# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Martin Smith' 'Mark Elsegood' 'Sean Durran' _publ_contact_author_name 'Martin Smith' _publ_contact_author_email m.b.smith@lboro.ac.uk _publ_section_title ; Flexible \^I4-PNN`O-tetradentate ligands: synthesis, complexation and structural studies ; # Attachment '- CIF (PNNO, MBSmith).CIF' # Manuscript submitted to: Dalton Trans. # Authors:Sean E. Durran, Mark R.J. Elsegood, Shelly # R Hammond, and Martin B. Smith. # Title: Flexible k4-PNN'O tetradentate ligands: # syhtesis, complexation ans structural studies. # Corresponding author for crystallography: # m.r.j.elsegood@lboro.ac.uk data_3a.HH _database_code_depnum_ccdc_archive 'CCDC 771445' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H23 N2 O2 P, C2 H6 O1' _chemical_formula_sum 'C29 H29 N2 O3 P' _chemical_formula_weight 484.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 11.0184(8) _cell_length_b 18.5035(13) _cell_length_c 12.7514(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.4002(13) _cell_angle_gamma 90.00 _cell_volume 2588.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7430 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.42 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.79 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.139 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.898 _exptl_absorpt_correction_T_max 0.992 _exptl_absorpt_process_details 'SADABS v2.03, Sheldrick, G.M., (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22131 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5901 _reflns_number_gt 4303 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0441P)^2^+1.6030P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except NH & OH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5901 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0694 _refine_ls_R_factor_gt 0.0442 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1003 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 P1 P 0.82305(4) 0.14465(3) 0.90581(4) 0.03134(13) Uani 1 1 d . . . C1 C 0.78405(16) 0.24061(10) 0.88286(14) 0.0306(4) Uani 1 1 d . . . C2 C 0.83848(18) 0.28368(11) 0.81027(16) 0.0399(5) Uani 1 1 d . . . H2B H 0.8964 0.2628 0.7686 0.048 Uiso 1 1 calc R . . C3 C 0.8095(2) 0.35618(12) 0.79807(16) 0.0434(5) Uani 1 1 d . . . H3A H 0.8473 0.3845 0.7482 0.052 Uiso 1 1 calc R . . C4 C 0.72553(19) 0.38760(11) 0.85836(15) 0.0389(5) Uani 1 1 d . . . H4 H 0.7061 0.4374 0.8503 0.047 Uiso 1 1 calc R . . C5 C 0.67021(17) 0.34616(10) 0.93020(14) 0.0318(4) Uani 1 1 d . . . H5 H 0.6125 0.3678 0.9713 0.038 Uiso 1 1 calc R . . C6 C 0.69790(15) 0.27295(9) 0.94328(13) 0.0277(4) Uani 1 1 d . . . C7 C 0.63525(15) 0.23022(9) 1.01984(14) 0.0285(4) Uani 1 1 d . . . H7 H 0.6384 0.1790 1.0163 0.034 Uiso 1 1 calc R . . N1 N 0.57805(15) 0.25902(8) 1.08938(12) 0.0349(4) Uani 1 1 d . . . C8 C 0.51670(19) 0.21109(9) 1.15825(15) 0.0351(4) Uani 1 1 d . . . H8A H 0.5765 0.1760 1.1911 0.042 Uiso 1 1 calc R . . H8B H 0.4528 0.1836 1.1154 0.042 Uiso 1 1 calc R . . C9 C 0.45898(16) 0.25136(9) 1.24381(14) 0.0277(4) Uani 1 1 d . . . O1 O 0.40142(12) 0.21855(7) 1.30677(10) 0.0369(3) Uani 1 1 d . . . N2 N 0.47700(14) 0.32266(8) 1.24457(12) 0.0296(3) Uani 1 1 d . . . H2 H 0.5206(19) 0.3378(11) 1.1953(16) 0.036 Uiso 1 1 d . . . C10 C 0.43496(16) 0.37584(9) 1.31157(13) 0.0276(4) Uani 1 1 d . . . C11 C 0.46961(17) 0.44658(10) 1.28893(15) 0.0322(4) Uani 1 1 d . . . O2 O 0.53851(15) 0.45386(8) 1.20672(12) 0.0470(4) Uani 1 1 d . . . H2A H 0.560(2) 0.4954(16) 1.197(2) 0.070 Uiso 1 1 d . . . C12 C 0.43228(19) 0.50333(10) 1.34884(16) 0.0390(5) Uani 1 1 d . . . H12 H 0.4553 0.5514 1.3337 0.047 Uiso 1 1 calc R . . C13 C 0.36123(18) 0.49011(11) 1.43103(16) 0.0400(5) Uani 1 1 d . . . H13 H 0.3356 0.5292 1.4719 0.048 Uiso 1 1 calc R . . C14 C 0.32777(18) 0.42068(11) 1.45356(15) 0.0380(4) Uani 1 1 d . . . H14 H 0.2794 0.4121 1.5102 0.046 Uiso 1 1 calc R . . C15 C 0.36421(17) 0.36279(10) 1.39402(14) 0.0319(4) Uani 1 1 d . . . H15 H 0.3409 0.3149 1.4097 0.038 Uiso 1 1 calc R . . C16 C 0.94268(17) 0.15183(10) 1.01548(14) 0.0324(4) Uani 1 1 d . . . C17 C 1.00480(19) 0.21526(11) 1.04500(16) 0.0404(5) Uani 1 1 d . . . H17 H 0.9842 0.2590 1.0085 0.048 Uiso 1 1 calc R . . C18 C 1.0965(2) 0.21511(13) 1.12726(18) 0.0485(5) Uani 1 1 d . . . H18 H 1.1374 0.2588 1.1475 0.058 Uiso 1 1 calc R . . C19 C 1.1285(2) 0.15183(14) 1.17992(17) 0.0492(6) Uani 1 1 d . . . H19 H 1.1922 0.1519 1.2355 0.059 Uiso 1 1 calc R . . C20 C 1.0679(2) 0.08835(13) 1.15180(17) 0.0460(5) Uani 1 1 d . . . H20 H 1.0900 0.0447 1.1879 0.055 Uiso 1 1 calc R . . C21 C 0.97472(18) 0.08853(11) 1.07079(15) 0.0379(4) Uani 1 1 d . . . H21 H 0.9321 0.0450 1.0527 0.045 Uiso 1 1 calc R . . C22 C 0.91155(16) 0.12081(10) 0.79604(14) 0.0316(4) Uani 1 1 d . . . C23 C 0.84891(18) 0.10947(12) 0.69731(16) 0.0436(5) Uani 1 1 d . . . H23 H 0.7642 0.1198 0.6866 0.052 Uiso 1 1 calc R . . C24 C 0.9089(2) 0.08328(13) 0.61479(17) 0.0472(5) Uani 1 1 d . . . H24 H 0.8656 0.0771 0.5474 0.057 Uiso 1 1 calc R . . C25 C 1.03105(18) 0.06603(12) 0.62951(16) 0.0408(5) Uani 1 1 d . . . H25 H 1.0712 0.0466 0.5731 0.049 Uiso 1 1 calc R . . C26 C 1.09436(17) 0.07715(12) 0.72627(16) 0.0395(5) Uani 1 1 d . . . H26 H 1.1787 0.0657 0.7366 0.047 Uiso 1 1 calc R . . C27 C 1.03531(17) 0.10512(11) 0.80900(15) 0.0352(4) Uani 1 1 d . . . H27 H 1.0802 0.1136 0.8752 0.042 Uiso 1 1 calc R . . C28 C 0.7091(4) 0.63259(19) 1.0018(2) 0.0916(11) Uani 1 1 d . . . H28A H 0.6557 0.6745 1.0070 0.110 Uiso 1 1 calc R . . H28B H 0.7197 0.6231 0.9276 0.110 Uiso 1 1 calc R . . H28C H 0.7886 0.6424 1.0402 0.110 Uiso 1 1 calc R . . C29 C 0.6562(3) 0.57166(15) 1.0459(2) 0.0773(9) Uani 1 1 d . . . H29A H 0.7139 0.5308 1.0434 0.093 Uiso 1 1 calc R . . H29B H 0.5818 0.5588 1.0000 0.093 Uiso 1 1 calc R . . O3 O 0.62376(15) 0.57751(8) 1.15096(12) 0.0466(4) Uani 1 1 d . . . H3 H 0.609(3) 0.6211(16) 1.165(2) 0.070 Uiso 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 P1 0.0287(2) 0.0325(3) 0.0344(3) -0.0012(2) 0.01106(19) 0.00372(19) C1 0.0267(9) 0.0352(10) 0.0307(9) 0.0010(8) 0.0066(7) 0.0025(7) C2 0.0364(10) 0.0482(12) 0.0375(11) 0.0060(9) 0.0154(8) 0.0051(9) C3 0.0482(12) 0.0465(12) 0.0374(11) 0.0141(9) 0.0136(9) -0.0009(10) C4 0.0463(12) 0.0345(10) 0.0357(10) 0.0084(8) 0.0028(9) 0.0029(9) C5 0.0328(9) 0.0337(10) 0.0293(9) 0.0025(8) 0.0043(7) 0.0045(8) C6 0.0258(9) 0.0309(9) 0.0266(9) 0.0002(7) 0.0033(7) 0.0015(7) C7 0.0277(9) 0.0257(9) 0.0327(9) 0.0001(7) 0.0064(7) 0.0028(7) N1 0.0466(9) 0.0261(8) 0.0346(8) 0.0005(6) 0.0176(7) 0.0009(7) C8 0.0479(11) 0.0224(9) 0.0378(10) -0.0009(7) 0.0190(9) -0.0012(8) C9 0.0296(9) 0.0240(8) 0.0303(9) 0.0018(7) 0.0075(7) 0.0006(7) O1 0.0457(8) 0.0257(6) 0.0426(8) 0.0028(6) 0.0217(6) -0.0032(6) N2 0.0372(9) 0.0225(7) 0.0315(8) 0.0006(6) 0.0157(7) -0.0012(6) C10 0.0293(9) 0.0252(9) 0.0284(9) -0.0024(7) 0.0031(7) 0.0033(7) C11 0.0353(10) 0.0275(9) 0.0337(10) -0.0001(7) 0.0030(8) 0.0006(7) O2 0.0693(10) 0.0244(7) 0.0514(9) -0.0008(6) 0.0276(8) -0.0091(7) C12 0.0461(11) 0.0263(9) 0.0434(11) -0.0051(8) -0.0011(9) 0.0046(8) C13 0.0412(11) 0.0383(11) 0.0397(11) -0.0140(9) -0.0006(9) 0.0120(9) C14 0.0331(10) 0.0489(12) 0.0326(10) -0.0074(9) 0.0065(8) 0.0079(9) C15 0.0318(9) 0.0335(10) 0.0311(9) -0.0007(7) 0.0065(7) 0.0031(8) C16 0.0338(9) 0.0363(10) 0.0290(9) -0.0010(8) 0.0132(7) 0.0064(8) C17 0.0442(11) 0.0369(11) 0.0405(11) -0.0004(9) 0.0060(9) 0.0035(9) C18 0.0447(12) 0.0548(14) 0.0459(12) -0.0075(10) 0.0035(10) -0.0030(10) C19 0.0396(11) 0.0715(16) 0.0365(11) 0.0009(11) 0.0044(9) 0.0089(11) C20 0.0463(12) 0.0548(14) 0.0385(11) 0.0104(10) 0.0122(9) 0.0155(10) C21 0.0409(11) 0.0389(11) 0.0362(10) 0.0026(8) 0.0151(9) 0.0074(9) C22 0.0294(9) 0.0329(9) 0.0334(10) -0.0030(8) 0.0078(7) 0.0023(7) C23 0.0279(10) 0.0611(14) 0.0413(11) -0.0107(10) 0.0012(8) 0.0092(9) C24 0.0420(12) 0.0656(15) 0.0330(11) -0.0131(10) -0.0011(9) 0.0048(10) C25 0.0383(11) 0.0490(12) 0.0368(11) -0.0113(9) 0.0117(9) 0.0020(9) C26 0.0266(9) 0.0529(12) 0.0401(11) -0.0073(9) 0.0093(8) 0.0051(9) C27 0.0288(9) 0.0464(11) 0.0309(10) -0.0033(8) 0.0055(7) 0.0026(8) C28 0.125(3) 0.093(2) 0.0647(18) 0.0105(17) 0.0545(19) 0.025(2) C29 0.108(2) 0.0517(16) 0.080(2) -0.0132(14) 0.0521(18) 0.0099(15) O3 0.0639(10) 0.0248(7) 0.0550(9) -0.0032(6) 0.0254(8) -0.0033(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 P1 C22 1.8334(18) . ? P1 C16 1.834(2) . ? P1 C1 1.8439(19) . ? C1 C2 1.398(3) . ? C1 C6 1.411(2) . ? C2 C3 1.384(3) . ? C3 C4 1.385(3) . ? C4 C5 1.380(3) . ? C5 C6 1.395(2) . ? C6 C7 1.477(2) . ? C7 N1 1.254(2) . ? N1 C8 1.458(2) . ? C8 C9 1.510(2) . ? C9 O1 1.229(2) . ? C9 N2 1.334(2) . ? N2 C10 1.410(2) . ? C10 C15 1.388(2) . ? C10 C11 1.401(2) . ? C11 O2 1.358(2) . ? C11 C12 1.384(3) . ? C12 C13 1.388(3) . ? C13 C14 1.374(3) . ? C14 C15 1.394(3) . ? C16 C17 1.393(3) . ? C16 C21 1.395(3) . ? C17 C18 1.386(3) . ? C18 C19 1.379(3) . ? C19 C20 1.382(3) . ? C20 C21 1.386(3) . ? C22 C27 1.389(3) . ? C22 C23 1.394(3) . ? C23 C24 1.382(3) . ? C24 C25 1.379(3) . ? C25 C26 1.375(3) . ? C26 C27 1.390(3) . ? C28 C29 1.410(4) . ? C29 O3 1.423(3) . ? 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 C22 P1 C16 101.76(8) . . ? C22 P1 C1 104.08(8) . . ? C16 P1 C1 101.03(8) . . ? C2 C1 C6 118.18(17) . . ? C2 C1 P1 123.08(14) . . ? C6 C1 P1 118.72(13) . . ? C3 C2 C1 121.18(18) . . ? C2 C3 C4 120.23(18) . . ? C5 C4 C3 119.67(18) . . ? C4 C5 C6 120.91(17) . . ? C5 C6 C1 119.83(16) . . ? C5 C6 C7 119.22(15) . . ? C1 C6 C7 120.95(16) . . ? N1 C7 C6 122.49(16) . . ? C7 N1 C8 117.37(15) . . ? N1 C8 C9 112.68(14) . . ? O1 C9 N2 124.70(16) . . ? O1 C9 C8 120.42(15) . . ? N2 C9 C8 114.88(15) . . ? C9 N2 C10 129.61(15) . . ? C15 C10 C11 120.14(16) . . ? C15 C10 N2 125.29(16) . . ? C11 C10 N2 114.57(15) . . ? O2 C11 C12 124.61(17) . . ? O2 C11 C10 115.76(16) . . ? C12 C11 C10 119.62(17) . . ? C11 C12 C13 120.10(19) . . ? C14 C13 C12 120.27(18) . . ? C13 C14 C15 120.52(18) . . ? C10 C15 C14 119.35(18) . . ? C17 C16 C21 118.45(18) . . ? C17 C16 P1 124.53(15) . . ? C21 C16 P1 117.01(15) . . ? C18 C17 C16 120.5(2) . . ? C19 C18 C17 120.3(2) . . ? C18 C19 C20 120.0(2) . . ? C19 C20 C21 119.8(2) . . ? C20 C21 C16 120.9(2) . . ? C27 C22 C23 118.24(17) . . ? C27 C22 P1 123.11(14) . . ? C23 C22 P1 118.18(14) . . ? C24 C23 C22 120.59(18) . . ? C25 C24 C23 120.56(19) . . ? C26 C25 C24 119.60(18) . . ? C25 C26 C27 120.17(18) . . ? C22 C27 C26 120.79(18) . . ? C28 C29 O3 117.7(2) . . ? 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 C22 P1 C1 C2 -12.68(19) . . . . ? C16 P1 C1 C2 92.56(17) . . . . ? C22 P1 C1 C6 169.21(14) . . . . ? C16 P1 C1 C6 -85.55(15) . . . . ? C6 C1 C2 C3 0.3(3) . . . . ? P1 C1 C2 C3 -177.78(16) . . . . ? C1 C2 C3 C4 0.2(3) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C3 C4 C5 C6 0.2(3) . . . . ? C4 C5 C6 C1 0.3(3) . . . . ? C4 C5 C6 C7 -179.05(17) . . . . ? C2 C1 C6 C5 -0.6(3) . . . . ? P1 C1 C6 C5 177.61(14) . . . . ? C2 C1 C6 C7 178.79(17) . . . . ? P1 C1 C6 C7 -3.0(2) . . . . ? C5 C6 C7 N1 -15.6(3) . . . . ? C1 C6 C7 N1 165.04(18) . . . . ? C6 C7 N1 C8 178.09(17) . . . . ? C7 N1 C8 C9 175.69(17) . . . . ? N1 C8 C9 O1 178.34(17) . . . . ? N1 C8 C9 N2 -2.2(2) . . . . ? O1 C9 N2 C10 -1.7(3) . . . . ? C8 C9 N2 C10 178.86(17) . . . . ? C9 N2 C10 C15 0.7(3) . . . . ? C9 N2 C10 C11 -178.96(18) . . . . ? C15 C10 C11 O2 -179.86(17) . . . . ? N2 C10 C11 O2 -0.2(2) . . . . ? C15 C10 C11 C12 -0.4(3) . . . . ? N2 C10 C11 C12 179.24(17) . . . . ? O2 C11 C12 C13 179.61(18) . . . . ? C10 C11 C12 C13 0.2(3) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C11 C10 C15 C14 0.3(3) . . . . ? N2 C10 C15 C14 -179.33(17) . . . . ? C13 C14 C15 C10 0.1(3) . . . . ? C22 P1 C16 C17 90.74(17) . . . . ? C1 P1 C16 C17 -16.34(18) . . . . ? C22 P1 C16 C21 -87.63(15) . . . . ? C1 P1 C16 C21 165.29(14) . . . . ? C21 C16 C17 C18 0.2(3) . . . . ? P1 C16 C17 C18 -178.16(15) . . . . ? C16 C17 C18 C19 1.0(3) . . . . ? C17 C18 C19 C20 -1.0(3) . . . . ? C18 C19 C20 C21 -0.2(3) . . . . ? C19 C20 C21 C16 1.3(3) . . . . ? C17 C16 C21 C20 -1.3(3) . . . . ? P1 C16 C21 C20 177.15(14) . . . . ? C16 P1 C22 C27 6.90(19) . . . . ? C1 P1 C22 C27 111.59(17) . . . . ? C16 P1 C22 C23 178.93(16) . . . . ? C1 P1 C22 C23 -76.38(18) . . . . ? C27 C22 C23 C24 0.0(3) . . . . ? P1 C22 C23 C24 -172.43(18) . . . . ? C22 C23 C24 C25 1.8(4) . . . . ? C23 C24 C25 C26 -2.0(4) . . . . ? C24 C25 C26 C27 0.5(3) . . . . ? C23 C22 C27 C26 -1.6(3) . . . . ? P1 C22 C27 C26 170.47(16) . . . . ? C25 C26 C27 C22 1.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 N1 0.87(2) 2.12(2) 2.638(2) 117.0(17) . O2 H2A O3 0.82(3) 1.79(3) 2.598(2) 167(3) . O3 H3 O1 0.85(3) 1.84(3) 2.6846(19) 172(3) 2_657 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.611 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.045 #===END data_3c.HH _database_code_depnum_ccdc_archive 'CCDC 771446' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H23 N2 O2 P, 0.5(C1 H1 Cl3)' _chemical_formula_sum 'C27.50 H23.50 Cl1.50 N2 O2 P' _chemical_formula_weight 498.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.7587(11) _cell_length_b 8.3781(5) _cell_length_c 17.3155(10) _cell_angle_alpha 90.00 _cell_angle_beta 114.6476(9) _cell_angle_gamma 90.00 _cell_volume 2473.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7577 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.21 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 0.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details 'SADABS, v.2.08, Sheldrick, G.M., (2003).' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20748 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0276 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5646 _reflns_number_gt 4273 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+1.8776P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except H2, H2A coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5646 _refine_ls_number_parameters 336 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0428 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1010 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.039 _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 P1 P 0.23613(3) 0.28025(6) 0.14728(3) 0.02499(12) Uani 1 1 d . . . C1 C 0.25368(11) 0.1561(2) 0.24122(11) 0.0257(4) Uani 1 1 d . . . C2 C 0.29038(12) 0.0075(2) 0.25250(12) 0.0323(4) Uani 1 1 d . . . H2B H 0.3076 -0.0294 0.2112 0.039 Uiso 1 1 calc R . . C3 C 0.30248(14) -0.0881(3) 0.32251(14) 0.0397(5) Uani 1 1 d . . . H3 H 0.3279 -0.1883 0.3287 0.048 Uiso 1 1 calc R . . C4 C 0.27740(14) -0.0371(3) 0.38351(14) 0.0411(5) Uani 1 1 d . . . H4 H 0.2861 -0.1014 0.4318 0.049 Uiso 1 1 calc R . . C5 C 0.23986(12) 0.1079(2) 0.37303(12) 0.0332(4) Uani 1 1 d . . . H5 H 0.2219 0.1420 0.4141 0.040 Uiso 1 1 calc R . . C6 C 0.22754(11) 0.2062(2) 0.30309(11) 0.0265(4) Uani 1 1 d . . . C7 C 0.18706(10) 0.3572(2) 0.29841(11) 0.0271(4) Uani 1 1 d . . . H7 H 0.1623 0.3736 0.3358 0.033 Uiso 1 1 calc R . . N1 N 0.18346(9) 0.46728(19) 0.24681(9) 0.0270(3) Uani 1 1 d . . . C8 C 0.13931(12) 0.6094(2) 0.24748(11) 0.0300(4) Uani 1 1 d . . . H8A H 0.1760 0.6902 0.2849 0.036 Uiso 1 1 calc R . . H8B H 0.1017 0.5819 0.2720 0.036 Uiso 1 1 calc R . . C9 C 0.09448(11) 0.6822(2) 0.16031(11) 0.0266(4) Uani 1 1 d . . . O1 O 0.05531(9) 0.80406(17) 0.15355(9) 0.0373(3) Uani 1 1 d . . . N2 N 0.10198(9) 0.6073(2) 0.09568(9) 0.0253(3) Uani 1 1 d . . . H2 H 0.1289(12) 0.523(3) 0.1100(12) 0.022(5) Uiso 1 1 d . . . C10 C 0.06825(10) 0.6476(2) 0.00789(11) 0.0235(4) Uani 1 1 d . . . C11 C 0.01690(11) 0.7749(2) -0.02622(12) 0.0292(4) Uani 1 1 d . . . H11 H 0.0023 0.8404 0.0096 0.035 Uiso 1 1 calc R . . C12 C -0.01296(11) 0.8058(2) -0.11287(12) 0.0312(4) Uani 1 1 d . . . H12 H -0.0479 0.8928 -0.1361 0.037 Uiso 1 1 calc R . . C13 C 0.00787(11) 0.7107(2) -0.16577(11) 0.0271(4) Uani 1 1 d . . . O2 O -0.02476(9) 0.74674(19) -0.25079(9) 0.0352(3) Uani 1 1 d . . . H2A H 0.0016(16) 0.707(3) -0.2738(17) 0.051(8) Uiso 1 1 d . . . C14 C 0.05868(11) 0.5832(2) -0.13239(11) 0.0273(4) Uani 1 1 d . . . H14 H 0.0730 0.5177 -0.1684 0.033 Uiso 1 1 calc R . . C15 C 0.08843(11) 0.5520(2) -0.04577(11) 0.0264(4) Uani 1 1 d . . . H15 H 0.1230 0.4644 -0.0228 0.032 Uiso 1 1 calc R . . C16 C 0.31839(11) 0.4215(2) 0.18858(11) 0.0261(4) Uani 1 1 d . . . C17 C 0.38568(12) 0.3976(3) 0.26318(13) 0.0371(5) Uani 1 1 d . . . H17 H 0.3910 0.3032 0.2956 0.045 Uiso 1 1 calc R . . C18 C 0.44480(14) 0.5108(3) 0.29027(15) 0.0466(6) Uani 1 1 d . . . H18 H 0.4902 0.4936 0.3415 0.056 Uiso 1 1 calc R . . C19 C 0.43884(14) 0.6483(3) 0.24413(15) 0.0441(5) Uani 1 1 d . . . H19 H 0.4800 0.7247 0.2631 0.053 Uiso 1 1 calc R . . C20 C 0.37241(14) 0.6736(3) 0.17005(15) 0.0394(5) Uani 1 1 d . . . H20 H 0.3678 0.7678 0.1378 0.047 Uiso 1 1 calc R . . C21 C 0.31271(12) 0.5620(2) 0.14289(13) 0.0318(4) Uani 1 1 d . . . H21 H 0.2670 0.5812 0.0923 0.038 Uiso 1 1 calc R . . C22 C 0.26623(11) 0.1444(2) 0.08316(11) 0.0266(4) Uani 1 1 d . . . C23 C 0.21311(12) 0.0239(2) 0.03867(12) 0.0339(4) Uani 1 1 d . . . H23 H 0.1659 0.0117 0.0460 0.041 Uiso 1 1 calc R . . C24 C 0.22838(14) -0.0779(3) -0.01587(12) 0.0388(5) Uani 1 1 d . . . H24 H 0.1929 -0.1616 -0.0440 0.047 Uiso 1 1 calc R . . C25 C 0.29545(14) -0.0567(3) -0.02894(13) 0.0398(5) Uani 1 1 d . . . H25 H 0.3053 -0.1244 -0.0674 0.048 Uiso 1 1 calc R . . C26 C 0.34824(13) 0.0620(2) 0.01331(13) 0.0364(5) Uani 1 1 d . . . H26 H 0.3941 0.0762 0.0037 0.044 Uiso 1 1 calc R . . C27 C 0.33435(12) 0.1612(2) 0.07014(12) 0.0304(4) Uani 1 1 d . . . H27 H 0.3716 0.2410 0.1003 0.036 Uiso 1 1 calc R . . C28 C 0.4741(3) 0.4323(7) -0.0245(3) 0.0598(14) Uani 0.50 1 d PDU . . H28 H 0.4210(7) 0.4116(18) -0.0614(9) 0.072 Uiso 0.50 1 d PD . . Cl1 Cl 0.52430(8) 0.2534(2) -0.01151(10) 0.0685(4) Uani 0.50 1 d PDU . . Cl2 Cl 0.4751(2) 0.5021(4) 0.0706(2) 0.0852(9) Uani 0.50 1 d PDU . . Cl3 Cl 0.5088(2) 0.5738(4) -0.0730(3) 0.1214(14) Uani 0.50 1 d PDU . . 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 P1 0.0263(2) 0.0270(2) 0.0215(2) 0.00127(18) 0.00982(18) 0.00132(19) C1 0.0265(9) 0.0274(9) 0.0234(9) 0.0014(7) 0.0104(7) -0.0020(7) C2 0.0393(11) 0.0312(10) 0.0293(10) 0.0033(8) 0.0173(9) 0.0034(8) C3 0.0515(13) 0.0294(11) 0.0409(12) 0.0091(9) 0.0219(10) 0.0057(10) C4 0.0561(14) 0.0355(12) 0.0335(11) 0.0096(9) 0.0204(10) -0.0025(10) C5 0.0409(11) 0.0358(11) 0.0271(9) -0.0021(8) 0.0181(9) -0.0076(9) C6 0.0258(9) 0.0284(10) 0.0242(9) -0.0012(7) 0.0094(7) -0.0051(7) C7 0.0252(9) 0.0338(10) 0.0228(9) -0.0058(8) 0.0104(7) -0.0041(8) N1 0.0261(8) 0.0317(8) 0.0224(7) -0.0018(6) 0.0093(6) 0.0026(6) C8 0.0338(10) 0.0339(10) 0.0218(9) -0.0029(8) 0.0112(8) 0.0056(8) C9 0.0291(9) 0.0277(10) 0.0248(9) -0.0018(7) 0.0131(8) 0.0010(7) O1 0.0557(9) 0.0312(8) 0.0300(7) 0.0017(6) 0.0230(7) 0.0138(7) N2 0.0286(8) 0.0261(8) 0.0221(7) 0.0011(6) 0.0115(6) 0.0054(7) C10 0.0251(9) 0.0249(9) 0.0221(8) 0.0000(7) 0.0114(7) -0.0015(7) C11 0.0346(10) 0.0285(10) 0.0276(9) 0.0005(8) 0.0159(8) 0.0037(8) C12 0.0314(10) 0.0298(10) 0.0308(10) 0.0065(8) 0.0115(8) 0.0043(8) C13 0.0269(9) 0.0316(10) 0.0230(9) 0.0020(7) 0.0105(7) -0.0079(8) O2 0.0353(8) 0.0464(9) 0.0240(7) 0.0075(6) 0.0126(6) -0.0031(7) C14 0.0296(9) 0.0307(10) 0.0247(9) -0.0044(7) 0.0142(8) -0.0033(8) C15 0.0279(9) 0.0263(9) 0.0261(9) 0.0002(7) 0.0124(8) 0.0013(7) C16 0.0299(9) 0.0263(9) 0.0256(9) -0.0029(7) 0.0151(8) 0.0004(7) C17 0.0353(11) 0.0362(11) 0.0334(11) 0.0043(9) 0.0080(9) -0.0033(9) C18 0.0377(12) 0.0522(14) 0.0384(12) -0.0039(10) 0.0045(10) -0.0092(11) C19 0.0447(13) 0.0392(12) 0.0514(13) -0.0112(10) 0.0230(11) -0.0156(10) C20 0.0499(13) 0.0285(11) 0.0479(13) 0.0001(9) 0.0284(11) -0.0031(9) C21 0.0355(10) 0.0302(10) 0.0318(10) 0.0016(8) 0.0162(8) 0.0013(8) C22 0.0332(10) 0.0252(9) 0.0198(8) 0.0011(7) 0.0096(7) 0.0006(8) C23 0.0370(11) 0.0362(11) 0.0261(9) -0.0016(8) 0.0109(8) -0.0058(9) C24 0.0536(13) 0.0299(11) 0.0259(10) -0.0040(8) 0.0097(9) -0.0053(9) C25 0.0604(14) 0.0311(11) 0.0268(10) -0.0020(8) 0.0172(10) 0.0084(10) C26 0.0431(12) 0.0363(11) 0.0335(11) 0.0005(9) 0.0196(9) 0.0066(9) C27 0.0327(10) 0.0292(10) 0.0288(9) -0.0010(8) 0.0125(8) -0.0001(8) C28 0.043(3) 0.085(4) 0.053(3) 0.014(3) 0.020(2) -0.005(3) Cl1 0.0474(7) 0.0789(10) 0.0726(9) -0.0168(8) 0.0187(7) -0.0016(7) Cl2 0.0844(15) 0.117(2) 0.0737(13) -0.0100(15) 0.0521(12) -0.0026(15) Cl3 0.112(3) 0.148(3) 0.128(2) 0.046(3) 0.0739(19) -0.032(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 P1 C22 1.8359(19) . ? P1 C16 1.8363(19) . ? P1 C1 1.8412(18) . ? C1 C2 1.396(3) . ? C1 C6 1.415(3) . ? C2 C3 1.390(3) . ? C3 C4 1.391(3) . ? C4 C5 1.377(3) . ? C5 C6 1.402(3) . ? C6 C7 1.461(3) . ? C7 N1 1.266(2) . ? N1 C8 1.453(2) . ? C8 C9 1.516(3) . ? C9 O1 1.234(2) . ? C9 N2 1.341(2) . ? N2 C10 1.422(2) . ? C10 C11 1.393(3) . ? C10 C15 1.393(2) . ? C11 C12 1.390(3) . ? C12 C13 1.387(3) . ? C13 O2 1.372(2) . ? C13 C14 1.387(3) . ? C14 C15 1.390(2) . ? C16 C17 1.394(3) . ? C16 C21 1.398(3) . ? C17 C18 1.384(3) . ? C18 C19 1.379(3) . ? C19 C20 1.382(3) . ? C20 C21 1.382(3) . ? C22 C27 1.394(3) . ? C22 C23 1.402(3) . ? C23 C24 1.388(3) . ? C24 C25 1.380(3) . ? C25 C26 1.378(3) . ? C26 C27 1.393(3) . ? C28 Cl3 1.729(6) . ? C28 Cl1 1.734(6) . ? C28 Cl2 1.741(7) . ? 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 C22 P1 C16 102.39(8) . . ? C22 P1 C1 101.37(8) . . ? C16 P1 C1 102.03(8) . . ? C2 C1 C6 117.70(17) . . ? C2 C1 P1 121.57(14) . . ? C6 C1 P1 120.69(14) . . ? C3 C2 C1 121.80(19) . . ? C2 C3 C4 120.1(2) . . ? C5 C4 C3 119.15(19) . . ? C4 C5 C6 121.52(19) . . ? C5 C6 C1 119.71(18) . . ? C5 C6 C7 116.84(17) . . ? C1 C6 C7 123.45(17) . . ? N1 C7 C6 122.94(17) . . ? C7 N1 C8 117.01(16) . . ? N1 C8 C9 113.77(15) . . ? O1 C9 N2 125.00(17) . . ? O1 C9 C8 119.21(16) . . ? N2 C9 C8 115.78(16) . . ? C9 N2 C10 128.79(16) . . ? C11 C10 C15 119.30(16) . . ? C11 C10 N2 123.75(16) . . ? C15 C10 N2 116.95(16) . . ? C12 C11 C10 119.78(17) . . ? C13 C12 C11 120.54(18) . . ? O2 C13 C14 122.55(17) . . ? O2 C13 C12 117.38(18) . . ? C14 C13 C12 120.06(17) . . ? C13 C14 C15 119.42(17) . . ? C14 C15 C10 120.90(17) . . ? C17 C16 C21 118.13(18) . . ? C17 C16 P1 123.89(15) . . ? C21 C16 P1 117.97(14) . . ? C18 C17 C16 120.2(2) . . ? C19 C18 C17 121.1(2) . . ? C18 C19 C20 119.3(2) . . ? C21 C20 C19 120.1(2) . . ? C20 C21 C16 121.17(19) . . ? C27 C22 C23 118.26(18) . . ? C27 C22 P1 124.67(14) . . ? C23 C22 P1 116.83(15) . . ? C24 C23 C22 121.0(2) . . ? C25 C24 C23 119.6(2) . . ? C26 C25 C24 120.55(19) . . ? C25 C26 C27 120.0(2) . . ? C26 C27 C22 120.52(19) . . ? Cl3 C28 Cl1 111.3(3) . . ? Cl3 C28 Cl2 111.8(4) . . ? Cl1 C28 Cl2 112.1(3) . . ? 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 C22 P1 C1 C2 6.79(18) . . . . ? C16 P1 C1 C2 -98.67(17) . . . . ? C22 P1 C1 C6 -170.82(15) . . . . ? C16 P1 C1 C6 83.71(16) . . . . ? C6 C1 C2 C3 -1.1(3) . . . . ? P1 C1 C2 C3 -178.80(17) . . . . ? C1 C2 C3 C4 0.4(3) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 C6 -1.1(3) . . . . ? C4 C5 C6 C1 0.3(3) . . . . ? C4 C5 C6 C7 179.97(19) . . . . ? C2 C1 C6 C5 0.7(3) . . . . ? P1 C1 C6 C5 178.44(14) . . . . ? C2 C1 C6 C7 -178.86(17) . . . . ? P1 C1 C6 C7 -1.2(2) . . . . ? C5 C6 C7 N1 168.27(18) . . . . ? C1 C6 C7 N1 -12.1(3) . . . . ? C6 C7 N1 C8 178.29(16) . . . . ? C7 N1 C8 C9 -143.65(17) . . . . ? N1 C8 C9 O1 -179.58(17) . . . . ? N1 C8 C9 N2 -0.4(2) . . . . ? O1 C9 N2 C10 -0.1(3) . . . . ? C8 C9 N2 C10 -179.25(17) . . . . ? C9 N2 C10 C11 -2.8(3) . . . . ? C9 N2 C10 C15 177.43(18) . . . . ? C15 C10 C11 C12 -0.5(3) . . . . ? N2 C10 C11 C12 179.70(17) . . . . ? C10 C11 C12 C13 0.1(3) . . . . ? C11 C12 C13 O2 179.03(17) . . . . ? C11 C12 C13 C14 0.2(3) . . . . ? O2 C13 C14 C15 -178.84(17) . . . . ? C12 C13 C14 C15 -0.1(3) . . . . ? C13 C14 C15 C10 -0.4(3) . . . . ? C11 C10 C15 C14 0.7(3) . . . . ? N2 C10 C15 C14 -179.55(16) . . . . ? C22 P1 C16 C17 -87.43(18) . . . . ? C1 P1 C16 C17 17.24(19) . . . . ? C22 P1 C16 C21 93.28(15) . . . . ? C1 P1 C16 C21 -162.05(14) . . . . ? C21 C16 C17 C18 -0.2(3) . . . . ? P1 C16 C17 C18 -179.46(17) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C17 C18 C19 C20 0.5(4) . . . . ? C18 C19 C20 C21 0.1(3) . . . . ? C19 C20 C21 C16 -0.8(3) . . . . ? C17 C16 C21 C20 0.8(3) . . . . ? P1 C16 C21 C20 -179.86(15) . . . . ? C16 P1 C22 C27 -2.85(18) . . . . ? C1 P1 C22 C27 -108.03(17) . . . . ? C16 P1 C22 C23 -177.12(14) . . . . ? C1 P1 C22 C23 77.70(16) . . . . ? C27 C22 C23 C24 1.1(3) . . . . ? P1 C22 C23 C24 175.70(15) . . . . ? C22 C23 C24 C25 -2.4(3) . . . . ? C23 C24 C25 C26 1.6(3) . . . . ? C24 C25 C26 C27 0.4(3) . . . . ? C25 C26 C27 C22 -1.7(3) . . . . ? C23 C22 C27 C26 1.0(3) . . . . ? P1 C22 C27 C26 -173.21(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 N1 0.84(2) 2.20(2) 2.688(2) 116.6(16) . O2 H2A O1 0.82(3) 1.91(3) 2.694(2) 158(3) 4_575 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.636 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.052 #===END data_4a _database_code_depnum_ccdc_archive 'CCDC 771447' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H23 Au Cl N2 O2 P' _chemical_formula_sum 'C27 H23 Au Cl N2 O2 P' _chemical_formula_weight 670.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.3440(6) _cell_length_b 16.0841(13) _cell_length_c 21.1068(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2493.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10253 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 6.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.322 _exptl_absorpt_correction_T_max 0.461 _exptl_absorpt_process_details 'SADABS, V2.08, Sheldrick, G.M.,(2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21675 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0364 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.97 _reflns_number_total 5974 _reflns_number_gt 5330 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0203P)^2^+2.0076P] 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, 2501 Friedel pairs' _refine_ls_abs_structure_Flack 0.555(6) _chemical_absolute_configuration ad _refine_ls_number_reflns 5974 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 Au1 Au 0.87894(2) 0.780739(11) 0.185436(9) 0.03782(6) Uani 1 1 d . . . Cl1 Cl 0.7003(2) 0.89543(10) 0.19427(11) 0.0930(7) Uani 1 1 d . . . P1 P 1.05500(13) 0.66840(6) 0.17742(5) 0.0236(2) Uani 1 1 d . . . C1 C 1.2187(6) 0.6538(3) 0.24183(19) 0.0254(9) Uani 1 1 d . . . C2 C 1.3840(7) 0.6162(3) 0.22658(19) 0.0333(9) Uani 1 1 d . . . H2B H 1.4011 0.5948 0.1851 0.040 Uiso 1 1 calc R . . C3 C 1.5231(6) 0.6093(3) 0.2699(2) 0.0311(10) Uani 1 1 d . . . H3 H 1.6338 0.5825 0.2587 0.037 Uiso 1 1 calc R . . C4 C 1.4998(6) 0.6417(3) 0.32992(19) 0.0271(9) Uani 1 1 d . . . H4 H 1.5971 0.6397 0.3596 0.033 Uiso 1 1 calc R . . C5 C 1.3359(5) 0.6771(3) 0.34703(18) 0.0263(9) Uani 1 1 d . . . H5 H 1.3200 0.6976 0.3889 0.032 Uiso 1 1 calc R . . C6 C 1.1923(5) 0.6830(2) 0.30332(18) 0.0234(8) Uani 1 1 d . . . C7 C 1.0180(5) 0.7189(3) 0.32681(18) 0.0268(8) Uani 1 1 d . . . H7 H 0.9074 0.7076 0.3051 0.032 Uiso 1 1 calc R . . N1 N 1.0173(5) 0.7640(3) 0.37502(18) 0.0345(9) Uani 1 1 d . . . C8 C 0.8482(5) 0.7984(3) 0.3996(2) 0.0318(10) Uani 1 1 d . . . H8A H 0.7685 0.7527 0.4142 0.038 Uiso 1 1 calc R . . H8B H 0.7840 0.8286 0.3653 0.038 Uiso 1 1 calc R . . C9 C 0.8851(6) 0.8574(2) 0.45421(18) 0.0250(8) Uani 1 1 d . . . O1 O 0.7601(4) 0.8887(2) 0.48380(16) 0.0387(8) Uani 1 1 d . . . N2 N 1.0633(4) 0.8690(2) 0.46679(16) 0.0246(8) Uani 1 1 d . . . H2 H 1.1390 0.8415 0.4422 0.030 Uiso 1 1 calc R . . C10 C 1.1458(5) 0.9187(2) 0.51345(17) 0.0223(8) Uani 1 1 d . . . C11 C 1.0572(6) 0.9804(3) 0.5484(2) 0.0285(9) Uani 1 1 d . . . H11 H 0.9314 0.9908 0.5417 0.034 Uiso 1 1 calc R . . C12 C 1.1521(6) 1.0265(3) 0.5929(2) 0.0331(10) Uani 1 1 d . . . H12 H 1.0917 1.0690 0.6160 0.040 Uiso 1 1 calc R . . C13 C 1.3368(6) 1.0107(3) 0.6037(2) 0.0331(10) Uani 1 1 d . . . H13 H 1.4016 1.0417 0.6347 0.040 Uiso 1 1 calc R . . C14 C 1.4246(5) 0.9497(3) 0.5692(2) 0.0290(9) Uani 1 1 d . . . H14 H 1.5498 0.9387 0.5767 0.035 Uiso 1 1 calc R . . C15 C 1.3324(5) 0.9049(2) 0.52407(18) 0.0220(8) Uani 1 1 d . . . O2 O 1.4112(4) 0.84432(18) 0.48763(13) 0.0298(6) Uani 1 1 d . . . H2A H 1.5216 0.8397 0.4974 0.045 Uiso 1 1 calc R . . C16 C 1.2016(6) 0.6728(3) 0.10778(19) 0.0265(9) Uani 1 1 d . . . C17 C 1.2069(6) 0.6093(3) 0.0635(2) 0.0323(10) Uani 1 1 d . . . H17 H 1.1297 0.5622 0.0675 0.039 Uiso 1 1 calc R . . C18 C 1.3280(6) 0.6161(3) 0.0128(2) 0.0425(12) Uani 1 1 d . . . H18 H 1.3327 0.5730 -0.0180 0.051 Uiso 1 1 calc R . . C19 C 1.4401(7) 0.6837(4) 0.0065(2) 0.0472(13) Uani 1 1 d . . . H19 H 1.5218 0.6871 -0.0282 0.057 Uiso 1 1 calc R . . C20 C 1.4345(7) 0.7465(3) 0.0504(3) 0.0508(14) Uani 1 1 d . . . H20 H 1.5125 0.7933 0.0462 0.061 Uiso 1 1 calc R . . C21 C 1.3138(7) 0.7412(3) 0.1012(2) 0.0418(12) Uani 1 1 d . . . H21 H 1.3086 0.7849 0.1314 0.050 Uiso 1 1 calc R . . C22 C 0.9227(5) 0.5736(3) 0.17114(18) 0.0251(9) Uani 1 1 d . . . C23 C 0.9564(6) 0.5052(3) 0.2102(2) 0.0314(10) Uani 1 1 d . . . H23 H 1.0558 0.5062 0.2390 0.038 Uiso 1 1 calc R . . C24 C 0.8449(7) 0.4360(3) 0.2068(2) 0.0383(11) Uani 1 1 d . . . H24 H 0.8672 0.3898 0.2338 0.046 Uiso 1 1 calc R . . C25 C 0.7005(7) 0.4336(3) 0.1643(2) 0.0387(11) Uani 1 1 d . . . H25 H 0.6240 0.3860 0.1623 0.046 Uiso 1 1 calc R . . C26 C 0.6688(6) 0.5007(3) 0.1248(2) 0.0357(11) Uani 1 1 d . . . H26 H 0.5717 0.4987 0.0951 0.043 Uiso 1 1 calc R . . C27 C 0.7779(6) 0.5710(3) 0.1283(2) 0.0297(9) Uani 1 1 d . . . H27 H 0.7541 0.6172 0.1015 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Au1 0.03378(8) 0.03450(8) 0.04517(9) -0.01384(8) -0.01585(8) 0.01380(8) Cl1 0.0684(10) 0.0602(9) 0.1505(18) -0.0572(11) -0.0662(12) 0.0440(8) P1 0.0225(4) 0.0265(5) 0.0219(5) -0.0031(4) -0.0028(4) 0.0051(4) C1 0.025(2) 0.027(2) 0.024(2) -0.0011(17) -0.0011(16) 0.0042(17) C2 0.031(2) 0.044(2) 0.0249(19) -0.0068(17) 0.000(2) 0.011(2) C3 0.022(2) 0.039(3) 0.033(2) -0.003(2) 0.0010(18) 0.0130(18) C4 0.0230(19) 0.032(2) 0.026(2) 0.0022(17) -0.0064(16) 0.0000(17) C5 0.026(2) 0.031(2) 0.0226(19) -0.0032(16) -0.0029(16) 0.0000(17) C6 0.0219(18) 0.0227(18) 0.026(2) -0.0021(16) -0.0022(15) -0.0002(14) C7 0.0210(17) 0.032(2) 0.027(2) 0.002(2) -0.0003(14) 0.0005(18) N1 0.0202(17) 0.048(3) 0.035(2) -0.0171(18) 0.0027(15) 0.0011(16) C8 0.019(2) 0.040(3) 0.036(2) -0.0119(18) 0.0015(17) 0.0006(17) C9 0.0168(18) 0.030(2) 0.0277(19) -0.0001(16) 0.0017(18) 0.0004(18) O1 0.0142(15) 0.053(2) 0.049(2) -0.0212(16) 0.0055(13) 0.0002(14) N2 0.0132(15) 0.036(2) 0.0241(17) -0.0085(15) 0.0015(12) 0.0014(13) C10 0.019(2) 0.0265(19) 0.0216(18) 0.0001(14) 0.0024(16) -0.0019(16) C11 0.024(2) 0.030(2) 0.032(2) 0.0019(18) 0.0088(17) 0.0040(16) C12 0.038(3) 0.024(2) 0.037(2) -0.0072(17) 0.011(2) -0.0022(19) C13 0.036(3) 0.033(2) 0.030(2) -0.0068(18) 0.0040(19) -0.0094(19) C14 0.020(2) 0.033(2) 0.033(2) 0.0037(18) -0.0017(17) -0.0065(16) C15 0.016(2) 0.026(2) 0.0238(19) 0.0006(16) 0.0060(15) -0.0011(15) O2 0.0173(15) 0.0360(16) 0.0362(16) -0.0091(13) 0.0004(12) 0.0037(12) C16 0.026(2) 0.027(2) 0.027(2) 0.0048(17) -0.0034(17) 0.0053(17) C17 0.030(2) 0.040(2) 0.027(2) -0.0067(19) 0.0043(18) -0.0053(19) C18 0.035(3) 0.064(3) 0.029(2) -0.009(2) 0.0065(19) -0.003(2) C19 0.035(3) 0.069(4) 0.038(3) 0.015(3) 0.006(2) -0.002(2) C20 0.048(3) 0.046(3) 0.059(3) 0.010(3) 0.009(3) -0.012(2) C21 0.043(3) 0.037(3) 0.046(3) -0.002(2) 0.006(2) 0.001(2) C22 0.021(2) 0.031(2) 0.024(2) -0.0070(16) 0.0035(15) 0.0044(15) C23 0.031(2) 0.035(2) 0.028(2) -0.0038(19) -0.0003(18) 0.0088(19) C24 0.047(3) 0.031(2) 0.037(2) -0.0017(18) 0.003(2) 0.006(2) C25 0.036(2) 0.037(3) 0.043(3) -0.009(2) 0.007(2) -0.001(2) C26 0.025(2) 0.049(3) 0.033(2) -0.015(2) -0.0005(18) 0.0027(19) C27 0.026(2) 0.038(2) 0.026(2) -0.0030(18) 0.0008(17) 0.0042(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 Au1 P1 2.2283(10) . ? Au1 Cl1 2.2714(12) . ? P1 C22 1.813(4) . ? P1 C16 1.823(4) . ? P1 C1 1.830(4) . ? C1 C2 1.393(6) . ? C1 C6 1.394(5) . ? C2 C3 1.376(6) . ? C3 C4 1.380(6) . ? C4 C5 1.379(6) . ? C5 C6 1.405(5) . ? C6 C7 1.489(5) . ? C7 N1 1.249(5) . ? N1 C8 1.455(5) . ? C8 C9 1.517(5) . ? C9 O1 1.220(5) . ? C9 N2 1.348(5) . ? N2 C10 1.406(5) . ? C10 C11 1.398(5) . ? C10 C15 1.407(5) . ? C11 C12 1.383(6) . ? C12 C13 1.399(6) . ? C13 C14 1.382(6) . ? C14 C15 1.373(6) . ? C15 O2 1.369(5) . ? C16 C21 1.382(6) . ? C16 C17 1.384(6) . ? C17 C18 1.396(6) . ? C18 C19 1.371(7) . ? C19 C20 1.370(8) . ? C20 C21 1.393(7) . ? C22 C23 1.396(6) . ? C22 C27 1.397(6) . ? C23 C24 1.384(7) . ? C24 C25 1.391(7) . ? C25 C26 1.385(7) . ? C26 C27 1.387(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Au1 Cl1 179.61(6) . . ? C22 P1 C16 106.84(18) . . ? C22 P1 C1 107.35(19) . . ? C16 P1 C1 102.47(19) . . ? C22 P1 Au1 112.13(13) . . ? C16 P1 Au1 111.88(13) . . ? C1 P1 Au1 115.41(14) . . ? C2 C1 C6 118.9(4) . . ? C2 C1 P1 117.2(3) . . ? C6 C1 P1 123.8(3) . . ? C3 C2 C1 121.9(4) . . ? C2 C3 C4 119.2(4) . . ? C5 C4 C3 120.3(4) . . ? C4 C5 C6 120.8(4) . . ? C1 C6 C5 119.0(4) . . ? C1 C6 C7 124.1(4) . . ? C5 C6 C7 116.9(3) . . ? N1 C7 C6 120.0(4) . . ? C7 N1 C8 121.0(3) . . ? N1 C8 C9 110.9(3) . . ? O1 C9 N2 124.9(4) . . ? O1 C9 C8 120.9(4) . . ? N2 C9 C8 114.2(3) . . ? C9 N2 C10 129.4(3) . . ? C11 C10 N2 125.0(4) . . ? C11 C10 C15 118.8(4) . . ? N2 C10 C15 116.2(3) . . ? C12 C11 C10 120.3(4) . . ? C11 C12 C13 120.1(4) . . ? C14 C13 C12 119.7(4) . . ? C15 C14 C13 120.6(4) . . ? O2 C15 C14 123.7(4) . . ? O2 C15 C10 115.8(3) . . ? C14 C15 C10 120.5(4) . . ? C21 C16 C17 120.1(4) . . ? C21 C16 P1 117.7(3) . . ? C17 C16 P1 122.2(3) . . ? C16 C17 C18 118.6(4) . . ? C19 C18 C17 121.2(5) . . ? C20 C19 C18 120.1(5) . . ? C19 C20 C21 119.6(5) . . ? C16 C21 C20 120.4(5) . . ? C23 C22 C27 119.6(4) . . ? C23 C22 P1 121.6(3) . . ? C27 C22 P1 118.7(3) . . ? C24 C23 C22 119.9(4) . . ? C23 C24 C25 120.4(4) . . ? C26 C25 C24 119.7(4) . . ? C25 C26 C27 120.4(4) . . ? C26 C27 C22 119.9(4) . . ? 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 C22 P1 C1 C2 86.6(4) . . . . ? C16 P1 C1 C2 -25.8(4) . . . . ? Au1 P1 C1 C2 -147.6(3) . . . . ? C22 P1 C1 C6 -98.0(4) . . . . ? C16 P1 C1 C6 149.6(4) . . . . ? Au1 P1 C1 C6 27.8(4) . . . . ? C6 C1 C2 C3 -1.8(7) . . . . ? P1 C1 C2 C3 173.8(4) . . . . ? C1 C2 C3 C4 -1.2(7) . . . . ? C2 C3 C4 C5 3.0(7) . . . . ? C3 C4 C5 C6 -1.9(6) . . . . ? C2 C1 C6 C5 2.9(6) . . . . ? P1 C1 C6 C5 -172.4(3) . . . . ? C2 C1 C6 C7 -175.6(4) . . . . ? P1 C1 C6 C7 9.0(6) . . . . ? C4 C5 C6 C1 -1.1(6) . . . . ? C4 C5 C6 C7 177.6(4) . . . . ? C1 C6 C7 N1 -160.1(4) . . . . ? C5 C6 C7 N1 21.4(6) . . . . ? C6 C7 N1 C8 -178.7(4) . . . . ? C7 N1 C8 C9 -174.5(4) . . . . ? N1 C8 C9 O1 -175.4(4) . . . . ? N1 C8 C9 N2 3.0(5) . . . . ? O1 C9 N2 C10 -1.5(7) . . . . ? C8 C9 N2 C10 -180.0(4) . . . . ? C9 N2 C10 C11 -14.3(6) . . . . ? C9 N2 C10 C15 166.8(4) . . . . ? N2 C10 C11 C12 -179.3(4) . . . . ? C15 C10 C11 C12 -0.3(6) . . . . ? C10 C11 C12 C13 -1.0(6) . . . . ? C11 C12 C13 C14 1.0(6) . . . . ? C12 C13 C14 C15 0.3(6) . . . . ? C13 C14 C15 O2 179.2(4) . . . . ? C13 C14 C15 C10 -1.7(6) . . . . ? C11 C10 C15 O2 -179.2(3) . . . . ? N2 C10 C15 O2 -0.1(5) . . . . ? C11 C10 C15 C14 1.7(6) . . . . ? N2 C10 C15 C14 -179.3(4) . . . . ? C22 P1 C16 C21 178.6(3) . . . . ? C1 P1 C16 C21 -68.7(4) . . . . ? Au1 P1 C16 C21 55.5(4) . . . . ? C22 P1 C16 C17 -3.4(4) . . . . ? C1 P1 C16 C17 109.3(4) . . . . ? Au1 P1 C16 C17 -126.5(3) . . . . ? C21 C16 C17 C18 0.4(7) . . . . ? P1 C16 C17 C18 -177.6(3) . . . . ? C16 C17 C18 C19 0.1(7) . . . . ? C17 C18 C19 C20 -0.2(8) . . . . ? C18 C19 C20 C21 -0.2(8) . . . . ? C17 C16 C21 C20 -0.8(7) . . . . ? P1 C16 C21 C20 177.3(4) . . . . ? C19 C20 C21 C16 0.7(8) . . . . ? C16 P1 C22 C23 107.8(3) . . . . ? C1 P1 C22 C23 -1.5(4) . . . . ? Au1 P1 C22 C23 -129.3(3) . . . . ? C16 P1 C22 C27 -75.5(3) . . . . ? C1 P1 C22 C27 175.2(3) . . . . ? Au1 P1 C22 C27 47.5(3) . . . . ? C27 C22 C23 C24 -1.0(6) . . . . ? P1 C22 C23 C24 175.7(3) . . . . ? C22 C23 C24 C25 0.8(6) . . . . ? C23 C24 C25 C26 0.3(7) . . . . ? C24 C25 C26 C27 -1.3(7) . . . . ? C25 C26 C27 C22 1.1(6) . . . . ? C23 C22 C27 C26 0.0(6) . . . . ? P1 C22 C27 C26 -176.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 N1 0.88 2.09 2.592(5) 115.5 . O2 H2A O1 0.84 1.94 2.661(4) 142.9 1_655 _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.177 _refine_diff_density_min -0.967 _refine_diff_density_rms 0.104 #===END data_7c _database_code_depnum_ccdc_archive 'CCDC 771448' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H26 Cl1 N2 O2 P Pd, C1 H2 Cl2' _chemical_formula_sum 'C29 H28 Cl3 N2 O2 P Pd' _chemical_formula_weight 680.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 13.6159(6) _cell_length_b 13.2505(6) _cell_length_c 16.1783(7) _cell_angle_alpha 90.00 _cell_angle_beta 95.7566(8) _cell_angle_gamma 90.00 _cell_volume 2904.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10080 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.61 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 1.000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.747 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick,2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25451 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0336 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 29.00 _reflns_number_total 7080 _reflns_number_gt 5579 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0235P)^2^+3.0958P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7080 _refine_ls_number_parameters 350 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0480 _refine_ls_R_factor_gt 0.0320 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0644 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 0.171289(13) 0.077923(13) -0.021249(11) 0.01849(5) Uani 1 1 d . . . P1 P 0.10003(4) 0.19059(4) 0.05265(4) 0.01727(12) Uani 1 1 d . . . Cl1 Cl 0.24140(4) -0.04883(4) -0.10419(4) 0.02300(13) Uani 1 1 d . . . C28 C 0.0967(2) 0.1301(2) -0.12775(15) 0.0368(7) Uani 1 1 d . . . H28A H 0.0646 0.1942 -0.1166 0.044 Uiso 1 1 calc R . . H28B H 0.0466 0.0806 -0.1484 0.044 Uiso 1 1 calc R . . H28C H 0.1430 0.1406 -0.1696 0.044 Uiso 1 1 calc R . . N1 N 0.26212(14) 0.03353(15) 0.09232(12) 0.0192(4) Uani 1 1 d . . . C1 C 0.07512(17) 0.13354(17) 0.15148(14) 0.0195(5) Uani 1 1 d . . . C2 C -0.01124(18) 0.15547(19) 0.18674(15) 0.0236(5) Uani 1 1 d . . . H2B H -0.0604 0.1958 0.1568 0.028 Uiso 1 1 calc R . . C3 C -0.0273(2) 0.1195(2) 0.26526(16) 0.0297(6) Uani 1 1 d . . . H3 H -0.0875 0.1339 0.2878 0.036 Uiso 1 1 calc R . . C4 C 0.0445(2) 0.0631(2) 0.31004(17) 0.0347(7) Uani 1 1 d . . . H4 H 0.0345 0.0397 0.3641 0.042 Uiso 1 1 calc R . . C5 C 0.1312(2) 0.0407(2) 0.27609(16) 0.0321(6) Uani 1 1 d . . . H5 H 0.1807 0.0024 0.3076 0.038 Uiso 1 1 calc R . . C6 C 0.14755(18) 0.07312(19) 0.19631(15) 0.0230(5) Uani 1 1 d . . . C7 C 0.24143(18) 0.04055(19) 0.16760(15) 0.0233(5) Uani 1 1 d . . . H7 H 0.2924 0.0227 0.2095 0.028 Uiso 1 1 calc R . . C8 C 0.36315(17) -0.00226(19) 0.08169(15) 0.0226(5) Uani 1 1 d . . . H8A H 0.3601 -0.0592 0.0419 0.027 Uiso 1 1 calc R . . H8B H 0.3957 -0.0263 0.1356 0.027 Uiso 1 1 calc R . . C9 C 0.42212(17) 0.08463(18) 0.04924(14) 0.0209(5) Uani 1 1 d . . . N2 N 0.41281(15) 0.09396(16) -0.03330(12) 0.0206(4) Uani 1 1 d . . . H2 H 0.375(2) 0.053(2) -0.0574(17) 0.025 Uiso 1 1 d . . . O1 O 0.47172(13) 0.14116(14) 0.09785(10) 0.0273(4) Uani 1 1 d . . . C10 C 0.44343(17) 0.17391(18) -0.08284(14) 0.0192(5) Uani 1 1 d . . . C11 C 0.42389(19) 0.1622(2) -0.16870(15) 0.0270(6) Uani 1 1 d . . . H11 H 0.3957 0.1011 -0.1906 0.032 Uiso 1 1 calc R . . C12 C 0.4453(2) 0.2388(2) -0.22220(15) 0.0289(6) Uani 1 1 d . . . H12 H 0.4317 0.2300 -0.2805 0.035 Uiso 1 1 calc R . . C13 C 0.48664(19) 0.3289(2) -0.19075(15) 0.0257(5) Uani 1 1 d . . . O2 O 0.50835(16) 0.40742(15) -0.24016(12) 0.0358(5) Uani 1 1 d . . . H2A H 0.498(3) 0.392(3) -0.288(2) 0.054 Uiso 1 1 d . . . C14 C 0.50654(19) 0.3398(2) -0.10548(15) 0.0277(6) Uani 1 1 d . . . H14 H 0.5349 0.4009 -0.0837 0.033 Uiso 1 1 calc R . . C15 C 0.48591(18) 0.26345(19) -0.05145(15) 0.0238(5) Uani 1 1 d . . . H15 H 0.5006 0.2721 0.0068 0.029 Uiso 1 1 calc R . . C16 C 0.18065(17) 0.29497(17) 0.08607(14) 0.0190(5) Uani 1 1 d . . . C17 C 0.25808(19) 0.32125(19) 0.03968(16) 0.0263(5) Uani 1 1 d . . . H17 H 0.2677 0.2854 -0.0097 0.032 Uiso 1 1 calc R . . C18 C 0.3210(2) 0.4000(2) 0.06605(18) 0.0323(6) Uani 1 1 d . . . H18 H 0.3732 0.4183 0.0343 0.039 Uiso 1 1 calc R . . C19 C 0.30788(19) 0.4520(2) 0.13830(16) 0.0263(6) Uani 1 1 d . . . H19 H 0.3524 0.5043 0.1570 0.032 Uiso 1 1 calc R . . C20 C 0.23025(19) 0.42806(19) 0.18330(15) 0.0263(5) Uani 1 1 d . . . H20 H 0.2200 0.4654 0.2318 0.032 Uiso 1 1 calc R . . C21 C 0.16728(19) 0.34963(19) 0.15774(15) 0.0237(5) Uani 1 1 d . . . H21 H 0.1144 0.3329 0.1893 0.028 Uiso 1 1 calc R . . C22 C -0.01685(17) 0.24747(18) 0.01314(14) 0.0196(5) Uani 1 1 d . . . C23 C -0.09143(19) 0.18471(19) -0.02187(15) 0.0258(5) Uani 1 1 d . . . H23 H -0.0800 0.1142 -0.0253 0.031 Uiso 1 1 calc R . . C24 C -0.18227(19) 0.2241(2) -0.05189(16) 0.0289(6) Uani 1 1 d . . . H24 H -0.2330 0.1804 -0.0752 0.035 Uiso 1 1 calc R . . C25 C -0.19949(19) 0.3266(2) -0.04810(16) 0.0289(6) Uani 1 1 d . . . H25 H -0.2618 0.3534 -0.0691 0.035 Uiso 1 1 calc R . . C26 C -0.12587(19) 0.3900(2) -0.01377(17) 0.0299(6) Uani 1 1 d . . . H26 H -0.1376 0.4605 -0.0111 0.036 Uiso 1 1 calc R . . C27 C -0.03488(18) 0.35089(19) 0.01691(15) 0.0241(5) Uani 1 1 d . . . H27 H 0.0154 0.3948 0.0406 0.029 Uiso 1 1 calc R . . C29 C 0.6738(2) 0.2875(2) 0.14450(19) 0.0414(7) Uani 1 1 d . . . H29A H 0.6208 0.2361 0.1393 0.050 Uiso 1 1 calc R . . H29B H 0.7199 0.2722 0.1026 0.050 Uiso 1 1 calc R . . Cl2 Cl 0.73703(8) 0.27994(7) 0.24320(6) 0.0618(3) Uani 1 1 d . . . Cl3 Cl 0.62156(7) 0.40755(6) 0.12396(6) 0.0572(2) 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 Pd1 0.02196(10) 0.01782(9) 0.01576(9) 0.00023(7) 0.00228(6) 0.00196(7) P1 0.0194(3) 0.0168(3) 0.0158(3) 0.0012(2) 0.0026(2) 0.0007(2) Cl1 0.0263(3) 0.0204(3) 0.0224(3) -0.0043(2) 0.0033(2) -0.0002(2) C28 0.0512(18) 0.0427(17) 0.0162(13) 0.0011(12) 0.0011(12) 0.0196(14) N1 0.0203(10) 0.0173(10) 0.0203(10) 0.0012(8) 0.0035(8) 0.0012(8) C1 0.0235(12) 0.0181(12) 0.0173(11) 0.0000(9) 0.0045(9) -0.0038(9) C2 0.0236(13) 0.0238(13) 0.0238(13) 0.0030(10) 0.0037(10) -0.0008(10) C3 0.0306(14) 0.0323(15) 0.0281(14) 0.0034(11) 0.0126(11) 0.0008(12) C4 0.0431(17) 0.0386(17) 0.0247(14) 0.0112(12) 0.0152(12) 0.0067(13) C5 0.0374(16) 0.0385(16) 0.0212(13) 0.0099(11) 0.0074(11) 0.0079(13) C6 0.0265(13) 0.0222(12) 0.0208(12) 0.0028(10) 0.0049(10) 0.0011(10) C7 0.0255(13) 0.0237(12) 0.0204(12) 0.0053(10) 0.0001(10) 0.0019(10) C8 0.0219(12) 0.0225(13) 0.0236(12) 0.0042(10) 0.0035(10) 0.0039(10) C9 0.0188(11) 0.0230(12) 0.0211(12) -0.0010(10) 0.0025(9) 0.0053(10) N2 0.0213(10) 0.0221(11) 0.0182(10) -0.0017(8) 0.0005(8) -0.0033(8) O1 0.0312(10) 0.0311(10) 0.0189(9) -0.0009(7) -0.0009(7) -0.0031(8) C10 0.0157(11) 0.0247(12) 0.0170(11) 0.0000(9) 0.0010(9) -0.0011(9) C11 0.0325(14) 0.0273(14) 0.0202(12) -0.0042(10) -0.0015(10) -0.0075(11) C12 0.0368(15) 0.0346(15) 0.0146(12) -0.0035(10) -0.0008(11) -0.0076(12) C13 0.0285(14) 0.0300(14) 0.0186(12) 0.0009(10) 0.0026(10) -0.0066(11) O2 0.0534(13) 0.0356(11) 0.0180(9) 0.0012(8) 0.0017(9) -0.0175(10) C14 0.0330(14) 0.0286(14) 0.0215(13) -0.0041(10) 0.0020(11) -0.0114(11) C15 0.0249(13) 0.0314(14) 0.0152(11) -0.0030(10) 0.0020(10) -0.0056(11) C16 0.0191(12) 0.0186(12) 0.0191(12) 0.0041(9) 0.0000(9) 0.0018(9) C17 0.0269(13) 0.0254(13) 0.0278(14) -0.0012(11) 0.0086(11) 0.0000(11) C18 0.0239(14) 0.0310(15) 0.0436(17) 0.0020(12) 0.0104(12) -0.0045(11) C19 0.0233(13) 0.0234(13) 0.0307(14) 0.0027(11) -0.0044(11) -0.0037(10) C20 0.0336(14) 0.0254(13) 0.0191(12) -0.0006(10) -0.0019(10) -0.0046(11) C21 0.0258(13) 0.0271(13) 0.0187(12) 0.0000(10) 0.0042(10) -0.0042(10) C22 0.0210(12) 0.0216(12) 0.0166(11) 0.0027(9) 0.0032(9) 0.0001(10) C23 0.0290(14) 0.0213(13) 0.0266(13) 0.0018(10) -0.0006(11) -0.0039(10) C24 0.0234(13) 0.0320(15) 0.0299(14) 0.0051(11) -0.0043(11) -0.0078(11) C25 0.0194(13) 0.0349(15) 0.0319(14) 0.0089(12) -0.0011(11) 0.0027(11) C26 0.0290(14) 0.0243(13) 0.0361(15) 0.0025(11) 0.0015(12) 0.0063(11) C27 0.0242(13) 0.0213(13) 0.0267(13) -0.0022(10) 0.0012(10) -0.0008(10) C29 0.0469(19) 0.0347(17) 0.0409(17) -0.0050(13) -0.0045(14) -0.0004(14) Cl2 0.0794(7) 0.0542(5) 0.0466(5) -0.0097(4) -0.0189(5) 0.0184(5) Cl3 0.0618(5) 0.0386(5) 0.0646(6) -0.0111(4) -0.0255(4) 0.0080(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C28 2.031(3) . ? Pd1 N1 2.1899(19) . ? Pd1 P1 2.1983(6) . ? Pd1 Cl1 2.4062(6) . ? P1 C16 1.814(2) . ? P1 C22 1.818(2) . ? P1 C1 1.831(2) . ? N1 C7 1.281(3) . ? N1 C8 1.481(3) . ? C1 C2 1.388(3) . ? C1 C6 1.413(3) . ? C2 C3 1.394(3) . ? C3 C4 1.377(4) . ? C4 C5 1.383(4) . ? C5 C6 1.399(3) . ? C6 C7 1.468(3) . ? C8 C9 1.527(3) . ? C9 O1 1.236(3) . ? C9 N2 1.335(3) . ? N2 C10 1.416(3) . ? C10 C15 1.393(3) . ? C10 C11 1.397(3) . ? C11 C12 1.384(4) . ? C12 C13 1.394(4) . ? C13 O2 1.362(3) . ? C13 C14 1.386(3) . ? C14 C15 1.384(3) . ? C16 C21 1.394(3) . ? C16 C17 1.398(3) . ? C17 C18 1.390(4) . ? C18 C19 1.383(4) . ? C19 C20 1.379(4) . ? C20 C21 1.384(3) . ? C22 C23 1.389(3) . ? C22 C27 1.395(3) . ? C23 C24 1.385(4) . ? C24 C25 1.380(4) . ? C25 C26 1.381(4) . ? C26 C27 1.388(3) . ? C29 Cl2 1.739(3) . ? C29 Cl3 1.760(3) . ? 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 C28 Pd1 N1 174.39(11) . . ? C28 Pd1 P1 91.15(8) . . ? N1 Pd1 P1 88.23(5) . . ? C28 Pd1 Cl1 87.53(8) . . ? N1 Pd1 Cl1 93.33(5) . . ? P1 Pd1 Cl1 177.18(2) . . ? C16 P1 C22 105.72(11) . . ? C16 P1 C1 102.36(11) . . ? C22 P1 C1 104.24(11) . . ? C16 P1 Pd1 113.14(8) . . ? C22 P1 Pd1 120.59(8) . . ? C1 P1 Pd1 108.97(8) . . ? C7 N1 C8 115.4(2) . . ? C7 N1 Pd1 128.23(17) . . ? C8 N1 Pd1 116.19(14) . . ? C2 C1 C6 119.0(2) . . ? C2 C1 P1 120.74(18) . . ? C6 C1 P1 120.09(18) . . ? C1 C2 C3 121.3(2) . . ? C4 C3 C2 119.8(2) . . ? C3 C4 C5 119.8(2) . . ? C4 C5 C6 121.4(3) . . ? C5 C6 C1 118.7(2) . . ? C5 C6 C7 115.2(2) . . ? C1 C6 C7 126.1(2) . . ? N1 C7 C6 127.1(2) . . ? N1 C8 C9 108.97(19) . . ? O1 C9 N2 124.8(2) . . ? O1 C9 C8 120.7(2) . . ? N2 C9 C8 114.4(2) . . ? C9 N2 C10 129.2(2) . . ? C15 C10 C11 119.2(2) . . ? C15 C10 N2 124.5(2) . . ? C11 C10 N2 116.3(2) . . ? C12 C11 C10 120.6(2) . . ? C11 C12 C13 120.2(2) . . ? O2 C13 C14 118.2(2) . . ? O2 C13 C12 122.9(2) . . ? C14 C13 C12 118.9(2) . . ? C15 C14 C13 121.4(2) . . ? C14 C15 C10 119.7(2) . . ? C21 C16 C17 119.0(2) . . ? C21 C16 P1 121.22(18) . . ? C17 C16 P1 119.75(18) . . ? C18 C17 C16 119.8(2) . . ? C19 C18 C17 120.4(2) . . ? C20 C19 C18 120.1(2) . . ? C19 C20 C21 120.0(2) . . ? C20 C21 C16 120.7(2) . . ? C23 C22 C27 118.8(2) . . ? C23 C22 P1 118.27(19) . . ? C27 C22 P1 122.94(19) . . ? C24 C23 C22 120.5(2) . . ? C25 C24 C23 120.3(2) . . ? C24 C25 C26 119.8(2) . . ? C25 C26 C27 120.2(2) . . ? C26 C27 C22 120.4(2) . . ? Cl2 C29 Cl3 112.27(17) . . ? 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 C28 Pd1 P1 C16 -103.94(13) . . . . ? N1 Pd1 P1 C16 70.49(9) . . . . ? C28 Pd1 P1 C22 22.56(13) . . . . ? N1 Pd1 P1 C22 -163.02(10) . . . . ? C28 Pd1 P1 C1 142.91(13) . . . . ? N1 Pd1 P1 C1 -42.66(10) . . . . ? P1 Pd1 N1 C7 27.2(2) . . . . ? Cl1 Pd1 N1 C7 -150.5(2) . . . . ? P1 Pd1 N1 C8 -147.93(16) . . . . ? Cl1 Pd1 N1 C8 34.42(16) . . . . ? C16 P1 C1 C2 98.3(2) . . . . ? C22 P1 C1 C2 -11.7(2) . . . . ? Pd1 P1 C1 C2 -141.69(18) . . . . ? C16 P1 C1 C6 -76.4(2) . . . . ? C22 P1 C1 C6 173.61(19) . . . . ? Pd1 P1 C1 C6 43.6(2) . . . . ? C6 C1 C2 C3 0.3(4) . . . . ? P1 C1 C2 C3 -174.4(2) . . . . ? C1 C2 C3 C4 1.6(4) . . . . ? C2 C3 C4 C5 -1.4(4) . . . . ? C3 C4 C5 C6 -0.8(5) . . . . ? C4 C5 C6 C1 2.6(4) . . . . ? C4 C5 C6 C7 -177.9(3) . . . . ? C2 C1 C6 C5 -2.4(4) . . . . ? P1 C1 C6 C5 172.4(2) . . . . ? C2 C1 C6 C7 178.3(2) . . . . ? P1 C1 C6 C7 -7.0(4) . . . . ? C8 N1 C7 C6 -179.6(2) . . . . ? Pd1 N1 C7 C6 5.3(4) . . . . ? C5 C6 C7 N1 157.9(3) . . . . ? C1 C6 C7 N1 -22.7(4) . . . . ? C7 N1 C8 C9 -111.0(2) . . . . ? Pd1 N1 C8 C9 64.7(2) . . . . ? N1 C8 C9 O1 91.4(3) . . . . ? N1 C8 C9 N2 -87.1(2) . . . . ? O1 C9 N2 C10 -9.6(4) . . . . ? C8 C9 N2 C10 168.8(2) . . . . ? C9 N2 C10 C15 -3.9(4) . . . . ? C9 N2 C10 C11 179.7(2) . . . . ? C15 C10 C11 C12 -0.7(4) . . . . ? N2 C10 C11 C12 175.9(2) . . . . ? C10 C11 C12 C13 -0.1(4) . . . . ? C11 C12 C13 O2 -179.3(3) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? O2 C13 C14 C15 179.6(2) . . . . ? C12 C13 C14 C15 -0.2(4) . . . . ? C13 C14 C15 C10 -0.6(4) . . . . ? C11 C10 C15 C14 1.1(4) . . . . ? N2 C10 C15 C14 -175.3(2) . . . . ? C22 P1 C16 C21 72.6(2) . . . . ? C1 P1 C16 C21 -36.3(2) . . . . ? Pd1 P1 C16 C21 -153.35(17) . . . . ? C22 P1 C16 C17 -107.7(2) . . . . ? C1 P1 C16 C17 143.4(2) . . . . ? Pd1 P1 C16 C17 26.3(2) . . . . ? C21 C16 C17 C18 0.8(4) . . . . ? P1 C16 C17 C18 -178.8(2) . . . . ? C16 C17 C18 C19 0.6(4) . . . . ? C17 C18 C19 C20 -2.1(4) . . . . ? C18 C19 C20 C21 2.2(4) . . . . ? C19 C20 C21 C16 -0.8(4) . . . . ? C17 C16 C21 C20 -0.7(4) . . . . ? P1 C16 C21 C20 178.96(19) . . . . ? C16 P1 C22 C23 176.00(19) . . . . ? C1 P1 C22 C23 -76.5(2) . . . . ? Pd1 P1 C22 C23 46.2(2) . . . . ? C16 P1 C22 C27 -4.4(2) . . . . ? C1 P1 C22 C27 103.1(2) . . . . ? Pd1 P1 C22 C27 -134.19(18) . . . . ? C27 C22 C23 C24 -0.5(4) . . . . ? P1 C22 C23 C24 179.15(19) . . . . ? C22 C23 C24 C25 0.6(4) . . . . ? C23 C24 C25 C26 -0.4(4) . . . . ? C24 C25 C26 C27 0.0(4) . . . . ? C25 C26 C27 C22 0.2(4) . . . . ? C23 C22 C27 C26 0.1(4) . . . . ? P1 C22 C27 C26 -179.55(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2 Cl1 0.82(3) 2.33(3) 3.131(2) 166(3) . O2 H2A O1 0.79(3) 1.90(3) 2.696(3) 178(4) 4_565 _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.679 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.087 #===END data_8a _database_code_depnum_ccdc_archive 'CCDC 771449' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H25 N2 O2 P Pt, C1 H1 Cl3' _chemical_formula_sum 'C29 H26 Cl3 N2 O2 P Pt' _chemical_formula_weight 766.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1632(14) _cell_length_b 11.944(2) _cell_length_c 14.872(2) _cell_angle_alpha 99.169(3) _cell_angle_beta 103.818(2) _cell_angle_gamma 112.534(2) _cell_volume 1401.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9680 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.92 _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.817 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 5.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.128 _exptl_absorpt_correction_T_max 0.643 _exptl_absorpt_process_details 'SADABS v2.01, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12247 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 28.92 _reflns_number_total 6407 _reflns_number_gt 5961 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0531P)^2^+3.0815P] 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 6407 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0355 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0855 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.006 _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 0.447165(19) 0.360310(13) 0.244693(10) 0.01752(6) Uani 1 1 d . . . C28 C 0.4693(7) 0.4216(4) 0.3859(3) 0.0275(10) Uani 1 1 d . . . H28A H 0.4800 0.5079 0.3996 0.041 Uiso 1 1 calc R . . H28B H 0.5689 0.4203 0.4276 0.041 Uiso 1 1 calc R . . H28C H 0.3698 0.3659 0.3981 0.041 Uiso 1 1 calc R . . P1 P 0.61814(14) 0.55145(10) 0.25345(8) 0.0176(2) Uani 1 1 d . . . C1 C 0.7016(6) 0.5532(4) 0.1534(3) 0.0209(8) Uani 1 1 d . . . C2 C 0.8457(6) 0.6603(4) 0.1619(3) 0.0238(9) Uani 1 1 d . . . H2A H 0.8953 0.7287 0.2189 0.029 Uiso 1 1 calc R . . C3 C 0.9178(6) 0.6693(5) 0.0898(4) 0.0275(10) Uani 1 1 d . . . H3 H 1.0138 0.7437 0.0968 0.033 Uiso 1 1 calc R . . C4 C 0.8487(6) 0.5692(5) 0.0075(4) 0.0292(10) Uani 1 1 d . . . H4 H 0.8976 0.5743 -0.0421 0.035 Uiso 1 1 calc R . . C5 C 0.7087(6) 0.4622(5) -0.0023(3) 0.0253(9) Uani 1 1 d . . . H5 H 0.6630 0.3936 -0.0588 0.030 Uiso 1 1 calc R . . C6 C 0.6317(5) 0.4518(4) 0.0693(3) 0.0195(8) Uani 1 1 d . . . C7 C 0.4831(6) 0.3317(4) 0.0454(3) 0.0218(8) Uani 1 1 d . . . H7 H 0.4416 0.2803 -0.0192 0.026 Uiso 1 1 calc R . . N1 N 0.4027(5) 0.2878(3) 0.1011(3) 0.0199(7) Uani 1 1 d . . . C8 C 0.2570(6) 0.1641(4) 0.0605(3) 0.0273(10) Uani 1 1 d . . . H8A H 0.2769 0.1105 0.0114 0.033 Uiso 1 1 calc R . . H8B H 0.1577 0.1750 0.0280 0.033 Uiso 1 1 calc R . . C9 C 0.2223(6) 0.0984(4) 0.1372(3) 0.0246(9) Uani 1 1 d . . . O1 O 0.1224(5) -0.0170(3) 0.1093(2) 0.0312(8) Uani 1 1 d . . . N2 N 0.2978(5) 0.1703(3) 0.2282(3) 0.0199(7) Uani 1 1 d . . . C10 C 0.2812(6) 0.1146(4) 0.3053(3) 0.0213(8) Uani 1 1 d . . . C11 C 0.1286(6) 0.0305(4) 0.3078(4) 0.0268(9) Uani 1 1 d . . . O2 O -0.0191(4) -0.0080(3) 0.2362(3) 0.0313(7) Uani 1 1 d . . . H2 H -0.0073 -0.0273 0.1825 0.047 Uiso 1 1 calc R . . C12 C 0.1229(8) -0.0154(5) 0.3899(4) 0.0366(12) Uani 1 1 d . . . H12 H 0.0187 -0.0722 0.3924 0.044 Uiso 1 1 calc R . . C13 C 0.2658(9) 0.0215(5) 0.4652(4) 0.0420(14) Uani 1 1 d . . . H13 H 0.2605 -0.0090 0.5201 0.050 Uiso 1 1 calc R . . C14 C 0.4186(8) 0.1033(5) 0.4616(4) 0.0386(13) Uani 1 1 d . . . H14 H 0.5183 0.1280 0.5136 0.046 Uiso 1 1 calc R . . C15 C 0.4250(6) 0.1486(4) 0.3826(3) 0.0286(10) Uani 1 1 d . . . H15 H 0.5302 0.2046 0.3806 0.034 Uiso 1 1 calc R . . C16 C 0.5321(5) 0.6665(4) 0.2542(3) 0.0217(8) Uani 1 1 d . . . C17 C 0.3720(6) 0.6293(5) 0.2615(3) 0.0275(9) Uani 1 1 d . . . H17 H 0.3125 0.5469 0.2664 0.033 Uiso 1 1 calc R . . C18 C 0.2998(7) 0.7124(5) 0.2617(4) 0.0361(11) Uani 1 1 d . . . H18 H 0.1912 0.6868 0.2669 0.043 Uiso 1 1 calc R . . C19 C 0.3851(8) 0.8314(5) 0.2543(4) 0.0391(12) Uani 1 1 d . . . H19 H 0.3351 0.8878 0.2540 0.047 Uiso 1 1 calc R . . C20 C 0.5431(8) 0.8693(5) 0.2471(5) 0.0418(13) Uani 1 1 d . . . H20 H 0.6015 0.9518 0.2419 0.050 Uiso 1 1 calc R . . C21 C 0.6173(7) 0.7870(5) 0.2474(4) 0.0335(11) Uani 1 1 d . . . H21 H 0.7266 0.8137 0.2430 0.040 Uiso 1 1 calc R . . C22 C 0.8059(5) 0.6219(4) 0.3590(3) 0.0205(8) Uani 1 1 d . . . C23 C 0.9276(6) 0.5773(5) 0.3624(4) 0.0289(10) Uani 1 1 d . . . H23 H 0.9158 0.5168 0.3078 0.035 Uiso 1 1 calc R . . C24 C 1.0630(7) 0.6204(6) 0.4438(4) 0.0385(12) Uani 1 1 d . . . H24 H 1.1469 0.5920 0.4449 0.046 Uiso 1 1 calc R . . C25 C 1.0786(7) 0.7048(6) 0.5244(4) 0.0398(13) Uani 1 1 d . . . H25 H 1.1718 0.7328 0.5813 0.048 Uiso 1 1 calc R . . C26 C 0.9602(7) 0.7487(5) 0.5229(3) 0.0349(11) Uani 1 1 d . . . H26 H 0.9722 0.8074 0.5787 0.042 Uiso 1 1 calc R . . C27 C 0.8218(6) 0.7076(4) 0.4398(3) 0.0267(9) Uani 1 1 d . . . H27 H 0.7398 0.7381 0.4387 0.032 Uiso 1 1 calc R . . C29 C -0.1508(10) 0.1924(7) 0.1770(6) 0.059(2) Uani 1 1 d . . . H29 H -0.1326 0.1240 0.2017 0.071 Uiso 1 1 calc R . . Cl1 Cl -0.31675(18) 0.20355(16) 0.20701(11) 0.0440(3) Uani 1 1 d . . . Cl2 Cl 0.0323(3) 0.3328(3) 0.2348(3) 0.1007(9) Uani 1 1 d . . . Cl3 Cl -0.1873(5) 0.1529(2) 0.0563(2) 0.1329(16) 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 Pt1 0.02079(10) 0.01556(9) 0.01640(9) 0.00385(6) 0.00677(6) 0.00804(7) C28 0.036(3) 0.021(2) 0.025(2) 0.0059(17) 0.014(2) 0.010(2) P1 0.0196(5) 0.0165(5) 0.0171(5) 0.0041(4) 0.0065(4) 0.0083(4) C1 0.024(2) 0.025(2) 0.0198(19) 0.0100(17) 0.0084(16) 0.0142(18) C2 0.024(2) 0.024(2) 0.025(2) 0.0073(17) 0.0096(17) 0.0111(18) C3 0.024(2) 0.029(2) 0.032(2) 0.015(2) 0.0114(19) 0.0106(19) C4 0.032(2) 0.038(3) 0.028(2) 0.016(2) 0.019(2) 0.019(2) C5 0.030(2) 0.032(2) 0.019(2) 0.0063(18) 0.0090(18) 0.018(2) C6 0.023(2) 0.024(2) 0.0163(18) 0.0080(16) 0.0066(16) 0.0143(18) C7 0.028(2) 0.023(2) 0.0135(18) 0.0027(16) 0.0041(16) 0.0130(18) N1 0.0238(18) 0.0163(16) 0.0219(17) 0.0055(14) 0.0078(14) 0.0109(15) C8 0.031(2) 0.023(2) 0.022(2) 0.0043(17) 0.0073(18) 0.0068(19) C9 0.027(2) 0.023(2) 0.023(2) 0.0062(17) 0.0076(18) 0.0119(19) O1 0.0353(19) 0.0178(15) 0.0295(17) 0.0030(13) 0.0073(15) 0.0039(14) N2 0.0207(17) 0.0158(16) 0.0189(17) 0.0049(13) 0.0037(14) 0.0050(14) C10 0.028(2) 0.0161(18) 0.022(2) 0.0061(16) 0.0079(17) 0.0111(17) C11 0.034(3) 0.020(2) 0.031(2) 0.0096(18) 0.015(2) 0.0132(19) O2 0.0275(17) 0.0274(17) 0.0367(19) 0.0104(15) 0.0116(15) 0.0086(14) C12 0.052(3) 0.026(2) 0.036(3) 0.015(2) 0.023(2) 0.013(2) C13 0.068(4) 0.031(3) 0.029(3) 0.015(2) 0.018(3) 0.020(3) C14 0.056(4) 0.029(3) 0.025(2) 0.009(2) 0.004(2) 0.020(3) C15 0.031(2) 0.023(2) 0.029(2) 0.0083(19) 0.006(2) 0.012(2) C16 0.022(2) 0.0210(19) 0.020(2) 0.0031(16) 0.0040(16) 0.0088(17) C17 0.029(2) 0.028(2) 0.030(2) 0.0112(19) 0.0126(19) 0.014(2) C18 0.031(3) 0.044(3) 0.043(3) 0.014(2) 0.015(2) 0.024(2) C19 0.042(3) 0.036(3) 0.046(3) 0.010(2) 0.012(3) 0.026(3) C20 0.047(3) 0.023(2) 0.059(4) 0.014(2) 0.015(3) 0.019(2) C21 0.029(2) 0.025(2) 0.046(3) 0.010(2) 0.011(2) 0.011(2) C22 0.020(2) 0.0207(19) 0.0203(19) 0.0090(16) 0.0064(16) 0.0072(17) C23 0.032(3) 0.028(2) 0.030(2) 0.0084(19) 0.013(2) 0.015(2) C24 0.034(3) 0.046(3) 0.039(3) 0.016(2) 0.012(2) 0.020(3) C25 0.027(3) 0.052(3) 0.027(2) 0.014(2) -0.001(2) 0.009(2) C26 0.037(3) 0.038(3) 0.019(2) 0.002(2) 0.005(2) 0.012(2) C27 0.030(2) 0.027(2) 0.020(2) 0.0035(18) 0.0064(18) 0.012(2) C29 0.072(5) 0.048(4) 0.100(6) 0.039(4) 0.062(5) 0.044(4) Cl1 0.0401(7) 0.0664(9) 0.0417(7) 0.0201(7) 0.0187(6) 0.0348(7) Cl2 0.0547(12) 0.0850(16) 0.166(3) 0.0302(17) 0.0560(16) 0.0245(12) Cl3 0.222(4) 0.0581(13) 0.112(2) -0.0007(13) 0.132(3) 0.0187(18) _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 C28 2.044(5) . ? Pt1 N1 2.050(4) . ? Pt1 N2 2.090(4) . ? Pt1 P1 2.1795(11) . ? P1 C22 1.819(4) . ? P1 C16 1.828(5) . ? P1 C1 1.828(4) . ? C1 C2 1.403(6) . ? C1 C6 1.408(6) . ? C2 C3 1.385(6) . ? C3 C4 1.382(7) . ? C4 C5 1.376(7) . ? C5 C6 1.407(6) . ? C6 C7 1.465(6) . ? C7 N1 1.279(6) . ? N1 C8 1.466(6) . ? C8 C9 1.512(6) . ? C9 O1 1.257(6) . ? C9 N2 1.333(6) . ? N2 C10 1.423(5) . ? C10 C11 1.388(7) . ? C10 C15 1.394(6) . ? C11 O2 1.362(6) . ? C11 C12 1.419(7) . ? C12 C13 1.365(9) . ? C13 C14 1.386(9) . ? C14 C15 1.375(7) . ? C16 C21 1.383(7) . ? C16 C17 1.398(7) . ? C17 C18 1.388(7) . ? C18 C19 1.373(8) . ? C19 C20 1.377(9) . ? C20 C21 1.394(7) . ? C22 C27 1.388(6) . ? C22 C23 1.403(7) . ? C23 C24 1.365(7) . ? C24 C25 1.377(9) . ? C25 C26 1.372(8) . ? C26 C27 1.399(7) . ? C29 Cl3 1.698(9) . ? C29 Cl1 1.729(6) . ? C29 Cl2 1.750(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C28 Pt1 N1 174.77(16) . . ? C28 Pt1 N2 95.44(17) . . ? N1 Pt1 N2 80.48(14) . . ? C28 Pt1 P1 89.05(14) . . ? N1 Pt1 P1 95.26(10) . . ? N2 Pt1 P1 173.78(11) . . ? C22 P1 C16 105.5(2) . . ? C22 P1 C1 102.9(2) . . ? C16 P1 C1 106.4(2) . . ? C22 P1 Pt1 113.49(14) . . ? C16 P1 Pt1 116.18(15) . . ? C1 P1 Pt1 111.26(15) . . ? C2 C1 C6 118.2(4) . . ? C2 C1 P1 118.2(3) . . ? C6 C1 P1 123.6(3) . . ? C3 C2 C1 122.0(4) . . ? C4 C3 C2 119.4(4) . . ? C5 C4 C3 119.9(4) . . ? C4 C5 C6 121.7(4) . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 113.8(4) . . ? C1 C6 C7 127.5(4) . . ? N1 C7 C6 127.8(4) . . ? C7 N1 C8 117.8(4) . . ? C7 N1 Pt1 130.4(3) . . ? C8 N1 Pt1 111.7(3) . . ? N1 C8 C9 111.8(4) . . ? O1 C9 N2 126.4(4) . . ? O1 C9 C8 117.3(4) . . ? N2 C9 C8 116.3(4) . . ? C9 N2 C10 120.0(4) . . ? C9 N2 Pt1 114.8(3) . . ? C10 N2 Pt1 125.1(3) . . ? C11 C10 C15 118.7(4) . . ? C11 C10 N2 123.2(4) . . ? C15 C10 N2 118.1(4) . . ? O2 C11 C10 123.2(4) . . ? O2 C11 C12 117.5(5) . . ? C10 C11 C12 119.3(5) . . ? C13 C12 C11 120.6(5) . . ? C12 C13 C14 120.1(5) . . ? C15 C14 C13 119.7(5) . . ? C14 C15 C10 121.7(5) . . ? C21 C16 C17 119.2(5) . . ? C21 C16 P1 123.2(4) . . ? C17 C16 P1 117.6(3) . . ? C18 C17 C16 120.2(5) . . ? C19 C18 C17 120.1(5) . . ? C18 C19 C20 120.3(5) . . ? C19 C20 C21 120.2(5) . . ? C16 C21 C20 120.1(5) . . ? C27 C22 C23 119.5(4) . . ? C27 C22 P1 121.3(4) . . ? C23 C22 P1 118.8(3) . . ? C24 C23 C22 120.2(5) . . ? C23 C24 C25 120.4(5) . . ? C26 C25 C24 120.3(5) . . ? C25 C26 C27 120.4(5) . . ? C22 C27 C26 119.2(5) . . ? Cl3 C29 Cl1 113.2(5) . . ? Cl3 C29 Cl2 110.5(4) . . ? Cl1 C29 Cl2 110.4(4) . . ? 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 C28 Pt1 P1 C22 47.9(2) . . . . ? N1 Pt1 P1 C22 -135.01(19) . . . . ? C28 Pt1 P1 C16 -74.6(2) . . . . ? N1 Pt1 P1 C16 102.40(19) . . . . ? C28 Pt1 P1 C1 163.4(2) . . . . ? N1 Pt1 P1 C1 -19.51(18) . . . . ? C22 P1 C1 C2 -40.7(4) . . . . ? C16 P1 C1 C2 70.0(4) . . . . ? Pt1 P1 C1 C2 -162.6(3) . . . . ? C22 P1 C1 C6 137.7(4) . . . . ? C16 P1 C1 C6 -111.6(4) . . . . ? Pt1 P1 C1 C6 15.8(4) . . . . ? C6 C1 C2 C3 1.2(7) . . . . ? P1 C1 C2 C3 179.7(4) . . . . ? C1 C2 C3 C4 -1.4(7) . . . . ? C2 C3 C4 C5 0.5(7) . . . . ? C3 C4 C5 C6 0.7(7) . . . . ? C4 C5 C6 C1 -0.9(7) . . . . ? C4 C5 C6 C7 179.2(4) . . . . ? C2 C1 C6 C5 -0.1(6) . . . . ? P1 C1 C6 C5 -178.5(3) . . . . ? C2 C1 C6 C7 179.8(4) . . . . ? P1 C1 C6 C7 1.5(6) . . . . ? C5 C6 C7 N1 168.8(4) . . . . ? C1 C6 C7 N1 -11.2(8) . . . . ? C6 C7 N1 C8 -179.7(4) . . . . ? C6 C7 N1 Pt1 -1.9(7) . . . . ? N2 Pt1 N1 C7 -158.9(4) . . . . ? P1 Pt1 N1 C7 16.5(4) . . . . ? N2 Pt1 N1 C8 19.0(3) . . . . ? P1 Pt1 N1 C8 -165.6(3) . . . . ? C7 N1 C8 C9 154.4(4) . . . . ? Pt1 N1 C8 C9 -23.8(5) . . . . ? N1 C8 C9 O1 -166.4(4) . . . . ? N1 C8 C9 N2 15.4(6) . . . . ? O1 C9 N2 C10 6.2(7) . . . . ? C8 C9 N2 C10 -175.7(4) . . . . ? O1 C9 N2 Pt1 -177.4(4) . . . . ? C8 C9 N2 Pt1 0.6(5) . . . . ? C28 Pt1 N2 C9 165.7(4) . . . . ? N1 Pt1 N2 C9 -11.0(3) . . . . ? C28 Pt1 N2 C10 -18.2(4) . . . . ? N1 Pt1 N2 C10 165.1(4) . . . . ? C9 N2 C10 C11 -47.8(6) . . . . ? Pt1 N2 C10 C11 136.2(4) . . . . ? C9 N2 C10 C15 133.6(5) . . . . ? Pt1 N2 C10 C15 -42.4(6) . . . . ? C15 C10 C11 O2 179.6(4) . . . . ? N2 C10 C11 O2 1.0(7) . . . . ? C15 C10 C11 C12 1.8(7) . . . . ? N2 C10 C11 C12 -176.8(4) . . . . ? O2 C11 C12 C13 -178.6(5) . . . . ? C10 C11 C12 C13 -0.7(8) . . . . ? C11 C12 C13 C14 -0.7(9) . . . . ? C12 C13 C14 C15 1.0(9) . . . . ? C13 C14 C15 C10 0.1(8) . . . . ? C11 C10 C15 C14 -1.5(7) . . . . ? N2 C10 C15 C14 177.1(5) . . . . ? C22 P1 C16 C21 61.6(4) . . . . ? C1 P1 C16 C21 -47.3(5) . . . . ? Pt1 P1 C16 C21 -171.7(4) . . . . ? C22 P1 C16 C17 -118.7(4) . . . . ? C1 P1 C16 C17 132.4(4) . . . . ? Pt1 P1 C16 C17 8.0(4) . . . . ? C21 C16 C17 C18 0.2(7) . . . . ? P1 C16 C17 C18 -179.5(4) . . . . ? C16 C17 C18 C19 0.2(8) . . . . ? C17 C18 C19 C20 -0.3(9) . . . . ? C18 C19 C20 C21 0.0(10) . . . . ? C17 C16 C21 C20 -0.6(8) . . . . ? P1 C16 C21 C20 179.1(4) . . . . ? C19 C20 C21 C16 0.5(9) . . . . ? C16 P1 C22 C27 27.6(4) . . . . ? C1 P1 C22 C27 138.9(4) . . . . ? Pt1 P1 C22 C27 -100.8(4) . . . . ? C16 P1 C22 C23 -159.9(4) . . . . ? C1 P1 C22 C23 -48.5(4) . . . . ? Pt1 P1 C22 C23 71.8(4) . . . . ? C27 C22 C23 C24 -1.7(7) . . . . ? P1 C22 C23 C24 -174.4(4) . . . . ? C22 C23 C24 C25 2.1(8) . . . . ? C23 C24 C25 C26 -1.5(9) . . . . ? C24 C25 C26 C27 0.4(8) . . . . ? C23 C22 C27 C26 0.6(7) . . . . ? P1 C22 C27 C26 173.1(4) . . . . ? C25 C26 C27 C22 0.0(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 1.78 2.543(5) 150.6 . _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.698 _refine_diff_density_min -2.572 _refine_diff_density_rms 0.155 #===END data_8b _database_code_depnum_ccdc_archive 'CCDC 771450' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H27 N2 O2 P Pt, 1.5(C7 H8)' _chemical_formula_sum 'C39.50 H39 N2 O2 P Pt' _chemical_formula_weight 799.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' 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 11.8821(10) _cell_length_b 14.1839(12) _cell_length_c 21.8916(18) _cell_angle_alpha 90.00 _cell_angle_beta 103.7463(13) _cell_angle_gamma 90.00 _cell_volume 3583.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11480 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 28.36 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 3.995 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.447 _exptl_absorpt_correction_T_max 0.796 _exptl_absorpt_process_details 'SADABS, v 2.08, Sheldrick, G.M. (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 30189 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 28.87 _reflns_number_total 8575 _reflns_number_gt 6516 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0537P)^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 8575 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 0.951 _refine_ls_restrained_S_all 0.951 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.113460(12) 0.327673(12) 0.414951(7) 0.02734(6) Uani 1 1 d . . . P1 P -0.07558(9) 0.33116(7) 0.38649(5) 0.0235(2) Uani 1 1 d . . . N1 N 0.1249(3) 0.3765(2) 0.50491(14) 0.0238(7) Uani 1 1 d . . . N2 N 0.2923(3) 0.3262(2) 0.44763(18) 0.0341(8) Uani 1 1 d . . . C29 C 0.1205(4) 0.2770(5) 0.3282(2) 0.0551(15) Uani 1 1 d . . . H29A H 0.1770 0.3136 0.3119 0.083 Uiso 1 1 calc R . . H29B H 0.0440 0.2826 0.2993 0.083 Uiso 1 1 calc R . . H29C H 0.1440 0.2106 0.3319 0.083 Uiso 1 1 calc R . . C1 C -0.1392(3) 0.3357(3) 0.45458(19) 0.0251(8) Uani 1 1 d . . . C2 C -0.2562(4) 0.3123(3) 0.4458(2) 0.0347(10) Uani 1 1 d . . . H2A H -0.2982 0.2917 0.4056 0.042 Uiso 1 1 calc R . . C3 C -0.3129(4) 0.3183(3) 0.4945(2) 0.0422(12) Uani 1 1 d . . . H3 H -0.3926 0.3024 0.4874 0.051 Uiso 1 1 calc R . . C4 C -0.2526(4) 0.3476(4) 0.5529(2) 0.0477(13) Uani 1 1 d . . . H4 H -0.2914 0.3514 0.5861 0.057 Uiso 1 1 calc R . . C5 C -0.1338(3) 0.3722(3) 0.5649(2) 0.0308(9) Uani 1 1 d . . . H5 H -0.0933 0.3928 0.6054 0.037 Uiso 1 1 calc R . . C6 C -0.0768(3) 0.3654(3) 0.51524(18) 0.0264(8) Uani 1 1 d . . . C7 C 0.0470(3) 0.3861(3) 0.53563(18) 0.0263(8) Uani 1 1 d . . . H7 H 0.0727 0.4099 0.5772 0.032 Uiso 1 1 calc R . . C8 C 0.2455(3) 0.3995(3) 0.53802(19) 0.0312(9) Uani 1 1 d . . . H8A H 0.2609 0.3747 0.5815 0.037 Uiso 1 1 calc R . . H8B H 0.2547 0.4689 0.5405 0.037 Uiso 1 1 calc R . . C9 C 0.3333(4) 0.3585(3) 0.5052(2) 0.0326(9) Uani 1 1 d . . . O1 O 0.4387(3) 0.3635(3) 0.53350(15) 0.0471(8) Uani 1 1 d . . . C10 C 0.3688(4) 0.2972(4) 0.4101(2) 0.0466(13) Uani 1 1 d . . . C11 C 0.3870(5) 0.2014(5) 0.4028(3) 0.0684(19) Uani 1 1 d . . . H11 H 0.3559 0.1562 0.4262 0.082 Uiso 1 1 calc R . . C12 C 0.4515(6) 0.1726(6) 0.3606(4) 0.094(3) Uani 1 1 d . . . H12 H 0.4651 0.1074 0.3552 0.113 Uiso 1 1 calc R . . C13 C 0.4950(5) 0.2390(7) 0.3270(3) 0.091(3) Uani 1 1 d . . . H13 H 0.5384 0.2189 0.2981 0.109 Uiso 1 1 calc R . . C14 C 0.4773(4) 0.3361(6) 0.3341(3) 0.074(2) Uani 1 1 d . . . H14 H 0.5072 0.3808 0.3097 0.089 Uiso 1 1 calc R . . C15 C 0.4154(4) 0.3659(5) 0.3771(2) 0.0509(14) Uani 1 1 d . . . C16 C 0.3956(4) 0.4684(4) 0.3883(2) 0.0578(16) Uani 1 1 d . . . H16A H 0.3132 0.4838 0.3700 0.069 Uiso 1 1 calc R . . H16B H 0.4114 0.4799 0.4342 0.069 Uiso 1 1 calc R . . O2 O 0.4666(3) 0.5291(3) 0.36185(16) 0.0663(12) Uani 1 1 d . . . H2 H 0.4641 0.5839 0.3761 0.100 Uiso 1 1 calc R . . C17 C -0.1475(4) 0.2308(3) 0.3416(2) 0.0342(10) Uani 1 1 d . . . C18 C -0.1327(7) 0.1438(4) 0.3697(3) 0.088(3) Uani 1 1 d . . . H18 H -0.0883 0.1376 0.4117 0.106 Uiso 1 1 calc R . . C19 C -0.1825(7) 0.0653(4) 0.3367(4) 0.109(3) Uani 1 1 d . . . H19 H -0.1718 0.0054 0.3567 0.131 Uiso 1 1 calc R . . C20 C -0.2466(5) 0.0715(4) 0.2764(3) 0.0684(18) Uani 1 1 d . . . H20 H -0.2807 0.0170 0.2543 0.082 Uiso 1 1 calc R . . C21 C -0.2601(5) 0.1560(4) 0.2495(2) 0.0503(14) Uani 1 1 d . . . H21 H -0.3048 0.1613 0.2074 0.060 Uiso 1 1 calc R . . C22 C -0.2114(4) 0.2365(3) 0.2802(2) 0.0359(10) Uani 1 1 d . . . H22 H -0.2219 0.2956 0.2593 0.043 Uiso 1 1 calc R . . C23 C -0.1333(3) 0.4332(3) 0.33865(17) 0.0264(8) Uani 1 1 d . . . C24 C -0.2485(3) 0.4633(3) 0.33004(18) 0.0283(9) Uani 1 1 d . . . H24 H -0.2991 0.4307 0.3504 0.034 Uiso 1 1 calc R . . C25 C -0.2888(4) 0.5396(3) 0.2923(2) 0.0419(11) Uani 1 1 d . . . H25 H -0.3673 0.5586 0.2863 0.050 Uiso 1 1 calc R . . C26 C -0.2164(5) 0.5884(4) 0.2635(2) 0.0534(14) Uani 1 1 d . . . H26 H -0.2449 0.6416 0.2383 0.064 Uiso 1 1 calc R . . C27 C -0.1012(5) 0.5605(4) 0.2708(2) 0.0530(14) Uani 1 1 d . . . H27 H -0.0511 0.5944 0.2508 0.064 Uiso 1 1 calc R . . C28 C -0.0613(4) 0.4828(3) 0.30782(19) 0.0366(10) Uani 1 1 d . . . H28 H 0.0165 0.4628 0.3124 0.044 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 Pt1 0.01269(8) 0.04252(10) 0.02597(9) -0.01294(7) 0.00294(6) -0.00157(7) P1 0.0137(5) 0.0312(5) 0.0244(5) -0.0066(4) 0.0019(4) -0.0023(4) N1 0.0148(16) 0.0304(18) 0.0253(17) -0.0071(14) 0.0027(13) -0.0029(13) N2 0.0094(15) 0.046(2) 0.045(2) -0.0216(17) 0.0041(14) -0.0035(15) C29 0.029(3) 0.097(4) 0.039(3) -0.036(3) 0.009(2) -0.003(3) C1 0.0131(18) 0.033(2) 0.030(2) 0.0030(16) 0.0050(15) 0.0049(16) C2 0.0134(19) 0.052(3) 0.035(2) 0.009(2) 0.0000(17) -0.0004(18) C3 0.017(2) 0.063(3) 0.048(3) 0.013(2) 0.010(2) 0.001(2) C4 0.029(3) 0.074(4) 0.046(3) 0.007(2) 0.020(2) 0.006(2) C5 0.0134(19) 0.046(2) 0.038(2) 0.006(2) 0.0170(17) 0.0062(18) C6 0.019(2) 0.032(2) 0.028(2) 0.0010(17) 0.0058(16) -0.0015(17) C7 0.021(2) 0.032(2) 0.025(2) -0.0065(16) 0.0053(16) -0.0007(16) C8 0.016(2) 0.050(3) 0.024(2) -0.0114(18) -0.0017(16) -0.0085(18) C9 0.018(2) 0.043(2) 0.035(2) -0.0049(19) 0.0019(17) -0.0053(18) O1 0.0161(15) 0.080(2) 0.0409(19) -0.0087(17) -0.0022(13) -0.0072(16) C10 0.010(2) 0.080(4) 0.048(3) -0.032(3) 0.0028(19) -0.002(2) C11 0.026(3) 0.083(4) 0.095(5) -0.047(4) 0.012(3) -0.002(3) C12 0.034(3) 0.130(7) 0.116(7) -0.082(6) 0.012(4) 0.003(4) C13 0.024(3) 0.168(8) 0.079(5) -0.078(5) 0.007(3) -0.004(4) C14 0.017(2) 0.157(7) 0.050(3) -0.049(4) 0.010(2) -0.015(3) C15 0.018(2) 0.100(4) 0.034(3) -0.031(3) 0.0042(19) -0.006(3) C16 0.028(3) 0.109(5) 0.035(3) 0.000(3) 0.005(2) -0.019(3) O2 0.051(2) 0.115(3) 0.0320(19) 0.002(2) 0.0076(17) -0.025(2) C17 0.026(2) 0.035(2) 0.037(2) -0.0057(19) -0.0028(18) 0.0019(18) C18 0.124(6) 0.034(3) 0.070(4) -0.005(3) -0.050(4) -0.009(3) C19 0.148(8) 0.040(3) 0.095(5) 0.004(3) -0.060(5) -0.024(4) C20 0.071(4) 0.050(3) 0.069(4) -0.022(3) -0.014(3) -0.018(3) C21 0.050(3) 0.055(3) 0.039(3) -0.017(2) -0.002(2) -0.011(2) C22 0.034(3) 0.044(3) 0.027(2) -0.0070(19) 0.0017(19) -0.004(2) C23 0.023(2) 0.035(2) 0.0182(18) -0.0048(16) -0.0005(15) -0.0037(17) C24 0.021(2) 0.039(2) 0.0229(19) -0.0003(17) 0.0012(16) -0.0012(17) C25 0.035(3) 0.049(3) 0.040(3) 0.014(2) 0.006(2) 0.003(2) C26 0.047(3) 0.061(3) 0.045(3) 0.027(3) -0.003(2) -0.005(3) C27 0.043(3) 0.073(4) 0.040(3) 0.022(3) 0.005(2) -0.015(3) C28 0.027(2) 0.054(3) 0.029(2) -0.002(2) 0.0064(18) -0.011(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 Pt1 C29 2.052(4) . ? Pt1 N1 2.061(3) . ? Pt1 N2 2.075(3) . ? Pt1 P1 2.1842(10) . ? P1 C23 1.822(4) . ? P1 C17 1.823(4) . ? P1 C1 1.826(4) . ? N1 C7 1.274(5) . ? N1 C8 1.480(5) . ? N2 C9 1.321(5) . ? N2 C10 1.424(5) . ? C1 C2 1.398(5) . ? C1 C6 1.422(5) . ? C2 C3 1.391(6) . ? C3 C4 1.373(7) . ? C4 C5 1.416(6) . ? C5 C6 1.414(5) . ? C6 C7 1.462(5) . ? C8 C9 1.516(6) . ? C9 O1 1.260(5) . ? C10 C11 1.391(8) . ? C10 C15 1.401(8) . ? C11 C12 1.394(9) . ? C12 C13 1.369(11) . ? C13 C14 1.408(10) . ? C14 C15 1.392(7) . ? C15 C16 1.502(8) . ? C16 O2 1.422(6) . ? C17 C18 1.372(7) . ? C17 C22 1.379(6) . ? C18 C19 1.381(8) . ? C19 C20 1.361(8) . ? C20 C21 1.329(8) . ? C21 C22 1.381(6) . ? C23 C28 1.399(6) . ? C23 C24 1.403(5) . ? C24 C25 1.377(6) . ? C25 C26 1.368(7) . ? C26 C27 1.397(7) . ? C27 C28 1.383(7) . ? 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 C29 Pt1 N1 173.98(16) . . ? C29 Pt1 N2 92.97(17) . . ? N1 Pt1 N2 81.04(13) . . ? C29 Pt1 P1 90.54(14) . . ? N1 Pt1 P1 95.45(9) . . ? N2 Pt1 P1 176.45(10) . . ? C23 P1 C17 104.24(19) . . ? C23 P1 C1 105.60(18) . . ? C17 P1 C1 103.7(2) . . ? C23 P1 Pt1 113.77(14) . . ? C17 P1 Pt1 117.03(15) . . ? C1 P1 Pt1 111.41(13) . . ? C7 N1 C8 117.2(3) . . ? C7 N1 Pt1 130.5(3) . . ? C8 N1 Pt1 112.2(2) . . ? C9 N2 C10 120.7(4) . . ? C9 N2 Pt1 116.2(3) . . ? C10 N2 Pt1 123.1(3) . . ? C2 C1 C6 118.6(4) . . ? C2 C1 P1 118.1(3) . . ? C6 C1 P1 123.2(3) . . ? C3 C2 C1 121.8(4) . . ? C4 C3 C2 119.5(4) . . ? C3 C4 C5 121.5(4) . . ? C6 C5 C4 118.6(4) . . ? C5 C6 C1 119.9(4) . . ? C5 C6 C7 112.5(4) . . ? C1 C6 C7 127.5(4) . . ? N1 C7 C6 128.4(4) . . ? N1 C8 C9 112.2(3) . . ? O1 C9 N2 125.9(4) . . ? O1 C9 C8 117.5(4) . . ? N2 C9 C8 116.5(4) . . ? C11 C10 C15 121.9(5) . . ? C11 C10 N2 119.1(5) . . ? C15 C10 N2 118.7(5) . . ? C10 C11 C12 119.1(7) . . ? C13 C12 C11 119.4(7) . . ? C12 C13 C14 121.9(6) . . ? C15 C14 C13 119.2(7) . . ? C14 C15 C10 118.3(6) . . ? C14 C15 C16 122.2(6) . . ? C10 C15 C16 119.5(4) . . ? O2 C16 C15 112.9(5) . . ? C18 C17 C22 118.2(4) . . ? C18 C17 P1 117.8(4) . . ? C22 C17 P1 123.9(3) . . ? C17 C18 C19 119.8(6) . . ? C20 C19 C18 121.7(6) . . ? C21 C20 C19 118.0(5) . . ? C20 C21 C22 122.4(5) . . ? C17 C22 C21 119.8(4) . . ? C28 C23 C24 118.1(4) . . ? C28 C23 P1 119.2(3) . . ? C24 C23 P1 122.7(3) . . ? C25 C24 C23 120.6(4) . . ? C26 C25 C24 120.5(5) . . ? C25 C26 C27 120.7(5) . . ? C28 C27 C26 118.9(4) . . ? C27 C28 C23 121.3(4) . . ? 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 C29 Pt1 P1 C23 -79.6(2) . . . . ? N1 Pt1 P1 C23 101.04(17) . . . . ? C29 Pt1 P1 C17 42.2(3) . . . . ? N1 Pt1 P1 C17 -137.2(2) . . . . ? C29 Pt1 P1 C1 161.2(2) . . . . ? N1 Pt1 P1 C1 -18.19(16) . . . . ? N2 Pt1 N1 C7 -167.3(4) . . . . ? P1 Pt1 N1 C7 12.2(4) . . . . ? N2 Pt1 N1 C8 10.0(3) . . . . ? P1 Pt1 N1 C8 -170.5(3) . . . . ? C29 Pt1 N2 C9 177.5(4) . . . . ? N1 Pt1 N2 C9 -3.0(3) . . . . ? C29 Pt1 N2 C10 0.8(4) . . . . ? N1 Pt1 N2 C10 -179.8(4) . . . . ? C23 P1 C1 C2 73.4(3) . . . . ? C17 P1 C1 C2 -35.9(4) . . . . ? Pt1 P1 C1 C2 -162.6(3) . . . . ? C23 P1 C1 C6 -104.1(3) . . . . ? C17 P1 C1 C6 146.6(3) . . . . ? Pt1 P1 C1 C6 19.9(4) . . . . ? C6 C1 C2 C3 0.8(6) . . . . ? P1 C1 C2 C3 -176.8(3) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C3 C4 C5 C6 -0.5(7) . . . . ? C4 C5 C6 C1 0.9(6) . . . . ? C4 C5 C6 C7 -175.7(4) . . . . ? C2 C1 C6 C5 -1.0(6) . . . . ? P1 C1 C6 C5 176.4(3) . . . . ? C2 C1 C6 C7 175.0(4) . . . . ? P1 C1 C6 C7 -7.5(6) . . . . ? C8 N1 C7 C6 -177.7(4) . . . . ? Pt1 N1 C7 C6 -0.5(6) . . . . ? C5 C6 C7 N1 171.6(4) . . . . ? C1 C6 C7 N1 -4.7(7) . . . . ? C7 N1 C8 C9 162.7(4) . . . . ? Pt1 N1 C8 C9 -14.9(4) . . . . ? C10 N2 C9 O1 -3.1(8) . . . . ? Pt1 N2 C9 O1 -180.0(4) . . . . ? C10 N2 C9 C8 172.2(4) . . . . ? Pt1 N2 C9 C8 -4.7(5) . . . . ? N1 C8 C9 O1 -171.2(4) . . . . ? N1 C8 C9 N2 13.1(6) . . . . ? C9 N2 C10 C11 102.9(5) . . . . ? Pt1 N2 C10 C11 -80.5(6) . . . . ? C9 N2 C10 C15 -82.7(6) . . . . ? Pt1 N2 C10 C15 93.9(4) . . . . ? C15 C10 C11 C12 -1.2(8) . . . . ? N2 C10 C11 C12 172.9(5) . . . . ? C10 C11 C12 C13 -0.4(10) . . . . ? C11 C12 C13 C14 0.4(10) . . . . ? C12 C13 C14 C15 1.0(9) . . . . ? C13 C14 C15 C10 -2.6(7) . . . . ? C13 C14 C15 C16 178.4(5) . . . . ? C11 C10 C15 C14 2.7(7) . . . . ? N2 C10 C15 C14 -171.5(4) . . . . ? C11 C10 C15 C16 -178.3(5) . . . . ? N2 C10 C15 C16 7.5(6) . . . . ? C14 C15 C16 O2 -13.1(7) . . . . ? C10 C15 C16 O2 167.9(4) . . . . ? C23 P1 C17 C18 -171.7(5) . . . . ? C1 P1 C17 C18 -61.4(5) . . . . ? Pt1 P1 C17 C18 61.7(5) . . . . ? C23 P1 C17 C22 11.3(5) . . . . ? C1 P1 C17 C22 121.6(4) . . . . ? Pt1 P1 C17 C22 -115.4(4) . . . . ? C22 C17 C18 C19 -0.8(11) . . . . ? P1 C17 C18 C19 -178.0(7) . . . . ? C17 C18 C19 C20 0.1(14) . . . . ? C18 C19 C20 C21 0.2(13) . . . . ? C19 C20 C21 C22 0.2(11) . . . . ? C18 C17 C22 C21 1.2(8) . . . . ? P1 C17 C22 C21 178.2(4) . . . . ? C20 C21 C22 C17 -0.9(9) . . . . ? C17 P1 C23 C28 -108.9(3) . . . . ? C1 P1 C23 C28 142.2(3) . . . . ? Pt1 P1 C23 C28 19.7(4) . . . . ? C17 P1 C23 C24 69.5(4) . . . . ? C1 P1 C23 C24 -39.4(4) . . . . ? Pt1 P1 C23 C24 -161.9(3) . . . . ? C28 C23 C24 C25 -0.1(6) . . . . ? P1 C23 C24 C25 -178.6(3) . . . . ? C23 C24 C25 C26 -1.1(7) . . . . ? C24 C25 C26 C27 1.2(8) . . . . ? C25 C26 C27 C28 -0.1(8) . . . . ? C26 C27 C28 C23 -1.2(8) . . . . ? C24 C23 C28 C27 1.3(6) . . . . ? P1 C23 C28 C27 179.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 2.17 2.758(5) 126.6 3_666 _diffrn_measured_fraction_theta_max 0.911 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.949 _refine_diff_density_min -2.115 _refine_diff_density_rms 0.131 #===END data_8d _database_code_depnum_ccdc_archive 'CCDC 771451' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H29 N2 O2 P Pt, 2(C7 H8)' _chemical_formula_sum 'C44 H45 N2 O2 P Pt' _chemical_formula_weight 859.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 14.8590(8) _cell_length_b 15.6070(8) _cell_length_c 16.2867(9) _cell_angle_alpha 90.00 _cell_angle_beta 95.8849(9) _cell_angle_gamma 90.00 _cell_volume 3757.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10344 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 3.817 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.366 _exptl_absorpt_correction_T_max 0.617 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 29318 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 29.05 _reflns_number_total 9048 _reflns_number_gt 6720 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0188P)^2^+5.8336P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9048 _refine_ls_number_parameters 523 _refine_ls_number_restraints 321 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0653 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.524063(9) 0.335864(9) 0.842356(9) 0.02175(5) Uani 1 1 d . . . P1 P 0.65992(6) 0.28835(6) 0.88312(6) 0.0215(2) Uani 1 1 d . . . N1 N 0.4566(2) 0.2376(2) 0.8964(2) 0.0268(7) Uani 1 1 d . . . N2 N 0.3917(2) 0.3713(2) 0.8062(2) 0.0274(7) Uani 1 1 d . . . C1 C 0.6589(3) 0.2082(2) 0.9650(2) 0.0235(8) Uani 1 1 d . . . C2 C 0.7391(3) 0.1900(3) 1.0134(3) 0.0320(10) Uani 1 1 d . . . H2A H 0.7922 0.2213 1.0046 0.038 Uiso 1 1 calc R . . C3 C 0.7439(3) 0.1273(3) 1.0743(3) 0.0379(10) Uani 1 1 d . . . H3 H 0.7994 0.1166 1.1070 0.045 Uiso 1 1 calc R . . C4 C 0.6679(3) 0.0808(3) 1.0871(3) 0.0388(11) Uani 1 1 d . . . H4 H 0.6709 0.0375 1.1283 0.047 Uiso 1 1 calc R . . C5 C 0.5875(3) 0.0972(2) 1.0399(3) 0.0331(10) Uani 1 1 d . . . H5 H 0.5356 0.0642 1.0484 0.040 Uiso 1 1 calc R . . C6 C 0.5804(3) 0.1615(2) 0.9795(2) 0.0256(8) Uani 1 1 d . . . C7 C 0.4876(3) 0.1750(2) 0.9410(2) 0.0299(9) Uani 1 1 d . . . H7 H 0.4453 0.1314 0.9506 0.036 Uiso 1 1 calc R . . C8 C 0.3563(3) 0.2384(3) 0.8720(3) 0.0345(10) Uani 1 1 d . . . H8 H 0.3348 0.1784 0.8607 0.041 Uiso 1 1 calc R . . C9 C 0.3079(3) 0.2758(3) 0.9412(3) 0.0456(12) Uani 1 1 d . . . H9A H 0.3248 0.3362 0.9490 0.068 Uiso 1 1 calc R . . H9B H 0.3253 0.2441 0.9923 0.068 Uiso 1 1 calc R . . H9C H 0.2424 0.2713 0.9270 0.068 Uiso 1 1 calc R . . C10 C 0.3400(3) 0.2911(3) 0.7935(3) 0.0363(10) Uani 1 1 d . . . H10A H 0.3603 0.2589 0.7463 0.044 Uiso 1 1 calc R . . H10B H 0.2747 0.3038 0.7814 0.044 Uiso 1 1 calc R . . C11 C 0.3461(3) 0.4441(3) 0.7990(2) 0.0274(9) Uani 1 1 d . . . O1 O 0.26366(18) 0.4484(2) 0.76869(18) 0.0388(7) Uani 1 1 d . . . C12 C 0.3903(3) 0.5260(2) 0.8275(2) 0.0255(8) Uani 1 1 d . . . C13 C 0.3532(3) 0.6038(3) 0.7957(3) 0.0336(10) Uani 1 1 d . . . O2 O 0.2786(2) 0.6056(2) 0.7410(2) 0.0504(10) Uani 1 1 d . . . H2 H 0.261(4) 0.558(4) 0.747(4) 0.076 Uiso 1 1 d . . . C14 C 0.3933(3) 0.6817(3) 0.8205(3) 0.0391(11) Uani 1 1 d . . . H14 H 0.3700 0.7338 0.7966 0.047 Uiso 1 1 calc R . . C15 C 0.4665(3) 0.6832(3) 0.8796(3) 0.0359(10) Uani 1 1 d . . . H15 H 0.4944 0.7362 0.8955 0.043 Uiso 1 1 calc R . . C16 C 0.4994(3) 0.6081(3) 0.9160(3) 0.0304(9) Uani 1 1 d . . . H16 H 0.5483 0.6095 0.9584 0.036 Uiso 1 1 calc R . . C17 C 0.4609(3) 0.5307(3) 0.8904(2) 0.0270(9) Uani 1 1 d . . . H17 H 0.4833 0.4793 0.9163 0.032 Uiso 1 1 calc R . . C18 C 0.7392(2) 0.3695(2) 0.9264(2) 0.0232(8) Uani 1 1 d . . . C19 C 0.7289(3) 0.4038(3) 1.0040(3) 0.0325(10) Uani 1 1 d . . . H19 H 0.6841 0.3814 1.0358 0.039 Uiso 1 1 calc R . . C20 C 0.7838(3) 0.4703(3) 1.0345(3) 0.0392(11) Uani 1 1 d . . . H20 H 0.7766 0.4934 1.0874 0.047 Uiso 1 1 calc R . . C21 C 0.8486(3) 0.5035(3) 0.9893(3) 0.0357(10) Uani 1 1 d . . . H21 H 0.8865 0.5488 1.0111 0.043 Uiso 1 1 calc R . . C22 C 0.8581(3) 0.4709(3) 0.9125(3) 0.0368(10) Uani 1 1 d . . . H22 H 0.9024 0.4944 0.8808 0.044 Uiso 1 1 calc R . . C23 C 0.8040(3) 0.4041(2) 0.8807(2) 0.0285(9) Uani 1 1 d . . . H23 H 0.8114 0.3819 0.8275 0.034 Uiso 1 1 calc R . . C24 C 0.7167(2) 0.2342(2) 0.8031(2) 0.0233(8) Uani 1 1 d . . . C25 C 0.8025(3) 0.1979(3) 0.8182(3) 0.0319(9) Uani 1 1 d . . . H25 H 0.8353 0.2030 0.8711 0.038 Uiso 1 1 calc R . . C26 C 0.8398(3) 0.1545(3) 0.7560(3) 0.0373(10) Uani 1 1 d . . . H26 H 0.8983 0.1299 0.7665 0.045 Uiso 1 1 calc R . . C27 C 0.7929(3) 0.1465(3) 0.6787(3) 0.0380(11) Uani 1 1 d . . . H27 H 0.8187 0.1159 0.6364 0.046 Uiso 1 1 calc R . . C28 C 0.7084(3) 0.1832(3) 0.6629(3) 0.0369(10) Uani 1 1 d . . . H28 H 0.6762 0.1785 0.6096 0.044 Uiso 1 1 calc R . . C29 C 0.6709(3) 0.2268(2) 0.7249(3) 0.0307(9) Uani 1 1 d . . . H29 H 0.6129 0.2522 0.7137 0.037 Uiso 1 1 calc R . . C30 C 0.5806(3) 0.4298(2) 0.7749(3) 0.0295(9) Uani 1 1 d . . . H30A H 0.5329 0.4581 0.7386 0.044 Uiso 1 1 calc R . . H30B H 0.6246 0.4038 0.7415 0.044 Uiso 1 1 calc R . . H30C H 0.6111 0.4721 0.8125 0.044 Uiso 1 1 calc R . . C31 C 0.5649(4) 0.3647(4) 0.4688(4) 0.0688(17) Uani 1 1 d D . . C32 C 0.5508(3) 0.2911(4) 0.4210(3) 0.0627(16) Uani 1 1 d D . . H32 H 0.5704 0.2883 0.3673 0.075 Uiso 1 1 calc R . . C33 C 0.5084(4) 0.2235(4) 0.4526(4) 0.0697(18) Uani 1 1 d D . . H33 H 0.4994 0.1732 0.4198 0.084 Uiso 1 1 calc R . . C34 C 0.4774(4) 0.2238(5) 0.5308(5) 0.093(3) Uani 1 1 d D . . H34 H 0.4488 0.1751 0.5517 0.112 Uiso 1 1 calc R . . C35 C 0.4906(4) 0.2980(6) 0.5759(4) 0.098(3) Uani 1 1 d D . . H35 H 0.4684 0.3016 0.6285 0.117 Uiso 1 1 calc R . . C36 C 0.5348(4) 0.3665(4) 0.5468(3) 0.074(2) Uani 1 1 d D . . H36 H 0.5451 0.4160 0.5803 0.089 Uiso 1 1 calc R . . C37 C 0.6135(5) 0.4360(5) 0.4362(5) 0.113(3) Uani 1 1 d D . . H37A H 0.6178 0.4832 0.4761 0.169 Uiso 1 1 calc R . . H37B H 0.5809 0.4555 0.3841 0.169 Uiso 1 1 calc R . . H37C H 0.6744 0.4173 0.4263 0.169 Uiso 1 1 calc R . . C38 C -0.1045(6) 0.4404(5) 0.6856(8) 0.0457(17) Uani 0.524(6) 1 d PDU A 1 C39 C -0.0353(7) 0.3893(6) 0.7229(8) 0.0505(18) Uani 0.524(6) 1 d PDU A 1 H39 H -0.0402 0.3287 0.7190 0.061 Uiso 0.524(6) 1 calc PR A 1 C40 C 0.0395(11) 0.4252(7) 0.7650(17) 0.056(2) Uani 0.524(6) 1 d PDU A 1 H40 H 0.0844 0.3894 0.7930 0.067 Uiso 0.524(6) 1 calc PR A 1 C41 C 0.0506(6) 0.5137(6) 0.7674(6) 0.0517(19) Uani 0.524(6) 1 d PDU A 1 H41 H 0.1049 0.5388 0.7924 0.062 Uiso 0.524(6) 1 calc PR A 1 C42 C -0.0198(5) 0.5643(5) 0.7322(6) 0.0474(18) Uani 0.524(6) 1 d PDU A 1 H42 H -0.0142 0.6249 0.7351 0.057 Uiso 0.524(6) 1 calc PR A 1 C43 C -0.0973(6) 0.5290(5) 0.6932(8) 0.0418(19) Uani 0.524(6) 1 d PDU A 1 H43 H -0.1458 0.5648 0.6715 0.050 Uiso 0.524(6) 1 calc PR A 1 C44 C -0.1856(6) 0.4016(7) 0.6416(6) 0.063(3) Uani 0.524(6) 1 d PDU A 1 H44A H -0.1842 0.4092 0.5820 0.095 Uiso 0.524(6) 1 calc PR A 1 H44B H -0.2397 0.4293 0.6590 0.095 Uiso 0.524(6) 1 calc PR A 1 H44C H -0.1870 0.3403 0.6544 0.095 Uiso 0.524(6) 1 calc PR A 1 C38X C -0.1261(6) 0.4599(5) 0.6703(9) 0.0435(18) Uani 0.476(6) 1 d PDU A 2 C39X C -0.0953(6) 0.3776(5) 0.6916(6) 0.0428(18) Uani 0.476(6) 1 d PDU A 2 H39X H -0.1310 0.3291 0.6743 0.051 Uiso 0.476(6) 1 calc PR A 2 C40X C -0.0136(7) 0.3667(6) 0.7376(9) 0.050(2) Uani 0.476(6) 1 d PDU A 2 H40X H 0.0042 0.3107 0.7554 0.060 Uiso 0.476(6) 1 calc PR A 2 C41X C 0.0438(13) 0.4348(7) 0.7590(19) 0.056(2) Uani 0.476(6) 1 d PDU A 2 H41X H 0.1026 0.4259 0.7865 0.067 Uiso 0.476(6) 1 calc PR A 2 C42X C 0.0123(7) 0.5167(8) 0.7389(7) 0.0576(19) Uani 0.476(6) 1 d PDU A 2 H42X H 0.0472 0.5651 0.7578 0.069 Uiso 0.476(6) 1 calc PR A 2 C43X C -0.0688(7) 0.5281(6) 0.6918(9) 0.047(2) Uani 0.476(6) 1 d PDU A 2 H43X H -0.0861 0.5841 0.6736 0.056 Uiso 0.476(6) 1 calc PR A 2 C44X C -0.2151(6) 0.4726(8) 0.6233(7) 0.068(3) Uani 0.476(6) 1 d PDU A 2 H44D H -0.2564 0.4994 0.6589 0.103 Uiso 0.476(6) 1 calc PR A 2 H44E H -0.2397 0.4171 0.6038 0.103 Uiso 0.476(6) 1 calc PR A 2 H44F H -0.2085 0.5099 0.5758 0.103 Uiso 0.476(6) 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 0.02032(7) 0.02122(7) 0.02363(8) -0.00160(7) 0.00193(5) 0.00052(7) P1 0.0221(5) 0.0209(5) 0.0219(5) -0.0015(4) 0.0035(4) 0.0009(4) N1 0.0263(17) 0.0261(17) 0.0280(19) -0.0045(15) 0.0018(15) -0.0047(14) N2 0.0250(17) 0.0265(16) 0.0294(19) -0.0023(15) -0.0030(15) 0.0006(14) C1 0.031(2) 0.0194(18) 0.021(2) -0.0024(16) 0.0031(16) 0.0014(16) C2 0.032(2) 0.035(2) 0.028(2) -0.0005(18) 0.0008(18) -0.0004(17) C3 0.041(3) 0.040(2) 0.031(3) 0.003(2) -0.003(2) 0.007(2) C4 0.052(3) 0.036(2) 0.028(2) 0.007(2) 0.003(2) 0.004(2) C5 0.042(3) 0.026(2) 0.032(2) 0.0014(18) 0.010(2) -0.0051(18) C6 0.033(2) 0.0209(18) 0.023(2) -0.0032(17) 0.0034(16) -0.0031(17) C7 0.032(2) 0.027(2) 0.032(2) -0.0035(18) 0.0076(18) -0.0065(17) C8 0.025(2) 0.036(2) 0.041(3) -0.001(2) -0.0054(19) -0.0083(18) C9 0.029(2) 0.061(3) 0.048(3) -0.002(3) 0.006(2) -0.005(2) C10 0.032(2) 0.036(2) 0.039(3) -0.008(2) -0.003(2) -0.0010(19) C11 0.024(2) 0.038(2) 0.020(2) -0.0060(17) 0.0016(16) 0.0017(17) O1 0.0251(15) 0.0495(18) 0.0389(18) -0.0094(15) -0.0113(13) 0.0085(13) C12 0.028(2) 0.029(2) 0.020(2) -0.0017(16) 0.0040(16) 0.0080(16) C13 0.035(2) 0.040(2) 0.025(2) 0.0011(19) 0.0050(19) 0.0182(19) O2 0.051(2) 0.051(2) 0.046(2) 0.0049(18) -0.0145(17) 0.0206(17) C14 0.057(3) 0.032(2) 0.029(2) 0.0037(19) 0.006(2) 0.013(2) C15 0.046(3) 0.028(2) 0.036(3) -0.0032(18) 0.018(2) -0.0004(18) C16 0.029(2) 0.036(2) 0.027(2) -0.0054(18) 0.0058(18) -0.0029(18) C17 0.028(2) 0.031(2) 0.022(2) -0.0019(17) 0.0042(17) 0.0031(16) C18 0.0207(18) 0.0255(18) 0.023(2) -0.0004(16) 0.0014(16) 0.0026(15) C19 0.028(2) 0.037(2) 0.034(3) -0.0063(19) 0.0093(18) -0.0069(18) C20 0.044(3) 0.042(3) 0.033(3) -0.018(2) 0.011(2) -0.008(2) C21 0.032(2) 0.036(2) 0.040(3) -0.008(2) 0.005(2) -0.0108(19) C22 0.038(2) 0.035(2) 0.038(3) 0.002(2) 0.010(2) -0.0092(19) C23 0.035(2) 0.028(2) 0.024(2) -0.0032(17) 0.0084(18) -0.0014(17) C24 0.025(2) 0.0213(19) 0.025(2) -0.0013(16) 0.0068(17) -0.0017(15) C25 0.029(2) 0.035(2) 0.031(2) -0.0031(19) 0.0026(18) 0.0013(18) C26 0.029(2) 0.039(2) 0.045(3) -0.007(2) 0.011(2) 0.0065(19) C27 0.044(3) 0.035(3) 0.038(3) -0.011(2) 0.018(2) 0.0008(19) C28 0.041(2) 0.041(3) 0.029(2) -0.0104(19) 0.005(2) 0.002(2) C29 0.032(2) 0.031(2) 0.029(2) -0.0038(18) -0.0004(18) 0.0054(18) C30 0.028(2) 0.028(2) 0.032(2) 0.0038(18) 0.0047(18) 0.0026(17) C31 0.044(3) 0.073(4) 0.086(5) 0.002(4) -0.006(3) 0.009(3) C32 0.044(3) 0.081(4) 0.060(4) -0.024(3) -0.009(3) 0.019(3) C33 0.049(4) 0.085(5) 0.072(5) -0.010(4) -0.011(3) 0.019(3) C34 0.045(4) 0.104(6) 0.123(7) -0.010(5) -0.026(4) 0.027(4) C35 0.048(4) 0.172(9) 0.071(5) 0.042(6) -0.008(4) 0.028(5) C36 0.054(4) 0.112(6) 0.053(4) -0.041(4) -0.011(3) 0.025(4) C37 0.125(7) 0.121(7) 0.096(6) 0.007(5) 0.029(5) 0.013(6) C38 0.049(4) 0.054(3) 0.038(4) 0.006(4) 0.020(3) 0.009(3) C39 0.054(4) 0.056(4) 0.045(4) 0.006(4) 0.025(3) 0.018(3) C40 0.050(4) 0.069(3) 0.051(4) 0.013(4) 0.022(3) 0.015(3) C41 0.040(4) 0.069(4) 0.049(5) 0.012(4) 0.019(3) 0.013(3) C42 0.044(4) 0.056(4) 0.044(4) 0.012(4) 0.018(3) 0.007(3) C43 0.041(4) 0.049(3) 0.040(4) 0.015(3) 0.025(4) 0.007(3) C44 0.065(5) 0.079(6) 0.048(6) 0.001(5) 0.013(4) -0.010(5) C38X 0.045(4) 0.051(4) 0.039(4) 0.011(4) 0.026(3) 0.012(3) C39X 0.048(4) 0.048(3) 0.036(4) 0.011(4) 0.021(3) 0.011(3) C40X 0.049(4) 0.063(4) 0.041(5) 0.005(4) 0.017(3) 0.018(3) C41X 0.047(4) 0.074(4) 0.050(5) 0.007(4) 0.020(4) 0.012(3) C42X 0.055(4) 0.069(4) 0.052(4) 0.009(4) 0.023(3) 0.005(4) C43X 0.053(4) 0.048(3) 0.044(4) 0.010(3) 0.029(4) 0.008(3) C44X 0.053(5) 0.096(8) 0.058(7) 0.036(6) 0.011(4) 0.013(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 C30 2.061(4) . ? Pt1 N2 2.070(3) . ? Pt1 N1 2.077(3) . ? Pt1 P1 2.1889(10) . ? P1 C18 1.821(4) . ? P1 C24 1.830(4) . ? P1 C1 1.831(4) . ? N1 C7 1.275(5) . ? N1 C8 1.502(5) . ? N2 C11 1.321(5) . ? N2 C10 1.472(5) . ? C1 C2 1.389(5) . ? C1 C6 1.415(5) . ? C2 C3 1.390(6) . ? C3 C4 1.376(6) . ? C4 C5 1.377(6) . ? C5 C6 1.401(5) . ? C6 C7 1.470(5) . ? C8 C9 1.514(6) . ? C8 C10 1.518(6) . ? C11 O1 1.275(4) . ? C11 C12 1.490(5) . ? C12 C17 1.391(5) . ? C12 C13 1.409(5) . ? C13 O2 1.350(5) . ? C13 C14 1.396(6) . ? C14 C15 1.377(6) . ? C15 C16 1.381(6) . ? C16 C17 1.383(5) . ? C18 C23 1.386(5) . ? C18 C19 1.395(5) . ? C19 C20 1.381(5) . ? C20 C21 1.372(6) . ? C21 C22 1.371(6) . ? C22 C23 1.384(5) . ? C24 C29 1.386(5) . ? C24 C25 1.393(5) . ? C25 C26 1.381(6) . ? C26 C27 1.381(6) . ? C27 C28 1.379(6) . ? C28 C29 1.381(5) . ? C31 C32 1.390(6) . ? C31 C36 1.391(6) . ? C31 C37 1.456(7) . ? C32 C33 1.358(6) . ? C33 C34 1.398(6) . ? C34 C35 1.375(7) . ? C35 C36 1.365(7) . ? C38 C39 1.390(7) . ? C38 C43 1.391(7) . ? C38 C44 1.469(8) . ? C39 C40 1.366(8) . ? C40 C41 1.391(8) . ? C41 C42 1.388(8) . ? C42 C43 1.373(7) . ? C38X C43X 1.386(7) . ? C38X C39X 1.395(7) . ? C38X C44X 1.473(8) . ? C39X C40X 1.371(8) . ? C40X C41X 1.385(8) . ? C41X C42X 1.388(8) . ? C42X C43X 1.372(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C30 Pt1 N2 94.90(14) . . ? C30 Pt1 N1 172.59(14) . . ? N2 Pt1 N1 80.31(13) . . ? C30 Pt1 P1 89.38(11) . . ? N2 Pt1 P1 175.43(9) . . ? N1 Pt1 P1 95.27(9) . . ? C18 P1 C24 105.66(17) . . ? C18 P1 C1 104.30(17) . . ? C24 P1 C1 103.99(17) . . ? C18 P1 Pt1 114.91(12) . . ? C24 P1 Pt1 114.76(13) . . ? C1 P1 Pt1 112.10(13) . . ? C7 N1 C8 116.6(3) . . ? C7 N1 Pt1 130.2(3) . . ? C8 N1 Pt1 113.0(2) . . ? C11 N2 C10 117.6(3) . . ? C11 N2 Pt1 135.9(3) . . ? C10 N2 Pt1 106.2(2) . . ? C2 C1 C6 118.4(4) . . ? C2 C1 P1 118.8(3) . . ? C6 C1 P1 122.8(3) . . ? C1 C2 C3 121.7(4) . . ? C4 C3 C2 119.8(4) . . ? C3 C4 C5 119.7(4) . . ? C4 C5 C6 121.6(4) . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 113.7(3) . . ? C1 C6 C7 127.4(4) . . ? N1 C7 C6 128.4(4) . . ? N1 C8 C9 109.9(3) . . ? N1 C8 C10 107.2(3) . . ? C9 C8 C10 111.8(4) . . ? N2 C10 C8 107.9(3) . . ? O1 C11 N2 122.9(4) . . ? O1 C11 C12 116.8(3) . . ? N2 C11 C12 120.3(3) . . ? C17 C12 C13 117.6(4) . . ? C17 C12 C11 123.3(3) . . ? C13 C12 C11 118.8(4) . . ? O2 C13 C14 118.0(4) . . ? O2 C13 C12 121.7(4) . . ? C14 C13 C12 120.3(4) . . ? C15 C14 C13 120.0(4) . . ? C14 C15 C16 120.4(4) . . ? C15 C16 C17 119.7(4) . . ? C16 C17 C12 121.7(4) . . ? C23 C18 C19 118.9(4) . . ? C23 C18 P1 121.4(3) . . ? C19 C18 P1 119.4(3) . . ? C20 C19 C18 119.9(4) . . ? C21 C20 C19 120.8(4) . . ? C22 C21 C20 119.6(4) . . ? C21 C22 C23 120.7(4) . . ? C22 C23 C18 120.1(4) . . ? C29 C24 C25 118.8(4) . . ? C29 C24 P1 118.3(3) . . ? C25 C24 P1 122.9(3) . . ? C26 C25 C24 120.0(4) . . ? C25 C26 C27 120.6(4) . . ? C28 C27 C26 119.8(4) . . ? C27 C28 C29 119.7(4) . . ? C28 C29 C24 121.1(4) . . ? C32 C31 C36 119.0(6) . . ? C32 C31 C37 118.6(6) . . ? C36 C31 C37 122.4(6) . . ? C33 C32 C31 118.6(5) . . ? C32 C33 C34 123.5(6) . . ? C35 C34 C33 116.6(7) . . ? C36 C35 C34 121.4(6) . . ? C35 C36 C31 120.8(6) . . ? C39 C38 C43 119.0(7) . . ? C39 C38 C44 120.6(7) . . ? C43 C38 C44 120.3(7) . . ? C40 C39 C38 120.8(8) . . ? C39 C40 C41 120.6(9) . . ? C42 C41 C40 118.2(9) . . ? C43 C42 C41 121.5(8) . . ? C42 C43 C38 119.6(7) . . ? C43X C38X C39X 117.8(8) . . ? C43X C38X C44X 121.6(7) . . ? C39X C38X C44X 120.5(7) . . ? C40X C39X C38X 120.0(8) . . ? C39X C40X C41X 122.0(9) . . ? C40X C41X C42X 117.6(10) . . ? C43X C42X C41X 120.5(9) . . ? C42X C43X C38X 121.5(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 C30 Pt1 P1 C18 51.37(18) . . . . ? N1 Pt1 P1 C18 -134.41(17) . . . . ? C30 Pt1 P1 C24 -71.44(18) . . . . ? N1 Pt1 P1 C24 102.78(16) . . . . ? C30 Pt1 P1 C1 170.22(17) . . . . ? N1 Pt1 P1 C1 -15.56(16) . . . . ? N2 Pt1 N1 C7 -178.2(4) . . . . ? P1 Pt1 N1 C7 3.0(4) . . . . ? N2 Pt1 N1 C8 7.5(3) . . . . ? P1 Pt1 N1 C8 -171.3(2) . . . . ? C30 Pt1 N2 C11 -45.4(4) . . . . ? N1 Pt1 N2 C11 140.3(4) . . . . ? C30 Pt1 N2 C10 140.8(3) . . . . ? N1 Pt1 N2 C10 -33.5(3) . . . . ? C18 P1 C1 C2 -36.8(3) . . . . ? C24 P1 C1 C2 73.7(3) . . . . ? Pt1 P1 C1 C2 -161.8(3) . . . . ? C18 P1 C1 C6 145.4(3) . . . . ? C24 P1 C1 C6 -104.1(3) . . . . ? Pt1 P1 C1 C6 20.5(3) . . . . ? C6 C1 C2 C3 0.6(6) . . . . ? P1 C1 C2 C3 -177.3(3) . . . . ? C1 C2 C3 C4 0.8(7) . . . . ? C2 C3 C4 C5 -0.6(7) . . . . ? C3 C4 C5 C6 -1.0(7) . . . . ? C4 C5 C6 C1 2.4(6) . . . . ? C4 C5 C6 C7 -174.6(4) . . . . ? C2 C1 C6 C5 -2.2(5) . . . . ? P1 C1 C6 C5 175.6(3) . . . . ? C2 C1 C6 C7 174.4(4) . . . . ? P1 C1 C6 C7 -7.9(6) . . . . ? C8 N1 C7 C6 -174.3(4) . . . . ? Pt1 N1 C7 C6 11.6(6) . . . . ? C5 C6 C7 N1 165.8(4) . . . . ? C1 C6 C7 N1 -10.9(7) . . . . ? C7 N1 C8 C9 82.5(5) . . . . ? Pt1 N1 C8 C9 -102.3(3) . . . . ? C7 N1 C8 C10 -155.8(4) . . . . ? Pt1 N1 C8 C10 19.3(4) . . . . ? C11 N2 C10 C8 -120.9(4) . . . . ? Pt1 N2 C10 C8 54.2(4) . . . . ? N1 C8 C10 N2 -47.9(4) . . . . ? C9 C8 C10 N2 72.5(4) . . . . ? C10 N2 C11 O1 -12.0(6) . . . . ? Pt1 N2 C11 O1 174.7(3) . . . . ? C10 N2 C11 C12 167.4(4) . . . . ? Pt1 N2 C11 C12 -5.8(6) . . . . ? O1 C11 C12 C17 151.8(4) . . . . ? N2 C11 C12 C17 -27.7(6) . . . . ? O1 C11 C12 C13 -21.3(5) . . . . ? N2 C11 C12 C13 159.2(4) . . . . ? C17 C12 C13 O2 -173.0(4) . . . . ? C11 C12 C13 O2 0.6(6) . . . . ? C17 C12 C13 C14 7.0(6) . . . . ? C11 C12 C13 C14 -179.4(4) . . . . ? O2 C13 C14 C15 176.4(4) . . . . ? C12 C13 C14 C15 -3.6(6) . . . . ? C13 C14 C15 C16 -1.4(7) . . . . ? C14 C15 C16 C17 2.6(6) . . . . ? C15 C16 C17 C12 1.1(6) . . . . ? C13 C12 C17 C16 -5.9(6) . . . . ? C11 C12 C17 C16 -179.1(4) . . . . ? C24 P1 C18 C23 25.9(4) . . . . ? C1 P1 C18 C23 135.2(3) . . . . ? Pt1 P1 C18 C23 -101.7(3) . . . . ? C24 P1 C18 C19 -160.5(3) . . . . ? C1 P1 C18 C19 -51.2(3) . . . . ? Pt1 P1 C18 C19 71.9(3) . . . . ? C23 C18 C19 C20 -0.9(6) . . . . ? P1 C18 C19 C20 -174.6(3) . . . . ? C18 C19 C20 C21 0.1(7) . . . . ? C19 C20 C21 C22 0.8(7) . . . . ? C20 C21 C22 C23 -0.9(7) . . . . ? C21 C22 C23 C18 0.2(6) . . . . ? C19 C18 C23 C22 0.8(6) . . . . ? P1 C18 C23 C22 174.4(3) . . . . ? C18 P1 C24 C29 -128.0(3) . . . . ? C1 P1 C24 C29 122.5(3) . . . . ? Pt1 P1 C24 C29 -0.3(3) . . . . ? C18 P1 C24 C25 54.0(4) . . . . ? C1 P1 C24 C25 -55.5(4) . . . . ? Pt1 P1 C24 C25 -178.3(3) . . . . ? C29 C24 C25 C26 -0.9(6) . . . . ? P1 C24 C25 C26 177.0(3) . . . . ? C24 C25 C26 C27 0.0(6) . . . . ? C25 C26 C27 C28 0.9(7) . . . . ? C26 C27 C28 C29 -0.7(7) . . . . ? C27 C28 C29 C24 -0.3(6) . . . . ? C25 C24 C29 C28 1.1(6) . . . . ? P1 C24 C29 C28 -177.0(3) . . . . ? C36 C31 C32 C33 -0.3(8) . . . . ? C37 C31 C32 C33 177.6(6) . . . . ? C31 C32 C33 C34 0.4(8) . . . . ? C32 C33 C34 C35 0.9(9) . . . . ? C33 C34 C35 C36 -2.5(9) . . . . ? C34 C35 C36 C31 2.7(9) . . . . ? C32 C31 C36 C35 -1.2(9) . . . . ? C37 C31 C36 C35 -179.1(6) . . . . ? C43 C38 C39 C40 -1(3) . . . . ? C44 C38 C39 C40 -178.9(19) . . . . ? C38 C39 C40 C41 -4(4) . . . . ? C39 C40 C41 C42 6(3) . . . . ? C40 C41 C42 C43 -2(2) . . . . ? C41 C42 C43 C38 -2.7(18) . . . . ? C39 C38 C43 C42 5(2) . . . . ? C44 C38 C43 C42 -177.9(10) . . . . ? C43X C38X C39X C40X 4.7(19) . . . . ? C44X C38X C39X C40X -177.9(13) . . . . ? C38X C39X C40X C41X -5(3) . . . . ? C39X C40X C41X C42X 6(4) . . . . ? C40X C41X C42X C43X -7(4) . . . . ? C41X C42X C43X C38X 7(3) . . . . ? C39X C38X C43X C42X -6(2) . . . . ? C44X C38X C43X C42X 177.0(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.79(5) 1.75(6) 2.509(5) 160(6) . _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.051 _refine_diff_density_min -1.060 _refine_diff_density_rms 0.125 #===END data_11a _database_code_depnum_ccdc_archive 'CCDC 771452' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H21 N2 O2 P Pt, C1 H4 O1' _chemical_formula_sum 'C28 H25 N2 O3 P Pt' _chemical_formula_weight 663.56 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5258(4) _cell_length_b 9.3993(4) _cell_length_c 15.6457(7) _cell_angle_alpha 91.4448(7) _cell_angle_beta 100.6844(7) _cell_angle_gamma 108.3565(7) _cell_volume 1164.66(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8488 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 28.96 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 648 _exptl_absorpt_coefficient_mu 6.128 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.146 _exptl_absorpt_correction_T_max 0.838 _exptl_absorpt_process_details 'SADABS v2.03, Sheldrick, G.M., (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10164 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.96 _reflns_number_total 5347 _reflns_number_gt 5037 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0250P)^2^+0.7545P] 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 5347 _refine_ls_number_parameters 318 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0582 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Pt1 Pt 0.555857(12) 0.540427(11) 0.677068(7) 0.01550(5) Uani 1 1 d . . . P1 P 0.76827(9) 0.71609(8) 0.76583(5) 0.01567(15) Uani 1 1 d . . . N1 N 0.4918(3) 0.6829(3) 0.59825(17) 0.0192(5) Uani 1 1 d . . . N2 N 0.3664(3) 0.3868(3) 0.59534(17) 0.0176(5) Uani 1 1 d . . . O2 O 0.5742(3) 0.3587(2) 0.73752(15) 0.0218(5) Uani 1 1 d . . . C1 C 0.8234(4) 0.8960(3) 0.7188(2) 0.0185(6) Uani 1 1 d . . . C2 C 0.9725(4) 1.0082(3) 0.7588(2) 0.0229(6) Uani 1 1 d . . . H2 H 1.0447 0.9866 0.8070 0.027 Uiso 1 1 calc R . . C3 C 1.0175(4) 1.1507(3) 0.7296(2) 0.0250(7) Uani 1 1 d . . . H3A H 1.1194 1.2255 0.7579 0.030 Uiso 1 1 calc R . . C4 C 0.9141(5) 1.1840(4) 0.6594(2) 0.0293(7) Uani 1 1 d . . . H4 H 0.9443 1.2816 0.6394 0.035 Uiso 1 1 calc R . . C5 C 0.7671(5) 1.0741(4) 0.6189(2) 0.0271(7) Uani 1 1 d . . . H5 H 0.6959 1.0975 0.5710 0.033 Uiso 1 1 calc R . . C6 C 0.7193(4) 0.9280(3) 0.6466(2) 0.0206(6) Uani 1 1 d . . . C7 C 0.5631(4) 0.8249(4) 0.5934(2) 0.0226(6) Uani 1 1 d . . . H7 H 0.5061 0.8686 0.5490 0.027 Uiso 1 1 calc R . . C8 C 0.3320(4) 0.6080(3) 0.5334(2) 0.0224(6) Uani 1 1 d . . . H8A H 0.3505 0.6334 0.4743 0.027 Uiso 1 1 calc R . . H8B H 0.2436 0.6483 0.5459 0.027 Uiso 1 1 calc R . . C9 C 0.2683(4) 0.4359(3) 0.5341(2) 0.0207(6) Uani 1 1 d . . . O1 O 0.1383(3) 0.3626(3) 0.48292(17) 0.0322(6) Uani 1 1 d . . . C10 C 0.3427(4) 0.2379(3) 0.6182(2) 0.0193(6) Uani 1 1 d . . . C11 C 0.2219(4) 0.1071(4) 0.5736(2) 0.0240(7) Uani 1 1 d . . . H11 H 0.1487 0.1126 0.5210 0.029 Uiso 1 1 calc R . . C12 C 0.2094(4) -0.0316(4) 0.6067(2) 0.0269(7) Uani 1 1 d . . . H12 H 0.1276 -0.1210 0.5767 0.032 Uiso 1 1 calc R . . C13 C 0.3173(4) -0.0387(3) 0.6840(2) 0.0263(7) Uani 1 1 d . . . H13 H 0.3073 -0.1331 0.7067 0.032 Uiso 1 1 calc R . . C14 C 0.4396(4) 0.0909(3) 0.7283(2) 0.0241(7) Uani 1 1 d . . . H14 H 0.5127 0.0845 0.7807 0.029 Uiso 1 1 calc R . . C15 C 0.4542(4) 0.2302(3) 0.6953(2) 0.0196(6) Uani 1 1 d . . . C16 C 0.7288(4) 0.7620(3) 0.8724(2) 0.0182(6) Uani 1 1 d . . . C17 C 0.7058(4) 0.6519(4) 0.9317(2) 0.0231(6) Uani 1 1 d . . . H17 H 0.7140 0.5563 0.9167 0.028 Uiso 1 1 calc R . . C18 C 0.6708(4) 0.6817(4) 1.0128(2) 0.0302(8) Uani 1 1 d . . . H18 H 0.6564 0.6072 1.0532 0.036 Uiso 1 1 calc R . . C19 C 0.6573(4) 0.8213(4) 1.0339(2) 0.0313(8) Uani 1 1 d . . . H19 H 0.6339 0.8421 1.0890 0.038 Uiso 1 1 calc R . . C20 C 0.6775(4) 0.9300(4) 0.9753(3) 0.0309(8) Uani 1 1 d . . . H20 H 0.6675 1.0249 0.9902 0.037 Uiso 1 1 calc R . . C21 C 0.7124(4) 0.9010(4) 0.8948(2) 0.0242(7) Uani 1 1 d . . . H21 H 0.7252 0.9759 0.8546 0.029 Uiso 1 1 calc R . . C22 C 0.9640(4) 0.6727(3) 0.7892(2) 0.0181(6) Uani 1 1 d . . . C23 C 1.0779(4) 0.7165(3) 0.8693(2) 0.0213(6) Uani 1 1 d . . . H23 H 1.0530 0.7702 0.9144 0.026 Uiso 1 1 calc R . . C24 C 1.2277(4) 0.6820(4) 0.8837(2) 0.0244(7) Uani 1 1 d . . . H24 H 1.3040 0.7109 0.9385 0.029 Uiso 1 1 calc R . . C25 C 1.2644(4) 0.6052(4) 0.8173(2) 0.0233(7) Uani 1 1 d . . . H25 H 1.3662 0.5812 0.8266 0.028 Uiso 1 1 calc R . . C26 C 1.1530(4) 0.5634(3) 0.7372(2) 0.0218(6) Uani 1 1 d . . . H26 H 1.1800 0.5123 0.6918 0.026 Uiso 1 1 calc R . . C27 C 1.0024(4) 0.5955(3) 0.7227(2) 0.0183(6) Uani 1 1 d . . . H27 H 0.9261 0.5651 0.6679 0.022 Uiso 1 1 calc R . . C28 C 0.9043(5) 0.3220(4) 0.9012(3) 0.0324(8) Uani 1 1 d . . . H28A H 0.9665 0.4045 0.9466 0.039 Uiso 1 1 calc R . . H28B H 0.9327 0.3515 0.8449 0.039 Uiso 1 1 calc R . . H28C H 0.9352 0.2323 0.9159 0.039 Uiso 1 1 calc R . . O3 O 0.7298(3) 0.2899(3) 0.89567(19) 0.0412(7) Uani 1 1 d . . . H3 H 0.6876 0.3174 0.8487 0.062 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 Pt1 0.01247(7) 0.01689(7) 0.01579(7) 0.00062(4) 0.00039(4) 0.00436(4) P1 0.0132(3) 0.0166(3) 0.0162(4) 0.0015(3) 0.0008(3) 0.0047(3) N1 0.0192(13) 0.0221(12) 0.0186(13) 0.0022(10) 0.0040(10) 0.0097(10) N2 0.0173(12) 0.0204(12) 0.0128(12) 0.0006(10) 0.0005(10) 0.0044(10) O2 0.0194(11) 0.0176(10) 0.0222(12) 0.0019(9) -0.0058(9) 0.0031(8) C1 0.0169(14) 0.0172(13) 0.0208(16) -0.0001(12) 0.0053(12) 0.0041(11) C2 0.0182(15) 0.0237(15) 0.0257(17) 0.0034(13) 0.0024(13) 0.0064(12) C3 0.0216(16) 0.0202(14) 0.0299(19) -0.0008(13) 0.0068(14) 0.0017(12) C4 0.038(2) 0.0196(14) 0.0296(19) 0.0064(13) 0.0097(15) 0.0056(14) C5 0.0330(18) 0.0235(15) 0.0245(17) 0.0057(13) 0.0034(14) 0.0100(14) C6 0.0204(15) 0.0197(14) 0.0213(16) 0.0024(12) 0.0028(12) 0.0068(12) C7 0.0247(16) 0.0252(15) 0.0189(16) 0.0055(13) 0.0011(13) 0.0113(13) C8 0.0216(15) 0.0254(15) 0.0177(15) 0.0043(12) -0.0026(12) 0.0079(12) C9 0.0168(14) 0.0270(15) 0.0159(15) 0.0011(12) -0.0003(12) 0.0059(12) O1 0.0267(13) 0.0307(12) 0.0271(13) 0.0020(10) -0.0093(10) 0.0009(10) C10 0.0164(14) 0.0213(14) 0.0197(16) -0.0018(12) 0.0044(12) 0.0053(11) C11 0.0206(16) 0.0244(15) 0.0240(17) -0.0022(13) 0.0035(13) 0.0038(12) C12 0.0235(16) 0.0196(14) 0.034(2) -0.0053(13) 0.0068(14) 0.0014(12) C13 0.0238(16) 0.0183(14) 0.036(2) 0.0019(13) 0.0083(14) 0.0042(12) C14 0.0196(15) 0.0230(15) 0.0283(18) 0.0029(13) 0.0011(13) 0.0070(12) C15 0.0154(14) 0.0192(13) 0.0229(16) 0.0003(12) 0.0033(12) 0.0041(11) C16 0.0118(13) 0.0225(14) 0.0178(15) -0.0031(12) 0.0011(11) 0.0035(11) C17 0.0214(15) 0.0264(15) 0.0230(17) 0.0029(13) 0.0044(13) 0.0097(12) C18 0.0226(17) 0.048(2) 0.0197(17) 0.0017(15) 0.0072(13) 0.0100(15) C19 0.0204(16) 0.046(2) 0.0226(18) -0.0072(15) 0.0042(14) 0.0052(15) C20 0.0220(17) 0.0322(17) 0.037(2) -0.0095(15) 0.0080(15) 0.0060(14) C21 0.0201(15) 0.0235(15) 0.0289(18) -0.0002(13) 0.0058(13) 0.0065(12) C22 0.0152(14) 0.0174(13) 0.0208(16) 0.0025(11) 0.0030(12) 0.0046(11) C23 0.0186(15) 0.0227(14) 0.0200(16) -0.0016(12) -0.0007(12) 0.0060(12) C24 0.0180(15) 0.0298(16) 0.0213(16) 0.0021(13) -0.0014(12) 0.0051(12) C25 0.0145(14) 0.0268(15) 0.0308(18) 0.0105(13) 0.0062(13) 0.0082(12) C26 0.0201(15) 0.0217(14) 0.0243(17) 0.0019(12) 0.0086(13) 0.0056(12) C27 0.0169(14) 0.0198(13) 0.0161(15) 0.0007(11) 0.0017(11) 0.0042(11) C28 0.035(2) 0.0301(17) 0.032(2) 0.0053(15) 0.0079(16) 0.0104(15) O3 0.0319(14) 0.0522(17) 0.0332(16) 0.0153(13) -0.0001(12) 0.0079(13) _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 N1 1.977(3) . ? Pt1 N2 2.000(3) . ? Pt1 O2 2.008(2) . ? Pt1 P1 2.2368(8) . ? P1 C22 1.815(3) . ? P1 C1 1.820(3) . ? P1 C16 1.828(3) . ? N1 C7 1.291(4) . ? N1 C8 1.493(4) . ? N2 C9 1.342(4) . ? N2 C10 1.414(4) . ? O2 C15 1.368(4) . ? C1 C2 1.396(4) . ? C1 C6 1.403(4) . ? C2 C3 1.386(4) . ? C3 C4 1.383(5) . ? C4 C5 1.378(5) . ? C5 C6 1.408(4) . ? C6 C7 1.463(5) . ? C8 C9 1.536(4) . ? C9 O1 1.227(4) . ? C10 C11 1.397(4) . ? C10 C15 1.409(4) . ? C11 C12 1.396(5) . ? C12 C13 1.393(5) . ? C13 C14 1.393(5) . ? C14 C15 1.397(4) . ? C16 C17 1.400(4) . ? C16 C21 1.401(4) . ? C17 C18 1.397(5) . ? C18 C19 1.389(5) . ? C19 C20 1.382(5) . ? C20 C21 1.386(5) . ? C22 C23 1.398(4) . ? C22 C27 1.399(4) . ? C23 C24 1.395(4) . ? C24 C25 1.387(5) . ? C25 C26 1.387(5) . ? C26 C27 1.389(4) . ? C28 O3 1.407(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N2 83.36(11) . . ? N1 Pt1 O2 166.11(10) . . ? N2 Pt1 O2 82.75(9) . . ? N1 Pt1 P1 95.34(8) . . ? N2 Pt1 P1 178.58(7) . . ? O2 Pt1 P1 98.56(6) . . ? C22 P1 C1 104.55(14) . . ? C22 P1 C16 105.32(14) . . ? C1 P1 C16 103.81(14) . . ? C22 P1 Pt1 114.27(10) . . ? C1 P1 Pt1 111.78(11) . . ? C16 P1 Pt1 115.95(10) . . ? C7 N1 C8 116.4(3) . . ? C7 N1 Pt1 131.7(2) . . ? C8 N1 Pt1 111.95(19) . . ? C9 N2 C10 128.3(3) . . ? C9 N2 Pt1 118.0(2) . . ? C10 N2 Pt1 113.2(2) . . ? C15 O2 Pt1 111.00(19) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 P1 118.2(2) . . ? C6 C1 P1 122.8(2) . . ? C3 C2 C1 121.3(3) . . ? C4 C3 C2 120.1(3) . . ? C5 C4 C3 119.3(3) . . ? C4 C5 C6 121.8(3) . . ? C1 C6 C5 118.5(3) . . ? C1 C6 C7 127.5(3) . . ? C5 C6 C7 114.0(3) . . ? N1 C7 C6 129.2(3) . . ? N1 C8 C9 113.5(2) . . ? O1 C9 N2 128.6(3) . . ? O1 C9 C8 119.0(3) . . ? N2 C9 C8 112.3(3) . . ? C11 C10 C15 120.4(3) . . ? C11 C10 N2 126.5(3) . . ? C15 C10 N2 113.0(3) . . ? C12 C11 C10 119.7(3) . . ? C13 C12 C11 119.8(3) . . ? C14 C13 C12 120.9(3) . . ? C13 C14 C15 119.7(3) . . ? O2 C15 C14 120.6(3) . . ? O2 C15 C10 120.0(3) . . ? C14 C15 C10 119.4(3) . . ? C17 C16 C21 119.0(3) . . ? C17 C16 P1 118.9(2) . . ? C21 C16 P1 122.1(2) . . ? C18 C17 C16 120.4(3) . . ? C19 C18 C17 119.5(3) . . ? C20 C19 C18 120.6(3) . . ? C19 C20 C21 120.2(3) . . ? C20 C21 C16 120.4(3) . . ? C23 C22 C27 119.4(3) . . ? C23 C22 P1 122.8(2) . . ? C27 C22 P1 117.7(2) . . ? C24 C23 C22 120.6(3) . . ? C25 C24 C23 119.5(3) . . ? C26 C25 C24 120.2(3) . . ? C25 C26 C27 120.8(3) . . ? C26 C27 C22 119.5(3) . . ? 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 N1 Pt1 P1 C22 -131.37(13) . . . . ? O2 Pt1 P1 C22 48.74(13) . . . . ? N1 Pt1 P1 C1 -12.89(13) . . . . ? O2 Pt1 P1 C1 167.22(13) . . . . ? N1 Pt1 P1 C16 105.82(13) . . . . ? O2 Pt1 P1 C16 -74.06(13) . . . . ? N2 Pt1 N1 C7 -171.2(3) . . . . ? O2 Pt1 N1 C7 -172.2(3) . . . . ? P1 Pt1 N1 C7 8.2(3) . . . . ? N2 Pt1 N1 C8 8.4(2) . . . . ? O2 Pt1 N1 C8 7.4(5) . . . . ? P1 Pt1 N1 C8 -172.16(19) . . . . ? N1 Pt1 N2 C9 -7.9(2) . . . . ? O2 Pt1 N2 C9 171.9(2) . . . . ? N1 Pt1 N2 C10 179.5(2) . . . . ? O2 Pt1 N2 C10 -0.7(2) . . . . ? N1 Pt1 O2 C15 0.4(5) . . . . ? N2 Pt1 O2 C15 -0.6(2) . . . . ? P1 Pt1 O2 C15 179.95(19) . . . . ? C22 P1 C1 C2 -44.3(3) . . . . ? C16 P1 C1 C2 65.9(3) . . . . ? Pt1 P1 C1 C2 -168.4(2) . . . . ? C22 P1 C1 C6 138.3(3) . . . . ? C16 P1 C1 C6 -111.5(3) . . . . ? Pt1 P1 C1 C6 14.2(3) . . . . ? C6 C1 C2 C3 1.3(5) . . . . ? P1 C1 C2 C3 -176.2(3) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C3 C4 C5 C6 -0.5(5) . . . . ? C2 C1 C6 C5 -1.9(5) . . . . ? P1 C1 C6 C5 175.4(2) . . . . ? C2 C1 C6 C7 177.0(3) . . . . ? P1 C1 C6 C7 -5.6(5) . . . . ? C4 C5 C6 C1 1.6(5) . . . . ? C4 C5 C6 C7 -177.5(3) . . . . ? C8 N1 C7 C6 -179.5(3) . . . . ? Pt1 N1 C7 C6 0.1(5) . . . . ? C1 C6 C7 N1 -3.5(6) . . . . ? C5 C6 C7 N1 175.4(3) . . . . ? C7 N1 C8 C9 171.5(3) . . . . ? Pt1 N1 C8 C9 -8.2(3) . . . . ? C10 N2 C9 O1 -1.7(6) . . . . ? Pt1 N2 C9 O1 -173.0(3) . . . . ? C10 N2 C9 C8 176.3(3) . . . . ? Pt1 N2 C9 C8 5.0(3) . . . . ? N1 C8 C9 O1 -179.6(3) . . . . ? N1 C8 C9 N2 2.2(4) . . . . ? C9 N2 C10 C11 8.8(5) . . . . ? Pt1 N2 C10 C11 -179.5(3) . . . . ? C9 N2 C10 C15 -169.8(3) . . . . ? Pt1 N2 C10 C15 1.9(3) . . . . ? C15 C10 C11 C12 1.4(5) . . . . ? N2 C10 C11 C12 -177.1(3) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C11 C12 C13 C14 -0.9(5) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? Pt1 O2 C15 C14 -177.4(2) . . . . ? Pt1 O2 C15 C10 2.0(3) . . . . ? C13 C14 C15 O2 -179.6(3) . . . . ? C13 C14 C15 C10 1.1(5) . . . . ? C11 C10 C15 O2 178.7(3) . . . . ? N2 C10 C15 O2 -2.6(4) . . . . ? C11 C10 C15 C14 -1.9(5) . . . . ? N2 C10 C15 C14 176.7(3) . . . . ? C22 P1 C16 C17 -61.5(3) . . . . ? C1 P1 C16 C17 -171.1(2) . . . . ? Pt1 P1 C16 C17 65.9(3) . . . . ? C22 P1 C16 C21 121.8(3) . . . . ? C1 P1 C16 C21 12.2(3) . . . . ? Pt1 P1 C16 C21 -110.8(2) . . . . ? C21 C16 C17 C18 -1.5(5) . . . . ? P1 C16 C17 C18 -178.3(3) . . . . ? C16 C17 C18 C19 0.7(5) . . . . ? C17 C18 C19 C20 0.2(5) . . . . ? C18 C19 C20 C21 -0.3(5) . . . . ? C19 C20 C21 C16 -0.5(5) . . . . ? C17 C16 C21 C20 1.4(5) . . . . ? P1 C16 C21 C20 178.1(3) . . . . ? C1 P1 C22 C23 90.7(3) . . . . ? C16 P1 C22 C23 -18.4(3) . . . . ? Pt1 P1 C22 C23 -146.8(2) . . . . ? C1 P1 C22 C27 -87.7(2) . . . . ? C16 P1 C22 C27 163.3(2) . . . . ? Pt1 P1 C22 C27 34.8(3) . . . . ? C27 C22 C23 C24 -0.9(4) . . . . ? P1 C22 C23 C24 -179.2(2) . . . . ? C22 C23 C24 C25 0.8(5) . . . . ? C23 C24 C25 C26 0.1(5) . . . . ? C24 C25 C26 C27 -1.0(5) . . . . ? C25 C26 C27 C22 0.9(4) . . . . ? C23 C22 C27 C26 0.0(4) . . . . ? P1 C22 C27 C26 178.4(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O2 0.84 1.94 2.775(4) 173.8 . _diffrn_measured_fraction_theta_max 0.865 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.358 _refine_diff_density_min -1.814 _refine_diff_density_rms 0.127 #===END data_11b _database_code_depnum_ccdc_archive 'CCDC 771453' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H21 N2 O2 P Pd, 0.5(C1 H1 Cl3), 0.5(C4 H10 O)' _chemical_formula_sum 'C29.50 H26.50 Cl1.50 N2 O2.50 P Pd' _chemical_formula_weight 639.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' 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 14.2900(9) _cell_length_b 24.1029(16) _cell_length_c 17.0697(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.6250(13) _cell_angle_gamma 90.00 _cell_volume 5502.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5711 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 28.45 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 0.911 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.868 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details 'SADABS v2.03, Sheldrick, G.M., (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 39875 _diffrn_reflns_av_R_equivalents 0.0860 _diffrn_reflns_av_sigmaI/netI 0.0965 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9684 _reflns_number_gt 5908 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0944P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0045(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9684 _refine_ls_number_parameters 632 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0973 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1643 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 0.940 _refine_ls_restrained_S_all 0.940 _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 0.05160(4) 0.32204(2) 0.39798(3) 0.02756(17) Uani 1 1 d . . . P1 P 0.17144(13) 0.25656(7) 0.43359(11) 0.0295(4) Uani 1 1 d . . . N1 N 0.1044(4) 0.3608(2) 0.3199(3) 0.0302(13) Uani 1 1 d . . . N2 N -0.0577(4) 0.3756(2) 0.3569(3) 0.0285(13) Uani 1 1 d . . . O2 O -0.0218(3) 0.29767(18) 0.4725(3) 0.0336(11) Uani 1 1 d . . . C1 C 0.2731(5) 0.2742(3) 0.3978(4) 0.0283(15) Uani 1 1 d . . . C2 C 0.3597(5) 0.2415(3) 0.4266(5) 0.0392(18) Uani 1 1 d . . . H2 H 0.3619 0.2106 0.4617 0.047 Uiso 1 1 calc R . . C3 C 0.4415(6) 0.2533(3) 0.4052(5) 0.046(2) Uani 1 1 d . . . H3 H 0.4986 0.2299 0.4238 0.055 Uiso 1 1 calc R . . C4 C 0.4412(5) 0.2999(3) 0.3559(5) 0.045(2) Uani 1 1 d . . . H4 H 0.4985 0.3092 0.3425 0.055 Uiso 1 1 calc R . . C5 C 0.3571(5) 0.3316(3) 0.3275(4) 0.0361(17) Uani 1 1 d . . . H5 H 0.3561 0.3627 0.2931 0.043 Uiso 1 1 calc R . . C6 C 0.2720(5) 0.3201(3) 0.3472(4) 0.0279(15) Uani 1 1 d . . . C7 C 0.1890(5) 0.3575(3) 0.3091(4) 0.0329(16) Uani 1 1 d . . . H7 H 0.1984 0.3834 0.2706 0.039 Uiso 1 1 calc R . . C8 C 0.0319(5) 0.4040(3) 0.2701(4) 0.0351(17) Uani 1 1 d . . . H8A H 0.0063 0.3927 0.2105 0.042 Uiso 1 1 calc R . . H8B H 0.0680 0.4396 0.2741 0.042 Uiso 1 1 calc R . . C9 C -0.0561(5) 0.4131(3) 0.2987(4) 0.0314(16) Uani 1 1 d . . . O1 O -0.1154(4) 0.45188(19) 0.2679(3) 0.0439(13) Uani 1 1 d . . . C10 C -0.1307(5) 0.3703(3) 0.3947(4) 0.0305(16) Uani 1 1 d . . . C11 C -0.2213(5) 0.3993(3) 0.3759(4) 0.0369(17) Uani 1 1 d . . . H11 H -0.2409 0.4253 0.3313 0.044 Uiso 1 1 calc R . . C12 C -0.2827(5) 0.3897(3) 0.4230(5) 0.0389(18) Uani 1 1 d . . . H12 H -0.3442 0.4091 0.4104 0.047 Uiso 1 1 calc R . . C13 C -0.2527(5) 0.3518(3) 0.4883(5) 0.0385(18) Uani 1 1 d . . . H13 H -0.2941 0.3453 0.5204 0.046 Uiso 1 1 calc R . . C14 C -0.1630(5) 0.3233(3) 0.5074(4) 0.0337(16) Uani 1 1 d . . . H14 H -0.1420 0.2990 0.5542 0.040 Uiso 1 1 calc R . . C15 C -0.1037(5) 0.3298(3) 0.4589(4) 0.0301(16) Uani 1 1 d . . . C16 C 0.2342(5) 0.2454(3) 0.5450(4) 0.0304(16) Uani 1 1 d . . . C17 C 0.2548(5) 0.1925(3) 0.5795(5) 0.0354(17) Uani 1 1 d . . . H17 H 0.2363 0.1605 0.5449 0.042 Uiso 1 1 calc R . . C18 C 0.3035(5) 0.1873(3) 0.6668(5) 0.0401(19) Uani 1 1 d . . . H18 H 0.3171 0.1515 0.6914 0.048 Uiso 1 1 calc R . . C19 C 0.3310(5) 0.2330(3) 0.7158(5) 0.0405(18) Uani 1 1 d . . . H19 H 0.3635 0.2287 0.7745 0.049 Uiso 1 1 calc R . . C20 C 0.3126(6) 0.2853(3) 0.6823(5) 0.049(2) Uani 1 1 d . . . H20 H 0.3339 0.3171 0.7170 0.059 Uiso 1 1 calc R . . C21 C 0.2617(6) 0.2912(3) 0.5953(5) 0.0431(19) Uani 1 1 d . . . H21 H 0.2464 0.3272 0.5716 0.052 Uiso 1 1 calc R . . C22 C 0.1192(5) 0.1895(3) 0.3897(4) 0.0284(15) Uani 1 1 d . . . C23 C 0.0235(5) 0.1777(3) 0.3900(5) 0.0388(18) Uani 1 1 d . . . H23 H -0.0108 0.2044 0.4108 0.047 Uiso 1 1 calc R . . C24 C -0.0215(6) 0.1272(3) 0.3602(5) 0.050(2) Uani 1 1 d . . . H24 H -0.0846 0.1180 0.3635 0.060 Uiso 1 1 calc R . . C25 C 0.0276(6) 0.0901(3) 0.3252(5) 0.048(2) Uani 1 1 d . . . H25 H -0.0049 0.0566 0.3013 0.058 Uiso 1 1 calc R . . C26 C 0.1216(6) 0.1008(3) 0.3245(5) 0.047(2) Uani 1 1 d . . . H26 H 0.1549 0.0742 0.3026 0.056 Uiso 1 1 calc R . . C27 C 0.1681(5) 0.1513(3) 0.3565(4) 0.0384(18) Uani 1 1 d . . . H27 H 0.2327 0.1594 0.3555 0.046 Uiso 1 1 calc R . . Pd2 Pd 0.17722(4) 0.45350(2) 0.06612(3) 0.03010(18) Uani 1 1 d . . . P2 P 0.23187(13) 0.36861(7) 0.05020(11) 0.0298(4) Uani 1 1 d . . . N3 N 0.1291(4) 0.4733(2) -0.0534(4) 0.0366(14) Uani 1 1 d . . . N4 N 0.1318(4) 0.5284(2) 0.0798(4) 0.0356(14) Uani 1 1 d . . . O3 O 0.2212(4) 0.45205(18) 0.1909(3) 0.0403(12) Uani 1 1 d . . . C28 C 0.1898(5) 0.3484(3) -0.0590(4) 0.0316(16) Uani 1 1 d . . . C29 C 0.1981(5) 0.2932(3) -0.0791(5) 0.0377(18) Uani 1 1 d . . . H29 H 0.2234 0.2672 -0.0348 0.045 Uiso 1 1 calc R . . C30 C 0.1711(6) 0.2743(3) -0.1609(5) 0.047(2) Uani 1 1 d . . . H30 H 0.1783 0.2363 -0.1721 0.056 Uiso 1 1 calc R . . C31 C 0.1335(6) 0.3119(4) -0.2259(5) 0.056(2) Uani 1 1 d . . . H31 H 0.1156 0.2999 -0.2823 0.067 Uiso 1 1 calc R . . C32 C 0.1222(6) 0.3668(3) -0.2086(5) 0.0444(19) Uani 1 1 d . . . H32 H 0.0951 0.3920 -0.2537 0.053 Uiso 1 1 calc R . . C33 C 0.1495(5) 0.3867(3) -0.1257(4) 0.0362(17) Uani 1 1 d . . . C34 C 0.1258(5) 0.4455(3) -0.1187(5) 0.0396(18) Uani 1 1 d . . . H34 H 0.1051 0.4659 -0.1696 0.048 Uiso 1 1 calc R . . C35 C 0.0958(5) 0.5320(3) -0.0671(5) 0.0403(19) Uani 1 1 d . . . H35A H 0.0249 0.5329 -0.1046 0.048 Uiso 1 1 calc R . . H35B H 0.1355 0.5515 -0.0959 0.048 Uiso 1 1 calc R . . C36 C 0.1060(5) 0.5628(3) 0.0126(5) 0.0400(19) Uani 1 1 d . . . O4 O 0.0914(4) 0.6130(2) 0.0105(4) 0.0545(16) Uani 1 1 d . . . C37 C 0.1465(5) 0.5426(3) 0.1636(5) 0.0364(17) Uani 1 1 d . . . C38 C 0.1190(5) 0.5915(3) 0.1934(5) 0.0416(19) Uani 1 1 d . . . H38 H 0.0861 0.6201 0.1555 0.050 Uiso 1 1 calc R . . C39 C 0.1398(6) 0.5980(4) 0.2785(6) 0.054(2) Uani 1 1 d . . . H39 H 0.1189 0.6307 0.2986 0.065 Uiso 1 1 calc R . . C40 C 0.1908(7) 0.5574(3) 0.3343(6) 0.053(2) Uani 1 1 d . . . H40 H 0.2053 0.5628 0.3926 0.063 Uiso 1 1 calc R . . C41 C 0.2209(6) 0.5091(3) 0.3066(5) 0.052(2) Uani 1 1 d . . . H41 H 0.2569 0.4816 0.3455 0.063 Uiso 1 1 calc R . . C42 C 0.1977(5) 0.5008(3) 0.2200(5) 0.0339(17) Uani 1 1 d . . . C43 C 0.3657(5) 0.3635(3) 0.0925(4) 0.0304(16) Uani 1 1 d . . . C44 C 0.4220(5) 0.3233(3) 0.0685(5) 0.0374(17) Uani 1 1 d . . . H44 H 0.3894 0.3005 0.0213 0.045 Uiso 1 1 calc R . . C45 C 0.5231(5) 0.3159(3) 0.1114(5) 0.044(2) Uani 1 1 d . . . H45 H 0.5590 0.2879 0.0948 0.053 Uiso 1 1 calc R . . C46 C 0.5713(6) 0.3498(3) 0.1788(5) 0.045(2) Uani 1 1 d . . . H46 H 0.6408 0.3451 0.2086 0.054 Uiso 1 1 calc R . . C47 C 0.5185(5) 0.3909(3) 0.2036(4) 0.0403(18) Uani 1 1 d . . . H47 H 0.5519 0.4141 0.2501 0.048 Uiso 1 1 calc R . . C48 C 0.4161(5) 0.3975(3) 0.1595(4) 0.0357(17) Uani 1 1 d . . . H48 H 0.3806 0.4259 0.1758 0.043 Uiso 1 1 calc R . . C49 C 0.1883(5) 0.3138(3) 0.1012(4) 0.0282(15) Uani 1 1 d . . . C50 C 0.2463(5) 0.2687(3) 0.1438(4) 0.0365(17) Uani 1 1 d . . . H50 H 0.3147 0.2662 0.1494 0.044 Uiso 1 1 calc R . . C51 C 0.2042(6) 0.2280(3) 0.1774(4) 0.0379(18) Uani 1 1 d . . . H51 H 0.2441 0.1977 0.2058 0.045 Uiso 1 1 calc R . . C52 C 0.1063(6) 0.2305(3) 0.1707(4) 0.0421(19) Uani 1 1 d . . . H52 H 0.0786 0.2018 0.1941 0.051 Uiso 1 1 calc R . . C53 C 0.0470(5) 0.2747(3) 0.1299(4) 0.0383(18) Uani 1 1 d . . . H53 H -0.0210 0.2767 0.1255 0.046 Uiso 1 1 calc R . . C54 C 0.0882(5) 0.3159(3) 0.0957(4) 0.0355(17) Uani 1 1 d . . . H54 H 0.0477 0.3462 0.0678 0.043 Uiso 1 1 calc R . . C55 C 0.1465(7) 0.4650(4) 0.5848(5) 0.059(2) Uani 1 1 d . . . H55 H 0.1301 0.5038 0.5967 0.070 Uiso 1 1 calc R . . Cl1 Cl 0.1723(3) 0.46545(14) 0.49291(18) 0.1041(11) Uani 1 1 d . . . Cl2 Cl 0.0448(2) 0.42307(13) 0.57453(15) 0.0860(9) Uani 1 1 d . . . Cl3 Cl 0.2536(2) 0.44240(11) 0.66921(17) 0.0774(8) 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 Pd1 0.0289(3) 0.0243(3) 0.0282(3) 0.0042(2) 0.0085(2) 0.0015(2) P1 0.0308(10) 0.0245(9) 0.0326(10) 0.0056(8) 0.0105(8) 0.0024(7) N1 0.027(3) 0.030(3) 0.022(3) 0.003(2) -0.006(2) 0.001(2) N2 0.032(3) 0.029(3) 0.024(3) 0.003(2) 0.009(3) -0.007(2) O2 0.038(3) 0.029(3) 0.030(3) 0.006(2) 0.008(2) 0.005(2) C1 0.026(4) 0.028(4) 0.030(4) 0.002(3) 0.010(3) 0.007(3) C2 0.043(4) 0.035(4) 0.042(4) 0.008(3) 0.018(4) 0.008(3) C3 0.039(4) 0.045(5) 0.057(5) 0.022(4) 0.021(4) 0.021(4) C4 0.032(4) 0.051(5) 0.065(6) 0.005(4) 0.031(4) 0.008(4) C5 0.045(5) 0.029(4) 0.038(4) 0.008(3) 0.019(4) 0.001(3) C6 0.030(4) 0.029(4) 0.027(4) 0.001(3) 0.012(3) 0.002(3) C7 0.038(4) 0.026(4) 0.040(4) 0.005(3) 0.021(3) 0.001(3) C8 0.041(4) 0.029(4) 0.034(4) 0.008(3) 0.011(3) 0.005(3) C9 0.032(4) 0.031(4) 0.027(4) -0.004(3) 0.005(3) 0.000(3) O1 0.049(3) 0.033(3) 0.045(3) 0.015(2) 0.010(3) 0.018(2) C10 0.030(4) 0.022(4) 0.032(4) -0.005(3) 0.002(3) -0.007(3) C11 0.038(4) 0.029(4) 0.039(4) 0.001(3) 0.007(3) 0.002(3) C12 0.037(4) 0.035(4) 0.047(5) -0.007(4) 0.017(4) 0.000(3) C13 0.042(4) 0.031(4) 0.053(5) -0.011(4) 0.030(4) -0.012(3) C14 0.033(4) 0.031(4) 0.039(4) -0.001(3) 0.014(3) 0.005(3) C15 0.036(4) 0.019(3) 0.036(4) -0.004(3) 0.014(3) -0.002(3) C16 0.030(4) 0.026(4) 0.039(4) 0.006(3) 0.018(3) 0.006(3) C17 0.024(4) 0.037(4) 0.043(4) 0.009(3) 0.009(3) 0.002(3) C18 0.033(4) 0.044(5) 0.042(4) 0.018(4) 0.011(4) 0.011(3) C19 0.040(4) 0.053(5) 0.028(4) 0.008(4) 0.011(3) 0.010(4) C20 0.055(5) 0.050(5) 0.036(5) -0.003(4) 0.009(4) 0.010(4) C21 0.056(5) 0.035(4) 0.035(4) 0.011(3) 0.011(4) 0.015(4) C22 0.029(4) 0.025(4) 0.030(4) 0.002(3) 0.008(3) 0.005(3) C23 0.034(4) 0.036(4) 0.045(5) 0.000(4) 0.013(4) -0.002(3) C24 0.033(4) 0.043(5) 0.072(6) 0.008(4) 0.018(4) -0.002(4) C25 0.051(5) 0.032(4) 0.054(5) -0.012(4) 0.009(4) -0.003(4) C26 0.054(5) 0.038(5) 0.045(5) -0.003(4) 0.012(4) 0.001(4) C27 0.035(4) 0.039(4) 0.043(4) 0.005(4) 0.016(4) 0.001(3) Pd2 0.0345(3) 0.0255(3) 0.0330(3) 0.0068(2) 0.0153(2) 0.0036(2) P2 0.0300(10) 0.0298(10) 0.0308(10) 0.0034(8) 0.0123(8) 0.0022(8) N3 0.033(3) 0.028(3) 0.048(4) 0.004(3) 0.014(3) 0.003(3) N4 0.038(3) 0.027(3) 0.047(4) 0.005(3) 0.022(3) -0.005(3) O3 0.050(3) 0.025(3) 0.046(3) 0.003(2) 0.018(3) 0.003(2) C28 0.028(4) 0.035(4) 0.032(4) -0.003(3) 0.010(3) -0.002(3) C29 0.035(4) 0.043(5) 0.038(4) -0.004(4) 0.017(3) 0.003(3) C30 0.047(5) 0.044(5) 0.054(5) -0.017(4) 0.023(4) -0.001(4) C31 0.048(5) 0.077(7) 0.038(5) 0.000(5) 0.012(4) -0.002(5) C32 0.046(5) 0.056(5) 0.032(4) -0.001(4) 0.015(4) -0.002(4) C33 0.036(4) 0.044(4) 0.030(4) -0.002(3) 0.013(3) -0.004(3) C34 0.029(4) 0.046(5) 0.042(5) 0.014(4) 0.012(3) -0.001(3) C35 0.031(4) 0.039(4) 0.048(5) 0.021(4) 0.010(4) -0.001(3) C36 0.023(4) 0.038(5) 0.051(5) 0.004(4) 0.003(3) 0.000(3) O4 0.050(3) 0.020(3) 0.075(4) 0.015(3) 0.000(3) 0.005(2) C37 0.029(4) 0.034(4) 0.052(5) -0.008(4) 0.022(4) -0.009(3) C38 0.040(4) 0.023(4) 0.075(6) -0.004(4) 0.038(4) -0.005(3) C39 0.056(5) 0.044(5) 0.074(6) -0.023(5) 0.036(5) -0.014(4) C40 0.075(6) 0.036(5) 0.067(6) -0.010(4) 0.051(5) -0.017(4) C41 0.066(6) 0.047(5) 0.054(5) -0.013(4) 0.032(5) -0.014(4) C42 0.043(4) 0.019(4) 0.047(4) -0.001(3) 0.026(4) -0.001(3) C43 0.040(4) 0.027(4) 0.026(4) 0.006(3) 0.014(3) 0.005(3) C44 0.036(4) 0.045(5) 0.033(4) -0.001(3) 0.014(3) -0.006(3) C45 0.031(4) 0.049(5) 0.056(5) -0.002(4) 0.020(4) 0.010(4) C46 0.031(4) 0.054(5) 0.048(5) 0.009(4) 0.010(4) 0.006(4) C47 0.038(4) 0.050(5) 0.030(4) -0.003(3) 0.008(3) -0.003(4) C48 0.035(4) 0.036(4) 0.040(4) 0.006(3) 0.018(3) 0.005(3) C49 0.036(4) 0.025(4) 0.027(4) 0.000(3) 0.016(3) 0.000(3) C50 0.035(4) 0.033(4) 0.041(4) 0.005(3) 0.013(3) 0.008(3) C51 0.051(5) 0.025(4) 0.039(4) 0.006(3) 0.017(4) 0.007(3) C52 0.053(5) 0.043(5) 0.034(4) 0.004(4) 0.019(4) -0.005(4) C53 0.028(4) 0.046(5) 0.040(4) 0.006(4) 0.010(3) -0.004(3) C54 0.033(4) 0.035(4) 0.035(4) 0.010(3) 0.008(3) 0.002(3) C55 0.086(7) 0.040(5) 0.055(6) -0.003(4) 0.032(5) -0.006(5) Cl1 0.145(3) 0.108(2) 0.0718(19) -0.0101(17) 0.0540(19) -0.048(2) Cl2 0.090(2) 0.104(2) 0.0537(15) -0.0097(14) 0.0129(14) -0.0448(17) Cl3 0.0739(17) 0.0644(16) 0.0815(18) 0.0027(13) 0.0119(14) 0.0063(13) _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 N2 1.957(5) . ? Pd1 N1 1.982(6) . ? Pd1 O2 2.001(5) . ? Pd1 P1 2.2494(18) . ? P1 C1 1.813(7) . ? P1 C16 1.814(7) . ? P1 C22 1.826(7) . ? N1 C7 1.289(8) . ? N1 C8 1.503(8) . ? N2 C9 1.349(8) . ? N2 C10 1.413(8) . ? O2 C15 1.353(8) . ? C1 C6 1.401(9) . ? C1 C2 1.402(9) . ? C2 C3 1.371(10) . ? C3 C4 1.403(10) . ? C4 C5 1.361(9) . ? C5 C6 1.399(9) . ? C6 C7 1.448(9) . ? C8 C9 1.517(9) . ? C9 O1 1.246(7) . ? C10 C11 1.405(9) . ? C10 C15 1.414(9) . ? C11 C12 1.403(10) . ? C12 C13 1.387(10) . ? C13 C14 1.389(9) . ? C14 C15 1.386(9) . ? C16 C21 1.367(10) . ? C16 C17 1.393(9) . ? C17 C18 1.411(10) . ? C18 C19 1.355(10) . ? C19 C20 1.371(10) . ? C20 C21 1.411(10) . ? C22 C27 1.392(9) . ? C22 C23 1.398(9) . ? C23 C24 1.387(10) . ? C24 C25 1.393(11) . ? C25 C26 1.372(11) . ? C26 C27 1.403(10) . ? Pd2 N4 1.960(6) . ? Pd2 N3 1.968(6) . ? Pd2 O3 1.997(5) . ? Pd2 P2 2.2403(19) . ? P2 C43 1.794(7) . ? P2 C49 1.809(7) . ? P2 C28 1.812(7) . ? N3 C34 1.287(9) . ? N3 C35 1.484(9) . ? N4 C36 1.358(9) . ? N4 C37 1.412(9) . ? O3 C42 1.363(8) . ? C28 C29 1.388(9) . ? C28 C33 1.421(10) . ? C29 C30 1.388(10) . ? C30 C31 1.386(11) . ? C31 C32 1.377(11) . ? C32 C33 1.412(10) . ? C33 C34 1.473(10) . ? C35 C36 1.512(11) . ? C36 O4 1.226(8) . ? C37 C38 1.393(9) . ? C37 C42 1.407(10) . ? C38 C39 1.385(11) . ? C39 C40 1.380(12) . ? C40 C41 1.382(11) . ? C41 C42 1.410(10) . ? C43 C48 1.385(9) . ? C43 C44 1.410(9) . ? C44 C45 1.382(10) . ? C45 C46 1.380(11) . ? C46 C47 1.398(10) . ? C47 C48 1.399(9) . ? C49 C54 1.400(9) . ? C49 C50 1.406(9) . ? C50 C51 1.375(10) . ? C51 C52 1.365(10) . ? C52 C53 1.386(10) . ? C53 C54 1.385(9) . ? C55 Cl2 1.728(9) . ? C55 Cl1 1.733(9) . ? C55 Cl3 1.779(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd1 N1 83.8(2) . . ? N2 Pd1 O2 83.7(2) . . ? N1 Pd1 O2 167.2(2) . . ? N2 Pd1 P1 174.70(16) . . ? N1 Pd1 P1 94.50(16) . . ? O2 Pd1 P1 98.18(13) . . ? C1 P1 C16 103.2(3) . . ? C1 P1 C22 109.2(3) . . ? C16 P1 C22 106.2(3) . . ? C1 P1 Pd1 111.6(2) . . ? C16 P1 Pd1 115.8(2) . . ? C22 P1 Pd1 110.3(2) . . ? C7 N1 C8 117.2(6) . . ? C7 N1 Pd1 131.7(5) . . ? C8 N1 Pd1 110.9(4) . . ? C9 N2 C10 127.2(6) . . ? C9 N2 Pd1 119.2(4) . . ? C10 N2 Pd1 113.6(4) . . ? C15 O2 Pd1 109.8(4) . . ? C6 C1 C2 118.4(6) . . ? C6 C1 P1 123.8(5) . . ? C2 C1 P1 117.6(5) . . ? C3 C2 C1 121.4(7) . . ? C2 C3 C4 120.2(7) . . ? C5 C4 C3 118.6(7) . . ? C4 C5 C6 122.5(7) . . ? C5 C6 C1 118.9(6) . . ? C5 C6 C7 114.4(6) . . ? C1 C6 C7 126.7(6) . . ? N1 C7 C6 129.5(6) . . ? N1 C8 C9 113.7(6) . . ? O1 C9 N2 128.8(7) . . ? O1 C9 C8 119.4(6) . . ? N2 C9 C8 111.8(6) . . ? C11 C10 N2 128.2(6) . . ? C11 C10 C15 119.9(7) . . ? N2 C10 C15 111.9(6) . . ? C12 C11 C10 120.0(7) . . ? C13 C12 C11 119.4(7) . . ? C12 C13 C14 120.8(7) . . ? C15 C14 C13 120.8(7) . . ? O2 C15 C14 120.4(6) . . ? O2 C15 C10 120.7(6) . . ? C14 C15 C10 118.9(6) . . ? C21 C16 C17 120.1(7) . . ? C21 C16 P1 117.8(5) . . ? C17 C16 P1 122.1(5) . . ? C16 C17 C18 118.7(7) . . ? C19 C18 C17 120.5(7) . . ? C18 C19 C20 121.2(7) . . ? C19 C20 C21 118.9(7) . . ? C16 C21 C20 120.5(7) . . ? C27 C22 C23 119.9(6) . . ? C27 C22 P1 124.1(5) . . ? C23 C22 P1 116.0(5) . . ? C24 C23 C22 120.4(7) . . ? C23 C24 C25 118.8(7) . . ? C26 C25 C24 121.7(7) . . ? C25 C26 C27 119.4(8) . . ? C22 C27 C26 119.7(7) . . ? N4 Pd2 N3 83.7(2) . . ? N4 Pd2 O3 83.2(2) . . ? N3 Pd2 O3 166.7(2) . . ? N4 Pd2 P2 178.85(17) . . ? N3 Pd2 P2 96.07(18) . . ? O3 Pd2 P2 96.97(14) . . ? C43 P2 C49 104.8(3) . . ? C43 P2 C28 108.4(3) . . ? C49 P2 C28 104.7(3) . . ? C43 P2 Pd2 112.4(2) . . ? C49 P2 Pd2 114.5(2) . . ? C28 P2 Pd2 111.5(2) . . ? C34 N3 C35 116.6(6) . . ? C34 N3 Pd2 131.6(5) . . ? C35 N3 Pd2 111.8(5) . . ? C36 N4 C37 127.4(6) . . ? C36 N4 Pd2 117.7(5) . . ? C37 N4 Pd2 114.0(4) . . ? C42 O3 Pd2 110.4(4) . . ? C29 C28 C33 118.0(6) . . ? C29 C28 P2 119.1(5) . . ? C33 C28 P2 122.9(5) . . ? C28 C29 C30 123.1(7) . . ? C31 C30 C29 118.8(8) . . ? C32 C31 C30 119.9(8) . . ? C31 C32 C33 122.0(8) . . ? C32 C33 C28 118.2(7) . . ? C32 C33 C34 114.7(7) . . ? C28 C33 C34 126.9(6) . . ? N3 C34 C33 129.3(7) . . ? N3 C35 C36 113.7(6) . . ? O4 C36 N4 128.3(8) . . ? O4 C36 C35 119.8(7) . . ? N4 C36 C35 111.8(6) . . ? C38 C37 C42 120.1(7) . . ? C38 C37 N4 127.9(7) . . ? C42 C37 N4 112.0(6) . . ? C39 C38 C37 119.6(8) . . ? C40 C39 C38 120.7(8) . . ? C39 C40 C41 120.8(8) . . ? C40 C41 C42 119.4(8) . . ? O3 C42 C37 120.2(6) . . ? O3 C42 C41 120.4(7) . . ? C37 C42 C41 119.3(7) . . ? C48 C43 C44 117.5(6) . . ? C48 C43 P2 117.6(5) . . ? C44 C43 P2 124.5(5) . . ? C45 C44 C43 122.1(7) . . ? C46 C45 C44 119.2(7) . . ? C45 C46 C47 120.5(7) . . ? C46 C47 C48 119.4(7) . . ? C43 C48 C47 121.2(7) . . ? C54 C49 C50 117.7(6) . . ? C54 C49 P2 117.2(5) . . ? C50 C49 P2 125.0(5) . . ? C51 C50 C49 120.1(7) . . ? C52 C51 C50 121.4(7) . . ? C51 C52 C53 120.1(7) . . ? C54 C53 C52 119.2(7) . . ? C53 C54 C49 121.5(6) . . ? Cl2 C55 Cl1 110.6(5) . . ? Cl2 C55 Cl3 110.8(5) . . ? Cl1 C55 Cl3 109.8(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 N1 Pd1 P1 C1 12.2(3) . . . . ? O2 Pd1 P1 C1 -165.8(3) . . . . ? N1 Pd1 P1 C16 129.9(3) . . . . ? O2 Pd1 P1 C16 -48.1(3) . . . . ? N1 Pd1 P1 C22 -109.4(3) . . . . ? O2 Pd1 P1 C22 72.5(3) . . . . ? N2 Pd1 N1 C7 170.8(6) . . . . ? O2 Pd1 N1 C7 156.8(8) . . . . ? P1 Pd1 N1 C7 -14.3(6) . . . . ? N2 Pd1 N1 C8 -4.5(4) . . . . ? O2 Pd1 N1 C8 -18.5(11) . . . . ? P1 Pd1 N1 C8 170.4(4) . . . . ? N1 Pd1 N2 C9 0.4(5) . . . . ? O2 Pd1 N2 C9 177.3(5) . . . . ? N1 Pd1 N2 C10 -178.7(4) . . . . ? O2 Pd1 N2 C10 -1.8(4) . . . . ? N2 Pd1 O2 C15 -1.5(4) . . . . ? N1 Pd1 O2 C15 12.4(11) . . . . ? P1 Pd1 O2 C15 -176.5(4) . . . . ? C16 P1 C1 C6 -130.9(6) . . . . ? C22 P1 C1 C6 116.4(6) . . . . ? Pd1 P1 C1 C6 -5.9(6) . . . . ? C16 P1 C1 C2 45.3(6) . . . . ? C22 P1 C1 C2 -67.4(6) . . . . ? Pd1 P1 C1 C2 170.4(5) . . . . ? C6 C1 C2 C3 -1.0(11) . . . . ? P1 C1 C2 C3 -177.4(6) . . . . ? C1 C2 C3 C4 2.2(12) . . . . ? C2 C3 C4 C5 -2.4(12) . . . . ? C3 C4 C5 C6 1.4(12) . . . . ? C4 C5 C6 C1 -0.2(11) . . . . ? C4 C5 C6 C7 -178.2(7) . . . . ? C2 C1 C6 C5 -0.1(10) . . . . ? P1 C1 C6 C5 176.1(5) . . . . ? C2 C1 C6 C7 177.7(6) . . . . ? P1 C1 C6 C7 -6.1(10) . . . . ? C8 N1 C7 C6 -179.3(7) . . . . ? Pd1 N1 C7 C6 5.7(11) . . . . ? C5 C6 C7 N1 -173.9(7) . . . . ? C1 C6 C7 N1 8.2(12) . . . . ? C7 N1 C8 C9 -168.3(6) . . . . ? Pd1 N1 C8 C9 7.7(7) . . . . ? C10 N2 C9 O1 2.7(11) . . . . ? Pd1 N2 C9 O1 -176.3(5) . . . . ? C10 N2 C9 C8 -177.2(6) . . . . ? Pd1 N2 C9 C8 3.8(7) . . . . ? N1 C8 C9 O1 172.6(6) . . . . ? N1 C8 C9 N2 -7.5(8) . . . . ? C9 N2 C10 C11 5.7(11) . . . . ? Pd1 N2 C10 C11 -175.3(5) . . . . ? C9 N2 C10 C15 -174.4(6) . . . . ? Pd1 N2 C10 C15 4.6(7) . . . . ? N2 C10 C11 C12 -177.4(6) . . . . ? C15 C10 C11 C12 2.7(10) . . . . ? C10 C11 C12 C13 0.4(10) . . . . ? C11 C12 C13 C14 0.0(10) . . . . ? C12 C13 C14 C15 -3.5(10) . . . . ? Pd1 O2 C15 C14 -175.6(5) . . . . ? Pd1 O2 C15 C10 4.9(7) . . . . ? C13 C14 C15 O2 -173.1(6) . . . . ? C13 C14 C15 C10 6.5(10) . . . . ? C11 C10 C15 O2 173.5(6) . . . . ? N2 C10 C15 O2 -6.4(8) . . . . ? C11 C10 C15 C14 -6.1(10) . . . . ? N2 C10 C15 C14 174.0(6) . . . . ? C1 P1 C16 C21 78.6(6) . . . . ? C22 P1 C16 C21 -166.6(6) . . . . ? Pd1 P1 C16 C21 -43.7(6) . . . . ? C1 P1 C16 C17 -101.2(6) . . . . ? C22 P1 C16 C17 13.6(7) . . . . ? Pd1 P1 C16 C17 136.5(5) . . . . ? C21 C16 C17 C18 0.5(10) . . . . ? P1 C16 C17 C18 -179.7(5) . . . . ? C16 C17 C18 C19 -1.0(11) . . . . ? C17 C18 C19 C20 -0.2(11) . . . . ? C18 C19 C20 C21 1.8(12) . . . . ? C17 C16 C21 C20 1.1(11) . . . . ? P1 C16 C21 C20 -178.7(6) . . . . ? C19 C20 C21 C16 -2.3(12) . . . . ? C1 P1 C22 C27 18.0(7) . . . . ? C16 P1 C22 C27 -92.8(6) . . . . ? Pd1 P1 C22 C27 141.0(5) . . . . ? C1 P1 C22 C23 -161.5(5) . . . . ? C16 P1 C22 C23 87.7(6) . . . . ? Pd1 P1 C22 C23 -38.5(6) . . . . ? C27 C22 C23 C24 2.3(11) . . . . ? P1 C22 C23 C24 -178.2(6) . . . . ? C22 C23 C24 C25 -4.0(11) . . . . ? C23 C24 C25 C26 4.3(12) . . . . ? C24 C25 C26 C27 -2.8(12) . . . . ? C23 C22 C27 C26 -0.8(10) . . . . ? P1 C22 C27 C26 179.7(5) . . . . ? C25 C26 C27 C22 1.0(11) . . . . ? N3 Pd2 P2 C43 110.8(3) . . . . ? O3 Pd2 P2 C43 -66.5(3) . . . . ? N3 Pd2 P2 C49 -129.8(3) . . . . ? O3 Pd2 P2 C49 53.0(3) . . . . ? N3 Pd2 P2 C28 -11.2(3) . . . . ? O3 Pd2 P2 C28 171.5(3) . . . . ? N4 Pd2 N3 C34 -178.0(7) . . . . ? O3 Pd2 N3 C34 171.3(8) . . . . ? P2 Pd2 N3 C34 3.1(7) . . . . ? N4 Pd2 N3 C35 5.2(4) . . . . ? O3 Pd2 N3 C35 -5.5(12) . . . . ? P2 Pd2 N3 C35 -173.7(4) . . . . ? N3 Pd2 N4 C36 -10.5(5) . . . . ? O3 Pd2 N4 C36 167.1(5) . . . . ? N3 Pd2 N4 C37 179.7(5) . . . . ? O3 Pd2 N4 C37 -2.7(4) . . . . ? N4 Pd2 O3 C42 0.5(4) . . . . ? N3 Pd2 O3 C42 11.2(12) . . . . ? P2 Pd2 O3 C42 179.4(4) . . . . ? C43 P2 C28 C29 69.5(6) . . . . ? C49 P2 C28 C29 -41.9(6) . . . . ? Pd2 P2 C28 C29 -166.3(5) . . . . ? C43 P2 C28 C33 -109.7(6) . . . . ? C49 P2 C28 C33 138.9(6) . . . . ? Pd2 P2 C28 C33 14.6(6) . . . . ? C33 C28 C29 C30 1.6(10) . . . . ? P2 C28 C29 C30 -177.7(6) . . . . ? C28 C29 C30 C31 -0.4(11) . . . . ? C29 C30 C31 C32 -1.0(12) . . . . ? C30 C31 C32 C33 1.2(12) . . . . ? C31 C32 C33 C28 0.0(11) . . . . ? C31 C32 C33 C34 -175.9(7) . . . . ? C29 C28 C33 C32 -1.3(10) . . . . ? P2 C28 C33 C32 177.9(5) . . . . ? C29 C28 C33 C34 174.0(7) . . . . ? P2 C28 C33 C34 -6.8(10) . . . . ? C35 N3 C34 C33 -177.2(7) . . . . ? Pd2 N3 C34 C33 6.1(12) . . . . ? C32 C33 C34 N3 169.9(7) . . . . ? C28 C33 C34 N3 -5.6(12) . . . . ? C34 N3 C35 C36 -177.5(6) . . . . ? Pd2 N3 C35 C36 -0.1(7) . . . . ? C37 N4 C36 O4 1.1(12) . . . . ? Pd2 N4 C36 O4 -167.1(6) . . . . ? C37 N4 C36 C35 -179.2(6) . . . . ? Pd2 N4 C36 C35 12.6(7) . . . . ? N3 C35 C36 O4 171.9(6) . . . . ? N3 C35 C36 N4 -7.8(8) . . . . ? C36 N4 C37 C38 14.1(11) . . . . ? Pd2 N4 C37 C38 -177.3(6) . . . . ? C36 N4 C37 C42 -164.3(6) . . . . ? Pd2 N4 C37 C42 4.3(7) . . . . ? C42 C37 C38 C39 -1.7(10) . . . . ? N4 C37 C38 C39 180.0(7) . . . . ? C37 C38 C39 C40 2.3(11) . . . . ? C38 C39 C40 C41 -0.9(12) . . . . ? C39 C40 C41 C42 -1.0(12) . . . . ? Pd2 O3 C42 C37 1.9(8) . . . . ? Pd2 O3 C42 C41 179.4(5) . . . . ? C38 C37 C42 O3 177.3(6) . . . . ? N4 C37 C42 O3 -4.2(9) . . . . ? C38 C37 C42 C41 -0.2(10) . . . . ? N4 C37 C42 C41 178.3(6) . . . . ? C40 C41 C42 O3 -175.9(7) . . . . ? C40 C41 C42 C37 1.6(11) . . . . ? C49 P2 C43 C48 -95.6(6) . . . . ? C28 P2 C43 C48 153.1(5) . . . . ? Pd2 P2 C43 C48 29.3(6) . . . . ? C49 P2 C43 C44 77.0(6) . . . . ? C28 P2 C43 C44 -34.3(7) . . . . ? Pd2 P2 C43 C44 -158.0(5) . . . . ? C48 C43 C44 C45 2.5(10) . . . . ? P2 C43 C44 C45 -170.2(6) . . . . ? C43 C44 C45 C46 -1.5(11) . . . . ? C44 C45 C46 C47 0.2(12) . . . . ? C45 C46 C47 C48 0.0(11) . . . . ? C44 C43 C48 C47 -2.2(10) . . . . ? P2 C43 C48 C47 170.9(5) . . . . ? C46 C47 C48 C43 1.1(11) . . . . ? C43 P2 C49 C54 165.1(5) . . . . ? C28 P2 C49 C54 -80.9(6) . . . . ? Pd2 P2 C49 C54 41.6(6) . . . . ? C43 P2 C49 C50 -16.8(7) . . . . ? C28 P2 C49 C50 97.2(6) . . . . ? Pd2 P2 C49 C50 -140.3(5) . . . . ? C54 C49 C50 C51 0.8(10) . . . . ? P2 C49 C50 C51 -177.2(5) . . . . ? C49 C50 C51 C52 -0.3(11) . . . . ? C50 C51 C52 C53 -0.4(11) . . . . ? C51 C52 C53 C54 0.5(11) . . . . ? C52 C53 C54 C49 0.1(11) . . . . ? C50 C49 C54 C53 -0.8(10) . . . . ? P2 C49 C54 C53 177.5(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.969 _refine_diff_density_min -1.281 _refine_diff_density_rms 0.147 #===END data_11c _database_code_depnum_ccdc_archive 'CCDC 771454' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H21 N2 Ni O2 P' _chemical_formula_sum 'C27 H21 N2 Ni O2 P' _chemical_formula_weight 495.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9313(4) _cell_length_b 11.5187(6) _cell_length_c 11.5474(6) _cell_angle_alpha 73.3268(8) _cell_angle_beta 84.8308(8) _cell_angle_gamma 70.0607(8) _cell_volume 1069.76(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5896 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 29.02 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 512 _exptl_absorpt_coefficient_mu 1.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.738 _exptl_absorpt_correction_T_max 0.897 _exptl_absorpt_process_details 'SADABS v2.03, Sheldrick, G.M., (2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9613 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 29.10 _reflns_number_total 4986 _reflns_number_gt 4309 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0384P)^2^+0.5121P] 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 4986 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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 Ni1 Ni 0.32175(3) 0.26413(2) 0.196942(19) 0.02223(7) Uani 1 1 d . . . P1 P 0.39862(5) 0.35617(4) 0.30722(4) 0.02139(10) Uani 1 1 d . . . N1 N 0.48738(17) 0.25965(13) 0.08581(12) 0.0232(3) Uani 1 1 d . . . N2 N 0.24411(17) 0.18876(13) 0.10504(13) 0.0241(3) Uani 1 1 d . . . O2 O 0.15704(15) 0.24912(12) 0.30158(11) 0.0280(3) Uani 1 1 d . . . C1 C 0.5518(2) 0.42265(16) 0.23469(15) 0.0237(3) Uani 1 1 d . . . C2 C 0.5869(2) 0.51284(17) 0.27623(16) 0.0286(4) Uani 1 1 d . . . H2 H 0.5224 0.5460 0.3370 0.034 Uiso 1 1 calc R . . C3 C 0.7142(2) 0.55528(18) 0.23076(17) 0.0315(4) Uani 1 1 d . . . H3 H 0.7353 0.6176 0.2595 0.038 Uiso 1 1 calc R . . C4 C 0.8103(2) 0.50593(19) 0.14292(17) 0.0330(4) Uani 1 1 d . . . H4 H 0.9004 0.5314 0.1138 0.040 Uiso 1 1 calc R . . C5 C 0.7738(2) 0.41960(18) 0.09829(16) 0.0300(4) Uani 1 1 d . . . H5 H 0.8393 0.3869 0.0376 0.036 Uiso 1 1 calc R . . C6 C 0.6428(2) 0.37890(17) 0.14015(15) 0.0247(3) Uani 1 1 d . . . C7 C 0.6077(2) 0.29901(16) 0.07478(15) 0.0252(3) Uani 1 1 d . . . H7 H 0.6842 0.2729 0.0165 0.030 Uiso 1 1 calc R . . C8 C 0.4824(2) 0.18696(17) -0.00093(16) 0.0272(4) Uani 1 1 d . . . H8A H 0.5721 0.1048 0.0165 0.033 Uiso 1 1 calc R . . H8B H 0.4948 0.2373 -0.0843 0.033 Uiso 1 1 calc R . . C9 C 0.3265(2) 0.16003(16) 0.00845(15) 0.0260(4) Uani 1 1 d . . . O1 O 0.29197(17) 0.11215(13) -0.06393(12) 0.0341(3) Uani 1 1 d . . . C10 C 0.1124(2) 0.15283(16) 0.15837(16) 0.0255(3) Uani 1 1 d . . . C11 C 0.0302(2) 0.08764(17) 0.11898(18) 0.0308(4) Uani 1 1 d . . . H11 H 0.0551 0.0676 0.0438 0.037 Uiso 1 1 calc R . . C12 C -0.0892(2) 0.05227(18) 0.19161(19) 0.0338(4) Uani 1 1 d . . . H12 H -0.1471 0.0088 0.1653 0.041 Uiso 1 1 calc R . . C13 C -0.1238(2) 0.08032(19) 0.30259(19) 0.0342(4) Uani 1 1 d . . . H13 H -0.2039 0.0544 0.3521 0.041 Uiso 1 1 calc R . . C14 C -0.0423(2) 0.14586(18) 0.34174(18) 0.0318(4) Uani 1 1 d . . . H14 H -0.0665 0.1643 0.4177 0.038 Uiso 1 1 calc R . . C15 C 0.0747(2) 0.18424(17) 0.26942(16) 0.0264(4) Uani 1 1 d . . . C16 C 0.2409(2) 0.49310(16) 0.33747(15) 0.0232(3) Uani 1 1 d . . . C17 C 0.2060(2) 0.50906(17) 0.45254(16) 0.0265(4) Uani 1 1 d . . . H17 H 0.2654 0.4463 0.5201 0.032 Uiso 1 1 calc R . . C18 C 0.0838(2) 0.61701(19) 0.46944(19) 0.0335(4) Uani 1 1 d . . . H18 H 0.0596 0.6274 0.5484 0.040 Uiso 1 1 calc R . . C19 C -0.0013(2) 0.70830(19) 0.3713(2) 0.0392(5) Uani 1 1 d . . . H19 H -0.0830 0.7825 0.3828 0.047 Uiso 1 1 calc R . . C20 C 0.0310(3) 0.6928(2) 0.2558(2) 0.0418(5) Uani 1 1 d . . . H20 H -0.0289 0.7557 0.1885 0.050 Uiso 1 1 calc R . . C21 C 0.1512(2) 0.58522(19) 0.23947(18) 0.0346(4) Uani 1 1 d . . . H21 H 0.1727 0.5740 0.1606 0.042 Uiso 1 1 calc R . . C22 C 0.4784(2) 0.25288(16) 0.45503(15) 0.0225(3) Uani 1 1 d . . . C23 C 0.4019(2) 0.16682(19) 0.51867(18) 0.0346(4) Uani 1 1 d . . . H23 H 0.3176 0.1575 0.4815 0.042 Uiso 1 1 calc R . . C24 C 0.4487(3) 0.0947(2) 0.63625(19) 0.0407(5) Uani 1 1 d . . . H24 H 0.3938 0.0382 0.6800 0.049 Uiso 1 1 calc R . . C25 C 0.5738(2) 0.10411(18) 0.68996(17) 0.0316(4) Uani 1 1 d . . . H25 H 0.6048 0.0545 0.7705 0.038 Uiso 1 1 calc R . . C26 C 0.6541(2) 0.18573(19) 0.62660(17) 0.0342(4) Uani 1 1 d . . . H26 H 0.7420 0.1910 0.6629 0.041 Uiso 1 1 calc R . . C27 C 0.6062(2) 0.26032(18) 0.50931(17) 0.0306(4) Uani 1 1 d . . . H27 H 0.6613 0.3168 0.4661 0.037 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.02550(12) 0.02390(12) 0.02114(12) -0.00954(8) -0.00012(8) -0.01008(9) P1 0.0243(2) 0.0239(2) 0.0198(2) -0.00803(16) 0.00135(16) -0.01128(17) N1 0.0279(7) 0.0205(7) 0.0196(7) -0.0063(5) -0.0021(6) -0.0046(6) N2 0.0286(7) 0.0228(7) 0.0234(7) -0.0077(6) -0.0040(6) -0.0093(6) O2 0.0298(6) 0.0351(7) 0.0290(6) -0.0167(5) 0.0031(5) -0.0172(6) C1 0.0251(8) 0.0250(8) 0.0224(8) -0.0048(6) -0.0005(6) -0.0112(7) C2 0.0347(10) 0.0295(9) 0.0258(9) -0.0078(7) 0.0017(7) -0.0160(8) C3 0.0376(10) 0.0321(10) 0.0297(9) -0.0052(7) -0.0021(8) -0.0196(8) C4 0.0321(10) 0.0389(10) 0.0302(9) -0.0020(8) -0.0002(8) -0.0205(8) C5 0.0285(9) 0.0358(10) 0.0250(9) -0.0056(7) 0.0023(7) -0.0126(8) C6 0.0260(8) 0.0257(8) 0.0208(8) -0.0029(6) -0.0012(6) -0.0090(7) C7 0.0272(8) 0.0248(8) 0.0213(8) -0.0061(6) 0.0018(7) -0.0063(7) C8 0.0326(9) 0.0261(9) 0.0237(8) -0.0119(7) -0.0002(7) -0.0062(7) C9 0.0337(9) 0.0178(8) 0.0234(8) -0.0063(6) -0.0071(7) -0.0023(7) O1 0.0413(8) 0.0350(7) 0.0304(7) -0.0173(6) -0.0054(6) -0.0097(6) C10 0.0260(8) 0.0213(8) 0.0292(9) -0.0079(7) -0.0056(7) -0.0056(7) C11 0.0322(9) 0.0268(9) 0.0369(10) -0.0141(8) -0.0081(8) -0.0076(8) C12 0.0328(10) 0.0280(9) 0.0460(11) -0.0133(8) -0.0089(8) -0.0118(8) C13 0.0307(10) 0.0325(10) 0.0454(11) -0.0128(8) 0.0012(8) -0.0161(8) C14 0.0296(9) 0.0348(10) 0.0363(10) -0.0145(8) 0.0009(8) -0.0133(8) C15 0.0254(8) 0.0242(8) 0.0320(9) -0.0105(7) -0.0040(7) -0.0078(7) C16 0.0220(8) 0.0240(8) 0.0275(8) -0.0097(7) -0.0005(6) -0.0100(7) C17 0.0276(9) 0.0276(9) 0.0284(9) -0.0104(7) 0.0017(7) -0.0125(7) C18 0.0326(10) 0.0340(10) 0.0426(11) -0.0193(8) 0.0111(8) -0.0170(8) C19 0.0269(9) 0.0292(10) 0.0645(14) -0.0178(10) 0.0033(9) -0.0095(8) C20 0.0374(11) 0.0300(10) 0.0532(13) -0.0045(9) -0.0166(10) -0.0066(9) C21 0.0408(11) 0.0330(10) 0.0301(9) -0.0076(8) -0.0086(8) -0.0107(8) C22 0.0238(8) 0.0226(8) 0.0217(8) -0.0077(6) 0.0015(6) -0.0074(7) C23 0.0325(10) 0.0398(11) 0.0341(10) -0.0001(8) -0.0069(8) -0.0214(9) C24 0.0407(11) 0.0435(12) 0.0373(11) 0.0068(9) -0.0058(9) -0.0263(10) C25 0.0323(10) 0.0289(9) 0.0274(9) -0.0005(7) -0.0041(7) -0.0073(8) C26 0.0314(10) 0.0389(11) 0.0328(10) -0.0023(8) -0.0081(8) -0.0165(8) C27 0.0307(9) 0.0345(10) 0.0293(9) -0.0036(7) -0.0015(7) -0.0178(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O2 1.8405(12) . ? Ni1 N2 1.8528(14) . ? Ni1 N1 1.8659(14) . ? Ni1 P1 2.1553(5) . ? P1 C1 1.8166(17) . ? P1 C16 1.8181(17) . ? P1 C22 1.8201(17) . ? N1 C7 1.285(2) . ? N1 C8 1.490(2) . ? N2 C9 1.339(2) . ? N2 C10 1.410(2) . ? O2 C15 1.350(2) . ? C1 C2 1.394(2) . ? C1 C6 1.408(2) . ? C2 C3 1.389(3) . ? C3 C4 1.389(3) . ? C4 C5 1.381(3) . ? C5 C6 1.402(2) . ? C6 C7 1.467(2) . ? C8 C9 1.515(3) . ? C9 O1 1.235(2) . ? C10 C11 1.394(2) . ? C10 C15 1.412(2) . ? C11 C12 1.394(3) . ? C12 C13 1.393(3) . ? C13 C14 1.391(3) . ? C14 C15 1.389(3) . ? C16 C17 1.387(2) . ? C16 C21 1.394(2) . ? C17 C18 1.397(3) . ? C18 C19 1.376(3) . ? C19 C20 1.387(3) . ? C20 C21 1.384(3) . ? C22 C27 1.388(2) . ? C22 C23 1.394(2) . ? C23 C24 1.388(3) . ? C24 C25 1.375(3) . ? C25 C26 1.380(3) . ? C26 C27 1.393(3) . ? 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 O2 Ni1 N2 86.95(6) . . ? O2 Ni1 N1 172.19(6) . . ? N2 Ni1 N1 86.20(6) . . ? O2 Ni1 P1 90.24(4) . . ? N2 Ni1 P1 176.78(5) . . ? N1 Ni1 P1 96.70(5) . . ? C1 P1 C16 103.96(8) . . ? C1 P1 C22 106.09(8) . . ? C16 P1 C22 105.25(8) . . ? C1 P1 Ni1 112.35(6) . . ? C16 P1 Ni1 113.34(5) . . ? C22 P1 Ni1 114.91(6) . . ? C7 N1 C8 115.00(15) . . ? C7 N1 Ni1 132.94(12) . . ? C8 N1 Ni1 111.88(11) . . ? C9 N2 C10 127.64(15) . . ? C9 N2 Ni1 118.91(12) . . ? C10 N2 Ni1 112.84(11) . . ? C15 O2 Ni1 111.49(11) . . ? C2 C1 C6 118.92(16) . . ? C2 C1 P1 120.38(13) . . ? C6 C1 P1 120.61(13) . . ? C3 C2 C1 121.51(17) . . ? C2 C3 C4 119.56(17) . . ? C5 C4 C3 119.46(17) . . ? C4 C5 C6 121.77(17) . . ? C5 C6 C1 118.56(16) . . ? C5 C6 C7 115.66(16) . . ? C1 C6 C7 125.68(15) . . ? N1 C7 C6 128.65(16) . . ? N1 C8 C9 110.85(14) . . ? O1 C9 N2 127.92(18) . . ? O1 C9 C8 120.99(16) . . ? N2 C9 C8 111.00(14) . . ? C11 C10 N2 128.67(17) . . ? C11 C10 C15 120.74(17) . . ? N2 C10 C15 110.45(15) . . ? C10 C11 C12 119.03(18) . . ? C13 C12 C11 120.29(17) . . ? C14 C13 C12 120.73(19) . . ? C15 C14 C13 119.77(18) . . ? O2 C15 C14 122.73(16) . . ? O2 C15 C10 117.86(16) . . ? C14 C15 C10 119.40(16) . . ? C17 C16 C21 119.12(17) . . ? C17 C16 P1 123.15(13) . . ? C21 C16 P1 117.73(14) . . ? C16 C17 C18 120.25(17) . . ? C19 C18 C17 119.80(19) . . ? C18 C19 C20 120.58(19) . . ? C21 C20 C19 119.50(19) . . ? C20 C21 C16 120.72(19) . . ? C27 C22 C23 118.81(16) . . ? C27 C22 P1 123.17(13) . . ? C23 C22 P1 117.94(13) . . ? C24 C23 C22 120.13(17) . . ? C25 C24 C23 120.62(18) . . ? C24 C25 C26 119.89(17) . . ? C25 C26 C27 119.91(17) . . ? C22 C27 C26 120.58(17) . . ? 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 O2 Ni1 P1 C1 -170.50(7) . . . . ? N1 Ni1 P1 C1 13.09(8) . . . . ? O2 Ni1 P1 C16 -53.01(7) . . . . ? N1 Ni1 P1 C16 130.58(7) . . . . ? O2 Ni1 P1 C22 68.07(7) . . . . ? N1 Ni1 P1 C22 -108.34(7) . . . . ? N2 Ni1 N1 C7 177.70(17) . . . . ? P1 Ni1 N1 C7 -0.91(17) . . . . ? N2 Ni1 N1 C8 -7.49(11) . . . . ? P1 Ni1 N1 C8 173.90(10) . . . . ? O2 Ni1 N2 C9 -174.70(13) . . . . ? N1 Ni1 N2 C9 1.54(13) . . . . ? O2 Ni1 N2 C10 -2.98(11) . . . . ? N1 Ni1 N2 C10 173.25(12) . . . . ? N2 Ni1 O2 C15 5.51(12) . . . . ? P1 Ni1 O2 C15 -176.06(11) . . . . ? C16 P1 C1 C2 40.49(16) . . . . ? C22 P1 C1 C2 -70.23(16) . . . . ? Ni1 P1 C1 C2 163.42(13) . . . . ? C16 P1 C1 C6 -142.99(14) . . . . ? C22 P1 C1 C6 106.29(14) . . . . ? Ni1 P1 C1 C6 -20.06(16) . . . . ? C6 C1 C2 C3 -3.3(3) . . . . ? P1 C1 C2 C3 173.28(14) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C2 C3 C4 C5 2.8(3) . . . . ? C3 C4 C5 C6 -0.7(3) . . . . ? C4 C5 C6 C1 -3.4(3) . . . . ? C4 C5 C6 C7 173.12(17) . . . . ? C2 C1 C6 C5 5.3(3) . . . . ? P1 C1 C6 C5 -171.27(13) . . . . ? C2 C1 C6 C7 -170.83(17) . . . . ? P1 C1 C6 C7 12.6(2) . . . . ? C8 N1 C7 C6 175.95(16) . . . . ? Ni1 N1 C7 C6 -9.4(3) . . . . ? C5 C6 C7 N1 -172.47(17) . . . . ? C1 C6 C7 N1 3.8(3) . . . . ? C7 N1 C8 C9 -172.63(14) . . . . ? Ni1 N1 C8 C9 11.56(17) . . . . ? C10 N2 C9 O1 11.1(3) . . . . ? Ni1 N2 C9 O1 -178.57(14) . . . . ? C10 N2 C9 C8 -165.57(15) . . . . ? Ni1 N2 C9 C8 4.77(19) . . . . ? N1 C8 C9 O1 172.70(15) . . . . ? N1 C8 C9 N2 -10.4(2) . . . . ? C9 N2 C10 C11 -5.1(3) . . . . ? Ni1 N2 C10 C11 -175.89(15) . . . . ? C9 N2 C10 C15 170.72(16) . . . . ? Ni1 N2 C10 C15 -0.11(18) . . . . ? N2 C10 C11 C12 174.63(17) . . . . ? C15 C10 C11 C12 -0.8(3) . . . . ? C10 C11 C12 C13 -0.9(3) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? C12 C13 C14 C15 0.2(3) . . . . ? Ni1 O2 C15 C14 171.64(14) . . . . ? Ni1 O2 C15 C10 -7.20(19) . . . . ? C13 C14 C15 O2 179.39(17) . . . . ? C13 C14 C15 C10 -1.8(3) . . . . ? C11 C10 C15 O2 -179.02(15) . . . . ? N2 C10 C15 O2 4.8(2) . . . . ? C11 C10 C15 C14 2.1(3) . . . . ? N2 C10 C15 C14 -174.06(16) . . . . ? C1 P1 C16 C17 -107.84(15) . . . . ? C22 P1 C16 C17 3.49(16) . . . . ? Ni1 P1 C16 C17 129.88(13) . . . . ? C1 P1 C16 C21 72.61(15) . . . . ? C22 P1 C16 C21 -176.06(14) . . . . ? Ni1 P1 C16 C21 -49.67(15) . . . . ? C21 C16 C17 C18 -0.9(3) . . . . ? P1 C16 C17 C18 179.59(13) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C17 C18 C19 C20 1.3(3) . . . . ? C18 C19 C20 C21 -0.7(3) . . . . ? C19 C20 C21 C16 -0.7(3) . . . . ? C17 C16 C21 C20 1.5(3) . . . . ? P1 C16 C21 C20 -178.97(16) . . . . ? C1 P1 C22 C27 17.90(17) . . . . ? C16 P1 C22 C27 -91.91(16) . . . . ? Ni1 P1 C22 C27 142.67(14) . . . . ? C1 P1 C22 C23 -165.37(15) . . . . ? C16 P1 C22 C23 84.82(16) . . . . ? Ni1 P1 C22 C23 -40.59(16) . . . . ? C27 C22 C23 C24 3.0(3) . . . . ? P1 C22 C23 C24 -173.91(17) . . . . ? C22 C23 C24 C25 -2.0(3) . . . . ? C23 C24 C25 C26 -0.2(3) . . . . ? C24 C25 C26 C27 1.3(3) . . . . ? C23 C22 C27 C26 -1.8(3) . . . . ? P1 C22 C27 C26 174.91(15) . . . . ? C25 C26 C27 C22 -0.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.868 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.368 _refine_diff_density_min -0.260 _refine_diff_density_rms 0.056 #===END data_11d _database_code_depnum_ccdc_archive 'CCDC 771455' #TrackingRef '- CIF (PNNO, MBSmith).CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H25 N2 O2 P Pt, C1 H1 Cl3' _chemical_formula_sum 'C30 H26 Cl3 N2 O2 P Pt' _chemical_formula_weight 778.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 18.5242(8) _cell_length_b 17.4935(8) _cell_length_c 9.2080(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2983.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10612 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 28.63 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.734 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 5.055 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_T_max 0.632 _exptl_absorpt_process_details 'SADABS v2.10 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25028 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6745 _reflns_number_gt 5392 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0180P)^2^+9.0106P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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, 3115 Friedel pairs' _refine_ls_abs_structure_Flack -0.025(8) _chemical_absolute_configuration ad _refine_ls_number_reflns 6745 _refine_ls_number_parameters 353 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0752 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.472269(10) 0.850543(10) 0.76550(4) 0.02354(6) Uani 1 1 d . . . P1 P 0.54061(8) 0.74747(9) 0.73704(19) 0.0257(5) Uani 1 1 d . . . N1 N 0.5256(3) 0.8860(3) 0.9383(6) 0.0241(11) Uani 1 1 d . . . N2 N 0.4138(3) 0.9454(3) 0.7990(6) 0.0295(15) Uani 1 1 d . . . O2 O 0.4169(3) 0.8207(3) 0.5914(5) 0.0366(12) Uani 1 1 d . . . C1 C 0.6292(3) 0.7590(4) 0.8171(7) 0.0248(14) Uani 1 1 d . . . C2 C 0.6856(3) 0.7113(3) 0.7734(12) 0.0282(12) Uani 1 1 d . . . H2 H 0.6786 0.6764 0.6956 0.034 Uiso 1 1 calc R . . C3 C 0.7530(4) 0.7148(4) 0.8441(8) 0.0325(16) Uani 1 1 d . . . H3 H 0.7910 0.6817 0.8151 0.039 Uiso 1 1 calc R . . C4 C 0.7635(4) 0.7661(4) 0.9548(8) 0.0316(16) Uani 1 1 d . . . H4 H 0.8086 0.7674 1.0038 0.038 Uiso 1 1 calc R . . C5 C 0.7094(4) 0.8158(4) 0.9959(8) 0.0288(14) Uani 1 1 d . . . H5 H 0.7181 0.8519 1.0709 0.035 Uiso 1 1 calc R . . C6 C 0.6411(4) 0.8136(4) 0.9277(7) 0.0244(13) Uani 1 1 d . . . C7 C 0.5893(4) 0.8692(4) 0.9838(7) 0.0259(14) Uani 1 1 d . . . H7 H 0.6050 0.8972 1.0664 0.031 Uiso 1 1 calc R . . C8 C 0.4823(4) 0.9421(4) 1.0241(7) 0.0309(15) Uani 1 1 d . . . H8 H 0.5154 0.9739 1.0849 0.037 Uiso 1 1 calc R . . C9 C 0.4312(4) 0.8985(5) 1.1219(8) 0.0409(19) Uani 1 1 d . . . H9A H 0.3937 0.8742 1.0629 0.061 Uiso 1 1 calc R . . H9B H 0.4088 0.9338 1.1911 0.061 Uiso 1 1 calc R . . H9C H 0.4582 0.8592 1.1750 0.061 Uiso 1 1 calc R . . C10 C 0.4430(4) 0.9931(4) 0.9173(8) 0.0336(16) Uani 1 1 d . . . H10A H 0.4033 1.0203 0.9670 0.040 Uiso 1 1 calc R . . H10B H 0.4768 1.0315 0.8771 0.040 Uiso 1 1 calc R . . C11 C 0.3603(4) 0.9742(4) 0.7184(7) 0.0291(16) Uani 1 1 d . . . O1 O 0.3358(2) 1.0405(2) 0.7406(6) 0.0322(14) Uani 1 1 d . . . C12 C 0.3297(4) 0.9276(4) 0.5975(7) 0.0278(14) Uani 1 1 d . . . C13 C 0.3586(4) 0.8581(4) 0.5424(7) 0.0280(14) Uani 1 1 d . . . C14 C 0.3239(4) 0.8225(4) 0.4241(8) 0.0345(16) Uani 1 1 d . . . H14 H 0.3439 0.7767 0.3858 0.041 Uiso 1 1 calc R . . C15 C 0.2628(4) 0.8515(4) 0.3626(8) 0.0386(17) Uani 1 1 d . . . H15 H 0.2403 0.8257 0.2838 0.046 Uiso 1 1 calc R . . C16 C 0.2335(4) 0.9190(5) 0.4162(9) 0.0403(18) Uani 1 1 d . . . H16 H 0.1909 0.9395 0.3742 0.048 Uiso 1 1 calc R . . C17 C 0.2666(4) 0.9562(4) 0.5308(8) 0.0362(17) Uani 1 1 d . . . H17 H 0.2461 1.0025 0.5658 0.043 Uiso 1 1 calc R . . C18 C 0.5026(4) 0.6631(4) 0.8201(7) 0.0268(14) Uani 1 1 d . . . C19 C 0.4278(4) 0.6521(4) 0.8115(8) 0.042(2) Uani 1 1 d . . . H19 H 0.3992 0.6865 0.7563 0.051 Uiso 1 1 calc R . . C20 C 0.3955(4) 0.5921(5) 0.8818(10) 0.046(2) Uani 1 1 d . . . H20 H 0.3448 0.5854 0.8737 0.055 Uiso 1 1 calc R . . C21 C 0.4354(4) 0.5413(4) 0.9645(9) 0.044(2) Uani 1 1 d . . . H21 H 0.4123 0.5010 1.0158 0.053 Uiso 1 1 calc R . . C22 C 0.5094(4) 0.5504(4) 0.9706(8) 0.0369(18) Uani 1 1 d . . . H22 H 0.5375 0.5149 1.0244 0.044 Uiso 1 1 calc R . . C23 C 0.5432(4) 0.6098(4) 0.9003(9) 0.0343(17) Uani 1 1 d . . . H23 H 0.5942 0.6149 0.9059 0.041 Uiso 1 1 calc R . . C24 C 0.5566(3) 0.7264(4) 0.5474(7) 0.0244(14) Uani 1 1 d . . . C25 C 0.5300(4) 0.6612(4) 0.4779(8) 0.0368(17) Uani 1 1 d . . . H25 H 0.5060 0.6227 0.5322 0.044 Uiso 1 1 calc R . . C26 C 0.5389(4) 0.6531(5) 0.3288(8) 0.0451(19) Uani 1 1 d . . . H26 H 0.5201 0.6093 0.2809 0.054 Uiso 1 1 calc R . . C27 C 0.5746(4) 0.7081(4) 0.2505(13) 0.0450(19) Uani 1 1 d . . . H27 H 0.5808 0.7019 0.1487 0.054 Uiso 1 1 calc R . . C28 C 0.6016(4) 0.7720(4) 0.3180(8) 0.0402(18) Uani 1 1 d . . . H28 H 0.6265 0.8097 0.2631 0.048 Uiso 1 1 calc R . . C29 C 0.5927(4) 0.7813(4) 0.4650(8) 0.0328(16) Uani 1 1 d . . . H29 H 0.6113 0.8256 0.5112 0.039 Uiso 1 1 calc R . . C30 C 0.7735(5) 0.9351(5) 0.4648(10) 0.058(3) Uani 1 1 d . . . H30 H 0.7310 0.9342 0.3981 0.070 Uiso 1 1 calc R . . Cl1 Cl 0.78382(16) 1.02929(16) 0.5284(3) 0.0794(8) Uani 1 1 d . . . Cl2 Cl 0.85114(18) 0.9085(2) 0.3617(5) 0.1138(14) Uani 1 1 d . . . Cl3 Cl 0.7586(2) 0.8693(2) 0.5984(4) 0.1399(19) 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 Pt1 0.02266(10) 0.02000(9) 0.02795(10) -0.0020(2) -0.0013(2) 0.00169(9) P1 0.0225(8) 0.0206(7) 0.0340(15) -0.0022(7) -0.0027(7) 0.0002(6) N1 0.022(3) 0.022(3) 0.028(3) -0.006(2) -0.002(2) -0.001(2) N2 0.027(3) 0.026(2) 0.036(5) -0.008(2) 0.003(2) 0.001(2) O2 0.032(3) 0.036(3) 0.042(3) -0.011(2) -0.013(2) 0.010(2) C1 0.021(3) 0.024(3) 0.029(3) -0.002(2) 0.004(2) 0.001(3) C2 0.025(3) 0.028(3) 0.032(3) -0.003(5) -0.002(4) 0.000(2) C3 0.025(4) 0.034(4) 0.039(4) 0.000(3) -0.001(3) 0.003(3) C4 0.019(4) 0.038(4) 0.037(4) 0.006(3) -0.007(3) 0.002(3) C5 0.029(4) 0.029(3) 0.029(3) -0.003(3) -0.003(3) -0.008(3) C6 0.025(3) 0.025(3) 0.023(3) 0.005(3) 0.000(3) -0.006(3) C7 0.028(4) 0.025(3) 0.025(3) -0.002(3) -0.006(3) -0.003(3) C8 0.028(4) 0.029(3) 0.036(4) -0.011(3) -0.002(3) 0.005(3) C9 0.042(5) 0.045(5) 0.035(4) 0.005(3) 0.007(3) 0.009(4) C10 0.038(4) 0.024(3) 0.039(4) -0.008(3) 0.007(3) 0.000(3) C11 0.023(3) 0.028(3) 0.036(4) 0.006(3) 0.010(3) 0.000(3) O1 0.034(2) 0.023(2) 0.040(4) 0.004(2) 0.002(2) 0.0075(17) C12 0.025(3) 0.027(3) 0.032(4) 0.008(3) 0.001(3) -0.002(3) C13 0.022(3) 0.029(4) 0.033(4) 0.001(3) 0.001(3) 0.001(3) C14 0.030(4) 0.036(4) 0.037(4) 0.001(3) -0.005(3) 0.005(3) C15 0.034(4) 0.042(4) 0.040(4) 0.004(4) -0.007(3) -0.001(4) C16 0.032(4) 0.047(5) 0.041(4) 0.002(4) -0.011(3) 0.014(4) C17 0.039(4) 0.036(4) 0.034(4) 0.010(3) 0.003(3) 0.005(3) C18 0.023(3) 0.028(4) 0.029(3) -0.003(3) -0.001(3) 0.001(3) C19 0.031(4) 0.027(3) 0.068(6) 0.010(3) -0.007(3) 0.005(3) C20 0.021(4) 0.043(5) 0.074(6) 0.001(4) 0.005(4) -0.004(3) C21 0.039(5) 0.029(4) 0.065(6) 0.007(4) 0.006(4) -0.003(3) C22 0.037(4) 0.025(3) 0.048(5) 0.009(3) -0.005(3) -0.003(3) C23 0.031(4) 0.025(4) 0.048(4) -0.001(3) -0.007(3) -0.001(3) C24 0.024(3) 0.027(3) 0.023(3) -0.001(3) -0.001(3) 0.006(3) C25 0.046(4) 0.030(4) 0.034(4) -0.006(3) -0.001(3) -0.012(3) C26 0.059(5) 0.043(4) 0.033(4) -0.011(4) -0.003(4) -0.011(4) C27 0.054(4) 0.050(4) 0.031(5) -0.002(5) 0.003(5) 0.004(3) C28 0.049(5) 0.039(4) 0.033(4) 0.004(3) 0.004(3) -0.003(4) C29 0.038(4) 0.026(3) 0.035(4) -0.006(3) -0.005(3) -0.007(3) C30 0.062(6) 0.052(6) 0.061(6) 0.022(5) -0.019(5) -0.016(5) Cl1 0.0687(18) 0.0749(18) 0.094(2) -0.0133(16) 0.0187(16) -0.0130(15) Cl2 0.0661(19) 0.085(2) 0.190(4) -0.028(2) 0.006(2) 0.0095(17) Cl3 0.125(3) 0.161(4) 0.133(3) 0.103(3) -0.071(3) -0.090(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 Pt1 N1 1.973(5) . ? Pt1 O2 1.974(5) . ? Pt1 N2 2.006(5) . ? Pt1 P1 2.2187(16) . ? P1 C18 1.806(7) . ? P1 C1 1.810(7) . ? P1 C24 1.810(7) . ? N1 C7 1.287(8) . ? N1 C8 1.494(8) . ? N2 C11 1.336(8) . ? N2 C10 1.475(8) . ? O2 C13 1.341(8) . ? C1 C2 1.397(8) . ? C1 C6 1.414(9) . ? C2 C3 1.409(10) . ? C3 C4 1.372(10) . ? C4 C5 1.380(10) . ? C5 C6 1.413(9) . ? C6 C7 1.460(9) . ? C8 C9 1.513(10) . ? C8 C10 1.513(10) . ? C11 O1 1.262(7) . ? C11 C12 1.492(9) . ? C12 C17 1.413(10) . ? C12 C13 1.422(9) . ? C13 C14 1.409(10) . ? C14 C15 1.364(10) . ? C15 C16 1.390(11) . ? C16 C17 1.383(11) . ? C18 C19 1.401(10) . ? C18 C23 1.406(10) . ? C19 C20 1.370(11) . ? C20 C21 1.384(11) . ? C21 C22 1.382(10) . ? C22 C23 1.375(10) . ? C24 C25 1.397(9) . ? C24 C29 1.394(9) . ? C25 C26 1.390(10) . ? C26 C27 1.372(11) . ? C27 C28 1.374(11) . ? C28 C29 1.373(10) . ? C30 Cl3 1.708(9) . ? C30 Cl1 1.759(10) . ? C30 Cl2 1.784(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 O2 176.9(2) . . ? N1 Pt1 N2 83.4(2) . . ? O2 Pt1 N2 93.6(2) . . ? N1 Pt1 P1 93.75(16) . . ? O2 Pt1 P1 89.19(14) . . ? N2 Pt1 P1 177.18(16) . . ? C18 P1 C1 105.8(3) . . ? C18 P1 C24 107.8(3) . . ? C1 P1 C24 105.5(3) . . ? C18 P1 Pt1 113.1(2) . . ? C1 P1 Pt1 112.3(2) . . ? C24 P1 Pt1 111.9(2) . . ? C7 N1 C8 118.1(5) . . ? C7 N1 Pt1 130.5(5) . . ? C8 N1 Pt1 111.4(4) . . ? C11 N2 C10 118.0(5) . . ? C11 N2 Pt1 128.8(4) . . ? C10 N2 Pt1 112.5(4) . . ? C13 O2 Pt1 124.3(4) . . ? C2 C1 C6 119.7(6) . . ? C2 C1 P1 119.6(5) . . ? C6 C1 P1 120.6(5) . . ? C1 C2 C3 120.2(8) . . ? C4 C3 C2 119.9(7) . . ? C3 C4 C5 120.8(6) . . ? C4 C5 C6 120.8(6) . . ? C5 C6 C1 118.5(6) . . ? C5 C6 C7 114.4(6) . . ? C1 C6 C7 127.1(6) . . ? N1 C7 C6 129.8(6) . . ? N1 C8 C9 108.6(6) . . ? N1 C8 C10 107.5(5) . . ? C9 C8 C10 112.6(6) . . ? N2 C10 C8 108.9(5) . . ? O1 C11 N2 121.5(6) . . ? O1 C11 C12 119.1(6) . . ? N2 C11 C12 119.3(6) . . ? C17 C12 C13 117.3(6) . . ? C17 C12 C11 116.4(6) . . ? C13 C12 C11 126.2(6) . . ? O2 C13 C14 114.3(6) . . ? O2 C13 C12 126.8(6) . . ? C14 C13 C12 118.8(6) . . ? C15 C14 C13 122.3(7) . . ? C14 C15 C16 119.5(7) . . ? C17 C16 C15 119.9(7) . . ? C16 C17 C12 122.1(7) . . ? C19 C18 C23 117.9(6) . . ? C19 C18 P1 118.3(5) . . ? C23 C18 P1 123.7(5) . . ? C20 C19 C18 120.7(7) . . ? C19 C20 C21 121.2(7) . . ? C22 C21 C20 118.5(7) . . ? C23 C22 C21 121.3(7) . . ? C22 C23 C18 120.3(7) . . ? C25 C24 C29 118.8(6) . . ? C25 C24 P1 123.4(5) . . ? C29 C24 P1 117.6(5) . . ? C26 C25 C24 119.6(7) . . ? C27 C26 C25 120.3(8) . . ? C26 C27 C28 120.5(10) . . ? C29 C28 C27 119.9(8) . . ? C28 C29 C24 120.8(6) . . ? Cl3 C30 Cl1 114.2(6) . . ? Cl3 C30 Cl2 109.8(6) . . ? Cl1 C30 Cl2 109.5(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 N1 Pt1 P1 C18 95.3(3) . . . . ? O2 Pt1 P1 C18 -85.7(3) . . . . ? N1 Pt1 P1 C1 -24.2(3) . . . . ? O2 Pt1 P1 C1 154.7(3) . . . . ? N1 Pt1 P1 C24 -142.7(3) . . . . ? O2 Pt1 P1 C24 36.3(3) . . . . ? N2 Pt1 N1 C7 -159.9(6) . . . . ? P1 Pt1 N1 C7 19.8(6) . . . . ? N2 Pt1 N1 C8 19.2(4) . . . . ? P1 Pt1 N1 C8 -161.1(4) . . . . ? N1 Pt1 N2 C11 175.6(6) . . . . ? O2 Pt1 N2 C11 -3.4(6) . . . . ? N1 Pt1 N2 C10 5.4(4) . . . . ? O2 Pt1 N2 C10 -173.6(4) . . . . ? N2 Pt1 O2 C13 -4.4(5) . . . . ? P1 Pt1 O2 C13 175.9(5) . . . . ? C18 P1 C1 C2 75.6(6) . . . . ? C24 P1 C1 C2 -38.5(7) . . . . ? Pt1 P1 C1 C2 -160.7(5) . . . . ? C18 P1 C1 C6 -101.9(6) . . . . ? C24 P1 C1 C6 144.0(5) . . . . ? Pt1 P1 C1 C6 21.9(6) . . . . ? C6 C1 C2 C3 3.3(11) . . . . ? P1 C1 C2 C3 -174.1(6) . . . . ? C1 C2 C3 C4 -1.0(12) . . . . ? C2 C3 C4 C5 -1.6(11) . . . . ? C3 C4 C5 C6 1.8(11) . . . . ? C4 C5 C6 C1 0.5(10) . . . . ? C4 C5 C6 C7 179.5(6) . . . . ? C2 C1 C6 C5 -3.0(10) . . . . ? P1 C1 C6 C5 174.4(5) . . . . ? C2 C1 C6 C7 178.1(7) . . . . ? P1 C1 C6 C7 -4.4(9) . . . . ? C8 N1 C7 C6 175.8(6) . . . . ? Pt1 N1 C7 C6 -5.2(11) . . . . ? C5 C6 C7 N1 173.7(7) . . . . ? C1 C6 C7 N1 -7.4(12) . . . . ? C7 N1 C8 C9 -97.8(7) . . . . ? Pt1 N1 C8 C9 83.0(6) . . . . ? C7 N1 C8 C10 140.1(6) . . . . ? Pt1 N1 C8 C10 -39.1(6) . . . . ? C11 N2 C10 C8 160.4(6) . . . . ? Pt1 N2 C10 C8 -28.2(7) . . . . ? N1 C8 C10 N2 42.8(7) . . . . ? C9 C8 C10 N2 -76.7(7) . . . . ? C10 N2 C11 O1 0.9(9) . . . . ? Pt1 N2 C11 O1 -168.8(5) . . . . ? C10 N2 C11 C12 179.8(6) . . . . ? Pt1 N2 C11 C12 10.0(8) . . . . ? O1 C11 C12 C17 -10.3(9) . . . . ? N2 C11 C12 C17 170.8(6) . . . . ? O1 C11 C12 C13 168.7(6) . . . . ? N2 C11 C12 C13 -10.1(10) . . . . ? Pt1 O2 C13 C14 -174.5(5) . . . . ? Pt1 O2 C13 C12 5.3(9) . . . . ? C17 C12 C13 O2 -178.8(6) . . . . ? C11 C12 C13 O2 2.2(11) . . . . ? C17 C12 C13 C14 1.1(9) . . . . ? C11 C12 C13 C14 -178.0(6) . . . . ? O2 C13 C14 C15 178.4(7) . . . . ? C12 C13 C14 C15 -1.5(11) . . . . ? C13 C14 C15 C16 0.9(12) . . . . ? C14 C15 C16 C17 0.1(12) . . . . ? C15 C16 C17 C12 -0.5(12) . . . . ? C13 C12 C17 C16 -0.1(10) . . . . ? C11 C12 C17 C16 179.0(7) . . . . ? C1 P1 C18 C19 162.0(5) . . . . ? C24 P1 C18 C19 -85.5(6) . . . . ? Pt1 P1 C18 C19 38.8(6) . . . . ? C1 P1 C18 C23 -14.2(7) . . . . ? C24 P1 C18 C23 98.3(6) . . . . ? Pt1 P1 C18 C23 -137.5(5) . . . . ? C23 C18 C19 C20 1.4(11) . . . . ? P1 C18 C19 C20 -175.1(6) . . . . ? C18 C19 C20 C21 0.7(13) . . . . ? C19 C20 C21 C22 -2.4(13) . . . . ? C20 C21 C22 C23 2.0(12) . . . . ? C21 C22 C23 C18 0.1(12) . . . . ? C19 C18 C23 C22 -1.7(11) . . . . ? P1 C18 C23 C22 174.5(6) . . . . ? C18 P1 C24 C25 11.4(7) . . . . ? C1 P1 C24 C25 124.0(6) . . . . ? Pt1 P1 C24 C25 -113.6(6) . . . . ? C18 P1 C24 C29 -173.7(5) . . . . ? C1 P1 C24 C29 -61.1(6) . . . . ? Pt1 P1 C24 C29 61.3(6) . . . . ? C29 C24 C25 C26 -1.1(11) . . . . ? P1 C24 C25 C26 173.8(6) . . . . ? C24 C25 C26 C27 1.1(12) . . . . ? C25 C26 C27 C28 -0.5(12) . . . . ? C26 C27 C28 C29 -0.2(12) . . . . ? C27 C28 C29 C24 0.2(12) . . . . ? C25 C24 C29 C28 0.4(11) . . . . ? P1 C24 C29 C28 -174.7(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.956 _refine_diff_density_min -1.482 _refine_diff_density_rms 0.128 #===END