# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is (C) The Royal Society of Chemistry 2006 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Tatsuro Imakubo' _publ_contact_author_address ; Imakubo Initiative Research Unit RIKEN 2-1 Hirosawa Wako Saitama 351-0198 ; _publ_contact_author_email IMAKUBO@RIKEN.JP _publ_section_title ; Trigonal supramolecular organic conductors based on diiodo(pyrazino)tetraselenafulvalene: high yield recovery of the neutral p-donor by a simple chemical reaction ; loop_ _publ_author_name 'Tatsuro Imakubo' 'Megumi Kibune' 'Takashi Shirahata' 'Hiroko Yoshino' # Attachment '1a_revised.cif' data_(DIPSe)3(PF6)1.33(CH2Cl2)1.2 _database_code_depnum_ccdc_archive 'CCDC 294686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.2 H8.40 Cl2.40 F8 I6 N6 P1.33 Se12' _chemical_formula_weight 2382.40 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 20.3226(18) _cell_length_b 20.3226(18) _cell_length_c 7.2569(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2595.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 5296 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.76 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2058 _exptl_absorpt_coefficient_mu 12.189 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.1840 _exptl_absorpt_correction_T_max 0.6413 _exptl_absorpt_process_details 'XPREP; Bruker AXS 2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18597 _diffrn_reflns_av_R_equivalents 0.0702 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 28.33 _reflns_number_total 1221 _reflns_number_gt 1053 _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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1221 _refine_ls_number_parameters 89 _refine_ls_number_restraints 81 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.1018 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 1.132 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.0000 0.0000 0.0908(17) 0.081(6) Uani 0.33 6 d SPD . . F1 F -0.0599(7) 0.0000 0.2500 0.109(6) Uani 0.67 4 d SPDU . . F2 F 0.0683(9) 0.0000 -0.039(3) 0.092(6) Uani 0.33 2 d SPDU . . P2 P 0.6667 0.3333 0.132(4) 0.263(14) Uani 0.17 3 d SPDU . 1 F3 F 0.5860(13) 0.280(2) 0.2500 0.214(15) Uani 0.33 2 d SPDU . 1 F4 F 0.6276(7) 0.3724(7) 0.0000 0.284(16) Uani 0.33 2 d SPDU A 1 C1 C 0.6424(4) 0.6044(4) 0.7500 0.0298(14) Uani 1 2 d S . . C2 C 0.4913(5) 0.4913(5) 0.7500 0.031(2) Uani 1 4 d S . . C3 C 0.4259(5) 0.4259(5) 0.7500 0.0275(19) Uani 1 4 d S . . C4 C 0.3159(4) 0.2762(4) 0.7500 0.0296(14) Uani 1 2 d S . . C5 C 0.2022(5) 0.1642(5) 0.7500 0.047(2) Uani 1 2 d S . . H5A H 0.1744 0.1102 0.7500 0.5(2) Uiso 1 2 calc SR . . C1T C 0.6667 0.3333 0.0000 0.277(16) Uani 0.60 6 d SPDU . 2 Cl1T Cl 0.7164(4) 0.4327(9) 0.0000 0.274(11) Uani 0.40 2 d SPDU B 2 I1 I 0.75969(3) 0.65148(3) 0.7500 0.03264(19) Uani 1 2 d S . . N1 N 0.2794(4) 0.2006(3) 0.7500 0.0367(14) Uani 1 2 d S . . Se1 Se 0.58712(4) 0.49690(4) 0.7500 0.0344(2) Uani 1 2 d S . . Se2 Se 0.42276(4) 0.33121(4) 0.7500 0.0322(2) Uani 1 2 d S . . 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 P1 0.035(3) 0.035(3) 0.172(18) 0.000 0.000 0.0176(16) F1 0.057(6) 0.088(11) 0.193(18) 0.000 0.000 0.044(5) F2 0.069(9) 0.078(12) 0.132(17) 0.000 0.009(11) 0.039(6) P2 0.250(15) 0.250(15) 0.29(2) 0.000 0.000 0.125(7) F3 0.18(2) 0.22(2) 0.25(2) 0.000 0.000 0.096(17) F4 0.261(16) 0.261(16) 0.34(2) 0.004(12) 0.004(12) 0.136(15) C1 0.024(3) 0.027(3) 0.031(3) 0.000 0.000 0.008(3) C2 0.028(4) 0.028(4) 0.038(5) 0.000 0.000 0.016(4) C3 0.027(3) 0.027(3) 0.032(5) 0.000 0.000 0.015(4) C4 0.030(4) 0.022(3) 0.034(3) 0.000 0.000 0.011(3) C5 0.031(4) 0.028(4) 0.074(5) 0.000 0.000 0.008(3) C1T 0.261(17) 0.261(17) 0.31(2) 0.000 0.000 0.131(8) Cl1T 0.214(13) 0.206(15) 0.40(3) 0.000 -0.044(17) 0.103(8) I1 0.0236(3) 0.0323(3) 0.0392(3) 0.000 0.000 0.0118(2) N1 0.030(3) 0.023(3) 0.056(4) 0.000 0.000 0.013(3) Se1 0.0259(4) 0.0255(4) 0.0516(5) 0.000 0.000 0.0128(3) Se2 0.0242(4) 0.0272(4) 0.0465(4) 0.000 0.000 0.0138(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 P1 1.32(3) 13 ? P1 F2 1.44(2) 13 ? P1 F2 1.44(2) 15 ? P1 F2 1.44(2) 14 ? P1 F2 1.678(8) 3 ? P1 F2 1.678(8) 2 ? P1 F2 1.678(8) . ? P1 F1 1.679(8) 3 ? P1 F1 1.679(8) . ? P1 F1 1.679(8) 2 ? P1 P1 2.31(3) 16_556 ? F1 F2 1.54(2) 4 ? F1 F2 1.54(2) 13 ? F1 P1 1.679(8) 16_556 ? F2 P1 1.44(2) 13 ? F2 F2 1.501(16) 15 ? F2 F2 1.501(16) 14 ? F2 F1 1.54(2) 13 ? P2 F3 1.678(8) 2_655 ? P2 F3 1.678(8) . ? P2 F3 1.678(8) 3_665 ? P2 F4 1.678(8) 2_655 ? P2 F4 1.678(8) 3_665 ? P2 F4 1.678(8) . ? P2 P2 1.71(6) 16_556 ? P2 P2 1.92(6) 10_665 ? F3 P2 1.678(8) 16_556 ? F4 P2 1.678(8) 10_665 ? C1 C1 1.338(15) 7_556 ? C1 Se1 1.893(7) . ? C1 I1 2.077(7) . ? C2 C3 1.328(14) . ? C2 Se1 1.893(6) 7_556 ? C2 Se1 1.893(6) . ? C3 Se2 1.893(5) 7_556 ? C3 Se2 1.893(5) . ? C4 N1 1.332(8) . ? C4 C4 1.397(13) 7_556 ? C4 Se2 1.881(7) . ? C5 C5 1.337(16) 7_556 ? C5 N1 1.359(10) . ? C5 H5A 0.9500 . ? C1T Cl1T 1.750(15) 3_665 ? C1T Cl1T 1.750(15) 2_655 ? C1T Cl1T 1.750(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 P1 F2 75.0(11) 13 13 ? P1 P1 F2 75.0(11) 13 15 ? F2 P1 F2 113.5(9) 13 15 ? P1 P1 F2 75.0(11) 13 14 ? F2 P1 F2 113.5(9) 13 14 ? F2 P1 F2 113.5(9) 15 14 ? P1 P1 F2 55.7(10) 13 3 ? F2 P1 F2 57.0(6) 13 3 ? F2 P1 F2 130.7(12) 15 3 ? F2 P1 F2 57.0(6) 14 3 ? P1 P1 F2 55.7(10) 13 2 ? F2 P1 F2 57.0(6) 13 2 ? F2 P1 F2 57.0(6) 15 2 ? F2 P1 F2 130.7(12) 14 2 ? F2 P1 F2 91.4(13) 3 2 ? P1 P1 F2 55.7(10) 13 . ? F2 P1 F2 130.7(12) 13 . ? F2 P1 F2 57.0(6) 15 . ? F2 P1 F2 57.0(6) 14 . ? F2 P1 F2 91.4(13) 3 . ? F2 P1 F2 91.4(13) 2 . ? P1 P1 F1 133.5(6) 13 3 ? F2 P1 F1 121.9(8) 13 3 ? F2 P1 F1 58.5(9) 15 3 ? F2 P1 F1 121.9(8) 14 3 ? F2 P1 F1 170.8(13) 3 3 ? F2 P1 F1 95.0(7) 2 3 ? F2 P1 F1 95.0(7) . 3 ? P1 P1 F1 133.5(6) 13 . ? F2 P1 F1 58.5(9) 13 . ? F2 P1 F1 121.9(8) 15 . ? F2 P1 F1 121.9(8) 14 . ? F2 P1 F1 95.0(7) 3 . ? F2 P1 F1 95.0(7) 2 . ? F2 P1 F1 170.8(13) . . ? F1 P1 F1 77.8(8) 3 . ? P1 P1 F1 133.5(6) 13 2 ? F2 P1 F1 121.9(8) 13 2 ? F2 P1 F1 121.9(8) 15 2 ? F2 P1 F1 58.5(9) 14 2 ? F2 P1 F1 95.0(7) 3 2 ? F2 P1 F1 170.8(13) 2 2 ? F2 P1 F1 95.0(7) . 2 ? F1 P1 F1 77.8(8) 3 2 ? F1 P1 F1 77.8(8) . 2 ? P1 P1 P1 180.0 13 16_556 ? F2 P1 P1 105.0(11) 13 16_556 ? F2 P1 P1 105.0(11) 15 16_556 ? F2 P1 P1 105.0(11) 14 16_556 ? F2 P1 P1 124.3(10) 3 16_556 ? F2 P1 P1 124.3(10) 2 16_556 ? F2 P1 P1 124.3(10) . 16_556 ? F1 P1 P1 46.5(6) 3 16_556 ? F1 P1 P1 46.5(6) . 16_556 ? F1 P1 P1 46.5(6) 2 16_556 ? F2 F1 F2 167.3(16) 4 13 ? F2 F1 P1 139.8(13) 4 . ? F2 F1 P1 52.8(5) 13 . ? F2 F1 P1 52.8(5) 4 16_556 ? F2 F1 P1 139.8(13) 13 16_556 ? P1 F1 P1 87.0(11) . 16_556 ? P1 F2 F2 69.7(5) 13 15 ? P1 F2 F2 69.7(5) 13 14 ? F2 F2 F2 106.4(19) 15 14 ? P1 F2 F1 68.6(12) 13 13 ? F2 F2 F1 109(2) 15 13 ? F2 F2 F1 109(2) 14 13 ? P1 F2 P1 49.3(12) 13 . ? F2 F2 P1 53.4(9) 15 . ? F2 F2 P1 53.4(8) 14 . ? F1 F2 P1 117.9(17) 13 . ? F3 P2 F3 96.4(17) 2_655 . ? F3 P2 F3 96.4(17) 2_655 3_665 ? F3 P2 F3 96.4(17) . 3_665 ? F3 P2 F4 93.5(14) 2_655 2_655 ? F3 P2 F4 80.1(12) . 2_655 ? F3 P2 F4 170(2) 3_665 2_655 ? F3 P2 F4 80.1(12) 2_655 3_665 ? F3 P2 F4 170(2) . 3_665 ? F3 P2 F4 93.5(14) 3_665 3_665 ? F4 P2 F4 90.5(19) 2_655 3_665 ? F3 P2 F4 170(2) 2_655 . ? F3 P2 F4 93.5(14) . . ? F3 P2 F4 80.1(12) 3_665 . ? F4 P2 F4 90.5(19) 2_655 . ? F4 P2 F4 90.5(19) 3_665 . ? F3 P2 P2 59.4(13) 2_655 16_556 ? F3 P2 P2 59.4(13) . 16_556 ? F3 P2 P2 59.4(13) 3_665 16_556 ? F4 P2 P2 124.9(13) 2_655 16_556 ? F4 P2 P2 124.9(13) 3_665 16_556 ? F4 P2 P2 124.9(13) . 16_556 ? F3 P2 P2 120.6(13) 2_655 10_665 ? F3 P2 P2 120.6(13) . 10_665 ? F3 P2 P2 120.6(13) 3_665 10_665 ? F4 P2 P2 55.1(13) 2_655 10_665 ? F4 P2 P2 55.1(13) 3_665 10_665 ? F4 P2 P2 55.1(13) . 10_665 ? P2 P2 P2 180.000(11) 16_556 10_665 ? P2 F3 P2 61(3) 16_556 . ? P2 F4 P2 70(3) . 10_665 ? C1 C1 Se1 119.0(2) 7_556 . ? C1 C1 I1 126.50(19) 7_556 . ? Se1 C1 I1 114.5(4) . . ? C3 C2 Se1 123.0(3) . 7_556 ? C3 C2 Se1 123.0(3) . . ? Se1 C2 Se1 114.0(5) 7_556 . ? C2 C3 Se2 121.7(3) . 7_556 ? C2 C3 Se2 121.7(3) . . ? Se2 C3 Se2 116.6(5) 7_556 . ? N1 C4 C4 121.1(4) . 7_556 ? N1 C4 Se2 119.8(5) . . ? C4 C4 Se2 119.03(19) 7_556 . ? C5 C5 N1 121.9(4) 7_556 . ? C5 C5 H5A 119.0 7_556 . ? N1 C5 H5A 119.0 . . ? Cl1T C1T Cl1T 120.000(1) 3_665 2_655 ? Cl1T C1T Cl1T 120.000(2) 3_665 . ? Cl1T C1T Cl1T 120.000(1) 2_655 . ? C4 N1 C5 117.0(6) . . ? C1 Se1 C2 94.0(4) . . ? C4 Se2 C3 92.7(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.036 _refine_diff_density_min -1.263 _refine_diff_density_rms 0.410 # Attachment '1b_revised.cif' data_(DIPSe)3(AsF6)1.33(CH2Cl2)1.2 _database_code_depnum_ccdc_archive 'CCDC 294687' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.2 H8.4 As1.33 Cl2.40 F8 I6 N6 Se12' _chemical_formula_weight 2440.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 20.3703(17) _cell_length_b 20.3703(17) _cell_length_c 7.2558(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2607.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 3863 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 27.69 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.109 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2106 _exptl_absorpt_coefficient_mu 12.685 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1858 _exptl_absorpt_correction_T_max 0.3636 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13782 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.30 _reflns_number_total 1179 _reflns_number_gt 913 _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^)+(0.0681P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1179 _refine_ls_number_parameters 88 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0464 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.1170 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.072 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.0000 0.0000 0.0887(11) 0.069(3) Uani 0.33 6 d SPD . . F1 F -0.0632(6) 0.0000 0.2500 0.086(6) Uani 0.67 4 d SPDU . . F2 F 0.0706(10) 0.0000 -0.046(4) 0.087(8) Uani 0.33 2 d SPDU . . As2 As 0.6667 0.3333 0.133(3) 0.233(12) Uani 0.17 3 d SPDU . 1 F3 F 0.5828(11) 0.275(2) 0.2500 0.133(13) Uani 0.33 2 d SPDU . 1 F4 F 0.6256(6) 0.3744(6) 0.0000 0.263(18) Uani 0.33 2 d SPDU A 1 C1 C 0.6436(5) 0.6062(5) 0.7500 0.0298(19) Uani 1 2 d S . . C2 C 0.4912(6) 0.4912(6) 0.7500 0.031(3) Uani 1 4 d S . . C3 C 0.4263(7) 0.4263(7) 0.7500 0.028(3) Uani 1 4 d S . . C4 C 0.3162(5) 0.2767(5) 0.7500 0.0280(19) Uani 1 2 d S . . C5 C 0.2036(6) 0.1654(6) 0.7500 0.049(3) Uani 1 2 d S . . H5A H 0.1758 0.1115 0.7500 0.059 Uiso 1 2 calc SR . . C1T C 0.6667 0.3333 0.0000 0.242(15) Uani 0.60 6 d SPDU . 2 Cl1T Cl 0.7171(5) 0.4342(10) 0.0000 0.285(15) Uani 0.40 2 d SPDU B 2 I1 I 0.75984(3) 0.65152(3) 0.7500 0.0324(2) Uani 1 2 d S . . N1 N 0.2804(4) 0.2015(4) 0.7500 0.038(2) Uani 1 2 d S . . Se1 Se 0.58755(5) 0.49757(5) 0.7500 0.0337(3) Uani 1 2 d S . . Se2 Se 0.42352(5) 0.33208(5) 0.7500 0.0319(3) Uani 1 2 d S . . 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 As1 0.0375(17) 0.0375(17) 0.132(8) 0.000 0.000 0.0187(8) F1 0.053(7) 0.063(10) 0.146(18) 0.000 0.000 0.032(5) F2 0.073(11) 0.075(14) 0.11(2) 0.000 0.001(13) 0.038(7) As2 0.199(11) 0.199(11) 0.30(2) 0.000 0.000 0.099(6) F3 0.074(17) 0.12(2) 0.17(3) 0.000 0.000 0.021(16) F4 0.244(18) 0.244(18) 0.32(3) 0.003(14) 0.003(14) 0.140(18) C1 0.027(5) 0.031(5) 0.030(5) 0.000 0.000 0.013(4) C2 0.027(5) 0.027(5) 0.042(8) 0.000 0.000 0.014(5) C3 0.030(5) 0.030(5) 0.031(7) 0.000 0.000 0.019(5) C4 0.031(5) 0.019(4) 0.034(5) 0.000 0.000 0.013(4) C5 0.031(5) 0.027(5) 0.082(9) 0.000 0.000 0.007(4) C1T 0.220(16) 0.220(16) 0.29(3) 0.000 0.000 0.110(8) Cl1T 0.237(18) 0.25(2) 0.37(3) 0.000 -0.03(2) 0.127(11) I1 0.0236(3) 0.0319(3) 0.0387(4) 0.000 0.000 0.0116(2) N1 0.025(4) 0.024(4) 0.063(6) 0.000 0.000 0.011(3) Se1 0.0251(5) 0.0253(5) 0.0506(7) 0.000 0.000 0.0124(4) Se2 0.0245(5) 0.0274(5) 0.0454(6) 0.000 0.000 0.0142(4) _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 As1 As1 1.287(17) 13 ? As1 F2 1.47(2) 15 ? As1 F2 1.47(2) 14 ? As1 F2 1.47(2) 13 ? As1 F2 1.739(9) 3 ? As1 F2 1.739(9) . ? As1 F2 1.739(9) 2 ? As1 F1 1.739(9) 3 ? As1 F1 1.739(9) 2 ? As1 F1 1.739(9) . ? As1 As1 2.341(17) 16_556 ? F1 F2 1.49(3) 4 ? F1 F2 1.49(3) 13 ? F1 As1 1.739(9) 16_556 ? F2 As1 1.47(2) 13 ? F2 F1 1.49(3) 13 ? F2 F2 1.586(15) 15 ? F2 F2 1.586(15) 14 ? As2 As2 1.70(5) 16_556 ? As2 F3 1.739(9) 2_655 ? As2 F3 1.739(9) . ? As2 F3 1.739(9) 3_665 ? As2 F4 1.739(9) 2_655 ? As2 F4 1.739(9) 3_665 ? As2 F4 1.739(9) . ? As2 As2 1.92(5) 10_665 ? F3 As2 1.739(9) 16_556 ? F4 As2 1.739(9) 10_665 ? C1 C1 1.321(19) 7_556 ? C1 Se1 1.916(9) . ? C1 I1 2.067(9) . ? C2 C3 1.322(19) . ? C2 Se1 1.901(7) . ? C2 Se1 1.901(7) 7_556 ? C3 Se2 1.892(7) 7_556 ? C3 Se2 1.892(7) . ? C4 N1 1.328(11) . ? C4 C4 1.394(17) 7_556 ? C4 Se2 1.893(9) . ? C5 C5 1.35(2) 7_556 ? C5 N1 1.357(13) . ? C5 H5A 0.9500 . ? C1T Cl1T 1.779(18) 3_665 ? C1T Cl1T 1.779(18) . ? C1T Cl1T 1.779(18) 2_655 ? 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 As1 As1 F2 77.8(11) 13 15 ? As1 As1 F2 77.8(11) 13 14 ? F2 As1 F2 115.7(7) 15 14 ? As1 As1 F2 77.8(11) 13 13 ? F2 As1 F2 115.7(7) 15 13 ? F2 As1 F2 115.7(7) 14 13 ? As1 As1 F2 55.8(11) 13 3 ? F2 As1 F2 133.7(8) 15 3 ? F2 As1 F2 58.5(7) 14 3 ? F2 As1 F2 58.5(7) 13 3 ? As1 As1 F2 55.8(11) 13 . ? F2 As1 F2 58.5(7) 15 . ? F2 As1 F2 58.5(7) 14 . ? F2 As1 F2 133.7(8) 13 . ? F2 As1 F2 91.5(16) 3 . ? As1 As1 F2 55.8(11) 13 2 ? F2 As1 F2 58.5(7) 15 2 ? F2 As1 F2 133.7(8) 14 2 ? F2 As1 F2 58.5(7) 13 2 ? F2 As1 F2 91.5(16) 3 2 ? F2 As1 F2 91.5(16) . 2 ? As1 As1 F1 132.3(4) 13 3 ? F2 As1 F1 54.5(11) 15 3 ? F2 As1 F1 120.2(7) 14 3 ? F2 As1 F1 120.2(7) 13 3 ? F2 As1 F1 171.9(13) 3 3 ? F2 As1 F1 94.1(9) . 3 ? F2 As1 F1 94.1(9) 2 3 ? As1 As1 F1 132.3(4) 13 2 ? F2 As1 F1 120.2(7) 15 2 ? F2 As1 F1 54.5(11) 14 2 ? F2 As1 F1 120.2(7) 13 2 ? F2 As1 F1 94.1(9) 3 2 ? F2 As1 F1 94.1(9) . 2 ? F2 As1 F1 171.9(13) 2 2 ? F1 As1 F1 79.7(6) 3 2 ? As1 As1 F1 132.3(4) 13 . ? F2 As1 F1 120.2(7) 15 . ? F2 As1 F1 120.2(7) 14 . ? F2 As1 F1 54.5(11) 13 . ? F2 As1 F1 94.1(9) 3 . ? F2 As1 F1 171.9(13) . . ? F2 As1 F1 94.1(9) 2 . ? F1 As1 F1 79.7(6) 3 . ? F1 As1 F1 79.7(6) 2 . ? As1 As1 As1 180.000(1) 13 16_556 ? F2 As1 As1 102.2(11) 15 16_556 ? F2 As1 As1 102.2(11) 14 16_556 ? F2 As1 As1 102.2(11) 13 16_556 ? F2 As1 As1 124.2(11) 3 16_556 ? F2 As1 As1 124.2(11) . 16_556 ? F2 As1 As1 124.2(11) 2 16_556 ? F1 As1 As1 47.7(4) 3 16_556 ? F1 As1 As1 47.7(4) 2 16_556 ? F1 As1 As1 47.7(4) . 16_556 ? F2 F1 F2 168.2(15) 4 13 ? F2 F1 As1 53.6(6) 4 16_556 ? F2 F1 As1 138.2(11) 13 16_556 ? F2 F1 As1 138.2(11) 4 . ? F2 F1 As1 53.6(6) 13 . ? As1 F1 As1 84.6(8) 16_556 . ? As1 F2 F1 72.0(16) 13 13 ? As1 F2 F2 69.2(5) 13 15 ? F1 F2 F2 112(2) 13 15 ? As1 F2 F2 69.2(5) 13 14 ? F1 F2 F2 112(2) 13 14 ? F2 F2 F2 104(3) 15 14 ? As1 F2 As1 46.3(8) 13 . ? F1 F2 As1 118.3(19) 13 . ? F2 F2 As1 52.3(10) 15 . ? F2 F2 As1 52.3(10) 14 . ? As2 As2 F3 60.7(9) 16_556 2_655 ? As2 As2 F3 60.7(9) 16_556 . ? F3 As2 F3 98.0(12) 2_655 . ? As2 As2 F3 60.7(9) 16_556 3_665 ? F3 As2 F3 98.0(12) 2_655 3_665 ? F3 As2 F3 98.0(12) . 3_665 ? As2 As2 F4 123.6(10) 16_556 2_655 ? F3 As2 F4 93.2(13) 2_655 2_655 ? F3 As2 F4 77.2(10) . 2_655 ? F3 As2 F4 168.4(16) 3_665 2_655 ? As2 As2 F4 123.6(10) 16_556 3_665 ? F3 As2 F4 77.2(10) 2_655 3_665 ? F3 As2 F4 168.4(16) . 3_665 ? F3 As2 F4 93.2(13) 3_665 3_665 ? F4 As2 F4 92.4(14) 2_655 3_665 ? As2 As2 F4 123.6(10) 16_556 . ? F3 As2 F4 168.4(16) 2_655 . ? F3 As2 F4 93.2(13) . . ? F3 As2 F4 77.2(10) 3_665 . ? F4 As2 F4 92.4(14) 2_655 . ? F4 As2 F4 92.4(14) 3_665 . ? As2 As2 As2 180.000(9) 16_556 10_665 ? F3 As2 As2 119.3(9) 2_655 10_665 ? F3 As2 As2 119.3(9) . 10_665 ? F3 As2 As2 119.3(9) 3_665 10_665 ? F4 As2 As2 56.4(10) 2_655 10_665 ? F4 As2 As2 56.4(10) 3_665 10_665 ? F4 As2 As2 56.4(10) . 10_665 ? As2 F3 As2 58.7(19) 16_556 . ? As2 F4 As2 67(2) . 10_665 ? C1 C1 Se1 118.9(3) 7_556 . ? C1 C1 I1 127.2(3) 7_556 . ? Se1 C1 I1 113.8(5) . . ? C3 C2 Se1 123.4(3) . . ? C3 C2 Se1 123.4(3) . 7_556 ? Se1 C2 Se1 113.3(7) . 7_556 ? C2 C3 Se2 121.5(3) . 7_556 ? C2 C3 Se2 121.5(3) . . ? Se2 C3 Se2 117.0(7) 7_556 . ? N1 C4 C4 121.6(5) . 7_556 ? N1 C4 Se2 119.5(7) . . ? C4 C4 Se2 118.9(2) 7_556 . ? C5 C5 N1 122.0(6) 7_556 . ? C5 C5 H5A 119.0 7_556 . ? N1 C5 H5A 119.0 . . ? Cl1T C1T Cl1T 120.000(2) 3_665 . ? Cl1T C1T Cl1T 120.000(1) 3_665 2_655 ? Cl1T C1T Cl1T 120.000(2) . 2_655 ? C4 N1 C5 116.4(9) . . ? C2 Se1 C1 94.4(4) . . ? C3 Se2 C4 92.6(4) . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.131 _refine_diff_density_min -0.752 _refine_diff_density_rms 0.182 # Attachment '1c_revised.cif' data_(DIPSe)3(SbF6)1.33(CH2Cl2)1.2 _database_code_depnum_ccdc_archive 'CCDC 294688' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25.2 H8.40 Cl2.40 F8 I6 N6 Sb1.33 Se12' _chemical_formula_weight 2503.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M P6(3)/mcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, z+1/2' 'y, -x+y, z+1/2' 'x-y, x, z+1/2' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-y, -x, -z' '-x+y, y, -z' 'x, x-y, -z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' 'x, y, -z-1/2' '-y, x-y, -z-1/2' '-x+y, -x, -z-1/2' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' 'y, x, z' 'x-y, -y, z' '-x, -x+y, z' _cell_length_a 20.4542(17) _cell_length_b 20.4542(17) _cell_length_c 7.2485(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 2626.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 2906 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 23.55 _exptl_crystal_description rod _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 3.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2235 _exptl_absorpt_coefficient_mu 12.805 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2497 _exptl_absorpt_correction_T_max 0.7000 _exptl_absorpt_process_details 'SADABS; Sheldrick 1996' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293 _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 8.366 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14629 _diffrn_reflns_av_R_equivalents 0.1042 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 28.27 _reflns_number_total 1194 _reflns_number_gt 889 _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^)+(0.0788P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1194 _refine_ls_number_parameters 88 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.1285 _refine_ls_wR_factor_gt 0.1004 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.0000 0.0000 0.1097(9) 0.0600(13) Uani 0.33 6 d SPD . . F1 F -0.0716(6) 0.0000 0.2500 0.094(7) Uani 0.67 4 d SPDU . . F2 F 0.0723(14) 0.0000 -0.028(6) 0.113(12) Uani 0.33 2 d SPDU . . Sb2 Sb 0.6667 0.3333 0.124(3) 0.184(7) Uani 0.17 3 d SPDU . 1 F3 F 0.5841(12) 0.270(2) 0.2500 0.129(14) Uani 0.33 2 d SPDU . 1 F4 F 0.6232(5) 0.3768(5) 0.0000 0.217(17) Uani 0.33 2 d SPDU A 1 C1 C 0.6437(6) 0.6066(6) 0.7500 0.030(2) Uani 1 2 d S . . C2 C 0.4922(8) 0.4922(8) 0.7500 0.033(3) Uani 1 4 d S . . C3 C 0.4290(7) 0.4290(7) 0.7500 0.030(3) Uani 1 4 d S . . C4 C 0.3185(5) 0.2791(5) 0.7500 0.028(2) Uani 1 2 d S . . C5 C 0.2068(6) 0.1687(6) 0.7500 0.054(4) Uani 1 2 d S . . H5A H 0.1791 0.1151 0.7500 0.065 Uiso 1 2 calc SR . . C1T C 0.6667 0.3333 0.0000 0.193(14) Uani 0.60 6 d SPDU . 2 Cl1T Cl 0.7170(4) 0.4340(9) 0.0000 0.195(10) Uani 0.40 2 d SPDU B 2 I1 I 0.76001(4) 0.65161(4) 0.7500 0.0333(3) Uani 1 2 d S . . N1 N 0.2830(5) 0.2043(5) 0.7500 0.041(2) Uani 1 2 d S . . Se1 Se 0.58854(6) 0.49898(6) 0.7500 0.0339(3) Uani 1 2 d S . . Se2 Se 0.42507(6) 0.33409(6) 0.7500 0.0324(3) Uani 1 2 d S . . 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 Sb1 0.0329(12) 0.0329(12) 0.114(4) 0.000 0.000 0.0165(6) F1 0.067(9) 0.057(11) 0.15(2) 0.000 0.000 0.028(5) F2 0.102(16) 0.112(19) 0.13(2) 0.000 0.026(17) 0.056(10) Sb2 0.124(6) 0.124(6) 0.302(19) 0.000 0.000 0.062(3) F3 0.09(2) 0.10(2) 0.15(3) 0.000 0.000 0.016(17) F4 0.196(17) 0.196(17) 0.27(3) 0.005(14) 0.005(14) 0.107(17) C1 0.022(5) 0.027(5) 0.034(6) 0.000 0.000 0.006(4) C2 0.035(6) 0.035(6) 0.034(9) 0.000 0.000 0.020(7) C3 0.030(6) 0.030(6) 0.036(9) 0.000 0.000 0.019(6) C4 0.026(5) 0.028(5) 0.031(6) 0.000 0.000 0.013(4) C5 0.029(6) 0.023(5) 0.106(12) 0.000 0.000 0.009(5) C1T 0.164(15) 0.164(15) 0.25(2) 0.000 0.000 0.082(7) Cl1T 0.155(13) 0.157(16) 0.27(2) 0.000 -0.039(17) 0.079(8) I1 0.0243(4) 0.0335(4) 0.0382(5) 0.000 0.000 0.0116(3) N1 0.030(5) 0.022(4) 0.068(7) 0.000 0.000 0.009(4) Se1 0.0263(5) 0.0264(5) 0.0489(8) 0.000 0.000 0.0131(4) Se2 0.0251(5) 0.0284(5) 0.0456(7) 0.000 0.000 0.0147(4) _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 Sb1 Sb1 1.590(13) 13 ? Sb1 F2 1.59(4) 15 ? Sb1 F2 1.59(4) 14 ? Sb1 F2 1.59(4) 13 ? Sb1 F2 1.783(10) 3 ? Sb1 F2 1.783(10) 2 ? Sb1 F2 1.783(10) . ? Sb1 F1 1.783(10) 3 ? Sb1 F1 1.783(10) . ? Sb1 F1 1.783(10) 2 ? Sb1 Sb1 2.034(13) 16_556 ? F1 F2 1.61(4) 13 ? F1 F2 1.61(4) 4 ? F1 Sb1 1.783(10) 16_556 ? F2 F2 1.532(13) 14 ? F2 F2 1.532(13) 15 ? F2 Sb1 1.59(4) 13 ? F2 F1 1.61(4) 13 ? Sb2 F3 1.783(10) 2_655 ? Sb2 F3 1.783(10) . ? Sb2 F3 1.783(10) 3_665 ? Sb2 F4 1.783(10) 2_655 ? Sb2 F4 1.783(10) 3_665 ? Sb2 F4 1.783(10) . ? Sb2 Sb2 1.79(4) 10_665 ? Sb2 Sb2 1.83(4) 16_556 ? F3 Sb2 1.783(10) 16_556 ? F4 Sb2 1.783(10) 10_665 ? C1 C1 1.32(2) 7_556 ? C1 Se1 1.906(10) . ? C1 I1 2.078(10) . ? C2 C3 1.29(2) . ? C2 Se1 1.905(9) . ? C2 Se1 1.905(9) 7_556 ? C3 Se2 1.902(8) . ? C3 Se2 1.902(8) 7_556 ? C4 N1 1.326(13) . ? C4 C4 1.39(2) 7_556 ? C4 Se2 1.889(10) . ? C5 C5 1.35(2) 7_556 ? C5 N1 1.352(15) . ? C5 H5A 0.9500 . ? C1T Cl1T 1.784(16) 3_665 ? C1T Cl1T 1.784(16) 2_655 ? C1T Cl1T 1.784(16) . ? 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 Sb1 Sb1 F2 68.1(11) 13 15 ? Sb1 Sb1 F2 68.1(11) 13 14 ? F2 Sb1 F2 107.0(12) 15 14 ? Sb1 Sb1 F2 68.1(11) 13 13 ? F2 Sb1 F2 107.0(12) 15 13 ? F2 Sb1 F2 107.0(12) 14 13 ? Sb1 Sb1 F2 56.0(16) 13 3 ? F2 Sb1 F2 124.1(8) 15 3 ? F2 Sb1 F2 53.6(4) 14 3 ? F2 Sb1 F2 53.6(4) 13 3 ? Sb1 Sb1 F2 56.0(16) 13 2 ? F2 Sb1 F2 53.6(4) 15 2 ? F2 Sb1 F2 124.1(8) 14 2 ? F2 Sb1 F2 53.6(4) 13 2 ? F2 Sb1 F2 92(2) 3 2 ? Sb1 Sb1 F2 56.0(16) 13 . ? F2 Sb1 F2 53.6(4) 15 . ? F2 Sb1 F2 53.6(4) 14 . ? F2 Sb1 F2 124.1(8) 13 . ? F2 Sb1 F2 92(2) 3 . ? F2 Sb1 F2 92(2) 2 . ? Sb1 Sb1 F1 124.8(3) 13 3 ? F2 Sb1 F1 56.6(11) 15 3 ? F2 Sb1 F1 126.4(5) 14 3 ? F2 Sb1 F1 126.4(5) 13 3 ? F2 Sb1 F1 179.2(17) 3 3 ? F2 Sb1 F1 88.8(11) 2 3 ? F2 Sb1 F1 88.8(11) . 3 ? Sb1 Sb1 F1 124.8(3) 13 . ? F2 Sb1 F1 126.4(5) 15 . ? F2 Sb1 F1 126.4(5) 14 . ? F2 Sb1 F1 56.6(11) 13 . ? F2 Sb1 F1 88.8(11) 3 . ? F2 Sb1 F1 88.8(11) 2 . ? F2 Sb1 F1 179.2(16) . . ? F1 Sb1 F1 90.7(5) 3 . ? Sb1 Sb1 F1 124.8(3) 13 2 ? F2 Sb1 F1 126.4(5) 15 2 ? F2 Sb1 F1 56.6(11) 14 2 ? F2 Sb1 F1 126.4(5) 13 2 ? F2 Sb1 F1 88.8(11) 3 2 ? F2 Sb1 F1 179.2(16) 2 2 ? F2 Sb1 F1 88.8(11) . 2 ? F1 Sb1 F1 90.7(5) 3 2 ? F1 Sb1 F1 90.7(5) . 2 ? Sb1 Sb1 Sb1 180.0 13 16_556 ? F2 Sb1 Sb1 111.9(11) 15 16_556 ? F2 Sb1 Sb1 111.9(11) 14 16_556 ? F2 Sb1 Sb1 111.9(11) 13 16_556 ? F2 Sb1 Sb1 124.0(16) 3 16_556 ? F2 Sb1 Sb1 124.0(16) 2 16_556 ? F2 Sb1 Sb1 124.0(16) . 16_556 ? F1 Sb1 Sb1 55.2(3) 3 16_556 ? F1 Sb1 Sb1 55.2(3) . 16_556 ? F1 Sb1 Sb1 55.2(3) 2 16_556 ? F2 F1 F2 179(2) 13 4 ? F2 F1 Sb1 125.3(11) 13 16_556 ? F2 F1 Sb1 55.7(9) 4 16_556 ? F2 F1 Sb1 55.7(9) 13 . ? F2 F1 Sb1 125.3(11) 4 . ? Sb1 F1 Sb1 69.6(6) 16_556 . ? F2 F2 F2 113(3) 14 15 ? F2 F2 Sb1 69.5(12) 14 13 ? F2 F2 Sb1 69.5(12) 15 13 ? F2 F2 F1 105(4) 14 13 ? F2 F2 F1 105(4) 15 13 ? Sb1 F2 F1 68(2) 13 13 ? F2 F2 Sb1 56.8(15) 14 . ? F2 F2 Sb1 56.8(15) 15 . ? Sb1 F2 Sb1 55.9(8) 13 . ? F1 F2 Sb1 123(3) 13 . ? F3 Sb2 F3 96.0(10) 2_655 . ? F3 Sb2 F3 96.0(10) 2_655 3_665 ? F3 Sb2 F3 96.0(10) . 3_665 ? F3 Sb2 F4 95.2(14) 2_655 2_655 ? F3 Sb2 F4 73.5(11) . 2_655 ? F3 Sb2 F4 165.4(17) 3_665 2_655 ? F3 Sb2 F4 73.5(11) 2_655 3_665 ? F3 Sb2 F4 165.4(17) . 3_665 ? F3 Sb2 F4 95.2(14) 3_665 3_665 ? F4 Sb2 F4 96.9(10) 2_655 3_665 ? F3 Sb2 F4 165.4(17) 2_655 . ? F3 Sb2 F4 95.2(14) . . ? F3 Sb2 F4 73.5(11) 3_665 . ? F4 Sb2 F4 96.9(10) 2_655 . ? F4 Sb2 F4 96.9(10) 3_665 . ? F3 Sb2 Sb2 120.9(7) 2_655 10_665 ? F3 Sb2 Sb2 120.9(7) . 10_665 ? F3 Sb2 Sb2 120.9(7) 3_665 10_665 ? F4 Sb2 Sb2 59.8(7) 2_655 10_665 ? F4 Sb2 Sb2 59.8(7) 3_665 10_665 ? F4 Sb2 Sb2 59.8(7) . 10_665 ? F3 Sb2 Sb2 59.1(7) 2_655 16_556 ? F3 Sb2 Sb2 59.1(7) . 16_556 ? F3 Sb2 Sb2 59.1(7) 3_665 16_556 ? F4 Sb2 Sb2 120.2(7) 2_655 16_556 ? F4 Sb2 Sb2 120.2(7) 3_665 16_556 ? F4 Sb2 Sb2 120.2(7) . 16_556 ? Sb2 Sb2 Sb2 180.000(5) 10_665 16_556 ? Sb2 F3 Sb2 61.8(15) 16_556 . ? Sb2 F4 Sb2 60.4(15) 10_665 . ? C1 C1 Se1 119.2(3) 7_556 . ? C1 C1 I1 127.4(3) 7_556 . ? Se1 C1 I1 113.4(5) . . ? C3 C2 Se1 123.6(4) . . ? C3 C2 Se1 123.6(4) . 7_556 ? Se1 C2 Se1 112.8(8) . 7_556 ? C2 C3 Se2 122.1(4) . . ? C2 C3 Se2 122.1(4) . 7_556 ? Se2 C3 Se2 115.8(8) . 7_556 ? N1 C4 C4 121.8(6) . 7_556 ? N1 C4 Se2 119.3(8) . . ? C4 C4 Se2 119.0(3) 7_556 . ? C5 C5 N1 122.2(6) 7_556 . ? C5 C5 H5A 118.9 7_556 . ? N1 C5 H5A 118.9 . . ? Cl1T C1T Cl1T 120.000(1) 3_665 2_655 ? Cl1T C1T Cl1T 120.000(2) 3_665 . ? Cl1T C1T Cl1T 120.000(1) 2_655 . ? C4 N1 C5 116.0(10) . . ? C2 Se1 C1 94.4(5) . . ? C4 Se2 C3 93.1(5) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 1.315 _refine_diff_density_min -0.916 _refine_diff_density_rms 0.211