# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address H.C.Jahr ; Kekule-Institut fur Organische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; M.Nieger ; Institut fur Anorganische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; K.H.Dotz ; Kekule-Institut fur Organische Chemie Universitat Bonn Gerhard-Domagk-Str. 1 D-53121 Bonn Bundesrepublik Deutschland ; _publ_contact_author_name 'Prof Karl Heinz Dotz' _publ_contact_author_address ; Kekule-Institut fur Organische Chemie und Biochemie Rheinische Friedrich-Wilhelms-Universitat Bonn Gerhard-Domagk-Strasse 1, D-53121 B D-53121 Bonn D - 53121 GERMANY ; _publ_contact_author_email DOETZ@UNI-BONN.DE _publ_requested_journal 'Chemical Communications' _publ_section_title ; Controlled haptotropic rearrangements - Towards a stereospecific molecular switch based on chiral arene chromium complexes ; #============================================================================== data_doe165 _database_code_CSD 205869 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tricarbonyl[eta6-1,2,3,4,4a,8a-1-tert.butyldimethylsilyloxy-2,3-diethyl- 4-methoxynaphthalene]chromium(0) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Cr O5 Si' _chemical_formula_sum 'C24 H32 Cr O5 Si' _chemical_formula_weight 480.59 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.4329(3) _cell_length_b 12.4050(3) _cell_length_c 18.1159(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.186(1) _cell_angle_gamma 90.00 _cell_volume 2467.45(11) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4717 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 0.543 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 40 mm, 60 sec./deg., 1 deg., 2 sets, 254 frames, mos.= 0.583(2) deg. ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 1 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 12750 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4322 _reflns_number_gt 3318 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0452P)^2^+0.3306P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4322 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cr1 Cr 0.65624(3) 0.34819(3) 0.35789(2) 0.01804(13) Uani 1 1 d . . . C1A C 0.6157(2) 0.29284(19) 0.44102(15) 0.0257(6) Uani 1 1 d . . . O1A O 0.58774(18) 0.25620(15) 0.49251(11) 0.0423(5) Uani 1 1 d . . . C1B C 0.8160(2) 0.3219(2) 0.40723(16) 0.0312(7) Uani 1 1 d . . . O1B O 0.91642(17) 0.30177(17) 0.43970(12) 0.0532(6) Uani 1 1 d . . . C1C C 0.6486(2) 0.2105(2) 0.32184(14) 0.0260(6) Uani 1 1 d . . . O1C O 0.64696(18) 0.12163(14) 0.30046(11) 0.0425(5) Uani 1 1 d . . . C1 C 0.6794(2) 0.46430(17) 0.26519(13) 0.0178(5) Uani 1 1 d . . . C2 C 0.57056(19) 0.40598(17) 0.23614(13) 0.0175(5) Uani 1 1 d . . . C3 C 0.4801(2) 0.40485(17) 0.27720(13) 0.0181(5) Uani 1 1 d . . . C4 C 0.5025(2) 0.46151(18) 0.34668(13) 0.0184(5) Uani 1 1 d . . . C4A C 0.6108(2) 0.52381(17) 0.37649(13) 0.0180(5) Uani 1 1 d . . . C5 C 0.6323(2) 0.58355(18) 0.44692(14) 0.0244(6) Uani 1 1 d . . . H5 H 0.5747 0.5808 0.4759 0.029 Uiso 1 1 calc R . . C6 C 0.7342(2) 0.6436(2) 0.47195(15) 0.0307(6) Uani 1 1 d . . . H6 H 0.7470 0.6838 0.5181 0.037 Uiso 1 1 calc R . . C7 C 0.8222(2) 0.6475(2) 0.43047(15) 0.0313(6) Uani 1 1 d . . . H7 H 0.8927 0.6911 0.4488 0.038 Uiso 1 1 calc R . . C8 C 0.8074(2) 0.58943(19) 0.36446(14) 0.0258(6) Uani 1 1 d . . . H8 H 0.8682 0.5915 0.3379 0.031 Uiso 1 1 calc R . . C8A C 0.7001(2) 0.52532(17) 0.33523(13) 0.0182(5) Uani 1 1 d . . . O1 O 0.75998(13) 0.47490(12) 0.22260(9) 0.0212(4) Uani 1 1 d . . . Si1 Si 0.88525(6) 0.41368(5) 0.21355(4) 0.02242(18) Uani 1 1 d . . . C11 C 0.8644(2) 0.2658(2) 0.20449(17) 0.0376(7) Uani 1 1 d . . . H11A H 0.7948 0.2494 0.1603 0.056 Uiso 1 1 calc R . . H11B H 0.8492 0.2371 0.2514 0.056 Uiso 1 1 calc R . . H11C H 0.9381 0.2327 0.1970 0.056 Uiso 1 1 calc R . . C12 C 1.0179(2) 0.4410(2) 0.29784(16) 0.0380(7) Uani 1 1 d . . . H12A H 1.0308 0.5190 0.3037 0.057 Uiso 1 1 calc R . . H12B H 1.0908 0.4069 0.2899 0.057 Uiso 1 1 calc R . . H12C H 1.0020 0.4116 0.3443 0.057 Uiso 1 1 calc R . . C13 C 0.9082(2) 0.4735(2) 0.12354(14) 0.0261(6) Uani 1 1 d . . . C14 C 0.8068(3) 0.4398(3) 0.05373(18) 0.0788(13) Uani 1 1 d . . . H14A H 0.7285 0.4651 0.0593 0.118 Uiso 1 1 calc R . . H14B H 0.8055 0.3610 0.0494 0.118 Uiso 1 1 calc R . . H14C H 0.8210 0.4715 0.0074 0.118 Uiso 1 1 calc R . . C15 C 0.9087(5) 0.5957(3) 0.1261(2) 0.0932(15) Uani 1 1 d . . . H15A H 0.8310 0.6214 0.1324 0.140 Uiso 1 1 calc R . . H15B H 0.9199 0.6241 0.0780 0.140 Uiso 1 1 calc R . . H15C H 0.9755 0.6205 0.1694 0.140 Uiso 1 1 calc R . . C16 C 1.0275(3) 0.4343(4) 0.1126(2) 0.0880(15) Uani 1 1 d . . . H16A H 1.0946 0.4559 0.1569 0.132 Uiso 1 1 calc R . . H16B H 1.0395 0.4661 0.0657 0.132 Uiso 1 1 calc R . . H16C H 1.0258 0.3555 0.1081 0.132 Uiso 1 1 calc R . . C21 C 0.5458(2) 0.35250(18) 0.15832(13) 0.0218(5) Uani 1 1 d . . . H21A H 0.4999 0.2848 0.1583 0.026 Uiso 1 1 calc R . . H21B H 0.6239 0.3341 0.1479 0.026 Uiso 1 1 calc R . . C22 C 0.4721(2) 0.4278(2) 0.09512(14) 0.0341(7) Uani 1 1 d . . . H22A H 0.4565 0.3919 0.0451 0.051 Uiso 1 1 calc R . . H22B H 0.5182 0.4942 0.0946 0.051 Uiso 1 1 calc R . . H22C H 0.3944 0.4453 0.1052 0.051 Uiso 1 1 calc R . . C31 C 0.3583(2) 0.34708(19) 0.24747(14) 0.0256(6) Uani 1 1 d . . . H31A H 0.3507 0.3221 0.1944 0.031 Uiso 1 1 calc R . . H31B H 0.2923 0.3999 0.2448 0.031 Uiso 1 1 calc R . . C32 C 0.3382(2) 0.2507(2) 0.29485(16) 0.0368(7) Uani 1 1 d . . . H32A H 0.2579 0.2193 0.2710 0.055 Uiso 1 1 calc R . . H32B H 0.3425 0.2745 0.3471 0.055 Uiso 1 1 calc R . . H32C H 0.4014 0.1965 0.2968 0.055 Uiso 1 1 calc R . . O4 O 0.41821(13) 0.45926(12) 0.38834(9) 0.0216(4) Uani 1 1 d . . . C41 C 0.3358(2) 0.54986(19) 0.37254(15) 0.0263(6) Uani 1 1 d . . . H41A H 0.2782 0.5439 0.4035 0.039 Uiso 1 1 calc R . . H41B H 0.2910 0.5503 0.3179 0.039 Uiso 1 1 calc R . . H41C H 0.3823 0.6169 0.3855 0.039 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 Cr1 0.0205(2) 0.0161(2) 0.0186(2) 0.00170(16) 0.00715(16) 0.00100(16) C1A 0.0329(14) 0.0188(13) 0.0263(15) 0.0004(12) 0.0099(12) 0.0075(11) O1A 0.0661(14) 0.0369(11) 0.0337(11) 0.0132(9) 0.0302(10) 0.0110(10) C1B 0.0328(15) 0.0260(14) 0.0335(16) 0.0075(12) 0.0071(13) 0.0006(12) O1B 0.0289(11) 0.0617(14) 0.0583(14) 0.0189(11) -0.0052(10) 0.0077(10) C1C 0.0302(14) 0.0278(15) 0.0225(14) 0.0040(12) 0.0117(11) -0.0008(11) O1C 0.0689(14) 0.0220(10) 0.0436(13) -0.0051(9) 0.0269(11) -0.0020(9) C1 0.0197(12) 0.0154(12) 0.0193(13) 0.0039(10) 0.0072(10) 0.0024(10) C2 0.0191(12) 0.0159(12) 0.0179(13) 0.0036(10) 0.0058(10) 0.0035(10) C3 0.0205(12) 0.0164(12) 0.0170(13) 0.0022(10) 0.0046(10) 0.0031(10) C4 0.0194(12) 0.0175(12) 0.0204(13) 0.0055(10) 0.0090(10) 0.0026(10) C4A 0.0219(12) 0.0147(12) 0.0169(13) 0.0031(10) 0.0050(10) 0.0044(10) C5 0.0331(14) 0.0195(13) 0.0214(14) -0.0011(11) 0.0089(11) 0.0006(11) C6 0.0370(15) 0.0319(15) 0.0208(14) -0.0077(12) 0.0041(12) -0.0030(12) C7 0.0296(14) 0.0286(15) 0.0300(15) -0.0031(13) -0.0008(12) -0.0106(12) C8 0.0236(13) 0.0256(14) 0.0272(15) 0.0038(12) 0.0055(11) -0.0038(11) C8A 0.0197(12) 0.0168(13) 0.0174(13) 0.0034(10) 0.0041(10) 0.0017(10) O1 0.0204(8) 0.0230(9) 0.0239(9) 0.0032(7) 0.0121(7) 0.0005(7) Si1 0.0184(3) 0.0240(4) 0.0272(4) 0.0024(3) 0.0101(3) 0.0007(3) C11 0.0312(15) 0.0285(15) 0.059(2) 0.0066(14) 0.0217(14) 0.0085(12) C12 0.0231(14) 0.0555(19) 0.0355(17) 0.0029(14) 0.0082(12) 0.0032(13) C13 0.0214(13) 0.0336(15) 0.0264(14) -0.0003(12) 0.0117(11) -0.0018(11) C14 0.057(2) 0.147(4) 0.0298(19) 0.011(2) 0.0065(16) -0.042(2) C15 0.191(5) 0.040(2) 0.075(3) 0.0052(19) 0.083(3) -0.025(2) C16 0.064(2) 0.145(4) 0.078(3) 0.058(3) 0.056(2) 0.058(2) C21 0.0205(12) 0.0263(14) 0.0202(13) -0.0028(11) 0.0084(10) 0.0011(10) C22 0.0382(15) 0.0457(17) 0.0178(14) -0.0008(12) 0.0071(12) 0.0092(13) C31 0.0210(12) 0.0340(15) 0.0233(14) -0.0038(12) 0.0085(11) -0.0058(11) C32 0.0342(15) 0.0374(16) 0.0397(17) -0.0081(14) 0.0117(13) -0.0166(13) O4 0.0248(9) 0.0208(9) 0.0239(9) 0.0020(7) 0.0144(7) 0.0036(7) C41 0.0251(13) 0.0265(14) 0.0312(15) 0.0020(12) 0.0141(11) 0.0074(11) _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 Cr1 C1C 1.822(3) . ? Cr1 C1B 1.825(3) . ? Cr1 C1A 1.828(3) . ? Cr1 C4 2.216(2) . ? Cr1 C3 2.246(2) . ? Cr1 C2 2.266(2) . ? Cr1 C1 2.283(2) . ? Cr1 C4A 2.286(2) . ? Cr1 C8A 2.316(2) . ? Cr1 Zar 1.768(2) . ? C1A O1A 1.160(3) . ? C1B O1B 1.162(3) . ? C1C O1C 1.167(3) . ? C1 O1 1.363(3) . ? C1 C2 1.408(3) . ? C1 C8A 1.439(3) . ? C2 C3 1.433(3) . ? C2 C21 1.512(3) . ? C3 C4 1.402(3) . ? C3 C31 1.525(3) . ? C4 O4 1.380(3) . ? C4 C4A 1.432(3) . ? C4A C8A 1.423(3) . ? C4A C5 1.436(3) . ? C5 C6 1.351(3) . ? C5 H5 0.9500 . ? C6 C7 1.414(4) . ? C6 H6 0.9500 . ? C7 C8 1.365(3) . ? C7 H7 0.9500 . ? C8 C8A 1.434(3) . ? C8 H8 0.9500 . ? O1 Si1 1.6690(16) . ? Si1 C11 1.851(3) . ? Si1 C12 1.859(3) . ? Si1 C13 1.875(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.513(4) . ? C13 C15 1.516(4) . ? C13 C14 1.517(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 C22 1.534(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 C32 1.526(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O4 C41 1.443(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1C Cr1 C1B 87.11(11) . . ? C1C Cr1 C1A 86.88(11) . . ? C1B Cr1 C1A 88.77(11) . . ? C1C Cr1 C4 127.19(10) . . ? C1B Cr1 C4 144.91(10) . . ? C1A Cr1 C4 86.38(9) . . ? C1C Cr1 C3 96.63(9) . . ? C1B Cr1 C3 165.45(10) . . ? C1A Cr1 C3 105.44(10) . . ? C4 Cr1 C3 36.60(8) . . ? C1C Cr1 C2 89.03(9) . . ? C1B Cr1 C2 129.44(10) . . ? C1A Cr1 C2 141.31(10) . . ? C4 Cr1 C2 66.01(8) . . ? C3 Cr1 C2 37.03(8) . . ? C1C Cr1 C1 109.35(10) . . ? C1B Cr1 C1 99.63(10) . . ? C1A Cr1 C1 161.94(9) . . ? C4 Cr1 C1 77.53(8) . . ? C3 Cr1 C1 65.85(8) . . ? C2 Cr1 C1 36.07(8) . . ? C1C Cr1 C4A 162.94(9) . . ? C1B Cr1 C4A 109.58(10) . . ? C1A Cr1 C4A 96.68(9) . . ? C4 Cr1 C4A 37.06(8) . . ? C3 Cr1 C4A 66.33(8) . . ? C2 Cr1 C4A 77.74(8) . . ? C1 Cr1 C4A 65.48(8) . . ? C1C Cr1 C8A 144.78(10) . . ? C1B Cr1 C8A 91.12(9) . . ? C1A Cr1 C8A 128.28(10) . . ? C4 Cr1 C8A 65.63(8) . . ? C3 Cr1 C8A 77.70(8) . . ? C2 Cr1 C8A 65.38(8) . . ? C1 Cr1 C8A 36.47(8) . . ? C4A Cr1 C8A 36.03(8) . . ? O1A C1A Cr1 178.3(2) . . ? O1B C1B Cr1 177.5(2) . . ? O1C C1C Cr1 177.9(2) . . ? O1 C1 C2 120.3(2) . . ? O1 C1 C8A 118.51(19) . . ? C2 C1 C8A 120.7(2) . . ? O1 C1 Cr1 135.45(15) . . ? C2 C1 Cr1 71.29(13) . . ? C8A C1 Cr1 73.00(13) . . ? C1 C2 C3 120.1(2) . . ? C1 C2 C21 119.4(2) . . ? C3 C2 C21 120.3(2) . . ? C1 C2 Cr1 72.64(13) . . ? C3 C2 Cr1 70.76(13) . . ? C21 C2 Cr1 133.38(15) . . ? C4 C3 C2 118.9(2) . . ? C4 C3 C31 118.2(2) . . ? C2 C3 C31 122.8(2) . . ? C4 C3 Cr1 70.50(12) . . ? C2 C3 Cr1 72.22(12) . . ? C31 C3 Cr1 130.37(16) . . ? O4 C4 C3 120.0(2) . . ? O4 C4 C4A 117.9(2) . . ? C3 C4 C4A 122.1(2) . . ? O4 C4 Cr1 126.45(15) . . ? C3 C4 Cr1 72.89(13) . . ? C4A C4 Cr1 74.15(13) . . ? C8A C4A C4 118.7(2) . . ? C8A C4A C5 119.3(2) . . ? C4 C4A C5 121.9(2) . . ? C8A C4A Cr1 73.12(13) . . ? C4 C4A Cr1 68.79(12) . . ? C5 C4A Cr1 129.28(15) . . ? C6 C5 C4A 120.0(2) . . ? C6 C5 H5 120.0 . . ? C4A C5 H5 120.0 . . ? C5 C6 C7 121.0(2) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C8 C7 C6 120.9(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C8A 120.0(2) . . ? C7 C8 H8 120.0 . . ? C8A C8 H8 120.0 . . ? C4A C8A C8 118.6(2) . . ? C4A C8A C1 119.4(2) . . ? C8 C8A C1 122.1(2) . . ? C4A C8A Cr1 70.86(13) . . ? C8 C8A Cr1 131.77(16) . . ? C1 C8A Cr1 70.54(12) . . ? C1 O1 Si1 138.21(14) . . ? O1 Si1 C11 111.51(10) . . ? O1 Si1 C12 111.24(11) . . ? C11 Si1 C12 108.01(13) . . ? O1 Si1 C13 103.72(10) . . ? C11 Si1 C13 111.14(13) . . ? C12 Si1 C13 111.23(12) . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C15 109.2(3) . . ? C16 C13 C14 108.0(3) . . ? C15 C13 C14 107.2(3) . . ? C16 C13 Si1 109.69(19) . . ? C15 C13 Si1 111.7(2) . . ? C14 C13 Si1 110.88(19) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C21 C22 110.49(19) . . ? C2 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C2 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C31 C32 115.8(2) . . ? C3 C31 H31A 108.3 . . ? C32 C31 H31A 108.3 . . ? C3 C31 H31B 108.3 . . ? C32 C31 H31B 108.3 . . ? H31A C31 H31B 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C4 O4 C41 113.10(17) . . ? O4 C41 H41A 109.5 . . ? O4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1C Cr1 C1A O1A -46(8) . . . . ? C1B Cr1 C1A O1A -133(8) . . . . ? C4 Cr1 C1A O1A 82(8) . . . . ? C3 Cr1 C1A O1A 50(8) . . . . ? C2 Cr1 C1A O1A 39(8) . . . . ? C1 Cr1 C1A O1A 109(8) . . . . ? C4A Cr1 C1A O1A 118(8) . . . . ? C8A Cr1 C1A O1A 137(8) . . . . ? C1C Cr1 C1B O1B -50(6) . . . . ? C1A Cr1 C1B O1B 37(6) . . . . ? C4 Cr1 C1B O1B 119(6) . . . . ? C3 Cr1 C1B O1B -155(6) . . . . ? C2 Cr1 C1B O1B -136(6) . . . . ? C1 Cr1 C1B O1B -159(6) . . . . ? C4A Cr1 C1B O1B 134(6) . . . . ? C8A Cr1 C1B O1B 166(6) . . . . ? C1B Cr1 C1C O1C 18(7) . . . . ? C1A Cr1 C1C O1C -71(7) . . . . ? C4 Cr1 C1C O1C -154(7) . . . . ? C3 Cr1 C1C O1C -176(100) . . . . ? C2 Cr1 C1C O1C 147(7) . . . . ? C1 Cr1 C1C O1C 117(7) . . . . ? C4A Cr1 C1C O1C -174(100) . . . . ? C8A Cr1 C1C O1C 106(7) . . . . ? C1C Cr1 C1 O1 -55.3(2) . . . . ? C1B Cr1 C1 O1 35.0(2) . . . . ? C1A Cr1 C1 O1 151.7(3) . . . . ? C4 Cr1 C1 O1 179.3(2) . . . . ? C3 Cr1 C1 O1 -144.0(2) . . . . ? C2 Cr1 C1 O1 -114.5(3) . . . . ? C4A Cr1 C1 O1 142.2(2) . . . . ? C8A Cr1 C1 O1 113.6(3) . . . . ? C1C Cr1 C1 C2 59.17(15) . . . . ? C1B Cr1 C1 C2 149.48(15) . . . . ? C1A Cr1 C1 C2 -93.8(3) . . . . ? C4 Cr1 C1 C2 -66.18(14) . . . . ? C3 Cr1 C1 C2 -29.49(13) . . . . ? C4A Cr1 C1 C2 -103.29(14) . . . . ? C8A Cr1 C1 C2 -131.85(19) . . . . ? C1C Cr1 C1 C8A -168.98(13) . . . . ? C1B Cr1 C1 C8A -78.67(15) . . . . ? C1A Cr1 C1 C8A 38.1(3) . . . . ? C4 Cr1 C1 C8A 65.67(13) . . . . ? C3 Cr1 C1 C8A 102.36(14) . . . . ? C2 Cr1 C1 C8A 131.85(19) . . . . ? C4A Cr1 C1 C8A 28.56(12) . . . . ? O1 C1 C2 C3 -173.16(19) . . . . ? C8A C1 C2 C3 -1.4(3) . . . . ? Cr1 C1 C2 C3 54.51(19) . . . . ? O1 C1 C2 C21 1.8(3) . . . . ? C8A C1 C2 C21 173.54(19) . . . . ? Cr1 C1 C2 C21 -130.52(19) . . . . ? O1 C1 C2 Cr1 132.33(19) . . . . ? C8A C1 C2 Cr1 -55.93(18) . . . . ? C1C Cr1 C2 C1 -125.88(15) . . . . ? C1B Cr1 C2 C1 -40.42(18) . . . . ? C1A Cr1 C2 C1 150.34(16) . . . . ? C4 Cr1 C2 C1 102.11(15) . . . . ? C3 Cr1 C2 C1 131.8(2) . . . . ? C4A Cr1 C2 C1 64.97(13) . . . . ? C8A Cr1 C2 C1 29.14(13) . . . . ? C1C Cr1 C2 C3 102.37(15) . . . . ? C1B Cr1 C2 C3 -172.18(14) . . . . ? C1A Cr1 C2 C3 18.6(2) . . . . ? C4 Cr1 C2 C3 -29.65(13) . . . . ? C1 Cr1 C2 C3 -131.8(2) . . . . ? C4A Cr1 C2 C3 -66.79(13) . . . . ? C8A Cr1 C2 C3 -102.61(14) . . . . ? C1C Cr1 C2 C21 -11.6(2) . . . . ? C1B Cr1 C2 C21 73.9(2) . . . . ? C1A Cr1 C2 C21 -95.4(3) . . . . ? C4 Cr1 C2 C21 -143.6(2) . . . . ? C3 Cr1 C2 C21 -114.0(3) . . . . ? C1 Cr1 C2 C21 114.3(3) . . . . ? C4A Cr1 C2 C21 179.3(2) . . . . ? C8A Cr1 C2 C21 143.4(2) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? C21 C2 C3 C4 -175.61(19) . . . . ? Cr1 C2 C3 C4 54.71(18) . . . . ? C1 C2 C3 C31 177.5(2) . . . . ? C21 C2 C3 C31 2.6(3) . . . . ? Cr1 C2 C3 C31 -127.1(2) . . . . ? C1 C2 C3 Cr1 -55.40(19) . . . . ? C21 C2 C3 Cr1 129.68(19) . . . . ? C1C Cr1 C3 C4 149.78(15) . . . . ? C1B Cr1 C3 C4 -106.0(4) . . . . ? C1A Cr1 C3 C4 61.20(15) . . . . ? C2 Cr1 C3 C4 -130.7(2) . . . . ? C1 Cr1 C3 C4 -101.95(15) . . . . ? C4A Cr1 C3 C4 -29.41(13) . . . . ? C8A Cr1 C3 C4 -65.49(14) . . . . ? C1C Cr1 C3 C2 -79.49(15) . . . . ? C1B Cr1 C3 C2 24.7(5) . . . . ? C1A Cr1 C3 C2 -168.08(14) . . . . ? C4 Cr1 C3 C2 130.7(2) . . . . ? C1 Cr1 C3 C2 28.77(13) . . . . ? C4A Cr1 C3 C2 101.31(14) . . . . ? C8A Cr1 C3 C2 65.23(13) . . . . ? C1C Cr1 C3 C31 38.8(2) . . . . ? C1B Cr1 C3 C31 143.0(4) . . . . ? C1A Cr1 C3 C31 -49.8(2) . . . . ? C4 Cr1 C3 C31 -111.0(3) . . . . ? C2 Cr1 C3 C31 118.3(3) . . . . ? C1 Cr1 C3 C31 147.1(2) . . . . ? C4A Cr1 C3 C31 -140.4(2) . . . . ? C8A Cr1 C3 C31 -176.5(2) . . . . ? C2 C3 C4 O4 -178.24(19) . . . . ? C31 C3 C4 O4 3.4(3) . . . . ? Cr1 C3 C4 O4 -122.69(19) . . . . ? C2 C3 C4 C4A 2.4(3) . . . . ? C31 C3 C4 C4A -175.9(2) . . . . ? Cr1 C3 C4 C4A 57.95(19) . . . . ? C2 C3 C4 Cr1 -55.54(18) . . . . ? C31 C3 C4 Cr1 126.14(19) . . . . ? C1C Cr1 C4 O4 76.2(2) . . . . ? C1B Cr1 C4 O4 -89.8(2) . . . . ? C1A Cr1 C4 O4 -7.12(19) . . . . ? C3 Cr1 C4 O4 115.1(2) . . . . ? C2 Cr1 C4 O4 145.0(2) . . . . ? C1 Cr1 C4 O4 -178.8(2) . . . . ? C4A Cr1 C4 O4 -113.2(2) . . . . ? C8A Cr1 C4 O4 -142.4(2) . . . . ? C1C Cr1 C4 C3 -38.87(19) . . . . ? C1B Cr1 C4 C3 155.15(18) . . . . ? C1A Cr1 C4 C3 -122.18(15) . . . . ? C2 Cr1 C4 C3 29.97(13) . . . . ? C1 Cr1 C4 C3 66.10(14) . . . . ? C4A Cr1 C4 C3 131.7(2) . . . . ? C8A Cr1 C4 C3 102.58(15) . . . . ? C1C Cr1 C4 C4A -170.59(14) . . . . ? C1B Cr1 C4 C4A 23.4(2) . . . . ? C1A Cr1 C4 C4A 106.10(15) . . . . ? C3 Cr1 C4 C4A -131.7(2) . . . . ? C2 Cr1 C4 C4A -101.75(14) . . . . ? C1 Cr1 C4 C4A -65.63(13) . . . . ? C8A Cr1 C4 C4A -29.15(13) . . . . ? O4 C4 C4A C8A 178.66(18) . . . . ? C3 C4 C4A C8A -2.0(3) . . . . ? Cr1 C4 C4A C8A 55.40(18) . . . . ? O4 C4 C4A C5 -0.7(3) . . . . ? C3 C4 C4A C5 178.7(2) . . . . ? Cr1 C4 C4A C5 -123.9(2) . . . . ? O4 C4 C4A Cr1 123.27(19) . . . . ? C3 C4 C4A Cr1 -57.37(19) . . . . ? C1C Cr1 C4A C8A -104.7(3) . . . . ? C1B Cr1 C4A C8A 63.00(15) . . . . ? C1A Cr1 C4A C8A 154.07(14) . . . . ? C4 Cr1 C4A C8A -131.04(19) . . . . ? C3 Cr1 C4A C8A -101.96(14) . . . . ? C2 Cr1 C4A C8A -64.79(13) . . . . ? C1 Cr1 C4A C8A -28.89(12) . . . . ? C1C Cr1 C4A C4 26.3(4) . . . . ? C1B Cr1 C4A C4 -165.97(15) . . . . ? C1A Cr1 C4A C4 -74.90(15) . . . . ? C3 Cr1 C4A C4 29.07(13) . . . . ? C2 Cr1 C4A C4 66.25(13) . . . . ? C1 Cr1 C4A C4 102.15(14) . . . . ? C8A Cr1 C4A C4 131.04(19) . . . . ? C1C Cr1 C4A C5 140.9(3) . . . . ? C1B Cr1 C4A C5 -51.4(2) . . . . ? C1A Cr1 C4A C5 39.6(2) . . . . ? C4 Cr1 C4A C5 114.5(3) . . . . ? C3 Cr1 C4A C5 143.6(2) . . . . ? C2 Cr1 C4A C5 -179.2(2) . . . . ? C1 Cr1 C4A C5 -143.3(2) . . . . ? C8A Cr1 C4A C5 -114.4(3) . . . . ? C8A C4A C5 C6 2.4(3) . . . . ? C4 C4A C5 C6 -178.2(2) . . . . ? Cr1 C4A C5 C6 94.1(3) . . . . ? C4A C5 C6 C7 -1.1(4) . . . . ? C5 C6 C7 C8 -0.9(4) . . . . ? C6 C7 C8 C8A 1.5(4) . . . . ? C4 C4A C8A C8 178.8(2) . . . . ? C5 C4A C8A C8 -1.8(3) . . . . ? Cr1 C4A C8A C8 -127.9(2) . . . . ? C4 C4A C8A C1 -0.2(3) . . . . ? C5 C4A C8A C1 179.17(19) . . . . ? Cr1 C4A C8A C1 53.13(18) . . . . ? C4 C4A C8A Cr1 -53.32(18) . . . . ? C5 C4A C8A Cr1 126.04(19) . . . . ? C7 C8 C8A C4A -0.1(3) . . . . ? C7 C8 C8A C1 178.9(2) . . . . ? C7 C8 C8A Cr1 -89.3(3) . . . . ? O1 C1 C8A C4A 173.73(18) . . . . ? C2 C1 C8A C4A 1.9(3) . . . . ? Cr1 C1 C8A C4A -53.28(18) . . . . ? O1 C1 C8A C8 -5.2(3) . . . . ? C2 C1 C8A C8 -177.1(2) . . . . ? Cr1 C1 C8A C8 127.8(2) . . . . ? O1 C1 C8A Cr1 -132.99(18) . . . . ? C2 C1 C8A Cr1 55.13(18) . . . . ? C1C Cr1 C8A C4A 150.53(17) . . . . ? C1B Cr1 C8A C4A -122.90(15) . . . . ? C1A Cr1 C8A C4A -33.59(17) . . . . ? C4 Cr1 C8A C4A 29.94(12) . . . . ? C3 Cr1 C8A C4A 66.50(13) . . . . ? C2 Cr1 C8A C4A 103.47(14) . . . . ? C1 Cr1 C8A C4A 132.31(18) . . . . ? C1C Cr1 C8A C8 -97.8(3) . . . . ? C1B Cr1 C8A C8 -11.3(3) . . . . ? C1A Cr1 C8A C8 78.0(3) . . . . ? C4 Cr1 C8A C8 141.6(3) . . . . ? C3 Cr1 C8A C8 178.1(3) . . . . ? C2 Cr1 C8A C8 -144.9(3) . . . . ? C1 Cr1 C8A C8 -116.1(3) . . . . ? C4A Cr1 C8A C8 111.6(3) . . . . ? C1C Cr1 C8A C1 18.2(2) . . . . ? C1B Cr1 C8A C1 104.79(15) . . . . ? C1A Cr1 C8A C1 -165.90(13) . . . . ? C4 Cr1 C8A C1 -102.38(14) . . . . ? C3 Cr1 C8A C1 -65.82(13) . . . . ? C2 Cr1 C8A C1 -28.84(12) . . . . ? C4A Cr1 C8A C1 -132.31(18) . . . . ? C2 C1 O1 Si1 -94.6(3) . . . . ? C8A C1 O1 Si1 93.4(3) . . . . ? Cr1 C1 O1 Si1 -1.0(4) . . . . ? C1 O1 Si1 C11 48.7(2) . . . . ? C1 O1 Si1 C12 -72.0(2) . . . . ? C1 O1 Si1 C13 168.3(2) . . . . ? O1 Si1 C13 C16 173.8(2) . . . . ? C11 Si1 C13 C16 -66.3(3) . . . . ? C12 Si1 C13 C16 54.1(3) . . . . ? O1 Si1 C13 C15 52.5(3) . . . . ? C11 Si1 C13 C15 172.5(2) . . . . ? C12 Si1 C13 C15 -67.1(3) . . . . ? O1 Si1 C13 C14 -67.0(2) . . . . ? C11 Si1 C13 C14 52.9(3) . . . . ? C12 Si1 C13 C14 173.3(2) . . . . ? C1 C2 C21 C22 -92.7(2) . . . . ? C3 C2 C21 C22 82.2(3) . . . . ? Cr1 C2 C21 C22 173.81(18) . . . . ? C4 C3 C31 C32 -67.8(3) . . . . ? C2 C3 C31 C32 114.0(3) . . . . ? Cr1 C3 C31 C32 19.9(3) . . . . ? C3 C4 O4 C41 -95.1(2) . . . . ? C4A C4 O4 C41 84.3(2) . . . . ? Cr1 C4 O4 C41 174.67(15) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C41 H41C O1A 0.98 2.66 3.367(3) 129.6 3_666 C7 H7 O1B 0.95 2.53 3.307(3) 139.3 3_766 C41 H41B O1C 0.98 2.59 3.316(3) 130.6 2_655 C5 H5 O4 0.95 2.49 3.238(3) 135.8 3_666 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.427 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.063 #============================================================================== data_doe167 _database_code_CSD 205870 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (S)-Tricarbonyl[eta6-4a,5,6,7,8,8a-1-tert.butyldimethylsilyloxy-2,3-diethyl- 4-methoxynaphthalene]chromium(0) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Cr O5 Si' _chemical_formula_sum 'C24 H32 Cr O5 Si' _chemical_formula_weight 480.59 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(1) _symmetry_Int_Tables_number 169 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z+1/2' 'y, -x+y, z+5/6' 'x-y, x, z+1/6' _cell_length_a 10.4461(1) _cell_length_b 10.4461(1) _cell_length_c 39.4227(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3725.50(6) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 11669 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description plates _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.285 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 50 mm, 180 sec./deg., 0.5 deg., 4 sets, 855 frames, mos.= 0.379(1) deg. ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 0.5 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 23954 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0416 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 24.99 _reflns_number_total 4366 _reflns_number_gt 3954 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics XP _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0259P)^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 riding _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 -0.005(12) _refine_ls_number_reflns 4366 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0302 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0526 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 Cr1 Cr 0.31279(4) 0.17953(4) 0.083041(8) 0.01787(9) Uani 1 1 d . . . C1A C 0.2703(2) 0.1150(3) 0.12734(6) 0.0258(5) Uani 1 1 d . . . O1A O 0.2419(2) 0.0744(2) 0.15517(4) 0.0431(5) Uani 1 1 d . . . C1B C 0.2884(3) 0.3384(3) 0.09446(6) 0.0306(6) Uani 1 1 d . . . O1B O 0.2682(2) 0.43350(19) 0.10188(5) 0.0506(5) Uani 1 1 d . . . C1C C 0.1163(3) 0.0745(3) 0.07251(6) 0.0268(5) Uani 1 1 d . . . O1C O -0.00732(18) 0.0066(2) 0.06527(5) 0.0441(5) Uani 1 1 d . . . C1 C 0.6390(2) 0.2325(2) 0.11608(5) 0.0161(4) Uani 1 1 d . . . C2 C 0.7389(2) 0.3721(2) 0.12635(5) 0.0186(4) Uani 1 1 d . . . C3 C 0.7566(2) 0.4977(2) 0.10740(5) 0.0193(5) Uani 1 1 d . . . C4 C 0.6643(2) 0.4755(2) 0.08037(5) 0.0182(5) Uani 1 1 d . . . C4A C 0.5588(2) 0.3311(2) 0.06934(5) 0.0164(4) Uani 1 1 d . . . C5 C 0.4619(2) 0.3046(2) 0.04102(5) 0.0200(5) Uani 1 1 d . . . H5 H 0.4633 0.3861 0.0299 0.024 Uiso 1 1 calc R . . C6 C 0.3663(2) 0.1623(2) 0.02955(5) 0.0208(5) Uani 1 1 d . . . H6 H 0.3107 0.1479 0.0094 0.025 Uiso 1 1 calc R . . C7 C 0.3514(2) 0.0393(2) 0.04759(5) 0.0208(5) Uani 1 1 d . . . H7 H 0.2847 -0.0580 0.0399 0.025 Uiso 1 1 calc R . . C8 C 0.4353(2) 0.0609(2) 0.07696(5) 0.0193(5) Uani 1 1 d . . . H8 H 0.4188 -0.0220 0.0902 0.023 Uiso 1 1 calc R . . C8A C 0.5451(2) 0.2056(2) 0.08731(5) 0.0161(4) Uani 1 1 d . . . O1 O 0.61530(14) 0.11116(15) 0.13488(3) 0.0177(3) Uani 1 1 d . . . Si1 Si 0.68436(6) -0.00248(6) 0.131136(14) 0.01709(13) Uani 1 1 d . . . C11 C 0.8820(2) 0.0918(2) 0.14398(6) 0.0264(5) Uani 1 1 d . . . H11A H 0.8916 0.1276 0.1673 0.040 Uiso 1 1 calc R . . H11B H 0.9399 0.1756 0.1288 0.040 Uiso 1 1 calc R . . H11C H 0.9186 0.0220 0.1426 0.040 Uiso 1 1 calc R . . C12 C 0.6681(2) -0.0689(2) 0.08698(5) 0.0243(5) Uani 1 1 d . . . H12A H 0.5642 -0.1183 0.0800 0.036 Uiso 1 1 calc R . . H12B H 0.7047 -0.1387 0.0856 0.036 Uiso 1 1 calc R . . H12C H 0.7268 0.0153 0.0720 0.036 Uiso 1 1 calc R . . C13 C 0.5635(2) -0.1558(2) 0.16108(5) 0.0241(5) Uani 1 1 d . . . C14 C 0.5744(3) -0.0943(3) 0.19701(6) 0.0364(6) Uani 1 1 d . . . H14A H 0.6770 -0.0477 0.2049 0.055 Uiso 1 1 calc R . . H14B H 0.5110 -0.1752 0.2124 0.055 Uiso 1 1 calc R . . H14C H 0.5422 -0.0209 0.1967 0.055 Uiso 1 1 calc R . . C15 C 0.6127(3) -0.2725(3) 0.16191(6) 0.0362(6) Uani 1 1 d . . . H15A H 0.7148 -0.2267 0.1701 0.054 Uiso 1 1 calc R . . H15B H 0.6065 -0.3118 0.1390 0.054 Uiso 1 1 calc R . . H15C H 0.5479 -0.3531 0.1772 0.054 Uiso 1 1 calc R . . C16 C 0.4032(2) -0.2295(3) 0.14845(7) 0.0359(6) Uani 1 1 d . . . H16A H 0.3975 -0.2679 0.1255 0.054 Uiso 1 1 calc R . . H16B H 0.3703 -0.1566 0.1482 0.054 Uiso 1 1 calc R . . H16C H 0.3396 -0.3111 0.1636 0.054 Uiso 1 1 calc R . . C21 C 0.8181(3) 0.3939(2) 0.16006(5) 0.0271(5) Uani 1 1 d . . . H21A H 0.9124 0.4892 0.1598 0.032 Uiso 1 1 calc R . . H21B H 0.8411 0.3137 0.1635 0.032 Uiso 1 1 calc R . . C22 C 0.7204(3) 0.3931(3) 0.18921(6) 0.0474(7) Uani 1 1 d . . . H22A H 0.7724 0.4074 0.2108 0.071 Uiso 1 1 calc R . . H22B H 0.6278 0.2982 0.1896 0.071 Uiso 1 1 calc R . . H22C H 0.6987 0.4733 0.1859 0.071 Uiso 1 1 calc R . . C31 C 0.8761(2) 0.6518(2) 0.11674(6) 0.0262(5) Uani 1 1 d . . . H31A H 0.8771 0.6639 0.1417 0.031 Uiso 1 1 calc R . . H31B H 0.8535 0.7244 0.1063 0.031 Uiso 1 1 calc R . . C32 C 1.0303(2) 0.6842(3) 0.10490(7) 0.0343(6) Uani 1 1 d . . . H32A H 1.1046 0.7846 0.1117 0.051 Uiso 1 1 calc R . . H32B H 1.0307 0.6754 0.0802 0.051 Uiso 1 1 calc R . . H32C H 1.0535 0.6131 0.1154 0.051 Uiso 1 1 calc R . . O4 O 0.66463(16) 0.59293(16) 0.06411(3) 0.0233(3) Uani 1 1 d . . . C41 C 0.7691(2) 0.6587(2) 0.03669(6) 0.0280(5) Uani 1 1 d . . . H41A H 0.7599 0.7397 0.0268 0.042 Uiso 1 1 calc R . . H41B H 0.7487 0.5838 0.0193 0.042 Uiso 1 1 calc R . . H41C H 0.8697 0.6972 0.0454 0.042 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 Cr1 0.01528(18) 0.01833(18) 0.01953(17) 0.00007(15) 0.00030(15) 0.00805(15) C1A 0.0262(13) 0.0245(12) 0.0285(14) -0.0018(11) 0.0022(11) 0.0139(11) O1A 0.0586(13) 0.0511(12) 0.0250(10) 0.0099(9) 0.0126(9) 0.0314(10) C1B 0.0273(13) 0.0307(14) 0.0327(14) 0.0049(11) 0.0048(11) 0.0137(12) O1B 0.0682(14) 0.0362(11) 0.0616(12) -0.0011(10) 0.0140(10) 0.0368(11) C1C 0.0230(14) 0.0286(13) 0.0276(13) -0.0020(10) 0.0047(10) 0.0118(11) O1C 0.0173(9) 0.0519(12) 0.0528(12) -0.0101(9) -0.0025(8) 0.0095(9) C1 0.0179(11) 0.0184(11) 0.0148(11) 0.0026(9) 0.0020(9) 0.0113(9) C2 0.0165(10) 0.0204(11) 0.0204(12) -0.0015(9) -0.0032(9) 0.0103(10) C3 0.0160(11) 0.0179(11) 0.0251(12) -0.0005(9) 0.0002(10) 0.0091(9) C4 0.0163(11) 0.0195(11) 0.0210(11) 0.0041(10) 0.0047(9) 0.0105(9) C4A 0.0143(11) 0.0204(11) 0.0169(11) 0.0020(9) 0.0026(9) 0.0104(9) C5 0.0193(11) 0.0234(12) 0.0200(11) 0.0055(9) 0.0020(9) 0.0127(10) C6 0.0177(11) 0.0291(13) 0.0174(11) -0.0027(10) -0.0023(9) 0.0131(10) C7 0.0179(11) 0.0228(12) 0.0221(11) -0.0050(10) -0.0022(9) 0.0105(10) C8 0.0171(11) 0.0199(11) 0.0213(11) 0.0006(9) 0.0012(9) 0.0095(9) C8A 0.0165(10) 0.0181(11) 0.0154(11) 0.0014(9) 0.0023(9) 0.0099(9) O1 0.0207(8) 0.0156(7) 0.0167(7) 0.0024(6) -0.0017(6) 0.0090(6) Si1 0.0163(3) 0.0180(3) 0.0172(3) 0.0014(2) 0.0001(2) 0.0088(2) C11 0.0225(12) 0.0286(13) 0.0291(13) -0.0036(10) -0.0037(10) 0.0136(10) C12 0.0253(12) 0.0293(13) 0.0223(12) -0.0039(10) -0.0030(10) 0.0165(10) C13 0.0267(13) 0.0248(12) 0.0245(12) 0.0061(10) 0.0045(10) 0.0157(11) C14 0.0495(16) 0.0364(14) 0.0271(13) 0.0113(12) 0.0136(12) 0.0244(13) C15 0.0438(16) 0.0307(14) 0.0384(15) 0.0136(12) 0.0100(12) 0.0219(13) C16 0.0253(13) 0.0239(13) 0.0514(16) 0.0159(12) 0.0106(12) 0.0071(11) C21 0.0337(14) 0.0204(12) 0.0284(12) -0.0056(10) -0.0139(11) 0.0144(11) C22 0.075(2) 0.0624(19) 0.0234(14) -0.0100(13) -0.0125(14) 0.0485(18) C31 0.0263(13) 0.0169(11) 0.0341(14) -0.0053(10) -0.0065(11) 0.0099(10) C32 0.0211(13) 0.0246(13) 0.0464(16) -0.0019(12) -0.0059(12) 0.0035(11) O4 0.0244(8) 0.0208(8) 0.0267(8) 0.0081(7) 0.0032(7) 0.0128(7) C41 0.0299(13) 0.0225(12) 0.0250(12) 0.0061(10) 0.0033(11) 0.0081(11) _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 Cr1 C1C 1.826(2) . ? Cr1 C1A 1.844(2) . ? Cr1 C1B 1.856(3) . ? Cr1 C8 2.195(2) . ? Cr1 C5 2.201(2) . ? Cr1 C7 2.203(2) . ? Cr1 C6 2.212(2) . ? Cr1 C8A 2.3092(19) . ? Cr1 C4A 2.310(2) . ? Cr1 Zar 1.767(2) . ? C1A O1A 1.160(3) . ? C1B O1B 1.152(3) . ? C1C O1C 1.156(3) . ? C1 C2 1.363(3) . ? C1 O1 1.380(2) . ? C1 C8A 1.432(3) . ? C2 C3 1.439(3) . ? C2 C21 1.521(3) . ? C3 C4 1.376(3) . ? C3 C31 1.508(3) . ? C4 O4 1.383(2) . ? C4 C4A 1.420(3) . ? C4A C8A 1.433(3) . ? C4A C5 1.438(3) . ? C5 C6 1.388(3) . ? C5 H5 0.9500 . ? C6 C7 1.408(3) . ? C6 H6 0.9500 . ? C7 C8 1.401(3) . ? C7 H7 0.9500 . ? C8 C8A 1.425(3) . ? C8 H8 0.9500 . ? O1 Si1 1.6756(14) . ? Si1 C12 1.850(2) . ? Si1 C11 1.859(2) . ? Si1 C13 1.879(2) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.534(3) . ? C13 C14 1.536(3) . ? C13 C15 1.541(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 C22 1.534(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 C32 1.543(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O4 C41 1.443(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1C Cr1 C1A 90.16(10) . . ? C1C Cr1 C1B 88.69(10) . . ? C1A Cr1 C1B 88.95(10) . . ? C1C Cr1 C8 115.68(9) . . ? C1A Cr1 C8 89.94(9) . . ? C1B Cr1 C8 155.61(9) . . ? C1C Cr1 C5 115.76(9) . . ? C1A Cr1 C5 154.07(9) . . ? C1B Cr1 C5 91.39(9) . . ? C8 Cr1 C5 79.25(8) . . ? C1C Cr1 C7 88.90(9) . . ? C1A Cr1 C7 116.64(9) . . ? C1B Cr1 C7 154.30(9) . . ? C8 Cr1 C7 37.15(7) . . ? C5 Cr1 C7 66.83(8) . . ? C1C Cr1 C6 89.33(9) . . ? C1A Cr1 C6 153.83(9) . . ? C1B Cr1 C6 117.20(9) . . ? C8 Cr1 C6 66.89(8) . . ? C5 Cr1 C6 36.66(7) . . ? C7 Cr1 C6 37.18(7) . . ? C1C Cr1 C8A 152.42(9) . . ? C1A Cr1 C8A 91.19(8) . . ? C1B Cr1 C8A 118.88(9) . . ? C8 Cr1 C8A 36.79(7) . . ? C5 Cr1 C8A 66.10(7) . . ? C7 Cr1 C8A 66.01(7) . . ? C6 Cr1 C8A 77.62(7) . . ? C1C Cr1 C4A 152.82(9) . . ? C1A Cr1 C4A 116.99(9) . . ? C1B Cr1 C4A 92.68(9) . . ? C8 Cr1 C4A 66.31(7) . . ? C5 Cr1 C4A 37.09(7) . . ? C7 Cr1 C4A 78.25(8) . . ? C6 Cr1 C4A 65.98(7) . . ? C8A Cr1 C4A 36.15(7) . . ? O1A C1A Cr1 179.1(2) . . ? O1B C1B Cr1 177.6(2) . . ? O1C C1C Cr1 178.5(2) . . ? C2 C1 O1 120.87(17) . . ? C2 C1 C8A 121.87(18) . . ? O1 C1 C8A 117.03(17) . . ? C1 C2 C3 120.13(18) . . ? C1 C2 C21 119.18(18) . . ? C3 C2 C21 120.32(18) . . ? C4 C3 C2 119.22(18) . . ? C4 C3 C31 120.34(18) . . ? C2 C3 C31 120.44(18) . . ? C3 C4 O4 121.23(18) . . ? C3 C4 C4A 121.49(18) . . ? O4 C4 C4A 117.17(18) . . ? C4 C4A C8A 119.33(18) . . ? C4 C4A C5 122.69(19) . . ? C8A C4A C5 117.97(18) . . ? C4 C4A Cr1 131.53(15) . . ? C8A C4A Cr1 71.90(11) . . ? C5 C4A Cr1 67.32(11) . . ? C6 C5 C4A 121.28(19) . . ? C6 C5 Cr1 72.11(12) . . ? C4A C5 Cr1 75.59(12) . . ? C6 C5 H5 119.4 . . ? C4A C5 H5 119.4 . . ? Cr1 C5 H5 124.5 . . ? C5 C6 C7 120.34(19) . . ? C5 C6 Cr1 71.23(12) . . ? C7 C6 Cr1 71.06(12) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? Cr1 C6 H6 130.5 . . ? C8 C7 C6 119.72(19) . . ? C8 C7 Cr1 71.11(12) . . ? C6 C7 Cr1 71.75(12) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? Cr1 C7 H7 129.4 . . ? C7 C8 C8A 120.97(19) . . ? C7 C8 Cr1 71.74(12) . . ? C8A C8 Cr1 75.98(11) . . ? C7 C8 H8 119.5 . . ? C8A C8 H8 119.5 . . ? Cr1 C8 H8 124.3 . . ? C8 C8A C1 122.95(18) . . ? C8 C8A C4A 119.19(18) . . ? C1 C8A C4A 117.80(18) . . ? C8 C8A Cr1 67.23(11) . . ? C1 C8A Cr1 131.06(14) . . ? C4A C8A Cr1 71.95(11) . . ? C1 O1 Si1 131.34(13) . . ? O1 Si1 C12 110.92(9) . . ? O1 Si1 C11 110.97(9) . . ? C12 Si1 C11 108.94(10) . . ? O1 Si1 C13 101.83(8) . . ? C12 Si1 C13 112.02(10) . . ? C11 Si1 C13 112.05(10) . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C14 110.06(19) . . ? C16 C13 C15 108.76(19) . . ? C14 C13 C15 109.07(18) . . ? C16 C13 Si1 108.86(15) . . ? C14 C13 Si1 110.18(15) . . ? C15 C13 Si1 109.88(15) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C21 C22 110.06(19) . . ? C2 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C2 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C31 C32 112.09(18) . . ? C3 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C3 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C4 O4 C41 115.81(16) . . ? O4 C41 H41A 109.5 . . ? O4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1C Cr1 C1A O1A -32(15) . . . . ? C1B Cr1 C1A O1A 57(15) . . . . ? C8 Cr1 C1A O1A -147(15) . . . . ? C5 Cr1 C1A O1A 148(15) . . . . ? C7 Cr1 C1A O1A -120(15) . . . . ? C6 Cr1 C1A O1A -120(15) . . . . ? C8A Cr1 C1A O1A 176(100) . . . . ? C4A Cr1 C1A O1A 150(15) . . . . ? C1C Cr1 C1B O1B 31(5) . . . . ? C1A Cr1 C1B O1B -59(5) . . . . ? C8 Cr1 C1B O1B -147(5) . . . . ? C5 Cr1 C1B O1B 147(5) . . . . ? C7 Cr1 C1B O1B 115(5) . . . . ? C6 Cr1 C1B O1B 119(5) . . . . ? C8A Cr1 C1B O1B -150(5) . . . . ? C4A Cr1 C1B O1B -176(100) . . . . ? C1A Cr1 C1C O1C -129(10) . . . . ? C1B Cr1 C1C O1C 142(10) . . . . ? C8 Cr1 C1C O1C -39(10) . . . . ? C5 Cr1 C1C O1C 52(10) . . . . ? C7 Cr1 C1C O1C -12(10) . . . . ? C6 Cr1 C1C O1C 25(10) . . . . ? C8A Cr1 C1C O1C -36(10) . . . . ? C4A Cr1 C1C O1C 49(10) . . . . ? O1 C1 C2 C3 -176.72(18) . . . . ? C8A C1 C2 C3 -2.4(3) . . . . ? O1 C1 C2 C21 -3.7(3) . . . . ? C8A C1 C2 C21 170.62(19) . . . . ? C1 C2 C3 C4 4.7(3) . . . . ? C21 C2 C3 C4 -168.29(19) . . . . ? C1 C2 C3 C31 -174.54(19) . . . . ? C21 C2 C3 C31 12.5(3) . . . . ? C2 C3 C4 O4 171.79(18) . . . . ? C31 C3 C4 O4 -9.0(3) . . . . ? C2 C3 C4 C4A -4.4(3) . . . . ? C31 C3 C4 C4A 174.88(19) . . . . ? C3 C4 C4A C8A 1.8(3) . . . . ? O4 C4 C4A C8A -174.51(17) . . . . ? C3 C4 C4A C5 -179.48(19) . . . . ? O4 C4 C4A C5 4.2(3) . . . . ? C3 C4 C4A Cr1 93.0(2) . . . . ? O4 C4 C4A Cr1 -83.3(2) . . . . ? C1C Cr1 C4A C4 117.9(2) . . . . ? C1A Cr1 C4A C4 -64.6(2) . . . . ? C1B Cr1 C4A C4 25.5(2) . . . . ? C8 Cr1 C4A C4 -141.6(2) . . . . ? C5 Cr1 C4A C4 114.3(2) . . . . ? C7 Cr1 C4A C4 -178.7(2) . . . . ? C6 Cr1 C4A C4 144.2(2) . . . . ? C8A Cr1 C4A C4 -113.5(2) . . . . ? C1C Cr1 C4A C8A -128.6(2) . . . . ? C1A Cr1 C4A C8A 48.88(14) . . . . ? C1B Cr1 C4A C8A 139.06(13) . . . . ? C8 Cr1 C4A C8A -28.13(11) . . . . ? C5 Cr1 C4A C8A -132.17(17) . . . . ? C7 Cr1 C4A C8A -65.21(12) . . . . ? C6 Cr1 C4A C8A -102.25(13) . . . . ? C1C Cr1 C4A C5 3.6(3) . . . . ? C1A Cr1 C4A C5 -178.95(13) . . . . ? C1B Cr1 C4A C5 -88.77(13) . . . . ? C8 Cr1 C4A C5 104.04(13) . . . . ? C7 Cr1 C4A C5 66.96(12) . . . . ? C6 Cr1 C4A C5 29.93(12) . . . . ? C8A Cr1 C4A C5 132.17(17) . . . . ? C4 C4A C5 C6 176.0(2) . . . . ? C8A C4A C5 C6 -5.3(3) . . . . ? Cr1 C4A C5 C6 -58.18(18) . . . . ? C4 C4A C5 Cr1 -125.85(19) . . . . ? C8A C4A C5 Cr1 52.90(16) . . . . ? C1C Cr1 C5 C6 -47.92(15) . . . . ? C1A Cr1 C5 C6 132.4(2) . . . . ? C1B Cr1 C5 C6 -137.14(13) . . . . ? C8 Cr1 C5 C6 65.54(12) . . . . ? C7 Cr1 C5 C6 28.79(12) . . . . ? C8A Cr1 C5 C6 101.69(13) . . . . ? C4A Cr1 C5 C6 130.26(18) . . . . ? C1C Cr1 C5 C4A -178.18(13) . . . . ? C1A Cr1 C5 C4A 2.1(3) . . . . ? C1B Cr1 C5 C4A 92.60(13) . . . . ? C8 Cr1 C5 C4A -64.72(12) . . . . ? C7 Cr1 C5 C4A -101.47(13) . . . . ? C6 Cr1 C5 C4A -130.26(18) . . . . ? C8A Cr1 C5 C4A -28.57(11) . . . . ? C4A C5 C6 C7 6.5(3) . . . . ? Cr1 C5 C6 C7 -53.41(18) . . . . ? C4A C5 C6 Cr1 59.86(18) . . . . ? C1C Cr1 C6 C5 138.05(14) . . . . ? C1A Cr1 C6 C5 -132.9(2) . . . . ? C1B Cr1 C6 C5 49.86(15) . . . . ? C8 Cr1 C6 C5 -103.52(13) . . . . ? C7 Cr1 C6 C5 -132.90(18) . . . . ? C8A Cr1 C6 C5 -66.43(12) . . . . ? C4A Cr1 C6 C5 -30.26(12) . . . . ? C1C Cr1 C6 C7 -89.06(13) . . . . ? C1A Cr1 C6 C7 -0.1(3) . . . . ? C1B Cr1 C6 C7 -177.24(13) . . . . ? C8 Cr1 C6 C7 29.38(12) . . . . ? C5 Cr1 C6 C7 132.90(18) . . . . ? C8A Cr1 C6 C7 66.46(12) . . . . ? C4A Cr1 C6 C7 102.64(13) . . . . ? C5 C6 C7 C8 -1.0(3) . . . . ? Cr1 C6 C7 C8 -54.50(18) . . . . ? C5 C6 C7 Cr1 53.48(18) . . . . ? C1C Cr1 C7 C8 -138.00(14) . . . . ? C1A Cr1 C7 C8 -48.37(15) . . . . ? C1B Cr1 C7 C8 137.3(2) . . . . ? C5 Cr1 C7 C8 103.24(13) . . . . ? C6 Cr1 C7 C8 131.65(18) . . . . ? C8A Cr1 C7 C8 30.21(12) . . . . ? C4A Cr1 C7 C8 66.10(12) . . . . ? C1C Cr1 C7 C6 90.35(13) . . . . ? C1A Cr1 C7 C6 179.98(12) . . . . ? C1B Cr1 C7 C6 5.7(3) . . . . ? C8 Cr1 C7 C6 -131.65(18) . . . . ? C5 Cr1 C7 C6 -28.41(11) . . . . ? C8A Cr1 C7 C6 -101.44(13) . . . . ? C4A Cr1 C7 C6 -65.55(12) . . . . ? C6 C7 C8 C8A -5.5(3) . . . . ? Cr1 C7 C8 C8A -60.30(17) . . . . ? C6 C7 C8 Cr1 54.80(18) . . . . ? C1C Cr1 C8 C7 47.93(15) . . . . ? C1A Cr1 C8 C7 138.08(14) . . . . ? C1B Cr1 C8 C7 -134.6(2) . . . . ? C5 Cr1 C8 C7 -65.63(13) . . . . ? C6 Cr1 C8 C7 -29.41(12) . . . . ? C8A Cr1 C8 C7 -129.85(18) . . . . ? C4A Cr1 C8 C7 -102.18(13) . . . . ? C1C Cr1 C8 C8A 177.78(12) . . . . ? C1A Cr1 C8 C8A -92.07(13) . . . . ? C1B Cr1 C8 C8A -4.8(3) . . . . ? C5 Cr1 C8 C8A 64.23(12) . . . . ? C7 Cr1 C8 C8A 129.85(18) . . . . ? C6 Cr1 C8 C8A 100.45(13) . . . . ? C4A Cr1 C8 C8A 27.67(11) . . . . ? C7 C8 C8A C1 -176.53(19) . . . . ? Cr1 C8 C8A C1 125.23(18) . . . . ? C7 C8 C8A C4A 6.5(3) . . . . ? Cr1 C8 C8A C4A -51.73(17) . . . . ? C7 C8 C8A Cr1 58.23(18) . . . . ? C2 C1 C8A C8 -177.15(19) . . . . ? O1 C1 C8A C8 -2.7(3) . . . . ? C2 C1 C8A C4A -0.1(3) . . . . ? O1 C1 C8A C4A 174.34(17) . . . . ? C2 C1 C8A Cr1 -89.8(2) . . . . ? O1 C1 C8A Cr1 84.6(2) . . . . ? C4 C4A C8A C8 177.65(18) . . . . ? C5 C4A C8A C8 -1.1(3) . . . . ? Cr1 C4A C8A C8 49.59(16) . . . . ? C4 C4A C8A C1 0.5(3) . . . . ? C5 C4A C8A C1 -178.27(18) . . . . ? Cr1 C4A C8A C1 -127.53(17) . . . . ? C4 C4A C8A Cr1 128.06(19) . . . . ? C5 C4A C8A Cr1 -50.74(16) . . . . ? C1C Cr1 C8A C8 -4.3(2) . . . . ? C1A Cr1 C8A C8 88.31(13) . . . . ? C1B Cr1 C8A C8 177.76(13) . . . . ? C5 Cr1 C8A C8 -104.60(13) . . . . ? C7 Cr1 C8A C8 -30.49(12) . . . . ? C6 Cr1 C8A C8 -67.83(12) . . . . ? C4A Cr1 C8A C8 -133.87(17) . . . . ? C1C Cr1 C8A C1 -118.9(2) . . . . ? C1A Cr1 C8A C1 -26.32(19) . . . . ? C1B Cr1 C8A C1 63.1(2) . . . . ? C8 Cr1 C8A C1 -114.6(2) . . . . ? C5 Cr1 C8A C1 140.8(2) . . . . ? C7 Cr1 C8A C1 -145.1(2) . . . . ? C6 Cr1 C8A C1 177.6(2) . . . . ? C4A Cr1 C8A C1 111.5(2) . . . . ? C1C Cr1 C8A C4A 129.54(19) . . . . ? C1A Cr1 C8A C4A -137.82(13) . . . . ? C1B Cr1 C8A C4A -48.37(15) . . . . ? C8 Cr1 C8A C4A 133.87(17) . . . . ? C5 Cr1 C8A C4A 29.27(11) . . . . ? C7 Cr1 C8A C4A 103.38(13) . . . . ? C6 Cr1 C8A C4A 66.04(12) . . . . ? C2 C1 O1 Si1 -96.7(2) . . . . ? C8A C1 O1 Si1 88.8(2) . . . . ? C1 O1 Si1 C12 -49.40(18) . . . . ? C1 O1 Si1 C11 71.85(18) . . . . ? C1 O1 Si1 C13 -168.75(16) . . . . ? O1 Si1 C13 C16 62.30(16) . . . . ? C12 Si1 C13 C16 -56.27(18) . . . . ? C11 Si1 C13 C16 -179.05(15) . . . . ? O1 Si1 C13 C14 -58.48(17) . . . . ? C12 Si1 C13 C14 -177.05(15) . . . . ? C11 Si1 C13 C14 60.16(18) . . . . ? O1 Si1 C13 C15 -178.69(15) . . . . ? C12 Si1 C13 C15 62.74(18) . . . . ? C11 Si1 C13 C15 -60.05(18) . . . . ? C1 C2 C21 C22 -82.9(2) . . . . ? C3 C2 C21 C22 90.2(2) . . . . ? C4 C3 C31 C32 -102.9(2) . . . . ? C2 C3 C31 C32 76.3(3) . . . . ? C3 C4 O4 C41 88.1(2) . . . . ? C4A C4 O4 C41 -95.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.187 _refine_diff_density_min -0.184 _refine_diff_density_rms 0.036 #============================================================================== data_doe204 _database_code_CSD 205871 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (R)-Tricarbonyl[(eta6-4a,5,6,7,8,8a)-1-tert.butyldimethylsilyloxy-2,3- diethyl-4-methoxynaphthalene]chromium(0) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H32 Cr O5 Si' _chemical_formula_sum 'C24 H32 Cr O5 Si' _chemical_formula_weight 480.59 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' Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P6(5) _symmetry_Int_Tables_number 170 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' '-x, -y, z+1/2' 'y, -x+y, z+1/6' 'x-y, x, z+5/6' _cell_length_a 10.4375(1) _cell_length_b 10.4375(1) _cell_length_c 39.4397(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 3720.98(6) _cell_formula_units_Z 6 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2902 _cell_measurement_theta_min 1 _cell_measurement_theta_max 27.5 _exptl_crystal_description needles _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; dx = 50 mm, 150 sec./deg., 0.5 deg., 4 sets, 983 frames, mos.= 0.503(1) deg. ; _diffrn_ambient_temperature 123(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 'Nonius KappaCCD' _diffrn_measurement_method 'rotation in phi and omega, 0.5 deg.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 32874 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5624 _reflns_number_gt 4879 _reflns_threshold_expression >2sigma(I) _computing_data_collection Collect _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL-NT _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0266P)^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 riding _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 -0.015(11) _refine_ls_number_reflns 5624 _refine_ls_number_parameters 280 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0277 _refine_ls_wR_factor_ref 0.0570 _refine_ls_wR_factor_gt 0.0545 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _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 Cr1 Cr 0.86675(3) 0.17961(3) 0.909104(6) 0.02012(7) Uani 1 1 d . . . C1A C 0.9580(2) 0.0743(2) 0.89870(5) 0.0292(4) Uani 1 1 d . . . O1A O 1.01414(18) 0.00662(18) 0.89139(4) 0.0470(4) Uani 1 1 d . . . C1B C 0.8449(2) 0.1154(2) 0.95339(5) 0.0289(4) Uani 1 1 d . . . O1B O 0.83244(17) 0.07458(17) 0.98118(4) 0.0448(4) Uani 1 1 d . . . C1C C 1.0502(2) 0.3384(2) 0.92049(5) 0.0324(5) Uani 1 1 d . . . O1C O 1.16539(17) 0.43367(18) 0.92795(4) 0.0534(4) Uani 1 1 d . . . C1 C 0.59341(19) 0.23241(19) 0.94220(4) 0.0192(4) Uani 1 1 d . . . C2 C 0.63388(19) 0.3727(2) 0.95244(4) 0.0223(4) Uani 1 1 d . . . C3 C 0.7410(2) 0.4976(2) 0.93347(4) 0.0218(4) Uani 1 1 d . . . C4 C 0.81078(19) 0.47542(19) 0.90651(5) 0.0209(4) Uani 1 1 d . . . C4A C 0.77211(19) 0.3312(2) 0.89536(4) 0.0187(4) Uani 1 1 d . . . C5 C 0.8425(2) 0.3047(2) 0.86707(4) 0.0224(4) Uani 1 1 d . . . H5 H 0.9225 0.3863 0.8560 0.027 Uiso 1 1 calc R . . C6 C 0.7962(2) 0.1624(2) 0.85561(5) 0.0230(4) Uani 1 1 d . . . H6 H 0.8378 0.1480 0.8355 0.028 Uiso 1 1 calc R . . C7 C 0.6875(2) 0.0391(2) 0.87369(4) 0.0231(4) Uani 1 1 d . . . H7 H 0.6567 -0.0583 0.8660 0.028 Uiso 1 1 calc R . . C8 C 0.6253(2) 0.0606(2) 0.90295(4) 0.0213(4) Uani 1 1 d . . . H8 H 0.5587 -0.0224 0.9162 0.026 Uiso 1 1 calc R . . C8A C 0.66052(18) 0.20595(19) 0.91329(4) 0.0188(4) Uani 1 1 d . . . O1 O 0.49606(13) 0.11136(13) 0.96095(3) 0.0204(3) Uani 1 1 d . . . Si1 Si 0.31307(5) -0.00256(5) 0.957215(12) 0.01957(11) Uani 1 1 d . . . C11 C 0.2632(2) -0.0690(2) 0.91299(5) 0.0272(4) Uani 1 1 d . . . H11A H 0.3178 -0.1184 0.9060 0.041 Uiso 1 1 calc R . . H11B H 0.2887 0.0152 0.8980 0.041 Uiso 1 1 calc R . . H11C H 0.1567 -0.1390 0.9116 0.041 Uiso 1 1 calc R . . C12 C 0.2096(2) 0.0921(2) 0.97005(5) 0.0299(4) Uani 1 1 d . . . H12A H 0.2356 0.1279 0.9934 0.045 Uiso 1 1 calc R . . H12B H 0.1030 0.0223 0.9686 0.045 Uiso 1 1 calc R . . H12C H 0.2356 0.1760 0.9549 0.045 Uiso 1 1 calc R . . C13 C 0.2807(2) -0.1558(2) 0.98723(5) 0.0275(4) Uani 1 1 d . . . C14 C 0.3317(2) -0.0940(2) 1.02303(5) 0.0384(5) Uani 1 1 d . . . H14A H 0.2756 -0.0475 1.0309 0.058 Uiso 1 1 calc R . . H14B H 0.4374 -0.0204 1.0226 0.058 Uiso 1 1 calc R . . H14C H 0.3147 -0.1748 1.0384 0.058 Uiso 1 1 calc R . . C15 C 0.1148(2) -0.2725(2) 0.98790(5) 0.0385(5) Uani 1 1 d . . . H15A H 0.0582 -0.2270 0.9961 0.058 Uiso 1 1 calc R . . H15B H 0.0987 -0.3537 1.0030 0.058 Uiso 1 1 calc R . . H15C H 0.0819 -0.3112 0.9650 0.058 Uiso 1 1 calc R . . C16 C 0.3668(2) -0.2296(2) 0.97445(6) 0.0388(5) Uani 1 1 d . . . H16A H 0.3334 -0.2684 0.9515 0.058 Uiso 1 1 calc R . . H16B H 0.3494 -0.3110 0.9897 0.058 Uiso 1 1 calc R . . H16C H 0.4727 -0.1567 0.9740 0.058 Uiso 1 1 calc R . . C21 C 0.5761(2) 0.3940(2) 0.98610(5) 0.0290(4) Uani 1 1 d . . . H21A H 0.4728 0.3136 0.9895 0.035 Uiso 1 1 calc R . . H21B H 0.5770 0.4893 0.9859 0.035 Uiso 1 1 calc R . . C22 C 0.6730(3) 0.3930(3) 1.01521(5) 0.0503(7) Uani 1 1 d . . . H22A H 0.6351 0.4068 1.0368 0.075 Uiso 1 1 calc R . . H22B H 0.7750 0.4735 1.0119 0.075 Uiso 1 1 calc R . . H22C H 0.6710 0.2981 1.0155 0.075 Uiso 1 1 calc R . . C31 C 0.7757(2) 0.6520(2) 0.94274(5) 0.0277(4) Uani 1 1 d . . . H31A H 0.8708 0.7245 0.9322 0.033 Uiso 1 1 calc R . . H31B H 0.7871 0.6643 0.9676 0.033 Uiso 1 1 calc R . . C32 C 0.6538(2) 0.6844(2) 0.93100(6) 0.0370(5) Uani 1 1 d . . . H32A H 0.6803 0.7851 0.9377 0.056 Uiso 1 1 calc R . . H32B H 0.5596 0.6135 0.9416 0.056 Uiso 1 1 calc R . . H32C H 0.6441 0.6751 0.9063 0.056 Uiso 1 1 calc R . . O4 O 0.92825(14) 0.59300(14) 0.89011(3) 0.0259(3) Uani 1 1 d . . . C41 C 0.8898(2) 0.6588(2) 0.86277(5) 0.0309(5) Uani 1 1 d . . . H41A H 0.9801 0.7401 0.8529 0.046 Uiso 1 1 calc R . . H41B H 0.8274 0.6970 0.8714 0.046 Uiso 1 1 calc R . . H41C H 0.8356 0.5840 0.8453 0.046 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 Cr1 0.01946(15) 0.02053(15) 0.02202(14) 0.00008(12) -0.00008(12) 0.01124(13) C1A 0.0292(11) 0.0315(11) 0.0304(11) -0.0008(8) -0.0051(8) 0.0177(9) O1A 0.0504(10) 0.0533(10) 0.0598(10) -0.0122(8) -0.0094(8) 0.0429(9) C1B 0.0252(10) 0.0274(11) 0.0332(12) -0.0031(9) -0.0046(8) 0.0125(9) O1B 0.0481(10) 0.0512(10) 0.0281(8) 0.0094(7) -0.0031(7) 0.0196(8) C1C 0.0320(12) 0.0308(12) 0.0368(12) 0.0040(9) -0.0004(9) 0.0174(10) O1C 0.0324(9) 0.0387(10) 0.0666(11) -0.0014(8) -0.0149(8) 0.0011(8) C1 0.0178(9) 0.0218(10) 0.0179(9) 0.0034(7) 0.0020(7) 0.0097(8) C2 0.0188(9) 0.0227(9) 0.0249(10) -0.0021(8) 0.0021(7) 0.0101(8) C3 0.0199(9) 0.0208(10) 0.0250(9) -0.0005(7) -0.0010(8) 0.0104(8) C4 0.0172(9) 0.0214(9) 0.0236(9) 0.0029(8) -0.0006(8) 0.0092(8) C4A 0.0162(9) 0.0217(9) 0.0197(9) 0.0015(7) -0.0008(7) 0.0106(8) C5 0.0205(9) 0.0270(10) 0.0208(9) 0.0040(8) 0.0037(7) 0.0126(8) C6 0.0228(10) 0.0302(11) 0.0204(9) -0.0027(8) -0.0002(8) 0.0164(9) C7 0.0218(10) 0.0249(10) 0.0238(9) -0.0054(8) -0.0037(8) 0.0127(8) C8 0.0202(9) 0.0216(9) 0.0228(9) 0.0002(7) 0.0006(7) 0.0109(8) C8A 0.0173(9) 0.0212(9) 0.0186(9) 0.0009(7) -0.0013(7) 0.0100(7) O1 0.0199(6) 0.0182(6) 0.0208(6) 0.0020(5) 0.0036(5) 0.0077(5) Si1 0.0185(3) 0.0200(3) 0.0207(2) 0.0012(2) 0.0014(2) 0.0099(2) C11 0.0243(10) 0.0289(11) 0.0279(10) -0.0029(9) -0.0018(8) 0.0128(9) C12 0.0280(11) 0.0323(11) 0.0332(11) -0.0042(9) -0.0005(9) 0.0179(9) C13 0.0230(10) 0.0263(10) 0.0301(10) 0.0058(8) 0.0021(8) 0.0101(9) C14 0.0403(13) 0.0392(13) 0.0289(11) 0.0116(9) -0.0015(10) 0.0148(11) C15 0.0301(11) 0.0305(12) 0.0453(13) 0.0135(10) 0.0026(10) 0.0079(10) C16 0.0376(13) 0.0262(11) 0.0547(14) 0.0148(10) 0.0025(10) 0.0176(10) C21 0.0281(11) 0.0224(10) 0.0296(10) -0.0049(8) 0.0086(8) 0.0074(9) C22 0.0419(14) 0.0656(17) 0.0278(12) -0.0125(11) 0.0020(10) 0.0152(13) C31 0.0251(10) 0.0177(9) 0.0350(11) -0.0042(8) 0.0014(8) 0.0067(8) C32 0.0407(13) 0.0271(11) 0.0500(14) -0.0023(10) 0.0038(10) 0.0219(11) O4 0.0221(7) 0.0229(7) 0.0299(7) 0.0083(6) 0.0048(6) 0.0091(6) C41 0.0392(12) 0.0256(11) 0.0274(10) 0.0061(8) 0.0035(9) 0.0158(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 Cr1 C1A 1.825(2) . ? Cr1 C1B 1.843(2) . ? Cr1 C1C 1.855(2) . ? Cr1 C8 2.1961(18) . ? Cr1 C5 2.2013(18) . ? Cr1 C7 2.2042(19) . ? Cr1 C6 2.2120(18) . ? Cr1 C8A 2.3083(17) . ? Cr1 C4A 2.3104(17) . ? Cr1 Zar 1.736(1) . ? C1A O1A 1.158(2) . ? C1B O1B 1.160(2) . ? C1C O1C 1.151(2) . ? C1 C2 1.366(3) . ? C1 O1 1.376(2) . ? C1 C8A 1.435(2) . ? C2 C3 1.433(3) . ? C2 C21 1.520(2) . ? C3 C4 1.373(2) . ? C3 C31 1.509(2) . ? C4 O4 1.387(2) . ? C4 C4A 1.419(2) . ? C4A C8A 1.430(2) . ? C4A C5 1.437(2) . ? C5 C6 1.387(2) . ? C5 H5 0.9500 . ? C6 C7 1.412(3) . ? C6 H6 0.9500 . ? C7 C8 1.396(2) . ? C7 H7 0.9500 . ? C8 C8A 1.430(2) . ? C8 H8 0.9500 . ? O1 Si1 1.6771(13) . ? Si1 C11 1.8527(19) . ? Si1 C12 1.862(2) . ? Si1 C13 1.8795(19) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.533(3) . ? C13 C16 1.533(3) . ? C13 C15 1.541(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C21 C22 1.534(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 C32 1.542(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? O4 C41 1.439(2) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A Cr1 C1B 90.07(9) . . ? C1A Cr1 C1C 88.64(9) . . ? C1B Cr1 C1C 88.86(9) . . ? C1A Cr1 C8 115.55(8) . . ? C1B Cr1 C8 90.04(8) . . ? C1C Cr1 C8 155.79(8) . . ? C1A Cr1 C5 115.92(8) . . ? C1B Cr1 C5 154.01(8) . . ? C1C Cr1 C5 91.47(8) . . ? C8 Cr1 C5 79.20(7) . . ? C1A Cr1 C7 88.96(8) . . ? C1B Cr1 C7 116.68(8) . . ? C1C Cr1 C7 154.35(8) . . ? C8 Cr1 C7 36.99(6) . . ? C5 Cr1 C7 66.82(7) . . ? C1A Cr1 C6 89.39(7) . . ? C1B Cr1 C6 153.97(8) . . ? C1C Cr1 C6 117.14(8) . . ? C8 Cr1 C6 66.90(7) . . ? C5 Cr1 C6 36.64(6) . . ? C7 Cr1 C6 37.29(7) . . ? C1A Cr1 C8A 152.42(8) . . ? C1B Cr1 C8A 91.28(7) . . ? C1C Cr1 C8A 118.92(8) . . ? C8 Cr1 C8A 36.92(6) . . ? C5 Cr1 C8A 65.97(6) . . ? C7 Cr1 C8A 65.96(6) . . ? C6 Cr1 C8A 77.62(6) . . ? C1A Cr1 C4A 152.94(7) . . ? C1B Cr1 C4A 116.97(8) . . ? C1C Cr1 C4A 92.78(8) . . ? C8 Cr1 C4A 66.35(7) . . ? C5 Cr1 C4A 37.06(6) . . ? C7 Cr1 C4A 78.21(7) . . ? C6 Cr1 C4A 65.98(6) . . ? C8A Cr1 C4A 36.06(6) . . ? O1A C1A Cr1 178.42(17) . . ? O1B C1B Cr1 179.18(18) . . ? O1C C1C Cr1 177.72(19) . . ? C2 C1 O1 121.06(15) . . ? C2 C1 C8A 121.46(16) . . ? O1 C1 C8A 117.24(15) . . ? C1 C2 C3 120.24(16) . . ? C1 C2 C21 118.86(16) . . ? C3 C2 C21 120.58(16) . . ? C4 C3 C2 119.28(16) . . ? C4 C3 C31 120.25(16) . . ? C2 C3 C31 120.46(16) . . ? C3 C4 O4 121.38(16) . . ? C3 C4 C4A 121.71(16) . . ? O4 C4 C4A 116.81(15) . . ? C4 C4A C8A 119.12(15) . . ? C4 C4A C5 122.92(17) . . ? C8A C4A C5 117.95(16) . . ? C4 C4A Cr1 131.42(13) . . ? C8A C4A Cr1 71.89(10) . . ? C5 C4A Cr1 67.34(10) . . ? C6 C5 C4A 121.44(17) . . ? C6 C5 Cr1 72.10(11) . . ? C4A C5 Cr1 75.60(10) . . ? C6 C5 H5 119.3 . . ? C4A C5 H5 119.3 . . ? Cr1 C5 H5 124.6 . . ? C5 C6 C7 120.14(17) . . ? C5 C6 Cr1 71.26(10) . . ? C7 C6 Cr1 71.06(11) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? Cr1 C6 H6 130.3 . . ? C8 C7 C6 119.85(17) . . ? C8 C7 Cr1 71.19(11) . . ? C6 C7 Cr1 71.66(11) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? Cr1 C7 H7 129.5 . . ? C7 C8 C8A 120.82(16) . . ? C7 C8 Cr1 71.82(11) . . ? C8A C8 Cr1 75.81(10) . . ? C7 C8 H8 119.6 . . ? C8A C8 H8 119.6 . . ? Cr1 C8 H8 124.4 . . ? C4A C8A C8 119.29(15) . . ? C4A C8A C1 118.01(16) . . ? C8 C8A C1 122.63(16) . . ? C4A C8A Cr1 72.05(9) . . ? C8 C8A Cr1 67.27(10) . . ? C1 C8A Cr1 130.81(12) . . ? C1 O1 Si1 131.33(11) . . ? O1 Si1 C11 110.81(8) . . ? O1 Si1 C12 110.92(8) . . ? C11 Si1 C12 109.01(9) . . ? O1 Si1 C13 101.79(7) . . ? C11 Si1 C13 112.15(9) . . ? C12 Si1 C13 112.04(9) . . ? Si1 C11 H11A 109.5 . . ? Si1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si1 C12 H12A 109.5 . . ? Si1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C16 110.29(17) . . ? C14 C13 C15 109.47(16) . . ? C16 C13 C15 108.52(17) . . ? C14 C13 Si1 110.23(14) . . ? C16 C13 Si1 108.64(13) . . ? C15 C13 Si1 109.66(13) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C2 C21 C22 109.96(17) . . ? C2 C21 H21A 109.7 . . ? C22 C21 H21A 109.7 . . ? C2 C21 H21B 109.7 . . ? C22 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C31 C32 112.17(16) . . ? C3 C31 H31A 109.2 . . ? C32 C31 H31A 109.2 . . ? C3 C31 H31B 109.2 . . ? C32 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C4 O4 C41 115.94(14) . . ? O4 C41 H41A 109.5 . . ? O4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1B Cr1 C1A O1A 141(8) . . . . ? C1C Cr1 C1A O1A -130(8) . . . . ? C8 Cr1 C1A O1A 51(8) . . . . ? C5 Cr1 C1A O1A -39(8) . . . . ? C7 Cr1 C1A O1A 24(8) . . . . ? C6 Cr1 C1A O1A -13(8) . . . . ? C8A Cr1 C1A O1A 48(8) . . . . ? C4A Cr1 C1A O1A -37(8) . . . . ? C1A Cr1 C1B O1B 16(15) . . . . ? C1C Cr1 C1B O1B -72(15) . . . . ? C8 Cr1 C1B O1B 132(15) . . . . ? C5 Cr1 C1B O1B -163(15) . . . . ? C7 Cr1 C1B O1B 105(15) . . . . ? C6 Cr1 C1B O1B 105(15) . . . . ? C8A Cr1 C1B O1B 169(76) . . . . ? C4A Cr1 C1B O1B -165(15) . . . . ? C1A Cr1 C1C O1C -35(5) . . . . ? C1B Cr1 C1C O1C 55(5) . . . . ? C8 Cr1 C1C O1C 143(5) . . . . ? C5 Cr1 C1C O1C -151(5) . . . . ? C7 Cr1 C1C O1C -120(5) . . . . ? C6 Cr1 C1C O1C -123(5) . . . . ? C8A Cr1 C1C O1C 146(5) . . . . ? C4A Cr1 C1C O1C 172(96) . . . . ? O1 C1 C2 C3 176.89(16) . . . . ? C8A C1 C2 C3 2.6(3) . . . . ? O1 C1 C2 C21 3.3(3) . . . . ? C8A C1 C2 C21 -170.90(16) . . . . ? C1 C2 C3 C4 -5.0(3) . . . . ? C21 C2 C3 C4 168.41(17) . . . . ? C1 C2 C3 C31 174.29(17) . . . . ? C21 C2 C3 C31 -12.3(3) . . . . ? C2 C3 C4 O4 -171.64(16) . . . . ? C31 C3 C4 O4 9.0(3) . . . . ? C2 C3 C4 C4A 4.6(3) . . . . ? C31 C3 C4 C4A -174.71(17) . . . . ? C3 C4 C4A C8A -1.8(3) . . . . ? O4 C4 C4A C8A 174.60(15) . . . . ? C3 C4 C4A C5 179.55(17) . . . . ? O4 C4 C4A C5 -4.0(3) . . . . ? C3 C4 C4A Cr1 -92.8(2) . . . . ? O4 C4 C4A Cr1 83.6(2) . . . . ? C1A Cr1 C4A C4 -118.3(2) . . . . ? C1B Cr1 C4A C4 64.26(19) . . . . ? C1C Cr1 C4A C4 -25.88(18) . . . . ? C8 Cr1 C4A C4 141.43(18) . . . . ? C5 Cr1 C4A C4 -114.6(2) . . . . ? C7 Cr1 C4A C4 178.36(18) . . . . ? C6 Cr1 C4A C4 -144.46(18) . . . . ? C8A Cr1 C4A C4 113.2(2) . . . . ? C1A Cr1 C4A C8A 128.44(18) . . . . ? C1B Cr1 C4A C8A -48.97(13) . . . . ? C1C Cr1 C4A C8A -139.11(11) . . . . ? C8 Cr1 C4A C8A 28.20(9) . . . . ? C5 Cr1 C4A C8A 132.13(15) . . . . ? C7 Cr1 C4A C8A 65.14(10) . . . . ? C6 Cr1 C4A C8A 102.31(11) . . . . ? C1A Cr1 C4A C5 -3.7(2) . . . . ? C1B Cr1 C4A C5 178.90(12) . . . . ? C1C Cr1 C4A C5 88.76(12) . . . . ? C8 Cr1 C4A C5 -103.93(12) . . . . ? C7 Cr1 C4A C5 -66.99(11) . . . . ? C6 Cr1 C4A C5 -29.81(11) . . . . ? C8A Cr1 C4A C5 -132.13(15) . . . . ? C4 C4A C5 C6 -176.21(17) . . . . ? C8A C4A C5 C6 5.1(3) . . . . ? Cr1 C4A C5 C6 58.08(15) . . . . ? C4 C4A C5 Cr1 125.72(17) . . . . ? C8A C4A C5 Cr1 -52.94(14) . . . . ? C1A Cr1 C5 C6 47.69(13) . . . . ? C1B Cr1 C5 C6 -132.68(18) . . . . ? C1C Cr1 C5 C6 136.89(12) . . . . ? C8 Cr1 C5 C6 -65.61(11) . . . . ? C7 Cr1 C5 C6 -29.01(11) . . . . ? C8A Cr1 C5 C6 -101.90(12) . . . . ? C4A Cr1 C5 C6 -130.45(16) . . . . ? C1A Cr1 C5 C4A 178.13(11) . . . . ? C1B Cr1 C5 C4A -2.2(2) . . . . ? C1C Cr1 C5 C4A -92.66(12) . . . . ? C8 Cr1 C5 C4A 64.84(11) . . . . ? C7 Cr1 C5 C4A 101.43(12) . . . . ? C6 Cr1 C5 C4A 130.45(16) . . . . ? C8A Cr1 C5 C4A 28.55(10) . . . . ? C4A C5 C6 C7 -6.2(3) . . . . ? Cr1 C5 C6 C7 53.60(16) . . . . ? C4A C5 C6 Cr1 -59.76(15) . . . . ? C1A Cr1 C6 C5 -138.31(12) . . . . ? C1B Cr1 C6 C5 132.79(18) . . . . ? C1C Cr1 C6 C5 -50.15(13) . . . . ? C8 Cr1 C6 C5 103.43(12) . . . . ? C7 Cr1 C6 C5 132.61(16) . . . . ? C8A Cr1 C6 C5 66.20(11) . . . . ? C4A Cr1 C6 C5 30.14(10) . . . . ? C1A Cr1 C6 C7 89.08(12) . . . . ? C1B Cr1 C6 C7 0.2(2) . . . . ? C1C Cr1 C6 C7 177.24(11) . . . . ? C8 Cr1 C6 C7 -29.18(10) . . . . ? C5 Cr1 C6 C7 -132.61(16) . . . . ? C8A Cr1 C6 C7 -66.41(11) . . . . ? C4A Cr1 C6 C7 -102.47(11) . . . . ? C5 C6 C7 C8 0.7(3) . . . . ? Cr1 C6 C7 C8 54.42(15) . . . . ? C5 C6 C7 Cr1 -53.70(16) . . . . ? C1A Cr1 C7 C8 137.81(12) . . . . ? C1B Cr1 C7 C8 48.26(13) . . . . ? C1C Cr1 C7 C8 -137.50(18) . . . . ? C5 Cr1 C7 C8 -103.28(12) . . . . ? C6 Cr1 C7 C8 -131.82(16) . . . . ? C8A Cr1 C7 C8 -30.38(10) . . . . ? C4A Cr1 C7 C8 -66.17(11) . . . . ? C1A Cr1 C7 C6 -90.36(12) . . . . ? C1B Cr1 C7 C6 -179.91(11) . . . . ? C1C Cr1 C7 C6 -5.7(2) . . . . ? C8 Cr1 C7 C6 131.82(16) . . . . ? C5 Cr1 C7 C6 28.54(10) . . . . ? C8A Cr1 C7 C6 101.44(11) . . . . ? C4A Cr1 C7 C6 65.65(10) . . . . ? C6 C7 C8 C8A 5.6(3) . . . . ? Cr1 C7 C8 C8A 60.23(15) . . . . ? C6 C7 C8 Cr1 -54.64(16) . . . . ? C1A Cr1 C8 C7 -48.09(13) . . . . ? C1B Cr1 C8 C7 -138.18(12) . . . . ? C1C Cr1 C8 C7 134.50(19) . . . . ? C5 Cr1 C8 C7 65.62(11) . . . . ? C6 Cr1 C8 C7 29.39(10) . . . . ? C8A Cr1 C8 C7 129.74(15) . . . . ? C4A Cr1 C8 C7 102.16(12) . . . . ? C1A Cr1 C8 C8A -177.83(10) . . . . ? C1B Cr1 C8 C8A 92.07(11) . . . . ? C1C Cr1 C8 C8A 4.8(2) . . . . ? C5 Cr1 C8 C8A -64.13(10) . . . . ? C7 Cr1 C8 C8A -129.74(15) . . . . ? C6 Cr1 C8 C8A -100.35(11) . . . . ? C4A Cr1 C8 C8A -27.59(9) . . . . ? C4 C4A C8A C8 -177.58(16) . . . . ? C5 C4A C8A C8 1.1(2) . . . . ? Cr1 C4A C8A C8 -49.65(14) . . . . ? C4 C4A C8A C1 -0.6(2) . . . . ? C5 C4A C8A C1 178.07(16) . . . . ? Cr1 C4A C8A C1 127.29(15) . . . . ? C4 C4A C8A Cr1 -127.92(16) . . . . ? C5 C4A C8A Cr1 50.78(14) . . . . ? C7 C8 C8A C4A -6.5(3) . . . . ? Cr1 C8 C8A C4A 51.82(14) . . . . ? C7 C8 C8A C1 176.74(17) . . . . ? Cr1 C8 C8A C1 -124.97(16) . . . . ? C7 C8 C8A Cr1 -58.28(15) . . . . ? C2 C1 C8A C4A 0.2(2) . . . . ? O1 C1 C8A C4A -174.29(15) . . . . ? C2 C1 C8A C8 176.99(17) . . . . ? O1 C1 C8A C8 2.5(2) . . . . ? C2 C1 C8A Cr1 90.0(2) . . . . ? O1 C1 C8A Cr1 -84.4(2) . . . . ? C1A Cr1 C8A C4A -129.67(16) . . . . ? C1B Cr1 C8A C4A 137.74(11) . . . . ? C1C Cr1 C8A C4A 48.34(13) . . . . ? C8 Cr1 C8A C4A -133.89(15) . . . . ? C5 Cr1 C8A C4A -29.30(10) . . . . ? C7 Cr1 C8A C4A -103.45(11) . . . . ? C6 Cr1 C8A C4A -66.01(10) . . . . ? C1A Cr1 C8A C8 4.2(2) . . . . ? C1B Cr1 C8A C8 -88.37(11) . . . . ? C1C Cr1 C8A C8 -177.77(11) . . . . ? C5 Cr1 C8A C8 104.60(11) . . . . ? C7 Cr1 C8A C8 30.44(10) . . . . ? C6 Cr1 C8A C8 67.88(10) . . . . ? C4A Cr1 C8A C8 133.89(15) . . . . ? C1A Cr1 C8A C1 118.5(2) . . . . ? C1B Cr1 C8A C1 25.88(17) . . . . ? C1C Cr1 C8A C1 -63.53(19) . . . . ? C8 Cr1 C8A C1 114.2(2) . . . . ? C5 Cr1 C8A C1 -141.16(18) . . . . ? C7 Cr1 C8A C1 144.68(18) . . . . ? C6 Cr1 C8A C1 -177.88(18) . . . . ? C4A Cr1 C8A C1 -111.9(2) . . . . ? C2 C1 O1 Si1 96.91(19) . . . . ? C8A C1 O1 Si1 -88.61(18) . . . . ? C1 O1 Si1 C11 49.42(16) . . . . ? C1 O1 Si1 C12 -71.80(16) . . . . ? C1 O1 Si1 C13 168.84(14) . . . . ? O1 Si1 C13 C14 58.31(15) . . . . ? C11 Si1 C13 C14 176.78(13) . . . . ? C12 Si1 C13 C14 -60.25(17) . . . . ? O1 Si1 C13 C16 -62.65(15) . . . . ? C11 Si1 C13 C16 55.83(16) . . . . ? C12 Si1 C13 C16 178.79(14) . . . . ? O1 Si1 C13 C15 178.90(13) . . . . ? C11 Si1 C13 C15 -62.63(16) . . . . ? C12 Si1 C13 C15 60.34(16) . . . . ? C1 C2 C21 C22 83.1(2) . . . . ? C3 C2 C21 C22 -90.4(2) . . . . ? C4 C3 C31 C32 103.0(2) . . . . ? C2 C3 C31 C32 -76.3(2) . . . . ? C3 C4 O4 C41 -88.1(2) . . . . ? C4A C4 O4 C41 95.53(19) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.196 _refine_diff_density_min -0.219 _refine_diff_density_rms 0.044 #============================================================================== #_eof # End of Crystallographic Information File