Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'M. Lappert' 'Peter B. Hitchcock' 'Rafael Sablong' _publ_contact_author_name 'Michael F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex BRIGHTON BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Reactions of M[CH(SiMe3)2] (M = Na or K) with PhCN, and related chemistry ; _publ_requested_category FM # Attachment 'mfl-jan-2006.cif' data_(7)-oct997 _database_code_depnum_ccdc_archive 'CCDC 297453' _audit_creation_date 2005-12-15T15:39:28-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C168 H232 N16 Na8 Si16, 4(C5 H12)' _chemical_formula_sum 'C188 H280 N16 Na8 Si16' _chemical_formula_weight 3397.64 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/n _symmetry_space_group_name_Hall '-P 4a' _symmetry_Int_Tables_number 85 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 32.690(7) _cell_length_b 32.690(7) _cell_length_c 9.819(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 10493(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.075 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \w--2\q _diffrn_reflns_av_R_equivalents 0.1122 _diffrn_reflns_av_unetI/netI 0.1855 _diffrn_reflns_number 6674 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 21.97 _diffrn_reflns_theta_full 21.97 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 6404 _reflns_number_gt 3063 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The solvate electron density was very diffuse and the solvate pentane molecule was included with isotropic C atoms, H atoms omitted , and 1,2 and 1,3 C...C constraints. 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^)+(0.1031P)^2^+5.6182P] 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_number_reflns 6404 _refine_ls_number_parameters 489 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1984 _refine_ls_R_factor_gt 0.0919 _refine_ls_wR_factor_ref 0.2617 _refine_ls_wR_factor_gt 0.2091 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.49 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.077 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 -0.19188(8) 0.44846(8) 0.3489(3) 0.0368(7) Uani 1 1 d . . . Si2 Si -0.22916(8) 0.52523(9) 0.8336(3) 0.0443(8) Uani 1 1 d . . . Si3 Si 0.00114(8) 0.58266(8) 0.7644(3) 0.0352(7) Uani 1 1 d . . . Si4 Si -0.08553(8) 0.61487(8) 0.3036(3) 0.0371(7) Uani 1 1 d . . . Na1 Na -0.16021(10) 0.53644(10) 0.5288(4) 0.0421(10) Uani 1 1 d . . . Na2 Na -0.03702(11) 0.66516(10) 0.6023(4) 0.0462(11) Uani 1 1 d . . . N1 N -0.2109(2) 0.4898(2) 0.4359(7) 0.0311(19) Uani 1 1 d . . . N2 N -0.2659(2) 0.5281(2) 0.5318(7) 0.0292(18) Uani 1 1 d . . . N3 N -0.0454(2) 0.5978(2) 0.7004(7) 0.0293(18) Uani 1 1 d . . . N4 N -0.1104(2) 0.5864(2) 0.6018(7) 0.0271(18) Uani 1 1 d . . . C1 C -0.2500(3) 0.4958(3) 0.4693(9) 0.030(2) Uani 1 1 d . . . C2 C -0.2391(3) 0.5605(3) 0.5674(9) 0.031(2) Uani 1 1 d . . . C3 C -0.2223(3) 0.5622(3) 0.6931(10) 0.039(3) Uani 1 1 d . . . H3 H -0.2051 0.5849 0.7112 0.047 Uiso 1 1 calc R . . C4 C -0.2821(3) 0.4647(3) 0.4357(10) 0.034(2) Uani 1 1 d . . . C5 C -0.3091(3) 0.4720(3) 0.3302(10) 0.046(3) Uani 1 1 d . . . H5 H -0.308 0.4974 0.2833 0.055 Uiso 1 1 calc R . . C6 C -0.3382(3) 0.4427(3) 0.2907(12) 0.060(3) Uani 1 1 d . . . H6 H -0.3567 0.4482 0.2184 0.072 Uiso 1 1 calc R . . C7 C -0.3394(3) 0.4065(3) 0.3569(12) 0.053(3) Uani 1 1 d . . . H7 H -0.3581 0.386 0.3278 0.063 Uiso 1 1 calc R . . C8 C -0.3144(3) 0.3990(3) 0.4646(12) 0.055(3) Uani 1 1 d . . . H8 H -0.3167 0.374 0.5133 0.066 Uiso 1 1 calc R . . C9 C -0.2853(3) 0.4278(3) 0.5039(10) 0.047(3) Uani 1 1 d . . . H9 H -0.2675 0.4221 0.578 0.056 Uiso 1 1 calc R . . C10 C -0.2335(3) 0.5930(3) 0.4605(10) 0.035(2) Uani 1 1 d . . . C11 C -0.2474(3) 0.5874(3) 0.3275(10) 0.042(3) Uani 1 1 d . . . H11 H -0.2589 0.5618 0.3029 0.051 Uiso 1 1 calc R . . C12 C -0.2449(3) 0.6177(3) 0.2308(12) 0.059(3) Uani 1 1 d . . . H12 H -0.255 0.6128 0.1415 0.07 Uiso 1 1 calc R . . C13 C -0.2279(3) 0.6547(4) 0.2622(15) 0.064(4) Uani 1 1 d . . . H13 H -0.2264 0.6757 0.1956 0.077 Uiso 1 1 calc R . . C14 C -0.2132(3) 0.6610(3) 0.3921(14) 0.060(3) Uani 1 1 d . . . H14 H -0.201 0.6866 0.4139 0.072 Uiso 1 1 calc R . . C15 C -0.2157(3) 0.6306(3) 0.4932(11) 0.044(3) Uani 1 1 d . . . H15 H -0.2054 0.6355 0.5822 0.053 Uiso 1 1 calc R . . C16 C -0.1796(3) 0.4046(3) 0.4634(11) 0.062(3) Uani 1 1 d . . . H16C H -0.1635 0.4143 0.541 0.093 Uiso 1 1 calc R . . H16B H -0.1639 0.3841 0.4129 0.093 Uiso 1 1 calc R . . H16A H -0.2051 0.3923 0.4965 0.093 Uiso 1 1 calc R . . C17 C -0.1415(3) 0.4644(3) 0.2739(10) 0.048(3) Uani 1 1 d . . . H17C H -0.1457 0.4875 0.2121 0.071 Uiso 1 1 calc R . . H17B H -0.1296 0.4414 0.2232 0.071 Uiso 1 1 calc R . . H17A H -0.1228 0.4725 0.3471 0.071 Uiso 1 1 calc R . . C18 C -0.2226(3) 0.4293(3) 0.2017(10) 0.051(3) Uani 1 1 d . . . H18C H -0.2292 0.4522 0.1409 0.076 Uiso 1 1 calc R . . H18B H -0.248 0.4169 0.2352 0.076 Uiso 1 1 calc R . . H18A H -0.2068 0.4088 0.1516 0.076 Uiso 1 1 calc R . . C19 C -0.2003(4) 0.5465(4) 0.9820(11) 0.080(4) Uani 1 1 d . . . H19C H -0.203 0.5279 1.0599 0.12 Uiso 1 1 calc R . . H19B H -0.2116 0.5733 1.0062 0.12 Uiso 1 1 calc R . . H19A H -0.1714 0.5494 0.9579 0.12 Uiso 1 1 calc R . . C20 C -0.2848(3) 0.5186(4) 0.8785(12) 0.077(4) Uani 1 1 d . . . H20C H -0.2873 0.4989 0.9531 0.115 Uiso 1 1 calc R . . H20B H -0.2997 0.5086 0.7988 0.115 Uiso 1 1 calc R . . H20A H -0.2962 0.545 0.9071 0.115 Uiso 1 1 calc R . . C21 C -0.2067(3) 0.4742(3) 0.7925(11) 0.063(3) Uani 1 1 d . . . H21C H -0.211 0.4556 0.8694 0.095 Uiso 1 1 calc R . . H21B H -0.1773 0.4772 0.7754 0.095 Uiso 1 1 calc R . . H21A H -0.2201 0.4631 0.7111 0.095 Uiso 1 1 calc R . . C22 C -0.0780(3) 0.5751(3) 0.6689(9) 0.029(2) Uani 1 1 d . . . C23 C -0.1147(2) 0.6290(3) 0.5747(9) 0.028(2) Uani 1 1 d . . . C24 C -0.1049(3) 0.6447(3) 0.4520(10) 0.035(2) Uani 1 1 d . . . H24 H -0.1081 0.6733 0.4401 0.042 Uiso 1 1 calc R . . C25 C -0.0802(2) 0.5308(2) 0.7106(9) 0.028(2) Uani 1 1 d . . . C26 C -0.0854(3) 0.5208(3) 0.8454(10) 0.039(2) Uani 1 1 d . . . H26 H -0.087 0.542 0.9113 0.047 Uiso 1 1 calc R . . C27 C -0.0882(3) 0.4805(3) 0.8871(11) 0.052(3) Uani 1 1 d . . . H27 H -0.0913 0.4744 0.9811 0.062 Uiso 1 1 calc R . . C28 C -0.0864(3) 0.4491(3) 0.7928(12) 0.053(3) Uani 1 1 d . . . H28 H -0.0881 0.4213 0.8209 0.063 Uiso 1 1 calc R . . C29 C -0.0822(3) 0.4591(3) 0.6561(11) 0.046(3) Uani 1 1 d . . . H29 H -0.0815 0.4379 0.5899 0.055 Uiso 1 1 calc R . . C30 C -0.0791(3) 0.4996(3) 0.6149(10) 0.037(2) Uani 1 1 d . . . H30 H -0.0761 0.5059 0.521 0.044 Uiso 1 1 calc R . . C31 C -0.1325(2) 0.6537(3) 0.6875(10) 0.033(2) Uani 1 1 d . . . C32 C -0.1413(3) 0.6358(3) 0.8133(10) 0.041(3) Uani 1 1 d . . . H32 H -0.1339 0.608 0.8288 0.05 Uiso 1 1 calc R . . C33 C -0.1604(3) 0.6576(4) 0.9155(11) 0.055(3) Uani 1 1 d . . . H33 H -0.1665 0.6445 0.9995 0.067 Uiso 1 1 calc R . . C34 C -0.1707(3) 0.6978(3) 0.8975(12) 0.053(3) Uani 1 1 d . . . H34 H -0.1837 0.7128 0.9683 0.063 Uiso 1 1 calc R . . C35 C -0.1619(3) 0.7163(3) 0.7748(14) 0.069(4) Uani 1 1 d . . . H35 H -0.1684 0.7443 0.7612 0.083 Uiso 1 1 calc R . . C36 C -0.1436(3) 0.6944(3) 0.6717(11) 0.052(3) Uani 1 1 d . . . H36 H -0.1384 0.7075 0.5871 0.062 Uiso 1 1 calc R . . C37 C 0.0052(3) 0.5922(4) 0.9512(10) 0.068(3) Uani 1 1 d . . . H37C H -0.0034 0.6203 0.9711 0.102 Uiso 1 1 calc R . . H37B H 0.0336 0.5884 0.9804 0.102 Uiso 1 1 calc R . . H37A H -0.0125 0.573 1.0001 0.102 Uiso 1 1 calc R . . C38 C 0.0174(3) 0.5293(3) 0.7249(11) 0.053(3) Uani 1 1 d . . . H38C H 0.0152 0.5245 0.6266 0.08 Uiso 1 1 calc R . . H38B H -0.0003 0.51 0.7735 0.08 Uiso 1 1 calc R . . H38A H 0.0458 0.5253 0.7538 0.08 Uiso 1 1 calc R . . C39 C 0.0400(3) 0.6172(3) 0.6825(11) 0.058(3) Uani 1 1 d . . . H39C H 0.0393 0.6135 0.5835 0.087 Uiso 1 1 calc R . . H39B H 0.0673 0.6104 0.7166 0.087 Uiso 1 1 calc R . . H39A H 0.0337 0.6457 0.7048 0.087 Uiso 1 1 calc R . . C40 C -0.0360(3) 0.5894(3) 0.3386(9) 0.047(3) Uani 1 1 d . . . H40C H -0.0158 0.6099 0.366 0.07 Uiso 1 1 calc R . . H40B H -0.0265 0.5754 0.2562 0.07 Uiso 1 1 calc R . . H40A H -0.0395 0.5694 0.4121 0.07 Uiso 1 1 calc R . . C41 C -0.1239(3) 0.5758(3) 0.2516(10) 0.058(3) Uani 1 1 d . . . H41C H -0.1501 0.5892 0.2331 0.086 Uiso 1 1 calc R . . H41B H -0.1273 0.5558 0.3252 0.086 Uiso 1 1 calc R . . H41A H -0.1143 0.5618 0.1693 0.086 Uiso 1 1 calc R . . C42 C -0.0791(3) 0.6514(3) 0.1587(9) 0.051(3) Uani 1 1 d . . . H42C H -0.1053 0.665 0.14 0.076 Uiso 1 1 calc R . . H42B H -0.0702 0.6365 0.0775 0.076 Uiso 1 1 calc R . . H42A H -0.0586 0.6721 0.1826 0.076 Uiso 1 1 calc R . . C43 C -0.2362(17) 0.307(2) 0.712(8) 0.92(8) Uiso 1 1 d D A 1 C44 C -0.2465(8) 0.3405(14) 0.815(6) 0.60(4) Uiso 1 1 d D A 1 C45 C -0.2908(10) 0.3350(7) 0.865(5) 0.44(3) Uiso 1 1 d D A 1 C46 C -0.3083(9) 0.3769(6) 0.907(4) 0.301(16) Uiso 1 1 d D A 1 C47 C -0.3511(9) 0.3703(8) 0.970(3) 0.291(15) Uiso 1 1 d D A 1 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 0.0333(16) 0.0338(16) 0.0434(17) -0.0058(14) 0.0003(14) 0.0038(13) Si2 0.0410(17) 0.0563(19) 0.0357(17) -0.0077(15) -0.0010(14) -0.0017(15) Si3 0.0304(15) 0.0359(16) 0.0394(17) -0.0039(14) -0.0042(13) 0.0036(13) Si4 0.0397(17) 0.0355(16) 0.0361(16) 0.0027(13) -0.0035(14) -0.0027(13) Na1 0.031(2) 0.039(2) 0.057(3) -0.008(2) -0.0008(19) -0.0026(18) Na2 0.046(2) 0.032(2) 0.060(3) 0.0108(19) -0.012(2) -0.0045(18) N1 0.022(4) 0.033(5) 0.038(5) -0.007(4) -0.002(4) 0.002(4) N2 0.021(4) 0.029(5) 0.037(5) -0.003(4) 0.003(4) -0.001(4) N3 0.030(4) 0.033(4) 0.025(4) 0.000(4) -0.003(4) -0.002(4) N4 0.028(4) 0.024(4) 0.030(4) 0.002(4) -0.006(4) 0.004(3) C1 0.031(6) 0.027(6) 0.032(6) 0.000(5) -0.009(5) -0.006(5) C2 0.022(5) 0.036(6) 0.035(6) -0.005(5) 0.009(5) 0.010(5) C3 0.027(5) 0.043(6) 0.047(7) -0.014(5) 0.000(5) -0.002(5) C4 0.027(5) 0.031(6) 0.044(6) -0.002(5) -0.005(5) 0.009(5) C5 0.039(6) 0.037(6) 0.060(7) 0.001(6) -0.011(6) 0.004(5) C6 0.046(7) 0.055(8) 0.079(9) -0.005(7) -0.034(6) 0.000(6) C7 0.040(7) 0.042(7) 0.076(8) -0.007(7) -0.007(6) -0.001(5) C8 0.051(7) 0.044(7) 0.072(8) 0.006(6) -0.001(7) -0.006(6) C9 0.044(7) 0.049(7) 0.047(7) 0.010(6) -0.009(5) -0.014(6) C10 0.024(5) 0.038(6) 0.042(6) -0.004(5) 0.002(5) -0.004(5) C11 0.038(6) 0.046(7) 0.044(7) 0.003(6) 0.003(5) 0.000(5) C12 0.064(8) 0.054(8) 0.058(8) 0.011(7) 0.013(6) -0.004(6) C13 0.044(7) 0.059(9) 0.089(11) 0.030(8) 0.019(7) 0.005(6) C14 0.036(7) 0.039(7) 0.106(11) 0.013(8) 0.015(7) -0.020(5) C15 0.025(5) 0.032(6) 0.076(8) 0.006(6) 0.007(5) -0.008(5) C16 0.048(7) 0.059(7) 0.080(8) 0.001(7) 0.002(6) 0.025(6) C17 0.042(6) 0.043(6) 0.058(7) -0.013(6) 0.004(6) 0.004(5) C18 0.052(7) 0.050(7) 0.049(7) -0.021(6) 0.006(6) -0.010(5) C19 0.086(9) 0.091(10) 0.063(8) -0.028(8) -0.012(7) -0.012(8) C20 0.046(7) 0.110(10) 0.074(9) 0.040(8) 0.025(7) 0.002(7) C21 0.078(8) 0.059(8) 0.053(7) 0.002(6) -0.004(7) 0.014(6) C22 0.024(5) 0.038(6) 0.025(5) 0.006(5) -0.004(5) 0.000(5) C23 0.012(5) 0.034(6) 0.038(6) 0.003(5) -0.015(4) -0.002(4) C24 0.038(6) 0.020(5) 0.048(7) -0.001(5) -0.011(5) -0.009(4) C25 0.027(5) 0.024(5) 0.032(6) -0.005(5) 0.005(4) -0.001(4) C26 0.050(6) 0.034(6) 0.034(6) 0.005(5) 0.004(5) 0.000(5) C27 0.056(7) 0.047(7) 0.052(7) 0.014(6) 0.002(6) 0.004(6) C28 0.053(7) 0.032(6) 0.074(9) 0.017(7) -0.004(6) 0.001(5) C29 0.054(7) 0.032(6) 0.052(7) -0.008(6) -0.001(6) 0.004(5) C30 0.042(6) 0.034(6) 0.033(6) 0.005(5) 0.002(5) -0.002(5) C31 0.017(5) 0.038(6) 0.044(6) 0.003(5) -0.001(5) 0.002(4) C32 0.032(6) 0.047(6) 0.046(7) -0.013(6) -0.009(5) 0.005(5) C33 0.041(7) 0.072(9) 0.053(7) -0.014(7) -0.002(6) 0.005(6) C34 0.047(7) 0.051(8) 0.060(8) -0.035(7) 0.017(6) -0.004(6) C35 0.076(9) 0.038(7) 0.093(10) -0.010(7) 0.024(8) -0.009(6) C36 0.066(8) 0.028(6) 0.062(8) -0.002(6) 0.023(6) -0.002(5) C37 0.078(8) 0.091(9) 0.035(6) -0.002(6) -0.016(6) 0.014(7) C38 0.035(6) 0.045(6) 0.080(8) -0.006(6) -0.002(6) 0.008(5) C39 0.030(6) 0.066(7) 0.077(8) 0.002(7) -0.013(6) -0.005(5) C40 0.063(7) 0.041(6) 0.036(6) 0.013(5) 0.012(5) 0.010(5) C41 0.074(8) 0.056(7) 0.042(7) -0.012(6) 0.000(6) -0.017(6) C42 0.048(7) 0.060(7) 0.045(7) 0.007(6) -0.010(6) -0.013(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 Si1 N1 1.714(7) . ? Si1 C16 1.866(10) . ? Si1 C18 1.869(9) . ? Si1 C17 1.879(9) . ? Si2 C3 1.847(10) . ? Si2 C21 1.865(10) . ? Si2 C19 1.870(10) . ? Si2 C20 1.883(10) . ? Si3 N3 1.718(7) . ? Si3 C38 1.864(9) . ? Si3 C37 1.864(10) . ? Si3 C39 1.881(10) . ? Si4 C40 1.852(9) . ? Si4 C41 1.861(9) . ? Si4 C24 1.863(9) . ? Si4 C42 1.871(9) . ? Na1 N4 2.417(7) . ? Na1 N1 2.431(7) . ? Na2 N2 2.376(7) 3_565 ? Na2 N3 2.420(7) . ? N1 C1 1.333(10) . ? N2 C1 1.327(10) . ? N2 C2 1.418(11) . ? N2 Na2 2.376(7) 4_455 ? N3 C22 1.335(10) . ? N4 C22 1.299(10) . ? N4 C23 1.425(10) . ? C1 C4 1.499(12) . ? C2 C3 1.352(12) . ? C2 C10 1.506(12) . ? C3 H3 0.95 . ? C4 C5 1.381(12) . ? C4 C9 1.383(12) . ? C5 C6 1.404(13) . ? C5 H5 0.95 . ? C6 C7 1.350(13) . ? C6 H6 0.95 . ? C7 C8 1.361(13) . ? C7 H7 0.95 . ? C8 C9 1.393(13) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 C11 1.394(12) . ? C10 C15 1.397(12) . ? C11 C12 1.374(13) . ? C11 H11 0.95 . ? C12 C13 1.366(14) . ? C12 H12 0.95 . ? C13 C14 1.380(15) . ? C13 H13 0.95 . ? C14 C15 1.409(14) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C16 H16C 0.98 . ? C16 H16B 0.98 . ? C16 H16A 0.98 . ? C17 H17C 0.98 . ? C17 H17B 0.98 . ? C17 H17A 0.98 . ? C18 H18C 0.98 . ? C18 H18B 0.98 . ? C18 H18A 0.98 . ? C19 H19C 0.98 . ? C19 H19B 0.98 . ? C19 H19A 0.98 . ? C20 H20C 0.98 . ? C20 H20B 0.98 . ? C20 H20A 0.98 . ? C21 H21C 0.98 . ? C21 H21B 0.98 . ? C21 H21A 0.98 . ? C22 C25 1.507(11) . ? C23 C24 1.348(11) . ? C23 C31 1.489(12) . ? C24 H24 0.95 . ? C25 C26 1.374(12) . ? C25 C30 1.388(11) . ? C26 C27 1.381(12) . ? C26 H26 0.95 . ? C27 C28 1.385(13) . ? C27 H27 0.95 . ? C28 C29 1.388(13) . ? C28 H28 0.95 . ? C29 C30 1.388(12) . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C36 1.386(12) . ? C31 C32 1.397(12) . ? C32 C33 1.380(12) . ? C32 H32 0.95 . ? C33 C34 1.371(14) . ? C33 H33 0.95 . ? C34 C35 1.379(14) . ? C34 H34 0.95 . ? C35 C36 1.377(14) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 H37C 0.98 . ? C37 H37B 0.98 . ? C37 H37A 0.98 . ? C38 H38C 0.98 . ? C38 H38B 0.98 . ? C38 H38A 0.98 . ? C39 H39C 0.98 . ? C39 H39B 0.98 . ? C39 H39A 0.98 . ? C40 H40C 0.98 . ? C40 H40B 0.98 . ? C40 H40A 0.98 . ? C41 H41C 0.98 . ? C41 H41B 0.98 . ? C41 H41A 0.98 . ? C42 H42C 0.98 . ? C42 H42B 0.98 . ? C42 H42A 0.98 . ? C43 C44 1.542(5) . ? C44 C45 1.539(5) . ? C45 C46 1.541(5) . ? C46 C47 1.543(5) . ? 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 C16 112.5(4) . . ? N1 Si1 C18 117.0(4) . . ? C16 Si1 C18 108.9(5) . . ? N1 Si1 C17 107.2(4) . . ? C16 Si1 C17 105.1(4) . . ? C18 Si1 C17 105.1(4) . . ? C3 Si2 C21 112.0(4) . . ? C3 Si2 C19 106.1(5) . . ? C21 Si2 C19 107.6(5) . . ? C3 Si2 C20 111.5(4) . . ? C21 Si2 C20 109.1(5) . . ? C19 Si2 C20 110.3(5) . . ? N3 Si3 C38 116.4(4) . . ? N3 Si3 C37 112.0(4) . . ? C38 Si3 C37 110.0(5) . . ? N3 Si3 C39 105.6(4) . . ? C38 Si3 C39 106.3(5) . . ? C37 Si3 C39 105.8(5) . . ? C40 Si4 C41 109.3(5) . . ? C40 Si4 C24 112.7(4) . . ? C41 Si4 C24 110.2(4) . . ? C40 Si4 C42 109.3(4) . . ? C41 Si4 C42 107.8(4) . . ? C24 Si4 C42 107.4(4) . . ? N4 Na1 N1 174.7(3) . . ? N2 Na2 N3 173.5(3) 3_565 . ? C1 N1 Si1 125.9(6) . . ? C1 N1 Na1 117.9(5) . . ? Si1 N1 Na1 115.7(3) . . ? C1 N2 C2 117.8(7) . . ? C1 N2 Na2 127.2(6) . 4_455 ? C2 N2 Na2 115.0(5) . 4_455 ? C22 N3 Si3 129.2(6) . . ? C22 N3 Na2 120.2(5) . . ? Si3 N3 Na2 107.9(3) . . ? C22 N4 C23 117.0(7) . . ? C22 N4 Na1 120.4(6) . . ? C23 N4 Na1 122.6(5) . . ? N2 C1 N1 127.3(8) . . ? N2 C1 C4 111.5(8) . . ? N1 C1 C4 121.1(8) . . ? C3 C2 N2 120.4(8) . . ? C3 C2 C10 123.9(9) . . ? N2 C2 C10 115.5(8) . . ? C2 C3 Si2 127.3(7) . . ? C2 C3 H3 116.4 . . ? Si2 C3 H3 116.4 . . ? C5 C4 C9 117.8(9) . . ? C5 C4 C1 119.7(8) . . ? C9 C4 C1 122.4(8) . . ? C4 C5 C6 121.4(9) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 119.0(10) . . ? C7 C6 H6 120.5 . . ? C5 C6 H6 120.5 . . ? C6 C7 C8 121.0(10) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C7 C8 C9 120.3(10) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C4 C9 C8 120.4(9) . . ? C4 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C15 117.8(9) . . ? C11 C10 C2 121.4(8) . . ? C15 C10 C2 120.7(9) . . ? C12 C11 C10 122.2(10) . . ? C12 C11 H11 118.9 . . ? C10 C11 H11 118.9 . . ? C13 C12 C11 120.4(11) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 118.9(11) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C13 C14 C15 121.7(10) . . ? C13 C14 H14 119.1 . . ? C15 C14 H14 119.1 . . ? C10 C15 C14 118.9(10) . . ? C10 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? Si1 C16 H16C 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16C C16 H16B 109.5 . . ? Si1 C16 H16A 109.5 . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? Si1 C17 H17C 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17C C17 H17B 109.5 . . ? Si1 C17 H17A 109.5 . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? Si1 C18 H18C 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18C C18 H18B 109.5 . . ? Si1 C18 H18A 109.5 . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? Si2 C19 H19C 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19C C19 H19B 109.5 . . ? Si2 C19 H19A 109.5 . . ? H19C C19 H19A 109.5 . . ? H19B C19 H19A 109.5 . . ? Si2 C20 H20C 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20C C20 H20B 109.5 . . ? Si2 C20 H20A 109.5 . . ? H20C C20 H20A 109.5 . . ? H20B C20 H20A 109.5 . . ? Si2 C21 H21C 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? Si2 C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? H21B C21 H21A 109.5 . . ? N4 C22 N3 127.5(8) . . ? N4 C22 C25 111.9(7) . . ? N3 C22 C25 120.5(7) . . ? C24 C23 N4 121.0(8) . . ? C24 C23 C31 123.5(8) . . ? N4 C23 C31 115.4(8) . . ? C23 C24 Si4 125.6(7) . . ? C23 C24 H24 117.2 . . ? Si4 C24 H24 117.2 . . ? C26 C25 C30 118.7(8) . . ? C26 C25 C22 119.8(8) . . ? C30 C25 C22 121.4(8) . . ? C25 C26 C27 121.4(9) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C28 120.4(10) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C29 118.4(9) . . ? C27 C28 H28 120.8 . . ? C29 C28 H28 120.8 . . ? C28 C29 C30 120.9(9) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C25 120.1(9) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C36 C31 C32 116.6(9) . . ? C36 C31 C23 122.6(9) . . ? C32 C31 C23 120.7(8) . . ? C33 C32 C31 121.3(9) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C34 C33 C32 120.9(11) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 118.8(10) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 120.6 . . ? C36 C35 C34 120.3(10) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 122.1(10) . . ? C35 C36 H36 119 . . ? C31 C36 H36 119 . . ? Si3 C37 H37C 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37C C37 H37B 109.5 . . ? Si3 C37 H37A 109.5 . . ? H37C C37 H37A 109.5 . . ? H37B C37 H37A 109.5 . . ? Si3 C38 H38C 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38C C38 H38B 109.5 . . ? Si3 C38 H38A 109.5 . . ? H38C C38 H38A 109.5 . . ? H38B C38 H38A 109.5 . . ? Si3 C39 H39C 109.5 . . ? Si3 C39 H39B 109.5 . . ? H39C C39 H39B 109.5 . . ? Si3 C39 H39A 109.5 . . ? H39C C39 H39A 109.5 . . ? H39B C39 H39A 109.5 . . ? Si4 C40 H40C 109.5 . . ? Si4 C40 H40B 109.5 . . ? H40C C40 H40B 109.5 . . ? Si4 C40 H40A 109.5 . . ? H40C C40 H40A 109.5 . . ? H40B C40 H40A 109.5 . . ? Si4 C41 H41C 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41C C41 H41B 109.5 . . ? Si4 C41 H41A 109.5 . . ? H41C C41 H41A 109.5 . . ? H41B C41 H41A 109.5 . . ? Si4 C42 H42C 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42C C42 H42B 109.5 . . ? Si4 C42 H42A 109.5 . . ? H42C C42 H42A 109.5 . . ? H42B C42 H42A 109.5 . . ? C45 C44 C43 109.1(5) . . ? C44 C45 C46 109.2(5) . . ? C45 C46 C47 108.6(5) . . ? #===END data_(8)-jan698 _database_code_depnum_ccdc_archive 'CCDC 297454' _audit_creation_date 2005-12-15T16:06:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C28 H48 K2 N2 Si4, 2(C6 H6)' _chemical_formula_sum 'C40 H60 K2 N2 Si4' _chemical_formula_weight 759.46 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 18.754(3) _cell_length_b 13.053(2) _cell_length_c 18.970(4) _cell_angle_alpha 90 _cell_angle_beta 105.88(2) _cell_angle_gamma 90 _cell_volume 4466.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \w--2\q _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_unetI/netI 0.066 _diffrn_reflns_number 5638 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 21.98 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 5447 _reflns_number_gt 3972 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Diffraction was weak and limited in extent. Some H atoms which might have been affected by interactions with K atoms were refined but showed no distortion from normal geometry. 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^)+(0.0265P)^2^+1.7300P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.00082(16) _refine_ls_number_reflns 5447 _refine_ls_number_parameters 467 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0964 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.01 _refine_ls_restrained_S_all 1.01 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.23 _refine_diff_density_min -0.217 _refine_diff_density_rms 0.045 #----------------------------------------------------------------------------# # 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' 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' 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 0.75847(4) 0.09810(6) -0.00922(4) 0.0311(2) Uani 1 1 d . . . K2 K 0.74110(4) 0.37544(6) -0.05161(4) 0.0338(2) Uani 1 1 d . . . Si1 Si 0.67225(5) 0.09632(8) -0.25875(5) 0.0306(3) Uani 1 1 d . A 1 Si2 Si 0.92329(5) 0.24960(8) -0.04199(5) 0.0293(3) Uani 1 1 d . A 1 Si3 Si 0.84611(5) 0.20729(8) 0.21135(5) 0.0287(3) Uani 1 1 d . A 1 Si4 Si 0.57587(5) 0.24819(8) -0.01662(5) 0.0297(3) Uani 1 1 d . A 1 N1 N 0.83239(14) 0.2257(2) -0.08281(14) 0.0244(7) Uani 1 1 d . A 1 N2 N 0.66876(14) 0.2496(2) 0.02469(14) 0.0243(7) Uani 1 1 d . A 1 C1 C 0.72552(18) 0.1547(3) -0.17241(19) 0.0265(9) Uani 1 1 d . A 1 H1 H 0.6954(17) 0.178(2) -0.1443(17) 0.032 Uiso 1 1 d . B 1 C2 C 0.79975(18) 0.1768(2) -0.14639(18) 0.0232(8) Uani 1 1 d . A 1 C3 C 0.84883(17) 0.1405(3) -0.19272(17) 0.0227(8) Uani 1 1 d . A 1 C4 C 0.88804(19) 0.0495(3) -0.17731(19) 0.0325(9) Uani 1 1 d . A 1 H4 H 0.8834 0.0084 -0.1375 0.039 Uiso 1 1 calc R A 1 C5 C 0.9340(2) 0.0174(3) -0.2192(2) 0.0422(10) Uani 1 1 d . A 1 H5 H 0.9602 -0.0455 -0.2083 0.051 Uiso 1 1 calc R A 1 C6 C 0.9418(2) 0.0767(3) -0.2764(2) 0.0419(10) Uani 1 1 d . A 1 H6 H 0.9733 0.0551 -0.3052 0.05 Uiso 1 1 calc R A 1 C7 C 0.90352(19) 0.1680(3) -0.29193(19) 0.0373(10) Uani 1 1 d . A 1 H7 H 0.9092 0.2095 -0.3311 0.045 Uiso 1 1 calc R A 1 C8 C 0.85707(18) 0.1992(3) -0.25083(17) 0.0296(9) Uani 1 1 d . A 1 H8 H 0.8305 0.2617 -0.2625 0.036 Uiso 1 1 calc R A 1 C9 C 0.6399(2) 0.1954(3) -0.3319(2) 0.0500(11) Uani 1 1 d . A 1 H9C H 0.6117 0.1622 -0.3773 0.075 Uiso 1 1 calc R A 1 H9B H 0.6829 0.2307 -0.3405 0.075 Uiso 1 1 calc R A 1 H9A H 0.6083 0.2452 -0.3162 0.075 Uiso 1 1 calc R A 1 C10 C 0.7210(2) -0.0053(3) -0.2976(2) 0.0437(11) Uani 1 1 d . . 1 H10C H 0.684(2) -0.034(3) -0.340(2) 0.066 Uiso 1 1 d . C 1 H10B H 0.743(2) -0.057(3) -0.264(2) 0.066 Uiso 1 1 d . D 1 H10A H 0.762(2) 0.021(3) -0.312(2) 0.066 Uiso 1 1 d . E 1 C11 C 0.5874(2) 0.0338(3) -0.2439(2) 0.0427(10) Uani 1 1 d . A 1 H11C H 0.5585 0.0024 -0.2898 0.064 Uiso 1 1 calc R A 1 H11B H 0.557 0.0854 -0.2281 0.064 Uiso 1 1 calc R A 1 H11A H 0.6022 -0.0191 -0.206 0.064 Uiso 1 1 calc R A 1 C12 C 0.9284(2) 0.3688(3) 0.0137(2) 0.0388(10) Uani 1 1 d . A 1 H12C H 0.909(2) 0.428(3) -0.016(2) 0.058 Uiso 1 1 d . F 1 H12B H 0.974(2) 0.380(3) 0.037(2) 0.058 Uiso 1 1 d . G 1 H12A H 0.899(2) 0.364(3) 0.047(2) 0.058 Uiso 1 1 d . H 1 C13 C 0.9650(2) 0.1431(3) 0.0220(2) 0.0528(12) Uani 1 1 d . A 1 H13C H 0.9631 0.0794 -0.0058 0.079 Uiso 1 1 calc R A 1 H13B H 0.9371 0.1344 0.0584 0.079 Uiso 1 1 calc R A 1 H13A H 1.0167 0.1596 0.047 0.079 Uiso 1 1 calc R A 1 C14 C 0.9872(2) 0.2751(3) -0.1008(2) 0.0496(12) Uani 1 1 d . A 1 H14C H 0.9878 0.2156 -0.1321 0.074 Uiso 1 1 calc R A 1 H14B H 1.0374 0.2878 -0.0694 0.074 Uiso 1 1 calc R A 1 H14A H 0.9699 0.3354 -0.1315 0.074 Uiso 1 1 calc R A 1 C15 C 0.78275(18) 0.2366(3) 0.12153(18) 0.0247(8) Uani 1 1 d . A 1 H15 H 0.8061(17) 0.258(2) 0.0880(17) 0.03 Uiso 1 1 d . I 1 C16 C 0.70672(18) 0.2320(2) 0.09551(17) 0.0226(8) Uani 1 1 d . A 1 C17 C 0.66311(17) 0.2037(3) 0.14844(17) 0.0244(8) Uani 1 1 d . A 1 C18 C 0.64602(18) 0.2764(3) 0.19438(18) 0.0321(9) Uani 1 1 d . A 1 H18 H 0.665 0.344 0.1949 0.038 Uiso 1 1 calc R A 1 C19 C 0.6018(2) 0.2522(3) 0.23952(19) 0.0432(11) Uani 1 1 d . A 1 H19 H 0.5904 0.3032 0.2705 0.052 Uiso 1 1 calc R A 1 C20 C 0.5743(2) 0.1546(4) 0.2397(2) 0.0464(11) Uani 1 1 d . A 1 H20 H 0.543 0.1383 0.2699 0.056 Uiso 1 1 calc R A 1 C21 C 0.5922(2) 0.0813(3) 0.1962(2) 0.0466(11) Uani 1 1 d . A 1 H21 H 0.5744 0.0133 0.1973 0.056 Uiso 1 1 calc R A 1 C22 C 0.63626(19) 0.1052(3) 0.15043(19) 0.0351(9) Uani 1 1 d . A 1 H22 H 0.6481 0.0536 0.1202 0.042 Uiso 1 1 calc R A 1 C23 C 0.8242(2) 0.2667(3) 0.29220(19) 0.0505(12) Uani 1 1 d . A 1 H23C H 0.8615 0.2459 0.337 0.076 Uiso 1 1 calc R A 1 H23B H 0.7751 0.244 0.2946 0.076 Uiso 1 1 calc R A 1 H23A H 0.8245 0.3415 0.2876 0.076 Uiso 1 1 calc R A 1 C24 C 0.8548(2) 0.0664(3) 0.2300(2) 0.0539(12) Uani 1 1 d . A 1 H24C H 0.8891 0.0545 0.2785 0.081 Uiso 1 1 calc R A 1 H24B H 0.8737 0.0327 0.1926 0.081 Uiso 1 1 calc R A 1 H24A H 0.806 0.0381 0.2287 0.081 Uiso 1 1 calc R A 1 C25 C 0.93898(19) 0.2574(3) 0.2089(2) 0.0504(12) Uani 1 1 d . A 1 H25C H 0.9753 0.2437 0.256 0.076 Uiso 1 1 calc R A 1 H25B H 0.9357 0.3314 0.2 0.076 Uiso 1 1 calc R A 1 H25A H 0.9546 0.2233 0.1695 0.076 Uiso 1 1 calc R A 1 C26 C 0.5108(2) 0.2928(4) 0.0362(2) 0.0596(13) Uani 1 1 d . A 1 H26C H 0.5259 0.3609 0.0566 0.089 Uiso 1 1 calc R A 1 H26B H 0.512 0.2446 0.0761 0.089 Uiso 1 1 calc R A 1 H26A H 0.4603 0.2963 0.0035 0.089 Uiso 1 1 calc R A 1 C27 C 0.5602(2) 0.3362(4) -0.0975(2) 0.0467(11) Uani 1 1 d . A 1 H27C H 0.572(2) 0.406(3) -0.083(2) 0.07 Uiso 1 1 d . J 1 H27B H 0.508(2) 0.337(3) -0.125(2) 0.07 Uiso 1 1 d . K 1 H27A H 0.586(2) 0.312(3) -0.134(2) 0.07 Uiso 1 1 d . L 1 C28 C 0.5425(2) 0.1186(3) -0.0531(2) 0.0510(11) Uani 1 1 d . A 1 H28C H 0.575 0.0916 -0.0814 0.076 Uiso 1 1 calc R A 1 H28B H 0.4918 0.1239 -0.0849 0.076 Uiso 1 1 calc R A 1 H28A H 0.5434 0.0723 -0.0122 0.076 Uiso 1 1 calc R A 1 C29 C 0.6756(3) 0.5849(3) -0.0055(3) 0.0561(12) Uani 1 1 d . A 2 H29 H 0.6275 0.5974 -0.037 0.067 Uiso 1 1 calc R A 2 C30 C 0.7352(3) 0.6155(3) -0.0262(3) 0.0557(12) Uani 1 1 d . A 2 H30 H 0.7288 0.6485 -0.0722 0.067 Uiso 1 1 calc R A 2 C31 C 0.8035(3) 0.5997(3) 0.0175(3) 0.0573(12) Uani 1 1 d . A 2 H31 H 0.8452 0.6214 0.0021 0.069 Uiso 1 1 calc R A 2 C32 C 0.8142(3) 0.5534(4) 0.0830(3) 0.0616(13) Uani 1 1 d . A 2 H32 H 0.8631 0.5442 0.1136 0.074 Uiso 1 1 calc R A 2 C33 C 0.7547(4) 0.5193(4) 0.1061(2) 0.0692(15) Uani 1 1 d . A 2 H33 H 0.7621 0.4855 0.1519 0.083 Uiso 1 1 calc R A 2 C34 C 0.6826(3) 0.5358(4) 0.0602(3) 0.0670(15) Uani 1 1 d . A 2 H34 H 0.6401 0.5137 0.0742 0.08 Uiso 1 1 calc R A 2 C35 C 0.7604(3) -0.1290(3) 0.0701(2) 0.0492(11) Uani 1 1 d . A 2 H35 H 0.7677 -0.1315 0.1217 0.059 Uiso 1 1 calc R A 2 C36 C 0.8201(2) -0.1289(3) 0.0420(2) 0.0461(11) Uani 1 1 d . A 2 H36 H 0.8689 -0.1315 0.0741 0.055 Uiso 1 1 calc R A 2 C37 C 0.8101(2) -0.1251(3) -0.0324(2) 0.0452(11) Uani 1 1 d . A 2 H37 H 0.8519 -0.1254 -0.0516 0.054 Uiso 1 1 calc R A 2 C38 C 0.7394(3) -0.1208(3) -0.0794(2) 0.0467(11) Uani 1 1 d . A 2 H38 H 0.7321 -0.1179 -0.131 0.056 Uiso 1 1 calc R A 2 C39 C 0.6792(2) -0.1209(3) -0.0501(2) 0.0490(11) Uani 1 1 d . A 2 H39 H 0.6302 -0.1178 -0.0817 0.059 Uiso 1 1 calc R A 2 C40 C 0.6904(3) -0.1256(3) 0.0243(3) 0.0493(11) Uani 1 1 d . A 2 H40 H 0.6491 -0.1265 0.0441 0.059 Uiso 1 1 calc R A 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 K1 0.0400(5) 0.0228(4) 0.0353(5) -0.0016(4) 0.0185(4) 0.0004(4) K2 0.0338(5) 0.0252(5) 0.0468(5) 0.0034(4) 0.0182(4) 0.0020(4) Si1 0.0250(6) 0.0378(6) 0.0289(6) 0.0001(5) 0.0073(5) -0.0046(5) Si2 0.0229(6) 0.0341(6) 0.0305(6) -0.0045(5) 0.0067(5) -0.0007(5) Si3 0.0235(6) 0.0376(6) 0.0235(6) -0.0002(5) 0.0038(5) 0.0005(5) Si4 0.0202(5) 0.0387(6) 0.0284(6) -0.0028(5) 0.0035(4) 0.0005(5) N1 0.0226(16) 0.0279(17) 0.0224(16) -0.0047(14) 0.0058(13) -0.0010(13) N2 0.0222(16) 0.0316(17) 0.0200(16) 0.0003(13) 0.0074(13) 0.0022(14) C1 0.019(2) 0.033(2) 0.030(2) -0.0007(17) 0.0112(17) 0.0041(17) C2 0.025(2) 0.0199(19) 0.027(2) 0.0045(16) 0.0105(17) 0.0015(16) C3 0.0156(18) 0.026(2) 0.025(2) -0.0038(16) 0.0022(15) -0.0021(16) C4 0.037(2) 0.029(2) 0.036(2) -0.0001(18) 0.0162(19) 0.0018(19) C5 0.039(2) 0.038(2) 0.053(3) -0.004(2) 0.018(2) 0.012(2) C6 0.034(2) 0.057(3) 0.039(2) -0.014(2) 0.018(2) -0.001(2) C7 0.032(2) 0.055(3) 0.026(2) 0.0004(19) 0.0112(18) -0.005(2) C8 0.026(2) 0.037(2) 0.026(2) 0.0022(18) 0.0077(17) -0.0004(18) C9 0.042(3) 0.062(3) 0.041(2) 0.012(2) 0.003(2) -0.002(2) C10 0.038(3) 0.052(3) 0.040(3) -0.016(2) 0.009(2) -0.009(2) C11 0.032(2) 0.054(3) 0.041(2) 0.000(2) 0.0061(19) -0.008(2) C12 0.031(2) 0.043(3) 0.041(3) -0.003(2) 0.007(2) -0.003(2) C13 0.048(3) 0.045(3) 0.056(3) -0.003(2) -0.002(2) 0.012(2) C14 0.025(2) 0.074(3) 0.052(3) -0.018(2) 0.015(2) -0.015(2) C15 0.022(2) 0.034(2) 0.0192(19) 0.0014(16) 0.0076(16) -0.0019(17) C16 0.026(2) 0.0175(19) 0.025(2) -0.0031(15) 0.0086(17) 0.0018(16) C17 0.0185(19) 0.032(2) 0.0224(19) 0.0009(17) 0.0044(16) 0.0014(17) C18 0.027(2) 0.039(2) 0.032(2) -0.0069(18) 0.0088(18) -0.0010(18) C19 0.029(2) 0.073(3) 0.030(2) -0.013(2) 0.0111(19) 0.009(2) C20 0.034(2) 0.082(4) 0.028(2) 0.004(2) 0.0162(19) -0.005(2) C21 0.048(3) 0.049(3) 0.049(3) 0.007(2) 0.024(2) -0.013(2) C22 0.037(2) 0.039(2) 0.032(2) 0.0003(19) 0.0156(19) 0.000(2) C23 0.041(3) 0.077(3) 0.030(2) -0.008(2) 0.005(2) 0.007(2) C24 0.052(3) 0.054(3) 0.049(3) 0.009(2) 0.001(2) 0.006(2) C25 0.026(2) 0.084(3) 0.036(2) 0.014(2) -0.0002(19) -0.004(2) C26 0.024(2) 0.098(4) 0.053(3) -0.012(3) 0.003(2) 0.016(2) C27 0.034(3) 0.053(3) 0.041(3) 0.004(2) -0.011(2) -0.001(2) C28 0.040(2) 0.055(3) 0.053(3) -0.004(2) 0.003(2) -0.014(2) C29 0.045(3) 0.052(3) 0.066(3) -0.016(3) 0.008(3) 0.018(2) C30 0.071(4) 0.027(2) 0.065(3) -0.004(2) 0.011(3) 0.008(2) C31 0.061(3) 0.045(3) 0.066(3) -0.021(3) 0.017(3) -0.015(3) C32 0.050(3) 0.068(3) 0.054(3) -0.025(3) -0.006(3) 0.010(3) C33 0.118(5) 0.056(3) 0.039(3) -0.003(2) 0.031(3) 0.015(3) C34 0.070(4) 0.064(3) 0.087(4) -0.028(3) 0.056(3) -0.013(3) C35 0.076(3) 0.033(2) 0.045(3) 0.005(2) 0.026(3) -0.005(2) C36 0.050(3) 0.032(2) 0.053(3) 0.003(2) 0.007(2) 0.008(2) C37 0.058(3) 0.023(2) 0.067(3) -0.005(2) 0.037(3) 0.004(2) C38 0.086(4) 0.022(2) 0.036(2) -0.0029(18) 0.023(3) 0.003(2) C39 0.046(3) 0.028(2) 0.068(3) -0.009(2) 0.007(2) 0.000(2) C40 0.058(3) 0.037(3) 0.065(3) -0.007(2) 0.037(3) -0.012(2) #----------------------------------------------------------------------------# # 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 K1 N1 2.775(3) . ? K1 N2 2.783(3) . ? K1 C16 3.000(3) . ? K1 C15 3.002(3) . ? K1 C1 3.077(4) . ? K1 C2 3.087(3) . ? K1 C38 3.132(4) . ? K1 C37 3.139(4) . ? K1 C39 3.218(4) . ? K1 C36 3.233(4) . ? K1 C40 3.317(4) . ? K1 C35 3.321(4) . ? K2 N1 2.767(3) . ? K2 N2 2.776(3) . ? K2 C30 3.177(4) . ? K2 C29 3.215(4) . ? K2 C31 3.289(4) . ? K2 C27 3.303(5) . ? K2 C34 3.370(4) . ? K2 C12 3.391(4) . ? K2 C32 3.447(4) . ? K2 C33 3.483(4) . ? K2 C10 3.496(4) 4_765 ? K2 C2 3.500(3) . ? Si1 C1 1.835(4) . ? Si1 C9 1.872(4) . ? Si1 C10 1.873(4) . ? Si1 C11 1.878(4) . ? Si2 N1 1.697(3) . ? Si2 C12 1.869(4) . ? Si2 C13 1.871(4) . ? Si2 C14 1.877(4) . ? Si3 C15 1.831(3) . ? Si3 C23 1.862(4) . ? Si3 C24 1.872(4) . ? Si3 C25 1.873(4) . ? Si4 N2 1.704(3) . ? Si4 C28 1.870(4) . ? Si4 C26 1.872(4) . ? Si4 C27 1.874(4) . ? N1 C2 1.354(4) . ? N2 C16 1.357(4) . ? C1 C2 1.374(4) . ? C1 H1 0.93(3) . ? C2 C3 1.512(4) . ? C3 C4 1.385(5) . ? C3 C8 1.386(4) . ? C4 C5 1.387(5) . ? C4 H4 0.95 . ? C5 C6 1.373(5) . ? C5 H5 0.95 . ? C6 C7 1.380(5) . ? C6 H6 0.95 . ? C7 C8 1.380(5) . ? C7 H7 0.95 . ? C8 H8 0.95 . ? C9 H9C 0.98 . ? C9 H9B 0.98 . ? C9 H9A 0.98 . ? C10 K2 3.496(4) 4_755 ? C10 H10C 0.98(4) . ? C10 H10B 0.94(4) . ? C10 H10A 0.95(4) . ? C11 H11C 0.98 . ? C11 H11B 0.98 . ? C11 H11A 0.98 . ? C12 H12C 0.96(4) . ? C12 H12B 0.87(4) . ? C12 H12A 0.94(4) . ? C13 H13C 0.98 . ? C13 H13B 0.98 . ? C13 H13A 0.98 . ? C14 H14C 0.98 . ? C14 H14B 0.98 . ? C14 H14A 0.98 . ? C15 C16 1.377(4) . ? C15 H15 0.91(3) . ? C16 C17 1.504(4) . ? C17 C18 1.384(5) . ? C17 C22 1.385(5) . ? C18 C19 1.382(5) . ? C18 H18 0.95 . ? C19 C20 1.375(5) . ? C19 H19 0.95 . ? C20 C21 1.364(5) . ? C20 H20 0.95 . ? C21 C22 1.389(5) . ? C21 H21 0.95 . ? C22 H22 0.95 . ? C23 H23C 0.98 . ? C23 H23B 0.98 . ? C23 H23A 0.98 . ? C24 H24C 0.98 . ? C24 H24B 0.98 . ? C24 H24A 0.98 . ? C25 H25C 0.98 . ? C25 H25B 0.98 . ? C25 H25A 0.98 . ? C26 H26C 0.98 . ? C26 H26B 0.98 . ? C26 H26A 0.98 . ? C27 H27C 0.96(4) . ? C27 H27B 0.98(4) . ? C27 H27A 1.00(4) . ? C28 H28C 0.98 . ? C28 H28B 0.98 . ? C28 H28A 0.98 . ? C29 C30 1.343(6) . ? C29 C34 1.375(6) . ? C29 H29 0.95 . ? C30 C31 1.339(6) . ? C30 H30 0.95 . ? C31 C32 1.347(6) . ? C31 H31 0.95 . ? C32 C33 1.378(6) . ? C32 H32 0.95 . ? C33 C34 1.411(7) . ? C33 H33 0.95 . ? C34 H34 0.95 . ? C35 C40 1.362(6) . ? C35 C36 1.366(5) . ? C35 H35 0.95 . ? C36 C37 1.372(5) . ? C36 H36 0.95 . ? C37 C38 1.383(6) . ? C37 H37 0.95 . ? C38 C39 1.389(5) . ? C38 H38 0.95 . ? C39 C40 1.371(6) . ? C39 H39 0.95 . ? C40 H40 0.95 . ? 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 K1 N2 96.12(8) . . ? N1 K1 C16 106.27(8) . . ? N2 K1 C16 26.80(8) . . ? N1 K1 C15 94.05(9) . . ? N2 K1 C15 49.14(8) . . ? C16 K1 C15 26.52(8) . . ? N1 K1 C1 48.71(8) . . ? N2 K1 C1 95.40(9) . . ? C16 K1 C1 120.93(9) . . ? C15 K1 C1 129.05(10) . . ? N1 K1 C2 26.01(8) . . ? N2 K1 C2 105.38(8) . . ? C16 K1 C2 124.44(9) . . ? C15 K1 C2 118.68(9) . . ? C1 K1 C2 25.77(8) . . ? N1 K1 C38 110.37(9) . . ? N2 K1 C38 137.80(11) . . ? C16 K1 C38 142.52(10) . . ? C15 K1 C38 151.03(10) . . ? C1 K1 C38 79.82(10) . . ? C2 K1 C38 88.32(10) . . ? N1 K1 C37 105.70(9) . . ? N2 K1 C37 157.09(9) . . ? C16 K1 C37 143.30(10) . . ? C15 K1 C37 133.77(11) . . ? C1 K1 C37 93.84(10) . . ? C2 K1 C37 91.87(10) . . ? C38 K1 C37 25.47(10) . . ? N1 K1 C39 132.31(10) . . ? N2 K1 C39 114.73(10) . . ? C16 K1 C39 117.75(10) . . ? C15 K1 C39 133.63(11) . . ? C1 K1 C39 91.06(11) . . ? C2 K1 C39 107.35(11) . . ? C38 K1 C39 25.22(10) . . ? C37 K1 C39 44.08(11) . . ? N1 K1 C36 120.95(10) . . ? N2 K1 C36 140.46(10) . . ? C16 K1 C36 119.29(10) . . ? C15 K1 C36 110.06(10) . . ? C1 K1 C36 118.66(10) . . ? C2 K1 C36 113.99(10) . . ? C38 K1 C36 44.03(11) . . ? C37 K1 C36 24.82(10) . . ? C39 K1 C36 50.34(11) . . ? N1 K1 C40 153.62(9) . . ? N2 K1 C40 107.02(9) . . ? C16 K1 C40 100.07(9) . . ? C15 K1 C40 110.55(10) . . ? C1 K1 C40 115.01(11) . . ? C2 K1 C40 130.76(10) . . ? C38 K1 C40 43.38(10) . . ? C37 K1 C40 50.17(10) . . ? C39 K1 C40 24.16(10) . . ? C36 K1 C40 42.27(11) . . ? N1 K1 C35 144.94(10) . . ? N2 K1 C35 117.53(9) . . ? C16 K1 C35 100.70(10) . . ? C15 K1 C35 100.53(10) . . ? C1 K1 C35 130.16(10) . . ? C2 K1 C35 134.82(10) . . ? C38 K1 C35 50.50(10) . . ? C37 K1 C35 43.04(10) . . ? C39 K1 C35 42.54(11) . . ? C36 K1 C35 24.01(10) . . ? C40 K1 C35 23.69(10) . . ? N1 K2 N2 96.47(8) . . ? N1 K2 C30 141.13(11) . . ? N2 K2 C30 117.52(11) . . ? N1 K2 C29 164.53(11) . . ? N2 K2 C29 94.79(11) . . ? C30 K2 C29 24.25(11) . . ? N1 K2 C31 122.71(10) . . ? N2 K2 C31 119.34(10) . . ? C30 K2 C31 23.82(11) . . ? C29 K2 C31 41.91(12) . . ? N1 K2 C27 119.00(10) . . ? N2 K2 C27 55.42(9) . . ? C30 K2 C27 96.72(12) . . ? C29 K2 C27 76.24(12) . . ? C31 K2 C27 118.10(12) . . ? N1 K2 C34 154.23(12) . . ? N2 K2 C34 75.50(10) . . ? C30 K2 C34 42.35(12) . . ? C29 K2 C34 23.95(11) . . ? C31 K2 C34 48.56(11) . . ? C27 K2 C34 76.96(12) . . ? N1 K2 C12 54.60(9) . . ? N2 K2 C12 113.55(10) . . ? C30 K2 C12 92.60(12) . . ? C29 K2 C12 110.92(11) . . ? C31 K2 C12 69.92(11) . . ? C27 K2 C12 168.16(11) . . ? C34 K2 C12 105.60(12) . . ? N1 K2 C32 119.40(10) . . ? N2 K2 C32 99.45(11) . . ? C30 K2 C32 41.08(11) . . ? C29 K2 C32 47.89(11) . . ? C31 K2 C32 22.91(11) . . ? C27 K2 C32 118.11(12) . . ? C34 K2 C32 41.15(11) . . ? C12 K2 C32 65.44(11) . . ? N1 K2 C33 131.34(11) . . ? N2 K2 C33 78.61(11) . . ? C30 K2 C33 48.33(12) . . ? C29 K2 C33 41.53(11) . . ? C31 K2 C33 40.81(12) . . ? C27 K2 C33 97.97(14) . . ? C34 K2 C33 23.70(11) . . ? C12 K2 C33 82.79(13) . . ? C32 K2 C33 22.94(11) . . ? N1 K2 C10 82.16(9) . 4_765 ? N2 K2 C10 158.07(10) . 4_765 ? C30 K2 C10 73.03(12) . 4_765 ? C29 K2 C10 91.27(12) . 4_765 ? C31 K2 C10 78.47(12) . 4_765 ? C27 K2 C10 106.09(11) . 4_765 ? C34 K2 C10 114.35(12) . 4_765 ? C12 K2 C10 83.60(11) . 4_765 ? C32 K2 C10 100.24(13) . 4_765 ? C33 K2 C10 118.65(12) . 4_765 ? N1 K2 C2 21.08(7) . . ? N2 K2 C2 95.54(8) . . ? C30 K2 C2 146.89(11) . . ? C29 K2 C2 165.24(11) . . ? C31 K2 C2 137.44(10) . . ? C27 K2 C2 101.19(10) . . ? C34 K2 C2 170.31(11) . . ? C12 K2 C2 74.29(9) . . ? C32 K2 C2 139.72(10) . . ? C33 K2 C2 151.83(11) . . ? C10 K2 C2 75.34(9) 4_765 . ? C1 Si1 C9 111.18(18) . . ? C1 Si1 C10 116.10(18) . . ? C9 Si1 C10 106.97(19) . . ? C1 Si1 C11 108.87(16) . . ? C9 Si1 C11 107.19(18) . . ? C10 Si1 C11 106.07(19) . . ? N1 Si2 C12 107.51(17) . . ? N1 Si2 C13 110.42(16) . . ? C12 Si2 C13 107.72(19) . . ? N1 Si2 C14 119.12(16) . . ? C12 Si2 C14 104.23(19) . . ? C13 Si2 C14 107.19(19) . . ? C15 Si3 C23 116.51(17) . . ? C15 Si3 C24 112.45(17) . . ? C23 Si3 C24 106.30(19) . . ? C15 Si3 C25 105.98(16) . . ? C23 Si3 C25 106.93(19) . . ? C24 Si3 C25 108.3(2) . . ? N2 Si4 C28 112.12(16) . . ? N2 Si4 C26 119.01(16) . . ? C28 Si4 C26 106.2(2) . . ? N2 Si4 C27 106.33(17) . . ? C28 Si4 C27 106.8(2) . . ? C26 Si4 C27 105.6(2) . . ? C2 N1 Si2 130.3(2) . . ? C2 N1 K2 111.6(2) . . ? Si2 N1 K2 112.04(12) . . ? C2 N1 K1 89.94(18) . . ? Si2 N1 K1 117.30(13) . . ? K2 N1 K1 83.85(7) . . ? C16 N2 Si4 130.3(2) . . ? C16 N2 K2 114.7(2) . . ? Si4 N2 K2 110.54(12) . . ? C16 N2 K1 85.53(18) . . ? Si4 N2 K1 119.51(13) . . ? K2 N2 K1 83.53(7) . . ? C2 C1 Si1 131.2(3) . . ? C2 C1 K1 77.53(19) . . ? Si1 C1 K1 135.13(16) . . ? C2 C1 H1 116(2) . . ? Si1 C1 H1 112(2) . . ? K1 C1 H1 59(2) . . ? N1 C2 C1 125.8(3) . . ? N1 C2 C3 117.8(3) . . ? C1 C2 C3 116.3(3) . . ? N1 C2 K1 64.05(16) . . ? C1 C2 K1 76.71(19) . . ? C3 C2 K1 135.9(2) . . ? N1 C2 K2 47.32(15) . . ? C1 C2 K2 84.8(2) . . ? C3 C2 K2 149.0(2) . . ? K1 C2 K2 68.09(7) . . ? C4 C3 C8 118.3(3) . . ? C4 C3 C2 121.2(3) . . ? C8 C3 C2 120.5(3) . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 120.0(4) . . ? C6 C5 H5 120 . . ? C4 C5 H5 120 . . ? C5 C6 C7 119.6(3) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C8 120.4(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C3 120.7(3) . . ? C7 C8 H8 119.6 . . ? C3 C8 H8 119.6 . . ? Si1 C9 H9C 109.5 . . ? Si1 C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? Si1 C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? Si1 C10 K2 150.2(2) . 4_755 ? Si1 C10 H10C 107(2) . . ? K2 C10 H10C 54(2) 4_755 . ? Si1 C10 H10B 114(3) . . ? K2 C10 H10B 95(3) 4_755 . ? H10C C10 H10B 111(4) . . ? Si1 C10 H10A 113(3) . . ? K2 C10 H10A 64(2) 4_755 . ? H10C C10 H10A 110(3) . . ? H10B C10 H10A 103(4) . . ? Si1 C11 H11C 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11C C11 H11B 109.5 . . ? Si1 C11 H11A 109.5 . . ? H11C C11 H11A 109.5 . . ? H11B C11 H11A 109.5 . . ? Si2 C12 K2 85.81(15) . . ? Si2 C12 H12C 113(2) . . ? K2 C12 H12C 65(2) . . ? Si2 C12 H12B 109(3) . . ? K2 C12 H12B 165(3) . . ? H12C C12 H12B 109(4) . . ? Si2 C12 H12A 112(2) . . ? K2 C12 H12A 61(2) . . ? H12C C12 H12A 104(3) . . ? H12B C12 H12A 110(3) . . ? Si2 C13 H13C 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? Si2 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? Si2 C14 H14C 109.5 . . ? Si2 C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? Si2 C14 H14A 109.5 . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C16 C15 Si3 132.0(3) . . ? C16 C15 K1 76.68(19) . . ? Si3 C15 K1 123.79(16) . . ? C16 C15 H15 114(2) . . ? Si3 C15 H15 114(2) . . ? K1 C15 H15 67(2) . . ? N2 C16 C15 124.0(3) . . ? N2 C16 C17 117.9(3) . . ? C15 C16 C17 118.0(3) . . ? N2 C16 K1 67.66(16) . . ? C15 C16 K1 76.80(19) . . ? C17 C16 K1 129.2(2) . . ? C18 C17 C22 118.1(3) . . ? C18 C17 C16 120.9(3) . . ? C22 C17 C16 121.0(3) . . ? C19 C18 C17 121.0(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C20 C19 C18 120.2(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C21 C20 C19 119.6(3) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C20 C21 C22 120.5(4) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 120.6(3) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? Si3 C23 H23C 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? Si3 C23 H23A 109.5 . . ? H23C C23 H23A 109.5 . . ? H23B C23 H23A 109.5 . . ? Si3 C24 H24C 109.5 . . ? Si3 C24 H24B 109.5 . . ? H24C C24 H24B 109.5 . . ? Si3 C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? Si3 C25 H25C 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25C C25 H25B 109.5 . . ? Si3 C25 H25A 109.5 . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? Si4 C26 H26C 109.5 . . ? Si4 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? Si4 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? Si4 C27 K2 87.70(15) . . ? Si4 C27 H27C 112(3) . . ? K2 C27 H27C 69(3) . . ? Si4 C27 H27B 111(2) . . ? K2 C27 H27B 161(2) . . ? H27C C27 H27B 105(3) . . ? Si4 C27 H27A 113(2) . . ? K2 C27 H27A 65(2) . . ? H27C C27 H27A 113(4) . . ? H27B C27 H27A 103(3) . . ? Si4 C28 H28C 109.5 . . ? Si4 C28 H28B 109.5 . . ? H28C C28 H28B 109.5 . . ? Si4 C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? C30 C29 C34 121.5(4) . . ? C30 C29 K2 76.3(2) . . ? C34 C29 K2 84.4(3) . . ? C30 C29 H29 119.2 . . ? C34 C29 H29 119.2 . . ? K2 C29 H29 110.1 . . ? C31 C30 C29 120.4(5) . . ? C31 C30 K2 82.8(3) . . ? C29 C30 K2 79.5(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? K2 C30 H30 108 . . ? C30 C31 C32 121.0(5) . . ? C30 C31 K2 73.4(2) . . ? C32 C31 K2 85.1(3) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? K2 C31 H31 112.1 . . ? C31 C32 C33 120.7(5) . . ? C31 C32 K2 71.9(2) . . ? C33 C32 K2 80.0(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? K2 C32 H32 119.3 . . ? C32 C33 C34 118.5(4) . . ? C32 C33 K2 77.1(2) . . ? C34 C33 K2 73.7(2) . . ? C32 C33 H33 120.8 . . ? C34 C33 H33 120.8 . . ? K2 C33 H33 119.6 . . ? C29 C34 C33 117.9(4) . . ? C29 C34 K2 71.7(2) . . ? C33 C34 K2 82.6(3) . . ? C29 C34 H34 121 . . ? C33 C34 H34 121 . . ? K2 C34 H34 115.4 . . ? C40 C35 C36 120.0(4) . . ? C40 C35 K1 78.0(2) . . ? C36 C35 K1 74.4(2) . . ? C40 C35 H35 120 . . ? C36 C35 H35 120 . . ? K1 C35 H35 118.5 . . ? C35 C36 C37 120.4(4) . . ? C35 C36 K1 81.6(2) . . ? C37 C36 K1 73.8(2) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? K1 C36 H36 115.3 . . ? C36 C37 C38 120.2(4) . . ? C36 C37 K1 81.4(2) . . ? C38 C37 K1 77.0(2) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? K1 C37 H37 112.1 . . ? C37 C38 C39 118.9(4) . . ? C37 C38 K1 77.6(2) . . ? C39 C38 K1 80.9(2) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? K1 C38 H38 111.6 . . ? C40 C39 C38 120.0(4) . . ? C40 C39 K1 82.0(2) . . ? C38 C39 K1 73.9(2) . . ? C40 C39 H39 120 . . ? C38 C39 H39 120 . . ? K1 C39 H39 114.6 . . ? C35 C40 C39 120.6(4) . . ? C35 C40 K1 78.3(2) . . ? C39 C40 K1 73.9(2) . . ? C35 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? K1 C40 H40 119 . . ? #===END data_(11)-mar898 _database_code_depnum_ccdc_archive 'CCDC 297455' _audit_creation_date 2005-12-16T15:37:39-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H58 N4 Ni Si4' _chemical_formula_sum 'C42 H58 N4 Ni Si4' _chemical_formula_weight 789.99 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 11.439(6) _cell_length_b 12.954(6) _cell_length_c 30.37(3) _cell_angle_alpha 90 _cell_angle_beta 97.85(6) _cell_angle_gamma 90 _cell_volume 4458(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.575 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_max 1.00 _exptl_absorpt_correction_min 0.87 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _diffrn_measurement_method \w--2\q _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_unetI/netI 0.1039 _diffrn_reflns_number 6560 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 23.42 _diffrn_reflns_theta_full 23.42 _diffrn_measured_fraction_theta_full 0.95 _diffrn_measured_fraction_theta_max 0.95 _reflns_number_total 6217 _reflns_number_gt 3832 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # 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^)+(0.0484P)^2^+39.7210P] 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_number_reflns 6217 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1486 _refine_ls_R_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.2267 _refine_ls_wR_factor_gt 0.1684 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.194 _refine_diff_density_min -1.612 _refine_diff_density_rms 0.122 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 Ni Ni 0.21072(10) 0.19930(8) 0.09271(4) 0.0311(3) Uani 1 1 d . . . Si1 Si 0.3569(3) -0.01433(18) 0.07544(8) 0.0396(7) Uani 1 1 d . . . Si2 Si -0.1123(3) 0.1144(2) 0.15190(10) 0.0510(8) Uani 1 1 d . . . Si3 Si 0.1919(2) 0.22193(19) -0.01753(8) 0.0366(6) Uani 1 1 d . . . Si4 Si 0.4580(3) 0.4743(2) 0.13796(10) 0.0488(8) Uani 1 1 d . . . N1 N 0.2370(6) 0.0507(5) 0.0920(2) 0.0319(17) Uani 1 1 d . . . N2 N 0.1711(7) 0.1367(5) 0.1447(2) 0.0372(19) Uani 1 1 d . . . N3 N 0.2345(6) 0.2621(5) 0.0368(2) 0.0334(18) Uani 1 1 d . . . N4 N 0.2021(6) 0.3454(5) 0.0959(2) 0.0273(16) Uani 1 1 d . . . C1 C 0.1988(8) 0.0445(7) 0.1316(3) 0.035(2) Uani 1 1 d . . . C2 C 0.1307(9) 0.1643(6) 0.1851(3) 0.040(2) Uani 1 1 d . . . C3 C 0.2280(10) 0.2034(7) 0.2187(3) 0.047(3) Uani 1 1 d . . . C4 C 0.2109(12) 0.2348(9) 0.2607(4) 0.080(4) Uani 1 1 d . . . H4 H 0.1336 0.2345 0.2688 0.096 Uiso 1 1 calc R . . C5 C 0.3080(15) 0.2679(10) 0.2923(4) 0.095(5) Uani 1 1 d . . . H5 H 0.2961 0.2889 0.3214 0.114 Uiso 1 1 calc R . . C6 C 0.4195(15) 0.2685(10) 0.2796(5) 0.088(5) Uani 1 1 d . . . H6 H 0.4841 0.2924 0.3001 0.105 Uiso 1 1 calc R . . C7 C 0.4395(12) 0.2365(10) 0.2394(4) 0.081(4) Uani 1 1 d . . . H7 H 0.5174 0.2351 0.2319 0.097 Uiso 1 1 calc R . . C8 C 0.3453(11) 0.2056(8) 0.2089(4) 0.063(3) Uani 1 1 d . . . H8 H 0.3599 0.1849 0.1802 0.076 Uiso 1 1 calc R . . C9 C 0.0160(9) 0.1587(7) 0.1909(3) 0.040(2) Uani 1 1 d . . . H9 H -0.0012 0.1808 0.2191 0.048 Uiso 1 1 calc R . . C10 C 0.1868(8) -0.0537(6) 0.1549(3) 0.038(2) Uani 1 1 d . . . C11 C 0.1470(9) -0.1413(7) 0.1305(3) 0.050(3) Uani 1 1 d . . . H11 H 0.1265 -0.1358 0.0992 0.06 Uiso 1 1 calc R . . C12 C 0.1371(11) -0.2351(7) 0.1507(4) 0.066(3) Uani 1 1 d . . . H12 H 0.1088 -0.2936 0.1336 0.079 Uiso 1 1 calc R . . C13 C 0.1683(10) -0.2439(8) 0.1961(4) 0.062(3) Uani 1 1 d . . . H13 H 0.1623 -0.3086 0.2103 0.075 Uiso 1 1 calc R . . C14 C 0.2081(10) -0.1586(7) 0.2206(3) 0.057(3) Uani 1 1 d . . . H14 H 0.2296 -0.1649 0.2518 0.069 Uiso 1 1 calc R . . C15 C 0.2173(8) -0.0646(7) 0.2008(3) 0.043(2) Uani 1 1 d . . . H15 H 0.2447 -0.0065 0.2183 0.052 Uiso 1 1 calc R . . C16 C 0.3098(10) -0.0919(8) 0.0253(3) 0.056(3) Uani 1 1 d . . . H16A H 0.2508 -0.1426 0.0317 0.084 Uiso 1 1 calc R . . H16B H 0.3782 -0.1278 0.0164 0.084 Uiso 1 1 calc R . . H16C H 0.2753 -0.0464 0.0012 0.084 Uiso 1 1 calc R . . C17 C 0.4316(11) -0.1012(9) 0.1197(4) 0.072(4) Uani 1 1 d . . . H17A H 0.376 -0.1544 0.1267 0.108 Uiso 1 1 calc R . . H17B H 0.4581 -0.0607 0.1464 0.108 Uiso 1 1 calc R . . H17C H 0.4997 -0.1341 0.1091 0.108 Uiso 1 1 calc R . . C18 C 0.4680(8) 0.0822(7) 0.0647(3) 0.048(3) Uani 1 1 d . . . H18A H 0.492 0.1224 0.0917 0.072 Uiso 1 1 calc R . . H18B H 0.4341 0.1284 0.0407 0.072 Uiso 1 1 calc R . . H18C H 0.537 0.0469 0.0558 0.072 Uiso 1 1 calc R . . C19 C -0.2409(10) 0.1789(10) 0.1700(4) 0.083(4) Uani 1 1 d . . . H19A H -0.3125 0.1584 0.1505 0.124 Uiso 1 1 calc R . . H19B H -0.2309 0.2539 0.1685 0.124 Uiso 1 1 calc R . . H19C H -0.2476 0.1588 0.2007 0.124 Uiso 1 1 calc R . . C20 C -0.0999(10) 0.1439(9) 0.0930(3) 0.064(3) Uani 1 1 d . . . H20A H -0.0309 0.1085 0.0844 0.096 Uiso 1 1 calc R . . H20B H -0.0911 0.2186 0.0895 0.096 Uiso 1 1 calc R . . H20C H -0.1712 0.1203 0.0741 0.096 Uiso 1 1 calc R . . C21 C -0.1361(11) -0.0273(9) 0.1576(4) 0.081(4) Uani 1 1 d . . . H21A H -0.0693 -0.065 0.1483 0.122 Uiso 1 1 calc R . . H21B H -0.209 -0.0476 0.1388 0.122 Uiso 1 1 calc R . . H21C H -0.1425 -0.0436 0.1887 0.122 Uiso 1 1 calc R . . C22 C 0.2274(7) 0.3554(6) 0.0550(3) 0.030(2) Uani 1 1 d . . . C23 C 0.2084(8) 0.4230(6) 0.1299(3) 0.037(2) Uani 1 1 d . . . C24 C 0.0938(9) 0.4369(6) 0.1475(3) 0.040(2) Uani 1 1 d . . . C25 C 0.0911(10) 0.4605(8) 0.1915(3) 0.056(3) Uani 1 1 d . . . H25 H 0.1629 0.4623 0.2114 0.067 Uiso 1 1 calc R . . C26 C -0.0156(12) 0.4821(9) 0.2077(4) 0.067(3) Uani 1 1 d . . . H26 H -0.0164 0.4988 0.2381 0.081 Uiso 1 1 calc R . . C27 C -0.1189(13) 0.4785(10) 0.1787(5) 0.082(4) Uani 1 1 d . . . H27 H -0.1915 0.4944 0.1891 0.098 Uiso 1 1 calc R . . C28 C -0.1185(10) 0.4529(9) 0.1359(4) 0.063(3) Uani 1 1 d . . . H28 H -0.1907 0.4499 0.1164 0.075 Uiso 1 1 calc R . . C29 C -0.0126(9) 0.4307(7) 0.1200(3) 0.045(3) Uani 1 1 d . . . H29 H -0.0137 0.411 0.0898 0.055 Uiso 1 1 calc R . . C30 C 0.3064(7) 0.4792(7) 0.1452(3) 0.039(2) Uani 1 1 d . . . H30 H 0.2898 0.534 0.1642 0.047 Uiso 1 1 calc R . . C31 C 0.2446(8) 0.4536(6) 0.0323(3) 0.034(2) Uani 1 1 d . . . C32 C 0.3287(8) 0.4599(7) 0.0040(3) 0.037(2) Uani 1 1 d . . . H32 H 0.377 0.4018 0.0003 0.044 Uiso 1 1 calc R . . C33 C 0.3433(9) 0.5493(7) -0.0188(3) 0.044(2) Uani 1 1 d . . . H33 H 0.4028 0.5527 -0.0378 0.053 Uiso 1 1 calc R . . C34 C 0.2737(9) 0.6333(7) -0.0148(3) 0.050(3) Uani 1 1 d . . . H34 H 0.2842 0.6946 -0.031 0.06 Uiso 1 1 calc R . . C35 C 0.1882(10) 0.6283(7) 0.0129(3) 0.053(3) Uani 1 1 d . . . H35 H 0.1382 0.6859 0.0156 0.064 Uiso 1 1 calc R . . C36 C 0.1756(8) 0.5392(7) 0.0367(3) 0.043(2) Uani 1 1 d . . . H36 H 0.118 0.5367 0.0564 0.051 Uiso 1 1 calc R . . C37 C 0.0844(9) 0.1163(7) -0.0152(3) 0.052(3) Uani 1 1 d . . . H37A H 0.0173 0.1416 -0.0013 0.078 Uiso 1 1 calc R . . H37B H 0.1224 0.0591 0.0024 0.078 Uiso 1 1 calc R . . H37C H 0.0564 0.0922 -0.0454 0.078 Uiso 1 1 calc R . . C38 C 0.3198(9) 0.1758(8) -0.0435(3) 0.052(3) Uani 1 1 d . . . H38A H 0.3761 0.2324 -0.0446 0.077 Uiso 1 1 calc R . . H38B H 0.2925 0.1517 -0.0738 0.077 Uiso 1 1 calc R . . H38C H 0.3583 0.1188 -0.026 0.077 Uiso 1 1 calc R . . C39 C 0.1181(9) 0.3262(7) -0.0535(3) 0.053(3) Uani 1 1 d . . . H39A H 0.1735 0.3832 -0.0552 0.079 Uiso 1 1 calc R . . H39B H 0.0491 0.3512 -0.0408 0.079 Uiso 1 1 calc R . . H39C H 0.0929 0.2988 -0.0834 0.079 Uiso 1 1 calc R . . C40 C 0.5010(9) 0.3506(8) 0.1128(4) 0.055(3) Uani 1 1 d . . . H40A H 0.5852 0.3526 0.1097 0.083 Uiso 1 1 calc R . . H40B H 0.4546 0.3416 0.0834 0.083 Uiso 1 1 calc R . . H40C H 0.4858 0.2927 0.132 0.083 Uiso 1 1 calc R . . C41 C 0.4977(10) 0.5887(7) 0.1059(4) 0.056(3) Uani 1 1 d . . . H41A H 0.5813 0.5851 0.1021 0.083 Uiso 1 1 calc R . . H41B H 0.4831 0.6519 0.122 0.083 Uiso 1 1 calc R . . H41C H 0.4494 0.5893 0.0766 0.083 Uiso 1 1 calc R . . C42 C 0.5404(9) 0.4839(9) 0.1958(3) 0.062(3) Uani 1 1 d . . . H42A H 0.6255 0.4816 0.1945 0.094 Uiso 1 1 calc R . . H42B H 0.5182 0.4261 0.2138 0.094 Uiso 1 1 calc R . . H42C H 0.5204 0.5492 0.2094 0.094 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 Ni 0.0449(7) 0.0216(6) 0.0261(6) 0.0036(5) 0.0023(5) 0.0040(5) Si1 0.0600(18) 0.0245(13) 0.0328(14) 0.0022(11) 0.0012(13) 0.0087(12) Si2 0.0568(19) 0.0485(17) 0.0467(18) -0.0079(14) 0.0032(15) -0.0076(15) Si3 0.0465(16) 0.0307(14) 0.0305(14) 0.0032(11) -0.0016(12) 0.0027(12) Si4 0.0526(18) 0.0393(16) 0.0518(18) -0.0019(14) -0.0021(14) -0.0114(14) N1 0.046(5) 0.023(4) 0.025(4) 0.008(3) 0.000(3) 0.008(3) N2 0.059(5) 0.023(4) 0.028(4) 0.004(3) 0.001(4) 0.005(4) N3 0.039(4) 0.025(4) 0.035(4) 0.005(3) 0.003(3) 0.008(3) N4 0.024(4) 0.029(4) 0.030(4) 0.007(3) 0.006(3) -0.002(3) C1 0.043(6) 0.033(5) 0.027(5) 0.006(4) -0.007(4) -0.002(4) C2 0.069(7) 0.027(5) 0.023(5) -0.002(4) 0.006(5) -0.013(5) C3 0.075(8) 0.024(5) 0.038(6) -0.001(5) -0.009(5) -0.005(5) C4 0.101(10) 0.076(8) 0.053(7) -0.032(7) -0.026(7) 0.036(8) C5 0.128(13) 0.082(10) 0.061(9) -0.039(7) -0.035(9) 0.041(10) C6 0.107(12) 0.059(8) 0.081(11) -0.013(7) -0.043(9) -0.005(8) C7 0.086(10) 0.079(9) 0.066(9) 0.012(7) -0.031(7) -0.034(7) C8 0.081(9) 0.059(7) 0.043(6) 0.013(6) -0.017(6) -0.024(7) C9 0.055(7) 0.034(5) 0.032(5) -0.003(4) 0.007(5) -0.008(5) C10 0.050(6) 0.023(5) 0.037(5) 0.006(4) -0.006(5) -0.003(4) C11 0.071(7) 0.034(5) 0.040(6) 0.009(5) -0.018(5) -0.012(5) C12 0.102(10) 0.031(6) 0.056(7) 0.004(5) -0.016(7) -0.030(6) C13 0.093(9) 0.033(6) 0.057(7) 0.012(5) 0.000(6) -0.008(6) C14 0.095(9) 0.040(6) 0.033(6) 0.009(5) -0.002(6) -0.005(6) C15 0.056(6) 0.027(5) 0.041(6) 0.005(4) -0.012(5) -0.005(5) C16 0.070(8) 0.040(6) 0.056(7) -0.009(5) 0.003(6) 0.002(5) C17 0.091(9) 0.057(7) 0.068(8) 0.028(6) 0.009(7) 0.033(7) C18 0.045(6) 0.046(6) 0.054(6) -0.002(5) 0.009(5) 0.007(5) C19 0.050(7) 0.105(11) 0.088(9) -0.027(8) -0.009(7) 0.002(7) C20 0.059(7) 0.074(8) 0.055(7) 0.001(6) -0.007(6) -0.032(6) C21 0.083(9) 0.067(8) 0.090(10) -0.009(7) -0.003(8) -0.017(7) C22 0.033(5) 0.020(5) 0.035(5) 0.006(4) 0.003(4) 0.002(4) C23 0.049(6) 0.028(5) 0.033(5) 0.007(4) 0.006(5) 0.015(4) C24 0.068(7) 0.021(5) 0.032(5) -0.004(4) 0.008(5) -0.001(5) C25 0.074(8) 0.046(6) 0.048(7) -0.010(5) 0.011(6) -0.014(6) C26 0.085(9) 0.067(8) 0.055(8) -0.026(6) 0.030(7) -0.007(7) C27 0.088(11) 0.065(8) 0.100(11) 0.007(8) 0.045(9) 0.007(8) C28 0.060(8) 0.063(8) 0.066(8) 0.021(6) 0.009(6) 0.013(6) C29 0.053(7) 0.050(6) 0.034(5) 0.010(5) 0.008(5) 0.012(5) C30 0.033(5) 0.029(5) 0.052(6) -0.005(4) -0.003(4) -0.018(4) C31 0.044(6) 0.028(5) 0.029(5) 0.001(4) -0.001(4) -0.003(4) C32 0.054(6) 0.025(5) 0.029(5) -0.003(4) -0.004(5) 0.001(4) C33 0.055(6) 0.042(6) 0.034(5) 0.000(5) 0.002(5) -0.010(5) C34 0.069(7) 0.030(6) 0.051(6) 0.012(5) 0.010(6) -0.011(5) C35 0.070(7) 0.027(5) 0.066(7) 0.015(5) 0.023(6) 0.010(5) C36 0.050(6) 0.028(5) 0.052(6) 0.006(5) 0.016(5) 0.002(5) C37 0.057(7) 0.042(6) 0.053(6) 0.002(5) -0.006(5) -0.009(5) C38 0.053(7) 0.055(6) 0.045(6) -0.002(5) 0.001(5) 0.011(5) C39 0.051(6) 0.050(6) 0.052(6) 0.017(5) -0.011(5) -0.002(5) C40 0.046(6) 0.049(6) 0.067(7) 0.012(6) -0.005(5) -0.006(5) C41 0.064(7) 0.041(6) 0.063(7) -0.006(5) 0.011(6) -0.016(5) C42 0.057(7) 0.064(7) 0.062(7) -0.003(6) -0.009(6) -0.016(6) #----------------------------------------------------------------------------# # 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 Ni N2 1.885(7) . ? Ni N4 1.898(7) . ? Ni N3 1.934(7) . ? Ni N1 1.949(6) . ? Ni C1 2.341(9) . ? Ni C22 2.344(8) . ? Si1 N1 1.741(7) . ? Si1 C16 1.841(10) . ? Si1 C18 1.844(10) . ? Si1 C17 1.868(10) . ? Si2 C19 1.840(12) . ? Si2 C9 1.848(10) . ? Si2 C20 1.852(11) . ? Si2 C21 1.867(12) . ? Si3 N3 1.737(8) . ? Si3 C37 1.847(9) . ? Si3 C38 1.854(10) . ? Si3 C39 1.864(9) . ? Si4 C30 1.779(9) . ? Si4 C41 1.864(10) . ? Si4 C40 1.870(10) . ? Si4 C42 1.882(10) . ? N1 C1 1.337(11) . ? N2 C1 1.312(11) . ? N2 C2 1.415(11) . ? N3 C22 1.335(10) . ? N4 C22 1.321(10) . ? N4 C23 1.437(11) . ? C1 C10 1.472(12) . ? C2 C9 1.349(13) . ? C2 C3 1.492(13) . ? C3 C4 1.380(14) . ? C3 C8 1.412(15) . ? C4 C5 1.430(17) . ? C4 H4 0.95 . ? C5 C6 1.382(19) . ? C5 H5 0.95 . ? C6 C7 1.340(18) . ? C6 H6 0.95 . ? C7 C8 1.380(14) . ? C7 H7 0.95 . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 C15 1.395(12) . ? C10 C11 1.398(12) . ? C11 C12 1.374(13) . ? C11 H11 0.95 . ? C12 C13 1.380(14) . ? C12 H12 0.95 . ? C13 C14 1.375(14) . ? C13 H13 0.95 . ? C14 C15 1.368(12) . ? C14 H14 0.95 . ? C15 H15 0.95 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C31 1.473(11) . ? C23 C30 1.364(12) . ? C23 C24 1.492(13) . ? C24 C25 1.374(13) . ? C24 C29 1.382(13) . ? C25 C26 1.405(15) . ? C25 H25 0.95 . ? C26 C27 1.374(17) . ? C26 H26 0.95 . ? C27 C28 1.343(16) . ? C27 H27 0.95 . ? C28 C29 1.394(14) . ? C28 H28 0.95 . ? C29 H29 0.95 . ? C30 H30 0.95 . ? C31 C32 1.377(12) . ? C31 C36 1.378(12) . ? C32 C33 1.371(12) . ? C32 H32 0.95 . ? C33 C34 1.364(13) . ? C33 H33 0.95 . ? C34 C35 1.375(13) . ? C34 H34 0.95 . ? C35 C36 1.381(12) . ? C35 H35 0.95 . ? C36 H36 0.95 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? 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 N2 Ni N4 111.4(3) . . ? N2 Ni N3 174.1(3) . . ? N4 Ni N3 68.9(3) . . ? N2 Ni N1 68.9(3) . . ? N4 Ni N1 174.0(3) . . ? N3 Ni N1 111.4(3) . . ? N2 Ni C1 34.1(3) . . ? N4 Ni C1 145.2(3) . . ? N3 Ni C1 145.9(3) . . ? N1 Ni C1 34.8(3) . . ? N2 Ni C22 145.6(3) . . ? N4 Ni C22 34.3(3) . . ? N3 Ni C22 34.7(3) . . ? N1 Ni C22 145.4(3) . . ? C1 Ni C22 178.5(3) . . ? N1 Si1 C16 110.5(4) . . ? N1 Si1 C18 108.2(4) . . ? C16 Si1 C18 110.7(5) . . ? N1 Si1 C17 112.6(4) . . ? C16 Si1 C17 108.6(5) . . ? C18 Si1 C17 106.1(5) . . ? C19 Si2 C9 105.4(5) . . ? C19 Si2 C20 111.4(6) . . ? C9 Si2 C20 113.3(5) . . ? C19 Si2 C21 106.6(6) . . ? C9 Si2 C21 111.0(5) . . ? C20 Si2 C21 108.9(6) . . ? N3 Si3 C37 106.7(4) . . ? N3 Si3 C38 111.5(4) . . ? C37 Si3 C38 110.2(5) . . ? N3 Si3 C39 112.7(4) . . ? C37 Si3 C39 108.0(5) . . ? C38 Si3 C39 107.7(5) . . ? C30 Si4 C41 110.3(5) . . ? C30 Si4 C40 113.4(4) . . ? C41 Si4 C40 111.8(5) . . ? C30 Si4 C42 104.8(5) . . ? C41 Si4 C42 108.0(5) . . ? C40 Si4 C42 108.3(5) . . ? C1 N1 Si1 126.7(6) . . ? C1 N1 Ni 88.8(5) . . ? Si1 N1 Ni 127.6(4) . . ? C1 N2 C2 127.9(7) . . ? C1 N2 Ni 92.4(5) . . ? C2 N2 Ni 139.7(6) . . ? C22 N3 Si3 129.7(6) . . ? C22 N3 Ni 89.7(5) . . ? Si3 N3 Ni 130.8(4) . . ? C22 N4 C23 127.8(7) . . ? C22 N4 Ni 91.7(5) . . ? C23 N4 Ni 137.5(5) . . ? N2 C1 N1 109.9(7) . . ? N2 C1 C10 126.7(8) . . ? N1 C1 C10 123.3(8) . . ? N2 C1 Ni 53.6(4) . . ? N1 C1 Ni 56.4(4) . . ? C10 C1 Ni 177.7(7) . . ? C9 C2 N2 122.6(8) . . ? C9 C2 C3 125.3(9) . . ? N2 C2 C3 112.1(9) . . ? C4 C3 C8 116.5(10) . . ? C4 C3 C2 123.1(11) . . ? C8 C3 C2 120.3(9) . . ? C3 C4 C5 120.9(14) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 118.4(13) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? C7 C6 C5 122.1(13) . . ? C7 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? C6 C7 C8 119.1(14) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C7 C8 C3 122.8(12) . . ? C7 C8 H8 118.6 . . ? C3 C8 H8 118.6 . . ? C2 C9 Si2 129.4(7) . . ? C2 C9 H9 115.3 . . ? Si2 C9 H9 115.3 . . ? C15 C10 C11 117.9(8) . . ? C15 C10 C1 122.7(8) . . ? C11 C10 C1 119.4(8) . . ? C12 C11 C10 121.4(9) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 119.6(9) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.7(9) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.2 . . ? C15 C14 C13 121.1(9) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C10 120.3(9) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si1 C17 H17A 109.5 . . ? Si1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si1 C18 H18A 109.5 . . ? Si1 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si1 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si2 C20 H20A 109.5 . . ? Si2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N4 C22 N3 109.5(7) . . ? N4 C22 C31 125.8(7) . . ? N3 C22 C31 124.7(8) . . ? N4 C22 Ni 54.0(4) . . ? N3 C22 Ni 55.6(4) . . ? C31 C22 Ni 176.9(6) . . ? C30 C23 N4 125.1(8) . . ? C30 C23 C24 122.4(8) . . ? N4 C23 C24 112.5(8) . . ? C25 C24 C29 117.8(10) . . ? C25 C24 C23 120.8(9) . . ? C29 C24 C23 121.3(8) . . ? C24 C25 C26 121.3(11) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 118.9(11) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C28 C27 C26 120.7(12) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 120.4(12) . . ? C27 C28 H28 119.8 . . ? C29 C28 H28 119.8 . . ? C24 C29 C28 120.8(10) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C23 C30 Si4 135.2(8) . . ? C23 C30 H30 112.4 . . ? Si4 C30 H30 112.4 . . ? C32 C31 C36 118.0(8) . . ? C32 C31 C22 119.5(8) . . ? C36 C31 C22 122.4(8) . . ? C33 C32 C31 120.6(9) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 121.0(9) . . ? C34 C33 H33 119.5 . . ? C32 C33 H33 119.5 . . ? C33 C34 C35 119.3(9) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C34 C35 C36 119.5(9) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 121.4(9) . . ? C31 C36 H36 119.3 . . ? C35 C36 H36 119.3 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si3 C39 H39A 109.5 . . ? Si3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si4 C40 H40A 109.5 . . ? Si4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ?