# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_placncn _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis(\m-2-di-t-butylphosphido)-dicyano-tetracarbonyl-hexa-platinum(i) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H72 N2 O4 P4 Pt6' _chemical_formula_sum 'C38 H72 N2 O4 P4 Pt6' _chemical_formula_weight 1915.40 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' P P 0.1023 0.0942 '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 Tetragonal _symmetry_space_group_name_H-M 'I 41/a m d ' _symmetry_space_group_name_Hall '-I 4bd 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+1/4, x+3/4, z+1/4' 'y+1/4, -x+1/4, z+3/4' '-x+1/2, y, -z+1/2' 'x, -y, -z' 'y+1/4, x+3/4, -z+1/4' '-y+1/4, -x+1/4, -z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+3/4, x+5/4, z+3/4' 'y+3/4, -x+3/4, z+5/4' '-x+1, y+1/2, -z+1' 'x+1/2, -y+1/2, -z+1/2' 'y+3/4, x+5/4, -z+3/4' '-y+3/4, -x+3/4, -z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-1/4, -x-3/4, -z-1/4' '-y-1/4, x-1/4, -z-3/4' 'x-1/2, -y, z-1/2' '-x, y, z' '-y-1/4, -x-3/4, z-1/4' 'y-1/4, x-1/4, z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y+1/4, -x-1/4, -z+1/4' '-y+1/4, x+1/4, -z-1/4' 'x, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' '-y+1/4, -x-1/4, z+1/4' 'y+1/4, x+1/4, z-1/4' _cell_length_a 17.4421(8) _cell_length_b 17.4421(8) _cell_length_c 17.738(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5396.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 35 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 18.69 _exptl_crystal_description Square_bipyramid _exptl_crystal_colour Red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3496 _exptl_absorpt_coefficient_mu 15.647 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.0392 _exptl_absorpt_correction_T_max 0.0805 _exptl_absorpt_process_details XPREP-5.1/NT(Bruker_AXS) _exptl_special_details ; 182 data employed for parameter estimation, R(int) before correction 0.1601, R(int) after correction 0.0523 ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '2\q/\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.5(1) _diffrn_reflns_number 3527 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_av_sigmaI/netI 0.0600 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 26.50 _reflns_number_total 1500 _reflns_number_gt 1068 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _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 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0602P)^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 1500 _refine_ls_number_parameters 55 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1246 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 Pt1 Pt 0.5000 0.2500 -0.06879(5) 0.0401(3) Uani 1 4 d S . . Pt2 Pt 0.42339(4) 0.2500 0.06483(3) 0.0342(2) Uani 1 2 d S . . C2 C 0.5000 0.271(2) -0.1780(19) 0.049(12) Uani 0.50 2 d SP . . N N 0.5000 0.273(9) -0.244(2) 0.13(7) Uani 0.50 2 d SP . . C1 C 0.3388(13) 0.2500 0.1257(12) 0.053(5) Uani 1 2 d S . . O O 0.2856(12) 0.2500 0.1616(12) 0.086(6) Uani 1 2 d S . . P P 0.3707(3) 0.2500 -0.0510(2) 0.0387(11) Uani 1 2 d S . . C4A C 0.3161(11) 0.1580(11) -0.0759(11) 0.062(3) Uiso 0.56(2) 1 d PG A 1 C5A C 0.2490(14) 0.1411(19) -0.0255(14) 0.062(3) Uiso 0.56(2) 1 d PG A 1 H5A1 H 0.2663 0.1373 0.0257 0.094 Uiso 0.56(2) 1 calc PR A 1 H5A2 H 0.2258 0.0936 -0.0405 0.094 Uiso 0.56(2) 1 calc PR A 1 H5A3 H 0.2121 0.1817 -0.0296 0.094 Uiso 0.56(2) 1 calc PR A 1 C6A C 0.3763(13) 0.0930(17) -0.0714(16) 0.062(3) Uiso 0.56(2) 1 d PG A 1 H6A1 H 0.4186 0.1048 -0.1040 0.094 Uiso 0.56(2) 1 calc PR A 1 H6A2 H 0.3533 0.0456 -0.0870 0.094 Uiso 0.56(2) 1 calc PR A 1 H6A3 H 0.3942 0.0882 -0.0205 0.094 Uiso 0.56(2) 1 calc PR A 1 C7A C 0.2882(17) 0.1639(19) -0.1560(12) 0.062(3) Uiso 0.56(2) 1 d PG A 1 H7A1 H 0.3307 0.1748 -0.1887 0.094 Uiso 0.56(2) 1 calc PR A 1 H7A2 H 0.2511 0.2045 -0.1598 0.094 Uiso 0.56(2) 1 calc PR A 1 H7A3 H 0.2649 0.1164 -0.1707 0.094 Uiso 0.56(2) 1 calc PR A 1 C4B C 0.3107(14) 0.1625(14) -0.0790(14) 0.062(3) Uiso 0.44(2) 1 d PG A 2 C5B C 0.2280(16) 0.172(2) -0.0576(19) 0.062(3) Uiso 0.44(2) 1 d PG A 2 H5B1 H 0.2243 0.1839 -0.0049 0.094 Uiso 0.44(2) 1 calc PR A 2 H5B2 H 0.2010 0.1249 -0.0675 0.094 Uiso 0.44(2) 1 calc PR A 2 H5B3 H 0.2057 0.2125 -0.0867 0.094 Uiso 0.44(2) 1 calc PR A 2 C6B C 0.348(2) 0.096(2) -0.0337(18) 0.062(3) Uiso 0.44(2) 1 d PG A 2 H6B1 H 0.4009 0.0914 -0.0482 0.094 Uiso 0.44(2) 1 calc PR A 2 H6B2 H 0.3215 0.0494 -0.0441 0.094 Uiso 0.44(2) 1 calc PR A 2 H6B3 H 0.3450 0.1076 0.0192 0.094 Uiso 0.44(2) 1 calc PR A 2 C7B C 0.316(2) 0.143(3) -0.1616(13) 0.062(3) Uiso 0.44(2) 1 d PG A 2 H7B1 H 0.3683 0.1374 -0.1759 0.094 Uiso 0.44(2) 1 calc PR A 2 H7B2 H 0.2930 0.1842 -0.1905 0.094 Uiso 0.44(2) 1 calc PR A 2 H7B3 H 0.2884 0.0966 -0.1713 0.094 Uiso 0.44(2) 1 calc PR A 2 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 0.0398(5) 0.0557(7) 0.0247(4) 0.000 0.000 0.000 Pt2 0.0339(4) 0.0445(4) 0.0241(3) 0.000 -0.0013(3) 0.000 C2 0.07(3) 0.05(3) 0.027(14) 0.017(15) 0.000 0.000 N 0.12(4) 0.2(2) 0.037(17) 0.04(5) 0.000 0.000 C1 0.041(11) 0.075(16) 0.043(10) 0.000 0.009(10) 0.000 O 0.064(12) 0.121(19) 0.074(12) 0.000 0.020(11) 0.000 P 0.037(2) 0.052(3) 0.027(2) 0.000 -0.0041(19) 0.000 _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 C2 1.97(3) 10_554 ? Pt1 C2 1.97(3) . ? Pt1 P 2.277(5) 10_554 ? Pt1 P 2.277(5) . ? Pt1 Pt2 2.7210(11) 10_554 ? Pt1 Pt2 2.7210(11) . ? Pt2 C1 1.83(2) . ? Pt2 P 2.251(4) . ? Pt2 Pt2 2.6725(14) 10_554 ? Pt2 Pt2 2.8508(11) 20_656 ? Pt2 Pt2 2.8508(11) 27_565 ? C2 C2 0.72(8) 10_554 ? C2 N 1.17(5) . ? C2 N 1.40(10) 10_554 ? N N 0.8(3) 10_554 ? N C2 1.40(10) 10_554 ? C1 O 1.13(3) . ? P C4B 1.92(2) . ? P C4B 1.92(2) 29 ? P C4A 1.917(19) . ? P C4A 1.917(19) 29 ? C4A C5A 1.5012 . ? C4A C7A 1.5055 . ? C4A C6A 1.5479 . ? C5A H5A1 0.9600 . ? C5A H5A2 0.9600 . ? C5A H5A3 0.9600 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A H7A1 0.9600 . ? C7A H7A2 0.9600 . ? C7A H7A3 0.9600 . ? C4B C5B 1.5012 . ? C4B C7B 1.5053 . ? C4B C6B 1.5479 . ? C5B H5B1 0.9600 . ? C5B H5B2 0.9600 . ? C5B H5B3 0.9600 . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B H7B1 0.9600 . ? C7B H7B2 0.9600 . ? C7B H7B3 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Pt1 C2 21(2) 10_554 . ? C2 Pt1 P 97.82(11) 10_554 10_554 ? C2 Pt1 P 97.82(11) . 10_554 ? C2 Pt1 P 97.82(11) 10_554 . ? C2 Pt1 P 97.82(11) . . ? P Pt1 P 164.1(2) 10_554 . ? C2 Pt1 Pt2 148.9(4) 10_554 10_554 ? C2 Pt1 Pt2 148.9(4) . 10_554 ? P Pt1 Pt2 52.64(11) 10_554 10_554 ? P Pt1 Pt2 111.46(11) . 10_554 ? C2 Pt1 Pt2 148.9(4) 10_554 . ? C2 Pt1 Pt2 148.9(4) . . ? P Pt1 Pt2 111.46(11) 10_554 . ? P Pt1 Pt2 52.64(11) . . ? Pt2 Pt1 Pt2 58.82(4) 10_554 . ? C1 Pt2 P 102.1(7) . . ? C1 Pt2 Pt2 143.8(7) . 10_554 ? P Pt2 Pt2 114.10(13) . 10_554 ? C1 Pt2 Pt1 155.6(7) . . ? P Pt2 Pt1 53.51(13) . . ? Pt2 Pt2 Pt1 60.588(18) 10_554 . ? C1 Pt2 Pt2 86.4(6) . 20_656 ? P Pt2 Pt2 151.03(4) . 20_656 ? Pt2 Pt2 Pt2 62.048(13) 10_554 20_656 ? Pt1 Pt2 Pt2 114.96(3) . 20_656 ? C1 Pt2 Pt2 86.4(6) . 27_565 ? P Pt2 Pt2 151.03(4) . 27_565 ? Pt2 Pt2 Pt2 62.048(13) 10_554 27_565 ? Pt1 Pt2 Pt2 114.96(3) . 27_565 ? Pt2 Pt2 Pt2 55.90(3) 20_656 27_565 ? C2 C2 N 92(8) 10_554 . ? C2 C2 N 57(6) 10_554 10_554 ? N C2 N 35(10) . 10_554 ? C2 C2 Pt1 79.4(11) 10_554 . ? N C2 Pt1 172(9) . . ? N C2 Pt1 136(6) 10_554 . ? N N C2 88(8) 10_554 . ? N N C2 57(6) 10_554 10_554 ? C2 N C2 31(4) . 10_554 ? O C1 Pt2 178(2) . . ? C4B P C4B 105.7(15) . 29 ? C4B P C4A 4.0(11) . . ? C4B P C4A 109.6(9) 29 . ? C4B P C4A 109.6(9) . 29 ? C4B P C4A 4.0(11) 29 29 ? C4A P C4A 113.6(12) . 29 ? C4B P Pt2 117.3(7) . . ? C4B P Pt2 117.3(7) 29 . ? C4A P Pt2 114.4(6) . . ? C4A P Pt2 114.4(6) 29 . ? C4B P Pt1 120.3(8) . . ? C4B P Pt1 120.3(8) 29 . ? C4A P Pt1 117.4(6) . . ? C4A P Pt1 117.4(6) 29 . ? Pt2 P Pt1 73.85(15) . . ? C5A C4A C7A 108.9 . . ? C5A C4A C6A 110.7 . . ? C7A C4A C6A 108.5 . . ? C5A C4A P 114.5(15) . . ? C7A C4A P 108.7(15) . . ? C6A C4A P 105.3(14) . . ? C4A C5A H5A1 109.5 . . ? C4A C5A H5A2 109.5 . . ? H5A1 C5A H5A2 109.5 . . ? C4A C5A H5A3 109.5 . . ? H5A1 C5A H5A3 109.5 . . ? H5A2 C5A H5A3 109.5 . . ? C4A C6A H6A1 109.5 . . ? C4A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C4A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C4A C7A H7A1 109.5 . . ? C4A C7A H7A2 109.5 . . ? H7A1 C7A H7A2 109.5 . . ? C4A C7A H7A3 109.5 . . ? H7A1 C7A H7A3 109.5 . . ? H7A2 C7A H7A3 109.5 . . ? C5B C4B C7B 108.9 . . ? C5B C4B C6B 110.7 . . ? C7B C4B C6B 108.5 . . ? C5B C4B P 111.9(19) . . ? C7B C4B P 113(2) . . ? C6B C4B P 103.2(19) . . ? C4B C5B H5B1 109.5 . . ? C4B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C4B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? C4B C6B H6B1 109.5 . . ? C4B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C4B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C4B C7B H7B1 109.5 . . ? C4B C7B H7B2 109.5 . . ? H7B1 C7B H7B2 109.5 . . ? C4B C7B H7B3 109.5 . . ? H7B1 C7B H7B3 109.5 . . ? H7B2 C7B H7B3 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.823 _refine_diff_density_min -1.530 _refine_diff_density_rms 0.322 _database_code_depnum_ccdc_archive 'CCDC 924368' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_plascn_p _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H72 N2 O4 P4 Pt6 S2' _chemical_formula_sum 'C38 H72 N2 O4 P4 Pt6 S2' _chemical_formula_weight 1979.52 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' 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_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 17.091(2) _cell_length_b 17.091(2) _cell_length_c 17.632(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5150.3(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20481 _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 33.175 _exptl_crystal_description 'Square bipyramid' _exptl_crystal_colour 'Deep red' _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.553 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3624 _exptl_absorpt_coefficient_mu 16.477 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. R.H. Blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.0162 _exptl_absorpt_correction_T_max 0.0552 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.70087 _diffrn_radiation_type 'synchrotron radiation' _diffrn_radiation_source synchrotron _diffrn_source_type 'multiple wiggler' _diffrn_radiation_monochromator 'double crystal monochromator Si(111)' _diffrn_measurement_device_type '2-dimensional detector charge coupled device' _diffrn_measurement_method 'Phi scan - Rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 127106 _diffrn_reflns_av_R_equivalents 0.1343 _diffrn_reflns_av_sigmaI/netI 0.0636 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 33.18 _reflns_number_total 20481 _reflns_number_gt 19769 _reflns_threshold_expression >2\s(I) _computing_data_collection 'marCCD (marUSA)' _computing_cell_refinement ? _computing_data_reduction 'DENZO-SCALEPACK (Otwinoski & Minor, 1997), CCP4' _computing_structure_solution 'SIR92 (A. Altomare et al., J. Appl. Crystallogr. 1993, 26, 343-350.' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'WINGX (L. J. Farrugia, 1999)' _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^ > 2\s(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. Owing to the large Friedel coverage and the high value (0.49) of the Flack parameter a racemic twinnig has been hypothesized. The twinning by inversion was then introduced and the BASF factor refined to 0.486. ; _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^)+(0.0699P)^2^+8.3732P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(2) _refine_ls_number_reflns 20481 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.498327(8) 0.742806(10) 0.179585(13) 0.01722(4) Uani 1 1 d . . . Pt2 Pt 0.423381(11) 0.759499(11) 0.315003(10) 0.01535(4) Uani 1 1 d . . . Pt3 Pt 0.577815(11) 0.742079(11) 0.313048(10) 0.01558(4) Uani 1 1 d . . . Pt4 Pt 0.493829(12) 0.673663(10) 0.435893(10) 0.01547(4) Uani 1 1 d . . . Pt5 Pt 0.510392(12) 0.828495(10) 0.435404(10) 0.01538(4) Uani 1 1 d . . . Pt6 Pt 0.502585(9) 0.750735(6) 0.570502(13) 0.01749(5) Uani 1 1 d . . . C1 C 0.3390(4) 0.7724(3) 0.3790(3) 0.0220(9) Uani 1 1 d . . . O1 O 0.2868(3) 0.7808(3) 0.4191(3) 0.0322(10) Uani 1 1 d . . . C2 C 0.6650(3) 0.7326(3) 0.3747(3) 0.0208(9) Uani 1 1 d . . . O2 O 0.7185(3) 0.7247(3) 0.4129(3) 0.0311(10) Uani 1 1 d . . . C3 C 0.4866(4) 0.5873(3) 0.3722(3) 0.0222(10) Uani 1 1 d . . . O3 O 0.4829(3) 0.5341(3) 0.3336(3) 0.0288(9) Uani 1 1 d . . . C4 C 0.5217(4) 0.9144(3) 0.3722(3) 0.0240(10) Uani 1 1 d . . . O4 O 0.5283(4) 0.9681(3) 0.3338(3) 0.0331(11) Uani 1 1 d . . . S1 S 0.48056(9) 0.72791(12) 0.04842(7) 0.0357(3) Uani 1 1 d . . . C5 C 0.5567(5) 0.7651(5) 0.0033(4) 0.0445(15) Uani 1 1 d . . . N1 N 0.6075(5) 0.7907(6) -0.0342(4) 0.068(3) Uani 1 1 d . . . S2 S 0.51559(15) 0.76769(12) 0.70178(8) 0.0520(5) Uani 1 1 d . . . C6 C 0.4823(5) 0.6942(4) 0.7517(3) 0.0398(14) Uani 1 1 d . . . N2 N 0.4584(7) 0.6453(5) 0.7920(4) 0.079(3) Uani 1 1 d . . . P1 P 0.36682(9) 0.75478(8) 0.20026(8) 0.0175(2) Uani 1 1 d . . . C7 C 0.3008(3) 0.6685(3) 0.1833(3) 0.0211(9) Uani 1 1 d . . . C8 C 0.3333(4) 0.6016(3) 0.2333(3) 0.0312(11) Uani 1 1 d . . . H8A H 0.3316 0.6174 0.2867 0.047 Uiso 1 1 calc R . . H8B H 0.3875 0.5905 0.2188 0.047 Uiso 1 1 calc R . . H8C H 0.3014 0.5546 0.2262 0.047 Uiso 1 1 calc R . . C9 C 0.2164(3) 0.6847(4) 0.2083(3) 0.0304(10) Uani 1 1 d . . . H9A H 0.2160 0.7012 0.2615 0.046 Uiso 1 1 calc R . . H9B H 0.1851 0.6370 0.2027 0.046 Uiso 1 1 calc R . . H9C H 0.1941 0.7263 0.1767 0.046 Uiso 1 1 calc R . . C10 C 0.3040(4) 0.6434(4) 0.1012(3) 0.0318(12) Uani 1 1 d . . . H10A H 0.3585 0.6334 0.0867 0.048 Uiso 1 1 calc R . . H10B H 0.2825 0.6851 0.0691 0.048 Uiso 1 1 calc R . . H10C H 0.2732 0.5956 0.0944 0.048 Uiso 1 1 calc R . . C11 C 0.3210(4) 0.8489(3) 0.1682(3) 0.0222(10) Uani 1 1 d . . . C12 C 0.2586(4) 0.8768(4) 0.2236(3) 0.0291(11) Uani 1 1 d . . . H12A H 0.2155 0.8390 0.2248 0.044 Uiso 1 1 calc R . . H12B H 0.2388 0.9279 0.2073 0.044 Uiso 1 1 calc R . . H12C H 0.2814 0.8814 0.2744 0.044 Uiso 1 1 calc R . . C13 C 0.3874(3) 0.9087(3) 0.1683(3) 0.0277(10) Uani 1 1 d . . . H13A H 0.4285 0.8917 0.1332 0.041 Uiso 1 1 calc R . . H13B H 0.4091 0.9130 0.2196 0.041 Uiso 1 1 calc R . . H13C H 0.3671 0.9597 0.1522 0.041 Uiso 1 1 calc R . . C14 C 0.2883(4) 0.8424(4) 0.0881(3) 0.0290(11) Uani 1 1 d . . . H14A H 0.2455 0.8042 0.0874 0.044 Uiso 1 1 calc R . . H14B H 0.3298 0.8252 0.0535 0.044 Uiso 1 1 calc R . . H14C H 0.2686 0.8935 0.0718 0.044 Uiso 1 1 calc R . . P2 P 0.63107(8) 0.73846(8) 0.19627(8) 0.0174(2) Uani 1 1 d . . . C15 C 0.6834(4) 0.6448(4) 0.1745(3) 0.0250(11) Uani 1 1 d . . . C16 C 0.6934(4) 0.6336(4) 0.0900(4) 0.0348(14) Uani 1 1 d . . . H16A H 0.7258 0.6759 0.0696 0.052 Uiso 1 1 calc R . . H16B H 0.6420 0.6344 0.0654 0.052 Uiso 1 1 calc R . . H16C H 0.7188 0.5832 0.0803 0.052 Uiso 1 1 calc R . . C17 C 0.7624(5) 0.6419(5) 0.2142(4) 0.0428(18) Uani 1 1 d . . . H17A H 0.7550 0.6494 0.2688 0.064 Uiso 1 1 calc R . . H17B H 0.7960 0.6836 0.1943 0.064 Uiso 1 1 calc R . . H17C H 0.7870 0.5910 0.2050 0.064 Uiso 1 1 calc R . . C18 C 0.6323(5) 0.5797(3) 0.2056(5) 0.0467(19) Uani 1 1 d . . . H18A H 0.6254 0.5869 0.2603 0.070 Uiso 1 1 calc R . . H18B H 0.6573 0.5291 0.1959 0.070 Uiso 1 1 calc R . . H18C H 0.5811 0.5811 0.1805 0.070 Uiso 1 1 calc R . . C19 C 0.6930(4) 0.8277(3) 0.1750(3) 0.0232(10) Uani 1 1 d . . . C20 C 0.7417(4) 0.8198(4) 0.1034(4) 0.0400(15) Uani 1 1 d . . . H20A H 0.7075 0.8070 0.0605 0.060 Uiso 1 1 calc R . . H20B H 0.7803 0.7779 0.1101 0.060 Uiso 1 1 calc R . . H20C H 0.7688 0.8692 0.0933 0.060 Uiso 1 1 calc R . . C21 C 0.7447(4) 0.8480(4) 0.2424(3) 0.0367(13) Uani 1 1 d . . . H21A H 0.7122 0.8537 0.2879 0.055 Uiso 1 1 calc R . . H21B H 0.7722 0.8972 0.2324 0.055 Uiso 1 1 calc R . . H21C H 0.7829 0.8061 0.2505 0.055 Uiso 1 1 calc R . . C22 C 0.6339(4) 0.8947(3) 0.1636(3) 0.0339(12) Uani 1 1 d . . . H22A H 0.6002 0.8828 0.1202 0.051 Uiso 1 1 calc R . . H22B H 0.6621 0.9436 0.1542 0.051 Uiso 1 1 calc R . . H22C H 0.6017 0.9002 0.2094 0.051 Uiso 1 1 calc R . . P3 P 0.49027(8) 0.61854(8) 0.55203(8) 0.0165(2) Uani 1 1 d . . . C23 C 0.3951(3) 0.5689(3) 0.5724(3) 0.0191(8) Uani 1 1 d . . . C24 C 0.3953(5) 0.5255(4) 0.6489(4) 0.0315(13) Uani 1 1 d . . . H24A H 0.4100 0.5619 0.6894 0.047 Uiso 1 1 calc R . . H24B H 0.4331 0.4824 0.6470 0.047 Uiso 1 1 calc R . . H24C H 0.3430 0.5045 0.6590 0.047 Uiso 1 1 calc R . . C25 C 0.3340(4) 0.6358(4) 0.5755(4) 0.0290(12) Uani 1 1 d . . . H25A H 0.3482 0.6727 0.6159 0.044 Uiso 1 1 calc R . . H25B H 0.2821 0.6139 0.5859 0.044 Uiso 1 1 calc R . . H25C H 0.3331 0.6633 0.5267 0.044 Uiso 1 1 calc R . . C26 C 0.3718(4) 0.5122(4) 0.5099(4) 0.0284(11) Uani 1 1 d . . . H26A H 0.3716 0.5396 0.4611 0.043 Uiso 1 1 calc R . . H26B H 0.3194 0.4916 0.5203 0.043 Uiso 1 1 calc R . . H26C H 0.4094 0.4689 0.5081 0.043 Uiso 1 1 calc R . . C27 C 0.5774(4) 0.5545(4) 0.5734(3) 0.0238(10) Uani 1 1 d . . . C28 C 0.5927(5) 0.5556(4) 0.6586(4) 0.0304(13) Uani 1 1 d . . . H28A H 0.5481 0.5323 0.6852 0.046 Uiso 1 1 calc R . . H28B H 0.5998 0.6098 0.6756 0.046 Uiso 1 1 calc R . . H28C H 0.6401 0.5255 0.6698 0.046 Uiso 1 1 calc R . . C29 C 0.6473(4) 0.5923(5) 0.5332(5) 0.0340(14) Uani 1 1 d . . . H29A H 0.6384 0.5920 0.4783 0.051 Uiso 1 1 calc R . . H29B H 0.6949 0.5627 0.5449 0.051 Uiso 1 1 calc R . . H29C H 0.6534 0.6464 0.5508 0.051 Uiso 1 1 calc R . . C30 C 0.5655(5) 0.4704(4) 0.5437(4) 0.0323(13) Uani 1 1 d . . . H30A H 0.5561 0.4718 0.4889 0.048 Uiso 1 1 calc R . . H30B H 0.5204 0.4467 0.5692 0.048 Uiso 1 1 calc R . . H30C H 0.6124 0.4393 0.5542 0.048 Uiso 1 1 calc R . . P4 P 0.51591(8) 0.88252(8) 0.55148(7) 0.0163(2) Uani 1 1 d . . . C31 C 0.4313(4) 0.9490(4) 0.5760(3) 0.0240(10) Uani 1 1 d . . . C32 C 0.4171(5) 0.9474(5) 0.6613(4) 0.0331(14) Uani 1 1 d . . . H32A H 0.4626 0.9694 0.6876 0.050 Uiso 1 1 calc R . . H32B H 0.4091 0.8932 0.6779 0.050 Uiso 1 1 calc R . . H32C H 0.3706 0.9785 0.6734 0.050 Uiso 1 1 calc R . . C33 C 0.4462(4) 1.0330(4) 0.5484(4) 0.0311(13) Uani 1 1 d . . . H33A H 0.4550 1.0327 0.4935 0.047 Uiso 1 1 calc R . . H33B H 0.4924 1.0542 0.5740 0.047 Uiso 1 1 calc R . . H33C H 0.4006 1.0657 0.5601 0.047 Uiso 1 1 calc R . . C34 C 0.3600(4) 0.9138(5) 0.5358(5) 0.0390(17) Uani 1 1 d . . . H34A H 0.3685 0.9147 0.4809 0.059 Uiso 1 1 calc R . . H34B H 0.3134 0.9446 0.5483 0.059 Uiso 1 1 calc R . . H34C H 0.3527 0.8597 0.5527 0.059 Uiso 1 1 calc R . . C35 C 0.6123(3) 0.9270(3) 0.5749(3) 0.0198(9) Uani 1 1 d . . . C36 C 0.6142(4) 0.9606(4) 0.6553(4) 0.0307(12) Uani 1 1 d . . . H36A H 0.5984 0.9201 0.6916 0.046 Uiso 1 1 calc R . . H36B H 0.5781 1.0049 0.6587 0.046 Uiso 1 1 calc R . . H36C H 0.6674 0.9782 0.6672 0.046 Uiso 1 1 calc R . . C37 C 0.6724(4) 0.8589(4) 0.5705(4) 0.0268(11) Uani 1 1 d . . . H37A H 0.6576 0.8179 0.6066 0.040 Uiso 1 1 calc R . . H37B H 0.7246 0.8787 0.5830 0.040 Uiso 1 1 calc R . . H37C H 0.6727 0.8373 0.5190 0.040 Uiso 1 1 calc R . . C38 C 0.6373(4) 0.9893(4) 0.5178(3) 0.0268(11) Uani 1 1 d . . . H38A H 0.6357 0.9673 0.4665 0.040 Uiso 1 1 calc R . . H38B H 0.6906 1.0066 0.5294 0.040 Uiso 1 1 calc R . . H38C H 0.6015 1.0340 0.5209 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pt1 0.01829(9) 0.01936(7) 0.01402(8) -0.00053(5) 0.00048(5) 0.00032(6) Pt2 0.01739(8) 0.01634(8) 0.01232(7) -0.00013(6) -0.00026(6) 0.00023(5) Pt3 0.01749(8) 0.01658(8) 0.01266(7) 0.00024(5) 0.00059(6) 0.00004(5) Pt4 0.01911(8) 0.01447(7) 0.01284(7) 0.00081(5) 0.00027(6) -0.00038(5) Pt5 0.01944(8) 0.01435(7) 0.01236(7) -0.00016(5) -0.00010(6) -0.00038(5) Pt6 0.02321(10) 0.01584(9) 0.01343(9) 0.00080(3) -0.00004(4) -0.00165(7) C1 0.025(2) 0.022(2) 0.019(2) -0.0018(17) 0.0037(18) 0.0031(18) O1 0.026(2) 0.036(2) 0.035(2) -0.0035(19) 0.0142(18) -0.0009(17) C2 0.023(2) 0.022(2) 0.0165(19) 0.0005(17) 0.0000(17) 0.0033(19) O2 0.0239(19) 0.036(2) 0.033(2) 0.004(2) -0.0089(17) -0.0018(17) C3 0.030(3) 0.0164(18) 0.020(2) -0.0006(16) 0.0006(18) -0.0034(18) O3 0.041(3) 0.0202(17) 0.026(2) -0.0043(14) -0.0020(18) 0.0008(16) C4 0.038(3) 0.0148(19) 0.020(2) 0.0034(17) -0.002(2) -0.0048(19) O4 0.050(3) 0.0224(19) 0.027(2) 0.0074(16) -0.002(2) -0.0023(18) S1 0.0326(7) 0.0543(9) 0.0202(5) -0.0029(6) 0.0000(5) -0.0051(7) C5 0.047(4) 0.057(4) 0.029(3) -0.005(3) -0.006(3) -0.012(4) N1 0.061(5) 0.108(7) 0.036(3) 0.019(4) 0.002(3) -0.024(5) S2 0.0994(16) 0.0382(7) 0.0186(5) 0.0008(6) -0.0008(7) -0.0186(11) C6 0.056(4) 0.035(3) 0.028(2) 0.001(2) 0.001(3) -0.010(3) N2 0.141(9) 0.056(5) 0.040(3) 0.005(3) 0.009(5) -0.043(5) P1 0.0184(5) 0.0187(5) 0.0152(5) -0.0014(4) -0.0018(4) 0.0008(4) C7 0.026(2) 0.0198(19) 0.0174(19) -0.0040(17) -0.0010(17) -0.0042(17) C8 0.032(3) 0.023(2) 0.038(3) 0.001(2) -0.007(2) -0.0020(19) C9 0.025(2) 0.034(3) 0.032(3) -0.001(2) 0.0036(19) -0.005(2) C10 0.039(3) 0.036(3) 0.021(2) -0.009(2) -0.001(2) -0.009(2) C11 0.027(2) 0.023(2) 0.016(2) 0.0029(16) 0.0014(17) 0.0020(18) C12 0.030(3) 0.032(3) 0.026(2) -0.002(2) 0.000(2) 0.008(2) C13 0.031(2) 0.024(2) 0.028(2) 0.0025(18) -0.003(2) -0.0049(19) C14 0.031(3) 0.029(3) 0.027(2) 0.004(2) -0.005(2) -0.001(2) P2 0.0181(5) 0.0178(5) 0.0163(5) 0.0006(4) 0.0017(4) 0.0004(4) C15 0.029(3) 0.025(2) 0.021(2) -0.0043(19) -0.001(2) 0.0087(19) C16 0.047(4) 0.032(3) 0.025(2) -0.009(2) 0.004(2) 0.008(3) C17 0.043(4) 0.047(4) 0.039(3) -0.014(3) -0.012(3) 0.019(3) C18 0.065(5) 0.017(2) 0.058(4) 0.005(3) 0.023(4) 0.005(3) C19 0.031(2) 0.023(2) 0.0148(19) 0.0037(17) -0.0015(18) -0.0093(19) C20 0.051(4) 0.037(3) 0.032(3) 0.004(2) 0.015(3) -0.014(3) C21 0.041(3) 0.038(3) 0.031(3) 0.001(2) -0.004(2) -0.013(3) C22 0.045(3) 0.024(2) 0.033(3) 0.005(2) 0.003(2) 0.000(2) P3 0.0191(5) 0.0157(4) 0.0148(5) 0.0021(4) -0.0004(4) -0.0017(4) C23 0.021(2) 0.023(2) 0.0129(18) 0.0034(16) 0.0021(16) -0.0014(16) C24 0.041(3) 0.028(3) 0.026(3) 0.006(2) 0.007(2) -0.002(2) C25 0.019(2) 0.034(3) 0.033(3) -0.001(2) 0.005(2) 0.003(2) C26 0.028(3) 0.032(3) 0.026(3) -0.006(2) -0.001(2) -0.007(2) C27 0.026(2) 0.031(2) 0.015(2) 0.0028(18) -0.0016(18) 0.003(2) C28 0.041(3) 0.034(3) 0.017(2) 0.001(2) -0.009(2) 0.002(3) C29 0.022(2) 0.043(3) 0.037(3) 0.012(3) 0.005(2) -0.001(2) C30 0.036(3) 0.025(2) 0.036(3) -0.003(2) 0.000(3) 0.007(2) P4 0.0192(5) 0.0158(5) 0.0138(5) -0.0018(4) -0.0001(4) -0.0012(4) C31 0.027(2) 0.029(2) 0.016(2) -0.0046(18) 0.0036(18) -0.001(2) C32 0.039(3) 0.043(3) 0.017(2) -0.003(2) 0.007(2) 0.004(3) C33 0.034(3) 0.023(2) 0.036(3) -0.005(2) -0.001(2) 0.006(2) C34 0.024(3) 0.051(4) 0.041(4) -0.016(3) -0.006(3) 0.005(3) C35 0.021(2) 0.023(2) 0.015(2) -0.0038(16) 0.0004(16) 0.0008(16) C36 0.034(3) 0.033(3) 0.026(3) -0.006(2) -0.004(2) -0.003(2) C37 0.019(2) 0.032(3) 0.029(3) 0.001(2) -0.003(2) 0.0059(19) C38 0.029(3) 0.029(2) 0.022(2) 0.0025(19) -0.0012(19) -0.010(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. At the end of refinement high negative reasidual density peaks remain near to four Pt atoms in the difference Fourier map. It is probably the result of an oversized absorption correction. ; 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 P1 2.2862(15) . ? Pt1 P2 2.2889(15) . ? Pt1 S1 2.3463(14) . ? Pt1 Pt3 2.7172(5) . ? Pt1 Pt2 2.7246(5) . ? Pt2 C1 1.844(6) . ? Pt2 P1 2.2437(14) . ? Pt2 Pt3 2.6564(5) . ? Pt2 Pt5 2.8476(4) . ? Pt2 Pt4 2.8540(4) . ? Pt3 C2 1.852(6) . ? Pt3 P2 2.2521(14) . ? Pt3 Pt4 2.8494(4) . ? Pt3 Pt5 2.8572(4) . ? Pt4 C3 1.859(5) . ? Pt4 P3 2.2548(14) . ? Pt4 Pt5 2.6613(5) . ? Pt4 Pt6 2.7186(5) . ? Pt5 C4 1.854(5) . ? Pt5 P4 2.2472(14) . ? Pt5 Pt6 2.7310(5) . ? Pt6 P4 2.2886(14) . ? Pt6 P3 2.2924(13) . ? Pt6 S2 2.3433(15) . ? C1 O1 1.148(7) . ? C2 O2 1.143(7) . ? C3 O3 1.138(7) . ? C4 O4 1.146(7) . ? S1 C5 1.652(8) . ? C5 N1 1.176(10) . ? S2 C6 1.636(7) . ? C6 N2 1.171(9) . ? P1 C11 1.876(6) . ? P1 C7 1.881(5) . ? C7 C10 1.511(8) . ? C7 C9 1.535(8) . ? C7 C8 1.547(8) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.523(9) . ? C11 C14 1.523(8) . ? C11 C13 1.526(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? P2 C15 1.873(6) . ? P2 C19 1.894(6) . ? C15 C16 1.511(9) . ? C15 C18 1.517(10) . ? C15 C17 1.520(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.518(9) . ? C19 C21 1.521(8) . ? C19 C22 1.540(9) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? P3 C23 1.869(6) . ? P3 C27 1.886(6) . ? C23 C26 1.520(8) . ? C23 C24 1.540(8) . ? C23 C25 1.550(9) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.524(8) . ? C27 C29 1.532(9) . ? C27 C30 1.545(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? P4 C35 1.861(6) . ? P4 C31 1.890(6) . ? C31 C32 1.525(9) . ? C31 C34 1.531(10) . ? C31 C33 1.537(9) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C38 1.526(8) . ? C35 C36 1.530(8) . ? C35 C37 1.553(8) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Pt1 P2 163.11(6) . . ? P1 Pt1 S1 92.27(5) . . ? P2 Pt1 S1 104.56(5) . . ? P1 Pt1 Pt3 110.72(4) . . ? P2 Pt1 Pt3 52.63(4) . . ? S1 Pt1 Pt3 156.61(4) . . ? P1 Pt1 Pt2 52.31(4) . . ? P2 Pt1 Pt2 110.90(4) . . ? S1 Pt1 Pt2 144.52(4) . . ? Pt3 Pt1 Pt2 58.437(14) . . ? C1 Pt2 P1 102.65(19) . . ? C1 Pt2 Pt3 142.96(19) . . ? P1 Pt2 Pt3 114.36(4) . . ? C1 Pt2 Pt1 156.39(19) . . ? P1 Pt2 Pt1 53.74(4) . . ? Pt3 Pt2 Pt1 60.644(8) . . ? C1 Pt2 Pt5 84.41(19) . . ? P1 Pt2 Pt5 155.80(4) . . ? Pt3 Pt2 Pt5 62.431(9) . . ? Pt1 Pt2 Pt5 116.820(14) . . ? C1 Pt2 Pt4 86.25(18) . . ? P1 Pt2 Pt4 146.80(4) . . ? Pt3 Pt2 Pt4 62.154(8) . . ? Pt1 Pt2 Pt4 113.726(14) . . ? Pt5 Pt2 Pt4 55.650(12) . . ? C2 Pt3 P2 102.07(18) . . ? C2 Pt3 Pt2 143.31(17) . . ? P2 Pt3 Pt2 114.61(4) . . ? C2 Pt3 Pt1 155.67(17) . . ? P2 Pt3 Pt1 53.87(4) . . ? Pt2 Pt3 Pt1 60.919(9) . . ? C2 Pt3 Pt4 85.59(18) . . ? P2 Pt3 Pt4 152.54(4) . . ? Pt2 Pt3 Pt4 62.328(8) . . ? Pt1 Pt3 Pt4 114.100(14) . . ? C2 Pt3 Pt5 85.80(17) . . ? P2 Pt3 Pt5 150.17(4) . . ? Pt2 Pt3 Pt5 62.065(7) . . ? Pt1 Pt3 Pt5 116.738(13) . . ? Pt4 Pt3 Pt5 55.597(12) . . ? C3 Pt4 P3 102.41(17) . . ? C3 Pt4 Pt5 142.64(17) . . ? P3 Pt4 Pt5 114.92(3) . . ? C3 Pt4 Pt6 156.32(17) . . ? P3 Pt4 Pt6 53.92(4) . . ? Pt5 Pt4 Pt6 61.000(8) . . ? C3 Pt4 Pt3 84.27(18) . . ? P3 Pt4 Pt3 151.09(4) . . ? Pt5 Pt4 Pt3 62.349(7) . . ? Pt6 Pt4 Pt3 115.918(13) . . ? C3 Pt4 Pt2 85.94(18) . . ? P3 Pt4 Pt2 151.84(4) . . ? Pt5 Pt4 Pt2 62.053(8) . . ? Pt6 Pt4 Pt2 115.227(14) . . ? Pt3 Pt4 Pt2 55.518(12) . . ? C4 Pt5 P4 102.58(18) . . ? C4 Pt5 Pt4 143.20(18) . . ? P4 Pt5 Pt4 114.21(4) . . ? C4 Pt5 Pt6 156.22(18) . . ? P4 Pt5 Pt6 53.68(4) . . ? Pt4 Pt5 Pt6 60.535(8) . . ? C4 Pt5 Pt2 86.23(19) . . ? P4 Pt5 Pt2 150.58(4) . . ? Pt4 Pt5 Pt2 62.297(7) . . ? Pt6 Pt5 Pt2 115.038(13) . . ? C4 Pt5 Pt3 85.03(19) . . ? P4 Pt5 Pt3 152.02(4) . . ? Pt4 Pt5 Pt3 62.054(8) . . ? Pt6 Pt5 Pt3 115.262(14) . . ? Pt2 Pt5 Pt3 55.504(12) . . ? P4 Pt6 P3 163.40(6) . . ? P4 Pt6 S2 90.78(6) . . ? P3 Pt6 S2 105.72(6) . . ? P4 Pt6 Pt4 110.76(3) . . ? P3 Pt6 Pt4 52.65(3) . . ? S2 Pt6 Pt4 158.05(5) . . ? P4 Pt6 Pt5 52.29(3) . . ? P3 Pt6 Pt5 111.11(4) . . ? S2 Pt6 Pt5 142.82(5) . . ? Pt4 Pt6 Pt5 58.465(14) . . ? O1 C1 Pt2 179.6(6) . . ? O2 C2 Pt3 178.3(6) . . ? O3 C3 Pt4 179.3(6) . . ? O4 C4 Pt5 179.1(6) . . ? C5 S1 Pt1 109.4(2) . . ? N1 C5 S1 174.6(7) . . ? C6 S2 Pt6 113.8(2) . . ? N2 C6 S2 174.9(6) . . ? C11 P1 C7 112.0(3) . . ? C11 P1 Pt2 114.89(19) . . ? C7 P1 Pt2 115.46(19) . . ? C11 P1 Pt1 116.0(2) . . ? C7 P1 Pt1 119.60(19) . . ? Pt2 P1 Pt1 73.94(4) . . ? C10 C7 C9 111.1(5) . . ? C10 C7 C8 108.9(5) . . ? C9 C7 C8 107.9(5) . . ? C10 C7 P1 110.7(4) . . ? C9 C7 P1 112.1(4) . . ? C8 C7 P1 105.9(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 111.1(5) . . ? C12 C11 C13 108.0(5) . . ? C14 C11 C13 108.8(5) . . ? C12 C11 P1 111.5(4) . . ? C14 C11 P1 111.7(4) . . ? C13 C11 P1 105.3(4) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 P2 C19 112.4(3) . . ? C15 P2 Pt3 113.8(2) . . ? C19 P2 Pt3 112.64(19) . . ? C15 P2 Pt1 118.3(2) . . ? C19 P2 Pt1 120.2(2) . . ? Pt3 P2 Pt1 73.50(4) . . ? C16 C15 C18 109.1(6) . . ? C16 C15 C17 110.4(6) . . ? C18 C15 C17 108.7(6) . . ? C16 C15 P2 111.3(4) . . ? C18 C15 P2 106.1(4) . . ? C17 C15 P2 110.9(5) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 110.6(6) . . ? C20 C19 C22 108.6(5) . . ? C21 C19 C22 108.2(5) . . ? C20 C19 P2 113.5(4) . . ? C21 C19 P2 110.7(4) . . ? C22 C19 P2 104.9(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C23 P3 C27 112.7(3) . . ? C23 P3 Pt4 112.82(17) . . ? C27 P3 Pt4 113.75(19) . . ? C23 P3 Pt6 120.00(19) . . ? C27 P3 Pt6 118.1(2) . . ? Pt4 P3 Pt6 73.43(4) . . ? C26 C23 C24 109.2(5) . . ? C26 C23 C25 108.6(5) . . ? C24 C23 C25 109.0(5) . . ? C26 C23 P3 112.2(4) . . ? C24 C23 P3 112.7(4) . . ? C25 C23 P3 105.0(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 108.5(6) . . ? C28 C27 C30 111.6(5) . . ? C29 C27 C30 109.8(6) . . ? C28 C27 P3 109.0(5) . . ? C29 C27 P3 106.2(4) . . ? C30 C27 P3 111.6(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C35 P4 C31 112.4(3) . . ? C35 P4 Pt5 114.01(18) . . ? C31 P4 Pt5 115.04(19) . . ? C35 P4 Pt6 117.22(19) . . ? C31 P4 Pt6 118.8(2) . . ? Pt5 P4 Pt6 74.03(4) . . ? C32 C31 C34 108.8(6) . . ? C32 C31 C33 110.9(6) . . ? C34 C31 C33 110.6(6) . . ? C32 C31 P4 109.6(5) . . ? C34 C31 P4 105.5(4) . . ? C33 C31 P4 111.3(4) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C38 C35 C36 110.1(5) . . ? C38 C35 C37 107.7(5) . . ? C36 C35 C37 108.2(5) . . ? C38 C35 P4 112.7(4) . . ? C36 C35 P4 112.2(4) . . ? C37 C35 P4 105.6(4) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 33.18 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.671 _refine_diff_density_min -4.748 _refine_diff_density_rms 0.450 _database_code_depnum_ccdc_archive 'CCDC 924370' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_planco_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H72 N2 O6 P4 Pt6' _chemical_formula_sum 'C38 H72 N2 O6 P4 Pt6' _chemical_formula_weight 1947.40 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' P P 0.1023 0.0942 '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 Tetragonal _symmetry_space_group_name_H-M 'I -4 2 d' _symmetry_space_group_name_Hall 'I -4 2bw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' '-x+1/2, y, -z+3/4' 'x+1/2, -y, -z+3/4' '-y+1/2, -x, z+3/4' 'y+1/2, x, z+3/4' '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' '-x+1, y+1/2, -z+5/4' 'x+1, -y+1/2, -z+5/4' '-y+1, -x+1/2, z+5/4' 'y+1, x+1/2, z+5/4' _cell_length_a 17.2432(5) _cell_length_b 17.2432(5) _cell_length_c 17.7825(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5287.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9227 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 34.89 _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3560 _exptl_absorpt_coefficient_mu 15.975 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3448 _exptl_absorpt_correction_T_max 0.7469 _exptl_absorpt_process_details SADABS-2008/1_(Bruker_AXS) _exptl_special_details ; R(int) before correction 0.1362 R(int) after correction 0.0690 ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32255 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 35.23 _reflns_number_total 5861 _reflns_number_gt 4950 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^ > 2\s(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. In the refinement 5 restraints have been used in order to force the disordered isocyanato group to be almost linear. ; _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^)+(0.0325P)^2^+56.6171P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(6) _refine_ls_number_reflns 5861 _refine_ls_number_parameters 128 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pt1 Pt 0.0000 0.0000 0.191113(16) 0.03045(8) Uani 1 2 d SD . . Pt2 Pt 0.077371(13) -0.007435(15) 0.060269(11) 0.02381(6) Uani 1 1 d . . . C1 C 0.1620(5) -0.0164(5) -0.0030(4) 0.0367(17) Uani 1 1 d . . . O1 O 0.2149(4) -0.0219(6) -0.0396(4) 0.068(2) Uani 1 1 d . . . P P 0.13074(11) -0.00953(12) 0.17547(8) 0.0285(3) Uani 1 1 d . A . C2 C 0.1767(6) -0.1031(5) 0.2018(5) 0.044(2) Uani 1 1 d . . . C3 C 0.1136(7) -0.1643(6) 0.1970(8) 0.065(3) Uani 1 1 d . . . H3A H 0.0929 -0.1654 0.1469 0.098 Uiso 1 1 calc R . . H3B H 0.0730 -0.1521 0.2320 0.098 Uiso 1 1 calc R . . H3C H 0.1352 -0.2141 0.2090 0.098 Uiso 1 1 calc R . . C4 C 0.2413(8) -0.1264(9) 0.1495(8) 0.079(4) Uani 1 1 d . . . H4A H 0.2215 -0.1305 0.0992 0.118 Uiso 1 1 calc R . . H4B H 0.2618 -0.1757 0.1650 0.118 Uiso 1 1 calc R . . H4C H 0.2816 -0.0881 0.1511 0.118 Uiso 1 1 calc R . . C5 C 0.2054(10) -0.1019(9) 0.2845(8) 0.078(4) Uani 1 1 d . . . H5A H 0.2476 -0.0659 0.2892 0.116 Uiso 1 1 calc R . . H5B H 0.2226 -0.1528 0.2985 0.116 Uiso 1 1 calc R . . H5C H 0.1637 -0.0862 0.3168 0.116 Uiso 1 1 calc R . . C6 C 0.1913(5) 0.0766(6) 0.2001(5) 0.044(2) Uani 1 1 d . A 2 C7 C 0.1542(10) 0.1452(7) 0.1581(10) 0.096(6) Uani 1 1 d . A 2 H7A H 0.1010 0.1504 0.1732 0.144 Uiso 1 1 calc R A 2 H7B H 0.1567 0.1360 0.1049 0.144 Uiso 1 1 calc R A 2 H7C H 0.1818 0.1919 0.1700 0.144 Uiso 1 1 calc R A 2 C8 C 0.1905(10) 0.0897(10) 0.2842(8) 0.096(6) Uani 1 1 d . A 2 H8A H 0.1381 0.0977 0.3008 0.144 Uiso 1 1 calc R A 2 H8B H 0.2211 0.1346 0.2961 0.144 Uiso 1 1 calc R A 2 H8C H 0.2119 0.0452 0.3092 0.144 Uiso 1 1 calc R A 2 C9 C 0.2733(8) 0.0706(10) 0.1704(10) 0.096(5) Uani 1 1 d . A 2 H9A H 0.2998 0.0289 0.1953 0.144 Uiso 1 1 calc R A 2 H9B H 0.3002 0.1184 0.1798 0.144 Uiso 1 1 calc R A 2 H9C H 0.2720 0.0608 0.1173 0.144 Uiso 1 1 calc R A 2 N1 N 0.0000 0.0000 0.3101(4) 0.074(4) Uani 1 2 d SD . 2 C10 C -0.037(3) -0.020(3) 0.358(2) 0.201 Uiso 0.50 1 d PD . 2 O2 O -0.0772(17) -0.014(4) 0.4139(10) 0.28(2) Uiso 0.50 1 d PD B 2 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 0.03404(17) 0.04287(19) 0.01443(11) 0.000 0.000 0.00438(16) Pt2 0.02527(10) 0.03263(12) 0.01352(7) 0.00004(9) -0.00188(7) 0.00069(9) C1 0.032(3) 0.051(5) 0.026(3) -0.003(3) 0.001(3) 0.000(3) O1 0.037(3) 0.111(7) 0.056(4) -0.010(4) 0.015(3) 0.004(4) P 0.0339(8) 0.0347(9) 0.0167(5) -0.0011(6) -0.0048(5) 0.0013(7) C2 0.057(5) 0.046(4) 0.030(4) -0.003(3) -0.016(4) 0.009(4) C3 0.076(7) 0.038(5) 0.082(8) 0.007(6) -0.015(7) 0.012(5) C4 0.073(8) 0.084(9) 0.080(8) 0.007(7) 0.014(7) 0.043(7) C5 0.108(11) 0.078(9) 0.046(7) 0.018(6) -0.026(7) 0.023(8) C6 0.046(4) 0.048(5) 0.038(5) 0.002(4) -0.020(4) -0.008(4) C7 0.124(13) 0.040(6) 0.124(14) 0.000(7) -0.057(11) -0.012(7) C8 0.120(12) 0.115(12) 0.052(8) -0.042(8) -0.013(7) -0.048(10) C9 0.069(8) 0.109(12) 0.109(13) -0.036(10) 0.015(8) -0.038(8) N1 0.038(5) 0.158(14) 0.026(4) 0.000 0.000 0.003(8) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N1 2.115(8) . ? Pt1 P 2.2773(18) . ? Pt1 P 2.2773(18) 2 ? Pt1 Pt2 2.6851(3) 2 ? Pt1 Pt2 2.6851(3) . ? Pt2 C1 1.849(7) . ? Pt2 P 2.2460(15) . ? Pt2 Pt2 2.6805(5) 2 ? Pt2 Pt2 2.8613(4) 3 ? Pt2 Pt2 2.8613(4) 4 ? C1 O1 1.125(9) . ? P C2 1.857(9) . ? P C6 1.867(9) . ? C2 C4 1.505(15) . ? C2 C3 1.518(15) . ? C2 C5 1.551(15) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C9 1.513(17) . ? C6 C8 1.514(17) . ? C6 C7 1.538(15) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? N1 C10 1.109(18) 2 ? N1 C10 1.109(18) . ? C10 O2 1.225(18) . ? C10 C10 1.44(9) 2 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Pt1 P 97.02(4) . . ? N1 Pt1 P 97.02(4) . 2 ? P Pt1 P 165.97(7) . 2 ? N1 Pt1 Pt2 150.057(5) . 2 ? P Pt1 Pt2 112.92(4) . 2 ? P Pt1 Pt2 53.05(4) 2 2 ? N1 Pt1 Pt2 150.057(5) . . ? P Pt1 Pt2 53.05(4) . . ? P Pt1 Pt2 112.92(4) 2 . ? Pt2 Pt1 Pt2 59.886(11) 2 . ? C1 Pt2 P 103.3(2) . . ? C1 Pt2 Pt2 142.5(2) . 2 ? P Pt2 Pt2 114.16(5) . 2 ? C1 Pt2 Pt1 157.4(2) . . ? P Pt2 Pt1 54.13(5) . . ? Pt2 Pt2 Pt1 60.057(5) 2 . ? C1 Pt2 Pt2 85.0(2) . 3 ? P Pt2 Pt2 152.36(5) . 3 ? Pt2 Pt2 Pt2 62.069(4) 2 3 ? Pt1 Pt2 Pt2 114.540(9) . 3 ? C1 Pt2 Pt2 85.4(2) . 4 ? P Pt2 Pt2 149.79(5) . 4 ? Pt2 Pt2 Pt2 62.069(4) 2 4 ? Pt1 Pt2 Pt2 114.540(9) . 4 ? Pt2 Pt2 Pt2 55.862(9) 3 4 ? O1 C1 Pt2 177.8(7) . . ? C2 P C6 113.1(4) . . ? C2 P Pt2 114.8(3) . . ? C6 P Pt2 115.5(3) . . ? C2 P Pt1 117.0(3) . . ? C6 P Pt1 117.9(3) . . ? Pt2 P Pt1 72.82(5) . . ? C4 C2 C3 108.0(10) . . ? C4 C2 C5 110.6(10) . . ? C3 C2 C5 106.9(10) . . ? C4 C2 P 113.1(8) . . ? C3 C2 P 106.5(6) . . ? C5 C2 P 111.3(8) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C9 C6 C8 111.3(11) . . ? C9 C6 C7 105.7(12) . . ? C8 C6 C7 111.2(12) . . ? C9 C6 P 112.8(8) . . ? C8 C6 P 110.2(8) . . ? C7 C6 P 105.4(7) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 N1 C10 81(6) 2 . ? C10 N1 Pt1 140(3) 2 . ? C10 N1 Pt1 140(3) . . ? N1 C10 O2 158(5) . . ? N1 C10 C10 50(3) . 2 ? O2 C10 C10 118(3) . 2 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 35.23 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.604 _refine_diff_density_min -3.369 _refine_diff_density_rms 0.268 #===END _database_code_depnum_ccdc_archive 'CCDC 924371'