data_publication_text _publ_requested_journal Inorg.Chem. _publ_contact_author_name 'Stephen J. Lippard' _publ_contact_author_address ;77 Massachusetts Ave, 18-498 Cambridge, MA 02139 ; _publ_contact_author_email lippard@mit.edu _publ_contact_author_phone (617)253-1892 _publ_contact_author_fax (617)258-8150 loop_ _publ_author_name _publ_author_address 'Wilson, Justin J.' ;77 Massachusetts Ave, 18-498 Cambridge, MA 02139 ; 'Lippard, Stephen J.' ;77 Massachusetts Ave, 18-498 Cambridge, MA 02139 ; data_[1](NO3)2*0.5H2O _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C4 H18 N6 O10.50 Pt2' _chemical_formula_weight 708.42 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 C2/c 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' '-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 19.1794(9) _cell_length_b 15.7804(7) _cell_length_c 10.8811(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.4520(10) _cell_angle_gamma 90.00 _cell_volume 3238.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 30.06 _exptl_crystal_description shard _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.906 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 17.320 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.0782 _exptl_absorpt_correction_T_max 0.7233 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35449 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0226 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 30.10 _reflns_number_total 4748 _reflns_number_gt 4318 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The asymmetric unit consisted of the [1]2+, a nitrate anion on a general crystallographic position in full occupancy, a nitrate anion residing on a crystallographic two-fold axis, and a nitrate anion disordered with a water molecule about a crystallographic inversion center. For the nitrate anion disordered about the inversion center, the bond distances and angles were restrained to be similar to those of the non-disordered nitrate anion. The occupancy factors of the disordered nitrate and water atoms were 50:50 as necessitated by crystallographic inversion center. The protons of this half occupancy water molecule could not be located on the difference Fourier map and were therefore not included in the final model. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0161P)^2^+9.1384P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4748 _refine_ls_number_parameters 233 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0227 _refine_ls_R_factor_gt 0.0182 _refine_ls_wR_factor_ref 0.0383 _refine_ls_wR_factor_gt 0.0370 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.444007(6) 0.205133(8) 0.839622(10) 0.01462(3) Uani 1 1 d . . . Pt2 Pt 0.324086(6) 0.226451(7) 0.968375(10) 0.01287(3) Uani 1 1 d . . . O1 O 0.41643(12) 0.32506(15) 0.7799(2) 0.0196(5) Uani 1 1 d . . . O3 O 0.33351(11) 0.34639(14) 0.89979(19) 0.0177(4) Uani 1 1 d . . . N3 N 0.36823(14) 0.27068(17) 1.1389(2) 0.0171(5) Uani 1 1 d . . . H3A H 0.3336 0.2809 1.1842 0.026 Uiso 1 1 calc R . . H3B H 0.3920 0.3196 1.1303 0.026 Uiso 1 1 calc R . . H3C H 0.3990 0.2315 1.1790 0.026 Uiso 1 1 calc R . . N2 N 0.46721(16) 0.08462(19) 0.8942(3) 0.0251(6) Uani 1 1 d . . . H2A H 0.5083 0.0686 0.8701 0.038 Uiso 1 1 calc R . . H2B H 0.4314 0.0498 0.8583 0.038 Uiso 1 1 calc R . . H2C H 0.4724 0.0811 0.9789 0.038 Uiso 1 1 calc R . . N1 N 0.52910(15) 0.2520(2) 0.9588(3) 0.0253(6) Uani 1 1 d . . . H1A H 0.5547 0.2860 0.9159 0.038 Uiso 1 1 calc R . . H1B H 0.5568 0.2084 0.9940 0.038 Uiso 1 1 calc R . . H1C H 0.5140 0.2826 1.0197 0.038 Uiso 1 1 calc R . . O2 O 0.36450(12) 0.16070(15) 0.7038(2) 0.0205(5) Uani 1 1 d . . . N4 N 0.30936(14) 0.11010(16) 1.0385(2) 0.0167(5) Uani 1 1 d . . . H4A H 0.3478 0.0960 1.0969 0.025 Uiso 1 1 calc R . . H4B H 0.3036 0.0713 0.9757 0.025 Uiso 1 1 calc R . . H4C H 0.2700 0.1108 1.0744 0.025 Uiso 1 1 calc R . . C3 C 0.29944(17) 0.1608(2) 0.7078(3) 0.0165(6) Uani 1 1 d . . . C4 C 0.24989(18) 0.1320(2) 0.5925(3) 0.0246(7) Uani 1 1 d . . . H4D H 0.2647 0.1564 0.5185 0.037 Uiso 1 1 calc R . . H4E H 0.2016 0.1508 0.5963 0.037 Uiso 1 1 calc R . . H4F H 0.2509 0.0701 0.5874 0.037 Uiso 1 1 calc R . . O9 O 0.45175(12) 0.06219(15) 0.1801(2) 0.0201(5) Uani 1 1 d . . . N6 N 0.5000 0.1025(3) 0.2500 0.0184(8) Uani 1 2 d S . . O8 O 0.5000 0.1815(2) 0.2500 0.0321(9) Uani 1 2 d S . . O7 O 0.40112(15) 0.0894(2) 0.4401(3) 0.0475(9) Uani 1 1 d D . . O5 O 0.31537(17) 0.15015(17) 0.3155(2) 0.0389(7) Uani 1 1 d D . . O6 O 0.31987(14) 0.01394(16) 0.3290(2) 0.0287(6) Uani 1 1 d D . . N5 N 0.34555(15) 0.08511(19) 0.3615(2) 0.0211(6) Uani 1 1 d D . . O4 O 0.27153(11) 0.18377(14) 0.79921(19) 0.0164(4) Uani 1 1 d . . . C1 C 0.37078(17) 0.3696(2) 0.8205(3) 0.0176(6) Uani 1 1 d . . . C2 C 0.36020(19) 0.4581(2) 0.7723(3) 0.0255(7) Uani 1 1 d . . . H2D H 0.3106 0.4660 0.7324 0.038 Uiso 1 1 calc R . . H2E H 0.3910 0.4684 0.7111 0.038 Uiso 1 1 calc R . . H2F H 0.3721 0.4981 0.8419 0.038 Uiso 1 1 calc R . . O10W O 0.4836(14) 0.3851(12) 1.127(2) 0.034(4) Uani 0.50 1 d P A -2 O10 O 0.4888(13) 0.3811(11) 1.1183(16) 0.027(4) Uani 0.50 1 d PD B -1 N7 N 0.4969(4) 0.4463(4) 1.0562(6) 0.0307(14) Uani 0.50 1 d PD B -1 O11 O 0.5351(4) 0.4428(5) 0.9747(7) 0.056(2) Uani 0.50 1 d PD B -1 O12 O 0.4696(5) 0.5139(5) 1.0738(8) 0.063(2) Uani 0.50 1 d PD B -1 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 0.01262(6) 0.01859(6) 0.01409(5) 0.00172(4) 0.00621(4) 0.00322(4) Pt2 0.01199(6) 0.01485(6) 0.01298(5) 0.00094(4) 0.00552(4) 0.00220(4) O1 0.0191(12) 0.0195(12) 0.0226(11) 0.0041(9) 0.0102(9) 0.0010(9) O3 0.0176(12) 0.0169(11) 0.0204(10) 0.0015(8) 0.0081(8) 0.0021(9) N3 0.0148(13) 0.0184(14) 0.0190(12) 0.0007(10) 0.0057(10) 0.0010(10) N2 0.0243(16) 0.0285(17) 0.0245(14) 0.0043(12) 0.0100(11) 0.0091(13) N1 0.0157(14) 0.0416(19) 0.0197(13) -0.0006(12) 0.0063(10) 0.0027(13) O2 0.0186(12) 0.0262(13) 0.0185(10) -0.0031(9) 0.0086(8) -0.0016(10) N4 0.0158(13) 0.0181(13) 0.0175(12) 0.0023(10) 0.0062(9) 0.0034(10) C3 0.0184(16) 0.0150(15) 0.0174(13) 0.0013(11) 0.0063(11) -0.0013(12) C4 0.0236(18) 0.0306(19) 0.0201(15) -0.0065(13) 0.0055(13) -0.0059(15) O9 0.0147(11) 0.0222(12) 0.0223(11) -0.0060(9) 0.0004(9) 0.0001(9) N6 0.0144(19) 0.022(2) 0.0200(18) 0.000 0.0062(14) 0.000 O8 0.0234(19) 0.0172(18) 0.052(2) 0.000 -0.0039(16) 0.000 O7 0.0231(15) 0.078(2) 0.0387(16) -0.0283(16) -0.0018(12) 0.0006(15) O5 0.068(2) 0.0245(15) 0.0288(13) 0.0072(11) 0.0199(13) 0.0027(14) O6 0.0301(15) 0.0238(13) 0.0316(13) -0.0003(10) 0.0039(11) -0.0044(11) N5 0.0185(14) 0.0298(16) 0.0166(12) -0.0024(11) 0.0072(10) -0.0040(12) O4 0.0159(11) 0.0196(11) 0.0150(10) -0.0008(8) 0.0062(8) 0.0018(9) C1 0.0152(15) 0.0175(15) 0.0191(14) 0.0013(11) 0.0008(11) -0.0006(12) C2 0.0229(18) 0.0175(17) 0.0375(19) 0.0077(14) 0.0097(14) -0.0008(14) O10W 0.030(7) 0.024(7) 0.052(10) -0.005(5) 0.017(6) -0.010(5) O10 0.045(10) 0.025(7) 0.011(4) 0.005(4) 0.007(5) -0.007(5) N7 0.034(4) 0.032(4) 0.026(3) -0.006(3) 0.006(3) -0.014(3) O11 0.085(6) 0.048(5) 0.047(4) -0.014(3) 0.046(4) -0.030(4) O12 0.075(6) 0.040(5) 0.083(6) 0.017(4) 0.039(5) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N2 2.018(3) . ? Pt1 N1 2.031(3) . ? Pt1 O1 2.039(2) . ? Pt1 O2 2.045(2) . ? Pt1 Pt2 2.92149(18) . ? Pt1 Pt1 3.1523(2) 2_656 ? Pt2 N3 2.019(3) . ? Pt2 N4 2.028(3) . ? Pt2 O4 2.046(2) . ? Pt2 O3 2.054(2) . ? Pt2 Pt2 3.1324(3) 7_557 ? O1 C1 1.263(4) . ? O3 C1 1.270(4) . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? O2 C3 1.256(4) . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? C3 O4 1.265(3) . ? C3 C4 1.500(4) . ? C4 H4D 0.9800 . ? C4 H4E 0.9800 . ? C4 H4F 0.9800 . ? O9 N6 1.258(3) . ? N6 O8 1.248(5) . ? N6 O9 1.258(3) 2_655 ? O7 N5 1.242(4) . ? O5 N5 1.239(4) . ? O6 N5 1.251(4) . ? C1 C2 1.494(4) . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C2 H2F 0.9800 . ? O10 N7 1.258(13) . ? N7 O12 1.219(10) . ? N7 O11 1.248(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt1 N1 92.67(13) . . ? N2 Pt1 O1 177.47(11) . . ? N1 Pt1 O1 89.84(11) . . ? N2 Pt1 O2 89.16(11) . . ? N1 Pt1 O2 173.54(10) . . ? O1 Pt1 O2 88.38(9) . . ? N2 Pt1 Pt2 96.78(8) . . ? N1 Pt1 Pt2 105.27(8) . . ? O1 Pt1 Pt2 82.21(6) . . ? O2 Pt1 Pt2 80.63(6) . . ? N2 Pt1 Pt1 92.50(8) . 2_656 ? N1 Pt1 Pt1 80.56(8) . 2_656 ? O1 Pt1 Pt1 88.25(6) . 2_656 ? O2 Pt1 Pt1 93.17(6) . 2_656 ? Pt2 Pt1 Pt1 168.740(6) . 2_656 ? N3 Pt2 N4 91.78(10) . . ? N3 Pt2 O4 175.36(10) . . ? N4 Pt2 O4 87.76(10) . . ? N3 Pt2 O3 88.02(10) . . ? N4 Pt2 O3 176.71(9) . . ? O4 Pt2 O3 92.17(9) . . ? N3 Pt2 Pt1 104.19(8) . . ? N4 Pt2 Pt1 104.58(7) . . ? O4 Pt2 Pt1 80.38(6) . . ? O3 Pt2 Pt1 78.64(6) . . ? N3 Pt2 Pt2 87.82(8) . 7_557 ? N4 Pt2 Pt2 86.46(7) . 7_557 ? O4 Pt2 Pt2 87.55(6) . 7_557 ? O3 Pt2 Pt2 90.25(6) . 7_557 ? Pt1 Pt2 Pt2 163.185(6) . 7_557 ? C1 O1 Pt1 124.1(2) . . ? C1 O3 Pt2 127.6(2) . . ? Pt2 N3 H3A 109.5 . . ? Pt2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Pt2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C3 O2 Pt1 126.1(2) . . ? Pt2 N4 H4A 109.5 . . ? Pt2 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Pt2 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? O2 C3 O4 126.3(3) . . ? O2 C3 C4 117.0(3) . . ? O4 C3 C4 116.7(3) . . ? C3 C4 H4D 109.5 . . ? C3 C4 H4E 109.5 . . ? H4D C4 H4E 109.5 . . ? C3 C4 H4F 109.5 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? O8 N6 O9 120.33(19) . . ? O8 N6 O9 120.33(19) . 2_655 ? O9 N6 O9 119.3(4) . 2_655 ? O5 N5 O7 120.9(3) . . ? O5 N5 O6 119.9(3) . . ? O7 N5 O6 119.2(3) . . ? C3 O4 Pt2 126.3(2) . . ? O1 C1 O3 126.1(3) . . ? O1 C1 C2 117.1(3) . . ? O3 C1 C2 116.8(3) . . ? C1 C2 H2D 109.5 . . ? C1 C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C1 C2 H2F 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? O12 N7 O11 118.3(7) . . ? O12 N7 O10 122.2(12) . . ? O11 N7 O10 119.5(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 30.10 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.320 _refine_diff_density_min -1.529 _refine_diff_density_rms 0.166 #===END data_[2](NO3)2*3DMF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H39 Cl2 N9 O13 Pt2' _chemical_formula_weight 990.61 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 13.3959(5) _cell_length_b 10.3272(4) _cell_length_c 25.3699(10) _cell_angle_alpha 90.00 _cell_angle_beta 121.7120(10) _cell_angle_gamma 90.00 _cell_volume 2985.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9798 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 29.24 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_absorpt_coefficient_mu 9.610 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.3464 _exptl_absorpt_correction_T_max 0.8310 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61247 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0248 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 29.33 _reflns_number_total 8166 _reflns_number_gt 7145 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of DMF was disordered over two orientations. The bond lengths and angles of the two disordered components were restrained to be similar to one another as were the thermal displacement parameters of the ellipsoids. The site occupancy factors of the disordered components refined to a ratio of 71:29 ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+11.0050P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8166 _refine_ls_number_parameters 387 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.475853(14) 0.923341(15) 0.391510(7) 0.01672(4) Uani 1 1 d . . . Pt2 Pt 0.625119(15) 0.734409(15) 0.423436(7) 0.01715(4) Uani 1 1 d . . . Cl1 Cl 0.34739(11) 1.10319(11) 0.37822(6) 0.0296(2) Uani 1 1 d . . . O1 O 0.6077(3) 1.0149(3) 0.46664(14) 0.0240(7) Uani 1 1 d . . . Cl2 Cl 0.76620(11) 0.56203(11) 0.46732(5) 0.0276(2) Uani 1 1 d . . . O4 O 0.5579(3) 0.6683(3) 0.47402(14) 0.0214(6) Uani 1 1 d . . . O2 O 0.4237(3) 0.8279(3) 0.44284(14) 0.0219(6) Uani 1 1 d . . . O3 O 0.7372(3) 0.8508(3) 0.49509(13) 0.0227(6) Uani 1 1 d . . . N2 N 0.3387(3) 0.8416(4) 0.31510(17) 0.0243(8) Uani 1 1 d . . . H2A H 0.2770 0.8975 0.2979 0.036 Uiso 1 1 calc R . . H2B H 0.3176 0.7671 0.3259 0.036 Uiso 1 1 calc R . . H2C H 0.3600 0.8235 0.2872 0.036 Uiso 1 1 calc R . . N3 N 0.6999(4) 0.7952(4) 0.37623(17) 0.0234(8) Uani 1 1 d . . . H3A H 0.7396 0.8703 0.3931 0.035 Uiso 1 1 calc R . . H3B H 0.6432 0.8089 0.3359 0.035 Uiso 1 1 calc R . . H3C H 0.7507 0.7337 0.3784 0.035 Uiso 1 1 calc R . . N4 N 0.5235(4) 0.6081(4) 0.35450(17) 0.0234(8) Uani 1 1 d . . . H4A H 0.5052 0.6427 0.3175 0.035 Uiso 1 1 calc R . . H4B H 0.4564 0.5924 0.3543 0.035 Uiso 1 1 calc R . . H4C H 0.5634 0.5326 0.3608 0.035 Uiso 1 1 calc R . . C1 C 0.7077(4) 0.9635(4) 0.5013(2) 0.0231(9) Uani 1 1 d . . . N1 N 0.5210(4) 1.0306(4) 0.34051(18) 0.0258(8) Uani 1 1 d . . . H1A H 0.4858 1.1095 0.3328 0.039 Uiso 1 1 calc R . . H1B H 0.4973 0.9895 0.3040 0.039 Uiso 1 1 calc R . . H1C H 0.6003 1.0410 0.3618 0.039 Uiso 1 1 calc R . . C3 C 0.4734(4) 0.7258(4) 0.47310(19) 0.0203(8) Uani 1 1 d . . . N7 N 0.8142(4) 0.5297(4) 0.63197(18) 0.0266(8) Uani 1 1 d . . . N6 N 0.4788(5) 0.8244(4) 0.21492(19) 0.0367(11) Uani 1 1 d . . . C4 C 0.4296(4) 0.6686(4) 0.5117(2) 0.0247(9) Uani 1 1 d . . . H4D H 0.4142 0.5760 0.5025 0.037 Uiso 1 1 calc R . . H4E H 0.3570 0.7123 0.5021 0.037 Uiso 1 1 calc R . . H4F H 0.4891 0.6801 0.5557 0.037 Uiso 1 1 calc R . . C2 C 0.7989(5) 1.0425(5) 0.5543(2) 0.0319(11) Uani 1 1 d . . . H2D H 0.7712 1.0645 0.5821 0.048 Uiso 1 1 calc R . . H2E H 0.8134 1.1222 0.5384 0.048 Uiso 1 1 calc R . . H2F H 0.8718 0.9926 0.5771 0.048 Uiso 1 1 calc R . . O11 O 0.6827(3) 0.4172(3) 0.64464(18) 0.0339(8) Uani 1 1 d . . . O10 O 0.5575(4) 0.9028(4) 0.25008(17) 0.0437(10) Uani 1 1 d . . . O9 O 0.4340(4) 0.7489(4) 0.23646(18) 0.0430(10) Uani 1 1 d . . . O8 O 0.4447(4) 0.8201(4) 0.15892(17) 0.0464(11) Uani 1 1 d . . . O12 O 0.0871(4) 0.8596(5) 0.2888(2) 0.0550(12) Uani 1 1 d . . . C5 C 0.7270(5) 0.5204(5) 0.6412(2) 0.0312(11) Uani 1 1 d . . . H5 H 0.6949 0.5988 0.6455 0.037 Uiso 1 1 calc R . . C6 C 0.8696(5) 0.4159(5) 0.6238(3) 0.0353(12) Uani 1 1 d . . . H6A H 0.8430 0.3378 0.6348 0.053 Uiso 1 1 calc R . . H6B H 0.9550 0.4233 0.6505 0.053 Uiso 1 1 calc R . . H6C H 0.8478 0.4102 0.5804 0.053 Uiso 1 1 calc R . . C7 C 0.8607(5) 0.6546(5) 0.6287(3) 0.0375(12) Uani 1 1 d . . . H7A H 0.8458 0.6675 0.5868 0.056 Uiso 1 1 calc R . . H7B H 0.9454 0.6570 0.6587 0.056 Uiso 1 1 calc R . . H7C H 0.8222 0.7235 0.6382 0.056 Uiso 1 1 calc R . . N8 N -0.0528(4) 0.9788(5) 0.2924(2) 0.0394(11) Uani 1 1 d . . . C8 C 0.0398(6) 0.9656(7) 0.2856(3) 0.0455(15) Uani 1 1 d . . . H8 H 0.0706 1.0411 0.2778 0.055 Uiso 1 1 calc R . . C9 C -0.1001(7) 0.8708(7) 0.3073(4) 0.0596(19) Uani 1 1 d . . . H9A H -0.0830 0.7909 0.2926 0.089 Uiso 1 1 calc R . . H9B H -0.1852 0.8811 0.2871 0.089 Uiso 1 1 calc R . . H9C H -0.0644 0.8662 0.3523 0.089 Uiso 1 1 calc R . . C10 C -0.0957(7) 1.1064(7) 0.2933(3) 0.0564(18) Uani 1 1 d . . . H10A H -0.0655 1.1325 0.3363 0.085 Uiso 1 1 calc R . . H10B H -0.1816 1.1053 0.2703 0.085 Uiso 1 1 calc R . . H10C H -0.0690 1.1681 0.2739 0.085 Uiso 1 1 calc R . . O6 O 0.8492(3) 0.6332(4) 0.35708(17) 0.0368(9) Uani 1 1 d . . . N5 N 0.7817(4) 0.5708(5) 0.3097(2) 0.0434(12) Uani 1 1 d . . . O7 O 0.6739(3) 0.5691(5) 0.28860(18) 0.0457(11) Uani 1 1 d . . . O5 O 0.8236(4) 0.5103(6) 0.2829(3) 0.0765(18) Uani 1 1 d . . . N9 N 0.8965(4) 0.2299(5) 0.4405(3) 0.0405(11) Uani 1 1 d U . . C12 C 0.9730(16) 0.222(2) 0.5009(6) 0.089(7) Uani 0.71(3) 1 d PDU A 1 H12A H 1.0322 0.2905 0.5133 0.133 Uiso 0.353(13) 1 calc PR A 1 H12B H 1.0114 0.1375 0.5108 0.133 Uiso 0.353(13) 1 calc PR A 1 H12C H 0.9321 0.2336 0.5232 0.133 Uiso 0.353(13) 1 calc PR A 1 H12D H 0.9516 0.1505 0.5182 0.133 Uiso 0.353(13) 1 calc PR A 1 H12E H 0.9724 0.3035 0.5207 0.133 Uiso 0.353(13) 1 calc PR A 1 H12F H 1.0517 0.2075 0.5084 0.133 Uiso 0.353(13) 1 calc PR A 1 C13 C 0.9018(14) 0.3524(10) 0.4091(9) 0.065(4) Uani 0.71(3) 1 d PDU A 1 H13A H 0.9725 0.4014 0.4379 0.098 Uiso 0.353(13) 1 calc PR A 1 H13B H 0.8322 0.4054 0.3969 0.098 Uiso 0.353(13) 1 calc PR A 1 H13C H 0.9040 0.3295 0.3723 0.098 Uiso 0.353(13) 1 calc PR A 1 H13D H 0.8333 0.3561 0.3668 0.098 Uiso 0.353(13) 1 calc PR A 1 H13E H 0.9736 0.3521 0.4078 0.098 Uiso 0.353(13) 1 calc PR A 1 H13F H 0.9018 0.4280 0.4324 0.098 Uiso 0.353(13) 1 calc PR A 1 O13 O 0.786(2) 0.0527(13) 0.4228(6) 0.047(2) Uani 0.71(3) 1 d PDU A 1 C11 C 0.8080(11) 0.1526(14) 0.4039(6) 0.041(3) Uani 0.71(3) 1 d PDU A 1 H11 H 0.7591 0.1747 0.3613 0.049 Uiso 0.71(3) 1 calc PR A 1 C12A C 1.000(2) 0.138(4) 0.4980(13) 0.066(8) Uani 0.29(3) 1 d PDU A 2 H12G H 1.0671 0.1920 0.5264 0.100 Uiso 0.147(13) 1 calc PR A 2 H12H H 1.0254 0.0703 0.4805 0.100 Uiso 0.147(13) 1 calc PR A 2 H12I H 0.9673 0.0974 0.5207 0.100 Uiso 0.147(13) 1 calc PR A 2 H12J H 0.9728 0.0478 0.4921 0.100 Uiso 0.147(13) 1 calc PR A 2 H12K H 1.0144 0.1695 0.5379 0.100 Uiso 0.147(13) 1 calc PR A 2 H12L H 1.0726 0.1424 0.4977 0.100 Uiso 0.147(13) 1 calc PR A 2 C13A C 0.942(3) 0.351(3) 0.456(2) 0.081(11) Uani 0.29(3) 1 d PDU A 2 H13G H 1.0206 0.3474 0.4931 0.121 Uiso 0.147(13) 1 calc PR A 2 H13H H 0.8912 0.4056 0.4635 0.121 Uiso 0.147(13) 1 calc PR A 2 H13I H 0.9469 0.3877 0.4215 0.121 Uiso 0.147(13) 1 calc PR A 2 H13J H 0.8852 0.4131 0.4256 0.121 Uiso 0.147(13) 1 calc PR A 2 H13K H 1.0146 0.3548 0.4552 0.121 Uiso 0.147(13) 1 calc PR A 2 H13L H 0.9589 0.3728 0.4972 0.121 Uiso 0.147(13) 1 calc PR A 2 O13A O 0.776(5) 0.058(4) 0.4067(16) 0.047(2) Uani 0.29(3) 1 d PDU A 2 C11A C 0.805(3) 0.174(3) 0.4148(16) 0.041(3) Uani 0.29(3) 1 d PD A 2 H11A H 0.7395 0.2307 0.3965 0.049 Uiso 0.29(3) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01991(9) 0.01401(7) 0.01625(7) -0.00073(5) 0.00953(6) -0.00070(6) Pt2 0.02172(9) 0.01527(7) 0.01535(7) -0.00089(5) 0.01036(6) -0.00172(6) Cl1 0.0314(6) 0.0214(5) 0.0388(6) -0.0009(4) 0.0205(5) 0.0030(4) O1 0.0251(18) 0.0212(16) 0.0216(15) -0.0068(12) 0.0094(14) -0.0044(13) Cl2 0.0304(6) 0.0234(5) 0.0291(5) 0.0059(4) 0.0158(5) 0.0051(4) O4 0.0291(18) 0.0189(15) 0.0218(14) 0.0013(12) 0.0173(14) 0.0006(12) O2 0.0275(18) 0.0201(15) 0.0222(15) -0.0006(12) 0.0159(14) -0.0016(12) O3 0.0249(17) 0.0225(16) 0.0164(14) -0.0040(12) 0.0079(13) -0.0031(13) N2 0.023(2) 0.0229(19) 0.0204(17) -0.0032(14) 0.0065(16) -0.0010(15) N3 0.027(2) 0.0249(19) 0.0197(17) -0.0004(15) 0.0130(16) -0.0053(16) N4 0.028(2) 0.0224(18) 0.0201(17) -0.0050(14) 0.0127(16) -0.0053(16) C1 0.027(2) 0.023(2) 0.0187(19) -0.0018(16) 0.0115(18) -0.0032(18) N1 0.031(2) 0.0213(19) 0.030(2) 0.0046(15) 0.0188(18) 0.0010(16) C3 0.023(2) 0.019(2) 0.0188(19) -0.0039(15) 0.0101(17) -0.0056(16) N7 0.022(2) 0.026(2) 0.0265(19) 0.0016(16) 0.0087(17) -0.0021(16) N6 0.061(3) 0.026(2) 0.024(2) 0.0058(17) 0.022(2) 0.017(2) C4 0.032(3) 0.020(2) 0.029(2) -0.0016(17) 0.021(2) -0.0024(18) C2 0.030(3) 0.034(3) 0.026(2) -0.011(2) 0.011(2) -0.008(2) O11 0.028(2) 0.0295(18) 0.045(2) -0.0017(16) 0.0199(17) -0.0081(15) O10 0.064(3) 0.033(2) 0.0254(18) 0.0007(15) 0.0172(19) 0.0137(19) O9 0.066(3) 0.037(2) 0.035(2) 0.0138(16) 0.033(2) 0.018(2) O8 0.090(3) 0.0260(19) 0.0243(18) 0.0026(15) 0.031(2) 0.003(2) O12 0.061(3) 0.058(3) 0.046(3) -0.004(2) 0.029(2) 0.008(2) C5 0.029(3) 0.028(3) 0.032(3) -0.001(2) 0.013(2) 0.000(2) C6 0.036(3) 0.031(3) 0.040(3) 0.006(2) 0.021(2) 0.002(2) C7 0.034(3) 0.031(3) 0.044(3) 0.002(2) 0.018(3) -0.007(2) N8 0.042(3) 0.038(3) 0.035(2) 0.005(2) 0.019(2) 0.000(2) C8 0.050(4) 0.052(4) 0.032(3) -0.001(3) 0.020(3) -0.008(3) C9 0.055(4) 0.050(4) 0.071(5) 0.014(4) 0.031(4) -0.008(3) C10 0.057(4) 0.045(4) 0.048(4) 0.002(3) 0.014(3) 0.000(3) O6 0.027(2) 0.050(2) 0.0313(18) -0.0131(17) 0.0142(16) -0.0061(17) N5 0.027(3) 0.064(3) 0.035(2) -0.019(2) 0.013(2) -0.001(2) O7 0.024(2) 0.073(3) 0.036(2) -0.012(2) 0.0125(17) -0.006(2) O5 0.049(3) 0.107(5) 0.067(3) -0.049(3) 0.026(3) -0.003(3) N9 0.036(3) 0.032(2) 0.065(3) -0.012(2) 0.035(2) -0.0098(19) C12 0.072(11) 0.111(14) 0.057(6) 0.004(7) 0.016(6) -0.057(10) C13 0.082(9) 0.034(5) 0.099(11) 0.011(6) 0.061(9) 0.005(5) O13 0.061(5) 0.043(3) 0.041(7) -0.008(4) 0.028(7) -0.028(3) C11 0.036(4) 0.058(6) 0.036(5) -0.003(4) 0.025(4) -0.011(4) C12A 0.033(13) 0.11(2) 0.041(12) -0.004(13) 0.009(9) 0.003(14) C13A 0.08(2) 0.059(11) 0.12(3) -0.043(14) 0.06(2) -0.043(12) O13A 0.061(5) 0.043(3) 0.041(7) -0.008(4) 0.028(7) -0.028(3) C11A 0.036(4) 0.058(6) 0.036(5) -0.003(4) 0.025(4) -0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.022(4) . ? Pt1 N2 2.025(4) . ? Pt1 O1 2.027(3) . ? Pt1 O2 2.028(3) . ? Pt1 Cl1 2.4321(12) . ? Pt1 Pt2 2.5997(2) . ? Pt2 N3 2.024(4) . ? Pt2 N4 2.027(4) . ? Pt2 O3 2.033(3) . ? Pt2 O4 2.034(3) . ? Pt2 Cl2 2.4017(11) . ? O1 C1 1.269(6) . ? O4 C3 1.269(5) . ? O2 C3 1.268(5) . ? O3 C1 1.266(6) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? C1 C2 1.496(6) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? C3 C4 1.501(6) . ? N7 C5 1.310(7) . ? N7 C7 1.454(6) . ? N7 C6 1.463(7) . ? N6 O8 1.244(5) . ? N6 O10 1.255(6) . ? N6 O9 1.270(6) . ? C4 H4D 0.9800 . ? C4 H4E 0.9800 . ? C4 H4F 0.9800 . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C2 H2F 0.9800 . ? O11 C5 1.246(6) . ? O12 C8 1.246(8) . ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? N8 C8 1.346(8) . ? N8 C9 1.428(8) . ? N8 C10 1.443(8) . ? C8 H8 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O6 N5 1.239(6) . ? N5 O7 1.249(6) . ? N5 O5 1.253(6) . ? N9 C11A 1.19(3) . ? N9 C11 1.323(13) . ? N9 C12 1.324(14) . ? N9 C13A 1.36(2) . ? N9 C13 1.515(11) . ? N9 C12A 1.68(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13D 0.9800 . ? C13 H13E 0.9800 . ? C13 H13F 0.9800 . ? O13 C11 1.235(11) . ? C11 H11 0.9500 . ? C12A H12G 0.9800 . ? C12A H12H 0.9800 . ? C12A H12I 0.9800 . ? C12A H12J 0.9800 . ? C12A H12K 0.9800 . ? C12A H12L 0.9800 . ? C13A H13G 0.9800 . ? C13A H13H 0.9800 . ? C13A H13I 0.9800 . ? C13A H13J 0.9800 . ? C13A H13K 0.9800 . ? C13A H13L 0.9800 . ? O13A C11A 1.241(18) . ? C11A H11A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N2 92.38(16) . . ? N1 Pt1 O1 86.57(15) . . ? N2 Pt1 O1 176.65(15) . . ? N1 Pt1 O2 175.58(14) . . ? N2 Pt1 O2 88.10(14) . . ? O1 Pt1 O2 92.70(13) . . ? N1 Pt1 Cl1 85.48(12) . . ? N2 Pt1 Cl1 88.04(12) . . ? O1 Pt1 Cl1 88.70(10) . . ? O2 Pt1 Cl1 90.15(9) . . ? N1 Pt1 Pt2 99.81(12) . . ? N2 Pt1 Pt2 98.49(11) . . ? O1 Pt1 Pt2 84.84(9) . . ? O2 Pt1 Pt2 84.46(9) . . ? Cl1 Pt1 Pt2 171.36(3) . . ? N3 Pt2 N4 90.33(15) . . ? N3 Pt2 O3 89.01(14) . . ? N4 Pt2 O3 175.54(15) . . ? N3 Pt2 O4 176.98(15) . . ? N4 Pt2 O4 90.54(14) . . ? O3 Pt2 O4 89.89(12) . . ? N3 Pt2 Cl2 89.46(12) . . ? N4 Pt2 Cl2 86.04(12) . . ? O3 Pt2 Cl2 89.55(10) . . ? O4 Pt2 Cl2 87.72(9) . . ? N3 Pt2 Pt1 97.00(12) . . ? N4 Pt2 Pt1 99.00(12) . . ? O3 Pt2 Pt1 85.46(9) . . ? O4 Pt2 Pt1 85.72(9) . . ? Cl2 Pt2 Pt1 171.76(3) . . ? C1 O1 Pt1 122.5(3) . . ? C3 O4 Pt2 121.2(3) . . ? C3 O2 Pt1 123.0(3) . . ? C1 O3 Pt2 121.5(3) . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Pt2 N3 H3A 109.5 . . ? Pt2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Pt2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Pt2 N4 H4A 109.5 . . ? Pt2 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Pt2 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? O3 C1 O1 125.7(4) . . ? O3 C1 C2 116.9(4) . . ? O1 C1 C2 117.4(4) . . ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? O2 C3 O4 125.4(4) . . ? O2 C3 C4 117.5(4) . . ? O4 C3 C4 117.1(4) . . ? C5 N7 C7 121.7(5) . . ? C5 N7 C6 122.2(4) . . ? C7 N7 C6 116.1(4) . . ? O8 N6 O10 120.1(5) . . ? O8 N6 O9 119.8(5) . . ? O10 N6 O9 120.1(4) . . ? C3 C4 H4D 109.5 . . ? C3 C4 H4E 109.5 . . ? H4D C4 H4E 109.5 . . ? C3 C4 H4F 109.5 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? C1 C2 H2D 109.5 . . ? C1 C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C1 C2 H2F 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? O11 C5 N7 125.3(5) . . ? O11 C5 H5 117.3 . . ? N7 C5 H5 117.3 . . ? N7 C6 H6A 109.5 . . ? N7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N7 C7 H7A 109.5 . . ? N7 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N7 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C8 N8 C9 121.4(6) . . ? C8 N8 C10 119.7(6) . . ? C9 N8 C10 118.3(6) . . ? O12 C8 N8 123.5(6) . . ? O12 C8 H8 118.3 . . ? N8 C8 H8 118.3 . . ? N8 C9 H9A 109.5 . . ? N8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N8 C10 H10A 109.5 . . ? N8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 N5 O7 120.8(5) . . ? O6 N5 O5 118.7(5) . . ? O7 N5 O5 120.5(5) . . ? C11A N9 C11 16(2) . . ? C11A N9 C12 123(2) . . ? C11 N9 C12 129.8(9) . . ? C11A N9 C13A 141(2) . . ? C11 N9 C13A 149(2) . . ? C12 N9 C13A 76(2) . . ? C11A N9 C13 116(2) . . ? C11 N9 C13 114.0(10) . . ? C12 N9 C13 115.8(9) . . ? C13A N9 C13 40.7(19) . . ? C11A N9 C12A 110(2) . . ? C11 N9 C12A 107.0(16) . . ? C12 N9 C12A 34.8(11) . . ? C13A N9 C12A 103.5(18) . . ? C13 N9 C12A 133.1(14) . . ? N9 C12 H12A 109.5 . . ? N9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N9 C12 H12D 109.5 . . ? H12A C12 H12D 141.1 . . ? H12B C12 H12D 56.3 . . ? H12C C12 H12D 56.3 . . ? N9 C12 H12E 109.5 . . ? H12A C12 H12E 56.3 . . ? H12B C12 H12E 141.1 . . ? H12C C12 H12E 56.3 . . ? H12D C12 H12E 109.5 . . ? N9 C12 H12F 109.5 . . ? H12A C12 H12F 56.3 . . ? H12B C12 H12F 56.3 . . ? H12C C12 H12F 141.1 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? N9 C13 H13A 109.5 . . ? N9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N9 C13 H13D 109.5 . . ? H13A C13 H13D 141.1 . . ? H13B C13 H13D 56.3 . . ? H13C C13 H13D 56.3 . . ? N9 C13 H13E 109.5 . . ? H13A C13 H13E 56.3 . . ? H13B C13 H13E 141.1 . . ? H13C C13 H13E 56.3 . . ? H13D C13 H13E 109.5 . . ? N9 C13 H13F 109.5 . . ? H13A C13 H13F 56.3 . . ? H13B C13 H13F 56.3 . . ? H13C C13 H13F 141.1 . . ? H13D C13 H13F 109.5 . . ? H13E C13 H13F 109.5 . . ? O13 C11 N9 122.6(14) . . ? O13 C11 H11 118.7 . . ? N9 C11 H11 118.7 . . ? N9 C12A H12G 109.5 . . ? N9 C12A H12H 109.5 . . ? H12G C12A H12H 109.5 . . ? N9 C12A H12I 109.5 . . ? H12G C12A H12I 109.5 . . ? H12H C12A H12I 109.5 . . ? N9 C12A H12J 109.5 . . ? H12G C12A H12J 141.1 . . ? H12H C12A H12J 56.3 . . ? H12I C12A H12J 56.3 . . ? N9 C12A H12K 109.5 . . ? H12G C12A H12K 56.3 . . ? H12H C12A H12K 141.1 . . ? H12I C12A H12K 56.3 . . ? H12J C12A H12K 109.5 . . ? N9 C12A H12L 109.5 . . ? H12G C12A H12L 56.3 . . ? H12H C12A H12L 56.3 . . ? H12I C12A H12L 141.1 . . ? H12J C12A H12L 109.5 . . ? H12K C12A H12L 109.5 . . ? N9 C13A H13G 109.5 . . ? N9 C13A H13H 109.5 . . ? H13G C13A H13H 109.5 . . ? N9 C13A H13I 109.5 . . ? H13G C13A H13I 109.5 . . ? H13H C13A H13I 109.5 . . ? N9 C13A H13J 109.5 . . ? H13G C13A H13J 141.1 . . ? H13H C13A H13J 56.3 . . ? H13I C13A H13J 56.3 . . ? N9 C13A H13K 109.5 . . ? H13G C13A H13K 56.3 . . ? H13H C13A H13K 141.1 . . ? H13I C13A H13K 56.3 . . ? H13J C13A H13K 109.5 . . ? N9 C13A H13L 109.5 . . ? H13G C13A H13L 56.3 . . ? H13H C13A H13L 56.3 . . ? H13I C13A H13L 141.1 . . ? H13J C13A H13L 109.5 . . ? H13K C13A H13L 109.5 . . ? N9 C11A O13A 134(4) . . ? N9 C11A H11A 112.9 . . ? O13A C11A H11A 112.9 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.643 _refine_diff_density_min -1.828 _refine_diff_density_rms 0.165 #===END data_[3](NO3)2*3DMF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H39 Br2 N9 O13 Pt2' _chemical_formula_weight 1079.53 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' 'Br' 'Br' -0.2901 2.4595 '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 24.2462(12) _cell_length_b 10.5186(5) _cell_length_c 26.2471(13) _cell_angle_alpha 90.00 _cell_angle_beta 113.6230(10) _cell_angle_gamma 90.00 _cell_volume 6133.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9904 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 28.86 _exptl_crystal_description shard _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 11.788 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.2708 _exptl_absorpt_correction_T_max 0.7187 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 124152 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.92 _reflns_number_total 16123 _reflns_number_gt 12937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. One molecule of DMF was disordered over two orientations. The bond lengths and angles of the two disordered components were restrained to be similar to one another as were the thermal displacement parameters of the ellipsoids. The site occupancy factors of the disordered components allowed to freely refine to a ratio of 52:48. The central nitrogen atom of one of the nitrate counterions (N9) gave non-positive definite ellipsoids upon anisotropic refinement. Attempts to constrain the ellipsoid parameters to match those of other well-behaved nitrate nitrogen atoms in the structure gave rise to spurious large electron density peaks and holes in the difference Fourier map near these atoms. In the final model, N9 was refined isotropically without restraints or constraints. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0106P)^2^+39.9760P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16123 _refine_ls_number_parameters 755 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.103 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.362494(9) 0.21725(2) 0.419591(10) 0.01392(5) Uani 1 1 d . . . Pt2 Pt 0.390920(9) 0.39743(2) 0.493539(10) 0.01387(5) Uani 1 1 d . . . Br1 Br 0.35023(3) 0.04629(6) 0.34647(3) 0.02165(13) Uani 1 1 d . . . Br2 Br 0.43381(3) 0.57701(6) 0.56342(3) 0.02190(13) Uani 1 1 d . . . N1 N 0.2752(2) 0.2677(5) 0.3784(2) 0.0207(11) Uani 1 1 d . . . H1A H 0.2731 0.3407 0.3592 0.031 Uiso 1 1 calc R . . H1B H 0.2582 0.2803 0.4033 0.031 Uiso 1 1 calc R . . H1C H 0.2552 0.2047 0.3544 0.031 Uiso 1 1 calc R . . N2 N 0.3366(2) 0.0826(5) 0.4607(2) 0.0219(12) Uani 1 1 d . . . H2A H 0.3019 0.1076 0.4635 0.033 Uiso 1 1 calc R . . H2B H 0.3659 0.0720 0.4954 0.033 Uiso 1 1 calc R . . H2C H 0.3302 0.0078 0.4418 0.033 Uiso 1 1 calc R . . N3 N 0.3134(2) 0.4986(5) 0.4649(2) 0.0205(11) Uani 1 1 d . . . H3A H 0.3120 0.5488 0.4926 0.031 Uiso 1 1 calc R . . H3B H 0.2814 0.4444 0.4533 0.031 Uiso 1 1 calc R . . H3C H 0.3118 0.5482 0.4359 0.031 Uiso 1 1 calc R . . N4 N 0.3675(2) 0.3024(5) 0.5489(2) 0.0175(11) Uani 1 1 d . . . H4A H 0.3912 0.2325 0.5612 0.026 Uiso 1 1 calc R . . H4B H 0.3282 0.2781 0.5322 0.026 Uiso 1 1 calc R . . H4C H 0.3724 0.3540 0.5782 0.026 Uiso 1 1 calc R . . O1 O 0.38686(18) 0.3433(4) 0.37378(18) 0.0173(9) Uani 1 1 d . . . O2 O 0.44983(17) 0.1629(4) 0.45892(17) 0.0154(8) Uani 1 1 d . . . O3 O 0.41383(18) 0.4978(4) 0.43919(18) 0.0181(9) Uani 1 1 d . . . O4 O 0.47211(17) 0.3106(4) 0.52661(18) 0.0161(9) Uani 1 1 d . . . C1 C 0.4062(3) 0.4535(6) 0.3916(3) 0.0192(13) Uani 1 1 d . . . C2 C 0.4197(3) 0.5414(6) 0.3535(3) 0.0235(14) Uani 1 1 d . . . H2D H 0.4525 0.5987 0.3753 0.035 Uiso 1 1 calc R . . H2E H 0.3837 0.5914 0.3320 0.035 Uiso 1 1 calc R . . H2F H 0.4317 0.4918 0.3280 0.035 Uiso 1 1 calc R . . C3 C 0.4855(2) 0.2174(5) 0.5032(2) 0.0130(11) Uani 1 1 d . . . C4 C 0.5483(2) 0.1678(6) 0.5299(3) 0.0207(13) Uani 1 1 d . . . H4D H 0.5736 0.2112 0.5142 0.031 Uiso 1 1 calc R . . H4E H 0.5483 0.0762 0.5231 0.031 Uiso 1 1 calc R . . H4F H 0.5641 0.1835 0.5700 0.031 Uiso 1 1 calc R . . Pt3 Pt 0.096084(9) 0.91799(2) 0.480066(10) 0.01388(5) Uani 1 1 d . . . Pt4 Pt 0.142196(9) 0.73647(2) 0.552241(10) 0.01518(5) Uani 1 1 d . . . Br3 Br 0.03812(3) 1.10006(6) 0.41642(3) 0.02332(14) Uani 1 1 d . . . Br4 Br 0.17225(3) 0.56582(7) 0.62693(3) 0.03055(16) Uani 1 1 d . . . N5 N 0.1008(2) 0.8307(5) 0.4135(2) 0.0213(11) Uani 1 1 d . . . H5A H 0.0790 0.7575 0.4064 0.032 Uiso 1 1 calc R . . H5B H 0.1399 0.8122 0.4207 0.032 Uiso 1 1 calc R . . H5C H 0.0856 0.8829 0.3835 0.032 Uiso 1 1 calc R . . N6 N 0.1707(2) 1.0230(5) 0.4942(2) 0.0217(12) Uani 1 1 d . . . H6A H 0.1917 0.9882 0.4757 0.033 Uiso 1 1 calc R . . H6B H 0.1942 1.0240 0.5313 0.033 Uiso 1 1 calc R . . H6C H 0.1598 1.1038 0.4821 0.033 Uiso 1 1 calc R . . N7 N 0.1558(2) 0.6074(5) 0.5016(2) 0.0191(11) Uani 1 1 d . . . H7A H 0.1829 0.6387 0.4888 0.029 Uiso 1 1 calc R . . H7B H 0.1204 0.5912 0.4724 0.029 Uiso 1 1 calc R . . H7C H 0.1703 0.5343 0.5208 0.029 Uiso 1 1 calc R . . N8 N 0.2292(2) 0.7903(5) 0.5787(2) 0.0227(12) Uani 1 1 d . . . H8A H 0.2351 0.8630 0.5990 0.034 Uiso 1 1 calc R . . H8B H 0.2385 0.8043 0.5489 0.034 Uiso 1 1 calc R . . H8C H 0.2533 0.7278 0.6003 0.034 Uiso 1 1 calc R . . O5 O 0.01760(17) 0.8247(4) 0.46191(18) 0.0180(9) Uani 1 1 d . . . O6 O 0.09065(18) 1.0141(4) 0.54511(19) 0.0223(10) Uani 1 1 d . . . O7 O 0.05630(17) 0.6744(4) 0.52810(19) 0.0189(9) Uani 1 1 d . . . O8 O 0.13123(18) 0.8588(4) 0.60740(18) 0.0211(9) Uani 1 1 d . . . C5 C 0.0130(2) 0.7267(6) 0.4883(3) 0.0175(12) Uani 1 1 d . . . C6 C -0.0477(3) 0.6670(6) 0.4713(3) 0.0221(14) Uani 1 1 d . . . H6D H -0.0471 0.5821 0.4561 0.033 Uiso 1 1 calc R . . H6E H -0.0777 0.7197 0.4429 0.033 Uiso 1 1 calc R . . H6F H -0.0579 0.6600 0.5037 0.033 Uiso 1 1 calc R . . C7 C 0.1088(3) 0.9683(6) 0.5941(3) 0.0220(14) Uani 1 1 d . . . C8 C 0.1062(3) 1.0515(7) 0.6386(3) 0.0300(16) Uani 1 1 d . . . H8D H 0.1393 1.1130 0.6496 0.045 Uiso 1 1 calc R . . H8E H 0.1098 0.9997 0.6708 0.045 Uiso 1 1 calc R . . H8F H 0.0676 1.0970 0.6248 0.045 Uiso 1 1 calc R . . N9 N 0.26659(18) 0.7989(4) 0.46133(19) 0.0069(8) Uiso 1 1 d . . . O9 O 0.3083(2) 0.7987(5) 0.4409(2) 0.0342(12) Uani 1 1 d . . . O10 O 0.2754(2) 0.8790(5) 0.4987(2) 0.0345(12) Uani 1 1 d . . . O11 O 0.2273(2) 0.7254(5) 0.4452(2) 0.0340(12) Uani 1 1 d . . . N10 N 0.2015(2) 0.3201(5) 0.4715(2) 0.0217(12) Uani 1 1 d . . . O12 O 0.1663(2) 0.3118(4) 0.4955(2) 0.0373(14) Uani 1 1 d . . . O13 O 0.1927(2) 0.4071(5) 0.4358(3) 0.0440(14) Uani 1 1 d . . . O14 O 0.2434(2) 0.2455(5) 0.4816(3) 0.0473(16) Uani 1 1 d . . . N11 N 0.3219(2) 0.5255(6) 0.6151(2) 0.0257(12) Uani 1 1 d . . . O15 O 0.3221(2) 0.6212(5) 0.6434(2) 0.0323(12) Uani 1 1 d . . . O16 O 0.2867(2) 0.5193(5) 0.5646(2) 0.0297(11) Uani 1 1 d . . . O17 O 0.3566(2) 0.4353(5) 0.6381(2) 0.0353(12) Uani 1 1 d . . . N12 N 0.1699(2) 1.0350(6) 0.3453(3) 0.0324(14) Uani 1 1 d . . . O18 O 0.1833(2) 1.1003(5) 0.3118(2) 0.0305(11) Uani 1 1 d . . . O19 O 0.2033(2) 1.0309(5) 0.3951(2) 0.0392(13) Uani 1 1 d . . . O20 O 0.1228(3) 0.9731(8) 0.3271(3) 0.084(3) Uani 1 1 d . . . C9 C 0.4694(3) 0.9864(5) 0.5996(3) 0.0185(12) Uani 1 1 d . . . H9 H 0.5100 0.9930 0.6035 0.022 Uiso 1 1 calc R . . C10 C 0.5047(3) 0.8181(6) 0.6671(3) 0.0289(16) Uani 1 1 d . . . H10A H 0.5428 0.8380 0.6641 0.043 Uiso 1 1 calc R . . H10B H 0.4945 0.7287 0.6574 0.043 Uiso 1 1 calc R . . H10C H 0.5088 0.8333 0.7053 0.043 Uiso 1 1 calc R . . C11 C 0.3968(3) 0.8808(8) 0.6260(4) 0.041(2) Uani 1 1 d . . . H11A H 0.3685 0.9315 0.5953 0.062 Uiso 1 1 calc R . . H11B H 0.3950 0.9078 0.6610 0.062 Uiso 1 1 calc R . . H11C H 0.3859 0.7907 0.6195 0.062 Uiso 1 1 calc R . . N13 N 0.4572(2) 0.8988(5) 0.6291(2) 0.0217(11) Uani 1 1 d . . . O21 O 0.4323(2) 1.0615(4) 0.5670(2) 0.0262(10) Uani 1 1 d . . . C12 C -0.0261(3) 0.5225(6) 0.6148(3) 0.0235(14) Uani 1 1 d . . . H12 H -0.0482 0.5987 0.6014 0.028 Uiso 1 1 calc R . . C13 C 0.0498(3) 0.6528(6) 0.6839(3) 0.0267(15) Uani 1 1 d . . . H13A H 0.0846 0.6753 0.6756 0.040 Uiso 1 1 calc R . . H13B H 0.0623 0.6467 0.7242 0.040 Uiso 1 1 calc R . . H13C H 0.0188 0.7185 0.6690 0.040 Uiso 1 1 calc R . . C14 C 0.0629(3) 0.4182(6) 0.6807(3) 0.0276(15) Uani 1 1 d . . . H14A H 0.0381 0.3415 0.6684 0.041 Uiso 1 1 calc R . . H14B H 0.0804 0.4220 0.7214 0.041 Uiso 1 1 calc R . . H14C H 0.0953 0.4156 0.6673 0.041 Uiso 1 1 calc R . . N14 N 0.0256(2) 0.5306(5) 0.6582(2) 0.0193(11) Uani 1 1 d . . . O22 O -0.04786(19) 0.4219(4) 0.5902(2) 0.0252(10) Uani 1 1 d . . . C15 C 0.2546(3) 0.6281(8) 0.3291(3) 0.0390(19) Uani 1 1 d . . . H15 H 0.2473 0.6690 0.3581 0.047 Uiso 1 1 calc R . . C16 C 0.2215(5) 0.8264(9) 0.2821(6) 0.103(5) Uani 1 1 d . . . H16A H 0.2500 0.8844 0.2761 0.155 Uiso 1 1 calc R . . H16B H 0.2187 0.8470 0.3174 0.155 Uiso 1 1 calc R . . H16C H 0.1818 0.8355 0.2516 0.155 Uiso 1 1 calc R . . C17 C 0.2544(7) 0.646(2) 0.2386(5) 0.153(8) Uani 1 1 d . . . H17A H 0.2775 0.7083 0.2275 0.229 Uiso 1 1 calc R . . H17B H 0.2162 0.6284 0.2071 0.229 Uiso 1 1 calc R . . H17C H 0.2776 0.5669 0.2500 0.229 Uiso 1 1 calc R . . N15 N 0.2426(3) 0.6948(6) 0.2839(3) 0.0388(16) Uani 1 1 d . . . O23 O 0.2736(2) 0.5214(6) 0.3385(3) 0.061(2) Uani 1 1 d . . . C18 C 0.5155(4) 0.0734(7) 0.7527(3) 0.0363(18) Uani 1 1 d . . . H18 H 0.5490 0.0291 0.7788 0.044 Uiso 1 1 calc R . . C19 C 0.5876(4) 0.1954(7) 0.7309(3) 0.0408(19) Uani 1 1 d . . . H19A H 0.5954 0.2859 0.7397 0.061 Uiso 1 1 calc R . . H19B H 0.5926 0.1763 0.6965 0.061 Uiso 1 1 calc R . . H19C H 0.6159 0.1443 0.7614 0.061 Uiso 1 1 calc R . . C20 C 0.4790(4) 0.2418(7) 0.6838(3) 0.0366(18) Uani 1 1 d . . . H20A H 0.4399 0.2106 0.6812 0.055 Uiso 1 1 calc R . . H20B H 0.4809 0.2357 0.6473 0.055 Uiso 1 1 calc R . . H20C H 0.4841 0.3307 0.6960 0.055 Uiso 1 1 calc R . . N16 N 0.5266(3) 0.1655(5) 0.7237(3) 0.0336(15) Uani 1 1 d . . . O24 O 0.4652(3) 0.0410(5) 0.7486(2) 0.0468(15) Uani 1 1 d . . . C21 C 0.9830(3) 0.5459(6) 0.7755(3) 0.0247(14) Uani 1 1 d . . . H21 H 1.0094 0.4751 0.7876 0.030 Uiso 1 1 calc R . . C22 C 0.9123(3) 0.4035(7) 0.7066(3) 0.0339(17) Uani 1 1 d . . . H22A H 0.9475 0.3477 0.7180 0.051 Uiso 1 1 calc R . . H22B H 0.8951 0.4132 0.6661 0.051 Uiso 1 1 calc R . . H22C H 0.8821 0.3662 0.7182 0.051 Uiso 1 1 calc R . . C23 C 0.8870(4) 0.6301(7) 0.7128(4) 0.046(2) Uani 1 1 d . . . H23A H 0.9064 0.7105 0.7294 0.069 Uiso 1 1 calc R . . H23B H 0.8532 0.6135 0.7234 0.069 Uiso 1 1 calc R . . H23C H 0.8722 0.6357 0.6722 0.069 Uiso 1 1 calc R . . N17 N 0.9303(3) 0.5277(5) 0.7326(2) 0.0276(13) Uani 1 1 d . . . O25 O 1.0001(2) 0.6467(5) 0.8005(2) 0.0344(12) Uani 1 1 d . . . N18 N 0.2860(3) 0.1934(6) 0.6805(3) 0.0345(14) Uani 1 1 d DU . . O26A O 0.2388(9) 0.054(2) 0.6106(11) 0.045(3) Uani 0.521(8) 1 d PDU A 1 C24A C 0.2891(6) 0.0825(12) 0.6569(6) 0.031(3) Uani 0.521(8) 1 d PDU A 1 H24A H 0.3232 0.0283 0.6711 0.037 Uiso 0.521(8) 1 calc PR A 1 C25A C 0.3408(7) 0.2338(15) 0.7290(6) 0.044(4) Uani 0.521(8) 1 d PDU A 1 H25A H 0.3734 0.1728 0.7348 0.065 Uiso 0.521(8) 1 calc PR A 1 H25B H 0.3320 0.2368 0.7623 0.065 Uiso 0.521(8) 1 calc PR A 1 H25C H 0.3533 0.3183 0.7219 0.065 Uiso 0.521(8) 1 calc PR A 1 C26A C 0.2392(7) 0.2762(14) 0.6549(8) 0.052(4) Uani 0.521(8) 1 d PDU A 1 H26A H 0.2537 0.3501 0.6412 0.078 Uiso 0.521(8) 1 calc PR A 1 H26B H 0.2228 0.3042 0.6817 0.078 Uiso 0.521(8) 1 calc PR A 1 H26C H 0.2076 0.2333 0.6237 0.078 Uiso 0.521(8) 1 calc PR A 1 O26B O 0.2541(10) 0.039(2) 0.6158(12) 0.045(3) Uani 0.479(8) 1 d PDU A 2 C24B C 0.2479(7) 0.1653(14) 0.6292(6) 0.037(3) Uani 0.479(8) 1 d PDU A 2 H24B H 0.2199 0.2237 0.6047 0.044 Uiso 0.479(8) 1 calc PR A 2 C25B C 0.2825(9) 0.3193(15) 0.7048(8) 0.053(4) Uani 0.479(8) 1 d PDU A 2 H25D H 0.3230 0.3465 0.7298 0.079 Uiso 0.479(8) 1 calc PR A 2 H25E H 0.2571 0.3126 0.7257 0.079 Uiso 0.479(8) 1 calc PR A 2 H25F H 0.2652 0.3817 0.6748 0.079 Uiso 0.479(8) 1 calc PR A 2 C26B C 0.3232(8) 0.1045(16) 0.7181(7) 0.049(4) Uani 0.479(8) 1 d PDU A 2 H26D H 0.3171 0.0208 0.7003 0.073 Uiso 0.479(8) 1 calc PR A 2 H26E H 0.3131 0.1001 0.7507 0.073 Uiso 0.479(8) 1 calc PR A 2 H26F H 0.3653 0.1301 0.7298 0.073 Uiso 0.479(8) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01253(9) 0.01172(10) 0.01566(12) 0.00172(9) 0.00370(8) 0.00045(8) Pt2 0.01333(9) 0.01152(10) 0.01609(12) 0.00146(9) 0.00519(8) 0.00190(8) Br1 0.0224(3) 0.0183(3) 0.0211(3) -0.0027(2) 0.0054(3) -0.0002(2) Br2 0.0233(3) 0.0176(3) 0.0237(4) -0.0050(3) 0.0083(3) -0.0006(2) N1 0.017(2) 0.020(3) 0.021(3) 0.004(2) 0.004(2) 0.004(2) N2 0.020(2) 0.016(3) 0.028(3) 0.005(2) 0.009(2) -0.002(2) N3 0.015(2) 0.016(2) 0.029(3) -0.001(2) 0.007(2) 0.0017(19) N4 0.020(2) 0.015(2) 0.018(3) 0.004(2) 0.008(2) 0.0037(19) O1 0.020(2) 0.017(2) 0.017(2) 0.0012(17) 0.0094(18) 0.0009(16) O2 0.0129(18) 0.015(2) 0.018(2) 0.0010(17) 0.0068(17) 0.0026(15) O3 0.024(2) 0.014(2) 0.018(2) 0.0011(17) 0.0100(19) -0.0011(16) O4 0.0121(18) 0.016(2) 0.018(2) 0.0009(17) 0.0044(17) 0.0020(15) C1 0.014(3) 0.019(3) 0.023(4) 0.005(3) 0.006(2) 0.005(2) C2 0.023(3) 0.022(3) 0.027(4) 0.007(3) 0.011(3) -0.002(2) C3 0.011(2) 0.014(3) 0.012(3) 0.003(2) 0.002(2) 0.000(2) C4 0.014(3) 0.018(3) 0.029(4) 0.004(3) 0.007(3) 0.003(2) Pt3 0.01234(9) 0.01142(10) 0.01681(12) -0.00255(9) 0.00473(8) 0.00030(8) Pt4 0.01262(9) 0.01621(11) 0.01631(12) 0.00018(9) 0.00536(9) 0.00133(8) Br3 0.0248(3) 0.0151(3) 0.0251(4) 0.0004(3) 0.0049(3) 0.0045(2) Br4 0.0265(3) 0.0353(4) 0.0303(4) 0.0156(3) 0.0119(3) 0.0058(3) N5 0.022(3) 0.020(3) 0.022(3) -0.004(2) 0.009(2) 0.001(2) N6 0.021(3) 0.014(3) 0.029(3) 0.001(2) 0.008(2) -0.002(2) N7 0.023(2) 0.014(2) 0.019(3) 0.003(2) 0.008(2) 0.004(2) N8 0.014(2) 0.025(3) 0.024(3) 0.001(2) 0.003(2) 0.001(2) O5 0.0116(18) 0.016(2) 0.026(3) -0.0053(18) 0.0070(18) 0.0002(15) O6 0.019(2) 0.020(2) 0.026(3) -0.012(2) 0.0081(19) -0.0007(17) O7 0.0140(19) 0.017(2) 0.026(3) 0.0012(18) 0.0091(18) -0.0013(16) O8 0.022(2) 0.024(2) 0.018(2) 0.0010(19) 0.0073(19) 0.0040(18) C5 0.014(3) 0.018(3) 0.021(3) -0.008(3) 0.008(2) 0.004(2) C6 0.013(3) 0.019(3) 0.035(4) -0.004(3) 0.012(3) -0.002(2) C7 0.015(3) 0.032(4) 0.018(3) -0.008(3) 0.005(2) -0.003(2) C8 0.028(3) 0.036(4) 0.025(4) -0.017(3) 0.010(3) 0.004(3) O9 0.027(2) 0.033(3) 0.050(4) 0.001(2) 0.022(2) -0.001(2) O10 0.032(3) 0.035(3) 0.041(3) 0.009(2) 0.019(2) 0.001(2) O11 0.027(2) 0.030(3) 0.051(4) 0.011(2) 0.023(2) 0.009(2) N10 0.020(3) 0.014(3) 0.034(4) -0.013(2) 0.014(2) -0.010(2) O12 0.034(3) 0.020(2) 0.072(4) -0.004(3) 0.036(3) 0.000(2) O13 0.047(3) 0.039(3) 0.054(4) -0.012(3) 0.029(3) -0.017(3) O14 0.026(3) 0.030(3) 0.090(5) -0.026(3) 0.028(3) -0.004(2) N11 0.023(3) 0.032(3) 0.023(3) 0.001(3) 0.010(2) 0.003(2) O15 0.026(2) 0.029(3) 0.037(3) -0.005(2) 0.007(2) 0.008(2) O16 0.023(2) 0.042(3) 0.022(3) -0.001(2) 0.007(2) 0.003(2) O17 0.044(3) 0.030(3) 0.034(3) 0.010(2) 0.017(3) 0.018(2) N12 0.022(3) 0.045(4) 0.025(4) -0.003(3) 0.003(3) -0.015(3) O18 0.028(2) 0.038(3) 0.024(3) 0.002(2) 0.008(2) -0.007(2) O19 0.027(3) 0.058(4) 0.028(3) 0.004(3) 0.006(2) -0.008(2) O20 0.078(5) 0.132(7) 0.033(4) -0.008(4) 0.015(4) -0.080(5) C9 0.025(3) 0.015(3) 0.015(3) 0.000(2) 0.008(3) 0.003(2) C10 0.043(4) 0.020(3) 0.023(4) 0.007(3) 0.012(3) 0.003(3) C11 0.029(4) 0.053(5) 0.047(5) 0.008(4) 0.021(4) -0.005(3) N13 0.024(3) 0.019(3) 0.023(3) 0.003(2) 0.011(2) 0.002(2) O21 0.030(2) 0.016(2) 0.025(3) -0.0001(19) 0.003(2) 0.0048(18) C12 0.024(3) 0.023(3) 0.023(4) -0.003(3) 0.010(3) 0.000(3) C13 0.036(4) 0.020(3) 0.019(4) -0.002(3) 0.006(3) -0.007(3) C14 0.028(3) 0.020(3) 0.032(4) 0.005(3) 0.009(3) 0.002(3) N14 0.025(3) 0.014(2) 0.018(3) -0.002(2) 0.007(2) -0.004(2) O22 0.026(2) 0.019(2) 0.029(3) -0.011(2) 0.009(2) -0.0066(18) C15 0.032(4) 0.062(6) 0.021(4) 0.004(4) 0.008(3) 0.016(4) C16 0.074(7) 0.030(5) 0.128(12) 0.021(6) -0.041(7) 0.010(5) C17 0.147(15) 0.28(2) 0.040(8) 0.032(12) 0.047(9) 0.037(16) N15 0.040(4) 0.028(3) 0.029(4) 0.011(3) -0.007(3) -0.004(3) O23 0.034(3) 0.047(4) 0.092(6) 0.044(4) 0.014(3) 0.016(3) C18 0.065(5) 0.022(4) 0.028(4) -0.003(3) 0.026(4) 0.001(4) C19 0.058(5) 0.033(4) 0.025(4) 0.007(3) 0.010(4) -0.002(4) C20 0.061(5) 0.024(4) 0.028(4) 0.006(3) 0.021(4) 0.008(3) N16 0.058(4) 0.019(3) 0.028(4) 0.002(3) 0.020(3) 0.002(3) O24 0.077(4) 0.031(3) 0.043(4) 0.001(3) 0.035(3) -0.001(3) C21 0.029(3) 0.024(3) 0.023(4) 0.005(3) 0.012(3) 0.005(3) C22 0.036(4) 0.031(4) 0.035(5) -0.001(3) 0.015(3) -0.003(3) C23 0.048(5) 0.034(4) 0.036(5) -0.004(4) -0.005(4) 0.015(4) N17 0.032(3) 0.025(3) 0.023(3) 0.000(2) 0.008(3) 0.004(2) O25 0.039(3) 0.030(3) 0.031(3) -0.007(2) 0.012(2) -0.003(2) N18 0.039(3) 0.025(3) 0.034(3) -0.003(3) 0.009(3) -0.003(2) O26A 0.032(8) 0.044(5) 0.036(5) -0.018(4) -0.009(5) -0.003(5) C24A 0.033(5) 0.029(5) 0.030(5) -0.002(4) 0.012(4) 0.001(4) C25A 0.060(8) 0.041(7) 0.025(7) -0.008(6) 0.013(6) -0.019(6) C26A 0.047(7) 0.034(7) 0.074(9) -0.002(7) 0.022(7) -0.002(6) O26B 0.032(8) 0.044(5) 0.036(5) -0.018(4) -0.009(5) -0.003(5) C24B 0.036(5) 0.033(5) 0.034(6) -0.002(5) 0.008(5) 0.006(5) C25B 0.071(9) 0.041(8) 0.035(8) -0.011(7) 0.010(7) 0.004(7) C26B 0.055(8) 0.048(8) 0.033(8) 0.006(7) 0.007(7) 0.009(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 N1 2.023(5) . ? Pt1 N2 2.028(5) . ? Pt1 O1 2.030(4) . ? Pt1 O2 2.031(4) . ? Pt1 Br1 2.5590(7) . ? Pt1 Pt2 2.6004(3) . ? Pt2 O3 2.023(4) . ? Pt2 O4 2.023(4) . ? Pt2 N4 2.024(5) . ? Pt2 N3 2.025(5) . ? Pt2 Br2 2.5465(7) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 H4A 0.9100 . ? N4 H4B 0.9100 . ? N4 H4C 0.9100 . ? O1 C1 1.268(7) . ? O2 C3 1.274(7) . ? O3 C1 1.274(7) . ? O4 C3 1.267(7) . ? C1 C2 1.493(8) . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C2 H2F 0.9800 . ? C3 C4 1.491(7) . ? C4 H4D 0.9800 . ? C4 H4E 0.9800 . ? C4 H4F 0.9800 . ? Pt3 N5 2.016(5) . ? Pt3 O5 2.021(4) . ? Pt3 N6 2.023(5) . ? Pt3 O6 2.033(4) . ? Pt3 Br3 2.5597(7) . ? Pt3 Pt4 2.6052(3) . ? Pt4 N7 2.017(5) . ? Pt4 N8 2.020(5) . ? Pt4 O7 2.026(4) . ? Pt4 O8 2.033(4) . ? Pt4 Br4 2.5399(7) . ? N5 H5A 0.9100 . ? N5 H5B 0.9100 . ? N5 H5C 0.9100 . ? N6 H6A 0.9100 . ? N6 H6B 0.9100 . ? N6 H6C 0.9100 . ? N7 H7A 0.9100 . ? N7 H7B 0.9100 . ? N7 H7C 0.9100 . ? N8 H8A 0.9100 . ? N8 H8B 0.9100 . ? N8 H8C 0.9100 . ? O5 C5 1.271(7) . ? O6 C7 1.275(8) . ? O7 C5 1.271(7) . ? O8 C7 1.261(8) . ? C5 C6 1.494(8) . ? C6 H6D 0.9800 . ? C6 H6E 0.9800 . ? C6 H6F 0.9800 . ? C7 C8 1.481(9) . ? C8 H8D 0.9800 . ? C8 H8E 0.9800 . ? C8 H8F 0.9800 . ? N9 O11 1.168(6) . ? N9 O10 1.245(7) . ? N9 O9 1.322(6) . ? N10 O14 1.226(7) . ? N10 O12 1.248(7) . ? N10 O13 1.266(8) . ? N11 O15 1.249(7) . ? N11 O17 1.251(7) . ? N11 O16 1.258(7) . ? N12 O19 1.231(7) . ? N12 O20 1.233(7) . ? N12 O18 1.256(7) . ? C9 O21 1.245(7) . ? C9 N13 1.311(8) . ? C9 H9 0.9500 . ? C10 N13 1.457(8) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N13 1.445(8) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 O22 1.242(7) . ? C12 N14 1.315(8) . ? C12 H12 0.9500 . ? C13 N14 1.461(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N14 1.462(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 O23 1.200(9) . ? C15 N15 1.308(10) . ? C15 H15 0.9500 . ? C16 N15 1.469(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N15 1.426(15) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 O24 1.228(9) . ? C18 N16 1.326(9) . ? C18 H18 0.9500 . ? C19 N16 1.447(10) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N16 1.450(9) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 O25 1.229(8) . ? C21 N17 1.336(8) . ? C21 H21 0.9500 . ? C22 N17 1.458(9) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 N17 1.447(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? N18 C24B 1.324(14) . ? N18 C24A 1.336(13) . ? N18 C26A 1.374(14) . ? N18 C26B 1.396(14) . ? N18 C25B 1.486(14) . ? N18 C25A 1.487(13) . ? O26A C24A 1.365(17) . ? C24A H24A 0.9500 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? O26B C24B 1.398(19) . ? C24B H24B 0.9500 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C26B H26D 0.9800 . ? C26B H26E 0.9800 . ? C26B H26F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 N2 89.2(2) . . ? N1 Pt1 O1 90.16(19) . . ? N2 Pt1 O1 175.9(2) . . ? N1 Pt1 O2 178.2(2) . . ? N2 Pt1 O2 90.88(18) . . ? O1 Pt1 O2 89.62(16) . . ? N1 Pt1 Br1 90.09(15) . . ? N2 Pt1 Br1 86.62(16) . . ? O1 Pt1 Br1 89.34(12) . . ? O2 Pt1 Br1 88.13(12) . . ? N1 Pt1 Pt2 96.60(15) . . ? N2 Pt1 Pt2 99.06(16) . . ? O1 Pt1 Pt2 85.02(12) . . ? O2 Pt1 Pt2 85.15(11) . . ? Br1 Pt1 Pt2 171.248(17) . . ? O3 Pt2 O4 92.48(16) . . ? O3 Pt2 N4 178.14(18) . . ? O4 Pt2 N4 88.51(18) . . ? O3 Pt2 N3 86.59(19) . . ? O4 Pt2 N3 174.64(19) . . ? N4 Pt2 N3 92.3(2) . . ? O3 Pt2 Br2 88.42(12) . . ? O4 Pt2 Br2 88.83(12) . . ? N4 Pt2 Br2 90.02(15) . . ? N3 Pt2 Br2 85.87(15) . . ? O3 Pt2 Pt1 85.39(12) . . ? O4 Pt2 Pt1 84.97(12) . . ? N4 Pt2 Pt1 96.28(15) . . ? N3 Pt2 Pt1 100.20(15) . . ? Br2 Pt2 Pt1 171.039(17) . . ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Pt2 N3 H3A 109.5 . . ? Pt2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Pt2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Pt2 N4 H4A 109.5 . . ? Pt2 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Pt2 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C1 O1 Pt1 122.0(4) . . ? C3 O2 Pt1 121.7(3) . . ? C1 O3 Pt2 121.8(4) . . ? C3 O4 Pt2 122.4(4) . . ? O1 C1 O3 125.7(6) . . ? O1 C1 C2 117.8(6) . . ? O3 C1 C2 116.5(6) . . ? C1 C2 H2D 109.5 . . ? C1 C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? C1 C2 H2F 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? O4 C3 O2 125.3(5) . . ? O4 C3 C4 117.0(5) . . ? O2 C3 C4 117.6(5) . . ? C3 C4 H4D 109.5 . . ? C3 C4 H4E 109.5 . . ? H4D C4 H4E 109.5 . . ? C3 C4 H4F 109.5 . . ? H4D C4 H4F 109.5 . . ? H4E C4 H4F 109.5 . . ? N5 Pt3 O5 87.09(19) . . ? N5 Pt3 N6 92.9(2) . . ? O5 Pt3 N6 175.36(19) . . ? N5 Pt3 O6 177.2(2) . . ? O5 Pt3 O6 93.89(17) . . ? N6 Pt3 O6 85.9(2) . . ? N5 Pt3 Br3 88.99(15) . . ? O5 Pt3 Br3 89.47(12) . . ? N6 Pt3 Br3 85.90(15) . . ? O6 Pt3 Br3 88.42(13) . . ? N5 Pt3 Pt4 98.00(15) . . ? O5 Pt3 Pt4 84.53(12) . . ? N6 Pt3 Pt4 100.06(15) . . ? O6 Pt3 Pt4 84.68(13) . . ? Br3 Pt3 Pt4 170.517(18) . . ? N7 Pt4 N8 89.5(2) . . ? N7 Pt4 O7 89.79(19) . . ? N8 Pt4 O7 177.1(2) . . ? N7 Pt4 O8 176.34(19) . . ? N8 Pt4 O8 89.7(2) . . ? O7 Pt4 O8 90.87(17) . . ? N7 Pt4 Br4 87.77(14) . . ? N8 Pt4 Br4 89.72(16) . . ? O7 Pt4 Br4 87.41(12) . . ? O8 Pt4 Br4 88.67(12) . . ? N7 Pt4 Pt3 98.61(14) . . ? N8 Pt4 Pt3 97.46(15) . . ? O7 Pt4 Pt3 85.46(12) . . ? O8 Pt4 Pt3 85.03(12) . . ? Br4 Pt4 Pt3 170.402(18) . . ? Pt3 N5 H5A 109.5 . . ? Pt3 N5 H5B 109.5 . . ? H5A N5 H5B 109.5 . . ? Pt3 N5 H5C 109.5 . . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? Pt3 N6 H6A 109.5 . . ? Pt3 N6 H6B 109.5 . . ? H6A N6 H6B 109.5 . . ? Pt3 N6 H6C 109.5 . . ? H6A N6 H6C 109.5 . . ? H6B N6 H6C 109.5 . . ? Pt4 N7 H7A 109.5 . . ? Pt4 N7 H7B 109.5 . . ? H7A N7 H7B 109.5 . . ? Pt4 N7 H7C 109.5 . . ? H7A N7 H7C 109.5 . . ? H7B N7 H7C 109.5 . . ? Pt4 N8 H8A 109.5 . . ? Pt4 N8 H8B 109.5 . . ? H8A N8 H8B 109.5 . . ? Pt4 N8 H8C 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? C5 O5 Pt3 123.0(4) . . ? C7 O6 Pt3 123.1(4) . . ? C5 O7 Pt4 121.6(4) . . ? C7 O8 Pt4 123.1(4) . . ? O7 C5 O5 125.1(5) . . ? O7 C5 C6 117.0(6) . . ? O5 C5 C6 117.9(5) . . ? C5 C6 H6D 109.5 . . ? C5 C6 H6E 109.5 . . ? H6D C6 H6E 109.5 . . ? C5 C6 H6F 109.5 . . ? H6D C6 H6F 109.5 . . ? H6E C6 H6F 109.5 . . ? O8 C7 O6 124.1(6) . . ? O8 C7 C8 118.1(6) . . ? O6 C7 C8 117.7(6) . . ? C7 C8 H8D 109.5 . . ? C7 C8 H8E 109.5 . . ? H8D C8 H8E 109.5 . . ? C7 C8 H8F 109.5 . . ? H8D C8 H8F 109.5 . . ? H8E C8 H8F 109.5 . . ? O11 N9 O10 126.2(5) . . ? O11 N9 O9 119.9(5) . . ? O10 N9 O9 113.9(4) . . ? O14 N10 O12 121.4(6) . . ? O14 N10 O13 120.0(6) . . ? O12 N10 O13 118.6(5) . . ? O15 N11 O17 118.8(6) . . ? O15 N11 O16 120.6(6) . . ? O17 N11 O16 120.6(6) . . ? O19 N12 O20 120.4(6) . . ? O19 N12 O18 121.2(5) . . ? O20 N12 O18 118.4(6) . . ? O21 C9 N13 125.4(6) . . ? O21 C9 H9 117.3 . . ? N13 C9 H9 117.3 . . ? N13 C10 H10A 109.5 . . ? N13 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N13 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N13 C11 H11A 109.5 . . ? N13 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N13 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 N13 C11 121.5(6) . . ? C9 N13 C10 120.6(5) . . ? C11 N13 C10 117.9(6) . . ? O22 C12 N14 124.4(6) . . ? O22 C12 H12 117.8 . . ? N14 C12 H12 117.8 . . ? N14 C13 H13A 109.5 . . ? N14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N14 C14 H14A 109.5 . . ? N14 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N14 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 N14 C13 121.6(5) . . ? C12 N14 C14 121.1(5) . . ? C13 N14 C14 117.2(5) . . ? O23 C15 N15 127.9(8) . . ? O23 C15 H15 116.1 . . ? N15 C15 H15 116.1 . . ? N15 C16 H16A 109.5 . . ? N15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N15 C17 H17A 109.5 . . ? N15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 N15 C17 121.1(10) . . ? C15 N15 C16 118.8(9) . . ? C17 N15 C16 119.8(11) . . ? O24 C18 N16 125.1(8) . . ? O24 C18 H18 117.4 . . ? N16 C18 H18 117.4 . . ? N16 C19 H19A 109.5 . . ? N16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N16 C20 H20A 109.5 . . ? N16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 N16 C19 121.1(7) . . ? C18 N16 C20 122.2(7) . . ? C19 N16 C20 116.7(6) . . ? O25 C21 N17 125.3(6) . . ? O25 C21 H21 117.4 . . ? N17 C21 H21 117.4 . . ? N17 C22 H22A 109.5 . . ? N17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N17 C23 H23A 109.5 . . ? N17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 N17 C23 120.5(6) . . ? C21 N17 C22 121.9(6) . . ? C23 N17 C22 117.5(6) . . ? C24B N18 C24A 58.7(9) . . ? C24B N18 C26A 62.7(10) . . ? C24A N18 C26A 121.0(10) . . ? C24B N18 C26B 124.0(11) . . ? C24A N18 C26B 66.6(9) . . ? C26A N18 C26B 160.5(13) . . ? C24B N18 C25B 119.8(10) . . ? C24A N18 C25B 177.8(11) . . ? C26A N18 C25B 57.8(10) . . ? C26B N18 C25B 115.2(11) . . ? C24B N18 C25A 162.5(11) . . ? C24A N18 C25A 116.8(9) . . ? C26A N18 C25A 121.1(11) . . ? C26B N18 C25A 58.9(10) . . ? C25B N18 C25A 64.1(10) . . ? N18 C24A O26A 114.2(12) . . ? N18 C24A H24A 122.9 . . ? O26A C24A H24A 122.9 . . ? N18 C25A H25A 109.5 . . ? N18 C25A H25B 109.5 . . ? N18 C25A H25C 109.5 . . ? N18 C26A H26A 109.5 . . ? N18 C26A H26B 109.5 . . ? N18 C26A H26C 109.5 . . ? N18 C24B O26B 111.5(13) . . ? N18 C24B H24B 124.2 . . ? O26B C24B H24B 124.2 . . ? N18 C25B H25D 109.5 . . ? N18 C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? N18 C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? N18 C26B H26D 109.5 . . ? N18 C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? N18 C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.92 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.673 _refine_diff_density_min -1.599 _refine_diff_density_rms 0.216 #===END data_[4](NO3)4*4DMF _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H62 F6 N16 O28 Pt4' _chemical_formula_weight 1917.26 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' 'F' 'F' 0.0171 0.0103 '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 C2/c 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' '-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 35.401(4) _cell_length_b 13.8473(14) _cell_length_c 12.8506(13) _cell_angle_alpha 90.00 _cell_angle_beta 107.367(2) _cell_angle_gamma 90.00 _cell_volume 6012.3(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7534 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.06 _exptl_crystal_description shard _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.118 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 9.384 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.2829 _exptl_absorpt_correction_T_max 0.9120 _exptl_absorpt_process_details 'Blessing, 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 45478 _diffrn_reflns_av_R_equivalents 0.0750 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.13 _reflns_number_total 5366 _reflns_number_gt 3877 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Half of the tetranuclear complex is related to the other half by a crystallographic inversion center. Also in the asymmetric unit were the two nitrate counterions and two molecules of DMF. One of the DMF molecules was disordered over two orientations. Similarity restraints were used to model this disorder, and the site occupancy factors refined to a ratio of 56:44. The axial trifluoroacetate ligand of 4 was also disordered. Only one carbon (C1) and one oxygen (O2) atoms were modeled in different orientations using the appropriate similarity restraints. The disordered components refined to site occupancy factors of 52:48. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+22.5580P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5366 _refine_ls_number_parameters 424 _refine_ls_number_restraints 261 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 -0.009 300 91 ' ' 2 0.500 0.500 0.012 300 91 ' ' _platon_squeeze_details ; The disordered electron density resided about crystallographic inversion center. We believe this electron density may correspond to two molecules of diethyl ether (84 e) per void. After drying crystalline samples under vacuum, elemental analyses is consistent with the presence of 4 DMF molecules per complex. Hence, we hypothesize that this density is due to ether, which is much more volatile than DMF ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt2 Pt 0.209193(14) 0.29961(3) 0.49141(4) 0.02871(17) Uani 1 1 d . . . Pt1 Pt 0.150858(15) 0.28792(3) 0.56946(4) 0.03179(17) Uani 1 1 d . A . N1 N 0.1128(3) 0.2212(7) 0.4417(9) 0.043(3) Uani 1 1 d . . . H1A H 0.0887 0.2161 0.4535 0.064 Uiso 1 1 calc R . . H1B H 0.1220 0.1612 0.4339 0.064 Uiso 1 1 calc R . . H1C H 0.1103 0.2562 0.3801 0.064 Uiso 1 1 calc R . . N2 N 0.1653(3) 0.1611(6) 0.6466(9) 0.043(3) Uani 1 1 d . . . H2A H 0.1902 0.1648 0.6938 0.065 Uiso 1 1 calc R . . H2B H 0.1644 0.1137 0.5968 0.065 Uiso 1 1 calc R . . H2C H 0.1479 0.1473 0.6842 0.065 Uiso 1 1 calc R . . N3 N 0.1832(3) 0.2357(7) 0.3456(8) 0.038(3) Uani 1 1 d . . . H3A H 0.2019 0.2053 0.3221 0.057 Uiso 1 1 calc R . . H3B H 0.1709 0.2813 0.2961 0.057 Uiso 1 1 calc R . . H3C H 0.1650 0.1918 0.3532 0.057 Uiso 1 1 calc R . . N4 N 0.2386(3) 0.1802(7) 0.5570(8) 0.032(2) Uani 1 1 d . . . H1N H 0.2252 0.1249 0.5277 0.038 Uiso 1 1 calc R . . H2N H 0.2441 0.1791 0.6317 0.038 Uiso 1 1 calc R . . O3 O 0.1346(3) 0.4185(6) 0.4959(7) 0.040(2) Uani 1 1 d . . . O4 O 0.1839(2) 0.4274(5) 0.4234(6) 0.0317(19) Uani 1 1 d . . . O5 O 0.1869(3) 0.3568(5) 0.7003(6) 0.036(2) Uani 1 1 d . . . O6 O 0.2386(2) 0.3684(5) 0.6325(6) 0.0330(19) Uani 1 1 d . . . C3 C 0.1534(4) 0.4582(8) 0.4380(10) 0.036(3) Uani 1 1 d . . . C4 C 0.1371(4) 0.5511(9) 0.3879(11) 0.049(4) Uani 1 1 d . . . H4A H 0.1541 0.5772 0.3469 0.073 Uiso 1 1 calc R . . H4B H 0.1360 0.5969 0.4452 0.073 Uiso 1 1 calc R . . H4C H 0.1103 0.5410 0.3386 0.073 Uiso 1 1 calc R . . C5 C 0.2215(4) 0.3813(8) 0.7064(9) 0.032(3) Uani 1 1 d . . . C6 C 0.2458(4) 0.4311(9) 0.8071(10) 0.043(3) Uani 1 1 d . . . H6A H 0.2299 0.4817 0.8273 0.065 Uiso 1 1 calc R . . H6B H 0.2691 0.4602 0.7934 0.065 Uiso 1 1 calc R . . H6C H 0.2543 0.3842 0.8666 0.065 Uiso 1 1 calc R . . O1 O 0.1060(4) 0.2981(7) 0.6573(8) 0.054(2) Uani 1 1 d DU . . O2 O 0.0558(6) 0.3405(18) 0.5198(15) 0.081(6) Uani 0.518(17) 1 d PDU A 1 C1 C 0.0724(8) 0.3201(17) 0.618(2) 0.076(4) Uani 0.518(17) 1 d PDU A 1 O2A O 0.0558(6) 0.2431(19) 0.5282(17) 0.079(6) Uani 0.482(17) 1 d PDU A 2 C1A C 0.0720(8) 0.2800(18) 0.620(2) 0.076(4) Uani 0.482(17) 1 d PDU A 2 C2 C 0.0491(7) 0.3073(17) 0.6954(19) 0.091(4) Uani 1 1 d DU . . F1 F 0.0661(4) 0.2691(10) 0.7938(12) 0.124(4) Uani 1 1 d U A . F2 F 0.0389(4) 0.3891(11) 0.7092(10) 0.120(4) Uani 1 1 d U A . F3 F 0.0130(4) 0.2564(15) 0.6561(15) 0.156(5) Uani 1 1 d U A . N5 N 0.1268(4) 0.0318(9) 0.2292(10) 0.058(3) Uani 1 1 d . . . O7 O 0.1083(4) 0.0978(10) 0.2574(11) 0.103(5) Uani 1 1 d . . . O9 O 0.1609(4) 0.0400(7) 0.2260(8) 0.062(3) Uani 1 1 d . . . O8 O 0.1081(3) -0.0495(8) 0.2060(9) 0.066(3) Uani 1 1 d . . . N6 N 0.2756(4) 0.1456(8) 0.8529(9) 0.048(3) Uani 1 1 d . . . O10 O 0.2708(4) 0.1091(9) 0.9350(9) 0.090(4) Uani 1 1 d . . . O11 O 0.3080(4) 0.1463(11) 0.8405(9) 0.091(4) Uani 1 1 d . . . O12 O 0.2477(3) 0.1871(7) 0.7845(8) 0.059(3) Uani 1 1 d . . . N7 N 0.1587(4) -0.1095(7) 0.4493(9) 0.054(3) Uani 1 1 d D . . C7 C 0.1832(4) -0.0364(8) 0.4515(10) 0.051(4) Uani 1 1 d D . . H7 H 0.2073 -0.0492 0.4361 0.061 Uiso 1 1 calc R . . C8 C 0.1205(5) -0.0949(13) 0.4671(14) 0.087(6) Uani 1 1 d D . . H8A H 0.1190 -0.1338 0.5294 0.131 Uiso 1 1 calc R . . H8B H 0.0994 -0.1145 0.4018 0.131 Uiso 1 1 calc R . . H8C H 0.1173 -0.0265 0.4821 0.131 Uiso 1 1 calc R . . C9 C 0.1685(6) -0.2061(9) 0.4221(14) 0.083(6) Uani 1 1 d D . . H9A H 0.1959 -0.2073 0.4199 0.124 Uiso 1 1 calc R . . H9B H 0.1507 -0.2246 0.3506 0.124 Uiso 1 1 calc R . . H9C H 0.1655 -0.2517 0.4774 0.124 Uiso 1 1 calc R . . O13 O 0.1760(3) 0.0475(5) 0.4726(7) 0.048(2) Uani 1 1 d D . . N8 N 0.0660(8) 0.355(2) 0.091(2) 0.078(5) Uani 0.438(19) 1 d PDU B 1 C10 C 0.0975(10) 0.384(3) 0.167(3) 0.073(5) Uani 0.438(19) 1 d PDU B 1 H10 H 0.1101 0.4418 0.1547 0.088 Uiso 0.438(19) 1 calc PR B 1 C11 C 0.0453(13) 0.266(3) 0.105(3) 0.104(11) Uani 0.438(19) 1 d PDU B 1 H11A H 0.0224 0.2566 0.0405 0.156 Uiso 0.219(10) 1 calc PR B 1 H11B H 0.0364 0.2725 0.1697 0.156 Uiso 0.219(10) 1 calc PR B 1 H11C H 0.0633 0.2112 0.1134 0.156 Uiso 0.219(10) 1 calc PR B 1 H11D H 0.0590 0.2369 0.1752 0.156 Uiso 0.219(10) 1 calc PR B 1 H11E H 0.0450 0.2211 0.0460 0.156 Uiso 0.219(10) 1 calc PR B 1 H11F H 0.0181 0.2824 0.1024 0.156 Uiso 0.219(10) 1 calc PR B 1 C12 C 0.0488(13) 0.402(3) -0.012(3) 0.086(7) Uani 0.438(19) 1 d PDU B 1 H12A H 0.0252 0.3665 -0.0544 0.129 Uiso 0.219(10) 1 calc PR B 1 H12B H 0.0681 0.4038 -0.0534 0.129 Uiso 0.219(10) 1 calc PR B 1 H12C H 0.0413 0.4682 0.0002 0.129 Uiso 0.219(10) 1 calc PR B 1 H12D H 0.0645 0.4592 -0.0173 0.129 Uiso 0.219(10) 1 calc PR B 1 H12E H 0.0216 0.4218 -0.0184 0.129 Uiso 0.219(10) 1 calc PR B 1 H12F H 0.0485 0.3575 -0.0719 0.129 Uiso 0.219(10) 1 calc PR B 1 O14 O 0.1118(19) 0.341(6) 0.256(4) 0.068(7) Uani 0.438(19) 1 d PDU B 1 N8A N 0.0625(7) 0.3962(16) 0.1231(16) 0.076(4) Uani 0.562(19) 1 d PDU B 2 C10A C 0.0993(8) 0.370(3) 0.172(3) 0.074(4) Uani 0.562(19) 1 d PDU B 2 H10A H 0.1187 0.3803 0.1360 0.088 Uiso 0.562(19) 1 calc PR B 2 C11A C 0.0315(8) 0.375(3) 0.173(2) 0.091(9) Uani 0.562(19) 1 d PDU B 2 H11G H 0.0060 0.3980 0.1258 0.137 Uiso 0.281(10) 1 calc PR B 2 H11H H 0.0376 0.4069 0.2442 0.137 Uiso 0.281(10) 1 calc PR B 2 H11I H 0.0301 0.3048 0.1832 0.137 Uiso 0.281(10) 1 calc PR B 2 H11J H 0.0431 0.3418 0.2430 0.137 Uiso 0.281(10) 1 calc PR B 2 H11K H 0.0116 0.3329 0.1247 0.137 Uiso 0.281(10) 1 calc PR B 2 H11L H 0.0190 0.4350 0.1856 0.137 Uiso 0.281(10) 1 calc PR B 2 C12A C 0.0522(11) 0.453(3) 0.025(2) 0.088(7) Uani 0.562(19) 1 d PDU B 2 H12G H 0.0235 0.4644 0.0002 0.132 Uiso 0.281(10) 1 calc PR B 2 H12H H 0.0600 0.4189 -0.0324 0.132 Uiso 0.281(10) 1 calc PR B 2 H12I H 0.0660 0.5155 0.0390 0.132 Uiso 0.281(10) 1 calc PR B 2 H12J H 0.0762 0.4681 0.0043 0.132 Uiso 0.281(10) 1 calc PR B 2 H12K H 0.0397 0.5137 0.0369 0.132 Uiso 0.281(10) 1 calc PR B 2 H12L H 0.0337 0.4170 -0.0345 0.132 Uiso 0.281(10) 1 calc PR B 2 O14A O 0.1098(15) 0.332(4) 0.264(3) 0.068(6) Uani 0.562(19) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt2 0.0419(3) 0.0170(2) 0.0249(3) -0.00084(16) 0.0064(2) 0.00151(18) Pt1 0.0422(3) 0.0212(3) 0.0300(3) 0.00034(18) 0.0078(2) 0.00111(19) N1 0.037(7) 0.043(6) 0.042(7) -0.001(5) 0.003(5) -0.004(5) N2 0.066(8) 0.016(5) 0.052(7) -0.001(4) 0.024(6) -0.014(5) N3 0.051(7) 0.031(5) 0.029(6) 0.001(4) 0.005(5) 0.003(5) N4 0.036(6) 0.025(5) 0.029(5) 0.007(4) 0.000(5) -0.016(4) O3 0.052(6) 0.030(4) 0.041(5) 0.002(4) 0.016(5) 0.002(4) O4 0.043(5) 0.017(4) 0.031(5) 0.004(3) 0.005(4) 0.000(3) O5 0.053(6) 0.027(4) 0.033(5) -0.004(3) 0.021(4) 0.008(4) O6 0.049(5) 0.022(4) 0.024(4) -0.004(3) 0.004(4) 0.001(4) C3 0.043(8) 0.023(6) 0.039(7) -0.004(5) 0.008(6) 0.002(5) C4 0.069(10) 0.031(7) 0.042(8) 0.015(6) 0.009(7) 0.006(6) C5 0.040(8) 0.021(6) 0.039(7) 0.003(5) 0.016(6) 0.008(5) C6 0.064(10) 0.029(6) 0.041(8) -0.015(5) 0.022(7) -0.008(6) O1 0.070(6) 0.066(6) 0.040(5) -0.008(4) 0.038(5) -0.007(5) O2 0.078(11) 0.100(12) 0.070(10) 0.001(10) 0.030(9) -0.012(10) C1 0.080(7) 0.092(8) 0.068(7) -0.004(7) 0.039(7) -0.010(7) O2A 0.077(11) 0.101(12) 0.070(10) -0.002(10) 0.039(9) -0.039(10) C1A 0.080(7) 0.095(8) 0.067(7) -0.003(7) 0.042(7) -0.009(7) C2 0.085(7) 0.111(8) 0.088(7) -0.007(7) 0.044(6) -0.002(7) F1 0.126(10) 0.132(10) 0.135(10) 0.042(8) 0.072(8) 0.019(8) F2 0.116(10) 0.135(10) 0.103(9) -0.016(7) 0.024(7) 0.004(8) F3 0.080(9) 0.209(13) 0.187(12) -0.044(11) 0.052(9) -0.041(9) N5 0.065(10) 0.055(8) 0.051(8) -0.021(6) 0.013(7) 0.016(7) O7 0.073(9) 0.103(10) 0.108(10) -0.063(8) -0.011(7) 0.026(7) O9 0.077(8) 0.038(6) 0.066(7) -0.006(5) 0.012(6) -0.003(5) O8 0.061(7) 0.061(7) 0.075(8) -0.010(6) 0.021(6) -0.011(6) N6 0.067(9) 0.039(6) 0.035(7) -0.007(5) 0.010(7) 0.002(6) O10 0.107(10) 0.094(9) 0.056(7) 0.043(7) 0.004(7) -0.038(8) O11 0.076(9) 0.144(13) 0.057(8) 0.005(8) 0.027(7) 0.027(9) O12 0.069(7) 0.052(6) 0.043(6) 0.007(5) -0.003(5) 0.018(5) N7 0.076(9) 0.037(6) 0.047(7) -0.018(5) 0.017(7) -0.026(6) C7 0.079(11) 0.029(7) 0.040(8) 0.001(6) 0.013(7) -0.016(7) C8 0.127(18) 0.090(14) 0.062(11) -0.022(10) 0.054(12) -0.053(12) C9 0.133(18) 0.041(9) 0.060(11) 0.013(7) 0.006(11) -0.024(9) O13 0.072(7) 0.022(4) 0.048(6) -0.005(4) 0.012(5) -0.006(4) N8 0.081(8) 0.094(11) 0.046(8) 0.009(7) 0.000(7) 0.017(8) C10 0.079(8) 0.089(11) 0.041(8) 0.008(7) 0.002(7) 0.019(8) C11 0.096(19) 0.117(19) 0.071(18) 0.018(17) -0.019(17) -0.007(17) C12 0.091(13) 0.108(15) 0.051(12) 0.013(12) 0.008(12) 0.015(13) O14 0.081(11) 0.073(13) 0.037(11) 0.004(10) -0.002(10) 0.017(10) N8A 0.079(8) 0.096(10) 0.042(8) 0.011(7) 0.001(7) 0.015(8) C10A 0.079(8) 0.089(10) 0.042(7) 0.008(7) 0.002(7) 0.019(8) C11A 0.069(15) 0.122(19) 0.066(15) 0.024(15) -0.004(13) -0.001(15) C12A 0.095(12) 0.111(15) 0.047(12) 0.015(11) 0.006(11) 0.014(13) O14A 0.082(10) 0.068(12) 0.039(9) 0.003(8) -0.003(9) 0.018(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 Pt2 N4 2.002(9) . ? Pt2 N3 2.028(9) . ? Pt2 O6 2.037(7) . ? Pt2 O4 2.057(7) . ? Pt2 N4 2.136(10) 7_556 ? Pt2 Pt1 2.5561(7) . ? Pt2 Pt2 3.1470(10) 7_556 ? Pt1 N2 2.006(9) . ? Pt1 N1 2.011(10) . ? Pt1 O5 2.021(8) . ? Pt1 O3 2.043(8) . ? Pt1 O1 2.210(9) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3A 0.9100 . ? N3 H3B 0.9100 . ? N3 H3C 0.9100 . ? N4 Pt2 2.136(10) 7_556 ? N4 H1N 0.9200 . ? N4 H2N 0.9200 . ? O3 C3 1.260(14) . ? O4 C3 1.225(14) . ? O5 C5 1.253(14) . ? O6 C5 1.281(13) . ? C3 C4 1.478(16) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.492(16) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O1 C1A 1.18(3) . ? O1 C1 1.18(3) . ? O2 C1 1.26(3) . ? C1 C2 1.48(3) . ? O2A C1A 1.26(3) . ? C1A C2 1.48(3) . ? C2 F2 1.22(2) . ? C2 F1 1.34(2) . ? C2 F3 1.41(3) . ? N5 O9 1.224(15) . ? N5 O7 1.241(15) . ? N5 O8 1.295(16) . ? N6 O11 1.203(16) . ? N6 O10 1.228(14) . ? N6 O12 1.250(14) . ? N7 C7 1.328(14) . ? N7 C8 1.450(18) . ? N7 C9 1.451(15) . ? C7 O13 1.236(13) . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? N8 C10 1.31(2) . ? N8 C12 1.44(2) . ? N8 C11 1.46(2) . ? C10 O14 1.245(18) . ? C10 H10 0.9500 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? N8A C10A 1.32(2) . ? N8A C12A 1.445(19) . ? N8A C11A 1.46(2) . ? C10A O14A 1.244(17) . ? C10A H10A 0.9500 . ? C11A H11G 0.9800 . ? C11A H11H 0.9800 . ? C11A H11I 0.9800 . ? C11A H11J 0.9800 . ? C11A H11K 0.9800 . ? C11A H11L 0.9800 . ? C12A H12G 0.9800 . ? C12A H12H 0.9800 . ? C12A H12I 0.9800 . ? C12A H12J 0.9800 . ? C12A H12K 0.9800 . ? C12A H12L 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pt2 N3 93.7(4) . . ? N4 Pt2 O6 87.0(3) . . ? N3 Pt2 O6 175.4(4) . . ? N4 Pt2 O4 174.7(3) . . ? N3 Pt2 O4 87.9(3) . . ? O6 Pt2 O4 91.0(3) . . ? N4 Pt2 N4 81.0(4) . 7_556 ? N3 Pt2 N4 89.0(4) . 7_556 ? O6 Pt2 N4 86.7(3) . 7_556 ? O4 Pt2 N4 94.0(3) . 7_556 ? N4 Pt2 Pt1 99.4(3) . . ? N3 Pt2 Pt1 97.9(3) . . ? O6 Pt2 Pt1 86.4(2) . . ? O4 Pt2 Pt1 85.4(2) . . ? N4 Pt2 Pt1 173.1(3) 7_556 . ? N4 Pt2 Pt2 42.1(3) . 7_556 ? N3 Pt2 Pt2 91.7(3) . 7_556 ? O6 Pt2 Pt2 85.9(2) . 7_556 ? O4 Pt2 Pt2 132.9(2) . 7_556 ? N4 Pt2 Pt2 38.9(2) 7_556 7_556 ? Pt1 Pt2 Pt2 141.01(2) . 7_556 ? N2 Pt1 N1 90.6(4) . . ? N2 Pt1 O5 89.9(4) . . ? N1 Pt1 O5 177.2(4) . . ? N2 Pt1 O3 177.3(4) . . ? N1 Pt1 O3 90.1(4) . . ? O5 Pt1 O3 89.3(3) . . ? N2 Pt1 O1 85.4(4) . . ? N1 Pt1 O1 92.1(4) . . ? O5 Pt1 O1 85.1(4) . . ? O3 Pt1 O1 92.0(4) . . ? N2 Pt1 Pt2 97.6(3) . . ? N1 Pt1 Pt2 97.6(3) . . ? O5 Pt1 Pt2 85.1(2) . . ? O3 Pt1 Pt2 84.9(2) . . ? O1 Pt1 Pt2 169.8(3) . . ? Pt1 N1 H1A 109.5 . . ? Pt1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Pt1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Pt1 N2 H2A 109.5 . . ? Pt1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Pt1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Pt2 N3 H3A 109.5 . . ? Pt2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Pt2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Pt2 N4 Pt2 99.0(4) . 7_556 ? Pt2 N4 H1N 112.0 . . ? Pt2 N4 H1N 112.0 7_556 . ? Pt2 N4 H2N 112.0 . . ? Pt2 N4 H2N 112.0 7_556 . ? H1N N4 H2N 109.7 . . ? C3 O3 Pt1 122.2(8) . . ? C3 O4 Pt2 121.8(8) . . ? C5 O5 Pt1 122.8(7) . . ? C5 O6 Pt2 119.8(8) . . ? O4 C3 O3 125.6(11) . . ? O4 C3 C4 118.9(12) . . ? O3 C3 C4 115.5(12) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O5 C5 O6 125.8(11) . . ? O5 C5 C6 118.7(11) . . ? O6 C5 C6 115.5(11) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1A O1 C1 27.2(16) . . ? C1A O1 Pt1 125.5(13) . . ? C1 O1 Pt1 125.6(13) . . ? O1 C1 O2 127(2) . . ? O1 C1 C2 112(2) . . ? O2 C1 C2 121(2) . . ? O1 C1A O2A 126(2) . . ? O1 C1A C2 112(2) . . ? O2A C1A C2 122(3) . . ? F2 C2 F1 107.4(19) . . ? F2 C2 F3 104(2) . . ? F1 C2 F3 104.1(19) . . ? F2 C2 C1 103.7(18) . . ? F1 C2 C1 120(2) . . ? F3 C2 C1 116.6(19) . . ? F2 C2 C1A 125.2(19) . . ? F1 C2 C1A 109.7(19) . . ? F3 C2 C1A 104.7(19) . . ? C1 C2 C1A 21.6(14) . . ? O9 N5 O7 123.6(14) . . ? O9 N5 O8 121.0(12) . . ? O7 N5 O8 115.3(15) . . ? O11 N6 O10 120.1(14) . . ? O11 N6 O12 119.2(13) . . ? O10 N6 O12 120.6(14) . . ? C7 N7 C8 121.6(12) . . ? C7 N7 C9 120.4(13) . . ? C8 N7 C9 117.9(12) . . ? O13 C7 N7 123.1(14) . . ? O13 C7 H7 118.4 . . ? N7 C7 H7 118.4 . . ? N7 C8 H8A 109.5 . . ? N7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N7 C9 H9A 109.5 . . ? N7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 N8 C12 125(2) . . ? C10 N8 C11 121(2) . . ? C12 N8 C11 114(2) . . ? O14 C10 N8 124(3) . . ? O14 C10 H10 118.1 . . ? N8 C10 H10 118.1 . . ? N8 C11 H11A 109.5 . . ? N8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N8 C11 H11D 109.5 . . ? H11A C11 H11D 141.1 . . ? H11B C11 H11D 56.3 . . ? H11C C11 H11D 56.3 . . ? N8 C11 H11E 109.5 . . ? H11A C11 H11E 56.3 . . ? H11B C11 H11E 141.1 . . ? H11C C11 H11E 56.3 . . ? H11D C11 H11E 109.5 . . ? N8 C11 H11F 109.5 . . ? H11A C11 H11F 56.3 . . ? H11B C11 H11F 56.3 . . ? H11C C11 H11F 141.1 . . ? H11D C11 H11F 109.5 . . ? H11E C11 H11F 109.5 . . ? N8 C12 H12A 109.5 . . ? N8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N8 C12 H12D 109.5 . . ? H12A C12 H12D 141.1 . . ? H12B C12 H12D 56.3 . . ? H12C C12 H12D 56.3 . . ? N8 C12 H12E 109.5 . . ? H12A C12 H12E 56.3 . . ? H12B C12 H12E 141.1 . . ? H12C C12 H12E 56.3 . . ? H12D C12 H12E 109.5 . . ? N8 C12 H12F 109.5 . . ? H12A C12 H12F 56.3 . . ? H12B C12 H12F 56.3 . . ? H12C C12 H12F 141.1 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C10A N8A C12A 122(2) . . ? C10A N8A C11A 119.8(19) . . ? C12A N8A C11A 118.1(19) . . ? O14A C10A N8A 123(3) . . ? O14A C10A H10A 118.5 . . ? N8A C10A H10A 118.5 . . ? N8A C11A H11G 109.5 . . ? N8A C11A H11H 109.5 . . ? H11G C11A H11H 109.5 . . ? N8A C11A H11I 109.5 . . ? H11G C11A H11I 109.5 . . ? H11H C11A H11I 109.5 . . ? N8A C11A H11J 109.5 . . ? H11G C11A H11J 141.1 . . ? H11H C11A H11J 56.3 . . ? H11I C11A H11J 56.3 . . ? N8A C11A H11K 109.5 . . ? H11G C11A H11K 56.3 . . ? H11H C11A H11K 141.1 . . ? H11I C11A H11K 56.3 . . ? H11J C11A H11K 109.5 . . ? N8A C11A H11L 109.5 . . ? H11G C11A H11L 56.3 . . ? H11H C11A H11L 56.3 . . ? H11I C11A H11L 141.1 . . ? H11J C11A H11L 109.5 . . ? H11K C11A H11L 109.5 . . ? N8A C12A H12G 109.5 . . ? N8A C12A H12H 109.5 . . ? H12G C12A H12H 109.5 . . ? N8A C12A H12I 109.5 . . ? H12G C12A H12I 109.5 . . ? H12H C12A H12I 109.5 . . ? N8A C12A H12J 109.5 . . ? H12G C12A H12J 141.1 . . ? H12H C12A H12J 56.3 . . ? H12I C12A H12J 56.3 . . ? N8A C12A H12K 109.5 . . ? H12G C12A H12K 56.3 . . ? H12H C12A H12K 141.1 . . ? H12I C12A H12K 56.3 . . ? H12J C12A H12K 109.5 . . ? N8A C12A H12L 109.5 . . ? H12G C12A H12L 56.3 . . ? H12H C12A H12L 56.3 . . ? H12I C12A H12L 141.1 . . ? H12J C12A H12L 109.5 . . ? H12K C12A H12L 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.13 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 4.849 _refine_diff_density_min -1.761 _refine_diff_density_rms 0.264 #===END