# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Izod, Keith' 'Watson, James' 'Clegg, William' 'Harrington, Ross' _publ_contact_author_name 'Izod, Keith' _publ_contact_author_email k.j.izod@ncl.ac.uk _publ_section_title ; Synthesis, Structures and Stabilities of Thioanisole-Functionalised Phosphido-Borane Complexes of the Alkali Metals ; # Attachment '- dalton.cif' data_ki397_compound_10 _database_code_depnum_ccdc_archive 'CCDC 836010' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H74 B2 Li2 O2 P2 S2 Si4' _chemical_formula_sum 'C36 H74 B2 Li2 O2 P2 S2 Si4' _chemical_formula_weight 812.87 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4504(5) _cell_length_b 16.2605(5) _cell_length_c 11.2638(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.733(4) _cell_angle_gamma 90.00 _cell_volume 2393.08(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7105 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 29.45 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.908 _exptl_absorpt_correction_T_max 0.914 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 15640 _diffrn_reflns_av_R_equivalents 0.0312 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 29.52 _reflns_number_total 5823 _reflns_number_gt 4054 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _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^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5823 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _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 P P 0.68642(3) 0.53374(2) 0.55561(3) 0.01568(9) Uani 1 1 d . . . S S 0.57870(3) 0.67116(2) 0.68670(4) 0.02749(11) Uani 1 1 d . . . Si1 Si 0.90042(3) 0.48870(2) 0.72553(4) 0.02329(11) Uani 1 1 d . . . Si2 Si 0.78281(3) 0.36421(2) 0.52500(4) 0.02378(11) Uani 1 1 d . . . O O 0.60736(8) 0.47619(6) 0.86022(9) 0.0276(2) Uani 1 1 d . . . B B 0.60858(13) 0.53093(10) 0.38466(16) 0.0206(4) Uani 1 1 d . . . H1A H 0.5416(11) 0.5762(8) 0.3783(14) 0.023(4) Uiso 1 1 d . . . H1B H 0.5767(11) 0.4669(8) 0.3624(14) 0.020(4) Uiso 1 1 d . . . H1C H 0.6568(12) 0.5525(9) 0.3204(16) 0.033(4) Uiso 1 1 d . . . Li Li 0.56587(19) 0.51126(15) 0.6939(2) 0.0244(5) Uani 1 1 d . . . C1 C 0.80859(10) 0.47556(8) 0.57092(14) 0.0183(3) Uani 1 1 d . . . H1 H 0.8433 0.5000 0.5099 0.022 Uiso 1 1 calc R . . C2 C 1.03355(13) 0.47488(12) 0.7055(2) 0.0456(5) Uani 1 1 d . . . H2A H 1.0827 0.4850 0.7835 0.068 Uiso 1 1 calc R . . H2B H 1.0458 0.5138 0.6441 0.068 Uiso 1 1 calc R . . H2C H 1.0419 0.4186 0.6784 0.068 Uiso 1 1 calc R . . C3 C 0.87316(14) 0.41364(10) 0.83979(16) 0.0357(4) Uani 1 1 d . . . H3A H 0.9121 0.4290 0.9218 0.054 Uiso 1 1 calc R . . H3B H 0.8932 0.3583 0.8201 0.054 Uiso 1 1 calc R . . H3C H 0.7998 0.4143 0.8373 0.054 Uiso 1 1 calc R . . C4 C 0.90056(13) 0.59185(9) 0.79911(16) 0.0353(4) Uani 1 1 d . . . H4A H 0.9472 0.5909 0.8804 0.053 Uiso 1 1 calc R . . H4B H 0.8312 0.6050 0.8067 0.053 Uiso 1 1 calc R . . H4C H 0.9233 0.6337 0.7487 0.053 Uiso 1 1 calc R . . C5 C 0.75185(15) 0.35175(10) 0.35571(16) 0.0406(4) Uani 1 1 d . . . H5A H 0.7356 0.2940 0.3348 0.061 Uiso 1 1 calc R . . H5B H 0.8109 0.3685 0.3245 0.061 Uiso 1 1 calc R . . H5C H 0.6928 0.3862 0.3188 0.061 Uiso 1 1 calc R . . C6 C 0.89786(15) 0.29652(10) 0.5787(2) 0.0480(5) Uani 1 1 d . . . H6A H 0.8810 0.2402 0.5500 0.072 Uiso 1 1 calc R . . H6B H 0.9181 0.2970 0.6682 0.072 Uiso 1 1 calc R . . H6C H 0.9544 0.3170 0.5459 0.072 Uiso 1 1 calc R . . C7 C 0.67589(13) 0.32336(9) 0.58617(18) 0.0368(4) Uani 1 1 d . . . H7A H 0.6674 0.2645 0.5679 0.055 Uiso 1 1 calc R . . H7B H 0.6125 0.3524 0.5480 0.055 Uiso 1 1 calc R . . H7C H 0.6913 0.3316 0.6749 0.055 Uiso 1 1 calc R . . C8 C 0.72994(10) 0.64173(8) 0.56771(13) 0.0173(3) Uani 1 1 d . . . C9 C 0.80753(11) 0.66821(8) 0.51376(15) 0.0250(3) Uani 1 1 d . . . H9 H 0.8348 0.6308 0.4650 0.030 Uiso 1 1 calc R . . C10 C 0.84602(12) 0.74764(9) 0.52931(17) 0.0309(4) Uani 1 1 d . . . H10 H 0.8991 0.7642 0.4919 0.037 Uiso 1 1 calc R . . C11 C 0.80647(12) 0.80235(9) 0.59958(17) 0.0306(4) Uani 1 1 d . . . H11 H 0.8345 0.8561 0.6136 0.037 Uiso 1 1 calc R . . C12 C 0.72660(12) 0.77962(8) 0.64961(15) 0.0251(3) Uani 1 1 d . . . H12 H 0.6983 0.8183 0.6956 0.030 Uiso 1 1 calc R . . C13 C 0.68715(10) 0.70014(8) 0.63303(14) 0.0186(3) Uani 1 1 d . . . C14 C 0.58247(13) 0.73616(9) 0.81586(16) 0.0326(4) Uani 1 1 d . . . H14A H 0.5729 0.7935 0.7889 0.049 Uiso 1 1 calc R . . H14B H 0.6488 0.7302 0.8743 0.049 Uiso 1 1 calc R . . H14C H 0.5277 0.7203 0.8552 0.049 Uiso 1 1 calc R . . C15 C 0.67274(12) 0.52371(10) 0.95614(15) 0.0295(4) Uani 1 1 d . . . H15A H 0.6361 0.5728 0.9757 0.035 Uiso 1 1 calc R . . H15B H 0.7349 0.5420 0.9309 0.035 Uiso 1 1 calc R . . C16 C 0.70091(12) 0.46718(10) 1.06532(15) 0.0320(4) Uani 1 1 d . . . H16A H 0.7144 0.4984 1.1430 0.038 Uiso 1 1 calc R . . H16B H 0.7615 0.4333 1.0629 0.038 Uiso 1 1 calc R . . C17 C 0.60511(12) 0.41472(9) 1.04935(15) 0.0286(4) Uani 1 1 d . . . H17A H 0.6204 0.3613 1.0919 0.034 Uiso 1 1 calc R . . H17B H 0.5514 0.4434 1.0803 0.034 Uiso 1 1 calc R . . C18 C 0.57304(13) 0.40325(9) 0.91242(15) 0.0301(4) Uani 1 1 d . . . H18A H 0.6053 0.3535 0.8876 0.036 Uiso 1 1 calc R . . H18B H 0.4978 0.3976 0.8851 0.036 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 P 0.01758(18) 0.01354(17) 0.0160(2) 0.00064(14) 0.00411(15) -0.00028(13) S 0.0286(2) 0.0257(2) 0.0315(2) -0.01102(17) 0.01379(18) -0.00699(16) Si1 0.0200(2) 0.0259(2) 0.0214(2) 0.00103(17) -0.00007(18) 0.00226(17) Si2 0.0318(2) 0.0160(2) 0.0227(2) -0.00125(16) 0.00471(19) 0.00448(17) O 0.0337(6) 0.0318(6) 0.0152(6) 0.0026(5) 0.0015(5) -0.0089(5) B 0.0217(8) 0.0203(8) 0.0181(9) 0.0007(7) 0.0014(7) -0.0022(7) Li 0.0246(13) 0.0298(13) 0.0184(14) 0.0026(11) 0.0041(11) -0.0035(10) C1 0.0197(7) 0.0174(7) 0.0186(8) 0.0019(6) 0.0060(6) 0.0024(6) C2 0.0227(9) 0.0598(12) 0.0516(13) 0.0033(10) 0.0037(9) 0.0044(8) C3 0.0470(11) 0.0356(9) 0.0223(10) 0.0043(7) 0.0038(8) 0.0047(8) C4 0.0398(10) 0.0314(9) 0.0265(10) -0.0050(7) -0.0082(8) -0.0029(7) C5 0.0587(12) 0.0332(9) 0.0284(10) -0.0097(8) 0.0071(9) 0.0071(8) C6 0.0543(12) 0.0338(10) 0.0514(14) -0.0087(9) 0.0037(10) 0.0207(8) C7 0.0494(11) 0.0204(8) 0.0407(11) 0.0015(7) 0.0108(9) -0.0071(7) C8 0.0182(7) 0.0147(6) 0.0166(8) 0.0017(6) -0.0003(6) 0.0003(5) C9 0.0254(8) 0.0194(7) 0.0321(10) 0.0029(6) 0.0107(7) 0.0023(6) C10 0.0260(8) 0.0231(8) 0.0463(11) 0.0082(7) 0.0140(8) -0.0017(6) C11 0.0312(9) 0.0149(7) 0.0435(11) 0.0025(7) 0.0041(8) -0.0059(6) C12 0.0278(8) 0.0181(7) 0.0278(9) -0.0037(6) 0.0035(7) 0.0003(6) C13 0.0178(7) 0.0181(7) 0.0177(8) 0.0008(6) 0.0001(6) 0.0003(5) C14 0.0443(10) 0.0267(8) 0.0315(10) -0.0087(7) 0.0180(8) -0.0008(7) C15 0.0293(9) 0.0360(9) 0.0218(9) -0.0020(7) 0.0034(7) -0.0093(7) C16 0.0280(9) 0.0459(10) 0.0201(9) -0.0008(7) 0.0016(7) 0.0018(7) C17 0.0378(9) 0.0280(8) 0.0204(9) 0.0044(7) 0.0079(7) 0.0040(7) C18 0.0419(10) 0.0264(8) 0.0208(9) 0.0030(7) 0.0052(8) -0.0051(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 P B 1.9617(18) . ? P Li 2.527(3) . ? P C1 1.8682(14) . ? P C8 1.8459(13) . ? S Li 2.608(2) . ? S C13 1.7702(15) . ? S C14 1.7891(16) . ? Si1 C1 1.8928(15) . ? Si1 C2 1.8708(18) . ? Si1 C3 1.8720(17) . ? Si1 C4 1.8707(16) . ? Si2 C1 1.8923(14) . ? Si2 C5 1.8637(18) . ? Si2 C6 1.8781(17) . ? Si2 C7 1.8587(18) . ? O Li 1.910(3) . ? O C15 1.4446(18) . ? O C18 1.4472(18) . ? B H1A 1.152(14) . ? B H1B 1.132(14) . ? B H1C 1.135(17) . ? Li H1A 2.053(14) 3_666 ? Li H1B 1.905(14) 3_666 ? C1 H1 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.395(2) . ? C8 C13 1.4056(19) . ? C9 H9 0.950 . ? C9 C10 1.387(2) . ? C10 H10 0.950 . ? C10 C11 1.379(2) . ? C11 H11 0.950 . ? C11 C12 1.377(2) . ? C12 H12 0.950 . ? C12 C13 1.3928(19) . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C15 C16 1.510(2) . ? C16 H16A 0.990 . ? C16 H16B 0.990 . ? C16 C17 1.520(2) . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.511(2) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? 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 B P Li 109.30(8) . . ? B P C1 109.36(7) . . ? B P C8 100.40(7) . . ? Li P C1 123.28(7) . . ? Li P C8 109.31(7) . . ? C1 P C8 102.61(6) . . ? Li S C13 109.99(7) . . ? Li S C14 123.56(8) . . ? C13 S C14 104.71(7) . . ? C1 Si1 C2 108.04(8) . . ? C1 Si1 C3 111.56(7) . . ? C1 Si1 C4 116.15(7) . . ? C2 Si1 C3 110.73(9) . . ? C2 Si1 C4 105.11(9) . . ? C3 Si1 C4 105.05(8) . . ? C1 Si2 C5 111.44(7) . . ? C1 Si2 C6 112.91(8) . . ? C1 Si2 C7 110.38(7) . . ? C5 Si2 C6 103.46(9) . . ? C5 Si2 C7 109.62(9) . . ? C6 Si2 C7 108.79(9) . . ? Li O C15 123.92(12) . . ? Li O C18 126.58(11) . . ? C15 O C18 109.31(11) . . ? P B H1A 105.9(8) . . ? P B H1B 108.9(8) . . ? P B H1C 111.5(8) . . ? H1A B H1B 108.9(10) . . ? H1A B H1C 108.6(11) . . ? H1B B H1C 112.8(11) . . ? P Li S 77.28(7) . . ? P Li O 124.52(12) . . ? P Li H1A 110.5(4) . 3_666 ? P Li H1B 120.7(5) . 3_666 ? S Li O 108.78(11) . . ? S Li H1A 136.4(4) . 3_666 ? S Li H1B 82.7(4) . 3_666 ? O Li H1A 101.3(4) . 3_666 ? O Li H1B 114.8(5) . 3_666 ? H1A Li H1B 55.9(6) 3_666 3_666 ? P C1 Si1 113.28(7) . . ? P C1 Si2 111.05(7) . . ? P C1 H1 106.2 . . ? Si1 C1 Si2 113.37(7) . . ? Si1 C1 H1 106.2 . . ? Si2 C1 H1 106.2 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P C8 C9 121.23(11) . . ? P C8 C13 121.29(10) . . ? C9 C8 C13 117.47(12) . . ? C8 C9 H9 119.1 . . ? C8 C9 C10 121.86(14) . . ? H9 C9 C10 119.1 . . ? C9 C10 H10 120.3 . . ? C9 C10 C11 119.35(14) . . ? H10 C10 C11 120.3 . . ? C10 C11 H11 119.8 . . ? C10 C11 C12 120.44(13) . . ? H11 C11 C12 119.8 . . ? C11 C12 H12 119.9 . . ? C11 C12 C13 120.24(14) . . ? H12 C12 C13 119.9 . . ? S C13 C8 118.16(10) . . ? S C13 C12 121.32(11) . . ? C8 C13 C12 120.45(13) . . ? S C14 H14A 109.5 . . ? S C14 H14B 109.5 . . ? S C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O C15 H15A 110.6 . . ? O C15 H15B 110.6 . . ? O C15 C16 105.91(12) . . ? H15A C15 H15B 108.7 . . ? H15A C15 C16 110.6 . . ? H15B C15 C16 110.6 . . ? C15 C16 H16A 111.4 . . ? C15 C16 H16B 111.4 . . ? C15 C16 C17 101.74(12) . . ? H16A C16 H16B 109.3 . . ? H16A C16 C17 111.4 . . ? H16B C16 C17 111.4 . . ? C16 C17 H17A 111.2 . . ? C16 C17 H17B 111.2 . . ? C16 C17 C18 102.63(13) . . ? H17A C17 H17B 109.2 . . ? H17A C17 C18 111.2 . . ? H17B C17 C18 111.2 . . ? O C18 C17 105.80(12) . . ? O C18 H18A 110.6 . . ? O C18 H18B 110.6 . . ? C17 C18 H18A 110.6 . . ? C17 C18 H18B 110.6 . . ? H18A C18 H18B 108.7 . . ? _diffrn_measured_fraction_theta_max 0.870 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.611 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.047 # Contents of RES file _computing_special_details ; TITL ki397 in P2(1)/c CELL 0.71073 13.4504 16.2605 11.2638 90.0000 103.733 90.0000 ZERR 2.00 0.0005 0.0005 0.0004 0.0000 0.004 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H O S Si Li B P UNIT 72 148 4 4 8 4 4 4 REM colourless block SIZE 0.32 0.30 0.30 TEMP -123 L.S. 8 ACTA 52 BOND $H EQIV $1 -x+1, -y+1, -z+1 BIND LI H1A_$1 BIND LI H1B_$1 FREE LI B_$1 FREE B LI_$1 BIND H1A LI_$1 BIND H1B LI_$1 FMAP 2 PLAN 10 REM EXTI 0.000000 WGHT 0.040400 FVAR 2.85744 P 8 0.686417 0.533735 0.555606 11.00000 0.01758 0.01354 = 0.01600 0.00064 0.00411 -0.00028 S 4 0.578705 0.671164 0.686702 11.00000 0.02861 0.02567 = 0.03153 -0.01102 0.01379 -0.00699 SI1 5 0.900415 0.488698 0.725528 11.00000 0.02002 0.02593 = 0.02142 0.00103 -0.00007 0.00226 SI2 5 0.782814 0.364208 0.525002 11.00000 0.03178 0.01599 = 0.02267 -0.00125 0.00471 0.00448 O 3 0.607358 0.476186 0.860216 11.00000 0.03366 0.03179 = 0.01519 0.00259 0.00154 -0.00888 B 7 0.608583 0.530930 0.384662 11.00000 0.02167 0.02029 = 0.01811 0.00069 0.00142 -0.00218 H1A 2 0.541629 0.576179 0.378290 11.00000 0.02332 H1B 2 0.576693 0.466876 0.362423 11.00000 0.02040 H1C 2 0.656754 0.552544 0.320431 11.00000 0.03252 LI 6 0.565871 0.511258 0.693894 11.00000 0.02457 0.02977 = 0.01836 0.00256 0.00409 -0.00354 C1 1 0.808587 0.475557 0.570916 11.00000 0.01974 0.01737 = 0.01864 0.00186 0.00602 0.00240 AFIX 13 H1 2 0.843252 0.500045 0.509925 11.00000 -1.20000 AFIX 0 C2 1 1.033549 0.474881 0.705496 11.00000 0.02271 0.05981 = 0.05163 0.00331 0.00374 0.00441 AFIX 137 H2A 2 1.082721 0.484993 0.783492 11.00000 -1.50000 H2B 2 1.045786 0.513841 0.644118 11.00000 -1.50000 H2C 2 1.041881 0.418573 0.678384 11.00000 -1.50000 AFIX 0 C3 1 0.873157 0.413643 0.839793 11.00000 0.04696 0.03564 = 0.02230 0.00435 0.00382 0.00474 AFIX 137 H3A 2 0.912119 0.429027 0.921788 11.00000 -1.50000 H3B 2 0.893245 0.358306 0.820087 11.00000 -1.50000 H3C 2 0.799838 0.414304 0.837323 11.00000 -1.50000 AFIX 0 C4 1 0.900564 0.591847 0.799110 11.00000 0.03982 0.03143 = 0.02649 -0.00504 -0.00820 -0.00285 AFIX 137 H4A 2 0.947227 0.590911 0.880441 11.00000 -1.50000 H4B 2 0.831236 0.604997 0.806700 11.00000 -1.50000 H4C 2 0.923305 0.633670 0.748736 11.00000 -1.50000 AFIX 0 C5 1 0.751849 0.351753 0.355711 11.00000 0.05867 0.03316 = 0.02844 -0.00965 0.00709 0.00709 AFIX 137 H5A 2 0.735636 0.294009 0.334765 11.00000 -1.50000 H5B 2 0.810860 0.368535 0.324512 11.00000 -1.50000 H5C 2 0.692767 0.386165 0.318838 11.00000 -1.50000 AFIX 0 C6 1 0.897857 0.296524 0.578704 11.00000 0.05432 0.03383 = 0.05140 -0.00870 0.00369 0.02073 AFIX 137 H6A 2 0.881014 0.240181 0.550004 11.00000 -1.50000 H6B 2 0.918147 0.297031 0.668213 11.00000 -1.50000 H6C 2 0.954442 0.317041 0.545916 11.00000 -1.50000 AFIX 0 C7 1 0.675886 0.323362 0.586172 11.00000 0.04938 0.02043 = 0.04069 0.00149 0.01078 -0.00707 AFIX 137 H7A 2 0.667396 0.264492 0.567947 11.00000 -1.50000 H7B 2 0.612548 0.352438 0.547969 11.00000 -1.50000 H7C 2 0.691338 0.331621 0.674852 11.00000 -1.50000 AFIX 0 C8 1 0.729942 0.641732 0.567707 11.00000 0.01824 0.01473 = 0.01658 0.00168 -0.00033 0.00032 C9 1 0.807529 0.668208 0.513755 11.00000 0.02541 0.01935 = 0.03214 0.00290 0.01070 0.00234 AFIX 43 H9 2 0.834791 0.630782 0.464966 11.00000 -1.20000 AFIX 0 C10 1 0.846017 0.747636 0.529313 11.00000 0.02595 0.02315 = 0.04629 0.00819 0.01396 -0.00166 AFIX 43 H10 2 0.899107 0.764177 0.491917 11.00000 -1.20000 AFIX 0 C11 1 0.806474 0.802348 0.599581 11.00000 0.03119 0.01487 = 0.04349 0.00255 0.00415 -0.00594 AFIX 43 H11 2 0.834524 0.856087 0.613575 11.00000 -1.20000 AFIX 0 C12 1 0.726601 0.779624 0.649611 11.00000 0.02782 0.01808 = 0.02783 -0.00369 0.00346 0.00033 AFIX 43 H12 2 0.698295 0.818301 0.695604 11.00000 -1.20000 AFIX 0 C13 1 0.687150 0.700139 0.633034 11.00000 0.01785 0.01814 = 0.01766 0.00083 0.00009 0.00027 C14 1 0.582472 0.736156 0.815864 11.00000 0.04425 0.02670 = 0.03153 -0.00874 0.01802 -0.00077 AFIX 137 H14A 2 0.572941 0.793515 0.788853 11.00000 -1.50000 H14B 2 0.648845 0.730223 0.874288 11.00000 -1.50000 H14C 2 0.527696 0.720328 0.855202 11.00000 -1.50000 AFIX 0 C15 1 0.672738 0.523708 0.956144 11.00000 0.02932 0.03601 = 0.02181 -0.00197 0.00339 -0.00925 AFIX 23 H15A 2 0.636096 0.572784 0.975744 11.00000 -1.20000 H15B 2 0.734851 0.541990 0.930889 11.00000 -1.20000 AFIX 0 C16 1 0.700913 0.467178 1.065321 11.00000 0.02800 0.04590 = 0.02008 -0.00084 0.00158 0.00185 AFIX 23 H16A 2 0.714446 0.498400 1.142961 11.00000 -1.20000 H16B 2 0.761547 0.433296 1.062870 11.00000 -1.20000 AFIX 0 C17 1 0.605107 0.414718 1.049352 11.00000 0.03784 0.02801 = 0.02038 0.00439 0.00791 0.00399 AFIX 23 H17A 2 0.620398 0.361296 1.091933 11.00000 -1.20000 H17B 2 0.551436 0.443425 1.080306 11.00000 -1.20000 AFIX 0 C18 1 0.573037 0.403249 0.912419 11.00000 0.04194 0.02640 = 0.02078 0.00296 0.00522 -0.00514 AFIX 23 H18A 2 0.605332 0.353467 0.887560 11.00000 -1.20000 H18B 2 0.497772 0.397578 0.885127 11.00000 -1.20000 HKLF 4 REM ki397 in P2(1)/c REM R1 = 0.0324 for 4054 Fo > 4sig(Fo) and 0.0539 for all 5823 data REM 245 parameters refined using 0 restraints END ; #===END data_ki385_compound_11 _database_code_depnum_ccdc_archive 'CCDC 836011' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H45 B N2 Na P S Si2' _chemical_formula_sum 'C20 H45 B N2 Na P S Si2' _chemical_formula_weight 466.59 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3566(9) _cell_length_b 13.2652(10) _cell_length_c 21.1564(18) _cell_angle_alpha 93.397(7) _cell_angle_beta 104.760(7) _cell_angle_gamma 97.552(6) _cell_volume 3040.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3364 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 29.65 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.019 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube with Enhance optics' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 26610 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.2516 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10697 _reflns_number_gt 4259 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _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^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10697 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1302 _refine_ls_R_factor_gt 0.0476 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 0.698 _refine_ls_restrained_S_all 0.698 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 1.00511(9) 1.17684(7) 0.20061(5) 0.0236(3) Uani 1 1 d . . . P2 P 1.06188(9) 1.69934(7) 0.32537(5) 0.0236(3) Uani 1 1 d . . . S1 S 0.95454(9) 1.37242(7) 0.12782(5) 0.0310(3) Uani 1 1 d . . . S2 S 1.08131(10) 1.91642(7) 0.40135(5) 0.0349(3) Uani 1 1 d . . . Si1 Si 0.72586(11) 1.07662(8) 0.11905(6) 0.0351(3) Uani 1 1 d . . . Si2 Si 0.80171(10) 1.14743(8) 0.27262(6) 0.0302(3) Uani 1 1 d . . . Si3 Si 0.85280(11) 1.62035(8) 0.39816(6) 0.0351(3) Uani 1 1 d . . . Si4 Si 0.79259(10) 1.64132(8) 0.24352(6) 0.0315(3) Uani 1 1 d . . . B1 B 1.0690(5) 1.0534(3) 0.2304(3) 0.0308(12) Uani 1 1 d . . . H1A H 1.062(3) 1.048(2) 0.2854(18) 0.035(10) Uiso 1 1 d . . . H1B H 1.170(3) 1.068(2) 0.2304(17) 0.039(10) Uiso 1 1 d . . . H1C H 1.017(3) 0.980(3) 0.1910(19) 0.060(12) Uiso 1 1 d . . . B2 B 1.1013(5) 1.5682(3) 0.2961(3) 0.0290(12) Uani 1 1 d . . . H2A H 1.200(3) 1.582(2) 0.2981(16) 0.031(9) Uiso 1 1 d . . . H2B H 1.048(3) 1.551(2) 0.2394(18) 0.031(10) Uiso 1 1 d . . . H2C H 1.076(3) 1.503(2) 0.3227(16) 0.032(9) Uiso 1 1 d . . . Na1 Na 1.14221(12) 1.38040(9) 0.26025(7) 0.0285(4) Uani 1 1 d . . . Na2 Na 1.15229(13) 1.88511(9) 0.27153(7) 0.0292(4) Uani 1 1 d . . . N1 N 1.3170(3) 1.3445(2) 0.35410(16) 0.0309(8) Uani 1 1 d . . . N2 N 1.3244(3) 1.3876(2) 0.21396(17) 0.0313(8) Uani 1 1 d . . . N3 N 1.3803(3) 1.9035(2) 0.32563(17) 0.0331(9) Uani 1 1 d . . . N4 N 1.2453(3) 1.8193(2) 0.18329(16) 0.0330(9) Uani 1 1 d . . . C1 C 0.8335(3) 1.1615(2) 0.19069(18) 0.0199(9) Uani 1 1 d . . . H1 H 0.8136 1.2312 0.1811 0.024 Uiso 1 1 calc R . . C2 C 0.7246(4) 1.1280(3) 0.0396(2) 0.0516(13) Uani 1 1 d . . . H2D H 0.7134 1.2000 0.0425 0.077 Uiso 1 1 calc R . . H2E H 0.6568 1.0891 0.0050 0.077 Uiso 1 1 calc R . . H2F H 0.8030 1.1223 0.0293 0.077 Uiso 1 1 calc R . . C3 C 0.7614(4) 0.9434(3) 0.1133(2) 0.0549(13) Uani 1 1 d . . . H3A H 0.7046 0.9043 0.0742 0.082 Uiso 1 1 calc R . . H3B H 0.7521 0.9110 0.1525 0.082 Uiso 1 1 calc R . . H3C H 0.8463 0.9451 0.1102 0.082 Uiso 1 1 calc R . . C4 C 0.5625(4) 1.0670(3) 0.1239(2) 0.0592(14) Uani 1 1 d . . . H4A H 0.5400 1.1356 0.1268 0.089 Uiso 1 1 calc R . . H4B H 0.5541 1.0335 0.1630 0.089 Uiso 1 1 calc R . . H4C H 0.5079 1.0268 0.0846 0.089 Uiso 1 1 calc R . . C5 C 0.6588(4) 1.2030(3) 0.2736(2) 0.0468(12) Uani 1 1 d . . . H5A H 0.6564 1.2637 0.2493 0.070 Uiso 1 1 calc R . . H5B H 0.6590 1.2221 0.3191 0.070 Uiso 1 1 calc R . . H5C H 0.5862 1.1522 0.2528 0.070 Uiso 1 1 calc R . . C6 C 0.7803(4) 1.0111(3) 0.2908(2) 0.0462(12) Uani 1 1 d . . . H6A H 0.8538 0.9810 0.2890 0.069 Uiso 1 1 calc R . . H6B H 0.7084 0.9730 0.2582 0.069 Uiso 1 1 calc R . . H6C H 0.7674 1.0077 0.3347 0.069 Uiso 1 1 calc R . . C7 C 0.9276(4) 1.2199(3) 0.33930(19) 0.0437(12) Uani 1 1 d . . . H7A H 0.9408 1.2914 0.3301 0.065 Uiso 1 1 calc R . . H7B H 1.0034 1.1905 0.3421 0.065 Uiso 1 1 calc R . . H7C H 0.9056 1.2161 0.3811 0.065 Uiso 1 1 calc R . . C8 C 1.0245(3) 1.1855(3) 0.11762(18) 0.0229(9) Uani 1 1 d . . . C9 C 1.0681(3) 1.1100(3) 0.0864(2) 0.0281(10) Uani 1 1 d . . . H9 H 1.0781 1.0481 0.1061 0.034 Uiso 1 1 calc R . . C10 C 1.0978(3) 1.1207(3) 0.0275(2) 0.0332(10) Uani 1 1 d . . . H10 H 1.1285 1.0676 0.0075 0.040 Uiso 1 1 calc R . . C11 C 1.0821(3) 1.2102(3) -0.00192(19) 0.0326(10) Uani 1 1 d . . . H11 H 1.1028 1.2194 -0.0422 0.039 Uiso 1 1 calc R . . C12 C 1.0362(3) 1.2862(3) 0.0275(2) 0.0293(10) Uani 1 1 d . . . H12 H 1.0234 1.3469 0.0067 0.035 Uiso 1 1 calc R . . C13 C 1.0087(3) 1.2754(2) 0.08653(19) 0.0220(9) Uani 1 1 d . . . C14 C 0.9587(4) 1.4773(3) 0.0782(2) 0.0416(12) Uani 1 1 d . . . H14A H 0.9070 1.4555 0.0335 0.062 Uiso 1 1 calc R . . H14B H 1.0437 1.4994 0.0768 0.062 Uiso 1 1 calc R . . H14C H 0.9276 1.5341 0.0971 0.062 Uiso 1 1 calc R . . C15 C 1.3278(4) 1.4757(3) 0.1763(2) 0.0509(13) Uani 1 1 d . . . H15A H 1.4064 1.4869 0.1647 0.076 Uiso 1 1 calc R . . H15B H 1.3195 1.5362 0.2027 0.076 Uiso 1 1 calc R . . H15C H 1.2599 1.4631 0.1361 0.076 Uiso 1 1 calc R . . C16 C 1.3349(4) 1.2969(3) 0.1737(2) 0.0424(12) Uani 1 1 d . . . H16A H 1.4179 1.3031 0.1673 0.064 Uiso 1 1 calc R . . H16B H 1.2740 1.2912 0.1310 0.064 Uiso 1 1 calc R . . H16C H 1.3196 1.2357 0.1960 0.064 Uiso 1 1 calc R . . C17 C 1.4254(4) 1.4074(3) 0.2736(2) 0.0350(11) Uani 1 1 d . . . H17A H 1.4270 1.4767 0.2943 0.042 Uiso 1 1 calc R . . H17B H 1.5041 1.4064 0.2617 0.042 Uiso 1 1 calc R . . C18 C 1.4161(3) 1.3314(3) 0.3227(2) 0.0359(11) Uani 1 1 d . . . H18A H 1.4008 1.2614 0.3004 0.043 Uiso 1 1 calc R . . H18B H 1.4955 1.3394 0.3569 0.043 Uiso 1 1 calc R . . C19 C 1.3563(4) 1.4285(3) 0.4064(2) 0.0417(12) Uani 1 1 d . . . H19A H 1.4294 1.4149 0.4390 0.063 Uiso 1 1 calc R . . H19B H 1.2898 1.4346 0.4274 0.063 Uiso 1 1 calc R . . H19C H 1.3763 1.4924 0.3877 0.063 Uiso 1 1 calc R . . C20 C 1.2852(4) 1.2503(3) 0.3837(2) 0.0423(12) Uani 1 1 d . . . H20A H 1.3581 1.2363 0.4163 0.063 Uiso 1 1 calc R . . H20B H 1.2566 1.1930 0.3494 0.063 Uiso 1 1 calc R . . H20C H 1.2197 1.2590 0.4052 0.063 Uiso 1 1 calc R . . C21 C 0.8958(3) 1.6842(2) 0.32812(18) 0.0227(9) Uani 1 1 d . . . H21 H 0.8816 1.7561 0.3360 0.027 Uiso 1 1 calc R . . C22 C 0.9171(4) 1.6995(3) 0.4777(2) 0.0500(13) Uani 1 1 d . . . H22A H 0.9001 1.7696 0.4726 0.075 Uiso 1 1 calc R . . H22B H 1.0063 1.7000 0.4921 0.075 Uiso 1 1 calc R . . H22C H 0.8788 1.6710 0.5107 0.075 Uiso 1 1 calc R . . C23 C 0.9005(4) 1.4914(3) 0.4071(2) 0.0485(13) Uani 1 1 d . . . H23A H 0.9901 1.4975 0.4147 0.073 Uiso 1 1 calc R . . H23B H 0.8599 1.4464 0.3669 0.073 Uiso 1 1 calc R . . H23C H 0.8766 1.4626 0.4444 0.073 Uiso 1 1 calc R . . C24 C 0.6828(4) 1.6031(3) 0.3874(2) 0.0608(14) Uani 1 1 d . . . H24A H 0.6536 1.6691 0.3811 0.091 Uiso 1 1 calc R . . H24B H 0.6640 1.5766 0.4266 0.091 Uiso 1 1 calc R . . H24C H 0.6417 1.5547 0.3489 0.091 Uiso 1 1 calc R . . C25 C 0.8618(4) 1.6954(3) 0.1798(2) 0.0416(11) Uani 1 1 d . . . H25D H 0.9387 1.6685 0.1812 0.062 Uiso 1 1 calc R . . H25E H 0.8791 1.7700 0.1882 0.062 Uiso 1 1 calc R . . H25F H 0.8041 1.6762 0.1363 0.062 Uiso 1 1 calc R . . C26 C 0.7582(4) 1.5000(3) 0.2253(2) 0.0410(11) Uani 1 1 d . . . H26A H 0.8354 1.4720 0.2305 0.062 Uiso 1 1 calc R . . H26B H 0.7070 1.4826 0.1801 0.062 Uiso 1 1 calc R . . H26C H 0.7140 1.4708 0.2558 0.062 Uiso 1 1 calc R . . C27 C 0.6429(4) 1.6921(3) 0.2331(2) 0.0498(13) Uani 1 1 d . . . H25A H 0.5937 1.6549 0.2586 0.075 Uiso 1 1 calc R . . H25B H 0.5975 1.6830 0.1866 0.075 Uiso 1 1 calc R . . H25C H 0.6593 1.7649 0.2487 0.075 Uiso 1 1 calc R . . C28 C 1.1520(3) 1.7292(2) 0.41139(18) 0.0238(9) Uani 1 1 d . . . C29 C 1.2209(3) 1.6602(3) 0.4439(2) 0.0299(10) Uani 1 1 d . . . H29 H 1.2128 1.5932 0.4231 0.036 Uiso 1 1 calc R . . C30 C 1.3015(4) 1.6855(3) 0.5060(2) 0.0394(11) Uani 1 1 d . . . H30 H 1.3469 1.6361 0.5273 0.047 Uiso 1 1 calc R . . C31 C 1.3151(4) 1.7822(3) 0.5364(2) 0.0426(11) Uani 1 1 d . . . H31 H 1.3713 1.8002 0.5785 0.051 Uiso 1 1 calc R . . C32 C 1.2472(4) 1.8538(3) 0.5058(2) 0.0363(11) Uani 1 1 d . . . H32 H 1.2555 1.9202 0.5275 0.044 Uiso 1 1 calc R . . C33 C 1.1675(3) 1.8289(3) 0.4439(2) 0.0263(10) Uani 1 1 d . . . C34 C 1.1318(4) 2.0341(2) 0.4550(2) 0.0462(12) Uani 1 1 d . . . H34A H 1.1155 2.0234 0.4976 0.069 Uiso 1 1 calc R . . H34B H 1.0870 2.0876 0.4352 0.069 Uiso 1 1 calc R . . H34C H 1.2204 2.0550 0.4612 0.069 Uiso 1 1 calc R . . C35 C 1.1804(4) 1.7188(3) 0.1500(2) 0.0463(12) Uani 1 1 d . . . H35A H 1.2256 1.6933 0.1203 0.069 Uiso 1 1 calc R . . H35B H 1.0971 1.7259 0.1248 0.069 Uiso 1 1 calc R . . H35C H 1.1753 1.6706 0.1829 0.069 Uiso 1 1 calc R . . C36 C 1.2437(4) 1.8913(3) 0.1333(2) 0.0448(12) Uani 1 1 d . . . H36A H 1.2922 1.8706 0.1039 0.067 Uiso 1 1 calc R . . H36B H 1.2792 1.9601 0.1547 0.067 Uiso 1 1 calc R . . H36C H 1.1585 1.8916 0.1078 0.067 Uiso 1 1 calc R . . C37 C 1.3707(4) 1.8095(3) 0.2189(2) 0.0459(12) Uani 1 1 d . . . H37A H 1.4202 1.8028 0.1869 0.055 Uiso 1 1 calc R . . H37B H 1.3689 1.7461 0.2412 0.055 Uiso 1 1 calc R . . C38 C 1.4324(4) 1.8977(3) 0.2687(2) 0.0472(12) Uani 1 1 d . . . H38A H 1.5211 1.8923 0.2845 0.057 Uiso 1 1 calc R . . H38B H 1.4257 1.9618 0.2473 0.057 Uiso 1 1 calc R . . C39 C 1.4199(4) 1.8252(3) 0.3680(2) 0.0524(13) Uani 1 1 d . . . H39A H 1.5098 1.8304 0.3786 0.079 Uiso 1 1 calc R . . H39B H 1.3821 1.7576 0.3454 0.079 Uiso 1 1 calc R . . H39C H 1.3946 1.8348 0.4086 0.079 Uiso 1 1 calc R . . C40 C 1.4243(4) 2.0036(3) 0.3634(2) 0.0606(14) Uani 1 1 d . . . H40A H 1.5144 2.0138 0.3787 0.091 Uiso 1 1 calc R . . H40B H 1.3898 2.0068 0.4013 0.091 Uiso 1 1 calc R . . H40C H 1.3981 2.0573 0.3355 0.091 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 P1 0.0268(6) 0.0207(5) 0.0255(7) 0.0025(5) 0.0096(5) 0.0057(4) P2 0.0238(6) 0.0198(5) 0.0266(7) -0.0012(5) 0.0057(5) 0.0045(4) S1 0.0450(7) 0.0216(5) 0.0312(7) 0.0037(5) 0.0150(6) 0.0117(5) S2 0.0461(7) 0.0218(5) 0.0350(7) 0.0014(5) 0.0063(6) 0.0082(5) Si1 0.0345(8) 0.0361(7) 0.0326(8) -0.0012(6) 0.0094(6) -0.0009(5) Si2 0.0287(7) 0.0368(6) 0.0292(8) 0.0033(6) 0.0139(6) 0.0073(5) Si3 0.0366(8) 0.0314(6) 0.0378(9) -0.0019(6) 0.0145(7) 0.0002(5) Si4 0.0237(7) 0.0314(6) 0.0372(8) -0.0035(6) 0.0036(6) 0.0077(5) B1 0.036(3) 0.027(3) 0.036(4) 0.010(3) 0.017(3) 0.011(2) B2 0.032(3) 0.018(2) 0.040(4) 0.003(2) 0.013(3) 0.007(2) Na1 0.0275(9) 0.0233(8) 0.0349(10) -0.0011(7) 0.0087(8) 0.0059(6) Na2 0.0292(9) 0.0245(8) 0.0377(11) 0.0064(7) 0.0128(8) 0.0079(7) N1 0.028(2) 0.0307(18) 0.036(2) 0.0018(17) 0.0099(18) 0.0126(15) N2 0.027(2) 0.0316(19) 0.035(2) 0.0043(17) 0.0070(19) 0.0045(15) N3 0.029(2) 0.0284(19) 0.040(2) -0.0010(18) 0.0071(19) 0.0019(15) N4 0.036(2) 0.0332(19) 0.035(2) 0.0056(18) 0.0151(19) 0.0126(17) C1 0.020(2) 0.0171(19) 0.022(2) 0.0064(17) 0.0034(19) 0.0032(16) C2 0.042(3) 0.066(3) 0.033(3) -0.001(2) -0.004(2) -0.012(2) C3 0.063(3) 0.037(3) 0.055(4) -0.017(2) 0.009(3) -0.003(2) C4 0.041(3) 0.077(3) 0.051(4) -0.013(3) 0.006(3) -0.003(2) C5 0.042(3) 0.066(3) 0.040(3) 0.002(2) 0.022(3) 0.015(2) C6 0.039(3) 0.057(3) 0.049(3) 0.021(2) 0.021(3) 0.006(2) C7 0.047(3) 0.061(3) 0.024(3) -0.003(2) 0.011(2) 0.012(2) C8 0.016(2) 0.026(2) 0.027(3) 0.0026(19) 0.0037(19) 0.0075(17) C9 0.032(3) 0.022(2) 0.033(3) 0.0029(19) 0.013(2) 0.0042(18) C10 0.036(3) 0.031(2) 0.037(3) -0.001(2) 0.016(2) 0.0123(19) C11 0.044(3) 0.034(2) 0.024(3) 0.002(2) 0.017(2) 0.004(2) C12 0.034(3) 0.023(2) 0.030(3) 0.003(2) 0.008(2) 0.0026(18) C13 0.022(2) 0.020(2) 0.024(3) -0.0028(18) 0.006(2) 0.0041(16) C14 0.062(3) 0.023(2) 0.046(3) 0.007(2) 0.019(3) 0.013(2) C15 0.053(3) 0.051(3) 0.052(3) 0.015(3) 0.016(3) 0.007(2) C16 0.038(3) 0.045(3) 0.042(3) -0.005(2) 0.010(2) 0.005(2) C17 0.021(3) 0.038(2) 0.044(3) -0.006(2) 0.009(2) 0.0012(19) C18 0.027(3) 0.040(2) 0.037(3) -0.004(2) 0.000(2) 0.0127(19) C19 0.046(3) 0.044(3) 0.036(3) -0.002(2) 0.009(2) 0.019(2) C20 0.044(3) 0.043(3) 0.045(3) 0.009(2) 0.016(2) 0.014(2) C21 0.018(2) 0.0137(18) 0.035(3) -0.0040(17) 0.007(2) 0.0007(15) C22 0.060(3) 0.057(3) 0.030(3) -0.008(2) 0.019(3) -0.007(2) C23 0.064(3) 0.037(2) 0.051(3) 0.005(2) 0.029(3) 0.003(2) C24 0.047(3) 0.082(3) 0.053(4) -0.005(3) 0.022(3) -0.001(3) C25 0.043(3) 0.047(3) 0.036(3) 0.007(2) 0.007(2) 0.014(2) C26 0.033(3) 0.045(3) 0.042(3) -0.012(2) 0.010(2) 0.001(2) C27 0.036(3) 0.049(3) 0.058(4) -0.005(2) 0.000(3) 0.013(2) C28 0.022(2) 0.020(2) 0.027(3) -0.0016(19) 0.005(2) -0.0009(17) C29 0.028(3) 0.024(2) 0.034(3) -0.001(2) 0.004(2) 0.0004(18) C30 0.039(3) 0.036(3) 0.040(3) 0.007(2) 0.003(3) 0.009(2) C31 0.045(3) 0.043(3) 0.030(3) 0.004(2) -0.005(2) 0.000(2) C32 0.050(3) 0.026(2) 0.026(3) -0.007(2) 0.003(2) 0.000(2) C33 0.024(2) 0.025(2) 0.029(3) 0.002(2) 0.005(2) 0.0029(17) C34 0.067(3) 0.016(2) 0.054(3) -0.007(2) 0.018(3) 0.002(2) C35 0.046(3) 0.041(3) 0.053(3) -0.003(2) 0.016(3) 0.012(2) C36 0.057(3) 0.047(3) 0.043(3) 0.015(2) 0.025(3) 0.022(2) C37 0.035(3) 0.057(3) 0.055(3) 0.006(3) 0.019(3) 0.023(2) C38 0.028(3) 0.052(3) 0.061(4) 0.006(3) 0.012(3) 0.004(2) C39 0.036(3) 0.062(3) 0.059(4) 0.015(3) 0.010(3) 0.008(2) C40 0.050(3) 0.050(3) 0.073(4) -0.013(3) 0.010(3) -0.003(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 P1 B1 1.951(4) . ? P1 Na1 2.9661(17) . ? P1 C1 1.888(3) . ? P1 C8 1.833(4) . ? P2 B2 1.957(4) . ? P2 Na2 2.9474(16) . ? P2 C21 1.887(3) . ? P2 C28 1.837(4) . ? S1 Na1 3.0441(19) . ? S1 C13 1.773(3) . ? S1 C14 1.795(3) . ? S2 Na2 3.0735(18) . ? S2 C33 1.758(4) . ? S2 C34 1.810(4) . ? Si1 C1 1.885(4) . ? Si1 C2 1.848(4) . ? Si1 C3 1.867(4) . ? Si1 C4 1.873(4) . ? Si2 C1 1.873(4) . ? Si2 C5 1.873(4) . ? Si2 C6 1.869(4) . ? Si2 C7 1.846(4) . ? Si3 C21 1.887(4) . ? Si3 C22 1.853(4) . ? Si3 C23 1.867(4) . ? Si3 C24 1.867(4) . ? Si4 C21 1.880(4) . ? Si4 C25 1.860(4) . ? Si4 C26 1.861(4) . ? Si4 C27 1.876(4) . ? B1 H1A 1.19(3) . ? B1 H1B 1.14(3) . ? B1 H1C 1.22(4) . ? B2 H2A 1.10(3) . ? B2 H2B 1.19(4) . ? B2 H2C 1.11(3) . ? Na1 H2B 2.64(3) . ? Na1 H2C 2.35(3) . ? Na1 N1 2.542(3) . ? Na1 N2 2.498(3) . ? Na1 C17 3.126(4) . ? Na2 H1A 2.54(3) 1_565 ? Na2 H1B 2.63(3) 1_565 ? Na2 H1C 2.51(4) 1_565 ? Na2 N3 2.523(3) . ? Na2 N4 2.533(3) . ? N1 C18 1.469(4) . ? N1 C19 1.461(5) . ? N1 C20 1.475(4) . ? N2 C15 1.455(4) . ? N2 C16 1.467(4) . ? N2 C17 1.456(5) . ? N3 C38 1.474(5) . ? N3 C39 1.453(5) . ? N3 C40 1.466(5) . ? N4 C35 1.477(5) . ? N4 C36 1.466(4) . ? N4 C37 1.458(5) . ? C1 H1 1.000 . ? C2 H2D 0.980 . ? C2 H2E 0.980 . ? C2 H2F 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.380(4) . ? C8 C13 1.406(4) . ? C9 H9 0.950 . ? C9 C10 1.382(5) . ? C10 H10 0.950 . ? C10 C11 1.384(5) . ? C11 H11 0.950 . ? C11 C12 1.380(5) . ? C12 H12 0.950 . ? C12 C13 1.373(5) . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.503(5) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C20 H20A 0.980 . ? C20 H20B 0.980 . ? C20 H20C 0.980 . ? C21 H21 1.000 . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? C24 H24A 0.980 . ? C24 H24B 0.980 . ? C24 H24C 0.980 . ? C25 H25D 0.980 . ? C25 H25E 0.980 . ? C25 H25F 0.980 . ? C26 H26A 0.980 . ? C26 H26B 0.980 . ? C26 H26C 0.980 . ? C27 H25A 0.980 . ? C27 H25B 0.980 . ? C27 H25C 0.980 . ? C28 C29 1.383(5) . ? C28 C33 1.421(5) . ? C29 H29 0.950 . ? C29 C30 1.390(5) . ? C30 H30 0.950 . ? C30 C31 1.371(5) . ? C31 H31 0.950 . ? C31 C32 1.389(5) . ? C32 H32 0.950 . ? C32 C33 1.382(5) . ? C34 H34A 0.980 . ? C34 H34B 0.980 . ? C34 H34C 0.980 . ? C35 H35A 0.980 . ? C35 H35B 0.980 . ? C35 H35C 0.980 . ? C36 H36A 0.980 . ? C36 H36B 0.980 . ? C36 H36C 0.980 . ? C37 H37A 0.990 . ? C37 H37B 0.990 . ? C37 C38 1.494(6) . ? C38 H38A 0.990 . ? C38 H38B 0.990 . ? C39 H39A 0.980 . ? C39 H39B 0.980 . ? C39 H39C 0.980 . ? C40 H40A 0.980 . ? C40 H40B 0.980 . ? C40 H40C 0.980 . ? 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 B1 P1 Na1 119.87(17) . . ? B1 P1 C1 110.23(18) . . ? B1 P1 C8 105.98(19) . . ? Na1 P1 C1 114.88(11) . . ? Na1 P1 C8 98.10(12) . . ? C1 P1 C8 105.55(16) . . ? B2 P2 Na2 118.70(15) . . ? B2 P2 C21 109.88(18) . . ? B2 P2 C28 106.0(2) . . ? Na2 P2 C21 116.09(11) . . ? Na2 P2 C28 99.01(11) . . ? C21 P2 C28 105.05(16) . . ? Na1 S1 C13 97.10(13) . . ? Na1 S1 C14 120.51(15) . . ? C13 S1 C14 104.20(17) . . ? Na2 S2 C33 97.34(13) . . ? Na2 S2 C34 122.45(14) . . ? C33 S2 C34 103.9(2) . . ? C1 Si1 C2 112.34(17) . . ? C1 Si1 C3 113.57(19) . . ? C1 Si1 C4 111.12(18) . . ? C2 Si1 C3 107.6(2) . . ? C2 Si1 C4 104.7(2) . . ? C3 Si1 C4 106.9(2) . . ? C1 Si2 C5 108.64(17) . . ? C1 Si2 C6 112.37(17) . . ? C1 Si2 C7 111.10(17) . . ? C5 Si2 C6 109.14(18) . . ? C5 Si2 C7 106.90(19) . . ? C6 Si2 C7 108.52(19) . . ? C21 Si3 C22 112.25(17) . . ? C21 Si3 C23 113.29(17) . . ? C21 Si3 C24 111.29(19) . . ? C22 Si3 C23 108.6(2) . . ? C22 Si3 C24 104.0(2) . . ? C23 Si3 C24 106.9(2) . . ? C21 Si4 C25 110.78(18) . . ? C21 Si4 C26 113.41(17) . . ? C21 Si4 C27 109.94(18) . . ? C25 Si4 C26 108.43(18) . . ? C25 Si4 C27 105.67(18) . . ? C26 Si4 C27 108.30(18) . . ? P1 B1 H1A 107.4(14) . . ? P1 B1 H1B 104.3(15) . . ? P1 B1 H1C 109.8(17) . . ? H1A B1 H1B 109(2) . . ? H1A B1 H1C 117(2) . . ? H1B B1 H1C 109(2) . . ? P2 B2 H2A 105.7(16) . . ? P2 B2 H2B 106.4(14) . . ? P2 B2 H2C 115.6(16) . . ? H2A B2 H2B 106(2) . . ? H2A B2 H2C 113(2) . . ? H2B B2 H2C 109(2) . . ? P1 Na1 S1 62.93(4) . . ? P1 Na1 H2B 122.6(8) . . ? P1 Na1 H2C 127.1(8) . . ? P1 Na1 N1 105.34(8) . . ? P1 Na1 N2 100.59(9) . . ? P1 Na1 C17 114.86(8) . . ? S1 Na1 H2B 66.0(8) . . ? S1 Na1 H2C 101.1(8) . . ? S1 Na1 N1 163.54(9) . . ? S1 Na1 N2 95.02(9) . . ? S1 Na1 C17 121.90(9) . . ? H2B Na1 H2C 43.7(10) . . ? H2B Na1 N1 129.3(8) . . ? H2B Na1 N2 108.3(7) . . ? H2B Na1 C17 113.3(7) . . ? H2C Na1 N1 95.3(8) . . ? H2C Na1 N2 131.9(8) . . ? H2C Na1 C17 115.8(8) . . ? N1 Na1 N2 75.12(11) . . ? N1 Na1 C17 50.29(10) . . ? N2 Na1 C17 27.19(10) . . ? P2 Na2 S2 63.43(4) . . ? P2 Na2 H1A 119.7(7) . 1_565 ? P2 Na2 H1B 162.0(8) . 1_565 ? P2 Na2 H1C 124.1(8) . 1_565 ? P2 Na2 N3 100.75(8) . . ? P2 Na2 N4 104.29(8) . . ? S2 Na2 H1A 65.6(8) . 1_565 ? S2 Na2 H1B 104.3(7) . 1_565 ? S2 Na2 H1C 106.2(8) . 1_565 ? S2 Na2 N3 94.46(9) . . ? S2 Na2 N4 162.51(9) . . ? H1A Na2 H1B 43.0(10) 1_565 1_565 ? H1A Na2 H1C 47.9(11) 1_565 1_565 ? H1A Na2 N3 113.2(8) 1_565 . ? H1A Na2 N4 131.2(8) 1_565 . ? H1B Na2 H1C 43.8(11) 1_565 1_565 ? H1B Na2 N3 93.0(8) 1_565 . ? H1B Na2 N4 90.4(7) 1_565 . ? H1C Na2 N3 135.1(8) 1_565 . ? H1C Na2 N4 91.0(8) 1_565 . ? N3 Na2 N4 74.96(11) . . ? Na1 N1 C18 103.7(2) . . ? Na1 N1 C19 112.2(2) . . ? Na1 N1 C20 112.9(2) . . ? C18 N1 C19 110.9(3) . . ? C18 N1 C20 109.2(3) . . ? C19 N1 C20 108.0(3) . . ? Na1 N2 C15 108.5(2) . . ? Na1 N2 C16 117.7(2) . . ? Na1 N2 C17 101.2(2) . . ? C15 N2 C16 109.1(3) . . ? C15 N2 C17 108.9(3) . . ? C16 N2 C17 110.9(3) . . ? Na2 N3 C38 102.2(2) . . ? Na2 N3 C39 116.1(2) . . ? Na2 N3 C40 110.4(2) . . ? C38 N3 C39 109.5(3) . . ? C38 N3 C40 110.0(3) . . ? C39 N3 C40 108.5(3) . . ? Na2 N4 C35 112.9(2) . . ? Na2 N4 C36 110.7(2) . . ? Na2 N4 C37 104.0(2) . . ? C35 N4 C36 108.1(3) . . ? C35 N4 C37 109.5(3) . . ? C36 N4 C37 111.6(3) . . ? P1 C1 Si1 119.61(18) . . ? P1 C1 Si2 109.50(18) . . ? P1 C1 H1 102.9 . . ? Si1 C1 Si2 116.21(17) . . ? Si1 C1 H1 102.9 . . ? Si2 C1 H1 102.9 . . ? Si1 C2 H2D 109.5 . . ? Si1 C2 H2E 109.5 . . ? Si1 C2 H2F 109.5 . . ? H2D C2 H2E 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C8 C9 121.9(3) . . ? P1 C8 C13 120.4(3) . . ? C9 C8 C13 117.3(3) . . ? C8 C9 H9 118.7 . . ? C8 C9 C10 122.7(3) . . ? H9 C9 C10 118.7 . . ? C9 C10 H10 120.5 . . ? C9 C10 C11 118.9(3) . . ? H10 C10 C11 120.5 . . ? C10 C11 H11 120.1 . . ? C10 C11 C12 119.7(4) . . ? H11 C11 C12 120.1 . . ? C11 C12 H12 119.5 . . ? C11 C12 C13 120.9(3) . . ? H12 C12 C13 119.5 . . ? S1 C13 C8 116.8(3) . . ? S1 C13 C12 122.8(3) . . ? C8 C13 C12 120.5(3) . . ? S1 C14 H14A 109.5 . . ? S1 C14 H14B 109.5 . . ? S1 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Na1 C17 N2 51.63(17) . . ? Na1 C17 H17A 85.1 . . ? Na1 C17 H17B 160.1 . . ? Na1 C17 C18 79.9(2) . . ? N2 C17 H17A 108.9 . . ? N2 C17 H17B 108.9 . . ? N2 C17 C18 113.4(3) . . ? H17A C17 H17B 107.7 . . ? H17A C17 C18 108.9 . . ? H17B C17 C18 108.9 . . ? N1 C18 C17 112.2(3) . . ? N1 C18 H18A 109.2 . . ? N1 C18 H18B 109.2 . . ? C17 C18 H18A 109.2 . . ? C17 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P2 C21 Si3 118.43(19) . . ? P2 C21 Si4 109.55(18) . . ? P2 C21 H21 103.3 . . ? Si3 C21 Si4 116.55(17) . . ? Si3 C21 H21 103.3 . . ? Si4 C21 H21 103.3 . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C24 H24A 109.5 . . ? Si3 C24 H24B 109.5 . . ? Si3 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si4 C25 H25D 109.5 . . ? Si4 C25 H25E 109.5 . . ? Si4 C25 H25F 109.5 . . ? H25D C25 H25E 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? Si4 C26 H26A 109.5 . . ? Si4 C26 H26B 109.5 . . ? Si4 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si4 C27 H25A 109.5 . . ? Si4 C27 H25B 109.5 . . ? Si4 C27 H25C 109.5 . . ? H25A C27 H25B 109.5 . . ? H25A C27 H25C 109.5 . . ? H25B C27 H25C 109.5 . . ? P2 C28 C29 121.1(3) . . ? P2 C28 C33 121.1(3) . . ? C29 C28 C33 117.2(4) . . ? C28 C29 H29 118.9 . . ? C28 C29 C30 122.2(4) . . ? H29 C29 C30 118.9 . . ? C29 C30 H30 120.2 . . ? C29 C30 C31 119.6(4) . . ? H30 C30 C31 120.2 . . ? C30 C31 H31 119.9 . . ? C30 C31 C32 120.3(4) . . ? H31 C31 C32 119.9 . . ? C31 C32 H32 119.9 . . ? C31 C32 C33 120.1(4) . . ? H32 C32 C33 119.9 . . ? S2 C33 C28 116.7(3) . . ? S2 C33 C32 122.7(3) . . ? C28 C33 C32 120.6(3) . . ? S2 C34 H34A 109.5 . . ? S2 C34 H34B 109.5 . . ? S2 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 108.8 . . ? N4 C37 H37B 108.8 . . ? N4 C37 C38 113.6(3) . . ? H37A C37 H37B 107.7 . . ? H37A C37 C38 108.8 . . ? H37B C37 C38 108.8 . . ? N3 C38 C37 113.7(3) . . ? N3 C38 H38A 108.8 . . ? N3 C38 H38B 108.8 . . ? C37 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? H38A C38 H38B 107.7 . . ? N3 C39 H39A 109.5 . . ? N3 C39 H39B 109.5 . . ? N3 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N3 C40 H40A 109.5 . . ? N3 C40 H40B 109.5 . . ? N3 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.326 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.055 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.261 0.141 0.601 11.4 0.2 2 0.500 0.500 1.000 281.7 3.2 3 0.739 0.858 0.399 11.4 0.4 _platon_squeeze_details ; ; # Contents of RES file _computing_special_details ; TITL ki385 in P-1 CELL 0.71073 11.3566 13.2652 21.1564 93.397 104.760 97.552 ZERR 4.00 0.0009 0.0010 0.0018 0.007 0.007 0.006 LATT 1 SFAC C H B N NA SI P S UNIT 80 180 4 8 4 8 4 4 REM colourless block SIZE 0.12 0.10 0.08 TEMP -123 OMIT -3 50 REM unidentified disordered solved treated by squeeze L.S. 8 BOND $H ACTA FMAP 2 PLAN 10 EQIV $1 x, y+1, z EQIV $2 x, y-1, z FREE B1 NA2_$2 FREE B2 NA1 FREE NA2 B1_$1 BIND NA2 H1A_$1 BIND NA2 H1B_$1 BIND NA2 H1C_$1 REM EXTI 0.000000 WGHT 0.031900 FVAR 2.19523 P1 7 1.005115 1.176837 0.200608 11.00000 0.02683 0.02065 = 0.02546 0.00254 0.00955 0.00565 P2 7 1.061880 1.699342 0.325368 11.00000 0.02381 0.01984 = 0.02657 -0.00123 0.00566 0.00455 S1 8 0.954540 1.372419 0.127818 11.00000 0.04497 0.02159 = 0.03117 0.00365 0.01503 0.01173 S2 8 1.081312 1.916421 0.401353 11.00000 0.04608 0.02177 = 0.03499 0.00137 0.00630 0.00817 SI1 6 0.725863 1.076624 0.119053 11.00000 0.03453 0.03614 = 0.03255 -0.00119 0.00935 -0.00088 SI2 6 0.801713 1.147433 0.272624 11.00000 0.02866 0.03684 = 0.02918 0.00334 0.01390 0.00734 SI3 6 0.852802 1.620346 0.398158 11.00000 0.03659 0.03144 = 0.03779 -0.00194 0.01454 0.00015 SI4 6 0.792593 1.641317 0.243524 11.00000 0.02371 0.03136 = 0.03718 -0.00349 0.00360 0.00768 B1 3 1.068976 1.053373 0.230387 11.00000 0.03607 0.02707 = 0.03558 0.00994 0.01656 0.01065 H1A 2 1.062394 1.048232 0.285381 11.00000 0.03536 H1B 2 1.170119 1.068148 0.230369 11.00000 0.03940 H1C 2 1.017367 0.980382 0.191006 11.00000 0.05954 B2 3 1.101318 1.568160 0.296137 11.00000 0.03182 0.01801 = 0.03976 0.00266 0.01281 0.00699 H2A 2 1.199986 1.582050 0.298099 11.00000 0.03148 H2B 2 1.047747 1.550644 0.239355 11.00000 0.03068 H2C 2 1.076191 1.502791 0.322685 11.00000 0.03178 NA1 5 1.142210 1.380395 0.260249 11.00000 0.02747 0.02335 = 0.03494 -0.00112 0.00867 0.00595 NA2 5 1.152285 1.885106 0.271532 11.00000 0.02916 0.02447 = 0.03767 0.00637 0.01282 0.00793 N1 4 1.316966 1.344496 0.354101 11.00000 0.02848 0.03070 = 0.03630 0.00183 0.00985 0.01258 N2 4 1.324416 1.387552 0.213956 11.00000 0.02701 0.03161 = 0.03468 0.00428 0.00697 0.00453 N3 4 1.380336 1.903507 0.325630 11.00000 0.02891 0.02839 = 0.03967 -0.00103 0.00705 0.00195 N4 4 1.245271 1.819258 0.183286 11.00000 0.03616 0.03321 = 0.03497 0.00559 0.01508 0.01258 C1 1 0.833518 1.161508 0.190694 11.00000 0.02005 0.01707 = 0.02193 0.00642 0.00339 0.00321 AFIX 13 H1 2 0.813565 1.231161 0.181106 11.00000 -1.20000 AFIX 0 C2 1 0.724610 1.128043 0.039632 11.00000 0.04165 0.06649 = 0.03261 -0.00098 -0.00430 -0.01198 AFIX 137 H2D 2 0.713385 1.200013 0.042468 11.00000 -1.50000 H2E 2 0.656795 1.089069 0.004990 11.00000 -1.50000 H2F 2 0.802987 1.122315 0.029320 11.00000 -1.50000 AFIX 0 C3 1 0.761442 0.943439 0.113295 11.00000 0.06283 0.03749 = 0.05532 -0.01651 0.00942 -0.00289 AFIX 137 H3A 2 0.704622 0.904299 0.074153 11.00000 -1.50000 H3B 2 0.752063 0.910972 0.152508 11.00000 -1.50000 H3C 2 0.846313 0.945147 0.110201 11.00000 -1.50000 AFIX 0 C4 1 0.562487 1.066987 0.123935 11.00000 0.04055 0.07696 = 0.05113 -0.01337 0.00635 -0.00305 AFIX 137 H4A 2 0.540022 1.135630 0.126838 11.00000 -1.50000 H4B 2 0.554053 1.033533 0.162962 11.00000 -1.50000 H4C 2 0.507883 1.026755 0.084560 11.00000 -1.50000 AFIX 0 C5 1 0.658814 1.203001 0.273566 11.00000 0.04238 0.06584 = 0.03958 0.00182 0.02179 0.01492 AFIX 137 H5A 2 0.656394 1.263706 0.249300 11.00000 -1.50000 H5B 2 0.659042 1.222147 0.319058 11.00000 -1.50000 H5C 2 0.586222 1.152230 0.252834 11.00000 -1.50000 AFIX 0 C6 1 0.780297 1.011072 0.290785 11.00000 0.03932 0.05687 = 0.04928 0.02133 0.02130 0.00566 AFIX 137 H6A 2 0.853826 0.980983 0.288951 11.00000 -1.50000 H6B 2 0.708391 0.973048 0.258188 11.00000 -1.50000 H6C 2 0.767443 1.007685 0.334738 11.00000 -1.50000 AFIX 0 C7 1 0.927638 1.219864 0.339305 11.00000 0.04737 0.06052 = 0.02440 -0.00279 0.01129 0.01247 AFIX 137 H7A 2 0.940766 1.291426 0.330133 11.00000 -1.50000 H7B 2 1.003412 1.190511 0.342114 11.00000 -1.50000 H7C 2 0.905579 1.216100 0.381062 11.00000 -1.50000 AFIX 0 C8 1 1.024469 1.185508 0.117616 11.00000 0.01621 0.02569 = 0.02691 0.00257 0.00367 0.00750 C9 1 1.068086 1.109983 0.086352 11.00000 0.03152 0.02218 = 0.03332 0.00289 0.01332 0.00424 AFIX 43 H9 2 1.078084 1.048110 0.106124 11.00000 -1.20000 AFIX 0 C10 1 1.097793 1.120747 0.027455 11.00000 0.03619 0.03131 = 0.03683 -0.00135 0.01551 0.01226 AFIX 43 H10 2 1.128503 1.067573 0.007465 11.00000 -1.20000 AFIX 0 C11 1 1.082072 1.210248 -0.001923 11.00000 0.04412 0.03369 = 0.02378 0.00222 0.01709 0.00353 AFIX 43 H11 2 1.102785 1.219359 -0.042190 11.00000 -1.20000 AFIX 0 C12 1 1.036167 1.286241 0.027523 11.00000 0.03406 0.02319 = 0.02995 0.00320 0.00784 0.00259 AFIX 43 H12 2 1.023433 1.346864 0.006663 11.00000 -1.20000 AFIX 0 C13 1 1.008653 1.275450 0.086530 11.00000 0.02158 0.02001 = 0.02437 -0.00284 0.00645 0.00406 C14 1 0.958664 1.477270 0.078176 11.00000 0.06179 0.02252 = 0.04570 0.00701 0.01945 0.01274 AFIX 137 H14A 2 0.906978 1.455520 0.033537 11.00000 -1.50000 H14B 2 1.043672 1.499409 0.076761 11.00000 -1.50000 H14C 2 0.927592 1.534135 0.097122 11.00000 -1.50000 AFIX 0 C15 1 1.327838 1.475663 0.176266 11.00000 0.05256 0.05099 = 0.05171 0.01511 0.01621 0.00740 AFIX 137 H15A 2 1.406436 1.486941 0.164656 11.00000 -1.50000 H15B 2 1.319485 1.536245 0.202655 11.00000 -1.50000 H15C 2 1.259899 1.463137 0.136103 11.00000 -1.50000 AFIX 0 C16 1 1.334851 1.296862 0.173725 11.00000 0.03832 0.04484 = 0.04230 -0.00537 0.01010 0.00512 AFIX 137 H16A 2 1.417851 1.303081 0.167273 11.00000 -1.50000 H16B 2 1.274028 1.291200 0.130986 11.00000 -1.50000 H16C 2 1.319642 1.235740 0.196047 11.00000 -1.50000 AFIX 0 C17 1 1.425389 1.407402 0.273599 11.00000 0.02134 0.03801 = 0.04363 -0.00606 0.00864 0.00125 AFIX 23 H17A 2 1.426994 1.476677 0.294278 11.00000 -1.20000 H17B 2 1.504121 1.406400 0.261716 11.00000 -1.20000 AFIX 0 C18 1 1.416121 1.331446 0.322728 11.00000 0.02740 0.03989 = 0.03689 -0.00416 0.00034 0.01273 AFIX 23 H18A 2 1.400827 1.261436 0.300369 11.00000 -1.20000 H18B 2 1.495465 1.339410 0.356916 11.00000 -1.20000 AFIX 0 C19 1 1.356346 1.428511 0.406354 11.00000 0.04581 0.04425 = 0.03649 -0.00154 0.00872 0.01872 AFIX 137 H19A 2 1.429410 1.414944 0.439024 11.00000 -1.50000 H19B 2 1.289752 1.434553 0.427417 11.00000 -1.50000 H19C 2 1.376287 1.492383 0.387663 11.00000 -1.50000 AFIX 0 C20 1 1.285177 1.250291 0.383728 11.00000 0.04386 0.04302 = 0.04491 0.00901 0.01584 0.01418 AFIX 137 H20A 2 1.358104 1.236274 0.416310 11.00000 -1.50000 H20B 2 1.256597 1.192993 0.349389 11.00000 -1.50000 H20C 2 1.219703 1.258996 0.405176 11.00000 -1.50000 AFIX 0 C21 1 0.895792 1.684166 0.328117 11.00000 0.01822 0.01367 = 0.03501 -0.00404 0.00742 0.00067 AFIX 13 H21 2 0.881615 1.756130 0.335961 11.00000 -1.20000 AFIX 0 C22 1 0.917076 1.699537 0.477747 11.00000 0.06042 0.05672 = 0.03041 -0.00764 0.01871 -0.00749 AFIX 137 H22A 2 0.900128 1.769569 0.472565 11.00000 -1.50000 H22B 2 1.006296 1.699959 0.492087 11.00000 -1.50000 H22C 2 0.878793 1.670962 0.510678 11.00000 -1.50000 AFIX 0 C23 1 0.900534 1.491424 0.407090 11.00000 0.06381 0.03737 = 0.05084 0.00457 0.02901 0.00323 AFIX 137 H23A 2 0.990093 1.497549 0.414673 11.00000 -1.50000 H23B 2 0.859935 1.446404 0.366883 11.00000 -1.50000 H23C 2 0.876634 1.462632 0.444404 11.00000 -1.50000 AFIX 0 C24 1 0.682826 1.603148 0.387416 11.00000 0.04719 0.08239 = 0.05340 -0.00489 0.02204 -0.00052 AFIX 137 H24A 2 0.653550 1.669063 0.381140 11.00000 -1.50000 H24B 2 0.664036 1.576636 0.426573 11.00000 -1.50000 H24C 2 0.641656 1.554714 0.348894 11.00000 -1.50000 AFIX 0 C25 1 0.861820 1.695421 0.179764 11.00000 0.04267 0.04698 = 0.03602 0.00708 0.00742 0.01410 AFIX 137 H25D 2 0.938688 1.668487 0.181198 11.00000 -1.50000 H25E 2 0.879129 1.770046 0.188176 11.00000 -1.50000 H25F 2 0.804116 1.676237 0.136324 11.00000 -1.50000 AFIX 0 C26 1 0.758173 1.499967 0.225328 11.00000 0.03326 0.04454 = 0.04210 -0.01152 0.01033 0.00057 AFIX 137 H26A 2 0.835418 1.472028 0.230457 11.00000 -1.50000 H26B 2 0.706975 1.482626 0.180143 11.00000 -1.50000 H26C 2 0.713996 1.470795 0.255800 11.00000 -1.50000 AFIX 0 C27 1 0.642902 1.692104 0.233122 11.00000 0.03615 0.04929 = 0.05776 -0.00457 -0.00025 0.01338 AFIX 137 H25A 2 0.593675 1.654906 0.258643 11.00000 -1.50000 H25B 2 0.597499 1.682996 0.186593 11.00000 -1.50000 H25C 2 0.659344 1.764938 0.248698 11.00000 -1.50000 AFIX 0 C28 1 1.152018 1.729217 0.411386 11.00000 0.02182 0.01984 = 0.02734 -0.00155 0.00497 -0.00088 C29 1 1.220873 1.660188 0.443931 11.00000 0.02756 0.02446 = 0.03391 -0.00075 0.00367 0.00042 AFIX 43 H29 2 1.212781 1.593230 0.423139 11.00000 -1.20000 AFIX 0 C30 1 1.301526 1.685499 0.506049 11.00000 0.03926 0.03591 = 0.03990 0.00668 0.00286 0.00870 AFIX 43 H30 2 1.346904 1.636146 0.527346 11.00000 -1.20000 AFIX 0 C31 1 1.315144 1.782152 0.536370 11.00000 0.04521 0.04256 = 0.02990 0.00382 -0.00464 -0.00026 AFIX 43 H31 2 1.371311 1.800185 0.578468 11.00000 -1.20000 AFIX 0 C32 1 1.247186 1.853843 0.505816 11.00000 0.05045 0.02620 = 0.02571 -0.00679 0.00341 -0.00016 AFIX 43 H32 2 1.255478 1.920181 0.527527 11.00000 -1.20000 AFIX 0 C33 1 1.167520 1.828862 0.443888 11.00000 0.02360 0.02486 = 0.02895 0.00213 0.00494 0.00292 C34 1 1.131841 2.034092 0.454960 11.00000 0.06685 0.01609 = 0.05440 -0.00667 0.01833 0.00165 AFIX 137 H34A 2 1.115533 2.023396 0.497569 11.00000 -1.50000 H34B 2 1.086968 2.087601 0.435170 11.00000 -1.50000 H34C 2 1.220385 2.055000 0.461168 11.00000 -1.50000 AFIX 0 C35 1 1.180354 1.718806 0.150024 11.00000 0.04617 0.04143 = 0.05347 -0.00257 0.01618 0.01184 AFIX 137 H35A 2 1.225636 1.693276 0.120284 11.00000 -1.50000 H35B 2 1.097071 1.725926 0.124810 11.00000 -1.50000 H35C 2 1.175274 1.670552 0.182902 11.00000 -1.50000 AFIX 0 C36 1 1.243667 1.891343 0.133265 11.00000 0.05678 0.04688 = 0.04258 0.01468 0.02495 0.02223 AFIX 137 H36A 2 1.292162 1.870591 0.103855 11.00000 -1.50000 H36B 2 1.279244 1.960063 0.154675 11.00000 -1.50000 H36C 2 1.158522 1.891562 0.107828 11.00000 -1.50000 AFIX 0 C37 1 1.370738 1.809481 0.218855 11.00000 0.03511 0.05680 = 0.05475 0.00629 0.01945 0.02323 AFIX 23 H37A 2 1.420249 1.802836 0.186916 11.00000 -1.20000 H37B 2 1.368922 1.746054 0.241233 11.00000 -1.20000 AFIX 0 C38 1 1.432449 1.897650 0.268693 11.00000 0.02817 0.05213 = 0.06100 0.00568 0.01233 0.00402 AFIX 23 H38A 2 1.521088 1.892298 0.284452 11.00000 -1.20000 H38B 2 1.425716 1.961797 0.247290 11.00000 -1.20000 AFIX 0 C39 1 1.419945 1.825213 0.367997 11.00000 0.03649 0.06183 = 0.05882 0.01479 0.00988 0.00847 AFIX 137 H39A 2 1.509842 1.830406 0.378567 11.00000 -1.50000 H39B 2 1.382141 1.757622 0.345386 11.00000 -1.50000 H39C 2 1.394561 1.834816 0.408608 11.00000 -1.50000 AFIX 0 C40 1 1.424310 2.003650 0.363410 11.00000 0.04976 0.05019 = 0.07278 -0.01322 0.00955 -0.00329 AFIX 137 H40A 2 1.514447 2.013792 0.378655 11.00000 -1.50000 H40B 2 1.389760 2.006770 0.401341 11.00000 -1.50000 H40C 2 1.398119 2.057329 0.335491 11.00000 -1.50000 HKLF 4 REM ki385 in P-1 REM R1 = 0.0476 for 4259 Fo > 4sig(Fo) and 0.1302 for all 10697 data REM 551 parameters refined using 0 restraints END ; #===END data_ki450_compound_12 _database_code_depnum_ccdc_archive 'CCDC 836012' #TrackingRef '- dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H104 B2 K2 N6 P2 S2 Si4' _chemical_formula_sum 'C46 H104 B2 K2 N6 P2 S2 Si4' _chemical_formula_weight 1079.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1081(6) _cell_length_b 12.0772(7) _cell_length_c 14.3398(7) _cell_angle_alpha 101.977(4) _cell_angle_beta 108.829(5) _cell_angle_gamma 105.691(5) _cell_volume 1658.67(15) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5761 _cell_measurement_theta_min 3.44 _cell_measurement_theta_max 62.21 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 3.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.443 _exptl_absorpt_correction_T_max 0.564 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'sealed tube with Enhance Ultra optics' _diffrn_radiation_monochromator none _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 8950 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_av_sigmaI/netI 0.0272 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 62.29 _reflns_number_total 5133 _reflns_number_gt 4426 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) ; _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^)+(0.0465P)^2^+0.5734P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00075(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5133 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 K K 0.33699(4) 0.36482(4) 0.36408(3) 0.02739(12) Uani 1 1 d . . . P P 0.36921(4) 0.64257(4) 0.29332(3) 0.02048(13) Uani 1 1 d . . . S S 0.08151(5) 0.51448(4) 0.28753(4) 0.03478(14) Uani 1 1 d . . . Si1 Si 0.29536(6) 0.72079(5) 0.09967(4) 0.03078(15) Uani 1 1 d . . . Si2 Si 0.59323(5) 0.71261(5) 0.20845(4) 0.02760(14) Uani 1 1 d . . . B B 0.5110(2) 0.6511(2) 0.42322(16) 0.0248(5) Uani 1 1 d . . . H1A H 0.570(2) 0.592(2) 0.4058(17) 0.040(6) Uiso 1 1 d . . . H1B H 0.586(2) 0.749(2) 0.4715(16) 0.036(6) Uiso 1 1 d . . . H1C H 0.446(2) 0.6134(18) 0.4645(15) 0.029(5) Uiso 1 1 d . . . N1 N 0.07285(17) 0.18220(15) 0.31199(13) 0.0323(4) Uani 1 1 d . . . N2 N 0.19544(16) 0.19418(14) 0.15482(12) 0.0260(3) Uani 1 1 d . . . N3 N 0.48360(16) 0.23030(15) 0.28416(12) 0.0296(4) Uani 1 1 d . . . C1 C 0.44100(18) 0.74075(17) 0.22320(14) 0.0229(4) Uani 1 1 d . . . H1 H 0.4742 0.8271 0.2683 0.027 Uiso 1 1 calc R . . C2 C 0.3479(3) 0.8329(2) 0.03340(19) 0.0495(6) Uani 1 1 d . . . H2A H 0.2662 0.8373 -0.0165 0.074 Uiso 1 1 calc R . . H2B H 0.4009 0.8066 -0.0034 0.074 Uiso 1 1 calc R . . H2C H 0.4038 0.9133 0.0856 0.074 Uiso 1 1 calc R . . C3 C 0.2293(3) 0.5641(2) 0.00615(17) 0.0512(6) Uani 1 1 d . . . H3A H 0.1489 0.5536 -0.0544 0.077 Uiso 1 1 calc R . . H3B H 0.2039 0.5046 0.0403 0.077 Uiso 1 1 calc R . . H3C H 0.3003 0.5518 -0.0166 0.077 Uiso 1 1 calc R . . C4 C 0.1492(2) 0.7478(3) 0.12489(18) 0.0484(6) Uani 1 1 d . . . H4A H 0.0831 0.7496 0.0611 0.073 Uiso 1 1 calc R . . H4B H 0.1830 0.8257 0.1800 0.073 Uiso 1 1 calc R . . H4C H 0.1048 0.6822 0.1468 0.073 Uiso 1 1 calc R . . C5 C 0.6363(3) 0.7670(2) 0.10572(19) 0.0480(6) Uani 1 1 d . . . H5A H 0.7207 0.7561 0.1060 0.072 Uiso 1 1 calc R . . H5B H 0.6491 0.8532 0.1202 0.072 Uiso 1 1 calc R . . H5C H 0.5617 0.7199 0.0374 0.072 Uiso 1 1 calc R . . C6 C 0.7483(2) 0.7971(2) 0.33229(17) 0.0423(5) Uani 1 1 d . . . H6A H 0.7366 0.7647 0.3874 0.063 Uiso 1 1 calc R . . H6B H 0.7612 0.8835 0.3524 0.063 Uiso 1 1 calc R . . H6C H 0.8284 0.7875 0.3222 0.063 Uiso 1 1 calc R . . C7 C 0.5627(2) 0.5465(2) 0.17156(17) 0.0382(5) Uani 1 1 d . . . H7A H 0.5422 0.5144 0.2244 0.057 Uiso 1 1 calc R . . H7B H 0.6446 0.5341 0.1671 0.057 Uiso 1 1 calc R . . H7C H 0.4854 0.5039 0.1039 0.057 Uiso 1 1 calc R . . C8 C 0.28796(18) 0.73305(17) 0.35403(13) 0.0219(4) Uani 1 1 d . . . C9 C 0.34753(19) 0.85866(17) 0.40211(14) 0.0254(4) Uani 1 1 d . . . H9 H 0.4329 0.9012 0.4019 0.030 Uiso 1 1 calc R . . C10 C 0.2864(2) 0.92339(18) 0.45017(15) 0.0299(4) Uani 1 1 d . . . H10 H 0.3282 1.0093 0.4807 0.036 Uiso 1 1 calc R . . C11 C 0.1644(2) 0.86232(19) 0.45336(16) 0.0339(5) Uani 1 1 d . . . H11 H 0.1227 0.9060 0.4874 0.041 Uiso 1 1 calc R . . C12 C 0.1026(2) 0.73808(19) 0.40734(16) 0.0335(5) Uani 1 1 d . . . H12 H 0.0189 0.6964 0.4105 0.040 Uiso 1 1 calc R . . C13 C 0.16220(19) 0.67305(17) 0.35606(15) 0.0260(4) Uani 1 1 d . . . C14 C -0.0842(2) 0.4810(2) 0.2928(2) 0.0499(6) Uani 1 1 d . . . H14A H -0.1424 0.3968 0.2496 0.075 Uiso 1 1 calc R . . H14B H -0.1262 0.5362 0.2668 0.075 Uiso 1 1 calc R . . H14C H -0.0739 0.4918 0.3650 0.075 Uiso 1 1 calc R . . C15 C 0.0119(3) 0.2344(3) 0.3769(2) 0.0543(7) Uani 1 1 d . . . H15A H 0.0642 0.2447 0.4498 0.081 Uiso 1 1 calc R . . H15B H -0.0826 0.1800 0.3548 0.081 Uiso 1 1 calc R . . H15C H 0.0132 0.3136 0.3698 0.081 Uiso 1 1 calc R . . C16 C 0.0828(3) 0.0715(2) 0.3315(2) 0.0513(6) Uani 1 1 d . . . H16A H 0.1290 0.0881 0.4066 0.077 Uiso 1 1 calc R . . H16B H 0.1351 0.0414 0.2958 0.077 Uiso 1 1 calc R . . H16C H -0.0091 0.0101 0.3054 0.077 Uiso 1 1 calc R . . C17 C -0.0052(2) 0.1632(2) 0.20263(16) 0.0341(5) Uani 1 1 d . . . H17A H -0.0118 0.2413 0.1953 0.041 Uiso 1 1 calc R . . H17B H -0.0990 0.1051 0.1810 0.041 Uiso 1 1 calc R . . C18 C 0.0557(2) 0.11515(19) 0.13001(16) 0.0332(5) Uani 1 1 d . . . H18A H 0.0555 0.0340 0.1330 0.040 Uiso 1 1 calc R . . H18B H -0.0029 0.1051 0.0578 0.040 Uiso 1 1 calc R . . C19 C 0.1938(2) 0.29303(19) 0.11108(16) 0.0341(5) Uani 1 1 d . . . H19A H 0.2875 0.3499 0.1345 0.051 Uiso 1 1 d R . . H19B H 0.1400 0.3358 0.1345 0.051 Uiso 1 1 d R . . H19C H 0.1527 0.2597 0.0349 0.051 Uiso 1 1 d R . . C20 C 0.2727(2) 0.12710(18) 0.11915(15) 0.0303(4) Uani 1 1 d . . . H20A H 0.2420 0.1084 0.0428 0.036 Uiso 1 1 calc R . . H20B H 0.2517 0.0489 0.1334 0.036 Uiso 1 1 calc R . . C21 C 0.4259(2) 0.19501(18) 0.17018(15) 0.0305(4) Uani 1 1 d . . . H21A H 0.4706 0.1431 0.1431 0.037 Uiso 1 1 calc R . . H21B H 0.4476 0.2691 0.1499 0.037 Uiso 1 1 calc R . . C22 C 0.6287(2) 0.3038(2) 0.32651(19) 0.0441(6) Uani 1 1 d . . . H22A H 0.6665 0.3261 0.4026 0.066 Uiso 1 1 calc R . . H22B H 0.6407 0.3777 0.3066 0.066 Uiso 1 1 calc R . . H22C H 0.6763 0.2571 0.2988 0.066 Uiso 1 1 calc R . . C23 C 0.4667(2) 0.1241(2) 0.31931(18) 0.0422(5) Uani 1 1 d . . . H23A H 0.5104 0.1507 0.3955 0.063 Uiso 1 1 calc R . . H23B H 0.5092 0.0729 0.2900 0.063 Uiso 1 1 calc R . . H23C H 0.3692 0.0776 0.2960 0.063 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 K 0.0277(2) 0.0263(2) 0.0228(2) 0.00592(17) 0.00661(17) 0.00755(17) P 0.0212(2) 0.0216(2) 0.0210(2) 0.00856(19) 0.00994(19) 0.00823(19) S 0.0271(3) 0.0264(3) 0.0523(3) 0.0120(2) 0.0204(2) 0.0072(2) Si1 0.0353(3) 0.0389(3) 0.0234(3) 0.0156(2) 0.0106(2) 0.0185(3) Si2 0.0272(3) 0.0338(3) 0.0288(3) 0.0137(2) 0.0168(2) 0.0120(2) B 0.0276(11) 0.0280(12) 0.0212(10) 0.0114(9) 0.0087(9) 0.0124(10) N1 0.0349(9) 0.0358(10) 0.0353(9) 0.0186(8) 0.0195(8) 0.0143(8) N2 0.0272(8) 0.0246(8) 0.0245(8) 0.0070(7) 0.0104(7) 0.0077(7) N3 0.0275(9) 0.0336(9) 0.0309(9) 0.0138(7) 0.0129(7) 0.0119(7) C1 0.0266(10) 0.0238(9) 0.0218(9) 0.0092(8) 0.0118(8) 0.0106(8) C2 0.0649(16) 0.0617(16) 0.0450(14) 0.0360(13) 0.0279(12) 0.0363(14) C3 0.0589(16) 0.0489(15) 0.0289(12) 0.0070(11) 0.0012(11) 0.0188(12) C4 0.0399(13) 0.0806(18) 0.0380(12) 0.0329(13) 0.0129(10) 0.0346(13) C5 0.0502(14) 0.0662(17) 0.0493(14) 0.0315(13) 0.0352(12) 0.0253(13) C6 0.0269(11) 0.0544(14) 0.0425(13) 0.0160(11) 0.0148(10) 0.0091(10) C7 0.0411(12) 0.0407(13) 0.0408(12) 0.0124(10) 0.0212(10) 0.0216(10) C8 0.0222(9) 0.0278(10) 0.0192(9) 0.0116(8) 0.0082(7) 0.0116(8) C9 0.0223(9) 0.0282(10) 0.0263(10) 0.0109(8) 0.0096(8) 0.0087(8) C10 0.0353(11) 0.0263(10) 0.0292(10) 0.0085(8) 0.0114(9) 0.0149(9) C11 0.0408(12) 0.0376(12) 0.0383(12) 0.0152(10) 0.0242(10) 0.0243(10) C12 0.0336(11) 0.0369(12) 0.0449(12) 0.0198(10) 0.0260(10) 0.0176(9) C13 0.0280(10) 0.0266(10) 0.0295(10) 0.0140(8) 0.0142(8) 0.0122(8) C14 0.0315(12) 0.0425(14) 0.0777(18) 0.0196(13) 0.0282(12) 0.0087(10) C15 0.0733(18) 0.0697(18) 0.0527(15) 0.0348(14) 0.0427(14) 0.0426(15) C16 0.0607(16) 0.0512(15) 0.0598(16) 0.0333(13) 0.0291(13) 0.0294(13) C17 0.0260(10) 0.0366(12) 0.0408(12) 0.0162(10) 0.0137(9) 0.0099(9) C18 0.0278(10) 0.0321(11) 0.0294(11) 0.0055(9) 0.0076(9) 0.0038(9) C19 0.0343(11) 0.0336(11) 0.0360(11) 0.0142(9) 0.0142(9) 0.0126(9) C20 0.0377(11) 0.0304(11) 0.0254(10) 0.0091(8) 0.0146(9) 0.0136(9) C21 0.0365(11) 0.0325(11) 0.0337(11) 0.0158(9) 0.0209(9) 0.0170(9) C22 0.0293(11) 0.0517(14) 0.0514(14) 0.0204(12) 0.0137(10) 0.0154(10) C23 0.0484(13) 0.0460(13) 0.0391(12) 0.0247(11) 0.0190(11) 0.0174(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K P 3.6617(6) . ? K S 3.7568(7) . ? K H1A 3.01(2) . ? K H1A 3.00(2) 2_666 ? K H1B 2.97(2) 2_666 ? K H1C 2.77(2) . ? K H1C 2.74(2) 2_666 ? K N1 2.9039(17) . ? K N2 2.8912(16) . ? K N3 2.9099(17) . ? K C19 3.266(2) . ? P B 1.975(2) . ? P C1 1.8852(18) . ? P C8 1.8473(18) . ? S C13 1.777(2) . ? S C14 1.805(2) . ? Si1 C1 1.8908(18) . ? Si1 C2 1.882(2) . ? Si1 C3 1.865(2) . ? Si1 C4 1.868(2) . ? Si2 C1 1.8792(18) . ? Si2 C5 1.875(2) . ? Si2 C6 1.866(2) . ? Si2 C7 1.870(2) . ? B H1A 1.14(2) . ? B H1B 1.15(2) . ? B H1C 1.14(2) . ? N1 C15 1.454(3) . ? N1 C16 1.447(3) . ? N1 C17 1.459(3) . ? N2 C18 1.466(2) . ? N2 C19 1.461(2) . ? N2 C20 1.463(2) . ? N3 C21 1.467(3) . ? N3 C22 1.457(3) . ? N3 C23 1.460(3) . ? C1 H1 1.000 . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.394(3) . ? C8 C13 1.402(3) . ? C9 H9 0.950 . ? C9 C10 1.383(3) . ? C10 H10 0.950 . ? C10 C11 1.377(3) . ? C11 H11 0.950 . ? C11 C12 1.378(3) . ? C12 H12 0.950 . ? C12 C13 1.397(3) . ? C14 H14A 0.980 . ? C14 H14B 0.980 . ? C14 H14C 0.980 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.514(3) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 H19A 0.980 . ? C19 H19B 0.980 . ? C19 H19C 0.980 . ? C20 H20A 0.990 . ? C20 H20B 0.990 . ? C20 C21 1.516(3) . ? C21 H21A 0.990 . ? C21 H21B 0.990 . ? C22 H22A 0.980 . ? C22 H22B 0.980 . ? C22 H22C 0.980 . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? 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 P K S 49.666(12) . . ? P K H1A 44.7(4) . . ? P K H1A 113.7(4) . 2_666 ? P K H1B 148.1(4) . 2_666 ? P K H1C 42.2(4) . . ? P K H1C 114.2(4) . 2_666 ? P K N1 122.00(4) . . ? P K N2 97.15(3) . . ? P K N3 111.48(3) . . ? P K C19 70.60(4) . . ? S K H1A 91.8(4) . . ? S K H1A 107.6(4) . 2_666 ? S K H1B 133.6(4) . 2_666 ? S K H1C 67.2(4) . . ? S K H1C 139.4(4) . 2_666 ? S K N1 74.28(3) . . ? S K N2 87.00(3) . . ? S K N3 143.22(3) . . ? S K C19 69.39(4) . . ? H1A K H1A 89.7(6) . 2_666 ? H1A K H1B 36.5(6) 2_666 2_666 ? H1A K H1B 110.3(6) . 2_666 ? H1A K H1C 37.8(6) . . ? H1A K H1C 38.0(6) 2_666 2_666 ? H1A K H1C 72.2(6) . 2_666 ? H1A K H1C 71.8(6) 2_666 . ? H1A K N1 166.1(4) . . ? H1A K N1 94.3(4) 2_666 . ? H1A K N2 118.3(4) . . ? H1A K N2 148.4(4) 2_666 . ? H1A K N3 86.6(4) . . ? H1A K N3 109.1(4) 2_666 . ? H1A K C19 98.0(4) . . ? H1A K C19 171.8(4) 2_666 . ? H1B K H1C 38.3(6) 2_666 2_666 ? H1B K H1C 106.3(6) 2_666 . ? H1B K N1 80.2(4) 2_666 . ? H1B K N2 114.2(4) 2_666 . ? H1B K N3 80.4(4) 2_666 . ? H1B K C19 140.6(4) 2_666 . ? H1C K H1C 78.5(6) . 2_666 ? H1C K N1 131.8(4) . . ? H1C K N1 118.3(4) 2_666 . ? H1C K N2 139.3(4) . . ? H1C K N2 133.6(4) 2_666 . ? H1C K N3 123.6(4) . . ? H1C K N3 74.5(4) 2_666 . ? H1C K C19 112.8(4) . . ? H1C K C19 147.9(4) 2_666 . ? N1 K N2 62.22(5) . . ? N1 K N3 104.57(5) . . ? N1 K C19 77.58(5) . . ? N2 K N3 62.10(5) . . ? N2 K C19 26.56(5) . . ? N3 K C19 74.45(5) . . ? K P B 62.01(7) . . ? K P C1 146.74(6) . . ? K P C8 110.79(6) . . ? B P C1 112.54(9) . . ? B P C8 97.38(9) . . ? C1 P C8 102.41(8) . . ? K S C13 108.84(6) . . ? K S C14 129.30(9) . . ? C13 S C14 102.32(10) . . ? C1 Si1 C2 111.97(10) . . ? C1 Si1 C3 110.95(10) . . ? C1 Si1 C4 112.34(9) . . ? C2 Si1 C3 108.57(12) . . ? C2 Si1 C4 104.99(11) . . ? C3 Si1 C4 107.73(13) . . ? C1 Si2 C5 113.46(10) . . ? C1 Si2 C6 110.00(9) . . ? C1 Si2 C7 110.78(9) . . ? C5 Si2 C6 105.67(11) . . ? C5 Si2 C7 106.59(11) . . ? C6 Si2 C7 110.17(11) . . ? P B H1A 110.8(11) . . ? P B H1B 112.6(11) . . ? P B H1C 100.9(10) . . ? H1A B H1B 109.5(16) . . ? H1A B H1C 111.6(15) . . ? H1B B H1C 111.2(15) . . ? K N1 C15 107.05(15) . . ? K N1 C16 112.88(14) . . ? K N1 C17 104.68(11) . . ? C15 N1 C16 108.60(17) . . ? C15 N1 C17 110.54(17) . . ? C16 N1 C17 112.92(18) . . ? K N2 C18 114.74(11) . . ? K N2 C19 91.18(11) . . ? K N2 C20 115.74(11) . . ? C18 N2 C19 110.31(16) . . ? C18 N2 C20 112.31(15) . . ? C19 N2 C20 110.58(15) . . ? K N3 C21 109.13(11) . . ? K N3 C22 110.64(13) . . ? K N3 C23 106.58(12) . . ? C21 N3 C22 110.06(16) . . ? C21 N3 C23 111.53(16) . . ? C22 N3 C23 108.85(17) . . ? P C1 Si1 107.85(9) . . ? P C1 Si2 111.07(9) . . ? P C1 H1 106.9 . . ? Si1 C1 Si2 116.70(9) . . ? Si1 C1 H1 106.9 . . ? Si2 C1 H1 106.9 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P C8 C9 123.47(14) . . ? P C8 C13 119.00(14) . . ? C9 C8 C13 117.48(16) . . ? C8 C9 H9 118.9 . . ? C8 C9 C10 122.14(17) . . ? H9 C9 C10 118.9 . . ? C9 C10 H10 120.3 . . ? C9 C10 C11 119.42(18) . . ? H10 C10 C11 120.3 . . ? C10 C11 H11 119.9 . . ? C10 C11 C12 120.24(18) . . ? H11 C11 C12 119.9 . . ? C11 C12 H12 119.8 . . ? C11 C12 C13 120.37(18) . . ? H12 C12 C13 119.8 . . ? S C13 C8 117.27(14) . . ? S C13 C12 122.40(15) . . ? C8 C13 C12 120.29(18) . . ? S C14 H14A 109.5 . . ? S C14 H14B 109.5 . . ? S C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? N1 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 H16A 109.5 . . ? N1 C16 H16B 109.5 . . ? N1 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N1 C17 H17A 108.8 . . ? N1 C17 H17B 108.8 . . ? N1 C17 C18 114.01(17) . . ? H17A C17 H17B 107.6 . . ? H17A C17 C18 108.8 . . ? H17B C17 C18 108.8 . . ? N2 C18 C17 113.56(16) . . ? N2 C18 H18A 108.9 . . ? N2 C18 H18B 108.9 . . ? C17 C18 H18A 108.9 . . ? C17 C18 H18B 108.9 . . ? H18A C18 H18B 107.7 . . ? K C19 N2 62.25(9) . . ? K C19 H19A 72.5 . . ? K C19 H19B 77.1 . . ? K C19 H19C 171.3 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 H20A 108.8 . . ? N2 C20 H20B 108.8 . . ? N2 C20 C21 113.74(16) . . ? H20A C20 H20B 107.7 . . ? H20A C20 C21 108.8 . . ? H20B C20 C21 108.8 . . ? N3 C21 C20 114.04(15) . . ? N3 C21 H21A 108.7 . . ? N3 C21 H21B 108.7 . . ? C20 C21 H21A 108.7 . . ? C20 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C23 H23A 109.5 . . ? N3 C23 H23B 109.5 . . ? N3 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 62.29 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.413 _refine_diff_density_min -0.227 _refine_diff_density_rms 0.044 # Contents of RES file _computing_special_details ; TITL ki450 in P-1 CELL 1.54178 11.1081 12.0772 14.3398 101.977 108.829 105.691 ZERR 1.00 0.0006 0.0007 0.0007 0.004 0.005 0.005 LATT 1 SFAC C H B N SI P S K UNIT 46 104 2 6 4 2 2 2 REM colourless block SIZE 0.30 0.20 0.20 TEMP -123 L.S. 8 ACTA BOND $H FMAP 2 PLAN 10 EQIV $1 -x+1, -y+1, -z+1 BIND K H1A_$1 BIND K H1B_$1 BIND K H1C_$1 FREE K B FREE K B_$1 FREE B K_$1 WGHT 0.046500 0.573400 EXTI 0.000748 FVAR 0.24898 K 8 0.336992 0.364815 0.364082 11.00000 0.02765 0.02629 = 0.02278 0.00592 0.00661 0.00755 P 6 0.369206 0.642568 0.293321 11.00000 0.02119 0.02160 = 0.02097 0.00856 0.00994 0.00823 S 7 0.081508 0.514482 0.287531 11.00000 0.02707 0.02642 = 0.05235 0.01195 0.02036 0.00724 SI1 5 0.295360 0.720788 0.099670 11.00000 0.03528 0.03887 = 0.02338 0.01560 0.01057 0.01852 SI2 5 0.593227 0.712614 0.208454 11.00000 0.02716 0.03378 = 0.02883 0.01368 0.01680 0.01204 B 3 0.511000 0.651095 0.423221 11.00000 0.02758 0.02800 = 0.02115 0.01136 0.00867 0.01242 H1A 2 0.570314 0.591523 0.405756 11.00000 0.03956 H1B 2 0.585784 0.748683 0.471517 11.00000 0.03596 H1C 2 0.445659 0.613418 0.464500 11.00000 0.02904 N1 4 0.072851 0.182196 0.311990 11.00000 0.03492 0.03579 = 0.03525 0.01855 0.01953 0.01429 N2 4 0.195441 0.194177 0.154818 11.00000 0.02723 0.02463 = 0.02448 0.00700 0.01039 0.00768 N3 4 0.483597 0.230302 0.284156 11.00000 0.02750 0.03364 = 0.03091 0.01379 0.01289 0.01195 C1 1 0.440996 0.740751 0.223205 11.00000 0.02656 0.02381 = 0.02181 0.00920 0.01178 0.01056 AFIX 13 H1 2 0.474224 0.827094 0.268337 11.00000 -1.20000 AFIX 0 C2 1 0.347865 0.832919 0.033403 11.00000 0.06486 0.06171 = 0.04504 0.03599 0.02790 0.03626 AFIX 137 H2A 2 0.266212 0.837327 -0.016487 11.00000 -1.50000 H2B 2 0.400918 0.806554 -0.003438 11.00000 -1.50000 H2C 2 0.403807 0.913265 0.085625 11.00000 -1.50000 AFIX 0 C3 1 0.229297 0.564116 0.006152 11.00000 0.05890 0.04887 = 0.02893 0.00704 0.00120 0.01881 AFIX 137 H3A 2 0.148894 0.553621 -0.054413 11.00000 -1.50000 H3B 2 0.203945 0.504634 0.040284 11.00000 -1.50000 H3C 2 0.300335 0.551762 -0.016559 11.00000 -1.50000 AFIX 0 C4 1 0.149184 0.747773 0.124890 11.00000 0.03992 0.08057 = 0.03796 0.03285 0.01288 0.03460 AFIX 137 H4A 2 0.083061 0.749627 0.061102 11.00000 -1.50000 H4B 2 0.182960 0.825688 0.180047 11.00000 -1.50000 H4C 2 0.104848 0.682161 0.146752 11.00000 -1.50000 AFIX 0 C5 1 0.636303 0.766963 0.105721 11.00000 0.05019 0.06619 = 0.04931 0.03147 0.03523 0.02532 AFIX 137 H5A 2 0.720686 0.756106 0.105959 11.00000 -1.50000 H5B 2 0.649058 0.853242 0.120155 11.00000 -1.50000 H5C 2 0.561678 0.719943 0.037360 11.00000 -1.50000 AFIX 0 C6 1 0.748251 0.797111 0.332295 11.00000 0.02692 0.05437 = 0.04252 0.01603 0.01476 0.00909 AFIX 137 H6A 2 0.736550 0.764702 0.387352 11.00000 -1.50000 H6B 2 0.761159 0.883528 0.352365 11.00000 -1.50000 H6C 2 0.828439 0.787468 0.322190 11.00000 -1.50000 AFIX 0 C7 1 0.562701 0.546490 0.171563 11.00000 0.04107 0.04073 = 0.04080 0.01244 0.02124 0.02159 AFIX 137 H7A 2 0.542170 0.514442 0.224362 11.00000 -1.50000 H7B 2 0.644563 0.534092 0.167124 11.00000 -1.50000 H7C 2 0.485370 0.503865 0.103866 11.00000 -1.50000 AFIX 0 C8 1 0.287962 0.733054 0.354034 11.00000 0.02222 0.02781 = 0.01924 0.01157 0.00824 0.01161 C9 1 0.347528 0.858658 0.402115 11.00000 0.02231 0.02818 = 0.02632 0.01093 0.00963 0.00866 AFIX 43 H9 2 0.432894 0.901187 0.401868 11.00000 -1.20000 AFIX 0 C10 1 0.286388 0.923391 0.450174 11.00000 0.03528 0.02628 = 0.02922 0.00850 0.01140 0.01493 AFIX 43 H10 2 0.328202 1.009250 0.480722 11.00000 -1.20000 AFIX 0 C11 1 0.164420 0.862323 0.453356 11.00000 0.04078 0.03760 = 0.03832 0.01523 0.02423 0.02426 AFIX 43 H11 2 0.122738 0.906018 0.487412 11.00000 -1.20000 AFIX 0 C12 1 0.102588 0.738081 0.407337 11.00000 0.03362 0.03688 = 0.04486 0.01983 0.02604 0.01760 AFIX 43 H12 2 0.018939 0.696381 0.410490 11.00000 -1.20000 AFIX 0 C13 1 0.162201 0.673054 0.356056 11.00000 0.02795 0.02664 = 0.02953 0.01401 0.01420 0.01216 C14 1 -0.084157 0.480989 0.292836 11.00000 0.03153 0.04249 = 0.07772 0.01961 0.02819 0.00867 AFIX 137 H14A 2 -0.142417 0.396817 0.249563 11.00000 -1.50000 H14B 2 -0.126161 0.536193 0.266831 11.00000 -1.50000 H14C 2 -0.073862 0.491768 0.364996 11.00000 -1.50000 AFIX 0 C15 1 0.011944 0.234403 0.376859 11.00000 0.07332 0.06966 = 0.05273 0.03477 0.04271 0.04256 AFIX 137 H15A 2 0.064223 0.244728 0.449757 11.00000 -1.50000 H15B 2 -0.082603 0.180031 0.354758 11.00000 -1.50000 H15C 2 0.013162 0.313639 0.369784 11.00000 -1.50000 AFIX 0 C16 1 0.082777 0.071518 0.331520 11.00000 0.06071 0.05117 = 0.05982 0.03326 0.02907 0.02939 AFIX 137 H16A 2 0.129048 0.088090 0.406572 11.00000 -1.50000 H16B 2 0.135082 0.041415 0.295844 11.00000 -1.50000 H16C 2 -0.009076 0.010067 0.305376 11.00000 -1.50000 AFIX 0 C17 1 -0.005163 0.163188 0.202628 11.00000 0.02601 0.03664 = 0.04078 0.01624 0.01367 0.00991 AFIX 23 H17A 2 -0.011806 0.241286 0.195276 11.00000 -1.20000 H17B 2 -0.099009 0.105146 0.181004 11.00000 -1.20000 AFIX 0 C18 1 0.055684 0.115151 0.130009 11.00000 0.02781 0.03209 = 0.02937 0.00554 0.00764 0.00382 AFIX 23 H18A 2 0.055512 0.033961 0.133038 11.00000 -1.20000 H18B 2 -0.002948 0.105060 0.057821 11.00000 -1.20000 AFIX 0 C19 1 0.193768 0.293025 0.111081 11.00000 0.03431 0.03360 = 0.03600 0.01416 0.01423 0.01264 AFIX 7 H19A 2 0.287477 0.349934 0.134473 11.00000 -1.50000 H19B 2 0.140045 0.335802 0.134542 11.00000 -1.50000 H19C 2 0.152657 0.259650 0.034887 11.00000 -1.50000 AFIX 0 C20 1 0.272691 0.127096 0.119148 11.00000 0.03772 0.03043 = 0.02536 0.00915 0.01464 0.01364 AFIX 23 H20A 2 0.242036 0.108405 0.042824 11.00000 -1.20000 H20B 2 0.251709 0.048910 0.133442 11.00000 -1.20000 AFIX 0 C21 1 0.425936 0.195009 0.170176 11.00000 0.03652 0.03245 = 0.03366 0.01575 0.02089 0.01702 AFIX 23 H21A 2 0.470589 0.143148 0.143132 11.00000 -1.20000 H21B 2 0.447609 0.269133 0.149927 11.00000 -1.20000 AFIX 0 C22 1 0.628650 0.303834 0.326513 11.00000 0.02928 0.05166 = 0.05143 0.02037 0.01367 0.01535 AFIX 137 H22A 2 0.666493 0.326146 0.402600 11.00000 -1.50000 H22B 2 0.640715 0.377686 0.306626 11.00000 -1.50000 H22C 2 0.676277 0.257112 0.298794 11.00000 -1.50000 AFIX 0 C23 1 0.466710 0.124137 0.319307 11.00000 0.04840 0.04597 = 0.03906 0.02473 0.01902 0.01741 AFIX 137 H23A 2 0.510432 0.150720 0.395506 11.00000 -1.50000 H23B 2 0.509195 0.072864 0.290037 11.00000 -1.50000 H23C 2 0.369171 0.077580 0.295968 11.00000 -1.50000 HKLF 4 REM ki450 in P-1 REM R1 = 0.0315 for 4426 Fo > 4sig(Fo) and 0.0388 for all 5133 data REM 314 parameters refined using 0 restraints END ; #===END