Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'Dominic S. Wright' 'Jamie F. Bickley' 'Andrew D. Bond' 'Felipe Garcia' 'Katja Jantos' 'Gavin T. Lawson' 'M. McPartlin' 'Alexander Steiner' _publ_contact_author_name 'Dr Dominic S. Wright' _publ_contact_author_address ; Chemistry Department University of Cambridge Lensfield Road Cambridge CB2 1EW UNITED KINGDOM ; _publ_contact_author_email 'DSW1000@CUS.CAM.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Syntheses and Structures of the Cubanes [PhOSb(mu-NCy)]4 and [pyOBi(mu-NCy)]4 (Cy= cyclohexyl, py = 2-pyridyl) ; data_dw0203 _database_code_CSD 192356 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H68 Bi4 N8 O4' _chemical_formula_weight 1693.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Bi' 'Bi' -4.1077 10.2566 '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 14.4053(4) _cell_length_b 14.7360(5) _cell_length_c 14.8018(5) _cell_angle_alpha 94.740(2) _cell_angle_beta 116.155(2) _cell_angle_gamma 103.563(2) _cell_volume 2678.67(15) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1588 _exptl_absorpt_coefficient_mu 13.149 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.726 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'KappaCCD' _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_detector_area_resol_mean 9 _diffrn_radiation_monochromator 'horizonally mounted graphite crystal' _diffrn_measurement_method 'CCD' _diffrn_reflns_number 26974 _diffrn_reflns_av_R_equivalents 0.0607 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9425 _reflns_number_observed 7521 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution teXsan _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _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^)+(0.0356P)^2^+0.9846P] 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 9401 _refine_ls_number_parameters 604 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.002 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 0.16097(2) 0.22330(2) 0.04091(2) 0.02351(8) Uani 1 1 d . . . Bi2 Bi 0.37163(2) 0.41389(2) 0.25593(2) 0.02296(8) Uani 1 1 d . . . Bi3 Bi 0.36951(2) 0.39518(2) 0.02142(2) 0.02478(8) Uani 1 1 d . . . Bi4 Bi 0.15220(2) 0.45496(2) 0.04513(2) 0.02337(8) Uani 1 1 d . . . O1 O 0.2171(4) 0.1628(4) 0.1945(4) 0.0355(13) Uani 1 1 d . . . N1 N 0.0359(5) 0.0938(5) 0.1163(5) 0.0374(17) Uani 1 1 d . . . C11 C 0.1355(7) 0.1103(6) 0.1974(6) 0.035(2) Uani 1 1 d . . . C12 C 0.1443(8) 0.0670(7) 0.2820(7) 0.051(2) Uani 1 1 d . . . H12 H 0.2137 0.0754 0.3386 0.061 Uiso 1 1 calc R . . C13 C 0.0514(11) 0.0124(7) 0.2821(9) 0.067(3) Uani 1 1 d . . . H13 H 0.0572 -0.0157 0.3392 0.080 Uiso 1 1 calc R . . C14 C -0.0485(9) -0.0008(7) 0.1995(9) 0.061(3) Uani 1 1 d . . . H14 H -0.1128 -0.0384 0.1978 0.073 Uiso 1 1 calc R . . C15 C -0.0528(8) 0.0424(7) 0.1184(9) 0.054(3) Uani 1 1 d . . . H15 H -0.1218 0.0351 0.0618 0.065 Uiso 1 1 calc R . . O2 O 0.2939(4) 0.5353(4) 0.2889(4) 0.0287(12) Uani 1 1 d . . . N2 N 0.4747(5) 0.5821(5) 0.3950(5) 0.0300(15) Uani 1 1 d . . . C21 C 0.3767(6) 0.5989(6) 0.3634(6) 0.0280(18) Uani 1 1 d . . . C22 C 0.3718(7) 0.6832(6) 0.4128(6) 0.0335(19) Uani 1 1 d . . . H22 H 0.3045 0.6963 0.3908 0.040 Uiso 1 1 calc R . . C23 C 0.4634(7) 0.7445(6) 0.4914(6) 0.041(2) Uani 1 1 d . . . H23 H 0.4599 0.8001 0.5254 0.049 Uiso 1 1 calc R . . C24 C 0.5627(7) 0.7274(6) 0.5229(6) 0.044(2) Uani 1 1 d . . . H24 H 0.6277 0.7708 0.5772 0.052 Uiso 1 1 calc R . . C25 C 0.5633(7) 0.6445(6) 0.4721(7) 0.038(2) Uani 1 1 d . . . H25 H 0.6306 0.6316 0.4934 0.046 Uiso 1 1 calc R . . O3 O 0.5617(4) 0.4295(4) 0.1408(4) 0.0338(13) Uani 1 1 d . . . N3 N 0.5744(5) 0.4421(5) 0.3016(5) 0.0323(16) Uani 1 1 d . . . C31 C 0.6161(6) 0.4279(6) 0.2368(7) 0.0322(19) Uani 1 1 d . . . C32 C 0.7187(6) 0.4126(6) 0.2768(7) 0.043(2) Uani 1 1 d . . . H32 H 0.7473 0.4000 0.2320 0.052 Uiso 1 1 calc R . . C33 C 0.7773(6) 0.4159(7) 0.3798(7) 0.043(2) Uani 1 1 d . . . H33 H 0.8468 0.4067 0.4069 0.051 Uiso 1 1 calc R . . C34 C 0.7336(7) 0.4329(7) 0.4442(7) 0.046(2) Uani 1 1 d . . . H34 H 0.7734 0.4367 0.5162 0.055 Uiso 1 1 calc R . . C35 C 0.6325(6) 0.4440(6) 0.4024(6) 0.0309(18) Uani 1 1 d . . . H35 H 0.6020 0.4535 0.4463 0.037 Uiso 1 1 calc R . . O4 O -0.0299(4) 0.3853(4) -0.0660(4) 0.0325(13) Uani 1 1 d . . . N4 N -0.0488(5) 0.2260(4) -0.0668(5) 0.0275(14) Uani 1 1 d . . . C41 C -0.0900(6) 0.2970(6) -0.1005(6) 0.0267(17) Uani 1 1 d . . . C42 C -0.2009(6) 0.2752(6) -0.1749(6) 0.0337(19) Uani 1 1 d . . . H42 H -0.2306 0.3250 -0.1985 0.040 Uiso 1 1 calc R . . C43 C -0.2643(7) 0.1820(7) -0.2123(7) 0.041(2) Uani 1 1 d . . . H43 H -0.3384 0.1667 -0.2625 0.050 Uiso 1 1 calc R . . C44 C -0.2205(6) 0.1097(6) -0.1770(6) 0.036(2) Uani 1 1 d . . . H44 H -0.2638 0.0446 -0.2015 0.044 Uiso 1 1 calc R . . C45 C -0.1135(6) 0.1350(6) -0.1059(6) 0.0339(19) Uani 1 1 d . . . H45 H -0.0829 0.0856 -0.0827 0.041 Uiso 1 1 calc R . . N5 N 0.3524(4) 0.4910(4) 0.1295(4) 0.0250(14) Uani 1 1 d . . . C51 C 0.4022(6) 0.5961(5) 0.1479(6) 0.0254(17) Uani 1 1 d . . . H51 H 0.3774 0.6280 0.1916 0.030 Uiso 1 1 calc R . . C52 C 0.3617(6) 0.6309(5) 0.0459(6) 0.0295(18) Uani 1 1 d . . . H52A H 0.3847 0.5999 0.0008 0.035 Uiso 1 1 calc R . . H52B H 0.2814 0.6112 0.0104 0.035 Uiso 1 1 calc R . . C53 C 0.4052(7) 0.7391(6) 0.0624(7) 0.039(2) Uani 1 1 d . . . H53A H 0.3830 0.7572 -0.0053 0.047 Uiso 1 1 calc R . . H53B H 0.3729 0.7701 0.0981 0.047 Uiso 1 1 calc R . . C54 C 0.5263(7) 0.7749(6) 0.1248(7) 0.042(2) Uani 1 1 d . . . H54A H 0.5502 0.8456 0.1406 0.050 Uiso 1 1 calc R . . H54B H 0.5588 0.7532 0.0837 0.050 Uiso 1 1 calc R . . C55 C 0.5677(6) 0.7398(6) 0.2255(6) 0.038(2) Uani 1 1 d . . . H55A H 0.6480 0.7605 0.2616 0.045 Uiso 1 1 calc R . . H55B H 0.5430 0.7677 0.2709 0.045 Uiso 1 1 calc R . . C56 C 0.5247(6) 0.6307(5) 0.2028(6) 0.0308(18) Uani 1 1 d . . . H56A H 0.5523 0.6084 0.2683 0.037 Uiso 1 1 calc R . . H56B H 0.5518 0.6030 0.1596 0.037 Uiso 1 1 calc R . . N6 N 0.1826(5) 0.3522(4) -0.0471(4) 0.0261(14) Uani 1 1 d . . . C61 C 0.1161(6) 0.3256(5) -0.1609(6) 0.0264(17) Uani 1 1 d . . . H61 H 0.0413 0.2869 -0.1777 0.032 Uiso 1 1 calc R . . C62 C 0.1069(8) 0.4118(6) -0.2104(6) 0.040(2) Uani 1 1 d . . . H62A H 0.0736 0.4502 -0.1826 0.048 Uiso 1 1 calc R . . H62B H 0.1803 0.4525 -0.1930 0.048 Uiso 1 1 calc R . . C63 C 0.0386(8) 0.3808(7) -0.3261(6) 0.050(2) Uani 1 1 d . . . H63A H 0.0361 0.4381 -0.3565 0.060 Uiso 1 1 calc R . . H63B H -0.0365 0.3451 -0.3432 0.060 Uiso 1 1 calc R . . C64 C 0.0831(8) 0.3182(7) -0.3727(7) 0.050(2) Uani 1 1 d . . . H64A H 0.0339 0.2961 -0.4477 0.060 Uiso 1 1 calc R . . H64B H 0.1550 0.3559 -0.3624 0.060 Uiso 1 1 calc R . . C65 C 0.0940(7) 0.2333(7) -0.3236(6) 0.045(2) Uani 1 1 d . . . H65A H 0.1276 0.1957 -0.3518 0.055 Uiso 1 1 calc R . . H65B H 0.0210 0.1918 -0.3409 0.055 Uiso 1 1 calc R . . C66 C 0.1620(7) 0.2634(6) -0.2088(6) 0.041(2) Uani 1 1 d . . . H66A H 0.2369 0.2999 -0.1917 0.049 Uiso 1 1 calc R . . H66B H 0.1653 0.2059 -0.1788 0.049 Uiso 1 1 calc R . . N7 N 0.1742(4) 0.3490(4) 0.1437(4) 0.0203(13) Uani 1 1 d . . . C71 C 0.1025(6) 0.3274(5) 0.1950(5) 0.0233(17) Uani 1 1 d . . . H71 H 0.0527 0.2607 0.1616 0.028 Uiso 1 1 calc R . . C72 C 0.1688(6) 0.3300(6) 0.3099(6) 0.0310(19) Uani 1 1 d . . . H72A H 0.2147 0.3962 0.3468 0.037 Uiso 1 1 calc R . . H72B H 0.2170 0.2895 0.3193 0.037 Uiso 1 1 calc R . . C73 C 0.0917(7) 0.2931(7) 0.3550(7) 0.044(2) Uani 1 1 d . . . H73A H 0.1350 0.2964 0.4296 0.053 Uiso 1 1 calc R . . H73B H 0.0492 0.2255 0.3210 0.053 Uiso 1 1 calc R . . C75 C -0.0456(6) 0.3575(6) 0.2267(7) 0.038(2) Uani 1 1 d . . . H75A H -0.0906 0.4007 0.2197 0.046 Uiso 1 1 calc R . . H75B H -0.0950 0.2930 0.1863 0.046 Uiso 1 1 calc R . . C74 C 0.0146(7) 0.3531(6) 0.3387(7) 0.041(2) Uani 1 1 d . . . H74A H -0.0383 0.3250 0.3621 0.049 Uiso 1 1 calc R . . H74B H 0.0565 0.4186 0.3807 0.049 Uiso 1 1 calc R . . C76 C 0.0310(6) 0.3932(6) 0.1815(6) 0.0285(18) Uani 1 1 d . . . H76A H 0.0771 0.4596 0.2176 0.034 Uiso 1 1 calc R . . H76B H -0.0120 0.3924 0.1075 0.034 Uiso 1 1 calc R . . N8 N 0.3465(5) 0.2923(4) 0.1143(5) 0.0244(14) Uani 1 1 d . . . C81 C 0.4151(6) 0.2261(5) 0.1291(6) 0.0252(17) Uani 1 1 d . . . H81 H 0.4800 0.2601 0.1227 0.030 Uiso 1 1 calc R . . C82 C 0.4569(6) 0.2000(6) 0.2348(6) 0.034(2) Uani 1 1 d . . . H82A H 0.3949 0.1635 0.2429 0.040 Uiso 1 1 calc R . . H82B H 0.4960 0.2591 0.2894 0.040 Uiso 1 1 calc R . . C83 C 0.5330(7) 0.1402(6) 0.2461(7) 0.041(2) Uani 1 1 d . . . H83A H 0.5980 0.1792 0.2442 0.049 Uiso 1 1 calc R . . H83B H 0.5574 0.1221 0.3139 0.049 Uiso 1 1 calc R . . C84 C 0.4792(7) 0.0509(6) 0.1620(7) 0.048(2) Uani 1 1 d . . . H84A H 0.4206 0.0076 0.1700 0.057 Uiso 1 1 calc R . . H84B H 0.5332 0.0172 0.1690 0.057 Uiso 1 1 calc R . . C85 C 0.4315(7) 0.0736(6) 0.0549(7) 0.044(2) Uani 1 1 d . . . H85A H 0.4908 0.1084 0.0422 0.053 Uiso 1 1 calc R . . H85B H 0.3898 0.0135 0.0020 0.053 Uiso 1 1 calc R . . C86 C 0.3573(6) 0.1346(5) 0.0477(6) 0.0315(19) Uani 1 1 d . . . H86A H 0.2953 0.0971 0.0550 0.038 Uiso 1 1 calc R . . H86B H 0.3281 0.1504 -0.0213 0.038 Uiso 1 1 calc R . . C1T C 0.7681(10) 1.0753(13) 0.3996(12) 0.093(4) Uani 1 1 d . . . C2T C 0.7072(15) 0.9879(11) 0.3841(12) 0.110(6) Uani 1 1 d . . . H2T H 0.6972 0.9398 0.3310 0.132 Uiso 1 1 calc R . . C3T C 0.6583(18) 0.9653(14) 0.4430(16) 0.150(8) Uani 1 1 d . . . H3T H 0.6146 0.9016 0.4303 0.180 Uiso 1 1 calc R . . C4T C 0.6712(17) 1.0341(17) 0.5221(14) 0.122(6) Uani 1 1 d . . . H4T H 0.6329 1.0206 0.5601 0.146 Uiso 1 1 calc R . . C5T C 0.7442(13) 1.1243(13) 0.5417(13) 0.105(6) Uani 1 1 d . . . H5T H 0.7621 1.1717 0.5992 0.126 Uiso 1 1 calc R . . C6T C 0.7895(11) 1.1450(10) 0.4796(13) 0.095(5) Uani 1 1 d . . . H6T H 0.8358 1.2073 0.4915 0.114 Uiso 1 1 calc R . . C7T C 0.8200(15) 1.0995(15) 0.334(2) 0.214(13) Uani 1 1 d . . . H7T1 H 0.7967 1.0436 0.2802 0.322 Uiso 1 1 calc R . . H7T2 H 0.8991 1.1187 0.3769 0.322 Uiso 1 1 calc R . . H7T3 H 0.7987 1.1523 0.3031 0.322 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 0.02510(15) 0.02489(17) 0.02366(17) 0.00630(13) 0.01258(13) 0.01057(13) Bi2 0.02291(15) 0.02937(17) 0.02183(16) 0.00854(13) 0.01302(12) 0.01107(13) Bi3 0.02920(16) 0.02896(17) 0.02501(17) 0.00840(13) 0.01821(13) 0.01231(13) Bi4 0.02505(15) 0.02531(17) 0.02511(17) 0.00865(13) 0.01380(13) 0.01195(13) O1 0.034(3) 0.045(4) 0.035(3) 0.018(3) 0.018(3) 0.018(3) N1 0.043(4) 0.030(4) 0.042(5) 0.008(3) 0.019(4) 0.017(3) C11 0.048(5) 0.024(5) 0.030(5) 0.007(4) 0.014(4) 0.015(4) C12 0.066(6) 0.049(6) 0.049(6) 0.025(5) 0.034(5) 0.022(5) C13 0.109(10) 0.043(7) 0.075(8) 0.021(6) 0.065(8) 0.021(7) C14 0.071(7) 0.036(6) 0.082(9) 0.001(6) 0.054(7) -0.007(5) C15 0.051(6) 0.039(6) 0.080(8) 0.006(6) 0.041(6) 0.009(5) O2 0.025(3) 0.033(3) 0.031(3) 0.007(3) 0.016(3) 0.008(3) N2 0.030(4) 0.036(4) 0.028(4) 0.008(3) 0.015(3) 0.014(3) C21 0.042(5) 0.029(5) 0.027(5) 0.010(4) 0.024(4) 0.017(4) C22 0.042(5) 0.028(5) 0.033(5) 0.008(4) 0.021(4) 0.010(4) C23 0.056(6) 0.037(5) 0.029(5) 0.009(4) 0.015(4) 0.022(5) C24 0.055(6) 0.037(5) 0.030(5) 0.015(4) 0.011(4) 0.013(5) C25 0.040(5) 0.042(6) 0.040(5) 0.015(4) 0.021(4) 0.017(4) O3 0.030(3) 0.042(4) 0.038(4) 0.009(3) 0.023(3) 0.013(3) N3 0.029(3) 0.042(4) 0.029(4) 0.008(3) 0.012(3) 0.019(3) C31 0.028(4) 0.035(5) 0.043(6) 0.015(4) 0.024(4) 0.009(4) C32 0.039(5) 0.051(6) 0.068(7) 0.032(5) 0.042(5) 0.023(5) C33 0.020(4) 0.060(6) 0.061(6) 0.034(5) 0.022(4) 0.018(4) C34 0.039(5) 0.057(6) 0.046(6) 0.023(5) 0.018(5) 0.020(5) C35 0.032(4) 0.036(5) 0.019(4) 0.004(4) 0.009(4) 0.008(4) O4 0.031(3) 0.035(4) 0.037(3) 0.014(3) 0.017(3) 0.017(3) N4 0.030(3) 0.029(4) 0.020(3) 0.002(3) 0.010(3) 0.005(3) C41 0.029(4) 0.032(5) 0.021(4) 0.006(4) 0.011(3) 0.014(4) C42 0.034(4) 0.038(5) 0.030(5) 0.008(4) 0.013(4) 0.017(4) C43 0.027(4) 0.055(6) 0.036(5) 0.001(5) 0.010(4) 0.015(5) C44 0.029(4) 0.031(5) 0.040(5) -0.001(4) 0.015(4) 0.000(4) C45 0.029(4) 0.032(5) 0.042(5) 0.015(4) 0.015(4) 0.010(4) N5 0.022(3) 0.026(4) 0.025(4) 0.008(3) 0.009(3) 0.008(3) C51 0.029(4) 0.025(4) 0.024(4) 0.002(3) 0.017(3) 0.003(3) C52 0.026(4) 0.031(5) 0.040(5) 0.016(4) 0.022(4) 0.009(4) C53 0.051(5) 0.028(5) 0.056(6) 0.020(4) 0.036(5) 0.018(4) C54 0.062(6) 0.026(5) 0.059(6) 0.014(4) 0.047(5) 0.011(4) C55 0.040(5) 0.034(5) 0.042(5) 0.002(4) 0.026(4) 0.004(4) C56 0.032(4) 0.032(5) 0.038(5) 0.010(4) 0.024(4) 0.010(4) N6 0.032(3) 0.033(4) 0.022(4) 0.012(3) 0.016(3) 0.018(3) C61 0.029(4) 0.019(4) 0.029(5) 0.005(3) 0.013(4) 0.003(3) C62 0.075(6) 0.036(5) 0.024(5) 0.016(4) 0.028(5) 0.029(5) C63 0.074(6) 0.042(6) 0.027(5) 0.014(4) 0.015(5) 0.020(5) C64 0.060(6) 0.058(7) 0.031(5) 0.004(5) 0.027(5) 0.009(5) C65 0.055(6) 0.050(6) 0.035(5) 0.003(5) 0.025(5) 0.017(5) C66 0.051(5) 0.046(6) 0.031(5) 0.010(4) 0.024(4) 0.018(5) N7 0.023(3) 0.021(3) 0.022(3) 0.008(3) 0.013(3) 0.010(3) C71 0.028(4) 0.031(4) 0.024(4) 0.011(3) 0.020(3) 0.014(4) C72 0.035(4) 0.038(5) 0.034(5) 0.011(4) 0.023(4) 0.018(4) C73 0.046(5) 0.063(6) 0.047(6) 0.026(5) 0.036(5) 0.025(5) C75 0.036(5) 0.039(5) 0.054(6) 0.014(4) 0.031(4) 0.019(4) C74 0.050(5) 0.045(6) 0.055(6) 0.017(5) 0.044(5) 0.019(5) C76 0.028(4) 0.031(5) 0.032(5) 0.009(4) 0.018(4) 0.012(4) N8 0.028(3) 0.022(3) 0.028(4) 0.011(3) 0.014(3) 0.012(3) C81 0.029(4) 0.028(4) 0.034(5) 0.012(4) 0.023(4) 0.016(4) C82 0.034(4) 0.038(5) 0.039(5) 0.016(4) 0.019(4) 0.023(4) C83 0.040(5) 0.045(6) 0.048(6) 0.023(5) 0.020(4) 0.028(5) C84 0.054(6) 0.044(6) 0.071(7) 0.032(5) 0.039(5) 0.034(5) C85 0.055(5) 0.038(5) 0.056(6) 0.008(5) 0.036(5) 0.025(5) C86 0.031(4) 0.031(5) 0.035(5) 0.006(4) 0.016(4) 0.014(4) C1T 0.057(8) 0.106(13) 0.100(11) 0.002(10) 0.024(8) 0.033(8) C2T 0.169(16) 0.045(9) 0.066(10) -0.010(8) 0.017(10) 0.034(10) C3T 0.21(2) 0.087(14) 0.084(14) 0.035(12) 0.022(14) 0.026(14) C4T 0.162(17) 0.143(18) 0.083(13) 0.061(13) 0.048(12) 0.093(16) C5T 0.097(12) 0.099(13) 0.094(12) -0.009(10) 0.012(9) 0.064(11) C6T 0.068(9) 0.060(9) 0.108(13) -0.020(9) 0.011(8) 0.013(7) C7T 0.117(15) 0.17(2) 0.37(4) -0.02(2) 0.16(2) 0.006(14) _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 N7 2.212(5) . ? Bi1 N8 2.311(6) . ? Bi1 O1 2.381(5) . ? Bi1 N6 2.427(6) . ? Bi1 N4 2.737(6) . ? Bi2 N5 2.217(6) . ? Bi2 O2 2.443(5) . ? Bi2 N7 2.462(5) . ? Bi2 N8 2.479(6) . ? Bi2 N3 2.609(6) . ? Bi2 N2 2.705(7) . ? Bi3 N5 2.180(6) . ? Bi3 N8 2.193(6) . ? Bi3 N6 2.317(6) . ? Bi3 O3 2.434(5) . ? Bi4 N6 2.201(6) . ? Bi4 N7 2.206(5) . ? Bi4 O4 2.301(5) . ? Bi4 N5 2.481(5) . ? O1 C11 1.266(10) . ? N1 C11 1.352(10) . ? N1 C15 1.338(11) . ? C11 C12 1.423(12) . ? C12 C13 1.391(14) . ? C13 C14 1.372(15) . ? C14 C15 1.389(14) . ? O2 C21 1.290(9) . ? N2 C25 1.330(10) . ? N2 C21 1.370(9) . ? C21 C22 1.421(10) . ? C22 C23 1.351(11) . ? C23 C24 1.388(11) . ? C24 C25 1.384(12) . ? O3 C31 1.291(9) . ? N3 C35 1.345(9) . ? N3 C31 1.362(9) . ? C31 C32 1.412(10) . ? C32 C33 1.368(12) . ? C33 C34 1.389(12) . ? C34 C35 1.366(10) . ? O4 C41 1.294(9) . ? N4 C41 1.346(9) . ? N4 C45 1.346(10) . ? C41 C42 1.421(10) . ? C42 C43 1.367(12) . ? C43 C44 1.386(11) . ? C44 C45 1.363(10) . ? N5 C51 1.491(9) . ? C51 C52 1.541(10) . ? C51 C56 1.509(10) . ? C52 C53 1.527(11) . ? C53 C54 1.498(12) . ? C54 C55 1.528(11) . ? C55 C56 1.530(11) . ? N6 C61 1.483(9) . ? C61 C62 1.521(10) . ? C61 C66 1.540(10) . ? C62 C63 1.511(11) . ? C63 C64 1.517(12) . ? C64 C65 1.504(12) . ? C65 C66 1.499(11) . ? N7 C71 1.524(8) . ? C71 C72 1.531(10) . ? C71 C76 1.536(9) . ? C72 C73 1.552(10) . ? C73 C74 1.528(10) . ? C75 C74 1.511(11) . ? C75 C76 1.541(10) . ? N8 C81 1.508(8) . ? C81 C82 1.528(10) . ? C81 C86 1.511(10) . ? C82 C83 1.524(9) . ? C83 C84 1.512(12) . ? C84 C85 1.527(12) . ? C85 C86 1.525(9) . ? C1T C6T 1.370(18) . ? C1T C2T 1.31(2) . ? C1T C7T 1.48(2) . ? C2T C3T 1.36(3) . ? C3T C4T 1.40(2) . ? C4T C5T 1.40(2) . ? C5T C6T 1.36(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N7 Bi1 N8 82.6(2) . . ? N7 Bi1 O1 82.58(19) . . ? N8 Bi1 O1 80.43(19) . . ? N7 Bi1 N6 76.7(2) . . ? N8 Bi1 N6 75.47(19) . . ? O1 Bi1 N6 149.9(2) . . ? N7 Bi1 N4 82.57(18) . . ? N8 Bi1 N4 152.60(19) . . ? O1 Bi1 N4 120.13(18) . . ? N6 Bi1 N4 78.77(18) . . ? N5 Bi2 O2 77.08(18) . . ? N5 Bi2 N7 79.8(2) . . ? O2 Bi2 N7 73.77(17) . . ? N5 Bi2 N8 76.0(2) . . ? O2 Bi2 N8 141.16(17) . . ? N7 Bi2 N8 74.35(18) . . ? N5 Bi2 N3 88.6(2) . . ? O2 Bi2 N3 125.77(19) . . ? N7 Bi2 N3 154.54(19) . . ? N8 Bi2 N3 80.90(19) . . ? N5 Bi2 N2 90.1(2) . . ? O2 Bi2 N2 51.73(17) . . ? N7 Bi2 N2 125.40(17) . . ? N8 Bi2 N2 153.94(19) . . ? N3 Bi2 N2 76.76(18) . . ? N5 Bi3 N8 83.0(2) . . ? N5 Bi3 N6 78.7(2) . . ? N8 Bi3 N6 80.0(2) . . ? N5 Bi3 O3 90.67(19) . . ? N8 Bi3 O3 84.49(19) . . ? N6 Bi3 O3 162.11(19) . . ? N6 Bi4 N7 81.7(2) . . ? N6 Bi4 O4 87.3(2) . . ? N7 Bi4 O4 97.73(19) . . ? N6 Bi4 N5 74.8(2) . . ? N7 Bi4 N5 79.6(2) . . ? O4 Bi4 N5 162.03(18) . . ? C11 O1 Bi1 110.3(5) . . ? C11 N1 C15 120.6(8) . . ? O1 C11 N1 118.9(7) . . ? O1 C11 C12 122.7(8) . . ? N1 C11 C12 118.4(8) . . ? C11 C12 C13 120.1(9) . . ? C14 C13 C12 119.7(10) . . ? C13 C14 C15 118.0(9) . . ? N1 C15 C14 123.0(10) . . ? C21 O2 Bi2 103.1(4) . . ? C25 N2 C21 119.2(6) . . ? C25 N2 Bi2 151.7(5) . . ? C21 N2 Bi2 88.9(4) . . ? O2 C21 N2 116.2(6) . . ? O2 C21 C22 124.4(7) . . ? N2 C21 C22 119.4(7) . . ? C23 C22 C21 119.6(7) . . ? C24 C23 C22 120.8(8) . . ? C23 C24 C25 117.3(8) . . ? N2 C25 C24 123.6(7) . . ? C31 O3 Bi3 134.2(4) . . ? C35 N3 C31 119.8(6) . . ? C35 N3 Bi2 109.0(5) . . ? C31 N3 Bi2 128.3(5) . . ? O3 C31 N3 119.5(6) . . ? O3 C31 C32 121.5(7) . . ? N3 C31 C32 119.0(7) . . ? C33 C32 C31 120.4(8) . . ? C32 C33 C34 119.2(7) . . ? C35 C34 C33 118.9(8) . . ? N3 C35 C34 122.7(7) . . ? C41 O4 Bi4 132.1(4) . . ? C41 N4 C45 119.0(6) . . ? C41 N4 Bi1 131.4(5) . . ? C45 N4 Bi1 108.1(4) . . ? O4 C41 N4 120.9(6) . . ? O4 C41 C42 119.2(6) . . ? N4 C41 C42 119.8(7) . . ? C43 C42 C41 119.4(7) . . ? C42 C43 C44 120.0(7) . . ? C45 C44 C43 117.9(8) . . ? N4 C45 C44 123.8(7) . . ? C51 N5 Bi3 119.2(4) . . ? C51 N5 Bi2 122.9(4) . . ? Bi3 N5 Bi2 103.2(2) . . ? C51 N5 Bi4 108.6(4) . . ? Bi3 N5 Bi4 100.7(2) . . ? Bi2 N5 Bi4 98.1(2) . . ? N5 C51 C52 110.8(6) . . ? N5 C51 C56 115.4(5) . . ? C52 C51 C56 108.1(6) . . ? C53 C52 C51 112.4(7) . . ? C54 C53 C52 111.9(6) . . ? C53 C54 C55 112.3(7) . . ? C56 C55 C54 109.8(7) . . ? C55 C56 C51 111.4(6) . . ? C61 N6 Bi4 120.7(4) . . ? C61 N6 Bi3 117.7(4) . . ? Bi4 N6 Bi3 105.3(3) . . ? C61 N6 Bi1 114.8(4) . . ? Bi4 N6 Bi1 96.0(2) . . ? Bi3 N6 Bi1 98.07(19) . . ? N6 C61 C62 113.0(6) . . ? N6 C61 C66 111.0(5) . . ? C62 C61 C66 109.1(6) . . ? C63 C62 C61 110.8(7) . . ? C62 C63 C64 111.9(7) . . ? C65 C64 C63 110.6(7) . . ? C64 C65 C66 111.3(8) . . ? C65 C66 C61 111.8(6) . . ? C71 N7 Bi4 118.8(4) . . ? C71 N7 Bi1 114.2(4) . . ? Bi4 N7 Bi1 102.3(2) . . ? C71 N7 Bi2 117.8(4) . . ? Bi4 N7 Bi2 98.9(2) . . ? Bi1 N7 Bi2 102.09(19) . . ? N7 C71 C72 111.9(5) . . ? N7 C71 C76 113.9(6) . . ? C72 C71 C76 109.2(6) . . ? C71 C72 C73 110.0(6) . . ? C72 C73 C74 110.5(7) . . ? C74 C75 C76 112.8(6) . . ? C75 C74 C73 111.2(6) . . ? C75 C76 C71 108.8(6) . . ? C81 N8 Bi3 113.1(4) . . ? C81 N8 Bi1 117.4(4) . . ? Bi3 N8 Bi1 105.4(2) . . ? C81 N8 Bi2 123.7(4) . . ? Bi3 N8 Bi2 94.8(2) . . ? Bi1 N8 Bi2 98.8(2) . . ? C82 C81 N8 113.9(5) . . ? C82 C81 C86 108.3(6) . . ? N8 C81 C86 112.9(6) . . ? C81 C82 C83 110.2(6) . . ? C84 C83 C82 112.1(7) . . ? C83 C84 C85 111.8(7) . . ? C86 C85 C84 109.4(6) . . ? C85 C86 C81 112.6(6) . . ? C6T C1T C2T 121.0(16) . . ? C6T C1T C7T 118.3(18) . . ? C2T C1T C7T 120.6(17) . . ? C3T C2T C1T 120.9(16) . . ? C2T C3T C4T 121.2(19) . . ? C5T C4T C3T 115.8(19) . . ? C6T C5T C4T 121.0(15) . . ? C5T C6T C1T 119.6(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.314 _refine_diff_density_min -1.792 _refine_diff_density_rms 0.189 data_domfg1 _database_code_CSD 192357 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51.50 H68 N4 O4 Sb4' _chemical_formula_weight 1294.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 '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 15.208(2) _cell_length_b 18.556(3) _cell_length_c 19.837(3) _cell_angle_alpha 86.902(18) _cell_angle_beta 75.876(17) _cell_angle_gamma 73.847(17) _cell_volume 5213.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 2.096 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.984 _exptl_absorpt_process_details semi-empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'SMART APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33535 _diffrn_reflns_av_R_equivalents 0.0567 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.04 _reflns_number_total 15421 _reflns_number_gt 13920 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0604P)^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 15421 _refine_ls_number_parameters 1144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.090 _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 Sb1 Sb 0.364255(18) 0.429898(14) 0.655949(13) 0.02155(8) Uani 1 1 d . . . Sb2 Sb 0.161689(18) 0.387501(14) 0.723765(14) 0.02318(8) Uani 1 1 d . . . Sb3 Sb 0.240822(18) 0.417512(15) 0.541596(13) 0.02321(8) Uani 1 1 d . . . Sb4 Sb 0.138160(18) 0.558441(14) 0.657161(13) 0.02144(8) Uani 1 1 d . . . Sb5 Sb 0.728673(19) 1.099620(15) 0.853159(14) 0.02401(8) Uani 1 1 d . . . Sb6 Sb 0.755758(19) 0.928556(15) 0.919569(14) 0.02493(8) Uani 1 1 d . . . Sb7 Sb 0.802462(19) 0.961769(15) 0.733432(13) 0.02327(8) Uani 1 1 d . . . Sb8 Sb 0.956830(19) 0.957994(15) 0.826701(14) 0.02414(8) Uani 1 1 d . . . O1 O 0.4097(2) 0.34439(16) 0.72062(15) 0.0298(7) Uani 1 1 d . . . O2 O 0.0544(2) 0.44690(16) 0.80198(15) 0.0336(7) Uani 1 1 d . . . O3 O 0.3725(2) 0.40394(18) 0.47632(15) 0.0338(7) Uani 1 1 d . . . O4 O 0.0685(2) 0.59565(15) 0.57974(15) 0.0305(7) Uani 1 1 d . . . O5 O 0.6088(2) 1.10984(16) 0.93050(15) 0.0349(8) Uani 1 1 d . . . O6 O 0.8495(2) 0.88435(17) 0.97976(15) 0.0332(7) Uani 1 1 d . . . O7 O 0.7542(2) 1.05369(16) 0.67530(15) 0.0305(7) Uani 1 1 d . . . O8 O 1.0411(2) 0.89211(18) 0.74201(15) 0.0357(7) Uani 1 1 d . . . N1 N 0.2344(2) 0.46682(18) 0.72670(17) 0.0229(7) Uani 1 1 d . . . N2 N 0.2992(2) 0.36006(18) 0.61978(17) 0.0239(8) Uani 1 1 d . . . N3 N 0.1080(2) 0.45691(18) 0.64925(17) 0.0235(8) Uani 1 1 d . . . N4 N 0.2627(2) 0.50952(18) 0.58461(16) 0.0220(7) Uani 1 1 d . . . N5 N 0.6983(2) 1.00627(19) 0.82093(17) 0.0242(8) Uani 1 1 d . . . N6 N 0.8049(2) 1.02388(19) 0.91254(17) 0.0257(8) Uani 1 1 d . . . N7 N 0.8771(2) 1.02654(19) 0.76486(18) 0.0251(8) Uani 1 1 d . . . N8 N 0.8644(2) 0.89269(18) 0.83183(17) 0.0246(8) Uani 1 1 d . . . C1 C 0.2271(3) 0.5021(2) 0.7947(2) 0.0280(10) Uani 1 1 d . . . H1 H 0.1598 0.5280 0.8136 0.034 Uiso 1 1 calc R . . C2 C 0.2805(3) 0.5618(3) 0.7839(3) 0.0373(11) Uani 1 1 d . . . H2A H 0.3467 0.5384 0.7614 0.045 Uiso 1 1 calc R . . H2B H 0.2545 0.5998 0.7525 0.045 Uiso 1 1 calc R . . C3 C 0.2757(4) 0.5997(4) 0.8503(3) 0.0573(15) Uani 1 1 d . . . H3A H 0.2106 0.6288 0.8699 0.069 Uiso 1 1 calc R . . H3B H 0.3151 0.6346 0.8402 0.069 Uiso 1 1 calc R . . C4 C 0.3089(5) 0.5437(4) 0.9029(3) 0.073(2) Uani 1 1 d . . . H4A H 0.3000 0.5696 0.9468 0.088 Uiso 1 1 calc R . . H4B H 0.3762 0.5188 0.8860 0.088 Uiso 1 1 calc R . . C5 C 0.2526(4) 0.4848(4) 0.9150(3) 0.0577(16) Uani 1 1 d . . . H5A H 0.2768 0.4473 0.9475 0.069 Uiso 1 1 calc R . . H5B H 0.1863 0.5095 0.9364 0.069 Uiso 1 1 calc R . . C6 C 0.2586(3) 0.4462(3) 0.8492(2) 0.0406(12) Uani 1 1 d . . . H6A H 0.2188 0.4117 0.8592 0.049 Uiso 1 1 calc R . . H6B H 0.3238 0.4166 0.8306 0.049 Uiso 1 1 calc R . . C7 C 0.3427(3) 0.2772(2) 0.6168(2) 0.0253(9) Uani 1 1 d . . . H7 H 0.3470 0.2615 0.6647 0.030 Uiso 1 1 calc R . . C8 C 0.4431(3) 0.2536(2) 0.5710(2) 0.0304(10) Uani 1 1 d . . . H8A H 0.4422 0.2686 0.5230 0.037 Uiso 1 1 calc R . . H8B H 0.4825 0.2793 0.5873 0.037 Uiso 1 1 calc R . . C9 C 0.4857(3) 0.1686(3) 0.5730(3) 0.0444(13) Uani 1 1 d . . . H9A H 0.5489 0.1549 0.5418 0.053 Uiso 1 1 calc R . . H9B H 0.4919 0.1542 0.6202 0.053 Uiso 1 1 calc R . . C10 C 0.4248(4) 0.1263(3) 0.5509(3) 0.0481(14) Uani 1 1 d . . . H10A H 0.4518 0.0723 0.5551 0.058 Uiso 1 1 calc R . . H10B H 0.4236 0.1368 0.5022 0.058 Uiso 1 1 calc R . . C11 C 0.3238(3) 0.1501(2) 0.5968(3) 0.0422(12) Uani 1 1 d . . . H11A H 0.2846 0.1244 0.5803 0.051 Uiso 1 1 calc R . . H11B H 0.3246 0.1349 0.6447 0.051 Uiso 1 1 calc R . . C12 C 0.2810(3) 0.2346(2) 0.5952(3) 0.0327(10) Uani 1 1 d . . . H12A H 0.2182 0.2482 0.6267 0.039 Uiso 1 1 calc R . . H12B H 0.2741 0.2491 0.5481 0.039 Uiso 1 1 calc R . . C13 C 0.0162(3) 0.4575(2) 0.6347(2) 0.0247(9) Uani 1 1 d . . . H13 H 0.0160 0.4784 0.5878 0.030 Uiso 1 1 calc R . . C14 C -0.0696(3) 0.5073(3) 0.6856(2) 0.0341(11) Uani 1 1 d . . . H14A H -0.0697 0.4897 0.7331 0.041 Uiso 1 1 calc R . . H14B H -0.0648 0.5590 0.6834 0.041 Uiso 1 1 calc R . . C15 C -0.1614(3) 0.5059(3) 0.6689(3) 0.0412(12) Uani 1 1 d . . . H15A H -0.1645 0.5285 0.6234 0.049 Uiso 1 1 calc R . . H15B H -0.2147 0.5357 0.7038 0.049 Uiso 1 1 calc R . . C16 C -0.1690(4) 0.4254(3) 0.6678(3) 0.0476(14) Uani 1 1 d . . . H16A H -0.1708 0.4040 0.7142 0.057 Uiso 1 1 calc R . . H16B H -0.2276 0.4256 0.6553 0.057 Uiso 1 1 calc R . . C17 C -0.0863(3) 0.3781(3) 0.6161(3) 0.0404(12) Uani 1 1 d . . . H17A H -0.0870 0.3977 0.5693 0.048 Uiso 1 1 calc R . . H17B H -0.0914 0.3266 0.6167 0.048 Uiso 1 1 calc R . . C18 C 0.0073(3) 0.3778(3) 0.6329(2) 0.0341(11) Uani 1 1 d . . . H18A H 0.0104 0.3544 0.6780 0.041 Uiso 1 1 calc R . . H18B H 0.0600 0.3480 0.5975 0.041 Uiso 1 1 calc R . . C19 C 0.3158(3) 0.5586(2) 0.5390(2) 0.0236(9) Uani 1 1 d . . . H19 H 0.3805 0.5270 0.5194 0.028 Uiso 1 1 calc R . . C20 C 0.3235(3) 0.6203(2) 0.5817(2) 0.0290(10) Uani 1 1 d . . . H20A H 0.3565 0.5979 0.6177 0.035 Uiso 1 1 calc R . . H20B H 0.2601 0.6498 0.6051 0.035 Uiso 1 1 calc R . . C21 C 0.3764(3) 0.6728(3) 0.5378(2) 0.0350(11) Uani 1 1 d . . . H21A H 0.3765 0.7136 0.5671 0.042 Uiso 1 1 calc R . . H21B H 0.4419 0.6449 0.5178 0.042 Uiso 1 1 calc R . . C22 C 0.3275(3) 0.7052(3) 0.4795(2) 0.0376(12) Uani 1 1 d . . . H22A H 0.2631 0.7354 0.4997 0.045 Uiso 1 1 calc R . . H22B H 0.3616 0.7381 0.4507 0.045 Uiso 1 1 calc R . . C23 C 0.3246(4) 0.6429(3) 0.4345(2) 0.0406(12) Uani 1 1 d . . . H23A H 0.3890 0.6144 0.4124 0.049 Uiso 1 1 calc R . . H23B H 0.2926 0.6646 0.3978 0.049 Uiso 1 1 calc R . . C24 C 0.2725(3) 0.5902(3) 0.4782(2) 0.0321(10) Uani 1 1 d . . . H24A H 0.2062 0.6176 0.4961 0.039 Uiso 1 1 calc R . . H24B H 0.2747 0.5487 0.4487 0.039 Uiso 1 1 calc R . . C25 C 0.4991(3) 0.3289(2) 0.7284(2) 0.0248(9) Uani 1 1 d . . . C26 C 0.5610(3) 0.2574(2) 0.7115(2) 0.0301(10) Uani 1 1 d . . . H26 H 0.5400 0.2205 0.6946 0.036 Uiso 1 1 calc R . . C27 C 0.6511(3) 0.2402(3) 0.7191(2) 0.0356(11) Uani 1 1 d . . . H27 H 0.6914 0.1919 0.7070 0.043 Uiso 1 1 calc R . . C28 C 0.6843(3) 0.2933(3) 0.7446(2) 0.0371(11) Uani 1 1 d . . . H28 H 0.7464 0.2813 0.7500 0.045 Uiso 1 1 calc R . . C29 C 0.6236(3) 0.3643(3) 0.7620(2) 0.0369(11) Uani 1 1 d . . . H29 H 0.6447 0.4009 0.7792 0.044 Uiso 1 1 calc R . . C30 C 0.5328(3) 0.3814(2) 0.7542(2) 0.0298(10) Uani 1 1 d . . . H30 H 0.4925 0.4297 0.7666 0.036 Uiso 1 1 calc R . . C31 C 0.0249(3) 0.4058(2) 0.8583(2) 0.0317(10) Uani 1 1 d . . . C32 C 0.0220(4) 0.4293(3) 0.9236(3) 0.0482(14) Uani 1 1 d . . . H32 H 0.0380 0.4737 0.9293 0.058 Uiso 1 1 calc R . . C33 C -0.0048(5) 0.3872(3) 0.9809(3) 0.0576(16) Uani 1 1 d . . . H33 H -0.0065 0.4034 1.0254 0.069 Uiso 1 1 calc R . . C34 C -0.0287(4) 0.3227(3) 0.9742(3) 0.0478(14) Uani 1 1 d . . . H34 H -0.0469 0.2948 1.0136 0.057 Uiso 1 1 calc R . . C35 C -0.0259(4) 0.2992(3) 0.9091(3) 0.0493(14) Uani 1 1 d . . . H35 H -0.0417 0.2547 0.9038 0.059 Uiso 1 1 calc R . . C36 C 0.0000(3) 0.3405(3) 0.8512(2) 0.0373(11) Uani 1 1 d . . . H36 H 0.0008 0.3244 0.8069 0.045 Uiso 1 1 calc R . . C37 C 0.3912(3) 0.3806(3) 0.4096(2) 0.0327(11) Uani 1 1 d . . . C38 C 0.4367(4) 0.4196(3) 0.3568(3) 0.0488(14) Uani 1 1 d . . . H38 H 0.4524 0.4624 0.3679 0.059 Uiso 1 1 calc R . . C39 C 0.4586(5) 0.3963(4) 0.2893(3) 0.0688(19) Uani 1 1 d . . . H39 H 0.4885 0.4238 0.2543 0.083 Uiso 1 1 calc R . . C40 C 0.4380(5) 0.3341(4) 0.2715(3) 0.0704(19) Uani 1 1 d . . . H40 H 0.4547 0.3182 0.2247 0.084 Uiso 1 1 calc R . . C41 C 0.3929(5) 0.2946(4) 0.3221(3) 0.0691(18) Uani 1 1 d . . . H41 H 0.3777 0.2519 0.3101 0.083 Uiso 1 1 calc R . . C42 C 0.3696(4) 0.3180(3) 0.3911(3) 0.0474(13) Uani 1 1 d . . . H42 H 0.3388 0.2908 0.4258 0.057 Uiso 1 1 calc R . . C43 C 0.0137(3) 0.6679(2) 0.5799(2) 0.0283(10) Uani 1 1 d . . . C44 C -0.0721(3) 0.6801(3) 0.5633(3) 0.0430(12) Uani 1 1 d . . . H44 H -0.0923 0.6392 0.5533 0.052 Uiso 1 1 calc R . . C45 C -0.1291(4) 0.7531(4) 0.5613(3) 0.0605(16) Uani 1 1 d . . . H45 H -0.1881 0.7611 0.5508 0.073 Uiso 1 1 calc R . . C46 C -0.1000(4) 0.8133(3) 0.5744(3) 0.0589(17) Uani 1 1 d . . . H46 H -0.1379 0.8624 0.5716 0.071 Uiso 1 1 calc R . . C47 C -0.0157(4) 0.8016(3) 0.5915(3) 0.0540(15) Uani 1 1 d . . . H47 H 0.0039 0.8427 0.6017 0.065 Uiso 1 1 calc R . . C48 C 0.0415(3) 0.7288(3) 0.5941(3) 0.0405(12) Uani 1 1 d . . . H48 H 0.0998 0.7213 0.6057 0.049 Uiso 1 1 calc R . . C49 C 0.5974(3) 1.0096(2) 0.8250(2) 0.0305(10) Uani 1 1 d . . . H49 H 0.5628 1.0189 0.8743 0.037 Uiso 1 1 calc R . . C50 C 0.5883(3) 0.9361(3) 0.8033(3) 0.0382(11) Uani 1 1 d . . . H50A H 0.6161 0.8959 0.8322 0.046 Uiso 1 1 calc R . . H50B H 0.6230 0.9247 0.7548 0.046 Uiso 1 1 calc R . . C51 C 0.4840(4) 0.9393(3) 0.8108(3) 0.0557(15) Uani 1 1 d . . . H51A H 0.4801 0.8919 0.7941 0.067 Uiso 1 1 calc R . . H51B H 0.4510 0.9455 0.8601 0.067 Uiso 1 1 calc R . . C52 C 0.4359(4) 1.0037(4) 0.7701(3) 0.0616(17) Uani 1 1 d . . . H52A H 0.3686 1.0068 0.7793 0.074 Uiso 1 1 calc R . . H52B H 0.4632 0.9942 0.7202 0.074 Uiso 1 1 calc R . . C53 C 0.4477(3) 1.0778(3) 0.7904(3) 0.0494(14) Uani 1 1 d . . . H53A H 0.4208 1.1177 0.7609 0.059 Uiso 1 1 calc R . . H53B H 0.4130 1.0906 0.8387 0.059 Uiso 1 1 calc R . . C54 C 0.5501(3) 1.0738(3) 0.7830(3) 0.0367(11) Uani 1 1 d . . . H54A H 0.5548 1.1214 0.7988 0.044 Uiso 1 1 calc R . . H54B H 0.5833 1.0665 0.7338 0.044 Uiso 1 1 calc R . . C55 C 0.8260(3) 1.0503(2) 0.9753(2) 0.0247(9) Uani 1 1 d . . . H55 H 0.8738 1.0082 0.9896 0.030 Uiso 1 1 calc R . . C56 C 0.7415(3) 1.0706(3) 1.0378(2) 0.0410(12) Uani 1 1 d . . . H56A H 0.6918 1.1114 1.0252 0.049 Uiso 1 1 calc R . . H56B H 0.7166 1.0271 1.0501 0.049 Uiso 1 1 calc R . . C57 C 0.7677(4) 1.0948(3) 1.0999(2) 0.0492(13) Uani 1 1 d . . . H57A H 0.8116 1.0520 1.1161 0.059 Uiso 1 1 calc R . . H57B H 0.7110 1.1106 1.1377 0.059 Uiso 1 1 calc R . . C58 C 0.8138(5) 1.1597(3) 1.0823(3) 0.0608(16) Uani 1 1 d . . . H58A H 0.7681 1.2043 1.0705 0.073 Uiso 1 1 calc R . . H58B H 0.8335 1.1721 1.1226 0.073 Uiso 1 1 calc R . . C59 C 0.8990(5) 1.1367(3) 1.0210(3) 0.0572(16) Uani 1 1 d . . . H59A H 0.9462 1.0940 1.0340 0.069 Uiso 1 1 calc R . . H59B H 0.9274 1.1784 1.0089 0.069 Uiso 1 1 calc R . . C60 C 0.8700(4) 1.1149(3) 0.9579(2) 0.0424(12) Uani 1 1 d . . . H60A H 0.8247 1.1581 0.9437 0.051 Uiso 1 1 calc R . . H60B H 0.9255 1.1003 0.9189 0.051 Uiso 1 1 calc R . . C61 C 0.9158(3) 1.0806(2) 0.7153(2) 0.0277(10) Uani 1 1 d . . . H61 H 0.8614 1.1182 0.7036 0.033 Uiso 1 1 calc R . . C62 C 0.9805(3) 1.0441(3) 0.6470(2) 0.0350(11) Uani 1 1 d . . . H62A H 1.0345 1.0055 0.6568 0.042 Uiso 1 1 calc R . . H62B H 0.9461 1.0197 0.6239 0.042 Uiso 1 1 calc R . . C63 C 1.0156(4) 1.1026(3) 0.5989(3) 0.0501(14) Uani 1 1 d . . . H63A H 1.0597 1.0775 0.5567 0.060 Uiso 1 1 calc R . . H63B H 0.9621 1.1380 0.5851 0.060 Uiso 1 1 calc R . . C64 C 1.0641(4) 1.1450(3) 0.6335(3) 0.0553(16) Uani 1 1 d . . . H64A H 1.0822 1.1839 0.6023 0.066 Uiso 1 1 calc R . . H64B H 1.1217 1.1105 0.6424 0.066 Uiso 1 1 calc R . . C65 C 1.0004(4) 1.1816(3) 0.7023(3) 0.0508(14) Uani 1 1 d . . . H65A H 0.9465 1.2206 0.6930 0.061 Uiso 1 1 calc R . . H65B H 1.0357 1.2053 0.7252 0.061 Uiso 1 1 calc R . . C66 C 0.9650(3) 1.1224(3) 0.7507(3) 0.0382(11) Uani 1 1 d . . . H66A H 1.0185 1.0866 0.7641 0.046 Uiso 1 1 calc R . . H66B H 0.9212 1.1473 0.7930 0.046 Uiso 1 1 calc R . . C67 C 0.9020(3) 0.8105(2) 0.8127(2) 0.0264(10) Uani 1 1 d . . . H67 H 0.9398 0.8065 0.7641 0.032 Uiso 1 1 calc R . . C68 C 0.8213(3) 0.7761(3) 0.8151(3) 0.0395(12) Uani 1 1 d . . . H68A H 0.7813 0.8050 0.7855 0.047 Uiso 1 1 calc R . . H68B H 0.7826 0.7791 0.8628 0.047 Uiso 1 1 calc R . . C69 C 0.8575(4) 0.6937(3) 0.7904(3) 0.0503(14) Uani 1 1 d . . . H69A H 0.8917 0.6905 0.7414 0.060 Uiso 1 1 calc R . . H69B H 0.8043 0.6724 0.7947 0.060 Uiso 1 1 calc R . . C70 C 0.9237(4) 0.6491(3) 0.8352(3) 0.0517(15) Uani 1 1 d . . . H70A H 0.8874 0.6482 0.8832 0.062 Uiso 1 1 calc R . . H70B H 0.9498 0.5972 0.8178 0.062 Uiso 1 1 calc R . . C71 C 1.0025(4) 0.6827(2) 0.8339(3) 0.0409(12) Uani 1 1 d . . . H71A H 1.0426 0.6789 0.7867 0.049 Uiso 1 1 calc R . . H71B H 1.0412 0.6543 0.8646 0.049 Uiso 1 1 calc R . . C72 C 0.9662(3) 0.7655(2) 0.8575(2) 0.0325(10) Uani 1 1 d . . . H72A H 0.9312 0.7692 0.9063 0.039 Uiso 1 1 calc R . . H72B H 1.0197 0.7864 0.8537 0.039 Uiso 1 1 calc R . . C73 C 0.5392(3) 1.1732(2) 0.9521(2) 0.0288(10) Uani 1 1 d . . . C74 C 0.5157(3) 1.2337(3) 0.9095(2) 0.0410(12) Uani 1 1 d . . . H74 H 0.5501 1.2325 0.8631 0.049 Uiso 1 1 calc R . . C75 C 0.4418(4) 1.2959(3) 0.9350(3) 0.0570(16) Uani 1 1 d . . . H75 H 0.4259 1.3362 0.9054 0.068 Uiso 1 1 calc R . . C76 C 0.3917(4) 1.2997(3) 1.0026(3) 0.070(2) Uani 1 1 d . . . H76 H 0.3421 1.3425 1.0197 0.084 Uiso 1 1 calc R . . C77 C 0.4149(4) 1.2396(4) 1.0460(3) 0.072(2) Uani 1 1 d . . . H77 H 0.3811 1.2416 1.0927 0.086 Uiso 1 1 calc R . . C78 C 0.4870(4) 1.1773(3) 1.0207(3) 0.0480(14) Uani 1 1 d . . . H78 H 0.5014 1.1365 1.0502 0.058 Uiso 1 1 calc R . . C79 C 0.8235(3) 0.8569(2) 1.0446(2) 0.0354(11) Uani 1 1 d . . . C80 C 0.7736(4) 0.8038(3) 1.0567(3) 0.0487(14) Uani 1 1 d . . . H80 H 0.7553 0.7857 1.0204 0.058 Uiso 1 1 calc R . . C81 C 0.7508(5) 0.7773(3) 1.1261(4) 0.073(2) Uani 1 1 d . . . H81 H 0.7169 0.7411 1.1361 0.088 Uiso 1 1 calc R . . C82 C 0.7783(5) 0.8048(4) 1.1782(3) 0.072(2) Uani 1 1 d . . . H82 H 0.7638 0.7865 1.2234 0.087 Uiso 1 1 calc R . . C83 C 0.8258(5) 0.8578(4) 1.1656(3) 0.072(2) Uani 1 1 d . . . H83 H 0.8424 0.8771 1.2021 0.086 Uiso 1 1 calc R . . C84 C 0.8497(4) 0.8831(3) 1.0988(3) 0.0515(14) Uani 1 1 d . . . H84 H 0.8845 0.9187 1.0899 0.062 Uiso 1 1 calc R . . C85 C 0.7431(3) 1.0450(2) 0.6109(2) 0.0285(10) Uani 1 1 d . . . C86 C 0.6946(3) 0.9967(3) 0.5968(2) 0.0372(11) Uani 1 1 d . . . H86 H 0.6687 0.9682 0.6329 0.045 Uiso 1 1 calc R . . C87 C 0.6836(4) 0.9899(3) 0.5303(3) 0.0524(14) Uani 1 1 d . . . H87 H 0.6507 0.9568 0.5214 0.063 Uiso 1 1 calc R . . C88 C 0.7212(5) 1.0316(3) 0.4769(3) 0.0612(17) Uani 1 1 d . . . H88 H 0.7146 1.0264 0.4317 0.073 Uiso 1 1 calc R . . C89 C 0.7679(4) 1.0805(3) 0.4902(3) 0.0583(16) Uani 1 1 d . . . H89 H 0.7928 1.1093 0.4540 0.070 Uiso 1 1 calc R . . C90 C 0.7791(4) 1.0880(3) 0.5567(2) 0.0440(12) Uani 1 1 d . . . H90 H 0.8108 1.1221 0.5652 0.053 Uiso 1 1 calc R . . C91 C 1.1361(3) 0.8704(3) 0.7296(2) 0.0300(10) Uani 1 1 d . . . C92 C 1.1835(3) 0.7939(3) 0.7232(3) 0.0434(12) Uani 1 1 d . . . H92 H 1.1487 0.7585 0.7278 0.052 Uiso 1 1 calc R . . C93 C 1.2792(4) 0.7700(3) 0.7106(3) 0.0562(15) Uani 1 1 d . . . H93 H 1.3096 0.7183 0.7078 0.067 Uiso 1 1 calc R . . C94 C 1.3324(4) 0.8213(4) 0.7017(3) 0.0550(15) Uani 1 1 d . . . H94 H 1.3985 0.8048 0.6920 0.066 Uiso 1 1 calc R . . C95 C 1.2865(4) 0.8967(4) 0.7074(3) 0.0519(14) Uani 1 1 d . . . H95 H 1.3220 0.9318 0.7012 0.062 Uiso 1 1 calc R . . C96 C 1.1905(4) 0.9216(3) 0.7218(2) 0.0407(12) Uani 1 1 d . . . H96 H 1.1606 0.9734 0.7265 0.049 Uiso 1 1 calc R . . C97 C 0.6710(6) 0.4091(4) 0.9231(3) 0.0695(19) Uani 1 1 d . . . C98 C 0.7492(6) 0.4336(5) 0.8961(4) 0.087(2) Uani 1 1 d . . . H98 H 0.8092 0.4014 0.8956 0.104 Uiso 1 1 calc R . . C99 C 0.7418(7) 0.5036(6) 0.8700(4) 0.105(3) Uani 1 1 d . . . H99 H 0.7971 0.5183 0.8517 0.126 Uiso 1 1 calc R . . C100 C 0.6595(7) 0.5519(5) 0.8693(4) 0.095(3) Uani 1 1 d . . . H100 H 0.6563 0.6003 0.8515 0.114 Uiso 1 1 calc R . . C101 C 0.5775(6) 0.5290(5) 0.8958(5) 0.091(2) Uani 1 1 d . . . H101 H 0.5183 0.5620 0.8950 0.109 Uiso 1 1 calc R . . C102 C 0.5829(5) 0.4597(5) 0.9226(4) 0.076(2) Uani 1 1 d . . . H102 H 0.5274 0.4452 0.9410 0.091 Uiso 1 1 calc R . . C103 C 0.6780(8) 0.3323(5) 0.9494(6) 0.129(4) Uani 1 1 d . . . H10C H 0.6784 0.2999 0.9125 0.194 Uiso 1 1 calc R . . H10D H 0.6244 0.3329 0.9879 0.194 Uiso 1 1 calc R . . H10E H 0.7358 0.3136 0.9650 0.194 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 Sb1 0.02077(15) 0.02171(14) 0.02242(15) 0.00174(12) -0.00622(10) -0.00555(11) Sb2 0.02557(16) 0.02072(14) 0.02178(15) 0.00570(12) -0.00426(11) -0.00617(11) Sb3 0.02464(15) 0.02676(15) 0.01964(15) 0.00147(12) -0.00650(11) -0.00847(12) Sb4 0.02236(15) 0.01968(14) 0.02116(15) 0.00265(12) -0.00439(11) -0.00509(11) Sb5 0.03006(16) 0.01937(14) 0.02210(15) 0.00322(12) -0.00946(11) -0.00368(12) Sb6 0.02906(16) 0.02255(15) 0.02143(15) 0.00364(12) -0.00352(11) -0.00707(12) Sb7 0.02711(16) 0.02286(14) 0.01990(15) 0.00052(12) -0.00685(11) -0.00589(11) Sb8 0.02554(16) 0.02459(15) 0.02282(15) 0.00471(12) -0.00906(11) -0.00565(12) O1 0.0318(17) 0.0282(15) 0.0301(16) 0.0072(14) -0.0094(12) -0.0090(13) O2 0.0348(17) 0.0269(15) 0.0300(16) 0.0071(14) 0.0035(13) -0.0046(13) O3 0.0289(16) 0.0455(18) 0.0241(16) -0.0061(15) 0.0016(12) -0.0109(14) O4 0.0377(17) 0.0247(15) 0.0313(16) 0.0064(14) -0.0156(13) -0.0066(13) O5 0.0358(18) 0.0291(16) 0.0312(17) 0.0052(14) -0.0014(13) -0.0014(13) O6 0.0399(18) 0.0329(16) 0.0248(16) 0.0082(14) -0.0090(13) -0.0071(14) O7 0.0439(18) 0.0258(15) 0.0241(15) 0.0022(13) -0.0140(13) -0.0085(13) O8 0.0341(18) 0.0419(18) 0.0288(16) -0.0041(15) -0.0042(13) -0.0084(14) N1 0.0193(17) 0.0237(17) 0.0223(17) 0.0007(15) -0.0044(13) -0.0010(14) N2 0.0256(18) 0.0237(17) 0.0221(17) 0.0047(15) -0.0082(14) -0.0049(14) N3 0.0238(18) 0.0246(17) 0.0227(17) 0.0074(15) -0.0075(13) -0.0073(14) N4 0.0184(17) 0.0263(17) 0.0194(17) 0.0042(15) -0.0023(13) -0.0057(14) N5 0.0250(18) 0.0258(17) 0.0217(17) 0.0005(15) -0.0058(14) -0.0065(14) N6 0.033(2) 0.0231(17) 0.0199(17) 0.0029(15) -0.0079(14) -0.0046(15) N7 0.0227(18) 0.0249(17) 0.0286(19) 0.0093(16) -0.0090(14) -0.0071(14) N8 0.0280(19) 0.0217(17) 0.0231(18) 0.0044(15) -0.0048(14) -0.0070(14) C1 0.029(2) 0.030(2) 0.021(2) -0.0017(19) -0.0084(17) 0.0009(18) C2 0.037(3) 0.039(3) 0.040(3) -0.011(2) -0.014(2) -0.010(2) C3 0.053(3) 0.070(4) 0.052(3) -0.025(3) -0.009(3) -0.021(3) C4 0.076(5) 0.103(5) 0.043(3) -0.022(4) -0.035(3) -0.006(4) C5 0.066(4) 0.071(4) 0.027(3) -0.004(3) -0.023(2) 0.007(3) C6 0.042(3) 0.046(3) 0.025(2) 0.003(2) -0.0098(19) 0.003(2) C7 0.027(2) 0.0196(19) 0.028(2) 0.0000(18) -0.0051(17) -0.0052(17) C8 0.027(2) 0.026(2) 0.035(2) -0.006(2) -0.0041(18) -0.0047(18) C9 0.033(3) 0.029(2) 0.066(4) -0.016(3) -0.007(2) 0.000(2) C10 0.043(3) 0.026(2) 0.070(4) -0.019(3) -0.009(3) -0.001(2) C11 0.038(3) 0.027(2) 0.062(3) -0.008(2) -0.003(2) -0.014(2) C12 0.028(2) 0.028(2) 0.043(3) -0.005(2) -0.0051(19) -0.0102(19) C13 0.022(2) 0.029(2) 0.026(2) 0.0078(19) -0.0088(16) -0.0104(17) C14 0.025(2) 0.037(2) 0.038(3) 0.001(2) -0.0061(19) -0.0054(19) C15 0.026(2) 0.057(3) 0.039(3) -0.001(2) -0.0052(19) -0.011(2) C16 0.040(3) 0.079(4) 0.039(3) 0.022(3) -0.019(2) -0.036(3) C17 0.049(3) 0.044(3) 0.042(3) 0.013(2) -0.021(2) -0.027(2) C18 0.037(3) 0.032(2) 0.039(3) 0.009(2) -0.017(2) -0.013(2) C19 0.020(2) 0.029(2) 0.023(2) 0.0094(18) -0.0031(16) -0.0108(17) C20 0.028(2) 0.037(2) 0.026(2) 0.006(2) -0.0066(17) -0.0162(19) C21 0.038(3) 0.031(2) 0.041(3) 0.010(2) -0.009(2) -0.021(2) C22 0.036(3) 0.038(3) 0.042(3) 0.014(2) -0.007(2) -0.019(2) C23 0.047(3) 0.046(3) 0.034(3) 0.023(2) -0.014(2) -0.021(2) C24 0.041(3) 0.037(2) 0.024(2) 0.012(2) -0.0108(19) -0.019(2) C25 0.029(2) 0.027(2) 0.018(2) 0.0067(18) -0.0073(16) -0.0065(17) C26 0.041(3) 0.025(2) 0.025(2) 0.006(2) -0.0126(19) -0.007(2) C27 0.036(3) 0.031(2) 0.029(2) 0.010(2) -0.0059(19) 0.004(2) C28 0.030(2) 0.050(3) 0.028(2) 0.011(2) -0.0088(18) -0.008(2) C29 0.042(3) 0.046(3) 0.028(2) 0.003(2) -0.012(2) -0.017(2) C30 0.031(2) 0.026(2) 0.029(2) 0.000(2) -0.0055(18) -0.0052(18) C31 0.031(2) 0.031(2) 0.025(2) 0.004(2) 0.0043(18) -0.0056(18) C32 0.068(4) 0.039(3) 0.034(3) -0.006(2) 0.002(2) -0.020(3) C33 0.095(5) 0.049(3) 0.025(3) 0.003(3) -0.005(3) -0.022(3) C34 0.062(3) 0.043(3) 0.033(3) 0.009(3) -0.003(2) -0.015(3) C35 0.056(3) 0.039(3) 0.050(3) 0.009(3) 0.001(3) -0.021(2) C36 0.039(3) 0.043(3) 0.029(2) -0.001(2) 0.0009(19) -0.017(2) C37 0.027(2) 0.038(2) 0.026(2) 0.002(2) -0.0050(18) 0.0009(19) C38 0.050(3) 0.061(3) 0.033(3) 0.007(3) 0.000(2) -0.020(3) C39 0.075(4) 0.091(5) 0.030(3) 0.005(3) 0.008(3) -0.025(4) C40 0.081(5) 0.093(5) 0.023(3) -0.013(3) -0.002(3) -0.007(4) C41 0.091(5) 0.060(4) 0.057(4) -0.018(3) -0.022(3) -0.015(4) C42 0.062(3) 0.049(3) 0.030(3) -0.007(3) -0.003(2) -0.020(3) C43 0.030(2) 0.029(2) 0.021(2) 0.0024(19) -0.0049(17) -0.0010(18) C44 0.036(3) 0.047(3) 0.048(3) 0.005(3) -0.022(2) -0.006(2) C45 0.042(3) 0.070(4) 0.061(4) -0.001(3) -0.025(3) 0.009(3) C46 0.060(4) 0.048(3) 0.048(3) 0.004(3) -0.011(3) 0.017(3) C47 0.065(4) 0.026(2) 0.063(4) 0.000(3) -0.016(3) 0.002(2) C48 0.040(3) 0.035(3) 0.044(3) 0.008(2) -0.012(2) -0.006(2) C49 0.028(2) 0.036(2) 0.025(2) 0.003(2) -0.0029(17) -0.0090(19) C50 0.036(3) 0.039(3) 0.046(3) -0.001(2) -0.013(2) -0.016(2) C51 0.041(3) 0.062(4) 0.074(4) 0.009(3) -0.016(3) -0.030(3) C52 0.039(3) 0.088(4) 0.070(4) 0.007(4) -0.025(3) -0.027(3) C53 0.029(3) 0.065(3) 0.053(3) 0.009(3) -0.019(2) -0.004(2) C54 0.034(3) 0.037(2) 0.041(3) 0.005(2) -0.019(2) -0.005(2) C55 0.029(2) 0.028(2) 0.018(2) 0.0028(18) -0.0112(16) -0.0049(17) C56 0.041(3) 0.054(3) 0.026(2) -0.010(2) -0.005(2) -0.011(2) C57 0.061(4) 0.060(3) 0.023(2) -0.011(3) -0.006(2) -0.011(3) C58 0.103(5) 0.050(3) 0.040(3) -0.006(3) -0.039(3) -0.017(3) C59 0.094(5) 0.059(3) 0.042(3) 0.012(3) -0.032(3) -0.047(3) C60 0.066(3) 0.043(3) 0.031(3) 0.004(2) -0.019(2) -0.029(3) C61 0.029(2) 0.027(2) 0.027(2) 0.0122(19) -0.0063(17) -0.0107(18) C62 0.036(3) 0.039(3) 0.032(2) 0.013(2) -0.0097(19) -0.015(2) C63 0.047(3) 0.062(3) 0.037(3) 0.018(3) -0.001(2) -0.020(3) C64 0.049(3) 0.063(4) 0.062(4) 0.029(3) -0.013(3) -0.033(3) C65 0.067(4) 0.045(3) 0.056(3) 0.021(3) -0.022(3) -0.037(3) C66 0.043(3) 0.039(3) 0.040(3) 0.012(2) -0.015(2) -0.019(2) C67 0.029(2) 0.020(2) 0.025(2) -0.0020(18) -0.0030(17) 0.0000(17) C68 0.042(3) 0.028(2) 0.051(3) 0.001(2) -0.016(2) -0.010(2) C69 0.059(3) 0.028(2) 0.064(4) -0.005(3) -0.015(3) -0.012(2) C70 0.076(4) 0.018(2) 0.053(3) 0.000(2) -0.010(3) -0.005(2) C71 0.051(3) 0.024(2) 0.038(3) 0.000(2) -0.007(2) 0.002(2) C72 0.035(2) 0.028(2) 0.031(2) 0.003(2) -0.0083(19) -0.0018(19) C73 0.028(2) 0.028(2) 0.026(2) -0.0013(19) -0.0033(17) -0.0039(18) C74 0.047(3) 0.036(3) 0.030(2) 0.001(2) -0.004(2) 0.001(2) C75 0.059(4) 0.040(3) 0.055(3) 0.008(3) -0.008(3) 0.007(3) C76 0.058(4) 0.049(3) 0.068(4) -0.001(3) 0.015(3) 0.016(3) C77 0.059(4) 0.079(4) 0.045(3) 0.000(3) 0.020(3) 0.005(3) C78 0.047(3) 0.046(3) 0.038(3) 0.009(3) 0.001(2) -0.004(2) C79 0.041(3) 0.027(2) 0.026(2) 0.004(2) -0.0057(19) 0.007(2) C80 0.058(3) 0.030(2) 0.050(3) 0.012(2) -0.007(3) -0.005(2) C81 0.062(4) 0.041(3) 0.095(5) 0.035(4) 0.003(4) -0.005(3) C82 0.068(4) 0.076(5) 0.040(3) 0.023(4) -0.003(3) 0.020(4) C83 0.084(5) 0.074(4) 0.036(3) 0.014(3) -0.020(3) 0.015(4) C84 0.057(3) 0.053(3) 0.037(3) 0.009(3) -0.018(2) 0.002(3) C85 0.034(2) 0.027(2) 0.023(2) -0.0031(19) -0.0114(17) -0.0015(18) C86 0.047(3) 0.032(2) 0.033(3) -0.002(2) -0.013(2) -0.009(2) C87 0.065(4) 0.051(3) 0.047(3) -0.011(3) -0.028(3) -0.012(3) C88 0.090(5) 0.055(3) 0.035(3) -0.009(3) -0.030(3) 0.003(3) C89 0.077(4) 0.060(4) 0.031(3) 0.017(3) -0.012(3) -0.011(3) C90 0.055(3) 0.045(3) 0.033(3) 0.009(2) -0.013(2) -0.015(2) C91 0.031(2) 0.037(2) 0.019(2) -0.003(2) -0.0018(17) -0.0068(19) C92 0.041(3) 0.038(3) 0.044(3) -0.010(2) -0.003(2) -0.004(2) C93 0.050(3) 0.051(3) 0.056(4) -0.010(3) -0.008(3) 0.003(3) C94 0.031(3) 0.074(4) 0.046(3) -0.009(3) -0.007(2) 0.007(3) C95 0.049(3) 0.078(4) 0.039(3) -0.002(3) -0.011(2) -0.034(3) C96 0.044(3) 0.042(3) 0.038(3) 0.006(2) -0.013(2) -0.013(2) C97 0.092(5) 0.071(4) 0.050(4) -0.017(3) -0.035(3) -0.011(4) C98 0.072(5) 0.107(6) 0.067(5) -0.019(5) -0.015(4) 0.000(5) C99 0.097(7) 0.141(8) 0.070(5) 0.020(6) -0.009(4) -0.036(6) C100 0.100(7) 0.099(6) 0.083(6) 0.009(5) -0.032(5) -0.018(5) C101 0.076(5) 0.081(5) 0.100(6) -0.012(5) -0.025(5) 0.008(4) C102 0.062(4) 0.095(5) 0.070(4) -0.026(4) -0.017(3) -0.014(4) C103 0.204(12) 0.080(6) 0.143(9) 0.012(6) -0.107(9) -0.049(7) _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 O1 2.060(3) . ? Sb1 N2 2.081(4) . ? Sb1 N1 2.083(3) . ? Sb1 N4 2.478(3) . ? Sb2 O2 2.058(3) . ? Sb2 N3 2.076(3) . ? Sb2 N1 2.082(3) . ? Sb2 N2 2.511(3) . ? Sb3 O3 2.059(3) . ? Sb3 N2 2.073(3) . ? Sb3 N4 2.090(4) . ? Sb3 N3 2.533(3) . ? Sb4 O4 2.056(3) . ? Sb4 N3 2.082(3) . ? Sb4 N4 2.083(3) . ? Sb4 N1 2.506(3) . ? Sb5 O5 2.046(3) . ? Sb5 N6 2.071(3) . ? Sb5 N5 2.081(4) . ? Sb5 N7 2.574(3) . ? Sb6 O6 2.051(3) . ? Sb6 N8 2.077(3) . ? Sb6 N6 2.089(3) . ? Sb6 N5 2.550(3) . ? Sb7 O7 2.069(3) . ? Sb7 N5 2.071(3) . ? Sb7 N7 2.075(4) . ? Sb7 N8 2.509(3) . ? Sb7 Sb8 3.3097(7) . ? Sb8 O8 2.064(3) . ? Sb8 N7 2.072(3) . ? Sb8 N8 2.078(3) . ? Sb8 N6 2.543(3) . ? O1 C25 1.355(5) . ? O2 C31 1.373(5) . ? O3 C37 1.353(6) . ? O4 C43 1.368(5) . ? O5 C73 1.352(5) . ? O6 C79 1.366(5) . ? O7 C85 1.353(5) . ? O8 C91 1.350(5) . ? N1 C1 1.497(6) . ? N2 C7 1.494(5) . ? N3 C13 1.490(5) . ? N4 C19 1.504(4) . ? N5 C49 1.500(5) . ? N6 C55 1.497(6) . ? N7 C61 1.503(5) . ? N8 C67 1.506(5) . ? C1 C2 1.523(6) . ? C1 C6 1.526(6) . ? C2 C3 1.504(8) . ? C3 C4 1.506(9) . ? C4 C5 1.541(9) . ? C5 C6 1.494(7) . ? C7 C12 1.528(6) . ? C7 C8 1.531(5) . ? C8 C9 1.531(6) . ? C9 C10 1.518(7) . ? C10 C11 1.538(7) . ? C11 C12 1.522(6) . ? C13 C18 1.525(6) . ? C13 C14 1.537(6) . ? C14 C15 1.519(6) . ? C15 C16 1.531(7) . ? C16 C17 1.503(8) . ? C17 C18 1.537(6) . ? C19 C20 1.508(6) . ? C19 C24 1.527(6) . ? C20 C21 1.535(5) . ? C21 C22 1.532(7) . ? C22 C23 1.514(7) . ? C23 C24 1.529(5) . ? C25 C30 1.391(6) . ? C25 C26 1.399(6) . ? C26 C27 1.363(6) . ? C27 C28 1.391(7) . ? C28 C29 1.387(7) . ? C29 C30 1.373(6) . ? C31 C32 1.375(7) . ? C31 C36 1.388(7) . ? C32 C33 1.388(7) . ? C33 C34 1.366(8) . ? C34 C35 1.373(8) . ? C35 C36 1.383(6) . ? C37 C42 1.381(7) . ? C37 C38 1.394(6) . ? C38 C39 1.362(8) . ? C39 C40 1.363(10) . ? C40 C41 1.371(9) . ? C41 C42 1.390(8) . ? C43 C48 1.376(7) . ? C43 C44 1.380(7) . ? C44 C45 1.396(8) . ? C45 C46 1.369(9) . ? C46 C47 1.363(9) . ? C47 C48 1.394(7) . ? C49 C50 1.504(6) . ? C49 C54 1.529(6) . ? C50 C51 1.541(7) . ? C51 C52 1.520(8) . ? C52 C53 1.523(9) . ? C53 C54 1.509(6) . ? C55 C60 1.513(6) . ? C55 C56 1.527(6) . ? C56 C57 1.510(7) . ? C57 C58 1.539(8) . ? C58 C59 1.523(9) . ? C59 C60 1.532(7) . ? C61 C66 1.513(7) . ? C61 C62 1.531(6) . ? C62 C63 1.529(6) . ? C63 C64 1.505(8) . ? C64 C65 1.533(8) . ? C65 C66 1.542(6) . ? C67 C68 1.523(6) . ? C67 C72 1.526(6) . ? C68 C69 1.537(7) . ? C69 C70 1.543(8) . ? C70 C71 1.493(8) . ? C71 C72 1.538(6) . ? C73 C74 1.387(6) . ? C73 C78 1.392(6) . ? C74 C75 1.384(7) . ? C75 C76 1.366(8) . ? C76 C77 1.391(8) . ? C77 C78 1.371(8) . ? C79 C80 1.380(7) . ? C79 C84 1.388(8) . ? C80 C81 1.431(8) . ? C81 C82 1.375(10) . ? C82 C83 1.353(11) . ? C83 C84 1.378(7) . ? C85 C86 1.386(7) . ? C85 C90 1.399(6) . ? C86 C87 1.387(7) . ? C87 C88 1.381(8) . ? C88 C89 1.369(9) . ? C89 C90 1.388(8) . ? C91 C92 1.399(7) . ? C91 C96 1.403(7) . ? C92 C93 1.361(7) . ? C93 C94 1.392(8) . ? C94 C95 1.375(8) . ? C95 C96 1.366(7) . ? C97 C98 1.368(10) . ? C97 C102 1.407(10) . ? C97 C103 1.476(10) . ? C98 C99 1.356(12) . ? C99 C100 1.323(12) . ? C100 C101 1.402(11) . ? C101 C102 1.354(11) . ? 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 O1 Sb1 N2 87.58(12) . . ? O1 Sb1 N1 91.37(12) . . ? N2 Sb1 N1 83.85(13) . . ? O1 Sb1 N4 158.80(11) . . ? N2 Sb1 N4 73.89(12) . . ? N1 Sb1 N4 76.75(12) . . ? O2 Sb2 N3 91.02(13) . . ? O2 Sb2 N1 88.64(13) . . ? N3 Sb2 N1 84.10(13) . . ? O2 Sb2 N2 160.00(11) . . ? N3 Sb2 N2 77.78(12) . . ? N1 Sb2 N2 73.90(12) . . ? O3 Sb3 N2 91.16(12) . . ? O3 Sb3 N4 86.80(12) . . ? N2 Sb3 N4 83.00(13) . . ? O3 Sb3 N3 158.25(12) . . ? N2 Sb3 N3 77.31(12) . . ? N4 Sb3 N3 73.66(11) . . ? O4 Sb4 N3 86.57(12) . . ? O4 Sb4 N4 91.44(12) . . ? N3 Sb4 N4 84.28(13) . . ? O4 Sb4 N1 157.80(12) . . ? N3 Sb4 N1 74.11(12) . . ? N4 Sb4 N1 76.11(11) . . ? O5 Sb5 N6 89.90(12) . . ? O5 Sb5 N5 85.31(13) . . ? N6 Sb5 N5 84.78(14) . . ? O5 Sb5 N7 154.62(11) . . ? N6 Sb5 N7 75.44(12) . . ? N5 Sb5 N7 72.99(12) . . ? O6 Sb6 N8 88.74(13) . . ? O6 Sb6 N6 86.39(13) . . ? N8 Sb6 N6 84.17(13) . . ? O6 Sb6 N5 155.27(11) . . ? N8 Sb6 N5 75.31(12) . . ? N6 Sb6 N5 73.48(12) . . ? O7 Sb7 N5 91.43(12) . . ? O7 Sb7 N7 85.43(12) . . ? N5 Sb7 N7 84.83(14) . . ? O7 Sb7 N8 156.88(12) . . ? N5 Sb7 N8 76.32(12) . . ? N7 Sb7 N8 74.13(12) . . ? O7 Sb7 Sb8 122.36(9) . . ? N5 Sb7 Sb8 87.00(10) . . ? N7 Sb7 Sb8 37.02(9) . . ? N8 Sb7 Sb8 38.87(8) . . ? O8 Sb8 N7 91.37(13) . . ? O8 Sb8 N8 86.43(13) . . ? N7 Sb8 N8 84.30(13) . . ? O8 Sb8 N6 157.22(13) . . ? N7 Sb8 N6 76.14(12) . . ? N8 Sb8 N6 73.58(12) . . ? O8 Sb8 Sb7 78.70(9) . . ? N7 Sb8 Sb7 37.09(10) . . ? N8 Sb8 Sb7 49.26(9) . . ? N6 Sb8 Sb7 79.96(8) . . ? C25 O1 Sb1 119.1(2) . . ? C31 O2 Sb2 115.6(2) . . ? C37 O3 Sb3 121.2(3) . . ? C43 O4 Sb4 121.0(3) . . ? C73 O5 Sb5 127.3(2) . . ? C79 O6 Sb6 122.9(3) . . ? C85 O7 Sb7 121.0(2) . . ? C91 O8 Sb8 122.7(3) . . ? C1 N1 Sb2 119.8(2) . . ? C1 N1 Sb1 120.6(3) . . ? Sb2 N1 Sb1 106.43(15) . . ? C1 N1 Sb4 109.9(2) . . ? Sb2 N1 Sb4 92.54(13) . . ? Sb1 N1 Sb4 102.69(12) . . ? C7 N2 Sb3 122.7(3) . . ? C7 N2 Sb1 119.5(3) . . ? Sb3 N2 Sb1 106.62(14) . . ? C7 N2 Sb2 107.2(2) . . ? Sb3 N2 Sb2 102.46(13) . . ? Sb1 N2 Sb2 92.71(13) . . ? C13 N3 Sb2 121.5(2) . . ? C13 N3 Sb4 119.2(2) . . ? Sb2 N3 Sb4 106.39(16) . . ? C13 N3 Sb3 110.6(2) . . ? Sb2 N3 Sb3 101.64(13) . . ? Sb4 N3 Sb3 92.22(11) . . ? C19 N4 Sb4 119.7(2) . . ? C19 N4 Sb3 120.0(2) . . ? Sb4 N4 Sb3 106.39(14) . . ? C19 N4 Sb1 109.4(2) . . ? Sb4 N4 Sb1 103.66(12) . . ? Sb3 N4 Sb1 93.27(12) . . ? C49 N5 Sb7 120.3(3) . . ? C49 N5 Sb5 118.7(3) . . ? Sb7 N5 Sb5 107.41(14) . . ? C49 N5 Sb6 110.8(2) . . ? Sb7 N5 Sb6 103.38(13) . . ? Sb5 N5 Sb6 91.26(13) . . ? C55 N6 Sb5 120.3(2) . . ? C55 N6 Sb6 119.2(2) . . ? Sb5 N6 Sb6 106.19(16) . . ? C55 N6 Sb8 110.5(2) . . ? Sb5 N6 Sb8 104.60(13) . . ? Sb6 N6 Sb8 91.53(13) . . ? C61 N7 Sb8 121.3(3) . . ? C61 N7 Sb7 120.1(3) . . ? Sb8 N7 Sb7 105.89(14) . . ? C61 N7 Sb5 109.3(2) . . ? Sb8 N7 Sb5 103.50(13) . . ? Sb7 N7 Sb5 91.44(12) . . ? C67 N8 Sb6 120.2(2) . . ? C67 N8 Sb8 120.1(2) . . ? Sb6 N8 Sb8 106.73(16) . . ? C67 N8 Sb7 108.5(2) . . ? Sb6 N8 Sb7 104.60(14) . . ? Sb8 N8 Sb7 91.86(11) . . ? N1 C1 C2 110.7(3) . . ? N1 C1 C6 114.2(3) . . ? C2 C1 C6 110.4(4) . . ? C3 C2 C1 113.5(4) . . ? C2 C3 C4 111.6(5) . . ? C3 C4 C5 109.8(5) . . ? C6 C5 C4 112.4(5) . . ? C5 C6 C1 111.8(4) . . ? N2 C7 C12 112.1(3) . . ? N2 C7 C8 113.5(3) . . ? C12 C7 C8 110.6(4) . . ? C9 C8 C7 111.1(3) . . ? C10 C9 C8 111.2(4) . . ? C9 C10 C11 110.3(4) . . ? C12 C11 C10 111.4(4) . . ? C11 C12 C7 111.2(4) . . ? N3 C13 C18 110.7(3) . . ? N3 C13 C14 113.5(4) . . ? C18 C13 C14 110.7(3) . . ? C15 C14 C13 111.5(4) . . ? C14 C15 C16 110.9(4) . . ? C17 C16 C15 110.3(4) . . ? C16 C17 C18 111.2(4) . . ? C13 C18 C17 110.8(4) . . ? N4 C19 C20 110.3(3) . . ? N4 C19 C24 112.5(3) . . ? C20 C19 C24 111.3(3) . . ? C19 C20 C21 112.6(3) . . ? C22 C21 C20 109.2(4) . . ? C23 C22 C21 110.6(4) . . ? C22 C23 C24 110.7(4) . . ? C19 C24 C23 111.6(4) . . ? O1 C25 C30 122.5(4) . . ? O1 C25 C26 120.1(4) . . ? C30 C25 C26 117.4(4) . . ? C27 C26 C25 121.3(4) . . ? C26 C27 C28 120.8(4) . . ? C29 C28 C27 118.5(5) . . ? C30 C29 C28 120.5(5) . . ? C29 C30 C25 121.4(4) . . ? O2 C31 C32 118.7(4) . . ? O2 C31 C36 122.1(4) . . ? C32 C31 C36 119.2(4) . . ? C31 C32 C33 119.5(5) . . ? C34 C33 C32 121.6(5) . . ? C33 C34 C35 118.9(4) . . ? C34 C35 C36 120.5(5) . . ? C35 C36 C31 120.3(5) . . ? O3 C37 C42 122.9(4) . . ? O3 C37 C38 119.2(5) . . ? C42 C37 C38 117.9(5) . . ? C39 C38 C37 120.5(6) . . ? C38 C39 C40 121.3(5) . . ? C39 C40 C41 119.7(6) . . ? C40 C41 C42 119.6(6) . . ? C37 C42 C41 121.0(5) . . ? O4 C43 C48 122.9(4) . . ? O4 C43 C44 118.2(4) . . ? C48 C43 C44 118.8(4) . . ? C43 C44 C45 119.9(5) . . ? C46 C45 C44 120.7(6) . . ? C47 C46 C45 119.6(5) . . ? C46 C47 C48 120.2(6) . . ? C43 C48 C47 120.7(5) . . ? N5 C49 C50 111.4(4) . . ? N5 C49 C54 112.9(3) . . ? C50 C49 C54 110.3(4) . . ? C49 C50 C51 110.8(4) . . ? C52 C51 C50 111.7(4) . . ? C51 C52 C53 110.9(5) . . ? C54 C53 C52 111.5(5) . . ? C53 C54 C49 111.7(4) . . ? N6 C55 C60 111.1(3) . . ? N6 C55 C56 114.2(4) . . ? C60 C55 C56 110.5(4) . . ? C57 C56 C55 111.8(4) . . ? C56 C57 C58 111.6(4) . . ? C59 C58 C57 109.4(5) . . ? C58 C59 C60 110.6(5) . . ? C55 C60 C59 110.4(4) . . ? N7 C61 C66 110.2(3) . . ? N7 C61 C62 113.7(3) . . ? C66 C61 C62 111.0(4) . . ? C63 C62 C61 110.8(4) . . ? C64 C63 C62 111.6(4) . . ? C63 C64 C65 111.7(4) . . ? C64 C65 C66 110.5(4) . . ? C61 C66 C65 111.2(4) . . ? N8 C67 C68 110.5(3) . . ? N8 C67 C72 113.7(4) . . ? C68 C67 C72 110.1(3) . . ? C67 C68 C69 111.7(4) . . ? C68 C69 C70 109.1(5) . . ? C71 C70 C69 111.7(4) . . ? C70 C71 C72 111.9(4) . . ? C67 C72 C71 110.4(4) . . ? O5 C73 C74 123.8(4) . . ? O5 C73 C78 118.1(4) . . ? C74 C73 C78 118.2(4) . . ? C75 C74 C73 120.4(4) . . ? C76 C75 C74 121.0(5) . . ? C75 C76 C77 119.2(5) . . ? C78 C77 C76 120.0(5) . . ? C77 C78 C73 121.2(5) . . ? O6 C79 C80 121.6(5) . . ? O6 C79 C84 118.1(4) . . ? C80 C79 C84 120.2(5) . . ? C79 C80 C81 117.8(6) . . ? C82 C81 C80 120.0(6) . . ? C83 C82 C81 121.3(6) . . ? C82 C83 C84 119.5(7) . . ? C83 C84 C79 121.2(6) . . ? O7 C85 C86 122.5(4) . . ? O7 C85 C90 119.0(4) . . ? C86 C85 C90 118.4(4) . . ? C85 C86 C87 120.9(5) . . ? C88 C87 C86 120.0(5) . . ? C89 C88 C87 119.8(5) . . ? C88 C89 C90 120.7(5) . . ? C89 C90 C85 120.1(5) . . ? O8 C91 C92 119.3(4) . . ? O8 C91 C96 122.8(4) . . ? C92 C91 C96 117.8(4) . . ? C93 C92 C91 121.0(5) . . ? C92 C93 C94 120.6(5) . . ? C95 C94 C93 118.9(5) . . ? C96 C95 C94 121.3(5) . . ? C95 C96 C91 120.4(5) . . ? C98 C97 C102 117.1(7) . . ? C98 C97 C103 121.9(8) . . ? C102 C97 C103 121.0(8) . . ? C99 C98 C97 121.2(8) . . ? C100 C99 C98 122.5(9) . . ? C99 C100 C101 118.3(9) . . ? C102 C101 C100 120.4(8) . . ? C101 C102 C97 120.6(7) . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 24.04 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 1.737 _refine_diff_density_min -1.926 _refine_diff_density_rms 0.158