data_publication_text _publ_requested_journal Inorg.Chem. _publ_section_title ; 'Five-Coordinate Silicon(II) Compounds with Si-M Bonds (M = Cr, Mo, W, Fe): Bis[N,N'-diisopropylbenzamidinato(-)]silicon(II) as a Ligand in Transition-Metal Complexes' ; _publ_contact_author_name 'Reinhold Tacke, Sebastian Riedel' _publ_contact_author_address ;Institut fuer Anorganische Chemie Julius-Maximilians-Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg Germany, Institut fuer Anorganische und Analytische Chemie Universitaet Freiburg Albertstrasse 21 D-79104 Freiburg i. Br. Germany ; _publ_contact_author_email r.tacke@uni-wuerzburg.de _publ_contact_author_phone '049 931 3185251' _publ_contact_author_fax '049 931 3184609' loop_ _publ_author_name _publ_author_address 'Junold, Konstantin' ;Institut fuer Anorganische Chemie Julius-Maximilians-Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg Germany ; 'Baus, Johannes A.' ;Institut fuer Anorganische Chemie Julius-Maximilians-Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg Germany ; 'Burschka, Christian' ;Institut fuer Anorganische Chemie Julius-Maximilians-Universitaet Wuerzburg Am Hubland D-97074 Wuerzburg Germany ; 'Vent-Schmidt, Thomas' ;Institut fuer Anorganische und Analytische Chemie Universitaet Freiburg Albertstrasse 21 D-79104 Freiburg i. Br. Germany ; 'Riedel, Sebastian' ;Institut fuer Anorganische und Analytische Chemie Universitaet Freiburg Albertstrasse 21 D-79104 Freiburg i. Br. Germany ; 'Tacke, Reinhold' ;Institut fuer Anorganische Chemie Julius-Maximilians-Universtitaet Wuerzburg Am Hubland D-97074 Wuerzburg Germany ; # ******************* Data Compound 2 ************************* data_jun84b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H38 Cr N4 O5 Si' _chemical_formula_sum 'C31 H38 Cr N4 O5 Si' _chemical_formula_weight 626.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.774(2) _cell_length_b 19.500(3) _cell_length_c 16.413(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.17(2) _cell_angle_gamma 90.00 _cell_volume 3294.5(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 29.15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.426 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate-STOE-IPDS _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35568 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 26.03 _reflns_number_total 6369 _reflns_number_gt 4882 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP/POV-Ray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0909P)^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 6369 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1253 _refine_ls_wR_factor_gt 0.1181 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Cr Cr 0.77658(3) 0.173522(16) 0.111120(19) 0.02224(12) Uani 1 1 d . . . Si Si 0.82087(5) 0.09242(3) 0.22764(3) 0.02157(14) Uani 1 1 d . . . O1 O 0.5849(2) 0.07654(11) -0.00597(12) 0.0560(5) Uani 1 1 d . . . O2 O 0.99218(18) 0.10059(10) 0.06154(10) 0.0458(4) Uani 1 1 d . . . N1 N 0.82736(16) 0.11688(8) 0.33445(10) 0.0217(3) Uani 1 1 d . . . N2 N 0.64116(16) 0.07633(9) 0.25759(10) 0.0234(4) Uani 1 1 d . . . N3 N 0.84237(16) 0.00220(8) 0.21245(10) 0.0218(3) Uani 1 1 d . . . O3 O 0.95946(17) 0.27617(9) 0.22429(13) 0.0477(5) Uani 1 1 d . . . N4 N 1.01565(15) 0.06420(8) 0.25815(9) 0.0204(3) Uani 1 1 d . . . O4 O 0.56914(18) 0.23437(9) 0.18017(12) 0.0464(4) Uani 1 1 d . . . C1 C 0.70113(19) 0.10578(10) 0.33004(12) 0.0217(4) Uani 1 1 d . . . C2 C 0.64024(19) 0.12610(11) 0.39703(12) 0.0247(4) Uani 1 1 d . . . C3 C 0.5776(2) 0.18890(12) 0.39236(14) 0.0324(5) Uani 1 1 d . . . H3 H 0.5728 0.2190 0.3460 0.039 Uiso 1 1 calc R . . C4 C 0.5222(2) 0.20778(15) 0.45541(16) 0.0440(6) Uani 1 1 d . . . H4 H 0.4795 0.2508 0.4522 0.053 Uiso 1 1 calc R . . C5 C 0.5292(3) 0.16406(16) 0.52273(16) 0.0496(7) Uani 1 1 d . . . H5 H 0.4922 0.1773 0.5662 0.060 Uiso 1 1 calc R . . O5 O 0.72194(18) 0.27176(10) -0.03598(12) 0.0512(5) Uani 1 1 d . . . C6 C 0.5895(3) 0.10125(16) 0.52728(15) 0.0460(7) Uani 1 1 d . . . H6 H 0.5934 0.0712 0.5735 0.055 Uiso 1 1 calc R . . C7 C 0.6443(2) 0.08203(13) 0.46435(14) 0.0342(5) Uani 1 1 d . . . H7 H 0.6848 0.0385 0.4672 0.041 Uiso 1 1 calc R . . C8 C 0.9287(2) 0.15052(11) 0.40246(12) 0.0277(5) Uani 1 1 d . . . H8 H 1.0051 0.1562 0.3802 0.033 Uiso 1 1 calc R . . C9 C 0.8915(3) 0.22247(15) 0.4236(2) 0.0601(9) Uani 1 1 d . . . H9A H 0.8518 0.2477 0.3707 0.090 Uiso 1 1 calc R . . H9B H 0.9694 0.2468 0.4572 0.090 Uiso 1 1 calc R . . H9C H 0.8292 0.2191 0.4566 0.090 Uiso 1 1 calc R . . C31 C 0.7436(2) 0.23465(12) 0.02080(14) 0.0321(5) Uani 1 1 d . . . C30 C 0.6468(2) 0.21053(11) 0.15349(13) 0.0296(5) Uani 1 1 d . . . C10 C 0.9742(3) 0.1059(2) 0.48097(17) 0.0621(9) Uani 1 1 d . . . H10A H 0.9924 0.0596 0.4643 0.093 Uiso 1 1 calc R . . H10B H 0.9063 0.1037 0.5096 0.093 Uiso 1 1 calc R . . H10C H 1.0534 0.1255 0.5200 0.093 Uiso 1 1 calc R . . C11 C 0.5018(2) 0.05867(12) 0.23738(13) 0.0302(5) Uani 1 1 d . . . H11 H 0.4615 0.0909 0.2697 0.036 Uiso 1 1 calc R . . C12 C 0.4319(2) 0.06769(14) 0.14299(14) 0.0407(6) Uani 1 1 d . . . H12A H 0.4709 0.0374 0.1097 0.061 Uiso 1 1 calc R . . H12B H 0.4398 0.1154 0.1266 0.061 Uiso 1 1 calc R . . H12C H 0.3399 0.0561 0.1318 0.061 Uiso 1 1 calc R . . C13 C 0.4844(2) -0.01353(13) 0.26611(17) 0.0413(6) Uani 1 1 d . . . H13A H 0.3918 -0.0225 0.2571 0.062 Uiso 1 1 calc R . . H13B H 0.5314 -0.0185 0.3268 0.062 Uiso 1 1 calc R . . H13C H 0.5187 -0.0464 0.2330 0.062 Uiso 1 1 calc R . . C14 C 0.97273(18) 0.00283(9) 0.23074(11) 0.0195(4) Uani 1 1 d . . . C15 C 1.05605(19) -0.05618(10) 0.22196(12) 0.0232(4) Uani 1 1 d . . . C16 C 1.1068(2) -0.05973(11) 0.15330(13) 0.0289(5) Uani 1 1 d . . . H16 H 1.0860 -0.0251 0.1107 0.035 Uiso 1 1 calc R . . C17 C 1.1872(2) -0.11340(12) 0.14688(16) 0.0383(6) Uani 1 1 d . . . H17 H 1.2217 -0.1156 0.0999 0.046 Uiso 1 1 calc R . . C18 C 1.2173(2) -0.16365(12) 0.20833(18) 0.0424(6) Uani 1 1 d . . . H18 H 1.2729 -0.2004 0.2039 0.051 Uiso 1 1 calc R . . C19 C 1.1672(3) -0.16089(12) 0.27648(17) 0.0431(6) Uani 1 1 d . . . H19 H 1.1879 -0.1958 0.3187 0.052 Uiso 1 1 calc R . . C20 C 1.0864(2) -0.10714(11) 0.28358(15) 0.0349(5) Uani 1 1 d . . . H20 H 1.0520 -0.1053 0.3306 0.042 Uiso 1 1 calc R . . C21 C 0.7507(2) -0.05175(10) 0.17065(14) 0.0303(5) Uani 1 1 d . . . H21 H 0.6621 -0.0308 0.1564 0.036 Uiso 1 1 calc R . . C22 C 0.7690(3) -0.07571(16) 0.08580(18) 0.0534(8) Uani 1 1 d . . . H22A H 0.6940 -0.1033 0.0547 0.080 Uiso 1 1 calc R . . H22B H 0.8482 -0.1034 0.0971 0.080 Uiso 1 1 calc R . . H22C H 0.7765 -0.0357 0.0515 0.080 Uiso 1 1 calc R . . C23 C 0.7503(3) -0.11119(14) 0.2299(2) 0.0575(8) Uani 1 1 d . . . H23A H 0.6736 -0.1398 0.2053 0.086 Uiso 1 1 calc R . . H23B H 0.7480 -0.0936 0.2853 0.086 Uiso 1 1 calc R . . H23C H 0.8290 -0.1387 0.2374 0.086 Uiso 1 1 calc R . . C24 C 1.15577(19) 0.08051(10) 0.28166(13) 0.0259(4) Uani 1 1 d . . . H24 H 1.1947 0.0525 0.2444 0.031 Uiso 1 1 calc R . . C25 C 1.1781(2) 0.15523(11) 0.26567(15) 0.0336(5) Uani 1 1 d . . . H25A H 1.1389 0.1657 0.2051 0.050 Uiso 1 1 calc R . . H25B H 1.2716 0.1644 0.2815 0.050 Uiso 1 1 calc R . . H25C H 1.1383 0.1840 0.3000 0.050 Uiso 1 1 calc R . . C26 C 1.2240(2) 0.06103(12) 0.37374(14) 0.0356(5) Uani 1 1 d . . . H26A H 1.2071 0.0127 0.3828 0.053 Uiso 1 1 calc R . . H26B H 1.1912 0.0897 0.4119 0.053 Uiso 1 1 calc R . . H26C H 1.3178 0.0682 0.3859 0.053 Uiso 1 1 calc R . . C27 C 0.6574(2) 0.11234(12) 0.04077(14) 0.0336(5) Uani 1 1 d . . . C28 C 0.9117(2) 0.12885(11) 0.08064(12) 0.0294(5) Uani 1 1 d . . . C29 C 0.8923(2) 0.23567(11) 0.18238(14) 0.0296(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr 0.02268(19) 0.02318(18) 0.02194(18) 0.00415(12) 0.00829(13) 0.00230(12) Si 0.0284(3) 0.0182(3) 0.0189(3) -0.00021(18) 0.0083(2) 0.0015(2) O1 0.0530(12) 0.0691(13) 0.0486(10) -0.0241(10) 0.0190(9) -0.0241(10) O2 0.0433(10) 0.0640(12) 0.0344(9) 0.0023(8) 0.0181(8) 0.0211(9) N1 0.0191(8) 0.0250(8) 0.0218(8) -0.0018(6) 0.0071(7) -0.0008(6) N2 0.0216(8) 0.0282(9) 0.0228(8) -0.0017(7) 0.0103(7) -0.0018(7) N3 0.0193(8) 0.0203(8) 0.0264(8) -0.0012(6) 0.0078(7) -0.0004(6) O3 0.0364(9) 0.0362(9) 0.0664(12) -0.0148(8) 0.0088(9) -0.0024(8) N4 0.0183(8) 0.0218(8) 0.0215(8) -0.0011(6) 0.0065(6) 0.0013(6) O4 0.0430(10) 0.0420(10) 0.0640(11) -0.0035(8) 0.0313(9) 0.0081(8) C1 0.0211(10) 0.0239(9) 0.0217(9) 0.0025(7) 0.0088(8) 0.0034(8) C2 0.0185(10) 0.0369(11) 0.0200(9) -0.0034(8) 0.0074(8) 0.0005(8) C3 0.0285(11) 0.0374(12) 0.0331(11) -0.0017(9) 0.0120(9) 0.0055(9) C4 0.0338(13) 0.0558(16) 0.0453(14) -0.0131(12) 0.0160(11) 0.0116(11) C5 0.0349(14) 0.089(2) 0.0310(12) -0.0087(12) 0.0185(11) 0.0141(14) O5 0.0376(10) 0.0649(12) 0.0529(10) 0.0398(9) 0.0161(8) 0.0131(9) C6 0.0378(14) 0.0772(19) 0.0278(11) 0.0084(11) 0.0172(11) 0.0092(13) C7 0.0296(12) 0.0459(13) 0.0302(11) 0.0077(9) 0.0137(10) 0.0071(10) C8 0.0213(10) 0.0377(11) 0.0237(10) -0.0083(8) 0.0060(8) -0.0023(9) C9 0.0340(14) 0.0566(17) 0.093(2) -0.0460(16) 0.0229(15) -0.0121(12) C31 0.0206(10) 0.0391(12) 0.0379(12) 0.0073(10) 0.0107(9) 0.0054(9) C30 0.0301(11) 0.0260(10) 0.0326(11) 0.0019(8) 0.0093(10) -0.0011(9) C10 0.0359(15) 0.110(3) 0.0335(13) 0.0218(15) 0.0000(12) -0.0109(16) C11 0.0208(10) 0.0398(12) 0.0311(11) -0.0054(9) 0.0094(9) -0.0050(9) C12 0.0292(12) 0.0559(15) 0.0329(12) -0.0026(11) 0.0028(10) -0.0100(11) C13 0.0315(12) 0.0488(14) 0.0469(13) 0.0021(11) 0.0167(11) -0.0110(11) C14 0.0202(9) 0.0217(9) 0.0167(8) 0.0015(7) 0.0055(7) 0.0025(7) C15 0.0214(10) 0.0214(9) 0.0254(9) -0.0026(7) 0.0045(8) 0.0021(7) C16 0.0290(11) 0.0299(11) 0.0283(10) -0.0031(8) 0.0092(9) 0.0042(9) C17 0.0334(12) 0.0407(13) 0.0418(13) -0.0134(10) 0.0126(11) 0.0050(10) C18 0.0318(13) 0.0300(12) 0.0598(15) -0.0104(11) 0.0046(12) 0.0110(10) C19 0.0433(14) 0.0292(12) 0.0507(14) 0.0095(10) 0.0047(12) 0.0131(10) C20 0.0404(13) 0.0293(11) 0.0351(11) 0.0055(9) 0.0115(10) 0.0071(10) C21 0.0227(10) 0.0230(10) 0.0439(12) -0.0075(9) 0.0079(9) -0.0048(8) C22 0.0380(14) 0.0610(17) 0.0545(16) -0.0354(14) 0.0035(12) -0.0028(12) C23 0.0472(16) 0.0319(13) 0.094(2) 0.0163(14) 0.0223(16) -0.0087(12) C24 0.0175(10) 0.0285(10) 0.0317(10) -0.0066(8) 0.0070(8) -0.0002(8) C25 0.0242(11) 0.0324(11) 0.0437(12) -0.0012(9) 0.0092(10) -0.0054(9) C26 0.0273(12) 0.0346(12) 0.0371(12) -0.0029(9) -0.0023(10) 0.0039(9) C27 0.0344(12) 0.0427(13) 0.0284(10) -0.0001(9) 0.0166(10) -0.0011(10) C28 0.0314(12) 0.0357(11) 0.0200(9) 0.0040(8) 0.0057(9) 0.0048(9) C29 0.0269(11) 0.0285(11) 0.0361(11) 0.0043(9) 0.0133(9) 0.0069(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 Cr C31 1.853(2) . ? Cr C29 1.879(2) . ? Cr C27 1.879(2) . ? Cr C30 1.880(2) . ? Cr C28 1.887(2) . ? Cr Si 2.4181(7) . ? Si N1 1.7982(17) . ? Si N3 1.8014(17) . ? Si N4 2.0825(17) . ? Si N2 2.1567(19) . ? Si C14 2.3838(19) . ? Si C1 2.416(2) . ? O1 C27 1.154(3) . ? O2 C28 1.146(3) . ? N1 C1 1.358(3) . ? N1 C8 1.466(2) . ? N2 C1 1.307(3) . ? N2 C11 1.479(3) . ? N3 C14 1.347(3) . ? N3 C21 1.467(2) . ? O3 C29 1.152(3) . ? N4 C14 1.314(2) . ? N4 C24 1.478(3) . ? O4 C30 1.150(3) . ? C1 C2 1.491(3) . ? C2 C3 1.389(3) . ? C2 C7 1.390(3) . ? C3 C4 1.389(3) . ? C4 C5 1.380(4) . ? C5 C6 1.378(4) . ? O5 C31 1.148(3) . ? C6 C7 1.384(3) . ? C8 C10 1.512(3) . ? C8 C9 1.527(3) . ? C11 C13 1.514(3) . ? C11 C12 1.520(3) . ? C14 C15 1.492(3) . ? C15 C20 1.386(3) . ? C15 C16 1.392(3) . ? C16 C17 1.383(3) . ? C17 C18 1.375(4) . ? C18 C19 1.380(4) . ? C19 C20 1.389(3) . ? C21 C23 1.513(3) . ? C21 C22 1.536(3) . ? C24 C25 1.512(3) . ? C24 C26 1.521(3) . ? 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 C31 Cr C29 91.05(10) . . ? C31 Cr C27 88.97(10) . . ? C29 Cr C27 178.54(10) . . ? C31 Cr C30 93.51(10) . . ? C29 Cr C30 87.21(9) . . ? C27 Cr C30 91.33(10) . . ? C31 Cr C28 93.76(10) . . ? C29 Cr C28 92.34(10) . . ? C27 Cr C28 89.12(10) . . ? C30 Cr C28 172.73(9) . . ? C31 Cr Si 179.07(8) . . ? C29 Cr Si 89.41(7) . . ? C27 Cr Si 90.59(7) . . ? C30 Cr Si 87.32(7) . . ? C28 Cr Si 85.42(7) . . ? N1 Si N3 115.11(8) . . ? N1 Si N4 95.11(7) . . ? N3 Si N4 67.27(7) . . ? N1 Si N2 66.14(7) . . ? N3 Si N2 92.88(7) . . ? N4 Si N2 144.64(7) . . ? N1 Si C14 110.16(7) . . ? N3 Si C14 34.08(7) . . ? N4 Si C14 33.35(6) . . ? N2 Si C14 123.04(7) . . ? N1 Si C1 33.72(7) . . ? N3 Si C1 108.57(8) . . ? N4 Si C1 124.63(7) . . ? N2 Si C1 32.58(6) . . ? C14 Si C1 124.63(7) . . ? N1 Si Cr 122.64(6) . . ? N3 Si Cr 122.19(6) . . ? N4 Si Cr 108.22(5) . . ? N2 Si Cr 107.13(5) . . ? C14 Si Cr 118.05(5) . . ? C1 Si Cr 117.28(5) . . ? C1 N1 C8 128.41(17) . . ? C1 N1 Si 98.95(12) . . ? C8 N1 Si 131.83(14) . . ? C1 N2 C11 120.19(17) . . ? C1 N2 Si 84.69(12) . . ? C11 N2 Si 154.52(13) . . ? C14 N3 C21 128.66(17) . . ? C14 N3 Si 97.38(12) . . ? C21 N3 Si 131.96(14) . . ? C14 N4 C24 120.96(16) . . ? C14 N4 Si 86.02(12) . . ? C24 N4 Si 152.24(13) . . ? N2 C1 N1 109.70(17) . . ? N2 C1 C2 125.51(18) . . ? N1 C1 C2 124.76(17) . . ? N2 C1 Si 62.73(11) . . ? N1 C1 Si 47.33(9) . . ? C2 C1 Si 169.54(15) . . ? C3 C2 C7 119.3(2) . . ? C3 C2 C1 120.39(19) . . ? C7 C2 C1 120.31(19) . . ? C4 C3 C2 120.1(2) . . ? C5 C4 C3 119.9(2) . . ? C6 C5 C4 120.4(2) . . ? C5 C6 C7 119.9(2) . . ? C6 C7 C2 120.4(2) . . ? N1 C8 C10 111.9(2) . . ? N1 C8 C9 113.42(18) . . ? C10 C8 C9 112.1(2) . . ? O5 C31 Cr 178.9(2) . . ? O4 C30 Cr 178.5(2) . . ? N2 C11 C13 110.96(18) . . ? N2 C11 C12 111.50(18) . . ? C13 C11 C12 110.82(19) . . ? N4 C14 N3 108.85(16) . . ? N4 C14 C15 125.07(17) . . ? N3 C14 C15 126.07(17) . . ? N4 C14 Si 60.64(10) . . ? N3 C14 Si 48.54(9) . . ? C15 C14 Si 172.60(13) . . ? C20 C15 C16 119.38(19) . . ? C20 C15 C14 120.09(19) . . ? C16 C15 C14 120.51(17) . . ? C17 C16 C15 120.3(2) . . ? C18 C17 C16 120.1(2) . . ? C17 C18 C19 120.2(2) . . ? C18 C19 C20 120.2(2) . . ? C15 C20 C19 119.9(2) . . ? N3 C21 C23 112.2(2) . . ? N3 C21 C22 113.1(2) . . ? C23 C21 C22 112.0(2) . . ? N4 C24 C25 111.37(16) . . ? N4 C24 C26 111.26(18) . . ? C25 C24 C26 110.98(17) . . ? O1 C27 Cr 176.5(2) . . ? O2 C28 Cr 178.6(2) . . ? O3 C29 Cr 176.86(19) . . ? 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 C31 Cr Si N1 165(5) . . . . ? C29 Cr Si N1 44.53(10) . . . . ? C27 Cr Si N1 -134.01(10) . . . . ? C30 Cr Si N1 -42.70(10) . . . . ? C28 Cr Si N1 136.93(10) . . . . ? C31 Cr Si N3 -18(5) . . . . ? C29 Cr Si N3 -138.40(10) . . . . ? C27 Cr Si N3 43.06(10) . . . . ? C30 Cr Si N3 134.36(9) . . . . ? C28 Cr Si N3 -46.01(10) . . . . ? C31 Cr Si N4 56(5) . . . . ? C29 Cr Si N4 -64.27(8) . . . . ? C27 Cr Si N4 117.19(9) . . . . ? C30 Cr Si N4 -151.50(8) . . . . ? C28 Cr Si N4 28.13(8) . . . . ? C31 Cr Si N2 -123(5) . . . . ? C29 Cr Si N2 116.76(8) . . . . ? C27 Cr Si N2 -61.78(9) . . . . ? C30 Cr Si N2 29.52(8) . . . . ? C28 Cr Si N2 -150.85(8) . . . . ? C31 Cr Si C14 21(5) . . . . ? C29 Cr Si C14 -99.07(9) . . . . ? C27 Cr Si C14 82.38(9) . . . . ? C30 Cr Si C14 173.69(8) . . . . ? C28 Cr Si C14 -6.68(9) . . . . ? C31 Cr Si C1 -157(5) . . . . ? C29 Cr Si C1 83.18(9) . . . . ? C27 Cr Si C1 -95.36(9) . . . . ? C30 Cr Si C1 -4.06(9) . . . . ? C28 Cr Si C1 175.57(9) . . . . ? N3 Si N1 C1 -86.06(13) . . . . ? N4 Si N1 C1 -153.33(12) . . . . ? N2 Si N1 C1 -4.49(11) . . . . ? C14 Si N1 C1 -122.71(12) . . . . ? Cr Si N1 C1 91.20(12) . . . . ? N3 Si N1 C8 103.90(18) . . . . ? N4 Si N1 C8 36.63(18) . . . . ? N2 Si N1 C8 -174.54(19) . . . . ? C14 Si N1 C8 67.25(19) . . . . ? C1 Si N1 C8 -170.0(2) . . . . ? Cr Si N1 C8 -78.85(18) . . . . ? N1 Si N2 C1 4.63(11) . . . . ? N3 Si N2 C1 120.89(12) . . . . ? N4 Si N2 C1 67.59(16) . . . . ? C14 Si N2 C1 103.95(12) . . . . ? Cr Si N2 C1 -114.10(11) . . . . ? N1 Si N2 C11 172.8(3) . . . . ? N3 Si N2 C11 -70.9(3) . . . . ? N4 Si N2 C11 -124.2(3) . . . . ? C14 Si N2 C11 -87.9(3) . . . . ? C1 Si N2 C11 168.2(4) . . . . ? Cr Si N2 C11 54.1(3) . . . . ? N1 Si N3 C14 -89.22(13) . . . . ? N4 Si N3 C14 -4.36(11) . . . . ? N2 Si N3 C14 -154.15(12) . . . . ? C1 Si N3 C14 -124.97(12) . . . . ? Cr Si N3 C14 93.51(12) . . . . ? N1 Si N3 C21 106.32(19) . . . . ? N4 Si N3 C21 -168.8(2) . . . . ? N2 Si N3 C21 41.39(19) . . . . ? C14 Si N3 C21 -164.5(3) . . . . ? C1 Si N3 C21 70.6(2) . . . . ? Cr Si N3 C21 -70.9(2) . . . . ? N1 Si N4 C14 119.56(12) . . . . ? N3 Si N4 C14 4.45(11) . . . . ? N2 Si N4 C14 64.70(16) . . . . ? C1 Si N4 C14 101.93(12) . . . . ? Cr Si N4 C14 -113.60(10) . . . . ? N1 Si N4 C24 -73.3(3) . . . . ? N3 Si N4 C24 171.6(3) . . . . ? N2 Si N4 C24 -128.2(3) . . . . ? C14 Si N4 C24 167.1(3) . . . . ? C1 Si N4 C24 -90.9(3) . . . . ? Cr Si N4 C24 53.5(3) . . . . ? C11 N2 C1 N1 179.89(17) . . . . ? Si N2 C1 N1 -5.97(14) . . . . ? C11 N2 C1 C2 -1.7(3) . . . . ? Si N2 C1 C2 172.45(19) . . . . ? C11 N2 C1 Si -174.14(19) . . . . ? C8 N1 C1 N2 177.76(18) . . . . ? Si N1 C1 N2 7.22(17) . . . . ? C8 N1 C1 C2 -0.7(3) . . . . ? Si N1 C1 C2 -171.21(17) . . . . ? C8 N1 C1 Si 170.5(2) . . . . ? N1 Si C1 N2 -172.35(19) . . . . ? N3 Si C1 N2 -64.70(13) . . . . ? N4 Si C1 N2 -139.44(11) . . . . ? C14 Si C1 N2 -98.62(12) . . . . ? Cr Si C1 N2 78.96(12) . . . . ? N3 Si C1 N1 107.65(13) . . . . ? N4 Si C1 N1 32.91(14) . . . . ? N2 Si C1 N1 172.35(19) . . . . ? C14 Si C1 N1 73.73(14) . . . . ? Cr Si C1 N1 -108.69(12) . . . . ? N1 Si C1 C2 43.8(7) . . . . ? N3 Si C1 C2 151.4(7) . . . . ? N4 Si C1 C2 76.7(8) . . . . ? N2 Si C1 C2 -143.9(8) . . . . ? C14 Si C1 C2 117.5(7) . . . . ? Cr Si C1 C2 -64.9(8) . . . . ? N2 C1 C2 C3 -85.2(3) . . . . ? N1 C1 C2 C3 92.9(2) . . . . ? Si C1 C2 C3 54.7(8) . . . . ? N2 C1 C2 C7 94.0(3) . . . . ? N1 C1 C2 C7 -87.8(3) . . . . ? Si C1 C2 C7 -126.0(7) . . . . ? C7 C2 C3 C4 1.3(3) . . . . ? C1 C2 C3 C4 -179.4(2) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C4 C5 C6 C7 0.5(4) . . . . ? C5 C6 C7 C2 0.8(4) . . . . ? C3 C2 C7 C6 -1.7(3) . . . . ? C1 C2 C7 C6 179.0(2) . . . . ? C1 N1 C8 C10 73.2(3) . . . . ? Si N1 C8 C10 -119.4(2) . . . . ? C1 N1 C8 C9 -54.8(3) . . . . ? Si N1 C8 C9 112.6(2) . . . . ? C29 Cr C31 O5 177(100) . . . . ? C27 Cr C31 O5 -4(12) . . . . ? C30 Cr C31 O5 -96(12) . . . . ? C28 Cr C31 O5 85(12) . . . . ? Si Cr C31 O5 57(15) . . . . ? C31 Cr C30 O4 -77(8) . . . . ? C29 Cr C30 O4 14(8) . . . . ? C27 Cr C30 O4 -166(8) . . . . ? C28 Cr C30 O4 100(8) . . . . ? Si Cr C30 O4 103(8) . . . . ? C1 N2 C11 C13 -91.4(2) . . . . ? Si N2 C11 C13 102.3(3) . . . . ? C1 N2 C11 C12 144.6(2) . . . . ? Si N2 C11 C12 -21.7(4) . . . . ? C24 N4 C14 N3 -178.85(16) . . . . ? Si N4 C14 N3 -5.80(14) . . . . ? C24 N4 C14 C15 1.4(3) . . . . ? Si N4 C14 C15 174.42(17) . . . . ? C24 N4 C14 Si -173.05(18) . . . . ? C21 N3 C14 N4 171.96(18) . . . . ? Si N3 C14 N4 6.75(17) . . . . ? C21 N3 C14 C15 -8.3(3) . . . . ? Si N3 C14 C15 -173.47(16) . . . . ? C21 N3 C14 Si 165.2(2) . . . . ? N1 Si C14 N4 -67.35(12) . . . . ? N3 Si C14 N4 -172.67(18) . . . . ? N2 Si C14 N4 -141.37(11) . . . . ? C1 Si C14 N4 -101.94(12) . . . . ? Cr Si C14 N4 80.49(11) . . . . ? N1 Si C14 N3 105.32(13) . . . . ? N4 Si C14 N3 172.67(18) . . . . ? N2 Si C14 N3 31.30(14) . . . . ? C1 Si C14 N3 70.73(14) . . . . ? Cr Si C14 N3 -106.84(12) . . . . ? N1 Si C14 C15 150.8(11) . . . . ? N3 Si C14 C15 45.5(11) . . . . ? N4 Si C14 C15 -141.9(12) . . . . ? N2 Si C14 C15 76.8(11) . . . . ? C1 Si C14 C15 116.2(11) . . . . ? Cr Si C14 C15 -61.4(11) . . . . ? N4 C14 C15 C20 100.7(2) . . . . ? N3 C14 C15 C20 -79.0(3) . . . . ? Si C14 C15 C20 -120.4(11) . . . . ? N4 C14 C15 C16 -77.6(2) . . . . ? N3 C14 C15 C16 102.7(2) . . . . ? Si C14 C15 C16 61.3(12) . . . . ? C20 C15 C16 C17 -0.3(3) . . . . ? C14 C15 C16 C17 177.96(19) . . . . ? C15 C16 C17 C18 0.1(3) . . . . ? C16 C17 C18 C19 0.2(4) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C16 C15 C20 C19 0.3(3) . . . . ? C14 C15 C20 C19 -178.1(2) . . . . ? C18 C19 C20 C15 0.1(4) . . . . ? C14 N3 C21 C23 76.2(3) . . . . ? Si N3 C21 C23 -123.7(2) . . . . ? C14 N3 C21 C22 -51.7(3) . . . . ? Si N3 C21 C22 108.4(2) . . . . ? C14 N4 C24 C25 149.61(18) . . . . ? Si N4 C24 C25 -15.4(4) . . . . ? C14 N4 C24 C26 -86.0(2) . . . . ? Si N4 C24 C26 109.0(3) . . . . ? C31 Cr C27 O1 19(4) . . . . ? C29 Cr C27 O1 110(5) . . . . ? C30 Cr C27 O1 113(4) . . . . ? C28 Cr C27 O1 -74(4) . . . . ? Si Cr C27 O1 -160(4) . . . . ? C31 Cr C28 O2 -106(8) . . . . ? C29 Cr C28 O2 163(8) . . . . ? C27 Cr C28 O2 -17(8) . . . . ? C30 Cr C28 O2 76(8) . . . . ? Si Cr C28 O2 73(8) . . . . ? C31 Cr C29 O3 37(4) . . . . ? C27 Cr C29 O3 -53(6) . . . . ? C30 Cr C29 O3 -56(4) . . . . ? C28 Cr C29 O3 131(4) . . . . ? Si Cr C29 O3 -143(4) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.489 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.066 # ******************* Data Compound 3 ************************* data_jun100c_multiscan _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H38 Mo N4 O5 Si' _chemical_formula_sum 'C31 H38 Mo N4 O5 Si' _chemical_formula_weight 670.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.7945(15) _cell_length_b 19.703(3) _cell_length_c 16.706(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.977(16) _cell_angle_gamma 90.00 _cell_volume 3398.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 29.15 _exptl_crystal_description block _exptl_crystal_colour pale_yellow _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7452 _exptl_absorpt_correction_T_max 0.9467 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image_plate-Stoe-IPDS _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22081 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 26.02 _reflns_number_total 6688 _reflns_number_gt 5782 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP/POV-Ray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+0.5785P] 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 6688 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0357 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _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 Mo Mo 0.776225(14) 0.174326(7) 0.108989(9) 0.02401(7) Uani 1 1 d . . . Si Si 0.82216(5) 0.08838(2) 0.23053(3) 0.02365(11) Uani 1 1 d . . . O1 O 0.57280(18) 0.07715(11) -0.01448(12) 0.0649(5) Uani 1 1 d . . . O2 O 1.00325(16) 0.09865(10) 0.05886(10) 0.0535(4) Uani 1 1 d . . . O3 O 0.96674(16) 0.28189(9) 0.22366(12) 0.0563(5) Uani 1 1 d . . . O4 O 0.55597(17) 0.23624(9) 0.17902(13) 0.0582(5) Uani 1 1 d . . . O5 O 0.72070(16) 0.27598(10) -0.04270(11) 0.0603(5) Uani 1 1 d . . . N1 N 0.82954(14) 0.11159(7) 0.33666(9) 0.0238(3) Uani 1 1 d . . . N2 N 0.64426(14) 0.07310(8) 0.26039(9) 0.0257(3) Uani 1 1 d . . . N3 N 0.84512(14) -0.00101(7) 0.21587(9) 0.0238(3) Uani 1 1 d . . . N4 N 1.01723(13) 0.06103(7) 0.25894(9) 0.0228(3) Uani 1 1 d . . . C1 C 0.70317(17) 0.10178(9) 0.33141(11) 0.0243(3) Uani 1 1 d . . . C2 C 0.64138(17) 0.12264(10) 0.39751(11) 0.0279(4) Uani 1 1 d . . . C3 C 0.6454(2) 0.07997(12) 0.46417(13) 0.0389(5) Uani 1 1 d . . . H3 H 0.6866 0.0370 0.4679 0.047 Uiso 1 1 calc R . . C4 C 0.5892(2) 0.09980(16) 0.52590(14) 0.0531(7) Uani 1 1 d . . . H4 H 0.5927 0.0707 0.5718 0.064 Uiso 1 1 calc R . . C5 C 0.5287(2) 0.16201(16) 0.51971(15) 0.0562(7) Uani 1 1 d . . . H5 H 0.4910 0.1759 0.5619 0.067 Uiso 1 1 calc R . . C6 C 0.5223(2) 0.20434(14) 0.45281(15) 0.0491(6) Uani 1 1 d . . . H6 H 0.4797 0.2469 0.4489 0.059 Uiso 1 1 calc R . . C7 C 0.5781(2) 0.18481(11) 0.39104(14) 0.0373(5) Uani 1 1 d . . . H7 H 0.5730 0.2138 0.3447 0.045 Uiso 1 1 calc R . . C8 C 0.92940(18) 0.14737(11) 0.40170(11) 0.0310(4) Uani 1 1 d . . . H8 H 1.0061 0.1518 0.3799 0.037 Uiso 1 1 calc R . . C9 C 0.8904(2) 0.21966(14) 0.4173(2) 0.0673(9) Uani 1 1 d . . . H9A H 0.8507 0.2421 0.3636 0.101 Uiso 1 1 calc R . . H9B H 0.9674 0.2450 0.4485 0.101 Uiso 1 1 calc R . . H9C H 0.8282 0.2181 0.4498 0.101 Uiso 1 1 calc R . . C10 C 0.9745(3) 0.10661(19) 0.48153(15) 0.0700(9) Uani 1 1 d . . . H10A H 0.9902 0.0596 0.4681 0.105 Uiso 1 1 calc R . . H10B H 0.9078 0.1076 0.5106 0.105 Uiso 1 1 calc R . . H10C H 1.0549 0.1262 0.5177 0.105 Uiso 1 1 calc R . . C11 C 0.50471(18) 0.05541(11) 0.23947(12) 0.0321(4) Uani 1 1 d . . . H11 H 0.4633 0.0872 0.2707 0.038 Uiso 1 1 calc R . . C12 C 0.4373(2) 0.06416(13) 0.14669(13) 0.0429(5) Uani 1 1 d . . . H12A H 0.4762 0.0334 0.1147 0.064 Uiso 1 1 calc R . . H12B H 0.4471 0.1112 0.1303 0.064 Uiso 1 1 calc R . . H12C H 0.3451 0.0535 0.1351 0.064 Uiso 1 1 calc R . . C13 C 0.4877(2) -0.01650(12) 0.26777(15) 0.0458(5) Uani 1 1 d . . . H13A H 0.3952 -0.0262 0.2570 0.069 Uiso 1 1 calc R . . H13B H 0.5315 -0.0208 0.3278 0.069 Uiso 1 1 calc R . . H13C H 0.5253 -0.0488 0.2368 0.069 Uiso 1 1 calc R . . C14 C 0.97514(16) 0.00039(9) 0.23230(10) 0.0225(3) Uani 1 1 d . . . C15 C 1.05810(17) -0.05799(9) 0.22265(11) 0.0259(4) Uani 1 1 d . . . C16 C 1.10763(19) -0.06119(10) 0.15427(12) 0.0328(4) Uani 1 1 d . . . H16 H 1.0868 -0.0268 0.1126 0.039 Uiso 1 1 calc R . . C17 C 1.1871(2) -0.11465(12) 0.14735(14) 0.0423(5) Uani 1 1 d . . . H17 H 1.2209 -0.1168 0.1009 0.051 Uiso 1 1 calc R . . C18 C 1.2174(2) -0.16459(11) 0.20735(17) 0.0458(6) Uani 1 1 d . . . H18 H 1.2717 -0.2012 0.2021 0.055 Uiso 1 1 calc R . . C19 C 1.1689(2) -0.16159(11) 0.27537(17) 0.0494(6) Uani 1 1 d . . . H19 H 1.1901 -0.1962 0.3168 0.059 Uiso 1 1 calc R . . C20 C 1.0895(2) -0.10822(11) 0.28321(14) 0.0393(5) Uani 1 1 d . . . H20 H 1.0567 -0.1061 0.3301 0.047 Uiso 1 1 calc R . . C21 C 0.75374(19) -0.05313(10) 0.17106(14) 0.0357(4) Uani 1 1 d . . . H21 H 0.6654 -0.0326 0.1589 0.043 Uiso 1 1 calc R . . C22 C 0.7720(2) -0.07175(17) 0.08543(18) 0.0636(8) Uani 1 1 d . . . H22A H 0.6977 -0.0986 0.0531 0.095 Uiso 1 1 calc R . . H22B H 0.8515 -0.0984 0.0941 0.095 Uiso 1 1 calc R . . H22C H 0.7782 -0.0301 0.0547 0.095 Uiso 1 1 calc R . . C23 C 0.7536(3) -0.11490(13) 0.2248(2) 0.0718(9) Uani 1 1 d . . . H23A H 0.6759 -0.1420 0.1996 0.108 Uiso 1 1 calc R . . H23B H 0.7538 -0.1004 0.2810 0.108 Uiso 1 1 calc R . . H23C H 0.8309 -0.1423 0.2287 0.108 Uiso 1 1 calc R . . C24 C 1.15680(16) 0.07783(9) 0.28180(12) 0.0276(4) Uani 1 1 d . . . H24 H 1.1965 0.0502 0.2454 0.033 Uiso 1 1 calc R . . C25 C 1.17725(19) 0.15223(10) 0.26556(13) 0.0356(4) Uani 1 1 d . . . H25A H 1.1394 0.1621 0.2059 0.053 Uiso 1 1 calc R . . H25B H 1.2702 0.1622 0.2820 0.053 Uiso 1 1 calc R . . H25C H 1.1353 0.1805 0.2984 0.053 Uiso 1 1 calc R . . C26 C 1.22477(19) 0.05906(11) 0.37264(13) 0.0394(5) Uani 1 1 d . . . H26A H 1.2081 0.0112 0.3819 0.059 Uiso 1 1 calc R . . H26B H 1.1916 0.0876 0.4099 0.059 Uiso 1 1 calc R . . H26C H 1.3182 0.0663 0.3845 0.059 Uiso 1 1 calc R . . C27 C 0.6461(2) 0.11031(11) 0.03211(13) 0.0379(5) Uani 1 1 d . . . C28 C 0.92239(19) 0.12679(11) 0.07641(11) 0.0336(4) Uani 1 1 d . . . C29 C 0.90016(19) 0.24160(10) 0.18370(13) 0.0344(4) Uani 1 1 d . . . C30 C 0.63456(19) 0.21415(10) 0.15316(13) 0.0346(4) Uani 1 1 d . . . C31 C 0.74148(18) 0.23937(11) 0.01304(13) 0.0367(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo 0.02408(10) 0.02526(10) 0.02317(10) 0.00433(6) 0.00764(7) 0.00233(6) Si 0.0309(2) 0.0205(2) 0.0202(2) -0.00087(17) 0.00847(19) 0.00175(18) O1 0.0548(11) 0.0858(14) 0.0547(10) -0.0306(10) 0.0171(9) -0.0274(10) O2 0.0474(9) 0.0760(12) 0.0406(9) 0.0015(8) 0.0184(7) 0.0262(9) O3 0.0404(9) 0.0438(9) 0.0790(12) -0.0187(9) 0.0086(8) -0.0043(7) O4 0.0506(10) 0.0529(10) 0.0833(13) -0.0089(9) 0.0389(10) 0.0087(8) O5 0.0454(9) 0.0758(12) 0.0616(11) 0.0468(10) 0.0187(8) 0.0168(9) N1 0.0210(7) 0.0292(8) 0.0224(7) -0.0014(6) 0.0084(6) 0.0009(6) N2 0.0230(7) 0.0293(8) 0.0270(7) -0.0015(6) 0.0107(6) -0.0014(6) N3 0.0222(7) 0.0212(7) 0.0287(7) -0.0020(6) 0.0083(6) -0.0007(5) N4 0.0212(7) 0.0230(7) 0.0242(7) -0.0020(6) 0.0070(6) 0.0014(6) C1 0.0245(8) 0.0251(8) 0.0248(8) 0.0031(7) 0.0098(7) 0.0028(7) C2 0.0223(8) 0.0396(10) 0.0231(8) -0.0043(7) 0.0084(7) 0.0002(7) C3 0.0357(11) 0.0531(13) 0.0317(10) 0.0066(9) 0.0158(8) 0.0089(9) C4 0.0442(13) 0.089(2) 0.0321(11) 0.0115(12) 0.0209(10) 0.0125(12) C5 0.0426(13) 0.096(2) 0.0350(12) -0.0096(12) 0.0193(10) 0.0193(13) C6 0.0396(12) 0.0612(15) 0.0493(13) -0.0127(12) 0.0172(10) 0.0158(11) C7 0.0329(10) 0.0441(12) 0.0368(11) -0.0035(9) 0.0132(9) 0.0056(9) C8 0.0255(9) 0.0414(11) 0.0261(9) -0.0096(8) 0.0079(7) -0.0018(8) C9 0.0406(13) 0.0547(16) 0.109(2) -0.0485(16) 0.0263(14) -0.0118(11) C10 0.0459(14) 0.123(3) 0.0320(12) 0.0193(15) -0.0036(10) -0.0167(16) C11 0.0242(9) 0.0411(11) 0.0324(10) -0.0065(8) 0.0105(7) -0.0055(8) C12 0.0324(10) 0.0556(13) 0.0368(11) -0.0048(10) 0.0041(9) -0.0092(10) C13 0.0357(11) 0.0525(14) 0.0520(13) 0.0016(11) 0.0169(10) -0.0138(10) C14 0.0243(8) 0.0240(8) 0.0194(8) 0.0000(6) 0.0066(6) 0.0016(7) C15 0.0226(8) 0.0226(8) 0.0306(9) -0.0043(7) 0.0049(7) 0.0018(7) C16 0.0330(10) 0.0337(10) 0.0313(9) -0.0032(8) 0.0088(8) 0.0060(8) C17 0.0351(11) 0.0473(13) 0.0456(12) -0.0162(10) 0.0133(9) 0.0072(9) C18 0.0331(11) 0.0331(11) 0.0655(15) -0.0132(10) 0.0055(10) 0.0103(9) C19 0.0488(13) 0.0319(11) 0.0614(15) 0.0113(10) 0.0066(12) 0.0129(10) C20 0.0437(12) 0.0346(11) 0.0405(11) 0.0077(9) 0.0137(9) 0.0091(9) C21 0.0261(9) 0.0273(9) 0.0524(12) -0.0101(9) 0.0097(9) -0.0054(7) C22 0.0407(13) 0.079(2) 0.0646(16) -0.0450(15) 0.0052(11) -0.0015(12) C23 0.0555(16) 0.0332(13) 0.127(3) 0.0129(15) 0.0272(17) -0.0106(11) C24 0.0205(8) 0.0283(9) 0.0331(9) -0.0059(7) 0.0064(7) 0.0007(7) C25 0.0281(9) 0.0340(10) 0.0431(11) -0.0025(9) 0.0081(8) -0.0067(8) C26 0.0308(10) 0.0383(11) 0.0401(11) -0.0030(9) -0.0038(8) 0.0036(8) C27 0.0374(11) 0.0476(12) 0.0315(10) -0.0019(9) 0.0142(9) -0.0041(9) C28 0.0358(10) 0.0405(11) 0.0234(9) 0.0050(8) 0.0070(8) 0.0061(8) C29 0.0298(10) 0.0316(10) 0.0418(11) 0.0021(9) 0.0105(8) 0.0046(8) C30 0.0356(10) 0.0289(10) 0.0395(11) 0.0013(8) 0.0113(9) 0.0003(8) C31 0.0236(9) 0.0458(12) 0.0421(11) 0.0129(9) 0.0122(8) 0.0061(8) _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 Mo C31 2.000(2) . ? Mo C29 2.032(2) . ? Mo C30 2.039(2) . ? Mo C27 2.039(2) . ? Mo C28 2.041(2) . ? Mo Si 2.5784(6) . ? Si N3 1.8052(15) . ? Si N1 1.8101(15) . ? Si N4 2.0894(15) . ? Si N2 2.1417(15) . ? Si C14 2.3884(17) . ? Si C1 2.4133(17) . ? O1 C27 1.140(3) . ? O2 C28 1.142(2) . ? O3 C29 1.145(3) . ? O4 C30 1.144(3) . ? O5 C31 1.147(2) . ? N1 C1 1.355(2) . ? N1 C8 1.468(2) . ? N2 C1 1.300(2) . ? N2 C11 1.485(2) . ? N3 C14 1.349(2) . ? N3 C21 1.469(2) . ? N4 C14 1.309(2) . ? N4 C24 1.480(2) . ? C1 C2 1.504(2) . ? C2 C3 1.386(3) . ? C2 C7 1.391(3) . ? C3 C4 1.396(3) . ? C4 C5 1.379(4) . ? C5 C6 1.380(4) . ? C6 C7 1.393(3) . ? C8 C10 1.510(3) . ? C8 C9 1.529(3) . ? C11 C12 1.518(3) . ? C11 C13 1.522(3) . ? C14 C15 1.495(2) . ? C15 C20 1.385(3) . ? C15 C16 1.397(3) . ? C16 C17 1.385(3) . ? C17 C18 1.374(3) . ? C18 C19 1.384(4) . ? C19 C20 1.387(3) . ? C21 C23 1.513(3) . ? C21 C22 1.544(3) . ? C24 C25 1.519(3) . ? C24 C26 1.526(3) . ? 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 C31 Mo C29 90.57(9) . . ? C31 Mo C30 93.35(8) . . ? C29 Mo C30 87.45(8) . . ? C31 Mo C27 87.60(9) . . ? C29 Mo C27 177.42(8) . . ? C30 Mo C27 90.84(8) . . ? C31 Mo C28 93.38(8) . . ? C29 Mo C28 92.38(8) . . ? C30 Mo C28 173.27(8) . . ? C27 Mo C28 89.55(8) . . ? C31 Mo Si 178.70(7) . . ? C29 Mo Si 90.23(6) . . ? C30 Mo Si 87.70(6) . . ? C27 Mo Si 91.63(6) . . ? C28 Mo Si 85.57(6) . . ? N3 Si N1 114.26(7) . . ? N3 Si N4 67.05(6) . . ? N1 Si N4 95.13(6) . . ? N3 Si N2 93.58(6) . . ? N1 Si N2 66.00(6) . . ? N4 Si N2 145.44(6) . . ? N3 Si C14 34.08(6) . . ? N1 Si C14 109.80(6) . . ? N4 Si C14 33.15(6) . . ? N2 Si C14 123.97(6) . . ? N3 Si C1 108.88(7) . . ? N1 Si C1 33.75(6) . . ? N4 Si C1 125.18(6) . . ? N2 Si C1 32.48(6) . . ? C14 Si C1 125.29(6) . . ? N3 Si Mo 122.44(5) . . ? N1 Si Mo 123.28(5) . . ? N4 Si Mo 107.32(5) . . ? N2 Si Mo 107.24(5) . . ? C14 Si Mo 117.37(4) . . ? C1 Si Mo 117.31(4) . . ? C1 N1 C8 128.61(14) . . ? C1 N1 Si 98.35(11) . . ? C8 N1 Si 131.22(12) . . ? C1 N2 C11 120.60(15) . . ? C1 N2 Si 85.33(10) . . ? C11 N2 Si 153.51(12) . . ? C14 N3 C21 128.45(15) . . ? C14 N3 Si 97.37(11) . . ? C21 N3 Si 130.77(12) . . ? C14 N4 C24 121.20(14) . . ? C14 N4 Si 86.07(10) . . ? C24 N4 Si 152.08(12) . . ? N2 C1 N1 109.63(15) . . ? N2 C1 C2 125.80(16) . . ? N1 C1 C2 124.56(16) . . ? N2 C1 Si 62.19(9) . . ? N1 C1 Si 47.91(8) . . ? C2 C1 Si 169.40(13) . . ? C3 C2 C7 119.74(17) . . ? C3 C2 C1 120.50(17) . . ? C7 C2 C1 119.76(17) . . ? C2 C3 C4 120.4(2) . . ? C5 C4 C3 119.5(2) . . ? C4 C5 C6 120.6(2) . . ? C5 C6 C7 120.2(2) . . ? C2 C7 C6 119.6(2) . . ? N1 C8 C10 112.08(19) . . ? N1 C8 C9 113.23(17) . . ? C10 C8 C9 112.2(2) . . ? N2 C11 C12 111.38(16) . . ? N2 C11 C13 110.59(17) . . ? C12 C11 C13 110.97(18) . . ? N4 C14 N3 108.96(14) . . ? N4 C14 C15 125.41(15) . . ? N3 C14 C15 125.62(15) . . ? N4 C14 Si 60.78(9) . . ? N3 C14 Si 48.55(8) . . ? C15 C14 Si 172.22(12) . . ? C20 C15 C16 119.64(17) . . ? C20 C15 C14 119.85(17) . . ? C16 C15 C14 120.48(16) . . ? C17 C16 C15 119.81(19) . . ? C18 C17 C16 120.3(2) . . ? C17 C18 C19 120.11(19) . . ? C18 C19 C20 120.2(2) . . ? C15 C20 C19 120.0(2) . . ? N3 C21 C23 112.2(2) . . ? N3 C21 C22 112.96(18) . . ? C23 C21 C22 112.4(2) . . ? N4 C24 C25 111.10(15) . . ? N4 C24 C26 111.11(16) . . ? C25 C24 C26 111.04(16) . . ? O1 C27 Mo 176.1(2) . . ? O2 C28 Mo 178.24(19) . . ? O3 C29 Mo 176.84(19) . . ? O4 C30 Mo 179.1(2) . . ? O5 C31 Mo 179.1(2) . . ? 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 C31 Mo Si N3 -10(3) . . . . ? C29 Mo Si N3 -137.85(8) . . . . ? C30 Mo Si N3 134.71(8) . . . . ? C27 Mo Si N3 43.94(8) . . . . ? C28 Mo Si N3 -45.49(8) . . . . ? C31 Mo Si N1 172(3) . . . . ? C29 Mo Si N1 44.00(8) . . . . ? C30 Mo Si N1 -43.44(8) . . . . ? C27 Mo Si N1 -134.21(8) . . . . ? C28 Mo Si N1 136.37(8) . . . . ? C31 Mo Si N4 64(3) . . . . ? C29 Mo Si N4 -64.46(7) . . . . ? C30 Mo Si N4 -151.90(7) . . . . ? C27 Mo Si N4 117.33(7) . . . . ? C28 Mo Si N4 27.91(7) . . . . ? C31 Mo Si N2 -116(3) . . . . ? C29 Mo Si N2 116.20(7) . . . . ? C30 Mo Si N2 28.76(7) . . . . ? C27 Mo Si N2 -62.01(8) . . . . ? C28 Mo Si N2 -151.43(7) . . . . ? C31 Mo Si C14 29(3) . . . . ? C29 Mo Si C14 -98.76(7) . . . . ? C30 Mo Si C14 173.80(7) . . . . ? C27 Mo Si C14 83.03(8) . . . . ? C28 Mo Si C14 -6.39(8) . . . . ? C31 Mo Si C1 -149(3) . . . . ? C29 Mo Si C1 82.70(8) . . . . ? C30 Mo Si C1 -4.74(8) . . . . ? C27 Mo Si C1 -95.51(8) . . . . ? C28 Mo Si C1 175.07(8) . . . . ? N3 Si N1 C1 -87.96(12) . . . . ? N4 Si N1 C1 -155.07(11) . . . . ? N2 Si N1 C1 -5.18(10) . . . . ? C14 Si N1 C1 -124.51(11) . . . . ? Mo Si N1 C1 90.32(11) . . . . ? N3 Si N1 C8 106.78(17) . . . . ? N4 Si N1 C8 39.67(17) . . . . ? N2 Si N1 C8 -170.44(18) . . . . ? C14 Si N1 C8 70.23(17) . . . . ? C1 Si N1 C8 -165.3(2) . . . . ? Mo Si N1 C8 -74.94(17) . . . . ? N3 Si N2 C1 120.37(11) . . . . ? N1 Si N2 C1 5.36(10) . . . . ? N4 Si N2 C1 67.10(15) . . . . ? C14 Si N2 C1 103.82(11) . . . . ? Mo Si N2 C1 -114.03(10) . . . . ? N3 Si N2 C11 -70.7(3) . . . . ? N1 Si N2 C11 174.2(3) . . . . ? N4 Si N2 C11 -124.0(3) . . . . ? C14 Si N2 C11 -87.3(3) . . . . ? C1 Si N2 C11 168.9(3) . . . . ? Mo Si N2 C11 54.9(3) . . . . ? N1 Si N3 C14 -89.82(11) . . . . ? N4 Si N3 C14 -4.65(10) . . . . ? N2 Si N3 C14 -155.06(10) . . . . ? C1 Si N3 C14 -125.74(10) . . . . ? Mo Si N3 C14 91.88(11) . . . . ? N1 Si N3 C21 110.21(17) . . . . ? N4 Si N3 C21 -164.63(18) . . . . ? N2 Si N3 C21 44.97(17) . . . . ? C14 Si N3 C21 -160.0(2) . . . . ? C1 Si N3 C21 74.28(17) . . . . ? Mo Si N3 C21 -68.09(17) . . . . ? N3 Si N4 C14 4.77(10) . . . . ? N1 Si N4 C14 118.97(10) . . . . ? N2 Si N4 C14 65.08(15) . . . . ? C1 Si N4 C14 102.33(11) . . . . ? Mo Si N4 C14 -113.79(9) . . . . ? N3 Si N4 C24 173.1(3) . . . . ? N1 Si N4 C24 -72.7(3) . . . . ? N2 Si N4 C24 -126.6(2) . . . . ? C14 Si N4 C24 168.3(3) . . . . ? C1 Si N4 C24 -89.4(3) . . . . ? Mo Si N4 C24 54.5(3) . . . . ? C11 N2 C1 N1 178.78(16) . . . . ? Si N2 C1 N1 -6.96(13) . . . . ? C11 N2 C1 C2 -2.5(3) . . . . ? Si N2 C1 C2 171.78(17) . . . . ? C11 N2 C1 Si -174.27(18) . . . . ? C8 N1 C1 N2 174.12(17) . . . . ? Si N1 C1 N2 8.30(16) . . . . ? C8 N1 C1 C2 -4.6(3) . . . . ? Si N1 C1 C2 -170.46(15) . . . . ? C8 N1 C1 Si 165.8(2) . . . . ? N3 Si C1 N2 -65.51(12) . . . . ? N1 Si C1 N2 -171.16(17) . . . . ? N4 Si C1 N2 -140.26(11) . . . . ? C14 Si C1 N2 -99.37(12) . . . . ? Mo Si C1 N2 79.05(11) . . . . ? N3 Si C1 N1 105.65(12) . . . . ? N4 Si C1 N1 30.90(13) . . . . ? N2 Si C1 N1 171.16(17) . . . . ? C14 Si C1 N1 71.79(13) . . . . ? Mo Si C1 N1 -109.80(11) . . . . ? N3 Si C1 C2 153.6(7) . . . . ? N1 Si C1 C2 47.9(7) . . . . ? N4 Si C1 C2 78.8(7) . . . . ? N2 Si C1 C2 -140.9(7) . . . . ? C14 Si C1 C2 119.7(7) . . . . ? Mo Si C1 C2 -61.9(7) . . . . ? N2 C1 C2 C3 95.3(2) . . . . ? N1 C1 C2 C3 -86.1(2) . . . . ? Si C1 C2 C3 -128.1(6) . . . . ? N2 C1 C2 C7 -83.7(2) . . . . ? N1 C1 C2 C7 94.8(2) . . . . ? Si C1 C2 C7 52.8(8) . . . . ? C7 C2 C3 C4 -1.7(3) . . . . ? C1 C2 C3 C4 179.3(2) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 C6 0.6(4) . . . . ? C4 C5 C6 C7 -0.6(4) . . . . ? C3 C2 C7 C6 1.7(3) . . . . ? C1 C2 C7 C6 -179.27(19) . . . . ? C5 C6 C7 C2 -0.6(4) . . . . ? C1 N1 C8 C10 74.4(3) . . . . ? Si N1 C8 C10 -124.36(19) . . . . ? C1 N1 C8 C9 -53.8(3) . . . . ? Si N1 C8 C9 107.4(2) . . . . ? C1 N2 C11 C12 145.16(18) . . . . ? Si N2 C11 C12 -21.9(4) . . . . ? C1 N2 C11 C13 -90.9(2) . . . . ? Si N2 C11 C13 101.9(3) . . . . ? C24 N4 C14 N3 -179.85(14) . . . . ? Si N4 C14 N3 -6.22(13) . . . . ? C24 N4 C14 C15 0.8(3) . . . . ? Si N4 C14 C15 174.42(16) . . . . ? C24 N4 C14 Si -173.64(17) . . . . ? C21 N3 C14 N4 167.90(17) . . . . ? Si N3 C14 N4 7.24(15) . . . . ? C21 N3 C14 C15 -12.7(3) . . . . ? Si N3 C14 C15 -173.39(15) . . . . ? C21 N3 C14 Si 160.7(2) . . . . ? N3 Si C14 N4 -172.15(16) . . . . ? N1 Si C14 N4 -67.83(11) . . . . ? N2 Si C14 N4 -141.65(10) . . . . ? C1 Si C14 N4 -101.95(11) . . . . ? Mo Si C14 N4 79.64(10) . . . . ? N1 Si C14 N3 104.31(11) . . . . ? N4 Si C14 N3 172.15(16) . . . . ? N2 Si C14 N3 30.49(13) . . . . ? C1 Si C14 N3 70.20(12) . . . . ? Mo Si C14 N3 -108.22(10) . . . . ? N3 Si C14 C15 43.7(9) . . . . ? N1 Si C14 C15 148.0(9) . . . . ? N4 Si C14 C15 -144.2(10) . . . . ? N2 Si C14 C15 74.2(10) . . . . ? C1 Si C14 C15 113.9(9) . . . . ? Mo Si C14 C15 -64.5(10) . . . . ? N4 C14 C15 C20 100.5(2) . . . . ? N3 C14 C15 C20 -78.7(2) . . . . ? Si C14 C15 C20 -118.3(9) . . . . ? N4 C14 C15 C16 -77.5(2) . . . . ? N3 C14 C15 C16 103.3(2) . . . . ? Si C14 C15 C16 63.7(10) . . . . ? C20 C15 C16 C17 0.3(3) . . . . ? C14 C15 C16 C17 178.29(18) . . . . ? C15 C16 C17 C18 0.1(3) . . . . ? C16 C17 C18 C19 -0.2(3) . . . . ? C17 C18 C19 C20 0.0(4) . . . . ? C16 C15 C20 C19 -0.5(3) . . . . ? C14 C15 C20 C19 -178.5(2) . . . . ? C18 C19 C20 C15 0.3(4) . . . . ? C14 N3 C21 C23 77.5(3) . . . . ? Si N3 C21 C23 -128.23(19) . . . . ? C14 N3 C21 C22 -50.8(3) . . . . ? Si N3 C21 C22 103.5(2) . . . . ? C14 N4 C24 C25 149.54(16) . . . . ? Si N4 C24 C25 -16.8(3) . . . . ? C14 N4 C24 C26 -86.3(2) . . . . ? Si N4 C24 C26 107.4(3) . . . . ? C31 Mo C27 O1 4(3) . . . . ? C29 Mo C27 O1 49(4) . . . . ? C30 Mo C27 O1 97(3) . . . . ? C28 Mo C27 O1 -90(3) . . . . ? Si Mo C27 O1 -175(3) . . . . ? C31 Mo C28 O2 -145(6) . . . . ? C29 Mo C28 O2 125(6) . . . . ? C30 Mo C28 O2 36(6) . . . . ? C27 Mo C28 O2 -57(6) . . . . ? Si Mo C28 O2 35(6) . . . . ? C31 Mo C29 O3 29(4) . . . . ? C30 Mo C29 O3 -64(3) . . . . ? C27 Mo C29 O3 -16(5) . . . . ? C28 Mo C29 O3 123(3) . . . . ? Si Mo C29 O3 -152(3) . . . . ? C31 Mo C30 O4 -152(12) . . . . ? C29 Mo C30 O4 -61(12) . . . . ? C27 Mo C30 O4 121(12) . . . . ? C28 Mo C30 O4 27(12) . . . . ? Si Mo C30 O4 29(12) . . . . ? C29 Mo C31 O5 169(100) . . . . ? C30 Mo C31 O5 -103(11) . . . . ? C27 Mo C31 O5 -13(11) . . . . ? C28 Mo C31 O5 77(11) . . . . ? Si Mo C31 O5 41(13) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.528 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.061 # ******************* Data Compound 5 ************************* data_jun83c_multiscan _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H38 Fe N4 O4 Si' _chemical_formula_sum 'C30 H38 Fe N4 O4 Si' _chemical_formula_weight 602.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.8895(13) _cell_length_b 21.702(3) _cell_length_c 14.547(2) _cell_angle_alpha 90.00 _cell_angle_beta 99.006(16) _cell_angle_gamma 90.00 _cell_volume 3083.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 4998 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 29.15 _exptl_crystal_description block _exptl_crystal_colour yellow-brown _exptl_crystal_size_max .8 _exptl_crystal_size_mid .6 _exptl_crystal_size_min .35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1272 _exptl_absorpt_coefficient_mu 0.568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.7275 _exptl_absorpt_correction_T_max 0.8322 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type image-plate_Stoe-IPDS _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22395 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 26.02 _reflns_number_total 6056 _reflns_number_gt 5096 _reflns_threshold_expression >2sigma(I) _computing_data_collection Stoe-IPDS _computing_cell_refinement Stoe-IPDS _computing_data_reduction Stoe-IPDS _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP/POV-Ray _computing_publication_material Bruker-SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+0.0053P] 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 6056 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0938 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Fe Fe 0.26610(2) 0.346394(10) 0.437187(15) 0.02404(9) Uani 1 1 d . . . Si Si 0.15617(4) 0.381647(17) 0.29447(3) 0.01945(10) Uani 1 1 d . . . O1 O 0.30753(19) 0.42064(7) 0.60799(10) 0.0550(4) Uani 1 1 d . . . O2 O 0.50254(15) 0.38712(9) 0.35557(12) 0.0592(4) Uani 1 1 d . . . O3 O 0.37324(17) 0.22249(6) 0.47620(11) 0.0537(4) Uani 1 1 d . . . O4 O -0.01338(14) 0.30590(8) 0.44480(10) 0.0520(4) Uani 1 1 d . . . N2 N 0.17121(13) 0.47114(5) 0.30916(9) 0.0218(3) Uani 1 1 d . . . N1 N 0.23632(13) 0.41581(6) 0.20221(9) 0.0240(3) Uani 1 1 d . . . N4 N 0.10282(12) 0.30430(6) 0.22516(9) 0.0218(3) Uani 1 1 d . . . N3 N -0.02846(13) 0.37772(6) 0.25659(9) 0.0228(3) Uani 1 1 d . . . C1 C 0.23380(16) 0.47353(7) 0.23561(11) 0.0242(3) Uani 1 1 d . . . C2 C 0.28981(19) 0.52875(7) 0.19362(11) 0.0306(4) Uani 1 1 d . . . C3 C 0.4292(2) 0.54050(9) 0.20572(14) 0.0413(4) Uani 1 1 d . . . H3 H 0.4915 0.5144 0.2439 0.050 Uiso 1 1 calc R . . C4 C 0.4769(3) 0.59128(10) 0.16099(18) 0.0597(7) Uani 1 1 d . . . H4 H 0.5722 0.5999 0.1692 0.072 Uiso 1 1 calc R . . C5 C 0.3873(3) 0.62872(10) 0.10543(17) 0.0638(8) Uani 1 1 d . . . H5 H 0.4210 0.6625 0.0741 0.077 Uiso 1 1 calc R . . C6 C 0.2491(3) 0.61768(10) 0.09490(17) 0.0630(7) Uani 1 1 d . . . H6 H 0.1874 0.6442 0.0569 0.076 Uiso 1 1 calc R . . C7 C 0.1988(2) 0.56802(9) 0.13943(14) 0.0460(5) Uani 1 1 d . . . H7 H 0.1030 0.5609 0.1329 0.055 Uiso 1 1 calc R . . C8 C 0.17975(17) 0.51606(7) 0.38630(11) 0.0261(3) Uani 1 1 d . . . H8 H 0.1420 0.4950 0.4379 0.031 Uiso 1 1 calc R . . C9 C 0.32606(18) 0.53439(8) 0.42518(12) 0.0339(4) Uani 1 1 d . . . H9A H 0.3825 0.4973 0.4373 0.051 Uiso 1 1 calc R . . H9B H 0.3270 0.5573 0.4834 0.051 Uiso 1 1 calc R . . H9C H 0.3629 0.5604 0.3799 0.051 Uiso 1 1 calc R . . C10 C 0.0907(2) 0.57288(8) 0.36043(14) 0.0380(4) Uani 1 1 d . . . H10A H 0.1274 0.5965 0.3125 0.057 Uiso 1 1 calc R . . H10B H 0.0906 0.5987 0.4157 0.057 Uiso 1 1 calc R . . H10C H -0.0032 0.5599 0.3365 0.057 Uiso 1 1 calc R . . C11 C 0.2656(2) 0.39498(8) 0.11069(12) 0.0389(4) Uani 1 1 d . . . H11 H 0.2513 0.3494 0.1092 0.047 Uiso 1 1 calc R . . C12 C 0.4139(4) 0.40495(16) 0.0998(3) 0.1053(15) Uani 1 1 d . . . H12A H 0.4336 0.3825 0.0449 0.158 Uiso 1 1 calc R . . H12B H 0.4736 0.3898 0.1553 0.158 Uiso 1 1 calc R . . H12C H 0.4305 0.4490 0.0920 0.158 Uiso 1 1 calc R . . C13 C 0.1648(5) 0.42077(15) 0.03104(16) 0.1082(15) Uani 1 1 d . . . H13A H 0.1751 0.3991 -0.0266 0.162 Uiso 1 1 calc R . . H13B H 0.1825 0.4648 0.0240 0.162 Uiso 1 1 calc R . . H13C H 0.0713 0.4151 0.0441 0.162 Uiso 1 1 calc R . . C14 C -0.02606(15) 0.32095(7) 0.21950(10) 0.0220(3) Uani 1 1 d . . . C15 C -0.14822(16) 0.28370(7) 0.18321(11) 0.0253(3) Uani 1 1 d . . . C16 C -0.24209(18) 0.26865(9) 0.24185(13) 0.0362(4) Uani 1 1 d . . . H16 H -0.2308 0.2842 0.3036 0.043 Uiso 1 1 calc R . . C17 C -0.35212(19) 0.23081(10) 0.20913(16) 0.0463(5) Uani 1 1 d . . . H17 H -0.4157 0.2199 0.2490 0.056 Uiso 1 1 calc R . . C18 C -0.36972(19) 0.20893(9) 0.11882(17) 0.0458(5) Uani 1 1 d . . . H18 H -0.4455 0.1831 0.0969 0.055 Uiso 1 1 calc R . . C19 C -0.27786(19) 0.22438(9) 0.06047(15) 0.0428(5) Uani 1 1 d . . . H19 H -0.2910 0.2097 -0.0018 0.051 Uiso 1 1 calc R . . C20 C -0.16625(17) 0.26146(7) 0.09276(12) 0.0306(3) Uani 1 1 d . . . H20 H -0.1021 0.2716 0.0529 0.037 Uiso 1 1 calc R . . C21 C 0.14732(16) 0.24054(7) 0.21027(12) 0.0284(3) Uani 1 1 d . . . H21 H 0.1042 0.2273 0.1466 0.034 Uiso 1 1 calc R . . C22 C 0.10316(19) 0.19526(8) 0.28075(15) 0.0385(4) Uani 1 1 d . . . H22A H 0.0032 0.1958 0.2758 0.058 Uiso 1 1 calc R . . H22B H 0.1445 0.2074 0.3438 0.058 Uiso 1 1 calc R . . H22C H 0.1335 0.1536 0.2677 0.058 Uiso 1 1 calc R . . C23 C 0.30168(17) 0.23897(8) 0.21445(13) 0.0339(4) Uani 1 1 d . . . H23A H 0.3308 0.1968 0.2037 0.051 Uiso 1 1 calc R . . H23B H 0.3460 0.2529 0.2759 0.051 Uiso 1 1 calc R . . H23C H 0.3278 0.2662 0.1664 0.051 Uiso 1 1 calc R . . C24 C -0.15200(17) 0.41622(8) 0.25193(12) 0.0309(4) Uani 1 1 d . . . H24 H -0.2325 0.3892 0.2298 0.037 Uiso 1 1 calc R . . C25 C -0.16736(19) 0.43881(9) 0.34910(14) 0.0399(4) Uani 1 1 d . . . H25A H -0.2472 0.4660 0.3450 0.060 Uiso 1 1 calc R . . H25B H -0.0849 0.4615 0.3759 0.060 Uiso 1 1 calc R . . H25C H -0.1798 0.4034 0.3888 0.060 Uiso 1 1 calc R . . C26 C -0.1525(2) 0.46765(9) 0.18153(15) 0.0462(5) Uani 1 1 d . . . H26A H -0.1488 0.4500 0.1200 0.069 Uiso 1 1 calc R . . H26B H -0.0727 0.4942 0.1998 0.069 Uiso 1 1 calc R . . H26C H -0.2364 0.4920 0.1793 0.069 Uiso 1 1 calc R . . C27 C 0.2896(2) 0.39321(8) 0.53916(13) 0.0356(4) Uani 1 1 d . . . C28 C 0.40774(18) 0.37153(9) 0.38686(13) 0.0359(4) Uani 1 1 d . . . C29 C 0.33228(19) 0.27178(8) 0.46094(12) 0.0349(4) Uani 1 1 d . . . C30 C 0.09649(19) 0.32351(8) 0.44179(12) 0.0342(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.02639(14) 0.02299(13) 0.02124(13) 0.00162(8) -0.00094(9) 0.00220(8) Si 0.0192(2) 0.02016(19) 0.0187(2) 0.00082(14) 0.00219(16) 0.00005(14) O1 0.0834(12) 0.0428(7) 0.0346(7) -0.0125(6) -0.0040(7) 0.0096(7) O2 0.0291(7) 0.0900(12) 0.0584(10) 0.0086(9) 0.0064(7) -0.0127(7) O3 0.0711(10) 0.0291(7) 0.0552(9) 0.0019(6) -0.0081(8) 0.0154(7) O4 0.0373(8) 0.0757(10) 0.0444(8) 0.0228(7) 0.0101(6) -0.0110(7) N2 0.0238(6) 0.0207(6) 0.0204(6) 0.0001(5) 0.0021(5) 0.0003(5) N1 0.0286(7) 0.0231(6) 0.0212(6) -0.0011(5) 0.0068(5) -0.0024(5) N4 0.0200(6) 0.0224(6) 0.0230(6) -0.0019(5) 0.0035(5) -0.0010(5) N3 0.0203(6) 0.0234(6) 0.0245(6) -0.0013(5) 0.0027(5) 0.0020(5) C1 0.0248(7) 0.0245(7) 0.0224(7) 0.0019(6) 0.0008(6) -0.0031(6) C2 0.0440(10) 0.0241(8) 0.0250(8) -0.0014(6) 0.0096(7) -0.0082(7) C3 0.0461(11) 0.0345(9) 0.0472(11) -0.0081(8) 0.0193(9) -0.0121(8) C4 0.0738(16) 0.0465(12) 0.0697(15) -0.0217(11) 0.0453(14) -0.0315(12) C5 0.113(2) 0.0343(10) 0.0548(14) 0.0015(10) 0.0463(15) -0.0203(13) C6 0.104(2) 0.0390(11) 0.0486(13) 0.0175(10) 0.0194(13) -0.0057(12) C7 0.0634(13) 0.0356(10) 0.0381(10) 0.0126(8) 0.0055(9) -0.0055(9) C8 0.0320(8) 0.0214(7) 0.0246(7) -0.0034(6) 0.0038(6) 0.0005(6) C9 0.0363(9) 0.0328(8) 0.0308(9) -0.0081(7) 0.0001(7) -0.0051(7) C10 0.0430(10) 0.0274(8) 0.0426(10) -0.0053(7) 0.0038(8) 0.0069(7) C11 0.0618(12) 0.0312(8) 0.0281(9) -0.0069(7) 0.0209(8) -0.0113(8) C12 0.108(2) 0.104(2) 0.129(3) -0.082(2) 0.099(2) -0.064(2) C13 0.215(5) 0.082(2) 0.0208(10) -0.0058(12) -0.0031(17) 0.039(2) C14 0.0221(7) 0.0245(7) 0.0194(7) 0.0016(5) 0.0028(6) -0.0008(6) C15 0.0202(7) 0.0246(7) 0.0295(8) 0.0012(6) -0.0010(6) 0.0001(6) C16 0.0255(8) 0.0464(10) 0.0362(9) 0.0069(8) 0.0035(7) -0.0040(7) C17 0.0231(9) 0.0505(11) 0.0640(14) 0.0191(10) 0.0028(9) -0.0066(8) C18 0.0263(9) 0.0306(9) 0.0744(15) 0.0018(9) -0.0115(9) -0.0060(7) C19 0.0348(10) 0.0359(10) 0.0520(12) -0.0123(8) -0.0115(9) 0.0022(8) C20 0.0268(8) 0.0298(8) 0.0332(9) -0.0034(7) -0.0016(7) 0.0025(6) C21 0.0270(8) 0.0244(7) 0.0326(8) -0.0076(6) 0.0007(7) 0.0026(6) C22 0.0338(9) 0.0237(8) 0.0562(11) 0.0019(7) 0.0016(8) -0.0021(7) C23 0.0278(8) 0.0363(9) 0.0377(9) -0.0060(7) 0.0053(7) 0.0063(7) C24 0.0214(8) 0.0303(8) 0.0396(9) -0.0027(7) 0.0001(7) 0.0054(6) C25 0.0330(9) 0.0397(10) 0.0498(11) -0.0082(8) 0.0155(8) 0.0055(8) C26 0.0428(11) 0.0431(11) 0.0492(11) 0.0081(9) -0.0040(9) 0.0135(8) C27 0.0436(10) 0.0283(8) 0.0325(9) 0.0019(7) -0.0012(8) 0.0058(7) C28 0.0287(9) 0.0408(9) 0.0345(9) 0.0013(7) -0.0060(7) 0.0003(7) C29 0.0399(10) 0.0322(9) 0.0297(9) -0.0017(7) -0.0035(7) 0.0019(7) C30 0.0402(10) 0.0399(9) 0.0223(8) 0.0102(7) 0.0043(7) 0.0013(8) _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 Fe C29 1.7604(18) . ? Fe C30 1.7605(19) . ? Fe C28 1.7655(19) . ? Fe C27 1.7829(18) . ? Fe Si 2.3175(6) . ? Si N1 1.8201(13) . ? Si N3 1.8247(14) . ? Si N2 1.9569(13) . ? Si N4 1.9864(13) . ? Si C1 2.3462(15) . ? Si C14 2.3573(16) . ? O1 C27 1.154(2) . ? O2 C28 1.155(2) . ? O3 C29 1.153(2) . ? O4 C30 1.159(2) . ? N2 C1 1.3182(19) . ? N2 C8 1.4789(18) . ? N1 C1 1.345(2) . ? N1 C11 1.4770(19) . ? N4 C14 1.3149(19) . ? N4 C21 1.4781(19) . ? N3 C14 1.347(2) . ? N3 C24 1.4728(19) . ? C1 C2 1.491(2) . ? C2 C3 1.385(3) . ? C2 C7 1.391(3) . ? C3 C4 1.399(3) . ? C4 C5 1.369(4) . ? C5 C6 1.373(4) . ? C6 C7 1.389(3) . ? C8 C9 1.522(2) . ? C8 C10 1.528(2) . ? C11 C13 1.513(4) . ? C11 C12 1.515(3) . ? C14 C15 1.481(2) . ? C15 C20 1.387(2) . ? C15 C16 1.394(2) . ? C16 C17 1.387(3) . ? C17 C18 1.382(3) . ? C18 C19 1.378(3) . ? C19 C20 1.387(3) . ? C21 C23 1.519(2) . ? C21 C22 1.532(2) . ? C24 C26 1.514(3) . ? C24 C25 1.526(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 C29 Fe C30 93.46(9) . . ? C29 Fe C28 94.06(9) . . ? C30 Fe C28 157.73(8) . . ? C29 Fe C27 111.40(8) . . ? C30 Fe C27 97.46(9) . . ? C28 Fe C27 99.24(9) . . ? C29 Fe Si 125.97(6) . . ? C30 Fe Si 79.11(6) . . ? C28 Fe Si 79.51(6) . . ? C27 Fe Si 122.61(6) . . ? N1 Si N3 109.09(6) . . ? N1 Si N2 69.01(5) . . ? N3 Si N2 97.74(6) . . ? N1 Si N4 94.68(6) . . ? N3 Si N4 68.51(5) . . ? N2 Si N4 154.64(6) . . ? N1 Si Fe 126.71(5) . . ? N3 Si Fe 124.20(5) . . ? N2 Si Fe 102.29(4) . . ? N4 Si Fe 103.05(4) . . ? N1 Si C1 34.86(5) . . ? N3 Si C1 107.37(6) . . ? N2 Si C1 34.18(5) . . ? N4 Si C1 127.52(5) . . ? Fe Si C1 118.24(4) . . ? N1 Si C14 106.03(6) . . ? N3 Si C14 34.70(5) . . ? N2 Si C14 130.14(6) . . ? N4 Si C14 33.89(5) . . ? Fe Si C14 116.58(4) . . ? C1 Si C14 125.18(6) . . ? C1 N2 C8 127.70(13) . . ? C1 N2 Si 89.31(9) . . ? C8 N2 Si 137.00(10) . . ? C1 N1 C11 128.90(13) . . ? C1 N1 Si 94.48(9) . . ? C11 N1 Si 135.20(11) . . ? C14 N4 C21 123.77(13) . . ? C14 N4 Si 88.71(9) . . ? C21 N4 Si 143.50(10) . . ? C14 N3 C24 124.54(13) . . ? C14 N3 Si 94.83(9) . . ? C24 N3 Si 140.45(11) . . ? N2 C1 N1 107.10(12) . . ? N2 C1 C2 128.04(14) . . ? N1 C1 C2 124.85(13) . . ? N2 C1 Si 56.51(7) . . ? N1 C1 Si 50.66(7) . . ? C2 C1 Si 175.30(12) . . ? C3 C2 C7 120.09(17) . . ? C3 C2 C1 121.47(17) . . ? C7 C2 C1 118.42(17) . . ? C2 C3 C4 119.2(2) . . ? C5 C4 C3 120.5(2) . . ? C4 C5 C6 120.21(19) . . ? C5 C6 C7 120.4(2) . . ? C6 C7 C2 119.5(2) . . ? N2 C8 C9 113.10(13) . . ? N2 C8 C10 112.51(13) . . ? C9 C8 C10 111.02(14) . . ? N1 C11 C13 112.22(19) . . ? N1 C11 C12 112.38(18) . . ? C13 C11 C12 113.6(3) . . ? N4 C14 N3 107.69(13) . . ? N4 C14 C15 126.96(14) . . ? N3 C14 C15 125.29(13) . . ? N4 C14 Si 57.40(8) . . ? N3 C14 Si 50.47(7) . . ? C15 C14 Si 172.79(11) . . ? C20 C15 C16 120.00(16) . . ? C20 C15 C14 120.32(14) . . ? C16 C15 C14 119.61(15) . . ? C17 C16 C15 119.38(18) . . ? C18 C17 C16 120.34(17) . . ? C19 C18 C17 120.31(17) . . ? C18 C19 C20 119.93(18) . . ? C15 C20 C19 120.03(16) . . ? N4 C21 C23 109.61(13) . . ? N4 C21 C22 112.32(13) . . ? C23 C21 C22 110.41(14) . . ? N3 C24 C26 111.35(14) . . ? N3 C24 C25 109.98(14) . . ? C26 C24 C25 113.54(15) . . ? O1 C27 Fe 176.17(16) . . ? O2 C28 Fe 178.29(18) . . ? O3 C29 Fe 178.76(18) . . ? O4 C30 Fe 177.13(17) . . ? 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 C29 Fe Si N1 -87.96(9) . . . . ? C30 Fe Si N1 -174.30(8) . . . . ? C28 Fe Si N1 -0.56(8) . . . . ? C27 Fe Si N1 93.76(9) . . . . ? C29 Fe Si N3 90.85(9) . . . . ? C30 Fe Si N3 4.51(8) . . . . ? C28 Fe Si N3 178.25(8) . . . . ? C27 Fe Si N3 -87.43(9) . . . . ? C29 Fe Si N2 -160.81(8) . . . . ? C30 Fe Si N2 112.85(7) . . . . ? C28 Fe Si N2 -73.41(7) . . . . ? C27 Fe Si N2 20.91(9) . . . . ? C29 Fe Si N4 18.14(9) . . . . ? C30 Fe Si N4 -68.20(7) . . . . ? C28 Fe Si N4 105.54(7) . . . . ? C27 Fe Si N4 -160.14(8) . . . . ? C29 Fe Si C1 -128.38(9) . . . . ? C30 Fe Si C1 145.28(8) . . . . ? C28 Fe Si C1 -40.98(8) . . . . ? C27 Fe Si C1 53.34(9) . . . . ? C29 Fe Si C14 51.33(9) . . . . ? C30 Fe Si C14 -35.01(7) . . . . ? C28 Fe Si C14 138.74(8) . . . . ? C27 Fe Si C14 -126.95(9) . . . . ? N1 Si N2 C1 -2.11(9) . . . . ? N3 Si N2 C1 -109.64(10) . . . . ? N4 Si N2 C1 -54.85(16) . . . . ? Fe Si N2 C1 122.76(9) . . . . ? C14 Si N2 C1 -95.73(10) . . . . ? N1 Si N2 C8 -154.21(16) . . . . ? N3 Si N2 C8 98.25(15) . . . . ? N4 Si N2 C8 153.05(14) . . . . ? Fe Si N2 C8 -29.35(15) . . . . ? C1 Si N2 C8 -152.1(2) . . . . ? C14 Si N2 C8 112.16(15) . . . . ? N3 Si N1 C1 93.21(10) . . . . ? N2 Si N1 C1 2.07(9) . . . . ? N4 Si N1 C1 162.07(10) . . . . ? Fe Si N1 C1 -87.83(10) . . . . ? C14 Si N1 C1 129.53(10) . . . . ? N3 Si N1 C11 -73.40(18) . . . . ? N2 Si N1 C11 -164.54(19) . . . . ? N4 Si N1 C11 -4.54(18) . . . . ? Fe Si N1 C11 105.56(17) . . . . ? C1 Si N1 C11 -166.6(2) . . . . ? C14 Si N1 C11 -37.08(18) . . . . ? N1 Si N4 C14 -112.02(9) . . . . ? N3 Si N4 C14 -3.33(8) . . . . ? N2 Si N4 C14 -63.81(15) . . . . ? Fe Si N4 C14 118.59(8) . . . . ? C1 Si N4 C14 -99.20(10) . . . . ? N1 Si N4 C21 93.26(17) . . . . ? N3 Si N4 C21 -158.06(18) . . . . ? N2 Si N4 C21 141.47(16) . . . . ? Fe Si N4 C21 -36.13(17) . . . . ? C1 Si N4 C21 106.08(17) . . . . ? C14 Si N4 C21 -154.7(2) . . . . ? N1 Si N3 C14 90.78(10) . . . . ? N2 Si N3 C14 161.17(9) . . . . ? N4 Si N3 C14 3.27(8) . . . . ? Fe Si N3 C14 -88.22(9) . . . . ? C1 Si N3 C14 127.50(9) . . . . ? N1 Si N3 C24 -83.97(17) . . . . ? N2 Si N3 C24 -13.58(17) . . . . ? N4 Si N3 C24 -171.48(18) . . . . ? Fe Si N3 C24 97.03(16) . . . . ? C1 Si N3 C24 -47.25(17) . . . . ? C14 Si N3 C24 -174.8(2) . . . . ? C8 N2 C1 N1 159.00(14) . . . . ? Si N2 C1 N1 2.79(12) . . . . ? C8 N2 C1 C2 -22.3(3) . . . . ? Si N2 C1 C2 -178.54(16) . . . . ? C8 N2 C1 Si 156.21(17) . . . . ? C11 N1 C1 N2 164.89(16) . . . . ? Si N1 C1 N2 -3.00(13) . . . . ? C11 N1 C1 C2 -13.8(3) . . . . ? Si N1 C1 C2 178.26(15) . . . . ? C11 N1 C1 Si 167.9(2) . . . . ? N1 Si C1 N2 176.56(15) . . . . ? N3 Si C1 N2 77.91(10) . . . . ? N4 Si C1 N2 153.79(9) . . . . ? Fe Si C1 N2 -68.86(10) . . . . ? C14 Si C1 N2 111.46(10) . . . . ? N3 Si C1 N1 -98.65(11) . . . . ? N2 Si C1 N1 -176.56(15) . . . . ? N4 Si C1 N1 -22.76(12) . . . . ? Fe Si C1 N1 114.58(9) . . . . ? C14 Si C1 N1 -65.10(11) . . . . ? N1 Si C1 C2 -17.7(15) . . . . ? N3 Si C1 C2 -116.3(15) . . . . ? N2 Si C1 C2 165.8(16) . . . . ? N4 Si C1 C2 -40.4(16) . . . . ? Fe Si C1 C2 96.9(15) . . . . ? C14 Si C1 C2 -82.8(15) . . . . ? N2 C1 C2 C3 104.4(2) . . . . ? N1 C1 C2 C3 -77.2(2) . . . . ? Si C1 C2 C3 -60.6(16) . . . . ? N2 C1 C2 C7 -77.2(2) . . . . ? N1 C1 C2 C7 101.2(2) . . . . ? Si C1 C2 C7 117.9(15) . . . . ? C7 C2 C3 C4 -1.6(3) . . . . ? C1 C2 C3 C4 176.83(16) . . . . ? C2 C3 C4 C5 -0.4(3) . . . . ? C3 C4 C5 C6 1.7(3) . . . . ? C4 C5 C6 C7 -0.9(4) . . . . ? C5 C6 C7 C2 -1.1(3) . . . . ? C3 C2 C7 C6 2.4(3) . . . . ? C1 C2 C7 C6 -176.09(18) . . . . ? C1 N2 C8 C9 -47.8(2) . . . . ? Si N2 C8 C9 95.92(17) . . . . ? C1 N2 C8 C10 79.0(2) . . . . ? Si N2 C8 C10 -137.29(14) . . . . ? C1 N1 C11 C13 -60.7(3) . . . . ? Si N1 C11 C13 102.0(2) . . . . ? C1 N1 C11 C12 68.7(3) . . . . ? Si N1 C11 C12 -128.5(2) . . . . ? C21 N4 C14 N3 166.62(13) . . . . ? Si N4 C14 N3 4.41(11) . . . . ? C21 N4 C14 C15 -10.8(2) . . . . ? Si N4 C14 C15 -173.00(14) . . . . ? C21 N4 C14 Si 162.21(15) . . . . ? C24 N3 C14 N4 171.12(13) . . . . ? Si N3 C14 N4 -4.82(12) . . . . ? C24 N3 C14 C15 -11.4(2) . . . . ? Si N3 C14 C15 172.65(13) . . . . ? C24 N3 C14 Si 175.94(17) . . . . ? N1 Si C14 N4 74.02(9) . . . . ? N3 Si C14 N4 174.55(14) . . . . ? N2 Si C14 N4 149.81(9) . . . . ? Fe Si C14 N4 -73.03(9) . . . . ? C1 Si C14 N4 106.66(10) . . . . ? N1 Si C14 N3 -100.53(10) . . . . ? N2 Si C14 N3 -24.73(11) . . . . ? N4 Si C14 N3 -174.55(14) . . . . ? Fe Si C14 N3 112.43(9) . . . . ? C1 Si C14 N3 -67.88(11) . . . . ? N1 Si C14 C15 -156.8(9) . . . . ? N3 Si C14 C15 -56.3(9) . . . . ? N2 Si C14 C15 -81.0(9) . . . . ? N4 Si C14 C15 129.1(9) . . . . ? Fe Si C14 C15 56.1(9) . . . . ? C1 Si C14 C15 -124.2(9) . . . . ? N4 C14 C15 C20 -58.5(2) . . . . ? N3 C14 C15 C20 124.51(17) . . . . ? Si C14 C15 C20 176.4(8) . . . . ? N4 C14 C15 C16 118.55(18) . . . . ? N3 C14 C15 C16 -58.4(2) . . . . ? Si C14 C15 C16 -6.6(10) . . . . ? C20 C15 C16 C17 0.7(3) . . . . ? C14 C15 C16 C17 -176.31(16) . . . . ? C15 C16 C17 C18 -0.9(3) . . . . ? C16 C17 C18 C19 0.2(3) . . . . ? C17 C18 C19 C20 0.8(3) . . . . ? C16 C15 C20 C19 0.2(3) . . . . ? C14 C15 C20 C19 177.22(16) . . . . ? C18 C19 C20 C15 -1.0(3) . . . . ? C14 N4 C21 C23 175.46(14) . . . . ? Si N4 C21 C23 -35.4(2) . . . . ? C14 N4 C21 C22 -61.4(2) . . . . ? Si N4 C21 C22 87.70(19) . . . . ? C14 N3 C24 C26 -104.75(18) . . . . ? Si N3 C24 C26 68.9(2) . . . . ? C14 N3 C24 C25 128.49(16) . . . . ? Si N3 C24 C25 -57.9(2) . . . . ? C29 Fe C27 O1 -6(3) . . . . ? C30 Fe C27 O1 91(3) . . . . ? C28 Fe C27 O1 -104(3) . . . . ? Si Fe C27 O1 173(3) . . . . ? C29 Fe C28 O2 -37(7) . . . . ? C30 Fe C28 O2 -147(7) . . . . ? C27 Fe C28 O2 75(7) . . . . ? Si Fe C28 O2 -163(7) . . . . ? C30 Fe C29 O3 13(8) . . . . ? C28 Fe C29 O3 -146(8) . . . . ? C27 Fe C29 O3 112(8) . . . . ? Si Fe C29 O3 -66(8) . . . . ? C29 Fe C30 O4 -12(3) . . . . ? C28 Fe C30 O4 98(3) . . . . ? C27 Fe C30 O4 -124(3) . . . . ? Si Fe C30 O4 114(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.416 _refine_diff_density_min -0.527 _refine_diff_density_rms 0.114