# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Wai-Yeung Wong' _publ_contact_author_email RWYWONG@HKBU.EDU.HK _publ_section_title ; Duplicating "sunlight" from simple WOLEDs for lighting application ; loop_ _publ_author_name 'Wai-Yeung Wong.' 'Cheuk-Lam Ho.' 'Dongge Ma.' 'Lixiang Wang.' 'Qi Wang.' ; Guijiang Zhou ; # Attachment 'WY1677WM_Pt-O.CIF' data_wy1677wm _database_code_depnum_ccdc_archive 'CCDC 716163' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H19 N O3 Pt' _chemical_formula_weight 540.47 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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.255(3) _cell_length_b 12.558(3) _cell_length_c 24.929(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3836.4(15) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.871 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 7.336 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3037 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19650 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 28.27 _reflns_number_total 4489 _reflns_number_gt 3547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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^)+(0.0563P)^2^+7.4714P] 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 4489 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1147 _refine_ls_wR_factor_gt 0.1039 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 C1 C 0.6396(5) 0.0201(5) 0.5464(2) 0.0418(13) Uani 1 1 d . . . H1A H 0.5997 0.0716 0.5647 0.050 Uiso 1 1 calc R . . C2 C 0.6904(5) -0.0595(5) 0.5756(3) 0.0472(15) Uani 1 1 d . . . H2A H 0.6865 -0.0612 0.6128 0.057 Uiso 1 1 calc R . . C3 C 0.7472(6) -0.1369(6) 0.5472(4) 0.057(2) Uani 1 1 d . . . H3A H 0.7815 -0.1918 0.5657 0.069 Uiso 1 1 calc R . . C4 C 0.7534(5) -0.1334(5) 0.4924(3) 0.0481(16) Uani 1 1 d . . . H4A H 0.7920 -0.1856 0.4739 0.058 Uiso 1 1 calc R . . C5 C 0.7018(4) -0.0517(4) 0.4643(3) 0.0373(12) Uani 1 1 d . . . C6 C 0.7006(4) -0.0353(4) 0.4065(2) 0.0377(12) Uani 1 1 d . . . C7 C 0.7529(5) -0.1008(5) 0.3690(3) 0.0472(16) Uani 1 1 d . . . H7A H 0.7887 -0.1620 0.3804 0.057 Uiso 1 1 calc R . . C8 C 0.7516(6) -0.0747(6) 0.3149(3) 0.0545(17) Uani 1 1 d . . . H8A H 0.7866 -0.1180 0.2899 0.065 Uiso 1 1 calc R . . C9 C 0.6967(6) 0.0178(5) 0.2982(3) 0.0495(15) Uani 1 1 d . . . C10 C 0.6446(5) 0.0839(5) 0.3353(2) 0.0439(13) Uani 1 1 d . . . H10A H 0.6096 0.1454 0.3236 0.053 Uiso 1 1 calc R . . C11 C 0.6449(5) 0.0581(4) 0.3898(2) 0.0358(12) Uani 1 1 d . . . C12 C 0.6406(8) 0.1259(6) 0.2241(3) 0.0580(19) Uani 1 1 d . . . C13 C 0.6973(7) 0.2105(7) 0.2024(3) 0.064(2) Uani 1 1 d . . . H13A H 0.7731 0.2104 0.2017 0.077 Uiso 1 1 calc R . . C14 C 0.6392(9) 0.2953(8) 0.1815(3) 0.076(2) Uani 1 1 d . . . H14A H 0.6769 0.3524 0.1666 0.091 Uiso 1 1 calc R . . C15 C 0.5292(9) 0.2973(8) 0.1821(3) 0.077(3) Uani 1 1 d . . . H15A H 0.4919 0.3556 0.1682 0.093 Uiso 1 1 calc R . . C16 C 0.4718(8) 0.2118(9) 0.2036(3) 0.074(2) Uani 1 1 d . . . H16A H 0.3959 0.2130 0.2042 0.089 Uiso 1 1 calc R . . C17 C 0.5271(9) 0.1256(7) 0.2239(3) 0.071(2) Uani 1 1 d . . . H17A H 0.4889 0.0675 0.2373 0.085 Uiso 1 1 calc R . . C18 C 0.4237(7) 0.3547(6) 0.5632(4) 0.057(2) Uani 1 1 d . . . H18A H 0.4457 0.3087 0.5920 0.085 Uiso 1 1 calc R . . H18B H 0.3457 0.3613 0.5631 0.085 Uiso 1 1 calc R . . H18C H 0.4559 0.4237 0.5681 0.085 Uiso 1 1 calc R . . C19 C 0.4611(5) 0.3086(4) 0.5107(2) 0.0357(12) Uani 1 1 d . . . C20 C 0.4375(5) 0.3635(5) 0.4626(3) 0.0427(14) Uani 1 1 d . . . H20A H 0.4001 0.4276 0.4661 0.051 Uiso 1 1 calc R . . C21 C 0.4643(5) 0.3320(5) 0.4101(2) 0.0391(13) Uani 1 1 d . . . C22 C 0.4342(6) 0.4035(6) 0.3635(3) 0.0558(18) Uani 1 1 d . . . H22A H 0.4577 0.3713 0.3305 0.084 Uiso 1 1 calc R . . H22B H 0.4691 0.4714 0.3677 0.084 Uiso 1 1 calc R . . H22C H 0.3565 0.4131 0.3627 0.084 Uiso 1 1 calc R . . N1 N 0.6458(4) 0.0260(3) 0.49314(18) 0.0343(10) Uani 1 1 d . . . O1 O 0.5122(3) 0.2207(3) 0.51421(15) 0.0385(9) Uani 1 1 d . . . O2 O 0.5158(3) 0.2469(3) 0.39682(14) 0.0388(9) Uani 1 1 d . . . O3 O 0.6995(5) 0.0388(5) 0.24306(19) 0.0727(16) Uani 1 1 d . . . Pt1 Pt 0.577563(17) 0.140054(16) 0.448183(8) 0.03079(11) 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 C1 0.044(3) 0.040(3) 0.041(3) 0.005(2) -0.002(2) -0.001(3) C2 0.049(4) 0.048(4) 0.045(3) 0.009(3) -0.004(3) -0.003(3) C3 0.034(4) 0.036(4) 0.101(7) 0.013(3) -0.011(3) 0.003(3) C4 0.042(4) 0.043(3) 0.059(4) 0.001(3) -0.003(3) 0.006(3) C5 0.027(3) 0.027(3) 0.058(3) -0.001(2) -0.003(2) -0.001(2) C6 0.033(3) 0.032(3) 0.048(3) -0.012(2) 0.000(2) 0.000(2) C7 0.045(4) 0.034(3) 0.063(4) -0.013(3) -0.005(3) 0.009(3) C8 0.055(4) 0.045(4) 0.063(4) -0.021(3) 0.007(3) 0.008(3) C9 0.058(4) 0.047(4) 0.044(3) -0.009(3) 0.007(3) 0.001(3) C10 0.052(4) 0.034(3) 0.045(3) -0.007(3) 0.003(3) 0.006(3) C11 0.036(3) 0.028(3) 0.044(3) -0.007(2) -0.001(2) 0.000(2) C12 0.083(6) 0.055(4) 0.036(3) -0.014(3) 0.000(3) 0.013(4) C13 0.068(5) 0.072(5) 0.054(4) -0.004(4) -0.004(4) -0.003(4) C14 0.094(7) 0.069(6) 0.064(5) 0.005(4) -0.010(4) -0.009(5) C15 0.097(7) 0.089(7) 0.046(4) 0.000(4) -0.012(4) 0.020(6) C16 0.069(5) 0.101(7) 0.052(4) -0.008(5) -0.003(4) 0.008(5) C17 0.094(7) 0.068(5) 0.051(5) -0.006(4) 0.013(4) -0.002(5) C18 0.070(6) 0.050(5) 0.052(4) -0.005(3) 0.015(3) 0.018(3) C19 0.034(3) 0.031(3) 0.042(3) -0.003(2) 0.007(2) 0.004(2) C20 0.047(4) 0.030(3) 0.051(4) 0.002(3) 0.004(3) 0.008(2) C21 0.039(3) 0.034(3) 0.045(3) 0.002(2) 0.000(3) 0.001(2) C22 0.063(5) 0.047(4) 0.058(4) 0.008(3) -0.002(3) 0.013(3) N1 0.033(2) 0.029(2) 0.041(3) -0.0018(19) 0.0014(19) -0.0030(18) O1 0.040(2) 0.035(2) 0.040(2) -0.0004(16) 0.0059(17) 0.0034(16) O2 0.047(2) 0.035(2) 0.035(2) -0.0007(16) -0.0005(17) 0.0067(18) O3 0.101(4) 0.072(4) 0.046(3) -0.013(2) 0.013(3) 0.023(3) Pt1 0.03201(16) 0.02325(15) 0.03712(16) -0.00169(8) 0.00123(8) 0.00041(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.331(7) . ? C1 C2 1.385(8) . ? C1 H1A 0.9300 . ? C2 C3 1.389(10) . ? C2 H2A 0.9300 . ? C3 C4 1.369(10) . ? C3 H3A 0.9300 . ? C4 C5 1.394(8) . ? C4 H4A 0.9300 . ? C5 N1 1.393(7) . ? C5 C6 1.455(8) . ? C6 C7 1.400(8) . ? C6 C11 1.421(8) . ? C7 C8 1.389(10) . ? C7 H7A 0.9300 . ? C8 C9 1.405(10) . ? C8 H8A 0.9300 . ? C9 C10 1.397(8) . ? C9 O3 1.400(8) . ? C10 C11 1.396(8) . ? C10 H10A 0.9300 . ? C11 Pt1 1.965(5) . ? C12 C13 1.380(11) . ? C12 C17 1.391(15) . ? C12 O3 1.393(9) . ? C13 C14 1.383(13) . ? C13 H13A 0.9300 . ? C14 C15 1.348(15) . ? C14 H14A 0.9300 . ? C15 C16 1.391(14) . ? C15 H15A 0.9300 . ? C16 C17 1.374(12) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C19 1.503(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 O1 1.273(6) . ? C19 C20 1.413(9) . ? C20 C21 1.408(9) . ? C20 H20A 0.9300 . ? C21 O2 1.284(7) . ? C21 C22 1.513(9) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? N1 Pt1 2.001(4) . ? O1 Pt1 2.092(4) . ? O2 Pt1 2.003(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 C1 C2 122.6(6) . . ? N1 C1 H1A 118.7 . . ? C2 C1 H1A 118.7 . . ? C1 C2 C3 117.6(6) . . ? C1 C2 H2A 121.2 . . ? C3 C2 H2A 121.2 . . ? C4 C3 C2 120.9(6) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? N1 C5 C4 118.7(6) . . ? N1 C5 C6 114.0(5) . . ? C4 C5 C6 127.3(6) . . ? C7 C6 C11 120.5(6) . . ? C7 C6 C5 125.0(5) . . ? C11 C6 C5 114.4(5) . . ? C8 C7 C6 120.3(6) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C7 C8 C9 119.2(6) . . ? C7 C8 H8A 120.4 . . ? C9 C8 H8A 120.4 . . ? C10 C9 O3 123.3(6) . . ? C10 C9 C8 120.9(6) . . ? O3 C9 C8 115.7(6) . . ? C11 C10 C9 120.4(6) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C6 118.6(5) . . ? C10 C11 Pt1 126.8(4) . . ? C6 C11 Pt1 114.6(4) . . ? C13 C12 C17 120.2(7) . . ? C13 C12 O3 118.5(8) . . ? C17 C12 O3 121.2(7) . . ? C12 C13 C14 118.8(8) . . ? C12 C13 H13A 120.6 . . ? C14 C13 H13A 120.6 . . ? C15 C14 C13 121.7(9) . . ? C15 C14 H14A 119.2 . . ? C13 C14 H14A 119.2 . . ? C14 C15 C16 119.7(9) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 120.0(9) . . ? C17 C16 H16A 120.0 . . ? C15 C16 H16A 120.0 . . ? C16 C17 C12 119.6(8) . . ? C16 C17 H17A 120.2 . . ? C12 C17 H17A 120.2 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 C20 125.6(5) . . ? O1 C19 C18 115.1(5) . . ? C20 C19 C18 119.3(6) . . ? C21 C20 C19 127.2(5) . . ? C21 C20 H20A 116.4 . . ? C19 C20 H20A 116.4 . . ? O2 C21 C20 126.0(5) . . ? O2 C21 C22 114.6(5) . . ? C20 C21 C22 119.3(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C1 N1 C5 120.2(5) . . ? C1 N1 Pt1 125.1(4) . . ? C5 N1 Pt1 114.8(4) . . ? C19 O1 Pt1 123.7(4) . . ? C21 O2 Pt1 125.4(4) . . ? C12 O3 C9 117.9(5) . . ? C11 Pt1 N1 82.2(2) . . ? C11 Pt1 O2 92.0(2) . . ? N1 Pt1 O2 174.28(17) . . ? C11 Pt1 O1 175.9(2) . . ? N1 Pt1 O1 93.77(16) . . ? O2 Pt1 O1 91.94(15) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 2.322 _refine_diff_density_min -1.615 _refine_diff_density_rms 0.177 # Attachment 'WY1695WC_Pt-Ge.CIF' data_wy1695wc _database_code_depnum_ccdc_archive 'CCDC 716164' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H29 Ge N O2 Pt' _chemical_formula_weight 751.26 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' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.798(2) _cell_length_b 13.3210(17) _cell_length_c 11.9372(15) _cell_angle_alpha 90.00 _cell_angle_beta 107.209(2) _cell_angle_gamma 90.00 _cell_volume 2855.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 5.978 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7523 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Smart CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16214 _diffrn_reflns_av_R_equivalents 0.0492 _diffrn_reflns_av_sigmaI/netI 0.0721 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.25 _reflns_number_total 6485 _reflns_number_gt 4409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1998)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction SAINT _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^)+(0.0276P)^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 6485 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0711 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 C1 C 0.6384(3) 0.0230(5) 0.9358(5) 0.0481(15) Uani 1 1 d . . . H1A H 0.6598 0.0768 0.9835 0.058 Uiso 1 1 calc R . . C2 C 0.6836(4) -0.0525(5) 0.9189(6) 0.0572(17) Uani 1 1 d . . . H2A H 0.7348 -0.0497 0.9544 0.069 Uiso 1 1 calc R . . C3 C 0.6522(4) -0.1331(5) 0.8481(6) 0.0539(16) Uani 1 1 d . . . H3A H 0.6820 -0.1844 0.8340 0.065 Uiso 1 1 calc R . . C4 C 0.5754(4) -0.1360(4) 0.7984(5) 0.0470(15) Uani 1 1 d . . . H4A H 0.5533 -0.1908 0.7529 0.056 Uiso 1 1 calc R . . C5 C 0.5314(3) -0.0571(4) 0.8166(5) 0.0374(13) Uani 1 1 d . . . C6 C 0.4506(3) -0.0474(4) 0.7712(4) 0.0350(12) Uani 1 1 d . . . C7 C 0.4053(3) -0.1183(4) 0.6985(5) 0.0414(13) Uani 1 1 d . . . H7A H 0.4259 -0.1753 0.6753 0.050 Uiso 1 1 calc R . . C8 C 0.3287(4) -0.1027(4) 0.6609(5) 0.0469(15) Uani 1 1 d . . . H8A H 0.2980 -0.1497 0.6120 0.056 Uiso 1 1 calc R . . C9 C 0.2972(3) -0.0182(4) 0.6951(5) 0.0369(13) Uani 1 1 d . . . C10 C 0.3444(3) 0.0520(4) 0.7681(5) 0.0400(14) Uani 1 1 d . . . H10A H 0.3236 0.1087 0.7914 0.048 Uiso 1 1 calc R . . C11 C 0.4216(3) 0.0396(4) 0.8072(5) 0.0361(13) Uani 1 1 d . . . C12 C 0.1538(4) -0.0505(4) 0.7758(5) 0.0452(15) Uani 1 1 d . . . C13 C 0.1965(4) -0.1126(5) 0.8623(6) 0.0592(18) Uani 1 1 d . . . H13A H 0.2428 -0.1339 0.8583 0.071 Uiso 1 1 calc R . . C14 C 0.1717(5) -0.1439(6) 0.9555(6) 0.078(2) Uani 1 1 d . . . H14A H 0.2014 -0.1853 1.0133 0.093 Uiso 1 1 calc R . . C15 C 0.1039(6) -0.1139(6) 0.9620(7) 0.081(3) Uani 1 1 d . . . H15A H 0.0878 -0.1338 1.0252 0.097 Uiso 1 1 calc R . . C16 C 0.0593(5) -0.0549(6) 0.8768(8) 0.081(3) Uani 1 1 d . . . H16A H 0.0123 -0.0364 0.8803 0.098 Uiso 1 1 calc R . . C17 C 0.0842(4) -0.0226(5) 0.7846(7) 0.067(2) Uani 1 1 d . . . H17A H 0.0538 0.0187 0.7274 0.081 Uiso 1 1 calc R . . C18 C 0.1653(3) 0.1439(4) 0.6318(6) 0.0464(15) Uani 1 1 d . . . C19 C 0.1804(4) 0.2077(5) 0.7295(6) 0.0536(17) Uani 1 1 d . . . H19A H 0.2012 0.1817 0.8043 0.064 Uiso 1 1 calc R . . C20 C 0.1642(4) 0.3101(5) 0.7149(7) 0.067(2) Uani 1 1 d . . . H20A H 0.1747 0.3523 0.7797 0.080 Uiso 1 1 calc R . . C21 C 0.1324(5) 0.3484(6) 0.6035(9) 0.076(2) Uani 1 1 d . . . H21A H 0.1215 0.4165 0.5937 0.091 Uiso 1 1 calc R . . C22 C 0.1171(5) 0.2872(6) 0.5080(8) 0.075(2) Uani 1 1 d . . . H22A H 0.0962 0.3134 0.4333 0.090 Uiso 1 1 calc R . . C23 C 0.1329(4) 0.1852(5) 0.5229(6) 0.0617(19) Uani 1 1 d . . . H23A H 0.1211 0.1437 0.4574 0.074 Uiso 1 1 calc R . . C24 C 0.1433(3) -0.0656(4) 0.5016(5) 0.0456(15) Uani 1 1 d . . . C25 C 0.0760(3) -0.1167(5) 0.4790(6) 0.0533(16) Uani 1 1 d . . . H25A H 0.0523 -0.1200 0.5371 0.064 Uiso 1 1 calc R . . C26 C 0.0437(4) -0.1625(5) 0.3726(7) 0.0640(19) Uani 1 1 d . . . H26A H -0.0010 -0.1970 0.3596 0.077 Uiso 1 1 calc R . . C27 C 0.0776(4) -0.1570(6) 0.2864(6) 0.069(2) Uani 1 1 d . . . H27A H 0.0558 -0.1878 0.2145 0.083 Uiso 1 1 calc R . . C28 C 0.1438(4) -0.1062(5) 0.3049(6) 0.066(2) Uani 1 1 d . . . H28A H 0.1668 -0.1024 0.2460 0.080 Uiso 1 1 calc R . . C29 C 0.1755(4) -0.0610(5) 0.4118(5) 0.0530(16) Uani 1 1 d . . . H29A H 0.2201 -0.0263 0.4239 0.064 Uiso 1 1 calc R . . C30 C 0.6396(5) 0.3427(5) 1.1504(7) 0.073(2) Uani 1 1 d . . . H30A H 0.6824 0.3030 1.1513 0.110 Uiso 1 1 calc R . . H30B H 0.6354 0.3472 1.2284 0.110 Uiso 1 1 calc R . . H30C H 0.6450 0.4088 1.1219 0.110 Uiso 1 1 calc R . . C31 C 0.5705(4) 0.2940(5) 1.0710(5) 0.0490(16) Uani 1 1 d . . . C32 C 0.5002(4) 0.3381(5) 1.0552(6) 0.0595(19) Uani 1 1 d . . . H32A H 0.5001 0.3978 1.0953 0.071 Uiso 1 1 calc R . . C33 C 0.4324(4) 0.3049(5) 0.9890(5) 0.0505(16) Uani 1 1 d . . . C34 C 0.3637(4) 0.3656(5) 0.9836(7) 0.072(2) Uani 1 1 d . . . H34A H 0.3206 0.3322 0.9338 0.108 Uiso 1 1 calc R . . H34B H 0.3680 0.4310 0.9525 0.108 Uiso 1 1 calc R . . H34C H 0.3587 0.3721 1.0610 0.108 Uiso 1 1 calc R . . Ge1 Ge 0.19003(3) 0.00091(5) 0.65038(5) 0.04121(15) Uani 1 1 d . . . N1 N 0.5640(3) 0.0222(3) 0.8857(4) 0.0385(11) Uani 1 1 d . . . O1 O 0.5818(2) 0.2130(3) 1.0212(3) 0.0482(10) Uani 1 1 d . . . O2 O 0.4183(2) 0.2257(3) 0.9262(3) 0.0470(10) Uani 1 1 d . . . Pt1 Pt 0.495890(13) 0.127898(16) 0.910819(18) 0.03576(8) 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 C1 0.044(4) 0.050(4) 0.050(4) 0.000(3) 0.014(3) -0.003(3) C2 0.044(4) 0.060(4) 0.067(5) 0.003(4) 0.016(3) 0.011(3) C3 0.042(4) 0.057(4) 0.065(4) 0.004(3) 0.020(3) 0.016(3) C4 0.053(4) 0.042(3) 0.050(4) -0.006(3) 0.021(3) 0.004(3) C5 0.042(3) 0.042(3) 0.033(3) 0.006(2) 0.019(3) 0.006(3) C6 0.038(3) 0.038(3) 0.030(3) 0.003(2) 0.012(2) -0.001(3) C7 0.049(4) 0.034(3) 0.042(3) 0.001(3) 0.015(3) 0.007(3) C8 0.049(4) 0.049(4) 0.043(3) -0.003(3) 0.015(3) -0.007(3) C9 0.035(3) 0.041(3) 0.037(3) 0.007(2) 0.016(3) -0.001(3) C10 0.053(4) 0.035(3) 0.035(3) -0.001(2) 0.019(3) 0.003(3) C11 0.043(3) 0.037(3) 0.034(3) 0.003(2) 0.021(3) -0.001(3) C12 0.053(4) 0.034(3) 0.048(4) -0.003(3) 0.015(3) 0.000(3) C13 0.054(4) 0.067(5) 0.050(4) 0.005(3) 0.005(3) -0.014(4) C14 0.093(7) 0.083(6) 0.047(4) 0.016(4) 0.005(4) -0.023(5) C15 0.129(9) 0.064(5) 0.068(5) -0.017(4) 0.058(6) -0.045(6) C16 0.096(7) 0.067(5) 0.107(7) -0.008(5) 0.069(6) -0.012(5) C17 0.068(5) 0.059(4) 0.088(6) 0.016(4) 0.043(4) 0.014(4) C18 0.043(4) 0.047(4) 0.053(4) 0.012(3) 0.020(3) 0.003(3) C19 0.050(4) 0.060(4) 0.055(4) 0.004(3) 0.023(3) 0.004(3) C20 0.063(5) 0.053(4) 0.092(6) -0.007(4) 0.035(4) -0.003(4) C21 0.072(6) 0.048(5) 0.121(8) 0.025(5) 0.050(6) 0.013(4) C22 0.086(6) 0.062(5) 0.089(6) 0.037(4) 0.042(5) 0.027(4) C23 0.076(5) 0.060(4) 0.056(4) 0.008(3) 0.029(4) 0.014(4) C24 0.043(4) 0.043(3) 0.049(4) 0.001(3) 0.010(3) 0.003(3) C25 0.038(4) 0.058(4) 0.060(4) -0.002(3) 0.008(3) 0.001(3) C26 0.044(4) 0.058(4) 0.079(5) -0.002(4) 0.002(4) -0.001(3) C27 0.067(5) 0.081(5) 0.047(4) -0.003(4) -0.005(4) 0.008(4) C28 0.066(5) 0.086(6) 0.045(4) 0.003(4) 0.014(4) 0.010(4) C29 0.042(4) 0.068(4) 0.049(4) 0.007(3) 0.012(3) -0.004(3) C30 0.091(6) 0.061(5) 0.070(5) -0.012(4) 0.026(5) -0.020(4) C31 0.064(5) 0.043(4) 0.041(4) -0.007(3) 0.017(3) -0.013(3) C32 0.085(6) 0.049(4) 0.050(4) -0.027(3) 0.029(4) -0.008(4) C33 0.072(5) 0.045(4) 0.039(4) -0.009(3) 0.023(3) -0.001(3) C34 0.082(6) 0.068(5) 0.071(5) -0.016(4) 0.031(4) 0.020(4) Ge1 0.0395(4) 0.0429(3) 0.0419(3) 0.0032(3) 0.0132(3) -0.0004(3) N1 0.038(3) 0.044(3) 0.035(3) 0.005(2) 0.012(2) 0.000(2) O1 0.055(3) 0.041(2) 0.046(2) -0.0056(19) 0.010(2) -0.005(2) O2 0.056(3) 0.044(2) 0.044(2) -0.0049(19) 0.020(2) 0.003(2) Pt1 0.04239(14) 0.03473(12) 0.03158(11) -0.00047(10) 0.01311(9) -0.00103(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 C1 N1 1.349(7) . ? C1 C2 1.370(8) . ? C1 H1A 0.9300 . ? C2 C3 1.387(9) . ? C2 H2A 0.9300 . ? C3 C4 1.389(9) . ? C3 H3A 0.9300 . ? C4 C5 1.394(7) . ? C4 H4A 0.9300 . ? C5 N1 1.369(7) . ? C5 C6 1.459(8) . ? C6 C7 1.391(7) . ? C6 C11 1.402(7) . ? C7 C8 1.392(8) . ? C7 H7A 0.9300 . ? C8 C9 1.389(7) . ? C8 H8A 0.9300 . ? C9 C10 1.401(7) . ? C9 Ge1 1.942(5) . ? C10 C11 1.397(8) . ? C10 H10A 0.9300 . ? C11 Pt1 1.960(6) . ? C12 C13 1.380(8) . ? C12 C17 1.394(8) . ? C12 Ge1 1.943(6) . ? C13 C14 1.392(9) . ? C13 H13A 0.9300 . ? C14 C15 1.360(11) . ? C14 H14A 0.9300 . ? C15 C16 1.360(12) . ? C15 H15A 0.9300 . ? C16 C17 1.385(9) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C23 1.377(8) . ? C18 C19 1.402(8) . ? C18 Ge1 1.958(6) . ? C19 C20 1.397(9) . ? C19 H19A 0.9300 . ? C20 C21 1.384(11) . ? C20 H20A 0.9300 . ? C21 C22 1.361(11) . ? C21 H21A 0.9300 . ? C22 C23 1.390(9) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C29 1.380(8) . ? C24 C25 1.391(8) . ? C24 Ge1 1.946(6) . ? C25 C26 1.378(9) . ? C25 H25A 0.9300 . ? C26 C27 1.363(10) . ? C26 H26A 0.9300 . ? C27 C28 1.375(10) . ? C27 H27A 0.9300 . ? C28 C29 1.377(9) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 C31 1.510(9) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 O1 1.278(7) . ? C31 C32 1.407(9) . ? C32 C33 1.359(9) . ? C32 H32A 0.9300 . ? C33 O2 1.276(7) . ? C33 C34 1.508(9) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N1 Pt1 1.984(4) . ? O1 Pt1 2.090(4) . ? O2 Pt1 2.004(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 C1 C2 122.5(6) . . ? N1 C1 H1A 118.8 . . ? C2 C1 H1A 118.8 . . ? C1 C2 C3 119.2(6) . . ? C1 C2 H2A 120.4 . . ? C3 C2 H2A 120.4 . . ? C2 C3 C4 118.9(6) . . ? C2 C3 H3A 120.5 . . ? C4 C3 H3A 120.5 . . ? C3 C4 C5 120.1(6) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? N1 C5 C4 119.8(5) . . ? N1 C5 C6 112.7(5) . . ? C4 C5 C6 127.5(5) . . ? C7 C6 C11 122.1(5) . . ? C7 C6 C5 123.4(5) . . ? C11 C6 C5 114.6(5) . . ? C6 C7 C8 119.0(5) . . ? C6 C7 H7A 120.5 . . ? C8 C7 H7A 120.5 . . ? C9 C8 C7 121.1(6) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C8 C9 C10 118.6(5) . . ? C8 C9 Ge1 121.5(4) . . ? C10 C9 Ge1 119.8(4) . . ? C11 C10 C9 122.2(5) . . ? C11 C10 H10A 118.9 . . ? C9 C10 H10A 118.9 . . ? C10 C11 C6 117.1(5) . . ? C10 C11 Pt1 128.0(4) . . ? C6 C11 Pt1 114.9(4) . . ? C13 C12 C17 117.0(6) . . ? C13 C12 Ge1 121.9(5) . . ? C17 C12 Ge1 121.0(5) . . ? C12 C13 C14 121.2(7) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C15 C14 C13 120.0(8) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 120.5(7) . . ? C16 C15 H15A 119.8 . . ? C14 C15 H15A 119.8 . . ? C15 C16 C17 119.7(8) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C16 C17 C12 121.5(7) . . ? C16 C17 H17A 119.3 . . ? C12 C17 H17A 119.3 . . ? C23 C18 C19 117.8(6) . . ? C23 C18 Ge1 121.3(5) . . ? C19 C18 Ge1 120.8(5) . . ? C20 C19 C18 120.3(7) . . ? C20 C19 H19A 119.8 . . ? C18 C19 H19A 119.8 . . ? C21 C20 C19 119.7(7) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C22 C21 C20 120.5(7) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C23 119.6(7) . . ? C21 C22 H22A 120.2 . . ? C23 C22 H22A 120.2 . . ? C18 C23 C22 121.9(7) . . ? C18 C23 H23A 119.0 . . ? C22 C23 H23A 119.0 . . ? C29 C24 C25 117.0(6) . . ? C29 C24 Ge1 120.4(5) . . ? C25 C24 Ge1 122.6(5) . . ? C26 C25 C24 121.6(6) . . ? C26 C25 H25A 119.2 . . ? C24 C25 H25A 119.2 . . ? C27 C26 C25 119.6(7) . . ? C27 C26 H26A 120.2 . . ? C25 C26 H26A 120.2 . . ? C26 C27 C28 120.6(7) . . ? C26 C27 H27A 119.7 . . ? C28 C27 H27A 119.7 . . ? C27 C28 C29 119.1(7) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? C28 C29 C24 122.1(6) . . ? C28 C29 H29A 118.9 . . ? C24 C29 H29A 118.9 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C31 C32 124.6(6) . . ? O1 C31 C30 115.1(6) . . ? C32 C31 C30 120.3(6) . . ? C33 C32 C31 128.6(6) . . ? C33 C32 H32A 115.7 . . ? C31 C32 H32A 115.7 . . ? O2 C33 C32 127.3(6) . . ? O2 C33 C34 113.1(6) . . ? C32 C33 C34 119.6(6) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C9 Ge1 C12 108.3(2) . . ? C9 Ge1 C24 110.0(2) . . ? C12 Ge1 C24 112.1(3) . . ? C9 Ge1 C18 110.5(2) . . ? C12 Ge1 C18 107.7(2) . . ? C24 Ge1 C18 108.2(3) . . ? C1 N1 C5 119.5(5) . . ? C1 N1 Pt1 123.9(4) . . ? C5 N1 Pt1 116.5(4) . . ? C31 O1 Pt1 123.2(4) . . ? C33 O2 Pt1 124.1(4) . . ? C11 Pt1 N1 81.4(2) . . ? C11 Pt1 O2 92.6(2) . . ? N1 Pt1 O2 173.97(18) . . ? C11 Pt1 O1 175.24(19) . . ? N1 Pt1 O1 93.90(18) . . ? O2 Pt1 O1 92.12(16) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 28.25 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 1.059 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.128