# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. #============================================================================== _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address L.Weber ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; P.Bayer ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; H.-G.Stammler ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; B.Neumann ; Fakultat f. Chemie Universitat Bielefeld 33615 Bielefeld Germany ; _publ_contact_author_name 'ProfD Lothar Weber' _publ_contact_author_address ; Fakultat fur Chemie University of Bielefeld Universitätsstr.25 Bielefeld 33615 GERMANY ; _publ_contact_author_email LOTHAR.WEBER@UNI-BIELEFELD.DE _publ_section_title ; Synthesis and Molecular Structure of Dicarbonylcyclopentadienyl-[1-(pentamethylcyclopentadienyldicarbonyliron) -3,3-bis(trimethylsilyl)-h3-1-arsa-2-phosphaallyl]molybdenum, the First Complex featuring an h3-Arsaphosphaallyl Ligand. ; #========================================================================= data_compound6 _database_code_depnum_ccdc_archive 'CCDC 250373' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 As Fe Mo O4 P Si2' _chemical_formula_sum 'C26 H38 As Fe Mo O4 P Si2' _chemical_formula_weight 728.42 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/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 12.96200(10) _cell_length_b 18.3280(2) _cell_length_c 13.7430(2) _cell_angle_alpha 90.00 _cell_angle_beta 104.2460(8) _cell_angle_gamma 90.00 _cell_volume 3164.49(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9523 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.03 _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 2.047 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6286 _exptl_absorpt_correction_T_max 0.6394 _exptl_absorpt_process_details 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18141 _diffrn_reflns_av_R_equivalents 0.0186 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 30.00 _reflns_number_total 9224 _reflns_number_gt 7859 _reflns_threshold_expression >2sigma(I) _computing_data_collection KappaCCD _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+3.6902P] 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 9224 _refine_ls_number_parameters 336 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0757 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 As1 As 0.480179(19) 0.158421(13) 0.289061(16) 0.02797(6) Uani 1 1 d . . . Mo1 Mo 0.578133(15) 0.127127(10) 0.136582(13) 0.02375(5) Uani 1 1 d . . . Fe1 Fe 0.38584(3) 0.272809(18) 0.27324(2) 0.02531(7) Uani 1 1 d . . . P1 P 0.65249(5) 0.18568(3) 0.30288(4) 0.02951(12) Uani 1 1 d . . . Si1 Si 0.67103(5) 0.01816(3) 0.37297(4) 0.02668(12) Uani 1 1 d . . . Si2 Si 0.84768(6) 0.10242(4) 0.29054(7) 0.04267(18) Uani 1 1 d . . . O1 O 0.27123(18) 0.23376(12) 0.07008(14) 0.0515(5) Uani 1 1 d . . . O2 O 0.55115(19) 0.35643(11) 0.21530(18) 0.0550(6) Uani 1 1 d . . . O3 O 0.35728(15) 0.05216(11) 0.10688(15) 0.0453(5) Uani 1 1 d . . . O4 O 0.64240(18) -0.03628(10) 0.13116(14) 0.0468(5) Uani 1 1 d . . . C1 C 0.24383(18) 0.30749(14) 0.30577(16) 0.0293(5) Uani 1 1 d . . . C2 C 0.27874(18) 0.24097(13) 0.35860(16) 0.0288(4) Uani 1 1 d . . . C3 C 0.37997(17) 0.25523(13) 0.42572(15) 0.0277(4) Uani 1 1 d . . . C4 C 0.40876(17) 0.32839(13) 0.41168(16) 0.0290(5) Uani 1 1 d . . . C5 C 0.32306(18) 0.36162(13) 0.33797(16) 0.0296(5) Uani 1 1 d . . . C6 C 0.1379(2) 0.31737(17) 0.23250(18) 0.0409(6) Uani 1 1 d . . . H6A H 0.0844 0.3309 0.2688 0.061 Uiso 1 1 calc R . . H6B H 0.1168 0.2716 0.1961 0.061 Uiso 1 1 calc R . . H6C H 0.1432 0.3560 0.1847 0.061 Uiso 1 1 calc R . . C7 C 0.2176(2) 0.17108(16) 0.3517(2) 0.0413(6) Uani 1 1 d . . . H7A H 0.2673 0.1299 0.3645 0.062 Uiso 1 1 calc R . . H7B H 0.1703 0.1664 0.2844 0.062 Uiso 1 1 calc R . . H7C H 0.1752 0.1712 0.4017 0.062 Uiso 1 1 calc R . . C8 C 0.4410(2) 0.20299(16) 0.50272(17) 0.0382(6) Uani 1 1 d . . . H8A H 0.4209 0.2102 0.5663 0.057 Uiso 1 1 calc R . . H8B H 0.5175 0.2118 0.5128 0.057 Uiso 1 1 calc R . . H8C H 0.4245 0.1528 0.4794 0.057 Uiso 1 1 calc R . . C9 C 0.5072(2) 0.36647(17) 0.4694(2) 0.0432(6) Uani 1 1 d . . . H9A H 0.5259 0.4055 0.4281 0.065 Uiso 1 1 calc R . . H9B H 0.5660 0.3314 0.4869 0.065 Uiso 1 1 calc R . . H9C H 0.4942 0.3874 0.5309 0.065 Uiso 1 1 calc R . . C10 C 0.3165(2) 0.44010(14) 0.3061(2) 0.0413(6) Uani 1 1 d . . . H10A H 0.2703 0.4445 0.2382 0.062 Uiso 1 1 calc R . . H10B H 0.3879 0.4580 0.3066 0.062 Uiso 1 1 calc R . . H10C H 0.2871 0.4691 0.3528 0.062 Uiso 1 1 calc R . . C11 C 0.3189(2) 0.24759(14) 0.14984(17) 0.0360(5) Uani 1 1 d . . . C12 C 0.4875(2) 0.32136(13) 0.23761(19) 0.0365(5) Uani 1 1 d . . . C13 C 0.70251(17) 0.09560(12) 0.29318(16) 0.0259(4) Uani 1 1 d . . . C14 C 0.5336(2) -0.02187(15) 0.3369(2) 0.0425(6) Uani 1 1 d . . . H14A H 0.5180 -0.0384 0.2670 0.064 Uiso 1 1 calc R . . H14B H 0.4816 0.0153 0.3441 0.064 Uiso 1 1 calc R . . H14C H 0.5294 -0.0634 0.3807 0.064 Uiso 1 1 calc R . . C15 C 0.6934(3) 0.05053(17) 0.50575(19) 0.0496(7) Uani 1 1 d . . . H15A H 0.6780 0.0108 0.5478 0.074 Uiso 1 1 calc R . . H15B H 0.6462 0.0919 0.5084 0.074 Uiso 1 1 calc R . . H15C H 0.7677 0.0659 0.5306 0.074 Uiso 1 1 calc R . . C16 C 0.7572(2) -0.06415(13) 0.37220(19) 0.0342(5) Uani 1 1 d . . . H16A H 0.8322 -0.0498 0.3925 0.051 Uiso 1 1 calc R . . H16B H 0.7415 -0.0850 0.3045 0.051 Uiso 1 1 calc R . . H16C H 0.7427 -0.1006 0.4193 0.051 Uiso 1 1 calc R . . C17 C 0.9345(3) 0.0885(2) 0.4209(3) 0.0815(14) Uani 1 1 d . . . H17A H 0.9260 0.0385 0.4428 0.122 Uiso 1 1 calc R . . H17B H 0.9136 0.1230 0.4671 0.122 Uiso 1 1 calc R . . H17C H 1.0091 0.0969 0.4205 0.122 Uiso 1 1 calc R . . C18 C 0.8860(3) 0.03521(19) 0.2034(3) 0.0680(11) Uani 1 1 d . . . H18A H 0.8405 0.0420 0.1356 0.102 Uiso 1 1 calc R . . H18B H 0.8770 -0.0144 0.2265 0.102 Uiso 1 1 calc R . . H18C H 0.9605 0.0429 0.2024 0.102 Uiso 1 1 calc R . . C19 C 0.8874(2) 0.19563(18) 0.2538(3) 0.0591(9) Uani 1 1 d . . . H19A H 0.9651 0.1983 0.2666 0.089 Uiso 1 1 calc R . . H19B H 0.8622 0.2330 0.2934 0.089 Uiso 1 1 calc R . . H19C H 0.8556 0.2039 0.1822 0.089 Uiso 1 1 calc R . . C20 C 0.4396(2) 0.08160(13) 0.12611(17) 0.0322(5) Uani 1 1 d . . . C21 C 0.6203(2) 0.02444(13) 0.13717(17) 0.0322(5) Uani 1 1 d . . . C22 C 0.6458(2) 0.23131(14) 0.0708(2) 0.0420(6) Uani 1 1 d . . . H22 H 0.6883 0.2666 0.1131 0.050 Uiso 1 1 calc R . . C23 C 0.6830(2) 0.16781(15) 0.0318(2) 0.0441(6) Uani 1 1 d . . . H23 H 0.7551 0.1526 0.0436 0.053 Uiso 1 1 calc R . . C24 C 0.5939(3) 0.13121(14) -0.02760(19) 0.0428(7) Uani 1 1 d . . . H24 H 0.5957 0.0869 -0.0629 0.051 Uiso 1 1 calc R . . C25 C 0.5023(3) 0.17107(14) -0.02583(18) 0.0406(6) Uani 1 1 d . . . H25 H 0.4314 0.1589 -0.0599 0.049 Uiso 1 1 calc R . . C26 C 0.5342(2) 0.23250(14) 0.03558(18) 0.0392(6) Uani 1 1 d . . . H26 H 0.4882 0.2687 0.0507 0.047 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 As1 0.03548(13) 0.03065(12) 0.02263(11) 0.00270(8) 0.01642(9) 0.00491(9) Mo1 0.03259(10) 0.02252(9) 0.02037(8) -0.00335(6) 0.01461(7) -0.00680(7) Fe1 0.02881(16) 0.03075(16) 0.01943(14) 0.00139(11) 0.01176(12) 0.00308(12) P1 0.0367(3) 0.0247(3) 0.0271(3) -0.0072(2) 0.0079(2) -0.0020(2) Si1 0.0312(3) 0.0280(3) 0.0242(3) -0.0001(2) 0.0135(2) 0.0002(2) Si2 0.0270(3) 0.0370(4) 0.0659(5) 0.0103(4) 0.0150(3) -0.0056(3) O1 0.0629(13) 0.0635(14) 0.0244(9) -0.0034(9) 0.0036(9) 0.0065(11) O2 0.0746(15) 0.0349(10) 0.0737(15) -0.0107(10) 0.0532(13) -0.0146(10) O3 0.0399(10) 0.0516(12) 0.0431(10) 0.0020(9) 0.0079(8) -0.0178(9) O4 0.0788(14) 0.0293(9) 0.0326(9) -0.0060(7) 0.0141(9) 0.0015(9) C1 0.0265(10) 0.0431(13) 0.0208(9) 0.0031(9) 0.0105(8) 0.0066(9) C2 0.0294(11) 0.0394(12) 0.0207(9) 0.0035(9) 0.0122(8) 0.0031(9) C3 0.0261(10) 0.0409(12) 0.0186(9) 0.0011(8) 0.0101(8) 0.0076(9) C4 0.0249(10) 0.0406(12) 0.0238(10) -0.0057(9) 0.0108(8) 0.0044(9) C5 0.0310(11) 0.0372(12) 0.0243(10) -0.0002(9) 0.0142(9) 0.0079(9) C6 0.0299(12) 0.0641(18) 0.0277(11) 0.0077(11) 0.0052(9) 0.0069(12) C7 0.0449(15) 0.0477(15) 0.0352(13) 0.0039(11) 0.0170(11) -0.0077(12) C8 0.0421(14) 0.0535(15) 0.0205(10) 0.0065(10) 0.0107(9) 0.0180(12) C9 0.0340(13) 0.0578(17) 0.0378(13) -0.0155(12) 0.0086(11) -0.0026(12) C10 0.0500(15) 0.0373(13) 0.0429(14) 0.0022(11) 0.0237(12) 0.0100(12) C11 0.0460(14) 0.0402(13) 0.0243(11) 0.0026(9) 0.0134(10) 0.0065(11) C12 0.0500(15) 0.0297(12) 0.0383(13) -0.0044(10) 0.0272(12) 0.0006(11) C13 0.0289(11) 0.0249(10) 0.0257(10) -0.0045(8) 0.0102(8) -0.0037(8) C14 0.0340(13) 0.0414(14) 0.0559(16) 0.0191(12) 0.0185(12) -0.0041(11) C15 0.075(2) 0.0501(16) 0.0248(12) 0.0003(11) 0.0150(13) 0.0150(15) C16 0.0392(13) 0.0309(12) 0.0376(12) 0.0026(10) 0.0191(10) 0.0034(10) C17 0.0441(18) 0.070(2) 0.108(3) 0.037(2) -0.0242(19) -0.0241(17) C18 0.061(2) 0.0525(19) 0.114(3) 0.0194(19) 0.065(2) 0.0136(16) C19 0.0357(15) 0.0508(18) 0.087(2) 0.0192(17) 0.0077(15) -0.0180(13) C20 0.0379(13) 0.0343(12) 0.0255(10) 0.0007(9) 0.0101(9) -0.0074(10) C21 0.0489(14) 0.0282(11) 0.0230(10) -0.0034(8) 0.0153(10) -0.0040(10) C22 0.0642(18) 0.0330(12) 0.0365(13) -0.0023(10) 0.0272(13) -0.0194(12) C23 0.0570(17) 0.0442(15) 0.0440(15) 0.0056(12) 0.0371(13) -0.0054(13) C24 0.078(2) 0.0309(12) 0.0282(12) -0.0011(9) 0.0299(13) -0.0042(13) C25 0.0627(17) 0.0358(13) 0.0251(11) 0.0047(9) 0.0145(11) -0.0084(12) C26 0.0641(18) 0.0299(12) 0.0314(12) 0.0049(9) 0.0270(12) 0.0000(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 As1 P1 2.2507(7) . ? As1 Fe1 2.4098(4) . ? As1 Mo1 2.7644(3) . ? Mo1 C20 1.953(2) . ? Mo1 C21 1.959(2) . ? Mo1 C24 2.316(2) . ? Mo1 C23 2.332(2) . ? Mo1 C25 2.349(3) . ? Mo1 C26 2.365(2) . ? Mo1 C22 2.371(2) . ? Mo1 C13 2.420(2) . ? Mo1 P1 2.4940(6) . ? Fe1 C12 1.757(3) . ? Fe1 C11 1.766(2) . ? Fe1 C1 2.097(2) . ? Fe1 C2 2.108(2) . ? Fe1 C5 2.112(2) . ? Fe1 C4 2.114(2) . ? Fe1 C3 2.140(2) . ? P1 C13 1.791(2) . ? Si1 C15 1.872(3) . ? Si1 C14 1.877(3) . ? Si1 C16 1.878(2) . ? Si1 C13 1.898(2) . ? Si2 C18 1.868(4) . ? Si2 C17 1.884(4) . ? Si2 C19 1.889(3) . ? Si2 C13 1.895(2) . ? O1 C11 1.146(3) . ? O2 C12 1.146(3) . ? O3 C20 1.167(3) . ? O4 C21 1.157(3) . ? C1 C5 1.418(3) . ? C1 C2 1.434(3) . ? C1 C6 1.501(3) . ? C2 C3 1.430(3) . ? C2 C7 1.497(4) . ? C3 C4 1.418(3) . ? C3 C8 1.500(3) . ? C4 C5 1.441(3) . ? C4 C9 1.499(3) . ? C5 C10 1.500(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C22 C26 1.408(4) . ? C22 C23 1.415(4) . ? C22 H22 0.9500 . ? C23 C24 1.410(4) . ? C23 H23 0.9500 . ? C24 C25 1.399(4) . ? C24 H24 0.9500 . ? C25 C26 1.407(4) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? 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 P1 As1 Fe1 106.587(19) . . ? P1 As1 Mo1 58.577(16) . . ? Fe1 As1 Mo1 115.444(11) . . ? C20 Mo1 C21 80.83(11) . . ? C20 Mo1 C24 104.00(10) . . ? C21 Mo1 C24 86.77(9) . . ? C20 Mo1 C23 139.12(10) . . ? C21 Mo1 C23 96.03(10) . . ? C24 Mo1 C23 35.30(11) . . ? C20 Mo1 C25 85.09(10) . . ? C21 Mo1 C25 112.60(9) . . ? C24 Mo1 C25 34.90(10) . . ? C23 Mo1 C25 58.32(11) . . ? C20 Mo1 C26 102.80(10) . . ? C21 Mo1 C26 144.44(9) . . ? C24 Mo1 C26 57.86(9) . . ? C23 Mo1 C26 57.94(10) . . ? C25 Mo1 C26 34.73(9) . . ? C20 Mo1 C22 137.37(11) . . ? C21 Mo1 C22 130.23(10) . . ? C24 Mo1 C22 58.21(9) . . ? C23 Mo1 C22 34.99(9) . . ? C25 Mo1 C22 57.95(10) . . ? C26 Mo1 C22 34.60(10) . . ? C20 Mo1 C13 111.27(9) . . ? C21 Mo1 C13 69.07(9) . . ? C24 Mo1 C13 132.44(9) . . ? C23 Mo1 C13 105.27(10) . . ? C25 Mo1 C13 163.40(9) . . ? C26 Mo1 C13 136.75(9) . . ? C22 Mo1 C13 107.64(9) . . ? C20 Mo1 P1 113.10(7) . . ? C21 Mo1 P1 111.41(7) . . ? C24 Mo1 P1 140.53(7) . . ? C23 Mo1 P1 106.00(8) . . ? C25 Mo1 P1 134.44(7) . . ? C26 Mo1 P1 99.75(7) . . ? C22 Mo1 P1 84.65(7) . . ? C13 Mo1 P1 42.71(5) . . ? C20 Mo1 As1 63.83(7) . . ? C21 Mo1 As1 112.09(7) . . ? C24 Mo1 As1 154.00(8) . . ? C23 Mo1 As1 147.97(7) . . ? C25 Mo1 As1 119.10(7) . . ? C26 Mo1 As1 100.74(6) . . ? C22 Mo1 As1 113.82(6) . . ? C13 Mo1 As1 72.85(5) . . ? P1 Mo1 As1 50.362(16) . . ? C12 Fe1 C11 95.15(12) . . ? C12 Fe1 C1 131.60(11) . . ? C11 Fe1 C1 91.99(10) . . ? C12 Fe1 C2 159.57(10) . . ? C11 Fe1 C2 103.12(11) . . ? C1 Fe1 C2 39.88(9) . . ? C12 Fe1 C5 96.90(10) . . ? C11 Fe1 C5 117.21(11) . . ? C1 Fe1 C5 39.38(9) . . ? C2 Fe1 C5 66.69(9) . . ? C12 Fe1 C4 93.31(10) . . ? C11 Fe1 C4 156.60(10) . . ? C1 Fe1 C4 66.32(9) . . ? C2 Fe1 C4 66.33(9) . . ? C5 Fe1 C4 39.89(9) . . ? C12 Fe1 C3 123.99(11) . . ? C11 Fe1 C3 140.69(11) . . ? C1 Fe1 C3 65.94(8) . . ? C2 Fe1 C3 39.33(9) . . ? C5 Fe1 C3 66.00(9) . . ? C4 Fe1 C3 38.93(9) . . ? C12 Fe1 As1 93.84(8) . . ? C11 Fe1 As1 88.70(8) . . ? C1 Fe1 As1 134.19(7) . . ? C2 Fe1 As1 95.62(7) . . ? C5 Fe1 As1 150.71(6) . . ? C4 Fe1 As1 112.47(7) . . ? C3 Fe1 As1 85.42(6) . . ? C13 P1 As1 99.15(7) . . ? C13 P1 Mo1 66.45(7) . . ? As1 P1 Mo1 71.061(18) . . ? C15 Si1 C14 106.90(15) . . ? C15 Si1 C16 108.08(13) . . ? C14 Si1 C16 102.20(12) . . ? C15 Si1 C13 108.80(12) . . ? C14 Si1 C13 117.68(11) . . ? C16 Si1 C13 112.63(10) . . ? C18 Si2 C17 109.2(2) . . ? C18 Si2 C19 106.97(16) . . ? C17 Si2 C19 103.79(16) . . ? C18 Si2 C13 112.99(14) . . ? C17 Si2 C13 109.66(15) . . ? C19 Si2 C13 113.71(13) . . ? C5 C1 C2 108.8(2) . . ? C5 C1 C6 126.7(2) . . ? C2 C1 C6 124.4(2) . . ? C5 C1 Fe1 70.87(12) . . ? C2 C1 Fe1 70.49(12) . . ? C6 C1 Fe1 126.86(16) . . ? C3 C2 C1 107.2(2) . . ? C3 C2 C7 125.8(2) . . ? C1 C2 C7 126.8(2) . . ? C3 C2 Fe1 71.53(12) . . ? C1 C2 Fe1 69.64(12) . . ? C7 C2 Fe1 127.76(17) . . ? C4 C3 C2 108.4(2) . . ? C4 C3 C8 126.1(2) . . ? C2 C3 C8 125.4(2) . . ? C4 C3 Fe1 69.53(12) . . ? C2 C3 Fe1 69.14(12) . . ? C8 C3 Fe1 130.33(15) . . ? C3 C4 C5 108.2(2) . . ? C3 C4 C9 125.9(2) . . ? C5 C4 C9 125.7(2) . . ? C3 C4 Fe1 71.54(12) . . ? C5 C4 Fe1 69.98(12) . . ? C9 C4 Fe1 127.84(16) . . ? C1 C5 C4 107.3(2) . . ? C1 C5 C10 126.5(2) . . ? C4 C5 C10 126.1(2) . . ? C1 C5 Fe1 69.75(13) . . ? C4 C5 Fe1 70.13(12) . . ? C10 C5 Fe1 128.05(16) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 Fe1 176.3(2) . . ? O2 C12 Fe1 176.3(2) . . ? P1 C13 Si2 108.67(11) . . ? P1 C13 Si1 120.88(12) . . ? Si2 C13 Si1 114.58(12) . . ? P1 C13 Mo1 70.85(8) . . ? Si2 C13 Mo1 114.49(10) . . ? Si1 C13 Mo1 120.09(10) . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 Mo1 170.9(2) . . ? O4 C21 Mo1 175.7(2) . . ? C26 C22 C23 107.4(2) . . ? C26 C22 Mo1 72.45(14) . . ? C23 C22 Mo1 71.00(14) . . ? C26 C22 H22 126.3 . . ? C23 C22 H22 126.3 . . ? Mo1 C22 H22 122.0 . . ? C24 C23 C22 107.7(3) . . ? C24 C23 Mo1 71.73(14) . . ? C22 C23 Mo1 74.01(14) . . ? C24 C23 H23 126.1 . . ? C22 C23 H23 126.1 . . ? Mo1 C23 H23 120.0 . . ? C25 C24 C23 108.6(2) . . ? C25 C24 Mo1 73.83(14) . . ? C23 C24 Mo1 72.97(14) . . ? C25 C24 H24 125.7 . . ? C23 C24 H24 125.7 . . ? Mo1 C24 H24 119.3 . . ? C24 C25 C26 107.6(3) . . ? C24 C25 Mo1 71.28(15) . . ? C26 C25 Mo1 73.25(14) . . ? C24 C25 H25 126.2 . . ? C26 C25 H25 126.2 . . ? Mo1 C25 H25 121.1 . . ? C25 C26 C22 108.6(2) . . ? C25 C26 Mo1 72.02(14) . . ? C22 C26 Mo1 72.96(15) . . ? C25 C26 H26 125.7 . . ? C22 C26 H26 125.7 . . ? Mo1 C26 H26 121.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.970 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.074 #========================================================================= data_bay03_compound6b _database_code_depnum_ccdc_archive 'CCDC 255257' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H38 As Fe O4 P Si2 W, C7 H14' _chemical_formula_sum 'C33 H52 As Fe O4 P Si2 W' _chemical_formula_weight 914.52 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' As As 0.0499 2.0058 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.53800(10) _cell_length_b 14.04200(10) _cell_length_c 14.3110(2) _cell_angle_alpha 100.3140(7) _cell_angle_beta 100.0740(7) _cell_angle_gamma 92.4090(8) _cell_volume 1851.33(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8465 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.641 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 4.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3439 _exptl_absorpt_correction_T_max 0.5699 _exptl_absorpt_process_details 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _exptl_special_details ; ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65197 _diffrn_reflns_av_R_equivalents 0.045 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8489 _reflns_number_gt 8006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD ' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+1.0174P] 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 8489 _refine_ls_number_parameters 400 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0199 _refine_ls_R_factor_gt 0.0177 _refine_ls_wR_factor_ref 0.0390 _refine_ls_wR_factor_gt 0.0384 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 W1 W 0.082638(7) 0.265007(5) 0.365130(5) 0.01284(3) Uani 1 1 d . . . As1 As 0.297550(19) 0.159589(13) 0.297742(14) 0.01420(4) Uani 1 1 d . . . Fe1 Fe 0.23753(3) -0.013511(19) 0.25643(2) 0.01354(6) Uani 1 1 d . . . P1 P 0.14199(5) 0.23134(3) 0.19988(4) 0.01440(10) Uani 1 1 d . . . Si1 Si 0.38038(5) 0.40672(4) 0.30101(4) 0.01486(11) Uani 1 1 d . . . Si2 Si 0.06509(6) 0.43484(4) 0.19774(4) 0.01574(11) Uani 1 1 d . . . O1 O 0.13492(16) -0.00337(11) 0.43812(11) 0.0242(3) Uani 1 1 d . . . O2 O -0.03232(15) 0.00704(11) 0.13357(12) 0.0264(3) Uani 1 1 d . . . O3 O 0.31273(15) 0.21466(11) 0.52884(11) 0.0264(3) Uani 1 1 d . . . O4 O 0.18015(15) 0.47370(10) 0.48226(11) 0.0234(3) Uani 1 1 d . . . C1 C 0.3525(2) -0.13353(14) 0.28501(14) 0.0160(4) Uani 1 1 d . . . C2 C 0.4510(2) -0.05159(14) 0.28884(15) 0.0163(4) Uani 1 1 d . . . C3 C 0.4272(2) -0.02508(14) 0.19583(15) 0.0167(4) Uani 1 1 d . . . C4 C 0.3128(2) -0.08829(14) 0.13562(14) 0.0175(4) Uani 1 1 d . . . C5 C 0.2671(2) -0.15624(14) 0.19035(15) 0.0165(4) Uani 1 1 d . . . C6 C 0.3467(2) -0.18846(15) 0.36515(15) 0.0207(4) Uani 1 1 d . . . H6A H 0.2496 -0.2177 0.3588 0.031 Uiso 1 1 calc R . . H6B H 0.3733 -0.1439 0.4275 0.031 Uiso 1 1 calc R . . H6C H 0.4134 -0.2396 0.3615 0.031 Uiso 1 1 calc R . . C7 C 0.5672(2) -0.00651(15) 0.37188(15) 0.0214(4) Uani 1 1 d . . . H7A H 0.6599 -0.0252 0.3572 0.032 Uiso 1 1 calc R . . H7B H 0.5517 -0.0292 0.4304 0.032 Uiso 1 1 calc R . . H7C H 0.5658 0.0643 0.3822 0.032 Uiso 1 1 calc R . . C8 C 0.5153(2) 0.05012(15) 0.16474(16) 0.0226(4) Uani 1 1 d . . . H8A H 0.5492 0.1033 0.2197 0.034 Uiso 1 1 calc R . . H8B H 0.4570 0.0755 0.1125 0.034 Uiso 1 1 calc R . . H8C H 0.5974 0.0208 0.1416 0.034 Uiso 1 1 calc R . . C9 C 0.2574(2) -0.09035(17) 0.03032(15) 0.0257(5) Uani 1 1 d . . . H9A H 0.3132 -0.1326 -0.0087 0.039 Uiso 1 1 calc R . . H9B H 0.2658 -0.0245 0.0170 0.039 Uiso 1 1 calc R . . H9C H 0.1568 -0.1153 0.0140 0.039 Uiso 1 1 calc R . . C10 C 0.1573(2) -0.24013(15) 0.15161(16) 0.0228(4) Uani 1 1 d . . . H10A H 0.0762 -0.2193 0.1099 0.034 Uiso 1 1 calc R . . H10B H 0.1244 -0.2629 0.2055 0.034 Uiso 1 1 calc R . . H10C H 0.1997 -0.2930 0.1141 0.034 Uiso 1 1 calc R . . C11 C 0.1749(2) -0.00504(14) 0.36646(15) 0.0181(4) Uani 1 1 d . . . C12 C 0.0745(2) 0.00164(14) 0.18365(15) 0.0182(4) Uani 1 1 d . . . C13 C 0.18705(19) 0.35460(13) 0.26230(14) 0.0131(4) Uani 1 1 d . . . C14 C 0.4883(2) 0.37598(15) 0.41261(15) 0.0202(4) Uani 1 1 d . . . H14A H 0.5807 0.4141 0.4286 0.030 Uiso 1 1 calc R . . H14B H 0.5039 0.3066 0.4012 0.030 Uiso 1 1 calc R . . H14C H 0.4369 0.3911 0.4664 0.030 Uiso 1 1 calc R . . C15 C 0.4799(2) 0.36885(16) 0.20026(16) 0.0230(4) Uani 1 1 d . . . H15A H 0.4270 0.3842 0.1403 0.034 Uiso 1 1 calc R . . H15B H 0.4901 0.2988 0.1917 0.034 Uiso 1 1 calc R . . H15C H 0.5748 0.4037 0.2160 0.034 Uiso 1 1 calc R . . C16 C 0.3914(2) 0.54355(14) 0.32636(15) 0.0210(4) Uani 1 1 d . . . H16A H 0.3472 0.5666 0.3823 0.032 Uiso 1 1 calc R . . H16B H 0.3410 0.5665 0.2698 0.032 Uiso 1 1 calc R . . H16C H 0.4918 0.5687 0.3402 0.032 Uiso 1 1 calc R . . C17 C 0.1499(2) 0.47406(15) 0.09996(15) 0.0223(4) Uani 1 1 d . . . H17A H 0.0936 0.5226 0.0724 0.033 Uiso 1 1 calc R . . H17B H 0.1530 0.4177 0.0491 0.033 Uiso 1 1 calc R . . H17C H 0.2473 0.5023 0.1275 0.033 Uiso 1 1 calc R . . C18 C 0.0225(2) 0.54415(15) 0.28130(16) 0.0238(5) Uani 1 1 d . . . H18A H 0.1114 0.5810 0.3163 0.036 Uiso 1 1 calc R . . H18B H -0.0311 0.5233 0.3276 0.036 Uiso 1 1 calc R . . H18C H -0.0352 0.5853 0.2437 0.036 Uiso 1 1 calc R . . C19 C -0.1125(2) 0.37376(16) 0.13046(16) 0.0234(5) Uani 1 1 d . . . H19A H -0.1725 0.3617 0.1768 0.035 Uiso 1 1 calc R . . H19B H -0.0977 0.3119 0.0906 0.035 Uiso 1 1 calc R . . H19C H -0.1599 0.4158 0.0889 0.035 Uiso 1 1 calc R . . C20 C 0.2334(2) 0.23175(15) 0.46311(15) 0.0186(4) Uani 1 1 d . . . C21 C 0.1486(2) 0.39698(15) 0.43603(15) 0.0173(4) Uani 1 1 d . . . C22 C -0.1538(2) 0.21174(15) 0.28421(16) 0.0216(4) Uani 1 1 d . . . H22 H -0.1803 0.2029 0.2159 0.026 Uiso 1 1 calc R . . C23 C -0.1567(2) 0.29933(15) 0.35148(16) 0.0215(4) Uani 1 1 d . . . H23 H -0.1854 0.3595 0.3361 0.026 Uiso 1 1 calc R . . C24 C -0.1089(2) 0.28053(15) 0.44571(16) 0.0214(4) Uani 1 1 d . . . H24 H -0.0995 0.3262 0.5045 0.026 Uiso 1 1 calc R . . C25 C -0.0777(2) 0.18193(15) 0.43687(16) 0.0211(4) Uani 1 1 d . . . H25 H -0.0448 0.1498 0.4887 0.025 Uiso 1 1 calc R . . C26 C -0.1042(2) 0.13991(15) 0.33770(16) 0.0204(4) Uani 1 1 d . . . H26 H -0.0911 0.0746 0.3112 0.024 Uiso 1 1 calc R . . C27 C 0.6699(2) 0.67121(16) 0.21684(17) 0.0263(5) Uani 1 1 d . . . H27A H 0.7161 0.6228 0.2520 0.032 Uiso 1 1 calc R . . H27B H 0.6069 0.7063 0.2570 0.032 Uiso 1 1 calc R . . C28 C 0.5805(2) 0.61910(17) 0.12110(18) 0.0303(5) Uani 1 1 d . . . H28A H 0.5052 0.5750 0.1337 0.036 Uiso 1 1 calc R . . H28B H 0.6420 0.5793 0.0832 0.036 Uiso 1 1 calc R . . C29 C 0.5113(2) 0.69152(18) 0.06263(18) 0.0319(5) Uani 1 1 d . . . H29A H 0.4591 0.6561 -0.0009 0.038 Uiso 1 1 calc R . . H29B H 0.4417 0.7263 0.0972 0.038 Uiso 1 1 calc R . . C30 C 0.6234(2) 0.76450(18) 0.04734(17) 0.0307(5) Uani 1 1 d . . . H30A H 0.5755 0.8137 0.0141 0.037 Uiso 1 1 calc R . . H30B H 0.6852 0.7307 0.0053 0.037 Uiso 1 1 calc R . . C31 C 0.7156(2) 0.81516(16) 0.14342(17) 0.0269(5) Uani 1 1 d . . . H31A H 0.7911 0.8588 0.1304 0.032 Uiso 1 1 calc R . . H31B H 0.6555 0.8555 0.1820 0.032 Uiso 1 1 calc R . . C32 C 0.7846(2) 0.74312(15) 0.20154(15) 0.0210(4) Uani 1 1 d . . . H32 H 0.8490 0.7058 0.1629 0.025 Uiso 1 1 calc R . . C33 C 0.8756(2) 0.79551(17) 0.29676(17) 0.0284(5) Uani 1 1 d . . . H33A H 0.9489 0.8397 0.2836 0.043 Uiso 1 1 calc R . . H33B H 0.9216 0.7478 0.3318 0.043 Uiso 1 1 calc R . . H33C H 0.8148 0.8327 0.3361 0.043 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 W1 0.01211(4) 0.01240(4) 0.01456(4) 0.00331(3) 0.00324(3) 0.00088(3) As1 0.01363(9) 0.01104(9) 0.01844(10) 0.00313(7) 0.00395(8) 0.00122(7) Fe1 0.01406(13) 0.01132(13) 0.01591(14) 0.00337(10) 0.00366(11) 0.00139(10) P1 0.0163(2) 0.0119(2) 0.0149(2) 0.00197(19) 0.00308(19) 0.00042(18) Si1 0.0140(2) 0.0145(3) 0.0157(3) 0.0025(2) 0.0028(2) -0.00077(19) Si2 0.0164(3) 0.0143(3) 0.0167(3) 0.0045(2) 0.0018(2) 0.0026(2) O1 0.0312(8) 0.0228(8) 0.0230(8) 0.0076(6) 0.0132(7) 0.0052(6) O2 0.0204(8) 0.0230(8) 0.0332(9) 0.0067(7) -0.0034(7) -0.0002(6) O3 0.0221(8) 0.0372(9) 0.0219(8) 0.0124(7) 0.0014(6) 0.0059(7) O4 0.0255(8) 0.0186(8) 0.0246(8) -0.0023(6) 0.0076(6) -0.0015(6) C1 0.0174(9) 0.0131(9) 0.0201(10) 0.0043(8) 0.0080(8) 0.0055(7) C2 0.0157(9) 0.0136(9) 0.0207(10) 0.0028(8) 0.0056(8) 0.0050(7) C3 0.0177(9) 0.0129(9) 0.0214(10) 0.0046(8) 0.0069(8) 0.0044(7) C4 0.0185(9) 0.0173(10) 0.0175(10) 0.0018(8) 0.0062(8) 0.0057(8) C5 0.0180(9) 0.0118(9) 0.0204(10) 0.0021(8) 0.0062(8) 0.0029(7) C6 0.0256(11) 0.0168(10) 0.0230(11) 0.0088(8) 0.0077(9) 0.0045(8) C7 0.0187(10) 0.0208(11) 0.0232(11) 0.0027(9) 0.0013(8) 0.0024(8) C8 0.0216(10) 0.0205(11) 0.0297(12) 0.0083(9) 0.0117(9) 0.0019(8) C9 0.0287(11) 0.0296(12) 0.0191(11) 0.0046(9) 0.0053(9) 0.0026(9) C10 0.0206(10) 0.0186(10) 0.0278(12) -0.0014(9) 0.0077(9) -0.0019(8) C11 0.0172(9) 0.0116(9) 0.0260(11) 0.0048(8) 0.0038(8) 0.0026(7) C12 0.0216(10) 0.0119(9) 0.0222(11) 0.0036(8) 0.0067(9) 0.0001(8) C13 0.0135(9) 0.0128(9) 0.0137(9) 0.0035(7) 0.0039(7) 0.0009(7) C14 0.0162(9) 0.0214(11) 0.0213(11) 0.0041(8) -0.0004(8) -0.0009(8) C15 0.0203(10) 0.0260(11) 0.0234(11) 0.0035(9) 0.0080(9) 0.0002(8) C16 0.0227(10) 0.0180(10) 0.0209(11) 0.0033(8) 0.0015(8) -0.0036(8) C17 0.0237(10) 0.0240(11) 0.0199(11) 0.0082(9) 0.0018(9) 0.0011(8) C18 0.0270(11) 0.0184(11) 0.0268(12) 0.0050(9) 0.0053(9) 0.0080(8) C19 0.0192(10) 0.0263(11) 0.0243(11) 0.0090(9) -0.0015(9) 0.0027(8) C20 0.0165(9) 0.0205(10) 0.0201(11) 0.0047(8) 0.0063(8) 0.0008(8) C21 0.0153(9) 0.0198(10) 0.0185(10) 0.0051(8) 0.0065(8) 0.0033(8) C22 0.0131(9) 0.0274(11) 0.0237(11) 0.0052(9) 0.0031(8) -0.0034(8) C23 0.0126(9) 0.0242(11) 0.0311(12) 0.0097(9) 0.0082(8) 0.0035(8) C24 0.0186(10) 0.0245(11) 0.0234(11) 0.0039(9) 0.0113(8) 0.0003(8) C25 0.0171(10) 0.0237(11) 0.0266(11) 0.0101(9) 0.0100(8) -0.0012(8) C26 0.0162(9) 0.0158(10) 0.0300(12) 0.0032(8) 0.0089(8) -0.0039(8) C27 0.0237(11) 0.0274(12) 0.0307(13) 0.0100(10) 0.0086(9) 0.0010(9) C28 0.0260(11) 0.0264(12) 0.0391(14) 0.0028(10) 0.0125(10) -0.0056(9) C29 0.0253(12) 0.0399(14) 0.0296(13) 0.0003(11) 0.0090(10) 0.0022(10) C30 0.0317(12) 0.0345(13) 0.0272(13) 0.0108(10) 0.0036(10) 0.0043(10) C31 0.0280(11) 0.0208(11) 0.0331(13) 0.0064(9) 0.0077(10) 0.0019(9) C32 0.0191(10) 0.0204(11) 0.0246(11) 0.0025(9) 0.0083(8) 0.0023(8) C33 0.0254(11) 0.0307(12) 0.0282(12) 0.0007(10) 0.0078(9) 0.0029(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C20 1.959(2) . ? W1 C21 1.966(2) . ? W1 C24 2.3230(19) . ? W1 C23 2.3351(19) . ? W1 C25 2.3630(19) . ? W1 C22 2.371(2) . ? W1 C26 2.3795(19) . ? W1 C13 2.4105(18) . ? W1 P1 2.4955(5) . ? W1 As1 2.7854(2) . ? As1 P1 2.2543(5) . ? As1 Fe1 2.4157(3) . ? Fe1 C12 1.758(2) . ? Fe1 C11 1.766(2) . ? Fe1 C5 2.1100(19) . ? Fe1 C4 2.1105(19) . ? Fe1 C1 2.1111(19) . ? Fe1 C2 2.1203(19) . ? Fe1 C3 2.1389(19) . ? P1 C13 1.7967(19) . ? Si1 C14 1.872(2) . ? Si1 C15 1.874(2) . ? Si1 C16 1.885(2) . ? Si1 C13 1.9044(19) . ? Si2 C18 1.875(2) . ? Si2 C19 1.883(2) . ? Si2 C17 1.884(2) . ? Si2 C13 1.8930(19) . ? O1 C11 1.152(2) . ? O2 C12 1.152(2) . ? O3 C20 1.167(2) . ? O4 C21 1.156(2) . ? C1 C5 1.428(3) . ? C1 C2 1.441(3) . ? C1 C6 1.500(3) . ? C2 C3 1.429(3) . ? C2 C7 1.501(3) . ? C3 C4 1.427(3) . ? C3 C8 1.498(3) . ? C4 C5 1.437(3) . ? C4 C9 1.502(3) . ? C5 C10 1.500(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C22 C26 1.420(3) . ? C22 C23 1.424(3) . ? C22 H22 0.9500 . ? C23 C24 1.421(3) . ? C23 H23 0.9500 . ? C24 C25 1.416(3) . ? C24 H24 0.9500 . ? C25 C26 1.410(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.523(3) . ? C27 C32 1.528(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.529(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.520(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.531(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.521(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.525(3) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 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 C20 W1 C21 81.45(8) . . ? C20 W1 C24 102.19(8) . . ? C21 W1 C24 85.78(8) . . ? C20 W1 C23 137.70(8) . . ? C21 W1 C23 92.15(8) . . ? C24 W1 C23 35.52(7) . . ? C20 W1 C25 86.02(8) . . ? C21 W1 C25 114.18(8) . . ? C24 W1 C25 35.18(7) . . ? C23 W1 C25 58.57(7) . . ? C20 W1 C22 140.44(8) . . ? C21 W1 C22 125.96(8) . . ? C24 W1 C22 58.60(7) . . ? C23 W1 C22 35.22(7) . . ? C25 W1 C22 58.04(7) . . ? C20 W1 C26 105.91(8) . . ? C21 W1 C26 143.93(7) . . ? C24 W1 C26 58.18(7) . . ? C23 W1 C26 58.28(7) . . ? C25 W1 C26 34.59(7) . . ? C22 W1 C26 34.79(7) . . ? C20 W1 C13 109.67(7) . . ? C21 W1 C13 70.28(7) . . ? C24 W1 C13 136.01(7) . . ? C23 W1 C13 107.17(7) . . ? C25 W1 C13 164.31(7) . . ? C22 W1 C13 106.75(7) . . ? C26 W1 C13 134.28(7) . . ? C20 W1 P1 112.43(6) . . ? C21 W1 P1 113.05(6) . . ? C24 W1 P1 142.29(6) . . ? C23 W1 P1 108.54(6) . . ? C25 W1 P1 131.23(5) . . ? C22 W1 P1 84.61(5) . . ? C26 W1 P1 96.96(5) . . ? C13 W1 P1 42.92(5) . . ? C20 W1 As1 63.36(6) . . ? C21 W1 As1 113.93(5) . . ? C24 W1 As1 151.58(5) . . ? C23 W1 As1 150.70(5) . . ? C25 W1 As1 116.62(5) . . ? C22 W1 As1 115.82(5) . . ? C26 W1 As1 100.45(5) . . ? C13 W1 As1 72.00(4) . . ? P1 W1 As1 50.171(12) . . ? P1 As1 Fe1 108.139(16) . . ? P1 As1 W1 58.224(13) . . ? Fe1 As1 W1 113.728(9) . . ? C12 Fe1 C11 97.24(9) . . ? C12 Fe1 C5 98.63(8) . . ? C11 Fe1 C5 114.39(8) . . ? C12 Fe1 C4 91.29(9) . . ? C11 Fe1 C4 154.06(8) . . ? C5 Fe1 C4 39.82(8) . . ? C12 Fe1 C1 135.13(8) . . ? C11 Fe1 C1 90.80(8) . . ? C5 Fe1 C1 39.54(8) . . ? C4 Fe1 C1 66.39(8) . . ? C12 Fe1 C2 157.24(9) . . ? C11 Fe1 C2 104.60(8) . . ? C5 Fe1 C2 66.64(7) . . ? C4 Fe1 C2 66.20(8) . . ? C1 Fe1 C2 39.82(7) . . ? C12 Fe1 C3 119.93(9) . . ? C11 Fe1 C3 142.66(8) . . ? C5 Fe1 C3 66.32(7) . . ? C4 Fe1 C3 39.25(7) . . ? C1 Fe1 C3 66.14(7) . . ? C2 Fe1 C3 39.19(8) . . ? C12 Fe1 As1 91.88(6) . . ? C11 Fe1 As1 88.08(6) . . ? C5 Fe1 As1 153.48(5) . . ? C4 Fe1 As1 116.18(6) . . ? C1 Fe1 As1 132.61(5) . . ? C2 Fe1 As1 95.12(5) . . ? C3 Fe1 As1 87.32(5) . . ? C13 P1 As1 97.87(6) . . ? C13 P1 W1 66.02(6) . . ? As1 P1 W1 71.604(15) . . ? C14 Si1 C15 106.91(10) . . ? C14 Si1 C16 103.75(9) . . ? C15 Si1 C16 106.83(10) . . ? C14 Si1 C13 118.24(9) . . ? C15 Si1 C13 109.48(9) . . ? C16 Si1 C13 110.95(9) . . ? C18 Si2 C19 105.61(10) . . ? C18 Si2 C17 109.89(10) . . ? C19 Si2 C17 103.47(10) . . ? C18 Si2 C13 112.91(9) . . ? C19 Si2 C13 115.16(9) . . ? C17 Si2 C13 109.32(9) . . ? C5 C1 C2 108.18(17) . . ? C5 C1 C6 126.07(18) . . ? C2 C1 C6 125.68(18) . . ? C5 C1 Fe1 70.19(11) . . ? C2 C1 Fe1 70.43(10) . . ? C6 C1 Fe1 127.47(13) . . ? C3 C2 C1 107.83(17) . . ? C3 C2 C7 125.06(18) . . ? C1 C2 C7 126.91(18) . . ? C3 C2 Fe1 71.11(11) . . ? C1 C2 Fe1 69.74(10) . . ? C7 C2 Fe1 128.67(14) . . ? C4 C3 C2 108.00(17) . . ? C4 C3 C8 126.02(19) . . ? C2 C3 C8 125.78(18) . . ? C4 C3 Fe1 69.30(11) . . ? C2 C3 Fe1 69.70(11) . . ? C8 C3 Fe1 130.47(14) . . ? C3 C4 C5 108.44(17) . . ? C3 C4 C9 126.29(18) . . ? C5 C4 C9 125.05(18) . . ? C3 C4 Fe1 71.45(11) . . ? C5 C4 Fe1 70.07(11) . . ? C9 C4 Fe1 128.45(14) . . ? C1 C5 C4 107.53(17) . . ? C1 C5 C10 126.74(18) . . ? C4 C5 C10 125.57(18) . . ? C1 C5 Fe1 70.27(11) . . ? C4 C5 Fe1 70.11(11) . . ? C10 C5 Fe1 128.54(14) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 Fe1 177.27(17) . . ? O2 C12 Fe1 176.68(18) . . ? P1 C13 Si2 107.92(10) . . ? P1 C13 Si1 121.51(10) . . ? Si2 C13 Si1 113.95(9) . . ? P1 C13 W1 71.06(6) . . ? Si2 C13 W1 115.99(8) . . ? Si1 C13 W1 119.50(9) . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si1 C16 H16A 109.5 . . ? Si1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? Si1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si2 C17 H17A 109.5 . . ? Si2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? Si2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si2 C18 H18A 109.5 . . ? Si2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? Si2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si2 C19 H19A 109.5 . . ? Si2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O3 C20 W1 172.24(17) . . ? O4 C21 W1 174.81(17) . . ? C26 C22 C23 107.64(19) . . ? C26 C22 W1 72.93(11) . . ? C23 C22 W1 71.01(11) . . ? C26 C22 H22 126.2 . . ? C23 C22 H22 126.2 . . ? W1 C22 H22 121.6 . . ? C24 C23 C22 107.70(18) . . ? C24 C23 W1 71.77(11) . . ? C22 C23 W1 73.76(11) . . ? C24 C23 H23 126.2 . . ? C22 C23 H23 126.2 . . ? W1 C23 H23 120.1 . . ? C25 C24 C23 108.21(19) . . ? C25 C24 W1 73.96(11) . . ? C23 C24 W1 72.71(11) . . ? C25 C24 H24 125.9 . . ? C23 C24 H24 125.9 . . ? W1 C24 H24 119.3 . . ? C26 C25 C24 107.99(19) . . ? C26 C25 W1 73.34(11) . . ? C24 C25 W1 70.87(11) . . ? C26 C25 H25 126.0 . . ? C24 C25 H25 126.0 . . ? W1 C25 H25 121.5 . . ? C25 C26 C22 108.46(18) . . ? C25 C26 W1 72.06(11) . . ? C22 C26 W1 72.28(11) . . ? C25 C26 H26 125.8 . . ? C22 C26 H26 125.8 . . ? W1 C26 H26 121.6 . . ? C28 C27 C32 111.52(18) . . ? C28 C27 H27A 109.3 . . ? C32 C27 H27A 109.3 . . ? C28 C27 H27B 109.3 . . ? C32 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? C27 C28 C29 111.09(19) . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C30 C29 C28 110.86(19) . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29B 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C29 C30 C31 111.43(19) . . ? C29 C30 H30A 109.3 . . ? C31 C30 H30A 109.3 . . ? C29 C30 H30B 109.3 . . ? C31 C30 H30B 109.3 . . ? H30A C30 H30B 108.0 . . ? C32 C31 C30 112.13(18) . . ? C32 C31 H31A 109.2 . . ? C30 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? C30 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? C31 C32 C33 111.00(18) . . ? C31 C32 C27 109.82(17) . . ? C33 C32 C27 112.15(18) . . ? C31 C32 H32 107.9 . . ? C33 C32 H32 107.9 . . ? C27 C32 H32 107.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.510 _refine_diff_density_min -0.891 _refine_diff_density_rms 0.079