# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2232 #============================================================================== data_global #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dr. Hans-Georg Stammler ; _publ_contact_author_phone '49 521 1066165' _publ_contact_author_fax '49 521 1066146' _publ_contact_author_email georg.stammler@uni-bielefeld.de _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for deposition. Dear Madam or Sir, please find enclosed the crystallographic data of compound6a for deposition in your data file. With kind regards i. A. Beate Neumann ; #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Synthesis, structure and reactivity of highly functionalized \h^1^-stibaallyl- iron complexes [(\h^1^-C~5~Me~5~)(CO)~2~Fe-Sb(X)C(OSiMe~3~)\\db CR^1^R^2^] [R^1^ = R^2^ = Ph; R^1^ = Me, R^2^ = Ph; R^1^ = c-C~6~H~11~, R^2^ = Ph; X = Me~3~Si, Cl, C\\tb C-Ph, C(N~2~SiMe~3~] ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Weber, Lothar' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Pumpenmeier, Lars' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Stammler, Hans-Georg' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; 'Neumann, Beate' ; Fakult\"at f. Chemie Universit\"at Bielefeld 33615 Bielefeld Germany ; #============================================================================== data_compound6a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H34 Cl Fe O3 Sb Si' _chemical_formula_weight 671.70 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Sb' 'Sb' -0.5866 1.5461 '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 8.565(2) _cell_length_b 17.591(3) _cell_length_c 20.285(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.87(2) _cell_angle_gamma 90.00 _cell_volume 3011.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 11.8 _exptl_crystal_description column _exptl_crystal_colour orange _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.534 _exptl_absorpt_correction_type 'semi-empirical from psi-scans' _exptl_absorpt_correction_T_min 0.430 _exptl_absorpt_correction_T_max 0.528 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P2(1) diffractometer' _diffrn_measurement_method 'Wyckoff-scan' _diffrn_refln_scan_width 1.20 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9302 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 29.99 _reflns_number_total 8766 _reflns_number_gt 6167 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'P3 (1989)' _computing_cell_refinement 'P3 (1989)' _computing_data_reduction 'SHELXTL-PLUS (1990)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-PLUS (1990)' _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 w=1/[\s^2^(Fo^2^)+(0.0278P)^2^+1.3166P] 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 8766 _refine_ls_number_parameters 333 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.0929 _refine_ls_wR_factor_gt 0.0820 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.56423(3) 0.732131(14) 0.832477(11) 0.02328(6) Uani 1 d . . . Fe1 Fe 0.72466(6) 0.65759(3) 0.92796(2) 0.02011(11) Uani 1 d . . . Cl1 Cl 0.29531(12) 0.70337(8) 0.84762(5) 0.0442(3) Uani 1 d . . . Si1 Si 0.31974(12) 0.56266(6) 0.70179(5) 0.0273(2) Uani 1 d . . . O1 O 0.9169(3) 0.58772(18) 0.83955(14) 0.0437(8) Uani 1 d . . . O2 O 0.4942(4) 0.53522(19) 0.91188(16) 0.0593(10) Uani 1 d . . . O3 O 0.4926(3) 0.58567(14) 0.74941(11) 0.0221(5) Uani 1 d . . . C1 C 0.8580(4) 0.75062(19) 0.97199(16) 0.0249(8) Uani 1 d . . . C2 C 0.9298(4) 0.6805(2) 0.99816(16) 0.0236(7) Uani 1 d . . . C3 C 0.8201(4) 0.6399(2) 1.02973(16) 0.0235(7) Uani 1 d . . . C4 C 0.6783(4) 0.6852(2) 1.02427(16) 0.0252(7) Uani 1 d . . . C5 C 0.7030(5) 0.7535(2) 0.98964(16) 0.0259(8) Uani 1 d . . . C6 C 0.9327(5) 0.8126(2) 0.9379(2) 0.0394(10) Uani 1 d . . . H6A H 0.9606 0.8549 0.9691 0.059 Uiso 1 calc R . . H6B H 0.8579 0.8303 0.8989 0.059 Uiso 1 calc R . . H6C H 1.0286 0.7932 0.9234 0.059 Uiso 1 calc R . . C7 C 1.0967(4) 0.6563(3) 0.99597(19) 0.0350(9) Uani 1 d . . . H7A H 1.1655 0.6715 1.0376 0.053 Uiso 1 calc R . . H7B H 1.1332 0.6807 0.9579 0.053 Uiso 1 calc R . . H7C H 1.1005 0.6010 0.9910 0.053 Uiso 1 calc R . . C8 C 0.8467(5) 0.5657(2) 1.06581(19) 0.0351(9) Uani 1 d . . . H8A H 0.9373 0.5396 1.0524 0.053 Uiso 1 calc R . . H8B H 0.7518 0.5339 1.0546 0.053 Uiso 1 calc R . . H8C H 0.8682 0.5749 1.1142 0.053 Uiso 1 calc R . . C9 C 0.5357(5) 0.6673(3) 1.0548(2) 0.0392(10) Uani 1 d . . . H9A H 0.5488 0.6892 1.0999 0.059 Uiso 1 calc R . . H9B H 0.5236 0.6121 1.0575 0.059 Uiso 1 calc R . . H9C H 0.4413 0.6890 1.0271 0.059 Uiso 1 calc R . . C10 C 0.5915(5) 0.8198(2) 0.97998(19) 0.0400(10) Uani 1 d . . . H10A H 0.4820 0.8014 0.9731 0.060 Uiso 1 calc R . . H10B H 0.6089 0.8492 0.9408 0.060 Uiso 1 calc R . . H10C H 0.6108 0.8524 1.0198 0.060 Uiso 1 calc R . . C11 C 0.8374(4) 0.6166(2) 0.87235(17) 0.0281(8) Uani 1 d . . . C12 C 0.5827(5) 0.5846(2) 0.91609(18) 0.0338(9) Uani 1 d . . . C13 C 0.5693(4) 0.65450(19) 0.74934(15) 0.0206(7) Uani 1 d . . . C14 C 0.6669(4) 0.67162(18) 0.70685(15) 0.0185(7) Uani 1 d . . . C15 C 0.7403(4) 0.74934(18) 0.70991(16) 0.0221(7) Uani 1 d . . . C16 C 0.8992(4) 0.7591(2) 0.73786(18) 0.0272(8) Uani 1 d . . . H16 H 0.9612 0.7164 0.7550 0.033 Uiso 1 calc R . . C17 C 0.9675(5) 0.8308(2) 0.7409(2) 0.0376(10) Uani 1 d . . . H17 H 1.0759 0.8368 0.7603 0.045 Uiso 1 calc R . . C18 C 0.8805(5) 0.8931(2) 0.71617(19) 0.0372(10) Uani 1 d . . . H18 H 0.9280 0.9421 0.7183 0.045 Uiso 1 calc R . . C19 C 0.7228(5) 0.8840(2) 0.6880(2) 0.0380(10) Uani 1 d . . . H19 H 0.6616 0.9268 0.6709 0.046 Uiso 1 calc R . . C20 C 0.6537(5) 0.8126(2) 0.68474(19) 0.0323(9) Uani 1 d . . . H20 H 0.5454 0.8070 0.6650 0.039 Uiso 1 calc R . . C21 C 0.7152(4) 0.6183(2) 0.65752(16) 0.0208(7) Uani 1 d . . . C22 C 0.7170(5) 0.6417(2) 0.59177(17) 0.0275(8) Uani 1 d . . . H22 H 0.6844 0.6918 0.5784 0.033 Uiso 1 calc R . . C23 C 0.7660(5) 0.5923(2) 0.54575(18) 0.0324(9) Uani 1 d . . . H23 H 0.7651 0.6086 0.5010 0.039 Uiso 1 calc R . . C24 C 0.8161(5) 0.5194(2) 0.56491(19) 0.0359(9) Uani 1 d . . . H24 H 0.8501 0.4859 0.5335 0.043 Uiso 1 calc R . . C25 C 0.8165(5) 0.4958(2) 0.63010(19) 0.0323(9) Uani 1 d . . . H25 H 0.8518 0.4461 0.6436 0.039 Uiso 1 calc R . . C26 C 0.7653(4) 0.5446(2) 0.67582(17) 0.0263(8) Uani 1 d . . . H26 H 0.7645 0.5276 0.7202 0.032 Uiso 1 calc R . . C27 C 0.2172(5) 0.6503(3) 0.6678(2) 0.0420(11) Uani 1 d . . . H27A H 0.2088 0.6854 0.7046 0.063 Uiso 1 calc R . . H27B H 0.1109 0.6375 0.6441 0.063 Uiso 1 calc R . . H27C H 0.2777 0.6745 0.6367 0.063 Uiso 1 calc R . . C28 C 0.3550(5) 0.5011(3) 0.6315(2) 0.0444(11) Uani 1 d . . . H28A H 0.4120 0.5300 0.6018 0.067 Uiso 1 calc R . . H28B H 0.2532 0.4839 0.6063 0.067 Uiso 1 calc R . . H28C H 0.4185 0.4570 0.6492 0.067 Uiso 1 calc R . . C29 C 0.2109(5) 0.5084(3) 0.7580(2) 0.0385(10) Uani 1 d . . . H29A H 0.2743 0.4645 0.7763 0.058 Uiso 1 calc R . . H29B H 0.1095 0.4909 0.7327 0.058 Uiso 1 calc R . . H29C H 0.1914 0.5413 0.7948 0.058 Uiso 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 Sb1 0.03051(12) 0.02314(11) 0.01634(9) -0.00086(10) 0.00443(8) 0.00504(11) Fe1 0.0226(2) 0.0198(2) 0.0175(2) -0.00089(19) 0.00225(18) -0.0020(2) Cl1 0.0250(5) 0.0785(8) 0.0303(5) -0.0029(5) 0.0082(4) 0.0074(5) Si1 0.0260(5) 0.0341(6) 0.0213(5) -0.0015(4) 0.0024(4) -0.0008(5) O1 0.0425(18) 0.054(2) 0.0354(15) -0.0103(14) 0.0083(13) 0.0179(16) O2 0.070(2) 0.051(2) 0.052(2) 0.0079(16) -0.0049(17) -0.0372(19) O3 0.0227(12) 0.0228(13) 0.0204(11) 0.0017(9) 0.0030(9) -0.0038(10) C1 0.0320(19) 0.0218(19) 0.0194(15) -0.0022(12) 0.0003(14) -0.0094(14) C2 0.0234(17) 0.0296(19) 0.0175(15) -0.0019(14) 0.0026(13) -0.0055(15) C3 0.0236(17) 0.0286(19) 0.0184(15) 0.0000(14) 0.0042(13) -0.0016(15) C4 0.0251(18) 0.0304(19) 0.0206(16) -0.0004(14) 0.0051(14) -0.0024(16) C5 0.035(2) 0.0245(19) 0.0176(15) -0.0015(13) 0.0021(14) 0.0004(15) C6 0.049(3) 0.035(2) 0.034(2) 0.0041(18) 0.0053(19) -0.017(2) C7 0.026(2) 0.047(3) 0.031(2) -0.0027(18) 0.0046(16) -0.0014(19) C8 0.039(2) 0.032(2) 0.033(2) 0.0077(17) 0.0026(17) -0.0046(19) C9 0.031(2) 0.054(3) 0.035(2) 0.004(2) 0.0134(17) -0.001(2) C10 0.061(3) 0.031(2) 0.029(2) -0.0027(17) 0.0073(19) 0.014(2) C11 0.030(2) 0.031(2) 0.0210(16) -0.0039(15) -0.0016(15) 0.0018(17) C12 0.042(2) 0.033(2) 0.0238(18) 0.0042(16) -0.0009(16) -0.0109(19) C13 0.0242(17) 0.0213(17) 0.0155(14) 0.0011(12) 0.0013(13) 0.0026(14) C14 0.0234(17) 0.0178(16) 0.0133(14) -0.0011(12) 0.0004(12) 0.0033(13) C15 0.0293(18) 0.0207(18) 0.0176(14) -0.0021(12) 0.0074(13) -0.0013(14) C16 0.0265(18) 0.0254(19) 0.0311(18) 0.0011(15) 0.0093(14) -0.0007(16) C17 0.030(2) 0.039(2) 0.044(2) -0.0047(19) 0.0087(18) -0.0055(19) C18 0.052(3) 0.025(2) 0.036(2) -0.0072(17) 0.0117(19) -0.0096(19) C19 0.051(3) 0.0187(19) 0.041(2) 0.0014(17) -0.002(2) -0.0004(19) C20 0.036(2) 0.026(2) 0.0317(19) 0.0035(16) -0.0023(16) -0.0024(17) C21 0.0210(16) 0.0212(17) 0.0203(15) -0.0025(13) 0.0041(13) -0.0034(14) C22 0.037(2) 0.0238(18) 0.0222(16) -0.0011(14) 0.0073(15) -0.0006(16) C23 0.047(2) 0.033(2) 0.0192(16) 0.0006(15) 0.0126(16) 0.0015(19) C24 0.047(3) 0.033(2) 0.0303(19) -0.0118(17) 0.0153(18) 0.0018(19) C25 0.043(2) 0.0215(18) 0.0329(19) -0.0027(15) 0.0067(17) 0.0049(17) C26 0.033(2) 0.0232(18) 0.0226(16) 0.0002(14) 0.0037(15) 0.0005(16) C27 0.041(2) 0.052(3) 0.031(2) 0.0035(19) -0.0021(18) 0.010(2) C28 0.047(3) 0.049(3) 0.035(2) -0.014(2) 0.0007(19) -0.007(2) C29 0.031(2) 0.044(3) 0.042(2) 0.0061(19) 0.0085(18) -0.0078(19) _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 Sb1 C13 2.176(3) . Y Sb1 Cl1 2.4286(12) . Y Sb1 Fe1 2.5391(7) . Y Fe1 C12 1.757(4) . Y Fe1 C11 1.760(4) . Y Fe1 C2 2.102(3) . Y Fe1 C1 2.105(3) . Y Fe1 C3 2.109(3) . Y Fe1 C4 2.115(3) . Y Fe1 C5 2.128(3) . Y Si1 O3 1.673(3) . Y Si1 C27 1.848(4) . Y Si1 C28 1.856(4) . Y Si1 C29 1.857(4) . Y O1 C11 1.149(4) . Y O2 C12 1.146(5) . Y O3 C13 1.378(4) . Y C1 C5 1.434(5) . Y C1 C2 1.439(5) . Y C1 C6 1.492(5) . Y C2 C3 1.417(5) . Y C2 C7 1.500(5) . Y C3 C4 1.440(5) . Y C3 C8 1.495(5) . Y C4 C5 1.426(5) . Y C4 C9 1.495(5) . Y C5 C10 1.499(5) . Y C13 C14 1.333(4) . Y C14 C21 1.482(4) . Y C14 C15 1.502(5) . Y C15 C20 1.386(5) . Y C15 C16 1.392(5) . Y C16 C17 1.387(5) . Y C17 C18 1.371(6) . Y C18 C19 1.383(6) . Y C19 C20 1.384(5) . Y C21 C26 1.395(5) . Y C21 C22 1.398(4) . Y C22 C23 1.391(5) . Y C23 C24 1.386(6) . Y C24 C25 1.386(5) . Y C25 C26 1.389(5) . Y 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 C13 Sb1 Cl1 96.48(10) . . Y C13 Sb1 Fe1 100.78(9) . . Y Cl1 Sb1 Fe1 101.35(3) . . Y C12 Fe1 C11 93.19(19) . . Y C12 Fe1 C2 135.36(16) . . Y C11 Fe1 C2 91.50(15) . . Y C12 Fe1 C1 159.90(17) . . Y C11 Fe1 C1 105.85(16) . . Y C2 Fe1 C1 40.00(14) . . Y C12 Fe1 C3 99.77(15) . . Y C11 Fe1 C3 113.82(15) . . Y C2 Fe1 C3 39.32(13) . . Y C1 Fe1 C3 66.93(14) . . Y C12 Fe1 C4 93.40(16) . . Y C11 Fe1 C4 153.66(15) . . Y C2 Fe1 C4 66.28(13) . . Y C1 Fe1 C4 66.67(14) . . Y C3 Fe1 C4 39.86(13) . . Y C12 Fe1 C5 122.16(18) . . Y C11 Fe1 C5 144.53(17) . . Y C2 Fe1 C5 66.22(14) . . Y C1 Fe1 C5 39.60(14) . . Y C3 Fe1 C5 66.39(14) . . Y C4 Fe1 C5 39.29(13) . . Y C12 Fe1 Sb1 90.09(13) . . Y C11 Fe1 Sb1 90.40(12) . . Y C2 Fe1 Sb1 134.27(10) . . Y C1 Fe1 Sb1 96.05(10) . . Y C3 Fe1 Sb1 153.01(10) . . Y C4 Fe1 Sb1 115.06(10) . . Y C5 Fe1 Sb1 87.06(9) . . Y O3 Si1 C27 109.29(17) . . Y O3 Si1 C28 109.90(17) . . Y C27 Si1 C28 109.2(2) . . Y O3 Si1 C29 104.92(16) . . Y C27 Si1 C29 113.7(2) . . Y C28 Si1 C29 109.7(2) . . Y C13 O3 Si1 126.0(2) . . Y C5 C1 C2 107.1(3) . . Y C5 C1 C6 125.3(3) . . Y C2 C1 C6 127.4(4) . . Y C5 C1 Fe1 71.1(2) . . Y C2 C1 Fe1 69.89(19) . . Y C6 C1 Fe1 128.0(3) . . Y C3 C2 C1 108.9(3) . . Y C3 C2 C7 125.5(3) . . Y C1 C2 C7 125.5(3) . . Y C3 C2 Fe1 70.61(19) . . Y C1 C2 Fe1 70.11(19) . . Y C7 C2 Fe1 128.0(2) . . Y C2 C3 C4 107.6(3) . . Y C2 C3 C8 127.2(3) . . Y C4 C3 C8 125.1(3) . . Y C2 C3 Fe1 70.07(19) . . Y C4 C3 Fe1 70.31(19) . . Y C8 C3 Fe1 127.5(3) . . Y C5 C4 C3 108.0(3) . . Y C5 C4 C9 125.6(4) . . Y C3 C4 C9 126.2(3) . . Y C5 C4 Fe1 70.82(19) . . Y C3 C4 Fe1 69.83(19) . . Y C9 C4 Fe1 129.1(3) . . Y C4 C5 C1 108.3(3) . . Y C4 C5 C10 125.2(4) . . Y C1 C5 C10 126.2(3) . . Y C4 C5 Fe1 69.9(2) . . Y C1 C5 Fe1 69.35(19) . . Y C10 C5 Fe1 131.2(3) . . Y O1 C11 Fe1 175.6(3) . . Y O2 C12 Fe1 176.0(3) . . Y C14 C13 O3 123.4(3) . . Y C14 C13 Sb1 117.2(2) . . Y O3 C13 Sb1 118.5(2) . . Y C13 C14 C21 124.9(3) . . Y C13 C14 C15 118.9(3) . . Y C21 C14 C15 116.2(3) . . Y C20 C15 C16 118.4(3) . . Y C20 C15 C14 121.5(3) . . Y C16 C15 C14 120.2(3) . . Y C17 C16 C15 120.4(4) . . Y C18 C17 C16 120.8(4) . . Y C17 C18 C19 119.3(4) . . Y C18 C19 C20 120.3(4) . . Y C19 C20 C15 120.8(4) . . Y C26 C21 C22 118.3(3) . . Y C26 C21 C14 121.2(3) . . Y C22 C21 C14 120.5(3) . . Y C23 C22 C21 120.7(3) . . Y C24 C23 C22 120.2(3) . . Y C25 C24 C23 119.6(3) . . Y C24 C25 C26 120.2(4) . . Y C25 C26 C21 121.0(3) . . Y _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 29.99 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.430 _refine_diff_density_min -0.497 _refine_diff_density_rms 0.112 # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./