# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Ramon Vilar' _publ_contact_author_email R.VILAR@IMPERIAL.AC.UK _publ_section_title ; Effect of metal coordination on the interaction of substituted phenanthroline and pyridine ligands with quadruplex DNA ; loop_ _publ_author_name 'Ramon Vilar-Compte' 'Stephen Neidle' 'Julie E. Reed' 'A White' # Attachment 'Dalton_10-08.cif' data_Compound_L1 _database_code_depnum_ccdc_archive 'CCDC 646776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H12 N4 O, C H2 Cl2, H2 O' _chemical_formula_sum 'C19 H16 Cl2 N4 O2' _chemical_formula_weight 403.26 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0384(3) _cell_length_b 9.2870(3) _cell_length_c 10.8833(3) _cell_angle_alpha 95.453(2) _cell_angle_beta 96.174(2) _cell_angle_gamma 97.0910(10) _cell_volume 895.85(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 8844 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description blades _exptl_crystal_colour 'Light yellow' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97119 _exptl_absorpt_correction_T_max 1.00071 _exptl_absorpt_process_details sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18498 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.43 _reflns_number_total 4075 _reflns_number_gt 3136 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.1479P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.016(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4075 _refine_ls_number_parameters 257 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0608 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1046 _refine_ls_wR_factor_gt 0.0982 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.36614(15) 0.10067(14) 0.18268(12) 0.0211(3) Uani 1 1 d . . . C2 C 0.28055(19) -0.02133(17) 0.13168(15) 0.0232(3) Uani 1 1 d . . . H2A H 0.1750 -0.0209 0.1191 0.028 Uiso 1 1 calc R . . C3 C 0.3367(2) -0.15066(18) 0.09539(15) 0.0259(4) Uani 1 1 d . . . H3A H 0.2707 -0.2348 0.0584 0.031 Uiso 1 1 calc R . . C4 C 0.4881(2) -0.15359(18) 0.11416(15) 0.0264(4) Uani 1 1 d . . . H4A H 0.5286 -0.2405 0.0912 0.032 Uiso 1 1 calc R . . C5 C 0.58374(18) -0.02683(17) 0.16775(14) 0.0224(3) Uani 1 1 d . . . C6 C 0.7434(2) -0.02153(19) 0.18852(16) 0.0268(4) Uani 1 1 d . . . H6A H 0.7874 -0.1066 0.1664 0.032 Uiso 1 1 calc R . . C7 C 0.83282(19) 0.10188(19) 0.23890(16) 0.0262(4) Uani 1 1 d . . . H7A H 0.9387 0.1029 0.2503 0.031 Uiso 1 1 calc R . . C8 C 0.76970(18) 0.23144(18) 0.27538(14) 0.0220(3) Uani 1 1 d . . . C9 C 0.85908(18) 0.35874(18) 0.33475(15) 0.0234(4) Uani 1 1 d . . . H9A H 0.9651 0.3625 0.3495 0.028 Uiso 1 1 calc R . . C10 C 0.79182(18) 0.47715(18) 0.37103(15) 0.0230(3) Uani 1 1 d . . . H10A H 0.8496 0.5630 0.4143 0.028 Uiso 1 1 calc R . . C11 C 0.63541(17) 0.46917(17) 0.34303(14) 0.0193(3) Uani 1 1 d . . . N12 N 0.54679(14) 0.35120(14) 0.28737(12) 0.0183(3) Uani 1 1 d . . . C13 C 0.61256(17) 0.23140(17) 0.25544(14) 0.0191(3) Uani 1 1 d . . . C14 C 0.51688(17) 0.09896(17) 0.20034(14) 0.0195(3) Uani 1 1 d . . . C15 C 0.56263(17) 0.60318(16) 0.37469(14) 0.0195(3) Uani 1 1 d . . . O15 O 0.64038(13) 0.72061(12) 0.41330(11) 0.0263(3) Uani 1 1 d . . . N16 N 0.41117(14) 0.58340(14) 0.35541(12) 0.0195(3) Uani 1 1 d D . . H16 H 0.3669(19) 0.4918(8) 0.3294(17) 0.029(5) Uiso 1 1 d D . . C17 C 0.31466(17) 0.69088(16) 0.36997(14) 0.0187(3) Uani 1 1 d . . . N18 N 0.17712(15) 0.64872(14) 0.30916(12) 0.0215(3) Uani 1 1 d . . . C19 C 0.07649(19) 0.74284(18) 0.31990(15) 0.0244(4) Uani 1 1 d . . . H19A H -0.0215 0.7154 0.2768 0.029 Uiso 1 1 calc R . . C20 C 0.10755(19) 0.87746(18) 0.39019(15) 0.0261(4) Uani 1 1 d . . . H20A H 0.0324 0.9400 0.3962 0.031 Uiso 1 1 calc R . . C21 C 0.2506(2) 0.91852(17) 0.45146(15) 0.0254(4) Uani 1 1 d . . . H21A H 0.2754 1.0106 0.5001 0.031 Uiso 1 1 calc R . . C22 C 0.35755(19) 0.82509(17) 0.44179(15) 0.0225(3) Uani 1 1 d . . . H22A H 0.4569 0.8514 0.4827 0.027 Uiso 1 1 calc R . . C30 C 0.2120(2) 0.39447(19) 0.07199(16) 0.0286(4) Uani 1 1 d . . . H30A H 0.2906 0.3442 0.1136 0.034 Uiso 1 1 calc R . . H30B H 0.1898 0.4731 0.1325 0.034 Uiso 1 1 calc R . . Cl1 Cl 0.27963(6) 0.47180(5) -0.05699(4) 0.03934(16) Uani 1 1 d . . . Cl2 Cl 0.04819(5) 0.26881(6) 0.02594(5) 0.04289(16) Uani 1 1 d . . . O40 O 0.20960(13) 0.28037(13) 0.34112(11) 0.0273(3) Uani 1 1 d D . . H40A H 0.265(2) 0.227(2) 0.2957(18) 0.049(6) Uiso 1 1 d D . . H40B H 0.249(3) 0.279(3) 0.4204(8) 0.071(8) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0214(7) 0.0215(7) 0.0209(7) 0.0016(5) 0.0042(5) 0.0038(5) C2 0.0248(9) 0.0217(8) 0.0230(8) 0.0020(6) 0.0044(6) 0.0021(6) C3 0.0349(10) 0.0194(8) 0.0232(8) 0.0010(6) 0.0058(7) 0.0019(7) C4 0.0368(10) 0.0203(8) 0.0250(9) 0.0045(7) 0.0085(7) 0.0100(7) C5 0.0276(9) 0.0234(8) 0.0195(8) 0.0065(6) 0.0079(7) 0.0088(7) C6 0.0309(9) 0.0283(9) 0.0262(9) 0.0076(7) 0.0081(7) 0.0162(7) C7 0.0209(8) 0.0343(9) 0.0277(9) 0.0093(7) 0.0074(7) 0.0122(7) C8 0.0202(8) 0.0289(9) 0.0199(8) 0.0085(6) 0.0052(6) 0.0080(7) C9 0.0151(8) 0.0330(9) 0.0235(8) 0.0076(7) 0.0029(6) 0.0043(7) C10 0.0198(8) 0.0272(8) 0.0216(8) 0.0037(6) 0.0019(6) 0.0010(6) C11 0.0182(8) 0.0236(8) 0.0168(7) 0.0048(6) 0.0030(6) 0.0030(6) N12 0.0185(7) 0.0191(6) 0.0178(6) 0.0029(5) 0.0035(5) 0.0029(5) C13 0.0196(8) 0.0229(8) 0.0171(7) 0.0060(6) 0.0052(6) 0.0067(6) C14 0.0230(8) 0.0220(8) 0.0159(7) 0.0054(6) 0.0062(6) 0.0069(6) C15 0.0204(8) 0.0207(8) 0.0169(7) 0.0025(6) 0.0009(6) 0.0019(6) O15 0.0237(6) 0.0210(6) 0.0318(6) 0.0005(5) -0.0009(5) -0.0011(5) N16 0.0195(7) 0.0162(7) 0.0219(7) -0.0005(5) 0.0012(5) 0.0024(5) C17 0.0212(8) 0.0180(7) 0.0176(7) 0.0032(6) 0.0036(6) 0.0034(6) N18 0.0218(7) 0.0212(7) 0.0221(7) 0.0031(5) 0.0024(5) 0.0044(5) C19 0.0232(9) 0.0263(9) 0.0260(8) 0.0074(7) 0.0044(7) 0.0075(7) C20 0.0299(9) 0.0241(8) 0.0283(9) 0.0083(7) 0.0081(7) 0.0113(7) C21 0.0354(10) 0.0180(8) 0.0240(8) 0.0018(6) 0.0069(7) 0.0052(7) C22 0.0254(9) 0.0198(8) 0.0219(8) 0.0016(6) 0.0028(6) 0.0022(6) C30 0.0335(10) 0.0306(9) 0.0214(8) 0.0011(7) 0.0001(7) 0.0071(7) Cl1 0.0601(3) 0.0280(3) 0.0346(3) 0.00803(18) 0.0157(2) 0.0121(2) Cl2 0.0335(3) 0.0496(3) 0.0418(3) -0.0037(2) 0.0035(2) -0.0015(2) O40 0.0243(6) 0.0314(7) 0.0275(6) -0.0007(5) 0.0040(5) 0.0114(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.327(2) . ? N1 C14 1.358(2) . ? C2 C3 1.400(2) . ? C3 C4 1.365(2) . ? C4 C5 1.408(2) . ? C5 C14 1.413(2) . ? C5 C6 1.430(2) . ? C6 C7 1.351(3) . ? C7 C8 1.435(2) . ? C8 C9 1.405(2) . ? C8 C13 1.413(2) . ? C9 C10 1.367(2) . ? C10 C11 1.405(2) . ? C11 N12 1.327(2) . ? C11 C15 1.506(2) . ? N12 C13 1.359(2) . ? C13 C14 1.451(2) . ? C15 O15 1.2328(18) . ? C15 N16 1.349(2) . ? N16 C17 1.413(2) . ? C17 N18 1.338(2) . ? C17 C22 1.395(2) . ? N18 C19 1.343(2) . ? C19 C20 1.383(2) . ? C20 C21 1.381(2) . ? C21 C22 1.382(2) . ? C30 Cl2 1.7629(18) . ? C30 Cl1 1.7685(18) . ? 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 C2 N1 C14 117.66(14) . . ? N1 C2 C3 123.85(16) . . ? C4 C3 C2 118.78(15) . . ? C3 C4 C5 119.55(15) . . ? C4 C5 C14 117.63(15) . . ? C4 C5 C6 122.53(15) . . ? C14 C5 C6 119.84(15) . . ? C7 C6 C5 121.38(15) . . ? C6 C7 C8 120.70(15) . . ? C9 C8 C13 118.21(14) . . ? C9 C8 C7 121.99(15) . . ? C13 C8 C7 119.77(15) . . ? C10 C9 C8 119.27(15) . . ? C9 C10 C11 118.57(15) . . ? N12 C11 C10 124.09(14) . . ? N12 C11 C15 117.30(13) . . ? C10 C11 C15 118.60(14) . . ? C11 N12 C13 117.49(13) . . ? N12 C13 C8 122.28(14) . . ? N12 C13 C14 118.35(13) . . ? C8 C13 C14 119.37(14) . . ? N1 C14 C5 122.53(14) . . ? N1 C14 C13 118.55(13) . . ? C5 C14 C13 118.93(14) . . ? O15 C15 N16 124.55(14) . . ? O15 C15 C11 120.36(14) . . ? N16 C15 C11 115.08(13) . . ? C15 N16 C17 127.20(13) . . ? N18 C17 C22 123.78(14) . . ? N18 C17 N16 112.62(13) . . ? C22 C17 N16 123.58(14) . . ? C17 N18 C19 116.84(13) . . ? N18 C19 C20 123.70(15) . . ? C21 C20 C19 118.24(15) . . ? C20 C21 C22 119.72(15) . . ? C21 C22 C17 117.72(15) . . ? Cl2 C30 Cl1 111.30(9) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.266 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.056 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 646777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H24 N10 O2 Pt2, Cl2, (C2 H6 O S), (C3 H6 O), 3.75(H2 O)' _chemical_formula_sum 'C41 H43.50 Cl2 N10 O7.75 Pt2 S' _chemical_formula_weight 1293.50 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 17.3137(15) _cell_length_b 11.0617(7) _cell_length_c 24.561(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.763(3) _cell_angle_gamma 90.00 _cell_volume 4548.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 139987 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description needles _exptl_crystal_colour Orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.889 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2510 _exptl_absorpt_coefficient_mu 6.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93408 _exptl_absorpt_correction_T_max 0.99295 _exptl_absorpt_process_details sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40815 _diffrn_reflns_av_R_equivalents 0.1310 _diffrn_reflns_av_sigmaI/netI 0.1644 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9074 _reflns_number_gt 5055 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0546P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9074 _refine_ls_number_parameters 617 _refine_ls_number_restraints 209 _refine_ls_R_factor_all 0.1560 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1184 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.020 _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 0.70116(3) 0.82349(4) 0.51580(2) 0.02750(16) Uani 1 1 d . . . Pt2 Pt 0.86793(3) 0.74206(4) 0.592232(19) 0.02513(15) Uani 1 1 d . . . N1 N 0.6497(6) 0.9744(8) 0.5382(4) 0.031(3) Uani 1 1 d . . . C2 C 0.6649(8) 1.0929(11) 0.5346(5) 0.039(3) Uani 1 1 d . . . H2A H 0.7072 1.1171 0.5189 0.047 Uiso 1 1 calc R . . C3 C 0.6191(9) 1.1839(12) 0.5539(6) 0.048(4) Uani 1 1 d . . . H3A H 0.6328 1.2668 0.5525 0.058 Uiso 1 1 calc R . . C4 C 0.5557(9) 1.1512(12) 0.5743(6) 0.047(4) Uani 1 1 d . . . H4A H 0.5231 1.2111 0.5850 0.056 Uiso 1 1 calc R . . C5 C 0.5393(8) 1.0278(12) 0.5793(5) 0.039(3) Uani 1 1 d . . . C6 C 0.4728(9) 0.9812(14) 0.5999(6) 0.056(4) Uani 1 1 d . . . H6A H 0.4391 1.0357 0.6130 0.067 Uiso 1 1 calc R . . C7 C 0.4593(9) 0.8613(13) 0.6004(6) 0.053(4) Uani 1 1 d . . . H7A H 0.4160 0.8336 0.6143 0.063 Uiso 1 1 calc R . . C8 C 0.5059(8) 0.7755(12) 0.5816(5) 0.033(3) Uani 1 1 d . . . C9 C 0.4971(8) 0.6483(13) 0.5797(6) 0.044(4) Uani 1 1 d . . . H9A H 0.4548 0.6125 0.5923 0.053 Uiso 1 1 calc R . . C10 C 0.5494(9) 0.5741(13) 0.5597(5) 0.048(4) Uani 1 1 d . . . H10A H 0.5428 0.4888 0.5588 0.057 Uiso 1 1 calc R . . C11 C 0.6111(7) 0.6267(10) 0.5413(5) 0.028(3) Uani 1 1 d . . . N12 N 0.6199(6) 0.7462(9) 0.5442(4) 0.030(2) Uani 1 1 d . . . C13 C 0.5688(8) 0.8196(11) 0.5633(5) 0.033(3) Uani 1 1 d . . . C14 C 0.5864(8) 0.9430(10) 0.5592(5) 0.032(3) Uani 1 1 d . . . C15 C 0.6711(8) 0.5662(10) 0.5168(5) 0.031(3) Uani 1 1 d . . . O15 O 0.6746(5) 0.4556(7) 0.5124(3) 0.041(2) Uani 1 1 d . . . N16 N 0.7253(6) 0.6482(8) 0.5062(4) 0.031(3) Uani 1 1 d . . . C17 C 0.7905(8) 0.6152(9) 0.4842(5) 0.026(3) Uani 1 1 d . . . N18 N 0.8620(7) 0.6572(8) 0.5167(4) 0.030(3) Uani 1 1 d . . . C19 C 0.9286(7) 0.6467(9) 0.4979(4) 0.020(3) Uani 1 1 d . . . C20 C 0.9223(8) 0.5834(10) 0.4453(5) 0.031(3) Uani 1 1 d . . . H20A H 0.9681 0.5751 0.4309 0.037 Uiso 1 1 calc R . . C21 C 0.8531(8) 0.5371(10) 0.4171(5) 0.032(3) Uani 1 1 d . . . H21A H 0.8508 0.4920 0.3838 0.038 Uiso 1 1 calc R . . C22 C 0.7829(8) 0.5528(10) 0.4352(5) 0.030(3) Uani 1 1 d . . . H22A H 0.7329 0.5217 0.4144 0.036 Uiso 1 1 calc R . . N23 N 0.9978(6) 0.6939(8) 0.5280(4) 0.032(3) Uani 1 1 d . . . N31 N 0.8739(6) 0.5904(8) 0.6412(4) 0.029(2) Uani 1 1 d . . . C32 C 0.8642(7) 0.4734(10) 0.6267(5) 0.032(3) Uani 1 1 d . . . H32A H 0.8541 0.4502 0.5883 0.038 Uiso 1 1 calc R . . C33 C 0.8692(8) 0.3838(12) 0.6694(6) 0.043(4) Uani 1 1 d . . . H33A H 0.8616 0.3011 0.6590 0.052 Uiso 1 1 calc R . . C34 C 0.8847(8) 0.4150(12) 0.7243(6) 0.044(4) Uani 1 1 d . . . H34A H 0.8894 0.3539 0.7522 0.053 Uiso 1 1 calc R . . C35 C 0.8937(7) 0.5377(10) 0.7407(5) 0.026(3) Uani 1 1 d . . . C36 C 0.9102(7) 0.5849(11) 0.7961(5) 0.035(3) Uani 1 1 d . . . H36A H 0.9146 0.5302 0.8265 0.041 Uiso 1 1 calc R . . C37 C 0.9200(8) 0.7031(11) 0.8074(5) 0.041(4) Uani 1 1 d . . . H37A H 0.9329 0.7290 0.8456 0.049 Uiso 1 1 calc R . . C38 C 0.9115(7) 0.7911(10) 0.7640(5) 0.028(3) Uani 1 1 d . . . C39 C 0.9161(7) 0.9154(11) 0.7701(5) 0.037(3) Uani 1 1 d . . . H39A H 0.9261 0.9506 0.8066 0.044 Uiso 1 1 calc R . . C40 C 0.9056(7) 0.9915(11) 0.7212(5) 0.036(3) Uani 1 1 d . . . H40A H 0.9086 1.0769 0.7252 0.043 Uiso 1 1 calc R . . C41 C 0.8915(7) 0.9402(10) 0.6690(5) 0.028(3) Uani 1 1 d . . . N42 N 0.8844(6) 0.8220(8) 0.6649(4) 0.028(2) Uani 1 1 d . . . C43 C 0.8937(7) 0.7451(10) 0.7096(5) 0.028(3) Uani 1 1 d . . . C44 C 0.8864(7) 0.6213(9) 0.6965(5) 0.025(3) Uani 1 1 d . . . C45 C 0.8803(7) 0.9992(11) 0.6136(5) 0.032(3) Uani 1 1 d . . . O45 O 0.8797(5) 1.1116(7) 0.6093(3) 0.043(2) Uani 1 1 d . . . N46 N 0.8679(5) 0.9172(7) 0.5703(4) 0.024(2) Uani 1 1 d . . . C47 C 0.8503(7) 0.9555(10) 0.5134(5) 0.026(3) Uani 1 1 d . . . N48 N 0.7819(6) 0.9070(8) 0.4799(4) 0.025(2) Uani 1 1 d . . . C49 C 0.7653(7) 0.9258(10) 0.4233(5) 0.028(3) Uani 1 1 d . . . C50 C 0.8135(8) 1.0031(10) 0.4009(5) 0.035(3) Uani 1 1 d . . . H50A H 0.8009 1.0189 0.3616 0.042 Uiso 1 1 calc R . . C51 C 0.8788(7) 1.0553(9) 0.4363(5) 0.027(3) Uani 1 1 d . . . H51A H 0.9106 1.1097 0.4213 0.033 Uiso 1 1 calc R . . C52 C 0.8998(8) 1.0310(10) 0.4932(5) 0.034(3) Uani 1 1 d . . . H52A H 0.9464 1.0650 0.5175 0.040 Uiso 1 1 calc R . . N53 N 0.7003(6) 0.8731(9) 0.3890(4) 0.037(3) Uani 1 1 d . . . Cl1 Cl 1.0803(2) 0.7054(3) 0.66496(13) 0.0401(8) Uani 1 1 d . . . Cl2 Cl 0.5696(2) 0.6432(3) 0.38010(15) 0.0490(9) Uani 1 1 d . . . O60 O 0.7103(10) 0.840(2) 0.6763(8) 0.111(7) Uani 0.743(19) 1 d PDU A 1 C60 C 0.7011(11) 0.893(2) 0.7154(8) 0.071(6) Uani 0.743(19) 1 d PDU A 1 C61 C 0.7033(16) 0.864(3) 0.7730(9) 0.105(7) Uani 0.743(19) 1 d PDU A 1 H61A H 0.6494 0.8703 0.7787 0.158 Uiso 0.743(19) 1 calc PR A 1 H61B H 0.7389 0.9202 0.7983 0.158 Uiso 0.743(19) 1 calc PR A 1 H61C H 0.7230 0.7811 0.7813 0.158 Uiso 0.743(19) 1 calc PR A 1 C62 C 0.6941(16) 1.028(2) 0.7083(10) 0.099(7) Uani 0.743(19) 1 d PDU A 1 H62A H 0.7026 1.0509 0.6717 0.148 Uiso 0.743(19) 1 calc PR A 1 H62B H 0.7345 1.0677 0.7384 0.148 Uiso 0.743(19) 1 calc PR A 1 H62C H 0.6408 1.0543 0.7103 0.148 Uiso 0.743(19) 1 calc PR A 1 O60' O 0.685(3) 0.730(5) 0.6797(19) 0.103(10) Uiso 0.257(19) 1 d PDU A 2 C60' C 0.693(3) 0.815(5) 0.7127(19) 0.083(9) Uiso 0.257(19) 1 d PDU A 2 C61' C 0.700(5) 0.780(6) 0.7719(19) 0.091(11) Uiso 0.257(19) 1 d PDU A 2 H61D H 0.6459 0.7678 0.7774 0.136 Uiso 0.257(19) 1 calc PR A 2 H61E H 0.7265 0.8447 0.7971 0.136 Uiso 0.257(19) 1 calc PR A 2 H61F H 0.7303 0.7053 0.7806 0.136 Uiso 0.257(19) 1 calc PR A 2 C62' C 0.699(5) 0.943(5) 0.697(3) 0.088(11) Uiso 0.257(19) 1 d PDU A 2 H62D H 0.7328 0.9500 0.6712 0.132 Uiso 0.257(19) 1 calc PR A 2 H62E H 0.7217 0.9903 0.7313 0.132 Uiso 0.257(19) 1 calc PR A 2 H62F H 0.6452 0.9737 0.6792 0.132 Uiso 0.257(19) 1 calc PR A 2 O70 O 0.6419(18) 1.099(3) 0.1921(11) 0.092(7) Uiso 0.366(4) 1 d PDU B 1 S70 S 0.6018(9) 1.0826(14) 0.2445(6) 0.072(4) Uiso 0.366(4) 1 d PDU B 1 C71 C 0.535(2) 0.952(3) 0.2289(17) 0.087(8) Uiso 0.366(4) 1 d PDU B 1 H71A H 0.4863 0.9748 0.2005 0.131 Uiso 0.366(4) 1 calc PR B 1 H71B H 0.5214 0.9258 0.2633 0.131 Uiso 0.366(4) 1 calc PR B 1 H71C H 0.5619 0.8862 0.2143 0.131 Uiso 0.366(4) 1 calc PR B 1 C72 C 0.681(2) 1.006(4) 0.2930(16) 0.086(8) Uiso 0.366(4) 1 d PDU B 1 H72A H 0.7254 1.0620 0.3069 0.129 Uiso 0.366(4) 1 calc PR B 1 H72B H 0.6992 0.9378 0.2740 0.129 Uiso 0.366(4) 1 calc PR B 1 H72C H 0.6617 0.9759 0.3247 0.129 Uiso 0.366(4) 1 calc PR B 1 O70' O 0.6773(18) 1.058(3) 0.2954(10) 0.064(7) Uiso 0.339(10) 1 d PDU C 2 S70' S 0.6324(15) 1.071(2) 0.2360(10) 0.134(6) Uiso 0.339(10) 1 d PDU C 2 C71' C 0.656(3) 1.210(3) 0.2082(18) 0.086(8) Uiso 0.339(10) 1 d PDU C 2 H71D H 0.6427 1.2772 0.2302 0.129 Uiso 0.339(10) 1 calc PR C 2 H71E H 0.6254 1.2180 0.1689 0.129 Uiso 0.339(10) 1 calc PR C 2 H71F H 0.7133 1.2125 0.2101 0.129 Uiso 0.339(10) 1 calc PR C 2 C72' C 0.663(3) 0.974(3) 0.1870(16) 0.091(8) Uiso 0.339(10) 1 d PDU C 2 H72D H 0.6557 0.8892 0.1964 0.136 Uiso 0.339(10) 1 calc PR C 2 H72E H 0.7196 0.9882 0.1889 0.136 Uiso 0.339(10) 1 calc PR C 2 H72F H 0.6309 0.9908 0.1488 0.136 Uiso 0.339(10) 1 calc PR C 2 O70" O 0.7014(15) 1.038(3) 0.2506(14) 0.054(7) Uiso 0.295(9) 1 d PDU D 3 S70" S 0.6146(14) 1.018(2) 0.2413(11) 0.133(7) Uiso 0.295(9) 1 d PDU D 3 C71" C 0.592(3) 0.893(4) 0.281(2) 0.097(8) Uiso 0.295(9) 1 d PDU D 3 H71G H 0.6215 0.8209 0.2737 0.146 Uiso 0.295(9) 1 calc PR D 3 H71H H 0.5349 0.8762 0.2701 0.146 Uiso 0.295(9) 1 calc PR D 3 H71I H 0.6089 0.9118 0.3214 0.146 Uiso 0.295(9) 1 calc PR D 3 C72" C 0.559(3) 1.144(4) 0.258(2) 0.072(8) Uiso 0.295(9) 1 d PDU D 3 H72G H 0.5682 1.2158 0.2366 0.108 Uiso 0.295(9) 1 calc PR D 3 H72H H 0.5761 1.1614 0.2982 0.108 Uiso 0.295(9) 1 calc PR D 3 H72I H 0.5017 1.1248 0.2474 0.108 Uiso 0.295(9) 1 calc PR D 3 O80 O 0.7300(5) 0.2689(7) 0.4554(4) 0.050(2) Uani 1 1 d . . . O90 O 0.8760(5) 1.3027(7) 0.5292(3) 0.037(2) Uani 1 1 d . . . O100 O 1.2591(6) 0.7267(8) 0.6564(4) 0.063(3) Uani 1 1 d . . . O110 O 0.6002(10) 0.4083(14) 0.3130(7) 0.040(5) Uani 0.50 1 d P . . O120 O 0.523(2) 0.849(3) 0.2831(15) 0.047(10) Uiso 0.25 1 d P E 4 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 0.0321(3) 0.0246(3) 0.0276(3) -0.0012(2) 0.0108(2) -0.0014(2) Pt2 0.0338(3) 0.0200(2) 0.0227(3) -0.0011(2) 0.0093(2) -0.0014(2) N1 0.041(7) 0.023(6) 0.030(6) -0.006(4) 0.013(6) -0.007(5) C2 0.039(9) 0.042(8) 0.035(8) 0.001(6) 0.008(7) 0.001(7) C3 0.062(11) 0.036(8) 0.051(9) -0.007(7) 0.023(9) 0.011(8) C4 0.063(11) 0.039(9) 0.043(9) -0.008(6) 0.023(8) 0.016(8) C5 0.041(10) 0.041(8) 0.037(8) -0.003(6) 0.010(7) 0.011(7) C6 0.041(11) 0.058(11) 0.069(12) -0.006(8) 0.013(9) 0.014(8) C7 0.042(10) 0.058(10) 0.055(10) -0.011(8) 0.006(8) 0.001(8) C8 0.026(8) 0.051(9) 0.023(7) -0.003(6) 0.011(6) -0.006(7) C9 0.026(9) 0.059(10) 0.054(10) 0.007(7) 0.023(8) -0.011(7) C10 0.050(10) 0.053(9) 0.040(9) 0.004(7) 0.013(8) -0.022(8) C11 0.033(8) 0.018(6) 0.029(7) 0.001(5) 0.000(6) -0.015(6) N12 0.031(7) 0.042(7) 0.023(6) 0.005(5) 0.015(5) -0.009(5) C13 0.040(9) 0.039(8) 0.022(7) 0.006(6) 0.008(7) 0.002(7) C14 0.041(9) 0.035(8) 0.017(7) 0.000(5) 0.002(7) 0.000(7) C15 0.038(9) 0.021(7) 0.034(8) 0.004(5) 0.011(7) -0.010(6) O15 0.055(7) 0.025(5) 0.049(6) -0.003(4) 0.027(5) -0.010(4) N16 0.027(7) 0.029(6) 0.038(7) 0.004(5) 0.007(5) 0.000(5) C17 0.036(9) 0.016(6) 0.030(7) 0.006(5) 0.015(7) -0.009(6) N18 0.051(8) 0.023(5) 0.017(5) -0.006(4) 0.009(6) -0.003(5) C19 0.029(8) 0.020(6) 0.015(6) 0.001(4) 0.015(6) 0.000(5) C20 0.042(9) 0.026(7) 0.027(7) 0.002(5) 0.012(7) -0.004(6) C21 0.043(9) 0.035(7) 0.021(7) 0.001(5) 0.016(7) -0.010(7) C22 0.040(9) 0.033(7) 0.013(7) -0.009(5) 0.000(6) -0.002(6) N23 0.035(7) 0.029(6) 0.033(6) -0.004(5) 0.011(5) -0.004(5) N31 0.034(7) 0.022(6) 0.035(7) -0.003(4) 0.014(5) 0.000(5) C32 0.035(8) 0.029(7) 0.032(8) 0.002(6) 0.009(6) -0.003(6) C33 0.054(10) 0.046(8) 0.037(9) 0.009(7) 0.026(8) -0.001(7) C34 0.051(10) 0.046(9) 0.041(9) 0.018(7) 0.019(8) 0.013(7) C35 0.036(8) 0.022(6) 0.024(7) 0.004(5) 0.016(6) 0.007(6) C36 0.040(9) 0.049(9) 0.013(7) 0.019(6) 0.006(6) 0.007(7) C37 0.062(10) 0.030(7) 0.025(7) 0.002(5) 0.001(7) 0.009(7) C38 0.038(8) 0.030(7) 0.018(7) -0.005(5) 0.011(6) -0.003(6) C39 0.035(9) 0.044(8) 0.027(8) -0.022(6) 0.001(6) 0.001(6) C40 0.044(9) 0.031(7) 0.038(8) 0.000(6) 0.022(7) -0.006(6) C41 0.034(8) 0.031(7) 0.022(7) -0.018(5) 0.012(6) -0.005(6) N42 0.032(6) 0.030(6) 0.024(6) -0.014(5) 0.011(5) -0.008(5) C43 0.034(8) 0.036(7) 0.016(6) 0.006(6) 0.008(6) 0.011(6) C44 0.034(8) 0.020(6) 0.020(7) -0.003(5) 0.007(6) 0.005(6) C45 0.036(9) 0.031(8) 0.030(8) -0.001(6) 0.010(7) 0.000(6) O45 0.063(7) 0.026(5) 0.040(6) -0.011(4) 0.014(5) 0.000(5) N46 0.029(6) 0.014(5) 0.030(6) -0.010(4) 0.007(5) -0.008(4) C47 0.030(8) 0.023(6) 0.030(8) -0.002(5) 0.014(7) -0.011(6) N48 0.030(7) 0.025(5) 0.021(6) 0.011(4) 0.006(5) -0.009(5) C49 0.013(7) 0.026(7) 0.048(9) 0.002(6) 0.014(7) 0.006(6) C50 0.053(10) 0.036(7) 0.019(7) 0.004(6) 0.016(7) 0.011(7) C51 0.035(9) 0.018(6) 0.034(8) 0.002(5) 0.016(7) -0.011(6) C52 0.055(10) 0.028(7) 0.019(7) -0.012(5) 0.012(7) 0.003(7) N53 0.034(7) 0.053(7) 0.022(6) 0.001(5) 0.004(5) -0.004(6) Cl1 0.053(2) 0.0375(18) 0.0293(18) -0.0030(13) 0.0097(17) -0.0040(16) Cl2 0.042(2) 0.047(2) 0.059(2) -0.0099(17) 0.0154(19) -0.0006(17) O60 0.065(10) 0.139(13) 0.113(12) -0.003(10) -0.005(9) 0.011(10) C60 0.069(10) 0.087(12) 0.055(11) -0.021(10) 0.012(10) 0.012(10) C61 0.084(13) 0.138(15) 0.104(13) 0.017(12) 0.040(12) -0.017(12) C62 0.077(13) 0.118(14) 0.096(13) 0.000(12) 0.013(11) 0.013(12) O80 0.048(6) 0.050(6) 0.052(6) -0.002(5) 0.015(5) -0.008(5) O90 0.045(6) 0.029(5) 0.044(6) -0.003(4) 0.023(5) -0.003(4) O100 0.050(7) 0.060(6) 0.069(7) 0.004(5) -0.003(6) 0.006(5) O110 0.045(12) 0.041(10) 0.045(11) 0.001(8) 0.031(10) 0.026(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 Pt1 N12 1.924(9) . ? Pt1 N16 2.010(9) . ? Pt1 N1 2.033(9) . ? Pt1 N48 2.052(9) . ? Pt1 Pt2 3.1480(7) . ? Pt2 N42 1.947(8) . ? Pt2 N46 2.010(8) . ? Pt2 N31 2.051(9) . ? Pt2 N18 2.058(9) . ? N1 C2 1.344(14) . ? N1 C14 1.370(15) . ? C2 C3 1.435(17) . ? C3 C4 1.365(18) . ? C4 C5 1.406(17) . ? C5 C14 1.412(17) . ? C5 C6 1.463(18) . ? C6 C7 1.348(18) . ? C7 C8 1.398(18) . ? C8 C13 1.370(17) . ? C8 C9 1.415(17) . ? C9 C10 1.401(18) . ? C10 C11 1.389(16) . ? C11 N12 1.331(13) . ? C11 C15 1.487(17) . ? N12 C13 1.367(15) . ? C13 C14 1.407(16) . ? C15 O15 1.231(13) . ? C15 N16 1.377(14) . ? N16 C17 1.417(15) . ? C17 C22 1.366(15) . ? C17 N18 1.372(15) . ? N18 C19 1.353(14) . ? C19 N23 1.342(14) . ? C19 C20 1.450(15) . ? C20 C21 1.325(16) . ? C21 C22 1.406(16) . ? N31 C32 1.342(13) . ? N31 C44 1.363(13) . ? C32 C33 1.428(16) . ? C33 C34 1.353(17) . ? C34 C35 1.413(16) . ? C35 C44 1.408(15) . ? C35 C36 1.416(15) . ? C36 C37 1.339(16) . ? C37 C38 1.425(16) . ? C38 C39 1.383(15) . ? C38 C43 1.389(15) . ? C39 C40 1.441(16) . ? C40 C41 1.365(15) . ? C41 N42 1.315(13) . ? C41 C45 1.477(16) . ? N42 C43 1.365(14) . ? C43 C44 1.405(15) . ? C45 O45 1.247(13) . ? C45 N46 1.372(14) . ? N46 C47 1.418(14) . ? C47 N48 1.368(14) . ? C47 C52 1.376(16) . ? N48 C49 1.362(14) . ? C49 N53 1.353(14) . ? C49 C50 1.402(16) . ? C50 C51 1.367(16) . ? C51 C52 1.380(15) . ? O60 C60 1.174(15) . ? C60 C61 1.443(16) . ? C60 C62 1.506(17) . ? O60' C60' 1.227(19) . ? C60' C62' 1.472(19) . ? C60' C61' 1.482(19) . ? O70 S70 1.621(18) . ? S70 C72 1.785(18) . ? S70 C71 1.825(18) . ? O70' S70' 1.475(18) . ? S70' C71' 1.778(19) . ? S70' C72' 1.791(19) . ? O70" S70" 1.478(18) . ? S70" C71" 1.799(19) . ? S70" C72" 1.800(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Pt1 N16 78.9(4) . . ? N12 Pt1 N1 81.6(4) . . ? N16 Pt1 N1 160.5(4) . . ? N12 Pt1 N48 175.8(4) . . ? N16 Pt1 N48 101.5(4) . . ? N1 Pt1 N48 98.1(4) . . ? N12 Pt1 Pt2 107.5(3) . . ? N16 Pt1 Pt2 66.9(3) . . ? N1 Pt1 Pt2 118.2(3) . . ? N48 Pt1 Pt2 76.3(3) . . ? N42 Pt2 N46 78.3(4) . . ? N42 Pt2 N31 82.0(4) . . ? N46 Pt2 N31 160.3(4) . . ? N42 Pt2 N18 174.6(4) . . ? N46 Pt2 N18 101.6(4) . . ? N31 Pt2 N18 98.0(4) . . ? N42 Pt2 Pt1 108.3(3) . . ? N46 Pt2 Pt1 68.1(3) . . ? N31 Pt2 Pt1 119.0(3) . . ? N18 Pt2 Pt1 76.4(3) . . ? C2 N1 C14 117.4(10) . . ? C2 N1 Pt1 132.5(9) . . ? C14 N1 Pt1 110.0(7) . . ? N1 C2 C3 121.9(13) . . ? C4 C3 C2 119.9(13) . . ? C3 C4 C5 119.3(12) . . ? C4 C5 C14 117.8(13) . . ? C4 C5 C6 124.5(13) . . ? C14 C5 C6 117.5(12) . . ? C7 C6 C5 120.2(13) . . ? C6 C7 C8 123.3(14) . . ? C13 C8 C7 116.2(13) . . ? C13 C8 C9 115.6(11) . . ? C7 C8 C9 128.2(13) . . ? C10 C9 C8 121.3(12) . . ? C11 C10 C9 119.3(12) . . ? N12 C11 C10 119.0(12) . . ? N12 C11 C15 112.8(10) . . ? C10 C11 C15 128.2(11) . . ? C11 N12 C13 122.3(10) . . ? C11 N12 Pt1 120.4(9) . . ? C13 N12 Pt1 117.2(8) . . ? N12 C13 C8 122.5(11) . . ? N12 C13 C14 112.5(12) . . ? C8 C13 C14 124.9(13) . . ? N1 C14 C13 118.7(11) . . ? N1 C14 C5 123.5(11) . . ? C13 C14 C5 117.7(13) . . ? O15 C15 N16 126.0(12) . . ? O15 C15 C11 122.5(11) . . ? N16 C15 C11 111.1(10) . . ? C15 N16 C17 123.3(9) . . ? C15 N16 Pt1 116.2(8) . . ? C17 N16 Pt1 120.2(7) . . ? C22 C17 N18 123.6(12) . . ? C22 C17 N16 124.0(12) . . ? N18 C17 N16 112.4(10) . . ? C19 N18 C17 119.7(10) . . ? C19 N18 Pt2 119.7(8) . . ? C17 N18 Pt2 120.6(8) . . ? N23 C19 N18 119.8(10) . . ? N23 C19 C20 122.2(11) . . ? N18 C19 C20 118.0(11) . . ? C21 C20 C19 120.3(12) . . ? C20 C21 C22 121.8(12) . . ? C17 C22 C21 116.4(12) . . ? C32 N31 C44 118.9(10) . . ? C32 N31 Pt2 130.6(8) . . ? C44 N31 Pt2 110.5(7) . . ? N31 C32 C33 119.7(12) . . ? C34 C33 C32 121.0(13) . . ? C33 C34 C35 120.5(12) . . ? C44 C35 C34 115.5(11) . . ? C44 C35 C36 117.1(10) . . ? C34 C35 C36 127.4(11) . . ? C37 C36 C35 123.0(11) . . ? C36 C37 C38 121.8(11) . . ? C39 C38 C43 117.5(11) . . ? C39 C38 C37 127.2(11) . . ? C43 C38 C37 115.2(11) . . ? C38 C39 C40 119.8(11) . . ? C41 C40 C39 119.7(11) . . ? N42 C41 C40 118.4(11) . . ? N42 C41 C45 112.4(10) . . ? C40 C41 C45 129.2(11) . . ? C41 N42 C43 124.7(10) . . ? C41 N42 Pt2 120.7(8) . . ? C43 N42 Pt2 114.4(7) . . ? N42 C43 C38 119.7(11) . . ? N42 C43 C44 116.0(10) . . ? C38 C43 C44 124.2(11) . . ? N31 C44 C43 117.0(10) . . ? N31 C44 C35 124.3(10) . . ? C43 C44 C35 118.6(10) . . ? O45 C45 N46 126.7(11) . . ? O45 C45 C41 120.9(11) . . ? N46 C45 C41 112.4(10) . . ? C45 N46 C47 121.2(9) . . ? C45 N46 Pt2 116.1(8) . . ? C47 N46 Pt2 122.5(7) . . ? N48 C47 C52 123.1(11) . . ? N48 C47 N46 114.2(9) . . ? C52 C47 N46 122.7(11) . . ? C49 N48 C47 118.6(9) . . ? C49 N48 Pt1 121.2(8) . . ? C47 N48 Pt1 119.9(7) . . ? N53 C49 N48 119.6(10) . . ? N53 C49 C50 120.2(12) . . ? N48 C49 C50 120.2(11) . . ? C51 C50 C49 119.2(11) . . ? C50 C51 C52 121.6(11) . . ? C47 C52 C51 117.1(12) . . ? O60 C60 C61 136(2) . . ? O60 C60 C62 115(2) . . ? C61 C60 C62 108.6(17) . . ? O60' C60' C62' 125(3) . . ? O60' C60' C61' 115(3) . . ? C62' C60' C61' 121(3) . . ? O70 S70 C72 99.9(17) . . ? O70 S70 C71 107.3(17) . . ? C72 S70 C71 95.8(12) . . ? O70' S70' C71' 110(2) . . ? O70' S70' C72' 116(2) . . ? C71' S70' C72' 97.2(13) . . ? O70" S70" C71" 112(2) . . ? O70" S70" C72" 116(2) . . ? C71" S70" C72" 106(3) . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.900 _refine_diff_density_max 0.964 _refine_diff_density_min -1.284 _refine_diff_density_rms 0.231 #===END data_Compound_6 _database_code_depnum_ccdc_archive 'CCDC 691324' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H22 N10 O4 Pd2' _chemical_formula_sum 'C34 H22 N10 O4 Pd2' _chemical_formula_weight 847.42 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' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 18.1469(4) _cell_length_b 8.8803(2) _cell_length_c 19.3940(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.9360(10) _cell_angle_gamma 90.00 _cell_volume 3108.58(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 14037 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prisms _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.811 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 1.216 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.78778 _exptl_absorpt_correction_T_max 0.84258 _exptl_absorpt_process_details sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20913 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0285 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3558 _reflns_number_gt 3137 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+5.2874P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00048(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3558 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0325 _refine_ls_R_factor_gt 0.0263 _refine_ls_wR_factor_ref 0.0628 _refine_ls_wR_factor_gt 0.0611 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pd Pd 0.156824(9) 0.023079(19) 0.007572(8) 0.01557(8) Uani 1 1 d . . . N1 N 0.13820(10) -0.1455(2) 0.06606(9) 0.0185(4) Uani 1 1 d . . . C2 C 0.17561(13) -0.1532(3) 0.12925(12) 0.0214(5) Uani 1 1 d . . . C3 C 0.16474(14) -0.2752(3) 0.17117(13) 0.0271(5) Uani 1 1 d . . . H3A H 0.1906 -0.2828 0.2162 0.033 Uiso 1 1 calc R . . C4 C 0.11531(15) -0.3862(3) 0.14618(15) 0.0321(6) Uani 1 1 d . . . H4A H 0.1086 -0.4725 0.1737 0.039 Uiso 1 1 calc R . . C5 C 0.07578(14) -0.3728(3) 0.08177(14) 0.0286(6) Uani 1 1 d . . . H5A H 0.0408 -0.4474 0.0652 0.034 Uiso 1 1 calc R . . C6 C 0.08835(13) -0.2481(3) 0.04189(12) 0.0219(5) Uani 1 1 d . . . C7 C 0.22474(13) -0.0194(3) 0.14781(12) 0.0206(5) Uani 1 1 d . . . O7 O 0.25475(10) -0.0027(2) 0.20677(9) 0.0269(4) Uani 1 1 d . . . N8 N 0.22872(10) 0.0712(2) 0.09197(9) 0.0168(4) Uani 1 1 d . . . C9 C 0.27270(12) 0.2011(3) 0.09675(10) 0.0162(4) Uani 1 1 d . . . N10 N 0.32261(10) 0.2095(2) 0.04994(9) 0.0159(4) Uani 1 1 d . . . C11 C 0.36385(13) 0.3349(3) 0.04729(11) 0.0207(5) Uani 1 1 d . . . H11A H 0.3987 0.3409 0.0141 0.025 Uiso 1 1 calc R . . C12 C 0.35719(14) 0.4550(3) 0.09121(13) 0.0255(5) Uani 1 1 d . . . H12A H 0.3867 0.5426 0.0881 0.031 Uiso 1 1 calc R . . C13 C 0.30649(14) 0.4455(3) 0.14011(12) 0.0245(5) Uani 1 1 d . . . H13A H 0.3011 0.5264 0.1712 0.029 Uiso 1 1 calc R . . C14 C 0.26417(13) 0.3173(3) 0.14292(11) 0.0212(5) Uani 1 1 d . . . H14A H 0.2295 0.3087 0.1762 0.025 Uiso 1 1 calc R . . C15 C 0.05030(13) -0.2134(3) -0.02876(12) 0.0221(5) Uani 1 1 d . . . O15 O 0.00382(9) -0.3032(2) -0.05560(9) 0.0288(4) Uani 1 1 d . . . N16 N 0.07409(10) -0.0838(2) -0.05546(9) 0.0204(4) Uani 1 1 d . . . C17 C 0.04345(13) -0.0335(3) -0.12174(12) 0.0215(5) Uani 1 1 d . . . N18 N 0.08852(13) 0.0542(3) -0.15372(11) 0.0313(5) Uani 1 1 d . . . C19 C 0.06349(16) 0.1133(3) -0.21508(13) 0.0360(7) Uani 1 1 d . . . H19A H 0.0955 0.1777 -0.2373 0.043 Uiso 1 1 calc R . . C20 C -0.00659(15) 0.0857(3) -0.24808(13) 0.0332(6) Uani 1 1 d . . . H20A H -0.0227 0.1298 -0.2917 0.040 Uiso 1 1 calc R . . C21 C -0.05196(16) -0.0084(3) -0.21500(15) 0.0347(6) Uani 1 1 d . . . H21A H -0.1001 -0.0319 -0.2363 0.042 Uiso 1 1 calc R . . C22 C -0.02785(14) -0.0686(3) -0.15115(14) 0.0303(6) Uani 1 1 d . . . H22A H -0.0591 -0.1325 -0.1277 0.036 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01602(11) 0.01619(11) 0.01436(10) -0.00077(6) 0.00095(6) -0.00196(6) N1 0.0185(9) 0.0158(10) 0.0217(9) 0.0012(8) 0.0044(7) -0.0004(8) C2 0.0203(11) 0.0213(13) 0.0228(11) 0.0018(9) 0.0037(9) 0.0010(9) C3 0.0259(13) 0.0262(14) 0.0293(13) 0.0087(10) 0.0031(10) 0.0012(10) C4 0.0322(14) 0.0228(14) 0.0425(15) 0.0125(11) 0.0092(12) -0.0003(11) C5 0.0269(13) 0.0193(13) 0.0403(14) 0.0009(11) 0.0067(11) -0.0046(10) C6 0.0189(11) 0.0190(12) 0.0285(12) -0.0019(9) 0.0050(9) -0.0006(9) C7 0.0192(11) 0.0252(13) 0.0175(11) 0.0038(9) 0.0023(9) 0.0013(9) O7 0.0286(10) 0.0342(11) 0.0172(8) 0.0060(7) -0.0013(7) -0.0064(7) N8 0.0181(9) 0.0195(10) 0.0127(8) -0.0001(7) 0.0006(7) -0.0028(8) C9 0.0164(10) 0.0187(12) 0.0127(10) 0.0014(8) -0.0019(8) -0.0006(9) N10 0.0152(9) 0.0174(10) 0.0146(8) 0.0003(7) -0.0015(7) 0.0003(7) C11 0.0197(11) 0.0225(13) 0.0198(11) 0.0024(9) 0.0011(9) -0.0034(9) C12 0.0279(13) 0.0215(13) 0.0261(12) -0.0001(10) -0.0017(10) -0.0070(10) C13 0.0304(13) 0.0215(13) 0.0201(11) -0.0060(9) -0.0040(10) 0.0013(10) C14 0.0223(12) 0.0240(13) 0.0171(10) -0.0008(9) 0.0012(9) 0.0025(10) C15 0.0192(11) 0.0193(12) 0.0280(12) -0.0068(10) 0.0029(9) -0.0007(9) O15 0.0256(9) 0.0238(10) 0.0360(10) -0.0062(8) -0.0007(7) -0.0070(7) N16 0.0199(10) 0.0208(10) 0.0201(9) -0.0042(8) 0.0008(7) -0.0032(8) C17 0.0215(12) 0.0234(13) 0.0195(11) -0.0072(9) 0.0017(9) 0.0018(9) N18 0.0308(12) 0.0409(14) 0.0214(10) -0.0030(9) -0.0011(9) -0.0074(10) C19 0.0393(16) 0.0456(18) 0.0226(13) -0.0014(12) 0.0006(11) -0.0078(13) C20 0.0331(14) 0.0435(17) 0.0219(12) -0.0037(11) -0.0030(10) 0.0027(13) C21 0.0255(14) 0.0439(18) 0.0330(15) -0.0078(12) -0.0054(11) 0.0029(12) C22 0.0221(12) 0.0357(15) 0.0329(13) -0.0046(12) 0.0021(10) -0.0001(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pd N1 1.9294(18) . ? Pd N8 2.0303(18) . ? Pd N10 2.0521(18) 2 ? Pd N16 2.0662(19) . ? N1 C6 1.334(3) . ? N1 C2 1.340(3) . ? C2 C3 1.381(3) . ? C2 C7 1.506(3) . ? C3 C4 1.386(4) . ? C4 C5 1.380(4) . ? C5 C6 1.383(3) . ? C6 C15 1.501(3) . ? C7 O7 1.224(3) . ? C7 N8 1.357(3) . ? N8 C9 1.400(3) . ? C9 N10 1.349(3) . ? C9 C14 1.386(3) . ? N10 C11 1.346(3) . ? N10 Pd 2.0521(18) 2 ? C11 C12 1.378(3) . ? C12 C13 1.390(4) . ? C13 C14 1.377(3) . ? C15 O15 1.236(3) . ? C15 N16 1.352(3) . ? N16 C17 1.419(3) . ? C17 N18 1.328(3) . ? C17 C22 1.394(3) . ? N18 C19 1.336(3) . ? C19 C20 1.385(4) . ? C20 C21 1.377(4) . ? C21 C22 1.378(4) . ? 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 Pd N8 80.01(8) . . ? N1 Pd N10 176.91(7) . 2 ? N8 Pd N10 97.50(7) . 2 ? N1 Pd N16 80.26(8) . . ? N8 Pd N16 160.17(8) . . ? N10 Pd N16 102.17(7) 2 . ? C6 N1 C2 123.2(2) . . ? C6 N1 Pd 118.48(16) . . ? C2 N1 Pd 118.31(16) . . ? N1 C2 C3 119.3(2) . . ? N1 C2 C7 114.2(2) . . ? C3 C2 C7 126.5(2) . . ? C2 C3 C4 118.6(2) . . ? C5 C4 C3 120.8(2) . . ? C4 C5 C6 118.3(2) . . ? N1 C6 C5 119.7(2) . . ? N1 C6 C15 114.3(2) . . ? C5 C6 C15 126.0(2) . . ? O7 C7 N8 128.2(2) . . ? O7 C7 C2 120.9(2) . . ? N8 C7 C2 110.9(2) . . ? C7 N8 C9 120.84(18) . . ? C7 N8 Pd 115.83(15) . . ? C9 N8 Pd 122.76(14) . . ? N10 C9 C14 121.4(2) . . ? N10 C9 N8 114.77(19) . . ? C14 C9 N8 123.73(19) . . ? C11 N10 C9 119.11(19) . . ? C11 N10 Pd 120.92(15) . 2 ? C9 N10 Pd 119.57(15) . 2 ? N10 C11 C12 122.1(2) . . ? C11 C12 C13 118.8(2) . . ? C14 C13 C12 119.2(2) . . ? C13 C14 C9 119.3(2) . . ? O15 C15 N16 128.3(2) . . ? O15 C15 C6 118.8(2) . . ? N16 C15 C6 112.9(2) . . ? C15 N16 C17 120.3(2) . . ? C15 N16 Pd 113.95(15) . . ? C17 N16 Pd 125.75(16) . . ? N18 C17 C22 122.0(2) . . ? N18 C17 N16 113.9(2) . . ? C22 C17 N16 124.1(2) . . ? C17 N18 C19 118.5(2) . . ? N18 C19 C20 123.6(3) . . ? C21 C20 C19 117.2(3) . . ? C20 C21 C22 120.3(3) . . ? C21 C22 C17 118.4(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.745 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.085 #===END data_Compound_L7 _database_code_depnum_ccdc_archive 'CCDC 691325' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H23 N3 O4, H2 O' _chemical_formula_sum 'C23 H25 N3 O5' _chemical_formula_weight 423.46 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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 9.24730(10) _cell_length_b 9.24730(10) _cell_length_c 23.1554(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1980.08(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 7845 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88228 _exptl_absorpt_correction_T_max 1.06279 _exptl_absorpt_process_details sortav _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4477 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0882 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2256 _reflns_number_gt 1801 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Results of chirality/polarity tests _refine_ls_R_factor_obs+ 0.0483 _refine_ls_wR_factor_obs+ 0.1019 _refine_ls_abs_structure_Flack+ 0.0(15) _refine_ls_R_factor_obs- 0.0484 _refine_ls_wR_factor_obs- 0.1019 _refine_ls_abs_structure_Flack- 1.1(15) ; _chemical_absolute_configuration unk _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^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.016(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(15) _refine_ls_number_reflns 2256 _refine_ls_number_parameters 155 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1019 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 1.42768(17) 0.42768(17) 0.0000 0.0248(5) Uani 1 2 d S . . C2 C 1.4172(2) 0.5454(2) 0.03375(8) 0.0258(5) Uani 1 1 d . . . C3 C 1.5209(2) 0.6538(2) 0.03525(9) 0.0279(5) Uani 1 1 d . . . H3A H 1.5097 0.7350 0.0600 0.033 Uiso 1 1 calc R . . C4 C 1.6412(2) 0.6412(2) 0.0000 0.0309(7) Uani 1 2 d S . . H4A H 1.7138 0.7138 0.0000 0.037 Uiso 1 2 calc SR . . C5 C 1.2844(2) 0.5627(2) 0.07058(9) 0.0257(5) Uani 1 1 d . . . O5 O 1.27019(15) 0.67425(14) 0.09971(6) 0.0326(4) Uani 1 1 d . . . N6 N 1.18705(17) 0.45465(17) 0.06874(7) 0.0244(4) Uani 1 1 d D . . H6 H 1.205(2) 0.3809(13) 0.0444(6) 0.022(5) Uiso 1 1 d D . . C7 C 1.0506(2) 0.4580(2) 0.09701(9) 0.0242(4) Uani 1 1 d . . . C8 C 0.9337(2) 0.3921(2) 0.06989(9) 0.0271(5) Uani 1 1 d . . . H8A H 0.9471 0.3429 0.0343 0.033 Uiso 1 1 calc R . . C9 C 0.7968(2) 0.3983(2) 0.09512(9) 0.0288(5) Uani 1 1 d . . . H9A H 0.7178 0.3521 0.0765 0.035 Uiso 1 1 calc R . . C10 C 0.7733(2) 0.47084(19) 0.14717(9) 0.0250(5) Uani 1 1 d . . . C11 C 0.8931(2) 0.5304(2) 0.17478(9) 0.0256(5) Uani 1 1 d . . . H11A H 0.8806 0.5761 0.2112 0.031 Uiso 1 1 calc R . . C12 C 1.0305(2) 0.5249(2) 0.15051(9) 0.0263(5) Uani 1 1 d . . . H12A H 1.1104 0.5665 0.1702 0.032 Uiso 1 1 calc R . . C13 C 0.6229(2) 0.4942(2) 0.17127(9) 0.0288(5) Uani 1 1 d . . . H13A H 0.6314 0.5181 0.2128 0.035 Uiso 1 1 calc R . . H13B H 0.5794 0.5788 0.1517 0.035 Uiso 1 1 calc R . . C14 C 0.5213(2) 0.3675(2) 0.16497(9) 0.0297(5) Uani 1 1 d . . . H14A H 0.5125 0.3401 0.1238 0.036 Uiso 1 1 calc R . . H14B H 0.5589 0.2833 0.1867 0.036 Uiso 1 1 calc R . . O15 O 0.38357(14) 0.40951(15) 0.18721(7) 0.0324(4) Uani 1 1 d D . . H15 H 0.323(2) 0.344(2) 0.1715(11) 0.069(9) Uiso 1 1 d D . . O20 O 0.32680(14) 0.67320(14) 0.2500 0.0289(5) Uani 1 2 d SD . . H20A H 0.342(3) 0.6004(18) 0.2249(8) 0.063(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.0239(7) 0.0239(7) 0.0268(12) 0.0016(8) -0.0016(8) 0.0008(10) C2 0.0282(11) 0.0265(10) 0.0228(10) 0.0028(9) -0.0036(9) 0.0015(8) C3 0.0308(11) 0.0239(10) 0.0290(11) 0.0005(9) -0.0027(10) -0.0021(8) C4 0.0286(9) 0.0286(9) 0.0355(18) 0.0028(10) -0.0028(10) -0.0049(12) C5 0.0270(11) 0.0225(10) 0.0277(11) 0.0032(9) -0.0017(9) 0.0014(8) O5 0.0344(9) 0.0234(7) 0.0401(9) -0.0044(7) 0.0022(7) -0.0002(6) N6 0.0242(9) 0.0247(9) 0.0243(9) -0.0021(8) 0.0014(8) 0.0012(7) C7 0.0246(10) 0.0212(10) 0.0267(11) 0.0038(9) 0.0008(9) 0.0010(8) C8 0.0319(11) 0.0234(10) 0.0261(11) -0.0018(9) 0.0006(9) 0.0032(9) C9 0.0286(11) 0.0299(11) 0.0279(12) -0.0022(9) -0.0002(9) -0.0042(9) C10 0.0287(11) 0.0208(10) 0.0254(11) 0.0015(9) 0.0010(9) 0.0008(8) C11 0.0292(11) 0.0240(10) 0.0235(11) -0.0019(9) 0.0003(9) 0.0010(9) C12 0.0276(11) 0.0253(10) 0.0262(11) 0.0006(9) -0.0016(9) -0.0016(9) C13 0.0317(11) 0.0292(11) 0.0253(11) -0.0010(9) 0.0002(9) 0.0002(9) C14 0.0270(11) 0.0307(11) 0.0316(13) -0.0004(9) 0.0018(9) 0.0010(9) O15 0.0255(8) 0.0349(9) 0.0368(9) -0.0054(7) 0.0034(7) -0.0017(6) O20 0.0287(7) 0.0287(7) 0.0293(12) -0.0014(7) -0.0014(7) 0.0042(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 N1 C2 1.344(2) . ? N1 C2 1.344(2) 7_645 ? C2 C3 1.387(3) . ? C2 C5 1.504(3) . ? C3 C4 1.384(2) . ? C4 C3 1.384(2) 7_645 ? C5 O5 1.239(2) . ? C5 N6 1.346(2) . ? N6 C7 1.422(2) . ? C7 C8 1.390(3) . ? C7 C12 1.398(3) . ? C8 C9 1.396(3) . ? C9 C10 1.396(3) . ? C10 C11 1.393(3) . ? C10 C13 1.514(3) . ? C11 C12 1.390(3) . ? C13 C14 1.508(3) . ? C14 O15 1.428(2) . ? 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 C2 N1 C2 117.1(2) . 7_645 ? N1 C2 C3 123.4(2) . . ? N1 C2 C5 118.34(17) . . ? C3 C2 C5 118.29(18) . . ? C4 C3 C2 118.7(2) . . ? C3 C4 C3 118.9(3) 7_645 . ? O5 C5 N6 124.37(18) . . ? O5 C5 C2 118.91(17) . . ? N6 C5 C2 116.71(18) . . ? C5 N6 C7 124.26(17) . . ? C8 C7 C12 119.41(18) . . ? C8 C7 N6 118.18(17) . . ? C12 C7 N6 122.41(17) . . ? C7 C8 C9 119.9(2) . . ? C8 C9 C10 121.48(19) . . ? C11 C10 C9 117.55(19) . . ? C11 C10 C13 120.36(18) . . ? C9 C10 C13 121.95(17) . . ? C12 C11 C10 121.80(19) . . ? C11 C12 C7 119.77(18) . . ? C14 C13 C10 115.22(17) . . ? O15 C14 C13 108.04(16) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.234 _refine_diff_density_min -0.176 _refine_diff_density_rms 0.046 #===END