# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Sella, Andrea' _publ_contact_author_email a.sella@ucl.ac.uk _publ_author_name A.Sella # Attachment '- 2-Sm.cif' data_2-Sm _database_code_depnum_ccdc_archive 'CCDC 776641' #TrackingRef '- 2-Sm.cif' _vrf_PLAT601_2-Sm ; RESPONSE: No peaks of sufficient magnitude were found in the final difference Fourier map to warrant refinement as (even partial-occupancy) solvent molecules or other species of chemical significance. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;hydro-(tris-3-t-butyl-5-methylpyrazolyl)borate samarium iodide bis THF adduct ; _chemical_melting_point ? _chemical_formula_moiety 'C32 H56 B I N6 O2 Sm, 0.5(C4 H10 O)' _chemical_formula_sum 'C34 H61 B I N6 O2.50 Sm' _chemical_formula_weight 881.95 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/m' _symmetry_space_group_name_Hall '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 21.609(3) _cell_length_b 12.869(2) _cell_length_c 15.323(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.350(13) _cell_angle_gamma 90.00 _cell_volume 4215.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 21.07 _cell_measurement_theta_max 26.28 _exptl_crystal_description block _exptl_crystal_colour 'blue black' _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1788 _exptl_absorpt_coefficient_mu 2.160 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.733 _exptl_absorpt_correction_T_max 0.917 _exptl_absorpt_process_details 'North, A.C.T.; Phillips, D.C.; Mathews, F.S. Acta Cryst. 1968. A24' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nicolet R3mV' _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3981 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 25.06 _reflns_number_total 3868 _reflns_number_gt 3091 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nicolet P3 software (Nicolet, 1980)' _computing_cell_refinement 'Nicolet P3 software (Nicolet, 1980)' _computing_data_reduction 'RDNIC (Howie. 1980)' _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^)+(0.0416P)^2^+22.8395P] 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 3868 _refine_ls_number_parameters 219 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0951 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.238784(19) 0.0000 0.19154(2) 0.03507(13) Uani 1 2 d S . . I I 0.26667(4) 0.0000 -0.00732(4) 0.0652(2) Uani 1 2 d S . . N11 N 0.1716(2) 0.0991(4) 0.3592(3) 0.0395(10) Uani 1 1 d . . . N12 N 0.1598(2) 0.1109(4) 0.2686(3) 0.0422(11) Uani 1 1 d . . . N21 N 0.2717(3) 0.0000 0.4202(4) 0.0383(14) Uani 1 2 d S . . N22 N 0.3060(3) 0.0000 0.3500(4) 0.0380(14) Uani 1 2 d S . . B1 B 0.1987(4) 0.0000 0.4054(5) 0.0377(19) Uani 1 2 d S . . H1 H 0.1857 0.0000 0.4641 0.045 Uiso 1 2 calc SR . . O1 O 0.2866(2) 0.1899(3) 0.1961(3) 0.0565(11) Uani 1 1 d . . . C13 C 0.1263(3) 0.1980(5) 0.2529(4) 0.0507(15) Uani 1 1 d . . . C14 C 0.1184(3) 0.2433(5) 0.3318(4) 0.0628(18) Uani 1 1 d . . . H14 H 0.0974 0.3051 0.3390 0.075 Uiso 1 1 calc R . . C15 C 0.1467(3) 0.1816(5) 0.3971(4) 0.0548(16) Uani 1 1 d . . . C16 C 0.1519(5) 0.1951(7) 0.4952(5) 0.101(3) Uani 1 1 d . . . H16A H 0.1917 0.1696 0.5228 0.121 Uiso 1 1 calc R . . H16B H 0.1191 0.1569 0.5168 0.121 Uiso 1 1 calc R . . H16C H 0.1482 0.2675 0.5089 0.121 Uiso 1 1 calc R . . C17 C 0.1000(3) 0.2310(6) 0.1607(4) 0.0624(18) Uani 1 1 d . . . C18 C 0.1111(5) 0.3483(8) 0.1519(7) 0.124(4) Uani 1 1 d . . . H18A H 0.1553 0.3620 0.1598 0.148 Uiso 1 1 calc R . . H18B H 0.0924 0.3849 0.1960 0.148 Uiso 1 1 calc R . . H18C H 0.0926 0.3713 0.0944 0.148 Uiso 1 1 calc R . . C19 C 0.1295(4) 0.1744(8) 0.0908(4) 0.104(3) Uani 1 1 d . . . H19A H 0.1228 0.1011 0.0959 0.124 Uiso 1 1 calc R . . H19B H 0.1736 0.1885 0.0987 0.124 Uiso 1 1 calc R . . H19C H 0.1109 0.1978 0.0335 0.124 Uiso 1 1 calc R . . C20 C 0.0301(3) 0.2144(10) 0.1476(5) 0.114(4) Uani 1 1 d . . . H20A H 0.0213 0.1418 0.1533 0.137 Uiso 1 1 calc R . . H20B H 0.0125 0.2379 0.0898 0.137 Uiso 1 1 calc R . . H20C H 0.0121 0.2530 0.1912 0.137 Uiso 1 1 calc R . . C23 C 0.3660(4) 0.0000 0.3850(5) 0.0427(18) Uani 1 2 d S . . C24 C 0.3708(4) 0.0000 0.4775(6) 0.055(2) Uani 1 2 d S . . H24 H 0.4075 0.0000 0.5176 0.066 Uiso 1 2 calc SR . . C25 C 0.3114(4) 0.0000 0.4967(5) 0.0443(19) Uani 1 2 d S . . C26 C 0.2910(5) 0.0000 0.5870(6) 0.072(3) Uani 1 2 d S . . H26A H 0.2611 0.0545 0.5901 0.087 Uiso 0.50 1 calc PR . . H26B H 0.3267 0.0112 0.6311 0.087 Uiso 0.50 1 calc PR . . H26C H 0.2723 -0.0657 0.5970 0.087 Uiso 0.50 1 calc PR . . C27 C 0.4198(4) 0.0000 0.3325(6) 0.054(2) Uani 1 2 d S . . C28 C 0.3986(4) 0.0000 0.2335(6) 0.070(3) Uani 1 2 d S . . H28A H 0.4345 0.0000 0.2033 0.084 Uiso 1 2 calc SR . . H28B H 0.3739 0.0609 0.2173 0.084 Uiso 0.50 1 calc PR . . H28C H 0.3739 -0.0609 0.2173 0.084 Uiso 0.50 1 calc PR . . C29 C 0.4604(4) 0.0967(7) 0.3569(5) 0.094(3) Uani 1 1 d . . . H29A H 0.4359 0.1581 0.3421 0.112 Uiso 1 1 calc R . . H29B H 0.4954 0.0962 0.3247 0.112 Uiso 1 1 calc R . . H29C H 0.4753 0.0963 0.4190 0.112 Uiso 1 1 calc R . . C31 C 0.3152(4) 0.2456(5) 0.1315(5) 0.072(2) Uani 1 1 d . . . H31A H 0.2834 0.2740 0.0866 0.086 Uiso 1 1 calc R . . H31B H 0.3419 0.1997 0.1032 0.086 Uiso 1 1 calc R . . C32 C 0.3524(3) 0.3298(6) 0.1782(5) 0.075(2) Uani 1 1 d . . . H32A H 0.3537 0.3901 0.1405 0.090 Uiso 1 1 calc R . . H32B H 0.3948 0.3071 0.1987 0.090 Uiso 1 1 calc R . . C33 C 0.3187(5) 0.3530(6) 0.2530(6) 0.092(3) Uani 1 1 d . . . H33A H 0.2866 0.4050 0.2367 0.110 Uiso 1 1 calc R . . H33B H 0.3472 0.3782 0.3033 0.110 Uiso 1 1 calc R . . C34 C 0.2903(3) 0.2525(5) 0.2740(4) 0.0657(19) Uani 1 1 d . . . H34A H 0.3161 0.2187 0.3229 0.079 Uiso 1 1 calc R . . H34B H 0.2490 0.2636 0.2898 0.079 Uiso 1 1 calc R . . O1S O 0.0000 0.0000 0.5000 0.172(5) Uiso 1 4 d S . . C1S C -0.0014(13) -0.052(2) 0.4234(16) 0.172(5) Uiso 0.50 1 d P . . H1SA H 0.0369 -0.0922 0.4272 0.206 Uiso 0.50 1 calc PR . . H1SB H -0.0357 -0.1014 0.4195 0.206 Uiso 0.50 1 calc PR . . C2S C -0.0075(10) 0.0000 0.3483(14) 0.172(5) Uiso 1 2 d S . . H2SA H -0.0084 -0.0478 0.3000 0.206 Uiso 0.50 1 calc PR . . H2SB H 0.0271 0.0467 0.3487 0.206 Uiso 0.50 1 calc PR . . H2SC H -0.0458 0.0390 0.3416 0.206 Uiso 0.50 1 calc PR . . 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 Sm 0.0369(2) 0.0388(2) 0.0308(2) 0.000 0.00918(14) 0.000 I 0.0986(5) 0.0625(4) 0.0387(3) 0.000 0.0238(3) 0.000 N11 0.042(2) 0.044(3) 0.035(2) -0.004(2) 0.0115(18) 0.005(2) N12 0.042(2) 0.045(3) 0.043(2) 0.001(2) 0.0154(19) 0.004(2) N21 0.040(3) 0.033(3) 0.043(4) 0.000 0.008(3) 0.000 N22 0.031(3) 0.046(4) 0.035(3) 0.000 0.001(3) 0.000 B1 0.038(5) 0.045(5) 0.031(4) 0.000 0.010(3) 0.000 O1 0.082(3) 0.041(2) 0.051(2) -0.0054(19) 0.023(2) -0.009(2) C13 0.046(3) 0.054(4) 0.054(3) 0.009(3) 0.013(3) 0.009(3) C14 0.070(4) 0.058(4) 0.063(4) -0.003(3) 0.019(3) 0.029(4) C15 0.060(4) 0.057(4) 0.049(3) -0.001(3) 0.014(3) 0.023(3) C16 0.151(8) 0.098(7) 0.053(4) -0.022(4) 0.012(5) 0.056(6) C17 0.053(4) 0.080(5) 0.056(4) 0.019(4) 0.016(3) 0.020(4) C18 0.159(10) 0.104(8) 0.105(7) 0.058(6) 0.013(7) 0.008(7) C19 0.114(7) 0.152(9) 0.045(4) 0.018(5) 0.014(4) 0.058(7) C20 0.057(4) 0.206(12) 0.076(5) 0.029(7) 0.000(4) 0.024(6) C23 0.042(4) 0.037(4) 0.048(5) 0.000 0.003(3) 0.000 C24 0.052(5) 0.060(6) 0.049(5) 0.000 -0.005(4) 0.000 C25 0.046(5) 0.056(5) 0.028(4) 0.000 -0.003(3) 0.000 C26 0.060(6) 0.113(9) 0.041(5) 0.000 -0.004(4) 0.000 C27 0.039(4) 0.058(6) 0.064(6) 0.000 0.009(4) 0.000 C28 0.043(5) 0.114(9) 0.057(6) 0.000 0.016(4) 0.000 C29 0.065(5) 0.126(8) 0.089(6) 0.002(5) 0.010(4) -0.039(5) C31 0.108(6) 0.051(4) 0.064(4) 0.012(3) 0.040(4) -0.005(4) C32 0.065(4) 0.079(5) 0.082(5) 0.011(4) 0.014(4) -0.022(4) C33 0.129(7) 0.056(5) 0.094(6) -0.016(4) 0.029(5) -0.028(5) C34 0.082(5) 0.057(4) 0.062(4) -0.020(3) 0.022(4) -0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm N12 2.632(4) 6 ? Sm N12 2.632(4) . ? Sm N22 2.642(6) . ? Sm O1 2.651(4) . ? Sm O1 2.651(4) 6 ? Sm I 3.1908(9) . ? N11 C15 1.359(7) . ? N11 N12 1.383(6) . ? N11 B1 1.532(6) . ? N12 C13 1.337(7) . ? N21 C25 1.348(9) . ? N21 N22 1.392(8) . ? N21 B1 1.562(11) . ? N22 C23 1.329(9) . ? B1 N11 1.532(6) 6 ? O1 C34 1.431(7) . ? O1 C31 1.433(7) . ? C13 C14 1.375(8) . ? C13 C17 1.505(8) . ? C14 C15 1.352(9) . ? C15 C16 1.501(9) . ? C17 C19 1.510(10) . ? C17 C20 1.510(9) . ? C17 C18 1.537(12) . ? C23 C24 1.405(11) . ? C23 C27 1.507(11) . ? C24 C25 1.358(12) . ? C25 C26 1.511(11) . ? C27 C28 1.521(12) . ? C27 C29 1.537(9) . ? C27 C29 1.537(9) 6 ? C31 C32 1.471(10) . ? C32 C33 1.476(10) . ? C33 C34 1.486(10) . ? O1S C1S 1.35(2) . ? O1S C1S 1.35(2) 2_556 ? C1S C2S 1.32(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Sm N12 65.6(2) 6 . ? N12 Sm N22 83.91(14) 6 . ? N12 Sm N22 83.91(14) . . ? N12 Sm O1 139.79(13) 6 . ? N12 Sm O1 76.36(14) . . ? N22 Sm O1 79.37(10) . . ? N12 Sm O1 76.36(14) 6 6 ? N12 Sm O1 139.79(13) . 6 ? N22 Sm O1 79.37(10) . 6 ? O1 Sm O1 134.47(19) . 6 ? N12 Sm I 130.76(10) 6 . ? N12 Sm I 130.76(10) . . ? N22 Sm I 136.28(13) . . ? O1 Sm I 84.17(8) . . ? O1 Sm I 84.17(8) 6 . ? C15 N11 N12 108.5(4) . . ? C15 N11 B1 126.9(5) . . ? N12 N11 B1 123.9(4) . . ? C13 N12 N11 106.7(4) . . ? C13 N12 Sm 138.0(4) . . ? N11 N12 Sm 110.7(3) . . ? C25 N21 N22 109.2(6) . . ? C25 N21 B1 129.0(6) . . ? N22 N21 B1 121.8(6) . . ? C23 N22 N21 106.6(6) . . ? C23 N22 Sm 138.2(5) . . ? N21 N22 Sm 115.3(4) . . ? N11 B1 N11 112.7(6) 6 . ? N11 B1 N21 112.1(4) 6 . ? N11 B1 N21 112.1(4) . . ? C34 O1 C31 108.5(5) . . ? C34 O1 Sm 121.0(3) . . ? C31 O1 Sm 130.4(4) . . ? N12 C13 C14 109.3(5) . . ? N12 C13 C17 121.7(5) . . ? C14 C13 C17 128.9(6) . . ? C15 C14 C13 107.6(6) . . ? C14 C15 N11 107.9(5) . . ? C14 C15 C16 129.3(6) . . ? N11 C15 C16 122.8(6) . . ? C13 C17 C19 112.9(6) . . ? C13 C17 C20 108.6(5) . . ? C19 C17 C20 110.7(7) . . ? C13 C17 C18 108.5(7) . . ? C19 C17 C18 108.9(7) . . ? C20 C17 C18 107.0(8) . . ? N22 C23 C24 109.4(7) . . ? N22 C23 C27 124.6(7) . . ? C24 C23 C27 126.0(7) . . ? C25 C24 C23 106.5(7) . . ? N21 C25 C24 108.3(7) . . ? N21 C25 C26 124.2(7) . . ? C24 C25 C26 127.5(7) . . ? C23 C27 C28 112.9(7) . . ? C23 C27 C29 109.2(5) . . ? C28 C27 C29 108.7(5) . . ? C23 C27 C29 109.2(5) . 6 ? C28 C27 C29 108.7(5) . 6 ? C29 C27 C29 108.1(9) . 6 ? O1 C31 C32 107.0(6) . . ? C31 C32 C33 103.3(6) . . ? C32 C33 C34 104.9(6) . . ? O1 C34 C33 106.5(5) . . ? C1S O1S C1S 120(2) . 2_556 ? C2S C1S O1S 119(2) . . ? 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 C15 N11 N12 C13 -2.0(6) . . . . ? B1 N11 N12 C13 168.8(5) . . . . ? C15 N11 N12 Sm 158.7(4) . . . . ? B1 N11 N12 Sm -30.5(6) . . . . ? N12 Sm N12 C13 -140.8(5) 6 . . . ? N22 Sm N12 C13 133.1(6) . . . . ? O1 Sm N12 C13 52.6(6) . . . . ? O1 Sm N12 C13 -161.3(5) 6 . . . ? I Sm N12 C13 -17.0(6) . . . . ? N12 Sm N12 N11 67.5(3) 6 . . . ? N22 Sm N12 N11 -18.5(3) . . . . ? O1 Sm N12 N11 -99.0(3) . . . . ? O1 Sm N12 N11 47.0(4) 6 . . . ? I Sm N12 N11 -168.7(3) . . . . ? C25 N21 N22 C23 0.000(1) . . . . ? B1 N21 N22 C23 180.0 . . . . ? C25 N21 N22 Sm 180.0 . . . . ? B1 N21 N22 Sm 0.0 . . . . ? N12 Sm N22 C23 146.98(10) 6 . . . ? N12 Sm N22 C23 -146.98(10) . . . . ? O1 Sm N22 C23 -69.76(10) . . . . ? O1 Sm N22 C23 69.76(10) 6 . . . ? I Sm N22 C23 0.0 . . . . ? N12 Sm N22 N21 -33.02(10) 6 . . . ? N12 Sm N22 N21 33.02(10) . . . . ? O1 Sm N22 N21 110.24(10) . . . . ? O1 Sm N22 N21 -110.24(10) 6 . . . ? I Sm N22 N21 180.0 . . . . ? C15 N11 B1 N11 129.4(6) . . . 6 ? N12 N11 B1 N11 -39.6(8) . . . 6 ? C15 N11 B1 N21 -103.0(7) . . . . ? N12 N11 B1 N21 88.0(6) . . . . ? C25 N21 B1 N11 -116.0(5) . . . 6 ? N22 N21 B1 N11 64.0(5) . . . 6 ? C25 N21 B1 N11 116.0(5) . . . . ? N22 N21 B1 N11 -64.0(5) . . . . ? N12 Sm O1 C34 25.2(6) 6 . . . ? N12 Sm O1 C34 44.4(5) . . . . ? N22 Sm O1 C34 -41.8(5) . . . . ? O1 Sm O1 C34 -105.3(5) 6 . . . ? I Sm O1 C34 178.8(5) . . . . ? N12 Sm O1 C31 -158.9(5) 6 . . . ? N12 Sm O1 C31 -139.7(6) . . . . ? N22 Sm O1 C31 134.0(6) . . . . ? O1 Sm O1 C31 70.6(6) 6 . . . ? I Sm O1 C31 -5.3(5) . . . . ? N11 N12 C13 C14 1.9(6) . . . . ? Sm N12 C13 C14 -150.5(5) . . . . ? N11 N12 C13 C17 -174.8(5) . . . . ? Sm N12 C13 C17 32.8(9) . . . . ? N12 C13 C14 C15 -1.1(8) . . . . ? C17 C13 C14 C15 175.3(7) . . . . ? C13 C14 C15 N11 -0.2(8) . . . . ? C13 C14 C15 C16 -179.9(8) . . . . ? N12 N11 C15 C14 1.3(7) . . . . ? B1 N11 C15 C14 -169.1(6) . . . . ? N12 N11 C15 C16 -178.9(7) . . . . ? B1 N11 C15 C16 10.7(10) . . . . ? N12 C13 C17 C19 -15.6(9) . . . . ? C14 C13 C17 C19 168.4(8) . . . . ? N12 C13 C17 C20 107.5(8) . . . . ? C14 C13 C17 C20 -68.4(10) . . . . ? N12 C13 C17 C18 -136.5(7) . . . . ? C14 C13 C17 C18 47.6(10) . . . . ? N21 N22 C23 C24 0.0 . . . . ? Sm N22 C23 C24 180.000(1) . . . . ? N21 N22 C23 C27 180.0 . . . . ? Sm N22 C23 C27 0.000(1) . . . . ? N22 C23 C24 C25 0.000(1) . . . . ? C27 C23 C24 C25 180.000(1) . . . . ? N22 N21 C25 C24 0.000(1) . . . . ? B1 N21 C25 C24 180.000(1) . . . . ? N22 N21 C25 C26 180.000(1) . . . . ? B1 N21 C25 C26 0.000(2) . . . . ? C23 C24 C25 N21 0.000(1) . . . . ? C23 C24 C25 C26 180.000(1) . . . . ? N22 C23 C27 C28 0.000(1) . . . . ? C24 C23 C27 C28 180.000(1) . . . . ? N22 C23 C27 C29 121.0(6) . . . . ? C24 C23 C27 C29 -59.0(6) . . . . ? N22 C23 C27 C29 -121.0(6) . . . 6 ? C24 C23 C27 C29 59.0(6) . . . 6 ? C34 O1 C31 C32 15.9(8) . . . . ? Sm O1 C31 C32 -160.4(4) . . . . ? O1 C31 C32 C33 -29.0(8) . . . . ? C31 C32 C33 C34 30.8(9) . . . . ? C31 O1 C34 C33 3.8(8) . . . . ? Sm O1 C34 C33 -179.5(5) . . . . ? C32 C33 C34 O1 -21.8(9) . . . . ? C1S O1S C1S C2S 175(3) 2_556 . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.733 _refine_diff_density_min -1.048 _refine_diff_density_rms 0.104 # Attachment '- 2-Yb-CNtBu.cif' data_2-Yb-CNtBu _database_code_depnum_ccdc_archive 'CCDC 776643' #TrackingRef '- 2-Yb-CNtBu.cif' _vrf_PLAT601_2-Yb-CNtBu ; RESPONSE: No peaks of sufficient magnitude were found in the final difference Fourier map to warrant refinement as (even partial-occupancy) solvent molecules or other species of chemical significance. ; _vrf_PLAT242_2-Yb-CNtBu ; RESPONSE: The named carbons (C2, C17, C27) are the quaternary carbons of t-butyl groups, thus would be expected to have Ueq's significantly lower than the attached methyl carbons. Only for the CNtBu group was the tBu modelled as disordered. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;(tris-3-t-butyl-5-methylpyrazolyl)borate ytterbium iodide t- butylisonitrile ; _chemical_melting_point ? _chemical_formula_moiety 'C29 H49 B I N7 Yb' _chemical_formula_sum 'C29 H49 B I N7 Yb' _chemical_formula_weight 806.50 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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' _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 10.581(2) _cell_length_b 21.078(6) _cell_length_c 16.443(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.700(19) _cell_angle_gamma 90.00 _cell_volume 3667.0(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 26 _cell_measurement_theta_min 12.12 _cell_measurement_theta_max 30.19 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.6 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 3.418 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.551 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'North, A.C.T.; Phillips, D.C.; Mathews, F.S. Acta Cryst. 1968. A24' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Nicolet R3mV' _diffrn_measurement_method \q-2\q _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6781 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 25.05 _reflns_number_total 6416 _reflns_number_gt 5131 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nicolet P3 software (Nicolet, 1980)' _computing_cell_refinement 'Nicolet P3 software (Nicolet, 1980)' _computing_data_reduction 'RDNIC (Howie. 1980)' _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^)+(0.0288P)^2^+10.5969P] 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 6416 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0385 _refine_ls_wR_factor_ref 0.0878 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 1.02765(2) 0.223893(12) 0.853519(16) 0.04494(9) Uani 1 1 d . . . I1 I 1.22652(4) 0.12292(2) 0.89090(3) 0.06411(14) Uani 1 1 d . . . N1 N 1.1958(6) 0.3724(3) 0.7921(4) 0.0695(16) Uani 1 1 d . A . N11 N 0.8498(5) 0.3035(2) 0.7304(3) 0.0486(12) Uani 1 1 d . . . N12 N 0.9451(4) 0.2582(2) 0.7228(3) 0.0505(12) Uani 1 1 d . . . N21 N 0.8408(4) 0.3444(2) 0.8784(3) 0.0471(12) Uani 1 1 d . . . N22 N 0.9367(4) 0.3158(2) 0.9225(3) 0.0475(11) Uani 1 1 d . . . N31 N 0.7222(4) 0.2443(2) 0.8360(3) 0.0466(11) Uani 1 1 d . . . N32 N 0.8021(4) 0.1970(2) 0.8629(3) 0.0463(11) Uani 1 1 d . . . C1 C 1.1727(7) 0.3225(4) 0.8148(5) 0.0666(18) Uani 1 1 d . . . C2 C 1.2164(9) 0.4363(4) 0.7617(6) 0.084(2) Uani 1 1 d . . . C3 C 1.1233(18) 0.4466(8) 0.6916(14) 0.150(8) Uani 0.70 1 d P A 1 H3A H 1.1392 0.4162 0.6495 0.225 Uiso 0.70 1 calc PR A 1 H3B H 1.1334 0.4887 0.6704 0.225 Uiso 0.70 1 calc PR A 1 H3C H 1.0386 0.4414 0.7107 0.225 Uiso 0.70 1 calc PR A 1 C4 C 1.3490(13) 0.4377(7) 0.7228(12) 0.124(6) Uani 0.70 1 d P A 1 H4A H 1.4125 0.4319 0.7644 0.186 Uiso 0.70 1 calc PR A 1 H4B H 1.3615 0.4778 0.6964 0.186 Uiso 0.70 1 calc PR A 1 H4C H 1.3552 0.4042 0.6835 0.186 Uiso 0.70 1 calc PR A 1 C5 C 1.201(3) 0.4821(7) 0.8281(11) 0.159(9) Uani 0.70 1 d P A 1 H5A H 1.2606 0.4725 0.8710 0.238 Uiso 0.70 1 calc PR A 1 H5B H 1.1170 0.4796 0.8485 0.238 Uiso 0.70 1 calc PR A 1 H5C H 1.2169 0.5242 0.8081 0.238 Uiso 0.70 1 calc PR A 1 C3A C 1.087(5) 0.469(3) 0.779(4) 0.160(18) Uiso 0.30 1 d P A 2 H3AA H 1.0658 0.4629 0.8354 0.240 Uiso 0.30 1 calc PR A 2 H3AB H 1.0221 0.4502 0.7454 0.240 Uiso 0.30 1 calc PR A 2 H3AC H 1.0926 0.5134 0.7677 0.240 Uiso 0.30 1 calc PR A 2 C4A C 1.248(5) 0.434(2) 0.679(3) 0.146(15) Uiso 0.30 1 d P A 2 H4AA H 1.3271 0.4121 0.6730 0.220 Uiso 0.30 1 calc PR A 2 H4AB H 1.2557 0.4764 0.6582 0.220 Uiso 0.30 1 calc PR A 2 H4AC H 1.1832 0.4118 0.6491 0.220 Uiso 0.30 1 calc PR A 2 C5A C 1.314(5) 0.465(3) 0.828(3) 0.16(2) Uiso 0.30 1 d P A 2 H5AA H 1.2731 0.4686 0.8796 0.242 Uiso 0.30 1 calc PR A 2 H5AB H 1.3412 0.5064 0.8107 0.242 Uiso 0.30 1 calc PR A 2 H5AC H 1.3860 0.4376 0.8331 0.242 Uiso 0.30 1 calc PR A 2 C13 C 0.9822(6) 0.2607(3) 0.6452(4) 0.0548(16) Uani 1 1 d . . . C14 C 0.9121(7) 0.3066(3) 0.6044(4) 0.0656(19) Uani 1 1 d . . . H14 H 0.9201 0.3180 0.5501 0.079 Uiso 1 1 calc R . . C15 C 0.8302(7) 0.3319(3) 0.6577(4) 0.0589(17) Uani 1 1 d . . . C16 C 0.7299(10) 0.3811(4) 0.6446(5) 0.101(3) Uani 1 1 d . . . H16A H 0.7477 0.4173 0.6784 0.151 Uiso 1 1 calc R . . H16B H 0.6491 0.3638 0.6585 0.151 Uiso 1 1 calc R . . H16C H 0.7287 0.3939 0.5886 0.151 Uiso 1 1 calc R . . C17 C 1.0831(7) 0.2163(4) 0.6126(4) 0.0674(19) Uani 1 1 d . . . C18 C 1.1312(11) 0.1727(6) 0.6745(6) 0.143(5) Uani 1 1 d . . . H18A H 1.0626 0.1482 0.6958 0.214 Uiso 1 1 calc R . . H18B H 1.1705 0.1965 0.7178 0.214 Uiso 1 1 calc R . . H18C H 1.1922 0.1448 0.6508 0.214 Uiso 1 1 calc R . . C19 C 1.0300(10) 0.1816(6) 0.5405(7) 0.145(5) Uani 1 1 d . . . H19A H 0.9612 0.1552 0.5573 0.218 Uiso 1 1 calc R . . H19B H 1.0947 0.1556 0.5170 0.218 Uiso 1 1 calc R . . H19C H 1.0001 0.2116 0.5008 0.218 Uiso 1 1 calc R . . C20 C 1.1910(9) 0.2574(6) 0.5779(7) 0.127(4) Uani 1 1 d . . . H20A H 1.2304 0.2810 0.6212 0.191 Uiso 1 1 calc R . . H20B H 1.1570 0.2862 0.5381 0.191 Uiso 1 1 calc R . . H20C H 1.2525 0.2304 0.5530 0.191 Uiso 1 1 calc R . . C23 C 0.9660(6) 0.3549(3) 0.9830(4) 0.0532(15) Uani 1 1 d . . . C24 C 0.8918(7) 0.4084(3) 0.9782(5) 0.072(2) Uani 1 1 d . . . H24 H 0.8939 0.4430 1.0132 0.087 Uiso 1 1 calc R . . C25 C 0.8142(7) 0.4005(3) 0.9117(4) 0.0630(18) Uani 1 1 d . . . C26 C 0.7116(9) 0.4438(4) 0.8809(6) 0.105(3) Uani 1 1 d . . . H26A H 0.6370 0.4195 0.8688 0.157 Uiso 1 1 calc R . . H26B H 0.7393 0.4648 0.8324 0.157 Uiso 1 1 calc R . . H26C H 0.6929 0.4749 0.9217 0.157 Uiso 1 1 calc R . . C27 C 1.0672(7) 0.3395(4) 1.0451(4) 0.0685(19) Uani 1 1 d . . . C28 C 1.1763(10) 0.3858(6) 1.0359(8) 0.156(6) Uani 1 1 d . . . H28A H 1.2125 0.3810 0.9830 0.233 Uiso 1 1 calc R . . H28B H 1.2396 0.3773 1.0768 0.233 Uiso 1 1 calc R . . H28C H 1.1459 0.4284 1.0421 0.233 Uiso 1 1 calc R . . C29 C 1.1137(11) 0.2738(5) 1.0371(7) 0.145(5) Uani 1 1 d . . . H29A H 1.0443 0.2448 1.0427 0.217 Uiso 1 1 calc R . . H29B H 1.1759 0.2655 1.0787 0.217 Uiso 1 1 calc R . . H29C H 1.1509 0.2684 0.9846 0.217 Uiso 1 1 calc R . . C30 C 1.0160(11) 0.3498(7) 1.1299(6) 0.147(5) Uani 1 1 d . . . H30A H 0.9481 0.3206 1.1393 0.220 Uiso 1 1 calc R . . H30B H 0.9853 0.3925 1.1346 0.220 Uiso 1 1 calc R . . H30C H 1.0821 0.3428 1.1694 0.220 Uiso 1 1 calc R . . C33 C 0.7281(6) 0.1478(3) 0.8810(4) 0.0531(15) Uani 1 1 d . . . C34 C 0.6022(6) 0.1626(3) 0.8654(4) 0.0596(17) Uani 1 1 d . . . H34 H 0.5326 0.1363 0.8724 0.071 Uiso 1 1 calc R . . C35 C 0.6017(5) 0.2234(3) 0.8377(4) 0.0536(15) Uani 1 1 d . . . C36 C 0.4909(6) 0.2631(4) 0.8116(5) 0.079(2) Uani 1 1 d . . . H36A H 0.5042 0.2787 0.7576 0.118 Uiso 1 1 calc R . . H36B H 0.4821 0.2983 0.8482 0.118 Uiso 1 1 calc R . . H36C H 0.4155 0.2378 0.8124 0.118 Uiso 1 1 calc R . . C37 C 0.7836(7) 0.0863(3) 0.9152(5) 0.070(2) Uani 1 1 d . . . C38 C 0.8560(8) 0.0530(4) 0.8445(6) 0.088(3) Uani 1 1 d . . . H38A H 0.9233 0.0800 0.8267 0.131 Uiso 1 1 calc R . . H38B H 0.7986 0.0451 0.8000 0.131 Uiso 1 1 calc R . . H38C H 0.8904 0.0135 0.8636 0.131 Uiso 1 1 calc R . . C39 C 0.8748(8) 0.0995(4) 0.9841(5) 0.081(2) Uani 1 1 d . . . H39A H 0.9417 0.1262 0.9652 0.122 Uiso 1 1 calc R . . H39B H 0.9096 0.0602 1.0037 0.122 Uiso 1 1 calc R . . H39C H 0.8312 0.1204 1.0274 0.122 Uiso 1 1 calc R . . C40 C 0.6756(9) 0.0436(4) 0.9440(7) 0.111(4) Uani 1 1 d . . . H40A H 0.6321 0.0640 0.9877 0.167 Uiso 1 1 calc R . . H40B H 0.7094 0.0038 0.9626 0.167 Uiso 1 1 calc R . . H40C H 0.6175 0.0362 0.8997 0.167 Uiso 1 1 calc R . . B1 B 0.7701(6) 0.3093(3) 0.8076(4) 0.0475(16) Uani 1 1 d . . . H1 H 0.6957 0.3348 0.7934 0.057 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 Yb1 0.04158(14) 0.03957(14) 0.05368(15) 0.00500(13) 0.00141(10) 0.00343(12) I1 0.0563(2) 0.0554(3) 0.0805(3) 0.0004(2) -0.0042(2) 0.0139(2) N1 0.073(4) 0.059(4) 0.077(4) 0.007(3) 0.013(3) -0.015(3) N11 0.055(3) 0.044(3) 0.046(3) 0.002(2) -0.005(2) 0.000(2) N12 0.045(3) 0.057(3) 0.049(3) 0.004(2) 0.003(2) 0.004(2) N21 0.050(3) 0.042(3) 0.049(3) -0.003(2) -0.004(2) 0.008(2) N22 0.046(3) 0.043(3) 0.053(3) -0.002(2) -0.002(2) 0.002(2) N31 0.044(3) 0.044(3) 0.052(3) 0.000(2) 0.001(2) 0.000(2) N32 0.045(3) 0.039(3) 0.056(3) -0.003(2) 0.002(2) 0.003(2) C1 0.060(4) 0.060(5) 0.080(5) 0.000(4) 0.008(4) -0.006(4) C2 0.100(6) 0.060(5) 0.093(6) 0.010(4) 0.010(5) -0.012(4) C3 0.142(15) 0.097(12) 0.21(2) 0.073(13) -0.080(15) -0.033(10) C4 0.092(10) 0.093(10) 0.187(17) 0.053(11) 0.032(10) -0.028(8) C5 0.29(3) 0.057(9) 0.126(14) -0.016(9) 0.038(17) -0.015(13) C13 0.060(4) 0.060(4) 0.045(3) 0.002(3) 0.006(3) -0.010(3) C14 0.097(5) 0.055(4) 0.044(4) 0.009(3) 0.000(4) -0.002(4) C15 0.082(5) 0.041(3) 0.054(4) 0.006(3) -0.009(3) -0.002(3) C16 0.153(9) 0.074(6) 0.074(5) 0.024(4) -0.013(6) 0.040(6) C17 0.067(4) 0.081(5) 0.055(4) 0.001(4) 0.019(3) 0.005(4) C18 0.178(11) 0.142(10) 0.110(8) 0.044(7) 0.072(8) 0.107(9) C19 0.119(8) 0.192(13) 0.126(9) -0.085(9) 0.003(7) 0.042(9) C20 0.091(7) 0.135(10) 0.157(10) 0.005(8) 0.050(7) 0.005(6) C23 0.057(4) 0.049(4) 0.053(4) -0.009(3) -0.003(3) 0.000(3) C24 0.086(5) 0.051(4) 0.080(5) -0.017(4) -0.015(4) 0.010(4) C25 0.077(5) 0.046(4) 0.065(4) -0.002(3) -0.005(4) 0.015(3) C26 0.134(8) 0.068(5) 0.111(7) -0.022(5) -0.032(6) 0.045(5) C27 0.074(5) 0.067(5) 0.064(4) -0.009(4) -0.018(4) 0.000(4) C28 0.106(8) 0.173(12) 0.186(12) 0.032(10) -0.078(8) -0.061(8) C29 0.185(11) 0.100(8) 0.147(10) -0.035(7) -0.112(9) 0.066(8) C30 0.151(10) 0.217(15) 0.072(6) -0.023(8) -0.034(6) 0.062(10) C33 0.053(4) 0.045(3) 0.062(4) -0.003(3) 0.012(3) -0.013(3) C34 0.046(4) 0.059(4) 0.074(4) -0.006(4) 0.005(3) -0.013(3) C35 0.042(3) 0.064(4) 0.055(4) -0.011(3) 0.000(3) 0.000(3) C36 0.046(4) 0.095(6) 0.095(6) 0.004(5) -0.008(4) 0.002(4) C37 0.071(4) 0.043(4) 0.098(6) 0.007(4) 0.020(4) -0.005(3) C38 0.089(6) 0.055(5) 0.119(7) -0.018(5) 0.027(5) -0.004(4) C39 0.096(6) 0.071(5) 0.078(5) 0.024(4) 0.005(5) 0.020(4) C40 0.102(7) 0.061(5) 0.172(10) 0.037(6) 0.041(7) -0.012(5) B1 0.048(4) 0.040(4) 0.055(4) 0.000(3) -0.006(3) 0.007(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 Yb1 N12 2.421(5) . ? Yb1 N22 2.448(5) . ? Yb1 N32 2.460(5) . ? Yb1 C1 2.666(8) . ? Yb1 I1 3.0502(7) . ? N1 C1 1.143(9) . ? N1 C2 1.454(10) . ? N11 C15 1.351(8) . ? N11 N12 1.394(7) . ? N11 B1 1.538(9) . ? N12 C13 1.341(8) . ? N21 C25 1.335(8) . ? N21 N22 1.379(6) . ? N21 B1 1.561(8) . ? N22 C23 1.325(7) . ? N31 C35 1.351(7) . ? N31 N32 1.377(6) . ? N31 B1 1.536(8) . ? N32 C33 1.335(7) . ? C2 C4A 1.41(4) . ? C2 C5 1.468(17) . ? C2 C3 1.522(17) . ? C2 C4 1.550(15) . ? C2 C3A 1.56(5) . ? C2 C5A 1.61(5) . ? C13 C14 1.388(9) . ? C13 C17 1.522(9) . ? C14 C15 1.348(10) . ? C15 C16 1.499(10) . ? C17 C18 1.458(11) . ? C17 C19 1.498(12) . ? C17 C20 1.548(12) . ? C23 C24 1.376(9) . ? C23 C27 1.506(9) . ? C24 C25 1.370(9) . ? C25 C26 1.502(10) . ? C27 C29 1.477(11) . ? C27 C30 1.517(12) . ? C27 C28 1.521(12) . ? C33 C34 1.390(9) . ? C33 C37 1.528(9) . ? C34 C35 1.359(9) . ? C35 C36 1.499(9) . ? C37 C39 1.505(11) . ? C37 C40 1.533(10) . ? C37 C38 1.566(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 N12 Yb1 N22 92.03(16) . . ? N12 Yb1 N32 77.58(16) . . ? N22 Yb1 N32 76.49(16) . . ? N12 Yb1 C1 76.0(2) . . ? N22 Yb1 C1 74.0(2) . . ? N32 Yb1 C1 139.18(19) . . ? N12 Yb1 I1 128.91(12) . . ? N22 Yb1 I1 137.12(11) . . ? N32 Yb1 I1 119.59(11) . . ? C1 Yb1 I1 101.22(16) . . ? C1 N1 C2 176.1(8) . . ? C15 N11 N12 109.1(5) . . ? C15 N11 B1 128.0(5) . . ? N12 N11 B1 122.2(5) . . ? C13 N12 N11 106.2(5) . . ? C13 N12 Yb1 138.6(4) . . ? N11 N12 Yb1 112.3(3) . . ? C25 N21 N22 109.2(5) . . ? C25 N21 B1 128.6(5) . . ? N22 N21 B1 121.9(5) . . ? C23 N22 N21 106.7(5) . . ? C23 N22 Yb1 138.6(4) . . ? N21 N22 Yb1 113.1(3) . . ? C35 N31 N32 109.4(5) . . ? C35 N31 B1 127.8(5) . . ? N32 N31 B1 122.8(5) . . ? C33 N32 N31 106.0(5) . . ? C33 N32 Yb1 139.9(4) . . ? N31 N32 Yb1 113.8(3) . . ? N1 C1 Yb1 157.2(6) . . ? C4A C2 N1 110(2) . . ? N1 C2 C5 109.6(9) . . ? N1 C2 C3 107.1(8) . . ? C5 C2 C3 113.2(14) . . ? N1 C2 C4 107.4(8) . . ? C5 C2 C4 113.6(14) . . ? C3 C2 C4 105.4(12) . . ? C4A C2 C3A 114(3) . . ? N1 C2 C3A 102(2) . . ? C4A C2 C5A 121(3) . . ? N1 C2 C5A 102(2) . . ? C3A C2 C5A 105(3) . . ? N12 C13 C14 109.0(6) . . ? N12 C13 C17 121.8(6) . . ? C14 C13 C17 129.2(6) . . ? C15 C14 C13 107.8(6) . . ? C14 C15 N11 107.9(6) . . ? C14 C15 C16 129.8(6) . . ? N11 C15 C16 122.3(7) . . ? C18 C17 C19 111.7(9) . . ? C18 C17 C13 112.4(6) . . ? C19 C17 C13 108.8(7) . . ? C18 C17 C20 110.9(8) . . ? C19 C17 C20 104.6(8) . . ? C13 C17 C20 108.0(7) . . ? N22 C23 C24 109.8(6) . . ? N22 C23 C27 122.2(6) . . ? C24 C23 C27 128.0(6) . . ? C25 C24 C23 106.4(6) . . ? N21 C25 C24 107.9(6) . . ? N21 C25 C26 123.7(6) . . ? C24 C25 C26 128.3(7) . . ? C29 C27 C23 112.0(6) . . ? C29 C27 C30 109.8(9) . . ? C23 C27 C30 109.5(7) . . ? C29 C27 C28 109.8(9) . . ? C23 C27 C28 109.2(7) . . ? C30 C27 C28 106.3(9) . . ? N32 C33 C34 110.3(6) . . ? N32 C33 C37 121.2(6) . . ? C34 C33 C37 128.5(6) . . ? C35 C34 C33 105.9(6) . . ? N31 C35 C34 108.3(5) . . ? N31 C35 C36 123.2(6) . . ? C34 C35 C36 128.5(6) . . ? C39 C37 C33 111.1(6) . . ? C39 C37 C40 110.5(7) . . ? C33 C37 C40 109.1(6) . . ? C39 C37 C38 109.1(6) . . ? C33 C37 C38 107.2(6) . . ? C40 C37 C38 109.9(7) . . ? N31 B1 N11 111.5(5) . . ? N31 B1 N21 110.6(5) . . ? N11 B1 N21 113.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 N11 N12 C13 0.6(7) . . . . ? B1 N11 N12 C13 171.7(5) . . . . ? C15 N11 N12 Yb1 164.8(4) . . . . ? B1 N11 N12 Yb1 -24.0(6) . . . . ? N22 Yb1 N12 C13 139.9(6) . . . . ? N32 Yb1 N12 C13 -144.4(7) . . . . ? C1 Yb1 N12 C13 66.9(6) . . . . ? I1 Yb1 N12 C13 -26.3(7) . . . . ? N22 Yb1 N12 N11 -17.0(4) . . . . ? N32 Yb1 N12 N11 58.7(4) . . . . ? C1 Yb1 N12 N11 -89.9(4) . . . . ? I1 Yb1 N12 N11 176.9(3) . . . . ? C25 N21 N22 C23 0.8(7) . . . . ? B1 N21 N22 C23 -172.9(5) . . . . ? C25 N21 N22 Yb1 -167.6(4) . . . . ? B1 N21 N22 Yb1 18.6(6) . . . . ? N12 Yb1 N22 C23 -143.7(6) . . . . ? N32 Yb1 N22 C23 139.6(7) . . . . ? C1 Yb1 N22 C23 -68.9(6) . . . . ? I1 Yb1 N22 C23 20.4(7) . . . . ? N12 Yb1 N22 N21 19.4(4) . . . . ? N32 Yb1 N22 N21 -57.3(4) . . . . ? C1 Yb1 N22 N21 94.1(4) . . . . ? I1 Yb1 N22 N21 -176.5(3) . . . . ? C35 N31 N32 C33 -0.2(6) . . . . ? B1 N31 N32 C33 -179.0(5) . . . . ? C35 N31 N32 Yb1 175.4(4) . . . . ? B1 N31 N32 Yb1 -3.4(6) . . . . ? N12 Yb1 N32 C33 128.1(6) . . . . ? N22 Yb1 N32 C33 -136.8(7) . . . . ? C1 Yb1 N32 C33 178.6(6) . . . . ? I1 Yb1 N32 C33 0.1(7) . . . . ? N12 Yb1 N32 N31 -45.3(4) . . . . ? N22 Yb1 N32 N31 49.9(4) . . . . ? C1 Yb1 N32 N31 5.3(5) . . . . ? I1 Yb1 N32 N31 -173.2(3) . . . . ? C2 N1 C1 Yb1 -7(13) . . . . ? N12 Yb1 C1 N1 45.3(16) . . . . ? N22 Yb1 C1 N1 -51.0(16) . . . . ? N32 Yb1 C1 N1 -5.7(18) . . . . ? I1 Yb1 C1 N1 173.0(16) . . . . ? C1 N1 C2 C4A -90(12) . . . . ? C1 N1 C2 C5 91(12) . . . . ? C1 N1 C2 C3 -32(12) . . . . ? C1 N1 C2 C4 -145(12) . . . . ? C1 N1 C2 C3A 31(12) . . . . ? C1 N1 C2 C5A 140(12) . . . . ? N11 N12 C13 C14 0.1(7) . . . . ? Yb1 N12 C13 C14 -157.6(5) . . . . ? N11 N12 C13 C17 -178.0(6) . . . . ? Yb1 N12 C13 C17 24.3(10) . . . . ? N12 C13 C14 C15 -0.8(8) . . . . ? C17 C13 C14 C15 177.2(7) . . . . ? C13 C14 C15 N11 1.1(8) . . . . ? C13 C14 C15 C16 -177.3(8) . . . . ? N12 N11 C15 C14 -1.1(7) . . . . ? B1 N11 C15 C14 -171.5(6) . . . . ? N12 N11 C15 C16 177.5(7) . . . . ? B1 N11 C15 C16 7.0(11) . . . . ? N12 C13 C17 C18 0.1(11) . . . . ? C14 C13 C17 C18 -177.6(9) . . . . ? N12 C13 C17 C19 124.4(8) . . . . ? C14 C13 C17 C19 -53.3(11) . . . . ? N12 C13 C17 C20 -122.6(8) . . . . ? C14 C13 C17 C20 59.7(10) . . . . ? N21 N22 C23 C24 -0.6(7) . . . . ? Yb1 N22 C23 C24 163.1(5) . . . . ? N21 N22 C23 C27 179.6(6) . . . . ? Yb1 N22 C23 C27 -16.6(10) . . . . ? N22 C23 C24 C25 0.3(9) . . . . ? C27 C23 C24 C25 180.0(7) . . . . ? N22 N21 C25 C24 -0.7(8) . . . . ? B1 N21 C25 C24 172.6(6) . . . . ? N22 N21 C25 C26 -178.0(7) . . . . ? B1 N21 C25 C26 -4.8(12) . . . . ? C23 C24 C25 N21 0.3(9) . . . . ? C23 C24 C25 C26 177.5(8) . . . . ? N22 C23 C27 C29 -8.4(11) . . . . ? C24 C23 C27 C29 171.9(9) . . . . ? N22 C23 C27 C30 -130.5(9) . . . . ? C24 C23 C27 C30 49.8(11) . . . . ? N22 C23 C27 C28 113.5(9) . . . . ? C24 C23 C27 C28 -66.2(11) . . . . ? N31 N32 C33 C34 0.5(7) . . . . ? Yb1 N32 C33 C34 -173.2(5) . . . . ? N31 N32 C33 C37 -178.4(6) . . . . ? Yb1 N32 C33 C37 7.9(10) . . . . ? N32 C33 C34 C35 -0.6(7) . . . . ? C37 C33 C34 C35 178.2(7) . . . . ? N32 N31 C35 C34 -0.2(7) . . . . ? B1 N31 C35 C34 178.5(6) . . . . ? N32 N31 C35 C36 -179.5(6) . . . . ? B1 N31 C35 C36 -0.8(10) . . . . ? C33 C34 C35 N31 0.5(7) . . . . ? C33 C34 C35 C36 179.8(7) . . . . ? N32 C33 C37 C39 47.9(9) . . . . ? C34 C33 C37 C39 -130.8(7) . . . . ? N32 C33 C37 C40 169.9(7) . . . . ? C34 C33 C37 C40 -8.8(11) . . . . ? N32 C33 C37 C38 -71.2(8) . . . . ? C34 C33 C37 C38 110.1(8) . . . . ? C35 N31 B1 N11 -113.6(6) . . . . ? N32 N31 B1 N11 65.0(7) . . . . ? C35 N31 B1 N21 119.7(6) . . . . ? N32 N31 B1 N21 -61.7(7) . . . . ? C15 N11 B1 N31 122.3(6) . . . . ? N12 N11 B1 N31 -47.1(7) . . . . ? C15 N11 B1 N21 -112.4(6) . . . . ? N12 N11 B1 N21 78.3(7) . . . . ? C25 N21 B1 N31 -120.7(7) . . . . ? N22 N21 B1 N31 51.7(7) . . . . ? C25 N21 B1 N11 113.5(7) . . . . ? N22 N21 B1 N11 -74.1(7) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.503 _refine_diff_density_min -0.797 _refine_diff_density_rms 0.104 # Attachment '- 5a-Sm.cif' data_5a-Sm _database_code_depnum_ccdc_archive 'CCDC 776645' #TrackingRef '- 5a-Sm.cif' _vrf_CHEMW03_5a-Sm ; RESPONSE: The SQUEEZE routine (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) of the program PLATON (Spek, A. L. Acta Crystogr. 1990, A46, C-34) was used to remove the contributions of the two disordered solvent methylcyclohexane molecules to the observed structure factors. A large (934 cubic Angstroms) void centred at (0.036, 0.456, 0.500) with scattering associated with a total density equivalent to 218 electrons was found and attributed to the four molecules of methylcyclohexane located within in the unit cell (i.e. two solvent molecules per molecule of the Sm complex). ; _vrf_PLAT602_5a-Sm ; RESPONSE: See above note in response to the CHEMW03 alert. ; _vrf_PLAT043_5a-Sm ; RESPONSE: See above note in response to the CHEMW03 alert. ; _vrf_PLAT049_5a-Sm ; RESPONSE: See above note in response to the CHEMW03 alert. ; _vrf_PLAT041_5a-Sm ; RESPONSE: See above note in response to the CHEMW03 alert. ; _vrf_PLAT068_5a-Sm ; RESPONSE: See above note in response to the CHEMW03 alert. ; _vrf_FORMU01_5a-Sm ; RESPONSE: See above note in response to the CHEMW03 alert. ; _vrf_CELLZ01_5a-Sm ; RESPONSE: See above note in response to the CHEMW03 alert. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C35 H67 B N6 O Si2 Sm, 2(C7 H14)' _chemical_formula_sum 'C49 H95 B N6 O Si2 Sm' _chemical_formula_weight 1001.65 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' 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' Sm Sm -0.1638 3.4418 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1033(9) _cell_length_b 16.3329(13) _cell_length_c 16.7012(13) _cell_angle_alpha 65.7920(10) _cell_angle_beta 70.6740(10) _cell_angle_gamma 89.696(2) _cell_volume 2808.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5146 _cell_measurement_theta_min 2.384 _cell_measurement_theta_max 25.874 _exptl_crystal_description fragment _exptl_crystal_colour green-black _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.184 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 1.125 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7740 _exptl_absorpt_correction_T_max 0.9356 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21176 _diffrn_reflns_av_R_equivalents 0.0588 _diffrn_reflns_av_sigmaI/netI 0.1021 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.46 _reflns_number_total 11447 _reflns_number_gt 8354 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0506P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11447 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.954 _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 Sm Sm 0.18815(2) 0.209756(17) 0.09811(2) 0.03041(9) Uani 1 1 d . . . Si1 Si -0.09302(12) 0.07236(9) 0.24684(11) 0.0377(3) Uani 1 1 d . . . Si2 Si 0.09720(13) -0.04969(9) 0.29840(10) 0.0381(3) Uani 1 1 d . . . O O 0.3356(3) 0.1572(2) -0.0245(3) 0.0511(10) Uani 1 1 d . . . N11 N 0.2369(3) 0.4085(3) -0.1009(3) 0.0334(9) Uani 1 1 d . . . N12 N 0.1720(4) 0.3223(3) -0.0629(3) 0.0376(10) Uani 1 1 d . . . N21 N 0.3982(3) 0.3985(2) -0.0278(3) 0.0337(9) Uani 1 1 d . . . N22 N 0.3910(3) 0.3096(3) 0.0369(3) 0.0361(10) Uani 1 1 d . . . N31 N 0.1884(3) 0.4259(2) 0.0525(3) 0.0321(9) Uani 1 1 d . . . N32 N 0.1699(3) 0.3520(2) 0.1364(3) 0.0321(9) Uani 1 1 d . . . C1 C 0.0561(4) 0.0447(3) 0.2125(3) 0.0334(11) Uani 1 1 d . . . H1 H 0.0553 0.0205 0.1665 0.040 Uiso 1 1 calc R . . C2 C -0.1002(5) 0.1982(4) 0.1818(4) 0.0499(14) Uani 1 1 d . . . H2A H -0.0745 0.2153 0.1141 0.060 Uiso 1 1 calc R . . H2B H -0.0480 0.2343 0.1932 0.060 Uiso 1 1 calc R . . H2C H -0.1817 0.2095 0.2046 0.060 Uiso 1 1 calc R . . C3 C -0.1998(5) 0.0144(4) 0.2202(5) 0.0563(16) Uani 1 1 d . . . H3A H -0.1735 0.0340 0.1521 0.068 Uiso 1 1 calc R . . H3B H -0.2786 0.0305 0.2426 0.068 Uiso 1 1 calc R . . H3C H -0.2031 -0.0515 0.2521 0.068 Uiso 1 1 calc R . . C4 C -0.1601(5) 0.0467(4) 0.3742(4) 0.0558(16) Uani 1 1 d . . . H4A H -0.1817 -0.0191 0.4120 0.067 Uiso 1 1 calc R . . H4B H -0.2311 0.0758 0.3849 0.067 Uiso 1 1 calc R . . H4C H -0.1026 0.0700 0.3925 0.067 Uiso 1 1 calc R . . C5 C 0.2293(5) -0.0919(4) 0.2381(4) 0.0574(16) Uani 1 1 d . . . H5A H 0.2925 -0.0406 0.1936 0.069 Uiso 1 1 calc R . . H5B H 0.2066 -0.1215 0.2042 0.069 Uiso 1 1 calc R . . H5C H 0.2575 -0.1356 0.2852 0.069 Uiso 1 1 calc R . . C6 C -0.0206(5) -0.1547(3) 0.3768(4) 0.0477(14) Uani 1 1 d . . . H6A H -0.0933 -0.1375 0.4098 0.057 Uiso 1 1 calc R . . H6B H 0.0081 -0.1995 0.4229 0.057 Uiso 1 1 calc R . . H6C H -0.0371 -0.1810 0.3380 0.057 Uiso 1 1 calc R . . C7 C 0.1366(6) -0.0204(4) 0.3841(4) 0.0547(16) Uani 1 1 d . . . H7A H 0.2068 0.0264 0.3501 0.066 Uiso 1 1 calc R . . H7B H 0.1534 -0.0748 0.4300 0.066 Uiso 1 1 calc R . . H7C H 0.0702 0.0025 0.4169 0.066 Uiso 1 1 calc R . . C13 C 0.1425(4) 0.3194(4) -0.1337(4) 0.0388(12) Uani 1 1 d . . . C14 C 0.1855(5) 0.4015(4) -0.2134(4) 0.0461(13) Uani 1 1 d . . . H14 H 0.1763 0.4170 -0.2720 0.055 Uiso 1 1 calc R . . C15 C 0.2442(5) 0.4564(4) -0.1908(4) 0.0523(15) Uani 1 1 d . . . C16 C 0.3057(6) 0.5519(4) -0.2515(4) 0.0650(18) Uani 1 1 d . . . H16A H 0.3891 0.5548 -0.2574 0.078 Uiso 1 1 calc R . . H16B H 0.2676 0.5914 -0.2228 0.078 Uiso 1 1 calc R . . H16C H 0.3008 0.5722 -0.3140 0.078 Uiso 1 1 calc R . . C17 C 0.0703(5) 0.2394(4) -0.1241(4) 0.0477(14) Uani 1 1 d . . . C18 C 0.1245(7) 0.2220(5) -0.2097(5) 0.085(2) Uani 1 1 d . . . H18A H 0.2086 0.2175 -0.2206 0.103 Uiso 1 1 calc R . . H18B H 0.1168 0.2721 -0.2646 0.103 Uiso 1 1 calc R . . H18C H 0.0836 0.1650 -0.1995 0.103 Uiso 1 1 calc R . . C19 C -0.0546(6) 0.2602(5) -0.1180(6) 0.089(2) Uani 1 1 d . . . H19A H -0.0506 0.3130 -0.1756 0.106 Uiso 1 1 calc R . . H19B H -0.0912 0.2732 -0.0636 0.106 Uiso 1 1 calc R . . H19C H -0.1021 0.2076 -0.1110 0.106 Uiso 1 1 calc R . . C20 C 0.0618(7) 0.1526(4) -0.0376(5) 0.072(2) Uani 1 1 d . . . H20A H 0.1417 0.1408 -0.0388 0.086 Uiso 1 1 calc R . . H20B H 0.0202 0.1015 -0.0379 0.086 Uiso 1 1 calc R . . H20C H 0.0181 0.1599 0.0195 0.086 Uiso 1 1 calc R . . C23 C 0.4992(4) 0.2979(3) 0.0357(4) 0.0387(12) Uani 1 1 d . . . C24 C 0.5787(5) 0.3765(4) -0.0302(4) 0.0439(13) Uani 1 1 d . . . H24 H 0.6619 0.3856 -0.0455 0.053 Uiso 1 1 calc R . . C25 C 0.5120(4) 0.4378(3) -0.0684(4) 0.0380(12) Uani 1 1 d . . . C26 C 0.5539(5) 0.5346(3) -0.1408(4) 0.0459(14) Uani 1 1 d . . . H26A H 0.4987 0.5734 -0.1224 0.055 Uiso 1 1 calc R . . H26B H 0.5573 0.5393 -0.2020 0.055 Uiso 1 1 calc R . . H26C H 0.6329 0.5544 -0.1453 0.055 Uiso 1 1 calc R . . C27 C 0.5268(4) 0.2116(3) 0.1020(4) 0.0444(14) Uani 1 1 d . . . C28 C 0.6221(6) 0.1749(5) 0.0444(6) 0.089(3) Uani 1 1 d . . . H28A H 0.5915 0.1589 0.0044 0.107 Uiso 1 1 calc R . . H28B H 0.6436 0.1208 0.0871 0.107 Uiso 1 1 calc R . . H28C H 0.6923 0.2215 0.0049 0.107 Uiso 1 1 calc R . . C29 C 0.4178(5) 0.1387(3) 0.1623(4) 0.0512(15) Uani 1 1 d . . . H29A H 0.3885 0.1229 0.1215 0.061 Uiso 1 1 calc R . . H29B H 0.3559 0.1617 0.1989 0.061 Uiso 1 1 calc R . . H29C H 0.4390 0.0845 0.2051 0.061 Uiso 1 1 calc R . . C30 C 0.5719(7) 0.2325(4) 0.1689(6) 0.085(3) Uani 1 1 d . . . H30A H 0.5096 0.2541 0.2069 0.102 Uiso 1 1 calc R . . H30B H 0.6419 0.2795 0.1319 0.102 Uiso 1 1 calc R . . H30C H 0.5929 0.1773 0.2104 0.102 Uiso 1 1 calc R . . C33 C 0.0942(4) 0.3718(3) 0.2025(4) 0.0344(11) Uani 1 1 d . . . C34 C 0.0598(4) 0.4566(3) 0.1622(4) 0.0380(12) Uani 1 1 d . . . H34 H 0.0057 0.4856 0.1936 0.046 Uiso 1 1 calc R . . C35 C 0.1219(4) 0.4892(3) 0.0664(4) 0.0380(12) Uani 1 1 d . . . C36 C 0.1161(5) 0.5751(3) -0.0092(4) 0.0490(14) Uani 1 1 d . . . H36A H 0.1358 0.5684 -0.0678 0.059 Uiso 1 1 calc R . . H36B H 0.1727 0.6237 -0.0183 0.059 Uiso 1 1 calc R . . H36C H 0.0358 0.5904 0.0083 0.059 Uiso 1 1 calc R . . C37 C 0.0611(5) 0.3091(3) 0.3068(4) 0.0407(12) Uani 1 1 d . . . C38 C 0.1092(5) 0.2190(3) 0.3216(4) 0.0475(14) Uani 1 1 d . . . H38A H 0.0733 0.1869 0.2958 0.057 Uiso 1 1 calc R . . H38B H 0.0896 0.1813 0.3891 0.057 Uiso 1 1 calc R . . H38C H 0.1954 0.2311 0.2895 0.057 Uiso 1 1 calc R . . C39 C 0.1176(6) 0.3583(4) 0.3493(4) 0.0545(15) Uani 1 1 d . . . H39A H 0.0964 0.3201 0.4169 0.065 Uiso 1 1 calc R . . H39B H 0.0882 0.4163 0.3397 0.065 Uiso 1 1 calc R . . H39C H 0.2040 0.3694 0.3183 0.065 Uiso 1 1 calc R . . C40 C -0.0729(5) 0.2929(4) 0.3563(4) 0.0547(15) Uani 1 1 d . . . H40A H -0.1102 0.2623 0.3299 0.066 Uiso 1 1 calc R . . H40B H -0.1013 0.3512 0.3470 0.066 Uiso 1 1 calc R . . H40C H -0.0933 0.2546 0.4237 0.066 Uiso 1 1 calc R . . C41 C 0.4149(5) 0.2240(4) -0.1146(4) 0.0558(16) Uani 1 1 d . . . H41A H 0.4686 0.2623 -0.1057 0.067 Uiso 1 1 calc R . . H41B H 0.3693 0.2637 -0.1504 0.067 Uiso 1 1 calc R . . C42 C 0.4838(8) 0.1745(5) -0.1661(6) 0.100(3) Uani 1 1 d . . . H42A H 0.5629 0.1700 -0.1606 0.119 Uiso 1 1 calc R . . H42B H 0.4942 0.2051 -0.2336 0.119 Uiso 1 1 calc R . . C43 C 0.4110(7) 0.0821(4) -0.1194(5) 0.075(2) Uani 1 1 d . . . H43A H 0.3542 0.0805 -0.1500 0.090 Uiso 1 1 calc R . . H43B H 0.4621 0.0349 -0.1214 0.090 Uiso 1 1 calc R . . C44 C 0.3487(6) 0.0690(4) -0.0220(5) 0.0672(19) Uani 1 1 d . . . H44A H 0.2700 0.0316 0.0045 0.081 Uiso 1 1 calc R . . H44B H 0.3949 0.0376 0.0177 0.081 Uiso 1 1 calc R . . B B 0.2868(5) 0.4410(4) -0.0422(4) 0.0357(13) Uani 1 1 d . . . H1B H 0.3127 0.5081 -0.0793 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 Sm 0.02670(13) 0.02710(13) 0.03538(15) -0.01268(10) -0.00982(10) 0.00562(9) Si1 0.0347(8) 0.0329(7) 0.0439(9) -0.0134(6) -0.0166(7) 0.0045(6) Si2 0.0410(8) 0.0318(7) 0.0388(8) -0.0110(6) -0.0166(7) 0.0076(6) O 0.049(2) 0.042(2) 0.053(2) -0.0232(19) -0.005(2) 0.0098(18) N11 0.032(2) 0.032(2) 0.032(2) -0.0123(18) -0.0068(19) 0.0094(17) N12 0.036(2) 0.037(2) 0.042(3) -0.018(2) -0.016(2) 0.0082(18) N21 0.028(2) 0.026(2) 0.040(2) -0.0113(18) -0.0086(19) 0.0030(16) N22 0.030(2) 0.030(2) 0.046(3) -0.0148(19) -0.013(2) 0.0072(17) N31 0.032(2) 0.031(2) 0.039(2) -0.0196(19) -0.0138(19) 0.0108(17) N32 0.030(2) 0.031(2) 0.036(2) -0.0164(19) -0.0108(19) 0.0078(17) C1 0.031(3) 0.031(2) 0.036(3) -0.012(2) -0.012(2) 0.002(2) C2 0.051(3) 0.054(3) 0.058(4) -0.029(3) -0.028(3) 0.022(3) C3 0.044(3) 0.049(3) 0.077(4) -0.022(3) -0.030(3) 0.001(3) C4 0.046(3) 0.051(3) 0.057(4) -0.018(3) -0.008(3) 0.006(3) C5 0.064(4) 0.041(3) 0.058(4) -0.016(3) -0.018(3) 0.021(3) C6 0.058(4) 0.026(3) 0.041(3) -0.002(2) -0.012(3) -0.002(2) C7 0.064(4) 0.055(4) 0.050(4) -0.019(3) -0.032(3) 0.014(3) C13 0.038(3) 0.054(3) 0.033(3) -0.026(3) -0.015(2) 0.024(2) C14 0.050(3) 0.058(3) 0.035(3) -0.020(3) -0.020(3) 0.017(3) C15 0.047(3) 0.052(4) 0.044(3) -0.010(3) -0.015(3) 0.022(3) C16 0.079(5) 0.053(4) 0.051(4) -0.004(3) -0.033(4) 0.002(3) C17 0.050(3) 0.064(4) 0.046(3) -0.036(3) -0.023(3) 0.018(3) C18 0.112(7) 0.085(5) 0.071(5) -0.051(4) -0.024(5) 0.016(5) C19 0.062(5) 0.106(6) 0.135(7) -0.072(6) -0.055(5) 0.028(4) C20 0.093(5) 0.059(4) 0.069(5) -0.029(4) -0.035(4) -0.009(4) C23 0.026(3) 0.037(3) 0.051(3) -0.017(2) -0.014(2) 0.004(2) C24 0.029(3) 0.048(3) 0.063(4) -0.029(3) -0.020(3) 0.012(2) C25 0.034(3) 0.038(3) 0.041(3) -0.018(2) -0.012(2) 0.004(2) C26 0.040(3) 0.036(3) 0.047(3) -0.009(2) -0.009(3) -0.003(2) C27 0.032(3) 0.035(3) 0.070(4) -0.019(3) -0.029(3) 0.010(2) C28 0.062(5) 0.053(4) 0.111(6) -0.014(4) -0.009(4) 0.026(3) C29 0.040(3) 0.037(3) 0.065(4) -0.011(3) -0.018(3) 0.008(2) C30 0.094(5) 0.053(4) 0.120(7) -0.017(4) -0.078(5) 0.004(4) C33 0.031(3) 0.038(3) 0.038(3) -0.021(2) -0.012(2) 0.007(2) C34 0.039(3) 0.039(3) 0.044(3) -0.026(2) -0.014(3) 0.018(2) C35 0.034(3) 0.036(3) 0.054(3) -0.026(3) -0.020(3) 0.012(2) C36 0.045(3) 0.041(3) 0.056(4) -0.015(3) -0.020(3) 0.020(3) C37 0.042(3) 0.043(3) 0.037(3) -0.020(2) -0.010(2) 0.003(2) C38 0.064(4) 0.039(3) 0.032(3) -0.009(2) -0.016(3) 0.008(3) C39 0.069(4) 0.053(3) 0.045(3) -0.024(3) -0.020(3) 0.000(3) C40 0.050(4) 0.050(3) 0.047(4) -0.017(3) -0.003(3) 0.001(3) C41 0.053(4) 0.047(3) 0.045(3) -0.018(3) 0.006(3) 0.007(3) C42 0.100(6) 0.084(5) 0.089(6) -0.055(5) 0.020(5) 0.001(5) C43 0.080(5) 0.059(4) 0.093(6) -0.047(4) -0.022(4) 0.019(4) C44 0.070(4) 0.050(4) 0.084(5) -0.036(4) -0.021(4) 0.021(3) B 0.039(3) 0.021(3) 0.036(3) -0.005(2) -0.010(3) 0.013(2) _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 Sm N22 2.598(4) . ? Sm N12 2.634(4) . ? Sm N32 2.641(4) . ? Sm O 2.668(4) . ? Sm C1 2.697(4) . ? Si1 C1 1.820(5) . ? Si1 C4 1.868(6) . ? Si1 C3 1.871(5) . ? Si1 C2 1.908(5) . ? Si2 C1 1.825(5) . ? Si2 C7 1.876(6) . ? Si2 C5 1.881(6) . ? Si2 C6 1.907(5) . ? O C44 1.435(7) . ? O C41 1.444(6) . ? N11 C15 1.350(7) . ? N11 N12 1.397(5) . ? N11 B 1.559(7) . ? N12 C13 1.362(6) . ? N21 C25 1.344(6) . ? N21 N22 1.390(5) . ? N21 B 1.557(7) . ? N22 C23 1.317(6) . ? N31 C35 1.354(6) . ? N31 N32 1.370(5) . ? N31 B 1.556(7) . ? N32 C33 1.335(6) . ? C13 C14 1.388(7) . ? C13 C17 1.497(7) . ? C14 C15 1.384(8) . ? C15 C16 1.493(8) . ? C17 C18 1.505(8) . ? C17 C19 1.527(8) . ? C17 C20 1.527(8) . ? C23 C24 1.392(7) . ? C23 C27 1.512(7) . ? C24 C25 1.367(7) . ? C25 C26 1.502(7) . ? C27 C29 1.525(7) . ? C27 C28 1.532(9) . ? C27 C30 1.544(8) . ? C33 C34 1.400(6) . ? C33 C37 1.524(7) . ? C34 C35 1.385(7) . ? C35 C36 1.474(7) . ? C37 C40 1.523(7) . ? C37 C38 1.535(7) . ? C37 C39 1.553(7) . ? C41 C42 1.476(8) . ? C42 C43 1.501(9) . ? C43 C44 1.471(9) . ? 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 N22 Sm N12 84.97(12) . . ? N22 Sm N32 67.09(12) . . ? N12 Sm N32 84.49(12) . . ? N22 Sm O 74.95(12) . . ? N12 Sm O 77.31(12) . . ? N32 Sm O 139.05(11) . . ? N22 Sm C1 146.20(13) . . ? N12 Sm C1 125.09(13) . . ? N32 Sm C1 124.85(14) . . ? O Sm C1 95.31(13) . . ? C1 Si1 C4 113.7(3) . . ? C1 Si1 C3 113.8(3) . . ? C4 Si1 C3 107.2(3) . . ? C1 Si1 C2 113.0(2) . . ? C4 Si1 C2 104.7(3) . . ? C3 Si1 C2 103.6(3) . . ? C1 Si2 C7 113.9(2) . . ? C1 Si2 C5 110.9(2) . . ? C7 Si2 C5 106.6(3) . . ? C1 Si2 C6 115.9(2) . . ? C7 Si2 C6 103.8(3) . . ? C5 Si2 C6 104.8(3) . . ? C44 O C41 108.2(4) . . ? C44 O Sm 131.4(4) . . ? C41 O Sm 120.2(3) . . ? C15 N11 N12 110.1(4) . . ? C15 N11 B 127.6(4) . . ? N12 N11 B 122.2(4) . . ? C13 N12 N11 105.3(4) . . ? C13 N12 Sm 139.1(3) . . ? N11 N12 Sm 113.4(3) . . ? C25 N21 N22 108.6(4) . . ? C25 N21 B 128.8(4) . . ? N22 N21 B 122.6(4) . . ? C23 N22 N21 106.8(4) . . ? C23 N22 Sm 137.9(3) . . ? N21 N22 Sm 113.9(3) . . ? C35 N31 N32 110.5(4) . . ? C35 N31 B 124.6(4) . . ? N32 N31 B 124.1(4) . . ? C33 N32 N31 105.9(4) . . ? C33 N32 Sm 135.4(3) . . ? N31 N32 Sm 105.9(3) . . ? Si1 C1 Si2 119.1(3) . . ? Si1 C1 Sm 102.46(19) . . ? Si2 C1 Sm 125.7(2) . . ? N12 C13 C14 110.1(5) . . ? N12 C13 C17 124.0(5) . . ? C14 C13 C17 125.8(5) . . ? C15 C14 C13 106.5(5) . . ? N11 C15 C14 107.8(5) . . ? N11 C15 C16 123.9(6) . . ? C14 C15 C16 128.2(5) . . ? C13 C17 C18 109.7(5) . . ? C13 C17 C19 109.5(5) . . ? C18 C17 C19 107.9(6) . . ? C13 C17 C20 112.9(5) . . ? C18 C17 C20 108.0(5) . . ? C19 C17 C20 108.8(6) . . ? N22 C23 C24 110.3(4) . . ? N22 C23 C27 122.7(4) . . ? C24 C23 C27 126.9(4) . . ? C25 C24 C23 105.7(4) . . ? N21 C25 C24 108.6(4) . . ? N21 C25 C26 123.9(4) . . ? C24 C25 C26 127.5(5) . . ? C23 C27 C29 112.1(4) . . ? C23 C27 C28 109.0(5) . . ? C29 C27 C28 108.8(5) . . ? C23 C27 C30 109.2(4) . . ? C29 C27 C30 107.8(5) . . ? C28 C27 C30 109.9(6) . . ? N32 C33 C34 110.9(4) . . ? N32 C33 C37 121.3(4) . . ? C34 C33 C37 127.7(5) . . ? C35 C34 C33 105.1(4) . . ? N31 C35 C34 107.6(4) . . ? N31 C35 C36 124.8(5) . . ? C34 C35 C36 127.6(5) . . ? C40 C37 C33 109.9(4) . . ? C40 C37 C38 110.9(4) . . ? C33 C37 C38 111.4(4) . . ? C40 C37 C39 108.3(5) . . ? C33 C37 C39 107.5(4) . . ? C38 C37 C39 108.7(5) . . ? O C41 C42 107.5(5) . . ? C41 C42 C43 104.4(6) . . ? C44 C43 C42 103.7(6) . . ? O C44 C43 107.3(5) . . ? N31 B N21 112.2(4) . . ? N31 B N11 111.0(4) . . ? N21 B N11 112.8(4) . . ? 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 N22 Sm O C44 139.5(5) . . . . ? N12 Sm O C44 -132.4(5) . . . . ? N32 Sm O C44 161.8(5) . . . . ? C1 Sm O C44 -7.6(5) . . . . ? N22 Sm O C41 -45.5(4) . . . . ? N12 Sm O C41 42.7(4) . . . . ? N32 Sm O C41 -23.1(5) . . . . ? C1 Sm O C41 167.5(4) . . . . ? C15 N11 N12 C13 1.2(5) . . . . ? B N11 N12 C13 179.1(4) . . . . ? C15 N11 N12 Sm 167.8(3) . . . . ? B N11 N12 Sm -14.3(5) . . . . ? N22 Sm N12 C13 133.8(5) . . . . ? N32 Sm N12 C13 -158.8(5) . . . . ? O Sm N12 C13 58.1(5) . . . . ? C1 Sm N12 C13 -29.4(5) . . . . ? N22 Sm N12 N11 -26.2(3) . . . . ? N32 Sm N12 N11 41.2(3) . . . . ? O Sm N12 N11 -101.9(3) . . . . ? C1 Sm N12 N11 170.6(3) . . . . ? C25 N21 N22 C23 1.4(5) . . . . ? B N21 N22 C23 -175.8(5) . . . . ? C25 N21 N22 Sm -167.6(3) . . . . ? B N21 N22 Sm 15.2(5) . . . . ? N12 Sm N22 C23 -138.4(5) . . . . ? N32 Sm N22 C23 135.4(6) . . . . ? O Sm N22 C23 -60.2(5) . . . . ? C1 Sm N22 C23 16.5(7) . . . . ? N12 Sm N22 N21 25.8(3) . . . . ? N32 Sm N22 N21 -60.4(3) . . . . ? O Sm N22 N21 103.9(3) . . . . ? C1 Sm N22 N21 -179.3(3) . . . . ? C35 N31 N32 C33 -2.0(5) . . . . ? B N31 N32 C33 168.7(4) . . . . ? C35 N31 N32 Sm 146.2(3) . . . . ? B N31 N32 Sm -43.0(5) . . . . ? N22 Sm N32 C33 -153.3(5) . . . . ? N12 Sm N32 C33 119.9(4) . . . . ? O Sm N32 C33 -176.7(4) . . . . ? C1 Sm N32 C33 -9.7(5) . . . . ? N22 Sm N32 N31 72.8(3) . . . . ? N12 Sm N32 N31 -14.0(3) . . . . ? O Sm N32 N31 49.4(3) . . . . ? C1 Sm N32 N31 -143.5(2) . . . . ? C4 Si1 C1 Si2 30.9(4) . . . . ? C3 Si1 C1 Si2 -92.2(4) . . . . ? C2 Si1 C1 Si2 150.0(3) . . . . ? C4 Si1 C1 Sm -112.9(2) . . . . ? C3 Si1 C1 Sm 124.0(2) . . . . ? C2 Si1 C1 Sm 6.3(3) . . . . ? C7 Si2 C1 Si1 -80.3(4) . . . . ? C5 Si2 C1 Si1 159.4(3) . . . . ? C6 Si2 C1 Si1 40.0(4) . . . . ? C7 Si2 C1 Sm 54.4(4) . . . . ? C5 Si2 C1 Sm -65.9(4) . . . . ? C6 Si2 C1 Sm 174.8(3) . . . . ? N22 Sm C1 Si1 147.8(2) . . . . ? N12 Sm C1 Si1 -63.3(3) . . . . ? N32 Sm C1 Si1 47.0(3) . . . . ? O Sm C1 Si1 -141.5(2) . . . . ? N22 Sm C1 Si2 7.3(5) . . . . ? N12 Sm C1 Si2 156.2(2) . . . . ? N32 Sm C1 Si2 -93.5(3) . . . . ? O Sm C1 Si2 78.0(3) . . . . ? N11 N12 C13 C14 -1.0(5) . . . . ? Sm N12 C13 C14 -162.0(4) . . . . ? N11 N12 C13 C17 -179.0(4) . . . . ? Sm N12 C13 C17 20.0(8) . . . . ? N12 C13 C14 C15 0.5(6) . . . . ? C17 C13 C14 C15 178.5(5) . . . . ? N12 N11 C15 C14 -0.9(6) . . . . ? B N11 C15 C14 -178.7(4) . . . . ? N12 N11 C15 C16 178.8(5) . . . . ? B N11 C15 C16 1.0(8) . . . . ? C13 C14 C15 N11 0.2(6) . . . . ? C13 C14 C15 C16 -179.4(6) . . . . ? N12 C13 C17 C18 -136.6(6) . . . . ? C14 C13 C17 C18 45.8(7) . . . . ? N12 C13 C17 C19 105.2(6) . . . . ? C14 C13 C17 C19 -72.4(7) . . . . ? N12 C13 C17 C20 -16.1(7) . . . . ? C14 C13 C17 C20 166.2(5) . . . . ? N21 N22 C23 C24 -1.4(6) . . . . ? Sm N22 C23 C24 163.5(4) . . . . ? N21 N22 C23 C27 175.4(5) . . . . ? Sm N22 C23 C27 -19.7(9) . . . . ? N22 C23 C24 C25 0.9(6) . . . . ? C27 C23 C24 C25 -175.7(5) . . . . ? N22 N21 C25 C24 -0.8(6) . . . . ? B N21 C25 C24 176.1(5) . . . . ? N22 N21 C25 C26 -178.8(5) . . . . ? B N21 C25 C26 -1.9(8) . . . . ? C23 C24 C25 N21 0.0(6) . . . . ? C23 C24 C25 C26 177.8(5) . . . . ? N22 C23 C27 C29 5.4(8) . . . . ? C24 C23 C27 C29 -178.3(5) . . . . ? N22 C23 C27 C28 126.0(6) . . . . ? C24 C23 C27 C28 -57.8(7) . . . . ? N22 C23 C27 C30 -113.9(6) . . . . ? C24 C23 C27 C30 62.3(8) . . . . ? N31 N32 C33 C34 2.1(5) . . . . ? Sm N32 C33 C34 -131.8(4) . . . . ? N31 N32 C33 C37 -174.1(4) . . . . ? Sm N32 C33 C37 52.0(6) . . . . ? N32 C33 C34 C35 -1.5(6) . . . . ? C37 C33 C34 C35 174.5(5) . . . . ? N32 N31 C35 C34 1.1(5) . . . . ? B N31 C35 C34 -169.6(4) . . . . ? N32 N31 C35 C36 -177.0(5) . . . . ? B N31 C35 C36 12.4(7) . . . . ? C33 C34 C35 N31 0.2(5) . . . . ? C33 C34 C35 C36 178.2(5) . . . . ? N32 C33 C37 C40 -132.2(5) . . . . ? C34 C33 C37 C40 52.2(7) . . . . ? N32 C33 C37 C38 -8.8(6) . . . . ? C34 C33 C37 C38 175.6(5) . . . . ? N32 C33 C37 C39 110.2(5) . . . . ? C34 C33 C37 C39 -65.4(7) . . . . ? C44 O C41 C42 -3.6(8) . . . . ? Sm O C41 C42 -179.8(5) . . . . ? O C41 C42 C43 20.8(9) . . . . ? C41 C42 C43 C44 -29.5(8) . . . . ? C41 O C44 C43 -15.5(7) . . . . ? Sm O C44 C43 160.0(4) . . . . ? C42 C43 C44 O 28.0(8) . . . . ? C35 N31 B N21 138.8(4) . . . . ? N32 N31 B N21 -30.6(6) . . . . ? C35 N31 B N11 -93.9(5) . . . . ? N32 N31 B N11 96.6(5) . . . . ? C25 N21 B N31 -127.2(5) . . . . ? N22 N21 B N31 49.4(6) . . . . ? C25 N21 B N11 106.6(6) . . . . ? N22 N21 B N11 -76.9(6) . . . . ? C15 N11 B N31 126.4(5) . . . . ? N12 N11 B N31 -51.1(5) . . . . ? C15 N11 B N21 -106.7(5) . . . . ? N12 N11 B N21 75.8(5) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.46 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.246 _refine_diff_density_min -0.849 _refine_diff_density_rms 0.100 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.036 0.456 0.500 934 218 ' ' _platon_squeeze_details ; The SQUEEZE routine (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) of the program PLATON (Spek, A. L. Acta Crystogr. 1990, A46, C-34) was used to remove the contributions of the two disordered solvent methylcyclohexane molecules to the observed structure factors. A large (934 cubic Angstroms) void centred at (0.036, 0.456, 0.500) with scattering associated with a total density equivalent to 218 electrons was found and attributed to the four molecules of methylcyclohexane located within in the unit cell (i.e. two solvent molecules per molecule of the Sm complex). ; # Attachment '- 5-Sm.cif' data_5-Sm _database_code_depnum_ccdc_archive 'CCDC 776646' #TrackingRef '- 5-Sm.cif' _vrf_CHEMW03_5-Sm ; RESPONSE: Attempts to refine peaks of residual electron density as carbon atoms of a second full-occupancy molecule of solvent toluene were unsuccessful. The data were corrected for disordered electron density through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). A total solvent-accessible void volume of 983.5 cubic Angstroms with a total electron count of 271 (consistent with four molecules of solvent toluene, or one molecule per formula unit of the samarium complex) was found in the unit cell. ; _vrf_PLAT330_5-Sm ; RESPONSE: This solvent toluene molecule is disordered about the twofold axis (1/4, y, 1/4). ; _vrf_PLAT602_5-Sm ; RESPONSE: See above response to the CHEMW03 alert. ; _vrf_PLAT043_5-Sm ; RESPONSE: See above response to the CHEMW03 alert. ; _vrf_PLAT332_5-Sm ; RESPONSE: This solvent toluene molecule is disordered about the twofold axis (1/4, y, 1/4). ; _vrf_PLAT041_5-Sm ; RESPONSE: See above response to the CHEMW03 alert. ; _vrf_PLAT042_5-Sm ; RESPONSE: See above response to the CHEMW03 alert. ; _vrf_PLAT068_5-Sm ; RESPONSE: See above response to the CHEMW03 alert. ; _vrf_FORMU01_5-Sm ; RESPONSE: See above response to the CHEMW03 alert. ; _vrf_CELLZ01_5-Sm ; RESPONSE: See above response to the CHEMW03 alert. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H59 B N6 Si2 Sm, 1.5(C7 H8)' _chemical_formula_sum 'C41.50 H71 B N6 Si2 Sm' _chemical_formula_weight 871.38 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' Sm Sm -0.1638 3.4418 '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 2/n' _symmetry_space_group_name_Hall '-P 2yac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 17.8391(18) _cell_length_b 11.9006(12) _cell_length_c 24.176(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.6876(17) _cell_angle_gamma 90.00 _cell_volume 4916.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4300 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 25.85 _exptl_crystal_description prism _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1828 _exptl_absorpt_coefficient_mu 1.275 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5626 _exptl_absorpt_correction_T_max 0.8417 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32605 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0682 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 26.40 _reflns_number_total 10069 _reflns_number_gt 7249 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 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^)+(0.0678P)^2^+0.9449P] 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 10069 _refine_ls_number_parameters 397 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1347 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.269629(14) 0.26982(2) 0.517346(10) 0.03379(10) Uani 1 1 d . . . Si1 Si 0.18910(10) 0.47642(14) 0.58498(7) 0.0479(4) Uani 1 1 d . . . Si2 Si 0.09735(10) 0.25652(16) 0.59739(8) 0.0561(5) Uani 1 1 d . . . N11 N 0.4558(2) 0.2844(3) 0.52534(16) 0.0337(9) Uani 1 1 d . . . N12 N 0.4171(2) 0.2597(3) 0.56606(17) 0.0356(9) Uani 1 1 d . . . N21 N 0.3745(2) 0.3230(3) 0.42100(16) 0.0345(9) Uani 1 1 d . . . N22 N 0.3022(2) 0.3517(3) 0.42653(16) 0.0337(9) Uani 1 1 d . . . N31 N 0.3915(2) 0.1216(3) 0.45804(17) 0.0349(9) Uani 1 1 d . . . N32 N 0.3239(2) 0.1024(3) 0.47309(18) 0.0387(10) Uani 1 1 d . . . C1 C 0.1541(3) 0.3363(5) 0.5594(2) 0.0450(13) Uani 1 1 d . . . H1 H 0.1127 0.3553 0.5229 0.054 Uiso 1 1 calc R . . C2 C 0.2806(3) 0.5164(5) 0.5649(2) 0.0518(14) Uani 1 1 d . . . H2A H 0.2976 0.5915 0.5800 0.062 Uiso 1 1 calc R . . H2B H 0.2693 0.5166 0.5228 0.062 Uiso 1 1 calc R . . H2C H 0.3221 0.4619 0.5816 0.062 Uiso 1 1 calc R . . C3 C 0.1167(5) 0.5933(6) 0.5531(3) 0.084(2) Uani 1 1 d . . . H3A H 0.1381 0.6654 0.5700 0.101 Uiso 1 1 calc R . . H3B H 0.0671 0.5787 0.5617 0.101 Uiso 1 1 calc R . . H3C H 0.1075 0.5958 0.5111 0.101 Uiso 1 1 calc R . . C4 C 0.2181(4) 0.4925(6) 0.6658(3) 0.0687(19) Uani 1 1 d . . . H4A H 0.2349 0.5701 0.6762 0.082 Uiso 1 1 calc R . . H4B H 0.2613 0.4411 0.6834 0.082 Uiso 1 1 calc R . . H4C H 0.1733 0.4749 0.6801 0.082 Uiso 1 1 calc R . . C5 C 0.0232(4) 0.3390(7) 0.6225(3) 0.075(2) Uani 1 1 d . . . H5A H -0.0042 0.2886 0.6423 0.090 Uiso 1 1 calc R . . H5B H -0.0146 0.3732 0.5892 0.090 Uiso 1 1 calc R . . H5C H 0.0499 0.3980 0.6492 0.090 Uiso 1 1 calc R . . C6 C 0.0378(5) 0.1493(8) 0.5506(4) 0.093(3) Uani 1 1 d . . . H6A H 0.0076 0.1079 0.5720 0.111 Uiso 1 1 calc R . . H6B H 0.0720 0.0971 0.5379 0.111 Uiso 1 1 calc R . . H6C H 0.0019 0.1854 0.5169 0.111 Uiso 1 1 calc R . . C7 C 0.1591(4) 0.1881(8) 0.6646(4) 0.092(3) Uani 1 1 d . . . H7A H 0.1255 0.1465 0.6832 0.111 Uiso 1 1 calc R . . H7B H 0.1883 0.2457 0.6911 0.111 Uiso 1 1 calc R . . H7C H 0.1959 0.1361 0.6547 0.111 Uiso 1 1 calc R . . C13 C 0.4625(3) 0.2969(4) 0.6166(2) 0.0382(12) Uani 1 1 d . . . C14 C 0.5302(3) 0.3477(5) 0.6095(2) 0.0449(13) Uani 1 1 d . . . H14 H 0.5717 0.3810 0.6387 0.054 Uiso 1 1 calc R . . C15 C 0.5239(3) 0.3392(4) 0.5513(2) 0.0395(12) Uani 1 1 d . . . C16 C 0.5781(3) 0.3806(5) 0.5192(3) 0.0512(14) Uani 1 1 d . . . H16A H 0.6215 0.4215 0.5457 0.061 Uiso 1 1 calc R . . H16B H 0.5499 0.4310 0.4882 0.061 Uiso 1 1 calc R . . H16C H 0.5988 0.3167 0.5027 0.061 Uiso 1 1 calc R . . C17 C 0.4417(3) 0.2784(5) 0.6725(2) 0.0463(13) Uani 1 1 d . . . C18 C 0.3612(4) 0.2256(6) 0.6610(2) 0.0565(15) Uani 1 1 d . . . H18A H 0.3495 0.2131 0.6977 0.068 Uiso 1 1 calc R . . H18B H 0.3603 0.1537 0.6411 0.068 Uiso 1 1 calc R . . H18C H 0.3219 0.2761 0.6367 0.068 Uiso 1 1 calc R . . C19 C 0.4428(4) 0.3913(6) 0.7035(2) 0.0630(18) Uani 1 1 d . . . H19A H 0.4306 0.3789 0.7400 0.076 Uiso 1 1 calc R . . H19B H 0.4036 0.4416 0.6789 0.076 Uiso 1 1 calc R . . H19C H 0.4948 0.4253 0.7112 0.076 Uiso 1 1 calc R . . C20 C 0.5030(4) 0.1997(6) 0.7114(3) 0.0688(19) Uani 1 1 d . . . H20A H 0.4903 0.1874 0.7478 0.083 Uiso 1 1 calc R . . H20B H 0.5550 0.2340 0.7195 0.083 Uiso 1 1 calc R . . H20C H 0.5027 0.1276 0.6918 0.083 Uiso 1 1 calc R . . C23 C 0.2662(3) 0.4137(4) 0.3798(2) 0.0360(11) Uani 1 1 d . . . C24 C 0.3156(3) 0.4260(5) 0.3450(2) 0.0431(13) Uani 1 1 d . . . H24 H 0.3052 0.4670 0.3098 0.052 Uiso 1 1 calc R . . C25 C 0.3829(3) 0.3669(4) 0.3716(2) 0.0380(12) Uani 1 1 d . . . C26 C 0.4557(3) 0.3508(6) 0.3524(2) 0.0556(16) Uani 1 1 d . . . H26A H 0.4478 0.3846 0.3142 0.067 Uiso 1 1 calc R . . H26B H 0.4664 0.2704 0.3505 0.067 Uiso 1 1 calc R . . H26C H 0.5002 0.3872 0.3801 0.067 Uiso 1 1 calc R . . C27 C 0.1852(3) 0.4626(5) 0.3696(2) 0.0405(12) Uani 1 1 d . . . C28 C 0.1430(3) 0.4098(5) 0.4101(2) 0.0513(14) Uani 1 1 d . . . H28A H 0.1402 0.3282 0.4045 0.062 Uiso 1 1 calc R . . H28B H 0.0900 0.4406 0.4015 0.062 Uiso 1 1 calc R . . H28C H 0.1719 0.4268 0.4502 0.062 Uiso 1 1 calc R . . C29 C 0.1911(4) 0.5867(6) 0.3793(4) 0.076(2) Uani 1 1 d . . . H29A H 0.2170 0.6209 0.3528 0.091 Uiso 1 1 calc R . . H29B H 0.2217 0.6021 0.4192 0.091 Uiso 1 1 calc R . . H29C H 0.1385 0.6185 0.3723 0.091 Uiso 1 1 calc R . . C30 C 0.1389(4) 0.4386(8) 0.3076(3) 0.080(2) Uani 1 1 d . . . H30A H 0.1643 0.4752 0.2814 0.096 Uiso 1 1 calc R . . H30B H 0.0856 0.4678 0.3004 0.096 Uiso 1 1 calc R . . H30C H 0.1369 0.3573 0.3009 0.096 Uiso 1 1 calc R . . C33 C 0.3063(3) -0.0040(4) 0.4612(2) 0.0426(12) Uani 1 1 d . A . C34 C 0.3612(3) -0.0551(5) 0.4384(3) 0.0499(14) Uani 1 1 d . . . H34 H 0.3618 -0.1311 0.4265 0.060 Uiso 1 1 calc R . . C35 C 0.4141(3) 0.0272(4) 0.4368(2) 0.0410(12) Uani 1 1 d . . . C36 C 0.4843(3) 0.0163(5) 0.4161(2) 0.0512(14) Uani 1 1 d . . . H36A H 0.4755 0.0561 0.3793 0.061 Uiso 1 1 calc R . . H36B H 0.4942 -0.0634 0.4106 0.061 Uiso 1 1 calc R . . H36C H 0.5296 0.0489 0.4447 0.061 Uiso 1 1 calc R . . C37 C 0.2356(4) -0.0558(5) 0.4739(3) 0.0666(19) Uani 1 1 d D . . C38A C 0.1802(7) -0.1008(10) 0.4131(5) 0.095(3) Uiso 0.75 1 d P A 1 H38A H 0.1332 -0.1352 0.4189 0.114 Uiso 0.75 1 calc PR A 1 H38B H 0.2086 -0.1568 0.3972 0.114 Uiso 0.75 1 calc PR A 1 H38C H 0.1651 -0.0377 0.3861 0.114 Uiso 0.75 1 calc PR A 1 C39A C 0.1937(6) 0.0189(8) 0.5020(4) 0.072(2) Uiso 0.75 1 d P A 1 H39A H 0.1477 -0.0199 0.5072 0.086 Uiso 0.75 1 calc PR A 1 H39B H 0.1768 0.0858 0.4780 0.086 Uiso 0.75 1 calc PR A 1 H39C H 0.2281 0.0414 0.5398 0.086 Uiso 0.75 1 calc PR A 1 C40A C 0.2577(8) -0.1584(12) 0.5103(6) 0.112(4) Uiso 0.75 1 d P A 1 H40A H 0.2107 -0.1920 0.5167 0.134 Uiso 0.75 1 calc PR A 1 H40B H 0.2944 -0.1380 0.5476 0.134 Uiso 0.75 1 calc PR A 1 H40C H 0.2825 -0.2127 0.4906 0.134 Uiso 0.75 1 calc PR A 1 C38B C 0.2060(14) -0.1662(11) 0.4418(10) 0.095(3) Uiso 0.25 1 d PD A 2 H38D H 0.1594 -0.1920 0.4519 0.114 Uiso 0.25 1 calc PR A 2 H38E H 0.2470 -0.2235 0.4530 0.114 Uiso 0.25 1 calc PR A 2 H38F H 0.1926 -0.1534 0.4001 0.114 Uiso 0.25 1 calc PR A 2 C39B C 0.1693(10) 0.0320(15) 0.4601(10) 0.072(2) Uiso 0.25 1 d PD A 2 H39D H 0.1221 -0.0011 0.4663 0.086 Uiso 0.25 1 calc PR A 2 H39E H 0.1583 0.0556 0.4197 0.086 Uiso 0.25 1 calc PR A 2 H39F H 0.1854 0.0973 0.4854 0.086 Uiso 0.25 1 calc PR A 2 C40B C 0.2634(16) -0.078(2) 0.5395(4) 0.112(4) Uiso 0.25 1 d PD A 2 H40D H 0.2235 -0.1208 0.5510 0.134 Uiso 0.25 1 calc PR A 2 H40E H 0.2719 -0.0056 0.5601 0.134 Uiso 0.25 1 calc PR A 2 H40F H 0.3125 -0.1201 0.5491 0.134 Uiso 0.25 1 calc PR A 2 B B 0.4298(3) 0.2401(5) 0.4626(2) 0.0359(13) Uani 1 1 d . . . H1B H 0.4780 0.2327 0.4496 0.043 Uiso 1 1 calc R . . C10S C 0.245(3) -0.1994(15) 0.2362(14) 0.129(9) Uiso 0.50 1 d P . . H10A H 0.2931 -0.2266 0.2295 0.155 Uiso 0.50 1 calc PR . . H10B H 0.1996 -0.2329 0.2078 0.155 Uiso 0.50 1 calc PR . . H10C H 0.2438 -0.2206 0.2752 0.155 Uiso 0.50 1 calc PR . . C11S C 0.2408(14) -0.0732(17) 0.2304(7) 0.107(7) Uiso 0.50 1 d P . . C12S C 0.1765(12) -0.0072(18) 0.2388(9) 0.105(6) Uiso 0.50 1 d P . . H12S H 0.1318 -0.0449 0.2435 0.126 Uiso 0.50 1 calc PR . . C13S C 0.1784(13) 0.1228(19) 0.2402(10) 0.111(6) Uiso 0.50 1 d P . . H13S H 0.1371 0.1663 0.2467 0.134 Uiso 0.50 1 calc PR . . C14S C 0.243(2) 0.170(2) 0.2315(10) 0.143(10) Uiso 0.50 1 d P . . H14S H 0.2466 0.2495 0.2337 0.172 Uiso 0.50 1 calc PR . . C15S C 0.307(2) 0.111(3) 0.2193(15) 0.192(14) Uiso 0.50 1 d P . . H15S H 0.3496 0.1471 0.2110 0.230 Uiso 0.50 1 calc PR . . C16S C 0.2975(15) -0.019(2) 0.2209(11) 0.133(8) Uiso 0.50 1 d P . . H16S H 0.3385 -0.0624 0.2140 0.159 Uiso 0.50 1 calc PR . . 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 Sm 0.03204(15) 0.03659(15) 0.03660(14) 0.00085(11) 0.01603(10) 0.00209(12) Si1 0.0538(10) 0.0545(10) 0.0402(8) 0.0008(7) 0.0214(7) 0.0124(8) Si2 0.0411(9) 0.0737(13) 0.0618(10) 0.0122(8) 0.0285(8) 0.0035(8) N11 0.030(2) 0.038(2) 0.035(2) -0.0004(17) 0.0131(17) 0.0015(18) N12 0.032(2) 0.040(3) 0.037(2) -0.0009(17) 0.0138(18) 0.0000(17) N21 0.033(2) 0.036(2) 0.039(2) -0.0010(17) 0.0164(18) 0.0004(18) N22 0.034(2) 0.035(2) 0.033(2) -0.0016(16) 0.0120(17) 0.0015(17) N31 0.032(2) 0.036(2) 0.040(2) 0.0000(17) 0.0158(18) 0.0056(18) N32 0.035(2) 0.031(3) 0.053(3) 0.0012(18) 0.016(2) 0.0012(18) C1 0.047(3) 0.057(4) 0.035(3) 0.006(2) 0.019(2) 0.007(3) C2 0.057(4) 0.053(4) 0.046(3) -0.003(3) 0.015(3) -0.006(3) C3 0.104(6) 0.065(5) 0.088(5) 0.008(4) 0.036(5) 0.028(4) C4 0.079(5) 0.072(5) 0.062(4) -0.010(3) 0.031(4) 0.011(4) C5 0.045(4) 0.120(7) 0.070(4) 0.009(4) 0.032(3) 0.011(4) C6 0.067(5) 0.109(7) 0.120(7) -0.007(5) 0.055(5) -0.025(5) C7 0.061(5) 0.127(7) 0.102(6) 0.061(5) 0.043(4) 0.023(5) C13 0.033(3) 0.042(3) 0.038(3) 0.002(2) 0.008(2) 0.006(2) C14 0.031(3) 0.055(4) 0.046(3) -0.005(2) 0.007(2) 0.000(2) C15 0.029(3) 0.042(3) 0.048(3) -0.003(2) 0.012(2) -0.001(2) C16 0.036(3) 0.060(4) 0.065(4) -0.006(3) 0.026(3) -0.012(3) C17 0.042(3) 0.059(4) 0.038(3) 0.003(2) 0.012(2) 0.004(3) C18 0.060(4) 0.072(4) 0.043(3) 0.005(3) 0.023(3) -0.009(3) C19 0.063(4) 0.087(5) 0.042(3) -0.017(3) 0.020(3) -0.004(4) C20 0.062(4) 0.093(6) 0.050(4) 0.020(3) 0.014(3) 0.018(4) C23 0.041(3) 0.037(3) 0.031(2) -0.001(2) 0.012(2) 0.000(2) C24 0.041(3) 0.049(3) 0.040(3) 0.008(2) 0.014(2) 0.005(2) C25 0.036(3) 0.050(3) 0.033(3) 0.002(2) 0.019(2) -0.001(2) C26 0.049(4) 0.076(5) 0.049(3) 0.010(3) 0.027(3) 0.003(3) C27 0.037(3) 0.055(4) 0.029(3) 0.007(2) 0.010(2) 0.009(2) C28 0.034(3) 0.069(4) 0.052(3) 0.007(3) 0.014(3) 0.009(3) C29 0.059(4) 0.065(5) 0.113(6) 0.022(4) 0.039(4) 0.023(3) C30 0.044(4) 0.152(8) 0.036(3) 0.002(4) 0.000(3) 0.018(4) C33 0.038(3) 0.033(3) 0.056(3) -0.001(2) 0.012(2) -0.003(2) C34 0.048(3) 0.039(3) 0.063(4) -0.008(3) 0.018(3) 0.003(3) C35 0.047(3) 0.036(3) 0.042(3) 0.001(2) 0.015(2) 0.009(2) C36 0.049(3) 0.054(4) 0.054(3) -0.008(3) 0.022(3) 0.011(3) C37 0.059(4) 0.039(4) 0.109(6) 0.001(3) 0.036(4) -0.004(3) B 0.031(3) 0.045(4) 0.035(3) 0.000(2) 0.014(2) 0.003(2) _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 Sm N12 2.558(4) . ? Sm N32 2.579(4) . ? Sm N22 2.616(4) . ? Sm C1 2.667(5) . ? Si1 C1 1.825(6) . ? Si1 C4 1.883(6) . ? Si1 C2 1.892(6) . ? Si1 C3 1.904(7) . ? Si2 C1 1.818(5) . ? Si2 C6 1.829(8) . ? Si2 C7 1.868(7) . ? Si2 C5 1.882(7) . ? N11 C15 1.362(6) . ? N11 N12 1.386(5) . ? N11 B 1.546(7) . ? N12 C13 1.333(6) . ? N21 C25 1.351(6) . ? N21 N22 1.377(5) . ? N21 B 1.546(7) . ? N22 C23 1.348(6) . ? N31 C35 1.345(6) . ? N31 N32 1.375(5) . ? N31 B 1.556(7) . ? N32 C33 1.317(7) . ? C13 C14 1.403(7) . ? C13 C17 1.517(7) . ? C14 C15 1.384(7) . ? C15 C16 1.487(7) . ? C17 C18 1.518(8) . ? C17 C19 1.535(8) . ? C17 C20 1.537(8) . ? C23 C24 1.390(7) . ? C23 C27 1.512(7) . ? C24 C25 1.380(7) . ? C25 C26 1.512(7) . ? C27 C29 1.494(9) . ? C27 C30 1.518(7) . ? C27 C28 1.529(7) . ? C33 C34 1.394(8) . ? C33 C37 1.513(8) . ? C34 C35 1.368(8) . ? C35 C36 1.481(7) . ? C37 C39A 1.450(11) . ? C37 C40A 1.489(15) . ? C37 C38B 1.5400(10) . ? C37 C39B 1.5403(10) . ? C37 C40B 1.5404(10) . ? C37 C38A 1.610(13) . ? C10S C11S 1.51(2) . ? C11S C16S 1.28(3) . ? C11S C12S 1.45(3) . ? C12S C13S 1.55(3) . ? C13S C14S 1.35(3) . ? C14S C15S 1.44(4) . ? C15S C16S 1.55(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N12 Sm N32 72.27(13) . . ? N12 Sm N22 87.53(12) . . ? N32 Sm N22 74.87(12) . . ? N12 Sm C1 130.06(15) . . ? N32 Sm C1 144.22(16) . . ? N22 Sm C1 126.29(14) . . ? C1 Si1 C4 114.2(3) . . ? C1 Si1 C2 112.3(3) . . ? C4 Si1 C2 103.9(3) . . ? C1 Si1 C3 113.8(3) . . ? C4 Si1 C3 107.4(3) . . ? C2 Si1 C3 104.3(3) . . ? C1 Si2 C6 111.2(3) . . ? C1 Si2 C7 113.1(3) . . ? C6 Si2 C7 109.0(4) . . ? C1 Si2 C5 115.8(3) . . ? C6 Si2 C5 103.1(4) . . ? C7 Si2 C5 103.9(3) . . ? C15 N11 N12 109.5(4) . . ? C15 N11 B 126.2(4) . . ? N12 N11 B 123.7(4) . . ? C13 N12 N11 106.6(4) . . ? C13 N12 Sm 132.9(3) . . ? N11 N12 Sm 108.6(3) . . ? C25 N21 N22 109.5(4) . . ? C25 N21 B 127.6(4) . . ? N22 N21 B 122.4(4) . . ? C23 N22 N21 106.7(4) . . ? C23 N22 Sm 137.8(3) . . ? N21 N22 Sm 115.4(3) . . ? C35 N31 N32 110.1(4) . . ? C35 N31 B 127.6(4) . . ? N32 N31 B 122.2(4) . . ? C33 N32 N31 106.0(4) . . ? C33 N32 Sm 137.6(3) . . ? N31 N32 Sm 116.3(3) . . ? Si2 C1 Si1 119.5(3) . . ? Si2 C1 Sm 129.9(3) . . ? Si1 C1 Sm 100.0(2) . . ? N12 C13 C14 110.4(4) . . ? N12 C13 C17 121.9(5) . . ? C14 C13 C17 127.6(5) . . ? C15 C14 C13 105.8(4) . . ? N11 C15 C14 107.7(4) . . ? N11 C15 C16 123.2(5) . . ? C14 C15 C16 129.1(5) . . ? C13 C17 C18 110.9(4) . . ? C13 C17 C19 109.6(5) . . ? C18 C17 C19 109.3(5) . . ? C13 C17 C20 108.7(5) . . ? C18 C17 C20 109.2(5) . . ? C19 C17 C20 109.2(5) . . ? N22 C23 C24 109.5(4) . . ? N22 C23 C27 123.3(4) . . ? C24 C23 C27 127.2(4) . . ? C25 C24 C23 106.3(4) . . ? N21 C25 C24 107.9(4) . . ? N21 C25 C26 123.0(5) . . ? C24 C25 C26 129.1(5) . . ? C29 C27 C23 109.5(5) . . ? C29 C27 C30 109.5(6) . . ? C23 C27 C30 108.1(4) . . ? C29 C27 C28 109.3(5) . . ? C23 C27 C28 111.2(4) . . ? C30 C27 C28 109.1(5) . . ? N32 C33 C34 110.7(5) . . ? N32 C33 C37 120.6(5) . . ? C34 C33 C37 128.7(5) . . ? C35 C34 C33 105.6(5) . . ? N31 C35 C34 107.6(5) . . ? N31 C35 C36 125.2(5) . . ? C34 C35 C36 127.2(5) . . ? C39A C37 C40A 108.1(8) . . ? C39A C37 C33 114.6(6) . . ? C40A C37 C33 111.0(7) . . ? C33 C37 C38B 115.5(11) . . ? C33 C37 C39B 108.2(10) . . ? C38B C37 C39B 109.79(10) . . ? C33 C37 C40B 103.7(12) . . ? C38B C37 C40B 109.78(10) . . ? C39B C37 C40B 109.75(10) . . ? C39A C37 C38A 111.6(7) . . ? C40A C37 C38A 104.9(8) . . ? C33 C37 C38A 106.1(6) . . ? N21 B N11 112.1(4) . . ? N21 B N31 110.3(4) . . ? N11 B N31 112.3(4) . . ? C16S C11S C12S 117(2) . . ? C16S C11S C10S 120(3) . . ? C12S C11S C10S 123(2) . . ? C11S C12S C13S 122.1(19) . . ? C14S C13S C12S 115(2) . . ? C13S C14S C15S 126(3) . . ? C14S C15S C16S 113(3) . . ? C11S C16S C15S 127(3) . . ? 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 C15 N11 N12 C13 -1.5(5) . . . . ? B N11 N12 C13 170.4(4) . . . . ? C15 N11 N12 Sm 146.6(3) . . . . ? B N11 N12 Sm -41.4(5) . . . . ? N32 Sm N12 C13 -156.9(5) . . . . ? N22 Sm N12 C13 128.2(5) . . . . ? C1 Sm N12 C13 -9.4(5) . . . . ? N32 Sm N12 N11 66.7(3) . . . . ? N22 Sm N12 N11 -8.2(3) . . . . ? C1 Sm N12 N11 -145.7(3) . . . . ? C25 N21 N22 C23 0.1(5) . . . . ? B N21 N22 C23 -172.6(4) . . . . ? C25 N21 N22 Sm 177.7(3) . . . . ? B N21 N22 Sm 5.0(5) . . . . ? N12 Sm N22 C23 -158.2(5) . . . . ? N32 Sm N22 C23 129.5(5) . . . . ? C1 Sm N22 C23 -18.0(5) . . . . ? N12 Sm N22 N21 25.2(3) . . . . ? N32 Sm N22 N21 -47.1(3) . . . . ? C1 Sm N22 N21 165.3(3) . . . . ? C35 N31 N32 C33 0.5(5) . . . . ? B N31 N32 C33 176.9(4) . . . . ? C35 N31 N32 Sm 178.7(3) . . . . ? B N31 N32 Sm -4.9(5) . . . . ? N12 Sm N32 C33 132.1(5) . . . . ? N22 Sm N32 C33 -135.7(5) . . . . ? C1 Sm N32 C33 -3.3(7) . . . . ? N12 Sm N32 N31 -45.4(3) . . . . ? N22 Sm N32 N31 46.9(3) . . . . ? C1 Sm N32 N31 179.2(3) . . . . ? C6 Si2 C1 Si1 157.6(4) . . . . ? C7 Si2 C1 Si1 -79.3(5) . . . . ? C5 Si2 C1 Si1 40.4(5) . . . . ? C6 Si2 C1 Sm -65.3(5) . . . . ? C7 Si2 C1 Sm 57.7(5) . . . . ? C5 Si2 C1 Sm 177.5(3) . . . . ? C4 Si1 C1 Si2 35.5(5) . . . . ? C2 Si1 C1 Si2 153.5(3) . . . . ? C3 Si1 C1 Si2 -88.3(4) . . . . ? C4 Si1 C1 Sm -112.4(3) . . . . ? C2 Si1 C1 Sm 5.6(3) . . . . ? C3 Si1 C1 Sm 123.8(3) . . . . ? N12 Sm C1 Si2 -87.9(4) . . . . ? N32 Sm C1 Si2 31.2(5) . . . . ? N22 Sm C1 Si2 148.9(3) . . . . ? N12 Sm C1 Si1 55.1(3) . . . . ? N32 Sm C1 Si1 174.17(17) . . . . ? N22 Sm C1 Si1 -68.1(3) . . . . ? N11 N12 C13 C14 1.1(6) . . . . ? Sm N12 C13 C14 -135.9(4) . . . . ? N11 N12 C13 C17 -176.2(4) . . . . ? Sm N12 C13 C17 46.8(7) . . . . ? N12 C13 C14 C15 -0.2(6) . . . . ? C17 C13 C14 C15 176.8(5) . . . . ? N12 N11 C15 C14 1.4(5) . . . . ? B N11 C15 C14 -170.3(5) . . . . ? N12 N11 C15 C16 -178.1(5) . . . . ? B N11 C15 C16 10.2(8) . . . . ? C13 C14 C15 N11 -0.7(6) . . . . ? C13 C14 C15 C16 178.8(6) . . . . ? N12 C13 C17 C18 -6.1(7) . . . . ? C14 C13 C17 C18 177.1(5) . . . . ? N12 C13 C17 C19 -126.8(5) . . . . ? C14 C13 C17 C19 56.4(7) . . . . ? N12 C13 C17 C20 114.0(6) . . . . ? C14 C13 C17 C20 -62.8(8) . . . . ? N21 N22 C23 C24 -0.9(5) . . . . ? Sm N22 C23 C24 -177.7(4) . . . . ? N21 N22 C23 C27 -179.5(4) . . . . ? Sm N22 C23 C27 3.7(8) . . . . ? N22 C23 C24 C25 1.4(6) . . . . ? C27 C23 C24 C25 179.9(5) . . . . ? N22 N21 C25 C24 0.8(6) . . . . ? B N21 C25 C24 173.0(5) . . . . ? N22 N21 C25 C26 -179.9(5) . . . . ? B N21 C25 C26 -7.6(8) . . . . ? C23 C24 C25 N21 -1.3(6) . . . . ? C23 C24 C25 C26 179.4(6) . . . . ? N22 C23 C27 C29 107.0(6) . . . . ? C24 C23 C27 C29 -71.3(7) . . . . ? N22 C23 C27 C30 -133.7(6) . . . . ? C24 C23 C27 C30 48.0(8) . . . . ? N22 C23 C27 C28 -14.0(7) . . . . ? C24 C23 C27 C28 167.7(5) . . . . ? N31 N32 C33 C34 -0.2(6) . . . . ? Sm N32 C33 C34 -177.8(4) . . . . ? N31 N32 C33 C37 178.4(5) . . . . ? Sm N32 C33 C37 0.8(9) . . . . ? N32 C33 C34 C35 -0.2(7) . . . . ? C37 C33 C34 C35 -178.6(6) . . . . ? N32 N31 C35 C34 -0.6(6) . . . . ? B N31 C35 C34 -176.8(5) . . . . ? N32 N31 C35 C36 179.9(5) . . . . ? B N31 C35 C36 3.7(8) . . . . ? C33 C34 C35 N31 0.5(6) . . . . ? C33 C34 C35 C36 179.9(5) . . . . ? N32 C33 C37 C39A -3.0(9) . . . . ? C34 C33 C37 C39A 175.3(7) . . . . ? N32 C33 C37 C40A -125.9(8) . . . . ? C34 C33 C37 C40A 52.4(10) . . . . ? N32 C33 C37 C38B 161.6(10) . . . . ? C34 C33 C37 C38B -20.2(12) . . . . ? N32 C33 C37 C39B 38.1(11) . . . . ? C34 C33 C37 C39B -143.6(11) . . . . ? N32 C33 C37 C40B -78.4(10) . . . . ? C34 C33 C37 C40B 99.9(11) . . . . ? N32 C33 C37 C38A 120.7(7) . . . . ? C34 C33 C37 C38A -61.0(9) . . . . ? C25 N21 B N11 125.7(5) . . . . ? N22 N21 B N11 -62.9(6) . . . . ? C25 N21 B N31 -108.2(5) . . . . ? N22 N21 B N31 63.1(5) . . . . ? C15 N11 B N21 -96.9(5) . . . . ? N12 N11 B N21 92.6(5) . . . . ? C15 N11 B N31 138.2(5) . . . . ? N12 N11 B N31 -32.4(6) . . . . ? C35 N31 B N21 112.0(5) . . . . ? N32 N31 B N21 -63.8(5) . . . . ? C35 N31 B N11 -122.1(5) . . . . ? N32 N31 B N11 62.1(6) . . . . ? C16S C11S C12S C13S -4(3) . . . . ? C10S C11S C12S C13S 172(2) . . . . ? C11S C12S C13S C14S 2(3) . . . . ? C12S C13S C14S C15S 2(4) . . . . ? C13S C14S C15S C16S -4(4) . . . . ? C12S C11S C16S C15S 2(4) . . . . ? C10S C11S C16S C15S -174(3) . . . . ? C14S C15S C16S C11S 1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.976 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.105 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.250 0.168 0.250 492 136 ' ' 2 0.250 -0.169 0.750 492 135 ' ' _platon_squeeze_details ; Attempts to refine peaks of residual electron density as carbon atoms of a second full-occupancy molecule of solvent toluene were unsuccessful. The data were corrected for disordered electron density through use of the SQUEEZE procedure (Sluis, P. van der; Spek, A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON (Spek, A.L. Acta Crystallogr. 1990, A46, C34. PLATON - a multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands). A total solvent-accessible void volume of 983.5 cubic Angstroms with a total electron count of 271 (consistent with four molecules of solvent toluene, or one molecule per formula unit of the samarium complex) was found in the unit cell. ; # Attachment '- 5-Yb.cif' data_5-Yb _database_code_depnum_ccdc_archive 'CCDC 776647' #TrackingRef '- 5-Yb.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H59 B N6 Si2 Yb, 0.5(C4 H10 O)' _chemical_formula_sum 'C33 H64 B N6 O0.50 Si2 Yb' _chemical_formula_weight 792.93 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' 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' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.487(5) _cell_length_b 18.263(5) _cell_length_c 27.122(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.320(6) _cell_angle_gamma 90.00 _cell_volume 8160(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 430 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 23.28 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.291 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3288 _exptl_absorpt_coefficient_mu 2.380 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5353 _exptl_absorpt_correction_T_max 0.6475 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens PLATFORM diffractometer/SMART 1K CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15486 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 23.28 _reflns_number_total 5782 _reflns_number_gt 4962 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Siemens SMART (Siemens, 1994)' _computing_cell_refinement 'Siemens SMART (Siemens, 1994)' _computing_data_reduction 'Siemens SAINT (Siemens, 1994)' _computing_structure_solution 'SHELXS-86 (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^)+(0.0515P)^2^+17.9241P] 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 5782 _refine_ls_number_parameters 422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb Yb 0.196489(13) 0.076576(13) 0.137063(7) 0.03050(11) Uani 1 1 d . . . Si1 Si 0.26740(10) 0.19581(9) 0.22369(5) 0.0370(4) Uani 1 1 d . . . Si2 Si 0.24334(11) 0.04937(10) 0.28301(6) 0.0437(4) Uani 1 1 d . . . N11 N 0.2635(3) 0.0804(2) 0.02490(15) 0.0306(10) Uani 1 1 d . . . N12 N 0.2973(3) 0.0729(2) 0.07208(15) 0.0339(11) Uani 1 1 d . . . N21 N 0.1311(2) 0.1496(2) 0.04018(14) 0.0304(10) Uani 1 1 d . . . N22 N 0.0958(3) 0.1477(2) 0.08620(15) 0.0343(10) Uani 1 1 d . . . N31 N 0.1313(2) 0.0092(2) 0.03175(14) 0.0300(10) Uani 1 1 d . . . N32 N 0.1366(3) -0.0145(2) 0.08011(15) 0.0337(10) Uani 1 1 d . . . C1 C 0.2176(3) 0.1059(3) 0.22869(17) 0.0355(13) Uani 1 1 d . . . H1 H 0.1615 0.1218 0.2365 0.043 Uiso 1 1 calc R . . C2 C 0.2653(3) 0.2304(3) 0.15714(19) 0.0416(13) Uani 1 1 d . . . H2A H 0.2089 0.2344 0.1446 0.050 Uiso 1 1 calc R . . H2B H 0.2947 0.1959 0.1366 0.050 Uiso 1 1 calc R . . H2C H 0.2913 0.2786 0.1561 0.050 Uiso 1 1 calc R . . C3 C 0.2163(4) 0.2700(4) 0.2589(2) 0.0555(16) Uani 1 1 d . . . H3A H 0.2376 0.3178 0.2492 0.067 Uiso 1 1 calc R . . H3B H 0.2271 0.2626 0.2944 0.067 Uiso 1 1 calc R . . H3C H 0.1577 0.2683 0.2516 0.067 Uiso 1 1 calc R . . C4 C 0.3777(4) 0.1964(4) 0.2438(2) 0.0510(16) Uani 1 1 d . . . H4A H 0.4022 0.2429 0.2344 0.061 Uiso 1 1 calc R . . H4B H 0.4056 0.1559 0.2279 0.061 Uiso 1 1 calc R . . H4C H 0.3829 0.1906 0.2797 0.061 Uiso 1 1 calc R . . C5 C 0.1571(5) -0.0144(4) 0.2972(2) 0.072(2) Uani 1 1 d . . . H5A H 0.1668 -0.0356 0.3301 0.086 Uiso 1 1 calc R . . H5B H 0.1539 -0.0537 0.2726 0.086 Uiso 1 1 calc R . . H5C H 0.1060 0.0130 0.2962 0.086 Uiso 1 1 calc R . . C6 C 0.2630(4) 0.1012(4) 0.3429(2) 0.0570(17) Uani 1 1 d . . . H6A H 0.3097 0.1338 0.3396 0.068 Uiso 1 1 calc R . . H6B H 0.2745 0.0663 0.3698 0.068 Uiso 1 1 calc R . . H6C H 0.2150 0.1302 0.3503 0.068 Uiso 1 1 calc R . . C7 C 0.3350(5) -0.0102(4) 0.2767(2) 0.065(2) Uani 1 1 d . . . H7A H 0.3420 -0.0415 0.3060 0.078 Uiso 1 1 calc R . . H7B H 0.3832 0.0206 0.2737 0.078 Uiso 1 1 calc R . . H7C H 0.3277 -0.0409 0.2473 0.078 Uiso 1 1 calc R . . C13 C 0.3769(3) 0.0642(3) 0.06708(18) 0.0296(12) Uani 1 1 d . . . C14 C 0.3954(4) 0.0680(3) 0.0169(2) 0.0387(13) Uani 1 1 d . . . H14 H 0.4476 0.0646 0.0034 0.046 Uiso 1 1 calc R . . C15 C 0.3221(3) 0.0775(3) -0.00848(19) 0.0329(12) Uani 1 1 d . . . C16 C 0.3049(4) 0.0841(3) -0.0630(2) 0.0407(14) Uani 1 1 d . . . H16A H 0.2812 0.1322 -0.0704 0.049 Uiso 1 1 calc R . . H16B H 0.2667 0.0457 -0.0738 0.049 Uiso 1 1 calc R . . H16C H 0.3556 0.0786 -0.0803 0.049 Uiso 1 1 calc R . . C17 C 0.4374(3) 0.0540(3) 0.11068(19) 0.0389(13) Uani 1 1 d . . . C18 C 0.3941(4) 0.0252(4) 0.1558(2) 0.0544(17) Uani 1 1 d . . . H18A H 0.4340 0.0164 0.1829 0.065 Uiso 1 1 calc R . . H18B H 0.3662 -0.0207 0.1472 0.065 Uiso 1 1 calc R . . H18C H 0.3543 0.0614 0.1661 0.065 Uiso 1 1 calc R . . C19 C 0.5032(4) -0.0004(4) 0.0967(2) 0.0578(18) Uani 1 1 d . . . H19A H 0.5441 -0.0043 0.1239 0.069 Uiso 1 1 calc R . . H19B H 0.5291 0.0167 0.0670 0.069 Uiso 1 1 calc R . . H19C H 0.4786 -0.0485 0.0904 0.069 Uiso 1 1 calc R . . C20 C 0.4790(4) 0.1273(4) 0.1233(2) 0.0596(19) Uani 1 1 d . . . H20A H 0.5194 0.1201 0.1504 0.071 Uiso 1 1 calc R . . H20B H 0.4383 0.1628 0.1334 0.071 Uiso 1 1 calc R . . H20C H 0.5059 0.1458 0.0943 0.071 Uiso 1 1 calc R . . C23 C 0.0547(3) 0.2103(3) 0.08997(19) 0.0330(12) Uani 1 1 d . . . C24 C 0.0633(3) 0.2529(3) 0.0479(2) 0.0391(13) Uani 1 1 d . . . H24 H 0.0406 0.2999 0.0415 0.047 Uiso 1 1 calc R . . C25 C 0.1111(3) 0.2134(3) 0.01761(19) 0.0334(12) Uani 1 1 d . . . C26 C 0.1414(4) 0.2339(3) -0.03225(19) 0.0478(15) Uani 1 1 d . . . H26A H 0.1257 0.2845 -0.0400 0.057 Uiso 1 1 calc R . . H26B H 0.1175 0.2010 -0.0574 0.057 Uiso 1 1 calc R . . H26C H 0.2007 0.2296 -0.0317 0.057 Uiso 1 1 calc R . . C27 C 0.0021(3) 0.2273(4) 0.1334(2) 0.0439(14) Uani 1 1 d . . . C28 C -0.0842(4) 0.2428(4) 0.1135(2) 0.0608(19) Uani 1 1 d . . . H28A H -0.0839 0.2858 0.0919 0.073 Uiso 1 1 calc R . . H28B H -0.1194 0.2522 0.1410 0.073 Uiso 1 1 calc R . . H28C H -0.1046 0.2003 0.0947 0.073 Uiso 1 1 calc R . . C29 C 0.0339(5) 0.2961(4) 0.1607(3) 0.067(2) Uani 1 1 d . . . H29A H 0.0889 0.2869 0.1742 0.080 Uiso 1 1 calc R . . H29B H -0.0018 0.3078 0.1876 0.080 Uiso 1 1 calc R . . H29C H 0.0348 0.3373 0.1375 0.080 Uiso 1 1 calc R . . C30 C 0.0001(4) 0.1629(4) 0.1695(2) 0.0620(19) Uani 1 1 d . . . H30A H 0.0529 0.1587 0.1873 0.074 Uiso 1 1 calc R . . H30B H -0.0114 0.1176 0.1512 0.074 Uiso 1 1 calc R . . H30C H -0.0423 0.1712 0.1932 0.074 Uiso 1 1 calc R . . C33 C 0.1009(3) -0.0803(3) 0.0808(2) 0.0371(13) Uani 1 1 d . A . C34 C 0.0735(3) -0.1005(3) 0.03310(19) 0.0372(13) Uani 1 1 d . . . H34 H 0.0466 -0.1446 0.0235 0.045 Uiso 1 1 calc R . . C35 C 0.0938(3) -0.0427(3) 0.00296(19) 0.0344(12) Uani 1 1 d . . . C36 C 0.0811(4) -0.0362(3) -0.05207(18) 0.0413(14) Uani 1 1 d . . . H36A H 0.0433 -0.0743 -0.0640 0.050 Uiso 1 1 calc R . . H36B H 0.1332 -0.0423 -0.0678 0.050 Uiso 1 1 calc R . . H36C H 0.0586 0.0121 -0.0603 0.050 Uiso 1 1 calc R . . C37 C 0.0959(4) -0.1238(3) 0.1286(2) 0.0429(14) Uani 1 1 d . . . C38A C 0.0074(8) -0.1463(8) 0.1363(5) 0.064(3) Uiso 0.60 1 d P A 1 H38A H -0.0263 -0.1023 0.1387 0.077 Uiso 0.60 1 calc PR A 1 H38B H 0.0046 -0.1748 0.1668 0.077 Uiso 0.60 1 calc PR A 1 H38C H -0.0125 -0.1761 0.1083 0.077 Uiso 0.60 1 calc PR A 1 C39A C 0.1274(9) -0.0820(7) 0.1727(5) 0.058(3) Uiso 0.60 1 d P A 1 H39A H 0.0932 -0.0389 0.1775 0.070 Uiso 0.60 1 calc PR A 1 H39B H 0.1833 -0.0664 0.1676 0.070 Uiso 0.60 1 calc PR A 1 H39C H 0.1262 -0.1134 0.2020 0.070 Uiso 0.60 1 calc PR A 1 C40A C 0.1450(10) -0.1993(8) 0.1213(5) 0.068(4) Uiso 0.60 1 d P A 1 H40A H 0.2022 -0.1884 0.1160 0.081 Uiso 0.60 1 calc PR A 1 H40B H 0.1217 -0.2256 0.0926 0.081 Uiso 0.60 1 calc PR A 1 H40C H 0.1409 -0.2298 0.1508 0.081 Uiso 0.60 1 calc PR A 1 C38B C 0.0078(13) -0.1107(14) 0.1494(8) 0.075(6) Uiso 0.40 1 d P A 2 H38D H -0.0337 -0.1246 0.1243 0.090 Uiso 0.40 1 calc PR A 2 H38E H 0.0014 -0.0588 0.1578 0.090 Uiso 0.40 1 calc PR A 2 H38F H 0.0016 -0.1406 0.1791 0.090 Uiso 0.40 1 calc PR A 2 C39B C 0.1638(12) -0.0961(10) 0.1662(7) 0.053(4) Uiso 0.40 1 d P A 2 H39D H 0.1537 -0.0447 0.1744 0.064 Uiso 0.40 1 calc PR A 2 H39E H 0.2168 -0.1006 0.1515 0.064 Uiso 0.40 1 calc PR A 2 H39F H 0.1632 -0.1257 0.1963 0.064 Uiso 0.40 1 calc PR A 2 C40B C 0.1083(14) -0.2014(12) 0.1204(8) 0.066(6) Uiso 0.40 1 d P A 2 H40D H 0.0802 -0.2161 0.0894 0.079 Uiso 0.40 1 calc PR A 2 H40E H 0.0867 -0.2293 0.1478 0.079 Uiso 0.40 1 calc PR A 2 H40F H 0.1665 -0.2113 0.1184 0.079 Uiso 0.40 1 calc PR A 2 B B 0.1703(4) 0.0814(3) 0.0153(2) 0.0289(13) Uani 1 1 d . . . H1B H 0.1597 0.0861 -0.0211 0.035 Uiso 1 1 calc R . . O1S O 0.2416(15) 0.2387(10) 0.5081(8) 0.084(4) Uani 0.50 1 d P B -1 C1S C 0.287(3) 0.1850(19) 0.4878(14) 0.134(15) Uani 0.50 1 d P B -1 H1SA H 0.2592 0.1730 0.4557 0.161 Uiso 0.50 1 calc PR B -1 H1SB H 0.3391 0.2079 0.4801 0.161 Uiso 0.50 1 calc PR B -1 C2S C 0.303(2) 0.1270(17) 0.5072(15) 0.140(13) Uani 0.50 1 d P B -1 H2SA H 0.3400 0.0994 0.4865 0.167 Uiso 0.50 1 calc PR B -1 H2SB H 0.2537 0.0987 0.5114 0.167 Uiso 0.50 1 calc PR B -1 H2SC H 0.3304 0.1357 0.5396 0.167 Uiso 0.50 1 calc PR B -1 C3S C 0.2194(17) 0.296(2) 0.4920(12) 0.118(12) Uani 0.50 1 d P B -1 H3SA H 0.1907 0.2843 0.4602 0.142 Uiso 0.50 1 calc PR B -1 H3SB H 0.2697 0.3218 0.4835 0.142 Uiso 0.50 1 calc PR B -1 C4S C 0.168(2) 0.353(2) 0.5150(9) 0.130(12) Uani 0.50 1 d P B -1 H4SA H 0.1682 0.3974 0.4948 0.156 Uiso 0.50 1 calc PR B -1 H4SB H 0.1907 0.3641 0.5482 0.156 Uiso 0.50 1 calc PR B -1 H4SC H 0.1128 0.3347 0.5172 0.156 Uiso 0.50 1 calc PR B -1 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 Yb 0.03066(16) 0.03838(18) 0.02201(15) -0.00222(9) -0.00458(10) -0.00032(10) Si1 0.0426(9) 0.0433(9) 0.0247(7) -0.0045(6) -0.0031(6) -0.0008(7) Si2 0.0531(10) 0.0502(10) 0.0275(8) 0.0021(7) -0.0027(7) -0.0063(8) N11 0.036(3) 0.033(3) 0.022(2) -0.0027(17) -0.0056(19) 0.0015(19) N12 0.033(3) 0.046(3) 0.022(2) -0.0019(19) -0.0053(19) -0.002(2) N21 0.030(2) 0.040(3) 0.021(2) 0.0001(19) -0.0001(17) -0.0046(19) N22 0.034(2) 0.042(3) 0.027(2) -0.0055(19) -0.0038(18) -0.001(2) N31 0.030(2) 0.036(3) 0.024(2) -0.0005(18) -0.0060(18) 0.0007(19) N32 0.037(3) 0.038(3) 0.026(2) 0.0049(19) -0.0074(19) -0.002(2) C1 0.037(3) 0.050(3) 0.020(3) -0.002(2) -0.003(2) 0.003(3) C2 0.042(3) 0.050(4) 0.032(3) 0.000(3) -0.001(2) -0.003(3) C3 0.071(5) 0.057(4) 0.038(3) -0.004(3) 0.000(3) 0.006(4) C4 0.051(4) 0.066(4) 0.035(3) -0.008(3) -0.005(3) -0.004(3) C5 0.087(6) 0.082(6) 0.047(4) 0.010(4) 0.002(4) -0.030(4) C6 0.072(5) 0.068(5) 0.030(3) 0.007(3) -0.003(3) -0.001(4) C7 0.092(6) 0.061(5) 0.042(4) 0.009(3) -0.002(4) 0.012(4) C13 0.031(3) 0.030(3) 0.027(3) -0.008(2) -0.002(2) -0.002(2) C14 0.036(3) 0.047(4) 0.033(3) -0.005(2) 0.004(2) 0.002(3) C15 0.037(3) 0.037(3) 0.025(3) -0.003(2) 0.001(2) 0.004(2) C16 0.040(3) 0.050(4) 0.032(3) 0.000(3) 0.004(2) 0.003(3) C17 0.032(3) 0.058(4) 0.026(3) -0.011(3) -0.007(2) 0.006(3) C18 0.044(4) 0.079(5) 0.040(3) 0.000(3) -0.009(3) 0.008(3) C19 0.050(4) 0.078(5) 0.045(4) -0.006(3) -0.008(3) 0.023(4) C20 0.041(4) 0.080(5) 0.056(4) -0.016(4) -0.015(3) -0.001(3) C23 0.032(3) 0.034(3) 0.032(3) -0.003(2) -0.006(2) 0.002(2) C24 0.043(3) 0.033(3) 0.041(3) 0.002(2) -0.006(3) 0.006(2) C25 0.037(3) 0.031(3) 0.033(3) 0.001(2) 0.001(2) -0.003(2) C26 0.062(4) 0.051(4) 0.030(3) 0.009(3) 0.004(3) 0.002(3) C27 0.039(3) 0.051(4) 0.042(3) -0.003(3) 0.008(3) 0.010(3) C28 0.042(4) 0.085(5) 0.056(4) 0.008(4) 0.008(3) 0.014(4) C29 0.073(5) 0.073(5) 0.056(4) -0.026(4) 0.019(4) 0.003(4) C30 0.073(5) 0.078(5) 0.036(3) 0.003(3) 0.011(3) 0.017(4) C33 0.038(3) 0.036(3) 0.037(3) -0.001(2) -0.004(2) -0.001(3) C34 0.034(3) 0.040(3) 0.037(3) -0.006(3) -0.009(2) -0.003(3) C35 0.027(3) 0.042(3) 0.033(3) -0.004(2) -0.006(2) 0.003(2) C36 0.045(3) 0.049(4) 0.029(3) -0.004(3) -0.009(2) -0.001(3) C37 0.056(4) 0.035(3) 0.037(3) 0.006(2) -0.009(3) -0.005(3) B 0.035(3) 0.029(3) 0.023(3) 0.001(2) -0.003(2) -0.004(3) O1S 0.096(14) 0.042(13) 0.116(16) 0.018(9) 0.028(11) -0.016(9) C1S 0.20(3) 0.09(2) 0.12(3) -0.07(2) 0.02(2) 0.04(2) C2S 0.13(2) 0.08(2) 0.21(4) -0.03(2) 0.07(2) -0.067(19) C3S 0.089(16) 0.14(3) 0.12(3) -0.06(2) -0.042(16) 0.076(18) C4S 0.22(4) 0.10(2) 0.072(14) -0.023(15) 0.050(18) -0.01(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 Yb N32 2.451(4) . ? Yb N12 2.472(4) . ? Yb N22 2.482(4) . ? Yb C1 2.552(5) . ? Si1 C1 1.842(6) . ? Si1 C3 1.877(6) . ? Si1 C4 1.878(6) . ? Si1 C2 1.911(5) . ? Si2 C1 1.835(5) . ? Si2 C7 1.876(7) . ? Si2 C5 1.889(7) . ? Si2 C6 1.897(6) . ? N11 C15 1.351(7) . ? N11 N12 1.382(6) . ? N11 B 1.549(7) . ? N12 C13 1.334(7) . ? N21 C25 1.351(7) . ? N21 N22 1.399(6) . ? N21 B 1.568(7) . ? N22 C23 1.335(7) . ? N31 C35 1.360(7) . ? N31 N32 1.380(6) . ? N31 B 1.542(7) . ? N32 C33 1.338(7) . ? C13 C14 1.408(8) . ? C13 C17 1.527(7) . ? C14 C15 1.379(8) . ? C15 C16 1.498(7) . ? C17 C19 1.530(8) . ? C17 C18 1.535(8) . ? C17 C20 1.536(9) . ? C23 C24 1.394(8) . ? C23 C27 1.523(7) . ? C24 C25 1.365(8) . ? C25 C26 1.508(7) . ? C27 C28 1.528(8) . ? C27 C30 1.532(9) . ? C27 C29 1.538(9) . ? C33 C34 1.402(8) . ? C33 C37 1.526(8) . ? C34 C35 1.385(8) . ? C35 C36 1.503(7) . ? C37 C40B 1.45(2) . ? C37 C39A 1.494(13) . ? C37 C38A 1.538(14) . ? C37 C39B 1.567(18) . ? C37 C38B 1.60(2) . ? C37 C40A 1.616(15) . ? O1S C3S 1.19(4) . ? O1S C1S 1.36(4) . ? C1S C2S 1.21(5) . ? C3S C4S 1.49(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N32 Yb N12 78.31(14) . . ? N32 Yb N22 76.23(14) . . ? N12 Yb N22 94.12(14) . . ? N32 Yb C1 142.38(16) . . ? N12 Yb C1 129.09(16) . . ? N22 Yb C1 119.53(16) . . ? C1 Si1 C3 113.3(3) . . ? C1 Si1 C4 114.4(3) . . ? C3 Si1 C4 107.3(3) . . ? C1 Si1 C2 111.9(2) . . ? C3 Si1 C2 104.6(3) . . ? C4 Si1 C2 104.7(3) . . ? C1 Si2 C7 114.5(3) . . ? C1 Si2 C5 111.1(3) . . ? C7 Si2 C5 106.0(4) . . ? C1 Si2 C6 115.6(3) . . ? C7 Si2 C6 104.9(3) . . ? C5 Si2 C6 103.7(3) . . ? C15 N11 N12 110.1(4) . . ? C15 N11 B 128.3(4) . . ? N12 N11 B 121.1(4) . . ? C13 N12 N11 106.2(4) . . ? C13 N12 Yb 140.2(3) . . ? N11 N12 Yb 113.6(3) . . ? C25 N21 N22 108.8(4) . . ? C25 N21 B 126.0(4) . . ? N22 N21 B 123.9(4) . . ? C23 N22 N21 106.2(4) . . ? C23 N22 Yb 137.4(3) . . ? N21 N22 Yb 102.5(3) . . ? C35 N31 N32 109.7(4) . . ? C35 N31 B 128.0(4) . . ? N32 N31 B 122.1(4) . . ? C33 N32 N31 106.5(4) . . ? C33 N32 Yb 140.1(3) . . ? N31 N32 Yb 113.2(3) . . ? Si2 C1 Si1 118.1(3) . . ? Si2 C1 Yb 133.0(3) . . ? Si1 C1 Yb 99.2(2) . . ? N12 C13 C14 110.2(5) . . ? N12 C13 C17 123.4(5) . . ? C14 C13 C17 126.4(5) . . ? C15 C14 C13 105.6(5) . . ? N11 C15 C14 107.8(5) . . ? N11 C15 C16 123.1(5) . . ? C14 C15 C16 129.1(5) . . ? C13 C17 C19 109.6(4) . . ? C13 C17 C18 110.4(5) . . ? C19 C17 C18 109.4(5) . . ? C13 C17 C20 109.8(5) . . ? C19 C17 C20 107.9(5) . . ? C18 C17 C20 109.8(5) . . ? N22 C23 C24 110.2(5) . . ? N22 C23 C27 122.7(5) . . ? C24 C23 C27 126.9(5) . . ? C25 C24 C23 106.2(5) . . ? N21 C25 C24 108.6(5) . . ? N21 C25 C26 122.5(5) . . ? C24 C25 C26 128.9(5) . . ? C23 C27 C28 108.3(5) . . ? C23 C27 C30 111.4(5) . . ? C28 C27 C30 109.0(5) . . ? C23 C27 C29 110.2(5) . . ? C28 C27 C29 108.3(6) . . ? C30 C27 C29 109.6(5) . . ? N32 C33 C34 110.4(5) . . ? N32 C33 C37 121.2(5) . . ? C34 C33 C37 128.3(5) . . ? C35 C34 C33 105.5(5) . . ? N31 C35 C34 107.9(4) . . ? N31 C35 C36 123.9(5) . . ? C34 C35 C36 128.2(5) . . ? C40B C37 C33 111.4(10) . . ? C39A C37 C33 112.7(6) . . ? C39A C37 C38A 109.2(8) . . ? C33 C37 C38A 109.8(6) . . ? C40B C37 C39B 108.3(12) . . ? C33 C37 C39B 108.9(8) . . ? C40B C37 C38B 109.7(13) . . ? C33 C37 C38B 107.7(9) . . ? C39B C37 C38B 110.9(12) . . ? C39A C37 C40A 112.0(8) . . ? C33 C37 C40A 107.1(7) . . ? C38A C37 C40A 105.7(9) . . ? N31 B N11 111.3(4) . . ? N31 B N21 111.8(4) . . ? N11 B N21 111.2(4) . . ? C3S O1S C1S 131(3) . . ? C2S C1S O1S 125(5) . . ? O1S C3S C4S 129(4) . . ? 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 C15 N11 N12 C13 -1.0(5) . . . . ? B N11 N12 C13 172.0(4) . . . . ? C15 N11 N12 Yb -179.7(3) . . . . ? B N11 N12 Yb -6.8(5) . . . . ? N32 Yb N12 C13 -127.8(6) . . . . ? N22 Yb N12 C13 157.2(5) . . . . ? C1 Yb N12 C13 23.2(6) . . . . ? N32 Yb N12 N11 50.3(3) . . . . ? N22 Yb N12 N11 -24.7(3) . . . . ? C1 Yb N12 N11 -158.7(3) . . . . ? C25 N21 N22 C23 0.6(5) . . . . ? B N21 N22 C23 -167.2(4) . . . . ? C25 N21 N22 Yb -147.5(3) . . . . ? B N21 N22 Yb 44.8(5) . . . . ? N32 Yb N22 C23 158.5(5) . . . . ? N12 Yb N22 C23 -124.6(5) . . . . ? C1 Yb N22 C23 15.5(6) . . . . ? N32 Yb N22 N21 -70.1(3) . . . . ? N12 Yb N22 N21 6.8(3) . . . . ? C1 Yb N22 N21 146.9(3) . . . . ? C35 N31 N32 C33 -1.1(6) . . . . ? B N31 N32 C33 -176.3(5) . . . . ? C35 N31 N32 Yb -176.9(3) . . . . ? B N31 N32 Yb 7.9(5) . . . . ? N12 Yb N32 C33 135.7(6) . . . . ? N22 Yb N32 C33 -127.1(6) . . . . ? C1 Yb N32 C33 -6.2(7) . . . . ? N12 Yb N32 N31 -50.7(3) . . . . ? N22 Yb N32 N31 46.6(3) . . . . ? C1 Yb N32 N31 167.5(3) . . . . ? C7 Si2 C1 Si1 -86.6(4) . . . . ? C5 Si2 C1 Si1 153.4(4) . . . . ? C6 Si2 C1 Si1 35.5(5) . . . . ? C7 Si2 C1 Yb 51.6(5) . . . . ? C5 Si2 C1 Yb -68.5(5) . . . . ? C6 Si2 C1 Yb 173.7(4) . . . . ? C3 Si1 C1 Si2 -83.2(4) . . . . ? C4 Si1 C1 Si2 40.1(4) . . . . ? C2 Si1 C1 Si2 158.9(3) . . . . ? C3 Si1 C1 Yb 126.4(2) . . . . ? C4 Si1 C1 Yb -110.2(3) . . . . ? C2 Si1 C1 Yb 8.5(3) . . . . ? N32 Yb C1 Si2 40.1(5) . . . . ? N12 Yb C1 Si2 -88.7(4) . . . . ? N22 Yb C1 Si2 146.7(3) . . . . ? N32 Yb C1 Si1 -176.52(18) . . . . ? N12 Yb C1 Si1 54.7(3) . . . . ? N22 Yb C1 Si1 -69.8(3) . . . . ? N11 N12 C13 C14 1.5(6) . . . . ? Yb N12 C13 C14 179.7(4) . . . . ? N11 N12 C13 C17 180.0(5) . . . . ? Yb N12 C13 C17 -1.8(8) . . . . ? N12 C13 C14 C15 -1.5(6) . . . . ? C17 C13 C14 C15 -179.9(5) . . . . ? N12 N11 C15 C14 0.0(6) . . . . ? B N11 C15 C14 -172.3(5) . . . . ? N12 N11 C15 C16 -179.9(5) . . . . ? B N11 C15 C16 7.8(8) . . . . ? C13 C14 C15 N11 0.9(6) . . . . ? C13 C14 C15 C16 -179.2(5) . . . . ? N12 C13 C17 C19 142.9(6) . . . . ? C14 C13 C17 C19 -38.9(8) . . . . ? N12 C13 C17 C18 22.4(7) . . . . ? C14 C13 C17 C18 -159.4(5) . . . . ? N12 C13 C17 C20 -98.8(6) . . . . ? C14 C13 C17 C20 79.4(7) . . . . ? N21 N22 C23 C24 -0.7(6) . . . . ? Yb N22 C23 C24 129.6(5) . . . . ? N21 N22 C23 C27 175.4(5) . . . . ? Yb N22 C23 C27 -54.3(8) . . . . ? N22 C23 C24 C25 0.6(6) . . . . ? C27 C23 C24 C25 -175.3(5) . . . . ? N22 N21 C25 C24 -0.3(6) . . . . ? B N21 C25 C24 167.2(5) . . . . ? N22 N21 C25 C26 178.2(5) . . . . ? B N21 C25 C26 -14.4(8) . . . . ? C23 C24 C25 N21 -0.2(6) . . . . ? C23 C24 C25 C26 -178.5(5) . . . . ? N22 C23 C27 C28 -122.6(6) . . . . ? C24 C23 C27 C28 52.9(8) . . . . ? N22 C23 C27 C30 -2.7(8) . . . . ? C24 C23 C27 C30 172.7(6) . . . . ? N22 C23 C27 C29 119.2(6) . . . . ? C24 C23 C27 C29 -65.4(7) . . . . ? N31 N32 C33 C34 1.0(6) . . . . ? Yb N32 C33 C34 174.9(4) . . . . ? N31 N32 C33 C37 179.6(5) . . . . ? Yb N32 C33 C37 -6.5(9) . . . . ? N32 C33 C34 C35 -0.5(6) . . . . ? C37 C33 C34 C35 -179.0(6) . . . . ? N32 N31 C35 C34 0.8(6) . . . . ? B N31 C35 C34 175.7(5) . . . . ? N32 N31 C35 C36 -177.2(5) . . . . ? B N31 C35 C36 -2.4(8) . . . . ? C33 C34 C35 N31 -0.2(6) . . . . ? C33 C34 C35 C36 177.7(5) . . . . ? N32 C33 C37 C40B -141.2(11) . . . . ? C34 C33 C37 C40B 37.1(13) . . . . ? N32 C33 C37 C39A 5.2(10) . . . . ? C34 C33 C37 C39A -176.5(8) . . . . ? N32 C33 C37 C38A 127.2(8) . . . . ? C34 C33 C37 C38A -54.5(10) . . . . ? N32 C33 C37 C39B -21.9(10) . . . . ? C34 C33 C37 C39B 156.4(9) . . . . ? N32 C33 C37 C38B 98.4(11) . . . . ? C34 C33 C37 C38B -83.3(11) . . . . ? N32 C33 C37 C40A -118.5(8) . . . . ? C34 C33 C37 C40A 59.9(9) . . . . ? C35 N31 B N11 -113.2(5) . . . . ? N32 N31 B N11 61.1(6) . . . . ? C35 N31 B N21 121.8(5) . . . . ? N32 N31 B N21 -63.9(6) . . . . ? C15 N11 B N31 110.2(6) . . . . ? N12 N11 B N31 -61.3(6) . . . . ? C15 N11 B N21 -124.4(5) . . . . ? N12 N11 B N21 64.1(6) . . . . ? C25 N21 B N31 -137.5(5) . . . . ? N22 N21 B N31 28.1(6) . . . . ? C25 N21 B N11 97.4(6) . . . . ? N22 N21 B N11 -97.0(5) . . . . ? C3S O1S C1S C2S -177(4) . . . . ? C1S O1S C3S C4S 179(4) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.865 _refine_diff_density_min -2.362 _refine_diff_density_rms 0.125 # Attachment '- 6a-Yb.cif' data_6a-Yb _database_code_depnum_ccdc_archive 'CCDC 776648' #TrackingRef '- 6a-Yb.cif' _vrf_PLAT601_6a-Yb ; RESPONSE: The final difference Fourier map shows no peaks of residual electron density located in the aformentioned VOIDS that would warrant being modelled as cocrystallized solvent. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H59 B N6 O Si Yb' _chemical_formula_sum 'C32 H59 B N6 O Si Yb' _chemical_formula_weight 755.79 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' 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' Yb Yb -0.3850 5.5486 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9336(11) _cell_length_b 13.1957(13) _cell_length_c 14.0307(12) _cell_angle_alpha 83.721(7) _cell_angle_beta 71.087(8) _cell_angle_gamma 86.607(8) _cell_volume 1902.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.07 _cell_measurement_theta_max 12.31 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 2.519 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3776 _exptl_absorpt_correction_T_max 0.5604 _exptl_absorpt_process_details 'Bruker SHELXTL' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6962 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6660 _reflns_number_gt 5849 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Enraf-Nonius CAD4/PC (Enraf-Nonius, 1993)' _computing_cell_refinement 'Enraf-Nonius CAD4/PC (Enraf-Nonius, 1993)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SHELXS-86 (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^)+(0.0576P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6660 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Yb Yb 0.243452(17) 0.260433(12) 0.253586(13) 0.02406(8) Uani 1 1 d . . . Si Si 0.60375(13) 0.13395(9) 0.17417(10) 0.0334(3) Uani 1 1 d . . . O O 0.2320(3) 0.2543(2) 0.0803(2) 0.0384(8) Uani 1 1 d . . . N11 N -0.0210(3) 0.3909(2) 0.2833(3) 0.0274(8) Uani 1 1 d . . . N12 N 0.1071(3) 0.4164(2) 0.2382(3) 0.0262(7) Uani 1 1 d . . . N21 N -0.0640(3) 0.2057(2) 0.3644(3) 0.0264(8) Uani 1 1 d . . . N22 N 0.0479(4) 0.1552(2) 0.3117(3) 0.0293(8) Uani 1 1 d . . . N31 N 0.0127(3) 0.3342(2) 0.4532(3) 0.0269(8) Uani 1 1 d . . . N32 N 0.1388(3) 0.2983(3) 0.4348(3) 0.0281(8) Uani 1 1 d . . . C1 C 0.4870(4) 0.2407(3) 0.1964(4) 0.0321(10) Uani 1 1 d . . . H1A H 0.5140 0.2839 0.1321 0.039 Uiso 1 1 calc R . . H1B H 0.5114 0.2776 0.2442 0.039 Uiso 1 1 calc R . . C2 C 0.5721(5) 0.0303(4) 0.2819(4) 0.0478(13) Uani 1 1 d . . . H2A H 0.4832 0.0094 0.3008 0.057 Uiso 1 1 calc R . . H2B H 0.5871 0.0557 0.3394 0.057 Uiso 1 1 calc R . . H2C H 0.6298 -0.0277 0.2609 0.057 Uiso 1 1 calc R . . C3 C 0.6012(5) 0.0706(4) 0.0609(4) 0.0491(13) Uani 1 1 d . . . H3A H 0.5137 0.0509 0.0702 0.059 Uiso 1 1 calc R . . H3B H 0.6576 0.0104 0.0537 0.059 Uiso 1 1 calc R . . H3C H 0.6309 0.1177 0.0005 0.059 Uiso 1 1 calc R . . C4 C 0.7781(5) 0.1671(4) 0.1454(4) 0.0494(13) Uani 1 1 d . . . H4A H 0.7873 0.2004 0.2009 0.059 Uiso 1 1 calc R . . H4B H 0.8051 0.2127 0.0837 0.059 Uiso 1 1 calc R . . H4C H 0.8315 0.1053 0.1369 0.059 Uiso 1 1 calc R . . C5 C 0.3381(5) 0.2336(4) -0.0096(4) 0.0463(13) Uani 1 1 d . . . H5A H 0.3779 0.1664 0.0000 0.056 Uiso 1 1 calc R . . H5B H 0.4042 0.2854 -0.0254 0.056 Uiso 1 1 calc R . . C6 C 0.2787(7) 0.2367(5) -0.0936(4) 0.0600(17) Uani 1 1 d . . . H6A H 0.2811 0.3054 -0.1285 0.072 Uiso 1 1 calc R . . H6B H 0.3235 0.1888 -0.1430 0.072 Uiso 1 1 calc R . . C7 C 0.1411(6) 0.2054(5) -0.0377(5) 0.0577(16) Uani 1 1 d . . . H7A H 0.0824 0.2318 -0.0751 0.069 Uiso 1 1 calc R . . H7B H 0.1348 0.1310 -0.0252 0.069 Uiso 1 1 calc R . . C8 C 0.1125(5) 0.2539(4) 0.0593(4) 0.0437(12) Uani 1 1 d . . . H8A H 0.0784 0.3237 0.0521 0.052 Uiso 1 1 calc R . . H8B H 0.0483 0.2147 0.1144 0.052 Uiso 1 1 calc R . . C13 C 0.1085(4) 0.4921(3) 0.1658(3) 0.0286(9) Uani 1 1 d . . . C14 C -0.0165(5) 0.5141(3) 0.1632(3) 0.0348(11) Uani 1 1 d . . . H14 H -0.0415 0.5633 0.1189 0.042 Uiso 1 1 calc R . . C15 C -0.0965(5) 0.4490(3) 0.2389(3) 0.0312(10) Uani 1 1 d . . . C16 C -0.2403(5) 0.4400(4) 0.2705(4) 0.0433(12) Uani 1 1 d . . . H16A H -0.2776 0.4506 0.3416 0.052 Uiso 1 1 calc R . . H16B H -0.2611 0.3726 0.2599 0.052 Uiso 1 1 calc R . . H16C H -0.2754 0.4910 0.2306 0.052 Uiso 1 1 calc R . . C17 C 0.2310(5) 0.5449(3) 0.1010(3) 0.0358(11) Uani 1 1 d . . . C18 C 0.3479(5) 0.4995(4) 0.1278(4) 0.0447(12) Uani 1 1 d . . . H18A H 0.3586 0.4281 0.1157 0.054 Uiso 1 1 calc R . . H18B H 0.3352 0.5058 0.1986 0.054 Uiso 1 1 calc R . . H18C H 0.4246 0.5358 0.0862 0.054 Uiso 1 1 calc R . . C19 C 0.2500(5) 0.5364(4) -0.0106(4) 0.0467(13) Uani 1 1 d . . . H19A H 0.2602 0.4652 -0.0235 0.056 Uiso 1 1 calc R . . H19B H 0.3268 0.5726 -0.0521 0.056 Uiso 1 1 calc R . . H19C H 0.1752 0.5661 -0.0271 0.056 Uiso 1 1 calc R . . C20 C 0.2158(6) 0.6582(3) 0.1203(4) 0.0492(13) Uani 1 1 d . . . H20A H 0.1414 0.6880 0.1032 0.059 Uiso 1 1 calc R . . H20B H 0.2930 0.6937 0.0788 0.059 Uiso 1 1 calc R . . H20C H 0.2033 0.6642 0.1912 0.059 Uiso 1 1 calc R . . C23 C 0.0160(4) 0.0578(3) 0.3172(3) 0.0318(10) Uani 1 1 d . . . C24 C -0.1145(5) 0.0457(3) 0.3715(4) 0.0405(11) Uani 1 1 d . . . H24 H -0.1612 -0.0146 0.3849 0.049 Uiso 1 1 calc R . . C25 C -0.1606(4) 0.1392(3) 0.4011(4) 0.0346(10) Uani 1 1 d . . . C26 C -0.2948(5) 0.1694(4) 0.4623(5) 0.0524(14) Uani 1 1 d . . . H26A H -0.2917 0.2043 0.5187 0.063 Uiso 1 1 calc R . . H26B H -0.3462 0.1088 0.4876 0.063 Uiso 1 1 calc R . . H26C H -0.3336 0.2145 0.4201 0.063 Uiso 1 1 calc R . . C27 C 0.1115(5) -0.0234(3) 0.2692(4) 0.0397(11) Uani 1 1 d . . . C28 C 0.1093(7) -0.1114(4) 0.3487(5) 0.070(2) Uani 1 1 d . . . H28A H 0.0225 -0.1374 0.3769 0.085 Uiso 1 1 calc R . . H28B H 0.1355 -0.0878 0.4022 0.085 Uiso 1 1 calc R . . H28C H 0.1686 -0.1652 0.3180 0.085 Uiso 1 1 calc R . . C29 C 0.0723(7) -0.0612(5) 0.1844(5) 0.0682(18) Uani 1 1 d . . . H29A H -0.0145 -0.0874 0.2118 0.082 Uiso 1 1 calc R . . H29B H 0.1321 -0.1151 0.1545 0.082 Uiso 1 1 calc R . . H29C H 0.0745 -0.0053 0.1330 0.082 Uiso 1 1 calc R . . C30 C 0.2471(5) 0.0171(4) 0.2242(5) 0.0642(18) Uani 1 1 d . . . H30A H 0.2481 0.0731 0.1731 0.077 Uiso 1 1 calc R . . H30B H 0.3060 -0.0369 0.1935 0.077 Uiso 1 1 calc R . . H30C H 0.2739 0.0409 0.2772 0.077 Uiso 1 1 calc R . . C33 C 0.1711(4) 0.3142(3) 0.5156(3) 0.0279(9) Uani 1 1 d . . . C34 C 0.0677(5) 0.3602(3) 0.5857(3) 0.0324(10) Uani 1 1 d . . . H34 H 0.0657 0.3794 0.6488 0.039 Uiso 1 1 calc R . . C35 C -0.0298(4) 0.3720(3) 0.5444(3) 0.0291(9) Uani 1 1 d . . . C36 C -0.1642(5) 0.4167(3) 0.5878(4) 0.0372(11) Uani 1 1 d . . . H36A H -0.1867 0.4602 0.5353 0.045 Uiso 1 1 calc R . . H36B H -0.1669 0.4566 0.6426 0.045 Uiso 1 1 calc R . . H36C H -0.2253 0.3620 0.6133 0.045 Uiso 1 1 calc R . . C37 C 0.3023(5) 0.2830(3) 0.5244(4) 0.0336(10) Uani 1 1 d . . . C38 C 0.3992(5) 0.3677(4) 0.4721(5) 0.0506(14) Uani 1 1 d . . . H38A H 0.3692 0.4302 0.5038 0.061 Uiso 1 1 calc R . . H38B H 0.4064 0.3788 0.4010 0.061 Uiso 1 1 calc R . . H38C H 0.4832 0.3475 0.4785 0.061 Uiso 1 1 calc R . . C39 C 0.2938(6) 0.2638(5) 0.6357(4) 0.0576(16) Uani 1 1 d . . . H39A H 0.2324 0.2107 0.6689 0.069 Uiso 1 1 calc R . . H39B H 0.2655 0.3260 0.6684 0.069 Uiso 1 1 calc R . . H39C H 0.3782 0.2425 0.6405 0.069 Uiso 1 1 calc R . . C40 C 0.3510(5) 0.1838(4) 0.4741(4) 0.0399(11) Uani 1 1 d . . . H40A H 0.2904 0.1301 0.5071 0.048 Uiso 1 1 calc R . . H40B H 0.4351 0.1642 0.4806 0.048 Uiso 1 1 calc R . . H40C H 0.3582 0.1946 0.4030 0.048 Uiso 1 1 calc R . . B B -0.0670(5) 0.3193(3) 0.3836(4) 0.0275(10) Uani 1 1 d . . . H1 H -0.1579 0.3388 0.4193 0.033 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 Yb 0.02476(11) 0.02187(10) 0.02340(11) -0.00330(6) -0.00445(7) -0.00029(6) Si 0.0311(7) 0.0318(6) 0.0360(7) -0.0055(5) -0.0090(6) 0.0026(5) O 0.0359(18) 0.0483(19) 0.0350(18) -0.0132(15) -0.0148(15) 0.0043(15) N11 0.032(2) 0.0227(16) 0.0266(19) -0.0032(14) -0.0085(16) 0.0029(14) N12 0.0269(19) 0.0234(16) 0.0250(18) -0.0023(14) -0.0043(15) 0.0008(14) N21 0.0258(19) 0.0270(17) 0.0242(19) -0.0010(14) -0.0057(15) -0.0005(14) N22 0.032(2) 0.0221(16) 0.031(2) -0.0027(14) -0.0055(16) -0.0003(14) N31 0.0280(19) 0.0257(16) 0.0241(19) -0.0048(14) -0.0042(15) 0.0038(14) N32 0.0258(19) 0.0298(18) 0.0271(19) -0.0030(15) -0.0063(16) 0.0007(15) C1 0.027(2) 0.030(2) 0.035(3) -0.0022(18) -0.005(2) -0.0009(18) C2 0.050(3) 0.041(3) 0.054(3) 0.002(2) -0.021(3) 0.004(2) C3 0.044(3) 0.052(3) 0.050(3) -0.021(3) -0.010(3) 0.010(2) C4 0.034(3) 0.055(3) 0.057(4) -0.003(3) -0.015(3) 0.003(2) C5 0.047(3) 0.058(3) 0.033(3) -0.015(2) -0.009(2) 0.007(3) C6 0.085(5) 0.063(4) 0.033(3) -0.008(3) -0.021(3) 0.007(3) C7 0.074(4) 0.057(3) 0.060(4) -0.016(3) -0.043(4) 0.004(3) C8 0.043(3) 0.048(3) 0.046(3) -0.008(2) -0.021(3) 0.000(2) C13 0.038(3) 0.0222(19) 0.026(2) -0.0049(16) -0.0114(19) 0.0037(17) C14 0.050(3) 0.028(2) 0.027(2) -0.0013(18) -0.016(2) 0.009(2) C15 0.037(3) 0.026(2) 0.032(2) -0.0049(18) -0.014(2) 0.0046(18) C16 0.043(3) 0.048(3) 0.042(3) 0.000(2) -0.020(2) 0.008(2) C17 0.046(3) 0.027(2) 0.029(2) -0.0003(18) -0.006(2) -0.0022(19) C18 0.039(3) 0.042(3) 0.042(3) 0.007(2) -0.001(2) -0.006(2) C19 0.056(3) 0.049(3) 0.027(3) 0.003(2) -0.002(2) -0.011(2) C20 0.060(4) 0.028(2) 0.053(3) 0.002(2) -0.011(3) -0.008(2) C23 0.037(3) 0.025(2) 0.033(2) -0.0001(18) -0.011(2) -0.0048(18) C24 0.038(3) 0.030(2) 0.049(3) 0.001(2) -0.007(2) -0.012(2) C25 0.027(2) 0.040(2) 0.035(3) 0.000(2) -0.008(2) -0.0073(19) C26 0.030(3) 0.051(3) 0.067(4) -0.002(3) -0.002(3) -0.010(2) C27 0.045(3) 0.026(2) 0.046(3) -0.003(2) -0.011(2) -0.001(2) C28 0.090(5) 0.040(3) 0.070(4) 0.004(3) -0.016(4) 0.021(3) C29 0.077(5) 0.063(4) 0.070(4) -0.037(3) -0.023(4) 0.013(3) C30 0.047(3) 0.037(3) 0.101(5) -0.027(3) -0.008(3) 0.004(2) C33 0.032(2) 0.026(2) 0.024(2) -0.0001(16) -0.0074(19) -0.0023(17) C34 0.042(3) 0.036(2) 0.018(2) -0.0037(17) -0.0079(19) 0.002(2) C35 0.036(3) 0.0229(19) 0.026(2) -0.0016(17) -0.0067(19) -0.0014(17) C36 0.038(3) 0.036(2) 0.032(3) -0.011(2) -0.002(2) 0.006(2) C37 0.035(3) 0.035(2) 0.030(3) -0.0043(19) -0.011(2) 0.000(2) C38 0.038(3) 0.046(3) 0.071(4) -0.004(3) -0.021(3) -0.005(2) C39 0.057(4) 0.082(4) 0.042(3) -0.011(3) -0.027(3) 0.017(3) C40 0.030(3) 0.042(3) 0.045(3) 0.000(2) -0.010(2) 0.005(2) B 0.028(3) 0.024(2) 0.029(3) -0.0041(19) -0.007(2) 0.0006(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Yb N22 2.478(4) . ? Yb O 2.486(3) . ? Yb N12 2.500(3) . ? Yb N32 2.519(3) . ? Yb C1 2.526(4) . ? Si C1 1.826(4) . ? Si C2 1.881(5) . ? Si C3 1.883(5) . ? Si C4 1.884(5) . ? O C8 1.430(6) . ? O C5 1.449(6) . ? N11 C15 1.345(5) . ? N11 N12 1.382(5) . ? N11 B 1.559(6) . ? N12 C13 1.343(5) . ? N21 C25 1.344(6) . ? N21 N22 1.382(5) . ? N21 B 1.550(5) . ? N22 C23 1.340(5) . ? N31 C35 1.352(5) . ? N31 N32 1.382(5) . ? N31 B 1.539(6) . ? N32 C33 1.332(6) . ? C5 C6 1.515(8) . ? C6 C7 1.512(9) . ? C7 C8 1.500(7) . ? C13 C14 1.391(6) . ? C13 C17 1.513(6) . ? C14 C15 1.385(7) . ? C15 C16 1.498(7) . ? C17 C18 1.519(7) . ? C17 C19 1.527(6) . ? C17 C20 1.537(6) . ? C23 C24 1.391(7) . ? C23 C27 1.503(6) . ? C24 C25 1.361(6) . ? C25 C26 1.496(6) . ? C27 C28 1.515(7) . ? C27 C30 1.515(7) . ? C27 C29 1.528(8) . ? C33 C34 1.394(6) . ? C33 C37 1.509(6) . ? C34 C35 1.363(6) . ? C35 C36 1.507(6) . ? C37 C39 1.529(7) . ? C37 C38 1.538(7) . ? C37 C40 1.540(6) . ? 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 N22 Yb O 85.99(12) . . ? N22 Yb N12 90.09(11) . . ? O Yb N12 79.11(11) . . ? N22 Yb N32 76.56(11) . . ? O Yb N32 150.23(11) . . ? N12 Yb N32 77.01(11) . . ? N22 Yb C1 140.29(13) . . ? O Yb C1 93.31(13) . . ? N12 Yb C1 128.81(13) . . ? N32 Yb C1 115.54(14) . . ? C1 Si C2 114.3(2) . . ? C1 Si C3 110.4(2) . . ? C2 Si C3 105.8(3) . . ? C1 Si C4 115.9(2) . . ? C2 Si C4 105.0(2) . . ? C3 Si C4 104.5(3) . . ? C8 O C5 109.4(4) . . ? C8 O Yb 122.9(3) . . ? C5 O Yb 126.9(3) . . ? C15 N11 N12 110.4(4) . . ? C15 N11 B 126.7(4) . . ? N12 N11 B 121.9(3) . . ? C13 N12 N11 106.0(3) . . ? C13 N12 Yb 135.8(3) . . ? N11 N12 Yb 107.9(2) . . ? C25 N21 N22 109.5(3) . . ? C25 N21 B 127.6(4) . . ? N22 N21 B 122.6(3) . . ? C23 N22 N21 105.8(4) . . ? C23 N22 Yb 139.2(3) . . ? N21 N22 Yb 114.6(2) . . ? C35 N31 N32 109.5(3) . . ? C35 N31 B 127.2(4) . . ? N32 N31 B 122.9(3) . . ? C33 N32 N31 106.2(3) . . ? C33 N32 Yb 140.0(3) . . ? N31 N32 Yb 112.1(2) . . ? Si C1 Yb 135.8(2) . . ? O C5 C6 105.5(4) . . ? C7 C6 C5 103.0(5) . . ? C8 C7 C6 102.1(5) . . ? O C8 C7 106.6(4) . . ? N12 C13 C14 110.0(4) . . ? N12 C13 C17 122.7(4) . . ? C14 C13 C17 127.2(4) . . ? C15 C14 C13 106.2(4) . . ? N11 C15 C14 107.3(4) . . ? N11 C15 C16 123.4(4) . . ? C14 C15 C16 129.3(4) . . ? C13 C17 C18 111.3(4) . . ? C13 C17 C19 109.6(4) . . ? C18 C17 C19 110.1(4) . . ? C13 C17 C20 108.1(4) . . ? C18 C17 C20 108.8(4) . . ? C19 C17 C20 109.0(4) . . ? N22 C23 C24 110.1(4) . . ? N22 C23 C27 122.8(4) . . ? C24 C23 C27 127.0(4) . . ? C25 C24 C23 105.9(4) . . ? N21 C25 C24 108.6(4) . . ? N21 C25 C26 123.1(4) . . ? C24 C25 C26 128.4(4) . . ? C23 C27 C28 108.8(4) . . ? C23 C27 C30 111.6(4) . . ? C28 C27 C30 109.7(5) . . ? C23 C27 C29 109.1(4) . . ? C28 C27 C29 109.3(5) . . ? C30 C27 C29 108.3(5) . . ? N32 C33 C34 110.1(4) . . ? N32 C33 C37 121.9(4) . . ? C34 C33 C37 128.0(4) . . ? C35 C34 C33 106.3(4) . . ? N31 C35 C34 107.9(4) . . ? N31 C35 C36 123.0(4) . . ? C34 C35 C36 129.0(4) . . ? C33 C37 C39 110.1(4) . . ? C33 C37 C38 109.9(4) . . ? C39 C37 C38 109.4(5) . . ? C33 C37 C40 110.1(4) . . ? C39 C37 C40 108.2(4) . . ? C38 C37 C40 109.2(4) . . ? N31 B N21 110.5(3) . . ? N31 B N11 111.1(4) . . ? N21 B N11 112.4(3) . . ? 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 N22 Yb O C8 34.7(3) . . . . ? N12 Yb O C8 -56.1(3) . . . . ? N32 Yb O C8 -19.0(5) . . . . ? C1 Yb O C8 174.9(3) . . . . ? N22 Yb O C5 -134.1(4) . . . . ? N12 Yb O C5 135.0(4) . . . . ? N32 Yb O C5 172.2(3) . . . . ? C1 Yb O C5 6.1(4) . . . . ? C15 N11 N12 C13 0.5(4) . . . . ? B N11 N12 C13 -168.9(3) . . . . ? C15 N11 N12 Yb -150.6(3) . . . . ? B N11 N12 Yb 39.9(4) . . . . ? N22 Yb N12 C13 -127.7(4) . . . . ? O Yb N12 C13 -41.8(4) . . . . ? N32 Yb N12 C13 156.1(4) . . . . ? C1 Yb N12 C13 43.6(5) . . . . ? N22 Yb N12 N11 10.6(3) . . . . ? O Yb N12 N11 96.5(3) . . . . ? N32 Yb N12 N11 -65.6(2) . . . . ? C1 Yb N12 N11 -178.1(2) . . . . ? C25 N21 N22 C23 0.4(5) . . . . ? B N21 N22 C23 175.2(4) . . . . ? C25 N21 N22 Yb -173.7(3) . . . . ? B N21 N22 Yb 1.1(5) . . . . ? O Yb N22 C23 79.1(5) . . . . ? N12 Yb N22 C23 158.2(5) . . . . ? N32 Yb N22 C23 -125.2(5) . . . . ? C1 Yb N22 C23 -11.2(6) . . . . ? O Yb N22 N21 -109.6(3) . . . . ? N12 Yb N22 N21 -30.5(3) . . . . ? N32 Yb N22 N21 46.1(3) . . . . ? C1 Yb N22 N21 160.1(3) . . . . ? C35 N31 N32 C33 0.4(4) . . . . ? B N31 N32 C33 -172.9(4) . . . . ? C35 N31 N32 Yb -168.0(3) . . . . ? B N31 N32 Yb 18.6(4) . . . . ? N22 Yb N32 C33 141.3(4) . . . . ? O Yb N32 C33 -163.0(4) . . . . ? N12 Yb N32 C33 -125.5(4) . . . . ? C1 Yb N32 C33 1.6(5) . . . . ? N22 Yb N32 N31 -56.2(2) . . . . ? O Yb N32 N31 -0.4(4) . . . . ? N12 Yb N32 N31 37.1(2) . . . . ? C1 Yb N32 N31 164.1(2) . . . . ? C2 Si C1 Yb -50.6(4) . . . . ? C3 Si C1 Yb 68.4(4) . . . . ? C4 Si C1 Yb -173.0(3) . . . . ? N22 Yb C1 Si 3.0(5) . . . . ? O Yb C1 Si -84.7(3) . . . . ? N12 Yb C1 Si -163.4(3) . . . . ? N32 Yb C1 Si 102.9(3) . . . . ? C8 O C5 C6 8.8(6) . . . . ? Yb O C5 C6 178.8(3) . . . . ? O C5 C6 C7 -28.2(6) . . . . ? C5 C6 C7 C8 36.1(6) . . . . ? C5 O C8 C7 14.6(6) . . . . ? Yb O C8 C7 -155.9(3) . . . . ? C6 C7 C8 O -31.8(6) . . . . ? N11 N12 C13 C14 -0.8(4) . . . . ? Yb N12 C13 C14 138.0(3) . . . . ? N11 N12 C13 C17 177.5(4) . . . . ? Yb N12 C13 C17 -43.7(6) . . . . ? N12 C13 C14 C15 0.8(5) . . . . ? C17 C13 C14 C15 -177.4(4) . . . . ? N12 N11 C15 C14 0.0(5) . . . . ? B N11 C15 C14 168.8(4) . . . . ? N12 N11 C15 C16 -180.0(4) . . . . ? B N11 C15 C16 -11.1(7) . . . . ? C13 C14 C15 N11 -0.5(5) . . . . ? C13 C14 C15 C16 179.5(4) . . . . ? N12 C13 C17 C18 1.2(6) . . . . ? C14 C13 C17 C18 179.2(4) . . . . ? N12 C13 C17 C19 123.2(4) . . . . ? C14 C13 C17 C19 -58.8(6) . . . . ? N12 C13 C17 C20 -118.2(5) . . . . ? C14 C13 C17 C20 59.8(6) . . . . ? N21 N22 C23 C24 0.6(5) . . . . ? Yb N22 C23 C24 172.4(3) . . . . ? N21 N22 C23 C27 -179.9(4) . . . . ? Yb N22 C23 C27 -8.1(7) . . . . ? N22 C23 C24 C25 -1.4(6) . . . . ? C27 C23 C24 C25 179.1(5) . . . . ? N22 N21 C25 C24 -1.3(5) . . . . ? B N21 C25 C24 -175.8(4) . . . . ? N22 N21 C25 C26 179.8(5) . . . . ? B N21 C25 C26 5.3(7) . . . . ? C23 C24 C25 N21 1.6(6) . . . . ? C23 C24 C25 C26 -179.6(5) . . . . ? N22 C23 C27 C28 126.6(5) . . . . ? C24 C23 C27 C28 -53.9(7) . . . . ? N22 C23 C27 C30 5.4(7) . . . . ? C24 C23 C27 C30 -175.1(5) . . . . ? N22 C23 C27 C29 -114.2(5) . . . . ? C24 C23 C27 C29 65.2(7) . . . . ? N31 N32 C33 C34 -0.3(5) . . . . ? Yb N32 C33 C34 162.9(3) . . . . ? N31 N32 C33 C37 178.9(4) . . . . ? Yb N32 C33 C37 -17.9(7) . . . . ? N32 C33 C34 C35 0.1(5) . . . . ? C37 C33 C34 C35 -179.1(4) . . . . ? N32 N31 C35 C34 -0.4(5) . . . . ? B N31 C35 C34 172.6(4) . . . . ? N32 N31 C35 C36 -179.7(4) . . . . ? B N31 C35 C36 -6.7(6) . . . . ? C33 C34 C35 N31 0.2(5) . . . . ? C33 C34 C35 C36 179.4(4) . . . . ? N32 C33 C37 C39 -154.0(4) . . . . ? C34 C33 C37 C39 25.1(6) . . . . ? N32 C33 C37 C38 85.5(5) . . . . ? C34 C33 C37 C38 -95.4(6) . . . . ? N32 C33 C37 C40 -34.8(6) . . . . ? C34 C33 C37 C40 144.3(5) . . . . ? C35 N31 B N21 -120.4(4) . . . . ? N32 N31 B N21 51.7(5) . . . . ? C35 N31 B N11 114.1(4) . . . . ? N32 N31 B N11 -73.8(4) . . . . ? C25 N21 B N31 108.0(5) . . . . ? N22 N21 B N31 -65.8(5) . . . . ? C25 N21 B N11 -127.2(5) . . . . ? N22 N21 B N11 59.0(5) . . . . ? C15 N11 B N31 -133.7(4) . . . . ? N12 N11 B N31 33.9(5) . . . . ? C15 N11 B N21 101.8(5) . . . . ? N12 N11 B N21 -90.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.131 _refine_diff_density_min -1.428 _refine_diff_density_rms 0.109 data_1-Yb _database_code_depnum_ccdc_archive 'CCDC 795065' #TrackingRef '- 1-Yb.cif' _vrf_PLAT029_1-Yb ; RESPONSE: This CIF was transcribed from the original hardcopy report from the structure determination that was completed in 1993. The model was more than satisfactory for our purposes, and the refinement was conducted in a manner consistent with the common best practices of the time. Unfortunately re-refinement of the structure to address the checkCIF alerts is not possible. Although the original diffraction data files had been archived to tape, the media are no longer readable with modern equipment. ; _vrf_PLAT601_1-Yb ; RESPONSE: The residual electron density in the solvent-accessible voids was too diffusely distributed to be reliably modelled as even badly-disordered solvent. Unfortunately, tools such as SQUEEZE (for calculating the contribution of such badly-behaved solvent) were not available to us at the time. ; _vrf_CHEMW03_1-Yb ; RESPONSE: Errors in calculated vs. reported formula, molecular weight, density, and absorption coefficient would be inevitable since hydrogen atoms were not included in the final model. This was our practice at the time if some of the atoms in the model were badly behaved (particularly the THF carbons) and a satisfactory disorder model could not be obtained. ; _audit_creation_method 'hand-edited from a paper report produced in 1993' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H38 B I N6 O2 Yb' _chemical_formula_sum 'C23 H38 B I N6 O2 Yb' _chemical_formula_weight 741.35 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 n m a' _symmetry_space_group_name_Hall '-P 2ac 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.229(7) _cell_length_b 14.689(9) _cell_length_c 16.264(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3399(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 3.84 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; North, A.C.T.; Phillips, D.C.; Mathews, F.S. Acta Cryst. 1968. A24, 351. ; _diffrn_ambient_temperature 293(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 'Enraf-Nonius CAD4' _diffrn_measurement_method '\q-2\q scans' _diffrn_reflns_number 3373 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.0 _diffrn_reflns_theta_max 25.0 _reflns_number_total 3373 _reflns_number_gt 1578 _reflns_threshold_expression Fo>5\s(Fo) _computing_data_collection 'Enraf-Nonius CAD4/PC' _computing_cell_refinement 'Enraf-Nonius CAD4/PC' _computing_data_reduction ; B. A. Frenz & Associates Inc. (1983). SDP-Plus Structure Determination Package. College Station, Texas, USA, and Enraf-Nonius, Delft, The Netherlands. ; _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELX-76 (Sheldrick, 1976)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s(Fo^2^)+(0.0033Fo^2^]' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens notdet _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_number_reflns 3373 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_R_factor_all ? _refine_ls_R_factor_gt 0.073 _refine_ls_wR_factor_ref ? _refine_ls_wR_factor_gt 0.098 _refine_ls_goodness_of_fit_ref 1.93 _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? 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 Yb Yb 0.84193(8) 0.2500 0.07813(6) 0.046 Uani 1 2 d . . . I I 0.7069(2) 0.2500 0.2249(1) 0.098 Uani 1 2 d . . . O O 0.927(1) 0.1256(9) 0.1392(7) 0.077 Uani 1 1 d . . . N11 N 0.938(2) 0.2500 -0.113(1) 0.053 Uani 1 2 d . . . N12 N 0.969(2) 0.2500 -0.030(1) 0.062 Uani 1 2 d . . . N21 N 0.785(1) 0.164(1) -0.1073(8) 0.049 Uani 1 1 d . . . N22 N 0.776(1) 0.144(1) -0.0266(9) 0.067 Uani 1 1 d . . . C1 C 0.951(2) 0.114(1) 0.226(1) 0.079 Uani 1 1 d . . . C2 C 1.009(2) 0.032(2) 0.236(2) 0.114 Uani 1 1 d . . . C3 C 1.021(3) 0.003(2) 0.145(2) 0.159 Uani 1 1 d . . . C4 C 0.970(2) 0.051(2) 0.096(2) 0.123 Uani 1 1 d . . . C13 C 1.059(2) 0.2500 -0.029(2) 0.066 Uani 1 2 d . . . C14 C 1.092(2) 0.2500 -0.108(2) 0.058 Uani 1 2 d . . . C15 C 1.018(2) 0.2500 -0.161(1) 0.055 Uani 1 2 d . . . C16 C 1.011(3) 0.2500 -0.252(2) 0.076 Uani 1 2 d . . . C17 C 1.106(3) 0.2500 0.048(2) 0.104 Uani 1 2 d . . . C23 C 0.732(2) 0.061(2) -0.022(1) 0.090 Uani 1 1 d . . . C24 C 0.716(2) 0.030(1) -0.101(1) 0.082 Uani 1 1 d . . . C25 C 0.749(1) 0.093(1) -0.153(1) 0.061 Uani 1 1 d . . . C26 C 0.754(2) 0.091(1) -0.245(1) 0.073 Uani 1 1 d . . . C27 C 0.700(3) 0.024(2) 0.061(2) 0.159 Uani 1 1 d . . . B B 0.830(2) 0.2500 -0.141(1) 0.044 Uani 1 2 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Yb 0.0678(7) 0.0414(6) 0.0290(5) 0.0000 0.0013(6) 0.0000 I 0.084(2) 0.144(2) 0.065(1) 0.0000 0.025(1) 0.0000 O 0.14(1) 0.047(8) 0.045(7) 0.040(8) -0.014(7) -0.011(6) N11 0.08(2) 0.04(1) 0.04(1) 0.0000 0.03(1) 0.0000 N12 0.06(2) 0.10(2) 0.03(1) 0.0000 0.00(1) 0.0000 N21 0.08(1) 0.043(8) 0.026(6) -0.012(7) 0.005(6) -0.006(6) N22 0.12(1) 0.032(8) 0.048(9) -0.017(9) -0.007(9) 0.000(7) C1 0.12(2) 0.06(1) 0.06(1) 0.01(1) -0.02(1) 0.00(1) C2 0.15(2) 0.08(2) 0.12(2) 0.04(2) -0.02(2) 0.03(2) C3 0.25(4) 0.11(3) 0.12(2) 0.10(3) 0.01(3) 0.00(2) C4 0.18(3) 0.10(2) 0.09(2) 0.08(2) -0.01(2) -0.01(2) C13 0.06(2) 0.10(2) 0.03(1) 0.0000 0.01(1) 0.0000 C14 0.03(1) 0.09(2) 0.05(1) 0.0000 -0.01(1) 0.0000 C15 0.08(2) 0.05(2) 0.04(1) 0.0000 0.01(1) 0.0000 C16 0.11(2) 0.09(2) 0.03(1) 0.0000 0.00(1) 0.0000 C17 0.13(3) 0.10(3) 0.08(2) 0.0000 0.01(2) 0.0000 C23 0.16(2) 0.07(2) 0.04(1) -0.06(2) -0.02(1) 0.00(1) C24 0.14(2) 0.05(1) 0.06(1) -0.03(1) -0.03(1) 0.00(1) C25 0.09(1) 0.05(1) 0.05(1) -0.02(1) -0.02(1) 0.000(9) C26 0.12(2) 0.05(1) 0.04(1) -0.02(1) -0.02(1) -0.02(1) C27 0.32(5) 0.08(2) 0.07(2) -0.09(3) -0.01(2) 0.04(1) B 0.07(2) 0.04(1) 0.03(1) 0.0000 0.01(1) 0.0000 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 Yb I 3.065(2) . ? Yb O 2.40(1) . ? Yb N12 2.53(2) . ? Yb N22 2.49(1) . ? O C1 1.47(2) . ? O C4 1.44(3) . ? N11 N12 1.41(3) . ? N11 C15 1.39(3) . ? N11 B 1.60(4) . ? N12 C13 1.29(3) . ? N21 N22 1.35(2) . ? N21 C25 1.39(2) . ? N21 B 1.51(2) . ? N22 C23 1.37(2) . ? C1 C2 1.46(3) . ? C2 C3 1.55(5) . ? C3 C4 1.29(4) . ? C13 C14 1.36(4) . ? C13 C17 1.43(5) . ? C14 C15 1.37(3) . ? C15 C16 1.48(3) . ? C23 C24 1.38(3) . ? C23 C27 1.52(3) . ? C24 C25 1.35(3) . ? C25 C26 1.49(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 I Yb O 89.6(3) . . ? I Yb N12 173.1(5) . . ? O Yb N12 85.9(5) . . ? I Yb N22 107.3(4) . . ? O Yb N22 89.6(5) . . ? N12 Yb N22 77.9(6) . . ? O Yb O 99.0(7) . 7_565 ? N22 Yb O 161.2(5) . 7_565 ? N22 Yb N22 77.6(7) . 7_565 ? Yb O C1 127(1) . . ? Yb O C4 126(1) . . ? C1 O C4 106(2) . . ? N12 N11 C15 106(2) . . ? N12 N11 B 125(2) . . ? C15 N11 B 129(2) . . ? Yb N12 N11 116(1) . . ? Yb N12 C13 135(2) . . ? N11 N12 C13 109(2) . . ? N22 N21 C25 109(1) . . ? N22 N21 B 125(1) . . ? C25 N21 B 126(1) . . ? Yb N22 N21 119(1) . . ? Yb N22 C23 134(1) . . ? N21 N22 C23 107(1) . . ? O C1 C2 109(2) . . ? C1 C2 C3 101(2) . . ? C2 C3 C4 112(3) . . ? O C4 C3 111(2) . . ? N12 C13 C14 110(2) . . ? N12 C13 C17 119(3) . . ? C14 C13 C17 131(3) . . ? C13 C14 C15 109(2) . . ? N11 C15 C14 106(2) . . ? N11 C15 C16 121(3) . . ? C14 C15 C16 132(3) . . ? N22 C23 C24 109(2) . . ? N22 C23 C27 120(2) . . ? C24 C23 C27 131(2) . . ? C23 C24 C25 108(2) . . ? N21 C25 C24 108(2) . . ? N21 C25 C26 122(2) . . ? C24 C25 C26 130(2) . . ? N11 B N21 108(1) . . ? N21 B N21 112(2) . 7_565 ? _diffrn_reflns_theta_full 25.0 _diffrn_measured_fraction_theta_full ? _refine_diff_density_max 3.6 _refine_diff_density_min ?