Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_contact_author_name 'Prof Michael F. Lappert' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry University of Sussex Brighton BN1 9QJ UNITED KINGDOM ; _publ_section_title ; Synthesis and P-P cleavage reactions of [P(X)X']2; X-ray structures of [Co{P(X)X'}(CO)3] and P4[P(X)X']2 [X = N(SiMe3)2, X' = N(i-Pr)2] ; _publ_requested_category FM loop_ _publ_author_name 'Michael F. Lappert' 'Jean Philippe Bezombes' 'Peter B. Hitchcock' 'Jacek E. Nycz' data_aug3302 _database_code_depnum_ccdc_archive 'CCDC 218767' _chemical_name_common (Co(CO)3(P(N(iPr)2)(N(SiMe3)2))) _audit_creation_date 2002-08-22T11:06:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C15 H32 Co1 N2 O3 P1 Si2' _chemical_formula_sum 'C15 H32 Co1 N2 O3 P1 Si2' _chemical_formula_weight 434.51 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7190(6) _cell_length_b 9.8945(7) _cell_length_c 13.6614(12) _cell_angle_alpha 88.878(4) _cell_angle_beta 89.121(4) _cell_angle_gamma 61.153(4) _cell_volume 1150.48(15) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 17407 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.933 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8882 _exptl_absorpt_correction_T_max 0.9732 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_unetI/netI 0.0794 _diffrn_reflns_number 8590 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 23.06 _diffrn_reflns_theta_full 23.06 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 3147 _reflns_number_gt 2327 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0777P)^2^+2.5683P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 3147 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1011 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.783 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Co Co 0.16643(10) 0.71064(11) 0.25175(7) 0.0500(4) Uani 1 1 d . . . P P -0.06435(18) 0.76366(19) 0.24996(12) 0.0391(4) Uani 1 1 d . . . Si1 Si -0.2772(2) 1.0449(2) 0.13800(15) 0.0535(6) Uani 1 1 d . . . Si2 Si -0.2673(3) 1.0392(3) 0.36550(15) 0.0584(6) Uani 1 1 d . . . O1 O 0.1822(8) 0.9973(8) 0.2425(6) 0.101(2) Uani 1 1 d . . . O2 O 0.3477(8) 0.5238(9) 0.0867(6) 0.104(2) Uani 1 1 d . . . O3 O 0.3245(9) 0.5475(9) 0.4297(5) 0.111(2) Uani 1 1 d . . . N1 N -0.1510(6) 0.6579(6) 0.2480(4) 0.0419(13) Uani 1 1 d . . . N2 N -0.2124(6) 0.9449(5) 0.2508(4) 0.0380(12) Uani 1 1 d . . . C1 C 0.1710(8) 0.8862(11) 0.2471(6) 0.065(2) Uani 1 1 d . . . C2 C 0.2783(9) 0.5961(9) 0.1544(7) 0.069(2) Uani 1 1 d . . . C3 C 0.2648(10) 0.6094(10) 0.3585(7) 0.071(2) Uani 1 1 d . . . C4 C -0.4920(10) 1.1110(11) 0.1220(7) 0.085(3) Uani 1 1 d . . . H4A H -0.5511 1.1792 0.175 0.128 Uiso 1 1 calc R . . H4B H -0.5091 1.0221 0.1229 0.128 Uiso 1 1 calc R . . H4C H -0.5267 1.1658 0.06 0.128 Uiso 1 1 calc R . . C5 C -0.1682(11) 0.9162(11) 0.0362(6) 0.084(3) Uani 1 1 d . . . H5A H -0.1854 0.8274 0.0376 0.127 Uiso 1 1 calc R . . H5B H -0.057 0.882 0.0429 0.127 Uiso 1 1 calc R . . H5C H -0.2051 0.9716 -0.0255 0.127 Uiso 1 1 calc R . . C6 C -0.2432(15) 1.2150(12) 0.1342(8) 0.109(4) Uani 1 1 d . . . H6A H -0.3002 1.2834 0.1875 0.163 Uiso 1 1 calc R . . H6B H -0.2799 1.2698 0.0723 0.163 Uiso 1 1 calc R . . H6C H -0.1318 1.1804 0.1407 0.163 Uiso 1 1 calc R . . C7 C -0.4811(12) 1.1534(16) 0.3740(8) 0.147(6) Uani 1 1 d . . . H7A H -0.5276 1.0876 0.3629 0.221 Uiso 1 1 calc R . . H7B H -0.5186 1.2355 0.325 0.221 Uiso 1 1 calc R . . H7C H -0.5106 1.1978 0.4387 0.221 Uiso 1 1 calc R . . C8 C -0.176(2) 1.1600(17) 0.3864(9) 0.156(6) Uani 1 1 d . . . H8A H -0.0632 1.0978 0.3819 0.234 Uiso 1 1 calc R . . H8B H -0.2054 1.2046 0.4511 0.234 Uiso 1 1 calc R . . H8C H -0.2126 1.242 0.3374 0.234 Uiso 1 1 calc R . . C9 C -0.1995(14) 0.8911(13) 0.4650(6) 0.108(4) Uani 1 1 d . . . H9A H -0.0861 0.8292 0.4619 0.162 Uiso 1 1 calc R . . H9B H -0.2468 0.8252 0.4571 0.162 Uiso 1 1 calc R . . H9C H -0.2304 0.9415 0.5278 0.162 Uiso 1 1 calc R . . C10 C -0.0595(9) 0.4835(8) 0.2451(6) 0.059(2) Uani 1 1 d . . . H10 H -0.1387 0.4479 0.2465 0.071 Uiso 1 1 calc R . . C11 C 0.0289(11) 0.4285(11) 0.1493(9) 0.102(4) Uani 1 1 d . . . H11A H -0.0428 0.4768 0.0952 0.153 Uiso 1 1 calc R . . H11B H 0.0742 0.3173 0.1457 0.153 Uiso 1 1 calc R . . H11C H 0.112 0.4562 0.1456 0.153 Uiso 1 1 calc R . . C12 C 0.0415(12) 0.4131(11) 0.3363(9) 0.107(4) Uani 1 1 d . . . H12A H -0.0232 0.4531 0.3945 0.161 Uiso 1 1 calc R . . H12B H 0.1253 0.4397 0.3367 0.161 Uiso 1 1 calc R . . H12C H 0.0863 0.3017 0.3355 0.161 Uiso 1 1 calc R . . C13 C -0.3254(8) 0.7174(8) 0.2487(5) 0.0523(18) Uani 1 1 d . . . H13 H -0.3758 0.8311 0.2535 0.063 Uiso 1 1 calc R . . C14 C -0.3811(10) 0.6828(10) 0.1536(6) 0.075(2) Uani 1 1 d . . . H14A H -0.3461 0.7225 0.0987 0.113 Uiso 1 1 calc R . . H14B H -0.4949 0.7318 0.154 0.113 Uiso 1 1 calc R . . H14C H -0.3377 0.5721 0.1475 0.113 Uiso 1 1 calc R . . C15 C -0.3795(10) 0.6596(11) 0.3373(6) 0.078(3) Uani 1 1 d . . . H15A H -0.3438 0.6851 0.3966 0.116 Uiso 1 1 calc R . . H15B H -0.3359 0.5485 0.3338 0.116 Uiso 1 1 calc R . . H15C H -0.4933 0.7083 0.338 0.116 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 Co 0.0310(5) 0.0440(6) 0.0672(7) 0.0034(5) -0.0041(4) -0.0121(4) P 0.0301(9) 0.0344(10) 0.0464(10) 0.0025(7) -0.0032(7) -0.0107(8) Si1 0.0567(12) 0.0463(12) 0.0494(12) 0.0130(9) -0.0132(10) -0.0187(10) Si2 0.0600(13) 0.0568(14) 0.0478(12) -0.0127(10) 0.0056(10) -0.0195(11) O1 0.098(5) 0.067(4) 0.159(7) -0.004(4) 0.006(4) -0.056(4) O2 0.094(5) 0.095(5) 0.114(6) -0.028(5) 0.041(5) -0.038(4) O3 0.120(6) 0.103(6) 0.104(5) 0.042(5) -0.060(5) -0.049(5) N1 0.033(3) 0.040(3) 0.044(3) 0.005(2) -0.006(2) -0.011(3) N2 0.035(3) 0.030(3) 0.041(3) -0.004(2) 0.002(2) -0.010(2) C1 0.039(4) 0.079(6) 0.076(6) 0.000(5) -0.005(4) -0.028(4) C2 0.041(4) 0.050(5) 0.105(7) 0.001(5) 0.006(5) -0.015(4) C3 0.065(5) 0.066(6) 0.084(6) 0.017(5) -0.024(5) -0.034(5) C4 0.076(6) 0.082(7) 0.080(6) 0.028(5) -0.037(5) -0.023(5) C5 0.097(7) 0.088(7) 0.047(5) 0.012(5) 0.001(5) -0.029(6) C6 0.158(11) 0.090(8) 0.109(8) 0.048(6) -0.051(7) -0.085(8) C7 0.078(7) 0.167(13) 0.089(8) -0.049(8) 0.015(6) 0.028(7) C8 0.279(19) 0.162(13) 0.104(9) -0.063(9) 0.048(11) -0.167(14) C9 0.139(10) 0.118(9) 0.041(5) -0.001(5) -0.008(5) -0.041(7) C10 0.049(4) 0.040(4) 0.085(6) 0.001(4) -0.006(4) -0.020(4) C11 0.084(7) 0.065(6) 0.154(10) -0.049(7) 0.047(7) -0.033(5) C12 0.102(8) 0.060(6) 0.159(10) 0.058(6) -0.077(7) -0.040(6) C13 0.039(4) 0.044(4) 0.068(5) 0.003(4) -0.004(3) -0.015(3) C14 0.071(5) 0.078(6) 0.086(6) 0.011(5) -0.031(5) -0.042(5) C15 0.061(5) 0.102(7) 0.083(6) -0.001(5) 0.016(5) -0.051(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Co C2 1.749(10) . ? Co C1 1.759(9) . ? Co C3 1.762(9) . ? Co P 2.0426(18) . ? P N1 1.630(5) . ? P N2 1.672(5) . ? Si1 N2 1.767(5) . ? Si1 C5 1.844(9) . ? Si1 C6 1.865(9) . ? Si1 C4 1.878(9) . ? Si2 N2 1.778(5) . ? Si2 C7 1.828(10) . ? Si2 C8 1.825(11) . ? Si2 C9 1.856(10) . ? O1 C1 1.156(9) . ? O2 C2 1.168(10) . ? O3 C3 1.144(10) . ? N1 C13 1.502(8) . ? N1 C10 1.513(8) . ? C10 C11 1.513(12) . ? C10 C12 1.531(11) . ? C13 C14 1.521(10) . ? C13 C15 1.521(10) . ? 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 C2 Co C1 108.8(4) . . ? C2 Co C3 105.3(4) . . ? C1 Co C3 108.0(4) . . ? C2 Co P 114.2(3) . . ? C1 Co P 107.1(2) . . ? C3 Co P 113.1(3) . . ? N1 P N2 104.2(3) . . ? N1 P Co 132.8(2) . . ? N2 P Co 123.03(19) . . ? N2 Si1 C5 109.9(3) . . ? N2 Si1 C6 110.0(4) . . ? C5 Si1 C6 108.9(5) . . ? N2 Si1 C4 109.9(3) . . ? C5 Si1 C4 108.4(4) . . ? C6 Si1 C4 109.6(5) . . ? N2 Si2 C7 109.9(4) . . ? N2 Si2 C8 112.5(4) . . ? C7 Si2 C8 110.5(8) . . ? N2 Si2 C9 108.9(4) . . ? C7 Si2 C9 108.1(6) . . ? C8 Si2 C9 106.8(6) . . ? C13 N1 C10 112.2(5) . . ? C13 N1 P 125.7(4) . . ? C10 N1 P 122.1(4) . . ? P N2 Si1 118.5(3) . . ? P N2 Si2 117.5(3) . . ? Si1 N2 Si2 122.6(3) . . ? O1 C1 Co 176.4(7) . . ? O2 C2 Co 177.0(8) . . ? O3 C3 Co 177.6(9) . . ? C11 C10 N1 111.3(6) . . ? C11 C10 C12 114.3(8) . . ? N1 C10 C12 112.5(6) . . ? N1 C13 C14 111.8(6) . . ? N1 C13 C15 112.3(6) . . ? C14 C13 C15 111.5(6) . . ? #===END data_mar1901 _database_code_depnum_ccdc_archive 'CCDC 218768' _chemical_name_common (P4(P(NiPr2)(N(SiMe3)2))2) _audit_creation_date 2001-03-19T14:38:41-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C24 H64 N4 P6 Si4' _chemical_formula_structural 'C24 H64 N4 P6 SI4' _chemical_formula_sum 'C24 H64 N4 P6 Si4' _chemical_formula_weight 706.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Pa _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z' _cell_length_a 13.8004(7) _cell_length_b 11.0049(5) _cell_length_c 14.7827(7) _cell_angle_alpha 90 _cell_angle_beta 112.336(2) _cell_angle_gamma 90 _cell_volume 2076.63(17) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7324 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.131 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_T_min 0.8909 _exptl_absorpt_correction_T_max 0.8909 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_orient_matrix_ub_33 0.01 _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 9087 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 25.05 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 5552 _reflns_number_gt 4876 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The P atoms are disordered 75:25 over the arrangement shown and that related by inversion through the centre of the P4 group. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+2.2740P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5552 _refine_ls_number_parameters 398 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1207 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(18) _refine_diff_density_max 0.688 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.055 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Si1 Si 0.61148(13) 0.45443(14) 0.39967(13) 0.0399(4) Uani 1 1 d . . . Si2 Si 0.67551(13) 0.26465(16) 0.28601(11) 0.0400(4) Uani 1 1 d . . . Si3 Si 1.16901(13) 0.03503(15) 0.93412(13) 0.0421(4) Uani 1 1 d . C . Si4 Si 1.11631(13) 0.23839(15) 1.04620(12) 0.0400(4) Uani 1 1 d . C . N1 N 0.6514(3) 0.3037(4) 0.3912(3) 0.0303(10) Uani 1 1 d . C . N2 N 0.5911(4) 0.1131(4) 0.4834(4) 0.0398(12) Uani 1 1 d . . . N3 N 1.1318(4) 0.1874(4) 0.9394(3) 0.0321(10) Uani 1 1 d . . . N4 N 1.1807(4) 0.3930(4) 0.8494(3) 0.0372(11) Uani 1 1 d . . . C1 C 0.5418(6) 0.4819(6) 0.4836(5) 0.0523(17) Uani 1 1 d . C . H1A H 0.4802 0.429 0.4654 0.078 Uiso 1 1 calc R . . H1B H 0.5195 0.567 0.4788 0.078 Uiso 1 1 calc R . . H1C H 0.5889 0.4642 0.551 0.078 Uiso 1 1 calc R . . C2 C 0.7286(6) 0.5591(6) 0.4418(6) 0.062(2) Uani 1 1 d . C . H2A H 0.7687 0.5479 0.4001 0.093 Uiso 1 1 calc R . . H2B H 0.7732 0.5401 0.5097 0.093 Uiso 1 1 calc R . . H2C H 0.7048 0.6436 0.4375 0.093 Uiso 1 1 calc R . . C3 C 0.5140(6) 0.5043(7) 0.2793(5) 0.0584(19) Uani 1 1 d . C . H3A H 0.5434 0.4935 0.229 0.088 Uiso 1 1 calc R . . H3B H 0.4972 0.5902 0.2828 0.088 Uiso 1 1 calc R . . H3C H 0.4502 0.4555 0.2626 0.088 Uiso 1 1 calc R . . C4 C 0.7352(7) 0.3910(8) 0.2425(6) 0.077(2) Uani 1 1 d . C . H4A H 0.7999 0.4171 0.2955 0.115 Uiso 1 1 calc R . . H4B H 0.686 0.4593 0.2223 0.115 Uiso 1 1 calc R . . H4C H 0.7514 0.3635 0.1868 0.115 Uiso 1 1 calc R . . C5 C 0.5535(6) 0.2175(7) 0.1853(5) 0.070(2) Uani 1 1 d . C . H5A H 0.5213 0.1503 0.2074 0.104 Uiso 1 1 calc R . . H5B H 0.5697 0.1909 0.1294 0.104 Uiso 1 1 calc R . . H5C H 0.5048 0.2862 0.1659 0.104 Uiso 1 1 calc R . . C6 C 0.7730(7) 0.1392(8) 0.3088(5) 0.072(2) Uani 1 1 d . C . H6A H 0.8386 0.1627 0.3617 0.109 Uiso 1 1 calc R . . H6B H 0.786 0.1237 0.2491 0.109 Uiso 1 1 calc R . . H6C H 0.7454 0.0654 0.3275 0.109 Uiso 1 1 calc R . . C7 C 0.5053(4) 0.1776(6) 0.5059(5) 0.0531(16) Uani 1 1 d . C . H7 H 0.5258 0.2652 0.5166 0.064 Uiso 1 1 calc R A 2 C8 C 0.4041(6) 0.1724(8) 0.4169(7) 0.088(3) Uani 1 1 d . . . H8A H 0.4156 0.2052 0.3602 0.133 Uiso 1 1 calc R C . H8B H 0.3505 0.2207 0.4288 0.133 Uiso 1 1 calc R . . H8C H 0.3806 0.0878 0.404 0.133 Uiso 1 1 calc R . . C9 C 0.4965(7) 0.1333(8) 0.5980(7) 0.080(3) Uani 1 1 d . . . H9A H 0.5643 0.1421 0.6524 0.12 Uiso 1 1 calc R C . H9B H 0.4758 0.0476 0.5906 0.12 Uiso 1 1 calc R . . H9C H 0.4435 0.1813 0.6114 0.12 Uiso 1 1 calc R . . C10 C 0.5736(5) -0.0192(5) 0.4653(5) 0.0546(15) Uani 1 1 d . C . H10 H 0.5066 -0.0407 0.4726 0.065 Uiso 1 1 calc R . . C11 C 0.5651(7) -0.0584(8) 0.3666(6) 0.076(2) Uani 1 1 d . . . H11A H 0.5082 -0.0136 0.3169 0.114 Uiso 1 1 calc R C . H11B H 0.5502 -0.1457 0.359 0.114 Uiso 1 1 calc R . . H11C H 0.6312 -0.0417 0.3587 0.114 Uiso 1 1 calc R . . C12 C 0.6645(6) -0.0906(6) 0.5452(6) 0.068(2) Uani 1 1 d . . . H12A H 0.6693 -0.0652 0.6103 0.101 Uiso 1 1 calc R C . H12B H 0.7308 -0.0733 0.5381 0.101 Uiso 1 1 calc R . . H12C H 0.65 -0.178 0.5373 0.101 Uiso 1 1 calc R . . C13 C 1.2321(7) 0.0069(6) 0.8454(6) 0.065(2) Uani 1 1 d . . . H13A H 1.1848 0.0324 0.78 0.098 Uiso 1 1 calc R C . H13B H 1.2475 -0.0799 0.8445 0.098 Uiso 1 1 calc R . . H13C H 1.2975 0.0535 0.8647 0.098 Uiso 1 1 calc R . . C14 C 1.0550(6) -0.0670(6) 0.9006(6) 0.066(2) Uani 1 1 d . . . H14A H 1.0025 -0.0422 0.8372 0.099 Uiso 1 1 calc R C . H14B H 1.0246 -0.0625 0.9506 0.099 Uiso 1 1 calc R . . H14C H 1.0772 -0.1506 0.8961 0.099 Uiso 1 1 calc R . . C15 C 1.2665(6) -0.0147(7) 1.0549(5) 0.070(2) Uani 1 1 d . . . H15A H 1.3277 0.0391 1.0745 0.105 Uiso 1 1 calc R C . H15B H 1.2885 -0.0982 1.0497 0.105 Uiso 1 1 calc R . . H15C H 1.2348 -0.0111 1.1039 0.105 Uiso 1 1 calc R . . C16 C 1.0548(8) 0.1173(8) 1.0953(6) 0.078(3) Uani 1 1 d . . . H16A H 1.0984 0.044 1.1089 0.117 Uiso 1 1 calc R C . H16B H 0.9849 0.0986 1.0469 0.117 Uiso 1 1 calc R . . H16C H 1.0489 0.1459 1.1558 0.117 Uiso 1 1 calc R . . C17 C 1.2462(7) 0.2811(8) 1.1420(5) 0.074(2) Uani 1 1 d . . . H17A H 1.2947 0.2124 1.1539 0.111 Uiso 1 1 calc R C . H17B H 1.2372 0.3022 1.2027 0.111 Uiso 1 1 calc R . . H17C H 1.2748 0.3512 1.1194 0.111 Uiso 1 1 calc R . . C18 C 1.0265(6) 0.3696(7) 1.0260(5) 0.0607(19) Uani 1 1 d . . . H18A H 1.0538 0.4384 1.0008 0.091 Uiso 1 1 calc R C . H18B H 1.0211 0.3925 1.088 0.091 Uiso 1 1 calc R . . H18C H 0.957 0.3474 0.9785 0.091 Uiso 1 1 calc R . . C19 C 1.2775(5) 0.3949(7) 0.8362(5) 0.0640(19) Uani 1 1 d . C . H19 H 1.2963 0.483 0.8398 0.077 Uiso 1 1 calc R . . C20 C 1.3695(6) 0.3365(7) 0.9179(6) 0.070(2) Uani 1 1 d . . . H20A H 1.3711 0.3651 0.9813 0.105 Uiso 1 1 calc R C . H20B H 1.4349 0.359 0.9109 0.105 Uiso 1 1 calc R . . H20C H 1.3615 0.248 0.9142 0.105 Uiso 1 1 calc R . . C21 C 1.2711(6) 0.3560(7) 0.7365(6) 0.068(2) Uani 1 1 d . . . H21A H 1.2122 0.3974 0.6863 0.101 Uiso 1 1 calc R C . H21B H 1.2605 0.2679 0.7297 0.101 Uiso 1 1 calc R . . H21C H 1.3364 0.3774 0.7286 0.101 Uiso 1 1 calc R . . C22 C 1.1329(5) 0.5118(5) 0.8657(4) 0.0471(14) Uani 1 1 d . C . H22 H 1.0677 0.4923 0.8772 0.056 Uiso 1 1 calc R B 2 C23 C 1.1038(6) 0.5936(5) 0.7776(5) 0.0561(18) Uani 1 1 d . . . H23A H 1.054 0.5516 0.7203 0.084 Uiso 1 1 calc R C . H23B H 1.1669 0.6145 0.7655 0.084 Uiso 1 1 calc R . . H23C H 1.0716 0.6681 0.7896 0.084 Uiso 1 1 calc R . . C24 C 1.2111(7) 0.5758(6) 0.9588(5) 0.063(2) Uani 1 1 d . . . H24A H 1.2283 0.521 1.0149 0.094 Uiso 1 1 calc R C . H24B H 1.179 0.65 0.9714 0.094 Uiso 1 1 calc R . . H24C H 1.2752 0.5968 0.9485 0.094 Uiso 1 1 calc R . . P1 P 0.8776(3) 0.1528(3) 0.6941(2) 0.0333(7) Uani 0.753(4) 1 d P C 1 P2 P 0.9146(2) 0.3066(3) 0.6218(2) 0.0381(7) Uani 0.753(4) 1 d P C 1 P3 P 0.75359(15) 0.28475(18) 0.61700(14) 0.0343(5) Uani 0.753(4) 1 d P C 1 P4 P 0.94571(16) 0.31793(19) 0.77954(15) 0.0363(6) Uani 0.753(4) 1 d P C 1 P5 P 0.69132(15) 0.1825(2) 0.47573(14) 0.0283(5) Uani 0.753(4) 1 d P C 1 P6 P 1.11362(16) 0.2578(2) 0.83018(15) 0.0304(5) Uani 0.753(4) 1 d P C 1 P1A P 0.9002(8) 0.3551(9) 0.6435(7) 0.039(2) Uani 0.247(4) 1 d P C 2 P2A P 0.8664(9) 0.2013(10) 0.7128(7) 0.038(2) Uani 0.247(4) 1 d P C 2 P3A P 0.8351(4) 0.1851(5) 0.5543(4) 0.0295(17) Uani 0.247(4) 1 d P C 2 P4A P 1.0271(4) 0.2169(5) 0.7149(4) 0.0313(17) Uani 0.247(4) 1 d P C 2 P5A P 1.0902(5) 0.3197(6) 0.8578(4) 0.0252(15) Uani 0.247(4) 1 d P C 2 P6A P 0.6659(4) 0.2431(6) 0.5026(4) 0.0253(15) Uani 0.247(4) 1 d P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0356(8) 0.0395(8) 0.0436(10) 0.0008(7) 0.0138(8) 0.0018(7) Si2 0.0421(9) 0.0487(9) 0.0258(8) 0.0022(7) 0.0091(7) 0.0098(8) Si3 0.0426(9) 0.0387(9) 0.0433(10) 0.0000(7) 0.0145(8) 0.0033(7) Si4 0.0470(10) 0.0437(9) 0.0282(8) 0.0031(7) 0.0128(8) 0.0055(8) N1 0.023(2) 0.034(2) 0.027(2) 0.0035(19) 0.002(2) 0.000(2) N2 0.047(3) 0.027(2) 0.042(3) 0.002(2) 0.013(3) 0.001(2) N3 0.032(2) 0.036(2) 0.028(2) 0.0017(19) 0.011(2) 0.000(2) N4 0.042(3) 0.028(2) 0.039(3) -0.005(2) 0.013(2) -0.011(2) C1 0.056(4) 0.048(4) 0.051(4) -0.008(3) 0.019(3) 0.011(3) C2 0.062(4) 0.037(3) 0.086(6) -0.007(4) 0.028(4) -0.005(3) C3 0.059(4) 0.058(4) 0.064(5) 0.017(4) 0.029(4) 0.025(4) C4 0.088(6) 0.086(6) 0.073(6) 0.021(4) 0.050(5) 0.006(5) C5 0.068(5) 0.080(5) 0.040(4) -0.014(4) -0.004(4) 0.013(4) C6 0.084(5) 0.083(5) 0.051(4) -0.003(4) 0.027(4) 0.046(5) C7 0.037(3) 0.056(4) 0.072(4) 0.002(3) 0.028(3) -0.005(3) C8 0.052(5) 0.060(5) 0.116(8) 0.006(5) -0.010(5) 0.006(4) C9 0.096(6) 0.079(5) 0.090(6) -0.009(5) 0.063(6) 0.000(5) C10 0.058(4) 0.041(3) 0.054(4) -0.006(3) 0.010(3) -0.002(3) C11 0.086(6) 0.077(5) 0.069(5) -0.037(4) 0.034(5) -0.034(5) C12 0.086(5) 0.034(3) 0.076(5) 0.010(3) 0.024(5) 0.008(4) C13 0.087(5) 0.042(4) 0.079(5) 0.009(4) 0.046(5) 0.020(4) C14 0.062(5) 0.045(4) 0.083(6) -0.009(4) 0.019(4) -0.009(4) C15 0.075(5) 0.061(4) 0.058(5) 0.011(4) 0.008(4) 0.024(4) C16 0.113(7) 0.082(5) 0.074(6) 0.017(4) 0.075(6) 0.006(5) C17 0.076(5) 0.078(5) 0.041(4) -0.013(4) -0.010(4) 0.016(4) C18 0.068(4) 0.074(5) 0.040(4) 0.003(3) 0.022(4) 0.021(4) C19 0.044(3) 0.089(5) 0.061(4) 0.012(4) 0.022(3) -0.007(4) C20 0.044(4) 0.065(5) 0.090(6) -0.001(4) 0.011(4) -0.005(4) C21 0.061(4) 0.071(5) 0.086(6) -0.023(4) 0.044(4) -0.008(4) C22 0.052(3) 0.038(3) 0.046(3) -0.010(2) 0.012(3) -0.001(3) C23 0.071(5) 0.033(3) 0.068(5) 0.011(3) 0.030(4) 0.011(3) C24 0.081(5) 0.047(3) 0.062(5) -0.023(4) 0.028(4) -0.023(4) P1 0.0321(13) 0.0287(16) 0.0277(15) 0.0020(12) -0.0015(11) -0.0019(13) P2 0.0306(13) 0.0509(19) 0.0275(15) 0.0059(13) 0.0050(11) -0.0103(15) P3 0.0271(10) 0.0407(11) 0.0275(11) -0.0066(8) 0.0017(8) 0.0037(9) P4 0.0292(11) 0.0418(12) 0.0303(11) -0.0086(9) 0.0028(9) 0.0034(9) P5 0.0265(10) 0.0312(11) 0.0213(10) -0.0005(9) 0.0024(8) 0.0003(9) P6 0.0299(10) 0.0323(12) 0.0251(10) -0.0009(9) 0.0059(9) -0.0007(10) P1A 0.033(4) 0.037(5) 0.039(5) -0.008(4) 0.004(3) -0.001(4) P2A 0.040(5) 0.041(6) 0.030(5) -0.004(4) 0.008(4) -0.009(5) P3A 0.022(3) 0.032(3) 0.023(3) -0.007(2) -0.003(2) 0.006(2) P4A 0.022(3) 0.039(3) 0.024(3) -0.007(2) -0.001(2) 0.001(3) P5A 0.026(3) 0.022(3) 0.025(3) -0.001(2) 0.005(3) 0.002(3) P6A 0.021(3) 0.027(3) 0.025(3) -0.009(3) 0.005(3) 0.002(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Si1 N1 1.767(5) . ? Si1 C3 1.860(7) . ? Si1 C1 1.862(7) . ? Si1 C2 1.887(7) . ? Si1 P6A 2.724(6) . ? Si2 N1 1.762(5) . ? Si2 C5 1.848(7) . ? Si2 C4 1.852(8) . ? Si2 C6 1.867(7) . ? Si3 N3 1.764(5) . ? Si3 C14 1.841(7) . ? Si3 C13 1.856(8) . ? Si3 C15 1.863(7) . ? Si4 N3 1.763(5) . ? Si4 C18 1.852(7) . ? Si4 C16 1.868(8) . ? Si4 C17 1.874(8) . ? N1 P6A 1.717(7) . ? N1 P5 1.767(5) . ? N2 C10 1.483(7) . ? N2 C7 1.522(8) . ? N2 P5 1.621(5) . ? N2 P6A 1.724(7) . ? N3 P6 1.722(5) . ? N3 P5A 1.838(7) . ? N4 C19 1.422(8) . ? N4 C22 1.524(7) . ? N4 P5A 1.531(7) . ? N4 P6 1.717(5) . ? C7 C9 1.494(10) . ? C7 C8 1.513(10) . ? C7 P6A 2.349(8) . ? C10 C11 1.482(9) . ? C10 C12 1.569(9) . ? C19 C21 1.504(9) . ? C19 C20 1.523(10) . ? C22 C23 1.507(8) . ? C22 C24 1.557(9) . ? C22 P5A 2.187(8) . ? P1 P2 2.165(5) . ? P1 P3 2.203(4) . ? P1 P4 2.209(4) . ? P2 P4 2.209(4) . ? P2 P3 2.209(4) . ? P3 P5 2.237(3) . ? P4 P6 2.247(3) . ? P1A P2A 2.120(16) . ? P1A P4A 2.256(11) . ? P1A P3A 2.269(11) . ? P2A P4A 2.213(13) . ? P2A P3A 2.222(11) . ? P3A P6A 2.255(8) . ? P4A P5A 2.258(9) . ? 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 N1 Si1 C3 109.9(3) . . ? N1 Si1 C1 117.0(3) . . ? C3 Si1 C1 102.8(3) . . ? N1 Si1 C2 110.2(3) . . ? C3 Si1 C2 110.7(3) . . ? C1 Si1 C2 106.0(3) . . ? N1 Si1 P6A 37.9(2) . . ? C3 Si1 P6A 137.1(3) . . ? C1 Si1 P6A 82.5(3) . . ? C2 Si1 P6A 108.5(3) . . ? N1 Si2 C5 111.1(3) . . ? N1 Si2 C4 112.4(3) . . ? C5 Si2 C4 108.7(4) . . ? N1 Si2 C6 112.7(3) . . ? C5 Si2 C6 108.1(4) . . ? C4 Si2 C6 103.5(4) . . ? N3 Si3 C14 111.0(3) . . ? N3 Si3 C13 114.4(3) . . ? C14 Si3 C13 106.9(4) . . ? N3 Si3 C15 110.7(3) . . ? C14 Si3 C15 108.1(4) . . ? C13 Si3 C15 105.4(4) . . ? N3 Si4 C18 113.9(3) . . ? N3 Si4 C16 110.4(3) . . ? C18 Si4 C16 104.1(4) . . ? N3 Si4 C17 110.5(3) . . ? C18 Si4 C17 108.4(4) . . ? C16 Si4 C17 109.3(4) . . ? P6A N1 Si2 139.4(4) . . ? P6A N1 Si1 102.9(4) . . ? Si2 N1 Si1 117.4(3) . . ? P6A N1 P5 30.3(2) . . ? Si2 N1 P5 109.1(3) . . ? Si1 N1 P5 132.9(3) . . ? C10 N2 C7 114.2(5) . . ? C10 N2 P5 122.3(4) . . ? C7 N2 P5 123.4(4) . . ? C10 N2 P6A 153.0(5) . . ? C7 N2 P6A 92.5(4) . . ? P5 N2 P6A 31.5(2) . . ? P6 N3 Si4 132.3(3) . . ? P6 N3 Si3 109.1(3) . . ? Si4 N3 Si3 118.6(3) . . ? P6 N3 P5A 29.5(2) . . ? Si4 N3 P5A 102.8(3) . . ? Si3 N3 P5A 138.3(4) . . ? C19 N4 C22 119.6(5) . . ? C19 N4 P5A 148.9(6) . . ? C22 N4 P5A 91.4(5) . . ? C19 N4 P6 117.7(5) . . ? C22 N4 P6 122.1(4) . . ? P5A N4 P6 32.0(3) . . ? C9 C7 C8 114.3(7) . . ? C9 C7 N2 112.7(6) . . ? C8 C7 N2 109.3(6) . . ? C9 C7 P6A 121.6(5) . . ? C8 C7 P6A 124.1(6) . . ? N2 C7 P6A 47.2(3) . . ? C11 C10 N2 114.2(6) . . ? C11 C10 C12 109.7(6) . . ? N2 C10 C12 109.1(5) . . ? N4 C19 C21 114.9(6) . . ? N4 C19 C20 115.3(6) . . ? C21 C19 C20 112.2(7) . . ? C23 C22 N4 111.4(5) . . ? C23 C22 C24 111.1(5) . . ? N4 C22 C24 109.4(5) . . ? C23 C22 P5A 123.6(4) . . ? N4 C22 P5A 44.4(3) . . ? C24 C22 P5A 124.6(4) . . ? P2 P1 P3 60.77(13) . . ? P2 P1 P4 60.65(12) . . ? P3 P1 P4 80.30(13) . . ? P1 P2 P4 60.67(13) . . ? P1 P2 P3 60.48(14) . . ? P4 P2 P3 80.18(13) . . ? P1 P3 P2 58.75(14) . . ? P1 P3 P5 95.65(13) . . ? P2 P3 P5 96.29(13) . . ? P2 P4 P1 58.68(14) . . ? P2 P4 P6 95.58(13) . . ? P1 P4 P6 96.28(13) . . ? N2 P5 N1 111.1(2) . . ? N2 P5 P3 101.9(2) . . ? N1 P5 P3 100.72(19) . . ? N4 P6 N3 110.9(3) . . ? N4 P6 P4 102.9(2) . . ? N3 P6 P4 102.1(2) . . ? P2A P1A P4A 60.7(4) . . ? P2A P1A P3A 60.7(4) . . ? P4A P1A P3A 77.4(4) . . ? P1A P2A P4A 62.7(5) . . ? P1A P2A P3A 63.0(4) . . ? P4A P2A P3A 79.2(4) . . ? P2A P3A P6A 95.5(4) . . ? P2A P3A P1A 56.3(4) . . ? P6A P3A P1A 95.4(4) . . ? P2A P4A P1A 56.6(4) . . ? P2A P4A P5A 94.6(4) . . ? P1A P4A P5A 93.1(4) . . ? N4 P5A N3 114.2(4) . . ? N4 P5A C22 44.2(3) . . ? N3 P5A C22 136.1(4) . . ? N4 P5A P4A 103.0(4) . . ? N3 P5A P4A 97.5(4) . . ? C22 P5A P4A 122.3(3) . . ? N1 P6A N2 108.7(4) . . ? N1 P6A P3A 99.4(4) . . ? N2 P6A P3A 107.4(4) . . ? N1 P6A C7 111.9(3) . . ? N2 P6A C7 40.4(3) . . ? P3A P6A C7 140.3(4) . . ? N1 P6A Si1 39.2(2) . . ? N2 P6A Si1 126.6(3) . . ? P3A P6A Si1 117.5(3) . . ? C7 P6A Si1 102.2(3) . . ? #===END