36 C31 P1 115.2(10) . . ? C31 C36 C35 119.7(13) . . ? C31 C36 N41 116.3(11) . . ? C35 C36 N41 124.0(11) . . ? C34 C35 C36 119.9(13) . . ? C33 C34 C35 121.2(14) . . ? C34 C33 C32 119.6(14) . . ? C31 C32 C33 120.1(13) . . ? N41 C42 C43 125.6(14) . . ? C42 C43 C48 126.5(13) . . ? C42 C43 C44 115.2(14) . . ? C48 C43 C44 118.2(13) . . ? C45 C44 C43 121.5(15) . . ? C44 C45 O450 125.5(17) . . ? C44 C45 C46 119.5(13) . . ? O450 C45 C46 115.1(14) . . ? C45 O450 C451 117.8(14) . . ? C47 C46 C45 122.3(14) . . ? C46 C47 C48 119.9(16) . . ? O49 C48 C43 124.1(13) . . ? O49 C48 C47 117.5(14) . . ? C43 C48 C47 118.4(13) . . ? C48 O49 Pt1 124.4(11) . . ? C23 C22 C21 119.4(17) . . ? C24 C23 C22 121.2(17) . . ? C23 C24 C25 119.1(15) . . ? C26 C25 C24 119.4(17) . . ? C21 C26 C25 120.9(16) . . ? C13 C12 C11 121.6(16) . . ? C12 C13 C14 119.8(19) . . ? C13 C14 C15 118.5(17) . . ? C16 C15 C14 121.5(15) . . ? C15 C16 C11 119.2(16) . . ? C26 C21 C22 119.9(14) . . ? C26 C21 P1 118.6(11) . . ? C22 C21 P1 121.5(12) . . ? C12 C11 C16 119.4(14) . . ? C12 C11 P1 121.8(11) . . ? C16 C11 P1 118.4(11) . . ? Cl2 C100 Cl1 116.3(18) . . ? _refine_diff_density_max 2.726 _refine_diff_density_min -2.386 _refine_diff_density_rms 0.358 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_20 _database_code_depnum_ccdc_archive 'CCDC 249211' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H39 Cl2 N O5 P2 Pd' _chemical_formula_weight 925.02 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' Pd Pd -0.9988 1.0072 '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' Cl Cl 0.1484 0.1585 '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 12.454(15) _cell_length_b 20.25(2) _cell_length_c 17.000(18) _cell_angle_alpha 90.00 _cell_angle_beta 99.090(10) _cell_angle_gamma 90.00 _cell_volume 4234(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.89 _cell_measurement_theta_max 26.00 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.687 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.654 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10955 _diffrn_reflns_av_R_equivalents 0.1021 _diffrn_reflns_av_sigmaI/netI 0.1255 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6295 _reflns_number_gt 3109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.1425P)^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 0.0009(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6295 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1720 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.2400 _refine_ls_wR_factor_gt 0.1944 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _refine_ls_shift/su_max 0.098 _refine_ls_shift/su_mean 0.025 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.40584(6) 0.93495(4) 0.16765(4) 0.0525(3) Uani 1 d . . . P1 P 0.4979(2) 0.84173(12) 0.15771(14) 0.0528(7) Uani 1 d . . . P2 P 0.4260(2) 0.94028(12) 0.30395(14) 0.0512(6) Uani 1 d . . . Cl1 Cl -0.1466(3) 1.07357(16) 0.2296(2) 0.0856(9) Uani 1 d . . . Cl45 Cl -0.0305(3) 1.10489(16) -0.08802(19) 0.0907(10) Uani 1 d . . . N41 N 0.3852(6) 0.9339(3) 0.0447(4) 0.0462(17) Uani 1 d . . . O11 O -0.0562(8) 1.0331(5) 0.2237(6) 0.134(4) Uani 1 d . . . O12 O -0.2447(7) 1.0410(5) 0.2008(5) 0.110(3) Uani 1 d . . . O13 O -0.1443(8) 1.0969(7) 0.3080(6) 0.152(5) Uani 1 d . . . O14 O -0.1319(12) 1.1295(5) 0.1778(7) 0.172(5) Uani 1 d . . . O49 O 0.3111(6) 1.0158(3) 0.1661(4) 0.072(2) Uani 1 d . . . C11 C 0.4175(9) 0.7688(5) 0.1694(6) 0.061(3) Uani 1 d . . . C12 C 0.4495(12) 0.7048(6) 0.1537(7) 0.096(4) Uani 1 d . . . C13 C 0.3836(14) 0.6519(7) 0.1619(9) 0.109(5) Uani 1 d . . . C14 C 0.2848(17) 0.6623(8) 0.1876(9) 0.123(7) Uani 1 d . . . C15 C 0.2520(12) 0.7242(9) 0.2053(8) 0.112(5) Uani 1 d . . . C16 C 0.3166(11) 0.7793(5) 0.1945(6) 0.080(4) Uani 1 d . . . C21 C 0.6356(8) 0.8293(4) 0.2071(5) 0.053(2) Uani 1 d . . . C22 C 0.6734(8) 0.7721(4) 0.2441(5) 0.050(2) Uani 1 d . . . C23 C 0.7841(9) 0.7650(5) 0.2756(6) 0.062(3) Uani 1 d . . . C24 C 0.8533(9) 0.8158(6) 0.2683(6) 0.068(3) Uani 1 d . . . C25 C 0.8172(10) 0.8734(6) 0.2308(6) 0.072(3) Uani 1 d . . . C26 C 0.7087(11) 0.8806(5) 0.2006(6) 0.074(3) Uani 1 d . . . C31 C 0.5134(8) 0.8448(5) 0.0526(5) 0.054(2) Uani 1 d . . . C32 C 0.5813(9) 0.8027(5) 0.0216(6) 0.075(3) Uani 1 d . . . C33 C 0.5927(10) 0.8084(6) -0.0566(8) 0.094(4) Uani 1 d . . . C34 C 0.5354(10) 0.8558(6) -0.1066(6) 0.082(3) Uani 1 d . . . C35 C 0.4694(8) 0.8967(5) -0.0726(5) 0.063(3) Uani 1 d . . . C36 C 0.4556(7) 0.8920(4) 0.0044(5) 0.048(2) Uani 1 d . . . C42 C 0.3115(8) 0.9680(5) 0.0019(5) 0.057(3) Uani 1 d . . . C43 C 0.2347(8) 1.0135(4) 0.0284(5) 0.057(3) Uani 1 d . . . C44 C 0.1517(8) 1.0366(5) -0.0332(6) 0.064(3) Uani 1 d . . . C45 C 0.0732(9) 1.0753(5) -0.0140(6) 0.068(3) Uani 1 d . . . C46 C 0.0690(11) 1.0940(6) 0.0627(8) 0.095(4) Uani 1 d . . . C47 C 0.1514(11) 1.0738(6) 0.1215(7) 0.083(4) Uani 1 d . . . C48 C 0.2371(9) 1.0331(5) 0.1083(6) 0.060(3) Uani 1 d . . . C51 C 0.3016(8) 0.9284(5) 0.3441(6) 0.061(3) Uani 1 d . . . C52 C 0.3030(8) 0.9152(6) 0.4263(6) 0.071(3) Uani 1 d . . . C53 C 0.2123(11) 0.9103(7) 0.4583(7) 0.088(4) Uani 1 d . . . C54 C 0.1115(11) 0.9181(7) 0.4138(9) 0.091(4) Uani 1 d . . . C55 C 0.1056(9) 0.9334(6) 0.3330(8) 0.086(4) Uani 1 d . . . C56 C 0.2000(9) 0.9373(5) 0.2988(6) 0.068(3) Uani 1 d . . . C57 C 0.0054(10) 0.9116(8) 0.4479(8) 0.114(5) Uani 1 d . . . C61 C 0.5199(8) 0.8829(5) 0.3614(5) 0.054(2) Uani 1 d . . . C62 C 0.6250(8) 0.8999(5) 0.3905(5) 0.052(2) Uani 1 d . . . C63 C 0.6970(9) 0.8547(5) 0.4295(5) 0.063(3) Uani 1 d . . . C64 C 0.6665(10) 0.7912(5) 0.4385(6) 0.066(3) Uani 1 d . . . C65 C 0.5589(10) 0.7736(5) 0.4094(6) 0.070(3) Uani 1 d . . . C66 C 0.4870(9) 0.8180(5) 0.3708(5) 0.064(3) Uani 1 d . . . C67 C 0.7413(10) 0.7376(6) 0.4782(6) 0.089(4) Uani 1 d . . . C71 C 0.4741(5) 1.0234(2) 0.3346(3) 0.047(2) Uani 1 d G . . C72 C 0.4315(4) 1.0575(3) 0.3936(3) 0.060(3) Uani 1 d G . . C73 C 0.4716(5) 1.1196(3) 0.4174(3) 0.067(3) Uani 1 d G . . C74 C 0.5543(6) 1.1476(2) 0.3824(4) 0.063(3) Uani 1 d G . . C75 C 0.5969(5) 1.1135(3) 0.3234(4) 0.069(3) Uani 1 d G . . C76 C 0.5569(5) 1.0514(3) 0.2995(3) 0.068(3) Uani 1 d G . . C77 C 0.6013(11) 1.2143(5) 0.4093(6) 0.090(4) Uani 1 d . . . H12 H 0.5164 0.6980 0.1374 0.116 Uiso 1 calc R . . H13 H 0.4050 0.6095 0.1504 0.131 Uiso 1 calc R . . H14 H 0.2399 0.6264 0.1929 0.147 Uiso 1 calc R . . H15 H 0.1867 0.7299 0.2245 0.135 Uiso 1 calc R . . H16 H 0.2932 0.8218 0.2038 0.096 Uiso 1 calc R . . H22 H 0.6254 0.7376 0.2486 0.060 Uiso 1 calc R . . H23 H 0.8098 0.7261 0.3009 0.075 Uiso 1 calc R . . H24 H 0.9265 0.8114 0.2893 0.082 Uiso 1 calc R . . H25 H 0.8658 0.9074 0.2258 0.087 Uiso 1 calc R . . H26 H 0.6838 0.9199 0.1757 0.089 Uiso 1 calc R . . H32 H 0.6194 0.7704 0.0535 0.090 Uiso 1 calc R . . H33 H 0.6398 0.7800 -0.0773 0.112 Uiso 1 calc R . . H34 H 0.5422 0.8591 -0.1602 0.098 Uiso 1 calc R . . H35 H 0.4320 0.9296 -0.1038 0.075 Uiso 1 calc R . . H42 H 0.3066 0.9630 -0.0529 0.068 Uiso 1 calc R . . H44 H 0.1524 1.0248 -0.0860 0.077 Uiso 1 calc R . . H46 H 0.0120 1.1198 0.0749 0.114 Uiso 1 calc R . . H47 H 0.1497 1.0881 0.1732 0.100 Uiso 1 calc R . . H47A H 0.6171 1.2153 0.4664 0.108 Uiso 1 calc R . . H47B H 0.5497 1.2482 0.3909 0.108 Uiso 1 calc R . . H47C H 0.6670 1.2215 0.3877 0.108 Uiso 1 calc R . . H52 H 0.3697 0.9098 0.4590 0.085 Uiso 1 calc R . . H53 H 0.2177 0.9013 0.5124 0.105 Uiso 1 calc R . . H55 H 0.0383 0.9411 0.3020 0.103 Uiso 1 calc R . . H56 H 0.1946 0.9459 0.2446 0.082 Uiso 1 calc R . . H57A H -0.0514 0.9351 0.4145 0.137 Uiso 1 calc R . . H57B H 0.0150 0.9299 0.5007 0.137 Uiso 1 calc R . . H57C H -0.0139 0.8658 0.4500 0.137 Uiso 1 calc R . . H62 H 0.6483 0.9429 0.3837 0.063 Uiso 1 calc R . . H63 H 0.7674 0.8679 0.4500 0.075 Uiso 1 calc R . . H65 H 0.5360 0.7306 0.4165 0.084 Uiso 1 calc R . . H66 H 0.4163 0.8051 0.3509 0.077 Uiso 1 calc R . . H67A H 0.8155 0.7521 0.4830 0.107 Uiso 1 calc R . . H67B H 0.7319 0.6981 0.4466 0.107 Uiso 1 calc R . . H67C H 0.7240 0.7286 0.5303 0.107 Uiso 1 calc R . . H72 H 0.3762 1.0388 0.4170 0.073 Uiso 1 calc R . . H73 H 0.4431 1.1425 0.4569 0.081 Uiso 1 calc R . . H75 H 0.6523 1.1322 0.2999 0.083 Uiso 1 calc R . . H76 H 0.5854 1.0285 0.2601 0.082 Uiso 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 0.0590(6) 0.0510(5) 0.0477(5) 0.0024(3) 0.0089(3) 0.0042(4) Cl1 0.070(2) 0.078(2) 0.108(2) -0.0178(17) 0.0143(18) -0.0032(18) Cl45 0.074(2) 0.086(2) 0.107(2) 0.0121(17) -0.0025(17) 0.0209(17) P1 0.0568(19) 0.0506(15) 0.0500(14) 0.0034(10) 0.0056(12) 0.0006(13) P2 0.0443(17) 0.0566(16) 0.0529(14) 0.0023(11) 0.0084(11) 0.0016(12) N41 0.037(5) 0.044(4) 0.057(4) 0.004(3) 0.008(4) 0.000(4) O11 0.093(8) 0.116(8) 0.193(11) -0.003(7) 0.024(7) 0.028(7) O12 0.066(6) 0.148(9) 0.117(7) -0.021(6) 0.016(5) -0.020(6) O13 0.112(9) 0.261(15) 0.086(7) -0.029(7) 0.022(6) -0.034(9) O14 0.272(16) 0.082(7) 0.175(11) 0.013(7) 0.074(11) -0.017(9) O49 0.085(6) 0.065(5) 0.061(4) -0.006(3) 0.000(4) 0.011(4) C11 0.066(8) 0.057(7) 0.060(6) -0.001(5) 0.006(6) -0.002(6) C12 0.126(12) 0.058(8) 0.095(9) -0.004(6) -0.015(8) -0.034(8) C13 0.113(13) 0.069(9) 0.123(12) 0.004(8) -0.047(11) -0.001(10) C14 0.150(18) 0.081(11) 0.114(12) 0.033(9) -0.049(12) -0.044(12) C15 0.096(12) 0.145(15) 0.093(10) 0.032(10) 0.004(8) -0.032(11) C16 0.102(11) 0.060(7) 0.071(7) 0.012(5) -0.007(7) -0.031(7) C21 0.067(8) 0.040(5) 0.048(5) -0.002(4) 0.000(5) 0.008(5) C22 0.049(7) 0.047(6) 0.055(5) -0.001(4) 0.015(5) -0.006(5) C23 0.064(9) 0.061(7) 0.062(6) -0.006(5) 0.011(6) 0.008(6) C24 0.046(8) 0.078(8) 0.081(7) -0.003(6) 0.014(6) 0.008(6) C25 0.055(8) 0.077(8) 0.082(7) -0.001(6) 0.003(6) -0.009(7) C26 0.091(10) 0.053(7) 0.076(7) 0.012(5) 0.007(6) -0.009(7) C31 0.051(7) 0.055(6) 0.060(6) 0.003(4) 0.014(5) 0.004(5) C32 0.092(9) 0.080(8) 0.055(7) 0.014(5) 0.018(6) 0.020(7) C33 0.075(9) 0.095(10) 0.118(11) 0.008(8) 0.036(8) 0.032(8) C34 0.097(10) 0.099(9) 0.058(7) 0.003(6) 0.039(6) 0.023(8) C35 0.062(8) 0.073(7) 0.055(6) 0.005(5) 0.015(5) 0.021(6) C36 0.049(6) 0.053(6) 0.044(5) 0.003(4) 0.014(4) -0.001(5) C42 0.074(8) 0.061(6) 0.035(5) 0.001(4) 0.004(5) 0.003(6) C43 0.065(7) 0.049(6) 0.054(6) 0.004(4) 0.005(5) 0.016(5) C44 0.059(7) 0.061(6) 0.072(7) 0.005(5) 0.013(6) 0.011(6) C45 0.076(9) 0.058(7) 0.073(7) 0.012(5) 0.021(6) 0.024(6) C46 0.102(11) 0.073(8) 0.108(10) -0.014(7) 0.015(8) 0.032(8) C47 0.108(11) 0.083(9) 0.064(7) -0.005(6) 0.026(7) 0.022(8) C48 0.073(8) 0.051(6) 0.057(6) 0.004(4) 0.012(5) 0.012(6) C51 0.045(7) 0.064(7) 0.072(7) 0.005(5) 0.005(5) 0.000(5) C52 0.028(6) 0.107(9) 0.078(8) 0.017(6) 0.013(5) 0.009(6) C53 0.065(10) 0.132(11) 0.074(8) 0.005(7) 0.034(7) -0.005(8) C54 0.053(10) 0.098(10) 0.132(13) -0.017(8) 0.043(9) -0.014(7) C55 0.040(8) 0.104(10) 0.113(11) 0.013(7) 0.008(7) 0.002(7) C56 0.048(8) 0.093(8) 0.061(6) 0.005(5) 0.001(6) -0.006(6) C57 0.048(9) 0.157(14) 0.142(13) -0.005(10) 0.033(8) -0.006(9) C61 0.054(7) 0.052(6) 0.058(5) 0.006(4) 0.016(5) -0.005(5) C62 0.054(8) 0.058(6) 0.047(5) 0.005(4) 0.010(5) -0.001(5) C63 0.057(7) 0.072(8) 0.055(6) -0.004(5) -0.004(5) -0.007(6) C64 0.069(9) 0.068(8) 0.062(6) 0.001(5) 0.007(6) 0.025(6) C65 0.080(9) 0.056(7) 0.072(7) 0.000(5) 0.010(6) 0.000(6) C66 0.058(7) 0.072(7) 0.056(6) 0.001(5) -0.010(5) -0.008(6) C67 0.085(10) 0.098(9) 0.079(8) 0.001(6) -0.005(7) 0.040(8) C71 0.046(6) 0.063(6) 0.034(5) 0.011(4) 0.012(4) -0.007(5) C72 0.058(7) 0.082(8) 0.044(5) 0.010(5) 0.016(5) 0.001(6) C73 0.064(8) 0.072(7) 0.066(6) -0.002(5) 0.011(5) 0.011(6) C74 0.075(8) 0.051(6) 0.062(6) -0.009(5) 0.012(5) -0.002(6) C75 0.082(9) 0.066(7) 0.067(6) -0.013(5) 0.035(6) -0.023(6) C76 0.080(9) 0.068(8) 0.063(6) -0.009(5) 0.036(6) -0.003(6) C77 0.128(11) 0.073(8) 0.076(8) -0.012(6) 0.033(7) -0.018(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 O49 2.016(7) . ? Pd1 N41 2.066(7) . ? Pd1 P1 2.229(3) . ? Pd1 P2 2.294(3) . ? P1 C21 1.804(10) . ? P1 C11 1.812(11) . ? P1 C31 1.828(9) . ? C21 C22 1.365(12) . ? C21 C26 1.398(13) . ? C22 C23 1.406(13) . ? C23 C24 1.360(14) . ? C24 C25 1.370(14) . ? C25 C26 1.376(15) . ? C11 C16 1.405(15) . ? C11 C12 1.394(16) . ? C12 C13 1.370(18) . ? C13 C14 1.39(2) . ? C14 C15 1.37(2) . ? C15 C16 1.404(17) . ? C31 C32 1.363(13) . ? C31 C36 1.385(12) . ? C36 C35 1.350(12) . ? C36 N41 1.465(11) . ? C35 C34 1.359(13) . ? C34 C33 1.400(15) . ? C33 C32 1.364(15) . ? P2 C51 1.804(11) . ? P2 C61 1.819(10) . ? P2 C71 1.834(5) . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C74 C77 1.513(11) . ? C75 C76 1.3900 . ? C51 C56 1.386(13) . ? C51 C52 1.420(14) . ? C52 C53 1.333(15) . ? C53 C54 1.369(16) . ? C54 C55 1.397(16) . ? C54 C57 1.531(16) . ? C55 C56 1.395(15) . ? C61 C62 1.369(12) . ? C61 C66 1.393(13) . ? C62 C63 1.375(13) . ? C63 C64 1.356(14) . ? C64 C65 1.399(14) . ? C64 C67 1.519(14) . ? C65 C66 1.362(14) . ? N41 C42 1.279(11) . ? C42 C43 1.451(13) . ? C43 C48 1.410(12) . ? C43 C44 1.429(13) . ? C44 C45 1.333(13) . ? C45 C46 1.367(15) . ? C45 Cl45 1.760(11) . ? C46 C47 1.376(16) . ? C47 C48 1.395(15) . ? C48 O49 1.285(11) . ? Cl1 O11 1.409(10) . ? Cl1 O12 1.406(9) . ? Cl1 O13 1.410(10) . ? Cl1 O14 1.464(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O49 Pd1 N41 90.9(3) . . ? O49 Pd1 P1 173.7(2) . . ? N41 Pd1 P1 84.1(2) . . ? O49 Pd1 P2 86.86(19) . . ? N41 Pd1 P2 177.7(2) . . ? P1 Pd1 P2 98.11(9) . . ? C21 P1 C11 109.6(5) . . ? C21 P1 C31 102.7(4) . . ? C11 P1 C31 106.3(4) . . ? C21 P1 Pd1 123.1(3) . . ? C11 P1 Pd1 112.5(4) . . ? C31 P1 Pd1 100.4(3) . . ? C22 C21 C26 119.1(9) . . ? C22 C21 P1 124.5(8) . . ? C26 C21 P1 116.2(7) . . ? C21 C22 C23 120.5(9) . . ? C24 C23 C22 119.0(10) . . ? C23 C24 C25 121.4(10) . . ? C24 C25 C26 119.7(10) . . ? C25 C26 C21 120.3(10) . . ? C16 C11 C12 119.6(11) . . ? C16 C11 P1 116.5(8) . . ? C12 C11 P1 123.9(10) . . ? C13 C12 C11 121.0(15) . . ? C12 C13 C14 119.3(15) . . ? C15 C14 C13 121.3(16) . . ? C14 C15 C16 120.1(16) . . ? C11 C16 C15 118.6(13) . . ? C32 C31 C36 119.9(9) . . ? C32 C31 P1 121.7(8) . . ? C36 C31 P1 118.4(7) . . ? C35 C36 C31 119.2(9) . . ? C35 C36 N41 126.1(8) . . ? C31 C36 N41 114.6(8) . . ? C36 C35 C34 123.2(10) . . ? C35 C34 C33 116.3(10) . . ? C32 C33 C34 121.9(11) . . ? C33 C32 C31 119.4(10) . . ? C51 P2 C61 103.3(5) . . ? C51 P2 C71 106.1(4) . . ? C61 P2 C71 106.2(4) . . ? C51 P2 Pd1 114.4(4) . . ? C61 P2 Pd1 118.1(3) . . ? C71 P2 Pd1 108.0(2) . . ? C72 C71 C76 120.0 . . ? C72 C71 P2 121.1(4) . . ? C76 C71 P2 118.9(4) . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 C77 120.7(6) . . ? C75 C74 C77 119.2(6) . . ? C76 C75 C74 120.0 . . ? C75 C76 C71 120.0 . . ? C56 C51 C52 116.1(9) . . ? C56 C51 P2 122.4(8) . . ? C52 C51 P2 121.3(8) . . ? C53 C52 C51 122.4(11) . . ? C52 C53 C54 121.9(12) . . ? C53 C54 C55 118.1(11) . . ? C53 C54 C57 123.5(14) . . ? C55 C54 C57 118.5(13) . . ? C56 C55 C54 120.4(11) . . ? C51 C56 C55 121.1(10) . . ? C62 C61 C66 118.5(9) . . ? C62 C61 P2 122.1(7) . . ? C66 C61 P2 119.3(8) . . ? C61 C62 C63 121.4(9) . . ? C64 C63 C62 120.8(10) . . ? C63 C64 C65 118.2(9) . . ? C63 C64 C67 124.4(11) . . ? C65 C64 C67 117.5(11) . . ? C66 C65 C64 121.4(10) . . ? C65 C66 C61 119.7(10) . . ? C42 N41 C36 118.4(8) . . ? C42 N41 Pd1 122.2(6) . . ? C36 N41 Pd1 119.4(5) . . ? N41 C42 C43 128.0(8) . . ? C48 C43 C44 121.1(9) . . ? C48 C43 C42 124.2(8) . . ? C44 C43 C42 114.6(8) . . ? C45 C44 C43 119.1(10) . . ? C44 C45 C46 122.5(11) . . ? C44 C45 Cl45 120.5(9) . . ? C46 C45 Cl45 116.9(9) . . ? C45 C46 C47 118.2(11) . . ? C46 C47 C48 124.1(11) . . ? O49 C48 C47 120.8(9) . . ? O49 C48 C43 124.3(9) . . ? C47 C48 C43 114.9(9) . . ? C48 O49 Pd1 125.4(6) . . ? O11 Cl1 O12 111.2(6) . . ? O11 Cl1 O13 111.4(7) . . ? O12 Cl1 O13 111.8(6) . . ? O11 Cl1 O14 103.3(7) . . ? O12 Cl1 O14 109.8(7) . . ? O13 Cl1 O14 108.9(7) . . ? _refine_diff_density_max 0.666 _refine_diff_density_min -0.762 _refine_diff_density_rms 0.108 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1997) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #===END data_26 _database_code_depnum_ccdc_archive 'CCDC 249212' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H39 Cl2 N O5 P2 Pt' _chemical_formula_weight 1013.71 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' Pt Pt -1.7033 8.3905 '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' Cl Cl 0.1484 0.1585 '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 12.410(14) _cell_length_b 20.28(2) _cell_length_c 16.972(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.960(10) _cell_angle_gamma 90.00 _cell_volume 4220(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.94 _cell_measurement_theta_max 26.07 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 3.575 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.220 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 10 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10800 _diffrn_reflns_av_R_equivalents 0.2278 _diffrn_reflns_av_sigmaI/netI 0.4268 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.07 _reflns_number_total 6522 _reflns_number_gt 2301 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics PLATON(Spek,1994) _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 w=1/[\s^2^(Fo^2^)+(0.1323P)^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 6522 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.3498 _refine_ls_R_factor_gt 0.1197 _refine_ls_wR_factor_ref 0.3193 _refine_ls_wR_factor_gt 0.2512 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.033 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.40508(10) 0.93402(6) 0.16781(6) 0.0452(5) Uani 1 d . . . P1 P 0.4953(6) 0.8410(4) 0.1562(4) 0.044(2) Uani 1 d . . . P2 P 0.4234(6) 0.9405(4) 0.3027(4) 0.0382(18) Uani 1 d . . . Cl1 Cl -0.1478(8) 1.0745(5) 0.2270(5) 0.080(3) Uani 1 d . . . Cl45 Cl -0.0314(7) 1.1043(5) -0.0882(5) 0.081(3) Uani 1 d . . . N41 N 0.3844(16) 0.9314(11) 0.0457(10) 0.036(5) Uiso 1 d . . . O11 O -0.059(3) 1.0316(18) 0.2196(18) 0.140(11) Uiso 1 d . . . O12 O -0.249(2) 1.0427(13) 0.1997(13) 0.094(8) Uiso 1 d . . . O13 O -0.143(2) 1.0978(15) 0.3018(17) 0.116(9) Uiso 1 d . . . O14 O -0.133(3) 1.131(3) 0.174(2) 0.203(17) Uiso 1 d . . . O49 O 0.3077(16) 1.0145(10) 0.1655(10) 0.061(6) Uiso 1 d . . . C11 C 0.411(2) 0.7691(13) 0.1685(15) 0.046(7) Uiso 1 d . . . C12 C 0.450(3) 0.7063(16) 0.1557(16) 0.063(9) Uiso 1 d . . . C13 C 0.375(3) 0.6574(18) 0.1647(17) 0.070(10) Uiso 1 d . . . C14 C 0.275(3) 0.659(2) 0.186(2) 0.097(12) Uiso 1 d . . . C15 C 0.250(3) 0.725(2) 0.205(2) 0.095(12) Uiso 1 d . . . C16 C 0.313(3) 0.7798(17) 0.1972(16) 0.066(9) Uiso 1 d . . . C21 C 0.636(2) 0.8271(12) 0.2076(13) 0.032(6) Uiso 1 d . . . C22 C 0.677(2) 0.7762(14) 0.2483(14) 0.047(7) Uiso 1 d . . . C23 C 0.775(2) 0.7662(15) 0.2722(15) 0.050(8) Uiso 1 d . . . C24 C 0.859(3) 0.8151(18) 0.2694(18) 0.077(10) Uiso 1 d . . . C25 C 0.817(3) 0.8752(17) 0.2317(16) 0.065(9) Uiso 1 d . . . C26 C 0.698(2) 0.8793(14) 0.1986(14) 0.046(7) Uiso 1 d . . . C31 C 0.506(2) 0.8436(12) 0.0537(12) 0.027(6) Uiso 1 d . . . C32 C 0.575(3) 0.8069(18) 0.0270(19) 0.080(11) Uiso 1 d . . . C33 C 0.595(3) 0.8065(18) -0.0551(18) 0.075(10) Uiso 1 d . . . C34 C 0.534(3) 0.8520(16) -0.1014(18) 0.062(9) Uiso 1 d . . . C35 C 0.470(2) 0.8996(16) -0.0693(16) 0.055(8) Uiso 1 d . . . C36 C 0.4527(19) 0.8894(12) 0.0045(12) 0.027(6) Uiso 1 d . . . C42 C 0.310(2) 0.9645(16) 0.0024(17) 0.060(8) Uiso 1 d . . . C43 C 0.234(2) 1.0136(13) 0.0285(13) 0.035(6) Uiso 1 d . . . C44 C 0.158(2) 1.0368(15) -0.0343(16) 0.053(8) Uiso 1 d . . . C45 C 0.077(3) 1.0773(16) -0.0190(17) 0.063(9) Uiso 1 d . . . C46 C 0.074(3) 1.0934(17) 0.0658(18) 0.076(10) Uiso 1 d . . . C47 C 0.160(2) 1.0725(16) 0.1226(17) 0.061(8) Uiso 1 d . . . C48 C 0.237(2) 1.0295(15) 0.1064(15) 0.047(7) Uiso 1 d . . . C51 C 0.298(2) 0.9286(17) 0.3420(16) 0.061(8) Uiso 1 d . . . C52 C 0.304(3) 0.9193(16) 0.4226(18) 0.068(9) Uiso 1 d . . . C53 C 0.202(4) 0.917(2) 0.456(3) 0.121(16) Uiso 1 d . . . C54 C 0.106(3) 0.9197(18) 0.407(2) 0.083(11) Uiso 1 d . . . C55 C 0.101(3) 0.9274(15) 0.3247(17) 0.062(8) Uiso 1 d . . . C56 C 0.200(3) 0.9386(16) 0.2958(17) 0.063(8) Uiso 1 d . . . C57 C 0.002(3) 0.919(2) 0.445(2) 0.113(15) Uiso 1 d . . . C61 C 0.518(2) 0.8813(15) 0.3578(14) 0.046(7) Uiso 1 d . . . C62 C 0.626(2) 0.9003(15) 0.3891(15) 0.051(8) Uiso 1 d . . . C63 C 0.690(3) 0.8592(17) 0.4281(17) 0.069(9) Uiso 1 d . . . C64 C 0.670(3) 0.7949(18) 0.4376(18) 0.075(10) Uiso 1 d . . . C65 C 0.557(2) 0.7724(16) 0.4109(15) 0.057(8) Uiso 1 d . . . C66 C 0.487(2) 0.8174(14) 0.3692(14) 0.049(7) Uiso 1 d . . . C67 C 0.744(2) 0.7354(15) 0.4756(16) 0.061(9) Uiso 1 d . . . C71 C 0.4746(14) 1.0229(7) 0.3337(9) 0.040(7) Uiso 1 d G . . C72 C 0.4320(12) 1.0558(8) 0.3938(9) 0.039(6) Uiso 1 d G . . C73 C 0.4701(15) 1.1182(8) 0.4177(9) 0.057(8) Uiso 1 d G . . C74 C 0.5509(16) 1.1477(7) 0.3816(11) 0.066(9) Uiso 1 d G . . C75 C 0.5935(13) 1.1149(9) 0.3215(10) 0.064(9) Uiso 1 d G . . C76 C 0.5554(14) 1.0525(8) 0.2975(8) 0.042(7) Uiso 1 d G . . C77 C 0.597(3) 1.216(2) 0.408(2) 0.103(13) Uiso 1 d . . . H12 H 0.5187 0.6981 0.1426 0.075 Uiso 1 calc R . . H13 H 0.3983 0.6153 0.1536 0.084 Uiso 1 calc R . . H14 H 0.2297 0.6226 0.1889 0.116 Uiso 1 calc R . . H15 H 0.1848 0.7321 0.2237 0.114 Uiso 1 calc R . . H16 H 0.2920 0.8217 0.2105 0.079 Uiso 1 calc R . . H22 H 0.6284 0.7444 0.2604 0.057 Uiso 1 calc R . . H23 H 0.7953 0.7249 0.2933 0.059 Uiso 1 calc R . . H24 H 0.9326 0.8082 0.2897 0.093 Uiso 1 calc R . . H25 H 0.8633 0.9110 0.2279 0.078 Uiso 1 calc R . . H26 H 0.6679 0.9170 0.1727 0.055 Uiso 1 calc R . . H32 H 0.6149 0.7780 0.0626 0.096 Uiso 1 calc R . . H33 H 0.6439 0.7781 -0.0739 0.090 Uiso 1 calc R . . H34 H 0.5353 0.8518 -0.1561 0.074 Uiso 1 calc R . . H35 H 0.4423 0.9362 -0.0985 0.066 Uiso 1 calc R . . H42 H 0.3027 0.9571 -0.0523 0.072 Uiso 1 calc R . . H44 H 0.1624 1.0245 -0.0864 0.063 Uiso 1 calc R . . H46 H 0.0162 1.1169 0.0807 0.091 Uiso 1 calc R . . H47 H 0.1652 1.0889 0.1742 0.073 Uiso 1 calc R . . H47A H 0.5963 1.2218 0.4644 0.123 Uiso 1 calc R . . H47B H 0.5528 1.2500 0.3794 0.123 Uiso 1 calc R . . H47C H 0.6705 1.2200 0.3977 0.123 Uiso 1 calc R . . H52 H 0.3711 0.9142 0.4553 0.081 Uiso 1 calc R . . H53 H 0.2032 0.9147 0.5111 0.145 Uiso 1 calc R . . H55 H 0.0354 0.9253 0.2903 0.074 Uiso 1 calc R . . H56 H 0.1982 0.9533 0.2437 0.076 Uiso 1 calc R . . H57A H -0.0483 0.9506 0.4196 0.136 Uiso 1 calc R . . H57B H 0.0203 0.9288 0.5009 0.136 Uiso 1 calc R . . H57C H -0.0300 0.8755 0.4390 0.136 Uiso 1 calc R . . H62 H 0.6501 0.9429 0.3810 0.061 Uiso 1 calc R . . H63 H 0.7580 0.8748 0.4523 0.082 Uiso 1 calc R . . H65 H 0.5347 0.7300 0.4216 0.069 Uiso 1 calc R . . H66 H 0.4163 0.8041 0.3482 0.058 Uiso 1 calc R . . H67A H 0.8091 0.7527 0.5071 0.074 Uiso 1 calc R . . H67B H 0.7638 0.7083 0.4338 0.074 Uiso 1 calc R . . H67C H 0.7047 0.7096 0.5089 0.074 Uiso 1 calc R . . H72 H 0.3779 1.0360 0.4179 0.046 Uiso 1 calc R . . H73 H 0.4416 1.1402 0.4579 0.069 Uiso 1 calc R . . H75 H 0.6476 1.1347 0.2973 0.077 Uiso 1 calc R . . H76 H 0.5839 1.0305 0.2573 0.050 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0482(8) 0.0440(7) 0.0428(6) 0.0031(7) 0.0055(5) 0.0061(8) P1 0.049(6) 0.041(5) 0.042(4) 0.005(3) 0.003(4) 0.001(4) P2 0.027(4) 0.037(5) 0.053(4) -0.005(4) 0.015(3) 0.002(4) Cl45 0.056(6) 0.076(7) 0.108(7) 0.011(5) 0.002(5) 0.026(5) Cl1 0.072(7) 0.076(7) 0.091(6) -0.036(5) 0.010(5) 0.000(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 Pt1 O49 2.03(2) . ? Pt1 N41 2.049(17) . ? Pt1 P1 2.219(8) . ? Pt1 P2 2.269(7) . ? P1 C31 1.77(2) . ? P1 C11 1.82(3) . ? P1 C21 1.84(2) . ? C21 C22 1.30(3) . ? C21 C26 1.33(3) . ? C22 C23 1.23(3) . ? C23 C24 1.45(4) . ? C24 C25 1.44(4) . ? C25 C26 1.51(4) . ? C11 C12 1.39(4) . ? C11 C16 1.40(4) . ? C12 C13 1.38(4) . ? C13 C14 1.35(4) . ? C14 C15 1.42(5) . ? C15 C16 1.38(5) . ? C31 C32 1.26(4) . ? C31 C36 1.35(3) . ? C36 C35 1.32(3) . ? C36 N41 1.46(3) . ? C35 C34 1.41(4) . ? C34 C33 1.36(4) . ? C33 C32 1.45(4) . ? P2 C51 1.80(3) . ? P2 C61 1.83(3) . ? P2 C71 1.835(15) . ? C71 C72 1.3900 . ? C71 C76 1.3900 . ? C72 C73 1.3900 . ? C73 C74 1.3900 . ? C74 C75 1.3900 . ? C74 C77 1.55(4) . ? C75 C76 1.3900 . ? C51 C56 1.36(4) . ? C51 C52 1.37(4) . ? C52 C53 1.47(5) . ? C53 C54 1.34(5) . ? C54 C55 1.40(4) . ? C54 C57 1.52(5) . ? C55 C56 1.41(4) . ? C61 C66 1.38(4) . ? C61 C62 1.42(4) . ? C62 C63 1.27(4) . ? C63 C64 1.34(4) . ? C64 C65 1.47(4) . ? C64 C67 1.59(4) . ? C65 C66 1.38(4) . ? N41 C42 1.28(3) . ? C42 C43 1.49(4) . ? C43 C48 1.36(3) . ? C43 C44 1.39(3) . ? C44 C45 1.35(4) . ? C45 C46 1.48(4) . ? C45 Cl45 1.73(3) . ? C46 C47 1.39(4) . ? C47 C48 1.35(4) . ? C48 O49 1.26(3) . ? Cl1 O13 1.35(3) . ? Cl1 O12 1.42(3) . ? Cl1 O11 1.42(3) . ? Cl1 O14 1.49(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 O49 Pt1 N41 91.2(8) . . ? O49 Pt1 P1 172.1(5) . . ? N41 Pt1 P1 82.7(6) . . ? O49 Pt1 P2 86.5(5) . . ? N41 Pt1 P2 177.7(6) . . ? P1 Pt1 P2 99.6(3) . . ? C31 P1 C11 105.6(12) . . ? C31 P1 C21 105.0(12) . . ? C11 P1 C21 109.8(12) . . ? C31 P1 Pt1 100.3(8) . . ? C11 P1 Pt1 111.4(10) . . ? C21 P1 Pt1 122.7(8) . . ? C22 C21 C26 120(3) . . ? C22 C21 P1 130(2) . . ? C26 C21 P1 110.2(19) . . ? C23 C22 C21 126(3) . . ? C22 C23 C24 124(3) . . ? C25 C24 C23 112(3) . . ? C24 C25 C26 119(3) . . ? C21 C26 C25 118(3) . . ? C12 C11 C16 123(3) . . ? C12 C11 P1 120(3) . . ? C16 C11 P1 117(2) . . ? C13 C12 C11 113(3) . . ? C14 C13 C12 133(4) . . ? C13 C14 C15 109(4) . . ? C16 C15 C14 127(4) . . ? C15 C16 C11 117(3) . . ? C32 C31 C36 118(2) . . ? C32 C31 P1 120(2) . . ? C36 C31 P1 121.5(19) . . ? C35 C36 C31 124(3) . . ? C35 C36 N41 124(2) . . ? C31 C36 N41 111.9(19) . . ? C36 C35 C34 117(3) . . ? C33 C34 C35 122(3) . . ? C34 C33 C32 113(3) . . ? C31 C32 C33 125(3) . . ? C51 P2 C61 104.2(14) . . ? C51 P2 C71 107.2(12) . . ? C61 P2 C71 106.5(11) . . ? C51 P2 Pt1 114.2(9) . . ? C61 P2 Pt1 115.7(9) . . ? C71 P2 Pt1 108.5(6) . . ? C72 C71 C76 120.0 . . ? C72 C71 P2 119.5(10) . . ? C76 C71 P2 120.5(10) . . ? C71 C72 C73 120.0 . . ? C74 C73 C72 120.0 . . ? C73 C74 C75 120.0 . . ? C73 C74 C77 121.2(19) . . ? C75 C74 C77 118.7(19) . . ? C76 C75 C74 120.0 . . ? C75 C76 C71 120.0 . . ? C56 C51 C52 120(3) . . ? C56 C51 P2 121(2) . . ? C52 C51 P2 118(2) . . ? C51 C52 C53 118(3) . . ? C54 C53 C52 120(4) . . ? C53 C54 C55 121(4) . . ? C53 C54 C57 117(4) . . ? C55 C54 C57 121(3) . . ? C54 C55 C56 118(3) . . ? C51 C56 C55 122(3) . . ? C66 C61 C62 118(3) . . ? C66 C61 P2 121(2) . . ? C62 C61 P2 121(2) . . ? C63 C62 C61 120(3) . . ? C62 C63 C64 126(3) . . ? C63 C64 C65 117(3) . . ? C63 C64 C67 132(3) . . ? C65 C64 C67 111(3) . . ? C66 C65 C64 117(3) . . ? C65 C66 C61 122(3) . . ? C42 N41 C36 117(2) . . ? C42 N41 Pt1 122(2) . . ? C36 N41 Pt1 120.7(14) . . ? N41 C42 C43 128(3) . . ? C48 C43 C44 125(3) . . ? C48 C43 C42 122(2) . . ? C44 C43 C42 113(2) . . ? C45 C44 C43 120(3) . . ? C44 C45 C46 117(3) . . ? C44 C45 Cl45 126(2) . . ? C46 C45 Cl45 117(3) . . ? C47 C46 C45 118(3) . . ? C48 C47 C46 123(3) . . ? O49 C48 C47 115(2) . . ? O49 C48 C43 129(3) . . ? C47 C48 C43 116(2) . . ? C48 O49 Pt1 123.2(18) . . ? O13 Cl1 O12 111.8(17) . . ? O13 Cl1 O11 112.3(18) . . ? O12 Cl1 O11 110.3(19) . . ? O13 Cl1 O14 108(2) . . ? O12 Cl1 O14 110(2) . . ? O11 Cl1 O14 105(2) . . ? _refine_diff_density_max 1.003 _refine_diff_density_min -1.272 _refine_diff_density_rms 0.211 #===END