# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Keith Izod' 'William Clegg' 'Ross W. Harrington' 'William McFarlane' 'Brent V. Tyson' _publ_contact_author_name 'Dr Keith Izod' _publ_contact_author_address ; Chemistry University of Newcastle Newcastle upon Tyne NE1 7RU UNITED KINGDOM ; _publ_contact_author_email K.J.IZOD@NCL.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Synthesis and structural characterisation of a novel phosphine-borane-stabilised dicarbanion and an unusual bis(phosphine-borane). ; data_ki132 _database_code_depnum_ccdc_archive 'CCDC 225174' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H102 B2 Li2 N6 P2 Si2' _chemical_formula_sum 'C40 H102 B2 Li2 N6 P2 Si2' _chemical_formula_weight 820.90 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' 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' B B 0.0013 0.0007 '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/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 11.6349(6) _cell_length_b 19.2561(9) _cell_length_c 12.5695(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.174(1) _cell_angle_gamma 90.00 _cell_volume 2794.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 11228 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.68 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.976 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19093 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4914 _reflns_number_gt 3686 _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^)+(0.0537P)^2^+2.3831P] 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 4914 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0725 _refine_ls_R_factor_gt 0.0486 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _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 0.60148(5) 0.53577(3) 0.74153(5) 0.02799(17) Uani 1 1 d . . . Si Si 0.76230(6) 0.55082(4) 0.56647(5) 0.03147(19) Uani 1 1 d . . . N1 N 0.71051(18) 0.76002(11) 0.96585(19) 0.0420(5) Uani 1 1 d . . . N2 N 0.94421(19) 0.70959(11) 0.95623(19) 0.0430(6) Uani 1 1 d . . . N3 N 0.8655(2) 0.61430(13) 1.11262(19) 0.0554(7) Uani 1 1 d . . . B B 0.7174(3) 0.57902(18) 0.8426(2) 0.0396(7) Uani 1 1 d . . . H0A H 0.795(3) 0.5457(16) 0.865(3) 0.068(10) Uiso 1 1 d . . . H0B H 0.673(2) 0.5893(14) 0.916(2) 0.048(8) Uiso 1 1 d . . . H0C H 0.741(2) 0.6278(15) 0.812(2) 0.046(8) Uiso 1 1 d . . . Li Li 0.7864(4) 0.6597(2) 0.9676(3) 0.0354(9) Uani 1 1 d . . . C1 C 0.63253(19) 0.51827(12) 0.61474(18) 0.0281(5) Uani 1 1 d . . . C2 C 0.54148(19) 0.47833(11) 0.53955(17) 0.0252(5) Uani 1 1 d . . . H2A H 0.4942 0.4507 0.5843 0.030 Uiso 1 1 calc R . . H2B H 0.5826 0.4452 0.4974 0.030 Uiso 1 1 calc R . . C3 C 0.9029(2) 0.5269(2) 0.6495(3) 0.0614(9) Uani 1 1 d . . . H3A H 0.9026 0.5442 0.7228 0.092 Uiso 1 1 calc R . . H3B H 0.9676 0.5478 0.6180 0.092 Uiso 1 1 calc R . . H3C H 0.9116 0.4763 0.6509 0.092 Uiso 1 1 calc R . . C4 C 0.7687(3) 0.64770(16) 0.5478(3) 0.0627(9) Uani 1 1 d . . . H4A H 0.7079 0.6620 0.4909 0.094 Uiso 1 1 calc R . . H4B H 0.8446 0.6606 0.5278 0.094 Uiso 1 1 calc R . . H4C H 0.7568 0.6710 0.6149 0.094 Uiso 1 1 calc R . . C5 C 0.7754(2) 0.51356(16) 0.4302(2) 0.0441(7) Uani 1 1 d . . . H5A H 0.7738 0.4627 0.4339 0.066 Uiso 1 1 calc R . . H5B H 0.8486 0.5287 0.4067 0.066 Uiso 1 1 calc R . . H5C H 0.7105 0.5298 0.3789 0.066 Uiso 1 1 calc R . . C6 C 0.5574(2) 0.45656(13) 0.80748(19) 0.0371(6) Uani 1 1 d . . . H6A H 0.5380 0.4687 0.8797 0.045 Uiso 1 1 calc R . . H6B H 0.4866 0.4376 0.7655 0.045 Uiso 1 1 calc R . . C7 C 0.6503(3) 0.40098(15) 0.8185(3) 0.0550(8) Uani 1 1 d . . . H7A H 0.7178 0.4178 0.8675 0.066 Uiso 1 1 calc R . . H7B H 0.6763 0.3926 0.7475 0.066 Uiso 1 1 calc R . . C8 C 0.6084(4) 0.33304(17) 0.8613(3) 0.0767(12) Uani 1 1 d . . . H8A H 0.5885 0.3402 0.9340 0.115 Uiso 1 1 calc R . . H8B H 0.6697 0.2981 0.8628 0.115 Uiso 1 1 calc R . . H8C H 0.5397 0.3170 0.8146 0.115 Uiso 1 1 calc R . . C9 C 0.4698(2) 0.58958(14) 0.74077(19) 0.0362(6) Uani 1 1 d . . . H9A H 0.4882 0.6366 0.7158 0.043 Uiso 1 1 calc R . . H9B H 0.4097 0.5699 0.6864 0.043 Uiso 1 1 calc R . . C10 C 0.4167(2) 0.59784(18) 0.8442(2) 0.0523(8) Uani 1 1 d . . . H10A H 0.4749 0.6187 0.8991 0.063 Uiso 1 1 calc R . . H10B H 0.3968 0.5513 0.8701 0.063 Uiso 1 1 calc R . . C11 C 0.3088(3) 0.6428(2) 0.8321(3) 0.0747(12) Uani 1 1 d . . . H11A H 0.3296 0.6905 0.8154 0.112 Uiso 1 1 calc R . . H11B H 0.2741 0.6423 0.8992 0.112 Uiso 1 1 calc R . . H11C H 0.2530 0.6246 0.7739 0.112 Uiso 1 1 calc R . . C12 C 0.6245(3) 0.7755(2) 1.0402(4) 0.0923(14) Uani 1 1 d . . . H12A H 0.6058 0.8251 1.0369 0.138 Uiso 1 1 calc R . . H12B H 0.6570 0.7632 1.1135 0.138 Uiso 1 1 calc R . . H12C H 0.5540 0.7484 1.0194 0.138 Uiso 1 1 calc R . . C13 C 0.6559(3) 0.77419(19) 0.8582(3) 0.0783(11) Uani 1 1 d . . . H13A H 0.6376 0.8238 0.8511 0.117 Uiso 1 1 calc R . . H13B H 0.5844 0.7471 0.8440 0.117 Uiso 1 1 calc R . . H13C H 0.7087 0.7613 0.8065 0.117 Uiso 1 1 calc R . . C14 C 0.8115(3) 0.80496(16) 0.9955(3) 0.0608(9) Uani 1 1 d . . . H14A H 0.8322 0.8037 1.0743 0.073 Uiso 1 1 calc R . . H14B H 0.7906 0.8534 0.9749 0.073 Uiso 1 1 calc R . . C15 C 0.9155(2) 0.78358(14) 0.9427(3) 0.0489(7) Uani 1 1 d . . . H15A H 0.9004 0.7942 0.8651 0.059 Uiso 1 1 calc R . . H15B H 0.9832 0.8115 0.9732 0.059 Uiso 1 1 calc R . . C16 C 1.0057(3) 0.68559(18) 0.8679(3) 0.0709(11) Uani 1 1 d . . . H16A H 0.9556 0.6912 0.7997 0.106 Uiso 1 1 calc R . . H16B H 1.0261 0.6365 0.8785 0.106 Uiso 1 1 calc R . . H16C H 1.0764 0.7130 0.8665 0.106 Uiso 1 1 calc R . . C17 C 1.0113(3) 0.69572(18) 1.0613(3) 0.0703(11) Uani 1 1 d . . . H17A H 0.9912 0.7307 1.1137 0.084 Uiso 1 1 calc R . . H17B H 1.0949 0.7002 1.0552 0.084 Uiso 1 1 calc R . . C18 C 0.9877(3) 0.6251(2) 1.1012(3) 0.0767(11) Uani 1 1 d . . . H18A H 1.0120 0.5901 1.0507 0.092 Uiso 1 1 calc R . . H18B H 1.0346 0.6178 1.1716 0.092 Uiso 1 1 calc R . . C19 C 0.8343(4) 0.6470(2) 1.2095(3) 0.0940(14) Uani 1 1 d . . . H19A H 0.8816 0.6275 1.2723 0.141 Uiso 1 1 calc R . . H19B H 0.7522 0.6385 1.2150 0.141 Uiso 1 1 calc R . . H19C H 0.8479 0.6972 1.2063 0.141 Uiso 1 1 calc R . . C20 C 0.8414(4) 0.53919(18) 1.1205(3) 0.0834(13) Uani 1 1 d . . . H20A H 0.8874 0.5201 1.1845 0.125 Uiso 1 1 calc R . . H20B H 0.8620 0.5154 1.0566 0.125 Uiso 1 1 calc R . . H20C H 0.7589 0.5323 1.1258 0.125 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 0.0281(3) 0.0328(4) 0.0220(3) -0.0054(3) -0.0010(2) 0.0003(3) Si 0.0239(3) 0.0363(4) 0.0340(4) -0.0017(3) 0.0026(3) 0.0014(3) N1 0.0333(12) 0.0366(13) 0.0558(14) -0.0021(11) 0.0042(10) -0.0060(10) N2 0.0351(12) 0.0355(13) 0.0560(15) 0.0080(11) -0.0031(10) -0.0026(10) N3 0.0727(18) 0.0465(15) 0.0404(14) 0.0096(11) -0.0189(12) -0.0171(13) B 0.0402(18) 0.046(2) 0.0307(16) -0.0124(14) -0.0020(13) -0.0088(14) Li 0.038(2) 0.033(2) 0.033(2) 0.0012(18) -0.0061(17) -0.0076(18) C1 0.0268(12) 0.0331(13) 0.0235(12) -0.0042(10) -0.0003(9) -0.0007(10) C2 0.0274(12) 0.0256(12) 0.0222(11) -0.0024(9) 0.0011(9) 0.0022(9) C3 0.0302(15) 0.101(3) 0.0520(18) -0.0028(18) -0.0005(13) 0.0097(16) C4 0.0535(19) 0.0435(18) 0.096(3) -0.0012(17) 0.0301(18) -0.0082(15) C5 0.0390(15) 0.0582(19) 0.0372(15) 0.0023(13) 0.0129(12) -0.0011(13) C6 0.0485(16) 0.0391(15) 0.0241(12) -0.0043(11) 0.0059(11) -0.0045(12) C7 0.073(2) 0.0353(16) 0.0569(19) 0.0007(14) 0.0107(16) 0.0073(15) C8 0.136(4) 0.0428(19) 0.055(2) 0.0058(16) 0.028(2) 0.007(2) C9 0.0366(14) 0.0427(16) 0.0285(13) -0.0059(11) 0.0014(11) 0.0057(11) C10 0.0436(16) 0.077(2) 0.0376(16) -0.0044(15) 0.0091(13) 0.0180(15) C11 0.060(2) 0.115(3) 0.050(2) -0.008(2) 0.0125(16) 0.041(2) C12 0.072(3) 0.087(3) 0.127(4) -0.021(3) 0.046(3) -0.007(2) C13 0.076(3) 0.058(2) 0.092(3) 0.014(2) -0.027(2) 0.0107(19) C14 0.0479(18) 0.0387(17) 0.096(3) -0.0062(17) 0.0080(17) -0.0102(14) C15 0.0406(16) 0.0362(16) 0.070(2) 0.0061(14) 0.0089(14) -0.0088(12) C16 0.0499(19) 0.057(2) 0.112(3) 0.000(2) 0.033(2) 0.0039(16) C17 0.0489(19) 0.059(2) 0.093(3) 0.0152(19) -0.0313(18) -0.0182(16) C18 0.065(2) 0.079(3) 0.075(2) 0.027(2) -0.0345(19) -0.0094(19) C19 0.151(4) 0.089(3) 0.041(2) 0.0098(19) 0.006(2) -0.024(3) C20 0.114(3) 0.052(2) 0.073(2) 0.0265(18) -0.033(2) -0.020(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 P B 1.924(3) . ? P C1 1.711(2) . ? P C6 1.839(3) . ? P C9 1.848(2) . ? Si C1 1.808(2) . ? Si C3 1.884(3) . ? Si C4 1.883(3) . ? Si C5 1.881(3) . ? N1 Li 2.124(5) . ? N1 C12 1.482(4) . ? N1 C13 1.447(4) . ? N1 C14 1.470(4) . ? N2 Li 2.094(5) . ? N2 C15 1.468(3) . ? N2 C16 1.469(4) . ? N2 C17 1.472(4) . ? N3 Li 2.125(5) . ? N3 C18 1.461(5) . ? N3 C19 1.456(5) . ? N3 C20 1.479(4) . ? B H0A 1.11(3) . ? B H0B 1.13(3) . ? B H0C 1.07(3) . ? B Li 2.282(5) . ? Li H0B 1.94(3) . ? Li H0C 2.05(3) . ? Li C18 2.787(5) . ? C1 C2 1.535(3) . ? C2 C2 1.542(4) 3_666 ? C2 H2A 0.990 . ? C2 H2B 0.990 . ? 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 0.990 . ? C6 H6B 0.990 . ? C6 C7 1.516(4) . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C7 C8 1.518(4) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.516(4) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.516(4) . ? C11 H11A 0.980 . ? C11 H11B 0.980 . ? C11 H11C 0.980 . ? C12 H12A 0.980 . ? C12 H12B 0.980 . ? C12 H12C 0.980 . ? C13 H13A 0.980 . ? C13 H13B 0.980 . ? C13 H13C 0.980 . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C14 C15 1.509(4) . ? C15 H15A 0.990 . ? C15 H15B 0.990 . ? C16 H16A 0.980 . ? C16 H16B 0.980 . ? C16 H16C 0.980 . ? C17 H17A 0.990 . ? C17 H17B 0.990 . ? C17 C18 1.487(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 . ? 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 C1 119.24(13) . . ? B P C6 105.86(14) . . ? B P C9 105.84(14) . . ? C1 P C6 111.09(12) . . ? C1 P C9 112.14(11) . . ? C6 P C9 100.92(12) . . ? C1 Si C3 115.66(13) . . ? C1 Si C4 115.65(13) . . ? C1 Si C5 109.83(12) . . ? C3 Si C4 105.44(17) . . ? C3 Si C5 104.36(14) . . ? C4 Si C5 104.79(15) . . ? Li N1 C12 119.3(3) . . ? Li N1 C13 108.3(2) . . ? Li N1 C14 102.4(2) . . ? C12 N1 C13 107.5(3) . . ? C12 N1 C14 107.6(3) . . ? C13 N1 C14 111.7(3) . . ? Li N2 C15 105.4(2) . . ? Li N2 C16 114.9(2) . . ? Li N2 C17 103.1(2) . . ? C15 N2 C16 110.0(2) . . ? C15 N2 C17 111.6(2) . . ? C16 N2 C17 111.6(3) . . ? Li N3 C18 100.4(2) . . ? Li N3 C19 114.4(3) . . ? Li N3 C20 113.2(2) . . ? C18 N3 C19 111.6(3) . . ? C18 N3 C20 109.9(3) . . ? C19 N3 C20 107.3(3) . . ? P B H0A 113.3(16) . . ? P B H0B 105.4(14) . . ? P B H0C 109.8(14) . . ? H0A B H0B 109(2) . . ? H0A B H0C 111(2) . . ? H0B B H0C 108(2) . . ? N1 Li N2 87.04(17) . . ? N1 Li N3 121.2(2) . . ? N1 Li H0B 111.6(8) . . ? N1 Li H0C 101.9(8) . . ? N1 Li C18 122.7(2) . . ? N2 Li N3 87.55(18) . . ? N2 Li H0B 149.5(9) . . ? N2 Li H0C 101.2(8) . . ? N2 Li C18 58.16(14) . . ? N3 Li H0B 101.6(8) . . ? N3 Li H0C 136.5(8) . . ? N3 Li C18 31.04(12) . . ? H0B Li H0C 52.7(11) . . ? H0B Li C18 121.1(8) . . ? H0C Li C18 126.7(8) . . ? P C1 Si 121.78(13) . . ? P C1 C2 117.53(16) . . ? Si C1 C2 120.53(16) . . ? C1 C2 C2 117.0(2) . 3_666 ? C1 C2 H2A 108.0 . . ? C1 C2 H2B 108.0 . . ? C2 C2 H2A 108.0 3_666 . ? C2 C2 H2B 108.0 3_666 . ? H2A C2 H2B 107.3 . . ? Si C3 H3A 109.5 . . ? Si C3 H3B 109.5 . . ? Si C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si C4 H4A 109.5 . . ? Si C4 H4B 109.5 . . ? Si C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si C5 H5A 109.5 . . ? Si C5 H5B 109.5 . . ? Si C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? P C6 H6A 109.0 . . ? P C6 H6B 109.0 . . ? P C6 C7 113.00(19) . . ? H6A C6 H6B 107.8 . . ? H6A C6 C7 109.0 . . ? H6B C6 C7 109.0 . . ? C6 C7 H7A 109.1 . . ? C6 C7 H7B 109.1 . . ? C6 C7 C8 112.5(3) . . ? H7A C7 H7B 107.8 . . ? H7A C7 C8 109.1 . . ? H7B C7 C8 109.1 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P C9 H9A 107.6 . . ? P C9 H9B 107.6 . . ? P C9 C10 118.75(19) . . ? H9A C9 H9B 107.1 . . ? H9A C9 C10 107.6 . . ? H9B C9 C10 107.6 . . ? C9 C10 H10A 108.9 . . ? C9 C10 H10B 108.9 . . ? C9 C10 C11 113.3(2) . . ? H10A C10 H10B 107.7 . . ? H10A C10 C11 108.9 . . ? H10B C10 C11 108.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N1 C13 H13A 109.5 . . ? N1 C13 H13B 109.5 . . ? N1 C13 H13C 109.5 . . ? H13A C13 H13B 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 H14A 109.0 . . ? N1 C14 H14B 109.0 . . ? N1 C14 C15 112.8(3) . . ? H14A C14 H14B 107.8 . . ? H14A C14 C15 109.0 . . ? H14B C14 C15 109.0 . . ? N2 C15 C14 113.4(2) . . ? N2 C15 H15A 108.9 . . ? N2 C15 H15B 108.9 . . ? C14 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? 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 . . ? N2 C17 H17A 109.3 . . ? N2 C17 H17B 109.3 . . ? N2 C17 C18 111.6(3) . . ? H17A C17 H17B 108.0 . . ? H17A C17 C18 109.3 . . ? H17B C17 C18 109.3 . . ? N3 C18 Li 48.59(16) . . ? N3 C18 C17 112.7(3) . . ? N3 C18 H18A 109.1 . . ? N3 C18 H18B 109.1 . . ? Li C18 C17 75.81(19) . . ? Li C18 H18A 93.6 . . ? Li C18 H18B 154.2 . . ? C17 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.683 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.047 #===END data_ki126 _database_code_depnum_ccdc_archive 'CCDC 225175' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H58 B2 P2 Si2' _chemical_formula_sum 'C22 H58 B2 P2 Si2' _chemical_formula_weight 462.42 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' 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' B B 0.0013 0.0007 '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/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 14.1618(11) _cell_length_b 6.9841(5) _cell_length_c 16.5204(12) _cell_angle_alpha 90.00 _cell_angle_beta 107.859(2) _cell_angle_gamma 90.00 _cell_volume 1555.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5915 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.5 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.987 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 516 _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .957 _exptl_absorpt_correction_T_max 0.978 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8510 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2728 _reflns_number_gt 2160 _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^)+(0.0463P)^2^+0.6261P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2728 _refine_ls_number_parameters 133 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0964 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 0.35326(4) 0.41878(8) 0.61072(3) 0.02833(17) Uani 1 1 d . . . Si Si 0.28393(4) 0.25854(9) 0.42131(4) 0.03156(18) Uani 1 1 d . . . B B 0.3819(3) 0.1710(4) 0.66186(19) 0.0466(7) Uani 1 1 d . . . H0A H 0.3754 0.1747 0.7192 0.070 Uiso 1 1 calc R . . H0B H 0.4498 0.1342 0.6652 0.070 Uiso 1 1 calc R . . H0C H 0.3352 0.0773 0.6273 0.070 Uiso 1 1 calc R . . C1 C 0.36455(14) 0.4296(3) 0.50405(12) 0.0250(4) Uani 1 1 d . . . H1 H 0.3442 0.5619 0.4826 0.030 Uiso 1 1 calc R . . C2 C 0.47519(15) 0.4063(3) 0.50562(14) 0.0289(5) Uani 1 1 d . . . H2A H 0.5135 0.3479 0.5605 0.035 Uiso 1 1 calc R . . H2B H 0.4776 0.3170 0.4598 0.035 Uiso 1 1 calc R . . C3 C 0.15608(19) 0.2233(4) 0.42761(19) 0.0543(7) Uani 1 1 d . . . H3A H 0.1248 0.3482 0.4282 0.081 Uiso 1 1 calc R . . H3B H 0.1592 0.1534 0.4798 0.081 Uiso 1 1 calc R . . H3C H 0.1170 0.1497 0.3782 0.081 Uiso 1 1 calc R . . C4 C 0.34381(18) 0.0190(3) 0.42840(16) 0.0444(6) Uani 1 1 d . . . H4A H 0.2978 -0.0707 0.3904 0.067 Uiso 1 1 calc R . . H4B H 0.3609 -0.0280 0.4870 0.067 Uiso 1 1 calc R . . H4C H 0.4042 0.0298 0.4115 0.067 Uiso 1 1 calc R . . C5 C 0.2715(2) 0.3718(4) 0.31655(16) 0.0515(7) Uani 1 1 d . . . H5A H 0.3371 0.3824 0.3086 0.077 Uiso 1 1 calc R . . H5B H 0.2425 0.4997 0.3148 0.077 Uiso 1 1 calc R . . H5C H 0.2284 0.2928 0.2710 0.077 Uiso 1 1 calc R . . C6 C 0.22941(16) 0.4990(3) 0.60541(14) 0.0339(5) Uani 1 1 d . . . H6A H 0.1817 0.3980 0.5770 0.041 Uiso 1 1 calc R . . H6B H 0.2264 0.5109 0.6643 0.041 Uiso 1 1 calc R . . C7 C 0.19455(17) 0.6876(3) 0.55961(17) 0.0400(6) Uani 1 1 d . . . H7A H 0.2422 0.7900 0.5864 0.048 Uiso 1 1 calc R . . H7B H 0.1933 0.6759 0.4996 0.048 Uiso 1 1 calc R . . C8 C 0.09212(19) 0.7426(4) 0.56258(17) 0.0485(6) Uani 1 1 d . . . H8A H 0.0437 0.6475 0.5314 0.073 Uiso 1 1 calc R . . H8B H 0.0743 0.8688 0.5364 0.073 Uiso 1 1 calc R . . H8C H 0.0922 0.7472 0.6219 0.073 Uiso 1 1 calc R . . C9 C 0.43526(16) 0.6036(3) 0.67237(14) 0.0334(5) Uani 1 1 d . . . H9A H 0.5046 0.5680 0.6780 0.040 Uiso 1 1 calc R . . H9B H 0.4209 0.7254 0.6403 0.040 Uiso 1 1 calc R . . C10 C 0.4266(2) 0.6369(4) 0.76074(15) 0.0506(7) Uani 1 1 d . . . H10A H 0.4299 0.5121 0.7900 0.061 Uiso 1 1 calc R . . H10B H 0.3612 0.6949 0.7555 0.061 Uiso 1 1 calc R . . C11 C 0.5080(2) 0.7672(4) 0.81432(16) 0.0565(8) Uani 1 1 d . . . H11A H 0.5728 0.7077 0.8218 0.085 Uiso 1 1 calc R . . H11B H 0.4986 0.7869 0.8701 0.085 Uiso 1 1 calc R . . H11C H 0.5051 0.8908 0.7856 0.085 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 0.0349(3) 0.0218(3) 0.0303(3) 0.0031(2) 0.0131(2) -0.0001(2) Si 0.0313(3) 0.0282(3) 0.0346(3) -0.0025(3) 0.0091(3) 0.0003(2) B 0.073(2) 0.0277(14) 0.0446(17) 0.0112(13) 0.0257(15) 0.0047(14) C1 0.0274(11) 0.0187(10) 0.0304(11) 0.0030(8) 0.0111(9) 0.0030(8) C2 0.0303(12) 0.0233(10) 0.0340(11) 0.0043(9) 0.0114(9) 0.0027(9) C3 0.0392(14) 0.0551(17) 0.0696(18) -0.0219(14) 0.0183(13) -0.0133(12) C4 0.0509(15) 0.0309(12) 0.0478(15) -0.0083(11) 0.0099(12) 0.0035(11) C5 0.0570(17) 0.0535(16) 0.0374(14) 0.0023(12) 0.0047(12) -0.0005(13) C6 0.0355(12) 0.0326(12) 0.0390(12) -0.0025(10) 0.0192(10) -0.0034(10) C7 0.0331(13) 0.0325(12) 0.0568(15) -0.0002(11) 0.0171(11) 0.0019(10) C8 0.0442(14) 0.0549(16) 0.0510(15) -0.0038(13) 0.0216(12) 0.0128(12) C9 0.0357(12) 0.0294(11) 0.0340(12) -0.0006(10) 0.0090(10) 0.0010(9) C10 0.0686(18) 0.0488(16) 0.0348(14) -0.0038(11) 0.0164(12) -0.0083(13) C11 0.078(2) 0.0441(15) 0.0345(14) -0.0039(12) -0.0016(13) 0.0038(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P B 1.914(3) . ? P C1 1.819(2) . ? P C6 1.818(2) . ? P C9 1.824(2) . ? Si C1 1.908(2) . ? Si C3 1.861(3) . ? Si C4 1.863(2) . ? Si C5 1.861(3) . ? C1 C2 1.568(3) . ? C2 C2 1.524(4) 3_666 ? C6 C7 1.523(3) . ? C7 C8 1.516(3) . ? C9 C10 1.520(3) . ? C10 C11 1.522(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag B P C1 113.30(11) . . ? B P C6 111.76(13) . . ? B P C9 112.39(12) . . ? C1 P C6 108.10(10) . . ? C1 P C9 106.36(10) . . ? C6 P C9 104.39(11) . . ? C1 Si C3 114.91(11) . . ? C1 Si C4 110.86(10) . . ? C1 Si C5 105.38(11) . . ? C3 Si C4 108.03(12) . . ? C3 Si C5 106.98(13) . . ? C4 Si C5 110.57(13) . . ? P C1 Si 117.19(11) . . ? P C1 C2 111.35(13) . . ? Si C1 C2 108.81(13) . . ? C1 C2 C2 113.9(2) . 3_666 ? P C6 C7 116.83(15) . . ? C6 C7 C8 111.8(2) . . ? P C9 C10 114.80(17) . . ? C9 C10 C11 112.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B P C1 Si 58.14(16) . . . . ? B P C1 C2 -68.01(17) . . . . ? C6 P C1 Si -66.28(13) . . . . ? C6 P C1 C2 167.57(13) . . . . ? C9 P C1 Si -177.90(11) . . . . ? C9 P C1 C2 55.95(15) . . . . ? C3 Si C1 P 38.87(16) . . . . ? C3 Si C1 C2 166.26(15) . . . . ? C4 Si C1 P -83.97(14) . . . . ? C4 Si C1 C2 43.42(17) . . . . ? C5 Si C1 P 156.37(12) . . . . ? C5 Si C1 C2 -76.24(16) . . . . ? P C1 C2 C2 -102.7(2) . . . 3_666 ? Si C1 C2 C2 126.7(2) . . . 3_666 ? B P C6 C7 -175.29(18) . . . . ? C1 P C6 C7 -49.9(2) . . . . ? C9 P C6 C7 62.99(19) . . . . ? P C6 C7 C8 -177.72(17) . . . . ? B P C9 C10 -63.3(2) . . . . ? C1 P C9 C10 172.16(17) . . . . ? C6 P C9 C10 58.0(2) . . . . ? P C9 C10 C11 170.36(17) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.343 _refine_diff_density_min -0.173 _refine_diff_density_rms 0.046 #===END