# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'John Kennedy' _publ_contact_author_email J.D.KENNEDY@LEEDS.AC.UK loop_ _publ_author_name J.Kennedy J.Boulda data_jb428eCompound1 _database_code_depnum_ccdc_archive 'CCDC 672233' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H40 B10 N2 P2 Pd Pt' _chemical_formula_sum 'C28 H40 B10 N2 P2 Pd Pt' _chemical_formula_weight 876.15 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' B B 0.0013 0.0007 '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' Pd Pd -0.9988 1.0072 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6626(12) _cell_length_b 12.9085(12) _cell_length_c 14.5518(14) _cell_angle_alpha 71.088(5) _cell_angle_beta 74.801(5) _cell_angle_gamma 81.734(6) _cell_volume 2167.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description block _exptl_crystal_colour ; dark red ; _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.343 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 3.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2675 _exptl_absorpt_correction_T_max 0.7066 _exptl_absorpt_process_details ; See Sheldrick, G. M. (2002). SADABS. Version 2.03. University of Gottingen, Germany. ; _exptl_special_details ; The crystal temperature was held constant using an Oxford Cryosystems Cryostream 600 system. The power of the FR591 generator was 3.6kW ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Bruker Nonius FR591 rotating anode generator ; _diffrn_radiation_monochromator ; graphite model mounted in "parallel" mode ; _diffrn_measurement_device_type ; Mach3 kappa-type 4-circle goniostat. ; _diffrn_radiation_detector 'ApexII camera' _diffrn_measurement_method 'rotation images' _diffrn_detector_area_resol_mean ; 120 microns ; _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 52168 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.83 _reflns_number_total 11253 _reflns_number_gt 10237 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; APEX 2 software, Bruker Nonius 2004 ; _computing_cell_refinement ; APEX 2 software, Bruker Nonius 2004 ; _computing_data_reduction ; SAINT - Bruker Integration program embedded in APEX 2 software, Bruker Nonius 2004 ; _computing_molecular_graphics 'ORTEP-III Version 1.08 (Farrugia, 2005)' _computing_publication_material ; enCIFer: A program for viewing, editing and visualising CIFs. F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler, J. Applied Cryst., 37, 331-334, 2004 ; _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. Restraints were applied to the atoms of one phenyl ring due to disorder, and all the atoms in this disordered fragment were refined with constrained thermal parameters. The routine SQUEEZE was applied to the data due to the presence of three disordered dichloroethane molecules of crystallisation. It was not possible to model the disorder to a satisfactory level. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+1.0463*P+(0.0319P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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 11253 _refine_ls_number_parameters 419 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0254 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0596 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.201264(15) 0.214361(14) 0.498544(13) 0.01727(4) Uani 1 1 d . . . N1 N 0.23582(17) 0.06478(17) 0.45474(16) 0.0208(4) Uani 1 1 d . . . Pt2 Pt 0.329595(7) 0.400974(7) 0.389001(7) 0.01751(3) Uani 1 1 d . A . C2 C 0.3172(2) -0.0133(2) 0.4713(2) 0.0245(5) Uani 1 1 d . . . H121 H 0.3719 -0.0007 0.4996 0.029 Uiso 1 1 calc R . . C3 C 0.3257(2) -0.1130(2) 0.4487(2) 0.0284(6) Uani 1 1 d . . . H131 H 0.3847 -0.1658 0.4615 0.034 Uiso 1 1 calc R . . B3 B 0.1718(2) 0.3837(2) 0.5181(2) 0.0187(5) Uani 1 1 d . . . H3 H 0.1017 0.4271 0.4840 0.022 Uiso 1 1 calc R . . C4 C 0.2467(2) -0.1323(2) 0.4080(2) 0.0293(6) Uani 1 1 d . . . H141 H 0.2512 -0.1990 0.3923 0.035 Uiso 1 1 calc R . . B4 B 0.1512(2) 0.2646(2) 0.6349(2) 0.0213(5) Uani 1 1 d . . . H4 H 0.0683 0.2350 0.6777 0.026 Uiso 1 1 calc R . . C5 C 0.1581(2) -0.0529(2) 0.38920(19) 0.0250(5) Uani 1 1 d . . . B5 B 0.2763(2) 0.1739(2) 0.6270(2) 0.0209(5) Uani 1 1 d . . . H5 H 0.2777 0.0831 0.6641 0.025 Uiso 1 1 calc R . . B6 B 0.3731(2) 0.2386(2) 0.5062(2) 0.0194(5) Uani 1 1 d . . . H6 H 0.4336 0.1876 0.4646 0.023 Uiso 1 1 calc R . . C7 C 0.0720(3) -0.0660(2) 0.3466(2) 0.0304(6) Uani 1 1 d . . . H171 H 0.0715 -0.1324 0.3318 0.036 Uiso 1 1 calc R . . B7 B 0.2822(2) 0.4601(2) 0.5243(2) 0.0210(5) Uani 1 1 d . . . H7 H 0.2805 0.5519 0.4989 0.025 Uiso 1 1 calc R . . C8 C -0.0088(3) 0.0144(2) 0.3268(2) 0.0315(6) Uani 1 1 d . . . H181 H -0.0630 0.0040 0.2966 0.038 Uiso 1 1 calc R . . B8 B 0.1863(2) 0.3931(2) 0.6350(2) 0.0217(6) Uani 1 1 d . . . H8 H 0.1243 0.4439 0.6755 0.026 Uiso 1 1 calc R . . C9 C -0.0132(2) 0.1162(2) 0.35148(19) 0.0237(5) Uani 1 1 d . . . B9 B 0.2515(2) 0.2655(2) 0.7001(2) 0.0220(6) Uani 1 1 d . . . H9 H 0.2343 0.2335 0.7835 0.026 Uiso 1 1 calc R . . C10 C -0.0967(2) 0.2015(2) 0.3345(2) 0.0291(6) Uani 1 1 d . . . H101 H -0.1520 0.1952 0.3038 0.035 Uiso 1 1 calc R . . B10 B 0.3860(2) 0.2488(2) 0.6223(2) 0.0219(6) Uani 1 1 d . . . H10 H 0.4567 0.2037 0.6546 0.026 Uiso 1 1 calc R . . C11 C -0.0970(2) 0.2942(2) 0.3632(2) 0.0284(6) Uani 1 1 d . . . H111 H -0.1524 0.3519 0.3525 0.034 Uiso 1 1 calc R . . B11 B 0.4106(2) 0.3678(2) 0.5162(2) 0.0219(6) Uani 1 1 d . . . H11 H 0.4954 0.3974 0.4852 0.026 Uiso 1 1 calc R . . C12 C -0.0134(2) 0.3012(2) 0.4086(2) 0.0242(5) Uani 1 1 d . . . H112 H -0.0147 0.3645 0.4288 0.029 Uiso 1 1 calc R . . B12 B 0.3309(2) 0.3826(2) 0.6326(2) 0.0223(6) Uani 1 1 d . . . H12 H 0.3643 0.4258 0.6733 0.027 Uiso 1 1 calc R . . N13 N 0.06812(18) 0.22263(17) 0.42468(16) 0.0215(4) Uani 1 1 d . . . C14 C 0.0686(2) 0.1303(2) 0.39611(18) 0.0200(5) Uani 1 1 d . . . C15 C 0.1564(2) 0.0454(2) 0.41394(18) 0.0206(5) Uani 1 1 d . . . P21 P 0.47120(6) 0.34764(5) 0.27006(5) 0.02401(14) Uani 1 1 d . . . C21 C 0.5055(3) 0.4362(2) 0.1393(2) 0.0317(6) Uani 1 1 d . A . H21A H 0.5676 0.4014 0.1011 0.048 Uiso 1 1 calc R . . H21B H 0.5252 0.5076 0.1376 0.048 Uiso 1 1 calc R . . H21C H 0.4419 0.4465 0.1100 0.048 Uiso 1 1 calc R . . P22 P 0.24496(5) 0.54036(5) 0.27840(5) 0.02043(13) Uani 1 1 d . . . C22 C 0.6048(2) 0.3262(3) 0.3032(2) 0.0347(7) Uani 1 1 d . A . H22A H 0.6023 0.2655 0.3651 0.052 Uiso 1 1 calc R . . H22B H 0.6215 0.3932 0.3128 0.052 Uiso 1 1 calc R . . H22C H 0.6618 0.3084 0.2494 0.052 Uiso 1 1 calc R . . C23 C 0.4544(3) 0.2203(5) 0.2510(5) 0.0206(10) Uani 0.80 1 d P A 1 C24 C 0.3585(4) 0.2139(5) 0.2212(6) 0.0261(11) Uani 0.80 1 d P A 1 H24 H 0.3038 0.2727 0.2179 0.031 Uiso 0.80 1 calc PR A 1 C25 C 0.3431(5) 0.1219(5) 0.1964(6) 0.0318(12) Uani 0.80 1 d P A 1 H25 H 0.2792 0.1191 0.1749 0.038 Uiso 0.80 1 calc PR A 1 C26 C 0.4232(4) 0.0335(5) 0.2035(5) 0.0321(12) Uani 0.80 1 d P A 1 H26 H 0.4132 -0.0289 0.1863 0.039 Uiso 0.80 1 calc PR A 1 C27 C 0.5162(4) 0.0368(4) 0.2354(4) 0.0311(11) Uani 0.80 1 d P A 1 H27 H 0.5692 -0.0236 0.2407 0.037 Uiso 0.80 1 calc PR A 1 C28 C 0.5325(4) 0.1288(5) 0.2599(5) 0.0261(10) Uani 0.80 1 d P A 1 H28 H 0.5961 0.1301 0.2826 0.031 Uiso 0.80 1 calc PR A 1 C29 C 0.4268(18) 0.216(2) 0.248(2) 0.0206(10) Uani 0.20 1 d PD A 2 C30 C 0.506(2) 0.128(2) 0.250(2) 0.0261(10) Uani 0.20 1 d PD A 2 H30 H 0.5726 0.1278 0.2687 0.031 Uiso 0.20 1 calc PR A 2 C31 C 0.485(2) 0.039(2) 0.222(2) 0.0311(11) Uani 0.20 1 d PD A 2 H31 H 0.5363 -0.0221 0.2232 0.037 Uiso 0.20 1 calc PR A 2 C32 C 0.388(2) 0.041(2) 0.194(2) 0.0321(12) Uani 0.20 1 d PD A 2 H32 H 0.3720 -0.0203 0.1790 0.039 Uiso 0.20 1 calc PR A 2 C33 C 0.317(3) 0.132(2) 0.188(3) 0.0318(12) Uani 0.20 1 d PD A 2 H33 H 0.2526 0.1338 0.1645 0.038 Uiso 0.20 1 calc PR A 2 C34 C 0.333(2) 0.223(3) 0.214(3) 0.0261(11) Uani 0.20 1 d PD A 2 H34 H 0.2835 0.2860 0.2082 0.031 Uiso 0.20 1 calc PR A 2 C221 C 0.1766(3) 0.5035(2) 0.1974(2) 0.0340(6) Uani 1 1 d . A . H13A H 0.1424 0.5699 0.1576 0.051 Uiso 1 1 calc R . . H13B H 0.1203 0.4523 0.2386 0.051 Uiso 1 1 calc R . . H13C H 0.2308 0.4688 0.1528 0.051 Uiso 1 1 calc R . . C222 C 0.1372(2) 0.6281(2) 0.3338(2) 0.0314(6) Uani 1 1 d . A . H14A H 0.1217 0.6945 0.2815 0.047 Uiso 1 1 calc R . . H14B H 0.1619 0.6485 0.3837 0.047 Uiso 1 1 calc R . . H14C H 0.0705 0.5881 0.3659 0.047 Uiso 1 1 calc R . . C223 C 0.3436(2) 0.6405(2) 0.19326(19) 0.0221(5) Uani 1 1 d . A . C224 C 0.4239(2) 0.6674(2) 0.2317(2) 0.0256(5) Uani 1 1 d . . . H20 H 0.4248 0.6351 0.3002 0.031 Uiso 1 1 calc R A . C225 C 0.5016(3) 0.7410(2) 0.1696(2) 0.0330(6) Uani 1 1 d . A . H19 H 0.5544 0.7600 0.1963 0.040 Uiso 1 1 calc R . . C226 C 0.5029(3) 0.7876(2) 0.0677(2) 0.0366(7) Uani 1 1 d . . . H18 H 0.5572 0.8366 0.0253 0.044 Uiso 1 1 calc R A . C227 C 0.4238(3) 0.7615(3) 0.0289(2) 0.0370(7) Uani 1 1 d . A . H17 H 0.4241 0.7926 -0.0399 0.044 Uiso 1 1 calc R . . C228 C 0.3443(3) 0.6897(2) 0.0916(2) 0.0306(6) Uani 1 1 d . . . H16 H 0.2896 0.6737 0.0651 0.037 Uiso 1 1 calc R A . 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 0.01725(9) 0.01601(8) 0.01942(9) -0.00672(7) -0.00556(7) 0.00199(6) N1 0.0207(10) 0.0204(10) 0.0209(10) -0.0072(8) -0.0034(8) -0.0001(8) Pt2 0.01816(5) 0.01661(5) 0.01545(5) -0.00413(3) -0.00256(3) 0.00219(3) C2 0.0234(13) 0.0231(12) 0.0255(13) -0.0077(10) -0.0039(10) 0.0017(10) C3 0.0306(14) 0.0211(12) 0.0278(14) -0.0058(10) -0.0014(11) 0.0034(10) B3 0.0192(13) 0.0178(12) 0.0184(13) -0.0062(10) -0.0028(10) 0.0002(10) C4 0.0355(15) 0.0200(12) 0.0301(14) -0.0113(11) -0.0007(12) 0.0010(11) B4 0.0211(14) 0.0211(13) 0.0205(13) -0.0072(10) -0.0022(11) -0.0005(10) C5 0.0294(14) 0.0225(12) 0.0213(12) -0.0082(10) 0.0004(10) -0.0039(10) B5 0.0228(14) 0.0203(12) 0.0170(13) -0.0020(10) -0.0053(11) -0.0007(10) B6 0.0230(14) 0.0193(12) 0.0158(12) -0.0064(10) -0.0046(10) 0.0026(10) C7 0.0396(16) 0.0265(13) 0.0286(14) -0.0143(11) -0.0032(12) -0.0079(12) B7 0.0238(14) 0.0197(12) 0.0198(13) -0.0072(10) -0.0049(11) -0.0001(10) C8 0.0339(15) 0.0377(15) 0.0288(14) -0.0141(12) -0.0093(12) -0.0070(12) B8 0.0246(14) 0.0208(13) 0.0192(13) -0.0078(10) -0.0042(11) 0.0023(10) C9 0.0257(13) 0.0269(12) 0.0197(12) -0.0067(10) -0.0060(10) -0.0048(10) B9 0.0245(14) 0.0222(13) 0.0194(13) -0.0073(11) -0.0058(11) 0.0023(11) C10 0.0254(14) 0.0365(15) 0.0281(14) -0.0101(12) -0.0099(11) -0.0031(11) B10 0.0250(14) 0.0237(13) 0.0191(13) -0.0076(11) -0.0084(11) 0.0014(11) C11 0.0253(14) 0.0286(13) 0.0315(14) -0.0080(11) -0.0104(11) 0.0027(10) B11 0.0213(14) 0.0201(13) 0.0230(14) -0.0051(11) -0.0058(11) 0.0007(10) C12 0.0248(13) 0.0214(12) 0.0263(13) -0.0070(10) -0.0071(10) 0.0002(10) B12 0.0249(14) 0.0224(13) 0.0203(13) -0.0073(11) -0.0058(11) -0.0003(11) N13 0.0223(11) 0.0202(10) 0.0204(10) -0.0047(8) -0.0038(8) -0.0020(8) C14 0.0215(12) 0.0205(11) 0.0167(11) -0.0057(9) -0.0007(9) -0.0034(9) C15 0.0213(12) 0.0205(11) 0.0181(11) -0.0062(9) 0.0003(9) -0.0031(9) P21 0.0236(3) 0.0226(3) 0.0193(3) -0.0043(2) 0.0003(3) 0.0045(2) C21 0.0381(16) 0.0250(13) 0.0218(13) -0.0041(11) 0.0039(12) 0.0032(11) P22 0.0220(3) 0.0183(3) 0.0191(3) -0.0043(2) -0.0055(2) 0.0032(2) C22 0.0227(14) 0.0418(16) 0.0330(15) -0.0092(13) -0.0006(12) 0.0036(12) C23 0.016(3) 0.0235(14) 0.0184(13) -0.0054(10) 0.000(2) 0.0019(19) C24 0.024(3) 0.0257(18) 0.0238(19) -0.0049(15) -0.006(2) 0.0068(19) C25 0.035(4) 0.035(2) 0.024(2) -0.0062(18) -0.006(2) -0.005(2) C26 0.045(4) 0.0216(17) 0.026(2) -0.0056(15) -0.002(3) -0.003(2) C27 0.036(3) 0.0208(14) 0.027(2) -0.0028(14) -0.0030(19) 0.007(2) C28 0.025(3) 0.0262(13) 0.020(2) -0.0010(12) -0.0045(18) 0.0037(18) C29 0.016(3) 0.0235(14) 0.0184(13) -0.0054(10) 0.000(2) 0.0019(19) C30 0.025(3) 0.0262(13) 0.020(2) -0.0010(12) -0.0045(18) 0.0037(18) C31 0.036(3) 0.0208(14) 0.027(2) -0.0028(14) -0.0030(19) 0.007(2) C32 0.045(4) 0.0216(17) 0.026(2) -0.0056(15) -0.002(3) -0.003(2) C33 0.035(4) 0.035(2) 0.024(2) -0.0062(18) -0.006(2) -0.005(2) C34 0.024(3) 0.0257(18) 0.0238(19) -0.0049(15) -0.006(2) 0.0068(19) C221 0.0387(17) 0.0319(14) 0.0345(16) -0.0057(12) -0.0177(13) -0.0048(12) C222 0.0263(14) 0.0238(13) 0.0335(15) -0.0043(11) 0.0009(11) 0.0072(10) C223 0.0255(13) 0.0187(11) 0.0196(12) -0.0044(9) -0.0046(10) 0.0025(9) C224 0.0325(14) 0.0243(12) 0.0184(12) -0.0043(10) -0.0070(10) 0.0005(10) C225 0.0387(16) 0.0360(15) 0.0263(14) -0.0100(12) -0.0068(12) -0.0087(13) C226 0.0460(18) 0.0325(15) 0.0267(15) -0.0029(12) -0.0009(13) -0.0160(13) C227 0.0513(19) 0.0367(16) 0.0189(13) 0.0002(11) -0.0085(13) -0.0094(14) C228 0.0352(16) 0.0324(14) 0.0237(13) -0.0042(11) -0.0113(12) -0.0020(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 2.176(2) . ? Pd1 B4 2.195(3) . ? Pd1 B5 2.197(3) . ? Pd1 N13 2.198(2) . ? Pd1 B3 2.261(3) . ? Pd1 B6 2.278(3) . ? Pd1 Pt2 2.8745(3) . ? N1 C2 1.346(3) . ? N1 C15 1.381(3) . ? Pt2 B11 2.239(3) . ? Pt2 B7 2.246(3) . ? Pt2 B6 2.334(3) . ? Pt2 P22 2.3343(7) . ? Pt2 B3 2.337(3) . ? Pt2 P21 2.3399(7) . ? C2 C3 1.411(4) . ? C2 H121 0.9500 . ? C3 C4 1.375(4) . ? C3 H131 0.9500 . ? B3 B8 1.802(4) . ? B3 B7 1.859(4) . ? B3 B4 1.873(4) . ? B3 H3 1.1200 . ? C4 C5 1.425(4) . ? C4 H141 0.9500 . ? B4 B9 1.776(4) . ? B4 B8 1.778(4) . ? B4 B5 1.831(4) . ? B4 H4 1.1200 . ? C5 C15 1.423(3) . ? C5 C7 1.442(4) . ? B5 B9 1.778(4) . ? B5 B10 1.778(4) . ? B5 B6 1.871(4) . ? B5 H5 1.1200 . ? B6 B10 1.787(4) . ? B6 B11 1.858(4) . ? B6 H6 1.1200 . ? C7 C8 1.365(4) . ? C7 H171 0.9500 . ? B7 B12 1.781(4) . ? B7 B8 1.786(4) . ? B7 B11 1.873(4) . ? B7 H7 1.1200 . ? C8 C9 1.461(4) . ? C8 H181 0.9500 . ? B8 B12 1.807(4) . ? B8 B9 1.817(4) . ? B8 H8 1.1200 . ? C9 C14 1.418(4) . ? C9 C10 1.420(4) . ? B9 B12 1.793(4) . ? B9 B10 1.808(4) . ? B9 H9 1.1200 . ? C10 C11 1.388(4) . ? C10 H101 0.9500 . ? B10 B11 1.786(4) . ? B10 B12 1.805(4) . ? B10 H10 1.1200 . ? C11 C12 1.413(4) . ? C11 H111 0.9500 . ? B11 B12 1.784(4) . ? B11 H11 1.1200 . ? C12 N13 1.350(3) . ? C12 H112 0.9500 . ? B12 H12 1.1200 . ? N13 C14 1.382(3) . ? C14 C15 1.457(3) . ? P21 C23 1.803(6) . ? P21 C22 1.838(3) . ? P21 C21 1.848(3) . ? P21 C29 2.01(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? P22 C222 1.834(3) . ? P22 C221 1.838(3) . ? P22 C223 1.839(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.414(5) . ? C23 C28 1.422(5) . ? C24 C25 1.399(6) . ? C24 H24 0.9500 . ? C25 C26 1.409(7) . ? C25 H25 0.9500 . ? C26 C27 1.385(6) . ? C26 H26 0.9500 . ? C27 C28 1.401(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.381(17) . ? C29 C30 1.403(18) . ? C30 C31 1.411(18) . ? C30 H30 0.9500 . ? C31 C32 1.376(17) . ? C31 H31 0.9500 . ? C32 C33 1.374(18) . ? C32 H32 0.9500 . ? C33 C34 1.404(19) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C221 H13A 0.9800 . ? C221 H13B 0.9800 . ? C221 H13C 0.9800 . ? C222 H14A 0.9800 . ? C222 H14B 0.9800 . ? C222 H14C 0.9800 . ? C223 C228 1.407(4) . ? C223 C224 1.411(4) . ? C224 C225 1.392(4) . ? C224 H20 0.9500 . ? C225 C226 1.405(4) . ? C225 H19 0.9500 . ? C226 C227 1.397(5) . ? C226 H18 0.9500 . ? C227 C228 1.393(4) . ? C227 H17 0.9500 . ? C228 H16 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pd1 B4 139.30(9) . . ? N1 Pd1 B5 102.93(9) . . ? B4 Pd1 B5 49.29(11) . . ? N1 Pd1 N13 77.63(8) . . ? B4 Pd1 N13 114.73(10) . . ? B5 Pd1 N13 154.90(9) . . ? N1 Pd1 B3 171.01(9) . . ? B4 Pd1 B3 49.69(10) . . ? B5 Pd1 B3 83.92(10) . . ? N13 Pd1 B3 98.70(9) . . ? N1 Pd1 B6 99.18(9) . . ? B4 Pd1 B6 83.61(10) . . ? B5 Pd1 B6 49.41(10) . . ? N13 Pd1 B6 155.69(9) . . ? B3 Pd1 B6 80.74(10) . . ? N1 Pd1 Pt2 120.54(6) . . ? B4 Pd1 Pt2 93.39(7) . . ? B5 Pd1 Pt2 93.25(7) . . ? N13 Pd1 Pt2 108.22(5) . . ? B3 Pd1 Pt2 52.49(7) . . ? B6 Pd1 Pt2 52.33(7) . . ? C2 N1 C15 117.8(2) . . ? C2 N1 Pd1 128.14(18) . . ? C15 N1 Pd1 113.68(16) . . ? B11 Pt2 B7 49.37(11) . . ? B11 Pt2 B6 47.88(10) . . ? B7 Pt2 B6 81.57(10) . . ? B11 Pt2 P22 142.85(7) . . ? B7 Pt2 P22 100.73(7) . . ? B6 Pt2 P22 165.05(7) . . ? B11 Pt2 B3 81.71(10) . . ? B7 Pt2 B3 47.82(10) . . ? B6 Pt2 B3 78.01(10) . . ? P22 Pt2 B3 92.51(7) . . ? B11 Pt2 P21 101.55(8) . . ? B7 Pt2 P21 147.32(8) . . ? B6 Pt2 P21 87.56(7) . . ? P22 Pt2 P21 97.63(2) . . ? B3 Pt2 P21 157.33(7) . . ? B11 Pt2 Pd1 89.71(7) . . ? B7 Pt2 Pd1 89.36(7) . . ? B6 Pt2 Pd1 50.57(7) . . ? P22 Pt2 Pd1 114.508(18) . . ? B3 Pt2 Pd1 50.14(6) . . ? P21 Pt2 Pd1 107.227(19) . . ? N1 C2 C3 123.5(3) . . ? N1 C2 H121 118.3 . . ? C3 C2 H121 118.3 . . ? C4 C3 C2 118.7(3) . . ? C4 C3 H131 120.6 . . ? C2 C3 H131 120.6 . . ? B8 B3 B7 58.39(16) . . ? B8 B3 B4 57.83(15) . . ? B7 B3 B4 105.96(19) . . ? B8 B3 Pd1 116.15(16) . . ? B7 B3 Pd1 123.11(16) . . ? B4 B3 Pd1 63.32(12) . . ? B8 B3 Pt2 117.00(17) . . ? B7 B3 Pt2 63.52(12) . . ? B4 B3 Pt2 123.70(16) . . ? Pd1 B3 Pt2 77.37(8) . . ? B8 B3 H3 122.0 . . ? B7 B3 H3 121.6 . . ? B4 B3 H3 121.7 . . ? Pd1 B3 H3 108.1 . . ? Pt2 B3 H3 107.4 . . ? C3 C4 C5 120.4(2) . . ? C3 C4 H141 119.8 . . ? C5 C4 H141 119.8 . . ? B9 B4 B8 61.48(17) . . ? B9 B4 B5 59.04(16) . . ? B8 B4 B5 108.1(2) . . ? B9 B4 B3 107.8(2) . . ? B8 B4 B3 59.07(15) . . ? B5 B4 B3 107.15(18) . . ? B9 B4 Pd1 119.35(17) . . ? B8 B4 Pd1 120.58(17) . . ? B5 B4 Pd1 65.39(12) . . ? B3 B4 Pd1 66.99(12) . . ? B9 B4 H4 119.8 . . ? B8 B4 H4 119.1 . . ? B5 B4 H4 123.4 . . ? B3 B4 H4 122.8 . . ? Pd1 B4 H4 109.6 . . ? C15 C5 C4 117.0(2) . . ? C15 C5 C7 118.7(2) . . ? C4 C5 C7 124.3(2) . . ? B9 B5 B10 61.11(16) . . ? B9 B5 B4 58.93(16) . . ? B10 B5 B4 107.52(19) . . ? B9 B5 B6 107.42(19) . . ? B10 B5 B6 58.58(15) . . ? B4 B5 B6 107.30(18) . . ? B9 B5 Pd1 119.19(17) . . ? B10 B5 Pd1 120.38(17) . . ? B4 B5 Pd1 65.32(13) . . ? B6 B5 Pd1 67.56(13) . . ? B9 B5 H5 120.1 . . ? B10 B5 H5 119.7 . . ? B4 B5 H5 123.5 . . ? B6 B5 H5 122.7 . . ? Pd1 B5 H5 109.5 . . ? B10 B6 B11 58.64(15) . . ? B10 B6 B5 58.10(16) . . ? B11 B6 B5 106.49(18) . . ? B10 B6 Pd1 115.88(17) . . ? B11 B6 Pd1 122.69(16) . . ? B5 B6 Pd1 63.03(12) . . ? B10 B6 Pt2 117.05(16) . . ? B11 B6 Pt2 63.38(12) . . ? B5 B6 Pt2 123.74(16) . . ? Pd1 B6 Pt2 77.09(9) . . ? B10 B6 H6 121.9 . . ? B11 B6 H6 121.5 . . ? B5 B6 H6 121.4 . . ? Pd1 B6 H6 108.6 . . ? Pt2 B6 H6 107.6 . . ? C8 C7 C5 121.9(2) . . ? C8 C7 H171 119.1 . . ? C5 C7 H171 119.1 . . ? B12 B7 B8 60.88(16) . . ? B12 B7 B3 107.01(19) . . ? B8 B7 B3 59.20(16) . . ? B12 B7 B11 58.39(16) . . ? B8 B7 B11 107.27(19) . . ? B3 B7 B11 106.71(18) . . ? B12 B7 Pt2 119.09(17) . . ? B8 B7 Pt2 122.37(17) . . ? B3 B7 Pt2 68.66(12) . . ? B11 B7 Pt2 65.14(12) . . ? B12 B7 H7 120.7 . . ? B8 B7 H7 118.9 . . ? B3 B7 H7 122.5 . . ? B11 B7 H7 124.3 . . ? Pt2 B7 H7 108.4 . . ? C7 C8 C9 120.8(3) . . ? C7 C8 H181 119.6 . . ? C9 C8 H181 119.6 . . ? B4 B8 B7 113.5(2) . . ? B4 B8 B3 63.11(16) . . ? B7 B8 B3 62.41(16) . . ? B4 B8 B12 108.01(19) . . ? B7 B8 B12 59.41(16) . . ? B3 B8 B12 108.37(19) . . ? B4 B8 B9 59.21(16) . . ? B7 B8 B9 109.0(2) . . ? B3 B8 B9 109.20(19) . . ? B12 B8 B9 59.32(16) . . ? B4 B8 H8 119.4 . . ? B7 B8 H8 119.2 . . ? B3 B8 H8 119.8 . . ? B12 B8 H8 123.0 . . ? B9 B8 H8 122.3 . . ? C14 C9 C10 118.0(2) . . ? C14 C9 C8 118.8(2) . . ? C10 C9 C8 123.2(2) . . ? B4 B9 B5 62.03(16) . . ? B4 B9 B12 108.7(2) . . ? B5 B9 B12 109.0(2) . . ? B4 B9 B10 108.6(2) . . ? B5 B9 B10 59.45(16) . . ? B12 B9 B10 60.17(16) . . ? B4 B9 B8 59.31(16) . . ? B5 B9 B8 108.7(2) . . ? B12 B9 B8 60.08(16) . . ? B10 B9 B8 107.3(2) . . ? B4 B9 H9 120.9 . . ? B5 B9 H9 120.7 . . ? B12 B9 H9 121.2 . . ? B10 B9 H9 122.2 . . ? B8 B9 H9 122.2 . . ? C11 C10 C9 119.6(3) . . ? C11 C10 H101 120.2 . . ? C9 C10 H101 120.2 . . ? B5 B10 B11 113.9(2) . . ? B5 B10 B6 63.32(16) . . ? B11 B10 B6 62.66(16) . . ? B5 B10 B12 108.4(2) . . ? B11 B10 B12 59.57(16) . . ? B6 B10 B12 108.9(2) . . ? B5 B10 B9 59.44(16) . . ? B11 B10 B9 109.5(2) . . ? B6 B10 B9 109.8(2) . . ? B12 B10 B9 59.52(16) . . ? B5 B10 H10 119.2 . . ? B11 B10 H10 118.9 . . ? B6 B10 H10 119.4 . . ? B12 B10 H10 122.8 . . ? B9 B10 H10 122.0 . . ? C10 C11 C12 118.8(3) . . ? C10 C11 H111 120.6 . . ? C12 C11 H111 120.6 . . ? B12 B11 B10 60.75(16) . . ? B12 B11 B6 106.70(19) . . ? B10 B11 B6 58.70(15) . . ? B12 B11 B7 58.22(16) . . ? B10 B11 B7 106.8(2) . . ? B6 B11 B7 106.65(19) . . ? B12 B11 Pt2 119.25(18) . . ? B10 B11 Pt2 121.94(18) . . ? B6 B11 Pt2 68.73(13) . . ? B7 B11 Pt2 65.48(13) . . ? B12 B11 H11 120.8 . . ? B10 B11 H11 119.5 . . ? B6 B11 H11 122.7 . . ? B7 B11 H11 124.4 . . ? Pt2 B11 H11 108.3 . . ? N13 C12 C11 123.3(2) . . ? N13 C12 H112 118.3 . . ? C11 C12 H112 118.3 . . ? B7 B12 B11 63.40(16) . . ? B7 B12 B9 110.3(2) . . ? B11 B12 B9 110.2(2) . . ? B7 B12 B10 110.0(2) . . ? B11 B12 B10 59.68(16) . . ? B9 B12 B10 60.31(16) . . ? B7 B12 B8 59.71(16) . . ? B11 B12 B8 110.3(2) . . ? B9 B12 B8 60.60(16) . . ? B10 B12 B8 107.8(2) . . ? B7 B12 H12 119.7 . . ? B11 B12 H12 119.6 . . ? B9 B12 H12 120.5 . . ? B10 B12 H12 122.0 . . ? B8 B12 H12 121.7 . . ? C12 N13 C14 117.9(2) . . ? C12 N13 Pd1 129.12(17) . . ? C14 N13 Pd1 112.89(16) . . ? N13 C14 C9 122.3(2) . . ? N13 C14 C15 117.8(2) . . ? C9 C14 C15 119.9(2) . . ? N1 C15 C5 122.5(2) . . ? N1 C15 C14 117.6(2) . . ? C5 C15 C14 119.9(2) . . ? C23 P21 C22 104.18(16) . . ? C23 P21 C21 100.3(2) . . ? C22 P21 C21 101.51(14) . . ? C23 P21 C29 9.5(7) . . ? C22 P21 C29 113.5(6) . . ? C21 P21 C29 99.5(9) . . ? C23 P21 Pt2 114.94(17) . . ? C22 P21 Pt2 112.67(10) . . ? C21 P21 Pt2 121.01(9) . . ? C29 P21 Pt2 108.1(8) . . ? P21 C21 H21A 109.5 . . ? P21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P21 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C222 P22 C221 101.55(15) . . ? C222 P22 C223 101.95(12) . . ? C221 P22 C223 105.26(13) . . ? C222 P22 Pt2 116.37(10) . . ? C221 P22 Pt2 118.92(10) . . ? C223 P22 Pt2 110.87(9) . . ? P21 C22 H22A 109.5 . . ? P21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C28 118.4(5) . . ? C24 C23 P21 117.0(4) . . ? C28 C23 P21 124.6(3) . . ? C25 C24 C23 120.9(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 119.5(4) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 120.5(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 120.4(4) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 120.3(4) . . ? C27 C28 H28 119.9 . . ? C23 C28 H28 119.9 . . ? C34 C29 C30 123(3) . . ? C34 C29 P21 120(2) . . ? C30 C29 P21 115.7(17) . . ? C29 C30 C31 118(2) . . ? C29 C30 H30 121.1 . . ? C31 C30 H30 121.1 . . ? C32 C31 C30 120(3) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C33 C32 C31 120(3) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 123(3) . . ? C32 C33 H33 118.6 . . ? C34 C33 H33 118.6 . . ? C29 C34 C33 116(3) . . ? C29 C34 H34 122.0 . . ? C33 C34 H34 122.0 . . ? P22 C221 H13A 109.5 . . ? P22 C221 H13B 109.5 . . ? H13A C221 H13B 109.5 . . ? P22 C221 H13C 109.5 . . ? H13A C221 H13C 109.5 . . ? H13B C221 H13C 109.5 . . ? P22 C222 H14A 109.5 . . ? P22 C222 H14B 109.5 . . ? H14A C222 H14B 109.5 . . ? P22 C222 H14C 109.5 . . ? H14A C222 H14C 109.5 . . ? H14B C222 H14C 109.5 . . ? C228 C223 C224 118.6(2) . . ? C228 C223 P22 123.3(2) . . ? C224 C223 P22 118.14(19) . . ? C225 C224 C223 120.2(2) . . ? C225 C224 H20 119.9 . . ? C223 C224 H20 119.9 . . ? C224 C225 C226 120.6(3) . . ? C224 C225 H19 119.7 . . ? C226 C225 H19 119.7 . . ? C227 C226 C225 119.6(3) . . ? C227 C226 H18 120.2 . . ? C225 C226 H18 120.2 . . ? C228 C227 C226 119.8(3) . . ? C228 C227 H17 120.1 . . ? C226 C227 H17 120.1 . . ? C227 C228 C223 121.2(3) . . ? C227 C228 H16 119.4 . . ? C223 C228 H16 119.4 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.83 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.621 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.098 data_jb428f3Compound2 _database_code_depnum_ccdc_archive 'CCDC 672234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H40 B10 N2 O2 P2 Pd Pt S, 3(C H2 Cl2)' _chemical_formula_sum 'C31 H46 B10 Cl6 N2 O2 P2 Pd Pt S' _chemical_formula_weight 1194.99 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Pt Pt -1.7033 8.3905 '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 14.689(2) _cell_length_b 17.188(2) _cell_length_c 18.742(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.046(8) _cell_angle_gamma 90.00 _cell_volume 4685.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.694 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 3.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4710 _exptl_absorpt_correction_T_max 0.8307 _exptl_absorpt_process_details ; See Sheldrick, G. M. (2002). SADABS. Version 2.03. University of Gottingen, Germany. ; _exptl_special_details ; The crystal temperature was held constant using an Oxford Cryosystems Cryostream 600 system. The power of the FR591 generator was 3.6kW ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ; Bruker Nonius FR591 rotating anode generator ; _diffrn_radiation_monochromator ; graphite model mounted in "parallel" mode ; _diffrn_measurement_device_type ; Mach3 kappa-type 4-circle goniostat. ; _diffrn_radiation_detector 'ApexII camera' _diffrn_measurement_method 'rotation images' _diffrn_detector_area_resol_mean ; 120 microns ; _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 109904 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0354 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 29.43 _reflns_number_total 12289 _reflns_number_gt 10072 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; APEX 2 software, Bruker Nonius 2004 ; _computing_cell_refinement ; APEX 2 software, Bruker Nonius 2004 ; _computing_data_reduction ; SAINT - Bruker Integration program embedded in APEX 2 software, Bruker Nonius 2004 ; _computing_molecular_graphics 'ORTEP-III Version 1.08 (Farrugia, 2005)' _computing_publication_material ; enCIFer: A program for viewing, editing and visualising CIFs. F. H. Allen, O. Johnson, G. P. Shields, B. R. Smith, M. Towler, J. Applied Cryst., 37, 331-334, 2004 ; _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. Crystals were weakly diffracting. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+11.5720*P+(0.0333P)^2^+0.0000sin\q/\l] where P = 0.00000Fo^2^ + 1.00000Fc^2^ ; _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 12289 _refine_ls_number_parameters 509 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0799 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.734619(18) 0.137909(16) 0.113556(14) 0.01684(6) Uani 1 1 d . . . Cl1S Cl 0.78924(17) -0.03017(14) 0.60164(12) 0.0972(7) Uani 1 1 d . . . S1 S 0.82659(6) 0.21267(6) 0.04103(5) 0.02367(19) Uani 1 1 d . . . O1 O 0.8669(2) 0.1720(2) -0.01636(16) 0.0392(8) Uani 1 1 d . . . N1 N 0.7046(2) 0.04462(18) 0.03157(16) 0.0198(6) Uani 1 1 d . . . C1S C 0.8712(5) -0.0733(4) 0.5520(4) 0.0718(19) Uani 1 1 d . . . H2S H 0.9334 -0.0681 0.5797 0.086 Uiso 1 1 calc R . . H1S H 0.8576 -0.1295 0.5457 0.086 Uiso 1 1 calc R . . Pt2 Pt 0.904749(9) 0.203933(8) 0.164341(7) 0.01593(4) Uani 1 1 d . . . Cl2S Cl 0.86965(18) -0.02976(14) 0.46677(11) 0.1007(7) Uani 1 1 d . . . O2 O 0.7864(2) 0.28900(17) 0.01886(17) 0.0353(7) Uani 1 1 d . . . C2 C 0.7494(3) -0.0218(2) 0.0252(2) 0.0262(8) Uani 1 1 d . . . H21 H 0.8050 -0.0308 0.0566 0.031 Uiso 1 1 calc R . . C2S C 1.5491(4) 0.3634(3) 0.2543(3) 0.0458(12) Uani 1 1 d . . . H4S H 1.6061 0.3947 0.2574 0.055 Uiso 1 1 calc R . . H3S H 1.5646 0.3090 0.2436 0.055 Uiso 1 1 calc R . . Cl3S Cl 1.50660(15) 0.36669(9) 0.33821(9) 0.0708(5) Uani 1 1 d . . . C3 C 0.7178(3) -0.0798(2) -0.0262(2) 0.0300(9) Uani 1 1 d . . . H31 H 0.7513 -0.1268 -0.0287 0.036 Uiso 1 1 calc R . . C3S C 1.1107(5) 0.6730(5) 0.1475(4) 0.080(2) Uani 1 1 d . . . H5S H 1.0929 0.7232 0.1235 0.096 Uiso 1 1 calc R . . H6S H 1.1696 0.6565 0.1323 0.096 Uiso 1 1 calc R . . B3 B 0.7600(3) 0.2324(3) 0.1966(2) 0.0201(8) Uani 1 1 d . . . H3 H 0.7357 0.2890 0.1711 0.024 Uiso 1 1 calc R . . Cl4S Cl 1.46744(11) 0.39966(10) 0.18356(9) 0.0680(4) Uani 1 1 d . . . C4 C 0.6367(3) -0.0669(2) -0.0731(2) 0.0284(9) Uani 1 1 d . . . H41 H 0.6150 -0.1046 -0.1085 0.034 Uiso 1 1 calc R . . B4 B 0.6750(3) 0.1544(3) 0.2159(2) 0.0226(8) Uani 1 1 d . . . H4 H 0.5985 0.1610 0.2041 0.027 Uiso 1 1 calc R . . Cl5S Cl 1.12745(18) 0.68751(17) 0.24278(13) 0.1164(9) Uani 1 1 d . . . C5 C 0.5869(3) 0.0030(2) -0.0676(2) 0.0233(8) Uani 1 1 d . . . B5 B 0.7295(3) 0.0617(3) 0.2110(2) 0.0215(8) Uani 1 1 d . . . H5 H 0.6893 0.0074 0.1957 0.026 Uiso 1 1 calc R . . Cl6S Cl 1.02776(19) 0.60452(14) 0.11891(13) 0.1078(8) Uani 1 1 d . . . C6 C 0.6233(2) 0.0576(2) -0.01417(18) 0.0186(7) Uani 1 1 d . . . B6 B 0.8499(3) 0.0795(2) 0.1884(2) 0.0187(8) Uani 1 1 d . . . H6 H 0.8847 0.0357 0.1572 0.022 Uiso 1 1 calc R . . C7 C 0.4995(3) 0.0193(2) -0.1119(2) 0.0269(8) Uani 1 1 d . . . H71 H 0.4746 -0.0172 -0.1475 0.032 Uiso 1 1 calc R . . B7 B 0.8577(3) 0.2272(3) 0.2724(2) 0.0205(8) Uani 1 1 d . . . H7 H 0.8948 0.2801 0.2962 0.025 Uiso 1 1 calc R . . C8 C 0.4529(3) 0.0862(2) -0.1029(2) 0.0260(8) Uani 1 1 d . . . H81 H 0.3956 0.0954 -0.1320 0.031 Uiso 1 1 calc R . . B8 B 0.7412(3) 0.2096(3) 0.2865(2) 0.0226(8) Uani 1 1 d . . . H8 H 0.7056 0.2537 0.3168 0.027 Uiso 1 1 calc R . . C9 C 0.4889(3) 0.1438(2) -0.0501(2) 0.0233(8) Uani 1 1 d . . . B9 B 0.7244(3) 0.1063(3) 0.2968(2) 0.0231(9) Uani 1 1 d . . . H9 H 0.6802 0.0819 0.3355 0.028 Uiso 1 1 calc R . . C10 C 0.4424(3) 0.2137(2) -0.0389(2) 0.0281(9) Uani 1 1 d . . . H101 H 0.3846 0.2248 -0.0665 0.034 Uiso 1 1 calc R . . B10 B 0.8285(3) 0.0596(3) 0.2789(2) 0.0219(8) Uani 1 1 d . . . H10 H 0.8514 0.0025 0.3041 0.026 Uiso 1 1 calc R . . C11 C 0.4820(3) 0.2662(3) 0.0127(2) 0.0310(9) Uani 1 1 d . . . H111 H 0.4523 0.3141 0.0198 0.037 Uiso 1 1 calc R . . B11 B 0.9141(3) 0.1325(2) 0.2679(2) 0.0203(8) Uani 1 1 d . . . H11 H 0.9883 0.1217 0.2886 0.024 Uiso 1 1 calc R . . C12 C 0.5670(3) 0.2475(2) 0.0548(2) 0.0267(8) Uani 1 1 d . . . H121 H 0.5934 0.2836 0.0902 0.032 Uiso 1 1 calc R . . B12 B 0.8327(3) 0.1486(2) 0.3289(2) 0.0221(8) Uani 1 1 d . . . H12 H 0.8567 0.1506 0.3883 0.027 Uiso 1 1 calc R . . N13 N 0.6115(2) 0.18084(18) 0.04672(17) 0.0209(6) Uani 1 1 d . . . C14 C 0.5741(2) 0.1293(2) -0.00528(18) 0.0185(7) Uani 1 1 d . . . P21 P 1.04031(7) 0.14690(6) 0.12980(5) 0.02068(19) Uani 1 1 d . . . P22 P 0.95461(7) 0.33488(5) 0.16495(5) 0.01891(18) Uani 1 1 d . . . C211 C 1.0224(3) 0.0642(3) 0.0677(3) 0.0370(11) Uani 1 1 d . . . H211 H 0.9786 0.0789 0.0254 0.056 Uiso 1 1 calc R . . H1B H 0.9978 0.0201 0.0921 0.056 Uiso 1 1 calc R . . H1C H 1.0810 0.0495 0.0523 0.056 Uiso 1 1 calc R . . C212 C 1.1216(3) 0.1061(3) 0.2039(2) 0.0360(10) Uani 1 1 d . . . H15A H 1.1788 0.0917 0.1859 0.054 Uiso 1 1 calc R . . H15B H 1.0946 0.0598 0.2231 0.054 Uiso 1 1 calc R . . H15C H 1.1347 0.1450 0.2422 0.054 Uiso 1 1 calc R . . C213 C 1.1128(3) 0.2117(2) 0.0842(2) 0.0223(7) Uani 1 1 d . . . C214 C 1.1869(3) 0.2523(2) 0.1231(2) 0.0283(9) Uani 1 1 d . . . H214 H 1.2009 0.2454 0.1738 0.034 Uiso 1 1 calc R . . C215 C 1.2405(3) 0.3032(3) 0.0873(3) 0.0428(12) Uani 1 1 d . . . H215 H 1.2901 0.3306 0.1140 0.051 Uiso 1 1 calc R . . C216 C 1.2210(4) 0.3136(3) 0.0127(3) 0.0449(12) Uani 1 1 d . . . H216 H 1.2573 0.3480 -0.0113 0.054 Uiso 1 1 calc R . . C217 C 1.1477(3) 0.2731(3) -0.0267(2) 0.0388(11) Uani 1 1 d . . . H217 H 1.1346 0.2798 -0.0774 0.047 Uiso 1 1 calc R . . C218 C 1.0939(3) 0.2225(3) 0.0087(2) 0.0302(9) Uani 1 1 d . . . H218 H 1.0442 0.1953 -0.0182 0.036 Uiso 1 1 calc R . . C221 C 0.8712(3) 0.4065(2) 0.1885(2) 0.0278(8) Uani 1 1 d . . . H21A H 0.8514 0.3921 0.2345 0.042 Uiso 1 1 calc R . . H21B H 0.8178 0.4076 0.1508 0.042 Uiso 1 1 calc R . . H21C H 0.8999 0.4581 0.1929 0.042 Uiso 1 1 calc R . . C222 C 0.9808(3) 0.3764(2) 0.0797(2) 0.0267(8) Uani 1 1 d . . . H23A H 0.9305 0.3647 0.0411 0.040 Uiso 1 1 calc R . . H23B H 1.0380 0.3537 0.0679 0.040 Uiso 1 1 calc R . . H23C H 0.9879 0.4329 0.0848 0.040 Uiso 1 1 calc R . . C223 C 1.0598(3) 0.3510(2) 0.2295(2) 0.0229(8) Uani 1 1 d . . . C224 C 1.1166(3) 0.4159(3) 0.2224(2) 0.0377(11) Uani 1 1 d . . . H65 H 1.0996 0.4522 0.1846 0.045 Uiso 1 1 calc R . . C225 C 1.1972(4) 0.4275(3) 0.2697(3) 0.0464(13) Uani 1 1 d . . . H54 H 1.2346 0.4715 0.2638 0.056 Uiso 1 1 calc R . . C226 C 1.2236(3) 0.3756(3) 0.3254(3) 0.0385(11) Uani 1 1 d . . . H47 H 1.2791 0.3837 0.3571 0.046 Uiso 1 1 calc R . . C227 C 1.1686(3) 0.3118(3) 0.3347(2) 0.0298(9) Uani 1 1 d . . . H60 H 1.1861 0.2766 0.3732 0.036 Uiso 1 1 calc R . . C228 C 1.0870(3) 0.2990(2) 0.2872(2) 0.0246(8) Uani 1 1 d . . . H18 H 1.0498 0.2551 0.2939 0.030 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 0.01616(12) 0.01900(13) 0.01506(12) -0.00282(10) 0.00109(10) -0.00038(10) Cl1S 0.1109(17) 0.0993(16) 0.0860(14) -0.0190(12) 0.0297(13) -0.0088(13) S1 0.0221(4) 0.0341(5) 0.0141(4) 0.0007(4) -0.0001(3) -0.0067(4) O1 0.0326(16) 0.066(2) 0.0190(14) -0.0105(14) 0.0030(12) -0.0087(16) N1 0.0182(14) 0.0236(15) 0.0179(14) -0.0015(12) 0.0038(12) -0.0005(12) C1S 0.100(6) 0.059(4) 0.056(4) 0.000(3) 0.011(4) 0.007(4) Pt2 0.01751(7) 0.01712(7) 0.01326(6) -0.00164(5) 0.00247(4) -0.00117(5) Cl2S 0.1244(18) 0.1108(17) 0.0675(12) 0.0311(12) 0.0155(12) -0.0100(14) O2 0.0347(16) 0.0341(17) 0.0333(16) 0.0116(13) -0.0088(13) -0.0064(13) C2 0.0189(18) 0.030(2) 0.030(2) -0.0076(16) 0.0044(15) 0.0018(15) C2S 0.046(3) 0.043(3) 0.048(3) 0.006(2) 0.005(2) 0.003(2) Cl3S 0.1157(15) 0.0518(8) 0.0487(8) 0.0008(7) 0.0246(9) -0.0095(9) C3 0.028(2) 0.028(2) 0.036(2) -0.0125(18) 0.0108(17) 0.0031(17) C3S 0.079(5) 0.077(5) 0.088(5) 0.022(4) 0.029(4) 0.009(4) B3 0.0225(19) 0.022(2) 0.0159(18) -0.0017(15) 0.0044(15) -0.0026(16) Cl4S 0.0600(9) 0.0754(11) 0.0616(9) 0.0122(8) -0.0154(7) -0.0126(8) C4 0.035(2) 0.028(2) 0.0229(19) -0.0095(16) 0.0069(16) -0.0059(17) B4 0.023(2) 0.027(2) 0.0184(19) -0.0022(16) 0.0053(16) -0.0029(17) Cl5S 0.1025(17) 0.152(2) 0.0835(15) 0.0294(15) -0.0273(13) -0.0277(16) C5 0.0255(19) 0.027(2) 0.0183(17) -0.0031(15) 0.0045(15) -0.0057(15) B5 0.024(2) 0.023(2) 0.0182(19) -0.0035(16) 0.0050(16) -0.0026(16) Cl6S 0.1272(19) 0.0847(14) 0.1002(16) 0.0231(12) -0.0240(14) -0.0076(13) C6 0.0204(17) 0.0236(18) 0.0127(15) -0.0008(13) 0.0051(13) -0.0049(14) B6 0.0191(18) 0.0200(19) 0.0167(18) -0.0012(15) 0.0008(15) -0.0014(15) C7 0.032(2) 0.031(2) 0.0162(17) -0.0014(15) -0.0004(15) -0.0127(17) B7 0.025(2) 0.023(2) 0.0133(18) -0.0029(15) 0.0031(15) -0.0048(17) C8 0.028(2) 0.027(2) 0.0201(18) 0.0083(15) -0.0055(15) -0.0065(16) B8 0.025(2) 0.026(2) 0.0179(19) -0.0038(16) 0.0073(16) -0.0037(17) C9 0.0248(18) 0.0253(19) 0.0193(18) 0.0071(15) 0.0010(15) -0.0022(15) B9 0.029(2) 0.023(2) 0.019(2) -0.0006(16) 0.0087(17) -0.0051(17) C10 0.0258(19) 0.031(2) 0.025(2) 0.0066(16) -0.0062(16) 0.0013(16) B10 0.026(2) 0.023(2) 0.0169(19) -0.0004(15) 0.0036(16) -0.0038(17) C11 0.033(2) 0.027(2) 0.031(2) 0.0018(17) -0.0012(18) 0.0083(18) B11 0.023(2) 0.023(2) 0.0154(18) -0.0006(15) 0.0020(15) -0.0034(16) C12 0.030(2) 0.0238(19) 0.025(2) -0.0032(15) -0.0018(16) 0.0032(16) B12 0.028(2) 0.023(2) 0.0151(18) -0.0018(15) 0.0025(16) -0.0061(17) N13 0.0192(15) 0.0223(15) 0.0207(15) -0.0011(12) 0.0012(12) 0.0013(12) C14 0.0195(17) 0.0222(18) 0.0139(16) 0.0016(13) 0.0025(13) -0.0033(14) P21 0.0209(4) 0.0200(5) 0.0222(5) -0.0018(4) 0.0068(4) 0.0012(4) P22 0.0229(5) 0.0170(4) 0.0171(4) -0.0012(3) 0.0038(4) -0.0010(4) C211 0.037(2) 0.026(2) 0.053(3) -0.017(2) 0.022(2) -0.0037(18) C212 0.033(2) 0.039(2) 0.038(2) 0.010(2) 0.0126(19) 0.016(2) C213 0.0198(17) 0.0244(19) 0.0244(18) -0.0029(15) 0.0087(14) 0.0031(14) C214 0.0252(19) 0.031(2) 0.030(2) -0.0011(17) 0.0079(16) -0.0007(16) C215 0.031(2) 0.041(3) 0.059(3) -0.008(2) 0.017(2) -0.009(2) C216 0.042(3) 0.042(3) 0.057(3) 0.008(2) 0.032(2) -0.004(2) C217 0.041(3) 0.051(3) 0.029(2) 0.009(2) 0.020(2) 0.011(2) C218 0.028(2) 0.039(2) 0.024(2) -0.0011(17) 0.0084(16) 0.0062(18) C221 0.035(2) 0.0159(18) 0.032(2) -0.0031(15) 0.0055(18) 0.0019(16) C222 0.036(2) 0.0206(19) 0.0239(19) 0.0038(15) 0.0070(17) -0.0003(16) C223 0.0237(18) 0.0235(19) 0.0212(18) -0.0052(14) 0.0024(15) -0.0022(15) C224 0.046(3) 0.034(2) 0.032(2) 0.0016(19) 0.000(2) -0.016(2) C225 0.045(3) 0.047(3) 0.044(3) -0.001(2) -0.004(2) -0.027(2) C226 0.029(2) 0.051(3) 0.033(2) -0.011(2) -0.0014(18) -0.008(2) C227 0.028(2) 0.038(2) 0.023(2) -0.0056(17) 0.0034(16) -0.0004(17) C228 0.0238(18) 0.0265(19) 0.0238(19) -0.0024(15) 0.0040(15) -0.0012(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 N13 2.180(3) . ? Pd1 N1 2.222(3) . ? Pd1 B4 2.236(4) . ? Pd1 B3 2.245(4) . ? Pd1 B5 2.257(4) . ? Pd1 B6 2.275(4) . ? Pd1 S1 2.4161(10) . ? Pd1 Pt2 2.7880(5) . ? Cl1S C1S 1.783(7) . ? S1 O1 1.474(3) . ? S1 O2 1.474(3) . ? S1 Pt2 2.4369(10) . ? N1 C2 1.331(5) . ? N1 C6 1.388(4) . ? C1S Cl2S 1.761(7) . ? C1S H2S 0.9900 . ? C1S H1S 0.9900 . ? Pt2 B7 2.265(4) . ? Pt2 B11 2.286(4) . ? Pt2 B3 2.343(4) . ? Pt2 B6 2.351(4) . ? Pt2 P22 2.3664(10) . ? Pt2 P21 2.3886(10) . ? C2 C3 1.420(5) . ? C2 H21 0.9500 . ? C2S Cl4S 1.773(5) . ? C2S Cl3S 1.772(6) . ? C2S H4S 0.9900 . ? C2S H3S 0.9900 . ? C3 C4 1.395(6) . ? C3 H31 0.9500 . ? C3S Cl6S 1.724(8) . ? C3S Cl5S 1.786(8) . ? C3S H5S 0.9900 . ? C3S H6S 0.9900 . ? B3 B8 1.788(6) . ? B3 B7 1.874(6) . ? B3 B4 1.901(6) . ? B3 H3 1.1200 . ? C4 C5 1.417(6) . ? C4 H41 0.9500 . ? B4 B9 1.789(6) . ? B4 B5 1.791(6) . ? B4 B8 1.799(6) . ? B4 H4 1.1200 . ? C5 C6 1.421(5) . ? C5 C7 1.456(5) . ? B5 B9 1.791(6) . ? B5 B10 1.794(6) . ? B5 B6 1.901(6) . ? B5 H5 1.1200 . ? C6 C14 1.451(5) . ? B6 B10 1.801(6) . ? B6 B11 1.883(6) . ? B6 H6 1.1200 . ? C7 C8 1.361(6) . ? C7 H71 0.9500 . ? B7 B12 1.787(6) . ? B7 B8 1.793(6) . ? B7 B11 1.835(6) . ? B7 H7 1.1200 . ? C8 C9 1.447(5) . ? C8 H81 0.9500 . ? B8 B12 1.800(6) . ? B8 B9 1.807(6) . ? B8 H8 1.1200 . ? C9 C10 1.413(6) . ? C9 C14 1.428(5) . ? B9 B12 1.776(6) . ? B9 B10 1.799(6) . ? B9 H9 1.1200 . ? C10 C11 1.389(6) . ? C10 H101 0.9500 . ? B10 B12 1.789(6) . ? B10 B11 1.807(6) . ? B10 H10 1.1200 . ? C11 C12 1.418(5) . ? C11 H111 0.9500 . ? B11 B12 1.787(6) . ? B11 H11 1.1200 . ? C12 N13 1.338(5) . ? C12 H121 0.9500 . ? B12 H12 1.1200 . ? N13 C14 1.373(5) . ? P21 C213 1.833(4) . ? P21 C211 1.833(4) . ? P21 C212 1.839(4) . ? P22 C221 1.834(4) . ? P22 C222 1.839(4) . ? P22 C223 1.846(4) . ? C211 H211 0.9800 . ? C211 H1B 0.9800 . ? C211 H1C 0.9800 . ? C212 H15A 0.9800 . ? C212 H15B 0.9800 . ? C212 H15C 0.9800 . ? C213 C214 1.409(5) . ? C213 C218 1.416(6) . ? C214 C215 1.407(6) . ? C214 H214 0.9500 . ? C215 C216 1.400(8) . ? C215 H215 0.9500 . ? C216 C217 1.401(8) . ? C216 H216 0.9500 . ? C217 C218 1.403(6) . ? C217 H217 0.9500 . ? C218 H218 0.9500 . ? C221 H21A 0.9800 . ? C221 H21B 0.9800 . ? C221 H21C 0.9800 . ? C222 H23A 0.9800 . ? C222 H23B 0.9800 . ? C222 H23C 0.9800 . ? C223 C224 1.410(6) . ? C223 C228 1.417(5) . ? C224 C225 1.391(6) . ? C224 H65 0.9500 . ? C225 C226 1.386(7) . ? C225 H54 0.9500 . ? C226 C227 1.388(6) . ? C226 H47 0.9500 . ? C227 C228 1.406(5) . ? C227 H60 0.9500 . ? C228 H18 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N13 Pd1 N1 77.22(11) . . ? N13 Pd1 B4 93.25(14) . . ? N1 Pd1 B4 128.42(14) . . ? N13 Pd1 B3 101.38(14) . . ? N1 Pd1 B3 178.13(13) . . ? B4 Pd1 B3 50.21(15) . . ? N13 Pd1 B5 122.84(14) . . ? N1 Pd1 B5 96.61(13) . . ? B4 Pd1 B5 46.98(16) . . ? B3 Pd1 B5 83.09(15) . . ? N13 Pd1 B6 171.77(13) . . ? N1 Pd1 B6 99.58(13) . . ? B4 Pd1 B6 82.77(16) . . ? B3 Pd1 B6 81.64(15) . . ? B5 Pd1 B6 49.58(15) . . ? N13 Pd1 S1 88.91(9) . . ? N1 Pd1 S1 93.85(8) . . ? B4 Pd1 S1 137.08(12) . . ? B3 Pd1 S1 87.35(11) . . ? B5 Pd1 S1 148.05(11) . . ? B6 Pd1 S1 98.92(11) . . ? N13 Pd1 Pt2 133.66(8) . . ? N1 Pd1 Pt2 127.68(8) . . ? B4 Pd1 Pt2 95.49(11) . . ? B3 Pd1 Pt2 54.19(11) . . ? B5 Pd1 Pt2 95.16(11) . . ? B6 Pd1 Pt2 54.19(10) . . ? S1 Pd1 Pt2 55.29(2) . . ? O1 S1 O2 113.7(2) . . ? O1 S1 Pd1 118.15(15) . . ? O2 S1 Pd1 113.49(14) . . ? O1 S1 Pt2 118.62(14) . . ? O2 S1 Pt2 116.04(13) . . ? Pd1 S1 Pt2 70.13(3) . . ? C2 N1 C6 118.4(3) . . ? C2 N1 Pd1 128.9(3) . . ? C6 N1 Pd1 112.4(2) . . ? Cl2S C1S Cl1S 111.9(4) . . ? Cl2S C1S H2S 109.2 . . ? Cl1S C1S H2S 109.2 . . ? Cl2S C1S H1S 109.2 . . ? Cl1S C1S H1S 109.2 . . ? H2S C1S H1S 107.9 . . ? B7 Pt2 B11 47.55(15) . . ? B7 Pt2 B3 47.96(15) . . ? B11 Pt2 B3 80.88(15) . . ? B7 Pt2 B6 80.42(15) . . ? B11 Pt2 B6 47.90(14) . . ? B3 Pt2 B6 78.02(15) . . ? B7 Pt2 P22 87.74(11) . . ? B11 Pt2 P22 121.70(10) . . ? B3 Pt2 P22 95.26(11) . . ? B6 Pt2 P22 168.05(10) . . ? B7 Pt2 P21 133.26(11) . . ? B11 Pt2 P21 93.24(11) . . ? B3 Pt2 P21 167.69(11) . . ? B6 Pt2 P21 90.00(11) . . ? P22 Pt2 P21 97.03(3) . . ? B7 Pt2 S1 132.41(11) . . ? B11 Pt2 S1 143.42(10) . . ? B3 Pt2 S1 84.71(10) . . ? B6 Pt2 S1 96.27(10) . . ? P22 Pt2 S1 92.89(3) . . ? P21 Pt2 S1 93.91(4) . . ? B7 Pt2 Pd1 90.33(11) . . ? B11 Pt2 Pd1 90.89(10) . . ? B3 Pt2 Pd1 50.99(10) . . ? B6 Pt2 Pd1 51.70(10) . . ? P22 Pt2 Pd1 130.60(2) . . ? P21 Pt2 Pd1 118.80(3) . . ? S1 Pt2 Pd1 54.59(2) . . ? N1 C2 C3 123.0(4) . . ? N1 C2 H21 118.5 . . ? C3 C2 H21 118.5 . . ? Cl4S C2S Cl3S 111.5(3) . . ? Cl4S C2S H4S 109.3 . . ? Cl3S C2S H4S 109.3 . . ? Cl4S C2S H3S 109.3 . . ? Cl3S C2S H3S 109.3 . . ? H4S C2S H3S 108.0 . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H31 120.5 . . ? C2 C3 H31 120.5 . . ? Cl6S C3S Cl5S 113.5(4) . . ? Cl6S C3S H5S 108.9 . . ? Cl5S C3S H5S 108.9 . . ? Cl6S C3S H6S 108.9 . . ? Cl5S C3S H6S 108.9 . . ? H5S C3S H6S 107.7 . . ? B8 B3 B7 58.6(2) . . ? B8 B3 B4 58.3(2) . . ? B7 B3 B4 106.0(3) . . ? B8 B3 Pd1 117.5(3) . . ? B7 B3 Pd1 121.7(3) . . ? B4 B3 Pd1 64.66(18) . . ? B8 B3 Pt2 117.5(3) . . ? B7 B3 Pt2 63.85(18) . . ? B4 B3 Pt2 123.1(3) . . ? Pd1 B3 Pt2 74.82(13) . . ? B8 B3 H3 120.8 . . ? B7 B3 H3 121.9 . . ? B4 B3 H3 121.1 . . ? Pd1 B3 H3 108.7 . . ? Pt2 B3 H3 108.4 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H41 120.2 . . ? C5 C4 H41 120.2 . . ? B9 B4 B5 60.0(2) . . ? B9 B4 B8 60.5(2) . . ? B5 B4 B8 107.9(3) . . ? B9 B4 B3 106.7(3) . . ? B5 B4 B3 107.9(3) . . ? B8 B4 B3 57.7(2) . . ? B9 B4 Pd1 120.4(3) . . ? B5 B4 Pd1 67.14(19) . . ? B8 B4 Pd1 117.5(3) . . ? B3 B4 Pd1 65.13(18) . . ? B9 B4 H4 119.5 . . ? B5 B4 H4 121.5 . . ? B8 B4 H4 121.1 . . ? B3 B4 H4 123.9 . . ? Pd1 B4 H4 110.2 . . ? C4 C5 C6 117.7(3) . . ? C4 C5 C7 123.0(3) . . ? C6 C5 C7 119.3(4) . . ? B9 B5 B4 59.9(2) . . ? B9 B5 B10 60.2(2) . . ? B4 B5 B10 107.8(3) . . ? B9 B5 B6 106.7(3) . . ? B4 B5 B6 107.7(3) . . ? B10 B5 B6 58.3(2) . . ? B9 B5 Pd1 119.2(3) . . ? B4 B5 Pd1 65.88(19) . . ? B10 B5 Pd1 118.1(2) . . ? B6 B5 Pd1 65.69(18) . . ? B9 B5 H5 120.0 . . ? B4 B5 H5 122.1 . . ? B10 B5 H5 120.7 . . ? B6 B5 H5 123.4 . . ? Pd1 B5 H5 110.6 . . ? N1 C6 C5 122.4(3) . . ? N1 C6 C14 117.7(3) . . ? C5 C6 C14 119.9(3) . . ? B10 B6 B11 58.7(2) . . ? B10 B6 B5 57.9(2) . . ? B11 B6 B5 106.3(3) . . ? B10 B6 Pd1 116.9(2) . . ? B11 B6 Pd1 121.5(2) . . ? B5 B6 Pd1 64.72(18) . . ? B10 B6 Pt2 117.6(2) . . ? B11 B6 Pt2 64.23(17) . . ? B5 B6 Pt2 123.0(2) . . ? Pd1 B6 Pt2 74.11(12) . . ? B10 B6 H6 121.0 . . ? B11 B6 H6 121.6 . . ? B5 B6 H6 121.0 . . ? Pd1 B6 H6 109.3 . . ? Pt2 B6 H6 108.6 . . ? C8 C7 C5 120.7(3) . . ? C8 C7 H71 119.6 . . ? C5 C7 H71 119.6 . . ? B12 B7 B8 60.4(2) . . ? B12 B7 B11 59.1(2) . . ? B8 B7 B11 107.6(3) . . ? B12 B7 B3 106.6(3) . . ? B8 B7 B3 58.3(2) . . ? B11 B7 B3 108.1(3) . . ? B12 B7 Pt2 120.6(3) . . ? B8 B7 Pt2 121.3(2) . . ? B11 B7 Pt2 66.81(18) . . ? B3 B7 Pt2 68.19(18) . . ? B12 B7 H7 120.4 . . ? B8 B7 H7 120.0 . . ? B11 B7 H7 122.7 . . ? B3 B7 H7 122.9 . . ? Pt2 B7 H7 107.9 . . ? C7 C8 C9 121.4(3) . . ? C7 C8 H81 119.3 . . ? C9 C8 H81 119.3 . . ? B3 B8 B7 63.1(2) . . ? B3 B8 B4 64.0(2) . . ? B7 B8 B4 114.2(3) . . ? B3 B8 B12 109.9(3) . . ? B7 B8 B12 59.7(2) . . ? B4 B8 B12 108.1(3) . . ? B3 B8 B9 111.0(3) . . ? B7 B8 B9 109.3(3) . . ? B4 B8 B9 59.5(2) . . ? B12 B8 B9 59.0(2) . . ? B3 B8 H8 118.3 . . ? B7 B8 H8 118.9 . . ? B4 B8 H8 119.1 . . ? B12 B8 H8 122.9 . . ? B9 B8 H8 122.0 . . ? C10 C9 C14 117.5(3) . . ? C10 C9 C8 123.1(3) . . ? C14 C9 C8 119.4(4) . . ? B12 B9 B4 109.6(3) . . ? B12 B9 B5 109.4(3) . . ? B4 B9 B5 60.0(2) . . ? B12 B9 B10 60.1(2) . . ? B4 B9 B10 107.7(3) . . ? B5 B9 B10 60.0(2) . . ? B12 B9 B8 60.3(2) . . ? B4 B9 B8 60.0(2) . . ? B5 B9 B8 107.5(3) . . ? B10 B9 B8 106.6(3) . . ? B12 B9 H9 120.4 . . ? B4 B9 H9 121.2 . . ? B5 B9 H9 121.4 . . ? B10 B9 H9 122.5 . . ? B8 B9 H9 122.5 . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H101 120.3 . . ? C9 C10 H101 120.3 . . ? B12 B10 B5 108.6(3) . . ? B12 B10 B9 59.3(2) . . ? B5 B10 B9 59.8(2) . . ? B12 B10 B6 109.4(3) . . ? B5 B10 B6 63.8(2) . . ? B9 B10 B6 110.8(3) . . ? B12 B10 B11 59.6(2) . . ? B5 B10 B11 114.4(3) . . ? B9 B10 B11 109.6(3) . . ? B6 B10 B11 62.9(2) . . ? B12 B10 H10 122.9 . . ? B5 B10 H10 118.8 . . ? B9 B10 H10 121.7 . . ? B6 B10 H10 118.7 . . ? B11 B10 H10 118.9 . . ? C10 C11 C12 119.3(4) . . ? C10 C11 H111 120.3 . . ? C12 C11 H111 120.3 . . ? B12 B11 B10 59.7(2) . . ? B12 B11 B7 59.1(2) . . ? B10 B11 B7 106.5(3) . . ? B12 B11 B6 106.0(3) . . ? B10 B11 B6 58.4(2) . . ? B7 B11 B6 106.6(3) . . ? B12 B11 Pt2 119.6(3) . . ? B10 B11 Pt2 120.6(2) . . ? B7 B11 Pt2 65.64(18) . . ? B6 B11 Pt2 67.87(18) . . ? B12 B11 H11 120.7 . . ? B10 B11 H11 120.4 . . ? B7 B11 H11 123.7 . . ? B6 B11 H11 123.3 . . ? Pt2 B11 H11 108.8 . . ? N13 C12 C11 122.5(4) . . ? N13 C12 H121 118.7 . . ? C11 C12 H121 118.7 . . ? B9 B12 B11 111.6(3) . . ? B9 B12 B7 110.9(3) . . ? B11 B12 B7 61.8(2) . . ? B9 B12 B10 60.6(2) . . ? B11 B12 B10 60.7(2) . . ? B7 B12 B10 109.4(3) . . ? B9 B12 B8 60.7(2) . . ? B11 B12 B8 109.4(3) . . ? B7 B12 B8 60.0(2) . . ? B10 B12 B8 107.3(3) . . ? B9 B12 H12 119.5 . . ? B11 B12 H12 119.6 . . ? B7 B12 H12 120.2 . . ? B10 B12 H12 122.0 . . ? B8 B12 H12 122.2 . . ? C12 N13 C14 118.6(3) . . ? C12 N13 Pd1 127.1(3) . . ? C14 N13 Pd1 114.0(2) . . ? N13 C14 C9 122.4(3) . . ? N13 C14 C6 118.3(3) . . ? C9 C14 C6 119.3(3) . . ? C213 P21 C211 102.48(19) . . ? C213 P21 C212 103.0(2) . . ? C211 P21 C212 101.8(2) . . ? C213 P21 Pt2 115.97(12) . . ? C211 P21 Pt2 116.05(15) . . ? C212 P21 Pt2 115.44(15) . . ? C221 P22 C222 100.19(19) . . ? C221 P22 C223 105.49(18) . . ? C222 P22 C223 104.68(19) . . ? C221 P22 Pt2 115.02(14) . . ? C222 P22 Pt2 117.86(13) . . ? C223 P22 Pt2 112.11(13) . . ? P21 C211 H211 109.5 . . ? P21 C211 H1B 109.5 . . ? H211 C211 H1B 109.5 . . ? P21 C211 H1C 109.5 . . ? H211 C211 H1C 109.5 . . ? H1B C211 H1C 109.5 . . ? P21 C212 H15A 109.5 . . ? P21 C212 H15B 109.5 . . ? H15A C212 H15B 109.5 . . ? P21 C212 H15C 109.5 . . ? H15A C212 H15C 109.5 . . ? H15B C212 H15C 109.5 . . ? C214 C213 C218 118.8(4) . . ? C214 C213 P21 121.2(3) . . ? C218 C213 P21 120.0(3) . . ? C215 C214 C213 120.3(4) . . ? C215 C214 H214 119.9 . . ? C213 C214 H214 119.9 . . ? C216 C215 C214 120.4(5) . . ? C216 C215 H215 119.8 . . ? C214 C215 H215 119.8 . . ? C215 C216 C217 119.8(4) . . ? C215 C216 H216 120.1 . . ? C217 C216 H216 120.1 . . ? C218 C217 C216 120.1(4) . . ? C218 C217 H217 120.0 . . ? C216 C217 H217 120.0 . . ? C217 C218 C213 120.6(4) . . ? C217 C218 H218 119.7 . . ? C213 C218 H218 119.7 . . ? P22 C221 H21A 109.5 . . ? P22 C221 H21B 109.5 . . ? H21A C221 H21B 109.5 . . ? P22 C221 H21C 109.5 . . ? H21A C221 H21C 109.5 . . ? H21B C221 H21C 109.5 . . ? P22 C222 H23A 109.5 . . ? P22 C222 H23B 109.5 . . ? H23A C222 H23B 109.5 . . ? P22 C222 H23C 109.5 . . ? H23A C222 H23C 109.5 . . ? H23B C222 H23C 109.5 . . ? C224 C223 C228 117.7(4) . . ? C224 C223 P22 120.6(3) . . ? C228 C223 P22 121.7(3) . . ? C225 C224 C223 121.0(4) . . ? C225 C224 H65 119.5 . . ? C223 C224 H65 119.5 . . ? C226 C225 C224 120.7(4) . . ? C226 C225 H54 119.7 . . ? C224 C225 H54 119.7 . . ? C225 C226 C227 119.8(4) . . ? C225 C226 H47 120.1 . . ? C227 C226 H47 120.1 . . ? C226 C227 C228 120.3(4) . . ? C226 C227 H60 119.9 . . ? C228 C227 H60 119.9 . . ? C227 C228 C223 120.5(4) . . ? C227 C228 H18 119.7 . . ? C223 C228 H18 119.7 . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 29.43 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.442 _refine_diff_density_min -1.308 _refine_diff_density_rms 0.133