# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_rrm1s_compound_7a _database_code_depnum_ccdc_archive 'CCDC 881653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H31 Cl4 N2 P Pd' _chemical_formula_weight 638.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 21.6139(4) _cell_length_b 21.6139(4) _cell_length_c 11.7959(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5510.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 28.25 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.136 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7721 _exptl_absorpt_correction_T_max 0.8391 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 62664 _diffrn_reflns_av_R_equivalents 0.0235 _diffrn_reflns_av_sigmaI/netI 0.0142 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 28.25 _reflns_number_total 6569 _reflns_number_gt 6447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+8.2314P] 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 'NH free, Me rigid, othes riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 6569 _refine_ls_number_parameters 302 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0793 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.098 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.484563(9) 0.353584(9) 0.20017(2) 0.01403(6) Uani 1 1 d . . . N1 N 0.42403(11) 0.42586(11) 0.1879(2) 0.0157(5) Uani 1 1 d . . . H01 H 0.4511(16) 0.4595(16) 0.206(3) 0.018(8) Uiso 1 1 d . . . N2 N 0.41218(11) 0.29227(12) 0.1815(2) 0.0163(5) Uani 1 1 d . . . Cl1 Cl 0.55799(3) 0.27609(3) 0.20335(8) 0.02005(13) Uani 1 1 d . . . Cl2 Cl 0.56164(3) 0.42611(3) 0.22439(6) 0.01935(15) Uani 1 1 d . . . P1 P 0.37453(3) 0.29991(3) 0.06379(6) 0.01499(14) Uani 1 1 d . . . C1 C 0.39966(14) 0.43026(14) 0.0704(2) 0.0180(6) Uani 1 1 d . . . H1A H 0.4346 0.4275 0.0165 0.022 Uiso 1 1 calc R . . H1B H 0.3799 0.4712 0.0602 0.022 Uiso 1 1 calc R . . C2 C 0.35318(14) 0.38023(14) 0.0426(3) 0.0188(5) Uani 1 1 d . . . H2A H 0.3414 0.3852 -0.0380 0.023 Uiso 1 1 calc R . . H2B H 0.3156 0.3883 0.0883 0.023 Uiso 1 1 calc R . . C3 C 0.37472(14) 0.43188(14) 0.2747(2) 0.0189(6) Uani 1 1 d . . . H3A H 0.3477 0.3950 0.2716 0.023 Uiso 1 1 calc R . . H3B H 0.3490 0.4686 0.2570 0.023 Uiso 1 1 calc R . . C4 C 0.40065(15) 0.43841(15) 0.3939(3) 0.0215(6) Uani 1 1 d . . . H4A H 0.4361 0.4674 0.3933 0.026 Uiso 1 1 calc R . . H4B H 0.4155 0.3977 0.4212 0.026 Uiso 1 1 calc R . . C5 C 0.35014(18) 0.46284(17) 0.4730(3) 0.0284(7) Uani 1 1 d . . . H5A H 0.3383 0.5047 0.4497 0.043 Uiso 1 1 calc R . . H5B H 0.3658 0.4638 0.5510 0.043 Uiso 1 1 calc R . . H5C H 0.3139 0.4356 0.4691 0.043 Uiso 1 1 calc R . . C11 C 0.41484(14) 0.23593(14) 0.2442(3) 0.0175(6) Uani 1 1 d . . . C12 C 0.40040(13) 0.17811(13) 0.1995(3) 0.0202(5) Uani 1 1 d . . . H12 H 0.3870 0.1748 0.1230 0.024 Uiso 1 1 calc R . . C13 C 0.40553(15) 0.12473(14) 0.2664(3) 0.0218(6) Uani 1 1 d . . . H13 H 0.3948 0.0857 0.2348 0.026 Uiso 1 1 calc R . . C14 C 0.42596(15) 0.12771(15) 0.3777(3) 0.0228(6) Uani 1 1 d . . . C15 C 0.44007(17) 0.18576(16) 0.4221(3) 0.0255(7) Uani 1 1 d . . . H15 H 0.4540 0.1889 0.4982 0.031 Uiso 1 1 calc R . . C16 C 0.43420(15) 0.23918(15) 0.3574(3) 0.0203(6) Uani 1 1 d . . . H16 H 0.4434 0.2782 0.3902 0.024 Uiso 1 1 calc R . . C17 C 0.43434(19) 0.06993(17) 0.4468(3) 0.0312(7) Uani 1 1 d . . . H17A H 0.4132 0.0354 0.4095 0.037 Uiso 1 1 calc R . . H17B H 0.4168 0.0762 0.5226 0.037 Uiso 1 1 calc R . . H17C H 0.4785 0.0605 0.4535 0.037 Uiso 1 1 calc R . . C21 C 0.30014(14) 0.26246(14) 0.0727(3) 0.0192(6) Uani 1 1 d . . . C22 C 0.27634(15) 0.22312(15) -0.0107(3) 0.0217(6) Uani 1 1 d . . . H22 H 0.3005 0.2126 -0.0751 0.026 Uiso 1 1 calc R . . C23 C 0.21675(17) 0.19964(18) 0.0021(3) 0.0283(7) Uani 1 1 d . . . H23 H 0.2000 0.1732 -0.0545 0.034 Uiso 1 1 calc R . . C24 C 0.18163(15) 0.21458(18) 0.0966(3) 0.0294(7) Uani 1 1 d . . . H24 H 0.1411 0.1982 0.1045 0.035 Uiso 1 1 calc R . . C25 C 0.20543(15) 0.25335(17) 0.1798(3) 0.0271(7) Uani 1 1 d . . . H25 H 0.1813 0.2634 0.2445 0.033 Uiso 1 1 calc R . . C26 C 0.26446(15) 0.27717(16) 0.1676(3) 0.0236(6) Uani 1 1 d . . . H26 H 0.2809 0.3038 0.2243 0.028 Uiso 1 1 calc R . . C31 C 0.41557(14) 0.27294(14) -0.0594(3) 0.0186(6) Uani 1 1 d . . . C32 C 0.39310(15) 0.28293(15) -0.1696(3) 0.0213(6) Uani 1 1 d . . . H32 H 0.3559 0.3056 -0.1806 0.026 Uiso 1 1 calc R . . C33 C 0.42499(16) 0.25989(15) -0.2620(3) 0.0251(7) Uani 1 1 d . . . H33 H 0.4091 0.2657 -0.3363 0.030 Uiso 1 1 calc R . . C34 C 0.48056(17) 0.22816(16) -0.2462(3) 0.0269(7) Uani 1 1 d . . . H34 H 0.5025 0.2125 -0.3098 0.032 Uiso 1 1 calc R . . C35 C 0.50383(16) 0.21936(16) -0.1374(3) 0.0246(7) Uani 1 1 d . . . H35 H 0.5419 0.1982 -0.1269 0.029 Uiso 1 1 calc R . . C36 C 0.47156(15) 0.24149(14) -0.0441(3) 0.0215(6) Uani 1 1 d . . . H36 H 0.4875 0.2353 0.0301 0.026 Uiso 1 1 calc R . . C99 C 0.5695(4) 0.1184(4) 0.1365(8) 0.055(2) Uiso 0.591(10) 1 d PD A 1 H99A H 0.5344 0.1095 0.0850 0.065 Uiso 0.591(10) 1 calc PR A 1 H99B H 0.5593 0.1568 0.1783 0.065 Uiso 0.591(10) 1 calc PR A 1 Cl3 Cl 0.5755(2) 0.0584(2) 0.2335(4) 0.0823(11) Uiso 0.591(10) 1 d PD A 1 Cl4 Cl 0.6339(2) 0.1317(2) 0.0561(5) 0.0900(12) Uiso 0.591(10) 1 d PD A 1 C99' C 0.5856(6) 0.1228(6) 0.2009(16) 0.071(4) Uiso 0.409(10) 1 d PD A 2 H99C H 0.6015 0.1337 0.2771 0.085 Uiso 0.409(10) 1 calc PR A 2 H99D H 0.5510 0.1512 0.1830 0.085 Uiso 0.409(10) 1 calc PR A 2 Cl3' Cl 0.55810(18) 0.04616(16) 0.2023(4) 0.0489(12) Uiso 0.409(10) 1 d PD A 2 Cl4' Cl 0.6462(3) 0.1331(3) 0.0983(7) 0.0963(19) Uiso 0.409(10) 1 d PD A 2 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 0.01342(10) 0.01433(10) 0.01433(9) 0.00024(9) -0.00039(8) -0.00060(8) N1 0.0161(11) 0.0154(11) 0.0155(12) -0.0013(10) -0.0002(10) -0.0004(9) N2 0.0158(11) 0.0173(11) 0.0158(13) 0.0014(9) -0.0022(9) -0.0005(9) Cl1 0.0166(3) 0.0191(3) 0.0244(3) 0.0021(3) -0.0019(3) 0.0024(2) Cl2 0.0174(3) 0.0184(3) 0.0222(4) -0.0010(3) -0.0005(2) -0.0036(2) P1 0.0141(3) 0.0162(3) 0.0147(3) 0.0000(3) -0.0009(3) -0.0003(3) C1 0.0204(14) 0.0180(14) 0.0156(13) -0.0001(11) 0.0003(11) 0.0016(11) C2 0.0185(13) 0.0204(13) 0.0175(13) 0.0019(11) -0.0025(11) 0.0016(11) C3 0.0172(13) 0.0224(14) 0.0171(14) 0.0006(11) 0.0021(10) 0.0011(11) C4 0.0259(16) 0.0200(15) 0.0185(14) -0.0022(12) -0.0011(12) -0.0004(12) C5 0.0360(18) 0.0328(17) 0.0165(14) -0.0020(12) 0.0060(14) 0.0007(15) C11 0.0139(13) 0.0212(14) 0.0173(13) 0.0022(11) 0.0026(11) -0.0010(11) C12 0.0226(13) 0.0203(13) 0.0175(12) -0.0014(13) -0.0027(13) 0.0010(11) C13 0.0244(15) 0.0162(13) 0.0248(15) -0.0003(11) 0.0014(12) -0.0011(11) C14 0.0230(15) 0.0215(15) 0.0240(15) 0.0049(12) 0.0050(12) -0.0001(12) C15 0.0326(18) 0.0280(17) 0.0158(14) 0.0008(12) -0.0003(12) 0.0009(13) C16 0.0255(16) 0.0178(14) 0.0177(14) -0.0020(11) -0.0011(12) -0.0017(12) C17 0.041(2) 0.0249(18) 0.0282(15) 0.0071(14) 0.0016(15) 0.0027(13) C21 0.0160(13) 0.0218(15) 0.0200(14) 0.0022(11) -0.0032(11) -0.0036(11) C22 0.0215(15) 0.0233(15) 0.0203(14) -0.0010(12) -0.0018(12) -0.0029(12) C23 0.0243(16) 0.0332(18) 0.0275(16) -0.0030(14) -0.0038(13) -0.0079(14) C24 0.0175(15) 0.0387(19) 0.0321(18) 0.0027(15) -0.0004(13) -0.0081(13) C25 0.0206(15) 0.0351(17) 0.0255(17) 0.0005(13) 0.0041(12) -0.0050(13) C26 0.0224(15) 0.0284(16) 0.0201(14) 0.0000(12) 0.0006(11) -0.0021(12) C31 0.0181(13) 0.0179(13) 0.0198(14) -0.0014(11) 0.0038(11) -0.0051(11) C32 0.0210(14) 0.0213(15) 0.0216(15) 0.0000(11) 0.0000(11) -0.0032(11) C33 0.0321(17) 0.0264(16) 0.0167(14) -0.0019(12) -0.0003(13) -0.0049(14) C34 0.0291(17) 0.0269(16) 0.0246(15) -0.0069(13) 0.0069(14) -0.0059(13) C35 0.0228(15) 0.0219(15) 0.0290(16) -0.0046(13) 0.0034(13) 0.0016(12) C36 0.0234(15) 0.0196(14) 0.0214(14) -0.0007(12) -0.0012(12) -0.0019(12) _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 N1 2.043(2) . ? Pd1 N2 2.062(2) . ? Pd1 Cl2 2.3053(7) . ? Pd1 Cl1 2.3077(7) . ? N1 C3 1.483(4) . ? N1 C1 1.486(4) . ? N2 C11 1.426(4) . ? N2 P1 1.618(3) . ? P1 C31 1.799(3) . ? P1 C21 1.803(3) . ? P1 C2 1.814(3) . ? C1 C2 1.512(4) . ? C3 C4 1.520(4) . ? C4 C5 1.531(5) . ? C11 C12 1.392(4) . ? C11 C16 1.400(4) . ? C12 C13 1.402(4) . ? C13 C14 1.387(5) . ? C14 C15 1.393(5) . ? C14 C17 1.502(4) . ? C15 C16 1.390(4) . ? C21 C26 1.396(4) . ? C21 C22 1.398(4) . ? C22 C23 1.393(5) . ? C23 C24 1.387(5) . ? C24 C25 1.389(5) . ? C25 C26 1.383(4) . ? C31 C36 1.400(4) . ? C31 C32 1.404(4) . ? C32 C33 1.383(5) . ? C33 C34 1.396(5) . ? C34 C35 1.392(5) . ? C35 C36 1.387(5) . ? C99 Cl4 1.710(8) . ? C99 Cl3 1.735(9) . ? C99' Cl3' 1.761(13) . ? C99' Cl4' 1.797(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 89.89(10) . . ? N1 Pd1 Cl2 87.23(7) . . ? N2 Pd1 Cl2 176.88(7) . . ? N1 Pd1 Cl1 175.31(7) . . ? N2 Pd1 Cl1 93.27(7) . . ? Cl2 Pd1 Cl1 89.69(3) . . ? C3 N1 C1 112.5(2) . . ? C3 N1 Pd1 118.59(19) . . ? C1 N1 Pd1 110.00(18) . . ? C11 N2 P1 123.6(2) . . ? C11 N2 Pd1 117.55(19) . . ? P1 N2 Pd1 114.07(13) . . ? N2 P1 C31 114.33(14) . . ? N2 P1 C21 110.65(14) . . ? C31 P1 C21 109.95(14) . . ? N2 P1 C2 110.12(14) . . ? C31 P1 C2 108.92(14) . . ? C21 P1 C2 102.17(14) . . ? N1 C1 C2 113.1(2) . . ? C1 C2 P1 119.1(2) . . ? N1 C3 C4 112.4(2) . . ? C3 C4 C5 109.5(3) . . ? C12 C11 C16 118.3(3) . . ? C12 C11 N2 124.1(3) . . ? C16 C11 N2 117.6(3) . . ? C11 C12 C13 120.5(3) . . ? C14 C13 C12 121.3(3) . . ? C13 C14 C15 117.8(3) . . ? C13 C14 C17 120.9(3) . . ? C15 C14 C17 121.2(3) . . ? C16 C15 C14 121.5(3) . . ? C15 C16 C11 120.6(3) . . ? C26 C21 C22 120.0(3) . . ? C26 C21 P1 115.9(2) . . ? C22 C21 P1 124.1(2) . . ? C23 C22 C21 119.1(3) . . ? C24 C23 C22 120.5(3) . . ? C23 C24 C25 120.4(3) . . ? C26 C25 C24 119.5(3) . . ? C25 C26 C21 120.5(3) . . ? C36 C31 C32 119.5(3) . . ? C36 C31 P1 118.7(2) . . ? C32 C31 P1 121.8(2) . . ? C33 C32 C31 120.1(3) . . ? C32 C33 C34 120.0(3) . . ? C35 C34 C33 120.1(3) . . ? C36 C35 C34 120.2(3) . . ? C35 C36 C31 120.0(3) . . ? Cl4 C99 Cl3 115.5(6) . . ? Cl3' C99' Cl4' 111.7(9) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H01 Cl2 0.96(4) 2.50(4) 3.243(2) 135(3) 2_665 _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.874 _refine_diff_density_min -1.108 _refine_diff_density_rms 0.094 data_rrm37s_compound_u-8b _database_code_depnum_ccdc_archive 'CCDC 881654' #TrackingRef 'daltontrans-completo.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H30 Br Cl2 N2 P Pd' _chemical_formula_weight 694.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5072(4) _cell_length_b 20.6152(9) _cell_length_c 16.0082(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.562(2) _cell_angle_gamma 90.00 _cell_volume 2789.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7729 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.68 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.369 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.773 _exptl_absorpt_correction_T_max 0.9323 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32047 _diffrn_reflns_av_R_equivalents 0.0439 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.22 _reflns_number_total 6497 _reflns_number_gt 5640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+1.6864P] 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 'NH free, Me rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6497 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0782 _refine_ls_wR_factor_gt 0.0750 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.42187(2) 0.628533(10) 0.961333(13) 0.01174(6) Uani 1 1 d . . . N1 N 0.4862(3) 0.69927(11) 0.88127(14) 0.0133(5) Uani 1 1 d . . . N2 N 0.6555(3) 0.60121(12) 0.99030(14) 0.0129(5) Uani 1 1 d . . . H02 H 0.639(3) 0.5635(15) 1.0032(18) 0.007(7) Uiso 1 1 d . . . P1 P 0.57037(8) 0.67380(3) 0.80171(4) 0.01140(14) Uani 1 1 d . . . Cl1 Cl 0.15927(8) 0.65326(4) 0.92524(5) 0.02132(16) Uani 1 1 d . . . Cl2 Cl 0.36402(8) 0.55357(3) 1.06006(4) 0.01841(15) Uani 1 1 d . . . Br1 Br 0.20709(3) 0.969003(14) 0.92217(2) 0.02256(8) Uani 1 1 d . . . C1 C 0.6524(3) 0.59446(13) 0.83416(16) 0.0121(5) Uani 1 1 d . . . H1 H 0.5601 0.5663 0.8431 0.015 Uiso 1 1 calc R . . C2 C 0.7548(3) 0.59880(14) 0.91977(16) 0.0142(5) Uani 1 1 d . . . H2A H 0.8257 0.5606 0.9269 0.017 Uiso 1 1 calc R . . H2B H 0.8216 0.6382 0.9211 0.017 Uiso 1 1 calc R . . C3 C 0.7344(3) 0.63679(14) 1.06494(18) 0.0183(6) Uani 1 1 d . . . H3A H 0.6657 0.6345 1.1108 0.022 Uiso 1 1 calc R . . H3B H 0.7447 0.6830 1.0498 0.022 Uiso 1 1 calc R . . C4 C 0.8978(3) 0.61058(15) 1.09754(19) 0.0218(6) Uani 1 1 d . . . H4A H 0.9690 0.6162 1.0533 0.026 Uiso 1 1 calc R . . H4B H 0.9412 0.6367 1.1468 0.026 Uiso 1 1 calc R . . C5 C 0.8979(4) 0.53937(16) 1.1230(2) 0.0303(8) Uani 1 1 d . . . H5A H 0.8152 0.5319 1.1598 0.036 Uiso 1 1 calc R . . H5B H 1.0012 0.5280 1.1529 0.036 Uiso 1 1 calc R . . H5C H 0.8773 0.5123 1.0725 0.036 Uiso 1 1 calc R . . C11 C 0.4287(3) 0.76306(13) 0.88888(17) 0.0133(5) Uani 1 1 d . . . C12 C 0.4131(3) 0.80827(13) 0.82362(17) 0.0156(6) Uani 1 1 d . . . H12 H 0.4457 0.7967 0.7708 0.019 Uiso 1 1 calc R . . C13 C 0.3511(3) 0.86967(13) 0.83385(18) 0.0172(6) Uani 1 1 d . . . H13 H 0.3426 0.8999 0.7888 0.021 Uiso 1 1 calc R . . C14 C 0.3020(3) 0.88629(13) 0.91038(19) 0.0159(6) Uani 1 1 d . . . C15 C 0.3191(3) 0.84365(14) 0.97706(18) 0.0159(6) Uani 1 1 d . . . H15 H 0.2886 0.8560 1.0300 0.019 Uiso 1 1 calc R . . C16 C 0.3812(3) 0.78269(14) 0.96612(17) 0.0146(6) Uani 1 1 d . . . H16 H 0.3920 0.7533 1.0121 0.018 Uiso 1 1 calc R . . C21 C 0.7214(3) 0.73075(13) 0.77822(17) 0.0141(5) Uani 1 1 d . . . C22 C 0.7268(4) 0.75625(14) 0.69785(18) 0.0196(6) Uani 1 1 d . . . H22 H 0.6545 0.7411 0.6524 0.023 Uiso 1 1 calc R . . C23 C 0.8368(4) 0.80360(15) 0.6838(2) 0.0263(7) Uani 1 1 d . . . H23 H 0.8375 0.8219 0.6293 0.032 Uiso 1 1 calc R . . C24 C 0.9457(4) 0.82408(15) 0.7496(2) 0.0265(7) Uani 1 1 d . . . H24 H 1.0232 0.8555 0.7397 0.032 Uiso 1 1 calc R . . C25 C 0.9423(4) 0.79917(15) 0.8291(2) 0.0248(7) Uani 1 1 d . . . H25 H 1.0179 0.8130 0.8738 0.030 Uiso 1 1 calc R . . C26 C 0.8276(3) 0.75355(14) 0.84404(19) 0.0192(6) Uani 1 1 d . . . H26 H 0.8222 0.7380 0.8995 0.023 Uiso 1 1 calc R . . C31 C 0.4392(3) 0.66249(13) 0.70597(17) 0.0146(6) Uani 1 1 d . . . C32 C 0.4936(3) 0.63793(14) 0.63298(18) 0.0172(6) Uani 1 1 d . . . H32 H 0.6003 0.6240 0.6343 0.021 Uiso 1 1 calc R . . C33 C 0.3923(4) 0.63386(14) 0.55859(18) 0.0208(6) Uani 1 1 d . . . H33 H 0.4293 0.6168 0.5093 0.025 Uiso 1 1 calc R . . C34 C 0.2370(4) 0.65486(15) 0.55660(19) 0.0217(6) Uani 1 1 d . . . H34 H 0.1682 0.6532 0.5055 0.026 Uiso 1 1 calc R . . C35 C 0.1818(3) 0.67837(15) 0.62928(19) 0.0216(6) Uani 1 1 d . . . H35 H 0.0750 0.6923 0.6276 0.026 Uiso 1 1 calc R . . C36 C 0.2811(3) 0.68174(14) 0.70432(18) 0.0168(6) Uani 1 1 d . . . H36 H 0.2421 0.6970 0.7540 0.020 Uiso 1 1 calc R . . C41 C 0.7364(3) 0.56114(13) 0.76725(17) 0.0142(5) Uani 1 1 d . . . C42 C 0.6655(3) 0.50716(14) 0.72659(18) 0.0183(6) Uani 1 1 d . . . H42 H 0.5675 0.4916 0.7417 0.022 Uiso 1 1 calc R . . C43 C 0.7370(4) 0.47581(15) 0.66412(19) 0.0237(7) Uani 1 1 d . . . H43 H 0.6874 0.4392 0.6362 0.028 Uiso 1 1 calc R . . C44 C 0.8796(4) 0.49768(15) 0.64258(19) 0.0225(6) Uani 1 1 d . . . H44 H 0.9278 0.4765 0.5993 0.027 Uiso 1 1 calc R . . C45 C 0.9529(3) 0.55028(15) 0.68363(19) 0.0204(6) Uani 1 1 d . . . H45 H 1.0525 0.5646 0.6693 0.024 Uiso 1 1 calc R . . C46 C 0.8818(3) 0.58260(14) 0.74605(18) 0.0163(6) Uani 1 1 d . . . H46 H 0.9324 0.6190 0.7739 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01177(11) 0.01162(11) 0.01233(11) 0.00150(8) 0.00358(7) -0.00091(8) N1 0.0148(11) 0.0133(11) 0.0125(11) 0.0013(9) 0.0055(9) 0.0011(9) N2 0.0153(12) 0.0115(12) 0.0119(12) 0.0029(9) 0.0021(9) -0.0006(9) P1 0.0111(3) 0.0122(3) 0.0110(3) 0.0016(3) 0.0020(2) -0.0003(3) Cl1 0.0116(3) 0.0262(4) 0.0262(4) 0.0026(3) 0.0028(3) -0.0019(3) Cl2 0.0256(4) 0.0129(3) 0.0186(3) 0.0019(3) 0.0107(3) -0.0021(3) Br1 0.02292(16) 0.01666(15) 0.02860(18) -0.00192(12) 0.00512(12) 0.00639(12) C1 0.0129(12) 0.0111(13) 0.0123(13) 0.0015(10) 0.0012(10) -0.0005(10) C2 0.0146(13) 0.0165(14) 0.0119(13) 0.0013(11) 0.0034(10) 0.0009(11) C3 0.0195(14) 0.0194(15) 0.0158(14) -0.0032(11) 0.0013(11) 0.0001(12) C4 0.0200(15) 0.0305(17) 0.0140(14) -0.0027(12) -0.0024(11) 0.0002(12) C5 0.0367(19) 0.0317(19) 0.0201(17) 0.0032(14) -0.0073(14) 0.0116(15) C11 0.0097(12) 0.0141(14) 0.0160(14) -0.0004(11) 0.0004(10) -0.0022(10) C12 0.0173(14) 0.0149(14) 0.0152(14) 0.0009(11) 0.0049(11) 0.0012(11) C13 0.0215(14) 0.0125(14) 0.0176(15) 0.0042(11) 0.0022(11) -0.0003(11) C14 0.0125(13) 0.0108(13) 0.0246(15) -0.0039(11) 0.0034(11) 0.0007(10) C15 0.0133(13) 0.0210(15) 0.0139(14) -0.0053(11) 0.0034(10) -0.0003(11) C16 0.0129(13) 0.0172(14) 0.0134(14) 0.0027(11) 0.0002(10) -0.0009(11) C21 0.0146(13) 0.0109(13) 0.0175(14) 0.0032(11) 0.0045(11) -0.0004(10) C22 0.0256(15) 0.0167(15) 0.0174(15) 0.0009(11) 0.0063(12) -0.0014(12) C23 0.0384(19) 0.0179(16) 0.0255(17) 0.0019(13) 0.0160(14) -0.0064(13) C24 0.0263(16) 0.0174(16) 0.038(2) -0.0015(14) 0.0150(14) -0.0082(13) C25 0.0207(15) 0.0208(16) 0.0320(18) -0.0023(13) -0.0003(13) -0.0040(12) C26 0.0184(14) 0.0175(15) 0.0214(15) 0.0022(12) 0.0008(11) -0.0016(11) C31 0.0154(13) 0.0150(14) 0.0130(13) 0.0026(11) 0.0002(10) -0.0009(11) C32 0.0142(13) 0.0193(15) 0.0181(15) 0.0029(11) 0.0011(11) 0.0011(11) C33 0.0285(16) 0.0203(16) 0.0134(14) -0.0018(11) 0.0012(12) -0.0010(12) C34 0.0220(15) 0.0249(16) 0.0167(15) 0.0035(12) -0.0050(12) -0.0015(12) C35 0.0153(14) 0.0242(16) 0.0244(16) 0.0039(13) -0.0015(12) 0.0004(12) C36 0.0179(14) 0.0163(14) 0.0157(14) 0.0021(11) 0.0005(11) -0.0016(11) C41 0.0155(13) 0.0155(14) 0.0113(13) 0.0032(11) 0.0004(10) 0.0051(11) C42 0.0171(14) 0.0204(15) 0.0177(15) -0.0017(12) 0.0023(11) -0.0004(11) C43 0.0276(16) 0.0226(16) 0.0202(16) -0.0064(13) -0.0005(12) 0.0000(13) C44 0.0249(16) 0.0246(16) 0.0186(15) -0.0023(12) 0.0053(12) 0.0088(13) C45 0.0166(14) 0.0231(16) 0.0226(16) 0.0045(12) 0.0073(12) 0.0052(12) C46 0.0170(13) 0.0141(14) 0.0180(14) 0.0028(11) 0.0024(11) 0.0015(11) _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 N1 2.057(2) . ? Pd1 N2 2.067(2) . ? Pd1 Cl1 2.2999(7) . ? Pd1 Cl2 2.3035(7) . ? N1 C11 1.413(3) . ? N1 P1 1.618(2) . ? N2 C2 1.486(3) . ? N2 C3 1.494(3) . ? P1 C31 1.805(3) . ? P1 C21 1.811(3) . ? P1 C1 1.830(3) . ? Br1 C14 1.905(3) . ? C1 C41 1.518(4) . ? C1 C2 1.540(4) . ? C3 C4 1.527(4) . ? C4 C5 1.523(4) . ? C11 C12 1.395(4) . ? C11 C16 1.404(4) . ? C12 C13 1.388(4) . ? C13 C14 1.382(4) . ? C14 C15 1.378(4) . ? C15 C16 1.382(4) . ? C21 C26 1.389(4) . ? C21 C22 1.395(4) . ? C22 C23 1.389(4) . ? C23 C24 1.387(5) . ? C24 C25 1.376(5) . ? C25 C26 1.395(4) . ? C31 C32 1.400(4) . ? C31 C36 1.400(4) . ? C32 C33 1.391(4) . ? C33 C34 1.388(4) . ? C34 C35 1.391(4) . ? C35 C36 1.389(4) . ? C41 C42 1.391(4) . ? C41 C46 1.392(4) . ? C42 C43 1.388(4) . ? C43 C44 1.374(4) . ? C44 C45 1.379(4) . ? C45 C46 1.395(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 N2 90.88(9) . . ? N1 Pd1 Cl1 90.37(6) . . ? N2 Pd1 Cl1 176.68(7) . . ? N1 Pd1 Cl2 175.06(7) . . ? N2 Pd1 Cl2 86.48(7) . . ? Cl1 Pd1 Cl2 92.49(3) . . ? C11 N1 P1 123.95(19) . . ? C11 N1 Pd1 119.11(17) . . ? P1 N1 Pd1 115.71(12) . . ? C2 N2 C3 112.4(2) . . ? C2 N2 Pd1 117.00(16) . . ? C3 N2 Pd1 112.20(17) . . ? N1 P1 C31 115.10(12) . . ? N1 P1 C21 109.95(12) . . ? C31 P1 C21 106.97(13) . . ? N1 P1 C1 104.78(12) . . ? C31 P1 C1 107.70(12) . . ? C21 P1 C1 112.44(12) . . ? C41 C1 C2 113.0(2) . . ? C41 C1 P1 113.52(18) . . ? C2 C1 P1 111.05(18) . . ? N2 C2 C1 111.4(2) . . ? N2 C3 C4 114.1(2) . . ? C5 C4 C3 113.9(3) . . ? C12 C11 C16 117.0(2) . . ? C12 C11 N1 124.2(2) . . ? C16 C11 N1 118.8(2) . . ? C13 C12 C11 121.7(3) . . ? C14 C13 C12 119.2(3) . . ? C15 C14 C13 120.8(3) . . ? C15 C14 Br1 120.2(2) . . ? C13 C14 Br1 119.0(2) . . ? C14 C15 C16 119.4(3) . . ? C15 C16 C11 121.8(3) . . ? C26 C21 C22 119.0(3) . . ? C26 C21 P1 118.5(2) . . ? C22 C21 P1 122.3(2) . . ? C23 C22 C21 120.5(3) . . ? C24 C23 C22 119.7(3) . . ? C25 C24 C23 120.4(3) . . ? C24 C25 C26 119.9(3) . . ? C21 C26 C25 120.3(3) . . ? C32 C31 C36 119.7(3) . . ? C32 C31 P1 121.6(2) . . ? C36 C31 P1 118.6(2) . . ? C33 C32 C31 120.3(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C35 120.1(3) . . ? C36 C35 C34 120.7(3) . . ? C35 C36 C31 119.4(3) . . ? C42 C41 C46 119.3(3) . . ? C42 C41 C1 118.6(2) . . ? C46 C41 C1 122.1(2) . . ? C43 C42 C41 120.5(3) . . ? C44 C43 C42 120.0(3) . . ? C43 C44 C45 120.2(3) . . ? C44 C45 C46 120.5(3) . . ? C41 C46 C45 119.5(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H02 Cl2 0.82(3) 2.62(3) 3.290(3) 140(3) 3_667 _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.840 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.109 data_rrm127xs_compound_u-9a _database_code_depnum_ccdc_archive 'CCDC 881655' #TrackingRef 'daltontrans-completo.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H36 Cl2 N3 P Pd' _chemical_formula_weight 622.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.6505(13) _cell_length_b 7.6545(5) _cell_length_c 20.4198(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.675(2) _cell_angle_gamma 90.00 _cell_volume 2909.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8979 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.57 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8551 _exptl_absorpt_correction_T_max 0.8999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33932 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 28.57 _reflns_number_total 6990 _reflns_number_gt 6792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0176P)^2^+5.8891P] 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 'NH free, Me rigid, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6990 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0846 _refine_ls_goodness_of_fit_ref 1.301 _refine_ls_restrained_S_all 1.301 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.329799(11) 0.55838(3) 1.007944(10) 0.01296(6) Uani 1 1 d . . . N1 N 0.23588(12) 0.4236(3) 0.99104(11) 0.0150(5) Uani 1 1 d . . . N2 N 0.38758(13) 0.3425(3) 0.98241(11) 0.0147(5) Uani 1 1 d . . . H02 H 0.4290(19) 0.381(4) 0.9845(16) 0.016(8) Uiso 1 1 d . . . P1 P 0.22288(4) 0.34242(9) 0.91904(3) 0.01329(14) Uani 1 1 d . . . Cl1 Cl 0.26613(4) 0.80085(9) 1.03859(4) 0.02027(14) Uani 1 1 d . . . Cl2 Cl 0.43721(4) 0.70457(9) 1.02735(4) 0.02247(15) Uani 1 1 d . . . C1 C 0.29781(15) 0.2029(4) 0.90274(14) 0.0167(5) Uani 1 1 d . . . H1A H 0.2953 0.0978 0.9307 0.020 Uiso 1 1 calc R . . H1B H 0.2915 0.1636 0.8565 0.020 Uiso 1 1 calc R . . C2 C 0.37346(15) 0.2809(4) 0.91365(14) 0.0182(6) Uani 1 1 d . . . H2 H 0.4082 0.1842 0.9068 0.022 Uiso 1 1 calc R . . C3 C 0.39078(18) 0.4273(5) 0.86663(16) 0.0281(7) Uani 1 1 d . . . H3A H 0.3601 0.5283 0.8740 0.034 Uiso 1 1 calc R . . H3B H 0.3821 0.3867 0.8213 0.034 Uiso 1 1 calc R . . H3C H 0.4413 0.4609 0.8743 0.034 Uiso 1 1 calc R . . C4 C 0.38638(15) 0.1980(4) 1.03134(14) 0.0174(6) Uani 1 1 d . . . H4A H 0.4097 0.0933 1.0138 0.021 Uiso 1 1 calc R . . H4B H 0.3359 0.1675 1.0388 0.021 Uiso 1 1 calc R . . C5 C 0.42513(16) 0.2503(4) 1.09611(14) 0.0187(6) Uani 1 1 d . . . H5A H 0.4016 0.3547 1.1137 0.022 Uiso 1 1 calc R . . H5B H 0.4755 0.2815 1.0886 0.022 Uiso 1 1 calc R . . C6 C 0.42444(19) 0.1032(4) 1.14606(15) 0.0265(7) Uani 1 1 d . . . H6A H 0.4367 -0.0081 1.1247 0.032 Uiso 1 1 calc R . . H6B H 0.3755 0.0916 1.1617 0.032 Uiso 1 1 calc R . . C7 C 0.4777(2) 0.1364(5) 1.20451(17) 0.0350(8) Uani 1 1 d . . . H7A H 0.5262 0.1483 1.1892 0.042 Uiso 1 1 calc R . . H7B H 0.4766 0.0381 1.2352 0.042 Uiso 1 1 calc R . . H7C H 0.4645 0.2441 1.2268 0.042 Uiso 1 1 calc R . . C11 C 0.18391(15) 0.4260(4) 1.03883(13) 0.0146(5) Uani 1 1 d . . . C12 C 0.11463(15) 0.4896(4) 1.02571(13) 0.0164(5) Uani 1 1 d . . . H12 H 0.1014 0.5381 0.9838 0.020 Uiso 1 1 calc R . . C13 C 0.06441(15) 0.4832(4) 1.07316(14) 0.0177(6) Uani 1 1 d . . . H13 H 0.0172 0.5257 1.0629 0.021 Uiso 1 1 calc R . . C14 C 0.08216(16) 0.4155(4) 1.13548(14) 0.0182(6) Uani 1 1 d . . . C15 C 0.15245(16) 0.3582(4) 1.14842(14) 0.0209(6) Uani 1 1 d . . . H15 H 0.1665 0.3145 1.1909 0.025 Uiso 1 1 calc R . . C16 C 0.20237(16) 0.3631(4) 1.10147(14) 0.0194(6) Uani 1 1 d . . . H16 H 0.2499 0.3231 1.1121 0.023 Uiso 1 1 calc R . . C17 C 0.02806(18) 0.4052(5) 1.18715(15) 0.0272(7) Uani 1 1 d . . . H17A H 0.0374 0.3008 1.2141 0.033 Uiso 1 1 calc R . . H17B H -0.0205 0.3986 1.1659 0.033 Uiso 1 1 calc R . . H17C H 0.0321 0.5095 1.2150 0.033 Uiso 1 1 calc R . . C21 C 0.14450(15) 0.2043(4) 0.91392(13) 0.0153(5) Uani 1 1 d . . . C22 C 0.14077(16) 0.0700(4) 0.96012(14) 0.0197(6) Uani 1 1 d . . . H22 H 0.1792 0.0529 0.9923 0.024 Uiso 1 1 calc R . . C23 C 0.08126(17) -0.0375(4) 0.95890(15) 0.0237(6) Uani 1 1 d . . . H23 H 0.0790 -0.1288 0.9902 0.028 Uiso 1 1 calc R . . C24 C 0.02468(17) -0.0130(4) 0.91210(16) 0.0260(7) Uani 1 1 d . . . H24 H -0.0161 -0.0875 0.9114 0.031 Uiso 1 1 calc R . . C25 C 0.02788(16) 0.1196(4) 0.86672(15) 0.0242(6) Uani 1 1 d . . . H25 H -0.0110 0.1370 0.8350 0.029 Uiso 1 1 calc R . . C26 C 0.08766(15) 0.2280(4) 0.86721(14) 0.0185(6) Uani 1 1 d . . . H26 H 0.0898 0.3185 0.8356 0.022 Uiso 1 1 calc R . . C31 C 0.21050(14) 0.4997(4) 0.85376(13) 0.0145(5) Uani 1 1 d . . . C32 C 0.21609(16) 0.4501(4) 0.78844(14) 0.0204(6) Uani 1 1 d . . . H32 H 0.2301 0.3343 0.7784 0.024 Uiso 1 1 calc R . . C33 C 0.20134(18) 0.5686(4) 0.73829(15) 0.0249(7) Uani 1 1 d . . . H33 H 0.2048 0.5341 0.6939 0.030 Uiso 1 1 calc R . . C34 C 0.18134(17) 0.7387(4) 0.75306(15) 0.0245(7) Uani 1 1 d . . . H34 H 0.1709 0.8202 0.7187 0.029 Uiso 1 1 calc R . . C35 C 0.17671(17) 0.7891(4) 0.81746(15) 0.0227(6) Uani 1 1 d . . . H35 H 0.1633 0.9055 0.8272 0.027 Uiso 1 1 calc R . . C36 C 0.19152(15) 0.6705(4) 0.86839(14) 0.0184(6) Uani 1 1 d . . . H36 H 0.1887 0.7061 0.9127 0.022 Uiso 1 1 calc R . . N9 N 0.31905(17) 0.4090(4) 0.24396(14) 0.0329(7) Uani 1 1 d . . . C91 C 0.33772(17) 0.5360(4) 0.22255(15) 0.0239(6) Uani 1 1 d . . . C92 C 0.36170(19) 0.7000(5) 0.19438(17) 0.0309(7) Uani 1 1 d . . . H92A H 0.4099 0.6844 0.1788 0.037 Uiso 1 1 calc R . . H92B H 0.3629 0.7916 0.2279 0.037 Uiso 1 1 calc R . . H92C H 0.3283 0.7338 0.1575 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.01150(10) 0.01132(10) 0.01598(11) -0.00082(7) 0.00015(7) 0.00092(7) N1 0.0116(10) 0.0173(12) 0.0161(11) -0.0019(9) 0.0010(8) -0.0003(9) N2 0.0111(11) 0.0151(11) 0.0179(12) -0.0004(9) 0.0023(9) 0.0002(9) P1 0.0138(3) 0.0113(3) 0.0145(3) -0.0013(3) -0.0007(2) 0.0014(3) Cl1 0.0171(3) 0.0144(3) 0.0289(4) -0.0041(3) -0.0021(3) 0.0034(3) Cl2 0.0147(3) 0.0158(3) 0.0373(4) -0.0051(3) 0.0046(3) -0.0027(3) C1 0.0174(13) 0.0156(13) 0.0168(13) -0.0053(10) -0.0006(10) 0.0036(11) C2 0.0163(13) 0.0189(14) 0.0196(14) -0.0035(11) 0.0017(11) 0.0027(11) C3 0.0248(16) 0.0344(18) 0.0254(16) -0.0006(14) 0.0039(13) -0.0043(14) C4 0.0181(13) 0.0126(13) 0.0210(14) 0.0006(11) -0.0023(11) 0.0023(10) C5 0.0194(14) 0.0150(13) 0.0212(14) -0.0001(11) -0.0015(11) -0.0035(11) C6 0.0350(18) 0.0208(15) 0.0232(15) 0.0023(12) -0.0015(13) -0.0005(13) C7 0.042(2) 0.038(2) 0.0238(17) 0.0058(15) -0.0054(15) 0.0014(16) C11 0.0161(13) 0.0135(12) 0.0143(12) -0.0049(10) 0.0006(10) -0.0008(10) C12 0.0161(13) 0.0184(13) 0.0143(13) 0.0020(10) -0.0026(10) 0.0022(11) C13 0.0132(13) 0.0209(14) 0.0185(13) -0.0006(11) -0.0022(10) 0.0024(11) C14 0.0217(14) 0.0150(13) 0.0180(13) -0.0031(11) 0.0023(11) -0.0037(11) C15 0.0265(15) 0.0195(14) 0.0161(13) 0.0016(11) -0.0034(11) 0.0040(12) C16 0.0177(14) 0.0218(15) 0.0181(14) -0.0002(11) -0.0044(11) 0.0059(11) C17 0.0297(17) 0.0328(18) 0.0198(15) 0.0014(13) 0.0076(13) -0.0003(14) C21 0.0165(13) 0.0128(13) 0.0168(13) -0.0050(10) 0.0030(10) 0.0006(10) C22 0.0229(14) 0.0161(14) 0.0203(14) -0.0004(11) 0.0040(11) 0.0036(11) C23 0.0317(17) 0.0143(14) 0.0263(16) -0.0027(12) 0.0126(13) -0.0011(12) C24 0.0239(15) 0.0235(16) 0.0321(17) -0.0126(13) 0.0121(13) -0.0113(13) C25 0.0180(14) 0.0324(17) 0.0221(15) -0.0081(13) 0.0003(12) -0.0041(13) C26 0.0196(14) 0.0182(14) 0.0177(14) -0.0020(11) 0.0009(11) 0.0000(11) C31 0.0111(12) 0.0161(13) 0.0161(13) 0.0015(10) -0.0012(10) -0.0004(10) C32 0.0268(15) 0.0154(14) 0.0186(14) -0.0039(11) -0.0008(11) 0.0007(12) C33 0.0341(17) 0.0233(16) 0.0172(14) -0.0001(12) 0.0002(12) -0.0003(13) C34 0.0287(16) 0.0214(15) 0.0232(15) 0.0072(12) -0.0010(12) 0.0004(13) C35 0.0256(15) 0.0127(13) 0.0299(16) 0.0021(12) 0.0025(12) 0.0027(12) C36 0.0174(13) 0.0190(14) 0.0189(14) -0.0023(11) 0.0034(11) 0.0006(11) N9 0.0412(17) 0.0324(16) 0.0251(14) 0.0041(12) 0.0028(12) -0.0068(13) C91 0.0245(15) 0.0301(17) 0.0170(14) -0.0001(12) 0.0001(11) -0.0009(13) C92 0.0339(18) 0.0298(18) 0.0288(17) 0.0068(14) 0.0012(14) -0.0038(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1 2.043(2) . ? Pd1 N2 2.058(2) . ? Pd1 Cl2 2.3066(7) . ? Pd1 Cl1 2.3111(7) . ? N1 C11 1.419(3) . ? N1 P1 1.600(2) . ? N2 C2 1.488(4) . ? N2 C4 1.492(4) . ? P1 C31 1.800(3) . ? P1 C21 1.802(3) . ? P1 C1 1.807(3) . ? C1 C2 1.535(4) . ? C2 C3 1.523(4) . ? C4 C5 1.520(4) . ? C5 C6 1.520(4) . ? C6 C7 1.524(5) . ? C11 C16 1.389(4) . ? C11 C12 1.391(4) . ? C12 C13 1.391(4) . ? C13 C14 1.394(4) . ? C14 C15 1.392(4) . ? C14 C17 1.508(4) . ? C15 C16 1.379(4) . ? C21 C26 1.392(4) . ? C21 C22 1.400(4) . ? C22 C23 1.381(4) . ? C23 C24 1.390(5) . ? C24 C25 1.379(5) . ? C25 C26 1.389(4) . ? C31 C36 1.392(4) . ? C31 C32 1.397(4) . ? C32 C33 1.383(4) . ? C33 C34 1.393(4) . ? C34 C35 1.378(4) . ? C35 C36 1.394(4) . ? N9 C91 1.130(4) . ? C91 C92 1.463(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 N1 Pd1 N2 90.52(9) . . ? N1 Pd1 Cl2 178.70(7) . . ? N2 Pd1 Cl2 88.28(7) . . ? N1 Pd1 Cl1 90.08(7) . . ? N2 Pd1 Cl1 178.88(7) . . ? Cl2 Pd1 Cl1 91.12(3) . . ? C11 N1 P1 124.52(19) . . ? C11 N1 Pd1 119.58(17) . . ? P1 N1 Pd1 115.41(13) . . ? C2 N2 C4 112.8(2) . . ? C2 N2 Pd1 115.41(17) . . ? C4 N2 Pd1 113.27(17) . . ? N1 P1 C31 115.17(13) . . ? N1 P1 C21 110.85(13) . . ? C31 P1 C21 106.52(13) . . ? N1 P1 C1 109.00(13) . . ? C31 P1 C1 108.83(13) . . ? C21 P1 C1 106.06(13) . . ? C2 C1 P1 117.3(2) . . ? N2 C2 C3 109.3(2) . . ? N2 C2 C1 111.4(2) . . ? C3 C2 C1 115.1(2) . . ? N2 C4 C5 111.1(2) . . ? C4 C5 C6 111.4(2) . . ? C5 C6 C7 111.6(3) . . ? C16 C11 C12 118.1(3) . . ? C16 C11 N1 119.3(2) . . ? C12 C11 N1 122.6(2) . . ? C11 C12 C13 120.8(3) . . ? C12 C13 C14 121.2(3) . . ? C15 C14 C13 117.1(3) . . ? C15 C14 C17 121.0(3) . . ? C13 C14 C17 121.9(3) . . ? C16 C15 C14 122.0(3) . . ? C15 C16 C11 120.7(3) . . ? C26 C21 C22 119.3(3) . . ? C26 C21 P1 122.9(2) . . ? C22 C21 P1 117.8(2) . . ? C23 C22 C21 120.0(3) . . ? C22 C23 C24 120.4(3) . . ? C25 C24 C23 119.9(3) . . ? C24 C25 C26 120.3(3) . . ? C25 C26 C21 120.2(3) . . ? C36 C31 C32 119.7(3) . . ? C36 C31 P1 119.4(2) . . ? C32 C31 P1 120.8(2) . . ? C33 C32 C31 120.4(3) . . ? C32 C33 C34 119.8(3) . . ? C35 C34 C33 120.1(3) . . ? C34 C35 C36 120.5(3) . . ? C31 C36 C35 119.5(3) . . ? N9 C91 C92 179.6(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H02 Cl2 0.82(3) 2.61(3) 3.306(2) 144(3) 3_667 C22 H22 Cl1 0.95 2.65 3.435(3) 139.7 1_545 C92 H92C Cl1 0.98 2.67 3.628(3) 164.9 1_554 C1 H1B N9 0.99 2.45 3.401(4) 160.6 4_566 N2 H02 Cl2 0.82(3) 2.63(3) 3.045(2) 113(3) . _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.723 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.089 data_plame_compound_u,l-12 _database_code_depnum_ccdc_archive 'CCDC 881656' #TrackingRef 'daltontrans-completo.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H35 Cl8 N2 P Pd' _chemical_formula_weight 868.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(1)/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0275(6) _cell_length_b 14.4426(16) _cell_length_c 25.536(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.837(6) _cell_angle_gamma 90.00 _cell_volume 3693.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 99 _cell_measurement_theta_min 5.48 _cell_measurement_theta_max 12.44 _exptl_crystal_description lath _exptl_crystal_colour red _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.562 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1752 _exptl_absorpt_coefficient_mu 1.150 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.70268 _exptl_absorpt_correction_T_max 0.83033 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens P4' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 247 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 6676 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6467 _reflns_number_gt 4809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^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 'NH free, others riding' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6467 _refine_ls_number_parameters 403 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.934 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd -0.43688(3) -0.605169(19) 0.783912(11) 0.01730(9) Uani 1 1 d . . . P1 P -0.27180(9) -0.75828(6) 0.83998(4) 0.0184(2) Uani 1 1 d . . . N1 N -0.3144(3) -0.6512(2) 0.84449(12) 0.0185(7) Uani 1 1 d . . . N2 N -0.5783(3) -0.7021(2) 0.80272(13) 0.0215(7) Uani 1 1 d . . . H02 H -0.634(4) -0.692(2) 0.7789(15) 0.012(10) Uiso 1 1 d . . . Cl1 Cl -0.28149(9) -0.49658(6) 0.76160(4) 0.0237(2) Uani 1 1 d . . . Cl2 Cl -0.57984(10) -0.56358(6) 0.71299(4) 0.0258(2) Uani 1 1 d . . . C1 C -0.4205(4) -0.8290(2) 0.83145(14) 0.0205(8) Uani 1 1 d . . . H1A H -0.3920 -0.8920 0.8215 0.025 Uiso 1 1 calc R . . H1B H -0.4603 -0.8343 0.8660 0.025 Uiso 1 1 calc R . . C2 C -0.5321(4) -0.7986(3) 0.79145(15) 0.0223(8) Uani 1 1 d . . . H2 H -0.6098 -0.8408 0.7959 0.027 Uiso 1 1 calc R . . C3 C -0.6414(4) -0.6940(3) 0.85453(16) 0.0255(9) Uani 1 1 d . . . H3 H -0.5828 -0.7283 0.8807 0.031 Uiso 1 1 calc R . . C4 C -0.7783(5) -0.7412(3) 0.8530(2) 0.0558(15) Uani 1 1 d . . . H4A H -0.7697 -0.8049 0.8403 0.067 Uiso 1 1 calc R . . H4B H -0.8405 -0.7070 0.8293 0.067 Uiso 1 1 calc R . . H4C H -0.8123 -0.7420 0.8883 0.067 Uiso 1 1 calc R . . C5 C -0.4937(4) -0.8073(3) 0.73503(15) 0.0279(9) Uani 1 1 d . . . H5A H -0.5684 -0.7869 0.7116 0.033 Uiso 1 1 calc R . . H5B H -0.4725 -0.8720 0.7275 0.033 Uiso 1 1 calc R . . H5C H -0.4154 -0.7686 0.7295 0.033 Uiso 1 1 calc R . . C11 C -0.1955(4) -0.7964(2) 0.90171(14) 0.0211(8) Uani 1 1 d D . . C12 C -0.2662(4) -0.7830(3) 0.94658(15) 0.0289(9) Uani 1 1 d D . . H12 H -0.3514 -0.7543 0.9438 0.035 Uiso 1 1 calc R . . C13 C -0.2142(5) -0.8108(3) 0.99496(16) 0.0386(11) Uani 1 1 d D . . H13 H -0.2639 -0.8019 1.0253 0.046 Uiso 1 1 calc R . . C14 C -0.0894(4) -0.8519(3) 0.99930(17) 0.0366(11) Uani 1 1 d D . . H14 H -0.0533 -0.8712 1.0326 0.044 Uiso 1 1 calc R . . C15 C -0.0172(4) -0.8647(3) 0.95508(17) 0.0330(10) Uani 1 1 d D . . H15 H 0.0690 -0.8921 0.9582 0.040 Uiso 1 1 calc R . . C16 C -0.0705(4) -0.8377(3) 0.90611(15) 0.0254(9) Uani 1 1 d D . . H16 H -0.0214 -0.8474 0.8757 0.031 Uiso 1 1 calc R . . C21 C -0.1603(4) -0.7885(3) 0.78941(14) 0.0213(8) Uani 1 1 d D . . C22 C -0.1015(4) -0.7195(3) 0.76073(15) 0.0302(10) Uani 1 1 d D . . H22 H -0.1230 -0.6564 0.7666 0.036 Uiso 1 1 calc R . . C23 C -0.0112(5) -0.7427(3) 0.72344(18) 0.0428(12) Uani 1 1 d D . . H23 H 0.0296 -0.6953 0.7040 0.051 Uiso 1 1 calc R . . C24 C 0.0194(5) -0.8344(3) 0.71451(17) 0.0407(12) Uani 1 1 d D . . H24 H 0.0823 -0.8499 0.6893 0.049 Uiso 1 1 calc R . . C25 C -0.0406(4) -0.9032(3) 0.74196(17) 0.0353(10) Uani 1 1 d D . . H25 H -0.0202 -0.9662 0.7352 0.042 Uiso 1 1 calc R . . C26 C -0.1309(4) -0.8812(3) 0.77945(16) 0.0267(9) Uani 1 1 d D . . H26 H -0.1726 -0.9290 0.7983 0.032 Uiso 1 1 calc R . . C31 C -0.2347(3) -0.5844(2) 0.87345(14) 0.0177(8) Uani 1 1 d D . . C32 C -0.0967(4) -0.5888(3) 0.87966(15) 0.0248(9) Uani 1 1 d D . . H32 H -0.0501 -0.6380 0.8639 0.030 Uiso 1 1 calc R . . C33 C -0.0262(4) -0.5221(3) 0.90860(16) 0.0297(10) Uani 1 1 d D . . H33 H 0.0682 -0.5272 0.9129 0.036 Uiso 1 1 calc R . . C34 C -0.0897(4) -0.4485(3) 0.93127(16) 0.0298(10) Uani 1 1 d D . . C35 C -0.2281(4) -0.4446(3) 0.92483(16) 0.0279(9) Uani 1 1 d D . . H35 H -0.2745 -0.3952 0.9405 0.033 Uiso 1 1 calc R . . C36 C -0.3002(4) -0.5108(3) 0.89621(15) 0.0243(9) Uani 1 1 d D . . H36 H -0.3946 -0.5060 0.8921 0.029 Uiso 1 1 calc R . . C37 C -0.0115(5) -0.3745(3) 0.9621(2) 0.0453(13) Uani 1 1 d . . . H37A H -0.0735 -0.3288 0.9754 0.054 Uiso 1 1 calc R . . H37B H 0.0503 -0.3438 0.9392 0.054 Uiso 1 1 calc R . . H37C H 0.0391 -0.4034 0.9916 0.054 Uiso 1 1 calc R . . C41 C -0.6521(3) -0.5963(3) 0.87418(14) 0.0226(8) Uani 1 1 d D . . C42 C -0.6309(4) -0.5791(3) 0.92787(16) 0.0304(10) Uani 1 1 d D . . H42 H -0.6077 -0.6290 0.9508 0.036 Uiso 1 1 calc R . . C43 C -0.6428(4) -0.4915(3) 0.94822(17) 0.0354(10) Uani 1 1 d D . . H43 H -0.6279 -0.4814 0.9848 0.043 Uiso 1 1 calc R . . C44 C -0.6764(5) -0.4183(3) 0.91554(17) 0.0393(11) Uani 1 1 d D . . H44 H -0.6833 -0.3576 0.9295 0.047 Uiso 1 1 calc R . . C45 C -0.7002(5) -0.4334(3) 0.86245(17) 0.0351(10) Uani 1 1 d D . . H45 H -0.7229 -0.3829 0.8399 0.042 Uiso 1 1 calc R . . C46 C -0.6907(4) -0.5223(3) 0.84203(15) 0.0259(9) Uani 1 1 d D . . H46 H -0.7109 -0.5326 0.8058 0.031 Uiso 1 1 calc R . . C99 C -0.2767(4) -0.9437(3) 1.13673(17) 0.0371(11) Uani 1 1 d D . . H99 H -0.3107 -0.9680 1.1702 0.044 Uiso 1 1 calc R . . Cl3 Cl -0.35829(14) -1.00294(9) 1.08395(5) 0.0533(3) Uani 1 1 d D . . Cl4 Cl -0.10381(13) -0.96348(10) 1.13697(5) 0.0533(3) Uani 1 1 d D . . Cl5 Cl -0.31056(12) -0.82444(8) 1.13288(4) 0.0406(3) Uani 1 1 d D . . C98 C -0.3317(5) -1.1383(3) 0.91468(18) 0.0374(11) Uani 1 1 d . . . H98 H -0.4084 -1.1266 0.8890 0.045 Uiso 1 1 calc R . . Cl6 Cl -0.2599(2) -1.03312(11) 0.93249(8) 0.0961(7) Uani 1 1 d . . . Cl7 Cl -0.21535(16) -1.20849(12) 0.88467(6) 0.0706(5) Uani 1 1 d . . . Cl8 Cl -0.39175(16) -1.19488(11) 0.96939(6) 0.0681(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.02004(15) 0.01344(14) 0.01842(15) 0.00098(12) 0.00090(10) -0.00109(12) P1 0.0210(5) 0.0155(5) 0.0188(5) 0.0002(4) 0.0026(4) 0.0013(4) N1 0.0200(16) 0.0160(16) 0.0198(16) 0.0004(13) 0.0034(13) -0.0003(13) N2 0.0215(17) 0.0193(17) 0.0231(18) 0.0039(14) -0.0056(15) -0.0012(14) Cl1 0.0255(5) 0.0188(5) 0.0269(5) 0.0038(4) 0.0035(4) -0.0030(4) Cl2 0.0337(5) 0.0217(5) 0.0214(5) 0.0023(4) -0.0039(4) 0.0009(4) C1 0.027(2) 0.0134(18) 0.0216(19) -0.0003(16) 0.0030(16) -0.0019(15) C2 0.025(2) 0.0174(19) 0.024(2) -0.0048(16) -0.0030(16) -0.0031(16) C3 0.023(2) 0.025(2) 0.028(2) 0.0073(17) 0.0073(17) 0.0020(17) C4 0.040(3) 0.033(3) 0.097(4) -0.016(3) 0.037(3) -0.015(2) C5 0.036(2) 0.028(2) 0.020(2) -0.0024(17) 0.0028(18) -0.0059(18) C11 0.026(2) 0.0145(18) 0.023(2) 0.0022(16) -0.0007(16) -0.0012(16) C12 0.037(2) 0.027(2) 0.023(2) -0.0017(18) 0.0046(18) 0.0046(18) C13 0.058(3) 0.039(3) 0.019(2) -0.0025(19) 0.003(2) -0.005(2) C14 0.049(3) 0.033(2) 0.026(2) 0.006(2) -0.015(2) -0.008(2) C15 0.034(2) 0.025(2) 0.039(3) 0.0020(19) -0.009(2) 0.0003(18) C16 0.029(2) 0.022(2) 0.026(2) 0.0024(17) -0.0023(17) -0.0022(17) C21 0.0204(19) 0.027(2) 0.0168(19) 0.0005(16) 0.0008(15) 0.0066(16) C22 0.033(2) 0.029(2) 0.029(2) 0.0058(19) 0.0069(19) 0.0118(18) C23 0.043(3) 0.046(3) 0.041(3) 0.017(2) 0.021(2) 0.017(2) C24 0.043(3) 0.055(3) 0.025(2) 0.006(2) 0.014(2) 0.019(2) C25 0.034(2) 0.035(2) 0.037(2) -0.010(2) -0.0030(19) 0.015(2) C26 0.028(2) 0.024(2) 0.028(2) -0.0023(17) -0.0008(17) 0.0055(17) C31 0.0207(19) 0.0148(19) 0.0180(18) 0.0018(15) 0.0034(15) -0.0014(14) C32 0.024(2) 0.019(2) 0.030(2) 0.0003(17) -0.0004(17) 0.0024(16) C33 0.023(2) 0.026(2) 0.039(2) 0.0021(19) -0.0062(19) -0.0021(17) C34 0.035(2) 0.027(2) 0.027(2) 0.0007(18) -0.0079(19) -0.0073(19) C35 0.033(2) 0.023(2) 0.028(2) -0.0079(18) 0.0061(18) -0.0045(18) C36 0.021(2) 0.024(2) 0.028(2) -0.0027(17) 0.0031(17) -0.0023(16) C37 0.046(3) 0.034(3) 0.054(3) -0.006(2) -0.020(2) -0.009(2) C41 0.0134(17) 0.028(2) 0.027(2) 0.0028(18) 0.0035(15) -0.0002(16) C42 0.025(2) 0.041(3) 0.025(2) 0.0048(19) 0.0001(17) 0.0005(18) C43 0.037(2) 0.045(3) 0.025(2) -0.010(2) 0.0038(19) -0.006(2) C44 0.043(3) 0.034(3) 0.041(3) -0.013(2) 0.011(2) -0.006(2) C45 0.049(3) 0.025(2) 0.031(2) 0.0027(19) 0.011(2) -0.001(2) C46 0.028(2) 0.030(2) 0.019(2) 0.0005(17) 0.0019(17) -0.0004(17) C99 0.050(3) 0.032(2) 0.031(2) 0.006(2) 0.010(2) 0.009(2) Cl3 0.0695(9) 0.0415(7) 0.0485(8) -0.0084(6) 0.0005(7) -0.0042(6) Cl4 0.0534(8) 0.0588(8) 0.0482(7) -0.0022(6) 0.0059(6) 0.0189(6) Cl5 0.0584(7) 0.0319(6) 0.0321(6) -0.0002(5) 0.0083(5) 0.0081(5) C98 0.038(3) 0.031(2) 0.042(3) 0.004(2) -0.006(2) -0.005(2) Cl6 0.1182(15) 0.0426(8) 0.1216(16) 0.0026(9) -0.0536(13) -0.0299(9) Cl7 0.0723(10) 0.0797(11) 0.0615(9) 0.0201(8) 0.0209(8) 0.0335(9) Cl8 0.0803(10) 0.0711(10) 0.0547(9) 0.0237(7) 0.0213(8) 0.0085(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 Pd N1 2.039(3) . ? Pd N2 2.066(3) . ? Pd Cl1 2.3021(10) . ? Pd Cl2 2.3321(10) . ? P1 N1 1.610(3) . ? P1 C21 1.803(4) . ? P1 C11 1.804(4) . ? P1 C1 1.812(4) . ? N1 C31 1.434(5) . ? N2 C3 1.499(5) . ? N2 C2 1.501(5) . ? C1 C2 1.541(5) . ? C2 C5 1.515(5) . ? C3 C41 1.503(5) . ? C3 C4 1.532(6) . ? C11 C16 1.387(5) . ? C11 C12 1.390(5) . ? C12 C13 1.377(6) . ? C13 C14 1.384(6) . ? C14 C15 1.384(6) . ? C15 C16 1.392(5) . ? C21 C22 1.385(5) . ? C21 C26 1.397(5) . ? C22 C23 1.387(6) . ? C23 C24 1.381(6) . ? C24 C25 1.372(6) . ? C25 C26 1.387(6) . ? C31 C32 1.386(5) . ? C31 C36 1.392(5) . ? C32 C33 1.386(5) . ? C33 C34 1.381(6) . ? C34 C35 1.391(5) . ? C34 C37 1.522(6) . ? C35 C36 1.385(5) . ? C41 C46 1.391(5) . ? C41 C42 1.399(5) . ? C42 C43 1.375(6) . ? C43 C44 1.378(6) . ? C44 C45 1.382(6) . ? C45 C46 1.391(6) . ? C99 Cl4 1.756(4) . ? C99 Cl5 1.758(4) . ? C99 Cl3 1.763(5) . ? C98 Cl6 1.733(5) . ? C98 Cl7 1.750(5) . ? C98 Cl8 1.750(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 N1 Pd N2 89.85(12) . . ? N1 Pd Cl1 91.15(9) . . ? N2 Pd Cl1 178.98(10) . . ? N1 Pd Cl2 175.89(9) . . ? N2 Pd Cl2 87.27(10) . . ? Cl1 Pd Cl2 91.71(4) . . ? N1 P1 C21 117.36(17) . . ? N1 P1 C11 109.48(16) . . ? C21 P1 C11 107.51(17) . . ? N1 P1 C1 109.31(16) . . ? C21 P1 C1 108.26(18) . . ? C11 P1 C1 104.10(17) . . ? C31 N1 P1 122.7(2) . . ? C31 N1 Pd 118.1(2) . . ? P1 N1 Pd 114.27(16) . . ? C3 N2 C2 112.9(3) . . ? C3 N2 Pd 118.5(2) . . ? C2 N2 Pd 111.3(2) . . ? C2 C1 P1 119.0(3) . . ? N2 C2 C5 110.8(3) . . ? N2 C2 C1 111.0(3) . . ? C5 C2 C1 113.4(3) . . ? N2 C3 C41 114.1(3) . . ? N2 C3 C4 111.0(4) . . ? C41 C3 C4 110.4(3) . . ? C16 C11 C12 119.2(4) . . ? C16 C11 P1 123.0(3) . . ? C12 C11 P1 117.8(3) . . ? C13 C12 C11 120.9(4) . . ? C12 C13 C14 119.8(4) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C16 120.1(4) . . ? C11 C16 C15 119.9(4) . . ? C22 C21 C26 119.6(4) . . ? C22 C21 P1 120.0(3) . . ? C26 C21 P1 120.4(3) . . ? C21 C22 C23 119.9(4) . . ? C24 C23 C22 120.2(4) . . ? C25 C24 C23 120.2(4) . . ? C24 C25 C26 120.3(4) . . ? C25 C26 C21 119.8(4) . . ? C32 C31 C36 118.4(3) . . ? C32 C31 N1 123.8(3) . . ? C36 C31 N1 117.8(3) . . ? C31 C32 C33 120.6(4) . . ? C34 C33 C32 121.6(4) . . ? C33 C34 C35 117.4(4) . . ? C33 C34 C37 121.4(4) . . ? C35 C34 C37 121.2(4) . . ? C36 C35 C34 121.7(4) . . ? C35 C36 C31 120.2(4) . . ? C46 C41 C42 117.8(4) . . ? C46 C41 C3 123.1(3) . . ? C42 C41 C3 118.9(3) . . ? C43 C42 C41 121.5(4) . . ? C42 C43 C44 120.0(4) . . ? C43 C44 C45 119.9(4) . . ? C44 C45 C46 120.1(4) . . ? C45 C46 C41 120.7(4) . . ? Cl4 C99 Cl5 110.3(2) . . ? Cl4 C99 Cl3 110.2(2) . . ? Cl5 C99 Cl3 110.6(2) . . ? Cl6 C98 Cl7 110.2(3) . . ? Cl6 C98 Cl8 110.8(3) . . ? Cl7 C98 Cl8 110.0(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C99 H99 Cl1 1.00 2.39 3.306(5) 151.5 4_546 C2 H2 Cl1 1.00 2.87 3.641(4) 134.2 2_446 C1 H1A Cl2 0.99 2.64 3.573(4) 156.9 2_446 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.529 _refine_diff_density_min -0.526 _refine_diff_density_rms 0.088 #===END