# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2003 _publ_contact_author_name 'Dr Tito Trindade' _publ_contact_author_address ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; _publ_contact_author_email 'ttrindade@dq.ua.pt' _publ_contact_author_fax '+351 234 370084' _publ_contact_author_phone '+351 234 370726' _journal_name_full 'Journal of Materials Chemistry' loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Monteiro, Olinda C.' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Trindade, Tito' . ; Department of Chemistry University of Aveiro CICECO 3810-193 Aveiro Portugal ; 'Almeida Paz, Filipe A.' . ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW United Kingdom ; 'Klinowski, Jacek' . ; Department of Chemistry University of Cambridge Lensfield Road Cambridge CB2 1EW United Kingdom ; 'Waters, John' . ; The Manchester Materials Science Centre Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL United Kingdom ; 'O'Brien, Paul' . ; The Manchester Materials Science Centre Department of Chemistry University of Manchester Oxford Road Manchester M13 9PL United Kingdom ; data_I _audit_creation_method 'SHELXL-97, manual editing plus enCIFer' _audit_creation_date '1st of September, 2003' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H54 Bi N3 Se6' _chemical_formula_sum 'C27 H54 Bi N3 Se6' _chemical_formula_weight 1103.47 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' 'Bi' 'Bi' -4.1077 10.2566 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.39620(10) _cell_length_b 11.97520(10) _cell_length_c 28.0596(4) _cell_angle_alpha 81.8236(5) _cell_angle_beta 86.7661(4) _cell_angle_gamma 86.6659(8) _cell_volume 3779.51(7) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 35639 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.939 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2096 _exptl_absorpt_coefficient_mu 10.463 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.143 _exptl_absorpt_correction_T_max 0.283 _exptl_absorpt_process_details ; Multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; Common bond length restraints were used for the -(CH2)3-CH3 chains. Four -(CH2)-CH3 terminal groups have been modelled with common isotropic temperature factors. One terminal -CH3 group in one of these chains is disordered over two sites. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_standards_number 0 _diffrn_reflns_number 34123 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0688 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 27.49 _reflns_number_total 16822 _reflns_number_gt 12557 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Collect (Nonius 1998)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare at al. 1994)' _computing_structure_refinement 'SHELXTL (Bruker 2001)' _computing_molecular_graphics 'SHELXTL (Bruker 2001)' _computing_publication_material 'SHELXTL (Bruker 2001)' _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^)+(0.0534P)^2^+36.7877P] 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 16822 _refine_ls_number_parameters 633 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0585 _refine_ls_wR_factor_ref 0.1477 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.037 _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 Bi1 Bi 0.43897(3) 0.55601(3) 0.580343(12) 0.03245(9) Uani 1 1 d . . . Se1 Se 0.21224(8) 0.64831(9) 0.59967(4) 0.0452(3) Uani 1 1 d . . . Se2 Se 0.24708(9) 0.41960(9) 0.55002(4) 0.0463(3) Uani 1 1 d . . . Se3 Se 0.65093(8) 0.43220(9) 0.63210(3) 0.0410(2) Uani 1 1 d . . . Se4 Se 0.46354(8) 0.60249(10) 0.67858(4) 0.0430(2) Uani 1 1 d . . . Se5 Se 0.54358(9) 0.76602(9) 0.55724(4) 0.0442(2) Uani 1 1 d . . . Se6 Se 0.41392(8) 0.65032(8) 0.47981(3) 0.0342(2) Uani 1 1 d . . . C1 C 0.1487(8) 0.5259(8) 0.5767(3) 0.034(2) Uani 1 1 d . . . C2 C 0.5999(8) 0.5080(8) 0.6845(3) 0.035(2) Uani 1 1 d . . . C3 C 0.5103(8) 0.7623(8) 0.4920(3) 0.036(2) Uani 1 1 d . . . N1 N 0.0320(6) 0.5164(6) 0.5806(3) 0.0408(19) Uani 1 1 d D . . N2 N 0.5512(7) 0.8393(7) 0.4578(3) 0.0408(19) Uani 1 1 d D . . N3 N 0.6575(6) 0.4918(6) 0.7251(3) 0.0367(18) Uani 1 1 d D . . C4 C -0.0483(8) 0.5924(8) 0.6069(3) 0.043(2) Uani 1 1 d D . . H4A H -0.0042 0.6211 0.6317 0.052 Uiso 1 1 calc R . . H4B H -0.1132 0.5486 0.6237 0.052 Uiso 1 1 calc R . . C5 C -0.0991(9) 0.6908(8) 0.5737(4) 0.047(3) Uani 1 1 d D . . H5A H -0.0392 0.7153 0.5480 0.057 Uiso 1 1 calc R . . H5B H -0.1673 0.6664 0.5583 0.057 Uiso 1 1 calc R . . C6 C -0.1375(14) 0.7882(10) 0.5995(5) 0.081(5) Uani 1 1 d D . . H6A H -0.0662 0.8243 0.6072 0.098 Uiso 1 1 calc R . . H6B H -0.1818 0.8443 0.5770 0.098 Uiso 1 1 calc R . . C7 C -0.2095(13) 0.7642(13) 0.6435(5) 0.081(4) Uani 1 1 d D . . H7A H -0.2293 0.8344 0.6570 0.122 Uiso 1 1 calc R . . H7B H -0.1660 0.7111 0.6668 0.122 Uiso 1 1 calc R . . H7C H -0.2820 0.7307 0.6365 0.122 Uiso 1 1 calc R . . C8 C -0.0260(8) 0.4225(8) 0.5631(4) 0.043(2) Uani 1 1 d D . . H8A H 0.0184 0.4012 0.5341 0.052 Uiso 1 1 calc R . . H8B H -0.1068 0.4483 0.5539 0.052 Uiso 1 1 calc R . . C9 C -0.0313(9) 0.3205(7) 0.6018(4) 0.045(2) Uani 1 1 d D . . H9A H 0.0490 0.2979 0.6126 0.055 Uiso 1 1 calc R . . H9B H -0.0803 0.3403 0.6299 0.055 Uiso 1 1 calc R . . C10 C -0.0826(10) 0.2231(9) 0.5828(4) 0.059(3) Uani 1 1 d D . . H10A H -0.0320 0.2012 0.5554 0.070 Uiso 1 1 calc R . . H10B H -0.1618 0.2464 0.5710 0.070 Uiso 1 1 calc R . . C11 C -0.0913(13) 0.1222(10) 0.6229(5) 0.076(4) Uani 1 1 d D . . H11A H -0.1245 0.0592 0.6103 0.114 Uiso 1 1 calc R . . H11B H -0.1423 0.1439 0.6497 0.114 Uiso 1 1 calc R . . H11C H -0.0127 0.0990 0.6343 0.114 Uiso 1 1 calc R . . C12 C 0.7677(8) 0.4194(7) 0.7310(3) 0.040(2) Uani 1 1 d D . . H12A H 0.8148 0.4461 0.7553 0.048 Uiso 1 1 calc R . . H12B H 0.8147 0.4269 0.7000 0.048 Uiso 1 1 calc R . . C13 C 0.7433(9) 0.2958(7) 0.7466(4) 0.045(2) Uani 1 1 d D . . H13A H 0.6974 0.2684 0.7221 0.054 Uiso 1 1 calc R . . H13B H 0.6958 0.2879 0.7774 0.054 Uiso 1 1 calc R . . C14 C 0.8577(10) 0.2244(9) 0.7529(5) 0.062(3) Uani 1 1 d D . . H14A H 0.9036 0.2515 0.7775 0.074 Uiso 1 1 calc R . . H14B H 0.9053 0.2319 0.7221 0.074 Uiso 1 1 calc R . . C15 C 0.8314(15) 0.1010(9) 0.7685(6) 0.089(5) Uani 1 1 d D . . H15A H 0.9055 0.0557 0.7727 0.133 Uiso 1 1 calc R . . H15B H 0.7871 0.0741 0.7438 0.133 Uiso 1 1 calc R . . H15C H 0.7846 0.0937 0.7991 0.133 Uiso 1 1 calc R . . C16 C 0.6189(9) 0.5510(8) 0.7669(3) 0.042(2) Uani 1 1 d D . . H16A H 0.6442 0.5050 0.7971 0.050 Uiso 1 1 calc R . . H16B H 0.5319 0.5604 0.7689 0.050 Uiso 1 1 calc R . . C17 C 0.6711(10) 0.6656(8) 0.7618(3) 0.049(3) Uani 1 1 d D . . H17A H 0.7580 0.6556 0.7594 0.058 Uiso 1 1 calc R . . H17B H 0.6455 0.7111 0.7316 0.058 Uiso 1 1 calc R . . C18 C 0.6354(11) 0.7283(9) 0.8032(4) 0.056(3) Uani 1 1 d D . . H18A H 0.6565 0.6812 0.8337 0.067 Uiso 1 1 calc R . . H18B H 0.5491 0.7433 0.8043 0.067 Uiso 1 1 calc R . . C19 C 0.6955(14) 0.8388(10) 0.7985(5) 0.077(4) Uani 1 1 d D . . H19A H 0.6706 0.8782 0.8260 0.115 Uiso 1 1 calc R . . H19B H 0.6737 0.8860 0.7685 0.115 Uiso 1 1 calc R . . H19C H 0.7810 0.8239 0.7979 0.115 Uiso 1 1 calc R . . C20 C 0.6253(8) 0.9323(8) 0.4668(4) 0.048(3) Uani 1 1 d D . . H20A H 0.6096 0.9474 0.5004 0.058 Uiso 1 1 calc R . . H20B H 0.6027 1.0019 0.4451 0.058 Uiso 1 1 calc R . . C21 C 0.7551(8) 0.9044(10) 0.4587(6) 0.069(4) Uani 1 1 d D . . H21A H 0.7674 0.8638 0.4303 0.083 Uiso 1 1 calc R . . H21B H 0.7838 0.8536 0.4871 0.083 Uiso 1 1 calc R . . C22 C 0.8261(13) 1.0105(14) 0.4505(7) 0.104(6) Uani 1 1 d D . . H22A H 0.9093 0.9889 0.4424 0.125 Uiso 1 1 calc R . . H22B H 0.7957 1.0620 0.4226 0.125 Uiso 1 1 calc R . . C23 C 0.8210(18) 1.0702(16) 0.4923(7) 0.120(7) Uani 1 1 d D . . H23A H 0.8682 1.1369 0.4852 0.180 Uiso 1 1 calc R . . H23B H 0.8522 1.0201 0.5199 0.180 Uiso 1 1 calc R . . H23C H 0.7391 1.0938 0.5000 0.180 Uiso 1 1 calc R . . C24 C 0.5263(8) 0.8421(9) 0.4061(3) 0.044(2) Uani 1 1 d D . . H24A H 0.5152 0.7644 0.3997 0.053 Uiso 1 1 calc R . . H24B H 0.5947 0.8712 0.3858 0.053 Uiso 1 1 calc R . . C25 C 0.4172(8) 0.9161(10) 0.3924(3) 0.052(3) Uani 1 1 d D . . H25A H 0.3462 0.8769 0.4060 0.062 Uiso 1 1 calc R . . H25B H 0.4187 0.9875 0.4063 0.062 Uiso 1 1 calc R . . C26 C 0.4111(11) 0.9425(11) 0.3384(4) 0.065(3) Uani 1 1 d D . . H26A H 0.4260 0.8717 0.3240 0.078 Uiso 1 1 calc R . . H26B H 0.3308 0.9728 0.3304 0.078 Uiso 1 1 calc R . . C27 C 0.4982(13) 1.0263(15) 0.3164(5) 0.101(6) Uani 1 1 d D . . H27A H 0.4907 1.0406 0.2814 0.151 Uiso 1 1 calc R . . H27B H 0.5781 0.9961 0.3235 0.151 Uiso 1 1 calc R . . H27C H 0.4829 1.0971 0.3299 0.151 Uiso 1 1 calc R . . Bi2 Bi 0.90858(3) 0.42066(3) 0.930032(12) 0.03490(10) Uani 1 1 d . . . Se7 Se 0.75555(9) 0.29955(10) 0.88159(4) 0.0465(3) Uani 1 1 d . . . Se8 Se 0.65797(8) 0.47619(10) 0.95163(4) 0.0448(2) Uani 1 1 d . . . Se9 Se 0.92602(10) 0.21534(11) 0.99465(5) 0.0637(4) Uani 1 1 d . . . Se10 Se 1.13149(8) 0.39095(9) 0.99044(3) 0.0368(2) Uani 1 1 d . . . Se11 Se 1.08057(9) 0.36169(10) 0.85590(4) 0.0459(3) Uani 1 1 d . . . Se12 Se 0.93042(11) 0.59999(12) 0.84560(4) 0.0614(3) Uani 1 1 d . . . N4 N 1.1306(6) 0.1785(7) 1.0463(3) 0.0406(19) Uani 1 1 d D . . N6 N 0.5175(7) 0.3674(7) 0.8962(3) 0.046(2) Uani 1 1 d D . . N5 N 1.0990(8) 0.5330(8) 0.7777(3) 0.059(3) Uani 1 1 d D . . C28 C 0.6274(8) 0.3780(9) 0.9081(3) 0.039(2) Uani 1 1 d . . . C29 C 1.0719(8) 0.2522(9) 1.0159(3) 0.036(2) Uani 1 1 d . . . C30 C 1.0443(9) 0.5023(10) 0.8205(4) 0.050(3) Uani 1 1 d . . . C31 C 0.4136(8) 0.4318(9) 0.9154(4) 0.054(3) Uani 1 1 d D . . H31A H 0.4265 0.4439 0.9488 0.064 Uiso 1 1 calc R . . H31B H 0.3425 0.3877 0.9160 0.064 Uiso 1 1 calc R . . C32 C 0.3946(9) 0.5447(9) 0.8842(4) 0.059(3) Uani 1 1 d D . . H32A H 0.4673 0.5869 0.8822 0.070 Uiso 1 1 calc R . . H32B H 0.3777 0.5323 0.8512 0.070 Uiso 1 1 calc R . . C33 C 0.2941(17) 0.6132(14) 0.9046(8) 0.127(4) Uiso 1 1 d D . . H33A H 0.3065 0.6177 0.9389 0.153 Uiso 1 1 calc R . . H33B H 0.2198 0.5753 0.9029 0.153 Uiso 1 1 calc R . . C34 C 0.284(3) 0.7311(17) 0.8770(11) 0.202(7) Uiso 1 1 d D . . H34A H 0.2183 0.7739 0.8911 0.303 Uiso 1 1 calc R . . H34B H 0.2702 0.7267 0.8432 0.303 Uiso 1 1 calc R . . H34C H 0.3572 0.7690 0.8790 0.303 Uiso 1 1 calc R . . C35 C 0.4902(11) 0.2932(10) 0.8603(4) 0.065(4) Uani 1 1 d D . . H35A H 0.5599 0.2842 0.8383 0.078 Uiso 1 1 calc R . . H35B H 0.4247 0.3289 0.8409 0.078 Uiso 1 1 calc R . . C36 C 0.4565(15) 0.1795(11) 0.8851(6) 0.107(7) Uani 1 1 d D . . H36A H 0.5284 0.1381 0.8979 0.129 Uiso 1 1 calc R . . H36B H 0.4025 0.1909 0.9131 0.129 Uiso 1 1 calc R . . C37 C 0.4000(18) 0.1077(15) 0.8558(7) 0.127(4) Uiso 1 1 d D . . H37A H 0.3778 0.0379 0.8768 0.153 Uiso 1 1 calc R . . H37B H 0.3265 0.1478 0.8441 0.153 Uiso 1 1 calc R . . C38 C 0.469(3) 0.076(3) 0.8151(9) 0.202(7) Uiso 1 1 d D . . H38A H 0.4274 0.0221 0.8002 0.303 Uiso 1 1 calc R . . H38C H 0.5450 0.0417 0.8258 0.303 Uiso 1 1 calc R . . H38B H 0.4824 0.1437 0.7916 0.303 Uiso 1 1 calc R . . C39 C 1.0882(9) 0.0647(9) 1.0649(4) 0.049(3) Uani 1 1 d D . . H39A H 1.1567 0.0109 1.0710 0.059 Uiso 1 1 calc R . . H39B H 1.0422 0.0385 1.0401 0.059 Uiso 1 1 calc R . . C40 C 1.0130(10) 0.0650(10) 1.1105(4) 0.062(3) Uani 1 1 d D A . H40A H 0.9504 0.1258 1.1056 0.075 Uiso 1 1 calc R . . H40B H 1.0619 0.0817 1.1365 0.075 Uiso 1 1 calc R . . C41 C 0.9569(12) -0.0464(12) 1.1263(5) 0.090(5) Uani 1 1 d D . . H41A H 0.9176 -0.0461 1.1587 0.108 Uiso 0.69(3) 1 calc PR A 3 H41B H 1.0183 -0.1086 1.1284 0.108 Uiso 0.69(3) 1 calc PR A 3 H41C H 1.0173 -0.1095 1.1286 0.108 Uiso 0.31(3) 1 calc PR A 4 H41D H 0.8986 -0.0597 1.1031 0.108 Uiso 0.31(3) 1 calc PR A 4 C42' C 0.8654(16) -0.0658(17) 1.0897(8) 0.099(11) Uani 0.69(3) 1 d PD A 3 H42D H 0.8302 -0.1386 1.1000 0.149 Uiso 0.69(3) 1 calc PR A 3 H42E H 0.9046 -0.0659 1.0577 0.149 Uiso 0.69(3) 1 calc PR A 3 H42F H 0.8037 -0.0051 1.0884 0.149 Uiso 0.69(3) 1 calc PR A 3 C42 C 0.895(3) -0.036(3) 1.1772(9) 0.059(13) Uani 0.31(3) 1 d PD A 4 H42A H 0.8561 -0.1059 1.1894 0.089 Uiso 0.31(3) 1 calc PR A 4 H42B H 0.8365 0.0275 1.1743 0.089 Uiso 0.31(3) 1 calc PR A 4 H42C H 0.9541 -0.0231 1.1996 0.089 Uiso 0.31(3) 1 calc PR A 4 C43 C 1.2457(7) 0.2046(10) 1.0642(4) 0.050(3) Uani 1 1 d D . . H43A H 1.2526 0.1680 1.0979 0.059 Uiso 1 1 calc R . . H43B H 1.2484 0.2872 1.0638 0.059 Uiso 1 1 calc R . . C44 C 1.3485(7) 0.1636(10) 1.0334(4) 0.048(3) Uani 1 1 d D . . H44A H 1.3466 0.0809 1.0341 0.058 Uiso 1 1 calc R . . H44B H 1.3417 0.1998 0.9997 0.058 Uiso 1 1 calc R . . C45 C 1.4640(8) 0.1918(13) 1.0519(5) 0.073(4) Uani 1 1 d D . . H45A H 1.4686 0.1583 1.0861 0.087 Uiso 1 1 calc R . . H45B H 1.4664 0.2747 1.0502 0.087 Uiso 1 1 calc R . . C46 C 1.5698(9) 0.1482(14) 1.0232(6) 0.080(4) Uani 1 1 d D . . H46A H 1.6423 0.1687 1.0362 0.121 Uiso 1 1 calc R . . H46B H 1.5664 0.1820 0.9893 0.121 Uiso 1 1 calc R . . H46C H 1.5690 0.0658 1.0254 0.121 Uiso 1 1 calc R . . C47 C 1.1955(10) 0.4607(11) 0.7581(4) 0.068(4) Uani 1 1 d D . . H47A H 1.2338 0.4132 0.7853 0.081 Uiso 1 1 calc R . . H47B H 1.2553 0.5096 0.7405 0.081 Uiso 1 1 calc R . . C48 C 1.1533(13) 0.3858(12) 0.7250(5) 0.084(5) Uani 1 1 d D . . H48A H 1.1174 0.4314 0.6968 0.101 Uiso 1 1 calc R . . H48B H 1.0941 0.3351 0.7420 0.101 Uiso 1 1 calc R . . C49 C 1.2661(16) 0.3152(16) 0.7086(8) 0.127(4) Uiso 1 1 d D . . H49A H 1.3057 0.3562 0.6796 0.153 Uiso 1 1 calc R . . H49B H 1.3226 0.3010 0.7346 0.153 Uiso 1 1 calc R . . C50 C 1.224(2) 0.2088(18) 0.6981(11) 0.202(7) Uiso 1 1 d D . . H50C H 1.2908 0.1607 0.6882 0.303 Uiso 1 1 calc R . . H50A H 1.1691 0.2242 0.6720 0.303 Uiso 1 1 calc R . . H50B H 1.1834 0.1701 0.7270 0.303 Uiso 1 1 calc R . . C51 C 1.0631(13) 0.6388(11) 0.7453(5) 0.079(4) Uani 1 1 d D . . H51A H 1.0691 0.6236 0.7114 0.095 Uiso 1 1 calc R . . H51B H 0.9799 0.6602 0.7532 0.095 Uiso 1 1 calc R . . C52 C 1.1374(16) 0.7352(12) 0.7499(7) 0.113(6) Uani 1 1 d D . . H52A H 1.2210 0.7154 0.7418 0.135 Uiso 1 1 calc R . . H52B H 1.1308 0.7527 0.7834 0.135 Uiso 1 1 calc R . . C53 C 1.0933(18) 0.8386(14) 0.7148(8) 0.127(4) Uiso 1 1 d D . . H53A H 1.0917 0.8183 0.6819 0.153 Uiso 1 1 calc R . . H53B H 1.0125 0.8632 0.7251 0.153 Uiso 1 1 calc R . . C54 C 1.175(3) 0.9324(18) 0.7152(11) 0.202(7) Uiso 1 1 d D . . H54A H 1.1486 0.9985 0.6930 0.303 Uiso 1 1 calc R . . H54B H 1.2550 0.9074 0.7049 0.303 Uiso 1 1 calc R . . H54C H 1.1757 0.9525 0.7478 0.303 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.02738(17) 0.0410(2) 0.02950(18) -0.00517(14) -0.00565(12) -0.00168(13) Se1 0.0318(5) 0.0494(6) 0.0592(7) -0.0246(5) -0.0069(4) 0.0030(4) Se2 0.0330(5) 0.0448(6) 0.0644(7) -0.0212(5) 0.0030(5) -0.0031(4) Se3 0.0359(5) 0.0587(6) 0.0299(5) -0.0116(4) -0.0080(4) 0.0055(4) Se4 0.0351(5) 0.0640(7) 0.0304(5) -0.0107(4) -0.0045(4) 0.0051(4) Se5 0.0518(6) 0.0445(6) 0.0397(6) -0.0094(4) -0.0170(4) -0.0071(5) Se6 0.0323(5) 0.0413(5) 0.0303(5) -0.0070(4) -0.0074(3) -0.0032(4) C1 0.030(4) 0.035(5) 0.036(5) -0.003(4) -0.006(4) 0.004(4) C2 0.032(5) 0.041(5) 0.031(5) -0.001(4) -0.006(4) -0.005(4) C3 0.028(4) 0.038(5) 0.040(5) -0.008(4) -0.004(4) 0.006(4) N1 0.032(4) 0.045(5) 0.049(5) -0.015(4) -0.009(4) 0.000(3) N2 0.042(5) 0.039(5) 0.041(5) -0.003(4) -0.002(4) -0.006(4) N3 0.040(4) 0.047(5) 0.025(4) -0.009(3) -0.003(3) -0.003(4) C4 0.034(5) 0.065(7) 0.031(5) -0.008(5) -0.009(4) -0.001(5) C5 0.040(5) 0.053(7) 0.050(6) -0.010(5) -0.009(5) 0.002(5) C6 0.105(12) 0.072(10) 0.070(10) -0.028(8) -0.025(9) 0.036(8) C7 0.078(10) 0.080(11) 0.085(11) -0.016(8) -0.001(8) 0.012(8) C8 0.032(5) 0.056(7) 0.045(6) -0.014(5) -0.008(4) -0.004(4) C9 0.032(5) 0.051(6) 0.055(7) -0.012(5) -0.005(4) -0.004(4) C10 0.040(6) 0.064(8) 0.077(9) -0.022(7) -0.006(6) -0.007(5) C11 0.067(9) 0.068(9) 0.093(11) -0.002(8) -0.011(8) -0.017(7) C12 0.035(5) 0.054(6) 0.032(5) -0.007(4) -0.007(4) 0.001(4) C13 0.057(6) 0.053(7) 0.027(5) -0.002(4) -0.011(4) -0.004(5) C14 0.073(8) 0.061(8) 0.050(7) -0.007(6) -0.017(6) 0.015(6) C15 0.123(14) 0.049(8) 0.092(12) -0.004(8) -0.016(10) 0.010(8) C16 0.044(6) 0.053(6) 0.028(5) -0.002(4) -0.009(4) -0.002(5) C17 0.059(7) 0.060(7) 0.031(5) -0.016(5) -0.010(5) -0.004(5) C18 0.074(8) 0.056(7) 0.040(6) -0.016(5) -0.015(5) 0.008(6) C19 0.113(12) 0.069(9) 0.052(8) -0.014(7) -0.028(8) 0.009(8) C20 0.050(6) 0.033(6) 0.063(7) -0.008(5) -0.003(5) -0.005(4) C21 0.038(6) 0.073(9) 0.100(11) -0.023(8) 0.000(6) -0.019(6) C22 0.069(10) 0.123(16) 0.126(17) -0.030(13) -0.007(10) -0.018(10) C23 0.123(16) 0.15(2) 0.090(14) -0.029(13) -0.029(12) -0.009(14) C24 0.049(6) 0.049(6) 0.034(5) -0.006(4) 0.006(4) -0.008(5) C25 0.038(6) 0.069(8) 0.049(7) -0.012(6) -0.001(5) -0.007(5) C26 0.070(8) 0.080(9) 0.046(7) -0.015(6) -0.013(6) 0.006(7) C27 0.085(11) 0.134(15) 0.064(10) 0.043(10) 0.013(8) 0.005(10) Bi2 0.02840(17) 0.0522(2) 0.02394(17) -0.00197(15) -0.00367(12) -0.00672(15) Se7 0.0366(5) 0.0676(7) 0.0409(6) -0.0237(5) -0.0074(4) -0.0036(5) Se8 0.0328(5) 0.0649(7) 0.0408(6) -0.0199(5) -0.0042(4) -0.0038(4) Se9 0.0497(6) 0.0710(8) 0.0667(8) 0.0233(6) -0.0274(6) -0.0279(6) Se10 0.0309(4) 0.0469(6) 0.0339(5) -0.0075(4) -0.0061(4) -0.0047(4) Se11 0.0428(5) 0.0599(7) 0.0326(5) -0.0025(5) 0.0032(4) 0.0033(5) Se12 0.0643(7) 0.0691(8) 0.0420(6) 0.0109(6) 0.0086(5) 0.0151(6) N4 0.036(4) 0.052(5) 0.034(4) -0.005(4) -0.009(3) -0.001(4) N6 0.034(4) 0.069(6) 0.037(5) -0.011(4) -0.005(3) -0.015(4) N5 0.048(5) 0.084(8) 0.041(5) 0.007(5) 0.009(4) -0.006(5) C28 0.037(5) 0.051(6) 0.029(5) -0.003(4) -0.003(4) -0.008(4) C29 0.028(4) 0.049(6) 0.028(5) -0.001(4) -0.002(3) -0.001(4) C30 0.044(6) 0.071(8) 0.034(6) -0.004(5) -0.005(4) -0.012(5) C31 0.028(5) 0.091(9) 0.042(6) -0.010(6) -0.002(4) -0.004(5) C32 0.042(6) 0.087(9) 0.048(7) -0.015(6) -0.006(5) 0.004(6) C35 0.045(6) 0.088(10) 0.072(9) -0.035(7) -0.018(6) -0.013(6) C36 0.090(12) 0.081(12) 0.162(19) -0.032(12) -0.056(12) -0.019(9) C39 0.048(6) 0.052(7) 0.047(7) 0.000(5) -0.011(5) -0.004(5) C40 0.062(8) 0.066(8) 0.051(7) 0.013(6) 0.003(6) -0.002(6) C41 0.066(9) 0.081(11) 0.107(13) 0.037(9) 0.008(9) -0.013(8) C42' 0.052(12) 0.077(15) 0.15(3) 0.037(15) 0.031(14) -0.009(10) C42 0.06(2) 0.07(3) 0.05(2) 0.002(19) -0.008(18) -0.02(2) C43 0.041(6) 0.068(8) 0.041(6) -0.005(5) -0.016(5) 0.001(5) C44 0.039(5) 0.053(7) 0.053(7) -0.014(5) 0.000(5) 0.002(5) C45 0.046(7) 0.091(11) 0.083(10) -0.014(8) -0.016(6) -0.002(7) C46 0.035(6) 0.097(11) 0.109(13) -0.017(9) 0.000(7) 0.004(7) C47 0.053(7) 0.096(11) 0.049(7) 0.003(7) 0.013(6) -0.014(7) C48 0.088(11) 0.105(13) 0.056(9) -0.004(8) 0.011(8) -0.006(9) C51 0.096(11) 0.096(11) 0.042(7) -0.001(7) 0.006(7) -0.007(9) C52 0.089(13) 0.118(16) 0.132(18) -0.012(13) -0.001(11) -0.023(11) _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 Bi1 Se1 2.8058(10) . no Bi1 Se5 2.8220(11) . no Bi1 Se6 2.9089(10) . no Bi1 Se4 2.9202(10) . no Bi1 Se2 3.0324(11) . no Bi1 Se3 3.0836(10) . no Se1 C1 1.881(10) . no Se2 C1 1.856(9) . no Se3 C2 1.884(10) . no Se4 C2 1.870(9) . no Se5 C3 1.897(10) . no Se6 C3 1.861(10) . no C1 N1 1.338(11) . no C2 N3 1.330(11) . no C3 N2 1.318(12) . no N1 C8 1.491(10) . no N1 C4 1.493(10) . no N2 C24 1.490(10) . no N2 C20 1.493(10) . no N3 C12 1.487(10) . no N3 C16 1.490(10) . no C4 C5 1.503(11) . no C4 H4A 0.9900 . no C4 H4B 0.9900 . no C5 C6 1.489(12) . no C5 H5A 0.9900 . no C5 H5B 0.9900 . no C6 C7 1.448(14) . no C6 H6A 0.9900 . no C6 H6B 0.9900 . no C7 H7A 0.9800 . no C7 H7B 0.9800 . no C7 H7C 0.9800 . no C8 C9 1.516(11) . no C8 H8A 0.9900 . no C8 H8B 0.9900 . no C9 C10 1.509(12) . no C9 H9A 0.9900 . no C9 H9B 0.9900 . no C10 C11 1.534(13) . no C10 H10A 0.9900 . no C10 H10B 0.9900 . no C11 H11A 0.9800 . no C11 H11B 0.9800 . no C11 H11C 0.9800 . no C12 C13 1.520(11) . no C12 H12A 0.9900 . no C12 H12B 0.9900 . no C13 C14 1.521(12) . no C13 H13A 0.9900 . no C13 H13B 0.9900 . no C14 C15 1.523(13) . no C14 H14A 0.9900 . no C14 H14B 0.9900 . no C15 H15A 0.9800 . no C15 H15B 0.9800 . no C15 H15C 0.9800 . no C16 C17 1.512(11) . no C16 H16A 0.9900 . no C16 H16B 0.9900 . no C17 C18 1.495(11) . no C17 H17A 0.9900 . no C17 H17B 0.9900 . no C18 C19 1.510(13) . no C18 H18A 0.9900 . no C18 H18B 0.9900 . no C19 H19A 0.9800 . no C19 H19B 0.9800 . no C19 H19C 0.9800 . no C20 C21 1.509(12) . no C20 H20A 0.9900 . no C20 H20B 0.9900 . no C21 C22 1.529(14) . no C21 H21A 0.9900 . no C21 H21B 0.9900 . no C22 C23 1.455(15) . no C22 H22A 0.9900 . no C22 H22B 0.9900 . no C23 H23A 0.9800 . no C23 H23B 0.9800 . no C23 H23C 0.9800 . no C24 C25 1.518(12) . no C24 H24A 0.9900 . no C24 H24B 0.9900 . no C25 C26 1.510(12) . no C25 H25A 0.9900 . no C25 H25B 0.9900 . no C26 C27 1.499(14) . no C26 H26A 0.9900 . no C26 H26B 0.9900 . no C27 H27A 0.9800 . no C27 H27B 0.9800 . no C27 H27C 0.9800 . no Bi2 Se9 2.8440(12) . no Bi2 Se7 2.8487(10) . no Bi2 Se11 2.9093(11) . no Bi2 Se8 2.9436(10) . no Bi2 Se12 2.9723(12) . no Bi2 Se10 3.1084(9) . no Se7 C28 1.867(10) . no Se8 C28 1.870(10) . no Se9 C29 1.894(9) . no Se10 C29 1.863(10) . no Se11 C30 1.867(12) . no Se12 C30 1.871(12) . no N4 C29 1.318(12) . no N4 C39 1.485(11) . no N4 C43 1.495(10) . no N6 C28 1.333(12) . no N6 C35 1.490(11) . no N6 C31 1.492(11) . no N5 C30 1.335(13) . no N5 C47 1.489(12) . no N5 C51 1.501(12) . no C31 C32 1.514(12) . no C31 H31A 0.9900 . no C31 H31B 0.9900 . no C32 C33 1.503(15) . no C32 H32A 0.9900 . no C32 H32B 0.9900 . no C33 C34 1.511(16) . no C33 H33A 0.9900 . no C33 H33B 0.9900 . no C34 H34A 0.9800 . no C34 H34B 0.9800 . no C34 H34C 0.9800 . no C35 C36 1.498(14) . no C35 H35A 0.9900 . no C35 H35B 0.9900 . no C36 C37 1.469(15) . no C36 H36A 0.9900 . no C36 H36B 0.9900 . no C37 C38 1.432(17) . no C37 H37A 0.9900 . no C37 H37B 0.9900 . no C38 H38A 0.9800 . no C38 H38C 0.9800 . no C38 H38B 0.9800 . no C39 C40 1.501(12) . no C39 H39A 0.9900 . no C39 H39B 0.9900 . no C40 C41 1.510(13) . no C40 H40A 0.9900 . no C40 H40B 0.9900 . no C41 C42' 1.553(16) . no C41 C42 1.575(18) . no C41 H41A 0.9900 . no C41 H41B 0.9900 . no C41 H41C 0.9900 . no C41 H41D 0.9900 . no C42' H42D 0.9800 . no C42' H42E 0.9800 . no C42' H42F 0.9800 . no C42 H42A 0.9800 . no C42 H42B 0.9800 . no C42 H42C 0.9800 . no C43 C44 1.514(12) . no C43 H43A 0.9900 . no C43 H43B 0.9900 . no C44 C45 1.514(12) . no C44 H44A 0.9900 . no C44 H44B 0.9900 . no C45 C46 1.521(13) . no C45 H45A 0.9900 . no C45 H45B 0.9900 . no C46 H46A 0.9800 . no C46 H46B 0.9800 . no C46 H46C 0.9800 . no C47 C48 1.494(14) . no C47 H47A 0.9900 . no C47 H47B 0.9900 . no C48 C49 1.581(15) . no C48 H48A 0.9900 . no C48 H48B 0.9900 . no C49 C50 1.462(17) . no C49 H49A 0.9900 . no C49 H49B 0.9900 . no C50 H50C 0.9800 . no C50 H50A 0.9800 . no C50 H50B 0.9800 . no C51 C52 1.495(15) . no C51 H51A 0.9900 . no C51 H51B 0.9900 . no C52 C53 1.546(15) . no C52 H52A 0.9900 . no C52 H52B 0.9900 . no C53 C54 1.505(17) . no C53 H53A 0.9900 . no C53 H53B 0.9900 . no C54 H54A 0.9800 . no C54 H54B 0.9800 . no C54 H54C 0.9800 . no 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 Se1 Bi1 Se5 95.29(3) . . no Se1 Bi1 Se6 87.79(3) . . no Se5 Bi1 Se6 68.02(3) . . no Se1 Bi1 Se4 80.13(3) . . no Se5 Bi1 Se4 82.08(3) . . no Se6 Bi1 Se4 146.55(3) . . no Se1 Bi1 Se2 67.28(3) . . no Se5 Bi1 Se2 141.83(3) . . no Se6 Bi1 Se2 77.27(3) . . no Se4 Bi1 Se2 124.57(3) . . no Se1 Bi1 Se3 141.15(3) . . no Se5 Bi1 Se3 95.77(3) . . no Se6 Bi1 Se3 130.77(3) . . no Se4 Bi1 Se3 64.76(3) . . no Se2 Bi1 Se3 119.40(3) . . no C1 Se1 Bi1 89.3(3) . . no C1 Se2 Bi1 83.0(3) . . no C2 Se3 Bi1 86.0(3) . . no C2 Se4 Bi1 91.2(3) . . no C3 Se5 Bi1 87.9(3) . . no C3 Se6 Bi1 86.0(3) . . no N1 C1 Se2 121.1(7) . . no N1 C1 Se1 118.7(7) . . no Se2 C1 Se1 120.2(5) . . no N3 C2 Se4 121.2(7) . . no N3 C2 Se3 120.8(7) . . no Se4 C2 Se3 118.0(5) . . no N2 C3 Se6 122.7(7) . . no N2 C3 Se5 120.1(7) . . no Se6 C3 Se5 117.1(5) . . no C1 N1 C8 122.3(8) . . no C1 N1 C4 122.4(8) . . no C8 N1 C4 115.0(7) . . no C3 N2 C24 122.7(8) . . no C3 N2 C20 123.9(8) . . no C24 N2 C20 113.4(8) . . no C2 N3 C12 122.9(8) . . no C2 N3 C16 121.6(8) . . no C12 N3 C16 115.3(7) . . no N1 C4 C5 112.2(8) . . no N1 C4 H4A 109.2 . . no C5 C4 H4A 109.2 . . no N1 C4 H4B 109.2 . . no C5 C4 H4B 109.2 . . no H4A C4 H4B 107.9 . . no C6 C5 C4 112.4(8) . . no C6 C5 H5A 109.1 . . no C4 C5 H5A 109.1 . . no C6 C5 H5B 109.1 . . no C4 C5 H5B 109.1 . . no H5A C5 H5B 107.9 . . no C7 C6 C5 117.0(11) . . no C7 C6 H6A 108.1 . . no C5 C6 H6A 108.1 . . no C7 C6 H6B 108.1 . . no C5 C6 H6B 108.1 . . no H6A C6 H6B 107.3 . . no C6 C7 H7A 109.5 . . no C6 C7 H7B 109.5 . . no H7A C7 H7B 109.5 . . no C6 C7 H7C 109.5 . . no H7A C7 H7C 109.5 . . no H7B C7 H7C 109.5 . . no N1 C8 C9 110.8(7) . . no N1 C8 H8A 109.5 . . no C9 C8 H8A 109.5 . . no N1 C8 H8B 109.5 . . no C9 C8 H8B 109.5 . . no H8A C8 H8B 108.1 . . no C10 C9 C8 110.6(8) . . no C10 C9 H9A 109.5 . . no C8 C9 H9A 109.5 . . no C10 C9 H9B 109.5 . . no C8 C9 H9B 109.5 . . no H9A C9 H9B 108.1 . . no C9 C10 C11 109.9(9) . . no C9 C10 H10A 109.7 . . no C11 C10 H10A 109.7 . . no C9 C10 H10B 109.7 . . no C11 C10 H10B 109.7 . . no H10A C10 H10B 108.2 . . no C10 C11 H11A 109.5 . . no C10 C11 H11B 109.5 . . no H11A C11 H11B 109.5 . . no C10 C11 H11C 109.5 . . no H11A C11 H11C 109.5 . . no H11B C11 H11C 109.5 . . no N3 C12 C13 112.1(7) . . no N3 C12 H12A 109.2 . . no C13 C12 H12A 109.2 . . no N3 C12 H12B 109.2 . . no C13 C12 H12B 109.2 . . no H12A C12 H12B 107.9 . . no C12 C13 C14 110.8(8) . . no C12 C13 H13A 109.5 . . no C14 C13 H13A 109.5 . . no C12 C13 H13B 109.5 . . no C14 C13 H13B 109.5 . . no H13A C13 H13B 108.1 . . no C13 C14 C15 110.0(10) . . no C13 C14 H14A 109.7 . . no C15 C14 H14A 109.7 . . no C13 C14 H14B 109.7 . . no C15 C14 H14B 109.7 . . no H14A C14 H14B 108.2 . . no C14 C15 H15A 109.5 . . no C14 C15 H15B 109.5 . . no H15A C15 H15B 109.5 . . no C14 C15 H15C 109.5 . . no H15A C15 H15C 109.5 . . no H15B C15 H15C 109.5 . . no N3 C16 C17 110.6(7) . . no N3 C16 H16A 109.5 . . no C17 C16 H16A 109.5 . . no N3 C16 H16B 109.5 . . no C17 C16 H16B 109.5 . . no H16A C16 H16B 108.1 . . no C18 C17 C16 112.6(9) . . no C18 C17 H17A 109.1 . . no C16 C17 H17A 109.1 . . no C18 C17 H17B 109.1 . . no C16 C17 H17B 109.1 . . no H17A C17 H17B 107.8 . . no C17 C18 C19 111.1(10) . . no C17 C18 H18A 109.4 . . no C19 C18 H18A 109.4 . . no C17 C18 H18B 109.4 . . no C19 C18 H18B 109.4 . . no H18A C18 H18B 108.0 . . no C18 C19 H19A 109.5 . . no C18 C19 H19B 109.5 . . no H19A C19 H19B 109.5 . . no C18 C19 H19C 109.5 . . no H19A C19 H19C 109.5 . . no H19B C19 H19C 109.5 . . no N2 C20 C21 112.5(8) . . no N2 C20 H20A 109.1 . . no C21 C20 H20A 109.1 . . no N2 C20 H20B 109.1 . . no C21 C20 H20B 109.1 . . no H20A C20 H20B 107.8 . . no C20 C21 C22 111.9(10) . . no C20 C21 H21A 109.2 . . no C22 C21 H21A 109.2 . . no C20 C21 H21B 109.2 . . no C22 C21 H21B 109.2 . . no H21A C21 H21B 107.9 . . no C23 C22 C21 112.9(13) . . no C23 C22 H22A 109.0 . . no C21 C22 H22A 109.0 . . no C23 C22 H22B 109.0 . . no C21 C22 H22B 109.0 . . no H22A C22 H22B 107.8 . . no C22 C23 H23A 109.5 . . no C22 C23 H23B 109.5 . . no H23A C23 H23B 109.5 . . no C22 C23 H23C 109.5 . . no H23A C23 H23C 109.5 . . no H23B C23 H23C 109.5 . . no N2 C24 C25 112.0(8) . . no N2 C24 H24A 109.2 . . no C25 C24 H24A 109.2 . . no N2 C24 H24B 109.2 . . no C25 C24 H24B 109.2 . . no H24A C24 H24B 107.9 . . no C26 C25 C24 111.0(9) . . no C26 C25 H25A 109.4 . . no C24 C25 H25A 109.4 . . no C26 C25 H25B 109.4 . . no C24 C25 H25B 109.4 . . no H25A C25 H25B 108.0 . . no C27 C26 C25 112.6(10) . . no C27 C26 H26A 109.1 . . no C25 C26 H26A 109.1 . . no C27 C26 H26B 109.1 . . no C25 C26 H26B 109.1 . . no H26A C26 H26B 107.8 . . no C26 C27 H27A 109.5 . . no C26 C27 H27B 109.5 . . no H27A C27 H27B 109.5 . . no C26 C27 H27C 109.5 . . no H27A C27 H27C 109.5 . . no H27B C27 H27C 109.5 . . no Se9 Bi2 Se7 83.66(4) . . no Se9 Bi2 Se11 98.42(4) . . no Se7 Bi2 Se11 83.35(3) . . no Se9 Bi2 Se8 96.95(4) . . no Se7 Bi2 Se8 67.03(3) . . no Se11 Bi2 Se8 144.71(3) . . no Se9 Bi2 Se12 164.76(4) . . no Se7 Bi2 Se12 91.89(4) . . no Se11 Bi2 Se12 66.52(3) . . no Se8 Bi2 Se12 94.69(3) . . no Se9 Bi2 Se10 65.40(3) . . no Se7 Bi2 Se10 142.65(3) . . no Se11 Bi2 Se10 81.20(3) . . no Se8 Bi2 Se10 134.07(3) . . no Se12 Bi2 Se10 112.35(3) . . no C28 Se7 Bi2 88.9(3) . . no C28 Se8 Bi2 86.1(3) . . no C29 Se9 Bi2 91.9(3) . . no C29 Se10 Bi2 84.5(3) . . no C30 Se11 Bi2 88.1(4) . . no C30 Se12 Bi2 86.1(3) . . no C29 N4 C39 122.8(8) . . no C29 N4 C43 121.5(8) . . no C39 N4 C43 115.7(8) . . no C28 N6 C35 121.8(9) . . no C28 N6 C31 123.4(8) . . no C35 N6 C31 114.8(8) . . no C30 N5 C47 121.7(10) . . no C30 N5 C51 122.3(10) . . no C47 N5 C51 115.9(10) . . no N6 C28 Se7 122.0(7) . . no N6 C28 Se8 120.2(8) . . no Se7 C28 Se8 117.8(5) . . no N4 C29 Se10 121.9(7) . . no N4 C29 Se9 119.9(7) . . no Se10 C29 Se9 118.2(5) . . no N5 C30 Se11 120.4(9) . . no N5 C30 Se12 120.3(9) . . no Se11 C30 Se12 119.3(6) . . no N6 C31 C32 110.3(8) . . no N6 C31 H31A 109.6 . . no C32 C31 H31A 109.6 . . no N6 C31 H31B 109.6 . . no C32 C31 H31B 109.6 . . no H31A C31 H31B 108.1 . . no C33 C32 C31 111.0(10) . . no C33 C32 H32A 109.4 . . no C31 C32 H32A 109.4 . . no C33 C32 H32B 109.4 . . no C31 C32 H32B 109.4 . . no H32A C32 H32B 108.0 . . no C32 C33 C34 111.1(15) . . no C32 C33 H33A 109.4 . . no C34 C33 H33A 109.4 . . no C32 C33 H33B 109.4 . . no C34 C33 H33B 109.4 . . no H33A C33 H33B 108.0 . . no C33 C34 H34A 109.5 . . no C33 C34 H34B 109.5 . . no H34A C34 H34B 109.5 . . no C33 C34 H34C 109.5 . . no H34A C34 H34C 109.5 . . no H34B C34 H34C 109.5 . . no N6 C35 C36 110.7(10) . . no N6 C35 H35A 109.5 . . no C36 C35 H35A 109.5 . . no N6 C35 H35B 109.5 . . no C36 C35 H35B 109.5 . . no H35A C35 H35B 108.1 . . no C37 C36 C35 116.5(13) . . no C37 C36 H36A 108.2 . . no C35 C36 H36A 108.2 . . no C37 C36 H36B 108.2 . . no C35 C36 H36B 108.2 . . no H36A C36 H36B 107.3 . . no C38 C37 C36 115.9(15) . . no C38 C37 H37A 108.3 . . no C36 C37 H37A 108.3 . . no C38 C37 H37B 108.3 . . no C36 C37 H37B 108.3 . . no H37A C37 H37B 107.4 . . no C37 C38 H38A 109.5 . . no C37 C38 H38C 109.5 . . no H38A C38 H38C 109.5 . . no C37 C38 H38B 109.5 . . no H38A C38 H38B 109.5 . . no H38C C38 H38B 109.5 . . no N4 C39 C40 112.0(9) . . no N4 C39 H39A 109.2 . . no C40 C39 H39A 109.2 . . no N4 C39 H39B 109.2 . . no C40 C39 H39B 109.2 . . no H39A C39 H39B 107.9 . . no C39 C40 C41 112.5(10) . . no C39 C40 H40A 109.1 . . no C41 C40 H40A 109.1 . . no C39 C40 H40B 109.1 . . no C41 C40 H40B 109.1 . . no H40A C40 H40B 107.8 . . no C40 C41 C42' 110.0(11) . . no C40 C41 C42 105.5(13) . . no C42' C41 C42 110.7(18) . . no C40 C41 H41A 109.7 . . no C42' C41 H41A 109.7 . . no C42 C41 H41A 4.3 . . no C40 C41 H41B 109.7 . . no C42' C41 H41B 109.7 . . no C42 C41 H41B 111.2 . . no H41A C41 H41B 108.2 . . no C40 C41 H41C 110.6 . . no C42' C41 H41C 109.3 . . no C42 C41 H41C 110.6 . . no H41A C41 H41C 107.6 . . no H41B C41 H41C 1.0 . . no C40 C41 H41D 110.6 . . no C42' C41 H41D 0.7 . . no C42 C41 H41D 110.6 . . no H41A C41 H41D 109.5 . . no H41B C41 H41D 109.2 . . no H41C C41 H41D 108.8 . . no C41 C42' H42D 109.5 . . no C41 C42' H42E 109.5 . . no H42D C42' H42E 109.5 . . no C41 C42' H42F 109.5 . . no H42D C42' H42F 109.5 . . no H42E C42' H42F 109.5 . . no C41 C42 H42A 109.5 . . no C41 C42 H42B 109.5 . . no H42A C42 H42B 109.5 . . no C41 C42 H42C 109.5 . . no H42A C42 H42C 109.5 . . no H42B C42 H42C 109.5 . . no N4 C43 C44 111.5(8) . . no N4 C43 H43A 109.3 . . no C44 C43 H43A 109.3 . . no N4 C43 H43B 109.3 . . no C44 C43 H43B 109.3 . . no H43A C43 H43B 108.0 . . no C45 C44 C43 110.6(9) . . no C45 C44 H44A 109.5 . . no C43 C44 H44A 109.5 . . no C45 C44 H44B 109.5 . . no C43 C44 H44B 109.5 . . no H44A C44 H44B 108.1 . . no C44 C45 C46 112.4(10) . . no C44 C45 H45A 109.1 . . no C46 C45 H45A 109.1 . . no C44 C45 H45B 109.1 . . no C46 C45 H45B 109.1 . . no H45A C45 H45B 107.9 . . no C45 C46 H46A 109.5 . . no C45 C46 H46B 109.5 . . no H46A C46 H46B 109.5 . . no C45 C46 H46C 109.5 . . no H46A C46 H46C 109.5 . . no H46B C46 H46C 109.5 . . no N5 C47 C48 112.9(10) . . no N5 C47 H47A 109.0 . . no C48 C47 H47A 109.0 . . no N5 C47 H47B 109.0 . . no C48 C47 H47B 109.0 . . no H47A C47 H47B 107.8 . . no C47 C48 C49 105.7(11) . . no C47 C48 H48A 110.6 . . no C49 C48 H48A 110.6 . . no C47 C48 H48B 110.6 . . no C49 C48 H48B 110.6 . . no H48A C48 H48B 108.7 . . no C50 C49 C48 105.9(14) . . no C50 C49 H49A 110.6 . . no C48 C49 H49A 110.6 . . no C50 C49 H49B 110.6 . . no C48 C49 H49B 110.6 . . no H49A C49 H49B 108.7 . . no C49 C50 H50C 109.5 . . no C49 C50 H50A 109.5 . . no H50C C50 H50A 109.5 . . no C49 C50 H50B 109.5 . . no H50C C50 H50B 109.5 . . no H50A C50 H50B 109.5 . . no C52 C51 N5 112.6(11) . . no C52 C51 H51A 109.1 . . no N5 C51 H51A 109.1 . . no C52 C51 H51B 109.1 . . no N5 C51 H51B 109.1 . . no H51A C51 H51B 107.8 . . no C51 C52 C53 108.0(12) . . no C51 C52 H52A 110.1 . . no C53 C52 H52A 110.1 . . no C51 C52 H52B 110.1 . . no C53 C52 H52B 110.1 . . no H52A C52 H52B 108.4 . . no C54 C53 C52 108.5(14) . . no C54 C53 H53A 110.0 . . no C52 C53 H53A 110.0 . . no C54 C53 H53B 110.0 . . no C52 C53 H53B 110.0 . . no H53A C53 H53B 108.4 . . no C53 C54 H54A 109.5 . . no C53 C54 H54B 109.5 . . no H54A C54 H54B 109.5 . . no C53 C54 H54C 109.5 . . no H54A C54 H54C 109.5 . . no H54B C54 H54C 109.5 . . no 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 Se5 Bi1 Se1 C1 147.5(3) . . . . no Se6 Bi1 Se1 C1 79.9(3) . . . . no Se4 Bi1 Se1 C1 -131.5(3) . . . . no Se2 Bi1 Se1 C1 2.7(3) . . . . no Se3 Bi1 Se1 C1 -106.4(3) . . . . no Se1 Bi1 Se2 C1 -2.8(3) . . . . no Se5 Bi1 Se2 C1 -71.0(3) . . . . no Se6 Bi1 Se2 C1 -95.8(3) . . . . no Se4 Bi1 Se2 C1 56.3(3) . . . . no Se3 Bi1 Se2 C1 134.4(3) . . . . no Se1 Bi1 Se3 C2 -28.3(3) . . . . no Se5 Bi1 Se3 C2 77.5(3) . . . . no Se6 Bi1 Se3 C2 143.4(3) . . . . no Se4 Bi1 Se3 C2 -0.9(3) . . . . no Se2 Bi1 Se3 C2 -117.9(3) . . . . no Se1 Bi1 Se4 C2 163.8(3) . . . . no Se5 Bi1 Se4 C2 -99.4(3) . . . . no Se6 Bi1 Se4 C2 -125.7(3) . . . . no Se2 Bi1 Se4 C2 110.4(3) . . . . no Se3 Bi1 Se4 C2 0.9(3) . . . . no Se1 Bi1 Se5 C3 -91.4(3) . . . . no Se6 Bi1 Se5 C3 -6.0(3) . . . . no Se4 Bi1 Se5 C3 -170.7(3) . . . . no Se2 Bi1 Se5 C3 -32.1(3) . . . . no Se3 Bi1 Se5 C3 125.9(3) . . . . no Se1 Bi1 Se6 C3 102.7(3) . . . . no Se5 Bi1 Se6 C3 6.1(3) . . . . no Se4 Bi1 Se6 C3 34.4(3) . . . . no Se2 Bi1 Se6 C3 169.9(3) . . . . no Se3 Bi1 Se6 C3 -72.1(3) . . . . no Bi1 Se2 C1 N1 -174.5(8) . . . . no Bi1 Se2 C1 Se1 4.5(5) . . . . no Bi1 Se1 C1 N1 174.2(7) . . . . no Bi1 Se1 C1 Se2 -4.8(5) . . . . no Bi1 Se4 C2 N3 -179.5(7) . . . . no Bi1 Se4 C2 Se3 -1.5(5) . . . . no Bi1 Se3 C2 N3 179.4(8) . . . . no Bi1 Se3 C2 Se4 1.4(4) . . . . no Bi1 Se6 C3 N2 173.0(8) . . . . no Bi1 Se6 C3 Se5 -9.5(4) . . . . no Bi1 Se5 C3 N2 -172.7(7) . . . . no Bi1 Se5 C3 Se6 9.8(4) . . . . no Se2 C1 N1 C8 -1.4(12) . . . . no Se1 C1 N1 C8 179.6(7) . . . . no Se2 C1 N1 C4 172.7(7) . . . . no Se1 C1 N1 C4 -6.3(12) . . . . no Se6 C3 N2 C24 -1.4(12) . . . . no Se5 C3 N2 C24 -178.8(7) . . . . no Se6 C3 N2 C20 177.9(7) . . . . no Se5 C3 N2 C20 0.5(12) . . . . no Se4 C2 N3 C12 -178.6(6) . . . . no Se3 C2 N3 C12 3.5(12) . . . . no Se4 C2 N3 C16 -2.3(12) . . . . no Se3 C2 N3 C16 179.8(6) . . . . no C1 N1 C4 C5 95.0(11) . . . . no C8 N1 C4 C5 -90.5(10) . . . . no N1 C4 C5 C6 -156.9(10) . . . . no C4 C5 C6 C7 -48.5(16) . . . . no C1 N1 C8 C9 87.5(11) . . . . no C4 N1 C8 C9 -87.0(10) . . . . no N1 C8 C9 C10 -176.2(8) . . . . no C8 C9 C10 C11 -178.0(10) . . . . no C2 N3 C12 C13 -85.7(11) . . . . no C16 N3 C12 C13 97.7(9) . . . . no N3 C12 C13 C14 -179.3(8) . . . . no C12 C13 C14 C15 -180.0(10) . . . . no C2 N3 C16 C17 -86.2(11) . . . . no C12 N3 C16 C17 90.4(9) . . . . no N3 C16 C17 C18 -179.7(8) . . . . no C16 C17 C18 C19 176.3(10) . . . . no C3 N2 C20 C21 96.6(12) . . . . no C24 N2 C20 C21 -84.0(11) . . . . no N2 C20 C21 C22 160.0(11) . . . . no C20 C21 C22 C23 63.9(19) . . . . no C3 N2 C24 C25 91.6(11) . . . . no C20 N2 C24 C25 -87.7(10) . . . . no N2 C24 C25 C26 165.2(9) . . . . no C24 C25 C26 C27 -73.6(14) . . . . no Se9 Bi2 Se7 C28 102.9(3) . . . . no Se11 Bi2 Se7 C28 -157.8(3) . . . . no Se8 Bi2 Se7 C28 2.6(3) . . . . no Se12 Bi2 Se7 C28 -91.7(3) . . . . no Se10 Bi2 Se7 C28 136.2(3) . . . . no Se9 Bi2 Se8 C28 -82.6(3) . . . . no Se7 Bi2 Se8 C28 -2.6(3) . . . . no Se11 Bi2 Se8 C28 32.7(3) . . . . no Se12 Bi2 Se8 C28 87.5(3) . . . . no Se10 Bi2 Se8 C28 -144.9(3) . . . . no Se7 Bi2 Se9 C29 157.5(3) . . . . no Se11 Bi2 Se9 C29 75.2(3) . . . . no Se8 Bi2 Se9 C29 -136.7(3) . . . . no Se12 Bi2 Se9 C29 83.8(3) . . . . no Se10 Bi2 Se9 C29 -1.1(3) . . . . no Se9 Bi2 Se10 C29 1.1(3) . . . . no Se7 Bi2 Se10 C29 -35.8(3) . . . . no Se11 Bi2 Se10 C29 -102.4(3) . . . . no Se8 Bi2 Se10 C29 76.1(3) . . . . no Se12 Bi2 Se10 C29 -162.5(3) . . . . no Se9 Bi2 Se11 C30 177.7(3) . . . . no Se7 Bi2 Se11 C30 95.2(3) . . . . no Se8 Bi2 Se11 C30 62.8(3) . . . . no Se12 Bi2 Se11 C30 0.2(3) . . . . no Se10 Bi2 Se11 C30 -118.9(3) . . . . no Se9 Bi2 Se12 C30 -9.5(4) . . . . no Se7 Bi2 Se12 C30 -82.1(3) . . . . no Se11 Bi2 Se12 C30 -0.2(3) . . . . no Se8 Bi2 Se12 C30 -149.2(3) . . . . no Se10 Bi2 Se12 C30 68.8(3) . . . . no C35 N6 C28 Se7 -0.8(13) . . . . no C31 N6 C28 Se7 -177.8(7) . . . . no C35 N6 C28 Se8 177.8(8) . . . . no C31 N6 C28 Se8 0.8(13) . . . . no Bi2 Se7 C28 N6 174.4(8) . . . . no Bi2 Se7 C28 Se8 -4.2(5) . . . . no Bi2 Se8 C28 N6 -174.6(8) . . . . no Bi2 Se8 C28 Se7 4.1(5) . . . . no C39 N4 C29 Se10 -176.3(7) . . . . no C43 N4 C29 Se10 3.3(13) . . . . no C39 N4 C29 Se9 0.7(13) . . . . no C43 N4 C29 Se9 -179.7(7) . . . . no Bi2 Se10 C29 N4 175.4(8) . . . . no Bi2 Se10 C29 Se9 -1.7(5) . . . . no Bi2 Se9 C29 N4 -175.3(8) . . . . no Bi2 Se9 C29 Se10 1.8(5) . . . . no C47 N5 C30 Se11 -4.0(15) . . . . no C51 N5 C30 Se11 172.6(9) . . . . no C47 N5 C30 Se12 175.9(8) . . . . no C51 N5 C30 Se12 -7.5(15) . . . . no Bi2 Se11 C30 N5 179.6(9) . . . . no Bi2 Se11 C30 Se12 -0.3(5) . . . . no Bi2 Se12 C30 N5 -179.6(9) . . . . no Bi2 Se12 C30 Se11 0.3(5) . . . . no C28 N6 C31 C32 87.3(12) . . . . no C35 N6 C31 C32 -89.9(11) . . . . no N6 C31 C32 C33 -177.0(12) . . . . no C31 C32 C33 C34 173.3(19) . . . . no C28 N6 C35 C36 95.8(13) . . . . no C31 N6 C35 C36 -86.9(13) . . . . no N6 C35 C36 C37 165.6(14) . . . . no C35 C36 C37 C38 62(3) . . . . no C29 N4 C39 C40 -90.2(12) . . . . no C43 N4 C39 C40 90.2(11) . . . . no N4 C39 C40 C41 172.8(9) . . . . no C39 C40 C41 C42' -67.2(16) . . . . no C39 C40 C41 C42 173.3(18) . . . . no C29 N4 C43 C44 -93.3(12) . . . . no C39 N4 C43 C44 86.3(11) . . . . no N4 C43 C44 C45 179.5(10) . . . . no C43 C44 C45 C46 177.9(12) . . . . no C30 N5 C47 C48 95.1(14) . . . . no C51 N5 C47 C48 -81.7(14) . . . . no N5 C47 C48 C49 -179.3(12) . . . . no C47 C48 C49 C50 152.0(19) . . . . no C30 N5 C51 C52 97.5(16) . . . . no C47 N5 C51 C52 -85.7(16) . . . . no N5 C51 C52 C53 179.6(15) . . . . no C51 C52 C53 C54 -174(2) . . . . no _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 2.287 _refine_diff_density_min -2.767 _refine_diff_density_rms 0.218 #=== END