# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_4a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H40 Cl N O P2 Pd Se' _chemical_formula_weight 881.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.4301(3) _cell_length_b 16.8918(6) _cell_length_c 43.8939(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.019(2) _cell_angle_gamma 90.00 _cell_volume 7722.6(4) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 4.03 _cell_measurement_theta_max 62.73 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3568 _exptl_absorpt_coefficient_mu 6.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5027 _exptl_absorpt_correction_T_max 0.8255 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 135477 _diffrn_reflns_av_R_equivalents 0.0896 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 59.99 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 11447 _reflns_number_gt 8889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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. CHECKCIF (Alert G) and PLATON indicated a non spacegroup translational symmetry element present (C) with 83 percent fit. Upon using MATCH in Olex clearly indicated, while the heavy atoms can overlay one on another, the phenyl groups do not show the symmetry element present. ; _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^)+(0.0314P)^2^+23.2377P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11447 _refine_ls_number_parameters 923 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1A Pd 0.66809(3) 0.913770(19) 0.637364(7) 0.01386(9) Uani 1 1 d . . . Pd1 Pd 0.83932(3) 0.595582(19) 0.357730(7) 0.01483(9) Uani 1 1 d . . . Se1 Se 0.68246(5) 0.66195(3) 0.387631(10) 0.01949(12) Uani 1 1 d . . . Se1A Se 0.81904(5) 0.83888(3) 0.609003(10) 0.01881(12) Uani 1 1 d . . . Cl1 Cl 0.98015(11) 0.52901(7) 0.32656(2) 0.0239(3) Uani 1 1 d . . . P2A P 0.83033(11) 0.91695(7) 0.67555(2) 0.0148(2) Uani 1 1 d . . . P2 P 0.67630(11) 0.58866(7) 0.31990(2) 0.0150(2) Uani 1 1 d . . . P1A P 0.50523(11) 0.89799(7) 0.59894(2) 0.0159(2) Uani 1 1 d . . . P1 P 0.99752(11) 0.60299(7) 0.39763(2) 0.0162(2) Uani 1 1 d . . . Cl1A Cl 0.53627(11) 1.00110(7) 0.66258(2) 0.0247(3) Uani 1 1 d . . . O60 O 0.3848(4) 0.7131(2) 0.73706(9) 0.0399(9) Uani 1 1 d . . . C37 C 0.4348(5) 0.5434(3) 0.33991(10) 0.0223(11) Uani 1 1 d . . . H37 H 0.4079 0.5962 0.3358 0.027 Uiso 1 1 calc R . . C35A C 1.0123(4) 0.8170(3) 0.70548(10) 0.0191(10) Uani 1 1 d . . . H35A H 1.0521 0.8643 0.7129 0.023 Uiso 1 1 calc R . . C18A C 0.3857(4) 0.8317(3) 0.61412(10) 0.0187(10) Uani 1 1 d . . . N1 N 0.5740(4) 0.4722(3) 0.46089(10) 0.0346(11) Uani 1 1 d . . . C24A C 0.7929(4) 0.9556(3) 0.71302(10) 0.0169(10) Uani 1 1 d . . . C34A C 1.0632(4) 0.7444(3) 0.71416(10) 0.0208(11) Uani 1 1 d . . . H34A H 1.1376 0.7420 0.7276 0.025 Uiso 1 1 calc R . . C10 C 0.9299(5) 0.5694(3) 0.45724(10) 0.0253(11) Uani 1 1 d . . . H10 H 0.9408 0.5155 0.4519 0.030 Uiso 1 1 calc R . . C39A C 1.1322(5) 1.0878(3) 0.64069(10) 0.0260(12) Uani 1 1 d . . . H39A H 1.1927 1.1239 0.6332 0.031 Uiso 1 1 calc R . . C37A C 1.0753(4) 0.9560(3) 0.65501(10) 0.0210(10) Uani 1 1 d . . . H37A H 1.0970 0.9014 0.6567 0.025 Uiso 1 1 calc R . . C24 C 0.7208(4) 0.5546(3) 0.28234(9) 0.0162(10) Uani 1 1 d . . . C25 C 0.7106(4) 0.4773(3) 0.27232(10) 0.0211(10) Uani 1 1 d . . . H25 H 0.6761 0.4381 0.2851 0.025 Uiso 1 1 calc R . . C36 C 0.5579(4) 0.5202(3) 0.33338(9) 0.0175(10) Uani 1 1 d . . . C29A C 0.6758(5) 0.9378(3) 0.72486(10) 0.0228(11) Uani 1 1 d . . . H29A H 0.6130 0.9098 0.7127 0.027 Uiso 1 1 calc R . . C30 C 0.5950(4) 0.6809(3) 0.30985(9) 0.0147(10) Uani 1 1 d . . . C31A C 0.8456(4) 0.7510(3) 0.67522(10) 0.0189(10) Uani 1 1 d . . . H31A H 0.7706 0.7529 0.6620 0.023 Uiso 1 1 calc R . . C29 C 0.7741(4) 0.6109(3) 0.26327(10) 0.0209(10) Uani 1 1 d . . . H29 H 0.7838 0.6641 0.2700 0.025 Uiso 1 1 calc R . . C25A C 0.8849(5) 0.9962(3) 0.73118(10) 0.0209(10) Uani 1 1 d . . . H25A H 0.9656 1.0089 0.7233 0.025 Uiso 1 1 calc R . . C10A C 0.5600(5) 0.9054(3) 0.53738(10) 0.0259(11) Uani 1 1 d . . . H10A H 0.5555 0.9611 0.5401 0.031 Uiso 1 1 calc R . . C22A C 0.2863(5) 0.7753(3) 0.65771(11) 0.0241(11) Uani 1 1 d . . . H22A H 0.2822 0.7703 0.6792 0.029 Uiso 1 1 calc R . . C27A C 0.7399(5) 1.0003(3) 0.77233(10) 0.0253(11) Uani 1 1 d . . . H27A H 0.7220 1.0156 0.7925 0.030 Uiso 1 1 calc R . . C38A C 1.1632(5) 1.0098(3) 0.64424(10) 0.0265(12) Uani 1 1 d . . . H38A H 1.2459 0.9919 0.6393 0.032 Uiso 1 1 calc R . . C14 C 1.0913(4) 0.3683(3) 0.40306(10) 0.0220(11) Uani 1 1 d . . . H14 H 1.0569 0.3198 0.3952 0.026 Uiso 1 1 calc R . . C21A C 0.1991(5) 0.7353(3) 0.63839(12) 0.0285(12) Uani 1 1 d . . . H21A H 0.1357 0.7025 0.6467 0.034 Uiso 1 1 calc R . . C31 C 0.6452(5) 0.7528(3) 0.32094(10) 0.0203(10) Uani 1 1 d . . . H31 H 0.7194 0.7530 0.3345 0.024 Uiso 1 1 calc R . . C36A C 0.9565(4) 0.9819(3) 0.66326(9) 0.0175(10) Uani 1 1 d . . . C26 C 0.7504(5) 0.4562(3) 0.24359(11) 0.0249(11) Uani 1 1 d . . . H26 H 0.7425 0.4028 0.2369 0.030 Uiso 1 1 calc R . . C17 C 1.1960(5) 0.5100(3) 0.42456(10) 0.0226(11) Uani 1 1 d . . . H17 H 1.2329 0.5586 0.4315 0.027 Uiso 1 1 calc R . . C15 C 1.1989(5) 0.3678(3) 0.42242(10) 0.0222(11) Uani 1 1 d . . . H15 H 1.2366 0.3189 0.4287 0.027 Uiso 1 1 calc R . . C18 C 1.1205(4) 0.6743(3) 0.38857(10) 0.0186(10) Uani 1 1 d . . . C41A C 0.9243(5) 1.0622(3) 0.65942(10) 0.0236(11) Uani 1 1 d . . . H41A H 0.8422 1.0807 0.6646 0.028 Uiso 1 1 calc R . . C34 C 0.4310(5) 0.7524(3) 0.28087(10) 0.0238(11) Uani 1 1 d . . . H34 H 0.3577 0.7525 0.2671 0.029 Uiso 1 1 calc R . . C33A C 1.0059(5) 0.6752(3) 0.70341(10) 0.0229(11) Uani 1 1 d . . . H33A H 1.0409 0.6253 0.7094 0.027 Uiso 1 1 calc R . . C23A C 0.3796(5) 0.8226(3) 0.64551(10) 0.0201(10) Uani 1 1 d . . . H23A H 0.4401 0.8493 0.6588 0.024 Uiso 1 1 calc R . . C3 C 0.5454(5) 0.5503(3) 0.46313(11) 0.0328(13) Uani 1 1 d . . . H3 H 0.5022 0.5674 0.4805 0.039 Uiso 1 1 calc R . . C12 C 1.0825(4) 0.5104(3) 0.40561(9) 0.0166(10) Uani 1 1 d . . . C11A C 0.5384(4) 0.8555(3) 0.56186(10) 0.0192(10) Uani 1 1 d . . . C40A C 1.0117(5) 1.1142(3) 0.64815(11) 0.0296(12) Uani 1 1 d . . . H40A H 0.9896 1.1684 0.6455 0.036 Uiso 1 1 calc R . . C11 C 0.9513(4) 0.6294(3) 0.43598(9) 0.0198(10) Uani 1 1 d . . . C30A C 0.9027(4) 0.8213(3) 0.68578(9) 0.0164(10) Uani 1 1 d . . . C13A C 0.4714(5) 1.0611(3) 0.59291(11) 0.0271(12) Uani 1 1 d . . . H13A H 0.5539 1.0647 0.6031 0.032 Uiso 1 1 calc R . . C28A C 0.6492(5) 0.9604(3) 0.75418(11) 0.0266(11) Uani 1 1 d . . . H28A H 0.5680 0.9483 0.7619 0.032 Uiso 1 1 calc R . . C32A C 0.8976(5) 0.6789(3) 0.68389(10) 0.0231(11) Uani 1 1 d . . . H32A H 0.8587 0.6314 0.6764 0.028 Uiso 1 1 calc R . . C32 C 0.5873(5) 0.8234(3) 0.31231(10) 0.0250(11) Uani 1 1 d . . . H32 H 0.6213 0.8719 0.3202 0.030 Uiso 1 1 calc R . . C27 C 0.8011(5) 0.5121(3) 0.22491(10) 0.0232(11) Uani 1 1 d . . . H27 H 0.8281 0.4975 0.2054 0.028 Uiso 1 1 calc R . . C6 C 0.9326(5) 0.7074(3) 0.44430(10) 0.0257(11) Uani 1 1 d . . . H6 H 0.9435 0.7485 0.4299 0.031 Uiso 1 1 calc R . . C33 C 0.4801(5) 0.8241(3) 0.29228(11) 0.0263(12) Uani 1 1 d . . . H33 H 0.4404 0.8727 0.2864 0.032 Uiso 1 1 calc R . . C5A C 0.8268(5) 0.9954(3) 0.58174(11) 0.0295(12) Uani 1 1 d . . . H5A H 0.7906 1.0149 0.5997 0.035 Uiso 1 1 calc R . . C39 C 0.3882(5) 0.4133(3) 0.35847(10) 0.0278(12) Uani 1 1 d . . . H39 H 0.3299 0.3769 0.3667 0.033 Uiso 1 1 calc R . . C22 C 1.2484(5) 0.7359(3) 0.35056(12) 0.0277(12) Uani 1 1 d . . . H22 H 1.2673 0.7427 0.3298 0.033 Uiso 1 1 calc R . . C41 C 0.5971(5) 0.4427(3) 0.34027(10) 0.0201(10) Uani 1 1 d . . . H41 H 0.6821 0.4265 0.3366 0.024 Uiso 1 1 calc R . . C35 C 0.4879(4) 0.6814(3) 0.28944(10) 0.0198(10) Uani 1 1 d . . . H35 H 0.4541 0.6331 0.2814 0.024 Uiso 1 1 calc R . . N1A N 0.9043(5) 1.0246(3) 0.53260(12) 0.0546(15) Uani 1 1 d . . . C2 C 0.5750(5) 0.6058(3) 0.44199(11) 0.0267(11) Uani 1 1 d . . . H2 H 0.5499 0.6594 0.4444 0.032 Uiso 1 1 calc R . . C16 C 1.2534(5) 0.4393(3) 0.43303(11) 0.0261(11) Uani 1 1 d . . . H16 H 1.3293 0.4390 0.4460 0.031 Uiso 1 1 calc R . . C12A C 0.4172(4) 0.9878(3) 0.58731(10) 0.0191(10) Uani 1 1 d . . . C6A C 0.5462(5) 0.7741(3) 0.55736(10) 0.0236(11) Uani 1 1 d . . . H6A H 0.5349 0.7393 0.5740 0.028 Uiso 1 1 calc R . . C28 C 0.8125(4) 0.5896(3) 0.23471(10) 0.0219(11) Uani 1 1 d . . . H28 H 0.8469 0.6284 0.2218 0.026 Uiso 1 1 calc R . . C13 C 1.0323(4) 0.4395(3) 0.39484(10) 0.0197(10) Uani 1 1 d . . . H13 H 0.9569 0.4394 0.3817 0.024 Uiso 1 1 calc R . . C8A C 0.5919(5) 0.7941(4) 0.50512(11) 0.0355(14) Uani 1 1 d . . . H8A H 0.6098 0.7730 0.4857 0.043 Uiso 1 1 calc R . . C38 C 0.3506(5) 0.4904(3) 0.35232(11) 0.0266(12) Uani 1 1 d . . . H38 H 0.2665 0.5072 0.3566 0.032 Uiso 1 1 calc R . . C1A C 0.8521(5) 0.9155(3) 0.57871(11) 0.0249(11) Uani 1 1 d . . . C9A C 0.5877(5) 0.8749(3) 0.50917(11) 0.0299(12) Uani 1 1 d . . . H9A H 0.6038 0.9095 0.4927 0.036 Uiso 1 1 calc R . . C23 C 1.1506(5) 0.6855(3) 0.35831(11) 0.0262(12) Uani 1 1 d . . . H23 H 1.1030 0.6579 0.3426 0.031 Uiso 1 1 calc R . . C4 C 0.6377(5) 0.4521(3) 0.43667(11) 0.0311(12) Uani 1 1 d . . . H4 H 0.6605 0.3980 0.4345 0.037 Uiso 1 1 calc R . . C7 C 0.8978(5) 0.7259(3) 0.47362(11) 0.0341(13) Uani 1 1 d . . . H7 H 0.8880 0.7797 0.4794 0.041 Uiso 1 1 calc R . . C20A C 0.2040(5) 0.7428(3) 0.60729(12) 0.0326(13) Uani 1 1 d . . . H20A H 0.1443 0.7152 0.5941 0.039 Uiso 1 1 calc R . . C2A C 0.9067(5) 0.8913(3) 0.55185(12) 0.0346(13) Uani 1 1 d . . . H2A H 0.9279 0.8372 0.5489 0.042 Uiso 1 1 calc R . . C19A C 0.2969(5) 0.7910(3) 0.59527(11) 0.0285(12) Uani 1 1 d . . . H19A H 0.2997 0.7963 0.5738 0.034 Uiso 1 1 calc R . . C7A C 0.5702(5) 0.7434(3) 0.52911(11) 0.0320(13) Uani 1 1 d . . . H7A H 0.5717 0.6877 0.5261 0.038 Uiso 1 1 calc R . . C26A C 0.8589(5) 1.0178(3) 0.76048(11) 0.0250(11) Uani 1 1 d . . . H26A H 0.9223 1.0449 0.7728 0.030 Uiso 1 1 calc R . . C61 C 0.4958(5) 0.7218(3) 0.74587(12) 0.0284(12) Uani 1 1 d . . . C5 C 0.6730(5) 0.5040(3) 0.41454(10) 0.0256(12) Uani 1 1 d . . . H5 H 0.7183 0.4854 0.3977 0.031 Uiso 1 1 calc R . . C1 C 0.6423(4) 0.5833(3) 0.41676(10) 0.0223(11) Uani 1 1 d . . . C40 C 0.5123(5) 0.3895(3) 0.35248(11) 0.0289(12) Uani 1 1 d . . . H40 H 0.5389 0.3367 0.3568 0.035 Uiso 1 1 calc R . . C16A C 0.2327(6) 1.0516(4) 0.56264(12) 0.0401(15) Uani 1 1 d . . . H16A H 0.1511 1.0485 0.5520 0.048 Uiso 1 1 calc R . . C17A C 0.2968(5) 0.9835(3) 0.57209(11) 0.0323(13) Uani 1 1 d . . . H17A H 0.2584 0.9332 0.5682 0.039 Uiso 1 1 calc R . . C4A C 0.8546(6) 1.0462(4) 0.55855(13) 0.0443(15) Uani 1 1 d . . . H4A H 0.8369 1.1008 0.5613 0.053 Uiso 1 1 calc R . . C19 C 1.1944(5) 0.7154(3) 0.41088(12) 0.0347(13) Uani 1 1 d . . . H19 H 1.1782 0.7083 0.4318 0.042 Uiso 1 1 calc R . . C14A C 0.4071(6) 1.1297(3) 0.58386(12) 0.0350(13) Uani 1 1 d . . . H14A H 0.4451 1.1799 0.5881 0.042 Uiso 1 1 calc R . . C9 C 0.8926(5) 0.5894(4) 0.48624(11) 0.0341(13) Uani 1 1 d . . . H9 H 0.8776 0.5488 0.5006 0.041 Uiso 1 1 calc R . . O60A O 0.1382(6) 0.7141(4) 0.53790(11) 0.094(2) Uani 1 1 d . . . C20 C 1.2904(6) 0.7664(3) 0.40288(12) 0.0377(14) Uani 1 1 d . . . H20 H 1.3378 0.7950 0.4183 0.045 Uiso 1 1 calc R . . C62 C 0.6014(6) 0.7261(4) 0.72426(13) 0.0417(14) Uani 1 1 d . . . H62D H 0.5654 0.7205 0.7033 0.063 Uiso 1 1 calc R . . H62E H 0.6630 0.6833 0.7288 0.063 Uiso 1 1 calc R . . H62F H 0.6451 0.7773 0.7265 0.063 Uiso 1 1 calc R . . C8 C 0.8775(5) 0.6665(4) 0.49427(11) 0.0376(14) Uani 1 1 d . . . H8 H 0.8529 0.6794 0.5142 0.045 Uiso 1 1 calc R . . C21 C 1.3183(6) 0.7762(3) 0.37310(12) 0.0360(13) Uani 1 1 d . . . H21 H 1.3857 0.8108 0.3679 0.043 Uiso 1 1 calc R . . C15A C 0.2897(6) 1.1252(3) 0.56895(12) 0.0376(15) Uani 1 1 d . . . H15A H 0.2461 1.1723 0.5628 0.045 Uiso 1 1 calc R . . C63 C 0.5329(7) 0.7293(4) 0.77869(14) 0.0541(17) Uani 1 1 d . . . H63D H 0.5725 0.7811 0.7826 0.081 Uiso 1 1 calc R . . H63E H 0.5943 0.6875 0.7847 0.081 Uiso 1 1 calc R . . H63F H 0.4564 0.7242 0.7906 0.081 Uiso 1 1 calc R . . C3A C 0.9294(6) 0.9460(4) 0.52983(13) 0.0446(16) Uani 1 1 d . . . H3A H 0.9648 0.9280 0.5115 0.053 Uiso 1 1 calc R . . C61A C 0.1938(6) 0.7254(4) 0.51491(14) 0.0512(17) Uani 1 1 d . . . C62A C 0.2204(8) 0.8064(4) 0.50365(17) 0.067(2) Uani 1 1 d . . . H62A H 0.3124 0.8178 0.5067 0.100 Uiso 1 1 calc R . . H62B H 0.1715 0.8451 0.5150 0.100 Uiso 1 1 calc R . . H62C H 0.1950 0.8099 0.4819 0.100 Uiso 1 1 calc R . . C63A C 0.2394(8) 0.6588(4) 0.49625(16) 0.071(2) Uani 1 1 d . . . H63A H 0.1695 0.6410 0.4821 0.106 Uiso 1 1 calc R . . H63B H 0.2669 0.6149 0.5097 0.106 Uiso 1 1 calc R . . H63C H 0.3119 0.6765 0.4847 0.106 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 Pd1A 0.01239(18) 0.01417(18) 0.01505(16) -0.00237(13) 0.00110(13) 0.00185(13) Pd1 0.01520(18) 0.01653(18) 0.01276(16) -0.00155(13) 0.00073(13) 0.00365(14) Se1 0.0211(3) 0.0199(3) 0.0176(2) -0.0028(2) 0.00244(19) 0.0051(2) Se1A 0.0189(3) 0.0186(3) 0.0192(2) -0.0023(2) 0.0031(2) 0.0044(2) Cl1 0.0221(6) 0.0314(7) 0.0182(5) -0.0061(5) 0.0013(4) 0.0107(5) P2A 0.0134(6) 0.0151(6) 0.0158(5) -0.0016(5) 0.0007(4) 0.0005(5) P2 0.0160(6) 0.0142(6) 0.0147(5) -0.0020(5) 0.0004(4) 0.0027(5) P1A 0.0150(6) 0.0173(6) 0.0154(5) -0.0005(5) 0.0003(4) 0.0016(5) P1 0.0182(6) 0.0162(6) 0.0140(5) -0.0006(5) -0.0007(4) 0.0034(5) Cl1A 0.0233(6) 0.0268(6) 0.0239(6) -0.0087(5) -0.0002(5) 0.0095(5) O60 0.030(2) 0.037(2) 0.052(2) -0.0062(19) 0.0007(18) -0.0040(18) C37 0.025(3) 0.024(3) 0.018(2) 0.002(2) -0.001(2) -0.002(2) C35A 0.017(3) 0.019(3) 0.021(2) -0.001(2) 0.0022(19) -0.002(2) C18A 0.009(2) 0.020(3) 0.027(2) -0.003(2) -0.0005(19) 0.002(2) N1 0.035(3) 0.039(3) 0.031(2) 0.001(2) 0.009(2) 0.001(2) C24A 0.013(2) 0.019(2) 0.018(2) 0.0002(19) -0.0029(18) 0.0038(19) C34A 0.017(3) 0.027(3) 0.018(2) 0.007(2) 0.0010(19) 0.002(2) C10 0.023(3) 0.033(3) 0.020(2) 0.005(2) -0.001(2) 0.003(2) C39A 0.028(3) 0.029(3) 0.022(2) -0.001(2) 0.009(2) -0.015(2) C37A 0.021(3) 0.021(3) 0.021(2) 0.002(2) 0.000(2) 0.002(2) C24 0.014(2) 0.017(3) 0.017(2) -0.0039(19) -0.0035(18) 0.0052(19) C25 0.019(3) 0.023(3) 0.021(2) 0.001(2) 0.0016(19) 0.004(2) C36 0.021(3) 0.020(3) 0.011(2) -0.0030(19) -0.0015(18) 0.001(2) C29A 0.021(3) 0.025(3) 0.022(2) -0.001(2) 0.001(2) -0.001(2) C30 0.015(2) 0.016(2) 0.013(2) 0.0020(18) 0.0034(18) 0.0039(19) C31A 0.016(2) 0.023(3) 0.018(2) 0.001(2) -0.0008(18) 0.000(2) C29 0.019(3) 0.019(2) 0.025(2) -0.001(2) 0.001(2) 0.000(2) C25A 0.020(3) 0.018(3) 0.024(2) 0.000(2) -0.002(2) -0.001(2) C10A 0.026(3) 0.026(3) 0.026(3) 0.005(2) 0.002(2) 0.005(2) C22A 0.026(3) 0.023(3) 0.024(2) 0.002(2) 0.008(2) 0.001(2) C27A 0.029(3) 0.028(3) 0.019(2) -0.004(2) -0.002(2) 0.007(2) C38A 0.018(3) 0.038(3) 0.025(3) -0.002(2) 0.007(2) -0.001(2) C14 0.015(3) 0.023(3) 0.028(3) 0.000(2) 0.003(2) 0.001(2) C21A 0.026(3) 0.022(3) 0.039(3) -0.003(2) 0.010(2) 0.001(2) C31 0.026(3) 0.021(3) 0.014(2) -0.0010(19) 0.0023(19) 0.000(2) C36A 0.025(3) 0.015(2) 0.013(2) -0.0018(18) 0.0023(19) -0.003(2) C26 0.023(3) 0.023(3) 0.029(3) -0.011(2) 0.000(2) 0.000(2) C17 0.020(3) 0.020(3) 0.027(3) -0.008(2) -0.002(2) 0.003(2) C15 0.024(3) 0.016(3) 0.027(3) 0.003(2) 0.005(2) 0.007(2) C18 0.018(3) 0.013(2) 0.025(2) 0.000(2) -0.0010(19) 0.008(2) C41A 0.021(3) 0.024(3) 0.026(2) 0.000(2) 0.003(2) 0.002(2) C34 0.019(3) 0.031(3) 0.021(2) 0.007(2) 0.004(2) 0.004(2) C33A 0.025(3) 0.019(3) 0.024(2) 0.006(2) 0.005(2) 0.006(2) C23A 0.022(3) 0.018(3) 0.021(2) -0.002(2) 0.0001(19) 0.000(2) C3 0.032(3) 0.043(4) 0.024(3) -0.002(2) 0.009(2) 0.005(3) C12 0.015(2) 0.019(2) 0.016(2) 0.0012(19) 0.0023(18) 0.006(2) C11A 0.015(2) 0.024(3) 0.019(2) 0.000(2) -0.0010(19) 0.004(2) C40A 0.044(3) 0.015(3) 0.030(3) 0.000(2) 0.008(2) -0.004(2) C11 0.018(3) 0.028(3) 0.013(2) -0.002(2) -0.0032(18) 0.006(2) C30A 0.016(2) 0.019(3) 0.015(2) 0.0029(19) 0.0036(18) 0.000(2) C13A 0.025(3) 0.024(3) 0.032(3) 0.002(2) 0.003(2) 0.006(2) C28A 0.024(3) 0.031(3) 0.025(3) 0.001(2) 0.005(2) 0.003(2) C32A 0.026(3) 0.021(3) 0.023(2) -0.001(2) 0.003(2) -0.004(2) C32 0.036(3) 0.015(3) 0.024(2) 0.001(2) 0.005(2) 0.002(2) C27 0.021(3) 0.032(3) 0.017(2) -0.006(2) 0.0027(19) 0.006(2) C6 0.026(3) 0.031(3) 0.019(2) -0.001(2) -0.003(2) 0.010(2) C33 0.036(3) 0.017(3) 0.026(3) 0.006(2) 0.008(2) 0.012(2) C5A 0.035(3) 0.026(3) 0.029(3) 0.005(2) 0.013(2) 0.005(2) C39 0.030(3) 0.037(3) 0.016(2) -0.003(2) 0.003(2) -0.015(2) C22 0.028(3) 0.023(3) 0.033(3) 0.007(2) 0.011(2) 0.005(2) C41 0.019(3) 0.018(3) 0.023(2) -0.001(2) 0.003(2) 0.000(2) C35 0.019(3) 0.020(3) 0.021(2) 0.001(2) 0.0030(19) 0.001(2) N1A 0.065(4) 0.051(3) 0.051(3) 0.016(3) 0.035(3) 0.014(3) C2 0.028(3) 0.027(3) 0.025(3) -0.002(2) 0.004(2) 0.004(2) C16 0.022(3) 0.032(3) 0.023(2) -0.002(2) -0.004(2) 0.009(2) C12A 0.021(3) 0.021(3) 0.016(2) -0.0011(19) 0.0036(19) 0.005(2) C6A 0.027(3) 0.023(3) 0.020(2) 0.000(2) -0.004(2) 0.006(2) C28 0.021(3) 0.025(3) 0.021(2) 0.005(2) 0.0037(19) 0.003(2) C13 0.016(2) 0.020(3) 0.023(2) -0.002(2) -0.0024(19) -0.003(2) C8A 0.032(3) 0.056(4) 0.019(3) -0.010(3) 0.001(2) 0.012(3) C38 0.018(3) 0.038(3) 0.024(2) -0.005(2) 0.003(2) 0.001(2) C1A 0.017(3) 0.030(3) 0.028(3) 0.004(2) 0.004(2) 0.000(2) C9A 0.032(3) 0.037(3) 0.022(3) 0.003(2) 0.009(2) 0.006(2) C23 0.031(3) 0.023(3) 0.024(3) -0.002(2) 0.003(2) 0.009(2) C4 0.040(3) 0.028(3) 0.025(3) 0.000(2) 0.001(2) 0.002(3) C7 0.035(3) 0.038(3) 0.029(3) -0.010(3) -0.003(2) 0.021(3) C20A 0.027(3) 0.038(3) 0.032(3) -0.008(2) 0.001(2) -0.016(3) C2A 0.040(3) 0.031(3) 0.034(3) 0.001(2) 0.015(2) 0.009(3) C19A 0.023(3) 0.043(3) 0.020(2) -0.001(2) 0.000(2) -0.007(2) C7A 0.031(3) 0.035(3) 0.029(3) -0.012(2) -0.004(2) 0.011(2) C26A 0.025(3) 0.024(3) 0.025(3) -0.002(2) -0.006(2) 0.003(2) C61 0.031(3) 0.016(3) 0.038(3) 0.002(2) 0.001(2) -0.001(2) C5 0.029(3) 0.030(3) 0.019(2) -0.002(2) 0.003(2) 0.000(2) C1 0.016(3) 0.028(3) 0.023(2) -0.005(2) -0.0007(19) 0.001(2) C40 0.038(3) 0.019(3) 0.029(3) 0.001(2) 0.006(2) -0.006(2) C16A 0.031(3) 0.056(4) 0.032(3) -0.001(3) -0.010(2) 0.024(3) C17A 0.024(3) 0.043(3) 0.030(3) -0.004(3) -0.004(2) 0.004(3) C4A 0.053(4) 0.032(3) 0.050(4) 0.011(3) 0.019(3) 0.008(3) C19 0.035(3) 0.042(3) 0.028(3) -0.001(2) 0.003(2) -0.007(3) C14A 0.040(4) 0.024(3) 0.042(3) 0.005(2) 0.009(3) 0.012(3) C9 0.030(3) 0.051(4) 0.022(3) 0.010(3) 0.004(2) 0.010(3) O60A 0.087(4) 0.158(6) 0.036(3) -0.014(3) 0.004(3) -0.037(4) C20 0.042(4) 0.034(3) 0.037(3) -0.011(3) 0.001(3) -0.013(3) C62 0.040(4) 0.036(3) 0.050(4) -0.001(3) 0.005(3) -0.003(3) C8 0.037(3) 0.059(4) 0.017(3) 0.000(3) 0.002(2) 0.017(3) C21 0.037(3) 0.033(3) 0.040(3) -0.010(3) 0.012(3) -0.003(3) C15A 0.049(4) 0.038(4) 0.026(3) 0.007(2) 0.010(3) 0.030(3) C63 0.055(4) 0.063(5) 0.043(4) 0.006(3) -0.002(3) 0.008(4) C3A 0.049(4) 0.050(4) 0.037(3) 0.008(3) 0.026(3) 0.011(3) C61A 0.047(4) 0.069(5) 0.035(4) -0.005(3) -0.018(3) 0.003(3) C62A 0.067(5) 0.055(5) 0.077(5) 0.010(4) -0.021(4) 0.012(4) C63A 0.091(6) 0.054(5) 0.063(4) -0.018(4) -0.043(4) 0.025(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1A P2A 2.3189(12) . ? Pd1A Cl1A 2.3349(11) . ? Pd1A P1A 2.3451(12) . ? Pd1A Se1A 2.4157(5) . ? Pd1 P2 2.3161(12) . ? Pd1 P1 2.3454(12) . ? Pd1 Cl1 2.3462(11) . ? Pd1 Se1 2.4254(5) . ? Se1 C1 1.906(5) . ? Se1A C1A 1.900(5) . ? P2A C36A 1.816(5) . ? P2A C30A 1.829(5) . ? P2A C24A 1.830(4) . ? P2 C36 1.814(5) . ? P2 C30 1.817(4) . ? P2 C24 1.829(4) . ? P1A C18A 1.828(5) . ? P1A C11A 1.828(4) . ? P1A C12A 1.832(5) . ? P1 C18 1.819(5) . ? P1 C12 1.822(4) . ? P1 C11 1.831(4) . ? O60 C61 1.210(6) . ? C37 C38 1.385(7) . ? C37 C36 1.387(7) . ? C37 H37 0.9500 . ? C35A C34A 1.381(7) . ? C35A C30A 1.399(6) . ? C35A H35A 0.9500 . ? C18A C19A 1.391(7) . ? C18A C23A 1.391(6) . ? N1 C4 1.327(6) . ? N1 C3 1.357(7) . ? C24A C29A 1.385(6) . ? C24A C25A 1.395(6) . ? C34A C33A 1.385(7) . ? C34A H34A 0.9500 . ? C10 C9 1.392(7) . ? C10 C11 1.403(7) . ? C10 H10 0.9500 . ? C39A C38A 1.364(7) . ? C39A C40A 1.388(7) . ? C39A H39A 0.9500 . ? C37A C36A 1.381(7) . ? C37A C38A 1.392(7) . ? C37A H37A 0.9500 . ? C24 C25 1.380(6) . ? C24 C29 1.401(6) . ? C25 C26 1.395(6) . ? C25 H25 0.9500 . ? C36 C41 1.399(6) . ? C29A C28A 1.384(7) . ? C29A H29A 0.9500 . ? C30 C35 1.395(6) . ? C30 C31 1.399(6) . ? C31A C32A 1.379(7) . ? C31A C30A 1.396(6) . ? C31A H31A 0.9500 . ? C29 C28 1.384(6) . ? C29 H29 0.9500 . ? C25A C26A 1.378(6) . ? C25A H25A 0.9500 . ? C10A C9A 1.386(7) . ? C10A C11A 1.393(6) . ? C10A H10A 0.9500 . ? C22A C21A 1.386(7) . ? C22A C23A 1.388(7) . ? C22A H22A 0.9500 . ? C27A C28A 1.380(7) . ? C27A C26A 1.403(7) . ? C27A H27A 0.9500 . ? C38A H38A 0.9500 . ? C14 C15 1.372(7) . ? C14 C13 1.390(7) . ? C14 H14 0.9500 . ? C21A C20A 1.374(7) . ? C21A H21A 0.9500 . ? C31 C32 1.381(7) . ? C31 H31 0.9500 . ? C36A C41A 1.406(7) . ? C26 C27 1.374(7) . ? C26 H26 0.9500 . ? C17 C16 1.379(7) . ? C17 C12 1.410(6) . ? C17 H17 0.9500 . ? C15 C16 1.404(7) . ? C15 H15 0.9500 . ? C18 C23 1.394(7) . ? C18 C19 1.399(7) . ? C41A C40A 1.377(7) . ? C41A H41A 0.9500 . ? C34 C35 1.381(7) . ? C34 C33 1.397(7) . ? C34 H34 0.9500 . ? C33A C32A 1.383(7) . ? C33A H33A 0.9500 . ? C23A H23A 0.9500 . ? C3 C2 1.366(7) . ? C3 H3 0.9500 . ? C12 C13 1.380(6) . ? C11A C6A 1.392(7) . ? C40A H40A 0.9500 . ? C11 C6 1.383(7) . ? C13A C12A 1.377(7) . ? C13A C14A 1.386(7) . ? C13A H13A 0.9500 . ? C28A H28A 0.9500 . ? C32A H32A 0.9500 . ? C32 C33 1.386(7) . ? C32 H32 0.9500 . ? C27 C28 1.382(7) . ? C27 H27 0.9500 . ? C6 C7 1.391(7) . ? C6 H6 0.9500 . ? C33 H33 0.9500 . ? C5A C4A 1.374(7) . ? C5A C1A 1.383(7) . ? C5A H5A 0.9500 . ? C39 C38 1.383(7) . ? C39 C40 1.394(7) . ? C39 H39 0.9500 . ? C22 C21 1.377(8) . ? C22 C23 1.385(7) . ? C22 H22 0.9500 . ? C41 C40 1.389(7) . ? C41 H41 0.9500 . ? C35 H35 0.9500 . ? N1A C4A 1.327(7) . ? N1A C3A 1.361(8) . ? C2 C1 1.395(6) . ? C2 H2 0.9500 . ? C16 H16 0.9500 . ? C12A C17A 1.393(7) . ? C6A C7A 1.380(7) . ? C6A H6A 0.9500 . ? C28 H28 0.9500 . ? C13 H13 0.9500 . ? C8A C9A 1.378(8) . ? C8A C7A 1.385(8) . ? C8A H8A 0.9500 . ? C38 H38 0.9500 . ? C1A C2A 1.397(7) . ? C9A H9A 0.9500 . ? C23 H23 0.9500 . ? C4 C5 1.373(7) . ? C4 H4 0.9500 . ? C7 C8 1.375(8) . ? C7 H7 0.9500 . ? C20A C19A 1.391(7) . ? C20A H20A 0.9500 . ? C2A C3A 1.366(8) . ? C2A H2A 0.9500 . ? C19A H19A 0.9500 . ? C7A H7A 0.9500 . ? C26A H26A 0.9500 . ? C61 C63 1.477(8) . ? C61 C62 1.493(7) . ? C5 C1 1.382(7) . ? C5 H5 0.9500 . ? C40 H40 0.9500 . ? C16A C17A 1.385(8) . ? C16A C15A 1.398(9) . ? C16A H16A 0.9500 . ? C17A H17A 0.9500 . ? C4A H4A 0.9500 . ? C19 C20 1.380(8) . ? C19 H19 0.9500 . ? C14A C15A 1.360(8) . ? C14A H14A 0.9500 . ? C9 C8 1.361(8) . ? C9 H9 0.9500 . ? O60A C61A 1.205(8) . ? C20 C21 1.364(7) . ? C20 H20 0.9500 . ? C62 H62D 0.9800 . ? C62 H62E 0.9800 . ? C62 H62F 0.9800 . ? C8 H8 0.9500 . ? C21 H21 0.9500 . ? C15A H15A 0.9500 . ? C63 H63D 0.9800 . ? C63 H63E 0.9800 . ? C63 H63F 0.9800 . ? C3A H3A 0.9500 . ? C61A C63A 1.484(9) . ? C61A C62A 1.487(10) . ? C62A H62A 0.9800 . ? C62A H62B 0.9800 . ? C62A H62C 0.9800 . ? C63A H63A 0.9800 . ? C63A H63B 0.9800 . ? C63A H63C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2A Pd1A Cl1A 93.91(4) . . ? P2A Pd1A P1A 174.80(4) . . ? Cl1A Pd1A P1A 89.46(4) . . ? P2A Pd1A Se1A 85.07(3) . . ? Cl1A Pd1A Se1A 172.39(4) . . ? P1A Pd1A Se1A 92.11(3) . . ? P2 Pd1 P1 177.48(4) . . ? P2 Pd1 Cl1 90.94(4) . . ? P1 Pd1 Cl1 91.35(4) . . ? P2 Pd1 Se1 85.44(3) . . ? P1 Pd1 Se1 92.25(3) . . ? Cl1 Pd1 Se1 176.29(3) . . ? C1 Se1 Pd1 102.66(14) . . ? C1A Se1A Pd1A 98.69(15) . . ? C36A P2A C30A 108.1(2) . . ? C36A P2A C24A 104.1(2) . . ? C30A P2A C24A 101.5(2) . . ? C36A P2A Pd1A 108.16(15) . . ? C30A P2A Pd1A 115.64(15) . . ? C24A P2A Pd1A 118.41(15) . . ? C36 P2 C30 108.0(2) . . ? C36 P2 C24 107.6(2) . . ? C30 P2 C24 100.86(19) . . ? C36 P2 Pd1 106.58(14) . . ? C30 P2 Pd1 116.51(15) . . ? C24 P2 Pd1 116.76(15) . . ? C18A P1A C11A 104.4(2) . . ? C18A P1A C12A 105.5(2) . . ? C11A P1A C12A 101.1(2) . . ? C18A P1A Pd1A 106.84(15) . . ? C11A P1A Pd1A 121.39(15) . . ? C12A P1A Pd1A 116.07(16) . . ? C18 P1 C12 105.6(2) . . ? C18 P1 C11 105.2(2) . . ? C12 P1 C11 100.5(2) . . ? C18 P1 Pd1 110.40(15) . . ? C12 P1 Pd1 114.44(15) . . ? C11 P1 Pd1 119.40(15) . . ? C38 C37 C36 120.8(5) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? C34A C35A C30A 120.4(4) . . ? C34A C35A H35A 119.8 . . ? C30A C35A H35A 119.8 . . ? C19A C18A C23A 118.1(4) . . ? C19A C18A P1A 122.1(4) . . ? C23A C18A P1A 119.7(4) . . ? C4 N1 C3 115.3(4) . . ? C29A C24A C25A 119.0(4) . . ? C29A C24A P2A 119.6(3) . . ? C25A C24A P2A 121.1(3) . . ? C35A C34A C33A 120.2(4) . . ? C35A C34A H34A 119.9 . . ? C33A C34A H34A 119.9 . . ? C9 C10 C11 119.7(5) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C38A C39A C40A 119.7(4) . . ? C38A C39A H39A 120.1 . . ? C40A C39A H39A 120.1 . . ? C36A C37A C38A 119.9(4) . . ? C36A C37A H37A 120.0 . . ? C38A C37A H37A 120.0 . . ? C25 C24 C29 118.6(4) . . ? C25 C24 P2 124.5(3) . . ? C29 C24 P2 116.9(3) . . ? C24 C25 C26 120.5(4) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C37 C36 C41 118.9(4) . . ? C37 C36 P2 122.7(4) . . ? C41 C36 P2 118.1(3) . . ? C28A C29A C24A 120.9(5) . . ? C28A C29A H29A 119.5 . . ? C24A C29A H29A 119.5 . . ? C35 C30 C31 119.4(4) . . ? C35 C30 P2 120.6(3) . . ? C31 C30 P2 119.9(3) . . ? C32A C31A C30A 120.3(4) . . ? C32A C31A H31A 119.8 . . ? C30A C31A H31A 119.8 . . ? C28 C29 C24 120.5(4) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C26A C25A C24A 120.0(4) . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C9A C10A C11A 120.9(5) . . ? C9A C10A H10A 119.5 . . ? C11A C10A H10A 119.5 . . ? C21A C22A C23A 119.7(4) . . ? C21A C22A H22A 120.2 . . ? C23A C22A H22A 120.2 . . ? C28A C27A C26A 118.8(4) . . ? C28A C27A H27A 120.6 . . ? C26A C27A H27A 120.6 . . ? C39A C38A C37A 120.9(5) . . ? C39A C38A H38A 119.6 . . ? C37A C38A H38A 119.6 . . ? C15 C14 C13 120.1(5) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C20A C21A C22A 120.4(5) . . ? C20A C21A H21A 119.8 . . ? C22A C21A H21A 119.8 . . ? C32 C31 C30 120.2(4) . . ? C32 C31 H31 119.9 . . ? C30 C31 H31 119.9 . . ? C37A C36A C41A 119.1(4) . . ? C37A C36A P2A 124.1(4) . . ? C41A C36A P2A 116.5(4) . . ? C27 C26 C25 120.4(4) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C16 C17 C12 120.1(5) . . ? C16 C17 H17 119.9 . . ? C12 C17 H17 119.9 . . ? C14 C15 C16 120.3(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C23 C18 C19 117.1(5) . . ? C23 C18 P1 119.7(4) . . ? C19 C18 P1 123.0(4) . . ? C40A C41A C36A 120.0(5) . . ? C40A C41A H41A 120.0 . . ? C36A C41A H41A 120.0 . . ? C35 C34 C33 120.7(5) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C32A C33A C34A 119.7(4) . . ? C32A C33A H33A 120.1 . . ? C34A C33A H33A 120.1 . . ? C22A C23A C18A 121.0(4) . . ? C22A C23A H23A 119.5 . . ? C18A C23A H23A 119.5 . . ? N1 C3 C2 124.1(5) . . ? N1 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? C13 C12 C17 119.3(4) . . ? C13 C12 P1 120.4(3) . . ? C17 C12 P1 120.1(4) . . ? C6A C11A C10A 118.3(4) . . ? C6A C11A P1A 121.9(3) . . ? C10A C11A P1A 119.7(4) . . ? C41A C40A C39A 120.3(5) . . ? C41A C40A H40A 119.8 . . ? C39A C40A H40A 119.8 . . ? C6 C11 C10 118.8(4) . . ? C6 C11 P1 121.5(4) . . ? C10 C11 P1 119.6(4) . . ? C31A C30A C35A 118.8(4) . . ? C31A C30A P2A 120.4(3) . . ? C35A C30A P2A 120.7(3) . . ? C12A C13A C14A 120.8(5) . . ? C12A C13A H13A 119.6 . . ? C14A C13A H13A 119.6 . . ? C27A C28A C29A 120.4(5) . . ? C27A C28A H28A 119.8 . . ? C29A C28A H28A 119.8 . . ? C31A C32A C33A 120.6(5) . . ? C31A C32A H32A 119.7 . . ? C33A C32A H32A 119.7 . . ? C31 C32 C33 120.5(5) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C26 C27 C28 119.7(4) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C11 C6 C7 120.4(5) . . ? C11 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C32 C33 C34 119.2(4) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C4A C5A C1A 119.3(5) . . ? C4A C5A H5A 120.3 . . ? C1A C5A H5A 120.3 . . ? C38 C39 C40 119.5(5) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C21 C22 C23 119.8(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C40 C41 C36 120.3(5) . . ? C40 C41 H41 119.9 . . ? C36 C41 H41 119.9 . . ? C34 C35 C30 119.9(4) . . ? C34 C35 H35 120.0 . . ? C30 C35 H35 120.0 . . ? C4A N1A C3A 115.5(5) . . ? C3 C2 C1 119.5(5) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C17 C16 C15 119.6(4) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C13A C12A C17A 119.0(5) . . ? C13A C12A P1A 120.0(4) . . ? C17A C12A P1A 121.0(4) . . ? C7A C6A C11A 120.9(5) . . ? C7A C6A H6A 119.5 . . ? C11A C6A H6A 119.5 . . ? C27 C28 C29 120.3(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C12 C13 C14 120.5(4) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9A C8A C7A 120.5(5) . . ? C9A C8A H8A 119.8 . . ? C7A C8A H8A 119.8 . . ? C39 C38 C37 120.4(5) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C5A C1A C2A 117.0(5) . . ? C5A C1A Se1A 123.7(4) . . ? C2A C1A Se1A 119.2(4) . . ? C8A C9A C10A 119.6(5) . . ? C8A C9A H9A 120.2 . . ? C10A C9A H9A 120.2 . . ? C22 C23 C18 121.6(5) . . ? C22 C23 H23 119.2 . . ? C18 C23 H23 119.2 . . ? N1 C4 C5 124.6(5) . . ? N1 C4 H4 117.7 . . ? C5 C4 H4 117.7 . . ? C8 C7 C6 120.1(5) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C21A C20A C19A 119.6(5) . . ? C21A C20A H20A 120.2 . . ? C19A C20A H20A 120.2 . . ? C3A C2A C1A 119.5(5) . . ? C3A C2A H2A 120.2 . . ? C1A C2A H2A 120.2 . . ? C20A C19A C18A 121.3(5) . . ? C20A C19A H19A 119.4 . . ? C18A C19A H19A 119.4 . . ? C6A C7A C8A 119.7(5) . . ? C6A C7A H7A 120.2 . . ? C8A C7A H7A 120.2 . . ? C25A C26A C27A 120.8(5) . . ? C25A C26A H26A 119.6 . . ? C27A C26A H26A 119.6 . . ? O60 C61 C63 121.2(5) . . ? O60 C61 C62 121.9(5) . . ? C63 C61 C62 116.8(5) . . ? C4 C5 C1 119.8(4) . . ? C4 C5 H5 120.1 . . ? C1 C5 H5 120.1 . . ? C5 C1 C2 116.7(4) . . ? C5 C1 Se1 124.7(3) . . ? C2 C1 Se1 118.7(4) . . ? C41 C40 C39 120.1(5) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C17A C16A C15A 119.1(5) . . ? C17A C16A H16A 120.5 . . ? C15A C16A H16A 120.5 . . ? C16A C17A C12A 120.6(5) . . ? C16A C17A H17A 119.7 . . ? C12A C17A H17A 119.7 . . ? N1A C4A C5A 124.9(6) . . ? N1A C4A H4A 117.6 . . ? C5A C4A H4A 117.6 . . ? C20 C19 C18 120.8(5) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C15A C14A C13A 120.1(5) . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C8 C9 C10 120.7(5) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C21 C20 C19 120.9(5) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C61 C62 H62D 109.5 . . ? C61 C62 H62E 109.5 . . ? H62D C62 H62E 109.5 . . ? C61 C62 H62F 109.5 . . ? H62D C62 H62F 109.5 . . ? H62E C62 H62F 109.5 . . ? C9 C8 C7 120.2(5) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C20 C21 C22 119.8(5) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C14A C15A C16A 120.5(5) . . ? C14A C15A H15A 119.7 . . ? C16A C15A H15A 119.7 . . ? C61 C63 H63D 109.5 . . ? C61 C63 H63E 109.5 . . ? H63D C63 H63E 109.5 . . ? C61 C63 H63F 109.5 . . ? H63D C63 H63F 109.5 . . ? H63E C63 H63F 109.5 . . ? N1A C3A C2A 123.7(5) . . ? N1A C3A H3A 118.1 . . ? C2A C3A H3A 118.1 . . ? O60A C61A C63A 121.6(7) . . ? O60A C61A C62A 122.0(7) . . ? C63A C61A C62A 116.3(6) . . ? C61A C62A H62A 109.5 . . ? C61A C62A H62B 109.5 . . ? H62A C62A H62B 109.5 . . ? C61A C62A H62C 109.5 . . ? H62A C62A H62C 109.5 . . ? H62B C62A H62C 109.5 . . ? C61A C63A H63A 109.5 . . ? C61A C63A H63B 109.5 . . ? H63A C63A H63B 109.5 . . ? C61A C63A H63C 109.5 . . ? H63A C63A H63C 109.5 . . ? H63B C63A H63C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd1 Se1 C1 106.98(15) . . . . ? P1 Pd1 Se1 C1 -71.99(15) . . . . ? Cl1 Pd1 Se1 C1 94.4(6) . . . . ? P2A Pd1A Se1A C1A -110.87(16) . . . . ? Cl1A Pd1A Se1A C1A -28.3(3) . . . . ? P1A Pd1A Se1A C1A 73.51(16) . . . . ? Cl1A Pd1A P2A C36A -101.67(16) . . . . ? P1A Pd1A P2A C36A 128.1(4) . . . . ? Se1A Pd1A P2A C36A 70.77(15) . . . . ? Cl1A Pd1A P2A C30A 137.00(15) . . . . ? P1A Pd1A P2A C30A 6.8(5) . . . . ? Se1A Pd1A P2A C30A -50.56(15) . . . . ? Cl1A Pd1A P2A C24A 16.31(18) . . . . ? P1A Pd1A P2A C24A -113.9(5) . . . . ? Se1A Pd1A P2A C24A -171.26(17) . . . . ? P1 Pd1 P2 C36 -44.4(10) . . . . ? Cl1 Pd1 P2 C36 110.63(15) . . . . ? Se1 Pd1 P2 C36 -68.56(15) . . . . ? P1 Pd1 P2 C30 76.2(10) . . . . ? Cl1 Pd1 P2 C30 -128.78(15) . . . . ? Se1 Pd1 P2 C30 52.03(15) . . . . ? P1 Pd1 P2 C24 -164.7(9) . . . . ? Cl1 Pd1 P2 C24 -9.62(17) . . . . ? Se1 Pd1 P2 C24 171.19(17) . . . . ? P2A Pd1A P1A C18A 53.2(5) . . . . ? Cl1A Pd1A P1A C18A -77.14(15) . . . . ? Se1A Pd1A P1A C18A 110.32(15) . . . . ? P2A Pd1A P1A C11A -66.1(5) . . . . ? Cl1A Pd1A P1A C11A 163.55(18) . . . . ? Se1A Pd1A P1A C11A -9.00(18) . . . . ? P2A Pd1A P1A C12A 170.6(4) . . . . ? Cl1A Pd1A P1A C12A 40.21(16) . . . . ? Se1A Pd1A P1A C12A -132.34(16) . . . . ? P2 Pd1 P1 C18 -132.9(10) . . . . ? Cl1 Pd1 P1 C18 72.04(15) . . . . ? Se1 Pd1 P1 C18 -108.83(15) . . . . ? P2 Pd1 P1 C12 108.2(10) . . . . ? Cl1 Pd1 P1 C12 -46.88(16) . . . . ? Se1 Pd1 P1 C12 132.25(15) . . . . ? P2 Pd1 P1 C11 -10.8(10) . . . . ? Cl1 Pd1 P1 C11 -165.90(19) . . . . ? Se1 Pd1 P1 C11 13.23(19) . . . . ? C11A P1A C18A C19A -30.8(5) . . . . ? C12A P1A C18A C19A 75.3(4) . . . . ? Pd1A P1A C18A C19A -160.6(4) . . . . ? C11A P1A C18A C23A 151.0(4) . . . . ? C12A P1A C18A C23A -102.8(4) . . . . ? Pd1A P1A C18A C23A 21.3(4) . . . . ? C36A P2A C24A C29A 159.2(4) . . . . ? C30A P2A C24A C29A -88.6(4) . . . . ? Pd1A P2A C24A C29A 39.1(4) . . . . ? C36A P2A C24A C25A -27.0(4) . . . . ? C30A P2A C24A C25A 85.2(4) . . . . ? Pd1A P2A C24A C25A -147.1(3) . . . . ? C30A C35A C34A C33A 0.0(7) . . . . ? C36 P2 C24 C25 -24.8(5) . . . . ? C30 P2 C24 C25 -137.8(4) . . . . ? Pd1 P2 C24 C25 94.9(4) . . . . ? C36 P2 C24 C29 158.1(3) . . . . ? C30 P2 C24 C29 45.1(4) . . . . ? Pd1 P2 C24 C29 -82.2(4) . . . . ? C29 C24 C25 C26 -1.1(7) . . . . ? P2 C24 C25 C26 -178.1(4) . . . . ? C38 C37 C36 C41 -1.6(7) . . . . ? C38 C37 C36 P2 -175.1(3) . . . . ? C30 P2 C36 C37 -11.3(4) . . . . ? C24 P2 C36 C37 -119.4(4) . . . . ? Pd1 P2 C36 C37 114.6(4) . . . . ? C30 P2 C36 C41 175.2(3) . . . . ? C24 P2 C36 C41 67.1(4) . . . . ? Pd1 P2 C36 C41 -58.9(4) . . . . ? C25A C24A C29A C28A 0.5(7) . . . . ? P2A C24A C29A C28A 174.4(4) . . . . ? C36 P2 C30 C35 -54.1(4) . . . . ? C24 P2 C30 C35 58.6(4) . . . . ? Pd1 P2 C30 C35 -173.9(3) . . . . ? C36 P2 C30 C31 130.4(3) . . . . ? C24 P2 C30 C31 -116.9(4) . . . . ? Pd1 P2 C30 C31 10.6(4) . . . . ? C25 C24 C29 C28 1.5(7) . . . . ? P2 C24 C29 C28 178.8(4) . . . . ? C29A C24A C25A C26A 0.2(7) . . . . ? P2A C24A C25A C26A -173.6(4) . . . . ? C40A C39A C38A C37A 0.5(7) . . . . ? C36A C37A C38A C39A -2.3(7) . . . . ? C23A C22A C21A C20A -0.5(7) . . . . ? C35 C30 C31 C32 1.5(6) . . . . ? P2 C30 C31 C32 177.1(3) . . . . ? C38A C37A C36A C41A 2.6(7) . . . . ? C38A C37A C36A P2A 176.4(3) . . . . ? C30A P2A C36A C37A 16.7(4) . . . . ? C24A P2A C36A C37A 124.0(4) . . . . ? Pd1A P2A C36A C37A -109.2(4) . . . . ? C30A P2A C36A C41A -169.5(3) . . . . ? C24A P2A C36A C41A -62.1(4) . . . . ? Pd1A P2A C36A C41A 64.7(4) . . . . ? C24 C25 C26 C27 0.3(7) . . . . ? C13 C14 C15 C16 -2.7(7) . . . . ? C12 P1 C18 C23 92.4(4) . . . . ? C11 P1 C18 C23 -161.9(4) . . . . ? Pd1 P1 C18 C23 -31.8(4) . . . . ? C12 P1 C18 C19 -83.0(4) . . . . ? C11 P1 C18 C19 22.7(5) . . . . ? Pd1 P1 C18 C19 152.8(4) . . . . ? C37A C36A C41A C40A -1.3(7) . . . . ? P2A C36A C41A C40A -175.5(4) . . . . ? C35A C34A C33A C32A 0.1(7) . . . . ? C21A C22A C23A C18A 1.1(7) . . . . ? C19A C18A C23A C22A -1.0(7) . . . . ? P1A C18A C23A C22A 177.3(4) . . . . ? C4 N1 C3 C2 1.9(8) . . . . ? C16 C17 C12 C13 -2.2(7) . . . . ? C16 C17 C12 P1 173.6(4) . . . . ? C18 P1 C12 C13 -138.6(4) . . . . ? C11 P1 C12 C13 112.3(4) . . . . ? Pd1 P1 C12 C13 -17.0(4) . . . . ? C18 P1 C12 C17 45.7(4) . . . . ? C11 P1 C12 C17 -63.5(4) . . . . ? Pd1 P1 C12 C17 167.3(3) . . . . ? C9A C10A C11A C6A 0.4(7) . . . . ? C9A C10A C11A P1A 178.8(4) . . . . ? C18A P1A C11A C6A -38.9(5) . . . . ? C12A P1A C11A C6A -148.3(4) . . . . ? Pd1A P1A C11A C6A 81.5(4) . . . . ? C18A P1A C11A C10A 142.7(4) . . . . ? C12A P1A C11A C10A 33.3(4) . . . . ? Pd1A P1A C11A C10A -96.8(4) . . . . ? C36A C41A C40A C39A -0.4(7) . . . . ? C38A C39A C40A C41A 0.8(8) . . . . ? C9 C10 C11 C6 -1.1(7) . . . . ? C9 C10 C11 P1 -178.9(4) . . . . ? C18 P1 C11 C6 43.3(5) . . . . ? C12 P1 C11 C6 152.8(4) . . . . ? Pd1 P1 C11 C6 -81.3(4) . . . . ? C18 P1 C11 C10 -139.0(4) . . . . ? C12 P1 C11 C10 -29.5(4) . . . . ? Pd1 P1 C11 C10 96.4(4) . . . . ? C32A C31A C30A C35A -0.6(6) . . . . ? C32A C31A C30A P2A -177.5(3) . . . . ? C34A C35A C30A C31A 0.3(6) . . . . ? C34A C35A C30A P2A 177.2(3) . . . . ? C36A P2A C30A C31A -133.1(4) . . . . ? C24A P2A C30A C31A 117.7(4) . . . . ? Pd1A P2A C30A C31A -11.8(4) . . . . ? C36A P2A C30A C35A 50.0(4) . . . . ? C24A P2A C30A C35A -59.1(4) . . . . ? Pd1A P2A C30A C35A 171.4(3) . . . . ? C26A C27A C28A C29A 0.3(7) . . . . ? C24A C29A C28A C27A -0.8(8) . . . . ? C30A C31A C32A C33A 0.8(7) . . . . ? C34A C33A C32A C31A -0.5(7) . . . . ? C30 C31 C32 C33 -0.9(7) . . . . ? C25 C26 C27 C28 0.0(7) . . . . ? C10 C11 C6 C7 2.4(7) . . . . ? P1 C11 C6 C7 -179.9(4) . . . . ? C31 C32 C33 C34 0.0(7) . . . . ? C35 C34 C33 C32 0.3(7) . . . . ? C37 C36 C41 C40 2.2(7) . . . . ? P2 C36 C41 C40 175.9(4) . . . . ? C33 C34 C35 C30 0.4(7) . . . . ? C31 C30 C35 C34 -1.3(6) . . . . ? P2 C30 C35 C34 -176.8(3) . . . . ? N1 C3 C2 C1 -2.2(8) . . . . ? C12 C17 C16 C15 0.6(7) . . . . ? C14 C15 C16 C17 1.8(7) . . . . ? C14A C13A C12A C17A 0.6(7) . . . . ? C14A C13A C12A P1A 179.0(4) . . . . ? C18A P1A C12A C13A 139.3(4) . . . . ? C11A P1A C12A C13A -112.1(4) . . . . ? Pd1A P1A C12A C13A 21.3(4) . . . . ? C18A P1A C12A C17A -42.3(4) . . . . ? C11A P1A C12A C17A 66.3(4) . . . . ? Pd1A P1A C12A C17A -160.4(3) . . . . ? C10A C11A C6A C7A -2.2(7) . . . . ? P1A C11A C6A C7A 179.4(4) . . . . ? C26 C27 C28 C29 0.5(7) . . . . ? C24 C29 C28 C27 -1.3(7) . . . . ? C17 C12 C13 C14 1.3(7) . . . . ? P1 C12 C13 C14 -174.5(3) . . . . ? C15 C14 C13 C12 1.2(7) . . . . ? C40 C39 C38 C37 0.9(7) . . . . ? C36 C37 C38 C39 0.1(7) . . . . ? C4A C5A C1A C2A 0.7(8) . . . . ? C4A C5A C1A Se1A 179.8(4) . . . . ? Pd1A Se1A C1A C5A 19.1(5) . . . . ? Pd1A Se1A C1A C2A -161.9(4) . . . . ? C7A C8A C9A C10A -0.8(8) . . . . ? C11A C10A C9A C8A 1.2(8) . . . . ? C21 C22 C23 C18 0.0(8) . . . . ? C19 C18 C23 C22 -0.8(7) . . . . ? P1 C18 C23 C22 -176.4(4) . . . . ? C3 N1 C4 C5 -0.9(8) . . . . ? C11 C6 C7 C8 -2.2(8) . . . . ? C22A C21A C20A C19A -0.2(8) . . . . ? C5A C1A C2A C3A -1.6(8) . . . . ? Se1A C1A C2A C3A 179.3(5) . . . . ? C21A C20A C19A C18A 0.3(8) . . . . ? C23A C18A C19A C20A 0.3(8) . . . . ? P1A C18A C19A C20A -177.9(4) . . . . ? C11A C6A C7A C8A 2.6(8) . . . . ? C9A C8A C7A C6A -1.1(8) . . . . ? C24A C25A C26A C27A -0.7(7) . . . . ? C28A C27A C26A C25A 0.4(7) . . . . ? N1 C4 C5 C1 0.2(8) . . . . ? C4 C5 C1 C2 -0.3(7) . . . . ? C4 C5 C1 Se1 -179.1(4) . . . . ? C3 C2 C1 C5 1.3(7) . . . . ? C3 C2 C1 Se1 -179.9(4) . . . . ? Pd1 Se1 C1 C5 -14.7(4) . . . . ? Pd1 Se1 C1 C2 166.6(4) . . . . ? C36 C41 C40 C39 -1.2(7) . . . . ? C38 C39 C40 C41 -0.4(7) . . . . ? C15A C16A C17A C12A -0.9(8) . . . . ? C13A C12A C17A C16A 0.2(7) . . . . ? P1A C12A C17A C16A -178.2(4) . . . . ? C3A N1A C4A C5A -0.8(10) . . . . ? C1A C5A C4A N1A 0.5(10) . . . . ? C23 C18 C19 C20 1.6(8) . . . . ? P1 C18 C19 C20 177.1(4) . . . . ? C12A C13A C14A C15A -0.8(8) . . . . ? C11 C10 C9 C8 -0.4(8) . . . . ? C18 C19 C20 C21 -1.8(9) . . . . ? C10 C9 C8 C7 0.6(8) . . . . ? C6 C7 C8 C9 0.7(8) . . . . ? C19 C20 C21 C22 1.1(9) . . . . ? C23 C22 C21 C20 -0.2(8) . . . . ? C13A C14A C15A C16A 0.1(8) . . . . ? C17A C16A C15A C14A 0.7(8) . . . . ? C4A N1A C3A C2A -0.2(10) . . . . ? C1A C2A C3A N1A 1.5(10) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.408 _refine_diff_density_min -0.822 _refine_diff_density_rms 0.085 _database_code_depnum_ccdc_archive 'CCDC 924432' ####################################################################### # # 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_sdb #TrackingRef 'web_deposit_cif_file_1_Dr.SandipDey_1360841986.sdb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H34 Cl N P2 Pt Se' _chemical_formula_weight 623.89 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' Cl Cl 0.1484 0.1585 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.4320(6) _cell_length_b 10.6073(5) _cell_length_c 15.4103(7) _cell_angle_alpha 90.00 _cell_angle_beta 105.0360(10) _cell_angle_gamma 90.00 _cell_volume 2278.31(18) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 35.99 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.819 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 8.014 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1338 _exptl_absorpt_correction_T_max 0.2392 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'APEX II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47227 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.50 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 5237 _reflns_number_gt 4966 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; APEX-II(BRUKER-NONIUS, 2003) ; _computing_data_reduction APEX-II _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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. Elongated thermal ellipsoids on C14 and C15 indicated disorder and was modeled successfully with a 81:19 ratio. Restraints and constraints were used to keep the bond distances and the thermal ellipsoids meaningful. ; _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^)+(0.0175P)^2^+2.6568P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5237 _refine_ls_number_parameters 222 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0177 _refine_ls_R_factor_gt 0.0162 _refine_ls_wR_factor_ref 0.0405 _refine_ls_wR_factor_gt 0.0396 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Pt1 Pt 0.511280(5) 0.743329(7) 0.297623(5) 0.01687(3) Uani 1 1 d . A . Se1 Se 0.565488(15) 0.52724(2) 0.327736(14) 0.02018(5) Uani 1 1 d . . . Cl1 Cl 0.46350(4) 0.95514(5) 0.27951(4) 0.02943(12) Uani 1 1 d . . . P1 P 0.37692(4) 0.71099(6) 0.35080(4) 0.02101(11) Uani 1 1 d . . . P2 P 0.64646(4) 0.78324(6) 0.24830(4) 0.02184(11) Uani 1 1 d D . . N1 N 0.41438(17) 0.3026(2) 0.06457(15) 0.0343(5) Uani 1 1 d . . . C1 C 0.50028(14) 0.4404(2) 0.22166(15) 0.0201(4) Uani 1 1 d . . . C2 C 0.49665(15) 0.3088(2) 0.22147(16) 0.0234(4) Uani 1 1 d . . . H2 H 0.5232 0.2629 0.2751 0.028 Uiso 1 1 calc R . . C3 C 0.45410(18) 0.2457(2) 0.14245(19) 0.0284(5) Uani 1 1 d . . . H3 H 0.4532 0.1561 0.1439 0.034 Uiso 1 1 calc R . . C4 C 0.4170(2) 0.4287(3) 0.06589(17) 0.0341(6) Uani 1 1 d . . . H4 H 0.3889 0.4718 0.0113 0.041 Uiso 1 1 calc R . . C5 C 0.45769(17) 0.5011(2) 0.14086(15) 0.0267(5) Uani 1 1 d . . . H5 H 0.4566 0.5906 0.1373 0.032 Uiso 1 1 calc R . . C6 C 0.35695(17) 0.5528(2) 0.38975(17) 0.0273(5) Uani 1 1 d . . . H6A H 0.3573 0.4923 0.3409 0.033 Uiso 1 1 calc R . . H6B H 0.4117 0.5313 0.4412 0.033 Uiso 1 1 calc R . . C7 C 0.26420(19) 0.5338(3) 0.41871(19) 0.0364(6) Uani 1 1 d . . . H7A H 0.2090 0.5426 0.3664 0.055 Uiso 1 1 calc R . . H7B H 0.2602 0.5973 0.4638 0.055 Uiso 1 1 calc R . . H7C H 0.2640 0.4494 0.4445 0.055 Uiso 1 1 calc R . . C8 C 0.26574(19) 0.7552(3) 0.26934(19) 0.0340(6) Uani 1 1 d . . . H8A H 0.2121 0.7467 0.2980 0.041 Uiso 1 1 calc R . . H8B H 0.2698 0.8450 0.2533 0.041 Uiso 1 1 calc R . . C9 C 0.2430(2) 0.6773(3) 0.18375(19) 0.0468(7) Uani 1 1 d . . . H9A H 0.1823 0.7060 0.1438 0.070 Uiso 1 1 calc R . . H9B H 0.2376 0.5882 0.1986 0.070 Uiso 1 1 calc R . . H9C H 0.2946 0.6873 0.1536 0.070 Uiso 1 1 calc R . . C10 C 0.37876(19) 0.8148(3) 0.44549(17) 0.0317(5) Uani 1 1 d . . . H10A H 0.3742 0.9033 0.4245 0.038 Uiso 1 1 calc R . . H10B H 0.3219 0.7969 0.4681 0.038 Uiso 1 1 calc R . . C11 C 0.4686(2) 0.7996(3) 0.52205(19) 0.0456(7) Uani 1 1 d . . . H11A H 0.5254 0.8086 0.4989 0.068 Uiso 1 1 calc R . . H11B H 0.4688 0.7160 0.5491 0.068 Uiso 1 1 calc R . . H11C H 0.4697 0.8645 0.5676 0.068 Uiso 1 1 calc R . . C12 C 0.6511(2) 0.9358(2) 0.19598(18) 0.0335(6) Uani 1 1 d . A . H12A H 0.6366 1.0024 0.2355 0.040 Uiso 1 1 calc R . . H12B H 0.7170 0.9503 0.1903 0.040 Uiso 1 1 calc R . . C13 C 0.5814(2) 0.9471(3) 0.10391(19) 0.0417(7) Uani 1 1 d . . . H13A H 0.5996 0.8876 0.0626 0.063 Uiso 1 1 calc R A . H13B H 0.5833 1.0332 0.0813 0.063 Uiso 1 1 calc R . . H13C H 0.5164 0.9280 0.1083 0.063 Uiso 1 1 calc R . . C14 C 0.7556(2) 0.7657(3) 0.3415(2) 0.0300(7) Uani 0.807(4) 1 d PD A 1 H14A H 0.7701 0.6749 0.3520 0.036 Uiso 0.807(4) 1 calc PR A 1 H14B H 0.8104 0.8052 0.3242 0.036 Uiso 0.807(4) 1 calc PR A 1 C15 C 0.7454(3) 0.8254(4) 0.4280(2) 0.0408(8) Uani 0.807(4) 1 d PD A 1 H15A H 0.7291 0.9148 0.4176 0.061 Uiso 0.807(4) 1 calc PR A 1 H15B H 0.8060 0.8175 0.4744 0.061 Uiso 0.807(4) 1 calc PR A 1 H15C H 0.6943 0.7824 0.4479 0.061 Uiso 0.807(4) 1 calc PR A 1 C16 C 0.66983(17) 0.6733(2) 0.16552(17) 0.0273(5) Uani 1 1 d . A . H16A H 0.6734 0.5870 0.1906 0.033 Uiso 1 1 calc R . . H16B H 0.6149 0.6757 0.1115 0.033 Uiso 1 1 calc R . . C17 C 0.76207(18) 0.6994(3) 0.13670(19) 0.0332(5) Uani 1 1 d . . . H17A H 0.7700 0.6350 0.0936 0.050 Uiso 1 1 calc R A . H17B H 0.8172 0.6971 0.1895 0.050 Uiso 1 1 calc R . . H17C H 0.7579 0.7828 0.1085 0.050 Uiso 1 1 calc R . . C14A C 0.7467(7) 0.8402(12) 0.3412(6) 0.0300(7) Uani 0.193(4) 1 d PD A 2 H14C H 0.8028 0.8585 0.3176 0.036 Uiso 0.193(4) 1 calc PR A 2 H14D H 0.7274 0.9196 0.3654 0.036 Uiso 0.193(4) 1 calc PR A 2 C15A C 0.7750(13) 0.7443(13) 0.4165(9) 0.0408(8) Uani 0.193(4) 1 d PD A 2 H15D H 0.7848 0.6619 0.3915 0.061 Uiso 0.193(4) 1 calc PR A 2 H15E H 0.7239 0.7377 0.4476 0.061 Uiso 0.193(4) 1 calc PR A 2 H15F H 0.8346 0.7712 0.4592 0.061 Uiso 0.193(4) 1 calc PR 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 Pt1 0.01752(5) 0.01968(5) 0.01382(5) -0.00083(3) 0.00483(3) -0.00033(3) Se1 0.02151(10) 0.02178(11) 0.01700(10) 0.00100(8) 0.00454(7) 0.00068(8) Cl1 0.0350(3) 0.0226(3) 0.0345(3) 0.0030(2) 0.0158(2) 0.0053(2) P1 0.0190(2) 0.0269(3) 0.0184(3) 0.0001(2) 0.0071(2) 0.0005(2) P2 0.0194(3) 0.0297(3) 0.0167(3) -0.0006(2) 0.0052(2) -0.0041(2) N1 0.0404(12) 0.0308(11) 0.0298(11) -0.0093(9) 0.0056(9) -0.0026(9) C1 0.0169(9) 0.0239(11) 0.0201(10) -0.0033(8) 0.0060(7) -0.0006(8) C2 0.0202(10) 0.0236(11) 0.0273(11) 0.0008(9) 0.0075(8) 0.0016(8) C3 0.0257(12) 0.0233(12) 0.0367(15) -0.0048(9) 0.0091(10) 0.0007(8) C4 0.0434(14) 0.0310(13) 0.0233(12) -0.0027(10) 0.0004(10) -0.0001(11) C5 0.0339(12) 0.0233(11) 0.0222(11) -0.0014(9) 0.0058(9) -0.0005(9) C6 0.0263(11) 0.0295(12) 0.0271(12) 0.0018(10) 0.0085(9) -0.0049(9) C7 0.0315(12) 0.0441(15) 0.0380(14) 0.0002(12) 0.0169(11) -0.0093(11) C8 0.0209(12) 0.0501(17) 0.0311(14) 0.0109(11) 0.0068(10) 0.0051(10) C9 0.0350(14) 0.066(2) 0.0308(15) 0.0044(14) -0.0067(11) -0.0087(14) C10 0.0424(14) 0.0322(13) 0.0268(12) -0.0043(10) 0.0204(11) -0.0003(11) C11 0.0629(19) 0.0515(18) 0.0221(13) -0.0094(12) 0.0101(13) -0.0055(15) C12 0.0447(14) 0.0231(12) 0.0395(14) -0.0047(10) 0.0234(12) -0.0100(10) C13 0.0620(18) 0.0319(14) 0.0368(15) 0.0096(12) 0.0231(13) 0.0132(13) C14 0.0238(14) 0.0382(19) 0.0252(15) 0.0007(14) 0.0013(11) -0.0040(13) C15 0.047(2) 0.0412(19) 0.0260(16) -0.0057(15) -0.0045(13) -0.0072(15) C16 0.0306(12) 0.0256(11) 0.0313(12) 0.0029(9) 0.0180(10) 0.0023(9) C17 0.0309(12) 0.0380(14) 0.0371(14) 0.0067(11) 0.0201(11) 0.0038(11) C14A 0.0238(14) 0.0382(19) 0.0252(15) 0.0007(14) 0.0013(11) -0.0040(13) C15A 0.047(2) 0.0412(19) 0.0260(16) -0.0057(15) -0.0045(13) -0.0072(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 Pt1 P2 2.3092(6) . ? Pt1 P1 2.3182(6) . ? Pt1 Cl1 2.3455(6) . ? Pt1 Se1 2.4275(2) . ? Se1 C1 1.900(2) . ? P1 C10 1.822(2) . ? P1 C8 1.823(3) . ? P1 C6 1.830(2) . ? P2 C12 1.817(3) . ? P2 C16 1.823(2) . ? P2 C14 1.846(3) . ? P2 C14A 1.853(5) . ? N1 C3 1.333(4) . ? N1 C4 1.338(3) . ? C1 C5 1.395(3) . ? C1 C2 1.396(3) . ? C2 C3 1.386(4) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.530(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.518(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.519(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.516(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.517(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.534(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C14A C15A 1.518(6) . ? C14A H14C 0.9900 . ? C14A H14D 0.9900 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 177.56(2) . . ? P2 Pt1 Cl1 91.87(2) . . ? P1 Pt1 Cl1 86.37(2) . . ? P2 Pt1 Se1 88.747(17) . . ? P1 Pt1 Se1 92.886(16) . . ? Cl1 Pt1 Se1 175.892(16) . . ? C1 Se1 Pt1 103.32(7) . . ? C10 P1 C8 102.92(13) . . ? C10 P1 C6 105.18(12) . . ? C8 P1 C6 106.02(12) . . ? C10 P1 Pt1 110.73(9) . . ? C8 P1 Pt1 112.70(9) . . ? C6 P1 Pt1 117.97(8) . . ? C12 P2 C16 102.96(11) . . ? C12 P2 C14 108.24(14) . . ? C16 P2 C14 101.80(14) . . ? C12 P2 C14A 86.6(4) . . ? C16 P2 C14A 120.0(5) . . ? C14 P2 C14A 25.0(4) . . ? C12 P2 Pt1 116.15(9) . . ? C16 P2 Pt1 116.01(8) . . ? C14 P2 Pt1 110.41(11) . . ? C14A P2 Pt1 111.2(4) . . ? C3 N1 C4 115.8(2) . . ? C5 C1 C2 116.9(2) . . ? C5 C1 Se1 123.29(17) . . ? C2 C1 Se1 119.77(17) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? N1 C3 C2 124.1(2) . . ? N1 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? N1 C4 C5 124.8(2) . . ? N1 C4 H4 117.6 . . ? C5 C4 H4 117.6 . . ? C4 C5 C1 118.8(2) . . ? C4 C5 H5 120.6 . . ? C1 C5 H5 120.6 . . ? C7 C6 P1 116.15(19) . . ? C7 C6 H6A 108.2 . . ? P1 C6 H6A 108.2 . . ? C7 C6 H6B 108.2 . . ? P1 C6 H6B 108.2 . . ? H6A C6 H6B 107.4 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 P1 114.3(2) . . ? C9 C8 H8A 108.7 . . ? P1 C8 H8A 108.7 . . ? C9 C8 H8B 108.7 . . ? P1 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 112.97(19) . . ? C11 C10 H10A 109.0 . . ? P1 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? P1 C10 H10B 109.0 . . ? H10A C10 H10B 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 P2 113.21(19) . . ? C13 C12 H12A 108.9 . . ? P2 C12 H12A 108.9 . . ? C13 C12 H12B 108.9 . . ? P2 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 P2 112.5(2) . . ? C15 C14 H14A 109.1 . . ? P2 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? P2 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C17 C16 P2 114.80(18) . . ? C17 C16 H16A 108.6 . . ? P2 C16 H16A 108.6 . . ? C17 C16 H16B 108.6 . . ? P2 C16 H16B 108.6 . . ? H16A C16 H16B 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15A C14A P2 112.0(8) . . ? C15A C14A H14C 109.2 . . ? P2 C14A H14C 109.2 . . ? C15A C14A H14D 109.2 . . ? P2 C14A H14D 109.2 . . ? H14C C14A H14D 107.9 . . ? C14A C15A H15D 109.5 . . ? C14A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C14A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 Se1 C1 -94.89(7) . . . . ? P1 Pt1 Se1 C1 86.92(7) . . . . ? Cl1 Pt1 Se1 C1 166.4(2) . . . . ? P2 Pt1 P1 C10 -12.4(5) . . . . ? Cl1 Pt1 P1 C10 -56.29(10) . . . . ? Se1 Pt1 P1 C10 119.67(10) . . . . ? P2 Pt1 P1 C8 102.3(5) . . . . ? Cl1 Pt1 P1 C8 58.39(10) . . . . ? Se1 Pt1 P1 C8 -125.66(10) . . . . ? P2 Pt1 P1 C6 -133.6(5) . . . . ? Cl1 Pt1 P1 C6 -177.49(9) . . . . ? Se1 Pt1 P1 C6 -1.54(9) . . . . ? P1 Pt1 P2 C12 -56.0(5) . . . . ? Cl1 Pt1 P2 C12 -12.21(10) . . . . ? Se1 Pt1 P2 C12 171.85(10) . . . . ? P1 Pt1 P2 C16 -177.2(5) . . . . ? Cl1 Pt1 P2 C16 -133.39(9) . . . . ? Se1 Pt1 P2 C16 50.67(9) . . . . ? P1 Pt1 P2 C14 67.7(5) . . . . ? Cl1 Pt1 P2 C14 111.49(12) . . . . ? Se1 Pt1 P2 C14 -64.45(12) . . . . ? P1 Pt1 P2 C14A 40.9(7) . . . . ? Cl1 Pt1 P2 C14A 84.7(4) . . . . ? Se1 Pt1 P2 C14A -91.2(4) . . . . ? Pt1 Se1 C1 C5 16.73(19) . . . . ? Pt1 Se1 C1 C2 -165.76(16) . . . . ? C5 C1 C2 C3 1.6(3) . . . . ? Se1 C1 C2 C3 -176.08(17) . . . . ? C4 N1 C3 C2 -0.3(4) . . . . ? C1 C2 C3 N1 -0.7(4) . . . . ? C3 N1 C4 C5 0.3(4) . . . . ? N1 C4 C5 C1 0.6(4) . . . . ? C2 C1 C5 C4 -1.5(3) . . . . ? Se1 C1 C5 C4 176.06(19) . . . . ? C10 P1 C6 C7 59.7(2) . . . . ? C8 P1 C6 C7 -48.9(2) . . . . ? Pt1 P1 C6 C7 -176.30(16) . . . . ? C10 P1 C8 C9 -177.1(2) . . . . ? C6 P1 C8 C9 -66.9(2) . . . . ? Pt1 P1 C8 C9 63.6(2) . . . . ? C8 P1 C10 C11 -177.4(2) . . . . ? C6 P1 C10 C11 71.7(2) . . . . ? Pt1 P1 C10 C11 -56.8(2) . . . . ? C16 P2 C12 C13 56.5(2) . . . . ? C14 P2 C12 C13 163.8(2) . . . . ? C14A P2 C12 C13 176.5(5) . . . . ? Pt1 P2 C12 C13 -71.4(2) . . . . ? C12 P2 C14 C15 84.8(3) . . . . ? C16 P2 C14 C15 -167.1(2) . . . . ? C14A P2 C14 C15 53.4(10) . . . . ? Pt1 P2 C14 C15 -43.3(3) . . . . ? C12 P2 C16 C17 54.2(2) . . . . ? C14 P2 C16 C17 -57.9(2) . . . . ? C14A P2 C16 C17 -39.5(5) . . . . ? Pt1 P2 C16 C17 -177.82(15) . . . . ? C12 P2 C14A C15A 177.2(12) . . . . ? C16 P2 C14A C15A -79.8(12) . . . . ? C14 P2 C14A C15A -32.6(9) . . . . ? Pt1 P2 C14A C15A 60.4(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.675 _refine_diff_density_min -0.985 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 924433' ####################################################################### # # 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_mono1 #TrackingRef 'web_deposit_cif_file_2_Dr.SandipDey_1360841986.mono.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 N2 P2 Pd Se2' _chemical_formula_weight 945.04 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.1330(11) _cell_length_b 12.8723(14) _cell_length_c 15.0542(16) _cell_angle_alpha 90.00 _cell_angle_beta 91.1260(10) _cell_angle_gamma 90.00 _cell_volume 1963.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9988 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 2.444 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3745 _exptl_absorpt_correction_T_max 0.6958 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'APEX II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30774 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.48 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 8936 _reflns_number_gt 8155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; APEX-II(BRUKER-NONIUS, 2003) ; _computing_data_reduction APEX-II _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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^)+(0.0711P)^2^+2.5593P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 8936 _refine_ls_number_parameters 479 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0485 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.25254(3) 0.50163(4) 0.26000(2) 0.01625(9) Uani 1 1 d . . . Se1 Se 0.08339(4) 0.51090(4) 0.37401(3) 0.02369(14) Uani 1 1 d . . . Se2 Se 0.41658(4) 0.49565(4) 0.14231(3) 0.01984(11) Uani 1 1 d . . . P1 P 0.17316(11) 0.66444(10) 0.21518(8) 0.0171(2) Uani 1 1 d . . . P2 P 0.33126(11) 0.33519(11) 0.29741(8) 0.0170(2) Uani 1 1 d . . . N1 N 0.2972(6) 0.4856(4) 0.6540(3) 0.0445(13) Uani 1 1 d . . . N2 N 0.1579(5) 0.4811(3) -0.1216(3) 0.0327(11) Uani 1 1 d . . . C1 C 0.1743(5) 0.4994(5) 0.4849(3) 0.0257(9) Uani 1 1 d . . . C2 C 0.3097(5) 0.5060(5) 0.4965(3) 0.0319(11) Uani 1 1 d . . . H2 H 0.3645 0.5158 0.4467 0.038 Uiso 1 1 calc R . . C3 C 0.3657(6) 0.4980(6) 0.5818(4) 0.0445(14) Uani 1 1 d . . . H3 H 0.4590 0.5018 0.5878 0.053 Uiso 1 1 calc R . . C4 C 0.1642(8) 0.4826(5) 0.6431(4) 0.0462(17) Uani 1 1 d . . . H4 H 0.1118 0.4759 0.6944 0.055 Uiso 1 1 calc R . . C5 C 0.1014(6) 0.4888(5) 0.5616(3) 0.0367(13) Uani 1 1 d . . . H5 H 0.0078 0.4858 0.5576 0.044 Uiso 1 1 calc R . . C6 C 0.3088(4) 0.4883(4) 0.0373(3) 0.0197(9) Uani 1 1 d . . . C7 C 0.3587(5) 0.5224(4) -0.0430(3) 0.0269(11) Uani 1 1 d . . . H7 H 0.4459 0.5491 -0.0457 0.032 Uiso 1 1 calc R . . C8 C 0.2813(6) 0.5169(4) -0.1175(3) 0.0327(12) Uani 1 1 d . . . H8 H 0.3182 0.5407 -0.1714 0.039 Uiso 1 1 calc R . . C9 C 0.1116(5) 0.4478(4) -0.0440(4) 0.0331(12) Uani 1 1 d . . . H9 H 0.0238 0.4220 -0.0434 0.040 Uiso 1 1 calc R . . C10 C 0.1823(5) 0.4484(4) 0.0351(4) 0.0272(11) Uani 1 1 d . . . H10 H 0.1444 0.4216 0.0876 0.033 Uiso 1 1 calc R . . C11 C 0.2163(5) 0.7710(4) 0.2924(3) 0.0249(11) Uani 1 1 d . . . C12 C 0.2555(5) 0.7497(4) 0.3801(4) 0.0287(12) Uani 1 1 d . . . H12 H 0.2638 0.6796 0.3991 0.034 Uiso 1 1 calc R . . C13 C 0.2821(6) 0.8288(5) 0.4392(4) 0.0376(13) Uani 1 1 d . . . H13 H 0.3108 0.8129 0.4981 0.045 Uiso 1 1 calc R . . C14 C 0.2678(6) 0.9299(6) 0.4138(4) 0.0475(16) Uani 1 1 d . . . H14 H 0.2820 0.9839 0.4559 0.057 Uiso 1 1 calc R . . C15 C 0.2327(7) 0.9541(5) 0.3272(5) 0.0463(16) Uani 1 1 d . . . H15 H 0.2266 1.0248 0.3097 0.056 Uiso 1 1 calc R . . C16 C 0.2060(6) 0.8762(5) 0.2653(4) 0.0376(13) Uani 1 1 d . . . H16 H 0.1812 0.8933 0.2059 0.045 Uiso 1 1 calc R . . C17 C -0.0075(4) 0.6641(4) 0.2039(3) 0.0187(9) Uani 1 1 d . . . C18 C -0.0809(5) 0.7524(4) 0.2162(4) 0.0270(11) Uani 1 1 d . . . H18 H -0.0380 0.8152 0.2332 0.032 Uiso 1 1 calc R . . C19 C -0.2167(5) 0.7510(5) 0.2039(4) 0.0332(13) Uani 1 1 d . . . H19 H -0.2665 0.8123 0.2137 0.040 Uiso 1 1 calc R . . C20 C -0.2791(5) 0.6619(5) 0.1779(3) 0.0279(12) Uani 1 1 d . . . H20 H -0.3722 0.6611 0.1690 0.033 Uiso 1 1 calc R . . C21 C -0.2061(5) 0.5724(5) 0.1645(3) 0.0273(11) Uani 1 1 d . . . H21 H -0.2492 0.5105 0.1458 0.033 Uiso 1 1 calc R . . C22 C -0.0703(5) 0.5729(4) 0.1783(3) 0.0227(10) Uani 1 1 d . . . H22 H -0.0207 0.5111 0.1704 0.027 Uiso 1 1 calc R . . C23 C 0.2255(5) 0.7192(4) 0.1100(3) 0.0201(10) Uani 1 1 d . . . C24 C 0.3526(5) 0.7597(4) 0.1026(4) 0.0270(11) Uani 1 1 d . . . H24 H 0.4113 0.7577 0.1526 0.032 Uiso 1 1 calc R . . C25 C 0.3936(5) 0.8017(4) 0.0259(4) 0.0338(13) Uani 1 1 d . . . H25 H 0.4808 0.8284 0.0224 0.041 Uiso 1 1 calc R . . C26 C 0.3086(6) 0.8065(5) -0.0491(4) 0.0348(13) Uani 1 1 d . . . H26 H 0.3377 0.8364 -0.1029 0.042 Uiso 1 1 calc R . . C27 C 0.1833(5) 0.7673(4) -0.0434(3) 0.0291(12) Uani 1 1 d . . . H27 H 0.1254 0.7698 -0.0938 0.035 Uiso 1 1 calc R . . C28 C 0.1400(5) 0.7238(4) 0.0356(3) 0.0224(10) Uani 1 1 d . . . H28 H 0.0527 0.6974 0.0392 0.027 Uiso 1 1 calc R . . C29 C 0.2784(5) 0.2448(4) 0.2099(3) 0.0257(11) Uani 1 1 d . . . C30 C 0.1532(6) 0.2004(5) 0.2123(4) 0.0424(15) Uani 1 1 d . . . H30 H 0.0984 0.2138 0.2615 0.051 Uiso 1 1 calc R . . C31 C 0.1077(7) 0.1376(6) 0.1448(5) 0.0519(18) Uani 1 1 d . . . H31 H 0.0231 0.1062 0.1479 0.062 Uiso 1 1 calc R . . C32 C 0.1870(7) 0.1201(5) 0.0714(4) 0.0461(16) Uani 1 1 d . . . H32 H 0.1585 0.0748 0.0250 0.055 Uiso 1 1 calc R . . C33 C 0.3039(6) 0.1682(5) 0.0678(4) 0.0419(14) Uani 1 1 d . . . H33 H 0.3561 0.1598 0.0165 0.050 Uiso 1 1 calc R . . C34 C 0.3509(6) 0.2303(5) 0.1374(4) 0.0358(13) Uani 1 1 d . . . H34 H 0.4349 0.2626 0.1334 0.043 Uiso 1 1 calc R . . C35 C 0.5105(4) 0.3297(4) 0.3022(3) 0.0171(9) Uani 1 1 d . . . C36 C 0.5806(5) 0.2379(4) 0.2881(3) 0.0251(11) Uani 1 1 d . . . H36 H 0.5349 0.1754 0.2740 0.030 Uiso 1 1 calc R . . C37 C 0.7186(5) 0.2386(4) 0.2950(4) 0.0293(12) Uani 1 1 d . . . H37 H 0.7670 0.1767 0.2847 0.035 Uiso 1 1 calc R . . C38 C 0.7840(5) 0.3290(5) 0.3166(4) 0.0315(12) Uani 1 1 d . . . H38 H 0.8777 0.3292 0.3209 0.038 Uiso 1 1 calc R . . C39 C 0.7158(5) 0.4189(4) 0.3321(3) 0.0264(11) Uani 1 1 d . . . H39 H 0.7619 0.4805 0.3483 0.032 Uiso 1 1 calc R . . C40 C 0.5796(5) 0.4198(4) 0.3240(3) 0.0190(9) Uani 1 1 d . . . H40 H 0.5328 0.4826 0.3335 0.023 Uiso 1 1 calc R . . C41 C 0.2869(5) 0.2706(4) 0.4015(3) 0.0197(10) Uani 1 1 d . . . C42 C 0.3787(5) 0.2422(5) 0.4644(3) 0.0297(12) Uani 1 1 d . . . H42 H 0.4698 0.2513 0.4528 0.036 Uiso 1 1 calc R . . C43 C 0.3409(6) 0.2001(5) 0.5456(4) 0.0365(14) Uani 1 1 d . . . H43 H 0.4066 0.1811 0.5885 0.044 Uiso 1 1 calc R . . C44 C 0.2109(6) 0.1859(4) 0.5640(4) 0.0343(13) Uani 1 1 d . . . H44 H 0.1862 0.1561 0.6189 0.041 Uiso 1 1 calc R . . C45 C 0.1173(7) 0.2147(5) 0.5033(4) 0.0432(16) Uani 1 1 d . . . H45 H 0.0267 0.2044 0.5158 0.052 Uiso 1 1 calc R . . C46 C 0.1522(5) 0.2589(5) 0.4231(4) 0.0351(13) Uani 1 1 d . . . H46 H 0.0854 0.2815 0.3823 0.042 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 0.01295(14) 0.02201(16) 0.01381(15) 0.00489(19) 0.00116(10) 0.00178(12) Se1 0.0156(2) 0.0405(4) 0.0150(2) 0.0029(3) 0.00223(14) 0.0008(2) Se2 0.01540(19) 0.0263(3) 0.0179(2) 0.0071(2) 0.00260(14) 0.0022(2) P1 0.0151(5) 0.0215(6) 0.0148(5) 0.0018(4) 0.0013(4) 0.0010(4) P2 0.0158(5) 0.0203(6) 0.0150(5) 0.0027(4) -0.0013(4) -0.0019(4) N1 0.075(4) 0.031(3) 0.027(2) 0.000(2) -0.019(2) 0.004(3) N2 0.044(3) 0.021(2) 0.032(2) -0.0033(18) -0.014(2) 0.0054(19) C1 0.030(2) 0.028(2) 0.019(2) 0.006(3) -0.0019(17) -0.003(3) C2 0.032(2) 0.034(3) 0.030(2) -0.011(3) -0.0054(19) 0.009(3) C3 0.042(3) 0.045(3) 0.046(3) -0.016(4) -0.021(3) 0.014(3) C4 0.085(5) 0.036(4) 0.018(2) 0.006(2) -0.003(3) -0.021(3) C5 0.039(3) 0.048(4) 0.023(2) 0.015(3) 0.002(2) -0.014(3) C6 0.021(2) 0.020(2) 0.0181(19) 0.0025(19) 0.0023(15) 0.0056(19) C7 0.028(2) 0.027(3) 0.026(2) 0.002(2) 0.0014(19) 0.001(2) C8 0.048(3) 0.028(3) 0.023(2) 0.004(2) -0.003(2) 0.001(2) C9 0.030(3) 0.025(3) 0.045(3) -0.010(2) 0.000(2) 0.000(2) C10 0.026(3) 0.029(3) 0.026(3) -0.006(2) 0.003(2) 0.000(2) C11 0.017(2) 0.030(3) 0.028(3) -0.006(2) 0.0006(19) -0.003(2) C12 0.025(3) 0.032(3) 0.029(3) -0.003(2) -0.003(2) -0.003(2) C13 0.038(3) 0.046(3) 0.028(3) -0.016(3) -0.007(2) 0.002(3) C14 0.044(4) 0.057(4) 0.041(4) -0.026(3) -0.006(3) -0.001(3) C15 0.053(4) 0.026(3) 0.060(4) -0.011(3) 0.002(3) 0.001(3) C16 0.043(3) 0.033(3) 0.037(3) -0.006(2) -0.006(3) 0.000(3) C17 0.016(2) 0.022(2) 0.018(2) 0.0032(18) -0.0002(17) -0.0026(18) C18 0.021(2) 0.027(3) 0.033(3) 0.005(2) 0.000(2) 0.004(2) C19 0.020(3) 0.035(3) 0.044(3) 0.005(3) 0.005(2) 0.010(2) C20 0.014(2) 0.041(3) 0.028(3) 0.007(2) 0.0001(19) 0.000(2) C21 0.020(2) 0.033(3) 0.029(3) 0.001(2) -0.004(2) -0.004(2) C22 0.023(2) 0.026(3) 0.019(2) 0.0006(19) 0.0000(18) 0.001(2) C23 0.022(2) 0.016(2) 0.022(2) 0.0040(18) 0.0077(19) 0.0034(18) C24 0.023(3) 0.026(3) 0.032(3) 0.002(2) 0.002(2) -0.002(2) C25 0.027(3) 0.031(3) 0.044(3) 0.006(2) 0.014(2) -0.004(2) C26 0.043(3) 0.033(3) 0.030(3) 0.015(2) 0.016(2) 0.007(2) C27 0.038(3) 0.028(3) 0.021(3) 0.011(2) 0.006(2) 0.014(2) C28 0.022(2) 0.024(2) 0.021(2) 0.0018(19) 0.0066(19) 0.0016(19) C29 0.033(3) 0.026(3) 0.018(2) 0.0003(19) -0.003(2) -0.008(2) C30 0.036(3) 0.057(4) 0.035(3) -0.008(3) 0.000(3) -0.015(3) C31 0.040(3) 0.073(5) 0.043(4) -0.004(3) -0.004(3) -0.019(3) C32 0.057(4) 0.054(4) 0.027(3) -0.017(3) -0.010(3) -0.006(3) C33 0.051(4) 0.049(4) 0.026(3) -0.008(3) 0.001(3) 0.007(3) C34 0.038(3) 0.037(3) 0.033(3) -0.007(2) 0.000(3) 0.000(2) C35 0.014(2) 0.027(2) 0.0107(19) 0.0031(18) 0.0004(16) 0.0036(19) C36 0.026(3) 0.021(2) 0.029(3) -0.002(2) -0.001(2) 0.003(2) C37 0.027(3) 0.024(3) 0.037(3) -0.002(2) 0.000(2) 0.009(2) C38 0.019(2) 0.041(3) 0.034(3) 0.005(3) -0.004(2) 0.006(2) C39 0.023(3) 0.032(3) 0.024(2) 0.005(2) -0.011(2) -0.007(2) C40 0.020(2) 0.018(2) 0.019(2) 0.0029(18) 0.0022(17) 0.0033(18) C41 0.023(2) 0.017(2) 0.018(2) -0.0005(18) -0.0004(19) -0.0044(18) C42 0.028(3) 0.038(3) 0.023(3) 0.011(2) 0.002(2) -0.002(2) C43 0.050(4) 0.036(3) 0.023(3) 0.010(2) -0.005(2) -0.002(3) C44 0.059(4) 0.020(3) 0.025(3) 0.004(2) 0.012(3) 0.002(2) C45 0.043(3) 0.043(4) 0.044(4) 0.012(3) 0.024(3) -0.004(3) C46 0.026(3) 0.046(4) 0.033(3) 0.018(3) 0.004(2) -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.3395(14) . ? Pd1 P2 2.3507(15) . ? Pd1 Se1 2.4521(6) . ? Pd1 Se2 2.4544(5) . ? Se1 C1 1.896(4) . ? Se2 C6 1.906(4) . ? P1 C23 1.821(5) . ? P1 C17 1.836(4) . ? P1 C11 1.845(5) . ? P2 C35 1.817(4) . ? P2 C29 1.830(5) . ? P2 C41 1.838(5) . ? N1 C3 1.310(8) . ? N1 C4 1.355(9) . ? N2 C8 1.333(7) . ? N2 C9 1.338(8) . ? C1 C2 1.383(7) . ? C1 C5 1.390(7) . ? C2 C3 1.397(7) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.374(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.381(7) . ? C6 C7 1.391(6) . ? C7 C8 1.358(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.378(8) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.398(7) . ? C11 C16 1.418(8) . ? C12 C13 1.376(8) . ? C12 H12 0.9500 . ? C13 C14 1.363(10) . ? C13 H13 0.9500 . ? C14 C15 1.380(9) . ? C14 H14 0.9500 . ? C15 C16 1.392(8) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.373(7) . ? C17 C22 1.386(7) . ? C18 C19 1.385(7) . ? C18 H18 0.9500 . ? C19 C20 1.364(9) . ? C19 H19 0.9500 . ? C20 C21 1.385(8) . ? C20 H20 0.9500 . ? C21 C22 1.387(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.396(7) . ? C23 C28 1.404(7) . ? C24 C25 1.348(8) . ? C24 H24 0.9500 . ? C25 C26 1.407(8) . ? C25 H25 0.9500 . ? C26 C27 1.371(8) . ? C26 H26 0.9500 . ? C27 C28 1.393(7) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.340(8) . ? C29 C30 1.393(8) . ? C30 C31 1.372(9) . ? C30 H30 0.9500 . ? C31 C32 1.396(9) . ? C31 H31 0.9500 . ? C32 C33 1.339(9) . ? C32 H32 0.9500 . ? C33 C34 1.395(8) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C40 1.391(7) . ? C35 C36 1.396(7) . ? C36 C37 1.400(7) . ? C36 H36 0.9500 . ? C37 C38 1.376(8) . ? C37 H37 0.9500 . ? C38 C39 1.370(8) . ? C38 H38 0.9500 . ? C39 C40 1.383(7) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.364(7) . ? C41 C46 1.417(7) . ? C42 C43 1.397(7) . ? C42 H42 0.9500 . ? C43 C44 1.364(9) . ? C43 H43 0.9500 . ? C44 C45 1.356(9) . ? C44 H44 0.9500 . ? C45 C46 1.387(8) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 P2 177.05(4) . . ? P1 Pd1 Se1 85.25(3) . . ? P2 Pd1 Se1 96.62(3) . . ? P1 Pd1 Se2 93.08(3) . . ? P2 Pd1 Se2 85.00(3) . . ? Se1 Pd1 Se2 177.99(2) . . ? C1 Se1 Pd1 106.16(14) . . ? C6 Se2 Pd1 102.41(13) . . ? C23 P1 C17 103.2(2) . . ? C23 P1 C11 101.0(2) . . ? C17 P1 C11 106.5(2) . . ? C23 P1 Pd1 119.53(16) . . ? C17 P1 Pd1 111.17(16) . . ? C11 P1 Pd1 114.10(18) . . ? C35 P2 C29 106.4(2) . . ? C35 P2 C41 102.1(2) . . ? C29 P2 C41 104.7(2) . . ? C35 P2 Pd1 112.29(17) . . ? C29 P2 Pd1 108.28(18) . . ? C41 P2 Pd1 121.95(17) . . ? C3 N1 C4 116.4(5) . . ? C8 N2 C9 114.6(5) . . ? C2 C1 C5 116.3(4) . . ? C2 C1 Se1 124.8(4) . . ? C5 C1 Se1 118.8(4) . . ? C1 C2 C3 119.7(5) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? N1 C3 C2 124.0(5) . . ? N1 C3 H3 118.0 . . ? C2 C3 H3 118.0 . . ? N1 C4 C5 123.3(6) . . ? N1 C4 H4 118.4 . . ? C5 C4 H4 118.4 . . ? C4 C5 C1 120.2(5) . . ? C4 C5 H5 119.9 . . ? C1 C5 H5 119.9 . . ? C10 C6 C7 116.8(4) . . ? C10 C6 Se2 123.7(4) . . ? C7 C6 Se2 119.5(4) . . ? C8 C7 C6 119.2(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? N2 C8 C7 125.5(5) . . ? N2 C8 H8 117.2 . . ? C7 C8 H8 117.2 . . ? N2 C9 C10 124.6(5) . . ? N2 C9 H9 117.7 . . ? C10 C9 H9 117.7 . . ? C9 C10 C6 119.3(5) . . ? C9 C10 H10 120.4 . . ? C6 C10 H10 120.4 . . ? C12 C11 C16 118.5(5) . . ? C12 C11 P1 120.6(4) . . ? C16 C11 P1 120.9(4) . . ? C13 C12 C11 121.0(6) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.3(6) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C16 120.9(6) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 118.9(6) . . ? C15 C16 H16 120.6 . . ? C11 C16 H16 120.6 . . ? C18 C17 C22 119.5(4) . . ? C18 C17 P1 121.8(4) . . ? C22 C17 P1 118.7(4) . . ? C17 C18 C19 120.7(5) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 120.2(5) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C20 C21 C22 120.4(5) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 119.6(5) . . ? C17 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C28 118.4(4) . . ? C24 C23 P1 120.0(4) . . ? C28 C23 P1 121.6(4) . . ? C25 C24 C23 121.3(5) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 120.6(5) . . ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 119.2(5) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 120.6(5) . . ? C26 C27 H27 119.7 . . ? C28 C27 H27 119.7 . . ? C27 C28 C23 119.9(5) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? C34 C29 C30 118.6(5) . . ? C34 C29 P2 121.2(4) . . ? C30 C29 P2 119.7(4) . . ? C31 C30 C29 121.0(6) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 119.4(6) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C33 C32 C31 118.7(5) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 121.6(6) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C29 C34 C33 120.5(6) . . ? C29 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C40 C35 C36 119.1(4) . . ? C40 C35 P2 118.4(4) . . ? C36 C35 P2 122.6(4) . . ? C35 C36 C37 119.6(5) . . ? C35 C36 H36 120.2 . . ? C37 C36 H36 120.2 . . ? C38 C37 C36 119.9(5) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 120.8(5) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C38 C39 C40 119.9(5) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? C39 C40 C35 120.7(4) . . ? C39 C40 H40 119.6 . . ? C35 C40 H40 119.6 . . ? C42 C41 C46 117.3(5) . . ? C42 C41 P2 122.6(4) . . ? C46 C41 P2 119.7(4) . . ? C41 C42 C43 121.1(5) . . ? C41 C42 H42 119.4 . . ? C43 C42 H42 119.4 . . ? C44 C43 C42 120.8(5) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C45 C44 C43 119.5(5) . . ? C45 C44 H44 120.2 . . ? C43 C44 H44 120.2 . . ? C44 C45 C46 120.7(6) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C45 C46 C41 120.4(5) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 Se1 C1 -121.8(2) . . . . ? P2 Pd1 Se1 C1 60.4(2) . . . . ? Se2 Pd1 Se1 C1 -155.9(8) . . . . ? P1 Pd1 Se2 C6 -66.13(17) . . . . ? P2 Pd1 Se2 C6 111.62(17) . . . . ? Se1 Pd1 Se2 C6 -32.2(8) . . . . ? P2 Pd1 P1 C23 -39.0(9) . . . . ? Se1 Pd1 P1 C23 -168.57(19) . . . . ? Se2 Pd1 P1 C23 10.30(19) . . . . ? P2 Pd1 P1 C17 81.0(9) . . . . ? Se1 Pd1 P1 C17 -48.57(16) . . . . ? Se2 Pd1 P1 C17 130.30(16) . . . . ? P2 Pd1 P1 C11 -158.6(9) . . . . ? Se1 Pd1 P1 C11 71.87(18) . . . . ? Se2 Pd1 P1 C11 -109.26(18) . . . . ? P1 Pd1 P2 C35 96.4(9) . . . . ? Se1 Pd1 P2 C35 -134.31(16) . . . . ? Se2 Pd1 P2 C35 46.89(16) . . . . ? P1 Pd1 P2 C29 -20.7(9) . . . . ? Se1 Pd1 P2 C29 108.56(18) . . . . ? Se2 Pd1 P2 C29 -70.25(18) . . . . ? P1 Pd1 P2 C41 -142.1(9) . . . . ? Se1 Pd1 P2 C41 -12.82(18) . . . . ? Se2 Pd1 P2 C41 168.38(18) . . . . ? Pd1 Se1 C1 C2 11.6(6) . . . . ? Pd1 Se1 C1 C5 -171.8(5) . . . . ? C5 C1 C2 C3 2.3(9) . . . . ? Se1 C1 C2 C3 178.9(5) . . . . ? C4 N1 C3 C2 -1.3(10) . . . . ? C1 C2 C3 N1 -0.9(11) . . . . ? C3 N1 C4 C5 1.9(10) . . . . ? N1 C4 C5 C1 -0.4(10) . . . . ? C2 C1 C5 C4 -1.7(10) . . . . ? Se1 C1 C5 C4 -178.6(5) . . . . ? Pd1 Se2 C6 C10 -25.7(5) . . . . ? Pd1 Se2 C6 C7 155.8(4) . . . . ? C10 C6 C7 C8 1.4(7) . . . . ? Se2 C6 C7 C8 -180.0(4) . . . . ? C9 N2 C8 C7 -0.6(8) . . . . ? C6 C7 C8 N2 0.1(9) . . . . ? C8 N2 C9 C10 -0.4(8) . . . . ? N2 C9 C10 C6 1.9(8) . . . . ? C7 C6 C10 C9 -2.3(7) . . . . ? Se2 C6 C10 C9 179.1(4) . . . . ? C23 P1 C11 C12 -148.1(4) . . . . ? C17 P1 C11 C12 104.5(4) . . . . ? Pd1 P1 C11 C12 -18.5(5) . . . . ? C23 P1 C11 C16 34.2(5) . . . . ? C17 P1 C11 C16 -73.2(5) . . . . ? Pd1 P1 C11 C16 163.8(4) . . . . ? C16 C11 C12 C13 0.7(8) . . . . ? P1 C11 C12 C13 -177.1(4) . . . . ? C11 C12 C13 C14 1.6(9) . . . . ? C12 C13 C14 C15 -3.2(10) . . . . ? C13 C14 C15 C16 2.7(11) . . . . ? C14 C15 C16 C11 -0.4(10) . . . . ? C12 C11 C16 C15 -1.2(9) . . . . ? P1 C11 C16 C15 176.5(5) . . . . ? C23 P1 C17 C18 -79.1(4) . . . . ? C11 P1 C17 C18 26.7(5) . . . . ? Pd1 P1 C17 C18 151.6(4) . . . . ? C23 P1 C17 C22 97.9(4) . . . . ? C11 P1 C17 C22 -156.3(4) . . . . ? Pd1 P1 C17 C22 -31.4(4) . . . . ? C22 C17 C18 C19 0.5(8) . . . . ? P1 C17 C18 C19 177.5(4) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C18 C19 C20 C21 0.6(8) . . . . ? C19 C20 C21 C22 0.7(8) . . . . ? C18 C17 C22 C21 0.8(7) . . . . ? P1 C17 C22 C21 -176.3(4) . . . . ? C20 C21 C22 C17 -1.3(7) . . . . ? C17 P1 C23 C24 161.4(4) . . . . ? C11 P1 C23 C24 51.4(5) . . . . ? Pd1 P1 C23 C24 -74.6(4) . . . . ? C17 P1 C23 C28 -17.2(5) . . . . ? C11 P1 C23 C28 -127.2(4) . . . . ? Pd1 P1 C23 C28 106.8(4) . . . . ? C28 C23 C24 C25 -0.6(8) . . . . ? P1 C23 C24 C25 -179.3(4) . . . . ? C23 C24 C25 C26 0.4(9) . . . . ? C24 C25 C26 C27 -0.3(9) . . . . ? C25 C26 C27 C28 0.4(8) . . . . ? C26 C27 C28 C23 -0.6(8) . . . . ? C24 C23 C28 C27 0.7(7) . . . . ? P1 C23 C28 C27 179.3(4) . . . . ? C35 P2 C29 C34 -33.8(5) . . . . ? C41 P2 C29 C34 -141.4(5) . . . . ? Pd1 P2 C29 C34 87.1(5) . . . . ? C35 P2 C29 C30 154.7(5) . . . . ? C41 P2 C29 C30 47.1(5) . . . . ? Pd1 P2 C29 C30 -84.4(5) . . . . ? C34 C29 C30 C31 4.1(10) . . . . ? P2 C29 C30 C31 175.9(5) . . . . ? C29 C30 C31 C32 -1.6(11) . . . . ? C30 C31 C32 C33 -2.2(11) . . . . ? C31 C32 C33 C34 3.6(10) . . . . ? C30 C29 C34 C33 -2.8(9) . . . . ? P2 C29 C34 C33 -174.4(5) . . . . ? C32 C33 C34 C29 -1.1(10) . . . . ? C29 P2 C35 C40 146.6(4) . . . . ? C41 P2 C35 C40 -103.9(4) . . . . ? Pd1 P2 C35 C40 28.4(4) . . . . ? C29 P2 C35 C36 -35.8(5) . . . . ? C41 P2 C35 C36 73.6(4) . . . . ? Pd1 P2 C35 C36 -154.1(4) . . . . ? C40 C35 C36 C37 -0.9(7) . . . . ? P2 C35 C36 C37 -178.4(4) . . . . ? C35 C36 C37 C38 0.9(8) . . . . ? C36 C37 C38 C39 0.3(9) . . . . ? C37 C38 C39 C40 -1.4(8) . . . . ? C38 C39 C40 C35 1.4(7) . . . . ? C36 C35 C40 C39 -0.2(7) . . . . ? P2 C35 C40 C39 177.4(4) . . . . ? C35 P2 C41 C42 7.0(5) . . . . ? C29 P2 C41 C42 117.7(5) . . . . ? Pd1 P2 C41 C42 -119.2(4) . . . . ? C35 P2 C41 C46 -179.9(5) . . . . ? C29 P2 C41 C46 -69.2(5) . . . . ? Pd1 P2 C41 C46 53.8(5) . . . . ? C46 C41 C42 C43 2.1(8) . . . . ? P2 C41 C42 C43 175.3(4) . . . . ? C41 C42 C43 C44 0.2(9) . . . . ? C42 C43 C44 C45 -1.1(9) . . . . ? C43 C44 C45 C46 -0.4(10) . . . . ? C44 C45 C46 C41 2.8(10) . . . . ? C42 C41 C46 C45 -3.6(9) . . . . ? P2 C41 C46 C45 -177.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.155 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.130 _database_code_depnum_ccdc_archive 'CCDC 924434' ####################################################################### # # 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_pca21 #TrackingRef 'web_deposit_cif_file_3_Dr.SandipDey_1360841986.pca21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H38 N2 P2 Pt Se2' _chemical_formula_weight 745.49 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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 19.975(3) _cell_length_b 9.0763(15) _cell_length_c 14.380(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2607.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9936 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.899 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 8.309 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1245 _exptl_absorpt_correction_T_max 0.2404 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'APEX II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 27666 _diffrn_reflns_av_R_equivalents 0.0558 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.50 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 5919 _reflns_number_gt 5442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; APEX-II(BRUKER-NONIUS, 2003) ; _computing_data_reduction APEX-II _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.085(6) _refine_ls_number_reflns 5919 _refine_ls_number_parameters 262 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0281 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0511 _refine_ls_wR_factor_gt 0.0499 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7408(2) 0.1193(4) 0.6122(3) 0.0133(9) Uani 1 1 d . . . C2 C 0.6990(2) 0.1080(5) 0.6895(3) 0.0156(10) Uani 1 1 d . . . H2 H 0.6562 0.1537 0.6895 0.019 Uiso 1 1 calc R . . C3 C 0.7206(2) 0.0296(5) 0.7660(3) 0.0184(10) Uani 1 1 d . . . H3 H 0.6908 0.0211 0.8172 0.022 Uiso 1 1 calc R . . C4 C 0.8199(2) -0.0210(5) 0.6996(3) 0.0178(10) Uani 1 1 d . . . H4 H 0.8632 -0.0643 0.7028 0.021 Uiso 1 1 calc R . . C5 C 0.8031(2) 0.0513(5) 0.6191(3) 0.0124(9) Uani 1 1 d . . . H5 H 0.8336 0.0550 0.5685 0.015 Uiso 1 1 calc R . . C6 C 0.5016(2) 0.6330(5) 0.5016(3) 0.0146(7) Uani 1 1 d . . . C7 C 0.5383(2) 0.6460(5) 0.4188(3) 0.0146(7) Uani 1 1 d . . . H7 H 0.5817 0.6040 0.4135 0.018 Uiso 1 1 calc R . . C8 C 0.5100(2) 0.7211(5) 0.3453(4) 0.0191(11) Uani 1 1 d . . . H8 H 0.5356 0.7271 0.2897 0.023 Uiso 1 1 calc R . . C9 C 0.4157(2) 0.7712(5) 0.4241(4) 0.0179(10) Uani 1 1 d . . . H9 H 0.3725 0.8143 0.4266 0.021 Uiso 1 1 calc R . . C10 C 0.4382(2) 0.6972(4) 0.5035(4) 0.0138(9) Uani 1 1 d . . . H10 H 0.4110 0.6908 0.5574 0.017 Uiso 1 1 calc R . . C11 C 0.6781(2) 0.5975(5) 0.7389(3) 0.0177(10) Uani 1 1 d U . . H11A H 0.7115 0.6708 0.7601 0.021 Uiso 1 1 calc R . . H11B H 0.6336 0.6454 0.7400 0.021 Uiso 1 1 calc R . . C12 C 0.6778(4) 0.4688(7) 0.8055(4) 0.0465(18) Uani 1 1 d U . . H12A H 0.6490 0.3906 0.7810 0.070 Uiso 1 1 calc R . . H12B H 0.6607 0.5012 0.8661 0.070 Uiso 1 1 calc R . . H12C H 0.7235 0.4313 0.8128 0.070 Uiso 1 1 calc R . . C13 C 0.7864(2) 0.4917(5) 0.6235(3) 0.0168(11) Uani 1 1 d . . . H13A H 0.7907 0.4016 0.6618 0.020 Uiso 1 1 calc R . . H13B H 0.8006 0.4659 0.5595 0.020 Uiso 1 1 calc R . . C14 C 0.8346(2) 0.6056(6) 0.6610(4) 0.0236(12) Uani 1 1 d . . . H14A H 0.8332 0.6937 0.6216 0.035 Uiso 1 1 calc R . . H14B H 0.8801 0.5650 0.6610 0.035 Uiso 1 1 calc R . . H14C H 0.8218 0.6319 0.7246 0.035 Uiso 1 1 calc R . . C15 C 0.6962(2) 0.7195(5) 0.5575(4) 0.0187(10) Uani 1 1 d . . . H15A H 0.6493 0.7548 0.5542 0.022 Uiso 1 1 calc R . . H15B H 0.7221 0.7927 0.5937 0.022 Uiso 1 1 calc R . . C16 C 0.7238(3) 0.7132(7) 0.4617(4) 0.0296(14) Uani 1 1 d . . . H16A H 0.7156 0.8072 0.4302 0.044 Uiso 1 1 calc R . . H16B H 0.7020 0.6335 0.4272 0.044 Uiso 1 1 calc R . . H16C H 0.7721 0.6948 0.4646 0.044 Uiso 1 1 calc R . . C17 C 0.5814(2) 0.1664(5) 0.3577(3) 0.0158(10) Uani 1 1 d . . . H17A H 0.6220 0.1045 0.3629 0.019 Uiso 1 1 calc R . . H17B H 0.5461 0.1064 0.3276 0.019 Uiso 1 1 calc R . . C18 C 0.5970(3) 0.2986(6) 0.2955(4) 0.0269(12) Uani 1 1 d . . . H18A H 0.6092 0.2639 0.2332 0.040 Uiso 1 1 calc R . . H18B H 0.6345 0.3543 0.3220 0.040 Uiso 1 1 calc R . . H18C H 0.5575 0.3623 0.2914 0.040 Uiso 1 1 calc R . . C19 C 0.4670(2) 0.2753(6) 0.4562(4) 0.0204(11) Uani 1 1 d . . . H19A H 0.4482 0.3039 0.5173 0.024 Uiso 1 1 calc R . . H19B H 0.4674 0.3646 0.4167 0.024 Uiso 1 1 calc R . . C20 C 0.4205(2) 0.1651(5) 0.4126(4) 0.0246(12) Uani 1 1 d . . . H20A H 0.4378 0.1363 0.3514 0.037 Uiso 1 1 calc R . . H20B H 0.3760 0.2092 0.4053 0.037 Uiso 1 1 calc R . . H20C H 0.4173 0.0779 0.4525 0.037 Uiso 1 1 calc R . . C21 C 0.5478(2) 0.0372(5) 0.5304(3) 0.0152(10) Uani 1 1 d U . . H21A H 0.5239 -0.0312 0.4882 0.018 Uiso 1 1 calc R . . H21B H 0.5936 -0.0019 0.5395 0.018 Uiso 1 1 calc R . . C22 C 0.5115(3) 0.0383(7) 0.6252(4) 0.0292(13) Uani 1 1 d U . . H22A H 0.4644 0.0646 0.6160 0.044 Uiso 1 1 calc R . . H22B H 0.5327 0.1107 0.6662 0.044 Uiso 1 1 calc R . . H22C H 0.5144 -0.0597 0.6535 0.044 Uiso 1 1 calc R . . N1 N 0.7804(2) -0.0352(4) 0.7733(3) 0.0205(9) Uani 1 1 d . . . N2 N 0.4502(2) 0.7860(5) 0.3451(3) 0.0215(9) Uani 1 1 d . . . P1 P 0.55365(6) 0.21671(13) 0.47401(8) 0.0121(2) Uani 1 1 d . . . P2 P 0.69757(6) 0.54359(13) 0.61990(8) 0.0107(2) Uani 1 1 d . . . Pt1 Pt 0.624952(7) 0.377407(16) 0.55061(2) 0.00896(4) Uani 1 1 d . . . Se1 Se 0.71593(2) 0.21360(5) 0.49973(3) 0.01271(10) Uani 1 1 d . . . Se2 Se 0.53341(2) 0.53303(5) 0.60872(3) 0.01296(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.013(2) 0.007(2) 0.020(2) -0.003(2) -0.0025(19) 0.0000(16) C2 0.010(2) 0.015(3) 0.022(3) -0.002(2) 0.0004(19) 0.0033(18) C3 0.021(3) 0.013(2) 0.021(3) 0.001(2) 0.009(2) 0.001(2) C4 0.013(2) 0.011(2) 0.029(3) -0.003(2) -0.006(2) 0.0004(19) C5 0.011(2) 0.006(2) 0.020(2) -0.0012(19) 0.0009(19) -0.0019(17) C6 0.0101(15) 0.0101(16) 0.0235(19) -0.0009(14) 0.0020(14) -0.0010(12) C7 0.0101(15) 0.0101(16) 0.0235(19) -0.0009(14) 0.0020(14) -0.0010(12) C8 0.018(2) 0.019(3) 0.021(3) 0.003(2) 0.005(2) 0.000(2) C9 0.014(2) 0.014(3) 0.026(3) -0.006(2) -0.003(2) 0.0032(19) C10 0.011(2) 0.006(2) 0.024(2) -0.004(2) 0.003(2) 0.0001(17) C11 0.019(2) 0.017(2) 0.017(2) -0.003(2) -0.001(2) -0.002(2) C12 0.089(5) 0.031(4) 0.020(3) 0.000(3) 0.006(3) -0.018(4) C13 0.012(2) 0.015(2) 0.024(3) -0.0018(19) -0.004(2) -0.0017(18) C14 0.011(2) 0.019(3) 0.042(3) 0.002(2) -0.003(2) 0.000(2) C15 0.016(2) 0.007(2) 0.033(3) 0.001(3) -0.004(2) -0.0019(16) C16 0.024(3) 0.032(3) 0.033(3) 0.016(3) 0.002(3) -0.004(2) C17 0.015(2) 0.013(2) 0.020(3) -0.0021(19) -0.0023(19) 0.0012(19) C18 0.038(3) 0.023(3) 0.020(3) 0.006(2) 0.005(2) 0.005(3) C19 0.013(2) 0.017(3) 0.031(3) -0.007(2) -0.001(2) -0.001(2) C20 0.014(2) 0.014(3) 0.046(3) -0.006(2) -0.005(2) 0.000(2) C21 0.021(2) 0.010(2) 0.014(3) 0.0017(17) 0.0012(18) -0.0080(18) C22 0.030(3) 0.030(3) 0.028(3) 0.000(3) 0.002(2) -0.008(3) N1 0.025(2) 0.015(2) 0.022(2) 0.0032(18) -0.0062(18) 0.0020(19) N2 0.022(2) 0.014(2) 0.029(2) 0.0026(19) -0.0028(19) 0.0011(18) P1 0.0109(6) 0.0096(6) 0.0159(6) -0.0011(5) 0.0013(5) -0.0007(5) P2 0.0105(5) 0.0065(6) 0.0150(6) 0.0009(5) 0.0002(5) 0.0007(4) Pt1 0.00786(7) 0.00596(7) 0.01306(7) 0.00040(8) 0.00053(7) 0.00067(5) Se1 0.0118(2) 0.0114(2) 0.0150(2) -0.0003(2) 0.00127(19) 0.00384(18) Se2 0.0103(2) 0.0118(2) 0.0168(2) -0.0015(2) 0.0010(2) 0.00300(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.392(6) . ? C1 C2 1.394(6) . ? C1 Se1 1.896(5) . ? C2 C3 1.379(7) . ? C2 H2 0.9500 . ? C3 N1 1.336(6) . ? C3 H3 0.9500 . ? C4 N1 1.328(6) . ? C4 C5 1.373(7) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.393(6) . ? C6 C7 1.403(7) . ? C6 Se2 1.897(5) . ? C7 C8 1.378(7) . ? C7 H7 0.9500 . ? C8 N2 1.332(6) . ? C8 H8 0.9500 . ? C9 N2 1.335(6) . ? C9 C10 1.399(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.511(7) . ? C11 P2 1.821(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.512(6) . ? C13 P2 1.837(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.485(8) . ? C15 P2 1.832(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.528(7) . ? C17 P1 1.821(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.502(7) . ? C19 P1 1.829(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.543(6) . ? C21 P1 1.824(5) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? P1 Pt1 2.3171(12) . ? P2 Pt1 2.3178(12) . ? Pt1 Se2 2.4570(5) . ? Pt1 Se1 2.4594(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 C5 C1 C2 116.5(4) . . ? C5 C1 Se1 119.7(4) . . ? C2 C1 Se1 123.8(3) . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? N1 C3 C2 124.7(4) . . ? N1 C3 H3 117.6 . . ? C2 C3 H3 117.6 . . ? N1 C4 C5 125.0(4) . . ? N1 C4 H4 117.5 . . ? C5 C4 H4 117.5 . . ? C4 C5 C1 119.4(4) . . ? C4 C5 H5 120.3 . . ? C1 C5 H5 120.3 . . ? C10 C6 C7 117.1(4) . . ? C10 C6 Se2 119.2(4) . . ? C7 C6 Se2 123.7(3) . . ? C8 C7 C6 118.6(4) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? N2 C8 C7 126.0(5) . . ? N2 C8 H8 117.0 . . ? C7 C8 H8 117.0 . . ? N2 C9 C10 125.2(4) . . ? N2 C9 H9 117.4 . . ? C10 C9 H9 117.4 . . ? C6 C10 C9 118.5(5) . . ? C6 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C12 C11 P2 112.9(4) . . ? C12 C11 H11A 109.0 . . ? P2 C11 H11A 109.0 . . ? C12 C11 H11B 109.0 . . ? P2 C11 H11B 109.0 . . ? H11A C11 H11B 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P2 116.7(3) . . ? C14 C13 H13A 108.1 . . ? P2 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? P2 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 P2 114.5(4) . . ? C16 C15 H15A 108.6 . . ? P2 C15 H15A 108.6 . . ? C16 C15 H15B 108.6 . . ? P2 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 P1 113.8(3) . . ? C18 C17 H17A 108.8 . . ? P1 C17 H17A 108.8 . . ? C18 C17 H17B 108.8 . . ? P1 C17 H17B 108.8 . . ? H17A C17 H17B 107.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 P1 116.8(4) . . ? C20 C19 H19A 108.1 . . ? P1 C19 H19A 108.1 . . ? C20 C19 H19B 108.1 . . ? P1 C19 H19B 108.1 . . ? H19A C19 H19B 107.3 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P1 114.6(4) . . ? C22 C21 H21A 108.6 . . ? P1 C21 H21A 108.6 . . ? C22 C21 H21B 108.6 . . ? P1 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4 N1 C3 115.2(4) . . ? C8 N2 C9 114.6(4) . . ? C17 P1 C21 101.8(2) . . ? C17 P1 C19 103.4(2) . . ? C21 P1 C19 105.1(2) . . ? C17 P1 Pt1 114.06(16) . . ? C21 P1 Pt1 112.99(15) . . ? C19 P1 Pt1 117.73(16) . . ? C11 P2 C15 102.9(2) . . ? C11 P2 C13 104.4(2) . . ? C15 P2 C13 104.6(2) . . ? C11 P2 Pt1 116.42(16) . . ? C15 P2 Pt1 110.31(17) . . ? C13 P2 Pt1 116.73(15) . . ? P1 Pt1 P2 177.05(5) . . ? P1 Pt1 Se2 93.79(3) . . ? P2 Pt1 Se2 86.87(3) . . ? P1 Pt1 Se1 86.12(3) . . ? P2 Pt1 Se1 93.37(3) . . ? Se2 Pt1 Se1 177.01(2) . . ? C1 Se1 Pt1 102.29(14) . . ? C6 Se2 Pt1 104.36(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -1.3(6) . . . . ? Se1 C1 C2 C3 176.3(3) . . . . ? C1 C2 C3 N1 1.7(7) . . . . ? N1 C4 C5 C1 1.5(7) . . . . ? C2 C1 C5 C4 -0.2(6) . . . . ? Se1 C1 C5 C4 -177.8(3) . . . . ? C10 C6 C7 C8 0.3(6) . . . . ? Se2 C6 C7 C8 179.9(3) . . . . ? C6 C7 C8 N2 0.9(8) . . . . ? C7 C6 C10 C9 -0.8(6) . . . . ? Se2 C6 C10 C9 179.6(3) . . . . ? N2 C9 C10 C6 0.1(7) . . . . ? C5 C4 N1 C3 -1.1(7) . . . . ? C2 C3 N1 C4 -0.6(7) . . . . ? C7 C8 N2 C9 -1.6(7) . . . . ? C10 C9 N2 C8 1.1(7) . . . . ? C18 C17 P1 C21 -174.7(4) . . . . ? C18 C17 P1 C19 76.4(4) . . . . ? C18 C17 P1 Pt1 -52.7(4) . . . . ? C22 C21 P1 C17 -168.1(4) . . . . ? C22 C21 P1 C19 -60.6(4) . . . . ? C22 C21 P1 Pt1 69.1(4) . . . . ? C20 C19 P1 C17 57.5(5) . . . . ? C20 C19 P1 C21 -48.9(5) . . . . ? C20 C19 P1 Pt1 -175.7(3) . . . . ? C12 C11 P2 C15 -178.7(4) . . . . ? C12 C11 P2 C13 -69.7(5) . . . . ? C12 C11 P2 Pt1 60.6(4) . . . . ? C16 C15 P2 C11 168.3(4) . . . . ? C16 C15 P2 C13 59.4(4) . . . . ? C16 C15 P2 Pt1 -66.9(4) . . . . ? C14 C13 P2 C11 -55.1(4) . . . . ? C14 C13 P2 C15 52.6(5) . . . . ? C14 C13 P2 Pt1 174.8(3) . . . . ? C17 P1 Pt1 P2 33.2(9) . . . . ? C21 P1 Pt1 P2 148.8(8) . . . . ? C19 P1 Pt1 P2 -88.3(9) . . . . ? C17 P1 Pt1 Se2 136.06(17) . . . . ? C21 P1 Pt1 Se2 -108.32(17) . . . . ? C19 P1 Pt1 Se2 14.6(2) . . . . ? C17 P1 Pt1 Se1 -46.94(17) . . . . ? C21 P1 Pt1 Se1 68.69(17) . . . . ? C19 P1 Pt1 Se1 -168.4(2) . . . . ? C11 P2 Pt1 P1 150.2(8) . . . . ? C15 P2 Pt1 P1 33.5(9) . . . . ? C13 P2 Pt1 P1 -85.7(9) . . . . ? C11 P2 Pt1 Se2 47.10(18) . . . . ? C15 P2 Pt1 Se2 -69.58(18) . . . . ? C13 P2 Pt1 Se2 171.28(19) . . . . ? C11 P2 Pt1 Se1 -129.92(18) . . . . ? C15 P2 Pt1 Se1 113.40(18) . . . . ? C13 P2 Pt1 Se1 -5.74(19) . . . . ? C5 C1 Se1 Pt1 -160.8(3) . . . . ? C2 C1 Se1 Pt1 21.8(4) . . . . ? P1 Pt1 Se1 C1 -107.71(13) . . . . ? P2 Pt1 Se1 C1 75.20(13) . . . . ? Se2 Pt1 Se1 C1 -19.4(4) . . . . ? C10 C6 Se2 Pt1 161.5(3) . . . . ? C7 C6 Se2 Pt1 -18.1(4) . . . . ? P1 Pt1 Se2 C6 -71.49(14) . . . . ? P2 Pt1 Se2 C6 105.64(14) . . . . ? Se1 Pt1 Se2 C6 -159.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.445 _refine_diff_density_min -1.015 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 924435' ####################################################################### # # 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_sdb1 #TrackingRef 'web_deposit_cif_file_4_Dr.SandipDey_1360841986.sdb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H36 N2 O2 P2 Pd Se2' _chemical_formula_weight 854.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7931(8) _cell_length_b 10.5303(5) _cell_length_c 21.2888(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.650(3) _cell_angle_gamma 90.00 _cell_volume 3409.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 4816 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 61.67 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.666 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1704 _exptl_absorpt_coefficient_mu 7.999 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4228 _exptl_absorpt_correction_T_max 0.7953 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9607 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_sigmaI/netI 0.0573 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 59.99 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 5063 _reflns_number_gt 3976 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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. The crystal used had two twin components as was found from CELL_NOW. Integration was done using APEX2 including both the components. TWINABS was used for absorption correction as well as to separate one twin component. 64570 data ( 9947 unique ) involve domain 1 only, mean I/sigma 2.8 64417 data ( 9950 unique ) involve domain 2 only, mean I/sigma 2.6 Only the first component was used for structure solution as well as the least squares refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(1.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0466P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^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 5063 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0446 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0828 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 0.20069(2) 0.04138(3) 0.932446(16) 0.01391(11) Uani 1 1 d . . . Se1 Se 0.22464(3) -0.18384(5) 0.90875(3) 0.02204(15) Uani 1 1 d . . . Se2 Se 0.23384(3) 0.00487(5) 1.05159(2) 0.01917(14) Uani 1 1 d . . . P1 P 0.17107(7) 0.24744(12) 0.94944(6) 0.0159(3) Uani 1 1 d . . . P2 P 0.14443(8) 0.08629(12) 0.82508(6) 0.0153(3) Uani 1 1 d . . . N1 N 0.4619(3) -0.2047(5) 0.8134(2) 0.0358(12) Uani 1 1 d . . . N2 N 0.5037(3) -0.2172(5) 1.1135(2) 0.0324(11) Uani 1 1 d . . . C1 C 0.3200(3) -0.1900(5) 0.8695(3) 0.0258(12) Uani 1 1 d . . . C2 C 0.3454(3) -0.3083(6) 0.8473(3) 0.0319(14) Uani 1 1 d . . . H2 H 0.3146 -0.3837 0.8518 0.038 Uiso 1 1 calc R . . C3 C 0.4105(4) -0.3130(6) 0.8208(3) 0.0374(16) Uani 1 1 d . . . H3 H 0.4249 -0.3928 0.8056 0.045 Uiso 1 1 calc R . . C4 C 0.4396(4) -0.0982(5) 0.8336(3) 0.0308(13) Uani 1 1 d . . . H4 H 0.4726 -0.0249 0.8293 0.037 Uiso 1 1 calc R . . C5 C 0.3683(3) -0.0836(6) 0.8619(3) 0.0287(13) Uani 1 1 d . . . H5 H 0.3540 -0.0023 0.8755 0.034 Uiso 1 1 calc R . . C6 C 0.3435(3) -0.0841(5) 1.0747(2) 0.0194(11) Uani 1 1 d . . . C7 C 0.4010(3) -0.0867(5) 1.0359(3) 0.0235(12) Uani 1 1 d . . . H7 H 0.3870 -0.0433 0.9953 0.028 Uiso 1 1 calc R . . C8 C 0.4789(3) -0.1528(5) 1.0568(3) 0.0275(13) Uani 1 1 d . . . H8 H 0.5175 -0.1529 1.0294 0.033 Uiso 1 1 calc R . . C9 C 0.4476(3) -0.2119(5) 1.1511(3) 0.0304(13) Uani 1 1 d . . . H9 H 0.4634 -0.2557 1.1917 0.036 Uiso 1 1 calc R . . C10 C 0.3689(3) -0.1473(5) 1.1347(2) 0.0228(12) Uani 1 1 d . . . H10 H 0.3325 -0.1455 1.1637 0.027 Uiso 1 1 calc R . . C11 C 0.2682(3) 0.3448(5) 0.9830(2) 0.0186(11) Uani 1 1 d . . . C12 C 0.3472(3) 0.2850(5) 1.0109(2) 0.0244(12) Uani 1 1 d . . . H12 H 0.3509 0.1949 1.0110 0.029 Uiso 1 1 calc R . . C13 C 0.4219(3) 0.3579(5) 1.0390(3) 0.0301(13) Uani 1 1 d . . . H13 H 0.4765 0.3169 1.0578 0.036 Uiso 1 1 calc R . . C14 C 0.4171(3) 0.4873(5) 1.0397(3) 0.0272(13) Uani 1 1 d . . . H14 H 0.4676 0.5361 1.0602 0.033 Uiso 1 1 calc R . . C15 C 0.3385(3) 0.5468(5) 1.0107(3) 0.0268(12) Uani 1 1 d . . . H15 H 0.3353 0.6369 1.0103 0.032 Uiso 1 1 calc R . . C16 C 0.2642(3) 0.4759(5) 0.9821(3) 0.0257(12) Uani 1 1 d . . . H16 H 0.2104 0.5175 0.9619 0.031 Uiso 1 1 calc R . . C17 C 0.0956(3) 0.2793(5) 0.9986(2) 0.0157(10) Uani 1 1 d . . . C18 C 0.1180(3) 0.3553(5) 1.0533(3) 0.0292(13) Uani 1 1 d . . . H18 H 0.1758 0.3889 1.0680 0.035 Uiso 1 1 calc R . . C19 C 0.0557(3) 0.3830(5) 1.0870(3) 0.0299(13) Uani 1 1 d . . . H19 H 0.0711 0.4356 1.1247 0.036 Uiso 1 1 calc R . . C20 C -0.0270(3) 0.3346(5) 1.0661(2) 0.0236(12) Uani 1 1 d . . . H20 H -0.0694 0.3555 1.0886 0.028 Uiso 1 1 calc R . . C21 C -0.0497(3) 0.2561(5) 1.0128(2) 0.0235(12) Uani 1 1 d . . . H21 H -0.1073 0.2213 0.9991 0.028 Uiso 1 1 calc R . . C22 C 0.0113(3) 0.2281(5) 0.9795(2) 0.0228(11) Uani 1 1 d . . . H22 H -0.0042 0.1728 0.9429 0.027 Uiso 1 1 calc R . . C23 C 0.1144(3) 0.3177(5) 0.8703(2) 0.0177(11) Uani 1 1 d . . . H23A H 0.0503 0.3034 0.8612 0.021 Uiso 1 1 calc R . . H23B H 0.1250 0.4104 0.8715 0.021 Uiso 1 1 calc R . . C24 C 0.1479(3) 0.2581(5) 0.8166(2) 0.0193(11) Uani 1 1 d . . . H24A H 0.2089 0.2862 0.8204 0.023 Uiso 1 1 calc R . . H24B H 0.1105 0.2843 0.7733 0.023 Uiso 1 1 calc R . . C25 C 0.0271(3) 0.0497(5) 0.8042(2) 0.0166(11) Uani 1 1 d . . . C26 C -0.0069(3) -0.0249(5) 0.8453(2) 0.0181(11) Uani 1 1 d . . . H26 H 0.0317 -0.0626 0.8827 0.022 Uiso 1 1 calc R . . C27 C -0.0962(3) -0.0449(5) 0.8322(3) 0.0249(12) Uani 1 1 d . . . H27 H -0.1189 -0.0963 0.8606 0.030 Uiso 1 1 calc R . . C28 C -0.1529(3) 0.0100(5) 0.7777(3) 0.0281(13) Uani 1 1 d . . . H28 H -0.2145 -0.0031 0.7689 0.034 Uiso 1 1 calc R . . C29 C -0.1198(3) 0.0836(5) 0.7365(3) 0.0241(12) Uani 1 1 d . . . H29 H -0.1588 0.1212 0.6992 0.029 Uiso 1 1 calc R . . C30 C -0.0299(3) 0.1035(5) 0.7488(2) 0.0215(11) Uani 1 1 d . . . H30 H -0.0074 0.1533 0.7197 0.026 Uiso 1 1 calc R . . C31 C 0.1837(3) 0.0204(5) 0.7602(2) 0.0195(11) Uani 1 1 d . . . C32 C 0.1521(3) -0.0969(5) 0.7331(2) 0.0240(12) Uani 1 1 d . . . H32 H 0.1083 -0.1401 0.7479 0.029 Uiso 1 1 calc R . . C33 C 0.1843(4) -0.1506(6) 0.6849(3) 0.0385(15) Uani 1 1 d . . . H33 H 0.1632 -0.2311 0.6673 0.046 Uiso 1 1 calc R . . C34 C 0.2465(4) -0.0882(6) 0.6623(3) 0.0412(17) Uani 1 1 d . . . H34 H 0.2672 -0.1247 0.6284 0.049 Uiso 1 1 calc R . . C35 C 0.2791(4) 0.0280(6) 0.6887(3) 0.0367(15) Uani 1 1 d . . . H35 H 0.3231 0.0700 0.6736 0.044 Uiso 1 1 calc R . . C36 C 0.2475(3) 0.0832(6) 0.7372(2) 0.0280(13) Uani 1 1 d . . . H36 H 0.2691 0.1634 0.7548 0.034 Uiso 1 1 calc R . . O50 O 0.6518(2) -0.3712(4) 1.1764(2) 0.0455(11) Uani 1 1 d . . . H50A H 0.6370 -0.3743 1.2120 0.068 Uiso 1 1 d R . . H50B H 0.6148 -0.3265 1.1489 0.068 Uiso 1 1 d R . . O60 O 0.6357(3) -0.1760(4) 0.8062(2) 0.0561(13) Uani 1 1 d . . . H60A H 0.6608 -0.1925 0.8460 0.084 Uiso 1 1 d R . . H60B H 0.5803 -0.1805 0.7996 0.084 Uiso 1 1 d 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 0.01372(17) 0.0141(2) 0.0138(2) 0.00054(14) 0.00349(13) 0.00059(14) Se1 0.0210(3) 0.0206(3) 0.0257(3) -0.0004(2) 0.0083(2) -0.0010(2) Se2 0.0183(3) 0.0228(3) 0.0168(3) 0.0005(2) 0.0054(2) 0.0014(2) P1 0.0141(6) 0.0169(7) 0.0170(7) -0.0004(5) 0.0049(5) -0.0002(5) P2 0.0151(6) 0.0160(7) 0.0149(6) 0.0013(5) 0.0043(5) 0.0006(5) N1 0.026(2) 0.055(4) 0.029(3) 0.004(2) 0.012(2) 0.009(2) N2 0.023(2) 0.031(3) 0.042(3) -0.001(2) 0.008(2) 0.000(2) C1 0.018(3) 0.031(4) 0.025(3) 0.001(2) 0.001(2) 0.001(2) C2 0.022(3) 0.032(4) 0.035(3) 0.008(3) -0.004(3) -0.008(2) C3 0.049(4) 0.042(4) 0.020(3) -0.010(3) 0.007(3) 0.031(3) C4 0.037(3) 0.022(3) 0.029(3) -0.001(2) 0.002(3) -0.008(3) C5 0.026(3) 0.035(4) 0.025(3) 0.002(2) 0.006(2) -0.003(2) C6 0.019(2) 0.015(3) 0.024(3) -0.002(2) 0.005(2) -0.005(2) C7 0.023(3) 0.021(3) 0.026(3) -0.001(2) 0.007(2) -0.005(2) C8 0.022(3) 0.027(3) 0.036(3) -0.001(2) 0.011(2) -0.003(2) C9 0.032(3) 0.026(3) 0.028(3) 0.008(2) -0.002(3) -0.001(3) C10 0.025(3) 0.023(3) 0.026(3) 0.005(2) 0.015(2) -0.002(2) C11 0.020(3) 0.022(3) 0.014(3) 0.000(2) 0.005(2) -0.001(2) C12 0.022(3) 0.019(3) 0.032(3) -0.002(2) 0.007(2) 0.000(2) C13 0.018(3) 0.026(4) 0.043(4) -0.006(3) 0.002(2) 0.000(2) C14 0.023(3) 0.030(4) 0.029(3) -0.007(2) 0.008(2) -0.006(2) C15 0.030(3) 0.014(3) 0.033(3) -0.003(2) 0.004(2) -0.007(2) C16 0.024(3) 0.022(3) 0.029(3) 0.002(2) 0.003(2) -0.001(2) C17 0.014(2) 0.015(3) 0.019(3) 0.004(2) 0.006(2) 0.002(2) C18 0.017(3) 0.041(4) 0.029(3) -0.017(3) 0.006(2) -0.012(2) C19 0.029(3) 0.035(4) 0.028(3) -0.012(3) 0.011(2) -0.007(2) C20 0.021(3) 0.028(3) 0.025(3) -0.001(2) 0.013(2) 0.002(2) C21 0.017(3) 0.025(3) 0.028(3) 0.000(2) 0.007(2) -0.008(2) C22 0.028(3) 0.021(3) 0.020(3) -0.008(2) 0.007(2) -0.003(2) C23 0.019(2) 0.012(3) 0.020(3) 0.003(2) 0.002(2) 0.002(2) C24 0.020(2) 0.022(3) 0.014(3) 0.004(2) 0.000(2) -0.005(2) C25 0.016(2) 0.017(3) 0.018(3) -0.005(2) 0.008(2) 0.000(2) C26 0.016(2) 0.021(3) 0.016(3) 0.000(2) 0.002(2) 0.003(2) C27 0.027(3) 0.020(3) 0.030(3) -0.005(2) 0.013(2) -0.003(2) C28 0.021(3) 0.022(3) 0.041(3) -0.012(3) 0.008(3) -0.001(2) C29 0.021(3) 0.014(3) 0.030(3) -0.001(2) -0.004(2) 0.004(2) C30 0.024(3) 0.014(3) 0.026(3) -0.001(2) 0.006(2) 0.001(2) C31 0.022(3) 0.023(3) 0.012(3) 0.005(2) 0.002(2) 0.008(2) C32 0.037(3) 0.019(3) 0.019(3) 0.004(2) 0.010(2) 0.008(2) C33 0.063(4) 0.023(4) 0.032(3) 0.007(3) 0.018(3) 0.017(3) C34 0.063(4) 0.042(4) 0.022(3) 0.011(3) 0.019(3) 0.037(3) C35 0.026(3) 0.059(5) 0.027(3) 0.017(3) 0.011(3) 0.015(3) C36 0.026(3) 0.037(4) 0.021(3) 0.009(2) 0.007(2) 0.005(2) O50 0.027(2) 0.039(3) 0.070(3) 0.003(2) 0.013(2) 0.0044(19) O60 0.032(2) 0.077(4) 0.058(3) -0.033(3) 0.011(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P2 2.2675(12) . ? Pd1 P1 2.2691(13) . ? Pd1 Se1 2.4750(6) . ? Pd1 Se2 2.4777(6) . ? Se1 C1 1.911(5) . ? Se2 C6 1.912(5) . ? P1 C17 1.817(5) . ? P1 C11 1.824(5) . ? P1 C23 1.837(5) . ? P2 C31 1.800(5) . ? P2 C24 1.820(5) . ? P2 C25 1.826(5) . ? N1 C4 1.284(7) . ? N1 C3 1.432(8) . ? N2 C9 1.346(7) . ? N2 C8 1.347(7) . ? C1 C5 1.389(8) . ? C1 C2 1.427(8) . ? C2 C3 1.301(8) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.421(8) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.383(7) . ? C6 C10 1.401(7) . ? C7 C8 1.378(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.377(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.381(7) . ? C11 C16 1.381(7) . ? C12 C13 1.399(7) . ? C12 H12 0.9500 . ? C13 C14 1.365(8) . ? C13 H13 0.9500 . ? C14 C15 1.378(7) . ? C14 H14 0.9500 . ? C15 C16 1.386(7) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.378(7) . ? C17 C22 1.391(7) . ? C18 C19 1.397(7) . ? C18 H18 0.9500 . ? C19 C20 1.360(7) . ? C19 H19 0.9500 . ? C20 C21 1.370(7) . ? C20 H20 0.9500 . ? C21 C22 1.375(7) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.519(6) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.387(7) . ? C25 C30 1.397(7) . ? C26 C27 1.378(7) . ? C26 H26 0.9500 . ? C27 C28 1.387(8) . ? C27 H27 0.9500 . ? C28 C29 1.376(8) . ? C28 H28 0.9500 . ? C29 C30 1.388(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.397(7) . ? C31 C36 1.398(7) . ? C32 C33 1.383(7) . ? C32 H32 0.9500 . ? C33 C34 1.373(9) . ? C33 H33 0.9500 . ? C34 C35 1.387(9) . ? C34 H34 0.9500 . ? C35 C36 1.390(8) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? O50 H50A 0.8500 . ? O50 H50B 0.8500 . ? O60 H60A 0.8500 . ? O60 H60B 0.8498 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pd1 P1 85.40(5) . . ? P2 Pd1 Se1 91.96(4) . . ? P1 Pd1 Se1 176.59(4) . . ? P2 Pd1 Se2 168.93(3) . . ? P1 Pd1 Se2 88.91(3) . . ? Se1 Pd1 Se2 93.34(2) . . ? C1 Se1 Pd1 107.66(17) . . ? C6 Se2 Pd1 105.41(15) . . ? C17 P1 C11 106.5(2) . . ? C17 P1 C23 102.8(2) . . ? C11 P1 C23 106.4(2) . . ? C17 P1 Pd1 117.64(16) . . ? C11 P1 Pd1 114.35(16) . . ? C23 P1 Pd1 108.01(16) . . ? C31 P2 C24 106.3(2) . . ? C31 P2 C25 105.6(2) . . ? C24 P2 C25 104.0(2) . . ? C31 P2 Pd1 124.83(16) . . ? C24 P2 Pd1 107.06(15) . . ? C25 P2 Pd1 107.28(16) . . ? C4 N1 C3 116.3(5) . . ? C9 N2 C8 115.7(5) . . ? C5 C1 C2 117.0(5) . . ? C5 C1 Se1 123.1(4) . . ? C2 C1 Se1 119.9(4) . . ? C3 C2 C1 120.1(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 N1 123.8(5) . . ? C2 C3 H3 118.1 . . ? N1 C3 H3 118.1 . . ? N1 C4 C5 123.9(5) . . ? N1 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C1 C5 C4 119.0(5) . . ? C1 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C7 C6 C10 117.5(5) . . ? C7 C6 Se2 123.5(4) . . ? C10 C6 Se2 119.0(4) . . ? C8 C7 C6 119.4(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? N2 C8 C7 124.2(5) . . ? N2 C8 H8 117.9 . . ? C7 C8 H8 117.9 . . ? N2 C9 C10 124.3(5) . . ? N2 C9 H9 117.9 . . ? C10 C9 H9 117.9 . . ? C9 C10 C6 118.9(5) . . ? C9 C10 H10 120.5 . . ? C6 C10 H10 120.5 . . ? C12 C11 C16 119.6(5) . . ? C12 C11 P1 118.6(4) . . ? C16 C11 P1 121.7(4) . . ? C11 C12 C13 119.6(5) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 120.6(5) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C13 C14 C15 119.7(5) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C14 C15 C16 120.3(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 120.1(5) . . ? C11 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C22 118.6(4) . . ? C18 C17 P1 122.3(4) . . ? C22 C17 P1 119.0(4) . . ? C17 C18 C19 120.0(5) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.8(5) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C22 119.5(5) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C17 121.0(5) . . ? C21 C22 H22 119.5 . . ? C17 C22 H22 119.5 . . ? C24 C23 P1 110.0(3) . . ? C24 C23 H23A 109.7 . . ? P1 C23 H23A 109.7 . . ? C24 C23 H23B 109.7 . . ? P1 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? C23 C24 P2 108.1(3) . . ? C23 C24 H24A 110.1 . . ? P2 C24 H24A 110.1 . . ? C23 C24 H24B 110.1 . . ? P2 C24 H24B 110.1 . . ? H24A C24 H24B 108.4 . . ? C26 C25 C30 119.4(4) . . ? C26 C25 P2 120.4(4) . . ? C30 C25 P2 120.0(4) . . ? C27 C26 C25 120.6(5) . . ? C27 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C26 C27 C28 120.0(5) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 119.8(5) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.7(5) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C29 C30 C25 119.4(5) . . ? C29 C30 H30 120.3 . . ? C25 C30 H30 120.3 . . ? C32 C31 C36 119.0(5) . . ? C32 C31 P2 119.9(4) . . ? C36 C31 P2 121.1(4) . . ? C33 C32 C31 120.4(5) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C34 C33 C32 120.4(6) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 120.2(5) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 120.1(5) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C35 C36 C31 119.9(6) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? H50A O50 H50B 109.5 . . ? H60A O60 H60B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pd1 Se1 C1 71.41(16) . . . . ? P1 Pd1 Se1 C1 110.5(6) . . . . ? Se2 Pd1 Se1 C1 -118.30(16) . . . . ? P2 Pd1 Se2 C6 169.1(2) . . . . ? P1 Pd1 Se2 C6 -131.90(15) . . . . ? Se1 Pd1 Se2 C6 50.66(15) . . . . ? P2 Pd1 P1 C17 119.85(17) . . . . ? Se1 Pd1 P1 C17 80.6(7) . . . . ? Se2 Pd1 P1 C17 -50.65(17) . . . . ? P2 Pd1 P1 C11 -114.05(17) . . . . ? Se1 Pd1 P1 C11 -153.3(6) . . . . ? Se2 Pd1 P1 C11 75.44(17) . . . . ? P2 Pd1 P1 C23 4.21(17) . . . . ? Se1 Pd1 P1 C23 -35.0(7) . . . . ? Se2 Pd1 P1 C23 -166.29(16) . . . . ? P1 Pd1 P2 C31 144.4(2) . . . . ? Se1 Pd1 P2 C31 -37.7(2) . . . . ? Se2 Pd1 P2 C31 -156.3(2) . . . . ? P1 Pd1 P2 C24 19.57(17) . . . . ? Se1 Pd1 P2 C24 -162.58(17) . . . . ? Se2 Pd1 P2 C24 78.8(3) . . . . ? P1 Pd1 P2 C25 -91.51(17) . . . . ? Se1 Pd1 P2 C25 86.34(16) . . . . ? Se2 Pd1 P2 C25 -32.3(3) . . . . ? Pd1 Se1 C1 C5 4.4(5) . . . . ? Pd1 Se1 C1 C2 -176.6(4) . . . . ? C5 C1 C2 C3 -0.6(8) . . . . ? Se1 C1 C2 C3 -179.6(4) . . . . ? C1 C2 C3 N1 1.5(8) . . . . ? C4 N1 C3 C2 -1.2(8) . . . . ? C3 N1 C4 C5 -0.1(8) . . . . ? C2 C1 C5 C4 -0.6(7) . . . . ? Se1 C1 C5 C4 178.4(4) . . . . ? N1 C4 C5 C1 1.0(8) . . . . ? Pd1 Se2 C6 C7 18.4(4) . . . . ? Pd1 Se2 C6 C10 -163.6(4) . . . . ? C10 C6 C7 C8 1.6(7) . . . . ? Se2 C6 C7 C8 179.6(4) . . . . ? C9 N2 C8 C7 -1.4(8) . . . . ? C6 C7 C8 N2 0.3(8) . . . . ? C8 N2 C9 C10 0.6(8) . . . . ? N2 C9 C10 C6 1.2(8) . . . . ? C7 C6 C10 C9 -2.3(7) . . . . ? Se2 C6 C10 C9 179.6(4) . . . . ? C17 P1 C11 C12 115.1(4) . . . . ? C23 P1 C11 C12 -135.7(4) . . . . ? Pd1 P1 C11 C12 -16.6(4) . . . . ? C17 P1 C11 C16 -63.7(5) . . . . ? C23 P1 C11 C16 45.4(5) . . . . ? Pd1 P1 C11 C16 164.6(4) . . . . ? C16 C11 C12 C13 1.1(8) . . . . ? P1 C11 C12 C13 -177.7(4) . . . . ? C11 C12 C13 C14 0.8(8) . . . . ? C12 C13 C14 C15 -2.1(8) . . . . ? C13 C14 C15 C16 1.5(8) . . . . ? C12 C11 C16 C15 -1.7(8) . . . . ? P1 C11 C16 C15 177.1(4) . . . . ? C14 C15 C16 C11 0.5(8) . . . . ? C11 P1 C17 C18 -5.2(5) . . . . ? C23 P1 C17 C18 -116.9(5) . . . . ? Pd1 P1 C17 C18 124.6(4) . . . . ? C11 P1 C17 C22 173.0(4) . . . . ? C23 P1 C17 C22 61.3(4) . . . . ? Pd1 P1 C17 C22 -57.1(4) . . . . ? C22 C17 C18 C19 -2.2(8) . . . . ? P1 C17 C18 C19 176.1(4) . . . . ? C17 C18 C19 C20 0.2(9) . . . . ? C18 C19 C20 C21 1.6(9) . . . . ? C19 C20 C21 C22 -1.3(8) . . . . ? C20 C21 C22 C17 -0.7(8) . . . . ? C18 C17 C22 C21 2.5(8) . . . . ? P1 C17 C22 C21 -175.9(4) . . . . ? C17 P1 C23 C24 -158.0(3) . . . . ? C11 P1 C23 C24 90.2(4) . . . . ? Pd1 P1 C23 C24 -33.0(4) . . . . ? P1 C23 C24 P2 49.7(4) . . . . ? C31 P2 C24 C23 179.6(3) . . . . ? C25 P2 C24 C23 68.3(3) . . . . ? Pd1 P2 C24 C23 -45.0(3) . . . . ? C31 P2 C25 C26 118.9(4) . . . . ? C24 P2 C25 C26 -129.4(4) . . . . ? Pd1 P2 C25 C26 -16.2(4) . . . . ? C31 P2 C25 C30 -65.2(4) . . . . ? C24 P2 C25 C30 46.5(4) . . . . ? Pd1 P2 C25 C30 159.7(4) . . . . ? C30 C25 C26 C27 -0.8(7) . . . . ? P2 C25 C26 C27 175.1(4) . . . . ? C25 C26 C27 C28 -0.1(8) . . . . ? C26 C27 C28 C29 0.5(8) . . . . ? C27 C28 C29 C30 0.1(8) . . . . ? C28 C29 C30 C25 -1.0(8) . . . . ? C26 C25 C30 C29 1.4(7) . . . . ? P2 C25 C30 C29 -174.6(4) . . . . ? C24 P2 C31 C32 -149.2(4) . . . . ? C25 P2 C31 C32 -39.1(4) . . . . ? Pd1 P2 C31 C32 85.6(4) . . . . ? C24 P2 C31 C36 32.5(4) . . . . ? C25 P2 C31 C36 142.5(4) . . . . ? Pd1 P2 C31 C36 -92.7(4) . . . . ? C36 C31 C32 C33 0.8(7) . . . . ? P2 C31 C32 C33 -177.6(4) . . . . ? C31 C32 C33 C34 -1.2(8) . . . . ? C32 C33 C34 C35 1.5(9) . . . . ? C33 C34 C35 C36 -1.4(8) . . . . ? C34 C35 C36 C31 1.0(8) . . . . ? C32 C31 C36 C35 -0.7(7) . . . . ? P2 C31 C36 C35 177.6(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 59.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.067 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 924436' ####################################################################### # # 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_twin4 #TrackingRef 'web_deposit_cif_file_5_Dr.SandipDey_1360841986.twin4.cif' # start Validation Reply Form _vrf_REFLT03_I ; PROBLEM: Reflection count > 15% excess reflns - sys abs data present? RESPONSE: The crystal used had two twin components. While reflections from one of the twin components (separated using TWINABS) was used for structure solution, reflections from both the components were used for final least squares refinement. This reflects in the reflection count and reports much higher number than actual completeness. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H35 N2 O0.50 P2 Pt Se2' _chemical_formula_weight 930.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -4.5932 6.9264 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5487(12) _cell_length_b 10.7006(13) _cell_length_c 14.9796(16) _cell_angle_alpha 91.771(9) _cell_angle_beta 94.027(9) _cell_angle_gamma 95.391(9) _cell_volume 1678.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 472 _cell_measurement_theta_min 5.33 _cell_measurement_theta_max 61.64 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.842 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 902 _exptl_absorpt_coefficient_mu 11.443 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5468 _exptl_absorpt_correction_T_max 0.7253 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER GADDS D8 Discover' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9931 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0429 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 62.60 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 9942 _reflns_number_gt 8854 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'FRAMBO (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; CELL-NOW (Sheldrick, 2003) and SAINT (BRUKER-NONIUS, 2003) ; _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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. Crystal used was twinned with two components. APEX2 was used to integrate the data including both the components. TWINABS was used for absorption correction as well as to separate the twin components and to create the batch hkl file including all the reflections from both components. 18796 data ( 3080 unique ) involve domain 1 only, mean I/sigma 7.7 18759 data ( 3076 unique ) involve domain 2 only, mean I/sigma 7.6 18691 data ( 3832 unique ) involve 2 domains, mean I/sigma 10.3 hkl file with only one component was used for structure solution and all the reflections were used for final least squares refinement. ; _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^)+(0.0802P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9942 _refine_ls_number_parameters 407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0423 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _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 Pt1 Pt 0.77798(2) 0.75194(2) 0.753848(14) 0.01091(9) Uani 1 1 d . . . Se1 Se 0.67582(6) 0.86990(6) 0.86993(4) 0.01598(16) Uani 1 1 d . . . Se2 Se 0.71524(7) 0.88483(6) 0.62890(4) 0.01844(17) Uani 1 1 d . . . P1 P 0.85862(15) 0.63490(14) 0.64595(9) 0.0130(3) Uani 1 1 d . . . P2 P 0.84722(15) 0.63235(15) 0.86607(10) 0.0147(3) Uani 1 1 d . . . N1 N 0.2319(6) 0.8334(6) 0.7872(4) 0.0348(15) Uani 1 1 d . . . N2 N 0.4369(7) 1.1840(6) 0.7097(4) 0.0440(18) Uani 1 1 d . . . C1 C 0.5017(6) 0.8563(6) 0.8321(4) 0.0223(15) Uani 1 1 d . . . C2 C 0.4188(6) 0.9349(6) 0.8704(4) 0.0217(15) Uani 1 1 d . . . H2 H 0.4520 0.9985 0.9137 0.026 Uiso 1 1 calc R . . C3 C 0.2900(7) 0.9204(7) 0.8455(5) 0.0299(17) Uani 1 1 d . . . H3 H 0.2384 0.9772 0.8720 0.036 Uiso 1 1 calc R . . C4 C 0.3114(6) 0.7598(6) 0.7496(5) 0.0310(17) Uani 1 1 d . . . H4 H 0.2743 0.6965 0.7072 0.037 Uiso 1 1 calc R . . C5 C 0.4415(6) 0.7679(6) 0.7669(4) 0.0235(15) Uani 1 1 d . . . H5 H 0.4909 0.7141 0.7352 0.028 Uiso 1 1 calc R . . C6 C 0.6017(6) 1.0051(6) 0.6641(4) 0.0220(15) Uani 1 1 d . . . C7 C 0.6451(7) 1.1072(6) 0.7218(4) 0.0235(15) Uani 1 1 d . . . H7 H 0.7307 1.1176 0.7472 0.028 Uiso 1 1 calc R . . C8 C 0.5593(8) 1.1931(7) 0.7410(5) 0.040(2) Uani 1 1 d . . . H8 H 0.5898 1.2636 0.7793 0.048 Uiso 1 1 calc R . . C9 C 0.3979(7) 1.0855(8) 0.6527(5) 0.040(2) Uani 1 1 d . . . H9 H 0.3121 1.0769 0.6278 0.048 Uiso 1 1 calc R . . C10 C 0.4777(6) 0.9970(6) 0.6291(4) 0.0267(16) Uani 1 1 d . . . H10 H 0.4463 0.9297 0.5881 0.032 Uiso 1 1 calc R . . C11 C 0.7421(6) 0.5101(5) 0.6002(4) 0.0170(14) Uani 1 1 d . . . C12 C 0.6182(6) 0.5089(6) 0.6217(5) 0.0260(16) Uani 1 1 d . . . H12 H 0.5948 0.5734 0.6606 0.031 Uiso 1 1 calc R . . C13 C 0.5252(7) 0.4144(7) 0.5874(6) 0.041(2) Uani 1 1 d . . . H13 H 0.4398 0.4142 0.6037 0.049 Uiso 1 1 calc R . . C14 C 0.5576(7) 0.3226(6) 0.5305(5) 0.0305(18) Uani 1 1 d . . . H14 H 0.4946 0.2588 0.5067 0.037 Uiso 1 1 calc R . . C15 C 0.6813(7) 0.3226(7) 0.5079(5) 0.0301(17) Uani 1 1 d . . . H15 H 0.7037 0.2590 0.4679 0.036 Uiso 1 1 calc R . . C16 C 0.7732(7) 0.4142(7) 0.5428(5) 0.0304(18) Uani 1 1 d . . . H16 H 0.8590 0.4122 0.5276 0.037 Uiso 1 1 calc R . . C17 C 0.9158(6) 0.7196(6) 0.5504(4) 0.0181(14) Uani 1 1 d . . . C18 C 0.8586(6) 0.7005(6) 0.4656(4) 0.0239(15) Uani 1 1 d . . . H18 H 0.7851 0.6422 0.4546 0.029 Uiso 1 1 calc R . . C19 C 0.9091(8) 0.7674(7) 0.3950(4) 0.0362(19) Uani 1 1 d . . . H19 H 0.8697 0.7544 0.3360 0.043 Uiso 1 1 calc R . . C20 C 1.0161(8) 0.8523(6) 0.4110(5) 0.036(2) Uani 1 1 d . . . H20 H 1.0504 0.8974 0.3632 0.043 Uiso 1 1 calc R . . C21 C 1.0723(8) 0.8710(6) 0.4963(5) 0.037(2) Uani 1 1 d . . . H21 H 1.1461 0.9291 0.5070 0.044 Uiso 1 1 calc R . . C22 C 1.0240(6) 0.8073(6) 0.5665(4) 0.0225(15) Uani 1 1 d . . . H22 H 1.0631 0.8223 0.6255 0.027 Uiso 1 1 calc R . . C23 C 0.9980(6) 0.5545(6) 0.6791(4) 0.0174(14) Uani 1 1 d . . . H23A H 1.0178 0.5008 0.6279 0.021 Uiso 1 1 calc R . . H23B H 1.0718 0.6180 0.6928 0.021 Uiso 1 1 calc R . . C24 C 0.9818(6) 0.4720(6) 0.7612(4) 0.0227(14) Uani 1 1 d . . . H24A H 0.8987 0.4201 0.7534 0.027 Uiso 1 1 calc R . . H24B H 1.0501 0.4146 0.7653 0.027 Uiso 1 1 calc R . . C25 C 0.9875(6) 0.5525(6) 0.8484(4) 0.0220(15) Uani 1 1 d . . . H25A H 1.0619 0.6163 0.8491 0.026 Uiso 1 1 calc R . . H25B H 1.0024 0.4978 0.8995 0.026 Uiso 1 1 calc R . . C26 C 0.9008(6) 0.7217(6) 0.9698(4) 0.0156(13) Uani 1 1 d . . . C27 C 1.0093(7) 0.8058(6) 0.9691(5) 0.0276(16) Uani 1 1 d . . . H27 H 1.0524 0.8159 0.9159 0.033 Uiso 1 1 calc R . . C28 C 1.0546(8) 0.8754(7) 1.0472(5) 0.040(2) Uani 1 1 d . . . H28 H 1.1313 0.9297 1.0481 0.048 Uiso 1 1 calc R . . C29 C 0.9875(8) 0.8651(6) 1.1232(5) 0.0348(19) Uani 1 1 d . . . H29 H 1.0170 0.9148 1.1756 0.042 Uiso 1 1 calc R . . C30 C 0.8801(7) 0.7846(7) 1.1238(4) 0.0326(18) Uani 1 1 d . . . H30 H 0.8351 0.7779 1.1764 0.039 Uiso 1 1 calc R . . C31 C 0.8358(7) 0.7120(6) 1.0474(4) 0.0233(15) Uani 1 1 d . . . H31 H 0.7608 0.6556 1.0481 0.028 Uiso 1 1 calc R . . C32 C 0.7300(6) 0.5101(6) 0.8981(4) 0.0151(14) Uani 1 1 d . . . C33 C 0.7651(8) 0.4096(7) 0.9476(5) 0.037(2) Uani 1 1 d . . . H33 H 0.8530 0.4024 0.9630 0.044 Uiso 1 1 calc R . . C34 C 0.6732(8) 0.3189(7) 0.9752(5) 0.044(2) Uani 1 1 d . . . H34 H 0.6986 0.2511 1.0096 0.053 Uiso 1 1 calc R . . C35 C 0.5492(8) 0.3278(6) 0.9529(4) 0.0330(19) Uani 1 1 d . . . H35 H 0.4873 0.2649 0.9706 0.040 Uiso 1 1 calc R . . C36 C 0.5101(8) 0.4262(6) 0.9052(5) 0.0334(19) Uani 1 1 d . . . H36 H 0.4218 0.4328 0.8913 0.040 Uiso 1 1 calc R . . C37 C 0.6020(7) 0.5171(6) 0.8770(5) 0.0251(16) Uani 1 1 d . . . H37 H 0.5753 0.5845 0.8429 0.030 Uiso 1 1 calc R . . O1 O 0.2976(9) 1.4003(10) 0.7325(7) 0.045(3) Uani 0.50 1 d P . . H1A H 0.3388 1.3365 0.7261 0.067 Uiso 0.50 1 d PR . . H1B H 0.3569 1.4568 0.7501 0.067 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.00908(15) 0.01243(14) 0.01128(13) 0.00161(10) 0.00095(10) 0.00078(9) Se1 0.0151(4) 0.0198(4) 0.0132(3) -0.0017(3) 0.0012(3) 0.0030(3) Se2 0.0232(4) 0.0182(4) 0.0156(3) 0.0039(3) 0.0030(3) 0.0087(3) P1 0.0141(9) 0.0130(8) 0.0124(7) 0.0003(6) 0.0028(6) 0.0030(7) P2 0.0169(9) 0.0157(8) 0.0117(7) 0.0040(6) 0.0006(6) 0.0027(7) N1 0.027(4) 0.044(4) 0.036(3) 0.013(3) 0.008(3) 0.007(3) N2 0.062(5) 0.042(4) 0.035(3) 0.007(3) 0.005(3) 0.040(4) C1 0.013(4) 0.028(4) 0.027(3) 0.009(3) 0.004(3) -0.003(3) C2 0.024(4) 0.021(4) 0.023(3) 0.008(3) 0.007(3) 0.009(3) C3 0.024(4) 0.032(4) 0.039(4) 0.010(3) 0.016(3) 0.016(3) C4 0.015(4) 0.038(4) 0.040(4) 0.004(4) 0.005(3) 0.000(3) C5 0.012(4) 0.025(4) 0.033(4) 0.000(3) 0.001(3) 0.002(3) C6 0.031(4) 0.023(4) 0.013(3) 0.003(3) 0.010(3) 0.002(3) C7 0.033(4) 0.019(4) 0.021(3) 0.005(3) 0.001(3) 0.010(3) C8 0.063(6) 0.038(5) 0.022(3) 0.000(3) -0.001(4) 0.026(4) C9 0.027(5) 0.061(6) 0.035(4) 0.000(4) 0.000(3) 0.028(4) C10 0.026(4) 0.030(4) 0.025(3) 0.004(3) 0.002(3) 0.002(3) C11 0.024(4) 0.007(3) 0.020(3) 0.003(3) 0.003(3) 0.003(3) C12 0.018(4) 0.015(4) 0.042(4) -0.007(3) -0.002(3) -0.006(3) C13 0.019(5) 0.026(4) 0.076(6) -0.017(4) 0.004(4) 0.000(4) C14 0.027(5) 0.023(4) 0.038(4) -0.007(3) -0.007(3) -0.004(3) C15 0.024(4) 0.034(4) 0.032(4) -0.006(3) 0.001(3) 0.003(3) C16 0.019(4) 0.034(4) 0.038(4) -0.007(3) 0.006(3) -0.002(3) C17 0.024(4) 0.012(3) 0.022(3) 0.006(3) 0.010(3) 0.015(3) C18 0.022(4) 0.029(4) 0.021(3) 0.002(3) 0.005(3) 0.003(3) C19 0.054(6) 0.037(5) 0.021(3) 0.001(3) 0.014(3) 0.015(4) C20 0.067(6) 0.016(4) 0.032(4) 0.016(3) 0.032(4) 0.011(4) C21 0.050(6) 0.014(4) 0.050(5) 0.004(3) 0.032(4) 0.000(4) C22 0.019(4) 0.023(4) 0.025(3) 0.004(3) 0.003(3) -0.003(3) C23 0.023(4) 0.017(3) 0.014(3) 0.005(2) 0.005(3) 0.009(3) C24 0.026(4) 0.021(3) 0.022(3) 0.003(3) 0.000(3) 0.006(3) C25 0.019(4) 0.027(4) 0.021(3) 0.003(3) 0.000(3) 0.004(3) C26 0.014(4) 0.018(3) 0.015(3) 0.002(2) -0.003(2) 0.002(3) C27 0.028(4) 0.022(4) 0.033(4) 0.002(3) 0.002(3) 0.005(3) C28 0.036(5) 0.024(4) 0.056(5) -0.017(4) -0.008(4) -0.011(4) C29 0.056(6) 0.019(4) 0.027(4) -0.006(3) -0.021(4) 0.011(4) C30 0.046(5) 0.033(4) 0.020(3) -0.001(3) 0.000(3) 0.012(4) C31 0.031(4) 0.019(4) 0.021(3) 0.006(3) 0.004(3) 0.004(3) C32 0.019(4) 0.012(3) 0.014(3) 0.006(2) 0.000(2) -0.002(3) C33 0.033(5) 0.029(4) 0.044(4) 0.022(4) -0.017(4) -0.008(4) C34 0.051(6) 0.022(4) 0.053(5) 0.020(4) -0.024(4) -0.011(4) C35 0.061(6) 0.016(4) 0.022(3) -0.001(3) 0.016(4) -0.009(4) C36 0.032(5) 0.016(4) 0.056(5) 0.004(3) 0.029(4) 0.000(3) C37 0.031(4) 0.009(3) 0.038(4) 0.010(3) 0.013(3) 0.002(3) O1 0.027(6) 0.042(6) 0.064(7) -0.014(6) -0.013(5) 0.017(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2656(15) . ? Pt1 P1 2.2744(15) . ? Pt1 Se2 2.4760(7) . ? Pt1 Se1 2.4822(7) . ? Se1 C1 1.875(6) . ? Se2 C6 1.925(6) . ? P1 C11 1.811(6) . ? P1 C23 1.819(6) . ? P1 C17 1.825(6) . ? P2 C25 1.808(6) . ? P2 C32 1.814(6) . ? P2 C26 1.825(6) . ? N1 C3 1.331(9) . ? N1 C4 1.344(9) . ? N2 C8 1.337(10) . ? N2 C9 1.350(10) . ? C1 C2 1.407(9) . ? C1 C5 1.412(9) . ? C2 C3 1.377(9) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.373(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C10 1.369(9) . ? C6 C7 1.394(9) . ? C7 C8 1.387(9) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.379(9) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.366(9) . ? C11 C16 1.396(9) . ? C12 C13 1.401(10) . ? C12 H12 0.9500 . ? C13 C14 1.363(10) . ? C13 H13 0.9500 . ? C14 C15 1.371(10) . ? C14 H14 0.9500 . ? C15 C16 1.376(10) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C18 1.368(9) . ? C17 C22 1.410(9) . ? C18 C19 1.404(9) . ? C18 H18 0.9500 . ? C19 C20 1.383(11) . ? C19 H19 0.9500 . ? C20 C21 1.371(11) . ? C20 H20 0.9500 . ? C21 C22 1.374(9) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.546(8) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.537(8) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.389(9) . ? C26 C31 1.391(8) . ? C27 C28 1.397(9) . ? C27 H27 0.9500 . ? C28 C29 1.384(11) . ? C28 H28 0.9500 . ? C29 C30 1.358(11) . ? C29 H29 0.9500 . ? C30 C31 1.390(9) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ? C32 C37 1.374(9) . ? C32 C33 1.389(9) . ? C33 C34 1.400(10) . ? C33 H33 0.9500 . ? C34 C35 1.341(11) . ? C34 H34 0.9500 . ? C35 C36 1.370(10) . ? C35 H35 0.9500 . ? C36 C37 1.403(9) . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? O1 H1A 0.8499 . ? O1 H1B 0.8502 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 Pt1 P1 93.58(5) . . ? P2 Pt1 Se2 176.69(4) . . ? P1 Pt1 Se2 84.65(4) . . ? P2 Pt1 Se1 86.47(4) . . ? P1 Pt1 Se1 175.98(4) . . ? Se2 Pt1 Se1 95.49(2) . . ? C1 Se1 Pt1 105.3(2) . . ? C6 Se2 Pt1 112.10(17) . . ? C11 P1 C23 104.0(3) . . ? C11 P1 C17 106.2(3) . . ? C23 P1 C17 100.5(3) . . ? C11 P1 Pt1 111.4(2) . . ? C23 P1 Pt1 117.03(19) . . ? C17 P1 Pt1 116.2(2) . . ? C25 P2 C32 104.6(3) . . ? C25 P2 C26 100.1(3) . . ? C32 P2 C26 105.0(3) . . ? C25 P2 Pt1 116.7(2) . . ? C32 P2 Pt1 114.8(2) . . ? C26 P2 Pt1 113.8(2) . . ? C3 N1 C4 114.0(6) . . ? C8 N2 C9 116.1(6) . . ? C2 C1 C5 114.4(6) . . ? C2 C1 Se1 120.7(5) . . ? C5 C1 Se1 124.9(5) . . ? C3 C2 C1 120.5(6) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? N1 C3 C2 125.4(6) . . ? N1 C3 H3 117.3 . . ? C2 C3 H3 117.3 . . ? N1 C4 C5 125.8(7) . . ? N1 C4 H4 117.1 . . ? C5 C4 H4 117.1 . . ? C4 C5 C1 119.8(6) . . ? C4 C5 H5 120.1 . . ? C1 C5 H5 120.1 . . ? C10 C6 C7 117.9(6) . . ? C10 C6 Se2 120.9(5) . . ? C7 C6 Se2 121.1(5) . . ? C8 C7 C6 117.9(7) . . ? C8 C7 H7 121.1 . . ? C6 C7 H7 121.1 . . ? N2 C8 C7 124.8(7) . . ? N2 C8 H8 117.6 . . ? C7 C8 H8 117.6 . . ? N2 C9 C10 122.7(7) . . ? N2 C9 H9 118.7 . . ? C10 C9 H9 118.7 . . ? C6 C10 C9 120.6(7) . . ? C6 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C16 118.0(6) . . ? C12 C11 P1 119.4(5) . . ? C16 C11 P1 122.6(5) . . ? C11 C12 C13 121.1(7) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C14 C13 C12 119.8(7) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 119.9(7) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 120.3(7) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 120.8(7) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C18 C17 C22 119.9(6) . . ? C18 C17 P1 122.7(5) . . ? C22 C17 P1 117.4(5) . . ? C17 C18 C19 119.7(7) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.2(7) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 119.7(6) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 121.2(7) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C17 119.4(6) . . ? C21 C22 H22 120.3 . . ? C17 C22 H22 120.3 . . ? C24 C23 P1 114.2(4) . . ? C24 C23 H23A 108.7 . . ? P1 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? P1 C23 H23B 108.7 . . ? H23A C23 H23B 107.6 . . ? C25 C24 C23 111.4(5) . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24B 109.3 . . ? C23 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C24 C25 P2 115.6(5) . . ? C24 C25 H25A 108.4 . . ? P2 C25 H25A 108.4 . . ? C24 C25 H25B 108.4 . . ? P2 C25 H25B 108.4 . . ? H25A C25 H25B 107.4 . . ? C27 C26 C31 119.3(6) . . ? C27 C26 P2 117.6(5) . . ? C31 C26 P2 123.1(5) . . ? C26 C27 C28 119.6(7) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C29 C28 C27 119.9(7) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C30 C29 C28 120.6(6) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C31 120.1(7) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C30 C31 C26 120.3(7) . . ? C30 C31 H31 119.8 . . ? C26 C31 H31 119.8 . . ? C37 C32 C33 117.7(6) . . ? C37 C32 P2 120.6(5) . . ? C33 C32 P2 121.6(5) . . ? C32 C33 C34 121.0(7) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C35 C34 C33 119.7(7) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 121.1(7) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C37 119.3(7) . . ? C35 C36 H36 120.4 . . ? C37 C36 H36 120.4 . . ? C32 C37 C36 121.1(6) . . ? C32 C37 H37 119.5 . . ? C36 C37 H37 119.5 . . ? H1A O1 H1B 101.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P2 Pt1 Se1 C1 -121.8(2) . . . . ? P1 Pt1 Se1 C1 -31.0(6) . . . . ? Se2 Pt1 Se1 C1 60.8(2) . . . . ? P2 Pt1 Se2 C6 -133.4(8) . . . . ? P1 Pt1 Se2 C6 168.9(2) . . . . ? Se1 Pt1 Se2 C6 -7.0(2) . . . . ? P2 Pt1 P1 C11 91.2(2) . . . . ? Se2 Pt1 P1 C11 -91.6(2) . . . . ? Se1 Pt1 P1 C11 0.6(7) . . . . ? P2 Pt1 P1 C23 -28.3(2) . . . . ? Se2 Pt1 P1 C23 148.9(2) . . . . ? Se1 Pt1 P1 C23 -118.9(6) . . . . ? P2 Pt1 P1 C17 -146.9(2) . . . . ? Se2 Pt1 P1 C17 30.3(2) . . . . ? Se1 Pt1 P1 C17 122.5(6) . . . . ? P1 Pt1 P2 C25 27.8(3) . . . . ? Se2 Pt1 P2 C25 -29.7(9) . . . . ? Se1 Pt1 P2 C25 -156.3(3) . . . . ? P1 Pt1 P2 C32 -95.2(2) . . . . ? Se2 Pt1 P2 C32 -152.6(7) . . . . ? Se1 Pt1 P2 C32 80.8(2) . . . . ? P1 Pt1 P2 C26 143.7(2) . . . . ? Se2 Pt1 P2 C26 86.3(8) . . . . ? Se1 Pt1 P2 C26 -40.3(2) . . . . ? Pt1 Se1 C1 C2 -165.4(4) . . . . ? Pt1 Se1 C1 C5 16.4(6) . . . . ? C5 C1 C2 C3 1.6(9) . . . . ? Se1 C1 C2 C3 -176.8(5) . . . . ? C4 N1 C3 C2 -2.6(10) . . . . ? C1 C2 C3 N1 1.6(10) . . . . ? C3 N1 C4 C5 0.4(10) . . . . ? N1 C4 C5 C1 2.7(11) . . . . ? C2 C1 C5 C4 -3.5(9) . . . . ? Se1 C1 C5 C4 174.8(5) . . . . ? Pt1 Se2 C6 C10 -113.2(5) . . . . ? Pt1 Se2 C6 C7 70.7(5) . . . . ? C10 C6 C7 C8 0.9(9) . . . . ? Se2 C6 C7 C8 177.1(5) . . . . ? C9 N2 C8 C7 -2.6(11) . . . . ? C6 C7 C8 N2 1.4(10) . . . . ? C8 N2 C9 C10 1.5(11) . . . . ? C7 C6 C10 C9 -1.9(9) . . . . ? Se2 C6 C10 C9 -178.1(5) . . . . ? N2 C9 C10 C6 0.7(11) . . . . ? C23 P1 C11 C12 137.0(5) . . . . ? C17 P1 C11 C12 -117.4(5) . . . . ? Pt1 P1 C11 C12 10.1(6) . . . . ? C23 P1 C11 C16 -43.4(6) . . . . ? C17 P1 C11 C16 62.2(6) . . . . ? Pt1 P1 C11 C16 -170.3(5) . . . . ? C16 C11 C12 C13 0.1(11) . . . . ? P1 C11 C12 C13 179.7(6) . . . . ? C11 C12 C13 C14 -0.9(13) . . . . ? C12 C13 C14 C15 0.6(12) . . . . ? C13 C14 C15 C16 0.5(12) . . . . ? C14 C15 C16 C11 -1.3(11) . . . . ? C12 C11 C16 C15 1.0(10) . . . . ? P1 C11 C16 C15 -178.6(5) . . . . ? C11 P1 C17 C18 10.8(6) . . . . ? C23 P1 C17 C18 118.9(6) . . . . ? Pt1 P1 C17 C18 -113.7(5) . . . . ? C11 P1 C17 C22 -168.9(5) . . . . ? C23 P1 C17 C22 -60.8(5) . . . . ? Pt1 P1 C17 C22 66.6(5) . . . . ? C22 C17 C18 C19 0.8(10) . . . . ? P1 C17 C18 C19 -178.9(5) . . . . ? C17 C18 C19 C20 0.0(11) . . . . ? C18 C19 C20 C21 -0.2(11) . . . . ? C19 C20 C21 C22 -0.3(11) . . . . ? C20 C21 C22 C17 1.0(11) . . . . ? C18 C17 C22 C21 -1.3(10) . . . . ? P1 C17 C22 C21 178.4(5) . . . . ? C11 P1 C23 C24 -70.4(5) . . . . ? C17 P1 C23 C24 179.7(4) . . . . ? Pt1 P1 C23 C24 52.9(5) . . . . ? P1 C23 C24 C25 -74.1(6) . . . . ? C23 C24 C25 P2 74.7(6) . . . . ? C32 P2 C25 C24 75.2(5) . . . . ? C26 P2 C25 C24 -176.2(5) . . . . ? Pt1 P2 C25 C24 -52.9(5) . . . . ? C25 P2 C26 C27 59.0(6) . . . . ? C32 P2 C26 C27 167.3(5) . . . . ? Pt1 P2 C26 C27 -66.3(5) . . . . ? C25 P2 C26 C31 -123.2(5) . . . . ? C32 P2 C26 C31 -14.9(6) . . . . ? Pt1 P2 C26 C31 111.5(5) . . . . ? C31 C26 C27 C28 2.7(10) . . . . ? P2 C26 C27 C28 -179.4(5) . . . . ? C26 C27 C28 C29 -3.4(11) . . . . ? C27 C28 C29 C30 2.3(12) . . . . ? C28 C29 C30 C31 -0.4(11) . . . . ? C29 C30 C31 C26 -0.3(10) . . . . ? C27 C26 C31 C30 -0.9(10) . . . . ? P2 C26 C31 C30 -178.7(5) . . . . ? C25 P2 C32 C37 -149.2(5) . . . . ? C26 P2 C32 C37 105.8(5) . . . . ? Pt1 P2 C32 C37 -20.0(6) . . . . ? C25 P2 C32 C33 33.6(6) . . . . ? C26 P2 C32 C33 -71.4(6) . . . . ? Pt1 P2 C32 C33 162.8(5) . . . . ? C37 C32 C33 C34 -0.1(11) . . . . ? P2 C32 C33 C34 177.2(6) . . . . ? C32 C33 C34 C35 0.7(12) . . . . ? C33 C34 C35 C36 -1.5(12) . . . . ? C34 C35 C36 C37 1.8(11) . . . . ? C33 C32 C37 C36 0.4(10) . . . . ? P2 C32 C37 C36 -176.9(5) . . . . ? C35 C36 C37 C32 -1.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 62.60 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.065 _refine_diff_density_min -1.036 _refine_diff_density_rms 0.165 _database_code_depnum_ccdc_archive 'CCDC 924437' ####################################################################### # # 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_7a # start Validation Reply Form _vrf_PLAT026_I ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 24 % RESPONSE: higly absorbing species present ; _vrf_PLAT220_I ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.3 Ratio RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; _vrf_PLAT222_I ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 8.8 Ratio RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; _vrf_PLAT241_I ; PROBLEM: Check High Ueq as Compared to Neighbors for C17 RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; _vrf_PLAT242_I ; PROBLEM: Check Low Ueq as Compared to Neighbors for P2 RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; _vrf_PLAT342_I ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0240 Ang. RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; # end Validation Reply Form # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.545 0.147 0.882 19 6 ' ' 2 0.045 0.353 0.382 19 6 ' ' 3 0.955 0.647 0.618 19 6 ' ' 4 0.455 0.853 0.118 19 6 ' ' _platon_squeeze_details ; A total of 24 electrons are present in the different voids These may correspond to water molecules, but can not be established correctly ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H57 Cl3 N3 P3 Pd3 Se3' _chemical_formula_weight 1251.16 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 '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' Cl Cl 0.1484 0.1585 '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' H H 0.0000 0.0000 '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 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.2500(12) _cell_length_b 13.984(6) _cell_length_c 24.400(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.330(13) _cell_angle_gamma 90.00 _cell_volume 4689(2) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.2 _cell_measurement_theta_max 13.4 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.772 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 3.766 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.4528 _exptl_absorpt_correction_T_max 0.7045 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.05 _diffrn_reflns_number 14523 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_unetI/netI 0.3827 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 10760 _reflns_number_gt 2564 _reflns_threshold_expression >2sigma(I) _computing_data_collection WInAFC _computing_cell_refinement WinAFC _computing_data_reduction 'Crystal Structure' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0607P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10760 _refine_ls_number_parameters 410 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.3474 _refine_ls_R_factor_gt 0.0745 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 0.750 _refine_ls_restrained_S_all 0.756 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7927(13) 0.4288(10) 0.3921(6) 0.060(4) Uani 1 1 d . . . C2 C 0.8693(11) 0.4560(13) 0.4371(7) 0.086(5) Uani 1 1 d . . . H2 H 0.9250 0.4186 0.4484 0.104 Uiso 1 1 calc R . . C3 C 0.8608(10) 0.5394(12) 0.4643(6) 0.066(4) Uani 1 1 d . . . H3 H 0.9126 0.5581 0.4943 0.079 Uiso 1 1 calc R . . C4 C 0.7085(10) 0.5660(11) 0.4084(7) 0.058(4) Uani 1 1 d . . . H4 H 0.6523 0.6032 0.3992 0.070 Uiso 1 1 calc R . . C5 C 0.7088(11) 0.4853(13) 0.3778(6) 0.067(4) Uani 1 1 d . . . H5 H 0.6553 0.4681 0.3484 0.080 Uiso 1 1 calc R . . C6 C 0.6051(13) 0.3204(12) 0.2156(6) 0.110(6) Uani 1 1 d . . . H6A H 0.6594 0.3647 0.2236 0.132 Uiso 1 1 calc R . . H6B H 0.5872 0.3075 0.1751 0.132 Uiso 1 1 calc R . . C7 C 0.5217(12) 0.3668(15) 0.2305(8) 0.151(8) Uani 1 1 d . . . H7A H 0.5051 0.4247 0.2091 0.226 Uiso 1 1 calc R . . H7B H 0.5391 0.3813 0.2704 0.226 Uiso 1 1 calc R . . H7C H 0.4669 0.3242 0.2218 0.226 Uiso 1 1 calc R . . C8 C 0.7542(11) 0.1757(12) 0.2319(6) 0.093(5) Uani 1 1 d . . . H8A H 0.7377 0.1699 0.1908 0.111 Uiso 1 1 calc R . . H8B H 0.8022 0.2263 0.2428 0.111 Uiso 1 1 calc R . . C9 C 0.7987(12) 0.0818(15) 0.2585(7) 0.137(8) Uani 1 1 d . . . H9A H 0.8561 0.0681 0.2464 0.205 Uiso 1 1 calc R . . H9B H 0.7524 0.0311 0.2466 0.205 Uiso 1 1 calc R . . H9C H 0.8154 0.0873 0.2992 0.205 Uiso 1 1 calc R . . C10 C 0.5566(10) 0.1214(13) 0.2227(7) 0.115(7) Uani 1 1 d . . . H10A H 0.5775 0.0613 0.2419 0.138 Uiso 1 1 calc R . . H10B H 0.4961 0.1390 0.2313 0.138 Uiso 1 1 calc R . . C11 C 0.5340(11) 0.1030(14) 0.1591(7) 0.134(7) Uani 1 1 d . . . H11A H 0.4856 0.0538 0.1488 0.202 Uiso 1 1 calc R . . H11B H 0.5922 0.0829 0.1496 0.202 Uiso 1 1 calc R . . H11C H 0.5101 0.1607 0.1389 0.202 Uiso 1 1 calc R . . C12 C 0.6427(10) 0.6027(9) 0.5467(5) 0.055(4) Uani 1 1 d . . . C13 C 0.7322(9) 0.5563(9) 0.5729(5) 0.059(4) Uani 1 1 d . . . H13 H 0.7906 0.5798 0.5681 0.071 Uiso 1 1 calc R . . C14 C 0.7312(9) 0.4767(10) 0.6052(5) 0.057(4) Uani 1 1 d . . . H14 H 0.7907 0.4485 0.6226 0.068 Uiso 1 1 calc R . . C15 C 0.5686(10) 0.4811(10) 0.5906(6) 0.060(4) Uani 1 1 d . . . H15 H 0.5127 0.4569 0.5984 0.072 Uiso 1 1 calc R . . C16 C 0.5586(9) 0.5583(11) 0.5567(6) 0.068(4) Uani 1 1 d . . . H16 H 0.4971 0.5828 0.5398 0.082 Uiso 1 1 calc R . . C23 C 0.7449(9) 0.2445(9) 0.5583(5) 0.058(4) Uani 1 1 d . . . C24 C 0.8167(9) 0.2322(9) 0.5317(6) 0.064(4) Uani 1 1 d . . . H24 H 0.8806 0.2253 0.5534 0.077 Uiso 1 1 calc R . . C25 C 0.7970(9) 0.2297(9) 0.4732(7) 0.068(5) Uani 1 1 d . . . H25 H 0.8485 0.2220 0.4568 0.081 Uiso 1 1 calc R . . C26 C 0.6338(10) 0.2478(9) 0.4638(6) 0.062(4) Uani 1 1 d . . . H26 H 0.5703 0.2523 0.4410 0.074 Uiso 1 1 calc R . . C27 C 0.6497(9) 0.2516(9) 0.5226(6) 0.063(4) Uani 1 1 d . . . H27 H 0.5974 0.2587 0.5383 0.075 Uiso 1 1 calc R . . C29 C 0.4474(13) 0.1515(18) 0.6750(8) 0.191(10) Uani 1 1 d DU . . H29A H 0.3834 0.1411 0.6797 0.287 Uiso 1 1 calc R . . H29B H 0.4671 0.0965 0.6572 0.287 Uiso 1 1 calc R . . H29C H 0.4468 0.2067 0.6515 0.287 Uiso 1 1 calc R . . C31 C 0.6780(19) -0.0093(15) 0.7410(11) 0.256(15) Uani 1 1 d DU . . H31A H 0.7050 -0.0631 0.7260 0.384 Uiso 1 1 calc R . . H31B H 0.6130 -0.0242 0.7426 0.384 Uiso 1 1 calc R . . H31C H 0.7174 0.0049 0.7785 0.384 Uiso 1 1 calc R . . Se1 Se 0.80941(11) 0.32148(12) 0.34572(6) 0.0764(5) Uani 1 1 d . . . Se2 Se 0.63149(10) 0.71549(11) 0.50439(7) 0.0781(5) Uani 1 1 d . . . Se3 Se 0.77722(11) 0.23868(12) 0.63727(6) 0.0793(5) Uani 1 1 d . . . Pd1 Pd 0.67200(7) 0.22341(8) 0.34818(4) 0.0600(4) Uani 1 1 d . . . Pd2 Pd 0.78633(7) 0.73735(8) 0.48490(4) 0.0612(4) Uani 1 1 d . . . Pd3 Pd 0.64915(7) 0.31566(8) 0.66711(4) 0.0614(4) Uani 1 1 d . . . Cl1 Cl 0.5410(3) 0.1258(3) 0.35185(17) 0.0957(14) Uani 1 1 d . . . Cl2 Cl 0.9376(3) 0.7576(3) 0.4674(2) 0.1100(16) Uani 1 1 d . . . Cl3 Cl 0.5399(3) 0.3975(3) 0.70680(16) 0.0958(14) Uani 1 1 d . . . N1 N 0.7815(9) 0.5963(8) 0.4502(5) 0.058(3) Uani 1 1 d . . . N2 N 0.6524(8) 0.4366(7) 0.6139(4) 0.051(3) Uani 1 1 d . . . N3 N 0.7063(8) 0.2379(6) 0.4389(4) 0.054(3) Uani 1 1 d . . . C18 C 0.8050(14) 0.9790(14) 0.4199(8) 0.155(8) Uani 1 1 d . . . H18A H 0.8399 1.0264 0.4046 0.232 Uiso 1 1 calc R . . H18B H 0.7385 0.9988 0.4138 0.232 Uiso 1 1 calc R . . H18C H 0.8072 0.9190 0.4011 0.232 Uiso 1 1 calc R . . C17 C 0.8501(14) 0.9681(14) 0.4813(10) 0.161(8) Uani 1 1 d . . . H17A H 0.8511 1.0306 0.4988 0.193 Uiso 1 1 calc R . . H17B H 0.9173 0.9489 0.4863 0.193 Uiso 1 1 calc R . . C22 C 0.926(3) 0.953(2) 0.6230(12) 0.40(2) Uani 1 1 d D . . H22A H 0.9739 0.9337 0.6570 0.596 Uiso 1 1 calc R . . H22B H 0.8701 0.9777 0.6325 0.596 Uiso 1 1 calc R . . H22C H 0.9536 1.0010 0.6038 0.596 Uiso 1 1 calc R . . C21 C 0.8997(17) 0.8729(18) 0.5871(9) 0.249(15) Uani 1 1 d D . . H21A H 0.8823 0.8217 0.6094 0.299 Uiso 1 1 calc R . . H21B H 0.9569 0.8520 0.5760 0.299 Uiso 1 1 calc R . . C28 C 0.5198(12) 0.1677(16) 0.7337(9) 0.170(7) Uani 1 1 d DU . . H28A H 0.5222 0.1118 0.7576 0.204 Uiso 1 1 calc R . . H28B H 0.5002 0.2223 0.7525 0.204 Uiso 1 1 calc R . . C30 C 0.6759(14) 0.0750(13) 0.7037(8) 0.160(4) Uani 1 1 d DU . . H30A H 0.6340 0.0583 0.6667 0.192 Uiso 1 1 calc R . . H30B H 0.7410 0.0820 0.6990 0.192 Uiso 1 1 calc R . . C32 C 0.7026(15) 0.2104(16) 0.7920(8) 0.206(6) Uani 1 1 d DU . . H32A H 0.6779 0.2692 0.8040 0.248 Uiso 1 1 calc R . . H32B H 0.6871 0.1591 0.8149 0.248 Uiso 1 1 calc R . . C33 C 0.8115(15) 0.2182(17) 0.8051(8) 0.227(10) Uani 1 1 d DU . . H33A H 0.8377 0.2309 0.8449 0.341 Uiso 1 1 calc R . . H33B H 0.8285 0.2694 0.7834 0.341 Uiso 1 1 calc R . . H33C H 0.8378 0.1593 0.7955 0.341 Uiso 1 1 calc R . . C19 C 0.6986(16) 0.9370(17) 0.5522(9) 0.210(10) Uani 1 1 d DU . . H19A H 0.6688 0.8878 0.5701 0.253 Uiso 1 1 calc R . . H19B H 0.7237 0.9877 0.5793 0.253 Uiso 1 1 calc R . . C20 C 0.6321(16) 0.973(2) 0.5002(11) 0.272(10) Uani 1 1 d DU . . H20A H 0.5773 1.0031 0.5092 0.408 Uiso 1 1 calc R . . H20B H 0.6099 0.9212 0.4744 0.408 Uiso 1 1 calc R . . H20C H 0.6653 1.0192 0.4829 0.408 Uiso 1 1 calc R . . P1 P 0.6446(3) 0.2091(3) 0.25360(15) 0.0699(12) Uani 1 1 d . . . P2 P 0.7961(3) 0.8863(3) 0.5196(2) 0.0929(15) Uani 1 1 d DU . . P3 P 0.6392(3) 0.1892(3) 0.72066(18) 0.0838(13) Uani 1 1 d U . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.076(11) 0.059(11) 0.051(10) 0.012(8) 0.029(9) -0.006(9) C2 0.065(12) 0.116(16) 0.073(13) -0.020(11) 0.009(10) 0.013(11) C3 0.049(10) 0.074(12) 0.073(12) -0.014(10) 0.011(9) 0.000(9) C4 0.042(10) 0.048(11) 0.082(12) 0.015(9) 0.013(9) -0.004(8) C5 0.060(11) 0.068(13) 0.069(12) 0.004(10) 0.010(9) -0.014(10) C6 0.130(16) 0.111(16) 0.070(12) -0.005(11) -0.010(11) 0.006(13) C7 0.098(16) 0.18(2) 0.139(18) -0.020(16) -0.028(13) 0.038(15) C8 0.097(12) 0.111(15) 0.085(12) -0.008(11) 0.050(10) 0.007(11) C9 0.121(16) 0.19(2) 0.095(15) -0.027(15) 0.012(12) 0.057(15) C10 0.086(12) 0.177(19) 0.075(13) -0.038(13) 0.009(10) -0.057(12) C11 0.114(15) 0.18(2) 0.097(16) -0.038(14) 0.006(12) -0.012(13) C12 0.051(9) 0.066(11) 0.038(8) -0.001(7) -0.008(7) 0.008(8) C13 0.051(9) 0.055(10) 0.070(10) 0.028(8) 0.011(8) -0.013(8) C14 0.046(9) 0.064(11) 0.053(10) 0.004(8) 0.002(8) -0.014(8) C15 0.064(11) 0.060(11) 0.061(10) 0.033(9) 0.024(8) 0.010(9) C16 0.032(8) 0.082(13) 0.095(13) 0.002(10) 0.024(8) 0.001(8) C23 0.048(8) 0.079(11) 0.055(9) 0.011(8) 0.029(8) 0.008(8) C24 0.057(9) 0.091(12) 0.045(9) -0.006(9) 0.012(8) -0.002(8) C25 0.016(7) 0.086(12) 0.095(13) 0.014(10) 0.002(8) 0.002(8) C26 0.068(10) 0.063(11) 0.055(10) -0.005(8) 0.017(8) -0.007(8) C27 0.052(9) 0.089(12) 0.056(10) -0.006(9) 0.031(8) 0.008(8) C29 0.139(12) 0.23(3) 0.182 0.05(2) 0.010(12) -0.058(19) C31 0.30(3) 0.117(13) 0.31(4) 0.099(19) 0.011 0.013(19) Se1 0.0792(11) 0.0856(13) 0.0747(11) -0.0214(10) 0.0387(9) -0.0178(9) Se2 0.0630(10) 0.0656(11) 0.1162(14) 0.0245(10) 0.0420(9) 0.0112(8) Se3 0.0714(10) 0.1120(15) 0.0577(10) 0.0223(10) 0.0227(8) 0.0273(10) Pd1 0.0639(7) 0.0615(8) 0.0580(7) -0.0103(6) 0.0220(6) -0.0020(6) Pd2 0.0547(7) 0.0576(8) 0.0733(8) -0.0006(6) 0.0202(6) -0.0060(6) Pd3 0.0650(7) 0.0742(9) 0.0493(7) 0.0085(6) 0.0227(6) 0.0024(6) Cl1 0.100(3) 0.101(4) 0.090(3) -0.015(3) 0.032(2) -0.039(3) Cl2 0.072(3) 0.109(4) 0.168(4) -0.032(3) 0.065(3) -0.023(3) Cl3 0.119(3) 0.102(3) 0.086(3) 0.008(3) 0.061(3) 0.024(3) N1 0.053(8) 0.055(9) 0.067(9) -0.003(7) 0.018(7) -0.005(7) N2 0.057(8) 0.055(8) 0.040(7) 0.026(6) 0.014(6) -0.001(7) N3 0.078(8) 0.038(7) 0.065(8) -0.010(6) 0.051(7) -0.001(6) C18 0.19(2) 0.130(19) 0.14(2) 0.033(16) 0.037(16) 0.047(16) C17 0.147 0.095 0.22(2) 0.048(18) 0.013 -0.024(13) C22 0.60(7) 0.340 0.267 -0.01(4) 0.15(4) -0.05(5) C21 0.247 0.20(3) 0.27(3) -0.16(3) 0.008 -0.05(2) C28 0.104(9) 0.151(19) 0.241 0.039(18) 0.025 -0.016(15) C30 0.169 0.124(12) 0.178 0.057(11) 0.030 0.058(14) C32 0.265(16) 0.193 0.124(11) 0.046(12) -0.014 -0.162 C33 0.230(16) 0.29(3) 0.104(17) 0.080(18) -0.062(13) -0.154 C19 0.19(2) 0.18(2) 0.255 -0.05(2) 0.043(17) 0.082(18) C20 0.163(16) 0.27(4) 0.354 0.07(3) 0.03(2) 0.078 P1 0.075(3) 0.076(3) 0.050(2) -0.006(2) 0.002 0.001(2) P2 0.100(3) 0.066(3) 0.101(4) -0.005(3) 0.005 -0.017(3) P3 0.088(3) 0.083(3) 0.070(3) 0.016(3) 0.003 -0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.381(17) . ? C1 C5 1.398(17) . ? C1 Se1 1.932(14) . ? C2 C3 1.363(17) . ? C2 H2 0.9300 . ? C3 N1 1.351(15) . ? C3 H3 0.9300 . ? C4 N1 1.320(15) . ? C4 C5 1.353(17) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.480(19) . ? C6 P1 1.823(16) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.526(19) . ? C8 P1 1.837(13) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.521(17) . ? C10 P1 1.773(14) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.423(15) . ? C12 C16 1.427(16) . ? C12 Se2 1.868(13) . ? C13 C14 1.368(15) . ? C13 H13 0.9300 . ? C14 N2 1.321(13) . ? C14 H14 0.9300 . ? C15 N2 1.334(14) . ? C15 C16 1.345(16) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C23 C24 1.361(14) . ? C23 C27 1.409(15) . ? C23 Se3 1.860(12) . ? C24 C25 1.380(16) . ? C24 H24 0.9300 . ? C25 N3 1.347(13) . ? C25 H25 0.9300 . ? C26 N3 1.337(14) . ? C26 C27 1.392(15) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C29 C28 1.544(15) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 C30 1.484(15) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? Se1 Pd1 2.4043(18) . ? Se2 Pd2 2.3965(17) . ? Se3 Pd3 2.3921(17) . ? Pd1 N3 2.146(10) . ? Pd1 P1 2.245(4) . ? Pd1 Cl1 2.333(4) . ? Pd2 N1 2.141(11) . ? Pd2 P2 2.239(5) . ? Pd2 Cl2 2.323(4) . ? Pd3 N2 2.140(9) . ? Pd3 P3 2.226(4) . ? Pd3 Cl3 2.339(4) . ? C18 C17 1.48(2) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C17 P2 1.776(18) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C22 C21 1.407(17) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C21 P2 1.909(16) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C28 P3 1.836(17) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C30 P3 1.763(19) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C32 C33 1.503(16) . ? C32 P3 1.761(19) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C19 C20 1.459(17) . ? C19 P2 1.91(2) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 119.1(14) . . ? C2 C1 Se1 119.0(13) . . ? C5 C1 Se1 121.5(13) . . ? C1 C2 C3 118.0(15) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? N1 C3 C2 123.8(14) . . ? N1 C3 H3 118.1 . . ? C2 C3 H3 118.1 . . ? N1 C4 C5 125.2(14) . . ? N1 C4 H4 117.4 . . ? C5 C4 H4 117.4 . . ? C4 C5 C1 117.5(14) . . ? C4 C5 H5 121.3 . . ? C1 C5 H5 121.3 . . ? C7 C6 P1 114.1(13) . . ? C7 C6 H6A 108.7 . . ? P1 C6 H6A 108.7 . . ? C7 C6 H6B 108.7 . . ? P1 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 P1 112.6(11) . . ? C9 C8 H8A 109.1 . . ? P1 C8 H8A 109.1 . . ? C9 C8 H8B 109.1 . . ? P1 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 119.0(12) . . ? C11 C10 H10A 107.6 . . ? P1 C10 H10A 107.6 . . ? C11 C10 H10B 107.6 . . ? P1 C10 H10B 107.6 . . ? H10A C10 H10B 107.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C16 114.7(12) . . ? C13 C12 Se2 124.7(10) . . ? C16 C12 Se2 120.6(11) . . ? C14 C13 C12 119.0(12) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? N2 C14 C13 125.3(13) . . ? N2 C14 H14 117.4 . . ? C13 C14 H14 117.4 . . ? N2 C15 C16 125.0(13) . . ? N2 C15 H15 117.5 . . ? C16 C15 H15 117.5 . . ? C15 C16 C12 119.9(13) . . ? C15 C16 H16 120.1 . . ? C12 C16 H16 120.1 . . ? C24 C23 C27 115.8(12) . . ? C24 C23 Se3 118.5(11) . . ? C27 C23 Se3 125.4(9) . . ? C23 C24 C25 121.7(13) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? N3 C25 C24 122.7(12) . . ? N3 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? N3 C26 C27 122.5(13) . . ? N3 C26 H26 118.8 . . ? C27 C26 H26 118.8 . . ? C26 C27 C23 120.3(11) . . ? C26 C27 H27 119.9 . . ? C23 C27 H27 119.9 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C1 Se1 Pd1 101.6(4) . . ? C12 Se2 Pd2 105.6(4) . . ? C23 Se3 Pd3 107.2(4) . . ? N3 Pd1 P1 177.0(3) . . ? N3 Pd1 Cl1 89.0(3) . . ? P1 Pd1 Cl1 93.65(14) . . ? N3 Pd1 Se1 90.4(3) . . ? P1 Pd1 Se1 86.95(11) . . ? Cl1 Pd1 Se1 178.71(13) . . ? N1 Pd2 P2 177.8(3) . . ? N1 Pd2 Cl2 88.5(3) . . ? P2 Pd2 Cl2 89.33(16) . . ? N1 Pd2 Se2 91.5(3) . . ? P2 Pd2 Se2 90.69(13) . . ? Cl2 Pd2 Se2 179.13(14) . . ? N2 Pd3 P3 177.6(3) . . ? N2 Pd3 Cl3 89.3(3) . . ? P3 Pd3 Cl3 89.61(16) . . ? N2 Pd3 Se3 91.7(3) . . ? P3 Pd3 Se3 89.61(13) . . ? Cl3 Pd3 Se3 172.44(13) . . ? C4 N1 C3 116.3(13) . . ? C4 N1 Pd2 122.5(11) . . ? C3 N1 Pd2 120.4(11) . . ? C14 N2 C15 115.9(11) . . ? C14 N2 Pd3 126.0(9) . . ? C15 N2 Pd3 117.8(9) . . ? C26 N3 C25 117.2(12) . . ? C26 N3 Pd1 119.1(9) . . ? C25 N3 Pd1 123.5(9) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18 C17 P2 117.9(15) . . ? C18 C17 H17A 107.8 . . ? P2 C17 H17A 107.8 . . ? C18 C17 H17B 107.8 . . ? P2 C17 H17B 107.8 . . ? H17A C17 H17B 107.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C22 C21 P2 119(2) . . ? C22 C21 H21A 107.7 . . ? P2 C21 H21A 107.7 . . ? C22 C21 H21B 107.7 . . ? P2 C21 H21B 107.7 . . ? H21A C21 H21B 107.1 . . ? C29 C28 P3 106.6(14) . . ? C29 C28 H28A 110.4 . . ? P3 C28 H28A 110.4 . . ? C29 C28 H28B 110.4 . . ? P3 C28 H28B 110.4 . . ? H28A C28 H28B 108.6 . . ? C31 C30 P3 122.3(17) . . ? C31 C30 H30A 106.8 . . ? P3 C30 H30A 106.8 . . ? C31 C30 H30B 106.8 . . ? P3 C30 H30B 106.8 . . ? H30A C30 H30B 106.6 . . ? C33 C32 P3 117.0(15) . . ? C33 C32 H32A 108.0 . . ? P3 C32 H32A 108.0 . . ? C33 C32 H32B 108.0 . . ? P3 C32 H32B 108.0 . . ? H32A C32 H32B 107.3 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C20 C19 P2 98.2(15) . . ? C20 C19 H19A 112.1 . . ? P2 C19 H19A 112.1 . . ? C20 C19 H19B 112.1 . . ? P2 C19 H19B 112.1 . . ? H19A C19 H19B 109.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C10 P1 C6 106.6(8) . . ? C10 P1 C8 105.2(8) . . ? C6 P1 C8 104.0(8) . . ? C10 P1 Pd1 114.2(6) . . ? C6 P1 Pd1 113.1(5) . . ? C8 P1 Pd1 112.9(5) . . ? C17 P2 C19 116.4(11) . . ? C17 P2 C21 100.0(11) . . ? C19 P2 C21 99.1(11) . . ? C17 P2 Pd2 113.1(8) . . ? C19 P2 Pd2 121.6(8) . . ? C21 P2 Pd2 101.0(7) . . ? C32 P3 C30 106.2(10) . . ? C32 P3 C28 96.5(9) . . ? C30 P3 C28 103.8(10) . . ? C32 P3 Pd3 110.5(6) . . ? C30 P3 Pd3 120.9(7) . . ? C28 P3 Pd3 115.9(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -2(2) . . . . ? Se1 C1 C2 C3 171.1(11) . . . . ? C1 C2 C3 N1 1(2) . . . . ? N1 C4 C5 C1 1(2) . . . . ? C2 C1 C5 C4 2(2) . . . . ? Se1 C1 C5 C4 -171.7(9) . . . . ? C16 C12 C13 C14 -1.0(18) . . . . ? Se2 C12 C13 C14 176.6(10) . . . . ? C12 C13 C14 N2 1(2) . . . . ? N2 C15 C16 C12 -5(2) . . . . ? C13 C12 C16 C15 2.5(19) . . . . ? Se2 C12 C16 C15 -175.2(10) . . . . ? C27 C23 C24 C25 2(2) . . . . ? Se3 C23 C24 C25 175.9(10) . . . . ? C23 C24 C25 N3 -1(2) . . . . ? N3 C26 C27 C23 0(2) . . . . ? C24 C23 C27 C26 -1(2) . . . . ? Se3 C23 C27 C26 -174.9(10) . . . . ? C2 C1 Se1 Pd1 127.2(11) . . . . ? C5 C1 Se1 Pd1 -59.4(11) . . . . ? C13 C12 Se2 Pd2 14.2(11) . . . . ? C16 C12 Se2 Pd2 -168.3(9) . . . . ? C24 C23 Se3 Pd3 160.6(10) . . . . ? C27 C23 Se3 Pd3 -25.9(13) . . . . ? C1 Se1 Pd1 N3 -48.5(6) . . . . ? C1 Se1 Pd1 P1 133.0(5) . . . . ? C1 Se1 Pd1 Cl1 -110(5) . . . . ? C12 Se2 Pd2 N1 53.1(5) . . . . ? C12 Se2 Pd2 P2 -127.5(4) . . . . ? C12 Se2 Pd2 Cl2 -37(8) . . . . ? C23 Se3 Pd3 N2 -48.5(5) . . . . ? C23 Se3 Pd3 P3 129.5(4) . . . . ? C23 Se3 Pd3 Cl3 -146.4(10) . . . . ? C5 C4 N1 C3 -2.5(19) . . . . ? C5 C4 N1 Pd2 167.3(10) . . . . ? C2 C3 N1 C4 2(2) . . . . ? C2 C3 N1 Pd2 -168.3(11) . . . . ? P2 Pd2 N1 C4 -109(10) . . . . ? Cl2 Pd2 N1 C4 -125.6(10) . . . . ? Se2 Pd2 N1 C4 55.3(10) . . . . ? P2 Pd2 N1 C3 60(10) . . . . ? Cl2 Pd2 N1 C3 43.8(10) . . . . ? Se2 Pd2 N1 C3 -135.4(9) . . . . ? C13 C14 N2 C15 -2.9(19) . . . . ? C13 C14 N2 Pd3 -177.2(10) . . . . ? C16 C15 N2 C14 5(2) . . . . ? C16 C15 N2 Pd3 179.4(11) . . . . ? P3 Pd3 N2 C14 -163(7) . . . . ? Cl3 Pd3 N2 C14 133.1(10) . . . . ? Se3 Pd3 N2 C14 -39.4(10) . . . . ? P3 Pd3 N2 C15 22(8) . . . . ? Cl3 Pd3 N2 C15 -41.1(9) . . . . ? Se3 Pd3 N2 C15 146.4(9) . . . . ? C27 C26 N3 C25 1.3(18) . . . . ? C27 C26 N3 Pd1 175.9(9) . . . . ? C24 C25 N3 C26 -0.8(19) . . . . ? C24 C25 N3 Pd1 -175.1(10) . . . . ? P1 Pd1 N3 C26 171(5) . . . . ? Cl1 Pd1 N3 C26 -39.9(9) . . . . ? Se1 Pd1 N3 C26 141.2(8) . . . . ? P1 Pd1 N3 C25 -15(6) . . . . ? Cl1 Pd1 N3 C25 134.3(10) . . . . ? Se1 Pd1 N3 C25 -44.6(9) . . . . ? C11 C10 P1 C6 56.1(16) . . . . ? C11 C10 P1 C8 -53.9(16) . . . . ? C11 C10 P1 Pd1 -178.2(12) . . . . ? C7 C6 P1 C10 74.6(14) . . . . ? C7 C6 P1 C8 -174.6(12) . . . . ? C7 C6 P1 Pd1 -51.8(14) . . . . ? C9 C8 P1 C10 -67.0(14) . . . . ? C9 C8 P1 C6 -178.9(12) . . . . ? C9 C8 P1 Pd1 58.1(13) . . . . ? N3 Pd1 P1 C10 140(5) . . . . ? Cl1 Pd1 P1 C10 -9.7(7) . . . . ? Se1 Pd1 P1 C10 169.2(7) . . . . ? N3 Pd1 P1 C6 -98(5) . . . . ? Cl1 Pd1 P1 C6 112.5(6) . . . . ? Se1 Pd1 P1 C6 -68.6(6) . . . . ? N3 Pd1 P1 C8 20(5) . . . . ? Cl1 Pd1 P1 C8 -129.7(6) . . . . ? Se1 Pd1 P1 C8 49.2(6) . . . . ? C18 C17 P2 C19 -90.6(19) . . . . ? C18 C17 P2 C21 163.9(18) . . . . ? C18 C17 P2 Pd2 57.3(18) . . . . ? C20 C19 P2 C17 58(2) . . . . ? C20 C19 P2 C21 164(2) . . . . ? C20 C19 P2 Pd2 -87(2) . . . . ? C22 C21 P2 C17 66(3) . . . . ? C22 C21 P2 C19 -53(3) . . . . ? C22 C21 P2 Pd2 -178(3) . . . . ? N1 Pd2 P2 C17 21(10) . . . . ? Cl2 Pd2 P2 C17 38.1(8) . . . . ? Se2 Pd2 P2 C17 -142.8(7) . . . . ? N1 Pd2 P2 C19 168(10) . . . . ? Cl2 Pd2 P2 C19 -175.8(8) . . . . ? Se2 Pd2 P2 C19 3.3(8) . . . . ? N1 Pd2 P2 C21 -84(10) . . . . ? Cl2 Pd2 P2 C21 -67.8(10) . . . . ? Se2 Pd2 P2 C21 111.3(10) . . . . ? C33 C32 P3 C30 64.8(18) . . . . ? C33 C32 P3 C28 171.2(17) . . . . ? C33 C32 P3 Pd3 -67.9(18) . . . . ? C31 C30 P3 C32 48(2) . . . . ? C31 C30 P3 C28 -53(2) . . . . ? C31 C30 P3 Pd3 174.8(16) . . . . ? C29 C28 P3 C32 177.3(16) . . . . ? C29 C28 P3 C30 -74.3(17) . . . . ? C29 C28 P3 Pd3 60.7(17) . . . . ? N2 Pd3 P3 C32 -137(7) . . . . ? Cl3 Pd3 P3 C32 -73.5(9) . . . . ? Se3 Pd3 P3 C32 99.0(9) . . . . ? N2 Pd3 P3 C30 98(7) . . . . ? Cl3 Pd3 P3 C30 161.7(8) . . . . ? Se3 Pd3 P3 C30 -25.8(8) . . . . ? N2 Pd3 P3 C28 -29(7) . . . . ? Cl3 Pd3 P3 C28 34.9(8) . . . . ? Se3 Pd3 P3 C28 -152.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.032 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.150 _database_code_depnum_ccdc_archive 'CCDC 924438' ####################################################################### # # 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_sdb2 #TrackingRef 'web_deposit_cif_file_7_Dr.SandipDey_1360841986.sdb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H38 Cl2 N2 P2 Pd2 Se2' _chemical_formula_weight 1122.34 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' Cl Cl 0.1484 0.1585 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.1799(12) _cell_length_b 14.6690(17) _cell_length_c 14.8568(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.4050(10) _cell_angle_gamma 90.00 _cell_volume 2214.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.683 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 2.683 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5536 _exptl_absorpt_correction_T_max 0.7390 _exptl_absorpt_process_details 'SADABS; (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'APEX II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24421 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.49 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _reflns_number_total 5068 _reflns_number_gt 4788 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-II (BRUKER-NONIUS, 2003)' _computing_cell_refinement ; APEX-II(BRUKER-NONIUS, 2003) ; _computing_data_reduction APEX-II _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Olex2 _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^)+(0.0187P)^2^+1.6290P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5068 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0178 _refine_ls_wR_factor_ref 0.0443 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.868141(11) 0.077874(8) 0.527846(8) 0.01295(4) Uani 1 1 d . . . Se1 Se 1.042696(15) 0.073103(10) 0.426227(10) 0.01334(4) Uani 1 1 d . . . Cl1 Cl 0.72099(4) 0.07153(3) 0.64177(3) 0.02093(9) Uani 1 1 d . . . P1 P 0.78862(4) 0.21656(3) 0.47917(3) 0.01302(8) Uani 1 1 d . . . N1 N 0.85109(18) 0.00469(12) 0.13745(11) 0.0338(4) Uani 1 1 d . . . C1 C 0.96112(16) 0.04316(11) 0.31004(11) 0.0174(3) Uani 1 1 d . . . C2 C 0.83448(18) 0.00833(12) 0.29846(12) 0.0246(4) Uani 1 1 d . . . H2 H 0.7833 -0.0029 0.3487 0.030 Uiso 1 1 calc R . . C3 C 0.7850(2) -0.00956(14) 0.21122(14) 0.0312(4) Uani 1 1 d . . . H3 H 0.6984 -0.0336 0.2034 0.037 Uiso 1 1 calc R . . C4 C 0.9733(2) 0.03736(14) 0.15091(13) 0.0319(4) Uani 1 1 d . . . H4 H 1.0226 0.0473 0.0995 0.038 Uiso 1 1 calc R . . C5 C 1.03281(18) 0.05764(12) 0.23479(12) 0.0238(4) Uani 1 1 d . . . H5 H 1.1201 0.0808 0.2406 0.029 Uiso 1 1 calc R . . C6 C 0.84245(15) 0.30686(11) 0.55713(11) 0.0168(3) Uani 1 1 d . . . C7 C 0.87859(17) 0.28457(13) 0.64657(12) 0.0233(4) Uani 1 1 d . . . H7 H 0.8781 0.2227 0.6656 0.028 Uiso 1 1 calc R . . C8 C 0.91521(19) 0.35297(14) 0.70774(13) 0.0300(4) Uani 1 1 d . . . H8 H 0.9394 0.3377 0.7686 0.036 Uiso 1 1 calc R . . C9 C 0.91671(19) 0.44308(14) 0.68070(14) 0.0297(4) Uani 1 1 d . . . H9 H 0.9416 0.4895 0.7230 0.036 Uiso 1 1 calc R . . C10 C 0.88195(19) 0.46573(13) 0.59213(13) 0.0280(4) Uani 1 1 d . . . H10 H 0.8836 0.5277 0.5736 0.034 Uiso 1 1 calc R . . C11 C 0.84448(17) 0.39804(12) 0.53001(12) 0.0211(3) Uani 1 1 d . . . H11 H 0.8203 0.4139 0.4693 0.025 Uiso 1 1 calc R . . C12 C 0.60979(15) 0.22221(11) 0.46682(10) 0.0163(3) Uani 1 1 d . . . C13 C 0.54642(17) 0.30641(12) 0.46060(13) 0.0259(4) Uani 1 1 d . . . H13 H 0.5965 0.3611 0.4633 0.031 Uiso 1 1 calc R . . C14 C 0.40963(19) 0.31024(14) 0.45043(15) 0.0342(5) Uani 1 1 d . . . H14 H 0.3664 0.3676 0.4468 0.041 Uiso 1 1 calc R . . C15 C 0.33670(17) 0.23100(14) 0.44563(13) 0.0291(4) Uani 1 1 d . . . H15 H 0.2434 0.2340 0.4388 0.035 Uiso 1 1 calc R . . C16 C 0.39905(17) 0.14708(13) 0.45077(12) 0.0240(4) Uani 1 1 d . . . H16 H 0.3486 0.0926 0.4470 0.029 Uiso 1 1 calc R . . C17 C 0.53572(16) 0.14263(11) 0.46149(11) 0.0190(3) Uani 1 1 d . . . H17 H 0.5784 0.0850 0.4652 0.023 Uiso 1 1 calc R . . C18 C 0.84122(16) 0.25313(10) 0.37012(10) 0.0152(3) Uani 1 1 d . . . C19 C 0.76142(17) 0.23983(12) 0.29146(11) 0.0211(3) Uani 1 1 d . . . H19 H 0.6746 0.2168 0.2949 0.025 Uiso 1 1 calc R . . C20 C 0.80933(19) 0.26037(13) 0.20800(12) 0.0276(4) Uani 1 1 d . . . H20 H 0.7547 0.2516 0.1546 0.033 Uiso 1 1 calc R . . C21 C 0.9359(2) 0.29346(13) 0.20206(12) 0.0275(4) Uani 1 1 d . . . H21 H 0.9680 0.3071 0.1449 0.033 Uiso 1 1 calc R . . C22 C 1.01564(18) 0.30654(12) 0.28004(12) 0.0229(4) Uani 1 1 d . . . H22 H 1.1025 0.3293 0.2762 0.028 Uiso 1 1 calc R . . C23 C 0.96898(16) 0.28659(11) 0.36339(11) 0.0182(3) Uani 1 1 d . . . H23 H 1.0241 0.2957 0.4165 0.022 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 0.01269(6) 0.01310(6) 0.01346(6) 0.00137(4) 0.00410(4) 0.00185(4) Se1 0.01235(8) 0.01339(8) 0.01459(8) 0.00107(5) 0.00338(6) 0.00059(5) Cl1 0.0219(2) 0.02138(19) 0.02074(19) 0.00424(14) 0.01186(15) 0.00553(15) P1 0.01243(18) 0.01324(18) 0.01361(18) 0.00081(14) 0.00250(14) 0.00053(14) N1 0.0419(10) 0.0333(9) 0.0254(8) -0.0072(7) -0.0056(7) 0.0003(8) C1 0.0202(8) 0.0143(7) 0.0174(8) -0.0014(6) 0.0003(6) 0.0026(6) C2 0.0220(9) 0.0257(9) 0.0265(9) -0.0062(7) 0.0031(7) -0.0018(7) C3 0.0272(10) 0.0307(10) 0.0349(11) -0.0106(8) -0.0052(8) -0.0026(8) C4 0.0426(12) 0.0337(10) 0.0196(9) -0.0011(8) 0.0044(8) -0.0001(9) C5 0.0260(9) 0.0261(9) 0.0196(8) 0.0008(7) 0.0030(7) -0.0004(7) C6 0.0136(7) 0.0190(8) 0.0179(8) -0.0035(6) 0.0022(6) 0.0004(6) C7 0.0238(9) 0.0264(9) 0.0196(8) -0.0005(7) 0.0007(7) 0.0009(7) C8 0.0280(10) 0.0428(11) 0.0189(9) -0.0068(8) -0.0004(7) 0.0001(8) C9 0.0230(9) 0.0347(10) 0.0317(10) -0.0168(8) 0.0035(8) -0.0028(8) C10 0.0286(10) 0.0196(9) 0.0360(10) -0.0079(7) 0.0041(8) -0.0021(7) C11 0.0208(8) 0.0195(8) 0.0229(8) -0.0020(7) 0.0007(7) 0.0000(6) C12 0.0142(7) 0.0194(8) 0.0155(7) 0.0011(6) 0.0024(6) 0.0003(6) C13 0.0176(9) 0.0190(8) 0.0409(11) 0.0011(7) 0.0012(7) 0.0005(6) C14 0.0196(9) 0.0262(10) 0.0562(13) -0.0013(9) -0.0021(9) 0.0069(7) C15 0.0134(8) 0.0366(10) 0.0370(10) -0.0037(8) -0.0003(7) -0.0005(7) C16 0.0191(8) 0.0289(9) 0.0239(9) -0.0016(7) 0.0006(7) -0.0060(7) C17 0.0192(8) 0.0191(8) 0.0188(8) -0.0006(6) 0.0014(6) -0.0001(6) C18 0.0177(8) 0.0128(7) 0.0155(7) 0.0014(6) 0.0039(6) 0.0018(6) C19 0.0209(8) 0.0231(8) 0.0193(8) 0.0002(6) 0.0012(6) -0.0017(6) C20 0.0342(10) 0.0317(10) 0.0166(8) 0.0002(7) 0.0002(7) 0.0003(8) C21 0.0370(11) 0.0267(9) 0.0201(9) 0.0050(7) 0.0119(8) 0.0018(8) C22 0.0225(9) 0.0199(8) 0.0273(9) 0.0045(7) 0.0091(7) -0.0001(7) C23 0.0188(8) 0.0147(7) 0.0213(8) 0.0015(6) 0.0031(6) 0.0005(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 P1 2.2908(4) . ? Pd1 Cl1 2.3278(4) . ? Pd1 Se1 2.4001(3) . ? Pd1 Se1 2.4739(3) 3_756 ? Se1 C1 1.9215(16) . ? Se1 Pd1 2.4740(3) 3_756 ? P1 C18 1.8172(16) . ? P1 C12 1.8207(16) . ? P1 C6 1.8223(16) . ? N1 C3 1.336(3) . ? N1 C4 1.337(3) . ? C1 C5 1.387(2) . ? C1 C2 1.388(2) . ? C2 C3 1.387(3) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 C7 1.396(2) . ? C6 C11 1.397(2) . ? C7 C8 1.390(3) . ? C7 H7 0.9500 . ? C8 C9 1.382(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.393(2) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.389(2) . ? C12 C13 1.394(2) . ? C13 C14 1.393(3) . ? C13 H13 0.9500 . ? C14 C15 1.379(3) . ? C14 H14 0.9500 . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 C17 1.393(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.397(2) . ? C18 C23 1.399(2) . ? C19 C20 1.392(2) . ? C19 H19 0.9500 . ? C20 C21 1.385(3) . ? C20 H20 0.9500 . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.384(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pd1 Cl1 91.975(15) . . ? P1 Pd1 Se1 95.063(12) . . ? Cl1 Pd1 Se1 171.368(12) . . ? P1 Pd1 Se1 177.509(12) . 3_756 ? Cl1 Pd1 Se1 90.291(12) . 3_756 ? Se1 Pd1 Se1 82.772(7) . 3_756 ? C1 Se1 Pd1 105.97(5) . . ? C1 Se1 Pd1 100.08(5) . 3_756 ? Pd1 Se1 Pd1 97.227(7) . 3_756 ? C18 P1 C12 104.04(7) . . ? C18 P1 C6 104.99(7) . . ? C12 P1 C6 106.98(7) . . ? C18 P1 Pd1 115.23(5) . . ? C12 P1 Pd1 113.87(5) . . ? C6 P1 Pd1 110.95(5) . . ? C3 N1 C4 116.27(16) . . ? C5 C1 C2 119.06(16) . . ? C5 C1 Se1 117.97(13) . . ? C2 C1 Se1 122.97(13) . . ? C3 C2 C1 117.92(17) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? N1 C3 C2 124.37(18) . . ? N1 C3 H3 117.8 . . ? C2 C3 H3 117.8 . . ? N1 C4 C5 124.40(18) . . ? N1 C4 H4 117.8 . . ? C5 C4 H4 117.8 . . ? C4 C5 C1 117.97(17) . . ? C4 C5 H5 121.0 . . ? C1 C5 H5 121.0 . . ? C7 C6 C11 119.40(15) . . ? C7 C6 P1 119.14(13) . . ? C11 C6 P1 121.43(13) . . ? C8 C7 C6 119.90(17) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.50(18) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 120.00(17) . . ? C8 C9 H9 120.0 . . ? C10 C9 H9 120.0 . . ? C9 C10 C11 120.24(18) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 119.96(16) . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? C17 C12 C13 119.55(15) . . ? C17 C12 P1 120.23(12) . . ? C13 C12 P1 120.20(13) . . ? C14 C13 C12 119.91(17) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C15 C14 C13 120.22(18) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.19(17) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 119.97(16) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C16 120.15(16) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C23 119.09(15) . . ? C19 C18 P1 121.14(12) . . ? C23 C18 P1 119.44(12) . . ? C20 C19 C18 119.85(16) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 120.61(17) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.71(16) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 120.20(17) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 120.53(16) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 Pd1 Se1 C1 -76.06(5) . . . . ? Cl1 Pd1 Se1 C1 139.44(9) . . . . ? Se1 Pd1 Se1 C1 102.70(5) 3_756 . . . ? P1 Pd1 Se1 Pd1 -178.762(12) . . . 3_756 ? Cl1 Pd1 Se1 Pd1 36.74(8) . . . 3_756 ? Se1 Pd1 Se1 Pd1 0.0 3_756 . . 3_756 ? Cl1 Pd1 P1 C18 -167.26(6) . . . . ? Se1 Pd1 P1 C18 17.74(6) . . . . ? Se1 Pd1 P1 C18 -11.8(3) 3_756 . . . ? Cl1 Pd1 P1 C12 -47.14(6) . . . . ? Se1 Pd1 P1 C12 137.86(6) . . . . ? Se1 Pd1 P1 C12 108.3(3) 3_756 . . . ? Cl1 Pd1 P1 C6 73.61(6) . . . . ? Se1 Pd1 P1 C6 -101.38(6) . . . . ? Se1 Pd1 P1 C6 -130.9(3) 3_756 . . . ? Pd1 Se1 C1 C5 164.44(12) . . . . ? Pd1 Se1 C1 C5 -94.97(13) 3_756 . . . ? Pd1 Se1 C1 C2 -15.30(15) . . . . ? Pd1 Se1 C1 C2 85.29(14) 3_756 . . . ? C5 C1 C2 C3 -0.6(3) . . . . ? Se1 C1 C2 C3 179.10(14) . . . . ? C4 N1 C3 C2 0.8(3) . . . . ? C1 C2 C3 N1 -0.2(3) . . . . ? C3 N1 C4 C5 -0.8(3) . . . . ? N1 C4 C5 C1 0.0(3) . . . . ? C2 C1 C5 C4 0.7(3) . . . . ? Se1 C1 C5 C4 -179.04(14) . . . . ? C18 P1 C6 C7 -148.14(13) . . . . ? C12 P1 C6 C7 101.72(14) . . . . ? Pd1 P1 C6 C7 -23.03(15) . . . . ? C18 P1 C6 C11 33.83(15) . . . . ? C12 P1 C6 C11 -76.31(15) . . . . ? Pd1 P1 C6 C11 158.94(12) . . . . ? C11 C6 C7 C8 0.5(3) . . . . ? P1 C6 C7 C8 -177.62(14) . . . . ? C6 C7 C8 C9 -0.3(3) . . . . ? C7 C8 C9 C10 -0.2(3) . . . . ? C8 C9 C10 C11 0.4(3) . . . . ? C9 C10 C11 C6 -0.2(3) . . . . ? C7 C6 C11 C10 -0.2(3) . . . . ? P1 C6 C11 C10 177.83(13) . . . . ? C18 P1 C12 C17 108.27(14) . . . . ? C6 P1 C12 C17 -140.93(13) . . . . ? Pd1 P1 C12 C17 -17.97(15) . . . . ? C18 P1 C12 C13 -70.28(15) . . . . ? C6 P1 C12 C13 40.52(16) . . . . ? Pd1 P1 C12 C13 163.48(12) . . . . ? C17 C12 C13 C14 0.9(3) . . . . ? P1 C12 C13 C14 179.48(16) . . . . ? C12 C13 C14 C15 -0.6(3) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C14 C15 C16 C17 0.5(3) . . . . ? C13 C12 C17 C16 -0.5(2) . . . . ? P1 C12 C17 C16 -179.10(13) . . . . ? C15 C16 C17 C12 -0.2(3) . . . . ? C12 P1 C18 C19 -28.20(15) . . . . ? C6 P1 C18 C19 -140.45(13) . . . . ? Pd1 P1 C18 C19 97.17(13) . . . . ? C12 P1 C18 C23 158.43(13) . . . . ? C6 P1 C18 C23 46.18(14) . . . . ? Pd1 P1 C18 C23 -76.19(13) . . . . ? C23 C18 C19 C20 -0.4(2) . . . . ? P1 C18 C19 C20 -173.76(14) . . . . ? C18 C19 C20 C21 0.4(3) . . . . ? C19 C20 C21 C22 -0.2(3) . . . . ? C20 C21 C22 C23 0.0(3) . . . . ? C21 C22 C23 C18 0.0(3) . . . . ? C19 C18 C23 C22 0.2(2) . . . . ? P1 C18 C23 C22 173.70(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.492 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.057 _database_code_depnum_ccdc_archive 'CCDC 924439' ####################################################################### # # 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_7c # start Validation Reply Form _vrf_PLAT026_I ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 22 % RESPONSE: Higly absorbing species present ; _vrf_PLAT029_I ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.946 RESPONSE: ... ; _vrf_PLAT220_I ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.4 Ratio RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; _vrf_PLAT222_I ; PROBLEM: Large Non-Solvent H Uiso(max)/Uiso(min) .. 7.9 Ratio RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; _vrf_PLAT242_I ; PROBLEM: Check Low Ueq as Compared to Neighbors for P1 RESPONSE: Due to largely disordered terminal triethyl phosphine groups and data collected at Room Temperature ; _vrf_PLAT342_I ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0381 Ang. RESPONSE: Presence of disorder as data collected at Room temperature ; # end Validation Reply Form # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 43 15 ' ' 2 0.500 0.000 1.000 43 15 ' ' _platon_squeeze_details ; A total of 30 electrons are present in the different voids These may correspond to water molecules ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H58 Cl6 N3 P3 Pt3 Se3' _chemical_formula_weight 1636.59 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' Se Se -0.0929 2.2259 '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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/a 1' _symmetry_space_group_name_Hall '-P 2yab' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 14.501(3) _cell_length_b 24.574(3) _cell_length_c 14.763(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.72(2) _cell_angle_gamma 90.00 _cell_volume 5131.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.1 _cell_measurement_theta_max 12.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 10.719 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.1413 _exptl_absorpt_correction_T_max 0.2962 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7S' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -13.49 _diffrn_reflns_number 14086 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_UnetI/netI 0.5167 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 28.02 _reflns_number_total 11757 _reflns_number_gt 2643 _reflns_threshold_expression >2sigma(I) _computing_data_collection WInAFC _computing_cell_refinement WinAFC _computing_data_reduction 'Crystal Structure' _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.0577P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11757 _refine_ls_number_parameters 363 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.3843 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2161 _refine_ls_wR_factor_gt 0.1331 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.885 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5831(9) 0.9286(6) 0.8022(13) 0.064(7) Uani 1 1 d G . . C2 C 0.5615(12) 0.9061(7) 0.8814(10) 0.072(8) Uani 1 1 d G . . H2 H 0.6034 0.9100 0.9386 0.086 Uiso 1 1 calc R . . C3 C 0.4774(14) 0.8778(6) 0.8751(12) 0.080(9) Uani 1 1 d G . . H3 H 0.4630 0.8627 0.9282 0.096 Uiso 1 1 calc R . . N1 N 0.4148(10) 0.8720(5) 0.7897(16) 0.077(7) Uani 1 1 d G . . C4 C 0.4363(11) 0.8945(6) 0.7105(11) 0.065(8) Uani 1 1 d G . . H4 H 0.3944 0.8906 0.6533 0.078 Uiso 1 1 calc R . . C5 C 0.5205(13) 0.9228(6) 0.7167(10) 0.071(8) Uani 1 1 d G . . H5 H 0.5349 0.9379 0.6637 0.085 Uiso 1 1 calc R . . C7 C 0.835(3) 1.0714(15) 0.533(3) 0.248(6) Uani 1 1 d DU . . H7A H 0.8772 1.0876 0.4997 0.372 Uiso 1 1 calc R . . H7B H 0.8417 1.0887 0.5926 0.372 Uiso 1 1 calc R . . H7C H 0.7707 1.0758 0.4986 0.372 Uiso 1 1 calc R . . C6 C 0.856(2) 1.0131(14) 0.547(3) 0.183 Uani 1 1 d DU . . H6A H 0.9224 1.0092 0.5764 0.219 Uiso 1 1 calc R . . H6B H 0.8464 0.9959 0.4862 0.219 Uiso 1 1 calc R . . C8 C 0.746(3) 0.9266(15) 0.521(3) 0.189(18) Uani 1 1 d DU . . H8A H 0.7004 0.9429 0.4705 0.227 Uiso 1 1 calc R . . H8B H 0.7994 0.9136 0.4978 0.227 Uiso 1 1 calc R . . C9 C 0.702(3) 0.8811(16) 0.564(3) 0.22(2) Uani 1 1 d DU . . H9A H 0.6345 0.8851 0.5493 0.329 Uiso 1 1 calc R . . H9B H 0.7244 0.8821 0.6306 0.329 Uiso 1 1 calc R . . H9C H 0.7188 0.8469 0.5410 0.329 Uiso 1 1 calc R . . C10 C 0.879(3) 0.9432(17) 0.690(3) 0.187(15) Uani 1 1 d DU . . H10A H 0.8541 0.9130 0.7200 0.225 Uiso 1 1 calc R . . H10B H 0.9203 0.9282 0.6532 0.225 Uiso 1 1 calc R . . C11 C 0.936(3) 0.978(2) 0.764(4) 0.28(3) Uani 1 1 d DU . . H11A H 0.9843 0.9569 0.8031 0.427 Uiso 1 1 calc R . . H11B H 0.8960 0.9942 0.8004 0.427 Uiso 1 1 calc R . . H11C H 0.9655 1.0068 0.7355 0.427 Uiso 1 1 calc R . . C12 C 0.2472(12) 0.9540(5) 0.8622(15) 0.080 Uani 1 1 d G . . C13 C 0.2317(12) 0.9649(6) 0.7677(14) 0.090(10) Uani 1 1 d G . . H13 H 0.2272 0.9364 0.7255 0.108 Uiso 1 1 calc R . . C14 C 0.2230(11) 1.0183(8) 0.7362(10) 0.077(8) Uani 1 1 d G . . H14 H 0.2126 1.0256 0.6730 0.092 Uiso 1 1 calc R . . N2 N 0.2298(10) 1.0609(5) 0.7993(14) 0.064(6) Uani 1 1 d G . . C15 C 0.2453(11) 1.0500(7) 0.8939(13) 0.066(8) Uani 1 1 d G . . H15 H 0.2498 1.0785 0.9361 0.079 Uiso 1 1 calc R . . C16 C 0.2540(12) 0.9966(9) 0.9253(10) 0.080(9) Uani 1 1 d G . . H16 H 0.2643 0.9893 0.9886 0.096 Uiso 1 1 calc R . . C17 C 0.193(3) 0.7060(14) 0.788(2) 0.169 Uani 1 1 d DU . . H17A H 0.1357 0.6848 0.7790 0.203 Uiso 1 1 calc R . . H17B H 0.2285 0.6937 0.7428 0.203 Uiso 1 1 calc R . . C18 C 0.251(2) 0.6962(14) 0.883(2) 0.191(10) Uani 1 1 d DU . . H18A H 0.2126 0.7019 0.9278 0.286 Uiso 1 1 calc R . . H18B H 0.3035 0.7210 0.8957 0.286 Uiso 1 1 calc R . . H18C H 0.2742 0.6595 0.8880 0.286 Uiso 1 1 calc R . . C19 C 0.097(3) 0.7751(14) 0.649(3) 0.186(11) Uani 1 1 d DU . . H19A H 0.1350 0.7587 0.6101 0.223 Uiso 1 1 calc R . . H19B H 0.0407 0.7531 0.6455 0.223 Uiso 1 1 calc R . . C20 C 0.070(3) 0.8319(15) 0.617(3) 0.24(2) Uani 1 1 d DU . . H20A H 0.0330 0.8310 0.5547 0.366 Uiso 1 1 calc R . . H20B H 0.1261 0.8530 0.6192 0.366 Uiso 1 1 calc R . . H20C H 0.0337 0.8481 0.6572 0.366 Uiso 1 1 calc R . . C21 C 0.093(3) 0.7970(16) 0.851(3) 0.206 Uani 1 1 d DU . . H21A H 0.1350 0.7997 0.9120 0.248 Uiso 1 1 calc R . . H21B H 0.0668 0.8329 0.8348 0.248 Uiso 1 1 calc R . . C22 C 0.016(3) 0.7595(19) 0.857(3) 0.301 Uani 1 1 d DU . . H22A H 0.0022 0.7618 0.9173 0.452 Uiso 1 1 calc R . . H22B H 0.0341 0.7230 0.8456 0.452 Uiso 1 1 calc R . . H22C H -0.0395 0.7693 0.8107 0.452 Uiso 1 1 calc R . . C23 C 0.4410(12) 1.1182(6) 0.7929(13) 0.081(9) Uani 1 1 d GU . . C24 C 0.4169(9) 1.0952(7) 0.7048(12) 0.075(8) Uani 1 1 d G . . H24 H 0.3565 1.1002 0.6683 0.090 Uiso 1 1 calc R . . C25 C 0.4830(13) 1.0648(6) 0.6712(9) 0.075(9) Uani 1 1 d G . . H25 H 0.4669 1.0495 0.6123 0.090 Uiso 1 1 calc R . . N3 N 0.5733(11) 1.0574(5) 0.7258(12) 0.059(6) Uani 1 1 d G . . C26 C 0.5975(9) 1.0804(6) 0.8139(11) 0.055(7) Uani 1 1 d G . . H26 H 0.6579 1.0754 0.8504 0.066 Uiso 1 1 calc R . . C27 C 0.5313(14) 1.1108(6) 0.8474(9) 0.062(7) Uani 1 1 d GU . . H27 H 0.5475 1.1261 0.9064 0.074 Uiso 1 1 calc R . . C28 C 0.101(2) 1.2394(11) 0.599(3) 0.173(12) Uani 1 1 d DU . . H28A H 0.1277 1.2250 0.5486 0.208 Uiso 1 1 calc R . . H28B H 0.0475 1.2168 0.6025 0.208 Uiso 1 1 calc R . . C29 C 0.065(3) 1.2956(12) 0.571(3) 0.22(2) Uani 1 1 d DU . . H29A H 0.1167 1.3209 0.5825 0.329 Uiso 1 1 calc R . . H29B H 0.0199 1.3058 0.6069 0.329 Uiso 1 1 calc R . . H29C H 0.0351 1.2959 0.5063 0.329 Uiso 1 1 calc R . . C30 C 0.171(3) 1.2686(15) 0.796(3) 0.174 Uani 1 1 d DU . . H30A H 0.2216 1.2950 0.8036 0.209 Uiso 1 1 calc R . . H30B H 0.1142 1.2888 0.7683 0.209 Uiso 1 1 calc R . . C31 C 0.160(4) 1.2621(17) 0.894(3) 0.28(3) Uani 1 1 d DU . . H31A H 0.1820 1.2943 0.9287 0.417 Uiso 1 1 calc R . . H31B H 0.1958 1.2313 0.9217 0.417 Uiso 1 1 calc R . . H31C H 0.0942 1.2565 0.8939 0.417 Uiso 1 1 calc R . . P1 P 0.7850(7) 0.9766(4) 0.6169(6) 0.106 Uani 1 1 d D . . P3 P 0.1892(6) 1.2301(4) 0.7054(7) 0.104(3) Uani 1 1 d U . . P2 P 0.1634(7) 0.7779(4) 0.7676(7) 0.110 Uani 1 1 d . . . Cl1 Cl 0.6241(6) 1.0636(3) 0.5299(5) 0.107(3) Uani 1 1 d . . . Cl3 Cl 0.0673(6) 1.1162(3) 0.6640(6) 0.119(3) Uani 1 1 d . . . Cl2 Cl 0.3304(6) 0.7775(3) 0.6613(6) 0.104(3) Uani 1 1 d . . . Se1 Se 0.70195(19) 0.95963(11) 0.81044(19) 0.0693(9) Uani 1 1 d . . . Se3 Se 0.3625(2) 1.16411(11) 0.8495(2) 0.0765(9) Uani 1 1 d . . . Se2 Se 0.2585(2) 0.88184(11) 0.9100(2) 0.0838(10) Uani 1 1 d . . . Pt1 Pt 0.67270(8) 1.01527(4) 0.67067(7) 0.0642(4) Uani 1 1 d . . . Pt3 Pt 0.21263(8) 1.14305(4) 0.75190(8) 0.0673(4) Uani 1 1 d . . . Pt2 Pt 0.29140(8) 0.82842(4) 0.78260(8) 0.0704(4) Uani 1 1 d . . . Cl3S Cl 0.9763(17) 0.1822(7) 0.9135(17) 0.436(15) Uani 1 1 d GD . . Cl2S Cl 0.8670(12) 0.0896(9) 0.8688(19) 0.49(2) Uani 1 1 d GD . . Cl4S Cl 1.0404(16) 0.0825(10) 0.9832(18) 0.49(2) Uani 1 1 d GD . . C1S C 0.9763(18) 0.1142(10) 0.891(2) 0.29(4) Uani 1 1 d D . . H1S H 1.0044 0.1078 0.8375 0.344 Uiso 1 1 calc R . . C32 C 0.282(2) 1.2733(17) 0.689(3) 0.182(17) Uani 1 1 d DU . . H32A H 0.2609 1.3108 0.6850 0.218 Uiso 1 1 calc R . . H32B H 0.3351 1.2702 0.7424 0.218 Uiso 1 1 calc R . . C33 C 0.313(4) 1.258(3) 0.603(4) 0.35(4) Uani 1 1 d DU . . H33A H 0.3642 1.2810 0.5950 0.520 Uiso 1 1 calc R . . H33B H 0.2613 1.2615 0.5502 0.520 Uiso 1 1 calc R . . H33C H 0.3346 1.2206 0.6074 0.520 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.059(19) 0.059(17) 0.063 -0.010 -0.007 0.023(14) C2 0.08(2) 0.09(2) 0.039(17) 0.019(15) 0.011(16) -0.018(18) C3 0.09(3) 0.038(16) 0.12(3) -0.017(17) 0.05(2) -0.030(16) N1 0.055(16) 0.067(15) 0.11(2) 0.002(15) 0.015(16) -0.032(12) C4 0.08(2) 0.040(16) 0.08(2) -0.012(15) 0.038(19) -0.016(15) C5 0.11(3) 0.041(16) 0.059(19) 0.009(13) 0.017(19) -0.011(16) C7 0.242 0.250 0.242 0.07(4) 0.03(4) -0.019 C6 0.188 0.163 0.183 0.09(3) 0.008 -0.014 C8 0.18(4) 0.21(5) 0.20(4) 0.03(4) 0.09(3) 0.07(4) C9 0.32(6) 0.18(4) 0.20(4) 0.08(3) 0.13(4) 0.03(4) C10 0.13(4) 0.255 0.17(4) -0.01(3) 0.02(3) 0.07(3) C11 0.19(5) 0.32(5) 0.31(6) -0.09(5) -0.017 -0.10(4) C12 0.072 0.076 0.081 0.021(18) -0.004 -0.021 C13 0.09(2) 0.039(17) 0.15(3) -0.012(18) 0.05(2) -0.004(15) C14 0.09(2) 0.058(18) 0.08(2) -0.022(19) 0.021(18) -0.013(18) N2 0.041(14) 0.063(15) 0.089(18) -0.019(14) 0.016(13) -0.007(11) C15 0.08(2) 0.07(2) 0.05(2) -0.029(15) 0.019(17) -0.020(16) C16 0.08(2) 0.061(19) 0.09(2) -0.003(19) 0.003(18) 0.007(16) C17 0.141 0.166 0.174 -0.028 -0.022 -0.010 C18 0.11(3) 0.179 0.236 0.07(3) -0.05(3) -0.091 C19 0.193 0.14(3) 0.198 -0.056 -0.010 -0.09(3) C20 0.20(4) 0.25(5) 0.242 -0.12(4) -0.021 -0.11(4) C21 0.159 0.163 0.248 -0.010 -0.062 -0.08(3) C22 0.281 0.281 0.273 -0.130 -0.090 -0.05(4) C23 0.076(19) 0.068(18) 0.10(3) 0.010(18) 0.019(16) 0.018(17) C24 0.10(2) 0.065 0.055 -0.004 -0.004 -0.002 C25 0.08(2) 0.055(17) 0.07(2) 0.006(15) -0.026(19) 0.014(16) N3 0.061(16) 0.068(14) 0.050(14) 0.002(12) 0.016(13) -0.008(12) C26 0.034 0.066(17) 0.051(18) 0.003 -0.020(14) 0.023(13) C27 0.081(18) 0.030(14) 0.07(2) 0.010(13) 0.018(16) -0.014(15) C28 0.13(3) 0.10(2) 0.221 -0.02(2) -0.104(16) 0.00(2) C29 0.18(4) 0.14(3) 0.29(5) 0.03(3) -0.06(4) 0.05(3) C30 0.141 0.181 0.188 -0.060(14) 0.010 0.05(3) C31 0.46(9) 0.21(4) 0.130(13) -0.068 0.001 0.13(4) P1 0.097 0.126 0.087 -0.008 0.004 0.018(6) P3 0.082(7) 0.106 0.113(6) -0.004 0.001 0.009(5) P2 0.093 0.097 0.128 -0.013(6) 0.002 -0.018(6) Cl1 0.111(7) 0.131(7) 0.086(6) 0.038(5) 0.037(6) 0.024(6) Cl3 0.088(6) 0.094(6) 0.144(8) -0.003(6) -0.038(6) -0.004(5) Cl2 0.123(7) 0.086(5) 0.114(7) -0.032(5) 0.052(6) -0.018(5) Se1 0.060(2) 0.079(2) 0.068(2) 0.0048(15) 0.0121(17) 0.0017(15) Se3 0.070(2) 0.0640(18) 0.093(2) -0.0205(16) 0.0114(18) 0.0053(16) Se2 0.124(3) 0.0612(18) 0.075(2) -0.0016(16) 0.041(2) -0.0104(18) Pt1 0.0613(8) 0.0715(7) 0.0626(8) 0.0008(6) 0.0200(6) -0.0007(6) Pt3 0.0664(8) 0.0523(7) 0.0812(9) -0.0071(6) 0.0116(7) 0.0094(6) Pt2 0.0886(9) 0.0513(7) 0.0730(8) -0.0035(6) 0.0212(7) -0.0134(7) Cl3S 0.43(4) 0.48(4) 0.38(3) -0.06(3) 0.05(3) -0.03(3) Cl2S 0.26(2) 0.42(3) 0.87(6) -0.23(4) 0.32(3) -0.12(2) Cl4S 0.38(4) 0.68(5) 0.41(3) 0.18(3) 0.08(3) 0.30(4) C1S 0.46(12) 0.11(4) 0.32(8) -0.07(5) 0.12(8) -0.04(6) C32 0.08(3) 0.26(5) 0.17(4) 0.08(3) -0.044(15) -0.04(2) C33 0.25(7) 0.54(11) 0.30(7) 0.20(6) 0.17(6) 0.10(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3900 . ? C1 C5 1.3900 . ? C1 Se1 1.864(13) . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 N1 1.3900 . ? C3 H3 0.9300 . ? N1 C4 1.3900 . ? N1 Pt2 2.068(12) . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C6 1.469(19) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C6 P1 1.849(18) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C8 C9 1.498(19) . ? C8 P1 1.86(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C11 1.489(19) . ? C10 P1 1.75(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.3900 . ? C12 C16 1.3900 . ? C12 Se2 1.902(12) . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 N2 1.3900 . ? C14 H14 0.9300 . ? N2 C15 1.3900 . ? N2 Pt3 2.133(12) . ? C15 C16 1.3900 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.490(18) . ? C17 P2 1.83(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.499(19) . ? C19 P2 1.80(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.470(19) . ? C21 P2 1.82(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.3900 . ? C23 C27 1.3900 . ? C23 Se3 1.921(12) . ? C24 C25 1.3900 . ? C24 H24 0.9300 . ? C25 N3 1.3900 . ? C25 H25 0.9300 . ? N3 C26 1.3900 . ? N3 Pt1 2.080(12) . ? C26 C27 1.3900 . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.503(18) . ? C28 P3 1.81(3) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.490(19) . ? C30 P3 1.71(3) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? P1 Pt1 2.181(9) . ? P3 C32 1.77(4) . ? P3 Pt3 2.250(9) . ? P2 Pt2 2.203(9) . ? Cl1 Pt1 2.362(7) . ? Cl3 Pt3 2.315(7) . ? Cl2 Pt2 2.353(7) . ? Se1 Pt1 2.434(3) . ? Se3 Pt3 2.385(3) . ? Se2 Pt2 2.426(3) . ? Cl3S C1S 1.704(18) . ? Cl2S C1S 1.659(19) . ? Cl4S C1S 1.660(19) . ? C1S H1S 0.9800 . ? C32 C33 1.498(14) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 120.0 . . ? C2 C1 Se1 118.9(12) . . ? C5 C1 Se1 120.8(12) . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 N1 120.0 . . ? C2 C3 H3 120.0 . . ? N1 C3 H3 120.0 . . ? C4 N1 C3 120.0 . . ? C4 N1 Pt2 121.0(13) . . ? C3 N1 Pt2 119.0(13) . . ? C5 C4 N1 120.0 . . ? C5 C4 H4 120.0 . . ? N1 C4 H4 120.0 . . ? C4 C5 C1 120.0 . . ? C4 C5 H5 120.0 . . ? C1 C5 H5 120.0 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C7 C6 P1 115(3) . . ? C7 C6 H6A 108.6 . . ? P1 C6 H6A 108.6 . . ? C7 C6 H6B 108.6 . . ? P1 C6 H6B 108.6 . . ? H6A C6 H6B 107.5 . . ? C9 C8 P1 105(3) . . ? C9 C8 H8A 110.8 . . ? P1 C8 H8A 110.8 . . ? C9 C8 H8B 110.8 . . ? P1 C8 H8B 110.8 . . ? H8A C8 H8B 108.9 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 114(3) . . ? C11 C10 H10A 108.7 . . ? P1 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? P1 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C16 120.0 . . ? C13 C12 Se2 122.2(13) . . ? C16 C12 Se2 117.8(13) . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 N2 120.0 . . ? C13 C14 H14 120.0 . . ? N2 C14 H14 120.0 . . ? C15 N2 C14 120.0 . . ? C15 N2 Pt3 119.5(12) . . ? C14 N2 Pt3 120.4(12) . . ? N2 C15 C16 120.0 . . ? N2 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C12 120.0 . . ? C15 C16 H16 120.0 . . ? C12 C16 H16 120.0 . . ? C18 C17 P2 112(3) . . ? C18 C17 H17A 109.2 . . ? P2 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? P2 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 P2 108(3) . . ? C20 C19 H19A 110.0 . . ? P2 C19 H19A 110.0 . . ? C20 C19 H19B 110.0 . . ? P2 C19 H19B 110.0 . . ? H19A C19 H19B 108.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 P2 115(3) . . ? C22 C21 H21A 108.5 . . ? P2 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? P2 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C27 120.0 . . ? C24 C23 Se3 126.5(12) . . ? C27 C23 Se3 113.5(12) . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? N3 C25 C24 120.0 . . ? N3 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C26 N3 C25 120.0 . . ? C26 N3 Pt1 121.0(11) . . ? C25 N3 Pt1 118.9(11) . . ? N3 C26 C27 120.0 . . ? N3 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C23 120.0 . . ? C26 C27 H27 120.0 . . ? C23 C27 H27 120.0 . . ? C29 C28 P3 119(2) . . ? C29 C28 H28A 107.5 . . ? P3 C28 H28A 107.5 . . ? C29 C28 H28B 107.5 . . ? P3 C28 H28B 107.5 . . ? H28A C28 H28B 107.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 P3 140(3) . . ? C31 C30 H30A 102.0 . . ? P3 C30 H30A 102.0 . . ? C31 C30 H30B 102.0 . . ? P3 C30 H30B 102.0 . . ? H30A C30 H30B 104.8 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C10 P1 C6 96.9(19) . . ? C10 P1 C8 103.1(19) . . ? C6 P1 C8 90.5(18) . . ? C10 P1 Pt1 121.4(14) . . ? C6 P1 Pt1 123.1(13) . . ? C8 P1 Pt1 115.9(13) . . ? C30 P3 C32 91.6(19) . . ? C30 P3 C28 114.4(18) . . ? C32 P3 C28 102.7(17) . . ? C30 P3 Pt3 109.0(14) . . ? C32 P3 Pt3 122.8(15) . . ? C28 P3 Pt3 114.6(10) . . ? C19 P2 C21 114(2) . . ? C19 P2 C17 100.3(16) . . ? C21 P2 C17 106.6(19) . . ? C19 P2 Pt2 112.2(14) . . ? C21 P2 Pt2 111.7(12) . . ? C17 P2 Pt2 111.3(13) . . ? C1 Se1 Pt1 100.8(6) . . ? C23 Se3 Pt3 99.1(6) . . ? C12 Se2 Pt2 103.5(7) . . ? N3 Pt1 P1 175.3(5) . . ? N3 Pt1 Cl1 89.8(5) . . ? P1 Pt1 Cl1 90.0(3) . . ? N3 Pt1 Se1 87.4(4) . . ? P1 Pt1 Se1 93.4(3) . . ? Cl1 Pt1 Se1 172.3(2) . . ? N2 Pt3 P3 177.4(5) . . ? N2 Pt3 Cl3 86.6(5) . . ? P3 Pt3 Cl3 92.4(3) . . ? N2 Pt3 Se3 89.0(5) . . ? P3 Pt3 Se3 92.0(2) . . ? Cl3 Pt3 Se3 175.4(2) . . ? N1 Pt2 P2 175.7(6) . . ? N1 Pt2 Cl2 87.9(5) . . ? P2 Pt2 Cl2 87.8(3) . . ? N1 Pt2 Se2 89.8(5) . . ? P2 Pt2 Se2 94.5(3) . . ? Cl2 Pt2 Se2 177.5(2) . . ? Cl2S C1S Cl4S 109.3(13) . . ? Cl2S C1S Cl3S 110.8(13) . . ? Cl4S C1S Cl3S 109.0(12) . . ? Cl2S C1S H1S 109.3 . . ? Cl4S C1S H1S 109.3 . . ? Cl3S C1S H1S 109.3 . . ? C33 C32 P3 110(3) . . ? C33 C32 H32A 109.7 . . ? P3 C32 H32A 109.7 . . ? C33 C32 H32B 109.7 . . ? P3 C32 H32B 109.7 . . ? H32A C32 H32B 108.2 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 0.0 . . . . ? Se1 C1 C2 C3 -173.3(10) . . . . ? C1 C2 C3 N1 0.0 . . . . ? C2 C3 N1 C4 0.0 . . . . ? C2 C3 N1 Pt2 178.9(9) . . . . ? C3 N1 C4 C5 0.0 . . . . ? Pt2 N1 C4 C5 -178.9(10) . . . . ? N1 C4 C5 C1 0.0 . . . . ? C2 C1 C5 C4 0.0 . . . . ? Se1 C1 C5 C4 173.2(10) . . . . ? C16 C12 C13 C14 0.0 . . . . ? Se2 C12 C13 C14 179.3(12) . . . . ? C12 C13 C14 N2 0.0 . . . . ? C13 C14 N2 C15 0.0 . . . . ? C13 C14 N2 Pt3 -178.3(10) . . . . ? C14 N2 C15 C16 0.0 . . . . ? Pt3 N2 C15 C16 178.3(10) . . . . ? N2 C15 C16 C12 0.0 . . . . ? C13 C12 C16 C15 0.0 . . . . ? Se2 C12 C16 C15 -179.4(12) . . . . ? C27 C23 C24 C25 0.0 . . . . ? Se3 C23 C24 C25 176.9(11) . . . . ? C23 C24 C25 N3 0.0 . . . . ? C24 C25 N3 C26 0.0 . . . . ? C24 C25 N3 Pt1 -176.7(9) . . . . ? C25 N3 C26 C27 0.0 . . . . ? Pt1 N3 C26 C27 176.6(9) . . . . ? N3 C26 C27 C23 0.0 . . . . ? C24 C23 C27 C26 0.0 . . . . ? Se3 C23 C27 C26 -177.3(10) . . . . ? C11 C10 P1 C6 76(4) . . . . ? C11 C10 P1 C8 168(4) . . . . ? C11 C10 P1 Pt1 -60(5) . . . . ? C7 C6 P1 C10 -132(4) . . . . ? C7 C6 P1 C8 125(4) . . . . ? C7 C6 P1 Pt1 3(4) . . . . ? C9 C8 P1 C10 70(3) . . . . ? C9 C8 P1 C6 167(3) . . . . ? C9 C8 P1 Pt1 -65(3) . . . . ? C31 C30 P3 C32 -131(6) . . . . ? C31 C30 P3 C28 125(6) . . . . ? C31 C30 P3 Pt3 -5(6) . . . . ? C29 C28 P3 C30 41(5) . . . . ? C29 C28 P3 C32 -57(4) . . . . ? C29 C28 P3 Pt3 167(3) . . . . ? C20 C19 P2 C21 70(4) . . . . ? C20 C19 P2 C17 -177(4) . . . . ? C20 C19 P2 Pt2 -59(4) . . . . ? C22 C21 P2 C19 62(4) . . . . ? C22 C21 P2 C17 -48(4) . . . . ? C22 C21 P2 Pt2 -170(3) . . . . ? C18 C17 P2 C19 179(3) . . . . ? C18 C17 P2 C21 -62(3) . . . . ? C18 C17 P2 Pt2 61(3) . . . . ? C2 C1 Se1 Pt1 -161.7(6) . . . . ? C5 C1 Se1 Pt1 25.0(8) . . . . ? C24 C23 Se3 Pt3 17.8(8) . . . . ? C27 C23 Se3 Pt3 -165.1(6) . . . . ? C13 C12 Se2 Pt2 17.9(9) . . . . ? C16 C12 Se2 Pt2 -162.7(7) . . . . ? C26 N3 Pt1 P1 -45(7) . . . . ? C25 N3 Pt1 P1 131(6) . . . . ? C26 N3 Pt1 Cl1 -133.1(7) . . . . ? C25 N3 Pt1 Cl1 43.5(7) . . . . ? C26 N3 Pt1 Se1 54.1(7) . . . . ? C25 N3 Pt1 Se1 -129.3(7) . . . . ? C10 P1 Pt1 N3 77(7) . . . . ? C6 P1 Pt1 N3 -48(7) . . . . ? C8 P1 Pt1 N3 -157(6) . . . . ? C10 P1 Pt1 Cl1 164.4(18) . . . . ? C6 P1 Pt1 Cl1 39.9(16) . . . . ? C8 P1 Pt1 Cl1 -69.3(15) . . . . ? C10 P1 Pt1 Se1 -22.5(18) . . . . ? C6 P1 Pt1 Se1 -147.0(16) . . . . ? C8 P1 Pt1 Se1 103.8(14) . . . . ? C1 Se1 Pt1 N3 61.2(7) . . . . ? C1 Se1 Pt1 P1 -123.5(6) . . . . ? C1 Se1 Pt1 Cl1 -7.3(17) . . . . ? C15 N2 Pt3 P3 -55(13) . . . . ? C14 N2 Pt3 P3 123(12) . . . . ? C15 N2 Pt3 Cl3 -122.3(8) . . . . ? C14 N2 Pt3 Cl3 56.0(8) . . . . ? C15 N2 Pt3 Se3 56.5(8) . . . . ? C14 N2 Pt3 Se3 -125.3(8) . . . . ? C30 P3 Pt3 N2 42(13) . . . . ? C32 P3 Pt3 N2 147(12) . . . . ? C28 P3 Pt3 N2 -88(13) . . . . ? C30 P3 Pt3 Cl3 108.8(15) . . . . ? C32 P3 Pt3 Cl3 -146.3(17) . . . . ? C28 P3 Pt3 Cl3 -20.8(17) . . . . ? C30 P3 Pt3 Se3 -69.8(15) . . . . ? C32 P3 Pt3 Se3 35.1(17) . . . . ? C28 P3 Pt3 Se3 160.7(17) . . . . ? C23 Se3 Pt3 N2 63.0(7) . . . . ? C23 Se3 Pt3 P3 -119.4(5) . . . . ? C23 Se3 Pt3 Cl3 79(3) . . . . ? C4 N1 Pt2 P2 58(9) . . . . ? C3 N1 Pt2 P2 -121(9) . . . . ? C4 N1 Pt2 Cl2 50.4(7) . . . . ? C3 N1 Pt2 Cl2 -128.5(7) . . . . ? C4 N1 Pt2 Se2 -130.6(7) . . . . ? C3 N1 Pt2 Se2 50.5(7) . . . . ? C19 P2 Pt2 N1 -59(9) . . . . ? C21 P2 Pt2 N1 172(9) . . . . ? C17 P2 Pt2 N1 53(9) . . . . ? C19 P2 Pt2 Cl2 -51.4(16) . . . . ? C21 P2 Pt2 Cl2 179.2(15) . . . . ? C17 P2 Pt2 Cl2 60.1(13) . . . . ? C19 P2 Pt2 Se2 129.7(16) . . . . ? C21 P2 Pt2 Se2 0.3(15) . . . . ? C17 P2 Pt2 Se2 -118.8(13) . . . . ? C12 Se2 Pt2 N1 61.8(8) . . . . ? C12 Se2 Pt2 P2 -118.9(6) . . . . ? C12 Se2 Pt2 Cl2 86(5) . . . . ? C30 P3 C32 C33 -172(4) . . . . ? C28 P3 C32 C33 -57(4) . . . . ? Pt3 P3 C32 C33 74(4) . . . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 1.000 _refine_diff_density_min -1.247 _refine_diff_density_rms 0.215 _iucr_refine_instructions_details ; TITL CELL 0.71069 14.5008 24.5744 14.7630 90.000 102.720 90.000 ZERR 4.00 0.0031 0.0027 0.0037 0.000 0.020 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, - Z SFAC C H N P CL SE PT UNIT 136 232 12 12 24 12 12 MERG 2 DFIX 1.51 C32 C33 DFIX 1.51 C6 C7 DFIX 1.51 C30 C31 C8 C9 C28 C29 DFIX 1.51 C32 C33 DFIX 1.51 C10 C11 DFIX 1.82 P1 C6 SIMU P1 C6 C7 C8 C9 C10 C11 SIMU P2 C17 C18 C19 C20 C21 C22 DELU P3 C28 C29 C30 C31 C32 C33 DFIX 1.510 0.020 C22 C21 DFIX 1.510 0.020 C17 C18 DFIX 1.510 0.020 C19 C20 DFIX 1.670 0.020 CL4S C1S DFIX 1.670 0.020 C1S CL3S DFIX 1.670 0.020 C1S CL2S DELU 0.010 0.010 C23 C27 FMAP 2 PLAN 25 SIZE 0.15 0.15 0.30 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 40 TEMP 25.00 WGHT 0.057700 FVAR 0.01360 AFIX 66 C1 1 0.583067 0.928621 0.802161 11.00000 0.05946 0.05935 = 10.06349 9.98985 9.99317 0.02295 C2 1 0.561525 0.906123 0.881386 11.00000 0.08117 0.09305 = 0.03911 0.01924 0.01064 -0.01800 AFIX 43 H2 2 0.603409 0.910019 0.938568 11.00000 -1.20000 AFIX 65 C3 1 0.477382 0.877803 0.875146 11.00000 0.08869 0.03763 = 0.12494 -0.01746 0.04602 -0.02999 AFIX 43 H3 2 0.462969 0.862750 0.928152 11.00000 -1.20000 AFIX 65 N1 3 0.414780 0.871980 0.789681 11.00000 0.05475 0.06701 = 0.10729 0.00157 0.01537 -0.03247 C4 1 0.436320 0.894478 0.710455 11.00000 0.08098 0.04040 = 0.08261 -0.01200 0.03772 -0.01611 AFIX 43 H4 2 0.394435 0.890582 0.653274 11.00000 -1.20000 AFIX 65 C5 1 0.520463 0.922798 0.716694 11.00000 0.11152 0.04079 = 0.05880 0.00913 0.01693 -0.01111 AFIX 43 H5 2 0.534876 0.937850 0.663687 11.00000 -1.20000 AFIX 0 C7 1 0.834542 1.071367 0.533212 11.00000 10.24152 10.25044 = 10.24180 0.07147 0.03260 9.98092 AFIX 33 H7A 2 0.877164 1.087648 0.499693 11.00000 -1.50000 H7B 2 0.841658 1.088745 0.592590 11.00000 -1.50000 H7C 2 0.770702 1.075767 0.498583 11.00000 -1.50000 AFIX 0 C6 1 0.856125 1.013123 0.546635 11.00000 10.18780 10.16257 = 10.18258 0.08953 10.00807 9.98603 AFIX 23 H6A 2 0.922446 1.009209 0.576368 11.00000 -1.20000 H6B 2 0.846439 0.995877 0.486171 11.00000 -1.20000 AFIX 0 C8 1 0.745987 0.926605 0.521214 11.00000 0.17985 0.20612 = 0.20344 0.03339 0.08996 0.07349 AFIX 23 H8A 2 0.700363 0.942902 0.470477 11.00000 -1.20000 H8B 2 0.799432 0.913591 0.497765 11.00000 -1.20000 AFIX 0 C9 1 0.701968 0.881119 0.564435 11.00000 0.31662 0.17970 = 0.19522 0.08417 0.13075 0.03383 AFIX 137 H9A 2 0.634456 0.885114 0.549348 11.00000 -1.50000 H9B 2 0.724413 0.882144 0.630634 11.00000 -1.50000 H9C 2 0.718819 0.846946 0.541023 11.00000 -1.50000 AFIX 0 C10 1 0.879072 0.943181 0.690443 11.00000 0.12666 10.25488 = 0.17327 -0.00718 0.01799 0.06566 AFIX 23 H10A 2 0.854075 0.913017 0.719999 11.00000 -1.20000 H10B 2 0.920285 0.928161 0.653174 11.00000 -1.20000 AFIX 0 C11 1 0.936304 0.978372 0.763889 11.00000 0.18973 0.31564 = 0.31467 -0.08795 9.98284 -0.09707 AFIX 33 H11A 2 0.984272 0.956857 0.803138 11.00000 -1.50000 H11B 2 0.896009 0.994164 0.800417 11.00000 -1.50000 H11C 2 0.965541 1.006788 0.735478 11.00000 -1.50000 AFIX 66 C12 1 0.247214 0.953984 0.862236 11.00000 10.07201 10.07560 = 10.08148 0.02077 9.99580 9.97895 C13 1 0.231719 0.964859 0.767688 11.00000 0.09326 0.03908 = 0.14860 -0.01190 0.04800 -0.00350 AFIX 43 H13 2 0.227189 0.936364 0.725480 11.00000 -1.20000 AFIX 65 C14 1 0.222994 1.018322 0.736223 11.00000 0.08984 0.05777 = 0.08395 -0.02177 0.02120 -0.01329 AFIX 43 H14 2 0.212626 1.025598 0.672964 11.00000 -1.20000 AFIX 65 N2 3 0.229763 1.060912 0.799306 11.00000 0.04119 0.06318 = 0.08929 -0.01853 0.01573 -0.00739 C15 1 0.245258 1.050039 0.893854 11.00000 0.07802 0.07066 = 0.05076 -0.02879 0.01859 -0.02019 AFIX 43 H15 2 0.249787 1.078535 0.936061 11.00000 -1.20000 AFIX 65 C16 1 0.253983 0.996575 0.925320 11.00000 0.08108 0.06058 = 0.09005 -0.00283 0.00336 0.00688 AFIX 43 H16 2 0.264350 0.989299 0.988579 11.00000 -1.20000 AFIX 0 C17 1 0.193442 0.705956 0.787912 11.00000 10.14138 10.16567 = 10.17363 9.97233 9.97846 9.98989 AFIX 23 H17A 2 0.135699 0.684774 0.779029 11.00000 -1.20000 H17B 2 0.228479 0.693698 0.742823 11.00000 -1.20000 AFIX 0 C18 1 0.251070 0.696213 0.883321 11.00000 0.11478 10.17914 = 10.23622 0.07356 -0.05143 9.90869 AFIX 137 H18A 2 0.212617 0.701871 0.927753 11.00000 -1.50000 H18B 2 0.303510 0.721005 0.895666 11.00000 -1.50000 H18C 2 0.274203 0.659488 0.887998 11.00000 -1.50000 AFIX 0 C19 1 0.097041 0.775061 0.649308 11.00000 10.19266 0.14234 = 10.19787 9.94406 9.98987 -0.09202 AFIX 23 H19A 2 0.135036 0.758658 0.610131 11.00000 -1.20000 H19B 2 0.040731 0.753095 0.645452 11.00000 -1.20000 AFIX 0 C20 1 0.070020 0.831904 0.617205 11.00000 0.20330 0.25483 = 10.24243 -0.11638 9.97923 -0.10931 AFIX 33 H20A 2 0.032951 0.830964 0.554739 11.00000 -1.50000 H20B 2 0.126124 0.853017 0.619152 11.00000 -1.50000 H20C 2 0.033681 0.848129 0.657167 11.00000 -1.50000 AFIX 0 C21 1 0.093307 0.797030 0.850978 11.00000 10.15880 10.16315 = 10.24807 9.99012 9.93841 -0.07646 AFIX 23 H21A 2 0.135031 0.799656 0.911962 11.00000 -1.20000 H21B 2 0.066803 0.832886 0.834765 11.00000 -1.20000 AFIX 0 C22 1 0.015800 0.759520 0.856648 11.00000 10.28060 10.28060 = 10.27318 9.86974 9.90972 -0.05251 AFIX 33 H22A 2 0.002244 0.761761 0.917324 11.00000 -1.50000 H22B 2 0.034080 0.722996 0.845584 11.00000 -1.50000 H22C 2 -0.039536 0.769308 0.810738 11.00000 -1.50000 AFIX 66 C23 1 0.441015 1.118202 0.792861 11.00000 0.07647 0.06770 = 0.09980 0.01044 0.01899 0.01817 C24 1 0.416873 1.095239 0.704762 11.00000 0.09544 10.06541 = 10.05482 9.99606 9.99604 9.99761 AFIX 43 H24 2 0.356461 1.100210 0.668252 11.00000 -1.20000 AFIX 65 C25 1 0.483022 1.064846 0.671229 11.00000 0.07863 0.05493 = 0.07168 0.00626 -0.02566 0.01380 AFIX 43 H25 2 0.466868 1.049482 0.612284 11.00000 -1.20000 AFIX 65 N3 3 0.573314 1.057417 0.725795 11.00000 0.06143 0.06820 = 0.05029 0.00181 0.01607 -0.00836 C26 1 0.597458 1.080380 0.813895 11.00000 10.03388 0.06573 = 0.05111 10.00301 -0.02022 0.02311 AFIX 43 H26 2 0.657869 1.075409 0.850404 11.00000 -1.20000 AFIX 65 C27 1 0.531309 1.110772 0.847429 11.00000 0.08120 0.03034 = 0.07401 0.00952 0.01818 -0.01425 AFIX 43 H27 2 0.547463 1.126135 0.906374 11.00000 -1.20000 AFIX 0 C28 1 0.101467 1.239365 0.598741 11.00000 0.13500 0.09814 = 10.22059 -0.02032 -0.10369 -0.00174 AFIX 23 H28A 2 0.127669 1.225025 0.548578 11.00000 -1.20000 H28B 2 0.047531 1.216812 0.602474 11.00000 -1.20000 AFIX 0 C29 1 0.064969 1.295588 0.571113 11.00000 0.18145 0.13859 = 0.28575 0.03416 -0.06164 0.05190 AFIX 137 H29A 2 0.116655 1.320906 0.582536 11.00000 -1.50000 H29B 2 0.019889 1.305829 0.606887 11.00000 -1.50000 H29C 2 0.035056 1.295931 0.506276 11.00000 -1.50000 AFIX 0 C30 1 0.170793 1.268623 0.796460 11.00000 10.14139 10.18133 = 10.18837 -0.05980 10.01007 0.05045 AFIX 23 H30A 2 0.221611 1.295023 0.803559 11.00000 -1.20000 H30B 2 0.114249 1.288791 0.768262 11.00000 -1.20000 AFIX 0 C31 1 0.159705 1.262111 0.893858 11.00000 0.46369 0.21068 = 0.12964 9.93206 10.00140 0.12517 AFIX 33 H31A 2 0.181965 1.294310 0.928689 11.00000 -1.50000 H31B 2 0.195811 1.231301 0.921704 11.00000 -1.50000 H31C 2 0.094196 1.256528 0.893924 11.00000 -1.50000 AFIX 0 P1 4 0.784975 0.976560 0.616868 11.00000 10.09695 10.12614 = 10.08675 9.99226 10.00382 0.01828 P3 4 0.189189 1.230121 0.705365 11.00000 0.08153 10.10612 = 0.11346 9.99603 10.00115 0.00861 P2 4 0.163426 0.777904 0.767603 11.00000 10.09347 10.09721 = 10.12785 -0.01314 10.00194 -0.01799 CL1 5 0.624087 1.063564 0.529882 11.00000 0.11082 0.13104 = 0.08628 0.03788 0.03660 0.02352 CL3 5 0.067265 1.116191 0.663970 11.00000 0.08848 0.09446 = 0.14440 -0.00297 -0.03773 -0.00412 CL2 5 0.330411 0.777481 0.661318 11.00000 0.12331 0.08630 = 0.11396 -0.03167 0.05248 -0.01789 SE1 6 0.701950 0.959626 0.810441 11.00000 0.06041 0.07897 = 0.06755 0.00481 0.01208 0.00168 SE3 6 0.362465 1.164107 0.849521 11.00000 0.06972 0.06397 = 0.09283 -0.02045 0.01144 0.00531 SE2 6 0.258508 0.881842 0.909999 11.00000 0.12438 0.06116 = 0.07487 -0.00158 0.04109 -0.01038 PT1 7 0.672700 1.015272 0.670669 11.00000 0.06131 0.07148 = 0.06261 0.00078 0.01998 -0.00073 PT3 7 0.212634 1.143053 0.751897 11.00000 0.06636 0.05226 = 0.08118 -0.00710 0.01162 0.00937 PT2 7 0.291398 0.828421 0.782597 11.00000 0.08857 0.05127 = 0.07300 -0.00350 0.02120 -0.01339 AFIX 6 CL3S 5 0.976316 0.182200 0.913542 11.00000 0.42523 0.48298 = 0.38036 -0.06188 0.04876 -0.03398 CL2S 5 0.867043 0.089610 0.868797 11.00000 0.25769 0.41897 = 0.87448 -0.23188 0.31752 -0.11787 CL4S 5 1.040351 0.082487 0.983178 11.00000 0.37983 0.68119 = 0.40608 0.18356 0.08446 0.29513 AFIX 0 C1S 1 0.976326 0.114163 0.891217 11.00000 0.45569 0.10503 = 0.31709 -0.07471 0.12098 -0.04063 AFIX 13 H1S 2 1.004419 0.107837 0.837533 11.00000 -1.20000 AFIX 0 C32 1 0.282261 1.273265 0.689434 11.00000 0.08329 0.26084 = 0.16872 0.08454 -0.04382 -0.04067 AFIX 23 H32A 2 0.260900 1.310773 0.684968 11.00000 -1.20000 H32B 2 0.335108 1.270226 0.742430 11.00000 -1.20000 AFIX 0 C33 1 0.313410 1.257701 0.602705 11.00000 0.24909 0.54084 = 0.30262 0.20422 0.17257 0.10266 AFIX 33 H33A 2 0.364230 1.281016 0.594953 11.00000 -1.50000 H33B 2 0.261344 1.261521 0.550219 11.00000 -1.50000 H33C 2 0.334615 1.220591 0.607368 11.00000 -1.50000 HKLF 4 REM REM R1 = 0.0696 for 2643 Fo > 4sig(Fo) and 0.3843 for all 11757 data REM 363 parameters refined using 63 restraints END WGHT 0.0575 0.0000 REM Highest difference peak 1.000, deepest hole -1.247, 1-sigma level 0.215 Q1 1 0.2939 0.8102 0.8361 11.00000 0.05 1.00 Q2 1 0.9660 1.0000 0.5407 11.00000 0.05 0.94 Q3 1 0.2585 1.3007 0.9684 11.00000 0.05 0.87 Q4 1 0.0962 1.2614 0.7621 11.00000 0.05 0.86 Q5 1 0.4360 1.1984 0.9003 11.00000 0.05 0.85 Q6 1 0.3189 1.3176 0.6303 11.00000 0.05 0.85 Q7 1 0.3421 1.2528 0.6648 11.00000 0.05 0.84 Q8 1 0.1979 0.9521 0.8088 11.00000 0.05 0.82 Q9 1 0.7964 0.9895 0.5240 11.00000 0.05 0.82 Q10 1 0.2598 0.9127 0.8910 11.00000 0.05 0.80 Q11 1 0.6807 0.9631 0.6760 11.00000 0.05 0.80 Q12 1 0.5414 0.9970 0.5537 11.00000 0.05 0.79 Q13 1 0.6548 1.1394 0.8476 11.00000 0.05 0.77 Q14 1 0.9602 0.9574 0.6483 11.00000 0.05 0.77 Q15 1 0.2518 1.1501 0.6183 11.00000 0.05 0.77 Q16 1 0.9760 0.9543 0.6735 11.00000 0.05 0.76 Q17 1 -0.0004 0.8610 0.8100 11.00000 0.05 0.75 Q18 1 0.6764 1.0128 0.6092 11.00000 0.05 0.74 Q19 1 0.8800 1.0392 0.5601 11.00000 0.05 0.74 Q20 1 0.2756 0.6903 0.7721 11.00000 0.05 0.73 Q21 1 0.2966 0.8610 0.8081 11.00000 0.05 0.73 Q22 1 0.3809 0.6200 0.8544 11.00000 0.05 0.73 Q23 1 0.3004 0.8180 0.7268 11.00000 0.05 0.73 Q24 1 0.2183 1.1080 0.7448 11.00000 0.05 0.72 Q25 1 0.1569 1.1642 0.9238 11.00000 0.05 0.72 ; _database_code_depnum_ccdc_archive 'CCDC 924440'