# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1339 data_global _publ_requested_journal 'Chem.Comm' _publ_contact_author 'Mark A. Fox' _publ_contact_author_address ; Chemistry Department, Durham University Science Laboratories, South Road, Durham, DH1 3LE U.K. ; _publ_contact_author_email 'm.a.fox@durham.ac.uk' _publ_section_title ; Deboronation of ortho-carborane by an iminophosphorane: crystal structures of the novel carborane adduct nido-C2B10H12.HNP(NMe2)3 and the borenium salt {[(NMe2)3PN]2B[HNP(NMe2)3]}2O^2+^[C2B9H12^-^]2 ; loop_ _publ_author_name 'Davidson, Matthew G.' 'Fox, Mark A.' 'Hibbert, Thomas G.' 'Howard, Judith A. K.' 'Mackinnon, Angus' 'Neretin, Ivan S.' 'Wade, Kenneth' _journal_name_full 'Chemical Communications' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1999' _ccdc_journal_depnumber '?' #===========================================END data_(3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '1,2-dicarbadodecaborane-imino-tris(dimethylamino)phosphorane adduct' _chemical_melting_point ? _chemical_formula_moiety 'C2 H12 B10,C6 H19 N4 P' _chemical_formula_sum 'C8 H31 B10 N4 P' _chemical_formula_weight 322.44 _ccdc_compound_id '3' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; ? ; _ccdc_comments '?' 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.799(2) _cell_length_b 17.252(4) _cell_length_c 20.326(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3786.9(13) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.141 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 10 s), each set at different \f and/or 2\q angles, nominally covered over a hemisphere of reciprocal space. The first 50 scans were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 25525 _diffrn_reflns_av_R_equivalents 0.1712 _diffrn_reflns_av_sigmaI/netI 0.1165 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4337 _reflns_number_gt 2221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+4.3755P] 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 SHELXL _refine_ls_extinction_coef 0.0006(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4337 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1681 _refine_ls_R_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.1873 _refine_ls_wR_factor_gt 0.1457 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.25223(9) 0.24518(6) 0.64315(4) 0.0242(2) Uani 1 1 d . . . N1 N 0.3050(3) 0.2853(2) 0.71138(16) 0.0300(8) Uani 1 1 d . . . H1 H 0.369(4) 0.270(3) 0.716(2) 0.051(16) Uiso 1 1 d . . . B1 B 0.2551(5) 0.4897(3) 0.9143(2) 0.0364(10) Uani 1 1 d . . . H1' H 0.280(4) 0.526(3) 0.955(2) 0.062(14) Uiso 1 1 d . . . N2 N 0.3415(3) 0.17456(18) 0.61935(16) 0.0322(8) Uani 1 1 d . . . B2 B 0.1657(5) 0.4030(3) 0.9233(2) 0.0379(12) Uani 1 1 d . . . H2 H 0.122(4) 0.379(2) 0.9700(19) 0.044(12) Uiso 1 1 d . . . N3 N 0.2531(3) 0.30910(17) 0.58438(13) 0.0265(7) Uani 1 1 d . . . B3 B 0.0993(5) 0.4853(3) 0.8843(2) 0.0360(11) Uani 1 1 d . . . H3 H 0.016(4) 0.519(2) 0.9001(17) 0.043(11) Uiso 1 1 d . . . N4 N 0.1135(3) 0.21379(18) 0.65895(15) 0.0263(7) Uani 1 1 d . . . B4 B 0.2167(5) 0.5293(3) 0.8358(3) 0.0358(12) Uani 1 1 d . . . H4 H 0.207(3) 0.589(2) 0.8251(17) 0.034(11) Uiso 1 1 d . . . B5 B 0.3543(4) 0.4767(3) 0.8456(2) 0.0327(11) Uani 1 1 d . . . H5 H 0.449(4) 0.506(2) 0.8433(18) 0.043(11) Uiso 1 1 d . . . B6 B 0.3226(4) 0.3969(3) 0.9009(2) 0.0335(11) Uani 1 1 d . . . H6 H 0.393(3) 0.3727(19) 0.9355(16) 0.023(9) Uiso 1 1 d . . . C7 C 0.0929(4) 0.3950(2) 0.8501(2) 0.0347(10) Uani 1 1 d . . . H7 H 0.004(4) 0.370(2) 0.8485(19) 0.047(12) Uiso 1 1 d . . . C8 C 0.1197(4) 0.4621(2) 0.8029(2) 0.0329(10) Uani 1 1 d . . . H8 H 0.053(4) 0.480(2) 0.7736(19) 0.048(13) Uiso 1 1 d . . . B9 B 0.2623(4) 0.4586(3) 0.7739(2) 0.0296(10) Uani 1 1 d . . . H9 H 0.281(4) 0.482(2) 0.7221(19) 0.044(12) Uiso 1 1 d . . . B10 B 0.3383(4) 0.3809(3) 0.8148(2) 0.0278(10) Uani 1 1 d . . . H10 H 0.430(3) 0.3477(19) 0.8055(16) 0.025(9) Uiso 1 1 d . . . B11 B 0.2124(4) 0.3359(3) 0.8586(2) 0.0305(10) Uani 1 1 d . . . H11 H 0.198(3) 0.275(2) 0.8729(16) 0.028(10) Uiso 1 1 d . . . B12 B 0.2370(4) 0.3397(3) 0.7566(2) 0.0295(10) Uani 1 1 d . . . H12 H 0.131(3) 0.341(2) 0.7422(17) 0.030(10) Uiso 1 1 d . . . C21 C 0.4707(4) 0.1883(3) 0.6000(2) 0.0446(12) Uani 1 1 d . . . H21A H 0.4890 0.2438 0.6028 0.067 Uiso 1 1 calc R . . H21B H 0.4832 0.1705 0.5546 0.067 Uiso 1 1 calc R . . H21C H 0.5260 0.1596 0.6295 0.067 Uiso 1 1 calc R . . C22 C 0.3013(4) 0.0943(2) 0.6110(2) 0.0432(11) Uani 1 1 d . . . H22A H 0.2113 0.0912 0.6165 0.065 Uiso 1 1 calc R . . H22B H 0.3418 0.0616 0.6440 0.065 Uiso 1 1 calc R . . H22C H 0.3237 0.0763 0.5668 0.065 Uiso 1 1 calc R . . C31 C 0.2665(4) 0.2900(3) 0.51390(18) 0.0404(11) Uani 1 1 d . . . H31A H 0.2869 0.2350 0.5092 0.061 Uiso 1 1 calc R . . H31B H 0.3330 0.3215 0.4948 0.061 Uiso 1 1 calc R . . H31C H 0.1886 0.3010 0.4910 0.061 Uiso 1 1 calc R . . C32 C 0.2135(4) 0.3897(2) 0.5955(2) 0.0399(11) Uani 1 1 d . . . H32A H 0.2745 0.4251 0.5763 0.060 Uiso 1 1 calc R . . H32B H 0.2071 0.3994 0.6429 0.060 Uiso 1 1 calc R . . H32C H 0.1327 0.3982 0.5748 0.060 Uiso 1 1 calc R . . C41 C 0.0172(4) 0.2100(2) 0.6073(2) 0.0378(10) Uani 1 1 d . . . H41A H 0.0109 0.1568 0.5908 0.057 Uiso 1 1 calc R . . H41B H 0.0394 0.2448 0.5711 0.057 Uiso 1 1 calc R . . H41C H -0.0627 0.2259 0.6259 0.057 Uiso 1 1 calc R . . C42 C 0.0848(4) 0.1690(3) 0.71854(19) 0.0380(10) Uani 1 1 d . . . H42A H 0.0061 0.1870 0.7371 0.057 Uiso 1 1 calc R . . H42B H 0.1510 0.1763 0.7510 0.057 Uiso 1 1 calc R . . H42C H 0.0782 0.1140 0.7073 0.057 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 0.0190(4) 0.0250(5) 0.0287(4) 0.0019(4) -0.0007(5) 0.0024(5) N1 0.0187(17) 0.040(2) 0.0313(18) 0.0005(15) -0.0046(15) 0.0058(16) B1 0.040(3) 0.037(3) 0.032(2) -0.007(2) 0.007(2) -0.001(3) N2 0.0179(16) 0.0254(18) 0.053(2) 0.0014(16) 0.0064(15) 0.0006(14) B2 0.036(3) 0.043(3) 0.035(3) 0.004(2) 0.006(2) 0.001(2) N3 0.0313(17) 0.0218(16) 0.0264(14) 0.0004(12) -0.0013(15) 0.0016(15) B3 0.032(3) 0.028(3) 0.048(3) -0.006(2) 0.011(2) 0.004(2) N4 0.0162(15) 0.0284(18) 0.0343(17) 0.0033(14) 0.0008(13) 0.0010(13) B4 0.037(3) 0.022(3) 0.048(3) 0.003(2) 0.004(2) 0.000(2) B5 0.026(2) 0.032(3) 0.040(3) -0.005(2) -0.001(2) -0.008(2) B6 0.026(2) 0.044(3) 0.030(2) 0.005(2) -0.002(2) 0.003(2) C7 0.023(2) 0.029(2) 0.051(3) -0.001(2) 0.0023(19) -0.0030(18) C8 0.027(2) 0.031(2) 0.040(2) -0.0005(19) -0.0019(19) 0.0049(18) B9 0.024(2) 0.030(2) 0.035(2) 0.0036(19) 0.001(2) -0.003(2) B10 0.018(2) 0.035(3) 0.031(2) -0.001(2) -0.0020(19) -0.0016(19) B11 0.022(2) 0.031(3) 0.039(3) 0.010(2) 0.0059(19) 0.0014(18) B12 0.029(3) 0.029(2) 0.030(2) -0.0009(18) -0.002(2) 0.001(2) C21 0.021(2) 0.042(3) 0.071(3) -0.003(2) 0.010(2) 0.0047(19) C22 0.029(2) 0.031(3) 0.070(3) 0.001(2) 0.012(2) 0.0014(19) C31 0.046(3) 0.047(3) 0.028(2) -0.0029(18) 0.000(2) 0.007(2) C32 0.055(3) 0.030(2) 0.034(2) 0.0021(18) -0.004(2) 0.009(2) C41 0.024(2) 0.041(3) 0.048(2) -0.002(2) -0.006(2) -0.0013(19) C42 0.029(2) 0.043(3) 0.042(2) 0.006(2) 0.0075(19) -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 N4 1.625(3) . ? P1 N3 1.626(3) . ? P1 N2 1.627(3) . ? P1 N1 1.651(3) . ? N1 B12 1.506(6) . ? N1 H1 0.75(4) . ? B1 B5 1.774(7) . ? B1 B6 1.779(7) . ? B1 B4 1.784(7) . ? B1 B2 1.789(7) . ? B1 B3 1.791(7) . ? B1 H1' 1.08(4) . ? N2 C22 1.461(5) . ? N2 C21 1.469(5) . ? B2 C7 1.689(7) . ? B2 B6 1.757(7) . ? B2 B3 1.777(7) . ? B2 B11 1.822(7) . ? B2 H2 1.14(4) . ? N3 C32 1.472(5) . ? N3 C31 1.477(4) . ? B3 C7 1.708(6) . ? B3 C8 1.715(6) . ? B3 B4 1.775(7) . ? B3 H3 1.12(4) . ? N4 C42 1.469(5) . ? N4 C41 1.479(5) . ? B4 C8 1.699(6) . ? B4 B5 1.753(7) . ? B4 B9 1.821(7) . ? B4 H4 1.06(4) . ? B5 B10 1.776(6) . ? B5 B9 1.792(6) . ? B5 B6 1.811(7) . ? B5 H5 1.14(4) . ? B6 B10 1.781(6) . ? B6 B11 1.806(7) . ? B6 H6 1.12(3) . ? C7 C8 1.530(6) . ? C7 B11 1.654(6) . ? C7 H7 1.05(4) . ? C8 B9 1.651(6) . ? C8 H8 0.98(4) . ? B9 B10 1.779(6) . ? B9 B12 2.099(6) . ? B9 H9 1.14(4) . ? B10 B12 1.761(6) . ? B10 B11 1.802(6) . ? B10 H10 1.16(3) . ? B11 B12 2.091(6) . ? B11 H11 1.10(4) . ? B12 H12 1.18(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 N4 P1 N3 112.10(16) . . ? N4 P1 N2 110.82(16) . . ? N3 P1 N2 106.63(16) . . ? N4 P1 N1 106.97(17) . . ? N3 P1 N1 109.33(17) . . ? N2 P1 N1 111.03(18) . . ? B12 N1 P1 127.3(3) . . ? B12 N1 H1 127(4) . . ? P1 N1 H1 106(4) . . ? B5 B1 B6 61.3(3) . . ? B5 B1 B4 59.0(3) . . ? B6 B1 B4 107.7(3) . . ? B5 B1 B2 107.5(3) . . ? B6 B1 B2 59.0(3) . . ? B4 B1 B2 106.6(3) . . ? B5 B1 B3 107.1(3) . . ? B6 B1 B3 107.2(3) . . ? B4 B1 B3 59.5(3) . . ? B2 B1 B3 59.5(3) . . ? B5 B1 H1' 122(2) . . ? B6 B1 H1' 122(2) . . ? B4 B1 H1' 122(2) . . ? B2 B1 H1' 123(2) . . ? B3 B1 H1' 122(2) . . ? C22 N2 C21 113.8(3) . . ? C22 N2 P1 124.6(3) . . ? C21 N2 P1 121.5(3) . . ? C7 B2 B6 102.5(3) . . ? C7 B2 B3 59.0(3) . . ? B6 B2 B3 108.8(4) . . ? C7 B2 B1 103.3(3) . . ? B6 B2 B1 60.2(3) . . ? B3 B2 B1 60.3(3) . . ? C7 B2 B11 56.0(2) . . ? B6 B2 B11 60.6(3) . . ? B3 B2 B11 107.3(3) . . ? B1 B2 B11 108.0(3) . . ? C7 B2 H2 121(2) . . ? B6 B2 H2 126(2) . . ? B3 B2 H2 120(2) . . ? B1 B2 H2 128(2) . . ? B11 B2 H2 119(2) . . ? C32 N3 C31 112.8(3) . . ? C32 N3 P1 121.8(2) . . ? C31 N3 P1 124.2(3) . . ? C7 B3 C8 53.1(2) . . ? C7 B3 B4 101.1(3) . . ? C8 B3 B4 58.2(3) . . ? C7 B3 B2 57.9(3) . . ? C8 B3 B2 101.0(3) . . ? B4 B3 B2 107.5(3) . . ? C7 B3 B1 102.4(3) . . ? C8 B3 B1 102.6(3) . . ? B4 B3 B1 60.0(3) . . ? B2 B3 B1 60.2(3) . . ? C7 B3 H3 124(2) . . ? C8 B3 H3 120.1(19) . . ? B4 B3 H3 121(2) . . ? B2 B3 H3 127.9(19) . . ? B1 B3 H3 129(2) . . ? C42 N4 C41 114.4(3) . . ? C42 N4 P1 122.1(3) . . ? C41 N4 P1 121.6(3) . . ? C8 B4 B5 102.4(3) . . ? C8 B4 B3 59.1(3) . . ? B5 B4 B3 108.8(3) . . ? C8 B4 B1 103.5(3) . . ? B5 B4 B1 60.2(3) . . ? B3 B4 B1 60.4(3) . . ? C8 B4 B9 55.8(2) . . ? B5 B4 B9 60.2(3) . . ? B3 B4 B9 106.9(3) . . ? B1 B4 B9 107.4(3) . . ? C8 B4 H4 122(2) . . ? B5 B4 H4 128(2) . . ? B3 B4 H4 117(2) . . ? B1 B4 H4 125(2) . . ? B9 B4 H4 122(2) . . ? B4 B5 B1 60.8(3) . . ? B4 B5 B10 111.1(3) . . ? B1 B5 B10 109.6(3) . . ? B4 B5 B9 61.8(3) . . ? B1 B5 B9 109.1(3) . . ? B10 B5 B9 59.8(2) . . ? B4 B5 B6 107.6(3) . . ? B1 B5 B6 59.5(3) . . ? B10 B5 B6 59.5(3) . . ? B9 B5 B6 105.5(3) . . ? B4 B5 H5 122(2) . . ? B1 B5 H5 121.1(19) . . ? B10 B5 H5 119(2) . . ? B9 B5 H5 122.7(19) . . ? B6 B5 H5 122.3(19) . . ? B2 B6 B1 60.8(3) . . ? B2 B6 B10 110.8(3) . . ? B1 B6 B10 109.2(3) . . ? B2 B6 B11 61.5(3) . . ? B1 B6 B11 109.1(3) . . ? B10 B6 B11 60.3(3) . . ? B2 B6 B5 107.3(3) . . ? B1 B6 B5 59.2(3) . . ? B10 B6 B5 59.3(3) . . ? B11 B6 B5 105.8(3) . . ? B2 B6 H6 121.2(17) . . ? B1 B6 H6 121.3(17) . . ? B10 B6 H6 119.6(17) . . ? B11 B6 H6 122.1(18) . . ? B5 B6 H6 123.0(18) . . ? C8 C7 B11 112.6(3) . . ? C8 C7 B2 113.7(3) . . ? B11 C7 B2 66.1(3) . . ? C8 C7 B3 63.7(3) . . ? B11 C7 B3 119.2(3) . . ? B2 C7 B3 63.1(3) . . ? C8 C7 H7 118(2) . . ? B11 C7 H7 117(2) . . ? B2 C7 H7 119(2) . . ? B3 C7 H7 115(2) . . ? C7 C8 B9 111.9(3) . . ? C7 C8 B4 112.7(3) . . ? B9 C8 B4 65.8(3) . . ? C7 C8 B3 63.2(3) . . ? B9 C8 B3 118.2(3) . . ? B4 C8 B3 62.6(3) . . ? C7 C8 H8 119(3) . . ? B9 C8 H8 118(2) . . ? B4 C8 H8 118(3) . . ? B3 C8 H8 115(2) . . ? C8 B9 B10 106.9(3) . . ? C8 B9 B5 102.7(3) . . ? B10 B9 B5 59.7(3) . . ? C8 B9 B4 58.4(3) . . ? B10 B9 B4 107.8(3) . . ? B5 B9 B4 58.0(3) . . ? C8 B9 B12 88.5(3) . . ? B10 B9 B12 53.2(2) . . ? B5 B9 B12 112.2(3) . . ? B4 B9 B12 137.3(3) . . ? C8 B9 H9 119(2) . . ? B10 B9 H9 128(2) . . ? B5 B9 H9 126(2) . . ? B4 B9 H9 117(2) . . ? B12 B9 H9 102(2) . . ? B12 B10 B5 132.2(3) . . ? B12 B10 B9 72.7(3) . . ? B5 B10 B9 60.5(3) . . ? B12 B10 B6 131.6(3) . . ? B5 B10 B6 61.2(3) . . ? B9 B10 B6 107.4(3) . . ? B12 B10 B11 71.9(3) . . ? B5 B10 B11 107.5(3) . . ? B9 B10 B11 102.0(3) . . ? B6 B10 B11 60.6(3) . . ? B12 B10 H10 102.8(17) . . ? B5 B10 H10 115.8(17) . . ? B9 B10 H10 133.7(17) . . ? B6 B10 H10 108.6(16) . . ? B11 B10 H10 120.8(17) . . ? C7 B11 B10 105.8(3) . . ? C7 B11 B6 101.8(3) . . ? B10 B11 B6 59.1(2) . . ? C7 B11 B2 57.9(3) . . ? B10 B11 B2 107.0(3) . . ? B6 B11 B2 57.9(3) . . ? C7 B11 B12 88.6(3) . . ? B10 B11 B12 53.2(2) . . ? B6 B11 B12 111.7(3) . . ? B2 B11 B12 136.9(3) . . ? C7 B11 H11 120.7(19) . . ? B10 B11 H11 130.1(19) . . ? B6 B11 H11 121.4(18) . . ? B2 B11 H11 112.3(18) . . ? B12 B11 H11 108.0(17) . . ? N1 B12 B10 111.0(3) . . ? N1 B12 B11 130.4(3) . . ? B10 B12 B11 55.0(2) . . ? N1 B12 B9 130.4(3) . . ? B10 B12 B9 54.1(2) . . ? B11 B12 B9 83.2(2) . . ? N1 B12 H12 109.3(17) . . ? B10 B12 H12 139.7(17) . . ? B11 B12 H12 97.1(17) . . ? B9 B12 H12 98.8(17) . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.450 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.072 #========================================================END data_(4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; tris(dimethylamino)phosphiniminium 7,8-dicarba-nido-undecaborane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C2 H12 B9 1-,C6 H20 N4 P 1+' _chemical_formula_sum 'C8 H32 B9 N4 P' _chemical_formula_weight 312.64 _ccdc_compound_id '4' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; Hydrogens of the C(7)H3 methyl group are rotationally disordered over 2 positions, A and B, with equal occupancies. ; _ccdc_comments '?' 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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.580(2) _cell_length_b 13.182(3) _cell_length_c 12.385(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.88(5) _cell_angle_gamma 90.00 _cell_volume 1889.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 474 _cell_measurement_theta_min 12 _cell_measurement_theta_max 23 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.140 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9462 _exptl_absorpt_correction_T_max 0.9726 _exptl_absorpt_process_details ? _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 10 s), each set at different \f and/or 2\q angles, nominally covered over a hemisphere of reciprocal space. The first 50 scans (340 reflections) were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 340 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '8 hours' _diffrn_standards_decay_% 0.2 _diffrn_reflns_number 14804 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 29.13 _reflns_number_total 4992 _reflns_number_gt 4283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. Carborane and NH2 hydrogens were located from Fourier map and refined in isotropic approximation (refall). Methyl hydrogens were refined in rigid-body model (for non-overlapping positions) or treated in riding model (for overlapping positions). ; _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^)+(0.0502P)^2^+0.7894P] 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 4992 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.1178 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.006 _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 0.23856(3) 0.70307(2) 0.19997(2) 0.02233(10) Uani 1 1 d . . . N1 N 0.17870(10) 0.60266(9) 0.14852(10) 0.0276(2) Uani 1 1 d . A . H13 H 0.1103(18) 0.5859(15) 0.1664(16) 0.046(5) Uiso 1 1 d . . . H14 H 0.2023(17) 0.5789(15) 0.0901(17) 0.044(5) Uiso 1 1 d . . . N2 N 0.26946(16) 0.68016(15) 0.32750(12) 0.0424(4) Uani 0.815(2) 1 d P A 1 C1 C 0.1800(2) 0.6346(2) 0.39442(14) 0.0695(7) Uani 1 1 d . . . H23 H 0.1276 0.5933 0.3490 0.104 Uiso 0.815(2) 1 d PR A 1 H24 H 0.1367 0.6903 0.4265 0.104 Uiso 0.815(2) 1 d PR A 1 H25 H 0.2147 0.5924 0.4520 0.104 Uiso 0.815(2) 1 d PR A 1 H23A H 0.1544 0.6629 0.4610 0.104 Uiso 0.185(2) 1 d PR A 2 H24A H 0.1222 0.5892 0.3653 0.104 Uiso 0.185(2) 1 d PR A 2 H25A H 0.2508 0.5982 0.4077 0.104 Uiso 0.185(2) 1 d PR A 2 C2 C 0.3692(3) 0.7235(3) 0.3873(2) 0.0789(10) Uani 0.815(2) 1 d P A 1 H26 H 0.4245 0.7500 0.3361 0.095(7) Uiso 0.815(2) 1 d PR A 1 H27 H 0.4064 0.6707 0.4319 0.095(7) Uiso 0.815(2) 1 d PR A 1 H28 H 0.3432 0.7786 0.4337 0.095(7) Uiso 0.815(2) 1 d PR A 1 N2A N 0.1953(6) 0.7150(5) 0.3221(5) 0.0269(13) Uiso 0.185(2) 1 d P A 2 C2A C 0.1846(9) 0.8108(8) 0.3786(9) 0.048(2) Uiso 0.185(2) 1 d P A 2 H26A H 0.1549 0.8627 0.3283 0.072 Uiso 0.185(2) 1 d PR A 2 H27A H 0.2606 0.8316 0.4080 0.072 Uiso 0.185(2) 1 d PR A 2 H28A H 0.1312 0.8030 0.4378 0.072 Uiso 0.185(2) 1 d PR A 2 N3 N 0.36214(13) 0.72163(12) 0.14397(18) 0.0322(4) Uani 0.815(2) 1 d P A 1 C3 C 0.45679(17) 0.64834(19) 0.1518(3) 0.0626(8) Uani 0.815(2) 1 d P A 1 H29 H 0.4398 0.5971 0.2064 0.077(6) Uiso 0.815(2) 1 d PR A 1 H30 H 0.5287 0.6835 0.1725 0.077(6) Uiso 0.815(2) 1 d PR A 1 H31 H 0.4653 0.6152 0.0817 0.077(6) Uiso 0.815(2) 1 d PR A 1 C4 C 0.37741(17) 0.79853(15) 0.06071(15) 0.0363(4) Uani 0.815(2) 1 d P A 1 H32 H 0.3122 0.8459 0.0605 0.056(4) Uiso 0.815(2) 1 d PR A 1 H33 H 0.3808 0.7656 -0.0100 0.056(4) Uiso 0.815(2) 1 d PR A 1 H34 H 0.4495 0.8356 0.0758 0.056(4) Uiso 0.815(2) 1 d PR A 1 N3A N 0.3719(7) 0.7164(6) 0.1888(7) 0.0298(19) Uiso 0.185(2) 1 d P A 2 C3A C 0.4518(9) 0.6825(8) 0.2779(8) 0.048(2) Uiso 0.185(2) 1 d P A 2 H29A H 0.4668 0.6096 0.2708 0.073 Uiso 0.185(2) 1 d PR A 2 H30A H 0.4167 0.6957 0.3474 0.073 Uiso 0.185(2) 1 d PR A 2 H31A H 0.5248 0.7199 0.2743 0.073 Uiso 0.185(2) 1 d PR A 2 C4A C 0.4276(10) 0.7265(9) 0.0844(9) 0.054(3) Uiso 0.185(2) 1 d P A 2 H32A H 0.4889 0.7777 0.0905 0.081 Uiso 0.185(2) 1 d PR A 2 H33A H 0.3702 0.7473 0.0288 0.081 Uiso 0.185(2) 1 d PR A 2 H34A H 0.4611 0.6611 0.0645 0.081 Uiso 0.185(2) 1 d PR A 2 N4 N 0.15225(13) 0.79660(11) 0.18690(14) 0.0335(4) Uani 0.815(2) 1 d P A 1 C5 C 0.07110(15) 0.80966(14) 0.09166(16) 0.0477(4) Uani 1 1 d . . . H37A H 0.0564 0.8716 0.0528 0.072 Uiso 0.185(2) 1 d PR A 2 H36A H 0.0545 0.7529 0.0451 0.072 Uiso 0.185(2) 1 d PR A 2 H35A H 0.0227 0.8067 0.1531 0.072 Uiso 0.185(2) 1 d PR A 2 H35 H 0.0662 0.7460 0.0509 0.072 Uiso 0.815(2) 1 d PR A 1 H36 H 0.0989 0.8638 0.0449 0.072 Uiso 0.815(2) 1 d PR A 1 H37 H -0.0056 0.8275 0.1170 0.072 Uiso 0.815(2) 1 d PR A 1 C6 C 0.1679(2) 0.88670(19) 0.2552(3) 0.0713(9) Uani 0.815(2) 1 d P A 1 H38 H 0.2231 0.8715 0.3147 0.108(8) Uiso 0.815(2) 1 d PR A 1 H39 H 0.0936 0.9062 0.2847 0.108(8) Uiso 0.815(2) 1 d PR A 1 H40 H 0.1975 0.9427 0.2121 0.108(8) Uiso 0.815(2) 1 d PR A 1 N4A N 0.1864(5) 0.8062(5) 0.1282(5) 0.0257(13) Uiso 0.185(2) 1 d P A 2 C6A C 0.2431(9) 0.9071(8) 0.1279(8) 0.049(2) Uiso 0.185(2) 1 d P A 2 H38A H 0.3180 0.9029 0.1668 0.074 Uiso 0.185(2) 1 d PR A 2 H39A H 0.1940 0.9565 0.1637 0.074 Uiso 0.185(2) 1 d PR A 2 H40A H 0.2547 0.9287 0.0534 0.074 Uiso 0.185(2) 1 d PR A 2 B1 B 0.91979(13) 0.46410(11) 0.22737(13) 0.0281(3) Uani 1 1 d . . . H1 H 1.0099(16) 0.4371(14) 0.2310(15) 0.041(5) Uiso 1 1 d . . . B2 B 0.85161(14) 0.51574(11) 0.33986(13) 0.0287(3) Uani 1 1 d . . . H2 H 0.8926(16) 0.5294(15) 0.4187(16) 0.045(5) Uiso 1 1 d . . . B3 B 0.88614(13) 0.59521(11) 0.23195(14) 0.0299(3) Uani 1 1 d . . . H3 H 0.9423(16) 0.6613(14) 0.2401(15) 0.041(5) Uiso 1 1 d . . . B4 B 0.86527(14) 0.52702(12) 0.11049(13) 0.0303(3) Uani 1 1 d . . . H4 H 0.9139(16) 0.5510(14) 0.0422(15) 0.042(5) Uiso 1 1 d . . . B5 B 0.81095(14) 0.40644(11) 0.14131(12) 0.0277(3) Uani 1 1 d . . . H5 H 0.8296(15) 0.3388(14) 0.0916(15) 0.040(5) Uiso 1 1 d . . . B6 B 0.80133(14) 0.39926(11) 0.28770(12) 0.0284(3) Uani 1 1 d . . . H6 H 0.8152(15) 0.3276(14) 0.3325(15) 0.039(5) Uiso 1 1 d . . . C7 C 0.75106(11) 0.59767(10) 0.28416(11) 0.0276(3) Uani 1 1 d . . . H7 H 0.7348(16) 0.6607(15) 0.3187(15) 0.040(5) Uiso 1 1 d . . . C8 C 0.75758(12) 0.60248(10) 0.15907(12) 0.0299(3) Uani 1 1 d . . . H8 H 0.7482(16) 0.6691(15) 0.1294(16) 0.044(5) Uiso 1 1 d . . . B9 B 0.71312(14) 0.50171(13) 0.09761(13) 0.0316(3) Uani 1 1 d . . . H9 H 0.6715(17) 0.5054(15) 0.0177(16) 0.051(5) Uiso 1 1 d . . . B10 B 0.67458(14) 0.41229(12) 0.20372(13) 0.0308(3) Uani 1 1 d . . . H10 H 0.6151(16) 0.3474(15) 0.1953(15) 0.046(5) Uiso 1 1 d . . . B11 B 0.69853(14) 0.49176(12) 0.32581(12) 0.0292(3) Uani 1 1 d . . . H11 H 0.6495(16) 0.4847(15) 0.3993(16) 0.046(5) Uiso 1 1 d . . . H12 H 0.627(2) 0.485(2) 0.220(2) 0.080(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P1 0.02178(16) 0.02498(17) 0.02021(16) -0.00005(11) 0.00050(11) -0.00331(11) N1 0.0252(5) 0.0294(6) 0.0283(6) -0.0062(4) 0.0036(4) -0.0048(4) N2 0.0486(10) 0.0559(10) 0.0219(7) 0.0051(7) -0.0091(6) -0.0198(8) C1 0.0776(14) 0.1058(19) 0.0253(8) 0.0154(10) 0.0039(8) -0.0297(13) C2 0.092(2) 0.093(2) 0.0498(14) 0.0085(14) -0.0386(15) -0.0444(18) N3 0.0199(7) 0.0330(8) 0.0441(11) 0.0100(7) 0.0067(7) -0.0001(5) C3 0.0231(9) 0.0474(13) 0.118(2) 0.0201(14) 0.0110(11) 0.0065(9) C4 0.0336(9) 0.0438(10) 0.0320(9) 0.0054(7) 0.0077(7) -0.0082(8) N4 0.0272(7) 0.0250(7) 0.0485(10) -0.0027(6) 0.0067(7) 0.0042(5) C5 0.0366(8) 0.0509(10) 0.0559(10) 0.0202(8) 0.0066(7) 0.0186(7) C6 0.0510(14) 0.0386(12) 0.124(3) -0.0382(15) 0.0068(15) 0.0025(10) B1 0.0284(7) 0.0209(6) 0.0352(8) -0.0001(5) 0.0046(6) 0.0036(5) B2 0.0322(7) 0.0245(7) 0.0295(7) -0.0032(5) 0.0014(6) -0.0020(6) B3 0.0273(7) 0.0203(6) 0.0429(8) -0.0017(6) 0.0115(6) -0.0012(5) B4 0.0345(8) 0.0256(7) 0.0316(7) 0.0041(6) 0.0143(6) 0.0059(6) B5 0.0355(8) 0.0220(6) 0.0260(7) -0.0026(5) 0.0051(6) 0.0025(6) B6 0.0377(8) 0.0204(6) 0.0272(7) 0.0008(5) 0.0035(6) -0.0022(6) C7 0.0289(6) 0.0214(6) 0.0332(6) -0.0060(5) 0.0098(5) 0.0009(5) C8 0.0339(7) 0.0216(6) 0.0349(7) 0.0039(5) 0.0109(5) 0.0083(5) B9 0.0345(8) 0.0337(8) 0.0268(7) 0.0007(6) 0.0035(6) 0.0076(6) B10 0.0325(8) 0.0286(7) 0.0315(7) -0.0057(6) 0.0051(6) -0.0064(6) B11 0.0323(7) 0.0288(7) 0.0272(7) -0.0043(6) 0.0096(6) -0.0063(6) _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 N3A 1.564(8) . ? P1 N4 1.5920(15) . ? P1 N2A 1.616(6) . ? P1 N1 1.6154(12) . ? P1 N3 1.6291(17) . ? P1 N2 1.6360(16) . ? P1 N4A 1.723(6) . ? N1 H13 0.86(2) . ? N1 H14 0.84(2) . ? N2 C2 1.467(3) . ? N2 C1 1.475(3) . ? N2 H25A 1.4875 . ? C1 N2A 1.402(6) . ? C1 H23 0.9800 . ? C1 H24 0.9800 . ? C1 H25 0.9800 . ? C1 H23A 0.9600 . ? C1 H24A 0.9600 . ? C1 H25A 0.9600 . ? C2 H26 0.9799 . ? C2 H27 0.9800 . ? C2 H28 0.9801 . ? C2 H30A 0.8356 . ? N2A C2A 1.452(12) . ? N2A H24 1.5154 . ? C2A H26A 0.9799 . ? C2A H27A 0.9801 . ? C2A H28A 0.9800 . ? C2A H38 1.2193 . ? N3 C4 1.461(2) . ? N3 C3 1.462(3) . ? N3 H33A 1.4714 . ? C3 H29 0.9800 . ? C3 H30 0.9800 . ? C3 H31 0.9800 . ? C3 H34A 1.0975 . ? C4 H32 0.9800 . ? C4 H33 0.9800 . ? C4 H34 0.9799 . ? C4 H32A 1.3590 . ? C4 H33A 0.7850 . ? N3A C4A 1.469(13) . ? N3A C3A 1.486(13) . ? C3A H26 1.1953 . ? C3A H29 1.4355 . ? C3A H29A 0.9801 . ? C3A H30A 0.9801 . ? C3A H31A 0.9801 . ? C4A H31 1.5310 . ? C4A H33 1.3737 . ? C4A H34 1.4651 . ? C4A H32A 0.9799 . ? C4A H33A 0.9800 . ? C4A H34A 0.9800 . ? N4 C6 1.466(3) . ? N4 C5 1.494(3) . ? C5 N4A 1.397(6) . ? C5 H37A 0.9600 . ? C5 H36A 0.9600 . ? C5 H35A 0.9600 . ? C5 H35 0.9800 . ? C5 H36 0.9800 . ? C5 H37 0.9801 . ? C6 H26A 0.9746 . ? C6 H38 0.9801 . ? C6 H39 0.9800 . ? C6 H40 0.9800 . ? C6 H39A 1.4985 . ? N4A C6A 1.483(12) . ? C6A H32 1.4257 . ? C6A H40 1.2728 . ? C6A H38A 0.9800 . ? C6A H39A 0.9800 . ? C6A H40A 0.9800 . ? B1 B2 1.761(2) . ? B1 B4 1.767(2) . ? B1 B3 1.773(2) . ? B1 B5 1.793(2) . ? B1 B6 1.799(2) . ? B1 H1 1.101(18) . ? B2 C7 1.716(2) . ? B2 B3 1.754(2) . ? B2 B6 1.758(2) . ? B2 B11 1.803(2) . ? B2 H2 1.086(19) . ? B3 C7 1.712(2) . ? B3 C8 1.718(2) . ? B3 B4 1.762(2) . ? B3 H3 1.090(19) . ? B4 C8 1.719(2) . ? B4 B5 1.756(2) . ? B4 B9 1.795(2) . ? B4 H4 1.079(19) . ? B5 B9 1.765(2) . ? B5 B10 1.783(2) . ? B5 B6 1.823(2) . ? B5 H5 1.108(18) . ? B6 B11 1.779(2) . ? B6 B10 1.779(2) . ? B6 H6 1.105(18) . ? C7 C8 1.555(2) . ? C7 B11 1.614(2) . ? C7 H7 0.956(19) . ? C8 B9 1.607(2) . ? C8 H8 0.96(2) . ? B9 B10 1.831(2) . ? B9 H9 1.09(2) . ? B10 B11 1.853(2) . ? B10 H10 1.101(19) . ? B10 H12 1.13(3) . ? B11 H11 1.092(19) . ? B11 H12 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3A P1 N4 121.5(3) . . ? N3A P1 N2A 114.2(4) . . ? N4 P1 N2A 78.9(2) . . ? N3A P1 N1 118.0(3) . . ? N4 P1 N1 109.54(8) . . ? N2A P1 N1 107.8(2) . . ? N3A P1 N3 20.3(3) . . ? N4 P1 N3 113.43(8) . . ? N2A P1 N3 133.4(2) . . ? N1 P1 N3 109.07(8) . . ? N3A P1 N2 85.5(3) . . ? N4 P1 N2 110.97(10) . . ? N2A P1 N2 34.8(2) . . ? N1 P1 N2 107.88(8) . . ? N3 P1 N2 105.75(11) . . ? N3A P1 N4A 101.3(4) . . ? N4 P1 N4A 29.3(2) . . ? N2A P1 N4A 107.0(3) . . ? N1 P1 N4A 107.7(2) . . ? N3 P1 N4A 87.7(2) . . ? N2 P1 N4A 134.9(2) . . ? P1 N1 H13 119.7(13) . . ? P1 N1 H14 119.8(13) . . ? H13 N1 H14 117.1(18) . . ? C2 N2 C1 115.50(18) . . ? C2 N2 P1 123.99(16) . . ? C1 N2 P1 118.82(14) . . ? C2 N2 H25A 94.3 . . ? C1 N2 H25A 37.8 . . ? P1 N2 H25A 138.3 . . ? N2A C1 N2 39.5(3) . . ? N2A C1 H23 98.2 . . ? N2 C1 H23 109.7 . . ? N2A C1 H24 76.8 . . ? N2 C1 H24 107.6 . . ? H23 C1 H24 109.5 . . ? N2A C1 H25 146.7 . . ? N2 C1 H25 111.2 . . ? H23 C1 H25 109.5 . . ? H24 C1 H25 109.5 . . ? N2A C1 H23A 107.8 . . ? N2 C1 H23A 124.6 . . ? H23 C1 H23A 120.4 . . ? H24 C1 H23A 35.5 . . ? H25 C1 H23A 74.1 . . ? N2A C1 H24A 109.4 . . ? N2 C1 H24A 122.4 . . ? H23 C1 H24A 13.0 . . ? H24 C1 H24A 105.1 . . ? H25 C1 H24A 100.5 . . ? H23A C1 H24A 109.5 . . ? N2A C1 H25A 111.2 . . ? N2 C1 H25A 71.8 . . ? H23 C1 H25A 109.3 . . ? H24 C1 H25A 138.7 . . ? H25 C1 H25A 42.6 . . ? H23A C1 H25A 109.5 . . ? H24A C1 H25A 109.5 . . ? C1 N2A C2A 109.5(6) . . ? C1 N2A P1 125.0(4) . . ? C2A N2A P1 124.7(6) . . ? C1 N2A H24 39.0 . . ? C2A N2A H24 74.2 . . ? P1 N2A H24 159.9 . . ? N2A C2A H26A 109.5 . . ? N2A C2A H27A 109.4 . . ? H26A C2A H27A 109.5 . . ? N2A C2A H28A 109.5 . . ? H26A C2A H28A 109.5 . . ? H27A C2A H28A 109.5 . . ? N2A C2A H38 102.6 . . ? H26A C2A H38 42.1 . . ? H27A C2A H38 73.4 . . ? H28A C2A H38 143.9 . . ? C4 N3 C3 113.43(17) . . ? C4 N3 P1 122.21(14) . . ? C3 N3 P1 122.66(15) . . ? P1 N3 H33A 122.1 . . ? H32A C4 H33A 92.6 . . ? C4A N3A C3A 113.6(8) . . ? C4A N3A P1 123.5(7) . . ? C3A N3A P1 119.5(7) . . ? N3A C3A H26 93.1 . . ? N3A C3A H29 74.5 . . ? N3A C3A H29A 109.6 . . ? N3A C3A H30A 109.4 . . ? H29A C3A H30A 109.5 . . ? N3A C3A H31A 109.4 . . ? H29A C3A H31A 109.5 . . ? H30A C3A H31A 109.5 . . ? N3A C4A H31 93.8 . . ? N3A C4A H33 127.6 . . ? N3A C4A H34 103.6 . . ? N3A C4A H32A 109.4 . . ? N3A C4A H33A 109.6 . . ? H32A C4A H33A 109.5 . . ? N3A C4A H34A 109.3 . . ? H32A C4A H34A 109.5 . . ? H33A C4A H34A 109.5 . . ? C6 N4 C5 115.16(18) . . ? C6 N4 P1 120.21(16) . . ? C5 N4 P1 123.11(13) . . ? N4A C5 N4 33.9(3) . . ? N4A C5 H37A 110.0 . . ? N4 C5 H37A 126.2 . . ? N4A C5 H36A 109.8 . . ? N4 C5 H36A 119.5 . . ? H37A C5 H36A 109.5 . . ? N4A C5 H35A 108.6 . . ? N4 C5 H35A 74.8 . . ? H37A C5 H35A 109.5 . . ? H36A C5 H35A 109.5 . . ? N4A C5 H35 100.2 . . ? N4 C5 H35 109.4 . . ? H37A C5 H35 117.6 . . ? H36A C5 H35 10.4 . . ? H35A C5 H35 110.3 . . ? N4A C5 H36 83.5 . . ? N4 C5 H36 109.9 . . ? H37A C5 H36 30.8 . . ? H36A C5 H36 106.0 . . ? H35A C5 H36 135.2 . . ? H35 C5 H36 109.5 . . ? N4A C5 H37 140.4 . . ? N4 C5 H37 109.1 . . ? H37A C5 H37 79.0 . . ? H36A C5 H37 102.4 . . ? H35A C5 H37 36.7 . . ? H35 C5 H37 109.5 . . ? H36 C5 H37 109.5 . . ? H26A C6 H38 49.7 . . ? H26A C6 H39 64.9 . . ? H26A C6 H40 145.0 . . ? H26A C6 H39A 160.5 . . ? C5 N4A C6A 112.9(6) . . ? C5 N4A P1 120.5(4) . . ? C6A N4A P1 124.1(6) . . ? N4A C6A H32 75.6 . . ? N4A C6A H40 97.6 . . ? N4A C6A H38A 109.4 . . ? N4A C6A H39A 109.4 . . ? H38A C6A H39A 109.5 . . ? N4A C6A H40A 109.7 . . ? H38A C6A H40A 109.5 . . ? H39A C6A H40A 109.5 . . ? B2 B1 B4 108.02(11) . . ? B2 B1 B3 59.54(9) . . ? B4 B1 B3 59.71(9) . . ? B2 B1 B5 108.04(11) . . ? B4 B1 B5 59.11(9) . . ? B3 B1 B5 106.34(11) . . ? B2 B1 B6 59.16(9) . . ? B4 B1 B6 107.84(11) . . ? B3 B1 B6 106.16(10) . . ? B5 B1 B6 60.98(9) . . ? B2 B1 H1 122.8(10) . . ? B4 B1 H1 119.8(10) . . ? B3 B1 H1 121.5(10) . . ? B5 B1 H1 122.2(10) . . ? B6 B1 H1 124.3(9) . . ? C7 B2 B3 59.11(9) . . ? C7 B2 B6 100.94(11) . . ? B3 B2 B6 108.82(11) . . ? C7 B2 B1 103.96(11) . . ? B3 B2 B1 60.58(9) . . ? B6 B2 B1 61.52(9) . . ? C7 B2 B11 54.53(9) . . ? B3 B2 B11 106.20(12) . . ? B6 B2 B11 59.91(9) . . ? B1 B2 B11 108.71(11) . . ? C7 B2 H2 121.9(10) . . ? B3 B2 H2 118.8(10) . . ? B6 B2 H2 127.2(10) . . ? B1 B2 H2 125.5(10) . . ? B11 B2 H2 121.0(10) . . ? C7 B3 C8 53.90(8) . . ? C7 B3 B2 59.33(9) . . ? C8 B3 B2 102.61(11) . . ? C7 B3 B4 103.33(11) . . ? C8 B3 B4 59.19(9) . . ? B2 B3 B4 108.50(11) . . ? C7 B3 B1 103.59(10) . . ? C8 B3 B1 103.01(11) . . ? B2 B3 B1 59.88(9) . . ? B4 B3 B1 59.97(9) . . ? C7 B3 H3 119.9(10) . . ? C8 B3 H3 120.5(10) . . ? B2 B3 H3 123.8(10) . . ? B4 B3 H3 123.5(10) . . ? B1 B3 H3 130.6(10) . . ? C8 B4 B5 100.29(11) . . ? C8 B4 B3 59.13(9) . . ? B5 B4 B3 108.44(11) . . ? C8 B4 B1 103.22(11) . . ? B5 B4 B1 61.18(9) . . ? B3 B4 B1 60.31(9) . . ? C8 B4 B9 54.38(9) . . ? B5 B4 B9 59.58(9) . . ? B3 B4 B9 106.10(11) . . ? B1 B4 B9 107.99(11) . . ? C8 B4 H4 120.6(10) . . ? B5 B4 H4 129.5(10) . . ? B3 B4 H4 117.3(10) . . ? B1 B4 H4 126.7(10) . . ? B9 B4 H4 121.4(10) . . ? B4 B5 B9 61.32(9) . . ? B4 B5 B10 112.57(11) . . ? B9 B5 B10 62.17(9) . . ? B4 B5 B1 59.71(9) . . ? B9 B5 B1 108.20(11) . . ? B10 B5 B1 109.84(10) . . ? B4 B5 B6 107.29(11) . . ? B9 B5 B6 106.41(11) . . ? B10 B5 B6 59.13(10) . . ? B1 B5 B6 59.69(9) . . ? B4 B5 H5 121.9(10) . . ? B9 B5 H5 122.5(9) . . ? B10 B5 H5 117.9(9) . . ? B1 B5 H5 121.7(9) . . ? B6 B5 H5 122.0(9) . . ? B2 B6 B11 61.32(9) . . ? B2 B6 B10 112.80(11) . . ? B11 B6 B10 62.77(9) . . ? B2 B6 B1 59.32(9) . . ? B11 B6 B1 108.10(10) . . ? B10 B6 B1 109.69(11) . . ? B2 B6 B5 106.86(10) . . ? B11 B6 B5 106.96(11) . . ? B10 B6 B5 59.31(9) . . ? B1 B6 B5 59.33(9) . . ? B2 B6 H6 121.4(9) . . ? B11 B6 H6 122.7(9) . . ? B10 B6 H6 118.7(9) . . ? B1 B6 H6 121.0(9) . . ? B5 B6 H6 122.1(10) . . ? C8 C7 B11 112.63(11) . . ? C8 C7 B3 63.24(10) . . ? B11 C7 B3 117.57(11) . . ? C8 C7 B2 111.82(11) . . ? B11 C7 B2 65.49(9) . . ? B3 C7 B2 61.56(9) . . ? C8 C7 H7 115.2(11) . . ? B11 C7 H7 121.8(11) . . ? B3 C7 H7 112.4(11) . . ? B2 C7 H7 120.6(11) . . ? C7 C8 B9 114.39(11) . . ? C7 C8 B3 62.86(10) . . ? B9 C8 B3 117.47(11) . . ? C7 C8 B4 112.61(11) . . ? B9 C8 B4 65.22(10) . . ? B3 C8 B4 61.68(9) . . ? C7 C8 H8 114.3(12) . . ? B9 C8 H8 123.1(12) . . ? B3 C8 H8 109.8(11) . . ? B4 C8 H8 118.1(12) . . ? C8 B9 B5 104.51(12) . . ? C8 B9 B4 60.40(9) . . ? B5 B9 B4 59.11(9) . . ? C8 B9 B10 105.90(11) . . ? B5 B9 B10 59.40(9) . . ? B4 B9 B10 108.50(11) . . ? C8 B9 H9 121.3(11) . . ? B5 B9 H9 124.9(11) . . ? B4 B9 H9 118.5(10) . . ? B10 B9 H9 124.8(11) . . ? B6 B10 B5 61.56(9) . . ? B6 B10 B9 105.42(11) . . ? B5 B10 B9 58.43(9) . . ? B6 B10 B11 58.60(9) . . ? B5 B10 B11 105.51(11) . . ? B9 B10 B11 100.85(11) . . ? B6 B10 H10 118.8(10) . . ? B5 B10 H10 119.0(10) . . ? B9 B10 H10 126.7(10) . . ? B11 B10 H10 126.4(10) . . ? B6 B10 H12 112.0(13) . . ? B5 B10 H12 123.9(13) . . ? B9 B10 H12 73.2(13) . . ? B11 B10 H12 55.4(13) . . ? H10 B10 H12 111.9(16) . . ? C7 B11 B6 104.21(11) . . ? C7 B11 B2 59.98(9) . . ? B6 B11 B2 58.76(9) . . ? C7 B11 B10 106.02(11) . . ? B6 B11 B10 58.63(9) . . ? B2 B11 B10 107.35(11) . . ? C7 B11 H11 123.5(10) . . ? B6 B11 H11 122.2(10) . . ? B2 B11 H11 118.1(10) . . ? B10 B11 H11 124.3(10) . . ? C7 B11 H12 88.4(10) . . ? B6 B11 H12 94.8(10) . . ? B2 B11 H12 126.5(9) . . ? B10 B11 H12 37.6(10) . . ? H11 B11 H12 115.4(14) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.392 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.043 #========================================================END data_(6) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '7,8-dicarba-nido-undecaborane borenium salt' _chemical_melting_point ? _chemical_formula_moiety 'C24 H74 B2 N16 O P4 2+,(C2 B9 H12 1-)2' _chemical_formula_sum 'C28 H98 B20 N16 O P4' _chemical_formula_weight 1015.30 _ccdc_compound_id '6' _ccdc_biological_activity '?' _ccdc_polymorph '?' _ccdc_disorder ; ? ; _ccdc_comments '?' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.105(3) _cell_length_b 16.529(3) _cell_length_c 25.563(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5960(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.168 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Four sets of \w scans (each scan 0.3\% in \w, exposure time 10 s), each set at different \f and/or 2\q angles, nominally covered over a hemisphere of reciprocal space. The first 50 scans were repeated at the end of data collection, revealing no significant crystal decay. Crystal to detector distance 4.51 cm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 44070 _diffrn_reflns_av_R_equivalents 0.1603 _diffrn_reflns_av_sigmaI/netI 0.3049 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 30.48 _reflns_number_total 16579 _reflns_number_gt 5792 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0408P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(9) _refine_ls_number_reflns 16579 _refine_ls_number_parameters 737 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2453 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1383 _refine_ls_wR_factor_gt 0.0949 _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_restrained_S_all 0.893 _refine_ls_shift/su_max 0.071 _refine_ls_shift/su_mean 0.003 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O -0.94607(18) -1.50176(16) -0.39933(10) 0.0307(7) Uani 1 1 d . . . P1 P -1.19747(8) -1.43528(7) -0.34746(4) 0.0292(3) Uani 1 1 d . . . B1'' B -0.9451(4) -1.1071(4) -0.4584(3) 0.0561(17) Uani 1 1 d . . . H1'' H -0.916(3) -1.142(3) -0.4845(17) 0.067 Uiso 1 1 d . . . B1' B -0.4548(5) -1.1611(4) -0.1980(3) 0.0604(19) Uani 1 1 d . . . H1' H -0.421(3) -1.121(3) -0.1772(17) 0.073 Uiso 1 1 d . . . N1 N -1.1073(2) -1.4593(2) -0.37883(12) 0.0299(8) Uani 1 1 d . . . B1 B -1.0107(4) -1.4658(3) -0.36656(18) 0.0280(12) Uani 1 1 d . . . P2 P -0.84112(8) -1.64949(7) -0.46158(4) 0.0317(3) Uani 1 1 d . . . B2'' B -1.0006(4) -1.0161(4) -0.4759(2) 0.0525(17) Uani 1 1 d . . . H2'' H -1.009(3) -0.986(3) -0.5116(15) 0.063 Uiso 1 1 d . . . B2' B -0.4149(6) -1.1861(6) -0.2589(3) 0.088(3) Uani 1 1 d . . . H2' H -0.346(4) -1.165(3) -0.282(2) 0.106 Uiso 1 1 d . . . N2 N -0.9058(2) -1.5785(2) -0.47953(11) 0.0308(9) Uani 1 1 d . . . B2 B -0.9564(3) -1.5189(3) -0.4533(2) 0.0313(12) Uani 1 1 d . . . P3 P -0.86400(8) -1.41536(7) -0.29639(4) 0.0326(3) Uani 1 1 d . . . B3'' B -0.9017(4) -1.0140(4) -0.4358(3) 0.0524(17) Uani 1 1 d . . . H3'' H -0.837(3) -0.983(2) -0.4465(15) 0.063 Uiso 1 1 d . . . B3' B -0.5163(6) -1.1260(5) -0.2518(3) 0.087(2) Uani 1 1 d . . . H3' H -0.518(4) -1.052(3) -0.2721(18) 0.104 Uiso 1 1 d . . . N3 N -0.9703(3) -1.4361(2) -0.31748(14) 0.0330(10) Uani 1 1 d . . . H3 H -1.012(3) -1.431(2) -0.2969(13) 0.032(14) Uiso 1 1 d . . . P4 P -1.03359(8) -1.44624(7) -0.54230(4) 0.0336(3) Uani 1 1 d . . . B4'' B -0.9059(4) -1.0975(4) -0.3929(2) 0.0514(17) Uani 1 1 d . . . H4'' H -0.849(3) -1.128(3) -0.3771(16) 0.062 Uiso 1 1 d . . . B4' B -0.5813(5) -1.1618(5) -0.2022(3) 0.073(2) Uani 1 1 d . . . H4' H -0.620(4) -1.130(3) -0.1811(18) 0.088 Uiso 1 1 d . . . N4 N -1.0235(2) -1.4664(2) -0.48074(13) 0.0309(9) Uani 1 1 d . . . H4 H -1.071(3) -1.449(2) -0.4610(14) 0.030(12) Uiso 1 1 d . . . B5 B -1.0138(4) -1.1519(4) -0.4070(3) 0.065(2) Uani 1 1 d . . . H5 H -1.022(3) -1.214(3) -0.4067(17) 0.079 Uiso 1 1 d . . . B5' B -0.5181(6) -1.2452(6) -0.1725(3) 0.095(3) Uani 1 1 d . . . H5' H -0.519(4) -1.258(3) -0.136(2) 0.114 Uiso 1 1 d . . . B6 B -1.0702(4) -1.1004(4) -0.4596(3) 0.0606(19) Uani 1 1 d . . . H6 H -1.116(3) -1.130(3) -0.4852(17) 0.073 Uiso 1 1 d . . . B6' B -0.4167(6) -1.2567(5) -0.2057(4) 0.097(3) Uani 1 1 d . . . H6' H -0.347(4) -1.281(3) -0.196(2) 0.116 Uiso 1 1 d . . . C7'' C -1.0943(4) -1.0094(3) -0.4321(2) 0.0621(16) Uani 1 1 d . . . H7'' H -1.152(3) -0.981(3) -0.4484(16) 0.074 Uiso 1 1 d . . . C7' C -0.4603(9) -1.2736(4) -0.2700(3) 0.133(4) Uani 1 1 d . . . H7' H -0.437(5) -1.309(4) -0.304(3) 0.15(3) Uiso 1 1 d . . . C8'' C -1.0009(4) -0.9615(3) -0.4179(2) 0.0560(15) Uani 1 1 d . . . H8'' H -1.008(3) -0.895(3) -0.4257(16) 0.067(14) Uiso 1 1 d . . . C8' C -0.5179(5) -1.2096(6) -0.2901(3) 0.115(3) Uani 1 1 d . . . H8' H -0.488(5) -1.188(4) -0.332(2) 0.13(2) Uiso 1 1 d . . . B9 B -0.9422(5) -1.0019(4) -0.3704(2) 0.0521(17) Uani 1 1 d . . . H9 H -0.894(3) -0.964(2) -0.3455(15) 0.056(13) Uiso 1 1 d . . . B9' B -0.6131(5) -1.1920(4) -0.2648(2) 0.0521(17) Uani 1 1 d . . . H9' H -0.677(3) -1.168(3) -0.2883(16) 0.073(15) Uiso 1 1 d . . . B10 B -1.0067(5) -1.0897(4) -0.3512(3) 0.0601(18) Uani 1 1 d . . . H10 H -1.005(4) -1.113(3) -0.3109(19) 0.103(19) Uiso 1 1 d . . . H12 H -1.073(6) -1.038(5) -0.359(3) 0.20(3) Uiso 1 1 d . . . B10' B -0.6185(6) -1.2596(6) -0.2092(3) 0.093(3) Uani 1 1 d . . . H10' H -0.670(5) -1.281(4) -0.198(2) 0.13(3) Uiso 1 1 d . . . H12' H -0.599(5) -1.285(4) -0.251(3) 0.15(3) Uiso 1 1 d . . . B11 B -1.1072(4) -1.0869(3) -0.3930(3) 0.0526(17) Uani 1 1 d . . . H11 H -1.186(3) -1.112(2) -0.3841(13) 0.040(11) Uiso 1 1 d . . . B11' B -0.5025(5) -1.3204(4) -0.2277(3) 0.070(2) Uani 1 1 d . . . H11' H -0.501(4) -1.374(3) -0.213(2) 0.10(2) Uiso 1 1 d . . . C11 C -1.2820(3) -1.5280(3) -0.42210(18) 0.0603(15) Uani 1 1 d . . . H11A H -1.3108 -1.5080 -0.4536 0.090 Uiso 1 1 calc R . . H11B H -1.3143 -1.5761 -0.4109 0.090 Uiso 1 1 calc R . . H11C H -1.2166 -1.5402 -0.4286 0.090 Uiso 1 1 calc R . . N11 N -1.2888(2) -1.4660(2) -0.38101(13) 0.0391(10) Uani 1 1 d . . . C12 C -1.3873(3) -1.4477(3) -0.36674(18) 0.0549(14) Uani 1 1 d . . . H12A H -1.4192 -1.4240 -0.3961 0.082 Uiso 1 1 calc R . . H12B H -1.3881 -1.4105 -0.3379 0.082 Uiso 1 1 calc R . . H12C H -1.4191 -1.4967 -0.3568 0.082 Uiso 1 1 calc R . . N12 N -1.1915(2) -1.4711(2) -0.28691(12) 0.0357(9) Uani 1 1 d . . . C13 C -1.1586(3) -1.5546(3) -0.27961(17) 0.0456(12) Uani 1 1 d . . . H13A H -1.1344 -1.5610 -0.2447 0.068 Uiso 1 1 calc R . . H13B H -1.1093 -1.5662 -0.3044 0.068 Uiso 1 1 calc R . . H13C H -1.2105 -1.5912 -0.2849 0.068 Uiso 1 1 calc R . . N13 N -1.2212(2) -1.3386(2) -0.33742(13) 0.0337(9) Uani 1 1 d . . . C14 C -1.2661(3) -1.4516(3) -0.24845(16) 0.0576(15) Uani 1 1 d . . . H14A H -1.2412 -1.4574 -0.2137 0.086 Uiso 1 1 calc R . . H14A H -1.3187 -1.4877 -0.2531 0.086 Uiso 1 1 calc R . . H14B H -1.2869 -1.3968 -0.2536 0.086 Uiso 1 1 calc R . . C15 C -1.1624(3) -1.2927(3) -0.30020(18) 0.0537(14) Uani 1 1 d . . . H15A H -1.1955 -1.2448 -0.2896 0.081 Uiso 1 1 calc R . . H15B H -1.1037 -1.2779 -0.3167 0.081 Uiso 1 1 calc R . . H15C H -1.1494 -1.3256 -0.2701 0.081 Uiso 1 1 calc R . . C16 C -1.2517(3) -1.2881(3) -0.38148(17) 0.0460(13) Uani 1 1 d . . . H16A H -1.2955 -1.2479 -0.3693 0.069 Uiso 1 1 calc R . . H16B H -1.2821 -1.3213 -0.4073 0.069 Uiso 1 1 calc R . . H16C H -1.1975 -1.2620 -0.3967 0.069 Uiso 1 1 calc R . . C21 C -0.9037(4) -1.7808(3) -0.5110(2) 0.0632(16) Uani 1 1 d . . . H21A H -0.8806 -1.8276 -0.5292 0.095 Uiso 1 1 calc R . . H21B H -0.9557 -1.7577 -0.5300 0.095 Uiso 1 1 calc R . . H21C H -0.9247 -1.7963 -0.4767 0.095 Uiso 1 1 calc R . . N21 N -0.8281(2) -1.7215(2) -0.50643(13) 0.0358(9) Uani 1 1 d . . . C22 C -0.7890(4) -1.6974(3) -0.55703(16) 0.0556(14) Uani 1 1 d . . . H22A H -0.7656 -1.7443 -0.5750 0.083 Uiso 1 1 calc R . . H22B H -0.7381 -1.6597 -0.5517 0.083 Uiso 1 1 calc R . . H22A H -0.8378 -1.6723 -0.5776 0.083 Uiso 1 1 calc R . . N22 N -0.7313(2) -1.6221(2) -0.45156(13) 0.0357(9) Uani 1 1 d . . . C23 C -0.7120(3) -1.5443(3) -0.42534(16) 0.0426(12) Uani 1 1 d . . . H23A H -0.6802 -1.5541 -0.3927 0.064 Uiso 1 1 calc R . . H23B H -0.7707 -1.5168 -0.4189 0.064 Uiso 1 1 calc R . . H23C H -0.6725 -1.5115 -0.4474 0.064 Uiso 1 1 calc R . . N23 N -0.8831(3) -1.6950(2) -0.40875(13) 0.0391(10) Uani 1 1 d . . . C24 C -0.6474(3) -1.6730(3) -0.45800(19) 0.0529(13) Uani 1 1 d . . . H24A H -0.6033 -1.6468 -0.4810 0.079 Uiso 1 1 calc R . . H24B H -0.6657 -1.7242 -0.4727 0.079 Uiso 1 1 calc R . . H24C H -0.6181 -1.6817 -0.4246 0.079 Uiso 1 1 calc R . . C25 C -0.9835(3) -1.6978(3) -0.39602(19) 0.0533(14) Uani 1 1 d . . . H25A H -0.9922 -1.6839 -0.3599 0.080 Uiso 1 1 calc R . . H25B H -1.0073 -1.7513 -0.4022 0.080 Uiso 1 1 calc R . . H25C H -1.0172 -1.6599 -0.4176 0.080 Uiso 1 1 calc R . . C26 C -0.8263(4) -1.7551(3) -0.38094(18) 0.0609(16) Uani 1 1 d . . . H26A H -0.8370 -1.7500 -0.3440 0.091 Uiso 1 1 calc R . . H26B H -0.7604 -1.7464 -0.3884 0.091 Uiso 1 1 calc R . . H26C H -0.8442 -1.8084 -0.3922 0.091 Uiso 1 1 calc R . . C31 C -0.7007(3) -1.3798(3) -0.34480(19) 0.0583(14) Uani 1 1 d . . . H31A H -0.6759 -1.3963 -0.3781 0.087 Uiso 1 1 calc R . . H31B H -0.6786 -1.4162 -0.3182 0.087 Uiso 1 1 calc R . . H31C H -0.6796 -1.3259 -0.3370 0.087 Uiso 1 1 calc R . . N31 N -0.8052(2) -1.3815(2) -0.34648(13) 0.0371(9) Uani 1 1 d . . . C32 C -0.8448(4) -1.3306(3) -0.38733(17) 0.0580(14) Uani 1 1 d . . . H32A H -0.8268 -1.3514 -0.4209 0.087 Uiso 1 1 calc R . . H32B H -0.8210 -1.2764 -0.3835 0.087 Uiso 1 1 calc R . . H32C H -0.9127 -1.3301 -0.3845 0.087 Uiso 1 1 calc R . . N32 N -0.8143(2) -1.4937(2) -0.27047(12) 0.0367(9) Uani 1 1 d . . . C33 C -0.8324(3) -1.5749(2) -0.28976(16) 0.0452(12) Uani 1 1 d . . . H33A H -0.8600 -1.6069 -0.2624 0.068 Uiso 1 1 calc R . . H33B H -0.7739 -1.5991 -0.3008 0.068 Uiso 1 1 calc R . . H33C H -0.8754 -1.5723 -0.3188 0.068 Uiso 1 1 calc R . . N33 N -0.8667(3) -1.3480(2) -0.24957(13) 0.0377(9) Uani 1 1 d . . . C34 C -0.7390(3) -1.4894(3) -0.23053(17) 0.0592(15) Uani 1 1 d . . . H34A H -0.6812 -1.5108 -0.2447 0.089 Uiso 1 1 calc R . . H34B H -0.7574 -1.5206 -0.2005 0.089 Uiso 1 1 calc R . . H34C H -0.7295 -1.4341 -0.2204 0.089 Uiso 1 1 calc R . . C35 C -0.8712(4) -1.2616(3) -0.26189(19) 0.0554(15) Uani 1 1 d . . . H35A H -0.8450 -1.2310 -0.2334 0.083 Uiso 1 1 calc R . . H35B H -0.9361 -1.2460 -0.2672 0.083 Uiso 1 1 calc R . . H35C H -0.8355 -1.2510 -0.2931 0.083 Uiso 1 1 calc R . . C36 C -0.9094(4) -1.3671(3) -0.19873(19) 0.0671(16) Uani 1 1 d . . . H36A H -0.8722 -1.3433 -0.1713 0.101 Uiso 1 1 calc R . . H36B H -0.9113 -1.4247 -0.1941 0.101 Uiso 1 1 calc R . . H36C H -0.9727 -1.3459 -0.1975 0.101 Uiso 1 1 calc R . . C41 C -0.8515(4) -1.3989(3) -0.5402(2) 0.0751(17) Uani 1 1 d . . . H41A H -0.8191 -1.3639 -0.5643 0.113 Uiso 1 1 calc R . . H41B H -0.8077 -1.4379 -0.5264 0.113 Uiso 1 1 calc R . . H41C H -0.8774 -1.3674 -0.5121 0.113 Uiso 1 1 calc R . . N41 N -0.9277(2) -1.4406(2) -0.56734(13) 0.0426(10) Uani 1 1 d . . . C42 C -0.8971(4) -1.4878(4) -0.6124(2) 0.0766(18) Uani 1 1 d . . . H42A H -0.8806 -1.4519 -0.6405 0.115 Uiso 1 1 calc R . . H42B H -0.9477 -1.5228 -0.6234 0.115 Uiso 1 1 calc R . . H42C H -0.8429 -1.5197 -0.6030 0.115 Uiso 1 1 calc R . . N42 N -1.0857(3) -1.3594(2) -0.54956(15) 0.0421(10) Uani 1 1 d . . . C43 C -1.0397(5) -1.2859(3) -0.5625(3) 0.113(3) Uani 1 1 d . . . H43A H -1.0771 -1.2568 -0.5875 0.170 Uiso 1 1 calc R . . H43B H -0.9785 -1.2974 -0.5771 0.170 Uiso 1 1 calc R . . H43C H -1.0322 -1.2538 -0.5315 0.170 Uiso 1 1 calc R . . N43 N -1.0995(3) -1.5114(2) -0.57170(13) 0.0396(10) Uani 1 1 d . . . C44 C -1.1790(3) -1.3466(3) -0.5259(2) 0.0655(16) Uani 1 1 d . . . H44A H -1.2175 -1.3145 -0.5489 0.098 Uiso 1 1 calc R . . H44B H -1.1717 -1.3190 -0.4931 0.098 Uiso 1 1 calc R . . H44C H -1.2091 -1.3980 -0.5201 0.098 Uiso 1 1 calc R . . C45 C -1.1416(3) -1.4957(3) -0.62328(14) 0.0521(14) Uani 1 1 d . . . H45A H -1.2086 -1.5053 -0.6218 0.078 Uiso 1 1 calc R . . H45B H -1.1135 -1.5311 -0.6487 0.078 Uiso 1 1 calc R . . H45C H -1.1301 -1.4405 -0.6330 0.078 Uiso 1 1 calc R . . C46 C -1.1069(3) -1.5956(3) -0.55466(18) 0.0510(14) Uani 1 1 d . . . H46A H -1.1725 -1.6099 -0.5508 0.077 Uiso 1 1 calc R . . H46B H -1.0751 -1.6020 -0.5217 0.077 Uiso 1 1 calc R . . H46C H -1.0779 -1.6302 -0.5802 0.077 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 O1 0.0255(16) 0.0391(18) 0.0276(16) -0.0044(14) -0.0022(14) 0.0095(14) P1 0.0261(6) 0.0289(7) 0.0326(6) -0.0011(5) 0.0018(6) 0.0005(6) B1'' 0.036(4) 0.046(4) 0.087(5) -0.012(4) 0.004(4) 0.008(3) B1' 0.053(4) 0.063(5) 0.065(4) -0.021(4) -0.020(4) -0.004(4) N1 0.023(2) 0.036(2) 0.0306(19) -0.0027(16) 0.0000(17) 0.0027(17) B1 0.033(3) 0.022(3) 0.028(3) 0.000(2) 0.000(3) 0.004(2) P2 0.0309(7) 0.0299(7) 0.0344(6) -0.0022(6) 0.0027(6) 0.0025(6) B2'' 0.036(3) 0.049(4) 0.072(4) -0.001(3) 0.007(4) 0.006(3) B2' 0.059(5) 0.132(9) 0.073(6) -0.032(5) 0.012(4) -0.004(5) N2 0.0271(19) 0.035(2) 0.031(2) 0.0015(17) 0.0041(16) 0.0093(18) B2 0.021(3) 0.032(3) 0.041(3) -0.001(3) 0.000(3) 0.001(2) P3 0.0303(7) 0.0315(7) 0.0359(7) -0.0035(6) -0.0012(6) 0.0015(6) B3'' 0.032(3) 0.051(4) 0.074(5) 0.001(3) -0.004(3) -0.004(3) B3' 0.073(6) 0.087(6) 0.101(6) 0.016(5) -0.021(5) -0.015(5) N3 0.023(2) 0.041(2) 0.034(2) -0.010(2) 0.006(2) 0.003(2) P4 0.0305(7) 0.0394(7) 0.0310(6) 0.0007(6) 0.0003(6) 0.0082(6) B4'' 0.037(4) 0.049(4) 0.068(4) 0.012(3) -0.004(3) 0.003(3) B4' 0.045(4) 0.093(6) 0.081(5) -0.054(5) 0.001(4) 0.020(4) N4 0.027(2) 0.034(2) 0.031(2) -0.0017(17) 0.0000(19) 0.0081(19) B5 0.035(4) 0.036(4) 0.125(6) 0.007(4) 0.001(4) -0.006(3) B5' 0.067(5) 0.182(10) 0.037(4) 0.051(5) -0.008(4) -0.011(6) B6 0.031(3) 0.050(4) 0.100(5) -0.018(4) -0.007(4) 0.003(3) B6' 0.067(5) 0.088(6) 0.135(8) -0.031(6) -0.053(6) 0.025(5) C7'' 0.031(3) 0.050(4) 0.105(5) 0.016(3) -0.003(3) 0.003(3) C7' 0.258(12) 0.053(5) 0.088(6) 0.000(4) 0.057(7) 0.057(6) C8'' 0.045(3) 0.038(3) 0.085(4) 0.001(3) 0.008(3) -0.008(3) C8' 0.061(5) 0.233(10) 0.051(4) -0.009(6) 0.007(4) 0.056(6) B9 0.052(4) 0.045(4) 0.059(4) 0.006(3) -0.008(4) 0.000(3) B9' 0.051(4) 0.051(4) 0.054(4) 0.009(3) -0.012(4) 0.001(3) B10 0.043(4) 0.056(4) 0.081(5) 0.018(4) 0.012(4) 0.005(3) B10' 0.080(6) 0.134(8) 0.064(5) 0.029(5) -0.013(5) -0.068(6) B11 0.036(4) 0.035(4) 0.087(5) -0.005(3) 0.005(4) -0.006(3) B11' 0.077(5) 0.031(4) 0.103(6) 0.015(4) -0.036(5) 0.003(4) C11 0.046(3) 0.065(4) 0.070(3) -0.020(3) -0.011(3) -0.003(3) N11 0.027(2) 0.040(2) 0.050(2) -0.0050(19) -0.003(2) -0.0001(19) C12 0.030(3) 0.064(4) 0.071(4) 0.004(3) -0.001(3) 0.001(3) N12 0.032(2) 0.038(2) 0.037(2) 0.0099(17) 0.011(2) 0.0071(18) C13 0.041(3) 0.038(3) 0.057(3) 0.011(2) -0.003(3) 0.003(3) N13 0.035(2) 0.026(2) 0.040(2) -0.0017(18) 0.0040(19) 0.0041(18) C14 0.052(3) 0.078(4) 0.042(3) 0.019(3) 0.019(3) 0.017(3) C15 0.058(3) 0.037(3) 0.066(3) -0.021(3) -0.003(3) 0.009(3) C16 0.054(3) 0.034(3) 0.050(3) 0.009(2) 0.011(3) 0.008(3) C21 0.080(4) 0.043(3) 0.067(4) -0.014(3) 0.002(3) -0.015(3) N21 0.032(2) 0.033(2) 0.042(2) -0.0045(18) 0.006(2) -0.0014(18) C22 0.064(4) 0.053(3) 0.050(3) -0.017(3) 0.014(3) -0.006(3) N22 0.026(2) 0.032(2) 0.050(2) -0.0053(19) -0.0010(19) 0.0069(17) C23 0.035(3) 0.042(3) 0.052(3) -0.006(2) -0.009(2) -0.002(2) N23 0.041(2) 0.034(2) 0.042(2) 0.0110(18) 0.004(2) -0.0017(19) C24 0.037(3) 0.051(3) 0.071(3) -0.004(3) 0.002(3) 0.015(3) C25 0.055(4) 0.042(3) 0.064(3) 0.000(3) 0.021(3) 0.000(3) C26 0.081(4) 0.046(3) 0.056(3) 0.024(3) 0.000(3) 0.002(3) C31 0.044(3) 0.069(4) 0.062(3) -0.016(3) 0.013(3) -0.025(3) N31 0.033(2) 0.043(2) 0.035(2) -0.0001(19) 0.007(2) -0.0047(19) C32 0.074(4) 0.046(3) 0.054(3) 0.009(3) 0.006(3) 0.001(3) N32 0.037(2) 0.034(2) 0.039(2) -0.0001(18) -0.0082(19) 0.0012(19) C33 0.055(3) 0.033(3) 0.048(3) -0.003(2) -0.007(3) 0.011(2) N33 0.039(2) 0.037(2) 0.037(2) -0.0081(18) -0.0031(19) -0.003(2) C34 0.053(3) 0.060(4) 0.064(3) -0.001(3) -0.028(3) 0.009(3) C35 0.054(3) 0.032(3) 0.080(4) -0.015(3) -0.004(3) -0.003(3) C36 0.086(4) 0.069(4) 0.046(3) -0.018(3) 0.015(3) -0.003(3) C41 0.052(3) 0.103(5) 0.071(3) 0.017(4) 0.011(4) -0.032(3) N41 0.029(2) 0.062(3) 0.037(2) 0.002(2) 0.0015(19) 0.008(2) C42 0.055(4) 0.101(5) 0.074(4) -0.017(4) 0.023(3) 0.010(4) N42 0.039(2) 0.032(2) 0.055(3) 0.007(2) 0.007(2) 0.0050(19) C43 0.117(6) 0.054(4) 0.169(7) 0.038(4) 0.073(5) 0.038(4) N43 0.045(2) 0.043(3) 0.030(2) -0.0072(19) -0.0086(19) 0.001(2) C44 0.046(3) 0.052(3) 0.099(4) 0.010(3) 0.003(3) 0.013(3) C45 0.057(3) 0.071(3) 0.028(2) -0.005(3) -0.007(3) 0.006(3) C46 0.049(3) 0.045(3) 0.059(3) -0.012(3) -0.012(3) 0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 B1 1.373(5) . ? O1 B2 1.416(5) . ? P1 N1 1.555(3) . ? P1 N11 1.629(4) . ? P1 N13 1.652(3) . ? P1 N12 1.659(3) . ? B1'' B2'' 1.754(8) . ? B1'' B3'' 1.754(9) . ? B1'' B6 1.768(8) . ? B1'' B4'' 1.769(9) . ? B1'' B5 1.792(9) . ? B1'' H1'' 0.97(4) . ? B1' B6' 1.681(10) . ? B1' B2' 1.707(10) . ? B1' B3' 1.728(10) . ? B1' B5' 1.776(11) . ? B1' B4' 1.788(9) . ? B1' H1' 0.97(4) . ? N1 B1 1.402(6) . ? B1 N3 1.463(5) . ? P2 N2 1.554(3) . ? P2 N22 1.635(3) . ? P2 N23 1.656(4) . ? P2 N21 1.663(3) . ? B2'' B3'' 1.731(8) . ? B2'' C8'' 1.735(8) . ? B2'' C7'' 1.736(8) . ? B2'' B6 1.755(9) . ? B2'' H2'' 1.05(4) . ? B2' C7' 1.607(11) . ? B2' C8' 1.702(10) . ? B2' B3' 1.750(12) . ? B2' B6' 1.793(13) . ? B2' H2' 1.19(5) . ? N2 B2 1.389(5) . ? B2 N4 1.464(6) . ? P3 N32 1.614(4) . ? P3 N31 1.625(3) . ? P3 N3 1.630(4) . ? P3 N33 1.635(3) . ? B3'' C8'' 1.709(8) . ? B3'' B4'' 1.764(8) . ? B3'' B9 1.778(9) . ? B3'' H3'' 1.07(4) . ? B3' B4' 1.674(11) . ? B3' C8' 1.693(11) . ? B3' B9' 1.779(10) . ? B3' H3' 1.32(5) . ? N3 H3 0.79(4) . ? P4 N43 1.609(4) . ? P4 N4 1.615(3) . ? P4 N42 1.624(4) . ? P4 N41 1.628(4) . ? B4'' B9 1.758(9) . ? B4'' B10 1.782(9) . ? B4'' B5 1.803(8) . ? B4'' H4'' 1.03(4) . ? B4' B10' 1.709(11) . ? B4' B9' 1.736(9) . ? B4' B5' 1.808(11) . ? B4' H4' 0.93(5) . ? N4 H4 0.89(4) . ? B5 B11 1.737(9) . ? B5 B10 1.761(10) . ? B5 B6 1.779(10) . ? B5 H5 1.04(5) . ? B5' B6' 1.674(12) . ? B5' B10' 1.715(11) . ? B5' B11' 1.894(11) . ? B5' H5' 0.96(5) . ? B6 C7'' 1.696(8) . ? B6 B11 1.795(10) . ? B6 H6 1.04(4) . ? B6' B11' 1.700(10) . ? B6' C7' 1.778(13) . ? B6' H6' 1.10(6) . ? C7'' C8'' 1.580(7) . ? C7'' B11 1.636(8) . ? C7'' H7'' 1.03(5) . ? C7' C8' 1.431(9) . ? C7' B11' 1.456(10) . ? C7' H7' 1.10(7) . ? C8'' B9 1.615(8) . ? C8'' H8'' 1.12(4) . ? C8' B9' 1.517(9) . ? C8' H8' 1.22(6) . ? B9 B10 1.782(9) . ? B9 H9 1.13(4) . ? B9' B10' 1.811(10) . ? B9' H9' 1.15(5) . ? B9' H12' 1.59(7) . ? B10 B11 1.776(10) . ? B10 H10 1.10(5) . ? B10 H12 1.28(8) . ? B10' B11' 1.977(13) . ? B10' H10' 0.87(7) . ? B10' H12' 1.17(7) . ? B11 H12 1.29(8) . ? B11 H11 1.20(4) . ? B11' H12' 1.59(7) . ? B11' H11' 0.97(5) . ? C11 N11 1.470(5) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? N11 C12 1.468(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? N12 C13 1.468(5) . ? N12 C14 1.476(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? N13 C16 1.467(5) . ? N13 C15 1.473(5) . ? C14 H14A 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C21 N21 1.453(5) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N21 C22 1.461(5) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22A 0.9600 . ? N22 C24 1.461(5) . ? N22 C23 1.475(5) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N23 C25 1.453(5) . ? N23 C26 1.461(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C31 N31 1.475(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N31 C32 1.453(5) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N32 C33 1.453(5) . ? N32 C34 1.475(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? N33 C35 1.464(5) . ? N33 C36 1.467(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C41 N41 1.452(6) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? N41 C42 1.456(5) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N42 C43 1.416(6) . ? N42 C44 1.465(6) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? N43 C46 1.461(5) . ? N43 C45 1.469(5) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? 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 O1 B2 127.8(3) . . ? N1 P1 N11 107.22(17) . . ? N1 P1 N13 119.51(18) . . ? N11 P1 N13 102.88(18) . . ? N1 P1 N12 110.38(17) . . ? N11 P1 N12 114.84(18) . . ? N13 P1 N12 102.14(17) . . ? B2'' B1'' B3'' 59.1(3) . . ? B2'' B1'' B6 59.8(3) . . ? B3'' B1'' B6 107.4(4) . . ? B2'' B1'' B4'' 107.7(5) . . ? B3'' B1'' B4'' 60.1(4) . . ? B6 B1'' B4'' 108.8(5) . . ? B2'' B1'' B5 107.4(4) . . ? B3'' B1'' B5 108.0(5) . . ? B6 B1'' B5 60.0(4) . . ? B4'' B1'' B5 60.8(4) . . ? B2'' B1'' H1'' 121(3) . . ? B3'' B1'' H1'' 127(3) . . ? B6 B1'' H1'' 117(3) . . ? B4'' B1'' H1'' 125(3) . . ? B5 B1'' H1'' 119(3) . . ? B6' B1' B2' 63.9(5) . . ? B6' B1' B3' 112.5(6) . . ? B2' B1' B3' 61.3(5) . . ? B6' B1' B5' 57.9(5) . . ? B2' B1' B5' 108.1(6) . . ? B3' B1' B5' 107.6(5) . . ? B6' B1' B4' 107.8(5) . . ? B2' B1' B4' 105.8(5) . . ? B3' B1' B4' 56.8(4) . . ? B5' B1' B4' 61.0(4) . . ? B6' B1' H1' 123(3) . . ? B2' B1' H1' 120(3) . . ? B3' B1' H1' 117(3) . . ? B5' B1' H1' 125(3) . . ? B4' B1' H1' 122(3) . . ? B1 N1 P1 134.4(3) . . ? O1 B1 N1 122.8(4) . . ? O1 B1 N3 114.2(4) . . ? N1 B1 N3 123.0(4) . . ? N2 P2 N22 113.15(18) . . ? N2 P2 N23 111.96(18) . . ? N22 P2 N23 109.70(19) . . ? N2 P2 N21 113.66(18) . . ? N22 P2 N21 101.62(18) . . ? N23 P2 N21 106.07(18) . . ? B3'' B2'' C8'' 59.1(3) . . ? B3'' B2'' C7'' 103.4(4) . . ? C8'' B2'' C7'' 54.2(3) . . ? B3'' B2'' B1'' 60.4(4) . . ? C8'' B2'' B1'' 103.3(4) . . ? C7'' B2'' B1'' 103.3(4) . . ? B3'' B2'' B6 109.1(5) . . ? C8'' B2'' B6 102.1(4) . . ? C7'' B2'' B6 58.1(3) . . ? B1'' B2'' B6 60.5(3) . . ? B3'' B2'' H2'' 127(3) . . ? C8'' B2'' H2'' 120(2) . . ? C7'' B2'' H2'' 116(2) . . ? B1'' B2'' H2'' 133(2) . . ? B6 B2'' H2'' 121(3) . . ? C7' B2' C8' 51.1(5) . . ? C7' B2' B1' 104.4(6) . . ? C8' B2' B1' 101.7(5) . . ? C7' B2' B3' 101.8(6) . . ? C8' B2' B3' 58.7(5) . . ? B1' B2' B3' 60.0(4) . . ? C7' B2' B6' 62.7(6) . . ? C8' B2' B6' 101.3(6) . . ? B1' B2' B6' 57.3(4) . . ? B3' B2' B6' 106.3(6) . . ? C7' B2' H2' 120(3) . . ? C8' B2' H2' 122(3) . . ? B1' B2' H2' 131(3) . . ? B3' B2' H2' 123(3) . . ? B6' B2' H2' 126(3) . . ? B2 N2 P2 134.0(3) . . ? N2 B2 O1 124.0(4) . . ? N2 B2 N4 121.5(4) . . ? O1 B2 N4 114.5(4) . . ? N32 P3 N31 112.21(18) . . ? N32 P3 N3 111.50(19) . . ? N31 P3 N3 106.32(19) . . ? N32 P3 N33 104.82(18) . . ? N31 P3 N33 110.73(19) . . ? N3 P3 N33 111.37(19) . . ? C8'' B3'' B2'' 60.6(3) . . ? C8'' B3'' B1'' 104.4(4) . . ? B2'' B3'' B1'' 60.4(3) . . ? C8'' B3'' B4'' 101.8(4) . . ? B2'' B3'' B4'' 109.0(4) . . ? B1'' B3'' B4'' 60.4(4) . . ? C8'' B3'' B9 55.1(3) . . ? B2'' B3'' B9 107.4(4) . . ? B1'' B3'' B9 107.2(5) . . ? B4'' B3'' B9 59.5(3) . . ? C8'' B3'' H3'' 121(2) . . ? B2'' B3'' H3'' 123(2) . . ? B1'' B3'' H3'' 129(2) . . ? B4'' B3'' H3'' 124(2) . . ? B9 B3'' H3'' 117(2) . . ? B4' B3' C8' 98.1(6) . . ? B4' B3' B1' 63.4(4) . . ? C8' B3' B1' 101.1(6) . . ? B4' B3' B2' 108.9(6) . . ? C8' B3' B2' 59.2(5) . . ? B1' B3' B2' 58.8(4) . . ? B4' B3' B9' 60.3(4) . . ? C8' B3' B9' 51.8(4) . . ? B1' B3' B9' 109.2(5) . . ? B2' B3' B9' 105.0(6) . . ? B4' B3' H3' 128(2) . . ? C8' B3' H3' 122(2) . . ? B1' B3' H3' 129(2) . . ? B2' B3' H3' 120(2) . . ? B9' B3' H3' 119(2) . . ? B1 N3 P3 135.5(3) . . ? B1 N3 H3 108(3) . . ? P3 N3 H3 116(3) . . ? N43 P4 N4 111.58(19) . . ? N43 P4 N42 106.10(19) . . ? N4 P4 N42 109.48(19) . . ? N43 P4 N41 112.6(2) . . ? N4 P4 N41 108.32(18) . . ? N42 P4 N41 108.7(2) . . ? B9 B4'' B3'' 60.6(3) . . ? B9 B4'' B1'' 107.4(4) . . ? B3'' B4'' B1'' 59.5(3) . . ? B9 B4'' B10 60.4(4) . . ? B3'' B4'' B10 110.0(4) . . ? B1'' B4'' B10 108.9(4) . . ? B9 B4'' B5 105.5(4) . . ? B3'' B4'' B5 107.1(4) . . ? B1'' B4'' B5 60.2(4) . . ? B10 B4'' B5 58.8(4) . . ? B9 B4'' H4'' 123(2) . . ? B3'' B4'' H4'' 127(2) . . ? B1'' B4'' H4'' 125(2) . . ? B10 B4'' H4'' 115(2) . . ? B5 B4'' H4'' 119(2) . . ? B3' B4' B10' 115.1(6) . . ? B3' B4' B9' 62.8(4) . . ? B10' B4' B9' 63.4(4) . . ? B3' B4' B1' 59.8(4) . . ? B10' B4' B1' 108.6(6) . . ? B9' B4' B1' 108.4(5) . . ? B3' B4' B5' 108.6(5) . . ? B10' B4' B5' 58.3(5) . . ? B9' B4' B5' 107.2(5) . . ? B1' B4' B5' 59.2(4) . . ? B3' B4' H4' 124(3) . . ? B10' B4' H4' 114(3) . . ? B9' B4' H4' 123(3) . . ? B1' B4' H4' 123(3) . . ? B5' B4' H4' 118(3) . . ? B2 N4 P4 130.2(3) . . ? B2 N4 H4 114(2) . . ? P4 N4 H4 115(2) . . ? B11 B5 B10 61.0(4) . . ? B11 B5 B6 61.4(4) . . ? B10 B5 B6 111.0(5) . . ? B11 B5 B1'' 107.8(5) . . ? B10 B5 B1'' 108.8(5) . . ? B6 B5 B1'' 59.3(3) . . ? B11 B5 B4'' 106.9(5) . . ? B10 B5 B4'' 60.0(4) . . ? B6 B5 B4'' 106.9(4) . . ? B1'' B5 B4'' 59.0(3) . . ? B11 B5 H5 122(3) . . ? B10 B5 H5 126(3) . . ? B6 B5 H5 115(3) . . ? B1'' B5 H5 119(3) . . ? B4'' B5 H5 126(3) . . ? B6' B5' B10' 114.3(6) . . ? B6' B5' B1' 58.2(4) . . ? B10' B5' B1' 108.9(5) . . ? B6' B5' B4' 107.2(5) . . ? B10' B5' B4' 58.0(4) . . ? B1' B5' B4' 59.8(4) . . ? B6' B5' B11' 56.5(5) . . ? B10' B5' B11' 66.2(5) . . ? B1' B5' B11' 100.4(5) . . ? B4' B5' B11' 104.1(4) . . ? B6' B5' H5' 118(4) . . ? B10' B5' H5' 120(4) . . ? B1' B5' H5' 122(4) . . ? B4' B5' H5' 125(4) . . ? B11' B5' H5' 125(3) . . ? C7'' B6 B2'' 60.4(3) . . ? C7'' B6 B1'' 104.4(4) . . ? B2'' B6 B1'' 59.7(3) . . ? C7'' B6 B5 101.6(5) . . ? B2'' B6 B5 108.0(4) . . ? B1'' B6 B5 60.7(4) . . ? C7'' B6 B11 55.8(3) . . ? B2'' B6 B11 106.8(4) . . ? B1'' B6 B11 106.4(5) . . ? B5 B6 B11 58.2(4) . . ? C7'' B6 H6 123(3) . . ? B2'' B6 H6 125(3) . . ? B1'' B6 H6 127(2) . . ? B5 B6 H6 122(3) . . ? B11 B6 H6 118(3) . . ? B5' B6' B1' 63.9(5) . . ? B5' B6' B11' 68.3(5) . . ? B1' B6' B11' 113.2(5) . . ? B5' B6' C7' 101.0(6) . . ? B1' B6' C7' 98.4(5) . . ? B11' B6' C7' 49.5(4) . . ? B5' B6' B2' 108.8(6) . . ? B1' B6' B2' 58.7(5) . . ? B11' B6' B2' 99.3(6) . . ? C7' B6' B2' 53.5(4) . . ? B5' B6' H6' 134(3) . . ? B1' B6' H6' 128(3) . . ? B11' B6' H6' 119(3) . . ? C7' B6' H6' 117(3) . . ? B2' B6' H6' 114(3) . . ? C8'' C7'' B11 110.2(4) . . ? C8'' C7'' B6 111.9(4) . . ? B11 C7'' B6 65.2(4) . . ? C8'' C7'' B2'' 62.9(3) . . ? B11 C7'' B2'' 115.3(4) . . ? B6 C7'' B2'' 61.5(3) . . ? C8'' C7'' H7'' 122(3) . . ? B11 C7'' H7'' 121(3) . . ? B6 C7'' H7'' 113(3) . . ? B2'' C7'' H7'' 112(2) . . ? C8' C7' B11' 115.3(9) . . ? C8' C7' B2' 67.9(5) . . ? B11' C7' B2' 120.6(7) . . ? C8' C7' B6' 114.4(6) . . ? B11' C7' B6' 62.5(5) . . ? B2' C7' B6' 63.8(6) . . ? C8' C7' H7' 107(4) . . ? B11' C7' H7' 115(4) . . ? B2' C7' H7' 120(4) . . ? B6' C7' H7' 135(4) . . ? C7'' C8'' B9 113.1(4) . . ? C7'' C8'' B3'' 111.5(4) . . ? B9 C8'' B3'' 64.6(4) . . ? C7'' C8'' B2'' 63.0(3) . . ? B9 C8'' B2'' 115.2(4) . . ? B3'' C8'' B2'' 60.3(3) . . ? C7'' C8'' H8'' 112(2) . . ? B9 C8'' H8'' 126(2) . . ? B3'' C8'' H8'' 122(2) . . ? B2'' C8'' H8'' 111(2) . . ? C7' C8' B9' 119.5(8) . . ? C7' C8' B3' 112.9(6) . . ? B9' C8' B3' 67.0(5) . . ? C7' C8' B2' 61.0(5) . . ? B9' C8' B2' 120.8(5) . . ? B3' C8' B2' 62.1(5) . . ? C7' C8' H8' 110(3) . . ? B9' C8' H8' 129(3) . . ? B3' C8' H8' 105(3) . . ? B2' C8' H8' 93(3) . . ? C8'' B9 B4'' 106.0(5) . . ? C8'' B9 B3'' 60.3(3) . . ? B4'' B9 B3'' 59.8(3) . . ? C8'' B9 B10 106.4(5) . . ? B4'' B9 B10 60.5(4) . . ? B3'' B9 B10 109.4(5) . . ? C8'' B9 H9 120(2) . . ? B4'' B9 H9 121(2) . . ? B3'' B9 H9 113(2) . . ? B10 B9 H9 128(2) . . ? C8' B9' B4' 102.7(5) . . ? C8' B9' B3' 61.2(5) . . ? B4' B9' B3' 56.9(4) . . ? C8' B9' B10' 104.7(6) . . ? B4' B9' B10' 57.5(4) . . ? B3' B9' B10' 105.3(5) . . ? C8' B9' H9' 122(2) . . ? B4' B9' H9' 125(2) . . ? B3' B9' H9' 119(2) . . ? B10' B9' H9' 126(2) . . ? C8' B9' H12' 78(3) . . ? B4' B9' H12' 92(3) . . ? B3' B9' H12' 117(3) . . ? B10' B9' H12' 40(3) . . ? H9' B9' H12' 124(3) . . ? B5 B10 B11 58.8(4) . . ? B5 B10 B9 106.3(5) . . ? B11 B10 B9 102.8(5) . . ? B5 B10 B4'' 61.2(4) . . ? B11 B10 B4'' 106.2(4) . . ? B9 B10 B4'' 59.1(3) . . ? B5 B10 H10 123(3) . . ? B11 B10 H10 126(3) . . ? B9 B10 H10 122(3) . . ? B4'' B10 H10 121(3) . . ? B5 B10 H12 103(4) . . ? B11 B10 H12 46(4) . . ? B9 B10 H12 78(3) . . ? B4'' B10 H12 123(3) . . ? H10 B10 H12 114(5) . . ? B4' B10' B5' 63.8(5) . . ? B4' B10' B9' 59.0(4) . . ? B5' B10' B9' 108.0(5) . . ? B4' B10' B11' 104.6(5) . . ? B5' B10' B11' 61.3(5) . . ? B9' B10' B11' 95.2(6) . . ? B4' B10' H10' 128(5) . . ? B5' B10' H10' 125(4) . . ? B9' B10' H10' 124(4) . . ? B11' B10' H10' 125(5) . . ? B4' B10' H12' 111(3) . . ? B5' B10' H12' 110(4) . . ? B9' B10' H12' 60(3) . . ? B11' B10' H12' 53(4) . . ? H10' B10' H12' 111(6) . . ? C7'' B11 B5 105.9(5) . . ? C7'' B11 B10 107.4(4) . . ? B5 B11 B10 60.2(4) . . ? C7'' B11 B6 59.0(4) . . ? B5 B11 B6 60.5(4) . . ? B10 B11 B6 109.6(4) . . ? C7'' B11 H12 83(4) . . ? B5 B11 H12 104(4) . . ? B10 B11 H12 46(4) . . ? B6 B11 H12 128(3) . . ? C7'' B11 H11 118.9(17) . . ? B5 B11 H11 122.0(17) . . ? B10 B11 H11 127.9(17) . . ? B6 B11 H11 113.9(17) . . ? H12 B11 H11 116(4) . . ? C7' B11' B6' 68.1(6) . . ? C7' B11' B5' 104.6(5) . . ? B6' B11' B5' 55.2(4) . . ? C7' B11' B10' 104.3(6) . . ? B6' B11' B10' 101.2(5) . . ? B5' B11' B10' 52.5(4) . . ? C7' B11' H12' 83(3) . . ? B6' B11' H12' 120(2) . . ? B5' B11' H12' 86(3) . . ? B10' B11' H12' 36(3) . . ? C7' B11' H11' 141(3) . . ? B6' B11' H11' 115(3) . . ? B5' B11' H11' 108(3) . . ? B10' B11' H11' 113(4) . . ? H12' B11' H11' 120(4) . . ? N11 C11 H11A 109.5 . . ? N11 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N11 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C12 N11 C11 112.5(4) . . ? C12 N11 P1 123.6(3) . . ? C11 N11 P1 122.8(3) . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C13 N12 C14 110.3(3) . . ? C13 N12 P1 118.0(3) . . ? C14 N12 P1 120.5(3) . . ? N12 C13 H13A 109.5 . . ? N12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 N13 C15 111.6(3) . . ? C16 N13 P1 119.4(3) . . ? C15 N13 P1 118.9(3) . . ? N12 C14 H14A 109.5 . . ? N12 C14 H14A 109.5 . . ? H14A C14 H14A 109.5 . . ? N12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N13 C15 H15A 109.5 . . ? N13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N13 C16 H16A 109.5 . . ? N13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N21 C21 H21A 109.5 . . ? N21 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N21 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C21 N21 C22 112.9(3) . . ? C21 N21 P2 117.2(3) . . ? C22 N21 P2 117.2(3) . . ? N21 C22 H22A 109.5 . . ? N21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N21 C22 H22A 109.5 . . ? H22A C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C24 N22 C23 113.8(3) . . ? C24 N22 P2 126.2(3) . . ? C23 N22 P2 119.2(3) . . ? N22 C23 H23A 109.5 . . ? N22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 N23 C26 113.8(4) . . ? C25 N23 P2 123.0(3) . . ? C26 N23 P2 120.7(3) . . ? N22 C24 H24A 109.5 . . ? N22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N23 C25 H25A 109.5 . . ? N23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N23 C26 H26A 109.5 . . ? N23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N31 C31 H31A 109.5 . . ? N31 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N31 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 N31 C31 113.2(4) . . ? C32 N31 P3 124.8(3) . . ? C31 N31 P3 119.6(3) . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C33 N32 C34 113.9(4) . . ? C33 N32 P3 121.7(3) . . ? C34 N32 P3 124.0(3) . . ? N32 C33 H33A 109.5 . . ? N32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 N33 C36 112.5(4) . . ? C35 N33 P3 120.5(3) . . ? C36 N33 P3 120.7(3) . . ? N32 C34 H34A 109.5 . . ? N32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N33 C35 H35A 109.5 . . ? N33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N33 C36 H36A 109.5 . . ? N33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N41 C41 H41A 109.5 . . ? N41 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N41 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C41 N41 C42 114.4(4) . . ? C41 N41 P4 121.2(3) . . ? C42 N41 P4 123.5(3) . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C43 N42 C44 112.7(4) . . ? C43 N42 P4 125.3(3) . . ? C44 N42 P4 119.1(3) . . ? N42 C43 H43A 109.5 . . ? N42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C46 N43 C45 114.0(3) . . ? C46 N43 P4 122.6(3) . . ? C45 N43 P4 122.3(3) . . ? N42 C44 H44A 109.5 . . ? N42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N43 C45 H45A 109.5 . . ? N43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N43 C46 H46A 109.5 . . ? N43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 30.48 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.537 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.061 #========================================================END