# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Katja Heinze' _publ_contact_author_name 'Katja Heinze' _publ_contact_author_email katja.heinze@uni-mainz.de _publ_section_title ; Rhenium(I) and Platinum(II) Complexes with Diimine Ligands Bearing Acidic Phenol Substituents: Hydrogen-Bonding, Acid-Base Chemistry and Optical Properties ; # Attachment '- complex1.cif' data_1106a _database_code_depnum_ccdc_archive 'CCDC 775540' #TrackingRef '- complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H10 Cl N2 O4 Re' _chemical_formula_weight 503.90 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4274(8) _cell_length_b 9.1175(6) _cell_length_c 14.0330(9) _cell_angle_alpha 90.00 _cell_angle_beta 100.057(4) _cell_angle_gamma 90.00 _cell_volume 1565.60(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 7.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1209 _exptl_absorpt_correction_T_max 0.6919 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 48112 _diffrn_reflns_av_R_equivalents 0.1176 _diffrn_reflns_av_sigmaI/netI 0.0311 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3079 _reflns_number_gt 2875 _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. ; _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^)+(0.0460P)^2^+1.2433P] 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 3079 _refine_ls_number_parameters 208 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0675 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl1 Cl 0.56399(8) 0.55640(11) 0.64921(7) 0.0328(2) Uani 1 1 d U . . Re1 Re 0.596335(10) 0.321183(14) 0.739669(8) 0.01638(8) Uani 1 1 d U . . C3 C 0.7333(3) 0.3836(4) 0.8134(2) 0.0208(7) Uani 1 1 d . . . O3 O 0.8184(2) 0.4159(3) 0.85549(19) 0.0303(6) Uani 1 1 d . . . N2 N 0.6626(2) 0.2463(3) 0.61483(19) 0.0181(6) Uani 1 1 d . . . C10 C 0.3440(3) 0.2498(4) 0.6501(2) 0.0221(7) Uani 1 1 d . . . O2 O 0.4757(2) 0.4265(4) 0.9001(2) 0.0386(7) Uani 1 1 d . . . N1 N 0.4555(2) 0.2487(3) 0.6350(2) 0.0203(6) Uani 1 1 d . . . O4 O 0.0243(2) 0.2491(4) 0.6968(2) 0.0413(7) Uani 1 1 d . . . H4A H -0.0073 0.1705 0.6771 0.062 Uiso 1 1 calc R . . O1 O 0.6279(3) 0.0380(4) 0.8558(2) 0.0480(8) Uani 1 1 d . . . C2 C 0.5205(3) 0.3892(4) 0.8403(3) 0.0233(7) Uani 1 1 d . . . C5 C 0.8045(4) 0.1792(4) 0.5284(3) 0.0269(9) Uani 1 1 d . . . H5A H 0.8804 0.1709 0.5270 0.032 Uiso 1 1 calc R . . C11 C 0.3177(3) 0.1730(4) 0.7285(3) 0.0257(9) Uani 1 1 d . . . H11A H 0.3737 0.1240 0.7716 0.031 Uiso 1 1 calc R . . C15 C 0.2629(4) 0.3235(4) 0.5872(3) 0.0311(10) Uani 1 1 d . . . H15A H 0.2803 0.3746 0.5329 0.037 Uiso 1 1 calc R . . C12 C 0.2113(4) 0.1670(4) 0.7446(3) 0.0302(9) Uani 1 1 d . . . H12A H 0.1934 0.1112 0.7968 0.036 Uiso 1 1 calc R . . C4 C 0.7690(3) 0.2341(4) 0.6095(3) 0.0229(7) Uani 1 1 d . . . H4B H 0.8219 0.2641 0.6632 0.028 Uiso 1 1 calc R . . C8 C 0.5875(3) 0.2064(4) 0.5367(3) 0.0213(7) Uani 1 1 d . . . C9 C 0.4746(3) 0.2140(4) 0.5509(3) 0.0237(7) Uani 1 1 d . . . H9A H 0.4163 0.1937 0.4991 0.028 Uiso 1 1 calc R . . C14 C 0.1562(4) 0.3218(5) 0.6046(4) 0.0380(11) Uani 1 1 d . . . H14A H 0.1008 0.3739 0.5628 0.046 Uiso 1 1 calc R . . C13 C 0.1298(3) 0.2448(5) 0.6823(3) 0.0323(9) Uani 1 1 d . . . C1 C 0.6162(3) 0.1345(5) 0.8101(3) 0.0292(9) Uani 1 1 d . . . C6 C 0.7278(3) 0.1363(5) 0.4490(3) 0.0289(8) Uani 1 1 d . . . H6A H 0.7505 0.0974 0.3929 0.035 Uiso 1 1 calc R . . C7 C 0.6169(3) 0.1514(4) 0.4530(3) 0.0260(8) Uani 1 1 d . . . H7A H 0.5627 0.1244 0.3994 0.031 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 Cl1 0.0374(5) 0.0301(5) 0.0321(5) 0.0031(4) 0.0094(4) 0.0040(4) Re1 0.01639(11) 0.01905(12) 0.01394(11) -0.00122(4) 0.00328(7) -0.00007(4) C3 0.0264(18) 0.0164(17) 0.0183(16) -0.0025(13) 0.0005(14) 0.0021(14) O3 0.0251(14) 0.0299(14) 0.0320(14) -0.0055(11) -0.0063(12) -0.0007(11) N2 0.0202(14) 0.0187(15) 0.0161(13) -0.0010(11) 0.0048(11) 0.0001(11) C10 0.0187(16) 0.0244(19) 0.0224(17) -0.0043(14) 0.0016(13) -0.0016(14) O2 0.0388(16) 0.0511(19) 0.0313(15) -0.0089(13) 0.0216(13) -0.0054(14) N1 0.0195(14) 0.0211(16) 0.0204(14) 0.0013(11) 0.0042(11) -0.0007(12) O4 0.0194(14) 0.052(2) 0.054(2) 0.0044(16) 0.0106(13) -0.0018(14) O1 0.061(2) 0.0324(17) 0.053(2) 0.0019(16) 0.0156(17) -0.0027(16) C2 0.0220(17) 0.0260(19) 0.0227(17) 0.0017(14) 0.0062(14) -0.0025(15) C5 0.025(2) 0.032(2) 0.027(2) 0.0008(14) 0.0131(17) 0.0025(14) C11 0.0200(19) 0.035(2) 0.0224(19) -0.0024(14) 0.0041(16) 0.0002(13) C15 0.023(2) 0.042(3) 0.028(2) 0.0063(15) 0.0001(17) 0.0029(15) C12 0.025(2) 0.037(2) 0.030(2) -0.0004(15) 0.0107(18) -0.0038(15) C4 0.0211(17) 0.0217(18) 0.0260(18) -0.0004(14) 0.0043(14) -0.0003(14) C8 0.0222(18) 0.0219(16) 0.0199(17) 0.0037(14) 0.0041(14) 0.0023(14) C9 0.0264(19) 0.0235(17) 0.0195(17) -0.0007(14) -0.0009(15) -0.0007(15) C14 0.024(2) 0.047(3) 0.041(3) 0.0083(18) 0.000(2) 0.0061(16) C13 0.0214(18) 0.041(2) 0.035(2) -0.0066(18) 0.0046(16) -0.0009(17) C1 0.026(2) 0.049(2) 0.0125(17) 0.0058(18) 0.0028(14) 0.0163(19) C6 0.034(2) 0.033(2) 0.0230(18) -0.0024(16) 0.0130(16) 0.0039(18) C7 0.031(2) 0.0287(18) 0.0182(18) -0.0002(15) 0.0044(16) -0.0009(16) _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 Cl1 Re1 2.4887(10) . ? Re1 C3 1.917(3) . ? Re1 C2 1.932(4) . ? Re1 C1 1.962(5) . ? Re1 N2 2.172(3) . ? Re1 N1 2.182(3) . ? C3 O3 1.156(4) . ? N2 C4 1.342(5) . ? N2 C8 1.360(5) . ? C10 C11 1.390(5) . ? C10 C15 1.391(5) . ? C10 N1 1.438(4) . ? O2 C2 1.136(5) . ? N1 C9 1.284(5) . ? O4 C13 1.362(5) . ? O4 H4A 0.8400 . ? O1 C1 1.084(5) . ? C5 C4 1.384(5) . ? C5 C6 1.389(6) . ? C5 H5A 0.9500 . ? C11 C12 1.380(6) . ? C11 H11A 0.9500 . ? C15 C14 1.390(7) . ? C15 H15A 0.9500 . ? C12 C13 1.409(6) . ? C12 H12A 0.9500 . ? C4 H4B 0.9500 . ? C8 C7 1.383(5) . ? C8 C9 1.454(5) . ? C9 H9A 0.9500 . ? C14 C13 1.384(6) . ? C14 H14A 0.9500 . ? C6 C7 1.397(6) . ? C6 H6A 0.9500 . ? C7 H7A 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 C3 Re1 C2 90.63(15) . . ? C3 Re1 C1 87.94(16) . . ? C2 Re1 C1 86.84(16) . . ? C3 Re1 N2 95.88(13) . . ? C2 Re1 N2 173.04(13) . . ? C1 Re1 N2 95.84(13) . . ? C3 Re1 N1 170.20(13) . . ? C2 Re1 N1 98.77(13) . . ? C1 Re1 N1 95.29(15) . . ? N2 Re1 N1 74.62(10) . . ? C3 Re1 Cl1 93.91(10) . . ? C2 Re1 Cl1 92.30(11) . . ? C1 Re1 Cl1 177.96(12) . . ? N2 Re1 Cl1 84.81(8) . . ? N1 Re1 Cl1 83.01(8) . . ? O3 C3 Re1 176.6(3) . . ? C4 N2 C8 118.5(3) . . ? C4 N2 Re1 126.0(2) . . ? C8 N2 Re1 115.5(2) . . ? C11 C10 C15 120.1(4) . . ? C11 C10 N1 118.6(3) . . ? C15 C10 N1 121.3(3) . . ? C9 N1 C10 118.4(3) . . ? C9 N1 Re1 116.0(2) . . ? C10 N1 Re1 125.4(2) . . ? C13 O4 H4A 109.5 . . ? O2 C2 Re1 178.6(3) . . ? C4 C5 C6 119.3(4) . . ? C4 C5 H5A 120.4 . . ? C6 C5 H5A 120.4 . . ? C12 C11 C10 120.9(4) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C14 C15 C10 119.4(4) . . ? C14 C15 H15A 120.3 . . ? C10 C15 H15A 120.3 . . ? C11 C12 C13 119.0(4) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? N2 C4 C5 122.3(3) . . ? N2 C4 H4B 118.8 . . ? C5 C4 H4B 118.8 . . ? N2 C8 C7 122.4(3) . . ? N2 C8 C9 114.8(3) . . ? C7 C8 C9 122.5(3) . . ? N1 C9 C8 118.4(3) . . ? N1 C9 H9A 120.8 . . ? C8 C9 H9A 120.8 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? O4 C13 C14 118.1(4) . . ? O4 C13 C12 122.0(4) . . ? C14 C13 C12 120.0(4) . . ? O1 C1 Re1 174.1(4) . . ? C5 C6 C7 118.9(3) . . ? C5 C6 H6A 120.6 . . ? C7 C6 H6A 120.6 . . ? C8 C7 C6 118.6(4) . . ? C8 C7 H7A 120.7 . . ? C6 C7 H7A 120.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Re1 C3 O3 153(5) . . . . ? C1 Re1 C3 O3 66(5) . . . . ? N2 Re1 C3 O3 -30(5) . . . . ? N1 Re1 C3 O3 -44(6) . . . . ? Cl1 Re1 C3 O3 -115(5) . . . . ? C3 Re1 N2 C4 8.7(3) . . . . ? C2 Re1 N2 C4 167.9(10) . . . . ? C1 Re1 N2 C4 -79.8(3) . . . . ? N1 Re1 N2 C4 -173.7(3) . . . . ? Cl1 Re1 N2 C4 102.1(3) . . . . ? C3 Re1 N2 C8 -172.6(3) . . . . ? C2 Re1 N2 C8 -13.4(12) . . . . ? C1 Re1 N2 C8 98.9(3) . . . . ? N1 Re1 N2 C8 5.0(2) . . . . ? Cl1 Re1 N2 C8 -79.2(2) . . . . ? C11 C10 N1 C9 128.6(4) . . . . ? C15 C10 N1 C9 -50.2(5) . . . . ? C11 C10 N1 Re1 -57.4(4) . . . . ? C15 C10 N1 Re1 123.8(3) . . . . ? C3 Re1 N1 C9 7.2(9) . . . . ? C2 Re1 N1 C9 170.7(3) . . . . ? C1 Re1 N1 C9 -101.7(3) . . . . ? N2 Re1 N1 C9 -7.1(3) . . . . ? Cl1 Re1 N1 C9 79.4(3) . . . . ? C3 Re1 N1 C10 -166.9(7) . . . . ? C2 Re1 N1 C10 -3.4(3) . . . . ? C1 Re1 N1 C10 84.2(3) . . . . ? N2 Re1 N1 C10 178.8(3) . . . . ? Cl1 Re1 N1 C10 -94.7(3) . . . . ? C3 Re1 C2 O2 -103(14) . . . . ? C1 Re1 C2 O2 -15(14) . . . . ? N2 Re1 C2 O2 98(14) . . . . ? N1 Re1 C2 O2 80(14) . . . . ? Cl1 Re1 C2 O2 163(14) . . . . ? C15 C10 C11 C12 0.8(6) . . . . ? N1 C10 C11 C12 -178.1(3) . . . . ? C11 C10 C15 C14 1.2(6) . . . . ? N1 C10 C15 C14 -180.0(4) . . . . ? C10 C11 C12 C13 -2.4(6) . . . . ? C8 N2 C4 C5 -1.6(5) . . . . ? Re1 N2 C4 C5 177.1(3) . . . . ? C6 C5 C4 N2 0.6(6) . . . . ? C4 N2 C8 C7 1.2(5) . . . . ? Re1 N2 C8 C7 -177.6(3) . . . . ? C4 N2 C8 C9 176.1(3) . . . . ? Re1 N2 C8 C9 -2.7(4) . . . . ? C10 N1 C9 C8 -177.3(3) . . . . ? Re1 N1 C9 C8 8.2(4) . . . . ? N2 C8 C9 N1 -3.7(5) . . . . ? C7 C8 C9 N1 171.2(4) . . . . ? C10 C15 C14 C13 -1.5(6) . . . . ? C15 C14 C13 O4 178.9(4) . . . . ? C15 C14 C13 C12 -0.2(7) . . . . ? C11 C12 C13 O4 -176.9(4) . . . . ? C11 C12 C13 C14 2.1(6) . . . . ? C3 Re1 C1 O1 56(4) . . . . ? C2 Re1 C1 O1 -34(4) . . . . ? N2 Re1 C1 O1 152(4) . . . . ? N1 Re1 C1 O1 -133(4) . . . . ? Cl1 Re1 C1 O1 -99(5) . . . . ? C4 C5 C6 C7 0.7(6) . . . . ? N2 C8 C7 C6 0.1(6) . . . . ? C9 C8 C7 C6 -174.5(4) . . . . ? C5 C6 C7 C8 -1.0(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.251 _refine_diff_density_min -1.290 _refine_diff_density_rms 0.148 # Attachment '- complex4.cif' data_w1106a _database_code_depnum_ccdc_archive 'CCDC 775541' #TrackingRef '- complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H16 Cl N2 O5 Re' _chemical_formula_weight 573.99 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' Cl Cl 0.1484 0.1585 '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' Re Re -1.0185 7.2310 '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 7.08950(10) _cell_length_b 11.2851(2) _cell_length_c 12.3164(2) _cell_angle_alpha 97.4140(10) _cell_angle_beta 97.2240(10) _cell_angle_gamma 94.2410(10) _cell_volume 965.31(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.975 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 6.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3304 _exptl_absorpt_correction_T_max 0.8816 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 33461 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0213 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 27.90 _reflns_number_total 4617 _reflns_number_gt 4395 _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 ? _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^)+(0.0151P)^2^+0.4730P] 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 4617 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0166 _refine_ls_R_factor_gt 0.0150 _refine_ls_wR_factor_ref 0.0351 _refine_ls_wR_factor_gt 0.0346 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.739903(11) 0.720177(7) 0.053569(7) 0.01524(3) Uani 1 1 d . . . O1 O 0.7954(2) 0.46478(15) -0.04772(16) 0.0305(4) Uani 1 1 d . . . O2 O 0.3694(3) 0.68641(18) -0.11024(15) 0.0343(4) Uani 1 1 d . . . O3 O 0.5339(3) 0.61214(18) 0.22865(15) 0.0335(4) Uani 1 1 d . . . Cl1 Cl 0.68634(8) 0.92398(5) 0.13882(5) 0.02389(11) Uani 1 1 d . . . O5 O 0.6954(3) 0.90700(17) -0.47388(14) 0.0307(4) Uani 1 1 d . . . O4 O 1.2828(3) 0.55530(17) 0.52963(15) 0.0343(4) Uani 1 1 d . . . N2 N 1.0244(3) 0.75040(16) 0.15072(15) 0.0165(4) Uani 1 1 d . . . N1 N 0.9184(3) 0.81397(16) -0.04468(15) 0.0182(4) Uani 1 1 d . . . C11 C 1.1489(3) 0.81368(19) 0.10880(18) 0.0187(4) Uani 1 1 d . . . H11A H 1.2741 0.8359 0.1468 0.022 Uiso 1 1 calc R . . C12 C 1.0903(3) 0.8494(2) 0.00197(18) 0.0199(4) Uani 1 1 d . . . H12A H 1.1748 0.8970 -0.0325 0.024 Uiso 1 1 calc R . . C4 C 1.0842(3) 0.7075(2) 0.25301(18) 0.0181(4) Uani 1 1 d . . . C9 C 1.2117(3) 0.7761(2) 0.33587(18) 0.0211(4) Uani 1 1 d . . . H9A H 1.2530 0.8560 0.3276 0.025 Uiso 1 1 calc R . . C8 C 1.2802(3) 0.7298(2) 0.43095(19) 0.0236(5) Uani 1 1 d . . . H8A H 1.3661 0.7781 0.4878 0.028 Uiso 1 1 calc R . . C7 C 1.2216(3) 0.6119(2) 0.44197(19) 0.0245(5) Uani 1 1 d . . . C6 C 1.0891(3) 0.5432(2) 0.3596(2) 0.0263(5) Uani 1 1 d . . . H6A H 1.0469 0.4634 0.3679 0.032 Uiso 1 1 calc R . . C5 C 1.0196(3) 0.5907(2) 0.26658(19) 0.0224(5) Uani 1 1 d . . . H5A H 0.9279 0.5443 0.2116 0.027 Uiso 1 1 calc R . . C2 C 0.5067(3) 0.7016(2) -0.04713(19) 0.0217(5) Uani 1 1 d . . . C3 C 0.6084(3) 0.6513(2) 0.16177(19) 0.0214(5) Uani 1 1 d . . . C19 C 0.7958(4) 0.8636(3) -0.5629(2) 0.0404(7) Uani 1 1 d . . . H19A H 0.7359 0.8876 -0.6318 0.061 Uiso 1 1 calc R . . H19B H 0.7908 0.7759 -0.5703 0.061 Uiso 1 1 calc R . . H19C H 0.9292 0.8976 -0.5474 0.061 Uiso 1 1 calc R . . C16 C 0.7605(3) 0.8811(2) -0.37112(19) 0.0228(5) Uani 1 1 d . . . C17 C 0.9286(3) 0.8287(2) -0.34452(19) 0.0244(5) Uani 1 1 d . . . H17A H 1.0071 0.8074 -0.3998 0.029 Uiso 1 1 calc R . . C18 C 0.9811(3) 0.8079(2) -0.23674(19) 0.0230(5) Uani 1 1 d . . . H18A H 1.0969 0.7733 -0.2181 0.028 Uiso 1 1 calc R . . C13 C 0.8657(3) 0.8370(2) -0.15600(18) 0.0192(4) Uani 1 1 d . . . C14 C 0.6952(3) 0.8887(2) -0.18309(18) 0.0195(4) Uani 1 1 d . . . H14A H 0.6148 0.9077 -0.1284 0.023 Uiso 1 1 calc R . . C15 C 0.6450(3) 0.9117(2) -0.28977(19) 0.0227(5) Uani 1 1 d . . . H15A H 0.5313 0.9486 -0.3080 0.027 Uiso 1 1 calc R . . C10 C 1.4253(5) 0.6198(3) 0.6127(2) 0.0431(7) Uani 1 1 d . . . H10A H 1.4568 0.5700 0.6708 0.065 Uiso 1 1 calc R . . H10B H 1.3768 0.6937 0.6447 0.065 Uiso 1 1 calc R . . H10C H 1.5401 0.6400 0.5796 0.065 Uiso 1 1 calc R . . C1 C 0.7800(3) 0.5625(2) -0.01022(19) 0.0203(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Re1 0.01459(5) 0.01684(5) 0.01488(5) 0.00294(3) 0.00263(3) 0.00296(3) O1 0.0266(9) 0.0232(9) 0.0392(10) -0.0063(8) 0.0065(8) 0.0021(7) O2 0.0232(9) 0.0498(12) 0.0297(10) 0.0102(9) -0.0024(8) 0.0051(8) O3 0.0295(10) 0.0444(11) 0.0316(10) 0.0165(9) 0.0120(8) 0.0020(8) Cl1 0.0296(3) 0.0197(3) 0.0248(3) 0.0031(2) 0.0099(2) 0.0078(2) O5 0.0354(10) 0.0420(11) 0.0160(8) 0.0075(7) 0.0012(7) 0.0111(8) O4 0.0382(10) 0.0404(11) 0.0245(9) 0.0178(8) -0.0048(8) -0.0028(8) N2 0.0178(9) 0.0159(9) 0.0157(9) 0.0006(7) 0.0023(7) 0.0040(7) N1 0.0213(9) 0.0190(9) 0.0158(9) 0.0031(7) 0.0047(7) 0.0060(7) C11 0.0189(10) 0.0190(10) 0.0179(10) 0.0002(8) 0.0031(8) 0.0021(8) C12 0.0213(11) 0.0199(11) 0.0200(11) 0.0036(9) 0.0078(9) 0.0026(8) C4 0.0164(10) 0.0204(11) 0.0184(10) 0.0031(8) 0.0043(8) 0.0041(8) C9 0.0234(11) 0.0197(11) 0.0202(11) 0.0022(9) 0.0038(9) 0.0016(9) C8 0.0238(12) 0.0272(12) 0.0192(11) 0.0031(9) 0.0013(9) 0.0007(9) C7 0.0237(12) 0.0328(13) 0.0191(11) 0.0110(10) 0.0028(9) 0.0044(10) C6 0.0255(12) 0.0252(12) 0.0293(13) 0.0109(10) 0.0028(10) -0.0021(9) C5 0.0211(11) 0.0233(11) 0.0226(11) 0.0045(9) 0.0016(9) 0.0001(9) C2 0.0205(11) 0.0256(12) 0.0214(11) 0.0074(9) 0.0056(9) 0.0055(9) C3 0.0168(10) 0.0225(11) 0.0242(12) 0.0021(9) -0.0002(9) 0.0036(9) C19 0.0488(17) 0.0570(19) 0.0177(12) 0.0066(12) 0.0062(12) 0.0153(14) C16 0.0270(12) 0.0213(11) 0.0195(11) 0.0028(9) 0.0012(9) 0.0022(9) C17 0.0266(12) 0.0304(13) 0.0180(11) 0.0037(9) 0.0074(9) 0.0068(10) C18 0.0212(11) 0.0267(12) 0.0227(12) 0.0049(9) 0.0044(9) 0.0077(9) C13 0.0186(10) 0.0209(11) 0.0185(11) 0.0041(9) 0.0015(8) 0.0039(8) C14 0.0217(11) 0.0197(11) 0.0186(11) 0.0037(9) 0.0054(8) 0.0048(9) C15 0.0237(11) 0.0214(11) 0.0237(12) 0.0033(9) 0.0028(9) 0.0073(9) C10 0.0519(18) 0.0485(18) 0.0270(14) 0.0140(13) -0.0100(13) 0.0018(14) C1 0.0151(10) 0.0252(12) 0.0204(11) 0.0033(9) 0.0014(8) 0.0011(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 C1 1.906(2) . ? Re1 C2 1.919(2) . ? Re1 C3 1.929(2) . ? Re1 N1 2.1689(18) . ? Re1 N2 2.1911(18) . ? Re1 Cl1 2.4785(5) . ? O1 C1 1.158(3) . ? O2 C2 1.154(3) . ? O3 C3 1.150(3) . ? O5 C16 1.367(3) . ? O5 C19 1.434(3) . ? O4 C7 1.365(3) . ? O4 C10 1.427(3) . ? N2 C11 1.293(3) . ? N2 C4 1.434(3) . ? N1 C12 1.291(3) . ? N1 C13 1.437(3) . ? C11 C12 1.446(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C4 C9 1.385(3) . ? C4 C5 1.401(3) . ? C9 C8 1.390(3) . ? C9 H9A 0.9500 . ? C8 C7 1.393(3) . ? C8 H8A 0.9500 . ? C7 C6 1.401(3) . ? C6 C5 1.378(3) . ? C6 H6A 0.9500 . ? C5 H5A 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C16 C17 1.391(3) . ? C16 C15 1.397(3) . ? C17 C18 1.388(3) . ? C17 H17A 0.9500 . ? C18 C13 1.388(3) . ? C18 H18A 0.9500 . ? C13 C14 1.401(3) . ? C14 C15 1.380(3) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 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 C1 Re1 C2 86.25(10) . . ? C1 Re1 C3 89.20(10) . . ? C2 Re1 C3 90.23(9) . . ? C1 Re1 N1 95.98(8) . . ? C2 Re1 N1 98.04(8) . . ? C3 Re1 N1 170.49(8) . . ? C1 Re1 N2 93.43(8) . . ? C2 Re1 N2 172.32(8) . . ? C3 Re1 N2 97.44(8) . . ? N1 Re1 N2 74.35(7) . . ? C1 Re1 Cl1 179.18(7) . . ? C2 Re1 Cl1 93.93(7) . . ? C3 Re1 Cl1 90.00(7) . . ? N1 Re1 Cl1 84.79(5) . . ? N2 Re1 Cl1 86.50(5) . . ? C16 O5 C19 117.2(2) . . ? C7 O4 C10 117.2(2) . . ? C11 N2 C4 118.10(19) . . ? C11 N2 Re1 114.78(15) . . ? C4 N2 Re1 127.12(14) . . ? C12 N1 C13 117.71(19) . . ? C12 N1 Re1 115.72(15) . . ? C13 N1 Re1 126.54(14) . . ? N2 C11 C12 117.5(2) . . ? N2 C11 H11A 121.2 . . ? C12 C11 H11A 121.2 . . ? N1 C12 C11 117.2(2) . . ? N1 C12 H12A 121.4 . . ? C11 C12 H12A 121.4 . . ? C9 C4 C5 119.4(2) . . ? C9 C4 N2 121.69(19) . . ? C5 C4 N2 118.8(2) . . ? C4 C9 C8 121.1(2) . . ? C4 C9 H9A 119.5 . . ? C8 C9 H9A 119.5 . . ? C9 C8 C7 119.2(2) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? O4 C7 C8 124.8(2) . . ? O4 C7 C6 115.3(2) . . ? C8 C7 C6 119.9(2) . . ? C5 C6 C7 120.3(2) . . ? C5 C6 H6A 119.8 . . ? C7 C6 H6A 119.8 . . ? C6 C5 C4 120.0(2) . . ? C6 C5 H5A 120.0 . . ? C4 C5 H5A 120.0 . . ? O2 C2 Re1 177.1(2) . . ? O3 C3 Re1 178.0(2) . . ? O5 C19 H19A 109.5 . . ? O5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O5 C16 C17 124.7(2) . . ? O5 C16 C15 115.2(2) . . ? C17 C16 C15 120.0(2) . . ? C18 C17 C16 119.5(2) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C13 120.6(2) . . ? C17 C18 H18A 119.7 . . ? C13 C18 H18A 119.7 . . ? C18 C13 C14 119.9(2) . . ? C18 C13 N1 120.6(2) . . ? C14 C13 N1 119.47(19) . . ? C15 C14 C13 119.5(2) . . ? C15 C14 H14A 120.2 . . ? C13 C14 H14A 120.2 . . ? C14 C15 C16 120.4(2) . . ? C14 C15 H15A 119.8 . . ? C16 C15 H15A 119.8 . . ? O4 C10 H10A 109.5 . . ? O4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C1 Re1 176.56(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Re1 N2 C11 100.10(16) . . . . ? C2 Re1 N2 C11 12.7(7) . . . . ? C3 Re1 N2 C11 -170.26(16) . . . . ? N1 Re1 N2 C11 4.84(15) . . . . ? Cl1 Re1 N2 C11 -80.72(15) . . . . ? C1 Re1 N2 C4 -79.57(18) . . . . ? C2 Re1 N2 C4 -166.9(6) . . . . ? C3 Re1 N2 C4 10.07(18) . . . . ? N1 Re1 N2 C4 -174.82(18) . . . . ? Cl1 Re1 N2 C4 99.62(16) . . . . ? C1 Re1 N1 C12 -97.34(17) . . . . ? C2 Re1 N1 C12 175.62(17) . . . . ? C3 Re1 N1 C12 25.4(6) . . . . ? N2 Re1 N1 C12 -5.44(15) . . . . ? Cl1 Re1 N1 C12 82.38(16) . . . . ? C1 Re1 N1 C13 80.89(18) . . . . ? C2 Re1 N1 C13 -6.15(18) . . . . ? C3 Re1 N1 C13 -156.4(4) . . . . ? N2 Re1 N1 C13 172.79(18) . . . . ? Cl1 Re1 N1 C13 -99.39(17) . . . . ? C4 N2 C11 C12 175.87(19) . . . . ? Re1 N2 C11 C12 -3.8(2) . . . . ? C13 N1 C12 C11 -173.00(19) . . . . ? Re1 N1 C12 C11 5.4(3) . . . . ? N2 C11 C12 N1 -1.0(3) . . . . ? C11 N2 C4 C9 37.1(3) . . . . ? Re1 N2 C4 C9 -143.20(18) . . . . ? C11 N2 C4 C5 -139.3(2) . . . . ? Re1 N2 C4 C5 40.3(3) . . . . ? C5 C4 C9 C8 1.6(3) . . . . ? N2 C4 C9 C8 -174.8(2) . . . . ? C4 C9 C8 C7 1.0(4) . . . . ? C10 O4 C7 C8 -3.8(4) . . . . ? C10 O4 C7 C6 176.8(2) . . . . ? C9 C8 C7 O4 178.0(2) . . . . ? C9 C8 C7 C6 -2.5(4) . . . . ? O4 C7 C6 C5 -179.1(2) . . . . ? C8 C7 C6 C5 1.4(4) . . . . ? C7 C6 C5 C4 1.2(4) . . . . ? C9 C4 C5 C6 -2.7(3) . . . . ? N2 C4 C5 C6 173.8(2) . . . . ? C1 Re1 C2 O2 -16(4) . . . . ? C3 Re1 C2 O2 -106(4) . . . . ? N1 Re1 C2 O2 79(4) . . . . ? N2 Re1 C2 O2 71(4) . . . . ? Cl1 Re1 C2 O2 164(4) . . . . ? C1 Re1 C3 O3 120(6) . . . . ? C2 Re1 C3 O3 -153(6) . . . . ? N1 Re1 C3 O3 -3(6) . . . . ? N2 Re1 C3 O3 27(6) . . . . ? Cl1 Re1 C3 O3 -59(6) . . . . ? C19 O5 C16 C17 8.0(4) . . . . ? C19 O5 C16 C15 -172.3(2) . . . . ? O5 C16 C17 C18 179.3(2) . . . . ? C15 C16 C17 C18 -0.4(4) . . . . ? C16 C17 C18 C13 1.0(4) . . . . ? C17 C18 C13 C14 -0.4(4) . . . . ? C17 C18 C13 N1 179.1(2) . . . . ? C12 N1 C13 C18 49.2(3) . . . . ? Re1 N1 C13 C18 -129.0(2) . . . . ? C12 N1 C13 C14 -131.3(2) . . . . ? Re1 N1 C13 C14 50.5(3) . . . . ? C18 C13 C14 C15 -0.9(3) . . . . ? N1 C13 C14 C15 179.5(2) . . . . ? C13 C14 C15 C16 1.6(3) . . . . ? O5 C16 C15 C14 179.3(2) . . . . ? C17 C16 C15 C14 -1.0(4) . . . . ? C2 Re1 C1 O1 -55(3) . . . . ? C3 Re1 C1 O1 35(3) . . . . ? N1 Re1 C1 O1 -153(3) . . . . ? N2 Re1 C1 O1 133(3) . . . . ? Cl1 Re1 C1 O1 47(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.831 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.083 # Attachment '- complex7.cif' data_1105 _database_code_depnum_ccdc_archive 'CCDC 775542' #TrackingRef '- complex7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H36 N2 O4 Pt' _chemical_formula_weight 683.70 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 23.3474(5) _cell_length_b 9.2838(2) _cell_length_c 26.4446(5) _cell_angle_alpha 90.00 _cell_angle_beta 107.1440(10) _cell_angle_gamma 90.00 _cell_volume 5477.2(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.658 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2720 _exptl_absorpt_coefficient_mu 5.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4405 _exptl_absorpt_correction_T_max 0.6264 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _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 62851 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.14 _reflns_number_total 6647 _reflns_number_gt 5488 _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. ; _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^)+(0.0224P)^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 6647 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0288 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0458 _refine_ls_wR_factor_gt 0.0441 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.232075(4) 0.415088(10) 0.133367(4) 0.01664(3) Uani 1 1 d . . . O2 O 0.19659(8) 0.26905(17) 0.07888(6) 0.0180(4) Uani 1 1 d . . . N2 N 0.17738(10) 0.5799(2) 0.10545(8) 0.0204(4) Uani 1 1 d . . . N1 N 0.26394(10) 0.5625(2) 0.18935(8) 0.0198(5) Uani 1 1 d . . . C20 C 0.31284(12) 0.5796(3) 0.28549(10) 0.0231(5) Uani 1 1 d . . . H20A H 0.2791 0.6292 0.2899 0.028 Uiso 1 1 calc R . . O1 O 0.28762(7) 0.25545(19) 0.16332(6) 0.0192(4) Uani 1 1 d . . . O3 O 0.01045(9) 0.5885(2) -0.09496(8) 0.0344(5) Uani 1 1 d . . . C4 C 0.24722(12) -0.0952(3) 0.06435(10) 0.0210(5) Uani 1 1 d . . . H4A H 0.2380 -0.1765 0.0416 0.025 Uiso 1 1 calc R . . C23 C 0.18532(13) 0.6935(3) 0.13624(11) 0.0248(6) Uani 1 1 d . . . H23A H 0.1607 0.7767 0.1274 0.030 Uiso 1 1 calc R . . O4 O 0.45421(10) 0.4421(2) 0.36827(8) 0.0382(5) Uani 1 1 d . . . C11 C 0.15964(12) 0.0388(3) -0.00072(10) 0.0191(5) Uani 1 1 d . . . C24 C 0.13256(12) 0.5839(3) 0.05527(10) 0.0205(5) Uani 1 1 d . . . C12 C 0.10090(12) 0.0647(3) 0.01310(11) 0.0281(6) Uani 1 1 d . . . H12A H 0.1045 0.1530 0.0341 0.042 Uiso 1 1 calc R . . H12B H 0.0931 -0.0171 0.0336 0.042 Uiso 1 1 calc R . . H12C H 0.0677 0.0747 -0.0196 0.042 Uiso 1 1 calc R . . C6 C 0.22788(11) 0.1435(3) 0.08650(10) 0.0165(5) Uani 1 1 d . . . C7 C 0.36929(12) 0.0050(3) 0.19381(10) 0.0221(6) Uani 1 1 d . . . C27 C 0.04859(13) 0.5921(3) -0.04447(11) 0.0252(6) Uani 1 1 d . . . C1 C 0.27720(11) 0.1356(3) 0.13248(10) 0.0173(5) Uani 1 1 d . . . C2 C 0.31315(11) 0.0104(3) 0.14556(10) 0.0190(5) Uani 1 1 d . . . C19 C 0.31397(12) 0.5383(3) 0.23489(10) 0.0200(5) Uani 1 1 d . . . C3 C 0.29582(12) -0.1044(3) 0.11026(10) 0.0216(6) Uani 1 1 d . . . H3A H 0.3178 -0.1918 0.1177 0.026 Uiso 1 1 calc R . . C5 C 0.21182(11) 0.0273(3) 0.05050(10) 0.0178(5) Uani 1 1 d . . . C17 C 0.41252(13) 0.4389(3) 0.27215(11) 0.0276(6) Uani 1 1 d . . . H17A H 0.4471 0.3932 0.2676 0.033 Uiso 1 1 calc R . . C14 C 0.15263(14) -0.0998(3) -0.03382(11) 0.0286(6) Uani 1 1 d . . . H14A H 0.1896 -0.1180 -0.0431 0.043 Uiso 1 1 calc R . . H14B H 0.1192 -0.0887 -0.0662 0.043 Uiso 1 1 calc R . . H14C H 0.1446 -0.1811 -0.0132 0.043 Uiso 1 1 calc R . . C16 C 0.41031(13) 0.4752(3) 0.32251(11) 0.0271(6) Uani 1 1 d . . . C9 C 0.41489(12) 0.1170(3) 0.18639(11) 0.0265(6) Uani 1 1 d . . . H9A H 0.3967 0.2131 0.1825 0.040 Uiso 1 1 calc R . . H9B H 0.4264 0.0934 0.1546 0.040 Uiso 1 1 calc R . . H9C H 0.4505 0.1156 0.2173 0.040 Uiso 1 1 calc R . . C29 C 0.14485(12) 0.5182(3) 0.01187(10) 0.0222(6) Uani 1 1 d . . . H29A H 0.1821 0.4707 0.0164 0.027 Uiso 1 1 calc R . . C13 C 0.17185(12) 0.1619(3) -0.03497(10) 0.0233(6) Uani 1 1 d . . . H13A H 0.1768 0.2524 -0.0150 0.035 Uiso 1 1 calc R . . H13B H 0.1380 0.1708 -0.0672 0.035 Uiso 1 1 calc R . . H13C H 0.2085 0.1412 -0.0445 0.035 Uiso 1 1 calc R . . C8 C 0.35372(13) 0.0368(3) 0.24524(11) 0.0300(7) Uani 1 1 d . . . H8A H 0.3341 0.1310 0.2425 0.045 Uiso 1 1 calc R . . H8B H 0.3905 0.0376 0.2750 0.045 Uiso 1 1 calc R . . H8C H 0.3266 -0.0379 0.2510 0.045 Uiso 1 1 calc R . . C18 C 0.36424(12) 0.4695(3) 0.22872(11) 0.0247(6) Uani 1 1 d . . . H18A H 0.3655 0.4432 0.1943 0.030 Uiso 1 1 calc R . . C21 C 0.36087(13) 0.5482(3) 0.32888(11) 0.0258(6) Uani 1 1 d . . . H21A H 0.3602 0.5764 0.3632 0.031 Uiso 1 1 calc R . . C25 C 0.07784(13) 0.6523(3) 0.04813(11) 0.0257(6) Uani 1 1 d . . . H25A H 0.0691 0.6965 0.0774 0.031 Uiso 1 1 calc R . . C22 C 0.23327(13) 0.6833(3) 0.18368(11) 0.0250(6) Uani 1 1 d . . . H22A H 0.2425 0.7579 0.2094 0.030 Uiso 1 1 calc R . . C10 C 0.40029(13) -0.1434(3) 0.19997(12) 0.0322(7) Uani 1 1 d . . . H10A H 0.3726 -0.2175 0.2050 0.048 Uiso 1 1 calc R . . H10B H 0.4361 -0.1418 0.2308 0.048 Uiso 1 1 calc R . . H10C H 0.4119 -0.1651 0.1681 0.048 Uiso 1 1 calc R . . C15 C 0.50248(16) 0.3547(5) 0.36308(15) 0.0606(12) Uani 1 1 d . . . H15A H 0.5312 0.3391 0.3981 0.091 Uiso 1 1 calc R . . H15B H 0.5226 0.4034 0.3401 0.091 Uiso 1 1 calc R . . H15C H 0.4868 0.2618 0.3475 0.091 Uiso 1 1 calc R . . C26 C 0.03561(13) 0.6567(3) -0.00164(12) 0.0280(6) Uani 1 1 d . . . H26A H -0.0018 0.7035 -0.0063 0.034 Uiso 1 1 calc R . . C28 C 0.10334(13) 0.5221(3) -0.03704(11) 0.0249(6) Uani 1 1 d . . . H28A H 0.1119 0.4768 -0.0662 0.030 Uiso 1 1 calc R . . C30 C -0.04143(14) 0.6782(3) -0.10683(13) 0.0396(8) Uani 1 1 d . . . H30A H -0.0648 0.6651 -0.1440 0.059 Uiso 1 1 calc R . . H30B H -0.0291 0.7792 -0.1007 0.059 Uiso 1 1 calc R . . H30C H -0.0661 0.6519 -0.0840 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.02071(5) 0.01356(5) 0.01681(5) -0.00051(4) 0.00734(4) 0.00082(4) O2 0.0212(9) 0.0144(8) 0.0174(8) -0.0007(7) 0.0042(7) 0.0023(7) N2 0.0239(11) 0.0172(10) 0.0225(11) 0.0002(9) 0.0107(9) -0.0008(9) N1 0.0250(12) 0.0179(11) 0.0191(11) -0.0008(8) 0.0105(9) -0.0026(9) C20 0.0238(13) 0.0227(13) 0.0251(13) -0.0057(11) 0.0108(11) -0.0030(12) O1 0.0213(9) 0.0153(8) 0.0200(9) -0.0017(7) 0.0047(7) 0.0018(7) O3 0.0317(11) 0.0377(12) 0.0285(11) -0.0006(9) 0.0006(9) 0.0094(10) C4 0.0251(14) 0.0161(12) 0.0229(13) -0.0023(10) 0.0087(11) -0.0006(11) C23 0.0312(16) 0.0177(12) 0.0282(14) 0.0000(11) 0.0130(12) 0.0059(11) O4 0.0301(11) 0.0528(14) 0.0271(11) -0.0104(10) 0.0012(9) 0.0091(10) C11 0.0205(13) 0.0174(12) 0.0186(13) -0.0021(10) 0.0045(11) -0.0005(10) C24 0.0236(13) 0.0158(11) 0.0231(13) 0.0024(11) 0.0083(11) 0.0016(11) C12 0.0213(14) 0.0370(17) 0.0253(14) -0.0016(12) 0.0057(12) -0.0013(12) C6 0.0186(13) 0.0132(11) 0.0191(12) 0.0023(10) 0.0079(10) 0.0014(10) C7 0.0193(14) 0.0219(13) 0.0239(14) 0.0030(11) 0.0044(11) 0.0037(11) C27 0.0274(14) 0.0203(13) 0.0268(14) 0.0046(12) 0.0062(12) -0.0002(12) C1 0.0189(13) 0.0162(11) 0.0189(12) -0.0009(10) 0.0088(10) -0.0017(10) C2 0.0184(13) 0.0192(13) 0.0208(13) 0.0026(10) 0.0080(11) -0.0016(10) C19 0.0232(14) 0.0157(12) 0.0217(13) -0.0028(10) 0.0078(11) -0.0042(10) C3 0.0209(13) 0.0181(13) 0.0265(14) 0.0021(10) 0.0080(11) 0.0052(10) C5 0.0180(13) 0.0163(11) 0.0208(13) -0.0007(10) 0.0085(11) -0.0012(10) C17 0.0233(14) 0.0308(16) 0.0310(15) -0.0103(12) 0.0115(12) 0.0006(12) C14 0.0341(16) 0.0218(14) 0.0251(14) -0.0044(11) 0.0014(12) -0.0017(12) C16 0.0256(15) 0.0281(14) 0.0260(15) -0.0069(12) 0.0049(12) -0.0038(12) C9 0.0194(14) 0.0294(15) 0.0292(15) -0.0021(11) 0.0048(12) -0.0017(11) C29 0.0248(14) 0.0177(12) 0.0253(14) 0.0019(11) 0.0092(12) 0.0035(11) C13 0.0278(15) 0.0210(13) 0.0203(13) 0.0012(11) 0.0057(11) 0.0010(11) C8 0.0271(16) 0.0398(17) 0.0222(14) 0.0044(12) 0.0055(12) 0.0040(13) C18 0.0271(15) 0.0258(13) 0.0237(14) -0.0082(11) 0.0116(12) -0.0039(12) C21 0.0286(15) 0.0295(15) 0.0217(14) -0.0079(11) 0.0111(12) -0.0029(12) C25 0.0291(15) 0.0229(14) 0.0279(15) -0.0003(12) 0.0128(12) 0.0040(12) C22 0.0352(16) 0.0186(13) 0.0238(14) -0.0033(11) 0.0130(13) 0.0000(12) C10 0.0283(16) 0.0252(14) 0.0384(17) 0.0038(13) 0.0026(14) 0.0060(13) C15 0.036(2) 0.097(3) 0.040(2) -0.016(2) -0.0021(17) 0.029(2) C26 0.0239(15) 0.0251(14) 0.0358(16) 0.0029(13) 0.0099(13) 0.0065(12) C28 0.0307(16) 0.0201(13) 0.0252(14) 0.0002(11) 0.0103(12) 0.0013(12) C30 0.0336(18) 0.0389(18) 0.0389(18) 0.0060(15) -0.0010(15) 0.0078(15) _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 O2 1.9741(16) . ? Pt1 O1 1.9748(17) . ? Pt1 N2 1.990(2) . ? Pt1 N1 1.992(2) . ? O2 C6 1.359(3) . ? N2 C23 1.311(3) . ? N2 C24 1.428(3) . ? N1 C22 1.315(3) . ? N1 C19 1.427(3) . ? C20 C21 1.378(4) . ? C20 C19 1.400(3) . ? C20 H20A 0.9500 . ? O1 C1 1.359(3) . ? O3 C27 1.369(3) . ? O3 C30 1.426(3) . ? C4 C5 1.390(3) . ? C4 C3 1.399(4) . ? C4 H4A 0.9500 . ? C23 C22 1.417(4) . ? C23 H23A 0.9500 . ? O4 C16 1.371(3) . ? O4 C15 1.428(4) . ? C11 C5 1.535(4) . ? C11 C13 1.537(4) . ? C11 C14 1.537(3) . ? C11 C12 1.539(4) . ? C24 C25 1.389(4) . ? C24 C29 1.402(4) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C6 C1 1.409(3) . ? C6 C5 1.415(3) . ? C7 C8 1.536(4) . ? C7 C2 1.537(4) . ? C7 C9 1.541(4) . ? C7 C10 1.542(4) . ? C27 C26 1.392(4) . ? C27 C28 1.395(4) . ? C1 C2 1.415(3) . ? C2 C3 1.396(3) . ? C19 C18 1.387(4) . ? C3 H3A 0.9500 . ? C17 C18 1.381(4) . ? C17 C16 1.389(4) . ? C17 H17A 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C16 C21 1.391(4) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C29 C28 1.369(4) . ? C29 H29A 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C18 H18A 0.9500 . ? C21 H21A 0.9500 . ? C25 C26 1.393(4) . ? C25 H25A 0.9500 . ? C22 H22A 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C26 H26A 0.9500 . ? C28 H28A 0.9500 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 O2 Pt1 O1 82.07(7) . . ? O2 Pt1 N2 99.90(8) . . ? O1 Pt1 N2 178.01(8) . . ? O2 Pt1 N1 177.04(8) . . ? O1 Pt1 N1 99.23(8) . . ? N2 Pt1 N1 78.80(9) . . ? C6 O2 Pt1 112.91(14) . . ? C23 N2 C24 119.1(2) . . ? C23 N2 Pt1 115.46(18) . . ? C24 N2 Pt1 125.40(16) . . ? C22 N1 C19 120.9(2) . . ? C22 N1 Pt1 115.43(18) . . ? C19 N1 Pt1 123.53(16) . . ? C21 C20 C19 119.9(3) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C1 O1 Pt1 113.19(14) . . ? C27 O3 C30 117.8(2) . . ? C5 C4 C3 123.1(2) . . ? C5 C4 H4A 118.5 . . ? C3 C4 H4A 118.5 . . ? N2 C23 C22 115.2(2) . . ? N2 C23 H23A 122.4 . . ? C22 C23 H23A 122.4 . . ? C16 O4 C15 116.7(2) . . ? C5 C11 C13 109.6(2) . . ? C5 C11 C14 111.6(2) . . ? C13 C11 C14 107.1(2) . . ? C5 C11 C12 109.4(2) . . ? C13 C11 C12 110.9(2) . . ? C14 C11 C12 108.3(2) . . ? C25 C24 C29 119.3(2) . . ? C25 C24 N2 122.1(2) . . ? C29 C24 N2 118.6(2) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C6 C1 116.1(2) . . ? O2 C6 C5 122.0(2) . . ? C1 C6 C5 121.9(2) . . ? C8 C7 C2 111.2(2) . . ? C8 C7 C9 109.6(2) . . ? C2 C7 C9 108.9(2) . . ? C8 C7 C10 107.7(2) . . ? C2 C7 C10 112.1(2) . . ? C9 C7 C10 107.2(2) . . ? O3 C27 C26 124.7(3) . . ? O3 C27 C28 115.6(2) . . ? C26 C27 C28 119.8(3) . . ? O1 C1 C6 115.6(2) . . ? O1 C1 C2 122.5(2) . . ? C6 C1 C2 121.9(2) . . ? C3 C2 C1 115.4(2) . . ? C3 C2 C7 122.6(2) . . ? C1 C2 C7 121.9(2) . . ? C18 C19 C20 119.6(3) . . ? C18 C19 N1 118.9(2) . . ? C20 C19 N1 121.5(2) . . ? C2 C3 C4 122.4(2) . . ? C2 C3 H3A 118.8 . . ? C4 C3 H3A 118.8 . . ? C4 C5 C6 115.3(2) . . ? C4 C5 C11 123.0(2) . . ? C6 C5 C11 121.6(2) . . ? C18 C17 C16 119.7(3) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C16 C17 124.2(3) . . ? O4 C16 C21 115.7(2) . . ? C17 C16 C21 120.1(3) . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C28 C29 C24 120.2(3) . . ? C28 C29 H29A 119.9 . . ? C24 C29 H29A 119.9 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18A 119.7 . . ? C19 C18 H18A 119.7 . . ? C20 C21 C16 120.2(3) . . ? C20 C21 H21A 119.9 . . ? C16 C21 H21A 119.9 . . ? C24 C25 C26 120.6(3) . . ? C24 C25 H25A 119.7 . . ? C26 C25 H25A 119.7 . . ? N1 C22 C23 114.8(2) . . ? N1 C22 H22A 122.6 . . ? C23 C22 H22A 122.6 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C15 H15A 109.5 . . ? O4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C27 C26 C25 119.5(3) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? O3 C30 H30A 109.5 . . ? O3 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pt1 O2 C6 -3.73(15) . . . . ? N2 Pt1 O2 C6 176.55(16) . . . . ? N1 Pt1 O2 C6 -119.8(14) . . . . ? O2 Pt1 N2 C23 173.39(19) . . . . ? O1 Pt1 N2 C23 1(2) . . . . ? N1 Pt1 N2 C23 -3.90(19) . . . . ? O2 Pt1 N2 C24 -8.2(2) . . . . ? O1 Pt1 N2 C24 180(100) . . . . ? N1 Pt1 N2 C24 174.5(2) . . . . ? O2 Pt1 N1 C22 -59.3(15) . . . . ? O1 Pt1 N1 C22 -174.96(18) . . . . ? N2 Pt1 N1 C22 4.86(19) . . . . ? O2 Pt1 N1 C19 116.4(14) . . . . ? O1 Pt1 N1 C19 0.8(2) . . . . ? N2 Pt1 N1 C19 -179.4(2) . . . . ? O2 Pt1 O1 C1 3.46(16) . . . . ? N2 Pt1 O1 C1 176(7) . . . . ? N1 Pt1 O1 C1 -179.23(16) . . . . ? C24 N2 C23 C22 -176.1(2) . . . . ? Pt1 N2 C23 C22 2.4(3) . . . . ? C23 N2 C24 C25 -37.7(4) . . . . ? Pt1 N2 C24 C25 143.9(2) . . . . ? C23 N2 C24 C29 141.4(3) . . . . ? Pt1 N2 C24 C29 -36.9(3) . . . . ? Pt1 O2 C6 C1 3.4(3) . . . . ? Pt1 O2 C6 C5 -176.77(19) . . . . ? C30 O3 C27 C26 11.8(4) . . . . ? C30 O3 C27 C28 -169.6(3) . . . . ? Pt1 O1 C1 C6 -2.6(3) . . . . ? Pt1 O1 C1 C2 177.65(18) . . . . ? O2 C6 C1 O1 -0.5(3) . . . . ? C5 C6 C1 O1 179.6(2) . . . . ? O2 C6 C1 C2 179.2(2) . . . . ? C5 C6 C1 C2 -0.6(4) . . . . ? O1 C1 C2 C3 178.8(2) . . . . ? C6 C1 C2 C3 -0.9(4) . . . . ? O1 C1 C2 C7 -4.2(4) . . . . ? C6 C1 C2 C7 176.1(2) . . . . ? C8 C7 C2 C3 -124.6(3) . . . . ? C9 C7 C2 C3 114.5(3) . . . . ? C10 C7 C2 C3 -3.9(4) . . . . ? C8 C7 C2 C1 58.7(3) . . . . ? C9 C7 C2 C1 -62.2(3) . . . . ? C10 C7 C2 C1 179.3(2) . . . . ? C21 C20 C19 C18 -1.8(4) . . . . ? C21 C20 C19 N1 176.9(2) . . . . ? C22 N1 C19 C18 -140.8(3) . . . . ? Pt1 N1 C19 C18 43.7(3) . . . . ? C22 N1 C19 C20 40.6(4) . . . . ? Pt1 N1 C19 C20 -134.9(2) . . . . ? C1 C2 C3 C4 1.6(4) . . . . ? C7 C2 C3 C4 -175.3(2) . . . . ? C5 C4 C3 C2 -1.0(4) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C3 C4 C5 C11 178.1(2) . . . . ? O2 C6 C5 C4 -178.5(2) . . . . ? C1 C6 C5 C4 1.3(4) . . . . ? O2 C6 C5 C11 2.8(4) . . . . ? C1 C6 C5 C11 -177.4(2) . . . . ? C13 C11 C5 C4 -119.0(3) . . . . ? C14 C11 C5 C4 -0.5(4) . . . . ? C12 C11 C5 C4 119.3(3) . . . . ? C13 C11 C5 C6 59.7(3) . . . . ? C14 C11 C5 C6 178.1(2) . . . . ? C12 C11 C5 C6 -62.1(3) . . . . ? C15 O4 C16 C17 -5.2(5) . . . . ? C15 O4 C16 C21 173.9(3) . . . . ? C18 C17 C16 O4 176.0(3) . . . . ? C18 C17 C16 C21 -3.0(4) . . . . ? C25 C24 C29 C28 0.3(4) . . . . ? N2 C24 C29 C28 -178.8(2) . . . . ? C16 C17 C18 C19 1.0(4) . . . . ? C20 C19 C18 C17 1.3(4) . . . . ? N1 C19 C18 C17 -177.3(2) . . . . ? C19 C20 C21 C16 -0.2(4) . . . . ? O4 C16 C21 C20 -176.5(2) . . . . ? C17 C16 C21 C20 2.6(4) . . . . ? C29 C24 C25 C26 -0.5(4) . . . . ? N2 C24 C25 C26 178.7(2) . . . . ? C19 N1 C22 C23 179.1(2) . . . . ? Pt1 N1 C22 C23 -5.0(3) . . . . ? N2 C23 C22 N1 1.7(4) . . . . ? O3 C27 C26 C25 179.4(3) . . . . ? C28 C27 C26 C25 0.8(4) . . . . ? C24 C25 C26 C27 -0.1(4) . . . . ? C24 C29 C28 C27 0.4(4) . . . . ? O3 C27 C28 C29 -179.7(2) . . . . ? C26 C27 C28 C29 -0.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 28.14 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.248 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.101