# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/262 data_JFN-4 _audit_creation_date 1999-09-07T12:21:05-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[(CtBu)3P3Se3]' _chemical_formula_moiety 'C15 H27 P3 Se3' _chemical_formula_structural 'C15 H27 P3 Se3' _chemical_formula_sum 'C15 H27 P3 Se3' _chemical_formula_weight 537.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/N _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7751(3) _cell_length_b 16.2798(7) _cell_length_c 11.6992(3) _cell_angle_alpha 90 _cell_angle_beta 102.264(2) _cell_angle_gamma 90 _cell_volume 2005.40(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9479 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.779 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1056 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.734 _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 0.3897 _exptl_absorpt_correction_T_max 0.5386 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 16312 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.84 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.986 _reflns_number_total 5787 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0344P)^2^+1.1175P] 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_number_reflns 5787 _refine_ls_number_parameters 190 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.038 _refine_ls_wR_factor_ref 0.0901 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.641 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.102 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Se1 Se 0.06806(3) 0.146682(19) 0.90146(2) 0.03500(9) Uani 1 1 d . . . Se2 Se -0.05525(3) 0.136789(19) 0.49306(2) 0.03535(9) Uani 1 1 d . . . Se3 Se -0.25352(3) 0.26005(2) 0.65996(3) 0.04375(10) Uani 1 1 d . . . P1 P 0.09391(7) 0.09089(4) 0.65119(6) 0.02940(15) Uani 1 1 d . . . P2 P -0.07921(6) 0.20573(4) 0.65571(6) 0.02643(14) Uani 1 1 d . . . P3 P 0.18405(6) 0.23767(5) 0.82563(6) 0.03042(15) Uani 1 1 d . . . C1 C 0.0767(2) 0.26274(16) 0.6837(2) 0.0266(5) Uani 1 1 d . . . C2 C 0.1778(2) 0.19336(16) 0.6782(2) 0.0266(5) Uani 1 1 d . . . C3 C -0.0259(2) 0.11374(17) 0.7438(2) 0.0272(5) Uani 1 1 d . . . C4 C 0.0654(3) 0.35522(17) 0.6434(3) 0.0373(6) Uani 1 1 d . . . C5 C -0.0111(4) 0.3633(2) 0.5177(3) 0.0541(9) Uani 1 1 d . . . H5A H -0.0918 0.3365 0.5109 0.081 Uiso 1 1 calc R . . H5B H 0.0348 0.338 0.4651 0.081 Uiso 1 1 calc R . . H5C H -0.0244 0.4203 0.4982 0.081 Uiso 1 1 calc R . . C6 C 0.0010(4) 0.4023(2) 0.7295(4) 0.0582(9) Uani 1 1 d . . . H6A H -0.0804 0.3783 0.7292 0.087 Uiso 1 1 calc R . . H6B H -0.01 0.4588 0.7059 0.087 Uiso 1 1 calc R . . H6C H 0.0532 0.3992 0.8068 0.087 Uiso 1 1 calc R . . C7 C 0.1933(3) 0.3980(2) 0.6505(3) 0.0500(8) Uani 1 1 d . . . H7A H 0.2433 0.3936 0.7286 0.075 Uiso 1 1 calc R . . H7B H 0.1793 0.455 0.6303 0.075 Uiso 1 1 calc R . . H7C H 0.2376 0.3724 0.5969 0.075 Uiso 1 1 calc R . . C8 C 0.3015(3) 0.19341(19) 0.6266(2) 0.0348(6) Uani 1 1 d . . . C9 C 0.2699(3) 0.2115(3) 0.4950(3) 0.0517(9) Uani 1 1 d . . . H9A H 0.2311 0.2647 0.4817 0.078 Uiso 1 1 calc R . . H9B H 0.2123 0.1706 0.4555 0.078 Uiso 1 1 calc R . . H9C H 0.3465 0.2106 0.4655 0.078 Uiso 1 1 calc R . . C10 C 0.4060(3) 0.2525(2) 0.6898(3) 0.0512(9) Uani 1 1 d . . . H10A H 0.3746 0.3078 0.6822 0.077 Uiso 1 1 calc R . . H10B H 0.4791 0.2482 0.6555 0.077 Uiso 1 1 calc R . . H10C H 0.4292 0.2381 0.7712 0.077 Uiso 1 1 calc R . . C11 C 0.3638(3) 0.1082(2) 0.6455(4) 0.0554(9) Uani 1 1 d . . . H11A H 0.3045 0.0673 0.6086 0.083 Uiso 1 1 calc R . . H11B H 0.3881 0.097 0.7278 0.083 Uiso 1 1 calc R . . H11C H 0.4377 0.1071 0.612 0.083 Uiso 1 1 calc R . . C12 C -0.1205(3) 0.04254(19) 0.7576(3) 0.0372(6) Uani 1 1 d . . . C13 C -0.2014(3) 0.0676(2) 0.8453(3) 0.0493(8) Uani 1 1 d . . . H13A H -0.2506 0.1153 0.8169 0.074 Uiso 1 1 calc R . . H13B H -0.1468 0.0797 0.9195 0.074 Uiso 1 1 calc R . . H13C H -0.2573 0.0233 0.8544 0.074 Uiso 1 1 calc R . . C14 C -0.2116(3) 0.0184(2) 0.6434(3) 0.0520(9) Uani 1 1 d . . . H14A H -0.2621 0.0652 0.6124 0.078 Uiso 1 1 calc R . . H14B H -0.2662 -0.025 0.6584 0.078 Uiso 1 1 calc R . . H14C H -0.1637 0.0001 0.5878 0.078 Uiso 1 1 calc R . . C15 C -0.0430(4) -0.0341(2) 0.8036(3) 0.0547(9) Uani 1 1 d . . . H15A H 0.0075 -0.0503 0.749 0.082 Uiso 1 1 calc R . . H15B H -0.0996 -0.078 0.8128 0.082 Uiso 1 1 calc R . . H15C H 0.0116 -0.022 0.8778 0.082 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 Se1 0.03650(16) 0.04246(18) 0.02512(14) 0.00167(11) 0.00452(11) -0.00584(12) Se2 0.03829(16) 0.03973(17) 0.02605(14) -0.00628(11) 0.00236(11) -0.00265(12) Se3 0.02842(15) 0.0504(2) 0.05130(19) -0.00117(14) 0.00587(13) 0.01100(13) P1 0.0305(3) 0.0246(3) 0.0338(3) -0.0014(3) 0.0082(3) 0.0015(3) P2 0.0236(3) 0.0263(3) 0.0278(3) -0.0022(2) 0.0019(2) 0.0011(2) P3 0.0273(3) 0.0347(4) 0.0272(3) -0.0023(3) 0.0011(3) -0.0038(3) C1 0.0247(11) 0.0265(13) 0.0272(12) 0.0011(10) 0.0026(10) -0.0001(10) C2 0.0233(11) 0.0282(13) 0.0280(12) 0.0015(10) 0.0053(10) -0.0008(10) C3 0.0281(12) 0.0273(13) 0.0258(12) -0.0007(10) 0.0050(10) 0.0007(10) C4 0.0369(14) 0.0239(14) 0.0487(17) 0.0028(11) 0.0040(13) 0.0001(11) C5 0.060(2) 0.0365(18) 0.058(2) 0.0185(15) -0.0047(17) -0.0027(16) C6 0.057(2) 0.0286(17) 0.090(3) -0.0166(17) 0.018(2) 0.0010(15) C7 0.0507(19) 0.0321(17) 0.066(2) 0.0011(15) 0.0088(16) -0.0113(14) C8 0.0303(13) 0.0390(16) 0.0380(14) -0.0001(12) 0.0136(11) -0.0016(11) C9 0.0518(19) 0.068(3) 0.0411(17) 0.0033(16) 0.0230(15) -0.0096(17) C10 0.0297(15) 0.058(2) 0.067(2) -0.0066(17) 0.0125(15) -0.0097(14) C11 0.0373(17) 0.048(2) 0.086(3) 0.0041(19) 0.0240(17) 0.0120(15) C12 0.0393(15) 0.0335(16) 0.0399(15) -0.0005(12) 0.0113(12) -0.0093(12) C13 0.0462(17) 0.054(2) 0.0530(18) -0.0062(16) 0.0236(15) -0.0163(16) C14 0.0521(19) 0.051(2) 0.0526(19) -0.0099(16) 0.0106(16) -0.0283(16) C15 0.062(2) 0.0337(18) 0.071(2) 0.0137(16) 0.0203(18) -0.0032(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Se1 C3 1.980(2) . ? Se1 P3 2.2392(8) . ? Se2 P2 2.2707(7) . ? Se2 P1 2.3023(7) . ? Se3 P2 2.0862(7) . ? P1 C3 1.890(3) . ? P1 C2 1.892(3) . ? P1 P2 2.6494(10) . ? P2 C3 1.839(3) . ? P2 C1 1.886(3) . ? P3 C1 1.857(2) . ? P3 C2 1.858(3) . ? C1 C4 1.574(4) . ? C1 C2 1.580(4) . ? C2 C8 1.575(4) . ? C3 C12 1.574(4) . ? C4 C7 1.531(4) . ? C4 C5 1.532(5) . ? C4 C6 1.543(5) . ? C8 C9 1.533(4) . ? C8 C11 1.536(5) . ? C8 C10 1.545(4) . ? C12 C14 1.532(4) . ? C12 C15 1.534(5) . ? C12 C13 1.536(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Se1 P3 91.61(8) . . ? P2 Se2 P1 70.81(2) . . ? C3 P1 C2 95.24(12) . . ? C3 P1 Se2 87.22(8) . . ? C2 P1 Se2 94.31(8) . . ? C3 P1 P2 43.96(8) . . ? C2 P1 P2 71.83(8) . . ? Se2 P1 P2 54.04(2) . . ? C3 P2 C1 98.22(11) . . ? C3 P2 Se3 120.49(9) . . ? C1 P2 Se3 124.10(9) . . ? C3 P2 Se2 89.40(8) . . ? C1 P2 Se2 97.63(8) . . ? Se3 P2 Se2 119.52(3) . . ? C3 P2 P1 45.51(8) . . ? C1 P2 P1 75.27(8) . . ? Se3 P2 P1 160.20(4) . . ? Se2 P2 P1 55.15(2) . . ? C1 P3 C2 50.35(11) . . ? C1 P3 Se1 101.89(9) . . ? C2 P3 Se1 101.42(8) . . ? C4 C1 C2 133.0(2) . . ? C4 C1 P3 118.15(18) . . ? C2 C1 P3 64.88(13) . . ? C4 C1 P2 114.16(18) . . ? C2 C1 P2 103.75(17) . . ? P3 C1 P2 114.17(13) . . ? C8 C2 C1 131.4(2) . . ? C8 C2 P3 119.27(18) . . ? C1 C2 P3 64.77(13) . . ? C8 C2 P1 110.48(18) . . ? C1 C2 P1 109.14(16) . . ? P3 C2 P1 114.76(13) . . ? C12 C3 P2 121.67(19) . . ? C12 C3 P1 116.72(19) . . ? P2 C3 P1 90.53(12) . . ? C12 C3 Se1 108.54(17) . . ? P2 C3 Se1 109.78(13) . . ? P1 C3 Se1 108.11(12) . . ? C7 C4 C5 107.9(3) . . ? C7 C4 C6 105.3(3) . . ? C5 C4 C6 111.0(3) . . ? C7 C4 C1 114.1(2) . . ? C5 C4 C1 111.1(2) . . ? C6 C4 C1 107.3(3) . . ? C9 C8 C11 108.4(3) . . ? C9 C8 C10 110.2(3) . . ? C11 C8 C10 104.0(3) . . ? C9 C8 C2 111.1(2) . . ? C11 C8 C2 108.9(2) . . ? C10 C8 C2 114.0(2) . . ? C14 C12 C15 107.3(3) . . ? C14 C12 C13 107.5(3) . . ? C15 C12 C13 109.0(3) . . ? C14 C12 C3 114.1(2) . . ? C15 C12 C3 108.6(2) . . ? C13 C12 C3 110.2(2) . . ? #===END data_JFN-5 _audit_creation_date 2000-06-21T14:06:59-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic _publ_requested_category FO #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C15 H27 P3 Se4' _chemical_formula_weight 616.12 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.902(2) _cell_length_b 10.340(4) _cell_length_c 12.760(4) _cell_angle_alpha 69.17 _cell_angle_beta 71.11(2) _cell_angle_gamma 61.57 _cell_volume 1054.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.94 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.18 _exptl_absorpt_correction_T_min 0.1878 _exptl_absorpt_correction_T_max 0.3277 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_number 5081 _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.0436 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.97 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 5081 _reflns_number_gt 3999 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0394P)^2^+1.2458P] 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_number_reflns 5081 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0367 _refine_ls_wR_factor_ref 0.0868 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.088 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.152 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Se1 Se -0.17821(5) 1.33323(5) -0.00205(4) 0.02262(11) Uani 1 1 d . . . Se2 Se -0.33032(5) 1.18553(5) 0.08835(4) 0.02163(11) Uani 1 1 d . . . Se3 Se 0.04376(5) 0.98034(5) 0.14064(4) 0.01863(10) Uani 1 1 d . . . Se4 Se -0.19730(5) 1.23205(5) 0.41010(4) 0.02168(11) Uani 1 1 d . . . P1 P -0.11874(13) 1.33373(13) 0.15173(10) 0.0176(2) Uani 1 1 d . . . P2 P -0.31526(12) 1.14107(13) 0.26914(9) 0.0171(2) Uani 1 1 d . . . P3 P -0.00092(13) 1.03803(13) 0.34015(9) 0.0173(2) Uani 1 1 d . . . C1 C -0.2853(5) 1.3089(5) 0.2670(4) 0.0165(8) Uani 1 1 d . . . C2 C -0.1150(5) 0.9842(5) 0.2852(3) 0.0165(8) Uani 1 1 d . . . C3 C 0.0473(5) 1.1415(5) 0.1899(4) 0.0182(9) Uani 1 1 d . . . C4 C -0.4384(5) 1.4553(5) 0.2788(4) 0.0221(9) Uani 1 1 d . . . C5 C -0.5581(6) 1.4190(6) 0.3814(5) 0.0396(14) Uani 1 1 d . . . H5A H -0.5117 1.3706 0.4501 0.059 Uiso 1 1 calc R . . H5B H -0.5896 1.3501 0.3684 0.059 Uiso 1 1 calc R . . H5C H -0.6501 1.5129 0.3916 0.059 Uiso 1 1 calc R . . C6 C -0.4001(6) 1.5733(6) 0.2965(5) 0.0364(13) Uani 1 1 d . . . H6A H -0.3232 1.5975 0.2311 0.055 Uiso 1 1 calc R . . H6B H -0.357 1.5319 0.3663 0.055 Uiso 1 1 calc R . . H6C H -0.4957 1.6656 0.3033 0.055 Uiso 1 1 calc R . . C7 C -0.5153(6) 1.5305(6) 0.1735(5) 0.0318(12) Uani 1 1 d . . . H7A H -0.4407 1.555 0.1062 0.048 Uiso 1 1 calc R . . H7B H -0.6075 1.6237 0.1851 0.048 Uiso 1 1 calc R . . H7C H -0.547 1.4608 0.1619 0.048 Uiso 1 1 calc R . . C8 C -0.1263(5) 0.8300(5) 0.3513(4) 0.0230(9) Uani 1 1 d . . . C9 C -0.2182(6) 0.8422(6) 0.4720(4) 0.0354(12) Uani 1 1 d . . . H9A H -0.3219 0.9257 0.4678 0.053 Uiso 1 1 calc R . . H9B H -0.162 0.8616 0.5113 0.053 Uiso 1 1 calc R . . H9C H -0.2298 0.7471 0.5142 0.053 Uiso 1 1 calc R . . C10 C -0.2092(7) 0.7921(6) 0.2906(5) 0.0362(13) Uani 1 1 d . . . H10A H -0.1495 0.7845 0.2134 0.054 Uiso 1 1 calc R . . H10B H -0.3145 0.8723 0.2862 0.054 Uiso 1 1 calc R . . H10C H -0.2163 0.6952 0.3337 0.054 Uiso 1 1 calc R . . C11 C 0.0351(6) 0.6994(5) 0.3591(5) 0.0321(12) Uani 1 1 d . . . H11A H 0.0949 0.6908 0.282 0.048 Uiso 1 1 calc R . . H11B H 0.023 0.6046 0.4016 0.048 Uiso 1 1 calc R . . H11C H 0.0907 0.7191 0.3987 0.048 Uiso 1 1 calc R . . C12 C 0.2066(5) 1.1550(5) 0.1528(4) 0.0240(10) Uani 1 1 d . . . C13 C 0.2005(6) 1.2662(6) 0.2096(5) 0.0298(11) Uani 1 1 d . . . H13A H 0.1772 1.2301 0.2928 0.045 Uiso 1 1 calc R . . H13B H 0.1186 1.3664 0.1855 0.045 Uiso 1 1 calc R . . H13C H 0.3017 1.2732 0.1869 0.045 Uiso 1 1 calc R . . C14 C 0.2429(6) 1.2101(6) 0.0227(4) 0.0313(11) Uani 1 1 d . . . H14A H 0.2466 1.1384 -0.0129 0.047 Uiso 1 1 calc R . . H14B H 0.3443 1.217 -0.0004 0.047 Uiso 1 1 calc R . . H14C H 0.1612 1.3102 -0.0019 0.047 Uiso 1 1 calc R . . C15 C 0.3411(5) 1.0008(6) 0.1879(5) 0.0372(13) Uani 1 1 d . . . H15A H 0.3209 0.9627 0.271 0.056 Uiso 1 1 calc R . . H15B H 0.4397 1.0131 0.1639 0.056 Uiso 1 1 calc R . . H15C H 0.3483 0.9285 0.1512 0.056 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 Se1 0.0272(2) 0.0285(3) 0.0130(2) 0.00158(18) -0.00597(17) -0.0152(2) Se2 0.0241(2) 0.0292(2) 0.0176(2) -0.00406(18) -0.00746(17) -0.01443(19) Se3 0.0202(2) 0.0209(2) 0.0155(2) -0.00449(17) -0.00121(16) -0.01021(17) Se4 0.0231(2) 0.0289(2) 0.0151(2) -0.00722(18) -0.00517(17) -0.00985(19) P1 0.0200(5) 0.0191(5) 0.0161(5) -0.0017(4) -0.0041(4) -0.0112(4) P2 0.0171(5) 0.0217(6) 0.0148(5) -0.0029(4) -0.0025(4) -0.0112(4) P3 0.0175(5) 0.0213(6) 0.0139(5) -0.0011(4) -0.0043(4) -0.0100(4) C1 0.020(2) 0.017(2) 0.015(2) -0.0029(16) -0.0057(16) -0.0095(17) C2 0.019(2) 0.019(2) 0.013(2) -0.0027(16) -0.0022(16) -0.0099(17) C3 0.019(2) 0.020(2) 0.016(2) -0.0007(17) -0.0018(16) -0.0114(17) C4 0.023(2) 0.024(2) 0.020(2) -0.0099(19) -0.0023(18) -0.0078(18) C5 0.024(3) 0.034(3) 0.039(3) -0.008(2) 0.007(2) -0.004(2) C6 0.038(3) 0.030(3) 0.042(3) -0.013(2) -0.017(2) -0.005(2) C7 0.030(3) 0.024(3) 0.036(3) -0.012(2) -0.015(2) 0.001(2) C8 0.028(2) 0.018(2) 0.026(2) 0.0004(18) -0.0046(19) -0.0162(19) C9 0.041(3) 0.035(3) 0.026(3) 0.005(2) 0.000(2) -0.024(2) C10 0.044(3) 0.026(3) 0.050(4) -0.004(2) -0.019(3) -0.020(2) C11 0.037(3) 0.018(2) 0.040(3) 0.002(2) -0.013(2) -0.013(2) C12 0.020(2) 0.028(2) 0.025(2) -0.001(2) -0.0048(18) -0.0140(19) C13 0.028(2) 0.037(3) 0.035(3) -0.014(2) -0.001(2) -0.021(2) C14 0.027(2) 0.038(3) 0.029(3) -0.006(2) 0.004(2) -0.020(2) C15 0.016(2) 0.037(3) 0.051(3) 0.004(3) -0.009(2) -0.012(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Se1 P1 2.2260(13) . ? Se1 Se2 2.3966(9) . ? Se2 P2 2.2267(14) . ? Se3 C3 1.997(4) . ? Se3 C2 1.998(4) . ? Se3 P3 2.6705(14) . ? Se4 C1 2.016(4) . ? Se4 P3 2.2445(14) . ? P1 C1 1.874(4) . ? P1 C3 1.900(4) . ? P2 C1 1.885(4) . ? P2 C2 1.890(4) . ? P3 C2 1.862(4) . ? P3 C3 1.867(4) . ? C1 C4 1.562(6) . ? C2 C8 1.554(6) . ? C3 C12 1.552(6) . ? C4 C5 1.527(7) . ? C4 C7 1.531(6) . ? C4 C6 1.542(7) . ? C8 C9 1.529(7) . ? C8 C11 1.529(6) . ? C8 C10 1.537(7) . ? C12 C14 1.532(7) . ? C12 C13 1.534(7) . ? C12 C15 1.540(6) . ? 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 Se1 Se2 99.32(4) . . ? P2 Se2 Se1 99.16(4) . . ? C3 Se3 C2 79.51(17) . . ? C3 Se3 P3 44.28(12) . . ? C2 Se3 P3 44.14(12) . . ? C1 Se4 P3 89.22(13) . . ? C1 P1 C3 101.13(19) . . ? C1 P1 Se1 102.37(13) . . ? C3 P1 Se1 105.24(14) . . ? C1 P2 C2 100.99(19) . . ? C1 P2 Se2 102.24(13) . . ? C2 P2 Se2 105.05(14) . . ? C2 P3 C3 86.51(19) . . ? C2 P3 Se4 99.25(14) . . ? C3 P3 Se4 99.77(14) . . ? C2 P3 Se3 48.36(13) . . ? C3 P3 Se3 48.34(14) . . ? Se4 P3 Se3 127.27(5) . . ? C4 C1 P1 116.5(3) . . ? C4 C1 P2 114.9(3) . . ? P1 C1 P2 111.7(2) . . ? C4 C1 Se4 107.8(3) . . ? P1 C1 Se4 102.66(19) . . ? P2 C1 Se4 101.21(19) . . ? C8 C2 P3 115.7(3) . . ? C8 C2 P2 110.9(3) . . ? P3 C2 P2 111.6(2) . . ? C8 C2 Se3 115.3(3) . . ? P3 C2 Se3 87.49(17) . . ? P2 C2 Se3 114.0(2) . . ? C12 C3 P3 117.1(3) . . ? C12 C3 P1 111.0(3) . . ? P3 C3 P1 111.4(2) . . ? C12 C3 Se3 115.0(3) . . ? P3 C3 Se3 87.37(18) . . ? P1 C3 Se3 113.2(2) . . ? C5 C4 C7 107.8(4) . . ? C5 C4 C6 108.7(4) . . ? C7 C4 C6 106.9(4) . . ? C5 C4 C1 110.3(4) . . ? C7 C4 C1 113.7(4) . . ? C6 C4 C1 109.2(4) . . ? C9 C8 C11 108.9(4) . . ? C9 C8 C10 110.0(4) . . ? C11 C8 C10 107.3(4) . . ? C9 C8 C2 108.3(4) . . ? C11 C8 C2 112.0(4) . . ? C10 C8 C2 110.4(4) . . ? C14 C12 C13 110.0(4) . . ? C14 C12 C15 107.7(4) . . ? C13 C12 C15 108.2(4) . . ? C14 C12 C3 109.8(4) . . ? C13 C12 C3 109.7(4) . . ? C15 C12 C3 111.4(4) . . ? #===END data_JFN-7 _audit_creation_date 1999-09-04T12:10:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common sep699 _chemical_formula_moiety 'C18 H36 Cl2 P3 Pt1 Se4' _chemical_formula_structural 'C18 H36 CL2 P3 PT SE4' _chemical_formula_sum 'C18 H36 Cl2 P4 Pt Se4' _chemical_formula_weight 958.18 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall '-R 3' _symmetry_Int_Tables_number 148 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 34.5455(6) _cell_length_b 34.5455(6) _cell_length_c 16.7221(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 17282.4(5) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22280 _cell_measurement_theta_min 4.076 _cell_measurement_theta_max 30.034 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8136 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.756 _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 0.179 _exptl_absorpt_correction_T_max 0.227 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 41518 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0492 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.81 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _reflns_number_total 10989 _reflns_number_gt 7872 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'HELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0330P)^2^+94.1303P] 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 SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.000022(6) _refine_ls_number_reflns 10989 _refine_ls_number_parameters 263 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0386 _refine_ls_wR_factor_ref 0.095 _refine_ls_wR_factor_gt 0.0825 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.262 _refine_diff_density_min -1.155 _refine_diff_density_rms 0.126 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pt Pt 0.112291(6) 0.370850(6) 0.026890(10) 0.03742(7) Uani 1 1 d . . . Se1 Se 0.147335(16) 0.355443(17) -0.08667(3) 0.04238(12) Uani 1 1 d . . . Se2 Se 0.170411(18) 0.449586(18) 0.02420(3) 0.04965(13) Uani 1 1 d . . . Se3 Se 0.157186(16) 0.354820(18) 0.12182(3) 0.04364(12) Uani 1 1 d . . . Se4 Se 0.298026(18) 0.41990(2) 0.04388(3) 0.05690(15) Uani 1 1 d . . . Cl1 Cl 0.05567(5) 0.29295(5) 0.03383(8) 0.0566(3) Uani 1 1 d . . . Cl2 Cl 0.08017(5) 0.38492(5) 0.14454(8) 0.0558(3) Uani 1 1 d . . . P1 P 0.21218(4) 0.36481(5) -0.04192(7) 0.0418(3) Uani 1 1 d . . . P2 P 0.23374(4) 0.45260(5) 0.05948(8) 0.0482(3) Uani 1 1 d . . . P3 P 0.24547(5) 0.37693(6) 0.13194(8) 0.0546(4) Uani 1 1 d . . . P4 P 0.06561(5) 0.38147(5) -0.05793(8) 0.0495(3) Uani 1 1 d . . . C1 C 0.25119(16) 0.42503(18) -0.0186(3) 0.0460(11) Uani 1 1 d . . . C2 C 0.21659(16) 0.4109(2) 0.1425(3) 0.0499(13) Uani 1 1 d . . . C3 C 0.19902(17) 0.34014(18) 0.0608(3) 0.0441(11) Uani 1 1 d . . . C4 C 0.27472(19) 0.45554(19) -0.0945(3) 0.0541(13) Uani 1 1 d . . . C5 C 0.3140(3) 0.5001(2) -0.0699(5) 0.093(2) Uani 1 1 d . . . H5A H 0.3348 0.4952 -0.0396 0.139 Uiso 1 1 calc R . . H5B H 0.3036 0.516 -0.0377 0.139 Uiso 1 1 calc R . . H5C H 0.3286 0.5173 -0.1168 0.139 Uiso 1 1 calc R . . C6 C 0.2916(3) 0.4320(3) -0.1508(4) 0.089(2) Uani 1 1 d . . . H6A H 0.2669 0.4038 -0.1673 0.134 Uiso 1 1 calc R . . H6B H 0.3132 0.4271 -0.1234 0.134 Uiso 1 1 calc R . . H6C H 0.3052 0.4503 -0.197 0.134 Uiso 1 1 calc R . . C7 C 0.2421(2) 0.4652(3) -0.1421(4) 0.083(2) Uani 1 1 d . . . H7A H 0.2168 0.4374 -0.1589 0.124 Uiso 1 1 calc R . . H7B H 0.2571 0.4829 -0.1883 0.124 Uiso 1 1 calc R . . H7C H 0.2321 0.4811 -0.1088 0.124 Uiso 1 1 calc R . . C8 C 0.2216(2) 0.4319(2) 0.2272(3) 0.0657(17) Uani 1 1 d . . . C9 C 0.2722(2) 0.4629(3) 0.2421(4) 0.083(2) Uani 1 1 d . . . H9A H 0.2871 0.4458 0.2393 0.124 Uiso 1 1 calc R . . H9B H 0.2766 0.4762 0.2941 0.124 Uiso 1 1 calc R . . H9C H 0.2842 0.4859 0.2021 0.124 Uiso 1 1 calc R . . C10 C 0.1984(3) 0.4589(3) 0.2327(5) 0.103(3) Uani 1 1 d . . . H10A H 0.2101 0.4818 0.1925 0.155 Uiso 1 1 calc R . . H10B H 0.2034 0.4724 0.2847 0.155 Uiso 1 1 calc R . . H10C H 0.1669 0.4397 0.2244 0.155 Uiso 1 1 calc R . . C11 C 0.2026(3) 0.3948(3) 0.2913(4) 0.104(3) Uani 1 1 d . . . H11A H 0.2173 0.3776 0.2878 0.156 Uiso 1 1 calc R . . H11B H 0.1711 0.3757 0.2827 0.156 Uiso 1 1 calc R . . H11C H 0.2074 0.4082 0.3434 0.156 Uiso 1 1 calc R . . C12 C 0.1861(2) 0.2900(2) 0.0635(4) 0.0614(15) Uani 1 1 d . . . C13 C 0.2278(3) 0.2874(3) 0.0432(5) 0.084(2) Uani 1 1 d . . . H13A H 0.251 0.3047 0.0812 0.126 Uiso 1 1 calc R . . H13B H 0.2379 0.2991 -0.0096 0.126 Uiso 1 1 calc R . . H13C H 0.2209 0.2568 0.0451 0.126 Uiso 1 1 calc R . . C14 C 0.1492(3) 0.2622(2) 0.0033(4) 0.079(2) Uani 1 1 d . . . H14A H 0.1228 0.2635 0.0165 0.119 Uiso 1 1 calc R . . H14B H 0.1425 0.2317 0.0053 0.119 Uiso 1 1 calc R . . H14C H 0.1589 0.2739 -0.0495 0.119 Uiso 1 1 calc R . . C15 C 0.1705(3) 0.2700(3) 0.1469(4) 0.086(2) Uani 1 1 d . . . H15A H 0.144 0.2709 0.1608 0.129 Uiso 1 1 calc R . . H15B H 0.1936 0.287 0.1851 0.129 Uiso 1 1 calc R . . H15C H 0.1641 0.2396 0.1471 0.129 Uiso 1 1 calc R . . C16 C 0.0889(3) 0.4362(3) -0.0993(5) 0.106(3) Uani 1 1 d . . . H16A H 0.0993 0.4578 -0.0569 0.159 Uiso 1 1 calc R . . H16B H 0.0665 0.4384 -0.1296 0.159 Uiso 1 1 calc R . . H16C H 0.1135 0.4419 -0.1337 0.159 Uiso 1 1 calc R . . C17 C 0.0473(2) 0.3445(2) -0.1419(3) 0.0713(19) Uani 1 1 d . . . H17A H 0.0344 0.3142 -0.1235 0.107 Uiso 1 1 calc R . . H17B H 0.0724 0.3514 -0.1759 0.107 Uiso 1 1 calc R . . H17C H 0.0254 0.3479 -0.1714 0.107 Uiso 1 1 calc R . . C18 C 0.0154(3) 0.3715(4) -0.0080(4) 0.100(3) Uani 1 1 d . . . H18A H 0.023 0.3905 0.038 0.151 Uiso 1 1 calc R . . H18B H -0.0013 0.3408 0.0084 0.151 Uiso 1 1 calc R . . H18C H -0.0024 0.3779 -0.0439 0.151 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 Pt 0.03290(10) 0.04553(12) 0.03636(10) -0.00375(7) -0.00105(6) 0.02152(9) Se1 0.0409(3) 0.0532(3) 0.0354(2) -0.00575(19) -0.00091(18) 0.0253(2) Se2 0.0404(3) 0.0445(3) 0.0670(3) -0.0066(2) -0.0021(2) 0.0235(2) Se3 0.0393(3) 0.0612(3) 0.0348(2) 0.0006(2) 0.00108(18) 0.0284(2) Se4 0.0367(3) 0.0803(4) 0.0578(3) 0.0008(3) -0.0005(2) 0.0323(3) Cl1 0.0466(7) 0.0516(8) 0.0582(7) -0.0019(6) 0.0041(6) 0.0145(6) Cl2 0.0493(7) 0.0713(9) 0.0497(7) -0.0108(6) 0.0070(5) 0.0324(7) P1 0.0406(7) 0.0519(8) 0.0383(6) -0.0012(5) 0.0040(5) 0.0272(6) P2 0.0360(7) 0.0530(8) 0.0536(7) -0.0125(6) -0.0041(5) 0.0209(6) P3 0.0446(8) 0.0825(11) 0.0452(7) 0.0025(7) -0.0037(6) 0.0382(8) P4 0.0474(8) 0.0605(9) 0.0493(7) -0.0081(6) -0.0107(6) 0.0335(7) C1 0.038(3) 0.053(3) 0.047(3) -0.004(2) -0.003(2) 0.023(2) C2 0.034(3) 0.074(4) 0.043(3) -0.010(2) -0.0042(19) 0.029(3) C3 0.043(3) 0.056(3) 0.043(2) 0.007(2) 0.0040(19) 0.032(3) C4 0.046(3) 0.057(3) 0.054(3) 0.006(2) 0.006(2) 0.021(3) C5 0.076(5) 0.070(5) 0.089(5) 0.015(4) 0.000(4) 0.005(4) C6 0.090(5) 0.103(6) 0.078(5) 0.020(4) 0.044(4) 0.051(5) C7 0.074(5) 0.108(6) 0.065(4) 0.033(4) 0.010(3) 0.043(4) C8 0.050(3) 0.100(5) 0.045(3) -0.023(3) -0.010(2) 0.036(4) C9 0.066(4) 0.115(6) 0.063(4) -0.040(4) -0.025(3) 0.043(4) C10 0.076(5) 0.164(9) 0.085(5) -0.069(5) -0.022(4) 0.071(6) C11 0.089(6) 0.159(9) 0.045(4) -0.019(4) -0.006(3) 0.048(6) C12 0.069(4) 0.066(4) 0.066(4) 0.013(3) 0.010(3) 0.046(3) C13 0.099(6) 0.087(5) 0.105(5) 0.019(4) 0.021(4) 0.075(5) C14 0.093(5) 0.050(4) 0.098(5) -0.004(3) -0.006(4) 0.039(4) C15 0.109(6) 0.090(5) 0.079(5) 0.031(4) 0.022(4) 0.065(5) C16 0.128(7) 0.072(5) 0.111(6) 0.006(4) -0.058(5) 0.045(5) C17 0.074(4) 0.101(5) 0.057(3) -0.029(3) -0.031(3) 0.058(4) C18 0.082(5) 0.187(10) 0.074(4) -0.027(5) -0.018(4) 0.098(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pt P4 2.3103(13) . ? Pt Cl1 2.4120(14) . ? Pt Cl2 2.4241(12) . ? Pt Se2 2.4434(6) . ? Pt Se1 2.4493(5) . ? Pt Se3 2.4679(5) . ? Se1 P1 2.2266(13) . ? Se2 P2 2.2175(14) . ? Se3 C2 2.026(5) . ? Se3 C3 2.030(5) . ? Se3 P3 2.7540(15) . ? Se4 C1 2.007(5) . ? Se4 P3 2.2301(16) . ? P1 C1 1.869(5) . ? P1 C3 1.869(5) . ? P2 C2 1.872(6) . ? P2 C1 1.885(5) . ? P3 C3 1.889(5) . ? P3 C2 1.890(6) . ? P4 C16 1.784(8) . ? P4 C17 1.788(6) . ? P4 C18 1.797(7) . ? C1 C4 1.589(7) . ? C2 C8 1.560(7) . ? C3 C12 1.559(8) . ? C4 C5 1.513(9) . ? C4 C6 1.538(9) . ? C4 C7 1.546(9) . ? C8 C10 1.507(10) . ? C8 C11 1.542(11) . ? C8 C9 1.546(9) . ? C12 C13 1.527(8) . ? C12 C14 1.529(9) . ? C12 C15 1.529(8) . ? 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 P4 Pt Cl1 88.03(5) . . ? P4 Pt Cl2 92.33(5) . . ? Cl1 Pt Cl2 89.28(5) . . ? P4 Pt Se2 93.57(4) . . ? Cl1 Pt Se2 178.16(4) . . ? Cl2 Pt Se2 89.74(4) . . ? P4 Pt Se1 91.06(4) . . ? Cl1 Pt Se1 90.46(4) . . ? Cl2 Pt Se1 176.58(4) . . ? Se2 Pt Se1 90.418(18) . . ? P4 Pt Se3 175.77(4) . . ? Cl1 Pt Se3 88.21(4) . . ? Cl2 Pt Se3 85.70(4) . . ? Se2 Pt Se3 90.161(19) . . ? Se1 Pt Se3 90.891(17) . . ? P1 Se1 Pt 106.17(3) . . ? P2 Se2 Pt 106.84(4) . . ? C2 Se3 C3 79.5(2) . . ? C2 Se3 Pt 110.20(16) . . ? C3 Se3 Pt 109.78(13) . . ? C2 Se3 P3 43.32(16) . . ? C3 Se3 P3 43.29(15) . . ? Pt Se3 P3 135.27(4) . . ? C1 Se4 P3 88.79(15) . . ? C1 P1 C3 101.0(2) . . ? C1 P1 Se1 110.18(17) . . ? C3 P1 Se1 104.17(16) . . ? C2 P2 C1 100.5(2) . . ? C2 P2 Se2 103.67(16) . . ? C1 P2 Se2 110.44(16) . . ? C3 P3 C2 86.7(2) . . ? C3 P3 Se4 99.61(15) . . ? C2 P3 Se4 98.94(18) . . ? C3 P3 Se3 47.47(15) . . ? C2 P3 Se3 47.37(16) . . ? Se4 P3 Se3 124.34(6) . . ? C16 P4 C17 105.3(4) . . ? C16 P4 C18 105.3(5) . . ? C17 P4 C18 105.4(4) . . ? C16 P4 Pt 115.2(3) . . ? C17 P4 Pt 113.2(2) . . ? C18 P4 Pt 111.6(2) . . ? C4 C1 P1 114.7(3) . . ? C4 C1 P2 113.9(4) . . ? P1 C1 P2 118.2(3) . . ? C4 C1 Se4 107.9(3) . . ? P1 C1 Se4 100.1(2) . . ? P2 C1 Se4 99.2(2) . . ? C8 C2 P2 113.3(4) . . ? C8 C2 P3 113.8(4) . . ? P2 C2 P3 110.3(2) . . ? C8 C2 Se3 115.0(4) . . ? P2 C2 Se3 112.9(2) . . ? P3 C2 Se3 89.3(2) . . ? C12 C3 P1 113.8(4) . . ? C12 C3 P3 113.8(4) . . ? P1 C3 P3 109.9(3) . . ? C12 C3 Se3 114.8(3) . . ? P1 C3 Se3 112.9(2) . . ? P3 C3 Se3 89.2(2) . . ? C5 C4 C6 108.7(6) . . ? C5 C4 C7 107.5(6) . . ? C6 C4 C7 107.9(6) . . ? C5 C4 C1 111.0(5) . . ? C6 C4 C1 110.0(5) . . ? C7 C4 C1 111.6(4) . . ? C10 C8 C11 109.5(6) . . ? C10 C8 C9 109.1(6) . . ? C11 C8 C9 109.2(6) . . ? C10 C8 C2 112.0(5) . . ? C11 C8 C2 110.1(6) . . ? C9 C8 C2 107.0(4) . . ? C13 C12 C14 109.4(6) . . ? C13 C12 C15 107.9(5) . . ? C14 C12 C15 108.7(6) . . ? C13 C12 C3 107.7(5) . . ? C14 C12 C3 111.4(5) . . ? C15 C12 C3 111.7(5) . . ? #===END