data_global _publ_requested_journal Inorg.Chem. _publ_contact_author_name ;Barbara Ventura; Raymond Ziessel ; _publ_contact_author_address ;Instituto per la Sintesi Organica e la Fotoreattivit\`a Consiglio Nazionale delle Ricerche (ISOF-CNR) Via P. Gobetti 101 40129 Bologna Italy Laboratoire de Chimie Universit\'e Louis Pasteur, d'Electronique et de Photonique Moleculaires ECPM, 1 rue Blaise Pascal Strasbourg F-67008 FRANCE ; _publ_contact_author_email 'bventura@isof.cnr.it; ziessel@chimie.u-strasbg.fr' _publ_contact_author_phone '33 3 90242689' _publ_contact_author_fax '33 3 90242635' loop_ _publ_author_name _publ_author_address 'Ventura, Barbara' ;Instituto per la Sintesi Organica e la Fotoreattivit\`a Consiglio Nazionale delle Ricerche (ISOF-CNR) Via P. Gobetti 101 40129 Bologna Italy ; 'Barbieri, Andrea' ;Instituto per la Sintesi Organica e la Fotoreattivit\`a Consiglio Nazionale delle Ricerche (ISOF-CNR) Via P. Gobetti 101 40129 Bologna Italy ; 'Barigelletti, Francesco' ;Instituto per la Sintesi Organica e la Fotoreattivit\`a Consiglio Nazionale delle Ricerche (ISOF-CNR) Via P. Gobetti 101 40129 Bologna Italy ; 'Seneclauze, Julie Batcha' ;Laboratoire de Chimie Mol\'eculaire, Ecole de Chimie, Polym\`eres, Mat\'eriaux (ECPM), Universite Louis Pasteur (ULP), 25 rue Becquerel 67087 Strasbourg Cedex 02 France ; 'RETAILLEAU, Pascal' ;ICSN-CNRS 1 avenue de la Terrasse 91198 Gif sur Yvette France ; 'ZIESSEL, Raymond' ;Laboratoire de Chimie Mol\'eculaire, Ecole de Chimie, Polym\`eres, Mat\'eriaux (ECPM), Universite Louis Pasteur (ULP), 25 rue Becquerel 67087 Strasbourg Cedex 02 France ; _audit_creation_date 27-02-08 _publ_contact_letter ; ; _publ_requested_category FM _publ_section_title ; Trichromophoric Systems Comprising Planar Pt-bipyridine-acetylide and Octahedral Ru- and Os- bipyridine centres. Syntheses, Structures, Electrochemical Behavior, Spectroscopic Properties and Bipartition of Energy Transfer ; _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; A.L. Spek, (2005) PLATON 2005, Utrecht University, The Netherland. KappaCCD Operation Manual (1997), Nonius B.V., Delft, The Nederlands. Otwinowski, Z. & Minor, W. (1997), Methods in Enzymology, 276, 307-326. Sheldrick, G.M. (1997). SHELXL97. Program for the refinement of crystal structures. University of Gottingen. Germany. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; data_jbs139sqz _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H38 N6 Pt, C H2 Cl2, C6 H12, C H4 O' _chemical_formula_sum 'C50 H56 Cl2 N6 O Pt' _chemical_formula_weight 1023 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.383(1) _cell_length_b 13.710(1) _cell_length_c 14.576(2) _cell_angle_alpha 80.24(3) _cell_angle_beta 86.36(3) _cell_angle_gamma 61.93(4) _cell_volume 2325.3(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5685 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 24.108 _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1036 _exptl_absorpt_coefficient_mu 3.18 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.442 _exptl_absorpt_correction_T_max 0.566 _exptl_absorpt_process_details 'Scalepack(Otwinowski & Minor, 1997)' _exptl_special_details ; 16783 reflections were collected using the program Collect ("Collect" Data collection software, Nonius B.V., 1998). The conditions were as follows: crystal to detector distance = 31.0 mm. Scan angle = 2.0 deg; 151 scans of 30 sec per frame. Data collection was divided into 4 sets (Phi + omega scans) with the following starting angles and number of frames : Phi scan1 len= 183.0;theta= 4.171 phi= -1.5 omega= 160.000 kappa= 0.000 Omega scan1 len= 43.4;theta= -3.885 phi=-90.359 omega=-152.104 kappa=-165.85 Omega scan2 len= 97.5;theta= -1.823 phi=170.437 omega=-151.916 kappa=-166.273 Omega scan3 len= 97.5;theta= -1.823 phi= 36.596 omega=-161.291 kappa=-144.710 Overall R-merge linear = 0.068. Friedel opposites unmerged. Crystal absorption: use of spherical harmonics (Katayama,C.(1986)Acta Cryst.A42:19-23; Blessing,R.H.(1995) Acta Cryst.A51,33) expansion of the absorption surface as implemented in Scalepack. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa-CCD diffractometer' _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 16783 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0724 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 24.45 _reflns_number_total 7473 _reflns_number_gt 5647 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) COLLECT (Hooft, 1998)' _computing_data_reduction 'HKL package (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1980-2004)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections except two truncated by the beamstop. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The PLATON SQUEEZE procedure was used to treat regions of diffuse solvent which could not be sensibly modelled in terms of atomic sites. Their contribution to the diffraction pattern was removed and modified F^2^ written to a new HKL file. The number of electrons thus located, 133 per unit cell, is included in the formula, formula weight, calculated density,? and F(000). This residual electron density was assigned to one molecule of cyclohexane, and one molecule of methanol per asymmetric unit. ; _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^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7471 _refine_ls_number_parameters 497 _refine_ls_number_restraints 114 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1119 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.02653(2) 0.009930(19) 0.188756(18) 0.05393(12) Uani 1 1 d . . . N1 N 0.0896(4) -0.1566(4) 0.2468(4) 0.0534(13) Uani 1 1 d . . . N2 N 0.1335(4) -0.0672(4) 0.0853(4) 0.0538(13) Uani 1 1 d . . . N3 N -0.3576(5) 0.2917(4) 0.4966(4) 0.0666(16) Uani 1 1 d . . . N4 N -0.4000(5) 0.2101(5) 0.7376(4) 0.0671(16) Uani 1 1 d . . . N5 N -0.2071(5) 0.5643(5) 0.0457(4) 0.0733(17) Uani 1 1 d . . . N6 N -0.2079(6) 0.7376(5) -0.1686(5) 0.097(2) Uani 1 1 d . . . C1 C 0.0668(6) -0.1971(6) 0.3316(5) 0.068(2) Uani 1 1 d . . . H30 H 0.0148 -0.1466 0.3678 0.082 Uiso 1 1 calc . . . C2 C 0.1155(7) -0.3071(6) 0.3670(5) 0.072(2) Uani 1 1 d . . . H40 H 0.0949 -0.3302 0.4256 0.086 Uiso 1 1 calc . . . C3 C 0.1953(5) -0.3858(5) 0.3177(5) 0.0554(16) Uani 1 1 d . . . C4 C 0.2198(6) -0.3442(5) 0.2297(5) 0.0589(17) Uani 1 1 d . . . H27 H 0.2718 -0.3937 0.1929 0.071 Uiso 1 1 calc . . . C5 C 0.1683(5) -0.2314(5) 0.1966(5) 0.0546(16) Uani 1 1 d . . . C6 C 0.1933(5) -0.1814(5) 0.1061(4) 0.0491(15) Uani 1 1 d . . . C7 C 0.2716(6) -0.2412(6) 0.0451(5) 0.0618(18) Uani 1 1 d . . . H35 H 0.3109 -0.3188 0.0599 0.074 Uiso 1 1 calc . . . C8 C 0.2941(6) -0.1890(6) -0.0386(5) 0.0603(17) Uani 1 1 d . A . C9 C 0.2301(6) -0.0750(6) -0.0575(5) 0.0657(19) Uani 1 1 d . . . H38 H 0.2397 -0.0365 -0.1134 0.079 Uiso 1 1 calc R . . C10 C 0.1524(6) -0.0165(6) 0.0041(5) 0.0621(18) Uani 1 1 d . . . H19 H 0.1114 0.0610 -0.0108 0.075 Uiso 1 1 calc R . . C11 C 0.2503(6) -0.5107(5) 0.3581(5) 0.0650(19) Uani 1 1 d . . . C12 C 0.1587(7) -0.5463(7) 0.3747(8) 0.105(3) Uani 1 1 d . . . H43A H 0.1921 -0.6244 0.4003 0.158 Uiso 1 1 calc R . . H43B H 0.1208 -0.5336 0.3168 0.158 Uiso 1 1 calc R . . H43C H 0.1050 -0.5034 0.4176 0.158 Uiso 1 1 calc R . . C13 C 0.3081(9) -0.5277(7) 0.4488(6) 0.106(3) Uani 1 1 d . . . H44A H 0.3424 -0.6055 0.4754 0.159 Uiso 1 1 calc R . . H44B H 0.2534 -0.4845 0.4910 0.159 Uiso 1 1 calc R . . H44C H 0.3654 -0.5039 0.4381 0.159 Uiso 1 1 calc R . . C14 C 0.3360(9) -0.5810(6) 0.2906(7) 0.124(4) Uani 1 1 d . . . H1A H 0.3697 -0.6587 0.3176 0.186 Uiso 1 1 calc R . . H1B H 0.3940 -0.5582 0.2788 0.186 Uiso 1 1 calc R . . H1C H 0.2980 -0.5700 0.2332 0.186 Uiso 1 1 calc R . . C15 C 0.3840(5) -0.2560(5) -0.1069(4) 0.0676(18) Uani 1 1 d DU . . C16A C 0.3519(8) -0.3374(8) -0.1383(7) 0.085(4) Uani 0.764(14) 1 d PDU A 1 H16A H 0.2802 -0.2966 -0.1709 0.128 Uiso 0.764(14) 1 calc PR A 1 H16B H 0.3464 -0.3863 -0.0850 0.128 Uiso 0.764(14) 1 calc PR A 1 H16C H 0.4088 -0.3809 -0.1790 0.128 Uiso 0.764(14) 1 calc PR A 1 C17A C 0.4970(7) -0.3188(9) -0.0558(7) 0.105(5) Uani 0.764(14) 1 d PDU A 1 H17A H 0.5165 -0.2664 -0.0363 0.158 Uiso 0.764(14) 1 calc PR A 1 H17B H 0.5540 -0.3621 -0.0964 0.158 Uiso 0.764(14) 1 calc PR A 1 H17C H 0.4922 -0.3677 -0.0022 0.158 Uiso 0.764(14) 1 calc PR A 1 C18A C 0.3943(10) -0.1798(9) -0.1908(6) 0.107(5) Uani 0.764(14) 1 d PDU A 1 H18A H 0.3232 -0.1392 -0.2243 0.161 Uiso 0.764(14) 1 calc PR A 1 H18B H 0.4519 -0.2238 -0.2307 0.161 Uiso 0.764(14) 1 calc PR A 1 H18C H 0.4142 -0.1280 -0.1706 0.161 Uiso 0.764(14) 1 calc PR A 1 C16B C 0.4380(16) -0.3795(8) -0.0680(16) 0.099(13) Uani 0.236(14) 1 d PDU A 2 H16D H 0.3819 -0.4049 -0.0640 0.149 Uiso 0.236(14) 1 calc PR A 2 H16E H 0.4692 -0.3917 -0.0071 0.149 Uiso 0.236(14) 1 calc PR A 2 H16F H 0.4973 -0.4204 -0.1082 0.149 Uiso 0.236(14) 1 calc PR A 2 C17B C 0.4719(14) -0.2154(17) -0.1146(14) 0.099(12) Uani 0.236(14) 1 d PDU A 2 H17D H 0.4372 -0.1372 -0.1403 0.149 Uiso 0.236(14) 1 calc PR A 2 H17E H 0.5312 -0.2568 -0.1546 0.149 Uiso 0.236(14) 1 calc PR A 2 H17F H 0.5031 -0.2263 -0.0540 0.149 Uiso 0.236(14) 1 calc PR A 2 C18B C 0.333(2) -0.2385(16) -0.2016(8) 0.086(12) Uani 0.236(14) 1 d PDU A 2 H18D H 0.2776 -0.2653 -0.1956 0.129 Uiso 0.236(14) 1 calc PR A 2 H18E H 0.3912 -0.2788 -0.2425 0.129 Uiso 0.236(14) 1 calc PR A 2 H18F H 0.2967 -0.1601 -0.2266 0.129 Uiso 0.236(14) 1 calc PR A 2 C1' C -0.0692(5) 0.0694(5) 0.2930(5) 0.0608(18) Uani 1 1 d . . . C2' C -0.1266(6) 0.1034(6) 0.3582(5) 0.0641(18) Uani 1 1 d . . . C3' C -0.1934(5) 0.1413(5) 0.4377(5) 0.0561(17) Uani 1 1 d . . . C4' C -0.1747(6) 0.0794(5) 0.5254(5) 0.0670(19) Uani 1 1 d . . . H4' H -0.1131 0.0083 0.5369 0.080 Uiso 1 1 calc . . . C5' C -0.2465(6) 0.1223(5) 0.5959(5) 0.0629(18) Uani 1 1 d . . . H5' H -0.2337 0.0796 0.6548 0.076 Uiso 1 1 calc . . . C6' C -0.3374(5) 0.2280(5) 0.5804(4) 0.0499(15) Uani 1 1 d . . . C7' C -0.2888(7) 0.2500(6) 0.4285(5) 0.073(2) Uani 1 1 d . . . H7' H -0.3036 0.2947 0.3704 0.088 Uiso 1 1 calc . . . C8' C -0.4158(5) 0.2775(5) 0.6554(5) 0.0536(16) Uani 1 1 d . . . C9' C -0.5019(6) 0.3873(5) 0.6400(5) 0.0634(18) Uani 1 1 d . . . H9' H -0.5110 0.4325 0.5826 0.076 Uiso 1 1 calc . . . C10' C -0.5733(7) 0.4274(6) 0.7124(6) 0.079(2) Uani 1 1 d . . . H10' H -0.6316 0.5007 0.7036 0.095 Uiso 1 1 calc . . . C11' C -0.5599(7) 0.3614(7) 0.7962(6) 0.084(2) Uani 1 1 d . . . H11' H -0.6082 0.3876 0.8451 0.101 Uiso 1 1 calc . . . C12' C -0.4724(6) 0.2548(7) 0.8057(5) 0.078(2) Uani 1 1 d . . . H12' H -0.4618 0.2097 0.8633 0.093 Uiso 1 1 calc R . . C1" C -0.0238(5) 0.1626(6) 0.1240(5) 0.0563(16) Uani 1 1 d . . . C2" C -0.0519(6) 0.2550(6) 0.0843(5) 0.0653(18) Uani 1 1 d . . . C3" C -0.0909(6) 0.3684(5) 0.0381(5) 0.0603(17) Uani 1 1 d . . . C4" C -0.0601(6) 0.4000(6) -0.0504(5) 0.072(2) Uani 1 1 d . . . H4" H -0.0105 0.3452 -0.0843 0.086 Uiso 1 1 calc R . . C5" C -0.1012(6) 0.5093(6) -0.0882(5) 0.073(2) Uani 1 1 d . . . H5" H -0.0780 0.5291 -0.1467 0.087 Uiso 1 1 calc R . . C6" C -0.1765(6) 0.5903(5) -0.0402(5) 0.0621(18) Uani 1 1 d . . . C7" C -0.1644(7) 0.4572(6) 0.0826(5) 0.079(2) Uani 1 1 d . . . H7" H -0.1852 0.4401 0.1428 0.095 Uiso 1 1 calc R . . C8" C -0.2260(6) 0.7115(6) -0.0790(5) 0.0661(19) Uani 1 1 d . . . C9" C -0.2903(7) 0.7939(6) -0.0256(6) 0.085(2) Uani 1 1 d . . . H9" H -0.3035 0.7746 0.0366 0.102 Uiso 1 1 calc R . . C10" C -0.3341(8) 0.9042(7) -0.0656(8) 0.101(3) Uani 1 1 d . . . H10" H -0.3782 0.9601 -0.0306 0.121 Uiso 1 1 calc R . . C11" C -0.3136(8) 0.9320(7) -0.1552(8) 0.102(3) Uani 1 1 d . . . H11" H -0.3403 1.0063 -0.1829 0.123 Uiso 1 1 calc R . . C12" C -0.2524(9) 0.8468(8) -0.2028(7) 0.121(4) Uani 1 1 d . . . H12" H -0.2399 0.8657 -0.2653 0.145 Uiso 1 1 calc R . . Cl2 Cl -0.0797(3) -0.2224(2) 0.5733(2) 0.1206(9) Uani 1 1 d . . . Cl1 Cl 0.1124(3) -0.4172(3) 0.6601(3) 0.1552(13) Uani 1 1 d . . . C1C C 0.0022(9) -0.2903(8) 0.6752(7) 0.108(3) Uani 1 1 d . . . H1CA H 0.0316 -0.2437 0.6934 0.129 Uiso 1 1 calc R . . H1CB H -0.0450 -0.3012 0.7249 0.129 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 0.05771(17) 0.04457(16) 0.05045(17) -0.01140(11) 0.01236(11) -0.01661(12) N1 0.061(3) 0.049(3) 0.049(3) -0.013(2) 0.013(3) -0.025(3) N2 0.054(3) 0.047(3) 0.053(3) -0.006(2) 0.009(2) -0.018(3) N3 0.076(4) 0.051(3) 0.050(4) -0.010(3) 0.009(3) -0.012(3) N4 0.077(4) 0.059(3) 0.047(3) -0.005(3) 0.016(3) -0.020(3) N5 0.087(4) 0.049(3) 0.067(4) -0.007(3) 0.022(3) -0.021(3) N6 0.106(5) 0.071(4) 0.079(5) 0.006(4) 0.029(4) -0.021(4) C1 0.085(5) 0.051(4) 0.057(5) -0.011(3) 0.022(4) -0.025(4) C2 0.090(5) 0.060(4) 0.059(5) -0.006(4) 0.022(4) -0.034(4) C3 0.060(4) 0.046(3) 0.056(4) -0.011(3) 0.004(3) -0.020(3) C4 0.070(4) 0.049(4) 0.058(4) -0.017(3) 0.016(3) -0.027(3) C5 0.061(4) 0.049(4) 0.053(4) -0.016(3) 0.008(3) -0.023(3) C6 0.056(4) 0.049(4) 0.040(4) -0.013(3) 0.012(3) -0.022(3) C7 0.069(4) 0.056(4) 0.059(4) -0.018(3) 0.013(3) -0.028(4) C8 0.061(4) 0.065(4) 0.055(4) -0.019(3) 0.010(3) -0.028(4) C9 0.081(5) 0.070(5) 0.044(4) -0.005(3) 0.021(3) -0.038(4) C10 0.067(4) 0.060(4) 0.049(4) -0.001(3) 0.013(3) -0.026(4) C11 0.086(5) 0.047(4) 0.062(5) 0.000(3) 0.002(4) -0.035(4) C12 0.095(6) 0.064(5) 0.150(9) 0.010(5) -0.009(6) -0.039(5) C13 0.133(8) 0.077(6) 0.088(7) 0.009(5) -0.022(6) -0.037(6) C14 0.153(9) 0.048(4) 0.120(8) -0.012(5) 0.054(7) -0.011(5) C15 0.063(4) 0.070(4) 0.066(4) -0.020(3) 0.021(3) -0.027(4) C16A 0.073(7) 0.097(8) 0.082(8) -0.045(7) 0.020(6) -0.029(6) C17A 0.063(6) 0.166(14) 0.072(8) -0.047(7) 0.018(5) -0.035(7) C18A 0.136(11) 0.102(8) 0.065(7) -0.030(5) 0.057(7) -0.042(7) C16B 0.11(3) 0.078(11) 0.07(2) -0.026(13) 0.051(19) -0.009(15) C17B 0.07(2) 0.15(3) 0.10(3) -0.08(2) 0.062(18) -0.06(2) C18B 0.075(19) 0.09(2) 0.071(15) -0.050(15) 0.022(13) -0.012(17) C1' 0.052(4) 0.049(4) 0.069(5) -0.002(3) 0.006(3) -0.017(3) C2' 0.071(4) 0.054(4) 0.058(5) -0.011(3) 0.018(4) -0.023(4) C3' 0.059(4) 0.047(4) 0.054(4) -0.016(3) 0.016(3) -0.017(3) C4' 0.070(4) 0.050(4) 0.066(5) -0.011(3) 0.019(4) -0.017(4) C5' 0.071(4) 0.051(4) 0.048(4) -0.001(3) 0.008(3) -0.016(4) C6' 0.050(3) 0.041(3) 0.048(4) -0.006(3) -0.001(3) -0.013(3) C7' 0.090(5) 0.054(4) 0.048(4) -0.008(3) 0.019(4) -0.014(4) C8' 0.050(4) 0.052(4) 0.053(4) -0.015(3) 0.005(3) -0.018(3) C9' 0.066(4) 0.052(4) 0.058(4) -0.008(3) 0.006(3) -0.016(4) C10' 0.081(5) 0.065(4) 0.063(5) -0.014(4) 0.008(4) -0.010(4) C11' 0.076(5) 0.085(6) 0.076(6) -0.038(5) 0.025(4) -0.019(5) C12' 0.083(5) 0.078(5) 0.049(4) -0.005(4) 0.016(4) -0.022(5) C1" 0.056(4) 0.054(4) 0.060(4) -0.018(3) 0.016(3) -0.025(3) C2" 0.076(5) 0.055(4) 0.060(5) -0.010(4) 0.009(4) -0.027(4) C3" 0.064(4) 0.052(4) 0.057(4) -0.008(3) 0.008(3) -0.021(3) C4" 0.082(5) 0.054(4) 0.055(4) -0.010(3) 0.015(4) -0.013(4) C5" 0.095(5) 0.055(4) 0.047(4) -0.008(3) 0.018(4) -0.021(4) C6" 0.064(4) 0.051(4) 0.063(5) -0.007(3) 0.010(3) -0.021(3) C7" 0.093(6) 0.056(4) 0.066(5) 0.002(4) 0.029(4) -0.023(4) C8" 0.061(4) 0.054(4) 0.077(5) -0.007(4) 0.010(4) -0.024(4) C9" 0.101(6) 0.057(5) 0.081(6) -0.007(4) 0.009(5) -0.025(5) C10" 0.104(7) 0.053(5) 0.134(9) -0.022(5) 0.022(6) -0.027(5) C11" 0.111(7) 0.061(5) 0.113(8) 0.008(5) 0.016(6) -0.031(5) C12" 0.125(8) 0.070(6) 0.103(8) 0.026(5) 0.021(6) -0.008(6) Cl2 0.146(2) 0.1033(18) 0.110(2) -0.0087(15) 0.0137(17) -0.0609(18) Cl1 0.123(2) 0.150(3) 0.146(3) -0.050(2) 0.008(2) -0.019(2) C1C 0.136(8) 0.110(7) 0.094(7) -0.024(6) 0.017(6) -0.071(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1' 1.950(7) . ? Pt1 C1" 1.952(7) . ? Pt1 N1 2.065(5) . ? Pt1 N2 2.070(5) . ? N1 C1 1.344(8) . ? N1 C5 1.355(8) . ? N2 C10 1.340(8) . ? N2 C6 1.370(8) . ? N3 C7' 1.320(8) . ? N3 C6' 1.336(8) . ? N4 C8' 1.344(8) . ? N4 C12' 1.350(9) . ? N5 C7" 1.324(9) . ? N5 C6" 1.336(9) . ? N6 C8" 1.332(9) . ? N6 C12" 1.338(10) . ? C1 C2 1.350(9) . ? C1 H30 0.9300 . ? C2 C3 1.379(9) . ? C2 H40 0.9300 . ? C3 C4 1.398(9) . ? C3 C11 1.532(9) . ? C4 C5 1.373(9) . ? C4 H27 0.9300 . ? C5 C6 1.475(9) . ? C6 C7 1.372(8) . ? C7 C8 1.397(9) . ? C7 H35 0.9300 . ? C8 C9 1.369(9) . ? C8 C15 1.549(9) . ? C9 C10 1.368(9) . ? C9 H38 0.9300 . ? C10 H19 0.9300 . ? C11 C13 1.502(11) . ? C11 C12 1.512(11) . ? C11 C14 1.533(11) . ? C12 H43A 0.9600 . ? C12 H43B 0.9600 . ? C12 H43C 0.9600 . ? C13 H44A 0.9600 . ? C13 H44B 0.9600 . ? C13 H44C 0.9600 . ? C14 H1A 0.9600 . ? C14 H1B 0.9600 . ? C14 H1C 0.9600 . ? C15 C17A 1.511(6) . ? C15 C17B 1.512(6) . ? C15 C16A 1.512(6) . ? C15 C18B 1.512(6) . ? C15 C16B 1.512(6) . ? C15 C18A 1.512(6) . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C17A H17A 0.9600 . ? C17A H17B 0.9600 . ? C17A H17C 0.9600 . ? C18A H18A 0.9600 . ? C18A H18B 0.9600 . ? C18A H18C 0.9600 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? C17B H17D 0.9600 . ? C17B H17E 0.9600 . ? C17B H17F 0.9600 . ? C18B H18D 0.9600 . ? C18B H18E 0.9600 . ? C18B H18F 0.9600 . ? C1' C2' 1.197(9) . ? C2' C3' 1.430(9) . ? C3' C4' 1.374(10) . ? C3' C7' 1.426(9) . ? C4' C5' 1.368(9) . ? C4' H4' 0.9300 . ? C5' C6' 1.377(9) . ? C5' H5' 0.9300 . ? C6' C8' 1.481(9) . ? C7' H7' 0.9300 . ? C8' C9' 1.389(9) . ? C9' C10' 1.380(10) . ? C9' H9' 0.9300 . ? C10' C11' 1.358(11) . ? C10' H10' 0.9300 . ? C11' C12' 1.366(11) . ? C11' H11' 0.9300 . ? C12' H12' 0.9300 . ? C1" C2" 1.188(9) . ? C2" C3" 1.439(9) . ? C3" C7" 1.389(9) . ? C3" C4" 1.390(9) . ? C4" C5" 1.354(9) . ? C4" H4" 0.9300 . ? C5" C6" 1.363(9) . ? C5" H5" 0.9300 . ? C6" C8" 1.488(9) . ? C7" H7" 0.9300 . ? C8" C9" 1.386(10) . ? C9" C10" 1.372(11) . ? C9" H9" 0.9300 . ? C10" C11" 1.345(13) . ? C10" H10" 0.9300 . ? C11" C12" 1.350(13) . ? C11" H11" 0.9300 . ? C12" H12" 0.9300 . ? Cl2 C1C 1.747(10) . ? Cl1 C1C 1.710(10) . ? C1C H1CA 0.9700 . ? C1C H1CB 0.9700 . ? 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 C1' Pt1 C1" 89.4(3) . . ? C1' Pt1 N1 95.9(2) . . ? C1" Pt1 N1 174.6(2) . . ? C1' Pt1 N2 174.9(2) . . ? C1" Pt1 N2 95.6(2) . . ? N1 Pt1 N2 79.0(2) . . ? C1 N1 C5 117.2(5) . . ? C1 N1 Pt1 126.6(4) . . ? C5 N1 Pt1 116.0(4) . . ? C10 N2 C6 118.5(5) . . ? C10 N2 Pt1 126.7(4) . . ? C6 N2 Pt1 114.8(4) . . ? C7' N3 C6' 118.2(6) . . ? C8' N4 C12' 116.5(6) . . ? C7" N5 C6" 118.2(6) . . ? C8" N6 C12" 116.5(7) . . ? N1 C1 C2 123.4(6) . . ? N1 C1 H30 118.3 . . ? C2 C1 H30 118.3 . . ? C1 C2 C3 121.0(6) . . ? C1 C2 H40 119.5 . . ? C3 C2 H40 119.5 . . ? C2 C3 C4 115.8(6) . . ? C2 C3 C11 120.8(6) . . ? C4 C3 C11 123.3(6) . . ? C5 C4 C3 121.1(6) . . ? C5 C4 H27 119.4 . . ? C3 C4 H27 119.4 . . ? N1 C5 C4 121.4(6) . . ? N1 C5 C6 114.7(5) . . ? C4 C5 C6 124.0(5) . . ? N2 C6 C7 120.0(6) . . ? N2 C6 C5 115.5(5) . . ? C7 C6 C5 124.5(6) . . ? C6 C7 C8 121.9(6) . . ? C6 C7 H35 119.0 . . ? C8 C7 H35 119.0 . . ? C9 C8 C7 115.8(6) . . ? C9 C8 C15 122.1(6) . . ? C7 C8 C15 122.1(6) . . ? C10 C9 C8 121.5(6) . . ? C10 C9 H38 119.2 . . ? C8 C9 H38 119.2 . . ? N2 C10 C9 122.1(6) . . ? N2 C10 H19 118.9 . . ? C9 C10 H19 118.9 . . ? C13 C11 C12 109.8(7) . . ? C13 C11 C3 108.4(6) . . ? C12 C11 C3 108.6(6) . . ? C13 C11 C14 110.2(8) . . ? C12 C11 C14 108.8(7) . . ? C3 C11 C14 111.0(6) . . ? C11 C12 H43A 109.5 . . ? C11 C12 H43B 109.5 . . ? H43A C12 H43B 109.5 . . ? C11 C12 H43C 109.5 . . ? H43A C12 H43C 109.5 . . ? H43B C12 H43C 109.5 . . ? C11 C13 H44A 109.5 . . ? C11 C13 H44B 109.5 . . ? H44A C13 H44B 109.5 . . ? C11 C13 H44C 109.5 . . ? H44A C13 H44C 109.5 . . ? H44B C13 H44C 109.5 . . ? C11 C14 H1A 109.5 . . ? C11 C14 H1B 109.5 . . ? H1A C14 H1B 109.5 . . ? C11 C14 H1C 109.5 . . ? H1A C14 H1C 109.5 . . ? H1B C14 H1C 109.5 . . ? C17A C15 C17B 56.31(17) . . ? C17A C15 C16A 110.2(4) . . ? C17B C15 C16A 144.3(13) . . ? C17A C15 C18B 140.3(12) . . ? C17B C15 C18B 110.4(7) . . ? C16A C15 C18B 56.28(17) . . ? C17A C15 C16B 56.30(17) . . ? C17B C15 C16B 110.0(7) . . ? C16A C15 C16B 56.29(17) . . ? C18B C15 C16B 108.5(8) . . ? C17A C15 C18A 108.2(5) . . ? C17B C15 C18A 56.29(17) . . ? C16A C15 C18A 109.6(4) . . ? C18B C15 C18A 56.26(17) . . ? C16B C15 C18A 138.7(12) . . ? C17A C15 C8 107.9(6) . . ? C17B C15 C8 106.4(12) . . ? C16A C15 C8 109.2(6) . . ? C18B C15 C8 111.8(12) . . ? C16B C15 C8 109.6(12) . . ? C18A C15 C8 111.7(6) . . ? C15 C16A H16A 109.5 . . ? C15 C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15 C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? C15 C17A H17A 109.5 . . ? C15 C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C15 C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? C15 C18A H18A 109.5 . . ? C15 C18A H18B 109.5 . . ? H18A C18A H18B 109.5 . . ? C15 C18A H18C 109.5 . . ? H18A C18A H18C 109.5 . . ? H18B C18A H18C 109.5 . . ? C15 C16B H16D 109.5 . . ? C15 C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15 C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C15 C17B H17D 109.5 . . ? C15 C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C15 C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C15 C18B H18D 109.5 . . ? C15 C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C15 C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C2' C1' Pt1 178.4(6) . . ? C1' C2' C3' 178.5(8) . . ? C4' C3' C7' 115.2(6) . . ? C4' C3' C2' 125.0(6) . . ? C7' C3' C2' 119.9(6) . . ? C5' C4' C3' 120.2(6) . . ? C5' C4' H4' 119.9 . . ? C3' C4' H4' 119.9 . . ? C4' C5' C6' 120.7(6) . . ? C4' C5' H5' 119.6 . . ? C6' C5' H5' 119.6 . . ? N3 C6' C5' 121.1(6) . . ? N3 C6' C8' 116.8(5) . . ? C5' C6' C8' 122.1(6) . . ? N3 C7' C3' 124.7(6) . . ? N3 C7' H7' 117.7 . . ? C3' C7' H7' 117.7 . . ? N4 C8' C9' 122.5(6) . . ? N4 C8' C6' 116.4(5) . . ? C9' C8' C6' 121.1(6) . . ? C10' C9' C8' 118.1(6) . . ? C10' C9' H9' 121.0 . . ? C8' C9' H9' 121.0 . . ? C11' C10' C9' 120.9(7) . . ? C11' C10' H10' 119.5 . . ? C9' C10' H10' 119.5 . . ? C10' C11' C12' 117.2(7) . . ? C10' C11' H11' 121.4 . . ? C12' C11' H11' 121.4 . . ? N4 C12' C11' 124.9(7) . . ? N4 C12' H12' 117.6 . . ? C11' C12' H12' 117.6 . . ? C2" C1" Pt1 178.5(6) . . ? C1" C2" C3" 177.4(8) . . ? C7" C3" C4" 114.5(6) . . ? C7" C3" C2" 120.1(6) . . ? C4" C3" C2" 125.4(6) . . ? C5" C4" C3" 121.2(6) . . ? C5" C4" H4" 119.4 . . ? C3" C4" H4" 119.4 . . ? C4" C5" C6" 119.9(7) . . ? C4" C5" H5" 120.1 . . ? C6" C5" H5" 120.1 . . ? N5 C6" C5" 121.2(6) . . ? N5 C6" C8" 116.6(6) . . ? C5" C6" C8" 122.2(6) . . ? N5 C7" C3" 125.0(7) . . ? N5 C7" H7" 117.5 . . ? C3" C7" H7" 117.5 . . ? N6 C8" C9" 121.2(7) . . ? N6 C8" C6" 116.9(6) . . ? C9" C8" C6" 121.9(7) . . ? C10" C9" C8" 119.1(8) . . ? C10" C9" H9" 120.5 . . ? C8" C9" H9" 120.5 . . ? C11" C10" C9" 120.4(8) . . ? C11" C10" H10" 119.8 . . ? C9" C10" H10" 119.8 . . ? C10" C11" C12" 116.7(8) . . ? C10" C11" H11" 121.6 . . ? C12" C11" H11" 121.6 . . ? N6 C12" C11" 126.0(9) . . ? N6 C12" H12" 117.0 . . ? C11" C12" H12" 117.0 . . ? Cl1 C1C Cl2 111.3(6) . . ? Cl1 C1C H1CA 109.4 . . ? Cl2 C1C H1CA 109.4 . . ? Cl1 C1C H1CB 109.4 . . ? Cl2 C1C H1CB 109.4 . . ? H1CA C1C H1CB 108.0 . . ? 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 C1' Pt1 N1 C1 -2.1(6) . . . . ? N2 Pt1 N1 C1 177.4(6) . . . . ? C1' Pt1 N1 C5 -176.8(5) . . . . ? N2 Pt1 N1 C5 2.8(5) . . . . ? C1" Pt1 N2 C10 0.0(6) . . . . ? N1 Pt1 N2 C10 -179.8(6) . . . . ? C1" Pt1 N2 C6 176.9(5) . . . . ? N1 Pt1 N2 C6 -2.9(4) . . . . ? C5 N1 C1 C2 -2.1(11) . . . . ? Pt1 N1 C1 C2 -176.7(6) . . . . ? N1 C1 C2 C3 1.6(13) . . . . ? C1 C2 C3 C4 -1.1(11) . . . . ? C1 C2 C3 C11 -180.0(7) . . . . ? C2 C3 C4 C5 1.3(10) . . . . ? C11 C3 C4 C5 -179.8(6) . . . . ? C1 N1 C5 C4 2.2(10) . . . . ? Pt1 N1 C5 C4 177.4(5) . . . . ? C1 N1 C5 C6 -177.4(6) . . . . ? Pt1 N1 C5 C6 -2.2(7) . . . . ? C3 C4 C5 N1 -1.9(10) . . . . ? C3 C4 C5 C6 177.6(6) . . . . ? C10 N2 C6 C7 0.9(9) . . . . ? Pt1 N2 C6 C7 -176.3(5) . . . . ? C10 N2 C6 C5 179.8(6) . . . . ? Pt1 N2 C6 C5 2.6(7) . . . . ? N1 C5 C6 N2 -0.3(8) . . . . ? C4 C5 C6 N2 -179.9(6) . . . . ? N1 C5 C6 C7 178.6(6) . . . . ? C4 C5 C6 C7 -1.0(11) . . . . ? N2 C6 C7 C8 0.8(11) . . . . ? C5 C6 C7 C8 -178.1(6) . . . . ? C6 C7 C8 C9 -2.4(11) . . . . ? C6 C7 C8 C15 178.9(6) . . . . ? C7 C8 C9 C10 2.5(11) . . . . ? C15 C8 C9 C10 -178.8(6) . . . . ? C6 N2 C10 C9 -0.8(10) . . . . ? Pt1 N2 C10 C9 176.0(5) . . . . ? C8 C9 C10 N2 -1.0(12) . . . . ? C2 C3 C11 C13 -58.7(9) . . . . ? C4 C3 C11 C13 122.6(8) . . . . ? C2 C3 C11 C12 60.6(9) . . . . ? C4 C3 C11 C12 -118.2(8) . . . . ? C2 C3 C11 C14 -179.9(8) . . . . ? C4 C3 C11 C14 1.4(10) . . . . ? C9 C8 C15 C17A 121.7(7) . . . . ? C7 C8 C15 C17A -59.6(8) . . . . ? C9 C8 C15 C17B 62.6(8) . . . . ? C7 C8 C15 C17B -118.8(7) . . . . ? C9 C8 C15 C16A -118.5(7) . . . . ? C7 C8 C15 C16A 60.2(8) . . . . ? C9 C8 C15 C18B -58.1(8) . . . . ? C7 C8 C15 C18B 120.6(7) . . . . ? C9 C8 C15 C16B -178.5(7) . . . . ? C7 C8 C15 C16B 0.1(8) . . . . ? C9 C8 C15 C18A 2.9(9) . . . . ? C7 C8 C15 C18A -178.4(7) . . . . ? C7' C3' C4' C5' 1.3(11) . . . . ? C2' C3' C4' C5' -177.6(7) . . . . ? C3' C4' C5' C6' -0.8(12) . . . . ? C7' N3 C6' C5' 0.9(11) . . . . ? C7' N3 C6' C8' 179.7(7) . . . . ? C4' C5' C6' N3 -0.4(11) . . . . ? C4' C5' C6' C8' -179.2(7) . . . . ? C6' N3 C7' C3' -0.2(12) . . . . ? C4' C3' C7' N3 -0.9(12) . . . . ? C2' C3' C7' N3 178.1(7) . . . . ? C12' N4 C8' C9' -0.3(11) . . . . ? C12' N4 C8' C6' -179.2(7) . . . . ? N3 C6' C8' N4 175.2(6) . . . . ? C5' C6' C8' N4 -5.9(10) . . . . ? N3 C6' C8' C9' -3.7(9) . . . . ? C5' C6' C8' C9' 175.1(7) . . . . ? N4 C8' C9' C10' -0.2(11) . . . . ? C6' C8' C9' C10' 178.7(7) . . . . ? C8' C9' C10' C11' 0.0(13) . . . . ? C9' C10' C11' C12' 0.6(14) . . . . ? C8' N4 C12' C11' 1.0(12) . . . . ? C10' C11' C12' N4 -1.2(14) . . . . ? C7" C3" C4" C5" -0.6(12) . . . . ? C2" C3" C4" C5" -179.9(8) . . . . ? C3" C4" C5" C6" -1.9(12) . . . . ? C7" N5 C6" C5" -1.6(12) . . . . ? C7" N5 C6" C8" -179.9(7) . . . . ? C4" C5" C6" N5 3.1(12) . . . . ? C4" C5" C6" C8" -178.7(7) . . . . ? C6" N5 C7" C3" -1.1(13) . . . . ? C4" C3" C7" N5 2.2(13) . . . . ? C2" C3" C7" N5 -178.5(8) . . . . ? C12" N6 C8" C9" 1.6(13) . . . . ? C12" N6 C8" C6" -179.7(9) . . . . ? N5 C6" C8" N6 -171.5(7) . . . . ? C5" C6" C8" N6 10.3(11) . . . . ? N5 C6" C8" C9" 7.2(11) . . . . ? C5" C6" C8" C9" -171.1(8) . . . . ? N6 C8" C9" C10" -1.1(13) . . . . ? C6" C8" C9" C10" -179.7(8) . . . . ? C8" C9" C10" C11" -0.9(15) . . . . ? C9" C10" C11" C12" 2.3(16) . . . . ? C8" N6 C12" C11" -0.1(17) . . . . ? C10" C11" C12" N6 -1.9(19) . . . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 24.45 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.655 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.113 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 0.500 492.0 133.2 _platon_squeeze_details ; ? ;