# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name "P. O'Brien" _publ_contact_author_address ; School of Chemistry The University of Manchester Oxford Road Manchester M13 9PL UNITED KINGDOM ; _publ_contact_author_email PAUL.OBRIEN@MANCHESTER.AC.UK _publ_section_title ; Metal complexes of bis(di-alkylselenophosphinyl)selenide [(R2PSe2)Se]: [M(R2PSe2)n] (M = ZnII, CdII, PbII, InIII, GaIII, CuI, , BiIII, NiII; R = iPr, Ph) and MoV2O2Se2(Se2PiPr2)2] ; loop_ _publ_author_name P.O'Brien 'Adekunle Adeogun' 'Mohammad Afzaal' 'Mohammad Afzaal' 'Chinh Q. Nguyen' # Attachment 'Mo-complex.cif' data_s2164m _database_code_depnum_ccdc_archive 'CCDC 282909' _publ_section_exptl_refinement ; The structure was solved by direct methods. The non-hydrogen atoms were refined anisotropically, except where the ADP becomes NPD or unrealistic. H atoms were included in calculated positions, except where they were largely indeterminate. ; # Insert blank lines between references _publ_section_references ; # # Put all your general crystallographic references here # Delete as required from the document CIF # Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 Mo2 O2 P2 Se6' _chemical_formula_weight 931.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5073(12) _cell_length_b 14.1178(15) _cell_length_c 16.0926(17) _cell_angle_alpha 90.00 _cell_angle_beta 97.671(2) _cell_angle_gamma 90.00 _cell_volume 2591.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used input _cell_measurement_theta_min 2.2925 _cell_measurement_theta_max 25.665 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 9.525 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.3291 _exptl_absorpt_correction_T_max 0.4493 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15944 _diffrn_reflns_av_R_equivalents 0.0889 _diffrn_reflns_av_sigmaI/netI 0.1470 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6046 _reflns_number_gt 3314 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6046 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1299 _refine_ls_wR_factor_gt 0.1190 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6567(10) 0.2846(9) 0.9046(7) 0.039(3) Uani 1 1 d . . . H1 H 0.5935 0.3334 0.8942 0.047 Uiso 1 1 calc R . . C2 C 0.6023(10) 0.1977(9) 0.9371(7) 0.041(3) Uani 1 1 d . . . H2A H 0.6621 0.1483 0.9488 0.062 Uiso 1 1 calc R . . H2B H 0.5393 0.1747 0.8950 0.062 Uiso 1 1 calc R . . H2C H 0.5702 0.2134 0.9888 0.062 Uiso 1 1 calc R . . C3 C 0.7533(11) 0.3266(8) 0.9667(8) 0.046(3) Uani 1 1 d . . . H3A H 0.7271 0.3300 1.0221 0.069 Uiso 1 1 calc R . . H3B H 0.7720 0.3904 0.9485 0.069 Uiso 1 1 calc R . . H3C H 0.8233 0.2865 0.9697 0.069 Uiso 1 1 calc R . . C4 C 0.7677(9) 0.3696(7) 0.7660(7) 0.032(3) Uani 1 1 d . . . H4 H 0.8290 0.3942 0.8106 0.038 Uiso 1 1 calc R . . C5 C 0.6698(10) 0.4433(8) 0.7508(9) 0.050(4) Uani 1 1 d . . . H5A H 0.7004 0.5012 0.7280 0.076 Uiso 1 1 calc R . . H5B H 0.6408 0.4579 0.8039 0.076 Uiso 1 1 calc R . . H5C H 0.6055 0.4181 0.7108 0.076 Uiso 1 1 calc R . . C6 C 0.8235(11) 0.3568(9) 0.6858(8) 0.050(3) Uani 1 1 d . . . H6A H 0.7681 0.3245 0.6435 0.075 Uiso 1 1 calc R . . H6B H 0.8949 0.3186 0.6979 0.075 Uiso 1 1 calc R . . H6C H 0.8434 0.4189 0.6644 0.075 Uiso 1 1 calc R . . C7 C 0.9172(10) -0.1835(8) 0.3914(7) 0.033(3) Uani 1 1 d . . . H7 H 0.9837 -0.2293 0.3925 0.039 Uiso 1 1 calc R . . C8 C 0.9703(11) -0.0877(9) 0.4079(7) 0.051(4) Uani 1 1 d . . . H8A H 1.0281 -0.0762 0.3694 0.077 Uiso 1 1 calc R . . H8B H 1.0090 -0.0845 0.4659 0.077 Uiso 1 1 calc R . . H8C H 0.9086 -0.0394 0.3991 0.077 Uiso 1 1 calc R . . C9 C 0.8469(12) -0.1909(10) 0.3063(7) 0.059(4) Uani 1 1 d . . . H9A H 0.7822 -0.1452 0.3018 0.088 Uiso 1 1 calc R . . H9B H 0.8153 -0.2551 0.2980 0.088 Uiso 1 1 calc R . . H9C H 0.8973 -0.1770 0.2633 0.088 Uiso 1 1 calc R . . C10 C 0.7934(10) -0.3470(7) 0.4550(7) 0.035(3) Uani 1 1 d . . . H10 H 0.7571 -0.3545 0.3954 0.042 Uiso 1 1 calc R . . C11 C 0.9056(10) -0.4079(8) 0.4674(8) 0.045(3) Uani 1 1 d . . . H11A H 0.9389 -0.4074 0.5267 0.067 Uiso 1 1 calc R . . H11B H 0.9629 -0.3819 0.4336 0.067 Uiso 1 1 calc R . . H11C H 0.8864 -0.4731 0.4496 0.067 Uiso 1 1 calc R . . C12 C 0.7049(11) -0.3813(9) 0.5100(9) 0.057(4) Uani 1 1 d . . . H12A H 0.6921 -0.4495 0.5017 0.086 Uiso 1 1 calc R . . H12B H 0.6306 -0.3476 0.4951 0.086 Uiso 1 1 calc R . . H12C H 0.7347 -0.3690 0.5690 0.086 Uiso 1 1 calc R . . Mo1 Mo 0.68324(7) 0.03573(6) 0.73863(6) 0.0219(2) Uani 1 1 d . . . Mo2 Mo 0.72021(7) -0.11720(6) 0.63031(5) 0.0190(2) Uani 1 1 d . . . O1 O 0.6107(6) -0.0135(5) 0.8096(4) 0.0307(18) Uani 1 1 d . . . O2 O 0.6506(6) -0.2061(5) 0.6702(4) 0.0287(18) Uani 1 1 d . . . P1 P 0.7088(2) 0.2607(2) 0.80350(19) 0.0281(7) Uani 1 1 d . . . P2 P 0.8287(2) -0.22237(19) 0.47171(17) 0.0236(6) Uani 1 1 d . . . Se1 Se 0.57701(9) 0.19771(8) 0.70953(8) 0.0310(3) Uani 1 1 d . . . Se2 Se 0.84004(9) 0.14701(8) 0.81653(7) 0.0295(3) Uani 1 1 d . . . Se3 Se 0.57544(10) 0.00876(8) 0.59994(7) 0.0315(3) Uani 1 1 d . . . Se4 Se 0.86546(11) -0.05506(9) 0.74262(8) 0.0433(3) Uani 1 1 d . . . Se5 Se 0.67348(9) -0.13298(8) 0.46855(7) 0.0281(3) Uani 1 1 d . . . Se6 Se 0.91452(9) -0.19337(8) 0.59802(7) 0.0284(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(7) 0.046(8) 0.035(7) -0.009(6) 0.015(6) 0.009(6) C2 0.033(7) 0.053(8) 0.040(8) -0.002(7) 0.012(6) -0.006(6) C3 0.053(8) 0.043(8) 0.045(8) -0.013(7) 0.014(6) -0.019(6) C4 0.032(6) 0.025(6) 0.042(7) -0.003(6) 0.012(5) 0.001(5) C5 0.045(8) 0.030(7) 0.077(11) -0.001(7) 0.008(7) 0.003(6) C6 0.058(9) 0.050(8) 0.045(8) 0.008(7) 0.022(7) 0.014(7) C7 0.040(7) 0.038(7) 0.023(6) 0.001(5) 0.009(5) 0.012(6) C8 0.070(10) 0.059(9) 0.027(7) 0.006(7) 0.014(6) -0.011(7) C9 0.076(11) 0.076(10) 0.026(7) -0.013(8) 0.012(7) -0.003(8) C10 0.043(7) 0.029(6) 0.031(7) -0.008(6) -0.001(5) 0.001(5) C11 0.051(8) 0.035(7) 0.045(8) 0.002(6) -0.001(6) 0.013(6) C12 0.056(9) 0.036(7) 0.084(11) -0.020(8) 0.023(8) -0.003(7) Mo1 0.0173(4) 0.0262(5) 0.0217(5) -0.0035(4) 0.0011(4) 0.0016(4) Mo2 0.0177(4) 0.0213(4) 0.0176(5) -0.0023(4) 0.0009(3) 0.0008(4) O1 0.023(4) 0.041(5) 0.028(4) -0.004(4) 0.005(3) -0.003(3) O2 0.023(4) 0.032(4) 0.032(4) -0.005(4) 0.007(3) -0.004(3) P1 0.0196(14) 0.0315(16) 0.0326(17) -0.0091(14) 0.0017(12) 0.0003(12) P2 0.0223(14) 0.0271(15) 0.0210(15) -0.0021(12) 0.0018(11) 0.0103(12) Se1 0.0213(6) 0.0287(6) 0.0403(7) -0.0096(6) -0.0061(5) 0.0050(5) Se2 0.0169(5) 0.0336(6) 0.0360(7) -0.0080(5) -0.0038(5) 0.0014(5) Se3 0.0353(7) 0.0311(6) 0.0275(6) -0.0053(5) 0.0023(5) 0.0086(5) Se4 0.0441(8) 0.0461(8) 0.0402(8) -0.0037(7) 0.0071(6) 0.0003(6) Se5 0.0276(6) 0.0353(6) 0.0192(6) -0.0073(5) -0.0053(4) 0.0139(5) Se6 0.0193(5) 0.0443(7) 0.0209(6) 0.0011(5) 0.0002(4) 0.0092(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.502(16) . ? C1 C3 1.513(15) . ? C1 P1 1.838(12) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.527(16) . ? C4 C5 1.528(15) . ? C4 P1 1.816(11) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.494(15) . ? C7 C9 1.499(15) . ? C7 P2 1.834(11) . ? C7 H7 1.0000 . ? 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 C12 1.516(17) . ? C10 C11 1.542(15) . ? C10 P2 1.818(11) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? Mo1 O1 1.656(7) . ? Mo1 Se3 2.4344(14) . ? Mo1 Se4 2.4511(16) . ? Mo1 Se2 2.5869(13) . ? Mo1 Se1 2.6057(14) . ? Mo1 Mo2 2.8424(12) . ? Mo2 O2 1.663(7) . ? Mo2 Se3 2.4412(14) . ? Mo2 Se4 2.4543(15) . ? Mo2 Se6 2.5954(14) . ? Mo2 Se5 2.5964(13) . ? P1 Se1 2.183(3) . ? P1 Se2 2.195(3) . ? P2 Se6 2.177(3) . ? P2 Se5 2.182(3) . ? 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 C1 C3 113.1(10) . . ? C2 C1 P1 111.1(8) . . ? C3 C1 P1 111.0(8) . . ? C2 C1 H1 107.1 . . ? C3 C1 H1 107.1 . . ? P1 C1 H1 107.1 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 109.3(10) . . ? C6 C4 P1 113.4(8) . . ? C5 C4 P1 109.3(8) . . ? C6 C4 H4 108.2 . . ? C5 C4 H4 108.2 . . ? P1 C4 H4 108.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C9 112.5(10) . . ? C8 C7 P2 113.5(8) . . ? C9 C7 P2 109.9(9) . . ? C8 C7 H7 106.8 . . ? C9 C7 H7 106.8 . . ? P2 C7 H7 106.8 . . ? 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 . . ? C12 C10 C11 111.3(10) . . ? C12 C10 P2 112.1(8) . . ? C11 C10 P2 110.7(8) . . ? C12 C10 H10 107.5 . . ? C11 C10 H10 107.5 . . ? P2 C10 H10 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 Mo1 Se3 109.0(2) . . ? O1 Mo1 Se4 105.7(2) . . ? Se3 Mo1 Se4 105.77(5) . . ? O1 Mo1 Se2 107.7(2) . . ? Se3 Mo1 Se2 140.93(6) . . ? Se4 Mo1 Se2 76.46(5) . . ? O1 Mo1 Se1 103.0(3) . . ? Se3 Mo1 Se1 78.64(4) . . ? Se4 Mo1 Se1 147.43(6) . . ? Se2 Mo1 Se1 80.46(4) . . ? O1 Mo1 Mo2 103.6(2) . . ? Se3 Mo1 Mo2 54.45(3) . . ? Se4 Mo1 Mo2 54.64(4) . . ? Se2 Mo1 Mo2 127.35(4) . . ? Se1 Mo1 Mo2 131.41(5) . . ? O2 Mo2 Se3 106.0(2) . . ? O2 Mo2 Se4 107.5(2) . . ? Se3 Mo2 Se4 105.46(5) . . ? O2 Mo2 Se6 103.7(2) . . ? Se3 Mo2 Se6 147.66(5) . . ? Se4 Mo2 Se6 77.02(5) . . ? O2 Mo2 Se5 106.1(2) . . ? Se3 Mo2 Se5 79.47(4) . . ? Se4 Mo2 Se5 142.99(6) . . ? Se6 Mo2 Se5 80.35(4) . . ? O2 Mo2 Mo1 102.5(2) . . ? Se3 Mo2 Mo1 54.23(4) . . ? Se4 Mo2 Mo1 54.54(4) . . ? Se6 Mo2 Mo1 129.87(4) . . ? Se5 Mo2 Mo1 130.70(4) . . ? C4 P1 C1 108.6(5) . . ? C4 P1 Se1 111.7(4) . . ? C1 P1 Se1 114.1(4) . . ? C4 P1 Se2 111.6(4) . . ? C1 P1 Se2 110.6(4) . . ? Se1 P1 Se2 100.00(12) . . ? C10 P2 C7 108.6(5) . . ? C10 P2 Se6 112.6(4) . . ? C7 P2 Se6 112.1(4) . . ? C10 P2 Se5 113.0(4) . . ? C7 P2 Se5 109.9(4) . . ? Se6 P2 Se5 100.43(12) . . ? P1 Se1 Mo1 88.12(8) . . ? P1 Se2 Mo1 88.37(8) . . ? Mo1 Se3 Mo2 71.32(4) . . ? Mo1 Se4 Mo2 70.82(4) . . ? P2 Se5 Mo2 88.10(8) . . ? P2 Se6 Mo2 88.24(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Mo1 Mo2 O2 2.9(3) . . . . ? Se3 Mo1 Mo2 O2 -100.9(2) . . . . ? Se4 Mo1 Mo2 O2 102.7(2) . . . . ? Se2 Mo1 Mo2 O2 128.2(2) . . . . ? Se1 Mo1 Mo2 O2 -118.5(2) . . . . ? O1 Mo1 Mo2 Se3 103.8(2) . . . . ? Se4 Mo1 Mo2 Se3 -156.42(6) . . . . ? Se2 Mo1 Mo2 Se3 -130.92(7) . . . . ? Se1 Mo1 Mo2 Se3 -17.66(6) . . . . ? O1 Mo1 Mo2 Se4 -99.8(2) . . . . ? Se3 Mo1 Mo2 Se4 156.42(6) . . . . ? Se2 Mo1 Mo2 Se4 25.50(6) . . . . ? Se1 Mo1 Mo2 Se4 138.77(8) . . . . ? O1 Mo1 Mo2 Se6 -117.2(2) . . . . ? Se3 Mo1 Mo2 Se6 139.03(7) . . . . ? Se4 Mo1 Mo2 Se6 -17.40(6) . . . . ? Se2 Mo1 Mo2 Se6 8.10(9) . . . . ? Se1 Mo1 Mo2 Se6 121.37(7) . . . . ? O1 Mo1 Mo2 Se5 127.3(2) . . . . ? Se3 Mo1 Mo2 Se5 23.54(6) . . . . ? Se4 Mo1 Mo2 Se5 -132.89(7) . . . . ? Se2 Mo1 Mo2 Se5 -107.39(7) . . . . ? Se1 Mo1 Mo2 Se5 5.88(9) . . . . ? C6 C4 P1 C1 175.1(8) . . . . ? C5 C4 P1 C1 -62.7(10) . . . . ? C6 C4 P1 Se1 -58.2(9) . . . . ? C5 C4 P1 Se1 64.0(9) . . . . ? C6 C4 P1 Se2 52.9(9) . . . . ? C5 C4 P1 Se2 175.1(7) . . . . ? C2 C1 P1 C4 177.7(8) . . . . ? C3 C1 P1 C4 -55.6(10) . . . . ? C2 C1 P1 Se1 52.3(9) . . . . ? C3 C1 P1 Se1 179.0(7) . . . . ? C2 C1 P1 Se2 -59.5(9) . . . . ? C3 C1 P1 Se2 67.3(9) . . . . ? C12 C10 P2 C7 -171.1(9) . . . . ? C11 C10 P2 C7 63.9(9) . . . . ? C12 C10 P2 Se6 64.1(9) . . . . ? C11 C10 P2 Se6 -60.9(9) . . . . ? C12 C10 P2 Se5 -48.9(10) . . . . ? C11 C10 P2 Se5 -173.9(7) . . . . ? C8 C7 P2 C10 -169.2(8) . . . . ? C9 C7 P2 C10 63.8(9) . . . . ? C8 C7 P2 Se6 -44.1(9) . . . . ? C9 C7 P2 Se6 -171.1(7) . . . . ? C8 C7 P2 Se5 66.7(9) . . . . ? C9 C7 P2 Se5 -60.3(9) . . . . ? C4 P1 Se1 Mo1 132.6(4) . . . . ? C1 P1 Se1 Mo1 -103.7(4) . . . . ? Se2 P1 Se1 Mo1 14.32(11) . . . . ? O1 Mo1 Se1 P1 94.0(3) . . . . ? Se3 Mo1 Se1 P1 -158.90(10) . . . . ? Se4 Mo1 Se1 P1 -57.34(14) . . . . ? Se2 Mo1 Se1 P1 -12.10(9) . . . . ? Mo2 Mo1 Se1 P1 -144.32(10) . . . . ? C4 P1 Se2 Mo1 -132.7(4) . . . . ? C1 P1 Se2 Mo1 106.2(4) . . . . ? Se1 P1 Se2 Mo1 -14.43(11) . . . . ? O1 Mo1 Se2 P1 -88.7(3) . . . . ? Se3 Mo1 Se2 P1 70.44(12) . . . . ? Se4 Mo1 Se2 P1 168.88(10) . . . . ? Se1 Mo1 Se2 P1 12.03(9) . . . . ? Mo2 Mo1 Se2 P1 147.71(10) . . . . ? O1 Mo1 Se3 Mo2 -93.4(3) . . . . ? Se4 Mo1 Se3 Mo2 19.81(5) . . . . ? Se2 Mo1 Se3 Mo2 107.63(8) . . . . ? Se1 Mo1 Se3 Mo2 166.58(5) . . . . ? O2 Mo2 Se3 Mo1 94.1(3) . . . . ? Se4 Mo2 Se3 Mo1 -19.75(5) . . . . ? Se6 Mo2 Se3 Mo1 -109.81(9) . . . . ? Se5 Mo2 Se3 Mo1 -162.07(5) . . . . ? O1 Mo1 Se4 Mo2 95.7(2) . . . . ? Se3 Mo1 Se4 Mo2 -19.76(5) . . . . ? Se2 Mo1 Se4 Mo2 -159.39(5) . . . . ? Se1 Mo1 Se4 Mo2 -113.31(10) . . . . ? O2 Mo2 Se4 Mo1 -93.1(3) . . . . ? Se3 Mo2 Se4 Mo1 19.67(5) . . . . ? Se6 Mo2 Se4 Mo1 166.38(5) . . . . ? Se5 Mo2 Se4 Mo1 112.65(8) . . . . ? C10 P2 Se5 Mo2 106.2(4) . . . . ? C7 P2 Se5 Mo2 -132.3(4) . . . . ? Se6 P2 Se5 Mo2 -14.01(10) . . . . ? O2 Mo2 Se5 P2 -89.9(3) . . . . ? Se3 Mo2 Se5 P2 166.28(9) . . . . ? Se4 Mo2 Se5 P2 64.52(12) . . . . ? Se6 Mo2 Se5 P2 11.68(9) . . . . ? Mo1 Mo2 Se5 P2 147.03(9) . . . . ? C10 P2 Se6 Mo2 -106.4(4) . . . . ? C7 P2 Se6 Mo2 130.7(4) . . . . ? Se5 P2 Se6 Mo2 14.01(10) . . . . ? O2 Mo2 Se6 P2 92.6(3) . . . . ? Se3 Mo2 Se6 P2 -63.76(13) . . . . ? Se4 Mo2 Se6 P2 -162.22(9) . . . . ? Se5 Mo2 Se6 P2 -11.71(8) . . . . ? Mo1 Mo2 Se6 P2 -147.75(9) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 2.286 _refine_diff_density_min -2.890 _refine_diff_density_rms 0.222 # Attachment 'Cu-Complex.cif' data_s2200ma _database_code_depnum_ccdc_archive 'CCDC 282910' _publ_section_exptl_refinement ; The structure was solved by direct methods. The non-hydrogen atoms were refined anisotropically, except where the ADP becomes NPD or unrealistic. H atoms were included in calculated positions, except where they were largely indeterminate. ; # Insert blank lines between references _publ_section_references ; # # Put all your general crystallographic references here # Delete as required from the document CIF # Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 Cu4 P4 Se8' _chemical_formula_weight 1354.41 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 12.9380(16) _cell_length_b 17.527(2) _cell_length_c 18.617(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.453(2) _cell_angle_gamma 90.00 _cell_volume 4220.3(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used input _cell_measurement_theta_min 2.2605 _cell_measurement_theta_max 28.228 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 9.056 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1437 _exptl_absorpt_correction_T_max 0.2646 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35597 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9970 _reflns_number_gt 8830 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+7.7605P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9970 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0253 _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0570 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.8926(2) 0.08779(16) 0.37333(15) 0.0150(5) Uani 1 1 d . . . H1 H 0.9306 0.0382 0.3720 0.018 Uiso 1 1 calc R . . C2 C 0.8890(3) 0.11862(18) 0.29628(15) 0.0219(6) Uani 1 1 d . . . H2A H 0.8454 0.0853 0.2659 0.033 Uiso 1 1 calc R . . H2B H 0.9591 0.1199 0.2776 0.033 Uiso 1 1 calc R . . H2C H 0.8600 0.1703 0.2960 0.033 Uiso 1 1 calc R . . C3 C 0.7851(2) 0.07025(18) 0.40025(16) 0.0208(6) Uani 1 1 d . . . H3A H 0.7448 0.1175 0.4021 0.031 Uiso 1 1 calc R . . H3B H 0.7909 0.0479 0.4484 0.031 Uiso 1 1 calc R . . H3C H 0.7505 0.0341 0.3675 0.031 Uiso 1 1 calc R . . C4 C 1.0926(2) 0.16225(17) 0.39345(16) 0.0172(6) Uani 1 1 d . . . H4 H 1.0799 0.1871 0.3457 0.021 Uiso 1 1 calc R . . C5 C 1.1455(3) 0.08565(19) 0.3800(2) 0.0277(7) Uani 1 1 d . . . H5A H 1.2134 0.0946 0.3593 0.041 Uiso 1 1 calc R . . H5B H 1.1028 0.0553 0.3464 0.041 Uiso 1 1 calc R . . H5C H 1.1542 0.0580 0.4255 0.041 Uiso 1 1 calc R . . C6 C 1.1633(2) 0.2151(2) 0.43778(19) 0.0259(7) Uani 1 1 d . . . H6A H 1.1768 0.1925 0.4853 0.039 Uiso 1 1 calc R . . H6B H 1.1296 0.2647 0.4433 0.039 Uiso 1 1 calc R . . H6C H 1.2287 0.2218 0.4132 0.039 Uiso 1 1 calc R . . C7 C 1.0605(3) 0.32779(18) 0.78812(16) 0.0220(6) Uani 1 1 d . . . H7 H 1.1363 0.3385 0.7921 0.026 Uiso 1 1 calc R . . C8 C 1.0255(3) 0.3025(2) 0.86230(17) 0.0305(8) Uani 1 1 d . . . H8A H 1.0369 0.3441 0.8968 0.046 Uiso 1 1 calc R . . H8B H 1.0655 0.2577 0.8779 0.046 Uiso 1 1 calc R . . H8C H 0.9519 0.2896 0.8598 0.046 Uiso 1 1 calc R . . C9 C 1.0068(3) 0.4019(2) 0.7667(2) 0.0352(9) Uani 1 1 d . . . H9A H 0.9317 0.3947 0.7673 0.053 Uiso 1 1 calc R . . H9B H 1.0271 0.4164 0.7182 0.053 Uiso 1 1 calc R . . H9C H 1.0271 0.4422 0.8006 0.053 Uiso 1 1 calc R . . C10 C 1.1136(3) 0.17118(19) 0.75590(18) 0.0246(7) Uani 1 1 d . . . H10 H 1.0849 0.1593 0.8040 0.029 Uiso 1 1 calc R . . C11 C 1.1019(3) 0.1008(2) 0.7099(2) 0.0367(9) Uani 1 1 d . . . H11A H 1.1292 0.1110 0.6622 0.055 Uiso 1 1 calc R . . H11B H 1.0286 0.0872 0.7052 0.055 Uiso 1 1 calc R . . H11C H 1.1404 0.0586 0.7324 0.055 Uiso 1 1 calc R . . C12 C 1.2276(3) 0.1915(2) 0.7673(2) 0.0384(9) Uani 1 1 d . . . H12A H 1.2663 0.1458 0.7821 0.058 Uiso 1 1 calc R . . H12B H 1.2346 0.2306 0.8047 0.058 Uiso 1 1 calc R . . H12C H 1.2551 0.2111 0.7223 0.058 Uiso 1 1 calc R . . C13 C 0.5780(3) 0.0987(2) 0.7044(2) 0.0320(8) Uani 1 1 d . . . H13 H 0.5491 0.0535 0.6780 0.038 Uiso 1 1 calc R . . C14 C 0.5078(4) 0.1137(3) 0.7670(3) 0.0630(16) Uani 1 1 d . . . H14A H 0.5140 0.0717 0.8016 0.095 Uiso 1 1 calc R . . H14B H 0.4360 0.1175 0.7493 0.095 Uiso 1 1 calc R . . H14C H 0.5280 0.1616 0.7905 0.095 Uiso 1 1 calc R . . C15 C 0.6832(3) 0.0775(3) 0.7309(2) 0.0438(10) Uani 1 1 d . . . H15A H 0.7145 0.1208 0.7567 0.066 Uiso 1 1 calc R . . H15B H 0.7259 0.0640 0.6901 0.066 Uiso 1 1 calc R . . H15C H 0.6787 0.0337 0.7635 0.066 Uiso 1 1 calc R . . C16 C 0.4409(2) 0.1803(2) 0.6060(2) 0.0274(7) Uani 1 1 d . . . H16 H 0.3961 0.1916 0.6477 0.033 Uiso 1 1 calc R . . C17 C 0.4049(3) 0.1041(2) 0.5747(3) 0.0509(12) Uani 1 1 d . . . H17A H 0.3323 0.1082 0.5588 0.076 Uiso 1 1 calc R . . H17B H 0.4118 0.0644 0.6115 0.076 Uiso 1 1 calc R . . H17C H 0.4473 0.0909 0.5337 0.076 Uiso 1 1 calc R . . C18 C 0.4228(3) 0.2441(2) 0.5512(2) 0.0308(8) Uani 1 1 d . . . H18A H 0.4590 0.2320 0.5070 0.046 Uiso 1 1 calc R . . H18B H 0.4491 0.2923 0.5710 0.046 Uiso 1 1 calc R . . H18C H 0.3485 0.2489 0.5404 0.046 Uiso 1 1 calc R . . C19 C 0.6362(2) 0.52739(17) 0.56870(17) 0.0208(6) Uani 1 1 d . . . H19 H 0.5765 0.5383 0.5351 0.025 Uiso 1 1 calc R . . C20 C 0.5917(3) 0.4915(2) 0.63604(18) 0.0271(7) Uani 1 1 d . . . H20A H 0.6471 0.4845 0.6723 0.041 Uiso 1 1 calc R . . H20B H 0.5610 0.4419 0.6238 0.041 Uiso 1 1 calc R . . H20C H 0.5385 0.5251 0.6552 0.041 Uiso 1 1 calc R . . C21 C 0.6890(3) 0.60378(19) 0.58505(19) 0.0283(7) Uani 1 1 d . . . H21A H 0.6419 0.6366 0.6115 0.042 Uiso 1 1 calc R . . H21B H 0.7069 0.6287 0.5399 0.042 Uiso 1 1 calc R . . H21C H 0.7520 0.5950 0.6142 0.042 Uiso 1 1 calc R . . C22 C 0.7821(2) 0.51698(17) 0.45149(16) 0.0180(6) Uani 1 1 d . . . H22 H 0.8177 0.5614 0.4751 0.022 Uiso 1 1 calc R . . C23 C 0.6996(3) 0.54862(19) 0.39888(18) 0.0267(7) Uani 1 1 d . . . H23A H 0.7325 0.5821 0.3640 0.040 Uiso 1 1 calc R . . H23B H 0.6484 0.5777 0.4255 0.040 Uiso 1 1 calc R . . H23C H 0.6653 0.5063 0.3735 0.040 Uiso 1 1 calc R . . C24 C 0.8632(3) 0.47181(19) 0.41139(18) 0.0259(7) Uani 1 1 d . . . H24A H 0.8310 0.4264 0.3897 0.039 Uiso 1 1 calc R . . H24B H 0.9187 0.4562 0.4451 0.039 Uiso 1 1 calc R . . H24C H 0.8920 0.5038 0.3736 0.039 Uiso 1 1 calc R . . Cu1 Cu 0.93437(3) 0.31235(2) 0.553251(18) 0.01495(7) Uani 1 1 d . . . Cu2 Cu 0.77916(3) 0.31176(2) 0.649418(19) 0.01655(8) Uani 1 1 d . . . Cu3 Cu 0.74217(3) 0.26306(2) 0.504382(18) 0.01419(7) Uani 1 1 d . . . Cu4 Cu 0.84978(3) 0.17203(2) 0.598873(18) 0.01411(7) Uani 1 1 d . . . P1 P 0.96636(5) 0.15045(4) 0.43547(4) 0.01201(14) Uani 1 1 d . . . P2 P 1.04123(6) 0.25402(4) 0.71850(4) 0.01481(14) Uani 1 1 d . . . P3 P 0.57554(6) 0.17994(5) 0.64074(4) 0.01771(15) Uani 1 1 d . . . P4 P 0.72182(6) 0.46045(4) 0.52205(4) 0.01436(14) Uani 1 1 d . . . Se1 Se 0.89467(2) 0.265778(16) 0.434420(14) 0.01281(6) Uani 1 1 d . . . Se2 Se 0.98117(2) 0.100292(16) 0.540379(15) 0.01542(6) Uani 1 1 d . . . Se3 Se 0.87694(2) 0.220882(17) 0.718202(15) 0.01518(6) Uani 1 1 d . . . Se4 Se 1.09855(2) 0.292643(19) 0.617597(16) 0.02068(7) Uani 1 1 d . . . Se5 Se 0.67759(2) 0.146721(16) 0.552637(15) 0.01393(6) Uani 1 1 d . . . Se6 Se 0.60692(2) 0.28819(2) 0.690322(17) 0.02306(7) Uani 1 1 d . . . Se7 Se 0.84723(2) 0.424354(16) 0.598463(15) 0.01476(6) Uani 1 1 d . . . Se8 Se 0.62947(2) 0.368941(16) 0.477027(16) 0.01616(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0186(14) 0.0127(14) 0.0136(13) -0.0014(11) 0.0015(10) -0.0002(11) C2 0.0327(17) 0.0210(16) 0.0118(14) -0.0013(12) -0.0005(12) -0.0059(13) C3 0.0211(15) 0.0223(16) 0.0188(15) -0.0054(12) 0.0004(11) -0.0064(12) C4 0.0172(14) 0.0195(15) 0.0150(14) -0.0021(11) 0.0033(11) 0.0003(11) C5 0.0206(16) 0.0246(17) 0.0382(19) -0.0046(15) 0.0094(14) 0.0026(13) C6 0.0177(15) 0.0306(18) 0.0296(18) -0.0053(14) 0.0033(13) -0.0054(13) C7 0.0259(16) 0.0227(16) 0.0170(15) -0.0061(12) -0.0062(12) -0.0052(13) C8 0.044(2) 0.0305(19) 0.0169(16) -0.0013(14) -0.0061(14) -0.0010(16) C9 0.058(3) 0.0184(17) 0.0291(19) -0.0068(14) -0.0010(17) -0.0027(16) C10 0.0259(17) 0.0235(17) 0.0240(16) 0.0016(13) -0.0071(13) 0.0050(13) C11 0.047(2) 0.0278(19) 0.035(2) -0.0038(16) -0.0142(17) 0.0138(17) C12 0.0229(18) 0.041(2) 0.051(2) 0.0082(19) -0.0112(16) 0.0049(16) C13 0.035(2) 0.0306(19) 0.0303(19) 0.0123(15) 0.0098(15) 0.0031(15) C14 0.080(4) 0.059(3) 0.053(3) 0.034(2) 0.048(3) 0.030(3) C15 0.037(2) 0.052(3) 0.043(2) 0.030(2) 0.0028(17) 0.0011(19) C16 0.0142(15) 0.0300(18) 0.0382(19) 0.0040(15) 0.0059(13) -0.0049(13) C17 0.036(2) 0.035(2) 0.082(3) 0.008(2) -0.012(2) -0.0171(18) C18 0.0176(16) 0.034(2) 0.040(2) 0.0011(16) -0.0096(14) 0.0017(14) C19 0.0195(15) 0.0169(15) 0.0260(16) -0.0028(12) -0.0021(12) 0.0059(12) C20 0.0214(16) 0.0304(18) 0.0299(18) -0.0050(14) 0.0060(13) 0.0052(13) C21 0.0355(19) 0.0180(16) 0.0315(18) -0.0077(14) 0.0018(14) 0.0040(14) C22 0.0220(15) 0.0115(14) 0.0204(15) 0.0032(11) -0.0037(11) -0.0046(11) C23 0.0321(18) 0.0225(17) 0.0251(17) 0.0073(13) -0.0076(14) -0.0021(14) C24 0.0332(18) 0.0210(17) 0.0239(16) 0.0048(13) 0.0072(13) -0.0005(13) Cu1 0.01516(17) 0.01545(17) 0.01423(17) -0.00188(13) 0.00037(13) -0.00055(13) Cu2 0.01557(17) 0.01949(19) 0.01459(17) -0.00028(14) 0.00046(13) 0.00178(14) Cu3 0.01516(17) 0.01358(17) 0.01379(17) 0.00059(13) -0.00051(13) 0.00043(13) Cu4 0.01466(17) 0.01457(17) 0.01307(16) -0.00023(13) -0.00012(12) 0.00013(13) P1 0.0143(3) 0.0112(3) 0.0105(3) 0.0000(3) 0.0011(2) 0.0003(3) P2 0.0138(3) 0.0138(4) 0.0166(4) -0.0021(3) -0.0041(3) 0.0002(3) P3 0.0162(4) 0.0193(4) 0.0179(4) 0.0057(3) 0.0052(3) 0.0028(3) P4 0.0151(3) 0.0118(3) 0.0160(3) -0.0007(3) -0.0024(3) 0.0009(3) Se1 0.01640(13) 0.01076(13) 0.01128(13) 0.00072(10) 0.00071(10) 0.00086(10) Se2 0.01968(14) 0.01479(14) 0.01179(13) 0.00155(10) 0.00053(10) 0.00515(11) Se3 0.01408(13) 0.01920(15) 0.01217(13) -0.00005(11) -0.00145(10) -0.00103(10) Se4 0.01407(14) 0.03175(18) 0.01618(14) -0.00146(12) -0.00041(11) -0.00361(12) Se5 0.01414(13) 0.01480(14) 0.01286(13) 0.00036(10) 0.00049(10) -0.00156(10) Se6 0.01771(15) 0.03064(18) 0.02112(16) -0.00846(13) 0.00613(11) 0.00041(12) Se7 0.01504(14) 0.01431(14) 0.01477(13) -0.00270(10) -0.00292(10) 0.00146(10) Se8 0.01492(14) 0.01251(14) 0.02077(15) 0.00002(11) -0.00512(11) -0.00002(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.521(4) . ? C1 C2 1.532(4) . ? C1 P1 1.844(3) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.528(4) . ? C4 C5 1.531(4) . ? C4 P1 1.841(3) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.521(5) . ? C7 C8 1.529(5) . ? C7 P2 1.843(3) . ? C7 H7 1.0000 . ? 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 C11 1.507(5) . ? C10 C12 1.527(5) . ? C10 P2 1.854(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.484(5) . ? C13 C14 1.518(5) . ? C13 P3 1.853(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.525(5) . ? C16 C18 1.528(5) . ? C16 P3 1.842(3) . ? C16 H16 1.0000 . ? 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 1.528(5) . ? C19 C21 1.530(4) . ? C19 P4 1.846(3) . ? C19 H19 1.0000 . ? 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 C24 1.524(4) . ? C22 C23 1.534(4) . ? C22 P4 1.835(3) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Cu1 Se1 2.4014(5) . ? Cu1 Se7 2.4253(5) . ? Cu1 Se4 2.4366(5) . ? Cu1 Cu2 2.7240(6) . ? Cu1 Cu3 2.7646(6) . ? Cu1 Cu4 2.8310(6) . ? Cu2 Se7 2.3690(5) . ? Cu2 Se3 2.3865(5) . ? Cu2 Se6 2.4089(5) . ? Cu2 Cu4 2.7860(6) . ? Cu2 Cu3 2.8606(6) . ? Cu3 Se5 2.3877(5) . ? Cu3 Se1 2.3920(5) . ? Cu3 Se8 2.4066(5) . ? Cu3 Cu4 2.7303(5) . ? Cu4 Se2 2.3980(5) . ? Cu4 Se3 2.3984(5) . ? Cu4 Se5 2.4091(5) . ? P1 Se2 2.1459(8) . ? P1 Se1 2.2239(8) . ? P2 Se4 2.1465(9) . ? P2 Se3 2.2034(8) . ? P3 Se6 2.1442(9) . ? P3 Se5 2.2096(8) . ? P4 Se8 2.1569(8) . ? P4 Se7 2.2224(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 C3 C1 C2 111.9(2) . . ? C3 C1 P1 112.1(2) . . ? C2 C1 P1 112.4(2) . . ? C3 C1 H1 106.7 . . ? C2 C1 H1 106.7 . . ? P1 C1 H1 106.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 110.9(3) . . ? C6 C4 P1 111.3(2) . . ? C5 C4 P1 112.1(2) . . ? C6 C4 H4 107.4 . . ? C5 C4 H4 107.4 . . ? P1 C4 H4 107.4 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 109.9(3) . . ? C9 C7 P2 111.2(2) . . ? C8 C7 P2 113.2(2) . . ? C9 C7 H7 107.4 . . ? C8 C7 H7 107.4 . . ? P2 C7 H7 107.4 . . ? 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 . . ? C11 C10 C12 110.6(3) . . ? C11 C10 P2 112.6(2) . . ? C12 C10 P2 110.3(2) . . ? C11 C10 H10 107.7 . . ? C12 C10 H10 107.7 . . ? P2 C10 H10 107.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 110.5(4) . . ? C15 C13 P3 113.9(3) . . ? C14 C13 P3 110.9(3) . . ? C15 C13 H13 107.0 . . ? C14 C13 H13 107.0 . . ? P3 C13 H13 107.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 110.2(3) . . ? C17 C16 P3 114.1(3) . . ? C18 C16 P3 111.4(2) . . ? C17 C16 H16 106.9 . . ? C18 C16 H16 106.9 . . ? P3 C16 H16 106.9 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 111.9(3) . . ? C20 C19 P4 111.6(2) . . ? C21 C19 P4 112.3(2) . . ? C20 C19 H19 106.9 . . ? C21 C19 H19 106.9 . . ? P4 C19 H19 106.9 . . ? 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 . . ? C24 C22 C23 110.6(3) . . ? C24 C22 P4 112.4(2) . . ? C23 C22 P4 110.5(2) . . ? C24 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? P4 C22 H22 107.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Se1 Cu1 Se7 120.291(17) . . ? Se1 Cu1 Se4 124.625(18) . . ? Se7 Cu1 Se4 110.564(17) . . ? Se1 Cu1 Cu2 117.397(18) . . ? Se7 Cu1 Cu2 54.407(13) . . ? Se4 Cu1 Cu2 108.925(19) . . ? Se1 Cu1 Cu3 54.619(12) . . ? Se7 Cu1 Cu3 86.843(16) . . ? Se4 Cu1 Cu3 152.023(19) . . ? Cu2 Cu1 Cu3 62.818(15) . . ? Se1 Cu1 Cu4 84.596(15) . . ? Se7 Cu1 Cu4 114.355(18) . . ? Se4 Cu1 Cu4 93.911(16) . . ? Cu2 Cu1 Cu4 60.165(13) . . ? Cu3 Cu1 Cu4 58.395(12) . . ? Se7 Cu2 Se3 124.995(19) . . ? Se7 Cu2 Se6 128.733(19) . . ? Se3 Cu2 Se6 101.419(18) . . ? Se7 Cu2 Cu1 56.356(13) . . ? Se3 Cu2 Cu1 88.029(16) . . ? Se6 Cu2 Cu1 155.744(19) . . ? Se7 Cu2 Cu4 117.944(18) . . ? Se3 Cu2 Cu4 54.590(14) . . ? Se6 Cu2 Cu4 105.662(18) . . ? Cu1 Cu2 Cu4 61.822(13) . . ? Se7 Cu2 Cu3 85.732(16) . . ? Se3 Cu2 Cu3 112.398(18) . . ? Se6 Cu2 Cu3 96.503(16) . . ? Cu1 Cu2 Cu3 59.284(14) . . ? Cu4 Cu2 Cu3 57.813(12) . . ? Se5 Cu3 Se1 121.549(17) . . ? Se5 Cu3 Se8 121.480(19) . . ? Se1 Cu3 Se8 111.908(18) . . ? Se5 Cu3 Cu4 55.677(13) . . ? Se1 Cu3 Cu4 87.037(16) . . ? Se8 Cu3 Cu4 152.042(18) . . ? Se5 Cu3 Cu1 117.611(16) . . ? Se1 Cu3 Cu1 54.936(14) . . ? Se8 Cu3 Cu1 111.333(18) . . ? Cu4 Cu3 Cu1 62.020(14) . . ? Se5 Cu3 Cu2 87.217(15) . . ? Se1 Cu3 Cu2 112.797(17) . . ? Se8 Cu3 Cu2 93.187(16) . . ? Cu4 Cu3 Cu2 59.723(14) . . ? Cu1 Cu3 Cu2 57.898(12) . . ? Se2 Cu4 Se3 121.261(18) . . ? Se2 Cu4 Se5 113.639(18) . . ? Se3 Cu4 Se5 120.606(17) . . ? Se2 Cu4 Cu3 111.689(18) . . ? Se3 Cu4 Cu3 116.649(18) . . ? Se5 Cu4 Cu3 54.939(13) . . ? Se2 Cu4 Cu2 148.940(18) . . ? Se3 Cu4 Cu2 54.191(12) . . ? Se5 Cu4 Cu2 88.528(15) . . ? Cu3 Cu4 Cu2 62.463(15) . . ? Se2 Cu4 Cu1 92.026(16) . . ? Se3 Cu4 Cu1 85.359(16) . . ? Se5 Cu4 Cu1 114.444(16) . . ? Cu3 Cu4 Cu1 59.585(14) . . ? Cu2 Cu4 Cu1 58.013(14) . . ? C4 P1 C1 104.54(13) . . ? C4 P1 Se2 111.91(10) . . ? C1 P1 Se2 111.10(9) . . ? C4 P1 Se1 105.58(10) . . ? C1 P1 Se1 109.07(10) . . ? Se2 P1 Se1 114.08(3) . . ? C7 P2 C10 103.14(15) . . ? C7 P2 Se4 110.53(11) . . ? C10 P2 Se4 113.15(12) . . ? C7 P2 Se3 107.45(11) . . ? C10 P2 Se3 105.82(11) . . ? Se4 P2 Se3 115.83(3) . . ? C16 P3 C13 103.16(16) . . ? C16 P3 Se6 108.34(12) . . ? C13 P3 Se6 113.87(13) . . ? C16 P3 Se5 108.54(12) . . ? C13 P3 Se5 105.78(12) . . ? Se6 P3 Se5 116.27(4) . . ? C22 P4 C19 105.36(14) . . ? C22 P4 Se8 111.38(10) . . ? C19 P4 Se8 108.80(10) . . ? C22 P4 Se7 107.17(10) . . ? C19 P4 Se7 108.48(10) . . ? Se8 P4 Se7 115.17(3) . . ? P1 Se1 Cu3 109.07(2) . . ? P1 Se1 Cu1 102.79(2) . . ? Cu3 Se1 Cu1 70.444(15) . . ? P1 Se2 Cu4 98.66(2) . . ? P2 Se3 Cu2 108.88(3) . . ? P2 Se3 Cu4 102.42(2) . . ? Cu2 Se3 Cu4 71.219(16) . . ? P2 Se4 Cu1 99.13(2) . . ? P3 Se5 Cu3 106.00(3) . . ? P3 Se5 Cu4 104.52(3) . . ? Cu3 Se5 Cu4 69.385(14) . . ? P3 Se6 Cu2 100.50(2) . . ? P4 Se7 Cu2 102.75(2) . . ? P4 Se7 Cu1 110.28(2) . . ? Cu2 Se7 Cu1 69.237(16) . . ? P4 Se8 Cu3 99.47(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Se1 Cu1 Cu2 Se7 -109.13(2) . . . . ? Se4 Cu1 Cu2 Se7 102.195(18) . . . . ? Cu3 Cu1 Cu2 Se7 -106.943(16) . . . . ? Cu4 Cu1 Cu2 Se7 -174.323(17) . . . . ? Se1 Cu1 Cu2 Se3 115.46(2) . . . . ? Se7 Cu1 Cu2 Se3 -135.415(18) . . . . ? Se4 Cu1 Cu2 Se3 -33.220(19) . . . . ? Cu3 Cu1 Cu2 Se3 117.642(18) . . . . ? Cu4 Cu1 Cu2 Se3 50.262(14) . . . . ? Se1 Cu1 Cu2 Se6 1.52(6) . . . . ? Se7 Cu1 Cu2 Se6 110.64(5) . . . . ? Se4 Cu1 Cu2 Se6 -147.16(4) . . . . ? Cu3 Cu1 Cu2 Se6 3.70(5) . . . . ? Cu4 Cu1 Cu2 Se6 -63.68(5) . . . . ? Se1 Cu1 Cu2 Cu4 65.195(18) . . . . ? Se7 Cu1 Cu2 Cu4 174.323(17) . . . . ? Se4 Cu1 Cu2 Cu4 -83.482(17) . . . . ? Cu3 Cu1 Cu2 Cu4 67.379(13) . . . . ? Se1 Cu1 Cu2 Cu3 -2.184(16) . . . . ? Se7 Cu1 Cu2 Cu3 106.943(16) . . . . ? Se4 Cu1 Cu2 Cu3 -150.86(2) . . . . ? Cu4 Cu1 Cu2 Cu3 -67.379(13) . . . . ? Se1 Cu1 Cu3 Se5 110.75(2) . . . . ? Se7 Cu1 Cu3 Se5 -118.04(2) . . . . ? Se4 Cu1 Cu3 Se5 12.20(5) . . . . ? Cu2 Cu1 Cu3 Se5 -66.871(19) . . . . ? Cu4 Cu1 Cu3 Se5 3.212(16) . . . . ? Se7 Cu1 Cu3 Se1 131.204(17) . . . . ? Se4 Cu1 Cu3 Se1 -98.55(4) . . . . ? Cu2 Cu1 Cu3 Se1 -177.621(17) . . . . ? Cu4 Cu1 Cu3 Se1 -107.539(17) . . . . ? Se1 Cu1 Cu3 Se8 -102.431(18) . . . . ? Se7 Cu1 Cu3 Se8 28.773(19) . . . . ? Se4 Cu1 Cu3 Se8 159.02(3) . . . . ? Cu2 Cu1 Cu3 Se8 79.948(17) . . . . ? Cu4 Cu1 Cu3 Se8 150.03(2) . . . . ? Se1 Cu1 Cu3 Cu4 107.539(17) . . . . ? Se7 Cu1 Cu3 Cu4 -121.257(17) . . . . ? Se4 Cu1 Cu3 Cu4 8.99(4) . . . . ? Cu2 Cu1 Cu3 Cu4 -70.083(15) . . . . ? Se1 Cu1 Cu3 Cu2 177.621(17) . . . . ? Se7 Cu1 Cu3 Cu2 -51.174(13) . . . . ? Se4 Cu1 Cu3 Cu2 79.07(4) . . . . ? Cu4 Cu1 Cu3 Cu2 70.083(15) . . . . ? Se7 Cu2 Cu3 Se5 178.323(15) . . . . ? Se3 Cu2 Cu3 Se5 52.08(2) . . . . ? Se6 Cu2 Cu3 Se5 -53.142(17) . . . . ? Cu1 Cu2 Cu3 Se5 125.329(16) . . . . ? Cu4 Cu2 Cu3 Se5 51.295(15) . . . . ? Se7 Cu2 Cu3 Se1 55.106(18) . . . . ? Se3 Cu2 Cu3 Se1 -71.14(2) . . . . ? Se6 Cu2 Cu3 Se1 -176.359(17) . . . . ? Cu1 Cu2 Cu3 Se1 2.112(16) . . . . ? Cu4 Cu2 Cu3 Se1 -71.922(18) . . . . ? Se7 Cu2 Cu3 Se8 -60.283(17) . . . . ? Se3 Cu2 Cu3 Se8 173.470(17) . . . . ? Se6 Cu2 Cu3 Se8 68.252(19) . . . . ? Cu1 Cu2 Cu3 Se8 -113.277(17) . . . . ? Cu4 Cu2 Cu3 Se8 172.689(17) . . . . ? Se7 Cu2 Cu3 Cu4 127.028(17) . . . . ? Se3 Cu2 Cu3 Cu4 0.781(16) . . . . ? Se6 Cu2 Cu3 Cu4 -104.437(18) . . . . ? Cu1 Cu2 Cu3 Cu4 74.034(15) . . . . ? Se7 Cu2 Cu3 Cu1 52.994(13) . . . . ? Se3 Cu2 Cu3 Cu1 -73.253(18) . . . . ? Se6 Cu2 Cu3 Cu1 -178.471(19) . . . . ? Cu4 Cu2 Cu3 Cu1 -74.034(15) . . . . ? Se5 Cu3 Cu4 Se2 104.36(2) . . . . ? Se1 Cu3 Cu4 Se2 -27.685(19) . . . . ? Se8 Cu3 Cu4 Se2 -162.06(3) . . . . ? Cu1 Cu3 Cu4 Se2 -79.084(18) . . . . ? Cu2 Cu3 Cu4 Se2 -146.34(2) . . . . ? Se5 Cu3 Cu4 Se3 -110.10(2) . . . . ? Se1 Cu3 Cu4 Se3 117.848(18) . . . . ? Se8 Cu3 Cu4 Se3 -16.53(5) . . . . ? Cu1 Cu3 Cu4 Se3 66.449(18) . . . . ? Cu2 Cu3 Cu4 Se3 -0.804(16) . . . . ? Se1 Cu3 Cu4 Se5 -132.047(17) . . . . ? Se8 Cu3 Cu4 Se5 93.58(4) . . . . ? Cu1 Cu3 Cu4 Se5 176.554(17) . . . . ? Cu2 Cu3 Cu4 Se5 109.301(16) . . . . ? Se5 Cu3 Cu4 Cu2 -109.301(16) . . . . ? Se1 Cu3 Cu4 Cu2 118.652(16) . . . . ? Se8 Cu3 Cu4 Cu2 -15.72(4) . . . . ? Cu1 Cu3 Cu4 Cu2 67.253(14) . . . . ? Se5 Cu3 Cu4 Cu1 -176.554(17) . . . . ? Se1 Cu3 Cu4 Cu1 51.399(13) . . . . ? Se8 Cu3 Cu4 Cu1 -82.98(4) . . . . ? Cu2 Cu3 Cu4 Cu1 -67.253(14) . . . . ? Se7 Cu2 Cu4 Se2 22.37(4) . . . . ? Se3 Cu2 Cu4 Se2 -92.43(3) . . . . ? Se6 Cu2 Cu4 Se2 174.54(3) . . . . ? Cu1 Cu2 Cu4 Se2 17.02(3) . . . . ? Cu3 Cu2 Cu4 Se2 86.68(3) . . . . ? Se7 Cu2 Cu4 Se3 114.80(2) . . . . ? Se6 Cu2 Cu4 Se3 -93.035(19) . . . . ? Cu1 Cu2 Cu4 Se3 109.449(18) . . . . ? Cu3 Cu2 Cu4 Se3 179.114(18) . . . . ? Se7 Cu2 Cu4 Se5 -114.921(19) . . . . ? Se3 Cu2 Cu4 Se5 130.281(17) . . . . ? Se6 Cu2 Cu4 Se5 37.246(19) . . . . ? Cu1 Cu2 Cu4 Se5 -120.270(17) . . . . ? Cu3 Cu2 Cu4 Se5 -50.605(13) . . . . ? Se7 Cu2 Cu4 Cu3 -64.316(19) . . . . ? Se3 Cu2 Cu4 Cu3 -179.114(18) . . . . ? Se6 Cu2 Cu4 Cu3 87.851(18) . . . . ? Cu1 Cu2 Cu4 Cu3 -69.665(15) . . . . ? Se7 Cu2 Cu4 Cu1 5.349(16) . . . . ? Se3 Cu2 Cu4 Cu1 -109.449(17) . . . . ? Se6 Cu2 Cu4 Cu1 157.516(19) . . . . ? Cu3 Cu2 Cu4 Cu1 69.665(16) . . . . ? Se1 Cu1 Cu4 Se2 62.740(15) . . . . ? Se7 Cu1 Cu4 Se2 -176.375(16) . . . . ? Se4 Cu1 Cu4 Se2 -61.704(17) . . . . ? Cu2 Cu1 Cu4 Se2 -171.309(17) . . . . ? Cu3 Cu1 Cu4 Se2 114.083(17) . . . . ? Se1 Cu1 Cu4 Se3 -176.055(15) . . . . ? Se7 Cu1 Cu4 Se3 -55.170(18) . . . . ? Se4 Cu1 Cu4 Se3 59.501(16) . . . . ? Cu2 Cu1 Cu4 Se3 -50.105(14) . . . . ? Cu3 Cu1 Cu4 Se3 -124.713(16) . . . . ? Se1 Cu1 Cu4 Se5 -54.441(18) . . . . ? Se7 Cu1 Cu4 Se5 66.44(2) . . . . ? Se4 Cu1 Cu4 Se5 -178.885(16) . . . . ? Cu2 Cu1 Cu4 Se5 71.510(19) . . . . ? Cu3 Cu1 Cu4 Se5 -3.098(15) . . . . ? Se1 Cu1 Cu4 Cu3 -51.342(13) . . . . ? Se7 Cu1 Cu4 Cu3 69.542(18) . . . . ? Se4 Cu1 Cu4 Cu3 -175.786(17) . . . . ? Cu2 Cu1 Cu4 Cu3 74.608(16) . . . . ? Se1 Cu1 Cu4 Cu2 -125.950(17) . . . . ? Se7 Cu1 Cu4 Cu2 -5.066(15) . . . . ? Se4 Cu1 Cu4 Cu2 109.606(18) . . . . ? Cu3 Cu1 Cu4 Cu2 -74.608(16) . . . . ? C6 C4 P1 C1 178.5(2) . . . . ? C5 C4 P1 C1 -56.6(2) . . . . ? C6 C4 P1 Se2 -61.1(2) . . . . ? C5 C4 P1 Se2 63.7(2) . . . . ? C6 C4 P1 Se1 63.5(2) . . . . ? C5 C4 P1 Se1 -171.6(2) . . . . ? C3 C1 P1 C4 179.0(2) . . . . ? C2 C1 P1 C4 -54.0(2) . . . . ? C3 C1 P1 Se2 58.1(2) . . . . ? C2 C1 P1 Se2 -174.87(18) . . . . ? C3 C1 P1 Se1 -68.5(2) . . . . ? C2 C1 P1 Se1 58.5(2) . . . . ? C9 C7 P2 C10 179.4(3) . . . . ? C8 C7 P2 C10 -56.2(3) . . . . ? C9 C7 P2 Se4 58.2(3) . . . . ? C8 C7 P2 Se4 -177.5(2) . . . . ? C9 C7 P2 Se3 -69.1(3) . . . . ? C8 C7 P2 Se3 55.3(3) . . . . ? C11 C10 P2 C7 175.6(3) . . . . ? C12 C10 P2 C7 -60.3(3) . . . . ? C11 C10 P2 Se4 -65.0(3) . . . . ? C12 C10 P2 Se4 59.1(3) . . . . ? C11 C10 P2 Se3 62.9(3) . . . . ? C12 C10 P2 Se3 -173.0(2) . . . . ? C17 C16 P3 C13 -54.1(3) . . . . ? C18 C16 P3 C13 -179.6(3) . . . . ? C17 C16 P3 Se6 -175.1(3) . . . . ? C18 C16 P3 Se6 59.4(3) . . . . ? C17 C16 P3 Se5 57.8(3) . . . . ? C18 C16 P3 Se5 -67.7(3) . . . . ? C15 C13 P3 C16 170.0(3) . . . . ? C14 C13 P3 C16 -64.5(4) . . . . ? C15 C13 P3 Se6 -72.8(3) . . . . ? C14 C13 P3 Se6 52.7(4) . . . . ? C15 C13 P3 Se5 56.1(3) . . . . ? C14 C13 P3 Se5 -178.4(3) . . . . ? C24 C22 P4 C19 175.0(2) . . . . ? C23 C22 P4 C19 -60.9(2) . . . . ? C24 C22 P4 Se8 -67.2(2) . . . . ? C23 C22 P4 Se8 56.9(2) . . . . ? C24 C22 P4 Se7 59.6(2) . . . . ? C23 C22 P4 Se7 -176.35(19) . . . . ? C20 C19 P4 C22 -171.9(2) . . . . ? C21 C19 P4 C22 -45.4(3) . . . . ? C20 C19 P4 Se8 68.5(2) . . . . ? C21 C19 P4 Se8 -165.0(2) . . . . ? C20 C19 P4 Se7 -57.4(2) . . . . ? C21 C19 P4 Se7 69.1(2) . . . . ? C4 P1 Se1 Cu3 -170.95(10) . . . . ? C1 P1 Se1 Cu3 77.21(10) . . . . ? Se2 P1 Se1 Cu3 -47.66(4) . . . . ? C4 P1 Se1 Cu1 -97.49(10) . . . . ? C1 P1 Se1 Cu1 150.67(10) . . . . ? Se2 P1 Se1 Cu1 25.80(4) . . . . ? Se5 Cu3 Se1 P1 -6.28(3) . . . . ? Se8 Cu3 Se1 P1 -161.42(2) . . . . ? Cu4 Cu3 Se1 P1 39.75(2) . . . . ? Cu1 Cu3 Se1 P1 97.23(2) . . . . ? Cu2 Cu3 Se1 P1 95.04(3) . . . . ? Se5 Cu3 Se1 Cu1 -103.50(2) . . . . ? Se8 Cu3 Se1 Cu1 101.349(19) . . . . ? Cu4 Cu3 Se1 Cu1 -57.478(15) . . . . ? Cu2 Cu3 Se1 Cu1 -2.186(16) . . . . ? Se7 Cu1 Se1 P1 -166.41(2) . . . . ? Se4 Cu1 Se1 P1 39.73(3) . . . . ? Cu2 Cu1 Se1 P1 -103.57(3) . . . . ? Cu3 Cu1 Se1 P1 -105.96(2) . . . . ? Cu4 Cu1 Se1 P1 -51.30(2) . . . . ? Se7 Cu1 Se1 Cu3 -60.46(2) . . . . ? Se4 Cu1 Se1 Cu3 145.68(2) . . . . ? Cu2 Cu1 Se1 Cu3 2.383(17) . . . . ? Cu4 Cu1 Se1 Cu3 54.658(13) . . . . ? C4 P1 Se2 Cu4 142.21(10) . . . . ? C1 P1 Se2 Cu4 -101.35(10) . . . . ? Se1 P1 Se2 Cu4 22.43(4) . . . . ? Se3 Cu4 Se2 P1 -137.82(3) . . . . ? Se5 Cu4 Se2 P1 65.85(3) . . . . ? Cu3 Cu4 Se2 P1 5.90(3) . . . . ? Cu2 Cu4 Se2 P1 -66.40(4) . . . . ? Cu1 Cu4 Se2 P1 -52.02(2) . . . . ? C7 P2 Se3 Cu2 81.88(11) . . . . ? C10 P2 Se3 Cu2 -168.45(11) . . . . ? Se4 P2 Se3 Cu2 -42.21(4) . . . . ? C7 P2 Se3 Cu4 156.03(11) . . . . ? C10 P2 Se3 Cu4 -94.30(11) . . . . ? Se4 P2 Se3 Cu4 31.94(4) . . . . ? Se7 Cu2 Se3 P2 -4.67(3) . . . . ? Se6 Cu2 Se3 P2 -161.68(3) . . . . ? Cu1 Cu2 Se3 P2 40.84(3) . . . . ? Cu4 Cu2 Se3 P2 97.11(3) . . . . ? Cu3 Cu2 Se3 P2 96.30(3) . . . . ? Se7 Cu2 Se3 Cu4 -101.78(2) . . . . ? Se6 Cu2 Se3 Cu4 101.206(18) . . . . ? Cu1 Cu2 Se3 Cu4 -56.271(15) . . . . ? Cu3 Cu2 Se3 Cu4 -0.811(16) . . . . ? Se2 Cu4 Se3 P2 36.95(3) . . . . ? Se5 Cu4 Se3 P2 -168.35(3) . . . . ? Cu3 Cu4 Se3 P2 -105.09(3) . . . . ? Cu2 Cu4 Se3 P2 -105.97(3) . . . . ? Cu1 Cu4 Se3 P2 -52.61(2) . . . . ? Se2 Cu4 Se3 Cu2 142.91(2) . . . . ? Se5 Cu4 Se3 Cu2 -62.38(2) . . . . ? Cu3 Cu4 Se3 Cu2 0.879(18) . . . . ? Cu1 Cu4 Se3 Cu2 53.360(15) . . . . ? C7 P2 Se4 Cu1 -108.36(11) . . . . ? C10 P2 Se4 Cu1 136.55(12) . . . . ? Se3 P2 Se4 Cu1 14.12(4) . . . . ? Se1 Cu1 Se4 P2 -131.49(3) . . . . ? Se7 Cu1 Se4 P2 72.48(3) . . . . ? Cu2 Cu1 Se4 P2 14.39(3) . . . . ? Cu3 Cu1 Se4 P2 -53.03(5) . . . . ? Cu4 Cu1 Se4 P2 -45.36(3) . . . . ? C16 P3 Se5 Cu3 97.19(12) . . . . ? C13 P3 Se5 Cu3 -152.67(13) . . . . ? Se6 P3 Se5 Cu3 -25.20(4) . . . . ? C16 P3 Se5 Cu4 169.48(12) . . . . ? C13 P3 Se5 Cu4 -80.37(14) . . . . ? Se6 P3 Se5 Cu4 47.09(4) . . . . ? Se1 Cu3 Se5 P3 160.32(3) . . . . ? Se8 Cu3 Se5 P3 -46.88(3) . . . . ? Cu4 Cu3 Se5 P3 99.84(3) . . . . ? Cu1 Cu3 Se5 P3 96.40(3) . . . . ? Cu2 Cu3 Se5 P3 45.15(3) . . . . ? Se1 Cu3 Se5 Cu4 60.48(2) . . . . ? Se8 Cu3 Se5 Cu4 -146.72(2) . . . . ? Cu1 Cu3 Se5 Cu4 -3.435(17) . . . . ? Cu2 Cu3 Se5 Cu4 -54.689(14) . . . . ? Se2 Cu4 Se5 P3 157.37(3) . . . . ? Se3 Cu4 Se5 P3 0.86(3) . . . . ? Cu3 Cu4 Se5 P3 -101.93(3) . . . . ? Cu2 Cu4 Se5 P3 -45.09(3) . . . . ? Cu1 Cu4 Se5 P3 -98.67(3) . . . . ? Se2 Cu4 Se5 Cu3 -100.70(2) . . . . ? Se3 Cu4 Se5 Cu3 102.80(2) . . . . ? Cu2 Cu4 Se5 Cu3 56.841(16) . . . . ? Cu1 Cu4 Se5 Cu3 3.265(16) . . . . ? C16 P3 Se6 Cu2 -139.07(12) . . . . ? C13 P3 Se6 Cu2 106.79(13) . . . . ? Se5 P3 Se6 Cu2 -16.57(4) . . . . ? Se7 Cu2 Se6 P3 132.58(3) . . . . ? Se3 Cu2 Se6 P3 -71.63(3) . . . . ? Cu1 Cu2 Se6 P3 39.64(6) . . . . ? Cu4 Cu2 Se6 P3 -15.50(3) . . . . ? Cu3 Cu2 Se6 P3 42.84(3) . . . . ? C22 P4 Se7 Cu2 -154.38(10) . . . . ? C19 P4 Se7 Cu2 92.32(11) . . . . ? Se8 P4 Se7 Cu2 -29.85(4) . . . . ? C22 P4 Se7 Cu1 -82.07(11) . . . . ? C19 P4 Se7 Cu1 164.63(11) . . . . ? Se8 P4 Se7 Cu1 42.46(4) . . . . ? Se3 Cu2 Se7 P4 166.02(3) . . . . ? Se6 Cu2 Se7 P4 -43.36(3) . . . . ? Cu1 Cu2 Se7 P4 107.11(3) . . . . ? Cu4 Cu2 Se7 P4 101.45(3) . . . . ? Cu3 Cu2 Se7 P4 51.55(2) . . . . ? Se3 Cu2 Se7 Cu1 58.91(2) . . . . ? Se6 Cu2 Se7 Cu1 -150.47(2) . . . . ? Cu4 Cu2 Se7 Cu1 -5.665(17) . . . . ? Cu3 Cu2 Se7 Cu1 -55.556(14) . . . . ? Se1 Cu1 Se7 P4 7.32(3) . . . . ? Se4 Cu1 Se7 P4 164.53(3) . . . . ? Cu2 Cu1 Se7 P4 -96.41(3) . . . . ? Cu3 Cu1 Se7 P4 -37.95(3) . . . . ? Cu4 Cu1 Se7 P4 -91.00(3) . . . . ? Se1 Cu1 Se7 Cu2 103.72(2) . . . . ? Se4 Cu1 Se7 Cu2 -99.06(2) . . . . ? Cu3 Cu1 Se7 Cu2 58.456(15) . . . . ? Cu4 Cu1 Se7 Cu2 5.405(16) . . . . ? C22 P4 Se8 Cu3 105.25(11) . . . . ? C19 P4 Se8 Cu3 -139.05(11) . . . . ? Se7 P4 Se8 Cu3 -17.05(4) . . . . ? Se5 Cu3 Se8 P4 135.37(3) . . . . ? Se1 Cu3 Se8 P4 -69.46(3) . . . . ? Cu4 Cu3 Se8 P4 60.24(5) . . . . ? Cu1 Cu3 Se8 P4 -9.97(3) . . . . ? Cu2 Cu3 Se8 P4 46.68(3) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 3.240 _refine_diff_density_min -1.665 _refine_diff_density_rms 0.114 # Attachment 'In-complex.cif' data_s2239m _database_code_depnum_ccdc_archive 'CCDC 291036' _publ_section_exptl_refinement ; The structure was solved by direct methods. The non-hydrogen atoms were refined anisotropically, except where the ADP becomes NPD or unrealistic. H atoms were included in calculated positions, except where they were largely indeterminate. ; # Insert blank lines between references _publ_section_references ; # # Put all your general crystallographic references here # Delete as required from the document CIF # Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H42 In P3 Se6' _chemical_formula_weight 940.01 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' 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' In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n 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 15.925(3) _cell_length_b 10.4450(17) _cell_length_c 37.635(6) _cell_angle_alpha 90.00 _cell_angle_beta 92.853(3) _cell_angle_gamma 90.00 _cell_volume 6252.3(18) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used input _cell_measurement_theta_min 2.232 _cell_measurement_theta_max 28.184 _exptl_crystal_description cube _exptl_crystal_colour white _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.997 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 7.901 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.2753 _exptl_absorpt_correction_T_max 0.3010 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52876 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.30 _reflns_number_total 14861 _reflns_number_gt 10719 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0074P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14861 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0602 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 0.822 _refine_ls_restrained_S_all 0.822 _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 C1 C 0.8828(3) 0.8240(4) 0.01843(11) 0.0163(9) Uani 1 1 d . . . H1 H 0.8279 0.8442 0.0056 0.020 Uiso 1 1 calc R . . C2 C 0.9522(3) 0.8385(4) -0.00807(12) 0.0237(11) Uani 1 1 d . . . H2A H 0.9511 0.9256 -0.0177 0.036 Uiso 1 1 calc R . . H2B H 0.9428 0.7769 -0.0275 0.036 Uiso 1 1 calc R . . H2C H 1.0070 0.8222 0.0041 0.036 Uiso 1 1 calc R . . C3 C 0.8950(3) 0.9178(4) 0.04915(11) 0.0223(11) Uani 1 1 d . . . H3A H 0.9497 0.9025 0.0615 0.033 Uiso 1 1 calc R . . H3B H 0.8503 0.9058 0.0658 0.033 Uiso 1 1 calc R . . H3C H 0.8930 1.0056 0.0399 0.033 Uiso 1 1 calc R . . C4 C 0.8723(3) 0.5536(4) -0.00324(11) 0.0190(10) Uani 1 1 d . . . H4 H 0.9265 0.5630 -0.0154 0.023 Uiso 1 1 calc R . . C5 C 0.8012(3) 0.5915(4) -0.02970(11) 0.0240(11) Uani 1 1 d . . . H5A H 0.8017 0.5354 -0.0506 0.036 Uiso 1 1 calc R . . H5B H 0.8089 0.6805 -0.0371 0.036 Uiso 1 1 calc R . . H5C H 0.7473 0.5831 -0.0185 0.036 Uiso 1 1 calc R . . C6 C 0.8640(3) 0.4137(4) 0.00767(11) 0.0226(11) Uani 1 1 d . . . H6A H 0.8108 0.4014 0.0192 0.034 Uiso 1 1 calc R . . H6B H 0.9109 0.3906 0.0243 0.034 Uiso 1 1 calc R . . H6C H 0.8649 0.3591 -0.0135 0.034 Uiso 1 1 calc R . . C7 C 0.6910(3) 0.8665(4) 0.17367(11) 0.0160(9) Uani 1 1 d . . . H7 H 0.7134 0.9514 0.1819 0.019 Uiso 1 1 calc R . . C8 C 0.6651(3) 0.8776(4) 0.13442(12) 0.0296(12) Uani 1 1 d . . . H8A H 0.6374 0.7983 0.1263 0.044 Uiso 1 1 calc R . . H8B H 0.7151 0.8922 0.1208 0.044 Uiso 1 1 calc R . . H8C H 0.6261 0.9496 0.1308 0.044 Uiso 1 1 calc R . . C9 C 0.6148(3) 0.8332(4) 0.19580(13) 0.0279(12) Uani 1 1 d . . . H9A H 0.5716 0.8995 0.1923 0.042 Uiso 1 1 calc R . . H9B H 0.6328 0.8287 0.2211 0.042 Uiso 1 1 calc R . . H9C H 0.5916 0.7503 0.1881 0.042 Uiso 1 1 calc R . . C10 C 0.7982(3) 0.7421(4) 0.22934(11) 0.0185(10) Uani 1 1 d . . . H10 H 0.7459 0.7129 0.2405 0.022 Uiso 1 1 calc R . . C11 C 0.8670(3) 0.6464(4) 0.23978(12) 0.0240(11) Uani 1 1 d . . . H11A H 0.9205 0.6755 0.2308 0.036 Uiso 1 1 calc R . . H11B H 0.8525 0.5625 0.2295 0.036 Uiso 1 1 calc R . . H11C H 0.8725 0.6394 0.2658 0.036 Uiso 1 1 calc R . . C12 C 0.8196(3) 0.8756(4) 0.24446(12) 0.0235(11) Uani 1 1 d . . . H12A H 0.8333 0.8689 0.2701 0.035 Uiso 1 1 calc R . . H12B H 0.7712 0.9325 0.2404 0.035 Uiso 1 1 calc R . . H12C H 0.8680 0.9104 0.2326 0.035 Uiso 1 1 calc R . . C13 C 1.0457(3) 0.2106(4) 0.13099(11) 0.0151(9) Uani 1 1 d . . . H13 H 1.0815 0.1877 0.1527 0.018 Uiso 1 1 calc R . . C14 C 1.0962(3) 0.3026(4) 0.10886(12) 0.0243(11) Uani 1 1 d . . . H14A H 1.1457 0.2583 0.1005 0.036 Uiso 1 1 calc R . . H14B H 1.1142 0.3761 0.1235 0.036 Uiso 1 1 calc R . . H14C H 1.0610 0.3323 0.0884 0.036 Uiso 1 1 calc R . . C15 C 1.0251(3) 0.0862(4) 0.11077(12) 0.0252(11) Uani 1 1 d . . . H15A H 0.9939 0.1062 0.0884 0.038 Uiso 1 1 calc R . . H15B H 0.9908 0.0310 0.1253 0.038 Uiso 1 1 calc R . . H15C H 1.0774 0.0419 0.1057 0.038 Uiso 1 1 calc R . . C16 C 0.9080(3) 0.1746(4) 0.17937(11) 0.0153(9) Uani 1 1 d . . . H16 H 0.9028 0.0878 0.1683 0.018 Uiso 1 1 calc R . . C17 C 0.8210(3) 0.2156(4) 0.18959(12) 0.0249(11) Uani 1 1 d . . . H17A H 0.7994 0.1539 0.2065 0.037 Uiso 1 1 calc R . . H17B H 0.7832 0.2186 0.1683 0.037 Uiso 1 1 calc R . . H17C H 0.8242 0.3006 0.2006 0.037 Uiso 1 1 calc R . . C18 C 0.9693(3) 0.1640(4) 0.21197(12) 0.0256(11) Uani 1 1 d . . . H18A H 0.9779 0.2489 0.2227 0.038 Uiso 1 1 calc R . . H18B H 1.0232 0.1304 0.2047 0.038 Uiso 1 1 calc R . . H18C H 0.9460 0.1060 0.2294 0.038 Uiso 1 1 calc R . . C19 C 0.5580(3) 0.3711(4) 0.11838(12) 0.0194(10) Uani 1 1 d . . . H19 H 0.5982 0.3901 0.1390 0.023 Uiso 1 1 calc R . . C20 C 0.5979(3) 0.2668(4) 0.09602(13) 0.0283(12) Uani 1 1 d . . . H20A H 0.5584 0.2418 0.0765 0.042 Uiso 1 1 calc R . . H20B H 0.6113 0.1921 0.1110 0.042 Uiso 1 1 calc R . . H20C H 0.6496 0.2999 0.0863 0.042 Uiso 1 1 calc R . . C21 C 0.5449(3) 0.4961(4) 0.09702(13) 0.0285(12) Uani 1 1 d . . . H21A H 0.5986 0.5239 0.0880 0.043 Uiso 1 1 calc R . . H21B H 0.5234 0.5627 0.1125 0.043 Uiso 1 1 calc R . . H21C H 0.5043 0.4812 0.0770 0.043 Uiso 1 1 calc R . . C22 C 0.4229(3) 0.4452(4) 0.16514(11) 0.0176(10) Uani 1 1 d . . . H22 H 0.4157 0.5236 0.1501 0.021 Uiso 1 1 calc R . . C23 C 0.3371(3) 0.4125(4) 0.17941(12) 0.0237(11) Uani 1 1 d . . . H23A H 0.3424 0.3370 0.1948 0.036 Uiso 1 1 calc R . . H23B H 0.2969 0.3946 0.1594 0.036 Uiso 1 1 calc R . . H23C H 0.3169 0.4851 0.1931 0.036 Uiso 1 1 calc R . . C24 C 0.4866(3) 0.4757(4) 0.19477(12) 0.0260(11) Uani 1 1 d . . . H24A H 0.4671 0.5490 0.2084 0.039 Uiso 1 1 calc R . . H24B H 0.5405 0.4966 0.1847 0.039 Uiso 1 1 calc R . . H24C H 0.4937 0.4013 0.2105 0.039 Uiso 1 1 calc R . . C25 C 0.3738(3) -0.0320(4) -0.00186(11) 0.0205(10) Uani 1 1 d . . . H25 H 0.4285 -0.0597 -0.0113 0.025 Uiso 1 1 calc R . . C26 C 0.3038(3) -0.0747(4) -0.02859(12) 0.0292(12) Uani 1 1 d . . . H26A H 0.2490 -0.0594 -0.0186 0.044 Uiso 1 1 calc R . . H26B H 0.3100 -0.1661 -0.0336 0.044 Uiso 1 1 calc R . . H26C H 0.3075 -0.0258 -0.0507 0.044 Uiso 1 1 calc R . . C27 C 0.3764(3) 0.1131(4) 0.00198(12) 0.0243(11) Uani 1 1 d . . . H27A H 0.3858 0.1520 -0.0212 0.036 Uiso 1 1 calc R . . H27B H 0.4222 0.1372 0.0190 0.036 Uiso 1 1 calc R . . H27C H 0.3228 0.1434 0.0106 0.036 Uiso 1 1 calc R . . C28 C 0.3546(3) -0.2814(4) 0.03346(12) 0.0218(11) Uani 1 1 d . . . H28 H 0.3031 -0.2962 0.0177 0.026 Uiso 1 1 calc R . . C29 C 0.3433(3) -0.3513(4) 0.06856(12) 0.0255(11) Uani 1 1 d . . . H29A H 0.3402 -0.4437 0.0642 0.038 Uiso 1 1 calc R . . H29B H 0.2913 -0.3223 0.0789 0.038 Uiso 1 1 calc R . . H29C H 0.3913 -0.3327 0.0851 0.038 Uiso 1 1 calc R . . C30 C 0.4298(3) -0.3344(4) 0.01470(13) 0.0278(12) Uani 1 1 d . . . H30A H 0.4816 -0.3152 0.0288 0.042 Uiso 1 1 calc R . . H30B H 0.4324 -0.2949 -0.0088 0.042 Uiso 1 1 calc R . . H30C H 0.4239 -0.4274 0.0120 0.042 Uiso 1 1 calc R . . C31 C 0.2975(3) -0.0999(4) 0.23592(11) 0.0211(10) Uani 1 1 d . . . H31 H 0.2481 -0.0597 0.2469 0.025 Uiso 1 1 calc R . . C32 C 0.3131(3) -0.2305(4) 0.25414(12) 0.0293(12) Uani 1 1 d . . . H32A H 0.3583 -0.2755 0.2426 0.044 Uiso 1 1 calc R . . H32B H 0.2616 -0.2818 0.2521 0.044 Uiso 1 1 calc R . . H32C H 0.3293 -0.2171 0.2793 0.044 Uiso 1 1 calc R . . C33 C 0.3720(3) -0.0110(4) 0.24244(11) 0.0249(11) Uani 1 1 d . . . H33A H 0.3822 0.0019 0.2681 0.037 Uiso 1 1 calc R . . H33B H 0.3600 0.0716 0.2309 0.037 Uiso 1 1 calc R . . H33C H 0.4220 -0.0491 0.2325 0.037 Uiso 1 1 calc R . . C34 C 0.1809(3) -0.2320(4) 0.18442(12) 0.0208(10) Uani 1 1 d . . . H34 H 0.2006 -0.3157 0.1947 0.025 Uiso 1 1 calc R . . C35 C 0.1531(3) -0.2550(4) 0.14524(12) 0.0291(12) Uani 1 1 d . . . H35A H 0.1091 -0.3207 0.1438 0.044 Uiso 1 1 calc R . . H35B H 0.2013 -0.2839 0.1322 0.044 Uiso 1 1 calc R . . H35C H 0.1311 -0.1752 0.1347 0.044 Uiso 1 1 calc R . . C36 C 0.1078(3) -0.1863(5) 0.20588(13) 0.0297(12) Uani 1 1 d . . . H36A H 0.0905 -0.1006 0.1979 0.044 Uiso 1 1 calc R . . H36B H 0.1255 -0.1834 0.2312 0.044 Uiso 1 1 calc R . . H36C H 0.0605 -0.2457 0.2024 0.044 Uiso 1 1 calc R . . In1 In 0.866867(19) 0.56505(3) 0.119914(8) 0.01269(7) Uani 1 1 d . . . In2 In 0.365940(19) 0.03024(3) 0.121645(8) 0.01258(7) Uani 1 1 d . . . P1 P 0.87667(7) 0.65941(10) 0.03561(3) 0.0141(2) Uani 1 1 d . . . P2 P 0.77511(7) 0.74684(10) 0.18113(3) 0.0125(2) Uani 1 1 d . . . P3 P 0.94925(7) 0.28403(10) 0.14601(3) 0.0128(2) Uani 1 1 d . . . P4 P 0.45943(7) 0.31537(10) 0.13658(3) 0.0132(2) Uani 1 1 d . . . P5 P 0.36421(7) -0.10908(10) 0.04147(3) 0.0152(2) Uani 1 1 d . . . P6 P 0.27048(7) -0.11930(10) 0.18815(3) 0.0143(2) Uani 1 1 d . . . Se1 Se 0.98517(3) 0.61790(4) 0.071145(11) 0.01535(10) Uani 1 1 d . . . Se2 Se 0.76209(3) 0.63856(4) 0.064532(11) 0.01595(10) Uani 1 1 d . . . Se3 Se 0.88509(3) 0.80203(4) 0.152773(11) 0.01475(9) Uani 1 1 d . . . Se4 Se 0.73225(3) 0.55867(4) 0.163213(11) 0.01435(10) Uani 1 1 d . . . Se5 Se 0.97845(3) 0.46903(4) 0.170200(11) 0.01499(10) Uani 1 1 d . . . Se6 Se 0.85655(3) 0.30991(4) 0.102251(11) 0.01528(10) Uani 1 1 d . . . Se7 Se 0.48424(3) 0.14225(4) 0.167507(11) 0.01588(10) Uani 1 1 d . . . Se8 Se 0.36469(3) 0.27298(4) 0.094541(11) 0.01524(10) Uani 1 1 d . . . Se9 Se 0.47581(3) -0.06952(4) 0.075647(11) 0.01532(10) Uani 1 1 d . . . Se10 Se 0.25273(3) -0.04112(4) 0.067067(12) 0.01704(10) Uani 1 1 d . . . Se11 Se 0.37654(3) -0.19411(4) 0.160741(11) 0.01597(10) Uani 1 1 d . . . Se12 Se 0.23551(3) 0.06585(4) 0.165507(11) 0.01483(10) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.020(3) 0.018(2) 0.011(2) 0.0014(17) 0.0000(18) 0.0006(18) C2 0.026(3) 0.022(3) 0.024(3) -0.001(2) 0.008(2) -0.009(2) C3 0.028(3) 0.017(2) 0.021(3) -0.0001(19) -0.004(2) -0.001(2) C4 0.017(3) 0.028(3) 0.012(2) -0.0055(19) 0.0001(19) -0.0036(19) C5 0.023(3) 0.034(3) 0.015(2) -0.001(2) -0.001(2) -0.007(2) C6 0.026(3) 0.025(3) 0.017(2) -0.007(2) 0.004(2) -0.003(2) C7 0.017(2) 0.014(2) 0.016(2) -0.0013(18) -0.0014(19) 0.0068(18) C8 0.031(3) 0.036(3) 0.021(3) 0.002(2) -0.007(2) 0.013(2) C9 0.014(3) 0.028(3) 0.042(3) -0.004(2) 0.004(2) 0.005(2) C10 0.019(3) 0.025(2) 0.012(2) -0.0009(19) 0.0068(19) -0.003(2) C11 0.026(3) 0.028(3) 0.017(2) 0.000(2) -0.004(2) 0.001(2) C12 0.026(3) 0.026(3) 0.019(3) -0.005(2) 0.000(2) -0.002(2) C13 0.014(2) 0.018(2) 0.013(2) 0.0008(17) -0.0014(18) 0.0051(18) C14 0.020(3) 0.027(3) 0.027(3) 0.000(2) 0.009(2) 0.002(2) C15 0.030(3) 0.018(2) 0.028(3) -0.006(2) 0.009(2) 0.004(2) C16 0.019(3) 0.013(2) 0.014(2) 0.0041(17) 0.0028(18) 0.0003(18) C17 0.028(3) 0.025(3) 0.023(3) 0.001(2) 0.012(2) -0.004(2) C18 0.029(3) 0.026(3) 0.022(3) 0.006(2) -0.002(2) 0.000(2) C19 0.017(3) 0.023(2) 0.018(2) -0.0011(19) 0.0015(19) -0.0039(19) C20 0.019(3) 0.037(3) 0.031(3) -0.006(2) 0.012(2) -0.008(2) C21 0.022(3) 0.031(3) 0.033(3) 0.012(2) 0.005(2) -0.009(2) C22 0.022(3) 0.015(2) 0.015(2) -0.0023(18) 0.000(2) 0.0025(18) C23 0.024(3) 0.025(3) 0.023(3) -0.009(2) 0.006(2) 0.002(2) C24 0.025(3) 0.026(3) 0.028(3) -0.009(2) -0.001(2) 0.003(2) C25 0.020(3) 0.032(3) 0.010(2) 0.0011(19) 0.0030(19) 0.010(2) C26 0.028(3) 0.039(3) 0.020(3) 0.000(2) -0.007(2) 0.010(2) C27 0.029(3) 0.028(3) 0.016(2) 0.004(2) 0.002(2) 0.008(2) C28 0.025(3) 0.018(2) 0.022(3) -0.0064(19) 0.000(2) 0.002(2) C29 0.026(3) 0.017(2) 0.033(3) -0.009(2) 0.004(2) -0.001(2) C30 0.033(3) 0.023(3) 0.027(3) -0.004(2) 0.004(2) 0.000(2) C31 0.020(3) 0.027(3) 0.017(2) 0.005(2) 0.007(2) 0.006(2) C32 0.030(3) 0.040(3) 0.017(3) 0.011(2) -0.003(2) -0.003(2) C33 0.029(3) 0.034(3) 0.012(2) 0.003(2) -0.007(2) -0.004(2) C34 0.019(3) 0.020(2) 0.023(3) 0.0055(19) 0.003(2) 0.0007(19) C35 0.024(3) 0.036(3) 0.027(3) 0.001(2) -0.003(2) -0.016(2) C36 0.013(3) 0.044(3) 0.032(3) 0.004(2) 0.005(2) -0.003(2) In1 0.01339(16) 0.01459(15) 0.01018(15) 0.00026(12) 0.00149(12) 0.00093(12) In2 0.01399(16) 0.01280(15) 0.01102(15) -0.00033(12) 0.00139(12) -0.00113(12) P1 0.0129(6) 0.0184(6) 0.0110(6) 0.0000(4) 0.0012(5) -0.0023(5) P2 0.0117(6) 0.0145(6) 0.0113(6) -0.0002(4) 0.0018(4) -0.0006(4) P3 0.0143(6) 0.0136(6) 0.0106(6) -0.0003(4) 0.0011(5) 0.0005(4) P4 0.0136(6) 0.0129(5) 0.0130(6) -0.0006(4) 0.0011(5) -0.0005(4) P5 0.0152(6) 0.0194(6) 0.0110(6) -0.0025(5) -0.0001(5) 0.0013(5) P6 0.0126(6) 0.0168(6) 0.0135(6) 0.0029(5) 0.0014(5) 0.0007(5) Se1 0.0120(2) 0.0221(2) 0.0119(2) 0.00112(18) 0.00113(17) -0.00020(18) Se2 0.0118(2) 0.0242(2) 0.0120(2) 0.00208(18) 0.00211(18) 0.00062(18) Se3 0.0153(2) 0.0149(2) 0.0143(2) -0.00041(17) 0.00428(18) -0.00267(18) Se4 0.0136(2) 0.0149(2) 0.0147(2) -0.00159(17) 0.00296(18) -0.00227(17) Se5 0.0164(2) 0.0147(2) 0.0136(2) -0.00098(17) -0.00188(18) -0.00009(17) Se6 0.0159(2) 0.0163(2) 0.0132(2) -0.00098(17) -0.00247(18) 0.00052(18) Se7 0.0173(2) 0.0150(2) 0.0149(2) 0.00156(17) -0.00309(18) -0.00020(18) Se8 0.0161(2) 0.0150(2) 0.0143(2) 0.00215(17) -0.00268(18) -0.00189(18) Se9 0.0127(2) 0.0203(2) 0.0130(2) -0.00195(18) 0.00096(18) -0.00032(18) Se10 0.0126(2) 0.0234(2) 0.0152(2) -0.00370(18) 0.00106(18) -0.00040(18) Se11 0.0164(2) 0.0142(2) 0.0177(2) 0.00197(18) 0.00427(18) 0.00214(18) Se12 0.0148(2) 0.0164(2) 0.0133(2) 0.00137(17) 0.00169(18) 0.00330(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.521(5) . ? C1 C2 1.533(5) . ? C1 P1 1.841(4) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.522(6) . ? C4 C6 1.526(6) . ? C4 P1 1.831(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.518(6) . ? C7 C9 1.546(6) . ? C7 P2 1.843(4) . ? C7 H7 1.0000 . ? 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 C11 1.521(6) . ? C10 C12 1.537(6) . ? C10 P2 1.834(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.526(5) . ? C13 C15 1.533(5) . ? C13 P3 1.831(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.518(6) . ? C16 C18 1.533(6) . ? C16 P3 1.843(4) . ? C16 H16 1.0000 . ? 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 1.533(6) . ? C19 C21 1.542(6) . ? C19 P4 1.839(4) . ? C19 H19 1.0000 . ? 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 C24 1.503(6) . ? C22 C23 1.532(6) . ? C22 P4 1.843(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.523(6) . ? C25 C26 1.530(6) . ? C25 P5 1.832(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.525(6) . ? C28 C29 1.528(6) . ? C28 P5 1.830(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.517(6) . ? C31 C32 1.541(6) . ? C31 P6 1.839(5) . ? C31 H31 1.0000 . ? 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 C36 1.526(6) . ? C34 C35 1.538(6) . ? C34 P6 1.849(4) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? In1 Se2 2.7151(6) . ? In1 Se5 2.7222(6) . ? In1 Se6 2.7495(7) . ? In1 Se1 2.7509(6) . ? In1 Se4 2.7575(6) . ? In1 Se3 2.7757(6) . ? In2 Se9 2.7287(6) . ? In2 Se8 2.7327(6) . ? In2 Se12 2.7421(6) . ? In2 Se7 2.7519(6) . ? In2 Se10 2.7670(6) . ? In2 Se11 2.7676(6) . ? P1 Se1 2.1754(13) . ? P1 Se2 2.1817(12) . ? P2 Se3 2.1738(12) . ? P2 Se4 2.1767(12) . ? P3 Se6 2.1732(12) . ? P3 Se5 2.1765(12) . ? P4 Se7 2.1760(12) . ? P4 Se8 2.1766(12) . ? P5 Se10 2.1803(12) . ? P5 Se9 2.1810(13) . ? P6 Se11 2.1681(12) . ? P6 Se12 2.1746(12) . ? 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 C1 C2 111.2(4) . . ? C3 C1 P1 110.0(3) . . ? C2 C1 P1 111.9(3) . . ? C3 C1 H1 107.9 . . ? C2 C1 H1 107.9 . . ? P1 C1 H1 107.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C6 110.7(4) . . ? C5 C4 P1 111.2(3) . . ? C6 C4 P1 111.3(3) . . ? C5 C4 H4 107.8 . . ? C6 C4 H4 107.8 . . ? P1 C4 H4 107.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 C9 111.1(4) . . ? C8 C7 P2 111.1(3) . . ? C9 C7 P2 110.5(3) . . ? C8 C7 H7 108.0 . . ? C9 C7 H7 108.0 . . ? P2 C7 H7 108.0 . . ? 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 . . ? C11 C10 C12 110.9(4) . . ? C11 C10 P2 112.3(3) . . ? C12 C10 P2 111.8(3) . . ? C11 C10 H10 107.2 . . ? C12 C10 H10 107.2 . . ? P2 C10 H10 107.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 111.6(3) . . ? C14 C13 P3 112.2(3) . . ? C15 C13 P3 110.2(3) . . ? C14 C13 H13 107.5 . . ? C15 C13 H13 107.5 . . ? P3 C13 H13 107.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C18 111.7(4) . . ? C17 C16 P3 111.0(3) . . ? C18 C16 P3 110.8(3) . . ? C17 C16 H16 107.7 . . ? C18 C16 H16 107.7 . . ? P3 C16 H16 107.7 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C21 111.4(4) . . ? C20 C19 P4 111.4(3) . . ? C21 C19 P4 111.4(3) . . ? C20 C19 H19 107.5 . . ? C21 C19 H19 107.5 . . ? P4 C19 H19 107.5 . . ? 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 . . ? C24 C22 C23 111.6(4) . . ? C24 C22 P4 111.6(3) . . ? C23 C22 P4 110.7(3) . . ? C24 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? P4 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C27 C25 C26 111.5(4) . . ? C27 C25 P5 110.9(3) . . ? C26 C25 P5 111.5(3) . . ? C27 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? P5 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 110.8(4) . . ? C30 C28 P5 111.9(3) . . ? C29 C28 P5 109.9(3) . . ? C30 C28 H28 108.0 . . ? C29 C28 H28 108.0 . . ? P5 C28 H28 108.0 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 C32 111.2(4) . . ? C33 C31 P6 111.6(3) . . ? C32 C31 P6 111.2(3) . . ? C33 C31 H31 107.5 . . ? C32 C31 H31 107.5 . . ? P6 C31 H31 107.5 . . ? 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 . . ? C36 C34 C35 111.4(4) . . ? C36 C34 P6 111.5(3) . . ? C35 C34 P6 110.9(3) . . ? C36 C34 H34 107.6 . . ? C35 C34 H34 107.6 . . ? P6 C34 H34 107.6 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Se2 In1 Se5 173.139(17) . . ? Se2 In1 Se6 93.522(17) . . ? Se5 In1 Se6 80.798(16) . . ? Se2 In1 Se1 81.151(19) . . ? Se5 In1 Se1 95.32(2) . . ? Se6 In1 Se1 93.891(16) . . ? Se2 In1 Se4 89.68(2) . . ? Se5 In1 Se4 94.590(19) . . ? Se6 In1 Se4 94.620(15) . . ? Se1 In1 Se4 167.847(17) . . ? Se2 In1 Se3 97.844(18) . . ? Se5 In1 Se3 88.204(18) . . ? Se6 In1 Se3 167.341(18) . . ? Se1 In1 Se3 93.350(16) . . ? Se4 In1 Se3 79.945(15) . . ? Se9 In2 Se8 96.340(17) . . ? Se9 In2 Se12 164.280(17) . . ? Se8 In2 Se12 96.155(16) . . ? Se9 In2 Se7 96.87(2) . . ? Se8 In2 Se7 80.310(16) . . ? Se12 In2 Se7 94.60(2) . . ? Se9 In2 Se10 80.842(19) . . ? Se8 In2 Se10 88.880(17) . . ? Se12 In2 Se10 89.91(2) . . ? Se7 In2 Se10 168.667(17) . . ? Se9 In2 Se11 89.421(17) . . ? Se8 In2 Se11 169.468(18) . . ? Se12 In2 Se11 79.794(16) . . ? Se7 In2 Se11 90.274(18) . . ? Se10 In2 Se11 100.769(18) . . ? C4 P1 C1 106.49(19) . . ? C4 P1 Se1 111.58(15) . . ? C1 P1 Se1 110.36(15) . . ? C4 P1 Se2 109.81(15) . . ? C1 P1 Se2 109.17(14) . . ? Se1 P1 Se2 109.38(5) . . ? C10 P2 C7 106.10(19) . . ? C10 P2 Se3 111.48(15) . . ? C7 P2 Se3 110.03(14) . . ? C10 P2 Se4 109.06(14) . . ? C7 P2 Se4 110.53(15) . . ? Se3 P2 Se4 109.59(5) . . ? C13 P3 C16 106.48(19) . . ? C13 P3 Se6 111.52(14) . . ? C16 P3 Se6 109.98(15) . . ? C13 P3 Se5 109.62(14) . . ? C16 P3 Se5 109.97(14) . . ? Se6 P3 Se5 109.24(5) . . ? C19 P4 C22 106.6(2) . . ? C19 P4 Se7 109.05(15) . . ? C22 P4 Se7 110.71(14) . . ? C19 P4 Se8 111.57(15) . . ? C22 P4 Se8 110.26(15) . . ? Se7 P4 Se8 108.70(5) . . ? C28 P5 C25 107.2(2) . . ? C28 P5 Se10 109.26(15) . . ? C25 P5 Se10 110.87(15) . . ? C28 P5 Se9 110.02(16) . . ? C25 P5 Se9 109.88(16) . . ? Se10 P5 Se9 109.58(5) . . ? C31 P6 C34 106.6(2) . . ? C31 P6 Se11 110.78(15) . . ? C34 P6 Se11 110.54(15) . . ? C31 P6 Se12 109.16(14) . . ? C34 P6 Se12 110.78(15) . . ? Se11 P6 Se12 108.93(5) . . ? P1 Se1 In1 84.31(3) . . ? P1 Se2 In1 85.07(4) . . ? P2 Se3 In1 85.03(3) . . ? P2 Se4 In1 85.42(3) . . ? P3 Se5 In1 85.29(3) . . ? P3 Se6 In1 84.68(3) . . ? P4 Se7 In2 85.26(3) . . ? P4 Se8 In2 85.73(3) . . ? P5 Se9 In2 85.24(3) . . ? P5 Se10 In2 84.32(4) . . ? P6 Se11 In2 85.38(3) . . ? P6 Se12 In2 85.89(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C4 P1 C1 -54.0(4) . . . . ? C6 C4 P1 C1 -178.0(3) . . . . ? C5 C4 P1 Se1 -174.5(3) . . . . ? C6 C4 P1 Se1 61.5(3) . . . . ? C5 C4 P1 Se2 64.1(3) . . . . ? C6 C4 P1 Se2 -59.9(3) . . . . ? C3 C1 P1 C4 -174.6(3) . . . . ? C2 C1 P1 C4 -50.5(4) . . . . ? C3 C1 P1 Se1 -53.3(3) . . . . ? C2 C1 P1 Se1 70.8(3) . . . . ? C3 C1 P1 Se2 66.9(3) . . . . ? C2 C1 P1 Se2 -169.0(3) . . . . ? C11 C10 P2 C7 179.9(3) . . . . ? C12 C10 P2 C7 -54.7(4) . . . . ? C11 C10 P2 Se3 -60.4(3) . . . . ? C12 C10 P2 Se3 65.1(3) . . . . ? C11 C10 P2 Se4 60.8(3) . . . . ? C12 C10 P2 Se4 -173.8(3) . . . . ? C8 C7 P2 C10 -179.0(3) . . . . ? C9 C7 P2 C10 -55.3(4) . . . . ? C8 C7 P2 Se3 60.2(3) . . . . ? C9 C7 P2 Se3 -176.0(3) . . . . ? C8 C7 P2 Se4 -60.9(3) . . . . ? C9 C7 P2 Se4 62.8(3) . . . . ? C14 C13 P3 C16 -168.6(3) . . . . ? C15 C13 P3 C16 66.4(3) . . . . ? C14 C13 P3 Se6 71.4(3) . . . . ? C15 C13 P3 Se6 -53.6(3) . . . . ? C14 C13 P3 Se5 -49.7(3) . . . . ? C15 C13 P3 Se5 -174.7(3) . . . . ? C17 C16 P3 C13 -171.3(3) . . . . ? C18 C16 P3 C13 63.9(3) . . . . ? C17 C16 P3 Se6 -50.3(3) . . . . ? C18 C16 P3 Se6 -175.1(3) . . . . ? C17 C16 P3 Se5 70.0(3) . . . . ? C18 C16 P3 Se5 -54.8(3) . . . . ? C20 C19 P4 C22 176.1(3) . . . . ? C21 C19 P4 C22 -58.8(4) . . . . ? C20 C19 P4 Se7 56.6(3) . . . . ? C21 C19 P4 Se7 -178.4(3) . . . . ? C20 C19 P4 Se8 -63.5(3) . . . . ? C21 C19 P4 Se8 61.6(3) . . . . ? C24 C22 P4 C19 -59.5(4) . . . . ? C23 C22 P4 C19 175.6(3) . . . . ? C24 C22 P4 Se7 59.0(3) . . . . ? C23 C22 P4 Se7 -66.0(3) . . . . ? C24 C22 P4 Se8 179.3(3) . . . . ? C23 C22 P4 Se8 54.4(3) . . . . ? C30 C28 P5 C25 58.4(4) . . . . ? C29 C28 P5 C25 -178.1(3) . . . . ? C30 C28 P5 Se10 178.6(3) . . . . ? C29 C28 P5 Se10 -57.9(3) . . . . ? C30 C28 P5 Se9 -61.1(4) . . . . ? C29 C28 P5 Se9 62.5(3) . . . . ? C27 C25 P5 C28 176.3(3) . . . . ? C26 C25 P5 C28 51.3(4) . . . . ? C27 C25 P5 Se10 57.1(3) . . . . ? C26 C25 P5 Se10 -67.8(3) . . . . ? C27 C25 P5 Se9 -64.2(3) . . . . ? C26 C25 P5 Se9 170.9(3) . . . . ? C33 C31 P6 C34 178.8(3) . . . . ? C32 C31 P6 C34 53.9(4) . . . . ? C33 C31 P6 Se11 58.4(3) . . . . ? C32 C31 P6 Se11 -66.5(3) . . . . ? C33 C31 P6 Se12 -61.5(3) . . . . ? C32 C31 P6 Se12 173.6(3) . . . . ? C36 C34 P6 C31 55.2(4) . . . . ? C35 C34 P6 C31 180.0(3) . . . . ? C36 C34 P6 Se11 175.6(3) . . . . ? C35 C34 P6 Se11 -59.5(3) . . . . ? C36 C34 P6 Se12 -63.5(3) . . . . ? C35 C34 P6 Se12 61.3(3) . . . . ? C4 P1 Se1 In1 -118.97(15) . . . . ? C1 P1 Se1 In1 122.84(14) . . . . ? Se2 P1 Se1 In1 2.73(4) . . . . ? Se2 In1 Se1 P1 -2.09(3) . . . . ? Se5 In1 Se1 P1 171.98(3) . . . . ? Se6 In1 Se1 P1 90.87(3) . . . . ? Se4 In1 Se1 P1 -43.50(9) . . . . ? Se3 In1 Se1 P1 -99.52(3) . . . . ? C4 P1 Se2 In1 120.00(16) . . . . ? C1 P1 Se2 In1 -123.60(15) . . . . ? Se1 P1 Se2 In1 -2.76(4) . . . . ? Se5 In1 Se2 P1 -57.38(15) . . . . ? Se6 In1 Se2 P1 -91.31(3) . . . . ? Se1 In1 Se2 P1 2.08(3) . . . . ? Se4 In1 Se2 P1 174.08(3) . . . . ? Se3 In1 Se2 P1 94.27(3) . . . . ? C10 P2 Se3 In1 119.75(15) . . . . ? C7 P2 Se3 In1 -122.82(15) . . . . ? Se4 P2 Se3 In1 -1.09(4) . . . . ? Se2 In1 Se3 P2 89.09(4) . . . . ? Se5 In1 Se3 P2 -94.16(4) . . . . ? Se6 In1 Se3 P2 -64.59(9) . . . . ? Se1 In1 Se3 P2 170.61(3) . . . . ? Se4 In1 Se3 P2 0.82(3) . . . . ? C10 P2 Se4 In1 -121.20(15) . . . . ? C7 P2 Se4 In1 122.53(14) . . . . ? Se3 P2 Se4 In1 1.09(4) . . . . ? Se2 In1 Se4 P2 -98.85(3) . . . . ? Se5 In1 Se4 P2 86.53(3) . . . . ? Se6 In1 Se4 P2 167.65(3) . . . . ? Se1 In1 Se4 P2 -58.03(9) . . . . ? Se3 In1 Se4 P2 -0.82(3) . . . . ? C13 P3 Se5 In1 121.89(14) . . . . ? C16 P3 Se5 In1 -121.37(15) . . . . ? Se6 P3 Se5 In1 -0.59(4) . . . . ? Se2 In1 Se5 P3 -33.92(15) . . . . ? Se6 In1 Se5 P3 0.44(3) . . . . ? Se1 In1 Se5 P3 -92.65(3) . . . . ? Se4 In1 Se5 P3 94.39(3) . . . . ? Se3 In1 Se5 P3 174.15(3) . . . . ? C13 P3 Se6 In1 -120.74(14) . . . . ? C16 P3 Se6 In1 121.37(14) . . . . ? Se5 P3 Se6 In1 0.58(4) . . . . ? Se2 In1 Se6 P3 175.68(3) . . . . ? Se5 In1 Se6 P3 -0.44(3) . . . . ? Se1 In1 Se6 P3 94.32(3) . . . . ? Se4 In1 Se6 P3 -94.36(3) . . . . ? Se3 In1 Se6 P3 -30.43(9) . . . . ? C19 P4 Se7 In2 -121.95(15) . . . . ? C22 P4 Se7 In2 121.13(16) . . . . ? Se8 P4 Se7 In2 -0.12(4) . . . . ? Se9 In2 Se7 P4 95.39(3) . . . . ? Se8 In2 Se7 P4 0.09(3) . . . . ? Se12 In2 Se7 P4 -95.38(3) . . . . ? Se10 In2 Se7 P4 17.76(10) . . . . ? Se11 In2 Se7 P4 -175.16(3) . . . . ? C19 P4 Se8 In2 120.41(15) . . . . ? C22 P4 Se8 In2 -121.40(15) . . . . ? Se7 P4 Se8 In2 0.12(4) . . . . ? Se9 In2 Se8 P4 -96.02(3) . . . . ? Se12 In2 Se8 P4 93.54(3) . . . . ? Se7 In2 Se8 P4 -0.09(3) . . . . ? Se10 In2 Se8 P4 -176.68(3) . . . . ? Se11 In2 Se8 P4 26.80(11) . . . . ? C28 P5 Se9 In2 -119.25(15) . . . . ? C25 P5 Se9 In2 122.95(15) . . . . ? Se10 P5 Se9 In2 0.90(4) . . . . ? Se8 In2 Se9 P5 -88.51(3) . . . . ? Se12 In2 Se9 P5 53.95(8) . . . . ? Se7 In2 Se9 P5 -169.46(3) . . . . ? Se10 In2 Se9 P5 -0.68(3) . . . . ? Se11 In2 Se9 P5 100.33(3) . . . . ? C28 P5 Se10 In2 119.72(16) . . . . ? C25 P5 Se10 In2 -122.35(16) . . . . ? Se9 P5 Se10 In2 -0.89(4) . . . . ? Se9 In2 Se10 P5 0.68(3) . . . . ? Se8 In2 Se10 P5 97.28(3) . . . . ? Se12 In2 Se10 P5 -166.56(3) . . . . ? Se7 In2 Se10 P5 79.88(9) . . . . ? Se11 In2 Se10 P5 -86.97(3) . . . . ? C31 P6 Se11 In2 -119.60(15) . . . . ? C34 P6 Se11 In2 122.42(16) . . . . ? Se12 P6 Se11 In2 0.48(4) . . . . ? Se9 In2 Se11 P6 -168.87(3) . . . . ? Se8 In2 Se11 P6 67.77(11) . . . . ? Se12 In2 Se11 P6 -0.37(3) . . . . ? Se7 In2 Se11 P6 94.26(4) . . . . ? Se10 In2 Se11 P6 -88.31(4) . . . . ? C31 P6 Se12 In2 120.60(16) . . . . ? C34 P6 Se12 In2 -122.28(15) . . . . ? Se11 P6 Se12 In2 -0.48(4) . . . . ? Se9 In2 Se12 P6 47.71(8) . . . . ? Se8 In2 Se12 P6 -169.81(3) . . . . ? Se7 In2 Se12 P6 -89.09(4) . . . . ? Se10 In2 Se12 P6 101.33(4) . . . . ? Se11 In2 Se12 P6 0.36(3) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.330 _refine_diff_density_min -0.846 _refine_diff_density_rms 0.152 # Attachment 'Ga-complex.cif' data_s2243ma _database_code_depnum_ccdc_archive 'CCDC 291037' _publ_section_synopsis ; # Insert blank lines between paragraphs ? ; _publ_section_abstract ; # Insert blank lines between paragraphs ? ; _publ_section_comment ; # Insert blank lines between paragraphs ? ; _publ_section_exptl_prep ; ? ; _publ_section_exptl_refinement ; The structure was solved by direct methods. The non-hydrogen atoms were refined anisotropically, except where the ADP becomes NPD or unrealistic. H atoms were included in calculated positions, except where they were largely indeterminate. ; # Insert blank lines between references _publ_section_references ; # # Put all your general crystallographic references here # Delete as required from the document CIF # Sheldrick, G.M. (1993) SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1997) SHELXL97. Program for crystal structure refinement. University of Gottingen, Germany. Sheldrick, G.M. (1985). SHELXS86. In Crystallographic Computing 3, edited by G. M. Sheldrick, C. Kruger & R. Goddard, pp. 175-189. Oxford University Press. Sheldrick, G.M. (1997) SHELXS97. Program for Crystal Structure solution. University of Gottingen, Germany. Wilson, A.J.C. (1992) Ed. International Tables for Crystallography, Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands. ; _publ_section_figure_captions ; Figure 1. View of (I) (50% probability displacement ellipsoids) ; _publ_section_acknowledgements ; ? ; _publ_section_table_legends ; Table 1. Fractional atomic coordinates and equivalent isotropic displacement parameters (\%A^2^) Table 2. Selected geometric parameters (\%A ,\% ) ; #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H42 Ga P3 Se6' _chemical_formula_weight 894.91 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ga Ga 0.2307 1.6083 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.7140(12) _cell_length_b 20.684(3) _cell_length_c 16.941(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.457(2) _cell_angle_gamma 90.00 _cell_volume 3012.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used input _cell_measurement_theta_min 2.312 _cell_measurement_theta_max 28.2465 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.974 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 8.330 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2299 _exptl_absorpt_correction_T_max 0.4347 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25581 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7111 _reflns_number_gt 6297 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+1.6851P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7111 _refine_ls_number_parameters 265 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0297 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0523 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9986(3) 0.10922(12) 0.50755(14) 0.0136(5) Uani 1 1 d . . . H1 H 0.9930 0.0763 0.4640 0.016 Uiso 1 1 calc R . . C2 C 1.1314(3) 0.09033(14) 0.57373(17) 0.0210(6) Uani 1 1 d . . . H2A H 1.2277 0.0860 0.5513 0.031 Uiso 1 1 calc R . . H2B H 1.1071 0.0490 0.5972 0.031 Uiso 1 1 calc R . . H2C H 1.1449 0.1238 0.6152 0.031 Uiso 1 1 calc R . . C3 C 1.0285(3) 0.17496(14) 0.47201(18) 0.0253(6) Uani 1 1 d . . . H3A H 1.0384 0.2079 0.5141 0.038 Uiso 1 1 calc R . . H3B H 0.9414 0.1860 0.4298 0.038 Uiso 1 1 calc R . . H3C H 1.1248 0.1731 0.4493 0.038 Uiso 1 1 calc R . . C4 C 0.6572(3) 0.12380(12) 0.45974(14) 0.0134(5) Uani 1 1 d . . . H4 H 0.6784 0.1661 0.4350 0.016 Uiso 1 1 calc R . . C5 C 0.6550(3) 0.07038(14) 0.39679(15) 0.0196(6) Uani 1 1 d . . . H5A H 0.6335 0.0287 0.4202 0.029 Uiso 1 1 calc R . . H5B H 0.7563 0.0686 0.3789 0.029 Uiso 1 1 calc R . . H5C H 0.5738 0.0797 0.3510 0.029 Uiso 1 1 calc R . . C6 C 0.4993(3) 0.12806(13) 0.48817(16) 0.0180(5) Uani 1 1 d . . . H6A H 0.4173 0.1355 0.4421 0.027 Uiso 1 1 calc R . . H6B H 0.5009 0.1639 0.5261 0.027 Uiso 1 1 calc R . . H6C H 0.4789 0.0875 0.5145 0.027 Uiso 1 1 calc R . . C7 C 0.3796(3) 0.23214(13) 0.77218(15) 0.0168(5) Uani 1 1 d . . . H7 H 0.3999 0.2718 0.8061 0.020 Uiso 1 1 calc R . . C8 C 0.4103(3) 0.24980(14) 0.68832(16) 0.0236(6) Uani 1 1 d . . . H8A H 0.3824 0.2132 0.6521 0.035 Uiso 1 1 calc R . . H8B H 0.5208 0.2600 0.6907 0.035 Uiso 1 1 calc R . . H8C H 0.3474 0.2875 0.6685 0.035 Uiso 1 1 calc R . . C9 C 0.2095(3) 0.21311(14) 0.77146(18) 0.0242(6) Uani 1 1 d . . . H9A H 0.1412 0.2453 0.7411 0.036 Uiso 1 1 calc R . . H9B H 0.1886 0.2113 0.8265 0.036 Uiso 1 1 calc R . . H9C H 0.1899 0.1706 0.7463 0.036 Uiso 1 1 calc R . . C10 C 0.4499(3) 0.14177(13) 0.90882(15) 0.0166(5) Uani 1 1 d . . . H10 H 0.3411 0.1254 0.8937 0.020 Uiso 1 1 calc R . . C11 C 0.5511(3) 0.08618(13) 0.94642(16) 0.0209(6) Uani 1 1 d . . . H11A H 0.6589 0.1010 0.9608 0.031 Uiso 1 1 calc R . . H11B H 0.5466 0.0505 0.9080 0.031 Uiso 1 1 calc R . . H11C H 0.5130 0.0713 0.9946 0.031 Uiso 1 1 calc R . . C12 C 0.4476(4) 0.19801(14) 0.96753(17) 0.0264(6) Uani 1 1 d . . . H12A H 0.4121 0.1824 1.0161 0.040 Uiso 1 1 calc R . . H12B H 0.3766 0.2317 0.9425 0.040 Uiso 1 1 calc R . . H12C H 0.5526 0.2160 0.9815 0.040 Uiso 1 1 calc R . . C13 C 0.9589(3) -0.07833(12) 0.92358(15) 0.0153(5) Uani 1 1 d . . . H13 H 1.0444 -0.0527 0.9558 0.018 Uiso 1 1 calc R . . C14 C 0.8081(3) -0.06326(14) 0.95526(16) 0.0219(6) Uani 1 1 d . . . H14A H 0.7233 -0.0895 0.9265 0.033 Uiso 1 1 calc R . . H14B H 0.7828 -0.0173 0.9470 0.033 Uiso 1 1 calc R . . H14C H 0.8217 -0.0733 1.0125 0.033 Uiso 1 1 calc R . . C15 C 1.0000(3) -0.15016(13) 0.93525(17) 0.0235(6) Uani 1 1 d . . . H15A H 1.0023 -0.1619 0.9915 0.035 Uiso 1 1 calc R . . H15B H 1.1024 -0.1582 0.9204 0.035 Uiso 1 1 calc R . . H15C H 0.9216 -0.1763 0.9013 0.035 Uiso 1 1 calc R . . C16 C 1.1219(3) -0.07005(13) 0.77984(16) 0.0193(5) Uani 1 1 d . . . H16 H 1.1206 -0.0429 0.7309 0.023 Uiso 1 1 calc R . . C17 C 1.1315(4) -0.14030(14) 0.75308(19) 0.0295(7) Uani 1 1 d . . . H17A H 1.2239 -0.1460 0.7277 0.044 Uiso 1 1 calc R . . H17B H 1.0382 -0.1511 0.7147 0.044 Uiso 1 1 calc R . . H17C H 1.1385 -0.1689 0.7997 0.044 Uiso 1 1 calc R . . C18 C 1.2662(3) -0.05006(15) 0.83839(18) 0.0255(6) Uani 1 1 d . . . H18A H 1.2792 -0.0788 0.8850 0.038 Uiso 1 1 calc R . . H18B H 1.2543 -0.0054 0.8557 0.038 Uiso 1 1 calc R . . H18C H 1.3580 -0.0532 0.8120 0.038 Uiso 1 1 calc R . . Ga1 Ga 0.75350(3) 0.083439(13) 0.716567(15) 0.01220(6) Uani 1 1 d . . . P1 P 0.81271(7) 0.10812(3) 0.54465(4) 0.01055(12) Uani 1 1 d . . . P2 P 0.51746(7) 0.16979(3) 0.81698(4) 0.01227(13) Uani 1 1 d . . . P3 P 0.94057(8) -0.05165(3) 0.81822(4) 0.01365(13) Uani 1 1 d . . . Se1 Se 0.77521(3) 0.014303(12) 0.601441(14) 0.01269(6) Uani 1 1 d . . . Se2 Se 0.81366(3) 0.178782(12) 0.641834(14) 0.01296(6) Uani 1 1 d . . . Se3 Se 0.48681(3) 0.084692(12) 0.735181(15) 0.01360(6) Uani 1 1 d . . . Se4 Se 0.74810(3) 0.207258(12) 0.839871(15) 0.01494(6) Uani 1 1 d . . . Se5 Se 0.93931(3) 0.056475(12) 0.831536(15) 0.01572(6) Uani 1 1 d . . . Se6 Se 0.74054(3) -0.090677(13) 0.745629(16) 0.02008(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0116(11) 0.0159(13) 0.0139(11) -0.0021(10) 0.0041(9) 0.0006(9) C2 0.0129(12) 0.0275(15) 0.0225(14) 0.0032(12) 0.0026(10) 0.0031(11) C3 0.0165(13) 0.0279(16) 0.0334(16) 0.0132(13) 0.0103(12) 0.0008(11) C4 0.0106(11) 0.0146(13) 0.0141(11) 0.0031(10) -0.0009(9) 0.0020(9) C5 0.0170(13) 0.0265(15) 0.0147(12) -0.0025(11) 0.0008(10) 0.0010(11) C6 0.0134(12) 0.0190(14) 0.0216(13) -0.0002(11) 0.0034(10) 0.0006(10) C7 0.0166(13) 0.0127(12) 0.0209(13) -0.0014(10) 0.0026(10) 0.0041(10) C8 0.0295(15) 0.0214(15) 0.0207(14) 0.0050(11) 0.0062(12) 0.0085(12) C9 0.0184(14) 0.0239(15) 0.0297(15) -0.0021(12) 0.0022(12) 0.0048(11) C10 0.0192(13) 0.0164(13) 0.0157(12) -0.0007(10) 0.0070(10) -0.0017(10) C11 0.0231(14) 0.0222(15) 0.0177(13) 0.0038(11) 0.0042(11) -0.0010(11) C12 0.0377(17) 0.0249(16) 0.0190(14) -0.0037(12) 0.0120(13) -0.0041(13) C13 0.0156(12) 0.0150(13) 0.0138(12) 0.0019(10) -0.0019(10) -0.0012(10) C14 0.0226(14) 0.0264(15) 0.0172(13) 0.0036(11) 0.0048(11) -0.0013(12) C15 0.0285(15) 0.0172(14) 0.0235(14) 0.0063(11) 0.0008(12) -0.0011(11) C16 0.0237(14) 0.0167(13) 0.0186(13) 0.0020(11) 0.0070(11) 0.0020(11) C17 0.0369(17) 0.0202(15) 0.0343(16) -0.0012(13) 0.0143(14) 0.0056(13) C18 0.0195(14) 0.0297(16) 0.0280(15) 0.0025(13) 0.0061(12) 0.0005(12) Ga1 0.01279(13) 0.01317(14) 0.01080(13) 0.00119(10) 0.00244(10) 0.00120(10) P1 0.0109(3) 0.0102(3) 0.0108(3) -0.0001(2) 0.0024(2) 0.0002(2) P2 0.0138(3) 0.0103(3) 0.0129(3) -0.0015(2) 0.0030(2) 0.0000(2) P3 0.0155(3) 0.0116(3) 0.0132(3) 0.0008(2) 0.0003(2) -0.0008(2) Se1 0.01646(12) 0.00925(12) 0.01274(12) -0.00020(9) 0.00350(9) 0.00008(9) Se2 0.01594(12) 0.00977(12) 0.01362(11) -0.00141(9) 0.00379(9) -0.00063(9) Se3 0.01226(12) 0.01242(12) 0.01636(12) -0.00392(9) 0.00313(9) -0.00159(9) Se4 0.01511(12) 0.01278(12) 0.01686(12) -0.00216(10) 0.00237(10) -0.00286(9) Se5 0.01909(13) 0.01123(12) 0.01493(12) 0.00055(9) -0.00290(10) 0.00017(10) Se6 0.02283(14) 0.01498(13) 0.01926(13) 0.00369(10) -0.00588(11) -0.00608(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.524(4) . ? C1 C3 1.527(4) . ? C1 P1 1.831(2) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C6 1.533(3) . ? C4 C5 1.534(4) . ? C4 P1 1.836(2) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C9 1.531(4) . ? C7 C8 1.533(4) . ? C7 P2 1.839(3) . ? C7 H7 1.0000 . ? 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 C11 1.523(4) . ? C10 C12 1.533(4) . ? C10 P2 1.845(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.531(4) . ? C13 C15 1.533(4) . ? C13 P3 1.850(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.526(4) . ? C16 C17 1.529(4) . ? C16 P3 1.844(3) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Ga1 Se5 2.3854(4) . ? Ga1 Se3 2.3962(5) . ? Ga1 Se2 2.4464(4) . ? Ga1 Se1 2.4507(4) . ? P1 Se2 2.2005(7) . ? P1 Se1 2.2140(7) . ? P2 Se4 2.1294(7) . ? P2 Se3 2.2290(7) . ? P3 Se6 2.1208(7) . ? P3 Se5 2.2480(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 C2 C1 C3 111.1(2) . . ? C2 C1 P1 110.62(17) . . ? C3 C1 P1 111.36(18) . . ? C2 C1 H1 107.9 . . ? C3 C1 H1 107.9 . . ? P1 C1 H1 107.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 110.5(2) . . ? C6 C4 P1 110.43(17) . . ? C5 C4 P1 109.92(17) . . ? C6 C4 H4 108.6 . . ? C5 C4 H4 108.6 . . ? P1 C4 H4 108.6 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C7 C8 111.7(2) . . ? C9 C7 P2 112.88(19) . . ? C8 C7 P2 110.35(18) . . ? C9 C7 H7 107.2 . . ? C8 C7 H7 107.2 . . ? P2 C7 H7 107.2 . . ? 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 . . ? C11 C10 C12 111.7(2) . . ? C11 C10 P2 110.29(18) . . ? C12 C10 P2 110.41(18) . . ? C11 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? P2 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C15 110.3(2) . . ? C14 C13 P3 109.54(17) . . ? C15 C13 P3 113.26(18) . . ? C14 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? P3 C13 H13 107.8 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 111.8(2) . . ? C18 C16 P3 112.18(19) . . ? C17 C16 P3 113.1(2) . . ? C18 C16 H16 106.4 . . ? C17 C16 H16 106.4 . . ? P3 C16 H16 106.4 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Se5 Ga1 Se3 115.974(16) . . ? Se5 Ga1 Se2 115.888(15) . . ? Se3 Ga1 Se2 110.752(13) . . ? Se5 Ga1 Se1 112.494(16) . . ? Se3 Ga1 Se1 108.324(13) . . ? Se2 Ga1 Se1 90.424(15) . . ? C1 P1 C4 108.04(11) . . ? C1 P1 Se2 110.72(8) . . ? C4 P1 Se2 112.36(8) . . ? C1 P1 Se1 111.23(8) . . ? C4 P1 Se1 110.65(8) . . ? Se2 P1 Se1 103.87(3) . . ? C7 P2 C10 106.91(12) . . ? C7 P2 Se4 110.67(9) . . ? C10 P2 Se4 112.53(9) . . ? C7 P2 Se3 107.08(9) . . ? C10 P2 Se3 104.71(9) . . ? Se4 P2 Se3 114.44(3) . . ? C16 P3 C13 109.59(12) . . ? C16 P3 Se6 112.77(9) . . ? C13 P3 Se6 112.24(9) . . ? C16 P3 Se5 105.03(9) . . ? C13 P3 Se5 101.60(9) . . ? Se6 P3 Se5 114.82(3) . . ? P1 Se1 Ga1 82.57(2) . . ? P1 Se2 Ga1 82.94(2) . . ? P2 Se3 Ga1 94.05(2) . . ? P3 Se5 Ga1 99.47(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 C1 P1 C4 -174.76(18) . . . . ? C3 C1 P1 C4 61.2(2) . . . . ? C2 C1 P1 Se2 61.81(19) . . . . ? C3 C1 P1 Se2 -62.3(2) . . . . ? C2 C1 P1 Se1 -53.1(2) . . . . ? C3 C1 P1 Se1 -177.23(16) . . . . ? C6 C4 P1 C1 -176.15(18) . . . . ? C5 C4 P1 C1 61.6(2) . . . . ? C6 C4 P1 Se2 -53.72(19) . . . . ? C5 C4 P1 Se2 -175.94(15) . . . . ? C6 C4 P1 Se1 61.87(19) . . . . ? C5 C4 P1 Se1 -60.35(18) . . . . ? C9 C7 P2 C10 -44.4(2) . . . . ? C8 C7 P2 C10 -170.24(19) . . . . ? C9 C7 P2 Se4 -167.29(16) . . . . ? C8 C7 P2 Se4 66.9(2) . . . . ? C9 C7 P2 Se3 67.36(19) . . . . ? C8 C7 P2 Se3 -58.5(2) . . . . ? C11 C10 P2 C7 175.68(18) . . . . ? C12 C10 P2 C7 -60.4(2) . . . . ? C11 C10 P2 Se4 -62.61(19) . . . . ? C12 C10 P2 Se4 61.3(2) . . . . ? C11 C10 P2 Se3 62.27(19) . . . . ? C12 C10 P2 Se3 -173.79(17) . . . . ? C18 C16 P3 C13 -46.1(2) . . . . ? C17 C16 P3 C13 81.4(2) . . . . ? C18 C16 P3 Se6 -171.95(17) . . . . ? C17 C16 P3 Se6 -44.4(2) . . . . ? C18 C16 P3 Se5 62.3(2) . . . . ? C17 C16 P3 Se5 -170.13(18) . . . . ? C14 C13 P3 C16 -179.79(18) . . . . ? C15 C13 P3 C16 -56.1(2) . . . . ? C14 C13 P3 Se6 -53.7(2) . . . . ? C15 C13 P3 Se6 69.97(19) . . . . ? C14 C13 P3 Se5 69.48(18) . . . . ? C15 C13 P3 Se5 -166.88(17) . . . . ? C1 P1 Se1 Ga1 122.82(9) . . . . ? C4 P1 Se1 Ga1 -117.08(9) . . . . ? Se2 P1 Se1 Ga1 3.70(2) . . . . ? Se5 Ga1 Se1 P1 -121.63(2) . . . . ? Se3 Ga1 Se1 P1 108.84(2) . . . . ? Se2 Ga1 Se1 P1 -3.226(19) . . . . ? C1 P1 Se2 Ga1 -123.17(9) . . . . ? C4 P1 Se2 Ga1 115.92(9) . . . . ? Se1 P1 Se2 Ga1 -3.70(2) . . . . ? Se5 Ga1 Se2 P1 118.64(2) . . . . ? Se3 Ga1 Se2 P1 -106.57(2) . . . . ? Se1 Ga1 Se2 P1 3.243(19) . . . . ? C7 P2 Se3 Ga1 122.66(9) . . . . ? C10 P2 Se3 Ga1 -124.06(9) . . . . ? Se4 P2 Se3 Ga1 -0.39(3) . . . . ? Se5 Ga1 Se3 P2 67.04(2) . . . . ? Se2 Ga1 Se3 P2 -67.71(2) . . . . ? Se1 Ga1 Se3 P2 -165.40(2) . . . . ? C16 P3 Se5 Ga1 103.57(9) . . . . ? C13 P3 Se5 Ga1 -142.25(8) . . . . ? Se6 P3 Se5 Ga1 -20.88(3) . . . . ? Se3 Ga1 Se5 P3 88.24(2) . . . . ? Se2 Ga1 Se5 P3 -139.35(2) . . . . ? Se1 Ga1 Se5 P3 -37.23(2) . . . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.511 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.104