Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' #=========================================================================== _audit_creation_date 9-01-01 # 1. SUBMISSION DETAILS _publ_contact_author_name ; Dr. P. BRAUNSTEIN ; _publ_contact_author_address ; Prof P Braunstein Laboratoire de Chimie de Coordn. UMR 7513 CNRS Universite Louis Pasteur 4 rue Blaise Pascal Strasbourg cedex 67070 FRANCE ; _publ_contact_author_phone '0033-3902 41308' _publ_contact_author_email braunst@chimie.u-strasbg.fr _publ_contact_letter ; Please consider this CIF submission for publication as a new structure paper in Acta Crystallographica Section C. The figures, chemical structure diagram (scheme), Transfert of Copyright Agreement form and structure factors will be sent on receipt of your acknowledgement letter ; _publ_requested_category ? #=========================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Unexpected bonding similarities between the metalloligands [MoCp(CO)3]- and [PtI(CO)2(PPh3)]-. ; loop_ _publ_author_name 'Archambault, Christine' 'Bender, Robert' 'Braunstein, Pierre' 'Bouaoud, Salah Eddine' 'Rouag Djemel' 'Golhen, Stephane' 'Ouahab, Lahcene' # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; ? ; _publ_section_references ; OpenMoleN, Interactive Intelligent Structure solution (1997) Nonius B.V., Delft, The Netherlands. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ; ? ; #=========================================================================== data_abs _database_code_CSD 158327 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H55 I O2 P4 Pt3' _chemical_formula_weight 1740.17 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' 'O' 'O' 0.0106 0.0060 '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' 'I' 'I' -0.4742 1.8119 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.564(12) _cell_length_b 14.954(6) _cell_length_c 17.948(8) _cell_angle_alpha 69.64(3) _cell_angle_beta 75.44(4) _cell_angle_gamma 63.98(4) _cell_volume 3046(3) _cell_formula_units_Z 2 _cell_measurement_temperature 253(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.42 _cell_measurement_theta_max 10.88 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.897 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 7.528 _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_correction_T_min 0.759588 _exptl_absorpt_correction_T_max 0.997578 _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 'Nonius CAD4' _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 60 _diffrn_standards_interval_time 250 _diffrn_standards_decay_% ? _diffrn_reflns_number 11189 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0514 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 24.98 _reflns_number_total 10693 _reflns_number_gt 7879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4' _computing_cell_refinement 'Enraf Nonius CAD4' _computing_data_reduction MolEN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP III' _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 w==1/[\s^2^(Fo^2^)+(0.0597P)^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_number_reflns 10693 _refine_ls_number_parameters 703 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0742 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.1026 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt -0.16925(3) 0.16731(3) 0.25253(2) 0.02780(10) Uani 1 d . . . Pt2 Pt -0.13062(3) -0.01911(3) 0.23978(2) 0.02530(9) Uani 1 d . . . Pt3 Pt -0.33795(3) 0.13357(3) 0.23034(2) 0.02393(9) Uani 1 d . . . I I -0.27732(6) 0.13803(6) 0.40981(4) 0.04700(19) Uani 1 d . . . P1 P -0.1020(2) 0.28251(19) 0.25148(15) 0.0322(5) Uani 1 d . . . P2 P 0.0066(2) -0.17530(18) 0.25122(14) 0.0291(5) Uani 1 d . . . P3 P -0.5175(2) 0.21670(18) 0.20978(14) 0.0296(5) Uani 1 d . . . P4 P -0.29148(19) -0.03762(17) 0.24828(13) 0.0256(5) Uani 1 d . . . O1 O 0.0529(6) 0.0631(6) 0.1705(5) 0.060(2) Uani 1 d . . . O2 O -0.3286(6) 0.3470(5) 0.1468(4) 0.0468(18) Uani 1 d . . . C1 C -0.0317(8) 0.0654(7) 0.2047(6) 0.036(2) Uani 1 d . . . C2 C -0.3033(7) 0.2643(7) 0.1878(5) 0.0270(19) Uani 1 d . . . C3 C -0.0153(8) 0.3170(8) 0.1602(6) 0.043(3) Uani 1 d . . . C4 C -0.0263(12) 0.3051(9) 0.0907(7) 0.067(4) Uani 1 d . . . H4 H -0.0771 0.2784 0.0916 0.080 Uiso 1 calc R . . C5 C 0.0365(16) 0.3318(12) 0.0190(10) 0.107(7) Uani 1 d . . . H5 H 0.0280 0.3234 -0.0277 0.128 Uiso 1 calc R . . C6 C 0.1116(15) 0.3710(13) 0.0185(12) 0.117(9) Uani 1 d . . . H6 H 0.1539 0.3895 -0.0292 0.140 Uiso 1 calc R . . C7 C 0.1251(13) 0.3831(14) 0.0858(13) 0.117(8) Uani 1 d . . . H7 H 0.1775 0.4082 0.0845 0.141 Uiso 1 calc R . . C8 C 0.0608(10) 0.3582(10) 0.1574(8) 0.070(4) Uani 1 d . . . H8 H 0.0684 0.3689 0.2033 0.083 Uiso 1 calc R . . C9 C -0.0204(8) 0.2392(8) 0.3325(6) 0.038(2) Uani 1 d . . . C10 C 0.0265(8) 0.1349(8) 0.3698(6) 0.044(3) Uani 1 d . . . H10 H 0.0137 0.0879 0.3545 0.053 Uiso 1 calc R . . C11 C 0.0925(10) 0.0998(10) 0.4300(7) 0.056(3) Uani 1 d . . . H11 H 0.1226 0.0294 0.4554 0.067 Uiso 1 calc R . . C12 C 0.1137(10) 0.1672(12) 0.4524(7) 0.066(4) Uani 1 d . . . H12 H 0.1606 0.1428 0.4912 0.079 Uiso 1 calc R . . C13 C 0.0660(12) 0.2701(12) 0.4177(8) 0.069(4) Uani 1 d . . . H13 H 0.0782 0.3162 0.4346 0.083 Uiso 1 calc R . . C14 C -0.0003(11) 0.3076(10) 0.3578(8) 0.059(3) Uani 1 d . . . H14 H -0.0316 0.3785 0.3343 0.071 Uiso 1 calc R . . C15 C -0.2092(8) 0.4087(8) 0.2609(7) 0.043(3) Uani 1 d . . . C16 C -0.2720(11) 0.4144(10) 0.3345(9) 0.072(4) Uani 1 d . . . H16 H -0.2576 0.3575 0.3792 0.086 Uiso 1 calc R . . C17 C -0.3577(11) 0.5093(11) 0.3384(11) 0.082(5) Uani 1 d . . . H17 H -0.4024 0.5146 0.3867 0.098 Uiso 1 calc R . . C18 C -0.3779(11) 0.5929(12) 0.2752(12) 0.080(5) Uani 1 d . . . H18 H -0.4344 0.6553 0.2806 0.096 Uiso 1 calc R . . C19 C -0.3141(12) 0.5866(10) 0.2010(10) 0.074(4) Uani 1 d . . . H19 H -0.3279 0.6441 0.1567 0.088 Uiso 1 calc R . . C20 C -0.2317(10) 0.4945(9) 0.1954(8) 0.057(3) Uani 1 d . . . H20 H -0.1895 0.4891 0.1464 0.069 Uiso 1 calc R . . C21 C 0.1135(8) -0.1978(7) 0.3092(5) 0.031(2) Uani 1 d . . . C22 C 0.2241(9) -0.2585(8) 0.2960(7) 0.052(3) Uani 1 d . . . H22 H 0.2498 -0.2861 0.2524 0.063 Uiso 1 calc R . . C23 C 0.2961(10) -0.2784(10) 0.3465(9) 0.070(4) Uani 1 d . . . H23 H 0.3702 -0.3204 0.3375 0.084 Uiso 1 calc R . . C24 C 0.2611(11) -0.2380(11) 0.4088(8) 0.065(4) Uani 1 d . . . H24 H 0.3113 -0.2518 0.4424 0.078 Uiso 1 calc R . . C25 C 0.1533(10) -0.1772(9) 0.4237(7) 0.051(3) Uani 1 d . . . H25 H 0.1296 -0.1504 0.4676 0.061 Uiso 1 calc R . . C26 C 0.0796(9) -0.1554(8) 0.3735(6) 0.040(2) Uani 1 d . . . H26 H 0.0063 -0.1118 0.3826 0.048 Uiso 1 calc R . . C27 C 0.0826(8) -0.2051(8) 0.1570(6) 0.043(3) Uani 1 d . . . C28 C 0.1433(10) -0.3053(9) 0.1524(7) 0.062(4) Uani 1 d . . . H28 H 0.1470 -0.3604 0.1978 0.075 Uiso 1 calc R . . C29 C 0.1989(14) -0.3234(12) 0.0796(9) 0.097(6) Uani 1 d . . . H29 H 0.2356 -0.3909 0.0755 0.116 Uiso 1 calc R . . C30 C 0.2002(12) -0.2434(14) 0.0146(9) 0.088(5) Uani 1 d . . . H30 H 0.2425 -0.2564 -0.0330 0.105 Uiso 1 calc R . . C31 C 0.1407(12) -0.1454(12) 0.0182(7) 0.071(4) Uani 1 d . . . H31 H 0.1392 -0.0911 -0.0276 0.085 Uiso 1 calc R . . C32 C 0.0811(10) -0.1242(9) 0.0901(7) 0.054(3) Uani 1 d . . . H32 H 0.0411 -0.0563 0.0926 0.064 Uiso 1 calc R . . C33 C -0.0373(8) -0.2832(7) 0.3050(6) 0.037(2) Uani 1 d . . . C34 C -0.0779(10) -0.3215(8) 0.2643(8) 0.055(3) Uani 1 d . . . H34 H -0.0787 -0.2949 0.2092 0.066 Uiso 1 calc R . . C35 C -0.1170(10) -0.3983(9) 0.3051(9) 0.060(3) Uani 1 d . . . H35 H -0.1403 -0.4265 0.2774 0.071 Uiso 1 calc R . . C36 C -0.1214(11) -0.4330(9) 0.3866(9) 0.066(4) Uani 1 d . . . H36 H -0.1495 -0.4837 0.4145 0.079 Uiso 1 calc R . . C37 C -0.0851(11) -0.3941(10) 0.4270(7) 0.062(3) Uani 1 d . . . H37 H -0.0890 -0.4174 0.4825 0.074 Uiso 1 calc R . . C38 C -0.0427(10) -0.3203(8) 0.3859(7) 0.051(3) Uani 1 d . . . H38 H -0.0169 -0.2949 0.4141 0.061 Uiso 1 calc R . . C39 C -0.5987(7) 0.1384(7) 0.2325(5) 0.029(2) Uani 1 d . . . C40 C -0.6629(8) 0.1475(8) 0.1788(6) 0.041(2) Uani 1 d . . . H40 H -0.6675 0.1969 0.1295 0.049 Uiso 1 calc R . . C41 C -0.7196(9) 0.0843(9) 0.1979(7) 0.051(3) Uani 1 d . . . H41 H -0.7603 0.0895 0.1609 0.061 Uiso 1 calc R . . C42 C -0.7165(10) 0.0124(10) 0.2726(8) 0.060(3) Uani 1 d . . . H42 H -0.7551 -0.0304 0.2859 0.072 Uiso 1 calc R . . C43 C -0.6549(9) 0.0058(9) 0.3268(7) 0.051(3) Uani 1 d . . . H43 H -0.6534 -0.0412 0.3772 0.061 Uiso 1 calc R . . C44 C -0.5955(8) 0.0680(7) 0.3074(6) 0.038(2) Uani 1 d . . . H44 H -0.5541 0.0624 0.3441 0.046 Uiso 1 calc R . . C45 C -0.5256(8) 0.2834(8) 0.1041(5) 0.036(2) Uani 1 d . . . C46 C -0.5805(10) 0.3895(8) 0.0769(7) 0.055(3) Uani 1 d . . . H46 H -0.6167 0.4283 0.1135 0.066 Uiso 1 calc R . . C47 C -0.5822(13) 0.4384(12) -0.0039(9) 0.081(5) Uani 1 d . . . H47 H -0.6204 0.5095 -0.0212 0.098 Uiso 1 calc R . . C48 C -0.5288(13) 0.3835(13) -0.0582(8) 0.078(5) Uani 1 d . . . H48 H -0.5321 0.4172 -0.1125 0.094 Uiso 1 calc R . . C49 C -0.4692(13) 0.2778(13) -0.0340(8) 0.081(4) Uani 1 d . . . H49 H -0.4296 0.2403 -0.0713 0.097 Uiso 1 calc R . . C50 C -0.4704(12) 0.2287(10) 0.0491(7) 0.068(4) Uani 1 d . . . H50 H -0.4328 0.1574 0.0666 0.082 Uiso 1 calc R . . C51 C -0.6026(8) 0.3164(7) 0.2633(5) 0.033(2) Uani 1 d . . . C52 C -0.7175(9) 0.3496(9) 0.2742(8) 0.057(3) Uani 1 d . . . H52 H -0.7515 0.3188 0.2576 0.068 Uiso 1 calc R . . C53 C -0.7791(9) 0.4274(9) 0.3094(8) 0.061(4) Uani 1 d . . . H53 H -0.8557 0.4507 0.3156 0.074 Uiso 1 calc R . . C54 C -0.7306(11) 0.4722(9) 0.3360(7) 0.058(3) Uani 1 d . . . H54 H -0.7740 0.5253 0.3601 0.069 Uiso 1 calc R . . C55 C -0.6193(11) 0.4385(10) 0.3271(7) 0.062(3) Uani 1 d . . . H55 H -0.5860 0.4678 0.3459 0.075 Uiso 1 calc R . . C56 C -0.5546(9) 0.3607(8) 0.2901(6) 0.047(3) Uani 1 d . . . H56 H -0.4781 0.3386 0.2836 0.056 Uiso 1 calc R . . C57 C -0.3394(8) -0.1150(7) 0.3401(6) 0.034(2) Uani 1 d . . . C58 C -0.3604(10) -0.2000(8) 0.3460(7) 0.053(3) Uani 1 d . . . H58 H -0.3489 -0.2213 0.3005 0.063 Uiso 1 calc R . . C59 C -0.3981(11) -0.2534(9) 0.4186(8) 0.070(4) Uani 1 d . . . H59 H -0.4127 -0.3099 0.4216 0.084 Uiso 1 calc R . . C60 C -0.4139(12) -0.2245(10) 0.4850(8) 0.071(4) Uani 1 d . . . H60 H -0.4395 -0.2610 0.5337 0.085 Uiso 1 calc R . . C61 C -0.3929(13) -0.1428(11) 0.4815(7) 0.075(4) Uani 1 d . . . H61 H -0.4038 -0.1236 0.5279 0.090 Uiso 1 calc R . . C62 C -0.3552(10) -0.0874(9) 0.4096(6) 0.050(3) Uani 1 d . . . H62 H -0.3405 -0.0315 0.4079 0.060 Uiso 1 calc R . . C63 C -0.3132(8) -0.0704(7) 0.1672(5) 0.034(2) Uani 1 d . . . C64 C -0.2295(9) -0.0840(8) 0.1025(6) 0.047(3) Uani 1 d . . . H64 H -0.1627 -0.0814 0.1037 0.056 Uiso 1 calc R . . C65 C -0.2476(11) -0.1016(10) 0.0357(7) 0.063(4) Uani 1 d . . . H65 H -0.1926 -0.1104 -0.0073 0.076 Uiso 1 calc R . . C66 C -0.3443(12) -0.1057(10) 0.0339(7) 0.065(4) Uani 1 d . . . H66 H -0.3548 -0.1183 -0.0102 0.078 Uiso 1 calc R . . C67 C -0.4278(11) -0.0915(10) 0.0964(8) 0.065(4) Uani 1 d . . . H67 H -0.4943 -0.0938 0.0939 0.078 Uiso 1 calc R . . C68 C -0.4131(9) -0.0740(8) 0.1623(6) 0.041(2) Uani 1 d . . . H68 H -0.4699 -0.0644 0.2042 0.049 Uiso 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 0.0264(2) 0.02844(19) 0.03157(19) -0.01185(15) -0.00373(15) -0.01029(15) Pt2 0.02107(18) 0.02591(18) 0.02918(19) -0.01155(14) -0.00308(14) -0.00620(14) Pt3 0.02065(18) 0.02536(18) 0.02493(18) -0.00846(13) -0.00350(13) -0.00652(14) I 0.0604(5) 0.0655(5) 0.0266(3) -0.0142(3) -0.0001(3) -0.0359(4) P1 0.0275(13) 0.0337(13) 0.0406(14) -0.0159(11) 0.0012(11) -0.0148(11) P2 0.0275(13) 0.0272(12) 0.0318(13) -0.0139(10) -0.0054(10) -0.0044(10) P3 0.0240(13) 0.0300(13) 0.0328(13) -0.0089(10) -0.0059(10) -0.0071(10) P4 0.0250(12) 0.0260(12) 0.0254(11) -0.0080(9) -0.0032(9) -0.0087(10) O1 0.030(4) 0.064(5) 0.099(7) -0.044(5) 0.021(4) -0.028(4) O2 0.057(5) 0.035(4) 0.042(4) 0.005(3) -0.017(4) -0.018(4) C1 0.025(5) 0.037(6) 0.058(7) -0.028(5) -0.007(5) -0.009(4) C2 0.025(5) 0.031(5) 0.021(4) -0.008(4) -0.002(4) -0.008(4) C3 0.033(6) 0.035(6) 0.047(6) -0.007(5) 0.004(5) -0.009(5) C4 0.084(10) 0.055(8) 0.049(7) -0.016(6) 0.013(7) -0.026(7) C5 0.128(16) 0.076(11) 0.067(10) -0.014(8) 0.045(11) -0.031(11) C6 0.073(12) 0.072(11) 0.096(14) 0.033(11) 0.042(11) -0.001(9) C7 0.047(9) 0.110(14) 0.122(15) 0.048(13) 0.014(10) -0.040(9) C8 0.046(8) 0.080(9) 0.071(9) 0.013(7) -0.014(6) -0.036(7) C9 0.036(6) 0.050(6) 0.040(6) -0.019(5) 0.004(5) -0.026(5) C10 0.030(6) 0.050(7) 0.053(7) -0.022(5) -0.010(5) -0.009(5) C11 0.047(7) 0.063(8) 0.054(7) -0.020(6) -0.018(6) -0.008(6) C12 0.051(8) 0.118(12) 0.041(7) -0.023(8) -0.005(6) -0.044(8) C13 0.086(11) 0.096(11) 0.064(9) -0.027(8) -0.002(8) -0.067(9) C14 0.074(9) 0.062(8) 0.064(8) -0.022(6) -0.011(7) -0.042(7) C15 0.031(6) 0.038(6) 0.065(7) -0.032(5) -0.009(5) -0.003(5) C16 0.068(9) 0.060(8) 0.086(10) -0.038(7) 0.033(8) -0.032(7) C17 0.054(9) 0.062(9) 0.127(14) -0.053(9) 0.041(9) -0.029(7) C18 0.041(8) 0.066(10) 0.149(16) -0.067(11) -0.004(9) -0.010(7) C19 0.068(10) 0.049(8) 0.107(12) -0.029(8) -0.049(9) 0.000(7) C20 0.049(7) 0.046(7) 0.074(8) -0.030(6) -0.029(6) 0.006(6) C21 0.027(5) 0.031(5) 0.029(5) -0.004(4) -0.004(4) -0.009(4) C22 0.039(7) 0.051(7) 0.065(8) -0.027(6) -0.015(6) -0.003(5) C23 0.039(7) 0.074(9) 0.105(11) -0.034(8) -0.032(7) -0.008(6) C24 0.057(9) 0.086(10) 0.076(9) -0.026(8) -0.035(7) -0.031(7) C25 0.060(8) 0.060(7) 0.044(6) -0.011(5) -0.012(6) -0.033(6) C26 0.036(6) 0.045(6) 0.041(6) -0.019(5) -0.003(5) -0.013(5) C27 0.034(6) 0.048(6) 0.036(6) -0.019(5) -0.003(5) 0.000(5) C28 0.065(8) 0.047(7) 0.050(7) -0.029(6) -0.009(6) 0.014(6) C29 0.125(15) 0.077(10) 0.054(9) -0.042(8) 0.001(9) 0.002(10) C30 0.072(10) 0.125(14) 0.059(9) -0.064(10) 0.017(8) -0.014(10) C31 0.086(11) 0.085(10) 0.041(7) -0.014(7) 0.001(7) -0.038(9) C32 0.058(8) 0.056(7) 0.042(6) -0.023(6) 0.006(6) -0.018(6) C33 0.032(5) 0.027(5) 0.059(7) -0.021(5) -0.011(5) -0.008(4) C34 0.067(8) 0.034(6) 0.064(8) -0.012(5) -0.030(6) -0.010(6) C35 0.058(8) 0.041(7) 0.096(11) -0.027(7) -0.030(7) -0.015(6) C36 0.063(9) 0.043(7) 0.096(11) -0.011(7) -0.014(8) -0.030(7) C37 0.082(10) 0.062(8) 0.044(7) -0.012(6) 0.008(6) -0.040(7) C38 0.066(8) 0.048(7) 0.050(7) -0.020(5) 0.001(6) -0.031(6) C39 0.018(5) 0.030(5) 0.041(5) -0.013(4) -0.001(4) -0.011(4) C40 0.038(6) 0.046(6) 0.043(6) -0.014(5) -0.005(5) -0.019(5) C41 0.039(7) 0.070(8) 0.062(8) -0.029(6) 0.001(5) -0.031(6) C42 0.048(8) 0.062(8) 0.073(9) -0.021(7) 0.012(6) -0.033(7) C43 0.039(7) 0.057(7) 0.046(6) -0.014(5) 0.015(5) -0.020(6) C44 0.027(5) 0.042(6) 0.040(6) -0.007(5) 0.000(4) -0.014(5) C45 0.037(6) 0.054(6) 0.027(5) -0.004(4) -0.011(4) -0.027(5) C46 0.058(8) 0.038(6) 0.049(7) 0.005(5) -0.016(6) -0.007(6) C47 0.092(12) 0.068(9) 0.056(9) 0.018(7) -0.018(8) -0.027(8) C48 0.093(12) 0.108(13) 0.045(8) 0.017(8) -0.035(8) -0.064(10) C49 0.103(12) 0.101(12) 0.038(7) -0.020(7) -0.013(7) -0.036(10) C50 0.085(10) 0.062(8) 0.042(7) -0.017(6) -0.005(7) -0.014(7) C51 0.025(5) 0.037(5) 0.029(5) -0.010(4) -0.002(4) -0.005(4) C52 0.033(6) 0.052(7) 0.090(9) -0.026(7) -0.003(6) -0.017(6) C53 0.028(6) 0.049(7) 0.093(10) -0.029(7) 0.015(6) -0.006(5) C54 0.059(8) 0.045(7) 0.056(7) -0.027(6) 0.016(6) -0.011(6) C55 0.063(9) 0.068(8) 0.060(8) -0.031(7) -0.003(7) -0.022(7) C56 0.041(6) 0.050(7) 0.051(7) -0.029(5) 0.003(5) -0.012(5) C57 0.027(5) 0.032(5) 0.034(5) -0.002(4) -0.004(4) -0.008(4) C58 0.067(8) 0.045(6) 0.044(6) -0.008(5) 0.010(6) -0.032(6) C59 0.084(10) 0.047(7) 0.069(9) -0.018(6) 0.027(8) -0.034(7) C60 0.082(10) 0.061(8) 0.053(8) -0.006(7) 0.023(7) -0.036(8) C61 0.106(12) 0.088(10) 0.027(6) -0.008(6) -0.006(7) -0.042(9) C62 0.073(8) 0.060(7) 0.030(6) -0.016(5) -0.008(5) -0.033(6) C63 0.041(6) 0.035(5) 0.026(5) -0.014(4) -0.007(4) -0.010(4) C64 0.045(7) 0.056(7) 0.036(6) -0.023(5) 0.002(5) -0.013(5) C65 0.069(9) 0.082(9) 0.034(6) -0.028(6) -0.008(6) -0.016(7) C66 0.077(10) 0.089(10) 0.053(8) -0.047(7) -0.018(7) -0.026(8) C67 0.066(9) 0.075(9) 0.074(9) -0.034(7) -0.027(7) -0.024(7) C68 0.039(6) 0.048(6) 0.048(6) -0.017(5) -0.011(5) -0.021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 C1 2.037(10) . ? Pt1 C2 2.082(9) . ? Pt1 P1 2.268(3) . ? Pt1 Pt2 2.6832(13) . ? Pt1 Pt3 2.694(2) . ? Pt1 I 2.8165(17) . ? Pt2 C1 2.074(10) . ? Pt2 P2 2.238(3) . ? Pt2 P4 2.279(3) . ? Pt2 Pt3 2.736(2) . ? Pt3 C2 2.052(9) . ? Pt3 P3 2.256(3) . ? Pt3 P4 2.273(2) . ? P1 C9 1.813(10) . ? P1 C3 1.819(10) . ? P1 C15 1.843(10) . ? P2 C27 1.835(10) . ? P2 C33 1.833(10) . ? P2 C21 1.839(9) . ? P3 C45 1.815(9) . ? P3 C39 1.824(9) . ? P3 C51 1.846(10) . ? P4 C57 1.808(9) . ? P4 C63 1.812(9) . ? O1 C1 1.150(11) . ? O2 C2 1.144(10) . ? C3 C4 1.372(16) . ? C3 C8 1.399(16) . ? C4 C5 1.390(18) . ? C5 C6 1.38(3) . ? C6 C7 1.35(3) . ? C7 C8 1.39(2) . ? C9 C10 1.380(14) . ? C9 C14 1.399(14) . ? C10 C11 1.388(14) . ? C11 C12 1.362(17) . ? C12 C13 1.355(19) . ? C13 C14 1.379(17) . ? C15 C20 1.382(16) . ? C15 C16 1.387(16) . ? C16 C17 1.397(18) . ? C17 C18 1.34(2) . ? C18 C19 1.40(2) . ? C19 C20 1.358(16) . ? C21 C22 1.381(14) . ? C21 C26 1.390(13) . ? C22 C23 1.366(15) . ? C23 C24 1.339(18) . ? C24 C25 1.357(17) . ? C25 C26 1.371(14) . ? C27 C32 1.372(15) . ? C27 C28 1.378(14) . ? C28 C29 1.385(17) . ? C29 C30 1.35(2) . ? C30 C31 1.344(19) . ? C31 C32 1.399(16) . ? C33 C38 1.358(14) . ? C33 C34 1.390(14) . ? C34 C35 1.375(16) . ? C35 C36 1.368(18) . ? C36 C37 1.352(17) . ? C37 C38 1.367(15) . ? C39 C44 1.386(13) . ? C39 C40 1.391(13) . ? C40 C41 1.371(14) . ? C41 C42 1.393(17) . ? C42 C43 1.388(17) . ? C43 C44 1.387(14) . ? C45 C50 1.363(15) . ? C45 C46 1.385(14) . ? C46 C47 1.379(17) . ? C47 C48 1.35(2) . ? C48 C49 1.39(2) . ? C49 C50 1.415(17) . ? C51 C56 1.362(14) . ? C51 C52 1.396(14) . ? C52 C53 1.357(16) . ? C53 C54 1.370(17) . ? C54 C55 1.352(17) . ? C55 C56 1.382(15) . ? C57 C62 1.386(13) . ? C57 C58 1.385(14) . ? C58 C59 1.377(15) . ? C59 C60 1.343(18) . ? C60 C61 1.349(18) . ? C61 C62 1.381(16) . ? C63 C68 1.405(13) . ? C63 C64 1.407(13) . ? C64 C65 1.412(15) . ? C65 C66 1.347(17) . ? C66 C67 1.380(18) . ? C67 C68 1.374(15) . ? 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 Pt1 C2 120.8(4) . . ? C1 Pt1 P1 100.2(3) . . ? C2 Pt1 P1 100.9(3) . . ? C1 Pt1 Pt2 49.9(3) . . ? C2 Pt1 Pt2 102.5(2) . . ? P1 Pt1 Pt2 148.92(7) . . ? C1 Pt1 Pt3 104.5(3) . . ? C2 Pt1 Pt3 48.8(3) . . ? P1 Pt1 Pt3 148.19(7) . . ? Pt2 Pt1 Pt3 61.17(4) . . ? C1 Pt1 I 128.8(3) . . ? C2 Pt1 I 100.8(2) . . ? P1 Pt1 I 99.72(8) . . ? Pt2 Pt1 I 95.68(4) . . ? Pt3 Pt1 I 80.11(5) . . ? C1 Pt2 P2 96.8(3) . . ? C1 Pt2 P4 153.2(3) . . ? P2 Pt2 P4 107.82(10) . . ? C1 Pt2 Pt1 48.7(3) . . ? P2 Pt2 Pt1 139.01(7) . . ? P4 Pt2 Pt1 111.26(7) . . ? C1 Pt2 Pt3 102.0(3) . . ? P2 Pt2 Pt3 160.76(7) . . ? P4 Pt2 Pt3 52.95(7) . . ? Pt1 Pt2 Pt3 59.62(4) . . ? C2 Pt3 P3 95.2(3) . . ? C2 Pt3 P4 152.1(3) . . ? P3 Pt3 P4 107.55(10) . . ? C2 Pt3 Pt1 49.8(2) . . ? P3 Pt3 Pt1 141.12(7) . . ? P4 Pt3 Pt1 111.06(8) . . ? C2 Pt3 Pt2 101.6(2) . . ? P3 Pt3 Pt2 159.33(7) . . ? P4 Pt3 Pt2 53.15(7) . . ? Pt1 Pt3 Pt2 59.21(5) . . ? C9 P1 C3 105.7(5) . . ? C9 P1 C15 104.3(5) . . ? C3 P1 C15 103.2(5) . . ? C9 P1 Pt1 113.6(3) . . ? C3 P1 Pt1 114.7(4) . . ? C15 P1 Pt1 114.2(3) . . ? C27 P2 C33 104.4(5) . . ? C27 P2 C21 104.8(5) . . ? C33 P2 C21 102.9(4) . . ? C27 P2 Pt2 115.9(3) . . ? C33 P2 Pt2 114.1(3) . . ? C21 P2 Pt2 113.4(3) . . ? C45 P3 C39 104.3(4) . . ? C45 P3 C51 105.8(5) . . ? C39 P3 C51 103.3(4) . . ? C45 P3 Pt3 108.6(3) . . ? C39 P3 Pt3 117.6(3) . . ? C51 P3 Pt3 116.1(3) . . ? C57 P4 C63 106.5(5) . . ? C57 P4 Pt3 120.8(3) . . ? C63 P4 Pt3 115.6(3) . . ? C57 P4 Pt2 119.5(3) . . ? C63 P4 Pt2 118.4(3) . . ? Pt3 P4 Pt2 73.90(8) . . ? O1 C1 Pt1 137.5(8) . . ? O1 C1 Pt2 140.8(8) . . ? Pt1 C1 Pt2 81.5(4) . . ? O2 C2 Pt3 145.2(8) . . ? O2 C2 Pt1 133.3(7) . . ? Pt3 C2 Pt1 81.3(3) . . ? C4 C3 C8 118.3(11) . . ? C4 C3 P1 119.2(9) . . ? C8 C3 P1 122.5(9) . . ? C3 C4 C5 121.7(15) . . ? C6 C5 C4 118.6(18) . . ? C7 C6 C5 121.3(15) . . ? C6 C7 C8 120.2(18) . . ? C7 C8 C3 120.0(16) . . ? C10 C9 C14 118.1(10) . . ? C10 C9 P1 119.4(8) . . ? C14 C9 P1 122.5(9) . . ? C9 C10 C11 120.3(10) . . ? C12 C11 C10 120.7(12) . . ? C13 C12 C11 119.6(12) . . ? C12 C13 C14 121.1(12) . . ? C13 C14 C9 120.0(12) . . ? C20 C15 C16 120.4(11) . . ? C20 C15 P1 121.1(9) . . ? C16 C15 P1 118.4(9) . . ? C15 C16 C17 117.1(13) . . ? C18 C17 C16 122.4(14) . . ? C17 C18 C19 120.2(13) . . ? C20 C19 C18 118.4(14) . . ? C19 C20 C15 121.5(13) . . ? C22 C21 C26 117.7(9) . . ? C22 C21 P2 124.6(8) . . ? C26 C21 P2 117.7(7) . . ? C23 C22 C21 120.6(11) . . ? C24 C23 C22 120.6(12) . . ? C23 C24 C25 120.9(11) . . ? C24 C25 C26 119.6(11) . . ? C25 C26 C21 120.6(10) . . ? C32 C27 C28 119.7(10) . . ? C32 C27 P2 118.3(8) . . ? C28 C27 P2 122.0(9) . . ? C27 C28 C29 119.7(12) . . ? C30 C29 C28 120.3(13) . . ? C31 C30 C29 120.4(12) . . ? C30 C31 C32 120.7(13) . . ? C27 C32 C31 119.1(11) . . ? C38 C33 C34 117.9(10) . . ? C38 C33 P2 121.6(8) . . ? C34 C33 P2 120.1(9) . . ? C35 C34 C33 120.5(11) . . ? C36 C35 C34 119.4(11) . . ? C37 C36 C35 120.5(12) . . ? C36 C37 C38 119.7(12) . . ? C33 C38 C37 121.9(11) . . ? C44 C39 C40 119.9(9) . . ? C44 C39 P3 117.2(7) . . ? C40 C39 P3 122.9(7) . . ? C41 C40 C39 120.5(10) . . ? C40 C41 C42 120.4(11) . . ? C43 C42 C41 118.8(11) . . ? C42 C43 C44 121.2(11) . . ? C39 C44 C43 119.2(10) . . ? C50 C45 C46 118.4(10) . . ? C50 C45 P3 119.3(9) . . ? C46 C45 P3 122.2(8) . . ? C47 C46 C45 120.9(13) . . ? C48 C47 C46 120.4(14) . . ? C47 C48 C49 120.8(12) . . ? C48 C49 C50 117.9(14) . . ? C45 C50 C49 121.5(13) . . ? C56 C51 C52 119.3(10) . . ? C56 C51 P3 120.5(7) . . ? C52 C51 P3 120.2(8) . . ? C53 C52 C51 119.3(11) . . ? C52 C53 C54 121.3(11) . . ? C55 C54 C53 119.5(11) . . ? C54 C55 C56 120.5(12) . . ? C51 C56 C55 120.2(11) . . ? C62 C57 C58 117.8(9) . . ? C62 C57 P4 117.4(8) . . ? C58 C57 P4 124.9(8) . . ? C59 C58 C57 120.6(11) . . ? C60 C59 C58 120.4(12) . . ? C59 C60 C61 120.4(12) . . ? C60 C61 C62 120.6(12) . . ? C61 C62 C57 120.1(11) . . ? C68 C63 C64 118.2(9) . . ? C68 C63 P4 123.2(7) . . ? C64 C63 P4 118.3(8) . . ? C63 C64 C65 119.6(11) . . ? C66 C65 C64 120.3(11) . . ? C65 C66 C67 121.0(11) . . ? C68 C67 C66 120.3(12) . . ? C67 C68 C63 120.7(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 3.154 _refine_diff_density_min -2.053 _refine_diff_density_rms 0.201 #=========================================================================== data_st-Pt2Mo-367 _database_code_CSD 158328 #=========================================================================== # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C56 H47 Mo O4 P3 Pt2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C56 H47 Mo O4 P3 Pt2' _chemical_formula_weight 1363.04 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C ? 0.002 0.002 International_Tables_Vol_IV_Table_2.3.1 H ? 0.000 0.000 International_Tables_Vol_IV_Table_2.3.1 Mo ? -1.825 0.688 International_Tables_Vol_IV_Table_2.3.1 O ? 0.008 0.006 International_Tables_Vol_IV_Table_2.3.1 P ? 0.090 0.095 International_Tables_Vol_IV_Table_2.3.1 Pt ? -2.352 8.388 International_Tables_Vol_IV_Table_2.3.1 #=========================================================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' -x,-y,-z _cell_length_a 12.053(1) _cell_length_b 13.690(1) _cell_length_c 17.292(3) _cell_angle_alpha 109.271(6) _cell_angle_beta 92.541(6) _cell_angle_gamma 106.169(6) _cell_volume 2557.5(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 20.1 _cell_measurement_theta_max 21.0 _cell_special_details ; ? ; _exptl_crystal_description prism _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.77 _exptl_crystal_density_method 'none' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 5.886 _exptl_absorpt_correction_type refdelf_(Walker_&_Stuart,_1983) _exptl_absorpt_correction_T_min 0.7104 _exptl_absorpt_correction_T_max 1.0000 #=========================================================================== # 7. EXPERIMENTAL DATA _diffrn_special_details ; ? ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.70930 _diffrn_radiation_type Mo-K\a _diffrn_source xray_tube _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Enraf_Nonius_CAD4 _diffrn_measurement_method \q/2\q _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 3 3 3 1 1 -9 1 2 2 _diffrn_reflns_number 8988 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_sigmaI/netI 0.333 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 24.92 _reflns_number_total 8988 _reflns_number_gt 7078 _reflns_threshold_expression >3.0\s(I) _computing_data_collection 'CAD4_(Enraf-Nonius,_1994)' _computing_cell_refinement CAD4_(Enraf-Nonius,_1994) _computing_data_reduction 'process_OpenMoleN_(_1997)' _computing_structure_solution Direct_methods_(SIR,_Burla_et_al.,_1989) _computing_structure_refinement LSFM_OpenMoleN_(_1997) _computing_molecular_graphics ? _computing_publication_material CIFGEN_IN_OpenMoleN_(_1997) #=========================================================================== # 8. REFINEMENT DATA _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_expression ? _refine_ls_extinction_coef ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 7078 _refine_ls_number_parameters 594 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.023 _refine_ls_wR_factor_all 0.566 _refine_ls_wR_factor_ref 0.034 _refine_ls_goodness_of_fit_all 18.454 _refine_ls_goodness_of_fit_ref 1.095 _refine_ls_shift/su_max 0.015 _refine_ls_shift/esd_mean 0.000 _refine_diff_density_max 1.050 _refine_diff_density_min -0.168 #=========================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom _atom_site_type_symbol PT1 -0.04286(1) 0.12704(1) 0.23470(1) 0.02940(7) 1.000 Uani ? ? Pt PT2 0.11637(1) 0.31065(1) 0.25559(1) 0.02873(7) 1.000 Uani ? ? Pt MO -0.07739(3) 0.23916(3) 0.13139(2) 0.0334(2) 1.000 Uani ? ? Mo P1 0.1279(1) 0.19697(9) 0.32485(7) 0.0339(5) 1.000 Uani ? ? P P2 0.2720(1) 0.46183(9) 0.28994(7) 0.0340(5) 1.000 Uani ? ? P P3 -0.1694(1) -0.03555(9) 0.22358(8) 0.0341(5) 1.000 Uani ? ? P O1 -0.0063(3) 0.4761(3) 0.2560(3) 0.056(2) 1.000 Uani ? ? O O2 -0.2790(3) 0.1683(3) 0.2256(3) 0.075(2) 1.000 Uani ? ? O O3 0.0957(3) 0.1009(3) 0.0887(2) 0.077(2) 1.000 Uani ? ? O C1 0.2471(4) 0.1388(4) 0.3200(3) 0.044(2) 1.000 Uani ? ? C C2 0.3355(5) 0.1719(5) 0.3849(4) 0.061(3) 1.000 Uani ? ? C C3 0.4323(5) 0.1355(5) 0.3736(4) 0.080(3) 1.000 Uani ? ? C C4 0.4415(5) 0.0679(5) 0.2999(5) 0.086(4) 1.000 Uani ? ? C C5 0.3536(6) 0.0320(5) 0.2346(5) 0.085(4) 1.000 Uani ? ? C C6 0.2556(5) 0.0672(4) 0.2433(4) 0.060(3) 1.000 Uani ? ? C C7 0.1130(4) 0.2396(4) 0.4339(3) 0.043(2) 1.000 Uani ? ? C C8 0.0961(7) 0.1662(5) 0.4748(4) 0.083(4) 1.000 Uani ? ? C C9 0.0764(7) 0.2003(6) 0.5581(4) 0.105(4) 1.000 Uani ? ? C C10 0.0746(6) 0.3063(7) 0.5971(4) 0.071(4) 1.000 Uani ? ? C C11 0.0911(6) 0.3750(6) 0.5566(4) 0.072(4) 1.000 Uani ? ? C C12 0.1108(5) 0.3441(5) 0.4763(3) 0.058(3) 1.000 Uani ? ? C C13 0.4150(4) 0.4419(4) 0.2748(3) 0.040(2) 1.000 Uani ? ? C C14 0.4247(5) 0.3384(4) 0.2469(3) 0.047(2) 1.000 Uani ? ? C C15 0.5339(5) 0.3229(5) 0.2355(3) 0.058(3) 1.000 Uani ? ? C C16 0.6296(5) 0.4104(5) 0.2521(4) 0.070(3) 1.000 Uani ? ? C C17 0.6223(5) 0.5142(6) 0.2783(4) 0.067(4) 1.000 Uani ? ? C C18 0.5139(5) 0.5302(5) 0.2910(4) 0.055(3) 1.000 Uani ? ? C C19 0.2717(4) 0.5560(4) 0.2355(3) 0.048(2) 1.000 Uani ? ? C C20 0.2264(5) 0.5121(5) 0.1518(3) 0.064(3) 1.000 Uani ? ? C C21 0.2297(6) 0.5802(5) 0.1066(4) 0.090(4) 1.000 Uani ? ? C C22 0.2766(6) 0.6899(5) 0.1435(4) 0.096(4) 1.000 Uani ? ? C C23 0.3221(6) 0.7341(5) 0.2252(5) 0.080(3) 1.000 Uani ? ? C C24 0.3189(5) 0.6679(4) 0.2723(4) 0.058(3) 1.000 Uani ? ? C C25 0.2890(4) 0.5443(4) 0.3993(3) 0.037(2) 1.000 Uani ? ? C C26 0.2036(5) 0.5936(4) 0.4260(3) 0.050(3) 1.000 Uani ? ? C C27 0.2061(5) 0.6462(5) 0.5104(4) 0.062(3) 1.000 Uani ? ? C C28 0.2914(6) 0.6504(5) 0.5671(4) 0.061(4) 1.000 Uani ? ? C C29 0.3738(6) 0.6005(6) 0.5414(4) 0.067(4) 1.000 Uani ? ? C C30 0.3738(5) 0.5474(5) 0.4575(3) 0.057(3) 1.000 Uani ? ? C C31 -0.1077(4) -0.1459(4) 0.2087(3) 0.044(2) 1.000 Uani ? ? C C32 0.0012(5) -0.1248(4) 0.2480(4) 0.055(3) 1.000 Uani ? ? C C33 0.0492(6) -0.2088(5) 0.2389(4) 0.079(3) 1.000 Uani ? ? C C34 -0.0113(6) -0.3130(4) 0.1934(4) 0.075(3) 1.000 Uani ? ? C C35 -0.1196(6) -0.3348(5) 0.1553(4) 0.069(3) 1.000 Uani ? ? C C36 -0.1700(5) -0.2536(4) 0.1613(4) 0.057(3) 1.000 Uani ? ? C C37 -0.2841(4) -0.0875(4) 0.1363(3) 0.037(2) 1.000 Uani ? ? C C38 -0.2510(5) -0.1045(5) 0.0583(3) 0.050(3) 1.000 Uani ? ? C C39 -0.3322(5) -0.1347(6) -0.0112(3) 0.059(4) 1.000 Uani ? ? C C40 -0.4476(6) -0.1478(7) -0.0034(4) 0.075(4) 1.000 Uani ? ? C C41 -0.4809(5) -0.1329(8) 0.0719(4) 0.076(4) 1.000 Uani ? ? C C42 -0.4000(5) -0.1033(6) 0.1413(4) 0.065(3) 1.000 Uani ? ? C C43 -0.2431(4) -0.0352(4) 0.3134(3) 0.041(2) 1.000 Uani ? ? C C44 -0.2279(6) 0.0614(5) 0.3757(3) 0.065(3) 1.000 Uani ? ? C C45 -0.2784(7) 0.0657(6) 0.4468(4) 0.090(4) 1.000 Uani ? ? C C46 -0.3457(7) -0.0276(6) 0.4548(4) 0.085(4) 1.000 Uani ? ? C C47 -0.3621(7) -0.1250(6) 0.3919(4) 0.093(4) 1.000 Uani ? ? C C48 -0.3102(6) -0.1284(5) 0.3223(4) 0.063(3) 1.000 Uani ? ? C C49 -0.0101(4) 0.3853(4) 0.2203(3) 0.043(2) 1.000 Uani ? ? C C50 -0.1904(4) 0.1850(4) 0.1991(3) 0.046(2) 1.000 Uani ? ? C C51 0.0370(4) 0.1523(4) 0.1182(3) 0.051(2) 1.000 Uani ? ? C C52 -0.0621(6) 0.2558(6) 0.0022(3) 0.088(4) 1.000 Uani ? ? C C53 -0.1042(7) 0.3353(5) 0.0478(4) 0.082(4) 1.000 Uani ? ? C C54 -0.2139(5) 0.2860(5) 0.0659(4) 0.079(3) 1.000 Uani ? ? C C55 -0.2349(6) 0.1734(6) 0.0286(4) 0.075(4) 1.000 Uani ? ? C C56 -0.1440(6) 0.1567(5) -0.0098(4) 0.076(3) 1.000 Uani ? ? C O4 0.427(1) 0.428(1) 0.9892(9) 0.170(7) 0.500 Uiso ? ? O O5 0.462(1) 0.514(1) 0.946(1) 0.180(7) 0.500 Uiso ? ? O H1 0.3303 0.2199 0.4377 0.0768 1.000 Uiso calc C2 H H2 0.4929 0.1591 0.4189 0.0984 1.000 Uiso calc C3 H H3 0.5089 0.0447 0.2928 0.1099 1.000 Uiso calc C4 H H4 0.3596 -0.0177 0.1828 0.1115 1.000 Uiso calc C5 H H5 0.1955 0.0429 0.1976 0.0763 1.000 Uiso calc C6 H H6 0.0977 0.0941 0.4473 0.1037 1.000 Uiso calc C8 H H7 0.0645 0.1512 0.5873 0.1282 1.000 Uiso calc C9 H H8 0.0615 0.3296 0.6531 0.1150 1.000 Uiso calc C10 H H9 0.0891 0.4470 0.5840 0.1042 1.000 Uiso calc C11 H H10 0.1232 0.3952 0.4489 0.0796 1.000 Uiso calc C12 H H11 0.3570 0.2772 0.2354 0.0603 1.000 Uiso calc C14 H H12 0.5405 0.2515 0.2164 0.0740 1.000 Uiso calc C15 H H13 0.7037 0.3998 0.2454 0.0902 1.000 Uiso calc C16 H H14 0.6902 0.5747 0.2877 0.0978 1.000 Uiso calc C17 H H15 0.5083 0.6019 0.3109 0.0816 1.000 Uiso calc C18 H H16 0.1930 0.4356 0.1252 0.0781 1.000 Uiso calc C20 H H17 0.1989 0.5495 0.0493 0.1054 1.000 Uiso calc C21 H H18 0.2775 0.7356 0.1123 0.1120 1.000 Uiso calc C22 H H19 0.3564 0.8107 0.2505 0.1037 1.000 Uiso calc C23 H H20 0.3492 0.6999 0.3297 0.0785 1.000 Uiso calc C24 H H21 0.1442 0.5912 0.3869 0.0698 1.000 Uiso calc C26 H H22 0.1479 0.6795 0.5287 0.0844 1.000 Uiso calc C27 H H23 0.2935 0.6880 0.6245 0.0899 1.000 Uiso calc C28 H H24 0.4318 0.6020 0.5813 0.0958 1.000 Uiso calc C29 H H25 0.4318 0.5135 0.4402 0.0755 1.000 Uiso calc C30 H H26 0.0448 -0.0524 0.2819 0.0705 1.000 Uiso calc C32 H H27 0.1264 -0.1922 0.2654 0.0942 1.000 Uiso calc C33 H H28 0.0219 -0.3698 0.1884 0.0884 1.000 Uiso calc C34 H H29 -0.1630 -0.4081 0.1232 0.0947 1.000 Uiso calc C35 H H30 -0.2465 -0.2713 0.1333 0.0830 1.000 Uiso calc C36 H H31 -0.1711 -0.0952 0.0525 0.0748 1.000 Uiso calc C38 H H32 -0.3080 -0.1462 -0.0642 0.0935 1.000 Uiso calc C39 H H33 -0.5036 -0.1674 -0.0507 0.1120 1.000 Uiso calc C40 H H34 -0.5610 -0.1428 0.0774 0.1288 1.000 Uiso calc C41 H H35 -0.4257 -0.0936 0.1937 0.0942 1.000 Uiso calc C42 H H36 -0.1819 0.1270 0.3704 0.0923 1.000 Uiso calc C44 H H37 -0.2660 0.1338 0.4900 0.1256 1.000 Uiso calc C45 H H38 -0.3808 -0.0251 0.5033 0.1065 1.000 Uiso calc C46 H H39 -0.4095 -0.1905 0.3965 0.1164 1.000 Uiso calc C47 H H40 -0.3211 -0.1966 0.2797 0.0895 1.000 Uiso calc C48 H H41 0.0107 0.2663 -0.0179 0.1095 1.000 Uiso calc C52 H H42 -0.0660 0.4114 0.0648 0.1114 1.000 Uiso calc C53 H H43 -0.2636 0.3217 0.0969 0.0990 1.000 Uiso calc C54 H H44 -0.3021 0.1183 0.0302 0.1035 1.000 Uiso calc C55 H H45 -0.1370 0.0875 -0.0404 0.1084 1.000 Uiso calc C56 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol PT1 0.02920(8) 0.02881(7) 0.03021(7) 0.00836(6) 0.00532(7) 0.01039(6) Pt PT2 0.02929(8) 0.02821(7) 0.02869(7) 0.00867(6) 0.00333(7) 0.01069(6) Pt MO 0.0315(2) 0.0395(2) 0.0300(2) 0.0143(1) 0.0032(1) 0.0127(1) Mo P1 0.0339(5) 0.0352(5) 0.0328(5) 0.0121(4) 0.0047(5) 0.0140(4) P P2 0.0331(5) 0.0302(5) 0.0394(5) 0.0082(4) 0.0023(5) 0.0133(4) P P3 0.0318(5) 0.0316(5) 0.0393(6) 0.0084(4) 0.0080(5) 0.0115(4) P O1 0.064(2) 0.036(2) 0.075(2) 0.022(1) -0.007(2) 0.008(2) O O2 0.051(2) 0.079(2) 0.102(2) 0.039(1) 0.046(2) 0.050(2) O O3 0.077(2) 0.104(2) 0.057(2) 0.064(2) 0.036(2) 0.032(2) O C1 0.039(2) 0.044(2) 0.051(2) 0.017(2) 0.011(2) 0.026(2) C C2 0.047(3) 0.075(3) 0.064(3) 0.021(2) 0.007(3) 0.035(2) C C3 0.049(3) 0.096(3) 0.108(4) 0.031(2) 0.006(3) 0.062(2) C C4 0.056(3) 0.082(3) 0.140(5) 0.045(2) 0.031(3) 0.049(3) C C5 0.074(4) 0.067(3) 0.122(5) 0.038(3) 0.031(4) 0.026(4) C C6 0.054(3) 0.051(3) 0.077(3) 0.026(2) 0.015(3) 0.021(2) C C7 0.037(2) 0.060(2) 0.035(2) 0.013(2) 0.004(2) 0.024(2) C C8 0.106(5) 0.093(4) 0.059(3) 0.034(3) 0.022(3) 0.046(2) C C9 0.110(5) 0.149(5) 0.071(3) 0.042(4) 0.032(3) 0.078(3) C C10 0.069(4) 0.136(6) 0.038(3) 0.016(4) 0.008(3) 0.016(4) C C11 0.083(4) 0.082(4) 0.054(3) 0.014(4) 0.026(3) 0.004(3) C C12 0.062(3) 0.062(3) 0.050(3) 0.011(3) 0.022(3) 0.013(3) C C13 0.033(2) 0.046(2) 0.042(2) 0.013(2) 0.006(2) 0.019(2) C C14 0.053(3) 0.049(2) 0.039(2) 0.019(2) 0.010(2) 0.015(2) C C15 0.057(3) 0.070(3) 0.049(3) 0.032(2) 0.019(2) 0.017(2) C C16 0.050(3) 0.112(4) 0.061(3) 0.042(2) 0.019(3) 0.036(3) C C17 0.035(3) 0.085(4) 0.104(4) 0.009(3) 0.011(3) 0.040(3) C C18 0.037(3) 0.047(3) 0.094(4) 0.003(2) 0.007(3) 0.020(3) C C19 0.038(2) 0.046(2) 0.064(3) 0.016(2) 0.012(2) 0.031(2) C C20 0.058(3) 0.066(3) 0.066(3) 0.017(2) 0.012(3) 0.039(2) C C21 0.088(4) 0.100(3) 0.084(3) 0.030(3) 0.021(3) 0.067(2) C C22 0.078(4) 0.098(3) 0.116(4) 0.025(3) 0.022(3) 0.082(2) C C23 0.059(3) 0.062(3) 0.142(4) 0.016(2) 0.024(3) 0.067(2) C C24 0.043(3) 0.050(2) 0.093(4) 0.009(2) 0.003(3) 0.037(2) C C25 0.038(2) 0.033(2) 0.040(2) 0.008(2) 0.003(2) 0.006(2) C C26 0.054(3) 0.051(3) 0.046(3) 0.019(2) -0.002(2) 0.004(2) C C27 0.073(3) 0.056(3) 0.060(3) 0.030(2) 0.011(3) 0.004(3) C C28 0.082(4) 0.058(3) 0.048(3) 0.017(3) 0.003(3) -0.001(3) C C29 0.079(4) 0.077(4) 0.049(3) 0.027(3) -0.011(3) 0.003(3) C C30 0.057(3) 0.064(3) 0.050(3) 0.027(2) -0.003(3) 0.011(2) C C31 0.043(2) 0.037(2) 0.051(2) 0.014(2) 0.019(2) 0.019(2) C C32 0.054(3) 0.044(2) 0.071(3) 0.019(2) 0.011(3) 0.024(2) C C33 0.073(3) 0.066(3) 0.102(4) 0.038(2) 0.029(3) 0.045(3) C C34 0.088(4) 0.058(2) 0.082(3) 0.042(2) 0.037(3) 0.036(2) C C35 0.091(4) 0.040(3) 0.088(4) 0.026(3) 0.032(3) 0.017(3) C C36 0.067(3) 0.034(2) 0.080(4) 0.014(2) 0.007(3) 0.009(3) C C37 0.038(2) 0.036(2) 0.039(2) 0.007(2) 0.006(2) 0.008(2) C C38 0.040(3) 0.073(3) 0.044(3) 0.002(3) 0.010(2) 0.013(2) C C39 0.053(3) 0.101(5) 0.039(3) 0.009(3) 0.010(3) 0.008(3) C C40 0.056(4) 0.123(6) 0.060(4) 0.013(4) -0.006(3) 0.022(4) C C41 0.043(3) 0.174(7) 0.059(4) 0.034(4) 0.007(3) 0.015(4) C C42 0.045(3) 0.118(5) 0.053(3) 0.033(3) 0.014(3) 0.021(3) C C43 0.040(2) 0.041(2) 0.042(2) 0.012(2) 0.012(2) 0.017(2) C C44 0.103(4) 0.049(3) 0.054(3) 0.014(3) 0.042(3) 0.015(2) C C45 0.142(6) 0.075(4) 0.068(3) 0.026(4) 0.060(3) 0.020(3) C C46 0.108(5) 0.087(4) 0.065(3) 0.033(4) 0.043(3) 0.038(3) C C47 0.109(5) 0.081(4) 0.092(3) 0.018(4) 0.053(3) 0.053(3) C C48 0.083(4) 0.050(3) 0.062(3) 0.005(3) 0.031(3) 0.015(3) C C49 0.047(3) 0.041(2) 0.041(2) 0.017(2) 0.001(2) 0.016(2) C C50 0.043(2) 0.051(2) 0.044(2) 0.025(2) 0.015(2) 0.019(2) C C51 0.046(2) 0.076(3) 0.038(2) 0.032(2) 0.010(2) 0.020(2) C C52 0.092(4) 0.137(4) 0.054(3) 0.047(3) 0.023(3) 0.060(2) C C53 0.121(5) 0.064(3) 0.071(3) 0.016(3) -0.026(3) 0.038(2) C C54 0.084(3) 0.116(3) 0.051(3) 0.073(2) 0.003(3) 0.025(3) C C55 0.062(4) 0.097(4) 0.070(3) 0.008(3) -0.027(3) 0.035(3) C C56 0.124(4) 0.094(3) 0.037(3) 0.065(3) -0.014(3) 0.007(3) C # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag PT1 PT2 2.6047(2) . . ? PT1 MO 2.7965(5) . . ? PT1 P1 2.284(1) . . ? PT1 P3 2.262(1) . . ? PT1 C50 2.277(5) . . ? PT1 C51 2.357(6) . . ? P1 C1 1.818(5) . . ? P1 C7 1.814(5) . . ? P2 C13 1.835(5) . . ? P2 C19 1.830(6) . . ? P2 C25 1.823(5) . . ? P3 C31 1.814(5) . . ? P3 C37 1.803(5) . . ? P3 C43 1.822(5) . . ? O1 C49 1.178(6) . . ? O2 C50 1.174(6) . . ? O3 C51 1.152(6) . . ? C1 C2 1.374(8) . . ? C1 C6 1.393(8) . . ? C2 C3 1.389(9) . . ? C3 C4 1.34(1) . . ? C4 C5 1.37(1) . . ? C5 C6 1.391(9) . . ? C7 C8 1.386(9) . . ? C7 C12 1.383(8) . . ? C8 C9 1.41(1) . . ? C9 C10 1.39(1) . . ? C10 C11 1.33(1) . . ? C11 C12 1.365(9) . . ? C13 C14 1.379(8) . . ? C13 C18 1.380(8) . . ? C14 C15 1.402(8) . . ? C15 C16 1.35(1) . . ? C16 C17 1.37(1) . . ? C17 C18 1.399(9) . . ? C19 C20 1.389(8) . . ? C19 C24 1.384(8) . . ? C20 C21 1.394(9) . . ? C21 C22 1.36(1) . . ? C22 C23 1.36(1) . . ? C23 C24 1.400(9) . . ? C25 C26 1.397(8) . . ? C25 C30 1.383(8) . . ? C26 C27 1.393(8) . . ? C27 C28 1.365(9) . . ? C28 C29 1.37(1) . . ? C29 C30 1.392(9) . . ? C31 C32 1.360(8) . . ? C31 C36 1.393(8) . . ? C32 C33 1.393(8) . . ? C33 C34 1.35(1) . . ? C34 C35 1.34(1) . . ? C35 C36 1.385(9) . . ? C37 C38 1.388(7) . . ? C37 C42 1.365(8) . . ? C38 C39 1.385(9) . . ? C39 C40 1.370(9) . . ? C40 C41 1.35(1) . . ? C41 C42 1.382(9) . . ? C43 C44 1.360(8) . . ? C43 C48 1.368(8) . . ? C44 C45 1.388(9) . . ? C45 C46 1.36(1) . . ? C46 C47 1.37(1) . . ? C47 C48 1.374(9) . . ? C52 C53 1.36(1) . . ? C52 C56 1.38(1) . . ? C53 C54 1.41(1) . . ? C54 C55 1.40(1) . . ? C55 C56 1.34(1) . . ? O4 O5 1.56(2) . . ? loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag ? ? ? ? ? ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag PT2 PT1 MO 62.68(1) . . . ? PT2 PT1 P1 55.21(3) . . . ? PT2 PT1 P3 174.82(4) . . . ? PT2 PT1 C50 93.1(1) . . . ? PT2 PT1 C51 61.6(2) . . . ? MO PT1 P1 117.76(3) . . . ? MO PT1 P3 122.32(4) . . . ? MO PT1 C50 44.5(1) . . . ? MO PT1 C51 45.5(1) . . . ? P1 PT1 P3 119.69(5) . . . ? P1 PT1 C50 138.2(1) . . . ? P1 PT1 C51 97.5(1) . . . ? P3 PT1 C50 91.8(2) . . . ? P3 PT1 C51 120.3(2) . . . ? C50 PT1 C51 87.6(2) . . . ? C1 P1 C7 103.4(3) . . . ? C13 P2 C19 100.9(2) . . . ? C13 P2 C25 104.7(2) . . . ? C19 P2 C25 104.7(3) . . . ? C31 P3 C37 103.7(3) . . . ? C31 P3 C43 102.8(2) . . . ? C37 P3 C43 105.7(2) . . . ? P1 C1 C2 123.3(5) . . . ? P1 C1 C6 117.3(4) . . . ? C2 C1 C6 118.9(5) . . . ? C1 C2 C3 120.4(7) . . . ? C2 C3 C4 120.9(7) . . . ? C3 C4 C5 119.9(7) . . . ? C4 C5 C6 120.8(7) . . . ? C1 C6 C5 119.0(7) . . . ? P1 C7 C8 120.5(5) . . . ? P1 C7 C12 120.5(4) . . . ? C8 C7 C12 118.8(6) . . . ? C7 C8 C9 118.9(8) . . . ? C8 C9 C10 119.5(8) . . . ? C9 C10 C11 120.4(7) . . . ? C10 C11 C12 121.2(8) . . . ? C7 C12 C11 121.2(7) . . . ? P2 C13 C14 120.3(4) . . . ? P2 C13 C18 120.4(4) . . . ? C14 C13 C18 119.3(5) . . . ? C13 C14 C15 120.5(6) . . . ? C14 C15 C16 119.3(6) . . . ? C15 C16 C17 121.5(6) . . . ? C16 C17 C18 119.3(7) . . . ? C13 C18 C17 120.1(6) . . . ? P2 C19 C20 118.0(4) . . . ? P2 C19 C24 123.6(5) . . . ? C20 C19 C24 118.4(6) . . . ? C19 C20 C21 120.2(7) . . . ? C20 C21 C22 120.8(8) . . . ? C21 C22 C23 119.9(7) . . . ? C22 C23 C24 120.7(7) . . . ? C19 C24 C23 120.1(7) . . . ? P2 C25 C26 118.1(4) . . . ? P2 C25 C30 122.1(4) . . . ? C26 C25 C30 119.2(5) . . . ? C25 C26 C27 119.6(6) . . . ? C26 C27 C28 120.6(6) . . . ? C27 C28 C29 120.0(6) . . . ? C28 C29 C30 120.7(6) . . . ? C25 C30 C29 119.8(6) . . . ? P3 C31 C32 119.5(4) . . . ? P3 C31 C36 122.4(5) . . . ? C32 C31 C36 118.0(5) . . . ? C31 C32 C33 120.4(6) . . . ? C32 C33 C34 121.5(7) . . . ? C33 C34 C35 118.4(6) . . . ? C34 C35 C36 122.0(7) . . . ? C31 C36 C35 119.6(6) . . . ? P3 C37 C38 117.4(4) . . . ? P3 C37 C42 125.2(4) . . . ? C38 C37 C42 117.2(5) . . . ? C37 C38 C39 121.2(6) . . . ? C38 C39 C40 119.9(6) . . . ? C39 C40 C41 119.4(7) . . . ? C40 C41 C42 120.8(7) . . . ? C37 C42 C41 121.5(6) . . . ? P3 C43 C44 118.8(4) . . . ? P3 C43 C48 122.9(4) . . . ? C44 C43 C48 118.3(5) . . . ? C43 C44 C45 121.1(7) . . . ? C44 C45 C46 120.1(7) . . . ? C45 C46 C47 119.0(7) . . . ? C46 C47 C48 120.4(7) . . . ? C43 C48 C47 121.2(6) . . . ? C53 C52 C56 107.9(8) . . . ? C52 C53 C54 108.5(8) . . . ? C53 C54 C55 105.8(7) . . . ? C54 C55 C56 108.5(8) . . . ? C52 C56 C55 109.4(7) . . . ?