#============================================================================== data_global #============================================================================== _audit_creation_date 12-01-10 _audit_creation_method SHELXL-97 # 1. Submission Details _publ_contact_author_name 'Jun Okuda' _publ_contact_author_address ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52074 Aachen Germany ; _publ_contact_author_phone '0049-241-8094645' _publ_contact_author_fax '0049-241-8092644' _publ_contact_author_email 'jun.okuda@ac.rwth-aachen.de' _publ_requested_journal 'New Journal of Chemistry' _publ_requested_coeditor_name ? _publ_contact_letter ; This CIF file is part of a manuscript that is submitted for publication in the journal 'Organometallics'. ; # 3. TITLE AND AUTHOR LIST _publ_section_title ; ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Jean-Charles Buffet' ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; 'Okuda, Jun' ; Institute of Inorganic Chemistry RWTH Aachen University Landoltweg 1 D-52056 Aachen Germany ; #=============================================== _publ_section_abstract ; ; _publ_section_references ; Altomare, A.; Burla, M. C.; Cavalli, M.; Cascarano, G. L.; Giacovazzo, C.; Gagliardi, A.; Moliterni, A. G. G.; Polidori, G.; Spagna, R. (1999). J. Appl. Crystallogr. 32, 115. Bruker (1999). SAINT+. Version 6.02. Program for Reduction of Data Collected on Bruker CCD Area Detector Diffractometer, Bruker AXS Inc., Madison, Wisconson, USA. Bruker (2001). SMART. Version 5.624. Program for Bruker CCD X-ray Diffractometer Control. Bruker AXS Inc., Madison, Wisconson, USA. Farrugia, L. J. (1997). J. Appl. Crystallogr. 30, 565. Farrugia, L. J. (1999). J. Appl. Crystallogr. 32, 837. Sheldrick, G. M. (1996). SADABS. Program for Empirical Absorption Correction of Area Detector Data, University of G\"ottingen, Germany. Sheldrick, G. M. (2008). Acta Crystallogr. A64, 112. Spek, A. L. (2003). J. Appl. Crystallogr. 36, 7. ; #===================================================== data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H43 Mg N5 Si2' _chemical_formula_sum 'C17 H43 Mg N5 Si2' _chemical_formula_weight 398.05 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' 'Mg' 'Mg' 0.0486 0.0363 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _space_group_name_Hall '-P 2yn' 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 9.3930(12) _cell_length_b 15.2074(19) _cell_length_c 17.202(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.626(2) _cell_angle_gamma 90.00 _cell_volume 2429.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4271 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.86 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9559 _exptl_absorpt_correction_T_max 0.9732 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32793 _diffrn_reflns_av_R_equivalents 0.0943 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6069 _reflns_number_gt 4374 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _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^)+(0.0407P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6069 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_ref 0.1050 _refine_ls_wR_factor_gt 0.0976 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.955 _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 0.44742(5) 0.12580(3) 0.37611(3) 0.02266(12) Uani 1 1 d . . . Si2 Si 0.35388(5) 0.30894(3) 0.33779(3) 0.02291(12) Uani 1 1 d . . . N1 N 0.62640(17) 0.10484(9) 0.17065(8) 0.0334(4) Uani 1 1 d . . . N2 N 0.77086(15) 0.24496(10) 0.24391(8) 0.0303(3) Uani 1 1 d . . . N3 N 0.54028(14) 0.31823(8) 0.13095(8) 0.0226(3) Uani 1 1 d . . . N4 N 0.35744(16) 0.15908(9) 0.11405(8) 0.0302(3) Uani 1 1 d . . . N5 N 0.43929(14) 0.21522(8) 0.31621(7) 0.0202(3) Uani 1 1 d . . . Mg1 Mg 0.53057(6) 0.20473(3) 0.21582(3) 0.02097(14) Uani 1 1 d . . . C1 C 0.7793(2) 0.10034(13) 0.17712(12) 0.0462(6) Uani 1 1 d . . . H1A H 0.8104 0.1207 0.1276 0.055 Uiso 1 1 calc R . . H1B H 0.8120 0.0389 0.1868 0.055 Uiso 1 1 calc R . . C2 C 0.8443(2) 0.15838(13) 0.24477(12) 0.0432(5) Uani 1 1 d . . . H2A H 0.8373 0.1282 0.2950 0.052 Uiso 1 1 calc R . . H2B H 0.9476 0.1678 0.2417 0.052 Uiso 1 1 calc R . . C3 C 0.80252(19) 0.30019(12) 0.17772(10) 0.0332(4) Uani 1 1 d . . . H3A H 0.8929 0.2795 0.1607 0.040 Uiso 1 1 calc R . . H3B H 0.8175 0.3617 0.1960 0.040 Uiso 1 1 calc R . . C4 C 0.68260(18) 0.29772(11) 0.10806(10) 0.0287(4) Uani 1 1 d . . . H4A H 0.7038 0.3408 0.0682 0.034 Uiso 1 1 calc R . . H4B H 0.6791 0.2385 0.0839 0.034 Uiso 1 1 calc R . . C5 C 0.42332(19) 0.30449(11) 0.06423(10) 0.0308(4) Uani 1 1 d . . . H5A H 0.4493 0.3343 0.0171 0.037 Uiso 1 1 calc R . . H5B H 0.3342 0.3322 0.0768 0.037 Uiso 1 1 calc R . . C6 C 0.3937(2) 0.20843(12) 0.04522(10) 0.0342(4) Uani 1 1 d . . . H6A H 0.3128 0.2037 0.0014 0.041 Uiso 1 1 calc R . . H6B H 0.4797 0.1817 0.0278 0.041 Uiso 1 1 calc R . . C7 C 0.3913(2) 0.06457(12) 0.10707(11) 0.0438(5) Uani 1 1 d . . . H7A H 0.3401 0.0417 0.0566 0.053 Uiso 1 1 calc R . . H7B H 0.3566 0.0317 0.1502 0.053 Uiso 1 1 calc R . . C8 C 0.5515(2) 0.04951(12) 0.11056(12) 0.0473(6) Uani 1 1 d . . . H8A H 0.5750 -0.0129 0.1227 0.057 Uiso 1 1 calc R . . H8B H 0.5811 0.0638 0.0592 0.057 Uiso 1 1 calc R . . C9 C 0.8170(2) 0.28960(15) 0.31943(11) 0.0471(5) Uani 1 1 d . . . H9A H 0.9217 0.2977 0.3271 0.071 Uiso 1 1 calc R . . H9B H 0.7903 0.2537 0.3623 0.071 Uiso 1 1 calc R . . H9C H 0.7697 0.3471 0.3191 0.071 Uiso 1 1 calc R . . C10 C 0.53802(19) 0.41212(11) 0.15381(11) 0.0325(4) Uani 1 1 d . . . H10A H 0.5553 0.4490 0.1094 0.049 Uiso 1 1 calc R . . H10B H 0.6134 0.4229 0.1987 0.049 Uiso 1 1 calc R . . H10C H 0.4439 0.4266 0.1684 0.049 Uiso 1 1 calc R . . C11 C 0.2036(2) 0.16845(14) 0.12015(11) 0.0410(5) Uani 1 1 d . . . H11A H 0.1459 0.1395 0.0752 0.061 Uiso 1 1 calc R . . H11B H 0.1785 0.2310 0.1203 0.061 Uiso 1 1 calc R . . H11C H 0.1840 0.1411 0.1690 0.061 Uiso 1 1 calc R . . C12 C 0.5724(2) 0.03795(12) 0.35065(12) 0.0466(6) Uani 1 1 d . . . H12A H 0.5518 0.0254 0.2942 0.070 Uiso 1 1 calc R . . H12B H 0.5586 -0.0155 0.3804 0.070 Uiso 1 1 calc R . . H12C H 0.6722 0.0581 0.3640 0.070 Uiso 1 1 calc R . . C13 C 0.2691(2) 0.06948(12) 0.37386(12) 0.0417(5) Uani 1 1 d . . . H13A H 0.2002 0.1104 0.3917 0.063 Uiso 1 1 calc R . . H13B H 0.2808 0.0181 0.4087 0.063 Uiso 1 1 calc R . . H13C H 0.2332 0.0505 0.3200 0.063 Uiso 1 1 calc R . . C14 C 0.5171(2) 0.15080(13) 0.48182(10) 0.0410(5) Uani 1 1 d . . . H14A H 0.6068 0.1845 0.4851 0.062 Uiso 1 1 calc R . . H14B H 0.5356 0.0957 0.5111 0.062 Uiso 1 1 calc R . . H14C H 0.4454 0.1853 0.5045 0.062 Uiso 1 1 calc R . . C15 C 0.2207(2) 0.34833(12) 0.25305(10) 0.0356(4) Uani 1 1 d . . . H15A H 0.2675 0.3521 0.2059 0.053 Uiso 1 1 calc R . . H15B H 0.1851 0.4065 0.2652 0.053 Uiso 1 1 calc R . . H15C H 0.1400 0.3070 0.2437 0.053 Uiso 1 1 calc R . . C16 C 0.4816(2) 0.40135(12) 0.36812(12) 0.0431(5) Uani 1 1 d . . . H16A H 0.5514 0.3831 0.4134 0.065 Uiso 1 1 calc R . . H16B H 0.4278 0.4525 0.3825 0.065 Uiso 1 1 calc R . . H16C H 0.5326 0.4168 0.3243 0.065 Uiso 1 1 calc R . . C17 C 0.2434(2) 0.30272(12) 0.42030(11) 0.0369(5) Uani 1 1 d . . . H17A H 0.1786 0.2520 0.4122 0.055 Uiso 1 1 calc R . . H17B H 0.1866 0.3567 0.4212 0.055 Uiso 1 1 calc R . . H17C H 0.3076 0.2963 0.4704 0.055 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 0.0262(3) 0.0208(2) 0.0207(2) 0.00426(18) 0.00252(19) -0.00029(18) Si2 0.0276(3) 0.0203(2) 0.0219(2) 0.00105(18) 0.00729(19) 0.00158(19) N1 0.0466(10) 0.0259(8) 0.0298(8) -0.0006(6) 0.0122(7) 0.0098(7) N2 0.0243(8) 0.0427(9) 0.0240(8) 0.0033(7) 0.0036(6) 0.0043(7) N3 0.0233(7) 0.0219(7) 0.0223(7) 0.0011(6) 0.0029(6) 0.0011(6) N4 0.0412(9) 0.0290(8) 0.0198(7) -0.0011(6) 0.0025(6) -0.0088(7) N5 0.0255(7) 0.0183(7) 0.0169(7) 0.0018(5) 0.0036(5) 0.0008(5) Mg1 0.0260(3) 0.0202(3) 0.0167(3) 0.0011(2) 0.0028(2) 0.0027(2) C1 0.0597(14) 0.0398(12) 0.0438(12) 0.0118(10) 0.0230(11) 0.0274(10) C2 0.0296(10) 0.0597(14) 0.0420(12) 0.0210(10) 0.0112(9) 0.0190(10) C3 0.0237(9) 0.0423(11) 0.0348(10) 0.0066(8) 0.0087(8) 0.0022(8) C4 0.0304(10) 0.0315(10) 0.0259(9) 0.0063(7) 0.0102(7) 0.0017(8) C5 0.0340(10) 0.0364(10) 0.0206(9) 0.0090(7) -0.0009(7) -0.0004(8) C6 0.0441(11) 0.0416(11) 0.0153(9) 0.0016(8) -0.0007(8) -0.0082(9) C7 0.0733(16) 0.0279(10) 0.0305(11) -0.0079(8) 0.0090(10) -0.0142(10) C8 0.0867(17) 0.0216(10) 0.0377(12) -0.0037(8) 0.0230(11) 0.0051(10) C9 0.0289(10) 0.0777(16) 0.0321(11) -0.0050(11) -0.0032(9) -0.0071(10) C10 0.0346(10) 0.0241(9) 0.0398(11) 0.0031(8) 0.0089(8) 0.0007(8) C11 0.0371(11) 0.0554(13) 0.0282(10) -0.0003(9) -0.0023(8) -0.0172(9) C12 0.0643(14) 0.0319(11) 0.0491(13) 0.0194(9) 0.0257(11) 0.0196(10) C13 0.0416(12) 0.0307(11) 0.0514(13) 0.0062(9) 0.0022(10) -0.0115(9) C14 0.0451(12) 0.0485(12) 0.0263(10) 0.0094(9) -0.0050(9) -0.0002(10) C15 0.0385(11) 0.0355(10) 0.0339(11) 0.0073(8) 0.0094(8) 0.0128(8) C16 0.0498(13) 0.0298(10) 0.0524(13) -0.0119(9) 0.0161(10) -0.0061(9) C17 0.0461(12) 0.0357(11) 0.0327(10) 0.0028(8) 0.0181(9) 0.0087(9) _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 N5 1.7009(13) . ? Si1 C12 1.8734(18) . ? Si1 C13 1.8765(18) . ? Si1 C14 1.8769(18) . ? Si1 Mg1 3.2093(7) . ? Si2 N5 1.7036(13) . ? Si2 C16 1.8706(19) . ? Si2 C15 1.8711(18) . ? Si2 C17 1.8817(18) . ? N1 C1 1.426(2) . ? N1 C8 1.433(2) . ? N1 Mg1 1.9828(15) . ? N2 C9 1.472(2) . ? N2 C3 1.480(2) . ? N2 C2 1.486(2) . ? N2 Mg1 2.3183(15) . ? N3 C5 1.480(2) . ? N3 C10 1.482(2) . ? N3 C4 1.482(2) . ? N3 Mg1 2.2713(14) . ? N4 C11 1.471(2) . ? N4 C7 1.481(2) . ? N4 C6 1.484(2) . ? N4 Mg1 2.3103(15) . ? N5 Mg1 2.0462(14) . ? C1 C2 1.514(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.517(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.514(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.515(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 N5 Si1 C12 113.66(8) . . ? N5 Si1 C13 113.17(8) . . ? C12 Si1 C13 104.99(9) . . ? N5 Si1 C14 113.73(8) . . ? C12 Si1 C14 103.37(9) . . ? C13 Si1 C14 107.04(9) . . ? C12 Si1 Mg1 79.87(6) . . ? C13 Si1 Mg1 118.98(7) . . ? C14 Si1 Mg1 131.46(7) . . ? N5 Si2 C16 112.71(8) . . ? N5 Si2 C15 112.31(7) . . ? C16 Si2 C15 107.61(9) . . ? N5 Si2 C17 116.95(7) . . ? C16 Si2 C17 103.33(9) . . ? C15 Si2 C17 102.95(8) . . ? C1 N1 C8 114.07(15) . . ? C1 N1 Mg1 121.16(12) . . ? C8 N1 Mg1 122.01(13) . . ? C9 N2 C3 110.52(15) . . ? C9 N2 C2 108.97(15) . . ? C3 N2 C2 111.34(14) . . ? C9 N2 Mg1 117.00(11) . . ? C3 N2 Mg1 106.92(10) . . ? C2 N2 Mg1 101.80(11) . . ? C5 N3 C10 107.65(13) . . ? C5 N3 C4 111.01(13) . . ? C10 N3 C4 108.82(13) . . ? C5 N3 Mg1 107.13(9) . . ? C10 N3 Mg1 123.92(10) . . ? C4 N3 Mg1 97.79(9) . . ? C11 N4 C7 108.96(15) . . ? C11 N4 C6 110.69(14) . . ? C7 N4 C6 110.39(14) . . ? C11 N4 Mg1 120.27(11) . . ? C7 N4 Mg1 102.58(11) . . ? C6 N4 Mg1 103.47(10) . . ? Si1 N5 Si2 121.11(8) . . ? Si1 N5 Mg1 117.55(7) . . ? Si2 N5 Mg1 121.32(7) . . ? N1 Mg1 N5 131.51(6) . . ? N1 Mg1 N3 105.43(6) . . ? N5 Mg1 N3 123.07(5) . . ? N1 Mg1 N4 77.42(6) . . ? N5 Mg1 N4 109.06(6) . . ? N3 Mg1 N4 80.38(5) . . ? N1 Mg1 N2 78.40(6) . . ? N5 Mg1 N2 108.76(6) . . ? N3 Mg1 N2 78.56(5) . . ? N4 Mg1 N2 142.17(6) . . ? N1 Mg1 Si1 103.49(5) . . ? N5 Mg1 Si1 28.03(4) . . ? N3 Mg1 Si1 151.03(4) . . ? N4 Mg1 Si1 107.72(4) . . ? N2 Mg1 Si1 105.93(4) . . ? N1 C1 C2 108.50(15) . . ? N1 C1 H1A 110.0 . . ? C2 C1 H1A 110.0 . . ? N1 C1 H1B 110.0 . . ? C2 C1 H1B 110.0 . . ? H1A C1 H1B 108.4 . . ? N2 C2 C1 112.08(15) . . ? N2 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N2 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N2 C3 C4 112.49(14) . . ? N2 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.8 . . ? N3 C4 C3 112.17(13) . . ? N3 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? N3 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? N3 C5 C6 113.25(13) . . ? N3 C5 H5A 108.9 . . ? C6 C5 H5A 108.9 . . ? N3 C5 H5B 108.9 . . ? C6 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N4 C6 C5 111.86(14) . . ? N4 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N4 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N4 C7 C8 111.57(15) . . ? N4 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N4 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N1 C8 C7 108.49(15) . . ? N1 C8 H8A 110.0 . . ? C7 C8 H8A 110.0 . . ? N1 C8 H8B 110.0 . . ? C7 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C12 Si1 N5 Si2 -170.04(10) . . . . ? C13 Si1 N5 Si2 70.32(11) . . . . ? C14 Si1 N5 Si2 -52.12(12) . . . . ? Mg1 Si1 N5 Si2 178.23(14) . . . . ? C12 Si1 N5 Mg1 11.73(12) . . . . ? C13 Si1 N5 Mg1 -107.92(10) . . . . ? C14 Si1 N5 Mg1 129.65(9) . . . . ? C16 Si2 N5 Si1 109.50(10) . . . . ? C15 Si2 N5 Si1 -128.76(9) . . . . ? C17 Si2 N5 Si1 -10.05(13) . . . . ? C16 Si2 N5 Mg1 -72.33(11) . . . . ? C15 Si2 N5 Mg1 49.41(11) . . . . ? C17 Si2 N5 Mg1 168.12(9) . . . . ? C1 N1 Mg1 N5 -102.60(15) . . . . ? C8 N1 Mg1 N5 97.32(15) . . . . ? C1 N1 Mg1 N3 76.81(14) . . . . ? C8 N1 Mg1 N3 -83.27(14) . . . . ? C1 N1 Mg1 N4 152.97(14) . . . . ? C8 N1 Mg1 N4 -7.11(14) . . . . ? C1 N1 Mg1 N2 2.27(13) . . . . ? C8 N1 Mg1 N2 -157.81(15) . . . . ? C1 N1 Mg1 Si1 -101.54(13) . . . . ? C8 N1 Mg1 Si1 98.38(14) . . . . ? Si1 N5 Mg1 N1 2.19(12) . . . . ? Si2 N5 Mg1 N1 -176.04(8) . . . . ? Si1 N5 Mg1 N3 -177.13(6) . . . . ? Si2 N5 Mg1 N3 4.64(11) . . . . ? Si1 N5 Mg1 N4 92.07(8) . . . . ? Si2 N5 Mg1 N4 -86.16(9) . . . . ? Si1 N5 Mg1 N2 -88.78(8) . . . . ? Si2 N5 Mg1 N2 92.99(9) . . . . ? Si2 N5 Mg1 Si1 -178.23(14) . . . . ? C5 N3 Mg1 N1 79.84(11) . . . . ? C10 N3 Mg1 N1 -154.03(12) . . . . ? C4 N3 Mg1 N1 -35.05(11) . . . . ? C5 N3 Mg1 N5 -100.69(11) . . . . ? C10 N3 Mg1 N5 25.45(14) . . . . ? C4 N3 Mg1 N5 144.42(9) . . . . ? C5 N3 Mg1 N4 5.86(10) . . . . ? C10 N3 Mg1 N4 131.99(13) . . . . ? C4 N3 Mg1 N4 -109.03(10) . . . . ? C5 N3 Mg1 N2 154.25(11) . . . . ? C10 N3 Mg1 N2 -79.62(12) . . . . ? C4 N3 Mg1 N2 39.36(9) . . . . ? C5 N3 Mg1 Si1 -103.47(11) . . . . ? C10 N3 Mg1 Si1 22.66(17) . . . . ? C4 N3 Mg1 Si1 141.64(9) . . . . ? C11 N4 Mg1 N1 148.72(14) . . . . ? C7 N4 Mg1 N1 27.68(11) . . . . ? C6 N4 Mg1 N1 -87.19(12) . . . . ? C11 N4 Mg1 N5 18.83(14) . . . . ? C7 N4 Mg1 N5 -102.21(11) . . . . ? C6 N4 Mg1 N5 142.92(11) . . . . ? C11 N4 Mg1 N3 -102.96(13) . . . . ? C7 N4 Mg1 N3 135.99(11) . . . . ? C6 N4 Mg1 N3 21.12(11) . . . . ? C11 N4 Mg1 N2 -159.85(12) . . . . ? C7 N4 Mg1 N2 79.10(14) . . . . ? C6 N4 Mg1 N2 -35.77(16) . . . . ? C11 N4 Mg1 Si1 48.37(13) . . . . ? C7 N4 Mg1 Si1 -72.67(11) . . . . ? C6 N4 Mg1 Si1 172.46(10) . . . . ? C9 N2 Mg1 N1 -143.28(14) . . . . ? C3 N2 Mg1 N1 92.23(11) . . . . ? C2 N2 Mg1 N1 -24.65(11) . . . . ? C9 N2 Mg1 N5 -13.13(15) . . . . ? C3 N2 Mg1 N5 -137.62(11) . . . . ? C2 N2 Mg1 N5 105.50(11) . . . . ? C9 N2 Mg1 N3 108.15(14) . . . . ? C3 N2 Mg1 N3 -16.34(11) . . . . ? C2 N2 Mg1 N3 -133.22(11) . . . . ? C9 N2 Mg1 N4 165.56(13) . . . . ? C3 N2 Mg1 N4 41.07(16) . . . . ? C2 N2 Mg1 N4 -75.81(14) . . . . ? C9 N2 Mg1 Si1 -42.37(14) . . . . ? C3 N2 Mg1 Si1 -166.86(10) . . . . ? C2 N2 Mg1 Si1 76.25(10) . . . . ? N5 Si1 Mg1 N1 -178.31(10) . . . . ? C12 Si1 Mg1 N1 12.59(9) . . . . ? C13 Si1 Mg1 N1 -89.02(9) . . . . ? C14 Si1 Mg1 N1 111.53(10) . . . . ? C12 Si1 Mg1 N5 -169.10(11) . . . . ? C13 Si1 Mg1 N5 89.29(11) . . . . ? C14 Si1 Mg1 N5 -70.15(11) . . . . ? N5 Si1 Mg1 N3 4.97(11) . . . . ? C12 Si1 Mg1 N3 -164.13(11) . . . . ? C13 Si1 Mg1 N3 94.26(11) . . . . ? C14 Si1 Mg1 N3 -65.19(12) . . . . ? N5 Si1 Mg1 N4 -97.43(9) . . . . ? C12 Si1 Mg1 N4 93.47(8) . . . . ? C13 Si1 Mg1 N4 -8.14(9) . . . . ? C14 Si1 Mg1 N4 -167.59(9) . . . . ? N5 Si1 Mg1 N2 100.12(9) . . . . ? C12 Si1 Mg1 N2 -68.98(8) . . . . ? C13 Si1 Mg1 N2 -170.59(8) . . . . ? C14 Si1 Mg1 N2 29.97(10) . . . . ? C8 N1 C1 C2 -177.44(15) . . . . ? Mg1 N1 C1 C2 21.0(2) . . . . ? C9 N2 C2 C1 167.67(16) . . . . ? C3 N2 C2 C1 -70.17(19) . . . . ? Mg1 N2 C2 C1 43.46(16) . . . . ? N1 C1 C2 N2 -44.8(2) . . . . ? C9 N2 C3 C4 -139.68(16) . . . . ? C2 N2 C3 C4 99.06(17) . . . . ? Mg1 N2 C3 C4 -11.32(17) . . . . ? C5 N3 C4 C3 -172.88(13) . . . . ? C10 N3 C4 C3 68.82(17) . . . . ? Mg1 N3 C4 C3 -61.10(14) . . . . ? N2 C3 C4 N3 52.37(19) . . . . ? C10 N3 C5 C6 -168.52(14) . . . . ? C4 N3 C5 C6 72.48(17) . . . . ? Mg1 N3 C5 C6 -33.21(16) . . . . ? C11 N4 C6 C5 84.05(18) . . . . ? C7 N4 C6 C5 -155.22(16) . . . . ? Mg1 N4 C6 C5 -46.07(16) . . . . ? N3 C5 C6 N4 57.2(2) . . . . ? C11 N4 C7 C8 -173.05(15) . . . . ? C6 N4 C7 C8 65.20(19) . . . . ? Mg1 N4 C7 C8 -44.53(16) . . . . ? C1 N1 C8 C7 -176.81(15) . . . . ? Mg1 N1 C8 C7 -15.4(2) . . . . ? N4 C7 C8 N1 41.8(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.378 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.051 #==END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H43 Ca N5 Si2' _chemical_formula_sum 'C17 H43 Ca N5 Si2' _chemical_formula_weight 413.82 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' 'Ca' 'Ca' 0.2262 0.3064 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8305(10) _cell_length_b 14.9065(9) _cell_length_c 21.3107(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5028.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 4542 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.26 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 0.355 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9072 _exptl_absorpt_correction_T_max 0.9421 _exptl_absorpt_process_details 'Platon Mulabs' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66018 _diffrn_reflns_av_R_equivalents 0.1046 _diffrn_reflns_av_sigmaI/netI 0.0691 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6261 _reflns_number_gt 4249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _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^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6261 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0778 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 0.860 _refine_ls_restrained_S_all 0.860 _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 0.10265(3) 0.19682(3) 0.55383(2) 0.02207(11) Uani 1 1 d . A . Si2 Si 0.19978(3) 0.36717(3) 0.53012(2) 0.02304(12) Uani 1 1 d . A . N1 N 0.17193(9) 0.32704(9) 0.32699(6) 0.0290(3) Uani 1 1 d . A . N2 N -0.00006(9) 0.30330(10) 0.35397(6) 0.0304(4) Uani 1 1 d . A . N3 N 0.06330(9) 0.11469(9) 0.33003(6) 0.0281(3) Uani 1 1 d . . . N4 N 0.24720(9) 0.15769(10) 0.34822(6) 0.0278(3) Uani 1 1 d . . . N5 N 0.15353(8) 0.27057(9) 0.50822(6) 0.0216(3) Uani 1 1 d . . . Ca1 Ca 0.12822(2) 0.23412(2) 0.403425(14) 0.02156(9) Uani 1 1 d . A . C1 C 0.11341(12) 0.38219(12) 0.29363(8) 0.0356(5) Uani 1 1 d . . . H1A H 0.1010 0.3552 0.2522 0.043 Uiso 1 1 calc R A . H1B H 0.1382 0.4423 0.2867 0.043 Uiso 1 1 calc R . . C2 C 0.03271(12) 0.39069(12) 0.33120(9) 0.0383(5) Uani 1 1 d . A . H2A H 0.0432 0.4302 0.3677 0.046 Uiso 1 1 calc R . . H2B H -0.0109 0.4196 0.3048 0.046 Uiso 1 1 calc R . . C3 C -0.02807(12) 0.24638(13) 0.30083(8) 0.0366(5) Uani 1 1 d . . . H3A H 0.0078 0.2594 0.2639 0.044 Uiso 0.609(3) 1 calc PR A 1 H3B H -0.0869 0.2624 0.2898 0.044 Uiso 0.609(3) 1 calc PR A 1 H3C H -0.0442 0.2858 0.2654 0.044 Uiso 0.391(3) 1 calc PR A 2 H3D H -0.0792 0.2129 0.3138 0.044 Uiso 0.391(3) 1 calc PR A 2 C4A C -0.02399(19) 0.1467(2) 0.31476(14) 0.0364(9) Uani 0.609(3) 1 d P A 1 H4A H -0.0617 0.1332 0.3506 0.044 Uiso 0.609(3) 1 calc PR A 1 H4B H -0.0452 0.1132 0.2779 0.044 Uiso 0.609(3) 1 calc PR A 1 C5A C 0.12097(19) 0.1228(2) 0.27823(13) 0.0328(9) Uani 0.609(3) 1 d P A 1 H5A H 0.1165 0.1842 0.2608 0.039 Uiso 0.609(3) 1 calc PR A 1 H5B H 0.1035 0.0803 0.2449 0.039 Uiso 0.609(3) 1 calc PR A 1 C4B C 0.0384(3) 0.1788(3) 0.2775(2) 0.0316(13) Uani 0.391(3) 1 d P A 2 H4C H 0.0152 0.1442 0.2418 0.038 Uiso 0.391(3) 1 calc PR A 2 H4D H 0.0890 0.2115 0.2626 0.038 Uiso 0.391(3) 1 calc PR A 2 C5B C 0.1383(3) 0.0603(3) 0.3068(2) 0.0354(14) Uani 0.391(3) 1 d P A 2 H5C H 0.1496 0.0128 0.3382 0.042 Uiso 0.391(3) 1 calc PR A 2 H5D H 0.1210 0.0299 0.2676 0.042 Uiso 0.391(3) 1 calc PR A 2 C6 C 0.21426(12) 0.10427(13) 0.29507(8) 0.0367(5) Uani 1 1 d . A . H6A H 0.2204 0.0398 0.3053 0.044 Uiso 0.609(3) 1 calc PR A 1 H6B H 0.2495 0.1165 0.2577 0.044 Uiso 0.609(3) 1 calc PR A 1 H6C H 0.2064 0.1446 0.2586 0.044 Uiso 0.391(3) 1 calc PR A 2 H6D H 0.2572 0.0590 0.2833 0.044 Uiso 0.391(3) 1 calc PR A 2 C7 C 0.29762(11) 0.23544(12) 0.32662(9) 0.0365(5) Uani 1 1 d . A . H7A H 0.3435 0.2137 0.2989 0.044 Uiso 1 1 calc R . . H7B H 0.3242 0.2644 0.3635 0.044 Uiso 1 1 calc R . . C8 C 0.24594(12) 0.30497(13) 0.29138(8) 0.0393(5) Uani 1 1 d . . . H8A H 0.2803 0.3596 0.2845 0.047 Uiso 1 1 calc R A . H8B H 0.2293 0.2809 0.2499 0.047 Uiso 1 1 calc R . . C9 C -0.07111(12) 0.31893(14) 0.39732(9) 0.0470(6) Uani 1 1 d . . . H9A H -0.1153 0.3531 0.3758 0.070 Uiso 1 1 calc R A . H9B H -0.0512 0.3528 0.4338 0.070 Uiso 1 1 calc R . . H9C H -0.0941 0.2612 0.4112 0.070 Uiso 1 1 calc R . . C10A C 0.0529(2) 0.0177(2) 0.34909(14) 0.0376(9) Uani 0.609(3) 1 d P A 1 H10A H 0.0348 -0.0176 0.3127 0.056 Uiso 0.609(3) 1 calc PR A 1 H10B H 0.0103 0.0133 0.3823 0.056 Uiso 0.609(3) 1 calc PR A 1 H10C H 0.1069 -0.0054 0.3647 0.056 Uiso 0.609(3) 1 calc PR A 1 C10B C -0.0046(4) 0.0558(4) 0.3455(2) 0.0413(15) Uani 0.391(3) 1 d P A 2 H10D H -0.0225 0.0233 0.3078 0.062 Uiso 0.391(3) 1 calc PR A 2 H10E H -0.0521 0.0907 0.3619 0.062 Uiso 0.391(3) 1 calc PR A 2 H10F H 0.0142 0.0128 0.3773 0.062 Uiso 0.391(3) 1 calc PR A 2 C11 C 0.30093(12) 0.10161(13) 0.38863(9) 0.0411(5) Uani 1 1 d . A . H11A H 0.2689 0.0490 0.4026 0.062 Uiso 1 1 calc R . . H11B H 0.3189 0.1364 0.4253 0.062 Uiso 1 1 calc R . . H11C H 0.3507 0.0821 0.3650 0.062 Uiso 1 1 calc R . . C12 C 0.04503(11) 0.11649(11) 0.50048(8) 0.0315(4) Uani 1 1 d . . . H12A H 0.0060 0.1501 0.4736 0.047 Uiso 1 1 calc R A . H12B H 0.0131 0.0733 0.5258 0.047 Uiso 1 1 calc R . . H12C H 0.0860 0.0843 0.4743 0.047 Uiso 1 1 calc R . . C13 C 0.01980(11) 0.24567(13) 0.60672(8) 0.0392(5) Uani 1 1 d . . . H13A H 0.0465 0.2860 0.6371 0.059 Uiso 1 1 calc R A . H13B H -0.0092 0.1972 0.6291 0.059 Uiso 1 1 calc R . . H13C H -0.0212 0.2793 0.5816 0.059 Uiso 1 1 calc R . . C14 C 0.17268(11) 0.12533(12) 0.60396(8) 0.0331(4) Uani 1 1 d . . . H14A H 0.2142 0.0947 0.5774 0.050 Uiso 1 1 calc R A . H14B H 0.1384 0.0807 0.6261 0.050 Uiso 1 1 calc R . . H14C H 0.2021 0.1632 0.6346 0.050 Uiso 1 1 calc R . . C15 C 0.12701(11) 0.46521(12) 0.52025(9) 0.0354(5) Uani 1 1 d . . . H15A H 0.1074 0.4679 0.4767 0.053 Uiso 1 1 calc R A . H15B H 0.1572 0.5207 0.5306 0.053 Uiso 1 1 calc R . . H15C H 0.0784 0.4584 0.5483 0.053 Uiso 1 1 calc R . . C16 C 0.23488(12) 0.36971(12) 0.61466(8) 0.0388(5) Uani 1 1 d . . . H16A H 0.1856 0.3632 0.6421 0.058 Uiso 1 1 calc R A . H16B H 0.2629 0.4270 0.6234 0.058 Uiso 1 1 calc R . . H16C H 0.2744 0.3203 0.6224 0.058 Uiso 1 1 calc R . . C17 C 0.29578(11) 0.38988(12) 0.48121(8) 0.0350(5) Uani 1 1 d . . . H17A H 0.3358 0.3401 0.4857 0.052 Uiso 1 1 calc R A . H17B H 0.3225 0.4457 0.4953 0.052 Uiso 1 1 calc R . . H17C H 0.2793 0.3957 0.4371 0.052 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 0.0248(3) 0.0241(3) 0.0173(2) -0.0007(2) 0.00272(19) -0.0026(2) Si2 0.0260(3) 0.0233(3) 0.0198(2) -0.0013(2) -0.0017(2) -0.0039(2) N1 0.0339(9) 0.0314(9) 0.0216(8) 0.0051(7) -0.0006(7) 0.0002(7) N2 0.0291(8) 0.0339(9) 0.0282(8) -0.0078(7) -0.0054(7) 0.0017(7) N3 0.0342(9) 0.0280(8) 0.0222(8) -0.0018(7) -0.0012(7) -0.0050(7) N4 0.0303(8) 0.0314(9) 0.0218(8) 0.0033(6) 0.0021(6) 0.0011(7) N5 0.0259(8) 0.0234(7) 0.0154(7) -0.0009(6) 0.0001(6) -0.0046(6) Ca1 0.02432(18) 0.02589(19) 0.01448(16) -0.00068(14) -0.00027(14) -0.00315(15) C1 0.0489(13) 0.0293(11) 0.0286(10) 0.0055(8) -0.0095(9) -0.0051(9) C2 0.0464(13) 0.0311(11) 0.0374(11) -0.0004(9) -0.0148(10) 0.0069(10) C3 0.0337(11) 0.0436(12) 0.0324(10) -0.0055(9) -0.0132(9) 0.0007(9) C4A 0.0331(19) 0.043(2) 0.0332(18) -0.0099(15) -0.0073(14) -0.0066(16) C5A 0.042(2) 0.039(2) 0.0170(15) -0.0075(14) 0.0015(13) -0.0018(16) C4B 0.040(3) 0.034(3) 0.021(2) -0.004(2) -0.006(2) -0.007(2) C5B 0.053(4) 0.030(3) 0.024(3) -0.009(2) -0.006(2) -0.003(3) C6 0.0451(13) 0.0401(12) 0.0249(10) -0.0047(9) 0.0034(9) 0.0088(10) C7 0.0328(11) 0.0423(12) 0.0345(11) 0.0039(9) 0.0129(9) -0.0012(9) C8 0.0487(13) 0.0401(12) 0.0292(10) 0.0089(9) 0.0096(9) -0.0045(10) C9 0.0331(12) 0.0572(14) 0.0506(13) -0.0167(11) -0.0006(10) 0.0080(10) C10A 0.052(2) 0.033(2) 0.0284(18) -0.0067(15) 0.0000(17) -0.0131(18) C10B 0.055(4) 0.039(4) 0.030(3) -0.006(3) -0.002(3) -0.022(3) C11 0.0418(12) 0.0414(12) 0.0401(12) 0.0062(9) -0.0053(9) 0.0074(10) C12 0.0385(11) 0.0306(11) 0.0254(9) 0.0026(8) 0.0012(8) -0.0118(8) C13 0.0369(11) 0.0476(13) 0.0332(11) -0.0023(9) 0.0117(9) 0.0011(10) C14 0.0401(11) 0.0326(11) 0.0264(10) 0.0025(8) 0.0009(8) -0.0004(9) C15 0.0367(11) 0.0303(11) 0.0391(11) -0.0040(9) -0.0003(9) -0.0006(9) C16 0.0529(13) 0.0349(11) 0.0288(10) -0.0029(9) -0.0108(9) -0.0119(10) C17 0.0303(11) 0.0323(11) 0.0423(12) 0.0012(9) 0.0018(9) -0.0075(9) _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 N5 1.6740(13) . ? Si1 C14 1.8725(17) . ? Si1 C13 1.8763(17) . ? Si1 C12 1.8864(16) . ? Si1 Ca1 3.2782(6) . ? Si2 N5 1.6815(13) . ? Si2 C15 1.8727(17) . ? Si2 C17 1.8736(17) . ? Si2 C16 1.8857(17) . ? Si2 Ca1 3.5365(6) . ? N1 C1 1.428(2) . ? N1 C8 1.434(2) . ? N1 Ca1 2.2474(14) . ? N2 C9 1.474(2) . ? N2 C3 1.483(2) . ? N2 C2 1.484(2) . ? N2 Ca1 2.5096(14) . ? N3 C10B 1.426(5) . ? N3 C5A 1.438(3) . ? N3 C4A 1.498(3) . ? N3 C10A 1.510(3) . ? N3 C5B 1.521(5) . ? N3 C4B 1.524(4) . ? N3 Ca1 2.5830(14) . ? N4 C11 1.471(2) . ? N4 C6 1.480(2) . ? N4 C7 1.481(2) . ? N4 Ca1 2.4960(14) . ? N5 Ca1 2.3330(13) . ? Ca1 C7 3.1418(18) . ? Ca1 C5A 3.144(3) . ? Ca1 C4B 3.147(4) . ? Ca1 C2 3.1785(18) . ? Ca1 C8 3.2078(18) . ? Ca1 C1 3.2252(18) . ? C1 C2 1.513(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4A 1.516(3) . ? C3 C4B 1.540(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4A H4A 0.9900 . ? C4A H4B 0.9900 . ? C5A C6 1.545(3) . ? C5A H5A 0.9900 . ? C5A H5B 0.9900 . ? C4B H4C 0.9900 . ? C4B H4D 0.9900 . ? C5B C6 1.392(5) . ? C5B H5C 0.9900 . ? C5B H5D 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 H6C 0.9900 . ? C6 H6D 0.9900 . ? C7 C8 1.519(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10A H10A 0.9800 . ? C10A H10B 0.9800 . ? C10A H10C 0.9800 . ? C10B H10D 0.9800 . ? C10B H10E 0.9800 . ? C10B H10F 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 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 N5 Si1 C14 114.84(7) . . ? N5 Si1 C13 115.49(8) . . ? C14 Si1 C13 106.97(8) . . ? N5 Si1 C12 107.43(7) . . ? C14 Si1 C12 105.60(8) . . ? C13 Si1 C12 105.69(8) . . ? C14 Si1 Ca1 125.54(6) . . ? C13 Si1 Ca1 127.43(6) . . ? C12 Si1 Ca1 65.04(5) . . ? N5 Si2 C15 111.66(7) . . ? N5 Si2 C17 110.70(7) . . ? C15 Si2 C17 107.18(8) . . ? N5 Si2 C16 114.25(7) . . ? C15 Si2 C16 105.84(9) . . ? C17 Si2 C16 106.79(8) . . ? C15 Si2 Ca1 98.90(6) . . ? C17 Si2 Ca1 86.36(6) . . ? C16 Si2 Ca1 146.62(6) . . ? C1 N1 C8 113.48(14) . . ? C1 N1 Ca1 121.06(11) . . ? C8 N1 Ca1 119.58(11) . . ? C9 N2 C3 109.93(14) . . ? C9 N2 C2 109.45(14) . . ? C3 N2 C2 110.92(14) . . ? C9 N2 Ca1 114.78(11) . . ? C3 N2 Ca1 109.12(10) . . ? C2 N2 Ca1 102.43(10) . . ? C5A N3 C4A 113.1(2) . . ? C5A N3 C10A 110.8(2) . . ? C4A N3 C10A 105.3(2) . . ? C10B N3 C5B 109.6(3) . . ? C4A N3 C5B 145.1(2) . . ? C10B N3 C4B 111.1(3) . . ? C5B N3 C4B 107.3(3) . . ? C10B N3 Ca1 125.8(2) . . ? C5A N3 Ca1 98.89(13) . . ? C4A N3 Ca1 106.20(13) . . ? C10A N3 Ca1 122.68(14) . . ? C5B N3 Ca1 104.70(18) . . ? C4B N3 Ca1 96.64(18) . . ? C11 N4 C6 110.25(14) . . ? C11 N4 C7 108.37(14) . . ? C6 N4 C7 111.92(14) . . ? C11 N4 Ca1 114.82(10) . . ? C6 N4 Ca1 109.91(10) . . ? C7 N4 Ca1 101.31(10) . . ? Si1 N5 Si2 127.64(8) . . ? Si1 N5 Ca1 108.68(6) . . ? Si2 N5 Ca1 122.68(7) . . ? N1 Ca1 N5 119.82(5) . . ? N1 Ca1 N4 72.98(5) . . ? N5 Ca1 N4 115.33(5) . . ? N1 Ca1 N2 72.03(5) . . ? N5 Ca1 N2 116.44(5) . . ? N4 Ca1 N2 126.89(5) . . ? N1 Ca1 N3 96.23(5) . . ? N5 Ca1 N3 143.95(5) . . ? N4 Ca1 N3 72.56(5) . . ? N2 Ca1 N3 72.96(5) . . ? N1 Ca1 C7 49.89(5) . . ? N5 Ca1 C7 110.52(5) . . ? N4 Ca1 C7 27.52(4) . . ? N2 Ca1 C7 117.99(5) . . ? N3 Ca1 C7 91.63(5) . . ? N1 Ca1 C5A 73.84(7) . . ? N5 Ca1 C5A 160.29(7) . . ? N4 Ca1 C5A 52.17(6) . . ? N2 Ca1 C5A 80.27(7) . . ? N3 Ca1 C5A 26.85(6) . . ? C7 Ca1 C5A 65.95(7) . . ? N1 Ca1 C4B 71.49(9) . . ? N5 Ca1 C4B 162.73(10) . . ? N4 Ca1 C4B 79.59(9) . . ? N2 Ca1 C4B 51.97(9) . . ? N3 Ca1 C4B 28.75(9) . . ? C7 Ca1 C4B 86.73(9) . . ? C5A Ca1 C4B 28.55(10) . . ? N1 Ca1 C2 48.92(5) . . ? N5 Ca1 C2 111.98(5) . . ? N4 Ca1 C2 117.77(5) . . ? N2 Ca1 C2 27.12(5) . . ? N3 Ca1 C2 91.35(5) . . ? C7 Ca1 C2 98.58(5) . . ? C5A Ca1 C2 87.67(7) . . ? C4B Ca1 C2 64.19(9) . . ? N1 Ca1 C8 22.88(5) . . ? N5 Ca1 C8 122.42(5) . . ? N4 Ca1 C8 50.28(5) . . ? N2 Ca1 C8 91.27(5) . . ? N3 Ca1 C8 90.42(5) . . ? C7 Ca1 C8 27.66(4) . . ? C5A Ca1 C8 64.11(7) . . ? C4B Ca1 C8 73.37(9) . . ? C2 Ca1 C8 70.98(5) . . ? N1 Ca1 C1 22.29(5) . . ? N5 Ca1 C1 123.20(5) . . ? N4 Ca1 C1 91.45(5) . . ? N2 Ca1 C1 49.85(5) . . ? N3 Ca1 C1 90.20(5) . . ? C7 Ca1 C1 71.33(5) . . ? C5A Ca1 C1 75.11(7) . . ? C4B Ca1 C1 61.82(9) . . ? C2 Ca1 C1 27.32(4) . . ? C8 Ca1 C1 43.69(5) . . ? N1 Ca1 Si1 148.34(4) . . ? N5 Ca1 Si1 28.93(3) . . ? N4 Ca1 Si1 118.47(3) . . ? N2 Ca1 Si1 112.36(4) . . ? N3 Ca1 Si1 115.21(3) . . ? C7 Ca1 Si1 128.01(4) . . ? C5A Ca1 Si1 137.36(6) . . ? C4B Ca1 Si1 137.19(9) . . ? C2 Ca1 Si1 122.64(4) . . ? C8 Ca1 Si1 148.80(4) . . ? C1 Ca1 Si1 144.73(4) . . ? N1 C1 C2 109.42(14) . . ? C2 C1 Ca1 74.62(9) . . ? N1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? Ca1 C1 H1A 112.5 . . ? N1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? Ca1 C1 H1B 134.4 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 113.25(15) . . ? N2 C2 Ca1 50.45(8) . . ? C1 C2 Ca1 78.06(9) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? Ca1 C2 H2A 88.7 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? Ca1 C2 H2B 158.0 . . ? H2A C2 H2B 107.7 . . ? N2 C3 C4A 113.47(17) . . ? N2 C3 C4B 114.6(2) . . ? C4A C3 C4B 52.6(2) . . ? N2 C3 H3A 108.9 . . ? C4A C3 H3A 108.9 . . ? C4B C3 H3A 58.6 . . ? N2 C3 H3B 108.9 . . ? C4A C3 H3B 108.9 . . ? C4B C3 H3B 136.5 . . ? H3A C3 H3B 107.7 . . ? N2 C3 H3C 108.6 . . ? C4A C3 H3C 137.9 . . ? C4B C3 H3C 108.6 . . ? H3A C3 H3C 55.0 . . ? H3B C3 H3C 55.5 . . ? N2 C3 H3D 108.6 . . ? C4A C3 H3D 59.1 . . ? C4B C3 H3D 108.6 . . ? H3A C3 H3D 142.2 . . ? H3B C3 H3D 54.5 . . ? H3C C3 H3D 107.6 . . ? N3 C4A C3 113.2(2) . . ? N3 C4A H4A 108.9 . . ? C3 C4A H4A 108.9 . . ? N3 C4A H4B 108.9 . . ? C3 C4A H4B 108.9 . . ? H4A C4A H4B 107.7 . . ? N3 C5A C6 114.5(2) . . ? N3 C5A Ca1 54.25(11) . . ? C6 C5A Ca1 82.08(12) . . ? N3 C5A H5A 108.6 . . ? C6 C5A H5A 108.6 . . ? Ca1 C5A H5A 80.3 . . ? N3 C5A H5B 108.6 . . ? C6 C5A H5B 108.6 . . ? Ca1 C5A H5B 162.9 . . ? H5A C5A H5B 107.6 . . ? N3 C4B C3 110.5(3) . . ? N3 C4B Ca1 54.61(14) . . ? C3 C4B Ca1 82.05(18) . . ? N3 C4B H4C 109.6 . . ? C3 C4B H4C 109.6 . . ? Ca1 C4B H4C 163.7 . . ? N3 C4B H4D 109.6 . . ? C3 C4B H4D 109.6 . . ? Ca1 C4B H4D 77.2 . . ? H4C C4B H4D 108.1 . . ? C6 C5B N3 118.8(3) . . ? C6 C5B H5C 107.6 . . ? N3 C5B H5C 107.6 . . ? C6 C5B H5D 107.6 . . ? N3 C5B H5D 107.6 . . ? H5C C5B H5D 107.0 . . ? C5B C6 N4 114.8(2) . . ? C5B C6 C5A 45.6(2) . . ? N4 C6 C5A 114.76(16) . . ? C5B C6 H6A 65.7 . . ? N4 C6 H6A 108.6 . . ? C5A C6 H6A 108.6 . . ? C5B C6 H6B 135.9 . . ? N4 C6 H6B 108.6 . . ? C5A C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? C5B C6 H6C 108.6 . . ? N4 C6 H6C 108.6 . . ? C5A C6 H6C 65.7 . . ? H6A C6 H6C 140.8 . . ? H6B C6 H6C 47.7 . . ? C5B C6 H6D 108.6 . . ? N4 C6 H6D 108.6 . . ? C5A C6 H6D 136.0 . . ? H6A C6 H6D 47.7 . . ? H6B C6 H6D 62.3 . . ? H6C C6 H6D 107.5 . . ? N4 C7 C8 113.42(15) . . ? N4 C7 Ca1 51.17(8) . . ? C8 C7 Ca1 78.59(10) . . ? N4 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? Ca1 C7 H7A 159.1 . . ? N4 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? Ca1 C7 H7B 87.3 . . ? H7A C7 H7B 107.7 . . ? N1 C8 C7 109.56(14) . . ? C7 C8 Ca1 73.75(9) . . ? N1 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? Ca1 C8 H8A 134.4 . . ? N1 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? Ca1 C8 H8B 113.0 . . ? H8A C8 H8B 108.2 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10A H10A 109.5 . . ? N3 C10A H10B 109.5 . . ? N3 C10A H10C 109.5 . . ? N3 C10B H10D 109.5 . . ? N3 C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? N3 C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? N4 C11 H11A 109.5 . . ? N4 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N4 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si2 C15 H15A 109.5 . . ? Si2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si2 C16 H16A 109.5 . . ? Si2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Si1 N5 Si2 -75.04(12) . . . . ? C13 Si1 N5 Si2 50.21(13) . . . . ? C12 Si1 N5 Si2 167.83(10) . . . . ? Ca1 Si1 N5 Si2 168.67(14) . . . . ? C14 Si1 N5 Ca1 116.29(8) . . . . ? C13 Si1 N5 Ca1 -118.46(8) . . . . ? C12 Si1 N5 Ca1 -0.84(9) . . . . ? C15 Si2 N5 Si1 -94.38(11) . . . . ? C17 Si2 N5 Si1 146.28(10) . . . . ? C16 Si2 N5 Si1 25.69(13) . . . . ? Ca1 Si2 N5 Si1 -167.22(16) . . . . ? C15 Si2 N5 Ca1 72.84(10) . . . . ? C17 Si2 N5 Ca1 -46.50(10) . . . . ? C16 Si2 N5 Ca1 -167.09(8) . . . . ? C1 N1 Ca1 N5 -105.40(13) . . . . ? C8 N1 Ca1 N5 103.35(13) . . . . ? C1 N1 Ca1 N4 144.70(13) . . . . ? C8 N1 Ca1 N4 -6.55(12) . . . . ? C1 N1 Ca1 N2 5.31(12) . . . . ? C8 N1 Ca1 N2 -145.94(14) . . . . ? C1 N1 Ca1 N3 75.11(13) . . . . ? C8 N1 Ca1 N3 -76.14(13) . . . . ? C1 N1 Ca1 C7 161.99(15) . . . . ? C8 N1 Ca1 C7 10.74(12) . . . . ? C1 N1 Ca1 C5A 90.09(14) . . . . ? C8 N1 Ca1 C5A -61.16(14) . . . . ? C1 N1 Ca1 C4B 60.26(15) . . . . ? C8 N1 Ca1 C4B -90.99(15) . . . . ? C1 N1 Ca1 C2 -11.24(11) . . . . ? C8 N1 Ca1 C2 -162.49(16) . . . . ? C1 N1 Ca1 C8 151.2(2) . . . . ? C8 N1 Ca1 C1 -151.2(2) . . . . ? C1 N1 Ca1 Si1 -98.34(13) . . . . ? C8 N1 Ca1 Si1 110.41(13) . . . . ? Si1 N5 Ca1 N1 172.33(6) . . . . ? Si2 N5 Ca1 N1 2.99(10) . . . . ? Si1 N5 Ca1 N4 -103.51(7) . . . . ? Si2 N5 Ca1 N4 87.14(9) . . . . ? Si1 N5 Ca1 N2 88.77(7) . . . . ? Si2 N5 Ca1 N2 -80.58(9) . . . . ? Si1 N5 Ca1 N3 -8.53(12) . . . . ? Si2 N5 Ca1 N3 -177.88(7) . . . . ? Si1 N5 Ca1 C7 -133.00(6) . . . . ? Si2 N5 Ca1 C7 57.65(9) . . . . ? Si1 N5 Ca1 C5A -57.2(2) . . . . ? Si2 N5 Ca1 C5A 133.45(18) . . . . ? Si1 N5 Ca1 C4B 44.7(3) . . . . ? Si2 N5 Ca1 C4B -124.7(3) . . . . ? Si1 N5 Ca1 C2 118.17(7) . . . . ? Si2 N5 Ca1 C2 -51.18(9) . . . . ? Si1 N5 Ca1 C8 -161.04(6) . . . . ? Si2 N5 Ca1 C8 29.61(10) . . . . ? Si1 N5 Ca1 C1 146.42(6) . . . . ? Si2 N5 Ca1 C1 -22.93(10) . . . . ? Si2 N5 Ca1 Si1 -169.35(13) . . . . ? C11 N4 Ca1 N1 145.99(13) . . . . ? C6 N4 Ca1 N1 -89.05(11) . . . . ? C7 N4 Ca1 N1 29.46(10) . . . . ? C11 N4 Ca1 N5 30.48(13) . . . . ? C6 N4 Ca1 N5 155.45(10) . . . . ? C7 N4 Ca1 N5 -86.04(11) . . . . ? C11 N4 Ca1 N2 -163.29(11) . . . . ? C6 N4 Ca1 N2 -38.33(13) . . . . ? C7 N4 Ca1 N2 80.19(11) . . . . ? C11 N4 Ca1 N3 -111.59(12) . . . . ? C6 N4 Ca1 N3 13.37(11) . . . . ? C7 N4 Ca1 N3 131.88(11) . . . . ? C11 N4 Ca1 C7 116.53(17) . . . . ? C6 N4 Ca1 C7 -118.51(16) . . . . ? C11 N4 Ca1 C5A -131.53(15) . . . . ? C6 N4 Ca1 C5A -6.57(12) . . . . ? C7 N4 Ca1 C5A 111.94(13) . . . . ? C11 N4 Ca1 C4B -140.36(15) . . . . ? C6 N4 Ca1 C4B -15.39(13) . . . . ? C7 N4 Ca1 C4B 103.12(13) . . . . ? C11 N4 Ca1 C2 166.30(11) . . . . ? C6 N4 Ca1 C2 -68.73(12) . . . . ? C7 N4 Ca1 C2 49.78(11) . . . . ? C11 N4 Ca1 C8 142.68(14) . . . . ? C6 N4 Ca1 C8 -92.35(12) . . . . ? C7 N4 Ca1 C8 26.16(10) . . . . ? C11 N4 Ca1 C1 158.65(12) . . . . ? C6 N4 Ca1 C1 -76.38(11) . . . . ? C7 N4 Ca1 C1 42.13(10) . . . . ? C11 N4 Ca1 Si1 -1.86(13) . . . . ? C6 N4 Ca1 Si1 123.10(10) . . . . ? C7 N4 Ca1 Si1 -118.39(9) . . . . ? C9 N2 Ca1 N1 -146.61(13) . . . . ? C3 N2 Ca1 N1 89.51(12) . . . . ? C2 N2 Ca1 N1 -28.10(10) . . . . ? C9 N2 Ca1 N5 -31.61(14) . . . . ? C3 N2 Ca1 N5 -155.49(11) . . . . ? C2 N2 Ca1 N5 86.90(11) . . . . ? C9 N2 Ca1 N4 162.30(11) . . . . ? C3 N2 Ca1 N4 38.42(13) . . . . ? C2 N2 Ca1 N4 -79.19(11) . . . . ? C9 N2 Ca1 N3 110.76(13) . . . . ? C3 N2 Ca1 N3 -13.12(11) . . . . ? C2 N2 Ca1 N3 -130.73(11) . . . . ? C9 N2 Ca1 C7 -166.66(12) . . . . ? C3 N2 Ca1 C7 69.46(12) . . . . ? C2 N2 Ca1 C7 -48.15(11) . . . . ? C9 N2 Ca1 C5A 137.36(14) . . . . ? C3 N2 Ca1 C5A 13.47(12) . . . . ? C2 N2 Ca1 C5A -104.14(12) . . . . ? C9 N2 Ca1 C4B 133.19(17) . . . . ? C3 N2 Ca1 C4B 9.31(15) . . . . ? C2 N2 Ca1 C4B -108.31(15) . . . . ? C9 N2 Ca1 C2 -118.51(17) . . . . ? C3 N2 Ca1 C2 117.61(16) . . . . ? C9 N2 Ca1 C8 -159.19(12) . . . . ? C3 N2 Ca1 C8 76.93(12) . . . . ? C2 N2 Ca1 C8 -40.68(11) . . . . ? C9 N2 Ca1 C1 -143.97(14) . . . . ? C3 N2 Ca1 C1 92.14(12) . . . . ? C2 N2 Ca1 C1 -25.47(10) . . . . ? C9 N2 Ca1 Si1 -0.07(13) . . . . ? C3 N2 Ca1 Si1 -123.96(11) . . . . ? C2 N2 Ca1 Si1 118.43(10) . . . . ? C10B N3 Ca1 N1 -152.5(3) . . . . ? C5A N3 Ca1 N1 33.35(16) . . . . ? C4A N3 Ca1 N1 -83.98(15) . . . . ? C10A N3 Ca1 N1 155.2(2) . . . . ? C5B N3 Ca1 N1 79.5(2) . . . . ? C4B N3 Ca1 N1 -30.4(2) . . . . ? C10B N3 Ca1 N5 28.3(4) . . . . ? C5A N3 Ca1 N5 -145.90(15) . . . . ? C4A N3 Ca1 N5 96.77(16) . . . . ? C10A N3 Ca1 N5 -24.0(2) . . . . ? C5B N3 Ca1 N5 -99.7(2) . . . . ? C4B N3 Ca1 N5 150.40(19) . . . . ? C10B N3 Ca1 N4 137.6(3) . . . . ? C5A N3 Ca1 N4 -36.60(15) . . . . ? C4A N3 Ca1 N4 -153.93(16) . . . . ? C10A N3 Ca1 N4 85.3(2) . . . . ? C5B N3 Ca1 N4 9.6(2) . . . . ? C4B N3 Ca1 N4 -100.3(2) . . . . ? C10B N3 Ca1 N2 -83.4(3) . . . . ? C5A N3 Ca1 N2 102.37(15) . . . . ? C4A N3 Ca1 N2 -14.96(15) . . . . ? C10A N3 Ca1 N2 -135.8(2) . . . . ? C5B N3 Ca1 N2 148.5(2) . . . . ? C4B N3 Ca1 N2 38.66(19) . . . . ? C10B N3 Ca1 C7 157.7(3) . . . . ? C5A N3 Ca1 C7 -16.47(15) . . . . ? C4A N3 Ca1 C7 -133.80(15) . . . . ? C10A N3 Ca1 C7 105.4(2) . . . . ? C5B N3 Ca1 C7 29.7(2) . . . . ? C4B N3 Ca1 C7 -80.17(19) . . . . ? C10B N3 Ca1 C5A 174.2(4) . . . . ? C4A N3 Ca1 C5A -117.3(2) . . . . ? C10A N3 Ca1 C5A 121.9(2) . . . . ? C5B N3 Ca1 C5A 46.2(2) . . . . ? C4B N3 Ca1 C5A -63.7(2) . . . . ? C10B N3 Ca1 C4B -122.1(4) . . . . ? C5A N3 Ca1 C4B 63.7(2) . . . . ? C4A N3 Ca1 C4B -53.6(2) . . . . ? C10A N3 Ca1 C4B -174.4(3) . . . . ? C5B N3 Ca1 C4B 109.9(3) . . . . ? C10B N3 Ca1 C2 -103.7(3) . . . . ? C5A N3 Ca1 C2 82.15(15) . . . . ? C4A N3 Ca1 C2 -35.18(15) . . . . ? C10A N3 Ca1 C2 -156.0(2) . . . . ? C5B N3 Ca1 C2 128.3(2) . . . . ? C4B N3 Ca1 C2 18.4(2) . . . . ? C10B N3 Ca1 C8 -174.6(3) . . . . ? C5A N3 Ca1 C8 11.17(15) . . . . ? C4A N3 Ca1 C8 -106.16(15) . . . . ? C10A N3 Ca1 C8 133.0(2) . . . . ? C5B N3 Ca1 C8 57.3(2) . . . . ? C4B N3 Ca1 C8 -52.5(2) . . . . ? C10B N3 Ca1 C1 -131.0(3) . . . . ? C5A N3 Ca1 C1 54.86(15) . . . . ? C4A N3 Ca1 C1 -62.47(15) . . . . ? C10A N3 Ca1 C1 176.7(2) . . . . ? C5B N3 Ca1 C1 101.0(2) . . . . ? C4B N3 Ca1 C1 -8.85(19) . . . . ? C10B N3 Ca1 Si1 23.7(3) . . . . ? C5A N3 Ca1 Si1 -150.45(14) . . . . ? C4A N3 Ca1 Si1 92.22(15) . . . . ? C10A N3 Ca1 Si1 -28.6(2) . . . . ? C5B N3 Ca1 Si1 -104.3(2) . . . . ? C4B N3 Ca1 Si1 145.85(19) . . . . ? N5 Si1 Ca1 N1 -12.74(10) . . . . ? C14 Si1 Ca1 N1 -101.78(10) . . . . ? C13 Si1 Ca1 N1 75.27(11) . . . . ? C12 Si1 Ca1 N1 166.38(10) . . . . ? C14 Si1 Ca1 N5 -89.05(10) . . . . ? C13 Si1 Ca1 N5 88.01(10) . . . . ? C12 Si1 Ca1 N5 179.12(9) . . . . ? N5 Si1 Ca1 N4 91.44(8) . . . . ? C14 Si1 Ca1 N4 2.40(8) . . . . ? C13 Si1 Ca1 N4 179.45(9) . . . . ? C12 Si1 Ca1 N4 -89.44(7) . . . . ? N5 Si1 Ca1 N2 -104.55(8) . . . . ? C14 Si1 Ca1 N2 166.41(8) . . . . ? C13 Si1 Ca1 N2 -16.54(9) . . . . ? C12 Si1 Ca1 N2 74.57(7) . . . . ? N5 Si1 Ca1 N3 174.46(8) . . . . ? C14 Si1 Ca1 N3 85.42(8) . . . . ? C13 Si1 Ca1 N3 -97.53(9) . . . . ? C12 Si1 Ca1 N3 -6.42(7) . . . . ? N5 Si1 Ca1 C7 60.38(8) . . . . ? C14 Si1 Ca1 C7 -28.66(9) . . . . ? C13 Si1 Ca1 C7 148.39(9) . . . . ? C12 Si1 Ca1 C7 -120.50(8) . . . . ? N5 Si1 Ca1 C5A 155.26(11) . . . . ? C14 Si1 Ca1 C5A 66.22(11) . . . . ? C13 Si1 Ca1 C5A -116.73(11) . . . . ? C12 Si1 Ca1 C5A -25.62(10) . . . . ? N5 Si1 Ca1 C4B -162.12(14) . . . . ? C14 Si1 Ca1 C4B 108.83(14) . . . . ? C13 Si1 Ca1 C4B -74.11(15) . . . . ? C12 Si1 Ca1 C4B 16.99(14) . . . . ? N5 Si1 Ca1 C2 -76.11(8) . . . . ? C14 Si1 Ca1 C2 -165.16(8) . . . . ? C13 Si1 Ca1 C2 11.90(9) . . . . ? C12 Si1 Ca1 C2 103.00(7) . . . . ? N5 Si1 Ca1 C8 31.97(10) . . . . ? C14 Si1 Ca1 C8 -57.08(10) . . . . ? C13 Si1 Ca1 C8 119.98(11) . . . . ? C12 Si1 Ca1 C8 -148.91(9) . . . . ? N5 Si1 Ca1 C1 -53.28(9) . . . . ? C14 Si1 Ca1 C1 -142.33(9) . . . . ? C13 Si1 Ca1 C1 34.73(10) . . . . ? C12 Si1 Ca1 C1 125.84(9) . . . . ? C8 N1 C1 C2 171.98(15) . . . . ? Ca1 N1 C1 C2 19.11(19) . . . . ? C8 N1 C1 Ca1 152.9(2) . . . . ? N5 Ca1 C1 N1 88.32(13) . . . . ? N4 Ca1 C1 N1 -33.55(13) . . . . ? N2 Ca1 C1 N1 -173.39(15) . . . . ? N3 Ca1 C1 N1 -106.11(13) . . . . ? C7 Ca1 C1 N1 -14.45(12) . . . . ? C5A Ca1 C1 N1 -83.64(14) . . . . ? C4B Ca1 C1 N1 -110.93(16) . . . . ? C2 Ca1 C1 N1 161.32(19) . . . . ? C8 Ca1 C1 N1 -15.71(12) . . . . ? Si1 Ca1 C1 N1 115.93(12) . . . . ? N1 Ca1 C1 C2 -161.32(19) . . . . ? N5 Ca1 C1 C2 -73.00(11) . . . . ? N4 Ca1 C1 C2 165.12(10) . . . . ? N2 Ca1 C1 C2 25.29(9) . . . . ? N3 Ca1 C1 C2 92.56(10) . . . . ? C7 Ca1 C1 C2 -175.78(11) . . . . ? C5A Ca1 C1 C2 115.04(11) . . . . ? C4B Ca1 C1 C2 87.75(14) . . . . ? C8 Ca1 C1 C2 -177.03(13) . . . . ? Si1 Ca1 C1 C2 -45.40(13) . . . . ? C9 N2 C2 C1 171.91(14) . . . . ? C3 N2 C2 C1 -66.62(19) . . . . ? Ca1 N2 C2 C1 49.70(15) . . . . ? C9 N2 C2 Ca1 122.21(14) . . . . ? C3 N2 C2 Ca1 -116.32(14) . . . . ? N1 C1 C2 N2 -48.6(2) . . . . ? Ca1 C1 C2 N2 -36.94(12) . . . . ? N1 C1 C2 Ca1 -11.69(12) . . . . ? N1 Ca1 C2 N2 143.53(12) . . . . ? N5 Ca1 C2 N2 -105.39(10) . . . . ? N4 Ca1 C2 N2 117.39(10) . . . . ? N3 Ca1 C2 N2 46.44(10) . . . . ? C7 Ca1 C2 N2 138.30(10) . . . . ? C5A Ca1 C2 N2 73.05(11) . . . . ? C4B Ca1 C2 N2 56.18(13) . . . . ? C8 Ca1 C2 N2 136.42(11) . . . . ? C1 Ca1 C2 N2 134.26(16) . . . . ? Si1 Ca1 C2 N2 -74.97(10) . . . . ? N1 Ca1 C2 C1 9.27(9) . . . . ? N5 Ca1 C2 C1 120.35(10) . . . . ? N4 Ca1 C2 C1 -16.86(12) . . . . ? N2 Ca1 C2 C1 -134.26(16) . . . . ? N3 Ca1 C2 C1 -87.81(10) . . . . ? C7 Ca1 C2 C1 4.04(11) . . . . ? C5A Ca1 C2 C1 -61.21(11) . . . . ? C4B Ca1 C2 C1 -78.08(14) . . . . ? C8 Ca1 C2 C1 2.17(10) . . . . ? Si1 Ca1 C2 C1 150.78(9) . . . . ? C9 N2 C3 C4A -85.3(2) . . . . ? C2 N2 C3 C4A 153.54(19) . . . . ? Ca1 N2 C3 C4A 41.4(2) . . . . ? C9 N2 C3 C4B -143.3(2) . . . . ? C2 N2 C3 C4B 95.5(3) . . . . ? Ca1 N2 C3 C4B -16.6(3) . . . . ? C10B N3 C4A C3 165.0(3) . . . . ? C5A N3 C4A C3 -64.8(3) . . . . ? C10A N3 C4A C3 174.1(2) . . . . ? C5B N3 C4A C3 -108.7(4) . . . . ? C4B N3 C4A C3 -43.6(3) . . . . ? Ca1 N3 C4A C3 42.6(2) . . . . ? N2 C3 C4A N3 -60.4(3) . . . . ? C4B C3 C4A N3 43.5(2) . . . . ? C10B N3 C5A C6 -114.2(4) . . . . ? C4A N3 C5A C6 171.0(2) . . . . ? C10A N3 C5A C6 -71.0(3) . . . . ? C5B N3 C5A C6 -42.8(3) . . . . ? C4B N3 C5A C6 152.1(3) . . . . ? Ca1 N3 C5A C6 59.1(2) . . . . ? C10B N3 C5A Ca1 -173.3(4) . . . . ? C4A N3 C5A Ca1 111.95(18) . . . . ? C10A N3 C5A Ca1 -130.12(19) . . . . ? C5B N3 C5A Ca1 -101.9(3) . . . . ? C4B N3 C5A Ca1 93.0(2) . . . . ? N1 Ca1 C5A N3 -145.32(16) . . . . ? N5 Ca1 C5A N3 78.1(2) . . . . ? N4 Ca1 C5A N3 133.93(18) . . . . ? N2 Ca1 C5A N3 -71.35(14) . . . . ? C7 Ca1 C5A N3 161.92(17) . . . . ? C4B Ca1 C5A N3 -64.5(2) . . . . ? C2 Ca1 C5A N3 -97.62(15) . . . . ? C8 Ca1 C5A N3 -167.57(17) . . . . ? C1 Ca1 C5A N3 -122.21(15) . . . . ? Si1 Ca1 C5A N3 41.20(19) . . . . ? N1 Ca1 C5A C6 86.72(14) . . . . ? N5 Ca1 C5A C6 -49.9(3) . . . . ? N4 Ca1 C5A C6 5.97(11) . . . . ? N2 Ca1 C5A C6 160.69(15) . . . . ? N3 Ca1 C5A C6 -128.0(2) . . . . ? C7 Ca1 C5A C6 33.97(13) . . . . ? C4B Ca1 C5A C6 167.6(3) . . . . ? C2 Ca1 C5A C6 134.43(14) . . . . ? C8 Ca1 C5A C6 64.48(13) . . . . ? C1 Ca1 C5A C6 109.83(15) . . . . ? Si1 Ca1 C5A C6 -86.75(15) . . . . ? C10B N3 C4B C3 69.0(4) . . . . ? C5A N3 C4B C3 -160.1(4) . . . . ? C4A N3 C4B C3 41.8(2) . . . . ? C10A N3 C4B C3 109.1(4) . . . . ? C5B N3 C4B C3 -171.2(3) . . . . ? Ca1 N3 C4B C3 -63.5(3) . . . . ? C10B N3 C4B Ca1 132.5(3) . . . . ? C5A N3 C4B Ca1 -96.62(17) . . . . ? C4A N3 C4B Ca1 105.28(19) . . . . ? C10A N3 C4B Ca1 172.6(4) . . . . ? C5B N3 C4B Ca1 -107.7(2) . . . . ? N2 C3 C4B N3 60.0(3) . . . . ? C4A C3 C4B N3 -41.6(2) . . . . ? N2 C3 C4B Ca1 12.59(19) . . . . ? C4A C3 C4B Ca1 -89.0(2) . . . . ? N1 Ca1 C4B N3 148.0(2) . . . . ? N5 Ca1 C4B N3 -78.4(4) . . . . ? N4 Ca1 C4B N3 72.62(17) . . . . ? N2 Ca1 C4B N3 -130.7(2) . . . . ? C7 Ca1 C4B N3 99.41(18) . . . . ? C5A Ca1 C4B N3 57.9(2) . . . . ? C2 Ca1 C4B N3 -159.4(2) . . . . ? C8 Ca1 C4B N3 124.07(19) . . . . ? C1 Ca1 C4B N3 169.9(2) . . . . ? Si1 Ca1 C4B N3 -48.4(2) . . . . ? N1 Ca1 C4B C3 -89.85(19) . . . . ? N5 Ca1 C4B C3 43.8(4) . . . . ? N4 Ca1 C4B C3 -165.2(2) . . . . ? N2 Ca1 C4B C3 -8.54(13) . . . . ? N3 Ca1 C4B C3 122.1(3) . . . . ? C7 Ca1 C4B C3 -138.45(19) . . . . ? C5A Ca1 C4B C3 -179.9(4) . . . . ? C2 Ca1 C4B C3 -37.28(16) . . . . ? C8 Ca1 C4B C3 -113.79(19) . . . . ? C1 Ca1 C4B C3 -67.91(17) . . . . ? Si1 Ca1 C4B C3 73.8(2) . . . . ? C10B N3 C5B C6 -173.8(4) . . . . ? C5A N3 C5B C6 51.6(3) . . . . ? C4A N3 C5B C6 115.1(4) . . . . ? C10A N3 C5B C6 -156.4(4) . . . . ? C4B N3 C5B C6 65.5(4) . . . . ? Ca1 N3 C5B C6 -36.5(4) . . . . ? N3 C5B C6 N4 54.4(4) . . . . ? N3 C5B C6 C5A -46.7(3) . . . . ? C11 N4 C6 C5B 88.7(3) . . . . ? C7 N4 C6 C5B -150.6(3) . . . . ? Ca1 N4 C6 C5B -38.8(3) . . . . ? C11 N4 C6 C5A 139.2(2) . . . . ? C7 N4 C6 C5A -100.1(2) . . . . ? Ca1 N4 C6 C5A 11.7(2) . . . . ? N3 C5A C6 C5B 47.9(3) . . . . ? Ca1 C5A C6 C5B 92.5(3) . . . . ? N3 C5A C6 N4 -53.4(3) . . . . ? Ca1 C5A C6 N4 -8.78(16) . . . . ? C11 N4 C7 C8 -172.45(15) . . . . ? C6 N4 C7 C8 65.76(19) . . . . ? Ca1 N4 C7 C8 -51.29(15) . . . . ? C11 N4 C7 Ca1 -121.16(13) . . . . ? C6 N4 C7 Ca1 117.05(14) . . . . ? N1 Ca1 C7 N4 -142.05(13) . . . . ? N5 Ca1 C7 N4 105.68(10) . . . . ? N2 Ca1 C7 N4 -116.81(10) . . . . ? N3 Ca1 C7 N4 -45.28(10) . . . . ? C5A Ca1 C7 N4 -53.34(11) . . . . ? C4B Ca1 C7 N4 -73.62(13) . . . . ? C2 Ca1 C7 N4 -136.90(10) . . . . ? C8 Ca1 C7 N4 -133.07(16) . . . . ? C1 Ca1 C7 N4 -134.94(11) . . . . ? Si1 Ca1 C7 N4 78.99(11) . . . . ? N1 Ca1 C7 C8 -8.98(10) . . . . ? N5 Ca1 C7 C8 -121.25(11) . . . . ? N4 Ca1 C7 C8 133.07(16) . . . . ? N2 Ca1 C7 C8 16.26(12) . . . . ? N3 Ca1 C7 C8 87.79(11) . . . . ? C5A Ca1 C7 C8 79.73(12) . . . . ? C4B Ca1 C7 C8 59.45(13) . . . . ? C2 Ca1 C7 C8 -3.83(11) . . . . ? C1 Ca1 C7 C8 -1.87(10) . . . . ? Si1 Ca1 C7 C8 -147.93(9) . . . . ? C1 N1 C8 C7 -171.53(15) . . . . ? Ca1 N1 C8 C7 -18.2(2) . . . . ? C1 N1 C8 Ca1 -153.3(2) . . . . ? N4 C7 C8 N1 49.8(2) . . . . ? Ca1 C7 C8 N1 11.45(13) . . . . ? N4 C7 C8 Ca1 38.33(12) . . . . ? N5 Ca1 C8 N1 -90.60(13) . . . . ? N4 Ca1 C8 N1 171.85(15) . . . . ? N2 Ca1 C8 N1 32.20(13) . . . . ? N3 Ca1 C8 N1 105.16(13) . . . . ? C7 Ca1 C8 N1 -162.1(2) . . . . ? C5A Ca1 C8 N1 110.75(15) . . . . ? C4B Ca1 C8 N1 81.68(15) . . . . ? C2 Ca1 C8 N1 13.88(12) . . . . ? C1 Ca1 C8 N1 15.32(12) . . . . ? Si1 Ca1 C8 N1 -108.26(13) . . . . ? N1 Ca1 C8 C7 162.1(2) . . . . ? N5 Ca1 C8 C7 71.52(12) . . . . ? N4 Ca1 C8 C7 -26.03(10) . . . . ? N2 Ca1 C8 C7 -165.68(11) . . . . ? N3 Ca1 C8 C7 -92.72(11) . . . . ? C5A Ca1 C8 C7 -87.13(12) . . . . ? C4B Ca1 C8 C7 -116.20(14) . . . . ? C2 Ca1 C8 C7 176.00(12) . . . . ? C1 Ca1 C8 C7 177.44(14) . . . . ? Si1 Ca1 C8 C7 53.86(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.431 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.051 #==END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H52 Ca N6 Si4' _chemical_formula_sum 'C19 H52 Ca N6 Si4' _chemical_formula_weight 517.11 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' 'Ca' 'Ca' 0.2262 0.3064 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 19.245(2) _cell_length_b 10.3101(10) _cell_length_c 15.582(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.38(2) _cell_angle_gamma 90.00 _cell_volume 2966.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 8317 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 29.6 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas 1.16 _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.391 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9086 _exptl_absorpt_correction_T_max 0.9694 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'INCOATEC microsource' _diffrn_radiation_monochromator 'multilayer optics' _diffrn_measurement_device_type 'APEX Area Detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42827 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 29.63 _reflns_number_total 8317 _reflns_number_gt 6949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (2001)' _computing_cell_refinement 'Bruker SMART (2001)' _computing_data_reduction 'Bruker SAINT+ (1999)' _computing_structure_solution 'SIR-92 (Altomare 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-III (Farrugia, 1999)' _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^)+(0.0648P)^2^+1.5403P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8317 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1085 _refine_ls_wR_factor_gt 0.0986 _refine_ls_goodness_of_fit_ref 0.914 _refine_ls_restrained_S_all 0.914 _refine_ls_shift/su_max 0.003 _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 0.59214(2) 0.83676(4) 0.13086(3) 0.01905(9) Uani 1 1 d . . . Si2 Si 0.66225(2) 0.57909(4) 0.19740(3) 0.02150(10) Uani 1 1 d . . . Si3 Si 0.90351(2) 0.70827(4) 0.38028(3) 0.02052(10) Uani 1 1 d . . . Si4 Si 0.87521(2) 0.73721(4) 0.18207(3) 0.01951(9) Uani 1 1 d . . . N1 N 0.62222(7) 0.99787(12) 0.16569(9) 0.0211(3) Uani 1 1 d . . . N2 N 0.70029(7) 0.97486(14) 0.36402(9) 0.0241(3) Uani 1 1 d . . . N3 N 0.83628(7) 1.08857(13) 0.34036(10) 0.0257(3) Uani 1 1 d . . . N4 N 0.76061(8) 1.10062(13) 0.14234(9) 0.0242(3) Uani 1 1 d . . . N5 N 0.65863(7) 0.74190(12) 0.19002(9) 0.0210(3) Uani 1 1 d . . . N6 N 0.85686(7) 0.76508(12) 0.27952(8) 0.0194(2) Uani 1 1 d . . . Ca1 Ca 0.753766(15) 0.89733(3) 0.242618(19) 0.01576(7) Uani 1 1 d . . . C1 C 0.59665(9) 1.05614(17) 0.23772(12) 0.0270(3) Uani 1 1 d . . . H1A H 0.5431 1.0600 0.2181 0.032 Uiso 1 1 calc R . . H1B H 0.6149 1.1462 0.2478 0.032 Uiso 1 1 calc R . . C2 C 0.62045(9) 0.98269(17) 0.32539(11) 0.0271(3) Uani 1 1 d . . . H2A H 0.5994 1.0254 0.3692 0.032 Uiso 1 1 calc R . . H2B H 0.6006 0.8936 0.3157 0.032 Uiso 1 1 calc R . . C3 C 0.72994(10) 1.10017(18) 0.40190(13) 0.0329(4) Uani 1 1 d . . . H3A H 0.7167 1.1152 0.4581 0.039 Uiso 1 1 calc R . . H3B H 0.7077 1.1700 0.3595 0.039 Uiso 1 1 calc R . . C4 C 0.81159(10) 1.10756(19) 0.42128(13) 0.0338(4) Uani 1 1 d . . . H4A H 0.8284 1.1933 0.4476 0.041 Uiso 1 1 calc R . . H4B H 0.8340 1.0405 0.4660 0.041 Uiso 1 1 calc R . . C5 C 0.82609(10) 1.20772(16) 0.28614(13) 0.0325(4) Uani 1 1 d . . . H5A H 0.8664 1.2683 0.3123 0.039 Uiso 1 1 calc R . . H5B H 0.7804 1.2502 0.2880 0.039 Uiso 1 1 calc R . . C6 C 0.82340(10) 1.18117(17) 0.19039(14) 0.0336(4) Uani 1 1 d . . . H6A H 0.8214 1.2648 0.1586 0.040 Uiso 1 1 calc R . . H6B H 0.8686 1.1365 0.1889 0.040 Uiso 1 1 calc R . . C7 C 0.69370(9) 1.17790(16) 0.12612(12) 0.0278(3) Uani 1 1 d . . . H7A H 0.6927 1.2427 0.0789 0.033 Uiso 1 1 calc R . . H7B H 0.6942 1.2256 0.1814 0.033 Uiso 1 1 calc R . . C8 C 0.62560(9) 1.09566(16) 0.09778(12) 0.0274(3) Uani 1 1 d . . . H8A H 0.5827 1.1529 0.0868 0.033 Uiso 1 1 calc R . . H8B H 0.6239 1.0511 0.0409 0.033 Uiso 1 1 calc R . . C9 C 0.71607(11) 0.8734(2) 0.43362(12) 0.0349(4) Uani 1 1 d . . . H9A H 0.7686 0.8661 0.4597 0.052 Uiso 1 1 calc R . . H9B H 0.6967 0.7903 0.4069 0.052 Uiso 1 1 calc R . . H9C H 0.6934 0.8965 0.4805 0.052 Uiso 1 1 calc R . . C10 C 0.91436(9) 1.05722(17) 0.36965(13) 0.0304(4) Uani 1 1 d . . . H10A H 0.9317 1.0417 0.3171 0.046 Uiso 1 1 calc R . . H10B H 0.9221 0.9792 0.4071 0.046 Uiso 1 1 calc R . . H10C H 0.9411 1.1299 0.4042 0.046 Uiso 1 1 calc R . . C11 C 0.77170(11) 1.05929(18) 0.05685(12) 0.0341(4) Uani 1 1 d . . . H11A H 0.7323 1.0011 0.0259 0.051 Uiso 1 1 calc R . . H11B H 0.8181 1.0137 0.0682 0.051 Uiso 1 1 calc R . . H11C H 0.7721 1.1356 0.0195 0.051 Uiso 1 1 calc R . . C12 C 0.57682(10) 0.82794(18) 0.00648(11) 0.0298(4) Uani 1 1 d . . . H12A H 0.6226 0.8436 -0.0076 0.045 Uiso 1 1 calc R . . H12B H 0.5414 0.8939 -0.0228 0.045 Uiso 1 1 calc R . . H12C H 0.5584 0.7417 -0.0150 0.045 Uiso 1 1 calc R . . C13 C 0.49992(9) 0.81205(17) 0.14727(13) 0.0296(4) Uani 1 1 d . . . H13A H 0.4778 0.7338 0.1153 0.044 Uiso 1 1 calc R . . H13B H 0.4693 0.8873 0.1238 0.044 Uiso 1 1 calc R . . H13C H 0.5046 0.8022 0.2112 0.044 Uiso 1 1 calc R . . C14 C 0.66958(13) 0.5201(2) 0.31331(14) 0.0422(5) Uani 1 1 d . . . H14A H 0.7122 0.5590 0.3554 0.063 Uiso 1 1 calc R . . H14B H 0.6744 0.4254 0.3152 0.063 Uiso 1 1 calc R . . H14C H 0.6260 0.5449 0.3300 0.063 Uiso 1 1 calc R . . C15 C 0.58257(11) 0.49038(18) 0.12256(16) 0.0424(5) Uani 1 1 d . . . H15A H 0.5382 0.5173 0.1366 0.064 Uiso 1 1 calc R . . H15B H 0.5894 0.3967 0.1321 0.064 Uiso 1 1 calc R . . H15C H 0.5786 0.5109 0.0599 0.064 Uiso 1 1 calc R . . C16 C 0.88840(10) 0.53270(18) 0.40087(13) 0.0334(4) Uani 1 1 d . . . H16A H 0.8363 0.5149 0.3846 0.050 Uiso 1 1 calc R . . H16B H 0.9100 0.5127 0.4643 0.050 Uiso 1 1 calc R . . H16C H 0.9110 0.4787 0.3645 0.050 Uiso 1 1 calc R . . C17 C 1.00443(9) 0.72575(18) 0.40669(12) 0.0303(4) Uani 1 1 d . . . H17A H 1.0223 0.6708 0.3662 0.045 Uiso 1 1 calc R . . H17B H 1.0270 0.6991 0.4687 0.045 Uiso 1 1 calc R . . H17C H 1.0166 0.8165 0.3990 0.045 Uiso 1 1 calc R . . C18 C 0.95355(9) 0.83244(17) 0.16531(12) 0.0287(3) Uani 1 1 d . . . H18A H 0.9448 0.9253 0.1710 0.043 Uiso 1 1 calc R . . H18B H 0.9586 0.8147 0.1056 0.043 Uiso 1 1 calc R . . H18C H 0.9981 0.8070 0.2106 0.043 Uiso 1 1 calc R . . C19 C 0.89111(10) 0.56433(16) 0.15553(12) 0.0286(3) Uani 1 1 d . . . H19A H 0.9306 0.5281 0.2038 0.043 Uiso 1 1 calc R . . H19B H 0.9041 0.5607 0.0992 0.043 Uiso 1 1 calc R . . H19C H 0.8469 0.5139 0.1498 0.043 Uiso 1 1 calc R . . H4 H 0.8128(11) 0.7816(19) 0.1116(13) 0.029(5) Uiso 1 1 d . . . H3 H 0.8829(11) 0.779(2) 0.4459(13) 0.032(5) Uiso 1 1 d . . . H2 H 0.7238(11) 0.523(2) 0.1748(13) 0.034(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.01340(18) 0.0181(2) 0.0248(2) 0.00056(15) 0.00400(15) 0.00044(14) Si2 0.0166(2) 0.0161(2) 0.0311(2) 0.00005(16) 0.00568(17) 0.00028(15) Si3 0.0206(2) 0.0193(2) 0.0218(2) -0.00086(15) 0.00618(16) 0.00305(15) Si4 0.01689(19) 0.0194(2) 0.0217(2) -0.00161(15) 0.00466(15) 0.00158(15) N1 0.0194(6) 0.0165(6) 0.0282(6) 0.0007(5) 0.0078(5) 0.0021(5) N2 0.0236(6) 0.0265(7) 0.0245(6) -0.0035(5) 0.0102(5) -0.0002(5) N3 0.0192(6) 0.0208(6) 0.0358(7) -0.0084(5) 0.0056(5) -0.0008(5) N4 0.0262(7) 0.0195(6) 0.0301(7) 0.0025(5) 0.0130(6) -0.0004(5) N5 0.0149(6) 0.0162(6) 0.0295(7) 0.0010(5) 0.0025(5) -0.0003(4) N6 0.0162(6) 0.0196(6) 0.0223(6) -0.0020(5) 0.0052(5) 0.0026(5) Ca1 0.01345(13) 0.01441(14) 0.01971(14) -0.00075(10) 0.00515(10) 0.00034(9) C1 0.0193(7) 0.0261(8) 0.0367(9) -0.0048(7) 0.0100(6) 0.0043(6) C2 0.0228(8) 0.0300(8) 0.0326(8) -0.0049(7) 0.0146(7) 0.0005(6) C3 0.0311(9) 0.0328(9) 0.0368(9) -0.0159(7) 0.0128(7) -0.0018(7) C4 0.0283(9) 0.0367(10) 0.0349(9) -0.0177(8) 0.0065(7) -0.0033(7) C5 0.0263(8) 0.0173(8) 0.0507(11) -0.0066(7) 0.0055(8) -0.0033(6) C6 0.0283(9) 0.0239(8) 0.0518(11) 0.0051(7) 0.0165(8) -0.0050(7) C7 0.0292(8) 0.0187(7) 0.0360(9) 0.0064(6) 0.0099(7) 0.0020(6) C8 0.0266(8) 0.0206(8) 0.0320(8) 0.0064(6) 0.0030(7) 0.0026(6) C9 0.0377(10) 0.0411(10) 0.0284(9) 0.0047(7) 0.0137(8) 0.0025(8) C10 0.0198(8) 0.0267(8) 0.0416(10) -0.0100(7) 0.0032(7) -0.0024(6) C11 0.0471(11) 0.0298(9) 0.0319(9) 0.0076(7) 0.0217(8) 0.0042(8) C12 0.0280(8) 0.0309(9) 0.0283(8) -0.0017(7) 0.0044(7) -0.0014(7) C13 0.0164(7) 0.0296(8) 0.0431(10) 0.0015(7) 0.0085(7) -0.0004(6) C14 0.0557(13) 0.0292(10) 0.0427(11) 0.0100(8) 0.0155(9) -0.0004(9) C15 0.0325(10) 0.0205(8) 0.0648(14) -0.0071(8) -0.0014(9) -0.0038(7) C16 0.0354(9) 0.0261(9) 0.0401(10) 0.0052(7) 0.0130(8) -0.0011(7) C17 0.0222(8) 0.0302(9) 0.0334(9) 0.0010(7) -0.0003(7) 0.0004(6) C18 0.0282(8) 0.0293(9) 0.0311(8) -0.0021(7) 0.0127(7) -0.0031(7) C19 0.0305(8) 0.0244(8) 0.0321(8) -0.0058(6) 0.0106(7) 0.0023(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N5 1.6668(13) . ? Si1 N1 1.7921(14) . ? Si1 C12 1.8786(18) . ? Si1 C13 1.8804(16) . ? Si1 Ca1 3.1691(6) . ? Si2 N5 1.6827(13) . ? Si2 C14 1.873(2) . ? Si2 C15 1.8813(19) . ? Si3 N6 1.6789(14) . ? Si3 C16 1.8753(18) . ? Si3 C17 1.8772(17) . ? Si3 Ca1 3.6358(6) . ? Si4 N6 1.6778(13) . ? Si4 C19 1.8743(17) . ? Si4 C18 1.8781(17) . ? Si4 Ca1 3.2126(5) . ? N1 C1 1.474(2) . ? N1 C8 1.476(2) . ? N1 Ca1 2.6850(13) . ? N2 C3 1.467(2) . ? N2 C9 1.475(2) . ? N2 C2 1.486(2) . ? N2 Ca1 2.5247(13) . ? N3 C5 1.472(2) . ? N3 C4 1.481(2) . ? N3 C10 1.478(2) . ? N3 Ca1 2.7139(14) . ? N4 C11 1.470(2) . ? N4 C7 1.474(2) . ? N4 C6 1.483(2) . ? N4 Ca1 2.6396(14) . ? N5 Ca1 2.3970(13) . ? N6 Ca1 2.3416(13) . ? C1 C2 1.515(2) . ? C3 C4 1.516(3) . ? C5 C6 1.503(3) . ? C7 C8 1.518(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Si1 N1 104.14(6) . . ? N5 Si1 C12 114.51(8) . . ? N1 Si1 C12 107.49(7) . . ? N5 Si1 C13 116.88(8) . . ? N1 Si1 C13 108.73(7) . . ? C12 Si1 C13 104.73(8) . . ? N5 Si1 Ca1 47.95(4) . . ? N1 Si1 Ca1 57.84(4) . . ? C12 Si1 Ca1 114.87(6) . . ? C13 Si1 Ca1 140.33(6) . . ? N5 Si2 C14 112.36(8) . . ? N5 Si2 C15 115.58(8) . . ? C14 Si2 C15 105.45(10) . . ? N6 Si3 C16 115.40(8) . . ? N6 Si3 C17 114.76(7) . . ? C16 Si3 C17 104.83(8) . . ? N6 Si3 Ca1 30.17(4) . . ? C16 Si3 Ca1 118.89(6) . . ? C17 Si3 Ca1 132.60(6) . . ? N6 Si4 C19 116.84(7) . . ? N6 Si4 C18 114.73(7) . . ? C19 Si4 C18 106.20(8) . . ? N6 Si4 Ca1 44.78(4) . . ? C19 Si4 Ca1 136.97(6) . . ? C18 Si4 Ca1 116.82(6) . . ? C1 N1 C8 111.04(13) . . ? C1 N1 Si1 117.36(10) . . ? C8 N1 Si1 119.45(11) . . ? C1 N1 Ca1 107.01(9) . . ? C8 N1 Ca1 110.92(9) . . ? Si1 N1 Ca1 87.75(5) . . ? C3 N2 C9 110.63(14) . . ? C3 N2 C2 110.82(13) . . ? C9 N2 C2 108.14(13) . . ? C3 N2 Ca1 112.69(10) . . ? C9 N2 Ca1 106.46(10) . . ? C2 N2 Ca1 107.88(9) . . ? C5 N3 C4 110.82(14) . . ? C5 N3 C10 108.61(14) . . ? C4 N3 C10 107.97(14) . . ? C5 N3 Ca1 108.78(10) . . ? C4 N3 Ca1 107.24(10) . . ? C10 N3 Ca1 113.43(9) . . ? C11 N4 C7 110.13(14) . . ? C11 N4 C6 108.29(14) . . ? C7 N4 C6 109.38(13) . . ? C11 N4 Ca1 110.51(10) . . ? C7 N4 Ca1 110.10(9) . . ? C6 N4 Ca1 108.38(10) . . ? Si1 N5 Si2 129.32(8) . . ? Si1 N5 Ca1 100.96(6) . . ? Si2 N5 Ca1 129.09(7) . . ? Si4 N6 Si3 126.38(8) . . ? Si4 N6 Ca1 104.92(6) . . ? Si3 N6 Ca1 128.71(7) . . ? N6 Ca1 N5 101.97(5) . . ? N6 Ca1 N2 119.77(5) . . ? N5 Ca1 N2 91.97(5) . . ? N6 Ca1 N4 115.31(4) . . ? N5 Ca1 N4 119.29(5) . . ? N2 Ca1 N4 106.92(5) . . ? N6 Ca1 N1 164.03(4) . . ? N5 Ca1 N1 64.68(4) . . ? N2 Ca1 N1 71.34(4) . . ? N4 Ca1 N1 68.12(4) . . ? N6 Ca1 N3 87.94(4) . . ? N5 Ca1 N3 161.31(5) . . ? N2 Ca1 N3 69.34(4) . . ? N4 Ca1 N3 68.67(5) . . ? N1 Ca1 N3 107.39(4) . . ? N6 Ca1 Si1 130.74(3) . . ? N5 Ca1 Si1 31.09(3) . . ? N2 Ca1 Si1 85.98(3) . . ? N4 Ca1 Si1 92.08(3) . . ? N1 Ca1 Si1 34.41(3) . . ? N3 Ca1 Si1 141.25(3) . . ? N6 Ca1 Si4 30.31(3) . . ? N5 Ca1 Si4 96.02(3) . . ? N2 Ca1 Si4 150.08(3) . . ? N4 Ca1 Si4 94.15(3) . . ? N1 Ca1 Si4 137.71(3) . . ? N3 Ca1 Si4 100.32(3) . . ? Si1 Ca1 Si4 114.833(16) . . ? N6 Ca1 Si3 21.12(3) . . ? N5 Ca1 Si3 104.20(3) . . ? N2 Ca1 Si3 98.65(4) . . ? N4 Ca1 Si3 127.69(3) . . ? N1 Ca1 Si3 163.96(3) . . ? N3 Ca1 Si3 79.48(3) . . ? Si1 Ca1 Si3 135.269(14) . . ? Si4 Ca1 Si3 51.430(15) . . ? N1 C1 C2 113.69(13) . . ? N2 C2 C1 114.04(13) . . ? N2 C3 C4 112.83(14) . . ? N3 C4 C3 112.79(15) . . ? N3 C5 C6 112.29(14) . . ? N4 C6 C5 113.45(14) . . ? N4 C7 C8 112.87(13) . . ? N1 C8 C7 112.44(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Si1 N1 C1 -94.98(12) . . . . ? C12 Si1 N1 C1 143.16(12) . . . . ? C13 Si1 N1 C1 30.31(13) . . . . ? Ca1 Si1 N1 C1 -108.01(12) . . . . ? N5 Si1 N1 C8 125.88(12) . . . . ? C12 Si1 N1 C8 4.02(13) . . . . ? C13 Si1 N1 C8 -108.83(12) . . . . ? Ca1 Si1 N1 C8 112.84(12) . . . . ? N5 Si1 N1 Ca1 13.03(6) . . . . ? C12 Si1 N1 Ca1 -108.83(7) . . . . ? C13 Si1 N1 Ca1 138.32(7) . . . . ? N1 Si1 N5 Si2 173.63(10) . . . . ? C12 Si1 N5 Si2 -69.27(13) . . . . ? C13 Si1 N5 Si2 53.70(13) . . . . ? Ca1 Si1 N5 Si2 -171.47(14) . . . . ? N1 Si1 N5 Ca1 -14.90(7) . . . . ? C12 Si1 N5 Ca1 102.20(8) . . . . ? C13 Si1 N5 Ca1 -134.83(7) . . . . ? C14 Si2 N5 Si1 -116.58(12) . . . . ? C15 Si2 N5 Si1 4.50(15) . . . . ? C14 Si2 N5 Ca1 74.24(12) . . . . ? C15 Si2 N5 Ca1 -164.68(10) . . . . ? C19 Si4 N6 Si3 49.05(12) . . . . ? C18 Si4 N6 Si3 -76.22(12) . . . . ? Ca1 Si4 N6 Si3 179.83(13) . . . . ? C19 Si4 N6 Ca1 -130.78(7) . . . . ? C18 Si4 N6 Ca1 103.95(8) . . . . ? C16 Si3 N6 Si4 -75.47(12) . . . . ? C17 Si3 N6 Si4 46.60(12) . . . . ? Ca1 Si3 N6 Si4 -179.79(16) . . . . ? C16 Si3 N6 Ca1 104.32(10) . . . . ? C17 Si3 N6 Ca1 -133.60(9) . . . . ? Si4 N6 Ca1 N5 81.36(7) . . . . ? Si3 N6 Ca1 N5 -98.46(9) . . . . ? Si4 N6 Ca1 N2 -179.32(5) . . . . ? Si3 N6 Ca1 N2 0.85(11) . . . . ? Si4 N6 Ca1 N4 -49.43(7) . . . . ? Si3 N6 Ca1 N4 130.74(8) . . . . ? Si4 N6 Ca1 N1 49.43(19) . . . . ? Si3 N6 Ca1 N1 -130.40(14) . . . . ? Si4 N6 Ca1 N3 -114.63(7) . . . . ? Si3 N6 Ca1 N3 65.55(9) . . . . ? Si4 N6 Ca1 Si1 67.97(7) . . . . ? Si3 N6 Ca1 Si1 -111.86(8) . . . . ? Si3 N6 Ca1 Si4 -179.83(14) . . . . ? Si4 N6 Ca1 Si3 179.83(14) . . . . ? Si1 N5 Ca1 N6 -160.13(6) . . . . ? Si2 N5 Ca1 N6 11.37(10) . . . . ? Si1 N5 Ca1 N2 78.86(7) . . . . ? Si2 N5 Ca1 N2 -109.64(9) . . . . ? Si1 N5 Ca1 N4 -31.82(8) . . . . ? Si2 N5 Ca1 N4 139.68(8) . . . . ? Si1 N5 Ca1 N1 10.61(5) . . . . ? Si2 N5 Ca1 N1 -177.90(11) . . . . ? Si1 N5 Ca1 N3 79.09(15) . . . . ? Si2 N5 Ca1 N3 -109.41(14) . . . . ? Si2 N5 Ca1 Si1 171.50(14) . . . . ? Si1 N5 Ca1 Si4 -130.01(5) . . . . ? Si2 N5 Ca1 Si4 41.48(9) . . . . ? Si1 N5 Ca1 Si3 178.30(5) . . . . ? Si2 N5 Ca1 Si3 -10.20(10) . . . . ? C3 N2 Ca1 N6 91.14(12) . . . . ? C9 N2 Ca1 N6 -30.31(12) . . . . ? C2 N2 Ca1 N6 -146.19(10) . . . . ? C3 N2 Ca1 N5 -163.87(12) . . . . ? C9 N2 Ca1 N5 74.68(11) . . . . ? C2 N2 Ca1 N5 -41.20(10) . . . . ? C3 N2 Ca1 N4 -42.39(12) . . . . ? C9 N2 Ca1 N4 -163.85(11) . . . . ? C2 N2 Ca1 N4 80.28(11) . . . . ? C3 N2 Ca1 N1 -101.47(12) . . . . ? C9 N2 Ca1 N1 137.08(11) . . . . ? C2 N2 Ca1 N1 21.20(10) . . . . ? C3 N2 Ca1 N3 16.21(11) . . . . ? C9 N2 Ca1 N3 -105.24(11) . . . . ? C2 N2 Ca1 N3 138.88(11) . . . . ? C3 N2 Ca1 Si1 -133.34(11) . . . . ? C9 N2 Ca1 Si1 105.20(11) . . . . ? C2 N2 Ca1 Si1 -10.67(10) . . . . ? C3 N2 Ca1 Si4 90.46(13) . . . . ? C9 N2 Ca1 Si4 -31.00(14) . . . . ? C2 N2 Ca1 Si4 -146.87(9) . . . . ? C3 N2 Ca1 Si3 91.45(11) . . . . ? C9 N2 Ca1 Si3 -30.00(11) . . . . ? C2 N2 Ca1 Si3 -145.88(10) . . . . ? C11 N4 Ca1 N6 59.84(12) . . . . ? C7 N4 Ca1 N6 -178.28(10) . . . . ? C6 N4 Ca1 N6 -58.68(11) . . . . ? C11 N4 Ca1 N5 -62.04(12) . . . . ? C7 N4 Ca1 N5 59.84(12) . . . . ? C6 N4 Ca1 N5 179.44(10) . . . . ? C11 N4 Ca1 N2 -164.28(11) . . . . ? C7 N4 Ca1 N2 -42.39(11) . . . . ? C6 N4 Ca1 N2 77.21(11) . . . . ? C11 N4 Ca1 N1 -103.13(12) . . . . ? C7 N4 Ca1 N1 18.76(10) . . . . ? C6 N4 Ca1 N1 138.36(11) . . . . ? C11 N4 Ca1 N3 136.70(12) . . . . ? C7 N4 Ca1 N3 -101.42(11) . . . . ? C6 N4 Ca1 N3 18.19(10) . . . . ? C11 N4 Ca1 Si1 -77.85(11) . . . . ? C7 N4 Ca1 Si1 44.03(10) . . . . ? C6 N4 Ca1 Si1 163.63(10) . . . . ? C11 N4 Ca1 Si4 37.24(11) . . . . ? C7 N4 Ca1 Si4 159.12(10) . . . . ? C6 N4 Ca1 Si4 -81.28(10) . . . . ? C11 N4 Ca1 Si3 80.02(12) . . . . ? C7 N4 Ca1 Si3 -158.09(9) . . . . ? C6 N4 Ca1 Si3 -38.49(12) . . . . ? C1 N1 Ca1 N6 143.20(15) . . . . ? C8 N1 Ca1 N6 -95.55(18) . . . . ? Si1 N1 Ca1 N6 25.24(18) . . . . ? C1 N1 Ca1 N5 108.28(10) . . . . ? C8 N1 Ca1 N5 -130.47(11) . . . . ? Si1 N1 Ca1 N5 -9.69(5) . . . . ? C1 N1 Ca1 N2 6.74(9) . . . . ? C8 N1 Ca1 N2 127.99(11) . . . . ? Si1 N1 Ca1 N2 -111.22(6) . . . . ? C1 N1 Ca1 N4 -111.08(10) . . . . ? C8 N1 Ca1 N4 10.18(10) . . . . ? Si1 N1 Ca1 N4 130.96(6) . . . . ? C1 N1 Ca1 N3 -53.52(10) . . . . ? C8 N1 Ca1 N3 67.74(11) . . . . ? Si1 N1 Ca1 N3 -171.48(5) . . . . ? C1 N1 Ca1 Si1 117.96(11) . . . . ? C8 N1 Ca1 Si1 -120.78(12) . . . . ? C1 N1 Ca1 Si4 177.93(8) . . . . ? C8 N1 Ca1 Si4 -60.82(11) . . . . ? Si1 N1 Ca1 Si4 59.96(6) . . . . ? C1 N1 Ca1 Si3 59.87(16) . . . . ? C8 N1 Ca1 Si3 -178.88(9) . . . . ? Si1 N1 Ca1 Si3 -58.09(13) . . . . ? C5 N3 Ca1 N6 129.74(11) . . . . ? C4 N3 Ca1 N6 -110.34(11) . . . . ? C10 N3 Ca1 N6 8.77(12) . . . . ? C5 N3 Ca1 N5 -107.50(16) . . . . ? C4 N3 Ca1 N5 12.4(2) . . . . ? C10 N3 Ca1 N5 131.52(15) . . . . ? C5 N3 Ca1 N2 -107.26(11) . . . . ? C4 N3 Ca1 N2 12.65(11) . . . . ? C10 N3 Ca1 N2 131.77(13) . . . . ? C5 N3 Ca1 N4 11.50(10) . . . . ? C4 N3 Ca1 N4 131.41(12) . . . . ? C10 N3 Ca1 N4 -109.47(12) . . . . ? C5 N3 Ca1 N1 -45.71(11) . . . . ? C4 N3 Ca1 N1 74.20(11) . . . . ? C10 N3 Ca1 N1 -166.69(11) . . . . ? C5 N3 Ca1 Si1 -53.40(13) . . . . ? C4 N3 Ca1 Si1 66.51(13) . . . . ? C10 N3 Ca1 Si1 -174.37(9) . . . . ? C5 N3 Ca1 Si4 101.95(10) . . . . ? C4 N3 Ca1 Si4 -138.14(10) . . . . ? C10 N3 Ca1 Si4 -19.02(12) . . . . ? C5 N3 Ca1 Si3 149.23(11) . . . . ? C4 N3 Ca1 Si3 -90.85(11) . . . . ? C10 N3 Ca1 Si3 28.26(11) . . . . ? N5 Si1 Ca1 N6 26.03(8) . . . . ? N1 Si1 Ca1 N6 -171.09(7) . . . . ? C12 Si1 Ca1 N6 -75.36(8) . . . . ? C13 Si1 Ca1 N6 108.34(10) . . . . ? N1 Si1 Ca1 N5 162.87(8) . . . . ? C12 Si1 Ca1 N5 -101.39(9) . . . . ? C13 Si1 Ca1 N5 82.31(11) . . . . ? N5 Si1 Ca1 N2 -100.58(7) . . . . ? N1 Si1 Ca1 N2 62.30(6) . . . . ? C12 Si1 Ca1 N2 158.03(7) . . . . ? C13 Si1 Ca1 N2 -18.27(10) . . . . ? N5 Si1 Ca1 N4 152.60(7) . . . . ? N1 Si1 Ca1 N4 -44.52(6) . . . . ? C12 Si1 Ca1 N4 51.21(7) . . . . ? C13 Si1 Ca1 N4 -125.09(10) . . . . ? N5 Si1 Ca1 N1 -162.87(8) . . . . ? C12 Si1 Ca1 N1 95.74(8) . . . . ? C13 Si1 Ca1 N1 -80.56(10) . . . . ? N5 Si1 Ca1 N3 -149.82(8) . . . . ? N1 Si1 Ca1 N3 13.05(8) . . . . ? C12 Si1 Ca1 N3 108.79(8) . . . . ? C13 Si1 Ca1 N3 -67.51(11) . . . . ? N5 Si1 Ca1 Si4 57.06(7) . . . . ? N1 Si1 Ca1 Si4 -140.07(5) . . . . ? C12 Si1 Ca1 Si4 -44.33(7) . . . . ? C13 Si1 Ca1 Si4 139.37(9) . . . . ? N5 Si1 Ca1 Si3 -2.34(7) . . . . ? N1 Si1 Ca1 Si3 160.53(5) . . . . ? C12 Si1 Ca1 Si3 -103.73(7) . . . . ? C13 Si1 Ca1 Si3 79.97(9) . . . . ? C19 Si4 Ca1 N6 81.94(11) . . . . ? C18 Si4 Ca1 N6 -98.97(9) . . . . ? N6 Si4 Ca1 N5 -103.46(7) . . . . ? C19 Si4 Ca1 N5 -21.51(9) . . . . ? C18 Si4 Ca1 N5 157.57(7) . . . . ? N6 Si4 Ca1 N2 1.18(9) . . . . ? C19 Si4 Ca1 N2 83.12(11) . . . . ? C18 Si4 Ca1 N2 -97.80(9) . . . . ? N6 Si4 Ca1 N4 136.49(7) . . . . ? C19 Si4 Ca1 N4 -141.57(9) . . . . ? C18 Si4 Ca1 N4 37.51(7) . . . . ? N6 Si4 Ca1 N1 -161.91(8) . . . . ? C19 Si4 Ca1 N1 -79.96(10) . . . . ? C18 Si4 Ca1 N1 99.12(8) . . . . ? N6 Si4 Ca1 N3 67.43(7) . . . . ? C19 Si4 Ca1 N3 149.37(9) . . . . ? C18 Si4 Ca1 N3 -31.54(7) . . . . ? N6 Si4 Ca1 Si1 -129.29(6) . . . . ? C19 Si4 Ca1 Si1 -47.35(9) . . . . ? C18 Si4 Ca1 Si1 131.74(6) . . . . ? N6 Si4 Ca1 Si3 -0.08(6) . . . . ? C19 Si4 Ca1 Si3 81.86(9) . . . . ? C18 Si4 Ca1 Si3 -99.05(7) . . . . ? C16 Si3 Ca1 N6 -91.47(11) . . . . ? C17 Si3 Ca1 N6 63.29(12) . . . . ? N6 Si3 Ca1 N5 86.48(9) . . . . ? C16 Si3 Ca1 N5 -4.99(8) . . . . ? C17 Si3 Ca1 N5 149.76(9) . . . . ? N6 Si3 Ca1 N2 -179.25(10) . . . . ? C16 Si3 Ca1 N2 89.28(8) . . . . ? C17 Si3 Ca1 N2 -115.97(9) . . . . ? N6 Si3 Ca1 N4 -59.95(10) . . . . ? C16 Si3 Ca1 N4 -151.41(8) . . . . ? C17 Si3 Ca1 N4 3.34(9) . . . . ? N6 Si3 Ca1 N1 130.69(14) . . . . ? C16 Si3 Ca1 N1 39.22(13) . . . . ? C17 Si3 Ca1 N1 -166.02(13) . . . . ? N6 Si3 Ca1 N3 -112.29(9) . . . . ? C16 Si3 Ca1 N3 156.24(8) . . . . ? C17 Si3 Ca1 N3 -49.00(9) . . . . ? N6 Si3 Ca1 Si1 87.72(9) . . . . ? C16 Si3 Ca1 Si1 -3.74(7) . . . . ? C17 Si3 Ca1 Si1 151.01(8) . . . . ? N6 Si3 Ca1 Si4 0.11(9) . . . . ? C16 Si3 Ca1 Si4 -91.36(7) . . . . ? C17 Si3 Ca1 Si4 63.40(8) . . . . ? C8 N1 C1 C2 -155.87(14) . . . . ? Si1 N1 C1 C2 61.74(16) . . . . ? Ca1 N1 C1 C2 -34.69(15) . . . . ? C3 N2 C2 C1 73.83(17) . . . . ? C9 N2 C2 C1 -164.76(14) . . . . ? Ca1 N2 C2 C1 -49.98(15) . . . . ? N1 C1 C2 N2 60.93(19) . . . . ? C9 N2 C3 C4 74.23(19) . . . . ? C2 N2 C3 C4 -165.84(15) . . . . ? Ca1 N2 C3 C4 -44.83(18) . . . . ? C5 N3 C4 C3 78.42(18) . . . . ? C10 N3 C4 C3 -162.75(15) . . . . ? Ca1 N3 C4 C3 -40.18(17) . . . . ? N2 C3 C4 N3 59.8(2) . . . . ? C4 N3 C5 C6 -158.55(14) . . . . ? C10 N3 C5 C6 83.00(17) . . . . ? Ca1 N3 C5 C6 -40.89(16) . . . . ? C11 N4 C6 C5 -168.59(15) . . . . ? C7 N4 C6 C5 71.38(18) . . . . ? Ca1 N4 C6 C5 -48.68(16) . . . . ? N3 C5 C6 N4 64.11(19) . . . . ? C11 N4 C7 C8 74.91(18) . . . . ? C6 N4 C7 C8 -166.20(14) . . . . ? Ca1 N4 C7 C8 -47.20(16) . . . . ? C1 N1 C8 C7 80.65(17) . . . . ? Si1 N1 C8 C7 -137.85(12) . . . . ? Ca1 N1 C8 C7 -38.20(16) . . . . ? N4 C7 C8 N1 59.87(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 29.63 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.594 _refine_diff_density_min -0.231 _refine_diff_density_rms 0.070 #==END