Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_GLOBAL _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 # 1. SUBMISSION DETAILS _publ_contact_author_name 'Rolf Gleiter' _publ_contact_author_address ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 D-69120 Heidelberg Germany ; _publ_contact_author_phone '049 6221 54- 8400' _publ_contact_author_fax '049 6221 54- 4205' _publ_contact_author_email rolf.gleiter@urz.uni-heidelberg.de _publ_requested_coeditor_name ? _publ_contact_letter ; paper to be submitted for publication Dalton Transactions ; #========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A stepwise degradation of sterically hindered CpCo-cyclobutadiene complexes ; loop_ _publ_author_name _publ_author_address C.Schaefer ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; F.Rominger ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; R.Gleiter ; Organisch-Chemisches Institut Universitat Heidelberg Im Neuenheimer Feld 270 69120 Heidelberg Bundesrepublik Deutschland ; #======================================================================= data_cs4 _database_code_depnum_ccdc_archive 'CCDC 243854' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CS4 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H41 Co O4 Si2' _chemical_formula_weight 520.69 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.33360(10) _cell_length_b 13.78110(10) _cell_length_c 20.92110(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2691.02(4) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max .40 _exptl_crystal_size_mid .16 _exptl_crystal_size_min .12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.754 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27697 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0373 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 27.45 _reflns_number_total 6158 _reflns_number_gt 5518 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(9) _refine_ls_number_reflns 6158 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0660 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.150 _refine_ls_shift/su_mean 0.010 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 Co1 Co 0.93133(3) 0.892980(17) 0.892099(11) 0.02134(7) Uani 1 1 d . . . Si1 Si 1.02571(6) 1.04253(4) 1.05861(3) 0.02758(13) Uani 1 1 d . . . Si2 Si 0.94724(6) 0.92450(4) 0.69075(2) 0.02709(12) Uani 1 1 d . . . C1 C 0.8314(3) 0.76944(16) 0.85832(12) 0.0450(6) Uani 1 1 d . . . H1 H 0.8029 0.7593 0.8152 0.054 Uiso 1 1 calc R . . C2 C 0.7482(3) 0.81224(17) 0.90664(12) 0.0417(6) Uani 1 1 d . . . H2 H 0.6531 0.8358 0.9019 0.050 Uiso 1 1 calc R . . C3 C 0.8288(3) 0.81424(16) 0.96276(11) 0.0403(6) Uani 1 1 d . . . H3 H 0.7986 0.8397 1.0027 0.048 Uiso 1 1 calc R . . C4 C 0.9630(3) 0.77177(15) 0.94969(13) 0.0450(6) Uani 1 1 d . . . H4 H 1.0389 0.7634 0.9794 0.054 Uiso 1 1 calc R . . C5 C 0.9653(3) 0.74407(15) 0.88523(14) 0.0501(7) Uani 1 1 d . . . H5 H 1.0427 0.7138 0.8635 0.060 Uiso 1 1 calc R . . C6 C 1.0583(2) 0.97334(12) 0.83771(8) 0.0191(3) Uani 1 1 d . . . C7 C 1.0753(2) 0.99757(12) 0.90595(8) 0.0183(3) Uani 1 1 d . . . C8 C 1.2025(2) 1.01063(14) 0.95043(9) 0.0237(4) Uani 1 1 d . . . C9 C 1.2799(2) 0.91722(15) 0.96923(10) 0.0337(5) Uani 1 1 d . . . H9A H 1.2188 0.8791 0.9979 0.051 Uiso 1 1 calc R . . H9B H 1.3696 0.9334 0.9911 0.051 Uiso 1 1 calc R . . H9C H 1.3011 0.8793 0.9308 0.051 Uiso 1 1 calc R . . C10 C 1.3072(2) 1.08272(15) 0.92068(10) 0.0285(4) Uani 1 1 d . . . H10A H 1.3798 1.1009 0.9523 0.043 Uiso 1 1 calc R . . H10B H 1.2551 1.1408 0.9069 0.043 Uiso 1 1 calc R . . H10C H 1.3540 1.0528 0.8837 0.043 Uiso 1 1 calc R . . O11 O 1.15832(14) 1.05771(10) 1.00873(6) 0.0274(3) Uani 1 1 d . . . C12 C 1.0225(3) 0.92490(17) 1.10172(11) 0.0449(6) Uani 1 1 d . . . H12A H 1.1139 0.9154 1.1240 0.067 Uiso 1 1 calc R . . H12B H 1.0078 0.8721 1.0711 0.067 Uiso 1 1 calc R . . H12C H 0.9442 0.9251 1.1329 0.067 Uiso 1 1 calc R . . C13 C 1.0511(3) 1.14362(17) 1.11661(10) 0.0394(5) Uani 1 1 d . . . H13A H 1.0265 1.2053 1.0960 0.059 Uiso 1 1 calc R . . H13B H 1.1512 1.1453 1.1306 0.059 Uiso 1 1 calc R . . H13C H 0.9887 1.1334 1.1537 0.059 Uiso 1 1 calc R . . O14 O 0.87338(14) 1.04891(11) 1.01988(6) 0.0286(3) Uani 1 1 d . . . C15 C 0.8460(2) 1.09071(14) 0.95767(9) 0.0235(4) Uani 1 1 d . . . C16 C 0.6830(2) 1.08419(16) 0.95022(10) 0.0306(5) Uani 1 1 d . . . H16A H 0.6366 1.1175 0.9861 0.046 Uiso 1 1 calc R . . H16B H 0.6537 1.0159 0.9499 0.046 Uiso 1 1 calc R . . H16C H 0.6543 1.1150 0.9100 0.046 Uiso 1 1 calc R . . C17 C 0.8935(2) 1.19780(14) 0.95694(10) 0.0307(5) Uani 1 1 d . . . H17A H 0.9973 1.2015 0.9634 0.046 Uiso 1 1 calc R . . H17B H 0.8446 1.2330 0.9913 0.046 Uiso 1 1 calc R . . H17C H 0.8686 1.2270 0.9157 0.046 Uiso 1 1 calc R . . C18 C 0.9273(2) 1.03462(12) 0.90722(8) 0.0192(3) Uani 1 1 d . . . C19 C 0.9110(2) 1.01120(12) 0.83843(8) 0.0186(4) Uani 1 1 d . . . C20 C 0.8069(2) 1.03899(14) 0.78572(9) 0.0229(4) Uani 1 1 d . . . C21 C 0.6596(2) 0.98912(16) 0.79120(10) 0.0330(5) Uani 1 1 d . . . H21A H 0.6713 0.9189 0.7862 0.049 Uiso 1 1 calc R . . H21B H 0.5960 1.0137 0.7576 0.049 Uiso 1 1 calc R . . H21C H 0.6179 1.0031 0.8332 0.049 Uiso 1 1 calc R . . C22 C 0.7883(3) 1.14936(15) 0.78361(10) 0.0321(5) Uani 1 1 d . . . H22A H 0.7283 1.1670 0.7470 0.048 Uiso 1 1 calc R . . H22B H 0.8824 1.1803 0.7794 0.048 Uiso 1 1 calc R . . H22C H 0.7423 1.1714 0.8231 0.048 Uiso 1 1 calc R . . O23 O 0.86453(16) 1.01592(10) 0.72376(6) 0.0286(3) Uani 1 1 d . . . C24 C 0.8344(3) 0.81587(17) 0.67400(11) 0.0399(5) Uani 1 1 d . . . H24A H 0.7683 0.8303 0.6389 0.060 Uiso 1 1 calc R . . H24B H 0.7796 0.7989 0.7123 0.060 Uiso 1 1 calc R . . H24C H 0.8961 0.7613 0.6620 0.060 Uiso 1 1 calc R . . C25 C 1.0154(3) 0.97348(17) 0.61407(10) 0.0406(5) Uani 1 1 d . . . H25A H 1.0758 1.0302 0.6225 0.061 Uiso 1 1 calc R . . H25B H 0.9345 0.9925 0.5870 0.061 Uiso 1 1 calc R . . H25C H 1.0720 0.9236 0.5922 0.061 Uiso 1 1 calc R . . O26 O 1.07446(15) 0.88617(9) 0.73850(6) 0.0261(3) Uani 1 1 d . . . C27 C 1.1559(2) 0.94367(14) 0.78325(9) 0.0238(4) Uani 1 1 d . . . C28 C 1.2802(2) 0.87866(15) 0.80339(10) 0.0307(5) Uani 1 1 d . . . H28A H 1.3334 0.8578 0.7654 0.046 Uiso 1 1 calc R . . H28B H 1.2429 0.8216 0.8258 0.046 Uiso 1 1 calc R . . H28C H 1.3443 0.9148 0.8319 0.046 Uiso 1 1 calc R . . C29 C 1.2139(2) 1.03533(16) 0.75010(10) 0.0321(5) Uani 1 1 d . . . H29A H 1.1337 1.0772 0.7377 0.048 Uiso 1 1 calc R . . H29B H 1.2683 1.0166 0.7119 0.048 Uiso 1 1 calc R . . H29C H 1.2768 1.0705 0.7796 0.048 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 Co1 0.02226(12) 0.01679(11) 0.02497(12) 0.00236(10) -0.00091(11) -0.00367(11) Si1 0.0280(3) 0.0334(3) 0.0213(3) -0.0016(2) -0.0030(2) 0.0005(2) Si2 0.0292(3) 0.0288(3) 0.0232(2) -0.0049(2) -0.0023(2) 0.0012(2) C1 0.0673(18) 0.0274(11) 0.0404(13) -0.0011(10) -0.0052(13) -0.0211(12) C2 0.0346(12) 0.0328(12) 0.0577(15) 0.0105(11) -0.0018(11) -0.0181(10) C3 0.0513(15) 0.0324(12) 0.0373(12) 0.0121(10) 0.0079(11) -0.0176(11) C4 0.0493(16) 0.0251(11) 0.0607(16) 0.0209(11) -0.0133(12) -0.0098(10) C5 0.0618(18) 0.0165(10) 0.0721(18) 0.0025(11) 0.0222(15) -0.0010(10) C6 0.0195(9) 0.0145(8) 0.0233(8) 0.0008(6) -0.0001(8) -0.0016(8) C7 0.0166(8) 0.0157(7) 0.0226(8) 0.0003(6) -0.0004(8) -0.0008(7) C8 0.0208(10) 0.0242(10) 0.0260(10) -0.0034(8) -0.0028(8) 0.0037(8) C9 0.0328(11) 0.0325(12) 0.0359(11) -0.0016(9) -0.0107(9) 0.0097(9) C10 0.0170(9) 0.0317(11) 0.0367(10) -0.0070(8) -0.0018(8) -0.0034(8) O11 0.0239(7) 0.0342(8) 0.0240(7) -0.0076(6) -0.0037(5) 0.0013(6) C12 0.0601(16) 0.0441(13) 0.0305(11) 0.0065(10) -0.0093(11) -0.0041(11) C13 0.0381(13) 0.0502(13) 0.0298(11) -0.0103(9) -0.0037(10) 0.0022(11) O14 0.0252(7) 0.0409(8) 0.0198(6) 0.0028(6) 0.0011(5) -0.0030(6) C15 0.0206(9) 0.0273(10) 0.0226(9) -0.0002(8) 0.0019(7) -0.0005(8) C16 0.0192(9) 0.0422(13) 0.0303(10) -0.0007(9) 0.0021(8) 0.0041(9) C17 0.0338(12) 0.0235(10) 0.0349(11) -0.0057(8) 0.0028(9) 0.0032(8) C18 0.0181(8) 0.0163(8) 0.0233(8) 0.0011(6) -0.0020(8) -0.0023(8) C19 0.0192(10) 0.0154(8) 0.0212(8) 0.0006(6) 0.0005(7) -0.0013(7) C20 0.0230(9) 0.0255(10) 0.0203(9) -0.0010(7) -0.0025(7) 0.0020(8) C21 0.0212(10) 0.0436(13) 0.0341(11) 0.0025(9) -0.0061(9) -0.0024(9) C22 0.0369(12) 0.0282(11) 0.0312(11) 0.0030(9) -0.0029(9) 0.0096(10) O23 0.0322(8) 0.0321(8) 0.0215(7) -0.0024(6) -0.0030(6) 0.0059(6) C24 0.0360(13) 0.0415(13) 0.0422(13) -0.0128(10) -0.0092(10) -0.0029(11) C25 0.0518(14) 0.0413(13) 0.0286(11) -0.0027(10) -0.0015(11) 0.0039(11) O26 0.0279(7) 0.0251(6) 0.0254(6) -0.0070(5) -0.0028(6) 0.0009(7) C27 0.0214(9) 0.0246(10) 0.0255(9) -0.0060(8) -0.0012(8) -0.0001(8) C28 0.0235(10) 0.0336(12) 0.0349(11) -0.0108(9) -0.0013(8) 0.0053(9) C29 0.0301(11) 0.0358(12) 0.0303(10) -0.0018(9) 0.0075(9) -0.0066(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C18 1.9778(17) . ? Co1 C6 1.9813(18) . ? Co1 C19 1.9877(17) . ? Co1 C7 1.9918(18) . ? Co1 C2 2.062(2) . ? Co1 C1 2.066(2) . ? Co1 C3 2.068(2) . ? Co1 C4 2.081(2) . ? Co1 C5 2.081(2) . ? Si1 O11 1.6324(15) . ? Si1 O14 1.6388(15) . ? Si1 C12 1.855(2) . ? Si1 C13 1.863(2) . ? Si2 O23 1.6309(14) . ? Si2 O26 1.6391(14) . ? Si2 C25 1.853(2) . ? Si2 C24 1.863(2) . ? C1 C2 1.405(4) . ? C1 C5 1.414(4) . ? C2 C3 1.395(3) . ? C3 C4 1.409(4) . ? C4 C5 1.402(4) . ? C6 C19 1.471(3) . ? C6 C7 1.475(2) . ? C6 C27 1.515(3) . ? C7 C18 1.473(3) . ? C7 C8 1.519(3) . ? C8 O11 1.442(2) . ? C8 C10 1.526(3) . ? C8 C9 1.528(3) . ? O14 C15 1.446(2) . ? C15 C18 1.513(2) . ? C15 C16 1.532(3) . ? C15 C17 1.541(3) . ? C18 C19 1.483(2) . ? C19 C20 1.519(2) . ? C20 O23 1.439(2) . ? C20 C22 1.532(3) . ? C20 C21 1.541(3) . ? O26 C27 1.443(2) . ? C27 C28 1.526(3) . ? C27 C29 1.540(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 C18 Co1 C6 63.35(7) . . ? C18 Co1 C19 43.91(7) . . ? C6 Co1 C19 43.50(7) . . ? C18 Co1 C7 43.55(8) . . ? C6 Co1 C7 43.58(7) . . ? C19 Co1 C7 63.49(7) . . ? C18 Co1 C2 119.56(9) . . ? C6 Co1 C2 151.89(8) . . ? C19 Co1 C2 116.51(9) . . ? C7 Co1 C2 158.16(9) . . ? C18 Co1 C1 149.27(10) . . ? C6 Co1 C1 122.29(9) . . ? C19 Co1 C1 116.05(9) . . ? C7 Co1 C1 161.93(10) . . ? C2 Co1 C1 39.79(10) . . ? C18 Co1 C3 113.25(9) . . ? C6 Co1 C3 168.63(9) . . ? C19 Co1 C3 142.14(9) . . ? C7 Co1 C3 125.99(8) . . ? C2 Co1 C3 39.48(9) . . ? C1 Co1 C3 66.63(10) . . ? C18 Co1 C4 134.62(9) . . ? C6 Co1 C4 134.12(10) . . ? C19 Co1 C4 177.04(9) . . ? C7 Co1 C4 113.62(9) . . ? C2 Co1 C4 66.38(10) . . ? C1 Co1 C4 66.46(10) . . ? C3 Co1 C4 39.71(11) . . ? C18 Co1 C5 170.74(10) . . ? C6 Co1 C5 114.85(9) . . ? C19 Co1 C5 141.59(10) . . ? C7 Co1 C5 128.37(10) . . ? C2 Co1 C5 66.70(11) . . ? C1 Co1 C5 39.88(11) . . ? C3 Co1 C5 66.58(10) . . ? C4 Co1 C5 39.36(10) . . ? O11 Si1 O14 109.56(7) . . ? O11 Si1 C12 115.78(10) . . ? O14 Si1 C12 105.86(10) . . ? O11 Si1 C13 102.96(9) . . ? O14 Si1 C13 113.09(10) . . ? C12 Si1 C13 109.81(11) . . ? O23 Si2 O26 109.50(7) . . ? O23 Si2 C25 104.34(9) . . ? O26 Si2 C25 113.34(10) . . ? O23 Si2 C24 115.64(10) . . ? O26 Si2 C24 105.37(9) . . ? C25 Si2 C24 108.90(11) . . ? C2 C1 C5 107.8(2) . . ? C2 C1 Co1 69.97(12) . . ? C5 C1 Co1 70.65(13) . . ? C3 C2 C1 108.4(2) . . ? C3 C2 Co1 70.49(13) . . ? C1 C2 Co1 70.24(14) . . ? C2 C3 C4 107.9(2) . . ? C2 C3 Co1 70.03(13) . . ? C4 C3 Co1 70.61(13) . . ? C5 C4 C3 108.2(2) . . ? C5 C4 Co1 70.35(13) . . ? C3 C4 Co1 69.67(12) . . ? C4 C5 C1 107.6(2) . . ? C4 C5 Co1 70.29(13) . . ? C1 C5 Co1 69.47(13) . . ? C19 C6 C7 90.60(14) . . ? C19 C6 C27 131.72(16) . . ? C7 C6 C27 136.42(17) . . ? C19 C6 Co1 68.48(10) . . ? C7 C6 Co1 68.59(10) . . ? C27 C6 Co1 129.85(12) . . ? C18 C7 C6 89.71(14) . . ? C18 C7 C8 132.91(15) . . ? C6 C7 C8 134.74(17) . . ? C18 C7 Co1 67.71(10) . . ? C6 C7 Co1 67.83(10) . . ? C8 C7 Co1 134.60(13) . . ? O11 C8 C7 110.35(15) . . ? O11 C8 C10 103.60(15) . . ? C7 C8 C10 109.14(15) . . ? O11 C8 C9 107.25(16) . . ? C7 C8 C9 115.32(16) . . ? C10 C8 C9 110.53(16) . . ? C8 O11 Si1 134.43(12) . . ? C15 O14 Si1 128.29(12) . . ? O14 C15 C18 109.62(15) . . ? O14 C15 C16 104.10(15) . . ? C18 C15 C16 113.42(16) . . ? O14 C15 C17 109.86(15) . . ? C18 C15 C17 109.77(15) . . ? C16 C15 C17 109.91(16) . . ? C7 C18 C19 90.21(14) . . ? C7 C18 C15 131.33(15) . . ? C19 C18 C15 137.47(17) . . ? C7 C18 Co1 68.73(9) . . ? C19 C18 Co1 68.40(9) . . ? C15 C18 Co1 128.72(13) . . ? C6 C19 C18 89.48(14) . . ? C6 C19 C20 132.85(16) . . ? C18 C19 C20 135.70(16) . . ? C6 C19 Co1 68.02(9) . . ? C18 C19 Co1 67.68(9) . . ? C20 C19 Co1 132.68(13) . . ? O23 C20 C19 111.05(15) . . ? O23 C20 C22 103.64(16) . . ? C19 C20 C22 110.11(16) . . ? O23 C20 C21 107.57(16) . . ? C19 C20 C21 113.84(16) . . ? C22 C20 C21 110.12(17) . . ? C20 O23 Si2 136.80(12) . . ? C27 O26 Si2 126.87(12) . . ? O26 C27 C6 108.63(15) . . ? O26 C27 C28 104.91(15) . . ? C6 C27 C28 114.09(15) . . ? O26 C27 C29 110.11(15) . . ? C6 C27 C29 109.21(15) . . ? C28 C27 C29 109.79(17) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.244 _refine_diff_density_min -0.288 _refine_diff_density_rms 0.054 #===END data_cs32 _database_code_depnum_ccdc_archive 'CCDC 243855' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common CS32 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H53 Co O4 Si2' _chemical_formula_weight 893.08 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 16.61470(10) _cell_length_b 11.0728(2) _cell_length_c 24.7178(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.2880(10) _cell_angle_gamma 90.00 _cell_volume 4499.87(11) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour yellow _exptl_crystal_size_max .40 _exptl_crystal_size_mid .27 _exptl_crystal_size_min .20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; the phenyl group with c41 is disordered over two positions with nearly equal occupancy ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45831 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.24 _diffrn_reflns_theta_max 27.47 _reflns_number_total 10303 _reflns_number_gt 7328 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^2^+1.5271P] 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 10303 _refine_ls_number_parameters 596 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1194 _refine_ls_wR_factor_gt 0.1007 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.016 _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 Co1 Co 1.345301(16) 0.91747(2) 0.116752(11) 0.02500(9) Uani 1 1 d . . . Si1 Si 1.11195(3) 0.81409(5) 0.12846(3) 0.02912(14) Uani 1 1 d U . . Si2 Si 1.57986(3) 0.79734(6) 0.10272(2) 0.03131(15) Uani 1 1 d . . . O1 O 1.18463(9) 0.80980(15) 0.17963(6) 0.0378(4) Uani 1 1 d . A . O2 O 1.14210(9) 0.77450(17) 0.07186(6) 0.0409(4) Uani 1 1 d . A . O3 O 1.50497(8) 0.83566(14) 0.05601(6) 0.0313(3) Uani 1 1 d . . . O4 O 1.54351(8) 0.71333(14) 0.14762(6) 0.0310(3) Uani 1 1 d . . . C1 C 1.41673(16) 1.0679(2) 0.14401(12) 0.0453(6) Uani 1 1 d . . . H1 H 1.4677 1.0652 0.1670 0.054 Uiso 1 1 calc R . . C2 C 1.3416(2) 1.0766(2) 0.16157(13) 0.0575(8) Uani 1 1 d . . . H2 H 1.3319 1.0806 0.1985 0.069 Uiso 1 1 calc R . . C3 C 1.28175(16) 1.0787(2) 0.11466(17) 0.0637(10) Uani 1 1 d . . . H3 H 1.2246 1.0846 0.1141 0.076 Uiso 1 1 calc R . . C4 C 1.32304(19) 1.0703(2) 0.06890(13) 0.0543(8) Uani 1 1 d . . . H4 H 1.2986 1.0694 0.0317 0.065 Uiso 1 1 calc R . . C5 C 1.40560(16) 1.0637(2) 0.08769(12) 0.0463(6) Uani 1 1 d . . . H5 H 1.4475 1.0574 0.0655 0.056 Uiso 1 1 calc R . . C6 C 1.39860(12) 0.76066(17) 0.14181(8) 0.0213(4) Uani 1 1 d . . . C7 C 1.31123(11) 0.76149(17) 0.14762(7) 0.0206(4) Uani 1 1 d . A . C8 C 1.29005(11) 0.76711(17) 0.08744(7) 0.0220(4) Uani 1 1 d . A . C9 C 1.37783(11) 0.76886(18) 0.08234(8) 0.0225(4) Uani 1 1 d . . . C10 C 1.25832(12) 0.74229(19) 0.19337(8) 0.0268(4) Uani 1 1 d . . . C11 C 1.21218(12) 0.7327(2) 0.04984(8) 0.0283(5) Uani 1 1 d . . . C12 C 1.43200(12) 0.7676(2) 0.03713(8) 0.0313(5) Uani 1 1 d . . . C13 C 1.39592(14) 0.8328(3) -0.01505(9) 0.0471(7) Uani 1 1 d . . . H13A H 1.3778 0.9136 -0.0059 0.071 Uiso 1 1 calc R . . H13B H 1.3495 0.7868 -0.0334 0.071 Uiso 1 1 calc R . . H13C H 1.4373 0.8401 -0.0394 0.071 Uiso 1 1 calc R . . C14 C 1.45418(15) 0.6384(2) 0.02310(11) 0.0472(6) Uani 1 1 d . . . H14A H 1.4951 0.6403 -0.0018 0.071 Uiso 1 1 calc R . . H14B H 1.4054 0.5965 0.0054 0.071 Uiso 1 1 calc R . . H14C H 1.4762 0.5956 0.0567 0.071 Uiso 1 1 calc R . . C15 C 1.62917(15) 0.9374(2) 0.13095(11) 0.0470(6) Uani 1 1 d . . . H15A H 1.5879 0.9923 0.1416 0.071 Uiso 1 1 calc R . . H15B H 1.6569 0.9763 0.1032 0.071 Uiso 1 1 calc R . . H15C H 1.6689 0.9180 0.1631 0.071 Uiso 1 1 calc R . . C16 C 1.65644(15) 0.7030(3) 0.07492(12) 0.0528(7) Uani 1 1 d . . . H16A H 1.7030 0.6893 0.1034 0.079 Uiso 1 1 calc R . . H16B H 1.6748 0.7446 0.0439 0.079 Uiso 1 1 calc R . . H16C H 1.6320 0.6253 0.0627 0.079 Uiso 1 1 calc R . . C17 C 1.47721(12) 0.72715(19) 0.17914(8) 0.0258(4) Uani 1 1 d . . . C18 C 1.50266(14) 0.8185(2) 0.22455(9) 0.0343(5) Uani 1 1 d . . . H18A H 1.5508 0.7886 0.2484 0.051 Uiso 1 1 calc R . . H18B H 1.4581 0.8300 0.2460 0.051 Uiso 1 1 calc R . . H18C H 1.5155 0.8958 0.2084 0.051 Uiso 1 1 calc R . . C19 C 1.47039(14) 0.6010(2) 0.20238(9) 0.0340(5) Uani 1 1 d . . . H19A H 1.4568 0.5434 0.1724 0.051 Uiso 1 1 calc R . . H19B H 1.4276 0.6001 0.2258 0.051 Uiso 1 1 calc R . . H19C H 1.5224 0.5783 0.2239 0.051 Uiso 1 1 calc R . . C21 C 1.29750(12) 0.7936(2) 0.24909(8) 0.0287(5) Uani 1 1 d . A . C22 C 1.28686(14) 0.9148(2) 0.26075(9) 0.0345(5) Uani 1 1 d . . . H22 H 1.2537 0.9640 0.2351 0.041 Uiso 1 1 calc R A . C23 C 1.32419(15) 0.9647(2) 0.30961(10) 0.0429(6) Uani 1 1 d . A . H23 H 1.3173 1.0481 0.3168 0.052 Uiso 1 1 calc R . . C24 C 1.37125(16) 0.8938(3) 0.34774(10) 0.0457(6) Uani 1 1 d . . . H24 H 1.3983 0.9284 0.3806 0.055 Uiso 1 1 calc R A . C25 C 1.37857(15) 0.7727(3) 0.33774(9) 0.0424(6) Uani 1 1 d . A . H25 H 1.4093 0.7229 0.3644 0.051 Uiso 1 1 calc R . . C26 C 1.34128(14) 0.7224(2) 0.28887(9) 0.0361(5) Uani 1 1 d . . . H26 H 1.3460 0.6381 0.2828 0.043 Uiso 1 1 calc R A . C31 C 1.23558(15) 0.6092(2) 0.20136(9) 0.0377(6) Uani 1 1 d . A . C32 C 1.17480(19) 0.5849(3) 0.23405(11) 0.0610(9) Uani 1 1 d . . . H32 H 1.1474 0.6495 0.2489 0.073 Uiso 1 1 calc R A . C33 C 1.1550(2) 0.4665(4) 0.24460(12) 0.0810(12) Uani 1 1 d . A . H33 H 1.1135 0.4502 0.2663 0.097 Uiso 1 1 calc R . . C34 C 1.1952(3) 0.3722(3) 0.22371(13) 0.0855(13) Uani 1 1 d . . . H34 H 1.1819 0.2913 0.2316 0.103 Uiso 1 1 calc R A . C35 C 1.2542(2) 0.3947(3) 0.19172(13) 0.0679(9) Uani 1 1 d . A . H35 H 1.2813 0.3296 0.1770 0.081 Uiso 1 1 calc R . . C36 C 1.27435(17) 0.5138(2) 0.18074(9) 0.0435(6) Uani 1 1 d . . . H36 H 1.3155 0.5290 0.1586 0.052 Uiso 1 1 calc R A . C41 C 1.0743(2) 0.9752(2) 0.11394(17) 0.0341(13) Uani 0.552(6) 1 d PGU A 1 C42 C 1.0448(2) 1.0144(3) 0.06139(17) 0.0460(13) Uani 0.552(6) 1 d PGU A 1 H42 H 1.0435 0.9606 0.0313 0.055 Uiso 0.552(6) 1 calc PR A 1 C43 C 1.0174(2) 1.1324(3) 0.0528(2) 0.069(2) Uani 0.552(6) 1 d PGU A 1 H43 H 0.9972 1.1592 0.0169 0.083 Uiso 0.552(6) 1 calc PR A 1 C44 C 1.0194(3) 1.2111(2) 0.0968(3) 0.083(3) Uani 0.552(6) 1 d PGU A 1 H44 H 1.0006 1.2918 0.0909 0.100 Uiso 0.552(6) 1 calc PR A 1 C45 C 1.0488(3) 1.1719(3) 0.1493(2) 0.083(3) Uani 0.552(6) 1 d PGU A 1 H45 H 1.0502 1.2257 0.1794 0.100 Uiso 0.552(6) 1 calc PR A 1 C46 C 1.0763(2) 1.0539(4) 0.15791(19) 0.0556(17) Uani 0.552(6) 1 d PGU A 1 H46 H 1.0964 1.0271 0.1938 0.067 Uiso 0.552(6) 1 calc PR A 1 C51 C 1.02206(13) 0.7186(2) 0.13737(9) 0.0314(5) Uani 1 1 d . A . C52 C 1.02028(17) 0.5942(3) 0.13296(14) 0.0583(8) Uani 1 1 d . . . H52 H 1.0678 0.5527 0.1261 0.070 Uiso 1 1 calc R A . C53 C 0.95109(19) 0.5284(3) 0.13829(16) 0.0741(10) Uani 1 1 d . A . H53 H 0.9516 0.4430 0.1345 0.089 Uiso 1 1 calc R . . C54 C 0.88272(18) 0.5846(3) 0.14883(15) 0.0694(9) Uani 1 1 d . . . H54 H 0.8359 0.5386 0.1534 0.083 Uiso 1 1 calc R A . C55 C 0.88107(18) 0.7068(3) 0.15281(15) 0.0705(9) Uani 1 1 d . A . H55 H 0.8329 0.7466 0.1596 0.085 Uiso 1 1 calc R . . C56 C 0.95031(15) 0.7737(3) 0.14681(12) 0.0508(7) Uani 1 1 d . . . H56 H 0.9484 0.8592 0.1493 0.061 Uiso 1 1 calc R A . C61 C 1.20337(12) 0.7893(2) -0.00787(8) 0.0315(5) Uani 1 1 d . A . C62 C 1.20771(13) 0.7214(2) -0.05477(9) 0.0392(6) Uani 1 1 d . . . H62 H 1.2174 0.6369 -0.0520 0.047 Uiso 1 1 calc R A . C63 C 1.19782(15) 0.7777(3) -0.10579(10) 0.0491(7) Uani 1 1 d . A . H63 H 1.2012 0.7312 -0.1377 0.059 Uiso 1 1 calc R . . C64 C 1.18327(16) 0.8993(3) -0.11023(10) 0.0549(8) Uani 1 1 d . . . H64 H 1.1772 0.9371 -0.1451 0.066 Uiso 1 1 calc R A . C65 C 1.17744(15) 0.9671(3) -0.06412(10) 0.0487(7) Uani 1 1 d . A . H65 H 1.1669 1.0513 -0.0672 0.058 Uiso 1 1 calc R . . C66 C 1.18703(13) 0.9119(2) -0.01317(9) 0.0374(5) Uani 1 1 d . . . H66 H 1.1823 0.9586 0.0185 0.045 Uiso 1 1 calc R A . C71 C 1.20428(14) 0.5946(2) 0.04398(9) 0.0355(5) Uani 1 1 d . A . C72 C 1.12815(18) 0.5453(3) 0.02453(12) 0.0599(8) Uani 1 1 d . . . H72 H 1.0820 0.5966 0.0174 0.072 Uiso 1 1 calc R A . C73 C 1.1194(2) 0.4218(3) 0.01553(14) 0.0746(10) Uani 1 1 d . A . H73 H 1.0676 0.3900 0.0010 0.089 Uiso 1 1 calc R . . C74 C 1.1842(2) 0.3452(3) 0.02731(13) 0.0670(9) Uani 1 1 d . . . H74 H 1.1771 0.2605 0.0227 0.080 Uiso 1 1 calc R A . C75 C 1.25911(19) 0.3919(3) 0.04569(11) 0.0522(7) Uani 1 1 d . A . H75 H 1.3048 0.3398 0.0532 0.063 Uiso 1 1 calc R . . C76 C 1.26872(15) 0.5165(2) 0.05352(9) 0.0370(5) Uani 1 1 d . . . H76 H 1.3214 0.5478 0.0658 0.044 Uiso 1 1 calc R A . C41B C 1.0788(3) 0.9731(3) 0.1410(2) 0.0332(15) Uani 0.448(6) 1 d PGU A 2 C42B C 1.0556(3) 1.0483(4) 0.0965(2) 0.052(2) Uani 0.448(6) 1 d PGU A 2 H42B H 1.0604 1.0213 0.0606 0.062 Uiso 0.448(6) 1 calc PR A 2 C43B C 1.0255(3) 1.1631(4) 0.1044(3) 0.077(3) Uani 0.448(6) 1 d PGU A 2 H43B H 1.0096 1.2144 0.0740 0.093 Uiso 0.448(6) 1 calc PR A 2 C44B C 1.0185(3) 1.2026(3) 0.1569(3) 0.088(4) Uani 0.448(6) 1 d PGU A 2 H44B H 0.9979 1.2811 0.1623 0.106 Uiso 0.448(6) 1 calc PR A 2 C45B C 1.0416(3) 1.1274(4) 0.2015(3) 0.074(3) Uani 0.448(6) 1 d PGU A 2 H45B H 1.0369 1.1545 0.2373 0.089 Uiso 0.448(6) 1 calc PR A 2 C46B C 1.0718(3) 1.0127(4) 0.1935(2) 0.0484(17) Uani 0.448(6) 1 d PGU A 2 H46B H 1.0876 0.9613 0.2240 0.058 Uiso 0.448(6) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02519(15) 0.01942(14) 0.03085(16) 0.00361(11) 0.00562(11) 0.00059(11) Si1 0.0211(3) 0.0274(3) 0.0398(3) -0.0008(3) 0.0074(2) 0.0024(2) Si2 0.0225(3) 0.0420(4) 0.0300(3) 0.0043(3) 0.0056(2) 0.0004(3) O1 0.0229(8) 0.0560(10) 0.0356(9) -0.0173(8) 0.0083(6) 0.0011(7) O2 0.0218(8) 0.0747(12) 0.0271(8) 0.0145(8) 0.0065(6) 0.0077(8) O3 0.0232(7) 0.0424(9) 0.0290(8) 0.0053(7) 0.0055(6) -0.0048(6) O4 0.0230(7) 0.0392(9) 0.0318(8) 0.0068(7) 0.0071(6) 0.0065(6) C1 0.0440(14) 0.0262(12) 0.0627(17) 0.0034(11) -0.0032(12) -0.0060(10) C2 0.087(2) 0.0232(12) 0.070(2) -0.0101(12) 0.0383(18) -0.0114(13) C3 0.0323(14) 0.0174(12) 0.143(3) 0.0038(15) 0.0186(17) 0.0038(10) C4 0.0647(19) 0.0280(13) 0.0640(18) 0.0188(12) -0.0115(15) -0.0051(12) C5 0.0504(15) 0.0278(13) 0.0647(18) 0.0089(12) 0.0221(13) -0.0084(11) C6 0.0239(10) 0.0200(9) 0.0204(9) 0.0011(7) 0.0048(8) 0.0014(8) C7 0.0232(10) 0.0201(9) 0.0191(9) 0.0009(7) 0.0052(7) 0.0017(8) C8 0.0237(10) 0.0223(10) 0.0201(9) 0.0041(8) 0.0034(8) 0.0009(8) C9 0.0231(10) 0.0252(10) 0.0192(9) 0.0021(8) 0.0033(8) 0.0004(8) C10 0.0265(10) 0.0338(12) 0.0215(10) -0.0042(8) 0.0082(8) -0.0036(9) C11 0.0207(10) 0.0412(12) 0.0228(10) 0.0063(9) 0.0022(8) -0.0003(9) C12 0.0234(10) 0.0472(14) 0.0239(11) -0.0028(9) 0.0059(8) -0.0053(9) C13 0.0310(12) 0.088(2) 0.0227(11) 0.0109(12) 0.0057(9) -0.0127(13) C14 0.0408(14) 0.0559(17) 0.0495(15) -0.0205(13) 0.0225(12) -0.0061(12) C15 0.0360(13) 0.0572(17) 0.0463(15) 0.0048(12) 0.0004(11) -0.0159(12) C16 0.0344(13) 0.0710(19) 0.0571(17) 0.0091(14) 0.0207(12) 0.0123(13) C17 0.0224(10) 0.0320(11) 0.0231(10) 0.0036(8) 0.0037(8) 0.0019(8) C18 0.0336(12) 0.0418(13) 0.0260(11) -0.0019(10) -0.0012(9) -0.0045(10) C19 0.0343(12) 0.0352(13) 0.0324(12) 0.0108(10) 0.0048(9) 0.0065(10) C21 0.0252(10) 0.0401(12) 0.0225(10) -0.0056(9) 0.0096(8) -0.0065(9) C22 0.0333(12) 0.0391(13) 0.0323(12) -0.0069(10) 0.0090(9) -0.0056(10) C23 0.0460(14) 0.0453(14) 0.0391(14) -0.0164(11) 0.0113(11) -0.0122(12) C24 0.0449(15) 0.0636(18) 0.0289(12) -0.0136(12) 0.0066(11) -0.0171(13) C25 0.0436(14) 0.0599(17) 0.0240(11) 0.0009(11) 0.0066(10) -0.0028(12) C26 0.0432(13) 0.0430(14) 0.0239(11) -0.0010(10) 0.0115(10) -0.0044(11) C31 0.0501(14) 0.0427(14) 0.0206(11) -0.0022(9) 0.0061(10) -0.0191(11) C32 0.077(2) 0.076(2) 0.0355(14) -0.0088(14) 0.0251(14) -0.0394(17) C33 0.109(3) 0.097(3) 0.0394(16) 0.0010(18) 0.0202(17) -0.067(2) C34 0.143(4) 0.065(2) 0.0441(18) 0.0101(16) -0.003(2) -0.065(2) C35 0.109(3) 0.0392(16) 0.0506(17) 0.0005(13) -0.0051(18) -0.0207(17) C36 0.0635(17) 0.0351(13) 0.0296(12) 0.0009(10) -0.0006(11) -0.0141(12) C41 0.022(2) 0.026(2) 0.055(4) -0.003(2) 0.008(2) 0.0004(18) C42 0.033(2) 0.039(3) 0.067(3) 0.013(2) 0.009(3) 0.009(2) C43 0.043(3) 0.050(3) 0.116(6) 0.031(3) 0.016(3) 0.009(3) C44 0.041(3) 0.021(3) 0.186(8) 0.007(4) 0.011(4) 0.011(3) C45 0.042(4) 0.042(4) 0.159(7) -0.044(4) -0.012(4) 0.012(3) C46 0.037(3) 0.038(3) 0.087(5) -0.023(3) -0.003(3) 0.011(2) C51 0.0263(11) 0.0399(13) 0.0289(11) -0.0025(9) 0.0068(9) -0.0023(9) C52 0.0405(15) 0.0469(17) 0.093(2) -0.0115(15) 0.0296(15) -0.0059(12) C53 0.0581(19) 0.0501(18) 0.120(3) -0.0099(19) 0.0325(19) -0.0205(15) C54 0.0431(17) 0.076(2) 0.095(3) -0.0104(19) 0.0293(16) -0.0275(16) C55 0.0351(15) 0.079(2) 0.103(3) -0.015(2) 0.0289(16) -0.0081(15) C56 0.0331(13) 0.0529(17) 0.0687(18) -0.0061(14) 0.0150(12) -0.0024(12) C61 0.0193(10) 0.0507(14) 0.0236(11) 0.0102(10) 0.0002(8) -0.0018(9) C62 0.0274(11) 0.0598(16) 0.0302(12) 0.0047(11) 0.0034(9) -0.0030(11) C63 0.0337(13) 0.088(2) 0.0248(12) 0.0050(13) 0.0031(10) -0.0086(14) C64 0.0367(14) 0.097(2) 0.0293(13) 0.0266(14) -0.0015(10) -0.0125(15) C65 0.0365(13) 0.0634(17) 0.0437(15) 0.0262(13) -0.0033(11) -0.0055(12) C66 0.0269(11) 0.0533(15) 0.0310(12) 0.0109(11) 0.0006(9) -0.0008(10) C71 0.0378(12) 0.0432(14) 0.0235(11) 0.0037(10) -0.0020(9) -0.0123(11) C72 0.0462(16) 0.0645(19) 0.0633(19) 0.0131(15) -0.0119(14) -0.0195(14) C73 0.070(2) 0.069(2) 0.077(2) 0.0033(18) -0.0125(18) -0.0420(19) C74 0.089(2) 0.0483(18) 0.063(2) -0.0106(15) 0.0066(18) -0.0265(18) C75 0.0658(18) 0.0431(15) 0.0505(16) -0.0122(12) 0.0185(14) -0.0099(13) C76 0.0418(13) 0.0404(14) 0.0301(12) -0.0083(10) 0.0099(10) -0.0088(11) C41B 0.020(3) 0.035(3) 0.044(4) 0.006(3) 0.002(3) 0.007(2) C42B 0.036(3) 0.041(4) 0.082(5) 0.025(4) 0.019(4) 0.008(3) C43B 0.046(4) 0.022(4) 0.160(8) 0.026(5) -0.001(5) 0.011(3) C44B 0.048(5) 0.029(4) 0.177(9) -0.013(4) -0.022(6) 0.016(3) C45B 0.047(4) 0.056(4) 0.114(7) -0.038(4) -0.006(4) 0.013(3) C46B 0.035(3) 0.043(3) 0.065(4) -0.015(3) 0.001(3) 0.010(3) _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 Co1 C9 1.964(2) . ? Co1 C8 1.9869(19) . ? Co1 C7 2.0026(19) . ? Co1 C6 2.0062(19) . ? Co1 C4 2.067(2) . ? Co1 C3 2.071(2) . ? Co1 C5 2.086(2) . ? Co1 C2 2.087(3) . ? Co1 C1 2.099(2) . ? Si1 O2 1.6134(16) . ? Si1 O1 1.6186(16) . ? Si1 C51 1.869(2) . ? Si1 C41B 1.884(3) . ? Si1 C41 1.907(2) . ? Si2 O3 1.6271(15) . ? Si2 O4 1.6292(15) . ? Si2 C15 1.843(3) . ? Si2 C16 1.853(3) . ? O1 C10 1.433(3) . ? O2 C11 1.431(2) . ? O3 C12 1.446(2) . ? O4 C17 1.446(2) . ? C1 C5 1.378(4) . ? C1 C2 1.383(4) . ? C2 C3 1.414(5) . ? C3 C4 1.408(5) . ? C4 C5 1.385(4) . ? C6 C9 1.463(3) . ? C6 C7 1.479(3) . ? C6 C17 1.532(3) . ? C7 C8 1.480(3) . ? C7 C10 1.544(3) . ? C8 C9 1.482(3) . ? C8 C11 1.528(3) . ? C9 C12 1.533(3) . ? C10 C31 1.541(3) . ? C10 C21 1.544(3) . ? C11 C71 1.540(3) . ? C11 C61 1.545(3) . ? C12 C13 1.524(3) . ? C12 C14 1.530(3) . ? C17 C19 1.520(3) . ? C17 C18 1.525(3) . ? C21 C26 1.382(3) . ? C21 C22 1.389(3) . ? C22 C23 1.391(3) . ? C23 C24 1.380(4) . ? C24 C25 1.371(4) . ? C25 C26 1.392(3) . ? C31 C36 1.373(4) . ? C31 C32 1.407(3) . ? C32 C33 1.385(4) . ? C33 C34 1.380(6) . ? C34 C35 1.368(5) . ? C35 C36 1.397(4) . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C51 C52 1.382(4) . ? C51 C56 1.389(3) . ? C52 C53 1.383(4) . ? C53 C54 1.353(4) . ? C54 C55 1.357(4) . ? C55 C56 1.394(4) . ? C61 C66 1.387(3) . ? C61 C62 1.392(3) . ? C62 C63 1.395(3) . ? C63 C64 1.371(4) . ? C64 C65 1.380(4) . ? C65 C66 1.388(3) . ? C71 C76 1.371(3) . ? C71 C72 1.398(3) . ? C72 C73 1.390(4) . ? C73 C74 1.369(5) . ? C74 C75 1.364(4) . ? C75 C76 1.399(3) . ? C41B C42B 1.3900 . ? C41B C46B 1.3900 . ? C42B C43B 1.3900 . ? C43B C44B 1.3900 . ? C44B C45B 1.3900 . ? C45B C46B 1.3900 . ? 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 C9 Co1 C8 44.06(8) . . ? C9 Co1 C7 63.44(8) . . ? C8 Co1 C7 43.54(7) . . ? C9 Co1 C6 43.25(7) . . ? C8 Co1 C6 63.10(8) . . ? C7 Co1 C6 43.31(7) . . ? C9 Co1 C4 118.42(11) . . ? C8 Co1 C4 116.25(10) . . ? C7 Co1 C4 152.50(10) . . ? C6 Co1 C4 156.90(11) . . ? C9 Co1 C3 151.98(12) . . ? C8 Co1 C3 120.40(10) . . ? C7 Co1 C3 125.58(10) . . ? C6 Co1 C3 162.66(12) . . ? C4 Co1 C3 39.78(13) . . ? C9 Co1 C5 109.01(9) . . ? C8 Co1 C5 138.14(10) . . ? C7 Co1 C5 167.73(9) . . ? C6 Co1 C5 124.46(9) . . ? C4 Co1 C5 38.96(11) . . ? C3 Co1 C5 65.83(11) . . ? C9 Co1 C2 165.59(11) . . ? C8 Co1 C2 148.59(10) . . ? C7 Co1 C2 119.62(9) . . ? C6 Co1 C2 127.77(11) . . ? C4 Co1 C2 66.16(13) . . ? C3 Co1 C2 39.76(13) . . ? C5 Co1 C2 65.15(11) . . ? C9 Co1 C1 128.74(10) . . ? C8 Co1 C1 172.78(9) . . ? C7 Co1 C1 137.71(9) . . ? C6 Co1 C1 112.56(9) . . ? C4 Co1 C1 65.18(11) . . ? C3 Co1 C1 65.59(11) . . ? C5 Co1 C1 38.47(11) . . ? C2 Co1 C1 38.59(11) . . ? O2 Si1 O1 112.32(8) . . ? O2 Si1 C51 107.56(9) . . ? O1 Si1 C51 114.23(9) . . ? O2 Si1 C41B 122.13(16) . . ? O1 Si1 C41B 95.83(16) . . ? C51 Si1 C41B 104.56(16) . . ? O2 Si1 C41 103.02(15) . . ? O1 Si1 C41 111.23(13) . . ? C51 Si1 C41 107.78(14) . . ? C41B Si1 C41 20.15(13) . . ? O3 Si2 O4 108.15(8) . . ? O3 Si2 C15 107.57(10) . . ? O4 Si2 C15 114.24(10) . . ? O3 Si2 C16 112.30(11) . . ? O4 Si2 C16 105.82(11) . . ? C15 Si2 C16 108.85(13) . . ? C10 O1 Si1 135.74(13) . . ? C11 O2 Si1 142.08(13) . . ? C12 O3 Si2 127.80(14) . . ? C17 O4 Si2 133.83(13) . . ? C5 C1 C2 108.9(3) . . ? C5 C1 Co1 70.25(14) . . ? C2 C1 Co1 70.25(15) . . ? C1 C2 C3 107.7(3) . . ? C1 C2 Co1 71.16(15) . . ? C3 C2 Co1 69.49(15) . . ? C4 C3 C2 106.9(2) . . ? C4 C3 Co1 69.98(15) . . ? C2 C3 Co1 70.74(15) . . ? C5 C4 C3 107.9(3) . . ? C5 C4 Co1 71.23(14) . . ? C3 C4 Co1 70.23(15) . . ? C1 C5 C4 108.6(3) . . ? C1 C5 Co1 71.28(14) . . ? C4 C5 Co1 69.81(14) . . ? C9 C6 C7 90.26(14) . . ? C9 C6 C17 132.62(17) . . ? C7 C6 C17 134.93(16) . . ? C9 C6 Co1 66.83(10) . . ? C7 C6 Co1 68.22(10) . . ? C17 C6 Co1 134.07(14) . . ? C6 C7 C8 89.83(14) . . ? C6 C7 C10 137.79(17) . . ? C8 C7 C10 131.61(17) . . ? C6 C7 Co1 68.47(10) . . ? C8 C7 Co1 67.67(10) . . ? C10 C7 Co1 128.31(14) . . ? C7 C8 C9 89.53(14) . . ? C7 C8 C11 131.20(17) . . ? C9 C8 C11 135.12(17) . . ? C7 C8 Co1 68.79(10) . . ? C9 C8 Co1 67.14(11) . . ? C11 C8 Co1 137.45(14) . . ? C6 C9 C8 90.36(15) . . ? C6 C9 C12 130.81(17) . . ? C8 C9 C12 138.63(17) . . ? C6 C9 Co1 69.92(11) . . ? C8 C9 Co1 68.80(11) . . ? C12 C9 Co1 123.40(15) . . ? O1 C10 C31 108.20(17) . . ? O1 C10 C7 108.17(16) . . ? C31 C10 C7 113.68(17) . . ? O1 C10 C21 104.81(16) . . ? C31 C10 C21 108.47(17) . . ? C7 C10 C21 113.03(16) . . ? O2 C11 C8 110.60(17) . . ? O2 C11 C71 107.08(18) . . ? C8 C11 C71 110.97(17) . . ? O2 C11 C61 104.23(16) . . ? C8 C11 C61 114.80(17) . . ? C71 C11 C61 108.69(18) . . ? O3 C12 C13 103.62(18) . . ? O3 C12 C14 110.00(18) . . ? C13 C12 C14 109.2(2) . . ? O3 C12 C9 108.25(16) . . ? C13 C12 C9 114.35(18) . . ? C14 C12 C9 111.08(18) . . ? O4 C17 C19 102.15(16) . . ? O4 C17 C18 108.34(17) . . ? C19 C17 C18 111.05(17) . . ? O4 C17 C6 110.52(15) . . ? C19 C17 C6 110.27(17) . . ? C18 C17 C6 113.86(17) . . ? C26 C21 C22 118.2(2) . . ? C26 C21 C10 122.4(2) . . ? C22 C21 C10 119.3(2) . . ? C21 C22 C23 120.7(2) . . ? C24 C23 C22 120.3(2) . . ? C25 C24 C23 119.3(2) . . ? C24 C25 C26 120.5(2) . . ? C21 C26 C25 120.8(2) . . ? C36 C31 C32 118.6(2) . . ? C36 C31 C10 123.5(2) . . ? C32 C31 C10 117.8(2) . . ? C33 C32 C31 119.9(3) . . ? C34 C33 C32 120.3(3) . . ? C35 C34 C33 120.3(3) . . ? C34 C35 C36 119.7(3) . . ? C31 C36 C35 121.1(3) . . ? C42 C41 C46 120.0 . . ? C42 C41 Si1 122.01(19) . . ? C46 C41 Si1 117.99(19) . . ? C41 C42 C43 120.0 . . ? C44 C43 C42 120.0 . . ? C43 C44 C45 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C41 120.0 . . ? C52 C51 C56 116.2(2) . . ? C52 C51 Si1 124.28(18) . . ? C56 C51 Si1 119.42(19) . . ? C51 C52 C53 121.7(3) . . ? C54 C53 C52 120.5(3) . . ? C53 C54 C55 119.9(3) . . ? C54 C55 C56 119.8(3) . . ? C51 C56 C55 121.7(3) . . ? C66 C61 C62 118.9(2) . . ? C66 C61 C11 118.4(2) . . ? C62 C61 C11 122.7(2) . . ? C61 C62 C63 119.9(3) . . ? C64 C63 C62 120.5(3) . . ? C63 C64 C65 120.1(2) . . ? C64 C65 C66 119.8(3) . . ? C61 C66 C65 120.8(2) . . ? C76 C71 C72 117.3(2) . . ? C76 C71 C11 123.8(2) . . ? C72 C71 C11 118.8(2) . . ? C73 C72 C71 120.6(3) . . ? C74 C73 C72 120.9(3) . . ? C75 C74 C73 119.2(3) . . ? C74 C75 C76 120.0(3) . . ? C71 C76 C75 121.9(2) . . ? C42B C41B C46B 120.0 . . ? C42B C41B Si1 118.9(2) . . ? C46B C41B Si1 121.0(2) . . ? C41B C42B C43B 120.0 . . ? C42B C43B C44B 120.0 . . ? C45B C44B C43B 120.0 . . ? C46B C45B C44B 120.0 . . ? C45B C46B C41B 120.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.363 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.073 #===END data_cs50 _database_code_depnum_ccdc_archive 'CCDC 243856' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cs50 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H63 Co N4 O7 Si2' _chemical_formula_weight 767.00 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 19.8492(19) _cell_length_b 11.8567(11) _cell_length_c 21.220(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.753(2) _cell_angle_gamma 90.00 _cell_volume 4756.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour orange _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8328 _exptl_absorpt_correction_T_max 0.9519 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32511 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 23.59 _reflns_number_total 7095 _reflns_number_gt 5281 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0830P)^2^+22.8830P] 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 7095 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1081 _refine_ls_R_factor_gt 0.0795 _refine_ls_wR_factor_ref 0.2068 _refine_ls_wR_factor_gt 0.1894 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.004 _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 Co1 Co 0.27436(4) 0.85146(6) 0.82835(4) 0.0166(2) Uani 1 1 d . . . Si1 Si 0.41792(9) 1.14100(15) 0.87943(9) 0.0328(4) Uani 1 1 d . . . O1 O 0.3860(2) 1.0873(4) 0.8062(2) 0.0310(10) Uani 1 1 d . . . O2 O 0.3820(2) 1.0793(3) 0.9300(2) 0.0310(10) Uani 1 1 d . . . Si2 Si 0.05537(8) 0.81128(14) 0.76077(9) 0.0255(4) Uani 1 1 d . . . O3 O 0.0730(2) 0.9046(4) 0.8193(2) 0.0309(10) Uani 1 1 d . . . O4 O 0.1038(2) 0.8394(3) 0.7120(2) 0.0324(10) Uani 1 1 d . . . C1 C 0.2695(3) 1.0106(4) 0.7946(3) 0.0186(12) Uani 1 1 d . . . C2 C 0.2679(3) 1.0064(4) 0.8638(3) 0.0181(12) Uani 1 1 d . . . C3 C 0.1965(3) 0.9554(4) 0.8406(3) 0.0176(12) Uani 1 1 d . . . C4 C 0.1987(3) 0.9594(4) 0.7726(3) 0.0165(12) Uani 1 1 d . . . C5 C 0.3163(3) 1.0705(5) 0.7604(3) 0.0257(13) Uani 1 1 d . . . C6 C 0.3295(3) 1.0056(6) 0.7036(3) 0.0336(15) Uani 1 1 d . . . H6A H 0.3637 1.0469 0.6873 0.050 Uiso 1 1 calc R . . H6B H 0.2850 0.9974 0.6677 0.050 Uiso 1 1 calc R . . H6C H 0.3485 0.9308 0.7190 0.050 Uiso 1 1 calc R . . C7 C 0.2821(3) 1.1845(5) 0.7355(3) 0.0322(15) Uani 1 1 d . . . H7A H 0.2732 1.2258 0.7722 0.048 Uiso 1 1 calc R . . H7B H 0.2372 1.1722 0.7005 0.048 Uiso 1 1 calc R . . H7C H 0.3140 1.2286 0.7177 0.048 Uiso 1 1 calc R . . C8 C 0.5126(4) 1.1027(7) 0.9126(4) 0.054(2) Uani 1 1 d . . . H8A H 0.5170 1.0215 0.9213 0.081 Uiso 1 1 calc R . . H8B H 0.5342 1.1441 0.9538 0.081 Uiso 1 1 calc R . . H8C H 0.5368 1.1224 0.8801 0.081 Uiso 1 1 calc R . . C9 C 0.4116(4) 1.2990(6) 0.8781(4) 0.0468(19) Uani 1 1 d . . . H9A H 0.4386 1.3297 0.8504 0.070 Uiso 1 1 calc R . . H9B H 0.4309 1.3282 0.9233 0.070 Uiso 1 1 calc R . . H9C H 0.3619 1.3216 0.8600 0.070 Uiso 1 1 calc R . . C10 C 0.3088(3) 1.0697(5) 0.9264(3) 0.0240(13) Uani 1 1 d . . . C11 C 0.3098(3) 1.0078(5) 0.9897(3) 0.0311(15) Uani 1 1 d . . . H11A H 0.3282 0.9312 0.9888 0.047 Uiso 1 1 calc R . . H11B H 0.2616 1.0038 0.9929 0.047 Uiso 1 1 calc R . . H11C H 0.3402 1.0484 1.0280 0.047 Uiso 1 1 calc R . . C12 C 0.2780(3) 1.1881(5) 0.9260(3) 0.0294(14) Uani 1 1 d . . . H12A H 0.3078 1.2312 0.9636 0.044 Uiso 1 1 calc R . . H12B H 0.2300 1.1824 0.9296 0.044 Uiso 1 1 calc R . . H12C H 0.2763 1.2263 0.8846 0.044 Uiso 1 1 calc R . . C13 C 0.1396(3) 0.9427(5) 0.7079(3) 0.0219(13) Uani 1 1 d . . . C14 C 0.1639(4) 0.9296(6) 0.6470(3) 0.0357(16) Uani 1 1 d . . . H14A H 0.1998 0.8700 0.6547 0.054 Uiso 1 1 calc R . . H14B H 0.1843 1.0009 0.6380 0.054 Uiso 1 1 calc R . . H14C H 0.1234 0.9094 0.6089 0.054 Uiso 1 1 calc R . . C15 C 0.0906(3) 1.0445(5) 0.6985(3) 0.0362(16) Uani 1 1 d . . . H15A H 0.0503 1.0341 0.6585 0.054 Uiso 1 1 calc R . . H15B H 0.1166 1.1128 0.6939 0.054 Uiso 1 1 calc R . . H15C H 0.0735 1.0521 0.7369 0.054 Uiso 1 1 calc R . . C16 C 0.0763(4) 0.6636(5) 0.7868(4) 0.0417(17) Uani 1 1 d . . . H16A H 0.1276 0.6549 0.8058 0.062 Uiso 1 1 calc R . . H16B H 0.0592 0.6138 0.7483 0.062 Uiso 1 1 calc R . . H16C H 0.0532 0.6435 0.8200 0.062 Uiso 1 1 calc R . . C17 C -0.0404(3) 0.8297(6) 0.7177(4) 0.0438(18) Uani 1 1 d . . . H17A H -0.0675 0.8100 0.7479 0.066 Uiso 1 1 calc R . . H17B H -0.0547 0.7805 0.6788 0.066 Uiso 1 1 calc R . . H17C H -0.0498 0.9085 0.7038 0.066 Uiso 1 1 calc R . . C18 C 0.1362(3) 0.9370(5) 0.8700(3) 0.0215(13) Uani 1 1 d . . . C19 C 0.1499(3) 0.8508(6) 0.9250(3) 0.0373(16) Uani 1 1 d . . . H19A H 0.1137 0.8579 0.9476 0.056 Uiso 1 1 calc R . . H19B H 0.1967 0.8639 0.9568 0.056 Uiso 1 1 calc R . . H19C H 0.1480 0.7748 0.9064 0.056 Uiso 1 1 calc R . . C20 C 0.1169(3) 1.0511(5) 0.8950(3) 0.0336(15) Uani 1 1 d . . . H20A H 0.1170 1.1102 0.8627 0.050 Uiso 1 1 calc R . . H20B H 0.1516 1.0695 0.9376 0.050 Uiso 1 1 calc R . . H20C H 0.0697 1.0460 0.9005 0.050 Uiso 1 1 calc R . . C31 C 0.2511(3) 0.7382(5) 0.7632(3) 0.0243(14) Uani 1 1 d . . . N1 N 0.2427(3) 0.6637(4) 0.7276(3) 0.0315(12) Uani 1 1 d . . . C32 C 0.2313(4) 0.5684(5) 0.6812(3) 0.0332(15) Uani 1 1 d . . . C33 C 0.2024(6) 0.4717(6) 0.7112(4) 0.068(3) Uani 1 1 d . . . H33A H 0.2367 0.4509 0.7536 0.102 Uiso 1 1 calc R . . H33B H 0.1939 0.4069 0.6812 0.102 Uiso 1 1 calc R . . H33C H 0.1579 0.4945 0.7184 0.102 Uiso 1 1 calc R . . C34 C 0.3012(5) 0.5370(9) 0.6735(6) 0.096(4) Uani 1 1 d . . . H34A H 0.3204 0.6014 0.6556 0.144 Uiso 1 1 calc R . . H34B H 0.2951 0.4730 0.6431 0.144 Uiso 1 1 calc R . . H34C H 0.3339 0.5162 0.7167 0.144 Uiso 1 1 calc R . . C35 C 0.1801(6) 0.6039(7) 0.6165(4) 0.085(3) Uani 1 1 d . . . H35A H 0.1350 0.6246 0.6231 0.127 Uiso 1 1 calc R . . H35B H 0.1727 0.5414 0.5849 0.127 Uiso 1 1 calc R . . H35C H 0.1993 0.6690 0.5992 0.127 Uiso 1 1 calc R . . C36 C 0.2772(4) 0.7459(5) 0.8949(3) 0.0330(15) Uani 1 1 d . . . N2 N 0.2824(4) 0.6738(5) 0.9320(3) 0.0501(17) Uani 1 1 d . . . C37 C 0.2779(6) 0.5770(6) 0.9741(4) 0.071(3) Uani 1 1 d . . . C38 C 0.2451(8) 0.6150(8) 1.0239(5) 0.103(5) Uani 1 1 d . . . H38A H 0.2468 0.5539 1.0554 0.155 Uiso 1 1 calc R . . H38B H 0.1957 0.6358 1.0019 0.155 Uiso 1 1 calc R . . H38C H 0.2708 0.6806 1.0474 0.155 Uiso 1 1 calc R . . C39 C 0.3492(8) 0.5290(11) 1.0015(7) 0.137(6) Uani 1 1 d . . . H39A H 0.3666 0.5042 0.9653 0.206 Uiso 1 1 calc R . . H39B H 0.3473 0.4643 1.0297 0.206 Uiso 1 1 calc R . . H39C H 0.3811 0.5863 1.0278 0.206 Uiso 1 1 calc R . . C40 C 0.2284(9) 0.4902(8) 0.9268(5) 0.127(6) Uani 1 1 d . . . H40A H 0.2499 0.4662 0.8931 0.191 Uiso 1 1 calc R . . H40B H 0.1825 0.5254 0.9053 0.191 Uiso 1 1 calc R . . H40C H 0.2218 0.4245 0.9523 0.191 Uiso 1 1 calc R . . C41 C 0.3707(3) 0.8311(5) 0.8391(3) 0.0264(14) Uani 1 1 d . . . N3 N 0.4274(3) 0.8044(5) 0.8435(3) 0.0338(13) Uani 1 1 d . . . C42 C 0.4973(4) 0.7560(6) 0.8506(4) 0.048(2) Uani 1 1 d . . . C43 C 0.5350(4) 0.8348(8) 0.8163(4) 0.066(3) Uani 1 1 d . . . H43A H 0.5091 0.8376 0.7689 0.099 Uiso 1 1 calc R . . H43B H 0.5831 0.8073 0.8225 0.099 Uiso 1 1 calc R . . H43C H 0.5370 0.9106 0.8352 0.099 Uiso 1 1 calc R . . C44 C 0.5359(4) 0.7455(8) 0.9244(5) 0.068(3) Uani 1 1 d . . . H44A H 0.5411 0.8204 0.9448 0.103 Uiso 1 1 calc R . . H44B H 0.5828 0.7125 0.9308 0.103 Uiso 1 1 calc R . . H44C H 0.5087 0.6969 0.9450 0.103 Uiso 1 1 calc R . . C45 C 0.4831(5) 0.6430(10) 0.8153(8) 0.129(6) Uani 1 1 d . . . H45A H 0.4526 0.5974 0.8339 0.194 Uiso 1 1 calc R . . H45B H 0.5280 0.6034 0.8213 0.194 Uiso 1 1 calc R . . H45C H 0.4596 0.6552 0.7680 0.194 Uiso 1 1 calc R . . N4 N 0.2411(3) 1.2391(5) 0.5711(2) 0.0349(13) Uani 1 1 d . . . O11 O 0.2105(3) 1.3335(4) 0.5663(3) 0.0639(16) Uani 1 1 d . . . O12 O 0.2030(3) 1.1547(4) 0.5606(3) 0.0517(13) Uani 1 1 d . . . O13 O 0.3043(3) 1.2298(7) 0.5859(3) 0.090(3) Uani 1 1 d . . . C51 C 0.0229(8) 1.1609(13) 0.5153(8) 0.0756(12) Uiso 0.67 1 d P . . C52 C -0.0021(7) 1.2051(11) 0.5719(6) 0.0756(12) Uiso 0.79 1 d P . . C53 C 0.0407(5) 1.2952(9) 0.5891(5) 0.0756(12) Uiso 1 1 d . . . C54 C 0.0282(5) 1.3713(9) 0.5218(5) 0.0756(12) Uiso 1 1 d . . . C55 C 0.0181(7) 1.2456(12) 0.4655(7) 0.0756(12) Uiso 0.75 1 d P . . C56 C 0.0364(9) 1.2047(14) 0.4365(8) 0.0756(12) Uiso 0.63 1 d P . . C57 C -0.0141(6) 1.1355(10) 0.5317(6) 0.0756(12) Uiso 0.88 1 d P . . C58 C -0.0059(9) 1.3364(14) 0.4677(8) 0.0756(12) Uiso 0.62 1 d P . . 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 Co1 0.0182(4) 0.0143(4) 0.0182(4) 0.0024(3) 0.0069(3) 0.0043(3) Si1 0.0246(9) 0.0287(10) 0.0462(11) -0.0059(8) 0.0125(8) -0.0072(8) O1 0.023(2) 0.034(2) 0.038(2) -0.002(2) 0.0116(19) -0.0056(19) O2 0.023(2) 0.032(2) 0.034(2) -0.0042(19) 0.0028(18) -0.0032(19) Si2 0.0197(8) 0.0199(9) 0.0362(10) -0.0008(7) 0.0074(7) -0.0014(7) O3 0.024(2) 0.034(2) 0.037(2) -0.003(2) 0.0126(19) -0.0007(19) O4 0.034(2) 0.029(2) 0.032(2) -0.0044(19) 0.0082(19) -0.007(2) C1 0.023(3) 0.013(3) 0.020(3) 0.001(2) 0.007(2) 0.002(2) C2 0.019(3) 0.014(3) 0.021(3) 0.001(2) 0.006(2) 0.003(2) C3 0.020(3) 0.013(3) 0.020(3) -0.001(2) 0.006(2) 0.002(2) C4 0.020(3) 0.010(3) 0.021(3) 0.004(2) 0.010(2) 0.003(2) C5 0.030(3) 0.022(3) 0.027(3) 0.002(3) 0.013(3) -0.006(3) C6 0.037(4) 0.036(4) 0.035(4) -0.004(3) 0.023(3) -0.010(3) C7 0.038(4) 0.025(3) 0.036(4) 0.004(3) 0.015(3) -0.008(3) C8 0.029(4) 0.063(5) 0.070(5) -0.010(4) 0.014(4) -0.005(4) C9 0.055(5) 0.029(4) 0.060(5) -0.007(3) 0.024(4) -0.010(3) C10 0.023(3) 0.025(3) 0.025(3) -0.002(3) 0.009(3) -0.005(3) C11 0.037(4) 0.031(4) 0.022(3) -0.003(3) 0.003(3) -0.004(3) C12 0.041(4) 0.021(3) 0.026(3) -0.006(3) 0.009(3) 0.000(3) C13 0.024(3) 0.017(3) 0.022(3) 0.003(2) 0.001(2) -0.002(2) C14 0.039(4) 0.042(4) 0.022(3) 0.000(3) 0.004(3) -0.004(3) C15 0.032(4) 0.029(4) 0.035(4) 0.003(3) -0.007(3) 0.008(3) C16 0.037(4) 0.022(4) 0.069(5) 0.002(3) 0.021(4) -0.003(3) C17 0.026(4) 0.039(4) 0.060(5) -0.004(4) 0.003(3) -0.003(3) C18 0.018(3) 0.023(3) 0.024(3) -0.002(2) 0.007(2) -0.002(2) C19 0.033(4) 0.047(4) 0.038(4) 0.012(3) 0.021(3) 0.001(3) C20 0.029(3) 0.032(4) 0.043(4) -0.007(3) 0.017(3) 0.002(3) C31 0.024(3) 0.020(3) 0.030(3) 0.010(3) 0.012(3) 0.009(3) N1 0.047(3) 0.018(3) 0.036(3) -0.008(3) 0.022(3) 0.000(2) C32 0.047(4) 0.021(3) 0.029(4) -0.006(3) 0.007(3) 0.001(3) C33 0.126(8) 0.026(4) 0.066(6) -0.017(4) 0.049(6) -0.013(5) C34 0.058(6) 0.098(8) 0.137(10) -0.089(8) 0.040(6) -0.023(6) C35 0.137(9) 0.042(5) 0.047(5) -0.015(4) -0.015(6) 0.013(6) C36 0.049(4) 0.023(3) 0.035(4) 0.000(3) 0.025(3) 0.010(3) N2 0.094(5) 0.025(3) 0.047(4) 0.019(3) 0.044(4) 0.026(3) C37 0.152(9) 0.025(4) 0.057(5) 0.026(4) 0.061(6) 0.033(5) C38 0.214(14) 0.053(6) 0.078(7) 0.037(5) 0.098(9) 0.046(7) C39 0.167(14) 0.110(10) 0.141(12) 0.093(9) 0.056(10) 0.068(10) C40 0.271(19) 0.040(6) 0.071(7) 0.019(5) 0.054(9) -0.015(8) C41 0.028(4) 0.024(3) 0.026(3) -0.002(3) 0.007(3) 0.002(3) N3 0.021(3) 0.038(3) 0.040(3) -0.009(3) 0.006(2) 0.007(2) C42 0.024(4) 0.044(4) 0.076(6) -0.015(4) 0.016(4) 0.010(3) C43 0.034(4) 0.107(8) 0.063(5) 0.000(5) 0.026(4) 0.011(5) C44 0.034(4) 0.072(6) 0.088(7) 0.032(5) 0.002(4) 0.005(4) C45 0.050(6) 0.099(9) 0.242(16) -0.094(10) 0.050(8) 0.011(6) N4 0.039(4) 0.047(4) 0.021(3) 0.003(3) 0.012(2) -0.006(3) O11 0.106(5) 0.024(3) 0.076(4) -0.011(3) 0.048(4) -0.002(3) O12 0.057(3) 0.028(3) 0.065(3) -0.008(2) 0.013(3) -0.009(3) O13 0.026(3) 0.190(8) 0.052(4) 0.062(4) 0.007(3) -0.009(4) _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 Co1 C41 1.871(6) . ? Co1 C36 1.876(7) . ? Co1 C31 1.881(6) . ? Co1 C2 2.004(5) . ? Co1 C1 2.009(5) . ? Co1 C4 2.052(5) . ? Co1 C3 2.054(5) . ? Si1 O1 1.619(5) . ? Si1 O2 1.632(5) . ? Si1 C8 1.852(7) . ? Si1 C9 1.877(7) . ? O1 C5 1.442(7) . ? O2 C10 1.436(7) . ? Si2 O3 1.620(4) . ? Si2 O4 1.648(4) . ? Si2 C16 1.845(6) . ? Si2 C17 1.855(6) . ? O3 C18 1.433(7) . ? O4 C13 1.431(7) . ? C1 C4 1.471(8) . ? C1 C2 1.479(7) . ? C1 C5 1.518(8) . ? C2 C3 1.480(8) . ? C2 C10 1.526(8) . ? C3 C4 1.459(7) . ? C3 C18 1.526(7) . ? C4 C13 1.522(8) . ? C5 C6 1.520(8) . ? C5 C7 1.533(8) . ? C10 C11 1.526(8) . ? C10 C12 1.530(8) . ? C13 C14 1.519(8) . ? C13 C15 1.525(8) . ? C18 C19 1.513(8) . ? C18 C20 1.543(8) . ? C31 N1 1.141(7) . ? N1 C32 1.469(8) . ? C32 C34 1.493(11) . ? C32 C35 1.497(10) . ? C32 C33 1.507(10) . ? C36 N2 1.145(8) . ? N2 C37 1.474(9) . ? C37 C39 1.470(16) . ? C37 C38 1.470(12) . ? C37 C40 1.559(15) . ? C41 N3 1.145(7) . ? N3 C42 1.467(8) . ? C42 C43 1.514(11) . ? C42 C45 1.519(12) . ? C42 C44 1.523(11) . ? N4 O13 1.201(7) . ? N4 O12 1.233(7) . ? N4 O11 1.263(7) . ? C51 C57 0.953(16) . ? C51 C55 1.44(2) . ? C51 C52 1.52(2) . ? C51 C56 1.85(2) . ? C52 C57 1.158(15) . ? C52 C53 1.344(15) . ? C53 C54 1.643(14) . ? C54 C58 1.213(17) . ? C54 C55 1.882(18) . ? C55 C56 0.939(18) . ? C55 C58 1.184(19) . ? C56 C58 1.98(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 C41 Co1 C36 91.6(3) . . ? C41 Co1 C31 90.6(2) . . ? C36 Co1 C31 91.2(3) . . ? C41 Co1 C2 104.6(2) . . ? C36 Co1 C2 108.6(2) . . ? C31 Co1 C2 154.3(2) . . ? C41 Co1 C1 95.8(2) . . ? C36 Co1 C1 151.9(2) . . ? C31 Co1 C1 115.7(2) . . ? C2 Co1 C1 43.2(2) . . ? C41 Co1 C4 133.8(2) . . ? C36 Co1 C4 134.4(2) . . ? C31 Co1 C4 92.8(2) . . ? C2 Co1 C4 61.7(2) . . ? C1 Co1 C4 42.4(2) . . ? C41 Co1 C3 147.4(2) . . ? C36 Co1 C3 99.0(2) . . ? C31 Co1 C3 119.7(2) . . ? C2 Co1 C3 42.8(2) . . ? C1 Co1 C3 61.7(2) . . ? C4 Co1 C3 41.6(2) . . ? O1 Si1 O2 109.4(2) . . ? O1 Si1 C8 108.8(3) . . ? O2 Si1 C8 103.7(3) . . ? O1 Si1 C9 111.9(3) . . ? O2 Si1 C9 114.6(3) . . ? C8 Si1 C9 107.8(4) . . ? C5 O1 Si1 135.7(4) . . ? C10 O2 Si1 129.7(4) . . ? O3 Si2 O4 108.2(2) . . ? O3 Si2 C16 116.3(3) . . ? O4 Si2 C16 105.0(3) . . ? O3 Si2 C17 104.3(3) . . ? O4 Si2 C17 112.0(3) . . ? C16 Si2 C17 111.3(3) . . ? C18 O3 Si2 133.9(4) . . ? C13 O4 Si2 127.4(4) . . ? C4 C1 C2 89.7(4) . . ? C4 C1 C5 134.9(5) . . ? C2 C1 C5 133.7(5) . . ? C4 C1 Co1 70.3(3) . . ? C2 C1 Co1 68.2(3) . . ? C5 C1 Co1 129.8(4) . . ? C1 C2 C3 89.5(4) . . ? C1 C2 C10 132.9(5) . . ? C3 C2 C10 133.7(5) . . ? C1 C2 Co1 68.6(3) . . ? C3 C2 Co1 70.4(3) . . ? C10 C2 Co1 134.4(4) . . ? C4 C3 C2 90.1(4) . . ? C4 C3 C18 132.3(5) . . ? C2 C3 C18 135.6(5) . . ? C4 C3 Co1 69.1(3) . . ? C2 C3 Co1 66.8(3) . . ? C18 C3 Co1 132.9(4) . . ? C3 C4 C1 90.7(4) . . ? C3 C4 C13 129.9(5) . . ? C1 C4 C13 137.7(5) . . ? C3 C4 Co1 69.3(3) . . ? C1 C4 Co1 67.2(3) . . ? C13 C4 Co1 131.8(4) . . ? O1 C5 C1 110.1(5) . . ? O1 C5 C6 104.0(5) . . ? C1 C5 C6 115.0(5) . . ? O1 C5 C7 110.1(5) . . ? C1 C5 C7 107.9(5) . . ? C6 C5 C7 109.7(5) . . ? O2 C10 C11 104.5(5) . . ? O2 C10 C2 110.2(4) . . ? C11 C10 C2 113.0(5) . . ? O2 C10 C12 108.9(5) . . ? C11 C10 C12 110.2(5) . . ? C2 C10 C12 109.9(5) . . ? O4 C13 C14 104.9(5) . . ? O4 C13 C4 108.4(4) . . ? C14 C13 C4 115.1(5) . . ? O4 C13 C15 112.1(5) . . ? C14 C13 C15 108.9(5) . . ? C4 C13 C15 107.4(5) . . ? O3 C18 C19 108.0(5) . . ? O3 C18 C3 110.4(4) . . ? C19 C18 C3 115.7(5) . . ? O3 C18 C20 103.9(4) . . ? C19 C18 C20 109.4(5) . . ? C3 C18 C20 108.8(5) . . ? N1 C31 Co1 173.1(5) . . ? C31 N1 C32 179.4(7) . . ? N1 C32 C34 107.8(6) . . ? N1 C32 C35 108.7(5) . . ? C34 C32 C35 111.3(8) . . ? N1 C32 C33 107.6(5) . . ? C34 C32 C33 110.0(7) . . ? C35 C32 C33 111.3(7) . . ? N2 C36 Co1 172.6(5) . . ? C36 N2 C37 171.3(9) . . ? C39 C37 C38 114.8(10) . . ? C39 C37 N2 108.2(9) . . ? C38 C37 N2 108.6(6) . . ? C39 C37 C40 109.9(10) . . ? C38 C37 C40 109.5(11) . . ? N2 C37 C40 105.4(7) . . ? N3 C41 Co1 171.2(5) . . ? C41 N3 C42 172.8(7) . . ? N3 C42 C43 107.4(6) . . ? N3 C42 C45 105.4(6) . . ? C43 C42 C45 110.6(8) . . ? N3 C42 C44 107.6(6) . . ? C43 C42 C44 112.1(6) . . ? C45 C42 C44 113.2(9) . . ? O13 N4 O12 120.4(7) . . ? O13 N4 O11 122.8(7) . . ? O12 N4 O11 116.8(6) . . ? C57 C51 C55 127.1(18) . . ? C57 C51 C52 49.4(11) . . ? C55 C51 C52 112.0(13) . . ? C57 C51 C56 139.6(17) . . ? C55 C51 C56 30.1(8) . . ? C52 C51 C56 142.0(13) . . ? C57 C52 C53 137.6(14) . . ? C57 C52 C51 38.7(8) . . ? C53 C52 C51 99.1(11) . . ? C52 C53 C54 106.5(9) . . ? C58 C54 C53 121.9(12) . . ? C58 C54 C55 37.7(9) . . ? C53 C54 C55 94.3(7) . . ? C56 C55 C58 137(2) . . ? C56 C55 C51 99.7(18) . . ? C58 C55 C51 122.9(16) . . ? C56 C55 C54 146.9(17) . . ? C58 C55 C54 38.8(10) . . ? C51 C55 C54 96.7(10) . . ? C55 C56 C51 50.2(13) . . ? C55 C56 C58 23.9(12) . . ? C51 C56 C58 74.1(9) . . ? C51 C57 C52 91.9(16) . . ? C55 C58 C54 103.4(16) . . ? C55 C58 C56 18.7(9) . . ? C54 C58 C56 114.5(13) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.59 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.426 _refine_diff_density_min -0.543 _refine_diff_density_rms 0.103 #===END data_cs46 _database_code_depnum_ccdc_archive 'CCDC 243857' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cs46 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H38 O4 Si2' _chemical_formula_weight 398.68 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.2120(13) _cell_length_b 18.4130(15) _cell_length_c 15.2419(12) _cell_angle_alpha 90.00 _cell_angle_beta 94.735(2) _cell_angle_gamma 90.00 _cell_volume 4534.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9325 _exptl_absorpt_correction_T_max 0.9825 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23391 _diffrn_reflns_av_R_equivalents 0.0427 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _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 1.68 _diffrn_reflns_theta_max 28.32 _reflns_number_total 5647 _reflns_number_gt 4757 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+10.2425P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5647 _refine_ls_number_parameters 255 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0797 _refine_ls_wR_factor_ref 0.2006 _refine_ls_wR_factor_gt 0.1916 _refine_ls_goodness_of_fit_ref 1.153 _refine_ls_restrained_S_all 1.153 _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.003 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 0.05711(4) 0.37804(4) 0.55684(5) 0.01789(18) Uani 1 1 d . . . O1 O 0.13073(11) 0.43838(10) 0.57123(11) 0.0210(4) Uani 1 1 d . . . O2 O 0.07126(11) 0.31494(9) 0.63173(12) 0.0198(4) Uani 1 1 d . . . Si2 Si 0.40251(6) 0.37163(5) 0.94430(5) 0.0338(2) Uani 1 1 d . . . O3 O 0.40777(11) 0.32532(11) 0.85476(13) 0.0255(4) Uani 1 1 d . . . O4 O 0.34753(11) 0.44505(10) 0.92596(12) 0.0219(4) Uani 1 1 d . . . C1 C 0.25324(17) 0.42087(14) 0.80227(18) 0.0236(6) Uani 1 1 d . . . C2 C 0.20554(14) 0.41574(13) 0.71253(16) 0.0168(5) Uani 1 1 d . . . C3 C 0.19996(17) 0.34191(14) 0.71717(18) 0.0241(6) Uani 1 1 d . . . C4 C 0.26190(15) 0.33607(13) 0.79780(17) 0.0191(5) Uani 1 1 d . . . H4 H 0.239(2) 0.313(2) 0.851(2) 0.040(10) Uiso 1 1 d . . . C5 C 0.16708(16) 0.47200(13) 0.65017(16) 0.0199(5) Uani 1 1 d . . . C6 C 0.10007(18) 0.51314(16) 0.6955(2) 0.0292(6) Uani 1 1 d . . . H6A H 0.0735 0.5487 0.6545 0.044 Uiso 1 1 calc R . . H6B H 0.1254 0.5383 0.7476 0.044 Uiso 1 1 calc R . . H6C H 0.0585 0.4787 0.7133 0.044 Uiso 1 1 calc R . . C7 C 0.22923(19) 0.52489(16) 0.61819(19) 0.0302(6) Uani 1 1 d . . . H7A H 0.2733 0.4980 0.5921 0.045 Uiso 1 1 calc R . . H7B H 0.2531 0.5539 0.6679 0.045 Uiso 1 1 calc R . . H7C H 0.2016 0.5571 0.5738 0.045 Uiso 1 1 calc R . . C8 C -0.04926(17) 0.41096(16) 0.5697(2) 0.0278(6) Uani 1 1 d . . . H8A H -0.0892 0.3730 0.5508 0.042 Uiso 1 1 calc R . . H8B H -0.0602 0.4544 0.5334 0.042 Uiso 1 1 calc R . . H8C H -0.0547 0.4229 0.6316 0.042 Uiso 1 1 calc R . . C9 C 0.06374(18) 0.34650(16) 0.44220(18) 0.0282(6) Uani 1 1 d . . . H9A H 0.1201 0.3296 0.4349 0.042 Uiso 1 1 calc R . . H9B H 0.0500 0.3867 0.4014 0.042 Uiso 1 1 calc R . . H9C H 0.0246 0.3066 0.4296 0.042 Uiso 1 1 calc R . . C10 C 0.14827(15) 0.28407(13) 0.66810(16) 0.0176(5) Uani 1 1 d . . . C11 C 0.12167(18) 0.22631(16) 0.7313(2) 0.0300(6) Uani 1 1 d . . . H11A H 0.0909 0.2492 0.7767 0.045 Uiso 1 1 calc R . . H11B H 0.1708 0.2019 0.7592 0.045 Uiso 1 1 calc R . . H11C H 0.0862 0.1907 0.6988 0.045 Uiso 1 1 calc R . . C12 C 0.19265(17) 0.25014(15) 0.59400(18) 0.0251(6) Uani 1 1 d . . . H12A H 0.1541 0.2190 0.5583 0.038 Uiso 1 1 calc R . . H12B H 0.2394 0.2210 0.6191 0.038 Uiso 1 1 calc R . . H12C H 0.2131 0.2886 0.5570 0.038 Uiso 1 1 calc R . . C13 C 0.34609(16) 0.30041(15) 0.7867(2) 0.0263(6) Uani 1 1 d . . . C14 C 0.3430(2) 0.21864(16) 0.7964(2) 0.0344(7) Uani 1 1 d . . . H14A H 0.3988 0.1986 0.7943 0.052 Uiso 1 1 calc R . . H14B H 0.3064 0.1981 0.7483 0.052 Uiso 1 1 calc R . . H14C H 0.3218 0.2063 0.8529 0.052 Uiso 1 1 calc R . . C15 C 0.37933(17) 0.31982(18) 0.6981(2) 0.0312(7) Uani 1 1 d . . . H15A H 0.3733 0.3721 0.6877 0.047 Uiso 1 1 calc R . . H15B H 0.3479 0.2932 0.6507 0.047 Uiso 1 1 calc R . . H15C H 0.4379 0.3065 0.6994 0.047 Uiso 1 1 calc R . . C16 C 0.3513(4) 0.3195(2) 1.0296(3) 0.0714(16) Uani 1 1 d . . . H16A H 0.2935 0.3100 1.0086 0.107 Uiso 1 1 calc R . . H16B H 0.3531 0.3479 1.0841 0.107 Uiso 1 1 calc R . . H16C H 0.3803 0.2733 1.0408 0.107 Uiso 1 1 calc R . . C17 C 0.5100(3) 0.3944(3) 0.9808(4) 0.086(2) Uani 1 1 d . . . H17A H 0.5422 0.3497 0.9900 0.128 Uiso 1 1 calc R . . H17B H 0.5114 0.4217 1.0362 0.128 Uiso 1 1 calc R . . H17C H 0.5337 0.4241 0.9358 0.128 Uiso 1 1 calc R . . C18 C 0.31904(15) 0.47445(13) 0.84106(16) 0.0180(5) Uani 1 1 d . . . C19 C 0.27710(19) 0.54529(15) 0.8637(2) 0.0299(6) Uani 1 1 d . . . H19A H 0.2299 0.5348 0.8978 0.045 Uiso 1 1 calc R . . H19B H 0.2577 0.5706 0.8092 0.045 Uiso 1 1 calc R . . H19C H 0.3168 0.5761 0.8984 0.045 Uiso 1 1 calc R . . C20 C 0.39323(17) 0.49111(18) 0.7892(2) 0.0302(6) Uani 1 1 d . . . H20A H 0.4253 0.5310 0.8178 0.045 Uiso 1 1 calc R . . H20B H 0.3739 0.5052 0.7290 0.045 Uiso 1 1 calc R . . H20C H 0.4283 0.4478 0.7876 0.045 Uiso 1 1 calc R . . H1 H 0.204(2) 0.4265(19) 0.848(2) 0.035(9) 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 0.0169(3) 0.0181(3) 0.0178(3) 0.0005(2) -0.0037(2) -0.0005(2) O1 0.0229(9) 0.0225(9) 0.0165(8) 0.0040(7) -0.0053(7) -0.0064(7) O2 0.0165(8) 0.0194(9) 0.0225(9) 0.0037(7) -0.0037(7) -0.0004(7) Si2 0.0438(5) 0.0327(5) 0.0221(4) -0.0074(3) -0.0134(3) 0.0230(4) O3 0.0201(9) 0.0256(10) 0.0291(10) -0.0094(8) -0.0090(8) 0.0085(7) O4 0.0253(9) 0.0209(9) 0.0184(9) -0.0029(7) -0.0060(7) 0.0073(7) C1 0.0254(13) 0.0144(11) 0.0284(13) 0.0019(10) -0.0127(11) 0.0005(10) C2 0.0145(11) 0.0164(11) 0.0187(11) 0.0010(9) -0.0030(9) -0.0001(9) C3 0.0238(13) 0.0181(12) 0.0282(13) -0.0032(10) -0.0101(11) 0.0038(10) C4 0.0194(11) 0.0170(11) 0.0199(12) -0.0011(9) -0.0034(9) 0.0053(9) C5 0.0237(12) 0.0164(11) 0.0185(11) 0.0025(9) -0.0054(9) -0.0023(9) C6 0.0305(14) 0.0258(14) 0.0299(14) -0.0015(11) -0.0056(11) 0.0085(11) C7 0.0360(15) 0.0247(14) 0.0279(14) 0.0084(11) -0.0089(12) -0.0118(12) C8 0.0220(13) 0.0287(14) 0.0317(15) 0.0000(11) -0.0035(11) 0.0027(11) C9 0.0303(14) 0.0320(15) 0.0209(13) -0.0031(11) -0.0058(11) 0.0028(12) C10 0.0179(11) 0.0140(10) 0.0203(11) 0.0011(9) -0.0033(9) -0.0004(9) C11 0.0293(14) 0.0287(15) 0.0305(15) 0.0119(12) -0.0066(11) -0.0058(11) C12 0.0259(13) 0.0242(13) 0.0245(13) -0.0032(10) -0.0020(10) 0.0046(10) C13 0.0198(12) 0.0209(13) 0.0365(15) -0.0109(11) -0.0085(11) 0.0052(10) C14 0.0356(16) 0.0241(14) 0.0402(17) -0.0099(12) -0.0171(13) 0.0148(12) C15 0.0210(13) 0.0384(16) 0.0335(15) -0.0141(13) -0.0013(11) 0.0034(11) C16 0.137(5) 0.041(2) 0.038(2) 0.0109(17) 0.015(2) 0.035(3) C17 0.056(3) 0.084(3) 0.105(4) -0.070(3) -0.061(3) 0.046(2) C18 0.0190(11) 0.0149(11) 0.0190(11) -0.0023(9) -0.0055(9) 0.0013(9) C19 0.0369(16) 0.0201(13) 0.0308(14) -0.0040(11) -0.0079(12) 0.0092(11) C20 0.0206(13) 0.0403(17) 0.0287(14) 0.0002(12) -0.0044(11) -0.0077(12) _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 O1 1.6321(19) . ? Si1 O2 1.6318(18) . ? Si1 C8 1.853(3) . ? Si1 C9 1.853(3) . ? O1 C5 1.436(3) . ? O2 C10 1.440(3) . ? Si2 O3 1.617(2) . ? Si2 O4 1.6306(19) . ? Si2 C17 1.834(4) . ? Si2 C16 1.864(5) . ? O3 C13 1.454(3) . ? O4 C18 1.443(3) . ? C1 C2 1.518(3) . ? C1 C18 1.535(3) . ? C1 C4 1.570(3) . ? C2 C3 1.365(4) . ? C2 C5 1.506(3) . ? C3 C10 1.514(3) . ? C3 C4 1.525(3) . ? C4 C13 1.537(3) . ? C5 C7 1.511(4) . ? C5 C6 1.535(4) . ? C10 C11 1.521(4) . ? C10 C12 1.522(4) . ? C13 C14 1.514(4) . ? C13 C15 1.537(4) . ? C18 C19 1.524(4) . ? C18 C20 1.524(4) . ? 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 O1 Si1 O2 109.37(9) . . ? O1 Si1 C8 116.09(12) . . ? O2 Si1 C8 103.72(12) . . ? O1 Si1 C9 103.97(12) . . ? O2 Si1 C9 114.88(12) . . ? C8 Si1 C9 109.21(13) . . ? C5 O1 Si1 130.63(16) . . ? C10 O2 Si1 128.14(16) . . ? O3 Si2 O4 111.01(10) . . ? O3 Si2 C17 105.19(17) . . ? O4 Si2 C17 110.75(18) . . ? O3 Si2 C16 111.99(17) . . ? O4 Si2 C16 106.10(16) . . ? C17 Si2 C16 111.9(3) . . ? C13 O3 Si2 133.41(17) . . ? C18 O4 Si2 126.49(16) . . ? C2 C1 C18 132.3(2) . . ? C2 C1 C4 86.55(18) . . ? C18 C1 C4 126.5(2) . . ? C3 C2 C5 133.8(2) . . ? C3 C2 C1 92.7(2) . . ? C5 C2 C1 132.8(2) . . ? C2 C3 C10 135.4(2) . . ? C2 C3 C4 94.0(2) . . ? C10 C3 C4 130.5(2) . . ? C3 C4 C13 118.2(2) . . ? C3 C4 C1 84.81(18) . . ? C13 C4 C1 120.9(2) . . ? O1 C5 C2 110.6(2) . . ? O1 C5 C7 104.3(2) . . ? C2 C5 C7 113.2(2) . . ? O1 C5 C6 109.5(2) . . ? C2 C5 C6 109.1(2) . . ? C7 C5 C6 110.1(2) . . ? O2 C10 C3 109.84(19) . . ? O2 C10 C11 103.7(2) . . ? C3 C10 C11 110.7(2) . . ? O2 C10 C12 108.9(2) . . ? C3 C10 C12 112.3(2) . . ? C11 C10 C12 111.0(2) . . ? O3 C13 C14 105.7(2) . . ? O3 C13 C4 110.6(2) . . ? C14 C13 C4 112.2(2) . . ? O3 C13 C15 106.5(2) . . ? C14 C13 C15 109.5(2) . . ? C4 C13 C15 112.1(2) . . ? O4 C18 C19 103.6(2) . . ? O4 C18 C20 109.4(2) . . ? C19 C18 C20 109.3(2) . . ? O4 C18 C1 105.4(2) . . ? C19 C18 C1 109.2(2) . . ? C20 C18 C1 118.9(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.381 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.097 #===END data_cs47 _database_code_depnum_ccdc_archive 'CCDC 243858' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common cs47 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H38 O4 Si2' _chemical_formula_weight 398.68 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.4042(9) _cell_length_b 11.8988(9) _cell_length_c 17.095(1) _cell_angle_alpha 90.00 _cell_angle_beta 103.263(1) _cell_angle_gamma 90.00 _cell_volume 2257.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5502 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.33 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9420 _exptl_absorpt_correction_T_max 0.9790 _exptl_absorpt_process_details 'Blessing, Acta Cryst. (1995) A51 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23368 _diffrn_reflns_av_R_equivalents 0.0229 _diffrn_reflns_av_sigmaI/netI 0.0195 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.34 _reflns_number_total 5607 _reflns_number_gt 5024 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.8257P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5607 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0933 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 -0.07545(3) 0.72733(3) 0.20649(2) 0.01889(9) Uani 1 1 d . . . Si2 Si 0.43909(3) 0.77944(3) 0.043184(19) 0.01587(9) Uani 1 1 d . . . O1 O -0.09526(7) 0.68583(7) 0.11297(5) 0.01753(17) Uani 1 1 d . . . O2 O 0.06155(8) 0.77601(7) 0.23620(5) 0.01984(18) Uani 1 1 d . . . O3 O 0.44351(7) 0.72425(7) 0.13183(5) 0.01652(17) Uani 1 1 d . . . O4 O 0.34616(7) 0.70876(7) -0.02702(5) 0.01721(17) Uani 1 1 d . . . C1 C 0.19255(10) 0.67395(9) 0.04710(6) 0.0141(2) Uani 1 1 d . . . C2 C 0.09875(10) 0.69311(9) 0.08129(6) 0.0139(2) Uani 1 1 d . . . C3 C 0.15948(10) 0.64387(9) 0.16257(6) 0.0135(2) Uani 1 1 d . . . C4 C 0.26342(10) 0.60574(9) 0.11889(6) 0.0134(2) Uani 1 1 d . . . C5 C -0.03372(10) 0.72566(10) 0.05367(7) 0.0163(2) Uani 1 1 d . . . C6 C -0.09487(11) 0.66139(11) -0.02216(7) 0.0198(2) Uani 1 1 d . . . C7 C -0.05159(12) 0.85265(11) 0.04227(9) 0.0241(3) Uani 1 1 d . . . C8 C -0.11033(13) 0.60401(13) 0.26340(8) 0.0282(3) Uani 1 1 d . . . C9 C -0.17561(13) 0.84508(13) 0.21910(10) 0.0309(3) Uani 1 1 d . . . C10 C 0.17677(10) 0.72444(10) 0.23555(7) 0.0162(2) Uani 1 1 d . . . C11 C 0.25899(11) 0.82407(10) 0.23126(8) 0.0195(2) Uani 1 1 d . . . C12 C 0.21348(12) 0.65990(12) 0.31456(7) 0.0225(3) Uani 1 1 d . . . C13 C 0.40285(10) 0.61342(9) 0.14622(7) 0.0153(2) Uani 1 1 d . . . C14 C 0.45379(11) 0.58925(11) 0.23502(7) 0.0198(2) Uani 1 1 d . . . C15 C 0.45693(11) 0.52534(11) 0.09894(8) 0.0202(2) Uani 1 1 d . . . C16 C 0.39444(13) 0.92803(11) 0.05075(9) 0.0249(3) Uani 1 1 d . . . C17 C 0.58572(12) 0.76759(12) 0.01502(9) 0.0237(3) Uani 1 1 d . . . C18 C 0.21861(10) 0.69071(10) -0.03533(7) 0.0170(2) Uani 1 1 d . . . C19 C 0.18842(12) 0.58420(12) -0.08570(7) 0.0243(3) Uani 1 1 d . . . C20 C 0.15498(12) 0.79218(13) -0.08091(8) 0.0260(3) Uani 1 1 d . . . H3 H 0.1182(12) 0.5795(11) 0.1765(8) 0.009(3) Uiso 1 1 d . . . H4 H 0.2463(13) 0.5269(13) 0.1085(9) 0.018(3) Uiso 1 1 d . . . H6A H -0.0776(15) 0.5811(15) -0.0140(10) 0.029(4) Uiso 1 1 d . . . H6B H -0.0684(15) 0.6848(14) -0.0684(10) 0.025(4) Uiso 1 1 d . . . H6C H -0.1801(15) 0.6724(14) -0.0319(9) 0.026(4) Uiso 1 1 d . . . H7A H -0.0163(15) 0.8792(14) -0.0008(11) 0.031(4) Uiso 1 1 d . . . H7B H -0.0150(14) 0.8909(13) 0.0903(10) 0.022(4) Uiso 1 1 d . . . H7C H -0.1367(16) 0.8695(14) 0.0265(10) 0.029(4) Uiso 1 1 d . . . H8A H -0.0603(16) 0.5384(15) 0.2585(11) 0.033(4) Uiso 1 1 d . . . H8B H -0.1000(17) 0.6247(16) 0.3188(12) 0.041(5) Uiso 1 1 d . . . H8C H -0.1922(19) 0.5841(17) 0.2426(12) 0.047(5) Uiso 1 1 d . . . H9A H -0.1702(18) 0.9057(17) 0.1854(12) 0.045(5) Uiso 1 1 d . . . H9B H -0.2595(17) 0.8153(16) 0.2071(11) 0.040(5) Uiso 1 1 d . . . H9C H -0.1538(18) 0.8703(17) 0.2734(12) 0.045(5) Uiso 1 1 d . . . H11A H 0.2250(15) 0.8693(14) 0.1825(10) 0.027(4) Uiso 1 1 d . . . H11B H 0.3391(15) 0.8008(13) 0.2295(9) 0.022(4) Uiso 1 1 d . . . H11C H 0.2622(15) 0.8728(15) 0.2767(10) 0.032(4) Uiso 1 1 d . . . H12A H 0.1579(15) 0.6015(14) 0.3166(10) 0.028(4) Uiso 1 1 d . . . H12B H 0.2141(15) 0.7101(14) 0.3589(10) 0.027(4) Uiso 1 1 d . . . H12C H 0.2934(15) 0.6248(14) 0.3217(10) 0.029(4) Uiso 1 1 d . . . H14A H 0.4368(14) 0.6513(13) 0.2688(9) 0.021(4) Uiso 1 1 d . . . H14B H 0.5399(15) 0.5843(14) 0.2432(10) 0.027(4) Uiso 1 1 d . . . H14C H 0.4221(14) 0.5189(14) 0.2513(9) 0.025(4) Uiso 1 1 d . . . H15A H 0.5429(15) 0.5354(13) 0.1093(9) 0.023(4) Uiso 1 1 d . . . H15B H 0.4396(14) 0.4502(14) 0.1174(9) 0.023(4) Uiso 1 1 d . . . H15C H 0.4262(15) 0.5305(14) 0.0411(10) 0.027(4) Uiso 1 1 d . . . H16A H 0.3220(17) 0.9329(15) 0.0684(11) 0.038(5) Uiso 1 1 d . . . H16B H 0.3843(15) 0.9680(15) -0.0004(11) 0.034(4) Uiso 1 1 d . . . H16C H 0.4588(17) 0.9661(16) 0.0891(11) 0.040(5) Uiso 1 1 d . . . H17A H 0.6083(17) 0.6936(17) 0.0136(11) 0.040(5) Uiso 1 1 d . . . H17B H 0.6449(17) 0.8074(16) 0.0508(11) 0.037(5) Uiso 1 1 d . . . H17C H 0.5797(17) 0.7985(17) -0.0376(12) 0.043(5) Uiso 1 1 d . . . H19A H 0.2356(15) 0.5156(15) -0.0563(11) 0.033(4) Uiso 1 1 d . . . H19B H 0.2104(16) 0.5966(15) -0.1361(11) 0.036(5) Uiso 1 1 d . . . H19C H 0.1013(16) 0.5692(14) -0.0975(10) 0.030(4) Uiso 1 1 d . . . H20A H 0.1722(15) 0.8597(15) -0.0480(10) 0.029(4) Uiso 1 1 d . . . H20B H 0.1821(16) 0.8035(15) -0.1283(11) 0.034(4) Uiso 1 1 d . . . H20C H 0.0708(17) 0.7813(14) -0.0976(10) 0.032(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 0.01547(16) 0.02337(18) 0.01972(17) -0.00643(12) 0.00794(12) -0.00386(12) Si2 0.01478(15) 0.01617(16) 0.01811(16) -0.00088(11) 0.00673(12) -0.00239(11) O1 0.0148(4) 0.0217(4) 0.0172(4) -0.0023(3) 0.0061(3) -0.0027(3) O2 0.0159(4) 0.0229(4) 0.0223(4) -0.0088(3) 0.0078(3) -0.0027(3) O3 0.0163(4) 0.0167(4) 0.0169(4) -0.0016(3) 0.0043(3) -0.0039(3) O4 0.0145(4) 0.0224(4) 0.0162(4) -0.0008(3) 0.0064(3) -0.0036(3) C1 0.0145(5) 0.0147(5) 0.0126(5) -0.0004(4) 0.0022(4) -0.0022(4) C2 0.0139(5) 0.0137(5) 0.0138(5) -0.0005(4) 0.0025(4) -0.0017(4) C3 0.0137(5) 0.0142(5) 0.0127(5) -0.0011(4) 0.0036(4) -0.0017(4) C4 0.0140(5) 0.0145(5) 0.0120(5) -0.0007(4) 0.0037(4) -0.0011(4) C5 0.0138(5) 0.0182(5) 0.0173(5) 0.0012(4) 0.0043(4) -0.0007(4) C6 0.0144(5) 0.0279(6) 0.0162(5) 0.0012(5) 0.0016(4) -0.0017(5) C7 0.0200(6) 0.0199(6) 0.0328(7) 0.0043(5) 0.0067(5) 0.0032(5) C8 0.0291(7) 0.0368(8) 0.0213(6) -0.0030(5) 0.0107(5) -0.0117(6) C9 0.0202(6) 0.0360(8) 0.0387(8) -0.0159(6) 0.0116(6) -0.0002(5) C10 0.0146(5) 0.0195(5) 0.0153(5) -0.0041(4) 0.0048(4) -0.0023(4) C11 0.0176(5) 0.0196(6) 0.0224(6) -0.0067(5) 0.0069(4) -0.0035(4) C12 0.0235(6) 0.0311(7) 0.0136(5) -0.0019(5) 0.0055(4) -0.0049(5) C13 0.0146(5) 0.0151(5) 0.0160(5) -0.0004(4) 0.0034(4) -0.0009(4) C14 0.0171(5) 0.0237(6) 0.0171(5) 0.0013(5) 0.0011(4) 0.0006(4) C15 0.0193(6) 0.0198(6) 0.0222(6) -0.0022(5) 0.0065(5) 0.0031(4) C16 0.0289(7) 0.0182(6) 0.0310(7) -0.0003(5) 0.0139(6) -0.0008(5) C17 0.0181(6) 0.0271(7) 0.0280(7) -0.0009(5) 0.0101(5) -0.0030(5) C18 0.0140(5) 0.0235(6) 0.0139(5) 0.0016(4) 0.0040(4) -0.0034(4) C19 0.0247(6) 0.0340(7) 0.0159(5) -0.0073(5) 0.0082(5) -0.0110(5) C20 0.0201(6) 0.0356(7) 0.0220(6) 0.0131(5) 0.0042(5) -0.0009(5) _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 O2 1.6342(9) . ? Si1 O1 1.6386(9) . ? Si1 C9 1.8514(15) . ? Si1 C8 1.8535(15) . ? Si2 O4 1.6392(9) . ? Si2 O3 1.6417(9) . ? Si2 C17 1.8487(13) . ? Si2 C16 1.8525(14) . ? O1 C5 1.4391(13) . ? O2 C10 1.4525(14) . ? O3 C13 1.4377(13) . ? O4 C18 1.4448(13) . ? C1 C2 1.3508(15) . ? C1 C18 1.5185(15) . ? C1 C4 1.5372(15) . ? C2 C3 1.5206(15) . ? C2 C5 1.5258(15) . ? C3 C10 1.5497(15) . ? C3 C4 1.6047(15) . ? C3 H3 0.958(14) . ? C4 C13 1.5537(15) . ? C4 H4 0.967(15) . ? C5 C6 1.5287(16) . ? C5 C7 1.5311(17) . ? C6 H6A 0.979(18) . ? C6 H6B 0.950(17) . ? C6 H6C 0.957(17) . ? C7 H7A 0.969(18) . ? C7 H7B 0.947(16) . ? C7 H7C 0.966(17) . ? C8 H8A 0.982(18) . ? C8 H8B 0.96(2) . ? C8 H8C 0.95(2) . ? C9 H9A 0.93(2) . ? C9 H9B 1.00(2) . ? C9 H9C 0.95(2) . ? C10 C11 1.5236(16) . ? C10 C12 1.5264(17) . ? C11 H11A 0.993(17) . ? C11 H11B 0.962(16) . ? C11 H11C 0.964(18) . ? C12 H12A 0.946(17) . ? C12 H12B 0.964(17) . ? C12 H12C 0.985(17) . ? C13 C14 1.5231(16) . ? C13 C15 1.5365(16) . ? C14 H14A 0.984(16) . ? C14 H14B 0.962(17) . ? C14 H14C 0.977(17) . ? C15 H15A 0.963(16) . ? C15 H15B 0.983(16) . ? C15 H15C 0.973(17) . ? C16 H16A 0.945(19) . ? C16 H16B 0.979(18) . ? C16 H16C 0.976(19) . ? C17 H17A 0.92(2) . ? C17 H17B 0.930(19) . ? C17 H17C 0.96(2) . ? C18 C19 1.5265(17) . ? C18 C20 1.5270(18) . ? C19 H19A 1.041(18) . ? C19 H19B 0.962(18) . ? C19 H19C 0.983(17) . ? C20 H20A 0.974(18) . ? C20 H20B 0.941(19) . ? C20 H20C 0.945(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Si1 O1 108.55(4) . . ? O2 Si1 C9 105.48(6) . . ? O1 Si1 C9 113.01(6) . . ? O2 Si1 C8 114.99(6) . . ? O1 Si1 C8 105.99(6) . . ? C9 Si1 C8 109.00(7) . . ? O4 Si2 O3 110.39(4) . . ? O4 Si2 C17 103.99(5) . . ? O3 Si2 C17 111.83(6) . . ? O4 Si2 C16 113.51(6) . . ? O3 Si2 C16 105.55(5) . . ? C17 Si2 C16 111.75(6) . . ? C5 O1 Si1 127.42(7) . . ? C10 O2 Si1 130.54(7) . . ? C13 O3 Si2 125.60(7) . . ? C18 O4 Si2 127.99(7) . . ? C2 C1 C18 136.26(10) . . ? C2 C1 C4 93.85(9) . . ? C18 C1 C4 129.13(10) . . ? C1 C2 C3 95.20(9) . . ? C1 C2 C5 137.31(10) . . ? C3 C2 C5 126.28(9) . . ? C2 C3 C10 116.38(9) . . ? C2 C3 C4 85.06(8) . . ? C10 C3 C4 125.34(9) . . ? C2 C3 H3 112.9(8) . . ? C10 C3 H3 105.9(8) . . ? C4 C3 H3 110.3(8) . . ? C1 C4 C13 121.56(9) . . ? C1 C4 C3 85.01(8) . . ? C13 C4 C3 131.12(9) . . ? C1 C4 H4 108.6(9) . . ? C13 C4 H4 105.2(9) . . ? C3 C4 H4 102.7(9) . . ? O1 C5 C2 107.86(9) . . ? O1 C5 C6 103.37(9) . . ? C2 C5 C6 111.23(9) . . ? O1 C5 C7 110.03(10) . . ? C2 C5 C7 112.54(10) . . ? C6 C5 C7 111.37(10) . . ? C5 C6 H6A 109.3(10) . . ? C5 C6 H6B 112.9(10) . . ? H6A C6 H6B 108.2(14) . . ? C5 C6 H6C 109.1(10) . . ? H6A C6 H6C 108.8(14) . . ? H6B C6 H6C 108.6(13) . . ? C5 C7 H7A 110.6(10) . . ? C5 C7 H7B 110.2(10) . . ? H7A C7 H7B 108.9(14) . . ? C5 C7 H7C 109.6(10) . . ? H7A C7 H7C 106.7(14) . . ? H7B C7 H7C 110.8(14) . . ? Si1 C8 H8A 112.7(10) . . ? Si1 C8 H8B 108.8(11) . . ? H8A C8 H8B 110.3(15) . . ? Si1 C8 H8C 108.2(12) . . ? H8A C8 H8C 108.1(16) . . ? H8B C8 H8C 108.7(16) . . ? Si1 C9 H9A 112.5(12) . . ? Si1 C9 H9B 107.2(11) . . ? H9A C9 H9B 110.1(16) . . ? Si1 C9 H9C 108.7(12) . . ? H9A C9 H9C 108.6(17) . . ? H9B C9 H9C 109.7(16) . . ? O2 C10 C11 103.85(9) . . ? O2 C10 C12 105.71(9) . . ? C11 C10 C12 112.78(10) . . ? O2 C10 C3 108.62(9) . . ? C11 C10 C3 114.12(9) . . ? C12 C10 C3 111.07(10) . . ? C10 C11 H11A 109.7(10) . . ? C10 C11 H11B 112.1(9) . . ? H11A C11 H11B 108.7(13) . . ? C10 C11 H11C 109.8(10) . . ? H11A C11 H11C 106.5(14) . . ? H11B C11 H11C 109.8(13) . . ? C10 C12 H12A 110.6(10) . . ? C10 C12 H12B 109.6(10) . . ? H12A C12 H12B 108.0(14) . . ? C10 C12 H12C 112.4(10) . . ? H12A C12 H12C 107.0(14) . . ? H12B C12 H12C 109.0(14) . . ? O3 C13 C14 106.23(9) . . ? O3 C13 C15 110.58(9) . . ? C14 C13 C15 106.75(10) . . ? O3 C13 C4 110.52(9) . . ? C14 C13 C4 114.75(9) . . ? C15 C13 C4 107.95(9) . . ? C13 C14 H14A 111.3(9) . . ? C13 C14 H14B 107.5(10) . . ? H14A C14 H14B 107.0(13) . . ? C13 C14 H14C 111.3(9) . . ? H14A C14 H14C 109.9(13) . . ? H14B C14 H14C 109.8(13) . . ? C13 C15 H15A 109.4(10) . . ? C13 C15 H15B 108.4(9) . . ? H15A C15 H15B 109.0(13) . . ? C13 C15 H15C 113.4(10) . . ? H15A C15 H15C 107.0(13) . . ? H15B C15 H15C 109.4(13) . . ? Si2 C16 H16A 110.8(11) . . ? Si2 C16 H16B 112.3(10) . . ? H16A C16 H16B 108.9(15) . . ? Si2 C16 H16C 108.3(11) . . ? H16A C16 H16C 109.5(16) . . ? H16B C16 H16C 106.9(15) . . ? Si2 C17 H17A 110.8(12) . . ? Si2 C17 H17B 110.7(11) . . ? H17A C17 H17B 109.8(16) . . ? Si2 C17 H17C 109.9(12) . . ? H17A C17 H17C 107.6(16) . . ? H17B C17 H17C 107.9(16) . . ? O4 C18 C1 109.59(9) . . ? O4 C18 C19 105.70(9) . . ? C1 C18 C19 110.34(10) . . ? O4 C18 C20 106.42(9) . . ? C1 C18 C20 113.95(10) . . ? C19 C18 C20 110.44(11) . . ? C18 C19 H19A 110.8(10) . . ? C18 C19 H19B 107.8(11) . . ? H19A C19 H19B 109.9(14) . . ? C18 C19 H19C 110.7(10) . . ? H19A C19 H19C 110.1(14) . . ? H19B C19 H19C 107.6(14) . . ? C18 C20 H20A 110.4(10) . . ? C18 C20 H20B 109.9(11) . . ? H20A C20 H20B 108.4(15) . . ? C18 C20 H20C 112.1(11) . . ? H20A C20 H20C 110.0(14) . . ? H20B C20 H20C 105.8(15) . . ? 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 O2 Si1 O1 C5 -25.95(10) . . . . ? C9 Si1 O1 C5 90.69(10) . . . . ? C8 Si1 O1 C5 -149.99(10) . . . . ? O1 Si1 O2 C10 -54.45(11) . . . . ? C9 Si1 O2 C10 -175.84(11) . . . . ? C8 Si1 O2 C10 64.04(12) . . . . ? O4 Si2 O3 C13 17.28(10) . . . . ? C17 Si2 O3 C13 -97.97(9) . . . . ? C16 Si2 O3 C13 140.31(9) . . . . ? O3 Si2 O4 C18 60.30(10) . . . . ? C17 Si2 O4 C18 -179.61(9) . . . . ? C16 Si2 O4 C18 -57.96(11) . . . . ? C18 C1 C2 C3 177.72(13) . . . . ? C4 C1 C2 C3 7.61(9) . . . . ? C18 C1 C2 C5 10.6(2) . . . . ? C4 C1 C2 C5 -159.50(13) . . . . ? C1 C2 C3 C10 119.95(10) . . . . ? C5 C2 C3 C10 -70.87(14) . . . . ? C1 C2 C3 C4 -7.30(8) . . . . ? C5 C2 C3 C4 161.89(11) . . . . ? C2 C1 C4 C13 -143.35(10) . . . . ? C18 C1 C4 C13 45.45(16) . . . . ? C2 C1 C4 C3 -7.20(8) . . . . ? C18 C1 C4 C3 -178.40(11) . . . . ? C2 C3 C4 C1 6.40(7) . . . . ? C10 C3 C4 C1 -112.64(11) . . . . ? C2 C3 C4 C13 134.81(12) . . . . ? C10 C3 C4 C13 15.77(18) . . . . ? Si1 O1 C5 C2 65.21(12) . . . . ? Si1 O1 C5 C6 -176.91(8) . . . . ? Si1 O1 C5 C7 -57.88(13) . . . . ? C1 C2 C5 O1 155.31(13) . . . . ? C3 C2 C5 O1 -8.69(14) . . . . ? C1 C2 C5 C6 42.62(18) . . . . ? C3 C2 C5 C6 -121.38(12) . . . . ? C1 C2 C5 C7 -83.14(17) . . . . ? C3 C2 C5 C7 112.86(12) . . . . ? Si1 O2 C10 C11 153.48(9) . . . . ? Si1 O2 C10 C12 -87.59(11) . . . . ? Si1 O2 C10 C3 31.67(14) . . . . ? C2 C3 C10 O2 52.16(12) . . . . ? C4 C3 C10 O2 155.68(10) . . . . ? C2 C3 C10 C11 -63.16(13) . . . . ? C4 C3 C10 C11 40.36(15) . . . . ? C2 C3 C10 C12 168.00(9) . . . . ? C4 C3 C10 C12 -88.47(13) . . . . ? Si2 O3 C13 C14 165.75(8) . . . . ? Si2 O3 C13 C15 50.29(12) . . . . ? Si2 O3 C13 C4 -69.18(11) . . . . ? C1 C4 C13 O3 32.47(13) . . . . ? C3 C4 C13 O3 -81.15(13) . . . . ? C1 C4 C13 C14 152.55(10) . . . . ? C3 C4 C13 C14 38.92(16) . . . . ? C1 C4 C13 C15 -88.57(12) . . . . ? C3 C4 C13 C15 157.80(11) . . . . ? Si2 O4 C18 C1 -37.76(13) . . . . ? Si2 O4 C18 C19 -156.66(8) . . . . ? Si2 O4 C18 C20 85.88(11) . . . . ? C2 C1 C18 O4 150.95(13) . . . . ? C4 C1 C18 O4 -41.80(15) . . . . ? C2 C1 C18 C19 -93.06(16) . . . . ? C4 C1 C18 C19 74.19(14) . . . . ? C2 C1 C18 C20 31.85(19) . . . . ? C4 C1 C18 C20 -160.90(11) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.411 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.052 #===END #_eof # End of Crystallographic Information File #======================================================================= data_cs44 _database_code_depnum_ccdc_archive 'CCDC 250035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '8 in paper' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H36 O5 Si2' _chemical_formula_weight 412.67 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' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.1299(2) _cell_length_b 16.3989(4) _cell_length_c 15.8666(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.5110(10) _cell_angle_gamma 90.00 _cell_volume 2342.90(10) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9588 _exptl_absorpt_correction_T_max 0.9655 _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51 33-38.' ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18957 _diffrn_reflns_av_R_equivalents 0.0620 _diffrn_reflns_av_sigmaI/netI 0.0476 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 24.41 _reflns_number_total 3858 _reflns_number_gt 2771 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0773P)^2^+0.3237P] 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 3858 _refine_ls_number_parameters 256 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0714 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.1286 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.24990(8) 0.60677(4) 0.61938(5) 0.0347(2) Uani 1 1 d . . . O1 O 0.29378(19) 0.61570(10) 0.72394(11) 0.0386(5) Uani 1 1 d . . . O2 O 0.36413(17) 0.65873(10) 0.57018(10) 0.0316(4) Uani 1 1 d . . . Si2 Si 0.60810(8) 0.95468(4) 0.63164(4) 0.0329(2) Uani 1 1 d . . . O3 O 0.45162(18) 0.91704(10) 0.57994(10) 0.0349(4) Uani 1 1 d . . . O4 O 0.63715(18) 0.91330(10) 0.72683(10) 0.0337(4) Uani 1 1 d . . . C1 C 0.5217(3) 0.67488(15) 0.59588(15) 0.0312(6) Uani 1 1 d . . . C2 C 0.5357(2) 0.74089(14) 0.66688(14) 0.0270(5) Uani 1 1 d . . . C3 C 0.4125(2) 0.74408(15) 0.72101(14) 0.0283(6) Uani 1 1 d . . . C4 C 0.3368(3) 0.68739(15) 0.77485(15) 0.0325(6) Uani 1 1 d . . . C5 C 0.7203(3) 0.84426(15) 0.76350(15) 0.0320(6) Uani 1 1 d . . . C6 C 0.6905(3) 0.76778(15) 0.70505(15) 0.0323(6) Uani 1 1 d . . . O6 O 0.79871(19) 0.73009(12) 0.68956(13) 0.0495(5) Uani 1 1 d . . . C7 C 0.4090(2) 0.80234(14) 0.66635(15) 0.0265(5) Uani 1 1 d . . . C8 C 0.3402(3) 0.87510(15) 0.61840(16) 0.0319(6) Uani 1 1 d . . . C11 C 0.6009(3) 0.59548(16) 0.62653(18) 0.0413(7) Uani 1 1 d . . . H11A H 0.5686 0.5777 0.6795 0.062 Uiso 1 1 calc R . . H11B H 0.7085 0.6045 0.6371 0.062 Uiso 1 1 calc R . . H11C H 0.5763 0.5534 0.5826 0.062 Uiso 1 1 calc R . . C12 C 0.5757(3) 0.70654(17) 0.51617(17) 0.0395(7) Uani 1 1 d . . . H12A H 0.5572 0.6654 0.4709 0.059 Uiso 1 1 calc R . . H12B H 0.6825 0.7179 0.5294 0.059 Uiso 1 1 calc R . . H12C H 0.5223 0.7568 0.4969 0.059 Uiso 1 1 calc R . . C13 C 0.4417(3) 0.65778(19) 0.85303(17) 0.0494(8) Uani 1 1 d . . . H13A H 0.3917 0.6165 0.8827 0.074 Uiso 1 1 calc R . . H13B H 0.4709 0.7038 0.8915 0.074 Uiso 1 1 calc R . . H13C H 0.5303 0.6339 0.8354 0.074 Uiso 1 1 calc R . . C14 C 0.2008(3) 0.72851(19) 0.79904(19) 0.0508(8) Uani 1 1 d . . . H14A H 0.1308 0.7418 0.7471 0.076 Uiso 1 1 calc R . . H14B H 0.2307 0.7787 0.8309 0.076 Uiso 1 1 calc R . . H14C H 0.1530 0.6916 0.8348 0.076 Uiso 1 1 calc R . . C15 C 0.2564(4) 0.49586(17) 0.59775(19) 0.0511(8) Uani 1 1 d . . . H15A H 0.2475 0.4868 0.5361 0.077 Uiso 1 1 calc R . . H15B H 0.1741 0.4687 0.6190 0.077 Uiso 1 1 calc R . . H15C H 0.3509 0.4735 0.6268 0.077 Uiso 1 1 calc R . . C16 C 0.0606(3) 0.6442(2) 0.57820(19) 0.0497(8) Uani 1 1 d . . . H16A H 0.0500 0.7001 0.5982 0.074 Uiso 1 1 calc R . . H16B H -0.0124 0.6090 0.5990 0.074 Uiso 1 1 calc R . . H16C H 0.0440 0.6434 0.5156 0.074 Uiso 1 1 calc R . . C21 C 0.6750(3) 0.83001(18) 0.85048(16) 0.0454(7) Uani 1 1 d . . . H21A H 0.7097 0.8756 0.8886 0.068 Uiso 1 1 calc R . . H21B H 0.7197 0.7792 0.8750 0.068 Uiso 1 1 calc R . . H21C H 0.5666 0.8261 0.8439 0.068 Uiso 1 1 calc R . . C22 C 0.8855(3) 0.86555(19) 0.7758(2) 0.0484(7) Uani 1 1 d . . . H22A H 0.9167 0.8710 0.7199 0.073 Uiso 1 1 calc R . . H22B H 0.9431 0.8222 0.8084 0.073 Uiso 1 1 calc R . . H22C H 0.9026 0.9172 0.8070 0.073 Uiso 1 1 calc R . . C23 C 0.2749(3) 0.93172(18) 0.67899(19) 0.0485(7) Uani 1 1 d . . . H23A H 0.3537 0.9494 0.7250 0.073 Uiso 1 1 calc R . . H23B H 0.1982 0.9026 0.7035 0.073 Uiso 1 1 calc R . . H23C H 0.2308 0.9795 0.6473 0.073 Uiso 1 1 calc R . . C24 C 0.2209(3) 0.84913(18) 0.54477(18) 0.0457(7) Uani 1 1 d . . . H24A H 0.1840 0.8971 0.5110 0.069 Uiso 1 1 calc R . . H24B H 0.1388 0.8233 0.5675 0.069 Uiso 1 1 calc R . . H24C H 0.2630 0.8102 0.5084 0.069 Uiso 1 1 calc R . . C25 C 0.5918(3) 1.06541(17) 0.6488(2) 0.0502(8) Uani 1 1 d . . . H25A H 0.5203 1.0753 0.6875 0.075 Uiso 1 1 calc R . . H25B H 0.5575 1.0923 0.5940 0.075 Uiso 1 1 calc R . . H25C H 0.6889 1.0874 0.6742 0.075 Uiso 1 1 calc R . . C26 C 0.7511(3) 0.93105(18) 0.56517(18) 0.0462(7) Uani 1 1 d . . . H26A H 0.8441 0.9586 0.5889 0.069 Uiso 1 1 calc R . . H26B H 0.7174 0.9500 0.5066 0.069 Uiso 1 1 calc R . . H26C H 0.7676 0.8720 0.5648 0.069 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 0.0354(4) 0.0376(4) 0.0330(4) -0.0043(3) 0.0110(3) -0.0052(3) O1 0.0453(11) 0.0395(11) 0.0336(10) -0.0010(8) 0.0137(8) -0.0097(8) O2 0.0279(9) 0.0389(10) 0.0297(9) -0.0018(7) 0.0094(7) -0.0014(7) Si2 0.0343(4) 0.0319(4) 0.0337(4) 0.0028(3) 0.0098(3) 0.0008(3) O3 0.0376(10) 0.0384(10) 0.0302(9) 0.0045(8) 0.0092(8) -0.0019(8) O4 0.0332(10) 0.0353(10) 0.0334(10) 0.0009(8) 0.0082(8) 0.0022(8) C1 0.0291(13) 0.0374(15) 0.0298(14) -0.0030(11) 0.0126(11) 0.0019(11) C2 0.0253(13) 0.0324(14) 0.0255(13) 0.0021(10) 0.0105(10) 0.0043(10) C3 0.0242(13) 0.0382(15) 0.0241(13) -0.0036(11) 0.0086(10) 0.0020(11) C4 0.0356(14) 0.0378(15) 0.0266(13) -0.0028(11) 0.0127(11) -0.0076(11) C5 0.0276(13) 0.0384(15) 0.0293(14) 0.0031(11) 0.0029(11) -0.0005(11) C6 0.0284(14) 0.0383(15) 0.0329(14) 0.0071(11) 0.0127(11) 0.0033(11) O6 0.0273(10) 0.0528(13) 0.0702(14) -0.0111(10) 0.0133(9) 0.0083(9) C7 0.0217(12) 0.0318(14) 0.0275(13) -0.0042(11) 0.0083(10) 0.0017(10) C8 0.0288(13) 0.0338(14) 0.0354(14) 0.0012(11) 0.0115(11) 0.0022(11) C11 0.0403(16) 0.0377(16) 0.0481(17) -0.0032(13) 0.0134(13) 0.0058(12) C12 0.0381(15) 0.0510(18) 0.0334(15) -0.0034(12) 0.0177(12) -0.0009(12) C13 0.0613(19) 0.0552(19) 0.0323(15) 0.0070(13) 0.0093(14) -0.0142(15) C14 0.0462(17) 0.061(2) 0.0535(18) -0.0114(15) 0.0322(15) -0.0104(14) C15 0.0606(19) 0.0449(18) 0.0497(18) -0.0092(14) 0.0148(15) -0.0113(15) C16 0.0351(16) 0.065(2) 0.0510(18) -0.0065(15) 0.0133(13) -0.0093(14) C21 0.0501(18) 0.0556(18) 0.0300(15) 0.0014(13) 0.0050(13) -0.0020(14) C22 0.0324(15) 0.0541(19) 0.0569(19) -0.0037(15) 0.0023(14) -0.0030(13) C23 0.0436(17) 0.0452(17) 0.0611(19) -0.0014(15) 0.0217(15) 0.0132(13) C24 0.0378(15) 0.0460(17) 0.0498(17) 0.0107(14) -0.0032(13) 0.0015(13) C25 0.0561(19) 0.0398(17) 0.0540(19) 0.0015(14) 0.0073(15) -0.0007(14) C26 0.0457(17) 0.0522(18) 0.0443(17) 0.0082(14) 0.0183(14) 0.0025(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 O2 1.6408(17) . ? Si1 O1 1.6476(18) . ? Si1 C16 1.848(3) . ? Si1 C15 1.854(3) . ? O1 C4 1.444(3) . ? O2 C1 1.454(3) . ? Si2 O4 1.6369(18) . ? Si2 O3 1.6455(18) . ? Si2 C25 1.846(3) . ? Si2 C26 1.850(3) . ? O3 C8 1.444(3) . ? O4 C5 1.432(3) . ? C1 C12 1.523(3) . ? C1 C11 1.529(4) . ? C1 C2 1.552(3) . ? C2 C6 1.508(3) . ? C2 C3 1.525(3) . ? C2 C7 1.534(3) . ? C3 C7 1.287(3) . ? C3 C4 1.505(3) . ? C4 C13 1.516(4) . ? C4 C14 1.518(4) . ? C5 C21 1.522(3) . ? C5 C22 1.529(3) . ? C5 C6 1.557(4) . ? C6 O6 1.225(3) . ? C7 C8 1.496(3) . ? C8 C24 1.521(4) . ? C8 C23 1.527(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 O2 Si1 O1 111.41(9) . . ? O2 Si1 C16 106.85(12) . . ? O1 Si1 C16 112.58(12) . . ? O2 Si1 C15 112.29(11) . . ? O1 Si1 C15 105.29(12) . . ? C16 Si1 C15 108.48(14) . . ? C4 O1 Si1 129.36(15) . . ? C1 O2 Si1 129.70(15) . . ? O4 Si2 O3 107.42(9) . . ? O4 Si2 C25 106.02(12) . . ? O3 Si2 C25 110.99(12) . . ? O4 Si2 C26 114.65(11) . . ? O3 Si2 C26 105.89(12) . . ? C25 Si2 C26 111.84(14) . . ? C8 O3 Si2 125.60(15) . . ? C5 O4 Si2 134.18(15) . . ? O2 C1 C12 105.70(19) . . ? O2 C1 C11 109.1(2) . . ? C12 C1 C11 110.7(2) . . ? O2 C1 C2 106.84(17) . . ? C12 C1 C2 111.5(2) . . ? C11 C1 C2 112.6(2) . . ? C6 C2 C3 119.55(19) . . ? C6 C2 C7 117.8(2) . . ? C3 C2 C7 49.78(14) . . ? C6 C2 C1 117.05(19) . . ? C3 C2 C1 116.92(19) . . ? C7 C2 C1 118.85(19) . . ? C7 C3 C4 151.4(2) . . ? C7 C3 C2 65.46(16) . . ? C4 C3 C2 138.5(2) . . ? O1 C4 C3 107.07(18) . . ? O1 C4 C13 105.9(2) . . ? C3 C4 C13 112.0(2) . . ? O1 C4 C14 110.2(2) . . ? C3 C4 C14 109.9(2) . . ? C13 C4 C14 111.6(2) . . ? O4 C5 C21 106.5(2) . . ? O4 C5 C22 108.5(2) . . ? C21 C5 C22 109.2(2) . . ? O4 C5 C6 111.48(19) . . ? C21 C5 C6 111.7(2) . . ? C22 C5 C6 109.4(2) . . ? O6 C6 C2 120.4(2) . . ? O6 C6 C5 117.3(2) . . ? C2 C6 C5 122.3(2) . . ? C3 C7 C8 153.7(2) . . ? C3 C7 C2 64.76(17) . . ? C8 C7 C2 141.2(2) . . ? O3 C8 C7 109.22(18) . . ? O3 C8 C24 105.9(2) . . ? C7 C8 C24 110.8(2) . . ? O3 C8 C23 110.6(2) . . ? C7 C8 C23 109.8(2) . . ? C24 C8 C23 110.4(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.41 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.347 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.057 #===END #_eof # End of Crystallographic Information File