Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'J.Chem.Soc.,Dalton Trans.' loop_ _publ_author_name 'Clegg, W.' 'Liddle, Stephen T.' _publ_contact_author_name 'Prof W Clegg' _publ_contact_author_address ; Prof W Clegg Department of Chemistry University of Newcastle Bedson Building NEWCASTLE UPON TYNE NE1 7RU U.K. ; _publ_contact_author_email 'W.Clegg@newcastle.ac.uk' data_2 _database_code_CSD 152062 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H29 Li N2 O4 Si' _chemical_formula_weight 348.44 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9095(3) _cell_length_b 12.2197(4) _cell_length_c 16.2582(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.935(2) _cell_angle_gamma 90.00 _cell_volume 1939.20(11) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 13609 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.53 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.78 _exptl_crystal_size_mid 0.68 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.825 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13559 _diffrn_reflns_av_R_equivalents 0.0137 _diffrn_reflns_av_sigmaI/netI 0.0119 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3421 _reflns_number_gt 3138 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0382P)^2^+0.5802P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3421 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0749 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li -0.2040(2) 0.39036(16) 0.34093(12) 0.0268(4) Uani 1 1 d . . . N1 N -0.07855(10) 0.25261(8) 0.39847(6) 0.0245(2) Uani 1 1 d . . . N2 N -0.03610(10) 0.35389(8) 0.28714(6) 0.0237(2) Uani 1 1 d . . . C1 C -0.03972(13) 0.17787(10) 0.45795(7) 0.0285(3) Uani 1 1 d . . . H1A H -0.1045 0.1578 0.4921 0.034 Uiso 1 1 calc R . . C2 C 0.08663(13) 0.12762(10) 0.47380(8) 0.0308(3) Uani 1 1 d . . . H2A H 0.1079 0.0738 0.5162 0.037 Uiso 1 1 calc R . . C3 C 0.18157(13) 0.15950(10) 0.42460(8) 0.0303(3) Uani 1 1 d . . . H3A H 0.2710 0.1288 0.4341 0.036 Uiso 1 1 calc R . . C4 C 0.14612(12) 0.23516(10) 0.36256(8) 0.0275(3) Uani 1 1 d . . . H4A H 0.2116 0.2567 0.3294 0.033 Uiso 1 1 calc R . . C5 C 0.01206(11) 0.28231(9) 0.34693(7) 0.0217(2) Uani 1 1 d . . . Si1 Si 0.04605(3) 0.40963(3) 0.21379(2) 0.02455(11) Uani 1 1 d . . . C6 C 0.13087(16) 0.30841(13) 0.15184(9) 0.0440(4) Uani 1 1 d . . . H6A H 0.0638 0.2534 0.1274 0.066 Uiso 1 1 calc R . . H6B H 0.2065 0.2724 0.1887 0.066 Uiso 1 1 calc R . . H6C H 0.1664 0.3468 0.1071 0.066 Uiso 1 1 calc R . . C7 C -0.08270(14) 0.48332(12) 0.13550(8) 0.0378(3) Uani 1 1 d . . . H7A H -0.1297 0.5385 0.1640 0.057 Uiso 1 1 calc R . . H7B H -0.1498 0.4309 0.1071 0.057 Uiso 1 1 calc R . . H7C H -0.0360 0.5193 0.0944 0.057 Uiso 1 1 calc R . . C8 C 0.18090(13) 0.51003(11) 0.26083(8) 0.0311(3) Uani 1 1 d . . . H8A H 0.1377 0.5708 0.2859 0.047 Uiso 1 1 calc R . . H8B H 0.2285 0.5383 0.2172 0.047 Uiso 1 1 calc R . . H8C H 0.2469 0.4734 0.3039 0.047 Uiso 1 1 calc R . . O1 O -0.35826(9) 0.39986(7) 0.43005(5) 0.0326(2) Uani 1 1 d . . . O2 O -0.13300(9) 0.52051(7) 0.42856(5) 0.0305(2) Uani 1 1 d . . . O3 O -0.29944(8) 0.52207(7) 0.27597(5) 0.0283(2) Uani 1 1 d . . . O4 O -0.39213(8) 0.30955(7) 0.27610(5) 0.0287(2) Uani 1 1 d . . . C9 C -0.26793(15) 0.41633(11) 0.50735(8) 0.0348(3) Uani 1 1 d . . . H9A H -0.1990 0.3570 0.5172 0.042 Uiso 1 1 calc R . . H9B H -0.3198 0.4173 0.5542 0.042 Uiso 1 1 calc R . . C10 C -0.19969(14) 0.52448(11) 0.50022(8) 0.0357(3) Uani 1 1 d . . . H10A H -0.2686 0.5839 0.4937 0.043 Uiso 1 1 calc R . . H10B H -0.1317 0.5389 0.5512 0.043 Uiso 1 1 calc R . . C11 C -0.14867(14) 0.61744(11) 0.37879(9) 0.0361(3) Uani 1 1 d . . . H11A H -0.0760 0.6200 0.3440 0.043 Uiso 1 1 calc R . . H11B H -0.1380 0.6824 0.4157 0.043 Uiso 1 1 calc R . . C12 C -0.28686(14) 0.62100(10) 0.32322(9) 0.0346(3) Uani 1 1 d . . . H12A H -0.3605 0.6261 0.3572 0.041 Uiso 1 1 calc R . . H12B H -0.2933 0.6852 0.2856 0.041 Uiso 1 1 calc R . . C13 C -0.43545(13) 0.49919(11) 0.23533(9) 0.0356(3) Uani 1 1 d . . . H13A H -0.4613 0.5479 0.1865 0.043 Uiso 1 1 calc R . . H13B H -0.5008 0.5107 0.2742 0.043 Uiso 1 1 calc R . . C14 C -0.43788(14) 0.38169(12) 0.20782(8) 0.0362(3) Uani 1 1 d . . . H14A H -0.5324 0.3616 0.1817 0.043 Uiso 1 1 calc R . . H14B H -0.3783 0.3730 0.1652 0.043 Uiso 1 1 calc R . . C15 C -0.49007(13) 0.29048(11) 0.32953(8) 0.0309(3) Uani 1 1 d . . . H15A H -0.5338 0.2181 0.3172 0.037 Uiso 1 1 calc R . . H15B H -0.5624 0.3472 0.3201 0.037 Uiso 1 1 calc R . . C16 C -0.41762(14) 0.29403(11) 0.41855(8) 0.0324(3) Uani 1 1 d . . . H16A H -0.4832 0.2822 0.4573 0.039 Uiso 1 1 calc R . . H16B H -0.3459 0.2369 0.4288 0.039 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 Li1 0.0254(10) 0.0258(10) 0.0293(10) 0.0017(8) 0.0049(8) 0.0019(8) N1 0.0251(5) 0.0228(5) 0.0258(5) 0.0002(4) 0.0053(4) 0.0000(4) N2 0.0235(5) 0.0211(5) 0.0267(5) 0.0010(4) 0.0052(4) -0.0001(4) C1 0.0339(7) 0.0275(6) 0.0246(6) 0.0012(5) 0.0065(5) -0.0010(5) C2 0.0388(7) 0.0266(6) 0.0245(6) 0.0013(5) -0.0012(5) 0.0033(5) C3 0.0259(6) 0.0281(6) 0.0338(7) -0.0042(5) -0.0033(5) 0.0051(5) C4 0.0232(6) 0.0262(6) 0.0332(6) -0.0015(5) 0.0057(5) -0.0009(5) C5 0.0229(6) 0.0176(6) 0.0241(6) -0.0047(4) 0.0028(5) -0.0030(4) Si1 0.02572(19) 0.02517(19) 0.02339(18) 0.00006(13) 0.00600(13) -0.00188(13) C6 0.0506(9) 0.0461(9) 0.0392(8) -0.0092(7) 0.0193(7) 0.0000(7) C7 0.0356(7) 0.0480(8) 0.0287(7) 0.0091(6) 0.0022(6) -0.0026(6) C8 0.0287(6) 0.0312(7) 0.0335(7) 0.0043(5) 0.0058(5) -0.0046(5) O1 0.0398(5) 0.0287(5) 0.0279(5) -0.0015(4) 0.0015(4) -0.0053(4) O2 0.0319(5) 0.0276(5) 0.0315(5) -0.0033(4) 0.0041(4) -0.0001(4) O3 0.0249(4) 0.0263(5) 0.0331(5) 0.0032(4) 0.0031(4) 0.0026(3) O4 0.0276(4) 0.0298(5) 0.0279(4) -0.0002(4) 0.0030(4) 0.0011(4) C9 0.0421(8) 0.0402(8) 0.0219(6) -0.0043(5) 0.0048(5) -0.0021(6) C10 0.0402(8) 0.0374(8) 0.0291(7) -0.0105(6) 0.0048(6) -0.0015(6) C11 0.0382(7) 0.0232(7) 0.0469(8) -0.0021(6) 0.0076(6) -0.0057(5) C12 0.0371(7) 0.0205(6) 0.0467(8) 0.0038(6) 0.0088(6) 0.0037(5) C13 0.0276(7) 0.0372(7) 0.0385(7) 0.0107(6) -0.0037(5) 0.0037(6) C14 0.0350(7) 0.0443(8) 0.0258(6) 0.0030(6) -0.0049(5) -0.0030(6) C15 0.0253(6) 0.0288(7) 0.0384(7) -0.0006(5) 0.0050(5) -0.0050(5) C16 0.0340(7) 0.0299(7) 0.0346(7) 0.0025(5) 0.0096(6) -0.0070(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 N2 2.057(2) . ? Li1 O3 2.063(2) . ? Li1 O2 2.170(2) . ? Li1 N1 2.203(2) . ? Li1 O4 2.210(2) . ? Li1 O1 2.284(2) . ? N1 C1 1.3375(15) . ? N1 C5 1.3783(15) . ? N2 C5 1.3334(15) . ? N2 Si1 1.6981(10) . ? C1 C2 1.3784(18) . ? C2 C3 1.3915(19) . ? C3 C4 1.3687(18) . ? C4 C5 1.4300(16) . ? Si1 C7 1.8704(14) . ? Si1 C8 1.8770(13) . ? Si1 C6 1.8823(14) . ? O1 C16 1.4197(15) . ? O1 C9 1.4259(15) . ? O2 C11 1.4278(16) . ? O2 C10 1.4360(15) . ? O3 C13 1.4227(15) . ? O3 C12 1.4261(16) . ? O4 C14 1.4287(15) . ? O4 C15 1.4289(15) . ? C9 C10 1.4981(19) . ? C11 C12 1.5055(19) . ? C13 C14 1.503(2) . ? C15 C16 1.5011(18) . ? 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 Li1 O3 106.52(10) . . ? N2 Li1 O2 104.10(9) . . ? O3 Li1 O2 80.35(8) . . ? N2 Li1 N1 64.96(7) . . ? O3 Li1 N1 171.46(11) . . ? O2 Li1 N1 100.72(9) . . ? N2 Li1 O4 112.21(10) . . ? O3 Li1 O4 80.20(8) . . ? O2 Li1 O4 142.36(10) . . ? N1 Li1 O4 103.23(9) . . ? N2 Li1 O1 163.68(11) . . ? O3 Li1 O1 89.26(8) . . ? O2 Li1 O1 73.91(7) . . ? N1 Li1 O1 99.20(8) . . ? O4 Li1 O1 73.93(7) . . ? C1 N1 C5 118.89(10) . . ? C1 N1 Li1 154.12(10) . . ? C5 N1 Li1 85.38(8) . . ? C5 N2 Si1 128.35(8) . . ? C5 N2 Li1 92.64(9) . . ? Si1 N2 Li1 137.09(8) . . ? N1 C1 C2 125.31(12) . . ? C1 C2 C3 116.76(11) . . ? C4 C3 C2 119.98(11) . . ? C3 C4 C5 121.04(11) . . ? N2 C5 N1 115.29(10) . . ? N2 C5 C4 126.77(11) . . ? N1 C5 C4 117.94(10) . . ? N2 Si1 C7 108.52(6) . . ? N2 Si1 C8 111.71(5) . . ? C7 Si1 C8 108.46(6) . . ? N2 Si1 C6 115.13(6) . . ? C7 Si1 C6 105.51(7) . . ? C8 Si1 C6 107.17(7) . . ? C16 O1 C9 115.31(10) . . ? C16 O1 Li1 100.24(9) . . ? C9 O1 Li1 100.32(9) . . ? C11 O2 C10 114.30(10) . . ? C11 O2 Li1 104.17(9) . . ? C10 O2 Li1 114.53(9) . . ? C13 O3 C12 113.86(10) . . ? C13 O3 Li1 113.48(9) . . ? C12 O3 Li1 113.32(9) . . ? C14 O4 C15 114.53(10) . . ? C14 O4 Li1 102.91(9) . . ? C15 O4 Li1 112.87(8) . . ? O1 C9 C10 106.22(11) . . ? O2 C10 C9 108.06(10) . . ? O2 C11 C12 111.27(10) . . ? O3 C12 C11 106.54(10) . . ? O3 C13 C14 106.94(10) . . ? O4 C14 C13 111.82(10) . . ? O4 C15 C16 108.62(10) . . ? O1 C16 C15 105.77(10) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.279 _refine_diff_density_min -0.239 _refine_diff_density_rms 0.031 #===END data_3 _database_code_CSD 152063 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H74 N4 Na2 O10 Si2' _chemical_formula_weight 873.19 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.3161(5) _cell_length_b 22.3535(8) _cell_length_c 17.0658(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.458(2) _cell_angle_gamma 90.00 _cell_volume 4871.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 28852 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 28.63 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.76 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 0.145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33676 _diffrn_reflns_av_R_equivalents 0.0196 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8555 _reflns_number_gt 7097 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0512P)^2^+1.3944P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0005(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8555 _refine_ls_number_parameters 576 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0336 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.061 _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 Na1 Na 0.01838(4) 0.16872(3) 0.68757(3) 0.02764(14) Uani 1 1 d . . . N1 N -0.15938(10) 0.20395(6) 0.69566(7) 0.0275(3) Uani 1 1 d . . . N2 N -0.03012(9) 0.17898(6) 0.81197(7) 0.0274(3) Uani 1 1 d . . . C1 C -0.25779(12) 0.22078(7) 0.65888(10) 0.0305(3) Uani 1 1 d . . . H1 H -0.2773 0.2251 0.6011 0.037 Uiso 1 1 calc R . . C2 C -0.33295(12) 0.23239(7) 0.69776(10) 0.0322(4) Uani 1 1 d . . . H2 H -0.4018 0.2442 0.6683 0.039 Uiso 1 1 calc R . . C3 C -0.30351(12) 0.22606(7) 0.78238(10) 0.0314(4) Uani 1 1 d . . . H3 H -0.3526 0.2340 0.8121 0.038 Uiso 1 1 calc R . . C4 C -0.20398(12) 0.20837(7) 0.82277(9) 0.0273(3) Uani 1 1 d . . . H4 H -0.1846 0.2039 0.8805 0.033 Uiso 1 1 calc R . . C5 C -0.12842(11) 0.19644(6) 0.77920(9) 0.0235(3) Uani 1 1 d . . . Si1 Si 0.02851(3) 0.14778(2) 0.90355(2) 0.02814(11) Uani 1 1 d . . . C6 C 0.03510(15) 0.19609(9) 0.99499(10) 0.0417(4) Uani 1 1 d . . . H6A H 0.0793 0.2310 0.9942 0.062 Uiso 1 1 calc R . . H6B H 0.0650 0.1730 1.0450 0.062 Uiso 1 1 calc R . . H6C H -0.0356 0.2094 0.9934 0.062 Uiso 1 1 calc R . . C7 C -0.03622(17) 0.07623(9) 0.91951(12) 0.0510(5) Uani 1 1 d . . . H7A H -0.1093 0.0842 0.9173 0.077 Uiso 1 1 calc R . . H7B H 0.0005 0.0594 0.9730 0.077 Uiso 1 1 calc R . . H7C H -0.0337 0.0476 0.8766 0.077 Uiso 1 1 calc R . . C8 C 0.16629(14) 0.13207(10) 0.90388(11) 0.0495(5) Uani 1 1 d . . . H8A H 0.1663 0.1081 0.8558 0.074 Uiso 1 1 calc R . . H8B H 0.2020 0.1100 0.9536 0.074 Uiso 1 1 calc R . . H8C H 0.2029 0.1699 0.9024 0.074 Uiso 1 1 calc R . . N3 N 0.20021(9) 0.19213(6) 0.69123(7) 0.0259(3) Uani 1 1 d . . . N4 N 0.07211(10) 0.19296(6) 0.56785(8) 0.0299(3) Uani 1 1 d . . . C9 C 0.29985(12) 0.19964(7) 0.73447(9) 0.0287(3) Uani 1 1 d . . . H9 H 0.3158 0.1966 0.7922 0.034 Uiso 1 1 calc R . . C10 C 0.38138(12) 0.21144(7) 0.70217(10) 0.0330(4) Uani 1 1 d . . . H10 H 0.4508 0.2171 0.7360 0.040 Uiso 1 1 calc R . . C11 C 0.35706(12) 0.21465(8) 0.61725(11) 0.0350(4) Uani 1 1 d . . . H11 H 0.4109 0.2217 0.5919 0.042 Uiso 1 1 calc R . . C12 C 0.25627(12) 0.20772(7) 0.57053(10) 0.0307(3) Uani 1 1 d . . . H12 H 0.2407 0.2096 0.5127 0.037 Uiso 1 1 calc R . . C13 C 0.17338(11) 0.19761(6) 0.60731(9) 0.0244(3) Uani 1 1 d . . . Si2 Si 0.01088(3) 0.20971(2) 0.46933(3) 0.02988(12) Uani 1 1 d . . . C14 C 0.04443(17) 0.15925(9) 0.39225(12) 0.0506(5) Uani 1 1 d . . . H14A H 0.1188 0.1637 0.3957 0.076 Uiso 1 1 calc R . . H14B H 0.0018 0.1701 0.3372 0.076 Uiso 1 1 calc R . . H14C H 0.0302 0.1176 0.4036 0.076 Uiso 1 1 calc R . . C15 C 0.03389(14) 0.28912(8) 0.44295(10) 0.0384(4) Uani 1 1 d . . . H15A H 0.0085 0.3164 0.4781 0.058 Uiso 1 1 calc R . . H15B H -0.0038 0.2968 0.3856 0.058 Uiso 1 1 calc R . . H15C H 0.1090 0.2956 0.4514 0.058 Uiso 1 1 calc R . . C16 C -0.13244(14) 0.20150(10) 0.45561(12) 0.0515(5) Uani 1 1 d . . . H16A H -0.1481 0.1600 0.4663 0.077 Uiso 1 1 calc R . . H16B H -0.1710 0.2122 0.3995 0.077 Uiso 1 1 calc R . . H16C H -0.1535 0.2280 0.4939 0.077 Uiso 1 1 calc R . . O1 O -0.01541(9) 0.06296(5) 0.66494(7) 0.0400(3) Uani 1 1 d . . . C17 C -0.01874(15) 0.03955(9) 0.58593(12) 0.0464(5) Uani 1 1 d . . . H17A H 0.0215 0.0018 0.5916 0.056 Uiso 1 1 calc R . . H17B H 0.0119 0.0686 0.5554 0.056 Uiso 1 1 calc R . . C18 C -0.13373(16) 0.02837(10) 0.54096(12) 0.0514(5) Uani 1 1 d . . . H18A H -0.1537 0.0486 0.4871 0.062 Uiso 1 1 calc R . . H18B H -0.1482 -0.0150 0.5328 0.062 Uiso 1 1 calc R . . C19 C -0.19202(14) 0.05513(9) 0.59756(11) 0.0424(4) Uani 1 1 d . . . H19A H -0.2098 0.0976 0.5843 0.051 Uiso 1 1 calc R . . H19B H -0.2569 0.0326 0.5948 0.051 Uiso 1 1 calc R . . C20 C -0.11348(14) 0.04869(8) 0.67956(11) 0.0409(4) Uani 1 1 d . . . H20A H -0.1289 0.0767 0.7196 0.049 Uiso 1 1 calc R . . H20B H -0.1130 0.0073 0.7004 0.049 Uiso 1 1 calc R . . Na2 Na -0.00271(5) 0.45494(3) 0.76784(4) 0.02902(15) Uani 1 1 d . . . O2 O -0.18228(9) 0.41535(5) 0.71805(7) 0.0408(3) Uani 1 1 d . . . O3 O -0.01457(10) 0.38273(6) 0.65694(8) 0.0453(3) Uani 1 1 d . . . O4 O 0.10843(9) 0.36924(5) 0.81933(8) 0.0402(3) Uani 1 1 d . . . O5 O -0.05942(9) 0.40143(5) 0.87976(7) 0.0352(3) Uani 1 1 d . . . C21 C -0.19631(16) 0.39329(9) 0.63605(11) 0.0501(5) Uani 1 1 d . . . H21A H -0.1984 0.4276 0.5989 0.060 Uiso 1 1 calc R . . H21B H -0.2643 0.3722 0.6175 0.060 Uiso 1 1 calc R . . C22 C -0.11045(17) 0.35148(10) 0.63078(12) 0.0530(5) Uani 1 1 d . . . H22A H -0.1091 0.3161 0.6660 0.064 Uiso 1 1 calc R . . H22B H -0.1222 0.3375 0.5738 0.064 Uiso 1 1 calc R . . C23 C 0.07627(17) 0.34482(9) 0.68004(13) 0.0528(5) Uani 1 1 d . . . H23A H 0.1384 0.3680 0.6771 0.063 Uiso 1 1 calc R . . H23B H 0.0671 0.3113 0.6407 0.063 Uiso 1 1 calc R . . C24 C 0.09500(17) 0.32011(9) 0.76450(13) 0.0506(5) Uani 1 1 d . . . H24A H 0.0346 0.2955 0.7679 0.061 Uiso 1 1 calc R . . H24B H 0.1584 0.2946 0.7786 0.061 Uiso 1 1 calc R . . C25 C 0.10258(14) 0.35320(9) 0.89885(11) 0.0433(4) Uani 1 1 d . . . H25A H 0.1377 0.3844 0.9382 0.052 Uiso 1 1 calc R . . H25B H 0.1407 0.3152 0.9155 0.052 Uiso 1 1 calc R . . C26 C -0.00806(15) 0.34603(8) 0.90259(12) 0.0419(4) Uani 1 1 d . . . H26A H -0.0438 0.3141 0.8647 0.050 Uiso 1 1 calc R . . H26B H -0.0088 0.3351 0.9586 0.050 Uiso 1 1 calc R . . C27 C -0.17146(13) 0.39706(8) 0.85497(11) 0.0389(4) Uani 1 1 d . . . H27A H -0.2016 0.4370 0.8592 0.047 Uiso 1 1 calc R . . H27B H -0.1936 0.3698 0.8927 0.047 Uiso 1 1 calc R . . C28 C -0.21387(14) 0.37441(9) 0.76937(12) 0.0457(5) Uani 1 1 d . . . H28A H -0.1857 0.3341 0.7642 0.055 Uiso 1 1 calc R . . H28B H -0.2912 0.3719 0.7544 0.055 Uiso 1 1 calc R . . O6 O -0.07668(9) 0.52525(5) 0.65581(7) 0.0353(3) Uani 1 1 d . . . O7 O 0.13734(9) 0.50030(5) 0.71679(7) 0.0384(3) Uani 1 1 d . . . O8 O 0.12456(9) 0.51275(5) 0.87696(7) 0.0370(3) Uani 1 1 d . . . O9 O -0.09034(9) 0.53734(5) 0.81596(7) 0.0352(3) Uani 1 1 d . . . C29 C -0.00500(15) 0.53334(8) 0.60840(10) 0.0407(4) Uani 1 1 d . . . H29A H -0.0305 0.5659 0.5684 0.049 Uiso 1 1 calc R . . H29B H -0.0021 0.4962 0.5775 0.049 Uiso 1 1 calc R . . C30 C 0.10323(14) 0.54840(8) 0.66084(11) 0.0417(4) Uani 1 1 d . . . H30A H 0.1514 0.5534 0.6265 0.050 Uiso 1 1 calc R . . H30B H 0.1020 0.5862 0.6909 0.050 Uiso 1 1 calc R . . C31 C 0.22613(13) 0.51433(9) 0.78387(12) 0.0428(4) Uani 1 1 d . . . H31A H 0.2766 0.5381 0.7639 0.051 Uiso 1 1 calc R . . H31B H 0.2613 0.4768 0.8077 0.051 Uiso 1 1 calc R . . C32 C 0.19533(13) 0.54909(8) 0.84898(11) 0.0384(4) Uani 1 1 d . . . H32A H 0.2580 0.5585 0.8947 0.046 Uiso 1 1 calc R . . H32B H 0.1612 0.5871 0.8263 0.046 Uiso 1 1 calc R . . C33 C 0.06798(16) 0.54439(9) 0.92265(11) 0.0450(5) Uani 1 1 d . . . H33A H 0.1159 0.5725 0.9602 0.054 Uiso 1 1 calc R . . H33B H 0.0414 0.5157 0.9562 0.054 Uiso 1 1 calc R . . C34 C -0.02301(15) 0.57903(8) 0.86877(12) 0.0441(4) Uani 1 1 d . . . H34A H -0.0612 0.6001 0.9026 0.053 Uiso 1 1 calc R . . H34B H 0.0025 0.6091 0.8364 0.053 Uiso 1 1 calc R . . C35 C -0.16374(13) 0.56441(8) 0.74753(11) 0.0388(4) Uani 1 1 d . . . H35A H -0.1916 0.6014 0.7656 0.047 Uiso 1 1 calc R . . H35B H -0.2232 0.5367 0.7260 0.047 Uiso 1 1 calc R . . C36 C -0.11507(15) 0.57962(8) 0.68017(12) 0.0414(4) Uani 1 1 d . . . H36A H -0.1679 0.5978 0.6334 0.050 Uiso 1 1 calc R . . H36B H -0.0570 0.6085 0.7001 0.050 Uiso 1 1 calc R . . O10 O 0.2892(19) 0.3865(18) 0.5603(13) 0.48(3) Uani 0.508(11) 1 d P A 1 C37 C 0.4074(12) 0.3843(6) 0.6405(6) 0.117(4) Uani 0.508(11) 1 d P A 1 H37A H 0.4136 0.3470 0.6727 0.140 Uiso 0.508(11) 1 calc PR A 1 H37B H 0.4693 0.3884 0.6196 0.140 Uiso 0.508(11) 1 calc PR A 1 C38 C 0.3951(9) 0.4346(5) 0.6864(8) 0.117(4) Uani 0.508(11) 1 d P A 1 H38A H 0.3690 0.4219 0.7327 0.141 Uiso 0.508(11) 1 calc PR A 1 H38B H 0.4635 0.4546 0.7089 0.141 Uiso 0.508(11) 1 calc PR A 1 C39 C 0.3259(7) 0.4734(3) 0.6379(5) 0.073(2) Uani 0.508(11) 1 d P A 1 H39A H 0.2775 0.4885 0.6680 0.087 Uiso 0.508(11) 1 calc PR A 1 H39B H 0.3645 0.5079 0.6246 0.087 Uiso 0.508(11) 1 calc PR A 1 C40 C 0.2709(11) 0.4473(7) 0.5690(6) 0.086(5) Uani 0.508(11) 1 d P A 1 H40A H 0.2851 0.4689 0.5227 0.103 Uiso 0.508(11) 1 calc PR A 1 H40B H 0.1956 0.4525 0.5644 0.103 Uiso 0.508(11) 1 calc PR A 1 O10A O 0.3008(5) 0.3690(2) 0.5780(3) 0.085(2) Uani 0.492(11) 1 d P A 2 C37A C 0.3622(7) 0.3784(4) 0.6607(5) 0.073(2) Uani 0.492(11) 1 d P A 2 H37C H 0.4200 0.3492 0.6790 0.088 Uiso 0.492(11) 1 calc PR A 2 H37D H 0.3194 0.3794 0.6997 0.088 Uiso 0.492(11) 1 calc PR A 2 C38A C 0.4017(13) 0.4431(7) 0.6431(8) 0.138(6) Uani 0.492(11) 1 d P A 2 H38C H 0.4176 0.4688 0.6923 0.166 Uiso 0.492(11) 1 calc PR A 2 H38D H 0.4641 0.4406 0.6227 0.166 Uiso 0.492(11) 1 calc PR A 2 C39A C 0.3161(18) 0.4628(8) 0.5844(17) 0.162(12) Uani 0.492(11) 1 d P A 2 H39C H 0.3397 0.4874 0.5446 0.194 Uiso 0.492(11) 1 calc PR A 2 H39D H 0.2744 0.4889 0.6101 0.194 Uiso 0.492(11) 1 calc PR A 2 C40A C 0.2440(6) 0.4112(4) 0.5372(7) 0.079(2) Uani 0.492(11) 1 d P A 2 H40C H 0.1728 0.4123 0.5443 0.095 Uiso 0.492(11) 1 calc PR A 2 H40D H 0.2400 0.4102 0.4783 0.095 Uiso 0.492(11) 1 calc PR A 2 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 Na1 0.0247(3) 0.0351(3) 0.0253(3) -0.0003(2) 0.0108(2) -0.0012(2) N1 0.0251(7) 0.0325(7) 0.0248(7) 0.0028(5) 0.0068(5) 0.0013(5) N2 0.0228(6) 0.0368(7) 0.0228(6) 0.0008(5) 0.0067(5) 0.0018(5) C1 0.0267(8) 0.0322(9) 0.0292(8) 0.0052(6) 0.0026(6) -0.0010(6) C2 0.0203(7) 0.0315(9) 0.0419(9) 0.0047(7) 0.0043(7) -0.0011(6) C3 0.0249(8) 0.0312(9) 0.0424(9) -0.0019(7) 0.0163(7) -0.0025(6) C4 0.0274(8) 0.0296(8) 0.0271(8) -0.0013(6) 0.0110(6) -0.0029(6) C5 0.0238(7) 0.0223(7) 0.0252(7) -0.0008(6) 0.0084(6) -0.0033(6) Si1 0.0280(2) 0.0335(2) 0.0223(2) -0.00009(17) 0.00603(17) 0.00351(18) C6 0.0449(10) 0.0492(11) 0.0264(8) -0.0056(8) 0.0029(7) 0.0057(8) C7 0.0667(13) 0.0409(11) 0.0435(11) 0.0059(9) 0.0124(10) -0.0046(9) C8 0.0350(10) 0.0752(14) 0.0366(10) 0.0065(9) 0.0074(8) 0.0181(9) N3 0.0229(6) 0.0308(7) 0.0240(6) 0.0005(5) 0.0067(5) 0.0028(5) N4 0.0235(7) 0.0409(8) 0.0254(7) 0.0061(6) 0.0073(5) -0.0018(6) C9 0.0279(8) 0.0300(8) 0.0267(8) -0.0013(6) 0.0054(6) 0.0031(6) C10 0.0214(8) 0.0351(9) 0.0396(9) 0.0028(7) 0.0038(7) -0.0009(6) C11 0.0254(8) 0.0395(10) 0.0432(10) 0.0108(7) 0.0148(7) 0.0003(7) C12 0.0283(8) 0.0379(9) 0.0277(8) 0.0079(7) 0.0109(7) 0.0009(7) C13 0.0248(7) 0.0229(8) 0.0264(8) 0.0033(6) 0.0090(6) 0.0017(6) Si2 0.0253(2) 0.0397(3) 0.0234(2) 0.00421(18) 0.00480(17) -0.00370(18) C14 0.0651(13) 0.0498(12) 0.0361(10) -0.0065(9) 0.0128(9) -0.0050(10) C15 0.0398(10) 0.0436(10) 0.0303(9) 0.0071(7) 0.0079(7) -0.0005(8) C16 0.0288(9) 0.0742(15) 0.0453(11) 0.0171(10) 0.0005(8) -0.0068(9) O1 0.0381(7) 0.0431(7) 0.0423(7) -0.0082(5) 0.0172(5) -0.0051(5) C17 0.0513(11) 0.0463(11) 0.0495(11) -0.0135(9) 0.0271(9) -0.0012(9) C18 0.0584(12) 0.0515(12) 0.0444(11) -0.0130(9) 0.0149(9) -0.0001(10) C19 0.0393(10) 0.0424(10) 0.0476(11) -0.0050(8) 0.0155(8) -0.0054(8) C20 0.0454(10) 0.0396(10) 0.0432(10) -0.0026(8) 0.0215(8) -0.0099(8) Na2 0.0309(3) 0.0236(3) 0.0344(3) -0.0017(2) 0.0123(3) -0.0033(2) O2 0.0391(7) 0.0355(7) 0.0447(7) 0.0007(5) 0.0070(5) -0.0082(5) O3 0.0571(8) 0.0373(7) 0.0439(7) -0.0057(6) 0.0182(6) -0.0100(6) O4 0.0392(7) 0.0338(7) 0.0500(7) -0.0042(5) 0.0166(6) 0.0016(5) O5 0.0354(6) 0.0300(6) 0.0412(7) -0.0016(5) 0.0127(5) -0.0012(5) C21 0.0542(12) 0.0527(12) 0.0338(10) -0.0028(8) -0.0030(8) -0.0173(10) C22 0.0680(14) 0.0497(12) 0.0398(11) -0.0130(9) 0.0125(10) -0.0204(10) C23 0.0632(13) 0.0451(12) 0.0616(13) -0.0115(10) 0.0364(11) 0.0034(10) C24 0.0558(12) 0.0354(10) 0.0645(13) -0.0088(9) 0.0233(10) 0.0087(9) C25 0.0351(9) 0.0453(11) 0.0456(11) 0.0074(8) 0.0051(8) 0.0053(8) C26 0.0483(11) 0.0351(10) 0.0430(10) 0.0036(8) 0.0143(8) 0.0029(8) C27 0.0327(9) 0.0401(10) 0.0493(11) 0.0005(8) 0.0205(8) -0.0035(7) C28 0.0329(9) 0.0463(11) 0.0561(12) 0.0054(9) 0.0098(8) -0.0099(8) O6 0.0386(6) 0.0312(6) 0.0386(6) 0.0007(5) 0.0149(5) -0.0032(5) O7 0.0373(6) 0.0361(7) 0.0447(7) -0.0011(5) 0.0164(5) -0.0033(5) O8 0.0398(7) 0.0337(6) 0.0381(6) 0.0024(5) 0.0120(5) -0.0057(5) O9 0.0392(6) 0.0275(6) 0.0434(7) -0.0022(5) 0.0192(5) -0.0026(5) C29 0.0539(11) 0.0422(10) 0.0307(9) 0.0005(7) 0.0197(8) -0.0060(8) C30 0.0479(11) 0.0423(10) 0.0433(10) 0.0039(8) 0.0266(9) -0.0069(8) C31 0.0296(9) 0.0446(11) 0.0556(11) -0.0004(9) 0.0141(8) -0.0027(8) C32 0.0331(9) 0.0372(10) 0.0419(10) 0.0019(7) 0.0058(7) -0.0085(7) C33 0.0569(12) 0.0485(11) 0.0328(9) -0.0072(8) 0.0180(9) -0.0127(9) C34 0.0518(11) 0.0362(10) 0.0529(11) -0.0148(8) 0.0289(9) -0.0075(8) C35 0.0337(9) 0.0305(9) 0.0558(11) 0.0035(8) 0.0188(8) 0.0047(7) C36 0.0445(10) 0.0298(9) 0.0513(11) 0.0061(8) 0.0158(9) 0.0051(8) O10 0.29(2) 0.83(7) 0.25(2) 0.06(3) -0.055(16) -0.22(3) C37 0.173(12) 0.100(7) 0.085(6) -0.011(5) 0.047(6) 0.024(8) C38 0.105(6) 0.107(7) 0.133(9) -0.039(7) 0.024(6) 0.025(5) C39 0.077(4) 0.060(4) 0.089(5) -0.021(3) 0.037(4) 0.012(3) C40 0.091(8) 0.113(12) 0.062(4) -0.006(5) 0.033(4) 0.054(9) O10A 0.105(4) 0.090(3) 0.062(3) -0.013(2) 0.025(3) 0.036(3) C37A 0.075(5) 0.076(5) 0.068(5) 0.003(3) 0.018(3) -0.011(3) C38A 0.182(13) 0.132(11) 0.126(10) -0.057(9) 0.083(10) -0.101(10) C39A 0.18(2) 0.065(6) 0.30(3) -0.011(12) 0.16(2) 0.007(10) C40A 0.072(4) 0.056(4) 0.090(5) 0.008(4) -0.007(4) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 N2 2.3987(13) . ? Na1 N4 2.4099(13) . ? Na1 O1 2.4170(14) . ? Na1 N3 2.4606(13) . ? Na1 N1 2.5352(13) . ? N1 C1 1.337(2) . ? N1 C5 1.3775(19) . ? N2 C5 1.3281(19) . ? N2 Si1 1.6873(13) . ? C1 C2 1.373(2) . ? C2 C3 1.392(2) . ? C3 C4 1.367(2) . ? C4 C5 1.435(2) . ? Si1 C8 1.8664(18) . ? Si1 C7 1.873(2) . ? Si1 C6 1.8793(17) . ? N3 C9 1.334(2) . ? N3 C13 1.3798(19) . ? N4 C13 1.3298(19) . ? N4 Si2 1.6897(13) . ? C9 C10 1.375(2) . ? C10 C11 1.394(2) . ? C11 C12 1.362(2) . ? C12 C13 1.434(2) . ? Si2 C16 1.8648(18) . ? Si2 C15 1.8777(18) . ? Si2 C14 1.8802(19) . ? O1 C20 1.433(2) . ? O1 C17 1.435(2) . ? C17 C18 1.526(3) . ? C18 C19 1.523(3) . ? C19 C20 1.498(3) . ? Na2 O4 2.4281(13) . ? Na2 O9 2.4437(12) . ? Na2 O6 2.4553(13) . ? Na2 O3 2.4583(13) . ? Na2 O2 2.4641(13) . ? Na2 O7 2.4871(13) . ? Na2 O8 2.4943(13) . ? Na2 O5 2.5430(13) . ? O2 C28 1.411(2) . ? O2 C21 1.445(2) . ? O3 C22 1.412(2) . ? O3 C23 1.438(2) . ? O4 C24 1.421(2) . ? O4 C25 1.427(2) . ? O5 C26 1.415(2) . ? O5 C27 1.434(2) . ? C21 C22 1.499(3) . ? C23 C24 1.497(3) . ? C25 C26 1.501(3) . ? C27 C28 1.497(3) . ? O6 C36 1.425(2) . ? O6 C29 1.427(2) . ? O7 C30 1.424(2) . ? O7 C31 1.428(2) . ? O8 C33 1.417(2) . ? O8 C32 1.425(2) . ? O9 C34 1.423(2) . ? O9 C35 1.428(2) . ? C29 C30 1.503(3) . ? C31 C32 1.505(3) . ? C33 C34 1.511(3) . ? C35 C36 1.510(2) . ? O10 C40 1.40(4) . ? O10 C37 1.77(2) . ? C37 C38 1.406(15) . ? C38 C39 1.361(15) . ? C39 C40 1.331(18) . ? O10A C40A 1.286(9) . ? O10A C37A 1.432(10) . ? C37A C38A 1.595(16) . ? C38A C39A 1.36(2) . ? C39A C40A 1.57(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 N2 Na1 N4 161.42(5) . . ? N2 Na1 O1 98.65(5) . . ? N4 Na1 O1 99.84(5) . . ? N2 Na1 N3 117.83(5) . . ? N4 Na1 N3 56.45(4) . . ? O1 Na1 N3 110.45(5) . . ? N2 Na1 N1 55.42(4) . . ? N4 Na1 N1 118.84(5) . . ? O1 Na1 N1 100.26(5) . . ? N3 Na1 N1 149.29(5) . . ? C1 N1 C5 119.10(13) . . ? C1 N1 Na1 150.24(11) . . ? C5 N1 Na1 90.47(8) . . ? C5 N2 Si1 130.83(10) . . ? C5 N2 Na1 97.80(9) . . ? Si1 N2 Na1 127.61(7) . . ? N1 C1 C2 125.32(15) . . ? C1 C2 C3 116.89(14) . . ? C4 C3 C2 120.00(14) . . ? C3 C4 C5 120.94(14) . . ? N2 C5 N1 116.22(12) . . ? N2 C5 C4 126.04(14) . . ? N1 C5 C4 117.73(13) . . ? N2 Si1 C8 106.09(7) . . ? N2 Si1 C7 112.11(8) . . ? C8 Si1 C7 109.35(10) . . ? N2 Si1 C6 115.61(8) . . ? C8 Si1 C6 106.92(9) . . ? C7 Si1 C6 106.56(9) . . ? C9 N3 C13 119.19(13) . . ? C9 N3 Na1 149.14(10) . . ? C13 N3 Na1 91.66(8) . . ? C13 N4 Si2 128.37(11) . . ? C13 N4 Na1 95.18(9) . . ? Si2 N4 Na1 135.89(7) . . ? N3 C9 C10 125.24(15) . . ? C9 C10 C11 116.69(14) . . ? C12 C11 C10 120.19(14) . . ? C11 C12 C13 120.98(15) . . ? N4 C13 N3 116.48(13) . . ? N4 C13 C12 125.92(14) . . ? N3 C13 C12 117.60(13) . . ? N4 Si2 C16 106.93(8) . . ? N4 Si2 C15 112.49(7) . . ? C16 Si2 C15 107.07(9) . . ? N4 Si2 C14 114.83(8) . . ? C16 Si2 C14 106.90(10) . . ? C15 Si2 C14 108.19(9) . . ? C20 O1 C17 107.17(13) . . ? C20 O1 Na1 109.11(10) . . ? C17 O1 Na1 117.49(11) . . ? O1 C17 C18 106.96(14) . . ? C19 C18 C17 103.64(15) . . ? C20 C19 C18 102.03(15) . . ? O1 C20 C19 104.21(14) . . ? O4 Na2 O9 140.64(5) . . ? O4 Na2 O6 148.85(5) . . ? O9 Na2 O6 69.81(4) . . ? O4 Na2 O3 70.13(5) . . ? O9 Na2 O3 145.19(5) . . ? O6 Na2 O3 84.08(4) . . ? O4 Na2 O2 105.89(5) . . ? O9 Na2 O2 82.97(4) . . ? O6 Na2 O2 79.95(4) . . ? O3 Na2 O2 69.77(5) . . ? O4 Na2 O7 90.45(4) . . ? O9 Na2 O7 106.70(4) . . ? O6 Na2 O7 68.99(4) . . ? O3 Na2 O7 83.63(4) . . ? O2 Na2 O7 140.93(5) . . ? O4 Na2 O8 85.58(4) . . ? O9 Na2 O8 69.31(4) . . ? O6 Na2 O8 106.71(4) . . ? O3 Na2 O8 142.83(5) . . ? O2 Na2 O8 146.22(5) . . ? O7 Na2 O8 68.41(4) . . ? O4 Na2 O5 68.73(4) . . ? O9 Na2 O5 80.24(4) . . ? O6 Na2 O5 138.33(4) . . ? O3 Na2 O5 107.54(4) . . ? O2 Na2 O5 67.94(4) . . ? O7 Na2 O5 150.06(5) . . ? O8 Na2 O5 88.08(4) . . ? C28 O2 C21 113.61(14) . . ? C28 O2 Na2 116.74(10) . . ? C21 O2 Na2 107.64(10) . . ? C22 O3 C23 114.22(15) . . ? C22 O3 Na2 115.05(11) . . ? C23 O3 Na2 108.09(11) . . ? C24 O4 C25 113.68(14) . . ? C24 O4 Na2 114.92(11) . . ? C25 O4 Na2 110.52(10) . . ? C26 O5 C27 113.77(13) . . ? C26 O5 Na2 113.28(10) . . ? C27 O5 Na2 108.42(9) . . ? O2 C21 C22 112.29(15) . . ? O3 C22 C21 108.01(16) . . ? O3 C23 C24 112.28(15) . . ? O4 C24 C23 107.73(16) . . ? O4 C25 C26 112.70(14) . . ? O5 C26 C25 107.37(14) . . ? O5 C27 C28 112.59(14) . . ? O2 C28 C27 106.86(14) . . ? C36 O6 C29 114.22(13) . . ? C36 O6 Na2 114.62(10) . . ? C29 O6 Na2 109.72(10) . . ? C30 O7 C31 113.95(13) . . ? C30 O7 Na2 114.47(10) . . ? C31 O7 Na2 109.96(10) . . ? C33 O8 C32 113.89(13) . . ? C33 O8 Na2 108.34(10) . . ? C32 O8 Na2 114.77(10) . . ? C34 O9 C35 113.76(13) . . ? C34 O9 Na2 115.53(10) . . ? C35 O9 Na2 109.02(9) . . ? O6 C29 C30 111.91(14) . . ? O7 C30 C29 107.45(14) . . ? O7 C31 C32 111.61(14) . . ? O8 C32 C31 107.31(14) . . ? O8 C33 C34 112.37(14) . . ? O9 C34 C33 107.61(15) . . ? O9 C35 C36 112.10(14) . . ? O6 C36 C35 107.27(14) . . ? C40 O10 C37 95.0(17) . . ? C38 C37 O10 101.0(15) . . ? C39 C38 C37 109.6(9) . . ? C40 C39 C38 111.5(8) . . ? C39 C40 O10 116.9(12) . . ? C40A O10A C37A 120.7(7) . . ? O10A C37A C38A 94.3(8) . . ? C39A C38A C37A 100.4(11) . . ? C38A C39A C40A 113.8(14) . . ? O10A C40A C39A 94.6(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.391 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.036 #===END data_4 _database_code_CSD 152064 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H74 K2 N4 O8 Si2' _chemical_formula_weight 945.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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 10.5289(7) _cell_length_b 11.6308(8) _cell_length_c 11.9792(8) _cell_angle_alpha 71.065(2) _cell_angle_beta 88.749(2) _cell_angle_gamma 72.796(2) _cell_volume 1321.03(15) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 9231 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.59 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.54 _exptl_crystal_size_min 0.52 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 0.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.590 _exptl_absorpt_correction_T_max 0.888 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11488 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 28.59 _reflns_number_total 6034 _reflns_number_gt 4086 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0892P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.002(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6034 _refine_ls_number_parameters 285 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0717 _refine_ls_R_factor_gt 0.0564 _refine_ls_wR_factor_ref 0.1547 _refine_ls_wR_factor_gt 0.1484 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.980 _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 K1 K 0.59113(5) 0.56218(5) 0.56475(5) 0.02891(16) Uani 1 1 d . . . N1 N 0.68630(19) 0.32989(18) 0.51317(17) 0.0286(4) Uani 1 1 d . . . N2 N 0.55271(19) 0.31762(18) 0.66894(17) 0.0295(4) Uani 1 1 d . . . C1 C 0.7845(2) 0.2739(2) 0.4571(2) 0.0337(6) Uani 1 1 d . . . H1 H 0.8052 0.3261 0.3843 0.040 Uiso 1 1 calc R . . C2 C 0.8577(2) 0.1464(2) 0.4970(2) 0.0381(6) Uani 1 1 d . . . H2 H 0.9259 0.1115 0.4534 0.046 Uiso 1 1 calc R . . C3 C 0.8274(3) 0.0717(2) 0.6035(2) 0.0376(6) Uani 1 1 d . . . H3 H 0.8762 -0.0164 0.6349 0.045 Uiso 1 1 calc R . . C4 C 0.7273(3) 0.1240(2) 0.6641(2) 0.0343(6) Uani 1 1 d . . . H4 H 0.7071 0.0717 0.7371 0.041 Uiso 1 1 calc R . . C5 C 0.6531(2) 0.2568(2) 0.6184(2) 0.0268(5) Uani 1 1 d . . . Si1 Si 0.47877(7) 0.25322(6) 0.79011(6) 0.0341(2) Uani 1 1 d . . . C6 C 0.5873(3) 0.1799(3) 0.9328(2) 0.0549(8) Uani 1 1 d . . . H6A H 0.6598 0.1057 0.9293 0.082 Uiso 1 1 calc R . . H6B H 0.5339 0.1527 0.9985 0.082 Uiso 1 1 calc R . . H6C H 0.6250 0.2428 0.9452 0.082 Uiso 1 1 calc R . . C7 C 0.4106(4) 0.1256(3) 0.7786(3) 0.0643(9) Uani 1 1 d . . . H7A H 0.3658 0.1522 0.6995 0.096 Uiso 1 1 calc R . . H7B H 0.3465 0.1117 0.8383 0.096 Uiso 1 1 calc R . . H7C H 0.4838 0.0462 0.7922 0.096 Uiso 1 1 calc R . . C8 C 0.3359(3) 0.3865(3) 0.8058(3) 0.0507(8) Uani 1 1 d . . . H8A H 0.3680 0.4574 0.8060 0.076 Uiso 1 1 calc R . . H8B H 0.2963 0.3563 0.8803 0.076 Uiso 1 1 calc R . . H8C H 0.2685 0.4156 0.7393 0.076 Uiso 1 1 calc R . . O1 O 0.7575(3) 0.5279(3) 0.8026(3) 0.0795(8) Uani 1 1 d . . . O2 O 0.8628(2) 0.5291(4) 0.5864(3) 0.0997(11) Uani 1 1 d . . . O3 O 0.6705(3) 0.7740(2) 0.5569(2) 0.0728(7) Uani 1 1 d . . . O4 O 0.4969(2) 0.6892(2) 0.72833(19) 0.0554(6) Uani 1 1 d . . . C9 C 0.8365(5) 0.4153(5) 0.7890(5) 0.1158(19) Uani 1 1 d U . . H9A H 0.7811 0.3730 0.7612 0.139 Uiso 1 1 calc R . . H9B H 0.8864 0.3560 0.8650 0.139 Uiso 1 1 calc R . . C10 C 0.9299(4) 0.4523(7) 0.6996(5) 0.150(3) Uani 1 1 d U . . H10A H 0.9796 0.4999 0.7266 0.180 Uiso 1 1 calc R . . H10B H 0.9954 0.3742 0.6931 0.180 Uiso 1 1 calc R . . C11 C 0.8726(6) 0.6602(7) 0.5166(6) 0.154(2) Uani 1 1 d U . . H11A H 0.9683 0.6545 0.5145 0.184 Uiso 1 1 calc R . . H11B H 0.8368 0.6823 0.4341 0.184 Uiso 1 1 calc R . . C12 C 0.8082(6) 0.7603(7) 0.5565(6) 0.149(2) Uani 1 1 d U . . H12A H 0.8223 0.8402 0.5040 0.178 Uiso 1 1 calc R . . H12B H 0.8455 0.7430 0.6375 0.178 Uiso 1 1 calc R . . C13 C 0.6120(5) 0.8425(4) 0.6335(4) 0.0810(12) Uani 1 1 d U . . H13A H 0.5977 0.9349 0.5936 0.097 Uiso 1 1 calc R . . H13B H 0.6721 0.8138 0.7062 0.097 Uiso 1 1 calc R . . C14 C 0.4850(4) 0.8196(3) 0.6641(4) 0.0771(11) Uani 1 1 d U . . H14A H 0.4408 0.8728 0.7122 0.093 Uiso 1 1 calc R . . H14B H 0.4270 0.8474 0.5903 0.093 Uiso 1 1 calc R . . C15 C 0.5523(4) 0.6419(4) 0.8458(3) 0.0701(10) Uani 1 1 d U . . H15A H 0.4807 0.6365 0.9005 0.084 Uiso 1 1 calc R . . H15B H 0.5970 0.7006 0.8593 0.084 Uiso 1 1 calc R . . C16 C 0.6466(4) 0.5182(4) 0.8690(3) 0.0695(10) Uani 1 1 d U . . H16A H 0.6763 0.4801 0.9545 0.083 Uiso 1 1 calc R . . H16B H 0.6043 0.4619 0.8476 0.083 Uiso 1 1 calc R . . C17 C 1.0638(3) -0.1226(3) 0.8535(2) 0.0455(7) Uani 1 1 d . . . C18 C 0.9465(3) -0.1030(3) 0.9102(3) 0.0476(7) Uani 1 1 d . . . H18 H 0.9095 -0.0248 0.9250 0.057 Uiso 1 1 calc R . . C19 C 0.8834(3) -0.1956(3) 0.9452(3) 0.0535(8) Uani 1 1 d . . . H19 H 0.8025 -0.1804 0.9825 0.064 Uiso 1 1 calc R . . C20 C 0.9372(3) -0.3102(3) 0.9262(3) 0.0569(8) Uani 1 1 d . . . H20 H 0.8935 -0.3741 0.9499 0.068 Uiso 1 1 calc R . . C21 C 1.0551(3) -0.3316(3) 0.8725(3) 0.0561(8) Uani 1 1 d . . . H21 H 1.0935 -0.4109 0.8601 0.067 Uiso 1 1 calc R . . C22 C 1.1170(3) -0.2386(3) 0.8370(3) 0.0511(8) Uani 1 1 d . . . H22 H 1.1982 -0.2546 0.8002 0.061 Uiso 1 1 calc R . . C23 C 1.1275(4) -0.0180(4) 0.8083(3) 0.0757(11) Uani 1 1 d . . . H23A H 1.2195 -0.0486 0.8436 0.114 Uiso 1 1 calc R . . H23B H 1.0770 0.0561 0.8300 0.114 Uiso 1 1 calc R . . H23C H 1.1275 0.0066 0.7220 0.114 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 K1 0.0223(3) 0.0314(3) 0.0347(3) -0.0141(2) 0.0011(2) -0.0072(2) N1 0.0233(10) 0.0286(10) 0.0302(10) -0.0093(8) 0.0046(8) -0.0034(8) N2 0.0264(10) 0.0260(10) 0.0321(11) -0.0088(8) 0.0075(8) -0.0037(8) C1 0.0229(12) 0.0390(13) 0.0380(14) -0.0143(11) 0.0084(10) -0.0064(10) C2 0.0246(13) 0.0408(14) 0.0464(16) -0.0204(12) 0.0070(11) 0.0001(11) C3 0.0311(14) 0.0283(12) 0.0446(15) -0.0131(11) -0.0018(11) 0.0050(10) C4 0.0359(14) 0.0271(12) 0.0324(13) -0.0069(10) 0.0037(11) -0.0023(10) C5 0.0232(11) 0.0273(11) 0.0288(12) -0.0106(10) 0.0001(9) -0.0044(9) Si1 0.0366(4) 0.0284(4) 0.0341(4) -0.0081(3) 0.0130(3) -0.0085(3) C6 0.071(2) 0.0465(17) 0.0321(15) -0.0070(13) 0.0092(14) -0.0031(16) C7 0.079(2) 0.060(2) 0.066(2) -0.0192(17) 0.0251(19) -0.0424(19) C8 0.0419(17) 0.0462(16) 0.0567(19) -0.0139(14) 0.0249(14) -0.0079(13) O1 0.0561(16) 0.0889(19) 0.107(2) -0.0567(17) -0.0008(15) -0.0140(14) O2 0.0347(13) 0.169(3) 0.148(3) -0.116(3) 0.0278(16) -0.0385(17) O3 0.0720(17) 0.0796(17) 0.0763(17) -0.0140(14) 0.0089(14) -0.0502(14) O4 0.0621(14) 0.0554(13) 0.0587(14) -0.0334(11) 0.0114(11) -0.0169(11) C9 0.091(3) 0.116(4) 0.121(4) -0.075(3) -0.053(3) 0.041(3) C10 0.038(2) 0.260(6) 0.161(5) -0.152(5) -0.035(3) 0.037(3) C11 0.109(4) 0.263(7) 0.216(6) -0.173(5) 0.110(4) -0.144(5) C12 0.120(4) 0.237(7) 0.186(5) -0.121(5) 0.089(4) -0.144(5) C13 0.104(3) 0.051(2) 0.099(3) -0.031(2) -0.007(2) -0.033(2) C14 0.075(3) 0.054(2) 0.114(3) -0.050(2) -0.001(2) -0.0127(18) C15 0.071(2) 0.099(3) 0.0500(19) -0.0360(19) 0.0142(17) -0.028(2) C16 0.079(3) 0.079(2) 0.053(2) -0.0103(18) -0.0031(18) -0.039(2) C17 0.0399(16) 0.0591(18) 0.0353(15) -0.0077(13) -0.0046(12) -0.0201(14) C18 0.0427(17) 0.0464(16) 0.0465(17) -0.0125(14) 0.0007(13) -0.0063(13) C19 0.0343(16) 0.063(2) 0.0552(19) -0.0124(16) 0.0080(14) -0.0113(14) C20 0.055(2) 0.0542(19) 0.059(2) -0.0079(16) -0.0033(16) -0.0254(16) C21 0.057(2) 0.0524(19) 0.057(2) -0.0249(16) -0.0029(16) -0.0068(16) C22 0.0367(16) 0.074(2) 0.0384(16) -0.0208(15) 0.0029(12) -0.0086(15) C23 0.072(3) 0.100(3) 0.066(2) -0.017(2) 0.0062(19) -0.053(2) _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 K1 O2 2.778(2) . ? K1 O3 2.800(2) . ? K1 O4 2.816(2) . ? K1 N1 2.853(2) . ? K1 N2 2.858(2) . ? K1 N1 2.858(2) 2_666 ? K1 N2 2.912(2) 2_666 ? K1 O1 3.227(3) . ? N1 C1 1.342(3) . ? N1 C5 1.376(3) . ? N1 K1 2.858(2) 2_666 ? N2 C5 1.339(3) . ? N2 Si1 1.692(2) . ? N2 K1 2.912(2) 2_666 ? C1 C2 1.379(3) . ? C2 C3 1.382(4) . ? C3 C4 1.372(3) . ? C4 C5 1.433(3) . ? Si1 C8 1.870(3) . ? Si1 C7 1.872(3) . ? Si1 C6 1.876(3) . ? O1 C9 1.386(5) . ? O1 C16 1.409(4) . ? O2 C10 1.421(6) . ? O2 C11 1.516(7) . ? O3 C12 1.412(5) . ? O3 C13 1.420(5) . ? O4 C15 1.402(4) . ? O4 C14 1.430(4) . ? C9 C10 1.484(8) . ? C11 C12 1.386(8) . ? C13 C14 1.455(6) . ? C15 C16 1.428(5) . ? C17 C22 1.377(4) . ? C17 C18 1.391(4) . ? C17 C23 1.504(4) . ? C18 C19 1.377(4) . ? C19 C20 1.376(5) . ? C20 C21 1.380(5) . ? C21 C22 1.372(4) . ? 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 O2 K1 O3 62.22(9) . . ? O2 K1 O4 101.36(7) . . ? O3 K1 O4 60.98(7) . . ? O2 K1 N1 81.56(8) . . ? O3 K1 N1 140.04(7) . . ? O4 K1 N1 149.48(6) . . ? O2 K1 N2 107.74(9) . . ? O3 K1 N2 156.76(7) . . ? O4 K1 N2 104.02(6) . . ? N1 K1 N2 47.60(5) . . ? O2 K1 N1 161.74(10) . 2_666 ? O3 K1 N1 103.54(7) . 2_666 ? O4 K1 N1 79.07(6) . 2_666 ? N1 K1 N1 107.48(5) . 2_666 ? N2 K1 N1 89.64(6) . 2_666 ? O2 K1 N2 119.29(9) . 2_666 ? O3 K1 N2 94.53(7) . 2_666 ? O4 K1 N2 114.85(6) . 2_666 ? N1 K1 N2 88.67(6) . 2_666 ? N2 K1 N2 108.34(5) . 2_666 ? N1 K1 N2 47.08(5) 2_666 2_666 ? O2 K1 O1 54.83(8) . . ? O3 K1 O1 65.64(8) . . ? O4 K1 O1 54.61(7) . . ? N1 K1 O1 107.87(6) . . ? N2 K1 O1 91.31(7) . . ? N1 K1 O1 132.38(6) 2_666 . ? N2 K1 O1 160.03(7) 2_666 . ? C1 N1 C5 118.98(19) . . ? C1 N1 K1 138.85(16) . . ? C5 N1 K1 94.26(13) . . ? C1 N1 K1 127.23(16) . 2_666 ? C5 N1 K1 88.83(13) . 2_666 ? K1 N1 K1 72.52(5) . 2_666 ? C5 N2 Si1 127.71(16) . . ? C5 N2 K1 94.95(14) . . ? Si1 N2 K1 133.43(10) . . ? C5 N2 K1 87.30(13) . 2_666 ? Si1 N2 K1 121.57(10) . 2_666 ? K1 N2 K1 71.66(5) . 2_666 ? N1 C1 C2 125.0(2) . . ? C1 C2 C3 116.9(2) . . ? C4 C3 C2 120.4(2) . . ? C3 C4 C5 120.6(2) . . ? N2 C5 N1 116.19(19) . . ? N2 C5 C4 125.7(2) . . ? N1 C5 C4 118.1(2) . . ? N2 Si1 C8 106.38(11) . . ? N2 Si1 C7 113.95(13) . . ? C8 Si1 C7 107.84(16) . . ? N2 Si1 C6 115.44(13) . . ? C8 Si1 C6 107.60(14) . . ? C7 Si1 C6 105.28(16) . . ? C9 O1 C16 115.6(4) . . ? C9 O1 K1 84.8(2) . . ? C16 O1 K1 91.23(19) . . ? C10 O2 C11 124.8(4) . . ? C10 O2 K1 115.9(3) . . ? C11 O2 K1 103.0(3) . . ? C12 O3 C13 109.6(4) . . ? C12 O3 K1 117.6(3) . . ? C13 O3 K1 117.5(2) . . ? C15 O4 C14 116.4(3) . . ? C15 O4 K1 122.13(19) . . ? C14 O4 K1 103.9(2) . . ? O1 C9 C10 105.9(5) . . ? O2 C10 C9 112.3(4) . . ? C12 C11 O2 117.5(5) . . ? C11 C12 O3 109.5(4) . . ? O3 C13 C14 108.7(3) . . ? O4 C14 C13 113.8(3) . . ? O4 C15 C16 109.9(3) . . ? O1 C16 C15 109.9(3) . . ? C22 C17 C18 118.1(3) . . ? C22 C17 C23 121.3(3) . . ? C18 C17 C23 120.6(3) . . ? C19 C18 C17 120.8(3) . . ? C20 C19 C18 120.2(3) . . ? C19 C20 C21 119.4(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C17 121.3(3) . . ? _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.123 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.064 #===END data_5 _database_code_CSD 152065 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H58 N4 O8 Rb2 Si2' _chemical_formula_weight 853.94 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rb' 'Rb' -0.9393 2.9676 '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 9.8861(15) _cell_length_b 10.0654(15) _cell_length_c 11.9755(17) _cell_angle_alpha 106.949(2) _cell_angle_beta 108.155(2) _cell_angle_gamma 91.402(2) _cell_volume 1074.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 6778 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.53 _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 444 _exptl_absorpt_coefficient_mu 2.379 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.270 _exptl_absorpt_correction_T_max 0.449 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7660 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0701 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3719 _reflns_number_gt 2783 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3719 _refine_ls_number_parameters 220 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.962 _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 Rb1 Rb 0.58266(5) 0.67880(4) 0.58879(4) 0.0433(2) Uani 1 1 d . . . N1 N 0.6937(4) 0.4191(4) 0.6491(3) 0.0371(9) Uani 1 1 d . . . N2 N 0.4750(4) 0.4604(4) 0.6752(3) 0.0393(9) Uani 1 1 d . . . C1 C 0.8302(5) 0.3966(5) 0.6945(5) 0.0449(12) Uani 1 1 d U . . H1 H 0.8863 0.3838 0.6414 0.054 Uiso 1 1 calc R . . C2 C 0.8957(5) 0.3906(5) 0.8138(5) 0.0527(13) Uani 1 1 d U . . H2 H 0.9925 0.3730 0.8411 0.063 Uiso 1 1 calc R . . C3 C 0.8139(5) 0.4115(5) 0.8909(5) 0.0508(12) Uani 1 1 d U . . H3 H 0.8545 0.4091 0.9733 0.061 Uiso 1 1 calc R . . C4 C 0.6757(5) 0.4354(5) 0.8489(4) 0.0424(11) Uani 1 1 d U . . H4 H 0.6207 0.4499 0.9028 0.051 Uiso 1 1 calc R . . C5 C 0.6106(5) 0.4393(4) 0.7251(4) 0.0338(10) Uani 1 1 d U . . Si1 Si 0.34164(15) 0.48364(16) 0.73600(12) 0.0465(4) Uani 1 1 d . . . C6 C 0.1817(6) 0.5008(8) 0.6114(5) 0.0728(18) Uani 1 1 d . . . H6A H 0.2036 0.5793 0.5844 0.109 Uiso 1 1 calc R . . H6B H 0.1013 0.5180 0.6430 0.109 Uiso 1 1 calc R . . H6C H 0.1557 0.4142 0.5412 0.109 Uiso 1 1 calc R . . C7 C 0.2924(6) 0.3323(7) 0.7838(6) 0.0688(17) Uani 1 1 d . . . H7A H 0.2669 0.2465 0.7127 0.103 Uiso 1 1 calc R . . H7B H 0.2103 0.3503 0.8129 0.103 Uiso 1 1 calc R . . H7C H 0.3742 0.3212 0.8505 0.103 Uiso 1 1 calc R . . C8 C 0.3764(7) 0.6470(6) 0.8717(5) 0.0670(17) Uani 1 1 d . . . H8A H 0.4664 0.6465 0.9360 0.100 Uiso 1 1 calc R . . H8B H 0.2973 0.6505 0.9050 0.100 Uiso 1 1 calc R . . H8C H 0.3838 0.7292 0.8449 0.100 Uiso 1 1 calc R . . O1 O 0.8338(11) 0.8685(8) 0.5905(8) 0.167(3) Uani 1 1 d . . . O2 O 0.9281(11) 0.8768(8) 0.8334(8) 0.181(4) Uani 1 1 d . . . O3 O 0.6402(15) 0.8755(8) 0.8525(9) 0.238(6) Uani 1 1 d . . . O4 O 0.5903(8) 0.9733(5) 0.6498(7) 0.153(3) Uani 1 1 d . . . C9 C 0.931(2) 0.948(3) 0.6591(17) 0.319(12) Uani 1 1 d U . . H9A H 0.9056 1.0340 0.7092 0.383 Uiso 1 1 calc R . . H9B H 1.0011 0.9699 0.6213 0.383 Uiso 1 1 calc R . . C10 C 0.9816(14) 0.8176(15) 0.7394(15) 0.250(10) Uani 1 1 d U . . H10A H 0.9327 0.7222 0.6881 0.300 Uiso 1 1 calc R . . H10B H 1.0867 0.8163 0.7700 0.300 Uiso 1 1 calc R . . C11 C 0.871(2) 0.7941(10) 0.8973(14) 0.265(12) Uani 1 1 d U . . H11A H 0.8177 0.7030 0.8390 0.319 Uiso 1 1 calc R . . H11B H 0.9485 0.7781 0.9660 0.319 Uiso 1 1 calc R . . C12 C 0.781(3) 0.8819(17) 0.9401(17) 0.300(12) Uani 1 1 d U . . H12A H 0.8294 0.9793 0.9698 0.360 Uiso 1 1 calc R . . H12B H 0.7695 0.8606 1.0124 0.360 Uiso 1 1 calc R . . C13 C 0.6497(19) 1.0045(15) 0.8827(13) 0.223(6) Uani 1 1 d U . . H13A H 0.7487 1.0464 0.9002 0.267 Uiso 1 1 calc R . . H13B H 0.6205 1.0436 0.9564 0.267 Uiso 1 1 calc R . . C14 C 0.5497(16) 1.0286(13) 0.7732(13) 0.195(6) Uani 1 1 d U . . H14A H 0.5443 1.1305 0.7915 0.234 Uiso 1 1 calc R . . H14B H 0.4530 0.9825 0.7574 0.234 Uiso 1 1 calc R . . C15 C 0.6672(16) 1.0635(12) 0.6507(15) 0.196(7) Uani 1 1 d U . . H15A H 0.7391 1.1075 0.7339 0.235 Uiso 1 1 calc R . . H15B H 0.6137 1.1361 0.6225 0.235 Uiso 1 1 calc R . . C16 C 0.7337(18) 0.9868(12) 0.5624(15) 0.193(6) Uani 1 1 d U . . H16A H 0.7921 1.0570 0.5477 0.232 Uiso 1 1 calc R . . H16B H 0.6553 0.9416 0.4832 0.232 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 Rb1 0.0524(3) 0.0315(2) 0.0337(3) 0.00683(17) 0.0012(2) 0.00141(19) N1 0.030(2) 0.040(2) 0.041(2) 0.0155(17) 0.0091(18) 0.0054(16) N2 0.029(2) 0.060(2) 0.0262(19) 0.0136(18) 0.0058(17) 0.0096(18) C1 0.031(3) 0.050(3) 0.059(3) 0.019(2) 0.020(2) 0.006(2) C2 0.029(3) 0.059(3) 0.063(3) 0.024(2) 0.000(2) 0.006(2) C3 0.039(3) 0.064(3) 0.044(3) 0.024(2) -0.001(2) 0.005(2) C4 0.034(2) 0.057(3) 0.032(2) 0.017(2) 0.003(2) 0.003(2) C5 0.029(2) 0.040(2) 0.032(2) 0.0149(19) 0.0057(19) 0.0038(19) Si1 0.0350(8) 0.0710(9) 0.0371(8) 0.0223(7) 0.0114(6) 0.0155(7) C6 0.039(3) 0.126(5) 0.060(4) 0.041(4) 0.014(3) 0.031(3) C7 0.052(4) 0.090(4) 0.079(4) 0.038(4) 0.032(3) 0.014(3) C8 0.079(4) 0.081(4) 0.051(3) 0.027(3) 0.030(3) 0.030(3) O1 0.216(9) 0.112(5) 0.153(7) -0.007(5) 0.082(7) -0.036(6) O2 0.214(9) 0.130(6) 0.120(6) 0.036(5) -0.047(6) -0.015(6) O3 0.410(17) 0.085(5) 0.210(9) -0.054(5) 0.195(11) -0.106(7) O4 0.185(7) 0.047(3) 0.147(6) 0.036(3) -0.059(5) -0.007(4) C9 0.30(2) 0.37(2) 0.207(18) 0.034(16) 0.046(16) -0.251(18) C10 0.140(11) 0.198(13) 0.225(16) -0.132(10) -0.018(10) 0.106(10) C11 0.36(2) 0.059(5) 0.187(12) 0.070(7) -0.192(13) -0.053(9) C12 0.37(2) 0.116(8) 0.187(12) 0.013(9) -0.174(14) -0.078(10) C13 0.250(14) 0.170(9) 0.150(10) -0.050(9) 0.025(9) 0.049(9) C14 0.210(13) 0.142(8) 0.153(10) -0.044(8) 0.029(9) 0.097(8) C15 0.209(12) 0.062(6) 0.248(15) 0.058(7) -0.025(10) 0.014(7) C16 0.223(13) 0.079(7) 0.238(15) 0.069(8) 0.005(10) -0.004(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 Rb1 O4 2.832(5) . ? Rb1 N2 2.922(4) 2_666 ? Rb1 N2 2.990(4) . ? Rb1 N1 3.051(4) . ? Rb1 O3 3.065(8) . ? Rb1 O1 3.086(8) . ? Rb1 N1 3.152(4) 2_666 ? N1 C1 1.341(6) . ? N1 C5 1.382(6) . ? N1 Rb1 3.152(4) 2_666 ? N2 C5 1.336(5) . ? N2 Si1 1.684(4) . ? N2 Rb1 2.922(4) 2_666 ? C1 C2 1.393(7) . ? C2 C3 1.382(7) . ? C3 C4 1.354(7) . ? C4 C5 1.434(6) . ? Si1 C6 1.857(5) . ? Si1 C8 1.878(6) . ? Si1 C7 1.879(6) . ? O1 C9 1.151(14) . ? O1 C16 1.610(15) . ? O2 C10 1.378(16) . ? O2 C11 1.49(2) . ? O3 C13 1.235(15) . ? O3 C12 1.45(2) . ? O4 C15 1.166(15) . ? O4 C14 1.598(15) . ? C9 C10 1.83(2) . ? C11 C12 1.37(3) . ? C13 C14 1.465(17) . ? C15 C16 1.46(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 O4 Rb1 N2 112.96(18) . 2_666 ? O4 Rb1 N2 134.8(2) . . ? N2 Rb1 N2 104.06(9) 2_666 . ? O4 Rb1 N1 150.88(14) . . ? N2 Rb1 N1 90.98(10) 2_666 . ? N2 Rb1 N1 44.94(10) . . ? O4 Rb1 O3 56.3(3) . . ? N2 Rb1 O3 169.2(2) 2_666 . ? N2 Rb1 O3 85.72(15) . . ? N1 Rb1 O3 99.3(3) . . ? O4 Rb1 O1 57.6(3) . . ? N2 Rb1 O1 88.89(16) 2_666 . ? N2 Rb1 O1 150.0(2) . . ? N1 Rb1 O1 109.2(2) . . ? O3 Rb1 O1 84.57(19) . . ? O4 Rb1 N1 100.64(13) . 2_666 ? N2 Rb1 N1 44.50(10) 2_666 2_666 ? N2 Rb1 N1 87.82(9) . 2_666 ? N1 Rb1 N1 108.21(8) . 2_666 ? O3 Rb1 N1 133.2(3) . 2_666 ? O1 Rb1 N1 119.04(19) . 2_666 ? C1 N1 C5 118.6(4) . . ? C1 N1 Rb1 128.2(3) . . ? C5 N1 Rb1 85.7(2) . . ? C1 N1 Rb1 142.8(3) . 2_666 ? C5 N1 Rb1 91.0(2) . 2_666 ? Rb1 N1 Rb1 71.79(8) . 2_666 ? C5 N2 Si1 130.2(3) . . ? C5 N2 Rb1 102.4(3) . 2_666 ? Si1 N2 Rb1 121.54(17) . 2_666 ? C5 N2 Rb1 89.1(3) . . ? Si1 N2 Rb1 121.60(19) . . ? Rb1 N2 Rb1 75.94(9) 2_666 . ? N1 C1 C2 124.6(5) . . ? C3 C2 C1 117.3(5) . . ? C4 C3 C2 119.9(5) . . ? C3 C4 C5 121.7(5) . . ? N2 C5 N1 116.3(4) . . ? N2 C5 C4 125.8(4) . . ? N1 C5 C4 117.9(4) . . ? N2 Si1 C6 106.1(2) . . ? N2 Si1 C8 114.2(2) . . ? C6 Si1 C8 107.1(3) . . ? N2 Si1 C7 114.0(2) . . ? C6 Si1 C7 107.3(3) . . ? C8 Si1 C7 107.8(3) . . ? C9 O1 C16 94.4(16) . . ? C9 O1 Rb1 140.3(10) . . ? C16 O1 Rb1 92.7(7) . . ? C10 O2 C11 123.3(13) . . ? C13 O3 C12 91.4(10) . . ? C13 O3 Rb1 125.2(10) . . ? C12 O3 Rb1 115.9(12) . . ? C15 O4 C14 106.4(11) . . ? C15 O4 Rb1 134.7(10) . . ? C14 O4 Rb1 107.9(6) . . ? O1 C9 C10 87.9(15) . . ? O2 C10 C9 95.9(10) . . ? C12 C11 O2 100.7(11) . . ? C11 C12 O3 116.4(14) . . ? O3 C13 C14 102.8(13) . . ? C13 C14 O4 115.0(10) . . ? O4 C15 C16 100.8(11) . . ? C15 C16 O1 121.2(12) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.820 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.094 #===END data_6 _database_code_CSD 152066 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H84 Cs4 N8 O16' _chemical_formula_weight 1608.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'Cs' 'Cs' -0.3680 2.1192 '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 10.7464(7) _cell_length_b 11.5129(7) _cell_length_c 13.7340(8) _cell_angle_alpha 93.177(2) _cell_angle_beta 111.692(2) _cell_angle_gamma 93.177(2) _cell_volume 1571.16(17) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10055 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 29.12 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 2.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.588 _exptl_absorpt_correction_T_max 0.831 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69300 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15504 _diffrn_reflns_av_R_equivalents 0.0319 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 29.20 _reflns_number_total 8156 _reflns_number_gt 5920 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0438P)^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 8156 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0839 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _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 Cs1 Cs 0.36875(2) 0.61782(2) 0.515571(18) 0.01925(7) Uani 1 1 d . . . Cs2 Cs 0.55721(2) 0.41460(2) 0.792021(19) 0.02215(7) Uani 1 1 d . . . N1 N 0.7061(3) 0.6306(3) 0.6400(3) 0.0241(7) Uani 1 1 d . . . N2 N 0.6328(4) 0.6590(3) 0.4629(3) 0.0259(8) Uani 1 1 d . . . H2N H 0.633(5) 0.720(4) 0.421(4) 0.031 Uiso 1 1 d . . . C1 C 0.7794(4) 0.6708(4) 0.7397(3) 0.0281(9) Uani 1 1 d . . . H1 H 0.7817 0.6207 0.7929 0.034 Uiso 1 1 calc R . . C2 C 0.8511(4) 0.7770(4) 0.7718(3) 0.0287(10) Uani 1 1 d . . . H2 H 0.9020 0.7988 0.8441 0.034 Uiso 1 1 calc R . . C3 C 0.8465(4) 0.8520(4) 0.6947(4) 0.0286(10) Uani 1 1 d . . . H3 H 0.8933 0.9273 0.7133 0.034 Uiso 1 1 calc R . . C4 C 0.7733(4) 0.8154(4) 0.5913(3) 0.0253(9) Uani 1 1 d . . . H4 H 0.7694 0.8663 0.5383 0.030 Uiso 1 1 calc R . . C5 C 0.7025(4) 0.7014(3) 0.5618(3) 0.0194(8) Uani 1 1 d . . . N3 N 0.3060(4) 0.3002(3) 0.8413(3) 0.0275(8) Uani 1 1 d . . . N4 N 0.3474(4) 0.4055(3) 1.0041(3) 0.0357(9) Uani 1 1 d . . . H4N H 0.399(5) 0.461(4) 0.972(4) 0.043 Uiso 1 1 d . . . C6 C 0.2444(4) 0.2049(4) 0.7769(4) 0.0324(10) Uani 1 1 d . . . H6 H 0.2494 0.1998 0.7092 0.039 Uiso 1 1 calc R . . C7 C 0.1749(5) 0.1142(4) 0.8006(4) 0.0340(11) Uani 1 1 d . . . H7 H 0.1307 0.0505 0.7504 0.041 Uiso 1 1 calc R . . C8 C 0.1718(4) 0.1193(4) 0.9010(4) 0.0345(11) Uani 1 1 d . . . H8 H 0.1273 0.0573 0.9215 0.041 Uiso 1 1 calc R . . C9 C 0.2334(4) 0.2142(4) 0.9702(4) 0.0297(10) Uani 1 1 d . . . H9 H 0.2331 0.2168 1.0394 0.036 Uiso 1 1 calc R . . C10 C 0.2985(4) 0.3102(4) 0.9394(3) 0.0231(9) Uani 1 1 d . . . O1 O 0.8783(3) 0.4000(2) 0.8730(2) 0.0245(6) Uani 1 1 d . . . O2 O 0.7279(3) 0.2932(2) 0.9840(2) 0.0254(6) Uani 1 1 d . . . O3 O 0.5748(3) 0.1345(2) 0.8084(2) 0.0254(6) Uani 1 1 d . . . O4 O 0.7211(3) 0.2427(2) 0.6966(2) 0.0227(6) Uani 1 1 d . . . C11 C 0.9433(4) 0.3505(4) 0.9703(3) 0.0253(9) Uani 1 1 d . . . H11A H 1.0323 0.3929 1.0093 0.030 Uiso 1 1 calc R . . H11B H 0.9566 0.2675 0.9573 0.030 Uiso 1 1 calc R . . C12 C 0.8549(4) 0.3607(4) 1.0331(3) 0.0235(9) Uani 1 1 d . . . H12A H 0.9022 0.3342 1.1038 0.028 Uiso 1 1 calc R . . H12B H 0.8388 0.4438 1.0420 0.028 Uiso 1 1 calc R . . C13 C 0.7335(5) 0.1709(4) 0.9906(3) 0.0292(10) Uani 1 1 d . . . H13A H 0.7501 0.1513 1.0634 0.035 Uiso 1 1 calc R . . H13B H 0.8075 0.1439 0.9707 0.035 Uiso 1 1 calc R . . C14 C 0.6006(5) 0.1124(4) 0.9162(3) 0.0291(10) Uani 1 1 d . . . H14A H 0.6004 0.0271 0.9226 0.035 Uiso 1 1 calc R . . H14B H 0.5277 0.1411 0.9364 0.035 Uiso 1 1 calc R . . C15 C 0.6476(4) 0.0672(4) 0.7609(4) 0.0276(9) Uani 1 1 d . . . H15A H 0.6028 -0.0125 0.7380 0.033 Uiso 1 1 calc R . . H15B H 0.7400 0.0610 0.8118 0.033 Uiso 1 1 calc R . . C16 C 0.6516(4) 0.1279(4) 0.6676(3) 0.0260(9) Uani 1 1 d . . . H16A H 0.6967 0.0799 0.6306 0.031 Uiso 1 1 calc R . . H16B H 0.5585 0.1345 0.6182 0.031 Uiso 1 1 calc R . . C17 C 0.8630(4) 0.2395(4) 0.7437(3) 0.0252(9) Uani 1 1 d . . . H17A H 0.8992 0.2144 0.6900 0.030 Uiso 1 1 calc R . . H17B H 0.8861 0.1834 0.7986 0.030 Uiso 1 1 calc R . . C18 C 0.9226(4) 0.3603(4) 0.7917(3) 0.0258(9) Uani 1 1 d . . . H18A H 1.0218 0.3606 0.8211 0.031 Uiso 1 1 calc R . . H18B H 0.8979 0.4153 0.7359 0.031 Uiso 1 1 calc R . . O5 O 0.0943(3) 0.6206(3) 0.5430(2) 0.0320(7) Uani 1 1 d . . . O6 O 0.1905(3) 0.8474(3) 0.5207(2) 0.0333(7) Uani 1 1 d . . . O7 O 0.4224(3) 0.8154(3) 0.7059(2) 0.0301(7) Uani 1 1 d . . . O8 O 0.3234(3) 0.5888(3) 0.7232(2) 0.0305(7) Uani 1 1 d . . . C19 C 0.0093(4) 0.7066(4) 0.4848(3) 0.0269(9) Uani 1 1 d . . . H19A H -0.0811 0.6930 0.4876 0.032 Uiso 1 1 calc R . . H19B H -0.0006 0.6958 0.4103 0.032 Uiso 1 1 calc R . . C20 C 0.0624(4) 0.8286(4) 0.5258(4) 0.0341(11) Uani 1 1 d . . . H20A H 0.0012 0.8837 0.4831 0.041 Uiso 1 1 calc R . . H20B H 0.0690 0.8419 0.5995 0.041 Uiso 1 1 calc R . . C21 C 0.2767(5) 0.9383(4) 0.5957(3) 0.0285(10) Uani 1 1 d . . . H21A H 0.2249 1.0068 0.5953 0.034 Uiso 1 1 calc R . . H21B H 0.3516 0.9626 0.5737 0.034 Uiso 1 1 calc R . . C22 C 0.3335(4) 0.9006(4) 0.7053(4) 0.0305(10) Uani 1 1 d . . . H22A H 0.3817 0.9680 0.7556 0.037 Uiso 1 1 calc R . . H22B H 0.2605 0.8678 0.7258 0.037 Uiso 1 1 calc R . . C23 C 0.4671(4) 0.7566(4) 0.8035(3) 0.0277(9) Uani 1 1 d . . . H23A H 0.4940 0.8158 0.8642 0.033 Uiso 1 1 calc R . . H23B H 0.5469 0.7146 0.8085 0.033 Uiso 1 1 calc R . . C24 C 0.3598(5) 0.6719(4) 0.8090(4) 0.0330(10) Uani 1 1 d . . . H24A H 0.3935 0.6333 0.8755 0.040 Uiso 1 1 calc R . . H24B H 0.2807 0.7134 0.8072 0.040 Uiso 1 1 calc R . . C25 C 0.1920(4) 0.5271(4) 0.6969(4) 0.0302(10) Uani 1 1 d . . . H25A H 0.1812 0.5064 0.7625 0.036 Uiso 1 1 calc R . . H25B H 0.1868 0.4536 0.6541 0.036 Uiso 1 1 calc R . . C26 C 0.0789(5) 0.5979(4) 0.6371(4) 0.0357(11) Uani 1 1 d . . . H26A H -0.0088 0.5540 0.6224 0.043 Uiso 1 1 calc R . . H26B H 0.0826 0.6720 0.6786 0.043 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 Cs1 0.01768(13) 0.02471(14) 0.02042(13) 0.00436(10) 0.01191(10) 0.00690(10) Cs2 0.01990(13) 0.02152(14) 0.02388(14) 0.00051(10) 0.00622(11) 0.00745(10) N1 0.0237(18) 0.0228(18) 0.0263(19) 0.0038(14) 0.0096(15) 0.0006(14) N2 0.0243(19) 0.034(2) 0.0218(18) 0.0032(15) 0.0106(15) 0.0046(15) C1 0.026(2) 0.034(2) 0.027(2) 0.0118(19) 0.0103(19) 0.0038(18) C2 0.025(2) 0.034(3) 0.025(2) -0.0005(19) 0.0076(19) 0.0030(19) C3 0.026(2) 0.022(2) 0.040(3) -0.0022(19) 0.016(2) 0.0012(17) C4 0.028(2) 0.024(2) 0.032(2) 0.0090(18) 0.0179(19) 0.0102(17) C5 0.0138(18) 0.025(2) 0.024(2) 0.0048(16) 0.0109(16) 0.0076(15) N3 0.0270(19) 0.028(2) 0.030(2) 0.0029(16) 0.0139(16) 0.0066(15) N4 0.035(2) 0.031(2) 0.036(2) -0.0036(17) 0.0077(19) 0.0050(17) C6 0.028(2) 0.039(3) 0.030(2) -0.004(2) 0.012(2) 0.010(2) C7 0.029(2) 0.026(2) 0.046(3) -0.011(2) 0.015(2) 0.0012(19) C8 0.025(2) 0.027(2) 0.055(3) 0.011(2) 0.017(2) 0.0065(19) C9 0.028(2) 0.038(3) 0.028(2) 0.0112(19) 0.0131(19) 0.0127(19) C10 0.019(2) 0.025(2) 0.025(2) 0.0041(17) 0.0067(17) 0.0109(16) O1 0.0250(15) 0.0275(16) 0.0223(15) 0.0053(12) 0.0095(13) 0.0050(12) O2 0.0266(16) 0.0225(15) 0.0269(16) 0.0041(12) 0.0092(13) 0.0043(12) O3 0.0268(16) 0.0227(15) 0.0308(16) -0.0006(12) 0.0158(14) 0.0038(12) O4 0.0197(14) 0.0233(15) 0.0272(15) 0.0037(12) 0.0101(12) 0.0075(11) C11 0.020(2) 0.029(2) 0.023(2) 0.0051(17) 0.0031(17) 0.0033(17) C12 0.024(2) 0.026(2) 0.018(2) -0.0028(16) 0.0060(17) 0.0019(17) C13 0.042(3) 0.025(2) 0.026(2) 0.0054(18) 0.018(2) 0.0061(19) C14 0.037(3) 0.023(2) 0.035(3) 0.0043(18) 0.023(2) -0.0015(18) C15 0.029(2) 0.022(2) 0.036(2) -0.0039(18) 0.017(2) 0.0021(17) C16 0.026(2) 0.024(2) 0.027(2) -0.0054(17) 0.0096(18) 0.0025(17) C17 0.020(2) 0.040(3) 0.020(2) 0.0055(18) 0.0105(17) 0.0048(18) C18 0.023(2) 0.033(2) 0.027(2) 0.0095(18) 0.0143(18) 0.0031(17) O5 0.0288(17) 0.0353(18) 0.0382(18) -0.0014(14) 0.0207(15) 0.0001(13) O6 0.0280(17) 0.0422(19) 0.0323(17) 0.0088(15) 0.0129(14) 0.0057(14) O7 0.0268(16) 0.0258(16) 0.0405(19) -0.0027(13) 0.0167(15) 0.0017(13) O8 0.0369(18) 0.0254(16) 0.0356(18) 0.0054(13) 0.0194(15) 0.0112(13) C19 0.017(2) 0.037(3) 0.028(2) 0.0014(19) 0.0083(18) 0.0049(18) C20 0.024(2) 0.039(3) 0.039(3) 0.008(2) 0.009(2) 0.010(2) C21 0.039(3) 0.018(2) 0.031(2) 0.0044(17) 0.016(2) 0.0004(18) C22 0.027(2) 0.025(2) 0.037(3) -0.0043(19) 0.010(2) 0.0006(18) C23 0.030(2) 0.027(2) 0.025(2) 0.0045(18) 0.0066(19) 0.0099(18) C24 0.042(3) 0.030(2) 0.027(2) 0.0063(19) 0.012(2) 0.010(2) C25 0.030(2) 0.022(2) 0.047(3) 0.012(2) 0.023(2) 0.0008(18) C26 0.027(2) 0.044(3) 0.041(3) 0.005(2) 0.019(2) -0.001(2) _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 Cs1 O8 3.098(3) . ? Cs1 O5 3.110(3) . ? Cs1 N2 3.194(4) . ? Cs1 N2 3.216(4) 2_666 ? Cs1 O7 3.228(3) . ? Cs1 O4 3.258(3) 2_666 ? Cs1 N1 3.345(3) 2_666 ? Cs1 O6 3.362(3) . ? Cs1 N1 3.379(3) . ? Cs2 O2 3.064(3) . ? Cs2 N4 3.191(4) 2_667 ? Cs2 O8 3.200(3) . ? Cs2 O1 3.227(3) . ? Cs2 N3 3.246(4) . ? Cs2 O4 3.247(3) . ? Cs2 O3 3.256(3) . ? Cs2 N2 3.367(4) 2_666 ? N1 C1 1.342(5) . ? N1 C5 1.374(5) . ? N1 Cs1 3.345(3) 2_666 ? N2 C5 1.334(5) . ? N2 Cs1 3.216(4) 2_666 ? N2 Cs2 3.367(4) 2_666 ? C1 C2 1.367(6) . ? C2 C3 1.392(6) . ? C3 C4 1.372(6) . ? C4 C5 1.439(6) . ? N3 C6 1.343(6) . ? N3 C10 1.378(5) . ? N4 C10 1.324(5) . ? N4 Cs2 3.191(4) 2_667 ? C6 C7 1.373(7) . ? C7 C8 1.390(7) . ? C8 C9 1.369(7) . ? C9 C10 1.441(6) . ? O1 C11 1.427(5) . ? O1 C18 1.430(5) . ? O2 C13 1.419(5) . ? O2 C12 1.437(5) . ? O3 C15 1.425(5) . ? O3 C14 1.442(5) . ? O4 C17 1.423(5) . ? O4 C16 1.440(5) . ? O4 Cs1 3.258(3) 2_666 ? C11 C12 1.506(6) . ? C13 C14 1.508(6) . ? C15 C16 1.506(6) . ? C17 C18 1.505(6) . ? O5 C26 1.399(5) . ? O5 C19 1.449(5) . ? O6 C20 1.410(5) . ? O6 C21 1.443(5) . ? O7 C22 1.405(5) . ? O7 C23 1.466(5) . ? O8 C24 1.396(5) . ? O8 C25 1.454(5) . ? C19 C20 1.485(6) . ? C21 C22 1.499(6) . ? C23 C24 1.495(6) . ? C25 C26 1.504(6) . ? 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 O8 Cs1 O5 54.29(8) . . ? O8 Cs1 N2 132.98(9) . . ? O5 Cs1 N2 168.80(9) . . ? O8 Cs1 N2 76.02(8) . 2_666 ? O5 Cs1 N2 90.41(9) . 2_666 ? N2 Cs1 N2 99.63(9) . 2_666 ? O8 Cs1 O7 52.87(8) . . ? O5 Cs1 O7 75.93(8) . . ? N2 Cs1 O7 101.82(8) . . ? N2 Cs1 O7 125.34(8) 2_666 . ? O8 Cs1 O4 144.01(7) . 2_666 ? O5 Cs1 O4 95.69(8) . 2_666 ? N2 Cs1 O4 74.16(8) . 2_666 ? N2 Cs1 O4 128.94(8) 2_666 2_666 ? O7 Cs1 O4 105.22(7) . 2_666 ? O8 Cs1 N1 112.50(8) . 2_666 ? O5 Cs1 N1 96.31(8) . 2_666 ? N2 Cs1 N1 88.13(9) . 2_666 ? N2 Cs1 N1 41.20(9) 2_666 2_666 ? O7 Cs1 N1 165.34(8) . 2_666 ? O4 Cs1 N1 87.74(8) 2_666 2_666 ? O8 Cs1 O6 79.48(7) . . ? O5 Cs1 O6 51.67(8) . . ? N2 Cs1 O6 118.24(9) . . ? N2 Cs1 O6 142.07(8) 2_666 . ? O7 Cs1 O6 51.93(8) . . ? O4 Cs1 O6 65.25(7) 2_666 . ? N1 Cs1 O6 131.99(8) 2_666 . ? O8 Cs1 N1 92.05(8) . . ? O5 Cs1 N1 145.63(8) . . ? N2 Cs1 N1 41.06(9) . . ? N2 Cs1 N1 87.19(8) 2_666 . ? O7 Cs1 N1 77.68(8) . . ? O4 Cs1 N1 112.28(8) 2_666 . ? N1 Cs1 N1 104.06(7) 2_666 . ? O6 Cs1 N1 122.40(8) . . ? O2 Cs2 N4 70.56(9) . 2_667 ? O2 Cs2 O8 140.61(8) . . ? N4 Cs2 O8 79.48(9) 2_667 . ? O2 Cs2 O1 54.27(7) . . ? N4 Cs2 O1 79.81(9) 2_667 . ? O8 Cs2 O1 144.01(8) . . ? O2 Cs2 N3 84.13(8) . . ? N4 Cs2 N3 93.04(10) 2_667 . ? O8 Cs2 N3 72.30(8) . . ? O1 Cs2 N3 137.94(8) . . ? O2 Cs2 O4 76.99(7) . . ? N4 Cs2 O4 131.93(9) 2_667 . ? O8 Cs2 O4 142.00(7) . . ? O1 Cs2 O4 52.33(7) . . ? N3 Cs2 O4 118.15(8) . . ? O2 Cs2 O3 53.45(7) . . ? N4 Cs2 O3 121.96(9) 2_667 . ? O8 Cs2 O3 136.38(8) . . ? O1 Cs2 O3 79.59(7) . . ? N3 Cs2 O3 69.29(8) . . ? O4 Cs2 O3 52.12(7) . . ? O2 Cs2 N2 137.85(8) . 2_666 ? N4 Cs2 N2 150.97(9) 2_667 2_666 ? O8 Cs2 N2 72.57(8) . 2_666 ? O1 Cs2 N2 119.36(8) . 2_666 ? N3 Cs2 N2 85.94(9) . 2_666 ? O4 Cs2 N2 72.04(8) . 2_666 ? O3 Cs2 N2 84.77(8) . 2_666 ? C1 N1 C5 117.8(4) . . ? C1 N1 Cs1 140.0(3) . 2_666 ? C5 N1 Cs1 95.0(2) . 2_666 ? C1 N1 Cs1 127.8(3) . . ? C5 N1 Cs1 82.3(2) . . ? Cs1 N1 Cs1 75.94(7) 2_666 . ? C5 N2 Cs1 90.5(2) . . ? C5 N2 Cs1 101.8(3) . 2_666 ? Cs1 N2 Cs1 80.37(9) . 2_666 ? C5 N2 Cs2 172.8(3) . 2_666 ? Cs1 N2 Cs2 88.45(9) . 2_666 ? Cs1 N2 Cs2 85.05(9) 2_666 2_666 ? N1 C1 C2 126.2(4) . . ? C1 C2 C3 117.4(4) . . ? C4 C3 C2 119.0(4) . . ? C3 C4 C5 121.1(4) . . ? N2 C5 N1 117.2(4) . . ? N2 C5 C4 124.3(4) . . ? N1 C5 C4 118.5(4) . . ? C6 N3 C10 118.2(4) . . ? C6 N3 Cs2 112.7(3) . . ? C10 N3 Cs2 123.2(3) . . ? C10 N4 Cs2 162.3(3) . 2_667 ? N3 C6 C7 125.6(4) . . ? C6 C7 C8 117.3(4) . . ? C9 C8 C7 119.7(4) . . ? C8 C9 C10 120.8(4) . . ? N4 C10 N3 121.7(4) . . ? N4 C10 C9 120.0(4) . . ? N3 C10 C9 118.2(4) . . ? C11 O1 C18 113.5(3) . . ? C11 O1 Cs2 118.1(2) . . ? C18 O1 Cs2 113.2(2) . . ? C13 O2 C12 114.9(3) . . ? C13 O2 Cs2 126.0(2) . . ? C12 O2 Cs2 108.1(2) . . ? C15 O3 C14 114.0(3) . . ? C15 O3 Cs2 122.9(2) . . ? C14 O3 Cs2 107.4(2) . . ? C17 O4 C16 112.6(3) . . ? C17 O4 Cs2 122.3(2) . . ? C16 O4 Cs2 110.4(2) . . ? C17 O4 Cs1 112.1(2) . 2_666 ? C16 O4 Cs1 107.0(2) . 2_666 ? Cs2 O4 Cs1 89.48(6) . 2_666 ? O1 C11 C12 107.6(3) . . ? O2 C12 C11 112.6(3) . . ? O2 C13 C14 107.8(4) . . ? O3 C14 C13 112.1(3) . . ? O3 C15 C16 107.6(3) . . ? O4 C16 C15 112.8(3) . . ? O4 C17 C18 108.0(3) . . ? O1 C18 C17 112.9(3) . . ? C26 O5 C19 114.4(3) . . ? C26 O5 Cs1 122.8(3) . . ? C19 O5 Cs1 113.9(2) . . ? C20 O6 C21 114.1(3) . . ? C20 O6 Cs1 119.4(3) . . ? C21 O6 Cs1 109.1(2) . . ? C22 O7 C23 112.7(3) . . ? C22 O7 Cs1 123.9(3) . . ? C23 O7 Cs1 107.0(2) . . ? C24 O8 C25 114.3(3) . . ? C24 O8 Cs1 126.2(3) . . ? C25 O8 Cs1 107.8(2) . . ? C24 O8 Cs2 103.8(2) . . ? C25 O8 Cs2 111.4(2) . . ? Cs1 O8 Cs2 89.94(8) . . ? O5 C19 C20 113.3(3) . . ? O6 C20 C19 108.5(4) . . ? O6 C21 C22 112.8(3) . . ? O7 C22 C21 107.3(4) . . ? O7 C23 C24 112.1(4) . . ? O8 C24 C23 108.4(4) . . ? O8 C25 C26 112.7(3) . . ? O5 C26 C25 107.2(4) . . ? _diffrn_measured_fraction_theta_max 0.886 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.038 _refine_diff_density_min -2.141 _refine_diff_density_rms 0.144 #===END data_7 _database_code_CSD 152067 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H66 Cs2 N4 O8 Si2' _chemical_formula_weight 1040.96 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cs' 'Cs' -0.3680 2.1192 '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 10.4715(12) _cell_length_b 10.9862(13) _cell_length_c 12.0328(14) _cell_angle_alpha 65.913(2) _cell_angle_beta 71.886(2) _cell_angle_gamma 83.028(2) _cell_volume 1201.1(2) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 5428 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 28.41 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.439 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 530 _exptl_absorpt_coefficient_mu 1.616 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.273 _exptl_absorpt_correction_T_max 0.571 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9763 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.1026 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.66 _reflns_number_total 5365 _reflns_number_gt 2988 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0714P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5365 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 0.842 _refine_ls_restrained_S_all 0.842 _refine_ls_shift/su_max 0.679 _refine_ls_shift/su_mean 0.042 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 Cs1 Cs 0.81017(3) 0.93747(4) 0.60207(4) 0.05448(19) Uani 1 1 d . . . N1 N 1.0874(5) 0.8141(5) 0.6710(5) 0.0521(13) Uani 1 1 d . . . N2 N 1.0427(5) 1.0231(5) 0.6764(5) 0.0529(13) Uani 1 1 d . . . C1 C 1.1090(6) 0.6849(6) 0.7302(6) 0.0572(17) Uani 1 1 d . . . H1 H 1.1266 0.6315 0.6818 0.069 Uiso 1 1 calc R . . C2 C 1.1079(6) 0.6224(6) 0.8551(7) 0.0599(18) Uani 1 1 d . . . H2 H 1.1258 0.5298 0.8914 0.072 Uiso 1 1 calc R . . C3 C 1.0792(6) 0.7005(7) 0.9268(7) 0.0602(18) Uani 1 1 d . . . H3 H 1.0755 0.6619 1.0143 0.072 Uiso 1 1 calc R . . C4 C 1.0571(6) 0.8311(6) 0.8697(6) 0.0510(16) Uani 1 1 d . . . H4 H 1.0376 0.8842 0.9185 0.061 Uiso 1 1 calc R . . C5 C 1.0617(5) 0.8936(5) 0.7391(6) 0.0455(15) Uani 1 1 d . . . Si1 Si 1.00933(17) 1.15148(16) 0.72319(17) 0.0562(5) Uani 1 1 d . . . C6 C 1.1340(6) 1.1766(7) 0.7943(7) 0.072(2) Uani 1 1 d . . . H6A H 1.1253 1.1040 0.8778 0.087 Uiso 1 1 calc R . . H6B H 1.1172 1.2620 0.8039 0.087 Uiso 1 1 calc R . . H6C H 1.2251 1.1769 0.7385 0.087 Uiso 1 1 calc R . . C7 C 0.8385(6) 1.1424(7) 0.8400(6) 0.0639(19) Uani 1 1 d . . . H7A H 0.7693 1.1355 0.8036 0.077 Uiso 1 1 calc R . . H7B H 0.8237 1.2229 0.8582 0.077 Uiso 1 1 calc R . . H7C H 0.8337 1.0638 0.9189 0.077 Uiso 1 1 calc R . . C8 C 1.0158(8) 1.3047(6) 0.5766(7) 0.082(3) Uani 1 1 d . . . H8A H 1.1088 1.3220 0.5220 0.098 Uiso 1 1 calc R . . H8B H 0.9827 1.3808 0.6001 0.098 Uiso 1 1 calc R . . H8C H 0.9595 1.2919 0.5307 0.098 Uiso 1 1 calc R . . O1 O 0.6582(5) 0.6660(5) 0.6765(5) 0.0799(15) Uani 1 1 d . . . O2 O 0.5040(4) 0.9021(5) 0.6613(5) 0.0712(14) Uani 1 1 d . . . O3 O 0.5784(6) 0.9148(6) 0.8643(5) 0.0914(18) Uani 1 1 d . . . O4 O 0.6950(19) 0.6715(13) 0.8991(11) 0.254(9) Uani 1 1 d . . . C9 C 0.5214(9) 0.6661(9) 0.6969(9) 0.089(3) Uani 1 1 d . . . H9A H 0.4745 0.6418 0.7884 0.106 Uiso 1 1 calc R . . H9B H 0.4968 0.6000 0.6705 0.106 Uiso 1 1 calc R . . C10 C 0.4807(9) 0.8034(8) 0.6205(8) 0.081(2) Uani 1 1 d . . . H10A H 0.5318 0.8280 0.5298 0.097 Uiso 1 1 calc R . . H10B H 0.3841 0.8024 0.6276 0.097 Uiso 1 1 calc R . . C11 C 0.4065(8) 0.9040(9) 0.7656(10) 0.109(3) Uani 1 1 d . . . H11A H 0.3807 0.8117 0.8275 0.131 Uiso 1 1 calc R . . H11B H 0.3260 0.9498 0.7415 0.131 Uiso 1 1 calc R . . C12 C 0.4595(8) 0.9752(8) 0.8228(10) 0.102(3) Uani 1 1 d . . . H12A H 0.4824 1.0676 0.7600 0.122 Uiso 1 1 calc R . . H12B H 0.3875 0.9801 0.8970 0.122 Uiso 1 1 calc R . . C13 C 0.5460(12) 0.8130(11) 0.9803(9) 0.116(4) Uani 1 1 d . . . H13A H 0.4662 0.7641 0.9921 0.139 Uiso 1 1 calc R . . H13B H 0.5259 0.8471 1.0484 0.139 Uiso 1 1 calc R . . C14 C 0.6683(10) 0.7217(13) 0.9841(9) 0.121(4) Uani 1 1 d . . . H14A H 0.7473 0.7731 0.9700 0.145 Uiso 1 1 calc R . . H14B H 0.6515 0.6485 1.0694 0.145 Uiso 1 1 calc R . . C15 C 0.685(2) 0.5844(10) 0.8908(18) 0.210(12) Uani 1 1 d . . . H15A H 0.5932 0.5523 0.9462 0.252 Uiso 1 1 calc R . . H15B H 0.7469 0.5221 0.9345 0.252 Uiso 1 1 calc R . . C16 C 0.6999(9) 0.5537(8) 0.7769(9) 0.108(4) Uani 1 1 d . . . H16A H 0.7949 0.5324 0.7432 0.129 Uiso 1 1 calc R . . H16B H 0.6447 0.4743 0.8027 0.129 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 Cs1 0.0280(2) 0.0528(3) 0.0553(3) -0.00629(18) 0.00908(15) -0.01336(14) N1 0.040(3) 0.039(3) 0.047(3) 0.003(2) 0.000(2) 0.001(2) N2 0.047(3) 0.035(3) 0.046(3) 0.003(2) 0.002(2) 0.001(2) C1 0.050(4) 0.043(4) 0.057(4) -0.005(3) -0.006(3) 0.001(3) C2 0.051(4) 0.033(3) 0.067(5) 0.006(3) -0.014(3) 0.002(3) C3 0.051(4) 0.051(4) 0.054(4) 0.000(3) -0.008(3) -0.004(3) C4 0.039(3) 0.041(4) 0.052(4) -0.006(3) 0.000(3) -0.005(3) C5 0.031(3) 0.034(3) 0.046(4) -0.001(3) 0.004(2) 0.000(2) Si1 0.0450(9) 0.0354(9) 0.0483(10) 0.0022(8) 0.0143(8) 0.0004(7) C6 0.046(4) 0.057(4) 0.083(5) -0.016(4) 0.013(3) -0.013(3) C7 0.049(4) 0.058(4) 0.054(4) -0.007(3) 0.007(3) 0.000(3) C8 0.090(6) 0.037(4) 0.063(5) 0.003(3) 0.019(4) 0.005(4) O1 0.061(3) 0.083(4) 0.073(3) -0.024(3) 0.006(3) -0.010(3) O2 0.040(2) 0.064(3) 0.080(3) 0.000(3) -0.012(2) -0.007(2) O3 0.086(4) 0.109(4) 0.062(3) -0.033(3) 0.021(3) -0.052(3) O4 0.46(2) 0.183(11) 0.126(8) -0.065(9) -0.158(12) 0.181(14) C9 0.085(6) 0.098(7) 0.094(6) -0.059(6) -0.002(5) -0.027(5) C10 0.098(6) 0.067(5) 0.076(6) 0.002(4) -0.051(5) -0.031(4) C11 0.042(4) 0.086(7) 0.156(10) -0.027(6) 0.001(5) 0.002(4) C12 0.048(5) 0.072(6) 0.166(10) -0.053(6) 0.010(5) -0.015(4) C13 0.131(9) 0.125(8) 0.072(6) -0.049(6) 0.032(6) -0.058(7) C14 0.092(7) 0.214(13) 0.042(5) -0.023(7) -0.027(5) -0.023(8) C15 0.37(3) 0.053(7) 0.27(2) 0.030(10) -0.28(2) -0.054(10) C16 0.083(6) 0.051(5) 0.102(7) 0.016(5) 0.018(5) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cs1 N2 3.092(5) 2_776 ? Cs1 O2 3.097(4) . ? Cs1 N2 3.196(6) . ? Cs1 O1 3.211(5) . ? Cs1 N1 3.252(5) . ? Cs1 N1 3.255(5) 2_776 ? Cs1 O3 3.264(5) . ? Cs1 O4 3.524(14) . ? N1 C1 1.330(7) . ? N1 C5 1.377(8) . ? N1 Cs1 3.255(5) 2_776 ? N2 C5 1.335(7) . ? N2 Si1 1.683(5) . ? N2 Cs1 3.092(5) 2_776 ? C1 C2 1.371(9) . ? C2 C3 1.398(9) . ? C3 C4 1.341(8) . ? C4 C5 1.422(8) . ? Si1 C8 1.865(7) . ? Si1 C6 1.868(8) . ? Si1 C7 1.884(6) . ? O1 C9 1.376(9) . ? O1 C16 1.467(9) . ? O2 C11 1.356(10) . ? O2 C10 1.432(9) . ? O3 C13 1.356(10) . ? O3 C12 1.469(10) . ? O4 C15 1.023(14) . ? O4 C14 1.293(13) . ? C9 C10 1.503(11) . ? C11 C12 1.474(13) . ? C13 C14 1.528(14) . ? C15 C16 1.499(17) . ? 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 Cs1 O2 110.79(14) 2_776 . ? N2 Cs1 N2 100.33(13) 2_776 . ? O2 Cs1 N2 146.31(14) . . ? N2 Cs1 O1 96.15(13) 2_776 . ? O2 Cs1 O1 53.78(13) . . ? N2 Cs1 O1 136.55(13) . . ? N2 Cs1 N1 87.83(13) 2_776 . ? O2 Cs1 N1 147.65(12) . . ? N2 Cs1 N1 41.99(12) . . ? O1 Cs1 N1 99.53(13) . . ? N2 Cs1 N1 42.61(12) 2_776 2_776 ? O2 Cs1 N1 108.05(12) . 2_776 ? N2 Cs1 N1 86.06(13) . 2_776 ? O1 Cs1 N1 130.47(14) . 2_776 ? N1 Cs1 N1 103.51(10) . 2_776 ? N2 Cs1 O3 163.16(15) 2_776 . ? O2 Cs1 O3 53.02(14) . . ? N2 Cs1 O3 94.59(13) . . ? O1 Cs1 O3 77.95(12) . . ? N1 Cs1 O3 108.61(15) . . ? N1 Cs1 O3 131.98(14) 2_776 . ? N2 Cs1 O4 138.1(2) 2_776 . ? O2 Cs1 O4 71.3(3) . . ? N2 Cs1 O4 94.1(3) . . ? O1 Cs1 O4 49.7(3) . . ? N1 Cs1 O4 77.2(3) . . ? N1 Cs1 O4 179.1(2) 2_776 . ? O3 Cs1 O4 47.1(2) . . ? C1 N1 C5 118.3(5) . . ? C1 N1 Cs1 124.6(4) . . ? C5 N1 Cs1 84.6(3) . . ? C1 N1 Cs1 141.3(4) . 2_776 ? C5 N1 Cs1 93.6(3) . 2_776 ? Cs1 N1 Cs1 76.49(10) . 2_776 ? C5 N2 Si1 131.8(5) . . ? C5 N2 Cs1 102.0(3) . 2_776 ? Si1 N2 Cs1 122.1(2) . 2_776 ? C5 N2 Cs1 87.6(4) . . ? Si1 N2 Cs1 116.7(2) . . ? Cs1 N2 Cs1 79.67(13) 2_776 . ? N1 C1 C2 125.5(6) . . ? C1 C2 C3 117.2(6) . . ? C4 C3 C2 118.6(6) . . ? C3 C4 C5 122.8(6) . . ? N2 C5 N1 116.8(5) . . ? N2 C5 C4 125.6(6) . . ? N1 C5 C4 117.6(5) . . ? N2 Si1 C8 106.1(3) . . ? N2 Si1 C6 114.8(3) . . ? C8 Si1 C6 106.6(4) . . ? N2 Si1 C7 114.0(3) . . ? C8 Si1 C7 108.0(3) . . ? C6 Si1 C7 106.8(3) . . ? C9 O1 C16 111.6(6) . . ? C9 O1 Cs1 119.8(5) . . ? C16 O1 Cs1 111.8(5) . . ? C11 O2 C10 112.9(7) . . ? C11 O2 Cs1 127.0(5) . . ? C10 O2 Cs1 109.6(4) . . ? C13 O3 C12 112.3(7) . . ? C13 O3 Cs1 130.6(6) . . ? C12 O3 Cs1 104.3(5) . . ? C15 O4 C14 141(2) . . ? C15 O4 Cs1 112.6(14) . . ? C14 O4 Cs1 106.4(9) . . ? O1 C9 C10 108.4(7) . . ? O2 C10 C9 112.7(6) . . ? O2 C11 C12 108.2(7) . . ? O3 C12 C11 115.0(7) . . ? O3 C13 C14 106.2(8) . . ? O4 C14 C13 112.3(9) . . ? O4 C15 C16 131.7(17) . . ? O1 C16 C15 111.7(7) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.498 _refine_diff_density_min -1.656 _refine_diff_density_rms 0.124 #===END