# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1486 data_1 _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone 'Int. code + (231) 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Trans.' _publ_title ; Mono- and dinuclear complexes of (trpy)M(II) (M=Pd, Pt) with the model nucleobase 1-methylcytosine. Crystal structure and NMR solution studies. ; _publ_author_address ; Sultan Cosar, Matthias B. L. Janik, Matthias Flock, Eva Freisinger, and Bernhard Lippert Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany Etelka Farkas Department of Inorganic and Analytical Chemistry L. Kossuth University Debrecen Hungary ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[(terpyPd)(1-MeC-N3)](NO3)2 * 5H2O' _chemical_formula_analytical ? _chemical_formula_sum 'C20 H28 N8 O12 Pd' _chemical_formula_weight 678.90 _chemical_melting_point ? _chemical_compound_source ? 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 monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.104(2) _cell_length_b 10.193(2) _cell_length_c 24.365(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.34(3) _cell_angle_gamma 90.00 _cell_volume 2721.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7866 _cell_measurement_theta_min 3.37 _cell_measurement_theta_max 24.49 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.125 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method ? _exptl_crystal_F_000 1384 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.8332 _exptl_absorpt_correction_T_max 0.9112 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 60s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7866 _diffrn_reflns_av_R_equivalents 0.0514 _diffrn_reflns_av_sigmaI/netI 0.0818 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 24.49 _reflns_number_total 4461 _reflns_number_observed 3427 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 4456 _refine_ls_number_parameters 375 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0585 _refine_ls_R_factor_obs 0.0366 _refine_ls_wR_factor_all 0.0705 _refine_ls_wR_factor_obs 0.0641 _refine_ls_goodness_of_fit_all 0.912 _refine_ls_goodness_of_fit_obs 0.998 _refine_ls_restrained_S_all 0.952 _refine_ls_restrained_S_obs 0.998 _refine_ls_shift/esd_max 0.010 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.25002(3) 0.32236(4) 0.25008(2) 0.04164(12) Uani 1 d . . N1 N 0.4094(4) 0.4894(5) 0.4020(2) 0.0532(12) Uani 1 d . . C1 C 0.4662(6) 0.6172(7) 0.4170(3) 0.081(2) Uani 1 d . . H1A H 0.4166(29) 0.6855(8) 0.3979(20) 0.173(22) Uiso 1 calc R . H1B H 0.5459(23) 0.6196(23) 0.4066(24) 0.173(22) Uiso 1 calc R . H1C H 0.4731(52) 0.6300(27) 0.4565(4) 0.173(22) Uiso 1 calc R . C2 C 0.3656(5) 0.4615(7) 0.3475(2) 0.0521(15) Uani 1 d . . O2 O 0.3701(3) 0.5446(4) 0.3110(2) 0.0608(10) Uani 1 d . . N3 N 0.3132(7) 0.3407(6) 0.3326(3) 0.041(2) Uani 1 d . . C4 C 0.3048(5) 0.2522(8) 0.3725(3) 0.056(2) Uani 1 d . . N4 N 0.2499(4) 0.1383(5) 0.3589(2) 0.0595(14) Uani 1 d . . H4A H 0.2201(4) 0.1218(5) 0.3248(2) 0.066(13) Uiso 1 calc R . H4B H 0.2442(4) 0.0810(5) 0.3843(2) 0.066(13) Uiso 1 calc R . C5 C 0.3510(7) 0.2794(9) 0.4296(3) 0.063(2) Uani 1 d . . H5 H 0.3466(7) 0.2180(9) 0.4574(3) 0.064(13) Uiso 1 calc R . C6 C 0.4014(6) 0.3989(9) 0.4410(3) 0.064(2) Uani 1 d . . H6 H 0.4321(6) 0.4193(9) 0.4778(3) 0.064(13) Uiso 1 calc R . N1A N 0.0753(4) 0.3692(4) 0.2535(2) 0.0411(11) Uani 1 d . . C2A C 0.0044(5) 0.3758(5) 0.2017(2) 0.0472(14) Uani 1 d . . C3A C -0.1188(5) 0.4015(6) 0.1965(3) 0.057(2) Uani 1 d . . H3A H -0.1666(5) 0.4069(6) 0.1615(3) 0.050(4) Uiso 1 calc R . C4A C -0.1702(5) 0.4192(6) 0.2438(3) 0.064(2) Uani 1 d . . H4A1 H -0.2530(5) 0.4376(6) 0.2407(3) 0.050(4) Uiso 1 calc R . C5A C -0.1008(5) 0.4099(6) 0.2946(3) 0.062(2) Uani 1 d . . H5A H -0.1355(5) 0.4182(6) 0.3267(3) 0.050(4) Uiso 1 calc R . C6A C 0.0234(5) 0.3876(6) 0.2977(2) 0.0551(15) Uani 1 d . . H6A H 0.0721(5) 0.3856(6) 0.3325(2) 0.050(4) Uiso 1 calc R . N1B N 0.1885(7) 0.3161(5) 0.1713(3) 0.045(2) Uani 1 d . . C2B C 0.0696(5) 0.3489(5) 0.1548(2) 0.0435(14) Uani 1 d . . C3B C 0.0253(5) 0.3546(6) 0.0989(2) 0.057(2) Uani 1 d . . H3B H -0.0554(5) 0.3780(6) 0.0863(2) 0.050(4) Uiso 1 calc R . C4B C 0.1023(7) 0.3252(6) 0.0617(3) 0.053(2) Uani 1 d . . H4B1 H 0.0726(7) 0.3298(6) 0.0238(3) 0.050(4) Uiso 1 calc R . C5B C 0.2231(6) 0.2889(7) 0.0790(2) 0.053(2) Uani 1 d . . H5B H 0.2738(6) 0.2672(7) 0.0535(2) 0.050(4) Uiso 1 calc R . C6B C 0.2653(5) 0.2862(5) 0.1360(2) 0.0415(15) Uani 1 d . . N1C N 0.4022(4) 0.2638(5) 0.2222(2) 0.0417(11) Uani 1 d . . C2C C 0.3873(4) 0.2538(5) 0.1644(2) 0.0432(13) Uani 1 d . . C3C C 0.4841(5) 0.2147(5) 0.1380(2) 0.050(2) Uani 1 d . . H3C H 0.4744(5) 0.2111(5) 0.0994(2) 0.050(4) Uiso 1 calc R . C4C C 0.5944(5) 0.1814(6) 0.1698(2) 0.0539(14) Uani 1 d . . H4C H 0.6590(5) 0.1526(6) 0.1530(2) 0.050(4) Uiso 1 calc R . C5C C 0.6073(5) 0.1912(6) 0.2261(3) 0.057(2) Uani 1 d . . H5C H 0.6812(5) 0.1692(6) 0.2480(3) 0.050(4) Uiso 1 calc R . C6C C 0.5112(5) 0.2338(5) 0.2508(2) 0.0476(14) Uani 1 d . . H6C H 0.5231(5) 0.2421(5) 0.2893(2) 0.050(4) Uiso 1 calc R . N10 N -0.0380(6) 0.0440(6) 0.1192(3) 0.0693(15) Uani 1 d . . O11 O 0.0708(4) 0.0321(5) 0.1407(2) 0.0802(13) Uani 1 d . . O12 O -0.0677(5) 0.0168(6) 0.0697(2) 0.100(2) Uani 1 d . . O13 O -0.1130(6) 0.0755(6) 0.1479(3) 0.100(2) Uani 1 d . . N20 N 0.1504(5) 0.7288(7) 0.3976(2) 0.070(2) Uani 1 d . . O21 O 0.1951(5) 0.7229(5) 0.4479(2) 0.096(2) Uani 1 d . . O22 O 0.1599(5) 0.8266(6) 0.3702(2) 0.109(2) Uani 1 d . . O23 O 0.0977(7) 0.6311(6) 0.3748(2) 0.105(2) Uani 1 d . . O1W O 0.5754(3) 0.5638(4) 0.2602(2) 0.0620(11) Uani 1 d . . O2W O 0.7165(4) 0.4233(5) 0.0595(2) 0.087(2) Uani 1 d . . O3W O 0.8002(5) 0.4739(5) 0.4682(2) 0.098(2) Uani 1 d . . O4W O 0.6846(5) 0.1609(5) 0.0447(2) 0.0908(14) Uani 1 d . . O5W O 0.0430(5) 0.4291(6) 0.4479(2) 0.099(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0388(2) 0.0517(2) 0.0341(2) -0.0011(4) 0.00493(13) 0.0018(4) N1 0.048(3) 0.075(4) 0.036(3) -0.006(3) 0.006(2) -0.002(3) C1 0.071(4) 0.083(5) 0.086(5) -0.028(4) 0.005(4) -0.015(4) C2 0.040(3) 0.082(5) 0.034(4) 0.005(4) 0.008(3) 0.005(3) O2 0.055(2) 0.070(3) 0.058(3) -0.005(2) 0.011(2) -0.007(2) N3 0.043(4) 0.050(4) 0.030(4) 0.003(3) 0.001(3) -0.003(3) C4 0.047(4) 0.071(5) 0.048(4) -0.019(4) 0.006(3) 0.007(4) N4 0.074(4) 0.062(4) 0.041(3) 0.009(3) 0.007(2) 0.000(3) C5 0.073(6) 0.069(5) 0.049(5) 0.000(4) 0.012(4) -0.004(5) C6 0.056(4) 0.088(7) 0.044(5) -0.005(5) -0.007(3) 0.007(4) N1A 0.038(2) 0.039(3) 0.046(3) 0.000(2) 0.006(2) 0.006(2) C2A 0.048(3) 0.040(3) 0.051(4) -0.003(3) 0.003(3) 0.003(3) C3A 0.041(3) 0.070(4) 0.057(4) 0.000(3) -0.004(3) 0.001(3) C4A 0.041(3) 0.062(5) 0.091(5) -0.018(4) 0.016(4) 0.005(3) C5A 0.053(4) 0.068(5) 0.070(5) -0.007(4) 0.027(3) 0.003(3) C6A 0.062(4) 0.059(4) 0.046(4) -0.007(3) 0.013(3) 0.004(3) N1B 0.046(4) 0.048(4) 0.044(4) -0.009(3) 0.013(3) -0.002(3) C2B 0.048(3) 0.033(4) 0.046(4) 0.002(3) -0.001(3) -0.006(3) C3B 0.050(3) 0.061(5) 0.057(4) 0.001(3) -0.005(3) 0.004(3) C4B 0.075(5) 0.048(5) 0.032(4) -0.006(4) 0.001(4) -0.006(4) C5B 0.060(4) 0.065(5) 0.036(4) -0.004(3) 0.008(3) -0.007(4) C6B 0.053(4) 0.039(4) 0.034(3) -0.001(2) 0.010(3) -0.001(3) N1C 0.037(3) 0.045(3) 0.042(3) 0.003(2) 0.004(2) -0.003(2) C2C 0.044(3) 0.048(3) 0.038(3) 0.005(3) 0.009(3) -0.005(3) C3C 0.058(4) 0.052(4) 0.045(3) -0.001(3) 0.020(3) -0.002(3) C4C 0.052(3) 0.053(4) 0.061(4) 0.001(4) 0.021(3) 0.001(3) C5C 0.041(3) 0.053(4) 0.077(4) 0.006(4) 0.010(3) 0.004(3) C6C 0.042(3) 0.060(4) 0.039(3) -0.003(3) 0.000(3) 0.000(3) N10 0.085(5) 0.054(4) 0.066(4) 0.010(3) 0.000(4) -0.025(3) O11 0.082(3) 0.075(3) 0.080(3) -0.003(3) 0.002(3) 0.000(3) O12 0.128(4) 0.123(5) 0.043(3) -0.003(3) -0.004(3) -0.035(4) O13 0.083(4) 0.097(5) 0.128(5) -0.017(4) 0.038(4) -0.003(4) N20 0.057(3) 0.103(5) 0.050(4) 0.007(4) 0.006(3) -0.004(3) O21 0.106(4) 0.141(5) 0.039(3) 0.007(3) 0.006(3) -0.028(3) O22 0.128(5) 0.106(4) 0.081(4) 0.023(4) -0.015(3) -0.042(4) O23 0.128(5) 0.095(5) 0.088(5) 0.001(4) 0.002(4) -0.030(4) O1W 0.057(2) 0.059(3) 0.070(3) 0.000(2) 0.008(2) -0.007(2) O2W 0.073(3) 0.106(4) 0.082(4) 0.006(3) 0.014(3) 0.002(3) O3W 0.113(4) 0.078(4) 0.107(5) -0.004(3) 0.031(3) -0.021(3) O4W 0.101(4) 0.093(4) 0.080(3) -0.003(3) 0.020(3) 0.003(3) O5W 0.119(4) 0.096(4) 0.079(4) 0.012(3) 0.007(3) -0.006(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd1 N1B 1.932(7) . ? Pd1 N1C 2.011(4) . ? Pd1 N1A 2.013(4) . ? Pd1 N3 2.028(7) . ? N1 C6 1.338(8) . ? N1 C2 1.368(6) . ? N1 C1 1.467(8) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 O2 1.234(6) . ? C2 N3 1.385(9) . ? N3 C4 1.340(9) . ? C4 N4 1.328(8) . ? C4 C5 1.430(10) . ? N4 H4A 0.86 . ? N4 H4B 0.86 . ? C5 C6 1.351(11) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? N1A C6A 1.314(6) . ? N1A C2A 1.376(6) . ? C2A C3A 1.378(7) . ? C2A C2B 1.474(7) . ? C3A C4A 1.378(8) . ? C3A H3A 0.93 . ? C4A C5A 1.352(8) . ? C4A H4A1 0.93 . ? C5A C6A 1.388(7) . ? C5A H5A 0.93 . ? C6A H6A 0.93 . ? N1B C6B 1.341(8) . ? N1B C2B 1.358(9) . ? C2B C3B 1.374(7) . ? C3B C4B 1.375(9) . ? C3B H3B 0.93 . ? C4B C5B 1.390(9) . ? C4B H4B1 0.93 . ? C5B C6B 1.391(8) . ? C5B H5B 0.93 . ? C6B C2C 1.456(7) . ? N1C C6C 1.330(6) . ? N1C C2C 1.396(6) . ? C2C C3C 1.397(7) . ? C3C C4C 1.381(8) . ? C3C H3C 0.93 . ? C4C C5C 1.360(7) . ? C4C H4C 0.93 . ? C5C C6C 1.377(8) . ? C5C H5C 0.93 . ? C6C H6C 0.93 . ? N10 O13 1.214(7) . ? N10 O12 1.230(6) . ? N10 O11 1.242(6) . ? N20 O22 1.213(7) . ? N20 O23 1.240(8) . ? N20 O21 1.247(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 N1B Pd1 N1C 80.5(3) . . ? N1B Pd1 N1A 82.0(3) . . ? N1C Pd1 N1A 162.3(2) . . ? N1B Pd1 N3 176.6(2) . . ? N1C Pd1 N3 100.8(2) . . ? N1A Pd1 N3 96.8(2) . . ? C6 N1 C2 119.5(6) . . ? C6 N1 C1 120.6(6) . . ? C2 N1 C1 119.9(6) . . ? N1 C1 H1A 109.5(3) . . ? N1 C1 H1B 109.5(3) . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5(3) . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 N1 120.4(6) . . ? O2 C2 N3 119.1(6) . . ? N1 C2 N3 120.5(6) . . ? C4 N3 C2 119.0(7) . . ? C4 N3 Pd1 127.1(5) . . ? C2 N3 Pd1 113.9(5) . . ? N4 C4 N3 119.5(6) . . ? N4 C4 C5 119.3(7) . . ? N3 C4 C5 121.2(7) . . ? C4 N4 H4A 120.0(4) . . ? C4 N4 H4B 120.0(4) . . ? H4A N4 H4B 120.0 . . ? C6 C5 C4 116.5(8) . . ? C6 C5 H5 121.7(5) . . ? C4 C5 H5 121.7(5) . . ? N1 C6 C5 123.3(7) . . ? N1 C6 H6 118.4(4) . . ? C5 C6 H6 118.4(5) . . ? C6A N1A C2A 118.8(5) . . ? C6A N1A Pd1 128.4(4) . . ? C2A N1A Pd1 112.7(3) . . ? N1A C2A C3A 120.4(5) . . ? N1A C2A C2B 114.9(4) . . ? C3A C2A C2B 124.6(5) . . ? C2A C3A C4A 119.1(6) . . ? C2A C3A H3A 120.5(3) . . ? C4A C3A H3A 120.5(4) . . ? C5A C4A C3A 120.4(6) . . ? C5A C4A H4A1 119.8(3) . . ? C3A C4A H4A1 119.8(4) . . ? C4A C5A C6A 118.3(5) . . ? C4A C5A H5A 120.8(3) . . ? C6A C5A H5A 120.8(4) . . ? N1A C6A C5A 122.9(6) . . ? N1A C6A H6A 118.5(3) . . ? C5A C6A H6A 118.5(4) . . ? C6B N1B C2B 123.8(7) . . ? C6B N1B Pd1 119.1(6) . . ? C2B N1B Pd1 117.1(5) . . ? N1B C2B C3B 118.5(5) . . ? N1B C2B C2A 113.2(5) . . ? C3B C2B C2A 128.3(5) . . ? C2B C3B C4B 118.9(5) . . ? C2B C3B H3B 120.6(3) . . ? C4B C3B H3B 120.6(4) . . ? C3B C4B C5B 122.1(7) . . ? C3B C4B H4B1 118.9(4) . . ? C5B C4B H4B1 118.9(4) . . ? C4B C5B C6B 117.4(6) . . ? C4B C5B H5B 121.3(4) . . ? C6B C5B H5B 121.3(4) . . ? N1B C6B C5B 119.3(6) . . ? N1B C6B C2C 112.7(5) . . ? C5B C6B C2C 128.0(5) . . ? C6C N1C C2C 117.4(4) . . ? C6C N1C Pd1 129.4(4) . . ? C2C N1C Pd1 113.2(3) . . ? N1C C2C C3C 120.7(5) . . ? N1C C2C C6B 114.3(4) . . ? C3C C2C C6B 124.9(5) . . ? C4C C3C C2C 119.4(5) . . ? C4C C3C H3C 120.3(3) . . ? C2C C3C H3C 120.3(3) . . ? C5C C4C C3C 119.2(5) . . ? C5C C4C H4C 120.4(3) . . ? C3C C4C H4C 120.4(3) . . ? C4C C5C C6C 120.1(5) . . ? C4C C5C H5C 120.0(3) . . ? C6C C5C H5C 120.0(3) . . ? N1C C6C C5C 123.2(5) . . ? N1C C6C H6C 118.4(3) . . ? C5C C6C H6C 118.4(3) . . ? O13 N10 O12 121.6(7) . . ? O13 N10 O11 119.6(6) . . ? O12 N10 O11 118.7(7) . . ? O22 N20 O23 119.4(6) . . ? O22 N20 O21 121.5(7) . . ? O23 N20 O21 119.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 O2 178.6(5) . . . . ? C1 N1 C2 O2 -2.3(7) . . . . ? C6 N1 C2 N3 0.1(8) . . . . ? C1 N1 C2 N3 179.2(5) . . . . ? O2 C2 N3 C4 -177.8(6) . . . . ? N1 C2 N3 C4 0.7(9) . . . . ? O2 C2 N3 Pd1 -0.3(7) . . . . ? N1 C2 N3 Pd1 178.3(4) . . . . ? N1B Pd1 N3 C4 150.2(62) . . . . ? N1C Pd1 N3 C4 -96.8(6) . . . . ? N1A Pd1 N3 C4 81.1(6) . . . . ? N1B Pd1 N3 C2 -27.1(70) . . . . ? N1C Pd1 N3 C2 85.9(5) . . . . ? N1A Pd1 N3 C2 -96.2(5) . . . . ? C2 N3 C4 N4 177.1(5) . . . . ? Pd1 N3 C4 N4 -0.1(9) . . . . ? C2 N3 C4 C5 -1.3(10) . . . . ? Pd1 N3 C4 C5 -178.5(5) . . . . ? N4 C4 C5 C6 -177.4(6) . . . . ? N3 C4 C5 C6 1.0(10) . . . . ? C2 N1 C6 C5 -0.4(9) . . . . ? C1 N1 C6 C5 -179.5(7) . . . . ? C4 C5 C6 N1 -0.1(11) . . . . ? N1B Pd1 N1A C6A 175.7(5) . . . . ? N1C Pd1 N1A C6A 165.7(6) . . . . ? N3 Pd1 N1A C6A -7.5(5) . . . . ? N1B Pd1 N1A C2A -1.2(4) . . . . ? N1C Pd1 N1A C2A -11.1(9) . . . . ? N3 Pd1 N1A C2A 175.6(4) . . . . ? C6A N1A C2A C3A 0.2(8) . . . . ? Pd1 N1A C2A C3A 177.4(4) . . . . ? C6A N1A C2A C2B -177.8(5) . . . . ? Pd1 N1A C2A C2B -0.6(5) . . . . ? N1A C2A C3A C4A -0.7(8) . . . . ? C2B C2A C3A C4A 177.0(5) . . . . ? C2A C3A C4A C5A -0.7(10) . . . . ? C3A C4A C5A C6A 2.6(9) . . . . ? C2A N1A C6A C5A 1.8(8) . . . . ? Pd1 N1A C6A C5A -174.9(4) . . . . ? C4A C5A C6A N1A -3.2(9) . . . . ? N1C Pd1 N1B C6B -3.2(4) . . . . ? N1A Pd1 N1B C6B 179.8(5) . . . . ? N3 Pd1 N1B C6B 110.3(65) . . . . ? N1C Pd1 N1B C2B 179.9(5) . . . . ? N1A Pd1 N1B C2B 2.9(4) . . . . ? N3 Pd1 N1B C2B -66.6(68) . . . . ? C6B N1B C2B C3B -1.4(9) . . . . ? Pd1 N1B C2B C3B 175.4(4) . . . . ? C6B N1B C2B C2A 179.3(5) . . . . ? Pd1 N1B C2B C2A -4.0(6) . . . . ? N1A C2A C2B N1B 2.9(7) . . . . ? C3A C2A C2B N1B -175.0(5) . . . . ? N1A C2A C2B C3B -176.4(5) . . . . ? C3A C2A C2B C3B 5.7(9) . . . . ? N1B C2B C3B C4B 0.9(8) . . . . ? C2A C2B C3B C4B -179.9(6) . . . . ? C2B C3B C4B C5B 0.6(10) . . . . ? C3B C4B C5B C6B -1.6(10) . . . . ? C2B N1B C6B C5B 0.3(9) . . . . ? Pd1 N1B C6B C5B -176.4(4) . . . . ? C2B N1B C6B C2C -179.6(5) . . . . ? Pd1 N1B C6B C2C 3.7(7) . . . . ? C4B C5B C6B N1B 1.1(9) . . . . ? C4B C5B C6B C2C -178.9(6) . . . . ? N1B Pd1 N1C C6C -177.8(5) . . . . ? N1A Pd1 N1C C6C -167.8(5) . . . . ? N3 Pd1 N1C C6C 5.4(5) . . . . ? N1B Pd1 N1C C2C 1.9(4) . . . . ? N1A Pd1 N1C C2C 12.0(9) . . . . ? N3 Pd1 N1C C2C -174.9(4) . . . . ? C6C N1C C2C C3C -0.4(8) . . . . ? Pd1 N1C C2C C3C 179.8(4) . . . . ? C6C N1C C2C C6B 179.2(5) . . . . ? Pd1 N1C C2C C6B -0.6(6) . . . . ? N1B C6B C2C N1C -1.8(7) . . . . ? C5B C6B C2C N1C 178.2(5) . . . . ? N1B C6B C2C C3C 177.7(5) . . . . ? C5B C6B C2C C3C -2.2(9) . . . . ? N1C C2C C3C C4C 2.2(8) . . . . ? C6B C2C C3C C4C -177.4(5) . . . . ? C2C C3C C4C C5C -1.9(9) . . . . ? C3C C4C C5C C6C 0.1(9) . . . . ? C2C N1C C6C C5C -1.6(8) . . . . ? Pd1 N1C C6C C5C 178.1(4) . . . . ? C4C C5C C6C N1C 1.8(9) . . . . ? _refine_diff_density_max 0.282 _refine_diff_density_min -0.274 _refine_diff_density_rms 0.060 #=END data_2b _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone 'Int. code + (231) 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Trans.' _publ_title ; Mono- and dinuclear complexes of (trpy)M(II) (M=Pd, Pt) with the model nucleobase 1-methylcytosine. Crystal structure and NMR solution studies. ; _publ_author_address ; Sultan Cosar, Matthias B. L. Janik, Matthias Flock, Eva Freisinger, and Bernhard Lippert Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany Etelka Farkas Department of Inorganic and Analytical Chemistry L. Kossuth University Debrecen Hungary ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H30 Cl3 N9 O14 Pd2' _chemical_formula_weight 1119.83 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.309(3) _cell_length_b 10.961(2) _cell_length_c 25.975(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.95(3) _cell_angle_gamma 90.00 _cell_volume 3999.8(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11271 _cell_measurement_theta_min 4.66 _cell_measurement_theta_max 23.81 _exptl_crystal_description cube _exptl_crystal_colour 'reddish brown' _exptl_crystal_size_max 0.463 _exptl_crystal_size_mid 0.275 _exptl_crystal_size_min 0.250 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method ? _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 1.181 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.6127 _exptl_absorpt_correction_T_max 0.7567 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 22s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11271 _diffrn_reflns_av_R_equivalents 0.0486 _diffrn_reflns_av_sigmaI/netI 0.0979 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 4.66 _diffrn_reflns_theta_max 23.81 _reflns_number_total 5838 _reflns_number_observed 2980 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'refU, except H4 refall' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00004(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5830 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1087 _refine_ls_R_factor_obs 0.0439 _refine_ls_wR_factor_all 0.1137 _refine_ls_wR_factor_obs 0.0954 _refine_ls_goodness_of_fit_all 0.864 _refine_ls_goodness_of_fit_obs 1.092 _refine_ls_restrained_S_all 0.898 _refine_ls_restrained_S_obs 1.092 _refine_ls_shift/esd_max 1.331 _refine_ls_shift/esd_mean 0.055 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pd1 Pd 0.31307(3) 0.56446(5) 0.43186(2) 0.0447(2) Uani 1 d . . Pd2 Pd 0.14409(4) 0.43169(6) 0.36692(2) 0.0555(2) Uani 1 d . . N1 N 0.1737(4) 0.7798(5) 0.5266(2) 0.0538(15) Uiso 1 d . . C1 C 0.2079(6) 0.8743(7) 0.5645(3) 0.081(3) Uani 1 d . . H1A H 0.2535(24) 0.9242(25) 0.5515(8) 0.095(5) Uiso 1 calc R . H1B H 0.2375(27) 0.8375(7) 0.5971(6) 0.095(5) Uiso 1 calc R . H1C H 0.1554(8) 0.9239(24) 0.5700(13) 0.095(5) Uiso 1 calc R . C2 C 0.2363(5) 0.7321(6) 0.4966(3) 0.049(2) Uiso 1 d . . O2 O 0.3167(3) 0.7742(4) 0.5013(2) 0.0659(14) Uani 1 d . . N3 N 0.2048(4) 0.6388(5) 0.4638(2) 0.0425(13) Uiso 1 d . . C4 C 0.1142(5) 0.5950(6) 0.4563(3) 0.052(2) Uiso 1 d . . N4 N 0.0864(5) 0.5052(6) 0.4239(2) 0.062(2) Uani 1 d . . H4 H 0.0339(47) 0.4822(60) 0.4263(25) 0.051(23) Uiso 1 d . . C5 C 0.0505(5) 0.6519(6) 0.4867(3) 0.055(2) Uiso 1 d . . H5 H -0.0125(5) 0.6267(6) 0.4829(3) 0.095(5) Uiso 1 calc R . C6 C 0.0834(5) 0.7387(6) 0.5194(2) 0.057(2) Uiso 1 d . . H6 H 0.0423(5) 0.7743(6) 0.5388(2) 0.095(5) Uiso 1 calc R . N11 N 0.3067(4) 0.6693(5) 0.3667(2) 0.0485(14) Uiso 1 d . . C11A C 0.2547(5) 0.7702(7) 0.3532(3) 0.055(2) Uiso 1 d . . H11A H 0.2153(5) 0.7980(7) 0.3754(3) 0.095(5) Uiso 1 calc R . C11B C 0.2575(5) 0.8344(7) 0.3078(3) 0.063(2) Uiso 1 d . . H11B H 0.2211(5) 0.9044(7) 0.2994(3) 0.095(5) Uiso 1 calc R . C11C C 0.3162(5) 0.7917(7) 0.2748(3) 0.062(2) Uiso 1 d . . H11C H 0.3178(5) 0.8315(7) 0.2433(3) 0.095(5) Uiso 1 calc R . C11D C 0.3718(5) 0.6909(7) 0.2887(3) 0.061(2) Uiso 1 d . . H11D H 0.4128(5) 0.6639(7) 0.2673(3) 0.095(5) Uiso 1 calc R . C11E C 0.3670(5) 0.6295(6) 0.3344(3) 0.051(2) Uiso 1 d . . N12 N 0.4107(4) 0.4831(5) 0.4011(2) 0.0481(14) Uiso 1 d . . C12A C 0.4229(5) 0.5215(6) 0.3536(2) 0.047(2) Uiso 1 d . . C12B C 0.4869(5) 0.4545(6) 0.3285(3) 0.059(2) Uiso 1 d . . H12B H 0.4976(5) 0.4768(6) 0.2956(3) 0.095(5) Uiso 1 calc R . C12C C 0.5321(5) 0.3560(7) 0.3546(3) 0.064(2) Uiso 1 d . . H12C H 0.5739(5) 0.3112(7) 0.3386(3) 0.095(5) Uiso 1 calc R . C12D C 0.5184(5) 0.3209(7) 0.4029(3) 0.061(2) Uiso 1 d . . H12D H 0.5507(5) 0.2543(7) 0.4200(3) 0.095(5) Uiso 1 calc R . C12E C 0.4551(5) 0.3873(6) 0.4260(3) 0.048(2) Uiso 1 d . . N13 N 0.3606(4) 0.4421(5) 0.4892(2) 0.0469(13) Uiso 1 d . . C13A C 0.4298(5) 0.3661(6) 0.4784(2) 0.051(2) Uiso 1 d . . C13B C 0.4708(5) 0.2791(7) 0.5132(3) 0.063(2) Uiso 1 d . . H13B H 0.5179(5) 0.2284(7) 0.5049(3) 0.095(5) Uiso 1 calc R . C13C C 0.4420(6) 0.2668(7) 0.5607(3) 0.074(2) Uiso 1 d . . H13C H 0.4682(6) 0.2071(7) 0.5846(3) 0.095(5) Uiso 1 calc R . C13D C 0.3742(5) 0.3445(7) 0.5717(3) 0.062(2) Uiso 1 d . . H13D H 0.3550(5) 0.3386(7) 0.6039(3) 0.095(5) Uiso 1 calc R . C13E C 0.3337(5) 0.4309(7) 0.5365(2) 0.054(2) Uiso 1 d . . H13E H 0.2873(5) 0.4826(7) 0.5449(2) 0.095(5) Uiso 1 calc R . N21 N 0.0981(4) 0.5567(6) 0.3110(2) 0.063(2) Uiso 1 d . . C21A C 0.0404(6) 0.6512(8) 0.3137(3) 0.077(2) Uiso 1 d . . H21A H 0.0165(6) 0.6634(8) 0.3441(3) 0.095(5) Uiso 1 calc R . C21B C 0.0157(6) 0.7307(9) 0.2726(4) 0.091(3) Uani 1 d . . H21B H -0.0245(6) 0.7961(9) 0.2753(4) 0.095(5) Uiso 1 calc R . C21C C 0.0501(8) 0.7133(11) 0.2282(4) 0.105(3) Uani 1 d . . H21C H 0.0353(8) 0.7681(11) 0.2005(4) 0.095(5) Uiso 1 calc R . C21D C 0.1066(7) 0.6156(10) 0.2242(3) 0.083(3) Uani 1 d . . H21D H 0.1288(7) 0.6023(10) 0.1933(3) 0.095(5) Uiso 1 calc R . C21E C 0.1315(5) 0.5356(7) 0.2657(3) 0.062(2) Uiso 1 d . . N22 N 0.2006(4) 0.3652(6) 0.3113(2) 0.057(2) Uiso 1 d . . C22A C 0.1911(5) 0.4273(8) 0.2668(3) 0.064(2) Uani 1 d . . C22B C 0.2338(7) 0.3812(10) 0.2265(3) 0.089(3) Uani 1 d . . H22B H 0.2278(7) 0.4218(10) 0.1946(3) 0.095(5) Uiso 1 calc R . C22C C 0.2841(8) 0.2760(12) 0.2353(5) 0.109(4) Uani 1 d . . H22C H 0.3128(8) 0.2449(12) 0.2088(5) 0.095(5) Uiso 1 calc R . C22D C 0.2944(6) 0.2132(9) 0.2822(5) 0.096(3) Uani 1 d . . H22D H 0.3284(6) 0.1405(9) 0.2875(5) 0.095(5) Uiso 1 calc R . C22E C 0.2513(5) 0.2636(8) 0.3214(4) 0.070(2) Uani 1 d . . N23 N 0.2030(4) 0.2808(6) 0.4029(3) 0.064(2) Uiso 1 d . . C23A C 0.2526(6) 0.2144(8) 0.3736(4) 0.071(2) Uani 1 d . . C23B C 0.2997(7) 0.1095(10) 0.3934(6) 0.100(3) Uani 1 d . . H23B H 0.3335(7) 0.0647(10) 0.3726(6) 0.095(5) Uiso 1 calc R . C23C C 0.2973(9) 0.0715(11) 0.4422(7) 0.126(5) Uani 1 d . . H23C H 0.3290(9) 0.0008(11) 0.4554(7) 0.095(5) Uiso 1 calc R . C23D C 0.2471(8) 0.1390(12) 0.4726(4) 0.106(4) Uani 1 d . . H23D H 0.2454(8) 0.1160(12) 0.5069(4) 0.095(5) Uiso 1 calc R . C23E C 0.1984(6) 0.2438(9) 0.4504(4) 0.081(3) Uani 1 d . . H23E H 0.1620(6) 0.2880(9) 0.4699(4) 0.095(5) Uiso 1 calc R . Cl1 Cl -0.0396(2) 0.4738(3) 0.11351(12) 0.0979(8) Uani 1 d . . O11 O 0.0480(5) 0.4138(7) 0.1329(3) 0.129(2) Uani 1 d . . O12 O -0.1030(5) 0.3995(7) 0.0819(3) 0.137(3) Uani 1 d . . O13 O -0.0879(6) 0.4935(9) 0.1614(3) 0.171(4) Uani 1 d . . O14 O -0.0238(5) 0.5875(8) 0.1006(3) 0.153(3) Uani 1 d . . Cl2 Cl -0.1827(2) 0.4683(2) 0.35292(9) 0.0857(7) Uani 1 d . . O21 O -0.1452(8) 0.5224(12) 0.4027(5) 0.102(4) Uiso 0.60 d P . O21A O -0.1547(19) 0.5864(25) 0.3815(11) 0.185(11) Uiso 0.40 d P . O22A O -0.1291(12) 0.4746(16) 0.3139(7) 0.142(2) Uiso 0.50 d P . O23A O -0.1033(13) 0.3788(16) 0.3614(6) 0.142(2) Uiso 0.50 d P . O22 O -0.1816(13) 0.5197(16) 0.3040(7) 0.142(2) Uiso 0.50 d P . O23 O -0.2059(13) 0.3397(16) 0.3564(6) 0.142(2) Uiso 0.50 d P . O24 O -0.2797(12) 0.5137(16) 0.3317(6) 0.142(2) Uiso 0.50 d P . O24A O -0.2609(13) 0.4139(17) 0.3651(6) 0.142(2) Uiso 0.50 d P . Cl3 Cl 0.5441(2) 0.9943(2) 0.33299(9) 0.0776(7) Uani 1 d . . O31 O 0.4734(6) 1.0398(8) 0.2911(3) 0.148(3) Uani 1 d . . O32 O 0.6239(11) 1.0739(14) 0.3273(6) 0.092(4) Uani 0.60 d P 1 O33 O 0.5256(9) 1.0231(10) 0.3840(4) 0.077(3) Uani 0.60 d P 1 O34 O 0.5700(15) 0.8698(15) 0.3330(7) 0.115(7) Uani 0.60 d P 1 O32A O 0.6310(35) 1.0347(38) 0.3430(15) 0.188(20) Uiso 0.40 d P 2 O33A O 0.4827(15) 0.9843(20) 0.3705(8) 0.101(8) Uiso 0.40 d P 2 O34A O 0.5486(25) 0.8807(32) 0.3126(11) 0.117(12) Uiso 0.40 d P 2 O1W O 0.1677(6) 0.2865(9) 0.0758(3) 0.186(4) Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd1 0.0416(3) 0.0493(4) 0.0458(3) 0.0002(3) 0.0153(2) 0.0021(3) Pd2 0.0517(4) 0.0590(4) 0.0580(4) -0.0083(3) 0.0162(3) -0.0043(3) C1 0.099(7) 0.079(6) 0.072(5) -0.030(5) 0.037(5) -0.004(5) O2 0.050(3) 0.070(4) 0.079(3) -0.022(3) 0.019(3) -0.007(3) N4 0.045(4) 0.080(5) 0.066(4) -0.014(4) 0.022(4) -0.013(4) C21B 0.093(7) 0.077(7) 0.099(7) 0.010(6) 0.006(6) 0.009(5) C21C 0.125(10) 0.099(9) 0.078(7) 0.026(7) -0.015(7) -0.017(8) C21D 0.091(7) 0.086(7) 0.070(6) -0.007(5) 0.014(5) -0.023(6) C22A 0.060(5) 0.076(6) 0.060(5) -0.027(5) 0.017(4) -0.020(5) C22B 0.086(7) 0.115(9) 0.074(6) -0.028(6) 0.038(6) -0.032(6) C22C 0.092(8) 0.118(10) 0.136(10) -0.061(8) 0.070(8) -0.021(7) C22D 0.074(7) 0.077(7) 0.148(10) -0.033(7) 0.044(7) -0.002(5) C22E 0.051(5) 0.059(6) 0.102(7) -0.026(5) 0.019(5) -0.008(4) C23A 0.055(5) 0.048(6) 0.108(7) 0.002(5) 0.008(5) -0.008(5) C23B 0.077(7) 0.061(8) 0.156(11) -0.017(7) 0.004(7) -0.007(6) C23C 0.114(10) 0.069(8) 0.172(13) 0.035(9) -0.028(9) 0.005(8) C23D 0.097(9) 0.104(10) 0.110(9) 0.027(8) 0.001(7) -0.035(7) C23E 0.068(6) 0.063(7) 0.105(7) 0.007(5) -0.001(5) -0.019(5) Cl1 0.074(2) 0.080(2) 0.130(2) 0.004(2) -0.004(2) -0.009(2) O11 0.102(5) 0.136(7) 0.137(6) -0.010(5) -0.005(4) 0.040(5) O12 0.115(6) 0.134(7) 0.150(6) -0.057(5) 0.000(5) -0.032(5) O13 0.142(7) 0.213(9) 0.178(8) -0.007(7) 0.080(7) 0.008(7) O14 0.118(6) 0.135(7) 0.202(8) 0.085(6) 0.017(5) -0.025(5) Cl2 0.080(2) 0.096(2) 0.087(2) -0.0141(14) 0.0297(13) -0.0139(14) Cl3 0.090(2) 0.076(2) 0.072(2) 0.0051(13) 0.0293(15) 0.0107(15) O31 0.136(6) 0.212(9) 0.096(5) 0.021(5) 0.022(5) 0.060(6) O32 0.100(9) 0.082(10) 0.095(8) 0.010(8) 0.019(7) -0.047(7) O33 0.099(9) 0.073(8) 0.067(7) -0.009(5) 0.031(7) -0.005(7) O34 0.192(17) 0.070(9) 0.107(13) 0.031(9) 0.093(13) 0.037(9) _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 N12 1.951(5) . ? Pd1 N13 2.024(5) . ? Pd1 N11 2.033(5) . ? Pd1 N3 2.059(5) . ? Pd1 Pd2 3.0431(11) . ? Pd2 N22 1.928(6) . ? Pd2 N4 1.996(6) . ? Pd2 N23 2.005(7) . ? Pd2 N21 2.014(6) . ? N1 C6 1.348(8) . ? N1 C2 1.395(7) . ? N1 C1 1.448(8) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 O2 1.225(7) . ? C2 N3 1.352(8) . ? N3 C4 1.362(8) . ? C4 N4 1.308(8) . ? C4 C5 1.455(8) . ? N4 H4 0.81(6) . ? C5 C6 1.301(9) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? N11 C11A 1.342(8) . ? N11 C11E 1.384(7) . ? C11A C11B 1.383(9) . ? C11A H11A 0.93 . ? C11B C11C 1.390(8) . ? C11B H11B 0.93 . ? C11C C11D 1.369(9) . ? C11C H11C 0.93 . ? C11D C11E 1.376(8) . ? C11D H11D 0.93 . ? C11E C12A 1.462(9) . ? N12 C12E 1.330(7) . ? N12 C12A 1.345(7) . ? C12A C12B 1.425(8) . ? C12B C12C 1.370(9) . ? C12B H12B 0.93 . ? C12C C12D 1.363(9) . ? C12C H12C 0.93 . ? C12D C12E 1.383(8) . ? C12D H12D 0.93 . ? C12E C13A 1.491(8) . ? N13 C13E 1.361(7) . ? N13 C13A 1.364(7) . ? C13A C13B 1.368(9) . ? C13B C13C 1.380(9) . ? C13B H13B 0.93 . ? C13C C13D 1.361(9) . ? C13C H13C 0.93 . ? C13D C13E 1.367(9) . ? C13D H13D 0.93 . ? C13E H13E 0.93 . ? N21 C21A 1.334(9) . ? N21 C21E 1.371(8) . ? C21A C21B 1.370(11) . ? C21A H21A 0.93 . ? C21B C21C 1.352(12) . ? C21B H21B 0.93 . ? C21C C21D 1.357(12) . ? C21C H21C 0.93 . ? C21D C21E 1.382(11) . ? C21D H21D 0.93 . ? C21E C22A 1.458(10) . ? N22 C22A 1.324(8) . ? N22 C22E 1.329(9) . ? C22A C22B 1.404(10) . ? C22B C22C 1.355(13) . ? C22B H22B 0.93 . ? C22C C22D 1.384(13) . ? C22C H22C 0.93 . ? C22D C22E 1.400(11) . ? C22D H22D 0.93 . ? C22E C23A 1.456(10) . ? N23 C23E 1.312(9) . ? N23 C23A 1.347(9) . ? C23A C23B 1.381(12) . ? C23B C23C 1.342(14) . ? C23B H23B 0.93 . ? C23C C23D 1.379(14) . ? C23C H23C 0.93 . ? C23D C23E 1.409(13) . ? C23D H23D 0.93 . ? C23E H23E 0.93 . ? Cl1 O14 1.321(7) . ? Cl1 O12 1.370(7) . ? Cl1 O11 1.421(7) . ? Cl1 O13 1.547(7) . ? Cl2 O24A 1.36(2) . ? Cl2 O22A 1.38(2) . ? Cl2 O22 1.39(2) . ? Cl2 O21 1.431(12) . ? Cl2 O23 1.45(2) . ? Cl2 O23A 1.49(2) . ? Cl2 O21A 1.51(3) . ? Cl2 O24 1.48(2) . ? O21 O21A 0.89(3) . ? O22A O22 0.89(2) . ? O22A O23A 1.61(2) . ? O23A O23 1.51(2) . ? O22 O24 1.70(2) . ? O23 O24A 1.18(2) . ? O24 O24A 1.39(2) . ? Cl3 O32A 1.30(5) . ? Cl3 O34A 1.36(4) . ? Cl3 O34 1.41(2) . ? Cl3 O31 1.427(7) . ? Cl3 O33 1.436(9) . ? Cl3 O33A 1.44(2) . ? Cl3 O32 1.467(13) . ? 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 N12 Pd1 N13 80.3(2) . . ? N12 Pd1 N11 80.7(2) . . ? N13 Pd1 N11 160.5(2) . . ? N12 Pd1 N3 176.0(2) . . ? N13 Pd1 N3 98.0(2) . . ? N11 Pd1 N3 101.2(2) . . ? N12 Pd1 Pd2 96.3(2) . . ? N13 Pd1 Pd2 102.21(15) . . ? N11 Pd1 Pd2 84.5(2) . . ? N3 Pd1 Pd2 80.41(15) . . ? N22 Pd2 N4 178.4(3) . . ? N22 Pd2 N23 80.7(3) . . ? N4 Pd2 N23 100.6(3) . . ? N22 Pd2 N21 80.9(3) . . ? N4 Pd2 N21 97.8(3) . . ? N23 Pd2 N21 161.5(2) . . ? N22 Pd2 Pd1 101.2(2) . . ? N4 Pd2 Pd1 78.1(2) . . ? N23 Pd2 Pd1 85.2(2) . . ? N21 Pd2 Pd1 101.0(2) . . ? C6 N1 C2 119.8(6) . . ? C6 N1 C1 121.7(6) . . ? C2 N1 C1 118.6(6) . . ? N1 C1 H1A 109.4(4) . . ? N1 C1 H1B 109.5(4) . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5(4) . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 N3 122.8(6) . . ? O2 C2 N1 119.6(6) . . ? N3 C2 N1 117.6(6) . . ? C2 N3 C4 123.4(6) . . ? C2 N3 Pd1 111.6(4) . . ? C4 N3 Pd1 124.9(4) . . ? N4 C4 N3 121.5(6) . . ? N4 C4 C5 121.8(7) . . ? N3 C4 C5 116.7(6) . . ? C4 N4 Pd2 131.6(5) . . ? C4 N4 H4 110.9(48) . . ? Pd2 N4 H4 117.1(48) . . ? C6 C5 C4 118.8(7) . . ? C6 C5 H5 120.6(4) . . ? C4 C5 H5 120.6(4) . . ? C5 C6 N1 123.6(7) . . ? C5 C6 H6 118.2(4) . . ? N1 C6 H6 118.2(4) . . ? C11A N11 C11E 118.7(6) . . ? C11A N11 Pd1 128.1(4) . . ? C11E N11 Pd1 113.1(4) . . ? N11 C11A C11B 122.5(6) . . ? N11 C11A H11A 118.8(4) . . ? C11B C11A H11A 118.7(4) . . ? C11C C11B C11A 118.3(7) . . ? C11C C11B H11B 120.8(5) . . ? C11A C11B H11B 120.9(4) . . ? C11D C11C C11B 119.9(7) . . ? C11D C11C H11C 120.1(4) . . ? C11B C11C H11C 120.1(5) . . ? C11C C11D C11E 120.1(6) . . ? C11C C11D H11D 120.0(4) . . ? C11E C11D H11D 120.0(4) . . ? C11D C11E N11 120.5(6) . . ? C11D C11E C12A 125.3(6) . . ? N11 C11E C12A 114.3(6) . . ? C12E N12 C12A 124.0(5) . . ? C12E N12 Pd1 118.3(4) . . ? C12A N12 Pd1 117.4(4) . . ? N12 C12A C12B 117.7(6) . . ? N12 C12A C11E 114.1(5) . . ? C12B C12A C11E 128.1(6) . . ? C12C C12B C12A 117.7(6) . . ? C12C C12B H12B 121.2(4) . . ? C12A C12B H12B 121.2(4) . . ? C12D C12C C12B 122.7(7) . . ? C12D C12C H12C 118.6(5) . . ? C12B C12C H12C 118.6(4) . . ? C12C C12D C12E 118.1(7) . . ? C12C C12D H12D 120.9(5) . . ? C12E C12D H12D 120.9(4) . . ? N12 C12E C12D 119.8(6) . . ? N12 C12E C13A 113.0(6) . . ? C12D C12E C13A 127.2(6) . . ? C13E N13 C13A 118.2(6) . . ? C13E N13 Pd1 127.7(5) . . ? C13A N13 Pd1 114.1(4) . . ? C13B C13A N13 121.7(6) . . ? C13B C13A C12E 124.4(6) . . ? N13 C13A C12E 113.9(6) . . ? C13A C13B C13C 119.8(7) . . ? C13A C13B H13B 120.1(4) . . ? C13C C13B H13B 120.1(5) . . ? C13D C13C C13B 118.2(8) . . ? C13D C13C H13C 120.9(5) . . ? C13B C13C H13C 120.9(5) . . ? C13C C13D C13E 121.4(7) . . ? C13C C13D H13D 119.3(5) . . ? C13E C13D H13D 119.3(4) . . ? N13 C13E C13D 120.6(7) . . ? N13 C13E H13E 119.7(4) . . ? C13D C13E H13E 119.7(4) . . ? C21A N21 C21E 119.7(7) . . ? C21A N21 Pd2 127.7(5) . . ? C21E N21 Pd2 112.6(5) . . ? N21 C21A C21B 121.6(8) . . ? N21 C21A H21A 119.2(5) . . ? C21B C21A H21A 119.2(6) . . ? C21C C21B C21A 119.5(9) . . ? C21C C21B H21B 120.2(7) . . ? C21A C21B H21B 120.3(6) . . ? C21B C21C C21D 119.6(10) . . ? C21B C21C H21C 120.2(7) . . ? C21D C21C H21C 120.2(6) . . ? C21C C21D C21E 120.7(9) . . ? C21C C21D H21D 119.6(6) . . ? C21E C21D H21D 119.7(5) . . ? N21 C21E C21D 118.8(8) . . ? N21 C21E C22A 114.7(7) . . ? C21D C21E C22A 126.5(8) . . ? C22A N22 C22E 124.4(7) . . ? C22A N22 Pd2 118.1(5) . . ? C22E N22 Pd2 117.3(5) . . ? N22 C22A C22B 118.6(8) . . ? N22 C22A C21E 113.5(6) . . ? C22B C22A C21E 127.9(8) . . ? C22C C22B C22A 118.2(9) . . ? C22C C22B H22B 120.9(6) . . ? C22A C22B H22B 120.9(6) . . ? C22B C22C C22D 122.4(9) . . ? C22B C22C H22C 118.8(6) . . ? C22D C22C H22C 118.8(6) . . ? C22C C22D C22E 117.2(10) . . ? C22C C22D H22D 121.4(6) . . ? C22E C22D H22D 121.4(6) . . ? N22 C22E C22D 119.1(9) . . ? N22 C22E C23A 113.9(7) . . ? C22D C22E C23A 127.0(9) . . ? C23E N23 C23A 119.3(8) . . ? C23E N23 Pd2 127.0(6) . . ? C23A N23 Pd2 113.7(6) . . ? N23 C23A C23B 120.8(9) . . ? N23 C23A C22E 114.2(8) . . ? C23B C23A C22E 125.0(9) . . ? C23C C23B C23A 120.8(11) . . ? C23C C23B H23B 119.6(8) . . ? C23A C23B H23B 119.6(7) . . ? C23B C23C C23D 118.9(12) . . ? C23B C23C H23C 120.5(8) . . ? C23D C23C H23C 120.5(8) . . ? C23C C23D C23E 118.3(11) . . ? C23C C23D H23D 120.9(8) . . ? C23E C23D H23D 120.8(7) . . ? N23 C23E C23D 121.9(9) . . ? N23 C23E H23E 119.0(5) . . ? C23D C23E H23E 119.1(7) . . ? O14 Cl1 O12 122.3(6) . . ? O14 Cl1 O11 110.1(5) . . ? O12 Cl1 O11 112.1(5) . . ? O14 Cl1 O13 101.4(6) . . ? O12 Cl1 O13 102.6(5) . . ? O11 Cl1 O13 106.1(5) . . ? O24A Cl2 O22A 142.0(10) . . ? O24A Cl2 O22 122.9(11) . . ? O22A Cl2 O22 37.6(9) . . ? O24A Cl2 O21 99.0(8) . . ? O22A Cl2 O21 118.4(9) . . ? O22 Cl2 O21 126.1(9) . . ? O24A Cl2 O23 49.6(8) . . ? O22A Cl2 O23 105.0(10) . . ? O22 Cl2 O23 119.4(10) . . ? O21 Cl2 O23 113.3(8) . . ? O24A Cl2 O23A 108.4(10) . . ? O22A Cl2 O23A 68.2(8) . . ? O22 Cl2 O23A 105.2(9) . . ? O21 Cl2 O23A 89.7(8) . . ? O23 Cl2 O23A 61.8(8) . . ? O24A Cl2 O21A 114.7(12) . . ? O22A Cl2 O21A 100.6(12) . . ? O22 Cl2 O21A 93.0(13) . . ? O21 Cl2 O21A 35.0(10) . . ? O23 Cl2 O21A 147.6(13) . . ? O23A Cl2 O21A 111.7(12) . . ? O24A Cl2 O24 58.5(8) . . ? O22A Cl2 O24 108.7(10) . . ? O22 Cl2 O24 72.3(9) . . ? O21 Cl2 O24 111.2(8) . . ? O23 Cl2 O24 98.0(10) . . ? O23A Cl2 O24 156.2(9) . . ? O21A Cl2 O24 92.2(12) . . ? O21A O21 Cl2 77.2(21) . . ? O21 O21A Cl2 67.8(20) . . ? O22 O22A Cl2 71.7(18) . . ? O22 O22A O23A 129.6(23) . . ? Cl2 O22A O23A 58.9(9) . . ? Cl2 O23A O23 58.1(9) . . ? Cl2 O23A O22A 52.9(8) . . ? O23 O23A O22A 92.3(13) . . ? O22A O22 Cl2 70.7(18) . . ? O22A O22 O24 125.1(24) . . ? Cl2 O22 O24 56.2(9) . . ? O24A O23 Cl2 60.9(12) . . ? O24A O23 O23A 117.4(18) . . ? Cl2 O23 O23A 60.1(10) . . ? O24A O24 Cl2 56.4(10) . . ? O24A O24 O22 102.5(15) . . ? Cl2 O24 O22 51.5(8) . . ? O23 O24A O24 118.6(18) . . ? O23 O24A Cl2 69.5(13) . . ? O24 O24A Cl2 65.1(11) . . ? O32A Cl3 O34A 106.1(25) . . ? O32A Cl3 O31 123.1(16) . . ? O34A Cl3 O31 95.9(13) . . ? O34 Cl3 O31 119.1(10) . . ? O34 Cl3 O33 107.8(8) . . ? O31 Cl3 O33 113.4(6) . . ? O32A Cl3 O33A 125.2(19) . . ? O34A Cl3 O33A 106.0(16) . . ? O31 Cl3 O33A 96.2(9) . . ? O34 Cl3 O32 111.4(10) . . ? O31 Cl3 O32 99.6(8) . . ? O33 Cl3 O32 104.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N12 Pd1 Pd2 N22 -16.4(3) . . . . ? N13 Pd1 Pd2 N22 -97.8(2) . . . . ? N11 Pd1 Pd2 N22 63.7(2) . . . . ? N3 Pd1 Pd2 N22 166.0(2) . . . . ? N12 Pd1 Pd2 N4 165.1(3) . . . . ? N13 Pd1 Pd2 N4 83.6(2) . . . . ? N11 Pd1 Pd2 N4 -114.9(3) . . . . ? N3 Pd1 Pd2 N4 -12.5(2) . . . . ? N12 Pd1 Pd2 N23 63.2(2) . . . . ? N13 Pd1 Pd2 N23 -18.3(2) . . . . ? N11 Pd1 Pd2 N23 143.2(2) . . . . ? N3 Pd1 Pd2 N23 -114.5(2) . . . . ? N12 Pd1 Pd2 N21 -99.2(2) . . . . ? N13 Pd1 Pd2 N21 179.4(2) . . . . ? N11 Pd1 Pd2 N21 -19.1(2) . . . . ? N3 Pd1 Pd2 N21 83.2(2) . . . . ? C6 N1 C2 O2 176.1(6) . . . . ? C1 N1 C2 O2 -3.1(10) . . . . ? C6 N1 C2 N3 -4.8(9) . . . . ? C1 N1 C2 N3 176.0(6) . . . . ? O2 C2 N3 C4 -176.7(6) . . . . ? N1 C2 N3 C4 4.2(9) . . . . ? O2 C2 N3 Pd1 7.8(8) . . . . ? N1 C2 N3 Pd1 -171.3(4) . . . . ? N12 Pd1 N3 C2 152.9(28) . . . . ? N13 Pd1 N3 C2 87.6(4) . . . . ? N11 Pd1 N3 C2 -89.0(4) . . . . ? Pd2 Pd1 N3 C2 -171.3(4) . . . . ? N12 Pd1 N3 C4 -22.5(32) . . . . ? N13 Pd1 N3 C4 -87.8(5) . . . . ? N11 Pd1 N3 C4 95.6(5) . . . . ? Pd2 Pd1 N3 C4 13.3(5) . . . . ? C2 N3 C4 N4 179.5(6) . . . . ? Pd1 N3 C4 N4 -5.7(9) . . . . ? C2 N3 C4 C5 -1.4(9) . . . . ? Pd1 N3 C4 C5 173.5(4) . . . . ? N3 C4 N4 Pd2 -15.4(11) . . . . ? C5 C4 N4 Pd2 165.5(5) . . . . ? N22 Pd2 N4 C4 -43.9(99) . . . . ? N23 Pd2 N4 C4 101.7(7) . . . . ? N21 Pd2 N4 C4 -80.7(7) . . . . ? Pd1 Pd2 N4 C4 19.0(7) . . . . ? N4 C4 C5 C6 178.2(7) . . . . ? N3 C4 C5 C6 -1.0(9) . . . . ? C4 C5 C6 N1 0.3(10) . . . . ? C2 N1 C6 C5 2.6(10) . . . . ? C1 N1 C6 C5 -178.2(7) . . . . ? N12 Pd1 N11 C11A -175.1(6) . . . . ? N13 Pd1 N11 C11A -161.1(6) . . . . ? N3 Pd1 N11 C11A 8.5(6) . . . . ? Pd2 Pd1 N11 C11A 87.6(5) . . . . ? N12 Pd1 N11 C11E 2.8(4) . . . . ? N13 Pd1 N11 C11E 16.8(9) . . . . ? N3 Pd1 N11 C11E -173.6(4) . . . . ? Pd2 Pd1 N11 C11E -94.5(4) . . . . ? C11E N11 C11A C11B 1.5(10) . . . . ? Pd1 N11 C11A C11B 179.3(5) . . . . ? N11 C11A C11B C11C 0.4(11) . . . . ? C11A C11B C11C C11D -2.3(11) . . . . ? C11B C11C C11D C11E 2.3(11) . . . . ? C11C C11D C11E N11 -0.4(11) . . . . ? C11C C11D C11E C12A -179.6(7) . . . . ? C11A N11 C11E C11D -1.5(10) . . . . ? Pd1 N11 C11E C11D -179.6(5) . . . . ? C11A N11 C11E C12A 177.8(6) . . . . ? Pd1 N11 C11E C12A -0.3(7) . . . . ? N13 Pd1 N12 C12E 5.1(5) . . . . ? N11 Pd1 N12 C12E -179.6(5) . . . . ? N3 Pd1 N12 C12E -60.8(31) . . . . ? Pd2 Pd1 N12 C12E -96.2(5) . . . . ? N13 Pd1 N12 C12A 179.5(5) . . . . ? N11 Pd1 N12 C12A -5.2(5) . . . . ? N3 Pd1 N12 C12A 113.6(29) . . . . ? Pd2 Pd1 N12 C12A 78.2(5) . . . . ? C12E N12 C12A C12B 0.5(10) . . . . ? Pd1 N12 C12A C12B -173.6(5) . . . . ? C12E N12 C12A C11E -179.6(6) . . . . ? Pd1 N12 C12A C11E 6.4(7) . . . . ? C11D C11E C12A N12 175.5(7) . . . . ? N11 C11E C12A N12 -3.8(8) . . . . ? C11D C11E C12A C12B -4.6(11) . . . . ? N11 C11E C12A C12B 176.2(6) . . . . ? N12 C12A C12B C12C -0.5(10) . . . . ? C11E C12A C12B C12C 179.6(7) . . . . ? C12A C12B C12C C12D -0.2(11) . . . . ? C12B C12C C12D C12E 0.9(11) . . . . ? C12A N12 C12E C12D 0.2(10) . . . . ? Pd1 N12 C12E C12D 174.2(5) . . . . ? C12A N12 C12E C13A 179.0(6) . . . . ? Pd1 N12 C12E C13A -7.0(7) . . . . ? C12C C12D C12E N12 -0.9(10) . . . . ? C12C C12D C12E C13A -179.4(7) . . . . ? N12 Pd1 N13 C13E 175.8(6) . . . . ? N11 Pd1 N13 C13E 161.8(6) . . . . ? N3 Pd1 N13 C13E -7.9(6) . . . . ? Pd2 Pd1 N13 C13E -89.8(5) . . . . ? N12 Pd1 N13 C13A -1.9(4) . . . . ? N11 Pd1 N13 C13A -15.9(9) . . . . ? N3 Pd1 N13 C13A 174.4(4) . . . . ? Pd2 Pd1 N13 C13A 92.5(4) . . . . ? C13E N13 C13A C13B 1.1(10) . . . . ? Pd1 N13 C13A C13B 179.0(5) . . . . ? C13E N13 C13A C12E -179.1(6) . . . . ? Pd1 N13 C13A C12E -1.1(7) . . . . ? N12 C12E C13A C13B -175.0(7) . . . . ? C12D C12E C13A C13B 3.6(11) . . . . ? N12 C12E C13A N13 5.1(8) . . . . ? C12D C12E C13A N13 -176.2(7) . . . . ? N13 C13A C13B C13C 0.0(11) . . . . ? C12E C13A C13B C13C -179.8(7) . . . . ? C13A C13B C13C C13D -1.3(11) . . . . ? C13B C13C C13D C13E 1.4(11) . . . . ? C13A N13 C13E C13D -1.0(10) . . . . ? Pd1 N13 C13E C13D -178.6(5) . . . . ? C13C C13D C13E N13 -0.3(11) . . . . ? N22 Pd2 N21 C21A 176.4(7) . . . . ? N4 Pd2 N21 C21A -4.6(7) . . . . ? N23 Pd2 N21 C21A 167.9(7) . . . . ? Pd1 Pd2 N21 C21A -83.9(6) . . . . ? N22 Pd2 N21 C21E -2.6(5) . . . . ? N4 Pd2 N21 C21E 176.4(5) . . . . ? N23 Pd2 N21 C21E -11.0(11) . . . . ? Pd1 Pd2 N21 C21E 97.1(5) . . . . ? C21E N21 C21A C21B -2.0(12) . . . . ? Pd2 N21 C21A C21B 179.1(6) . . . . ? N21 C21A C21B C21C 0.1(14) . . . . ? C21A C21B C21C C21D 1.8(15) . . . . ? C21B C21C C21D C21E -1.9(15) . . . . ? C21A N21 C21E C21D 1.9(11) . . . . ? Pd2 N21 C21E C21D -179.1(6) . . . . ? C21A N21 C21E C22A -177.9(7) . . . . ? Pd2 N21 C21E C22A 1.2(8) . . . . ? C21C C21D C21E N21 0.1(13) . . . . ? C21C C21D C21E C22A 179.8(8) . . . . ? N4 Pd2 N22 C22A -33.0(98) . . . . ? N23 Pd2 N22 C22A -178.8(6) . . . . ? N21 Pd2 N22 C22A 3.9(5) . . . . ? Pd1 Pd2 N22 C22A -95.6(5) . . . . ? N4 Pd2 N22 C22E 143.0(94) . . . . ? N23 Pd2 N22 C22E -2.7(5) . . . . ? N21 Pd2 N22 C22E 180.0(6) . . . . ? Pd1 Pd2 N22 C22E 80.4(5) . . . . ? C22E N22 C22A C22B 2.8(11) . . . . ? Pd2 N22 C22A C22B 178.5(5) . . . . ? C22E N22 C22A C21E 180.0(7) . . . . ? Pd2 N22 C22A C21E -4.3(8) . . . . ? N21 C21E C22A N22 1.9(9) . . . . ? C21D C21E C22A N22 -177.9(8) . . . . ? N21 C21E C22A C22B 178.7(7) . . . . ? C21D C21E C22A C22B -1.0(13) . . . . ? N22 C22A C22B C22C -1.0(12) . . . . ? C21E C22A C22B C22C -177.7(8) . . . . ? C22A C22B C22C C22D 0.2(15) . . . . ? C22B C22C C22D C22E -0.8(15) . . . . ? C22A N22 C22E C22D -3.5(11) . . . . ? Pd2 N22 C22E C22D -179.3(6) . . . . ? C22A N22 C22E C23A 178.4(7) . . . . ? Pd2 N22 C22E C23A 2.7(9) . . . . ? C22C C22D C22E N22 2.4(12) . . . . ? C22C C22D C22E C23A -179.9(8) . . . . ? N22 Pd2 N23 C23E -178.4(7) . . . . ? N4 Pd2 N23 C23E 2.5(7) . . . . ? N21 Pd2 N23 C23E -170.0(7) . . . . ? Pd1 Pd2 N23 C23E 79.4(6) . . . . ? N22 Pd2 N23 C23A 2.3(5) . . . . ? N4 Pd2 N23 C23A -176.8(5) . . . . ? N21 Pd2 N23 C23A 10.7(11) . . . . ? Pd1 Pd2 N23 C23A -99.9(5) . . . . ? C23E N23 C23A C23B -1.2(12) . . . . ? Pd2 N23 C23A C23B 178.2(6) . . . . ? C23E N23 C23A C22E 179.1(7) . . . . ? Pd2 N23 C23A C22E -1.5(8) . . . . ? N22 C22E C23A N23 -0.7(10) . . . . ? C22D C22E C23A N23 -178.5(8) . . . . ? N22 C22E C23A C23B 179.6(8) . . . . ? C22D C22E C23A C23B 1.8(13) . . . . ? N23 C23A C23B C23C -0.1(14) . . . . ? C22E C23A C23B C23C 179.6(9) . . . . ? C23A C23B C23C C23D -0.1(17) . . . . ? C23B C23C C23D C23E 1.5(16) . . . . ? C23A N23 C23E C23D 2.7(12) . . . . ? Pd2 N23 C23E C23D -176.6(6) . . . . ? C23C C23D C23E N23 -2.9(14) . . . . ? O24A Cl2 O21 O21A -120.7(22) . . . . ? O22A Cl2 O21 O21A 65.9(23) . . . . ? O22 Cl2 O21 O21A 22.0(24) . . . . ? O23 Cl2 O21 O21A -170.4(21) . . . . ? O23A Cl2 O21 O21A 130.7(21) . . . . ? O21A Cl2 O21 O21A 0.000(12) . . . . ? O24 Cl2 O21 O21A -61.1(22) . . . . ? Cl2 O21 O21A Cl2 0.000(7) . . . . ? O24A Cl2 O21A O21 69.2(22) . . . . ? O22A Cl2 O21A O21 -125.2(19) . . . . ? O22 Cl2 O21A O21 -162.4(19) . . . . ? O21 Cl2 O21A O21 0.000(13) . . . . ? O23 Cl2 O21A O21 16.6(36) . . . . ? O23A Cl2 O21A O21 -54.7(21) . . . . ? O24 Cl2 O21A O21 125.2(19) . . . . ? O24A Cl2 O22A O22 77.4(26) . . . . ? O22 Cl2 O22A O22 0.000(8) . . . . ? O21 Cl2 O22A O22 -113.2(18) . . . . ? O23 Cl2 O22A O22 119.0(19) . . . . ? O23A Cl2 O22A O22 169.7(22) . . . . ? O21A Cl2 O22A O22 -81.0(21) . . . . ? O24 Cl2 O22A O22 14.9(21) . . . . ? O24A Cl2 O22A O23A -92.3(19) . . . . ? O22 Cl2 O22A O23A -169.7(22) . . . . ? O21 Cl2 O22A O23A 77.0(11) . . . . ? O23 Cl2 O22A O23A -50.7(10) . . . . ? O23A Cl2 O22A O23A 0.000(7) . . . . ? O21A Cl2 O22A O23A 109.2(13) . . . . ? O24 Cl2 O22A O23A -154.8(10) . . . . ? O24A Cl2 O23A O23 17.5(12) . . . . ? O22A Cl2 O23A O23 -122.1(12) . . . . ? O22 Cl2 O23A O23 -115.6(11) . . . . ? O21 Cl2 O23A O23 116.9(9) . . . . ? O23 Cl2 O23A O23 0.0 . . . . ? O21A Cl2 O23A O23 144.8(14) . . . . ? O24 Cl2 O23A O23 -35.0(23) . . . . ? O24A Cl2 O23A O22A 139.6(11) . . . . ? O22A Cl2 O23A O22A 0.000(7) . . . . ? O22 Cl2 O23A O22A 6.5(14) . . . . ? O21 Cl2 O23A O22A -121.0(10) . . . . ? O23 Cl2 O23A O22A 122.1(12) . . . . ? O21A Cl2 O23A O22A -93.1(14) . . . . ? O24 Cl2 O23A O22A 87.1(22) . . . . ? O22 O22A O23A Cl2 -12.7(27) . . . . ? Cl2 O22A O23A Cl2 0.000(9) . . . . ? O22 O22A O23A O23 33.4(32) . . . . ? Cl2 O22A O23A O23 46.0(9) . . . . ? Cl2 O22A O22 Cl2 0.000(6) . . . . ? O23A O22A O22 Cl2 11.4(24) . . . . ? Cl2 O22A O22 O24 -15.1(21) . . . . ? O23A O22A O22 O24 -3.7(43) . . . . ? O24A Cl2 O22 O22A -134.4(19) . . . . ? O22A Cl2 O22 O22A 0.000(8) . . . . ? O21 Cl2 O22 O22A 91.1(19) . . . . ? O23 Cl2 O22 O22A -75.8(21) . . . . ? O23A Cl2 O22 O22A -9.9(21) . . . . ? O21A Cl2 O22 O22A 103.5(21) . . . . ? O24 Cl2 O22 O22A -165.2(21) . . . . ? O24A Cl2 O22 O24 30.8(13) . . . . ? O22A Cl2 O22 O24 165.2(21) . . . . ? O21 Cl2 O22 O24 -103.7(11) . . . . ? O23 Cl2 O22 O24 89.3(12) . . . . ? O23A Cl2 O22 O24 155.3(10) . . . . ? O21A Cl2 O22 O24 -91.3(12) . . . . ? O24 Cl2 O22 O24 0.000(5) . . . . ? O24A Cl2 O23 O24A 0.000(4) . . . . ? O22A Cl2 O23 O24A -147.5(13) . . . . ? O22 Cl2 O23 O24A -109.8(14) . . . . ? O21 Cl2 O23 O24A 81.7(13) . . . . ? O23A Cl2 O23 O24A 158.0(16) . . . . ? O21A Cl2 O23 O24A 71.5(26) . . . . ? O24 Cl2 O23 O24A -35.6(13) . . . . ? O24A Cl2 O23 O23A -158.0(16) . . . . ? O22A Cl2 O23 O23A 54.5(11) . . . . ? O22 Cl2 O23 O23A 92.3(12) . . . . ? O21 Cl2 O23 O23A -76.2(10) . . . . ? O23A Cl2 O23 O23A 0.000(1) . . . . ? O21A Cl2 O23 O23A -86.5(24) . . . . ? O24 Cl2 O23 O23A 166.5(9) . . . . ? Cl2 O23A O23 O24A -21.7(15) . . . . ? O22A O23A O23 O24A -64.3(19) . . . . ? Cl2 O23A O23 Cl2 0.0 . . . . ? O22A O23A O23 Cl2 -42.6(9) . . . . ? O24A Cl2 O24 O24A 0.000(4) . . . . ? O22A Cl2 O24 O24A 140.2(12) . . . . ? O22 Cl2 O24 O24A 149.7(13) . . . . ? O21 Cl2 O24 O24A -87.7(11) . . . . ? O23 Cl2 O24 O24A 31.3(11) . . . . ? O23A Cl2 O24 O24A 62.0(23) . . . . ? O21A Cl2 O24 O24A -117.8(13) . . . . ? O24A Cl2 O24 O22 -149.7(13) . . . . ? O22A Cl2 O24 O22 -9.5(13) . . . . ? O22 Cl2 O24 O22 0.000(5) . . . . ? O21 Cl2 O24 O22 122.7(10) . . . . ? O23 Cl2 O24 O22 -118.4(10) . . . . ? O23A Cl2 O24 O22 -87.7(22) . . . . ? O21A Cl2 O24 O22 92.5(13) . . . . ? O22A O22 O24 O24A -8.3(31) . . . . ? Cl2 O22 O24 O24A -25.5(11) . . . . ? O22A O22 O24 Cl2 17.2(24) . . . . ? Cl2 O22 O24 Cl2 0.000(7) . . . . ? Cl2 O23 O24A O24 44.3(16) . . . . ? O23A O23 O24A O24 65.8(25) . . . . ? Cl2 O23 O24A Cl2 0.000(3) . . . . ? O23A O23 O24A Cl2 21.5(15) . . . . ? Cl2 O24 O24A O23 -46.1(17) . . . . ? O22 O24 O24A O23 -22.3(23) . . . . ? Cl2 O24 O24A Cl2 0.000(3) . . . . ? O22 O24 O24A Cl2 23.8(10) . . . . ? O22A Cl2 O24A O23 57.5(22) . . . . ? O22 Cl2 O24A O23 102.6(15) . . . . ? O21 Cl2 O24A O23 -113.1(12) . . . . ? O23 Cl2 O24A O23 0.000(3) . . . . ? O23A Cl2 O24A O23 -20.4(14) . . . . ? O21A Cl2 O24A O23 -146.0(16) . . . . ? O24 Cl2 O24A O23 137.5(16) . . . . ? O22A Cl2 O24A O24 -80.0(20) . . . . ? O22 Cl2 O24A O24 -34.9(14) . . . . ? O21 Cl2 O24A O24 109.4(10) . . . . ? O23 Cl2 O24A O24 -137.5(16) . . . . ? O23A Cl2 O24A O24 -157.9(10) . . . . ? O21A Cl2 O24A O24 76.5(15) . . . . ? O24 Cl2 O24A O24 0.000(3) . . . . ? _refine_diff_density_max 0.832 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.080 #=END data_3 _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone 'Int. code + (231) 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Trans.' _publ_title ; Mono- and dinuclear complexes of (trpy)M(II) (M=Pd, Pt) with the model nucleobase 1-methylcytosine. Crystal structure and NMR solution studies. ; _publ_author_address ; Sultan Cosar, Matthias B. L. Janik, Matthias Flock, Eva Freisinger, and Bernhard Lippert Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany Etelka Farkas Department of Inorganic and Analytical Chemistry L. Kossuth University Debrecen Hungary ; _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H28 N8 O12 Pt' _chemical_formula_weight 767.59 _chemical_melting_point ? _chemical_compound_source ? 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 monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 11.061(2) _cell_length_b 9.993(2) _cell_length_c 24.211(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.70(3) _cell_angle_gamma 90.00 _cell_volume 2645.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 126(2) _cell_measurement_reflns_used 8522 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 25.66 _exptl_crystal_description cube _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.927 _exptl_crystal_density_method ? _exptl_crystal_F_000 1512 _exptl_absorpt_coefficient_mu 5.382 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.1739 _exptl_absorpt_correction_T_max 0.2545 _exptl_special_details ; ? ; _diffrn_ambient_temperature 126(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 20s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8522 _diffrn_reflns_av_R_equivalents 0.0292 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 25.66 _reflns_number_total 4890 _reflns_number_observed 4699 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00016(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.007(6) _refine_ls_number_reflns 4886 _refine_ls_number_parameters 371 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_obs 0.0238 _refine_ls_wR_factor_all 0.0592 _refine_ls_wR_factor_obs 0.0579 _refine_ls_goodness_of_fit_all 1.042 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.058 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max -0.068 _refine_ls_shift/esd_mean 0.003 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.99974(2) 0.179137(13) 0.99992(2) 0.01590(7) Uani 1 d . . N1 N 1.1590(4) 0.0116(4) 1.1540(2) 0.0238(9) Uani 1 d . . C1 C 1.2147(5) -0.1217(6) 1.1699(2) 0.0319(13) Uani 1 d . . C2 C 1.1141(4) 0.0320(5) 1.0988(2) 0.0207(10) Uani 1 d . . O2 O 1.1179(3) -0.0552(3) 1.0633(2) 0.0253(8) Uani 1 d . . N3 N 1.0646(8) 0.1579(6) 1.0836(3) 0.0181(14) Uani 1 d . . C4 C 1.0542(5) 0.2525(5) 1.1230(2) 0.0206(11) Uani 1 d . . N4 N 0.9974(4) 0.3668(5) 1.1081(2) 0.0240(9) Uani 1 d . . C5 C 1.1031(7) 0.2290(7) 1.1798(3) 0.0277(13) Uani 1 d . . C6 C 1.1543(5) 0.1075(7) 1.1930(2) 0.0277(14) Uani 1 d . . N11 N 0.8245(4) 0.1327(4) 1.0047(2) 0.0196(9) Uani 1 d . . C21 C 0.7525(4) 0.1285(5) 0.9530(2) 0.0196(10) Uani 1 d . . C31 C 0.6287(4) 0.1031(5) 0.9486(2) 0.0232(11) Uani 1 d . . C41 C 0.5757(5) 0.0855(5) 0.9968(3) 0.0295(12) Uani 1 d . . C51 C 0.6487(4) 0.0959(5) 1.0484(2) 0.0241(11) Uani 1 d . . C61 C 0.7732(5) 0.1186(5) 1.0507(2) 0.0221(11) Uani 1 d . . N12 N 0.9364(7) 0.1864(4) 0.9207(3) 0.0136(15) Uani 1 d . . C22 C 0.8174(5) 0.1539(5) 0.9052(2) 0.0184(11) Uani 1 d . . C32 C 0.7707(5) 0.1493(5) 0.8489(2) 0.0236(11) Uani 1 d . . C42 C 0.8494(7) 0.1789(5) 0.8110(3) 0.0220(15) Uani 1 d . . C52 C 0.9694(6) 0.2128(6) 0.8277(2) 0.0236(11) Uani 1 d . . C62 C 1.0128(5) 0.2168(5) 0.8847(2) 0.0163(10) Uani 1 d . . N13 N 1.1535(3) 0.2368(4) 0.9704(2) 0.0190(9) Uani 1 d . . C23 C 1.1379(4) 0.2481(5) 0.9131(2) 0.0174(10) Uani 1 d . . C33 C 1.2314(5) 0.2891(5) 0.8859(2) 0.0201(10) Uani 1 d . . C43 C 1.3450(5) 0.3222(4) 0.9171(3) 0.0221(12) Uani 1 d . . C53 C 1.3596(5) 0.3145(4) 0.9748(3) 0.0217(12) Uani 1 d . . C63 C 1.2618(5) 0.2691(5) 1.0001(2) 0.0198(10) Uani 1 d . . N10 N 0.7072(4) 0.4601(4) 0.8694(2) 0.0255(10) Uani 1 d . . O11 O 0.6345(4) 0.4240(4) 0.9010(2) 0.0355(10) Uani 1 d . . O12 O 0.6722(4) 0.4856(4) 0.8189(2) 0.0326(9) Uani 1 d . . O13 O 0.8200(3) 0.4713(4) 0.8893(2) 0.0303(9) Uani 1 d . . N20 N 0.3976(4) 0.7290(5) 0.6465(2) 0.0289(10) Uani 1 d . . O21 O 0.4047(5) 0.8326(4) 0.6181(2) 0.0395(12) Uani 1 d . . O22 O 0.4418(4) 0.7262(4) 0.6966(2) 0.0326(9) Uani 1 d . . O23 O 0.3452(5) 0.6272(5) 0.6240(2) 0.0422(11) Uani 1 d . . O1W O 0.8229(3) 0.4458(4) 1.0107(2) 0.0261(8) Uani 1 d . . O2W O 1.0477(4) 0.4739(4) 0.7201(2) 0.0417(10) Uani 1 d . . O3W O 0.9686(3) 0.5807(4) 0.8134(2) 0.0333(9) Uani 1 d . . O4W O 0.4320(4) 0.3465(4) 0.7937(2) 0.0344(10) Uani 1 d . . O5W O 0.7872(4) 0.9280(4) 0.6970(2) 0.0354(9) Uani 1 d . . H1A H 1.2396 -0.1144 1.2148 0.094 Uiso 1 d . . H1B H 1.1630 -0.2010 1.1578 0.086 Uiso 1 d . . H1C H 1.2775 -0.1474 1.1385 0.086 Uiso 1 d . . H4A H 0.9800 0.3914 1.0726 0.050 Uiso 1 d . . H4B H 1.0000 0.4314 1.1392 0.050 Uiso 1 d . . H5 H 1.0800 0.3023 1.2107 0.050 Uiso 1 d . . H6 H 1.1800 0.0865 1.2336 0.050 Uiso 1 d . . H31 H 0.5800 0.0957 0.9081 0.050 Uiso 1 d . . H41 H 0.5000 0.0750 0.9982 0.050 Uiso 1 d . . H51 H 0.6200 0.0954 1.0874 0.050 Uiso 1 d . . H61 H 0.8200 0.1306 1.0895 0.050 Uiso 1 d . . H32 H 0.6800 0.1286 0.8336 0.050 Uiso 1 d . . H42 H 0.8200 0.1690 0.7725 0.050 Uiso 1 d . . H52 H 1.0200 0.2308 0.8042 0.050 Uiso 1 d . . H33 H 1.2200 0.3096 0.8436 0.050 Uiso 1 d . . H43 H 1.4200 0.3565 0.8923 0.050 Uiso 1 d . . H53 H 1.4400 0.3583 1.0010 0.050 Uiso 1 d . . H63 H 1.2600 0.2602 1.0385 0.050 Uiso 1 d . . H4WA H 0.8200 0.4485 0.9718 0.050 Uiso 1 d . . H4WB H 0.7600 0.4355 1.0204 0.050 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01545(10) 0.01673(10) 0.01539(10) 0.00015(13) 0.00193(6) -0.00048(12) N1 0.021(2) 0.027(2) 0.024(2) 0.006(2) 0.004(2) 0.004(2) C1 0.036(3) 0.029(3) 0.029(3) 0.009(3) 0.002(2) 0.013(3) C2 0.016(2) 0.026(3) 0.021(3) 0.005(2) 0.006(2) -0.001(2) O2 0.027(2) 0.021(2) 0.027(2) 0.000(2) 0.0024(15) 0.0028(15) N3 0.021(3) 0.022(2) 0.011(3) 0.001(2) 0.002(2) 0.000(2) C4 0.015(3) 0.024(3) 0.024(3) 0.001(2) 0.007(2) -0.003(2) N4 0.028(2) 0.022(2) 0.021(2) -0.002(2) 0.004(2) -0.001(2) C5 0.034(4) 0.032(4) 0.017(3) -0.002(3) 0.004(3) -0.002(3) C6 0.024(3) 0.035(4) 0.024(3) 0.003(3) 0.003(2) 0.001(3) N11 0.021(2) 0.014(2) 0.023(2) 0.000(2) 0.003(2) 0.000(2) C21 0.025(3) 0.011(2) 0.022(3) -0.001(2) 0.003(2) -0.002(2) C31 0.015(2) 0.021(3) 0.032(3) 0.001(2) -0.001(2) -0.001(2) C41 0.023(3) 0.022(3) 0.044(3) 0.006(3) 0.007(2) 0.002(2) C51 0.021(3) 0.021(2) 0.032(3) 0.002(2) 0.009(2) 0.001(2) C61 0.030(3) 0.013(2) 0.024(3) 0.001(2) 0.006(2) 0.000(2) N12 0.011(3) 0.019(3) 0.009(3) 0.000(2) -0.007(2) 0.003(2) C22 0.018(3) 0.011(2) 0.025(3) 0.001(2) -0.001(2) 0.001(2) C32 0.020(3) 0.020(2) 0.028(3) -0.003(2) -0.005(2) 0.002(2) C42 0.031(4) 0.018(4) 0.016(3) 0.004(2) 0.001(3) 0.002(2) C52 0.028(3) 0.021(3) 0.022(3) 0.005(2) 0.004(2) 0.000(3) C62 0.020(3) 0.016(2) 0.014(2) 0.002(2) 0.005(2) 0.001(2) N13 0.017(2) 0.015(2) 0.023(2) -0.001(2) -0.001(2) 0.002(2) C23 0.021(2) 0.011(2) 0.021(3) 0.000(2) 0.005(2) -0.002(2) C33 0.020(3) 0.018(2) 0.021(3) -0.001(2) 0.000(2) 0.000(2) C43 0.025(3) 0.017(3) 0.024(3) -0.001(2) 0.005(2) 0.004(2) C53 0.017(3) 0.015(3) 0.033(3) 0.000(2) 0.002(2) 0.001(2) C63 0.027(3) 0.014(2) 0.018(2) -0.003(2) 0.002(2) 0.002(2) N10 0.027(2) 0.021(2) 0.030(3) -0.004(2) 0.008(2) 0.004(2) O11 0.036(2) 0.033(2) 0.039(3) 0.002(2) 0.008(2) -0.002(2) O12 0.042(2) 0.037(2) 0.018(2) -0.001(2) 0.001(2) 0.009(2) O13 0.026(2) 0.026(2) 0.036(2) 0.001(2) -0.002(2) 0.003(2) N20 0.028(2) 0.032(3) 0.027(3) -0.001(2) 0.006(2) -0.005(2) O21 0.055(3) 0.036(3) 0.025(2) 0.011(2) -0.004(2) -0.015(2) O22 0.034(2) 0.045(2) 0.016(2) 0.000(2) -0.004(2) -0.011(2) O23 0.060(3) 0.034(3) 0.030(3) 0.001(2) -0.003(2) -0.023(2) O1W 0.018(2) 0.031(2) 0.030(2) -0.001(2) 0.0060(14) -0.003(2) O2W 0.044(2) 0.031(2) 0.054(3) 0.002(2) 0.018(2) -0.011(2) O3W 0.025(2) 0.034(2) 0.039(2) -0.005(2) -0.001(2) -0.003(2) O4W 0.040(3) 0.031(2) 0.033(2) 0.001(2) 0.007(2) -0.002(2) O5W 0.041(2) 0.030(2) 0.034(2) 0.006(2) 0.000(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N12 1.941(8) . ? Pt1 N11 2.014(4) . ? Pt1 N13 2.025(4) . ? Pt1 N3 2.056(8) . ? N1 C6 1.352(8) . ? N1 C2 1.367(6) . ? N1 C1 1.493(7) . ? C1 H1A 1.082(6) . ? C1 H1B 0.995(6) . ? C1 H1C 1.135(6) . ? C2 O2 1.229(6) . ? C2 N3 1.399(8) . ? N3 C4 1.360(9) . ? C4 N4 1.327(7) . ? C4 C5 1.419(8) . ? N4 H4A 0.887(4) . ? N4 H4B 0.989(4) . ? C5 C6 1.357(10) . ? C5 H5 1.104(7) . ? C6 H6 1.004(6) . ? N11 C61 1.330(7) . ? N11 C21 1.379(7) . ? C21 C31 1.380(7) . ? C21 C22 1.475(7) . ? C31 C41 1.394(8) . ? C31 H31 1.047(5) . ? C41 C51 1.386(8) . ? C41 H41 0.850(5) . ? C51 C61 1.389(7) . ? C51 H51 1.041(5) . ? C61 H61 1.009(5) . ? N12 C62 1.339(10) . ? N12 C22 1.352(10) . ? C22 C32 1.383(8) . ? C32 C42 1.390(9) . ? C32 H32 1.037(5) . ? C42 C52 1.370(10) . ? C42 H42 0.944(7) . ? C52 C62 1.392(8) . ? C52 H52 0.874(6) . ? C62 C23 1.483(7) . ? N13 C63 1.339(6) . ? N13 C23 1.377(6) . ? C23 C33 1.370(7) . ? C33 C43 1.405(8) . ? C33 H33 1.033(5) . ? C43 C53 1.383(9) . ? C43 H43 1.148(6) . ? C53 C63 1.397(8) . ? C53 H53 1.102(6) . ? C63 H63 0.938(5) . ? N10 O11 1.245(6) . ? N10 O12 1.252(6) . ? N10 O13 1.273(6) . ? N20 O22 1.237(6) . ? N20 O21 1.252(6) . ? N20 O23 1.254(7) . ? O1W H4WA 0.938(4) . ? O1W H4WB 0.774(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Pt1 N11 81.9(3) . . ? N12 Pt1 N13 80.7(3) . . ? N11 Pt1 N13 162.4(2) . . ? N12 Pt1 N3 176.2(2) . . ? N11 Pt1 N3 96.6(3) . . ? N13 Pt1 N3 101.0(3) . . ? C6 N1 C2 122.0(5) . . ? C6 N1 C1 120.6(4) . . ? C2 N1 C1 117.5(4) . . ? N1 C1 H1A 103.5(5) . . ? N1 C1 H1B 116.0(5) . . ? H1A C1 H1B 113.4(5) . . ? N1 C1 H1C 107.4(4) . . ? H1A C1 H1C 126.8(5) . . ? H1B C1 H1C 90.3(5) . . ? O2 C2 N1 122.1(5) . . ? O2 C2 N3 120.5(5) . . ? N1 C2 N3 117.5(5) . . ? C4 N3 C2 120.8(7) . . ? C4 N3 Pt1 124.5(5) . . ? C2 N3 Pt1 114.6(5) . . ? N4 C4 N3 119.6(5) . . ? N4 C4 C5 120.1(5) . . ? N3 C4 C5 120.3(6) . . ? C4 N4 H4A 121.9(5) . . ? C4 N4 H4B 113.4(4) . . ? H4A N4 H4B 122.2(5) . . ? C6 C5 C4 117.4(6) . . ? C6 C5 H5 124.5(6) . . ? C4 C5 H5 116.9(6) . . ? N1 C6 C5 121.9(5) . . ? N1 C6 H6 120.1(6) . . ? C5 C6 H6 117.6(6) . . ? C61 N11 C21 119.7(4) . . ? C61 N11 Pt1 127.5(4) . . ? C21 N11 Pt1 112.6(3) . . ? N11 C21 C31 120.4(5) . . ? N11 C21 C22 115.1(4) . . ? C31 C21 C22 124.4(5) . . ? C21 C31 C41 119.7(5) . . ? C21 C31 H31 116.8(5) . . ? C41 C31 H31 123.5(5) . . ? C51 C41 C31 118.9(5) . . ? C51 C41 H41 114.5(6) . . ? C31 C41 H41 126.3(6) . . ? C41 C51 C61 119.1(5) . . ? C41 C51 H51 127.0(5) . . ? C61 C51 H51 113.7(5) . . ? N11 C61 C51 122.0(5) . . ? N11 C61 H61 122.9(5) . . ? C51 C61 H61 114.9(5) . . ? C62 N12 C22 123.9(7) . . ? C62 N12 Pt1 118.9(5) . . ? C22 N12 Pt1 117.1(6) . . ? N12 C22 C32 119.0(6) . . ? N12 C22 C21 113.1(6) . . ? C32 C22 C21 127.9(5) . . ? C22 C32 C42 117.8(5) . . ? C22 C32 H32 123.8(6) . . ? C42 C32 H32 118.3(6) . . ? C52 C42 C32 122.2(6) . . ? C52 C42 H42 119.4(7) . . ? C32 C42 H42 118.3(7) . . ? C42 C52 C62 118.3(5) . . ? C42 C52 H52 123.1(6) . . ? C62 C52 H52 118.6(6) . . ? N12 C62 C52 118.8(6) . . ? N12 C62 C23 112.4(5) . . ? C52 C62 C23 128.7(5) . . ? C63 N13 C23 119.1(4) . . ? C63 N13 Pt1 127.6(3) . . ? C23 N13 Pt1 113.3(3) . . ? C33 C23 N13 121.4(4) . . ? C33 C23 C62 123.9(4) . . ? N13 C23 C62 114.7(4) . . ? C23 C33 C43 119.3(5) . . ? C23 C33 H33 123.3(5) . . ? C43 C33 H33 116.9(5) . . ? C53 C43 C33 119.3(5) . . ? C53 C43 H43 124.2(5) . . ? C33 C43 H43 116.5(5) . . ? C43 C53 C63 118.7(5) . . ? C43 C53 H53 121.3(5) . . ? C63 C53 H53 119.2(5) . . ? N13 C63 C53 122.2(5) . . ? N13 C63 H63 111.0(5) . . ? C53 C63 H63 126.8(5) . . ? O11 N10 O12 121.8(4) . . ? O11 N10 O13 118.6(4) . . ? O12 N10 O13 119.5(4) . . ? O22 N20 O21 120.5(5) . . ? O22 N20 O23 119.7(5) . . ? O21 N20 O23 119.7(5) . . ? H4WA O1W H4WB 114.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 N1 C2 O2 -179.8(5) . . . . ? C1 N1 C2 O2 0.5(7) . . . . ? C6 N1 C2 N3 1.3(7) . . . . ? C1 N1 C2 N3 -178.5(5) . . . . ? O2 C2 N3 C4 176.5(6) . . . . ? N1 C2 N3 C4 -4.5(10) . . . . ? O2 C2 N3 Pt1 0.9(8) . . . . ? N1 C2 N3 Pt1 179.9(4) . . . . ? N12 Pt1 N3 C4 -147.5(62) . . . . ? N11 Pt1 N3 C4 -80.9(6) . . . . ? N13 Pt1 N3 C4 97.6(6) . . . . ? N12 Pt1 N3 C2 27.9(72) . . . . ? N11 Pt1 N3 C2 94.5(5) . . . . ? N13 Pt1 N3 C2 -87.0(5) . . . . ? C2 N3 C4 N4 -174.2(6) . . . . ? Pt1 N3 C4 N4 0.9(9) . . . . ? C2 N3 C4 C5 5.5(10) . . . . ? Pt1 N3 C4 C5 -179.3(5) . . . . ? N4 C4 C5 C6 176.6(5) . . . . ? N3 C4 C5 C6 -3.1(10) . . . . ? C2 N1 C6 C5 1.0(8) . . . . ? C1 N1 C6 C5 -179.3(5) . . . . ? C4 C5 C6 N1 -0.1(9) . . . . ? N12 Pt1 N11 C61 -173.3(4) . . . . ? N13 Pt1 N11 C61 -164.7(5) . . . . ? N3 Pt1 N11 C61 10.3(5) . . . . ? N12 Pt1 N11 C21 0.5(3) . . . . ? N13 Pt1 N11 C21 9.0(8) . . . . ? N3 Pt1 N11 C21 -176.0(4) . . . . ? C61 N11 C21 C31 -3.3(7) . . . . ? Pt1 N11 C21 C31 -177.5(4) . . . . ? C61 N11 C21 C22 176.1(4) . . . . ? Pt1 N11 C21 C22 1.9(5) . . . . ? N11 C21 C31 C41 1.9(8) . . . . ? C22 C21 C31 C41 -177.5(5) . . . . ? C21 C31 C41 C51 0.9(8) . . . . ? C31 C41 C51 C61 -2.3(8) . . . . ? C21 N11 C61 C51 1.8(7) . . . . ? Pt1 N11 C61 C51 175.2(4) . . . . ? C41 C51 C61 N11 1.0(8) . . . . ? N11 Pt1 N12 C62 179.9(4) . . . . ? N13 Pt1 N12 C62 2.5(4) . . . . ? N3 Pt1 N12 C62 -113.0(66) . . . . ? N11 Pt1 N12 C22 -3.0(4) . . . . ? N13 Pt1 N12 C22 179.6(4) . . . . ? N3 Pt1 N12 C22 64.1(69) . . . . ? C62 N12 C22 C32 1.1(8) . . . . ? Pt1 N12 C22 C32 -175.8(4) . . . . ? C62 N12 C22 C21 -178.4(5) . . . . ? Pt1 N12 C22 C21 4.7(6) . . . . ? N11 C21 C22 N12 -4.2(7) . . . . ? C31 C21 C22 N12 175.1(5) . . . . ? N11 C21 C22 C32 176.4(5) . . . . ? C31 C21 C22 C32 -4.3(8) . . . . ? N12 C22 C32 C42 -0.2(7) . . . . ? C21 C22 C32 C42 179.2(5) . . . . ? C22 C32 C42 C52 -0.5(8) . . . . ? C32 C42 C52 C62 0.2(8) . . . . ? C22 N12 C62 C52 -1.3(8) . . . . ? Pt1 N12 C62 C52 175.5(4) . . . . ? C22 N12 C62 C23 -179.9(5) . . . . ? Pt1 N12 C62 C23 -3.0(6) . . . . ? C42 C52 C62 N12 0.6(8) . . . . ? C42 C52 C62 C23 178.9(5) . . . . ? N12 Pt1 N13 C63 175.4(4) . . . . ? N11 Pt1 N13 C63 166.9(5) . . . . ? N3 Pt1 N13 C63 -8.1(4) . . . . ? N12 Pt1 N13 C23 -1.4(3) . . . . ? N11 Pt1 N13 C23 -10.0(7) . . . . ? N3 Pt1 N13 C23 175.1(3) . . . . ? C63 N13 C23 C33 1.3(7) . . . . ? Pt1 N13 C23 C33 178.4(4) . . . . ? C63 N13 C23 C62 -176.8(4) . . . . ? Pt1 N13 C23 C62 0.3(5) . . . . ? N12 C62 C23 C33 -176.4(5) . . . . ? C52 C62 C23 C33 5.2(9) . . . . ? N12 C62 C23 N13 1.7(6) . . . . ? C52 C62 C23 N13 -176.7(5) . . . . ? N13 C23 C33 C43 -1.0(7) . . . . ? C62 C23 C33 C43 177.0(5) . . . . ? C23 C33 C43 C53 -0.9(7) . . . . ? C33 C43 C53 C63 2.3(7) . . . . ? C23 N13 C63 C53 0.2(7) . . . . ? Pt1 N13 C63 C53 -176.5(3) . . . . ? C43 C53 C63 N13 -2.0(7) . . . . ? _refine_diff_density_max 1.391 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.098 #=END data_4 _publ_contact_author_name 'Prof. Bernhard Lippert' _publ_contact_author_address ; Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany ; _publ_contact_author_email 'lippert@pop.uni-dortmund.de' _publ_contact_author_fax 'Int. code + (231) 755-3797' _publ_contact_author_phone 'Int. code + (231) 755-3840' _publ_contact_letter ? _publ_requested_journal 'Dalton Trans.' _publ_title ; Mono- and dinuclear complexes of (trpy)M(II) (M=Pd, Pt) with the model nucleobase 1-methylcytosine. Crystal structure and NMR solution studies. ; _publ_author_address ; Sultan Cosar, Matthias B. L. Janik, Matthias Flock, Eva Freisinger, and Bernhard Lippert Fachbereich Chemie Universit\"at Dortmund Otto-Hahn-Str. 6 D-44221 Dortmund Germany Etelka Farkas Department of Inorganic and Analytical Chemistry L. Kossuth University Debrecen Hungary ; _audit_creation_method 'SHELXL-93, SHELXL-97' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C35 H30 Cl3 N9 O14 Pt2' _chemical_formula_weight 1297.21 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pt' 'Pt' -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.066(3) _cell_length_b 10.988(2) _cell_length_c 25.783(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.70(3) _cell_angle_gamma 90.00 _cell_volume 3902.2(13) _cell_formula_units_Z 4 _cell_measurement_temperature 163(2) _cell_measurement_reflns_used 81110 _cell_measurement_theta_min 1.48 _cell_measurement_theta_max 23.85 _exptl_crystal_description stick _exptl_crystal_colour red _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2488 _exptl_absorpt_coefficient_mu 7.451 _exptl_absorpt_correction_type SCALEPACK _exptl_absorpt_correction_T_min 0.2134 _exptl_absorpt_correction_T_max 0.4561 _exptl_special_details ; ? ; _diffrn_ambient_temperature 163(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius-KappaCCD' _diffrn_measurement_method ; 360 frames via \w-rotation (\D\w\=1\%) and two times 60s per frame ; _diffrn_detector_area_resol_mean '19 vertical, 18 horizontal' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81110 _diffrn_reflns_av_R_equivalents 0.063 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 23.85 _reflns_number_total 5886 _reflns_number_observed 3277 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'KappaCCD (Nonius BV, Netherlands)' _computing_cell_refinement 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_data_reduction 'DENZO, SCALEPACK (Otwinowski, Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL-PLUS(VMS)' _computing_publication_material 'SHELXL-93' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 8 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00000(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5878 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0978 _refine_ls_R_factor_obs 0.0409 _refine_ls_wR_factor_all 0.1198 _refine_ls_wR_factor_obs 0.0747 _refine_ls_goodness_of_fit_all 0.865 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 1.233 _refine_ls_restrained_S_obs 1.062 _refine_ls_shift/esd_max -0.258 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Pt1 Pt 0.81467(3) 0.06522(4) 0.932307(15) 0.02962(14) Uani 1 d . . Pt2 Pt 0.64195(3) -0.06521(4) 0.865724(15) 0.03332(15) Uani 1 d . . N1 N 0.6721(7) 0.2845(8) 1.0267(3) 0.037(2) Uani 1 d . . C1 C 0.7045(8) 0.3847(10) 1.0645(5) 0.051(3) Uani 1 d . . H1A H 0.7633(52) 0.4193(79) 1.0575(34) 0.195(49) Uiso 1 calc R . H1B H 0.7160(92) 0.3536(25) 1.1000(5) 0.195(49) Uiso 1 calc R . H1C H 0.6551(41) 0.4463(56) 1.0604(36) 0.195(49) Uiso 1 calc R . C2 C 0.7366(9) 0.2398(9) 0.9968(4) 0.038(3) Uani 1 d . . O2 O 0.8171(5) 0.2842(6) 1.0002(3) 0.039(2) Uani 1 d . . N3 N 0.7062(6) 0.1437(7) 0.9633(3) 0.031(2) Uani 1 d . . C4 C 0.6116(8) 0.0997(9) 0.9558(4) 0.032(3) Uani 1 d . . N4 N 0.5823(7) 0.0093(8) 0.9214(3) 0.044(3) Uani 1 d . . H4 H 0.5275(7) -0.0222(8) 0.9239(3) 0.125(68) Uiso 1 calc R . C5 C 0.5465(9) 0.1515(9) 0.9863(4) 0.041(3) Uani 1 d . . H5 H 0.4832(9) 0.1232(9) 0.9828(4) 0.027(20) Uiso 1 calc R . C6 C 0.5807(9) 0.2428(10) 1.0203(4) 0.044(3) Uani 1 d . . H6 H 0.5393(9) 0.2780(10) 1.0399(4) 0.027(20) Uiso 1 calc R . N11A N 0.8594(5) -0.0575(7) 0.9907(3) 0.027(2) Uiso 1 d . . C21A C 0.9280(7) -0.1361(9) 0.9798(4) 0.033(3) Uiso 1 d . . C31A C 0.9708(8) -0.2240(9) 1.0152(4) 0.038(3) Uani 1 d . . H31A H 1.0192(8) -0.2746(9) 1.0076(4) 0.031(8) Uiso 1 calc R . C41A C 0.9384(8) -0.2341(9) 1.0635(5) 0.043(3) Uani 1 d . . H41A H 0.9631(8) -0.2944(9) 1.0878(5) 0.031(8) Uiso 1 calc R . C51A C 0.8705(8) -0.1542(10) 1.0739(4) 0.042(3) Uani 1 d . . H51A H 0.8500(8) -0.1584(10) 1.1060(4) 0.031(8) Uiso 1 calc R . C61A C 0.8320(7) -0.0672(10) 1.0370(4) 0.038(3) Uiso 1 d . . H61A H 0.7856(7) -0.0136(10) 1.0447(4) 0.031(8) Uiso 1 calc R . N11B N 0.9120(6) -0.0183(7) 0.9023(3) 0.030(2) Uiso 1 d . . C21B C 0.9552(7) -0.1181(8) 0.9282(4) 0.027(2) Uiso 1 d . . C31B C 1.0179(7) -0.1854(10) 0.9046(4) 0.037(3) Uiso 1 d . . H31B H 1.0494(7) -0.2530(10) 0.9217(4) 0.031(8) Uiso 1 calc R . C41B C 1.0335(7) -0.1520(9) 0.8559(4) 0.037(3) Uiso 1 d . . H41B H 1.0754(7) -0.1980(9) 0.8402(4) 0.031(8) Uiso 1 calc R . C51B C 0.9876(7) -0.0499(9) 0.8292(4) 0.036(3) Uiso 1 d . . H51B H 0.9969(7) -0.0279(9) 0.7957(4) 0.031(8) Uiso 1 calc R . C61B C 0.9286(7) 0.0156(9) 0.8549(4) 0.030(3) Uiso 1 d . . N11C N 0.8125(5) 0.1697(7) 0.8672(3) 0.027(2) Uiso 1 d . . C21C C 0.8720(7) 0.1276(8) 0.8353(4) 0.025(2) Uiso 1 d . . C31C C 0.8804(7) 0.1882(9) 0.7891(4) 0.034(3) Uiso 1 d . . H31C H 0.9226(7) 0.1606(9) 0.7682(4) 0.031(8) Uiso 1 calc R . C41C C 0.8238(7) 0.2913(9) 0.7752(4) 0.037(3) Uiso 1 d . . H41C H 0.8254(7) 0.3310(9) 0.7435(4) 0.031(8) Uiso 1 calc R . C51C C 0.7666(7) 0.3344(9) 0.8069(4) 0.034(3) Uiso 1 d . . H51C H 0.7309(7) 0.4053(9) 0.7981(4) 0.031(8) Uiso 1 calc R . C61C C 0.7616(7) 0.2717(9) 0.8531(4) 0.036(3) Uiso 1 d . . H61C H 0.7217(7) 0.3015(9) 0.8748(4) 0.031(8) Uiso 1 calc R . N12A N 0.6993(6) -0.2191(7) 0.9040(4) 0.039(2) Uiso 1 d . . C22A C 0.7492(8) -0.2873(11) 0.8737(5) 0.048(3) Uiso 1 d . . C32A C 0.7943(9) -0.3922(10) 0.8958(6) 0.061(4) Uani 1 d . . H32A H 0.8279(9) -0.4402(10) 0.8758(6) 0.037(9) Uiso 1 calc R . C42A C 0.7907(11) -0.4274(13) 0.9462(6) 0.077(5) Uani 1 d . . H42A H 0.8228(11) -0.4970(13) 0.9610(6) 0.037(9) Uiso 1 calc R . C52A C 0.7405(10) -0.3599(12) 0.9733(5) 0.060(4) Uani 1 d . . H52A H 0.7353(10) -0.3843(12) 1.0072(5) 0.037(9) Uiso 1 calc R . C62A C 0.6953(8) -0.2535(11) 0.9525(5) 0.050(3) Uani 1 d . . H62A H 0.6621(8) -0.2061(11) 0.9728(5) 0.037(9) Uiso 1 calc R . N12B N 0.6988(6) -0.1351(7) 0.8102(3) 0.037(2) Uiso 1 d . . C22B C 0.7480(8) -0.2420(10) 0.8214(5) 0.044(3) Uiso 1 d . . C32B C 0.7900(9) -0.2908(11) 0.7817(5) 0.055(4) Uani 1 d . . H32B H 0.8221(9) -0.3652(11) 0.7865(5) 0.037(9) Uiso 1 calc R . C42B C 0.7833(9) -0.2278(12) 0.7356(6) 0.064(4) Uani 1 d . . H42B H 0.8131(9) -0.2597(12) 0.7096(6) 0.037(9) Uiso 1 calc R . C52B C 0.7349(8) -0.1202(11) 0.7261(5) 0.048(3) Uiso 1 d . . H52B H 0.7310(8) -0.0799(11) 0.6940(5) 0.037(9) Uiso 1 calc R . C62B C 0.6924(7) -0.0732(9) 0.7644(4) 0.034(3) Uiso 1 d . . N12C N 0.5989(6) 0.0597(8) 0.8084(3) 0.036(2) Uiso 1 d . . C22C C 0.6348(8) 0.0383(9) 0.7638(4) 0.036(3) Uiso 1 d . . C32C C 0.6130(9) 0.1171(10) 0.7215(4) 0.047(3) Uani 1 d . . H32C H 0.6369(9) 0.1037(10) 0.6909(4) 0.037(9) Uiso 1 calc R . C42C C 0.5540(8) 0.2182(11) 0.7257(5) 0.054(4) Uani 1 d . . H42C H 0.5396(8) 0.2732(11) 0.6978(5) 0.037(9) Uiso 1 calc R . C52C C 0.5185(8) 0.2361(11) 0.7692(6) 0.056(4) Uani 1 d . . H52C H 0.4785(8) 0.3026(11) 0.7712(6) 0.037(9) Uiso 1 calc R . C62C C 0.5407(8) 0.1563(10) 0.8113(5) 0.044(3) Uani 1 d . . H62C H 0.5158(8) 0.1690(10) 0.8416(5) 0.037(9) Uiso 1 calc R . Cl1 Cl 1.0447(2) 0.4967(3) 0.83181(11) 0.0444(8) Uani 1 d . . O11 O 1.1306(6) 0.5697(7) 0.8317(3) 0.064(2) Uani 1 d . . O12 O 0.9720(6) 0.5351(7) 0.7873(3) 0.061(2) Uani 1 d . . O13 O 1.0643(6) 0.3716(7) 0.8251(3) 0.062(2) Uani 1 d . . O14 O 1.0125(7) 0.5137(7) 0.8797(3) 0.074(3) Uani 1 d . . Cl2 Cl 0.3126(2) -0.0355(3) 0.85042(12) 0.0500(8) Uani 1 d . . O21 O 0.2151(6) 0.0043(9) 0.8324(4) 0.092(3) Uani 1 d . . O22 O 0.3541(6) 0.0257(8) 0.8996(4) 0.085(3) Uani 1 d . . O23 O 0.3628(7) -0.0072(8) 0.8104(4) 0.084(3) Uani 1 d . . O24 O 0.3101(9) -0.1620(9) 0.8582(4) 0.130(5) Uani 1 d . . Cl3 Cl 0.5414(2) 0.4705(3) 0.8816(2) 0.0646(10) Uani 1 d . . O31 O 0.5247(6) 0.5836(7) 0.8991(3) 0.070(3) Uani 1 d . . O32 O 0.6058(6) 0.3972(7) 0.9180(3) 0.068(3) Uani 1 d . . O33 O 0.5892(7) 0.4905(9) 0.8337(4) 0.086(3) Uani 1 d . . O34 O 0.4499(6) 0.4059(7) 0.8634(3) 0.069(3) Uani 1 d . . O1W O 0.6715(8) 0.7224(10) 0.0821(5) 0.128(4) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.0326(3) 0.0260(3) 0.0297(3) 0.0006(2) 0.0051(2) 0.0009(2) Pt2 0.0344(3) 0.0308(3) 0.0339(3) -0.0038(2) 0.0049(2) -0.0019(2) N1 0.038(6) 0.039(6) 0.034(6) 0.002(5) 0.006(5) 0.007(5) C1 0.060(9) 0.041(7) 0.059(8) -0.017(6) 0.025(7) -0.007(6) C2 0.043(8) 0.031(7) 0.036(7) -0.003(6) -0.006(7) 0.007(6) O2 0.032(5) 0.031(4) 0.052(5) -0.006(4) 0.007(4) 0.002(4) N3 0.037(6) 0.024(5) 0.029(5) -0.008(4) -0.002(5) 0.000(4) C4 0.039(7) 0.032(7) 0.025(6) 0.001(5) 0.005(6) 0.009(5) N4 0.035(6) 0.049(6) 0.043(6) -0.007(5) -0.001(5) 0.000(5) C5 0.051(8) 0.036(7) 0.038(7) 0.002(6) 0.018(6) -0.011(6) C6 0.041(8) 0.049(8) 0.044(8) 0.005(6) 0.013(7) 0.006(7) C31A 0.043(7) 0.022(6) 0.050(8) -0.010(6) 0.009(6) 0.004(5) C41A 0.048(8) 0.033(7) 0.042(8) 0.009(6) -0.005(7) -0.002(6) C51A 0.041(7) 0.040(8) 0.045(7) 0.020(6) 0.010(6) -0.001(6) C32A 0.047(8) 0.042(8) 0.085(11) -0.010(7) -0.007(8) 0.002(6) C42A 0.091(12) 0.043(9) 0.079(12) -0.012(9) -0.022(9) 0.009(9) C52A 0.069(10) 0.049(9) 0.047(9) 0.026(7) -0.021(8) -0.035(8) C62A 0.044(8) 0.046(8) 0.058(9) -0.005(7) 0.006(7) -0.008(6) C32B 0.060(9) 0.027(7) 0.081(10) -0.015(7) 0.024(8) -0.012(6) C42B 0.050(9) 0.071(10) 0.079(11) -0.037(9) 0.035(8) -0.022(8) C32C 0.054(8) 0.050(8) 0.028(7) -0.008(6) -0.008(6) -0.008(7) C42C 0.044(9) 0.055(9) 0.057(9) 0.015(8) -0.006(7) -0.010(7) C52C 0.036(8) 0.043(8) 0.079(10) -0.003(8) -0.011(8) 0.004(6) C62C 0.039(7) 0.048(8) 0.040(7) -0.010(6) -0.002(6) 0.000(6) Cl1 0.053(2) 0.043(2) 0.039(2) 0.004(2) 0.012(2) 0.006(2) O11 0.052(5) 0.056(5) 0.081(6) 0.000(5) 0.005(5) -0.009(5) O12 0.054(5) 0.078(6) 0.051(5) 0.008(5) 0.010(5) 0.005(5) O13 0.085(7) 0.033(5) 0.074(6) -0.002(4) 0.033(5) 0.009(4) O14 0.105(8) 0.069(6) 0.058(6) 0.006(5) 0.041(6) 0.019(6) Cl2 0.049(2) 0.049(2) 0.052(2) -0.007(2) 0.009(2) -0.005(2) O21 0.054(6) 0.121(8) 0.095(8) -0.032(7) 0.006(6) 0.005(6) O22 0.063(6) 0.111(8) 0.072(6) -0.047(6) -0.006(5) -0.004(6) O23 0.096(8) 0.079(7) 0.085(7) -0.006(6) 0.037(6) -0.031(6) O24 0.240(15) 0.052(7) 0.100(9) 0.019(6) 0.039(9) 0.011(8) Cl3 0.050(2) 0.044(2) 0.089(3) -0.005(2) -0.012(2) 0.008(2) O31 0.068(6) 0.050(6) 0.084(7) -0.022(5) -0.001(5) 0.016(5) O32 0.057(6) 0.055(6) 0.078(6) 0.022(5) -0.019(5) 0.005(4) O33 0.091(8) 0.102(8) 0.076(7) 0.006(6) 0.038(6) -0.002(6) O34 0.063(6) 0.048(6) 0.084(7) -0.001(5) -0.009(5) -0.014(4) O1W 0.100(9) 0.139(10) 0.139(11) 0.008(8) 0.013(8) -0.007(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N11B 1.936(8) . ? Pt1 N11A 2.023(7) . ? Pt1 N11C 2.028(7) . ? Pt1 N3 2.050(8) . ? Pt1 Pt2 3.0350(10) . ? Pt2 N12B 1.935(9) . ? Pt2 N4 1.980(9) . ? Pt2 N12C 2.019(8) . ? Pt2 N12A 2.040(8) . ? N1 C6 1.344(13) . ? N1 C2 1.394(13) . ? N1 C1 1.480(13) . ? C1 H1A 0.96 . ? C1 H1B 0.96 . ? C1 H1C 0.96 . ? C2 O2 1.220(12) . ? C2 N3 1.376(12) . ? N3 C4 1.391(12) . ? C4 N4 1.341(12) . ? C4 C5 1.439(14) . ? N4 H4 0.86 . ? C5 C6 1.354(14) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? N11A C61A 1.332(12) . ? N11A C21A 1.365(12) . ? C21A C31A 1.380(13) . ? C21A C21B 1.471(13) . ? C31A C41A 1.414(14) . ? C31A H31A 0.93 . ? C41A C51A 1.364(14) . ? C41A H41A 0.93 . ? C51A C61A 1.380(13) . ? C51A H51A 0.93 . ? C61A H61A 0.93 . ? N11B C61B 1.342(12) . ? N11B C21B 1.361(11) . ? C21B C31B 1.384(12) . ? C31B C41B 1.366(13) . ? C31B H31B 0.93 . ? C41B C51B 1.403(13) . ? C41B H41B 0.93 . ? C51B C61B 1.367(13) . ? C51B H51B 0.93 . ? C61B C21C 1.497(12) . ? N11C C61C 1.340(11) . ? N11C C21C 1.368(11) . ? C21C C31C 1.390(12) . ? C31C C41C 1.389(13) . ? C31C H31C 0.93 . ? C41C C51C 1.344(12) . ? C41C H41C 0.93 . ? C51C C61C 1.388(13) . ? C51C H51C 0.93 . ? C61C H61C 0.93 . ? N12A C62A 1.318(13) . ? N12A C22A 1.373(13) . ? C22A C32A 1.381(15) . ? C22A C22B 1.435(14) . ? C32A C42A 1.37(2) . ? C32A H32A 0.93 . ? C42A C52A 1.32(2) . ? C42A H42A 0.93 . ? C52A C62A 1.386(15) . ? C52A H52A 0.93 . ? C62A H62A 0.93 . ? N12B C62B 1.348(12) . ? N12B C22B 1.364(12) . ? C22B C32B 1.389(15) . ? C32B C42B 1.36(2) . ? C32B H32B 0.93 . ? C42B C52B 1.362(15) . ? C42B H42B 0.93 . ? C52B C62B 1.357(14) . ? C52B H52B 0.93 . ? C62B C22C 1.467(13) . ? N12C C62C 1.352(12) . ? N12C C22C 1.366(12) . ? C22C C32C 1.376(14) . ? C32C C42C 1.404(15) . ? C32C H32C 0.93 . ? C42C C52C 1.33(2) . ? C42C H42C 0.93 . ? C52C C62C 1.383(15) . ? C52C H52C 0.93 . ? C62C H62C 0.93 . ? Cl1 O14 1.412(8) . ? Cl1 O13 1.420(7) . ? Cl1 O12 1.437(8) . ? Cl1 O11 1.450(8) . ? Cl2 O23 1.400(9) . ? Cl2 O24 1.406(10) . ? Cl2 O21 1.424(9) . ? Cl2 O22 1.449(8) . ? Cl3 O31 1.359(8) . ? Cl3 O32 1.416(7) . ? Cl3 O34 1.462(8) . ? Cl3 O33 1.536(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11B Pt1 N11A 81.0(3) . . ? N11B Pt1 N11C 80.3(3) . . ? N11A Pt1 N11C 160.5(3) . . ? N11B Pt1 N3 176.3(3) . . ? N11A Pt1 N3 97.7(3) . . ? N11C Pt1 N3 101.3(3) . . ? N11B Pt1 Pt2 95.7(2) . . ? N11A Pt1 Pt2 101.4(2) . . ? N11C Pt1 Pt2 85.6(2) . . ? N3 Pt1 Pt2 81.1(2) . . ? N12B Pt2 N4 178.6(3) . . ? N12B Pt2 N12C 80.5(3) . . ? N4 Pt2 N12C 98.2(3) . . ? N12B Pt2 N12A 81.2(3) . . ? N4 Pt2 N12A 100.1(4) . . ? N12C Pt2 N12A 161.5(4) . . ? N12B Pt2 Pt1 101.7(2) . . ? N4 Pt2 Pt1 78.7(3) . . ? N12C Pt2 Pt1 100.4(2) . . ? N12A Pt2 Pt1 85.7(2) . . ? C6 N1 C2 121.8(10) . . ? C6 N1 C1 119.6(10) . . ? C2 N1 C1 118.6(9) . . ? N1 C1 H1A 109.5(6) . . ? N1 C1 H1B 109.5(6) . . ? H1A C1 H1B 109.47(7) . . ? N1 C1 H1C 109.5(6) . . ? H1A C1 H1C 109.47(9) . . ? H1B C1 H1C 109.5 . . ? O2 C2 N3 121.2(11) . . ? O2 C2 N1 121.2(10) . . ? N3 C2 N1 117.6(11) . . ? C2 N3 C4 121.3(9) . . ? C2 N3 Pt1 113.9(7) . . ? C4 N3 Pt1 124.5(6) . . ? N4 C4 N3 120.4(10) . . ? N4 C4 C5 120.7(10) . . ? N3 C4 C5 119.0(9) . . ? C4 N4 Pt2 131.9(9) . . ? C4 N4 H4 114.1(7) . . ? Pt2 N4 H4 114.1(3) . . ? C6 C5 C4 117.6(11) . . ? C6 C5 H5 121.2(7) . . ? C4 C5 H5 121.2(6) . . ? N1 C6 C5 122.5(11) . . ? N1 C6 H6 118.7(6) . . ? C5 C6 H6 118.7(7) . . ? C61A N11A C21A 118.6(9) . . ? C61A N11A Pt1 128.1(7) . . ? C21A N11A Pt1 113.3(6) . . ? N11A C21A C31A 122.6(10) . . ? N11A C21A C21B 115.1(9) . . ? C31A C21A C21B 122.2(10) . . ? C21A C31A C41A 117.5(10) . . ? C21A C31A H31A 121.3(7) . . ? C41A C31A H31A 121.3(6) . . ? C51A C41A C31A 119.2(10) . . ? C51A C41A H41A 120.4(7) . . ? C31A C41A H41A 120.4(6) . . ? C41A C51A C61A 120.1(11) . . ? C41A C51A H51A 119.9(7) . . ? C61A C51A H51A 119.9(7) . . ? N11A C61A C51A 122.0(11) . . ? N11A C61A H61A 119.0(6) . . ? C51A C61A H61A 119.0(7) . . ? C61B N11B C21B 121.9(9) . . ? C61B N11B Pt1 120.0(7) . . ? C21B N11B Pt1 117.8(7) . . ? N11B C21B C31B 118.3(9) . . ? N11B C21B C21A 112.4(9) . . ? C31B C21B C21A 129.3(9) . . ? C41B C31B C21B 119.7(10) . . ? C41B C31B H31B 120.1(6) . . ? C21B C31B H31B 120.1(6) . . ? C31B C41B C51B 121.5(10) . . ? C31B C41B H41B 119.3(6) . . ? C51B C41B H41B 119.3(6) . . ? C61B C51B C41B 116.5(10) . . ? C61B C51B H51B 121.7(6) . . ? C41B C51B H51B 121.7(6) . . ? N11B C61B C51B 122.0(9) . . ? N11B C61B C21C 110.9(9) . . ? C51B C61B C21C 127.1(9) . . ? C61C N11C C21C 118.5(9) . . ? C61C N11C Pt1 128.1(7) . . ? C21C N11C Pt1 113.4(6) . . ? N11C C21C C31C 121.4(9) . . ? N11C C21C C61B 115.1(8) . . ? C31C C21C C61B 123.4(9) . . ? C41C C31C C21C 117.9(10) . . ? C41C C31C H31C 121.0(6) . . ? C21C C31C H31C 121.0(6) . . ? C51C C41C C31C 120.8(10) . . ? C51C C41C H41C 119.6(6) . . ? C31C C41C H41C 119.6(6) . . ? C41C C51C C61C 119.2(10) . . ? C41C C51C H51C 120.4(6) . . ? C61C C51C H51C 120.4(6) . . ? N11C C61C C51C 122.1(10) . . ? N11C C61C H61C 118.9(6) . . ? C51C C61C H61C 118.9(6) . . ? C62A N12A C22A 120.5(10) . . ? C62A N12A Pt2 127.4(8) . . ? C22A N12A Pt2 112.0(7) . . ? N12A C22A C32A 117.8(11) . . ? N12A C22A C22B 115.8(10) . . ? C32A C22A C22B 126.4(12) . . ? C42A C32A C22A 121.6(14) . . ? C42A C32A H32A 119.2(9) . . ? C22A C32A H32A 119.2(8) . . ? C52A C42A C32A 118.2(14) . . ? C52A C42A H42A 120.9(9) . . ? C32A C42A H42A 120.9(9) . . ? C42A C52A C62A 121.5(14) . . ? C42A C52A H52A 119.3(9) . . ? C62A C52A H52A 119.3(9) . . ? N12A C62A C52A 120.3(12) . . ? N12A C62A H62A 119.8(7) . . ? C52A C62A H62A 119.8(9) . . ? C62B N12B C22B 124.1(10) . . ? C62B N12B Pt2 118.9(7) . . ? C22B N12B Pt2 116.9(8) . . ? N12B C22B C32B 116.7(11) . . ? N12B C22B C22A 114.0(11) . . ? C32B C22B C22A 129.3(11) . . ? C42B C32B C22B 118.8(12) . . ? C42B C32B H32B 120.6(8) . . ? C22B C32B H32B 120.6(7) . . ? C32B C42B C52B 122.9(13) . . ? C32B C42B H42B 118.5(8) . . ? C52B C42B H42B 118.5(8) . . ? C62B C52B C42B 118.5(12) . . ? C62B C52B H52B 120.8(7) . . ? C42B C52B H52B 120.8(8) . . ? N12B C62B C52B 118.9(10) . . ? N12B C62B C22C 111.8(9) . . ? C52B C62B C22C 129.3(10) . . ? C62C N12C C22C 120.9(9) . . ? C62C N12C Pt2 125.9(7) . . ? C22C N12C Pt2 113.1(7) . . ? N12C C22C C32C 119.8(10) . . ? N12C C22C C62B 115.5(9) . . ? C32C C22C C62B 124.6(10) . . ? C22C C32C C42C 118.5(11) . . ? C22C C32C H32C 120.8(7) . . ? C42C C32C H32C 120.8(7) . . ? C52C C42C C32C 120.7(12) . . ? C52C C42C H42C 119.7(8) . . ? C32C C42C H42C 119.7(7) . . ? C42C C52C C62C 120.3(12) . . ? C42C C52C H52C 119.9(8) . . ? C62C C52C H52C 119.9(8) . . ? N12C C62C C52C 119.8(11) . . ? N12C C62C H62C 120.1(6) . . ? C52C C62C H62C 120.1(8) . . ? O14 Cl1 O13 109.8(5) . . ? O14 Cl1 O12 110.9(5) . . ? O13 Cl1 O12 108.1(5) . . ? O14 Cl1 O11 110.2(5) . . ? O13 Cl1 O11 110.7(5) . . ? O12 Cl1 O11 107.1(5) . . ? O23 Cl2 O24 110.8(6) . . ? O23 Cl2 O21 106.7(6) . . ? O24 Cl2 O21 107.5(7) . . ? O23 Cl2 O22 111.6(6) . . ? O24 Cl2 O22 110.6(6) . . ? O21 Cl2 O22 109.5(5) . . ? O31 Cl3 O32 115.5(6) . . ? O31 Cl3 O34 110.5(5) . . ? O32 Cl3 O34 109.9(5) . . ? O31 Cl3 O33 105.6(6) . . ? O32 Cl3 O33 106.8(6) . . ? O34 Cl3 O33 108.2(6) . . ? 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 N11B Pt1 Pt2 N12B -16.1(3) . . . . ? N11A Pt1 Pt2 N12B -98.0(3) . . . . ? N11C Pt1 Pt2 N12B 63.7(3) . . . . ? N3 Pt1 Pt2 N12B 165.9(3) . . . . ? N11B Pt1 Pt2 N4 165.3(3) . . . . ? N11A Pt1 Pt2 N4 83.4(3) . . . . ? N11C Pt1 Pt2 N4 -115.0(3) . . . . ? N3 Pt1 Pt2 N4 -12.8(3) . . . . ? N11B Pt1 Pt2 N12C -98.4(3) . . . . ? N11A Pt1 Pt2 N12C 179.7(4) . . . . ? N11C Pt1 Pt2 N12C -18.6(3) . . . . ? N3 Pt1 Pt2 N12C 83.6(3) . . . . ? N11B Pt1 Pt2 N12A 64.0(3) . . . . ? N11A Pt1 Pt2 N12A -17.9(3) . . . . ? N11C Pt1 Pt2 N12A 143.8(3) . . . . ? N3 Pt1 Pt2 N12A -114.0(3) . . . . ? C6 N1 C2 O2 174.7(10) . . . . ? C1 N1 C2 O2 -2.3(15) . . . . ? C6 N1 C2 N3 -5.2(14) . . . . ? C1 N1 C2 N3 177.8(9) . . . . ? O2 C2 N3 C4 -174.4(9) . . . . ? N1 C2 N3 C4 5.6(14) . . . . ? O2 C2 N3 Pt1 11.0(13) . . . . ? N1 C2 N3 Pt1 -169.0(7) . . . . ? N11B Pt1 N3 C2 158.0(46) . . . . ? N11A Pt1 N3 C2 88.7(7) . . . . ? N11C Pt1 N3 C2 -87.2(7) . . . . ? Pt2 Pt1 N3 C2 -170.9(7) . . . . ? N11B Pt1 N3 C4 -16.4(52) . . . . ? N11A Pt1 N3 C4 -85.7(8) . . . . ? N11C Pt1 N3 C4 98.4(8) . . . . ? Pt2 Pt1 N3 C4 14.7(7) . . . . ? C2 N3 C4 N4 177.3(9) . . . . ? Pt1 N3 C4 N4 -8.7(13) . . . . ? C2 N3 C4 C5 -3.7(14) . . . . ? Pt1 N3 C4 C5 170.3(7) . . . . ? N3 C4 N4 Pt2 -12.1(14) . . . . ? C5 C4 N4 Pt2 168.9(7) . . . . ? N12B Pt2 N4 C4 -87.0(161) . . . . ? N12C Pt2 N4 C4 -81.6(9) . . . . ? N12A Pt2 N4 C4 100.9(9) . . . . ? Pt1 Pt2 N4 C4 17.4(9) . . . . ? N4 C4 C5 C6 -179.8(9) . . . . ? N3 C4 C5 C6 1.2(14) . . . . ? C2 N1 C6 C5 3.0(15) . . . . ? C1 N1 C6 C5 179.9(10) . . . . ? C4 C5 C6 N1 -0.8(15) . . . . ? N11B Pt1 N11A C61A 175.7(9) . . . . ? N11C Pt1 N11A C61A 160.0(8) . . . . ? N3 Pt1 N11A C61A -7.9(9) . . . . ? Pt2 Pt1 N11A C61A -90.3(8) . . . . ? N11B Pt1 N11A C21A -2.5(7) . . . . ? N11C Pt1 N11A C21A -18.1(13) . . . . ? N3 Pt1 N11A C21A 174.0(7) . . . . ? Pt2 Pt1 N11A C21A 91.6(6) . . . . ? C61A N11A C21A C31A -0.8(15) . . . . ? Pt1 N11A C21A C31A 177.5(8) . . . . ? C61A N11A C21A C21B -179.1(9) . . . . ? Pt1 N11A C21A C21B -0.7(11) . . . . ? N11A C21A C31A C41A 2.5(15) . . . . ? C21B C21A C31A C41A -179.4(9) . . . . ? C21A C31A C41A C51A -3.0(15) . . . . ? C31A C41A C51A C61A 1.9(16) . . . . ? C21A N11A C61A C51A -0.3(15) . . . . ? Pt1 N11A C61A C51A -178.4(7) . . . . ? C41A C51A C61A N11A -0.2(16) . . . . ? N11A Pt1 N11B C61B 179.6(8) . . . . ? N11C Pt1 N11B C61B -5.7(7) . . . . ? N3 Pt1 N11B C61B 109.7(47) . . . . ? Pt2 Pt1 N11B C61B 78.9(7) . . . . ? N11A Pt1 N11B C21B 5.7(6) . . . . ? N11C Pt1 N11B C21B -179.5(7) . . . . ? N3 Pt1 N11B C21B -64.2(50) . . . . ? Pt2 Pt1 N11B C21B -95.0(6) . . . . ? C61B N11B C21B C31B 0.2(14) . . . . ? Pt1 N11B C21B C31B 173.9(7) . . . . ? C61B N11B C21B C21A 178.8(9) . . . . ? Pt1 N11B C21B C21A -7.5(10) . . . . ? N11A C21A C21B N11B 5.2(12) . . . . ? C31A C21A C21B N11B -173.1(9) . . . . ? N11A C21A C21B C31B -176.5(9) . . . . ? C31A C21A C21B C31B 5.3(17) . . . . ? N11B C21B C31B C41B -1.3(14) . . . . ? C21A C21B C31B C41B -179.6(10) . . . . ? C21B C31B C41B C51B 0.5(15) . . . . ? C31B C41B C51B C61B 1.4(15) . . . . ? C21B N11B C61B C51B 1.9(15) . . . . ? Pt1 N11B C61B C51B -171.8(7) . . . . ? C21B N11B C61B C21C 179.8(8) . . . . ? Pt1 N11B C61B C21C 6.2(11) . . . . ? C41B C51B C61B N11B -2.6(15) . . . . ? C41B C51B C61B C21C 179.8(9) . . . . ? N11B Pt1 N11C C61C -175.9(8) . . . . ? N11A Pt1 N11C C61C -160.2(9) . . . . ? N3 Pt1 N11C C61C 7.6(8) . . . . ? Pt2 Pt1 N11C C61C 87.6(8) . . . . ? N11B Pt1 N11C C21C 3.6(6) . . . . ? N11A Pt1 N11C C21C 19.2(12) . . . . ? N3 Pt1 N11C C21C -173.0(6) . . . . ? Pt2 Pt1 N11C C21C -93.0(6) . . . . ? C61C N11C C21C C31C 0.0(13) . . . . ? Pt1 N11C C21C C31C -179.5(7) . . . . ? C61C N11C C21C C61B 178.1(8) . . . . ? Pt1 N11C C21C C61B -1.4(10) . . . . ? N11B C61B C21C N11C -2.8(11) . . . . ? C51B C61B C21C N11C 175.0(10) . . . . ? N11B C61B C21C C31C 175.2(9) . . . . ? C51B C61B C21C C31C -7.0(15) . . . . ? N11C C21C C31C C41C -2.2(14) . . . . ? C61B C21C C31C C41C 180.0(8) . . . . ? C21C C31C C41C C51C 3.4(15) . . . . ? C31C C41C C51C C61C -2.6(15) . . . . ? C21C N11C C61C C51C 0.9(14) . . . . ? Pt1 N11C C61C C51C -179.7(7) . . . . ? C41C C51C C61C N11C 0.4(15) . . . . ? N12B Pt2 N12A C62A 179.9(10) . . . . ? N4 Pt2 N12A C62A -0.3(10) . . . . ? N12C Pt2 N12A C62A -172.4(9) . . . . ? Pt1 Pt2 N12A C62A 77.4(9) . . . . ? N12B Pt2 N12A C22A 2.3(7) . . . . ? N4 Pt2 N12A C22A -177.8(7) . . . . ? N12C Pt2 N12A C22A 10.1(15) . . . . ? Pt1 Pt2 N12A C22A -100.2(7) . . . . ? C62A N12A C22A C32A 0.3(16) . . . . ? Pt2 N12A C22A C32A 178.0(8) . . . . ? C62A N12A C22A C22B 179.5(10) . . . . ? Pt2 N12A C22A C22B -2.8(12) . . . . ? N12A C22A C32A C42A -0.7(18) . . . . ? C22B C22A C32A C42A -179.8(12) . . . . ? C22A C32A C42A C52A 1.8(20) . . . . ? C32A C42A C52A C62A -2.4(20) . . . . ? C22A N12A C62A C52A -0.9(16) . . . . ? Pt2 N12A C62A C52A -178.3(7) . . . . ? C42A C52A C62A N12A 2.0(18) . . . . ? N4 Pt2 N12B C62B 9.9(164) . . . . ? N12C Pt2 N12B C62B 4.5(7) . . . . ? N12A Pt2 N12B C62B -177.9(8) . . . . ? Pt1 Pt2 N12B C62B -94.2(7) . . . . ? N4 Pt2 N12B C22B -173.7(158) . . . . ? N12C Pt2 N12B C22B -179.1(8) . . . . ? N12A Pt2 N12B C22B -1.6(7) . . . . ? Pt1 Pt2 N12B C22B 82.2(7) . . . . ? C62B N12B C22B C32B -2.9(16) . . . . ? Pt2 N12B C22B C32B -179.0(8) . . . . ? C62B N12B C22B C22A 176.6(10) . . . . ? Pt2 N12B C22B C22A 0.5(12) . . . . ? N12A C22A C22B N12B 1.6(15) . . . . ? C32A C22A C22B N12B -179.3(11) . . . . ? N12A C22A C22B C32B -178.9(11) . . . . ? C32A C22A C22B C32B 0.2(20) . . . . ? N12B C22B C32B C42B 2.8(17) . . . . ? C22A C22B C32B C42B -176.7(12) . . . . ? C22B C32B C42B C52B -1.9(19) . . . . ? C32B C42B C52B C62B 0.8(18) . . . . ? C22B N12B C62B C52B 1.9(16) . . . . ? Pt2 N12B C62B C52B 178.0(8) . . . . ? C22B N12B C62B C22C 180.0(9) . . . . ? Pt2 N12B C62B C22C -4.0(11) . . . . ? C42B C52B C62B N12B -0.7(16) . . . . ? C42B C52B C62B C22C -178.4(10) . . . . ? N12B Pt2 N12C C62C 175.8(9) . . . . ? N4 Pt2 N12C C62C -4.1(9) . . . . ? N12A Pt2 N12C C62C 168.1(9) . . . . ? Pt1 Pt2 N12C C62C -83.9(8) . . . . ? N12B Pt2 N12C C22C -4.1(7) . . . . ? N4 Pt2 N12C C22C 176.0(7) . . . . ? N12A Pt2 N12C C22C -11.8(15) . . . . ? Pt1 Pt2 N12C C22C 96.2(7) . . . . ? C62C N12C C22C C32C 1.2(15) . . . . ? Pt2 N12C C22C C32C -178.9(8) . . . . ? C62C N12C C22C C62B -176.7(9) . . . . ? Pt2 N12C C22C C62B 3.2(11) . . . . ? N12B C62B C22C N12C 0.3(13) . . . . ? C52B C62B C22C N12C 178.1(10) . . . . ? N12B C62B C22C C32C -177.5(10) . . . . ? C52B C62B C22C C32C 0.3(18) . . . . ? N12C C22C C32C C42C 0.0(16) . . . . ? C62B C22C C32C C42C 177.7(10) . . . . ? C22C C32C C42C C52C -1.2(17) . . . . ? C32C C42C C52C C62C 1.2(18) . . . . ? C22C N12C C62C C52C -1.3(15) . . . . ? Pt2 N12C C62C C52C 178.8(7) . . . . ? C42C C52C C62C N12C 0.1(17) . . . . ? _refine_diff_density_max 1.450 _refine_diff_density_min -1.395 _refine_diff_density_rms 0.155