# Copyright The Royal Society of Chemistry, 1998 # CCDC Number: 186/1167 data_as15 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H130 B2 Mo2 N12 O10 Sm2' _chemical_formula_weight 1958.18 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' 'Mo' 'Mo' -1.6832 0.6857 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6825(5) _cell_length_b 13.7204(5) _cell_length_c 15.1643(6) _cell_angle_alpha 63.455(2) _cell_angle_beta 67.914(2) _cell_angle_gamma 88.812(2) _cell_volume 2322.26(15) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 13261 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.44 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.567 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.361 _exptl_absorpt_correction_T_max 0.502 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17258 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 28.48 _reflns_number_total 10241 _reflns_number_gt 9234 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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 w=1/[\s^2^(Fo^2^)+(0.0261P)^2^+1.1740P] 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 0.00045(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10241 _refine_ls_number_parameters 512 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0305 _refine_ls_R_factor_gt 0.0252 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.612315(16) 1.323773(16) -0.095608(17) 0.02405(6) Uani 1 d . . . C1 C 0.4872(2) 1.2183(2) 0.0145(2) 0.0275(5) Uani 1 d . . . O1 O 0.40992(15) 1.14812(15) 0.07936(15) 0.0362(4) Uani 1 d . . . C2 C 0.6835(2) 1.2612(2) 0.0027(3) 0.0387(6) Uani 1 d . . . O2 O 0.7256(2) 1.2252(2) 0.0614(2) 0.0648(7) Uani 1 d . . . C3 C 0.6399(2) 1.2067(2) -0.1309(2) 0.0276(5) Uani 1 d . . . O3 O 0.65103(17) 1.13314(16) -0.15216(16) 0.0409(5) Uani 1 d . . . C4 C 0.6606(2) 1.4661(2) -0.2764(2) 0.0367(6) Uani 1 d . . . C5 C 0.5538(2) 1.4665(2) -0.2154(2) 0.0378(6) Uani 1 d . . . H5 H 0.4930 1.4492 -0.2251 0.045 Uiso 1 calc R . . C6 C 0.5520(3) 1.4969(2) -0.1377(2) 0.0436(7) Uani 1 d . . . H6 H 0.4902 1.5041 -0.0863 0.052 Uiso 1 calc R . . C7 C 0.6563(3) 1.5146(2) -0.1495(3) 0.0433(7) Uani 1 d . . . H7 H 0.6783 1.5356 -0.1070 0.052 Uiso 1 calc R . . C8 C 0.7244(2) 1.4964(2) -0.2346(2) 0.0379(6) Uani 1 d . . . H8 H 0.8001 1.5032 -0.2597 0.045 Uiso 1 calc R . . C9 C 0.6988(4) 1.4466(3) -0.3721(3) 0.0642(11) Uani 1 d . . . H9A H 0.7646 1.4153 -0.3781 0.096 Uiso 1 calc R . . H9B H 0.7134 1.5170 -0.4377 0.096 Uiso 1 calc R . . H9C H 0.6435 1.3948 -0.3636 0.096 Uiso 1 calc R . . Sm1 Sm 0.336100(9) 0.973187(9) 0.258572(9) 0.01991(5) Uani 1 d . . . N1 N 0.17126(16) 0.81250(16) 0.39425(17) 0.0256(4) Uani 1 d . . . N2 N 0.17816(16) 0.73778(16) 0.48868(17) 0.0253(4) Uani 1 d . . . C10 C 0.0843(2) 0.7705(2) 0.3929(2) 0.0327(6) Uani 1 d . . . C11 C 0.0353(2) 0.6695(2) 0.4865(3) 0.0424(7) Uani 1 d . . . H11 H -0.0277 0.6229 0.5059 0.051 Uiso 1 calc R . . C12 C 0.0959(2) 0.6506(2) 0.5450(2) 0.0372(6) Uani 1 d . . . C13 C 0.0458(2) 0.8256(3) 0.3035(3) 0.0413(7) Uani 1 d . . . C14 C 0.1140(3) 0.9363(3) 0.2134(3) 0.0528(8) Uani 1 d . . . H14A H 0.0843 0.9678 0.1590 0.079 Uiso 1 calc R . . H14B H 0.1874 0.9261 0.1799 0.079 Uiso 1 calc R . . H14C H 0.1146 0.9867 0.2430 0.079 Uiso 1 calc R . . C15 C 0.0461(3) 0.7484(3) 0.2553(3) 0.0680(11) Uani 1 d . . . H15A H -0.0002 0.6773 0.3122 0.102 Uiso 1 calc R . . H15B H 0.1193 0.7365 0.2242 0.102 Uiso 1 calc R . . H15C H 0.0193 0.7821 0.1987 0.102 Uiso 1 calc R . . C16 C -0.0690(3) 0.8434(4) 0.3528(4) 0.0753(13) Uani 1 d . . . H16A H -0.1154 0.7717 0.4079 0.113 Uiso 1 calc R . . H16B H -0.0952 0.8793 0.2960 0.113 Uiso 1 calc R . . H16C H -0.0698 0.8905 0.3862 0.113 Uiso 1 calc R . . C17 C 0.0783(3) 0.5553(2) 0.6522(3) 0.0522(9) Uani 1 d . . . H17A H 0.0118 0.5051 0.6798 0.078 Uiso 1 calc R . . H17B H 0.0729 0.5828 0.7031 0.078 Uiso 1 calc R . . H17C H 0.1386 0.5154 0.6442 0.078 Uiso 1 calc R . . N3 N 0.43660(15) 0.82049(15) 0.34531(16) 0.0237(4) Uani 1 d . . . N4 N 0.37886(16) 0.74315(15) 0.45193(16) 0.0235(4) Uani 1 d . . . C18 C 0.5332(2) 0.7925(2) 0.3141(2) 0.0275(5) Uani 1 d . . . C19 C 0.5375(2) 0.6965(2) 0.4003(2) 0.0338(6) Uani 1 d . . . H19 H 0.5967 0.6590 0.3999 0.041 Uiso 1 calc R . . C20 C 0.4400(2) 0.6674(2) 0.4850(2) 0.0296(5) Uani 1 d . . . C21 C 0.62203(19) 0.8590(2) 0.2030(2) 0.0308(6) Uani 1 d . . . C22 C 0.7189(3) 0.8978(3) 0.2143(3) 0.0589(10) Uani 1 d . . . H22A H 0.7787 0.9361 0.1429 0.088 Uiso 1 calc R . . H22B H 0.7400 0.8336 0.2620 0.088 Uiso 1 calc R . . H22C H 0.6999 0.9485 0.2450 0.088 Uiso 1 calc R . . C23 C 0.5891(2) 0.9608(2) 0.1311(2) 0.0428(7) Uani 1 d . . . H23A H 0.6497 1.0021 0.0608 0.064 Uiso 1 calc R . . H23B H 0.5677 1.0082 0.1654 0.064 Uiso 1 calc R . . H23C H 0.5287 0.9375 0.1209 0.064 Uiso 1 calc R . . C24 C 0.6550(2) 0.7855(3) 0.1486(3) 0.0434(7) Uani 1 d . . . H24A H 0.7130 0.8282 0.0766 0.065 Uiso 1 calc R . . H24B H 0.5933 0.7595 0.1418 0.065 Uiso 1 calc R . . H24C H 0.6798 0.7217 0.1925 0.065 Uiso 1 calc R . . C25 C 0.4020(3) 0.5714(2) 0.5965(2) 0.0416(7) Uani 1 d . . . H25A H 0.4582 0.5264 0.6014 0.062 Uiso 1 calc R . . H25B H 0.3374 0.5261 0.6119 0.062 Uiso 1 calc R . . H25C H 0.3856 0.5988 0.6492 0.062 Uiso 1 calc R . . N5 N 0.32731(15) 0.96326(15) 0.43593(16) 0.0221(4) Uani 1 d . . . N6 N 0.27379(15) 0.86364(15) 0.52719(16) 0.0212(4) Uani 1 d . . . C26 C 0.33202(18) 1.03631(18) 0.47088(19) 0.0218(5) Uani 1 d . . . C27 C 0.2792(2) 0.9857(2) 0.5832(2) 0.0275(5) Uani 1 d . . . H27 H 0.2689 1.0197 0.6278 0.033 Uiso 1 calc R . . C28 C 0.24510(19) 0.8767(2) 0.6165(2) 0.0255(5) Uani 1 d . . . C29 C 0.39779(19) 1.15229(19) 0.3955(2) 0.0259(5) Uani 1 d . . . C30 C 0.4404(3) 1.1791(2) 0.2779(2) 0.0416(7) Uani 1 d . . . H30A H 0.4856 1.1258 0.2666 0.062 Uiso 1 calc R . . H30B H 0.4828 1.2541 0.2322 0.062 Uiso 1 calc R . . H30C H 0.3802 1.1748 0.2588 0.062 Uiso 1 calc R . . C31 C 0.3315(2) 1.2377(2) 0.4123(3) 0.0420(7) Uani 1 d . . . H31A H 0.3761 1.3115 0.3662 0.063 Uiso 1 calc R . . H31B H 0.3047 1.2207 0.4883 0.063 Uiso 1 calc R . . H31C H 0.2707 1.2358 0.3934 0.063 Uiso 1 calc R . . C32 C 0.4929(2) 1.1575(2) 0.4247(3) 0.0460(8) Uani 1 d . . . H32A H 0.5381 1.2310 0.3765 0.069 Uiso 1 calc R . . H32B H 0.5352 1.1012 0.4165 0.069 Uiso 1 calc R . . H32C H 0.4662 1.1436 0.4997 0.069 Uiso 1 calc R . . C33 C 0.1924(2) 0.7842(2) 0.7294(2) 0.0380(6) Uani 1 d . . . H33A H 0.1261 0.7468 0.7389 0.057 Uiso 1 calc R . . H33B H 0.1755 0.8138 0.7804 0.057 Uiso 1 calc R . . H33C H 0.2409 0.7312 0.7429 0.057 Uiso 1 calc R . . B1 B 0.2677(2) 0.7532(2) 0.5232(2) 0.0244(5) Uani 1 d . . . H1 H 0.2482 0.6921 0.5984 0.029 Uiso 1 calc R . . O4 O 0.20166(14) 1.10786(14) 0.28004(15) 0.0320(4) Uani 1 d . . . C34 C 0.1120(2) 1.0791(2) 0.3814(2) 0.0352(6) Uani 1 d . . . H34A H 0.1360 1.0892 0.4312 0.042 Uiso 1 calc R . . H34B H 0.0773 1.0010 0.4162 0.042 Uiso 1 calc R . . C35 C 0.0357(3) 1.1554(3) 0.3544(3) 0.0613(10) Uani 1 d . . . H35A H -0.0172 1.1219 0.3413 0.074 Uiso 1 calc R . . H35B H -0.0029 1.1735 0.4135 0.074 Uiso 1 calc R . . C36 C 0.1062(3) 1.2560(3) 0.2541(3) 0.0566(9) Uani 1 d . . . H36A H 0.1347 1.3074 0.2718 0.068 Uiso 1 calc R . . H36B H 0.0666 1.2953 0.2095 0.068 Uiso 1 calc R . . C37 C 0.1952(2) 1.2117(2) 0.1963(3) 0.0447(7) Uani 1 d . . . H37A H 0.1788 1.1991 0.1435 0.054 Uiso 1 calc R . . H37B H 0.2638 1.2643 0.1574 0.054 Uiso 1 calc R . . O5 O 0.1077(2) 1.3401(2) -0.0222(2) 0.0766(8) Uani 1 d . . . C38 C 0.0273(4) 1.3029(4) -0.0420(4) 0.0988(17) Uani 1 d . . . H38A H 0.0526 1.3277 -0.1203 0.119 Uiso 1 calc R . . H38B H -0.0373 1.3348 -0.0195 0.119 Uiso 1 calc R . . C39 C 0.0000(4) 1.1808(4) 0.0188(4) 0.0827(13) Uani 1 d . . . H39A H 0.0620 1.1494 -0.0089 0.124 Uiso 1 calc R . . H39B H -0.0606 1.1558 0.0099 0.124 Uiso 1 calc R . . H39C H -0.0194 1.1562 0.0956 0.124 Uiso 1 calc R . . C40 C 0.1502(5) 1.4500(4) -0.0850(4) 0.0996(17) Uani 1 d . . . H40A H 0.0923 1.4935 -0.0746 0.119 Uiso 1 calc R . . H40B H 0.1816 1.4675 -0.1620 0.119 Uiso 1 calc R . . C41 C 0.2345(5) 1.4832(5) -0.0590(5) 0.116(2) Uani 1 d . . . H41A H 0.2006 1.4931 0.0053 0.174 Uiso 1 calc R . . H41B H 0.2800 1.5529 -0.1201 0.174 Uiso 1 calc R . . H41C H 0.2784 1.4254 -0.0450 0.174 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 Mo1 0.02866(11) 0.02125(10) 0.02122(11) -0.00861(9) -0.01086(9) 0.00137(8) C1 0.0338(13) 0.0268(12) 0.0230(13) -0.0115(11) -0.0134(11) 0.0101(10) O1 0.0349(10) 0.0321(10) 0.0227(10) -0.0033(8) -0.0049(8) 0.0002(8) C2 0.0468(16) 0.0316(14) 0.0447(18) -0.0174(13) -0.0262(15) 0.0042(12) O2 0.0815(18) 0.0621(15) 0.0719(18) -0.0254(13) -0.0605(16) 0.0162(13) C3 0.0293(13) 0.0287(12) 0.0208(12) -0.0101(10) -0.0082(10) 0.0009(10) O3 0.0539(12) 0.0383(11) 0.0364(11) -0.0251(9) -0.0154(10) 0.0071(9) C4 0.0551(18) 0.0239(12) 0.0227(14) -0.0055(11) -0.0143(13) 0.0032(11) C5 0.0400(15) 0.0249(13) 0.0385(17) -0.0028(12) -0.0211(13) 0.0030(11) C6 0.0538(18) 0.0274(14) 0.0352(17) -0.0100(12) -0.0104(15) 0.0119(12) C7 0.068(2) 0.0257(13) 0.0388(17) -0.0142(13) -0.0249(16) 0.0002(13) C8 0.0371(15) 0.0250(13) 0.0378(17) -0.0058(12) -0.0124(13) -0.0028(11) C9 0.109(3) 0.0458(19) 0.0294(18) -0.0171(15) -0.021(2) 0.014(2) Sm1 0.02200(7) 0.01913(6) 0.01843(7) -0.00869(5) -0.00841(5) 0.00421(4) N1 0.0235(10) 0.0288(10) 0.0281(11) -0.0163(9) -0.0107(9) 0.0038(8) N2 0.0255(10) 0.0198(9) 0.0257(11) -0.0096(8) -0.0069(9) -0.0003(7) C10 0.0252(12) 0.0379(14) 0.0442(17) -0.0276(13) -0.0135(12) 0.0057(10) C11 0.0310(14) 0.0363(15) 0.057(2) -0.0213(14) -0.0152(14) -0.0056(11) C12 0.0314(14) 0.0282(13) 0.0446(17) -0.0175(13) -0.0076(13) -0.0035(10) C13 0.0304(14) 0.0594(19) 0.0507(19) -0.0359(16) -0.0210(14) 0.0093(13) C14 0.059(2) 0.059(2) 0.062(2) -0.0308(18) -0.0443(19) 0.0201(16) C15 0.078(3) 0.080(3) 0.073(3) -0.050(2) -0.039(2) 0.002(2) C16 0.0386(19) 0.133(4) 0.078(3) -0.062(3) -0.034(2) 0.035(2) C17 0.0468(18) 0.0279(14) 0.053(2) -0.0015(14) -0.0133(16) -0.0088(12) N3 0.0255(10) 0.0224(9) 0.0248(11) -0.0119(9) -0.0113(9) 0.0067(8) N4 0.0303(10) 0.0200(9) 0.0242(11) -0.0105(8) -0.0152(9) 0.0085(8) C18 0.0279(12) 0.0320(13) 0.0350(15) -0.0226(12) -0.0171(11) 0.0112(10) C19 0.0357(14) 0.0333(13) 0.0427(17) -0.0209(13) -0.0235(13) 0.0193(11) C20 0.0399(14) 0.0239(12) 0.0363(15) -0.0167(11) -0.0242(12) 0.0145(10) C21 0.0225(12) 0.0403(14) 0.0374(15) -0.0232(13) -0.0140(11) 0.0066(10) C22 0.0378(17) 0.093(3) 0.054(2) -0.041(2) -0.0176(16) -0.0086(17) C23 0.0330(15) 0.0398(15) 0.0376(17) -0.0134(13) -0.0024(13) 0.0041(12) C24 0.0423(16) 0.0539(18) 0.0430(18) -0.0326(16) -0.0151(14) 0.0156(14) C25 0.0591(19) 0.0288(14) 0.0394(17) -0.0114(13) -0.0291(15) 0.0198(13) N5 0.0263(10) 0.0182(9) 0.0210(10) -0.0079(8) -0.0105(8) 0.0037(7) N6 0.0250(10) 0.0192(9) 0.0193(10) -0.0082(8) -0.0101(8) 0.0038(7) C26 0.0228(11) 0.0223(11) 0.0262(13) -0.0128(10) -0.0145(10) 0.0070(8) C27 0.0328(13) 0.0292(12) 0.0284(14) -0.0185(11) -0.0145(11) 0.0084(10) C28 0.0256(12) 0.0297(12) 0.0235(13) -0.0133(10) -0.0116(10) 0.0067(9) C29 0.0289(12) 0.0208(11) 0.0306(14) -0.0124(10) -0.0144(11) 0.0037(9) C30 0.0514(17) 0.0299(14) 0.0314(16) -0.0124(12) -0.0067(14) -0.0092(12) C31 0.0487(17) 0.0222(13) 0.0506(19) -0.0156(13) -0.0181(15) 0.0103(11) C32 0.0422(16) 0.0346(15) 0.066(2) -0.0181(15) -0.0340(16) 0.0001(12) C33 0.0455(16) 0.0366(14) 0.0238(14) -0.0132(12) -0.0074(12) 0.0016(12) B1 0.0300(14) 0.0182(12) 0.0216(14) -0.0070(11) -0.0101(12) 0.0028(10) O4 0.0308(9) 0.0279(9) 0.0283(10) -0.0091(8) -0.0088(8) 0.0118(7) C34 0.0275(13) 0.0398(15) 0.0335(15) -0.0180(13) -0.0072(12) 0.0086(11) C35 0.0407(18) 0.0473(19) 0.067(3) -0.0156(18) -0.0086(17) 0.0211(15) C36 0.0383(17) 0.0364(16) 0.071(2) -0.0157(16) -0.0106(17) 0.0154(13) C37 0.0465(17) 0.0327(14) 0.0398(18) -0.0069(13) -0.0160(15) 0.0159(12) O5 0.0795(19) 0.080(2) 0.0606(18) -0.0159(15) -0.0409(16) 0.0060(15) C38 0.107(4) 0.094(4) 0.087(4) -0.017(3) -0.063(3) -0.001(3) C39 0.077(3) 0.092(3) 0.073(3) -0.036(3) -0.028(3) 0.016(3) C40 0.121(4) 0.081(3) 0.080(4) -0.006(3) -0.063(3) 0.000(3) C41 0.141(5) 0.094(4) 0.099(4) -0.006(3) -0.084(4) -0.012(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 Mo1 C3 1.897(3) . ? Mo1 C1 1.899(3) . ? Mo1 C2 1.955(3) . ? Mo1 C5 2.372(3) . ? Mo1 C8 2.379(3) . ? Mo1 C7 2.381(3) . ? Mo1 C4 2.382(3) . ? Mo1 C6 2.386(3) . ? C1 O1 1.194(3) . ? O1 Sm1 2.5244(18) . ? C2 O2 1.160(3) . ? C3 O3 1.181(3) . ? O3 Sm1 2.5773(18) 2_675 ? C4 C5 1.407(4) . ? C4 C8 1.416(4) . ? C4 C9 1.490(4) . ? C5 C6 1.407(4) . ? C6 C7 1.382(5) . ? C7 C8 1.404(4) . ? Sm1 O3 2.5773(18) 2_675 ? Sm1 N5 2.588(2) . ? Sm1 N3 2.6054(19) . ? Sm1 N1 2.616(2) . ? Sm1 O4 2.6173(17) . ? N1 C10 1.344(3) . ? N1 N2 1.377(3) . ? N2 C12 1.359(3) . ? N2 B1 1.553(3) . ? C10 C11 1.396(4) . ? C10 C13 1.513(4) . ? C11 C12 1.370(4) . ? C12 C17 1.494(4) . ? C13 C14 1.513(5) . ? C13 C15 1.532(4) . ? C13 C16 1.533(4) . ? N3 C18 1.338(3) . ? N3 N4 1.380(3) . ? N4 C20 1.358(3) . ? N4 B1 1.545(3) . ? C18 C19 1.401(4) . ? C18 C21 1.509(4) . ? C19 C20 1.366(4) . ? C20 C25 1.497(4) . ? C21 C23 1.525(4) . ? C21 C24 1.532(4) . ? C21 C22 1.532(4) . ? N5 C26 1.339(3) . ? N5 N6 1.381(3) . ? N6 C28 1.355(3) . ? N6 B1 1.549(3) . ? C26 C27 1.395(3) . ? C26 C29 1.519(3) . ? C27 C28 1.373(3) . ? C28 C33 1.493(4) . ? C29 C30 1.516(4) . ? C29 C31 1.520(3) . ? C29 C32 1.536(3) . ? O4 C34 1.443(3) . ? O4 C37 1.453(3) . ? C34 C35 1.499(4) . ? C35 C36 1.491(5) . ? C36 C37 1.505(4) . ? O5 C40 1.362(5) . ? O5 C38 1.404(5) . ? C38 C39 1.477(6) . ? C40 C41 1.490(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 C3 Mo1 C1 81.06(10) . . ? C3 Mo1 C2 89.09(11) . . ? C1 Mo1 C2 88.29(11) . . ? C3 Mo1 C5 112.11(11) . . ? C1 Mo1 C5 105.97(10) . . ? C2 Mo1 C5 155.74(10) . . ? C3 Mo1 C8 113.36(10) . . ? C1 Mo1 C8 160.23(10) . . ? C2 Mo1 C8 104.77(11) . . ? C5 Mo1 C8 56.89(10) . . ? C3 Mo1 C7 147.67(11) . . ? C1 Mo1 C7 130.05(11) . . ? C2 Mo1 C7 99.16(11) . . ? C5 Mo1 C7 56.63(10) . . ? C8 Mo1 C7 34.31(10) . . ? C3 Mo1 C4 95.65(10) . . ? C1 Mo1 C4 135.26(11) . . ? C2 Mo1 C4 136.42(11) . . ? C5 Mo1 C4 34.43(10) . . ? C8 Mo1 C4 34.60(10) . . ? C7 Mo1 C4 57.29(10) . . ? C3 Mo1 C6 146.47(11) . . ? C1 Mo1 C6 103.70(11) . . ? C2 Mo1 C6 123.89(11) . . ? C5 Mo1 C6 34.40(11) . . ? C8 Mo1 C6 56.73(10) . . ? C7 Mo1 C6 33.71(11) . . ? C4 Mo1 C6 57.34(10) . . ? O1 C1 Mo1 175.3(2) . . ? C1 O1 Sm1 144.27(17) . . ? O2 C2 Mo1 179.1(3) . . ? O3 C3 Mo1 176.2(2) . . ? C3 O3 Sm1 158.71(19) . 2_675 ? C5 C4 C8 106.6(3) . . ? C5 C4 C9 126.1(3) . . ? C8 C4 C9 127.1(3) . . ? C5 C4 Mo1 72.39(15) . . ? C8 C4 Mo1 72.60(15) . . ? C9 C4 Mo1 124.0(2) . . ? C6 C5 C4 108.8(3) . . ? C6 C5 Mo1 73.34(16) . . ? C4 C5 Mo1 73.18(15) . . ? C7 C6 C5 107.9(3) . . ? C7 C6 Mo1 72.96(16) . . ? C5 C6 Mo1 72.26(15) . . ? C6 C7 C8 108.7(3) . . ? C6 C7 Mo1 73.33(16) . . ? C8 C7 Mo1 72.78(15) . . ? C7 C8 C4 108.1(3) . . ? C7 C8 Mo1 72.91(15) . . ? C4 C8 Mo1 72.80(15) . . ? O1 Sm1 O3 87.46(6) . 2_675 ? O1 Sm1 N5 123.14(6) . . ? O3 Sm1 N5 146.53(6) 2_675 . ? O1 Sm1 N3 129.01(6) . . ? O3 Sm1 N3 81.15(6) 2_675 . ? N5 Sm1 N3 69.22(6) . . ? O1 Sm1 N1 144.10(6) . . ? O3 Sm1 N1 78.77(6) 2_675 . ? N5 Sm1 N1 81.78(6) . . ? N3 Sm1 N1 81.69(6) . . ? O1 Sm1 O4 74.66(6) . . ? O3 Sm1 O4 125.21(6) 2_675 . ? N5 Sm1 O4 80.03(6) . . ? N3 Sm1 O4 148.27(6) . . ? N1 Sm1 O4 86.47(6) . . ? C10 N1 N2 106.6(2) . . ? C10 N1 Sm1 137.22(18) . . ? N2 N1 Sm1 115.35(13) . . ? C12 N2 N1 109.7(2) . . ? C12 N2 B1 126.2(2) . . ? N1 N2 B1 124.04(18) . . ? N1 C10 C11 109.5(2) . . ? N1 C10 C13 124.7(2) . . ? C11 C10 C13 125.8(2) . . ? C12 C11 C10 106.7(2) . . ? N2 C12 C11 107.6(2) . . ? N2 C12 C17 123.7(3) . . ? C11 C12 C17 128.7(2) . . ? C10 C13 C14 113.7(2) . . ? C10 C13 C15 108.5(3) . . ? C14 C13 C15 108.5(3) . . ? C10 C13 C16 108.3(3) . . ? C14 C13 C16 108.5(3) . . ? C15 C13 C16 109.3(3) . . ? C18 N3 N4 106.81(19) . . ? C18 N3 Sm1 137.21(17) . . ? N4 N3 Sm1 115.97(13) . . ? C20 N4 N3 109.4(2) . . ? C20 N4 B1 126.7(2) . . ? N3 N4 B1 123.46(18) . . ? N3 C18 C19 109.3(2) . . ? N3 C18 C21 123.4(2) . . ? C19 C18 C21 127.3(2) . . ? C20 C19 C18 106.6(2) . . ? N4 C20 C19 107.8(2) . . ? N4 C20 C25 123.6(2) . . ? C19 C20 C25 128.6(2) . . ? C18 C21 C23 112.5(2) . . ? C18 C21 C24 109.2(2) . . ? C23 C21 C24 108.9(2) . . ? C18 C21 C22 109.1(2) . . ? C23 C21 C22 108.3(3) . . ? C24 C21 C22 108.8(2) . . ? C26 N5 N6 106.23(18) . . ? C26 N5 Sm1 135.99(15) . . ? N6 N5 Sm1 114.31(13) . . ? C28 N6 N5 109.71(18) . . ? C28 N6 B1 127.1(2) . . ? N5 N6 B1 122.42(19) . . ? N5 C26 C27 110.1(2) . . ? N5 C26 C29 122.2(2) . . ? C27 C26 C29 127.4(2) . . ? C28 C27 C26 106.2(2) . . ? N6 C28 C27 107.8(2) . . ? N6 C28 C33 123.9(2) . . ? C27 C28 C33 128.2(2) . . ? C30 C29 C26 112.0(2) . . ? C30 C29 C31 109.6(2) . . ? C26 C29 C31 110.5(2) . . ? C30 C29 C32 108.9(2) . . ? C26 C29 C32 107.3(2) . . ? C31 C29 C32 108.5(2) . . ? N4 B1 N6 110.41(19) . . ? N4 B1 N2 113.0(2) . . ? N6 B1 N2 111.89(19) . . ? C34 O4 C37 109.6(2) . . ? C34 O4 Sm1 121.85(14) . . ? C37 O4 Sm1 128.14(16) . . ? O4 C34 C35 106.0(2) . . ? C36 C35 C34 103.9(3) . . ? C35 C36 C37 104.2(2) . . ? O4 C37 C36 105.6(2) . . ? C40 O5 C38 115.4(4) . . ? O5 C38 C39 110.0(4) . . ? O5 C40 C41 112.2(4) . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 1.233 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.081 #=END data_as11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H130 B2 Mo2 N12 O10 Yb2' _chemical_formula_weight 2003.56 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' 'Mo' 'Mo' -1.6832 0.6857 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.6797(7) _cell_length_b 13.7364(8) _cell_length_c 15.1241(8) _cell_angle_alpha 63.213(2) _cell_angle_beta 67.115(2) _cell_angle_gamma 89.525(2) _cell_volume 2288.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 10980 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 28.58 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 2.351 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.556 _exptl_absorpt_correction_T_max 0.910 _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15610 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0594 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 28.60 _reflns_number_total 9993 _reflns_number_gt 8412 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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 w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+0.3151P] 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 0.00118(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9993 _refine_ls_number_parameters 512 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0698 _refine_ls_wR_factor_gt 0.0646 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.61304(3) 1.31692(3) -0.09821(3) 0.02062(8) Uani 1 d . . . C1 C 0.4906(3) 1.2038(3) 0.0187(3) 0.0237(8) Uani 1 d . . . O1 O 0.4156(2) 1.1284(2) 0.0881(2) 0.0291(7) Uani 1 d . . . C2 C 0.6918(4) 1.2587(4) -0.0072(4) 0.0337(10) Uani 1 d . . . O2 O 0.7393(3) 1.2270(3) 0.0456(3) 0.0557(10) Uani 1 d . . . C3 C 0.6405(3) 1.2034(3) -0.1389(3) 0.0233(8) Uani 1 d . . . O3 O 0.6518(2) 1.1312(2) -0.1623(2) 0.0328(7) Uani 1 d . . . C4 C 0.6609(4) 1.4657(3) -0.2795(3) 0.0329(10) Uani 1 d . . . C5 C 0.5518(4) 1.4582(3) -0.2148(3) 0.0342(11) Uani 1 d . . . H5 H 0.4917 1.4384 -0.2244 0.041 Uiso 1 calc R . . C6 C 0.5459(4) 1.4848(3) -0.1334(4) 0.0373(11) Uani 1 d . . . H6 H 0.4814 1.4864 -0.0793 0.045 Uiso 1 calc R . . C7 C 0.6503(4) 1.5081(3) -0.1456(3) 0.0344(10) Uani 1 d . . . H7 H 0.6696 1.5282 -0.1013 0.041 Uiso 1 calc R . . C8 C 0.7230(3) 1.4968(3) -0.2357(3) 0.0311(10) Uani 1 d . . . H8 H 0.7996 1.5079 -0.2623 0.037 Uiso 1 calc R . . C9 C 0.7062(5) 1.4517(4) -0.3797(4) 0.0642(17) Uani 1 d . . . H9A H 0.7747 1.4262 -0.3874 0.096 Uiso 1 calc R . . H9B H 0.7190 1.5232 -0.4448 0.096 Uiso 1 calc R . . H9C H 0.6544 1.3966 -0.3725 0.096 Uiso 1 calc R . . Yb1 Yb 0.335143(13) 0.967150(14) 0.265846(13) 0.01763(6) Uani 1 d . . . N1 N 0.1697(2) 0.8162(3) 0.3928(2) 0.0213(7) Uani 1 d . . . N2 N 0.1729(2) 0.7398(2) 0.4894(2) 0.0220(7) Uani 1 d . . . C10 C 0.0822(3) 0.7743(3) 0.3913(3) 0.0282(9) Uani 1 d . . . C11 C 0.0296(3) 0.6728(4) 0.4862(4) 0.0365(11) Uani 1 d . . . H11 H -0.0344 0.6261 0.5056 0.044 Uiso 1 calc R . . C12 C 0.0884(3) 0.6529(3) 0.5467(3) 0.0297(10) Uani 1 d . . . C13 C 0.0455(3) 0.8300(4) 0.3008(4) 0.0340(10) Uani 1 d . . . C14 C 0.1173(4) 0.9410(4) 0.2073(4) 0.0469(13) Uani 1 d . . . H14A H 0.0893 0.9715 0.1516 0.070 Uiso 1 calc R . . H14B H 0.1912 0.9306 0.1743 0.070 Uiso 1 calc R . . H14C H 0.1180 0.9927 0.2353 0.070 Uiso 1 calc R . . C15 C 0.0429(5) 0.7517(5) 0.2538(4) 0.0620(16) Uani 1 d . . . H15A H -0.0077 0.6813 0.3123 0.093 Uiso 1 calc R . . H15B H 0.1156 0.7371 0.2242 0.093 Uiso 1 calc R . . H15C H 0.0193 0.7868 0.1951 0.093 Uiso 1 calc R . . C16 C -0.0692(4) 0.8493(6) 0.3504(4) 0.0658(18) Uani 1 d . . . H16A H -0.1168 0.7788 0.4126 0.099 Uiso 1 calc R . . H16B H -0.0970 0.8783 0.2945 0.099 Uiso 1 calc R . . H16C H -0.0672 0.9033 0.3757 0.099 Uiso 1 calc R . . C17 C 0.0672(4) 0.5549(4) 0.6561(4) 0.0510(14) Uani 1 d . . . H17A H 0.0016 0.5026 0.6818 0.077 Uiso 1 calc R . . H17B H 0.0571 0.5807 0.7093 0.077 Uiso 1 calc R . . H17C H 0.1289 0.5176 0.6486 0.077 Uiso 1 calc R . . N3 N 0.4350(2) 0.8241(2) 0.3431(2) 0.0199(7) Uani 1 d . . . N4 N 0.3737(2) 0.7439(2) 0.4522(2) 0.0194(7) Uani 1 d . . . C18 C 0.5315(3) 0.7953(3) 0.3115(3) 0.0226(8) Uani 1 d . . . C19 C 0.5331(3) 0.6980(3) 0.3986(3) 0.0291(9) Uani 1 d . . . H19 H 0.5917 0.6602 0.3978 0.035 Uiso 1 calc R . . C20 C 0.4335(3) 0.6678(3) 0.4856(3) 0.0262(9) Uani 1 d . . . C21 C 0.6239(3) 0.8635(3) 0.1986(3) 0.0261(9) Uani 1 d . . . C22 C 0.7201(4) 0.9029(5) 0.2122(4) 0.0498(14) Uani 1 d . . . H22A H 0.7824 0.9432 0.1403 0.075 Uiso 1 calc R . . H22B H 0.7395 0.8382 0.2609 0.075 Uiso 1 calc R . . H22C H 0.6994 0.9524 0.2441 0.075 Uiso 1 calc R . . C23 C 0.5927(3) 0.9664(4) 0.1259(3) 0.0352(10) Uani 1 d . . . H23A H 0.6546 1.0084 0.0539 0.053 Uiso 1 calc R . . H23B H 0.5723 1.0136 0.1604 0.053 Uiso 1 calc R . . H23C H 0.5313 0.9430 0.1169 0.053 Uiso 1 calc R . . C24 C 0.6581(4) 0.7911(4) 0.1431(4) 0.0380(11) Uani 1 d . . . H24A H 0.7185 0.8351 0.0703 0.057 Uiso 1 calc R . . H24B H 0.5968 0.7653 0.1355 0.057 Uiso 1 calc R . . H24C H 0.6811 0.7268 0.1880 0.057 Uiso 1 calc R . . C25 C 0.3930(4) 0.5709(3) 0.5975(3) 0.0346(10) Uani 1 d . . . H25A H 0.4489 0.5264 0.6023 0.052 Uiso 1 calc R . . H25B H 0.3277 0.5250 0.6131 0.052 Uiso 1 calc R . . H25C H 0.3754 0.5972 0.6513 0.052 Uiso 1 calc R . . N5 N 0.3285(2) 0.9657(2) 0.4325(2) 0.0188(7) Uani 1 d . . . N6 N 0.2704(2) 0.8654(2) 0.5269(2) 0.0194(7) Uani 1 d . . . C26 C 0.3354(3) 1.0393(3) 0.4664(3) 0.0191(8) Uani 1 d . . . C27 C 0.2801(3) 0.9886(3) 0.5806(3) 0.0261(9) Uani 1 d . . . H27 H 0.2711 1.0228 0.6249 0.031 Uiso 1 calc R . . C28 C 0.2415(3) 0.8798(3) 0.6159(3) 0.0219(8) Uani 1 d . . . C29 C 0.4053(3) 1.1547(3) 0.3894(3) 0.0225(8) Uani 1 d . . . C30 C 0.4533(4) 1.1815(4) 0.2698(3) 0.0428(12) Uani 1 d . . . H30A H 0.4986 1.1281 0.2602 0.064 Uiso 1 calc R . . H30B H 0.4977 1.2571 0.2230 0.064 Uiso 1 calc R . . H30C H 0.3947 1.1766 0.2491 0.064 Uiso 1 calc R . . C31 C 0.3416(4) 1.2420(4) 0.4019(4) 0.0404(11) Uani 1 d . . . H31A H 0.3896 1.3157 0.3541 0.061 Uiso 1 calc R . . H31B H 0.3119 1.2262 0.4784 0.061 Uiso 1 calc R . . H31C H 0.2822 1.2407 0.3813 0.061 Uiso 1 calc R . . C32 C 0.4986(4) 1.1606(4) 0.4206(4) 0.0477(13) Uani 1 d . . . H32A H 0.5445 1.2353 0.3728 0.071 Uiso 1 calc R . . H32B H 0.5419 1.1056 0.4118 0.071 Uiso 1 calc R . . H32C H 0.4687 1.1445 0.4972 0.071 Uiso 1 calc R . . C33 C 0.1847(4) 0.7863(4) 0.7315(3) 0.0381(11) Uani 1 d . . . H33A H 0.1186 0.7475 0.7410 0.057 Uiso 1 calc R . . H33B H 0.1658 0.8162 0.7825 0.057 Uiso 1 calc R . . H33C H 0.2327 0.7339 0.7466 0.057 Uiso 1 calc R . . B1 B 0.2619(4) 0.7547(4) 0.5242(4) 0.0222(9) Uani 1 d . . . H1 H 0.2398 0.6930 0.6009 0.027 Uiso 1 calc R . . O4 O 0.2123(2) 1.1019(2) 0.2781(2) 0.0281(6) Uani 1 d . . . C34 C 0.1196(3) 1.0764(3) 0.3800(3) 0.0290(9) Uani 1 d . . . H34A H 0.1431 1.0883 0.4292 0.035 Uiso 1 calc R . . H34B H 0.0819 0.9979 0.4182 0.035 Uiso 1 calc R . . C35 C 0.0465(4) 1.1525(4) 0.3503(4) 0.0562(15) Uani 1 d . . . H35A H 0.0087 1.1734 0.4079 0.067 Uiso 1 calc R . . H35B H -0.0081 1.1172 0.3401 0.067 Uiso 1 calc R . . C36 C 0.1196(4) 1.2514(4) 0.2457(4) 0.0510(14) Uani 1 d . . . H36A H 0.1471 1.3068 0.2599 0.061 Uiso 1 calc R . . H36B H 0.0813 1.2871 0.1992 0.061 Uiso 1 calc R . . C37 C 0.2110(4) 1.2067(4) 0.1911(3) 0.0376(11) Uani 1 d . . . H37A H 0.1987 1.1944 0.1362 0.045 Uiso 1 calc R . . H37B H 0.2807 1.2597 0.1535 0.045 Uiso 1 calc R . . O5 O 0.1079(3) 1.3422(3) -0.0220(3) 0.0687(12) Uani 1 d . . . C38 C 0.0281(5) 1.3034(5) -0.0410(5) 0.079(2) Uani 1 d . . . H38A H 0.0530 1.3331 -0.1209 0.095 Uiso 1 calc R . . H38B H -0.0388 1.3301 -0.0135 0.095 Uiso 1 calc R . . C39 C 0.0043(5) 1.1804(5) 0.0150(5) 0.0728(18) Uani 1 d . . . H39A H 0.0689 1.1542 -0.0166 0.109 Uiso 1 calc R . . H39B H -0.0553 1.1543 0.0054 0.109 Uiso 1 calc R . . H39C H -0.0164 1.1510 0.0935 0.109 Uiso 1 calc R . . C40 C 0.1488(5) 1.4561(6) -0.0845(5) 0.084(2) Uani 1 d . . . H40A H 0.0890 1.4958 -0.0695 0.101 Uiso 1 calc R . . H40B H 0.1797 1.4776 -0.1633 0.101 Uiso 1 calc R . . C41 C 0.2342(6) 1.4908(6) -0.0605(6) 0.103(3) Uani 1 d . . . H41A H 0.2024 1.4755 0.0160 0.154 Uiso 1 calc R . . H41B H 0.2642 1.5707 -0.1096 0.154 Uiso 1 calc R . . H41C H 0.2920 1.4491 -0.0719 0.154 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 Mo1 0.02297(18) 0.01828(18) 0.01902(17) -0.00874(14) -0.00792(15) 0.00177(13) C1 0.030(2) 0.028(2) 0.021(2) -0.0166(18) -0.0127(18) 0.0116(17) O1 0.0255(16) 0.0277(16) 0.0197(14) -0.0055(12) -0.0034(12) 0.0000(12) C2 0.038(3) 0.027(2) 0.037(3) -0.017(2) -0.015(2) 0.0030(19) O2 0.064(2) 0.056(2) 0.069(2) -0.025(2) -0.055(2) 0.0161(18) C3 0.021(2) 0.026(2) 0.0173(19) -0.0080(17) -0.0060(16) 0.0001(16) O3 0.0410(18) 0.0329(17) 0.0302(16) -0.0212(14) -0.0135(14) 0.0071(13) C4 0.053(3) 0.014(2) 0.022(2) -0.0044(17) -0.013(2) 0.0049(18) C5 0.035(3) 0.022(2) 0.037(3) -0.0033(19) -0.021(2) -0.0003(18) C6 0.045(3) 0.025(2) 0.032(2) -0.011(2) -0.011(2) 0.013(2) C7 0.042(3) 0.024(2) 0.033(2) -0.0144(19) -0.011(2) -0.0011(19) C8 0.029(2) 0.022(2) 0.034(2) -0.0100(19) -0.010(2) -0.0005(17) C9 0.115(5) 0.035(3) 0.028(3) -0.011(2) -0.022(3) 0.007(3) Yb1 0.01915(9) 0.01703(9) 0.01617(9) -0.00848(6) -0.00662(7) 0.00338(6) N1 0.0207(17) 0.0243(18) 0.0207(16) -0.0130(14) -0.0082(14) 0.0045(13) N2 0.0230(18) 0.0159(17) 0.0215(17) -0.0075(14) -0.0064(14) 0.0013(13) C10 0.020(2) 0.034(2) 0.038(2) -0.024(2) -0.0115(19) 0.0059(17) C11 0.026(2) 0.030(2) 0.047(3) -0.016(2) -0.012(2) -0.0062(18) C12 0.025(2) 0.027(2) 0.029(2) -0.0127(19) -0.0049(19) -0.0017(17) C13 0.028(2) 0.049(3) 0.038(3) -0.028(2) -0.018(2) 0.010(2) C14 0.048(3) 0.047(3) 0.052(3) -0.017(3) -0.035(3) 0.013(2) C15 0.082(4) 0.068(4) 0.061(4) -0.044(3) -0.040(3) 0.009(3) C16 0.035(3) 0.121(6) 0.061(4) -0.054(4) -0.028(3) 0.032(3) C17 0.042(3) 0.021(2) 0.055(3) 0.005(2) -0.015(3) -0.009(2) N3 0.0214(17) 0.0175(16) 0.0190(16) -0.0077(13) -0.0084(14) 0.0024(13) N4 0.0236(17) 0.0166(16) 0.0206(16) -0.0096(13) -0.0113(14) 0.0089(13) C18 0.023(2) 0.026(2) 0.030(2) -0.0200(18) -0.0149(18) 0.0094(16) C19 0.028(2) 0.027(2) 0.037(2) -0.0162(19) -0.018(2) 0.0145(17) C20 0.032(2) 0.020(2) 0.033(2) -0.0139(18) -0.019(2) 0.0100(17) C21 0.016(2) 0.036(2) 0.030(2) -0.0188(19) -0.0096(18) 0.0055(17) C22 0.035(3) 0.069(4) 0.048(3) -0.031(3) -0.016(2) -0.006(2) C23 0.027(2) 0.035(3) 0.028(2) -0.011(2) -0.0011(19) 0.0025(19) C24 0.035(3) 0.046(3) 0.041(3) -0.030(2) -0.012(2) 0.014(2) C25 0.044(3) 0.024(2) 0.031(2) -0.0083(19) -0.018(2) 0.0135(19) N5 0.0227(17) 0.0149(16) 0.0190(16) -0.0088(13) -0.0085(14) 0.0048(12) N6 0.0201(17) 0.0211(17) 0.0134(15) -0.0068(13) -0.0057(13) 0.0021(13) C26 0.0188(19) 0.022(2) 0.0221(19) -0.0134(16) -0.0104(16) 0.0072(15) C27 0.031(2) 0.030(2) 0.026(2) -0.0196(18) -0.0145(19) 0.0091(17) C28 0.024(2) 0.022(2) 0.0198(19) -0.0111(16) -0.0090(17) 0.0067(16) C29 0.025(2) 0.0164(19) 0.030(2) -0.0121(17) -0.0139(18) 0.0045(15) C30 0.052(3) 0.031(3) 0.029(2) -0.016(2) 0.000(2) -0.014(2) C31 0.039(3) 0.025(2) 0.050(3) -0.019(2) -0.011(2) 0.013(2) C32 0.046(3) 0.031(3) 0.073(4) -0.018(3) -0.040(3) 0.003(2) C33 0.045(3) 0.039(3) 0.021(2) -0.014(2) -0.008(2) 0.004(2) B1 0.029(3) 0.015(2) 0.019(2) -0.0075(18) -0.009(2) 0.0041(18) O4 0.0278(16) 0.0245(15) 0.0233(15) -0.0085(12) -0.0067(13) 0.0094(12) C34 0.026(2) 0.033(2) 0.026(2) -0.0158(19) -0.0067(18) 0.0096(18) C35 0.040(3) 0.046(3) 0.052(3) -0.012(3) -0.005(3) 0.020(2) C36 0.034(3) 0.038(3) 0.061(3) -0.016(3) -0.012(3) 0.016(2) C37 0.039(3) 0.025(2) 0.031(2) -0.0051(19) -0.009(2) 0.0113(19) O5 0.064(3) 0.073(3) 0.059(2) -0.017(2) -0.035(2) 0.005(2) C38 0.072(5) 0.081(5) 0.068(4) -0.009(4) -0.047(4) 0.002(4) C39 0.063(4) 0.084(5) 0.061(4) -0.031(4) -0.022(3) 0.022(3) C40 0.082(5) 0.076(5) 0.065(4) -0.004(4) -0.042(4) -0.005(4) C41 0.109(6) 0.088(6) 0.091(5) -0.008(4) -0.067(5) -0.014(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 Mo1 C1 1.900(4) . ? Mo1 C3 1.905(4) . ? Mo1 C2 1.960(5) . ? Mo1 C5 2.370(4) . ? Mo1 C6 2.384(4) . ? Mo1 C8 2.385(4) . ? Mo1 C4 2.387(4) . ? Mo1 C7 2.390(4) . ? C1 O1 1.195(4) . ? O1 Yb1 2.390(3) . ? C2 O2 1.155(5) . ? C3 O3 1.184(5) . ? O3 Yb1 2.449(3) 2_675 ? C4 C5 1.405(6) . ? C4 C8 1.429(6) . ? C4 C9 1.499(6) . ? C5 C6 1.408(6) . ? C6 C7 1.388(6) . ? C7 C8 1.416(6) . ? Yb1 O3 2.449(3) 2_675 ? Yb1 N5 2.478(3) . ? Yb1 N1 2.494(3) . ? Yb1 N3 2.494(3) . ? Yb1 O4 2.510(3) . ? N1 C10 1.344(5) . ? N1 N2 1.381(4) . ? N2 C12 1.350(5) . ? N2 B1 1.549(5) . ? C10 C11 1.391(6) . ? C10 C13 1.516(6) . ? C11 C12 1.379(6) . ? C12 C17 1.503(6) . ? C13 C14 1.514(6) . ? C13 C16 1.534(6) . ? C13 C15 1.540(6) . ? N3 C18 1.341(5) . ? N3 N4 1.393(4) . ? N4 C20 1.359(5) . ? N4 B1 1.547(5) . ? C18 C19 1.399(5) . ? C18 C21 1.513(5) . ? C19 C20 1.372(5) . ? C20 C25 1.482(5) . ? C21 C23 1.531(6) . ? C21 C24 1.533(6) . ? C21 C22 1.546(5) . ? N5 C26 1.341(4) . ? N5 N6 1.389(4) . ? N6 C28 1.354(5) . ? N6 B1 1.546(5) . ? C26 C27 1.396(5) . ? C26 C29 1.509(5) . ? C27 C28 1.368(5) . ? C28 C33 1.499(5) . ? C29 C31 1.514(5) . ? C29 C30 1.522(5) . ? C29 C32 1.537(5) . ? O4 C34 1.451(4) . ? O4 C37 1.455(5) . ? C34 C35 1.484(6) . ? C35 C36 1.484(6) . ? C36 C37 1.504(6) . ? O5 C40 1.387(7) . ? O5 C38 1.397(6) . ? C38 C39 1.477(8) . ? C40 C41 1.489(8) . ? 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 Mo1 C3 80.94(16) . . ? C1 Mo1 C2 88.28(16) . . ? C3 Mo1 C2 90.20(17) . . ? C1 Mo1 C5 107.99(15) . . ? C3 Mo1 C5 110.73(16) . . ? C2 Mo1 C5 154.91(16) . . ? C1 Mo1 C6 103.78(16) . . ? C3 Mo1 C6 144.99(16) . . ? C2 Mo1 C6 124.28(17) . . ? C5 Mo1 C6 34.45(15) . . ? C1 Mo1 C8 160.62(16) . . ? C3 Mo1 C8 114.84(15) . . ? C2 Mo1 C8 102.21(16) . . ? C5 Mo1 C8 57.08(14) . . ? C6 Mo1 C8 56.85(15) . . ? C1 Mo1 C4 138.03(16) . . ? C3 Mo1 C4 95.74(15) . . ? C2 Mo1 C4 133.69(17) . . ? C5 Mo1 C4 34.34(15) . . ? C6 Mo1 C4 57.33(15) . . ? C8 Mo1 C4 34.85(14) . . ? C1 Mo1 C7 128.58(16) . . ? C3 Mo1 C7 149.28(15) . . ? C2 Mo1 C7 98.08(16) . . ? C5 Mo1 C7 56.87(15) . . ? C6 Mo1 C7 33.80(15) . . ? C8 Mo1 C7 34.49(14) . . ? C4 Mo1 C7 57.58(14) . . ? O1 C1 Mo1 175.2(3) . . ? C1 O1 Yb1 149.1(3) . . ? O2 C2 Mo1 178.3(4) . . ? O3 C3 Mo1 176.4(3) . . ? C3 O3 Yb1 159.4(3) . 2_675 ? C5 C4 C8 106.6(4) . . ? C5 C4 C9 127.6(4) . . ? C8 C4 C9 125.7(5) . . ? C5 C4 Mo1 72.1(2) . . ? C8 C4 Mo1 72.5(2) . . ? C9 C4 Mo1 123.4(3) . . ? C4 C5 C6 108.9(4) . . ? C4 C5 Mo1 73.5(2) . . ? C6 C5 Mo1 73.3(2) . . ? C7 C6 C5 108.4(4) . . ? C7 C6 Mo1 73.3(3) . . ? C5 C6 Mo1 72.2(3) . . ? C6 C7 C8 108.1(4) . . ? C6 C7 Mo1 72.9(2) . . ? C8 C7 Mo1 72.6(2) . . ? C7 C8 C4 108.0(4) . . ? C7 C8 Mo1 72.9(2) . . ? C4 C8 Mo1 72.7(2) . . ? O1 Yb1 O3 83.91(9) . 2_675 ? O1 Yb1 N5 122.78(9) . . ? O3 Yb1 N5 149.48(10) 2_675 . ? O1 Yb1 N1 141.88(10) . . ? O3 Yb1 N1 78.48(9) 2_675 . ? N5 Yb1 N1 86.02(10) . . ? O1 Yb1 N3 124.32(10) . . ? O3 Yb1 N3 80.79(10) 2_675 . ? N5 Yb1 N3 71.95(10) . . ? N1 Yb1 N3 85.94(10) . . ? O1 Yb1 O4 75.38(9) . . ? O3 Yb1 O4 124.20(9) 2_675 . ? N5 Yb1 O4 80.45(9) . . ? N1 Yb1 O4 87.03(9) . . ? N3 Yb1 O4 151.91(9) . . ? C10 N1 N2 106.3(3) . . ? C10 N1 Yb1 139.2(3) . . ? N2 N1 Yb1 113.5(2) . . ? C12 N2 N1 110.0(3) . . ? C12 N2 B1 126.3(3) . . ? N1 N2 B1 123.6(3) . . ? N1 C10 C11 109.7(4) . . ? N1 C10 C13 125.3(4) . . ? C11 C10 C13 125.1(4) . . ? C12 C11 C10 106.6(4) . . ? N2 C12 C11 107.4(4) . . ? N2 C12 C17 124.0(4) . . ? C11 C12 C17 128.6(4) . . ? C14 C13 C10 114.0(3) . . ? C14 C13 C16 108.1(4) . . ? C10 C13 C16 108.5(4) . . ? C14 C13 C15 108.4(4) . . ? C10 C13 C15 108.7(4) . . ? C16 C13 C15 109.2(4) . . ? C18 N3 N4 106.2(3) . . ? C18 N3 Yb1 139.9(3) . . ? N4 N3 Yb1 113.8(2) . . ? C20 N4 N3 109.5(3) . . ? C20 N4 B1 127.3(3) . . ? N3 N4 B1 122.6(3) . . ? N3 C18 C19 109.9(3) . . ? N3 C18 C21 123.2(3) . . ? C19 C18 C21 126.8(3) . . ? C20 C19 C18 106.5(3) . . ? N4 C20 C19 107.8(3) . . ? N4 C20 C25 123.7(4) . . ? C19 C20 C25 128.5(4) . . ? C18 C21 C23 111.9(3) . . ? C18 C21 C24 109.5(3) . . ? C23 C21 C24 109.3(3) . . ? C18 C21 C22 108.3(3) . . ? C23 C21 C22 108.3(4) . . ? C24 C21 C22 109.6(4) . . ? C26 N5 N6 106.2(3) . . ? C26 N5 Yb1 138.3(2) . . ? N6 N5 Yb1 112.0(2) . . ? C28 N6 N5 109.3(3) . . ? C28 N6 B1 127.9(3) . . ? N5 N6 B1 121.9(3) . . ? N5 C26 C27 110.0(3) . . ? N5 C26 C29 122.5(3) . . ? C27 C26 C29 127.1(3) . . ? C28 C27 C26 106.2(3) . . ? N6 C28 C27 108.3(3) . . ? N6 C28 C33 123.1(3) . . ? C27 C28 C33 128.4(4) . . ? C26 C29 C31 110.9(3) . . ? C26 C29 C30 112.4(3) . . ? C31 C29 C30 109.1(4) . . ? C26 C29 C32 107.7(3) . . ? C31 C29 C32 107.9(4) . . ? C30 C29 C32 108.6(4) . . ? N6 B1 N4 110.7(3) . . ? N6 B1 N2 112.0(3) . . ? N4 B1 N2 112.6(3) . . ? C34 O4 C37 108.7(3) . . ? C34 O4 Yb1 121.7(2) . . ? C37 O4 Yb1 129.3(2) . . ? O4 C34 C35 106.8(3) . . ? C34 C35 C36 104.4(4) . . ? C35 C36 C37 104.9(4) . . ? O4 C37 C36 106.2(3) . . ? C40 O5 C38 115.3(4) . . ? O5 C38 C39 110.4(5) . . ? O5 C40 C41 112.1(5) . . ? _diffrn_measured_fraction_theta_max 0.851 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 0.706 _refine_diff_density_min -0.698 _refine_diff_density_rms 0.115