# 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 _publ_contact_author_name 'Marc Visseaux' _publ_contact_author_email MARC.VISSEAUX@ENSC-LILLE.FR _publ_section_title ; Synthesis of samarium(II) borohydrides and their behaviour as initiators in styrene and ?-caprolactone polymerisation ; loop_ _publ_author_name 'Marc Visseaux' 'Fanny Bonnet' 'Florian Jaroschik' 'X.-F.Le Goff' 'Francois Nief' 'Louis Ricard' # Attachment '2010_Jaroschik_dalton.cif' #=============================================================================== data_fj189 _database_code_depnum_ccdc_archive 'CCDC 763184' #TrackingRef '2010_Jaroschik_dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H24 B2 O2 Sm' _chemical_formula_sum 'C8 H24 B2 O2 Sm' _chemical_formula_weight 324.24 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' O O 0.0106 0.0060 '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 'P21/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 4.342(1) _cell_length_b 7.978(1) _cell_length_c 18.689(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.009(1) _cell_angle_gamma 90.00 _cell_volume 647.40(17) _cell_formula_units_Z 2 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 806 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description plate _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 320 _exptl_absorpt_coefficient_mu 4.506 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4372 _exptl_absorpt_correction_T_max 0.7738 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4740 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0310 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.15 _diffrn_reflns_theta_max 30.03 _reflns_number_total 1845 _reflns_number_gt 1357 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0390P)^2^+2.2152P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0083(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 1845 _refine_ls_number_parameters 74 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0810 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 Sm1 Sm 0.0000 0.0000 0.0000 0.02127(14) Uani 1 2 d S . . O1 O 0.0029(8) 0.2069(4) -0.10413(16) 0.0293(7) Uani 1 1 d . . . C4 C -0.0091(13) 0.3877(6) -0.0995(3) 0.0352(11) Uani 1 1 d . . . H4A H 0.1599 0.4297 -0.0688 0.042 Uiso 1 1 calc R . . H4B H -0.2077 0.4239 -0.0786 0.042 Uiso 1 1 calc R . . C3 C 0.0238(19) 0.4542(7) -0.1736(3) 0.0481(16) Uani 1 1 d . . . H3A H -0.1346 0.5405 -0.1833 0.058 Uiso 1 1 calc R . . H3B H 0.2300 0.5047 -0.1804 0.058 Uiso 1 1 calc R . . C1 C 0.0280(17) 0.1580(6) -0.1775(3) 0.0471(14) Uani 1 1 d . . . H1A H -0.1300 0.0727 -0.1891 0.057 Uiso 1 1 calc R . . H1B H 0.2337 0.1092 -0.1867 0.057 Uiso 1 1 calc R . . C2 C -0.0176(14) 0.3080(6) -0.2217(3) 0.0413(12) Uani 1 1 d . . . H2A H -0.2269 0.3084 -0.2427 0.050 Uiso 1 1 calc R . . H2B H 0.1349 0.3112 -0.2610 0.050 Uiso 1 1 calc R . . B1 B 0.5000(12) 0.1876(7) 0.0685(3) 0.0259(9) Uani 1 1 d . . . H1 H 0.483(10) 0.195(8) 0.016(3) 0.031 Uiso 1 1 d . . . H2 H 0.659(12) 0.245(6) 0.086(3) 0.031 Uiso 1 1 d . . . H3 H 0.508(13) 0.054(7) 0.082(3) 0.031 Uiso 1 1 d . . . H4 H 0.319(12) 0.235(6) 0.086(3) 0.031 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.02663(19) 0.01787(17) 0.01929(17) 0.00168(11) 0.00108(10) 0.00004(11) O1 0.0445(18) 0.0203(13) 0.0231(14) 0.0022(12) 0.0026(13) 0.0005(13) C4 0.056(3) 0.0209(19) 0.028(2) -0.0012(18) 0.000(2) 0.006(2) C3 0.094(5) 0.022(2) 0.029(3) 0.003(2) 0.003(3) 0.001(3) C1 0.087(4) 0.027(2) 0.027(2) -0.0039(19) 0.000(3) 0.001(3) C2 0.070(4) 0.027(2) 0.027(2) 0.006(2) -0.001(2) -0.004(3) B1 0.022(2) 0.025(2) 0.031(2) -0.012(2) -0.0001(18) 0.0027(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 Sm1 O1 2.552(3) 3 ? Sm1 O1 2.552(3) . ? Sm1 B1 2.931(5) 3 ? Sm1 B1 2.931(5) . ? Sm1 B1 2.931(5) 3_655 ? Sm1 B1 2.931(5) 1_455 ? O1 C1 1.429(6) . ? O1 C4 1.446(5) . ? C4 C3 1.489(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C3 C2 1.484(7) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C1 C2 1.467(7) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? B1 Sm1 2.931(5) 1_655 ? B1 H1 1.00(5) . ? B1 H2 0.89(5) . ? B1 H3 1.09(6) . ? B1 H4 0.93(5) . ? 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 O1 Sm1 O1 180.00(13) 3 . ? O1 Sm1 B1 89.95(13) 3 3 ? O1 Sm1 B1 90.05(13) . 3 ? O1 Sm1 B1 90.05(13) 3 . ? O1 Sm1 B1 89.95(13) . . ? B1 Sm1 B1 180.0(2) 3 . ? O1 Sm1 B1 90.38(13) 3 3_655 ? O1 Sm1 B1 89.62(13) . 3_655 ? B1 Sm1 B1 95.57(14) 3 3_655 ? B1 Sm1 B1 84.43(14) . 3_655 ? O1 Sm1 B1 89.62(13) 3 1_455 ? O1 Sm1 B1 90.38(13) . 1_455 ? B1 Sm1 B1 84.43(14) 3 1_455 ? B1 Sm1 B1 95.57(14) . 1_455 ? B1 Sm1 B1 180.0(3) 3_655 1_455 ? C1 O1 C4 109.4(3) . . ? C1 O1 Sm1 123.8(3) . . ? C4 O1 Sm1 126.8(3) . . ? O1 C4 C3 107.3(4) . . ? O1 C4 H4A 110.3 . . ? C3 C4 H4A 110.3 . . ? O1 C4 H4B 110.3 . . ? C3 C4 H4B 110.3 . . ? H4A C4 H4B 108.5 . . ? C2 C3 C4 105.8(4) . . ? C2 C3 H3A 110.6 . . ? C4 C3 H3A 110.6 . . ? C2 C3 H3B 110.6 . . ? C4 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? O1 C1 C2 107.9(4) . . ? O1 C1 H1A 110.1 . . ? C2 C1 H1A 110.1 . . ? O1 C1 H1B 110.1 . . ? C2 C1 H1B 110.1 . . ? H1A C1 H1B 108.4 . . ? C1 C2 C3 106.5(4) . . ? C1 C2 H2A 110.4 . . ? C3 C2 H2A 110.4 . . ? C1 C2 H2B 110.4 . . ? C3 C2 H2B 110.4 . . ? H2A C2 H2B 108.6 . . ? Sm1 B1 Sm1 95.57(14) . 1_655 ? Sm1 B1 H1 63(3) . . ? Sm1 B1 H1 70(3) 1_655 . ? Sm1 B1 H2 175(3) . . ? Sm1 B1 H2 81(3) 1_655 . ? H1 B1 H2 113(4) . . ? Sm1 B1 H3 68(3) . . ? Sm1 B1 H3 65(3) 1_655 . ? H1 B1 H3 107(5) . . ? H2 B1 H3 113(4) . . ? Sm1 B1 H4 75(3) . . ? Sm1 B1 H4 171(3) 1_655 . ? H1 B1 H4 106(4) . . ? H2 B1 H4 108(4) . . ? H3 B1 H4 110(4) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.000 _refine_diff_density_min -0.821 _refine_diff_density_rms 0.137 #===END #compound 2 data_fj205 _database_code_depnum_ccdc_archive 'CCDC 763185' #TrackingRef '2010_Jaroschik_dalton.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H35 B O2 Sm' _chemical_formula_sum 'C18 H35 B O2 Sm' _chemical_formula_weight 444.62 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' O O 0.0106 0.0060 '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 'P21/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.129(1) _cell_length_b 13.423(1) _cell_length_c 14.753(1) _cell_angle_alpha 90.00 _cell_angle_beta 121.690(1) _cell_angle_gamma 90.00 _cell_volume 2043.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 2530 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 30.034 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.877 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5969 _exptl_absorpt_correction_T_max 0.6888 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _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 KappaCCD _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18388 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0397 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 30.03 _reflns_number_total 5958 _reflns_number_gt 4541 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0403P)^2^+0.4679P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5958 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0918 _refine_ls_wR_factor_gt 0.0768 _refine_ls_goodness_of_fit_ref 1.103 _refine_ls_restrained_S_all 1.103 _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 Sm1 Sm -0.185884(13) -0.006197(10) 0.358694(11) 0.02668(7) Uani 1 1 d . . . O1 O -0.1552(2) -0.03753(19) 0.19810(16) 0.0391(5) Uani 1 1 d . . . O2 O -0.2783(2) -0.18353(18) 0.28316(17) 0.0458(6) Uani 1 1 d . . . C1 C -0.4322(3) 0.0362(3) 0.3157(3) 0.0360(7) Uani 1 1 d . . . C2 C -0.4284(3) 0.0795(3) 0.2299(2) 0.0401(8) Uani 1 1 d . . . C3 C -0.3442(3) 0.1613(3) 0.2695(3) 0.0415(8) Uani 1 1 d . . . C4 C -0.2969(3) 0.1697(2) 0.3790(2) 0.0372(7) Uani 1 1 d . . . C5 C -0.3513(3) 0.0921(2) 0.4070(2) 0.0330(6) Uani 1 1 d . . . C6 C -0.5103(4) -0.0538(3) 0.3110(3) 0.0607(11) Uani 1 1 d . . . H6A H -0.4528 -0.1026 0.3645 0.091 Uiso 1 1 calc R . . H6B H -0.5516 -0.0839 0.2400 0.091 Uiso 1 1 calc R . . H6C H -0.5771 -0.0332 0.3256 0.091 Uiso 1 1 calc R . . C7 C -0.5078(4) 0.0480(4) 0.1143(3) 0.0718(14) Uani 1 1 d . . . H7A H -0.5503 -0.0158 0.1087 0.108 Uiso 1 1 calc R . . H7B H -0.4509 0.0408 0.0861 0.108 Uiso 1 1 calc R . . H7C H -0.5737 0.0987 0.0732 0.108 Uiso 1 1 calc R . . C8 C -0.3131(5) 0.2313(3) 0.2054(4) 0.0735(14) Uani 1 1 d . . . H8A H -0.3029 0.2992 0.2332 0.110 Uiso 1 1 calc R . . H8B H -0.3838 0.2299 0.1305 0.110 Uiso 1 1 calc R . . H8C H -0.2324 0.2102 0.2110 0.110 Uiso 1 1 calc R . . C9 C -0.2128(4) 0.2535(3) 0.4506(3) 0.0643(11) Uani 1 1 d . . . H9A H -0.1439 0.2676 0.4365 0.097 Uiso 1 1 calc R . . H9B H -0.1741 0.2338 0.5253 0.097 Uiso 1 1 calc R . . H9C H -0.2658 0.3133 0.4364 0.097 Uiso 1 1 calc R . . C10 C -0.3327(3) 0.0747(3) 0.5160(2) 0.0519(10) Uani 1 1 d . . . H10A H -0.4027 0.1074 0.5194 0.078 Uiso 1 1 calc R . . H10B H -0.2492 0.1025 0.5711 0.078 Uiso 1 1 calc R . . H10C H -0.3342 0.0030 0.5279 0.078 Uiso 1 1 calc R . . C11 C -0.1594(3) 0.0362(3) 0.1253(3) 0.0416(8) Uani 1 1 d . . . H11A H -0.1098 0.0963 0.1644 0.050 Uiso 1 1 calc R . . H11B H -0.2500 0.0559 0.0733 0.050 Uiso 1 1 calc R . . C12 C -0.0991(5) -0.0129(3) 0.0699(4) 0.0586(12) Uani 1 1 d . . . H12A H -0.0534 0.0363 0.0512 0.070 Uiso 1 1 calc R . . H12B H -0.1651 -0.0477 0.0044 0.070 Uiso 1 1 calc R . . C13 C -0.0053(5) -0.0857(4) 0.1524(4) 0.0957(18) Uani 1 1 d . . . H13A H 0.0079 -0.1441 0.1181 0.115 Uiso 1 1 calc R . . H13B H 0.0795 -0.0537 0.2005 0.115 Uiso 1 1 calc R . . C14 C -0.0661(4) -0.1152(3) 0.2103(3) 0.0563(10) Uani 1 1 d . . . H14A H -0.1131 -0.1788 0.1818 0.068 Uiso 1 1 calc R . . H14B H 0.0004 -0.1246 0.2867 0.068 Uiso 1 1 calc R . . C15 C -0.3681(4) -0.2113(3) 0.1745(3) 0.0544(10) Uani 1 1 d . . . H15A H -0.3652 -0.1629 0.1252 0.065 Uiso 1 1 calc R . . H15B H -0.4575 -0.2136 0.1601 0.065 Uiso 1 1 calc R . . C16 C -0.3258(4) -0.3142(3) 0.1605(3) 0.0660(12) Uani 1 1 d . . . H16A H -0.4013 -0.3592 0.1215 0.079 Uiso 1 1 calc R . . H16B H -0.2805 -0.3099 0.1210 0.079 Uiso 1 1 calc R . . C17 C -0.2356(5) -0.3505(4) 0.2726(4) 0.0927(16) Uani 1 1 d . . . H17A H -0.2611 -0.4177 0.2828 0.111 Uiso 1 1 calc R . . H17B H -0.1451 -0.3531 0.2894 0.111 Uiso 1 1 calc R . . C18 C -0.2495(6) -0.2754(3) 0.3407(4) 0.0900(17) Uani 1 1 d . . . H18A H -0.3206 -0.2942 0.3517 0.108 Uiso 1 1 calc R . . H18B H -0.1681 -0.2697 0.4111 0.108 Uiso 1 1 calc R . . B1 B -0.0600(3) -0.0995(3) 0.5651(3) 0.0375(8) Uani 1 1 d . . . H1 H -0.0216 -0.1183 0.5175 0.045 Uiso 1 1 d R . . H2 H -0.1625 -0.1280 0.5201 0.045 Uiso 1 1 d R . . H3 H 0.0035 -0.1378 0.6467 0.045 Uiso 1 1 d R . . H4 H -0.0606 -0.0137 0.5692 0.045 Uiso 1 1 d 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 Sm1 0.02749(10) 0.02906(10) 0.02475(9) -0.00090(6) 0.01458(7) -0.00057(6) O1 0.0504(13) 0.0390(13) 0.0384(12) 0.0016(11) 0.0306(11) 0.0034(11) O2 0.0605(15) 0.0321(13) 0.0433(13) -0.0067(10) 0.0263(11) -0.0080(11) C1 0.0297(15) 0.0356(18) 0.0478(18) -0.0071(15) 0.0238(14) -0.0009(13) C2 0.0347(17) 0.051(2) 0.0300(15) -0.0041(14) 0.0137(13) 0.0147(15) C3 0.053(2) 0.0343(19) 0.0508(19) 0.0135(15) 0.0370(17) 0.0171(16) C4 0.0396(17) 0.0294(17) 0.0475(18) -0.0069(14) 0.0262(14) 0.0011(13) C5 0.0387(16) 0.0335(17) 0.0347(15) -0.0026(13) 0.0246(13) 0.0032(13) C6 0.054(2) 0.051(3) 0.092(3) -0.024(2) 0.048(2) -0.017(2) C7 0.051(2) 0.115(4) 0.040(2) -0.014(2) 0.0181(18) 0.031(3) C8 0.118(4) 0.049(3) 0.100(3) 0.040(2) 0.089(3) 0.039(3) C9 0.065(3) 0.043(2) 0.097(3) -0.030(2) 0.050(2) -0.012(2) C10 0.058(2) 0.069(3) 0.0416(18) 0.0015(18) 0.0352(17) 0.008(2) C11 0.049(2) 0.048(2) 0.0343(16) 0.0023(16) 0.0262(15) 0.0012(17) C12 0.071(3) 0.073(3) 0.057(2) 0.0051(19) 0.051(2) 0.011(2) C13 0.120(4) 0.080(4) 0.142(4) 0.037(3) 0.106(4) 0.040(3) C14 0.067(3) 0.048(2) 0.066(2) 0.0040(19) 0.044(2) 0.015(2) C15 0.049(2) 0.050(2) 0.055(2) -0.0145(18) 0.0210(18) -0.0093(18) C16 0.072(3) 0.055(3) 0.088(3) -0.034(2) 0.054(3) -0.020(2) C17 0.073(3) 0.044(3) 0.119(4) -0.011(3) 0.022(3) 0.003(2) C18 0.138(5) 0.035(2) 0.069(3) 0.005(2) 0.035(3) -0.016(3) B1 0.040(2) 0.041(2) 0.0300(16) 0.0019(15) 0.0170(15) -0.0089(16) _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 Sm1 O2 2.618(2) . ? Sm1 O1 2.618(2) . ? Sm1 C1 2.768(3) . ? Sm1 C2 2.777(3) . ? Sm1 C5 2.789(3) . ? Sm1 C3 2.797(3) . ? Sm1 C4 2.811(3) . ? Sm1 B1 2.879(3) . ? Sm1 B1 2.941(4) 3_556 ? Sm1 H1 2.6107 . ? O1 C11 1.441(4) . ? O1 C14 1.443(4) . ? O2 C18 1.433(5) . ? O2 C15 1.435(4) . ? C1 C5 1.397(4) . ? C1 C2 1.415(4) . ? C1 C6 1.515(5) . ? C2 C3 1.402(5) . ? C2 C7 1.514(4) . ? C3 C4 1.406(4) . ? C3 C8 1.515(5) . ? C4 C5 1.406(4) . ? C4 C9 1.513(4) . ? C5 C10 1.521(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.506(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.509(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.446(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.525(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.507(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.495(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? B1 Sm1 2.941(4) 3_556 ? B1 H1 1.0569 . ? B1 H2 1.1247 . ? B1 H3 1.1541 . ? B1 H4 1.1545 . ? 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 O2 Sm1 O1 72.63(7) . . ? O2 Sm1 C1 85.41(9) . . ? O1 Sm1 C1 118.36(8) . . ? O2 Sm1 C2 91.28(9) . . ? O1 Sm1 C2 92.90(8) . . ? C1 Sm1 C2 29.56(9) . . ? O2 Sm1 C5 109.54(8) . . ? O1 Sm1 C5 140.40(8) . . ? C1 Sm1 C5 29.12(9) . . ? C2 Sm1 C5 48.16(8) . . ? O2 Sm1 C3 119.75(9) . . ? O1 Sm1 C3 95.29(8) . . ? C1 Sm1 C3 48.33(10) . . ? C2 Sm1 C3 29.13(10) . . ? C5 Sm1 C3 48.02(9) . . ? O2 Sm1 C4 133.40(8) . . ? O1 Sm1 C4 122.35(8) . . ? C1 Sm1 C4 48.08(10) . . ? C2 Sm1 C4 47.98(9) . . ? C5 Sm1 C4 29.07(9) . . ? C3 Sm1 C4 29.04(9) . . ? O2 Sm1 B1 85.71(9) . . ? O1 Sm1 B1 129.69(9) . . ? C1 Sm1 B1 103.93(10) . . ? C2 Sm1 B1 133.34(9) . . ? C5 Sm1 B1 89.37(10) . . ? C3 Sm1 B1 134.36(10) . . ? C4 Sm1 B1 105.70(10) . . ? O2 Sm1 B1 136.31(9) . 3_556 ? O1 Sm1 B1 79.97(8) . 3_556 ? C1 Sm1 B1 138.08(11) . 3_556 ? C2 Sm1 B1 123.97(11) . 3_556 ? C5 Sm1 B1 113.27(10) . 3_556 ? C3 Sm1 B1 95.71(11) . 3_556 ? C4 Sm1 B1 90.01(10) . 3_556 ? B1 Sm1 B1 86.43(10) . 3_556 ? O2 Sm1 H1 79.2 . . ? O1 Sm1 H1 108.4 . . ? C1 Sm1 H1 123.2 . . ? C2 Sm1 H1 152.5 . . ? C5 Sm1 H1 110.9 . . ? C3 Sm1 H1 153.8 . . ? C4 Sm1 H1 124.8 . . ? B1 Sm1 H1 21.5 . . ? B1 Sm1 H1 78.0 3_556 . ? C11 O1 C14 108.7(2) . . ? C11 O1 Sm1 126.7(2) . . ? C14 O1 Sm1 117.13(18) . . ? C18 O2 C15 104.1(3) . . ? C18 O2 Sm1 127.9(2) . . ? C15 O2 Sm1 128.0(2) . . ? C5 C1 C2 107.7(3) . . ? C5 C1 C6 125.3(3) . . ? C2 C1 C6 126.9(3) . . ? C5 C1 Sm1 76.26(17) . . ? C2 C1 Sm1 75.58(17) . . ? C6 C1 Sm1 114.9(2) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 C7 125.5(4) . . ? C1 C2 C7 126.4(4) . . ? C3 C2 Sm1 76.21(18) . . ? C1 C2 Sm1 74.86(17) . . ? C7 C2 Sm1 118.3(2) . . ? C2 C3 C4 108.0(3) . . ? C2 C3 C8 126.3(3) . . ? C4 C3 C8 125.6(4) . . ? C2 C3 Sm1 74.66(18) . . ? C4 C3 Sm1 76.06(18) . . ? C8 C3 Sm1 117.2(2) . . ? C5 C4 C3 107.9(3) . . ? C5 C4 C9 126.4(3) . . ? C3 C4 C9 125.5(3) . . ? C5 C4 Sm1 74.56(17) . . ? C3 C4 Sm1 74.90(18) . . ? C9 C4 Sm1 120.9(2) . . ? C1 C5 C4 108.4(3) . . ? C1 C5 C10 125.1(3) . . ? C4 C5 C10 126.4(3) . . ? C1 C5 Sm1 74.62(17) . . ? C4 C5 Sm1 76.37(16) . . ? C10 C5 Sm1 118.1(2) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O1 C11 C12 105.5(3) . . ? O1 C11 H11A 110.7 . . ? C12 C11 H11A 110.7 . . ? O1 C11 H11B 110.7 . . ? C12 C11 H11B 110.7 . . ? H11A C11 H11B 108.8 . . ? C11 C12 C13 102.8(3) . . ? C11 C12 H12A 111.2 . . ? C13 C12 H12A 111.2 . . ? C11 C12 H12B 111.2 . . ? C13 C12 H12B 111.2 . . ? H12A C12 H12B 109.1 . . ? C14 C13 C12 104.6(3) . . ? C14 C13 H13A 110.8 . . ? C12 C13 H13A 110.8 . . ? C14 C13 H13B 110.8 . . ? C12 C13 H13B 110.8 . . ? H13A C13 H13B 108.9 . . ? O1 C14 C13 108.0(3) . . ? O1 C14 H14A 110.1 . . ? C13 C14 H14A 110.1 . . ? O1 C14 H14B 110.1 . . ? C13 C14 H14B 110.1 . . ? H14A C14 H14B 108.4 . . ? O2 C15 C16 106.0(3) . . ? O2 C15 H15A 110.5 . . ? C16 C15 H15A 110.5 . . ? O2 C15 H15B 110.5 . . ? C16 C15 H15B 110.5 . . ? H15A C15 H15B 108.7 . . ? C17 C16 C15 104.2(3) . . ? C17 C16 H16A 110.9 . . ? C15 C16 H16A 110.9 . . ? C17 C16 H16B 110.9 . . ? C15 C16 H16B 110.9 . . ? H16A C16 H16B 108.9 . . ? C18 C17 C16 104.3(4) . . ? C18 C17 H17A 110.9 . . ? C16 C17 H17A 110.9 . . ? C18 C17 H17B 110.9 . . ? C16 C17 H17B 110.9 . . ? H17A C17 H17B 108.9 . . ? O2 C18 C17 105.1(4) . . ? O2 C18 H18A 110.7 . . ? C17 C18 H18A 110.7 . . ? O2 C18 H18B 110.7 . . ? C17 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? Sm1 B1 Sm1 93.57(10) . 3_556 ? Sm1 B1 H1 64.8 . . ? Sm1 B1 H1 69.9 3_556 . ? Sm1 B1 H2 73.5 . . ? Sm1 B1 H2 166.9 3_556 . ? H1 B1 H2 105.2 . . ? Sm1 B1 H3 171.7 . . ? Sm1 B1 H3 80.2 3_556 . ? H1 B1 H3 107.6 . . ? H2 B1 H3 112.9 . . ? Sm1 B1 H4 66.8 . . ? Sm1 B1 H4 62.1 3_556 . ? H1 B1 H4 106.8 . . ? H2 B1 H4 109.5 . . ? H3 B1 H4 114.1 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.614 _refine_diff_density_min -1.350 _refine_diff_density_rms 0.116 #===END