# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Peter Portius' 'Martin Davis' _publ_contact_author_name 'Peter Portius' _publ_contact_author_email PETER.PORTIUS@SHEFFIELD.AC.UK _publ_section_title ; A new Hexakis(isocyanato)silicate(IV) and the first isolated Lewis-Base Adducts of Silicontetraisocyanate ; # Attachment 'ch1ppx55m.cif' data_chppx55m _database_code_depnum_ccdc_archive 'CCDC 737982' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H12 K2 N10 O6 Si' _chemical_formula_sum 'C14 H12 K2 N10 O6 Si' _chemical_formula_weight 522.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 8.427(3) _cell_length_b 12.522(4) _cell_length_c 11.404(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.948(4) _cell_angle_gamma 90.00 _cell_volume 1172.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2797 _cell_measurement_theta_min 3.399 _cell_measurement_theta_max 26.16 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 0.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8547 _exptl_absorpt_correction_T_max 0.8754 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6946 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.40 _diffrn_reflns_theta_max 26.80 _reflns_number_total 2291 _reflns_number_gt 1713 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0485P)^2^+3.0619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2291 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1018 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1395 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 K1 K 0.65538(11) 0.01626(7) 0.41452(8) 0.0218(3) Uani 1 1 d . . . Si1 Si 1.0000 0.0000 1.0000 0.0170(4) Uani 1 2 d S . . O2 O 0.6107(4) -0.0035(3) 0.1690(3) 0.0348(8) Uani 1 1 d . . . O3 O 0.6907(4) -0.0203(3) 0.6603(3) 0.0441(10) Uani 1 1 d . . . O1 O 0.5009(4) -0.1691(3) 0.4675(3) 0.0410(9) Uani 1 1 d . . . N3 N 0.8683(4) 0.0002(3) 0.8483(3) 0.0270(9) Uani 1 1 d . . . N1 N 0.5109(4) -0.3547(3) 0.4972(4) 0.0283(9) Uani 1 1 d . . . C3 C 0.7817(5) -0.0103(4) 0.7569(4) 0.0229(10) Uani 1 1 d . . . N2 N 0.8206(4) -0.0078(3) 0.0627(3) 0.0284(9) Uani 1 1 d . . . N4 N 0.7924(5) 0.2063(3) 0.3542(4) 0.0404(11) Uani 1 1 d . . . C1 C 0.5067(5) -0.2634(4) 0.4826(4) 0.0221(10) Uani 1 1 d . . . C4 C 0.9183(5) 0.2361(4) 0.3510(4) 0.0272(10) Uani 1 1 d . . . C2 C 0.7192(5) -0.0057(3) 0.1164(3) 0.0211(9) Uani 1 1 d . . . N5 N 0.9119(6) -0.1133(4) 0.3927(4) 0.0584(15) Uani 1 1 d . . . C6 C 0.9853(6) -0.1779(4) 0.3606(4) 0.0323(11) Uani 1 1 d . . . C5 C 1.0815(5) 0.2743(4) 0.3495(5) 0.0364(12) Uani 1 1 d . . . H5A H 1.1150 0.3280 0.4128 0.055 Uiso 1 1 calc R . . H5B H 1.0811 0.3062 0.2710 0.055 Uiso 1 1 calc R . . H5C H 1.1580 0.2142 0.3639 0.055 Uiso 1 1 calc R . . C7 C 1.0806(5) -0.2607(4) 0.3219(4) 0.0373(12) Uani 1 1 d . . . H12A H 1.1932 -0.2565 0.3686 0.056 Uiso 1 1 calc R . . H12B H 1.0785 -0.2514 0.2363 0.056 Uiso 1 1 calc R . . H12C H 1.0349 -0.3306 0.3345 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 K1 0.0267(5) 0.0180(5) 0.0230(5) 0.0008(4) 0.0101(4) 0.0005(4) Si1 0.0155(7) 0.0164(9) 0.0193(8) -0.0011(7) 0.0042(6) -0.0024(6) O2 0.0251(15) 0.048(2) 0.0357(18) -0.0060(17) 0.0168(14) -0.0035(15) O3 0.0302(17) 0.078(3) 0.0211(17) 0.0038(18) -0.0008(15) -0.0017(18) O1 0.054(2) 0.019(2) 0.058(2) -0.0041(17) 0.030(2) -0.0060(16) N3 0.0230(18) 0.034(2) 0.0220(19) 0.0022(18) 0.0000(15) -0.0013(16) N1 0.032(2) 0.017(2) 0.036(2) 0.0002(18) 0.0069(16) 0.0019(16) C3 0.019(2) 0.028(3) 0.024(2) 0.001(2) 0.0106(19) 0.0016(19) N2 0.0235(18) 0.033(2) 0.030(2) 0.0027(18) 0.0097(16) -0.0027(17) N4 0.028(2) 0.038(3) 0.050(3) 0.010(2) -0.0005(19) -0.0086(19) C1 0.019(2) 0.026(3) 0.023(2) -0.006(2) 0.0097(17) -0.0032(18) C4 0.027(2) 0.025(3) 0.026(2) 0.004(2) -0.0011(19) 0.001(2) C2 0.023(2) 0.026(3) 0.0141(19) 0.0017(19) 0.0036(17) -0.0031(18) N5 0.072(3) 0.064(4) 0.037(3) 0.000(3) 0.008(2) 0.040(3) C6 0.030(2) 0.044(3) 0.022(2) 0.002(2) 0.003(2) 0.004(2) C5 0.027(2) 0.038(3) 0.046(3) 0.004(2) 0.011(2) -0.002(2) C7 0.024(2) 0.048(3) 0.038(3) -0.013(3) 0.004(2) 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 K1 O2 2.752(3) . ? K1 N5 2.758(5) . ? K1 O3 2.789(3) . ? K1 O1 2.793(3) . ? K1 N4 2.798(4) . ? K1 O1 2.829(3) 3_656 ? K1 O3 2.850(3) 3_656 ? Si1 N2 1.814(3) 1_556 ? Si1 N2 1.814(3) 3_756 ? Si1 N1 1.822(4) 4_656 ? Si1 N1 1.822(4) 2_656 ? Si1 N3 1.834(4) 3_757 ? Si1 N3 1.834(4) . ? O2 C2 1.201(5) . ? O3 C3 1.200(5) . ? O3 K1 2.850(3) 3_656 ? O1 C1 1.192(6) . ? O1 K1 2.829(3) 3_656 ? N3 C3 1.139(5) . ? N1 C1 1.155(6) . ? N1 Si1 1.822(4) 2_646 ? N2 C2 1.157(5) . ? N2 Si1 1.814(3) 1_554 ? N4 C4 1.133(6) . ? C4 C5 1.460(6) . ? N5 C6 1.128(6) . ? C6 C7 1.440(7) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 H12A 0.9800 . ? C7 H12B 0.9800 . ? C7 H12C 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 O2 K1 N5 77.67(12) . . ? O2 K1 O3 165.30(11) . . ? N5 K1 O3 94.85(12) . . ? O2 K1 O1 100.46(10) . . ? N5 K1 O1 86.74(15) . . ? O3 K1 O1 66.17(11) . . ? O2 K1 N4 78.23(12) . . ? N5 K1 N4 95.93(16) . . ? O3 K1 N4 115.46(12) . . ? O1 K1 N4 176.66(12) . . ? O2 K1 O1 124.93(11) . 3_656 ? N5 K1 O1 154.00(13) . 3_656 ? O3 K1 O1 65.78(11) . 3_656 ? O1 K1 O1 99.81(10) . 3_656 ? N4 K1 O1 78.64(12) . 3_656 ? O2 K1 O3 78.45(9) . 3_656 ? N5 K1 O3 138.91(15) . 3_656 ? O3 K1 O3 100.10(8) . 3_656 ? O1 K1 O3 65.44(11) . 3_656 ? N4 K1 O3 111.23(12) . 3_656 ? O1 K1 O3 64.90(11) 3_656 3_656 ? O2 K1 K1 125.97(8) . 3_656 ? N5 K1 K1 131.17(12) . 3_656 ? O3 K1 K1 50.79(7) . 3_656 ? O1 K1 K1 50.34(7) . 3_656 ? N4 K1 K1 128.04(10) . 3_656 ? O1 K1 K1 49.47(7) 3_656 3_656 ? O3 K1 K1 49.31(7) 3_656 3_656 ? N2 Si1 N2 180.000(1) 1_556 3_756 ? N2 Si1 N1 90.18(17) 1_556 4_656 ? N2 Si1 N1 89.82(17) 3_756 4_656 ? N2 Si1 N1 89.82(17) 1_556 2_656 ? N2 Si1 N1 90.18(17) 3_756 2_656 ? N1 Si1 N1 180.0(3) 4_656 2_656 ? N2 Si1 N3 90.56(16) 1_556 3_757 ? N2 Si1 N3 89.44(16) 3_756 3_757 ? N1 Si1 N3 89.60(17) 4_656 3_757 ? N1 Si1 N3 90.40(17) 2_656 3_757 ? N2 Si1 N3 89.44(16) 1_556 . ? N2 Si1 N3 90.56(16) 3_756 . ? N1 Si1 N3 90.40(17) 4_656 . ? N1 Si1 N3 89.60(17) 2_656 . ? N3 Si1 N3 180.000(1) 3_757 . ? C2 O2 K1 124.4(3) . . ? C3 O3 K1 143.9(3) . . ? C3 O3 K1 132.3(3) . 3_656 ? K1 O3 K1 79.90(8) . 3_656 ? C1 O1 K1 148.0(3) . . ? C1 O1 K1 127.6(3) . 3_656 ? K1 O1 K1 80.19(10) . 3_656 ? C3 N3 Si1 172.7(4) . . ? C1 N1 Si1 172.3(4) . 2_646 ? N3 C3 O3 179.3(5) . . ? C2 N2 Si1 170.5(4) . 1_554 ? C4 N4 K1 136.8(4) . . ? N1 C1 O1 179.4(4) . . ? N4 C4 C5 178.8(5) . . ? N2 C2 O2 178.1(4) . . ? C6 N5 K1 161.6(5) . . ? N5 C6 C7 178.9(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C6 C7 H12A 109.5 . . ? C6 C7 H12B 109.5 . . ? H12A C7 H12B 109.5 . . ? C6 C7 H12C 109.5 . . ? H12A C7 H12C 109.5 . . ? H12B C7 H12C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.913 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.542 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.090 # Attachment 'ch1ppx69_0m.cif' data_ch1ppx69_0m _database_code_depnum_ccdc_archive 'CCDC 737983' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H30 N P2), C6 N6 O6 Si1' _chemical_formula_sum 'C78 H60 N8 O6 P4 Si' _chemical_formula_weight 1357.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6037(5) _cell_length_b 12.9974(5) _cell_length_c 13.4729(6) _cell_angle_alpha 63.885(2) _cell_angle_beta 70.577(2) _cell_angle_gamma 75.503(2) _cell_volume 1707.67(12) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9886 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.20 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 706 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9471 _exptl_absorpt_correction_T_max 0.9595 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34308 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7811 _reflns_number_gt 6570 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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. The residual electron density (1.317) was found to be 0.71 Angstroms from O2. DFIX Restraints were applied to atoms N2 C2 and C2 O2 and refinement converged successfully. ; _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^)+(0.0498P)^2^+1.1541P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7811 _refine_ls_number_parameters 440 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1118 _refine_ls_wR_factor_gt 0.1046 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Si1 Si 0.0000 1.0000 0.0000 0.02593(16) Uani 1 2 d S . . P1 P 0.19131(4) 0.30352(3) 0.26845(4) 0.01753(10) Uani 1 1 d . . . P2 P 0.36555(4) 0.40965(3) 0.30098(3) 0.01587(10) Uani 1 1 d . . . N1 N 0.04729(15) 0.84553(14) 0.07263(15) 0.0327(4) Uani 1 1 d . . . N2 N -0.02516(15) 1.02014(14) 0.13406(10) 0.0345(4) Uani 1 1 d D . . N3 N 0.16025(14) 1.02722(15) -0.04307(16) 0.0351(4) Uani 1 1 d . . . N4 N 0.24460(12) 0.39925(12) 0.27821(12) 0.0198(3) Uani 1 1 d . . . O1 O 0.04718(15) 0.64924(12) 0.19769(14) 0.0452(4) Uani 1 1 d . . . O2 O -0.0564(2) 0.96685(19) 0.33178(10) 0.0811(7) Uani 1 1 d D . . O3 O 0.33921(13) 1.06520(13) -0.02469(15) 0.0443(4) Uani 1 1 d . . . C1 C 0.04622(16) 0.74906(16) 0.13546(17) 0.0276(4) Uani 1 1 d . . . C2 C -0.0428(2) 0.99279(17) 0.23222(10) 0.0389(5) Uani 1 1 d D . . C3 C 0.24770(16) 1.04556(15) -0.03170(16) 0.0280(4) Uani 1 1 d . . . C4 C 0.17353(15) 0.35139(14) 0.12660(14) 0.0205(3) Uani 1 1 d . . . C5 C 0.19124(15) 0.46389(15) 0.04856(14) 0.0234(3) Uani 1 1 d . . . H5 H 0.2166 0.5145 0.0688 0.028 Uiso 1 1 calc R . . C6 C 0.17154(16) 0.50194(17) -0.05949(15) 0.0290(4) Uani 1 1 d . . . H6 H 0.1833 0.5787 -0.1129 0.035 Uiso 1 1 calc R . . C7 C 0.13483(17) 0.42783(18) -0.08911(17) 0.0329(4) Uani 1 1 d . . . H7 H 0.1223 0.4538 -0.1630 0.040 Uiso 1 1 calc R . . C8 C 0.11635(18) 0.31594(18) -0.01121(18) 0.0344(4) Uani 1 1 d . . . H8 H 0.0909 0.2657 -0.0319 0.041 Uiso 1 1 calc R . . C9 C 0.13492(17) 0.27725(16) 0.09653(17) 0.0293(4) Uani 1 1 d . . . H9 H 0.1216 0.2008 0.1500 0.035 Uiso 1 1 calc R . . C10 C 0.03900(15) 0.28493(14) 0.36265(14) 0.0217(3) Uani 1 1 d . . . C11 C -0.01050(17) 0.18216(16) 0.40452(18) 0.0325(4) Uani 1 1 d . . . H11 H 0.0383 0.1181 0.3885 0.039 Uiso 1 1 calc R . . C12 C -0.13183(18) 0.17362(19) 0.4700(2) 0.0415(5) Uani 1 1 d . . . H12 H -0.1656 0.1034 0.4994 0.050 Uiso 1 1 calc R . . C13 C -0.20308(17) 0.26736(19) 0.49228(18) 0.0379(5) Uani 1 1 d . . . H13 H -0.2858 0.2612 0.5371 0.045 Uiso 1 1 calc R . . C14 C -0.15474(17) 0.37023(18) 0.44972(17) 0.0349(4) Uani 1 1 d . . . H14 H -0.2047 0.4345 0.4648 0.042 Uiso 1 1 calc R . . C15 C -0.03356(16) 0.37989(16) 0.38510(15) 0.0270(4) Uani 1 1 d . . . H15 H -0.0002 0.4503 0.3564 0.032 Uiso 1 1 calc R . . C16 C 0.28510(14) 0.16518(13) 0.30269(14) 0.0197(3) Uani 1 1 d . . . C21 C 0.36531(17) 0.12816(16) 0.21757(16) 0.0276(4) Uani 1 1 d . . . H21 H 0.3617 0.1699 0.1402 0.033 Uiso 1 1 calc R . . C20 C 0.45023(18) 0.03011(17) 0.24656(19) 0.0351(4) Uani 1 1 d . . . H20 H 0.5038 0.0044 0.1891 0.042 Uiso 1 1 calc R . . C19 C 0.45672(18) -0.02997(16) 0.35905(19) 0.0354(5) Uani 1 1 d . . . H19 H 0.5161 -0.0958 0.3782 0.042 Uiso 1 1 calc R . . C18 C 0.37686(18) 0.00552(16) 0.44393(18) 0.0313(4) Uani 1 1 d . . . H18 H 0.3814 -0.0364 0.5210 0.038 Uiso 1 1 calc R . . C17 C 0.29037(16) 0.10209(14) 0.41650(15) 0.0240(4) Uani 1 1 d . . . H17 H 0.2348 0.1253 0.4750 0.029 Uiso 1 1 calc R . . C22 C 0.35121(15) 0.36343(13) 0.45169(13) 0.0185(3) Uani 1 1 d . . . C23 C 0.24970(16) 0.30930(15) 0.53244(15) 0.0242(4) Uani 1 1 d . . . H23 H 0.1875 0.2985 0.5078 0.029 Uiso 1 1 calc R . . C24 C 0.23941(18) 0.27119(17) 0.64867(15) 0.0305(4) Uani 1 1 d . . . H24 H 0.1709 0.2333 0.7032 0.037 Uiso 1 1 calc R . . C25 C 0.32889(18) 0.28836(16) 0.68517(15) 0.0295(4) Uani 1 1 d . . . H25 H 0.3217 0.2619 0.7646 0.035 Uiso 1 1 calc R . . C26 C 0.42918(17) 0.34424(15) 0.60584(15) 0.0252(4) Uani 1 1 d . . . H26 H 0.4898 0.3567 0.6312 0.030 Uiso 1 1 calc R . . C27 C 0.44061(15) 0.38184(14) 0.48945(14) 0.0209(3) Uani 1 1 d . . . H27 H 0.5090 0.4201 0.4353 0.025 Uiso 1 1 calc R . . C28 C 0.39065(15) 0.55890(13) 0.23677(13) 0.0179(3) Uani 1 1 d . . . C29 C 0.29125(15) 0.64149(15) 0.25535(15) 0.0228(3) Uani 1 1 d . . . H29 H 0.2125 0.6183 0.3006 0.027 Uiso 1 1 calc R . . C30 C 0.30849(17) 0.75740(15) 0.20721(16) 0.0276(4) Uani 1 1 d . . . H30 H 0.2412 0.8134 0.2196 0.033 Uiso 1 1 calc R . . C31 C 0.42378(17) 0.79198(15) 0.14097(15) 0.0269(4) Uani 1 1 d . . . H31 H 0.4349 0.8713 0.1079 0.032 Uiso 1 1 calc R . . C32 C 0.52237(16) 0.71020(15) 0.12336(14) 0.0239(4) Uani 1 1 d . . . H32 H 0.6011 0.7337 0.0785 0.029 Uiso 1 1 calc R . . C33 C 0.50633(15) 0.59379(14) 0.17120(14) 0.0208(3) Uani 1 1 d . . . H33 H 0.5741 0.5381 0.1592 0.025 Uiso 1 1 calc R . . C34 C 0.50304(14) 0.33274(13) 0.24089(14) 0.0182(3) Uani 1 1 d . . . C35 C 0.52368(15) 0.35012(15) 0.12614(14) 0.0218(3) Uani 1 1 d . . . H35 H 0.4661 0.4003 0.0840 0.026 Uiso 1 1 calc R . . C36 C 0.62811(16) 0.29419(15) 0.07406(15) 0.0251(4) Uani 1 1 d . . . H36 H 0.6418 0.3062 -0.0036 0.030 Uiso 1 1 calc R . . C37 C 0.71231(17) 0.22086(16) 0.13533(16) 0.0293(4) Uani 1 1 d . . . H37 H 0.7834 0.1824 0.0997 0.035 Uiso 1 1 calc R . . C38 C 0.69292(18) 0.20358(16) 0.24856(16) 0.0321(4) Uani 1 1 d . . . H38 H 0.7512 0.1537 0.2901 0.039 Uiso 1 1 calc R . . C39 C 0.58810(16) 0.25918(15) 0.30190(15) 0.0255(4) Uani 1 1 d . . . H39 H 0.5749 0.2468 0.3796 0.031 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 Si1 0.0187(3) 0.0229(3) 0.0350(4) -0.0122(3) -0.0049(3) -0.0014(3) P1 0.01709(19) 0.0169(2) 0.0200(2) -0.00753(16) -0.00591(16) -0.00220(15) P2 0.01621(19) 0.0162(2) 0.0161(2) -0.00680(16) -0.00464(15) -0.00189(15) N1 0.0316(8) 0.0236(8) 0.0407(9) -0.0117(7) -0.0105(7) 0.0003(6) N2 0.0333(9) 0.0345(9) 0.0363(10) -0.0172(8) -0.0079(7) -0.0004(7) N3 0.0221(8) 0.0343(9) 0.0475(10) -0.0164(8) -0.0054(7) -0.0049(7) N4 0.0201(7) 0.0182(7) 0.0240(7) -0.0091(6) -0.0087(6) -0.0012(5) O1 0.0489(9) 0.0281(8) 0.0554(10) -0.0017(7) -0.0292(8) -0.0055(7) O2 0.141(2) 0.0795(14) 0.0251(9) -0.0245(9) -0.0035(10) -0.0342(14) O3 0.0306(8) 0.0329(8) 0.0692(11) -0.0125(8) -0.0190(7) -0.0090(6) C1 0.0216(8) 0.0315(10) 0.0351(10) -0.0165(9) -0.0115(7) 0.0002(7) C2 0.0405(11) 0.0329(11) 0.0477(13) -0.0170(10) -0.0203(10) 0.0028(9) C3 0.0243(9) 0.0179(8) 0.0335(10) -0.0052(7) -0.0044(7) -0.0023(7) C4 0.0187(8) 0.0233(8) 0.0220(8) -0.0107(7) -0.0076(6) 0.0000(6) C5 0.0192(8) 0.0276(9) 0.0234(8) -0.0105(7) -0.0050(6) -0.0025(7) C6 0.0231(9) 0.0338(10) 0.0231(9) -0.0073(8) -0.0050(7) -0.0001(7) C7 0.0281(9) 0.0466(12) 0.0273(10) -0.0183(9) -0.0140(8) 0.0066(8) C8 0.0350(10) 0.0400(11) 0.0428(11) -0.0254(10) -0.0221(9) 0.0052(8) C9 0.0321(10) 0.0268(9) 0.0354(10) -0.0132(8) -0.0170(8) -0.0014(7) C10 0.0187(8) 0.0229(8) 0.0228(8) -0.0077(7) -0.0055(6) -0.0033(6) C11 0.0225(9) 0.0261(9) 0.0472(12) -0.0133(9) -0.0060(8) -0.0060(7) C12 0.0261(10) 0.0355(11) 0.0559(14) -0.0106(10) -0.0052(9) -0.0130(8) C13 0.0199(9) 0.0484(12) 0.0387(11) -0.0141(10) -0.0015(8) -0.0066(8) C14 0.0255(9) 0.0395(11) 0.0365(11) -0.0186(9) -0.0024(8) 0.0012(8) C15 0.0265(9) 0.0260(9) 0.0268(9) -0.0105(8) -0.0049(7) -0.0028(7) C16 0.0180(7) 0.0159(7) 0.0264(8) -0.0079(7) -0.0075(6) -0.0024(6) C21 0.0281(9) 0.0256(9) 0.0301(9) -0.0132(8) -0.0063(7) -0.0019(7) C20 0.0284(9) 0.0301(10) 0.0483(12) -0.0230(9) -0.0051(9) 0.0021(8) C19 0.0282(9) 0.0210(9) 0.0538(13) -0.0121(9) -0.0147(9) 0.0035(7) C18 0.0325(10) 0.0199(9) 0.0374(11) -0.0027(8) -0.0152(8) -0.0043(7) C17 0.0244(8) 0.0202(8) 0.0269(9) -0.0068(7) -0.0072(7) -0.0053(7) C22 0.0219(8) 0.0169(7) 0.0163(7) -0.0070(6) -0.0052(6) -0.0004(6) C23 0.0232(8) 0.0277(9) 0.0232(9) -0.0115(7) -0.0037(7) -0.0056(7) C24 0.0315(9) 0.0361(10) 0.0203(9) -0.0102(8) 0.0016(7) -0.0110(8) C25 0.0396(10) 0.0307(10) 0.0181(8) -0.0099(7) -0.0072(7) -0.0037(8) C26 0.0311(9) 0.0255(9) 0.0239(9) -0.0118(7) -0.0115(7) -0.0020(7) C27 0.0228(8) 0.0194(8) 0.0204(8) -0.0077(7) -0.0048(6) -0.0037(6) C28 0.0214(8) 0.0177(7) 0.0173(7) -0.0066(6) -0.0077(6) -0.0039(6) C29 0.0212(8) 0.0233(8) 0.0253(9) -0.0105(7) -0.0070(7) -0.0018(6) C30 0.0305(9) 0.0201(8) 0.0349(10) -0.0118(8) -0.0138(8) 0.0019(7) C31 0.0391(10) 0.0176(8) 0.0272(9) -0.0049(7) -0.0159(8) -0.0063(7) C32 0.0277(9) 0.0271(9) 0.0196(8) -0.0064(7) -0.0080(7) -0.0105(7) C33 0.0213(8) 0.0234(8) 0.0193(8) -0.0084(7) -0.0064(6) -0.0036(6) C34 0.0185(7) 0.0167(7) 0.0198(8) -0.0082(6) -0.0039(6) -0.0024(6) C35 0.0221(8) 0.0242(8) 0.0207(8) -0.0093(7) -0.0065(6) -0.0033(6) C36 0.0278(9) 0.0293(9) 0.0213(8) -0.0142(7) -0.0026(7) -0.0055(7) C37 0.0266(9) 0.0270(9) 0.0294(9) -0.0140(8) -0.0014(7) 0.0027(7) C38 0.0298(9) 0.0288(10) 0.0280(10) -0.0087(8) -0.0089(8) 0.0100(8) C39 0.0275(9) 0.0249(9) 0.0194(8) -0.0076(7) -0.0056(7) 0.0021(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N3 1.8305(16) . ? Si1 N3 1.8305(16) 2_575 ? Si1 N1 1.8345(16) . ? Si1 N1 1.8345(16) 2_575 ? Si1 N2 1.8556(12) 2_575 ? Si1 N2 1.8556(12) . ? P1 N4 1.5910(14) . ? P1 C4 1.7982(17) . ? P1 C10 1.8013(17) . ? P1 C16 1.8040(16) . ? P2 N4 1.5811(14) . ? P2 C28 1.7984(16) . ? P2 C34 1.8042(16) . ? P2 C22 1.8064(16) . ? N1 C1 1.164(2) . ? N2 C2 1.1661(17) . ? N3 C3 1.169(2) . ? O1 C1 1.195(2) . ? O2 C2 1.1940(18) . ? O3 C3 1.194(2) . ? C4 C5 1.392(2) . ? C4 C9 1.405(2) . ? C5 C6 1.395(2) . ? C5 H5 0.9500 . ? C6 C7 1.388(3) . ? C6 H6 0.9500 . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 C9 1.385(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.392(2) . ? C10 C15 1.401(2) . ? C11 C12 1.392(3) . ? C11 H11 0.9500 . ? C12 C13 1.382(3) . ? C12 H12 0.9500 . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.389(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.399(2) . ? C16 C21 1.402(2) . ? C21 C20 1.392(3) . ? C21 H21 0.9500 . ? C20 C19 1.385(3) . ? C20 H20 0.9500 . ? C19 C18 1.387(3) . ? C19 H19 0.9500 . ? C18 C17 1.388(2) . ? C18 H18 0.9500 . ? C17 H17 0.9500 . ? C22 C23 1.398(2) . ? C22 C27 1.405(2) . ? C23 C24 1.391(2) . ? C23 H23 0.9500 . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 C26 1.392(3) . ? C25 H25 0.9500 . ? C26 C27 1.391(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.397(2) . ? C28 C29 1.404(2) . ? C29 C30 1.391(2) . ? C29 H29 0.9500 . ? C30 C31 1.394(3) . ? C30 H30 0.9500 . ? C31 C32 1.388(3) . ? C31 H31 0.9500 . ? C32 C33 1.394(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.392(2) . ? C34 C35 1.404(2) . ? C35 C36 1.390(2) . ? C35 H35 0.9500 . ? C36 C37 1.386(3) . ? C36 H36 0.9500 . ? C37 C38 1.387(3) . ? C37 H37 0.9500 . ? C38 C39 1.398(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? 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 N3 Si1 N3 180.000(1) . 2_575 ? N3 Si1 N1 89.65(7) . . ? N3 Si1 N1 90.35(7) 2_575 . ? N3 Si1 N1 90.35(7) . 2_575 ? N3 Si1 N1 89.65(7) 2_575 2_575 ? N1 Si1 N1 180.0 . 2_575 ? N3 Si1 N2 89.75(8) . 2_575 ? N3 Si1 N2 90.25(8) 2_575 2_575 ? N1 Si1 N2 90.26(7) . 2_575 ? N1 Si1 N2 89.74(7) 2_575 2_575 ? N3 Si1 N2 90.25(8) . . ? N3 Si1 N2 89.75(8) 2_575 . ? N1 Si1 N2 89.74(7) . . ? N1 Si1 N2 90.26(7) 2_575 . ? N2 Si1 N2 180.00(10) 2_575 . ? N4 P1 C4 110.15(8) . . ? N4 P1 C10 109.35(8) . . ? C4 P1 C10 105.89(8) . . ? N4 P1 C16 113.67(7) . . ? C4 P1 C16 108.83(8) . . ? C10 P1 C16 108.65(8) . . ? N4 P2 C28 109.16(7) . . ? N4 P2 C34 114.00(7) . . ? C28 P2 C34 106.48(7) . . ? N4 P2 C22 111.82(8) . . ? C28 P2 C22 105.86(7) . . ? C34 P2 C22 109.06(7) . . ? C1 N1 Si1 162.35(16) . . ? C2 N2 Si1 156.63(17) . . ? C3 N3 Si1 155.37(17) . . ? P2 N4 P1 136.83(9) . . ? N1 C1 O1 178.3(2) . . ? N2 C2 O2 177.1(3) . . ? N3 C3 O3 177.3(2) . . ? C5 C4 C9 119.87(16) . . ? C5 C4 P1 120.13(12) . . ? C9 C4 P1 119.90(13) . . ? C4 C5 C6 119.72(16) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C7 C6 C5 120.11(18) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.26(17) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.23(18) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C4 119.81(18) . . ? C8 C9 H9 120.1 . . ? C4 C9 H9 120.1 . . ? C11 C10 C15 120.08(16) . . ? C11 C10 P1 121.21(13) . . ? C15 C10 P1 118.47(13) . . ? C10 C11 C12 119.77(18) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C13 C12 C11 120.00(19) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.46(18) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C15 120.27(18) . . ? C13 C14 H14 119.9 . . ? C15 C14 H14 119.9 . . ? C14 C15 C10 119.41(17) . . ? C14 C15 H15 120.3 . . ? C10 C15 H15 120.3 . . ? C17 C16 C21 119.48(15) . . ? C17 C16 P1 117.91(12) . . ? C21 C16 P1 121.92(13) . . ? C20 C21 C16 119.91(18) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? C19 C20 C21 120.11(18) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C19 C18 120.30(17) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C17 C18 C19 120.19(18) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C17 C16 119.99(17) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C23 C22 C27 119.15(15) . . ? C23 C22 P2 119.98(13) . . ? C27 C22 P2 120.86(12) . . ? C24 C23 C22 120.30(16) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C23 120.13(17) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 120.26(16) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 119.95(16) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C22 120.18(16) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C33 C28 C29 119.65(15) . . ? C33 C28 P2 121.72(12) . . ? C29 C28 P2 118.62(12) . . ? C30 C29 C28 119.72(16) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C31 120.46(16) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C32 C31 C30 119.85(16) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 120.25(16) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C28 120.07(15) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C39 C34 C35 119.45(15) . . ? C39 C34 P2 123.47(12) . . ? C35 C34 P2 117.08(12) . . ? C36 C35 C34 120.20(16) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 120.07(16) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C38 120.11(16) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C39 120.32(17) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C34 C39 C38 119.84(16) . . ? C34 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.320 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.056 # Attachment 'ch1ppx70_0n.cif' data_ch1ppx70_0n _database_code_depnum_ccdc_archive 'CCDC 737984' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H8 N6 O4 Si, C2 H3 N' _chemical_formula_sum 'C18 H11 N7 O4 Si' _chemical_formula_weight 417.43 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 6.9932(9) _cell_length_b 18.085(2) _cell_length_c 14.1246(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1786.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 2074 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 27.04 _exptl_crystal_description sheet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9521 _exptl_absorpt_correction_T_max 0.9929 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9835 _diffrn_reflns_av_R_equivalents 0.0464 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2129 _reflns_number_gt 1824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0499P)^2^+0.0291P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2129 _refine_ls_number_parameters 273 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0467 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.74497(13) 0.98308(4) 0.07612(6) 0.01996(18) Uani 1 1 d . . . O1 O 0.9965(4) 1.11185(12) -0.12840(17) 0.0396(6) Uani 1 1 d . . . O2 O 0.6724(7) 1.17369(15) 0.2283(2) 0.0936(15) Uani 1 1 d . . . O3 O 1.2098(4) 1.01558(15) 0.23571(17) 0.0377(6) Uani 1 1 d . . . O4 O 0.2697(4) 0.94817(13) -0.08445(17) 0.0368(6) Uani 1 1 d . . . N1 N 0.8277(4) 1.03364(13) -0.02370(18) 0.0261(6) Uani 1 1 d . . . N2 N 0.6936(4) 1.06010(13) 0.15093(18) 0.0265(6) Uani 1 1 d . . . N3 N 0.9848(4) 0.97105(12) 0.12362(17) 0.0231(6) Uani 1 1 d . . . N4 N 0.4999(4) 0.97998(12) 0.03167(18) 0.0248(6) Uani 1 1 d . . . N5 N 0.6607(4) 0.91359(13) 0.17638(15) 0.0193(5) Uani 1 1 d . . . N6 N 0.7874(4) 0.88855(13) 0.00752(17) 0.0201(5) Uani 1 1 d . . . N7 N 0.6940(5) 0.21322(17) -0.0030(2) 0.0422(8) Uani 1 1 d . . . C1 C 0.9120(5) 1.07256(15) -0.0746(2) 0.0249(7) Uani 1 1 d . . . C2 C 0.6841(6) 1.11665(17) 0.1879(2) 0.0383(9) Uani 1 1 d . . . C3 C 1.0938(5) 0.99370(15) 0.1811(2) 0.0233(6) Uani 1 1 d . . . C4 C 0.3881(5) 0.96417(15) -0.0272(2) 0.0233(7) Uani 1 1 d . . . C5 C 0.5927(5) 0.92958(16) 0.26193(19) 0.0239(7) Uani 1 1 d . . . H024 H 0.5770 0.9799 0.2794 0.029 Uiso 1 1 calc R . . C6 C 0.5437(5) 0.87430(16) 0.3271(2) 0.0240(7) Uani 1 1 d . . . H021 H 0.4952 0.8878 0.3875 0.029 Uiso 1 1 calc R . . C7 C 0.5649(5) 0.80120(15) 0.3047(2) 0.0223(6) Uani 1 1 d . . . H022 H 0.5340 0.7638 0.3494 0.027 Uiso 1 1 calc R . . C8 C 0.6338(5) 0.78258(15) 0.2136(2) 0.0206(6) Uani 1 1 d . . . C9 C 0.6535(4) 0.70856(15) 0.1787(2) 0.0217(6) Uani 1 1 d . . . H020 H 0.6242 0.6681 0.2191 0.026 Uiso 1 1 calc R . . C10 C 0.7139(4) 0.69512(16) 0.0880(2) 0.0225(7) Uani 1 1 d . . . H012 H 0.7239 0.6456 0.0662 0.027 Uiso 1 1 calc R . . C11 C 0.7622(4) 0.75486(16) 0.0258(2) 0.0205(6) Uani 1 1 d . . . C12 C 0.8234(5) 0.74652(17) -0.0691(2) 0.0239(7) Uani 1 1 d . . . H016 H 0.8341 0.6987 -0.0965 0.029 Uiso 1 1 calc R . . C13 C 0.8671(5) 0.80845(16) -0.1210(2) 0.0250(7) Uani 1 1 d . . . H017 H 0.9106 0.8035 -0.1844 0.030 Uiso 1 1 calc R . . C14 C 0.8479(5) 0.87919(16) -0.0808(2) 0.0241(7) Uani 1 1 d . . . H027 H 0.8789 0.9214 -0.1178 0.029 Uiso 1 1 calc R . . C15 C 0.7457(4) 0.82757(15) 0.05914(19) 0.0176(6) Uani 1 1 d . . . C16 C 0.6796(4) 0.84079(15) 0.15277(19) 0.0180(6) Uani 1 1 d . . . C17 C 0.7200(6) 0.3363(2) 0.0888(3) 0.0484(11) Uani 1 1 d . . . H11A H 0.8082 0.3696 0.0558 0.073 Uiso 1 1 calc R . . H11B H 0.7683 0.3264 0.1527 0.073 Uiso 1 1 calc R . . H11C H 0.5936 0.3594 0.0930 0.073 Uiso 1 1 calc R . . C18 C 0.7053(5) 0.26764(19) 0.0371(2) 0.0308(8) Uani 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 Si1 0.0279(4) 0.0139(3) 0.0180(3) 0.0003(3) 0.0003(3) -0.0001(3) O1 0.0428(16) 0.0338(13) 0.0424(13) 0.0117(11) 0.0072(12) -0.0069(12) O2 0.219(5) 0.0284(15) 0.0331(14) -0.0080(12) -0.011(2) 0.024(2) O3 0.0391(17) 0.0482(15) 0.0258(12) -0.0096(10) -0.0056(12) -0.0045(12) O4 0.0418(16) 0.0389(14) 0.0298(12) 0.0051(11) -0.0080(12) -0.0087(11) N1 0.0370(17) 0.0186(12) 0.0228(12) 0.0015(10) -0.0004(13) -0.0025(12) N2 0.0348(17) 0.0175(13) 0.0271(13) -0.0004(10) 0.0015(13) 0.0012(11) N3 0.0295(16) 0.0192(13) 0.0205(12) -0.0009(10) 0.0003(12) -0.0021(11) N4 0.0290(16) 0.0216(13) 0.0237(12) 0.0014(10) -0.0032(13) 0.0035(11) N5 0.0231(14) 0.0172(11) 0.0175(11) -0.0004(9) 0.0002(11) 0.0008(10) N6 0.0217(15) 0.0192(12) 0.0194(11) -0.0002(9) -0.0005(10) -0.0015(10) N7 0.053(2) 0.0345(17) 0.0386(16) -0.0031(13) -0.0062(16) 0.0005(15) C1 0.0311(19) 0.0175(14) 0.0262(14) -0.0013(13) -0.0043(15) 0.0016(13) C2 0.074(3) 0.0199(16) 0.0208(14) 0.0009(13) -0.0028(17) 0.0061(16) C3 0.0292(18) 0.0174(13) 0.0235(14) -0.0019(11) 0.0047(14) 0.0005(13) C4 0.0299(19) 0.0177(14) 0.0222(14) 0.0060(12) 0.0042(15) 0.0005(13) C5 0.0297(19) 0.0212(14) 0.0207(13) -0.0036(11) 0.0004(14) 0.0009(13) C6 0.0269(18) 0.0263(15) 0.0189(13) 0.0000(11) 0.0016(13) -0.0006(14) C7 0.0224(17) 0.0219(14) 0.0226(13) 0.0018(12) -0.0027(13) -0.0019(13) C8 0.0200(17) 0.0201(14) 0.0216(14) 0.0018(11) -0.0027(13) 0.0007(12) C9 0.0200(17) 0.0175(14) 0.0276(15) 0.0051(11) -0.0027(13) -0.0018(12) C10 0.0229(17) 0.0153(13) 0.0294(15) -0.0032(12) -0.0037(14) 0.0018(11) C11 0.0209(16) 0.0180(14) 0.0226(14) -0.0044(11) -0.0021(14) 0.0007(12) C12 0.0257(17) 0.0217(15) 0.0242(14) -0.0041(12) -0.0012(14) 0.0039(12) C13 0.0291(19) 0.0255(16) 0.0204(14) -0.0023(12) 0.0016(14) 0.0011(13) C14 0.0296(19) 0.0242(15) 0.0185(13) 0.0007(12) 0.0022(14) -0.0016(13) C15 0.0190(14) 0.0153(13) 0.0185(15) -0.0018(9) -0.0019(12) -0.0016(12) C16 0.0182(16) 0.0176(14) 0.0182(13) -0.0013(10) -0.0030(13) 0.0004(11) C17 0.064(3) 0.0320(19) 0.049(2) -0.0076(17) -0.004(2) 0.0006(18) C18 0.033(2) 0.0299(19) 0.0295(16) 0.0063(14) -0.0005(15) 0.0042(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.777(3) . ? Si1 N2 1.785(3) . ? Si1 N3 1.820(3) . ? Si1 N4 1.826(3) . ? Si1 N5 1.983(2) . ? Si1 N6 1.987(3) . ? O1 C1 1.197(4) . ? O2 C2 1.182(4) . ? O3 C3 1.187(4) . ? O4 C4 1.193(4) . ? N1 C1 1.166(4) . ? N2 C2 1.150(4) . ? N3 C3 1.186(4) . ? N4 C4 1.177(4) . ? N5 C5 1.330(3) . ? N5 C16 1.365(3) . ? N6 C14 1.329(4) . ? N6 C15 1.354(4) . ? N7 C18 1.138(4) . ? C5 C6 1.401(4) . ? C5 H024 0.9500 . ? C6 C7 1.367(4) . ? C6 H021 0.9500 . ? C7 C8 1.415(4) . ? C7 H022 0.9500 . ? C8 C16 1.396(4) . ? C8 C9 1.433(4) . ? C9 C10 1.370(4) . ? C9 H020 0.9500 . ? C10 C11 1.434(4) . ? C10 H012 0.9500 . ? C11 C15 1.402(4) . ? C11 C12 1.414(4) . ? C12 C13 1.374(4) . ? C12 H016 0.9500 . ? C13 C14 1.406(4) . ? C13 H017 0.9500 . ? C14 H027 0.9500 . ? C15 C16 1.421(4) . ? C17 C18 1.444(5) . ? C17 H11A 0.9800 . ? C17 H11B 0.9800 . ? C17 H11C 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 N1 Si1 N2 97.68(12) . . ? N1 Si1 N3 93.09(13) . . ? N2 Si1 N3 93.47(12) . . ? N1 Si1 N4 92.79(13) . . ? N2 Si1 N4 92.22(13) . . ? N3 Si1 N4 171.21(11) . . ? N1 Si1 N5 171.64(12) . . ? N2 Si1 N5 90.68(11) . . ? N3 Si1 N5 86.27(11) . . ? N4 Si1 N5 86.97(11) . . ? N1 Si1 N6 90.42(11) . . ? N2 Si1 N6 171.89(12) . . ? N3 Si1 N6 86.52(11) . . ? N4 Si1 N6 86.91(11) . . ? N5 Si1 N6 81.22(10) . . ? C1 N1 Si1 164.6(3) . . ? C2 N2 Si1 167.0(3) . . ? C3 N3 Si1 143.4(2) . . ? C4 N4 Si1 150.9(3) . . ? C5 N5 C16 117.8(2) . . ? C5 N5 Si1 128.1(2) . . ? C16 N5 Si1 114.08(18) . . ? C14 N6 C15 118.1(3) . . ? C14 N6 Si1 128.0(2) . . ? C15 N6 Si1 113.96(19) . . ? N1 C1 O1 178.6(3) . . ? N2 C2 O2 178.0(4) . . ? N3 C3 O3 176.9(3) . . ? N4 C4 O4 177.6(4) . . ? N5 C5 C6 121.9(3) . . ? N5 C5 H024 119.0 . . ? C6 C5 H024 119.0 . . ? C7 C6 C5 120.8(3) . . ? C7 C6 H021 119.6 . . ? C5 C6 H021 119.6 . . ? C6 C7 C8 118.5(3) . . ? C6 C7 H022 120.8 . . ? C8 C7 H022 120.8 . . ? C16 C8 C7 117.3(3) . . ? C16 C8 C9 118.1(3) . . ? C7 C8 C9 124.6(3) . . ? C10 C9 C8 121.1(3) . . ? C10 C9 H020 119.4 . . ? C8 C9 H020 119.4 . . ? C9 C10 C11 120.8(3) . . ? C9 C10 H012 119.6 . . ? C11 C10 H012 119.6 . . ? C15 C11 C12 116.3(3) . . ? C15 C11 C10 118.8(2) . . ? C12 C11 C10 124.9(3) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 H016 120.4 . . ? C11 C12 H016 120.4 . . ? C12 C13 C14 120.3(3) . . ? C12 C13 H017 119.8 . . ? C14 C13 H017 119.8 . . ? N6 C14 C13 121.7(3) . . ? N6 C14 H027 119.1 . . ? C13 C14 H027 119.1 . . ? N6 C15 C11 124.4(2) . . ? N6 C15 C16 115.7(2) . . ? C11 C15 C16 119.8(2) . . ? N5 C16 C8 123.7(3) . . ? N5 C16 C15 114.9(2) . . ? C8 C16 C15 121.4(2) . . ? C18 C17 H11A 109.5 . . ? C18 C17 H11B 109.5 . . ? H11A C17 H11B 109.5 . . ? C18 C17 H11C 109.5 . . ? H11A C17 H11C 109.5 . . ? H11B C17 H11C 109.5 . . ? N7 C18 C17 179.4(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.265 _refine_diff_density_min -0.187 _refine_diff_density_rms 0.051 # Attachment 'ch1ppx75_0m.cif' data_ch1ppx75_0m _database_code_depnum_ccdc_archive 'CCDC 737985' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C36 H30 N P2), C6 N6 S6 Si, 2(C2 H3 N)' _chemical_formula_sum 'C82 H66 N10 P4 S6 Si' _chemical_formula_weight 1535.78 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7540(4) _cell_length_b 13.4160(6) _cell_length_c 14.4498(5) _cell_angle_alpha 100.540(2) _cell_angle_beta 102.120(2) _cell_angle_gamma 96.806(2) _cell_volume 1977.01(13) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9985 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 27.33 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 798 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9417 _exptl_absorpt_correction_T_max 0.9566 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 100 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 33304 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.45 _reflns_number_total 8974 _reflns_number_gt 7406 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0440P)^2^+0.7175P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8974 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0968 _refine_ls_wR_factor_gt 0.0905 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.5000 1.0000 0.0000 0.02045(14) Uani 1 2 d S . . P1 P 0.31840(4) 0.68070(3) 0.34130(3) 0.01538(9) Uani 1 1 d . . . P2 P 0.08796(4) 0.78241(3) 0.29552(3) 0.01475(9) Uani 1 1 d . . . S1 S 0.86494(4) 1.23891(3) 0.06448(3) 0.02817(11) Uani 1 1 d . . . S2 S 0.37092(7) 1.30078(5) 0.12107(4) 0.05078(17) Uani 1 1 d . . . S3 S 0.62359(5) 0.94311(4) 0.30871(3) 0.03425(12) Uani 1 1 d . . . N1 N 0.65492(13) 1.08199(11) 0.01900(10) 0.0245(3) Uani 1 1 d . . . N2 N 0.43045(13) 1.11319(11) 0.04125(10) 0.0248(3) Uani 1 1 d . . . N3 N 0.54388(14) 0.98198(11) 0.12461(10) 0.0256(3) Uani 1 1 d . . . N4 N 0.23412(12) 0.76877(10) 0.32877(9) 0.0184(3) Uani 1 1 d . . . N5 N 0.2588(2) 0.56236(19) 0.65821(13) 0.0547(5) Uani 1 1 d . . . C1 C 0.74334(15) 1.14802(13) 0.03735(11) 0.0204(3) Uani 1 1 d . . . C2 C 0.40439(17) 1.19218(15) 0.07365(12) 0.0262(4) Uani 1 1 d . . . C3 C 0.57710(15) 0.96524(13) 0.20195(12) 0.0233(4) Uani 1 1 d . . . C4 C 0.23049(14) 0.55580(12) 0.33733(11) 0.0173(3) Uani 1 1 d . . . C5 C 0.20931(15) 0.47607(13) 0.25557(11) 0.0198(3) Uani 1 1 d . . . H5 H 0.2446 0.4861 0.2023 0.024 Uiso 1 1 calc R . . C6 C 0.13624(15) 0.38191(14) 0.25244(13) 0.0240(4) Uani 1 1 d . . . H6 H 0.1209 0.3280 0.1967 0.029 Uiso 1 1 calc R . . C7 C 0.08589(16) 0.36676(14) 0.33052(13) 0.0268(4) Uani 1 1 d . . . H7 H 0.0360 0.3025 0.3280 0.032 Uiso 1 1 calc R . . C8 C 0.10805(17) 0.44525(15) 0.41253(13) 0.0285(4) Uani 1 1 d . . . H8 H 0.0747 0.4341 0.4663 0.034 Uiso 1 1 calc R . . C9 C 0.17876(16) 0.53985(14) 0.41584(12) 0.0227(3) Uani 1 1 d . . . H9 H 0.1921 0.5939 0.4713 0.027 Uiso 1 1 calc R . . C10 C 0.43220(14) 0.71870(13) 0.45743(11) 0.0182(3) Uani 1 1 d . . . C11 C 0.48420(16) 0.64533(14) 0.50481(12) 0.0248(4) Uani 1 1 d . . . H11 H 0.4572 0.5742 0.4768 0.030 Uiso 1 1 calc R . . C12 C 0.57520(16) 0.67641(15) 0.59272(12) 0.0288(4) Uani 1 1 d . . . H12 H 0.6102 0.6266 0.6247 0.035 Uiso 1 1 calc R . . C13 C 0.61460(16) 0.77976(15) 0.63349(12) 0.0264(4) Uani 1 1 d . . . H13 H 0.6769 0.8007 0.6935 0.032 Uiso 1 1 calc R . . C14 C 0.56391(16) 0.85354(15) 0.58746(12) 0.0257(4) Uani 1 1 d . . . H14 H 0.5915 0.9245 0.6161 0.031 Uiso 1 1 calc R . . C15 C 0.47243(15) 0.82317(13) 0.49917(11) 0.0214(3) Uani 1 1 d . . . H15 H 0.4376 0.8734 0.4676 0.026 Uiso 1 1 calc R . . C16 C 0.40912(14) 0.66232(12) 0.24983(11) 0.0174(3) Uani 1 1 d . . . C17 C 0.51261(16) 0.60794(14) 0.26247(13) 0.0266(4) Uani 1 1 d . . . H17 H 0.5367 0.5833 0.3202 0.032 Uiso 1 1 calc R . . C18 C 0.57983(17) 0.59010(16) 0.19064(14) 0.0332(4) Uani 1 1 d . . . H18 H 0.6491 0.5521 0.1987 0.040 Uiso 1 1 calc R . . C19 C 0.54620(17) 0.62765(15) 0.10671(13) 0.0309(4) Uani 1 1 d . . . H19 H 0.5931 0.6158 0.0580 0.037 Uiso 1 1 calc R . . C20 C 0.44455(17) 0.68219(14) 0.09419(12) 0.0271(4) Uani 1 1 d . . . H20 H 0.4221 0.7080 0.0369 0.033 Uiso 1 1 calc R . . C21 C 0.37500(15) 0.69941(13) 0.16523(11) 0.0210(3) Uani 1 1 d . . . H21 H 0.3047 0.7362 0.1562 0.025 Uiso 1 1 calc R . . C22 C 0.08693(15) 0.89299(12) 0.24079(11) 0.0177(3) Uani 1 1 d . . . C23 C 0.19877(16) 0.93684(13) 0.21945(11) 0.0214(3) Uani 1 1 d . . . H23 H 0.2776 0.9125 0.2387 0.026 Uiso 1 1 calc R . . C24 C 0.19447(18) 1.01672(13) 0.16960(12) 0.0265(4) Uani 1 1 d . . . H24 H 0.2704 1.0465 0.1545 0.032 Uiso 1 1 calc R . . C25 C 0.07960(19) 1.05259(14) 0.14207(13) 0.0308(4) Uani 1 1 d . . . H25 H 0.0770 1.1067 0.1078 0.037 Uiso 1 1 calc R . . C26 C -0.03166(18) 1.00994(15) 0.16429(13) 0.0311(4) Uani 1 1 d . . . H26 H -0.1098 1.0355 0.1458 0.037 Uiso 1 1 calc R . . C27 C -0.02925(16) 0.92999(13) 0.21347(12) 0.0238(4) Uani 1 1 d . . . H27 H -0.1055 0.9006 0.2285 0.029 Uiso 1 1 calc R . . C28 C -0.01296(14) 0.67712(12) 0.20528(11) 0.0173(3) Uani 1 1 d . . . C29 C -0.02909(16) 0.68146(14) 0.10721(12) 0.0246(4) Uani 1 1 d . . . H29 H 0.0058 0.7419 0.0898 0.030 Uiso 1 1 calc R . . C30 C -0.09596(18) 0.59759(15) 0.03586(12) 0.0305(4) Uani 1 1 d . . . H30 H -0.1070 0.6007 -0.0305 0.037 Uiso 1 1 calc R . . C31 C -0.14695(16) 0.50896(14) 0.06078(13) 0.0265(4) Uani 1 1 d . . . H31 H -0.1925 0.4517 0.0115 0.032 Uiso 1 1 calc R . . C32 C -0.13158(15) 0.50388(13) 0.15761(12) 0.0222(3) Uani 1 1 d . . . H32 H -0.1663 0.4430 0.1744 0.027 Uiso 1 1 calc R . . C33 C -0.06537(14) 0.58789(13) 0.23006(12) 0.0190(3) Uani 1 1 d . . . H33 H -0.0558 0.5847 0.2963 0.023 Uiso 1 1 calc R . . C34 C 0.01524(15) 0.80780(12) 0.39729(11) 0.0180(3) Uani 1 1 d . . . C35 C -0.11777(15) 0.78501(13) 0.38744(12) 0.0216(3) Uani 1 1 d . . . H35 H -0.1726 0.7507 0.3266 0.026 Uiso 1 1 calc R . . C36 C -0.16967(16) 0.81296(14) 0.46741(12) 0.0256(4) Uani 1 1 d . . . H36 H -0.2598 0.7965 0.4612 0.031 Uiso 1 1 calc R . . C37 C -0.09035(17) 0.86452(14) 0.55565(12) 0.0253(4) Uani 1 1 d . . . H37 H -0.1264 0.8839 0.6096 0.030 Uiso 1 1 calc R . . C38 C 0.04187(17) 0.88818(14) 0.56581(12) 0.0254(4) Uani 1 1 d . . . H38 H 0.0959 0.9239 0.6265 0.031 Uiso 1 1 calc R . . C39 C 0.09495(16) 0.85937(13) 0.48694(11) 0.0222(3) Uani 1 1 d . . . H39 H 0.1854 0.8747 0.4940 0.027 Uiso 1 1 calc R . . C40 C 0.3116(2) 0.76076(18) 0.71762(16) 0.0443(5) Uani 1 1 d . . . H40A H 0.3137 0.7927 0.6621 0.067 Uiso 1 1 calc R . . H40B H 0.3957 0.7798 0.7640 0.067 Uiso 1 1 calc R . . H40C H 0.2450 0.7846 0.7491 0.067 Uiso 1 1 calc R . . C41 C 0.2826(2) 0.6499(2) 0.68462(14) 0.0384(5) Uani 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 Si1 0.0195(3) 0.0177(3) 0.0231(3) 0.0055(3) 0.0034(2) 0.0000(3) P1 0.01434(19) 0.0166(2) 0.01457(18) 0.00273(16) 0.00197(14) 0.00346(15) P2 0.01480(19) 0.0148(2) 0.01475(18) 0.00333(15) 0.00315(14) 0.00338(15) S1 0.0229(2) 0.0201(2) 0.0384(3) 0.00701(19) 0.00325(18) -0.00292(17) S2 0.0872(5) 0.0430(3) 0.0428(3) 0.0181(3) 0.0360(3) 0.0412(3) S3 0.0393(3) 0.0359(3) 0.0256(2) 0.0108(2) 0.00031(19) 0.0048(2) N1 0.0224(7) 0.0218(8) 0.0279(8) 0.0055(6) 0.0043(6) 0.0004(6) N2 0.0232(7) 0.0217(8) 0.0299(8) 0.0069(6) 0.0069(6) 0.0021(6) N3 0.0259(7) 0.0229(8) 0.0259(8) 0.0062(6) 0.0031(6) 0.0001(6) N4 0.0170(6) 0.0172(7) 0.0200(7) 0.0028(5) 0.0029(5) 0.0034(5) N5 0.0688(14) 0.0618(15) 0.0312(10) 0.0158(10) 0.0108(9) -0.0053(11) C1 0.0223(8) 0.0206(9) 0.0203(8) 0.0077(7) 0.0049(6) 0.0070(7) C2 0.0281(9) 0.0312(11) 0.0263(9) 0.0149(8) 0.0122(7) 0.0085(8) C3 0.0197(8) 0.0192(9) 0.0299(9) 0.0040(7) 0.0052(7) 0.0015(7) C4 0.0143(7) 0.0187(8) 0.0189(7) 0.0060(6) 0.0011(6) 0.0048(6) C5 0.0172(7) 0.0214(9) 0.0198(8) 0.0037(7) 0.0020(6) 0.0053(6) C6 0.0191(8) 0.0204(9) 0.0276(9) 0.0012(7) -0.0015(7) 0.0027(7) C7 0.0187(8) 0.0210(9) 0.0399(10) 0.0108(8) 0.0028(7) 0.0007(7) C8 0.0270(9) 0.0317(11) 0.0305(9) 0.0138(8) 0.0097(7) 0.0028(8) C9 0.0233(8) 0.0247(9) 0.0204(8) 0.0044(7) 0.0057(7) 0.0043(7) C10 0.0147(7) 0.0230(9) 0.0159(7) 0.0028(6) 0.0025(6) 0.0038(6) C11 0.0249(9) 0.0216(9) 0.0244(8) 0.0037(7) -0.0017(7) 0.0044(7) C12 0.0250(9) 0.0355(11) 0.0237(9) 0.0103(8) -0.0022(7) 0.0047(8) C13 0.0187(8) 0.0385(11) 0.0171(8) 0.0025(7) -0.0008(6) 0.0003(8) C14 0.0229(8) 0.0269(10) 0.0222(8) -0.0032(7) 0.0038(7) 0.0001(7) C15 0.0193(8) 0.0231(9) 0.0212(8) 0.0040(7) 0.0045(6) 0.0036(7) C16 0.0153(7) 0.0174(8) 0.0179(7) 0.0011(6) 0.0038(6) 0.0011(6) C17 0.0232(8) 0.0334(11) 0.0280(9) 0.0120(8) 0.0086(7) 0.0102(8) C18 0.0250(9) 0.0422(12) 0.0398(11) 0.0121(9) 0.0148(8) 0.0171(9) C19 0.0286(9) 0.0369(11) 0.0316(10) 0.0061(8) 0.0172(8) 0.0067(8) C20 0.0308(9) 0.0293(10) 0.0229(8) 0.0070(7) 0.0093(7) 0.0035(8) C21 0.0211(8) 0.0206(9) 0.0208(8) 0.0030(7) 0.0049(6) 0.0039(7) C22 0.0219(8) 0.0153(8) 0.0155(7) 0.0024(6) 0.0039(6) 0.0039(6) C23 0.0244(8) 0.0178(9) 0.0213(8) 0.0009(7) 0.0068(7) 0.0031(7) C24 0.0368(10) 0.0185(9) 0.0249(9) 0.0033(7) 0.0128(7) 0.0002(7) C25 0.0479(11) 0.0208(10) 0.0267(9) 0.0105(8) 0.0095(8) 0.0078(8) C26 0.0341(10) 0.0293(11) 0.0327(10) 0.0125(8) 0.0046(8) 0.0136(8) C27 0.0217(8) 0.0229(9) 0.0273(9) 0.0073(7) 0.0048(7) 0.0051(7) C28 0.0148(7) 0.0164(8) 0.0203(8) 0.0029(6) 0.0033(6) 0.0042(6) C29 0.0297(9) 0.0222(9) 0.0204(8) 0.0046(7) 0.0044(7) 0.0001(7) C30 0.0403(11) 0.0288(10) 0.0185(8) 0.0020(7) 0.0038(7) 0.0009(8) C31 0.0235(8) 0.0229(9) 0.0266(9) -0.0036(7) 0.0016(7) 0.0000(7) C32 0.0171(8) 0.0184(9) 0.0308(9) 0.0038(7) 0.0064(7) 0.0028(6) C33 0.0160(7) 0.0202(9) 0.0214(8) 0.0049(7) 0.0042(6) 0.0048(6) C34 0.0204(8) 0.0174(8) 0.0181(7) 0.0054(6) 0.0061(6) 0.0054(6) C35 0.0204(8) 0.0236(9) 0.0197(8) 0.0028(7) 0.0036(6) 0.0040(7) C36 0.0213(8) 0.0306(10) 0.0279(9) 0.0071(8) 0.0102(7) 0.0064(7) C37 0.0313(9) 0.0273(10) 0.0213(8) 0.0058(7) 0.0127(7) 0.0086(8) C38 0.0289(9) 0.0277(10) 0.0173(8) 0.0002(7) 0.0049(7) 0.0037(8) C39 0.0192(8) 0.0252(9) 0.0210(8) 0.0040(7) 0.0036(6) 0.0024(7) C40 0.0429(12) 0.0530(15) 0.0407(12) 0.0124(11) 0.0150(10) 0.0090(11) C41 0.0363(11) 0.0578(16) 0.0229(9) 0.0164(10) 0.0084(8) 0.0003(10) _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 1.8232(14) . ? Si1 N1 1.8232(14) 2_675 ? Si1 N2 1.8292(15) 2_675 ? Si1 N2 1.8292(15) . ? Si1 N3 1.8311(14) . ? Si1 N3 1.8311(14) 2_675 ? P1 N4 1.5854(13) . ? P1 C16 1.7996(15) . ? P1 C10 1.8029(16) . ? P1 C4 1.8086(16) . ? P2 N4 1.5868(13) . ? P2 C28 1.8006(16) . ? P2 C34 1.8036(15) . ? P2 C22 1.8044(16) . ? S1 C1 1.6070(17) . ? S2 C2 1.608(2) . ? S3 C3 1.6114(17) . ? N1 C1 1.170(2) . ? N2 C2 1.168(2) . ? N3 C3 1.170(2) . ? N5 C41 1.146(3) . ? C4 C5 1.400(2) . ? C4 C9 1.403(2) . ? C5 C6 1.394(2) . ? C5 H5 0.9500 . ? C6 C7 1.386(2) . ? C6 H6 0.9500 . ? C7 C8 1.391(3) . ? C7 H7 0.9500 . ? C8 C9 1.388(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C15 1.397(2) . ? C10 C11 1.402(2) . ? C11 C12 1.390(2) . ? C11 H11 0.9500 . ? C12 C13 1.381(3) . ? C12 H12 0.9500 . ? C13 C14 1.391(3) . ? C13 H13 0.9500 . ? C14 C15 1.396(2) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.398(2) . ? C16 C17 1.400(2) . ? C17 C18 1.386(2) . ? C17 H17 0.9500 . ? C18 C19 1.392(3) . ? C18 H18 0.9500 . ? C19 C20 1.385(3) . ? C19 H19 0.9500 . ? C20 C21 1.394(2) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.394(2) . ? C22 C27 1.405(2) . ? C23 C24 1.396(2) . ? C23 H23 0.9500 . ? C24 C25 1.386(3) . ? C24 H24 0.9500 . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 C27 1.391(2) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.400(2) . ? C28 C29 1.404(2) . ? C29 C30 1.385(2) . ? C29 H29 0.9500 . ? C30 C31 1.389(3) . ? C30 H30 0.9500 . ? C31 C32 1.389(2) . ? C31 H31 0.9500 . ? C32 C33 1.392(2) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C35 1.398(2) . ? C34 C39 1.399(2) . ? C35 C36 1.396(2) . ? C35 H35 0.9500 . ? C36 C37 1.383(2) . ? C36 H36 0.9500 . ? C37 C38 1.390(2) . ? C37 H37 0.9500 . ? C38 C39 1.392(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C41 1.451(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 N1 Si1 N1 180.00(9) . 2_675 ? N1 Si1 N2 90.41(6) . 2_675 ? N1 Si1 N2 89.59(6) 2_675 2_675 ? N1 Si1 N2 89.59(6) . . ? N1 Si1 N2 90.41(6) 2_675 . ? N2 Si1 N2 180.00(9) 2_675 . ? N1 Si1 N3 90.11(6) . . ? N1 Si1 N3 89.89(6) 2_675 . ? N2 Si1 N3 89.94(7) 2_675 . ? N2 Si1 N3 90.06(7) . . ? N1 Si1 N3 89.89(6) . 2_675 ? N1 Si1 N3 90.11(6) 2_675 2_675 ? N2 Si1 N3 90.06(7) 2_675 2_675 ? N2 Si1 N3 89.94(7) . 2_675 ? N3 Si1 N3 180.00(9) . 2_675 ? N4 P1 C16 111.30(7) . . ? N4 P1 C10 108.50(7) . . ? C16 P1 C10 107.54(7) . . ? N4 P1 C4 115.85(7) . . ? C16 P1 C4 106.52(7) . . ? C10 P1 C4 106.75(7) . . ? N4 P2 C28 115.14(7) . . ? N4 P2 C34 111.58(7) . . ? C28 P2 C34 108.95(7) . . ? N4 P2 C22 107.06(7) . . ? C28 P2 C22 106.03(7) . . ? C34 P2 C22 107.66(7) . . ? C1 N1 Si1 168.20(14) . . ? C2 N2 Si1 170.13(15) . . ? C3 N3 Si1 175.12(15) . . ? P1 N4 P2 139.97(9) . . ? N1 C1 S1 179.03(15) . . ? N2 C2 S2 178.44(17) . . ? N3 C3 S3 179.53(18) . . ? C5 C4 C9 119.57(15) . . ? C5 C4 P1 120.90(12) . . ? C9 C4 P1 119.49(13) . . ? C6 C5 C4 119.84(15) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C7 C6 C5 120.16(16) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C6 C7 C8 120.28(16) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 120.09(16) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C4 120.04(16) . . ? C8 C9 H9 120.0 . . ? C4 C9 H9 120.0 . . ? C15 C10 C11 119.57(15) . . ? C15 C10 P1 119.30(12) . . ? C11 C10 P1 121.10(13) . . ? C12 C11 C10 120.17(17) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C13 C12 C11 119.95(16) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.61(16) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 119.91(17) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 119.79(16) . . ? C14 C15 H15 120.1 . . ? C10 C15 H15 120.1 . . ? C21 C16 C17 119.78(14) . . ? C21 C16 P1 120.59(12) . . ? C17 C16 P1 119.60(12) . . ? C18 C17 C16 119.91(16) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.22(16) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 120.10(16) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C19 C20 C21 120.27(16) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 119.72(15) . . ? C20 C21 H21 120.1 . . ? C16 C21 H21 120.1 . . ? C23 C22 C27 120.14(15) . . ? C23 C22 P2 120.08(12) . . ? C27 C22 P2 119.62(12) . . ? C22 C23 C24 119.70(16) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.08(16) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 120.36(16) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C27 120.32(17) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C26 C27 C22 119.39(16) . . ? C26 C27 H27 120.3 . . ? C22 C27 H27 120.3 . . ? C33 C28 C29 119.53(15) . . ? C33 C28 P2 121.62(12) . . ? C29 C28 P2 118.59(12) . . ? C30 C29 C28 119.91(16) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 120.35(16) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C32 120.19(16) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C31 C32 C33 120.04(16) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C28 119.97(15) . . ? C32 C33 H33 120.0 . . ? C28 C33 H33 120.0 . . ? C35 C34 C39 119.69(14) . . ? C35 C34 P2 122.21(12) . . ? C39 C34 P2 117.91(12) . . ? C36 C35 C34 119.70(15) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 120.27(15) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? C36 C37 C38 120.36(15) . . ? C36 C37 H37 119.8 . . ? C38 C37 H37 119.8 . . ? C37 C38 C39 119.89(16) . . ? C37 C38 H38 120.1 . . ? C39 C38 H38 120.1 . . ? C38 C39 C34 120.08(15) . . ? C38 C39 H39 120.0 . . ? C34 C39 H39 120.0 . . ? C41 C40 H40A 109.5 . . ? C41 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C41 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N5 C41 C40 179.5(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.641 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.054