# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2000 # CCDC Number: 440/226 data_global _audit_creation_method SHELXL-97 # SUBMISSION DETAILS _publ_requested_journal 'New J. Chem. Lett.' _publ_contact_author_name 'Visseaux, Marc' _publ_contact_author_address ; Laboratoire de Synth\`ese et d'Electrosynth\`ese Organom\'etalliques (LSEO - UMR CNRS 5632) Universit\'e de Bourgogne Facult\'e des Sciences Mirande 9 Avenue Savary 21000 DIJON France ; _publ_contact_author_email mvisseau@u-bourgogne.fr _publ_contact_author_fax '0380396084' _publ_contact_author_phone '0380396061' _publ_contact_letter ; Please consider this CIF submission for publication in New J. Chem. Lett. ; # TITLE AND AUTHOR LIST _publ_section_title ; New base-free metallocenes of samarium and neodymium, an approach of the stereoelectronic control in organolanthanide chemistry. ; loop_ _publ_author_name _publ_author_address 'Visseaux, Marc' ; Laboratoire de Synth\`ese et d'Electrosynth\`ese Organom\'etalliques (LSEO - UMR CNRS 5632) Universit\'e de Bourgogne Facult\'e des Sciences Mirande 9 Avenue Savary 21000 DIJON France ; 'Barbier-Baudry, Denise'; Laboratoire de Synth\`ese et d'Electrosynth\`ese Organom\'etalliques (LSEO - UMR CNRS 5632) Universit\'e de Bourgogne Facult\'e des Sciences Mirande 9 Avenue Savary 21000 DIJON France ; 'Blacque, Olivier' ; Laboratoire de Synth\`ese et d'Electrosynth\`ese Organom\'etalliques (LSEO - UMR CNRS 5632) Universit\'e de Bourgogne Facult\'e des Sciences Mirande 9 Avenue Savary 21000 DIJON France ; 'Hafid, Abderafia' ; Laboratoire de Synth\`ese et d'Electrosynth\`ese Organom\'etalliques (LSEO - UMR CNRS 5632) Universit\'e de Bourgogne Facult\'e des Sciences Mirande 9 Avenue Savary 21000 DIJON France ; 'Richard, Philippe' ; Laboratoire de Synth\`ese et d'Electrosynth\`ese Organom\'etalliques (LSEO - UMR CNRS 5632) Universit\'e de Bourgogne Facult\'e des Sciences Mirande 9 Avenue Savary 21000 DIJON France ; 'Weber, Frank' ; FB Chemie der Universit\"at Erwin-Schr\"odinger Str. 67663 Kaiserslautern Germany ; ################################################################# data_(I) # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common 'complex 1' _chemical_formula_moiety 'C34 H58 Sm' _chemical_formula_sum 'C34 H58 Sm' _chemical_formula_weight 617.15 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' 'Sm' 'Sm' -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 33.672(2) _cell_length_b 12.3080(11) _cell_length_c 16.5000(13) _cell_angle_alpha 90.00 _cell_angle_beta 111.932(4) _cell_angle_gamma 90.00 _cell_volume 6343.3(9) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 13070 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 1.870 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? # EXPERIMENTAL DATA _diffrn_ambient_temperature 110(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 'Nonius KappaCCD' _diffrn_measurement_method Omega-scans _diffrn_reflns_number 6811 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.45 _computing_data_collection 'COLLECT (Nonius, 1998)' _computing_cell_refinement 'COLLECT (Nonius, 1998)' _computing_data_reduction ; DENZO and SCALEPACK (Otwinowski & Minor, 1997) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' # REFINEMENT DATA _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. ; _reflns_number_total 6811 _reflns_number_gt 2719 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0174P)^2^+21.9380P] 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 3257 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0341 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0635 _refine_ls_wR_factor_gt 0.0594 _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 # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sm Sm 0.131201(7) 0.246393(16) 0.196175(12) 0.01748(8) Uani 1 d . . . C1 C 0.07814(13) 0.1601(3) 0.2734(2) 0.0153(9) Uani 1 d . . . H1 H 0.0529 0.1985 0.2622 0.020 Uiso 1 calc R . . C2 C 0.08356(12) 0.0745(3) 0.2216(2) 0.0125(9) Uani 1 d . . . C3 C 0.12678(13) 0.0392(3) 0.2610(2) 0.0124(9) Uani 1 d . . . C4 C 0.14734(13) 0.1035(3) 0.3371(2) 0.0132(9) Uani 1 d . . . C5 C 0.11674(12) 0.1787(3) 0.3447(2) 0.0123(9) Uani 1 d . . . C6 C 0.07812(13) 0.3683(3) 0.0554(2) 0.0151(9) Uani 1 d . . . H6 H 0.0498 0.3450 0.0311 0.020 Uiso 1 calc R . . C7 C 0.11108(13) 0.3323(3) 0.0293(2) 0.0154(9) Uani 1 d . . . C8 C 0.14929(13) 0.3867(3) 0.0832(2) 0.0133(9) Uani 1 d . . . C9 C 0.13818(13) 0.4570(3) 0.1410(2) 0.0138(9) Uani 1 d . . . C10 C 0.09395(13) 0.4449(3) 0.1238(2) 0.0144(9) Uani 1 d . . . C11 C 0.04908(13) 0.0238(3) 0.1431(2) 0.0176(9) Uani 1 d . . . H11 H 0.0613 0.0105 0.0987 0.023 Uiso 1 calc R . . C12 C 0.01053(13) 0.0978(3) 0.1032(2) 0.0259(11) Uani 1 d . . . H12A H -0.0104 0.0623 0.0538 0.034 Uiso 1 calc R . . H12B H 0.0194 0.1643 0.0845 0.034 Uiso 1 calc R . . H12C H -0.0017 0.1135 0.1459 0.034 Uiso 1 calc R . . C13 C 0.03475(14) -0.0857(3) 0.1668(3) 0.0270(11) Uani 1 d . . . H13A H 0.0129 -0.1162 0.1161 0.035 Uiso 1 calc R . . H13B H 0.0236 -0.0752 0.2119 0.035 Uiso 1 calc R . . H13C H 0.0588 -0.1342 0.1873 0.035 Uiso 1 calc R . . C14 C 0.14556(13) -0.0555(3) 0.2285(2) 0.0164(9) Uani 1 d . . . H14 H 0.1227 -0.0820 0.1755 0.021 Uiso 1 calc R . . C15 C 0.18320(13) -0.0263(3) 0.2019(2) 0.0226(10) Uani 1 d . . . H15A H 0.1931 -0.0905 0.1823 0.029 Uiso 1 calc R . . H15B H 0.2060 0.0037 0.2512 0.029 Uiso 1 calc R . . H15C H 0.1741 0.0262 0.1556 0.029 Uiso 1 calc R . . C16 C 0.15729(14) -0.1509(3) 0.2933(3) 0.0254(11) Uani 1 d . . . H16A H 0.1691 -0.2090 0.2705 0.033 Uiso 1 calc R . . H16B H 0.1321 -0.1760 0.3016 0.033 Uiso 1 calc R . . H16C H 0.1780 -0.1273 0.3483 0.033 Uiso 1 calc R . . C17 C 0.19400(13) 0.0945(3) 0.3973(2) 0.0162(9) Uani 1 d . . . H17 H 0.2059 0.0327 0.3764 0.021 Uiso 1 calc R . . C18 C 0.20101(14) 0.0701(3) 0.4929(2) 0.0242(10) Uani 1 d . . . H18A H 0.2312 0.0657 0.5268 0.032 Uiso 1 calc R . . H18B H 0.1876 0.0023 0.4963 0.032 Uiso 1 calc R . . H18C H 0.1886 0.1272 0.5155 0.032 Uiso 1 calc R . . C19 C 0.22000(13) 0.1955(3) 0.3912(2) 0.0224(10) Uani 1 d . . . H19A H 0.2493 0.1869 0.4301 0.029 Uiso 1 calc R . . H19B H 0.2082 0.2591 0.4073 0.029 Uiso 1 calc R . . H19C H 0.2187 0.2032 0.3324 0.029 Uiso 1 calc R . . C20 C 0.12180(13) 0.2558(3) 0.4205(2) 0.0167(9) Uani 1 d . . . H20 H 0.1525 0.2677 0.4528 0.022 Uiso 1 calc R . . C21 C 0.10316(14) 0.2026(4) 0.4823(3) 0.0300(11) Uani 1 d . . . H21A H 0.1165 0.1333 0.5009 0.039 Uiso 1 calc R . . H21B H 0.0729 0.1927 0.4524 0.039 Uiso 1 calc R . . H21C H 0.1084 0.2484 0.5323 0.039 Uiso 1 calc R . . C22 C 0.10077(15) 0.3661(3) 0.3907(3) 0.0285(11) Uani 1 d . . . H22A H 0.1050 0.4110 0.4408 0.037 Uiso 1 calc R . . H22B H 0.0707 0.3563 0.3587 0.037 Uiso 1 calc R . . H22C H 0.1134 0.4004 0.3539 0.037 Uiso 1 calc R . . C23 C 0.10422(14) 0.2549(3) -0.0456(2) 0.0169(9) Uani 1 d . . . H23 H 0.1312 0.2503 -0.0552 0.022 Uiso 1 calc R . . C24 C 0.09250(14) 0.1400(3) -0.0272(3) 0.0274(11) Uani 1 d . . . H24A H 0.0886 0.0945 -0.0768 0.036 Uiso 1 calc R . . H24B H 0.0664 0.1422 -0.0164 0.036 Uiso 1 calc R . . H24C H 0.1151 0.1112 0.0231 0.036 Uiso 1 calc R . . C25 C 0.07001(15) 0.2989(4) -0.1298(2) 0.0312(12) Uani 1 d . . . H25A H 0.0661 0.2487 -0.1767 0.041 Uiso 1 calc R . . H25B H 0.0791 0.3679 -0.1440 0.041 Uiso 1 calc R . . H25C H 0.0435 0.3076 -0.1215 0.041 Uiso 1 calc R . . C26 C 0.19355(13) 0.3709(3) 0.0811(2) 0.0170(9) Uani 1 d . . . H26 H 0.2132 0.4146 0.1291 0.022 Uiso 1 calc R . . C27 C 0.19708(13) 0.4144(3) -0.0034(2) 0.0248(10) Uani 1 d . . . H27A H 0.2256 0.4028 -0.0015 0.032 Uiso 1 calc R . . H27B H 0.1908 0.4908 -0.0086 0.032 Uiso 1 calc R . . H27C H 0.1770 0.3768 -0.0527 0.032 Uiso 1 calc R . . C28 C 0.20959(15) 0.2531(3) 0.0986(3) 0.0265(11) Uani 1 d . . . H28A H 0.2376 0.2482 0.0965 0.034 Uiso 1 calc R . . H28B H 0.1903 0.2063 0.0549 0.034 Uiso 1 calc R . . H28C H 0.2108 0.2311 0.1553 0.034 Uiso 1 calc R . . C29 C 0.16781(13) 0.5330(3) 0.2097(2) 0.0192(10) Uani 1 d . . . H29 H 0.1495 0.5752 0.2323 0.025 Uiso 1 calc R . . C30 C 0.19080(13) 0.6161(3) 0.1725(3) 0.0238(10) Uani 1 d . . . H30A H 0.2089 0.6615 0.2189 0.031 Uiso 1 calc R . . H30B H 0.1699 0.6602 0.1293 0.031 Uiso 1 calc R . . H30C H 0.2079 0.5784 0.1461 0.031 Uiso 1 calc R . . C31 C 0.20012(14) 0.4731(3) 0.2883(2) 0.0253(10) Uani 1 d . . . H31A H 0.2178 0.5251 0.3293 0.033 Uiso 1 calc R . . H31B H 0.2177 0.4267 0.2688 0.033 Uiso 1 calc R . . H31C H 0.1850 0.4300 0.3160 0.033 Uiso 1 calc R . . C32 C 0.06714(13) 0.5096(3) 0.1633(2) 0.0169(9) Uani 1 d . . . H32 H 0.0838 0.5166 0.2260 0.022 Uiso 1 calc R . . C33 C 0.02502(13) 0.4534(4) 0.1526(3) 0.0244(10) Uani 1 d . . . H33A H 0.0094 0.4974 0.1785 0.032 Uiso 1 calc R . . H33B H 0.0309 0.3839 0.1811 0.032 Uiso 1 calc R . . H33C H 0.0083 0.4435 0.0916 0.032 Uiso 1 calc R . . C34 C 0.05825(14) 0.6244(3) 0.1250(3) 0.0260(11) Uani 1 d . . . H34A H 0.0413 0.6633 0.1510 0.034 Uiso 1 calc R . . H34B H 0.0430 0.6201 0.0629 0.034 Uiso 1 calc R . . H34C H 0.0849 0.6618 0.1370 0.034 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm 0.01610(13) 0.01938(16) 0.01705(13) 0.00291(9) 0.00628(10) 0.00011(11) C1 0.011(2) 0.022(2) 0.0116(19) 0.0036(17) 0.0038(17) 0.001(2) C2 0.010(2) 0.017(2) 0.0091(18) -0.0021(17) 0.0020(17) -0.0020(19) C3 0.014(2) 0.014(2) 0.0097(18) 0.0017(17) 0.0047(17) 0.000(2) C4 0.011(2) 0.016(2) 0.0106(18) 0.0009(17) 0.0010(17) -0.001(2) C5 0.013(2) 0.013(2) 0.0118(18) 0.0004(17) 0.0052(18) 0.000(2) C6 0.009(2) 0.023(2) 0.0115(18) 0.0004(18) 0.0013(17) -0.003(2) C7 0.015(2) 0.020(2) 0.0128(18) 0.0008(18) 0.0063(18) 0.003(2) C8 0.011(2) 0.019(2) 0.0105(18) 0.0025(17) 0.0046(17) -0.001(2) C9 0.012(2) 0.014(2) 0.0148(19) 0.0021(17) 0.0050(18) 0.002(2) C10 0.017(2) 0.017(2) 0.0083(18) 0.0010(17) 0.0034(18) 0.002(2) C11 0.012(2) 0.026(3) 0.0134(19) -0.0027(19) 0.0036(18) 0.000(2) C12 0.019(3) 0.033(3) 0.020(2) -0.010(2) 0.000(2) -0.007(2) C13 0.027(3) 0.028(3) 0.023(2) -0.002(2) 0.006(2) -0.010(2) C14 0.015(2) 0.021(2) 0.0122(19) -0.0018(18) 0.0038(18) -0.001(2) C15 0.021(3) 0.029(3) 0.018(2) -0.0045(19) 0.007(2) 0.004(2) C16 0.029(3) 0.017(2) 0.030(2) 0.000(2) 0.011(2) 0.003(2) C17 0.015(2) 0.016(2) 0.0133(18) -0.0030(18) 0.0003(18) 0.002(2) C18 0.023(3) 0.032(3) 0.015(2) 0.0019(19) 0.0036(19) 0.004(2) C19 0.014(2) 0.034(3) 0.017(2) -0.003(2) 0.0034(19) 0.002(2) C20 0.011(2) 0.021(2) 0.0158(19) -0.0055(17) 0.0016(18) -0.002(2) C21 0.032(3) 0.040(3) 0.022(2) -0.011(2) 0.014(2) -0.008(3) C22 0.031(3) 0.027(3) 0.023(2) -0.008(2) 0.004(2) 0.007(3) C23 0.014(2) 0.022(3) 0.0127(19) -0.0071(18) 0.0027(17) -0.001(2) C24 0.030(3) 0.026(3) 0.024(2) -0.006(2) 0.008(2) -0.008(2) C25 0.046(3) 0.027(3) 0.016(2) -0.002(2) 0.008(2) 0.005(3) C26 0.014(2) 0.023(2) 0.0157(19) -0.0009(18) 0.0071(18) -0.004(2) C27 0.021(3) 0.034(3) 0.022(2) -0.003(2) 0.011(2) -0.006(2) C28 0.021(3) 0.029(3) 0.031(2) -0.003(2) 0.012(2) 0.003(2) C29 0.018(2) 0.023(2) 0.015(2) -0.0035(19) 0.0045(19) -0.002(2) C30 0.021(3) 0.023(2) 0.025(2) -0.003(2) 0.006(2) -0.006(2) C31 0.027(3) 0.031(3) 0.016(2) -0.002(2) 0.006(2) -0.004(2) C32 0.015(2) 0.020(2) 0.016(2) -0.0007(18) 0.0051(19) 0.000(2) C33 0.021(3) 0.031(3) 0.027(2) 0.000(2) 0.014(2) 0.004(2) C34 0.029(3) 0.023(3) 0.027(2) 0.001(2) 0.011(2) 0.002(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 C1 2.765(4) . ? Sm C8 2.770(4) . ? Sm C2 2.779(4) . ? Sm C6 2.782(4) . ? Sm C9 2.786(4) . ? Sm C7 2.786(4) . ? Sm C3 2.791(4) . ? Sm C5 2.799(3) . ? Sm C4 2.802(3) . ? Sm C10 2.802(4) . ? C1 C5 1.408(5) . ? C1 C2 1.411(5) . ? C1 H1 0.9300 . ? C2 C3 1.422(5) . ? C2 C11 1.514(5) . ? C3 C4 1.426(5) . ? C3 C14 1.516(5) . ? C4 C5 1.425(5) . ? C4 C17 1.517(5) . ? C5 C20 1.528(5) . ? C6 C7 1.403(5) . ? C6 C10 1.414(5) . ? C6 H6 0.9300 . ? C7 C8 1.428(5) . ? C7 C23 1.509(5) . ? C8 C9 1.438(5) . ? C8 C26 1.516(5) . ? C9 C10 1.416(5) . ? C9 C29 1.519(5) . ? C10 C32 1.520(5) . ? C11 C12 1.520(6) . ? C11 C13 1.530(5) . ? C11 H11 0.9800 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.531(5) . ? C14 C16 1.537(5) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.534(5) . ? C17 C19 1.545(5) . ? C17 H17 0.9800 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C22 1.525(5) . ? C20 C21 1.530(5) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.529(5) . ? C23 C25 1.535(5) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C28 1.537(5) . ? C26 C27 1.540(5) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C31 1.535(5) . ? C29 C30 1.542(5) . ? C29 H29 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.528(5) . ? C32 C34 1.531(5) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sm C8 153.10(12) . . ? C1 Sm C2 29.49(10) . . ? C8 Sm C2 149.33(10) . . ? C1 Sm C6 105.54(11) . . ? C8 Sm C6 48.41(11) . . ? C2 Sm C6 108.02(11) . . ? C1 Sm C9 130.97(12) . . ? C8 Sm C9 29.98(10) . . ? C2 Sm C9 151.78(12) . . ? C6 Sm C9 48.08(11) . . ? C1 Sm C7 129.85(11) . . ? C8 Sm C7 29.77(11) . . ? C2 Sm C7 119.79(11) . . ? C6 Sm C7 29.19(10) . . ? C9 Sm C7 48.95(11) . . ? C1 Sm C3 48.42(11) . . ? C8 Sm C3 152.12(11) . . ? C2 Sm C3 29.59(10) . . ? C6 Sm C3 134.68(11) . . ? C9 Sm C3 176.79(10) . . ? C7 Sm C3 134.22(11) . . ? C1 Sm C5 29.32(10) . . ? C8 Sm C5 158.26(11) . . ? C2 Sm C5 48.87(10) . . ? C6 Sm C5 128.63(11) . . ? C9 Sm C5 128.80(11) . . ? C7 Sm C5 157.05(12) . . ? C3 Sm C5 48.75(10) . . ? C1 Sm C4 48.31(12) . . ? C8 Sm C4 157.87(12) . . ? C2 Sm C4 48.79(11) . . ? C6 Sm C4 153.69(12) . . ? C9 Sm C4 147.26(11) . . ? C7 Sm C4 163.41(11) . . ? C3 Sm C4 29.54(10) . . ? C5 Sm C4 29.49(10) . . ? C1 Sm C10 105.54(12) . . ? C8 Sm C10 49.13(11) . . ? C2 Sm C10 122.43(12) . . ? C6 Sm C10 29.33(10) . . ? C9 Sm C10 29.35(10) . . ? C7 Sm C10 48.93(10) . . ? C3 Sm C10 151.74(12) . . ? C5 Sm C10 115.87(11) . . ? C4 Sm C10 144.91(11) . . ? C5 C1 C2 109.9(3) . . ? C5 C1 Sm 76.7(2) . . ? C2 C1 Sm 75.8(2) . . ? C5 C1 H1 125.1 . . ? C2 C1 H1 125.1 . . ? Sm C1 H1 114.4 . . ? C1 C2 C3 107.0(3) . . ? C1 C2 C11 126.5(3) . . ? C3 C2 C11 126.3(3) . . ? C1 C2 Sm 74.7(2) . . ? C3 C2 Sm 75.6(2) . . ? C11 C2 Sm 119.1(2) . . ? C2 C3 C4 108.1(3) . . ? C2 C3 C14 124.3(3) . . ? C4 C3 C14 127.5(4) . . ? C2 C3 Sm 74.8(2) . . ? C4 C3 Sm 75.6(2) . . ? C14 C3 Sm 118.6(2) . . ? C3 C4 C5 108.0(3) . . ? C3 C4 C17 125.5(4) . . ? C5 C4 C17 126.5(3) . . ? C3 C4 Sm 74.8(2) . . ? C5 C4 Sm 75.1(2) . . ? C17 C4 Sm 115.0(2) . . ? C1 C5 C4 107.0(3) . . ? C1 C5 C20 124.8(3) . . ? C4 C5 C20 127.8(3) . . ? C1 C5 Sm 74.0(2) . . ? C4 C5 Sm 75.37(19) . . ? C20 C5 Sm 121.9(2) . . ? C7 C6 C10 110.5(4) . . ? C7 C6 Sm 75.6(2) . . ? C10 C6 Sm 76.1(2) . . ? C7 C6 H6 124.8 . . ? C10 C6 H6 124.8 . . ? Sm C6 H6 115.4 . . ? C6 C7 C8 107.0(3) . . ? C6 C7 C23 123.6(4) . . ? C8 C7 C23 129.3(3) . . ? C6 C7 Sm 75.2(2) . . ? C8 C7 Sm 74.5(2) . . ? C23 C7 Sm 118.4(2) . . ? C7 C8 C9 107.4(3) . . ? C7 C8 C26 126.2(3) . . ? C9 C8 C26 126.4(4) . . ? C7 C8 Sm 75.7(2) . . ? C9 C8 Sm 75.6(2) . . ? C26 C8 Sm 113.6(2) . . ? C10 C9 C8 108.6(3) . . ? C10 C9 C29 124.3(3) . . ? C8 C9 C29 127.2(4) . . ? C10 C9 Sm 75.9(2) . . ? C8 C9 Sm 74.4(2) . . ? C29 C9 Sm 116.2(2) . . ? C6 C10 C9 106.6(4) . . ? C6 C10 C32 125.7(4) . . ? C9 C10 C32 127.4(3) . . ? C6 C10 Sm 74.5(2) . . ? C9 C10 Sm 74.7(2) . . ? C32 C10 Sm 121.1(2) . . ? C2 C11 C12 112.4(3) . . ? C2 C11 C13 111.0(3) . . ? C12 C11 C13 109.8(3) . . ? C2 C11 H11 107.8 . . ? C12 C11 H11 107.8 . . ? C13 C11 H11 107.8 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C3 C14 C15 114.8(3) . . ? C3 C14 C16 112.0(3) . . ? C15 C14 C16 110.7(3) . . ? C3 C14 H14 106.2 . . ? C15 C14 H14 106.2 . . ? C16 C14 H14 106.2 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C4 C17 C18 114.4(3) . . ? C4 C17 C19 111.8(3) . . ? C18 C17 C19 110.6(3) . . ? C4 C17 H17 106.5 . . ? C18 C17 H17 106.5 . . ? C19 C17 H17 106.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C22 C20 C5 113.2(3) . . ? C22 C20 C21 109.8(3) . . ? C5 C20 C21 109.3(3) . . ? C22 C20 H20 108.1 . . ? C5 C20 H20 108.1 . . ? C21 C20 H20 108.1 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C7 C23 C24 113.2(3) . . ? C7 C23 C25 110.7(3) . . ? C24 C23 C25 110.1(3) . . ? C7 C23 H23 107.5 . . ? C24 C23 H23 107.5 . . ? C25 C23 H23 107.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C8 C26 C28 113.3(3) . . ? C8 C26 C27 112.6(3) . . ? C28 C26 C27 111.0(3) . . ? C8 C26 H26 106.4 . . ? C28 C26 H26 106.4 . . ? C27 C26 H26 106.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C9 C29 C31 113.3(3) . . ? C9 C29 C30 113.5(3) . . ? C31 C29 C30 110.6(3) . . ? C9 C29 H29 106.3 . . ? C31 C29 H29 106.3 . . ? C30 C29 H29 106.3 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C10 C32 C33 112.8(3) . . ? C10 C32 C34 111.3(3) . . ? C33 C32 C34 109.9(3) . . ? C10 C32 H32 107.5 . . ? C33 C32 H32 107.5 . . ? C34 C32 H32 107.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.215 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.215 _refine_diff_density_max 0.542 _refine_diff_density_min -0.585 _refine_diff_density_rms 0.061 #===END data_(II) # CHEMICAL DATA _chemical_name_common 'complex 2' _chemical_name_systematic ? _chemical_formula_moiety 'C25 H37 Sm' _chemical_formula_sum 'C25 H37 Sm' _chemical_formula_weight 487.90 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' '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 8.498(2) _cell_length_b 28.893(5) _cell_length_c 10.2650(10) _cell_angle_alpha 90.00 _cell_angle_beta 112.641(10) _cell_angle_gamma 90.00 _cell_volume 2326.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 26.3 _exptl_crystal_description 'flat prism' _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 996 _exptl_absorpt_coefficient_mu 2.530 _exptl_absorpt_correction_type 'psi-scan' _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 20 _diffrn_reflns_number 4895 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 26.31 _reflns_number_total 4638 _reflns_number_gt 2972 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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_details 'calc w=1/[\s^2^(Fo^2^)+(0.0623P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4638 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0423 _refine_ls_wR_factor_all 0.1103 _refine_ls_wR_factor_ref 0.1004 _refine_ls_goodness_of_fit_all 0.989 _refine_ls_goodness_of_fit_ref 1.140 _refine_ls_restrained_S_all 0.989 _refine_ls_restrained_S_obs 1.140 _refine_ls_shift/su_max 0.004 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sm1 Sm 0.07320(4) 0.843156(10) 0.28842(3) 0.05892(13) Uani 1 d . . C1 C 0.0974(6) 0.9008(2) 0.0931(5) 0.0532(13) Uani 1 d . . H1 H 0.1979(6) 0.8990(2) 0.0774(5) 0.069 Uiso 1 calc R . C2 C -0.0510(6) 0.8740(2) 0.0215(5) 0.0492(12) Uani 1 d . . C3 C -0.1715(6) 0.8873(2) 0.0767(5) 0.0525(12) Uani 1 d . . C4 C -0.0997(7) 0.9215(2) 0.1806(6) 0.0570(13) Uani 1 d . . C5 C 0.0705(7) 0.9304(2) 0.1902(6) 0.0562(13) Uani 1 d . . C6 C -0.0763(7) 0.8409(2) -0.0992(5) 0.0617(15) Uani 1 d . . H6 H -0.1507(7) 0.8158(2) -0.0930(5) 0.080 Uiso 1 calc R . C7 C 0.0876(8) 0.8193(2) -0.0963(7) 0.080(2) Uani 1 d . . H7A H 0.0625(8) 0.7989(2) -0.1754(7) 0.104 Uiso 1 calc R . H7B H 0.1407(8) 0.8022(2) -0.0102(7) 0.104 Uiso 1 calc R . H7C H 0.1633(8) 0.8433(2) -0.1014(7) 0.104 Uiso 1 calc R . C8 C -0.1655(10) 0.8652(3) -0.2393(6) 0.103(3) Uani 1 d . . H8A H -0.1808(10) 0.8440(3) -0.3151(6) 0.134 Uiso 1 calc R . H8B H -0.0975(10) 0.8909(3) -0.2462(6) 0.134 Uiso 1 calc R . H8C H -0.2747(10) 0.8763(3) -0.2454(6) 0.134 Uiso 1 calc R . C9 C -0.3539(7) 0.8673(2) 0.0209(6) 0.068(2) Uani 1 d . . H9 H -0.3534(7) 0.8447(2) -0.0502(6) 0.089 Uiso 1 calc R . C10 C -0.3989(9) 0.8395(2) 0.1210(8) 0.093(2) Uani 1 d . . H10A H -0.3077(9) 0.8184(2) 0.1694(8) 0.121 Uiso 1 calc R . H10B H -0.5011(9) 0.8223(2) 0.0708(8) 0.121 Uiso 1 calc R . H10C H -0.4174(9) 0.8595(2) 0.1883(8) 0.121 Uiso 1 calc R . C11 C -0.4858(7) 0.9019(2) -0.0626(7) 0.089(2) Uani 1 d . . H11A H -0.4456(7) 0.9184(2) -0.1250(7) 0.115 Uiso 1 calc R . H11B H -0.5062(7) 0.9233(2) 0.0006(7) 0.115 Uiso 1 calc R . H11C H -0.5899(7) 0.8861(2) -0.1170(7) 0.115 Uiso 1 calc R . C12 C -0.1904(10) 0.9462(2) 0.2629(8) 0.087(2) Uani 1 d . . H12 H -0.3033(10) 0.9317(2) 0.2273(8) 0.113 Uiso 1 calc R . C13 C -0.1239(10) 0.9356(3) 0.4161(7) 0.108(3) Uani 1 d . . H13A H -0.1028(10) 0.9030(3) 0.4301(7) 0.140 Uiso 1 calc R . H13B H -0.2064(10) 0.9448(3) 0.4539(7) 0.140 Uiso 1 calc R . H13C H -0.0196(10) 0.9523(3) 0.4634(7) 0.140 Uiso 1 calc R . C14 C -0.2294(11) 0.9956(2) 0.2243(10) 0.114(3) Uani 1 d . . H14A H -0.2713(11) 0.9988(2) 0.1235(10) 0.149 Uiso 1 calc R . H14B H -0.1277(11) 1.0137(2) 0.2669(10) 0.149 Uiso 1 calc R . H14C H -0.3145(11) 1.0061(2) 0.2574(10) 0.149 Uiso 1 calc R . C15 C 0.1959(8) 0.9660(2) 0.2765(7) 0.075(2) Uani 1 d . . H15 H 0.1505(8) 0.9802(2) 0.3415(7) 0.097 Uiso 1 calc R . C16 C 0.3669(11) 0.9478(3) 0.3601(11) 0.167(5) Uani 1 d . . H16A H 0.3581(11) 0.9237(3) 0.4212(11) 0.217 Uiso 1 calc R . H16B H 0.4372(11) 0.9723(3) 0.4159(11) 0.217 Uiso 1 calc R . H16C H 0.4169(11) 0.9356(3) 0.2979(11) 0.217 Uiso 1 calc R . C17 C 0.2181(13) 1.0032(3) 0.1844(11) 0.171(5) Uani 1 d . . H17A H 0.1089(13) 1.0161(3) 0.1278(11) 0.223 Uiso 1 calc R . H17B H 0.2697(13) 0.9905(3) 0.1240(11) 0.223 Uiso 1 calc R . H17C H 0.2901(13) 1.0271(3) 0.2420(11) 0.223 Uiso 1 calc R . C18 C 0.3009(21) 0.7834(5) 0.3019(15) 0.139(5) Uani 1 d . . H18 H 0.3648(21) 0.7779(5) 0.2475(15) 0.180 Uiso 1 calc R . C19 C 0.1477(24) 0.7592(4) 0.2548(11) 0.130(4) Uani 1 d . . H19 H 0.1339(24) 0.7407(4) 0.1770(11) 0.169 Uiso 1 calc R . C20 C 0.0150(19) 0.7561(3) 0.2942(13) 0.133(4) Uani 1 d . . H20 H -0.0696(19) 0.7367(3) 0.2350(13) 0.173 Uiso 1 calc R . C21 C -0.0276(14) 0.7739(5) 0.3977(16) 0.132(4) Uani 1 d . . H21 H -0.1320(14) 0.7630(5) 0.3944(16) 0.171 Uiso 1 calc R . C22 C 0.0467(19) 0.8042(5) 0.5060(13) 0.126(4) Uani 1 d . . H22 H -0.0200(19) 0.8091(5) 0.5583(13) 0.164 Uiso 1 calc R . C23 C 0.1933(23) 0.8289(4) 0.5564(8) 0.129(4) Uani 1 d . . H23 H 0.2011(23) 0.8469(4) 0.6338(8) 0.168 Uiso 1 calc R . C24 C 0.3317(18) 0.8341(4) 0.5226(14) 0.142(5) Uani 1 d . . H24 H 0.4121(18) 0.8545(4) 0.5816(14) 0.185 Uiso 1 calc R . C25 C 0.3803(12) 0.8143(6) 0.4136(18) 0.143(5) Uani 1 d . . H25 H 0.4867(12) 0.8242(6) 0.4188(18) 0.186 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sm1 0.0717(2) 0.0545(2) 0.0415(2) 0.00617(14) 0.01176(12) 0.0113(2) C1 0.046(3) 0.062(3) 0.044(3) 0.001(2) 0.008(2) -0.009(2) C2 0.047(3) 0.059(3) 0.037(2) 0.010(2) 0.011(2) -0.007(2) C3 0.046(3) 0.059(3) 0.047(3) 0.013(2) 0.013(2) 0.000(2) C4 0.058(3) 0.051(3) 0.065(3) 0.015(3) 0.026(3) 0.012(3) C5 0.057(3) 0.049(3) 0.056(3) 0.000(2) 0.013(2) -0.004(2) C6 0.053(3) 0.084(4) 0.044(3) -0.014(3) 0.014(2) -0.023(3) C7 0.077(4) 0.099(5) 0.057(4) -0.020(3) 0.020(3) -0.008(4) C8 0.100(5) 0.157(7) 0.041(3) -0.002(4) 0.015(3) 0.028(5) C9 0.044(3) 0.086(4) 0.069(4) 0.003(3) 0.016(3) -0.004(3) C10 0.076(4) 0.101(6) 0.093(5) 0.015(4) 0.022(4) -0.026(4) C11 0.055(4) 0.115(6) 0.080(4) 0.021(4) 0.008(3) 0.002(4) C12 0.104(5) 0.076(4) 0.092(5) -0.002(4) 0.049(4) 0.028(4) C13 0.120(6) 0.125(7) 0.072(5) -0.029(5) 0.030(4) 0.037(5) C14 0.126(6) 0.072(5) 0.130(7) -0.012(5) 0.032(6) 0.037(5) C15 0.076(4) 0.067(4) 0.076(4) -0.014(3) 0.024(3) -0.015(3) C16 0.109(6) 0.106(7) 0.183(10) -0.066(7) -0.057(6) -0.010(5) C17 0.152(9) 0.119(8) 0.172(10) 0.048(7) -0.016(7) -0.079(7) C18 0.161(12) 0.152(12) 0.128(10) 0.083(9) 0.083(9) 0.111(10) C19 0.216(14) 0.082(7) 0.092(6) 0.013(6) 0.060(10) 0.064(9) C20 0.190(13) 0.056(5) 0.111(9) 0.021(5) 0.013(8) -0.007(6) C21 0.125(8) 0.128(10) 0.134(9) 0.073(8) 0.040(8) -0.002(7) C22 0.166(11) 0.154(11) 0.083(7) 0.056(7) 0.074(7) 0.054(8) C23 0.191(12) 0.125(9) 0.041(4) 0.005(4) 0.011(7) 0.023(9) C24 0.113(9) 0.144(10) 0.098(8) 0.036(7) -0.039(6) -0.017(8) C25 0.077(6) 0.187(13) 0.147(10) 0.112(10) 0.021(7) 0.052(8) _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 C18 2.557(9) . ? Sm1 C19 2.563(9) . ? Sm1 C25 2.564(8) . ? Sm1 C20 2.568(9) . ? Sm1 C24 2.570(8) . ? Sm1 C23 2.572(8) . ? Sm1 C22 2.587(8) . ? Sm1 C21 2.595(9) . ? Sm1 C1 2.675(5) . ? Sm1 C2 2.681(4) . ? Sm1 C3 2.682(5) . ? Sm1 C4 2.694(5) . ? C1 C5 1.396(7) . ? C1 C2 1.421(7) . ? C2 C3 1.402(7) . ? C2 C6 1.514(7) . ? C3 C4 1.409(7) . ? C3 C9 1.544(7) . ? C4 C5 1.434(7) . ? C4 C12 1.521(8) . ? C5 C15 1.502(8) . ? C6 C7 1.515(8) . ? C6 C8 1.516(8) . ? C9 C10 1.466(9) . ? C9 C11 1.501(8) . ? C12 C13 1.483(9) . ? C12 C14 1.484(10) . ? C15 C16 1.471(10) . ? C15 C17 1.491(10) . ? C18 C19 1.39(2) . ? C18 C25 1.40(2) . ? C19 C20 1.340(15) . ? C20 C21 1.349(14) . ? C21 C22 1.363(15) . ? C22 C23 1.35(2) . ? C23 C24 1.36(2) . ? C24 C25 1.45(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 C18 Sm1 C19 31.5(4) . . ? C18 Sm1 C25 31.8(4) . . ? C19 Sm1 C25 60.2(4) . . ? C18 Sm1 C20 59.1(4) . . ? C19 Sm1 C20 30.3(3) . . ? C25 Sm1 C20 80.7(4) . . ? C18 Sm1 C24 61.6(4) . . ? C19 Sm1 C24 82.1(4) . . ? C25 Sm1 C24 32.8(4) . . ? C20 Sm1 C24 88.9(3) . . ? C18 Sm1 C23 81.6(4) . . ? C19 Sm1 C23 88.6(3) . . ? C25 Sm1 C23 60.3(4) . . ? C20 Sm1 C23 79.6(3) . . ? C24 Sm1 C23 30.6(4) . . ? C18 Sm1 C22 88.6(3) . . ? C19 Sm1 C22 79.2(4) . . ? C25 Sm1 C22 80.6(4) . . ? C20 Sm1 C22 58.2(4) . . ? C24 Sm1 C22 58.3(4) . . ? C23 Sm1 C22 30.4(4) . . ? C18 Sm1 C21 79.9(4) . . ? C19 Sm1 C21 57.9(4) . . ? C25 Sm1 C21 88.5(3) . . ? C20 Sm1 C21 30.3(3) . . ? C24 Sm1 C21 79.8(4) . . ? C23 Sm1 C21 58.4(4) . . ? C22 Sm1 C21 30.5(3) . . ? C18 Sm1 C1 100.7(3) . . ? C19 Sm1 C1 113.2(3) . . ? C25 Sm1 C1 102.8(3) . . ? C20 Sm1 C1 134.3(3) . . ? C24 Sm1 C1 118.7(4) . . ? C23 Sm1 C1 142.0(4) . . ? C22 Sm1 C1 167.3(3) . . ? C21 Sm1 C1 159.7(4) . . ? C18 Sm1 C2 105.7(3) . . ? C19 Sm1 C2 101.4(3) . . ? C25 Sm1 C2 123.0(3) . . ? C20 Sm1 C2 110.2(3) . . ? C24 Sm1 C2 148.0(4) . . ? C23 Sm1 C2 169.8(3) . . ? C22 Sm1 C2 153.6(4) . . ? C21 Sm1 C2 129.2(3) . . ? C1 Sm1 C2 30.77(14) . . ? C18 Sm1 C3 134.4(3) . . ? C19 Sm1 C3 119.7(3) . . ? C25 Sm1 C3 152.0(3) . . ? C20 Sm1 C3 112.8(3) . . ? C24 Sm1 C3 157.4(3) . . ? C23 Sm1 C3 143.8(4) . . ? C22 Sm1 C3 127.5(3) . . ? C21 Sm1 C3 115.8(3) . . ? C1 Sm1 C3 49.9(2) . . ? C2 Sm1 C3 30.31(15) . . ? C18 Sm1 C4 150.6(3) . . ? C19 Sm1 C4 149.7(3) . . ? C25 Sm1 C4 140.2(4) . . ? C20 Sm1 C4 138.9(3) . . ? C24 Sm1 C4 127.2(3) . . ? C23 Sm1 C4 120.2(3) . . ? C22 Sm1 C4 120.4(2) . . ? C21 Sm1 C4 127.4(3) . . ? C1 Sm1 C4 49.9(2) . . ? C2 Sm1 C4 50.5(2) . . ? C3 Sm1 C4 30.4(2) . . ? C5 C1 C2 110.3(5) . . ? C5 C1 Sm1 76.4(3) . . ? C2 C1 Sm1 74.8(3) . . ? C3 C2 C1 106.4(5) . . ? C3 C2 C6 127.5(4) . . ? C1 C2 C6 125.9(5) . . ? C3 C2 Sm1 74.9(3) . . ? C1 C2 Sm1 74.4(3) . . ? C6 C2 Sm1 120.2(3) . . ? C2 C3 C4 109.1(4) . . ? C2 C3 C9 122.1(5) . . ? C4 C3 C9 128.7(5) . . ? C2 C3 Sm1 74.8(3) . . ? C4 C3 Sm1 75.3(3) . . ? C9 C3 Sm1 118.5(3) . . ? C3 C4 C5 108.0(5) . . ? C3 C4 C12 125.7(5) . . ? C5 C4 C12 126.3(6) . . ? C3 C4 Sm1 74.3(3) . . ? C5 C4 Sm1 75.2(3) . . ? C12 C4 Sm1 118.5(4) . . ? C1 C5 C4 106.3(5) . . ? C1 C5 C15 124.5(5) . . ? C4 C5 C15 129.1(5) . . ? C1 C5 Sm1 73.6(3) . . ? C4 C5 Sm1 74.0(3) . . ? C15 C5 Sm1 121.1(4) . . ? C2 C6 C7 113.8(4) . . ? C2 C6 C8 110.2(5) . . ? C7 C6 C8 109.3(5) . . ? C10 C9 C11 115.3(5) . . ? C10 C9 C3 116.2(5) . . ? C11 C9 C3 112.6(5) . . ? C13 C12 C14 115.8(7) . . ? C13 C12 C4 115.2(5) . . ? C14 C12 C4 114.2(6) . . ? C16 C15 C17 106.9(7) . . ? C16 C15 C5 114.6(6) . . ? C17 C15 C5 110.8(6) . . ? C19 C18 C25 134.0(11) . . ? C19 C18 Sm1 74.5(5) . . ? C25 C18 Sm1 74.4(6) . . ? C20 C19 C18 135.5(11) . . ? C20 C19 Sm1 75.1(5) . . ? C18 C19 Sm1 74.0(6) . . ? C19 C20 C21 136.4(12) . . ? C19 C20 Sm1 74.7(6) . . ? C21 C20 Sm1 76.0(6) . . ? C20 C21 C22 134.9(11) . . ? C20 C21 Sm1 73.7(6) . . ? C22 C21 Sm1 74.4(5) . . ? C23 C22 C21 136.0(10) . . ? C23 C22 Sm1 74.2(5) . . ? C21 C22 Sm1 75.1(5) . . ? C22 C23 C24 136.1(11) . . ? C22 C23 Sm1 75.4(5) . . ? C24 C23 Sm1 74.6(5) . . ? C23 C24 C25 133.4(11) . . ? C23 C24 Sm1 74.8(5) . . ? C25 C24 Sm1 73.4(5) . . ? C18 C25 C24 133.6(11) . . ? C18 C25 Sm1 73.8(5) . . ? C24 C25 Sm1 73.8(5) . . ? _refine_diff_density_max 1.106 _refine_diff_density_min -1.055 _refine_diff_density_rms 0.103 #===END data_(III) # CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common compound3 _chemical_formula_moiety 'C25 H37 Nd' _chemical_formula_sum 'C25 H37 Nd' _chemical_formula_weight 481.79 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' 'Nd' 'Nd' -0.1943 3.0179 '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/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 19.021(3) _cell_length_b 8.377(3) _cell_length_c 29.023(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.718(12) _cell_angle_gamma 90.00 _cell_volume 4622.4(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 26.3 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 2.252 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.80 _exptl_absorpt_correction_T_max 0.98 _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 Omega-scans _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 32 _diffrn_reflns_number 6485 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 22.78 _reflns_number_total 6241 _reflns_number_gt 4035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 EXPRESS' _computing_cell_refinement 'CAD4 EXPRESS' _computing_data_reduction 'XCAD4 (Harms, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.6353P] 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 6241 _refine_ls_number_parameters 457 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0666 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.002 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 Nd1 Nd 0.593130(16) 0.02892(4) 0.346609(10) 0.04707(11) Uani 1 1 d . . . Nd2 Nd 0.866898(18) 0.06724(5) 0.162140(11) 0.06643(14) Uani 1 1 d . . . C1 C 0.90776(18) 0.0124(4) 0.07389(12) 0.0434(13) Uani 1 1 d G . . C2 C 0.96021(19) -0.0606(4) 0.10227(13) 0.0472(14) Uani 1 1 d G . . H2 H 0.9684 -0.1697 0.1050 0.061 Uiso 1 1 calc R . . C3 C 0.99802(18) 0.0615(4) 0.12580(11) 0.0400(13) Uani 1 1 d G . . C4 C 0.96890(19) 0.2099(4) 0.11200(12) 0.0421(13) Uani 1 1 d G . . C5 C 0.91312(19) 0.1795(4) 0.07992(12) 0.0392(13) Uani 1 1 d G . . C6 C 0.60817(16) -0.1381(4) 0.42824(11) 0.0355(12) Uani 1 1 d G . . C7 C 0.65620(17) -0.0095(4) 0.43183(11) 0.0331(12) Uani 1 1 d G . . C8 C 0.70901(15) -0.0346(4) 0.39935(11) 0.0333(12) Uani 1 1 d G . . C9 C 0.69357(16) -0.1787(4) 0.37565(12) 0.0377(13) Uani 1 1 d G . . C10 C 0.63126(17) -0.2426(4) 0.39351(12) 0.0415(13) Uani 1 1 d G . . H10 H 0.6093 -0.3368 0.3841 0.054 Uiso 1 1 calc R . . C11 C 0.8606(3) -0.0811(7) 0.04013(19) 0.0571(16) Uani 1 1 d . . . H11 H 0.8289 -0.0052 0.0243 0.074 Uiso 1 1 calc R . . C41 C 0.9981(3) 0.3696(6) 0.12884(18) 0.0509(15) Uani 1 1 d . . . H41 H 1.0349 0.3439 0.1520 0.066 Uiso 1 1 calc R . . C51 C 0.8702(3) 0.3074(7) 0.05439(18) 0.0554(15) Uani 1 1 d . . . H51 H 0.8874 0.4106 0.0659 0.072 Uiso 1 1 calc R . . C52 C 0.7921(3) 0.3014(7) 0.0641(2) 0.076(2) Uani 1 1 d . . . H52A H 0.7681 0.3844 0.0471 0.098 Uiso 1 1 calc R . . H52B H 0.7856 0.3166 0.0965 0.098 Uiso 1 1 calc R . . H52C H 0.7734 0.1995 0.0548 0.098 Uiso 1 1 calc R . . C53 C 0.8819(3) 0.3062(8) 0.00242(19) 0.078(2) Uani 1 1 d . . . H53A H 0.9315 0.3102 -0.0030 0.102 Uiso 1 1 calc R . . H53B H 0.8593 0.3974 -0.0115 0.102 Uiso 1 1 calc R . . H53C H 0.8624 0.2104 -0.0108 0.102 Uiso 1 1 calc R . . C31 C 1.0645(3) 0.0330(6) 0.15549(19) 0.0518(15) Uani 1 1 d . . . H31 H 1.0720 0.1269 0.1752 0.067 Uiso 1 1 calc R . . C32 C 1.1276(3) 0.0174(10) 0.1248(2) 0.104(3) Uani 1 1 d . . . H32A H 1.1300 0.1090 0.1051 0.135 Uiso 1 1 calc R . . H32B H 1.1228 -0.0774 0.1064 0.135 Uiso 1 1 calc R . . H32C H 1.1699 0.0107 0.1437 0.135 Uiso 1 1 calc R . . C91 C 0.7354(3) -0.2631(6) 0.33857(17) 0.0441(14) Uani 1 1 d . . . H91 H 0.7743 -0.1928 0.3303 0.057 Uiso 1 1 calc R . . C81 C 0.7712(3) 0.0739(6) 0.39068(19) 0.0474(14) Uani 1 1 d . . . H81 H 0.7687 0.1620 0.4128 0.062 Uiso 1 1 calc R . . C82 C 0.7673(3) 0.1485(7) 0.34272(19) 0.0685(18) Uani 1 1 d . . . H82A H 0.8075 0.2158 0.3387 0.089 Uiso 1 1 calc R . . H82B H 0.7252 0.2111 0.3394 0.089 Uiso 1 1 calc R . . H82C H 0.7668 0.0656 0.3199 0.089 Uiso 1 1 calc R . . C83 C 0.8417(3) -0.0086(7) 0.3998(2) 0.077(2) Uani 1 1 d . . . H83A H 0.8792 0.0645 0.3938 0.100 Uiso 1 1 calc R . . H83B H 0.8452 -0.0997 0.3799 0.100 Uiso 1 1 calc R . . H83C H 0.8451 -0.0428 0.4313 0.100 Uiso 1 1 calc R . . C71 C 0.6522(3) 0.1229(6) 0.46794(16) 0.0424(13) Uani 1 1 d . . . H71 H 0.6096 0.1022 0.4851 0.055 Uiso 1 1 calc R . . C72 C 0.7137(3) 0.1149(7) 0.50305(19) 0.0680(18) Uani 1 1 d . . . H72A H 0.7176 0.0086 0.5151 0.088 Uiso 1 1 calc R . . H72B H 0.7056 0.1883 0.5278 0.088 Uiso 1 1 calc R . . H72C H 0.7564 0.1431 0.4883 0.088 Uiso 1 1 calc R . . C73 C 0.6440(3) 0.2904(6) 0.44780(18) 0.0560(16) Uani 1 1 d . . . H73A H 0.6051 0.2919 0.4259 0.073 Uiso 1 1 calc R . . H73B H 0.6863 0.3198 0.4327 0.073 Uiso 1 1 calc R . . H73C H 0.6354 0.3649 0.4721 0.073 Uiso 1 1 calc R . . C61 C 0.5476(3) -0.1710(6) 0.45943(18) 0.0490(14) Uani 1 1 d . . . H61 H 0.5231 -0.0698 0.4645 0.064 Uiso 1 1 calc R . . C62 C 0.4939(3) -0.2898(7) 0.4387(2) 0.077(2) Uani 1 1 d . . . H62A H 0.4568 -0.3059 0.4599 0.100 Uiso 1 1 calc R . . H62B H 0.5168 -0.3897 0.4330 0.100 Uiso 1 1 calc R . . H62C H 0.4746 -0.2480 0.4102 0.100 Uiso 1 1 calc R . . C63 C 0.5742(3) -0.2330(8) 0.5064(2) 0.078(2) Uani 1 1 d . . . H63A H 0.5349 -0.2529 0.5256 0.101 Uiso 1 1 calc R . . H63B H 0.6045 -0.1548 0.5207 0.101 Uiso 1 1 calc R . . H63C H 0.5999 -0.3304 0.5022 0.101 Uiso 1 1 calc R . . C100 C 0.5560(5) 0.0145(14) 0.2591(2) 0.093(3) Uani 1 1 d . . . H100 H 0.5741 -0.0396 0.2341 0.122 Uiso 1 1 calc R . . C101 C 0.5833(4) 0.1589(15) 0.2637(3) 0.097(3) Uani 1 1 d . . . H101 H 0.6151 0.1814 0.2409 0.126 Uiso 1 1 calc R . . C102 C 0.5766(5) 0.2819(11) 0.2934(4) 0.102(3) Uani 1 1 d . . . H102 H 0.6049 0.3680 0.2858 0.133 Uiso 1 1 calc R . . C103 C 0.5388(7) 0.3117(11) 0.3317(4) 0.116(4) Uani 1 1 d . . . H103 H 0.5485 0.4116 0.3443 0.151 Uiso 1 1 calc R . . C104 C 0.4895(6) 0.2284(18) 0.3561(3) 0.123(5) Uani 1 1 d . . . H104 H 0.4725 0.2859 0.3808 0.160 Uiso 1 1 calc R . . C105 C 0.4589(4) 0.0733(19) 0.3516(3) 0.119(4) Uani 1 1 d . . . H105 H 0.4269 0.0507 0.3743 0.154 Uiso 1 1 calc R . . C106 C 0.4671(4) -0.0554(12) 0.3193(4) 0.107(3) Uani 1 1 d . . . H106 H 0.4390 -0.1435 0.3252 0.138 Uiso 1 1 calc R . . C107 C 0.5087(6) -0.0739(10) 0.2812(3) 0.100(3) Uani 1 1 d . . . H107 H 0.5022 -0.1733 0.2674 0.130 Uiso 1 1 calc R . . C200 C 0.7983(6) -0.1694(12) 0.1982(4) 0.117(3) Uani 1 1 d . . . H200 H 0.7924 -0.2755 0.1896 0.152 Uiso 1 1 calc R . . C201 C 0.8570(6) -0.1448(14) 0.2271(3) 0.115(3) Uani 1 1 d . . . H201 H 0.8808 -0.2395 0.2337 0.149 Uiso 1 1 calc R . . C202 C 0.8885(5) -0.0162(17) 0.2482(3) 0.112(3) Uani 1 1 d . . . H202 H 0.9276 -0.0450 0.2664 0.145 Uiso 1 1 calc R . . C203 C 0.8762(5) 0.1444(16) 0.2489(2) 0.108(3) Uani 1 1 d . . . H203 H 0.9104 0.1996 0.2660 0.141 Uiso 1 1 calc R . . C204 C 0.8245(7) 0.2463(12) 0.2299(3) 0.113(3) Uani 1 1 d . . . H204 H 0.8314 0.3522 0.2385 0.147 Uiso 1 1 calc R . . C205 C 0.7660(6) 0.2265(16) 0.2016(4) 0.125(4) Uani 1 1 d . . . H205 H 0.7431 0.3222 0.1950 0.163 Uiso 1 1 calc R . . C206 C 0.7333(5) 0.0954(19) 0.1807(4) 0.126(5) Uani 1 1 d . . . H206 H 0.6933 0.1237 0.1633 0.164 Uiso 1 1 calc R . . C207 C 0.7466(6) -0.0697(19) 0.1796(3) 0.134(4) Uani 1 1 d . . . H207 H 0.7126 -0.1252 0.1624 0.174 Uiso 1 1 calc R . . C92 C 0.7671(4) -0.4167(8) 0.3574(2) 0.094(2) Uani 1 1 d . . . H92A H 0.7946 -0.3941 0.3849 0.122 Uiso 1 1 calc R . . H92B H 0.7966 -0.4635 0.3348 0.122 Uiso 1 1 calc R . . H92C H 0.7301 -0.4899 0.3645 0.122 Uiso 1 1 calc R . . C42 C 1.0347(4) 0.4618(7) 0.0911(2) 0.081(2) Uani 1 1 d . . . H42A H 1.0679 0.3933 0.0766 0.105 Uiso 1 1 calc R . . H42B H 1.0589 0.5520 0.1044 0.105 Uiso 1 1 calc R . . H42C H 1.0003 0.4980 0.0686 0.105 Uiso 1 1 calc R . . C93 C 0.6914(3) -0.2963(9) 0.2948(2) 0.091(2) Uani 1 1 d . . . H93A H 0.6718 -0.1981 0.2832 0.118 Uiso 1 1 calc R . . H93B H 0.6540 -0.3687 0.3017 0.118 Uiso 1 1 calc R . . H93C H 0.7206 -0.3430 0.2720 0.118 Uiso 1 1 calc R . . C12 C 0.8161(4) -0.2050(8) 0.0632(2) 0.098(2) Uani 1 1 d . . . H12A H 0.7882 -0.1547 0.0861 0.127 Uiso 1 1 calc R . . H12B H 0.8460 -0.2840 0.0775 0.127 Uiso 1 1 calc R . . H12C H 0.7856 -0.2552 0.0405 0.127 Uiso 1 1 calc R . . C33 C 1.0616(3) -0.1117(8) 0.1863(2) 0.089(2) Uani 1 1 d . . . H33A H 1.0219 -0.1031 0.2058 0.116 Uiso 1 1 calc R . . H33B H 1.1040 -0.1179 0.2050 0.116 Uiso 1 1 calc R . . H33C H 1.0570 -0.2062 0.1678 0.116 Uiso 1 1 calc R . . C43 C 0.9446(4) 0.4709(7) 0.1535(2) 0.0740(19) Uani 1 1 d . . . H43A H 0.9661 0.5695 0.1632 0.096 Uiso 1 1 calc R . . H43B H 0.9286 0.4142 0.1800 0.096 Uiso 1 1 calc R . . H43C H 0.9053 0.4929 0.1329 0.096 Uiso 1 1 calc R . . C13 C 0.9037(4) -0.1630(9) 0.0042(2) 0.101(3) Uani 1 1 d . . . H13A H 0.9323 -0.0856 -0.0108 0.132 Uiso 1 1 calc R . . H13B H 0.8729 -0.2134 -0.0182 0.132 Uiso 1 1 calc R . . H13C H 0.9334 -0.2421 0.0188 0.132 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 Nd1 0.04140(19) 0.0575(2) 0.04192(19) -0.00115(16) -0.00481(14) 0.00470(16) Nd2 0.0552(2) 0.0984(3) 0.0463(2) 0.01305(19) 0.01255(17) -0.00407(19) C1 0.048(3) 0.047(4) 0.035(3) -0.003(3) -0.005(3) -0.002(3) C2 0.055(4) 0.037(3) 0.050(3) 0.002(3) -0.003(3) 0.000(3) C3 0.048(3) 0.044(4) 0.028(3) 0.000(2) 0.000(2) -0.004(3) C4 0.050(3) 0.038(3) 0.038(3) 0.001(3) 0.006(3) 0.000(3) C5 0.044(3) 0.043(4) 0.030(3) 0.002(3) -0.003(2) 0.003(3) C6 0.027(3) 0.040(3) 0.039(3) 0.002(3) 0.005(2) 0.002(3) C7 0.034(3) 0.034(3) 0.032(3) 0.000(2) 0.002(2) 0.002(2) C8 0.022(3) 0.040(3) 0.038(3) 0.002(3) 0.003(2) -0.002(2) C9 0.030(3) 0.040(3) 0.044(3) -0.004(3) 0.009(2) 0.006(2) C10 0.034(3) 0.036(3) 0.055(3) -0.005(3) 0.005(3) -0.005(2) C11 0.061(4) 0.059(4) 0.050(4) -0.002(3) -0.023(3) -0.004(3) C41 0.064(4) 0.036(3) 0.053(4) -0.001(3) 0.000(3) -0.003(3) C51 0.058(4) 0.057(4) 0.051(4) 0.009(3) -0.001(3) 0.010(3) C52 0.064(5) 0.084(5) 0.079(5) 0.022(4) -0.004(4) 0.020(4) C53 0.087(5) 0.092(5) 0.056(4) 0.033(4) -0.001(4) 0.009(4) C31 0.057(4) 0.047(3) 0.050(4) -0.002(3) -0.013(3) 0.001(3) C32 0.046(4) 0.175(8) 0.092(5) 0.035(5) -0.001(4) -0.004(5) C91 0.048(3) 0.036(3) 0.050(4) -0.007(3) 0.017(3) -0.002(3) C81 0.039(3) 0.044(3) 0.059(4) -0.006(3) 0.007(3) -0.007(3) C82 0.080(5) 0.056(4) 0.070(4) 0.002(3) 0.022(4) -0.025(3) C83 0.032(3) 0.083(5) 0.116(6) -0.007(4) 0.000(3) -0.012(3) C71 0.044(3) 0.047(3) 0.036(3) -0.001(3) 0.001(3) 0.005(3) C72 0.078(4) 0.072(4) 0.053(4) -0.020(3) -0.013(3) 0.010(4) C73 0.065(4) 0.047(4) 0.056(4) -0.013(3) -0.002(3) 0.008(3) C61 0.041(3) 0.053(4) 0.054(4) -0.001(3) 0.017(3) 0.002(3) C62 0.057(4) 0.091(5) 0.085(5) -0.005(4) 0.029(4) -0.027(4) C63 0.077(5) 0.091(5) 0.068(5) 0.025(4) 0.034(4) 0.000(4) C100 0.100(7) 0.132(9) 0.047(5) -0.027(5) -0.014(5) 0.030(6) C101 0.083(6) 0.136(9) 0.070(6) 0.032(6) -0.014(5) 0.013(7) C102 0.124(8) 0.069(6) 0.110(8) 0.033(5) -0.045(7) -0.017(5) C103 0.144(11) 0.092(7) 0.109(9) -0.044(7) -0.067(7) 0.067(7) C104 0.075(8) 0.217(14) 0.076(7) -0.055(9) -0.020(6) 0.093(8) C105 0.028(4) 0.248(14) 0.081(7) 0.040(8) -0.002(4) 0.021(7) C106 0.056(5) 0.138(9) 0.122(8) 0.030(7) -0.040(6) -0.038(5) C107 0.105(7) 0.107(7) 0.084(7) -0.022(6) -0.043(6) -0.012(6) C200 0.113(8) 0.135(8) 0.105(8) 0.031(6) 0.037(7) -0.033(7) C201 0.118(9) 0.138(10) 0.090(8) 0.052(7) 0.031(6) 0.034(7) C202 0.088(7) 0.181(11) 0.066(6) 0.041(8) 0.005(5) 0.024(8) C203 0.108(8) 0.179(11) 0.039(5) -0.006(6) 0.022(5) -0.041(8) C204 0.144(10) 0.134(8) 0.064(6) 0.016(6) 0.050(6) 0.025(8) C205 0.108(9) 0.183(12) 0.087(8) 0.053(8) 0.045(6) 0.071(8) C206 0.064(6) 0.233(15) 0.082(7) 0.041(10) 0.009(5) 0.008(9) C207 0.078(8) 0.228(14) 0.095(8) 0.013(10) 0.009(6) -0.060(9) C92 0.112(6) 0.070(5) 0.103(6) -0.003(4) 0.044(5) 0.035(4) C42 0.092(5) 0.055(4) 0.096(5) -0.004(4) 0.017(4) -0.021(4) C93 0.081(5) 0.136(7) 0.056(4) -0.035(4) 0.020(4) 0.008(5) C12 0.096(6) 0.102(6) 0.094(6) -0.002(5) -0.033(5) -0.034(5) C33 0.073(5) 0.108(6) 0.086(5) 0.040(5) -0.018(4) -0.001(4) C43 0.103(5) 0.054(4) 0.064(4) -0.014(3) 0.001(4) -0.009(4) C13 0.101(6) 0.125(7) 0.077(5) -0.055(5) -0.020(4) 0.005(5) _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 Nd1 C105 2.589(7) . ? Nd1 C107 2.597(7) . ? Nd1 C106 2.600(7) . ? Nd1 C104 2.606(8) . ? Nd1 C103 2.616(8) . ? Nd1 C100 2.620(7) . ? Nd1 C102 2.636(7) . ? Nd1 C101 2.642(7) . ? Nd1 C8 2.698(3) . ? Nd1 C9 2.700(3) . ? Nd1 C7 2.735(3) . ? Nd1 C10 2.738(3) . ? Nd2 C203 2.600(7) . ? Nd2 C201 2.601(8) . ? Nd2 C200 2.610(8) . ? Nd2 C202 2.615(8) . ? Nd2 C204 2.620(8) . ? Nd2 C207 2.623(9) . ? Nd2 C206 2.625(10) . ? Nd2 C205 2.628(9) . ? Nd2 C5 2.734(4) . ? Nd2 C4 2.735(4) . ? Nd2 C3 2.737(4) . ? Nd2 C1 2.738(4) . ? C1 C2 1.413(2) . ? C1 C5 1.415(2) . ? C1 C11 1.525(6) . ? C2 C3 1.414(2) . ? C3 C4 1.414(2) . ? C3 C31 1.528(6) . ? C4 C5 1.413(2) . ? C4 C41 1.523(6) . ? C5 C51 1.526(6) . ? C6 C7 1.414(2) . ? C6 C10 1.415(2) . ? C6 C61 1.512(6) . ? C7 C8 1.414(2) . ? C7 C71 1.529(6) . ? C8 C9 1.416(2) . ? C8 C81 1.519(6) . ? C9 C10 1.413(2) . ? C9 C91 1.531(5) . ? C11 C12 1.508(8) . ? C11 C13 1.512(8) . ? C41 C43 1.521(8) . ? C41 C42 1.525(7) . ? C51 C52 1.520(7) . ? C51 C53 1.532(7) . ? C31 C33 1.509(8) . ? C31 C32 1.521(8) . ? C91 C92 1.515(8) . ? C91 C93 1.527(8) . ? C81 C83 1.525(7) . ? C81 C82 1.526(7) . ? C71 C73 1.527(7) . ? C71 C72 1.529(7) . ? C61 C63 1.530(7) . ? C61 C62 1.536(7) . ? C100 C101 1.322(11) . ? C100 C107 1.343(11) . ? C101 C102 1.351(11) . ? C102 C103 1.366(12) . ? C103 C104 1.381(13) . ? C104 C105 1.428(13) . ? C105 C106 1.440(13) . ? C106 C107 1.389(12) . ? C200 C207 1.387(13) . ? C200 C201 1.392(12) . ? C201 C202 1.369(12) . ? C202 C203 1.366(12) . ? C203 C204 1.402(12) . ? C204 C205 1.372(12) . ? C205 C206 1.393(13) . ? C206 C207 1.407(14) . ? 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 C105 Nd1 C107 60.0(3) . . ? C105 Nd1 C106 32.2(3) . . ? C107 Nd1 C106 31.0(3) . . ? C105 Nd1 C104 31.9(3) . . ? C107 Nd1 C104 80.6(3) . . ? C106 Nd1 C104 60.8(3) . . ? C105 Nd1 C103 59.6(3) . . ? C107 Nd1 C103 86.9(3) . . ? C106 Nd1 C103 80.7(3) . . ? C104 Nd1 C103 30.7(3) . . ? C105 Nd1 C100 79.8(3) . . ? C107 Nd1 C100 29.8(2) . . ? C106 Nd1 C100 58.2(3) . . ? C104 Nd1 C100 87.1(3) . . ? C103 Nd1 C100 77.7(3) . . ? C105 Nd1 C102 79.5(3) . . ? C107 Nd1 C102 77.2(3) . . ? C106 Nd1 C102 87.0(3) . . ? C104 Nd1 C102 57.9(3) . . ? C103 Nd1 C102 30.2(3) . . ? C100 Nd1 C102 56.3(3) . . ? C105 Nd1 C101 87.1(3) . . ? C107 Nd1 C101 56.3(3) . . ? C106 Nd1 C101 78.2(3) . . ? C104 Nd1 C101 78.4(3) . . ? C103 Nd1 C101 57.3(3) . . ? C100 Nd1 C101 29.1(2) . . ? C102 Nd1 C101 29.7(2) . . ? C105 Nd1 C8 141.9(2) . . ? C107 Nd1 C8 145.7(2) . . ? C106 Nd1 C8 148.1(2) . . ? C104 Nd1 C8 132.4(2) . . ? C103 Nd1 C8 125.8(2) . . ? C100 Nd1 C8 137.1(2) . . ? C102 Nd1 C8 124.87(19) . . ? C101 Nd1 C8 129.19(19) . . ? C105 Nd1 C9 139.9(3) . . ? C107 Nd1 C9 115.5(2) . . ? C106 Nd1 C9 123.9(2) . . ? C104 Nd1 C9 155.6(2) . . ? C103 Nd1 C9 155.2(2) . . ? C100 Nd1 C9 116.16(19) . . ? C102 Nd1 C9 140.5(2) . . ? C101 Nd1 C9 125.4(2) . . ? C8 Nd1 C9 30.40(5) . . ? C105 Nd1 C7 111.9(2) . . ? C107 Nd1 C7 150.1(3) . . ? C106 Nd1 C7 128.2(3) . . ? C104 Nd1 C7 107.0(2) . . ? C103 Nd1 C7 114.6(2) . . ? C100 Nd1 C7 165.89(19) . . ? C102 Nd1 C7 131.7(2) . . ? C101 Nd1 C7 152.7(2) . . ? C8 Nd1 C7 30.15(5) . . ? C9 Nd1 C7 49.82(8) . . ? C105 Nd1 C10 109.8(3) . . ? C107 Nd1 C10 103.7(2) . . ? C106 Nd1 C10 98.8(2) . . ? C104 Nd1 C10 132.1(3) . . ? C103 Nd1 C10 158.8(3) . . ? C100 Nd1 C10 120.2(2) . . ? C102 Nd1 C10 170.0(3) . . ? C101 Nd1 C10 143.7(3) . . ? C8 Nd1 C10 49.79(8) . . ? C9 Nd1 C10 30.12(5) . . ? C7 Nd1 C10 49.47(8) . . ? C203 Nd2 C201 58.2(3) . . ? C203 Nd2 C200 79.7(3) . . ? C201 Nd2 C200 31.0(3) . . ? C203 Nd2 C202 30.4(3) . . ? C201 Nd2 C202 30.4(3) . . ? C200 Nd2 C202 58.6(3) . . ? C203 Nd2 C204 31.2(3) . . ? C201 Nd2 C204 79.4(3) . . ? C200 Nd2 C204 88.0(3) . . ? C202 Nd2 C204 58.6(3) . . ? C203 Nd2 C207 87.5(3) . . ? C201 Nd2 C207 58.6(3) . . ? C200 Nd2 C207 30.7(3) . . ? C202 Nd2 C207 79.1(3) . . ? C204 Nd2 C207 79.3(3) . . ? C203 Nd2 C206 79.5(3) . . ? C201 Nd2 C206 79.7(3) . . ? C200 Nd2 C206 59.1(3) . . ? C202 Nd2 C206 87.4(3) . . ? C204 Nd2 C206 58.2(3) . . ? C207 Nd2 C206 31.1(3) . . ? C203 Nd2 C205 58.7(3) . . ? C201 Nd2 C205 87.8(3) . . ? C200 Nd2 C205 80.2(3) . . ? C202 Nd2 C205 79.3(3) . . ? C204 Nd2 C205 30.3(3) . . ? C207 Nd2 C205 59.0(4) . . ? C206 Nd2 C205 30.8(3) . . ? C203 Nd2 C5 138.2(2) . . ? C201 Nd2 C5 154.1(2) . . ? C200 Nd2 C5 142.1(2) . . ? C202 Nd2 C5 151.7(2) . . ? C204 Nd2 C5 124.9(2) . . ? C207 Nd2 C5 128.6(2) . . ? C206 Nd2 C5 119.1(2) . . ? C205 Nd2 C5 117.6(2) . . ? C203 Nd2 C4 112.2(2) . . ? C201 Nd2 C4 138.8(3) . . ? C200 Nd2 C4 156.5(2) . . ? C202 Nd2 C4 122.1(2) . . ? C204 Nd2 C4 112.9(2) . . ? C207 Nd2 C4 158.6(2) . . ? C206 Nd2 C4 141.0(3) . . ? C205 Nd2 C4 123.3(3) . . ? C5 Nd2 C4 29.96(5) . . ? C203 Nd2 C3 109.9(2) . . ? C201 Nd2 C3 110.7(2) . . ? C200 Nd2 C3 127.9(3) . . ? C202 Nd2 C3 104.1(2) . . ? C204 Nd2 C3 127.2(3) . . ? C207 Nd2 C3 151.3(3) . . ? C206 Nd2 C3 168.5(2) . . ? C205 Nd2 C3 149.6(3) . . ? C5 Nd2 C3 49.41(8) . . ? C4 Nd2 C3 29.95(5) . . ? C203 Nd2 C1 159.2(2) . . ? C201 Nd2 C1 126.3(3) . . ? C200 Nd2 C1 114.0(2) . . ? C202 Nd2 C1 143.9(3) . . ? C204 Nd2 C1 154.3(2) . . ? C207 Nd2 C1 112.4(2) . . ? C206 Nd2 C1 120.7(3) . . ? C205 Nd2 C1 136.4(2) . . ? C5 Nd2 C1 29.96(6) . . ? C4 Nd2 C1 49.44(8) . . ? C3 Nd2 C1 49.39(8) . . ? C2 C1 C5 108.0 . . ? C2 C1 C11 123.0(3) . . ? C5 C1 C11 128.8(3) . . ? C2 C1 Nd2 75.08(14) . . ? C5 C1 Nd2 74.89(14) . . ? C11 C1 Nd2 120.6(3) . . ? C1 C2 C3 108.0 . . ? C1 C2 Nd2 75.00(14) . . ? C3 C2 Nd2 74.97(14) . . ? C4 C3 C2 108.0 . . ? C4 C3 C31 127.4(3) . . ? C2 C3 C31 124.0(3) . . ? C4 C3 Nd2 74.93(14) . . ? C2 C3 Nd2 75.10(14) . . ? C31 C3 Nd2 122.3(3) . . ? C5 C4 C3 108.0 . . ? C5 C4 C41 128.9(3) . . ? C3 C4 C41 123.1(3) . . ? C5 C4 Nd2 75.01(14) . . ? C3 C4 Nd2 75.12(14) . . ? C41 C4 Nd2 118.1(3) . . ? C4 C5 C1 108.0 . . ? C4 C5 C51 125.0(3) . . ? C1 C5 C51 126.8(3) . . ? C4 C5 Nd2 75.03(14) . . ? C1 C5 Nd2 75.15(14) . . ? C51 C5 Nd2 118.9(3) . . ? C7 C6 C10 108.1 . . ? C7 C6 C61 126.6(3) . . ? C10 C6 C61 124.9(3) . . ? C7 C6 Nd1 74.16(13) . . ? C10 C6 Nd1 74.25(13) . . ? C61 C6 Nd1 123.0(3) . . ? C8 C7 C6 107.9 . . ? C8 C7 C71 128.0(3) . . ? C6 C7 C71 123.9(3) . . ? C8 C7 Nd1 73.48(13) . . ? C6 C7 Nd1 76.01(12) . . ? C71 C7 Nd1 120.3(3) . . ? C7 C8 C9 108.0 . . ? C7 C8 C81 126.4(3) . . ? C9 C8 C81 125.5(3) . . ? C7 C8 Nd1 76.37(13) . . ? C9 C8 Nd1 74.84(13) . . ? C81 C8 Nd1 114.5(3) . . ? C10 C9 C8 108.0 . . ? C10 C9 C91 122.8(3) . . ? C8 C9 C91 129.1(3) . . ? C10 C9 Nd1 76.43(13) . . ? C8 C9 Nd1 74.76(13) . . ? C91 C9 Nd1 117.2(3) . . ? C9 C10 C6 108.0 . . ? C9 C10 Nd1 73.45(13) . . ? C6 C10 Nd1 75.92(13) . . ? C12 C11 C13 108.5(6) . . ? C12 C11 C1 113.3(5) . . ? C13 C11 C1 110.8(5) . . ? C43 C41 C4 113.5(5) . . ? C43 C41 C42 112.5(5) . . ? C4 C41 C42 112.6(4) . . ? C52 C51 C5 113.5(4) . . ? C52 C51 C53 110.8(5) . . ? C5 C51 C53 112.4(4) . . ? C33 C31 C32 108.8(5) . . ? C33 C31 C3 114.5(4) . . ? C32 C31 C3 109.8(4) . . ? C92 C91 C93 110.4(5) . . ? C92 C91 C9 110.4(4) . . ? C93 C91 C9 112.6(4) . . ? C8 C81 C83 112.6(4) . . ? C8 C81 C82 112.3(4) . . ? C83 C81 C82 111.2(5) . . ? C73 C71 C72 111.3(4) . . ? C73 C71 C7 114.3(4) . . ? C72 C71 C7 111.9(4) . . ? C6 C61 C63 110.9(4) . . ? C6 C61 C62 113.2(4) . . ? C63 C61 C62 109.1(5) . . ? C101 C100 C107 136.3(8) . . ? C101 C100 Nd1 76.4(4) . . ? C107 C100 Nd1 74.1(4) . . ? C100 C101 C102 136.0(9) . . ? C100 C101 Nd1 74.5(5) . . ? C102 C101 Nd1 74.9(5) . . ? C101 C102 C103 136.0(9) . . ? C101 C102 Nd1 75.4(5) . . ? C103 C102 Nd1 74.1(5) . . ? C102 C103 C104 135.1(9) . . ? C102 C103 Nd1 75.8(5) . . ? C104 C103 Nd1 74.3(5) . . ? C103 C104 C105 133.9(9) . . ? C103 C104 Nd1 75.1(5) . . ? C105 C104 Nd1 73.4(5) . . ? C104 C105 C106 133.5(9) . . ? C104 C105 Nd1 74.7(4) . . ? C106 C105 Nd1 74.3(4) . . ? C107 C106 C105 132.7(8) . . ? C107 C106 Nd1 74.4(4) . . ? C105 C106 Nd1 73.5(4) . . ? C100 C107 C106 136.5(8) . . ? C100 C107 Nd1 76.0(4) . . ? C106 C107 Nd1 74.6(4) . . ? C207 C200 C201 133.8(11) . . ? C207 C200 Nd2 75.2(5) . . ? C201 C200 Nd2 74.2(5) . . ? C202 C201 C200 136.0(10) . . ? C202 C201 Nd2 75.3(5) . . ? C200 C201 Nd2 74.9(5) . . ? C203 C202 C201 135.1(10) . . ? C203 C202 Nd2 74.2(5) . . ? C201 C202 Nd2 74.2(5) . . ? C202 C203 C204 135.4(10) . . ? C202 C203 Nd2 75.4(5) . . ? C204 C203 Nd2 75.2(5) . . ? C205 C204 C203 135.1(10) . . ? C205 C204 Nd2 75.2(5) . . ? C203 C204 Nd2 73.6(5) . . ? C204 C205 C206 134.4(11) . . ? C204 C205 Nd2 74.5(5) . . ? C206 C205 Nd2 74.5(6) . . ? C205 C206 C207 134.9(11) . . ? C205 C206 Nd2 74.8(6) . . ? C207 C206 Nd2 74.4(6) . . ? C200 C207 C206 135.2(11) . . ? C200 C207 Nd2 74.1(5) . . ? C206 C207 Nd2 74.5(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.78 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.351 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.084 ##################################################################