# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full J.Mater.Chem. _journal_coden_cambridge 1145 #TrackingRef 'acrispini.CIF' _publ_contact_author_name 'Crispini, Alessandra' _publ_contact_author_address ; Dipartimento di Scienze Farmaceutiche Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; _publ_contact_author_email a.crispini@unical.it _publ_contact_author_fax 0984492066 _publ_contact_author_phone 0984492888 _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a Paper in Advanced Chemistry Of Materials ; _publ_requested_category FC _publ_section_title ; Impact of geometrical distorsions on the photoconductivity of organometallic Pd(II) and Pt(II) complexes ; _publ_section_title_footnote ; ? ; loop_ _publ_author_name _publ_author_address M.Ghedini ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; A.Golemme ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; I.Aiello ; Dipartimento di Scienze Farmaceutiche Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; N.Godbert ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; R.Termine ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; A.Crispini ; Dipartimento di Scienze Farmaceutiche Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; 'M.La Deda' ; Dipartimento di Chimica Universit\'a della Calabria 87030 Arcavacata di Rende (CS) Italy ; F.Lelj ; Dipartimento di Chimica Universit\'a degli Studi della Basilicata 85100 Potenza Italy ; A.Francesco ; Dipartimento di Chimica Universit\'a degli Studi della Basilicata 85100 Potenza Italy ; M.Amati ; Dipartimento di Chimica Universit\'a degli Studi della Basilicata 85100 Potenza Italy ; S.Belviso '' data_(AZPdON) _database_code_depnum_ccdc_archive 'CCDC 776860' #TrackingRef 'acrispini.CIF' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C74 H86 N6 O4 Pd2' _chemical_formula_sum 'C74 H86 N6 O4 Pd2' _chemical_formula_weight 1336.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.992(3) _cell_length_b 13.924(3) _cell_length_c 18.886(4) _cell_angle_alpha 95.33(3) _cell_angle_beta 91.63(3) _cell_angle_gamma 92.20(3) _cell_volume 3397.4(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3560 _cell_measurement_theta_min 2.93 _cell_measurement_theta_max 30.16 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.306 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.581 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.785 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12609 _diffrn_reflns_av_R_equivalents 0.0240 _diffrn_reflns_av_sigmaI/netI 0.0515 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 25.05 _reflns_number_total 12029 _reflns_number_gt 7668 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^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 12029 _refine_ls_number_parameters 775 _refine_ls_number_restraints 34 _refine_ls_R_factor_all 0.0743 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd1 Pd 0.20063(2) 0.28875(2) 0.385283(15) 0.05403(10) Uani 1 1 d . . . Pd2 Pd 1.30441(2) 0.19867(2) 0.689093(16) 0.06198(11) Uani 1 1 d . . . O1 O 0.3209(2) 0.3187(2) 0.32256(14) 0.0683(7) Uani 1 1 d . . . O2 O 0.6706(2) 0.3468(3) 0.2615(2) 0.1000(11) Uani 1 1 d . . . O3 O 1.3678(2) 0.1664(2) 0.59267(15) 0.0732(8) Uani 1 1 d . . . O4 O 1.4044(3) 0.0356(2) 0.35446(16) 0.0813(9) Uani 1 1 d . . . N1 N 0.2787(2) 0.3668(2) 0.46758(16) 0.0534(8) Uani 1 1 d . . . N2 N 0.1198(3) 0.2140(2) 0.30322(17) 0.0605(8) Uani 1 1 d . . . N3 N 0.0257(3) 0.1908(2) 0.3113(2) 0.0729(10) Uani 1 1 d . . . N4 N 1.1673(3) 0.1356(2) 0.65163(19) 0.0650(9) Uani 1 1 d . . . N5 N 1.4313(3) 0.2822(2) 0.72147(18) 0.0651(9) Uani 1 1 d . . . N6 N 1.4289(3) 0.3342(3) 0.7806(2) 0.0822(11) Uani 1 1 d . . . C1 C 0.3797(3) 0.3741(3) 0.4707(2) 0.0580(10) Uani 1 1 d . . . H1B H 0.4096 0.3974 0.5146 0.070 Uiso 1 1 calc R . . C2 C 0.4488(3) 0.3510(3) 0.4159(2) 0.0570(10) Uani 1 1 d . . . C3 C 0.5558(3) 0.3627(3) 0.4321(2) 0.0707(11) Uani 1 1 d . . . H3C H 0.5777 0.3744 0.4795 0.085 Uiso 1 1 calc R . . C4 C 0.6284(3) 0.3575(3) 0.3811(3) 0.0790(13) Uani 1 1 d . . . H4B H 0.6983 0.3622 0.3936 0.095 Uiso 1 1 calc R . . C5 C 0.5950(4) 0.3449(3) 0.3102(3) 0.0763(13) Uani 1 1 d . . . C6 C 0.4913(3) 0.3310(3) 0.2916(2) 0.0669(11) Uani 1 1 d . . . H6B H 0.4711 0.3208 0.2437 0.080 Uiso 1 1 calc R . . C7 C 0.4168(3) 0.3318(3) 0.3432(2) 0.0566(10) Uani 1 1 d . . . C8 C 0.6409(5) 0.3506(6) 0.1887(3) 0.137(2) Uani 1 1 d U . . H8A H 0.5928 0.4014 0.1839 0.164 Uiso 1 1 calc R . . H8B H 0.6079 0.2896 0.1695 0.164 Uiso 1 1 calc R . . C9 C 0.7385(7) 0.3708(9) 0.1494(5) 0.214(4) Uani 1 1 d U . . H9A H 0.7658 0.4350 0.1662 0.257 Uiso 1 1 calc R . . H9B H 0.7893 0.3253 0.1616 0.257 Uiso 1 1 calc R . . C10 C 0.7270(10) 0.3653(9) 0.0777(6) 0.275(6) Uani 1 1 d DU . . H10A H 0.6751 0.4098 0.0657 0.330 Uiso 1 1 calc R . . H10B H 0.7010 0.3007 0.0609 0.330 Uiso 1 1 calc R . . C11 C 0.8333(12) 0.3895(11) 0.0341(8) 0.277(7) Uani 1 1 d DU . . H11A H 0.8142 0.3961 -0.0152 0.333 Uiso 1 1 calc R . . H11B H 0.8641 0.4509 0.0543 0.333 Uiso 1 1 calc R . . C12 C 0.8970(12) 0.3286(16) 0.0359(13) 0.430(18) Uani 1 1 d D . . H12A H 0.8679 0.2646 0.0204 0.516 Uiso 1 1 calc R . . H12B H 0.9285 0.3284 0.0831 0.516 Uiso 1 1 calc R . . C13 C 0.9727(10) 0.3638(9) -0.0167(7) 0.311(8) Uani 1 1 d D . . H13A H 1.0279 0.3200 -0.0220 0.467 Uiso 1 1 calc R . . H13B H 1.0002 0.4269 0.0005 0.467 Uiso 1 1 calc R . . H13C H 0.9379 0.3667 -0.0620 0.467 Uiso 1 1 calc R . . C14 C 0.2272(3) 0.4144(3) 0.5269(2) 0.0543(9) Uani 1 1 d . . . C15 C 0.2509(3) 0.3954(3) 0.5963(2) 0.0632(10) Uani 1 1 d . . . H15A H 0.3018 0.3526 0.6053 0.076 Uiso 1 1 calc R . . C16 C 0.1983(4) 0.4403(3) 0.6518(2) 0.0744(12) Uani 1 1 d . . . H16A H 0.2145 0.4272 0.6981 0.089 Uiso 1 1 calc R . . C17 C 0.1218(4) 0.5046(3) 0.6401(3) 0.0748(12) Uani 1 1 d . . . C18 C 0.1032(3) 0.5236(3) 0.5708(3) 0.0701(12) Uani 1 1 d . . . H18A H 0.0544 0.5685 0.5617 0.084 Uiso 1 1 calc R . . C19 C 0.1536(3) 0.4791(3) 0.5143(2) 0.0605(10) Uani 1 1 d . . . H19A H 0.1377 0.4928 0.4681 0.073 Uiso 1 1 calc R . . C20 C 0.0646(4) 0.5510(4) 0.7012(3) 0.1052(18) Uani 1 1 d . . . H20A H 0.1086 0.5527 0.7437 0.126 Uiso 1 1 calc R . . H20B H 0.0535 0.6173 0.6922 0.126 Uiso 1 1 calc R . . C21 C -0.0341(4) 0.5063(4) 0.7162(3) 0.0880(14) Uani 1 1 d . . . H21A H -0.0225 0.4393 0.7231 0.106 Uiso 1 1 calc R . . H21B H -0.0778 0.5061 0.6737 0.106 Uiso 1 1 calc R . . C22 C -0.0929(4) 0.5458(4) 0.7761(3) 0.0952(16) Uani 1 1 d . . . H22A H -0.0478 0.5464 0.8180 0.114 Uiso 1 1 calc R . . H22B H -0.1032 0.6128 0.7686 0.114 Uiso 1 1 calc R . . C23 C -0.1909(4) 0.5065(5) 0.7952(3) 0.115(2) Uani 1 1 d . . . H23A H -0.1803 0.4407 0.8058 0.138 Uiso 1 1 calc R . . H23B H -0.2355 0.5026 0.7529 0.138 Uiso 1 1 calc R . . C24 C -0.2489(5) 0.5517(5) 0.8534(3) 0.134(2) Uani 1 1 d . . . H24A H -0.2049 0.5541 0.8959 0.161 Uiso 1 1 calc R . . H24B H -0.2579 0.6180 0.8434 0.161 Uiso 1 1 calc R . . C25 C -0.3472(5) 0.5141(6) 0.8715(4) 0.160(3) Uani 1 1 d . . . H25A H -0.3728 0.5542 0.9106 0.239 Uiso 1 1 calc R . . H25B H -0.3408 0.4496 0.8847 0.239 Uiso 1 1 calc R . . H25C H -0.3941 0.5132 0.8312 0.239 Uiso 1 1 calc R . . C26 C 0.0712(3) 0.2544(3) 0.4321(2) 0.0581(10) Uani 1 1 d . . . C27 C 0.0385(3) 0.2629(3) 0.5020(2) 0.0674(11) Uani 1 1 d . . . H27A H 0.0843 0.2879 0.5384 0.081 Uiso 1 1 calc R . . C28 C -0.0610(4) 0.2349(3) 0.5184(3) 0.0785(13) Uani 1 1 d . . . H28A H -0.0799 0.2405 0.5657 0.094 Uiso 1 1 calc R . . C29 C -0.1321(4) 0.1992(4) 0.4667(3) 0.0935(16) Uani 1 1 d . . . H29A H -0.1989 0.1823 0.4787 0.112 Uiso 1 1 calc R . . C30 C -0.1040(3) 0.1886(3) 0.3973(3) 0.0849(14) Uani 1 1 d . . . H30A H -0.1516 0.1655 0.3615 0.102 Uiso 1 1 calc R . . C31 C -0.0039(3) 0.2127(3) 0.3812(2) 0.0666(11) Uani 1 1 d . . . C32 C 0.1554(3) 0.1871(3) 0.2324(2) 0.0639(11) Uani 1 1 d . . . C33 C 0.2548(3) 0.1579(3) 0.2254(2) 0.0733(12) Uani 1 1 d . . . H33A H 0.2984 0.1566 0.2652 0.088 Uiso 1 1 calc R . . C34 C 0.2885(4) 0.1303(4) 0.1578(3) 0.0971(16) Uani 1 1 d . . . H34A H 0.3554 0.1103 0.1520 0.116 Uiso 1 1 calc R . . C35 C 0.2237(5) 0.1323(4) 0.0996(3) 0.1081(18) Uani 1 1 d . . . H35A H 0.2472 0.1145 0.0544 0.130 Uiso 1 1 calc R . . C36 C 0.1246(5) 0.1605(4) 0.1075(3) 0.1027(17) Uani 1 1 d . . . H36A H 0.0806 0.1610 0.0678 0.123 Uiso 1 1 calc R . . C37 C 0.0900(4) 0.1881(3) 0.1742(3) 0.0835(13) Uani 1 1 d . . . H37A H 0.0228 0.2074 0.1797 0.100 Uiso 1 1 calc R . . C38 C 1.1543(3) 0.0915(3) 0.5874(2) 0.0699(11) Uani 1 1 d . . . H38A H 1.0883 0.0651 0.5764 0.084 Uiso 1 1 calc R . . C39 C 1.2251(3) 0.0778(3) 0.5321(2) 0.0658(11) Uani 1 1 d . . . C40 C 1.3284(3) 0.1171(3) 0.5363(2) 0.0618(10) Uani 1 1 d . . . C41 C 1.3892(3) 0.1024(3) 0.4765(2) 0.0663(11) Uani 1 1 d . . . H41A H 1.4570 0.1266 0.4789 0.080 Uiso 1 1 calc R . . C42 C 1.3516(4) 0.0537(3) 0.4149(2) 0.0692(11) Uani 1 1 d . . . C43 C 1.2492(4) 0.0173(3) 0.4096(3) 0.0799(13) Uani 1 1 d . . . H43A H 1.2226 -0.0151 0.3673 0.096 Uiso 1 1 calc R . . C44 C 1.1901(4) 0.0300(3) 0.4668(3) 0.0803(13) Uani 1 1 d . . . H44A H 1.1223 0.0058 0.4628 0.096 Uiso 1 1 calc R . . C45 C 1.5108(4) 0.0677(3) 0.3544(2) 0.0775(12) Uani 1 1 d . . . H45A H 1.5513 0.0349 0.3880 0.093 Uiso 1 1 calc R . . H45B H 1.5180 0.1367 0.3676 0.093 Uiso 1 1 calc R . . C46 C 1.5467(4) 0.0436(4) 0.2792(2) 0.0866(14) Uani 1 1 d . . . H46A H 1.5364 -0.0254 0.2670 0.104 Uiso 1 1 calc R . . H46B H 1.5035 0.0758 0.2468 0.104 Uiso 1 1 calc R . . C47 C 1.6559(4) 0.0711(4) 0.2679(3) 0.0927(15) Uani 1 1 d . . . H47A H 1.6999 0.0372 0.2987 0.111 Uiso 1 1 calc R . . H47B H 1.6674 0.1398 0.2809 0.111 Uiso 1 1 calc R . . C48 C 1.6857(4) 0.0471(4) 0.1896(3) 0.1049(17) Uani 1 1 d . . . H48A H 1.6742 -0.0218 0.1774 0.126 Uiso 1 1 calc R . . H48B H 1.6397 0.0797 0.1593 0.126 Uiso 1 1 calc R . . C49 C 1.7922(5) 0.0736(6) 0.1732(4) 0.147(3) Uani 1 1 d . . . H49A H 1.8389 0.0417 0.2035 0.177 Uiso 1 1 calc R . . H49B H 1.8039 0.1427 0.1838 0.177 Uiso 1 1 calc R . . C50 C 1.8160(6) 0.0461(6) 0.0963(4) 0.164(3) Uani 1 1 d . . . H50A H 1.8866 0.0639 0.0884 0.246 Uiso 1 1 calc R . . H50B H 1.7717 0.0793 0.0660 0.246 Uiso 1 1 calc R . . H50C H 1.8049 -0.0223 0.0855 0.246 Uiso 1 1 calc R . . C51 C 1.0735(3) 0.1411(3) 0.6906(2) 0.0699(11) Uani 1 1 d . . . C52 C 1.0245(4) 0.0594(3) 0.7111(3) 0.0864(14) Uani 1 1 d . . . H52A H 1.0511 -0.0008 0.6991 0.104 Uiso 1 1 calc R . . C53 C 0.9364(5) 0.0664(4) 0.7493(3) 0.1120(19) Uani 1 1 d . . . H53A H 0.9047 0.0107 0.7635 0.134 Uiso 1 1 calc R . . C54 C 0.8944(5) 0.1531(5) 0.7668(4) 0.127(2) Uani 1 1 d D . . C55 C 0.9433(5) 0.2342(4) 0.7444(3) 0.117(2) Uani 1 1 d . . . H55A H 0.9149 0.2940 0.7549 0.140 Uiso 1 1 calc R . . C56 C 1.0326(4) 0.2293(3) 0.7073(3) 0.0888(15) Uani 1 1 d . . . H56A H 1.0648 0.2851 0.6936 0.107 Uiso 1 1 calc R . . C57 C 0.8066(7) 0.1612(9) 0.8237(8) 0.292(9) Uani 1 1 d D . . H57A H 0.8145 0.1085 0.8533 0.351 Uiso 1 1 calc R . . H57B H 0.8214 0.2204 0.8542 0.351 Uiso 1 1 calc R . . C58 C 0.7279(8) 0.1608(11) 0.8080(8) 0.294(8) Uani 1 1 d D . . H58A H 0.7143 0.0984 0.7813 0.353 Uiso 1 1 calc R . . H58B H 0.7245 0.2079 0.7733 0.353 Uiso 1 1 calc R . . C59 C 0.6275(9) 0.1779(12) 0.8551(8) 0.266(7) Uani 1 1 d DU . . H59A H 0.6275 0.2470 0.8679 0.320 Uiso 1 1 calc R . . H59B H 0.5689 0.1627 0.8224 0.320 Uiso 1 1 calc R . . C60 C 0.6054(14) 0.1396(14) 0.9108(7) 0.304(9) Uani 1 1 d DU . . H60A H 0.6591 0.1596 0.9465 0.365 Uiso 1 1 calc R . . H60B H 0.6087 0.0703 0.9004 0.365 Uiso 1 1 calc R . . C61 C 0.5002(8) 0.1599(11) 0.9450(6) 0.261(7) Uani 1 1 d D . . H61A H 0.4733 0.2171 0.9267 0.313 Uiso 1 1 calc R . . H61B H 0.4522 0.1062 0.9300 0.313 Uiso 1 1 calc R . . C62 C 0.5032(10) 0.1721(14) 1.0119(6) 0.391(13) Uani 1 1 d D . . H62A H 0.4345 0.1787 1.0287 0.586 Uiso 1 1 calc R . . H62B H 0.5441 0.2295 1.0274 0.586 Uiso 1 1 calc R . . H62C H 0.5332 0.1175 1.0307 0.586 Uiso 1 1 calc R . . C63 C 1.3440(4) 0.3103(4) 0.8189(2) 0.0820(13) Uani 1 1 d . . . C64 C 1.3391(5) 0.3540(4) 0.8883(3) 0.115(2) Uani 1 1 d . . . H64A H 1.3865 0.4031 0.9054 0.138 Uiso 1 1 calc R . . C65 C 1.2633(6) 0.3231(5) 0.9309(3) 0.131(2) Uani 1 1 d . . . H65A H 1.2596 0.3499 0.9777 0.158 Uiso 1 1 calc R . . C66 C 1.1934(5) 0.2526(5) 0.9039(3) 0.121(2) Uani 1 1 d . . . H66A H 1.1424 0.2318 0.9332 0.145 Uiso 1 1 calc R . . C67 C 1.1953(4) 0.2107(4) 0.8341(3) 0.0951(15) Uani 1 1 d . . . H67A H 1.1461 0.1628 0.8177 0.114 Uiso 1 1 calc R . . C68 C 1.2714(4) 0.2405(3) 0.7884(2) 0.0733(12) Uani 1 1 d . . . C69 C 1.5200(3) 0.3020(3) 0.6804(2) 0.0620(10) Uani 1 1 d . . . C70 C 1.5542(4) 0.3968(3) 0.6743(2) 0.0737(12) Uani 1 1 d . . . H70A H 1.5187 0.4483 0.6951 0.088 Uiso 1 1 calc R . . C71 C 1.6418(4) 0.4127(3) 0.6365(3) 0.0840(14) Uani 1 1 d . . . H71A H 1.6657 0.4755 0.6319 0.101 Uiso 1 1 calc R . . C72 C 1.6936(4) 0.3364(4) 0.6058(3) 0.0844(13) Uani 1 1 d . . . H72A H 1.7531 0.3479 0.5812 0.101 Uiso 1 1 calc R . . C73 C 1.6589(4) 0.2441(3) 0.6111(2) 0.0796(13) Uani 1 1 d . . . H73A H 1.6945 0.1929 0.5898 0.096 Uiso 1 1 calc R . . C74 C 1.5716(3) 0.2259(3) 0.6479(2) 0.0697(11) Uani 1 1 d . . . H74A H 1.5473 0.1627 0.6508 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.05070(18) 0.05094(18) 0.0599(2) 0.00473(14) -0.00021(14) -0.00251(13) Pd2 0.0704(2) 0.05374(19) 0.0610(2) 0.00171(15) -0.00189(16) 0.00408(16) O1 0.0556(17) 0.088(2) 0.0601(17) 0.0052(14) 0.0006(13) -0.0120(14) O2 0.072(2) 0.122(3) 0.105(3) -0.001(2) 0.032(2) -0.0063(19) O3 0.0676(18) 0.083(2) 0.0644(18) -0.0129(15) -0.0011(15) -0.0044(15) O4 0.091(2) 0.082(2) 0.067(2) -0.0114(16) 0.0024(17) 0.0011(17) N1 0.051(2) 0.0545(18) 0.0541(19) 0.0057(15) -0.0007(15) -0.0008(15) N2 0.061(2) 0.0516(18) 0.066(2) -0.0053(15) 0.0010(17) -0.0040(16) N3 0.058(2) 0.068(2) 0.088(3) -0.0079(19) 0.000(2) -0.0121(18) N4 0.070(2) 0.0535(19) 0.072(2) 0.0063(17) 0.0003(19) 0.0030(17) N5 0.073(2) 0.060(2) 0.061(2) -0.0021(17) -0.0091(18) 0.0060(17) N6 0.090(3) 0.079(3) 0.073(3) -0.013(2) -0.002(2) -0.002(2) C1 0.062(3) 0.056(2) 0.055(2) 0.0079(18) -0.007(2) 0.0004(19) C2 0.050(2) 0.055(2) 0.065(3) 0.0040(19) 0.003(2) -0.0010(18) C3 0.060(3) 0.070(3) 0.079(3) 0.003(2) -0.007(2) -0.004(2) C4 0.055(3) 0.085(3) 0.096(4) 0.004(3) 0.003(3) -0.003(2) C5 0.067(3) 0.070(3) 0.091(4) 0.001(2) 0.023(3) -0.006(2) C6 0.068(3) 0.067(3) 0.065(3) 0.002(2) 0.006(2) -0.006(2) C7 0.054(2) 0.052(2) 0.063(3) 0.0035(18) 0.005(2) -0.0035(18) C8 0.088(4) 0.217(8) 0.103(5) -0.001(5) 0.043(4) -0.015(4) C9 0.177(8) 0.338(13) 0.120(6) 0.014(8) 0.020(6) -0.062(8) C10 0.345(16) 0.301(13) 0.184(10) 0.053(10) 0.066(11) -0.049(12) C11 0.286(19) 0.320(17) 0.244(13) 0.092(12) 0.085(13) 0.028(14) C12 0.172(14) 0.55(4) 0.64(4) 0.35(3) 0.114(18) 0.087(16) C13 0.246(15) 0.308(17) 0.39(2) 0.042(15) 0.114(14) 0.068(13) C14 0.056(2) 0.047(2) 0.058(2) 0.0026(18) -0.0005(19) -0.0085(18) C15 0.069(3) 0.059(2) 0.063(3) 0.012(2) -0.001(2) 0.003(2) C16 0.094(3) 0.069(3) 0.059(3) 0.008(2) 0.008(2) -0.011(3) C17 0.079(3) 0.061(3) 0.082(3) -0.005(2) 0.016(3) -0.013(2) C18 0.057(3) 0.057(2) 0.095(4) -0.002(2) 0.008(2) 0.002(2) C19 0.058(2) 0.052(2) 0.071(3) 0.010(2) -0.005(2) -0.0012(19) C20 0.107(4) 0.089(4) 0.112(4) -0.030(3) 0.045(3) -0.018(3) C21 0.089(4) 0.091(3) 0.082(3) -0.010(3) 0.022(3) 0.005(3) C22 0.109(4) 0.089(4) 0.087(4) 0.000(3) 0.031(3) 0.003(3) C23 0.099(4) 0.136(5) 0.103(4) -0.024(4) 0.036(3) -0.005(4) C24 0.135(6) 0.147(6) 0.120(5) -0.003(4) 0.053(4) -0.005(5) C25 0.119(6) 0.217(8) 0.136(6) -0.018(6) 0.033(5) -0.019(6) C26 0.050(2) 0.047(2) 0.076(3) 0.0031(19) 0.006(2) -0.0019(17) C27 0.063(3) 0.057(2) 0.083(3) 0.011(2) 0.007(2) -0.004(2) C28 0.070(3) 0.075(3) 0.092(3) 0.010(3) 0.022(3) 0.001(2) C29 0.068(3) 0.092(4) 0.117(4) -0.008(3) 0.025(3) -0.016(3) C30 0.058(3) 0.084(3) 0.106(4) -0.018(3) 0.006(3) -0.016(2) C31 0.056(3) 0.061(2) 0.080(3) -0.004(2) 0.008(2) -0.006(2) C32 0.069(3) 0.052(2) 0.068(3) 0.000(2) -0.008(2) -0.005(2) C33 0.072(3) 0.072(3) 0.074(3) -0.004(2) 0.001(2) 0.007(2) C34 0.097(4) 0.108(4) 0.084(4) -0.013(3) 0.012(3) 0.017(3) C35 0.128(5) 0.119(5) 0.074(4) -0.012(3) 0.017(4) 0.008(4) C36 0.111(5) 0.124(5) 0.069(4) -0.003(3) -0.011(3) -0.003(4) C37 0.076(3) 0.089(3) 0.084(4) 0.000(3) -0.004(3) 0.000(3) C38 0.065(3) 0.060(3) 0.083(3) 0.005(2) -0.008(2) -0.004(2) C39 0.073(3) 0.051(2) 0.071(3) 0.001(2) -0.005(2) 0.001(2) C40 0.072(3) 0.049(2) 0.063(3) -0.0016(19) -0.004(2) 0.006(2) C41 0.071(3) 0.060(2) 0.066(3) -0.002(2) -0.004(2) 0.003(2) C42 0.086(3) 0.056(2) 0.065(3) 0.001(2) -0.003(3) 0.007(2) C43 0.091(4) 0.070(3) 0.073(3) -0.015(2) -0.011(3) -0.003(3) C44 0.081(3) 0.070(3) 0.086(3) -0.006(3) -0.011(3) -0.010(2) C45 0.092(4) 0.063(3) 0.076(3) 0.002(2) -0.003(3) 0.008(2) C46 0.094(4) 0.086(3) 0.078(3) -0.004(3) 0.010(3) 0.002(3) C47 0.095(4) 0.085(3) 0.098(4) 0.004(3) 0.005(3) 0.010(3) C48 0.098(4) 0.117(4) 0.100(4) 0.006(3) 0.013(3) -0.002(3) C49 0.133(6) 0.173(7) 0.133(6) 0.005(5) -0.009(5) 0.011(5) C50 0.166(7) 0.212(9) 0.114(6) 0.010(6) 0.033(5) -0.002(6) C51 0.070(3) 0.064(3) 0.076(3) 0.010(2) 0.001(2) -0.002(2) C52 0.094(4) 0.065(3) 0.098(4) 0.008(3) 0.009(3) -0.014(3) C53 0.118(5) 0.085(4) 0.131(5) 0.014(3) 0.029(4) -0.033(4) C54 0.110(5) 0.117(5) 0.155(6) 0.010(4) 0.055(4) -0.017(4) C55 0.115(5) 0.086(4) 0.155(6) 0.017(4) 0.060(4) 0.019(3) C56 0.092(4) 0.060(3) 0.119(4) 0.019(3) 0.035(3) 0.008(3) C57 0.133(8) 0.193(10) 0.56(3) 0.023(12) 0.189(14) -0.003(8) C58 0.132(9) 0.366(19) 0.380(19) -0.031(14) 0.067(12) 0.078(12) C59 0.136(8) 0.371(19) 0.288(17) -0.017(16) 0.021(11) 0.059(10) C60 0.34(2) 0.41(2) 0.170(13) 0.013(13) 0.004(13) 0.132(17) C61 0.163(9) 0.45(2) 0.181(10) 0.010(13) 0.055(9) 0.117(11) C62 0.185(12) 0.82(4) 0.175(12) 0.079(19) 0.027(11) 0.078(17) C63 0.089(4) 0.089(3) 0.066(3) -0.006(3) 0.004(3) 0.006(3) C64 0.126(5) 0.124(5) 0.085(4) -0.032(4) 0.010(4) -0.004(4) C65 0.144(6) 0.163(6) 0.080(4) -0.032(4) 0.026(4) 0.007(5) C66 0.121(5) 0.151(6) 0.088(4) 0.002(4) 0.029(4) -0.003(4) C67 0.111(4) 0.102(4) 0.072(3) 0.003(3) 0.016(3) 0.000(3) C68 0.082(3) 0.071(3) 0.066(3) 0.002(2) 0.000(2) 0.010(2) C69 0.061(3) 0.064(3) 0.060(2) 0.003(2) -0.011(2) 0.000(2) C70 0.083(3) 0.055(3) 0.082(3) 0.001(2) -0.007(3) 0.002(2) C71 0.092(4) 0.067(3) 0.094(4) 0.019(3) -0.008(3) -0.006(3) C72 0.072(3) 0.092(4) 0.091(4) 0.021(3) 0.000(3) 0.001(3) C73 0.080(3) 0.073(3) 0.085(3) 0.003(2) 0.007(3) 0.013(3) C74 0.075(3) 0.058(3) 0.075(3) 0.004(2) -0.004(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 C26 1.984(4) . ? Pd1 N2 2.028(3) . ? Pd1 N1 2.034(3) . ? Pd1 O1 2.041(3) . ? Pd2 C68 1.975(4) . ? Pd2 N5 2.027(3) . ? Pd2 N4 2.034(3) . ? Pd2 O3 2.039(3) . ? O1 C7 1.296(4) . ? O2 C5 1.366(5) . ? O2 C8 1.424(7) . ? O3 C40 1.294(4) . ? O4 C42 1.357(5) . ? O4 C45 1.437(5) . ? N1 C1 1.311(4) . ? N1 C14 1.442(5) . ? N2 N3 1.269(4) . ? N2 C32 1.449(5) . ? N3 C31 1.395(5) . ? N4 C38 1.312(5) . ? N4 C51 1.442(5) . ? N5 N6 1.275(4) . ? N5 C69 1.439(5) . ? N6 C63 1.383(6) . ? C1 C2 1.412(5) . ? C2 C3 1.415(5) . ? C2 C7 1.421(5) . ? C3 C4 1.366(6) . ? C4 C5 1.389(6) . ? C5 C6 1.385(6) . ? C6 C7 1.393(5) . ? C8 C9 1.518(9) . ? C9 C10 1.352(12) . ? C10 C11 1.669(14) . ? C11 C12 1.210(16) . ? C12 C13 1.519(16) . ? C14 C19 1.369(5) . ? C14 C15 1.390(5) . ? C15 C16 1.381(6) . ? C16 C17 1.389(6) . ? C17 C18 1.376(6) . ? C17 C20 1.500(6) . ? C18 C19 1.378(5) . ? C20 C21 1.450(6) . ? C21 C22 1.460(6) . ? C22 C23 1.435(7) . ? C23 C24 1.458(7) . ? C24 C25 1.424(8) . ? C26 C27 1.395(5) . ? C26 C31 1.419(5) . ? C27 C28 1.388(6) . ? C28 C29 1.369(6) . ? C29 C30 1.368(6) . ? C30 C31 1.379(6) . ? C32 C37 1.371(6) . ? C32 C33 1.375(6) . ? C33 C34 1.387(6) . ? C34 C35 1.368(7) . ? C35 C36 1.369(7) . ? C36 C37 1.374(7) . ? C38 C39 1.415(6) . ? C39 C44 1.399(6) . ? C39 C40 1.427(6) . ? C40 C41 1.401(5) . ? C41 C42 1.358(5) . ? C42 C43 1.403(6) . ? C43 C44 1.346(6) . ? C45 C46 1.519(6) . ? C46 C47 1.482(6) . ? C47 C48 1.551(7) . ? C48 C49 1.467(8) . ? C49 C50 1.512(8) . ? C51 C56 1.371(6) . ? C51 C52 1.374(6) . ? C52 C53 1.372(7) . ? C53 C54 1.361(8) . ? C54 C55 1.381(7) . ? C54 C57 1.590(10) . ? C55 C56 1.373(6) . ? C57 C58 1.056(13) . ? C58 C59 1.613(13) . ? C59 C60 1.259(15) . ? C60 C61 1.553(15) . ? C61 C62 1.260(12) . ? C63 C64 1.398(6) . ? C63 C68 1.401(6) . ? C64 C65 1.371(8) . ? C65 C66 1.364(8) . ? C66 C67 1.392(7) . ? C67 C68 1.407(6) . ? C69 C74 1.381(5) . ? C69 C70 1.392(5) . ? C70 C71 1.382(6) . ? C71 C72 1.372(6) . ? C72 C73 1.359(6) . ? C73 C74 1.374(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 C26 Pd1 N2 78.87(15) . . ? C26 Pd1 N1 100.48(15) . . ? N2 Pd1 N1 178.34(12) . . ? C26 Pd1 O1 171.02(14) . . ? N2 Pd1 O1 92.51(12) . . ? N1 Pd1 O1 88.07(11) . . ? C68 Pd2 N5 78.73(17) . . ? C68 Pd2 N4 101.06(17) . . ? N5 Pd2 N4 170.39(12) . . ? C68 Pd2 O3 168.36(16) . . ? N5 Pd2 O3 89.90(13) . . ? N4 Pd2 O3 90.57(13) . . ? C7 O1 Pd1 126.1(2) . . ? C5 O2 C8 118.3(4) . . ? C40 O3 Pd2 129.5(3) . . ? C42 O4 C45 118.5(3) . . ? C1 N1 C14 116.0(3) . . ? C1 N1 Pd1 121.5(3) . . ? C14 N1 Pd1 122.4(2) . . ? N3 N2 C32 113.9(3) . . ? N3 N2 Pd1 118.8(3) . . ? C32 N2 Pd1 127.2(3) . . ? N2 N3 C31 112.1(3) . . ? C38 N4 C51 113.4(4) . . ? C38 N4 Pd2 122.8(3) . . ? C51 N4 Pd2 123.6(3) . . ? N6 N5 C69 114.0(3) . . ? N6 N5 Pd2 118.1(3) . . ? C69 N5 Pd2 127.2(3) . . ? N5 N6 C63 111.7(4) . . ? N1 C1 C2 128.3(4) . . ? C1 C2 C3 118.4(4) . . ? C1 C2 C7 123.0(3) . . ? C3 C2 C7 117.8(4) . . ? C4 C3 C2 122.9(4) . . ? C3 C4 C5 118.2(4) . . ? O2 C5 C6 123.2(5) . . ? O2 C5 C4 115.8(4) . . ? C6 C5 C4 121.1(4) . . ? C5 C6 C7 121.1(4) . . ? O1 C7 C6 118.4(4) . . ? O1 C7 C2 122.8(3) . . ? C6 C7 C2 118.7(4) . . ? O2 C8 C9 106.8(6) . . ? C10 C9 C8 115.2(9) . . ? C9 C10 C11 115.6(12) . . ? C12 C11 C10 113.8(16) . . ? C11 C12 C13 100.1(17) . . ? C19 C14 C15 119.6(4) . . ? C19 C14 N1 119.3(4) . . ? C15 C14 N1 121.1(3) . . ? C16 C15 C14 119.7(4) . . ? C15 C16 C17 121.6(4) . . ? C18 C17 C16 116.8(4) . . ? C18 C17 C20 122.7(5) . . ? C16 C17 C20 120.5(5) . . ? C17 C18 C19 122.8(4) . . ? C14 C19 C18 119.4(4) . . ? C21 C20 C17 117.1(4) . . ? C20 C21 C22 120.2(4) . . ? C23 C22 C21 124.3(5) . . ? C22 C23 C24 122.1(5) . . ? C25 C24 C23 122.2(6) . . ? C27 C26 C31 114.5(4) . . ? C27 C26 Pd1 134.7(3) . . ? C31 C26 Pd1 110.8(3) . . ? C28 C27 C26 121.4(4) . . ? C29 C28 C27 121.7(5) . . ? C30 C29 C28 119.3(5) . . ? C29 C30 C31 119.0(5) . . ? C30 C31 N3 117.7(4) . . ? C30 C31 C26 123.8(4) . . ? N3 C31 C26 118.4(4) . . ? C37 C32 C33 121.1(4) . . ? C37 C32 N2 120.4(4) . . ? C33 C32 N2 118.4(4) . . ? C32 C33 C34 118.6(4) . . ? C35 C34 C33 120.3(5) . . ? C34 C35 C36 120.3(5) . . ? C35 C36 C37 120.0(5) . . ? C32 C37 C36 119.6(5) . . ? N4 C38 C39 130.1(4) . . ? C44 C39 C38 118.6(4) . . ? C44 C39 C40 117.1(4) . . ? C38 C39 C40 124.0(4) . . ? O3 C40 C41 118.7(4) . . ? O3 C40 C39 122.8(4) . . ? C41 C40 C39 118.5(4) . . ? C42 C41 C40 121.7(4) . . ? O4 C42 C41 126.0(4) . . ? O4 C42 C43 113.8(4) . . ? C41 C42 C43 120.2(4) . . ? C44 C43 C42 118.7(4) . . ? C43 C44 C39 123.6(4) . . ? O4 C45 C46 106.5(4) . . ? C47 C46 C45 115.0(4) . . ? C46 C47 C48 111.9(4) . . ? C49 C48 C47 115.7(5) . . ? C48 C49 C50 112.6(6) . . ? C56 C51 C52 119.5(4) . . ? C56 C51 N4 119.3(4) . . ? C52 C51 N4 121.2(4) . . ? C53 C52 C51 120.2(5) . . ? C54 C53 C52 121.5(5) . . ? C53 C54 C55 117.6(5) . . ? C53 C54 C57 119.8(7) . . ? C55 C54 C57 121.5(7) . . ? C56 C55 C54 122.0(5) . . ? C51 C56 C55 119.2(5) . . ? C58 C57 C54 121.4(17) . . ? C57 C58 C59 130.1(17) . . ? C60 C59 C58 127.2(15) . . ? C59 C60 C61 119.0(15) . . ? C62 C61 C60 114.9(12) . . ? N6 C63 C64 117.2(5) . . ? N6 C63 C68 119.2(4) . . ? C64 C63 C68 123.6(5) . . ? C65 C64 C63 118.8(6) . . ? C66 C65 C64 119.3(6) . . ? C65 C66 C67 122.6(6) . . ? C66 C67 C68 120.2(5) . . ? C63 C68 C67 115.5(4) . . ? C63 C68 Pd2 111.0(3) . . ? C67 C68 Pd2 133.3(4) . . ? C74 C69 C70 120.4(4) . . ? C74 C69 N5 119.2(4) . . ? C70 C69 N5 120.4(4) . . ? C71 C70 C69 118.6(4) . . ? C72 C71 C70 120.4(4) . . ? C73 C72 C71 120.6(5) . . ? C72 C73 C74 120.3(4) . . ? C73 C74 C69 119.6(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 C26 Pd1 O1 C7 -166.7(7) . . . . ? N2 Pd1 O1 C7 -150.6(3) . . . . ? N1 Pd1 O1 C7 31.0(3) . . . . ? C68 Pd2 O3 C40 172.4(7) . . . . ? N5 Pd2 O3 C40 -175.2(3) . . . . ? N4 Pd2 O3 C40 -4.8(3) . . . . ? C26 Pd1 N1 C1 154.0(3) . . . . ? N2 Pd1 N1 C1 -139(4) . . . . ? O1 Pd1 N1 C1 -28.8(3) . . . . ? C26 Pd1 N1 C14 -23.9(3) . . . . ? N2 Pd1 N1 C14 43(4) . . . . ? O1 Pd1 N1 C14 153.4(3) . . . . ? C26 Pd1 N2 N3 9.1(3) . . . . ? N1 Pd1 N2 N3 -58(4) . . . . ? O1 Pd1 N2 N3 -168.4(3) . . . . ? C26 Pd1 N2 C32 -174.7(3) . . . . ? N1 Pd1 N2 C32 118(4) . . . . ? O1 Pd1 N2 C32 7.9(3) . . . . ? C32 N2 N3 C31 176.4(3) . . . . ? Pd1 N2 N3 C31 -6.9(4) . . . . ? C68 Pd2 N4 C38 -175.9(3) . . . . ? N5 Pd2 N4 C38 96.4(9) . . . . ? O3 Pd2 N4 C38 3.6(3) . . . . ? C68 Pd2 N4 C51 8.9(3) . . . . ? N5 Pd2 N4 C51 -78.8(9) . . . . ? O3 Pd2 N4 C51 -171.6(3) . . . . ? C68 Pd2 N5 N6 -11.1(3) . . . . ? N4 Pd2 N5 N6 78.5(9) . . . . ? O3 Pd2 N5 N6 171.4(3) . . . . ? C68 Pd2 N5 C69 179.4(3) . . . . ? N4 Pd2 N5 C69 -91.0(9) . . . . ? O3 Pd2 N5 C69 1.9(3) . . . . ? C69 N5 N6 C63 -178.1(4) . . . . ? Pd2 N5 N6 C63 11.1(5) . . . . ? C14 N1 C1 C2 -167.2(4) . . . . ? Pd1 N1 C1 C2 14.8(5) . . . . ? N1 C1 C2 C3 -178.5(4) . . . . ? N1 C1 C2 C7 12.0(6) . . . . ? C1 C2 C3 C4 -169.2(4) . . . . ? C7 C2 C3 C4 0.8(6) . . . . ? C2 C3 C4 C5 3.3(7) . . . . ? C8 O2 C5 C6 10.7(7) . . . . ? C8 O2 C5 C4 -169.7(5) . . . . ? C3 C4 C5 O2 175.7(4) . . . . ? C3 C4 C5 C6 -4.7(7) . . . . ? O2 C5 C6 C7 -178.5(4) . . . . ? C4 C5 C6 C7 1.9(7) . . . . ? Pd1 O1 C7 C6 166.3(3) . . . . ? Pd1 O1 C7 C2 -16.3(5) . . . . ? C5 C6 C7 O1 179.7(4) . . . . ? C5 C6 C7 C2 2.3(6) . . . . ? C1 C2 C7 O1 -11.4(6) . . . . ? C3 C2 C7 O1 179.1(4) . . . . ? C1 C2 C7 C6 165.9(4) . . . . ? C3 C2 C7 C6 -3.6(5) . . . . ? C5 O2 C8 C9 169.6(6) . . . . ? O2 C8 C9 C10 172.3(11) . . . . ? C8 C9 C10 C11 178.8(9) . . . . ? C9 C10 C11 C12 70(3) . . . . ? C10 C11 C12 C13 171.6(12) . . . . ? C1 N1 C14 C19 126.0(4) . . . . ? Pd1 N1 C14 C19 -56.1(4) . . . . ? C1 N1 C14 C15 -54.3(5) . . . . ? Pd1 N1 C14 C15 123.6(3) . . . . ? C19 C14 C15 C16 1.4(6) . . . . ? N1 C14 C15 C16 -178.3(3) . . . . ? C14 C15 C16 C17 0.0(6) . . . . ? C15 C16 C17 C18 -1.9(6) . . . . ? C15 C16 C17 C20 178.8(4) . . . . ? C16 C17 C18 C19 2.7(6) . . . . ? C20 C17 C18 C19 -178.1(4) . . . . ? C15 C14 C19 C18 -0.6(5) . . . . ? N1 C14 C19 C18 179.1(3) . . . . ? C17 C18 C19 C14 -1.5(6) . . . . ? C18 C17 C20 C21 84.4(6) . . . . ? C16 C17 C20 C21 -96.4(6) . . . . ? C17 C20 C21 C22 178.3(5) . . . . ? C20 C21 C22 C23 -179.8(6) . . . . ? C21 C22 C23 C24 -176.8(6) . . . . ? C22 C23 C24 C25 178.5(7) . . . . ? N2 Pd1 C26 C27 172.4(4) . . . . ? N1 Pd1 C26 C27 -9.2(4) . . . . ? O1 Pd1 C26 C27 -171.2(6) . . . . ? N2 Pd1 C26 C31 -8.4(3) . . . . ? N1 Pd1 C26 C31 170.0(3) . . . . ? O1 Pd1 C26 C31 8.0(10) . . . . ? C31 C26 C27 C28 -1.8(6) . . . . ? Pd1 C26 C27 C28 177.4(3) . . . . ? C26 C27 C28 C29 -1.2(7) . . . . ? C27 C28 C29 C30 1.6(8) . . . . ? C28 C29 C30 C31 1.1(8) . . . . ? C29 C30 C31 N3 172.7(4) . . . . ? C29 C30 C31 C26 -4.4(7) . . . . ? N2 N3 C31 C30 -178.3(4) . . . . ? N2 N3 C31 C26 -1.1(5) . . . . ? C27 C26 C31 C30 4.6(6) . . . . ? Pd1 C26 C31 C30 -174.8(4) . . . . ? C27 C26 C31 N3 -172.5(4) . . . . ? Pd1 C26 C31 N3 8.2(5) . . . . ? N3 N2 C32 C37 33.6(5) . . . . ? Pd1 N2 C32 C37 -142.8(3) . . . . ? N3 N2 C32 C33 -144.5(4) . . . . ? Pd1 N2 C32 C33 39.1(5) . . . . ? C37 C32 C33 C34 0.7(7) . . . . ? N2 C32 C33 C34 178.8(4) . . . . ? C32 C33 C34 C35 0.0(8) . . . . ? C33 C34 C35 C36 -0.8(9) . . . . ? C34 C35 C36 C37 0.8(9) . . . . ? C33 C32 C37 C36 -0.7(7) . . . . ? N2 C32 C37 C36 -178.7(4) . . . . ? C35 C36 C37 C32 -0.1(8) . . . . ? C51 N4 C38 C39 175.3(4) . . . . ? Pd2 N4 C38 C39 -0.4(6) . . . . ? N4 C38 C39 C44 -177.9(4) . . . . ? N4 C38 C39 C40 -3.8(7) . . . . ? Pd2 O3 C40 C41 -178.1(3) . . . . ? Pd2 O3 C40 C39 2.5(6) . . . . ? C44 C39 C40 O3 176.8(4) . . . . ? C38 C39 C40 O3 2.6(6) . . . . ? C44 C39 C40 C41 -2.5(6) . . . . ? C38 C39 C40 C41 -176.7(4) . . . . ? O3 C40 C41 C42 -178.1(4) . . . . ? C39 C40 C41 C42 1.3(6) . . . . ? C45 O4 C42 C41 1.8(6) . . . . ? C45 O4 C42 C43 -178.6(4) . . . . ? C40 C41 C42 O4 -179.8(4) . . . . ? C40 C41 C42 C43 0.6(6) . . . . ? O4 C42 C43 C44 179.1(4) . . . . ? C41 C42 C43 C44 -1.2(7) . . . . ? C42 C43 C44 C39 -0.1(7) . . . . ? C38 C39 C44 C43 176.6(4) . . . . ? C40 C39 C44 C43 2.0(7) . . . . ? C42 O4 C45 C46 -176.3(3) . . . . ? O4 C45 C46 C47 -179.9(4) . . . . ? C45 C46 C47 C48 -178.2(4) . . . . ? C46 C47 C48 C49 178.9(5) . . . . ? C47 C48 C49 C50 178.9(6) . . . . ? C38 N4 C51 C56 -113.0(5) . . . . ? Pd2 N4 C51 C56 62.6(5) . . . . ? C38 N4 C51 C52 66.8(5) . . . . ? Pd2 N4 C51 C52 -117.6(4) . . . . ? C56 C51 C52 C53 -1.4(8) . . . . ? N4 C51 C52 C53 178.8(5) . . . . ? C51 C52 C53 C54 1.1(9) . . . . ? C52 C53 C54 C55 0.4(11) . . . . ? C52 C53 C54 C57 -167.6(8) . . . . ? C53 C54 C55 C56 -1.6(11) . . . . ? C57 C54 C55 C56 166.2(8) . . . . ? C52 C51 C56 C55 0.2(8) . . . . ? N4 C51 C56 C55 -180.0(5) . . . . ? C54 C55 C56 C51 1.3(10) . . . . ? C53 C54 C57 C58 -99.0(18) . . . . ? C55 C54 C57 C58 93.5(18) . . . . ? C54 C57 C58 C59 -173.6(12) . . . . ? C57 C58 C59 C60 -48(3) . . . . ? C58 C59 C60 C61 -175.2(12) . . . . ? C59 C60 C61 C62 -140(2) . . . . ? N5 N6 C63 C64 172.4(4) . . . . ? N5 N6 C63 C68 -3.8(6) . . . . ? N6 C63 C64 C65 -171.8(6) . . . . ? C68 C63 C64 C65 4.2(9) . . . . ? C63 C64 C65 C66 -1.7(11) . . . . ? C64 C65 C66 C67 -0.4(11) . . . . ? C65 C66 C67 C68 0.1(10) . . . . ? N6 C63 C68 C67 171.6(4) . . . . ? C64 C63 C68 C67 -4.4(7) . . . . ? N6 C63 C68 Pd2 -5.0(6) . . . . ? C64 C63 C68 Pd2 179.0(4) . . . . ? C66 C67 C68 C63 2.2(7) . . . . ? C66 C67 C68 Pd2 177.8(4) . . . . ? N5 Pd2 C68 C63 7.8(3) . . . . ? N4 Pd2 C68 C63 -162.4(3) . . . . ? O3 Pd2 C68 C63 20.4(10) . . . . ? N5 Pd2 C68 C67 -167.9(5) . . . . ? N4 Pd2 C68 C67 21.8(5) . . . . ? O3 Pd2 C68 C67 -155.3(6) . . . . ? N6 N5 C69 C74 136.4(4) . . . . ? Pd2 N5 C69 C74 -53.8(5) . . . . ? N6 N5 C69 C70 -43.0(5) . . . . ? Pd2 N5 C69 C70 126.9(4) . . . . ? C74 C69 C70 C71 -1.6(6) . . . . ? N5 C69 C70 C71 177.7(4) . . . . ? C69 C70 C71 C72 0.1(7) . . . . ? C70 C71 C72 C73 1.0(7) . . . . ? C71 C72 C73 C74 -0.5(7) . . . . ? C72 C73 C74 C69 -1.0(7) . . . . ? C70 C69 C74 C73 2.1(6) . . . . ? N5 C69 C74 C73 -177.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.491 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.051 #===END data_(AZPTON) _database_code_depnum_ccdc_archive 'CCDC 776861' #TrackingRef 'acrispini.CIF' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C74 H86 N6 O4 Pt2' _chemical_formula_sum 'C74 H86 N6 O4 Pt2' _chemical_formula_weight 1513.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.833(7) _cell_length_b 13.736(7) _cell_length_c 20.058(11) _cell_angle_alpha 101.049(11) _cell_angle_beta 107.842(10) _cell_angle_gamma 90.996(10) _cell_volume 3292(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8693 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.40 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.527 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 4.298 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.6390 _exptl_absorpt_correction_T_max 0.6943 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46321 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0386 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 26.37 _reflns_number_total 13391 _reflns_number_gt 10157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+4.0033P] 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 13391 _refine_ls_number_parameters 775 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 0.230932(13) 0.160688(12) 0.382224(9) 0.04181(6) Uani 1 1 d . . . Pt2 Pt 0.282745(14) 0.386249(12) 0.681874(9) 0.04616(6) Uani 1 1 d . . . O1 O 0.0766(2) 0.1073(2) 0.31909(16) 0.0535(8) Uani 1 1 d . . . O2 O -0.3037(3) 0.0377(3) 0.2565(3) 0.0919(13) Uani 1 1 d . . . O3 O 0.1646(2) 0.3724(2) 0.58477(16) 0.0523(8) Uani 1 1 d . . . O4 O -0.0077(3) 0.3928(2) 0.34479(17) 0.0607(9) Uani 1 1 d . . . N1 N 0.1958(3) 0.1211(2) 0.46447(19) 0.0415(8) Uani 1 1 d . . . N2 N 0.2681(3) 0.1960(3) 0.3007(2) 0.0477(9) Uani 1 1 d . . . N3 N 0.3683(3) 0.2189(3) 0.3077(2) 0.0582(11) Uani 1 1 d . . . N4 N 0.3935(3) 0.4324(3) 0.6407(2) 0.0481(9) Uani 1 1 d . . . N5 N 0.1792(3) 0.3214(3) 0.7187(2) 0.0502(9) Uani 1 1 d . . . N6 N 0.2130(4) 0.3012(3) 0.7808(2) 0.0656(11) Uani 1 1 d . . . C1 C 0.0954(3) 0.1139(3) 0.4669(2) 0.0463(10) Uani 1 1 d . . . H1A H 0.0888 0.1100 0.5113 0.056 Uiso 1 1 calc R . . C2 C -0.0033(3) 0.1112(3) 0.4119(2) 0.0456(10) Uani 1 1 d . . . C3 C -0.0086(4) 0.0995(3) 0.3398(3) 0.0479(11) Uani 1 1 d . . . C4 C -0.1099(4) 0.0744(4) 0.2871(3) 0.0573(12) Uani 1 1 d . . . H4A H -0.1140 0.0633 0.2391 0.069 Uiso 1 1 calc R . . C5 C -0.2031(4) 0.0658(4) 0.3052(3) 0.0635(14) Uani 1 1 d . . . C6 C -0.1994(4) 0.0845(4) 0.3764(3) 0.0684(15) Uani 1 1 d . . . H6A H -0.2639 0.0833 0.3883 0.082 Uiso 1 1 calc R . . C7 C -0.1019(4) 0.1045(4) 0.4279(3) 0.0564(12) Uani 1 1 d . . . H7A H -0.0995 0.1141 0.4755 0.068 Uiso 1 1 calc R . . C8 C -0.3111(6) 0.0008(7) 0.1848(4) 0.131(3) Uani 1 1 d . . . H8A H -0.2544 -0.0443 0.1823 0.157 Uiso 1 1 calc R . . H8B H -0.3009 0.0552 0.1623 0.157 Uiso 1 1 calc R . . C9 C -0.4243(9) -0.0541(12) 0.1462(6) 0.230(8) Uani 1 1 d . . . H9A H -0.4132 -0.1241 0.1444 0.277 Uiso 1 1 calc R . . H9B H -0.4669 -0.0362 0.1785 0.277 Uiso 1 1 calc R . . C10 C -0.4769(9) -0.0503(13) 0.0953(8) 0.267(9) Uani 1 1 d . . . H10A H -0.4335 -0.0666 0.0633 0.320 Uiso 1 1 calc R . . H10B H -0.4890 0.0195 0.0975 0.320 Uiso 1 1 calc R . . C11 C -0.5924(8) -0.1079(10) 0.0542(7) 0.198(6) Uani 1 1 d . . . H11A H -0.5879 -0.1524 0.0115 0.238 Uiso 1 1 calc R . . H11B H -0.6105 -0.1484 0.0844 0.238 Uiso 1 1 calc R . . C12 C -0.6719(10) -0.0505(12) 0.0354(7) 0.212(7) Uani 1 1 d . . . H12A H -0.6477 -0.0018 0.0130 0.254 Uiso 1 1 calc R . . H12B H -0.6846 -0.0145 0.0784 0.254 Uiso 1 1 calc R . . C13 C -0.7777(8) -0.1017(11) -0.0140(6) 0.227(7) Uani 1 1 d . . . H13A H -0.8311 -0.0539 -0.0233 0.341 Uiso 1 1 calc R . . H13B H -0.8029 -0.1503 0.0074 0.341 Uiso 1 1 calc R . . H13C H -0.7676 -0.1342 -0.0582 0.341 Uiso 1 1 calc R . . C14 C 0.2797(3) 0.0982(3) 0.5230(2) 0.0427(10) Uani 1 1 d . . . C15 C 0.2943(4) 0.1464(3) 0.5923(3) 0.0542(12) Uani 1 1 d . . . H15A H 0.2459 0.1927 0.6016 0.065 Uiso 1 1 calc R . . C16 C 0.3790(4) 0.1271(4) 0.6476(3) 0.0612(13) Uani 1 1 d . . . H16A H 0.3884 0.1613 0.6940 0.073 Uiso 1 1 calc R . . C17 C 0.4503(4) 0.0577(4) 0.6354(3) 0.0674(15) Uani 1 1 d . . . C18 C 0.4330(4) 0.0081(4) 0.5666(3) 0.0614(13) Uani 1 1 d . . . H18A H 0.4795 -0.0402 0.5575 0.074 Uiso 1 1 calc R . . C19 C 0.3484(4) 0.0277(3) 0.5103(3) 0.0493(11) Uani 1 1 d . . . H19A H 0.3384 -0.0072 0.4639 0.059 Uiso 1 1 calc R . . C20 C 0.5458(5) 0.0379(5) 0.6954(4) 0.104(2) Uani 1 1 d . . . H20A H 0.5225 0.0437 0.7375 0.125 Uiso 1 1 calc R . . H20B H 0.5615 -0.0308 0.6826 0.125 Uiso 1 1 calc R . . C21 C 0.6455(4) 0.0980(5) 0.7150(3) 0.0757(16) Uani 1 1 d . . . H21A H 0.6290 0.1665 0.7274 0.091 Uiso 1 1 calc R . . H21B H 0.6680 0.0921 0.6726 0.091 Uiso 1 1 calc R . . C22 C 0.7408(5) 0.0818(5) 0.7730(3) 0.0890(19) Uani 1 1 d . . . H22A H 0.7162 0.0860 0.8145 0.107 Uiso 1 1 calc R . . H22B H 0.7559 0.0131 0.7598 0.107 Uiso 1 1 calc R . . C23 C 0.8420(6) 0.1370(7) 0.7971(4) 0.124(3) Uani 1 1 d . . . H23A H 0.8281 0.2052 0.8135 0.149 Uiso 1 1 calc R . . H23B H 0.8650 0.1363 0.7553 0.149 Uiso 1 1 calc R . . C24 C 0.9366(6) 0.1151(7) 0.8521(5) 0.130(3) Uani 1 1 d . . . H24A H 0.9138 0.1168 0.8941 0.157 Uiso 1 1 calc R . . H24B H 0.9496 0.0466 0.8360 0.157 Uiso 1 1 calc R . . C25 C 1.0380(7) 0.1687(11) 0.8758(6) 0.212(6) Uani 1 1 d . . . H25A H 1.0871 0.1420 0.9133 0.318 Uiso 1 1 calc R . . H25B H 1.0298 0.2372 0.8937 0.318 Uiso 1 1 calc R . . H25C H 1.0673 0.1642 0.8368 0.318 Uiso 1 1 calc R . . C26 C 0.3855(3) 0.2128(3) 0.4285(3) 0.0458(10) Uani 1 1 d . . . C27 C 0.4540(4) 0.2384(3) 0.4990(3) 0.0519(11) Uani 1 1 d . . . H27A H 0.4256 0.2343 0.5359 0.062 Uiso 1 1 calc R . . C28 C 0.5633(4) 0.2699(4) 0.5153(3) 0.0635(13) Uani 1 1 d . . . H28A H 0.6069 0.2866 0.5630 0.076 Uiso 1 1 calc R . . C29 C 0.6091(4) 0.2771(4) 0.4632(3) 0.0719(16) Uani 1 1 d . . . H29A H 0.6836 0.2959 0.4753 0.086 Uiso 1 1 calc R . . C30 C 0.5451(4) 0.2566(4) 0.3936(3) 0.0691(15) Uani 1 1 d . . . H30A H 0.5746 0.2619 0.3574 0.083 Uiso 1 1 calc R . . C31 C 0.4341(4) 0.2272(4) 0.3776(3) 0.0526(12) Uani 1 1 d . . . C32 C 0.1952(4) 0.1952(4) 0.2314(3) 0.0524(11) Uani 1 1 d . . . C33 C 0.0935(4) 0.2300(4) 0.2243(3) 0.0577(12) Uani 1 1 d . . . H33A H 0.0715 0.2516 0.2644 0.069 Uiso 1 1 calc R . . C34 C 0.0254(5) 0.2326(5) 0.1576(3) 0.0797(17) Uani 1 1 d . . . H34A H -0.0430 0.2573 0.1528 0.096 Uiso 1 1 calc R . . C35 C 0.0544(5) 0.2002(6) 0.0981(3) 0.092(2) Uani 1 1 d . . . H35A H 0.0063 0.2015 0.0530 0.110 Uiso 1 1 calc R . . C36 C 0.1561(6) 0.1655(5) 0.1056(3) 0.0886(19) Uani 1 1 d . . . H36A H 0.1775 0.1437 0.0653 0.106 Uiso 1 1 calc R . . C37 C 0.2264(4) 0.1628(4) 0.1721(3) 0.0684(15) Uani 1 1 d . . . H37A H 0.2951 0.1389 0.1768 0.082 Uiso 1 1 calc R . . C38 C 0.3689(4) 0.4470(3) 0.5749(3) 0.0527(12) Uani 1 1 d . . . H38A H 0.4282 0.4687 0.5625 0.063 Uiso 1 1 calc R . . C39 C 0.2690(4) 0.4353(3) 0.5213(2) 0.0474(10) Uani 1 1 d . . . C40 C 0.1703(4) 0.3962(3) 0.5270(2) 0.0463(10) Uani 1 1 d . . . C41 C 0.0748(4) 0.3830(3) 0.4679(2) 0.0507(11) Uani 1 1 d . . . H41A H 0.0087 0.3595 0.4716 0.061 Uiso 1 1 calc R . . C42 C 0.0783(4) 0.4043(3) 0.4052(3) 0.0512(11) Uani 1 1 d . . . C43 C 0.1761(4) 0.4398(4) 0.3984(3) 0.0597(13) Uani 1 1 d . . . H43A H 0.1775 0.4533 0.3550 0.072 Uiso 1 1 calc R . . C44 C 0.2680(4) 0.4546(4) 0.4547(3) 0.0568(12) Uani 1 1 d . . . H44A H 0.3329 0.4783 0.4497 0.068 Uiso 1 1 calc R . . C45 C -0.1122(4) 0.3597(4) 0.3451(3) 0.0576(12) Uani 1 1 d . . . H45A H -0.1381 0.4080 0.3773 0.069 Uiso 1 1 calc R . . H45B H -0.1093 0.2967 0.3605 0.069 Uiso 1 1 calc R . . C46 C -0.1868(4) 0.3478(4) 0.2693(3) 0.0617(13) Uani 1 1 d . . . H46A H -0.1850 0.4109 0.2546 0.074 Uiso 1 1 calc R . . H46B H -0.1585 0.2996 0.2385 0.074 Uiso 1 1 calc R . . C47 C -0.3033(4) 0.3148(4) 0.2585(3) 0.0633(13) Uani 1 1 d . . . H47A H -0.3325 0.3636 0.2883 0.076 Uiso 1 1 calc R . . H47B H -0.3054 0.2522 0.2738 0.076 Uiso 1 1 calc R . . C48 C -0.3754(4) 0.3016(4) 0.1814(3) 0.0694(14) Uani 1 1 d . . . H48A H -0.3724 0.3643 0.1663 0.083 Uiso 1 1 calc R . . H48B H -0.3454 0.2530 0.1519 0.083 Uiso 1 1 calc R . . C49 C -0.4930(5) 0.2687(5) 0.1677(3) 0.0841(18) Uani 1 1 d . . . H49A H -0.4969 0.2036 0.1793 0.101 Uiso 1 1 calc R . . H49B H -0.5222 0.3146 0.1993 0.101 Uiso 1 1 calc R . . C50 C -0.5628(5) 0.2631(6) 0.0925(4) 0.107(2) Uani 1 1 d . . . H50A H -0.6373 0.2430 0.0874 0.161 Uiso 1 1 calc R . . H50B H -0.5364 0.2155 0.0610 0.161 Uiso 1 1 calc R . . H50C H -0.5596 0.3273 0.0806 0.161 Uiso 1 1 calc R . . C51 C 0.5090(4) 0.4442(3) 0.6785(2) 0.0497(11) Uani 1 1 d . . . C52 C 0.5625(4) 0.3637(4) 0.6961(3) 0.0611(13) Uani 1 1 d . . . H52A H 0.5244 0.3013 0.6841 0.073 Uiso 1 1 calc R . . C53 C 0.6727(4) 0.3752(4) 0.7317(3) 0.0704(15) Uani 1 1 d . . . H53A H 0.7096 0.3198 0.7428 0.084 Uiso 1 1 calc R . . C54 C 0.7305(4) 0.4674(5) 0.7517(3) 0.0689(15) Uani 1 1 d . . . C55 C 0.6747(4) 0.5459(4) 0.7336(3) 0.0679(14) Uani 1 1 d . . . H55A H 0.7120 0.6088 0.7470 0.081 Uiso 1 1 calc R . . C56 C 0.5657(4) 0.5355(4) 0.6965(3) 0.0614(13) Uani 1 1 d . . . H56A H 0.5297 0.5904 0.6834 0.074 Uiso 1 1 calc R . . C57 C 0.8517(5) 0.4805(6) 0.7946(4) 0.097(2) Uani 1 1 d . . . H57A H 0.8868 0.4219 0.7797 0.116 Uiso 1 1 calc R . . H57B H 0.8858 0.5373 0.7846 0.116 Uiso 1 1 calc R . . C58 C 0.8686(9) 0.4949(17) 0.8675(7) 0.363(16) Uani 1 1 d . . . H58A H 0.9454 0.4824 0.8848 0.436 Uiso 1 1 calc R . . H58B H 0.8684 0.5666 0.8800 0.436 Uiso 1 1 calc R . . C59 C 0.8343(9) 0.4695(11) 0.9131(6) 0.201(6) Uani 1 1 d . . . H59A H 0.8428 0.3987 0.9023 0.241 Uiso 1 1 calc R . . H59B H 0.7565 0.4743 0.8909 0.241 Uiso 1 1 calc R . . C60 C 0.8351(8) 0.4791(12) 0.9899(6) 0.218(7) Uani 1 1 d . . . H60A H 0.9114 0.5007 1.0166 0.261 Uiso 1 1 calc R . . H60B H 0.7959 0.5380 0.9967 0.261 Uiso 1 1 calc R . . C61 C 0.8093(11) 0.429(2) 1.0285(8) 0.390(18) Uani 1 1 d . . . H61A H 0.8475 0.3694 1.0228 0.468 Uiso 1 1 calc R . . H61B H 0.7322 0.4086 1.0040 0.468 Uiso 1 1 calc R . . C62 C 0.8166(13) 0.4482(11) 1.0956(7) 0.255(9) Uani 1 1 d . . . H62A H 0.7836 0.3925 1.1066 0.382 Uiso 1 1 calc R . . H62B H 0.7792 0.5063 1.1058 0.382 Uiso 1 1 calc R . . H62C H 0.8926 0.4597 1.1243 0.382 Uiso 1 1 calc R . . C63 C 0.3727(4) 0.3936(3) 0.7823(2) 0.0500(11) Uani 1 1 d . . . C64 C 0.4733(5) 0.4411(4) 0.8257(3) 0.0716(15) Uani 1 1 d . . . H64A H 0.5134 0.4782 0.8063 0.086 Uiso 1 1 calc R . . C65 C 0.5155(5) 0.4351(5) 0.8958(3) 0.0848(18) Uani 1 1 d . . . H65A H 0.5827 0.4696 0.9230 0.102 Uiso 1 1 calc R . . C66 C 0.4619(5) 0.3800(5) 0.9273(3) 0.090(2) Uani 1 1 d . . . H66A H 0.4933 0.3748 0.9747 0.108 Uiso 1 1 calc R . . C67 C 0.3625(5) 0.3335(5) 0.8880(3) 0.0868(19) Uani 1 1 d . . . H67A H 0.3241 0.2965 0.9084 0.104 Uiso 1 1 calc R . . C68 C 0.3175(5) 0.3412(4) 0.8168(3) 0.0652(14) Uani 1 1 d . . . C69 C 0.0689(4) 0.2824(3) 0.6791(2) 0.0489(11) Uani 1 1 d . . . C70 C 0.0379(4) 0.1842(4) 0.6733(3) 0.0622(13) Uani 1 1 d . . . H70A H 0.0888 0.1424 0.6940 0.075 Uiso 1 1 calc R . . C71 C -0.0677(5) 0.1490(4) 0.6373(3) 0.0679(14) Uani 1 1 d . . . H71A H -0.0891 0.0824 0.6330 0.082 Uiso 1 1 calc R . . C72 C -0.1427(4) 0.2095(4) 0.6072(3) 0.0700(15) Uani 1 1 d . . . H72A H -0.2153 0.1849 0.5832 0.084 Uiso 1 1 calc R . . C73 C -0.1109(4) 0.3064(4) 0.6126(3) 0.0695(15) Uani 1 1 d . . . H73A H -0.1620 0.3482 0.5921 0.083 Uiso 1 1 calc R . . C74 C -0.0043(4) 0.3430(4) 0.6478(3) 0.0590(12) Uani 1 1 d . . . H74A H 0.0177 0.4088 0.6502 0.071 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 0.03758(9) 0.04256(10) 0.04936(11) 0.01237(8) 0.01802(8) 0.00041(7) Pt2 0.05094(11) 0.04424(10) 0.04660(11) 0.01380(8) 0.01745(8) 0.00433(8) O1 0.0438(17) 0.071(2) 0.0460(18) 0.0085(16) 0.0173(14) -0.0093(15) O2 0.044(2) 0.111(3) 0.108(4) 0.038(3) -0.003(2) -0.017(2) O3 0.0510(18) 0.063(2) 0.0457(18) 0.0173(15) 0.0159(15) 0.0044(15) O4 0.060(2) 0.073(2) 0.050(2) 0.0230(17) 0.0128(17) 0.0021(17) N1 0.0413(19) 0.0394(19) 0.047(2) 0.0091(16) 0.0191(17) 0.0015(15) N2 0.042(2) 0.051(2) 0.058(2) 0.0237(19) 0.0199(18) 0.0049(17) N3 0.044(2) 0.074(3) 0.069(3) 0.034(2) 0.024(2) 0.005(2) N4 0.048(2) 0.047(2) 0.051(2) 0.0127(18) 0.0166(18) 0.0010(17) N5 0.057(2) 0.050(2) 0.050(2) 0.0163(18) 0.0207(19) 0.0065(18) N6 0.065(3) 0.078(3) 0.058(3) 0.025(2) 0.018(2) 0.000(2) C1 0.049(3) 0.045(2) 0.051(3) 0.011(2) 0.026(2) 0.002(2) C2 0.041(2) 0.040(2) 0.059(3) 0.012(2) 0.020(2) 0.0020(19) C3 0.044(2) 0.041(2) 0.060(3) 0.014(2) 0.018(2) -0.0011(19) C4 0.050(3) 0.060(3) 0.058(3) 0.015(2) 0.012(2) -0.005(2) C5 0.046(3) 0.055(3) 0.086(4) 0.027(3) 0.008(3) -0.004(2) C6 0.041(3) 0.073(4) 0.100(5) 0.029(3) 0.030(3) -0.001(2) C7 0.048(3) 0.060(3) 0.070(3) 0.018(3) 0.027(2) 0.002(2) C8 0.075(5) 0.194(9) 0.095(6) 0.043(6) -0.020(4) -0.050(5) C9 0.147(10) 0.355(19) 0.133(9) 0.109(11) -0.066(8) -0.109(11) C10 0.135(10) 0.36(2) 0.237(16) 0.151(16) -0.090(10) -0.084(12) C11 0.090(7) 0.234(15) 0.203(12) 0.014(10) -0.030(8) -0.008(8) C12 0.139(11) 0.286(19) 0.179(13) 0.015(12) 0.031(10) -0.060(12) C13 0.098(7) 0.328(18) 0.192(12) -0.025(12) 0.002(8) -0.033(9) C14 0.040(2) 0.040(2) 0.048(3) 0.009(2) 0.014(2) -0.0022(19) C15 0.058(3) 0.046(3) 0.058(3) 0.006(2) 0.020(2) -0.004(2) C16 0.070(3) 0.058(3) 0.050(3) 0.014(2) 0.008(3) -0.015(3) C17 0.054(3) 0.068(3) 0.079(4) 0.040(3) 0.003(3) -0.013(3) C18 0.044(3) 0.065(3) 0.085(4) 0.033(3) 0.024(3) 0.007(2) C19 0.047(3) 0.048(3) 0.060(3) 0.013(2) 0.026(2) 0.001(2) C20 0.079(4) 0.116(5) 0.105(5) 0.068(5) -0.015(4) -0.020(4) C21 0.058(3) 0.086(4) 0.080(4) 0.035(3) 0.007(3) 0.004(3) C22 0.073(4) 0.093(5) 0.085(4) 0.031(4) -0.006(3) -0.004(3) C23 0.072(4) 0.177(8) 0.112(6) 0.072(6) -0.013(4) -0.016(5) C24 0.078(5) 0.158(8) 0.130(7) 0.044(6) -0.013(5) -0.004(5) C25 0.089(7) 0.351(18) 0.181(11) 0.116(12) -0.013(7) -0.029(9) C26 0.036(2) 0.040(2) 0.066(3) 0.016(2) 0.020(2) 0.0031(18) C27 0.043(2) 0.049(3) 0.063(3) 0.012(2) 0.016(2) -0.002(2) C28 0.047(3) 0.064(3) 0.074(4) 0.019(3) 0.010(3) -0.004(2) C29 0.041(3) 0.087(4) 0.094(4) 0.043(3) 0.016(3) -0.002(3) C30 0.042(3) 0.097(4) 0.085(4) 0.049(3) 0.025(3) 0.006(3) C31 0.039(2) 0.062(3) 0.062(3) 0.028(2) 0.014(2) 0.004(2) C32 0.047(3) 0.057(3) 0.058(3) 0.021(2) 0.018(2) -0.002(2) C33 0.047(3) 0.069(3) 0.061(3) 0.023(3) 0.017(2) 0.003(2) C34 0.057(3) 0.108(5) 0.074(4) 0.032(4) 0.013(3) 0.004(3) C35 0.077(4) 0.133(6) 0.060(4) 0.033(4) 0.006(3) -0.004(4) C36 0.089(5) 0.121(6) 0.061(4) 0.022(4) 0.030(4) 0.000(4) C37 0.063(3) 0.086(4) 0.065(4) 0.025(3) 0.028(3) 0.007(3) C38 0.058(3) 0.046(3) 0.063(3) 0.017(2) 0.029(3) 0.005(2) C39 0.055(3) 0.043(2) 0.047(3) 0.012(2) 0.018(2) 0.006(2) C40 0.055(3) 0.046(2) 0.044(3) 0.015(2) 0.020(2) 0.011(2) C41 0.051(3) 0.048(3) 0.057(3) 0.017(2) 0.019(2) 0.006(2) C42 0.059(3) 0.045(3) 0.050(3) 0.014(2) 0.015(2) 0.009(2) C43 0.067(3) 0.067(3) 0.052(3) 0.025(3) 0.021(3) 0.003(3) C44 0.061(3) 0.063(3) 0.054(3) 0.019(2) 0.026(3) 0.000(2) C45 0.065(3) 0.058(3) 0.055(3) 0.017(2) 0.024(3) 0.008(2) C46 0.063(3) 0.068(3) 0.056(3) 0.019(3) 0.019(3) 0.005(3) C47 0.065(3) 0.065(3) 0.065(3) 0.013(3) 0.028(3) 0.005(3) C48 0.062(3) 0.081(4) 0.067(4) 0.016(3) 0.022(3) -0.002(3) C49 0.072(4) 0.096(5) 0.086(5) 0.015(4) 0.031(3) -0.003(3) C50 0.069(4) 0.150(7) 0.092(5) 0.031(5) 0.008(4) -0.017(4) C51 0.054(3) 0.049(3) 0.048(3) 0.009(2) 0.019(2) 0.003(2) C52 0.056(3) 0.048(3) 0.068(3) 0.009(2) 0.006(3) -0.001(2) C53 0.058(3) 0.063(3) 0.077(4) 0.012(3) 0.004(3) 0.008(3) C54 0.053(3) 0.091(4) 0.057(3) 0.016(3) 0.011(3) -0.011(3) C55 0.066(3) 0.061(3) 0.076(4) 0.017(3) 0.021(3) -0.014(3) C56 0.062(3) 0.054(3) 0.071(3) 0.019(3) 0.023(3) -0.005(2) C57 0.066(4) 0.131(6) 0.082(5) 0.033(4) 0.003(3) -0.019(4) C58 0.119(9) 0.83(5) 0.142(11) 0.217(19) -0.023(7) -0.171(16) C59 0.122(8) 0.335(18) 0.132(10) 0.080(11) 0.004(7) -0.025(10) C60 0.104(7) 0.40(2) 0.142(10) 0.144(12) -0.023(7) -0.035(10) C61 0.139(11) 0.93(6) 0.220(16) 0.36(3) 0.069(11) 0.091(19) C62 0.38(2) 0.318(18) 0.199(13) 0.166(13) 0.203(15) 0.181(17) C63 0.063(3) 0.044(2) 0.042(3) 0.004(2) 0.019(2) 0.003(2) C64 0.070(3) 0.086(4) 0.056(3) 0.015(3) 0.016(3) -0.007(3) C65 0.079(4) 0.107(5) 0.055(4) 0.015(3) 0.005(3) -0.010(4) C66 0.088(5) 0.127(6) 0.053(4) 0.035(4) 0.011(3) 0.001(4) C67 0.087(4) 0.118(5) 0.061(4) 0.044(4) 0.019(3) -0.006(4) C68 0.071(3) 0.073(4) 0.052(3) 0.019(3) 0.017(3) 0.003(3) C69 0.054(3) 0.052(3) 0.046(3) 0.017(2) 0.020(2) 0.004(2) C70 0.070(3) 0.051(3) 0.071(3) 0.021(3) 0.024(3) 0.012(3) C71 0.073(4) 0.050(3) 0.079(4) 0.013(3) 0.023(3) -0.002(3) C72 0.058(3) 0.068(4) 0.079(4) 0.006(3) 0.019(3) -0.003(3) C73 0.059(3) 0.064(3) 0.088(4) 0.024(3) 0.020(3) 0.012(3) C74 0.062(3) 0.050(3) 0.069(3) 0.019(3) 0.024(3) 0.003(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 C26 1.969(4) . ? Pt1 N2 1.978(4) . ? Pt1 N1 2.003(3) . ? Pt1 O1 2.030(3) . ? Pt2 C63 1.974(5) . ? Pt2 N5 1.979(4) . ? Pt2 N4 1.999(4) . ? Pt2 O3 2.041(3) . ? O1 C3 1.292(5) . ? O2 C5 1.354(6) . ? O2 C8 1.402(9) . ? O3 C40 1.284(5) . ? O4 C42 1.347(5) . ? O4 C45 1.412(6) . ? N1 C1 1.307(5) . ? N1 C14 1.419(5) . ? N2 N3 1.277(5) . ? N2 C32 1.416(6) . ? N3 C31 1.379(6) . ? N4 C38 1.314(6) . ? N4 C51 1.433(6) . ? N5 N6 1.274(5) . ? N5 C69 1.429(6) . ? N6 C68 1.361(7) . ? C1 C2 1.396(6) . ? C2 C7 1.402(6) . ? C2 C3 1.406(6) . ? C3 C4 1.389(6) . ? C4 C5 1.362(7) . ? C5 C6 1.388(8) . ? C6 C7 1.340(7) . ? C8 C9 1.525(11) . ? C9 C10 1.049(12) . ? C10 C11 1.569(14) . ? C11 C12 1.307(16) . ? C12 C13 1.482(13) . ? C14 C19 1.361(6) . ? C14 C15 1.374(6) . ? C15 C16 1.366(7) . ? C16 C17 1.373(8) . ? C17 C18 1.365(8) . ? C17 C20 1.502(7) . ? C18 C19 1.379(7) . ? C20 C21 1.415(8) . ? C21 C22 1.461(7) . ? C22 C23 1.391(8) . ? C23 C24 1.449(9) . ? C24 C25 1.383(11) . ? C26 C27 1.390(6) . ? C26 C31 1.392(6) . ? C27 C28 1.380(6) . ? C28 C29 1.364(7) . ? C29 C30 1.358(7) . ? C30 C31 1.394(6) . ? C32 C37 1.367(7) . ? C32 C33 1.373(6) . ? C33 C34 1.364(7) . ? C34 C35 1.355(8) . ? C35 C36 1.372(9) . ? C36 C37 1.369(8) . ? C38 C39 1.381(6) . ? C39 C44 1.406(6) . ? C39 C40 1.413(6) . ? C40 C41 1.400(6) . ? C41 C42 1.358(6) . ? C42 C43 1.393(7) . ? C43 C44 1.340(7) . ? C45 C46 1.504(7) . ? C46 C47 1.491(7) . ? C47 C48 1.512(7) . ? C48 C49 1.493(7) . ? C49 C50 1.486(8) . ? C51 C52 1.358(6) . ? C51 C56 1.366(6) . ? C52 C53 1.366(7) . ? C53 C54 1.381(7) . ? C54 C55 1.350(8) . ? C54 C57 1.518(8) . ? C55 C56 1.359(7) . ? C57 C58 1.385(13) . ? C58 C59 1.232(13) . ? C59 C60 1.517(15) . ? C60 C61 1.238(16) . ? C61 C62 1.294(16) . ? C63 C64 1.383(7) . ? C63 C68 1.404(7) . ? C64 C65 1.362(7) . ? C65 C66 1.371(8) . ? C66 C67 1.348(8) . ? C67 C68 1.392(7) . ? C69 C74 1.355(6) . ? C69 C70 1.372(6) . ? C70 C71 1.356(7) . ? C71 C72 1.359(7) . ? C72 C73 1.360(7) . ? C73 C74 1.367(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 C26 Pt1 N2 78.94(17) . . ? C26 Pt1 N1 100.67(16) . . ? N2 Pt1 N1 178.22(14) . . ? C26 Pt1 O1 170.55(15) . . ? N2 Pt1 O1 91.80(14) . . ? N1 Pt1 O1 88.53(13) . . ? C63 Pt2 N5 78.59(18) . . ? C63 Pt2 N4 101.55(18) . . ? N5 Pt2 N4 171.90(15) . . ? C63 Pt2 O3 168.77(16) . . ? N5 Pt2 O3 90.54(15) . . ? N4 Pt2 O3 89.61(14) . . ? C3 O1 Pt1 126.5(3) . . ? C5 O2 C8 118.7(5) . . ? C40 O3 Pt2 129.8(3) . . ? C42 O4 C45 119.3(4) . . ? C1 N1 C14 116.6(4) . . ? C1 N1 Pt1 122.3(3) . . ? C14 N1 Pt1 121.1(3) . . ? N3 N2 C32 113.6(4) . . ? N3 N2 Pt1 119.2(3) . . ? C32 N2 Pt1 127.1(3) . . ? N2 N3 C31 111.2(4) . . ? C38 N4 C51 113.7(4) . . ? C38 N4 Pt2 123.6(3) . . ? C51 N4 Pt2 122.5(3) . . ? N6 N5 C69 113.5(4) . . ? N6 N5 Pt2 119.8(3) . . ? C69 N5 Pt2 126.3(3) . . ? N5 N6 C68 111.4(4) . . ? N1 C1 C2 128.7(4) . . ? C1 C2 C7 118.4(4) . . ? C1 C2 C3 122.6(4) . . ? C7 C2 C3 118.3(4) . . ? O1 C3 C4 117.4(4) . . ? O1 C3 C2 123.6(4) . . ? C4 C3 C2 118.9(4) . . ? C5 C4 C3 120.5(5) . . ? O2 C5 C4 123.4(5) . . ? O2 C5 C6 115.8(5) . . ? C4 C5 C6 120.8(5) . . ? C7 C6 C5 119.3(5) . . ? C6 C7 C2 121.9(5) . . ? O2 C8 C9 108.4(8) . . ? C10 C9 C8 127.4(13) . . ? C9 C10 C11 128.0(15) . . ? C12 C11 C10 114.3(13) . . ? C11 C12 C13 115.8(14) . . ? C19 C14 C15 119.0(4) . . ? C19 C14 N1 119.4(4) . . ? C15 C14 N1 121.6(4) . . ? C16 C15 C14 120.8(5) . . ? C15 C16 C17 120.8(5) . . ? C18 C17 C16 117.8(5) . . ? C18 C17 C20 120.7(6) . . ? C16 C17 C20 121.4(6) . . ? C17 C18 C19 121.9(5) . . ? C14 C19 C18 119.6(5) . . ? C21 C20 C17 118.6(5) . . ? C20 C21 C22 120.7(5) . . ? C23 C22 C21 125.5(6) . . ? C22 C23 C24 123.9(7) . . ? C25 C24 C23 124.3(9) . . ? C27 C26 C31 114.8(4) . . ? C27 C26 Pt1 134.6(3) . . ? C31 C26 Pt1 110.6(3) . . ? C28 C27 C26 121.3(5) . . ? C29 C28 C27 121.7(5) . . ? C30 C29 C28 119.5(5) . . ? C29 C30 C31 118.5(5) . . ? N3 C31 C26 118.7(4) . . ? N3 C31 C30 117.2(4) . . ? C26 C31 C30 123.9(5) . . ? C37 C32 C33 120.1(5) . . ? C37 C32 N2 120.6(4) . . ? C33 C32 N2 119.3(4) . . ? C34 C33 C32 119.0(5) . . ? C35 C34 C33 121.9(6) . . ? C34 C35 C36 118.8(6) . . ? C37 C36 C35 120.5(6) . . ? C32 C37 C36 119.7(5) . . ? N4 C38 C39 130.3(4) . . ? C38 C39 C44 117.6(4) . . ? C38 C39 C40 124.0(4) . . ? C44 C39 C40 118.1(4) . . ? O3 C40 C41 118.5(4) . . ? O3 C40 C39 122.4(4) . . ? C41 C40 C39 119.1(4) . . ? C42 C41 C40 120.2(4) . . ? O4 C42 C41 125.3(4) . . ? O4 C42 C43 113.7(4) . . ? C41 C42 C43 121.0(5) . . ? C44 C43 C42 119.7(4) . . ? C43 C44 C39 121.7(5) . . ? O4 C45 C46 105.9(4) . . ? C47 C46 C45 114.4(4) . . ? C46 C47 C48 113.0(4) . . ? C49 C48 C47 115.1(5) . . ? C50 C49 C48 113.5(5) . . ? C52 C51 C56 119.9(5) . . ? C52 C51 N4 119.7(4) . . ? C56 C51 N4 120.4(4) . . ? C51 C52 C53 119.4(5) . . ? C52 C53 C54 121.3(5) . . ? C55 C54 C53 117.7(5) . . ? C55 C54 C57 121.2(6) . . ? C53 C54 C57 121.0(6) . . ? C54 C55 C56 121.8(5) . . ? C55 C56 C51 119.8(5) . . ? C58 C57 C54 112.0(7) . . ? C59 C58 C57 143.8(14) . . ? C58 C59 C60 151.7(15) . . ? C61 C60 C59 139.9(19) . . ? C60 C61 C62 133(3) . . ? C64 C63 C68 114.6(5) . . ? C64 C63 Pt2 134.7(4) . . ? C68 C63 Pt2 110.6(4) . . ? C65 C64 C63 122.1(5) . . ? C64 C65 C66 122.0(6) . . ? C67 C66 C65 118.5(5) . . ? C66 C67 C68 119.9(6) . . ? N6 C68 C67 118.2(5) . . ? N6 C68 C63 118.9(5) . . ? C67 C68 C63 122.8(5) . . ? C74 C69 C70 120.6(5) . . ? C74 C69 N5 119.6(4) . . ? C70 C69 N5 119.8(4) . . ? C71 C70 C69 119.2(5) . . ? C70 C71 C72 120.9(5) . . ? C71 C72 C73 119.5(5) . . ? C72 C73 C74 120.5(5) . . ? C69 C74 C73 119.3(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 C26 Pt1 O1 C3 -167.4(8) . . . . ? N2 Pt1 O1 C3 -156.0(4) . . . . ? N1 Pt1 O1 C3 25.8(4) . . . . ? C63 Pt2 O3 C40 168.1(7) . . . . ? N5 Pt2 O3 C40 -177.4(4) . . . . ? N4 Pt2 O3 C40 -5.5(4) . . . . ? C26 Pt1 N1 C1 156.4(3) . . . . ? N2 Pt1 N1 C1 -127(5) . . . . ? O1 Pt1 N1 C1 -25.8(3) . . . . ? C26 Pt1 N1 C14 -24.4(3) . . . . ? N2 Pt1 N1 C14 53(5) . . . . ? O1 Pt1 N1 C14 153.4(3) . . . . ? C26 Pt1 N2 N3 10.6(3) . . . . ? N1 Pt1 N2 N3 -67(5) . . . . ? O1 Pt1 N2 N3 -167.5(3) . . . . ? C26 Pt1 N2 C32 -172.4(4) . . . . ? N1 Pt1 N2 C32 110(5) . . . . ? O1 Pt1 N2 C32 9.5(4) . . . . ? C32 N2 N3 C31 174.6(4) . . . . ? Pt1 N2 N3 C31 -8.0(5) . . . . ? C63 Pt2 N4 C38 -174.7(4) . . . . ? N5 Pt2 N4 C38 95.1(11) . . . . ? O3 Pt2 N4 C38 4.0(4) . . . . ? C63 Pt2 N4 C51 11.0(4) . . . . ? N5 Pt2 N4 C51 -79.2(11) . . . . ? O3 Pt2 N4 C51 -170.3(3) . . . . ? C63 Pt2 N5 N6 -8.5(4) . . . . ? N4 Pt2 N5 N6 83.3(11) . . . . ? O3 Pt2 N5 N6 174.4(4) . . . . ? C63 Pt2 N5 C69 179.5(4) . . . . ? N4 Pt2 N5 C69 -88.7(11) . . . . ? O3 Pt2 N5 C69 2.3(4) . . . . ? C69 N5 N6 C68 -179.0(4) . . . . ? Pt2 N5 N6 C68 8.0(6) . . . . ? C14 N1 C1 C2 -165.3(4) . . . . ? Pt1 N1 C1 C2 14.0(6) . . . . ? N1 C1 C2 C7 -179.1(4) . . . . ? N1 C1 C2 C3 10.9(7) . . . . ? Pt1 O1 C3 C4 171.1(3) . . . . ? Pt1 O1 C3 C2 -11.5(6) . . . . ? C1 C2 C3 O1 -12.3(7) . . . . ? C7 C2 C3 O1 177.7(4) . . . . ? C1 C2 C3 C4 165.1(4) . . . . ? C7 C2 C3 C4 -4.8(6) . . . . ? O1 C3 C4 C5 -179.4(4) . . . . ? C2 C3 C4 C5 3.0(7) . . . . ? C8 O2 C5 C4 10.2(8) . . . . ? C8 O2 C5 C6 -168.9(6) . . . . ? C3 C4 C5 O2 -177.3(5) . . . . ? C3 C4 C5 C6 1.8(8) . . . . ? O2 C5 C6 C7 174.4(5) . . . . ? C4 C5 C6 C7 -4.7(8) . . . . ? C5 C6 C7 C2 2.8(8) . . . . ? C1 C2 C7 C6 -168.4(5) . . . . ? C3 C2 C7 C6 2.0(7) . . . . ? C5 O2 C8 C9 162.9(8) . . . . ? O2 C8 C9 C10 137(2) . . . . ? C8 C9 C10 C11 178.7(14) . . . . ? C9 C10 C11 C12 123(3) . . . . ? C10 C11 C12 C13 169.8(12) . . . . ? C1 N1 C14 C19 124.8(4) . . . . ? Pt1 N1 C14 C19 -54.5(5) . . . . ? C1 N1 C14 C15 -56.0(5) . . . . ? Pt1 N1 C14 C15 124.7(4) . . . . ? C19 C14 C15 C16 2.7(6) . . . . ? N1 C14 C15 C16 -176.6(4) . . . . ? C14 C15 C16 C17 -1.3(7) . . . . ? C15 C16 C17 C18 -0.8(7) . . . . ? C15 C16 C17 C20 178.1(5) . . . . ? C16 C17 C18 C19 1.4(7) . . . . ? C20 C17 C18 C19 -177.4(4) . . . . ? C15 C14 C19 C18 -2.0(6) . . . . ? N1 C14 C19 C18 177.3(4) . . . . ? C17 C18 C19 C14 0.0(7) . . . . ? C18 C17 C20 C21 92.5(8) . . . . ? C16 C17 C20 C21 -86.3(8) . . . . ? C17 C20 C21 C22 180.0(7) . . . . ? C20 C21 C22 C23 -179.3(8) . . . . ? C21 C22 C23 C24 -176.4(8) . . . . ? C22 C23 C24 C25 179.1(11) . . . . ? N2 Pt1 C26 C27 169.3(5) . . . . ? N1 Pt1 C26 C27 -12.4(5) . . . . ? O1 Pt1 C26 C27 -179.0(7) . . . . ? N2 Pt1 C26 C31 -9.9(3) . . . . ? N1 Pt1 C26 C31 168.4(3) . . . . ? O1 Pt1 C26 C31 1.8(11) . . . . ? C31 C26 C27 C28 -3.7(7) . . . . ? Pt1 C26 C27 C28 177.1(4) . . . . ? C26 C27 C28 C29 -0.1(8) . . . . ? C27 C28 C29 C30 2.6(8) . . . . ? C28 C29 C30 C31 -0.9(8) . . . . ? N2 N3 C31 C26 -1.3(6) . . . . ? N2 N3 C31 C30 -177.0(4) . . . . ? C27 C26 C31 N3 -169.9(4) . . . . ? Pt1 C26 C31 N3 9.5(5) . . . . ? C27 C26 C31 C30 5.5(7) . . . . ? Pt1 C26 C31 C30 -175.1(4) . . . . ? C29 C30 C31 N3 172.1(5) . . . . ? C29 C30 C31 C26 -3.3(8) . . . . ? N3 N2 C32 C37 36.5(6) . . . . ? Pt1 N2 C32 C37 -140.6(4) . . . . ? N3 N2 C32 C33 -141.7(5) . . . . ? Pt1 N2 C32 C33 41.2(6) . . . . ? C37 C32 C33 C34 -0.7(8) . . . . ? N2 C32 C33 C34 177.5(5) . . . . ? C32 C33 C34 C35 1.1(9) . . . . ? C33 C34 C35 C36 -1.1(10) . . . . ? C34 C35 C36 C37 0.7(11) . . . . ? C33 C32 C37 C36 0.3(8) . . . . ? N2 C32 C37 C36 -177.9(5) . . . . ? C35 C36 C37 C32 -0.3(10) . . . . ? C51 N4 C38 C39 174.6(5) . . . . ? Pt2 N4 C38 C39 -0.1(7) . . . . ? N4 C38 C39 C44 -178.6(5) . . . . ? N4 C38 C39 C40 -4.9(8) . . . . ? Pt2 O3 C40 C41 -177.1(3) . . . . ? Pt2 O3 C40 C39 2.7(6) . . . . ? C38 C39 C40 O3 3.4(7) . . . . ? C44 C39 C40 O3 177.1(4) . . . . ? C38 C39 C40 C41 -176.8(4) . . . . ? C44 C39 C40 C41 -3.1(6) . . . . ? O3 C40 C41 C42 -177.9(4) . . . . ? C39 C40 C41 C42 2.3(7) . . . . ? C45 O4 C42 C41 2.5(7) . . . . ? C45 O4 C42 C43 -178.4(4) . . . . ? C40 C41 C42 O4 178.8(4) . . . . ? C40 C41 C42 C43 -0.3(7) . . . . ? O4 C42 C43 C44 180.0(4) . . . . ? C41 C42 C43 C44 -0.9(8) . . . . ? C42 C43 C44 C39 -0.1(8) . . . . ? C38 C39 C44 C43 176.2(5) . . . . ? C40 C39 C44 C43 2.1(7) . . . . ? C42 O4 C45 C46 -176.0(4) . . . . ? O4 C45 C46 C47 -178.8(4) . . . . ? C45 C46 C47 C48 -178.8(5) . . . . ? C46 C47 C48 C49 -179.9(5) . . . . ? C47 C48 C49 C50 176.1(6) . . . . ? C38 N4 C51 C52 -112.3(5) . . . . ? Pt2 N4 C51 C52 62.5(5) . . . . ? C38 N4 C51 C56 67.3(6) . . . . ? Pt2 N4 C51 C56 -117.9(4) . . . . ? C56 C51 C52 C53 -0.1(8) . . . . ? N4 C51 C52 C53 179.5(5) . . . . ? C51 C52 C53 C54 1.5(9) . . . . ? C52 C53 C54 C55 -1.2(9) . . . . ? C52 C53 C54 C57 176.8(5) . . . . ? C53 C54 C55 C56 -0.7(8) . . . . ? C57 C54 C55 C56 -178.6(5) . . . . ? C54 C55 C56 C51 2.1(8) . . . . ? C52 C51 C56 C55 -1.7(8) . . . . ? N4 C51 C56 C55 178.7(5) . . . . ? C55 C54 C57 C58 92.1(13) . . . . ? C53 C54 C57 C58 -85.8(13) . . . . ? C54 C57 C58 C59 38(4) . . . . ? C57 C58 C59 C60 -174(2) . . . . ? C58 C59 C60 C61 -157(3) . . . . ? C59 C60 C61 C62 178.9(16) . . . . ? N5 Pt2 C63 C64 -170.5(6) . . . . ? N4 Pt2 C63 C64 17.8(6) . . . . ? O3 Pt2 C63 C64 -155.6(7) . . . . ? N5 Pt2 C63 C68 6.3(4) . . . . ? N4 Pt2 C63 C68 -165.4(4) . . . . ? O3 Pt2 C63 C68 21.2(10) . . . . ? C68 C63 C64 C65 1.3(8) . . . . ? Pt2 C63 C64 C65 178.0(5) . . . . ? C63 C64 C65 C66 1.4(10) . . . . ? C64 C65 C66 C67 -2.5(11) . . . . ? C65 C66 C67 C68 0.9(11) . . . . ? N5 N6 C68 C67 174.1(5) . . . . ? N5 N6 C68 C63 -1.9(7) . . . . ? C66 C67 C68 N6 -173.9(6) . . . . ? C66 C67 C68 C63 1.9(10) . . . . ? C64 C63 C68 N6 172.9(5) . . . . ? Pt2 C63 C68 N6 -4.6(6) . . . . ? C64 C63 C68 C67 -3.0(8) . . . . ? Pt2 C63 C68 C67 179.5(5) . . . . ? N6 N5 C69 C74 129.8(5) . . . . ? Pt2 N5 C69 C74 -57.7(6) . . . . ? N6 N5 C69 C70 -49.9(6) . . . . ? Pt2 N5 C69 C70 122.5(4) . . . . ? C74 C69 C70 C71 -1.5(8) . . . . ? N5 C69 C70 C71 178.2(4) . . . . ? C69 C70 C71 C72 -0.3(8) . . . . ? C70 C71 C72 C73 1.0(9) . . . . ? C71 C72 C73 C74 0.1(9) . . . . ? C70 C69 C74 C73 2.6(7) . . . . ? N5 C69 C74 C73 -177.2(5) . . . . ? C72 C73 C74 C69 -1.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.251 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.087 #===END data_(PYPDON) _database_code_depnum_ccdc_archive 'CCDC 776862' #TrackingRef 'acrispini.CIF' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C36 H42 N2 O2 Pd' _chemical_formula_sum 'C36 H42 N2 O2 Pd' _chemical_formula_weight 641.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 5.9863(4) _cell_length_b 8.2081(7) _cell_length_c 32.135(3) _cell_angle_alpha 94.509(4) _cell_angle_beta 92.828(4) _cell_angle_gamma 92.317(4) _cell_volume 1570.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 6726 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 26.82 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.625 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.7850 _exptl_absorpt_correction_T_max 0.8750 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28179 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.0393 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 0.64 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6328 _reflns_number_gt 5344 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0534P)^2^+0.1018P] 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 6328 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0848 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.154 _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 Pd Pd 0.80217(3) -0.05016(3) 0.738304(8) 0.03950(10) Uani 1 1 d . . . O1 O 0.6606(3) -0.1126(3) 0.67907(7) 0.0510(6) Uani 1 1 d . . . O2 O 0.1276(4) -0.1796(3) 0.56847(8) 0.0683(7) Uani 1 1 d . . . N1 N 0.5927(4) 0.1395(3) 0.74586(8) 0.0393(6) Uani 1 1 d . . . N2 N 1.0245(4) -0.2260(3) 0.72723(8) 0.0416(6) Uani 1 1 d . . . C1 C 0.4151(5) 0.1515(4) 0.72093(10) 0.0432(7) Uani 1 1 d . . . H1 H 0.3198 0.2331 0.7293 0.052 Uiso 1 1 calc R . . C2 C 0.3466(5) 0.0585(4) 0.68299(10) 0.0427(7) Uani 1 1 d . . . C3 C 0.1438(5) 0.0988(4) 0.66299(11) 0.0512(8) Uani 1 1 d . . . H3A H 0.0598 0.1788 0.6761 0.061 Uiso 1 1 calc R . . C4 C 0.0655(5) 0.0254(4) 0.62518(11) 0.0547(9) Uani 1 1 d . . . H4A H -0.0689 0.0549 0.6128 0.066 Uiso 1 1 calc R . . C5 C 0.1913(5) -0.0947(4) 0.60556(11) 0.0512(8) Uani 1 1 d . . . C6 C 0.3927(5) -0.1364(4) 0.62365(10) 0.0481(8) Uani 1 1 d . . . H6A H 0.4764 -0.2140 0.6095 0.058 Uiso 1 1 calc R . . C7 C 0.4743(5) -0.0647(4) 0.66274(10) 0.0423(7) Uani 1 1 d . . . C8 C -0.0840(6) -0.1471(5) 0.54916(12) 0.0649(10) Uani 1 1 d . . . H8A H -0.0831 -0.0352 0.5415 0.078 Uiso 1 1 calc R . . H8B H -0.2014 -0.1616 0.5685 0.078 Uiso 1 1 calc R . . C9 C -0.1267(7) -0.2632(5) 0.51100(12) 0.0693(11) Uani 1 1 d . . . H9A H -0.1367 -0.3744 0.5192 0.083 Uiso 1 1 calc R . . H9B H -0.0022 -0.2544 0.4930 0.083 Uiso 1 1 calc R . . C10 C -0.3406(7) -0.2276(6) 0.48717(13) 0.0738(12) Uani 1 1 d . . . H10A H -0.4635 -0.2362 0.5056 0.089 Uiso 1 1 calc R . . H10B H -0.3297 -0.1155 0.4797 0.089 Uiso 1 1 calc R . . C11 C -0.3956(7) -0.3368(6) 0.44845(13) 0.0792(12) Uani 1 1 d . . . H11A H -0.4158 -0.4483 0.4561 0.095 Uiso 1 1 calc R . . H11B H -0.2695 -0.3331 0.4307 0.095 Uiso 1 1 calc R . . C12 C -0.6015(7) -0.2935(6) 0.42391(14) 0.0849(14) Uani 1 1 d . . . H12A H -0.7247 -0.2919 0.4424 0.102 Uiso 1 1 calc R . . H12B H -0.5775 -0.1831 0.4158 0.102 Uiso 1 1 calc R . . C13 C -0.6712(9) -0.3975(7) 0.38670(16) 0.117(2) Uani 1 1 d . . . H13A H -0.8056 -0.3581 0.3743 0.175 Uiso 1 1 calc R . . H13B H -0.6991 -0.5074 0.3940 0.175 Uiso 1 1 calc R . . H13C H -0.5552 -0.3961 0.3671 0.175 Uiso 1 1 calc R . . C14 C 0.6245(5) 0.2663(4) 0.77901(9) 0.0386(7) Uani 1 1 d . . . C15 C 0.8209(5) 0.3647(4) 0.78191(10) 0.0444(7) Uani 1 1 d . . . H15A H 0.9271 0.3495 0.7620 0.053 Uiso 1 1 calc R . . C16 C 0.8576(5) 0.4838(4) 0.81408(10) 0.0476(8) Uani 1 1 d . . . H16A H 0.9886 0.5493 0.8155 0.057 Uiso 1 1 calc R . . C17 C 0.7043(5) 0.5091(4) 0.84464(10) 0.0460(7) Uani 1 1 d . . . C18 C 0.5076(5) 0.4114(4) 0.84077(10) 0.0476(8) Uani 1 1 d . . . H18A H 0.4014 0.4263 0.8607 0.057 Uiso 1 1 calc R . . C19 C 0.4665(5) 0.2934(4) 0.80824(10) 0.0446(7) Uani 1 1 d . . . H19A H 0.3319 0.2319 0.8059 0.054 Uiso 1 1 calc R . . C20 C 0.7529(6) 0.6345(4) 0.88118(11) 0.0565(9) Uani 1 1 d . . . H20A H 0.6221 0.6403 0.8978 0.068 Uiso 1 1 calc R . . H20B H 0.7786 0.7408 0.8706 0.068 Uiso 1 1 calc R . . C21 C 0.9532(6) 0.5984(5) 0.90905(12) 0.0629(10) Uani 1 1 d . . . H21A H 0.9365 0.4868 0.9167 0.076 Uiso 1 1 calc R . . H21B H 1.0872 0.6068 0.8934 0.076 Uiso 1 1 calc R . . C22 C 0.9827(7) 0.7119(5) 0.94824(12) 0.0699(11) Uani 1 1 d . . . H22A H 0.8539 0.6966 0.9649 0.084 Uiso 1 1 calc R . . H22B H 0.9859 0.8238 0.9405 0.084 Uiso 1 1 calc R . . C23 C 1.1930(8) 0.6872(7) 0.97485(14) 0.0898(14) Uani 1 1 d . . . H23A H 1.1942 0.5734 0.9810 0.108 Uiso 1 1 calc R . . H23B H 1.3219 0.7090 0.9587 0.108 Uiso 1 1 calc R . . C24 C 1.2181(11) 0.7913(8) 1.01496(17) 0.120(2) Uani 1 1 d . . . H24A H 1.0881 0.7712 1.0310 0.144 Uiso 1 1 calc R . . H24B H 1.2205 0.9052 1.0089 0.144 Uiso 1 1 calc R . . C25 C 1.4259(12) 0.7627(10) 1.0414(2) 0.161(3) Uani 1 1 d . . . H25A H 1.4312 0.8347 1.0665 0.242 Uiso 1 1 calc R . . H25B H 1.5559 0.7841 1.0260 0.242 Uiso 1 1 calc R . . H25C H 1.4226 0.6513 1.0485 0.242 Uiso 1 1 calc R . . C26 C 0.9688(5) -0.0321(4) 0.79392(10) 0.0430(7) Uani 1 1 d . . . C27 C 0.9226(6) 0.0516(4) 0.83199(10) 0.0494(8) Uani 1 1 d . . . H27A H 0.7934 0.1105 0.8337 0.059 Uiso 1 1 calc R . . C28 C 1.0654(6) 0.0483(5) 0.86697(11) 0.0590(9) Uani 1 1 d . . . H28A H 1.0312 0.1060 0.8918 0.071 Uiso 1 1 calc R . . C29 C 1.2592(7) -0.0393(5) 0.86595(12) 0.0640(10) Uani 1 1 d . . . H29A H 1.3551 -0.0391 0.8896 0.077 Uiso 1 1 calc R . . C30 C 1.3059(6) -0.1251(4) 0.82982(11) 0.0535(8) Uani 1 1 d . . . H30A H 1.4353 -0.1839 0.8287 0.064 Uiso 1 1 calc R . . C31 C 1.1619(5) -0.1261(4) 0.79429(10) 0.0421(7) Uani 1 1 d . . . C32 C 1.1942(5) -0.2305(4) 0.75662(10) 0.0413(7) Uani 1 1 d . . . C33 C 1.3721(5) -0.3308(4) 0.74927(11) 0.0480(8) Uani 1 1 d . . . H33A H 1.4894 -0.3328 0.7693 0.058 Uiso 1 1 calc R . . C34 C 1.3738(5) -0.4266(4) 0.71243(11) 0.0531(9) Uani 1 1 d . . . H34A H 1.4931 -0.4929 0.7071 0.064 Uiso 1 1 calc R . . C35 C 1.1962(6) -0.4240(4) 0.68316(12) 0.0538(8) Uani 1 1 d . . . H35A H 1.1923 -0.4903 0.6583 0.065 Uiso 1 1 calc R . . C36 C 1.0260(5) -0.3210(4) 0.69177(11) 0.0491(8) Uani 1 1 d . . . H36A H 0.9075 -0.3176 0.6721 0.059 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 Pd 0.03339(12) 0.03842(15) 0.04628(17) 0.00429(10) -0.00477(9) 0.00309(9) O1 0.0417(11) 0.0587(14) 0.0516(14) -0.0008(11) -0.0092(10) 0.0138(10) O2 0.0619(14) 0.0882(19) 0.0518(15) -0.0092(13) -0.0188(12) 0.0221(13) N1 0.0329(11) 0.0340(13) 0.0508(16) 0.0030(11) 0.0001(11) 0.0012(10) N2 0.0393(12) 0.0387(14) 0.0465(16) 0.0076(12) -0.0052(11) 0.0016(10) C1 0.0374(14) 0.0418(17) 0.051(2) 0.0056(14) -0.0007(14) 0.0056(12) C2 0.0368(14) 0.0447(18) 0.0469(19) 0.0089(15) -0.0041(13) 0.0019(13) C3 0.0459(16) 0.052(2) 0.055(2) 0.0052(16) -0.0038(15) 0.0122(15) C4 0.0455(17) 0.065(2) 0.054(2) 0.0064(17) -0.0121(16) 0.0151(16) C5 0.0492(17) 0.059(2) 0.045(2) 0.0064(16) -0.0057(15) 0.0049(15) C6 0.0468(16) 0.053(2) 0.0447(19) 0.0022(15) -0.0011(14) 0.0090(14) C7 0.0366(14) 0.0443(18) 0.0466(19) 0.0089(14) -0.0019(13) 0.0027(13) C8 0.0537(19) 0.081(3) 0.058(2) -0.001(2) -0.0119(18) 0.0116(18) C9 0.069(2) 0.084(3) 0.052(2) -0.006(2) -0.0131(19) 0.015(2) C10 0.065(2) 0.090(3) 0.063(3) -0.008(2) -0.017(2) 0.011(2) C11 0.079(3) 0.090(3) 0.065(3) -0.010(2) -0.018(2) 0.018(2) C12 0.075(3) 0.096(3) 0.079(3) -0.011(3) -0.020(2) 0.015(2) C13 0.117(4) 0.127(5) 0.097(4) -0.038(3) -0.042(3) 0.050(4) C14 0.0361(14) 0.0365(17) 0.0438(18) 0.0074(13) -0.0031(13) 0.0049(12) C15 0.0399(15) 0.0451(18) 0.0484(19) 0.0058(15) 0.0020(14) 0.0000(13) C16 0.0466(16) 0.0401(18) 0.055(2) 0.0079(15) -0.0041(15) -0.0072(13) C17 0.0490(16) 0.0392(17) 0.0491(19) 0.0023(14) -0.0069(15) 0.0062(13) C18 0.0421(15) 0.053(2) 0.048(2) 0.0055(16) 0.0044(14) 0.0107(14) C19 0.0370(14) 0.0429(18) 0.054(2) 0.0033(15) 0.0006(14) -0.0006(13) C20 0.064(2) 0.049(2) 0.055(2) -0.0053(17) -0.0070(17) 0.0102(16) C21 0.070(2) 0.058(2) 0.059(2) -0.0048(18) -0.0098(19) 0.0092(18) C22 0.081(3) 0.074(3) 0.053(2) -0.003(2) -0.005(2) 0.002(2) C23 0.095(3) 0.104(4) 0.065(3) -0.011(3) -0.014(2) 0.002(3) C24 0.134(5) 0.136(5) 0.083(4) -0.020(3) -0.024(3) -0.009(4) C25 0.146(6) 0.213(8) 0.111(5) -0.033(5) -0.056(5) -0.014(6) C26 0.0427(15) 0.0376(17) 0.049(2) 0.0108(14) -0.0047(14) -0.0041(13) C27 0.0551(18) 0.049(2) 0.045(2) 0.0094(15) -0.0015(15) 0.0035(15) C28 0.074(2) 0.056(2) 0.047(2) 0.0040(17) -0.0021(18) 0.0015(18) C29 0.073(2) 0.060(2) 0.058(2) 0.0101(19) -0.0238(19) 0.0014(19) C30 0.0539(18) 0.048(2) 0.058(2) 0.0077(17) -0.0136(17) 0.0062(15) C31 0.0426(15) 0.0329(16) 0.051(2) 0.0115(14) -0.0055(14) -0.0033(12) C32 0.0374(14) 0.0345(16) 0.053(2) 0.0132(14) -0.0024(14) -0.0014(12) C33 0.0411(15) 0.0445(19) 0.059(2) 0.0151(16) -0.0053(15) 0.0047(13) C34 0.0471(17) 0.046(2) 0.069(2) 0.0126(18) 0.0050(17) 0.0134(14) C35 0.0576(19) 0.0445(19) 0.060(2) 0.0001(16) 0.0053(17) 0.0091(15) C36 0.0420(16) 0.051(2) 0.054(2) 0.0047(17) -0.0055(15) 0.0035(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd C26 1.996(3) . ? Pd N2 2.026(3) . ? Pd N1 2.045(2) . ? Pd O1 2.063(2) . ? O1 C7 1.298(3) . ? O2 C5 1.362(4) . ? O2 C8 1.427(4) . ? N1 C1 1.311(4) . ? N1 C14 1.430(4) . ? N2 C36 1.330(4) . ? N2 C32 1.356(4) . ? C1 C2 1.420(4) . ? C2 C3 1.409(4) . ? C2 C7 1.428(4) . ? C3 C4 1.366(5) . ? C4 C5 1.395(5) . ? C5 C6 1.380(4) . ? C6 C7 1.401(4) . ? C8 C9 1.498(5) . ? C9 C10 1.510(5) . ? C10 C11 1.490(5) . ? C11 C12 1.500(6) . ? C12 C13 1.447(6) . ? C14 C19 1.378(4) . ? C14 C15 1.394(4) . ? C15 C16 1.369(4) . ? C16 C17 1.386(5) . ? C17 C18 1.392(4) . ? C17 C20 1.508(4) . ? C18 C19 1.373(4) . ? C20 C21 1.514(5) . ? C21 C22 1.505(5) . ? C22 C23 1.516(6) . ? C23 C24 1.487(6) . ? C24 C25 1.508(8) . ? C26 C27 1.401(5) . ? C26 C31 1.416(4) . ? C27 C28 1.381(5) . ? C28 C29 1.389(5) . ? C29 C30 1.357(5) . ? C30 C31 1.395(5) . ? C31 C32 1.453(4) . ? C32 C33 1.390(4) . ? C33 C34 1.370(5) . ? C34 C35 1.386(5) . ? C35 C36 1.375(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 C26 Pd N2 80.96(12) . . ? C26 Pd N1 100.80(11) . . ? N2 Pd N1 174.86(10) . . ? C26 Pd O1 168.56(11) . . ? N2 Pd O1 87.99(9) . . ? N1 Pd O1 90.47(9) . . ? C7 O1 Pd 127.9(2) . . ? C5 O2 C8 117.9(3) . . ? C1 N1 C14 114.9(2) . . ? C1 N1 Pd 122.1(2) . . ? C14 N1 Pd 123.05(18) . . ? C36 N2 C32 119.8(3) . . ? C36 N2 Pd 124.1(2) . . ? C32 N2 Pd 115.7(2) . . ? N1 C1 C2 129.7(3) . . ? C3 C2 C1 116.9(3) . . ? C3 C2 C7 118.3(3) . . ? C1 C2 C7 124.7(3) . . ? C4 C3 C2 122.7(3) . . ? C3 C4 C5 118.7(3) . . ? O2 C5 C6 115.3(3) . . ? O2 C5 C4 124.0(3) . . ? C6 C5 C4 120.6(3) . . ? C5 C6 C7 121.6(3) . . ? O1 C7 C6 119.2(3) . . ? O1 C7 C2 122.8(3) . . ? C6 C7 C2 118.0(3) . . ? O2 C8 C9 108.5(3) . . ? C8 C9 C10 111.4(3) . . ? C11 C10 C9 115.0(4) . . ? C10 C11 C12 114.3(4) . . ? C13 C12 C11 117.7(4) . . ? C19 C14 C15 119.2(3) . . ? C19 C14 N1 121.7(3) . . ? C15 C14 N1 119.1(3) . . ? C16 C15 C14 120.1(3) . . ? C15 C16 C17 121.6(3) . . ? C16 C17 C18 117.4(3) . . ? C16 C17 C20 121.0(3) . . ? C18 C17 C20 121.6(3) . . ? C19 C18 C17 121.7(3) . . ? C18 C19 C14 120.0(3) . . ? C17 C20 C21 113.8(3) . . ? C22 C21 C20 113.3(3) . . ? C21 C22 C23 114.2(4) . . ? C24 C23 C22 115.0(5) . . ? C23 C24 C25 114.3(6) . . ? C27 C26 C31 116.1(3) . . ? C27 C26 Pd 131.1(2) . . ? C31 C26 Pd 112.7(2) . . ? C28 C27 C26 121.2(3) . . ? C27 C28 C29 121.4(4) . . ? C30 C29 C28 118.8(3) . . ? C29 C30 C31 120.8(3) . . ? C30 C31 C26 121.5(3) . . ? C30 C31 C32 122.0(3) . . ? C26 C31 C32 116.3(3) . . ? N2 C32 C33 120.2(3) . . ? N2 C32 C31 113.0(3) . . ? C33 C32 C31 126.9(3) . . ? C34 C33 C32 119.7(3) . . ? C33 C34 C35 119.5(3) . . ? C36 C35 C34 118.4(3) . . ? N2 C36 C35 122.4(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 C26 Pd O1 C7 155.2(5) . . . . ? N2 Pd O1 C7 170.0(3) . . . . ? N1 Pd O1 C7 -14.9(3) . . . . ? C26 Pd N1 C1 -163.4(2) . . . . ? N2 Pd N1 C1 87.1(10) . . . . ? O1 Pd N1 C1 14.6(2) . . . . ? C26 Pd N1 C14 15.1(2) . . . . ? N2 Pd N1 C14 -94.4(11) . . . . ? O1 Pd N1 C14 -166.9(2) . . . . ? C26 Pd N2 C36 176.9(3) . . . . ? N1 Pd N2 C36 -72.8(11) . . . . ? O1 Pd N2 C36 -0.2(3) . . . . ? C26 Pd N2 C32 -10.8(2) . . . . ? N1 Pd N2 C32 99.5(10) . . . . ? O1 Pd N2 C32 172.2(2) . . . . ? C14 N1 C1 C2 172.7(3) . . . . ? Pd N1 C1 C2 -8.8(5) . . . . ? N1 C1 C2 C3 179.4(3) . . . . ? N1 C1 C2 C7 -4.6(5) . . . . ? C1 C2 C3 C4 176.1(3) . . . . ? C7 C2 C3 C4 -0.1(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C8 O2 C5 C6 177.3(3) . . . . ? C8 O2 C5 C4 -2.0(5) . . . . ? C3 C4 C5 O2 178.1(3) . . . . ? C3 C4 C5 C6 -1.1(5) . . . . ? O2 C5 C6 C7 -177.0(3) . . . . ? C4 C5 C6 C7 2.3(5) . . . . ? Pd O1 C7 C6 -172.3(2) . . . . ? Pd O1 C7 C2 7.4(4) . . . . ? C5 C6 C7 O1 177.5(3) . . . . ? C5 C6 C7 C2 -2.3(5) . . . . ? C3 C2 C7 O1 -178.5(3) . . . . ? C1 C2 C7 O1 5.5(5) . . . . ? C3 C2 C7 C6 1.2(5) . . . . ? C1 C2 C7 C6 -174.8(3) . . . . ? C5 O2 C8 C9 -175.4(3) . . . . ? O2 C8 C9 C10 -175.8(4) . . . . ? C8 C9 C10 C11 179.6(4) . . . . ? C9 C10 C11 C12 -176.7(4) . . . . ? C10 C11 C12 C13 -177.7(5) . . . . ? C1 N1 C14 C19 59.5(4) . . . . ? Pd N1 C14 C19 -119.0(3) . . . . ? C1 N1 C14 C15 -120.7(3) . . . . ? Pd N1 C14 C15 60.8(3) . . . . ? C19 C14 C15 C16 1.7(5) . . . . ? N1 C14 C15 C16 -178.1(3) . . . . ? C14 C15 C16 C17 0.7(5) . . . . ? C15 C16 C17 C18 -1.7(5) . . . . ? C15 C16 C17 C20 176.6(3) . . . . ? C16 C17 C18 C19 0.5(5) . . . . ? C20 C17 C18 C19 -177.8(3) . . . . ? C17 C18 C19 C14 1.8(5) . . . . ? C15 C14 C19 C18 -2.9(5) . . . . ? N1 C14 C19 C18 176.9(3) . . . . ? C16 C17 C20 C21 -62.9(5) . . . . ? C18 C17 C20 C21 115.3(4) . . . . ? C17 C20 C21 C22 -172.7(3) . . . . ? C20 C21 C22 C23 -175.1(4) . . . . ? C21 C22 C23 C24 -176.4(5) . . . . ? C22 C23 C24 C25 178.8(5) . . . . ? N2 Pd C26 C27 -168.8(3) . . . . ? N1 Pd C26 C27 16.1(3) . . . . ? O1 Pd C26 C27 -153.8(4) . . . . ? N2 Pd C26 C31 8.7(2) . . . . ? N1 Pd C26 C31 -166.4(2) . . . . ? O1 Pd C26 C31 23.7(6) . . . . ? C31 C26 C27 C28 3.3(5) . . . . ? Pd C26 C27 C28 -179.3(3) . . . . ? C26 C27 C28 C29 -0.7(5) . . . . ? C27 C28 C29 C30 -1.0(6) . . . . ? C28 C29 C30 C31 -0.2(6) . . . . ? C29 C30 C31 C26 3.1(5) . . . . ? C29 C30 C31 C32 -173.2(3) . . . . ? C27 C26 C31 C30 -4.6(4) . . . . ? Pd C26 C31 C30 177.6(2) . . . . ? C27 C26 C31 C32 171.9(3) . . . . ? Pd C26 C31 C32 -6.0(3) . . . . ? C36 N2 C32 C33 1.7(4) . . . . ? Pd N2 C32 C33 -171.0(2) . . . . ? C36 N2 C32 C31 -177.0(3) . . . . ? Pd N2 C32 C31 10.3(3) . . . . ? C30 C31 C32 N2 173.7(3) . . . . ? C26 C31 C32 N2 -2.8(4) . . . . ? C30 C31 C32 C33 -5.0(5) . . . . ? C26 C31 C32 C33 178.6(3) . . . . ? N2 C32 C33 C34 -0.9(5) . . . . ? C31 C32 C33 C34 177.7(3) . . . . ? C32 C33 C34 C35 -0.9(5) . . . . ? C33 C34 C35 C36 1.7(5) . . . . ? C32 N2 C36 C35 -0.8(5) . . . . ? Pd N2 C36 C35 171.2(3) . . . . ? C34 C35 C36 N2 -0.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.482 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.166 #===END data_(PYPTON) _database_code_depnum_ccdc_archive 'CCDC 776863' #TrackingRef 'acrispini.CIF' _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C36 H42 N2 O2 Pt' _chemical_formula_sum 'C36 H42 N2 O2 Pt' _chemical_formula_weight 729.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 6.0027(4) _cell_length_b 8.1666(5) _cell_length_c 32.286(2) _cell_angle_alpha 94.534(2) _cell_angle_beta 93.089(2) _cell_angle_gamma 92.243(2) _cell_volume 1573.98(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 8285 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 25.68 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 4.491 _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.6589 _exptl_absorpt_correction_T_max 0.7745 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25252 _diffrn_reflns_av_R_equivalents 0.0234 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5353 _reflns_number_gt 5261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0067P)^2^+3.9020P] 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 5353 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0697 _refine_ls_wR_factor_gt 0.0695 _refine_ls_goodness_of_fit_ref 1.440 _refine_ls_restrained_S_all 1.440 _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 Pt Pt -0.29789(3) 0.04793(3) -0.238817(7) 0.03905(7) Uani 1 1 d . . . O1 O -0.1582(6) 0.1099(5) -0.17934(12) 0.0516(10) Uani 1 1 d . . . O2 O 0.3715(7) 0.1781(6) -0.06848(13) 0.0697(13) Uani 1 1 d . . . N1 N -0.0846(7) -0.1360(5) -0.24622(14) 0.0413(10) Uani 1 1 d . . . N2 N -0.5198(7) 0.2229(5) -0.22787(14) 0.0403(10) Uani 1 1 d . . . C1 C 0.0917(9) -0.1516(7) -0.22133(18) 0.0467(13) Uani 1 1 d . . . H1 H 0.1858 -0.2342 -0.2297 0.056 Uiso 1 1 calc R . . C2 C 0.1583(8) -0.0594(6) -0.18325(17) 0.0426(12) Uani 1 1 d . . . C3 C 0.3609(9) -0.0986(7) -0.16323(19) 0.0506(14) Uani 1 1 d . . . H3A H 0.4466 -0.1773 -0.1764 0.061 Uiso 1 1 calc R . . C4 C 0.4374(10) -0.0260(8) -0.12527(19) 0.0565(15) Uani 1 1 d . . . H4A H 0.5715 -0.0553 -0.1127 0.068 Uiso 1 1 calc R . . C5 C 0.3091(10) 0.0933(7) -0.10575(18) 0.0527(14) Uani 1 1 d . . . C6 C 0.1104(9) 0.1337(7) -0.12394(17) 0.0494(14) Uani 1 1 d . . . H6A H 0.0260 0.2110 -0.1099 0.059 Uiso 1 1 calc R . . C7 C 0.0290(9) 0.0622(7) -0.16318(17) 0.0443(13) Uani 1 1 d . . . C8 C 0.5830(11) 0.1478(9) -0.0492(2) 0.0666(18) Uani 1 1 d . . . H8B H 0.6997 0.1651 -0.0682 0.080 Uiso 1 1 calc R . . H8A H 0.5852 0.0348 -0.0419 0.080 Uiso 1 1 calc R . . C9 C 0.6231(12) 0.2625(9) -0.0108(2) 0.0711(19) Uani 1 1 d . . . H9B H 0.4990 0.2508 0.0070 0.085 Uiso 1 1 calc R . . H9A H 0.6301 0.3749 -0.0185 0.085 Uiso 1 1 calc R . . C10 C 0.8381(12) 0.2289(10) 0.0133(2) 0.079(2) Uani 1 1 d . . . H10B H 0.8304 0.1156 0.0204 0.094 Uiso 1 1 calc R . . H10A H 0.9608 0.2404 -0.0048 0.094 Uiso 1 1 calc R . . C11 C 0.8903(13) 0.3373(10) 0.0524(2) 0.082(2) Uani 1 1 d . . . H11B H 0.7654 0.3296 0.0701 0.098 Uiso 1 1 calc R . . H11A H 0.9055 0.4503 0.0453 0.098 Uiso 1 1 calc R . . C12 C 1.0985(13) 0.2967(11) 0.0765(2) 0.090(3) Uani 1 1 d . . . H12B H 1.0810 0.1839 0.0836 0.107 Uiso 1 1 calc R . . H12A H 1.2214 0.3017 0.0583 0.107 Uiso 1 1 calc R . . C13 C 1.1620(17) 0.3985(13) 0.1144(3) 0.125(4) Uani 1 1 d . . . H13C H 1.2970 0.3602 0.1269 0.187 Uiso 1 1 calc R . . H13B H 1.0450 0.3922 0.1334 0.187 Uiso 1 1 calc R . . H13A H 1.1861 0.5104 0.1080 0.187 Uiso 1 1 calc R . . C14 C -0.1187(8) -0.2607(6) -0.27956(16) 0.0377(11) Uani 1 1 d . . . C19 C -0.3123(9) -0.3637(7) -0.28204(17) 0.0460(13) Uani 1 1 d . . . H19A H -0.4155 -0.3504 -0.2617 0.055 Uiso 1 1 calc R . . C18 C -0.3517(9) -0.4846(7) -0.31435(18) 0.0483(14) Uani 1 1 d . . . H18A H -0.4819 -0.5510 -0.3157 0.058 Uiso 1 1 calc R . . C17 C -0.1991(10) -0.5080(7) -0.34478(18) 0.0481(13) Uani 1 1 d . . . C16 C -0.0041(9) -0.4119(7) -0.34092(18) 0.0480(13) Uani 1 1 d . . . H16A H 0.1025 -0.4287 -0.3605 0.058 Uiso 1 1 calc R . . C15 C 0.0367(9) -0.2909(6) -0.30852(17) 0.0437(13) Uani 1 1 d . . . H15A H 0.1711 -0.2294 -0.3064 0.052 Uiso 1 1 calc R . . C20 C -0.2484(11) -0.6346(7) -0.38135(19) 0.0581(16) Uani 1 1 d . . . H20A H -0.1183 -0.6408 -0.3979 0.070 Uiso 1 1 calc R . . H20B H -0.2745 -0.7414 -0.3709 0.070 Uiso 1 1 calc R . . C21 C -0.4484(11) -0.5975(8) -0.4091(2) 0.0639(17) Uani 1 1 d . . . H21A H -0.4310 -0.4854 -0.4168 0.077 Uiso 1 1 calc R . . H21B H -0.5817 -0.6050 -0.3935 0.077 Uiso 1 1 calc R . . C22 C -0.4807(12) -0.7120(9) -0.4484(2) 0.0702(19) Uani 1 1 d . . . H22A H -0.3532 -0.6970 -0.4652 0.084 Uiso 1 1 calc R . . H22B H -0.4839 -0.8246 -0.4408 0.084 Uiso 1 1 calc R . . C23 C -0.6914(14) -0.6865(11) -0.4746(2) 0.089(2) Uani 1 1 d . . . H23A H -0.8191 -0.7079 -0.4583 0.107 Uiso 1 1 calc R . . H23B H -0.6924 -0.5721 -0.4807 0.107 Uiso 1 1 calc R . . C24 C -0.7187(18) -0.7911(13) -0.5145(3) 0.119(4) Uani 1 1 d . . . H24A H -0.7200 -0.9056 -0.5084 0.142 Uiso 1 1 calc R . . H24B H -0.5905 -0.7708 -0.5307 0.142 Uiso 1 1 calc R . . C25 C -0.927(2) -0.7628(17) -0.5404(3) 0.163(5) Uani 1 1 d . . . H25A H -0.9363 -0.8371 -0.5650 0.245 Uiso 1 1 calc R . . H25B H -0.9237 -0.6516 -0.5480 0.245 Uiso 1 1 calc R . . H25C H -1.0556 -0.7818 -0.5246 0.245 Uiso 1 1 calc R . . C26 C -0.4655(8) 0.0302(6) -0.29438(17) 0.0407(12) Uani 1 1 d . . . C27 C -0.4213(10) -0.0521(7) -0.33252(17) 0.0483(13) Uani 1 1 d . . . H27A H -0.2929 -0.1117 -0.3343 0.058 Uiso 1 1 calc R . . C28 C -0.5633(11) -0.0476(8) -0.36786(19) 0.0595(16) Uani 1 1 d . . . H28A H -0.5280 -0.1039 -0.3927 0.071 Uiso 1 1 calc R . . C29 C -0.7555(11) 0.0391(8) -0.3666(2) 0.0631(18) Uani 1 1 d . . . H29A H -0.8528 0.0385 -0.3900 0.076 Uiso 1 1 calc R . . C30 C -0.8012(10) 0.1263(7) -0.33021(19) 0.0535(15) Uani 1 1 d . . . H30A H -0.9292 0.1867 -0.3292 0.064 Uiso 1 1 calc R . . C31 C -0.6579(8) 0.1256(6) -0.29464(17) 0.0407(12) Uani 1 1 d . . . C32 C -0.6886(8) 0.2286(6) -0.25692(17) 0.0377(12) Uani 1 1 d . . . C33 C -0.8637(9) 0.3301(7) -0.24947(18) 0.0465(13) Uani 1 1 d . . . H33A H -0.9802 0.3336 -0.2695 0.056 Uiso 1 1 calc R . . C34 C -0.8661(9) 0.4257(7) -0.21263(19) 0.0500(14) Uani 1 1 d . . . H34A H -0.9852 0.4922 -0.2073 0.060 Uiso 1 1 calc R . . C35 C -0.6904(10) 0.4219(7) -0.1837(2) 0.0523(15) Uani 1 1 d . . . H35A H -0.6852 0.4898 -0.1591 0.063 Uiso 1 1 calc R . . C36 C -0.5186(9) 0.3139(8) -0.19183(18) 0.0559(16) Uani 1 1 d . . . H36A H -0.4029 0.3059 -0.1718 0.067 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 Pt 0.03361(11) 0.03650(11) 0.04660(13) 0.00436(8) -0.00354(8) 0.00197(8) O1 0.042(2) 0.060(2) 0.052(2) -0.0023(19) -0.0097(18) 0.0127(18) O2 0.062(3) 0.091(3) 0.052(3) -0.010(2) -0.018(2) 0.021(2) N1 0.035(2) 0.040(2) 0.049(3) 0.006(2) 0.001(2) -0.0023(19) N2 0.035(2) 0.032(2) 0.053(3) 0.006(2) -0.005(2) 0.0032(18) C1 0.043(3) 0.042(3) 0.054(3) 0.005(3) -0.002(3) 0.003(2) C2 0.035(3) 0.043(3) 0.049(3) 0.009(2) -0.004(2) 0.003(2) C3 0.047(3) 0.048(3) 0.058(4) 0.008(3) -0.002(3) 0.009(3) C4 0.048(3) 0.069(4) 0.052(4) 0.005(3) -0.012(3) 0.013(3) C5 0.052(4) 0.058(4) 0.048(3) 0.007(3) -0.006(3) 0.004(3) C6 0.047(3) 0.056(4) 0.045(3) 0.003(3) 0.000(3) 0.007(3) C7 0.040(3) 0.045(3) 0.048(3) 0.009(3) -0.002(2) 0.002(2) C8 0.057(4) 0.083(5) 0.057(4) -0.001(3) -0.012(3) 0.010(3) C9 0.072(5) 0.084(5) 0.055(4) -0.003(4) -0.013(3) 0.013(4) C10 0.067(5) 0.095(6) 0.070(5) -0.009(4) -0.017(4) 0.014(4) C11 0.082(5) 0.088(5) 0.071(5) -0.009(4) -0.021(4) 0.015(4) C12 0.075(5) 0.109(7) 0.080(5) -0.012(5) -0.021(4) 0.020(5) C13 0.122(8) 0.136(9) 0.105(7) -0.044(6) -0.053(6) 0.049(7) C14 0.032(3) 0.040(3) 0.042(3) 0.008(2) -0.002(2) 0.000(2) C19 0.042(3) 0.048(3) 0.048(3) 0.005(3) 0.005(2) 0.001(2) C18 0.045(3) 0.041(3) 0.057(4) 0.008(3) -0.004(3) -0.007(2) C17 0.054(3) 0.038(3) 0.052(3) 0.004(2) -0.005(3) 0.008(3) C16 0.038(3) 0.047(3) 0.059(4) 0.003(3) 0.005(3) 0.000(2) C15 0.037(3) 0.042(3) 0.053(3) -0.002(3) 0.006(2) 0.008(2) C20 0.062(4) 0.049(3) 0.060(4) -0.007(3) -0.007(3) 0.005(3) C21 0.072(4) 0.058(4) 0.059(4) -0.005(3) -0.012(3) 0.008(3) C22 0.084(5) 0.068(4) 0.056(4) -0.005(3) -0.006(4) 0.000(4) C23 0.094(6) 0.106(6) 0.063(5) -0.011(4) -0.013(4) 0.002(5) C24 0.132(9) 0.133(9) 0.080(6) -0.027(6) -0.029(6) -0.002(7) C25 0.143(10) 0.223(15) 0.108(8) -0.026(9) -0.055(8) -0.015(10) C26 0.038(3) 0.034(3) 0.051(3) 0.013(2) -0.003(2) -0.003(2) C27 0.050(3) 0.046(3) 0.050(3) 0.010(3) 0.001(3) 0.006(3) C28 0.079(5) 0.053(4) 0.046(3) 0.008(3) -0.004(3) 0.001(3) C29 0.073(4) 0.059(4) 0.056(4) 0.015(3) -0.024(3) 0.000(3) C30 0.052(4) 0.046(3) 0.061(4) 0.010(3) -0.016(3) 0.006(3) C31 0.039(3) 0.031(3) 0.052(3) 0.012(2) -0.004(2) -0.002(2) C32 0.032(3) 0.027(2) 0.056(3) 0.014(2) 0.000(2) 0.001(2) C33 0.039(3) 0.043(3) 0.059(4) 0.016(3) -0.004(3) 0.004(2) C34 0.044(3) 0.039(3) 0.069(4) 0.012(3) 0.007(3) 0.012(2) C35 0.051(3) 0.040(3) 0.066(4) -0.002(3) 0.003(3) 0.010(3) C36 0.032(3) 0.090(5) 0.044(3) 0.006(3) -0.001(2) -0.011(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 Pt C26 2.001(5) . ? Pt N2 2.015(4) . ? Pt N1 2.020(4) . ? Pt O1 2.071(4) . ? O1 C7 1.300(6) . ? O2 C5 1.367(7) . ? O2 C8 1.423(7) . ? N1 C1 1.310(7) . ? N1 C14 1.423(6) . ? N2 C36 1.330(7) . ? N2 C32 1.348(6) . ? C1 C2 1.420(8) . ? C2 C3 1.406(7) . ? C2 C7 1.422(7) . ? C3 C4 1.367(8) . ? C4 C5 1.397(8) . ? C5 C6 1.365(8) . ? C6 C7 1.407(8) . ? C8 C9 1.497(9) . ? C9 C10 1.516(9) . ? C10 C11 1.494(9) . ? C11 C12 1.499(9) . ? C12 C13 1.448(10) . ? C14 C15 1.371(7) . ? C14 C19 1.403(7) . ? C19 C18 1.383(8) . ? C18 C17 1.386(8) . ? C17 C16 1.378(8) . ? C17 C20 1.515(8) . ? C16 C15 1.386(7) . ? C20 C21 1.514(8) . ? C21 C22 1.514(8) . ? C22 C23 1.513(10) . ? C23 C24 1.486(10) . ? C24 C25 1.504(13) . ? C26 C27 1.399(8) . ? C26 C31 1.418(7) . ? C27 C28 1.390(8) . ? C28 C29 1.379(9) . ? C29 C30 1.370(9) . ? C30 C31 1.398(7) . ? C31 C32 1.449(7) . ? C32 C33 1.384(7) . ? C33 C34 1.371(8) . ? C34 C35 1.374(8) . ? C35 C36 1.406(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 C26 Pt N2 80.78(19) . . ? C26 Pt N1 101.4(2) . . ? N2 Pt N1 175.71(18) . . ? C26 Pt O1 168.37(18) . . ? N2 Pt O1 87.87(16) . . ? N1 Pt O1 90.09(16) . . ? C7 O1 Pt 127.4(4) . . ? C5 O2 C8 118.2(5) . . ? C1 N1 C14 115.0(4) . . ? C1 N1 Pt 123.8(4) . . ? C14 N1 Pt 121.2(3) . . ? C36 N2 C32 120.9(5) . . ? C36 N2 Pt 122.3(4) . . ? C32 N2 Pt 116.2(3) . . ? N1 C1 C2 128.7(5) . . ? C3 C2 C1 117.0(5) . . ? C3 C2 C7 118.4(5) . . ? C1 C2 C7 124.5(5) . . ? C4 C3 C2 122.9(6) . . ? C3 C4 C5 118.4(5) . . ? C6 C5 O2 115.7(5) . . ? C6 C5 C4 120.6(5) . . ? O2 C5 C4 123.8(5) . . ? C5 C6 C7 122.2(5) . . ? O1 C7 C6 119.1(5) . . ? O1 C7 C2 123.3(5) . . ? C6 C7 C2 117.6(5) . . ? O2 C8 C9 108.8(5) . . ? C8 C9 C10 111.9(6) . . ? C11 C10 C9 115.4(6) . . ? C10 C11 C12 114.3(6) . . ? C13 C12 C11 117.5(7) . . ? C15 C14 C19 117.9(5) . . ? C15 C14 N1 122.5(5) . . ? C19 C14 N1 119.4(5) . . ? C18 C19 C14 120.9(5) . . ? C19 C18 C17 120.6(5) . . ? C16 C17 C18 118.1(5) . . ? C16 C17 C20 121.4(6) . . ? C18 C17 C20 120.5(5) . . ? C17 C16 C15 121.5(5) . . ? C14 C15 C16 120.8(5) . . ? C21 C20 C17 113.7(5) . . ? C20 C21 C22 113.6(5) . . ? C23 C22 C21 114.2(6) . . ? C24 C23 C22 114.8(7) . . ? C23 C24 C25 114.2(9) . . ? C27 C26 C31 115.7(5) . . ? C27 C26 Pt 131.7(4) . . ? C31 C26 Pt 112.5(4) . . ? C28 C27 C26 122.1(6) . . ? C29 C28 C27 120.8(6) . . ? C30 C29 C28 119.0(6) . . ? C29 C30 C31 120.9(6) . . ? C30 C31 C26 121.4(5) . . ? C30 C31 C32 122.4(5) . . ? C26 C31 C32 116.1(5) . . ? N2 C32 C33 120.1(5) . . ? N2 C32 C31 113.1(4) . . ? C33 C32 C31 126.8(5) . . ? C34 C33 C32 120.2(5) . . ? C33 C34 C35 119.2(5) . . ? C34 C35 C36 118.9(6) . . ? N2 C36 C35 120.6(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 C26 Pt O1 C7 -156.9(8) . . . . ? N2 Pt O1 C7 -169.5(5) . . . . ? N1 Pt O1 C7 14.3(5) . . . . ? C26 Pt N1 C1 164.9(4) . . . . ? N2 Pt N1 C1 -75(2) . . . . ? O1 Pt N1 C1 -13.3(4) . . . . ? C26 Pt N1 C14 -15.6(4) . . . . ? N2 Pt N1 C14 105(2) . . . . ? O1 Pt N1 C14 166.2(4) . . . . ? C26 Pt N2 C36 -177.9(5) . . . . ? N1 Pt N2 C36 61(2) . . . . ? O1 Pt N2 C36 -0.5(4) . . . . ? C26 Pt N2 C32 10.6(4) . . . . ? N1 Pt N2 C32 -110(2) . . . . ? O1 Pt N2 C32 -172.0(4) . . . . ? C14 N1 C1 C2 -172.7(5) . . . . ? Pt N1 C1 C2 6.9(8) . . . . ? N1 C1 C2 C3 -177.9(5) . . . . ? N1 C1 C2 C7 5.7(9) . . . . ? C1 C2 C3 C4 -176.0(6) . . . . ? C7 C2 C3 C4 0.6(9) . . . . ? C2 C3 C4 C5 -0.6(9) . . . . ? C8 O2 C5 C6 -176.6(6) . . . . ? C8 O2 C5 C4 2.5(9) . . . . ? C3 C4 C5 C6 1.2(9) . . . . ? C3 C4 C5 O2 -177.8(6) . . . . ? O2 C5 C6 C7 177.1(5) . . . . ? C4 C5 C6 C7 -1.9(9) . . . . ? Pt O1 C7 C6 172.1(4) . . . . ? Pt O1 C7 C2 -7.7(8) . . . . ? C5 C6 C7 O1 -177.9(5) . . . . ? C5 C6 C7 C2 1.9(9) . . . . ? C3 C2 C7 O1 178.5(5) . . . . ? C1 C2 C7 O1 -5.1(9) . . . . ? C3 C2 C7 C6 -1.2(8) . . . . ? C1 C2 C7 C6 175.1(5) . . . . ? C5 O2 C8 C9 175.7(6) . . . . ? O2 C8 C9 C10 175.7(6) . . . . ? C8 C9 C10 C11 -179.6(7) . . . . ? C9 C10 C11 C12 177.5(8) . . . . ? C10 C11 C12 C13 179.0(9) . . . . ? C1 N1 C14 C15 -58.9(7) . . . . ? Pt N1 C14 C15 121.5(5) . . . . ? C1 N1 C14 C19 117.5(5) . . . . ? Pt N1 C14 C19 -62.1(6) . . . . ? C15 C14 C19 C18 -4.3(8) . . . . ? N1 C14 C19 C18 179.2(5) . . . . ? C14 C19 C18 C17 0.8(8) . . . . ? C19 C18 C17 C16 2.5(8) . . . . ? C19 C18 C17 C20 -176.8(5) . . . . ? C18 C17 C16 C15 -2.3(8) . . . . ? C20 C17 C16 C15 177.0(5) . . . . ? C19 C14 C15 C16 4.5(8) . . . . ? N1 C14 C15 C16 -179.0(5) . . . . ? C17 C16 C15 C14 -1.3(9) . . . . ? C16 C17 C20 C21 -115.5(7) . . . . ? C18 C17 C20 C21 63.8(8) . . . . ? C17 C20 C21 C22 172.9(6) . . . . ? C20 C21 C22 C23 174.7(7) . . . . ? C21 C22 C23 C24 176.5(8) . . . . ? C22 C23 C24 C25 -179.3(9) . . . . ? N2 Pt C26 C27 168.6(5) . . . . ? N1 Pt C26 C27 -15.2(5) . . . . ? O1 Pt C26 C27 155.9(8) . . . . ? N2 Pt C26 C31 -8.2(4) . . . . ? N1 Pt C26 C31 168.1(3) . . . . ? O1 Pt C26 C31 -20.9(12) . . . . ? C31 C26 C27 C28 -3.3(8) . . . . ? Pt C26 C27 C28 -180.0(4) . . . . ? C26 C27 C28 C29 -0.1(9) . . . . ? C27 C28 C29 C30 2.4(10) . . . . ? C28 C29 C30 C31 -1.1(9) . . . . ? C29 C30 C31 C26 -2.5(9) . . . . ? C29 C30 C31 C32 173.8(5) . . . . ? C27 C26 C31 C30 4.5(8) . . . . ? Pt C26 C31 C30 -178.2(4) . . . . ? C27 C26 C31 C32 -172.0(4) . . . . ? Pt C26 C31 C32 5.3(6) . . . . ? C36 N2 C32 C33 0.0(7) . . . . ? Pt N2 C32 C33 171.6(4) . . . . ? C36 N2 C32 C31 178.1(5) . . . . ? Pt N2 C32 C31 -10.3(5) . . . . ? C30 C31 C32 N2 -173.3(5) . . . . ? C26 C31 C32 N2 3.2(6) . . . . ? C30 C31 C32 C33 4.6(8) . . . . ? C26 C31 C32 C33 -179.0(5) . . . . ? N2 C32 C33 C34 0.2(8) . . . . ? C31 C32 C33 C34 -177.5(5) . . . . ? C32 C33 C34 C35 1.4(8) . . . . ? C33 C34 C35 C36 -3.2(9) . . . . ? C32 N2 C36 C35 -1.9(8) . . . . ? Pt N2 C36 C35 -173.0(4) . . . . ? C34 C35 C36 N2 3.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.803 _refine_diff_density_min -2.837 _refine_diff_density_rms 0.084 #===END