# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1950 data_nx383 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35.50 H58 Li N8 S2 Sb3' _chemical_formula_weight 1033.21 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' 'Li' 'Li' -0.0003 0.0001 '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' 'S' 'S' 0.1246 0.1234 '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 11.177(3) _cell_length_b 13.746(3) _cell_length_c 15.173(4) _cell_angle_alpha 70.146(10) _cell_angle_beta 87.83(2) _cell_angle_gamma 89.668(19) _cell_volume 2191.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1030 _exptl_absorpt_coefficient_mu 1.965 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.6512 _exptl_absorpt_correction_T_max 0.855 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Bruker P4' _diffrn_measurement_method theta/2theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.9 _diffrn_reflns_number 7104 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0939 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 23.00 _reflns_number_total 6004 _reflns_number_gt 3617 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker XSCANS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material 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^)+(0.1013P)^2^+8.7059P] 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 6004 _refine_ls_number_parameters 432 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.1047 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.2050 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 3.266 _refine_ls_shift/su_mean 0.115 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 0.27748(7) 0.29483(6) -0.64240(5) 0.0371(2) Uani 1 1 d . . . Sb2 Sb 0.05506(7) 0.41578(6) -0.58501(5) 0.0391(2) Uani 1 1 d . . . Sb3 Sb 0.02306(7) 0.16917(6) -0.54359(6) 0.0416(2) Uani 1 1 d . . . Li Li 0.0703(19) 0.2991(18) -0.7681(14) 0.054(6) Uani 1 1 d . . . S1 S 0.3818(3) 0.3327(3) -0.8234(2) 0.0464(8) Uani 1 1 d D . . C1 C 0.2764(8) 0.3537(8) -0.9083(6) 0.039(3) Uani 1 1 d D . . N11 N 0.1593(7) 0.3475(7) -0.8946(6) 0.044(3) Uani 1 1 d D . . C17 C 0.1121(11) 0.3688(10) -0.9810(7) 0.053(4) Uani 1 1 d D . . H17 H 0.0302 0.3693 -0.9930 0.064 Uiso 1 1 calc R . . C18 C 0.2022(10) 0.3889(11) -1.0460(8) 0.065(4) Uani 1 1 d D . . H18 H 0.1944 0.4062 -1.1110 0.078 Uiso 1 1 calc R . . N12 N 0.3055(8) 0.3799(8) -1.0012(6) 0.057(3) Uani 1 1 d D . . C19 C 0.4259(12) 0.4022(15) -1.0462(11) 0.103(6) Uani 1 1 d D . . H19A H 0.4204 0.4187 -1.1134 0.155 Uiso 1 1 calc R . . H19B H 0.4762 0.3421 -1.0213 0.155 Uiso 1 1 calc R . . H19C H 0.4604 0.4606 -1.0337 0.155 Uiso 1 1 calc R . . N1 N 0.1582(7) 0.4134(6) -0.6993(6) 0.038(2) Uani 1 1 d D . . C11 C 0.1961(7) 0.5131(7) -0.7667(7) 0.037(3) Uani 1 1 d D . . H11 H 0.2376 0.4991 -0.8199 0.044 Uiso 1 1 calc R . . C12 C 0.0909(9) 0.5817(7) -0.8059(7) 0.043(3) Uani 1 1 d D . . H12A H 0.0368 0.5445 -0.8329 0.051 Uiso 1 1 calc R . . H12B H 0.0469 0.5956 -0.7544 0.051 Uiso 1 1 calc R . . C13 C 0.1267(12) 0.6850(7) -0.8812(8) 0.061(4) Uani 1 1 d D . . H13A H 0.0555 0.7269 -0.9033 0.073 Uiso 1 1 calc R . . H13B H 0.1675 0.6730 -0.9349 0.073 Uiso 1 1 calc R . . C14 C 0.2101(10) 0.7403(8) -0.8364(10) 0.069(5) Uani 1 1 d D . . H14A H 0.2348 0.8071 -0.8826 0.083 Uiso 1 1 calc R . . H14B H 0.1676 0.7536 -0.7840 0.083 Uiso 1 1 calc R . . C15 C 0.3200(10) 0.6753(8) -0.8011(9) 0.062(4) Uani 1 1 d D . . H15A H 0.3727 0.7123 -0.7728 0.075 Uiso 1 1 calc R . . H15B H 0.3643 0.6646 -0.8540 0.075 Uiso 1 1 calc R . . C16 C 0.2845(10) 0.5688(7) -0.7274(8) 0.056(4) Uani 1 1 d D . . H16A H 0.3563 0.5265 -0.7093 0.067 Uiso 1 1 calc R . . H16B H 0.2489 0.5791 -0.6712 0.067 Uiso 1 1 calc R . . N2 N -0.0634(7) 0.3099(6) -0.5904(7) 0.040(2) Uani 1 1 d D . . C21 C -0.1944(8) 0.3236(8) -0.5872(6) 0.041(3) Uani 1 1 d D . . H21 H -0.2316 0.2623 -0.5958 0.049 Uiso 1 1 calc R . . C22 C -0.2302(9) 0.4171(9) -0.6677(8) 0.054(4) Uani 1 1 d D . . H22A H -0.2021 0.4098 -0.7271 0.064 Uiso 1 1 calc R . . H22B H -0.1927 0.4792 -0.6627 0.064 Uiso 1 1 calc R . . C23 C -0.3677(9) 0.4291(11) -0.6670(8) 0.063(4) Uani 1 1 d D . . H23A H -0.4045 0.3706 -0.6792 0.076 Uiso 1 1 calc R . . H23B H -0.3892 0.4926 -0.7172 0.076 Uiso 1 1 calc R . . C24 C -0.4164(10) 0.4333(8) -0.5728(6) 0.049(3) Uani 1 1 d D . . H24A H -0.3883 0.4970 -0.5645 0.059 Uiso 1 1 calc R . . H24B H -0.5041 0.4348 -0.5725 0.059 Uiso 1 1 calc R . . C25 C -0.3759(8) 0.3405(9) -0.4921(8) 0.052(4) Uani 1 1 d D . . H25A H -0.4143 0.2780 -0.4955 0.062 Uiso 1 1 calc R . . H25B H -0.4024 0.3487 -0.4327 0.062 Uiso 1 1 calc R . . C26 C -0.2382(8) 0.3266(10) -0.4932(6) 0.049(3) Uani 1 1 d D . . H26A H -0.1996 0.3841 -0.4806 0.059 Uiso 1 1 calc R . . H26B H -0.2171 0.2621 -0.4439 0.059 Uiso 1 1 calc R . . S3 S -0.1217(3) 0.0893(2) -0.6365(2) 0.0492(9) Uani 1 1 d D . . C3 C -0.1642(9) 0.1896(8) -0.7346(8) 0.051(3) Uani 1 1 d D . . N31 N -0.0988(8) 0.2662(7) -0.7920(6) 0.044(3) Uani 1 1 d D . . C37 C -0.1737(9) 0.3257(9) -0.8574(8) 0.053(3) Uani 1 1 d D . . H37 H -0.1506 0.3856 -0.9075 0.063 Uiso 1 1 calc R . . C38 C -0.2860(10) 0.2861(9) -0.8399(8) 0.056(4) Uani 1 1 d D . . H38 H -0.3541 0.3124 -0.8745 0.067 Uiso 1 1 calc R . . N32 N -0.2803(8) 0.2005(8) -0.7622(7) 0.053(3) Uani 1 1 d D . . C39 C -0.3814(11) 0.1343(12) -0.7122(12) 0.088(6) Uani 1 1 d D . . H39A H -0.4545 0.1595 -0.7448 0.132 Uiso 1 1 calc R . . H39B H -0.3894 0.1359 -0.6489 0.132 Uiso 1 1 calc R . . H39C H -0.3672 0.0639 -0.7101 0.132 Uiso 1 1 calc R . . N3 N 0.1530(7) 0.1894(6) -0.6518(6) 0.034(2) Uani 1 1 d D . . C31 C 0.1901(9) 0.0870(7) -0.6542(7) 0.052(4) Uani 1 1 d D . . H31 H 0.1290 0.0370 -0.6160 0.062 Uiso 1 1 calc R . . C32 C 0.1896(14) 0.0795(7) -0.7502(8) 0.061(4) Uani 1 1 d D . . H32A H 0.2480 0.1287 -0.7913 0.074 Uiso 1 1 calc R . . H32B H 0.1103 0.0982 -0.7760 0.074 Uiso 1 1 calc R . . C33 C 0.2202(11) -0.0296(8) -0.7486(11) 0.081(5) Uani 1 1 d D . . H33A H 0.1577 -0.0780 -0.7124 0.097 Uiso 1 1 calc R . . H33B H 0.2226 -0.0311 -0.8128 0.097 Uiso 1 1 calc R . . C34 C 0.3403(12) -0.0636(11) -0.7053(8) 0.092(6) Uani 1 1 d D . . H34A H 0.4037 -0.0202 -0.7460 0.110 Uiso 1 1 calc R . . H34B H 0.3549 -0.1352 -0.7015 0.110 Uiso 1 1 calc R . . C35 C 0.3461(13) -0.0561(8) -0.6075(9) 0.079(5) Uani 1 1 d D . . H35A H 0.4281 -0.0694 -0.5859 0.095 Uiso 1 1 calc R . . H35B H 0.2935 -0.1087 -0.5637 0.095 Uiso 1 1 calc R . . C36 C 0.3072(10) 0.0525(8) -0.6085(9) 0.061(4) Uani 1 1 d D . . H36A H 0.3006 0.0521 -0.5438 0.074 Uiso 1 1 calc R . . H36B H 0.3695 0.1029 -0.6418 0.074 Uiso 1 1 calc R . . N4 N 0.1546(8) 0.2877(8) -0.5226(6) 0.046(3) Uani 1 1 d D A . C41 C 0.1939(9) 0.2535(12) -0.4258(7) 0.083(5) Uani 1 1 d D . . H41A H 0.2199 0.1809 -0.4109 0.099 Uiso 0.551(10) 1 calc PR A 1 H41B H 0.2318 0.3197 -0.4294 0.099 Uiso 0.449(10) 1 calc PR A 2 C42 C 0.0987(12) 0.2530(15) -0.3543(7) 0.103(7) Uani 1 1 d D A . H42A H 0.0263 0.2212 -0.3675 0.123 Uiso 0.551(10) 1 calc PR A 1 H42B H 0.0795 0.3247 -0.3608 0.123 Uiso 0.551(10) 1 calc PR A 1 H42C H 0.0529 0.1881 -0.3356 0.123 Uiso 0.449(10) 1 calc PR A 2 H42D H 0.0435 0.3105 -0.3801 0.123 Uiso 0.449(10) 1 calc PR A 2 C43 C 0.1314(17) 0.1952(14) -0.2525(11) 0.060(6) Uiso 0.551(10) 1 d PD A 1 H43A H 0.0629 0.1883 -0.2085 0.073 Uiso 0.551(10) 1 calc PR A 1 H43B H 0.1649 0.1269 -0.2445 0.073 Uiso 0.551(10) 1 calc PR A 1 C44 C 0.2249(14) 0.2698(17) -0.2429(16) 0.076(6) Uiso 0.551(10) 1 d PD A 1 H44A H 0.2500 0.2483 -0.1779 0.091 Uiso 0.551(10) 1 calc PR A 1 H44B H 0.1909 0.3393 -0.2590 0.091 Uiso 0.551(10) 1 calc PR A 1 C45 C 0.3322(17) 0.2717(19) -0.3078(10) 0.066(6) Uiso 0.551(10) 1 d PD A 1 H45A H 0.3947 0.3165 -0.2984 0.079 Uiso 0.551(10) 1 calc PR A 1 H45B H 0.3647 0.2018 -0.2923 0.079 Uiso 0.551(10) 1 calc PR A 1 C46 C 0.2978(17) 0.3115(16) -0.4113(12) 0.064(6) Uiso 0.551(10) 1 d PD A 1 H46A H 0.2783 0.3852 -0.4299 0.077 Uiso 0.551(10) 1 calc PR A 1 H46B H 0.3660 0.3039 -0.4509 0.077 Uiso 0.551(10) 1 calc PR A 1 C43X C 0.166(3) 0.265(2) -0.261(2) 0.060(6) Uiso 0.449(10) 1 d P A 2 H43C H 0.1076 0.2597 -0.2102 0.073 Uiso 0.449(10) 1 calc PR A 2 H43D H 0.2076 0.3321 -0.2786 0.073 Uiso 0.449(10) 1 calc PR A 2 C44X C 0.249(3) 0.183(3) -0.234(2) 0.076(6) Uiso 0.449(10) 1 d P A 2 H44C H 0.2872 0.1838 -0.1773 0.091 Uiso 0.449(10) 1 calc PR A 2 H44D H 0.2051 0.1174 -0.2183 0.091 Uiso 0.449(10) 1 calc PR A 2 C45X C 0.346(3) 0.186(2) -0.308(2) 0.066(6) Uiso 0.449(10) 1 d P A 2 H45C H 0.3949 0.1237 -0.2861 0.079 Uiso 0.449(10) 1 calc PR A 2 H45D H 0.3991 0.2461 -0.3173 0.079 Uiso 0.449(10) 1 calc PR A 2 C46X C 0.293(3) 0.194(2) -0.401(2) 0.064(6) Uiso 0.449(10) 1 d P A 2 H46C H 0.3548 0.2215 -0.4507 0.077 Uiso 0.449(10) 1 calc PR A 2 H46D H 0.2729 0.1242 -0.3989 0.077 Uiso 0.449(10) 1 calc PR A 2 C1T C -0.052(4) 0.965(3) -1.007(3) 0.135(15) Uiso 0.50 1 d P . . C6T C -0.164(5) 0.941(3) -0.992(3) 0.142(16) Uiso 0.50 1 d P . . C5T C -0.238(6) 1.007(4) -0.943(4) 0.21(2) Uiso 0.50 1 d P . . C4T C -0.140(5) 1.040(4) -0.943(3) 0.135(16) Uiso 0.50 1 d P . . C3T C -0.109(5) 1.091(4) -0.900(4) 0.146(17) Uiso 0.50 1 d P . . C7T C 0.022(3) 0.929(2) -1.052(2) 0.223(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sb1 0.0247(4) 0.0492(4) 0.0372(4) -0.0144(3) -0.0014(3) 0.0056(3) Sb2 0.0326(4) 0.0491(4) 0.0381(4) -0.0185(3) 0.0031(3) 0.0048(4) Sb3 0.0302(4) 0.0437(4) 0.0407(4) -0.0019(3) 0.0065(4) 0.0087(3) Li 0.044(12) 0.082(14) 0.035(11) -0.021(10) 0.001(9) -0.002(11) S1 0.0269(15) 0.071(2) 0.0416(16) -0.0194(15) 0.0047(13) 0.0039(14) C1 0.032(6) 0.043(6) 0.041(6) -0.014(5) 0.004(5) 0.008(5) N11 0.030(5) 0.063(6) 0.044(5) -0.025(5) -0.010(4) 0.013(5) C17 0.049(8) 0.079(9) 0.024(6) -0.008(6) 0.003(6) 0.003(7) C18 0.062(9) 0.099(10) 0.032(7) -0.022(7) -0.007(7) 0.016(8) N12 0.049(7) 0.069(7) 0.046(6) -0.011(5) 0.007(5) -0.001(6) C19 0.070(11) 0.165(16) 0.073(10) -0.043(11) 0.039(9) 0.002(11) N1 0.019(5) 0.045(5) 0.043(5) -0.008(4) 0.003(4) 0.007(4) C11 0.031(6) 0.046(6) 0.036(6) -0.016(5) -0.003(5) 0.002(5) C12 0.034(6) 0.043(6) 0.045(7) -0.008(5) 0.003(6) -0.004(5) C13 0.078(10) 0.040(7) 0.058(8) -0.010(6) 0.002(8) 0.009(7) C14 0.082(11) 0.034(7) 0.079(10) -0.003(7) -0.009(9) 0.011(7) C15 0.061(9) 0.065(8) 0.062(8) -0.024(7) 0.000(7) -0.021(7) C16 0.034(7) 0.044(6) 0.106(10) -0.049(6) 0.022(7) -0.009(6) N2 0.025(5) 0.037(5) 0.054(6) -0.012(4) -0.001(4) 0.012(4) C21 0.027(6) 0.049(6) 0.051(7) -0.021(5) 0.000(5) 0.004(5) C22 0.045(7) 0.072(8) 0.040(7) -0.015(6) -0.001(6) 0.015(7) C23 0.045(8) 0.076(9) 0.070(9) -0.027(7) -0.002(7) 0.020(7) C24 0.037(7) 0.053(7) 0.057(8) -0.020(6) -0.002(6) 0.023(6) C25 0.029(6) 0.068(8) 0.057(8) -0.021(6) 0.006(6) 0.003(6) C26 0.039(7) 0.083(8) 0.018(5) -0.009(5) 0.009(5) -0.032(6) S3 0.0326(16) 0.0462(17) 0.063(2) -0.0115(15) 0.0011(15) -0.0013(14) C3 0.037(7) 0.050(7) 0.065(8) -0.019(6) -0.002(6) 0.003(6) N31 0.038(6) 0.050(6) 0.041(5) -0.010(5) 0.001(5) -0.002(5) C37 0.039(7) 0.067(8) 0.060(8) -0.031(6) -0.011(6) 0.005(6) C38 0.030(7) 0.080(9) 0.054(8) -0.018(7) -0.018(6) 0.018(7) N32 0.024(5) 0.065(7) 0.060(7) -0.006(6) 0.001(5) 0.005(5) C39 0.032(8) 0.106(12) 0.103(13) -0.005(10) 0.002(8) -0.031(8) N3 0.023(5) 0.044(5) 0.032(5) -0.011(4) -0.003(4) 0.008(4) C31 0.035(7) 0.041(7) 0.073(9) -0.012(6) -0.001(6) 0.013(6) C32 0.077(10) 0.044(7) 0.069(9) -0.026(6) -0.006(8) 0.005(7) C33 0.083(11) 0.072(9) 0.094(11) -0.038(8) 0.020(9) 0.007(9) C34 0.098(12) 0.066(9) 0.121(12) -0.052(8) 0.056(10) 0.001(9) C35 0.052(9) 0.050(8) 0.119(14) -0.008(8) 0.002(9) 0.025(7) C36 0.084(10) 0.040(7) 0.053(8) -0.006(6) -0.006(8) 0.022(7) N4 0.023(5) 0.068(6) 0.040(5) -0.012(5) 0.004(4) 0.019(5) C41 0.042(8) 0.161(14) 0.050(8) -0.041(9) -0.009(7) 0.041(9) C42 0.072(11) 0.186(18) 0.027(7) -0.007(9) -0.002(8) 0.053(12) _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 N3 2.058(8) . ? Sb1 N1 2.069(8) . ? Sb1 N4 2.212(9) . ? Sb1 S1 2.823(3) . ? Sb2 N2 1.997(9) . ? Sb2 N4 2.039(9) . ? Sb2 N1 2.055(9) . ? Sb3 N2 2.068(8) . ? Sb3 N3 2.098(8) . ? Sb3 N4 2.309(10) . ? Sb3 S3 2.656(4) . ? Li N31 2.02(2) . ? Li N11 2.03(2) . ? Li N3 2.13(2) . ? Li N1 2.40(2) . ? S1 C1 1.728(10) . ? C1 N11 1.317(11) . ? C1 N12 1.359(12) . ? N11 C17 1.368(12) . ? C17 C18 1.343(14) . ? C18 N12 1.346(13) . ? N12 C19 1.471(14) . ? N1 C11 1.459(10) . ? C11 C12 1.510(10) . ? C11 C16 1.510(11) . ? C12 C13 1.534(11) . ? C13 C14 1.523(12) . ? C14 C15 1.519(12) . ? C15 C16 1.553(11) . ? N2 C21 1.476(10) . ? C21 C22 1.507(11) . ? C21 C26 1.505(11) . ? C22 C23 1.544(11) . ? C23 C24 1.530(12) . ? C24 C25 1.518(11) . ? C25 C26 1.550(11) . ? S3 C3 1.730(10) . ? C3 N31 1.318(12) . ? C3 N32 1.370(12) . ? N31 C37 1.364(12) . ? C37 C38 1.351(14) . ? C38 N32 1.356(13) . ? N32 C39 1.470(13) . ? N3 C31 1.477(11) . ? C31 C32 1.495(11) . ? C31 C36 1.501(11) . ? C32 C33 1.529(12) . ? C33 C34 1.517(13) . ? C34 C35 1.526(13) . ? C35 C36 1.548(12) . ? N4 C41 1.466(11) . ? C41 C46 1.477(14) . ? C41 C46X 1.36(3) . ? C41 C42 1.488(12) . ? C42 C43 1.536(13) . ? C42 C43X 1.68(4) . ? C43 C44 1.513(15) . ? C44 C45 1.518(15) . ? C45 C46 1.541(14) . ? C43X C44X 1.42(4) . ? C44X C45X 1.52(4) . ? C45X C46X 1.52(4) . ? C1T C7T 1.26(5) . ? C1T C1T 1.57(9) 2_573 ? C1T C6T 1.29(6) . ? C1T C4T 2.26(7) 2_573 ? C1T C3T 2.52(7) 2_573 ? C6T C5T 1.58(7) . ? C6T C4T 1.78(7) . ? C5T C4T 1.18(7) . ? C5T C3T 2.09(8) . ? C5T C7T 2.56(7) 2_573 ? C4T C3T 1.17(6) . ? C4T C7T 1.38(6) 2_573 ? C4T C1T 2.26(7) 2_573 ? C3T C7T 1.27(6) 2_573 ? C3T C1T 2.52(7) 2_573 ? C7T C3T 1.27(6) 2_573 ? C7T C4T 1.38(6) 2_573 ? C7T C5T 2.56(7) 2_573 ? 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 N3 Sb1 N1 89.8(3) . . ? N3 Sb1 N4 79.5(4) . . ? N1 Sb1 N4 76.4(3) . . ? N3 Sb1 S1 95.2(2) . . ? N1 Sb1 S1 89.0(2) . . ? N4 Sb1 S1 164.4(2) . . ? N2 Sb2 N4 82.3(4) . . ? N2 Sb2 N1 95.7(4) . . ? N4 Sb2 N1 80.6(3) . . ? N2 Sb3 N3 100.8(3) . . ? N2 Sb3 N4 74.5(3) . . ? N3 Sb3 N4 76.5(3) . . ? N2 Sb3 S3 91.5(3) . . ? N3 Sb3 S3 88.5(2) . . ? N4 Sb3 S3 156.8(2) . . ? N31 Li N11 106.4(10) . . ? N31 Li N3 116.4(10) . . ? N11 Li N3 119.0(11) . . ? N31 Li N1 134.8(11) . . ? N11 Li N1 99.3(9) . . ? N3 Li N1 79.9(8) . . ? C1 S1 Sb1 112.7(3) . . ? N11 C1 N12 110.0(9) . . ? N11 C1 S1 126.8(7) . . ? N12 C1 S1 123.2(7) . . ? C1 N11 C17 106.5(9) . . ? C1 N11 Li 125.7(9) . . ? C17 N11 Li 127.5(9) . . ? C18 C17 N11 108.8(10) . . ? C17 C18 N12 107.6(10) . . ? C18 N12 C1 107.1(9) . . ? C18 N12 C19 125.8(11) . . ? C1 N12 C19 127.0(11) . . ? C11 N1 Sb2 116.9(7) . . ? C11 N1 Sb1 122.4(6) . . ? Sb2 N1 Sb1 103.4(4) . . ? C11 N1 Li 114.2(8) . . ? Sb2 N1 Li 109.9(6) . . ? Sb1 N1 Li 85.6(6) . . ? N1 C11 C12 112.1(7) . . ? N1 C11 C16 112.7(8) . . ? C12 C11 C16 110.7(8) . . ? C13 C12 C11 113.7(8) . . ? C12 C13 C14 107.1(9) . . ? C15 C14 C13 110.6(10) . . ? C14 C15 C16 111.1(9) . . ? C11 C16 C15 110.7(9) . . ? C21 N2 Sb2 123.9(7) . . ? C21 N2 Sb3 125.0(6) . . ? Sb2 N2 Sb3 106.2(4) . . ? N2 C21 C22 110.2(7) . . ? N2 C21 C26 111.2(8) . . ? C22 C21 C26 113.1(9) . . ? C21 C22 C23 110.3(9) . . ? C22 C23 C24 111.3(9) . . ? C25 C24 C23 111.1(9) . . ? C24 C25 C26 112.7(9) . . ? C21 C26 C25 109.9(8) . . ? C3 S3 Sb3 107.1(4) . . ? N31 C3 N32 109.3(9) . . ? N31 C3 S3 129.1(8) . . ? N32 C3 S3 121.6(8) . . ? C3 N31 C37 106.6(9) . . ? C3 N31 Li 124.3(9) . . ? C37 N31 Li 128.1(9) . . ? C38 C37 N31 110.1(10) . . ? C37 C38 N32 105.9(10) . . ? C3 N32 C38 108.0(9) . . ? C3 N32 C39 125.5(10) . . ? C38 N32 C39 126.4(10) . . ? C31 N3 Sb1 120.9(6) . . ? C31 N3 Sb3 109.1(6) . . ? Sb1 N3 Sb3 107.9(4) . . ? C31 N3 Li 121.3(9) . . ? Sb1 N3 Li 93.2(7) . . ? Sb3 N3 Li 102.1(7) . . ? N3 C31 C32 113.2(8) . . ? N3 C31 C36 112.7(8) . . ? C32 C31 C36 111.8(10) . . ? C31 C32 C33 111.5(9) . . ? C34 C33 C32 111.1(11) . . ? C33 C34 C35 112.3(11) . . ? C34 C35 C36 110.6(10) . . ? C31 C36 C35 113.6(10) . . ? C41 N4 Sb2 125.7(8) . . ? C41 N4 Sb1 122.3(6) . . ? Sb2 N4 Sb1 99.1(3) . . ? C41 N4 Sb3 110.7(8) . . ? Sb2 N4 Sb3 96.5(4) . . ? Sb1 N4 Sb3 96.0(4) . . ? C46 C41 C46X 67.0(17) . . ? C46 C41 N4 114.2(11) . . ? C46X C41 N4 120.7(17) . . ? C46 C41 C42 107.9(14) . . ? C46X C41 C42 120.6(16) . . ? N4 C41 C42 114.8(9) . . ? C41 C42 C43 114.7(12) . . ? C41 C42 C43X 107.6(15) . . ? C43 C42 C43X 36.0(12) . . ? C44 C43 C42 98.7(15) . . ? C43 C44 C45 109.6(18) . . ? C46 C45 C44 111.3(17) . . ? C41 C46 C45 110.9(15) . . ? C42 C43X C44X 105(3) . . ? C45X C44X C43X 115(3) . . ? C44X C45X C46X 111(3) . . ? C41 C46X C45X 117(3) . . ? C7T C1T C1T 88(5) . 2_573 ? C7T C1T C6T 125(5) . . ? C1T C1T C6T 146(6) 2_573 . ? C7T C1T C4T 33(3) . 2_573 ? C1T C1T C4T 55(3) 2_573 2_573 ? C6T C1T C4T 158(4) . 2_573 ? C7T C1T C3T 6(2) . 2_573 ? C1T C1T C3T 83(4) 2_573 2_573 ? C6T C1T C3T 131(4) . 2_573 ? C4T C1T C3T 27.6(17) 2_573 2_573 ? C5T C6T C1T 114(5) . . ? C5T C6T C4T 40(3) . . ? C1T C6T C4T 74(4) . . ? C4T C5T C6T 79(5) . . ? C4T C5T C3T 27(4) . . ? C6T C5T C3T 105(4) . . ? C4T C5T C7T 3(4) . 2_573 ? C6T C5T C7T 76(3) . 2_573 ? C3T C5T C7T 29.6(18) . 2_573 ? C3T C4T C7T 59(4) . 2_573 ? C3T C4T C5T 126(7) . . ? C7T C4T C5T 175(7) 2_573 . ? C3T C4T C1T 89(4) . 2_573 ? C7T C4T C1T 30(2) 2_573 2_573 ? C5T C4T C1T 145(6) . 2_573 ? C3T C4T C6T 167(5) . . ? C7T C4T C6T 114(4) 2_573 . ? C5T C4T C6T 61(4) . . ? C1T C4T C6T 84(3) 2_573 . ? C4T C3T C7T 69(4) . 2_573 ? C4T C3T C5T 27(4) . . ? C7T C3T C5T 96(4) 2_573 . ? C4T C3T C1T 64(4) . 2_573 ? C7T C3T C1T 6(2) 2_573 2_573 ? C5T C3T C1T 91(3) . 2_573 ? C3T C7T C4T 52(3) 2_573 2_573 ? C3T C7T C1T 168(5) 2_573 . ? C4T C7T C1T 117(4) 2_573 . ? C3T C7T C5T 55(3) 2_573 2_573 ? C4T C7T C5T 3(3) 2_573 2_573 ? C1T C7T C5T 115(3) . 2_573 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 23.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.341 _refine_diff_density_min -0.779 _refine_diff_density_rms 0.188 data_dw0002 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47.50 H66 N8 O4 Sb4' _chemical_formula_weight 1300.08 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 12.793(3) _cell_length_b 14.864(3) _cell_length_c 15.340(3) _cell_angle_alpha 65.45(3) _cell_angle_beta 74.73(3) _cell_angle_gamma 80.35(3) _cell_volume 2554.0(9) _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 0.70 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1286 _exptl_absorpt_coefficient_mu 2.142 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.3155 _exptl_absorpt_correction_T_max 0.8306 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 ? _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 20787 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_av_sigmaI/netI 0.1077 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8998 _reflns_number_gt 6142 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.0605P)^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 8998 _refine_ls_number_parameters 557 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.0961 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.100 _refine_ls_shift/su_mean 0.003 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 -0.84848(4) 0.65723(3) 0.28584(4) 0.02481(15) Uani 1 1 d . . . Sb2 Sb -0.89749(4) 0.51063(3) 0.18792(4) 0.02412(15) Uani 1 1 d . . . Sb3 Sb -0.74450(4) 0.72607(4) 0.04603(4) 0.02602(15) Uani 1 1 d . . . Sb4 Sb -1.01625(4) 0.73845(3) 0.10755(4) 0.02469(15) Uani 1 1 d . . . O1 O -0.6890(4) 0.6816(4) 0.2780(4) 0.0319(13) Uani 1 1 d . . . O2 O -0.9276(4) 0.4207(4) 0.3386(4) 0.0326(13) Uani 1 1 d . . . O3 O -0.7852(4) 0.8635(4) -0.0575(4) 0.0349(14) Uani 1 1 d . . . O4 O -1.1029(4) 0.6597(4) 0.0688(4) 0.0341(13) Uani 1 1 d . . . N1 N -0.7626(6) 0.7627(5) 0.3806(5) 0.0352(17) Uani 1 1 d . . . N2 N -0.8377(6) 0.2935(5) 0.2975(5) 0.0366(17) Uani 1 1 d . . . N3 N -0.6049(7) 0.8756(6) -0.1241(7) 0.074(3) Uani 1 1 d . . . N4 N -1.2648(6) 0.7329(5) 0.1198(5) 0.0415(18) Uani 1 1 d . . . N5 N -0.8518(5) 0.7725(4) 0.1501(4) 0.0256(15) Uani 1 1 d . . . N6 N -0.8820(5) 0.6730(4) 0.0401(4) 0.0228(14) Uani 1 1 d . . . N7 N -0.9964(5) 0.6162(4) 0.2345(4) 0.0234(14) Uani 1 1 d . . . N8 N -0.7732(5) 0.5748(4) 0.2011(4) 0.0262(15) Uani 1 1 d . . . C11 C -0.6759(7) 0.7166(5) 0.3424(6) 0.032(2) Uani 1 1 d . . . C12 C -0.5761(7) 0.7050(6) 0.3651(6) 0.039(2) Uani 1 1 d . . . H12A H -0.5165 0.6714 0.3364 0.047 Uiso 1 1 calc R . . C13 C -0.5636(7) 0.7424(6) 0.4293(6) 0.042(2) Uani 1 1 d . . . H13A H -0.4951 0.7356 0.4453 0.050 Uiso 1 1 calc R . . C14 C -0.6516(8) 0.7899(7) 0.4706(7) 0.047(2) Uani 1 1 d . . . H14A H -0.6454 0.8170 0.5151 0.057 Uiso 1 1 calc R . . C15 C -0.7481(8) 0.7968(6) 0.4453(7) 0.048(2) Uani 1 1 d . . . H15A H -0.8094 0.8277 0.4753 0.057 Uiso 1 1 calc R . . C41 C -1.2055(7) 0.6893(5) 0.0606(6) 0.033(2) Uani 1 1 d . . . C42 C -1.2441(8) 0.6746(6) -0.0090(7) 0.051(3) Uani 1 1 d . . . H42A H -1.1983 0.6454 -0.0513 0.061 Uiso 1 1 calc R . . C43 C -1.3516(10) 0.7041(7) -0.0144(10) 0.075(4) Uani 1 1 d . . . H43A H -1.3815 0.6950 -0.0604 0.090 Uiso 1 1 calc R . . C44 C -1.4143(9) 0.7468(8) 0.0480(11) 0.078(4) Uani 1 1 d . . . H44A H -1.4885 0.7667 0.0462 0.094 Uiso 1 1 calc R . . C45 C -1.3694(8) 0.7603(7) 0.1119(8) 0.058(3) Uani 1 1 d . . . H45A H -1.4138 0.7907 0.1537 0.070 Uiso 1 1 calc R . . C21 C -0.9069(7) 0.3237(6) 0.3625(6) 0.032(2) Uani 1 1 d . . . C22 C -0.9587(7) 0.2585(6) 0.4534(7) 0.045(2) Uani 1 1 d . . . H22A H -1.0084 0.2818 0.4988 0.055 Uiso 1 1 calc R . . C23 C -0.9348(10) 0.1579(7) 0.4752(8) 0.072(3) Uani 1 1 d . . . H23A H -0.9681 0.1112 0.5370 0.086 Uiso 1 1 calc R . . C24 C -0.8655(10) 0.1260(7) 0.4105(9) 0.067(3) Uani 1 1 d . . . H24A H -0.8499 0.0572 0.4250 0.081 Uiso 1 1 calc R . . C25 C -0.8180(8) 0.1947(6) 0.3234(8) 0.051(3) Uani 1 1 d . . . H25A H -0.7678 0.1718 0.2780 0.061 Uiso 1 1 calc R . . C51 C -0.8601(7) 0.8789(5) 0.1370(6) 0.035(2) Uani 1 1 d . . . H51A H -0.8865 0.9189 0.0752 0.042 Uiso 1 1 calc R . . C52 C -0.9433(7) 0.8970(6) 0.2195(7) 0.040(2) Uani 1 1 d . . . H52A H -0.9198 0.8582 0.2821 0.048 Uiso 1 1 calc R . . H52B H -1.0136 0.8734 0.2249 0.048 Uiso 1 1 calc R . . C53 C -0.9591(9) 1.0056(6) 0.2036(8) 0.057(3) Uani 1 1 d . . . H53A H -1.0117 1.0138 0.2605 0.068 Uiso 1 1 calc R . . H53B H -0.9890 1.0440 0.1443 0.068 Uiso 1 1 calc R . . C54 C -0.8510(9) 1.0451(6) 0.1913(8) 0.059(3) Uani 1 1 d . . . H54A H -0.8243 1.0109 0.2529 0.070 Uiso 1 1 calc R . . H54B H -0.8614 1.1169 0.1774 0.070 Uiso 1 1 calc R . . C55 C -0.7668(9) 1.0277(6) 0.1066(7) 0.053(3) Uani 1 1 d . . . H55A H -0.7911 1.0660 0.0442 0.064 Uiso 1 1 calc R . . H55B H -0.6964 1.0515 0.1006 0.064 Uiso 1 1 calc R . . C56 C -0.7522(7) 0.9168(5) 0.1249(6) 0.035(2) Uani 1 1 d . . . H56A H -0.6994 0.9070 0.0689 0.043 Uiso 1 1 calc R . . H56B H -0.7232 0.8790 0.1849 0.043 Uiso 1 1 calc R . . C61 C -0.8854(6) 0.6571(5) -0.0494(6) 0.0265(18) Uani 1 1 d . . . H61A H -0.9408 0.6079 -0.0289 0.032 Uiso 1 1 calc R . . C62 C -0.9201(7) 0.7508(5) -0.1302(6) 0.0293(19) Uani 1 1 d . . . H62A H -0.9931 0.7760 -0.1046 0.035 Uiso 1 1 calc R . . H62B H -0.8688 0.8023 -0.1497 0.035 Uiso 1 1 calc R . . C63 C -0.9229(7) 0.7325(6) -0.2201(6) 0.036(2) Uani 1 1 d . . . H63A H -0.9790 0.6857 -0.2022 0.043 Uiso 1 1 calc R . . H63B H -0.9428 0.7957 -0.2716 0.043 Uiso 1 1 calc R . . C64 C -0.8146(7) 0.6906(6) -0.2595(6) 0.038(2) Uani 1 1 d . . . H64A H -0.7595 0.7396 -0.2823 0.045 Uiso 1 1 calc R . . H64B H -0.8193 0.6771 -0.3163 0.045 Uiso 1 1 calc R . . C65 C -0.7796(7) 0.5938(6) -0.1796(6) 0.036(2) Uani 1 1 d . . . H65A H -0.7063 0.5692 -0.2053 0.043 Uiso 1 1 calc R . . H65B H -0.8307 0.5425 -0.1613 0.043 Uiso 1 1 calc R . . C66 C -0.7785(6) 0.6127(6) -0.0882(6) 0.0294(19) Uani 1 1 d . . . H66A H -0.7605 0.5493 -0.0361 0.035 Uiso 1 1 calc R . . H66B H -0.7211 0.6581 -0.1054 0.035 Uiso 1 1 calc R . . C71 C -1.0870(6) 0.5858(5) 0.3226(5) 0.0242(18) Uani 1 1 d . . . H71A H -1.0538 0.5455 0.3806 0.029 Uiso 1 1 calc R . . C72 C -1.1662(7) 0.5218(6) 0.3194(6) 0.035(2) Uani 1 1 d . . . H72A H -1.2003 0.5594 0.2624 0.042 Uiso 1 1 calc R . . H72B H -1.1262 0.4619 0.3109 0.042 Uiso 1 1 calc R . . C73 C -1.2539(7) 0.4909(6) 0.4129(7) 0.042(2) Uani 1 1 d . . . H73A H -1.3055 0.4512 0.4082 0.051 Uiso 1 1 calc R . . H73B H -1.2206 0.4493 0.4695 0.051 Uiso 1 1 calc R . . C74 C -1.3140(7) 0.5816(6) 0.4283(6) 0.042(2) Uani 1 1 d . . . H74A H -1.3697 0.5604 0.4902 0.051 Uiso 1 1 calc R . . H74B H -1.3518 0.6202 0.3739 0.051 Uiso 1 1 calc R . . C75 C -1.2380(7) 0.6474(6) 0.4327(6) 0.040(2) Uani 1 1 d . . . H75A H -1.2055 0.6115 0.4909 0.048 Uiso 1 1 calc R . . H75B H -1.2794 0.7078 0.4390 0.048 Uiso 1 1 calc R . . C76 C -1.1482(6) 0.6766(5) 0.3396(5) 0.0284(19) Uani 1 1 d . . . H76A H -1.1806 0.7190 0.2825 0.034 Uiso 1 1 calc R . . H76B H -1.0965 0.7157 0.3450 0.034 Uiso 1 1 calc R . . C81 C -0.6636(6) 0.5211(5) 0.2097(5) 0.0255(18) Uani 1 1 d . . . H81A H -0.6104 0.5720 0.1900 0.031 Uiso 1 1 calc R . . C82 C -0.6293(6) 0.4703(5) 0.1377(6) 0.0262(18) Uani 1 1 d . . . H82A H -0.6292 0.5201 0.0704 0.031 Uiso 1 1 calc R . . H82B H -0.6822 0.4213 0.1535 0.031 Uiso 1 1 calc R . . C83 C -0.5167(7) 0.4182(6) 0.1420(6) 0.036(2) Uani 1 1 d . . . H83A H -0.4979 0.3829 0.0971 0.043 Uiso 1 1 calc R . . H83B H -0.4627 0.4682 0.1196 0.043 Uiso 1 1 calc R . . C84 C -0.5113(7) 0.3449(6) 0.2453(6) 0.041(2) Uani 1 1 d . . . H84A H -0.5600 0.2912 0.2654 0.049 Uiso 1 1 calc R . . H84B H -0.4363 0.3147 0.2466 0.049 Uiso 1 1 calc R . . C85 C -0.5450(7) 0.3962(6) 0.3164(6) 0.039(2) Uani 1 1 d . . . H85A H -0.4922 0.4456 0.2997 0.047 Uiso 1 1 calc R . . H85B H -0.5442 0.3468 0.3838 0.047 Uiso 1 1 calc R . . C86 C -0.6582(6) 0.4479(6) 0.3132(6) 0.0303(19) Uani 1 1 d . . . H86A H -0.7121 0.3979 0.3359 0.036 Uiso 1 1 calc R . . H86B H -0.6767 0.4834 0.3580 0.036 Uiso 1 1 calc R . . C31 C -0.7032(8) 0.9192(6) -0.1188(7) 0.042(2) Uani 1 1 d . . . C32 C -0.7229(9) 1.0195(7) -0.1705(8) 0.065(3) Uani 1 1 d . . . H32A H -0.7946 1.0496 -0.1639 0.078 Uiso 1 1 calc R . . C33 C -0.6376(11) 1.0743(8) -0.2309(9) 0.086(4) Uani 1 1 d . . . H33A H -0.6502 1.1426 -0.2692 0.103 Uiso 1 1 calc R . . C34 C -0.5349(11) 1.0323(8) -0.2368(9) 0.094(5) Uani 1 1 d . . . H34A H -0.4743 1.0700 -0.2772 0.113 Uiso 1 1 calc R . . C35 C -0.5226(10) 0.9343(10) -0.1824(10) 0.113(6) Uani 1 1 d . . . H35A H -0.4508 0.9043 -0.1854 0.135 Uiso 1 1 calc R . . C1 C -0.5255(19) 0.9267(13) 0.5804(14) 0.139(6) Uiso 1 1 d . . . C2 C -0.4297(16) 0.9189(12) 0.5342(14) 0.127(6) Uiso 1 1 d . . . C3 C -0.3831(18) 0.9996(15) 0.4414(16) 0.147(7) Uiso 1 1 d . . . C4 C -0.288(3) 1.000(2) 0.394(2) 0.101(9) Uiso 0.50 1 d P . . 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 0.0225(3) 0.0292(3) 0.0250(3) -0.0129(2) -0.0060(2) -0.0002(2) Sb2 0.0219(3) 0.0254(3) 0.0265(3) -0.0120(2) -0.0050(2) -0.0004(2) Sb3 0.0202(3) 0.0314(3) 0.0263(3) -0.0105(2) -0.0047(2) -0.0037(2) Sb4 0.0209(3) 0.0260(3) 0.0271(3) -0.0106(2) -0.0064(2) 0.0015(2) O1 0.026(3) 0.048(3) 0.032(3) -0.022(3) -0.010(3) -0.005(2) O2 0.038(4) 0.029(3) 0.026(3) -0.008(2) -0.002(3) -0.001(2) O3 0.031(4) 0.036(3) 0.034(3) -0.006(3) -0.010(3) -0.008(3) O4 0.022(3) 0.042(3) 0.047(4) -0.023(3) -0.014(3) 0.004(2) N1 0.029(4) 0.043(4) 0.038(4) -0.022(4) -0.007(3) 0.001(3) N2 0.035(5) 0.037(4) 0.040(5) -0.017(3) -0.011(4) 0.003(3) N3 0.044(6) 0.054(5) 0.073(7) 0.015(5) 0.007(5) -0.008(4) N4 0.025(5) 0.056(5) 0.038(5) -0.017(4) -0.005(4) 0.006(3) N5 0.030(4) 0.023(3) 0.024(4) -0.008(3) -0.011(3) 0.002(3) N6 0.021(4) 0.027(3) 0.023(4) -0.010(3) -0.007(3) 0.000(3) N7 0.019(4) 0.026(3) 0.024(4) -0.010(3) -0.003(3) 0.000(3) N8 0.024(4) 0.029(3) 0.026(4) -0.011(3) -0.009(3) 0.004(3) C11 0.035(6) 0.026(4) 0.039(5) -0.008(4) -0.017(4) -0.009(4) C12 0.028(5) 0.048(5) 0.038(6) -0.011(4) -0.010(4) -0.007(4) C13 0.032(6) 0.062(6) 0.039(6) -0.017(5) -0.018(5) -0.012(5) C14 0.052(7) 0.058(6) 0.044(6) -0.027(5) -0.010(5) -0.019(5) C15 0.048(7) 0.051(6) 0.047(6) -0.027(5) -0.006(5) 0.001(5) C41 0.034(6) 0.027(4) 0.035(5) -0.008(4) -0.007(4) -0.006(4) C42 0.058(7) 0.051(6) 0.055(7) -0.023(5) -0.029(6) -0.005(5) C43 0.065(9) 0.055(7) 0.131(12) -0.037(7) -0.067(9) 0.006(6) C44 0.028(7) 0.077(8) 0.134(12) -0.034(8) -0.040(8) -0.001(6) C45 0.028(6) 0.066(7) 0.058(7) -0.019(6) 0.012(5) 0.006(5) C21 0.029(5) 0.032(5) 0.034(5) -0.007(4) -0.013(4) 0.000(4) C22 0.042(6) 0.035(5) 0.047(6) -0.007(4) -0.005(5) -0.003(4) C23 0.085(10) 0.043(6) 0.057(8) 0.010(5) -0.012(7) -0.011(6) C24 0.086(9) 0.034(6) 0.083(9) -0.021(6) -0.035(8) 0.013(6) C25 0.050(7) 0.034(5) 0.071(8) -0.026(5) -0.014(6) 0.007(4) C51 0.041(6) 0.021(4) 0.042(6) -0.008(4) -0.017(4) -0.002(4) C52 0.042(6) 0.034(5) 0.044(6) -0.018(4) -0.009(5) 0.005(4) C53 0.083(9) 0.028(5) 0.064(7) -0.023(5) -0.029(6) 0.015(5) C54 0.082(9) 0.031(5) 0.076(8) -0.027(5) -0.032(7) 0.002(5) C55 0.076(8) 0.028(5) 0.060(7) -0.004(4) -0.035(6) -0.017(5) C56 0.040(6) 0.028(4) 0.040(5) -0.013(4) -0.010(4) -0.008(4) C61 0.027(5) 0.029(4) 0.026(5) -0.013(3) -0.005(4) -0.004(3) C62 0.028(5) 0.031(4) 0.030(5) -0.011(4) -0.010(4) -0.002(3) C63 0.041(6) 0.035(5) 0.030(5) -0.007(4) -0.017(4) -0.002(4) C64 0.046(6) 0.042(5) 0.030(5) -0.014(4) -0.008(4) -0.012(4) C65 0.043(6) 0.042(5) 0.031(5) -0.022(4) -0.006(4) -0.006(4) C66 0.033(5) 0.035(4) 0.029(5) -0.019(4) -0.013(4) 0.005(4) C71 0.027(5) 0.027(4) 0.018(4) -0.010(3) -0.003(4) -0.001(3) C72 0.038(6) 0.035(5) 0.033(5) -0.013(4) -0.007(4) -0.010(4) C73 0.031(5) 0.048(5) 0.043(6) -0.011(4) -0.003(4) -0.015(4) C74 0.023(5) 0.073(6) 0.026(5) -0.018(5) 0.000(4) -0.001(4) C75 0.035(6) 0.048(5) 0.034(5) -0.021(4) -0.001(4) 0.004(4) C76 0.031(5) 0.036(4) 0.018(4) -0.014(4) 0.002(4) -0.004(4) C81 0.019(4) 0.036(4) 0.023(5) -0.012(4) -0.006(4) 0.000(3) C82 0.016(4) 0.040(4) 0.024(5) -0.015(4) -0.005(4) 0.000(3) C83 0.025(5) 0.044(5) 0.039(6) -0.021(4) -0.005(4) 0.005(4) C84 0.026(5) 0.042(5) 0.044(6) -0.010(4) -0.010(4) 0.013(4) C85 0.032(5) 0.046(5) 0.038(6) -0.013(4) -0.017(4) 0.008(4) C86 0.024(5) 0.044(5) 0.024(5) -0.015(4) -0.006(4) 0.002(4) C31 0.043(6) 0.040(5) 0.042(6) -0.017(4) -0.001(5) -0.005(5) C32 0.059(8) 0.041(6) 0.061(7) -0.003(5) 0.017(6) -0.012(5) C33 0.078(10) 0.048(7) 0.094(10) 0.007(6) -0.012(8) -0.010(7) C34 0.081(10) 0.057(7) 0.083(10) 0.024(7) 0.011(8) -0.027(7) C35 0.051(9) 0.101(10) 0.105(12) 0.027(9) 0.008(8) -0.013(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 N5 2.080(6) . ? Sb1 N8 2.095(6) . ? Sb1 O1 2.095(5) . ? Sb1 N7 2.479(6) . ? Sb2 N8 2.077(6) . ? Sb2 N7 2.089(6) . ? Sb2 O2 2.101(5) . ? Sb2 N6 2.527(6) . ? Sb3 N6 2.082(6) . ? Sb3 N5 2.087(6) . ? Sb3 O3 2.085(5) . ? Sb3 N8 2.494(6) . ? Sb4 N6 2.075(6) . ? Sb4 O4 2.078(5) . ? Sb4 N7 2.080(6) . ? Sb4 N5 2.543(6) . ? O1 C11 1.349(9) . ? O2 C21 1.329(9) . ? O3 C31 1.340(10) . ? O4 C41 1.333(9) . ? N1 C11 1.333(10) . ? N1 C15 1.349(10) . ? N2 C21 1.324(10) . ? N2 C25 1.350(10) . ? N3 C31 1.314(12) . ? N3 C35 1.354(13) . ? N4 C41 1.334(10) . ? N4 C45 1.354(12) . ? N5 C51 1.498(9) . ? N6 C61 1.500(9) . ? N7 C71 1.488(9) . ? N8 C81 1.502(9) . ? C11 C12 1.374(11) . ? C12 C13 1.368(11) . ? C13 C14 1.377(13) . ? C14 C15 1.365(12) . ? C41 C42 1.392(11) . ? C42 C43 1.385(14) . ? C43 C44 1.375(16) . ? C44 C45 1.353(15) . ? C21 C22 1.388(11) . ? C22 C23 1.388(13) . ? C23 C24 1.335(15) . ? C24 C25 1.358(14) . ? C51 C52 1.511(12) . ? C51 C56 1.516(11) . ? C52 C53 1.515(10) . ? C53 C54 1.528(13) . ? C54 C55 1.537(14) . ? C55 C56 1.540(10) . ? C61 C66 1.501(10) . ? C61 C62 1.523(10) . ? C62 C63 1.521(10) . ? C63 C64 1.501(12) . ? C64 C65 1.543(11) . ? C65 C66 1.543(10) . ? C71 C72 1.524(9) . ? C71 C76 1.528(10) . ? C72 C73 1.517(11) . ? C73 C74 1.511(11) . ? C74 C75 1.522(11) . ? C75 C76 1.528(11) . ? C81 C86 1.518(10) . ? C81 C82 1.519(10) . ? C82 C83 1.521(11) . ? C83 C84 1.516(11) . ? C84 C85 1.515(11) . ? C85 C86 1.525(11) . ? C31 C32 1.384(12) . ? C32 C33 1.361(14) . ? C33 C34 1.354(16) . ? C34 C35 1.351(15) . ? C1 C2 1.26(2) . ? C1 C3 1.47(2) 2_476 ? C2 C3 1.48(2) . ? C3 C4 1.25(3) . ? C3 C1 1.47(2) 2_476 ? 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 N5 Sb1 N8 83.8(2) . . ? N5 Sb1 O1 91.9(2) . . ? N8 Sb1 O1 84.1(2) . . ? N5 Sb1 N7 77.1(2) . . ? N8 Sb1 N7 74.1(2) . . ? O1 Sb1 N7 156.5(2) . . ? N8 Sb2 N7 83.5(2) . . ? N8 Sb2 O2 91.2(2) . . ? N7 Sb2 O2 83.6(2) . . ? N8 Sb2 N6 76.8(2) . . ? N7 Sb2 N6 73.6(2) . . ? O2 Sb2 N6 155.16(18) . . ? N6 Sb3 N5 84.1(2) . . ? N6 Sb3 O3 88.6(2) . . ? N5 Sb3 O3 85.9(2) . . ? N6 Sb3 N8 77.5(2) . . ? N5 Sb3 N8 74.4(2) . . ? O3 Sb3 N8 156.7(2) . . ? N6 Sb4 O4 83.7(2) . . ? N6 Sb4 N7 84.3(2) . . ? O4 Sb4 N7 91.7(2) . . ? N6 Sb4 N5 73.6(2) . . ? O4 Sb4 N5 154.92(19) . . ? N7 Sb4 N5 75.7(2) . . ? C11 O1 Sb1 116.2(5) . . ? C21 O2 Sb2 116.4(5) . . ? C31 O3 Sb3 117.0(5) . . ? C41 O4 Sb4 120.0(4) . . ? C11 N1 C15 116.2(7) . . ? C21 N2 C25 116.9(8) . . ? C31 N3 C35 116.5(9) . . ? C41 N4 C45 116.2(8) . . ? C51 N5 Sb1 121.8(5) . . ? C51 N5 Sb3 119.9(5) . . ? Sb1 N5 Sb3 106.2(3) . . ? C51 N5 Sb4 109.1(4) . . ? Sb1 N5 Sb4 102.2(2) . . ? Sb3 N5 Sb4 92.1(2) . . ? C61 N6 Sb4 120.1(4) . . ? C61 N6 Sb3 120.0(5) . . ? Sb4 N6 Sb3 107.3(2) . . ? C61 N6 Sb2 110.2(4) . . ? Sb4 N6 Sb2 92.2(2) . . ? Sb3 N6 Sb2 101.9(2) . . ? C71 N7 Sb4 121.2(5) . . ? C71 N7 Sb2 120.8(4) . . ? Sb4 N7 Sb2 106.0(3) . . ? C71 N7 Sb1 106.4(4) . . ? Sb4 N7 Sb1 104.3(2) . . ? Sb2 N7 Sb1 93.1(2) . . ? C81 N8 Sb2 121.3(4) . . ? C81 N8 Sb1 121.8(4) . . ? Sb2 N8 Sb1 105.8(3) . . ? C81 N8 Sb3 106.6(4) . . ? Sb2 N8 Sb3 103.1(2) . . ? Sb1 N8 Sb3 92.7(2) . . ? N1 C11 O1 117.0(7) . . ? N1 C11 C12 123.0(7) . . ? O1 C11 C12 120.0(8) . . ? C13 C12 C11 119.3(9) . . ? C12 C13 C14 119.2(8) . . ? C15 C14 C13 117.7(8) . . ? N1 C15 C14 124.5(9) . . ? O4 C41 N4 117.2(7) . . ? O4 C41 C42 118.9(8) . . ? N4 C41 C42 123.9(8) . . ? C41 C42 C43 117.7(10) . . ? C44 C43 C42 118.9(10) . . ? C45 C44 C43 119.4(10) . . ? N4 C45 C44 123.8(10) . . ? N2 C21 O2 118.0(7) . . ? N2 C21 C22 122.8(8) . . ? O2 C21 C22 119.2(8) . . ? C23 C22 C21 117.2(9) . . ? C24 C23 C22 120.9(10) . . ? C23 C24 C25 118.1(9) . . ? N2 C25 C24 124.0(9) . . ? N5 C51 C52 111.4(6) . . ? N5 C51 C56 113.3(6) . . ? C52 C51 C56 110.6(7) . . ? C51 C52 C53 112.2(7) . . ? C52 C53 C54 110.3(8) . . ? C53 C54 C55 110.1(7) . . ? C56 C55 C54 110.6(7) . . ? C51 C56 C55 110.0(7) . . ? N6 C61 C66 111.1(6) . . ? N6 C61 C62 113.2(6) . . ? C66 C61 C62 110.5(6) . . ? C63 C62 C61 112.1(6) . . ? C64 C63 C62 111.1(7) . . ? C63 C64 C65 110.6(7) . . ? C64 C65 C66 109.9(6) . . ? C61 C66 C65 112.6(7) . . ? N7 C71 C72 114.2(6) . . ? N7 C71 C76 110.5(5) . . ? C72 C71 C76 110.0(6) . . ? C73 C72 C71 111.2(6) . . ? C74 C73 C72 110.0(7) . . ? C73 C74 C75 112.0(7) . . ? C74 C75 C76 109.8(7) . . ? C71 C76 C75 111.8(6) . . ? N8 C81 C86 113.5(6) . . ? N8 C81 C82 109.7(6) . . ? C86 C81 C82 111.0(6) . . ? C81 C82 C83 111.0(6) . . ? C84 C83 C82 111.3(7) . . ? C85 C84 C83 110.5(7) . . ? C84 C85 C86 111.3(7) . . ? C81 C86 C85 110.7(7) . . ? N3 C31 O3 117.5(8) . . ? N3 C31 C32 122.3(9) . . ? O3 C31 C32 120.1(9) . . ? C33 C32 C31 118.7(11) . . ? C34 C33 C32 120.6(11) . . ? C35 C34 C33 116.9(11) . . ? C34 C35 N3 125.0(12) . . ? C2 C1 C3 134(2) . 2_476 ? C1 C2 C3 121.7(18) . . ? C4 C3 C2 126(3) . . ? C4 C3 C1 130(3) . 2_476 ? C2 C3 C1 104.4(18) . 2_476 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.468 _refine_diff_density_min -1.718 _refine_diff_density_rms 0.319 data_dw9825 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 N6 Na Sb3' _chemical_formula_weight 865.03 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' 'Na' 'Na' 0.0362 0.0249 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.599(2) _cell_length_b 21.379(4) _cell_length_c 17.097(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.82(3) _cell_angle_gamma 90.00 _cell_volume 3457.2(11) _cell_formula_units_Z 4 _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 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 2.366 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.644 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 ? _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 6596 _diffrn_reflns_av_R_equivalents 0.0881 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4499 _reflns_number_gt 3116 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _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^)+(0.1522P)^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 4499 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1155 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.2259 _refine_ls_wR_factor_gt 0.1986 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.09100(11) 0.60370(5) 0.26162(6) 0.0267(4) Uani 1 1 d . . . Sb2 Sb -0.16637(11) 0.55762(5) 0.34844(6) 0.0257(4) Uani 1 1 d . . . Sb3 Sb -0.43761(11) 0.64470(6) 0.35926(6) 0.0307(4) Uani 1 1 d . . . Na1 Na -0.1787(7) 0.6996(3) 0.2756(4) 0.0459(18) Uani 1 1 d . . . N1 N -0.3298(14) 0.6074(7) 0.2772(8) 0.033(3) Uani 1 1 d . . . N2 N -0.0700(12) 0.5448(6) 0.2396(8) 0.026(3) Uani 1 1 d . . . N3 N -0.2582(14) 0.6228(7) 0.4282(8) 0.034(4) Uani 1 1 d . . . N4 N -0.0084(13) 0.6267(6) 0.3542(7) 0.027(3) Uani 1 1 d . . . N5 N -0.3775(15) 0.7377(8) 0.3350(9) 0.045(4) Uani 1 1 d . . . N6 N -0.0074(14) 0.6791(7) 0.1909(8) 0.035(3) Uani 1 1 d . . . C41 C 0.0633(16) 0.6496(7) 0.4295(9) 0.024(4) Uani 1 1 d . . . H41A H -0.0092 0.6626 0.4602 0.028 Uiso 1 1 calc R . . C42 C 0.1523(17) 0.7067(8) 0.4193(10) 0.035(4) Uani 1 1 d . . . H42A H 0.0926 0.7383 0.3897 0.042 Uiso 1 1 calc R . . H42B H 0.2242 0.6951 0.3883 0.042 Uiso 1 1 calc R . . C43 C 0.224(2) 0.7345(9) 0.4976(11) 0.046(5) Uani 1 1 d . . . H43A H 0.1527 0.7501 0.5267 0.056 Uiso 1 1 calc R . . H43B H 0.2830 0.7694 0.4876 0.056 Uiso 1 1 calc R . . C44 C 0.3140(18) 0.6850(9) 0.5470(10) 0.043(5) Uani 1 1 d . . . H44A H 0.3527 0.7023 0.5986 0.051 Uiso 1 1 calc R . . H44B H 0.3923 0.6735 0.5209 0.051 Uiso 1 1 calc R . . C45 C 0.227(2) 0.6268(9) 0.5579(10) 0.043(5) Uani 1 1 d . . . H45A H 0.2877 0.5957 0.5876 0.052 Uiso 1 1 calc R . . H45B H 0.1542 0.6377 0.5887 0.052 Uiso 1 1 calc R . . C46 C 0.157(2) 0.5985(9) 0.4789(11) 0.046(5) Uani 1 1 d . . . H46A H 0.0982 0.5632 0.4884 0.055 Uiso 1 1 calc R . . H46B H 0.2283 0.5837 0.4497 0.055 Uiso 1 1 calc R . . C11 C -0.3983(16) 0.5800(8) 0.2011(10) 0.034(4) Uani 1 1 d . . . H11A H -0.3221 0.5632 0.1758 0.040 Uiso 1 1 calc R . . C12 C -0.4985(18) 0.5273(9) 0.2055(10) 0.041(5) Uani 1 1 d . . . H12A H -0.5767 0.5424 0.2295 0.049 Uiso 1 1 calc R . . H12B H -0.4502 0.4952 0.2400 0.049 Uiso 1 1 calc R . . C13 C -0.557(2) 0.4982(11) 0.1263(10) 0.056(6) Uani 1 1 d . . . H13A H -0.6266 0.4666 0.1330 0.067 Uiso 1 1 calc R . . H13B H -0.4815 0.4782 0.1044 0.067 Uiso 1 1 calc R . . C14 C -0.627(2) 0.5500(12) 0.0685(11) 0.061(6) Uani 1 1 d . . . H14A H -0.6572 0.5321 0.0162 0.073 Uiso 1 1 calc R . . H14B H -0.7099 0.5661 0.0872 0.073 Uiso 1 1 calc R . . C15 C -0.523(2) 0.6037(12) 0.0629(11) 0.065(7) Uani 1 1 d . . . H15A H -0.4429 0.5881 0.0411 0.078 Uiso 1 1 calc R . . H15B H -0.5694 0.6357 0.0274 0.078 Uiso 1 1 calc R . . C16 C -0.472(2) 0.6323(9) 0.1447(9) 0.045(5) Uani 1 1 d . . . H16A H -0.5508 0.6496 0.1659 0.054 Uiso 1 1 calc R . . H16B H -0.4050 0.6657 0.1405 0.054 Uiso 1 1 calc R . . C31 C -0.2488(18) 0.6043(8) 0.5132(9) 0.035(4) Uani 1 1 d . . . H31A H -0.1549 0.5858 0.5295 0.042 Uiso 1 1 calc R . . C32 C -0.354(2) 0.5560(9) 0.5307(10) 0.042(5) Uani 1 1 d . . . H32A H -0.3463 0.5190 0.4990 0.051 Uiso 1 1 calc R . . H32B H -0.4492 0.5726 0.5151 0.051 Uiso 1 1 calc R . . C33 C -0.333(3) 0.5372(10) 0.6201(11) 0.056(6) Uani 1 1 d . . . H33A H -0.4029 0.5065 0.6286 0.067 Uiso 1 1 calc R . . H33B H -0.2397 0.5188 0.6359 0.067 Uiso 1 1 calc R . . C34 C -0.346(2) 0.5943(8) 0.6684(9) 0.038(4) Uani 1 1 d . . . H34A H -0.4407 0.6116 0.6542 0.045 Uiso 1 1 calc R . . H34B H -0.3313 0.5836 0.7244 0.045 Uiso 1 1 calc R . . C35 C -0.240(2) 0.6410(11) 0.6532(10) 0.052(6) Uani 1 1 d . . . H35A H -0.1462 0.6236 0.6696 0.062 Uiso 1 1 calc R . . H35B H -0.2479 0.6778 0.6853 0.062 Uiso 1 1 calc R . . C36 C -0.257(2) 0.6601(9) 0.5673(10) 0.040(5) Uani 1 1 d . . . H36A H -0.1835 0.6898 0.5608 0.048 Uiso 1 1 calc R . . H36B H -0.3476 0.6807 0.5520 0.048 Uiso 1 1 calc R . . C21 C -0.0823(19) 0.4934(8) 0.1812(10) 0.037(4) Uani 1 1 d . . . H21A H -0.1547 0.5075 0.1373 0.045 Uiso 1 1 calc R . . C22 C -0.142(2) 0.4352(9) 0.2108(11) 0.046(5) Uani 1 1 d . . . H22A H -0.2320 0.4447 0.2261 0.055 Uiso 1 1 calc R . . H22B H -0.0784 0.4206 0.2577 0.055 Uiso 1 1 calc R . . C23 C -0.162(2) 0.3824(8) 0.1476(12) 0.047(5) Uani 1 1 d . . . H23A H -0.1852 0.3435 0.1716 0.056 Uiso 1 1 calc R . . H23B H -0.2393 0.3930 0.1053 0.056 Uiso 1 1 calc R . . C24 C -0.027(2) 0.3745(9) 0.1140(13) 0.056(6) Uani 1 1 d . . . H24A H 0.0444 0.3567 0.1548 0.067 Uiso 1 1 calc R . . H24B H -0.0445 0.3448 0.0706 0.067 Uiso 1 1 calc R . . C25 C 0.028(2) 0.4311(9) 0.0856(12) 0.051(5) Uani 1 1 d . . . H25A H -0.0350 0.4448 0.0382 0.061 Uiso 1 1 calc R . . H25B H 0.1193 0.4223 0.0710 0.061 Uiso 1 1 calc R . . C26 C 0.044(2) 0.4822(9) 0.1448(11) 0.050(5) Uani 1 1 d . . . H26A H 0.1230 0.4724 0.1865 0.060 Uiso 1 1 calc R . . H26B H 0.0673 0.5205 0.1193 0.060 Uiso 1 1 calc R . . C61 C 0.096(2) 0.7314(8) 0.1903(11) 0.054(6) Uani 1 1 d . . . H61A H 0.1612 0.7209 0.1557 0.082 Uiso 1 1 calc R . . H61B H 0.1465 0.7379 0.2431 0.082 Uiso 1 1 calc R . . H61C H 0.0458 0.7689 0.1718 0.082 Uiso 1 1 calc R . . C62 C -0.059(2) 0.6598(11) 0.1099(10) 0.054(6) Uani 1 1 d . . . H62A H 0.0194 0.6532 0.0828 0.082 Uiso 1 1 calc R . . H62B H -0.1193 0.6919 0.0831 0.082 Uiso 1 1 calc R . . H62C H -0.1119 0.6217 0.1100 0.082 Uiso 1 1 calc R . . C51 C -0.500(2) 0.7726(10) 0.2892(13) 0.063(6) Uani 1 1 d . . . H51A H -0.5650 0.7832 0.3238 0.094 Uiso 1 1 calc R . . H51B H -0.5462 0.7469 0.2467 0.094 Uiso 1 1 calc R . . H51C H -0.4660 0.8101 0.2679 0.094 Uiso 1 1 calc R . . C52 C -0.321(2) 0.7717(10) 0.4063(12) 0.059(6) Uani 1 1 d . . . H52A H -0.3977 0.7873 0.4303 0.088 Uiso 1 1 calc R . . H52B H -0.2652 0.8061 0.3933 0.088 Uiso 1 1 calc R . . H52C H -0.2634 0.7443 0.4428 0.088 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 0.0250(6) 0.0289(7) 0.0266(6) -0.0032(5) 0.0055(4) -0.0013(5) Sb2 0.0266(6) 0.0240(6) 0.0260(6) 0.0015(5) 0.0031(4) -0.0010(5) Sb3 0.0265(6) 0.0366(7) 0.0294(6) 0.0015(5) 0.0059(5) 0.0016(5) Na1 0.038(4) 0.042(4) 0.062(5) 0.015(4) 0.018(3) 0.006(4) N1 0.036(8) 0.035(8) 0.033(8) 0.001(7) 0.022(6) 0.007(7) N2 0.018(6) 0.011(7) 0.047(8) -0.008(6) 0.002(6) 0.005(5) N3 0.036(8) 0.039(9) 0.029(8) -0.007(7) 0.015(6) 0.023(7) N4 0.021(7) 0.025(8) 0.035(8) 0.004(6) 0.006(6) -0.002(6) N5 0.040(9) 0.051(10) 0.042(9) 0.005(8) 0.007(7) 0.021(8) N6 0.038(8) 0.038(9) 0.029(7) 0.002(7) 0.002(6) -0.007(7) C41 0.024(8) 0.019(8) 0.023(8) 0.001(7) -0.010(7) 0.003(7) C42 0.030(9) 0.041(11) 0.033(9) 0.003(9) 0.000(7) 0.005(8) C43 0.059(12) 0.031(11) 0.045(11) -0.013(9) -0.003(10) 0.004(10) C44 0.039(10) 0.041(12) 0.040(10) -0.016(9) -0.014(8) -0.011(9) C45 0.049(12) 0.045(12) 0.028(9) -0.008(9) -0.014(8) 0.006(10) C46 0.038(11) 0.047(12) 0.049(11) -0.004(10) -0.001(9) 0.001(9) C11 0.016(8) 0.045(11) 0.038(10) -0.009(9) 0.000(7) 0.016(8) C12 0.035(10) 0.051(12) 0.037(10) 0.003(9) 0.005(8) 0.002(9) C13 0.058(13) 0.074(16) 0.035(10) -0.020(11) 0.003(9) -0.016(12) C14 0.047(12) 0.095(19) 0.036(11) -0.003(12) -0.005(9) 0.007(13) C15 0.064(14) 0.088(18) 0.034(11) 0.002(12) -0.018(10) 0.029(14) C16 0.054(12) 0.046(12) 0.026(9) 0.008(9) -0.016(9) 0.007(10) C31 0.038(10) 0.042(11) 0.024(9) 0.004(8) 0.000(7) 0.006(9) C32 0.052(11) 0.044(12) 0.033(10) -0.003(9) 0.014(8) 0.003(10) C33 0.087(16) 0.052(13) 0.036(11) 0.012(10) 0.027(11) -0.005(12) C34 0.065(12) 0.029(10) 0.019(8) -0.004(8) 0.004(8) -0.004(9) C35 0.055(12) 0.075(16) 0.024(9) -0.006(10) 0.000(9) -0.011(12) C36 0.045(11) 0.040(11) 0.036(10) -0.001(9) 0.007(8) -0.013(9) C21 0.049(11) 0.023(10) 0.042(10) -0.017(8) 0.014(9) 0.000(9) C22 0.058(12) 0.034(11) 0.049(11) -0.009(10) 0.015(10) 0.001(10) C23 0.062(13) 0.017(10) 0.064(13) -0.013(9) 0.021(10) -0.018(9) C24 0.069(14) 0.028(11) 0.070(14) -0.019(11) 0.016(12) -0.017(11) C25 0.060(13) 0.034(11) 0.061(13) -0.004(10) 0.018(11) -0.004(10) C26 0.063(13) 0.040(12) 0.052(12) -0.014(10) 0.023(10) 0.012(10) C61 0.098(17) 0.025(11) 0.033(10) 0.019(9) -0.009(10) 0.000(11) C62 0.064(14) 0.067(15) 0.029(10) 0.002(10) 0.000(9) -0.020(12) C51 0.055(13) 0.059(14) 0.074(15) 0.020(12) 0.009(11) 0.035(12) C52 0.072(15) 0.046(13) 0.056(13) 0.002(11) 0.003(11) -0.004(12) _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 N2 1.980(12) . ? Sb1 N4 2.043(13) . ? Sb1 N6 2.136(14) . ? Sb1 Sb2 3.2446(16) . ? Sb1 Na1 3.342(7) . ? Sb2 N1 2.104(14) . ? Sb2 N4 2.108(13) . ? Sb2 N2 2.232(13) . ? Sb2 N3 2.233(12) . ? Sb2 Sb3 3.2316(16) . ? Sb2 Na1 3.275(7) . ? Sb3 N3 1.970(13) . ? Sb3 N1 2.043(12) . ? Sb3 N5 2.130(17) . ? Sb3 Na1 3.288(7) . ? Na1 N6 2.410(16) . ? Na1 N1 2.449(16) . ? Na1 N5 2.450(16) . ? Na1 N4 2.481(14) . ? N1 C11 1.47(2) . ? N2 C21 1.47(2) . ? N3 C31 1.50(2) . ? N4 C41 1.438(19) . ? N5 C52 1.44(2) . ? N5 C51 1.49(2) . ? N6 C62 1.45(2) . ? N6 C61 1.49(2) . ? C41 C42 1.52(2) . ? C41 C46 1.57(2) . ? C42 C43 1.52(2) . ? C43 C44 1.53(3) . ? C44 C45 1.53(3) . ? C45 C46 1.53(2) . ? C11 C12 1.49(2) . ? C11 C16 1.56(2) . ? C12 C13 1.51(2) . ? C13 C14 1.56(3) . ? C14 C15 1.53(3) . ? C15 C16 1.53(3) . ? C31 C32 1.51(2) . ? C31 C36 1.52(2) . ? C32 C33 1.56(2) . ? C33 C34 1.49(3) . ? C34 C35 1.48(3) . ? C35 C36 1.51(2) . ? C21 C26 1.47(2) . ? C21 C22 1.49(3) . ? C22 C23 1.55(2) . ? C23 C24 1.51(3) . ? C24 C25 1.44(3) . ? C25 C26 1.48(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Sb1 N4 81.3(5) . . ? N2 Sb1 N6 96.7(5) . . ? N4 Sb1 N6 92.1(5) . . ? N2 Sb1 Sb2 42.6(4) . . ? N4 Sb1 Sb2 39.3(4) . . ? N6 Sb1 Sb2 101.0(4) . . ? N2 Sb1 Na1 79.3(4) . . ? N4 Sb1 Na1 47.7(4) . . ? N6 Sb1 Na1 46.0(4) . . ? Sb2 Sb1 Na1 59.60(12) . . ? N1 Sb2 N4 97.6(5) . . ? N1 Sb2 N2 87.3(4) . . ? N4 Sb2 N2 74.2(5) . . ? N1 Sb2 N3 72.8(5) . . ? N4 Sb2 N3 83.7(5) . . ? N2 Sb2 N3 148.1(5) . . ? N1 Sb2 Sb3 38.1(3) . . ? N4 Sb2 Sb3 100.0(4) . . ? N2 Sb2 Sb3 124.8(3) . . ? N3 Sb2 Sb3 36.8(3) . . ? N1 Sb2 Sb1 97.6(3) . . ? N4 Sb2 Sb1 37.9(4) . . ? N2 Sb2 Sb1 36.9(3) . . ? N3 Sb2 Sb1 120.0(4) . . ? Sb3 Sb2 Sb1 122.35(5) . . ? N1 Sb2 Na1 48.4(4) . . ? N4 Sb2 Na1 49.3(4) . . ? N2 Sb2 Na1 77.9(3) . . ? N3 Sb2 Na1 70.2(4) . . ? Sb3 Sb2 Na1 60.71(12) . . ? Sb1 Sb2 Na1 61.68(12) . . ? N3 Sb3 N1 79.9(5) . . ? N3 Sb3 N5 95.7(6) . . ? N1 Sb3 N5 92.6(6) . . ? N3 Sb3 Sb2 42.8(4) . . ? N1 Sb3 Sb2 39.5(4) . . ? N5 Sb3 Sb2 106.2(4) . . ? N3 Sb3 Na1 72.3(4) . . ? N1 Sb3 Na1 48.0(4) . . ? N5 Sb3 Na1 48.1(4) . . ? Sb2 Sb3 Na1 60.29(13) . . ? N6 Na1 N1 109.0(5) . . ? N6 Na1 N5 165.9(6) . . ? N1 Na1 N5 76.0(5) . . ? N6 Na1 N4 76.0(5) . . ? N1 Na1 N4 80.0(5) . . ? N5 Na1 N4 118.2(5) . . ? N6 Na1 Sb2 94.4(4) . . ? N1 Na1 Sb2 40.0(3) . . ? N5 Na1 Sb2 97.5(4) . . ? N4 Na1 Sb2 40.1(3) . . ? N6 Na1 Sb3 147.2(4) . . ? N1 Na1 Sb3 38.3(3) . . ? N5 Na1 Sb3 40.4(4) . . ? N4 Na1 Sb3 91.0(4) . . ? Sb2 Na1 Sb3 59.00(12) . . ? N6 Na1 Sb1 39.6(3) . . ? N1 Na1 Sb1 88.6(4) . . ? N5 Na1 Sb1 154.3(5) . . ? N4 Na1 Sb1 37.5(3) . . ? Sb2 Na1 Sb1 58.72(12) . . ? Sb3 Na1 Sb1 117.7(2) . . ? C11 N1 Sb3 124.0(10) . . ? C11 N1 Sb2 119.1(10) . . ? Sb3 N1 Sb2 102.4(6) . . ? C11 N1 Na1 119.1(10) . . ? Sb3 N1 Na1 93.7(6) . . ? Sb2 N1 Na1 91.7(5) . . ? C21 N2 Sb1 124.9(10) . . ? C21 N2 Sb2 131.3(10) . . ? Sb1 N2 Sb2 100.6(5) . . ? C31 N3 Sb3 123.1(10) . . ? C31 N3 Sb2 117.6(10) . . ? Sb3 N3 Sb2 100.3(6) . . ? C41 N4 Sb1 124.1(10) . . ? C41 N4 Sb2 120.8(10) . . ? Sb1 N4 Sb2 102.8(6) . . ? C41 N4 Na1 116.2(10) . . ? Sb1 N4 Na1 94.8(5) . . ? Sb2 N4 Na1 90.7(5) . . ? C52 N5 C51 109.7(16) . . ? C52 N5 Sb3 112.4(12) . . ? C51 N5 Sb3 110.7(13) . . ? C52 N5 Na1 108.2(12) . . ? C51 N5 Na1 123.1(12) . . ? Sb3 N5 Na1 91.5(6) . . ? C62 N6 C61 109.0(14) . . ? C62 N6 Sb1 112.0(12) . . ? C61 N6 Sb1 109.8(10) . . ? C62 N6 Na1 117.9(12) . . ? C61 N6 Na1 112.9(12) . . ? Sb1 N6 Na1 94.5(5) . . ? N4 C41 C42 111.3(13) . . ? N4 C41 C46 112.7(13) . . ? C42 C41 C46 110.0(13) . . ? C41 C42 C43 113.1(14) . . ? C42 C43 C44 110.1(15) . . ? C43 C44 C45 111.1(14) . . ? C46 C45 C44 112.5(16) . . ? C45 C46 C41 109.0(15) . . ? N1 C11 C12 116.8(14) . . ? N1 C11 C16 110.3(14) . . ? C12 C11 C16 110.2(14) . . ? C11 C12 C13 114.3(16) . . ? C12 C13 C14 109.3(18) . . ? C15 C14 C13 111.0(16) . . ? C16 C15 C14 110.8(18) . . ? C15 C16 C11 108.7(16) . . ? N3 C31 C32 116.2(14) . . ? N3 C31 C36 112.5(14) . . ? C32 C31 C36 108.0(14) . . ? C31 C32 C33 112.8(15) . . ? C34 C33 C32 108.8(16) . . ? C35 C34 C33 108.9(16) . . ? C34 C35 C36 113.0(15) . . ? C35 C36 C31 111.9(16) . . ? N2 C21 C26 115.5(15) . . ? N2 C21 C22 112.4(14) . . ? C26 C21 C22 113.4(16) . . ? C21 C22 C23 112.3(15) . . ? C24 C23 C22 109.4(15) . . ? C25 C24 C23 115.0(18) . . ? C24 C25 C26 113.1(18) . . ? C21 C26 C25 114.2(17) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.831 _refine_diff_density_min -1.814 _refine_diff_density_rms 0.278