# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Kenneth Warnmark' _publ_contact_author_email KENNETH.WARNMARK@ORGANIC.LU.SE _publ_section_title ; Formation of an heterochiral supramolecular cage by diastereomer self-discrimination. Fluorescence enhancement and C60 sensing ; loop_ _publ_author_name 'Kenneth Warnmark' 'Carlos Solano Arribas' 'Carl-Johan Carling' 'Robert P. Lemieux' 'Anders Sundin' ; Ruiyao Wang ; 'Ola F. Wendt' data_rl03tsqz _database_code_depnum_ccdc_archive 'CCDC 757793' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H19 I2 N2' _chemical_formula_weight 517.15 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' _cell_length_a 12.8256(9) _cell_length_b 12.8256(9) _cell_length_c 10.7457(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1767.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.943 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 3.557 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1716 _exptl_absorpt_correction_T_max 0.3321 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 5255 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 1558 _reflns_number_gt 1459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0358P)^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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 1558 _refine_ls_number_parameters 96 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0657 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 N1 N 1.0828(2) 1.5459(3) 0.8584(3) 0.0318(7) Uani 1 1 d . . . I1 I 1.26448(2) 1.22481(2) 1.24782(7) 0.05384(15) Uani 1 1 d . . . C1 C 1.2024(3) 1.3302(4) 1.1172(3) 0.0392(10) Uani 1 1 d . . . C2 C 1.1069(3) 1.3107(3) 1.0625(3) 0.0348(9) Uani 1 1 d . . . H2A H 1.0695 1.2493 1.0836 0.042 Uiso 1 1 calc R . . C3 C 1.0653(3) 1.3805(3) 0.9768(4) 0.0324(9) Uani 1 1 d . . . C4 C 1.1209(3) 1.4710(3) 0.9464(3) 0.0306(9) Uani 1 1 d . . . C5 C 1.2173(4) 1.4914(3) 1.0043(4) 0.0370(10) Uani 1 1 d . . . H5A H 1.2545 1.5535 0.9854 0.044 Uiso 1 1 calc R . . C6 C 1.2575(4) 1.4204(4) 1.0891(4) 0.0433(11) Uani 1 1 d . . . H6A H 1.3227 1.4335 1.1280 0.052 Uiso 1 1 calc R . . C7 C 0.9595(3) 1.3607(4) 0.9182(4) 0.0347(9) Uani 1 1 d . . . H7A H 0.969(4) 1.310(4) 0.854(4) 0.042 Uiso 1 1 d . . . H7B H 0.922(4) 1.338(4) 0.981(4) 0.042 Uiso 1 1 d . . . C8 C 1.0000 1.5000 0.7812(5) 0.0362(14) Uani 1 2 d S . . H8 H 0.973(3) 1.559(3) 0.736(4) 0.043 Uiso 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 N1 0.0324(18) 0.0378(18) 0.0251(16) 0.0029(14) 0.0029(15) 0.0069(14) I1 0.0606(2) 0.0656(2) 0.03537(18) 0.0095(2) -0.0018(2) 0.03191(12) C1 0.043(2) 0.053(3) 0.0219(19) 0.0039(18) 0.0059(18) 0.021(2) C2 0.042(2) 0.035(2) 0.0267(19) 0.0007(17) 0.0047(18) 0.0104(18) C3 0.037(2) 0.036(2) 0.0241(19) -0.0016(16) 0.0047(17) 0.0115(17) C4 0.027(2) 0.041(2) 0.024(2) -0.0008(16) 0.0045(15) 0.0096(17) C5 0.033(2) 0.042(2) 0.037(2) 0.0015(18) 0.0048(19) 0.0002(19) C6 0.036(2) 0.060(3) 0.034(2) 0.001(2) -0.0063(18) 0.009(2) C7 0.040(3) 0.036(2) 0.028(2) -0.0030(18) 0.0002(18) 0.002(2) C8 0.037(3) 0.040(3) 0.032(4) 0.000 0.000 0.009(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C4 1.435(5) . ? N1 C7 1.464(5) 2_785 ? N1 C8 1.470(4) . ? I1 C1 2.105(4) . ? C1 C2 1.381(6) . ? C1 C6 1.389(7) . ? C2 C3 1.392(5) . ? C3 C4 1.400(6) . ? C3 C7 1.517(6) . ? C4 C5 1.408(6) . ? C5 C6 1.388(6) . ? C7 N1 1.464(5) 2_785 ? C8 N1 1.470(4) 2_785 ? 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 C4 N1 C7 112.6(3) . 2_785 ? C4 N1 C8 110.5(3) . . ? C7 N1 C8 107.9(3) 2_785 . ? C2 C1 C6 120.7(4) . . ? C2 C1 I1 120.2(3) . . ? C6 C1 I1 119.2(3) . . ? C1 C2 C3 120.4(4) . . ? C2 C3 C4 119.5(4) . . ? C2 C3 C7 120.7(4) . . ? C4 C3 C7 119.8(4) . . ? C3 C4 C5 119.9(4) . . ? C3 C4 N1 122.4(4) . . ? C5 C4 N1 117.7(4) . . ? C6 C5 C4 119.6(4) . . ? C5 C6 C1 120.0(4) . . ? N1 C7 C3 112.1(4) 2_785 . ? N1 C8 N1 111.4(4) . 2_785 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.0(6) . . . . ? I1 C1 C2 C3 179.5(3) . . . . ? C1 C2 C3 C4 -0.1(5) . . . . ? C1 C2 C3 C7 -178.8(4) . . . . ? C2 C3 C4 C5 -1.2(5) . . . . ? C7 C3 C4 C5 177.6(4) . . . . ? C2 C3 C4 N1 179.6(3) . . . . ? C7 C3 C4 N1 -1.7(6) . . . . ? C7 N1 C4 C3 103.4(4) 2_785 . . . ? C8 N1 C4 C3 -17.3(5) . . . . ? C7 N1 C4 C5 -75.8(4) 2_785 . . . ? C8 N1 C4 C5 163.4(3) . . . . ? C3 C4 C5 C6 1.4(6) . . . . ? N1 C4 C5 C6 -179.3(4) . . . . ? C4 C5 C6 C1 -0.5(6) . . . . ? C2 C1 C6 C5 -0.8(6) . . . . ? I1 C1 C6 C5 -179.3(3) . . . . ? C2 C3 C7 N1 164.5(4) . . . 2_785 ? C4 C3 C7 N1 -14.2(5) . . . 2_785 ? C4 N1 C8 N1 53.3(2) . . . 2_785 ? C7 N1 C8 N1 -70.2(2) 2_785 . . 2_785 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.342 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.088 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.000 0.000 0.062 218.0 59.8 2 0.500 0.500 -0.047 218.0 59.8 _platon_squeeze_details ; Difference electron density maps revealed the presence of disordered lattice solvate molecules, which were ultimately modeled through the use of the SQUEEZE subroutine of the PLATON software suite. PLATON Reference: P.v.d. Sluis & A.L. Spek. Acta Cryst. (1990), A46, 194. Two solvent accessible voids per lattice were found. Each void comprises a total volume of 218.0 A3 and contributes a total of 59.8 electrons. The void was assigned to a disordered hexane molecule, which contributes 50 electrons, and ocuppy about 120 A3 in space. The contributions have been included in all derived crystal quantities although the precise composition of the lattice solvate is somewhat speculative. ; # Attachment 'COMP3final.CIF' data_carlossq _database_code_depnum_ccdc_archive 'CCDC 767718' #TrackingRef 'COMP3final.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144 H142 F12 N8 O24 P4 Pt2 S4' _chemical_formula_weight 3238.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Pt Pt -1.7033 8.3905 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1' _symmetry_cell_setting triclinic loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7008(14) _cell_length_b 16.243(2) _cell_length_c 26.053(4) _cell_angle_alpha 81.532(11) _cell_angle_beta 88.552(10) _cell_angle_gamma 72.067(11) _cell_volume 4658.6(11) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4639 _cell_measurement_theta_min 2.2070 _cell_measurement_theta_max 33.0787 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1642 _exptl_absorpt_coefficient_mu 1.646 _exptl_absorpt_correction_T_min 0.87000 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 16.1829 _diffrn_measurement_device_type ; Oxford Diffraction Xcalibur ; _diffrn_measurement_method 'omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28809 _diffrn_reflns_av_R_equivalents 0.1030 _diffrn_reflns_av_sigmaI/netI 0.3355 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.03 _reflns_number_total 15896 _reflns_number_gt 6250 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 2006)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 2006)' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 2000)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1500P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15896 _refine_ls_number_parameters 721 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.2092 _refine_ls_R_factor_gt 0.1380 _refine_ls_wR_factor_ref 0.3524 _refine_ls_wR_factor_gt 0.3330 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Pt01 Pt 0.97493(7) 0.28063(6) 0.64938(3) 0.0538(3) Uani 1 1 d . . . P1 P 0.8785(4) 0.3349(3) 0.57160(18) 0.0468(13) Uani 1 1 d . . . S1 S 0.1961(5) 0.4721(5) 0.6123(3) 0.095(2) Uani 1 1 d . . . C1 C 1.1639(16) 0.2091(13) 0.5531(7) 0.058(5) Uiso 1 1 d . . . H1A H 1.1978 0.2550 0.5579 0.070 Uiso 1 1 calc R . . H1B H 1.2274 0.1613 0.5420 0.070 Uiso 1 1 calc R . . F1 F 0.4117(14) 0.4514(14) 0.6431(8) 0.156(7) Uani 1 1 d . . . O1 O 0.184(2) 0.5577(14) 0.5901(11) 0.187(11) Uani 1 1 d . . . P2 P 1.1045(4) 0.1707(3) 0.61467(17) 0.0505(13) Uani 1 1 d . . . S2 S 0.7307(7) 0.1222(6) 0.7618(4) 0.123(3) Uani 1 1 d . . . C2 C 1.0614(15) 0.2451(13) 0.5102(7) 0.060(5) Uani 1 1 d . . . H2A H 1.0966 0.2474 0.4761 0.072 Uiso 1 1 calc R . . H2B H 1.0125 0.2063 0.5122 0.072 Uiso 1 1 calc R . . O2 O 0.157(2) 0.4158(18) 0.5885(12) 0.221(14) Uani 1 1 d . . . F2 F 0.377(2) 0.3372(13) 0.6488(11) 0.226(13) Uani 1 1 d . . . N3 N 0.3236(14) 0.8593(14) 0.9242(6) 0.076(5) Uani 1 1 d . . . F3 F 0.4108(16) 0.4088(17) 0.5754(11) 0.207(11) Uani 1 1 d . . . C3 C 0.9821(15) 0.3377(13) 0.5182(7) 0.063(6) Uani 1 1 d . . . H3A H 0.9364 0.3664 0.4865 0.075 Uiso 1 1 calc R . . H3B H 1.0333 0.3719 0.5252 0.075 Uiso 1 1 calc R . . O3 O 0.1689(15) 0.4767(13) 0.6668(7) 0.125(7) Uani 1 1 d . . . N4 N 0.4559(14) 0.9499(11) 0.9003(6) 0.066(5) Uani 1 1 d . . . O4 O 0.775(2) 0.1743(13) 0.7245(6) 0.135(7) Uani 1 1 d . . . C4 C 1.2442(15) 0.1126(12) 0.6546(7) 0.050(5) Uani 1 1 d . . . C5 C 1.3409(17) 0.1379(17) 0.6458(8) 0.091(8) Uani 1 1 d . . . H5 H 1.3439 0.1809 0.6185 0.109 Uiso 1 1 calc R . . O5 O 0.799(2) 0.1032(16) 0.8137(10) 0.199(12) Uani 1 1 d . . . C6 C 1.4404(19) 0.095(2) 0.6807(9) 0.111(10) Uani 1 1 d . . . H6 H 1.5065 0.1159 0.6772 0.133 Uiso 1 1 calc R . . O6 O 0.7057(19) 0.0526(14) 0.7457(11) 0.169(10) Uani 1 1 d . . . C7 C 1.4460(19) 0.0286(18) 0.7179(9) 0.089(8) Uani 1 1 d . . . H7 H 1.5162 -0.0010 0.7372 0.106 Uiso 1 1 calc R . . O7 O 0.412(2) 0.056(2) 0.5205(10) 0.188(11) Uani 1 1 d . . . C8 C 1.334(3) 0.0036(14) 0.7271(10) 0.114(10) Uani 1 1 d . . . H8 H 1.3267 -0.0388 0.7541 0.137 Uiso 1 1 calc R . . O8 O 0.566(2) 0.2320(14) 0.3707(8) 0.141(7) Uani 1 1 d . . . C9 C 1.2389(18) 0.0499(14) 0.6913(8) 0.083(8) Uani 1 1 d . . . H9 H 1.1684 0.0346 0.6939 0.100 Uiso 1 1 calc R . . O9 O 0.742(3) 0.2893(19) 0.3124(11) 0.243(15) Uani 1 1 d . . . O10 O 0.936(3) 0.958(2) 0.0188(13) 0.239(15) Uani 1 1 d . . . C10 C 1.0850(12) 0.0362(11) 0.5660(5) 0.097(8) Uiso 1 1 d G . . H10 H 1.1432 0.0497 0.5444 0.116 Uiso 1 1 calc R . . C11 C 1.0423(15) -0.0320(10) 0.5582(6) 0.115(9) Uiso 1 1 d G . . H11 H 1.0720 -0.0642 0.5314 0.138 Uiso 1 1 calc R . . C12 C 0.9553(15) -0.0522(9) 0.5905(7) 0.103(9) Uiso 1 1 d G . . H12 H 0.9268 -0.0979 0.5852 0.124 Uiso 1 1 calc R . . C13 C 0.9109(12) -0.0041(11) 0.6305(6) 0.110(10) Uani 1 1 d G . . H13 H 0.8527 -0.0176 0.6521 0.132 Uiso 1 1 calc R . . C14 C 0.9535(12) 0.0641(10) 0.6383(5) 0.077(6) Uani 1 1 d G . . H14 H 0.9238 0.0963 0.6651 0.092 Uiso 1 1 calc R . . C15 C 1.0406(12) 0.0843(8) 0.6060(6) 0.063(5) Uiso 1 1 d G . . C16 C 0.7884(18) 0.4508(13) 0.5687(7) 0.060(5) Uani 1 1 d . . . C17 C 0.6640(16) 0.4751(12) 0.5647(9) 0.073(7) Uani 1 1 d . . . H17 H 0.6247 0.4333 0.5649 0.087 Uiso 1 1 calc R . . C18 C 0.601(2) 0.5622(18) 0.5605(9) 0.089(7) Uiso 1 1 d . . . H18 H 0.5176 0.5800 0.5557 0.107 Uiso 1 1 calc R . . C19 C 0.657(3) 0.6226(16) 0.5632(12) 0.134(13) Uani 1 1 d . . . H19 H 0.6120 0.6806 0.5639 0.160 Uiso 1 1 calc R . . C20 C 0.776(3) 0.5994(14) 0.5649(9) 0.080(7) Uani 1 1 d . . . H20 H 0.8131 0.6429 0.5634 0.096 Uiso 1 1 calc R . . C21 C 0.8436(19) 0.5180(13) 0.5687(8) 0.076(7) Uani 1 1 d . . . H21 H 0.9268 0.5039 0.5713 0.091 Uiso 1 1 calc R . . C22 C 0.7764(14) 0.2824(11) 0.5538(6) 0.046(5) Uani 1 1 d . . . C23 C 0.7463(17) 0.2845(16) 0.5031(8) 0.083(7) Uani 1 1 d . . . H23 H 0.7812 0.3120 0.4762 0.100 Uiso 1 1 calc R . . C24 C 0.657(2) 0.242(2) 0.4925(12) 0.115(10) Uani 1 1 d . . . H24 H 0.6373 0.2400 0.4585 0.137 Uiso 1 1 calc R . . C25 C 0.605(2) 0.2060(17) 0.5315(11) 0.100(9) Uani 1 1 d . . . H25 H 0.5410 0.1871 0.5239 0.121 Uiso 1 1 calc R . . C26 C 0.641(2) 0.1950(17) 0.5832(10) 0.102(9) Uani 1 1 d . . . H26 H 0.6116 0.1611 0.6090 0.122 Uiso 1 1 calc R . . C27 C 0.7229(17) 0.2377(14) 0.5944(8) 0.072(6) Uani 1 1 d . . . H27 H 0.7430 0.2370 0.6288 0.086 Uiso 1 1 calc R . . N1 N 1.0632(10) 0.2385(8) 0.7217(4) 0.028(3) Uiso 1 1 d . . . C28 C 1.0378(17) 0.1931(13) 0.7596(7) 0.068(6) Uani 1 1 d . . . H28 H 0.9748 0.1706 0.7559 0.082 Uiso 1 1 calc R . . C29 C 1.0969(19) 0.1731(15) 0.8079(7) 0.077(7) Uani 1 1 d . . . H29 H 1.0728 0.1391 0.8353 0.093 Uiso 1 1 calc R . . C30 C 1.1928(16) 0.2049(13) 0.8142(8) 0.057(5) Uani 1 1 d . . . C31 C 1.222(2) 0.2605(13) 0.7746(8) 0.077(7) Uani 1 1 d . . . H31 H 1.2790 0.2883 0.7793 0.092 Uiso 1 1 calc R . . C32 C 1.1610(13) 0.2734(13) 0.7258(7) 0.059(6) Uani 1 1 d . . . H32 H 1.1846 0.3043 0.6967 0.070 Uiso 1 1 calc R . . C33 C 1.251(2) 0.1887(15) 0.8642(8) 0.078(7) Uani 1 1 d . . . C34 C 1.3071(18) 0.1711(14) 0.9028(9) 0.074(6) Uani 1 1 d . . . N2 N 0.8615(8) 0.3805(5) 0.6838(3) 0.030(3) Uiso 1 1 d G . . C35 C 0.8921(6) 0.4531(6) 0.6934(3) 0.007(3) Uiso 1 1 d G . . H35 H 0.9638 0.4612 0.6811 0.009 Uiso 1 1 calc R . . C36 C 0.8155(9) 0.5137(5) 0.7212(4) 0.061(5) Uiso 1 1 d G . . H36 H 0.8360 0.5623 0.7276 0.074 Uiso 1 1 calc R . . C37 C 0.7083(8) 0.5017(7) 0.7395(4) 0.058(5) Uiso 1 1 d G . . C38 C 0.6777(8) 0.4291(8) 0.7299(5) 0.072(6) Uani 1 1 d G . . H38 H 0.6060 0.4211 0.7422 0.086 Uiso 1 1 calc R . . C39 C 0.7543(9) 0.3685(6) 0.7021(4) 0.074(7) Uani 1 1 d G . . H39 H 0.7338 0.3199 0.6957 0.089 Uiso 1 1 calc R . . C40 C 0.636(2) 0.5607(15) 0.7742(8) 0.094(9) Uani 1 1 d . . . C41 C 0.581(2) 0.6116(16) 0.8016(9) 0.087(8) Uani 1 1 d . . . C42 C 0.5109(15) 0.6743(9) 0.8330(5) 0.092(9) Uani 1 1 d G . . C43 C 0.4219(17) 0.6577(9) 0.8654(6) 0.124(11) Uani 1 1 d G . . H43 H 0.4043 0.6054 0.8666 0.149 Uiso 1 1 calc R . . C44 C 0.3593(13) 0.7193(12) 0.8962(6) 0.090(7) Uani 1 1 d G . . C45 C 0.3856(12) 0.7974(10) 0.8944(5) 0.065(6) Uiso 1 1 d G . . C46 C 0.4746(13) 0.8140(8) 0.8620(5) 0.065(6) Uani 1 1 d G . . C47 C 0.5372(11) 0.7525(11) 0.8312(5) 0.073(6) Uani 1 1 d G . . H47 H 0.5967 0.7636 0.8095 0.087 Uiso 1 1 calc R . . C48 C 0.509(2) 0.8940(15) 0.8616(7) 0.082(7) Uani 1 1 d . . . H48A H 0.5958 0.8769 0.8660 0.098 Uiso 1 1 calc R . . H48B H 0.4890 0.9288 0.8276 0.098 Uiso 1 1 calc R . . C49 C 0.3278(17) 0.9445(17) 0.9068(9) 0.079(7) Uani 1 1 d . . . H49A H 0.2869 0.9825 0.9314 0.094 Uiso 1 1 calc R . . H49B H 0.2849 0.9658 0.8738 0.094 Uiso 1 1 calc R . . C50 C 0.3651(19) 0.8381(18) 0.9798(8) 0.093(8) Uani 1 1 d . . . H50A H 0.3001 0.8670 1.0011 0.111 Uiso 1 1 calc R . . H50B H 0.3846 0.7756 0.9907 0.111 Uiso 1 1 calc R . . C51 C 0.4698(18) 0.8652(10) 0.9886(7) 0.052(5) Uani 1 1 d . . . C52 C 0.5177(18) 0.9134(14) 0.9515(10) 0.078(7) Uani 1 1 d . . . C53 C 0.624(2) 0.9286(15) 0.9569(8) 0.079(6) Uani 1 1 d . . . C54 C 0.683(2) 0.8962(18) 1.0051(9) 0.091(8) Uani 1 1 d . . . H54 H 0.7568 0.9045 1.0104 0.110 Uiso 1 1 calc R . . C55 C 0.636(2) 0.8525(15) 1.0453(8) 0.075(6) Uani 1 1 d . . . C56 C 0.5322(18) 0.8345(16) 1.0370(9) 0.082(7) Uani 1 1 d . . . H56 H 0.5021 0.8020 1.0633 0.098 Uiso 1 1 calc R . . C57 C 0.6762(19) 0.990(2) 0.9131(9) 0.106(9) Uani 1 1 d . . . C58 C 0.248(3) 0.697(2) 0.9301(14) 0.166(14) Uani 1 1 d . . . H58A H 0.2464 0.6399 0.9260 0.249 Uiso 1 1 calc R . . H58B H 0.1734 0.7397 0.9179 0.249 Uiso 1 1 calc R . . H58C H 0.2606 0.6993 0.9661 0.249 Uiso 1 1 calc R . . C59 C 0.361(2) 0.407(2) 0.6206(16) 0.119(11) Uani 1 1 d . . . C100 C 0.409(3) 0.0431(19) 0.4691(12) 0.115(9) Uiso 1 1 d . . . H10A H 0.3506 0.0941 0.4504 0.138 Uiso 1 1 calc R . . H10B H 0.3799 -0.0065 0.4679 0.138 Uiso 1 1 calc R . . C101 C 0.469(5) -0.027(3) 0.561(2) 0.24(2) Uiso 1 1 d . . . H10C H 0.4327 -0.0727 0.5618 0.285 Uiso 1 1 calc R . . H10D H 0.4754 -0.0132 0.5961 0.285 Uiso 1 1 calc R . . C106 C 0.159(3) 0.858(2) 0.7642(14) 0.164(13) Uiso 1 1 d D . . H10E H 0.2412 0.8353 0.7535 0.197 Uiso 1 1 calc R . . H10F H 0.1082 0.8854 0.7336 0.197 Uiso 1 1 calc R . . O14 O 0.150(5) 0.919(3) 0.799(2) 0.33(2) Uiso 1 1 d . . . C108 C 0.663(3) 0.175(2) 0.3556(12) 0.126(10) Uiso 1 1 d . . . H10G H 0.6451 0.1540 0.3248 0.151 Uiso 1 1 calc R . . H10H H 0.6922 0.1256 0.3828 0.151 Uiso 1 1 calc R . . C109 C 0.994(4) 0.925(3) -0.0333(17) 0.191(16) Uiso 1 1 d . . . H10I H 1.0697 0.8786 -0.0269 0.229 Uiso 1 1 calc R . . H10J H 0.9394 0.9056 -0.0528 0.229 Uiso 1 1 calc R . . C112 C 0.759(4) 0.222(3) 0.3438(16) 0.176(15) Uiso 1 1 d . . . H11A H 0.7817 0.2346 0.3766 0.212 Uiso 1 1 calc R . . H11B H 0.8296 0.1791 0.3323 0.212 Uiso 1 1 calc R . . C113 C 0.991(4) 0.989(3) 0.0594(17) 0.191(16) Uiso 1 1 d . . . H11C H 1.0674 0.9473 0.0711 0.229 Uiso 1 1 calc R . . H11D H 0.9384 0.9983 0.0890 0.229 Uiso 1 1 calc R . . C114 C 0.036(4) 0.949(3) 0.8011(18) 0.210(19) Uiso 1 1 d D . . H11E H 0.0036 0.9738 0.7664 0.252 Uiso 1 1 calc R . . H11F H 0.0170 0.9963 0.8219 0.252 Uiso 1 1 calc R . . C104 C 0.113(4) 0.779(2) 0.7979(15) 0.171(14) Uiso 1 1 d D . . H10K H 0.1353 0.7271 0.7814 0.206 Uiso 1 1 calc R . . H10L H 0.1442 0.7650 0.8332 0.206 Uiso 1 1 calc R . . C116 C -0.031(5) 0.875(3) 0.827(2) 0.25(2) Uiso 1 1 d D . . H11G H -0.0006 0.8493 0.8614 0.306 Uiso 1 1 calc R . . H11H H -0.1175 0.9023 0.8278 0.306 Uiso 1 1 calc R . . C60 C 0.605(3) 0.195(2) 0.7882(11) 0.22(3) Uani 1 1 d D . . F5 F 0.536(2) 0.1546(16) 0.8127(10) 0.254(15) Uani 1 1 d D . . F6 F 0.529(2) 0.2251(18) 0.7485(14) 0.278(17) Uani 1 1 d D . . C117 C 0.609(4) 0.338(3) 0.3224(16) 0.182(16) Uiso 1 1 d . . . H11I H 0.6100 0.3734 0.3494 0.218 Uiso 1 1 calc R . . H11J H 0.5782 0.3788 0.2911 0.218 Uiso 1 1 calc R . . F4 F 0.612(2) 0.2615(16) 0.8077(10) 0.184(10) Uiso 1 1 d D . . O12 O -0.006(5) 0.817(3) 0.796(2) 0.33(2) Uiso 1 1 d . . . C121 C 0.518(4) 0.292(3) 0.3375(18) 0.196(18) Uiso 1 1 d . . . H12A H 0.4475 0.3316 0.3508 0.236 Uiso 1 1 calc R . . H12B H 0.4949 0.2711 0.3078 0.236 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 Pt01 0.0483(5) 0.0672(6) 0.0418(5) 0.0067(4) -0.0075(3) -0.0179(4) P1 0.035(3) 0.055(3) 0.044(3) -0.004(2) -0.004(2) -0.007(2) S1 0.064(4) 0.124(6) 0.093(5) 0.012(5) -0.022(4) -0.036(4) F1 0.074(10) 0.197(19) 0.20(2) -0.027(16) -0.029(11) -0.047(12) O1 0.17(2) 0.097(16) 0.24(3) 0.071(17) -0.099(19) -0.009(15) P2 0.060(3) 0.053(3) 0.033(3) 0.005(2) -0.015(2) -0.014(3) S2 0.090(5) 0.142(8) 0.147(7) 0.010(6) -0.003(5) -0.064(5) C2 0.037(10) 0.072(15) 0.063(13) -0.005(11) -0.009(9) -0.004(10) O2 0.21(3) 0.22(3) 0.29(3) -0.14(3) -0.06(2) -0.09(2) F2 0.22(2) 0.098(15) 0.30(3) 0.094(18) -0.02(2) -0.013(15) N3 0.063(11) 0.117(17) 0.055(11) 0.006(11) 0.004(9) -0.044(12) F3 0.085(12) 0.29(3) 0.26(3) -0.10(2) 0.057(16) -0.046(15) C3 0.043(11) 0.082(16) 0.058(12) 0.031(11) -0.010(9) -0.031(11) O3 0.107(13) 0.153(17) 0.099(14) 0.039(12) 0.030(11) -0.047(12) N4 0.068(11) 0.074(12) 0.046(10) 0.006(9) -0.003(9) -0.012(9) O4 0.20(2) 0.123(16) 0.071(11) 0.000(11) 0.036(13) -0.041(15) C4 0.044(11) 0.047(12) 0.053(11) 0.005(10) -0.018(9) -0.011(9) C5 0.055(13) 0.17(2) 0.064(14) 0.032(15) 0.004(11) -0.076(15) O5 0.154(19) 0.18(2) 0.21(2) 0.080(19) -0.112(19) -0.029(17) C6 0.050(14) 0.20(3) 0.069(15) 0.047(19) -0.021(12) -0.052(17) O6 0.137(17) 0.123(17) 0.27(3) -0.032(19) -0.036(18) -0.073(15) C7 0.048(13) 0.14(2) 0.074(16) 0.000(16) -0.017(11) -0.032(15) O7 0.135(18) 0.29(3) 0.15(2) -0.11(3) 0.056(17) -0.06(2) C8 0.16(3) 0.037(14) 0.12(2) 0.020(14) -0.07(2) -0.003(16) O8 0.145(18) 0.126(17) 0.112(15) -0.001(14) -0.019(13) 0.009(14) C9 0.081(15) 0.093(17) 0.086(15) 0.055(14) -0.035(12) -0.070(14) O9 0.29(4) 0.16(2) 0.20(3) 0.11(2) 0.04(2) -0.03(2) O10 0.26(3) 0.32(4) 0.25(3) -0.10(3) 0.09(3) -0.25(3) C13 0.070(15) 0.12(2) 0.16(3) 0.02(2) 0.000(16) -0.075(16) C14 0.063(13) 0.083(17) 0.067(14) -0.002(13) 0.007(11) 0.001(12) C16 0.075(14) 0.078(15) 0.035(10) -0.018(10) 0.015(10) -0.034(12) C17 0.037(11) 0.042(13) 0.128(19) 0.018(12) 0.027(11) -0.012(10) C19 0.18(3) 0.040(16) 0.17(3) 0.014(17) 0.09(3) -0.03(2) C20 0.106(19) 0.019(13) 0.12(2) -0.004(12) 0.027(16) -0.024(13) C21 0.073(14) 0.034(14) 0.117(18) 0.031(12) -0.027(13) -0.028(12) C22 0.044(10) 0.049(12) 0.035(10) 0.012(9) 0.007(8) -0.008(9) C23 0.058(13) 0.14(2) 0.053(14) -0.031(14) -0.007(11) -0.021(14) C24 0.076(17) 0.19(3) 0.12(2) -0.08(2) -0.011(16) -0.071(19) C25 0.098(19) 0.11(2) 0.11(2) 0.000(18) 0.021(18) -0.063(17) C26 0.15(2) 0.13(2) 0.075(17) -0.003(16) -0.012(16) -0.11(2) C27 0.073(14) 0.090(17) 0.053(13) -0.004(12) -0.034(11) -0.027(13) C28 0.070(13) 0.075(15) 0.064(13) 0.032(12) -0.005(11) -0.050(12) C29 0.087(16) 0.101(18) 0.042(12) 0.005(12) -0.016(11) -0.032(14) C30 0.049(12) 0.059(14) 0.067(14) -0.022(12) -0.009(10) -0.014(10) C31 0.097(17) 0.067(15) 0.064(14) 0.026(12) -0.004(13) -0.038(13) C32 0.018(8) 0.108(17) 0.043(11) -0.008(11) 0.009(8) -0.011(10) C33 0.090(17) 0.099(19) 0.050(13) -0.007(13) -0.002(13) -0.036(14) C34 0.076(15) 0.069(15) 0.078(16) 0.007(12) -0.042(13) -0.030(12) C38 0.108(17) 0.058(14) 0.053(13) 0.004(11) -0.021(12) -0.034(13) C39 0.097(16) 0.092(17) 0.061(14) -0.059(13) 0.041(12) -0.047(14) C40 0.13(2) 0.063(16) 0.052(14) -0.019(12) -0.052(14) 0.041(14) C41 0.095(18) 0.077(18) 0.078(17) -0.042(15) -0.028(14) 0.004(14) C42 0.15(2) 0.047(15) 0.038(13) -0.016(11) -0.043(14) 0.031(15) C43 0.16(3) 0.18(3) 0.028(13) -0.039(17) 0.028(15) -0.03(2) C44 0.086(17) 0.14(2) 0.052(14) -0.018(15) -0.004(13) -0.040(16) C46 0.070(14) 0.067(16) 0.042(12) -0.019(11) -0.027(10) 0.010(12) C47 0.087(15) 0.069(16) 0.070(15) -0.048(13) -0.015(12) -0.018(13) C48 0.102(17) 0.098(19) 0.034(12) 0.012(13) -0.038(12) -0.023(15) C49 0.051(13) 0.11(2) 0.087(16) -0.048(16) -0.022(12) -0.025(13) C50 0.075(15) 0.14(2) 0.064(15) -0.028(15) -0.025(12) -0.035(16) C51 0.086(15) 0.008(9) 0.050(12) 0.003(8) -0.011(11) 0.000(9) C52 0.052(13) 0.065(16) 0.11(2) -0.023(15) -0.036(13) -0.005(12) C53 0.097(18) 0.085(17) 0.056(14) -0.004(13) -0.013(13) -0.034(14) C54 0.071(15) 0.16(2) 0.064(16) -0.041(17) -0.001(13) -0.048(16) C55 0.063(15) 0.094(18) 0.058(14) -0.023(13) 0.011(12) -0.005(13) C56 0.051(13) 0.12(2) 0.077(16) -0.047(15) 0.005(12) -0.011(13) C57 0.062(15) 0.18(3) 0.073(16) -0.018(18) 0.003(13) -0.030(17) C58 0.17(3) 0.14(3) 0.21(4) -0.07(3) 0.06(3) -0.07(3) C59 0.067(19) 0.14(3) 0.17(3) -0.04(3) 0.06(2) -0.06(2) C60 0.043(18) 0.48(9) 0.12(3) 0.07(4) -0.001(18) -0.11(3) F5 0.22(2) 0.24(3) 0.22(2) 0.09(2) 0.13(2) -0.01(2) F6 0.107(17) 0.25(3) 0.48(5) -0.12(3) 0.05(3) -0.051(18) _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 Pt01 N2 2.059(7) . ? Pt01 N1 2.089(11) . ? Pt01 P2 2.245(5) . ? Pt01 P1 2.266(4) . ? P1 C22 1.772(18) . ? P1 C3 1.827(18) . ? P1 C16 1.84(2) . ? S1 O2 1.37(2) . ? S1 O1 1.39(2) . ? S1 O3 1.456(18) . ? S1 C59 1.89(3) . ? C1 C2 1.57(2) . ? C1 P2 1.833(18) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? F1 C59 1.27(3) . ? P2 C15 1.824(12) . ? P2 C4 1.869(16) . ? S2 O6 1.37(2) . ? S2 O4 1.390(18) . ? S2 O5 1.53(2) . ? S2 C60 1.78(3) . ? C2 C3 1.54(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? F2 C59 1.22(3) . ? N3 C45 1.37(2) . ? N3 C49 1.41(3) . ? N3 C50 1.50(2) . ? F3 C59 1.30(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? N4 C48 1.45(2) . ? N4 C52 1.48(3) . ? N4 C49 1.53(2) . ? C4 C9 1.30(2) . ? C4 C5 1.32(2) . ? C5 C6 1.42(3) . ? C5 H5 0.9300 . ? C6 C7 1.33(3) . ? C6 H6 0.9300 . ? C7 C8 1.49(3) . ? C7 H7 0.9300 . ? O7 C100 1.39(3) . ? O7 C101 1.56(5) . ? C8 C9 1.41(3) . ? C8 H8 0.9300 . ? O8 C121 1.21(4) . ? O8 C108 1.32(3) . ? C9 H9 0.9300 . ? O9 C112 1.23(4) . ? O9 C117 1.55(4) . ? O10 C113 1.47(4) . ? O10 C109 1.60(4) . ? C10 C11 1.3900 . ? C10 C15 1.3900 . ? C10 H10 0.9300 . ? C11 C12 1.3900 . ? C11 H11 0.9300 . ? C12 C13 1.3900 . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 H13 0.9300 . ? C14 C15 1.3900 . ? C14 H14 0.9300 . ? C16 C17 1.39(2) . ? C16 C21 1.43(2) . ? C17 C18 1.37(3) . ? C17 H17 0.9300 . ? C18 C19 1.35(3) . ? C18 H18 0.9300 . ? C19 C20 1.33(3) . ? C19 H19 0.9300 . ? C20 C21 1.31(3) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.37(2) . ? C22 C27 1.43(2) . ? C23 C24 1.47(3) . ? C23 H23 0.9300 . ? C24 C25 1.32(3) . ? C24 H24 0.9300 . ? C25 C26 1.39(3) . ? C25 H25 0.9300 . ? C26 C27 1.41(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? N1 C28 1.231(18) . ? N1 C32 1.438(19) . ? C28 C29 1.40(2) . ? C28 H28 0.9300 . ? C29 C30 1.40(3) . ? C29 H29 0.9300 . ? C30 C31 1.38(3) . ? C30 C33 1.43(3) . ? C31 C32 1.43(2) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.17(2) . ? C34 C55 1.47(3) 2_767 ? N2 C35 1.3895 . ? N2 C39 1.3901 . ? C35 C36 1.3905 . ? C35 H35 0.9300 . ? C36 C37 1.3900 . ? C36 H36 0.9300 . ? C37 C38 1.3897 . ? C37 C40 1.48(2) . ? C38 C39 1.3900 . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.19(3) . ? C41 C42 1.44(3) . ? C42 C47 1.3903 . ? C42 C43 1.3903 . ? C43 C44 1.3904 . ? C43 H43 0.9300 . ? C44 C45 1.3896 . ? C44 C58 1.65(3) . ? C45 C46 1.3901 . ? C46 C47 1.3902 . ? C46 C48 1.47(2) . ? C47 H47 0.9300 . ? C48 H48A 0.9700 . ? C48 H48B 0.9700 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.46(3) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.37(3) . ? C51 C56 1.42(3) . ? C52 C53 1.36(3) . ? C53 C54 1.40(3) . ? C53 C57 1.64(3) . ? C54 C55 1.38(3) . ? C54 H54 0.9300 . ? C55 C56 1.36(3) . ? C55 C34 1.47(3) 2_767 ? C56 H56 0.9300 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C100 C101 1.58(5) 2_656 ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C101 C100 1.58(5) 2_656 ? C101 H10C 0.9700 . ? C101 H10D 0.9700 . ? C106 O14 1.41(5) . ? C106 C104 1.67(4) . ? C106 H10E 0.9700 . ? C106 H10F 0.9700 . ? O14 C114 1.27(5) . ? C108 C112 1.54(4) . ? C108 H10G 0.9700 . ? C108 H10H 0.9700 . ? C109 C113 1.52(5) 2_775 ? C109 H10I 0.9700 . ? C109 H10J 0.9700 . ? C112 H11A 0.9700 . ? C112 H11B 0.9700 . ? C113 C109 1.52(5) 2_775 ? C113 H11C 0.9700 . ? C113 H11D 0.9700 . ? C114 C116 1.68(4) . ? C114 H11E 0.9700 . ? C114 H11F 0.9700 . ? C104 O12 1.34(5) . ? C104 H10K 0.9700 . ? C104 H10L 0.9700 . ? C116 O12 1.28(6) . ? C116 H11G 0.9700 . ? C116 H11H 0.9700 . ? C60 F4 1.29(2) . ? C60 F5 1.294(19) . ? C60 F6 1.32(2) . ? C117 C121 1.49(5) . ? C117 H11I 0.9700 . ? C117 H11J 0.9700 . ? C121 H12A 0.9700 . ? C121 H12B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pt01 N1 85.7(4) . . ? N2 Pt01 P2 177.5(3) . . ? N1 Pt01 P2 91.9(3) . . ? N2 Pt01 P1 91.7(3) . . ? N1 Pt01 P1 176.5(4) . . ? P2 Pt01 P1 90.62(16) . . ? C22 P1 C3 107.6(8) . . ? C22 P1 C16 104.7(8) . . ? C3 P1 C16 102.9(9) . . ? C22 P1 Pt01 116.3(6) . . ? C3 P1 Pt01 112.6(6) . . ? C16 P1 Pt01 111.7(6) . . ? O2 S1 O1 123.2(18) . . ? O2 S1 O3 117.8(17) . . ? O1 S1 O3 105.1(15) . . ? O2 S1 C59 99.3(17) . . ? O1 S1 C59 110.0(15) . . ? O3 S1 C59 98.1(15) . . ? C2 C1 P2 110.4(12) . . ? C2 C1 H1A 109.6 . . ? P2 C1 H1A 109.6 . . ? C2 C1 H1B 109.6 . . ? P2 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C15 P2 C1 109.9(8) . . ? C15 P2 C4 104.2(7) . . ? C1 P2 C4 102.5(8) . . ? C15 P2 Pt01 112.8(5) . . ? C1 P2 Pt01 112.3(7) . . ? C4 P2 Pt01 114.4(6) . . ? O6 S2 O4 116.3(16) . . ? O6 S2 O5 116.2(16) . . ? O4 S2 O5 111.6(14) . . ? O6 S2 C60 113.3(13) . . ? O4 S2 C60 105.7(13) . . ? O5 S2 C60 90.3(15) . . ? C3 C2 C1 110.0(15) . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? C1 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C45 N3 C49 114.8(16) . . ? C45 N3 C50 113.2(17) . . ? C49 N3 C50 106.3(18) . . ? C2 C3 P1 112.1(12) . . ? C2 C3 H3A 109.2 . . ? P1 C3 H3A 109.2 . . ? C2 C3 H3B 109.2 . . ? P1 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C48 N4 C52 110.5(15) . . ? C48 N4 C49 105.4(16) . . ? C52 N4 C49 106.1(16) . . ? C9 C4 C5 123.5(17) . . ? C9 C4 P2 117.0(14) . . ? C5 C4 P2 119.5(15) . . ? C4 C5 C6 116.1(19) . . ? C4 C5 H5 121.9 . . ? C6 C5 H5 121.9 . . ? C7 C6 C5 125(2) . . ? C7 C6 H6 117.4 . . ? C5 C6 H6 117.4 . . ? C6 C7 C8 117(2) . . ? C6 C7 H7 121.7 . . ? C8 C7 H7 121.7 . . ? C100 O7 C101 117(3) . . ? C9 C8 C7 114(2) . . ? C9 C8 H8 122.8 . . ? C7 C8 H8 122.8 . . ? C121 O8 C108 114(3) . . ? C4 C9 C8 124.0(19) . . ? C4 C9 H9 118.0 . . ? C8 C9 H9 118.0 . . ? C112 O9 C117 102(3) . . ? C113 O10 C109 129(3) . . ? C11 C10 C15 120.0 . . ? C11 C10 H10 120.0 . . ? C15 C10 H10 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C15 120.0 . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.0 . . ? C14 C15 P2 122.8(10) . . ? C10 C15 P2 117.1(10) . . ? C17 C16 C21 118.2(18) . . ? C17 C16 P1 120.2(15) . . ? C21 C16 P1 121.6(15) . . ? C18 C17 C16 118.4(19) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C19 C18 C17 121(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C20 C19 C18 120(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 123(2) . . ? C21 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? C20 C21 C16 119(2) . . ? C20 C21 H21 120.3 . . ? C16 C21 H21 120.3 . . ? C23 C22 C27 119.7(18) . . ? C23 C22 P1 122.2(15) . . ? C27 C22 P1 118.1(13) . . ? C22 C23 C24 118(2) . . ? C22 C23 H23 121.0 . . ? C24 C23 H23 121.0 . . ? C25 C24 C23 120(2) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 124(2) . . ? C24 C25 H25 118.0 . . ? C26 C25 H25 118.0 . . ? C25 C26 C27 116(2) . . ? C25 C26 H26 121.8 . . ? C27 C26 H26 121.8 . . ? C26 C27 C22 121.2(18) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C28 N1 C32 119.2(14) . . ? C28 N1 Pt01 128.4(12) . . ? C32 N1 Pt01 112.3(10) . . ? N1 C28 C29 124.6(17) . . ? N1 C28 H28 117.7 . . ? C29 C28 H28 117.7 . . ? C30 C29 C28 118.9(19) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? C31 C30 C29 120.1(18) . . ? C31 C30 C33 119.7(18) . . ? C29 C30 C33 119.8(19) . . ? C30 C31 C32 116.7(19) . . ? C30 C31 H31 121.7 . . ? C32 C31 H31 121.7 . . ? C31 C32 N1 120.0(16) . . ? C31 C32 H32 120.0 . . ? N1 C32 H32 120.0 . . ? C34 C33 C30 174(3) . . ? C33 C34 C55 173(2) . 2_767 ? C35 N2 C39 120.0 . . ? C35 N2 Pt01 123.3(5) . . ? C39 N2 Pt01 116.4(5) . . ? N2 C35 C36 120.0 . . ? N2 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 C40 120.6(14) . . ? C36 C37 C40 119.0(13) . . ? C37 C38 C39 120.0 . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 N2 120.0 . . ? C38 C39 H39 120.0 . . ? N2 C39 H39 120.0 . . ? C41 C40 C37 176(3) . . ? C40 C41 C42 178(2) . . ? C47 C42 C43 120.0 . . ? C47 C42 C41 117.8(16) . . ? C43 C42 C41 122.2(16) . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 C58 123.3(16) . . ? C43 C44 C58 116.6(16) . . ? N3 C45 C44 120.6(14) . . ? N3 C45 C46 119.3(14) . . ? C44 C45 C46 120.0 . . ? C45 C46 C47 120.0 . . ? C45 C46 C48 121.1(14) . . ? C47 C46 C48 118.8(14) . . ? C46 C47 C42 120.0 . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? N4 C48 C46 117.3(18) . . ? N4 C48 H48A 108.0 . . ? C46 C48 H48A 108.0 . . ? N4 C48 H48B 108.0 . . ? C46 C48 H48B 108.0 . . ? H48A C48 H48B 107.2 . . ? N3 C49 N4 113.4(17) . . ? N3 C49 H49A 108.9 . . ? N4 C49 H49A 108.9 . . ? N3 C49 H49B 108.9 . . ? N4 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C51 C50 N3 112.6(19) . . ? C51 C50 H50A 109.1 . . ? N3 C50 H50A 109.1 . . ? C51 C50 H50B 109.1 . . ? N3 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C52 C51 C56 117(2) . . ? C52 C51 C50 124.1(18) . . ? C56 C51 C50 118.3(19) . . ? C53 C52 C51 124(2) . . ? C53 C52 N4 115(2) . . ? C51 C52 N4 120.6(17) . . ? C52 C53 C54 116(2) . . ? C52 C53 C57 123(2) . . ? C54 C53 C57 120(2) . . ? C55 C54 C53 123(2) . . ? C55 C54 H54 118.7 . . ? C53 C54 H54 118.7 . . ? C56 C55 C54 119(2) . . ? C56 C55 C34 120(2) . 2_767 ? C54 C55 C34 121(2) . 2_767 ? C55 C56 C51 120(2) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? C44 C58 H58A 109.5 . . ? C44 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C44 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? F2 C59 F1 106(4) . . ? F2 C59 F3 119(4) . . ? F1 C59 F3 101(2) . . ? F2 C59 S1 113(2) . . ? F1 C59 S1 107(2) . . ? F3 C59 S1 109(3) . . ? O7 C100 C101 118(3) . 2_656 ? O7 C100 H10A 107.9 . . ? C101 C100 H10A 107.9 2_656 . ? O7 C100 H10B 107.9 . . ? C101 C100 H10B 107.9 2_656 . ? H10A C100 H10B 107.2 . . ? O7 C101 C100 89(3) . 2_656 ? O7 C101 H10C 113.7 . . ? C100 C101 H10C 113.7 2_656 . ? O7 C101 H10D 113.7 . . ? C100 C101 H10D 113.7 2_656 . ? H10C C101 H10D 111.0 . . ? O14 C106 C104 105(3) . . ? O14 C106 H10E 110.8 . . ? C104 C106 H10E 110.8 . . ? O14 C106 H10F 110.8 . . ? C104 C106 H10F 110.8 . . ? H10E C106 H10F 108.8 . . ? C114 O14 C106 100(5) . . ? O8 C108 C112 108(3) . . ? O8 C108 H10G 110.1 . . ? C112 C108 H10G 110.1 . . ? O8 C108 H10H 110.1 . . ? C112 C108 H10H 110.1 . . ? H10G C108 H10H 108.4 . . ? C113 C109 O10 97(3) 2_775 . ? C113 C109 H10I 112.3 2_775 . ? O10 C109 H10I 112.3 . . ? C113 C109 H10J 112.3 2_775 . ? O10 C109 H10J 112.3 . . ? H10I C109 H10J 109.9 . . ? O9 C112 C108 122(4) . . ? O9 C112 H11A 106.7 . . ? C108 C112 H11A 106.7 . . ? O9 C112 H11B 106.7 . . ? C108 C112 H11B 106.7 . . ? H11A C112 H11B 106.6 . . ? O10 C113 C109 105(3) . 2_775 ? O10 C113 H11C 110.8 . . ? C109 C113 H11C 110.8 2_775 . ? O10 C113 H11D 110.8 . . ? C109 C113 H11D 110.8 2_775 . ? H11C C113 H11D 108.9 . . ? O14 C114 C116 115(5) . . ? O14 C114 H11E 108.6 . . ? C116 C114 H11E 108.6 . . ? O14 C114 H11F 108.6 . . ? C116 C114 H11F 108.6 . . ? H11E C114 H11F 107.5 . . ? O12 C104 C106 101(4) . . ? O12 C104 H10K 111.5 . . ? C106 C104 H10K 111.5 . . ? O12 C104 H10L 111.5 . . ? C106 C104 H10L 111.5 . . ? H10K C104 H10L 109.4 . . ? O12 C116 C114 105(5) . . ? O12 C116 H11G 110.7 . . ? C114 C116 H11G 110.7 . . ? O12 C116 H11H 110.7 . . ? C114 C116 H11H 110.7 . . ? H11G C116 H11H 108.8 . . ? F4 C60 F5 115(3) . . ? F4 C60 F6 107(3) . . ? F5 C60 F6 92(2) . . ? F4 C60 S2 122(2) . . ? F5 C60 S2 112(2) . . ? F6 C60 S2 103(2) . . ? C121 C117 O9 123(4) . . ? C121 C117 H11I 106.6 . . ? O9 C117 H11I 106.6 . . ? C121 C117 H11J 106.6 . . ? O9 C117 H11J 106.6 . . ? H11I C117 H11J 106.6 . . ? C116 O12 C104 108(5) . . ? O8 C121 C117 106(4) . . ? O8 C121 H12A 110.5 . . ? C117 C121 H12A 110.5 . . ? O8 C121 H12B 110.5 . . ? C117 C121 H12B 110.5 . . ? H12A C121 H12B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 7.035 _refine_diff_density_min -1.798 _refine_diff_density_rms 0.270 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.078 0.500 1.000 1372 638 'disordered dioxane' _platon_squeeze_details ; ;