# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- RIvard_merged_Nov2011.cif' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name E.Rivard _publ_contact_author_address ; Department of Chemistry University of Alberta Edmonton Alberta T6E 2G2 CANADA ; _publ_contact_author_email ERIVARD@UALBERTA.CA _publ_section_title ; Efficient generation of stable adducts of Si(II) dihydride ; loop_ _publ_author_name 'SM Ibrahim Al-Rafia' 'Adam C. Malcolm' 'Robert McDonald' 'Michael J. Ferguson' E.Rivard data_riv1174 _database_code_depnum_ccdc_archive 'CCDC 853340' #TrackingRef '- RIvard_merged_Nov2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 2 _chemical_melting_point ? _chemical_formula_moiety 'C27 H41 B N2 Si' _chemical_formula_sum 'C27 H41 B N2 Si' _chemical_formula_weight 432.52 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2366(7) _cell_length_b 13.7989(8) _cell_length_c 17.9086(11) _cell_angle_alpha 90.00 _cell_angle_beta 97.2660(10) _cell_angle_gamma 90.00 _cell_volume 2754.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6903 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 22.41 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.043 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 0.100 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9584 _exptl_absorpt_correction_T_max 0.9918 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21777 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5649 _reflns_number_gt 4146 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXD (Schneider & Sheldrick, 2002)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0483P)^2^+0.8772P] 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 5649 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1161 _refine_ls_wR_factor_gt 0.1028 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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 Si Si 0.52361(4) 0.62660(3) 0.19025(3) 0.03517(13) Uani 1 1 d . . . H1A H 0.5639(16) 0.5737(13) 0.1310(10) 0.048(5) Uiso 1 1 d . . . H1B H 0.6325(17) 0.6391(13) 0.2409(10) 0.054(5) Uiso 1 1 d . . . N1 N 0.48435(11) 0.50109(8) 0.31838(7) 0.0273(3) Uani 1 1 d . . . N2 N 0.35711(11) 0.47066(9) 0.22124(7) 0.0290(3) Uani 1 1 d . . . C1 C 0.45516(13) 0.52477(10) 0.24502(8) 0.0273(3) Uani 1 1 d . . . C2 C 0.40384(14) 0.43388(11) 0.34014(9) 0.0319(4) Uani 1 1 d . . . H2 H 0.4044 0.4068 0.3889 0.038 Uiso 1 1 calc R . . C3 C 0.32489(15) 0.41421(11) 0.27930(9) 0.0332(4) Uani 1 1 d . . . H3 H 0.2596 0.3701 0.2766 0.040 Uiso 1 1 calc R . . C11 C 0.59190(14) 0.53059(11) 0.36650(9) 0.0318(4) Uani 1 1 d . . . C12 C 0.69148(15) 0.46916(13) 0.36955(10) 0.0417(4) Uani 1 1 d . . . C13 C 0.79244(18) 0.49679(16) 0.41765(13) 0.0594(6) Uani 1 1 d . . . H13 H 0.8627 0.4579 0.4210 0.071 Uiso 1 1 calc R . . C14 C 0.79267(19) 0.57958(18) 0.46063(13) 0.0649(6) Uani 1 1 d . . . H14 H 0.8622 0.5959 0.4941 0.078 Uiso 1 1 calc R . . C15 C 0.69344(19) 0.63898(15) 0.45566(11) 0.0538(5) Uani 1 1 d . . . H15 H 0.6958 0.6962 0.4853 0.065 Uiso 1 1 calc R . . C16 C 0.58939(16) 0.61621(12) 0.40755(9) 0.0375(4) Uani 1 1 d . . . C17 C 0.69252(17) 0.37857(14) 0.32096(11) 0.0483(5) Uani 1 1 d . . . H17 H 0.6077 0.3650 0.2994 0.058 Uiso 1 1 calc R . . C18 C 0.7638(2) 0.39547(18) 0.25541(12) 0.0662(6) Uani 1 1 d . . . H18A H 0.7336 0.4536 0.2277 0.079 Uiso 1 1 calc R . . H18B H 0.7550 0.3393 0.2217 0.079 Uiso 1 1 calc R . . H18C H 0.8487 0.4044 0.2746 0.079 Uiso 1 1 calc R . . C19 C 0.7392(2) 0.28930(15) 0.36560(13) 0.0644(6) Uani 1 1 d . . . H19A H 0.6932 0.2798 0.4080 0.077 Uiso 1 1 calc R . . H19B H 0.8241 0.2985 0.3847 0.077 Uiso 1 1 calc R . . H19C H 0.7303 0.2322 0.3328 0.077 Uiso 1 1 calc R . . C20 C 0.47949(18) 0.68049(12) 0.40119(10) 0.0430(4) Uani 1 1 d . . . H20 H 0.4255 0.6604 0.3551 0.052 Uiso 1 1 calc R . . C21 C 0.4118(2) 0.66539(19) 0.46826(13) 0.0728(7) Uani 1 1 d . . . H21A H 0.3413 0.7079 0.4637 0.087 Uiso 1 1 calc R . . H21B H 0.4643 0.6809 0.5147 0.087 Uiso 1 1 calc R . . H21C H 0.3859 0.5977 0.4698 0.087 Uiso 1 1 calc R . . C22 C 0.5095(3) 0.78720(14) 0.39263(14) 0.0761(7) Uani 1 1 d . . . H22A H 0.4352 0.8251 0.3854 0.091 Uiso 1 1 calc R . . H22B H 0.5529 0.7956 0.3489 0.091 Uiso 1 1 calc R . . H22C H 0.5598 0.8096 0.4381 0.091 Uiso 1 1 calc R . . C31 C 0.30105(15) 0.46728(11) 0.14365(9) 0.0325(4) Uani 1 1 d . . . C32 C 0.19762(15) 0.52255(11) 0.12345(9) 0.0360(4) Uani 1 1 d . . . C33 C 0.14916(17) 0.51942(13) 0.04787(10) 0.0450(4) Uani 1 1 d . . . H33 H 0.0793 0.5562 0.0315 0.054 Uiso 1 1 calc R . . C34 C 0.20049(18) 0.46414(14) -0.00342(10) 0.0496(5) Uani 1 1 d . . . H34 H 0.1661 0.4639 -0.0547 0.059 Uiso 1 1 calc R . . C35 C 0.30099(18) 0.40916(14) 0.01845(10) 0.0466(5) Uani 1 1 d . . . H35 H 0.3342 0.3707 -0.0177 0.056 Uiso 1 1 calc R . . C36 C 0.35490(16) 0.40920(12) 0.09335(9) 0.0378(4) Uani 1 1 d . . . C37 C 0.13836(16) 0.58068(12) 0.18078(10) 0.0408(4) Uani 1 1 d . . . H37 H 0.2019 0.5996 0.2224 0.049 Uiso 1 1 calc R . . C38 C 0.07864(18) 0.67346(13) 0.14755(13) 0.0545(5) Uani 1 1 d . . . H38A H 0.1390 0.7147 0.1283 0.065 Uiso 1 1 calc R . . H38B H 0.0426 0.7084 0.1867 0.065 Uiso 1 1 calc R . . H38C H 0.0161 0.6568 0.1063 0.065 Uiso 1 1 calc R . . C39 C 0.04486(18) 0.51969(14) 0.21470(11) 0.0503(5) Uani 1 1 d . . . H39A H 0.0117 0.5573 0.2536 0.060 Uiso 1 1 calc R . . H39B H 0.0828 0.4608 0.2371 0.060 Uiso 1 1 calc R . . H39C H -0.0198 0.5019 0.1751 0.060 Uiso 1 1 calc R . . C40 C 0.46390(18) 0.34605(14) 0.11688(10) 0.0474(5) Uani 1 1 d . . . H40 H 0.5035 0.3709 0.1663 0.057 Uiso 1 1 calc R . . C41 C 0.5563(2) 0.34936(18) 0.06156(14) 0.0703(7) Uani 1 1 d . . . H41A H 0.6238 0.3068 0.0794 0.084 Uiso 1 1 calc R . . H41B H 0.5854 0.4159 0.0578 0.084 Uiso 1 1 calc R . . H41C H 0.5193 0.3274 0.0120 0.084 Uiso 1 1 calc R . . C42 C 0.4258(2) 0.24169(16) 0.12866(15) 0.0742(7) Uani 1 1 d . . . H42A H 0.3676 0.2403 0.1650 0.089 Uiso 1 1 calc R . . H42B H 0.4963 0.2031 0.1479 0.089 Uiso 1 1 calc R . . H42C H 0.3891 0.2146 0.0806 0.089 Uiso 1 1 calc R . . B B 0.4120(2) 0.73832(15) 0.16952(16) 0.0469(5) Uani 1 1 d . . . H2A H 0.344(2) 0.7206(16) 0.1201(13) 0.078(7) Uiso 1 1 d . . . H2B H 0.458(2) 0.7961(18) 0.1522(13) 0.088(8) Uiso 1 1 d . . . H2C H 0.373(2) 0.7484(17) 0.2175(14) 0.083(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si 0.0393(3) 0.0308(2) 0.0370(3) 0.00723(19) 0.0110(2) -0.00185(19) N1 0.0300(7) 0.0241(6) 0.0285(7) 0.0015(5) 0.0062(5) 0.0012(5) N2 0.0329(7) 0.0244(6) 0.0299(7) 0.0020(5) 0.0045(6) -0.0002(5) C1 0.0300(8) 0.0238(7) 0.0291(8) -0.0006(6) 0.0070(6) 0.0027(6) C2 0.0363(9) 0.0274(8) 0.0332(8) 0.0076(6) 0.0087(7) -0.0010(7) C3 0.0363(9) 0.0260(8) 0.0380(9) 0.0064(6) 0.0073(7) -0.0028(7) C11 0.0307(8) 0.0338(8) 0.0307(8) 0.0054(7) 0.0038(7) -0.0033(7) C12 0.0331(9) 0.0430(10) 0.0494(10) 0.0085(8) 0.0071(8) -0.0001(8) C13 0.0332(10) 0.0653(14) 0.0769(15) 0.0105(11) -0.0036(10) -0.0003(9) C14 0.0446(12) 0.0745(16) 0.0702(15) 0.0069(12) -0.0139(11) -0.0180(11) C15 0.0623(13) 0.0481(11) 0.0482(11) -0.0026(9) -0.0040(10) -0.0160(10) C16 0.0465(10) 0.0347(9) 0.0310(8) 0.0028(7) 0.0039(7) -0.0070(7) C17 0.0367(10) 0.0461(11) 0.0640(13) 0.0037(9) 0.0141(9) 0.0115(8) C18 0.0696(15) 0.0716(15) 0.0606(13) 0.0154(11) 0.0210(11) 0.0176(12) C19 0.0732(15) 0.0524(12) 0.0745(15) 0.0118(11) 0.0364(12) 0.0228(11) C20 0.0614(12) 0.0341(9) 0.0331(9) -0.0023(7) 0.0047(8) 0.0066(8) C21 0.0711(16) 0.0911(18) 0.0593(14) 0.0158(12) 0.0209(12) 0.0298(14) C22 0.113(2) 0.0350(11) 0.0808(17) -0.0044(11) 0.0143(15) 0.0070(12) C31 0.0393(9) 0.0270(8) 0.0305(8) 0.0019(6) 0.0012(7) -0.0062(7) C32 0.0399(9) 0.0246(8) 0.0417(9) 0.0045(7) -0.0013(7) -0.0072(7) C33 0.0485(11) 0.0378(9) 0.0449(10) 0.0086(8) -0.0090(8) -0.0076(8) C34 0.0603(13) 0.0539(12) 0.0317(9) 0.0059(8) -0.0053(9) -0.0169(10) C35 0.0586(12) 0.0482(11) 0.0336(9) -0.0034(8) 0.0085(9) -0.0131(9) C36 0.0456(10) 0.0343(9) 0.0338(9) -0.0006(7) 0.0064(8) -0.0058(8) C37 0.0402(10) 0.0288(8) 0.0505(11) -0.0015(7) -0.0050(8) 0.0010(7) C38 0.0486(11) 0.0319(9) 0.0802(15) 0.0036(9) -0.0036(10) 0.0035(8) C39 0.0529(12) 0.0405(10) 0.0582(12) -0.0006(9) 0.0101(9) 0.0035(9) C40 0.0551(12) 0.0473(11) 0.0408(10) -0.0076(8) 0.0095(9) 0.0069(9) C41 0.0739(16) 0.0656(14) 0.0773(16) -0.0027(12) 0.0327(13) 0.0176(12) C42 0.0869(18) 0.0529(13) 0.0837(17) 0.0178(12) 0.0141(14) 0.0158(12) B 0.0407(12) 0.0272(10) 0.0732(16) 0.0117(10) 0.0087(12) 0.0003(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 Si C1 1.9284(15) . ? Si B 1.992(2) . ? Si H1A 1.409(18) . ? Si H1B 1.439(18) . ? N1 C1 1.3534(19) . ? N1 C2 1.3855(19) . ? N1 C11 1.4510(19) . ? N2 C1 1.3543(19) . ? N2 C3 1.3836(19) . ? N2 C31 1.4520(19) . ? C2 C3 1.343(2) . ? C11 C16 1.394(2) . ? C11 C12 1.399(2) . ? C12 C13 1.388(3) . ? C12 C17 1.524(3) . ? C13 C14 1.377(3) . ? C14 C15 1.378(3) . ? C15 C16 1.398(3) . ? C16 C20 1.513(2) . ? C17 C18 1.520(3) . ? C17 C19 1.525(3) . ? C20 C21 1.515(3) . ? C20 C22 1.523(3) . ? C31 C32 1.399(2) . ? C31 C36 1.399(2) . ? C32 C33 1.394(2) . ? C32 C37 1.521(2) . ? C33 C34 1.376(3) . ? C34 C35 1.376(3) . ? C35 C36 1.400(2) . ? C36 C40 1.519(3) . ? C37 C39 1.530(2) . ? C37 C38 1.531(2) . ? C40 C41 1.524(3) . ? C40 C42 1.525(3) . ? B H2A 1.12(2) . ? B H2B 1.02(3) . ? B H2C 1.02(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si B 112.11(8) . . ? C1 Si H1A 101.1(7) . . ? B Si H1A 121.0(7) . . ? C1 Si H1B 97.4(7) . . ? B Si H1B 119.3(7) . . ? H1A Si H1B 102.0(10) . . ? C1 N1 C2 110.36(13) . . ? C1 N1 C11 126.18(12) . . ? C2 N1 C11 123.04(12) . . ? C1 N2 C3 110.73(13) . . ? C1 N2 C31 123.76(12) . . ? C3 N2 C31 125.32(13) . . ? N1 C1 N2 105.06(12) . . ? N1 C1 Si 127.33(11) . . ? N2 C1 Si 127.07(11) . . ? C3 C2 N1 107.16(13) . . ? C2 C3 N2 106.69(14) . . ? C16 C11 C12 124.22(16) . . ? C16 C11 N1 118.70(14) . . ? C12 C11 N1 117.07(14) . . ? C13 C12 C11 116.40(18) . . ? C13 C12 C17 120.98(17) . . ? C11 C12 C17 122.58(16) . . ? C14 C13 C12 121.2(2) . . ? C13 C14 C15 120.88(19) . . ? C14 C15 C16 120.88(19) . . ? C11 C16 C15 116.40(17) . . ? C11 C16 C20 121.87(15) . . ? C15 C16 C20 121.72(16) . . ? C18 C17 C12 110.97(17) . . ? C18 C17 C19 110.42(16) . . ? C12 C17 C19 112.97(17) . . ? C16 C20 C21 110.29(15) . . ? C16 C20 C22 112.66(18) . . ? C21 C20 C22 110.66(18) . . ? C32 C31 C36 123.96(15) . . ? C32 C31 N2 118.41(14) . . ? C36 C31 N2 117.63(14) . . ? C33 C32 C31 116.35(16) . . ? C33 C32 C37 121.40(16) . . ? C31 C32 C37 122.23(15) . . ? C34 C33 C32 121.34(18) . . ? C35 C34 C33 120.93(17) . . ? C34 C35 C36 120.84(18) . . ? C31 C36 C35 116.55(16) . . ? C31 C36 C40 123.31(15) . . ? C35 C36 C40 120.11(16) . . ? C32 C37 C39 111.04(14) . . ? C32 C37 C38 112.74(15) . . ? C39 C37 C38 108.97(15) . . ? C36 C40 C41 113.23(16) . . ? C36 C40 C42 110.47(17) . . ? C41 C40 C42 110.15(18) . . ? Si B H2A 109.2(12) . . ? Si B H2B 109.5(14) . . ? H2A B H2B 104.5(17) . . ? Si B H2C 106.0(13) . . ? H2A B H2C 111.6(17) . . ? H2B B H2C 115.9(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 N2 -0.90(16) . . . . ? C11 N1 C1 N2 171.75(13) . . . . ? C2 N1 C1 Si 171.06(11) . . . . ? C11 N1 C1 Si -16.3(2) . . . . ? C3 N2 C1 N1 0.40(16) . . . . ? C31 N2 C1 N1 -174.79(13) . . . . ? C3 N2 C1 Si -171.59(11) . . . . ? C31 N2 C1 Si 13.2(2) . . . . ? B Si C1 N1 -106.49(15) . . . . ? B Si C1 N2 63.77(16) . . . . ? C1 N1 C2 C3 1.08(17) . . . . ? C11 N1 C2 C3 -171.84(13) . . . . ? N1 C2 C3 N2 -0.78(17) . . . . ? C1 N2 C3 C2 0.25(17) . . . . ? C31 N2 C3 C2 175.34(14) . . . . ? C1 N1 C11 C16 90.43(19) . . . . ? C2 N1 C11 C16 -97.81(17) . . . . ? C1 N1 C11 C12 -90.79(18) . . . . ? C2 N1 C11 C12 80.97(19) . . . . ? C16 C11 C12 C13 0.7(3) . . . . ? N1 C11 C12 C13 -178.03(15) . . . . ? C16 C11 C12 C17 -177.05(16) . . . . ? N1 C11 C12 C17 4.2(2) . . . . ? C11 C12 C13 C14 1.0(3) . . . . ? C17 C12 C13 C14 178.77(19) . . . . ? C12 C13 C14 C15 -1.7(3) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C12 C11 C16 C15 -1.6(2) . . . . ? N1 C11 C16 C15 177.11(14) . . . . ? C12 C11 C16 C20 179.19(15) . . . . ? N1 C11 C16 C20 -2.1(2) . . . . ? C14 C15 C16 C11 0.8(3) . . . . ? C14 C15 C16 C20 -179.94(18) . . . . ? C13 C12 C17 C18 -74.3(2) . . . . ? C11 C12 C17 C18 103.3(2) . . . . ? C13 C12 C17 C19 50.3(2) . . . . ? C11 C12 C17 C19 -132.08(18) . . . . ? C11 C16 C20 C21 101.9(2) . . . . ? C15 C16 C20 C21 -77.3(2) . . . . ? C11 C16 C20 C22 -133.93(18) . . . . ? C15 C16 C20 C22 46.9(2) . . . . ? C1 N2 C31 C32 -100.44(18) . . . . ? C3 N2 C31 C32 85.08(18) . . . . ? C1 N2 C31 C36 79.01(18) . . . . ? C3 N2 C31 C36 -95.47(19) . . . . ? C36 C31 C32 C33 -1.4(2) . . . . ? N2 C31 C32 C33 178.03(14) . . . . ? C36 C31 C32 C37 176.80(15) . . . . ? N2 C31 C32 C37 -3.8(2) . . . . ? C31 C32 C33 C34 0.5(2) . . . . ? C37 C32 C33 C34 -177.71(16) . . . . ? C32 C33 C34 C35 0.7(3) . . . . ? C33 C34 C35 C36 -1.0(3) . . . . ? C32 C31 C36 C35 1.1(2) . . . . ? N2 C31 C36 C35 -178.37(14) . . . . ? C32 C31 C36 C40 -177.11(16) . . . . ? N2 C31 C36 C40 3.5(2) . . . . ? C34 C35 C36 C31 0.2(3) . . . . ? C34 C35 C36 C40 178.42(16) . . . . ? C33 C32 C37 C39 88.41(19) . . . . ? C31 C32 C37 C39 -89.69(19) . . . . ? C33 C32 C37 C38 -34.2(2) . . . . ? C31 C32 C37 C38 147.70(16) . . . . ? C31 C36 C40 C41 -137.98(18) . . . . ? C35 C36 C40 C41 43.9(2) . . . . ? C31 C36 C40 C42 97.9(2) . . . . ? C35 C36 C40 C42 -80.2(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.296 _refine_diff_density_min -0.258 _refine_diff_density_rms 0.035 #===END data_riv11a6 _database_code_depnum_ccdc_archive 'CCDC 853341' #TrackingRef '- RIvard_merged_Nov2011.cif' _vrf_PLAT213_riv11a6 ; RESPONSE: The shapes of some of the thermal ellipsoids in one of the 2,6-diisopropylphenyl groups suggest disorder. Attempts to break this group into two discrete sets of positions proved unsuccessful, requiring a large number of geometric restraints and shared thermal parameters, and resulting in no worthwhile improvement of the model. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 3 _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 N2 O5 Si W, 0.5(C6 H14)' _chemical_formula_sum 'C35 H45 N2 O5 Si W' _chemical_formula_weight 785.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.2434(15) _cell_length_b 18.594(2) _cell_length_c 27.175(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7196.9(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9403 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 23.53 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3176 _exptl_absorpt_coefficient_mu 3.284 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.5201 _exptl_absorpt_correction_T_max 0.6901 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 50262 _diffrn_reflns_av_R_equivalents 0.1106 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6703 _reflns_number_gt 4839 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0781P)^2^+163.3664P] 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 6703 _refine_ls_number_parameters 413 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1119 _refine_ls_R_factor_gt 0.0850 _refine_ls_wR_factor_ref 0.2254 _refine_ls_wR_factor_gt 0.2093 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.161 _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 W W -0.08831(4) -0.09280(3) 0.31101(2) 0.0324(2) Uani 1 1 d . . . Si Si -0.0356(2) 0.00671(19) 0.37075(13) 0.0296(8) Uani 1 1 d D . . H1 H -0.029(9) -0.001(7) 0.419(3) 0.03(2) Uiso 1 1 d D . . H2 H -0.096(8) 0.060(6) 0.378(5) 0.03(2) Uiso 1 1 d D . . O1 O -0.1680(8) -0.2085(6) 0.2384(4) 0.054(3) Uani 1 1 d . . . O2 O -0.1777(7) 0.0314(6) 0.2448(4) 0.049(3) Uani 1 1 d . . . O3 O 0.1165(7) -0.0943(6) 0.2635(4) 0.054(3) Uani 1 1 d . . . O4 O -0.0230(9) -0.2148(7) 0.3849(4) 0.065(3) Uani 1 1 d . . . O5 O -0.2794(8) -0.0897(7) 0.3714(4) 0.060(3) Uani 1 1 d . . . N1 N 0.1577(7) 0.0624(6) 0.3817(4) 0.028(2) Uani 1 1 d . . . N2 N 0.0860(7) 0.1145(6) 0.3215(4) 0.028(2) Uani 1 1 d . . . C1 C -0.1366(11) -0.1655(8) 0.2650(5) 0.042(3) Uani 1 1 d . . . C2 C -0.1417(11) -0.0133(8) 0.2677(5) 0.041(3) Uani 1 1 d . . . C3 C 0.0425(11) -0.0928(8) 0.2788(6) 0.043(3) Uani 1 1 d . . . C4 C -0.0478(11) -0.1696(8) 0.3578(5) 0.042(3) Uani 1 1 d . . . C5 C -0.2096(11) -0.0907(8) 0.3489(5) 0.042(3) Uani 1 1 d . . . C6 C 0.0729(8) 0.0655(7) 0.3573(4) 0.028(3) Uani 1 1 d . . . C7 C 0.2194(9) 0.1108(7) 0.3604(5) 0.033(3) Uani 1 1 d . . . H7 H 0.2821 0.1196 0.3707 0.040 Uiso 1 1 calc R . . C8 C 0.1760(9) 0.1432(7) 0.3228(5) 0.037(3) Uani 1 1 d . . . H8 H 0.2015 0.1785 0.3014 0.045 Uiso 1 1 calc R . . C11 C 0.1760(8) 0.0287(7) 0.4286(5) 0.031(3) Uani 1 1 d . . . C12 C 0.2118(9) -0.0426(8) 0.4283(5) 0.035(3) Uani 1 1 d . . . C13 C 0.2322(10) -0.0712(8) 0.4739(6) 0.044(4) Uani 1 1 d . . . H13 H 0.2575 -0.1184 0.4755 0.053 Uiso 1 1 calc R . . C14 C 0.2177(11) -0.0349(9) 0.5166(6) 0.048(4) Uani 1 1 d . . . H14 H 0.2314 -0.0570 0.5472 0.058 Uiso 1 1 calc R . . C15 C 0.1823(11) 0.0352(9) 0.5151(5) 0.047(4) Uani 1 1 d . . . H15 H 0.1734 0.0610 0.5449 0.057 Uiso 1 1 calc R . . C16 C 0.1602(10) 0.0672(8) 0.4709(5) 0.038(3) Uani 1 1 d . . . C17 C 0.2314(10) -0.0817(8) 0.3815(5) 0.041(3) Uani 1 1 d . . . H17 H 0.1861 -0.0640 0.3561 0.050 Uiso 1 1 calc R . . C18 C 0.2204(12) -0.1635(8) 0.3853(7) 0.061(5) Uani 1 1 d . . . H18A H 0.1563 -0.1750 0.3958 0.073 Uiso 1 1 calc R . . H18B H 0.2652 -0.1823 0.4094 0.073 Uiso 1 1 calc R . . H18C H 0.2325 -0.1854 0.3531 0.073 Uiso 1 1 calc R . . C19 C 0.3335(12) -0.0646(9) 0.3627(7) 0.059(5) Uani 1 1 d . . . H19A H 0.3447 -0.0898 0.3316 0.070 Uiso 1 1 calc R . . H19B H 0.3793 -0.0808 0.3873 0.070 Uiso 1 1 calc R . . H19C H 0.3401 -0.0127 0.3577 0.070 Uiso 1 1 calc R . . C20 C 0.1190(10) 0.1428(8) 0.4707(6) 0.042(3) Uani 1 1 d . . . H20 H 0.1159 0.1598 0.4359 0.051 Uiso 1 1 calc R . . C21 C 0.0187(11) 0.1413(9) 0.4915(6) 0.053(4) Uani 1 1 d . . . H21A H -0.0182 0.1048 0.4740 0.064 Uiso 1 1 calc R . . H21B H -0.0105 0.1886 0.4870 0.064 Uiso 1 1 calc R . . H21C H 0.0207 0.1295 0.5266 0.064 Uiso 1 1 calc R . . C22 C 0.1770(14) 0.1962(10) 0.4999(8) 0.072(6) Uani 1 1 d . . . H22A H 0.2415 0.1966 0.4873 0.087 Uiso 1 1 calc R . . H22B H 0.1774 0.1822 0.5347 0.087 Uiso 1 1 calc R . . H22C H 0.1497 0.2443 0.4966 0.087 Uiso 1 1 calc R . . C31 C 0.0162(8) 0.1432(7) 0.2881(5) 0.032(3) Uani 1 1 d . . . C32 C 0.0211(8) 0.1309(6) 0.2390(5) 0.030(3) Uani 1 1 d . . . C33 C -0.0412(10) 0.1671(8) 0.2077(6) 0.043(4) Uani 1 1 d . . . H33 H -0.0397 0.1582 0.1733 0.052 Uiso 1 1 calc R . . C34 C -0.1053(9) 0.2162(9) 0.2269(6) 0.048(4) Uani 1 1 d . . . H34 H -0.1473 0.2403 0.2054 0.058 Uiso 1 1 calc R . . C35 C -0.1087(8) 0.2305(7) 0.2772(6) 0.041(4) Uani 1 1 d . . . H35 H -0.1514 0.2656 0.2892 0.049 Uiso 1 1 calc R . . C36 C -0.0517(9) 0.1949(6) 0.3096(5) 0.032(3) Uani 1 1 d . . . C37 C 0.0923(10) 0.0793(10) 0.2166(5) 0.051(5) Uani 1 1 d . . . H37 H 0.1243 0.0530 0.2440 0.061 Uiso 1 1 calc R . . C38 C 0.0582(13) 0.0289(7) 0.1833(5) 0.055(5) Uani 1 1 d . . . H38A H 0.0121 -0.0021 0.1997 0.066 Uiso 1 1 calc R . . H38B H 0.1103 -0.0006 0.1710 0.066 Uiso 1 1 calc R . . H38C H 0.0282 0.0537 0.1556 0.066 Uiso 1 1 calc R . . C39 C 0.1681(10) 0.1227(10) 0.1875(6) 0.054(4) Uani 1 1 d . . . H39A H 0.2132 0.0893 0.1727 0.064 Uiso 1 1 calc R . . H39B H 0.2011 0.1552 0.2100 0.064 Uiso 1 1 calc R . . H39C H 0.1376 0.1509 0.1615 0.064 Uiso 1 1 calc R . . C40 C -0.0490(9) 0.2134(7) 0.3624(6) 0.038(3) Uani 1 1 d . . . H40 H -0.0151 0.1746 0.3806 0.045 Uiso 1 1 calc R . . C41 C -0.1490(10) 0.2224(10) 0.3848(6) 0.054(4) Uani 1 1 d . . . H41A H -0.1438 0.2385 0.4190 0.065 Uiso 1 1 calc R . . H41B H -0.1821 0.1762 0.3837 0.065 Uiso 1 1 calc R . . H41C H -0.1842 0.2581 0.3657 0.065 Uiso 1 1 calc R . . C42 C 0.0038(13) 0.2853(9) 0.3697(7) 0.065(5) Uani 1 1 d . . . H42A H 0.0073 0.2965 0.4048 0.078 Uiso 1 1 calc R . . H42B H -0.0299 0.3238 0.3525 0.078 Uiso 1 1 calc R . . H42C H 0.0674 0.2811 0.3562 0.078 Uiso 1 1 calc R . . C1SA C 0.496(3) 0.0253(16) 0.4782(9) 0.110(15) Uani 0.60 1 d PD . 1 H1SA H 0.5558 0.0274 0.4601 0.132 Uiso 0.60 1 calc PR . 1 H1SB H 0.4465 0.0077 0.4554 0.132 Uiso 0.60 1 calc PR . 1 C2SA C 0.470(4) 0.100(2) 0.497(2) 0.135(17) Uani 0.60 1 d PD A 1 H2SA H 0.4121 0.0981 0.5173 0.162 Uiso 0.60 1 calc PR A 1 H2SB H 0.5214 0.1208 0.5166 0.162 Uiso 0.60 1 calc PR A 1 C3SA C 0.454(7) 0.141(3) 0.4496(19) 0.12(2) Uani 0.60 1 d PD A 1 H3SA H 0.4376 0.1910 0.4574 0.148 Uiso 0.60 1 calc PR A 1 H3SB H 0.4025 0.1188 0.4311 0.148 Uiso 0.60 1 calc PR A 1 H3SC H 0.5114 0.1401 0.4298 0.148 Uiso 0.60 1 calc PR A 1 C1SB C 0.499(6) 0.0395(12) 0.507(3) 0.110(15) Uani 0.40 1 d PD . 2 H1SC H 0.4708 0.0458 0.5401 0.132 Uiso 0.40 1 calc PR . 2 H1SD H 0.5632 0.0598 0.5074 0.132 Uiso 0.40 1 calc PR . 2 C2SB C 0.439(6) 0.076(4) 0.468(3) 0.135(17) Uani 0.40 1 d PD B 2 H2SC H 0.4630 0.0629 0.4350 0.162 Uiso 0.40 1 calc PR B 2 H2SD H 0.3737 0.0589 0.4708 0.162 Uiso 0.40 1 calc PR B 2 C3SB C 0.441(12) 0.157(4) 0.474(4) 0.12(2) Uani 0.40 1 d PD B 2 H3SD H 0.4041 0.1795 0.4477 0.148 Uiso 0.40 1 calc PR B 2 H3SE H 0.5065 0.1742 0.4717 0.148 Uiso 0.40 1 calc PR B 2 H3SF H 0.4151 0.1705 0.5059 0.148 Uiso 0.40 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.0287(3) 0.0257(3) 0.0427(3) -0.0023(2) -0.0030(2) -0.0037(2) Si 0.0263(18) 0.0254(18) 0.0370(19) -0.0009(15) 0.0000(15) -0.0061(14) O1 0.061(7) 0.038(6) 0.061(7) -0.015(5) 0.000(6) -0.004(5) O2 0.037(6) 0.047(6) 0.064(7) 0.009(6) -0.003(5) 0.009(5) O3 0.032(6) 0.058(7) 0.072(8) 0.007(6) 0.012(5) 0.006(5) O4 0.081(9) 0.056(7) 0.057(7) 0.013(6) -0.004(6) 0.011(7) O5 0.035(6) 0.075(8) 0.072(8) 0.011(7) 0.006(5) -0.008(6) N1 0.020(5) 0.028(5) 0.035(6) 0.000(5) -0.001(4) -0.001(4) N2 0.015(5) 0.027(5) 0.043(6) 0.001(4) -0.005(4) -0.001(4) C1 0.043(9) 0.038(8) 0.043(8) -0.001(7) 0.000(7) 0.002(7) C2 0.048(9) 0.037(8) 0.037(8) -0.006(6) 0.006(7) -0.005(7) C3 0.052(10) 0.027(7) 0.050(9) -0.006(7) -0.012(7) 0.003(7) C4 0.048(9) 0.038(8) 0.041(8) -0.003(7) 0.000(7) -0.002(7) C5 0.046(9) 0.035(7) 0.044(8) 0.005(7) -0.007(7) -0.020(7) C6 0.018(6) 0.035(7) 0.032(6) -0.003(5) -0.001(5) 0.006(5) C7 0.020(6) 0.034(7) 0.045(8) -0.001(6) 0.004(6) -0.004(5) C8 0.019(6) 0.035(7) 0.058(9) 0.015(6) 0.000(6) -0.004(5) C11 0.017(6) 0.046(8) 0.031(7) 0.003(6) 0.001(5) -0.008(5) C12 0.020(6) 0.041(8) 0.045(8) 0.005(6) -0.002(6) -0.001(6) C13 0.031(8) 0.048(9) 0.055(9) 0.010(7) -0.001(7) 0.003(6) C14 0.043(9) 0.060(10) 0.042(8) 0.017(8) -0.003(7) -0.003(8) C15 0.044(9) 0.066(11) 0.032(7) 0.003(7) 0.001(6) -0.011(8) C16 0.029(7) 0.050(8) 0.037(7) -0.003(6) -0.002(6) -0.011(6) C17 0.036(8) 0.048(9) 0.040(7) -0.001(7) -0.008(6) 0.004(7) C18 0.046(10) 0.042(9) 0.094(13) -0.017(9) -0.006(9) -0.006(8) C19 0.058(11) 0.046(9) 0.072(11) -0.008(9) 0.024(9) 0.003(8) C20 0.038(8) 0.038(8) 0.051(9) -0.008(7) 0.004(7) 0.005(6) C21 0.040(9) 0.048(9) 0.071(11) -0.019(8) 0.002(8) -0.002(7) C22 0.065(12) 0.058(11) 0.094(15) -0.028(10) -0.005(11) -0.014(10) C31 0.016(6) 0.028(7) 0.050(8) 0.010(6) -0.004(5) -0.004(5) C32 0.017(6) 0.023(6) 0.050(8) 0.006(6) -0.009(5) -0.006(5) C33 0.039(8) 0.045(9) 0.045(8) 0.014(7) -0.011(7) -0.017(7) C34 0.020(7) 0.054(10) 0.070(11) 0.029(8) -0.009(7) -0.001(6) C35 0.017(6) 0.023(7) 0.082(11) 0.021(7) 0.011(6) 0.013(5) C36 0.025(6) 0.016(6) 0.054(8) 0.008(6) 0.001(6) 0.017(5) C37 0.024(7) 0.100(14) 0.029(7) 0.020(8) -0.002(6) 0.001(8) C38 0.097(13) 0.022(7) 0.045(9) 0.011(6) 0.024(9) 0.040(8) C39 0.025(7) 0.064(10) 0.072(11) 0.002(9) 0.007(7) -0.009(7) C40 0.019(6) 0.015(6) 0.079(11) 0.003(6) 0.001(6) 0.007(5) C41 0.031(8) 0.062(11) 0.070(11) -0.003(9) 0.011(7) 0.002(7) C42 0.056(11) 0.044(10) 0.095(14) -0.015(10) 0.013(10) -0.007(8) C1SA 0.08(2) 0.10(3) 0.14(5) -0.05(3) -0.05(3) -0.01(3) C2SA 0.14(4) 0.11(4) 0.16(5) -0.04(3) -0.03(3) -0.02(3) C3SA 0.15(4) 0.09(4) 0.13(6) -0.01(3) -0.01(6) -0.03(3) C1SB 0.08(2) 0.10(3) 0.14(5) -0.05(3) -0.05(3) -0.01(3) C2SB 0.14(4) 0.11(4) 0.16(5) -0.04(3) -0.03(3) -0.02(3) C3SB 0.15(4) 0.09(4) 0.13(6) -0.01(3) -0.01(6) -0.03(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W C1 1.966(15) . ? W C4 1.997(16) . ? W C5 2.011(16) . ? W C2 2.037(16) . ? W C3 2.059(17) . ? W Si 2.573(4) . ? Si C6 1.928(13) . ? Si H1 1.32(9) . ? Si H2 1.32(9) . ? O1 C1 1.167(17) . ? O2 C2 1.157(17) . ? O3 C3 1.134(18) . ? O4 C4 1.173(18) . ? O5 C5 1.167(18) . ? N1 C6 1.380(15) . ? N1 C7 1.386(16) . ? N1 C11 1.442(16) . ? N2 C6 1.344(16) . ? N2 C8 1.389(15) . ? N2 C31 1.449(16) . ? C7 C8 1.337(19) . ? C11 C16 1.374(19) . ? C11 C12 1.420(19) . ? C12 C13 1.379(19) . ? C12 C17 1.493(19) . ? C13 C14 1.36(2) . ? C14 C15 1.40(2) . ? C15 C16 1.38(2) . ? C16 C20 1.52(2) . ? C17 C18 1.53(2) . ? C17 C19 1.57(2) . ? C20 C22 1.52(2) . ? C20 C21 1.54(2) . ? C31 C32 1.355(19) . ? C31 C36 1.484(17) . ? C32 C33 1.402(18) . ? C32 C37 1.52(2) . ? C33 C34 1.39(2) . ? C34 C35 1.39(2) . ? C35 C36 1.369(18) . ? C36 C40 1.47(2) . ? C37 C38 1.39(2) . ? C37 C39 1.56(2) . ? C40 C42 1.55(2) . ? C40 C41 1.558(18) . ? C1SA C2SA 1.518(10) . ? C1SA C1SA 1.518(10) 5_656 ? C2SA C3SA 1.518(10) . ? C1SB C2SB 1.520(10) . ? C1SB C1SB 1.520(10) 5_656 ? C2SB C3SB 1.519(10) . ? 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 C1 W C4 90.8(6) . . ? C1 W C5 92.2(6) . . ? C4 W C5 86.3(6) . . ? C1 W C2 90.0(6) . . ? C4 W C2 174.1(6) . . ? C5 W C2 87.8(6) . . ? C1 W C3 92.6(6) . . ? C4 W C3 90.6(6) . . ? C5 W C3 174.3(5) . . ? C2 W C3 95.3(6) . . ? C1 W Si 176.2(4) . . ? C4 W Si 91.6(4) . . ? C5 W Si 85.0(4) . . ? C2 W Si 87.2(4) . . ? C3 W Si 90.3(4) . . ? C6 Si W 121.4(4) . . ? C6 Si H1 101(6) . . ? W Si H1 125(6) . . ? C6 Si H2 97(6) . . ? W Si H2 116(6) . . ? H1 Si H2 88(8) . . ? C6 N1 C7 109.1(10) . . ? C6 N1 C11 126.9(10) . . ? C7 N1 C11 122.5(10) . . ? C6 N2 C8 111.8(10) . . ? C6 N2 C31 127.3(10) . . ? C8 N2 C31 120.5(10) . . ? O1 C1 W 177.8(13) . . ? O2 C2 W 175.3(13) . . ? O3 C3 W 176.0(13) . . ? O4 C4 W 179.1(15) . . ? O5 C5 W 179.2(13) . . ? N2 C6 N1 104.7(10) . . ? N2 C6 Si 129.3(9) . . ? N1 C6 Si 125.9(9) . . ? C8 C7 N1 108.5(11) . . ? C7 C8 N2 105.9(11) . . ? C16 C11 C12 123.2(13) . . ? C16 C11 N1 119.0(12) . . ? C12 C11 N1 117.8(11) . . ? C13 C12 C11 115.6(13) . . ? C13 C12 C17 122.6(13) . . ? C11 C12 C17 121.7(12) . . ? C14 C13 C12 122.8(15) . . ? C13 C14 C15 119.7(14) . . ? C16 C15 C14 120.7(15) . . ? C11 C16 C15 117.9(14) . . ? C11 C16 C20 122.7(13) . . ? C15 C16 C20 119.4(14) . . ? C12 C17 C18 114.0(13) . . ? C12 C17 C19 110.5(12) . . ? C18 C17 C19 108.5(13) . . ? C22 C20 C16 113.1(13) . . ? C22 C20 C21 109.1(13) . . ? C16 C20 C21 109.9(12) . . ? C32 C31 N2 121.2(12) . . ? C32 C31 C36 122.1(12) . . ? N2 C31 C36 116.1(12) . . ? C31 C32 C33 118.9(13) . . ? C31 C32 C37 122.4(11) . . ? C33 C32 C37 118.7(13) . . ? C34 C33 C32 120.2(14) . . ? C33 C34 C35 121.1(13) . . ? C36 C35 C34 121.2(13) . . ? C35 C36 C40 122.0(12) . . ? C35 C36 C31 116.5(13) . . ? C40 C36 C31 121.1(11) . . ? C38 C37 C32 117.0(12) . . ? C38 C37 C39 105.1(13) . . ? C32 C37 C39 109.7(14) . . ? C36 C40 C42 109.8(13) . . ? C36 C40 C41 112.3(12) . . ? C42 C40 C41 107.6(12) . . ? C2SA C1SA C1SA 109(4) . 5_656 ? C3SA C2SA C1SA 102(4) . . ? C2SB C1SB C1SB 105(6) . 5_656 ? C3SB C2SB C1SB 111(7) . . ? 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 C1 W Si C6 -121(7) . . . . ? C4 W Si C6 109.2(6) . . . . ? C5 W Si C6 -164.6(6) . . . . ? C2 W Si C6 -76.7(6) . . . . ? C3 W Si C6 18.6(6) . . . . ? C4 W C1 O1 92(36) . . . . ? C5 W C1 O1 6(36) . . . . ? C2 W C1 O1 -82(36) . . . . ? C3 W C1 O1 -178(100) . . . . ? Si W C1 O1 -38(41) . . . . ? C1 W C2 O2 89(16) . . . . ? C4 W C2 O2 -10(19) . . . . ? C5 W C2 O2 -4(16) . . . . ? C3 W C2 O2 -179(100) . . . . ? Si W C2 O2 -89(16) . . . . ? C1 W C3 O3 -116(19) . . . . ? C4 W C3 O3 -25(19) . . . . ? C5 W C3 O3 32(23) . . . . ? C2 W C3 O3 154(19) . . . . ? Si W C3 O3 67(19) . . . . ? C1 W C4 O4 79(98) . . . . ? C5 W C4 O4 171(100) . . . . ? C2 W C4 O4 177(100) . . . . ? C3 W C4 O4 -14(98) . . . . ? Si W C4 O4 -104(98) . . . . ? C1 W C5 O5 121(98) . . . . ? C4 W C5 O5 30(98) . . . . ? C2 W C5 O5 -149(98) . . . . ? C3 W C5 O5 -27(100) . . . . ? Si W C5 O5 -62(98) . . . . ? C8 N2 C6 N1 -0.7(14) . . . . ? C31 N2 C6 N1 -173.6(12) . . . . ? C8 N2 C6 Si -177.2(10) . . . . ? C31 N2 C6 Si 9.9(19) . . . . ? C7 N1 C6 N2 1.1(13) . . . . ? C11 N1 C6 N2 167.1(11) . . . . ? C7 N1 C6 Si 177.7(9) . . . . ? C11 N1 C6 Si -16.2(18) . . . . ? W Si C6 N2 67.0(12) . . . . ? W Si C6 N1 -108.8(10) . . . . ? C6 N1 C7 C8 -1.1(15) . . . . ? C11 N1 C7 C8 -167.9(12) . . . . ? N1 C7 C8 N2 0.6(15) . . . . ? C6 N2 C8 C7 0.1(16) . . . . ? C31 N2 C8 C7 173.5(12) . . . . ? C6 N1 C11 C16 -85.7(16) . . . . ? C7 N1 C11 C16 78.6(15) . . . . ? C6 N1 C11 C12 95.9(15) . . . . ? C7 N1 C11 C12 -99.8(14) . . . . ? C16 C11 C12 C13 -1.2(19) . . . . ? N1 C11 C12 C13 177.2(11) . . . . ? C16 C11 C12 C17 -177.6(12) . . . . ? N1 C11 C12 C17 0.7(18) . . . . ? C11 C12 C13 C14 1(2) . . . . ? C17 C12 C13 C14 177.6(14) . . . . ? C12 C13 C14 C15 -1(2) . . . . ? C13 C14 C15 C16 1(2) . . . . ? C12 C11 C16 C15 1(2) . . . . ? N1 C11 C16 C15 -177.0(12) . . . . ? C12 C11 C16 C20 -178.1(12) . . . . ? N1 C11 C16 C20 3.5(19) . . . . ? C14 C15 C16 C11 -1(2) . . . . ? C14 C15 C16 C20 178.1(13) . . . . ? C13 C12 C17 C18 33.6(19) . . . . ? C11 C12 C17 C18 -150.3(13) . . . . ? C13 C12 C17 C19 -89.0(17) . . . . ? C11 C12 C17 C19 87.2(15) . . . . ? C11 C16 C20 C22 -128.2(16) . . . . ? C15 C16 C20 C22 52.3(19) . . . . ? C11 C16 C20 C21 109.6(15) . . . . ? C15 C16 C20 C21 -69.8(17) . . . . ? C6 N2 C31 C32 -115.2(15) . . . . ? C8 N2 C31 C32 72.5(17) . . . . ? C6 N2 C31 C36 73.4(16) . . . . ? C8 N2 C31 C36 -98.8(14) . . . . ? N2 C31 C32 C33 -172.1(11) . . . . ? C36 C31 C32 C33 -1.3(18) . . . . ? N2 C31 C32 C37 7.7(19) . . . . ? C36 C31 C32 C37 178.5(12) . . . . ? C31 C32 C33 C34 1.6(19) . . . . ? C37 C32 C33 C34 -178.2(13) . . . . ? C32 C33 C34 C35 0(2) . . . . ? C33 C34 C35 C36 -2(2) . . . . ? C34 C35 C36 C40 175.0(13) . . . . ? C34 C35 C36 C31 3(2) . . . . ? C32 C31 C36 C35 -0.8(19) . . . . ? N2 C31 C36 C35 170.5(11) . . . . ? C32 C31 C36 C40 -173.2(12) . . . . ? N2 C31 C36 C40 -1.9(17) . . . . ? C31 C32 C37 C38 131.0(14) . . . . ? C33 C32 C37 C38 -49.2(19) . . . . ? C31 C32 C37 C39 -109.6(14) . . . . ? C33 C32 C37 C39 70.2(16) . . . . ? C35 C36 C40 C42 -73.5(17) . . . . ? C31 C36 C40 C42 98.5(14) . . . . ? C35 C36 C40 C41 46.2(17) . . . . ? C31 C36 C40 C41 -141.9(13) . . . . ? C1SA C1SA C2SA C3SA -174(6) 5_656 . . . ? C1SB C1SB C2SB C3SB -173(11) 5_656 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 4.579 _refine_diff_density_min -4.960 _refine_diff_density_rms 0.222 #===END data_riv11c4 _database_code_depnum_ccdc_archive 'CCDC 853342' #TrackingRef '- RIvard_merged_Nov2011.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4 _chemical_melting_point ? _chemical_formula_moiety 'C56 H72 Cl4 N4 O2 Rh Si2, C2 Cl2 O2 Rh, 3(C H2 Cl2)' _chemical_formula_sum 'C61 H78 Cl12 N4 O4 Rh2 Si2' _chemical_formula_weight 1618.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 '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/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 13.2122(2) _cell_length_b 21.2410(3) _cell_length_c 13.2241(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.4269(6) _cell_angle_gamma 90.00 _cell_volume 3680.08(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9846 _cell_measurement_theta_min 3.37 _cell_measurement_theta_max 69.61 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1652 _exptl_absorpt_coefficient_mu 8.308 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2682 _exptl_absorpt_correction_T_max 0.3979 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24802 _diffrn_reflns_av_R_equivalents 0.0170 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 70.04 _reflns_number_total 6813 _reflns_number_gt 6390 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0712P)^2^+5.0144P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6813 _refine_ls_number_parameters 446 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0476 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.079 _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 Rh1 Rh 0.5000 0.0000 0.5000 0.03395(12) Uani 1 2 d S . . Cl1 Cl 0.41266(7) 0.16423(4) 0.45045(6) 0.0462(2) Uani 1 1 d . . . Cl2 Cl 0.24675(7) 0.07369(4) 0.54077(6) 0.0487(2) Uani 1 1 d . . . Si Si 0.36529(6) 0.07091(4) 0.44973(6) 0.03331(19) Uani 1 1 d . . . O1 O 0.3620(2) -0.07953(16) 0.6134(3) 0.0736(9) Uani 1 1 d . . . N1 N 0.2385(2) 0.00939(12) 0.28347(19) 0.0330(5) Uani 1 1 d . . . N2 N 0.2290(2) 0.10930(12) 0.2591(2) 0.0383(6) Uani 1 1 d . . . C1 C 0.4133(3) -0.05016(17) 0.5712(3) 0.0461(8) Uani 1 1 d . . . C2 C 0.2770(2) 0.06482(14) 0.3210(2) 0.0323(6) Uani 1 1 d . . . C3 C 0.1666(2) 0.01941(16) 0.1995(2) 0.0401(7) Uani 1 1 d . . . H3 H 0.1284 -0.0119 0.1599 0.048 Uiso 1 1 calc R . . C4 C 0.1612(3) 0.08176(16) 0.1845(3) 0.0427(7) Uani 1 1 d . . . H4 H 0.1185 0.1030 0.1320 0.051 Uiso 1 1 calc R . . C11 C 0.2710(3) -0.05307(15) 0.3181(2) 0.0379(7) Uani 1 1 d . . . C12 C 0.3618(3) -0.07620(18) 0.2874(3) 0.0468(8) Uani 1 1 d . . . C13 C 0.3898(4) -0.1367(2) 0.3205(3) 0.0668(12) Uani 1 1 d . . . H13 H 0.4515 -0.1542 0.3034 0.080 Uiso 1 1 calc R . . C14 C 0.3306(4) -0.1715(2) 0.3768(3) 0.0722(14) Uani 1 1 d . . . H14 H 0.3525 -0.2125 0.3989 0.087 Uiso 1 1 calc R . . C15 C 0.2409(4) -0.14881(18) 0.4019(3) 0.0610(11) Uani 1 1 d . . . H15 H 0.2003 -0.1746 0.4393 0.073 Uiso 1 1 calc R . . C16 C 0.2073(3) -0.08782(16) 0.3734(3) 0.0451(8) Uani 1 1 d . . . C17 C 0.4228(3) -0.0393(2) 0.2178(3) 0.0562(10) Uani 1 1 d . . . H17 H 0.4200 0.0061 0.2374 0.067 Uiso 1 1 calc R . . C18 C 0.5349(3) -0.0580(3) 0.2259(4) 0.0800(16) Uani 1 1 d . . . H18A H 0.5692 -0.0320 0.1794 0.096 Uiso 1 1 calc R . . H18B H 0.5401 -0.1025 0.2075 0.096 Uiso 1 1 calc R . . H18C H 0.5674 -0.0515 0.2960 0.096 Uiso 1 1 calc R . . C19 C 0.3751(4) -0.0449(3) 0.1060(3) 0.0771(14) Uani 1 1 d . . . H19A H 0.4167 -0.0215 0.0626 0.093 Uiso 1 1 calc R . . H19B H 0.3058 -0.0274 0.0982 0.093 Uiso 1 1 calc R . . H19C H 0.3722 -0.0893 0.0859 0.093 Uiso 1 1 calc R . . C20 C 0.1060(3) -0.06428(19) 0.3997(3) 0.0540(9) Uani 1 1 d . . . H20 H 0.1013 -0.0182 0.3842 0.065 Uiso 1 1 calc R . . C21 C 0.0954(4) -0.0731(2) 0.5132(3) 0.0651(11) Uani 1 1 d . . . H21A H 0.0285 -0.0577 0.5266 0.078 Uiso 1 1 calc R . . H21B H 0.1492 -0.0493 0.5547 0.078 Uiso 1 1 calc R . . H21C H 0.1018 -0.1179 0.5308 0.078 Uiso 1 1 calc R . . C22 C 0.0179(4) -0.0973(3) 0.3335(4) 0.0820(15) Uani 1 1 d . . . H22A H -0.0473 -0.0817 0.3513 0.098 Uiso 1 1 calc R . . H22B H 0.0224 -0.1428 0.3454 0.098 Uiso 1 1 calc R . . H22C H 0.0222 -0.0886 0.2614 0.098 Uiso 1 1 calc R . . C31 C 0.2485(3) 0.17687(16) 0.2564(2) 0.0431(8) Uani 1 1 d . . . C32 C 0.3255(3) 0.19655(19) 0.1985(3) 0.0521(9) Uani 1 1 d . . . C33 C 0.3384(4) 0.2621(2) 0.1933(3) 0.0660(13) Uani 1 1 d . . . H33 H 0.3895 0.2784 0.1561 0.079 Uiso 1 1 calc R . . C34 C 0.2789(4) 0.3037(2) 0.2406(3) 0.0655(12) Uani 1 1 d . . . H34 H 0.2896 0.3477 0.2355 0.079 Uiso 1 1 calc R . . C35 C 0.2053(3) 0.28188(17) 0.2943(3) 0.0576(10) Uani 1 1 d . . . H35 H 0.1652 0.3112 0.3262 0.069 Uiso 1 1 calc R . . C36 C 0.1867(3) 0.21738(15) 0.3039(3) 0.0455(8) Uani 1 1 d . . . C37 C 0.3873(4) 0.1519(2) 0.1433(3) 0.0649(11) Uani 1 1 d . . . H37 H 0.3731 0.1084 0.1669 0.078 Uiso 1 1 calc R . . C38 C 0.5001(5) 0.1629(4) 0.1685(5) 0.116(3) Uani 1 1 d . . . H38A H 0.5373 0.1320 0.1324 0.140 Uiso 1 1 calc R . . H38B H 0.5198 0.1585 0.2421 0.140 Uiso 1 1 calc R . . H38C H 0.5167 0.2055 0.1472 0.140 Uiso 1 1 calc R . . C39 C 0.3522(5) 0.1543(3) 0.0306(4) 0.0940(18) Uani 1 1 d . . . H39A H 0.3924 0.1246 -0.0046 0.113 Uiso 1 1 calc R . . H39B H 0.3616 0.1970 0.0053 0.113 Uiso 1 1 calc R . . H39C H 0.2798 0.1429 0.0177 0.113 Uiso 1 1 calc R . . C40 C 0.1008(3) 0.19471(17) 0.3596(3) 0.0526(9) Uani 1 1 d . . . H40 H 0.1102 0.1485 0.3717 0.063 Uiso 1 1 calc R . . C41 C 0.1012(4) 0.2266(2) 0.4631(4) 0.0705(12) Uani 1 1 d . . . H41A H 0.0446 0.2103 0.4965 0.085 Uiso 1 1 calc R . . H41B H 0.0934 0.2721 0.4534 0.085 Uiso 1 1 calc R . . H41C H 0.1660 0.2178 0.5057 0.085 Uiso 1 1 calc R . . C42 C -0.0012(4) 0.2044(3) 0.2920(5) 0.0837(15) Uani 1 1 d . . . H42A H 0.0003 0.1826 0.2268 0.100 Uiso 1 1 calc R . . H42B H -0.0125 0.2495 0.2795 0.100 Uiso 1 1 calc R . . H42C H -0.0566 0.1873 0.3263 0.100 Uiso 1 1 calc R . . Rh2 Rh -0.11440(5) 0.46906(4) 0.58742(5) 0.0571(2) Uani 0.50 1 d P A -1 Cl3 Cl -0.02817(19) 0.40648(11) 0.47876(16) 0.0641(5) Uani 0.50 1 d P A -1 Cl4 Cl -0.02493(17) 0.56111(11) 0.54939(14) 0.0592(5) Uani 0.50 1 d P A -1 O50 O -0.2310(7) 0.3613(7) 0.6441(8) 0.131(4) Uani 0.50 1 d P A -1 O60 O -0.2244(6) 0.5512(5) 0.7176(6) 0.111(3) Uani 0.50 1 d P A -1 C50 C -0.1861(8) 0.4017(5) 0.6223(8) 0.077(3) Uani 0.50 1 d P A -1 C60 C -0.1822(9) 0.5179(7) 0.6727(8) 0.081(3) Uani 0.50 1 d P A -1 Cl1S Cl -0.2250(3) 0.54442(19) 0.6136(4) 0.1221(13) Uani 0.50 1 d PD B -2 Cl2S Cl -0.1489(10) 0.4403(4) 0.7294(5) 0.297(6) Uani 0.50 1 d PD B -2 C1S C -0.1401(12) 0.4829(6) 0.6221(11) 0.134(8) Uani 0.50 1 d PD B -2 H1SA H -0.1549 0.4555 0.5614 0.161 Uiso 0.50 1 calc PR B -2 H1SB H -0.0698 0.4994 0.6236 0.161 Uiso 0.50 1 calc PR B -2 Cl3S Cl -0.1997(8) 0.2947(3) 0.4056(4) 0.1238(15) Uani 0.50 1 d PD C 1 Cl4S Cl -0.4087(3) 0.2736(2) 0.3992(3) 0.1183(13) Uani 0.50 1 d PD C 1 C2S C -0.3004(9) 0.2472(12) 0.350(2) 0.183(3) Uani 0.50 1 d PD C 1 H2SA H -0.3091 0.2515 0.2748 0.220 Uiso 0.50 1 calc PR C 1 H2SB H -0.2870 0.2024 0.3677 0.220 Uiso 0.50 1 calc PR C 1 Cl5S Cl -0.2687(6) 0.2384(3) 0.3585(6) 0.183(3) Uani 0.50 1 d PD D 2 Cl6S Cl -0.1854(5) 0.3187(3) 0.5240(5) 0.175(2) Uani 0.50 1 d PD D 2 C3S C -0.202(4) 0.3085(13) 0.3915(10) 0.1238(15) Uani 0.50 1 d PD D 2 H3SA H -0.1342 0.3069 0.3667 0.149 Uiso 0.50 1 calc PR D 2 H3SB H -0.2401 0.3447 0.3585 0.149 Uiso 0.50 1 calc PR D 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0353(2) 0.03572(19) 0.03027(18) 0.00185(11) 0.00203(12) 0.00331(12) Cl1 0.0545(5) 0.0353(4) 0.0445(4) -0.0031(3) -0.0094(3) 0.0003(3) Cl2 0.0480(5) 0.0628(5) 0.0366(4) -0.0009(3) 0.0106(3) 0.0114(4) Si 0.0362(4) 0.0349(4) 0.0278(4) -0.0010(3) 0.0002(3) 0.0030(3) O1 0.0575(18) 0.079(2) 0.087(2) 0.0383(18) 0.0188(16) -0.0006(15) N1 0.0316(14) 0.0370(13) 0.0298(12) -0.0016(10) 0.0016(10) -0.0002(10) N2 0.0399(15) 0.0379(14) 0.0353(13) 0.0069(10) -0.0026(10) -0.0046(11) C1 0.0432(19) 0.0481(19) 0.0464(18) 0.0071(15) 0.0031(15) 0.0065(15) C2 0.0319(15) 0.0363(15) 0.0286(14) 0.0018(11) 0.0029(11) -0.0017(11) C3 0.0353(17) 0.0469(17) 0.0360(16) -0.0008(13) -0.0038(12) -0.0048(13) C4 0.0402(18) 0.0468(18) 0.0382(17) 0.0078(14) -0.0066(13) -0.0053(14) C11 0.0415(17) 0.0379(16) 0.0322(15) -0.0046(12) -0.0028(12) 0.0039(13) C12 0.044(2) 0.058(2) 0.0360(16) -0.0117(15) -0.0034(14) 0.0127(15) C13 0.074(3) 0.074(3) 0.049(2) -0.010(2) -0.001(2) 0.039(2) C14 0.110(4) 0.049(2) 0.057(2) 0.0057(19) 0.005(2) 0.034(2) C15 0.089(3) 0.0402(19) 0.052(2) 0.0071(16) 0.003(2) 0.0089(19) C16 0.054(2) 0.0385(17) 0.0419(18) 0.0013(13) 0.0014(15) 0.0010(14) C17 0.042(2) 0.083(3) 0.044(2) -0.0146(18) 0.0067(15) 0.0073(18) C18 0.046(2) 0.128(4) 0.065(3) -0.034(3) 0.0055(19) 0.017(3) C19 0.055(3) 0.132(5) 0.045(2) -0.001(3) 0.0088(19) 0.002(3) C20 0.051(2) 0.050(2) 0.063(2) 0.0160(17) 0.0147(17) -0.0016(16) C21 0.071(3) 0.061(2) 0.069(3) 0.013(2) 0.028(2) 0.001(2) C22 0.060(3) 0.107(4) 0.077(3) 0.026(3) 0.004(2) -0.021(3) C31 0.0462(19) 0.0404(17) 0.0390(17) 0.0132(13) -0.0087(14) -0.0109(14) C32 0.056(2) 0.060(2) 0.0384(18) 0.0168(16) -0.0033(15) -0.0145(17) C33 0.081(3) 0.067(3) 0.047(2) 0.023(2) -0.002(2) -0.035(2) C34 0.090(3) 0.044(2) 0.057(2) 0.0148(18) -0.012(2) -0.024(2) C35 0.075(3) 0.0394(18) 0.054(2) 0.0119(16) -0.0115(19) -0.0107(18) C36 0.050(2) 0.0376(16) 0.0453(18) 0.0097(14) -0.0082(15) -0.0053(14) C37 0.067(3) 0.076(3) 0.054(2) 0.021(2) 0.017(2) -0.006(2) C38 0.072(4) 0.197(8) 0.083(4) -0.004(5) 0.021(3) -0.006(4) C39 0.126(5) 0.101(4) 0.056(3) -0.002(3) 0.015(3) 0.010(4) C40 0.050(2) 0.0375(17) 0.069(2) 0.0093(16) 0.0058(17) 0.0009(15) C41 0.081(3) 0.053(2) 0.082(3) 0.003(2) 0.026(3) 0.000(2) C42 0.055(3) 0.085(3) 0.108(4) 0.015(3) -0.004(3) -0.003(2) Rh2 0.0406(4) 0.0869(6) 0.0416(3) 0.0041(3) -0.0027(2) 0.0108(3) Cl3 0.0678(13) 0.0698(13) 0.0526(11) 0.0062(9) -0.0003(9) 0.0187(11) Cl4 0.0598(12) 0.0750(13) 0.0404(9) 0.0072(9) -0.0023(8) 0.0195(10) O50 0.078(6) 0.198(12) 0.111(7) 0.048(8) -0.005(5) -0.030(7) O60 0.066(5) 0.189(10) 0.082(5) -0.047(6) 0.025(4) 0.015(5) C50 0.058(6) 0.094(7) 0.074(6) 0.029(5) -0.014(4) -0.021(5) C60 0.054(6) 0.127(10) 0.057(6) 0.002(6) -0.013(5) 0.010(6) Cl1S 0.085(2) 0.109(3) 0.176(4) -0.024(3) 0.034(2) 0.0162(19) Cl2S 0.559(18) 0.218(7) 0.138(5) 0.094(5) 0.137(8) 0.114(9) C1S 0.157(18) 0.058(8) 0.20(2) -0.010(11) 0.060(16) -0.017(9) Cl3S 0.113(2) 0.110(3) 0.150(3) -0.008(2) 0.022(3) 0.013(3) Cl4S 0.116(3) 0.138(3) 0.102(2) 0.064(2) 0.0194(19) -0.019(2) C2S 0.223(6) 0.149(4) 0.152(4) 0.079(3) -0.071(4) -0.049(4) Cl5S 0.223(6) 0.149(4) 0.152(4) 0.079(3) -0.071(4) -0.049(4) Cl6S 0.232(6) 0.124(3) 0.157(4) 0.021(3) -0.017(4) -0.049(4) C3S 0.113(2) 0.110(3) 0.150(3) -0.008(2) 0.022(3) 0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.901(4) . ? Rh1 C1 1.901(4) 3_656 ? Rh1 Si 2.3605(8) 3_656 ? Rh1 Si 2.3605(8) . ? Cl1 Si 2.0783(11) . ? Cl2 Si 2.0960(12) . ? Si C2 1.939(3) . ? O1 C1 1.121(5) . ? N1 C2 1.352(4) . ? N1 C3 1.381(4) . ? N1 C11 1.450(4) . ? N2 C2 1.354(4) . ? N2 C4 1.375(4) . ? N2 C31 1.459(4) . ? C3 C4 1.340(5) . ? C11 C16 1.396(5) . ? C11 C12 1.405(5) . ? C12 C13 1.392(6) . ? C12 C17 1.518(6) . ? C13 C14 1.365(7) . ? C14 C15 1.360(7) . ? C15 C16 1.405(5) . ? C16 C20 1.511(5) . ? C17 C18 1.524(6) . ? C17 C19 1.535(6) . ? C20 C22 1.533(6) . ? C20 C21 1.537(6) . ? C31 C36 1.391(5) . ? C31 C32 1.412(5) . ? C32 C33 1.406(6) . ? C32 C37 1.502(6) . ? C33 C34 1.385(7) . ? C34 C35 1.358(6) . ? C35 C36 1.401(5) . ? C36 C40 1.509(5) . ? C37 C38 1.503(7) . ? C37 C39 1.503(7) . ? C40 C41 1.526(6) . ? C40 C42 1.532(6) . ? Rh2 C50 1.809(10) . ? Rh2 C60 1.847(14) . ? Rh2 Cl3 2.357(2) . ? Rh2 Cl4 2.372(3) . ? O50 C50 1.103(13) . ? O60 C60 1.117(15) . ? Cl1S C1S 1.715(9) . ? Cl2S C1S 1.700(9) . ? Cl3S C2S 1.754(10) . ? Cl4S C2S 1.739(10) . ? Cl5S C3S 1.758(10) . ? Cl6S C3S 1.751(10) . ? 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 C1 Rh1 C1 180.0 . 3_656 ? C1 Rh1 Si 89.06(11) . 3_656 ? C1 Rh1 Si 90.94(11) 3_656 3_656 ? C1 Rh1 Si 90.94(11) . . ? C1 Rh1 Si 89.06(11) 3_656 . ? Si Rh1 Si 180.0 3_656 . ? C2 Si Cl1 102.37(10) . . ? C2 Si Cl2 95.54(10) . . ? Cl1 Si Cl2 102.56(5) . . ? C2 Si Rh1 123.41(10) . . ? Cl1 Si Rh1 113.06(4) . . ? Cl2 Si Rh1 116.64(4) . . ? C2 N1 C3 110.4(3) . . ? C2 N1 C11 126.8(3) . . ? C3 N1 C11 122.7(3) . . ? C2 N2 C4 110.4(3) . . ? C2 N2 C31 129.1(3) . . ? C4 N2 C31 120.1(3) . . ? O1 C1 Rh1 179.7(4) . . ? N1 C2 N2 105.1(2) . . ? N1 C2 Si 122.4(2) . . ? N2 C2 Si 131.8(2) . . ? C4 C3 N1 106.8(3) . . ? C3 C4 N2 107.3(3) . . ? C16 C11 C12 124.2(3) . . ? C16 C11 N1 118.4(3) . . ? C12 C11 N1 117.3(3) . . ? C13 C12 C11 115.7(4) . . ? C13 C12 C17 121.9(4) . . ? C11 C12 C17 122.3(3) . . ? C14 C13 C12 121.6(4) . . ? C15 C14 C13 121.3(4) . . ? C14 C15 C16 121.2(4) . . ? C11 C16 C15 115.9(4) . . ? C11 C16 C20 123.9(3) . . ? C15 C16 C20 120.2(4) . . ? C12 C17 C18 114.2(4) . . ? C12 C17 C19 111.1(4) . . ? C18 C17 C19 108.8(3) . . ? C16 C20 C22 110.3(4) . . ? C16 C20 C21 112.3(3) . . ? C22 C20 C21 110.1(3) . . ? C36 C31 C32 124.6(3) . . ? C36 C31 N2 118.8(3) . . ? C32 C31 N2 116.5(3) . . ? C33 C32 C31 114.9(4) . . ? C33 C32 C37 121.6(4) . . ? C31 C32 C37 123.5(3) . . ? C34 C33 C32 122.0(4) . . ? C35 C34 C33 120.4(4) . . ? C34 C35 C36 121.8(4) . . ? C31 C36 C35 116.4(4) . . ? C31 C36 C40 123.0(3) . . ? C35 C36 C40 120.6(4) . . ? C32 C37 C38 112.3(5) . . ? C32 C37 C39 110.1(4) . . ? C38 C37 C39 112.6(5) . . ? C36 C40 C41 112.3(3) . . ? C36 C40 C42 109.4(4) . . ? C41 C40 C42 111.4(4) . . ? C50 Rh2 C60 88.7(6) . . ? C50 Rh2 Cl3 91.1(4) . . ? C60 Rh2 Cl3 179.8(5) . . ? C50 Rh2 Cl4 176.4(4) . . ? C60 Rh2 Cl4 87.8(5) . . ? Cl3 Rh2 Cl4 92.42(8) . . ? O50 C50 Rh2 178.8(14) . . ? O60 C60 Rh2 173.8(13) . . ? Cl2S C1S Cl1S 110.2(8) . . ? Cl4S C2S Cl3S 105.9(9) . . ? Cl6S C3S Cl5S 110.3(8) . . ? 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 C1 Rh1 Si C2 -93.83(16) . . . . ? C1 Rh1 Si C2 86.18(16) 3_656 . . . ? Si Rh1 Si C2 26(15) 3_656 . . . ? C1 Rh1 Si Cl1 142.14(12) . . . . ? C1 Rh1 Si Cl1 -37.86(12) 3_656 . . . ? Si Rh1 Si Cl1 -98(15) 3_656 . . . ? C1 Rh1 Si Cl2 23.59(12) . . . . ? C1 Rh1 Si Cl2 -156.41(12) 3_656 . . . ? Si Rh1 Si Cl2 143(15) 3_656 . . . ? C1 Rh1 C1 O1 40(82) 3_656 . . . ? Si Rh1 C1 O1 133(100) 3_656 . . . ? Si Rh1 C1 O1 -47(100) . . . . ? C3 N1 C2 N2 -0.5(3) . . . . ? C11 N1 C2 N2 174.8(3) . . . . ? C3 N1 C2 Si 171.0(2) . . . . ? C11 N1 C2 Si -13.7(4) . . . . ? C4 N2 C2 N1 0.3(4) . . . . ? C31 N2 C2 N1 -172.4(3) . . . . ? C4 N2 C2 Si -170.1(3) . . . . ? C31 N2 C2 Si 17.2(5) . . . . ? Cl1 Si C2 N1 172.0(2) . . . . ? Cl2 Si C2 N1 -83.8(3) . . . . ? Rh1 Si C2 N1 43.3(3) . . . . ? Cl1 Si C2 N2 -19.1(3) . . . . ? Cl2 Si C2 N2 85.1(3) . . . . ? Rh1 Si C2 N2 -147.7(3) . . . . ? C2 N1 C3 C4 0.4(4) . . . . ? C11 N1 C3 C4 -175.0(3) . . . . ? N1 C3 C4 N2 -0.2(4) . . . . ? C2 N2 C4 C3 0.0(4) . . . . ? C31 N2 C4 C3 173.4(3) . . . . ? C2 N1 C11 C16 107.1(4) . . . . ? C3 N1 C11 C16 -78.2(4) . . . . ? C2 N1 C11 C12 -77.1(4) . . . . ? C3 N1 C11 C12 97.6(4) . . . . ? C16 C11 C12 C13 -3.4(5) . . . . ? N1 C11 C12 C13 -178.9(3) . . . . ? C16 C11 C12 C17 173.3(3) . . . . ? N1 C11 C12 C17 -2.2(5) . . . . ? C11 C12 C13 C14 1.7(6) . . . . ? C17 C12 C13 C14 -175.0(4) . . . . ? C12 C13 C14 C15 0.9(7) . . . . ? C13 C14 C15 C16 -2.0(7) . . . . ? C12 C11 C16 C15 2.4(5) . . . . ? N1 C11 C16 C15 177.8(3) . . . . ? C12 C11 C16 C20 -175.5(3) . . . . ? N1 C11 C16 C20 -0.1(5) . . . . ? C14 C15 C16 C11 0.3(6) . . . . ? C14 C15 C16 C20 178.3(4) . . . . ? C13 C12 C17 C18 -26.2(5) . . . . ? C11 C12 C17 C18 157.3(4) . . . . ? C13 C12 C17 C19 97.2(5) . . . . ? C11 C12 C17 C19 -79.3(5) . . . . ? C11 C16 C20 C22 106.0(4) . . . . ? C15 C16 C20 C22 -71.8(5) . . . . ? C11 C16 C20 C21 -130.8(4) . . . . ? C15 C16 C20 C21 51.4(5) . . . . ? C2 N2 C31 C36 -99.4(4) . . . . ? C4 N2 C31 C36 88.5(4) . . . . ? C2 N2 C31 C32 85.0(4) . . . . ? C4 N2 C31 C32 -87.1(4) . . . . ? C36 C31 C32 C33 1.4(5) . . . . ? N2 C31 C32 C33 176.8(3) . . . . ? C36 C31 C32 C37 -176.6(3) . . . . ? N2 C31 C32 C37 -1.2(5) . . . . ? C31 C32 C33 C34 -0.7(6) . . . . ? C37 C32 C33 C34 177.3(4) . . . . ? C32 C33 C34 C35 0.0(6) . . . . ? C33 C34 C35 C36 0.0(6) . . . . ? C32 C31 C36 C35 -1.4(5) . . . . ? N2 C31 C36 C35 -176.7(3) . . . . ? C32 C31 C36 C40 176.0(3) . . . . ? N2 C31 C36 C40 0.8(5) . . . . ? C34 C35 C36 C31 0.7(5) . . . . ? C34 C35 C36 C40 -176.9(4) . . . . ? C33 C32 C37 C38 53.7(6) . . . . ? C31 C32 C37 C38 -128.4(5) . . . . ? C33 C32 C37 C39 -72.6(5) . . . . ? C31 C32 C37 C39 105.3(5) . . . . ? C31 C36 C40 C41 134.0(4) . . . . ? C35 C36 C40 C41 -48.7(5) . . . . ? C31 C36 C40 C42 -101.8(4) . . . . ? C35 C36 C40 C42 75.6(5) . . . . ? C60 Rh2 C50 O50 18(50) . . . . ? Cl3 Rh2 C50 O50 -162(50) . . . . ? Cl4 Rh2 C50 O50 24(54) . . . . ? C50 Rh2 C60 O60 -135(10) . . . . ? Cl3 Rh2 C60 O60 -139(100) . . . . ? Cl4 Rh2 C60 O60 46(10) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 68.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.203 _refine_diff_density_min -0.869 _refine_diff_density_rms 0.079